data_71-b-100k _audit_creation_date 2021-05-28 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelxl_version_number 2013-4 _audit_contact_author_address ? _audit_contact_author_email ? _audit_contact_author_name '' _audit_contact_author_phone ? _publ_contact_author_id_orcid ? _publ_section_references ; Dolomanov, O.V., Bourhis, L.J., Gildea, R.J, Howard, J.A.K. & Puschmann, H. (2009), J. Appl. Cryst. 42, 339-341. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C20 H42 Cu5 I7 N4, 2(C2 H3 N)' _chemical_formula_sum 'C24 H48 Cu5 I7 N6' _chemical_formula_weight 1626.68 _chemical_absolute_configuration ad _chemical_melting_point ? _chemical_oxdiff_formula c20h20n2Cu1I2 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'I' 'I' -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'triclinic' _space_group_IT_number 1 _space_group_name_H-M_alt 'P 1' _space_group_name_Hall 'P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' _cell_length_a 8.69065(18) _cell_length_b 13.3957(3) _cell_length_c 18.0042(5) _cell_angle_alpha 89.407(2) _cell_angle_beta 89.889(2) _cell_angle_gamma 79.2342(19) _cell_volume 2059.01(9) _cell_formula_units_Z 2 _cell_measurement_reflns_used 10369 _cell_measurement_temperature 100.00(10) _cell_measurement_theta_max 29.5150 _cell_measurement_theta_min 4.1840 _shelx_estimated_absorpt_T_max 0.387 _shelx_estimated_absorpt_T_min 0.278 _exptl_absorpt_coefficient_mu 7.813 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.74328 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.40.53 (Rigaku Oxford Diffraction, 2019) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour ? _exptl_crystal_density_diffrn 2.624 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 1500 _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.15 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_unetI/netI 0.0565 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.833 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 17610 _diffrn_reflns_point_group_measured_fraction_full 0.693 _diffrn_reflns_point_group_measured_fraction_max 0.553 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.704 _diffrn_reflns_theta_min 3.289 _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 100.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 5.2169 _diffrn_detector_type AtlasS2 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.833 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames -------------------------------------------------------------------------- 1 \w -19.00 23.00 1.00 10.00 -- -10.30 -99.00 60.00 42 2 \w 0.00 72.00 1.00 10.00 -- 12.02 38.00 -90.00 72 3 \w -8.00 52.00 1.00 10.00 -- 12.02 -99.00 30.00 60 4 \w -57.00 24.00 1.00 10.00 -- 12.02 -19.00-120.00 81 5 \w -16.00 43.00 1.00 10.00 -- 12.02 -19.00 90.00 59 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at home/near, AtlasS2' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0033840000 _diffrn_orient_matrix_UB_12 -0.0129900000 _diffrn_orient_matrix_UB_13 0.0383312000 _diffrn_orient_matrix_UB_21 -0.0135459000 _diffrn_orient_matrix_UB_22 0.0523024000 _diffrn_orient_matrix_UB_23 0.0091057000 _diffrn_orient_matrix_UB_31 -0.0818971000 _diffrn_orient_matrix_UB_32 0.0010255000 _diffrn_orient_matrix_UB_33 0.0000777000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.328 _reflns_Friedel_fraction_full 0.389 _reflns_Friedel_fraction_max 0.273 _reflns_number_gt 12120 _reflns_number_total 12926 _reflns_odcompleteness_completeness 99.73 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 26.32 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_collection 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_data_reduction 'CrysAlisPro 1.171.40.53 (Rigaku OD, 2019)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution ? _refine_diff_density_max 1.507 _refine_diff_density_min -1.143 _refine_diff_density_rms 0.209 _refine_ls_abs_structure_details ; Classical Flack method preferred over Parsons because s.u. lower. ; _refine_ls_abs_structure_Flack 0.00(3) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 769 _refine_ls_number_reflns 12926 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.0392 _refine_ls_R_factor_gt 0.0355 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0356P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0806 _refine_ls_wR_factor_ref 0.0834 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Rigid bond restraints C8, C9, C4, C3 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005 C46, N9, C46, C45 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 3. Uiso/Uaniso restraints and constraints Uanis(C4) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(N9) \\sim Ueq, Uanis(C46) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002 4.a Ternary CH refined with riding coordinates: C37(H37), C17(H17), C27(H27), C7(H7) 4.b Secondary CH2 refined with riding coordinates: C34(H34A,H34B), C31(H31A,H31B), C22(H22A,H22B), C14(H14A,H14B), C25(H25A, H25B), C15(H15A,H15B), C1(H1A,H1B), C12(H12A,H12B), C13(H13A,H13B), C5(H5A, H5B), C39(H39A,H39B), C26(H26A,H26B), C33(H33A,H33B), C35(H35A,H35B), C32(H32A, H32B), C24(H24A,H24B), C21(H21A,H21B), C36(H36A,H36B), C23(H23A,H23B), C3(H3A, H3B), C11(H11A,H11B), C6(H6A,H6B), C16(H16A,H16B), C19(H19A,H19B), C28(H28A, H28B), C4(H4A,H4B), C2(H2A,H2B), C8(H8A,H8B) 4.c Idealised Me refined as rotating group: C40(H40A,H40B,H40C), C20(H20A,H20B,H20C), C30(H30A,H30B,H30C), C10(H10A,H10B, H10C), C18(H18A,H18B,H18C), C29(H29A,H29B,H29C), C9(H9A,H9B,H9C), C38(H38A, H38B,H38C), C41(H41A,H41B,H41C), C47(H47A,H47B,H47C), C43(H43A,H43B,H43C), C45(H45A,H45B,H45C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary ? _atom_sites_solution_secondary ? loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group I13 I 0.72429(8) 0.49464(5) 0.22416(4) 0.01682(16) Uani 1 1 d . . . . . I12 I 0.78042(8) 0.30918(5) 0.43048(4) 0.01614(16) Uani 1 1 d . . . . . I003 I 0.56026(7) 0.20491(6) 0.22386(4) 0.01715(16) Uani 1 1 d . . . . . I11 I 1.08356(8) 0.21712(6) 0.23444(4) 0.01660(16) Uani 1 1 d . . . . . I9 I 0.81234(8) 0.30079(5) 0.03562(4) 0.01671(16) Uani 1 1 d . . . . . I3 I 0.32820(8) 0.79736(5) 0.91742(4) 0.01684(16) Uani 1 1 d . . . . . I4 I 0.44413(8) 0.46852(6) 0.85525(4) 0.01751(16) Uani 1 1 d . . . . . I1 I 0.29615(8) 0.80811(6) 0.52007(4) 0.01668(16) Uani 1 1 d . . . . . I8 I 0.91981(8) -0.02786(5) 0.10076(5) 0.01879(17) Uani 1 1 d . . . . . I5 I 0.08443(8) 0.69847(6) 0.72944(5) 0.01967(17) Uani 1 1 d . . . . . I6 I 0.60515(8) 0.71539(6) 0.71972(4) 0.01813(17) Uani 1 1 d . . . . . I2 I 0.24748(8) 0.98952(6) 0.72845(5) 0.02055(17) Uani 1 1 d . . . . . I10 I 0.88167(10) -0.00963(6) 0.34411(5) 0.02636(19) Uani 1 1 d . . . . . I7 I 0.41370(11) 0.48945(7) 0.61123(5) 0.0316(2) Uani 1 1 d . . . . . Cu5 Cu 0.51494(15) 0.64913(11) 0.85221(9) 0.0180(3) Uani 1 1 d . . . . . Cu10 Cu 0.62762(15) 0.35686(11) 0.30524(8) 0.0170(3) Uani 1 1 d . . . . . Cu7 Cu 0.79657(16) 0.30089(11) 0.18167(9) 0.0202(3) Uani 1 1 d . . . . . Cu1 Cu 0.15237(15) 0.85184(11) 0.64693(8) 0.0180(3) Uani 1 1 d . . . . . Cu4 Cu 0.31726(16) 0.79493(12) 0.77167(9) 0.0219(3) Uani 1 1 d . . . . . Cu6 Cu 0.99472(15) 0.15136(11) 0.10391(9) 0.0183(3) Uani 1 1 d . . . . . Cu8 Cu 0.82840(17) 0.07937(12) 0.21300(9) 0.0250(3) Uani 1 1 d . . . . . Cu9 Cu 0.85803(18) 0.18700(12) 0.32518(9) 0.0262(4) Uani 1 1 d . . . . . Cu2 Cu 0.38312(18) 0.68607(12) 0.62679(9) 0.0261(4) Uani 1 1 d . . . . . Cu3 Cu 0.35710(18) 0.57657(12) 0.74136(9) 0.0266(4) Uani 1 1 d . . . . . N1 N -0.0758(11) 0.9283(7) 0.6147(6) 0.020(2) Uani 1 1 d . . . . . N3 N 0.7244(9) 0.6312(7) 0.9158(6) 0.017(2) Uani 1 1 d . . . . . N5 N 1.2050(10) 0.1283(7) 0.0404(6) 0.017(2) Uani 1 1 d . . . . . N7 N 0.4031(10) 0.4265(7) 0.3449(5) 0.015(2) Uani 1 1 d . . . . . N4 N 0.9812(10) 0.6113(7) 0.9923(5) 0.014(2) Uani 1 1 d . . . . . C34 C 0.2514(12) 0.5771(9) 0.4133(6) 0.016(2) Uani 1 1 d . . . . . H34A H 0.2502 0.5939 0.4656 0.020 Uiso 1 1 calc R . . . . H34B H 0.2276 0.6399 0.3847 0.020 Uiso 1 1 calc R . . . . C31 C 0.3339(12) 0.3548(8) 0.3897(7) 0.018(2) Uani 1 1 d . . . . . H31A H 0.4106 0.3212 0.4253 0.021 Uiso 1 1 calc R . . . . H31B H 0.3054 0.3033 0.3578 0.021 Uiso 1 1 calc R . . . . C40 C -0.2576(16) 0.7069(11) 0.4157(10) 0.040(4) Uani 1 1 d . . . . . H40A H -0.3135 0.6726 0.3813 0.059 Uiso 1 1 calc GR . . . . H40B H -0.2842 0.7789 0.4072 0.059 Uiso 1 1 calc GR . . . . H40C H -0.2856 0.6916 0.4656 0.059 Uiso 1 1 calc GR . . . . C37 C -0.0323(13) 0.5593(10) 0.4280(8) 0.028(3) Uani 1 1 d . . . . . H37 H -0.1081 0.5226 0.4060 0.034 Uiso 1 1 calc R . . . . C22 C 1.3232(12) 0.0976(9) -0.0846(7) 0.019(3) Uani 1 1 d . . . . . H22A H 1.3478 0.0364 -0.1140 0.023 Uiso 1 1 calc R . . . . H22B H 1.2982 0.1554 -0.1182 0.023 Uiso 1 1 calc R . . . . N8 N 0.1306(10) 0.5115(7) 0.3976(6) 0.017(2) Uani 1 1 d . . . . . C20 C 1.3610(13) 0.4689(10) 1.0834(8) 0.024(3) Uani 1 1 d . . . . . H20A H 1.4179 0.4681 1.0376 0.036 Uiso 1 1 calc GR . . . . H20B H 1.3867 0.4034 1.1072 0.036 Uiso 1 1 calc GR . . . . H20C H 1.3888 0.5196 1.1154 0.036 Uiso 1 1 calc GR . . . . N2 N -0.3513(10) 1.0240(7) 0.5750(6) 0.018(2) Uani 1 1 d . . . . . C14 C 0.8495(13) 0.5867(11) 1.0390(7) 0.028(3) Uani 1 1 d . . . . . H14A H 0.8330 0.6317 1.0813 0.034 Uiso 1 1 calc R . . . . H14B H 0.8769 0.5174 1.0575 0.034 Uiso 1 1 calc R . . . . C17 C 1.1354(11) 0.5999(9) 1.0356(6) 0.015(2) Uani 1 1 d . . . . . H17 H 1.2159 0.6121 1.0002 0.018 Uiso 1 1 calc R . . . . C25 C 1.3319(12) 0.0531(9) 0.0757(7) 0.019(3) Uani 1 1 d . . . . . H25A H 1.2937 -0.0090 0.0866 0.023 Uiso 1 1 calc R . . . . H25B H 1.3621 0.0799 0.1222 0.023 Uiso 1 1 calc R . . . . C15 C 0.8492(12) 0.5526(8) 0.8830(7) 0.017(2) Uani 1 1 d . . . . . H15A H 0.8670 0.5710 0.8318 0.020 Uiso 1 1 calc R . . . . H15B H 0.8148 0.4878 0.8829 0.020 Uiso 1 1 calc R . . . . C1 C -0.1572(12) 0.8621(9) 0.5708(7) 0.017(2) Uani 1 1 d . . . . . H1A H -0.1629 0.8010 0.5992 0.021 Uiso 1 1 calc R . . . . H1B H -0.0982 0.8421 0.5258 0.021 Uiso 1 1 calc R . . . . C12 C 0.9317(14) 0.7164(10) 0.9655(10) 0.037(4) Uani 1 1 d . . . . . H12A H 1.0152 0.7361 0.9362 0.044 Uiso 1 1 calc R . . . . H12B H 0.9118 0.7616 1.0076 0.044 Uiso 1 1 calc R . . . . C13 C 0.6970(12) 0.5991(8) 0.9930(6) 0.014(2) Uani 1 1 d . . . . . H13A H 0.6601 0.5351 0.9924 0.017 Uiso 1 1 calc R . . . . H13B H 0.6167 0.6495 1.0159 0.017 Uiso 1 1 calc R . . . . C5 C -0.0668(15) 1.0206(10) 0.5703(7) 0.025(3) Uani 1 1 d . . . . . H5A H 0.0000 1.0019 0.5275 0.030 Uiso 1 1 calc R . . . . H5B H -0.0195 1.0667 0.6001 0.030 Uiso 1 1 calc R . . . . C39 C -0.0804(13) 0.6711(10) 0.4048(9) 0.031(3) Uani 1 1 d . . . . . H39A H -0.0536 0.6793 0.3530 0.038 Uiso 1 1 calc R . . . . H39B H -0.0237 0.7124 0.4344 0.038 Uiso 1 1 calc R . . . . N6 N 1.4638(10) 0.1081(7) -0.0366(5) 0.015(2) Uani 1 1 d . . . . . C26 C 1.4732(13) 0.0298(9) 0.0251(7) 0.020(3) Uani 1 1 d . . . . . H26A H 1.5677 0.0290 0.0538 0.024 Uiso 1 1 calc R . . . . H26B H 1.4789 -0.0370 0.0038 0.024 Uiso 1 1 calc R . . . . C33 C 0.1876(13) 0.4089(8) 0.4315(8) 0.022(3) Uani 1 1 d . . . . . H33A H 0.1058 0.3687 0.4289 0.026 Uiso 1 1 calc R . . . . H33B H 0.2130 0.4160 0.4834 0.026 Uiso 1 1 calc R . . . . C35 C 0.2885(12) 0.4655(9) 0.2840(6) 0.017(2) Uani 1 1 d . . . . . H35A H 0.2898 0.4130 0.2472 0.020 Uiso 1 1 calc R . . . . H35B H 0.3197 0.5236 0.2598 0.020 Uiso 1 1 calc R . . . . C32 C 0.4143(12) 0.5167(10) 0.3912(7) 0.023(3) Uani 1 1 d . . . . . H32A H 0.4706 0.5611 0.3637 0.028 Uiso 1 1 calc R . . . . H32B H 0.4735 0.4943 0.4358 0.028 Uiso 1 1 calc R . . . . C24 C 1.4252(13) 0.2109(9) 0.0007(8) 0.022(3) Uani 1 1 d . . . . . H24A H 1.5016 0.2153 0.0391 0.027 Uiso 1 1 calc R . . . . H24B H 1.4291 0.2645 -0.0356 0.027 Uiso 1 1 calc R . . . . C21 C 1.1828(13) 0.0922(9) -0.0342(7) 0.020(3) Uani 1 1 d . . . . . H21A H 1.0894 0.1331 -0.0558 0.024 Uiso 1 1 calc R . . . . H21B H 1.1670 0.0225 -0.0313 0.024 Uiso 1 1 calc R . . . . C27 C 1.6171(13) 0.0993(9) -0.0797(7) 0.021(3) Uani 1 1 d . . . . . H27 H 1.6934 0.1232 -0.0476 0.026 Uiso 1 1 calc R . . . . C36 C 0.1225(13) 0.4967(10) 0.3149(7) 0.025(3) Uani 1 1 d . . . . . H36A H 0.0709 0.5593 0.2911 0.030 Uiso 1 1 calc R . . . . H36B H 0.0622 0.4444 0.3045 0.030 Uiso 1 1 calc R . . . . C23 C 1.2631(13) 0.2241(9) 0.0343(7) 0.018(3) Uani 1 1 d . . . . . H23A H 1.2652 0.2531 0.0834 0.022 Uiso 1 1 calc R . . . . H23B H 1.1911 0.2717 0.0040 0.022 Uiso 1 1 calc R . . . . C30 C 1.6855(14) -0.0114(9) -0.1015(8) 0.028(3) Uani 1 1 d . . . . . H30A H 1.6991 -0.0536 -0.0577 0.041 Uiso 1 1 calc GR . . . . H30B H 1.7849 -0.0139 -0.1254 0.041 Uiso 1 1 calc GR . . . . H30C H 1.6149 -0.0355 -0.1349 0.041 Uiso 1 1 calc GR . . . . C3 C -0.1758(14) 0.9596(9) 0.6802(8) 0.024(3) Uani 1 1 d . U . . . H3A H -0.1226 0.9991 0.7129 0.029 Uiso 1 1 calc R . . . . H3B H -0.1924 0.8995 0.7073 0.029 Uiso 1 1 calc R . . . . C11 C 0.7822(12) 0.7273(8) 0.9176(8) 0.020(3) Uani 1 1 d . . . . . H11A H 0.7018 0.7801 0.9380 0.024 Uiso 1 1 calc R . . . . H11B H 0.8049 0.7474 0.8675 0.024 Uiso 1 1 calc R . . . . C6 C -0.2262(12) 1.0745(10) 0.5441(8) 0.024(3) Uani 1 1 d . . . . . H6A H -0.2437 1.1448 0.5599 0.028 Uiso 1 1 calc R . . . . H6B H -0.2300 1.0739 0.4903 0.028 Uiso 1 1 calc R . . . . C7 C -0.5183(15) 1.0770(10) 0.5521(9) 0.031(3) Uani 1 1 d . . . . . H7 H -0.5929 1.0372 0.5723 0.038 Uiso 1 1 calc R . . . . C10 C -0.5587(17) 1.1841(11) 0.5835(9) 0.040(4) Uani 1 1 d . . . . . H10A H -0.5533 1.1807 0.6367 0.060 Uiso 1 1 calc GR . . . . H10B H -0.6627 1.2152 0.5684 0.060 Uiso 1 1 calc GR . . . . H10C H -0.4854 1.2239 0.5651 0.060 Uiso 1 1 calc GR . . . . C16 C 1.0027(15) 0.5419(13) 0.9264(9) 0.041(4) Uani 1 1 d . . . . . H16A H 1.0351 0.4721 0.9432 0.050 Uiso 1 1 calc R . . . . H16B H 1.0841 0.5589 0.8944 0.050 Uiso 1 1 calc R . . . . C19 C 1.1894(14) 0.4931(10) 1.0678(8) 0.030(3) Uani 1 1 d . . . . . H19A H 1.1328 0.4867 1.1136 0.036 Uiso 1 1 calc R . . . . H19B H 1.1634 0.4439 1.0331 0.036 Uiso 1 1 calc R . . . . C28 C 1.5966(16) 0.1658(11) -0.1492(8) 0.033(3) Uani 1 1 d . . . . . H28A H 1.5490 0.1313 -0.1877 0.040 Uiso 1 1 calc R . . . . H28B H 1.5252 0.2286 -0.1383 0.040 Uiso 1 1 calc R . . . . C18 C 1.1285(16) 0.6787(11) 1.0964(8) 0.036(4) Uani 1 1 d . . . . . H18A H 1.0952 0.7454 1.0755 0.054 Uiso 1 1 calc GR . . . . H18B H 1.2304 0.6739 1.1181 0.054 Uiso 1 1 calc GR . . . . H18C H 1.0555 0.6665 1.1340 0.054 Uiso 1 1 calc GR . . . . C29 C 1.7478(18) 0.1906(13) -0.1785(11) 0.051(5) Uani 1 1 d . . . . . H29A H 1.7267 0.2335 -0.2217 0.076 Uiso 1 1 calc GR . . . . H29B H 1.8177 0.1290 -0.1914 0.076 Uiso 1 1 calc GR . . . . H29C H 1.7954 0.2253 -0.1410 0.076 Uiso 1 1 calc GR . . . . C9 C -0.7092(15) 1.1076(11) 0.4472(9) 0.036(3) Uani 1 1 d . U . . . H9A H -0.7193 1.1165 0.3944 0.054 Uiso 1 1 calc GR . . . . H9B H -0.7574 1.1692 0.4713 0.054 Uiso 1 1 calc GR . . . . H9C H -0.7598 1.0531 0.4629 0.054 Uiso 1 1 calc GR . . . . C4 C -0.3309(18) 1.0214(13) 0.6580(10) 0.045(4) Uani 1 1 d . U . . . H4A H -0.3387 1.0902 0.6759 0.054 Uiso 1 1 calc R . . . . H4B H -0.4141 0.9926 0.6808 0.054 Uiso 1 1 calc R . . . . C2 C -0.3182(15) 0.9147(10) 0.5507(11) 0.043(4) Uani 1 1 d . . . . . H2A H -0.3936 0.8791 0.5738 0.052 Uiso 1 1 calc R . . . . H2B H -0.3313 0.9123 0.4973 0.052 Uiso 1 1 calc R . . . . C8 C -0.5363(15) 1.0822(11) 0.4679(9) 0.036(3) Uani 1 1 d . U . . . H8A H -0.4890 1.0174 0.4467 0.043 Uiso 1 1 calc R . . . . H8B H -0.4828 1.1339 0.4478 0.043 Uiso 1 1 calc R . . . . C38 C -0.0420(16) 0.5465(11) 0.5122(8) 0.035(4) Uani 1 1 d . . . . . H38A H -0.0228 0.4754 0.5249 0.053 Uiso 1 1 calc GR . . . . H38B H -0.1444 0.5776 0.5291 0.053 Uiso 1 1 calc GR . . . . H38C H 0.0352 0.5783 0.5357 0.053 Uiso 1 1 calc GR . . . . C42 C 0.6377(19) -0.1983(12) 0.1575(10) 0.039(4) Uani 1 1 d . . . . . N11 N 0.5673(18) -0.1865(11) 0.1051(10) 0.057(4) Uani 1 1 d . . . . . N10 N 1.0714(17) 0.3245(12) 0.8540(10) 0.056(4) Uani 1 1 d . . . . . C48 C 1.1286(19) 0.3140(12) 0.8020(12) 0.049(5) Uani 1 1 d . . . . . C41 C 0.728(2) -0.2153(14) 0.2238(11) 0.056(5) Uani 1 1 d . . . . . H41A H 0.8272 -0.2578 0.2133 0.084 Uiso 1 1 calc GR . . . . H41B H 0.6729 -0.2482 0.2601 0.084 Uiso 1 1 calc GR . . . . H41C H 0.7445 -0.1514 0.2427 0.084 Uiso 1 1 calc GR . . . . C47 C 1.225(3) 0.2955(18) 0.7341(12) 0.076(7) Uani 1 1 d . . . . . H47A H 1.2109 0.3564 0.7044 0.115 Uiso 1 1 calc GR . . . . H47B H 1.1937 0.2420 0.7062 0.115 Uiso 1 1 calc GR . . . . H47C H 1.3334 0.2760 0.7477 0.115 Uiso 1 1 calc GR . . . . C43 C 0.293(2) -0.0829(14) 0.2704(12) 0.064(6) Uani 1 1 d . . . . . H43A H 0.2344 -0.0437 0.2313 0.096 Uiso 1 1 calc GR . . . . H43B H 0.4025 -0.0828 0.2637 0.096 Uiso 1 1 calc GR . . . . H43C H 0.2595 -0.0536 0.3175 0.096 Uiso 1 1 calc GR . . . . C45 C 0.828(3) 0.442(2) 0.6893(14) 0.101(7) Uani 1 1 d . U . . . H45A H 0.7839 0.4875 0.6502 0.151 Uiso 1 1 calc GR . . . . H45B H 0.9234 0.4602 0.7063 0.151 Uiso 1 1 calc GR . . . . H45C H 0.7548 0.4462 0.7297 0.151 Uiso 1 1 calc GR . . . . C44 C 0.267(3) -0.1818(15) 0.2684(11) 0.069(6) Uani 1 1 d . . . . . C46 C 0.860(4) 0.341(3) 0.662(2) 0.126(7) Uani 1 1 d . U . . . N12 N 0.241(3) -0.2618(14) 0.2713(11) 0.120(9) Uani 1 1 d . . . . . N9 N 0.866(3) 0.257(2) 0.6419(16) 0.130(7) Uani 1 1 d . U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 I13 0.0179(4) 0.0170(4) 0.0165(4) -0.0001(3) -0.0002(3) -0.0055(3) I12 0.0162(3) 0.0177(4) 0.0155(4) 0.0003(3) -0.0021(3) -0.0056(3) I003 0.0140(3) 0.0193(4) 0.0192(4) -0.0046(3) -0.0004(3) -0.0055(3) I11 0.0126(3) 0.0193(4) 0.0180(4) -0.0040(3) -0.0017(3) -0.0029(3) I9 0.0148(3) 0.0163(4) 0.0189(4) -0.0015(3) -0.0016(3) -0.0025(3) I3 0.0151(3) 0.0160(4) 0.0196(4) -0.0007(3) 0.0000(3) -0.0032(3) I4 0.0195(4) 0.0153(4) 0.0183(4) 0.0018(3) -0.0027(3) -0.0050(3) I1 0.0196(4) 0.0180(4) 0.0134(4) -0.0013(3) -0.0018(3) -0.0061(3) I8 0.0181(4) 0.0151(4) 0.0237(5) -0.0043(3) 0.0003(3) -0.0042(3) I5 0.0171(4) 0.0222(4) 0.0214(4) 0.0054(3) -0.0043(3) -0.0084(3) I6 0.0166(4) 0.0217(4) 0.0169(4) 0.0033(3) -0.0020(3) -0.0059(3) I2 0.0287(4) 0.0187(4) 0.0162(4) -0.0007(3) -0.0061(3) -0.0094(3) I10 0.0389(5) 0.0198(4) 0.0203(5) 0.0013(3) 0.0000(4) -0.0056(3) I7 0.0575(6) 0.0206(5) 0.0172(5) -0.0024(4) -0.0062(4) -0.0080(4) Cu5 0.0159(7) 0.0174(7) 0.0207(8) 0.0011(6) -0.0039(6) -0.0031(5) Cu10 0.0138(6) 0.0213(8) 0.0159(8) -0.0010(6) -0.0001(5) -0.0030(5) Cu7 0.0178(7) 0.0220(8) 0.0212(9) -0.0057(6) 0.0004(6) -0.0041(6) Cu1 0.0173(7) 0.0208(8) 0.0162(8) -0.0003(6) -0.0035(6) -0.0044(5) Cu4 0.0200(7) 0.0257(8) 0.0208(9) 0.0036(6) -0.0033(6) -0.0065(6) Cu6 0.0146(7) 0.0173(8) 0.0231(9) -0.0035(6) 0.0001(6) -0.0030(5) Cu8 0.0296(8) 0.0237(8) 0.0207(9) -0.0038(7) 0.0011(7) -0.0018(6) Cu9 0.0312(8) 0.0238(9) 0.0238(9) -0.0048(7) 0.0030(7) -0.0053(6) Cu2 0.0334(8) 0.0234(9) 0.0217(9) 0.0029(7) -0.0070(7) -0.0055(6) Cu3 0.0364(9) 0.0247(9) 0.0179(9) 0.0007(7) -0.0060(7) -0.0036(6) N1 0.020(5) 0.018(5) 0.020(6) -0.007(4) 0.000(4) 0.000(4) N3 0.005(4) 0.017(5) 0.027(6) -0.004(4) -0.001(4) 0.000(3) N5 0.017(5) 0.019(5) 0.017(6) -0.003(4) -0.004(4) -0.008(4) N7 0.015(5) 0.014(5) 0.015(5) -0.002(4) -0.004(4) -0.003(3) N4 0.015(4) 0.015(5) 0.014(5) 0.002(4) 0.001(4) -0.006(3) C34 0.023(6) 0.020(6) 0.008(6) -0.006(5) 0.002(5) -0.008(4) C31 0.014(5) 0.014(6) 0.026(7) 0.000(5) -0.002(5) -0.004(4) C40 0.033(8) 0.026(8) 0.059(12) -0.015(7) 0.005(7) -0.002(6) C37 0.016(6) 0.030(8) 0.039(9) -0.015(6) 0.000(6) -0.006(5) C22 0.017(6) 0.017(6) 0.024(7) -0.001(5) -0.001(5) -0.002(4) N8 0.018(5) 0.008(5) 0.028(6) -0.004(4) 0.000(4) -0.007(4) C20 0.017(6) 0.030(7) 0.022(7) -0.003(6) -0.003(5) 0.002(5) N2 0.018(5) 0.020(5) 0.015(5) 0.004(4) -0.005(4) 0.001(4) C14 0.022(6) 0.049(9) 0.017(7) 0.004(6) 0.009(5) -0.015(6) C17 0.005(5) 0.029(7) 0.012(6) -0.002(5) -0.001(4) -0.002(4) C25 0.017(5) 0.016(6) 0.025(7) 0.001(5) -0.007(5) -0.007(4) C15 0.020(6) 0.014(6) 0.017(6) -0.002(5) 0.006(5) -0.003(4) C1 0.013(5) 0.022(6) 0.017(6) -0.002(5) -0.004(4) -0.004(4) C12 0.020(6) 0.027(8) 0.066(12) 0.022(7) -0.029(6) -0.009(5) C13 0.015(5) 0.017(6) 0.008(6) 0.004(4) 0.002(4) 0.001(4) C5 0.035(7) 0.026(7) 0.014(7) 0.003(5) 0.004(5) -0.008(5) C39 0.021(6) 0.025(8) 0.050(10) -0.017(7) 0.006(6) -0.008(5) N6 0.018(4) 0.012(5) 0.014(5) -0.002(4) -0.001(4) -0.001(3) C26 0.021(6) 0.012(6) 0.028(8) 0.003(5) -0.003(5) -0.003(4) C33 0.019(6) 0.009(6) 0.039(8) 0.000(5) -0.003(5) -0.007(4) C35 0.021(6) 0.019(6) 0.011(6) 0.002(5) -0.008(4) -0.006(4) C32 0.007(5) 0.038(8) 0.026(8) -0.011(6) 0.003(5) -0.008(5) C24 0.024(6) 0.015(6) 0.031(8) -0.011(5) 0.006(5) -0.012(5) C21 0.023(6) 0.021(6) 0.016(7) -0.001(5) -0.005(5) -0.007(5) C27 0.016(6) 0.029(7) 0.020(7) -0.009(5) 0.002(5) -0.006(5) C36 0.023(6) 0.030(7) 0.021(7) -0.013(6) -0.009(5) -0.003(5) C23 0.020(6) 0.018(6) 0.018(7) -0.014(5) 0.006(5) -0.006(4) C30 0.022(6) 0.022(7) 0.039(9) -0.013(6) 0.012(6) -0.002(5) C3 0.028(5) 0.021(7) 0.026(7) -0.007(5) 0.010(5) -0.009(4) C11 0.015(5) 0.013(6) 0.031(8) 0.003(5) -0.009(5) 0.001(4) C6 0.012(5) 0.033(7) 0.027(8) 0.014(6) -0.006(5) -0.008(5) C7 0.022(6) 0.027(7) 0.042(10) 0.010(6) -0.002(6) 0.002(5) C10 0.037(8) 0.038(9) 0.040(10) 0.019(7) 0.005(7) 0.007(6) C16 0.028(7) 0.057(10) 0.033(9) -0.027(8) -0.005(6) 0.011(6) C19 0.027(7) 0.031(8) 0.031(8) 0.006(6) -0.010(6) -0.006(5) C28 0.041(8) 0.032(8) 0.029(9) -0.004(6) 0.013(7) -0.010(6) C18 0.031(7) 0.041(9) 0.030(9) -0.014(7) -0.014(6) 0.008(6) C29 0.054(10) 0.053(11) 0.051(12) -0.017(9) 0.010(9) -0.021(8) C9 0.036(4) 0.036(4) 0.036(4) 0.002(2) -0.002(2) -0.006(2) C4 0.045(4) 0.046(4) 0.045(4) 0.0000(12) 0.0001(12) -0.0071(13) C2 0.027(7) 0.021(8) 0.084(14) 0.011(8) -0.023(7) -0.009(5) C8 0.032(5) 0.039(9) 0.035(9) 0.011(7) 0.002(6) 0.002(6) C38 0.030(7) 0.044(9) 0.031(9) -0.011(7) 0.021(6) -0.001(6) C42 0.053(9) 0.034(9) 0.032(9) -0.005(7) 0.002(8) -0.015(7) N11 0.072(10) 0.044(9) 0.055(11) -0.010(8) -0.014(8) -0.010(7) N10 0.044(8) 0.069(11) 0.054(11) -0.011(9) 0.004(8) -0.004(7) C48 0.041(9) 0.033(9) 0.075(15) -0.011(9) 0.003(9) -0.012(7) C41 0.077(13) 0.047(11) 0.048(12) 0.008(9) -0.019(9) -0.025(9) C47 0.084(15) 0.085(17) 0.058(15) -0.025(13) 0.004(12) -0.010(12) C43 0.069(12) 0.047(12) 0.071(16) 0.013(10) 0.016(11) 0.001(9) C45 0.097(17) 0.150(12) 0.052(15) -0.020(15) -0.020(13) -0.016(13) C44 0.124(18) 0.039(12) 0.031(11) 0.014(9) 0.000(11) 0.019(11) C46 0.126(7) 0.126(7) 0.126(7) -0.0013(12) -0.0001(12) -0.0232(17) N12 0.26(3) 0.040(12) 0.044(13) 0.013(9) 0.002(15) 0.002(14) N9 0.132(7) 0.128(7) 0.130(7) -0.003(2) -0.002(2) -0.024(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I13 Cu10 2.6005(16) . ? I13 Cu7 2.6732(16) . ? I12 Cu10 2.6306(17) . ? I12 Cu9 2.5247(17) . ? I003 Cu10 2.6725(16) . ? I003 Cu7 2.7218(15) . ? I003 Cu8 2.6149(17) . ? I11 Cu7 2.7062(17) . ? I11 Cu6 2.6830(17) . ? I11 Cu9 2.6350(17) . ? I9 Cu7 2.6328(18) . ? I9 Cu6 2.6081(17) . ? I3 Cu5 2.6061(15) . ? I3 Cu4 2.6268(18) . ? I4 Cu5 2.6054(15) . ? I4 Cu3 2.5313(19) . ? I1 Cu1 2.6200(16) . ? I1 Cu2 2.5327(19) . ? I8 Cu6 2.6034(15) . ? I8 Cu8 2.5309(17) . ? I5 Cu1 2.6763(17) . ? I5 Cu4 2.7101(16) . ? I5 Cu3 2.6224(18) . ? I6 Cu5 2.7022(17) . ? I6 Cu4 2.6992(16) . ? I6 Cu2 2.6431(18) . ? I2 Cu1 2.6209(16) . ? I2 Cu4 2.6716(18) . ? I10 Cu8 2.636(2) . ? I10 Cu9 2.6222(18) . ? I7 Cu2 2.6154(18) . ? I7 Cu3 2.6326(18) . ? Cu5 Cu4 2.751(2) . ? Cu5 Cu3 2.713(2) . ? Cu5 N3 2.126(9) . ? Cu10 Cu7 2.698(2) . ? Cu10 Cu9 2.757(2) . ? Cu10 N7 2.125(9) . ? Cu7 Cu6 2.7745(19) . ? Cu7 Cu8 2.977(2) . ? Cu7 Cu9 2.985(2) . ? Cu1 Cu4 2.692(2) . ? Cu1 Cu2 2.726(2) . ? Cu1 N1 2.134(10) . ? Cu4 Cu2 3.003(2) . ? Cu4 Cu3 2.937(2) . ? Cu6 Cu8 2.711(2) . ? Cu6 N5 2.129(9) . ? Cu8 Cu9 2.535(2) . ? Cu2 Cu3 2.553(2) . ? N1 C1 1.471(14) . ? N1 C5 1.480(16) . ? N1 C3 1.480(15) . ? N3 C15 1.489(13) . ? N3 C13 1.482(15) . ? N3 C11 1.468(14) . ? N5 C25 1.486(15) . ? N5 C21 1.457(15) . ? N5 C23 1.468(13) . ? N7 C31 1.460(14) . ? N7 C35 1.505(15) . ? N7 C32 1.494(14) . ? N4 C14 1.502(13) . ? N4 C17 1.534(14) . ? N4 C12 1.470(16) . ? N4 C16 1.505(16) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C34 N8 1.518(13) . ? C34 C32 1.547(14) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 C33 1.540(15) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C40 C39 1.538(17) . ? C37 H37 0.9800 . ? C37 N8 1.543(14) . ? C37 C39 1.532(19) . ? C37 C38 1.53(2) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C22 N6 1.527(14) . ? C22 C21 1.531(15) . ? N8 C33 1.496(15) . ? N8 C36 1.508(16) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C20 C19 1.492(16) . ? N2 C6 1.488(14) . ? N2 C7 1.546(16) . ? N2 C4 1.50(2) . ? N2 C2 1.508(17) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 C13 1.546(17) . ? C17 H17 0.9800 . ? C17 C19 1.528(18) . ? C17 C18 1.521(16) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C25 C26 1.514(16) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 C16 1.530(18) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 C2 1.487(16) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 C11 1.544(16) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 C6 1.511(17) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? N6 C26 1.511(16) . ? N6 C24 1.519(14) . ? N6 C27 1.527(14) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C35 C36 1.530(15) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C24 C23 1.513(14) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C27 H27 0.9800 . ? C27 C30 1.546(16) . ? C27 C28 1.52(2) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 C4 1.50(2) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 H7 0.9800 . ? C7 C10 1.53(2) . ? C7 C8 1.52(2) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C28 C29 1.508(18) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C9 C8 1.523(19) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C42 N11 1.12(2) . ? C42 C41 1.42(2) . ? N10 C48 1.06(2) . ? C48 C47 1.48(3) . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C43 C44 1.39(3) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C45 C46 1.42(4) . ? C44 N12 1.14(3) . ? C46 N9 1.18(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu10 I13 Cu7 61.52(5) . . ? Cu9 I12 Cu10 64.61(5) . . ? Cu10 I003 Cu7 60.01(4) . . ? Cu8 I003 Cu10 103.79(5) . . ? Cu8 I003 Cu7 67.77(5) . . ? Cu6 I11 Cu7 61.97(5) . . ? Cu9 I11 Cu7 67.93(5) . . ? Cu9 I11 Cu6 102.99(5) . . ? Cu6 I9 Cu7 63.93(5) . . ? Cu5 I3 Cu4 63.42(5) . . ? Cu3 I4 Cu5 63.73(5) . . ? Cu2 I1 Cu1 63.87(5) . . ? Cu8 I8 Cu6 63.71(5) . . ? Cu1 I5 Cu4 59.97(5) . . ? Cu3 I5 Cu1 102.52(5) . . ? Cu3 I5 Cu4 66.82(5) . . ? Cu4 I6 Cu5 61.23(5) . . ? Cu2 I6 Cu5 104.21(5) . . ? Cu2 I6 Cu4 68.40(5) . . ? Cu1 I2 Cu4 61.14(5) . . ? Cu9 I10 Cu8 57.64(5) . . ? Cu2 I7 Cu3 58.21(5) . . ? I3 Cu5 I6 109.22(6) . . ? I3 Cu5 Cu4 58.66(5) . . ? I3 Cu5 Cu3 109.08(6) . . ? I4 Cu5 I3 118.75(5) . . ? I4 Cu5 I6 116.61(6) . . ? I4 Cu5 Cu4 116.13(6) . . ? I4 Cu5 Cu3 56.80(5) . . ? I6 Cu5 Cu4 59.33(5) . . ? I6 Cu5 Cu3 70.37(5) . . ? Cu3 Cu5 Cu4 65.04(6) . . ? N3 Cu5 I3 103.8(3) . . ? N3 Cu5 I4 103.6(3) . . ? N3 Cu5 I6 102.5(3) . . ? N3 Cu5 Cu4 140.3(3) . . ? N3 Cu5 Cu3 146.9(3) . . ? I13 Cu10 I12 115.49(5) . . ? I13 Cu10 I003 112.23(6) . . ? I13 Cu10 Cu7 60.57(5) . . ? I13 Cu10 Cu9 111.88(6) . . ? I12 Cu10 I003 117.63(6) . . ? I12 Cu10 Cu7 114.57(6) . . ? I12 Cu10 Cu9 55.83(5) . . ? I003 Cu10 Cu7 60.90(4) . . ? I003 Cu10 Cu9 70.65(5) . . ? Cu7 Cu10 Cu9 66.34(6) . . ? N7 Cu10 I13 105.5(3) . . ? N7 Cu10 I12 101.4(3) . . ? N7 Cu10 I003 102.1(2) . . ? N7 Cu10 Cu7 144.0(3) . . ? N7 Cu10 Cu9 141.8(3) . . ? I13 Cu7 I003 108.47(5) . . ? I13 Cu7 I11 109.31(5) . . ? I13 Cu7 Cu10 57.92(4) . . ? I13 Cu7 Cu6 148.60(6) . . ? I13 Cu7 Cu8 151.17(7) . . ? I13 Cu7 Cu9 103.23(6) . . ? I003 Cu7 Cu6 102.69(6) . . ? I003 Cu7 Cu8 54.41(4) . . ? I003 Cu7 Cu9 66.58(5) . . ? I11 Cu7 I003 115.30(6) . . ? I11 Cu7 Cu6 58.60(4) . . ? I11 Cu7 Cu8 67.50(5) . . ? I11 Cu7 Cu9 54.90(4) . . ? I9 Cu7 I13 107.37(6) . . ? I9 Cu7 I003 108.41(5) . . ? I9 Cu7 I11 107.70(5) . . ? I9 Cu7 Cu10 148.33(7) . . ? I9 Cu7 Cu6 57.60(5) . . ? I9 Cu7 Cu8 100.57(6) . . ? I9 Cu7 Cu9 148.76(6) . . ? Cu10 Cu7 I003 59.09(4) . . ? Cu10 Cu7 I11 103.82(6) . . ? Cu10 Cu7 Cu6 148.76(8) . . ? Cu10 Cu7 Cu8 94.20(6) . . ? Cu10 Cu7 Cu9 57.78(5) . . ? Cu6 Cu7 Cu8 56.11(5) . . ? Cu6 Cu7 Cu9 92.47(6) . . ? Cu8 Cu7 Cu9 50.33(5) . . ? I1 Cu1 I5 118.04(6) . . ? I1 Cu1 I2 116.95(5) . . ? I1 Cu1 Cu4 117.20(6) . . ? I1 Cu1 Cu2 56.51(5) . . ? I5 Cu1 Cu4 60.64(5) . . ? I5 Cu1 Cu2 71.67(5) . . ? I2 Cu1 I5 111.93(6) . . ? I2 Cu1 Cu4 60.36(5) . . ? I2 Cu1 Cu2 111.83(6) . . ? Cu4 Cu1 Cu2 67.31(6) . . ? N1 Cu1 I1 103.5(3) . . ? N1 Cu1 I5 101.4(3) . . ? N1 Cu1 I2 101.6(3) . . ? N1 Cu1 Cu4 139.3(3) . . ? N1 Cu1 Cu2 146.1(3) . . ? I3 Cu4 I5 108.94(6) . . ? I3 Cu4 I6 108.69(6) . . ? I3 Cu4 I2 105.75(6) . . ? I3 Cu4 Cu5 57.92(5) . . ? I3 Cu4 Cu1 147.86(7) . . ? I3 Cu4 Cu2 150.98(7) . . ? I3 Cu4 Cu3 102.14(6) . . ? I5 Cu4 Cu5 103.53(6) . . ? I5 Cu4 Cu2 67.02(5) . . ? I5 Cu4 Cu3 55.16(5) . . ? I6 Cu4 I5 115.55(6) . . ? I6 Cu4 Cu5 59.44(5) . . ? I6 Cu4 Cu2 54.92(4) . . ? I6 Cu4 Cu3 67.07(5) . . ? I2 Cu4 I5 109.31(6) . . ? I2 Cu4 I6 108.16(6) . . ? I2 Cu4 Cu5 146.85(7) . . ? I2 Cu4 Cu1 58.50(5) . . ? I2 Cu4 Cu2 102.46(6) . . ? I2 Cu4 Cu3 151.58(8) . . ? Cu5 Cu4 Cu2 94.20(6) . . ? Cu5 Cu4 Cu3 56.85(5) . . ? Cu1 Cu4 I5 59.39(5) . . ? Cu1 Cu4 I6 103.10(6) . . ? Cu1 Cu4 Cu5 149.72(8) . . ? Cu1 Cu4 Cu2 56.89(5) . . ? Cu1 Cu4 Cu3 94.39(6) . . ? Cu3 Cu4 Cu2 50.89(5) . . ? I11 Cu6 Cu7 59.43(5) . . ? I11 Cu6 Cu8 71.86(5) . . ? I9 Cu6 I11 109.13(5) . . ? I9 Cu6 Cu7 58.47(5) . . ? I9 Cu6 Cu8 108.63(6) . . ? I8 Cu6 I11 117.88(6) . . ? I8 Cu6 I9 118.17(6) . . ? I8 Cu6 Cu7 116.97(6) . . ? I8 Cu6 Cu8 56.84(5) . . ? Cu8 Cu6 Cu7 65.72(5) . . ? N5 Cu6 I11 103.2(3) . . ? N5 Cu6 I9 104.1(3) . . ? N5 Cu6 I8 101.8(2) . . ? N5 Cu6 Cu7 141.2(3) . . ? N5 Cu6 Cu8 146.6(3) . . ? I003 Cu8 I10 106.26(6) . . ? I003 Cu8 Cu7 57.82(4) . . ? I003 Cu8 Cu6 107.40(7) . . ? I8 Cu8 I003 125.21(7) . . ? I8 Cu8 I10 116.72(7) . . ? I8 Cu8 Cu7 112.49(7) . . ? I8 Cu8 Cu6 59.44(5) . . ? I8 Cu8 Cu9 156.01(8) . . ? I10 Cu8 Cu7 125.91(7) . . ? I10 Cu8 Cu6 137.92(7) . . ? Cu6 Cu8 Cu7 58.18(5) . . ? Cu9 Cu8 I003 75.12(6) . . ? Cu9 Cu8 I10 60.91(6) . . ? Cu9 Cu8 Cu7 65.00(6) . . ? Cu9 Cu8 Cu6 104.96(7) . . ? I12 Cu9 I11 118.96(6) . . ? I12 Cu9 I10 121.45(7) . . ? I12 Cu9 Cu10 59.55(5) . . ? I12 Cu9 Cu7 108.64(6) . . ? I12 Cu9 Cu8 158.95(8) . . ? I11 Cu9 Cu10 104.13(7) . . ? I11 Cu9 Cu7 57.17(5) . . ? I10 Cu9 I11 107.86(6) . . ? I10 Cu9 Cu10 138.79(7) . . ? I10 Cu9 Cu7 126.12(7) . . ? Cu10 Cu9 Cu7 55.88(5) . . ? Cu8 Cu9 I11 75.47(6) . . ? Cu8 Cu9 I10 61.45(6) . . ? Cu8 Cu9 Cu10 103.61(8) . . ? Cu8 Cu9 Cu7 64.67(6) . . ? I1 Cu2 I6 121.39(6) . . ? I1 Cu2 I7 121.57(7) . . ? I1 Cu2 Cu1 59.62(5) . . ? I1 Cu2 Cu4 109.69(6) . . ? I1 Cu2 Cu3 157.90(8) . . ? I6 Cu2 Cu1 103.67(6) . . ? I6 Cu2 Cu4 56.69(4) . . ? I7 Cu2 I6 106.53(7) . . ? I7 Cu2 Cu1 139.24(7) . . ? I7 Cu2 Cu4 124.45(7) . . ? Cu1 Cu2 Cu4 55.80(5) . . ? Cu3 Cu2 I6 73.79(6) . . ? Cu3 Cu2 I7 61.23(5) . . ? Cu3 Cu2 Cu1 103.01(7) . . ? Cu3 Cu2 Cu4 63.22(6) . . ? I4 Cu3 I5 123.84(7) . . ? I4 Cu3 I7 117.06(7) . . ? I4 Cu3 Cu5 59.46(5) . . ? I4 Cu3 Cu4 112.26(7) . . ? I4 Cu3 Cu2 157.63(8) . . ? I5 Cu3 I7 106.22(7) . . ? I5 Cu3 Cu5 107.01(6) . . ? I5 Cu3 Cu4 58.02(5) . . ? I7 Cu3 Cu5 139.10(7) . . ? I7 Cu3 Cu4 126.45(7) . . ? Cu5 Cu3 Cu4 58.11(5) . . ? Cu2 Cu3 I5 75.35(6) . . ? Cu2 Cu3 I7 60.56(6) . . ? Cu2 Cu3 Cu5 106.43(7) . . ? Cu2 Cu3 Cu4 65.89(6) . . ? C1 N1 Cu1 111.4(7) . . ? C1 N1 C5 108.7(10) . . ? C1 N1 C3 106.4(9) . . ? C5 N1 Cu1 110.8(7) . . ? C5 N1 C3 107.9(9) . . ? C3 N1 Cu1 111.4(8) . . ? C15 N3 Cu5 111.0(7) . . ? C13 N3 Cu5 110.8(6) . . ? C13 N3 C15 107.9(9) . . ? C11 N3 Cu5 110.1(7) . . ? C11 N3 C15 108.1(8) . . ? C11 N3 C13 108.9(9) . . ? C25 N5 Cu6 112.3(7) . . ? C21 N5 Cu6 112.4(6) . . ? C21 N5 C25 107.1(9) . . ? C21 N5 C23 108.6(9) . . ? C23 N5 Cu6 109.5(6) . . ? C23 N5 C25 106.7(8) . . ? C31 N7 Cu10 110.7(7) . . ? C31 N7 C35 107.3(8) . . ? C31 N7 C32 108.7(9) . . ? C35 N7 Cu10 113.6(7) . . ? C32 N7 Cu10 110.7(6) . . ? C32 N7 C35 105.6(9) . . ? C14 N4 C17 112.5(9) . . ? C14 N4 C16 108.5(10) . . ? C12 N4 C14 106.8(10) . . ? C12 N4 C17 110.6(8) . . ? C12 N4 C16 108.6(12) . . ? C16 N4 C17 109.7(9) . . ? H34A C34 H34B 108.4 . . ? N8 C34 H34A 110.1 . . ? N8 C34 H34B 110.1 . . ? N8 C34 C32 108.1(8) . . ? C32 C34 H34A 110.1 . . ? C32 C34 H34B 110.1 . . ? N7 C31 H31A 109.4 . . ? N7 C31 H31B 109.4 . . ? N7 C31 C33 111.4(9) . . ? H31A C31 H31B 108.0 . . ? C33 C31 H31A 109.4 . . ? C33 C31 H31B 109.4 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? N8 C37 H37 107.2 . . ? C39 C37 H37 107.2 . . ? C39 C37 N8 111.9(10) . . ? C38 C37 H37 107.2 . . ? C38 C37 N8 111.9(11) . . ? C38 C37 C39 111.1(11) . . ? H22A C22 H22B 108.3 . . ? N6 C22 H22A 109.9 . . ? N6 C22 H22B 109.9 . . ? N6 C22 C21 109.1(10) . . ? C21 C22 H22A 109.9 . . ? C21 C22 H22B 109.9 . . ? C34 N8 C37 111.8(8) . . ? C33 N8 C34 108.0(9) . . ? C33 N8 C37 111.0(9) . . ? C33 N8 C36 106.8(9) . . ? C36 N8 C34 108.8(9) . . ? C36 N8 C37 110.3(9) . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? C6 N2 C7 113.4(10) . . ? C6 N2 C4 106.4(10) . . ? C6 N2 C2 107.9(10) . . ? C4 N2 C7 111.7(10) . . ? C4 N2 C2 105.9(12) . . ? C2 N2 C7 111.1(9) . . ? N4 C14 H14A 109.5 . . ? N4 C14 H14B 109.5 . . ? N4 C14 C13 110.6(10) . . ? H14A C14 H14B 108.1 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? N4 C17 H17 107.0 . . ? C19 C17 N4 113.0(9) . . ? C19 C17 H17 107.0 . . ? C18 C17 N4 112.3(9) . . ? C18 C17 H17 107.0 . . ? C18 C17 C19 110.3(11) . . ? N5 C25 H25A 109.5 . . ? N5 C25 H25B 109.5 . . ? N5 C25 C26 110.9(10) . . ? H25A C25 H25B 108.1 . . ? C26 C25 H25A 109.5 . . ? C26 C25 H25B 109.5 . . ? N3 C15 H15A 109.3 . . ? N3 C15 H15B 109.3 . . ? N3 C15 C16 111.5(10) . . ? H15A C15 H15B 108.0 . . ? C16 C15 H15A 109.3 . . ? C16 C15 H15B 109.3 . . ? N1 C1 H1A 109.4 . . ? N1 C1 H1B 109.4 . . ? N1 C1 C2 111.1(10) . . ? H1A C1 H1B 108.0 . . ? C2 C1 H1A 109.4 . . ? C2 C1 H1B 109.4 . . ? N4 C12 H12A 109.4 . . ? N4 C12 H12B 109.4 . . ? N4 C12 C11 111.1(10) . . ? H12A C12 H12B 108.0 . . ? C11 C12 H12A 109.4 . . ? C11 C12 H12B 109.4 . . ? N3 C13 C14 110.5(8) . . ? N3 C13 H13A 109.5 . . ? N3 C13 H13B 109.5 . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 108.1 . . ? N1 C5 H5A 109.2 . . ? N1 C5 H5B 109.2 . . ? N1 C5 C6 112.1(9) . . ? H5A C5 H5B 107.9 . . ? C6 C5 H5A 109.2 . . ? C6 C5 H5B 109.2 . . ? C40 C39 H39A 109.6 . . ? C40 C39 H39B 109.6 . . ? C37 C39 C40 110.2(10) . . ? C37 C39 H39A 109.6 . . ? C37 C39 H39B 109.6 . . ? H39A C39 H39B 108.1 . . ? C26 N6 C22 106.9(8) . . ? C26 N6 C24 106.0(9) . . ? C26 N6 C27 112.5(9) . . ? C24 N6 C22 107.2(9) . . ? C24 N6 C27 109.9(8) . . ? C27 N6 C22 114.0(9) . . ? C25 C26 H26A 109.4 . . ? C25 C26 H26B 109.4 . . ? N6 C26 C25 111.0(9) . . ? N6 C26 H26A 109.4 . . ? N6 C26 H26B 109.4 . . ? H26A C26 H26B 108.0 . . ? C31 C33 H33A 109.7 . . ? C31 C33 H33B 109.7 . . ? N8 C33 C31 109.8(10) . . ? N8 C33 H33A 109.7 . . ? N8 C33 H33B 109.7 . . ? H33A C33 H33B 108.2 . . ? N7 C35 H35A 109.4 . . ? N7 C35 H35B 109.4 . . ? N7 C35 C36 111.1(10) . . ? H35A C35 H35B 108.0 . . ? C36 C35 H35A 109.4 . . ? C36 C35 H35B 109.4 . . ? N7 C32 C34 112.3(8) . . ? N7 C32 H32A 109.1 . . ? N7 C32 H32B 109.1 . . ? C34 C32 H32A 109.1 . . ? C34 C32 H32B 109.1 . . ? H32A C32 H32B 107.9 . . ? N6 C24 H24A 109.8 . . ? N6 C24 H24B 109.8 . . ? H24A C24 H24B 108.3 . . ? C23 C24 N6 109.2(8) . . ? C23 C24 H24A 109.8 . . ? C23 C24 H24B 109.8 . . ? N5 C21 C22 112.0(9) . . ? N5 C21 H21A 109.2 . . ? N5 C21 H21B 109.2 . . ? C22 C21 H21A 109.2 . . ? C22 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? N6 C27 H27 107.9 . . ? N6 C27 C30 112.4(9) . . ? C30 C27 H27 107.9 . . ? C28 C27 N6 111.4(10) . . ? C28 C27 H27 107.9 . . ? C28 C27 C30 109.2(11) . . ? N8 C36 C35 109.3(9) . . ? N8 C36 H36A 109.8 . . ? N8 C36 H36B 109.8 . . ? C35 C36 H36A 109.8 . . ? C35 C36 H36B 109.8 . . ? H36A C36 H36B 108.3 . . ? N5 C23 C24 112.9(9) . . ? N5 C23 H23A 109.0 . . ? N5 C23 H23B 109.0 . . ? C24 C23 H23A 109.0 . . ? C24 C23 H23B 109.0 . . ? H23A C23 H23B 107.8 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N1 C3 H3A 109.3 . . ? N1 C3 H3B 109.3 . . ? N1 C3 C4 111.5(12) . . ? H3A C3 H3B 108.0 . . ? C4 C3 H3A 109.3 . . ? C4 C3 H3B 109.3 . . ? N3 C11 C12 110.8(10) . . ? N3 C11 H11A 109.5 . . ? N3 C11 H11B 109.5 . . ? C12 C11 H11A 109.5 . . ? C12 C11 H11B 109.5 . . ? H11A C11 H11B 108.1 . . ? N2 C6 C5 110.6(10) . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? N2 C7 H7 108.3 . . ? C10 C7 N2 111.2(11) . . ? C10 C7 H7 108.3 . . ? C8 C7 N2 111.3(11) . . ? C8 C7 H7 108.3 . . ? C8 C7 C10 109.3(12) . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10B 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N4 C16 C15 110.1(10) . . ? N4 C16 H16A 109.6 . . ? N4 C16 H16B 109.6 . . ? C15 C16 H16A 109.6 . . ? C15 C16 H16B 109.6 . . ? H16A C16 H16B 108.2 . . ? C20 C19 C17 113.1(10) . . ? C20 C19 H19A 109.0 . . ? C20 C19 H19B 109.0 . . ? C17 C19 H19A 109.0 . . ? C17 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C27 C28 H28A 108.8 . . ? C27 C28 H28B 108.8 . . ? H28A C28 H28B 107.7 . . ? C29 C28 C27 113.6(14) . . ? C29 C28 H28A 108.8 . . ? C29 C28 H28B 108.8 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? H9A C9 H9B 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? N2 C4 H4A 109.3 . . ? N2 C4 H4B 109.3 . . ? C3 C4 N2 111.4(12) . . ? C3 C4 H4A 109.3 . . ? C3 C4 H4B 109.3 . . ? H4A C4 H4B 108.0 . . ? N2 C2 H2A 109.1 . . ? N2 C2 H2B 109.1 . . ? C1 C2 N2 112.4(10) . . ? C1 C2 H2A 109.1 . . ? C1 C2 H2B 109.1 . . ? H2A C2 H2B 107.9 . . ? C7 C8 C9 110.0(11) . . ? C7 C8 H8A 109.7 . . ? C7 C8 H8B 109.7 . . ? C9 C8 H8A 109.7 . . ? C9 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38B 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N11 C42 C41 178.9(19) . . ? N10 C48 C47 173(2) . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C48 C47 H47A 109.5 . . ? C48 C47 H47B 109.5 . . ? C48 C47 H47C 109.5 . . ? H47A C47 H47B 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? H43A C43 H43B 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C44 C43 H43A 109.5 . . ? C44 C43 H43B 109.5 . . ? C44 C43 H43C 109.5 . . ? H45A C45 H45B 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C46 C45 H45A 109.5 . . ? C46 C45 H45B 109.5 . . ? C46 C45 H45C 109.5 . . ? N12 C44 C43 175(2) . . ? N9 C46 C45 171(3) . . ? loop_ _refln_index_h _refln_index_k _refln_index_l _refln_F_squared_meas _refln_F_squared_sigma _refln_scale_group_code -11 -9 5 581.569 317.227 3 -11 -8 5 482.212 402.525 3 -11 -7 5 1710.91 553.661 3 -11 -6 5 13611.6 1482.2 3 -10 -11 6 4810.92 835.227 3 -10 -11 7 10936.7 1292.52 3 -10 -11 8 8388.84 1183.7 3 -10 -10 4 2829.67 632.641 3 -10 -10 5 4628.45 797.57 3 -10 -10 6 3842.07 772.158 3 -10 -10 7 707.643 412.237 3 -10 -10 8 1008.91 479.8 3 -10 -10 9 2226.94 677.435 3 -10 -9 4 2443.91 584.184 3 -10 -9 5 19883.5 1676.15 3 -10 -9 6 569.693 414.654 3 -10 -9 7 1918.57 578.72 3 -10 -9 8 5454.7 968.345 3 -10 -9 9 2178.1 625.593 3 -10 -8 4 14431.1 1422 3 -10 -8 5 5371.23 888.371 3 -10 -8 6 7316.8 1012.6 3 -10 -8 7 2600.88 617.6 3 -10 -8 8 7981.48 1138.85 3 -10 -8 9 6197.93 1054.42 3 -10 -7 4 9403.02 1134.21 3 -10 -7 5 1839.76 538.959 3 -10 -7 6 2000.9 552.241 3 -10 -7 7 229.993 367.383 3 -10 -7 8 1607.88 549.746 3 -10 -7 9 15340.9 1636.54 3 -10 -6 4 702.603 405.733 3 -10 -6 5 3287.43 716.128 3 -10 -6 6 10476.2 1254.92 3 -10 -6 7 15736.2 1567.95 3 -10 -6 8 2620.16 723.45 3 -10 -6 9 11757.5 1411.86 3 -10 -5 4 10536.2 1203.97 3 -10 -5 5 19094.1 1678.5 3 -10 -5 6 4070.93 821.22 3 -10 -5 7 27946.3 2134.88 3 -10 -5 8 23681.6 1989.01 3 -10 -5 9 3169.1 783.943 3 -10 -4 4 1564.77 506.283 3 -10 -4 5 2989.78 715.607 3 -10 -4 6 8368.54 1114.97 3 -10 -4 7 815.332 516.422 3 -10 -4 8 877.727 432.136 3 -10 -4 9 5696.46 995.249 3 -10 -3 5 12215.4 1343.97 3 -10 -3 6 6089.87 949.768 3 -10 -3 7 1937.12 576.501 3 -10 -3 8 4000.15 801.046 3 -10 -3 9 3836.23 823.2 3 -10 -2 5 9482.16 1213.9 3 -10 -2 6 1187.95 560.396 3 -10 -2 7 37306.3 2505.15 3 -10 -2 8 24158.4 2019.68 3 -10 -2 9 856.015 509.257 3 -10 -1 6 20435.6 1792.33 3 -10 -1 7 6944.5 1054.76 3 -10 -1 8 7693.69 1148.52 3 -10 0 7 849.504 403.691 3 -10 0 8 1441.54 497.961 3 -10 1 7 914.289 456.854 3 -9 -14 -1 1087.16 467.107 4 -9 -14 0 1014.76 550.467 4 -9 -14 1 4014.63 889.057 4 -9 -14 2 721.703 447.651 4 -9 -14 3 1354.44 559.329 4 -9 -14 4 7618.18 1155.14 4 -9 -13 -2 10100.2 1280.42 4 -9 -13 -1 1264.45 570.933 4 -9 -13 0 13664.9 1506.32 4 -9 -13 1 1578.37 629.88 4 -9 -13 2 10675.4 1380.41 4 -9 -13 3 14418.1 1611.21 4 -9 -12 -2 937.903 478.494 4 -9 -12 -1 3280.46 724.199 4 -9 -12 0 788.733 332.123 4 -9 -12 1 1891.23 603.763 4 -9 -12 2 7580.34 1093.55 4 -9 -12 3 41884.9 2611.54 4 -9 -12 8 7573.94 1046.75 3 -9 -12 9 4076.68 827.449 3 -9 -12 10 1420.34 583.486 3 -9 -11 -3 12310.6 1290.03 4 -9 -11 -2 10801.1 1209.73 4 -9 -11 -1 1133.11 422.2 4 -9 -11 0 1502.67 427.464 4 -9 -11 1 3398.56 714.712 4 -9 -11 2 11545.3 1263.98 4 -9 -11 3 478.615 333.08 3 -9 -11 4 23434.6 1656.35 3 -9 -11 5 2543.58 587.663 3 -9 -11 6 4281.29 753.881 3 -9 -11 7 15834.9 1473.79 3 -9 -11 8 16967 1584.34 3 -9 -11 9 4460.85 861.293 3 -9 -11 10 307.481 467.192 3 -9 -11 11 3559.14 827.45 3 -9 -10 -3 1273.42 389.134 4 -9 -10 -2 1810.39 504.789 4 -9 -10 -1 11840.5 1177.25 4 -9 -10 0 7728.73 962.805 4 -9 -10 1 8109.76 992.298 4 -9 -10 3 753.978 332.826 3 -9 -10 4 4439.29 733.978 3 -9 -10 5 9922.11 1086.46 3 -9 -10 6 4969.11 800.73 3 -9 -10 7 956.005 439.316 3 -9 -10 8 5290.04 904.135 3 -9 -10 9 5252.82 949.279 3 -9 -10 10 453.038 345.004 3 -9 -10 11 6103.36 1033.89 3 -9 -9 -2 14241.6 1183.51 4 -9 -9 -1 21294.3 1493.13 4 -9 -9 0 50777.7 2464.33 4 -9 -9 2 4274.92 683.575 3 -9 -9 3 2094.79 508.804 3 -9 -9 4 16415.4 1394.2 3 -9 -9 5 5109.63 801.953 3 -9 -9 6 12942.9 1299.49 3 -9 -9 7 199.986 269.638 3 -9 -9 8 2405.47 579.769 3 -9 -9 9 1085 443.275 3 -9 -9 10 11744.5 1379.37 3 -9 -9 11 9018.35 1266.79 3 -9 -9 12 871.213 555.205 3 -9 -8 -2 44.3726 239.468 4 -9 -8 -1 19385.7 1285.97 4 -9 -8 2 11795.7 1141.85 3 -9 -8 3 11428.2 1130.61 3 -9 -8 4 17126.9 1442.05 3 -9 -8 5 46887.4 2573.23 3 -9 -8 6 4504.76 790.903 3 -9 -8 7 686.178 373.698 3 -9 -8 8 4649.69 845.45 3 -9 -8 9 3302.54 760.455 3 -9 -8 10 15114.9 1592.51 3 -9 -8 11 11912.2 1458.64 3 -9 -8 12 5192.23 975.369 3 -9 -7 2 412.533 308.711 3 -9 -7 3 3537.69 638.567 3 -9 -7 4 10068 1102.03 3 -9 -7 5 8250.16 1020.19 3 -9 -7 6 8044.5 1031.23 3 -9 -7 7 4782.16 806.76 3 -9 -7 8 14754.3 1475.59 3 -9 -7 9 3829.77 751.106 3 -9 -7 10 8314.39 1186.05 3 -9 -7 11 2527.66 705.094 3 -9 -7 12 4044.96 854.127 3 -9 -6 2 4265.27 730.754 3 -9 -6 3 16254.9 1379.12 3 -9 -6 4 6040.8 816.984 3 -9 -6 5 7191.1 964.004 3 -9 -6 6 1790.33 543.447 3 -9 -6 7 8085.96 1040.89 3 -9 -6 8 10921 1266.89 3 -9 -6 9 4249.9 829.157 3 -9 -6 10 1230.3 484.594 3 -9 -6 11 3319.06 772.583 3 -9 -6 12 1869.35 652.392 3 -9 -5 3 9650.09 1081.83 3 -9 -5 4 6293.66 870.999 3 -9 -5 5 1453.13 444.142 3 -9 -5 6 30583.3 2065.51 3 -9 -5 7 20517 1733.89 3 -9 -5 8 29596.5 2129.17 3 -9 -5 9 24541.3 1982.14 3 -9 -5 10 5685.16 946.793 3 -9 -5 11 3949.69 854.032 3 -9 -5 12 4987.81 940.3 3 -9 -4 3 12944.2 1244.59 3 -9 -4 4 25206.1 1802.83 3 -9 -4 5 16830.3 1487.26 3 -9 -4 6 798.739 461.162 3 -9 -4 7 13680.6 1388.39 3 -9 -4 8 16430.7 1562.39 3 -9 -4 9 540.924 434.816 3 -9 -4 10 10880.7 1332.97 3 -9 -4 11 14078.2 1552.02 3 -9 -4 12 6237.78 1046.84 3 -9 -4 13 8498.47 1270.95 3 -9 -3 3 14686.9 1351.53 3 -9 -3 4 12433.5 1245.21 3 -9 -3 5 1354.78 497.86 3 -9 -3 6 730.358 383.653 3 -9 -3 7 7050.06 993.398 3 -9 -3 8 2297.69 597.534 3 -9 -3 9 3649.37 761.217 3 -9 -3 10 -148.171 303.318 3 -9 -3 11 3964.07 844.653 3 -9 -3 12 12661.5 1493.52 3 -9 -3 13 9246.49 1343.78 3 -9 -2 4 633.978 442.874 3 -9 -2 5 26088.3 1884.73 3 -9 -2 6 18728.3 1604.02 3 -9 -2 7 4648.51 880.843 3 -9 -2 8 16460.5 1586.36 3 -9 -2 9 24195.6 1962.1 3 -9 -2 10 5988.32 1005.98 3 -9 -2 11 4155.07 834.127 3 -9 -2 12 7764.2 1177.95 3 -9 -1 4 5409.17 826.28 3 -9 -1 5 1496.69 501.097 3 -9 -1 6 1576.82 494.283 3 -9 -1 7 27819.2 2025.31 3 -9 -1 8 32000.7 2226.69 3 -9 -1 9 4352.46 859.583 3 -9 -1 10 9516.37 1239.18 3 -9 -1 11 5054.06 921.989 3 -9 -1 12 4642.53 927.318 3 -9 0 5 2484.38 592.918 3 -9 0 6 1767.68 523.071 3 -9 0 7 592.619 348.129 3 -9 0 8 1430.66 505.226 3 -9 0 9 5112.51 896.325 3 -9 0 10 3866.37 762.032 3 -9 0 11 9712.55 1244.47 3 -9 0 12 17471.3 1766.83 3 -9 1 -11 5083.94 870.973 5 -9 1 -10 10252.4 1201 5 -9 1 -9 4411.02 736.905 5 -9 1 -8 770.062 330.046 5 -9 1 -7 11026.9 1034.68 5 -9 1 -6 3772.05 593.534 5 -9 1 -5 15322.9 1107.47 5 -9 1 -4 1266.59 344.7 5 -9 1 6 14965.5 1459.33 3 -9 1 7 5715.26 895.375 3 -9 1 8 143.041 262.636 3 -9 1 9 3146.71 726.36 3 -9 1 10 802.267 469.142 3 -9 1 11 7378.42 1104.8 3 -9 1 12 2025.68 708.78 3 -9 2 -15 12280.2 1552.47 5 -9 2 -14 755.637 503.414 5 -9 2 -13 2154.44 682.775 5 -9 2 -12 6484.5 1016.85 5 -9 2 -11 981.689 425.973 5 -9 2 -10 8661.77 1090.53 5 -9 2 -9 4164.22 771.335 5 -9 2 -8 9465.11 1042.22 5 -9 2 -7 10913.2 1070.85 5 -9 2 -6 15103.3 1219.28 5 -9 2 -5 20981.6 1394.27 5 -9 2 -4 17810.8 1224.79 5 -9 2 6 22481.3 1824.27 3 -9 2 7 1492.42 526.687 3 -9 2 8 349.015 338.57 3 -9 2 9 19456.7 1747.23 3 -9 2 10 2824.04 771.426 3 -9 2 11 5332.53 979.866 3 -9 3 -14 1650.15 621.911 5 -9 3 -13 2746.49 717.96 5 -9 3 -12 5246.55 935.193 5 -9 3 -11 11666 1318.24 5 -9 3 -10 16193.5 1521.07 5 -9 3 -9 5483.82 871.214 5 -9 3 -8 202.695 311.856 5 -9 3 -7 7730.89 951.011 5 -9 3 -6 4604.58 702.819 5 -9 3 -5 10442.4 1007.16 5 -9 3 -4 5028.7 685.974 5 -9 3 8 2501.57 628.771 3 -9 3 9 2643.65 723.401 3 -9 3 10 8478.03 1178.72 3 -9 4 -13 1018.68 522.793 5 -9 4 -12 5881.83 993.129 5 -9 4 -11 8693.89 1184.85 5 -9 4 -10 9691.68 1225.21 5 -9 4 -9 1083.69 456.696 5 -9 4 -8 1163.15 446.368 5 -9 4 -7 18134.5 1515.82 5 -9 4 -6 10399.9 1097.34 5 -9 4 -5 484.833 318.553 5 -9 4 9 1603.08 578.166 3 -9 5 -12 6347.74 1094.22 5 -9 5 -11 14179.9 1571.7 5 -9 5 -10 3524.66 850.487 5 -9 5 -9 5081.83 876.009 5 -9 5 -8 3306.83 743.389 5 -9 5 -7 14635.3 1433.6 5 -9 5 -6 4033.1 738.442 5 -9 6 -11 1374.3 625.252 5 -9 6 -10 1169.53 535.233 5 -9 6 -9 197.915 384.077 5 -8 -15 -7 1340.27 609.72 4 -8 -15 -6 -647.041 548.606 4 -8 -15 -5 2657.68 781.596 4 -8 -15 -4 1532.4 686.493 4 -8 -15 -3 9294.78 1367.8 4 -8 -15 -2 3564.84 957.383 4 -8 -15 -1 5287.6 1016.6 4 -8 -15 0 3425.73 849.195 4 -8 -15 1 2263.2 706.4 4 -8 -15 2 2785.96 747.326 4 -8 -15 3 5333.97 1025.48 4 -8 -15 4 1630.22 664.16 4 -8 -14 -9 599.411 532.142 4 -8 -14 -8 5634.03 1062.09 4 -8 -14 -7 2583.15 726.685 4 -8 -14 -6 5688.97 1011.95 4 -8 -14 -5 15513.9 1711.57 4 -8 -14 -4 19020.3 1858.71 4 -8 -14 -3 2019.3 709.612 4 -8 -14 -2 678.505 454.509 4 -8 -14 -1 3629.69 810.922 4 -8 -14 0 14024.3 1554.35 4 -8 -14 1 1745.62 581.612 4 -8 -14 2 210.942 322.979 4 -8 -14 3 1022.53 524.825 4 -8 -14 4 24381 2107.47 4 -8 -14 5 2924.39 802.221 4 -8 -14 6 9158.83 1297.62 4 -8 -13 -11 11237.7 1500.21 4 -8 -13 -10 3588.42 906.051 4 -8 -13 -9 5983.71 1040.43 4 -8 -13 -8 8732.53 1248.95 4 -8 -13 -7 7114.45 1122.82 4 -8 -13 -6 6834.68 1107.4 4 -8 -13 -5 33550.6 2409.77 4 -8 -13 -4 5242.25 978.619 4 -8 -13 -3 3677.91 805.638 4 -8 -13 -2 346.464 353.132 4 -8 -13 -1 11769.7 1359.17 4 -8 -13 0 3385.82 766.906 4 -8 -13 1 9752.38 1246.56 4 -8 -13 2 2582.58 705.233 4 -8 -13 3 374.122 398.059 4 -8 -13 4 10566 1335.42 4 -8 -13 5 30318.7 2279.47 4 -8 -12 -11 1072.88 552.311 4 -8 -12 -10 9112.82 1220.09 4 -8 -12 -9 8757.56 1192.08 4 -8 -12 -8 4745.44 882.904 4 -8 -12 -7 789.871 407.043 4 -8 -12 -6 2774.28 692.574 4 -8 -12 -5 4090.27 812.806 4 -8 -12 -4 418.074 447.616 4 -8 -12 -3 8272.73 1125.27 4 -8 -12 -2 2138.18 566.879 4 -8 -12 -1 6383.51 987.024 4 -8 -12 0 39819.8 2511.46 4 -8 -12 1 729.521 413.023 4 -8 -12 2 2891.78 703.042 4 -8 -12 3 7376.22 1061.92 4 -8 -12 3 6944.66 776.228 3 -8 -12 4 6092.55 775.341 3 -8 -12 4 5917.93 991.685 4 -8 -12 5 229.613 259.387 3 -8 -12 5 172.611 361.67 4 -8 -12 6 1759.07 501 3 -8 -12 7 1511 506.476 3 -8 -12 8 4642.7 783.875 3 -8 -12 9 648.945 384.277 3 -8 -12 10 4803.42 879.57 3 -8 -12 11 1035.48 461.436 3 -8 -12 12 8013.65 1167.84 3 -8 -11 -11 4183.36 885.049 4 -8 -11 -10 674.717 432.578 4 -8 -11 -9 4476.62 845.145 4 -8 -11 -8 1061.79 517.73 4 -8 -11 -7 12403.2 1343.95 4 -8 -11 -6 438.05 338.126 4 -8 -11 -5 5871.41 894.746 4 -8 -11 -4 23027.7 1799.06 4 -8 -11 -3 5989.32 922.723 4 -8 -11 -2 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3 -10 -1 6107.73 825.936 4 3 -10 0 949.875 248.719 1 3 -10 0 1320.02 379.866 3 3 -10 0 921.834 360.278 4 3 -10 1 999.987 281.554 1 3 -10 1 1211.72 343.46 3 3 -10 1 1071.49 370.36 4 3 -10 2 5734.67 618.713 1 3 -10 2 4890.21 651.242 3 3 -10 2 5813.05 801.141 4 3 -10 3 4177.19 529.942 1 3 -10 3 4176.62 694.645 4 3 -10 4 4472.62 559.942 1 3 -10 4 4538.88 713.742 4 3 -10 5 35296.8 1765.57 1 3 -10 5 36684.1 2140.88 4 3 -10 6 32009.2 1995.41 4 3 -10 7 18390.2 1482.32 4 3 -10 8 2922.28 589.557 4 3 -9 -10 30080.3 2037.76 4 3 -9 -9 905.534 495.656 4 3 -9 -8 16857.6 1060.81 3 3 -9 -8 17471.3 1450.54 4 3 -9 -7 26926.3 1399.72 3 3 -9 -7 28434.9 1846.54 4 3 -9 -6 12394.5 898.681 3 3 -9 -6 13871.3 1210.82 4 3 -9 -5 579.619 181.985 3 3 -9 -5 738.691 352.219 4 3 -9 -4 4052.39 494.071 1 3 -9 -4 3390.27 475.227 3 3 -9 -4 4126.05 649.448 4 3 -9 -3 6022.63 603.208 1 3 -9 -3 5271.42 611.067 3 3 -9 -3 5612.99 747.644 4 3 -9 -2 13438.5 915.972 1 3 -9 -2 11907.4 953.775 3 3 -9 -2 12365.7 1115.22 4 3 -9 -1 18080.4 1101.43 1 3 -9 -1 17656.2 1217.12 3 3 -9 -1 19348.5 1393.83 4 3 -9 0 140403 4276.9 1 3 -9 0 146489 4814.27 4 3 -9 0 131627 4453.47 3 3 -9 1 17911 1094.36 1 3 -9 1 17014 1293.99 4 3 -9 1 15239.1 1140.17 3 3 -9 2 9324.3 788.071 1 3 -9 2 9688.27 971.837 4 3 -9 2 8815.18 855.756 3 3 -9 3 959.999 272.972 1 3 -9 3 1716.89 442.687 4 3 -9 4 2612.33 440.462 1 3 -9 4 3500.15 592.834 4 3 -9 5 8856.04 934.709 4 3 -9 6 884.886 356.751 4 3 -9 7 45472.9 2352.42 4 3 -9 8 16564.3 1353.49 4 3 -8 -9 13920.1 1114.88 2 3 -8 -8 23158.4 1482.91 2 3 -8 -8 23334.9 1264.5 3 3 -8 -8 24444.4 1671.36 4 3 -8 -7 2133.3 453.237 2 3 -8 -7 2805.55 418.243 3 3 -8 -7 1949.73 467.319 4 3 -8 -6 -69.9595 220.482 2 3 -8 -6 -54.0454 151.674 3 3 -8 -6 268.228 211.987 4 3 -8 -5 7357.77 677.351 3 3 -8 -5 7290.83 790.933 2 3 -8 -5 8412.84 877.435 4 3 -8 -4 13341.7 908.384 1 3 -8 -4 11546.7 880.559 3 3 -8 -4 12612.2 1032.1 2 3 -8 -4 11565.2 1021.18 4 3 -8 -3 34849.4 1583.24 1 3 -8 -3 32143.8 1607.5 3 3 -8 -3 36551.3 1852.23 2 3 -8 -3 34441.1 1846.81 4 3 -8 -2 3615.1 462.516 1 3 -8 -2 3879.98 507.005 3 3 -8 -2 3971.23 574.275 2 3 -8 -2 4631.01 626.131 4 3 -8 -1 60667.1 2312.18 1 3 -8 -1 63204.8 2635.3 4 3 -8 -1 61676 2456.84 3 3 -8 0 14594.2 1114.21 4 3 -8 0 14587.1 1051.62 3 3 -8 1 42107 2055.57 4 3 -8 1 43433.9 2004.05 3 3 -8 2 13228 1090.07 4 3 -8 2 13592.4 1044.92 3 3 -8 3 44911.9 2172.78 4 3 -8 4 646.794 265.543 4 3 -8 5 8718.58 876.403 4 3 -8 6 4851 669.599 4 3 -8 7 9691.98 951.287 4 3 -8 8 26835.9 1679.94 4 3 -7 -12 19838 1416.12 2 3 -7 -11 3186.53 552.923 2 3 -7 -10 4640.01 618.092 2 3 -7 -9 11847.4 970.417 2 3 -7 -8 105965 3512.67 3 3 -7 -8 117700 3853.41 2 3 -7 -7 60264.7 2265.35 3 3 -7 -7 58932.5 2475.9 2 3 -7 -6 5286.12 617.787 2 3 -7 -6 4197.12 490.267 3 3 -7 -6 5469.12 692.257 4 3 -7 -5 5089.05 562.958 1 3 -7 -5 5005.03 644.216 2 3 -7 -5 5049.85 656.805 4 3 -7 -4 5043.97 538.017 1 3 -7 -4 4662.87 583.562 2 3 -7 -4 4423.27 590.547 4 3 -7 -3 45349.6 1884.39 1 3 -7 -3 47859.4 2097.48 2 3 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23349 1334.6 4 3 -6 6 32725.5 1648.5 4 3 -5 -13 6057.57 731.492 2 3 -5 -12 14662.4 1103.1 2 3 -5 -11 26434.5 1480.6 2 3 -5 -10 24000.1 1349.2 2 3 -5 -9 3294.29 469.017 2 3 -5 -8 9304.25 729.368 2 3 -5 -7 12832 863.481 2 3 -5 -6 11872.8 817.924 2 3 -5 -5 9606.47 716.836 2 3 -5 -4 420.812 168.115 2 3 -5 -3 10711.9 755.169 2 3 -5 -3 10787.6 785.975 4 3 -5 -2 2501.48 367.147 4 3 -5 -1 42572.9 1712.62 4 3 -5 0 194763 5426.21 4 3 -5 1 48002.3 1852.91 4 3 -5 2 7105.83 603.347 4 3 -5 3 662.561 206.671 4 3 -5 4 344.494 170.263 4 3 -5 5 14788 951.902 4 3 -4 -12 18314.2 1204.25 2 3 -4 -11 24888.2 1380.29 2 3 -4 -10 280.707 183.4 2 3 -4 -9 6135.02 582.605 2 3 -4 -8 6685.24 581.81 2 3 -4 -7 3247.46 392.111 2 3 -4 -6 6956.47 606.264 1 3 -4 -6 6055.71 531.892 2 3 -4 -5 227711 6074.01 2 3 -4 -4 10598.5 691.325 2 3 -4 -3 24712.8 1221.79 3 3 -4 -3 25931.8 1163.7 2 3 -4 -2 20151 1076.33 3 3 -4 -2 20073.4 1005.08 4 3 -4 -1 39654.1 1625.23 1 3 -4 -1 38769.8 1631.06 3 3 -4 -1 38983.9 1498.23 4 3 -4 0 1545.57 299.626 1 3 -4 0 1686.85 310.245 3 3 -4 0 1631.3 266.45 4 3 -4 1 16933.2 882.934 4 3 -4 1 17600 1018.05 3 3 -4 2 35431.8 1415.4 4 3 -4 3 10313.2 674.743 4 3 -4 4 41084.6 1603.92 4 3 -3 -10 5497.52 553.736 2 3 -3 -9 18047.7 997.561 2 3 -3 -8 62452.6 2149.15 2 3 -3 -7 2693.39 321.438 2 3 -3 -6 19540.5 914.496 2 3 -3 -5 1168.4 210.943 2 3 -3 -4 83178.2 2696.56 3 3 -3 -4 83299.4 2500.71 2 3 -3 -3 25382.2 1073.06 2 3 -3 -3 26195.4 1221.04 3 3 -3 -2 23885.4 1163.67 3 3 -3 -1 5321.85 510.168 1 3 -3 -1 5542.14 416.769 4 3 -3 -1 5771.86 521.515 3 3 -3 0 113194 3527.52 1 3 -3 0 119844 3254.27 4 3 -3 1 20100.2 862.972 4 3 -3 2 43747.6 1492.05 4 3 -3 3 44497.4 1532.92 4 3 -3 21 3882.83 919.068 2 3 -2 -8 345.489 152.967 2 3 -2 -7 12960 693.265 2 3 -2 -6 28925.8 1087.75 2 3 -2 -5 1039.48 164.254 2 3 -2 -5 525.628 174.301 3 3 -2 -4 49033.3 1531.67 2 3 -2 -3 132616 3523.51 2 3 -2 -1 10015.6 501.311 4 3 -2 0 1169.15 151.883 4 3 -2 1 5111.09 325.347 4 3 -2 2 34005.5 1096.2 4 3 -2 7 8399.97 766.631 5 3 -2 8 2429.01 436.062 5 3 -2 9 2018.13 406.548 5 3 -2 10 19639.1 1349.95 5 3 -2 11 55173.6 2568.47 5 3 -2 19 3014.23 743.317 2 3 -2 20 56022.1 3389.44 2 3 -2 21 7378.97 1217.09 2 3 -1 -6 461.974 123.561 2 3 -1 -5 12031.2 516.648 2 3 -1 -4 99875.4 2595.17 2 3 -1 -3 112556 2888.27 2 3 -1 0 34100.6 956.932 4 3 -1 4 102068 3132.6 5 3 -1 5 36506.8 1552.22 5 3 -1 6 18534.8 1067.14 5 3 -1 7 44425.6 1903.9 5 3 -1 8 161624 4943.83 5 3 -1 9 34352.3 1754.03 5 3 -1 10 1916.48 416.423 5 3 -1 11 27612.6 1659.15 5 3 -1 12 80761.7 3313.34 5 3 -1 17 12377 1375.91 2 3 -1 18 14794 1545.08 2 3 -1 19 4233.3 874.151 2 3 -1 20 4919.83 994.873 2 3 -1 21 28945.5 2391.09 2 3 -1 22 151.124 424.209 2 3 0 1 22429.9 1028.19 3 3 0 2 1439.51 203.723 5 3 0 2 1500.17 242.173 3 3 0 3 27474 1108.67 5 3 0 4 64015.8 2123.53 5 3 0 5 249821 6669.7 5 3 0 6 109000 3427.66 5 3 0 7 30354.7 1479.2 5 3 0 8 25729.6 1420.64 5 3 0 9 2082.74 398.729 5 3 0 10 34340.9 1814.06 5 3 0 11 39658.1 2060.67 5 3 0 12 4457.98 631.743 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1 10 3 -6 6420.59 948.647 1 10 3 -5 13942.8 1346.28 1 10 3 -4 1152.69 439.123 1 10 3 -3 10625.8 1181.03 1 10 3 -2 12537.3 1319.65 1 10 3 -1 3889.84 755.372 1 10 3 0 686.87 403.325 1 10 3 1 3534.79 691.202 1 10 3 2 2500.74 613.667 1 10 3 3 4515.59 844.085 1 10 3 3 7312.74 787.344 2 10 3 4 24969.5 1577.2 2 10 3 5 2544.04 558.419 2 10 3 6 3359.71 649.566 2 10 3 7 12313.2 1248.05 2 10 3 8 117.254 401.397 2 10 3 9 1228.08 406.19 2 10 3 10 4333.54 841.387 2 10 3 11 2563.63 631.38 2 10 3 12 481.352 413.02 2 10 3 13 8990.63 1307.28 2 10 4 -9 6616.51 890.466 1 10 4 -8 1000.78 432.861 1 10 4 -7 1827.56 526.088 1 10 4 -6 10561.2 1138.67 1 10 4 -5 3721.04 689.798 1 10 4 -4 1155.35 441.647 1 10 4 -3 16806.5 1490.86 1 10 4 -2 7124.59 971.747 1 10 4 -1 3567.42 733.589 1 10 4 0 2890.61 610.256 1 10 4 1 12582.2 1339.82 1 10 4 2 10949.7 1260.01 1 10 4 3 314.175 287.121 1 10 4 4 5624.41 738.021 2 10 4 5 3893.41 673.521 2 10 4 6 1950.85 551.409 2 10 4 7 8516.48 1023.99 2 10 4 8 2623.64 593.643 2 10 4 9 1154.78 472.916 2 10 4 10 569.161 368.573 2 10 4 11 13931.4 1513.12 2 10 4 12 6944.26 1089.5 2 10 4 13 1499.64 539.825 2 10 5 -8 25976.5 1785.33 1 10 5 -7 26826.1 1827.48 1 10 5 -6 4054.13 717.406 1 10 5 -5 20187.8 1586.74 1 10 5 -4 11233.5 1167.46 1 10 5 -3 2870.75 590.898 1 10 5 -2 2805.7 594.709 1 10 5 -1 15799 1443.95 1 10 5 0 7130.23 961.216 1 10 5 1 5744.2 873.867 1 10 5 2 12323.8 1312.27 1 10 5 3 11857.8 1294.55 1 10 5 4 3105.14 545.958 2 10 5 5 5920.25 822.39 2 10 5 6 36422.3 2193.38 2 10 5 7 17156.4 1490.04 2 10 5 8 2492.28 661.228 2 10 5 9 13857.5 1431.19 2 10 5 10 4931.68 897.606 2 10 5 11 5044.27 941.804 2 10 5 12 9916.2 1310.24 2 10 6 -8 4217.59 701.504 1 10 6 -7 16513.7 1370.55 1 10 6 -6 12454.4 1207.1 1 10 6 -5 3955.32 661.941 1 10 6 -4 179.329 294.388 1 10 6 -3 4421.88 728.225 1 10 6 -2 15405.8 1361.73 1 10 6 -1 2088.39 555.371 1 10 6 0 17785.1 1525.53 1 10 6 1 28908.7 2003.04 1 10 6 2 1746.78 494.94 1 10 6 3 1456.68 441.154 1 10 6 4 2729.51 560.318 2 10 6 5 196.483 276.897 2 10 6 6 10324.7 1136.36 2 10 6 7 11873.1 1265.19 2 10 6 8 20471.6 1757.43 2 10 6 9 75.183 331.913 2 10 6 10 3331.87 778.894 2 10 6 11 6240.24 1032.89 2 10 6 12 8108.62 1209.45 2 10 7 -7 432.671 222.732 1 10 7 -6 2168.25 504.598 1 10 7 -5 1819.53 445.958 1 10 7 -4 11136.9 1111.53 1 10 7 -3 1346.81 409.635 1 10 7 -2 10700.8 1102.88 1 10 7 -1 14369 1319.96 1 10 7 0 16799.7 1441.02 1 10 7 1 12325.3 1235.94 1 10 7 2 6068.59 865.26 1 10 7 3 9567.41 1121.97 1 10 7 4 781.2 376.801 1 10 7 4 1497.75 453.006 2 10 7 5 4687.04 736.594 2 10 7 6 3130.82 635.427 2 10 7 7 574.747 375.705 2 10 7 8 12959.8 1389.45 2 10 7 9 -53.1854 358.727 2 10 7 10 10799.5 1363.08 2 10 7 11 2641.53 705.047 2 10 7 12 2700.52 721.467 2 10 8 -6 6268.08 799.469 1 10 8 -5 5941.99 774.882 1 10 8 -4 12869.7 1172.05 1 10 8 -3 4368.04 682.022 1 10 8 -2 1781.29 444.234 1 10 8 -1 13292.2 1229.09 1 10 8 0 19116.7 1521.37 1 10 8 1 210.993 231.641 1 10 8 2 1229.21 370.961 1 10 8 3 5381.3 833.966 1 10 8 4 6843.66 970.182 1 10 8 4 8926.55 1010.26 2 10 8 5 14627.1 1341.01 2 10 8 6 5123.61 822.814 2 10 8 7 468.852 362.915 2 10 8 8 1699.56 624.721 2 10 8 9 33800.4 2376.48 2 10 8 10 7473.34 1148.62 2 10 8 11 2529.56 722.387 2 10 9 -4 2432.73 500.162 1 10 9 -3 927.262 353.153 1 10 9 -2 8476.19 915.085 1 10 9 -1 7359.66 894.129 1 10 9 0 8239.18 973.451 1 10 9 1 20388 1557.82 1 10 9 2 2783.4 585.207 1 10 9 3 1580.67 456.348 1 10 9 4 8721.63 1068.85 1 10 9 5 14828.1 1392.33 2 10 9 6 7391.45 1029.12 2 10 9 7 640.355 389.726 2 10 9 8 1345.45 565.185 2 10 9 9 2440.66 665.511 2 10 9 10 646.538 526.932 2 10 10 5 1747.93 496.507 1 10 10 6 5891.34 943.963 2 10 10 7 2228.28 680.745 2 10 10 8 1034.03 443.9 2 10 10 9 5865.08 1026.72 2 10 10 10 2779.03 774.403 2 10 11 6 2775.29 725.939 2 10 11 7 16416.1 1658.15 2 10 11 8 7134.18 1165.07 2 11 2 -4 10557.1 1302.79 1 11 2 -3 2870.49 721.165 1 11 2 -2 1168.95 503.919 1 11 2 -1 5220.13 925.082 1 11 2 0 2543.57 700.445 1 11 2 1 1497.12 537.918 1 11 2 2 3038.14 756.279 1 11 2 3 8804.34 1244.21 1 11 3 -6 11278.4 1308.85 1 11 3 -5 7731.26 1087.02 1 11 3 -4 20012.8 1758.67 1 11 3 -3 3645.16 773.073 1 11 3 -2 833.456 426.438 1 11 3 -1 6415.06 1009.38 1 11 3 0 6898.34 1064.48 1 11 3 1 5638.22 959.083 1 11 3 2 2759.55 690.426 1 11 3 3 7366.92 1118.71 1 11 3 4 6387.48 1070.17 1 11 4 -7 3227.42 703.923 1 11 4 -6 15034.4 1469.75 1 11 4 -5 14353 1445.84 1 11 4 -4 4160.47 794.408 1 11 4 -3 6459 980.033 1 11 4 -2 1071.91 423.804 1 11 4 -1 13673.3 1448.2 1 11 4 0 13009.6 1435.38 1 11 4 1 10413.1 1291.06 1 11 4 2 8286.44 1154.61 1 11 4 3 -217.114 428.864 1 11 4 4 12912.1 1489.45 1 11 4 5 16734.6 1728.39 1 11 5 -8 508.195 356.029 1 11 5 -7 9714.9 1133.8 1 11 5 -6 11329 1238.03 1 11 5 -5 5480.44 872.507 1 11 5 -4 15210.2 1463.69 1 11 5 -3 6545.45 968.633 1 11 5 -2 1353.21 458.814 1 11 5 -1 1406.48 494.352 1 11 5 0 4699.39 850.95 1 11 5 1 930.638 401.071 1 11 5 2 -444.451 479.904 1 11 5 3 8392.19 1169.89 1 11 5 4 3208.52 741.758 1 11 5 5 12174.7 1438.4 1 11 6 -8 5118.04 841.232 1 11 6 -7 844.415 394.871 1 11 6 -6 8692.14 1068.33 1 11 6 -5 15723.3 1452.72 1 11 6 -4 593.423 382.317 1 11 6 -3 6739.75 959.36 1 11 6 -2 12884.5 1336.96 1 11 6 -1 2441.47 572.174 1 11 6 0 -100.318 262.247 1 11 6 1 1459.21 499.139 1 11 6 2 4049.98 798.204 1 11 6 3 3890.03 815.587 1 11 6 4 22704.1 1932.32 1 11 6 5 3856.81 832.592 1 11 7 -7 3073.3 632.206 1 11 7 -6 3548.79 671.165 1 11 7 -5 1697.45 490.285 1 11 7 -4 12658.3 1277.11 1 11 7 -3 29508 2018.26 1 11 7 -2 3876.62 710.844 1 11 7 -1 22862.3 1788.1 1 11 7 0 5762.41 953.084 1 11 7 1 714.033 387.435 1 11 7 2 36312.7 2408.28 1 11 7 3 10010.3 1247.06 1 11 7 4 14313.5 1507.78 1 11 7 5 7745.51 1114.75 1 11 8 -5 -143.447 258.852 1 11 8 -4 2916.64 595.259 1 11 8 -3 7030.22 935.033 1 11 8 -2 15920.6 1424.49 1 11 8 -1 5589.37 854.056 1 11 8 0 9512.92 1125.23 1 11 8 1 15026.9 1446.72 1 11 8 2 3798.19 749.645 1 11 8 3 19794.7 1728.03 1 11 8 4 1841.18 556.063 1 11 8 5 1201.13 433.58 1 11 8 6 3384.73 746.103 1 11 9 2 5343.16 861.106 1 11 9 3 1119.29 441.928 1 11 9 4 486.23 312.23 1 11 9 5 434.025 280.753 1 _iucr_refine_instructions_details ; TITL 71-b-100k_a.res in P1 REM Old TITL 71-b-100K in P1 #1 REM SHELXT solution in P1 REM R1 0.085, Rweak 0.025, Alpha 0.000, Orientation as input REM Flack x = 0.023 ( 0.041 ) from Parsons' quotients REM Formula found by SHELXT: C23 N6 Cu10 I14 CELL 0.71073 8.690653 13.395725 18.004221 89.4074 89.8888 79.2342 ZERR 2 0.000176 0.000343 0.000524 0.0022 0.002 0.0019 LATT -1 SFAC C H Cu I N UNIT 48 96 10 14 12 DELU 0.005 0.005 C8 C9 C4 C3 DELU 0.001 0.001 C46 N9 C46 C45 ISOR 0.001 0.002 C4 C9 N9 C46 L.S. 4 0 0 PLAN 20 SIZE 0.22 0.21 0.15 BOND $H LIST 6 fmap 2 53 acta REM REM REM WGHT 0.035600 FVAR 1.58408 I13 4 0.724289 0.494642 0.224158 11.00000 0.01792 0.01696 = 0.01646 -0.00014 -0.00023 -0.00554 I12 4 0.780419 0.309179 0.430477 11.00000 0.01620 0.01770 = 0.01546 0.00028 -0.00210 -0.00564 I003 4 0.560259 0.204912 0.223860 11.00000 0.01400 0.01928 = 0.01919 -0.00462 -0.00044 -0.00547 I11 4 1.083559 0.217125 0.234435 11.00000 0.01256 0.01931 = 0.01797 -0.00397 -0.00175 -0.00289 I9 4 0.812344 0.300794 0.035623 11.00000 0.01479 0.01628 = 0.01894 -0.00154 -0.00163 -0.00253 I3 4 0.328202 0.797359 0.917421 11.00000 0.01508 0.01598 = 0.01958 -0.00075 0.00003 -0.00320 I4 4 0.444133 0.468523 0.855253 11.00000 0.01953 0.01534 = 0.01830 0.00180 -0.00268 -0.00498 I1 4 0.296152 0.808108 0.520069 11.00000 0.01964 0.01800 = 0.01341 -0.00133 -0.00181 -0.00610 I8 4 0.919812 -0.027857 0.100763 11.00000 0.01812 0.01509 = 0.02368 -0.00435 0.00028 -0.00425 I5 4 0.084432 0.698474 0.729441 11.00000 0.01712 0.02218 = 0.02141 0.00542 -0.00433 -0.00836 I6 4 0.605146 0.715387 0.719716 11.00000 0.01658 0.02170 = 0.01693 0.00326 -0.00198 -0.00590 I2 4 0.247477 0.989519 0.728452 11.00000 0.02870 0.01868 = 0.01622 -0.00065 -0.00608 -0.00940 I10 4 0.881670 -0.009630 0.344112 11.00000 0.03891 0.01983 = 0.02035 0.00127 0.00004 -0.00557 I7 4 0.413698 0.489445 0.611229 11.00000 0.05746 0.02055 = 0.01718 -0.00243 -0.00617 -0.00800 CU5 3 0.514942 0.649130 0.852213 11.00000 0.01592 0.01740 = 0.02072 0.00107 -0.00388 -0.00308 CU10 3 0.627616 0.356856 0.305242 11.00000 0.01376 0.02129 = 0.01589 -0.00099 -0.00012 -0.00302 CU7 3 0.796571 0.300895 0.181675 11.00000 0.01777 0.02197 = 0.02124 -0.00574 0.00040 -0.00405 CU1 3 0.152375 0.851837 0.646932 11.00000 0.01733 0.02077 = 0.01624 -0.00032 -0.00346 -0.00437 CU4 3 0.317256 0.794927 0.771667 11.00000 0.02004 0.02571 = 0.02076 0.00357 -0.00331 -0.00647 CU6 3 0.994723 0.151362 0.103912 11.00000 0.01464 0.01734 = 0.02312 -0.00354 0.00013 -0.00304 CU8 3 0.828404 0.079373 0.213003 11.00000 0.02958 0.02366 = 0.02072 -0.00376 0.00113 -0.00178 CU9 3 0.858030 0.187000 0.325184 11.00000 0.03117 0.02382 = 0.02381 -0.00483 0.00296 -0.00526 CU2 3 0.383115 0.686073 0.626792 11.00000 0.03337 0.02339 = 0.02166 0.00287 -0.00702 -0.00555 CU3 3 0.357105 0.576573 0.741358 11.00000 0.03636 0.02469 = 0.01790 0.00070 -0.00598 -0.00356 N1 5 -0.075792 0.928341 0.614697 11.00000 0.01969 0.01816 = 0.01966 -0.00691 0.00015 0.00034 N3 5 0.724412 0.631172 0.915799 11.00000 0.00532 0.01658 = 0.02707 -0.00392 -0.00117 -0.00040 N5 5 1.205038 0.128256 0.040381 11.00000 0.01701 0.01937 = 0.01739 -0.00288 -0.00417 -0.00763 N7 5 0.403107 0.426460 0.344900 11.00000 0.01529 0.01421 = 0.01534 -0.00163 -0.00371 -0.00315 N4 5 0.981191 0.611325 0.992327 11.00000 0.01536 0.01455 = 0.01447 0.00158 0.00060 -0.00585 C34 1 0.251364 0.577144 0.413253 11.00000 0.02292 0.02011 = 0.00768 -0.00614 0.00169 -0.00766 AFIX 23 H34A 2 0.250216 0.593866 0.465567 11.00000 -1.20000 H34B 2 0.227626 0.639934 0.384703 11.00000 -1.20000 AFIX 0 C31 1 0.333898 0.354810 0.389731 11.00000 0.01385 0.01447 = 0.02588 -0.00026 -0.00160 -0.00415 AFIX 23 H31A 2 0.410624 0.321166 0.425285 11.00000 -1.20000 H31B 2 0.305354 0.303308 0.357791 11.00000 -1.20000 AFIX 0 C40 1 -0.257581 0.706933 0.415747 11.00000 0.03266 0.02640 = 0.05852 -0.01457 0.00547 -0.00222 AFIX 137 H40A 2 -0.313486 0.672649 0.381319 11.00000 -1.50000 H40B 2 -0.284238 0.778939 0.407151 11.00000 -1.50000 H40C 2 -0.285630 0.691554 0.465601 11.00000 -1.50000 AFIX 0 C37 1 -0.032278 0.559310 0.428049 11.00000 0.01636 0.02991 = 0.03882 -0.01545 0.00049 -0.00581 AFIX 13 H37 2 -0.108126 0.522611 0.405965 11.00000 -1.20000 AFIX 0 C22 1 1.323190 0.097570 -0.084567 11.00000 0.01693 0.01657 = 0.02387 -0.00103 -0.00136 -0.00185 AFIX 23 H22A 2 1.347754 0.036422 -0.114019 11.00000 -1.20000 H22B 2 1.298241 0.155392 -0.118162 11.00000 -1.20000 AFIX 0 N8 5 0.130642 0.511545 0.397592 11.00000 0.01826 0.00771 = 0.02829 -0.00393 -0.00021 -0.00679 C20 1 1.361001 0.468890 1.083370 11.00000 0.01749 0.03034 = 0.02242 -0.00337 -0.00280 0.00196 AFIX 137 H20A 2 1.417887 0.468076 1.037553 11.00000 -1.50000 H20B 2 1.386734 0.403438 1.107164 11.00000 -1.50000 H20C 2 1.388780 0.519572 1.115398 11.00000 -1.50000 AFIX 0 N2 5 -0.351349 1.024022 0.575026 11.00000 0.01781 0.01994 = 0.01546 0.00352 -0.00457 0.00059 C14 1 0.849487 0.586736 1.038970 11.00000 0.02204 0.04889 = 0.01668 0.00364 0.00889 -0.01481 AFIX 23 H14A 2 0.833024 0.631653 1.081324 11.00000 -1.20000 H14B 2 0.876931 0.517433 1.057471 11.00000 -1.20000 AFIX 0 C17 1 1.135436 0.599922 1.035631 11.00000 0.00453 0.02872 = 0.01199 -0.00180 -0.00100 -0.00237 AFIX 13 H17 2 1.215902 0.612098 1.000239 11.00000 -1.20000 AFIX 0 C25 1 1.331865 0.053106 0.075666 11.00000 0.01695 0.01551 = 0.02530 0.00133 -0.00705 -0.00657 AFIX 23 H25A 2 1.293684 -0.009031 0.086551 11.00000 -1.20000 H25B 2 1.362057 0.079890 0.122173 11.00000 -1.20000 AFIX 0 C15 1 0.849231 0.552595 0.882972 11.00000 0.01980 0.01375 = 0.01667 -0.00180 0.00600 -0.00345 AFIX 23 H15A 2 0.867000 0.571016 0.831849 11.00000 -1.20000 H15B 2 0.814752 0.487777 0.882948 11.00000 -1.20000 AFIX 0 C1 1 -0.157227 0.862097 0.570784 11.00000 0.01342 0.02168 = 0.01734 -0.00157 -0.00361 -0.00399 AFIX 23 H1A 2 -0.162946 0.801005 0.599229 11.00000 -1.20000 H1B 2 -0.098218 0.842144 0.525839 11.00000 -1.20000 AFIX 0 C12 1 0.931695 0.716425 0.965497 11.00000 0.01971 0.02731 = 0.06566 0.02164 -0.02903 -0.00945 AFIX 23 H12A 2 1.015204 0.736117 0.936241 11.00000 -1.20000 H12B 2 0.911844 0.761627 1.007597 11.00000 -1.20000 AFIX 0 C13 1 0.696974 0.599091 0.992989 11.00000 0.01473 0.01694 = 0.00828 0.00420 0.00208 0.00095 AFIX 23 H13A 2 0.660129 0.535071 0.992402 11.00000 -1.20000 H13B 2 0.616692 0.649469 1.015886 11.00000 -1.20000 AFIX 0 C5 1 -0.066777 1.020631 0.570298 11.00000 0.03453 0.02620 = 0.01450 0.00284 0.00400 -0.00830 AFIX 23 H5A 2 -0.000039 1.001856 0.527510 11.00000 -1.20000 H5B 2 -0.019479 1.066730 0.600108 11.00000 -1.20000 AFIX 0 C39 1 -0.080359 0.671134 0.404803 11.00000 0.02063 0.02547 = 0.04996 -0.01692 0.00579 -0.00798 AFIX 23 H39A 2 -0.053640 0.679305 0.353042 11.00000 -1.20000 H39B 2 -0.023691 0.712405 0.434396 11.00000 -1.20000 AFIX 0 N6 5 1.463822 0.108090 -0.036590 11.00000 0.01811 0.01232 = 0.01431 -0.00202 -0.00145 -0.00126 C26 1 1.473209 0.029802 0.025095 11.00000 0.02100 0.01165 = 0.02801 0.00339 -0.00304 -0.00308 AFIX 23 H26A 2 1.567718 0.029018 0.053841 11.00000 -1.20000 H26B 2 1.478852 -0.037014 0.003818 11.00000 -1.20000 AFIX 0 C33 1 0.187563 0.408882 0.431505 11.00000 0.01860 0.00868 = 0.03908 0.00037 -0.00308 -0.00661 AFIX 23 H33A 2 0.105817 0.368663 0.428859 11.00000 -1.20000 H33B 2 0.212956 0.415972 0.483393 11.00000 -1.20000 AFIX 0 C35 1 0.288483 0.465496 0.284006 11.00000 0.02081 0.01928 = 0.01097 0.00207 -0.00761 -0.00597 AFIX 23 H35A 2 0.289804 0.413004 0.247175 11.00000 -1.20000 H35B 2 0.319734 0.523575 0.259772 11.00000 -1.20000 AFIX 0 C32 1 0.414263 0.516743 0.391179 11.00000 0.00744 0.03804 = 0.02604 -0.01081 0.00284 -0.00788 AFIX 23 H32A 2 0.470610 0.561150 0.363662 11.00000 -1.20000 H32B 2 0.473529 0.494273 0.435832 11.00000 -1.20000 AFIX 0 C24 1 1.425237 0.210943 0.000666 11.00000 0.02357 0.01542 = 0.03147 -0.01061 0.00577 -0.01184 AFIX 23 H24A 2 1.501617 0.215274 0.039143 11.00000 -1.20000 H24B 2 1.429051 0.264521 -0.035568 11.00000 -1.20000 AFIX 0 C21 1 1.182801 0.092214 -0.034218 11.00000 0.02292 0.02129 = 0.01632 -0.00060 -0.00486 -0.00698 AFIX 23 H21A 2 1.089439 0.133118 -0.055844 11.00000 -1.20000 H21B 2 1.166973 0.022496 -0.031262 11.00000 -1.20000 AFIX 0 C27 1 1.617077 0.099324 -0.079724 11.00000 0.01602 0.02923 = 0.01988 -0.00920 0.00210 -0.00614 AFIX 13 H27 2 1.693387 0.123217 -0.047646 11.00000 -1.20000 AFIX 0 C36 1 0.122537 0.496679 0.314861 11.00000 0.02293 0.03010 = 0.02054 -0.01336 -0.00901 -0.00307 AFIX 23 H36A 2 0.070925 0.559338 0.291131 11.00000 -1.20000 H36B 2 0.062213 0.444374 0.304500 11.00000 -1.20000 AFIX 0 C23 1 1.263101 0.224116 0.034328 11.00000 0.02022 0.01797 = 0.01761 -0.01352 0.00573 -0.00629 AFIX 23 H23A 2 1.265210 0.253054 0.083397 11.00000 -1.20000 H23B 2 1.191125 0.271688 0.003992 11.00000 -1.20000 AFIX 0 C30 1 1.685499 -0.011419 -0.101520 11.00000 0.02163 0.02165 = 0.03868 -0.01273 0.01197 -0.00174 AFIX 137 H30A 2 1.699112 -0.053607 -0.057714 11.00000 -1.50000 H30B 2 1.784937 -0.013903 -0.125446 11.00000 -1.50000 H30C 2 1.614936 -0.035516 -0.134935 11.00000 -1.50000 AFIX 0 C3 1 -0.175772 0.959577 0.680167 11.00000 0.02782 0.02085 = 0.02555 -0.00697 0.01044 -0.00868 AFIX 23 H3A 2 -0.122647 0.999148 0.712923 11.00000 -1.20000 H3B 2 -0.192350 0.899548 0.707299 11.00000 -1.20000 AFIX 0 C11 1 0.782169 0.727350 0.917641 11.00000 0.01463 0.01313 = 0.03116 0.00254 -0.00942 0.00066 AFIX 23 H11A 2 0.701795 0.780081 0.937973 11.00000 -1.20000 H11B 2 0.804859 0.747413 0.867477 11.00000 -1.20000 AFIX 0 C6 1 -0.226184 1.074494 0.544139 11.00000 0.01175 0.03292 = 0.02731 0.01357 -0.00618 -0.00756 AFIX 23 H6A 2 -0.243732 1.144751 0.559866 11.00000 -1.20000 H6B 2 -0.230028 1.073867 0.490308 11.00000 -1.20000 AFIX 0 C7 1 -0.518271 1.076984 0.552081 11.00000 0.02187 0.02746 = 0.04181 0.01050 -0.00187 0.00214 AFIX 13 H7 2 -0.592872 1.037201 0.572252 11.00000 -1.20000 AFIX 0 C10 1 -0.558677 1.184142 0.583503 11.00000 0.03715 0.03772 = 0.04021 0.01919 0.00478 0.00663 AFIX 137 H10A 2 -0.553321 1.180701 0.636744 11.00000 -1.50000 H10B 2 -0.662687 1.215171 0.568443 11.00000 -1.50000 H10C 2 -0.485426 1.223926 0.565076 11.00000 -1.50000 AFIX 0 C16 1 1.002716 0.541867 0.926425 11.00000 0.02752 0.05673 = 0.03334 -0.02661 -0.00541 0.01088 AFIX 23 H16A 2 1.035139 0.472066 0.943194 11.00000 -1.20000 H16B 2 1.084083 0.558882 0.894374 11.00000 -1.20000 AFIX 0 C19 1 1.189400 0.493110 1.067822 11.00000 0.02724 0.03079 = 0.03099 0.00617 -0.00977 -0.00572 AFIX 23 H19A 2 1.132783 0.486657 1.113572 11.00000 -1.20000 H19B 2 1.163355 0.443917 1.033108 11.00000 -1.20000 AFIX 0 C28 1 1.596551 0.165754 -0.149232 11.00000 0.04138 0.03164 = 0.02884 -0.00438 0.01350 -0.01038 AFIX 23 H28A 2 1.549034 0.131299 -0.187650 11.00000 -1.20000 H28B 2 1.525161 0.228649 -0.138340 11.00000 -1.20000 AFIX 0 C18 1 1.128489 0.678714 1.096390 11.00000 0.03138 0.04061 = 0.03025 -0.01446 -0.01432 0.00798 AFIX 137 H18A 2 1.095167 0.745438 1.075454 11.00000 -1.50000 H18B 2 1.230449 0.673897 1.118101 11.00000 -1.50000 H18C 2 1.055466 0.666531 1.133958 11.00000 -1.50000 AFIX 0 C29 1 1.747836 0.190640 -0.178495 11.00000 0.05356 0.05282 = 0.05119 -0.01688 0.01002 -0.02110 AFIX 137 H29A 2 1.726736 0.233533 -0.221729 11.00000 -1.50000 H29B 2 1.817697 0.128951 -0.191414 11.00000 -1.50000 H29C 2 1.795370 0.225278 -0.140968 11.00000 -1.50000 AFIX 0 C9 1 -0.709204 1.107569 0.447221 11.00000 0.03586 0.03559 = 0.03587 0.00207 -0.00249 -0.00612 AFIX 137 H9A 2 -0.719316 1.116452 0.394364 11.00000 -1.50000 H9B 2 -0.757429 1.169154 0.471293 11.00000 -1.50000 H9C 2 -0.759810 1.053079 0.462950 11.00000 -1.50000 AFIX 0 C4 1 -0.330890 1.021390 0.657951 11.00000 0.04487 0.04551 = 0.04456 0.00002 0.00011 -0.00709 AFIX 23 H4A 2 -0.338727 1.090180 0.675905 11.00000 -1.20000 H4B 2 -0.414123 0.992608 0.680801 11.00000 -1.20000 AFIX 0 C2 1 -0.318182 0.914721 0.550741 11.00000 0.02696 0.02066 = 0.08371 0.01139 -0.02337 -0.00910 AFIX 23 H2A 2 -0.393559 0.879072 0.573778 11.00000 -1.20000 H2B 2 -0.331301 0.912275 0.497341 11.00000 -1.20000 AFIX 0 C8 1 -0.536330 1.082215 0.467938 11.00000 0.03153 0.03854 = 0.03466 0.01102 0.00177 0.00150 AFIX 23 H8A 2 -0.489043 1.017446 0.446702 11.00000 -1.20000 H8B 2 -0.482782 1.133879 0.447844 11.00000 -1.20000 AFIX 0 C38 1 -0.041975 0.546471 0.512231 11.00000 0.02965 0.04357 = 0.03114 -0.01129 0.02126 -0.00113 AFIX 137 H38A 2 -0.022834 0.475424 0.524851 11.00000 -1.50000 H38B 2 -0.144415 0.577612 0.529095 11.00000 -1.50000 H38C 2 0.035229 0.578307 0.535653 11.00000 -1.50000 AFIX 0 C42 1 0.637697 -0.198341 0.157466 11.00000 0.05299 0.03436 = 0.03160 -0.00548 0.00158 -0.01481 N11 5 0.567280 -0.186514 0.105073 11.00000 0.07192 0.04351 = 0.05512 -0.00977 -0.01387 -0.01044 N10 5 1.071449 0.324497 0.854003 11.00000 0.04442 0.06881 = 0.05373 -0.01096 0.00410 -0.00419 C48 1 1.128637 0.313984 0.801972 11.00000 0.04088 0.03276 = 0.07508 -0.01101 0.00283 -0.01164 C41 1 0.727900 -0.215310 0.223773 11.00000 0.07652 0.04747 = 0.04829 0.00808 -0.01893 -0.02497 AFIX 137 H41A 2 0.827165 -0.257757 0.213274 11.00000 -1.50000 H41B 2 0.672929 -0.248201 0.260100 11.00000 -1.50000 H41C 2 0.744491 -0.151425 0.242700 11.00000 -1.50000 AFIX 0 C47 1 1.225117 0.295468 0.734123 11.00000 0.08370 0.08530 = 0.05831 -0.02495 0.00360 -0.00978 AFIX 137 H47A 2 1.210936 0.356382 0.704371 11.00000 -1.50000 H47B 2 1.193678 0.241964 0.706234 11.00000 -1.50000 H47C 2 1.333448 0.276023 0.747663 11.00000 -1.50000 AFIX 0 C43 1 0.292901 -0.082886 0.270369 11.00000 0.06879 0.04718 = 0.07056 0.01259 0.01625 0.00068 AFIX 137 H43A 2 0.234423 -0.043715 0.231336 11.00000 -1.50000 H43B 2 0.402492 -0.082813 0.263659 11.00000 -1.50000 H43C 2 0.259547 -0.053562 0.317494 11.00000 -1.50000 AFIX 0 C45 1 0.827836 0.441877 0.689307 11.00000 0.09666 0.15020 = 0.05245 -0.02013 -0.02050 -0.01585 AFIX 137 H45A 2 0.783883 0.487520 0.650152 11.00000 -1.50000 H45B 2 0.923375 0.460153 0.706316 11.00000 -1.50000 H45C 2 0.754780 0.446220 0.729736 11.00000 -1.50000 AFIX 0 C44 1 0.267274 -0.181826 0.268373 11.00000 0.12444 0.03883 = 0.03111 0.01368 -0.00006 0.01910 C46 1 0.859524 0.341123 0.662323 11.00000 0.12617 0.12609 = 0.12599 -0.00133 -0.00008 -0.02323 N12 5 0.240702 -0.261800 0.271297 11.00000 0.26266 0.04009 = 0.04393 0.01341 0.00151 0.00236 N9 5 0.866091 0.257237 0.641918 11.00000 0.13210 0.12801 = 0.13006 -0.00327 -0.00154 -0.02412 HKLF 4 REM 71-b-100k_a.res in P1 REM R1 = 0.0355 for 12120 Fo > 4sig(Fo) and 0.0392 for all 12926 data REM 769 parameters refined using 32 restraints END WGHT 0.0356 0.0000 REM Highest difference peak 1.507, deepest hole -1.143, 1-sigma level 0.209 Q1 1 0.9231 -0.0777 0.3565 11.00000 0.05 1.51 Q2 1 0.0437 0.7760 0.7221 11.00000 0.05 1.50 Q3 1 0.4697 0.3957 0.8617 11.00000 0.05 1.48 Q4 1 1.0400 0.2866 0.2196 11.00000 0.05 1.48 Q5 1 0.8803 0.0367 0.0835 11.00000 0.05 1.40 Q6 1 0.4205 0.6182 0.6400 11.00000 0.05 1.37 Q7 1 0.5567 0.7826 0.7020 11.00000 0.05 1.35 Q8 1 0.2899 0.8650 0.9001 11.00000 0.05 1.35 Q9 1 0.7324 0.3799 0.4195 11.00000 0.05 1.33 Q10 1 0.3812 0.5596 0.5995 11.00000 0.05 1.32 Q11 1 0.4100 0.5387 0.8419 11.00000 0.05 1.30 Q12 1 0.8209 0.2425 0.4398 11.00000 0.05 1.30 Q13 1 0.7706 0.4263 0.2343 11.00000 0.05 1.28 Q14 1 0.2539 0.8780 0.5076 11.00000 0.05 1.24 Q15 1 0.2934 0.9185 0.7424 11.00000 0.05 1.23 Q16 1 0.3417 0.7426 0.5341 11.00000 0.05 1.20 Q17 1 0.2423 1.0572 0.7339 11.00000 0.05 1.20 Q18 1 0.8417 0.2371 0.0517 11.00000 0.05 1.20 Q19 1 0.6970 0.5618 0.2125 11.00000 0.05 1.17 Q20 1 0.8569 0.0631 0.3367 11.00000 0.05 1.16 REM The information below was added by Olex2. REM REM R1 = 0.0355 for 12120 Fo > 4sig(Fo) and 0.0392 for all 17610 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.51, deepest hole -1.14 REM Mean Shift 0, Max Shift 0.001. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0392 REM R1_gt = 0.0355 REM wR_ref = 0.0834 REM GOOF = 1.037 REM Shift_max = 0.001 REM Shift_mean = 0 REM Reflections_all = 17610 REM Reflections_gt = 12120 REM Parameters = n/a REM Hole = -1.14 REM Peak = 1.51 REM Flack = -0.00(3) ; _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.250 _oxdiff_exptl_absorpt_empirical_full_min 0.704