data_r20200519c _audit_creation_date 2020-06-01 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _shelx_SHELXL_version_number '2018/3' _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. (2008). Acta Cryst. A64, 112-122. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C28 H44 N2 O2' _chemical_formula_sum 'C28 H44 N2 O2' _chemical_formula_weight 440.65 _chemical_absolute_configuration ad _chemical_melting_point ? _chemical_oxdiff_formula 'C11 H10 N O' 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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 '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 'orthorhombic' _space_group_IT_number 19 _space_group_name_H-M_alt 'P 21 21 21' _space_group_name_Hall 'P 2ac 2ab' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 9.7732(4) _cell_length_b 14.8171(7) _cell_length_c 18.3308(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 2654.49(19) _cell_formula_units_Z 4 _cell_measurement_reflns_used 15392 _cell_measurement_temperature 113(2) _cell_measurement_theta_max 32.9000 _cell_measurement_theta_min 2.5310 _shelx_estimated_absorpt_T_max 0.989 _shelx_estimated_absorpt_T_min 0.986 _exptl_absorpt_coefficient_mu 0.068 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.59805 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'CrysAlisPro 1.171.38.46 (Rigaku Oxford Diffraction, 2015)' _exptl_absorpt_special_details ? _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.103 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 968 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0490 _diffrn_reflns_av_unetI/netI 0.0370 _diffrn_reflns_Laue_measured_fraction_full 0.985 _diffrn_reflns_Laue_measured_fraction_max 0.987 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 22958 _diffrn_reflns_point_group_measured_fraction_full 0.989 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.371 _diffrn_reflns_theta_min 3.451 _diffrn_ambient_temperature 113.15 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.987 _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 -115.00 65.00 1.00 2.00 -- -25.00 45.00 0.00 180 2 \w -115.00 35.00 1.00 2.00 -- -25.00 45.00 90.00 150 3 \w -115.00 5.00 1.00 2.00 -- -25.00 45.00 180.00 120 ; _diffrn_measurement_device 'abstract diffractometer' _diffrn_measurement_device_type 'Rigaku Saturn 70 CCD' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0670638000 _diffrn_orient_matrix_UB_12 0.0097811000 _diffrn_orient_matrix_UB_13 -0.0125292000 _diffrn_orient_matrix_UB_21 0.0257160000 _diffrn_orient_matrix_UB_22 -0.0063685000 _diffrn_orient_matrix_UB_23 0.0358126000 _diffrn_orient_matrix_UB_31 0.0104676000 _diffrn_orient_matrix_UB_32 -0.0464224000 _diffrn_orient_matrix_UB_33 -0.0075909000 _diffrn_radiation_monochromator confocal _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'rotating anode' _diffrn_source_type 'Enhance (Mo) X-ray Source' _reflns_Friedel_coverage 0.776 _reflns_Friedel_fraction_full 0.995 _reflns_Friedel_fraction_max 0.995 _reflns_number_gt 4871 _reflns_number_total 5364 _reflns_odcompleteness_completeness 99.00 _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 1.171.38.46 (Rigaku OD, 2015)' _computing_data_collection CrystalClear(Rigaku,2008) _computing_data_reduction 'CrysAlisPro 1.171.38.46 (Rigaku OD, 2015)' _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 'XS (Sheldrick, 2008)' _refine_diff_density_max 0.167 _refine_diff_density_min -0.169 _refine_diff_density_rms 0.029 _refine_ls_abs_structure_details ; Flack x determined using 1958 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack -0.4(5) _refine_ls_extinction_coef 0.034(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_extinction_method 'SHELXL-2018/3 (Sheldrick 2018)' _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 297 _refine_ls_number_reflns 5364 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0433 _refine_ls_R_factor_gt 0.0378 _refine_ls_restrained_S_all 1.026 _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^)+(0.0454P)^2^+0.3621P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0877 _refine_ls_wR_factor_ref 0.0907 _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.a Ternary CH refined with riding coordinates: C11(H11) 2.b Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C18(H18A,H18B), C23(H23A, H23B), C24(H24A,H24B), C26(H26A,H26B), C27(H27A,H27B) 2.c Aromatic/amide H refined with riding coordinates: C6(H6), C7(H7), C9(H9), C10(H10) 2.d Idealised Me refined as rotating group: C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C20(H20A,H20B,H20C), C21(H21A,H21B, H21C), C22(H22A,H22B,H22C), C25(H25A,H25B,H25C), C28(H28A,H28B,H28C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _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 O1 O 0.95032(16) 1.04252(11) 0.29598(8) 0.0384(4) Uani 1 1 d . . . . . O2 O 0.01391(13) 0.96751(10) -0.00378(8) 0.0302(3) Uani 1 1 d . . . . . N1 N 0.76576(17) 1.06861(12) 0.17649(9) 0.0256(4) Uani 1 1 d . . . . . N2 N 0.24715(15) 0.95810(11) -0.02578(8) 0.0198(3) Uani 1 1 d . . . . . C1 C 0.8901(2) 1.01463(16) 0.16913(13) 0.0352(5) Uani 1 1 d . . . . . H1A H 0.925769 1.020076 0.118765 0.042 Uiso 1 1 calc R . . . . H1B H 0.868579 0.950329 0.178231 0.042 Uiso 1 1 calc R . . . . C2 C 0.9979(2) 1.04590(17) 0.22256(12) 0.0368(5) Uani 1 1 d . . . . . H2A H 1.080042 1.007222 0.217707 0.044 Uiso 1 1 calc R . . . . H2B H 1.024890 1.108582 0.210588 0.044 Uiso 1 1 calc R . . . . C3 C 0.8326(2) 1.09829(17) 0.30268(12) 0.0370(5) Uani 1 1 d . . . . . H3A H 0.858156 1.161469 0.291549 0.044 Uiso 1 1 calc R . . . . H3B H 0.799492 1.096192 0.353687 0.044 Uiso 1 1 calc R . . . . C4 C 0.7183(2) 1.06932(17) 0.25212(11) 0.0333(5) Uani 1 1 d . . . . . H4A H 0.686529 1.008225 0.265906 0.040 Uiso 1 1 calc R . . . . H4B H 0.640228 1.111426 0.257017 0.040 Uiso 1 1 calc R . . . . C5 C 0.66488(19) 1.05575(13) 0.12188(10) 0.0232(4) Uani 1 1 d . . . . . C6 C 0.5255(2) 1.05848(15) 0.13828(11) 0.0302(5) Uani 1 1 d . . . . . H6 H 0.497194 1.067325 0.187351 0.036 Uiso 1 1 calc R . . . . C7 C 0.4274(2) 1.04848(15) 0.08404(10) 0.0297(5) Uani 1 1 d . . . . . H7 H 0.333228 1.051135 0.096752 0.036 Uiso 1 1 calc R . . . . C8 C 0.46353(18) 1.03478(13) 0.01212(10) 0.0214(4) Uani 1 1 d . . . . . C9 C 0.60201(19) 1.03255(14) -0.00436(10) 0.0253(4) Uani 1 1 d . . . . . H9 H 0.629456 1.023723 -0.053564 0.030 Uiso 1 1 calc R . . . . C10 C 0.7016(2) 1.04286(15) 0.04892(10) 0.0280(5) Uani 1 1 d . . . . . H10 H 0.795516 1.041136 0.035712 0.034 Uiso 1 1 calc R . . . . C11 C 0.35588(18) 1.02114(13) -0.04706(10) 0.0198(4) Uani 1 1 d . . . . . H11 H 0.400712 0.999631 -0.092912 0.024 Uiso 1 1 calc R . . . . C12 C 0.12373(19) 1.00110(14) -0.02263(10) 0.0226(4) Uani 1 1 d . . . . . C13 C 0.14551(19) 1.09607(14) -0.04643(10) 0.0227(4) Uani 1 1 d . . . . . C14 C 0.27785(19) 1.10754(13) -0.06200(10) 0.0218(4) Uani 1 1 d . . . . . C15 C 0.2654(2) 0.85949(13) -0.01345(10) 0.0240(4) Uani 1 1 d . . . . . C16 C 0.4163(2) 0.83386(15) -0.02137(12) 0.0319(5) Uani 1 1 d . . . . . H16A H 0.451705 0.857657 -0.067528 0.048 Uiso 1 1 calc GR . . . . H16B H 0.425276 0.767990 -0.020944 0.048 Uiso 1 1 calc GR . . . . H16C H 0.468451 0.859505 0.019304 0.048 Uiso 1 1 calc GR . . . . C17 C 0.2224(2) 0.83802(17) 0.06558(11) 0.0367(5) Uani 1 1 d . . . . . H17A H 0.278431 0.873367 0.099483 0.055 Uiso 1 1 calc GR . . . . H17B H 0.235686 0.773546 0.075151 0.055 Uiso 1 1 calc GR . . . . H17C H 0.125745 0.853512 0.072330 0.055 Uiso 1 1 calc GR . . . . C18 C 0.1722(2) 0.80360(14) -0.06440(10) 0.0252(4) Uani 1 1 d . . . . . H18A H 0.077260 0.823594 -0.054647 0.030 Uiso 1 1 calc R . . . . H18B H 0.178291 0.740273 -0.047495 0.030 Uiso 1 1 calc R . . . . C19 C 0.1885(2) 0.80118(14) -0.14831(11) 0.0281(5) Uani 1 1 d . . . . . C20 C 0.3214(3) 0.75580(19) -0.17347(14) 0.0460(6) Uani 1 1 d . . . . . H20A H 0.398647 0.796636 -0.164879 0.069 Uiso 1 1 calc GR . . . . H20B H 0.315284 0.741940 -0.225639 0.069 Uiso 1 1 calc GR . . . . H20C H 0.335296 0.699832 -0.145956 0.069 Uiso 1 1 calc GR . . . . C21 C 0.0684(3) 0.74388(18) -0.17628(14) 0.0463(6) Uani 1 1 d . . . . . H21A H 0.076398 0.682346 -0.157150 0.069 Uiso 1 1 calc GR . . . . H21B H 0.070161 0.742252 -0.229716 0.069 Uiso 1 1 calc GR . . . . H21C H -0.018082 0.770499 -0.159809 0.069 Uiso 1 1 calc GR . . . . C22 C 0.1793(2) 0.89454(15) -0.18293(11) 0.0308(5) Uani 1 1 d . . . . . H22A H 0.094300 0.923980 -0.167456 0.046 Uiso 1 1 calc GR . . . . H22B H 0.179895 0.888640 -0.236181 0.046 Uiso 1 1 calc GR . . . . H22C H 0.257700 0.931011 -0.167420 0.046 Uiso 1 1 calc GR . . . . C23 C 0.0277(2) 1.15997(14) -0.05079(12) 0.0296(5) Uani 1 1 d . . . . . H23A H 0.063171 1.221429 -0.060349 0.035 Uiso 1 1 calc R . . . . H23B H -0.019512 1.161107 -0.003024 0.035 Uiso 1 1 calc R . . . . C24 C -0.0764(2) 1.13563(15) -0.11023(12) 0.0326(5) Uani 1 1 d . . . . . H24A H -0.030482 1.136721 -0.158353 0.039 Uiso 1 1 calc R . . . . H24B H -0.110223 1.073523 -0.101724 0.039 Uiso 1 1 calc R . . . . C25 C -0.1977(2) 1.20037(17) -0.11154(14) 0.0416(6) Uani 1 1 d . . . . . H25A H -0.262868 1.181130 -0.149055 0.062 Uiso 1 1 calc GR . . . . H25B H -0.165269 1.261450 -0.122617 0.062 Uiso 1 1 calc GR . . . . H25C H -0.242752 1.200158 -0.063790 0.062 Uiso 1 1 calc GR . . . . C26 C 0.3514(2) 1.18863(14) -0.09002(11) 0.0276(5) Uani 1 1 d . . . . . H26A H 0.431966 1.200317 -0.058712 0.033 Uiso 1 1 calc R . . . . H26B H 0.290018 1.241618 -0.086467 0.033 Uiso 1 1 calc R . . . . C27 C 0.3991(2) 1.17844(15) -0.16933(12) 0.0326(5) Uani 1 1 d . . . . . H27A H 0.452074 1.232663 -0.183405 0.039 Uiso 1 1 calc R . . . . H27B H 0.460762 1.125621 -0.172935 0.039 Uiso 1 1 calc R . . . . C28 C 0.2812(3) 1.16634(18) -0.22234(12) 0.0421(6) Uani 1 1 d . . . . . H28A H 0.316547 1.164976 -0.272350 0.063 Uiso 1 1 calc GR . . . . H28B H 0.216969 1.216733 -0.217097 0.063 Uiso 1 1 calc GR . . . . H28C H 0.233862 1.109504 -0.211788 0.063 Uiso 1 1 calc GR . . . . 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 O1 0.0407(9) 0.0417(9) 0.0326(8) 0.0015(7) -0.0167(7) 0.0078(8) O2 0.0170(7) 0.0423(8) 0.0314(7) 0.0026(6) 0.0065(6) 0.0009(6) N1 0.0217(8) 0.0343(9) 0.0209(8) -0.0010(7) -0.0051(7) 0.0003(7) N2 0.0149(7) 0.0259(8) 0.0187(7) 0.0009(6) 0.0004(6) -0.0001(6) C1 0.0293(11) 0.0398(13) 0.0365(12) -0.0099(10) -0.0112(9) 0.0093(10) C2 0.0286(11) 0.0432(13) 0.0387(12) -0.0030(10) -0.0127(9) 0.0080(10) C3 0.0385(13) 0.0448(13) 0.0276(11) -0.0018(10) -0.0112(9) 0.0049(11) C4 0.0322(11) 0.0449(13) 0.0229(10) -0.0006(9) -0.0050(9) -0.0021(10) C5 0.0208(9) 0.0261(11) 0.0227(9) 0.0000(8) -0.0045(7) -0.0011(8) C6 0.0236(10) 0.0486(13) 0.0185(9) -0.0084(9) 0.0001(8) 0.0008(10) C7 0.0159(9) 0.0491(13) 0.0240(9) -0.0055(9) -0.0006(8) 0.0028(9) C8 0.0181(9) 0.0254(10) 0.0207(9) -0.0019(8) -0.0019(7) 0.0005(8) C9 0.0201(9) 0.0382(11) 0.0177(9) -0.0008(8) 0.0018(7) -0.0021(8) C10 0.0149(9) 0.0443(13) 0.0250(9) 0.0001(9) 0.0012(7) -0.0020(9) C11 0.0159(9) 0.0275(10) 0.0159(8) -0.0015(7) -0.0006(7) -0.0018(8) C12 0.0176(9) 0.0333(11) 0.0168(8) -0.0022(8) -0.0004(7) 0.0016(8) C13 0.0221(10) 0.0274(10) 0.0186(9) -0.0057(8) -0.0036(7) 0.0032(8) C14 0.0237(10) 0.0253(10) 0.0163(8) -0.0051(7) -0.0041(7) 0.0019(8) C15 0.0224(9) 0.0260(10) 0.0235(10) 0.0065(8) -0.0019(8) -0.0009(8) C16 0.0230(10) 0.0278(11) 0.0447(12) 0.0055(9) -0.0085(10) 0.0044(9) C17 0.0418(13) 0.0452(13) 0.0230(10) 0.0121(9) -0.0027(9) -0.0050(11) C18 0.0235(10) 0.0250(10) 0.0271(10) 0.0055(8) 0.0021(8) -0.0029(8) C19 0.0265(11) 0.0300(11) 0.0277(10) -0.0025(8) 0.0010(8) -0.0056(9) C20 0.0455(15) 0.0498(15) 0.0425(14) -0.0088(12) 0.0104(12) 0.0088(12) C21 0.0501(15) 0.0492(15) 0.0396(13) -0.0068(11) -0.0013(12) -0.0227(13) C22 0.0333(11) 0.0379(12) 0.0211(9) 0.0017(9) -0.0048(9) -0.0051(9) C23 0.0248(10) 0.0312(11) 0.0326(11) -0.0057(9) -0.0017(9) 0.0072(9) C24 0.0261(10) 0.0413(12) 0.0302(11) 0.0005(9) -0.0036(9) 0.0072(10) C25 0.0277(12) 0.0493(15) 0.0476(14) 0.0115(11) -0.0013(10) 0.0094(11) C26 0.0293(11) 0.0238(11) 0.0297(10) -0.0025(8) -0.0072(8) -0.0025(9) C27 0.0337(12) 0.0278(11) 0.0361(12) 0.0067(9) 0.0045(9) -0.0025(10) C28 0.0563(15) 0.0427(13) 0.0273(11) 0.0076(10) -0.0047(11) -0.0081(12) _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 O1 C2 1.425(3) . ? O1 C3 1.422(3) . ? O2 C12 1.233(2) . ? N1 C1 1.461(3) . ? N1 C4 1.462(3) . ? N1 C5 1.418(2) . ? N2 C11 1.468(2) . ? N2 C12 1.365(2) . ? N2 C15 1.489(2) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C1 C2 1.511(3) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.513(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.396(3) . ? C5 C10 1.398(3) . ? C6 H6 0.9500 . ? C6 C7 1.389(3) . ? C7 H7 0.9500 . ? C7 C8 1.380(3) . ? C8 C9 1.387(3) . ? C8 C11 1.525(2) . ? C9 H9 0.9500 . ? C9 C10 1.387(3) . ? C10 H10 0.9500 . ? C11 H11 1.0000 . ? C11 C14 1.515(3) . ? C12 C13 1.489(3) . ? C13 C14 1.335(3) . ? C13 C23 1.493(3) . ? C14 C26 1.491(3) . ? C15 C16 1.529(3) . ? C15 C17 1.542(3) . ? C15 C18 1.546(3) . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C18 C19 1.547(3) . ? C19 C20 1.534(3) . ? C19 C21 1.537(3) . ? C19 C22 1.525(3) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 C24 1.534(3) . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C24 C25 1.525(3) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C26 C27 1.534(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C27 C28 1.518(3) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? 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 C3 O1 C2 108.99(15) . . ? C1 N1 C4 110.80(16) . . ? C5 N1 C1 116.08(16) . . ? C5 N1 C4 116.76(16) . . ? C11 N2 C15 125.30(15) . . ? C12 N2 C11 110.73(15) . . ? C12 N2 C15 123.87(15) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? N1 C1 C2 110.63(17) . . ? H1A C1 H1B 108.1 . . ? C2 C1 H1A 109.5 . . ? C2 C1 H1B 109.5 . . ? O1 C2 C1 111.93(19) . . ? O1 C2 H2A 109.2 . . ? O1 C2 H2B 109.2 . . ? C1 C2 H2A 109.2 . . ? C1 C2 H2B 109.2 . . ? H2A C2 H2B 107.9 . . ? O1 C3 H3A 109.1 . . ? O1 C3 H3B 109.1 . . ? O1 C3 C4 112.29(19) . . ? H3A C3 H3B 107.9 . . ? C4 C3 H3A 109.1 . . ? C4 C3 H3B 109.1 . . ? N1 C4 C3 110.42(18) . . ? N1 C4 H4A 109.6 . . ? N1 C4 H4B 109.6 . . ? C3 C4 H4A 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? C6 C5 N1 121.52(17) . . ? C6 C5 C10 117.41(17) . . ? C10 C5 N1 121.04(17) . . ? C5 C6 H6 119.5 . . ? C7 C6 C5 121.09(18) . . ? C7 C6 H6 119.5 . . ? C6 C7 H7 119.2 . . ? C8 C7 C6 121.53(18) . . ? C8 C7 H7 119.2 . . ? C7 C8 C9 117.48(17) . . ? C7 C8 C11 121.51(16) . . ? C9 C8 C11 121.00(16) . . ? C8 C9 H9 119.1 . . ? C8 C9 C10 121.89(17) . . ? C10 C9 H9 119.1 . . ? C5 C10 H10 119.7 . . ? C9 C10 C5 120.59(17) . . ? C9 C10 H10 119.7 . . ? N2 C11 C8 113.25(15) . . ? N2 C11 H11 109.7 . . ? N2 C11 C14 102.79(14) . . ? C8 C11 H11 109.7 . . ? C14 C11 C8 111.34(15) . . ? C14 C11 H11 109.7 . . ? O2 C12 N2 126.35(18) . . ? O2 C12 C13 126.05(18) . . ? N2 C12 C13 107.60(16) . . ? C12 C13 C23 120.33(18) . . ? C14 C13 C12 108.75(17) . . ? C14 C13 C23 130.9(2) . . ? C13 C14 C11 109.96(18) . . ? C13 C14 C26 130.00(19) . . ? C26 C14 C11 120.04(17) . . ? N2 C15 C16 110.18(16) . . ? N2 C15 C17 108.20(16) . . ? N2 C15 C18 111.31(15) . . ? C16 C15 C17 107.51(17) . . ? C16 C15 C18 112.22(17) . . ? C17 C15 C18 107.24(16) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16B 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C15 C18 H18A 106.4 . . ? C15 C18 H18B 106.4 . . ? C15 C18 C19 123.54(16) . . ? H18A C18 H18B 106.5 . . ? C19 C18 H18A 106.4 . . ? C19 C18 H18B 106.4 . . ? C20 C19 C18 113.35(18) . . ? C20 C19 C21 107.73(19) . . ? C21 C19 C18 105.42(17) . . ? C22 C19 C18 112.76(16) . . ? C22 C19 C20 108.82(18) . . ? C22 C19 C21 108.50(18) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C13 C23 H23A 108.8 . . ? C13 C23 H23B 108.8 . . ? C13 C23 C24 113.62(17) . . ? H23A C23 H23B 107.7 . . ? C24 C23 H23A 108.8 . . ? C24 C23 H23B 108.8 . . ? C23 C24 H24A 109.2 . . ? C23 C24 H24B 109.2 . . ? H24A C24 H24B 107.9 . . ? C25 C24 C23 112.26(18) . . ? C25 C24 H24A 109.2 . . ? C25 C24 H24B 109.2 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C14 C26 H26A 108.9 . . ? C14 C26 H26B 108.9 . . ? C14 C26 C27 113.18(16) . . ? H26A C26 H26B 107.8 . . ? C27 C26 H26A 108.9 . . ? C27 C26 H26B 108.9 . . ? C26 C27 H27A 109.0 . . ? C26 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? C28 C27 C26 112.78(18) . . ? C28 C27 H27A 109.0 . . ? C28 C27 H27B 109.0 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C3 C4 N1 -56.8(3) . . . . ? O2 C12 C13 C14 179.56(18) . . . . ? O2 C12 C13 C23 -1.5(3) . . . . ? N1 C1 C2 O1 57.1(3) . . . . ? N1 C5 C6 C7 178.06(19) . . . . ? N1 C5 C10 C9 -178.40(19) . . . . ? N2 C11 C14 C13 3.7(2) . . . . ? N2 C11 C14 C26 -176.26(15) . . . . ? N2 C12 C13 C14 -0.7(2) . . . . ? N2 C12 C13 C23 178.31(16) . . . . ? N2 C15 C18 C19 65.9(2) . . . . ? C1 N1 C4 C3 53.1(2) . . . . ? C1 N1 C5 C6 143.8(2) . . . . ? C1 N1 C5 C10 -38.4(3) . . . . ? C2 O1 C3 C4 59.0(2) . . . . ? C3 O1 C2 C1 -59.0(2) . . . . ? C4 N1 C1 C2 -53.4(2) . . . . ? C4 N1 C5 C6 10.2(3) . . . . ? C4 N1 C5 C10 -172.00(19) . . . . ? C5 N1 C1 C2 170.32(18) . . . . ? C5 N1 C4 C3 -170.99(18) . . . . ? C5 C6 C7 C8 0.5(4) . . . . ? C6 C5 C10 C9 -0.5(3) . . . . ? C6 C7 C8 C9 -0.9(3) . . . . ? C6 C7 C8 C11 178.2(2) . . . . ? C7 C8 C9 C10 0.5(3) . . . . ? C7 C8 C11 N2 -45.2(3) . . . . ? C7 C8 C11 C14 70.1(2) . . . . ? C8 C9 C10 C5 0.2(3) . . . . ? C8 C11 C14 C13 -117.84(17) . . . . ? C8 C11 C14 C26 62.2(2) . . . . ? C9 C8 C11 N2 133.88(19) . . . . ? C9 C8 C11 C14 -110.9(2) . . . . ? C10 C5 C6 C7 0.2(3) . . . . ? C11 N2 C12 O2 -177.07(18) . . . . ? C11 N2 C12 C13 3.15(19) . . . . ? C11 N2 C15 C16 3.6(2) . . . . ? C11 N2 C15 C17 120.90(18) . . . . ? C11 N2 C15 C18 -121.51(18) . . . . ? C11 C8 C9 C10 -178.58(19) . . . . ? C11 C14 C26 C27 70.8(2) . . . . ? C12 N2 C11 C8 116.10(17) . . . . ? C12 N2 C11 C14 -4.15(18) . . . . ? C12 N2 C15 C16 179.76(16) . . . . ? C12 N2 C15 C17 -63.0(2) . . . . ? C12 N2 C15 C18 54.6(2) . . . . ? C12 C13 C14 C11 -2.0(2) . . . . ? C12 C13 C14 C26 177.97(18) . . . . ? C12 C13 C23 C24 -66.8(2) . . . . ? C13 C14 C26 C27 -109.2(2) . . . . ? C13 C23 C24 C25 178.10(18) . . . . ? C14 C13 C23 C24 111.9(2) . . . . ? C14 C26 C27 C28 62.4(2) . . . . ? C15 N2 C11 C8 -67.3(2) . . . . ? C15 N2 C11 C14 172.41(15) . . . . ? C15 N2 C12 O2 6.3(3) . . . . ? C15 N2 C12 C13 -173.46(15) . . . . ? C15 C18 C19 C20 66.8(3) . . . . ? C15 C18 C19 C21 -175.65(19) . . . . ? C15 C18 C19 C22 -57.4(3) . . . . ? C16 C15 C18 C19 -58.1(3) . . . . ? C17 C15 C18 C19 -175.89(19) . . . . ? C23 C13 C14 C11 179.16(18) . . . . ? C23 C13 C14 C26 -0.9(4) . . . . ? _shelx_res_file ; TITL r20200519c in P212121 #19 r20200519c.res created by SHELXL-2018/3 at 16:37:27 on 01-Jun-2020 REM reset to P212121 #19 CELL 0.71073 9.7732 14.8171 18.3308 90 90 90 ZERR 4 0.0004 0.0007 0.0006 0 0 0 LATT -1 SYMM 0.5-X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,-Z SYMM -X,0.5+Y,0.5-Z SFAC C H N O UNIT 112 176 8 8 L.S. 4 PLAN 20 SIZE 0.2 0.18 0.16 TEMP -160 conf htab bond $h fmap 2 acta OMIT 0 1 1 OMIT 1 0 2 OMIT 1 1 2 OMIT 0 0 2 OMIT 0 1 2 OMIT 1 2 1 OMIT 0 2 0 OMIT 0 2 2 OMIT 0 2 1 OMIT 1 1 1 OMIT 1 1 0 OMIT -1 1 2 OMIT -1 1 1 OMIT 1 0 1 OMIT -1 2 1 REM REM REM WGHT 0.045400 0.362100 EXTI 0.034207 FVAR 1.44728 O1 4 0.950317 1.042516 0.295977 11.00000 0.04074 0.04172 = 0.03262 0.00151 -0.01669 0.00785 O2 4 0.013914 0.967507 -0.003778 11.00000 0.01698 0.04226 = 0.03141 0.00263 0.00648 0.00089 N1 3 0.765757 1.068607 0.176488 11.00000 0.02169 0.03433 = 0.02093 -0.00100 -0.00506 0.00031 N2 3 0.247153 0.958102 -0.025775 11.00000 0.01494 0.02590 = 0.01867 0.00088 0.00037 -0.00005 C1 1 0.890135 1.014635 0.169129 11.00000 0.02929 0.03982 = 0.03648 -0.00987 -0.01116 0.00926 AFIX 23 H1A 2 0.925769 1.020076 0.118765 11.00000 -1.20000 H1B 2 0.868579 0.950329 0.178231 11.00000 -1.20000 AFIX 0 C2 1 0.997947 1.045900 0.222562 11.00000 0.02860 0.04322 = 0.03873 -0.00296 -0.01275 0.00801 AFIX 23 H2A 2 1.080042 1.007222 0.217707 11.00000 -1.20000 H2B 2 1.024890 1.108582 0.210588 11.00000 -1.20000 AFIX 0 C3 1 0.832628 1.098294 0.302679 11.00000 0.03853 0.04484 = 0.02755 -0.00177 -0.01119 0.00489 AFIX 23 H3A 2 0.858156 1.161469 0.291549 11.00000 -1.20000 H3B 2 0.799492 1.096192 0.353687 11.00000 -1.20000 AFIX 0 C4 1 0.718347 1.069324 0.252124 11.00000 0.03222 0.04491 = 0.02289 -0.00060 -0.00500 -0.00208 AFIX 23 H4A 2 0.686529 1.008225 0.265906 11.00000 -1.20000 H4B 2 0.640228 1.111426 0.257017 11.00000 -1.20000 AFIX 0 C5 1 0.664885 1.055749 0.121880 11.00000 0.02077 0.02607 = 0.02270 0.00000 -0.00455 -0.00115 C6 1 0.525460 1.058481 0.138283 11.00000 0.02357 0.04856 = 0.01853 -0.00839 0.00011 0.00081 AFIX 43 H6 2 0.497194 1.067325 0.187351 11.00000 -1.20000 AFIX 0 C7 1 0.427378 1.048479 0.084041 11.00000 0.01593 0.04907 = 0.02401 -0.00551 -0.00057 0.00285 AFIX 43 H7 2 0.333228 1.051135 0.096752 11.00000 -1.20000 AFIX 0 C8 1 0.463528 1.034776 0.012123 11.00000 0.01806 0.02541 = 0.02067 -0.00193 -0.00189 0.00045 C9 1 0.602007 1.032555 -0.004363 11.00000 0.02011 0.03817 = 0.01767 -0.00081 0.00183 -0.00211 AFIX 43 H9 2 0.629456 1.023723 -0.053564 11.00000 -1.20000 AFIX 0 C10 1 0.701560 1.042858 0.048925 11.00000 0.01486 0.04432 = 0.02497 0.00007 0.00116 -0.00204 AFIX 43 H10 2 0.795516 1.041136 0.035712 11.00000 -1.20000 AFIX 0 C11 1 0.355876 1.021138 -0.047060 11.00000 0.01586 0.02750 = 0.01593 -0.00146 -0.00056 -0.00178 AFIX 13 H11 2 0.400712 0.999631 -0.092912 11.00000 -1.20000 AFIX 0 C12 1 0.123730 1.001100 -0.022631 11.00000 0.01756 0.03331 = 0.01678 -0.00217 -0.00036 0.00162 C13 1 0.145512 1.096071 -0.046427 11.00000 0.02212 0.02737 = 0.01858 -0.00566 -0.00360 0.00318 C14 1 0.277849 1.107540 -0.062000 11.00000 0.02373 0.02534 = 0.01634 -0.00515 -0.00413 0.00189 C15 1 0.265429 0.859492 -0.013454 11.00000 0.02237 0.02604 = 0.02347 0.00650 -0.00195 -0.00092 C16 1 0.416256 0.833860 -0.021366 11.00000 0.02303 0.02779 = 0.04474 0.00553 -0.00854 0.00442 AFIX 137 H16A 2 0.451705 0.857657 -0.067528 11.00000 -1.50000 H16B 2 0.425276 0.767990 -0.020944 11.00000 -1.50000 H16C 2 0.468451 0.859505 0.019304 11.00000 -1.50000 AFIX 0 C17 1 0.222404 0.838024 0.065575 11.00000 0.04177 0.04524 = 0.02305 0.01207 -0.00270 -0.00503 AFIX 137 H17A 2 0.278431 0.873367 0.099483 11.00000 -1.50000 H17B 2 0.235686 0.773546 0.075151 11.00000 -1.50000 H17C 2 0.125745 0.853512 0.072330 11.00000 -1.50000 AFIX 0 C18 1 0.172169 0.803601 -0.064400 11.00000 0.02346 0.02503 = 0.02708 0.00550 0.00210 -0.00288 AFIX 23 H18A 2 0.077260 0.823594 -0.054647 11.00000 -1.20000 H18B 2 0.178291 0.740273 -0.047495 11.00000 -1.20000 AFIX 0 C19 1 0.188477 0.801181 -0.148306 11.00000 0.02651 0.02996 = 0.02771 -0.00249 0.00101 -0.00563 C20 1 0.321430 0.755800 -0.173467 11.00000 0.04554 0.04980 = 0.04253 -0.00884 0.01038 0.00877 AFIX 137 H20A 2 0.398647 0.796636 -0.164879 11.00000 -1.50000 H20B 2 0.315284 0.741940 -0.225639 11.00000 -1.50000 H20C 2 0.335296 0.699832 -0.145956 11.00000 -1.50000 AFIX 0 C21 1 0.068357 0.743879 -0.176279 11.00000 0.05006 0.04920 = 0.03963 -0.00677 -0.00135 -0.02273 AFIX 137 H21A 2 0.076398 0.682346 -0.157150 11.00000 -1.50000 H21B 2 0.070161 0.742252 -0.229716 11.00000 -1.50000 H21C 2 -0.018082 0.770499 -0.159809 11.00000 -1.50000 AFIX 0 C22 1 0.179271 0.894541 -0.182933 11.00000 0.03332 0.03794 = 0.02109 0.00168 -0.00484 -0.00508 AFIX 137 H22A 2 0.094300 0.923980 -0.167456 11.00000 -1.50000 H22B 2 0.179895 0.888640 -0.236181 11.00000 -1.50000 H22C 2 0.257700 0.931011 -0.167420 11.00000 -1.50000 AFIX 0 C23 1 0.027711 1.159968 -0.050795 11.00000 0.02485 0.03120 = 0.03264 -0.00574 -0.00165 0.00724 AFIX 23 H23A 2 0.063171 1.221429 -0.060349 11.00000 -1.20000 H23B 2 -0.019512 1.161107 -0.003024 11.00000 -1.20000 AFIX 0 C24 1 -0.076428 1.135625 -0.110228 11.00000 0.02610 0.04133 = 0.03023 0.00053 -0.00362 0.00716 AFIX 23 H24A 2 -0.030482 1.136721 -0.158353 11.00000 -1.20000 H24B 2 -0.110223 1.073523 -0.101724 11.00000 -1.20000 AFIX 0 C25 1 -0.197656 1.200374 -0.111540 11.00000 0.02774 0.04932 = 0.04762 0.01149 -0.00133 0.00943 AFIX 137 H25A 2 -0.262868 1.181130 -0.149055 11.00000 -1.50000 H25B 2 -0.165269 1.261450 -0.122617 11.00000 -1.50000 H25C 2 -0.242752 1.200158 -0.063790 11.00000 -1.50000 AFIX 0 C26 1 0.351357 1.188628 -0.090025 11.00000 0.02929 0.02377 = 0.02968 -0.00246 -0.00719 -0.00246 AFIX 23 H26A 2 0.431966 1.200317 -0.058712 11.00000 -1.20000 H26B 2 0.290018 1.241618 -0.086467 11.00000 -1.20000 AFIX 0 C27 1 0.399095 1.178441 -0.169332 11.00000 0.03374 0.02782 = 0.03614 0.00672 0.00447 -0.00245 AFIX 23 H27A 2 0.452074 1.232663 -0.183405 11.00000 -1.20000 H27B 2 0.460762 1.125621 -0.172935 11.00000 -1.20000 AFIX 0 C28 1 0.281169 1.166341 -0.222339 11.00000 0.05632 0.04271 = 0.02735 0.00763 -0.00470 -0.00814 AFIX 137 H28A 2 0.316547 1.164976 -0.272350 11.00000 -1.50000 H28B 2 0.216969 1.216733 -0.217097 11.00000 -1.50000 H28C 2 0.233862 1.109504 -0.211788 11.00000 -1.50000 AFIX 0 HKLF 4 REM r20200519c in P212121 #19 REM wR2 = 0.0907, GooF = S = 1.026, Restrained GooF = 1.026 for all data REM R1 = 0.0378 for 4871 Fo > 4sig(Fo) and 0.0433 for all 5364 data REM 297 parameters refined using 0 restraints END WGHT 0.0454 0.3621 REM Instructions for potential hydrogen bonds EQIV $1 x+1, y, z HTAB C1 O2_$1 HTAB C10 O2_$1 EQIV $2 -x+3/2, -y+2, z-1/2 HTAB C11 O1_$2 HTAB C17 O2 HTAB C18 O2 REM Highest difference peak 0.167, deepest hole -0.169, 1-sigma level 0.029 Q1 1 0.6910 1.0172 0.0919 11.00000 0.05 0.17 Q2 1 0.6520 1.0011 0.0252 11.00000 0.05 0.16 Q3 1 0.2202 1.1057 -0.0244 11.00000 0.05 0.16 Q4 1 0.4105 1.0320 -0.0181 11.00000 0.05 0.16 Q5 1 0.5232 1.0054 0.0035 11.00000 0.05 0.15 Q6 1 0.2006 0.8069 -0.1088 11.00000 0.05 0.14 Q7 1 0.7432 1.0849 0.2139 11.00000 0.05 0.13 Q8 1 0.3422 0.8544 -0.0243 11.00000 0.05 0.13 Q9 1 0.3259 1.0691 -0.0565 11.00000 0.05 0.13 Q10 1 0.4409 1.0782 0.0419 11.00000 0.05 0.13 Q11 1 0.2970 0.9819 -0.0329 11.00000 0.05 0.13 Q12 1 0.2016 1.1055 -0.0775 11.00000 0.05 0.13 Q13 1 0.9268 1.0601 0.1345 11.00000 0.05 0.12 Q14 1 0.2603 0.7803 -0.1518 11.00000 0.05 0.12 Q15 1 0.7616 1.0363 0.3582 11.00000 0.05 0.12 Q16 1 0.4438 1.0134 0.0495 11.00000 0.05 0.11 Q17 1 0.0831 1.1216 -0.0639 11.00000 0.05 0.11 Q18 1 0.2156 0.8266 -0.0379 11.00000 0.05 0.11 Q19 1 0.1300 1.0554 -0.0366 11.00000 0.05 0.11 Q20 1 -0.0331 1.1386 -0.0727 11.00000 0.05 0.11 ; _shelx_res_checksum 23463 _shelx_hkl_file ; 0 0 -2 -0.40 1.00 0 0 2 0.03 0.71 0 0 2 -0.28 0.60 0 0 -2 -0.26 0.75 0 0 3 -0.25 1.24 0 0 -3 1.42 1.79 0 0 -3 -0.75 1.04 0 0 3 2.45 2.28 0 0 -3 3.59 2.52 0 0 5 0.91 2.88 0 0 -5 3.81 2.80 0 0 -5 3.44 4.04 0 0 -5 2.49 4.23 0 0 5 8.45 5.52 0 0 5 2.99 4.03 0 0 -7 -0.17 4.86 0 0 -7 2.56 2.72 0 0 7 -2.75 5.81 0 0 8 4484.09 75.87 0 0 -8 4089.88 74.37 0 0 -9 1.53 3.10 0 0 9 6.50 6.87 0 0 9 0.59 3.67 0 0 -9 -2.68 5.51 0 0 10 58.60 8.77 0 0 10 61.93 11.35 0 0 -10 72.73 13.46 0 0 -11 -0.84 6.65 0 0 11 1.59 4.80 0 0 11 2.39 8.95 0 0 12 765.89 32.00 0 0 -12 713.33 39.42 0 0 12 698.93 38.43 0 0 -13 13.99 10.24 0 0 13 0.42 6.89 0 0 13 11.17 12.86 0 0 14 53.80 15.44 0 0 14 66.88 12.98 0 0 -14 58.99 15.55 0 0 15 7.71 8.44 0 0 15 -8.77 13.45 0 0 -15 -2.57 10.34 0 0 16 993.57 45.30 0 0 16 882.79 52.92 0 0 17 -3.86 10.50 0 0 -17 1.86 10.98 0 0 17 8.67 12.02 0 0 18 1021.97 50.50 0 0 18 1043.76 62.00 0 0 -18 1013.53 61.72 0 0 19 10.34 15.24 0 0 19 -10.54 11.00 0 0 -19 -4.95 12.20 0 0 20 -30.59 20.02 0 0 -20 26.46 16.33 0 0 21 -2.86 15.45 0 0 -21 -0.30 14.00 0 0 22 64.67 22.95 0 0 -22 94.81 26.80 0 -1 1 -0.09 0.42 0 -1 -1 0.15 0.55 0 1 -1 -0.46 0.65 0 1 1 -0.43 0.80 0 -1 -2 -0.39 1.09 0 1 -2 -0.39 0.86 0 -1 2 1.31 1.18 0 -1 2 -0.60 1.09 0 -1 3 -1.37 1.47 0 1 3 15.23 3.04 0 -1 3 41.74 4.67 0 -1 -3 -0.99 2.87 0 1 3 44.30 5.86 0 1 -3 47.70 5.28 0 1 -3 48.80 4.87 0 1 -3 53.33 4.90 0 -1 3 58.56 5.41 0 1 4 3264.94 49.84 0 -1 4 3251.00 44.00 0 -1 -7 1680.23 28.21 0 -1 7 1582.24 42.33 0 1 7 1560.90 41.55 0 1 -7 1620.13 41.24 0 -1 7 1605.99 36.98 0 -1 7 1651.42 42.73 0 -1 -7 1582.38 45.12 0 1 -7 1607.85 34.87 0 1 -8 1212.76 39.02 0 1 8 1242.47 27.92 0 -1 8 1242.65 35.28 0 -1 -8 1154.98 25.43 0 1 8 1203.39 39.55 0 -1 8 1166.15 39.45 0 -1 -8 1145.31 41.32 0 1 9 1713.40 36.64 0 1 -9 1619.62 47.83 0 1 9 1702.14 49.80 0 -1 -9 1686.17 53.43 0 -1 9 1617.55 49.21 0 -1 -9 1674.82 33.09 0 -1 9 1633.89 42.41 0 -1 10 1800.26 47.95 0 1 10 1877.51 55.86 0 -1 -10 1785.63 35.91 0 1 -10 1728.51 52.82 0 -1 -10 1740.81 57.66 0 1 10 1931.91 40.86 0 -1 10 1881.04 56.25 0 1 11 780.46 27.96 0 1 11 686.27 36.19 0 -1 11 726.38 38.02 0 -1 -11 727.67 24.96 0 -1 11 725.37 31.84 0 1 -11 677.57 35.21 0 -1 -11 730.19 39.42 0 -1 12 1368.58 53.91 0 1 12 1382.24 54.25 0 1 -12 1436.60 53.91 0 1 12 1338.13 39.51 0 -1 12 1378.31 45.67 0 -1 -12 1338.52 55.74 0 -1 13 371.67 30.38 0 1 13 314.59 20.91 0 -1 -13 359.54 31.06 0 1 -13 407.42 31.01 0 -1 13 391.65 26.16 0 1 13 390.31 31.07 0 1 -14 33.44 12.12 0 -1 14 55.74 16.26 0 -1 14 33.10 10.63 0 1 14 74.31 19.82 0 1 14 51.44 11.45 0 -1 15 430.57 35.77 0 1 -15 322.66 30.84 0 1 15 307.23 29.84 0 -1 15 337.86 26.85 0 1 15 424.19 26.67 0 -1 -15 416.55 36.24 0 1 16 107.65 15.55 0 -1 16 106.72 16.99 0 -1 -16 133.01 23.07 0 1 -16 133.13 21.96 0 -1 16 128.61 23.33 0 1 16 137.73 23.91 0 1 -17 64.96 16.49 0 -1 17 106.65 21.73 0 1 17 92.92 16.40 0 -1 -17 47.97 17.33 0 -1 17 110.59 17.85 0 1 17 76.46 18.79 0 -1 18 151.16 21.44 0 1 18 186.80 28.48 0 1 -18 178.74 26.55 0 -1 -18 158.17 27.24 0 1 18 137.24 19.30 0 -1 18 157.53 27.87 0 -1 19 372.33 34.47 0 -1 19 306.02 37.16 0 -1 -19 376.96 41.11 0 1 -19 353.53 36.97 0 1 19 369.35 38.40 0 -1 -20 152.51 27.58 0 -1 20 150.51 24.54 0 1 -20 142.97 25.89 0 -1 20 137.68 28.13 0 1 20 130.52 27.39 0 -1 21 53.87 21.31 0 -1 -21 32.23 18.46 0 1 21 53.26 19.09 0 1 -21 13.35 13.31 0 1 22 668.86 58.76 0 -1 22 723.52 61.94 0 1 -22 674.53 57.10 0 -1 -22 713.07 61.99 0 -2 0 -0.14 0.87 0 -2 0 0.68 0.94 0 -2 0 0.14 0.92 0 -2 -1 1.28 0.98 0 -2 -1 0.54 0.90 0 -2 1 0.09 0.99 0 -2 -1 -0.08 0.99 0 -2 1 -0.43 0.80 0 -2 2 0.59 1.21 0 -2 2 1.04 2.22 0 -2 -2 -1.00 1.84 0 2 -5 2700.28 44.66 0 2 -5 2556.40 40.17 0 2 5 2707.04 45.20 0 -2 5 2655.11 43.49 0 -2 -5 2688.19 53.20 0 -2 5 2649.51 46.78 0 2 -5 2660.93 44.93 0 2 5 2688.96 52.61 0 -2 6 4244.29 61.31 0 2 -6 4252.33 58.34 0 -2 -6 4218.25 74.00 0 -2 -7 3160.05 68.24 0 -2 7 3332.19 58.52 0 -2 7 3352.17 59.60 0 -2 7 3112.56 60.82 0 2 7 3201.43 58.85 0 2 8 3910.24 70.23 0 2 -8 3563.33 62.93 0 -2 -8 3799.45 78.11 0 -2 8 3647.38 69.77 0 -2 8 3521.83 65.21 0 -2 9 1059.91 40.43 0 2 9 1055.54 39.44 0 -2 9 1092.94 38.11 0 2 -9 1006.58 36.62 0 2 9 1036.86 24.60 0 -2 -9 1089.13 24.26 0 2 10 1593.65 33.51 0 -2 10 1696.21 54.29 0 2 -10 1627.61 49.30 0 -2 -10 1729.54 32.91 0 -2 10 1642.15 49.05 0 2 10 1624.04 52.07 0 -2 -10 1691.58 58.85 0 2 11 1624.33 36.27 0 2 11 1613.28 54.88 0 -2 -11 1524.30 58.13 0 -2 11 1593.61 56.14 0 2 -11 1537.73 51.17 0 -2 11 1589.30 50.87 0 -2 -11 1616.73 33.64 0 -2 12 416.26 30.78 0 2 -12 396.69 27.70 0 2 12 386.46 29.69 0 -2 -12 448.89 19.11 0 -2 -12 383.37 31.45 0 2 12 419.98 20.58 0 -2 12 360.74 25.77 0 -2 -13 1578.46 65.00 0 -2 -13 1464.64 36.22 0 2 -13 1371.77 53.70 0 -2 13 1428.05 52.36 0 2 13 1519.46 40.62 0 -2 13 1416.79 58.32 0 2 13 1511.25 58.93 0 -2 -14 3.03 11.31 0 2 -14 21.66 10.36 0 -2 14 23.02 8.86 0 -2 14 6.85 11.37 0 2 14 -3.15 6.45 0 2 14 20.01 13.62 0 2 -15 454.36 34.75 0 2 15 530.57 39.73 0 -2 -15 525.79 41.71 0 -2 15 533.31 35.48 0 2 15 482.73 26.56 0 -2 15 488.73 38.56 0 2 16 214.96 19.33 0 2 16 198.66 26.61 0 2 -16 227.98 26.10 0 -2 16 224.29 24.78 0 -2 16 211.33 29.43 0 -2 -16 214.80 29.23 0 -2 -17 2744.92 101.70 0 2 -17 2620.42 89.31 0 -2 17 2489.23 81.87 0 2 17 2891.72 70.93 0 2 17 2909.69 96.05 0 -2 17 2767.29 97.39 0 -2 18 132.29 21.23 0 -2 18 83.21 21.98 0 2 18 111.57 23.92 0 2 -18 90.60 18.91 0 2 -19 112.46 22.96 0 2 19 129.44 26.48 0 -2 19 131.72 22.85 0 -2 19 148.04 26.68 0 -2 -19 109.74 25.39 0 -2 20 137.18 29.91 0 2 -20 119.72 23.59 0 -2 -20 147.40 28.99 0 2 20 90.42 24.83 0 -2 20 168.82 25.60 0 2 21 1.34 17.24 0 -2 -21 -10.05 18.93 0 2 -21 6.45 13.04 0 -2 21 -26.01 18.03 0 -2 21 17.67 19.22 0 -2 22 174.71 33.80 0 2 -22 138.79 27.71 0 2 22 161.46 33.35 0 -2 -22 99.78 25.48 0 3 0 7.02 2.51 0 -3 0 1.57 2.28 0 -3 0 -1.18 2.53 0 3 0 2.35 2.55 0 -3 3 2034.87 39.64 0 -3 -3 1972.25 42.00 0 3 3 1871.09 39.52 0 3 -3 1847.06 27.23 0 -3 3 1950.45 35.57 0 3 -3 2029.10 38.66 0 3 -3 1942.67 33.87 0 -3 4 403.47 19.32 0 -3 4 431.13 14.86 0 3 4 415.54 20.59 0 3 -4 373.64 17.79 0 3 -4 434.14 17.53 0 3 -4 424.95 14.41 0 -3 -4 429.54 21.63 0 -3 4 433.64 18.42 0 -3 5 1856.46 35.83 0 -3 5 1933.42 41.80 0 3 -5 1925.34 33.53 0 -3 5 1757.06 42.20 0 3 -5 1858.02 38.93 0 -3 -5 1750.64 47.54 0 -3 6 90.07 9.27 0 -3 6 108.27 11.40 0 -3 -6 93.39 12.74 0 -3 6 96.59 11.23 0 3 -6 101.60 8.86 0 3 6 90.63 10.07 0 3 7 29.01 7.20 0 -3 7 28.61 7.45 0 -3 -7 24.06 8.67 0 3 -7 20.72 5.15 0 -3 7 20.94 5.61 0 -3 7 18.04 6.24 0 -3 8 0.78 4.95 0 -3 8 9.95 7.22 0 3 -8 0.42 4.42 0 3 8 -0.40 5.04 0 -3 -8 12.24 9.06 0 -3 8 11.00 7.57 0 3 8 1.34 1.44 0 -3 9 5395.67 93.56 0 3 -9 5546.58 82.24 0 3 9 5327.33 88.73 0 -3 -9 5438.96 104.61 0 -3 9 5382.92 90.14 0 3 10 279.95 12.02 0 -3 10 250.97 22.22 0 -3 -10 257.76 25.01 0 -3 -10 267.83 11.69 0 3 10 251.12 21.08 0 -3 10 248.35 21.45 0 3 -10 284.04 20.01 0 -3 11 1674.95 58.25 0 3 11 1641.10 55.12 0 3 -11 1624.01 50.00 0 -3 -11 1613.05 30.70 0 3 11 1677.64 32.00 0 -3 -11 1640.94 64.11 0 -3 11 1634.91 54.09 0 -3 -12 145.84 10.00 0 3 -12 117.79 15.21 0 -3 -12 105.57 18.19 0 3 12 117.11 17.53 0 -3 12 117.52 16.86 0 3 12 133.99 10.46 0 -3 12 138.73 19.22 0 3 -13 129.27 16.48 0 3 13 143.42 20.47 0 3 13 170.89 12.93 0 -3 -13 150.27 22.91 0 -3 13 157.45 19.82 0 -3 -13 153.78 11.39 0 -3 13 143.62 21.08 0 -3 -14 178.39 26.35 0 -3 14 181.62 25.10 0 -3 14 183.43 21.58 0 3 -14 169.01 20.07 0 3 14 159.85 23.22 0 3 14 182.45 15.08 0 -3 -14 159.45 11.98 0 3 15 101.50 19.81 0 -3 15 72.49 15.97 0 3 15 72.55 10.31 0 3 -15 78.28 16.01 0 -3 15 72.51 17.87 0 -3 -15 68.64 17.74 0 3 16 692.97 30.51 0 -3 16 698.50 44.00 0 -3 16 672.49 47.80 0 3 -16 582.79 39.63 0 3 16 612.31 43.56 0 -3 -16 695.21 50.72 0 3 17 1296.95 65.20 0 -3 17 1146.41 58.50 0 -3 -17 1142.02 67.40 0 -3 17 1224.84 66.55 0 3 -17 1237.09 59.80 0 -3 18 101.94 23.89 0 -3 -18 101.29 24.83 0 -3 18 68.09 16.61 0 3 18 81.69 20.14 0 3 -18 63.98 16.97 0 3 -19 102.34 21.08 0 -3 19 75.57 22.03 0 3 19 94.76 22.54 0 -3 19 68.05 18.51 0 -3 -19 109.25 25.00 0 3 -20 102.30 22.97 0 -3 20 64.57 18.97 0 3 20 58.33 20.34 0 -3 -20 68.38 22.45 0 -3 20 43.71 18.86 0 3 -21 -6.15 16.86 0 3 21 14.28 18.50 0 -3 21 -2.00 16.74 0 -3 21 1.17 12.70 0 -3 -21 5.02 15.10 0 -3 22 -10.30 17.61 0 3 -22 -15.81 16.90 0 -3 -22 9.07 18.94 0 3 22 -0.20 17.20 0 4 -2 975.26 28.19 0 4 -2 970.10 20.01 0 -4 -2 918.55 28.86 0 -4 2 933.09 28.79 0 4 2 835.74 26.49 0 4 -2 943.40 24.04 0 -4 -2 923.29 23.43 0 4 2 988.24 26.76 0 4 2 983.52 21.29 0 -4 2 914.93 25.14 0 -4 2 998.34 19.69 0 4 3 14.58 5.29 0 4 -3 26.62 5.86 0 -4 -3 33.89 5.43 0 -4 3 9.80 4.85 0 -4 -3 21.16 6.85 0 4 -3 11.82 3.19 0 4 3 18.79 3.24 0 -4 3 19.01 5.23 0 4 3 10.84 3.81 0 -4 3 13.59 2.69 0 4 -3 8.86 4.45 0 -4 4 760.35 29.14 0 -4 4 698.84 17.81 0 4 4 753.44 14.55 0 -4 -4 695.48 29.06 0 4 -4 776.92 24.54 0 4 -4 736.35 19.76 0 -4 4 714.95 25.21 0 4 -5 9.99 4.98 0 4 -5 5.28 2.76 0 -4 5 8.07 4.88 0 -4 5 6.82 3.40 0 -4 -5 7.41 5.74 0 -4 5 1.45 4.54 0 -4 -6 6009.12 98.29 0 -4 6 5504.63 85.84 0 -4 7 36.42 9.26 0 -4 7 31.15 6.42 0 4 -7 51.18 7.00 0 -4 7 22.94 6.43 0 -4 -7 37.33 9.45 0 4 7 22.56 6.23 0 4 -8 865.58 28.87 0 -4 8 843.17 35.80 0 -4 8 810.65 36.30 0 4 8 837.67 33.10 0 -4 -8 832.94 40.82 0 -4 8 829.50 30.72 0 4 -9 710.99 28.23 0 -4 9 698.31 34.64 0 -4 9 660.91 29.94 0 -4 -9 731.30 39.70 0 -4 9 692.64 35.23 0 4 9 694.46 32.70 0 4 10 186.92 18.65 0 -4 10 176.16 20.10 0 4 -10 158.84 14.64 0 -4 -10 146.04 20.01 0 -4 10 140.86 16.63 0 4 11 612.93 15.33 0 -4 -11 649.79 42.15 0 4 -11 654.66 30.73 0 4 11 644.55 35.26 0 -4 11 623.48 36.74 0 -4 11 610.70 35.80 0 4 -12 545.67 30.29 0 4 12 546.52 34.89 0 -4 12 613.47 37.21 0 4 12 536.85 16.22 0 -4 12 565.07 36.85 0 -4 -12 559.07 40.72 0 4 13 554.46 18.30 0 -4 13 475.29 36.27 0 -4 13 455.73 33.91 0 4 13 501.78 34.96 0 4 -13 488.18 30.25 0 -4 -13 512.92 41.09 0 4 -14 -3.48 8.14 0 -4 -14 -8.40 13.96 0 4 14 -11.29 12.07 0 -4 14 3.41 10.74 0 -4 14 15.44 14.32 0 4 14 3.90 3.46 0 -4 15 24.79 13.07 0 4 15 22.50 5.53 0 4 15 9.87 12.19 0 4 -15 27.06 10.21 0 -4 15 25.90 14.40 0 -4 -15 29.88 16.73 0 -4 -16 351.80 38.00 0 4 16 315.44 32.56 0 -4 16 304.06 30.58 0 4 -16 304.48 28.29 0 -4 16 271.05 31.39 0 4 -17 50.05 14.30 0 -4 -17 51.03 19.49 0 4 17 58.64 19.97 0 -4 17 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113.74 27.48 0 -11 15 129.52 24.52 0 11 15 102.60 21.48 0 -11 -16 15.58 18.64 0 11 16 61.52 18.32 0 -11 16 26.81 21.66 0 -11 16 32.67 17.02 0 -11 17 57.40 20.61 0 11 17 77.85 19.38 0 -11 17 42.87 18.93 0 -11 -17 63.74 27.90 0 -11 18 -1.50 16.16 0 -11 -18 50.40 23.47 0 -11 18 17.43 19.22 0 11 18 16.59 15.21 0 12 0 460.16 30.09 0 -12 0 444.52 36.15 0 -12 0 460.35 28.65 0 12 1 212.79 21.42 0 -12 1 202.37 19.93 0 -12 -1 214.98 19.82 0 -12 1 228.32 27.96 0 -12 -1 165.29 22.94 0 12 -1 214.67 19.51 0 -12 -2 660.92 42.57 0 12 -2 711.35 33.41 0 -12 2 650.67 35.68 0 12 2 720.62 39.63 0 -12 2 670.25 45.94 0 -12 -3 469.43 35.48 0 -12 3 452.39 38.85 0 12 3 479.81 34.25 0 -12 3 483.34 31.44 0 12 -3 447.28 26.17 0 12 4 3.23 9.62 0 12 -4 -1.55 6.05 0 -12 4 8.85 8.89 0 -12 4 -7.72 13.27 0 -12 -4 8.96 9.37 0 12 5 155.20 21.84 0 12 -5 162.61 14.42 0 -12 5 122.70 22.91 0 -12 -5 155.28 20.52 0 -12 5 154.08 19.54 0 -12 6 11.82 11.83 0 12 -6 18.39 6.72 0 -12 6 -0.93 9.42 0 12 6 26.52 11.73 0 -12 7 23.56 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-1 0 16 1077.74 45.15 1 0 16 1050.25 59.37 1 0 16 1094.02 51.06 -1 0 16 1107.09 57.59 -1 0 17 377.51 28.44 -1 0 -17 377.19 36.68 1 0 17 396.94 38.30 -1 0 17 277.29 31.42 1 0 -17 300.42 33.78 1 0 17 378.23 32.24 1 0 18 296.55 35.55 -1 0 -18 285.62 33.97 -1 0 18 321.59 27.84 -1 0 18 325.42 36.24 1 0 18 313.34 30.56 1 0 -18 322.21 35.93 1 0 19 2.95 10.53 1 0 19 3.17 17.11 1 0 -19 9.54 14.32 -1 0 19 9.76 15.33 -1 0 -19 -14.81 16.00 -1 0 19 9.22 9.76 1 0 20 27.22 18.44 1 0 -20 0.46 13.34 -1 0 20 9.58 15.23 -1 0 -20 1.47 15.20 -1 0 21 -10.01 15.53 -1 0 -21 26.56 18.25 1 0 -21 3.40 14.97 1 0 21 12.38 16.22 1 0 -22 119.03 26.35 1 0 22 190.69 34.71 -1 0 22 151.37 33.01 -1 0 -22 71.24 23.59 1 1 -22 11.54 16.85 -1 -1 -22 3.75 17.49 1 -1 22 32.11 20.00 -1 1 22 36.59 22.04 1 1 -21 136.40 27.20 -1 -1 -21 173.50 30.77 -1 1 21 130.70 25.99 1 -1 21 137.30 30.52 1 1 -20 181.58 29.97 -1 -1 -20 292.27 37.71 -1 1 20 262.54 34.48 1 -1 20 182.38 29.85 1 -1 20 271.34 33.17 1 -1 19 95.68 20.39 -1 -1 -19 119.29 25.05 1 -1 19 22.57 18.10 1 1 -19 102.83 23.78 -1 1 19 50.35 18.38 1 -1 18 89.34 22.80 1 1 -18 63.20 16.76 -1 1 18 74.55 14.45 -1 1 18 101.94 20.86 1 -1 18 69.04 16.78 -1 -1 -18 94.05 22.75 -1 1 17 604.37 44.49 1 -1 17 561.68 45.45 -1 1 17 570.12 33.34 1 -1 17 608.03 42.36 -1 -1 -17 662.72 49.53 1 1 -17 639.76 46.11 1 -1 16 806.45 52.45 -1 1 16 823.95 38.06 -1 1 16 798.87 49.25 1 1 -16 735.82 47.72 1 -1 16 843.82 46.70 -1 -1 -16 764.02 49.93 1 1 -15 1074.70 54.71 -1 1 15 933.74 50.68 1 -1 15 965.91 55.19 -1 -1 -15 1116.19 58.96 1 -1 15 1019.87 49.37 -1 1 15 1038.52 39.85 1 -1 14 793.98 47.56 1 -1 14 714.47 40.29 -1 1 14 775.39 43.88 -1 -1 -14 771.11 46.99 1 1 -14 769.93 44.59 -1 1 14 734.22 31.87 1 -1 13 1117.34 54.00 -1 1 13 982.88 46.94 1 -1 13 1054.64 46.21 -1 1 13 1037.45 36.07 1 1 -13 1030.58 49.63 -1 -1 -13 1079.22 52.41 -1 1 12 125.39 12.74 -1 1 12 135.08 18.64 1 1 -12 126.23 17.57 1 -1 12 138.36 16.95 1 -1 12 142.78 20.90 -1 -1 -12 171.36 21.23 1 -1 11 428.60 30.48 -1 1 11 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71.52 27.43 11 4 7 84.98 27.68 11 4 7 54.23 22.04 -11 -4 7 62.86 21.95 11 -4 -7 35.54 21.44 11 -4 -8 5.34 21.83 11 4 8 25.81 18.81 11 4 8 53.73 21.34 -11 -4 8 36.40 19.16 -11 5 7 1.88 14.96 -11 -5 -7 3.14 13.14 11 -5 7 -0.10 19.08 11 5 -7 -14.83 21.81 -11 5 6 122.07 28.96 -11 -5 -6 68.89 19.80 11 -5 6 138.38 36.67 11 -5 6 199.87 35.34 11 5 -6 96.09 33.44 -11 5 5 4.32 14.87 -11 -5 -5 18.38 16.45 11 -5 5 -13.26 19.91 11 5 -5 22.54 21.36 11 -5 5 4.84 15.88 -11 5 4 104.85 25.23 -11 -5 -4 115.75 25.11 11 -5 4 127.12 34.10 11 5 -4 77.11 29.78 11 -5 4 154.74 31.01 11 -5 3 36.32 21.55 -11 5 3 11.19 15.10 -11 -5 -3 35.82 19.04 11 -5 3 -2.61 16.77 11 5 -3 2.56 16.30 11 -5 2 43.93 20.07 -11 -5 -2 76.39 21.85 11 -5 2 79.17 25.92 11 5 -2 23.60 21.02 11 -5 1 31.77 21.87 -11 -5 -1 7.44 14.67 11 -5 1 45.38 22.68 11 5 -1 23.36 19.81 -11 -5 0 81.90 23.76 11 5 0 26.90 18.21 11 -5 0 39.17 24.86 11 -5 -1 67.92 25.14 -11 -5 1 70.69 21.77 11 5 1 7.33 17.95 11 -5 -1 9.81 18.93 11 -5 -2 46.43 20.62 11 5 2 27.70 19.22 -11 -5 2 28.50 16.45 11 -5 -2 30.67 17.25 11 -5 -3 8.28 16.05 11 5 3 26.50 20.71 -11 -5 3 74.99 23.09 11 -5 -3 15.83 16.71 11 -5 -4 96.95 27.46 11 5 4 94.39 28.19 -11 -5 4 95.64 22.88 11 -5 -4 151.31 31.62 11 -5 -5 24.71 15.82 11 5 5 23.43 18.76 -11 -5 5 44.39 18.91 11 -5 -5 -0.23 16.55 11 -5 -6 112.26 29.95 11 5 6 118.13 30.82 -11 -5 6 126.10 27.72 11 -5 -6 152.71 32.71 11 -5 -7 -4.43 17.18 11 5 7 11.82 22.64 -11 -5 7 14.35 15.93 11 -5 -7 13.18 16.90 -11 6 6 1.92 17.30 -11 -6 -6 14.05 15.55 11 -6 6 31.24 23.96 11 6 -6 29.49 20.10 -11 6 5 106.50 24.14 -11 -6 -5 158.56 27.10 11 -6 5 151.45 36.58 11 6 -5 132.18 35.60 -11 6 4 199.54 34.04 -11 -6 -4 228.03 33.16 11 6 -4 274.47 46.23 11 -6 4 239.51 43.57 11 -6 4 238.28 35.60 11 -6 3 10.46 18.29 -11 -6 -3 19.06 18.18 11 -6 3 8.50 20.70 11 6 -3 -10.09 21.59 11 -6 2 80.89 24.71 -11 -6 -2 35.39 17.59 11 -6 2 28.82 21.95 11 6 -2 71.94 30.52 11 6 -1 333.82 49.10 -11 -6 -1 325.75 38.13 11 -6 1 430.98 54.49 11 -6 1 316.84 40.37 11 -6 0 14.52 19.37 -11 -6 0 6.15 12.60 11 6 0 19.91 17.32 11 -6 0 -12.20 21.37 11 6 1 370.59 50.55 -11 -6 1 379.27 40.92 11 -6 -1 367.19 49.10 11 -6 -1 377.00 45.56 11 -6 -2 56.53 22.92 11 6 2 44.61 22.03 -11 -6 2 70.73 21.19 11 -6 -2 58.74 26.14 11 -6 -3 7.96 18.59 11 6 3 -5.42 17.68 -11 -6 3 -9.17 16.57 11 -6 -3 -2.42 18.38 11 -6 -4 289.14 41.72 11 6 4 205.13 39.40 -11 -6 4 248.33 33.64 11 -6 -4 199.57 35.33 11 -6 -5 174.47 34.73 11 6 5 133.79 33.89 -11 -6 5 155.17 28.88 11 -6 -5 161.22 35.46 11 -6 -6 20.85 18.26 11 6 6 58.36 25.26 -11 -6 6 16.41 14.26 11 -6 -6 13.20 19.30 -11 -7 -4 87.01 22.10 11 -7 4 96.26 33.11 11 7 -4 79.48 29.38 -11 -7 -3 30.09 18.96 11 -7 3 14.48 20.83 11 7 -3 -37.08 27.11 -11 -7 -2 126.83 25.44 11 -7 2 154.63 36.96 11 7 -2 150.69 37.37 11 -7 2 220.50 33.81 11 -7 1 11.57 15.47 -11 -7 -1 14.07 13.97 11 -7 1 21.14 21.61 11 -7 0 188.11 32.32 -11 -7 0 215.46 31.65 11 -7 0 242.60 41.36 11 7 0 135.77 32.77 11 -7 -1 22.64 16.62 11 7 1 24.34 21.86 -11 -7 1 41.42 20.44 11 -7 -1 61.26 26.52 11 -7 -2 229.73 36.27 11 7 2 195.34 38.53 -11 -7 2 140.85 26.06 11 -7 -2 208.47 41.24 11 -7 -3 3.00 15.89 11 7 3 4.28 19.47 -11 -7 3 20.33 15.30 11 -7 -3 32.28 21.46 11 -7 -4 97.01 25.17 11 7 4 31.81 17.74 -11 -7 4 122.75 26.56 11 -7 -4 62.72 30.02 -11 -8 -1 32.45 16.68 11 8 -1 36.97 25.42 11 -8 1 29.30 20.90 11 -8 0 22.98 17.66 11 8 0 39.65 25.34 -11 -8 0 36.48 16.50 11 -8 0 32.32 19.62 11 -8 -1 11.69 16.02 11 8 1 48.98 27.58 -11 -8 1 26.15 17.27 11 -8 -1 5.53 19.13 -12 0 0 217.11 35.80 12 0 0 149.61 31.31 12 0 0 188.92 38.68 -12 0 -1 928.45 67.69 -12 0 1 793.84 63.58 12 0 1 954.78 71.03 12 0 1 1021.50 81.61 12 0 -1 984.89 69.92 12 0 -1 1077.69 85.14 -12 0 -2 -8.59 14.41 -12 0 2 -9.84 16.26 12 0 2 11.15 15.35 12 0 -2 -11.72 17.57 12 0 2 -10.80 20.38 12 0 -2 48.76 25.64 -12 0 3 221.59 36.44 -12 0 -3 151.14 29.96 12 0 3 296.58 46.75 12 0 3 195.15 36.86 12 0 -3 235.09 45.46 12 0 -3 165.84 30.62 12 0 -4 27.05 24.61 -12 0 -4 53.30 22.68 -12 0 4 26.32 17.97 12 0 4 43.79 25.74 12 0 4 7.42 17.95 12 0 -4 60.73 19.94 -12 -1 -4 35.55 19.93 -12 1 4 44.75 19.74 12 -1 4 49.45 22.95 12 -1 4 51.48 25.35 12 1 -4 53.63 21.33 12 1 -4 82.93 32.68 -12 -1 -3 83.10 25.99 -12 1 3 58.79 21.72 12 -1 3 96.58 29.60 12 1 -3 90.35 26.62 12 -1 3 141.52 32.77 12 1 -3 95.68 30.69 -12 -1 -2 -2.56 15.17 -12 1 2 -2.39 14.05 12 -1 2 17.85 19.26 12 1 -2 -3.82 14.44 12 -1 2 -3.78 20.82 12 1 -2 26.87 23.46 -12 1 1 212.44 36.90 -12 -1 -1 191.26 32.81 12 -1 1 217.53 38.45 12 1 -1 225.37 43.57 12 1 -1 288.47 40.41 12 -1 1 195.56 39.92 -12 1 0 10.00 15.43 -12 -1 0 27.92 18.70 12 -1 0 48.91 23.51 12 1 0 25.65 20.60 12 1 0 -13.15 20.06 12 -1 0 37.50 22.35 -12 1 -1 246.34 39.28 -12 -1 1 264.91 39.07 12 1 1 234.80 46.27 12 1 1 251.65 38.49 12 -1 -1 202.54 35.39 12 -1 -1 203.94 38.42 -12 1 -2 5.86 17.15 -12 -1 2 43.55 21.34 12 1 2 6.89 17.96 12 1 2 -4.59 18.91 12 -1 -2 32.55 22.80 12 -1 -2 0.71 19.78 12 -1 -3 132.09 35.59 -12 1 -3 72.36 22.62 -12 -1 3 63.44 22.09 12 1 3 156.12 32.89 12 1 3 53.68 23.36 12 -1 -3 72.13 23.88 12 -1 -4 95.51 30.46 -12 1 -4 72.94 23.91 -12 -1 4 30.59 20.25 12 1 4 30.63 18.96 12 1 4 46.56 26.20 12 -1 -4 41.76 22.76 -12 2 3 48.09 20.34 -12 -2 -3 107.63 24.55 12 -2 3 87.48 29.57 12 2 -3 156.85 29.34 12 -2 3 126.04 32.94 12 2 -3 81.91 31.15 -12 2 2 84.08 25.98 -12 -2 -2 165.24 31.77 12 -2 2 136.84 32.53 12 2 -2 162.08 30.41 12 2 -2 139.85 36.80 12 -2 2 182.85 36.02 -12 2 1 270.75 39.85 -12 -2 -1 285.47 38.92 12 -2 1 333.80 47.46 12 2 -1 419.58 55.95 12 2 -1 345.90 40.76 12 -2 1 381.94 50.52 -12 2 0 26.96 20.20 -12 -2 0 54.89 20.26 12 -2 0 60.86 24.25 12 2 0 34.50 17.90 12 2 0 38.09 26.95 12 -2 0 30.91 21.12 -12 2 -1 340.40 44.38 -12 -2 1 331.15 42.06 12 2 1 366.56 53.37 12 2 1 412.53 46.90 12 -2 -1 389.82 47.76 12 -2 -1 398.44 52.54 12 -2 -2 124.61 33.14 -12 2 -2 188.37 34.16 -12 -2 2 114.96 26.86 12 2 2 128.22 29.43 12 2 2 157.63 36.11 12 -2 -2 136.18 31.26 12 -2 -3 103.43 30.21 -12 2 -3 99.03 27.32 -12 -2 3 116.91 26.98 12 2 3 140.26 30.83 12 2 3 82.44 30.15 12 -2 -3 82.86 25.60 -12 3 2 58.44 21.86 -12 -3 -2 88.91 25.58 12 -3 2 62.61 24.91 12 3 -2 116.19 35.72 12 -3 2 87.04 30.39 -12 3 1 68.30 22.15 -12 -3 -1 86.80 26.53 12 -3 1 71.00 25.98 12 3 -1 107.27 33.45 12 -3 1 87.19 27.76 12 -3 0 116.37 32.13 -12 3 0 97.80 25.07 -12 -3 0 77.74 22.36 12 -3 0 109.54 30.12 12 3 0 50.75 27.56 12 -3 -1 85.07 28.70 -12 3 -1 46.68 19.49 -12 -3 1 27.82 17.20 12 3 1 64.14 26.68 12 -3 -1 107.38 30.11 12 -3 -2 25.33 25.19 -12 -3 2 74.67 24.16 12 3 2 35.90 26.03 12 -3 -2 93.02 30.66 0 0 0 0.00 0.00 TITL r20200519c in P2(1)2(1)2(1) REM P2(1)2(1)2(1) (#19 in standard setting) CELL 0.71073 9.773162 14.817146 18.330797 90.0000 90.0000 90.0000 ZERR 12.00 0.000368 0.000697 0.000641 0.0000 0.0000 0.0000 LATT -1 SYMM -x+1/2,-y, z+1/2 SYMM -x, y+1/2,-z+1/2 SYMM x+1/2,-y+1/2,-z SFAC C H N O UNIT 132.00 120.00 12.00 12.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 93461 _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 - Detector area scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.388 _oxdiff_exptl_absorpt_empirical_full_min 0.688