data_2 _audit_creation_date 2015-07-11 _audit_creation_method ; Olex2 1.2 (compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) ; _shelxl_version_number 2013-2 _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _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. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C68 H104 Cl2 Cu10 N4' _chemical_formula_sum 'C68 H104 Cl2 Cu10 N4' _chemical_formula_weight 1683.85 _chemical_absolute_configuration ? _chemical_melting_point ? _chemical_oxdiff_formula 'C104 H208 S2 Cu12' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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 18 _space_group_name_H-M_alt 'P 21 21 2' _space_group_name_Hall 'P 2 2ab' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z' _cell_length_a 12.9980(4) _cell_length_b 15.8415(5) _cell_length_c 18.0179(6) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3710.0(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4829 _cell_measurement_temperature 180.00(10) _cell_measurement_theta_max 27.6600 _cell_measurement_theta_min 3.3900 _shelx_estimated_absorpt_T_max 0.868 _shelx_estimated_absorpt_T_min 0.759 _exptl_absorpt_coefficient_mu 2.915 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.91684 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'metallic dark black' _exptl_crystal_colour_lustre metallic _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary black _exptl_crystal_density_diffrn 1.507 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 1728 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0284 _diffrn_reflns_av_unetI/netI 0.0509 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 11888 _diffrn_reflns_point_group_measured_fraction_full 0.950 _diffrn_reflns_point_group_measured_fraction_max 0.941 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.021 _diffrn_reflns_theta_min 2.809 _diffrn_ambient_temperature 180.00(10) _diffrn_detector_area_resol_mean 10.3914 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -31.00 60.00 1.0000 28.0800 omega____ theta____ kappa____ phi______ frames - -11.4829 0.0000 30.0000 91 #__ type_ start__ end____ width___ exp.time_ 2 omega -101.00 -57.00 1.0000 28.0800 omega____ theta____ kappa____ phi______ frames - -11.4829 0.0000 30.0000 44 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0279227000 _diffrn_orient_matrix_UB_12 -0.0246433000 _diffrn_orient_matrix_UB_13 -0.0259555000 _diffrn_orient_matrix_UB_21 0.0335792000 _diffrn_orient_matrix_UB_22 0.0135118000 _diffrn_orient_matrix_UB_23 -0.0286890000 _diffrn_orient_matrix_UB_31 0.0327424000 _diffrn_orient_matrix_UB_32 -0.0348521000 _diffrn_orient_matrix_UB_33 0.0072399000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.693 _reflns_Friedel_fraction_full 0.891 _reflns_Friedel_fraction_max 0.871 _reflns_number_gt 5811 _reflns_number_total 6894 _reflns_odcompleteness_completeness 99.51 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 25.97 _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, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'ShelXS (Sheldrick, 2008)' _refine_diff_density_max 1.049 _refine_diff_density_min -0.403 _refine_diff_density_rms 0.090 _refine_ls_abs_structure_details ; Flack x determined using 2140 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.369(12) _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 388 _refine_ls_number_reflns 6894 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0563 _refine_ls_R_factor_gt 0.0411 _refine_ls_restrained_S_all 1.072 _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^)+(0.0470P)^2^+3.7080P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0956 _refine_ls_wR_factor_ref 0.1042 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Others Fixed U13: Cu6(0) Cu5(0) Fixed U23: Cu6(0) Cu5(0) Fixed Uiso: H5(0.041) H13(0.049) H20A(0.048) H20B(0.048) H8(0.052) H23A(0.043) H23B(0.043) H27A(0.054) H27B(0.054) H26A(0.048) H26B(0.048) H24A(0.067) H24B(0.067) H16(0.06) H7(0.058) H17A(0.059) H17B(0.059) H19A(0.095) H19B(0.095) H19C(0.095) H21A(0.062) H21B(0.062) H6(0.056) H25A(0.107) H25B(0.107) H25C(0.107) H14(0.069) H15(0.083) H18A(0.089) H18B(0.089) H28A(0.098) H28B(0.098) H28C(0.098) H22A(0.113) H22B(0.113) H22C(0.113) H31A(0.103) H31B(0.103) H32A(0.131) H32B(0.131) H29A(0.164) H29B(0.164) H29C(0.164) H34A(0.173) H34B(0.173) H34C(0.173) H33A(0.135) H33B(0.135) H33C(0.135) H30A(0.174) H30B(0.174) H30C(0.174) Fixed X: Cu6(0) Cu5(0) H5(0.2866) H13(-0.1102) H20A(-0.0711) H20B(0.0132) H8(0.0599) H23A(-0.2231) H23B(-0.1343) H27A(-0.3731) H27B(-0.3098) H26A(- 0.3374) H26B(-0.3851) H24A(-0.1004) H24B(-0.0092) H16(-0.3536) H7(0.1961) H17A(-0.167) H17B(-0.226) H19A(-0.3106) H19B(-0.3081) H19C(-0.3564) H21A(- 0.109) H21B(-0.1934) H6(0.3121) H25A(-0.0352) H25B(-0.1563) H25C(-0.0777) H14(- 0.238) H15(-0.359) H18A(-0.1457) H18B(-0.1966) H28A(-0.4569) H28B(-0.4819) H28C(-0.5202) H22A(-0.2279) H22B(-0.1092) H22C(-0.1726) H31A(0.3643) H31B(0.2949) H32A(0.4304) H32B(0.4317) H29A(0.0883) H29B(0.1662) H29C(0.1273) H34A(0.374) H34B(0.4665) H34C(0.4404) H33A(0.2871) H33B(0.3935) H33C(0.2882) H30A(0.3034) H30B(0.2985) H30C(0.1974) Fixed Y: Cu6(0) Cu5(0) H5(0.1387) H13(-0.0509) H20A(0.418) H20B(0.405) H8(0.3104) H23A(0.061) H23B(-0.0083) H27A(0.1757) H27B(0.1636) H26A(0.0131) H26B(0.0306) H24A(0.1702) H24B(0.1024) H16(0.1108) H7(0.2512) H17A(0.3617) H17B(0.2754) H19A(0.3886) H19B(0.3384) H19C(0.295) H21A(0.3292) H21B(0.3425) H6(0.1675) H25A(0.1477) H25B(0.1307) H25C(0.053) H14(0.0222) H15(0.1032) H18A(0.3278) H18B(0.2375) H28A(0.1052) H28B(0.1979) H28C(0.1167) H22A(0.4451) H22B(0.4708) H22C(0.4944) H31A(0.4293) H31B(0.393) H32A(0.3169) H32B(0.3096) H29A(0.4175) H29B(0.4812) H29C(0.3986) H34A(0.1132) H34B(0.1539) H34C(0.1885) H33A(0.2407) H33B(0.1903) H33C(0.1452) H30A(0.3615) H30B(0.457) H30C(0.4126) Fixed Z: H5(0.1878) H13(0.4431) H20A(0.1975) H20B(0.1339) H8(0.0611) H23A(0.0774) H23B(0.0704) H27A(0.2026) H27B(0.1272) H26A(0.1392) H26B(0.2194) H24A(0.07) H24B(0.0674) H16(0.3161) H7(0.0002) H17A(0.2625) H17B(0.2476) H19A(0.3506) H19B(0.4277) H19C(0.3555) H21A(0.0616) H21B(0.1253) H6(0.0638) H25A(-0.0527) H25B(-0.0473) H25C(-0.0491) H14(0.5087) H15(0.444) H18A(0.3833) H18B(0.3698) H28A(0.07) H28B(0.1005) H28C(0.1455) H22A(0.039) H22B(0.0322) H22C(0.1055) H31A(0.3413) H31B(0.4069) H32A(0.4059) H32B(0.3178) H29A(0.3017) H29B(0.3417) H29C(0.3843) H34A(0.3231) H34B(0.3695) H34C(0.2882) H33A(0.4693) H33B(0.4637) H33C(0.4403) H30A(0.2067) H30B(0.2354) H30C(0.203) ; _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 Cu6 Cu 0.0000 0.0000 0.19217(7) 0.0277(3) Uani 1 2 d S T P . . Cu3 Cu 0.11597(7) 0.10960(5) 0.27305(5) 0.0289(2) Uani 1 1 d . . . . . Cu5 Cu 0.0000 0.0000 0.32486(7) 0.0325(3) Uani 1 2 d S T P . . Cu4 Cu -0.07378(7) 0.13724(5) 0.23435(5) 0.0316(2) Uani 1 1 d . . . . . Cu2 Cu 0.00748(8) 0.21613(6) 0.33661(5) 0.0379(2) Uani 1 1 d . . . . . Cu1 Cu 0.20631(8) 0.24036(6) 0.30169(6) 0.0417(3) Uani 1 1 d . . . . . Cl1 Cl 0.0659(2) 0.2398(2) 0.44549(13) 0.0703(8) Uani 1 1 d . . . . . C12 C -0.1506(5) -0.0116(5) 0.3387(4) 0.0321(16) Uani 1 1 d . . . . . C3 C 0.0827(6) 0.2567(4) 0.1625(4) 0.0324(17) Uani 1 1 d . . . . . C11 C -0.2258(6) 0.0391(5) 0.3003(5) 0.0344(18) Uani 1 1 d . . . . . C4 C 0.1508(6) 0.2040(5) 0.2024(4) 0.0326(17) Uani 1 1 d . . . . . C10 C -0.2263(6) 0.0448(5) 0.2172(5) 0.0319(17) Uani 1 1 d . . . . . C5 C 0.2379(6) 0.1728(5) 0.1624(4) 0.0339(18) Uani 1 1 d . . . . . H5 H 0.2866 0.1387 0.1878 0.041 Uiso 1 1 calc R . . . . C2 C -0.0132(6) 0.2961(4) 0.1947(4) 0.0334(17) Uani 1 1 d . . . . . C1 C -0.0692(6) 0.2610(5) 0.2504(4) 0.0350(17) Uani 1 1 d . . . . . N2 N 0.3390(5) 0.2280(5) 0.3666(4) 0.0504(18) Uani 1 1 d . U . . . C13 C -0.1582(6) -0.0172(5) 0.4167(4) 0.041(2) Uani 1 1 d . . . . . H13 H -0.1102 -0.0509 0.4431 0.049 Uiso 1 1 calc R . . . . C20 C -0.0471(7) 0.3788(5) 0.1584(4) 0.0397(19) Uani 1 1 d . . . . . H20A H -0.0711 0.4180 0.1975 0.048 Uiso 1 1 calc R . . . . H20B H 0.0132 0.4050 0.1339 0.048 Uiso 1 1 calc R . . . . C8 C 0.1045(7) 0.2736(5) 0.0876(5) 0.043(2) Uani 1 1 d . . . . . H8 H 0.0599 0.3104 0.0611 0.052 Uiso 1 1 calc R . . . . C23 C -0.1507(6) 0.0484(5) 0.0903(4) 0.0359(18) Uani 1 1 d . . . . . H23A H -0.2231 0.0610 0.0774 0.043 Uiso 1 1 calc R . . . . H23B H -0.1343 -0.0083 0.0704 0.043 Uiso 1 1 calc R . . . . C27 C -0.3652(6) 0.1394(5) 0.1582(5) 0.045(2) Uani 1 1 d . . . . . H27A H -0.3731 0.1757 0.2026 0.054 Uiso 1 1 calc R . . . . H27B H -0.3098 0.1636 0.1272 0.054 Uiso 1 1 calc R . . . . C26 C -0.3342(6) 0.0511(5) 0.1828(5) 0.040(2) Uani 1 1 d . . . . . H26A H -0.3374 0.0131 0.1392 0.048 Uiso 1 1 calc R . . . . H26B H -0.3851 0.0306 0.2194 0.048 Uiso 1 1 calc R . . . . C24 C -0.0814(8) 0.1130(6) 0.0525(5) 0.056(2) Uani 1 1 d . . . . . H24A H -0.1004 0.1702 0.0700 0.067 Uiso 1 1 calc R . . . . H24B H -0.0092 0.1024 0.0674 0.067 Uiso 1 1 calc R . . . . C16 C -0.3026(7) 0.0790(6) 0.3415(5) 0.050(2) Uani 1 1 d . . . . . H16 H -0.3536 0.1108 0.3161 0.060 Uiso 1 1 calc R . . . . C7 C 0.1862(7) 0.2400(6) 0.0515(5) 0.049(2) Uani 1 1 d . . . . . H7 H 0.1961 0.2512 0.0002 0.058 Uiso 1 1 calc R . . . . C9 C -0.1406(6) 0.0461(5) 0.1735(4) 0.0337(18) Uani 1 1 d . . . . . N1 N 0.2344(8) 0.3740(5) 0.3059(5) 0.075(3) Uani 1 1 d . . . . . C17 C -0.1695(7) 0.3013(6) 0.2766(5) 0.049(2) Uani 1 1 d . . . . . H17A H -0.1670 0.3617 0.2625 0.059 Uiso 1 1 calc R . . . . H17B H -0.2260 0.2754 0.2476 0.059 Uiso 1 1 calc R . . . . C19 C -0.3025(7) 0.3329(7) 0.3737(6) 0.063(3) Uani 1 1 d . . . . . H19A H -0.3106 0.3886 0.3506 0.095 Uiso 1 1 calc GR . . . . H19B H -0.3081 0.3384 0.4277 0.095 Uiso 1 1 calc GR . . . . H19C H -0.3564 0.2950 0.3555 0.095 Uiso 1 1 calc GR . . . . C21 C -0.1326(8) 0.3682(6) 0.1011(5) 0.051(2) Uani 1 1 d . . . . . H21A H -0.1090 0.3292 0.0616 0.062 Uiso 1 1 calc R . . . . H21B H -0.1934 0.3425 0.1253 0.062 Uiso 1 1 calc R . . . . C6 C 0.2539(7) 0.1902(6) 0.0887(5) 0.047(2) Uani 1 1 d . . . . . H6 H 0.3121 0.1675 0.0638 0.056 Uiso 1 1 calc R . . . . C25 C -0.0882(10) 0.1109(7) -0.0316(5) 0.072(3) Uani 1 1 d . . . . . H25A H -0.0352 0.1477 -0.0527 0.107 Uiso 1 1 calc GR . . . . H25B H -0.1563 0.1307 -0.0473 0.107 Uiso 1 1 calc GR . . . . H25C H -0.0777 0.0530 -0.0491 0.107 Uiso 1 1 calc GR . . . . C14 C -0.2351(8) 0.0259(6) 0.4561(5) 0.058(3) Uani 1 1 d . . . . . H14 H -0.2380 0.0222 0.5087 0.069 Uiso 1 1 calc R . . . . C15 C -0.3068(9) 0.0738(7) 0.4176(7) 0.069(3) Uani 1 1 d . . . . . H15 H -0.3590 0.1032 0.4440 0.083 Uiso 1 1 calc R . . . . C18 C -0.1984(8) 0.2973(8) 0.3540(6) 0.074(3) Uani 1 1 d . . . . . H18A H -0.1457 0.3278 0.3833 0.089 Uiso 1 1 calc R . . . . H18B H -0.1966 0.2375 0.3698 0.089 Uiso 1 1 calc R . . . . C28 C -0.4648(7) 0.1398(7) 0.1147(6) 0.065(3) Uani 1 1 d . . . . . H28A H -0.4569 0.1052 0.0700 0.098 Uiso 1 1 calc GR . . . . H28B H -0.4819 0.1979 0.1005 0.098 Uiso 1 1 calc GR . . . . H28C H -0.5202 0.1167 0.1455 0.098 Uiso 1 1 calc GR . . . . C22 C -0.1633(10) 0.4521(6) 0.0664(6) 0.075(4) Uani 1 1 d . . . . . H22A H -0.2279 0.4451 0.0390 0.113 Uiso 1 1 calc GR . . . . H22B H -0.1092 0.4708 0.0322 0.113 Uiso 1 1 calc GR . . . . H22C H -0.1726 0.4944 0.1055 0.113 Uiso 1 1 calc GR . . . . C31 C 0.3218(10) 0.3805(7) 0.3567(8) 0.085(4) Uani 1 1 d . . . . . H31A H 0.3643 0.4293 0.3413 0.103 Uiso 1 1 calc R . . . . H31B H 0.2949 0.3930 0.4069 0.103 Uiso 1 1 calc R . . . . C32 C 0.3860(12) 0.3096(9) 0.3618(10) 0.109(4) Uani 1 1 d . U . . . H32A H 0.4304 0.3169 0.4059 0.131 Uiso 1 1 calc R . . . . H32B H 0.4317 0.3096 0.3178 0.131 Uiso 1 1 calc R . . . . C29 C 0.1467(12) 0.4218(8) 0.3359(10) 0.109(5) Uani 1 1 d . U . . . H29A H 0.0883 0.4175 0.3017 0.164 Uiso 1 1 calc GR . . . . H29B H 0.1662 0.4812 0.3417 0.164 Uiso 1 1 calc GR . . . . H29C H 0.1273 0.3986 0.3843 0.164 Uiso 1 1 calc GR . . . . C34 C 0.4111(10) 0.1656(11) 0.3341(9) 0.115(5) Uani 1 1 d . U . . . H34A H 0.3740 0.1132 0.3231 0.173 Uiso 1 1 calc GR . . . . H34B H 0.4665 0.1539 0.3695 0.173 Uiso 1 1 calc GR . . . . H34C H 0.4404 0.1885 0.2882 0.173 Uiso 1 1 calc GR . . . . C33 C 0.3260(9) 0.1988(10) 0.4407(7) 0.090(4) Uani 1 1 d . U . . . H33A H 0.2871 0.2407 0.4693 0.135 Uiso 1 1 calc GR . . . . H33B H 0.3935 0.1903 0.4637 0.135 Uiso 1 1 calc GR . . . . H33C H 0.2882 0.1452 0.4403 0.135 Uiso 1 1 calc GR . . . . C30 C 0.2606(13) 0.4037(9) 0.2317(8) 0.116(5) Uani 1 1 d . U . . . H30A H 0.3034 0.3615 0.2067 0.174 Uiso 1 1 calc GR . . . . H30B H 0.2985 0.4570 0.2354 0.174 Uiso 1 1 calc GR . . . . H30C H 0.1974 0.4126 0.2030 0.174 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 Cu6 0.0257(6) 0.0303(6) 0.0271(6) 0.000 0.000 0.0033(6) Cu3 0.0306(4) 0.0290(4) 0.0270(5) 0.0008(4) -0.0020(4) 0.0009(4) Cu5 0.0300(6) 0.0395(7) 0.0282(7) 0.000 0.000 -0.0024(6) Cu4 0.0327(4) 0.0314(4) 0.0306(5) -0.0027(4) -0.0035(4) 0.0037(4) Cu2 0.0427(5) 0.0455(6) 0.0256(5) -0.0052(4) -0.0038(5) 0.0093(5) Cu1 0.0510(6) 0.0374(5) 0.0366(6) -0.0014(4) -0.0139(5) -0.0068(5) Cl1 0.0597(14) 0.113(2) 0.0378(13) -0.0256(14) -0.0156(11) 0.0286(16) C12 0.030(4) 0.038(4) 0.029(4) -0.002(4) 0.002(3) -0.003(3) C3 0.042(4) 0.024(3) 0.031(4) 0.000(3) -0.003(3) -0.003(3) C11 0.031(4) 0.033(4) 0.040(5) -0.009(4) 0.004(4) -0.001(3) C4 0.042(4) 0.032(4) 0.024(4) -0.004(3) 0.000(3) 0.000(4) C10 0.027(4) 0.026(4) 0.043(5) -0.004(3) 0.004(3) 0.001(3) C5 0.033(4) 0.035(4) 0.034(4) 0.002(3) -0.007(3) -0.009(3) C2 0.049(4) 0.028(3) 0.023(4) 0.000(3) -0.009(4) -0.004(4) C1 0.041(4) 0.033(4) 0.031(4) -0.004(3) -0.007(4) 0.006(3) N2 0.045(4) 0.062(4) 0.045(4) -0.001(4) -0.014(4) -0.004(4) C13 0.044(5) 0.047(5) 0.032(4) -0.006(4) 0.007(4) -0.002(4) C20 0.057(5) 0.029(4) 0.032(4) 0.000(3) -0.006(4) 0.005(4) C8 0.052(5) 0.045(5) 0.033(4) 0.009(4) -0.007(4) -0.004(4) C23 0.032(4) 0.040(4) 0.035(5) -0.006(4) -0.007(4) 0.004(4) C27 0.037(4) 0.046(5) 0.051(5) 0.008(4) -0.007(4) 0.009(4) C26 0.028(4) 0.043(4) 0.050(5) 0.006(4) -0.001(4) -0.003(4) C24 0.073(6) 0.051(5) 0.043(5) 0.009(4) -0.010(5) -0.006(5) C16 0.049(5) 0.051(5) 0.050(6) -0.002(4) 0.009(5) 0.019(4) C7 0.053(5) 0.065(6) 0.029(5) 0.008(4) 0.007(4) -0.014(5) C9 0.034(4) 0.033(4) 0.034(4) -0.008(3) -0.010(4) 0.008(3) N1 0.112(7) 0.039(4) 0.073(6) 0.000(4) -0.043(6) -0.018(5) C17 0.053(5) 0.050(5) 0.045(5) 0.000(4) 0.001(4) 0.017(4) C19 0.048(5) 0.090(8) 0.053(6) 0.006(6) 0.015(5) 0.021(6) C21 0.064(6) 0.049(5) 0.041(5) 0.006(4) -0.014(5) 0.008(5) C6 0.043(5) 0.059(6) 0.039(5) 0.000(4) 0.009(4) 0.002(4) C25 0.106(9) 0.067(6) 0.041(6) 0.007(5) 0.001(6) -0.002(7) C14 0.069(6) 0.069(6) 0.035(5) -0.012(5) 0.016(5) 0.010(6) C15 0.067(7) 0.066(7) 0.075(8) -0.019(6) 0.023(6) 0.018(6) C18 0.060(6) 0.109(9) 0.053(7) 0.021(6) 0.016(5) 0.032(7) C28 0.036(5) 0.082(7) 0.078(7) 0.023(6) -0.011(5) 0.004(5) C22 0.110(10) 0.057(6) 0.059(7) -0.009(5) -0.024(7) 0.036(7) C31 0.105(9) 0.054(7) 0.097(9) -0.014(6) -0.048(8) -0.017(7) C32 0.110(7) 0.099(6) 0.118(7) 0.002(5) -0.027(6) -0.033(5) C29 0.127(10) 0.065(7) 0.136(10) -0.027(7) -0.036(9) 0.013(7) C34 0.084(8) 0.171(11) 0.091(8) -0.022(8) -0.015(7) 0.036(8) C33 0.064(6) 0.143(9) 0.064(7) 0.025(7) -0.020(6) -0.014(7) C30 0.166(11) 0.084(7) 0.099(9) 0.025(7) -0.032(8) -0.049(8) _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 Cu6 Cu3 2.7221(11) 2 ? Cu6 Cu3 2.7221(11) . ? Cu6 Cu5 2.3909(18) . ? Cu6 Cu4 2.4948(9) . ? Cu6 Cu4 2.4947(9) 2 ? Cu6 C9 1.997(7) . ? Cu6 C9 1.997(7) 2 ? Cu3 Cu5 2.4815(10) . ? Cu3 Cu4 2.6002(12) . ? Cu3 Cu2 2.4796(13) . ? Cu3 Cu1 2.4364(13) . ? Cu3 C12 2.003(7) 2 ? Cu3 C4 2.015(8) . ? Cu5 Cu3 2.4816(10) 2 ? Cu5 Cu4 2.8820(11) . ? Cu5 Cu4 2.8819(11) 2 ? Cu5 C12 1.982(7) . ? Cu5 C12 1.982(7) 2 ? Cu4 Cu2 2.4642(13) . ? Cu4 C10 2.483(7) . ? Cu4 C1 1.983(7) . ? Cu4 C9 2.010(8) . ? Cu2 Cu1 2.6874(15) . ? Cu2 Cl1 2.137(2) . ? Cu2 C1 1.977(7) . ? Cu1 C4 2.013(7) . ? Cu1 N2 2.093(7) . ? Cu1 N1 2.149(8) . ? C12 Cu3 2.003(7) 2 ? C12 C11 1.441(11) . ? C12 C13 1.412(11) . ? C3 C4 1.414(10) . ? C3 C2 1.510(11) . ? C3 C8 1.405(11) . ? C11 C10 1.500(11) . ? C11 C16 1.395(11) . ? C4 C5 1.431(11) . ? C10 C26 1.538(11) . ? C10 C9 1.365(11) . ? C5 H5 0.9500 . ? C5 C6 1.371(12) . ? C2 C1 1.359(11) . ? C2 C20 1.530(10) . ? C1 C17 1.526(11) . ? N2 C32 1.433(15) . ? N2 C34 1.482(15) . ? N2 C33 1.423(13) . ? C13 H13 0.9500 . ? C13 C14 1.402(12) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C20 C21 1.526(12) . ? C8 H8 0.9500 . ? C8 C7 1.355(12) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 C24 1.525(12) . ? C23 C9 1.505(11) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C27 C26 1.521(11) . ? C27 C28 1.514(12) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C24 C25 1.518(13) . ? C16 H16 0.9500 . ? C16 C15 1.376(15) . ? C7 H7 0.9500 . ? C7 C6 1.360(13) . ? N1 C31 1.464(13) . ? N1 C29 1.471(17) . ? N1 C30 1.458(17) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C17 C18 1.446(14) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C19 C18 1.508(13) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C21 C22 1.523(12) . ? C6 H6 0.9500 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C14 H14 0.9500 . ? C14 C15 1.388(15) . ? C15 H15 0.9500 . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C31 C32 1.402(18) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 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 Cu3 Cu6 Cu3 115.27(6) . 2 ? Cu5 Cu6 Cu3 57.63(3) . . ? Cu5 Cu6 Cu3 57.63(3) . 2 ? Cu5 Cu6 Cu4 72.26(3) . . ? Cu5 Cu6 Cu4 72.26(3) . 2 ? Cu4 Cu6 Cu3 59.60(3) 2 2 ? Cu4 Cu6 Cu3 100.36(4) 2 . ? Cu4 Cu6 Cu3 100.36(4) . 2 ? Cu4 Cu6 Cu3 59.60(3) . . ? Cu4 Cu6 Cu4 144.52(7) 2 . ? C9 Cu6 Cu3 79.5(2) . 2 ? C9 Cu6 Cu3 111.3(2) . . ? C9 Cu6 Cu3 111.3(2) 2 2 ? C9 Cu6 Cu3 79.5(2) 2 . ? C9 Cu6 Cu5 99.7(2) 2 . ? C9 Cu6 Cu5 99.7(2) . . ? C9 Cu6 Cu4 136.2(2) . 2 ? C9 Cu6 Cu4 136.2(2) 2 . ? C9 Cu6 Cu4 51.7(2) 2 2 ? C9 Cu6 Cu4 51.7(2) . . ? C9 Cu6 C9 160.6(5) 2 . ? Cu5 Cu3 Cu6 54.47(4) . . ? Cu5 Cu3 Cu4 69.05(3) . . ? Cu4 Cu3 Cu6 55.85(3) . . ? Cu2 Cu3 Cu6 111.50(4) . . ? Cu2 Cu3 Cu5 87.54(4) . . ? Cu2 Cu3 Cu4 57.98(4) . . ? Cu1 Cu3 Cu6 157.30(5) . . ? Cu1 Cu3 Cu5 143.89(5) . . ? Cu1 Cu3 Cu4 111.76(5) . . ? Cu1 Cu3 Cu2 66.27(4) . . ? C12 Cu3 Cu6 86.9(2) 2 . ? C12 Cu3 Cu5 51.1(2) 2 . ? C12 Cu3 Cu4 120.1(2) 2 . ? C12 Cu3 Cu2 112.5(2) 2 . ? C12 Cu3 Cu1 115.2(2) 2 . ? C12 Cu3 C4 153.8(3) 2 . ? C4 Cu3 Cu6 105.0(2) . . ? C4 Cu3 Cu5 153.3(2) . . ? C4 Cu3 Cu4 85.3(2) . . ? C4 Cu3 Cu2 85.1(2) . . ? C4 Cu3 Cu1 52.7(2) . . ? Cu6 Cu5 Cu3 67.90(3) . 2 ? Cu6 Cu5 Cu3 67.90(3) . . ? Cu6 Cu5 Cu4 55.54(3) . 2 ? Cu6 Cu5 Cu4 55.54(3) . . ? Cu3 Cu5 Cu3 135.80(7) . 2 ? Cu3 Cu5 Cu4 57.42(3) . . ? Cu3 Cu5 Cu4 57.41(3) 2 2 ? Cu3 Cu5 Cu4 96.47(4) 2 . ? Cu3 Cu5 Cu4 96.47(4) . 2 ? Cu4 Cu5 Cu4 111.08(6) 2 . ? C12 Cu5 Cu6 97.2(2) 2 . ? C12 Cu5 Cu6 97.2(2) . . ? C12 Cu5 Cu3 51.9(2) . 2 ? C12 Cu5 Cu3 51.9(2) 2 . ? C12 Cu5 Cu3 135.4(2) 2 2 ? C12 Cu5 Cu3 135.4(2) . . ? C12 Cu5 Cu4 109.3(2) 2 . ? C12 Cu5 Cu4 79.2(2) 2 2 ? C12 Cu5 Cu4 109.3(2) . 2 ? C12 Cu5 Cu4 79.2(2) . . ? C12 Cu5 C12 165.6(4) . 2 ? Cu6 Cu4 Cu3 64.55(3) . . ? Cu6 Cu4 Cu5 52.20(4) . . ? Cu3 Cu4 Cu5 53.53(3) . . ? Cu2 Cu4 Cu6 120.33(4) . . ? Cu2 Cu4 Cu3 58.56(4) . . ? Cu2 Cu4 Cu5 79.45(4) . . ? Cu2 Cu4 C10 137.22(19) . . ? C10 Cu4 Cu6 75.84(17) . . ? C10 Cu4 Cu3 133.72(18) . . ? C10 Cu4 Cu5 83.75(18) . . ? C1 Cu4 Cu6 153.5(2) . . ? C1 Cu4 Cu3 95.7(2) . . ? C1 Cu4 Cu5 130.8(2) . . ? C1 Cu4 Cu2 51.4(2) . . ? C1 Cu4 C10 128.7(3) . . ? C1 Cu4 C9 143.4(3) . . ? C9 Cu4 Cu6 51.2(2) . . ? C9 Cu4 Cu3 115.8(2) . . ? C9 Cu4 Cu5 84.9(2) . . ? C9 Cu4 Cu2 163.2(2) . . ? C9 Cu4 C10 33.3(3) . . ? Cu3 Cu2 Cu1 56.09(4) . . ? Cu4 Cu2 Cu3 63.46(4) . . ? Cu4 Cu2 Cu1 108.03(4) . . ? Cl1 Cu2 Cu3 109.95(8) . . ? Cl1 Cu2 Cu4 158.08(11) . . ? Cl1 Cu2 Cu1 81.27(9) . . ? C1 Cu2 Cu3 99.7(2) . . ? C1 Cu2 Cu4 51.6(2) . . ? C1 Cu2 Cu1 104.5(2) . . ? C1 Cu2 Cl1 146.8(2) . . ? Cu3 Cu1 Cu2 57.64(4) . . ? C4 Cu1 Cu3 52.8(2) . . ? C4 Cu1 Cu2 79.8(2) . . ? C4 Cu1 N2 139.9(3) . . ? C4 Cu1 N1 112.0(3) . . ? N2 Cu1 Cu3 115.8(2) . . ? N2 Cu1 Cu2 130.4(2) . . ? N2 Cu1 N1 86.1(3) . . ? N1 Cu1 Cu3 157.9(2) . . ? N1 Cu1 Cu2 107.2(3) . . ? Cu5 C12 Cu3 77.0(3) . 2 ? C11 C12 Cu3 107.5(5) . 2 ? C11 C12 Cu5 123.9(6) . . ? C13 C12 Cu3 123.7(6) . 2 ? C13 C12 Cu5 101.5(5) . . ? C13 C12 C11 117.7(7) . . ? C4 C3 C2 124.4(7) . . ? C8 C3 C4 118.4(7) . . ? C8 C3 C2 117.2(7) . . ? C12 C11 C10 121.0(7) . . ? C16 C11 C12 118.9(8) . . ? C16 C11 C10 120.0(8) . . ? Cu1 C4 Cu3 74.4(3) . . ? C3 C4 Cu3 128.3(6) . . ? C3 C4 Cu1 120.5(5) . . ? C3 C4 C5 116.3(7) . . ? C5 C4 Cu3 103.9(5) . . ? C5 C4 Cu1 105.3(5) . . ? C11 C10 Cu4 84.7(5) . . ? C11 C10 C26 114.3(7) . . ? C26 C10 Cu4 137.7(5) . . ? C9 C10 Cu4 54.0(4) . . ? C9 C10 C11 125.0(7) . . ? C9 C10 C26 120.7(7) . . ? C4 C5 H5 118.7 . . ? C6 C5 C4 122.6(8) . . ? C6 C5 H5 118.7 . . ? C3 C2 C20 115.3(7) . . ? C1 C2 C3 123.9(6) . . ? C1 C2 C20 120.8(7) . . ? Cu2 C1 Cu4 77.0(3) . . ? C2 C1 Cu4 108.2(5) . . ? C2 C1 Cu2 117.2(5) . . ? C2 C1 C17 121.0(7) . . ? C17 C1 Cu4 115.7(6) . . ? C17 C1 Cu2 109.8(6) . . ? C32 N2 Cu1 103.5(8) . . ? C32 N2 C34 107.9(10) . . ? C34 N2 Cu1 111.2(7) . . ? C33 N2 Cu1 117.2(7) . . ? C33 N2 C32 113.7(11) . . ? C33 N2 C34 103.3(10) . . ? C12 C13 H13 119.2 . . ? C14 C13 C12 121.6(8) . . ? C14 C13 H13 119.2 . . ? C2 C20 H20A 108.8 . . ? C2 C20 H20B 108.8 . . ? H20A C20 H20B 107.7 . . ? C21 C20 C2 113.9(7) . . ? C21 C20 H20A 108.8 . . ? C21 C20 H20B 108.8 . . ? C3 C8 H8 118.5 . . ? C7 C8 C3 123.0(8) . . ? C7 C8 H8 118.5 . . ? H23A C23 H23B 107.6 . . ? C24 C23 H23A 108.7 . . ? C24 C23 H23B 108.7 . . ? C9 C23 H23A 108.7 . . ? C9 C23 H23B 108.7 . . ? C9 C23 C24 114.2(7) . . ? H27A C27 H27B 107.9 . . ? C26 C27 H27A 109.1 . . ? C26 C27 H27B 109.1 . . ? C28 C27 H27A 109.1 . . ? C28 C27 H27B 109.1 . . ? C28 C27 C26 112.4(8) . . ? C10 C26 H26A 108.6 . . ? C10 C26 H26B 108.6 . . ? C27 C26 C10 114.8(6) . . ? C27 C26 H26A 108.6 . . ? C27 C26 H26B 108.6 . . ? H26A C26 H26B 107.6 . . ? C23 C24 H24A 108.9 . . ? C23 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? C25 C24 C23 113.4(8) . . ? C25 C24 H24A 108.9 . . ? C25 C24 H24B 108.9 . . ? C11 C16 H16 118.9 . . ? C15 C16 C11 122.1(9) . . ? C15 C16 H16 118.9 . . ? C8 C7 H7 120.1 . . ? C8 C7 C6 119.9(8) . . ? C6 C7 H7 120.1 . . ? Cu6 C9 Cu4 77.0(3) . . ? C10 C9 Cu6 130.1(6) . . ? C10 C9 Cu4 92.7(5) . . ? C10 C9 C23 120.3(7) . . ? C23 C9 Cu6 104.9(5) . . ? C23 C9 Cu4 124.4(6) . . ? C31 N1 Cu1 102.9(6) . . ? C31 N1 C29 109.6(10) . . ? C29 N1 Cu1 112.9(8) . . ? C30 N1 Cu1 109.0(7) . . ? C30 N1 C31 111.7(11) . . ? C30 N1 C29 110.6(11) . . ? C1 C17 H17A 107.3 . . ? C1 C17 H17B 107.3 . . ? H17A C17 H17B 106.9 . . ? C18 C17 C1 120.1(8) . . ? C18 C17 H17A 107.3 . . ? C18 C17 H17B 107.3 . . ? H19A C19 H19B 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? C20 C21 H21A 109.2 . . ? C20 C21 H21B 109.2 . . ? H21A C21 H21B 107.9 . . ? C22 C21 C20 111.9(8) . . ? C22 C21 H21A 109.2 . . ? C22 C21 H21B 109.2 . . ? C5 C6 H6 120.1 . . ? C7 C6 C5 119.8(8) . . ? C7 C6 H6 120.1 . . ? 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 . . ? C13 C14 H14 120.3 . . ? C15 C14 C13 119.4(9) . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 120.3(9) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C17 C18 C19 116.3(9) . . ? C17 C18 H18A 108.2 . . ? C17 C18 H18B 108.2 . . ? C19 C18 H18A 108.2 . . ? C19 C18 H18B 108.2 . . ? H18A C18 H18B 107.4 . . ? 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 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N1 C31 H31A 108.2 . . ? N1 C31 H31B 108.2 . . ? H31A C31 H31B 107.3 . . ? C32 C31 N1 116.5(10) . . ? C32 C31 H31A 108.2 . . ? C32 C31 H31B 108.2 . . ? N2 C32 H32A 107.8 . . ? N2 C32 H32B 107.8 . . ? C31 C32 N2 118.2(12) . . ? C31 C32 H32A 107.8 . . ? C31 C32 H32B 107.8 . . ? H32A C32 H32B 107.1 . . ? N1 C29 H29A 109.5 . . ? N1 C29 H29B 109.5 . . ? N1 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N2 C34 H34A 109.5 . . ? N2 C34 H34B 109.5 . . ? N2 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N2 C33 H33A 109.5 . . ? N2 C33 H33B 109.5 . . ? N2 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N1 C30 H30A 109.5 . . ? N1 C30 H30B 109.5 . . ? N1 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 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 Cu3 C12 C11 C10 -31.5(9) 2 . . . ? Cu3 C12 C11 C16 144.6(7) 2 . . . ? Cu3 C12 C13 C14 -140.3(7) 2 . . . ? Cu3 C4 C5 C6 144.4(7) . . . . ? Cu5 C12 C11 C10 54.4(10) . . . . ? Cu5 C12 C11 C16 -129.5(7) . . . . ? Cu5 C12 C13 C14 137.7(8) . . . . ? Cu4 C10 C26 C27 -8.1(13) . . . . ? Cu4 C10 C9 Cu6 75.3(6) . . . . ? Cu4 C10 C9 C23 -133.0(8) . . . . ? Cu4 C1 C17 C18 80.6(11) . . . . ? Cu2 C1 C17 C18 -4.0(12) . . . . ? Cu1 C4 C5 C6 -138.2(7) . . . . ? Cu1 N2 C32 C31 33.9(16) . . . . ? Cu1 N1 C31 C32 25.8(15) . . . . ? C12 C11 C10 Cu4 -74.7(7) . . . . ? C12 C11 C10 C26 144.6(7) . . . . ? C12 C11 C10 C9 -36.6(12) . . . . ? C12 C11 C16 C15 2.2(14) . . . . ? C12 C13 C14 C15 1.3(14) . . . . ? C3 C4 C5 C6 -2.1(11) . . . . ? C3 C2 C1 Cu4 -38.9(8) . . . . ? C3 C2 C1 Cu2 45.5(9) . . . . ? C3 C2 C1 C17 -175.7(7) . . . . ? C3 C2 C20 C21 98.6(8) . . . . ? C3 C8 C7 C6 -2.9(14) . . . . ? C11 C12 C13 C14 -0.9(12) . . . . ? C11 C10 C26 C27 102.2(9) . . . . ? C11 C10 C9 Cu6 25.8(12) . . . . ? C11 C10 C9 Cu4 -49.5(8) . . . . ? C11 C10 C9 C23 177.4(7) . . . . ? C11 C16 C15 C14 -1.9(16) . . . . ? C4 C3 C2 C1 -29.3(11) . . . . ? C4 C3 C2 C20 152.7(7) . . . . ? C4 C3 C8 C7 1.8(12) . . . . ? C4 C5 C6 C7 1.1(13) . . . . ? C10 C11 C16 C15 178.4(9) . . . . ? C2 C3 C4 Cu3 43.2(10) . . . . ? C2 C3 C4 Cu1 -50.7(9) . . . . ? C2 C3 C4 C5 -179.8(7) . . . . ? C2 C3 C8 C7 -177.8(8) . . . . ? C2 C1 C17 C18 -145.5(10) . . . . ? C2 C20 C21 C22 -179.8(8) . . . . ? C1 C2 C20 C21 -79.5(9) . . . . ? C1 C17 C18 C19 -175.5(9) . . . . ? C13 C12 C11 C10 -176.9(7) . . . . ? C13 C12 C11 C16 -0.8(11) . . . . ? C13 C14 C15 C16 0.1(16) . . . . ? C20 C2 C1 Cu4 139.0(6) . . . . ? C20 C2 C1 Cu2 -136.6(6) . . . . ? C20 C2 C1 C17 2.2(11) . . . . ? C8 C3 C4 Cu3 -136.3(7) . . . . ? C8 C3 C4 Cu1 129.8(7) . . . . ? C8 C3 C4 C5 0.7(10) . . . . ? C8 C3 C2 C1 150.2(8) . . . . ? C8 C3 C2 C20 -27.8(10) . . . . ? C8 C7 C6 C5 1.4(14) . . . . ? C26 C10 C9 Cu6 -155.4(6) . . . . ? C26 C10 C9 Cu4 129.2(6) . . . . ? C26 C10 C9 C23 -3.8(11) . . . . ? C24 C23 C9 Cu6 -68.4(8) . . . . ? C24 C23 C9 Cu4 15.8(10) . . . . ? C24 C23 C9 C10 133.7(8) . . . . ? C16 C11 C10 Cu4 109.2(7) . . . . ? C16 C11 C10 C26 -31.5(10) . . . . ? C16 C11 C10 C9 147.4(8) . . . . ? C9 C10 C26 C27 -76.8(10) . . . . ? C9 C23 C24 C25 176.8(8) . . . . ? N1 C31 C32 N2 -44(2) . . . . ? C28 C27 C26 C10 171.5(8) . . . . ? C29 N1 C31 C32 146.2(14) . . . . ? C34 N2 C32 C31 151.8(14) . . . . ? C33 N2 C32 C31 -94.3(16) . . . . ? C30 N1 C31 C32 -90.9(15) . . . . ? _olex2_submission_special_instructions 'No special instructions were received' _platon_squeeze_details ; ; # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.568 25 1 ' ' 2 0.000 0.000 0.807 112 11 ' ' 3 0.000 0.500 0.478 41 3 ' ' 4 0.500 0.500 0.194 112 11 ' ' 5 0.500 0.000 0.522 41 3 ' ' 6 0.500 0.500 0.434 26 1 ' ' #===END data_3 _audit_creation_date 2015-07-11 _audit_creation_method ; Olex2 1.2 (compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) ; _shelxl_version_number 2013-2 _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Bourhis, L.J., Dolomanov, O.V., Gildea, R.J., Howard, J.A.K., Puschmann, H. (2013). in preparation. Bourhis, L.J., Dolomanov, O.V., Gildea, R.J., Howard, J.A.K., Puschmann, H. (2015). Acta Cryst. A71, 59-75. 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. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C92 H124 Cu12 S2' _chemical_formula_sum 'C92 H124 Cu12 S2' _chemical_formula_weight 2056.50 _chemical_melting_point ? _chemical_oxdiff_formula 'C52 H' 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 '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' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6667(5) _cell_length_b 13.5072(6) _cell_length_c 15.0381(6) _cell_angle_alpha 96.035(3) _cell_angle_beta 113.105(4) _cell_angle_gamma 110.051(4) _cell_volume 2135.82(17) _cell_formula_units_Z 1 _cell_measurement_reflns_used 6811 _cell_measurement_temperature 180.01(10) _cell_measurement_theta_max 28.0540 _cell_measurement_theta_min 3.3260 _shelx_estimated_absorpt_T_max 0.864 _shelx_estimated_absorpt_T_min 0.753 _exptl_absorpt_coefficient_mu 3.013 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.81145 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'light black' _exptl_crystal_colour_lustre ? _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary black _exptl_crystal_density_diffrn 1.599 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 1056 _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0407 _diffrn_reflns_av_unetI/netI 0.0606 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 20006 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.022 _diffrn_reflns_theta_min 2.961 _diffrn_ambient_temperature 180.01(10) _diffrn_detector_area_resol_mean 10.3914 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega 35.00 60.00 1.0000 4.5100 omega____ theta____ kappa____ phi______ frames - 10.8579 -178.0000 120.0000 25 #__ type_ start__ end____ width___ exp.time_ 2 omega -3.00 24.00 1.0000 4.5100 omega____ theta____ kappa____ phi______ frames - -11.6392 -99.0000 -90.0000 27 #__ type_ start__ end____ width___ exp.time_ 3 omega -14.00 12.00 1.0000 4.5100 omega____ theta____ kappa____ phi______ frames - -11.6392 -99.0000 150.0000 26 #__ type_ start__ end____ width___ exp.time_ 4 omega -3.00 22.00 1.0000 4.5100 omega____ theta____ kappa____ phi______ frames - -11.6392 -99.0000 -120.0000 25 #__ type_ start__ end____ width___ exp.time_ 5 omega -37.00 58.00 1.0000 4.5100 omega____ theta____ kappa____ phi______ frames - -11.6392 38.0000 -90.0000 95 #__ type_ start__ end____ width___ exp.time_ 6 omega -15.00 29.00 1.0000 4.5100 omega____ theta____ kappa____ phi______ frames - -11.6392 -99.0000 -30.0000 44 #__ type_ start__ end____ width___ exp.time_ 7 omega -79.00 -38.00 1.0000 4.5100 omega____ theta____ kappa____ phi______ frames - -11.6392 -38.0000 -30.0000 41 #__ type_ start__ end____ width___ exp.time_ 8 omega -15.00 11.00 1.0000 4.5100 omega____ theta____ kappa____ phi______ frames - -11.6392 -38.0000 -30.0000 26 #__ type_ start__ end____ width___ exp.time_ 9 omega -41.00 47.00 1.0000 4.5100 omega____ theta____ kappa____ phi______ frames - -11.6392 57.0000 150.0000 88 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 0.0224086000 _diffrn_orient_matrix_UB_12 0.0041974000 _diffrn_orient_matrix_UB_13 0.0521195000 _diffrn_orient_matrix_UB_21 -0.0267448000 _diffrn_orient_matrix_UB_22 0.0373610000 _diffrn_orient_matrix_UB_23 0.0047361000 _diffrn_orient_matrix_UB_31 -0.0572942000 _diffrn_orient_matrix_UB_32 -0.0444070000 _diffrn_orient_matrix_UB_33 -0.0104892000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6350 _reflns_number_total 8406 _reflns_odcompleteness_completeness 99.82 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 25.97 _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, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution 'olex2.solve (Bourhis et al., 2015)' _refine_diff_density_max 1.476 _refine_diff_density_min -1.116 _refine_diff_density_rms 0.112 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 484 _refine_ls_number_reflns 8406 _refine_ls_number_restraints 19 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0470 _refine_ls_restrained_S_all 1.061 _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^)+(0.0520P)^2^+3.4270P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1088 _refine_ls_wR_factor_ref 0.1236 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Rigid bond restraints C38, C38, C37, C37 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C38, C38, C37, C37 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 C7, C7 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 3. Uiso/Uaniso restraints and constraints Uanis(C38) \\sim Ueq, Uanis(C38) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 Uanis(C38) \\sim Ueq, Uanis(C38) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C44) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 4.a Secondary CH2 refined with riding coordinates: C31(H31A,H31B), C34(H34A,H34B), C40(H40A,H40B), C26(H26A,H26B), C32(H32A, H32B), C25(H25A,H25B), C29(H29A,H29B), C28(H28A,H28B), C35(H35A,H35B), C41(H41A,H41B), C37(H37A,H37B), C43(H43A,H43B), C46(H46A,H46B), C44(H44A,H44B), C45(H45A,H45B), C38(H38A,H38B) 4.b Aromatic/amide H refined with riding coordinates: C21(H21), C13(H13), C16(H16), C14(H14), C15(H15), C24(H24), C22(H22), C5(H5), C23(H23), C6(H6), C8(H8), C7(H7) 4.c Idealised Me refined as rotating group: C27(H27A,H27B,H27C), C42(H42A,H42B,H42C), C33(H33A,H33B,H33C), C36(H36A,H36B, H36C), C39(H39A,H39B,H39C), C30(H30A,H30B,H30C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _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 Cu2 Cu -1.04349(5) 0.37519(4) 0.29210(4) 0.02621(15) Uani 1 1 d . . . . . Cu6 Cu -0.96111(5) 0.42895(4) 0.49057(4) 0.02487(15) Uani 1 1 d . . . . . Cu4 Cu -1.18219(5) 0.45642(4) 0.33538(4) 0.02659(15) Uani 1 1 d . . . . . Cu5 Cu -1.19292(5) 0.38294(4) 0.48070(4) 0.02757(15) Uani 1 1 d . . . . . Cu1 Cu -1.27940(5) 0.30675(4) 0.18291(4) 0.02781(15) Uani 1 1 d . . . . . Cu3 Cu -1.18559(6) 0.26482(4) 0.35110(4) 0.02835(16) Uani 1 1 d . . . . . S1 S -1.45089(14) 0.15289(11) 0.06201(11) 0.0470(4) Uani 1 1 d . . . . . C31 C -1.3043(5) 0.1443(4) 0.4567(4) 0.0368(12) Uani 1 1 d . . . . . H31A H -1.2157 0.1726 0.5095 0.044 Uiso 1 1 calc R . . . . H31B H -1.3584 0.1360 0.4908 0.044 Uiso 1 1 calc R . . . . C9 C -1.3168(5) 0.2305(4) 0.3985(4) 0.0306(11) Uani 1 1 d . . . . . C20 C -0.9615(4) 0.3900(4) 0.6177(4) 0.0277(11) Uani 1 1 d . . . . . C19 C -1.0382(5) 0.3872(4) 0.6676(3) 0.0285(11) Uani 1 1 d . . . . . C21 C -0.8999(5) 0.3199(4) 0.6342(4) 0.0366(12) Uani 1 1 d . . . . . H21 H -0.8460 0.3227 0.6041 0.044 Uiso 1 1 calc R . . . . C34 C -1.5519(5) 0.1402(4) 0.3325(4) 0.0388(13) Uani 1 1 d . . . . . H34A H -1.5277 0.0955 0.3782 0.047 Uiso 1 1 calc R . . . . H34B H -1.5946 0.1774 0.3568 0.047 Uiso 1 1 calc R . . . . C40 C -1.1765(5) 0.4451(4) 0.7274(4) 0.0381(13) Uani 1 1 d . . . . . H40A H -1.1913 0.5111 0.7414 0.046 Uiso 1 1 calc R . . . . H40B H -1.1236 0.4369 0.7927 0.046 Uiso 1 1 calc R . . . . C10 C -1.4319(5) 0.2274(4) 0.3398(4) 0.0296(11) Uani 1 1 d . . . . . C13 C -1.3999(5) 0.4482(4) 0.1978(4) 0.0326(11) Uani 1 1 d . . . . . H13 H -1.3468 0.4882 0.1716 0.039 Uiso 1 1 calc R . . . . C16 C -1.5542(5) 0.3351(4) 0.2721(4) 0.0407(13) Uani 1 1 d . . . . . H16 H -1.6102 0.2952 0.2960 0.049 Uiso 1 1 calc R . . . . C17 C -1.1282(5) 0.5195(4) 0.5925(4) 0.0298(11) Uani 1 1 d . . . . . C1 C -1.1450(5) 0.3098(4) 0.1385(4) 0.0331(12) Uani 1 1 d . . . . . C14 C -1.5011(5) 0.4711(5) 0.1888(4) 0.0445(14) Uani 1 1 d . . . . . H14 H -1.5174 0.5251 0.1570 0.053 Uiso 1 1 calc R . . . . C4 C -1.0848(5) 0.2064(4) 0.3088(4) 0.0361(12) Uani 1 1 d . . . . . C12 C -1.3707(4) 0.3683(4) 0.2440(4) 0.0290(11) Uani 1 1 d . . . . . C18 C -1.1062(4) 0.4605(4) 0.6642(4) 0.0299(11) Uani 1 1 d . . . . . C11 C -1.4507(4) 0.3112(4) 0.2843(3) 0.0291(11) Uani 1 1 d . . . . . C26 C -1.2001(5) 0.4597(4) 0.0666(4) 0.0392(13) Uani 1 1 d . . . . . H26A H -1.1633 0.5027 0.1373 0.047 Uiso 1 1 calc R . . . . H26B H -1.2924 0.4197 0.0417 0.047 Uiso 1 1 calc R . . . . C15 C -1.5781(5) 0.4137(5) 0.2271(5) 0.0478(15) Uani 1 1 d . . . . . H15 H -1.6479 0.4286 0.2223 0.057 Uiso 1 1 calc R . . . . C2 C -1.1060(5) 0.2272(4) 0.1359(4) 0.0370(13) Uani 1 1 d . . . . . C24 C -1.0491(6) 0.3113(4) 0.7246(4) 0.0410(14) Uani 1 1 d . . . . . H24 H -1.1009 0.3073 0.7569 0.049 Uiso 1 1 calc R . . . . C3 C -1.0880(5) 0.1676(4) 0.2152(4) 0.0403(13) Uani 1 1 d . . . . . C32 C -1.3405(6) 0.0308(4) 0.3927(5) 0.0444(14) Uani 1 1 d . . . . . H32A H -1.4324 -0.0034 0.3464 0.053 Uiso 1 1 calc R . . . . H32B H -1.2951 0.0389 0.3514 0.053 Uiso 1 1 calc R . . . . C25 C -1.1446(5) 0.3770(4) 0.0639(4) 0.0372(13) Uani 1 1 d . . . . . H25A H -1.0562 0.4167 0.0763 0.045 Uiso 1 1 calc R . . . . H25B H -1.1923 0.3261 -0.0047 0.045 Uiso 1 1 calc R . . . . C29 C -0.9283(6) 0.2330(5) 0.0953(4) 0.0452(14) Uani 1 1 d . . . . . H29A H -0.8933 0.2134 0.1589 0.054 Uiso 1 1 calc R . . . . H29B H -0.8883 0.3139 0.1105 0.054 Uiso 1 1 calc R . . . . C22 C -0.9125(6) 0.2468(4) 0.6914(5) 0.0490(15) Uani 1 1 d . . . . . H22 H -0.8693 0.2005 0.6996 0.059 Uiso 1 1 calc R . . . . C5 C -1.0512(5) 0.1523(4) 0.3827(5) 0.0455(14) Uani 1 1 d . . . . . H5 H -1.0448 0.1792 0.4464 0.055 Uiso 1 1 calc R . . . . C28 C -1.0690(5) 0.1949(5) 0.0567(4) 0.0449(14) Uani 1 1 d . . . . . H28A H -1.1105 0.1140 0.0298 0.054 Uiso 1 1 calc R . . . . H28B H -1.1012 0.2259 0.0004 0.054 Uiso 1 1 calc R . . . . C23 C -0.9891(7) 0.2433(5) 0.7358(5) 0.0522(16) Uani 1 1 d . . . . . H23 H -1.0005 0.1932 0.7746 0.063 Uiso 1 1 calc R . . . . C35 C -1.6456(6) 0.0642(5) 0.2281(5) 0.0558(18) Uani 1 1 d . . . . . H35A H -1.6022 0.0315 0.2002 0.067 Uiso 1 1 calc R . . . . H35B H -1.6788 0.1066 0.1835 0.067 Uiso 1 1 calc R . . . . C27 C -1.1768(6) 0.5380(5) 0.0043(5) 0.0544(16) Uani 1 1 d . . . . . H27A H -1.2127 0.4962 -0.0658 0.082 Uiso 1 1 calc GR . . . . H27B H -1.0856 0.5808 0.0308 0.082 Uiso 1 1 calc GR . . . . H27C H -1.2171 0.5876 0.0077 0.082 Uiso 1 1 calc GR . . . . C41 C -1.3046(5) 0.3432(5) 0.6736(4) 0.0549(17) Uani 1 1 d . . . . . H41A H -1.3637 0.3588 0.6168 0.066 Uiso 1 1 calc R . . . . H41B H -1.2918 0.2812 0.6453 0.066 Uiso 1 1 calc R . . . . C42 C -1.3642(6) 0.3090(5) 0.7406(5) 0.0599(18) Uani 1 1 d . . . . . H42A H -1.4457 0.2453 0.7014 0.090 Uiso 1 1 calc GR . . . . H42B H -1.3774 0.3698 0.7690 0.090 Uiso 1 1 calc GR . . . . H42C H -1.3083 0.2897 0.7953 0.090 Uiso 1 1 calc GR . . . . C37 C -1.2181(6) 0.5758(5) 0.5846(5) 0.0519(15) Uani 1 1 d . U . . . H37A H -1.2688 0.5409 0.6179 0.062 Uiso 1 1 calc R . . . . H37B H -1.1643 0.6530 0.6257 0.062 Uiso 1 1 calc R . . . . C6 C -1.0270(7) 0.0619(5) 0.3672(6) 0.065(2) Uani 1 1 d . . . . . H6 H -1.0051 0.0269 0.4189 0.077 Uiso 1 1 calc R . . . . C8 C -1.0633(7) 0.0750(5) 0.2019(6) 0.066(2) Uani 1 1 d . . . . . H8 H -1.0664 0.0474 0.1398 0.080 Uiso 1 1 calc R . . . . C33 C -1.3080(8) -0.0433(5) 0.4579(6) 0.077(2) Uani 1 1 d . . . . . H33A H -1.3160 -0.1092 0.4165 0.116 Uiso 1 1 calc GR . . . . H33B H -1.3661 -0.0646 0.4874 0.116 Uiso 1 1 calc GR . . . . H33C H -1.2210 -0.0041 0.5117 0.116 Uiso 1 1 calc GR . . . . C36 C -1.7545(7) -0.0266(7) 0.2308(6) 0.099(3) Uani 1 1 d . . . . . H36A H -1.8055 -0.0819 0.1653 0.148 Uiso 1 1 calc GR . . . . H36B H -1.8072 0.0043 0.2458 0.148 Uiso 1 1 calc GR . . . . H36C H -1.7210 -0.0608 0.2831 0.148 Uiso 1 1 calc GR . . . . C43 C -1.4524(6) 0.1398(6) -0.0613(5) 0.073(2) Uani 1 1 d . . . . . H43A H -1.3824 0.2040 -0.0589 0.088 Uiso 1 1 calc R . . . . H43B H -1.4429 0.0725 -0.0819 0.088 Uiso 1 1 calc R . . . . C46 C -1.5951(6) 0.1735(6) 0.0153(5) 0.064(2) Uani 1 1 d . . . . . H46A H -1.6673 0.1059 0.0049 0.077 Uiso 1 1 calc R . . . . H46B H -1.5869 0.2337 0.0648 0.077 Uiso 1 1 calc R . . . . C7 C -1.0351(9) 0.0232(6) 0.2756(7) 0.086(3) Uani 1 1 d . U . . . H7 H -1.0208 -0.0403 0.2632 0.104 Uiso 1 1 calc R . . . . C44 C -1.5768(9) 0.1339(7) -0.1332(6) 0.090(3) Uani 1 1 d . U . . . H44A H -1.5696 0.1616 -0.1899 0.108 Uiso 1 1 calc R . . . . H44B H -1.6407 0.0567 -0.1607 0.108 Uiso 1 1 calc R . . . . C45 C -1.6171(9) 0.2012(8) -0.0802(7) 0.096(3) Uani 1 1 d . . . . . H45A H -1.5669 0.2803 -0.0678 0.116 Uiso 1 1 calc R . . . . H45B H -1.7077 0.1837 -0.1208 0.116 Uiso 1 1 calc R . . . . C39 C -1.3817(9) 0.6360(8) 0.4868(7) 0.096(3) Uani 1 1 d . U . . . H39A H -1.4232 0.6379 0.4170 0.144 Uiso 1 1 calc GR . . . . H39B H -1.3301 0.7112 0.5309 0.144 Uiso 1 1 calc GR . . . . H39C H -1.4459 0.5975 0.5069 0.144 Uiso 1 1 calc GR . . . . C38 C -1.2998(10) 0.5778(9) 0.4952(7) 0.104(3) Uani 1 1 d . U . . . H38A H -1.3564 0.5005 0.4556 0.125 Uiso 1 1 calc R . . . . H38B H -1.2495 0.6088 0.4603 0.125 Uiso 1 1 calc R . . . . C30 C -0.8941(7) 0.1826(6) 0.0202(5) 0.0611(18) Uani 1 1 d . . . . . H30A H -0.9269 0.2029 -0.0424 0.092 Uiso 1 1 calc GR . . . . H30B H -0.9317 0.1025 0.0061 0.092 Uiso 1 1 calc GR . . . . H30C H -0.8020 0.2101 0.0489 0.092 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 Cu2 0.0289(3) 0.0274(3) 0.0273(3) 0.0084(2) 0.0162(3) 0.0130(2) Cu6 0.0301(3) 0.0259(3) 0.0260(3) 0.0095(2) 0.0172(3) 0.0141(2) Cu4 0.0263(3) 0.0278(3) 0.0272(3) 0.0076(2) 0.0145(3) 0.0105(2) Cu5 0.0298(3) 0.0267(3) 0.0280(3) 0.0074(2) 0.0164(3) 0.0102(2) Cu1 0.0297(3) 0.0302(3) 0.0265(3) 0.0066(2) 0.0164(3) 0.0121(2) Cu3 0.0329(3) 0.0279(3) 0.0307(3) 0.0100(2) 0.0193(3) 0.0136(2) S1 0.0442(8) 0.0397(8) 0.0431(8) -0.0029(6) 0.0226(7) 0.0034(6) C31 0.038(3) 0.032(3) 0.034(3) 0.010(2) 0.017(3) 0.007(2) C9 0.036(3) 0.028(2) 0.028(3) 0.007(2) 0.017(2) 0.011(2) C20 0.026(3) 0.027(2) 0.031(3) 0.012(2) 0.014(2) 0.0100(19) C19 0.031(3) 0.024(2) 0.024(2) 0.0043(19) 0.013(2) 0.006(2) C21 0.038(3) 0.032(3) 0.043(3) 0.015(2) 0.019(3) 0.015(2) C34 0.035(3) 0.038(3) 0.040(3) 0.007(2) 0.022(3) 0.007(2) C40 0.037(3) 0.045(3) 0.033(3) 0.010(2) 0.022(3) 0.012(2) C10 0.033(3) 0.029(2) 0.028(3) 0.002(2) 0.019(2) 0.010(2) C13 0.034(3) 0.033(3) 0.033(3) 0.009(2) 0.016(2) 0.015(2) C16 0.033(3) 0.049(3) 0.041(3) 0.010(3) 0.022(3) 0.012(2) C17 0.039(3) 0.035(3) 0.028(3) 0.012(2) 0.022(2) 0.019(2) C1 0.033(3) 0.037(3) 0.026(3) 0.005(2) 0.015(2) 0.010(2) C14 0.042(3) 0.049(3) 0.051(4) 0.018(3) 0.019(3) 0.029(3) C4 0.040(3) 0.031(3) 0.046(3) 0.012(2) 0.027(3) 0.017(2) C12 0.025(3) 0.033(3) 0.024(2) 0.004(2) 0.010(2) 0.009(2) C18 0.023(2) 0.037(3) 0.027(3) 0.005(2) 0.014(2) 0.007(2) C11 0.025(3) 0.032(3) 0.024(2) -0.001(2) 0.010(2) 0.009(2) C26 0.039(3) 0.043(3) 0.033(3) 0.011(2) 0.020(3) 0.011(2) C15 0.037(3) 0.061(4) 0.058(4) 0.020(3) 0.025(3) 0.029(3) C2 0.035(3) 0.039(3) 0.038(3) 0.001(2) 0.022(3) 0.013(2) C24 0.061(4) 0.035(3) 0.037(3) 0.018(2) 0.032(3) 0.017(3) C3 0.045(3) 0.035(3) 0.057(4) 0.014(3) 0.037(3) 0.019(2) C32 0.047(3) 0.028(3) 0.058(4) 0.012(3) 0.027(3) 0.012(2) C25 0.030(3) 0.052(3) 0.025(3) 0.010(2) 0.013(2) 0.012(2) C29 0.051(4) 0.049(3) 0.044(3) 0.009(3) 0.030(3) 0.023(3) C22 0.061(4) 0.037(3) 0.058(4) 0.030(3) 0.025(3) 0.028(3) C5 0.049(4) 0.043(3) 0.064(4) 0.026(3) 0.036(3) 0.025(3) C28 0.048(4) 0.052(3) 0.039(3) 0.005(3) 0.026(3) 0.022(3) C23 0.079(5) 0.042(3) 0.047(4) 0.030(3) 0.035(4) 0.025(3) C35 0.045(4) 0.053(4) 0.045(4) 0.000(3) 0.021(3) -0.002(3) C27 0.060(4) 0.060(4) 0.043(4) 0.025(3) 0.022(3) 0.022(3) C41 0.034(3) 0.076(4) 0.039(3) 0.011(3) 0.020(3) 0.003(3) C42 0.049(4) 0.063(4) 0.063(4) 0.012(3) 0.038(3) 0.006(3) C37 0.042(3) 0.065(4) 0.051(3) -0.006(3) 0.024(3) 0.028(3) C6 0.086(5) 0.062(4) 0.100(6) 0.054(4) 0.066(5) 0.055(4) C8 0.100(6) 0.043(3) 0.101(6) 0.024(4) 0.081(5) 0.037(4) C33 0.101(6) 0.037(4) 0.085(6) 0.027(4) 0.030(5) 0.031(4) C36 0.062(5) 0.087(6) 0.071(5) -0.002(4) 0.024(4) -0.036(4) C43 0.062(4) 0.067(4) 0.065(5) -0.024(4) 0.048(4) -0.009(3) C46 0.042(4) 0.084(5) 0.040(4) -0.011(3) 0.011(3) 0.014(3) C7 0.147(8) 0.059(4) 0.159(8) 0.071(5) 0.128(7) 0.081(5) C44 0.094(4) 0.100(4) 0.064(4) 0.014(3) 0.042(4) 0.024(3) C45 0.079(6) 0.120(7) 0.076(6) 0.030(5) 0.024(5) 0.038(5) C39 0.120(6) 0.143(6) 0.101(6) 0.062(5) 0.070(5) 0.109(5) C38 0.118(5) 0.150(5) 0.078(4) 0.035(3) 0.036(3) 0.103(4) C30 0.062(4) 0.075(4) 0.068(5) 0.019(4) 0.046(4) 0.036(4) _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 Cu2 Cu6 2.6654(8) . ? Cu2 Cu4 2.6044(8) . ? Cu2 Cu1 2.5329(8) . ? Cu2 Cu3 2.4374(8) . ? Cu2 C17 2.041(5) 2_366 ? Cu2 C1 2.057(5) . ? Cu2 C4 2.222(5) . ? Cu2 C18 2.187(5) 2_366 ? Cu6 Cu6 2.4773(11) 2_366 ? Cu6 Cu4 3.0318(9) . ? Cu6 Cu4 2.4566(8) 2_366 ? Cu6 Cu5 2.4814(8) 2_366 ? Cu6 Cu5 2.7235(8) . ? Cu6 Cu3 2.7236(8) . ? Cu6 C20 2.037(5) . ? Cu6 C17 2.019(4) 2_366 ? Cu4 Cu6 2.4566(8) 2_366 ? Cu4 Cu5 2.5252(8) . ? Cu4 Cu1 2.4419(8) . ? Cu4 Cu3 2.6107(8) . ? Cu4 C20 2.052(4) 2_366 ? Cu4 C12 2.034(5) . ? Cu5 Cu6 2.4815(8) 2_366 ? Cu5 Cu3 2.4377(8) . ? Cu5 C9 1.989(5) . ? Cu5 C17 2.032(5) . ? Cu5 C18 2.479(5) . ? Cu1 Cu3 2.5561(9) . ? Cu1 S1 2.3138(14) . ? Cu1 C1 2.049(5) . ? Cu1 C12 2.051(5) . ? Cu3 C9 1.988(5) . ? Cu3 C4 1.970(5) . ? S1 C43 1.836(6) . ? S1 C46 1.814(7) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C31 C9 1.542(7) . ? C31 C32 1.533(7) . ? C9 C10 1.359(7) . ? C20 Cu4 2.052(4) 2_366 ? C20 C19 1.436(7) . ? C20 C21 1.404(7) . ? C19 C18 1.512(7) . ? C19 C24 1.409(7) . ? C21 H21 0.9500 . ? C21 C22 1.385(7) . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C34 C10 1.524(6) . ? C34 C35 1.513(7) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C40 C18 1.524(6) . ? C40 C41 1.544(7) . ? C10 C11 1.505(7) . ? C13 H13 0.9500 . ? C13 C14 1.378(8) . ? C13 C12 1.420(7) . ? C16 H16 0.9500 . ? C16 C11 1.403(7) . ? C16 C15 1.374(8) . ? C17 Cu2 2.041(5) 2_366 ? C17 Cu6 2.019(4) 2_366 ? C17 C18 1.405(7) . ? C17 C37 1.547(8) . ? C1 C2 1.368(8) . ? C1 C25 1.516(7) . ? C14 H14 0.9500 . ? C14 C15 1.378(8) . ? C4 C3 1.429(7) . ? C4 C5 1.402(8) . ? C12 C11 1.426(7) . ? C18 Cu2 2.187(4) 2_366 ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C26 C25 1.514(8) . ? C26 C27 1.515(7) . ? C15 H15 0.9500 . ? C2 C3 1.495(8) . ? C2 C28 1.516(7) . ? C24 H24 0.9500 . ? C24 C23 1.364(9) . ? C3 C8 1.402(8) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C32 C33 1.519(8) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C29 C28 1.509(8) . ? C29 C30 1.533(8) . ? C22 H22 0.9500 . ? C22 C23 1.368(9) . ? C5 H5 0.9500 . ? C5 C6 1.375(8) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C23 H23 0.9500 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C35 C36 1.517(8) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C41 C42 1.501(8) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C37 C38 1.347(10) . ? C6 H6 0.9500 . ? C6 C7 1.372(10) . ? C8 H8 0.9500 . ? C8 C7 1.367(10) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C43 C44 1.489(12) . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C46 C45 1.466(11) . ? C7 H7 0.9500 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C44 C45 1.486(12) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C39 C38 1.479(11) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 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 Cu4 Cu2 Cu6 70.23(2) . . ? Cu1 Cu2 Cu6 116.65(3) . . ? Cu1 Cu2 Cu4 56.74(2) . . ? Cu3 Cu2 Cu6 64.34(2) . . ? Cu3 Cu2 Cu4 62.27(2) . . ? Cu3 Cu2 Cu1 61.86(2) . . ? C17 Cu2 Cu6 48.61(13) 2_366 . ? C17 Cu2 Cu4 98.10(13) 2_366 . ? C17 Cu2 Cu1 154.55(14) 2_366 . ? C17 Cu2 Cu3 112.43(13) 2_366 . ? C17 Cu2 C1 144.65(18) 2_366 . ? C17 Cu2 C4 108.9(2) 2_366 . ? C17 Cu2 C18 38.63(19) 2_366 2_366 ? C1 Cu2 Cu6 166.73(13) . . ? C1 Cu2 Cu4 102.94(15) . . ? C1 Cu2 Cu1 51.76(14) . . ? C1 Cu2 Cu3 102.48(13) . . ? C1 Cu2 C4 89.2(2) . . ? C1 Cu2 C18 112.39(19) . 2_366 ? C4 Cu2 Cu6 83.23(14) . . ? C4 Cu2 Cu4 111.94(13) . . ? C4 Cu2 Cu1 86.49(14) . . ? C4 Cu2 Cu3 49.76(13) . . ? C18 Cu2 Cu6 79.64(13) 2_366 . ? C18 Cu2 Cu4 91.05(13) 2_366 . ? C18 Cu2 Cu1 128.95(14) 2_366 . ? C18 Cu2 Cu3 140.28(12) 2_366 . ? C18 Cu2 C4 144.5(2) 2_366 . ? Cu2 Cu6 Cu4 53.94(2) . . ? Cu2 Cu6 Cu5 95.54(3) . . ? Cu2 Cu6 Cu3 53.77(2) . . ? Cu6 Cu6 Cu2 100.33(3) 2_366 . ? Cu6 Cu6 Cu4 51.78(2) 2_366 . ? Cu6 Cu6 Cu5 56.76(2) 2_366 . ? Cu6 Cu6 Cu5 66.63(3) 2_366 2_366 ? Cu6 Cu6 Cu3 97.93(3) 2_366 . ? Cu4 Cu6 Cu2 155.14(3) 2_366 . ? Cu4 Cu6 Cu6 75.83(3) 2_366 2_366 ? Cu4 Cu6 Cu4 127.61(2) 2_366 . ? Cu4 Cu6 Cu5 102.24(3) 2_366 . ? Cu4 Cu6 Cu5 61.51(2) 2_366 2_366 ? Cu4 Cu6 Cu3 150.59(3) 2_366 . ? Cu5 Cu6 Cu2 94.19(2) 2_366 . ? Cu5 Cu6 Cu4 51.711(19) . . ? Cu5 Cu6 Cu4 93.58(3) 2_366 . ? Cu5 Cu6 Cu5 123.39(2) 2_366 . ? Cu5 Cu6 Cu3 142.72(3) 2_366 . ? Cu5 Cu6 Cu3 53.17(2) . . ? Cu3 Cu6 Cu4 53.63(2) . . ? C20 Cu6 Cu2 151.03(13) . . ? C20 Cu6 Cu6 93.05(14) . 2_366 ? C20 Cu6 Cu4 121.81(14) . . ? C20 Cu6 Cu4 53.35(13) . 2_366 ? C20 Cu6 Cu5 70.56(14) . . ? C20 Cu6 Cu5 114.73(13) . 2_366 ? C20 Cu6 Cu3 99.19(13) . . ? C17 Cu6 Cu2 49.32(14) 2_366 . ? C17 Cu6 Cu6 101.76(14) 2_366 2_366 ? C17 Cu6 Cu4 106.77(14) 2_366 2_366 ? C17 Cu6 Cu4 86.14(15) 2_366 . ? C17 Cu6 Cu5 52.46(13) 2_366 2_366 ? C17 Cu6 Cu5 137.78(15) 2_366 . ? C17 Cu6 Cu3 102.64(14) 2_366 . ? C17 Cu6 C20 151.5(2) 2_366 . ? Cu2 Cu4 Cu6 55.83(2) . . ? Cu2 Cu4 Cu3 55.73(2) . . ? Cu6 Cu4 Cu2 102.61(3) 2_366 . ? Cu6 Cu4 Cu6 52.40(2) 2_366 . ? Cu6 Cu4 Cu5 59.73(2) 2_366 . ? Cu6 Cu4 Cu3 101.54(3) 2_366 . ? Cu5 Cu4 Cu2 102.13(3) . . ? Cu5 Cu4 Cu6 57.84(2) . . ? Cu5 Cu4 Cu3 56.64(2) . . ? Cu1 Cu4 Cu2 60.15(2) . . ? Cu1 Cu4 Cu6 159.73(3) . 2_366 ? Cu1 Cu4 Cu6 107.37(3) . . ? Cu1 Cu4 Cu5 110.81(3) . . ? Cu1 Cu4 Cu3 60.67(2) . . ? Cu3 Cu4 Cu6 57.14(2) . . ? C20 Cu4 Cu2 88.94(14) 2_366 . ? C20 Cu4 Cu6 78.04(14) 2_366 . ? C20 Cu4 Cu6 52.80(13) 2_366 2_366 ? C20 Cu4 Cu5 112.41(13) 2_366 . ? C20 Cu4 Cu1 131.00(13) 2_366 . ? C20 Cu4 Cu3 132.98(14) 2_366 . ? C12 Cu4 Cu2 113.11(14) . . ? C12 Cu4 Cu6 139.18(13) . 2_366 ? C12 Cu4 Cu6 139.32(14) . . ? C12 Cu4 Cu5 92.90(14) . . ? C12 Cu4 Cu1 53.61(13) . . ? C12 Cu4 Cu3 83.77(14) . . ? C12 Cu4 C20 142.5(2) . 2_366 ? Cu6 Cu5 Cu6 56.61(2) 2_366 . ? Cu6 Cu5 Cu4 58.76(2) 2_366 . ? Cu4 Cu5 Cu6 70.45(2) . . ? Cu3 Cu5 Cu6 63.42(2) . . ? Cu3 Cu5 Cu6 105.92(3) . 2_366 ? Cu3 Cu5 Cu4 63.45(2) . . ? Cu3 Cu5 C18 145.23(13) . . ? C9 Cu5 Cu6 112.04(15) . . ? C9 Cu5 Cu6 154.25(14) . 2_366 ? C9 Cu5 Cu4 96.26(14) . . ? C9 Cu5 Cu3 52.19(14) . . ? C9 Cu5 C17 151.59(19) . . ? C9 Cu5 C18 127.32(17) . . ? C17 Cu5 Cu6 51.99(13) . 2_366 ? C17 Cu5 Cu6 93.66(14) . . ? C17 Cu5 Cu4 103.91(13) . . ? C17 Cu5 Cu3 156.07(14) . . ? C17 Cu5 C18 34.52(18) . . ? C18 Cu5 Cu6 93.76(11) . . ? C18 Cu5 Cu6 78.21(11) . 2_366 ? C18 Cu5 Cu4 136.18(11) . . ? Cu2 Cu1 Cu3 57.23(2) . . ? Cu4 Cu1 Cu2 63.11(2) . . ? Cu4 Cu1 Cu3 62.93(2) . . ? S1 Cu1 Cu2 140.35(5) . . ? S1 Cu1 Cu4 151.00(5) . . ? S1 Cu1 Cu3 111.10(5) . . ? C1 Cu1 Cu2 52.06(14) . . ? C1 Cu1 Cu4 108.99(13) . . ? C1 Cu1 Cu3 98.84(15) . . ? C1 Cu1 S1 99.93(14) . . ? C1 Cu1 C12 157.47(19) . . ? C12 Cu1 Cu2 115.41(13) . . ? C12 Cu1 Cu4 52.98(13) . . ? C12 Cu1 Cu3 84.87(14) . . ? C12 Cu1 S1 99.38(13) . . ? Cu2 Cu3 Cu6 61.90(2) . . ? Cu2 Cu3 Cu4 62.01(2) . . ? Cu2 Cu3 Cu5 109.88(3) . . ? Cu2 Cu3 Cu1 60.90(2) . . ? Cu4 Cu3 Cu6 69.23(2) . . ? Cu5 Cu3 Cu6 63.41(2) . . ? Cu5 Cu3 Cu4 59.91(2) . . ? Cu5 Cu3 Cu1 109.92(3) . . ? Cu1 Cu3 Cu6 113.82(3) . . ? Cu1 Cu3 Cu4 56.39(2) . . ? C9 Cu3 Cu2 155.64(15) . . ? C9 Cu3 Cu6 112.06(14) . . ? C9 Cu3 Cu4 93.64(14) . . ? C9 Cu3 Cu5 52.21(13) . . ? C9 Cu3 Cu1 106.45(15) . . ? C4 Cu3 Cu2 59.43(14) . . ? C4 Cu3 Cu6 86.50(15) . . ? C4 Cu3 Cu4 121.33(15) . . ? C4 Cu3 Cu5 148.00(16) . . ? C4 Cu3 Cu1 91.41(16) . . ? C4 Cu3 C9 144.8(2) . . ? C43 S1 Cu1 112.2(2) . . ? C46 S1 Cu1 112.0(2) . . ? C46 S1 C43 92.0(3) . . ? H31A C31 H31B 107.5 . . ? C9 C31 H31A 108.4 . . ? C9 C31 H31B 108.4 . . ? C32 C31 H31A 108.4 . . ? C32 C31 H31B 108.4 . . ? C32 C31 C9 115.3(4) . . ? Cu3 C9 Cu5 75.60(16) . . ? C31 C9 Cu5 113.2(3) . . ? C31 C9 Cu3 107.5(4) . . ? C10 C9 Cu5 111.0(4) . . ? C10 C9 Cu3 120.0(4) . . ? C10 C9 C31 121.0(4) . . ? Cu6 C20 Cu4 73.85(15) . 2_366 ? C19 C20 Cu6 134.9(4) . . ? C19 C20 Cu4 110.5(3) . 2_366 ? C21 C20 Cu6 104.7(3) . . ? C21 C20 Cu4 104.3(3) . 2_366 ? C21 C20 C19 116.5(4) . . ? C20 C19 C18 124.7(4) . . ? C24 C19 C20 117.2(5) . . ? C24 C19 C18 118.1(4) . . ? C20 C21 H21 117.8 . . ? C22 C21 C20 124.5(5) . . ? C22 C21 H21 117.8 . . ? H34A C34 H34B 107.5 . . ? C10 C34 H34A 108.5 . . ? C10 C34 H34B 108.5 . . ? C35 C34 H34A 108.5 . . ? C35 C34 H34B 108.5 . . ? C35 C34 C10 115.1(4) . . ? H40A C40 H40B 107.9 . . ? C18 C40 H40A 109.3 . . ? C18 C40 H40B 109.3 . . ? C18 C40 C41 111.7(4) . . ? C41 C40 H40A 109.3 . . ? C41 C40 H40B 109.3 . . ? C9 C10 C34 120.6(5) . . ? C9 C10 C11 123.9(4) . . ? C11 C10 C34 115.4(5) . . ? C14 C13 H13 118.2 . . ? C14 C13 C12 123.6(5) . . ? C12 C13 H13 118.2 . . ? C11 C16 H16 118.5 . . ? C15 C16 H16 118.5 . . ? C15 C16 C11 123.0(5) . . ? Cu6 C17 Cu2 82.07(18) 2_366 2_366 ? Cu6 C17 Cu5 75.55(16) 2_366 . ? Cu5 C17 Cu2 135.7(3) . 2_366 ? C18 C17 Cu2 76.3(3) . 2_366 ? C18 C17 Cu6 131.2(4) . 2_366 ? C18 C17 Cu5 90.4(3) . . ? C18 C17 C37 118.5(4) . . ? C37 C17 Cu2 105.7(3) . 2_366 ? C37 C17 Cu6 109.3(4) . 2_366 ? C37 C17 Cu5 117.6(4) . . ? Cu1 C1 Cu2 76.18(16) . . ? C2 C1 Cu2 95.1(4) . . ? C2 C1 Cu1 123.4(4) . . ? C2 C1 C25 119.8(4) . . ? C25 C1 Cu2 123.9(3) . . ? C25 C1 Cu1 110.4(4) . . ? C13 C14 H14 120.8 . . ? C15 C14 C13 118.4(5) . . ? C15 C14 H14 120.8 . . ? Cu3 C4 Cu2 70.81(16) . . ? C3 C4 Cu2 92.3(3) . . ? C3 C4 Cu3 135.8(4) . . ? C5 C4 Cu2 140.3(4) . . ? C5 C4 Cu3 99.2(4) . . ? C5 C4 C3 117.5(5) . . ? Cu4 C12 Cu1 73.41(16) . . ? C13 C12 Cu4 100.1(3) . . ? C13 C12 Cu1 110.0(3) . . ? C13 C12 C11 116.9(5) . . ? C11 C12 Cu4 119.9(3) . . ? C11 C12 Cu1 126.4(4) . . ? Cu2 C18 Cu5 107.75(19) 2_366 . ? C19 C18 Cu2 103.1(3) . 2_366 ? C19 C18 Cu5 81.4(3) . . ? C19 C18 C40 114.5(4) . . ? C40 C18 Cu2 114.8(3) . 2_366 ? C40 C18 Cu5 128.2(3) . . ? C17 C18 Cu2 65.1(3) . 2_366 ? C17 C18 Cu5 55.1(2) . . ? C17 C18 C19 123.1(4) . . ? C17 C18 C40 120.8(5) . . ? C16 C11 C10 117.4(4) . . ? C16 C11 C12 117.9(5) . . ? C12 C11 C10 124.7(5) . . ? H26A C26 H26B 107.7 . . ? C25 C26 H26A 108.8 . . ? C25 C26 H26B 108.8 . . ? C25 C26 C27 113.6(5) . . ? C27 C26 H26A 108.8 . . ? C27 C26 H26B 108.8 . . ? C16 C15 C14 120.2(6) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C1 C2 C3 122.4(4) . . ? C1 C2 C28 122.5(5) . . ? C3 C2 C28 114.9(5) . . ? C19 C24 H24 118.3 . . ? C23 C24 C19 123.5(5) . . ? C23 C24 H24 118.3 . . ? C4 C3 C2 122.3(5) . . ? C8 C3 C4 117.8(6) . . ? C8 C3 C2 119.6(5) . . ? C31 C32 H32A 109.3 . . ? C31 C32 H32B 109.3 . . ? H32A C32 H32B 108.0 . . ? C33 C32 C31 111.4(5) . . ? C33 C32 H32A 109.3 . . ? C33 C32 H32B 109.3 . . ? C1 C25 H25A 108.3 . . ? C1 C25 H25B 108.3 . . ? C26 C25 C1 115.9(4) . . ? C26 C25 H25A 108.3 . . ? C26 C25 H25B 108.3 . . ? H25A C25 H25B 107.4 . . ? H29A C29 H29B 107.8 . . ? C28 C29 H29A 109.0 . . ? C28 C29 H29B 109.0 . . ? C28 C29 C30 112.9(5) . . ? C30 C29 H29A 109.0 . . ? C30 C29 H29B 109.0 . . ? C21 C22 H22 121.1 . . ? C23 C22 C21 117.9(6) . . ? C23 C22 H22 121.1 . . ? C4 C5 H5 118.5 . . ? C6 C5 C4 123.0(6) . . ? C6 C5 H5 118.5 . . ? C2 C28 H28A 108.8 . . ? C2 C28 H28B 108.8 . . ? C29 C28 C2 113.7(5) . . ? C29 C28 H28A 108.8 . . ? C29 C28 H28B 108.8 . . ? H28A C28 H28B 107.7 . . ? C24 C23 C22 120.4(5) . . ? C24 C23 H23 119.8 . . ? C22 C23 H23 119.8 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? C34 C35 C36 110.9(5) . . ? H35A C35 H35B 108.0 . . ? C36 C35 H35A 109.5 . . ? C36 C35 H35B 109.5 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C40 C41 H41A 108.8 . . ? C40 C41 H41B 108.8 . . ? H41A C41 H41B 107.7 . . ? C42 C41 C40 113.9(5) . . ? C42 C41 H41A 108.8 . . ? C42 C41 H41B 108.8 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C17 C37 H37A 106.9 . . ? C17 C37 H37B 106.9 . . ? H37A C37 H37B 106.7 . . ? C38 C37 C17 121.8(6) . . ? C38 C37 H37A 106.9 . . ? C38 C37 H37B 106.9 . . ? C5 C6 H6 120.6 . . ? C7 C6 C5 118.7(6) . . ? C7 C6 H6 120.6 . . ? C3 C8 H8 119.0 . . ? C7 C8 C3 122.1(6) . . ? C7 C8 H8 119.0 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? S1 C43 H43A 110.5 . . ? S1 C43 H43B 110.5 . . ? H43A C43 H43B 108.7 . . ? C44 C43 S1 106.2(5) . . ? C44 C43 H43A 110.5 . . ? C44 C43 H43B 110.5 . . ? S1 C46 H46A 110.0 . . ? S1 C46 H46B 110.0 . . ? H46A C46 H46B 108.4 . . ? C45 C46 S1 108.5(5) . . ? C45 C46 H46A 110.0 . . ? C45 C46 H46B 110.0 . . ? C6 C7 H7 119.6 . . ? C8 C7 C6 120.8(6) . . ? C8 C7 H7 119.6 . . ? C43 C44 H44A 109.8 . . ? C43 C44 H44B 109.8 . . ? H44A C44 H44B 108.2 . . ? C45 C44 C43 109.4(7) . . ? C45 C44 H44A 109.8 . . ? C45 C44 H44B 109.8 . . ? C46 C45 C44 106.1(8) . . ? C46 C45 H45A 110.5 . . ? C46 C45 H45B 110.5 . . ? C44 C45 H45A 110.5 . . ? C44 C45 H45B 110.5 . . ? H45A C45 H45B 108.7 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? C37 C38 C39 122.3(8) . . ? C37 C38 H38A 106.7 . . ? C37 C38 H38B 106.7 . . ? C39 C38 H38A 106.7 . . ? C39 C38 H38B 106.7 . . ? H38A C38 H38B 106.6 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? _olex2_submission_special_instructions 'No special instructions were received' #===END data_5 _audit_creation_date 2015-07-11 _audit_creation_method ; Olex2 1.2 (compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) ; _shelxl_version_number 2014-3 _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _publ_section_references ; Burla, M.C., Caliandro, R., Camalli, M., Carrozzini, B., Cascarano, G.L., De Caro, L., Giacovazzo, C., Polidori, G., Siliqi, D., Spagna, R. (2007). J. Appl. Cryst. 40, 609-613. 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. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C60 H116 Cl4 Cu10 N4' _chemical_formula_sum 'C60 H116 Cl4 Cu10 N4' _chemical_formula_weight 1670.76 _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' 0.0033 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 '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 'monoclinic' _space_group_IT_number 14 _space_group_name_H-M_alt 'P 1 21/c 1' _space_group_name_Hall '-P 2ybc' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 16.307(3) _cell_length_b 13.054(2) _cell_length_c 35.207(6) _cell_angle_alpha 90 _cell_angle_beta 100.552(2) _cell_angle_gamma 90 _cell_volume 7368(2) _cell_formula_units_Z 4 _cell_measurement_reflns_used ? _cell_measurement_temperature 173.15 _cell_measurement_theta_max ? _cell_measurement_theta_min ? _shelx_estimated_absorpt_T_max 0.645 _shelx_estimated_absorpt_T_min 0.585 _exptl_absorpt_coefficient_mu 3.005 _exptl_absorpt_correction_T_max 0.618 _exptl_absorpt_correction_T_min 0.554 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ? _exptl_crystal_colour 'orangish yellow' _exptl_crystal_colour_modifier orangish _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.506 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 3448 _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0759 _diffrn_reflns_av_unetI/netI 0.0703 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 45 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_number 55143 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.471 _diffrn_reflns_theta_min 1.177 _diffrn_ambient_temperature 173.15 _diffrn_detector_area_resol_mean ? _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'RIGAKU CCD SATURN724' _diffrn_measurement_method ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source ? _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 14169 _reflns_number_total 16813 _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 ? _computing_data_collection ? _computing_data_reduction ? _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SIR2004 (Burla et al., 2007)' _refine_diff_density_max 1.571 _refine_diff_density_min -0.853 _refine_diff_density_rms 0.144 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.168 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 722 _refine_ls_number_reflns 16813 _refine_ls_number_restraints 52 _refine_ls_R_factor_all 0.0986 _refine_ls_R_factor_gt 0.0836 _refine_ls_restrained_S_all 1.176 _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^)+(0.0885P)^2^+22.8158P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2124 _refine_ls_wR_factor_ref 0.2263 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C44-C45 = C20-C21 1.54 with sigma of 0.01 C51-C52 1.5 with sigma of 0.02 N1-C52 \\sim N2-C51 \\sim N2-C51 with sigma of 0.02 3. Rigid bond restraints N2 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 C21, C52, C54 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 C21, C52, C54 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 C21 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 C21 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 C52 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 4. Uiso/Uaniso restraints and constraints Uanis(C52) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C51) \\sim Ueq, Uanis(C35) \\sim Ueq, Uanis(C36) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C45) \\sim Ueq, Uanis(C39) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C21) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 Uanis(C21) \\sim Ueq, Uanis(C52) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 Uanis(C21) \\sim Ueq, Uanis(C52) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004 5.a Riding coordinates: C53(H53A,H53B,H53C) 5.b Secondary CH2 refined with riding coordinates: C13(H13A,H13B), C14(H14A,H14B), C16(H16A,H16B), C17(H17A,H17B), C19(H19A, H19B), C20(H20A,H20B), C22(H22A,H22B), C23(H23A,H23B), C25(H25A,H25B), C26(H26A,H26B), C28(H28A,H28B), C29(H29A,H29B), C31(H31A,H31B), C32(H32A,H32B), C34(H34A,H34B), C35(H35A,H35B), C37(H37A,H37B), C38(H38A,H38B), C40(H40A, H40B), C41(H41A,H41B), C43(H43A,H43B), C44(H44A,H44B), C46(H46A,H46B), C47(H47A,H47B), C57(H57A,H57B), C58(H58A,H58B), C51(H51A,H51B), C52(H52A,H52B) 5.c Idealised Me refined as rotating group: C15(H15A,H15B,H15C), C18(H18A,H18B,H18C), C21(H21A,H21B,H21C), C24(H24A,H24B, H24C), C27(H27A,H27B,H27C), C30(H30A,H30B,H30C), C33(H33A,H33B,H33C), C36(H36A, H36B,H36C), C39(H39A,H39B,H39C), C42(H42A,H42B,H42C), C45(H45A,H45B,H45C), C48(H48A,H48B,H48C), C49(H49A,H49B,H49C), C50(H50A,H50B,H50C), C54(H54A,H54B, H54C), C55(H55A,H55B,H55C), C56(H56A,H56B,H56C), C59(H59A,H59B,H59C), C60(H60A, H60B,H60C) ; _atom_sites_solution_hydrogens mixed _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 Cu1 Cu 0.01651(7) 0.67980(8) 0.20136(3) 0.0606(3) Uani 1 1 d . . . . . Cu2 Cu 0.09288(6) 0.73699(6) 0.13628(3) 0.0430(2) Uani 1 1 d . . . . . Cu3 Cu 0.16063(6) 0.57614(7) 0.17879(3) 0.0466(2) Uani 1 1 d . . . . . Cu4 Cu 0.18536(5) 0.63426(6) 0.10601(2) 0.0386(2) Uani 1 1 d . . . . . Cu5 Cu 0.27548(5) 0.69463(6) 0.16789(2) 0.0396(2) Uani 1 1 d . . . . . Cu6 Cu 0.25188(5) 0.80834(6) 0.11195(2) 0.0387(2) Uani 1 1 d . . . . . Cu7 Cu 0.33412(5) 0.64732(6) 0.10369(2) 0.03788(19) Uani 1 1 d . . . . . Cu8 Cu 0.23295(5) 0.76550(6) 0.04416(2) 0.0400(2) Uani 1 1 d . . . . . Cu9 Cu 0.39085(5) 0.80364(7) 0.07541(2) 0.0423(2) Uani 1 1 d . . . . . Cu10 Cu 0.36186(6) 0.80793(7) -0.00628(3) 0.0506(2) Uani 1 1 d . . . . . Cl1 Cl 0.03945(13) 0.51537(15) 0.18601(6) 0.0563(5) Uani 1 1 d . . . . . Cl2 Cl 0.07238(13) 0.83105(15) 0.18423(6) 0.0540(5) Uani 1 1 d . . . . . Cl3 Cl 0.26603(12) 0.67947(14) -0.00345(5) 0.0476(4) Uani 1 1 d . . . . . Cl4 Cl 0.41539(12) 0.92868(14) 0.03788(5) 0.0489(4) Uani 1 1 d . . . . . N1 N -0.1166(6) 0.7180(8) 0.1936(3) 0.095(3) Uani 1 1 d D . . . . N2 N 0.0149(7) 0.6992(7) 0.2629(2) 0.082(3) Uani 1 1 d D U . . . N3 N 0.3245(6) 0.8803(7) -0.0639(2) 0.079(2) Uani 1 1 d . . . . . N4 N 0.4562(5) 0.7320(5) -0.0327(2) 0.065(2) Uani 1 1 d . . . . . C1 C 0.0667(4) 0.6711(5) 0.0847(2) 0.0404(14) Uani 1 1 d . . . . . C2 C 0.0524(4) 0.7443(6) 0.0561(2) 0.0421(15) Uani 1 1 d . . . . . C3 C 0.0893(4) 0.8501(5) 0.0602(2) 0.0422(15) Uani 1 1 d . . . . . C4 C 0.1718(4) 0.8724(5) 0.0682(2) 0.0407(14) Uani 1 1 d . . . . . C5 C 0.2652(4) 0.5196(5) 0.1022(2) 0.0403(14) Uani 1 1 d . . . . . C6 C 0.2805(5) 0.4568(5) 0.1335(2) 0.0434(15) Uani 1 1 d . . . . . C7 C 0.3187(5) 0.4882(5) 0.1744(2) 0.0449(16) Uani 1 1 d . . . . . C8 C 0.2828(5) 0.5582(5) 0.1946(2) 0.0456(16) Uani 1 1 d . . . . . C9 C 0.4479(4) 0.7141(5) 0.1173(2) 0.0409(14) Uani 1 1 d . . . . . C10 C 0.4608(4) 0.7601(5) 0.1523(2) 0.0421(15) Uani 1 1 d . . . . . C11 C 0.4068(4) 0.8411(5) 0.1656(2) 0.0436(15) Uani 1 1 d . . . . . C12 C 0.3231(4) 0.8349(6) 0.16446(19) 0.0413(15) Uani 1 1 d . . . . . C13 C 0.0196(4) 0.5694(5) 0.0799(2) 0.0443(15) Uani 1 1 d . . . . . H13A H 0.0155 0.5449 0.0530 0.053 Uiso 1 1 calc R . . . . H13B H 0.0512 0.5177 0.0973 0.053 Uiso 1 1 calc R . . . . C14 C -0.0678(5) 0.5797(6) 0.0891(2) 0.0516(18) Uani 1 1 d . . . . . H14A H -0.1008 0.6267 0.0701 0.062 Uiso 1 1 calc R . . . . H14B H -0.0638 0.6107 0.1150 0.062 Uiso 1 1 calc R . . . . C15 C -0.1137(6) 0.4768(7) 0.0882(3) 0.071(3) Uani 1 1 d . . . . . H15A H -0.1193 0.4466 0.0623 0.106 Uiso 1 1 calc GR . . . . H15B H -0.1692 0.4878 0.0944 0.106 Uiso 1 1 calc GR . . . . H15C H -0.0818 0.4302 0.1072 0.106 Uiso 1 1 calc GR . . . . C16 C -0.0070(4) 0.7261(6) 0.0178(2) 0.0484(17) Uani 1 1 d . . . . . H16A H -0.0267 0.6542 0.0169 0.058 Uiso 1 1 calc R . . . . H16B H -0.0563 0.7711 0.0166 0.058 Uiso 1 1 calc R . . . . C17 C 0.0330(5) 0.7465(6) -0.0175(2) 0.0530(18) Uani 1 1 d . . . . . H17A H 0.0552 0.8173 -0.0160 0.064 Uiso 1 1 calc R . . . . H17B H 0.0804 0.6990 -0.0171 0.064 Uiso 1 1 calc R . . . . C18 C -0.0288(5) 0.7331(7) -0.0553(2) 0.063(2) Uani 1 1 d . . . . . H18A H -0.0005 0.7463 -0.0771 0.094 Uiso 1 1 calc GR . . . . H18B H -0.0750 0.7815 -0.0561 0.094 Uiso 1 1 calc GR . . . . H18C H -0.0505 0.6629 -0.0570 0.094 Uiso 1 1 calc GR . . . . C19 C 0.0222(5) 0.9330(6) 0.0520(3) 0.060(2) Uani 1 1 d . . . . . H19A H 0.0498 1.0008 0.0538 0.072 Uiso 1 1 calc R . . . . H19B H -0.0081 0.9247 0.0251 0.072 Uiso 1 1 calc R . . . . C20 C -0.0399(8) 0.9317(9) 0.0785(4) 0.094(4) Uani 1 1 d D . . . . H20A H -0.0332 0.8668 0.0933 0.113 Uiso 1 1 calc R . . . . H20B H -0.0966 0.9316 0.0625 0.113 Uiso 1 1 calc R . . . . C21 C -0.0343(15) 1.0188(14) 0.1066(5) 0.199(9) Uani 1 1 d D U . . . H21A H 0.0077 1.0679 0.1014 0.299 Uiso 1 1 calc GR . . . . H21B H -0.0183 0.9924 0.1330 0.299 Uiso 1 1 calc GR . . . . H21C H -0.0886 1.0529 0.1038 0.299 Uiso 1 1 calc GR . . . . C22 C 0.2017(5) 0.9832(5) 0.0673(2) 0.0467(16) Uani 1 1 d . . . . . H22A H 0.1652 1.0276 0.0798 0.056 Uiso 1 1 calc R . . . . H22B H 0.2590 0.9883 0.0825 0.056 Uiso 1 1 calc R . . . . C23 C 0.2014(5) 1.0217(6) 0.0266(3) 0.0545(19) Uani 1 1 d . . . . . H23A H 0.1432 1.0243 0.0124 0.065 Uiso 1 1 calc R . . . . H23B H 0.2324 0.9726 0.0131 0.065 Uiso 1 1 calc R . . . . C24 C 0.2406(7) 1.1277(7) 0.0259(4) 0.085(4) Uani 1 1 d . . . . . H24A H 0.2441 1.1459 -0.0008 0.128 Uiso 1 1 calc GR . . . . H24B H 0.2968 1.1271 0.0416 0.128 Uiso 1 1 calc GR . . . . H24C H 0.2062 1.1783 0.0363 0.128 Uiso 1 1 calc GR . . . . C25 C 0.2315(5) 0.4742(5) 0.06175(19) 0.0432(15) Uani 1 1 d . . . . . H25A H 0.1918 0.4184 0.0642 0.052 Uiso 1 1 calc R . . . . H25B H 0.2008 0.5281 0.0451 0.052 Uiso 1 1 calc R . . . . C26 C 0.3009(5) 0.4325(6) 0.0425(2) 0.0528(18) Uani 1 1 d . . . . . H26A H 0.3279 0.3738 0.0577 0.063 Uiso 1 1 calc R . . . . H26B H 0.3437 0.4863 0.0424 0.063 Uiso 1 1 calc R . . . . C27 C 0.2678(7) 0.3978(7) 0.0010(2) 0.071(3) Uani 1 1 d . . . . . H27A H 0.2453 0.4570 -0.0147 0.107 Uiso 1 1 calc GR . . . . H27B H 0.2236 0.3469 0.0009 0.107 Uiso 1 1 calc GR . . . . H27C H 0.3133 0.3673 -0.0099 0.107 Uiso 1 1 calc GR . . . . C28 C 0.2633(5) 0.3421(5) 0.1308(2) 0.0501(18) Uani 1 1 d . . . . . H28A H 0.2462 0.3233 0.1033 0.060 Uiso 1 1 calc R . . . . H28B H 0.3157 0.3050 0.1410 0.060 Uiso 1 1 calc R . . . . C29 C 0.1968(6) 0.3070(6) 0.1525(3) 0.060(2) Uani 1 1 d . . . . . H29A H 0.1434 0.3404 0.1413 0.072 Uiso 1 1 calc R . . . . H29B H 0.2121 0.3291 0.1798 0.072 Uiso 1 1 calc R . . . . C30 C 0.1847(7) 0.1920(6) 0.1513(3) 0.070(3) Uani 1 1 d . . . . . H30A H 0.1811 0.1676 0.1247 0.105 Uiso 1 1 calc GR . . . . H30B H 0.1331 0.1748 0.1604 0.105 Uiso 1 1 calc GR . . . . H30C H 0.2321 0.1591 0.1680 0.105 Uiso 1 1 calc GR . . . . C31 C 0.3963(6) 0.4279(7) 0.1910(2) 0.060(2) Uani 1 1 d . . . . . H31A H 0.4205 0.4563 0.2167 0.072 Uiso 1 1 calc R . . . . H31B H 0.3804 0.3559 0.1947 0.072 Uiso 1 1 calc R . . . . C32 C 0.4616(5) 0.4301(8) 0.1657(3) 0.066(2) Uani 1 1 d . . . . . H32A H 0.4759 0.5023 0.1614 0.080 Uiso 1 1 calc R . . . . H32B H 0.4376 0.4000 0.1403 0.080 Uiso 1 1 calc R . . . . C33 C 0.5411(7) 0.3725(12) 0.1824(4) 0.113(5) Uani 1 1 d . . . . . H33A H 0.5836 0.3860 0.1666 0.169 Uiso 1 1 calc GR . . . . H33B H 0.5294 0.2989 0.1824 0.169 Uiso 1 1 calc GR . . . . H33C H 0.5615 0.3956 0.2090 0.169 Uiso 1 1 calc GR . . . . C34 C 0.3143(5) 0.5750(7) 0.2380(2) 0.0549(19) Uani 1 1 d . . . . . H34A H 0.3732 0.5531 0.2448 0.066 Uiso 1 1 calc R . . . . H34B H 0.3118 0.6490 0.2439 0.066 Uiso 1 1 calc R . . . . C35 C 0.2640(10) 0.5170(15) 0.2621(4) 0.135(5) Uani 1 1 d . U . . . H35A H 0.2752 0.4429 0.2602 0.162 Uiso 1 1 calc R . . . . H35B H 0.2039 0.5286 0.2521 0.162 Uiso 1 1 calc R . . . . C36 C 0.2849(10) 0.5508(15) 0.3051(4) 0.145(6) Uani 1 1 d . U . . . H36A H 0.2909 0.6255 0.3065 0.218 Uiso 1 1 calc GR . . . . H36B H 0.3373 0.5186 0.3176 0.218 Uiso 1 1 calc GR . . . . H36C H 0.2398 0.5296 0.3183 0.218 Uiso 1 1 calc GR . . . . C37 C 0.5114(5) 0.6420(6) 0.1049(2) 0.0525(18) Uani 1 1 d . . . . . H37A H 0.4855 0.6042 0.0813 0.063 Uiso 1 1 calc R . . . . H37B H 0.5310 0.5917 0.1256 0.063 Uiso 1 1 calc R . . . . C38 C 0.5889(7) 0.7094(10) 0.0962(3) 0.091(4) Uani 1 1 d . . . . . H38A H 0.5714 0.7523 0.0729 0.110 Uiso 1 1 calc R . . . . H38B H 0.6100 0.7547 0.1184 0.110 Uiso 1 1 calc R . . . . C39 C 0.6553(9) 0.6349(13) 0.0898(4) 0.127(5) Uani 1 1 d . U . . . H39A H 0.6325 0.5882 0.0687 0.191 Uiso 1 1 calc GR . . . . H39B H 0.6740 0.5954 0.1135 0.191 Uiso 1 1 calc GR . . . . H39C H 0.7026 0.6725 0.0830 0.191 Uiso 1 1 calc GR . . . . C40 C 0.5381(5) 0.7336(7) 0.1824(2) 0.0560(19) Uani 1 1 d . . . . . H40A H 0.5662 0.6740 0.1730 0.067 Uiso 1 1 calc R . . . . H40B H 0.5772 0.7922 0.1846 0.067 Uiso 1 1 calc R . . . . C41 C 0.5204(7) 0.7087(8) 0.2224(3) 0.070(3) Uani 1 1 d . . . . . H41A H 0.4975 0.7703 0.2331 0.084 Uiso 1 1 calc R . . . . H41B H 0.4777 0.6541 0.2201 0.084 Uiso 1 1 calc R . . . . C42 C 0.5968(8) 0.6742(9) 0.2498(3) 0.092(4) Uani 1 1 d . . . . . H42A H 0.6189 0.6121 0.2397 0.138 Uiso 1 1 calc GR . . . . H42B H 0.5823 0.6596 0.2750 0.138 Uiso 1 1 calc GR . . . . H42C H 0.6390 0.7284 0.2525 0.138 Uiso 1 1 calc GR . . . . C43 C 0.4567(5) 0.9349(6) 0.1833(3) 0.060(2) Uani 1 1 d . . . . . H43A H 0.4207 0.9758 0.1973 0.072 Uiso 1 1 calc R . . . . H43B H 0.5047 0.9104 0.2026 0.072 Uiso 1 1 calc R . . . . C44 C 0.4884(8) 1.0025(10) 0.1560(4) 0.102(4) Uani 1 1 d D U . . . H44A H 0.5137 0.9608 0.1377 0.123 Uiso 1 1 calc R . . . . H44B H 0.5322 1.0478 0.1703 0.123 Uiso 1 1 calc R . . . . C45 C 0.4195(8) 1.0656(11) 0.1343(4) 0.115(5) Uani 1 1 d D U . . . H45A H 0.4310 1.0810 0.1086 0.173 Uiso 1 1 calc GR . . . . H45B H 0.4151 1.1297 0.1483 0.173 Uiso 1 1 calc GR . . . . H45C H 0.3669 1.0277 0.1318 0.173 Uiso 1 1 calc GR . . . . C46 C 0.2780(5) 0.9173(5) 0.1834(2) 0.0455(16) Uani 1 1 d . . . . . H46A H 0.2194 0.9226 0.1699 0.055 Uiso 1 1 calc R . . . . H46B H 0.3053 0.9844 0.1816 0.055 Uiso 1 1 calc R . . . . C47 C 0.2806(6) 0.8899(7) 0.2258(2) 0.060(2) Uani 1 1 d . . . . . H47A H 0.3394 0.8868 0.2393 0.071 Uiso 1 1 calc R . . . . H47B H 0.2559 0.8210 0.2273 0.071 Uiso 1 1 calc R . . . . C48 C 0.2332(6) 0.9670(8) 0.2467(3) 0.075(3) Uani 1 1 d . . . . . H48A H 0.1751 0.9715 0.2333 0.113 Uiso 1 1 calc GR . . . . H48B H 0.2596 1.0345 0.2469 0.113 Uiso 1 1 calc GR . . . . H48C H 0.2347 0.9443 0.2734 0.113 Uiso 1 1 calc GR . . . . C49 C 0.0757(13) 0.7747(11) 0.2807(4) 0.143(7) Uani 1 1 d . . . . . H49A H 0.1321 0.7499 0.2799 0.215 Uiso 1 1 calc GR . . . . H49B H 0.0698 0.7855 0.3076 0.215 Uiso 1 1 calc GR . . . . H49C H 0.0662 0.8395 0.2665 0.215 Uiso 1 1 calc GR . . . . C50 C 0.0304(9) 0.6019(9) 0.2853(3) 0.096(4) Uani 1 1 d . . . . . H50A H -0.0022 0.5465 0.2711 0.144 Uiso 1 1 calc GR . . . . H50B H 0.0135 0.6106 0.3105 0.144 Uiso 1 1 calc GR . . . . H50C H 0.0898 0.5849 0.2892 0.144 Uiso 1 1 calc GR . . . . C53 C -0.1702(7) 0.6342(10) 0.1823(4) 0.091(3) Uani 1 1 d . . . . . H53A H -0.1697 0.6191 0.1551 0.136 Uiso 1 1 d R . . . . H53B H -0.2271 0.6514 0.1855 0.136 Uiso 1 1 d R . . . . H53C H -0.1508 0.5741 0.1981 0.136 Uiso 1 1 d R . . . . C54 C -0.1408(8) 0.8051(10) 0.1654(6) 0.146(8) Uani 1 1 d . U . . . H54A H -0.1062 0.8651 0.1739 0.220 Uiso 1 1 calc GR . . . . H54B H -0.1996 0.8223 0.1643 0.220 Uiso 1 1 calc GR . . . . H54C H -0.1322 0.7843 0.1397 0.220 Uiso 1 1 calc GR . . . . C55 C 0.4669(7) 0.6223(7) -0.0218(4) 0.084(3) Uani 1 1 d . . . . . H55A H 0.4802 0.6163 0.0064 0.126 Uiso 1 1 calc GR . . . . H55B H 0.5125 0.5931 -0.0330 0.126 Uiso 1 1 calc GR . . . . H55C H 0.4152 0.5852 -0.0316 0.126 Uiso 1 1 calc GR . . . . C56 C 0.5376(6) 0.7825(7) -0.0227(4) 0.083(3) Uani 1 1 d . . . . . H56A H 0.5313 0.8557 -0.0287 0.124 Uiso 1 1 calc GR . . . . H56B H 0.5764 0.7519 -0.0377 0.124 Uiso 1 1 calc GR . . . . H56C H 0.5594 0.7737 0.0049 0.124 Uiso 1 1 calc GR . . . . C57 C 0.4222(9) 0.7407(10) -0.0732(3) 0.101(4) Uani 1 1 d . . . . . H57A H 0.3753 0.6920 -0.0799 0.121 Uiso 1 1 calc R . . . . H57B H 0.4657 0.7212 -0.0882 0.121 Uiso 1 1 calc R . . . . C58 C 0.3915(9) 0.8477(10) -0.0850(3) 0.097(4) Uani 1 1 d . . . . . H58A H 0.4387 0.8964 -0.0794 0.117 Uiso 1 1 calc R . . . . H58B H 0.3697 0.8492 -0.1131 0.117 Uiso 1 1 calc R . . . . C59 C 0.2448(9) 0.8366(13) -0.0826(3) 0.125(6) Uani 1 1 d . . . . . H59A H 0.2470 0.7619 -0.0800 0.188 Uiso 1 1 calc GR . . . . H59B H 0.2341 0.8550 -0.1101 0.188 Uiso 1 1 calc GR . . . . H59C H 0.2000 0.8636 -0.0704 0.188 Uiso 1 1 calc GR . . . . C60 C 0.3211(8) 0.9937(9) -0.0625(3) 0.095(4) Uani 1 1 d . . . . . H60A H 0.2726 1.0150 -0.0517 0.142 Uiso 1 1 calc GR . . . . H60B H 0.3165 1.0212 -0.0888 0.142 Uiso 1 1 calc GR . . . . H60C H 0.3721 1.0198 -0.0463 0.142 Uiso 1 1 calc GR . . . . C51 C -0.0720(9) 0.7276(13) 0.2623(4) 0.127(5) Uani 1 1 d D U . . . H51A H -0.0997 0.6664 0.2708 0.153 Uiso 1 1 calc R . . . . H51B H -0.0716 0.7802 0.2826 0.153 Uiso 1 1 calc R . . . . C52 C -0.1255(14) 0.7652(17) 0.2285(5) 0.182(8) Uani 1 1 d D U . . . H52A H -0.1840 0.7568 0.2320 0.218 Uiso 1 1 calc R . . . . H52B H -0.1151 0.8395 0.2263 0.218 Uiso 1 1 calc R . . . . 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 Cu1 0.0653(6) 0.0501(6) 0.0713(7) -0.0001(5) 0.0254(5) 0.0000(5) Cu2 0.0486(5) 0.0363(4) 0.0461(5) -0.0011(4) 0.0139(4) -0.0012(3) Cu3 0.0546(5) 0.0423(5) 0.0455(5) 0.0024(4) 0.0157(4) -0.0002(4) Cu4 0.0398(4) 0.0346(4) 0.0416(4) 0.0010(3) 0.0082(3) -0.0007(3) Cu5 0.0484(5) 0.0350(4) 0.0360(4) 0.0003(3) 0.0095(3) 0.0003(3) Cu6 0.0417(4) 0.0348(4) 0.0388(4) 0.0013(3) 0.0051(3) -0.0019(3) Cu7 0.0397(4) 0.0365(4) 0.0378(4) 0.0008(3) 0.0082(3) -0.0012(3) Cu8 0.0424(4) 0.0361(4) 0.0409(4) -0.0009(3) 0.0061(3) -0.0029(3) Cu9 0.0433(4) 0.0421(5) 0.0414(5) 0.0044(4) 0.0071(3) -0.0035(3) Cu10 0.0550(5) 0.0470(5) 0.0502(5) 0.0010(4) 0.0108(4) -0.0040(4) Cl1 0.0639(12) 0.0435(10) 0.0667(12) 0.0030(9) 0.0258(10) -0.0040(8) Cl2 0.0610(11) 0.0493(10) 0.0580(11) -0.0092(9) 0.0274(9) -0.0090(8) Cl3 0.0544(10) 0.0479(9) 0.0431(9) -0.0045(7) 0.0154(8) -0.0089(8) Cl4 0.0557(10) 0.0414(9) 0.0509(10) 0.0056(8) 0.0128(8) -0.0084(7) N1 0.077(6) 0.099(7) 0.120(8) -0.014(6) 0.046(6) -0.009(5) N2 0.120(8) 0.069(5) 0.067(5) -0.002(4) 0.043(5) 0.009(5) N3 0.084(6) 0.098(7) 0.051(4) 0.019(4) 0.002(4) -0.015(5) N4 0.081(5) 0.040(4) 0.086(5) -0.012(4) 0.047(4) -0.009(3) C1 0.041(3) 0.035(3) 0.045(4) -0.001(3) 0.009(3) 0.004(3) C2 0.038(3) 0.047(4) 0.042(4) -0.003(3) 0.009(3) -0.004(3) C3 0.039(3) 0.043(4) 0.046(4) 0.002(3) 0.010(3) 0.001(3) C4 0.041(3) 0.035(3) 0.045(4) 0.001(3) 0.005(3) 0.001(3) C5 0.045(4) 0.034(3) 0.044(4) 0.004(3) 0.014(3) 0.001(3) C6 0.055(4) 0.032(3) 0.047(4) 0.003(3) 0.018(3) 0.009(3) C7 0.063(4) 0.036(3) 0.036(3) 0.005(3) 0.010(3) 0.006(3) C8 0.059(4) 0.041(4) 0.034(3) 0.007(3) 0.003(3) 0.000(3) C9 0.039(3) 0.041(4) 0.042(4) 0.004(3) 0.007(3) 0.000(3) C10 0.039(3) 0.044(4) 0.043(4) 0.004(3) 0.005(3) -0.006(3) C11 0.045(4) 0.042(4) 0.042(4) 0.004(3) 0.005(3) -0.001(3) C12 0.042(3) 0.047(4) 0.032(3) -0.005(3) 0.000(3) 0.001(3) C13 0.046(4) 0.039(4) 0.048(4) 0.003(3) 0.008(3) -0.004(3) C14 0.058(4) 0.038(4) 0.059(5) 0.001(3) 0.012(4) -0.009(3) C15 0.065(6) 0.064(6) 0.085(7) -0.007(5) 0.022(5) -0.021(4) C16 0.039(4) 0.050(4) 0.054(4) 0.009(3) 0.004(3) -0.003(3) C17 0.049(4) 0.055(5) 0.052(4) -0.005(4) 0.003(3) -0.007(3) C18 0.058(5) 0.072(6) 0.053(5) 0.005(4) -0.002(4) -0.007(4) C19 0.048(4) 0.053(5) 0.083(6) 0.009(4) 0.024(4) 0.007(4) C20 0.093(8) 0.075(7) 0.128(10) -0.027(7) 0.054(8) 0.001(6) C21 0.203(10) 0.200(10) 0.198(10) 0.000(4) 0.044(4) -0.002(4) C22 0.047(4) 0.036(3) 0.054(4) -0.001(3) -0.001(3) -0.005(3) C23 0.049(4) 0.044(4) 0.075(5) 0.012(4) 0.024(4) 0.004(3) C24 0.078(7) 0.041(5) 0.150(11) 0.025(6) 0.058(7) 0.006(4) C25 0.055(4) 0.038(3) 0.035(3) -0.005(3) 0.004(3) -0.008(3) C26 0.064(5) 0.055(5) 0.043(4) 0.002(3) 0.020(3) 0.006(4) C27 0.113(8) 0.055(5) 0.046(5) -0.008(4) 0.020(5) 0.002(5) C28 0.068(5) 0.033(3) 0.054(4) 0.001(3) 0.022(4) 0.013(3) C29 0.075(6) 0.047(4) 0.066(5) -0.013(4) 0.031(4) -0.015(4) C30 0.105(8) 0.045(5) 0.069(6) -0.005(4) 0.042(6) -0.017(5) C31 0.072(5) 0.059(5) 0.048(4) 0.009(4) 0.009(4) 0.022(4) C32 0.054(5) 0.072(6) 0.072(6) 0.011(5) 0.006(4) 0.007(4) C33 0.081(8) 0.172(14) 0.086(8) 0.036(9) 0.016(6) 0.063(9) C34 0.066(5) 0.060(5) 0.036(4) 0.002(3) 0.002(3) 0.007(4) C35 0.136(9) 0.178(10) 0.095(7) 0.007(7) 0.032(7) -0.031(8) C36 0.114(10) 0.257(16) 0.069(7) -0.004(9) 0.030(7) -0.037(11) C37 0.041(4) 0.063(5) 0.056(4) -0.003(4) 0.015(3) 0.012(3) C38 0.069(7) 0.137(11) 0.071(7) 0.005(7) 0.021(5) 0.033(7) C39 0.095(9) 0.186(13) 0.104(9) -0.026(9) 0.024(7) 0.013(9) C40 0.048(4) 0.064(5) 0.053(4) 0.001(4) 0.001(3) 0.009(4) C41 0.082(7) 0.074(6) 0.050(5) 0.005(4) -0.002(4) 0.011(5) C42 0.123(10) 0.090(8) 0.053(6) 0.004(5) -0.013(6) 0.040(7) C43 0.048(4) 0.044(4) 0.084(6) -0.011(4) 0.003(4) -0.001(3) C44 0.112(7) 0.082(6) 0.119(8) -0.005(6) 0.041(6) -0.018(6) C45 0.117(10) 0.141(11) 0.098(9) -0.008(8) 0.046(8) -0.013(9) C46 0.046(4) 0.039(4) 0.052(4) -0.007(3) 0.009(3) 0.000(3) C47 0.067(5) 0.064(5) 0.049(4) -0.019(4) 0.014(4) -0.003(4) C48 0.071(6) 0.076(6) 0.087(7) -0.039(5) 0.037(5) -0.007(5) C49 0.27(2) 0.097(10) 0.073(8) -0.020(7) 0.064(11) -0.065(12) C50 0.149(12) 0.075(7) 0.070(7) 0.016(6) 0.034(7) 0.007(7) C53 0.067(6) 0.111(9) 0.101(8) 0.005(7) 0.035(6) -0.023(6) C54 0.072(8) 0.088(9) 0.28(2) 0.049(12) 0.031(11) 0.031(7) C55 0.092(7) 0.048(5) 0.126(9) -0.015(6) 0.057(7) -0.003(5) C56 0.071(6) 0.056(5) 0.134(10) -0.004(6) 0.055(7) -0.003(5) C57 0.150(12) 0.092(9) 0.076(8) -0.026(7) 0.060(8) -0.030(8) C58 0.129(11) 0.118(10) 0.049(5) 0.004(6) 0.030(6) -0.032(8) C59 0.114(11) 0.178(15) 0.070(7) 0.039(9) -0.018(7) -0.054(10) C60 0.116(10) 0.080(7) 0.082(7) 0.037(6) 0.001(7) 0.002(7) C51 0.152(9) 0.139(9) 0.110(8) 0.021(7) 0.075(7) 0.047(7) C52 0.181(9) 0.182(9) 0.182(9) -0.002(2) 0.033(3) 0.001(2) _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 Cu1 Cu2 2.8988(14) . ? Cu1 Cu3 2.9446(15) . ? Cu1 Cl1 2.261(2) . ? Cu1 Cl2 2.301(2) . ? Cu1 N1 2.195(10) . ? Cu1 N2 2.185(8) . ? Cu2 Cu3 2.6951(13) . ? Cu2 Cu4 2.4077(12) . ? Cu2 Cu5 3.0327(13) . ? Cu2 Cu6 3.0229(13) . ? Cu2 Cl2 2.163(2) . ? Cu2 C1 1.985(7) . ? Cu3 Cu4 2.7716(13) . ? Cu3 Cu5 2.5121(13) . ? Cu3 Cl1 2.187(2) . ? Cu3 C8 1.982(8) . ? Cu4 Cu5 2.5209(12) . ? Cu4 Cu6 2.5104(12) . ? Cu4 Cu7 2.4481(12) . ? Cu4 Cu8 2.9831(12) . ? Cu4 C1 2.001(7) . ? Cu4 C5 2.004(7) . ? Cu5 Cu6 2.4399(12) . ? Cu5 Cu7 2.6828(12) . ? Cu5 C8 2.008(7) . ? Cu5 C12 2.001(7) . ? Cu6 Cu7 2.5385(12) . ? Cu6 Cu8 2.4155(12) . ? Cu6 Cu9 2.8039(13) . ? Cu6 C4 2.011(7) . ? Cu6 C12 2.025(6) . ? Cu7 Cu8 2.8684(12) . ? Cu7 Cu9 2.5196(12) . ? Cu7 C5 2.006(7) . ? Cu7 C9 2.027(7) . ? Cu8 Cu9 2.6554(13) . ? Cu8 Cu10 3.0409(13) . ? Cu8 Cl3 2.1662(19) . ? Cu8 C4 1.992(7) . ? Cu9 Cu10 2.8286(14) . ? Cu9 Cl4 2.1828(19) . ? Cu9 C9 1.977(7) . ? Cu10 Cl3 2.307(2) . ? Cu10 Cl4 2.273(2) . ? Cu10 N3 2.220(8) . ? Cu10 N4 2.177(7) . ? N1 C53 1.411(14) . ? N1 C54 1.513(17) . ? N1 C52 1.407(16) . ? N2 C49 1.455(17) . ? N2 C50 1.493(13) . ? N2 C51 1.463(14) . ? N3 C58 1.492(15) . ? N3 C59 1.461(14) . ? N3 C60 1.482(14) . ? N4 C55 1.484(12) . ? N4 C56 1.466(12) . ? N4 C57 1.438(15) . ? C1 C2 1.377(10) . ? C1 C13 1.528(9) . ? C2 C3 1.502(10) . ? C2 C16 1.528(10) . ? C3 C4 1.356(9) . ? C3 C19 1.528(10) . ? C4 C22 1.527(9) . ? C5 C6 1.361(9) . ? C5 C25 1.546(9) . ? C6 C7 1.516(10) . ? C6 C28 1.524(10) . ? C7 C8 1.354(10) . ? C7 C31 1.513(10) . ? C8 C34 1.537(10) . ? C9 C10 1.350(10) . ? C9 C37 1.522(10) . ? C10 C11 1.505(10) . ? C10 C40 1.530(10) . ? C11 C12 1.362(10) . ? C11 C43 1.536(10) . ? C12 C46 1.524(10) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 C14 1.524(10) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C14 C15 1.536(11) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C16 C17 1.527(11) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C17 C18 1.526(11) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C19 C20 1.498(12) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C20 C21 1.499(9) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C22 C23 1.519(11) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 C24 1.527(11) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C25 C26 1.522(10) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C26 C27 1.533(11) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C28 C29 1.506(11) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C29 C30 1.514(11) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C31 C32 1.509(12) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C32 C33 1.520(13) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9900 . ? C34 H34B 0.9900 . ? C34 C35 1.490(16) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C35 C36 1.553(18) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C37 C38 1.614(14) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C38 C39 1.502(17) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C40 C41 1.524(12) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C41 C42 1.497(13) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C43 C44 1.467(14) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C44 C45 1.487(9) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C46 C47 1.528(11) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C47 C48 1.536(11) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C53 H53A 0.9799 . ? C53 H53B 0.9800 . ? C53 H53C 0.9799 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C57 C58 1.515(18) . ? C58 H58A 0.9900 . ? C58 H58B 0.9900 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C51 C52 1.426(16) . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? 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 Cu2 Cu1 Cu3 54.93(3) . . ? Cl1 Cu1 Cu2 86.66(6) . . ? Cl1 Cu1 Cu3 47.48(6) . . ? Cl1 Cu1 Cl2 131.40(8) . . ? Cl2 Cu1 Cu2 47.45(5) . . ? Cl2 Cu1 Cu3 87.12(6) . . ? N1 Cu1 Cu2 113.6(3) . . ? N1 Cu1 Cu3 153.0(3) . . ? N1 Cu1 Cl1 112.9(3) . . ? N1 Cu1 Cl2 101.7(3) . . ? N2 Cu1 Cu2 146.9(3) . . ? N2 Cu1 Cu3 118.4(3) . . ? N2 Cu1 Cl1 112.3(2) . . ? N2 Cu1 Cl2 103.7(3) . . ? N2 Cu1 N1 84.6(4) . . ? Cu1 Cu2 Cu5 101.42(4) . . ? Cu1 Cu2 Cu6 144.91(4) . . ? Cu3 Cu2 Cu1 63.40(4) . . ? Cu3 Cu2 Cu5 51.62(3) . . ? Cu3 Cu2 Cu6 96.42(4) . . ? Cu4 Cu2 Cu1 126.94(5) . . ? Cu4 Cu2 Cu3 65.51(4) . . ? Cu4 Cu2 Cu5 53.73(3) . . ? Cu4 Cu2 Cu6 53.63(3) . . ? Cu6 Cu2 Cu5 47.52(3) . . ? Cl2 Cu2 Cu1 51.61(6) . . ? Cl2 Cu2 Cu3 96.61(7) . . ? Cl2 Cu2 Cu4 149.40(8) . . ? Cl2 Cu2 Cu5 95.67(7) . . ? Cl2 Cu2 Cu6 108.03(6) . . ? C1 Cu2 Cu1 124.1(2) . . ? C1 Cu2 Cu3 99.7(2) . . ? C1 Cu2 Cu4 53.1(2) . . ? C1 Cu2 Cu5 106.8(2) . . ? C1 Cu2 Cu6 85.7(2) . . ? C1 Cu2 Cl2 157.3(2) . . ? Cu2 Cu3 Cu1 61.67(4) . . ? Cu2 Cu3 Cu4 52.24(3) . . ? Cu4 Cu3 Cu1 112.47(4) . . ? Cu5 Cu3 Cu1 114.36(4) . . ? Cu5 Cu3 Cu2 71.14(4) . . ? Cu5 Cu3 Cu4 56.74(3) . . ? Cl1 Cu3 Cu1 49.64(6) . . ? Cl1 Cu3 Cu2 93.44(7) . . ? Cl1 Cu3 Cu4 119.63(7) . . ? Cl1 Cu3 Cu5 162.92(7) . . ? C8 Cu3 Cu1 142.1(2) . . ? C8 Cu3 Cu2 122.5(2) . . ? C8 Cu3 Cu4 89.0(2) . . ? C8 Cu3 Cu5 51.4(2) . . ? C8 Cu3 Cl1 143.9(2) . . ? Cu2 Cu4 Cu3 62.25(3) . . ? Cu2 Cu4 Cu5 75.91(4) . . ? Cu2 Cu4 Cu6 75.82(4) . . ? Cu2 Cu4 Cu7 132.90(5) . . ? Cu2 Cu4 Cu8 105.72(4) . . ? Cu3 Cu4 Cu8 158.97(4) . . ? Cu5 Cu4 Cu3 56.43(3) . . ? Cu5 Cu4 Cu8 105.24(4) . . ? Cu6 Cu4 Cu3 107.73(4) . . ? Cu6 Cu4 Cu5 58.02(3) . . ? Cu6 Cu4 Cu8 51.29(3) . . ? Cu7 Cu4 Cu3 111.27(4) . . ? Cu7 Cu4 Cu5 65.33(3) . . ? Cu7 Cu4 Cu6 61.57(3) . . ? Cu7 Cu4 Cu8 62.85(3) . . ? C1 Cu4 Cu2 52.5(2) . . ? C1 Cu4 Cu3 96.8(2) . . ? C1 Cu4 Cu5 128.3(2) . . ? C1 Cu4 Cu6 100.8(2) . . ? C1 Cu4 Cu7 150.0(2) . . ? C1 Cu4 Cu8 87.2(2) . . ? C1 Cu4 C5 138.5(3) . . ? C5 Cu4 Cu2 155.9(2) . . ? C5 Cu4 Cu3 93.69(19) . . ? C5 Cu4 Cu5 90.5(2) . . ? C5 Cu4 Cu6 113.9(2) . . ? C5 Cu4 Cu7 52.41(19) . . ? C5 Cu4 Cu8 96.92(19) . . ? Cu3 Cu5 Cu2 57.24(3) . . ? Cu3 Cu5 Cu4 66.83(4) . . ? Cu3 Cu5 Cu7 112.19(4) . . ? Cu4 Cu5 Cu2 50.36(3) . . ? Cu4 Cu5 Cu7 56.02(3) . . ? Cu6 Cu5 Cu2 66.03(3) . . ? Cu6 Cu5 Cu3 119.08(5) . . ? Cu6 Cu5 Cu4 60.77(3) . . ? Cu6 Cu5 Cu7 59.18(3) . . ? Cu7 Cu5 Cu2 102.14(4) . . ? C8 Cu5 Cu2 107.7(2) . . ? C8 Cu5 Cu3 50.5(2) . . ? C8 Cu5 Cu4 95.9(2) . . ? C8 Cu5 Cu6 154.8(2) . . ? C8 Cu5 Cu7 101.0(2) . . ? C12 Cu5 Cu2 100.2(2) . . ? C12 Cu5 Cu3 151.8(2) . . ? C12 Cu5 Cu4 113.89(19) . . ? C12 Cu5 Cu6 53.13(19) . . ? C12 Cu5 Cu7 87.6(2) . . ? C12 Cu5 C8 148.2(3) . . ? Cu4 Cu6 Cu2 50.56(3) . . ? Cu4 Cu6 Cu7 58.01(3) . . ? Cu4 Cu6 Cu9 108.37(4) . . ? Cu5 Cu6 Cu2 66.45(3) . . ? Cu5 Cu6 Cu4 61.21(3) . . ? Cu5 Cu6 Cu7 65.18(3) . . ? Cu5 Cu6 Cu9 109.62(4) . . ? Cu7 Cu6 Cu2 106.01(4) . . ? Cu7 Cu6 Cu9 56.01(3) . . ? Cu8 Cu6 Cu2 104.34(4) . . ? Cu8 Cu6 Cu4 74.52(4) . . ? Cu8 Cu6 Cu5 129.01(5) . . ? Cu8 Cu6 Cu7 70.71(3) . . ? Cu8 Cu6 Cu9 60.62(3) . . ? Cu9 Cu6 Cu2 158.52(4) . . ? C4 Cu6 Cu2 82.8(2) . . ? C4 Cu6 Cu4 95.9(2) . . ? C4 Cu6 Cu5 148.9(2) . . ? C4 Cu6 Cu7 122.6(2) . . ? C4 Cu6 Cu8 52.5(2) . . ? C4 Cu6 Cu9 97.1(2) . . ? C4 Cu6 C12 144.3(3) . . ? C12 Cu6 Cu2 99.9(2) . . ? C12 Cu6 Cu4 113.4(2) . . ? C12 Cu6 Cu5 52.2(2) . . ? C12 Cu6 Cu7 91.1(2) . . ? C12 Cu6 Cu8 152.9(2) . . ? C12 Cu6 Cu9 92.7(2) . . ? Cu4 Cu7 Cu5 58.64(3) . . ? Cu4 Cu7 Cu6 60.42(3) . . ? Cu4 Cu7 Cu8 67.73(3) . . ? Cu4 Cu7 Cu9 120.49(4) . . ? Cu5 Cu7 Cu8 104.23(4) . . ? Cu6 Cu7 Cu5 55.64(3) . . ? Cu6 Cu7 Cu8 52.64(3) . . ? Cu9 Cu7 Cu5 111.09(4) . . ? Cu9 Cu7 Cu6 67.33(4) . . ? Cu9 Cu7 Cu8 58.63(3) . . ? C5 Cu7 Cu4 52.34(19) . . ? C5 Cu7 Cu5 85.95(19) . . ? C5 Cu7 Cu6 112.70(19) . . ? C5 Cu7 Cu8 100.5(2) . . ? C5 Cu7 Cu9 155.1(2) . . ? C5 Cu7 C9 148.0(3) . . ? C9 Cu7 Cu4 153.1(2) . . ? C9 Cu7 Cu5 98.8(2) . . ? C9 Cu7 Cu6 95.5(2) . . ? C9 Cu7 Cu8 108.7(2) . . ? C9 Cu7 Cu9 50.13(19) . . ? Cu4 Cu8 Cu10 146.20(4) . . ? Cu6 Cu8 Cu4 54.19(3) . . ? Cu6 Cu8 Cu7 56.65(3) . . ? Cu6 Cu8 Cu9 66.94(3) . . ? Cu6 Cu8 Cu10 123.91(4) . . ? Cu7 Cu8 Cu4 49.42(3) . . ? Cu7 Cu8 Cu10 99.09(4) . . ? Cu9 Cu8 Cu4 99.64(4) . . ? Cu9 Cu8 Cu7 54.11(3) . . ? Cu9 Cu8 Cu10 59.09(3) . . ? Cl3 Cu8 Cu4 113.70(6) . . ? Cl3 Cu8 Cu6 151.60(7) . . ? Cl3 Cu8 Cu7 95.46(6) . . ? Cl3 Cu8 Cu9 93.32(6) . . ? Cl3 Cu8 Cu10 49.15(5) . . ? C4 Cu8 Cu4 82.8(2) . . ? C4 Cu8 Cu6 53.2(2) . . ? C4 Cu8 Cu7 109.4(2) . . ? C4 Cu8 Cu9 102.4(2) . . ? C4 Cu8 Cu10 125.0(2) . . ? C4 Cu8 Cl3 155.1(2) . . ? Cu6 Cu9 Cu10 117.87(4) . . ? Cu7 Cu9 Cu6 56.66(3) . . ? Cu7 Cu9 Cu8 67.26(3) . . ? Cu7 Cu9 Cu10 114.37(4) . . ? Cu8 Cu9 Cu6 52.44(3) . . ? Cu8 Cu9 Cu10 67.27(3) . . ? Cl4 Cu9 Cu6 120.97(6) . . ? Cl4 Cu9 Cu7 165.05(7) . . ? Cl4 Cu9 Cu8 99.25(6) . . ? Cl4 Cu9 Cu10 52.03(6) . . ? C9 Cu9 Cu6 88.8(2) . . ? C9 Cu9 Cu7 51.9(2) . . ? C9 Cu9 Cu8 119.1(2) . . ? C9 Cu9 Cu10 137.7(2) . . ? C9 Cu9 Cl4 141.3(2) . . ? Cu9 Cu10 Cu8 53.65(3) . . ? Cl3 Cu10 Cu8 45.26(5) . . ? Cl3 Cu10 Cu9 85.99(6) . . ? Cl4 Cu10 Cu8 86.95(6) . . ? Cl4 Cu10 Cu9 49.19(5) . . ? Cl4 Cu10 Cl3 130.76(8) . . ? N3 Cu10 Cu8 120.5(2) . . ? N3 Cu10 Cu9 154.7(3) . . ? N3 Cu10 Cl3 105.9(2) . . ? N3 Cu10 Cl4 109.7(3) . . ? N4 Cu10 Cu8 141.69(19) . . ? N4 Cu10 Cu9 115.2(2) . . ? N4 Cu10 Cl3 102.99(19) . . ? N4 Cu10 Cl4 113.3(2) . . ? N4 Cu10 N3 84.3(3) . . ? Cu3 Cl1 Cu1 82.88(8) . . ? Cu2 Cl2 Cu1 80.94(7) . . ? Cu8 Cl3 Cu10 85.60(7) . . ? Cu9 Cl4 Cu10 78.78(7) . . ? C53 N1 Cu1 114.0(8) . . ? C53 N1 C54 109.0(12) . . ? C54 N1 Cu1 112.7(7) . . ? C52 N1 Cu1 104.3(11) . . ? C52 N1 C53 115.3(13) . . ? C52 N1 C54 100.9(13) . . ? C49 N2 Cu1 112.0(7) . . ? C49 N2 C50 108.2(11) . . ? C49 N2 C51 114.6(12) . . ? C50 N2 Cu1 113.3(6) . . ? C51 N2 Cu1 101.7(8) . . ? C51 N2 C50 107.0(10) . . ? C58 N3 Cu10 103.3(7) . . ? C59 N3 Cu10 108.6(7) . . ? C59 N3 C58 109.6(10) . . ? C59 N3 C60 111.7(11) . . ? C60 N3 Cu10 113.7(7) . . ? C60 N3 C58 109.6(9) . . ? C55 N4 Cu10 112.8(5) . . ? C56 N4 Cu10 111.8(5) . . ? C56 N4 C55 108.3(8) . . ? C57 N4 Cu10 102.3(7) . . ? C57 N4 C55 109.8(8) . . ? C57 N4 C56 111.7(8) . . ? Cu2 C1 Cu4 74.3(2) . . ? C2 C1 Cu2 110.3(5) . . ? C2 C1 Cu4 117.6(5) . . ? C2 C1 C13 120.6(6) . . ? C13 C1 Cu2 119.8(5) . . ? C13 C1 Cu4 105.4(4) . . ? C1 C2 C3 123.8(6) . . ? C1 C2 C16 122.1(6) . . ? C3 C2 C16 114.0(6) . . ? C2 C3 C19 111.9(6) . . ? C4 C3 C2 125.6(6) . . ? C4 C3 C19 122.4(7) . . ? Cu8 C4 Cu6 74.2(2) . . ? C3 C4 Cu6 123.3(5) . . ? C3 C4 Cu8 108.5(5) . . ? C3 C4 C22 120.6(6) . . ? C22 C4 Cu6 104.1(4) . . ? C22 C4 Cu8 117.9(5) . . ? Cu4 C5 Cu7 75.2(2) . . ? C6 C5 Cu4 114.8(5) . . ? C6 C5 Cu7 117.4(5) . . ? C6 C5 C25 119.8(6) . . ? C25 C5 Cu4 102.9(5) . . ? C25 C5 Cu7 116.5(5) . . ? C5 C6 C7 126.2(6) . . ? C5 C6 C28 122.5(7) . . ? C7 C6 C28 111.3(6) . . ? C8 C7 C6 122.6(7) . . ? C8 C7 C31 123.9(7) . . ? C31 C7 C6 113.3(6) . . ? Cu3 C8 Cu5 78.0(3) . . ? C7 C8 Cu3 116.2(6) . . ? C7 C8 Cu5 110.3(5) . . ? C7 C8 C34 121.4(7) . . ? C34 C8 Cu3 113.4(5) . . ? C34 C8 Cu5 108.6(5) . . ? Cu9 C9 Cu7 78.0(2) . . ? C10 C9 Cu7 113.0(5) . . ? C10 C9 Cu9 113.0(5) . . ? C10 C9 C37 122.5(7) . . ? C37 C9 Cu7 107.9(5) . . ? C37 C9 Cu9 113.7(5) . . ? C9 C10 C11 126.5(6) . . ? C9 C10 C40 120.1(7) . . ? C11 C10 C40 113.4(6) . . ? C10 C11 C43 113.0(6) . . ? C12 C11 C10 126.0(7) . . ? C12 C11 C43 120.9(7) . . ? Cu5 C12 Cu6 74.6(2) . . ? C11 C12 Cu5 116.8(5) . . ? C11 C12 Cu6 116.3(5) . . ? C11 C12 C46 120.4(6) . . ? C46 C12 Cu5 113.3(5) . . ? C46 C12 Cu6 106.2(5) . . ? C1 C13 H13A 109.3 . . ? C1 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? C14 C13 C1 111.8(6) . . ? C14 C13 H13A 109.3 . . ? C14 C13 H13B 109.3 . . ? C13 C14 H14A 109.0 . . ? C13 C14 H14B 109.0 . . ? C13 C14 C15 112.9(7) . . ? H14A C14 H14B 107.8 . . ? C15 C14 H14A 109.0 . . ? C15 C14 H14B 109.0 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C2 C16 H16A 108.9 . . ? C2 C16 H16B 108.9 . . ? H16A C16 H16B 107.8 . . ? C17 C16 C2 113.2(6) . . ? C17 C16 H16A 108.9 . . ? C17 C16 H16B 108.9 . . ? C16 C17 H17A 109.2 . . ? C16 C17 H17B 109.2 . . ? H17A C17 H17B 107.9 . . ? C18 C17 C16 112.2(7) . . ? C18 C17 H17A 109.2 . . ? C18 C17 H17B 109.2 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C3 C19 H19A 108.6 . . ? C3 C19 H19B 108.6 . . ? H19A C19 H19B 107.6 . . ? C20 C19 C3 114.6(8) . . ? C20 C19 H19A 108.6 . . ? C20 C19 H19B 108.6 . . ? C19 C20 H20A 108.3 . . ? C19 C20 H20B 108.3 . . ? C19 C20 C21 115.9(12) . . ? H20A C20 H20B 107.4 . . ? C21 C20 H20A 108.3 . . ? C21 C20 H20B 108.3 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C4 C22 H22A 109.0 . . ? C4 C22 H22B 109.0 . . ? H22A C22 H22B 107.8 . . ? C23 C22 C4 112.7(6) . . ? C23 C22 H22A 109.0 . . ? C23 C22 H22B 109.0 . . ? C22 C23 H23A 109.0 . . ? C22 C23 H23B 109.0 . . ? C22 C23 C24 112.8(8) . . ? H23A C23 H23B 107.8 . . ? C24 C23 H23A 109.0 . . ? C24 C23 H23B 109.0 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C5 C25 H25A 109.2 . . ? C5 C25 H25B 109.2 . . ? H25A C25 H25B 107.9 . . ? C26 C25 C5 112.3(6) . . ? C26 C25 H25A 109.2 . . ? C26 C25 H25B 109.2 . . ? C25 C26 H26A 109.3 . . ? C25 C26 H26B 109.3 . . ? C25 C26 C27 111.7(7) . . ? H26A C26 H26B 107.9 . . ? C27 C26 H26A 109.3 . . ? C27 C26 H26B 109.3 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C6 C28 H28A 108.7 . . ? C6 C28 H28B 108.7 . . ? H28A C28 H28B 107.6 . . ? C29 C28 C6 114.2(6) . . ? C29 C28 H28A 108.7 . . ? C29 C28 H28B 108.7 . . ? C28 C29 H29A 109.0 . . ? C28 C29 H29B 109.0 . . ? C28 C29 C30 113.0(7) . . ? H29A C29 H29B 107.8 . . ? C30 C29 H29A 109.0 . . ? C30 C29 H29B 109.0 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C7 C31 H31A 109.0 . . ? C7 C31 H31B 109.0 . . ? H31A C31 H31B 107.8 . . ? C32 C31 C7 113.0(7) . . ? C32 C31 H31A 109.0 . . ? C32 C31 H31B 109.0 . . ? C31 C32 H32A 108.8 . . ? C31 C32 H32B 108.8 . . ? C31 C32 C33 114.0(8) . . ? H32A C32 H32B 107.7 . . ? C33 C32 H32A 108.8 . . ? C33 C32 H32B 108.8 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33B 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C8 C34 H34A 109.2 . . ? C8 C34 H34B 109.2 . . ? H34A C34 H34B 107.9 . . ? C35 C34 C8 112.0(9) . . ? C35 C34 H34A 109.2 . . ? C35 C34 H34B 109.2 . . ? C34 C35 H35A 109.4 . . ? C34 C35 H35B 109.4 . . ? C34 C35 C36 111.4(12) . . ? H35A C35 H35B 108.0 . . ? C36 C35 H35A 109.4 . . ? C36 C35 H35B 109.4 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C9 C37 H37A 110.0 . . ? C9 C37 H37B 110.0 . . ? C9 C37 C38 108.4(7) . . ? H37A C37 H37B 108.4 . . ? C38 C37 H37A 110.0 . . ? C38 C37 H37B 110.0 . . ? C37 C38 H38A 110.4 . . ? C37 C38 H38B 110.4 . . ? H38A C38 H38B 108.6 . . ? C39 C38 C37 106.7(11) . . ? C39 C38 H38A 110.4 . . ? C39 C38 H38B 110.4 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C10 C40 H40A 108.6 . . ? C10 C40 H40B 108.6 . . ? H40A C40 H40B 107.6 . . ? C41 C40 C10 114.6(7) . . ? C41 C40 H40A 108.6 . . ? C41 C40 H40B 108.6 . . ? C40 C41 H41A 109.1 . . ? C40 C41 H41B 109.1 . . ? H41A C41 H41B 107.8 . . ? C42 C41 C40 112.6(9) . . ? C42 C41 H41A 109.1 . . ? C42 C41 H41B 109.1 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C11 C43 H43A 108.3 . . ? C11 C43 H43B 108.3 . . ? H43A C43 H43B 107.4 . . ? C44 C43 C11 116.0(9) . . ? C44 C43 H43A 108.3 . . ? C44 C43 H43B 108.3 . . ? C43 C44 H44A 109.6 . . ? C43 C44 H44B 109.6 . . ? C43 C44 C45 110.2(11) . . ? H44A C44 H44B 108.1 . . ? C45 C44 H44A 109.6 . . ? C45 C44 H44B 109.6 . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45B 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C12 C46 H46A 109.8 . . ? C12 C46 H46B 109.8 . . ? C12 C46 C47 109.5(6) . . ? H46A C46 H46B 108.2 . . ? C47 C46 H46A 109.8 . . ? C47 C46 H46B 109.8 . . ? C46 C47 H47A 109.0 . . ? C46 C47 H47B 109.0 . . ? C46 C47 C48 112.8(8) . . ? H47A C47 H47B 107.8 . . ? C48 C47 H47A 109.0 . . ? C48 C47 H47B 109.0 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48B 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N2 C49 H49A 109.5 . . ? N2 C49 H49B 109.5 . . ? N2 C49 H49C 109.5 . . ? H49A C49 H49B 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N2 C50 H50A 109.5 . . ? N2 C50 H50B 109.5 . . ? N2 C50 H50C 109.5 . . ? H50A C50 H50B 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N1 C53 H53A 108.3 . . ? N1 C53 H53B 109.9 . . ? N1 C53 H53C 110.1 . . ? H53A C53 H53B 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N1 C54 H54A 109.5 . . ? N1 C54 H54B 109.5 . . ? N1 C54 H54C 109.5 . . ? H54A C54 H54B 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N4 C55 H55A 109.5 . . ? N4 C55 H55B 109.5 . . ? N4 C55 H55C 109.5 . . ? H55A C55 H55B 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N4 C56 H56A 109.5 . . ? N4 C56 H56B 109.5 . . ? N4 C56 H56C 109.5 . . ? H56A C56 H56B 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? N4 C57 H57A 109.0 . . ? N4 C57 H57B 109.0 . . ? N4 C57 C58 113.1(9) . . ? H57A C57 H57B 107.8 . . ? C58 C57 H57A 109.0 . . ? C58 C57 H57B 109.0 . . ? N3 C58 C57 111.3(9) . . ? N3 C58 H58A 109.4 . . ? N3 C58 H58B 109.4 . . ? C57 C58 H58A 109.4 . . ? C57 C58 H58B 109.4 . . ? H58A C58 H58B 108.0 . . ? N3 C59 H59A 109.5 . . ? N3 C59 H59B 109.5 . . ? N3 C59 H59C 109.5 . . ? H59A C59 H59B 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? N3 C60 H60A 109.5 . . ? N3 C60 H60B 109.5 . . ? N3 C60 H60C 109.5 . . ? H60A C60 H60B 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? N2 C51 H51A 106.6 . . ? N2 C51 H51B 106.6 . . ? H51A C51 H51B 106.6 . . ? C52 C51 N2 122.8(13) . . ? C52 C51 H51A 106.6 . . ? C52 C51 H51B 106.6 . . ? N1 C52 C51 115.7(17) . . ? N1 C52 H52A 108.4 . . ? N1 C52 H52B 108.4 . . ? C51 C52 H52A 108.4 . . ? C51 C52 H52B 108.4 . . ? H52A C52 H52B 107.4 . . ? 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 Cu1 N1 C52 C51 -33(2) . . . . ? Cu1 N2 C51 C52 -19(2) . . . . ? Cu2 C1 C2 C3 26.8(8) . . . . ? Cu2 C1 C2 C16 -149.7(6) . . . . ? Cu2 C1 C13 C14 63.1(7) . . . . ? Cu3 C8 C34 C35 48.9(11) . . . . ? Cu4 C1 C2 C3 -55.6(8) . . . . ? Cu4 C1 C2 C16 127.9(6) . . . . ? Cu4 C1 C13 C14 143.6(5) . . . . ? Cu4 C5 C6 C7 -61.0(9) . . . . ? Cu4 C5 C6 C28 121.3(6) . . . . ? Cu4 C5 C25 C26 147.2(5) . . . . ? Cu5 C8 C34 C35 133.6(10) . . . . ? Cu5 C12 C46 C47 57.6(7) . . . . ? Cu6 C4 C22 C23 137.2(5) . . . . ? Cu6 C12 C46 C47 137.5(6) . . . . ? Cu7 C5 C6 C7 24.6(9) . . . . ? Cu7 C5 C6 C28 -153.1(6) . . . . ? Cu7 C5 C25 C26 67.4(7) . . . . ? Cu7 C9 C10 C11 -55.7(9) . . . . ? Cu7 C9 C10 C40 126.5(6) . . . . ? Cu7 C9 C37 C38 153.4(6) . . . . ? Cu8 C4 C22 C23 57.8(7) . . . . ? Cu9 C9 C10 C11 30.5(9) . . . . ? Cu9 C9 C10 C40 -147.2(6) . . . . ? Cu9 C9 C37 C38 68.9(8) . . . . ? Cu10 N3 C58 C57 34.5(11) . . . . ? Cu10 N4 C57 C58 47.1(11) . . . . ? N2 C51 C52 N1 39(3) . . . . ? N4 C57 C58 N3 -59.9(14) . . . . ? C1 C2 C3 C4 58.4(11) . . . . ? C1 C2 C3 C19 -125.1(8) . . . . ? C1 C2 C16 C17 -126.7(7) . . . . ? C1 C13 C14 C15 -174.7(7) . . . . ? C2 C1 C13 C14 -80.3(8) . . . . ? C2 C3 C4 Cu6 -50.0(10) . . . . ? C2 C3 C4 Cu8 32.9(9) . . . . ? C2 C3 C4 C22 173.3(7) . . . . ? C2 C3 C19 C20 61.1(10) . . . . ? C2 C16 C17 C18 -177.1(7) . . . . ? C3 C2 C16 C17 56.4(9) . . . . ? C3 C4 C22 C23 -79.0(9) . . . . ? C3 C19 C20 C21 109.6(14) . . . . ? C4 C3 C19 C20 -122.3(9) . . . . ? C4 C22 C23 C24 -173.4(7) . . . . ? C5 C6 C7 C8 60.9(11) . . . . ? C5 C6 C7 C31 -123.6(8) . . . . ? C5 C6 C28 C29 -115.5(9) . . . . ? C5 C25 C26 C27 -174.2(6) . . . . ? C6 C5 C25 C26 -83.9(8) . . . . ? C6 C7 C8 Cu3 24.3(9) . . . . ? C6 C7 C8 Cu5 -62.0(8) . . . . ? C6 C7 C8 C34 169.3(7) . . . . ? C6 C7 C31 C32 53.8(10) . . . . ? C6 C28 C29 C30 -176.5(8) . . . . ? C7 C6 C28 C29 66.5(9) . . . . ? C7 C8 C34 C35 -97.0(12) . . . . ? C7 C31 C32 C33 178.3(10) . . . . ? C8 C7 C31 C32 -130.8(9) . . . . ? C8 C34 C35 C36 -168.9(12) . . . . ? C9 C10 C11 C12 52.9(11) . . . . ? C9 C10 C11 C43 -129.7(8) . . . . ? C9 C10 C40 C41 -130.9(8) . . . . ? C9 C37 C38 C39 171.7(9) . . . . ? C10 C9 C37 C38 -72.9(9) . . . . ? C10 C11 C12 Cu5 28.4(9) . . . . ? C10 C11 C12 Cu6 -56.9(9) . . . . ? C10 C11 C12 C46 172.5(7) . . . . ? C10 C11 C43 C44 72.5(10) . . . . ? C10 C40 C41 C42 174.8(8) . . . . ? C11 C10 C40 C41 51.1(10) . . . . ? C11 C12 C46 C47 -87.8(8) . . . . ? C11 C43 C44 C45 75.4(12) . . . . ? C12 C11 C43 C44 -110.0(10) . . . . ? C12 C46 C47 C48 -177.6(7) . . . . ? C13 C1 C2 C3 173.3(6) . . . . ? C13 C1 C2 C16 -3.2(10) . . . . ? C16 C2 C3 C4 -124.8(8) . . . . ? C16 C2 C3 C19 51.7(8) . . . . ? C19 C3 C4 Cu6 133.8(7) . . . . ? C19 C3 C4 Cu8 -143.3(6) . . . . ? C19 C3 C4 C22 -2.9(11) . . . . ? C25 C5 C6 C7 175.7(7) . . . . ? C25 C5 C6 C28 -2.0(10) . . . . ? C28 C6 C7 C8 -121.2(8) . . . . ? C28 C6 C7 C31 54.3(9) . . . . ? C31 C7 C8 Cu3 -150.7(7) . . . . ? C31 C7 C8 Cu5 123.0(7) . . . . ? C31 C7 C8 C34 -5.7(12) . . . . ? C37 C9 C10 C11 172.6(7) . . . . ? C37 C9 C10 C40 -5.2(11) . . . . ? C40 C10 C11 C12 -129.2(8) . . . . ? C40 C10 C11 C43 48.2(9) . . . . ? C43 C11 C12 Cu5 -148.8(6) . . . . ? C43 C11 C12 Cu6 125.9(7) . . . . ? C43 C11 C12 C46 -4.6(11) . . . . ? C49 N2 C51 C52 102(2) . . . . ? C50 N2 C51 C52 -137.7(18) . . . . ? C53 N1 C52 C51 92(2) . . . . ? C54 N1 C52 C51 -150.4(18) . . . . ? C55 N4 C57 C58 167.2(10) . . . . ? C56 N4 C57 C58 -72.7(12) . . . . ? C59 N3 C58 C57 -81.1(12) . . . . ? C60 N3 C58 C57 156.0(10) . . . . ? _olex2_submission_special_instructions 'No special instructions were received' #===END data_6 _audit_creation_date 2015-07-11 _audit_creation_method ; Olex2 1.2 (compiled 2015.01.26 svn.r3150 for OlexSys, GUI svn.r4998) ; _shelxl_version_number 2013-2 _publ_contact_author_address ? _publ_contact_author_email ? _publ_contact_author_name '' _publ_contact_author_phone ? _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. Palatinus, L. & Chapuis, G. (2007). J. Appl. Cryst., 40, 786-790; Palatinus, L. & van der Lee, A. (2008). J. Appl. Cryst. 41, 975-984; Palatinus, L., Prathapa, S. J. & van Smaalen, S. (2012). J. Appl. Cryst. 45, 575-580. Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122. ; _chemical_name_common ? _chemical_name_systematic ? _chemical_formula_moiety 'C48 H92 Cl4 Cu10 N4' _chemical_formula_sum 'C48 H92 Cl4 Cu10 N4' _chemical_formula_weight 1502.45 _chemical_melting_point ? _chemical_oxdiff_formula 'C50 H100 Cu10 Cl4 N4' 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8027(5) _cell_length_b 12.3566(4) _cell_length_c 24.9990(5) _cell_angle_alpha 87.633(2) _cell_angle_beta 83.322(3) _cell_angle_gamma 62.031(4) _cell_volume 3197.8(2) _cell_formula_units_Z 2 _cell_measurement_reflns_used 11396 _cell_measurement_temperature 180.00(10) _cell_measurement_theta_max 28.0810 _cell_measurement_theta_min 3.3430 _shelx_estimated_absorpt_T_max 0.846 _shelx_estimated_absorpt_T_min 0.724 _exptl_absorpt_coefficient_mu 3.452 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.92070 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear orangish yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier orangish _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.560 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_description block _exptl_crystal_F_000 1532 _exptl_crystal_preparation ? _exptl_crystal_recrystallization_method ? _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.05 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0363 _diffrn_reflns_av_unetI/netI 0.0601 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 30460 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 26.020 _diffrn_reflns_theta_min 3.009 _diffrn_ambient_temperature 180.00(10) _diffrn_detector_area_resol_mean 10.3914 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_details ; #__ type_ start__ end____ width___ exp.time_ 1 omega -17.00 57.00 1.0000 48.0000 omega____ theta____ kappa____ phi______ frames - 10.7017 57.0000 0.0000 74 #__ type_ start__ end____ width___ exp.time_ 2 omega 45.00 97.00 1.0000 48.0000 omega____ theta____ kappa____ phi______ frames - 10.7017 -178.0000 120.0000 52 #__ type_ start__ end____ width___ exp.time_ 3 omega -20.00 6.00 1.0000 48.0000 omega____ theta____ kappa____ phi______ frames - 10.7017 -38.0000 -180.0000 26 #__ type_ start__ end____ width___ exp.time_ 4 omega -86.00 15.00 1.0000 48.0000 omega____ theta____ kappa____ phi______ frames - -11.4829 -43.0000 97.0000 101 #__ type_ start__ end____ width___ exp.time_ 5 omega -19.00 14.00 1.0000 48.0000 omega____ theta____ kappa____ phi______ frames - -11.4829 -99.0000 120.0000 33 #__ type_ start__ end____ width___ exp.time_ 6 omega -58.00 52.00 1.0000 48.0000 omega____ theta____ kappa____ phi______ frames - -11.4829 19.0000 -60.0000 110 ; _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_UB_11 -0.0483872000 _diffrn_orient_matrix_UB_12 0.0512028000 _diffrn_orient_matrix_UB_13 0.0153059000 _diffrn_orient_matrix_UB_21 -0.0446691000 _diffrn_orient_matrix_UB_22 -0.0226848000 _diffrn_orient_matrix_UB_23 -0.0016924000 _diffrn_orient_matrix_UB_31 0.0187073000 _diffrn_orient_matrix_UB_32 -0.0329964000 _diffrn_orient_matrix_UB_33 0.0240649000 _diffrn_radiation_monochromator mirror _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'SuperNova (Mo) X-ray Source' _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 9543 _reflns_number_total 12575 _reflns_odcompleteness_completeness 99.77 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 25.97 _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, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.32 (release 02-08-2013 CrysAlis171 .NET) (compiled Aug 2 2013,16:46:58) ; _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2008)' _computing_structure_solution ; Superflip (Palatinus & Chapuis, 2007;Palatinus & van der Lee, 2008; Palatinus et al., 2012) ; _refine_diff_density_max 1.847 _refine_diff_density_min -1.294 _refine_diff_density_rms 0.122 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 615 _refine_ls_number_reflns 12575 _refine_ls_number_restraints 15 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0439 _refine_ls_restrained_S_all 1.075 _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^)+(0.0570P)^2^+3.0050P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1163 _refine_ls_wR_factor_ref 0.1310 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C8-C27 1.54 with sigma of 0.02 3. Rigid bond restraints C30 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C30, C29 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C27, C28 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 4. Uiso/Uaniso restraints and constraints Uanis(C30) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C30) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C28) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 Uanis(C28) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 Uanis(C28) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 Uanis(C28) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 5.a Secondary CH2 refined with riding coordinates: C15(H15A,H15B), C19(H19A,H19B), C33(H33A,H33B), C23(H23A,H23B), C35(H35A, H35B), C21(H21A,H21B), C31(H31A,H31B), C17(H17A,H17B), C13(H13A,H13B), C44(H44A,H44B), C29(H29A,H29B), C38(H38A,H38B), C25(H25A,H25B), C43(H43A,H43B), C37(H37A,H37B), C27(H27A,H27B) 5.b Idealised Me refined as rotating group: C34(H34A,H34B,H34C), C22(H22A,H22B,H22C), C24(H24A,H24B,H24C), C20(H20A,H20B, H20C), C16(H16A,H16B,H16C), C18(H18A,H18B,H18C), C45(H45A,H45B,H45C), C41(H41A, H41B,H41C), C32(H32A,H32B,H32C), C47(H47A,H47B,H47C), C36(H36A,H36B,H36C), C39(H39A,H39B,H39C), C14(H14A,H14B,H14C), C46(H46A,H46B,H46C), C40(H40A,H40B, H40C), C26(H26A,H26B,H26C), C42(H42A,H42B,H42C), C48(H48A,H48B,H48C), C30(H30A, H30B,H30C), C28(H28A,H28B,H28C) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _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 Cu7 Cu 0.55085(6) 0.63713(5) 0.23763(2) 0.02478(14) Uani 1 1 d . . . . . Cu9 Cu 0.72582(6) 0.56491(5) 0.16640(2) 0.02767(15) Uani 1 1 d . . . . . Cu4 Cu 0.68922(6) 0.73004(5) 0.26126(2) 0.02689(15) Uani 1 1 d . . . . . Cu6 Cu 0.55448(6) 0.82360(5) 0.18955(2) 0.02821(15) Uani 1 1 d . . . . . Cu5 Cu 0.44605(6) 0.82422(5) 0.28962(2) 0.02985(16) Uani 1 1 d . . . . . Cu2 Cu 0.67446(6) 0.61263(6) 0.33813(2) 0.02958(16) Uani 1 1 d . . . . . Cu8 Cu 0.48486(6) 0.71017(6) 0.13454(2) 0.03078(16) Uani 1 1 d . . . . . Cu3 Cu 0.55653(8) 0.87292(7) 0.35345(3) 0.04058(19) Uani 1 1 d . . . . . Cu1 Cu 0.61196(8) 0.69236(7) 0.44886(3) 0.04223(19) Uani 1 1 d . . . . . Cu10 Cu 0.69994(8) 0.53995(7) 0.05012(3) 0.04517(19) Uani 1 1 d . . . . . Cl1 Cl 0.56429(15) 0.56649(13) 0.40169(5) 0.0378(3) Uani 1 1 d . . . . . Cl4 Cl 0.82555(15) 0.59848(14) 0.09491(5) 0.0401(3) Uani 1 1 d . . . . . Cl3 Cl 0.50620(14) 0.56012(13) 0.08573(5) 0.0380(3) Uani 1 1 d . . . . . Cl2 Cl 0.67949(18) 0.83004(14) 0.41721(5) 0.0493(4) Uani 1 1 d . . . . . C34 C 0.1832(7) 0.6878(7) 0.1800(3) 0.0625(19) Uani 1 1 d . . . . . H34A H 0.2031 0.7210 0.1461 0.094 Uiso 1 1 calc GR . . . . H34B H 0.1066 0.6771 0.1779 0.094 Uiso 1 1 calc GR . . . . H34C H 0.2566 0.6084 0.1864 0.094 Uiso 1 1 calc GR . . . . C4 C 0.6927(5) 0.4654(4) 0.22505(19) 0.0277(11) Uani 1 1 d . . . . . C9 C 0.3849(5) 0.8807(5) 0.16091(19) 0.0314(11) Uani 1 1 d . . . . . C12 C 0.3633(5) 0.7291(4) 0.26509(19) 0.0290(11) Uani 1 1 d . . . . . C5 C 0.6757(5) 0.8748(4) 0.21658(19) 0.0285(11) Uani 1 1 d . . . . . N3 N 0.7034(5) 0.6091(5) -0.03085(17) 0.0408(12) Uani 1 1 d . . . . . C15 C 1.0227(6) 0.3917(5) 0.2469(2) 0.0440(14) Uani 1 1 d . . . . . H15A H 1.0717 0.4314 0.2588 0.053 Uiso 1 1 calc R . . . . H15B H 1.0515 0.3121 0.2652 0.053 Uiso 1 1 calc R . . . . C1 C 0.8332(5) 0.5814(5) 0.28976(19) 0.0288(11) Uani 1 1 d . . . . . C22 C 0.7984(7) 0.8975(6) 0.1311(2) 0.0576(18) Uani 1 1 d . . . . . H22A H 0.7419 0.8823 0.1102 0.086 Uiso 1 1 calc GR . . . . H22B H 0.8844 0.8661 0.1110 0.086 Uiso 1 1 calc GR . . . . H22C H 0.7624 0.9859 0.1375 0.086 Uiso 1 1 calc GR . . . . C8 C 0.4265(6) 0.9892(5) 0.3062(2) 0.0413(14) Uani 1 1 d D . . . . C24 C 0.7432(10) 1.0278(8) 0.3087(3) 0.085(3) Uani 1 1 d . . . . . H24A H 0.8087 0.9418 0.3100 0.128 Uiso 1 1 calc GR . . . . H24B H 0.6725 1.0444 0.3372 0.128 Uiso 1 1 calc GR . . . . H24C H 0.7820 1.0809 0.3140 0.128 Uiso 1 1 calc GR . . . . N4 N 0.8284(5) 0.3600(5) 0.01357(18) 0.0438(12) Uani 1 1 d . . . . . C20 C 0.6848(7) 0.3039(5) 0.1686(2) 0.0433(14) Uani 1 1 d . . . . . H20A H 0.6965 0.3457 0.1359 0.065 Uiso 1 1 calc GR . . . . H20B H 0.6315 0.2651 0.1623 0.065 Uiso 1 1 calc GR . . . . H20C H 0.7691 0.2411 0.1778 0.065 Uiso 1 1 calc GR . . . . C19 C 0.6181(5) 0.3967(5) 0.2149(2) 0.0339(12) Uani 1 1 d . . . . . H19A H 0.6089 0.3536 0.2480 0.041 Uiso 1 1 calc R . . . . H19B H 0.5305 0.4565 0.2065 0.041 Uiso 1 1 calc R . . . . C16 C 1.0540(6) 0.3689(6) 0.1864(2) 0.0596(19) Uani 1 1 d . . . . . H16A H 1.0253 0.4474 0.1679 0.089 Uiso 1 1 calc GR . . . . H16B H 1.0095 0.3257 0.1746 0.089 Uiso 1 1 calc GR . . . . H16C H 1.1473 0.3189 0.1777 0.089 Uiso 1 1 calc GR . . . . N1 N 0.4647(5) 0.7635(4) 0.51706(18) 0.0444(12) Uani 1 1 d . . . . . C33 C 0.1571(6) 0.7763(6) 0.2263(2) 0.0414(13) Uani 1 1 d . . . . . H33A H 0.0815 0.8558 0.2203 0.050 Uiso 1 1 calc R . . . . H33B H 0.1366 0.7428 0.2605 0.050 Uiso 1 1 calc R . . . . C23 C 0.6920(6) 1.0527(5) 0.2553(2) 0.0410(14) Uani 1 1 d . . . . . H23A H 0.7644 1.0313 0.2264 0.049 Uiso 1 1 calc R . . . . H23B H 0.6321 1.1412 0.2528 0.049 Uiso 1 1 calc R . . . . C11 C 0.2736(5) 0.7965(5) 0.23040(19) 0.0307(11) Uani 1 1 d . . . . . N2 N 0.7391(5) 0.5829(5) 0.5091(2) 0.0501(13) Uani 1 1 d . . . . . C35 C 0.3367(6) 0.6436(5) 0.3045(2) 0.0369(13) Uani 1 1 d . . . . . H35A H 0.4193 0.5775 0.3149 0.044 Uiso 1 1 calc R . . . . H35B H 0.2931 0.6053 0.2869 0.044 Uiso 1 1 calc R . . . . C3 C 0.7969(5) 0.4135(4) 0.25350(18) 0.0286(11) Uani 1 1 d . . . . . C21 C 0.8087(5) 0.8330(5) 0.1848(2) 0.0346(12) Uani 1 1 d . . . . . H21A H 0.8636 0.8506 0.2063 0.041 Uiso 1 1 calc R . . . . H21B H 0.8503 0.7434 0.1784 0.041 Uiso 1 1 calc R . . . . C2 C 0.8784(5) 0.4728(5) 0.26404(19) 0.0313(12) Uani 1 1 d . . . . . C6 C 0.6210(6) 0.9792(5) 0.2465(2) 0.0333(12) Uani 1 1 d . . . . . C31 C 0.1522(6) 1.0142(5) 0.1978(2) 0.0470(15) Uani 1 1 d . . . . . H31A H 0.0998 1.0147 0.2318 0.056 Uiso 1 1 calc R . . . . H31B H 0.1718 1.0835 0.1997 0.056 Uiso 1 1 calc R . . . . C17 C 0.8448(7) 0.2856(5) 0.2763(2) 0.0444(15) Uani 1 1 d . . . . . H17A H 0.9284 0.2303 0.2558 0.053 Uiso 1 1 calc R . . . . H17B H 0.7826 0.2554 0.2707 0.053 Uiso 1 1 calc R . . . . C18 C 0.8626(7) 0.2781(6) 0.3362(2) 0.0534(17) Uani 1 1 d . . . . . H18A H 0.9235 0.3083 0.3423 0.080 Uiso 1 1 calc GR . . . . H18B H 0.8965 0.1927 0.3477 0.080 Uiso 1 1 calc GR . . . . H18C H 0.7793 0.3284 0.3571 0.080 Uiso 1 1 calc GR . . . . C45 C 0.7706(8) 0.6835(7) -0.0344(3) 0.064(2) Uani 1 1 d . . . . . H45A H 0.7244 0.7536 -0.0094 0.097 Uiso 1 1 calc GR . . . . H45B H 0.7738 0.7131 -0.0713 0.097 Uiso 1 1 calc GR . . . . H45C H 0.8587 0.6337 -0.0250 0.097 Uiso 1 1 calc GR . . . . C41 C 0.8207(7) 0.6365(7) 0.5211(3) 0.063(2) Uani 1 1 d . . . . . H41A H 0.8828 0.6267 0.4896 0.095 Uiso 1 1 calc GR . . . . H41B H 0.8672 0.5950 0.5519 0.095 Uiso 1 1 calc GR . . . . H41C H 0.7667 0.7239 0.5297 0.095 Uiso 1 1 calc GR . . . . C32 C 0.0724(7) 1.0354(7) 0.1519(3) 0.073(2) Uani 1 1 d . . . . . H32A H 0.1217 1.0386 0.1180 0.109 Uiso 1 1 calc GR . . . . H32B H -0.0072 1.1131 0.1578 0.109 Uiso 1 1 calc GR . . . . H32C H 0.0509 0.9683 0.1499 0.109 Uiso 1 1 calc GR . . . . C47 C 0.7633(7) 0.2895(6) 0.0026(3) 0.0554(17) Uani 1 1 d . . . . . H47A H 0.7378 0.2602 0.0366 0.083 Uiso 1 1 calc GR . . . . H47B H 0.8219 0.2193 -0.0209 0.083 Uiso 1 1 calc GR . . . . H47C H 0.6863 0.3416 -0.0152 0.083 Uiso 1 1 calc GR . . . . C36 C 0.2509(7) 0.7154(6) 0.3550(2) 0.0513(16) Uani 1 1 d . . . . . H36A H 0.1725 0.7851 0.3443 0.077 Uiso 1 1 calc GR . . . . H36B H 0.2982 0.7454 0.3746 0.077 Uiso 1 1 calc GR . . . . H36C H 0.2274 0.6616 0.3782 0.077 Uiso 1 1 calc GR . . . . C13 C 0.9258(6) 0.6267(5) 0.3046(2) 0.0397(13) Uani 1 1 d . . . . . H13A H 0.9942 0.6089 0.2742 0.048 Uiso 1 1 calc R . . . . H13B H 0.8781 0.7167 0.3102 0.048 Uiso 1 1 calc R . . . . C39 C 0.3961(9) 0.8975(7) 0.5189(3) 0.083(3) Uani 1 1 d . . . . . H39A H 0.4582 0.9290 0.5198 0.125 Uiso 1 1 calc GR . . . . H39B H 0.3340 0.9255 0.5513 0.125 Uiso 1 1 calc GR . . . . H39C H 0.3503 0.9279 0.4869 0.125 Uiso 1 1 calc GR . . . . C44 C 0.7719(6) 0.4980(6) -0.0643(2) 0.0481(15) Uani 1 1 d . . . . . H44A H 0.8096 0.5169 -0.0986 0.058 Uiso 1 1 calc R . . . . H44B H 0.7099 0.4701 -0.0729 0.058 Uiso 1 1 calc R . . . . C14 C 0.9881(7) 0.5669(6) 0.3552(2) 0.0527(16) Uani 1 1 d . . . . . H14A H 1.0359 0.4779 0.3497 0.079 Uiso 1 1 calc GR . . . . H14B H 0.9209 0.5866 0.3856 0.079 Uiso 1 1 calc GR . . . . H14C H 1.0474 0.5978 0.3628 0.079 Uiso 1 1 calc GR . . . . C29 C 0.3811(6) 0.9858(5) 0.1246(2) 0.0431(14) Uani 1 1 d . U . . . H29A H 0.2914 1.0531 0.1269 0.052 Uiso 1 1 calc R . . . . H29B H 0.4352 1.0180 0.1382 0.052 Uiso 1 1 calc R . . . . C10 C 0.2795(5) 0.8944(5) 0.19398(19) 0.0302(11) Uani 1 1 d . . . . . C46 C 0.5755(7) 0.6858(6) -0.0485(3) 0.0575(18) Uani 1 1 d . . . . . H46A H 0.5250 0.6411 -0.0441 0.086 Uiso 1 1 calc GR . . . . H46B H 0.5850 0.7061 -0.0865 0.086 Uiso 1 1 calc GR . . . . H46C H 0.5310 0.7614 -0.0267 0.086 Uiso 1 1 calc GR . . . . C7 C 0.4815(6) 1.0406(5) 0.2712(2) 0.0412(14) Uani 1 1 d . . . . . C38 C 0.5390(8) 0.7168(8) 0.5639(3) 0.069(2) Uani 1 1 d . . . . . H38A H 0.4799 0.7177 0.5956 0.082 Uiso 1 1 calc R . . . . H38B H 0.5736 0.7728 0.5719 0.082 Uiso 1 1 calc R . . . . C40 C 0.3732(6) 0.7153(6) 0.5164(2) 0.0502(16) Uani 1 1 d . . . . . H40A H 0.3345 0.7364 0.4824 0.075 Uiso 1 1 calc GR . . . . H40B H 0.3053 0.7511 0.5465 0.075 Uiso 1 1 calc GR . . . . H40C H 0.4185 0.6260 0.5198 0.075 Uiso 1 1 calc GR . . . . C25 C 0.4027(7) 1.1724(6) 0.2487(3) 0.0619(19) Uani 1 1 d . . . . . H25A H 0.4529 1.1818 0.2160 0.074 Uiso 1 1 calc R . . . . H25B H 0.3213 1.1798 0.2379 0.074 Uiso 1 1 calc R . . . . C26 C 0.3705(9) 1.2745(7) 0.2870(3) 0.081(2) Uani 1 1 d . . . . . H26A H 0.3272 1.3530 0.2689 0.122 Uiso 1 1 calc GR . . . . H26B H 0.4499 1.2663 0.2994 0.122 Uiso 1 1 calc GR . . . . H26C H 0.3131 1.2715 0.3180 0.122 Uiso 1 1 calc GR . . . . C42 C 0.8189(7) 0.4567(7) 0.4925(3) 0.066(2) Uani 1 1 d . . . . . H42A H 0.7646 0.4229 0.4816 0.099 Uiso 1 1 calc GR . . . . H42B H 0.8649 0.4096 0.5225 0.099 Uiso 1 1 calc GR . . . . H42C H 0.8815 0.4518 0.4620 0.099 Uiso 1 1 calc GR . . . . C43 C 0.8778(7) 0.3964(7) -0.0368(2) 0.0568(17) Uani 1 1 d . . . . . H43A H 0.9237 0.3245 -0.0615 0.068 Uiso 1 1 calc R . . . . H43B H 0.9408 0.4237 -0.0289 0.068 Uiso 1 1 calc R . . . . C48 C 0.9357(7) 0.2840(7) 0.0450(3) 0.0642(19) Uani 1 1 d . . . . . H48A H 0.9761 0.3325 0.0553 0.096 Uiso 1 1 calc GR . . . . H48B H 0.9998 0.2130 0.0232 0.096 Uiso 1 1 calc GR . . . . H48C H 0.9030 0.2559 0.0775 0.096 Uiso 1 1 calc GR . . . . C37 C 0.6482(8) 0.5901(8) 0.5556(3) 0.068(2) Uani 1 1 d . . . . . H37A H 0.6941 0.5650 0.5883 0.081 Uiso 1 1 calc R . . . . H37B H 0.6138 0.5326 0.5501 0.081 Uiso 1 1 calc R . . . . C27 C 0.2811(7) 1.0604(6) 0.3280(3) 0.0568(17) Uani 1 1 d D U . . . H27A H 0.2410 1.1405 0.3100 0.068 Uiso 1 1 calc R . . . . H27B H 0.2367 1.0134 0.3194 0.068 Uiso 1 1 calc R . . . . C30 C 0.4278(11) 0.9469(8) 0.0672(3) 0.098(3) Uani 1 1 d . U . . . H30A H 0.4309 1.0149 0.0465 0.148 Uiso 1 1 calc GR . . . . H30B H 0.3689 0.9237 0.0523 0.148 Uiso 1 1 calc GR . . . . H30C H 0.5144 0.8766 0.0649 0.148 Uiso 1 1 calc GR . . . . C28 C 0.2650(11) 1.0798(12) 0.3858(4) 0.127(4) Uani 1 1 d . U . . . H28A H 0.3157 1.0019 0.4031 0.191 Uiso 1 1 calc GR . . . . H28B H 0.1737 1.1122 0.3994 0.191 Uiso 1 1 calc GR . . . . H28C H 0.2949 1.1386 0.3938 0.191 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 Cu7 0.0203(3) 0.0206(3) 0.0319(3) 0.0009(2) -0.0008(2) -0.0088(3) Cu9 0.0230(4) 0.0293(3) 0.0305(3) 0.0038(2) -0.0001(2) -0.0129(3) Cu4 0.0244(4) 0.0238(3) 0.0335(3) 0.0058(2) -0.0045(3) -0.0123(3) Cu6 0.0249(4) 0.0259(3) 0.0339(3) 0.0072(2) -0.0047(3) -0.0122(3) Cu5 0.0270(4) 0.0250(3) 0.0370(3) -0.0027(2) 0.0038(3) -0.0131(3) Cu2 0.0321(4) 0.0298(3) 0.0302(3) 0.0020(2) 0.0005(3) -0.0182(3) Cu8 0.0265(4) 0.0294(3) 0.0349(3) 0.0013(3) -0.0035(3) -0.0118(3) Cu3 0.0497(5) 0.0432(4) 0.0382(4) -0.0071(3) 0.0050(3) -0.0311(4) Cu1 0.0475(5) 0.0446(4) 0.0423(4) 0.0033(3) -0.0057(3) -0.0280(4) Cu10 0.0412(5) 0.0533(5) 0.0448(4) 0.0075(3) -0.0015(3) -0.0265(4) Cl1 0.0470(9) 0.0468(8) 0.0306(6) 0.0028(5) 0.0001(6) -0.0322(7) Cl4 0.0420(9) 0.0574(9) 0.0301(6) 0.0029(6) 0.0010(6) -0.0322(8) Cl3 0.0338(8) 0.0443(8) 0.0395(7) -0.0063(6) -0.0014(6) -0.0213(7) Cl2 0.0746(12) 0.0495(9) 0.0402(7) 0.0020(6) -0.0043(7) -0.0431(9) C34 0.040(4) 0.082(5) 0.078(5) -0.023(4) 0.002(3) -0.040(4) C4 0.026(3) 0.020(2) 0.035(3) 0.0014(19) 0.002(2) -0.011(2) C9 0.026(3) 0.026(3) 0.036(3) 0.006(2) -0.008(2) -0.007(2) C12 0.028(3) 0.026(3) 0.033(3) 0.000(2) 0.000(2) -0.013(2) C5 0.023(3) 0.024(3) 0.040(3) 0.007(2) -0.002(2) -0.012(2) N3 0.044(3) 0.055(3) 0.035(2) 0.009(2) -0.008(2) -0.032(3) C15 0.025(3) 0.043(3) 0.047(3) 0.003(3) -0.002(3) -0.003(3) C1 0.023(3) 0.032(3) 0.033(3) 0.008(2) -0.006(2) -0.014(2) C22 0.059(5) 0.060(4) 0.054(4) 0.005(3) 0.014(3) -0.033(4) C8 0.040(4) 0.028(3) 0.054(3) -0.008(2) 0.011(3) -0.017(3) C24 0.142(9) 0.091(6) 0.083(5) 0.027(4) -0.045(5) -0.100(7) N4 0.026(3) 0.050(3) 0.048(3) 0.000(2) -0.002(2) -0.013(2) C20 0.055(4) 0.037(3) 0.043(3) 0.000(2) -0.008(3) -0.025(3) C19 0.032(3) 0.022(3) 0.048(3) -0.001(2) 0.000(2) -0.013(2) C16 0.034(4) 0.068(5) 0.043(3) 0.014(3) 0.006(3) 0.000(3) N1 0.053(4) 0.045(3) 0.043(3) -0.001(2) 0.000(2) -0.031(3) C33 0.023(3) 0.053(4) 0.046(3) -0.002(3) -0.001(2) -0.017(3) C23 0.044(4) 0.030(3) 0.058(3) 0.002(2) -0.001(3) -0.026(3) C11 0.021(3) 0.033(3) 0.035(3) -0.004(2) 0.000(2) -0.010(2) N2 0.046(3) 0.063(4) 0.053(3) 0.018(3) -0.016(3) -0.034(3) C35 0.033(3) 0.037(3) 0.045(3) 0.007(2) -0.001(2) -0.021(3) C3 0.026(3) 0.022(2) 0.029(2) -0.0013(19) 0.003(2) -0.005(2) C21 0.027(3) 0.031(3) 0.052(3) 0.001(2) 0.000(2) -0.019(2) C2 0.024(3) 0.033(3) 0.029(3) 0.005(2) 0.000(2) -0.008(2) C6 0.035(3) 0.025(3) 0.042(3) 0.006(2) 0.000(2) -0.017(2) C31 0.034(4) 0.036(3) 0.048(3) 0.002(3) -0.005(3) 0.003(3) C17 0.056(4) 0.026(3) 0.045(3) 0.006(2) -0.013(3) -0.013(3) C18 0.074(5) 0.038(3) 0.048(3) 0.015(3) -0.015(3) -0.025(4) C45 0.087(6) 0.088(6) 0.055(4) 0.023(4) -0.020(4) -0.070(5) C41 0.055(5) 0.086(5) 0.066(4) 0.013(4) -0.025(4) -0.045(5) C32 0.038(4) 0.076(5) 0.074(5) 0.018(4) -0.018(4) 0.000(4) C47 0.053(5) 0.058(4) 0.060(4) -0.005(3) -0.009(3) -0.028(4) C36 0.048(4) 0.058(4) 0.045(3) 0.012(3) 0.006(3) -0.025(3) C13 0.034(3) 0.049(4) 0.043(3) 0.007(3) -0.006(3) -0.025(3) C39 0.106(8) 0.044(4) 0.087(5) -0.014(4) 0.034(5) -0.032(5) C44 0.044(4) 0.066(4) 0.036(3) 0.003(3) 0.002(3) -0.028(4) C14 0.046(4) 0.064(4) 0.053(4) 0.004(3) -0.018(3) -0.027(4) C29 0.039(4) 0.036(3) 0.046(3) 0.012(2) -0.010(3) -0.010(3) C10 0.024(3) 0.030(3) 0.030(3) -0.001(2) -0.007(2) -0.006(2) C46 0.066(5) 0.055(4) 0.052(4) 0.003(3) -0.012(3) -0.028(4) C7 0.039(4) 0.022(3) 0.062(4) -0.002(2) 0.002(3) -0.015(3) C38 0.079(6) 0.102(6) 0.042(4) -0.007(4) 0.003(4) -0.057(6) C40 0.042(4) 0.052(4) 0.051(4) 0.000(3) 0.004(3) -0.020(3) C25 0.040(4) 0.032(3) 0.104(5) -0.001(3) -0.003(4) -0.010(3) C26 0.072(6) 0.049(5) 0.113(7) -0.003(4) 0.000(5) -0.022(4) C42 0.048(5) 0.061(5) 0.094(5) 0.023(4) -0.022(4) -0.029(4) C43 0.044(4) 0.076(5) 0.049(4) 0.001(3) 0.001(3) -0.028(4) C48 0.032(4) 0.074(5) 0.073(5) 0.006(4) -0.011(3) -0.013(4) C37 0.061(5) 0.096(6) 0.053(4) 0.025(4) -0.014(4) -0.042(5) C27 0.056(5) 0.029(3) 0.079(3) -0.010(3) 0.006(4) -0.017(3) C30 0.136(7) 0.065(5) 0.061(4) 0.022(4) 0.015(4) -0.026(5) C28 0.099(7) 0.166(8) 0.083(4) -0.031(5) 0.000(5) -0.034(6) _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 Cu7 Cu9 2.4040(8) . ? Cu7 Cu4 2.5244(8) . ? Cu7 Cu6 2.5705(8) . ? Cu7 Cu5 2.3990(8) . ? Cu7 Cu2 2.9846(8) . ? Cu7 Cu8 2.7710(8) . ? Cu7 C4 2.001(5) . ? Cu7 C12 2.004(5) . ? Cu9 Cu4 3.0508(8) . ? Cu9 Cu6 2.9085(9) . ? Cu9 Cu8 2.7504(9) . ? Cu9 Cu10 3.0013(9) . ? Cu9 Cl4 2.1586(13) . ? Cu9 C4 1.995(4) . ? Cu4 Cu6 2.4178(8) . ? Cu4 Cu5 2.5605(9) . ? Cu4 Cu2 2.3995(7) . ? Cu4 Cu3 2.7900(9) . ? Cu4 C5 2.020(4) . ? Cu4 C1 2.004(5) . ? Cu6 Cu5 2.6727(8) . ? Cu6 Cu8 2.4562(9) . ? Cu6 C9 1.996(5) . ? Cu6 C5 2.003(5) . ? Cu5 Cu3 2.4306(9) . ? Cu5 C12 1.997(5) . ? Cu5 C8 1.998(5) . ? Cu2 Cu3 2.8649(9) . ? Cu2 Cu1 2.8714(9) . ? Cu2 Cl1 2.1634(13) . ? Cu2 C1 1.989(5) . ? Cu8 Cl3 2.1604(14) . ? Cu8 C9 1.966(5) . ? Cu3 Cl2 2.1621(17) . ? Cu3 C8 2.006(6) . ? Cu1 Cl1 2.2918(14) . ? Cu1 Cl2 2.2737(15) . ? Cu1 N1 2.169(5) . ? Cu1 N2 2.191(5) . ? Cu10 Cl4 2.3309(15) . ? Cu10 Cl3 2.2570(15) . ? Cu10 N3 2.168(4) . ? Cu10 N4 2.182(5) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C34 C33 1.528(8) . ? C4 C19 1.527(7) . ? C4 C3 1.362(7) . ? C9 C29 1.539(7) . ? C9 C10 1.354(7) . ? C12 C11 1.376(7) . ? C12 C35 1.529(7) . ? C5 C21 1.531(7) . ? C5 C6 1.352(7) . ? N3 C45 1.465(7) . ? N3 C44 1.460(8) . ? N3 C46 1.466(8) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C15 C16 1.519(8) . ? C15 C2 1.534(8) . ? C1 C2 1.349(7) . ? C1 C13 1.526(7) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C22 C21 1.520(8) . ? C8 C7 1.341(7) . ? C8 C27 1.556(8) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C24 C23 1.491(9) . ? N4 C47 1.456(8) . ? N4 C43 1.468(7) . ? N4 C48 1.469(8) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C20 C19 1.525(7) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? N1 C39 1.463(9) . ? N1 C38 1.476(9) . ? N1 C40 1.459(8) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C33 C11 1.523(7) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 C6 1.532(7) . ? C11 C10 1.507(7) . ? N2 C41 1.462(8) . ? N2 C42 1.440(9) . ? N2 C37 1.463(8) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C35 C36 1.536(8) . ? C3 C2 1.507(7) . ? C3 C17 1.518(7) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C6 C7 1.516(8) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C31 C32 1.505(9) . ? C31 C10 1.533(7) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C17 C18 1.530(8) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 C14 1.522(8) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C44 C43 1.506(9) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C29 C30 1.491(9) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C7 C25 1.567(8) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C38 C37 1.493(11) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C25 C26 1.489(10) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C27 C28 1.450(11) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? 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 Cu9 Cu7 Cu4 76.45(3) . . ? Cu9 Cu7 Cu6 71.47(2) . . ? Cu9 Cu7 Cu2 105.05(3) . . ? Cu9 Cu7 Cu8 63.75(2) . . ? Cu4 Cu7 Cu6 56.65(2) . . ? Cu4 Cu7 Cu2 50.806(19) . . ? Cu4 Cu7 Cu8 107.72(3) . . ? Cu6 Cu7 Cu2 105.28(3) . . ? Cu6 Cu7 Cu8 54.60(2) . . ? Cu5 Cu7 Cu9 131.54(3) . . ? Cu5 Cu7 Cu4 62.61(2) . . ? Cu5 Cu7 Cu6 64.96(2) . . ? Cu5 Cu7 Cu2 68.70(2) . . ? Cu5 Cu7 Cu8 104.03(3) . . ? Cu8 Cu7 Cu2 158.51(3) . . ? C4 Cu7 Cu9 52.91(13) . . ? C4 Cu7 Cu4 97.07(15) . . ? C4 Cu7 Cu6 123.41(13) . . ? C4 Cu7 Cu5 150.64(15) . . ? C4 Cu7 Cu2 82.06(14) . . ? C4 Cu7 Cu8 102.32(14) . . ? C4 Cu7 C12 140.60(19) . . ? C12 Cu7 Cu9 152.35(14) . . ? C12 Cu7 Cu4 115.64(14) . . ? C12 Cu7 Cu6 93.90(13) . . ? C12 Cu7 Cu5 53.03(14) . . ? C12 Cu7 Cu2 101.37(14) . . ? C12 Cu7 Cu8 88.61(14) . . ? Cu7 Cu9 Cu4 53.55(2) . . ? Cu7 Cu9 Cu6 56.93(2) . . ? Cu7 Cu9 Cu8 64.63(2) . . ? Cu7 Cu9 Cu10 125.06(3) . . ? Cu6 Cu9 Cu4 47.799(18) . . ? Cu6 Cu9 Cu10 102.87(3) . . ? Cu8 Cu9 Cu4 94.91(3) . . ? Cu8 Cu9 Cu6 51.36(2) . . ? Cu8 Cu9 Cu10 64.38(2) . . ? Cu10 Cu9 Cu4 148.82(3) . . ? Cl4 Cu9 Cu7 150.46(5) . . ? Cl4 Cu9 Cu4 112.81(4) . . ? Cl4 Cu9 Cu6 94.05(5) . . ? Cl4 Cu9 Cu8 93.92(5) . . ? Cl4 Cu9 Cu10 50.54(4) . . ? C4 Cu9 Cu7 53.13(14) . . ? C4 Cu9 Cu4 82.13(14) . . ? C4 Cu9 Cu6 109.30(14) . . ? C4 Cu9 Cu8 103.19(15) . . ? C4 Cu9 Cu10 123.69(14) . . ? C4 Cu9 Cl4 156.40(15) . . ? Cu7 Cu4 Cu9 50.00(2) . . ? Cu7 Cu4 Cu5 56.30(2) . . ? Cu7 Cu4 Cu3 104.99(3) . . ? Cu6 Cu4 Cu7 62.64(2) . . ? Cu6 Cu4 Cu9 63.02(2) . . ? Cu6 Cu4 Cu5 64.87(3) . . ? Cu6 Cu4 Cu3 106.24(3) . . ? Cu5 Cu4 Cu9 102.27(3) . . ? Cu5 Cu4 Cu3 53.83(2) . . ? Cu2 Cu4 Cu7 74.57(2) . . ? Cu2 Cu4 Cu9 103.22(3) . . ? Cu2 Cu4 Cu6 133.28(3) . . ? Cu2 Cu4 Cu5 76.58(3) . . ? Cu2 Cu4 Cu3 66.52(2) . . ? Cu3 Cu4 Cu9 154.88(3) . . ? C5 Cu4 Cu7 115.37(15) . . ? C5 Cu4 Cu9 96.04(14) . . ? C5 Cu4 Cu6 52.74(15) . . ? C5 Cu4 Cu5 94.30(15) . . ? C5 Cu4 Cu2 160.01(15) . . ? C5 Cu4 Cu3 93.68(15) . . ? C1 Cu4 Cu7 99.53(14) . . ? C1 Cu4 Cu9 85.50(14) . . ? C1 Cu4 Cu6 148.44(15) . . ? C1 Cu4 Cu5 128.98(14) . . ? C1 Cu4 Cu2 52.77(14) . . ? C1 Cu4 Cu3 103.47(14) . . ? C1 Cu4 C5 135.5(2) . . ? Cu7 Cu6 Cu9 51.60(2) . . ? Cu7 Cu6 Cu5 54.41(2) . . ? Cu4 Cu6 Cu7 60.71(2) . . ? Cu4 Cu6 Cu9 69.18(2) . . ? Cu4 Cu6 Cu5 60.15(2) . . ? Cu4 Cu6 Cu8 122.78(3) . . ? Cu5 Cu6 Cu9 103.31(2) . . ? Cu8 Cu6 Cu7 66.86(2) . . ? Cu8 Cu6 Cu9 61.00(2) . . ? Cu8 Cu6 Cu5 105.37(3) . . ? C9 Cu6 Cu7 94.73(14) . . ? C9 Cu6 Cu9 111.98(15) . . ? C9 Cu6 Cu4 148.93(14) . . ? C9 Cu6 Cu5 90.62(14) . . ? C9 Cu6 Cu8 51.15(15) . . ? C9 Cu6 C5 145.6(2) . . ? C5 Cu6 Cu7 114.10(13) . . ? C5 Cu6 Cu9 100.96(15) . . ? C5 Cu6 Cu4 53.39(13) . . ? C5 Cu6 Cu5 91.38(14) . . ? C5 Cu6 Cu8 157.46(15) . . ? Cu7 Cu5 Cu4 61.09(2) . . ? Cu7 Cu5 Cu6 60.62(2) . . ? Cu7 Cu5 Cu3 121.75(4) . . ? Cu4 Cu5 Cu6 54.98(2) . . ? Cu3 Cu5 Cu4 67.91(3) . . ? Cu3 Cu5 Cu6 109.56(3) . . ? C12 Cu5 Cu7 53.28(15) . . ? C12 Cu5 Cu4 114.37(15) . . ? C12 Cu5 Cu6 91.02(14) . . ? C12 Cu5 Cu3 152.90(14) . . ? C12 Cu5 C8 146.8(2) . . ? C8 Cu5 Cu7 150.25(16) . . ? C8 Cu5 Cu4 94.26(17) . . ? C8 Cu5 Cu6 92.23(16) . . ? C8 Cu5 Cu3 52.78(18) . . ? Cu4 Cu2 Cu7 54.62(2) . . ? Cu4 Cu2 Cu3 63.28(2) . . ? Cu4 Cu2 Cu1 126.84(3) . . ? Cu3 Cu2 Cu7 92.30(2) . . ? Cu3 Cu2 Cu1 65.58(2) . . ? Cu1 Cu2 Cu7 141.21(3) . . ? Cl1 Cu2 Cu7 106.86(4) . . ? Cl1 Cu2 Cu4 151.81(5) . . ? Cl1 Cu2 Cu3 100.39(5) . . ? Cl1 Cu2 Cu1 51.86(4) . . ? C1 Cu2 Cu7 86.13(14) . . ? C1 Cu2 Cu4 53.34(14) . . ? C1 Cu2 Cu3 101.33(14) . . ? C1 Cu2 Cu1 127.75(15) . . ? C1 Cu2 Cl1 154.14(15) . . ? Cu9 Cu8 Cu7 51.62(2) . . ? Cu6 Cu8 Cu7 58.54(2) . . ? Cu6 Cu8 Cu9 67.65(2) . . ? Cl3 Cu8 Cu7 112.03(4) . . ? Cl3 Cu8 Cu9 89.64(5) . . ? Cl3 Cu8 Cu6 156.62(5) . . ? C9 Cu8 Cu7 89.44(14) . . ? C9 Cu8 Cu9 119.70(15) . . ? C9 Cu8 Cu6 52.24(15) . . ? C9 Cu8 Cl3 150.63(16) . . ? Cu4 Cu3 Cu2 50.195(19) . . ? Cu5 Cu3 Cu4 58.26(2) . . ? Cu5 Cu3 Cu2 70.48(2) . . ? Cl2 Cu3 Cu4 111.60(6) . . ? Cl2 Cu3 Cu5 153.87(5) . . ? Cl2 Cu3 Cu2 84.73(5) . . ? C8 Cu3 Cu4 87.43(16) . . ? C8 Cu3 Cu5 52.46(15) . . ? C8 Cu3 Cu2 121.96(15) . . ? C8 Cu3 Cl2 153.23(16) . . ? Cl1 Cu1 Cu2 47.94(3) . . ? Cl2 Cu1 Cu2 82.65(4) . . ? Cl2 Cu1 Cl1 129.03(5) . . ? N1 Cu1 Cu2 147.04(14) . . ? N1 Cu1 Cl1 106.24(13) . . ? N1 Cu1 Cl2 112.50(13) . . ? N1 Cu1 N2 84.7(2) . . ? N2 Cu1 Cu2 120.04(16) . . ? N2 Cu1 Cl1 108.44(15) . . ? N2 Cu1 Cl2 106.95(14) . . ? Cl4 Cu10 Cu9 45.65(3) . . ? Cl3 Cu10 Cu9 81.75(4) . . ? Cl3 Cu10 Cl4 123.73(6) . . ? N3 Cu10 Cu9 147.09(13) . . ? N3 Cu10 Cl4 105.45(13) . . ? N3 Cu10 Cl3 114.64(14) . . ? N3 Cu10 N4 85.52(18) . . ? N4 Cu10 Cu9 115.08(13) . . ? N4 Cu10 Cl4 107.21(14) . . ? N4 Cu10 Cl3 113.50(14) . . ? Cu2 Cl1 Cu1 80.20(5) . . ? Cu9 Cl4 Cu10 83.81(5) . . ? Cu8 Cl3 Cu10 88.08(5) . . ? Cu3 Cl2 Cu1 88.86(6) . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? Cu9 C4 Cu7 73.96(16) . . ? C19 C4 Cu7 101.9(3) . . ? C19 C4 Cu9 119.5(3) . . ? C3 C4 Cu7 123.6(4) . . ? C3 C4 Cu9 108.5(4) . . ? C3 C4 C19 121.0(4) . . ? Cu8 C9 Cu6 76.61(19) . . ? C29 C9 Cu6 100.7(4) . . ? C29 C9 Cu8 119.8(4) . . ? C10 C9 Cu6 120.6(4) . . ? C10 C9 Cu8 110.1(4) . . ? C10 C9 C29 120.9(5) . . ? Cu5 C12 Cu7 73.69(18) . . ? C11 C12 Cu7 120.2(4) . . ? C11 C12 Cu5 111.0(3) . . ? C11 C12 C35 118.9(5) . . ? C35 C12 Cu7 105.9(3) . . ? C35 C12 Cu5 119.2(4) . . ? Cu6 C5 Cu4 73.87(16) . . ? C21 C5 Cu4 105.8(3) . . ? C21 C5 Cu6 118.4(4) . . ? C6 C5 Cu4 111.5(3) . . ? C6 C5 Cu6 116.4(4) . . ? C6 C5 C21 119.8(4) . . ? C45 N3 Cu10 109.6(3) . . ? C45 N3 C46 107.1(5) . . ? C44 N3 Cu10 103.6(3) . . ? C44 N3 C45 112.5(5) . . ? C44 N3 C46 109.8(5) . . ? C46 N3 Cu10 114.4(4) . . ? H15A C15 H15B 107.8 . . ? C16 C15 H15A 109.0 . . ? C16 C15 H15B 109.0 . . ? C16 C15 C2 113.0(5) . . ? C2 C15 H15A 109.0 . . ? C2 C15 H15B 109.0 . . ? Cu2 C1 Cu4 73.89(18) . . ? C2 C1 Cu4 119.0(4) . . ? C2 C1 Cu2 109.2(4) . . ? C2 C1 C13 120.6(5) . . ? C13 C1 Cu4 104.2(3) . . ? C13 C1 Cu2 121.2(4) . . ? H22A C22 H22B 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? Cu5 C8 Cu3 74.76(19) . . ? C7 C8 Cu5 119.7(4) . . ? C7 C8 Cu3 109.9(5) . . ? C7 C8 C27 121.0(5) . . ? C27 C8 Cu5 101.9(4) . . ? C27 C8 Cu3 120.7(4) . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? C47 N4 Cu10 114.0(4) . . ? C47 N4 C43 110.9(5) . . ? C47 N4 C48 108.5(5) . . ? C43 N4 Cu10 100.1(4) . . ? C43 N4 C48 109.8(5) . . ? C48 N4 Cu10 113.3(4) . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? C4 C19 H19A 109.1 . . ? C4 C19 H19B 109.1 . . ? C20 C19 C4 112.3(4) . . ? C20 C19 H19A 109.1 . . ? C20 C19 H19B 109.1 . . ? H19A C19 H19B 107.9 . . ? 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 . . ? C39 N1 Cu1 112.4(4) . . ? C39 N1 C38 110.0(6) . . ? C38 N1 Cu1 103.3(4) . . ? C40 N1 Cu1 110.6(4) . . ? C40 N1 C39 110.1(6) . . ? C40 N1 C38 110.4(5) . . ? C34 C33 H33A 109.4 . . ? C34 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? C11 C33 C34 111.1(5) . . ? C11 C33 H33A 109.4 . . ? C11 C33 H33B 109.4 . . ? C24 C23 H23A 109.2 . . ? C24 C23 H23B 109.2 . . ? C24 C23 C6 111.8(4) . . ? H23A C23 H23B 107.9 . . ? C6 C23 H23A 109.2 . . ? C6 C23 H23B 109.2 . . ? C12 C11 C33 121.1(5) . . ? C12 C11 C10 124.7(5) . . ? C10 C11 C33 114.2(4) . . ? C41 N2 Cu1 110.1(4) . . ? C41 N2 C37 111.7(5) . . ? C42 N2 Cu1 112.7(4) . . ? C42 N2 C41 109.6(6) . . ? C42 N2 C37 109.6(5) . . ? C37 N2 Cu1 103.0(4) . . ? C12 C35 H35A 109.6 . . ? C12 C35 H35B 109.6 . . ? C12 C35 C36 110.2(4) . . ? H35A C35 H35B 108.1 . . ? C36 C35 H35A 109.6 . . ? C36 C35 H35B 109.6 . . ? C4 C3 C2 124.6(4) . . ? C4 C3 C17 122.1(5) . . ? C2 C3 C17 113.3(5) . . ? C5 C21 H21A 109.3 . . ? C5 C21 H21B 109.3 . . ? C22 C21 C5 111.4(5) . . ? C22 C21 H21A 109.3 . . ? C22 C21 H21B 109.3 . . ? H21A C21 H21B 108.0 . . ? C1 C2 C15 122.2(5) . . ? C1 C2 C3 124.5(5) . . ? C3 C2 C15 113.0(4) . . ? C5 C6 C23 122.8(5) . . ? C5 C6 C7 124.0(5) . . ? C7 C6 C23 113.1(4) . . ? H31A C31 H31B 107.5 . . ? C32 C31 H31A 108.5 . . ? C32 C31 H31B 108.5 . . ? C32 C31 C10 115.1(5) . . ? C10 C31 H31A 108.5 . . ? C10 C31 H31B 108.5 . . ? C3 C17 H17A 108.7 . . ? C3 C17 H17B 108.7 . . ? C3 C17 C18 114.1(5) . . ? H17A C17 H17B 107.6 . . ? C18 C17 H17A 108.7 . . ? C18 C17 H17B 108.7 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N3 C45 H45A 109.5 . . ? N3 C45 H45B 109.5 . . ? N3 C45 H45C 109.5 . . ? H45A C45 H45B 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N2 C41 H41A 109.5 . . ? N2 C41 H41B 109.5 . . ? N2 C41 H41C 109.5 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32B 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N4 C47 H47A 109.5 . . ? N4 C47 H47B 109.5 . . ? N4 C47 H47C 109.5 . . ? H47A C47 H47B 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C1 C13 H13A 109.1 . . ? C1 C13 H13B 109.1 . . ? H13A C13 H13B 107.9 . . ? C14 C13 C1 112.3(4) . . ? C14 C13 H13A 109.1 . . ? C14 C13 H13B 109.1 . . ? N1 C39 H39A 109.5 . . ? N1 C39 H39B 109.5 . . ? N1 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N3 C44 H44A 109.2 . . ? N3 C44 H44B 109.2 . . ? N3 C44 C43 112.1(5) . . ? H44A C44 H44B 107.9 . . ? C43 C44 H44A 109.2 . . ? C43 C44 H44B 109.2 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C29 H29A 109.0 . . ? C9 C29 H29B 109.0 . . ? H29A C29 H29B 107.8 . . ? C30 C29 C9 112.8(5) . . ? C30 C29 H29A 109.0 . . ? C30 C29 H29B 109.0 . . ? C9 C10 C11 124.7(5) . . ? C9 C10 C31 122.3(5) . . ? C11 C10 C31 113.0(5) . . ? N3 C46 H46A 109.5 . . ? N3 C46 H46B 109.5 . . ? N3 C46 H46C 109.5 . . ? H46A C46 H46B 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C8 C7 C6 125.6(5) . . ? C8 C7 C25 122.2(6) . . ? C6 C7 C25 112.1(5) . . ? N1 C38 H38A 108.8 . . ? N1 C38 H38B 108.8 . . ? N1 C38 C37 113.6(6) . . ? H38A C38 H38B 107.7 . . ? C37 C38 H38A 108.8 . . ? C37 C38 H38B 108.8 . . ? N1 C40 H40A 109.5 . . ? N1 C40 H40B 109.5 . . ? N1 C40 H40C 109.5 . . ? H40A C40 H40B 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C7 C25 H25A 108.5 . . ? C7 C25 H25B 108.5 . . ? H25A C25 H25B 107.5 . . ? C26 C25 C7 115.0(6) . . ? C26 C25 H25A 108.5 . . ? C26 C25 H25B 108.5 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N2 C42 H42A 109.5 . . ? N2 C42 H42B 109.5 . . ? N2 C42 H42C 109.5 . . ? H42A C42 H42B 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N4 C43 C44 112.3(5) . . ? N4 C43 H43A 109.1 . . ? N4 C43 H43B 109.1 . . ? C44 C43 H43A 109.1 . . ? C44 C43 H43B 109.1 . . ? H43A C43 H43B 107.9 . . ? N4 C48 H48A 109.5 . . ? N4 C48 H48B 109.5 . . ? N4 C48 H48C 109.5 . . ? H48A C48 H48B 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N2 C37 C38 111.4(6) . . ? N2 C37 H37A 109.3 . . ? N2 C37 H37B 109.3 . . ? C38 C37 H37A 109.3 . . ? C38 C37 H37B 109.3 . . ? H37A C37 H37B 108.0 . . ? C8 C27 H27A 109.4 . . ? C8 C27 H27B 109.4 . . ? H27A C27 H27B 108.0 . . ? C28 C27 C8 111.0(7) . . ? C28 C27 H27A 109.4 . . ? C28 C27 H27B 109.4 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? 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 . . ? _olex2_submission_special_instructions 'No special instructions were received' # SQUEEZE RESULTS (APPEND TO CIF) # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 89 4 ' ' 2 0.000 0.000 0.500 191 19 ' ' 3 0.383 0.383 0.175 8 0 ' ' 4 0.617 0.617 0.825 8 0 ' ' _platon_squeeze_details ; ;