data_dm-skp-3-46_cu _audit_creation_date 2022-01-09 _audit_creation_method ; Olex2 1.3 (compiled Nov 21 2019 18:26:39 for OlexSys, GUI svn.r6003) ; _shelx_SHELXL_version_number '2014/7' _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. A71, 3-8. Sheldrick, G.M. (2015). Acta Cryst. C71, 3-8. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety '0.444(C24 H26 N2 O3)' _chemical_formula_sum 'C10.67 H11.56 N0.89 O1.33' _chemical_formula_weight 173.54 _chemical_melting_point ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 '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 61 _space_group_name_H-M_alt 'P b c a' _space_group_name_Hall '-P 2ac 2ab' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 7.72750(10) _cell_length_b 22.4337(4) _cell_length_c 24.2544(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4204.66(13) _cell_formula_units_Z 18 _cell_measurement_reflns_used 2291 _cell_measurement_temperature 150 _cell_measurement_theta_max 71.7220 _cell_measurement_theta_min 3.9370 _shelx_estimated_absorpt_T_max 0.950 _shelx_estimated_absorpt_T_min 0.938 _exptl_absorpt_coefficient_mu 0.653 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.19282 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.46 (Rigaku Oxford Diffraction, 2018) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_special_details ? _exptl_crystal_colour 'clear light yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.234 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 1664 _exptl_crystal_size_max 0.099 _exptl_crystal_size_mid 0.092 _exptl_crystal_size_min 0.08 _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0810 _diffrn_reflns_av_unetI/netI 0.0779 _diffrn_reflns_Laue_measured_fraction_full 0.993 _diffrn_reflns_Laue_measured_fraction_max 0.970 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 10894 _diffrn_reflns_point_group_measured_fraction_full 0.993 _diffrn_reflns_point_group_measured_fraction_max 0.970 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 72.708 _diffrn_reflns_theta_min 3.941 _diffrn_ambient_temperature 150 _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.970 _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 -191.00 -38.00 0.50 6.00 -- -101.00 0.00 108.00 306 2 \w -96.50 -1.00 0.50 6.00 -- -32.00 -72.00-108.00 191 3 \w -90.00 -19.00 0.50 6.00 -- -101.00 72.00 108.00 142 4 \w -122.00 -87.00 0.50 6.00 -- -101.00 72.00 36.00 70 5 \w -35.00 25.00 0.50 6.00 -- -32.00 72.00 108.00 120 ; _diffrn_measurement_device 'abstract diffractometer' _diffrn_measurement_device_type 'dtrek-CrysAlisPro-abstract goniometer imported rigaku-d*trek images' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.0802401000 _diffrn_orient_matrix_UB_12 -0.0607844000 _diffrn_orient_matrix_UB_13 -0.0148524000 _diffrn_orient_matrix_UB_21 -0.1431307000 _diffrn_orient_matrix_UB_22 0.0100600000 _diffrn_orient_matrix_UB_23 0.0431832000 _diffrn_orient_matrix_UB_31 -0.1129969000 _diffrn_orient_matrix_UB_32 0.0305046000 _diffrn_orient_matrix_UB_33 -0.0441036000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Cu) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 2670 _reflns_number_total 4061 _reflns_odcompleteness_completeness 96.53 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 72.56 _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 1.171.39.46 (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.46 (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2014/7 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _refine_diff_density_max 0.431 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.138 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 267 _refine_ls_number_reflns 4061 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1065 _refine_ls_R_factor_gt 0.0693 _refine_ls_restrained_S_all 1.074 _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^)+(0.1342P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1917 _refine_ls_wR_factor_ref 0.2512 _refine_special_details ? _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C00H(H00H), C00Q(H00Q) 2.b Aromatic/amide H refined with riding coordinates: C00B(H00B), C00C(H00C), C00D(H00D), C00E(H00E), C00I(H00I), C00J(H00J), C00K(H00K), C00L(H00L), C00P(H00P) 2.c Idealised Me refined as rotating group: C00M(H00A,H00F,H00G), C00O(H00M,H00N,H00O), C00R(H00R,H00S,H00T), C00S(H00U, H00V,H00W), C00T(H00X,H00Y,H) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _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 O001 O 0.8708(3) 0.35150(10) 0.39022(9) 0.0576(6) Uani 1 1 d . . . . . O002 O 0.8177(3) 0.41568(11) 0.76959(10) 0.0642(7) Uani 1 1 d . . . . . N003 N 0.7420(3) 0.44172(10) 0.39909(10) 0.0424(6) Uani 1 1 d . . . . . N004 N 0.7160(3) 0.37602(12) 0.78297(11) 0.0499(6) Uani 1 1 d . . . . . O005 O 0.6580(4) 0.37152(13) 0.82944(10) 0.0772(8) Uani 1 1 d . . . . . C006 C 0.5708(3) 0.34588(12) 0.48806(11) 0.0405(6) Uani 1 1 d . . . . . C007 C 0.5321(3) 0.32745(11) 0.54332(12) 0.0399(6) Uani 1 1 d . . . . . C008 C 0.7363(3) 0.37024(12) 0.47600(12) 0.0396(6) Uani 1 1 d . . . . . C009 C 0.6613(3) 0.33405(11) 0.58516(11) 0.0395(6) Uani 1 1 d . . . . . C00A C 0.6335(3) 0.31464(12) 0.64328(11) 0.0403(6) Uani 1 1 d . . . . . C00B C 0.3628(3) 0.30542(13) 0.55428(13) 0.0456(7) Uani 1 1 d . . . . . H00B H 0.3331 0.2939 0.5908 0.055 Uiso 1 1 calc R U . . . C00C C 0.8189(4) 0.35839(12) 0.57133(12) 0.0434(7) Uani 1 1 d . . . . . H00C H 0.9050 0.3628 0.5990 0.052 Uiso 1 1 calc R U . . . C00D C 0.8553(4) 0.37681(13) 0.51706(12) 0.0434(7) Uani 1 1 d . . . . . H00D H 0.9645 0.3941 0.5089 0.052 Uiso 1 1 calc R U . . . C00E C 0.5507(4) 0.24092(13) 0.71100(12) 0.0444(7) Uani 1 1 d . . . . . H00E H 0.5062 0.2023 0.7186 0.053 Uiso 1 1 calc R U . . . C00F C 0.5975(3) 0.27732(13) 0.75538(12) 0.0428(7) Uani 1 1 d . . . . . C00G C 0.7866(4) 0.38691(13) 0.41789(12) 0.0437(7) Uani 1 1 d . . . . . C00H C 0.8123(4) 0.46324(15) 0.34602(12) 0.0529(8) Uani 1 1 d . . . . . H00H H 0.7699 0.5051 0.3415 0.063 Uiso 1 1 calc R U . . . C00I C 0.2426(4) 0.30050(13) 0.51356(14) 0.0489(7) Uani 1 1 d . . . . . H00I H 0.1311 0.2850 0.5218 0.059 Uiso 1 1 calc R U . . . C00J C 0.5662(4) 0.25864(12) 0.65671(12) 0.0431(7) Uani 1 1 d . . . . . H00J H 0.5307 0.2324 0.6281 0.052 Uiso 1 1 calc R U . . . C00K C 0.6822(4) 0.35157(12) 0.68617(12) 0.0426(6) Uani 1 1 d . . . . . H00K H 0.7291 0.3898 0.6784 0.051 Uiso 1 1 calc R U . . . C00L C 0.4411(4) 0.33990(13) 0.44708(13) 0.0475(7) Uani 1 1 d . . . . . H00L H 0.4661 0.3514 0.4102 0.057 Uiso 1 1 calc R U . . . C00M C 0.7522(4) 0.53439(14) 0.45389(15) 0.0566(8) Uani 1 1 d . . . . . H00A H 0.8460 0.5181 0.4765 0.085 Uiso 1 1 calc R U . . . H00F H 0.6817 0.5615 0.4763 0.085 Uiso 1 1 calc R U . . . H00G H 0.8013 0.5562 0.4226 0.085 Uiso 1 1 calc R U . . . C00N C 0.6631(4) 0.33326(13) 0.74097(12) 0.0439(7) Uani 1 1 d . . . . . C00O C 0.5759(4) 0.25337(15) 0.81320(12) 0.0498(7) Uani 1 1 d . . . . . H00M H 0.4906 0.2775 0.8330 0.075 Uiso 1 1 calc R U . . . H00N H 0.6872 0.2551 0.8325 0.075 Uiso 1 1 calc R U . . . H00O H 0.5360 0.2120 0.8115 0.075 Uiso 1 1 calc R U . . . C00P C 0.2819(4) 0.31806(14) 0.45947(14) 0.0529(8) Uani 1 1 d . . . . . H00P H 0.1968 0.3146 0.4314 0.063 Uiso 1 1 calc R U . . . C00Q C 0.6397(4) 0.48377(13) 0.43268(12) 0.0445(7) Uani 1 1 d . . . . . H00Q H 0.5959 0.4614 0.4655 0.053 Uiso 1 1 calc R U . . . C00R C 0.4826(4) 0.50683(16) 0.40123(15) 0.0592(8) Uani 1 1 d . . . . . H00R H 0.5212 0.5302 0.3694 0.089 Uiso 1 1 calc R U . . . H00S H 0.4128 0.5321 0.4256 0.089 Uiso 1 1 calc R U . . . H00T H 0.4127 0.4731 0.3886 0.089 Uiso 1 1 calc R U . . . C00S C 0.7395(5) 0.42788(19) 0.29704(15) 0.0705(10) Uani 1 1 d . . . . . H00U H 0.7845 0.3871 0.2980 0.106 Uiso 1 1 calc R U . . . H00V H 0.7746 0.4471 0.2625 0.106 Uiso 1 1 calc R U . . . H00W H 0.6129 0.4270 0.2993 0.106 Uiso 1 1 calc R U . . . C00T C 1.0093(5) 0.46662(19) 0.34605(16) 0.0709(10) Uani 1 1 d . . . . . H00X H 1.0484 0.4886 0.3787 0.106 Uiso 1 1 calc R U . . . H00Y H 1.0487 0.4873 0.3127 0.106 Uiso 1 1 calc R U . . . H H 1.0575 0.4262 0.3468 0.106 Uiso 1 1 calc R 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 O001 0.0711(14) 0.0462(12) 0.0554(13) -0.0056(10) 0.0094(10) 0.0214(11) O002 0.0732(15) 0.0548(14) 0.0646(14) -0.0113(11) 0.0008(12) -0.0143(12) N003 0.0466(13) 0.0363(12) 0.0445(14) 0.0013(10) 0.0040(10) 0.0053(10) N004 0.0539(15) 0.0466(15) 0.0492(15) -0.0067(11) -0.0040(11) 0.0012(12) O005 0.106(2) 0.0740(18) 0.0513(14) -0.0139(13) 0.0132(14) -0.0159(15) C006 0.0397(14) 0.0311(13) 0.0507(16) -0.0046(11) -0.0013(12) 0.0023(11) C007 0.0418(14) 0.0280(12) 0.0499(15) -0.0055(11) 0.0022(12) 0.0007(10) C008 0.0444(14) 0.0299(13) 0.0444(15) 0.0016(11) 0.0035(11) 0.0047(11) C009 0.0414(14) 0.0317(13) 0.0454(15) -0.0055(11) -0.0009(12) 0.0058(11) C00A 0.0412(14) 0.0336(14) 0.0461(15) -0.0019(11) -0.0003(12) 0.0009(11) C00B 0.0427(15) 0.0372(15) 0.0567(17) -0.0023(13) 0.0017(13) 0.0002(11) C00C 0.0420(14) 0.0385(15) 0.0496(16) 0.0029(12) -0.0026(13) 0.0017(12) C00D 0.0403(14) 0.0353(14) 0.0547(17) 0.0029(12) -0.0010(12) -0.0034(11) C00E 0.0428(14) 0.0352(14) 0.0552(17) 0.0033(13) 0.0009(13) -0.0006(11) C00F 0.0381(14) 0.0400(15) 0.0504(16) 0.0018(12) -0.0012(12) 0.0023(11) C00G 0.0468(15) 0.0374(14) 0.0468(15) 0.0037(12) 0.0015(13) 0.0054(12) C00H 0.0656(19) 0.0441(17) 0.0491(18) 0.0090(13) 0.0092(15) 0.0120(14) C00I 0.0425(14) 0.0365(15) 0.068(2) -0.0038(14) -0.0035(14) -0.0043(12) C00J 0.0427(14) 0.0356(15) 0.0509(17) -0.0045(12) -0.0020(12) -0.0030(11) C00K 0.0425(14) 0.0342(14) 0.0513(16) -0.0006(12) -0.0029(13) 0.0019(11) C00L 0.0529(16) 0.0375(15) 0.0522(16) -0.0040(13) -0.0049(14) 0.0022(12) C00M 0.0649(19) 0.0383(16) 0.067(2) -0.0046(14) 0.0043(16) 0.0016(14) C00N 0.0401(15) 0.0404(15) 0.0512(16) -0.0050(12) -0.0018(13) 0.0022(11) C00O 0.0499(16) 0.0491(17) 0.0503(17) 0.0024(14) 0.0012(13) 0.0022(13) C00P 0.0500(17) 0.0465(17) 0.062(2) -0.0055(14) -0.0141(15) -0.0034(13) C00Q 0.0467(15) 0.0348(14) 0.0521(16) 0.0007(12) 0.0072(13) 0.0056(12) C00R 0.0518(17) 0.0526(19) 0.073(2) 0.0015(16) -0.0016(16) 0.0126(15) C00S 0.090(3) 0.071(2) 0.051(2) 0.0005(18) -0.0033(18) 0.017(2) C00T 0.067(2) 0.069(2) 0.077(2) 0.0081(19) 0.0232(19) 0.0003(18) _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 O001 C00G 1.226(3) . ? O002 N004 1.231(3) . ? N003 C00G 1.356(4) . ? N003 C00H 1.478(4) . ? N003 C00Q 1.476(3) . ? N004 O005 1.217(3) . ? N004 C00N 1.458(4) . ? C006 C007 1.434(4) . ? C006 C008 1.421(4) . ? C006 C00L 1.418(4) . ? C007 C009 1.431(4) . ? C007 C00B 1.424(4) . ? C008 C00D 1.363(4) . ? C008 C00G 1.509(4) . ? C009 C00A 1.491(4) . ? C009 C00C 1.376(4) . ? C00A C00J 1.398(4) . ? C00A C00K 1.382(4) . ? C00B H00B 0.9500 . ? C00B C00I 1.360(4) . ? C00C H00C 0.9500 . ? C00C C00D 1.408(4) . ? C00D H00D 0.9500 . ? C00E H00E 0.9500 . ? C00E C00F 1.399(4) . ? C00E C00J 1.381(4) . ? C00F C00N 1.398(4) . ? C00F C00O 1.511(4) . ? C00H H00H 1.0000 . ? C00H C00S 1.535(5) . ? C00H C00T 1.524(5) . ? C00I H00I 0.9500 . ? C00I C00P 1.403(5) . ? C00J H00J 0.9500 . ? C00K H00K 0.9500 . ? C00K C00N 1.399(4) . ? C00L H00L 0.9500 . ? C00L C00P 1.358(4) . ? C00M H00A 0.9800 . ? C00M H00F 0.9800 . ? C00M H00G 0.9800 . ? C00M C00Q 1.520(4) . ? C00O H00M 0.9800 . ? C00O H00N 0.9800 . ? C00O H00O 0.9800 . ? C00P H00P 0.9500 . ? C00Q H00Q 1.0000 . ? C00Q C00R 1.524(4) . ? C00R H00R 0.9800 . ? C00R H00S 0.9800 . ? C00R H00T 0.9800 . ? C00S H00U 0.9800 . ? C00S H00V 0.9800 . ? C00S H00W 0.9800 . ? C00T H00X 0.9800 . ? C00T H00Y 0.9800 . ? C00T H 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 C00G N003 C00H 119.7(2) . . ? C00G N003 C00Q 122.0(2) . . ? C00Q N003 C00H 118.0(2) . . ? O002 N004 C00N 118.1(3) . . ? O005 N004 O002 122.6(3) . . ? O005 N004 C00N 119.3(3) . . ? C008 C006 C007 119.4(3) . . ? C00L C006 C007 118.7(3) . . ? C00L C006 C008 121.9(3) . . ? C009 C007 C006 119.2(2) . . ? C00B C007 C006 117.8(3) . . ? C00B C007 C009 123.0(3) . . ? C006 C008 C00G 121.3(3) . . ? C00D C008 C006 119.9(3) . . ? C00D C008 C00G 118.8(2) . . ? C007 C009 C00A 122.7(2) . . ? C00C C009 C007 119.0(3) . . ? C00C C009 C00A 118.3(2) . . ? C00J C00A C009 122.4(2) . . ? C00K C00A C009 119.8(2) . . ? C00K C00A C00J 117.7(3) . . ? C007 C00B H00B 119.3 . . ? C00I C00B C007 121.3(3) . . ? C00I C00B H00B 119.3 . . ? C009 C00C H00C 119.3 . . ? C009 C00C C00D 121.4(3) . . ? C00D C00C H00C 119.3 . . ? C008 C00D C00C 121.1(3) . . ? C008 C00D H00D 119.4 . . ? C00C C00D H00D 119.4 . . ? C00F C00E H00E 118.5 . . ? C00J C00E H00E 118.5 . . ? C00J C00E C00F 122.9(3) . . ? C00E C00F C00O 118.6(3) . . ? C00N C00F C00E 115.2(3) . . ? C00N C00F C00O 126.3(3) . . ? O001 C00G N003 122.6(3) . . ? O001 C00G C008 119.2(3) . . ? N003 C00G C008 118.2(2) . . ? N003 C00H H00H 106.3 . . ? N003 C00H C00S 111.7(3) . . ? N003 C00H C00T 112.5(3) . . ? C00S C00H H00H 106.3 . . ? C00T C00H H00H 106.3 . . ? C00T C00H C00S 113.1(3) . . ? C00B C00I H00I 119.7 . . ? C00B C00I C00P 120.6(3) . . ? C00P C00I H00I 119.7 . . ? C00A C00J H00J 119.6 . . ? C00E C00J C00A 120.9(3) . . ? C00E C00J H00J 119.6 . . ? C00A C00K H00K 119.7 . . ? C00A C00K C00N 120.7(3) . . ? C00N C00K H00K 119.7 . . ? C006 C00L H00L 119.4 . . ? C00P C00L C006 121.3(3) . . ? C00P C00L H00L 119.4 . . ? H00A C00M H00F 109.5 . . ? H00A C00M H00G 109.5 . . ? H00F C00M H00G 109.5 . . ? C00Q C00M H00A 109.5 . . ? C00Q C00M H00F 109.5 . . ? C00Q C00M H00G 109.5 . . ? C00F C00N N004 121.2(3) . . ? C00F C00N C00K 122.6(3) . . ? C00K C00N N004 116.2(3) . . ? C00F C00O H00M 109.5 . . ? C00F C00O H00N 109.5 . . ? C00F C00O H00O 109.5 . . ? H00M C00O H00N 109.5 . . ? H00M C00O H00O 109.5 . . ? H00N C00O H00O 109.5 . . ? C00I C00P H00P 119.9 . . ? C00L C00P C00I 120.3(3) . . ? C00L C00P H00P 119.9 . . ? N003 C00Q C00M 111.0(2) . . ? N003 C00Q H00Q 107.4 . . ? N003 C00Q C00R 111.5(2) . . ? C00M C00Q H00Q 107.4 . . ? C00M C00Q C00R 111.8(3) . . ? C00R C00Q H00Q 107.4 . . ? C00Q C00R H00R 109.5 . . ? C00Q C00R H00S 109.5 . . ? C00Q C00R H00T 109.5 . . ? H00R C00R H00S 109.5 . . ? H00R C00R H00T 109.5 . . ? H00S C00R H00T 109.5 . . ? C00H C00S H00U 109.5 . . ? C00H C00S H00V 109.5 . . ? C00H C00S H00W 109.5 . . ? H00U C00S H00V 109.5 . . ? H00U C00S H00W 109.5 . . ? H00V C00S H00W 109.5 . . ? C00H C00T H00X 109.5 . . ? C00H C00T H00Y 109.5 . . ? C00H C00T H 109.5 . . ? H00X C00T H00Y 109.5 . . ? H00X C00T H 109.5 . . ? H00Y C00T H 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 O002 N004 C00N C00F 158.6(3) . . . . ? O002 N004 C00N C00K -21.4(4) . . . . ? O005 N004 C00N C00F -21.7(4) . . . . ? O005 N004 C00N C00K 158.3(3) . . . . ? C006 C007 C009 C00A -178.4(2) . . . . ? C006 C007 C009 C00C 0.5(4) . . . . ? C006 C007 C00B C00I 1.6(4) . . . . ? C006 C008 C00D C00C 1.7(4) . . . . ? C006 C008 C00G O001 -96.7(3) . . . . ? C006 C008 C00G N003 85.7(3) . . . . ? C006 C00L C00P C00I -0.3(5) . . . . ? C007 C006 C008 C00D -1.1(4) . . . . ? C007 C006 C008 C00G 176.4(2) . . . . ? C007 C006 C00L C00P 1.0(4) . . . . ? C007 C009 C00A C00J 47.8(4) . . . . ? C007 C009 C00A C00K -135.1(3) . . . . ? C007 C009 C00C C00D 0.0(4) . . . . ? C007 C00B C00I C00P -1.1(4) . . . . ? C008 C006 C007 C009 0.0(4) . . . . ? C008 C006 C007 C00B 177.6(2) . . . . ? C008 C006 C00L C00P -178.2(3) . . . . ? C009 C007 C00B C00I 179.1(3) . . . . ? C009 C00A C00J C00E 176.6(3) . . . . ? C009 C00A C00K C00N -177.6(2) . . . . ? C009 C00C C00D C008 -1.1(4) . . . . ? C00A C009 C00C C00D 179.0(2) . . . . ? C00A C00K C00N N004 -179.1(2) . . . . ? C00A C00K C00N C00F 1.0(4) . . . . ? C00B C007 C009 C00A 4.2(4) . . . . ? C00B C007 C009 C00C -176.9(2) . . . . ? C00B C00I C00P C00L 0.4(5) . . . . ? C00C C009 C00A C00J -131.1(3) . . . . ? C00C C009 C00A C00K 46.0(4) . . . . ? C00D C008 C00G O001 80.8(4) . . . . ? C00D C008 C00G N003 -96.8(3) . . . . ? C00E C00F C00N N004 179.5(2) . . . . ? C00E C00F C00N C00K -0.5(4) . . . . ? C00F C00E C00J C00A 1.1(4) . . . . ? C00G N003 C00H C00S 68.3(4) . . . . ? C00G N003 C00H C00T -60.2(4) . . . . ? C00G N003 C00Q C00M 106.8(3) . . . . ? C00G N003 C00Q C00R -127.9(3) . . . . ? C00G C008 C00D C00C -175.9(3) . . . . ? C00H N003 C00G O001 -7.1(4) . . . . ? C00H N003 C00G C008 170.3(3) . . . . ? C00H N003 C00Q C00M -66.6(3) . . . . ? C00H N003 C00Q C00R 58.8(3) . . . . ? C00J C00A C00K C00N -0.4(4) . . . . ? C00J C00E C00F C00N -0.5(4) . . . . ? C00J C00E C00F C00O -179.7(3) . . . . ? C00K C00A C00J C00E -0.6(4) . . . . ? C00L C006 C007 C009 -179.2(2) . . . . ? C00L C006 C007 C00B -1.6(4) . . . . ? C00L C006 C008 C00D 178.0(3) . . . . ? C00L C006 C008 C00G -4.5(4) . . . . ? C00O C00F C00N N004 -1.3(4) . . . . ? C00O C00F C00N C00K 178.7(3) . . . . ? C00Q N003 C00G O001 179.6(3) . . . . ? C00Q N003 C00G C008 -2.9(4) . . . . ? C00Q N003 C00H C00S -118.1(3) . . . . ? C00Q N003 C00H C00T 113.3(3) . . . . ? _shelx_res_file ; dm-skp-3-46_cu.res created by SHELXL-2014/7 TITL dm-skp-3-46_cu_a.res in Pbca REM Old TITL DM-SKP-3-46_Cu in Pbca REM SHELXT solution in Pbca REM R1 0.439, Rweak 0.175, Alpha 0.019, Orientation as input REM Formula found by SHELXT: C26 N O2 CELL 1.54184 7.7275 22.4337 24.2544 90 90 90 ZERR 18 0.0001 0.0004 0.0005 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H N O UNIT 192 208 16 24 L.S. 4 0 0 PLAN 2 SIZE 0.08 0.092 0.099 TEMP -123.15 CONF BOND $H list 4 fmap 2 53 acta MORE -1 REM REM REM WGHT 0.134200 FVAR 0.33665 O001 4 0.870760 0.351504 0.390222 11.00000 0.07109 0.04625 = 0.05544 -0.00561 0.00941 0.02143 O002 4 0.817727 0.415679 0.769587 11.00000 0.07318 0.05484 = 0.06458 -0.01125 0.00076 -0.01430 N003 3 0.742005 0.441724 0.399086 11.00000 0.04657 0.03630 = 0.04446 0.00131 0.00396 0.00534 N004 3 0.715977 0.376019 0.782968 11.00000 0.05386 0.04664 = 0.04923 -0.00674 -0.00404 0.00124 O005 4 0.658031 0.371522 0.829436 11.00000 0.10633 0.07400 = 0.05127 -0.01391 0.01318 -0.01592 C006 1 0.570812 0.345882 0.488058 11.00000 0.03968 0.03110 = 0.05070 -0.00459 -0.00128 0.00228 C007 1 0.532068 0.327452 0.543316 11.00000 0.04184 0.02801 = 0.04988 -0.00554 0.00220 0.00067 C008 1 0.736316 0.370245 0.476001 11.00000 0.04437 0.02992 = 0.04438 0.00155 0.00348 0.00473 C009 1 0.661255 0.334052 0.585162 11.00000 0.04140 0.03169 = 0.04543 -0.00549 -0.00086 0.00575 C00A 1 0.633532 0.314639 0.643280 11.00000 0.04116 0.03356 = 0.04613 -0.00187 -0.00026 0.00087 C00B 1 0.362756 0.305423 0.554284 11.00000 0.04270 0.03722 = 0.05673 -0.00225 0.00173 0.00024 AFIX 43 H00B 2 0.333095 0.293932 0.590779 11.00000 -1.20000 AFIX 0 C00C 1 0.818904 0.358388 0.571331 11.00000 0.04204 0.03852 = 0.04960 0.00290 -0.00256 0.00166 AFIX 43 H00C 2 0.904996 0.362846 0.598986 11.00000 -1.20000 AFIX 0 C00D 1 0.855258 0.376815 0.517060 11.00000 0.04033 0.03528 = 0.05473 0.00287 -0.00096 -0.00344 AFIX 43 H00D 2 0.964517 0.394118 0.508919 11.00000 -1.20000 AFIX 0 C00E 1 0.550706 0.240925 0.711002 11.00000 0.04281 0.03518 = 0.05523 0.00330 0.00086 -0.00064 AFIX 43 H00E 2 0.506247 0.202297 0.718552 11.00000 -1.20000 AFIX 0 C00F 1 0.597545 0.277319 0.755383 11.00000 0.03815 0.04001 = 0.05037 0.00176 -0.00119 0.00229 C00G 1 0.786631 0.386908 0.417887 11.00000 0.04681 0.03740 = 0.04677 0.00373 0.00147 0.00535 C00H 1 0.812350 0.463237 0.346016 11.00000 0.06557 0.04405 = 0.04908 0.00899 0.00924 0.01201 AFIX 13 H00H 2 0.769948 0.505072 0.341536 11.00000 -1.20000 AFIX 0 C00I 1 0.242625 0.300500 0.513556 11.00000 0.04249 0.03654 = 0.06757 -0.00385 -0.00349 -0.00428 AFIX 43 H00I 2 0.131136 0.285042 0.521802 11.00000 -1.20000 AFIX 0 C00J 1 0.566201 0.258635 0.656712 11.00000 0.04270 0.03561 = 0.05091 -0.00447 -0.00196 -0.00299 AFIX 43 H00J 2 0.530652 0.232430 0.628104 11.00000 -1.20000 AFIX 0 C00K 1 0.682231 0.351571 0.686170 11.00000 0.04247 0.03419 = 0.05129 -0.00061 -0.00289 0.00185 AFIX 43 H00K 2 0.729150 0.389790 0.678356 11.00000 -1.20000 AFIX 0 C00L 1 0.441133 0.339905 0.447080 11.00000 0.05286 0.03750 = 0.05218 -0.00396 -0.00489 0.00223 AFIX 43 H00L 2 0.466098 0.351410 0.410234 11.00000 -1.20000 AFIX 0 C00M 1 0.752177 0.534394 0.453888 11.00000 0.06494 0.03829 = 0.06670 -0.00463 0.00432 0.00160 AFIX 137 H00A 2 0.846025 0.518071 0.476485 11.00000 -1.50000 H00F 2 0.681744 0.561505 0.476253 11.00000 -1.50000 H00G 2 0.801304 0.556246 0.422598 11.00000 -1.50000 AFIX 0 C00N 1 0.663147 0.333256 0.740972 11.00000 0.04007 0.04038 = 0.05120 -0.00496 -0.00182 0.00223 C00O 1 0.575942 0.253373 0.813195 11.00000 0.04992 0.04912 = 0.05030 0.00245 0.00120 0.00219 AFIX 137 H00M 2 0.490627 0.277549 0.833037 11.00000 -1.50000 H00N 2 0.687182 0.255087 0.832534 11.00000 -1.50000 H00O 2 0.536005 0.211952 0.811515 11.00000 -1.50000 AFIX 0 C00P 1 0.281945 0.318057 0.459471 11.00000 0.05002 0.04645 = 0.06212 -0.00554 -0.01410 -0.00335 AFIX 43 H00P 2 0.196814 0.314644 0.431390 11.00000 -1.20000 AFIX 0 C00Q 1 0.639657 0.483766 0.432683 11.00000 0.04672 0.03477 = 0.05210 0.00065 0.00717 0.00564 AFIX 13 H00Q 2 0.595895 0.461373 0.465494 11.00000 -1.20000 AFIX 0 C00R 1 0.482578 0.506830 0.401230 11.00000 0.05183 0.05257 = 0.07329 0.00148 -0.00158 0.01262 AFIX 137 H00R 2 0.521224 0.530155 0.369362 11.00000 -1.50000 H00S 2 0.412811 0.532116 0.425551 11.00000 -1.50000 H00T 2 0.412700 0.473050 0.388553 11.00000 -1.50000 AFIX 0 C00S 1 0.739465 0.427883 0.297038 11.00000 0.08960 0.07060 = 0.05133 0.00047 -0.00328 0.01667 AFIX 137 H00U 2 0.784451 0.387054 0.298048 11.00000 -1.50000 H00V 2 0.774550 0.447051 0.262494 11.00000 -1.50000 H00W 2 0.612873 0.426979 0.299311 11.00000 -1.50000 AFIX 0 C00T 1 1.009286 0.466623 0.346050 11.00000 0.06652 0.06878 = 0.07739 0.00807 0.02324 0.00033 AFIX 137 H00X 2 1.048378 0.488566 0.378692 11.00000 -1.50000 H00Y 2 1.048677 0.487258 0.312722 11.00000 -1.50000 H 2 1.057465 0.426221 0.346757 11.00000 -1.50000 AFIX 0 HKLF 4 REM dm-skp-3-46_cu_a.res in Pbca REM R1 = 0.0693 for 2670 Fo > 4sig(Fo) and 0.1065 for all 4061 data REM 267 parameters refined using 0 restraints END WGHT 0.1331 0.0000 REM Highest difference peak 0.431, deepest hole -0.491, 1-sigma level 0.138 Q1 1 0.8781 0.3546 0.7599 11.00000 0.05 0.43 Q2 1 0.8674 0.5029 0.2435 11.00000 0.05 0.43 ; _shelx_res_checksum 18944 _shelx_hkl_file ; 0 0 4 580.36 14.89 0 0 5 1.70 1.31 0 0 6 107.50 7.98 0 0 7 -0.07 0.42 0 0 8 -0.84 0.63 0 0 9 0.01 0.32 0 0 10 69.20 8.09 0 0 11 -0.80 1.09 0 0 12 352.88 19.96 0 0 13 0.83 0.89 0 0 14 59.16 8.91 0 0 15 -0.10 1.43 0 0 16 272.03 21.02 0 0 17 0.37 1.16 0 0 -18 19.63 5.83 0 0 18 27.03 7.03 0 0 19 1.41 1.39 0 0 -19 -0.72 2.16 0 0 -20 109.68 14.31 0 0 -21 0.25 1.39 0 0 -22 9.00 3.84 0 0 -23 -2.00 2.35 0 0 -24 15.16 4.84 0 0 -25 0.19 1.24 0 0 -26 1.61 1.56 0 0 -27 0.51 1.41 0 0 -28 0.63 0.48 0 0 -29 -0.01 0.65 0 1 -1 0.23 0.07 0 -1 1 -0.10 0.17 0 -1 2 0.03 0.07 0 1 -2 0.22 0.39 0 -1 3 -0.62 0.35 0 -1 4 0.65 0.63 0 -1 5 -1.43 0.88 0 -1 6 2.21 1.63 0 1 7 0.53 0.84 0 -1 7 -1.32 1.25 0 1 8 0.76 1.51 0 -1 8 -0.82 1.18 0 1 9 -1.65 1.53 0 -1 9 -0.15 0.81 0 -1 10 -0.17 0.66 0 1 10 -0.14 0.96 0 1 11 0.51 0.63 0 -1 11 2.20 2.62 0 -1 12 -0.57 1.38 0 1 12 -0.06 1.06 0 1 13 -0.90 1.97 0 -1 13 -0.33 0.88 0 1 14 0.71 0.57 0 -1 14 1.49 1.74 0 1 15 0.37 1.87 0 -1 15 -1.09 1.50 0 1 16 0.33 1.50 0 -1 16 -1.83 2.11 0 1 17 -0.26 1.24 0 -1 17 3.21 3.09 0 1 -17 0.54 1.33 0 1 18 -1.15 1.41 0 1 -18 2.69 2.56 0 -1 -18 0.56 0.97 0 -1 18 -1.96 2.55 0 -1 -19 -0.18 0.58 0 1 -19 0.40 0.40 0 -1 19 0.89 0.54 0 1 19 0.03 1.17 0 -1 -20 1.43 1.05 0 1 -20 0.13 0.72 0 -1 -21 -1.61 2.48 0 1 -21 1.33 2.58 0 1 -22 -1.80 2.78 0 -1 -22 -1.26 2.07 0 -1 -23 -1.35 0.98 0 1 -23 -2.26 1.90 0 1 -24 -0.95 2.47 0 -1 -24 1.29 2.18 0 1 -25 1.06 1.82 0 -1 -25 0.92 1.06 0 1 -26 -0.70 1.65 0 -1 -26 -0.91 1.26 0 1 -27 -0.72 0.47 0 -1 -27 0.32 0.79 0 1 -28 2.80 2.02 0 -1 -28 0.88 1.09 0 -1 -29 -0.68 1.07 0 2 0 1277.22 9.93 0 -2 0 1466.61 9.25 0 -2 1 2745.97 18.27 0 2 -1 2666.74 20.33 0 2 -2 98.97 2.50 0 -2 2 102.87 4.70 0 -2 2 100.53 2.76 0 2 -2 92.40 4.93 0 -2 3 2966.16 16.91 0 -2 3 2795.32 29.22 0 -2 4 2398.28 30.79 0 -2 5 583.00 16.87 0 -2 6 432.92 15.70 0 -2 7 269.85 13.25 0 -2 8 -0.35 0.93 0 2 8 5.02 1.59 0 2 9 93.90 9.13 0 -2 9 0.22 1.06 0 -2 10 62.91 7.64 0 2 10 101.60 10.02 0 2 11 1213.20 36.09 0 -2 11 1241.30 35.82 0 -2 12 4.46 1.65 0 2 12 6.43 2.53 0 2 13 4.15 2.02 0 -2 13 7.06 2.45 0 2 14 29.49 6.18 0 -2 14 34.30 6.85 0 2 15 1.68 1.40 0 -2 15 2.81 2.35 0 2 16 172.68 16.86 0 2 -16 150.23 15.79 0 -2 16 181.45 17.04 0 2 17 32.58 7.70 0 2 -17 29.99 7.25 0 -2 17 45.24 8.81 0 2 18 16.98 5.18 0 -2 18 27.03 7.02 0 2 -18 16.85 5.67 0 2 19 67.50 11.51 0 -2 19 66.65 11.52 0 2 -19 60.24 10.47 0 -2 -19 60.93 10.21 0 2 -20 -0.59 1.38 0 -2 -20 1.94 2.37 0 -2 -21 184.44 18.25 0 2 -21 194.63 19.40 0 2 -22 6.54 3.62 0 -2 -22 7.05 3.63 0 -2 -23 16.79 5.37 0 2 -23 22.56 6.37 0 2 -24 19.85 6.18 0 -2 -24 19.89 5.77 0 -2 -25 13.43 4.32 0 2 -25 8.45 3.71 0 2 -26 2.47 2.45 0 -2 -26 5.56 2.52 0 2 -27 0.50 1.93 0 -2 -27 -0.02 0.48 0 2 -28 1.80 1.29 0 -2 -28 2.58 1.99 0 -2 -29 7.48 2.36 0 -3 0 0.37 0.15 0 3 0 -0.17 0.28 0 3 -1 0.19 0.29 0 -3 1 0.45 0.08 0 -3 2 -0.36 0.54 0 3 -2 -0.03 0.43 0 3 -2 -0.45 0.31 0 3 -3 1.46 0.84 0 -3 3 0.69 0.58 0 -3 3 -0.10 0.24 0 -3 4 -0.13 0.04 0 -3 4 1.06 0.88 0 -3 5 0.29 0.02 0 -3 5 -0.76 0.56 0 -3 6 2.02 1.06 0 -3 6 0.58 0.13 0 -3 7 -0.35 0.41 0 -3 7 0.39 0.52 0 -3 8 1.74 1.63 0 -3 9 2.37 1.60 0 3 9 -0.76 0.46 0 3 10 -0.26 1.09 0 -3 10 0.54 1.40 0 3 11 0.20 1.42 0 -3 11 -0.45 0.51 0 3 12 -0.30 0.62 0 -3 12 0.70 1.64 0 3 13 0.28 0.63 0 -3 13 0.65 1.62 0 3 14 -0.96 1.58 0 -3 14 -0.94 1.62 0 3 -15 0.90 1.08 0 3 15 -0.10 2.11 0 -3 15 0.65 1.52 0 3 -16 -1.36 1.48 0 3 16 -1.32 1.96 0 -3 16 3.56 2.87 0 3 17 3.07 3.21 0 3 -17 0.87 1.70 0 -3 17 2.01 2.23 0 3 -18 1.45 1.19 0 -3 18 0.78 0.99 0 3 18 2.76 3.23 0 -3 -19 -0.51 0.92 0 3 19 2.09 2.63 0 -3 19 0.55 2.14 0 3 -19 -2.99 3.30 0 3 -20 -1.46 0.44 0 -3 -20 -1.49 1.55 0 3 -21 0.34 1.64 0 -3 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77.93 9.50 -8 0 -2 89.82 10.93 -8 0 3 -1.75 1.98 -8 0 -3 0.61 2.28 -8 0 4 1.43 1.66 -8 0 -4 7.09 2.94 -8 0 5 3.01 2.15 -8 0 -5 -0.02 0.95 -8 0 -6 1.99 1.97 -8 0 -7 -0.35 1.17 -8 0 -8 48.56 7.64 8 0 -8 26.93 7.80 -8 0 -9 -1.20 1.71 8 0 -9 -1.24 1.09 -8 0 -10 0.26 1.61 8 0 -10 5.17 2.33 -8 0 -11 1.52 1.79 8 0 -11 1.21 1.07 8 0 -12 12.12 5.20 8 0 -13 3.48 2.96 8 0 -14 18.72 5.59 -8 1 0 2.89 2.34 -8 -1 0 0.39 0.74 -8 1 1 -1.92 1.80 -8 1 -1 0.61 0.61 -8 -1 1 0.02 1.37 -8 -1 -1 1.47 2.33 -8 1 2 -0.97 0.90 -8 1 -2 1.43 1.62 -8 -1 2 -1.21 1.40 -8 -1 -2 -0.04 0.67 -8 1 3 -0.18 1.09 -8 -1 3 0.09 1.23 -8 1 -3 1.84 2.54 -8 -1 -3 -0.80 1.16 -8 1 4 14.51 4.19 -8 -1 4 8.25 2.64 -8 1 -4 22.08 5.49 -8 -1 -4 16.45 4.65 -8 1 5 3.52 2.23 -8 1 -5 3.74 1.79 -8 -1 -5 7.72 2.83 -8 1 6 1.96 0.86 -8 1 -6 5.19 1.92 -8 -1 -6 6.60 2.88 -8 1 -7 5.14 2.37 -8 -1 -7 -0.30 1.69 8 -1 -7 5.87 4.41 -8 1 -8 13.22 4.31 -8 -1 -8 13.90 4.07 8 -1 -8 11.10 5.77 -8 1 -9 -0.35 0.73 -8 -1 -9 -0.33 1.38 8 -1 -9 -0.03 1.25 -8 1 -10 4.94 2.63 -8 -1 -10 2.51 1.79 8 1 -10 4.12 3.00 8 -1 -10 3.29 2.59 -8 1 -11 4.49 2.29 -8 -1 -11 1.85 1.44 8 1 -11 9.64 5.00 8 -1 -11 4.11 2.82 -8 1 -12 1.99 2.17 8 1 -12 -1.74 2.09 8 -1 -12 -1.21 2.11 8 -1 -13 17.53 5.48 8 1 -13 7.66 2.67 8 -1 -14 0.94 1.53 8 -1 -15 9.07 3.59 -8 2 0 57.70 8.75 -8 -2 0 47.02 7.52 -8 2 1 15.79 4.53 -8 2 -1 19.64 5.08 -8 -2 1 16.70 4.35 -8 -2 -1 13.21 3.88 -8 2 2 2.14 1.69 -8 2 -2 3.22 2.85 -8 -2 2 -0.83 0.90 -8 -2 -2 2.88 1.94 -8 2 3 -0.08 0.81 -8 2 -3 2.85 2.79 -8 -2 3 0.80 0.81 -8 -2 -3 3.16 1.69 -8 2 4 1.74 1.27 -8 2 -4 3.26 2.04 -8 -2 -4 4.03 2.64 -8 2 5 0.16 0.45 -8 2 -5 -1.40 1.95 -8 -2 -5 1.62 1.59 -8 2 6 0.97 0.18 -8 2 -6 2.41 1.93 -8 -2 -6 1.89 2.15 -8 2 7 12.56 3.28 -8 2 -7 23.53 5.51 -8 -2 -7 17.93 4.86 8 -2 -7 9.73 4.41 8 -2 -8 32.87 7.87 -8 2 -8 34.40 6.74 -8 -2 -8 33.88 6.50 8 -2 -9 36.15 8.39 -8 2 -9 42.26 7.28 -8 -2 -9 37.54 6.83 -8 2 -10 6.15 2.78 -8 -2 -10 4.86 2.08 8 -2 -10 3.22 2.54 -8 2 -11 -0.66 0.68 8 -2 -11 3.41 3.16 -8 2 -12 -0.31 1.13 8 -2 -12 2.77 1.65 8 -2 -13 5.52 3.02 8 -2 -14 1.19 1.55 8 -2 -15 1.89 2.13 -8 3 0 0.52 0.85 -8 -3 0 1.71 2.01 -8 3 1 4.61 2.55 -8 3 -1 4.35 2.62 -8 -3 1 0.19 4.61 -8 -3 -1 4.21 2.85 -8 3 2 3.55 2.84 -8 3 -2 4.50 2.34 -8 -3 2 1.46 1.17 -8 -3 -2 3.48 2.00 -8 3 3 2.82 1.80 -8 3 -3 2.56 2.20 -8 -3 -3 -0.23 1.19 -8 3 4 7.13 2.69 -8 3 -4 7.86 3.38 -8 -3 -4 11.45 3.73 -8 3 5 3.19 1.77 -8 3 -5 -1.10 2.09 -8 -3 -5 0.58 1.85 -8 3 6 2.83 1.54 -8 3 -6 4.10 2.85 -8 -3 -6 2.40 2.09 -8 3 7 1.75 1.46 -8 3 -7 -0.68 1.55 -8 -3 -7 -0.57 1.60 -8 3 8 3.96 2.00 -8 3 -8 3.29 1.65 -8 -3 -8 3.52 2.91 8 -3 -8 1.17 0.31 -8 3 -9 -0.24 1.07 8 -3 -9 -0.18 1.12 -8 3 -10 5.93 2.90 8 -3 -10 8.90 4.11 -8 3 -11 7.84 2.61 8 -3 -11 8.58 4.33 -8 3 -12 33.44 5.69 8 -3 -12 28.50 6.63 8 -3 -13 -2.45 2.33 8 -3 -14 2.37 1.62 8 -3 -15 1.56 1.50 -8 4 0 10.26 3.66 -8 -4 0 5.43 2.28 -8 4 1 3.58 1.68 -8 4 -1 5.24 2.91 -8 -4 -1 4.54 2.31 -8 4 2 14.11 4.34 -8 4 -2 21.00 5.37 -8 -4 -2 12.59 3.89 -8 4 3 3.17 1.50 -8 4 -3 0.79 1.66 -8 -4 -3 -0.62 1.95 -8 4 4 2.03 1.29 -8 4 -4 3.19 0.96 -8 -4 -4 -0.26 0.51 -8 4 5 7.22 3.23 -8 4 -5 5.40 3.11 -8 -4 -5 3.00 1.88 -8 4 -6 46.31 8.06 -8 -4 -6 45.61 7.36 -8 4 6 33.68 5.95 -8 4 -7 -0.09 0.98 -8 -4 -7 0.47 1.47 -8 4 7 0.63 1.32 -8 4 8 8.17 2.74 -8 4 -8 15.09 4.24 -8 -4 -8 11.12 3.65 -8 4 9 3.19 1.40 8 -4 -9 0.31 0.81 -8 4 -10 0.21 1.47 8 -4 -10 0.15 0.43 8 -4 -11 2.43 2.05 -8 4 -11 1.02 1.14 8 -4 -12 3.46 2.40 -8 4 -12 5.66 2.71 8 -4 -13 0.15 0.36 8 -4 -14 2.10 1.80 8 -4 -15 -0.45 1.06 -8 5 0 12.69 3.95 -8 5 1 -0.02 0.81 -8 5 -1 0.97 1.02 -8 -5 -1 -0.47 1.39 -8 5 2 12.25 3.88 -8 5 -2 7.69 2.87 -8 -5 -2 10.15 3.45 -8 5 -3 2.02 2.54 -8 -5 -3 3.11 1.65 -8 5 3 1.64 1.06 -8 5 -4 2.39 1.75 -8 -5 -4 1.07 1.73 -8 5 4 0.88 0.62 -8 5 -5 0.47 1.26 -8 -5 -5 -0.63 0.88 -8 5 5 -0.78 1.39 -8 5 -6 17.26 4.99 -8 -5 -6 14.83 3.92 -8 5 6 13.27 3.94 -8 5 -7 15.02 4.46 -8 5 7 9.43 2.96 -8 5 -8 1.19 1.50 -8 5 8 2.00 1.55 -8 5 -9 8.06 3.38 -8 5 9 3.02 1.55 -8 5 10 8.27 2.52 8 -5 -10 3.87 2.09 -8 5 -10 8.97 3.01 -8 5 -11 3.30 2.00 8 -5 -11 -0.28 0.85 8 -5 -12 4.15 2.33 -8 5 -12 12.59 3.38 8 -5 -13 1.86 2.17 8 -5 -14 18.11 4.38 -8 6 0 8.65 3.67 -8 6 1 8.40 2.99 -8 6 -1 12.96 4.21 -8 6 -2 7.02 3.17 -8 -6 -2 11.18 3.40 -8 6 2 15.32 4.47 -8 6 -3 3.97 2.34 -8 6 3 2.45 1.56 -8 6 -4 7.59 2.96 -8 6 4 8.63 3.11 -8 6 -5 4.35 2.98 -8 6 5 5.13 2.76 -8 6 -6 0.66 0.86 -8 6 6 0.59 1.28 -8 6 -7 2.53 0.71 -8 6 7 3.88 1.97 -8 6 -8 2.31 1.76 -8 6 8 0.03 0.12 -8 6 -9 4.17 1.82 -8 6 9 2.12 1.29 -8 6 -10 6.43 2.64 -8 6 10 2.13 1.31 8 -6 -11 0.62 1.68 -8 6 -11 -1.62 1.80 8 -6 -12 0.82 0.78 -8 6 -12 4.16 1.67 8 -6 -13 5.11 2.30 -8 7 0 103.41 11.78 -8 7 1 12.62 4.08 -8 7 -1 10.94 3.73 -8 7 -2 1.67 1.58 -8 7 2 0.37 1.26 -8 7 -3 3.16 2.37 -8 7 3 -0.53 0.93 -8 7 -4 18.98 5.10 -8 7 4 23.95 5.68 -8 7 -5 5.94 2.15 -8 7 5 10.41 3.80 -8 7 -6 -0.19 0.68 -8 7 6 1.81 1.86 -8 7 -7 -1.49 1.77 -8 7 7 2.38 1.87 -8 7 -8 -0.99 2.00 -8 7 8 0.87 0.65 -8 7 -9 16.16 4.28 -8 7 9 8.93 2.59 -8 7 -10 21.15 4.55 -8 7 10 13.10 3.00 -8 7 -11 -1.05 1.29 -8 7 11 0.07 0.19 -8 7 -12 2.06 1.37 -8 -8 0 42.33 6.34 -8 8 0 59.17 8.74 -8 8 -1 4.87 2.47 -8 8 1 5.93 3.04 -8 8 -2 5.97 2.93 -8 8 2 5.21 2.49 -8 8 -3 0.41 0.56 -8 8 3 2.66 2.02 -8 8 -4 11.11 4.00 -8 8 4 5.38 2.65 -8 8 -5 -2.17 2.27 -8 8 5 0.25 0.29 -8 8 -6 3.37 1.97 -8 8 6 7.05 2.66 -8 8 -7 1.06 1.01 -8 8 7 3.02 1.86 -8 8 -8 14.39 3.91 -8 8 8 12.16 3.37 -8 8 -9 25.52 4.92 -8 8 9 13.20 3.19 -8 8 -10 -0.37 0.93 -8 8 10 0.42 1.08 -8 8 -11 -0.51 0.59 -8 8 11 0.14 0.59 -8 8 -12 -0.63 0.34 -8 9 0 3.50 2.06 -8 -9 0 2.50 1.79 -8 -9 1 50.77 7.08 -8 9 1 66.64 9.13 -8 9 -1 68.23 9.17 -8 9 -2 4.48 2.33 -8 9 2 7.90 3.00 -8 9 -3 -0.68 1.05 -8 9 3 1.35 1.79 -8 9 -4 4.68 1.86 -8 9 4 5.78 2.31 -8 9 5 62.61 8.16 -8 9 -5 57.11 8.17 -8 9 -6 7.07 3.23 -8 9 6 4.59 2.07 -8 9 -7 9.04 3.20 -8 9 7 7.76 2.68 -8 9 -8 0.54 0.78 -8 9 8 0.39 0.30 -8 9 -9 0.23 0.71 -8 9 9 0.78 0.74 -8 9 -10 0.46 0.94 -8 9 10 1.20 1.06 -8 9 -11 3.90 1.73 -8 9 11 1.84 1.01 -8 -10 0 104.35 9.45 -8 10 0 140.04 12.84 -8 10 -1 0.16 0.83 -8 -10 1 0.68 1.17 -8 -10 -1 0.98 0.78 -8 10 1 0.90 1.05 -8 10 -2 0.81 1.14 -8 -10 2 0.41 0.82 -8 10 2 0.79 0.30 -8 10 -3 13.10 3.88 -8 -10 3 15.98 3.90 -8 10 3 10.99 3.23 -8 10 -4 6.14 1.85 -8 10 4 3.88 1.66 -8 10 -5 1.73 1.72 -8 10 5 4.14 1.94 -8 10 -6 33.35 5.69 -8 10 6 30.87 5.38 -8 10 -7 9.21 2.86 -8 10 7 11.99 3.28 -8 10 -8 14.50 3.44 -8 10 8 15.62 3.42 -8 10 -9 1.31 1.16 -8 10 9 -0.10 0.68 -8 10 -10 1.45 0.93 -8 10 10 1.99 0.84 -8 11 0 5.34 2.03 -8 -11 0 5.85 2.18 -8 11 -1 21.86 4.97 -8 -11 1 20.73 4.29 -8 -11 -1 15.15 3.63 -8 11 1 22.36 5.30 -8 11 -2 1.03 1.12 -8 -11 2 -1.03 1.13 -8 11 -3 1.33 0.51 -8 -11 3 0.15 0.75 -8 11 3 2.47 1.75 -8 -11 4 40.31 5.92 -8 11 4 48.09 7.00 -8 11 -4 47.27 6.93 -8 11 -5 0.70 0.52 -8 11 5 0.02 0.13 -8 11 -6 2.10 1.28 -8 11 6 0.97 1.21 -8 11 -7 20.87 4.30 -8 11 7 18.49 3.97 -8 11 -8 2.45 1.50 -8 11 8 2.37 1.65 -8 11 -9 0.99 1.19 -8 11 9 0.51 0.83 -8 11 10 1.54 0.94 -8 -12 0 91.28 8.11 -8 12 0 132.32 11.62 -8 12 1 44.63 6.96 -8 12 -1 49.76 6.94 -8 -12 1 25.57 4.43 -8 -12 -1 25.19 4.18 -8 12 -2 4.02 1.48 -8 -12 2 4.47 2.07 -8 12 2 8.20 2.99 -8 12 -3 31.27 5.53 -8 12 3 40.79 6.53 -8 -12 3 30.18 4.85 -8 -12 4 37.10 5.41 -8 12 4 40.13 6.34 -8 12 -4 43.28 6.29 -8 12 -5 5.24 2.23 -8 -12 5 2.65 1.91 -8 12 5 6.44 2.62 -8 12 -6 6.14 2.35 -8 -12 6 6.75 2.16 -8 12 6 8.37 2.43 -8 12 -7 0.24 0.19 -8 -12 7 0.17 0.23 -8 12 7 -0.15 0.55 -8 -12 8 1.66 1.06 -8 12 8 1.81 1.01 -8 -12 9 1.21 0.98 -8 12 9 2.01 1.30 -8 -12 10 -0.04 0.22 -8 -13 0 72.68 6.80 -8 13 0 115.93 10.17 -8 -13 -1 2.77 1.38 -8 13 1 4.20 1.89 -8 -13 1 2.78 1.65 -8 13 2 16.30 3.79 -8 13 -2 21.60 4.30 -8 -13 2 9.78 2.57 -8 13 -3 25.53 4.78 -8 -13 3 23.58 4.02 -8 13 3 28.81 5.13 -8 13 -4 17.37 3.82 -8 -13 4 11.95 2.95 -8 13 4 10.38 3.17 -8 13 -5 8.91 2.66 -8 -13 5 8.91 2.53 -8 13 5 7.58 2.48 -8 13 -6 12.48 2.82 -8 -13 6 21.26 3.69 -8 13 6 19.77 3.97 -8 -13 7 0.81 0.92 -8 13 7 -0.88 1.17 -8 -13 8 -1.13 0.65 -8 13 8 -0.02 0.74 -8 14 0 1.67 1.49 -8 14 1 5.38 2.20 -8 14 -1 3.17 1.59 -8 -14 1 1.36 0.84 -8 14 2 2.15 1.21 -8 14 -2 4.83 1.96 -8 -14 2 1.94 1.17 -8 14 3 0.81 0.80 -8 14 -3 0.28 0.80 -8 -14 3 -0.42 0.39 -8 -14 4 2.20 1.32 -8 14 4 3.21 1.64 -8 -14 5 0.27 0.32 -8 14 5 1.14 1.24 -8 14 6 0.73 1.13 -9 0 0 -0.53 0.70 -9 0 1 -0.95 0.98 -9 0 -1 -1.06 1.13 -9 0 -2 1.45 0.88 -9 0 -3 1.22 1.19 -9 0 -4 21.00 3.91 -9 0 -5 -0.35 0.89 -9 0 -6 5.23 2.08 -9 0 -7 0.06 0.65 -9 1 0 -0.68 0.68 -9 -1 0 2.31 1.16 -9 1 1 2.08 1.39 -9 1 -1 0.37 0.73 -9 -1 -1 0.11 0.74 -9 1 2 3.09 1.70 -9 1 -2 2.31 1.42 -9 -1 -2 0.37 0.80 -9 1 -3 1.09 0.92 -9 -1 -3 2.05 0.92 -9 1 -4 6.60 2.21 -9 -1 -4 4.93 1.90 -9 1 -5 2.02 1.21 -9 -1 -5 2.42 1.19 -9 1 -6 10.27 2.66 -9 -1 -6 12.02 2.86 -9 1 -7 3.18 1.42 -9 1 -8 1.43 1.11 -9 2 0 0.40 0.80 -9 2 1 1.60 1.22 -9 2 -1 2.24 1.40 -9 -2 -1 1.94 1.15 -9 2 2 -0.01 0.37 -9 2 -2 -0.90 1.06 -9 -2 -2 0.05 0.26 -9 2 3 -0.10 0.33 -9 2 -3 -0.04 0.72 -9 -2 -3 0.61 0.97 -9 2 -4 -0.10 0.83 -9 -2 -4 1.33 1.17 -9 2 -5 0.72 0.85 -9 2 -6 1.98 1.29 -9 2 -7 0.53 0.97 -9 2 -8 3.30 1.97 -9 3 0 1.31 1.08 -9 3 1 8.07 2.35 -9 3 -1 7.52 2.29 -9 3 2 3.11 1.56 -9 3 -2 4.13 1.83 -9 3 3 0.84 0.75 -9 3 -3 0.41 0.56 -9 3 4 0.84 1.02 -9 3 -4 2.20 1.44 -9 3 -5 2.65 1.61 -9 3 -6 -0.75 0.87 -9 3 -7 7.29 2.33 -9 3 -8 0.72 0.94 -9 4 0 0.03 0.77 -9 4 1 -0.57 1.20 -9 4 -1 3.02 1.61 -9 4 2 1.27 1.01 -9 4 -2 -1.51 1.39 -9 4 3 4.20 1.76 -9 4 -3 4.97 1.91 -9 4 4 13.64 2.74 -9 4 -4 18.44 3.77 -9 4 -5 1.36 1.49 -9 4 -6 4.41 1.64 -9 4 -7 2.93 1.23 -9 4 -8 3.24 1.47 -9 4 -9 8.08 2.28 -9 5 0 -0.30 0.29 -9 5 1 2.18 1.48 -9 5 -1 -0.51 0.75 -9 5 2 4.55 1.99 -9 5 -2 1.28 1.02 -9 5 3 2.48 1.41 -9 5 -3 3.12 1.18 -9 5 4 2.76 1.54 -9 5 -4 2.45 1.40 -9 5 -5 1.76 1.40 -9 5 -6 -0.11 0.45 -9 5 -7 3.82 1.66 -9 5 -8 1.07 0.67 -9 6 0 1.89 1.30 -9 6 1 5.85 2.00 -9 6 -1 3.56 1.70 -9 6 2 0.27 0.39 -9 6 -2 -0.76 1.19 -9 6 3 13.84 2.88 -9 6 -3 17.78 3.62 -9 6 4 1.36 1.01 -9 6 -4 0.66 1.07 -9 6 -5 17.38 3.43 -9 6 -6 9.16 2.46 -9 6 -7 15.36 3.10 -9 7 0 -0.62 0.76 -9 7 1 3.35 1.61 -9 7 -1 0.31 0.63 -9 7 2 0.07 0.73 -9 7 -2 -0.52 0.93 -9 7 3 3.01 1.52 -9 7 -3 2.40 1.54 -9 7 4 15.08 2.95 -9 7 -4 16.06 3.36 -9 7 -5 1.05 1.29 -9 7 -6 1.19 1.12 -9 8 0 1.42 1.31 -9 8 1 -0.56 0.99 -9 8 -1 2.30 1.63 -9 8 2 -0.03 0.47 -9 8 -2 0.61 0.88 -9 8 3 -0.28 0.72 -9 8 -3 1.59 1.15 -9 8 -4 -0.24 0.44 -9 8 -5 10.89 2.56 -9 9 0 0.90 1.12 -9 9 1 2.63 0.93 -9 9 -1 4.00 1.84 -9 9 2 0.55 0.92 -9 9 -2 -0.53 0.72 -9 9 -3 1.58 0.84 TITL DM-SKP-3-46_Cu in Pbca REM Pbca (#61 in standard setting) CELL 1.54184 7.727506 22.433704 24.254444 90.0000 90.0000 90.0000 ZERR 18.00 0.000142 0.000438 0.000463 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 198.00 180.00 18.00 18.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' ; _shelx_hkl_checksum 46249 _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 2.294 _oxdiff_exptl_absorpt_empirical_full_min 0.652