# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Tian, Yu-Peng' 'Zhang, Xun-Jun' 'Fun, Hoong-Kun' 'Xu, Zhi-Qiang' 'Usman, Anwar' 'Chantrapomma, Suchada' 'Thompson, Laurence K.' 'Li, Sheng-Li' 'Ma, Wen' 'Zhang, Ming-Liang' 'Jiang, Min-Hua' _publ_contact_author_name 'Dr Yu-Peng Tian' _publ_contact_author_address ; Nanjing University State Key Lab.of Coordination Chemistry 22 Hankou Road Nanjing Jiangsu 210093 CHINA ; _publ_contact_author_email '?' _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Structural Diversity and Properties of a Series of Dinuclear and Mononuclear Copper (II) and Copper (I) Carboxylato Complexes ; data_tian23m _database_code_CSD 181844 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H72 Cu2 N8 O12' _chemical_formula_weight 1320.42 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.15160(10) _cell_length_b 13.3088(2) _cell_length_c 24.2596(2) _cell_angle_alpha 90.00 _cell_angle_beta 96.1080(10) _cell_angle_gamma 90.00 _cell_volume 3259.00(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.69 _cell_measurement_theta_max 28.34 _exptl_crystal_description slab _exptl_crystal_colour red _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.34 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.346 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1380 _exptl_absorpt_coefficient_mu 0.720 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7330 _exptl_absorpt_correction_T_max 0.7918 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Siemens SMART CCD area detector diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% negligible _diffrn_reflns_number 22293 _diffrn_reflns_av_R_equivalents 0.0765 _diffrn_reflns_av_sigmaI/netI 0.0898 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 28.20 _reflns_number_total 7875 _reflns_number_gt 4472 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 1997)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material ; SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990) ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1044P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0040(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7875 _refine_ls_number_parameters 417 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1138 _refine_ls_R_factor_gt 0.0638 _refine_ls_wR_factor_ref 0.1930 _refine_ls_wR_factor_gt 0.1690 _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_restrained_S_all 0.962 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.37006(4) 0.51530(3) 0.490077(18) 0.03899(17) Uani 1 1 d . . . O1 O 0.1677(3) 0.5540(3) 0.47073(15) 0.0705(10) Uani 1 1 d . . . O2 O 0.4066(3) 0.5137(2) 0.41194(11) 0.0567(7) Uani 1 1 d . . . O3 O 0.3537(2) 0.36837(19) 0.48848(12) 0.0572(7) Uani 1 1 d . . . O4 O 0.3746(3) 0.5091(2) 0.57127(11) 0.0578(7) Uani 1 1 d . . . O5 O 0.4277(2) 0.65784(18) 0.49550(12) 0.0573(7) Uani 1 1 d . . . O6 O 1.1677(5) 0.5677(5) 0.6881(2) 0.145(2) Uani 1 1 d . . . N1 N 0.5792(3) 0.5225(3) 0.70001(13) 0.0540(8) Uani 1 1 d . A . N2 N 0.4635(3) 0.8625(2) 0.48703(14) 0.0530(8) Uani 1 1 d . A . N3 N 0.0275(4) 0.6612(3) 0.42368(17) 0.0744(11) Uani 1 1 d . . . N4 N 1.0293(4) 0.6558(4) 0.6240(2) 0.0871(13) Uani 1 1 d . . . C1 C 0.4796(4) 0.4968(3) 0.60280(16) 0.0464(9) Uani 1 1 d . . . C2 C 0.4635(4) 0.4903(3) 0.66412(16) 0.0584(11) Uani 1 1 d . . . H2A H 0.3886 0.5315 0.6717 0.070 Uiso 1 1 calc R A . H2B H 0.4433 0.4214 0.6731 0.070 Uiso 1 1 calc R . . C3 C 0.6845(4) 0.4621(3) 0.72193(16) 0.0556(10) Uani 1 1 d . . . C4 C 0.6996(5) 0.3592(4) 0.7188(2) 0.0770(13) Uani 1 1 d . A . H4A H 0.6352 0.3193 0.6994 0.092 Uiso 1 1 calc R . . C5 C 0.8141(6) 0.3176(5) 0.7455(2) 0.0980(18) Uani 1 1 d . . . H5A H 0.8261 0.2484 0.7443 0.118 Uiso 1 1 calc R A . C6 C 0.9116(6) 0.3767(6) 0.7740(2) 0.0977(19) Uani 1 1 d . A . H6A H 0.9867 0.3464 0.7921 0.117 Uiso 1 1 calc R . . C7 C 0.8985(5) 0.4797(5) 0.7760(2) 0.0810(15) Uani 1 1 d . . . H7A H 0.9648 0.5191 0.7945 0.097 Uiso 1 1 calc R A . C8 C 0.7832(4) 0.5241(4) 0.74946(17) 0.0613(11) Uani 1 1 d . A . C9 C 0.7363(4) 0.6264(4) 0.74256(16) 0.0591(11) Uani 1 1 d . . . C10 C 0.7893(5) 0.7203(4) 0.7592(2) 0.0803(14) Uani 1 1 d . A . H10A H 0.8720 0.7247 0.7796 0.096 Uiso 1 1 calc R . . C11 C 0.7181(6) 0.8052(5) 0.7450(2) 0.0943(17) Uani 1 1 d . . . H11A H 0.7524 0.8675 0.7564 0.113 Uiso 1 1 calc R A . C12 C 0.5956(5) 0.8000(4) 0.7140(2) 0.0827(14) Uani 1 1 d . A . H12A H 0.5498 0.8591 0.7047 0.099 Uiso 1 1 calc R . . C13 C 0.5396(5) 0.7093(4) 0.69670(19) 0.0704(12) Uani 1 1 d . . . H13A H 0.4571 0.7066 0.6761 0.084 Uiso 1 1 calc R A . C14 C 0.6113(4) 0.6216(3) 0.71118(15) 0.0544(10) Uani 1 1 d . A . C15 C 0.5451(4) 0.6866(3) 0.50309(16) 0.0499(9) Uani 1 1 d . . . C16 C 0.5741(4) 0.7989(3) 0.5037(2) 0.0787(15) Uani 1 1 d . . . H16A H 0.6097 0.8177 0.5410 0.094 Uiso 1 1 calc R A . H16B H 0.6423 0.8117 0.4795 0.094 Uiso 1 1 calc R . . C17 C 0.4169(5) 0.8844(3) 0.43233(18) 0.0614(11) Uani 1 1 d . . . C18 C 0.4731(8) 0.8548(5) 0.3840(3) 0.126(3) Uani 1 1 d . A . H18A H 0.4760 0.7820 0.3825 0.151 Uiso 1 1 calc R . . H18B H 0.5635 0.8794 0.3860 0.151 Uiso 1 1 calc R . . C19 C 0.3958(11) 0.8942(7) 0.3314(3) 0.142(4) Uani 1 1 d . . . H19A H 0.4220 0.8797 0.2967 0.171 Uiso 1 1 calc R A . C20 C 0.2849(13) 0.9526(8) 0.3369(4) 0.160(5) Uani 1 1 d . A . H20A H 0.2401 0.9761 0.3039 0.192 Uiso 1 1 calc R . . C21 C 0.2344(8) 0.9795(5) 0.3827(3) 0.119(3) Uani 1 1 d . . . H21A H 0.1585 1.0188 0.3819 0.142 Uiso 1 1 calc R A . C22 C 0.3023(5) 0.9452(3) 0.4328(2) 0.0727(14) Uani 1 1 d . A . C23 C 0.2798(4) 0.9563(3) 0.4893(2) 0.0671(13) Uani 1 1 d . . . C24 C 0.1822(6) 1.0073(4) 0.5183(4) 0.105(2) Uani 1 1 d . A . H24A H 0.1827 1.0780 0.5085 0.126 Uiso 1 1 calc R . . H24B H 0.0954 0.9809 0.5051 0.126 Uiso 1 1 calc R . . C25 C 0.2001(8) 0.9990(5) 0.5768(4) 0.106(2) Uani 1 1 d . . . H25A H 0.1398 1.0313 0.5970 0.127 Uiso 1 1 calc R A . C26 C 0.3000(9) 0.9469(5) 0.6049(3) 0.119(2) Uani 1 1 d . A . H26A H 0.3059 0.9446 0.6434 0.143 Uiso 1 1 calc R . . C27 C 0.3884(6) 0.8998(4) 0.5794(2) 0.0874(16) Uani 1 1 d . . . H27A H 0.4559 0.8637 0.5994 0.105 Uiso 1 1 calc R A . C28 C 0.3803(4) 0.9043(3) 0.52068(18) 0.0540(10) Uani 1 1 d . A . C29A C 0.1462(6) 0.6344(5) 0.4419(3) 0.063(2) Uani 0.629(11) 1 d PD A 1 H29A H 0.2174 0.6740 0.4341 0.075 Uiso 0.629(11) 1 calc PR A 1 C29B C 0.0777(11) 0.5507(11) 0.4653(6) 0.139(11) Uani 0.371(11) 1 d PD A 2 H29B H 0.0232 0.5018 0.4783 0.167 Uiso 0.371(11) 1 calc PR A 2 C30 C -0.0991(6) 0.6279(8) 0.4212(5) 0.223(6) Uani 1 1 d D A . H30A H -0.1026 0.5694 0.4442 0.335 Uiso 1 1 calc R . . H30B H -0.1303 0.6111 0.3836 0.335 Uiso 1 1 calc R . . H30C H -0.1542 0.6796 0.4342 0.335 Uiso 1 1 calc R . . C31 C 0.0322(10) 0.7495(8) 0.3890(6) 0.305(8) Uani 1 1 d D A . H31A H 0.1218 0.7733 0.3906 0.458 Uiso 1 1 calc R . . H31B H -0.0230 0.8011 0.4020 0.458 Uiso 1 1 calc R . . H31C H 0.0009 0.7325 0.3514 0.458 Uiso 1 1 calc R . . C32 C 1.0576(8) 0.5870(6) 0.6674(3) 0.121(2) Uani 1 1 d . . . H32A H 0.9869 0.5543 0.6810 0.145 Uiso 1 1 calc R . . C33 C 1.1413(7) 0.7009(6) 0.6067(3) 0.144(3) Uani 1 1 d . . . H33A H 1.2192 0.6712 0.6260 0.216 Uiso 1 1 calc R . . H33B H 1.1400 0.7716 0.6147 0.216 Uiso 1 1 calc R . . H33C H 1.1420 0.6912 0.5675 0.216 Uiso 1 1 calc R . . C34 C 0.8975(6) 0.6756(7) 0.6071(3) 0.158(3) Uani 1 1 d . . . H34A H 0.8426 0.6322 0.6265 0.237 Uiso 1 1 calc R . . H34B H 0.8802 0.6639 0.5679 0.237 Uiso 1 1 calc R . . H34C H 0.8783 0.7444 0.6151 0.237 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 0.0322(2) 0.0376(3) 0.0450(3) 0.00602(18) -0.00580(17) -0.00203(17) O1 0.0324(14) 0.079(2) 0.097(3) 0.0154(19) -0.0068(16) 0.0052(15) O2 0.0458(15) 0.0766(19) 0.0465(15) 0.0093(13) -0.0009(12) 0.0017(13) O3 0.0452(14) 0.0388(15) 0.084(2) 0.0060(13) -0.0086(14) -0.0050(11) O4 0.0472(15) 0.079(2) 0.0462(15) 0.0067(13) -0.0022(13) -0.0010(13) O5 0.0402(13) 0.0380(14) 0.090(2) 0.0043(13) -0.0089(13) -0.0053(11) O6 0.088(3) 0.227(6) 0.116(4) -0.008(4) -0.009(3) 0.039(4) N1 0.0504(18) 0.068(2) 0.0418(18) 0.0045(15) -0.0033(15) -0.0012(16) N2 0.0545(18) 0.0357(17) 0.067(2) 0.0050(15) -0.0031(16) -0.0002(14) N3 0.058(2) 0.084(3) 0.076(3) 0.018(2) -0.0150(19) 0.009(2) N4 0.071(3) 0.107(4) 0.082(3) -0.028(3) 0.000(2) -0.004(3) C1 0.047(2) 0.044(2) 0.046(2) 0.0040(15) -0.0018(17) -0.0068(15) C2 0.049(2) 0.079(3) 0.046(2) 0.008(2) -0.0010(18) -0.0115(19) C3 0.056(2) 0.071(3) 0.040(2) 0.0108(19) 0.0039(18) 0.003(2) C4 0.085(3) 0.078(3) 0.068(3) 0.008(2) 0.005(3) 0.008(3) C5 0.109(4) 0.091(4) 0.095(4) 0.023(3) 0.014(4) 0.034(4) C6 0.083(4) 0.127(5) 0.084(4) 0.036(4) 0.010(3) 0.040(4) C7 0.059(3) 0.121(5) 0.062(3) 0.020(3) 0.003(2) 0.009(3) C8 0.052(2) 0.088(3) 0.043(2) 0.010(2) 0.0024(19) -0.002(2) C9 0.055(2) 0.080(3) 0.042(2) 0.004(2) 0.0000(19) -0.006(2) C10 0.077(3) 0.092(4) 0.069(3) -0.003(3) -0.007(3) -0.018(3) C11 0.117(5) 0.082(4) 0.084(4) -0.014(3) 0.013(4) -0.016(4) C12 0.096(4) 0.070(3) 0.083(4) -0.004(3) 0.010(3) 0.010(3) C13 0.069(3) 0.086(4) 0.056(3) 0.011(2) 0.005(2) 0.011(3) C14 0.054(2) 0.071(3) 0.038(2) 0.0032(19) 0.0077(18) -0.002(2) C15 0.0477(19) 0.0377(19) 0.062(3) 0.0052(17) -0.0049(18) -0.0045(17) C16 0.055(2) 0.042(2) 0.134(5) 0.003(3) -0.014(3) -0.006(2) C17 0.084(3) 0.042(2) 0.058(3) 0.0000(19) 0.009(2) -0.023(2) C18 0.198(7) 0.083(4) 0.107(5) -0.022(4) 0.058(5) -0.074(5) C19 0.240(11) 0.123(7) 0.072(5) -0.031(5) 0.053(6) -0.099(7) C20 0.269(15) 0.131(8) 0.078(6) 0.015(5) 0.006(7) -0.097(8) C21 0.137(6) 0.088(4) 0.117(6) 0.041(4) -0.053(5) -0.039(4) C22 0.074(3) 0.045(2) 0.091(4) 0.024(2) -0.027(3) -0.020(2) C23 0.052(2) 0.042(2) 0.106(4) -0.002(2) 0.006(3) -0.0078(19) C24 0.072(3) 0.060(3) 0.183(8) 0.011(4) 0.015(4) -0.021(3) C25 0.106(5) 0.084(4) 0.135(7) -0.018(4) 0.057(5) -0.009(3) C26 0.146(7) 0.098(5) 0.120(6) -0.020(5) 0.043(5) -0.029(5) C27 0.115(4) 0.066(3) 0.083(4) -0.010(3) 0.018(3) -0.031(3) C28 0.059(2) 0.040(2) 0.061(3) 0.0001(18) 0.000(2) -0.0199(18) C29A 0.035(3) 0.067(5) 0.081(5) 0.028(4) -0.013(3) 0.001(3) C29B 0.20(2) 0.142(16) 0.097(13) -0.053(12) 0.101(15) -0.130(17) C30 0.078(5) 0.285(14) 0.312(14) -0.080(11) 0.046(6) -0.080(7) C31 0.360(19) 0.260(15) 0.293(16) 0.107(13) 0.022(14) -0.156(13) C32 0.117(6) 0.159(7) 0.092(5) -0.010(5) 0.034(5) -0.010(5) C33 0.132(6) 0.138(7) 0.166(8) -0.035(5) 0.033(5) -0.036(5) C34 0.085(4) 0.210(9) 0.168(8) -0.057(7) -0.041(5) 0.023(5) _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 O3 1.963(2) . ? Cu1 O4 1.967(3) . ? Cu1 O2 1.970(3) . ? Cu1 O5 1.986(2) . ? Cu1 O1 2.121(3) . ? Cu1 Cu1 2.6622(8) 3_666 ? O1 C29B 0.910(11) . ? O1 C29A 1.284(6) . ? O2 C1 1.254(5) 3_666 ? O3 C15 1.260(4) 3_666 ? O4 C1 1.255(4) . ? O5 C15 1.247(4) . ? O6 C32 1.203(8) . ? N1 C14 1.379(5) . ? N1 C3 1.396(5) . ? N1 C2 1.450(5) . ? N2 C28 1.355(5) . ? N2 C17 1.391(5) . ? N2 C16 1.430(5) . ? N3 C29A 1.289(6) . ? N3 C30 1.355(7) . ? N3 C31 1.449(8) . ? N3 C29B 1.826(12) . ? N4 C34 1.382(7) . ? N4 C33 1.390(7) . ? N4 C32 1.400(8) . ? C1 O2 1.254(5) 3_666 ? C1 C2 1.516(5) . ? C3 C4 1.382(7) . ? C3 C8 1.410(6) . ? C4 C5 1.384(7) . ? C5 C6 1.390(8) . ? C6 C7 1.378(8) . ? C7 C8 1.404(6) . ? C8 C9 1.446(6) . ? C9 C10 1.403(7) . ? C9 C14 1.410(5) . ? C10 C11 1.365(7) . ? C11 C12 1.384(7) . ? C12 C13 1.380(7) . ? C13 C14 1.400(6) . ? C15 O3 1.260(4) 3_666 ? C15 C16 1.524(5) . ? C17 C18 1.413(7) . ? C17 C22 1.418(7) . ? C18 C19 1.519(11) . ? C19 C20 1.386(13) . ? C20 C21 1.322(12) . ? C21 C22 1.408(7) . ? C22 C23 1.421(7) . ? C23 C28 1.390(6) . ? C23 C24 1.444(8) . ? C24 C25 1.416(10) . ? C25 C26 1.352(11) . ? C26 C27 1.304(8) . ? C27 C28 1.419(7) . ? 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 O3 Cu1 O4 88.33(12) . . ? O3 Cu1 O2 89.69(12) . . ? O4 Cu1 O2 167.51(11) . . ? O3 Cu1 O5 167.71(10) . . ? O4 Cu1 O5 89.91(12) . . ? O2 Cu1 O5 89.40(12) . . ? O3 Cu1 O1 99.17(13) . . ? O4 Cu1 O1 98.67(13) . . ? O2 Cu1 O1 93.82(13) . . ? O5 Cu1 O1 93.12(12) . . ? O3 Cu1 Cu1 86.07(7) . 3_666 ? O4 Cu1 Cu1 83.99(8) . 3_666 ? O2 Cu1 Cu1 83.57(8) . 3_666 ? O5 Cu1 Cu1 81.65(7) . 3_666 ? O1 Cu1 Cu1 174.16(10) . 3_666 ? C29B O1 C29A 81.5(9) . . ? C29B O1 Cu1 162.5(9) . . ? C29A O1 Cu1 115.3(3) . . ? C1 O2 Cu1 123.3(3) 3_666 . ? C15 O3 Cu1 120.6(2) 3_666 . ? C1 O4 Cu1 123.0(3) . . ? C15 O5 Cu1 125.0(2) . . ? C14 N1 C3 108.7(3) . . ? C14 N1 C2 124.0(3) . . ? C3 N1 C2 126.7(4) . . ? C28 N2 C17 108.6(3) . . ? C28 N2 C16 126.4(4) . . ? C17 N2 C16 124.8(4) . . ? C29A N3 C30 140.6(7) . . ? C29A N3 C31 109.6(5) . . ? C30 N3 C31 109.2(7) . . ? C29A N3 C29B 52.5(5) . . ? C30 N3 C29B 88.2(5) . . ? C31 N3 C29B 161.8(6) . . ? C34 N4 C33 128.7(7) . . ? C34 N4 C32 117.6(7) . . ? C33 N4 C32 113.6(6) . . ? O2 C1 O4 126.1(4) 3_666 . ? O2 C1 C2 118.2(3) 3_666 . ? O4 C1 C2 115.6(3) . . ? N1 C2 C1 114.0(3) . . ? C4 C3 N1 129.4(4) . . ? C4 C3 C8 121.9(4) . . ? N1 C3 C8 108.7(4) . . ? C3 C4 C5 117.6(5) . . ? C4 C5 C6 121.7(6) . . ? C7 C6 C5 120.9(5) . . ? C6 C7 C8 118.8(5) . . ? C7 C8 C3 119.1(5) . . ? C7 C8 C9 134.2(5) . . ? C3 C8 C9 106.7(4) . . ? C10 C9 C14 119.4(4) . . ? C10 C9 C8 134.0(4) . . ? C14 C9 C8 106.6(4) . . ? C11 C10 C9 119.2(5) . . ? C10 C11 C12 121.1(5) . . ? C13 C12 C11 121.7(5) . . ? C12 C13 C14 117.8(4) . . ? N1 C14 C13 130.0(4) . . ? N1 C14 C9 109.2(4) . . ? C13 C14 C9 120.8(4) . . ? O5 C15 O3 126.6(3) . 3_666 ? O5 C15 C16 118.8(3) . . ? O3 C15 C16 114.5(3) 3_666 . ? N2 C16 C15 115.7(3) . . ? N2 C17 C18 127.3(5) . . ? N2 C17 C22 107.9(4) . . ? C18 C17 C22 124.8(5) . . ? C17 C18 C19 112.5(7) . . ? C20 C19 C18 117.8(8) . . ? C21 C20 C19 128.6(10) . . ? C20 C21 C22 116.1(9) . . ? C21 C22 C17 120.3(7) . . ? C21 C22 C23 133.2(6) . . ? C17 C22 C23 106.5(4) . . ? C28 C23 C22 107.0(4) . . ? C28 C23 C24 118.0(5) . . ? C22 C23 C24 135.0(5) . . ? C25 C24 C23 115.4(6) . . ? C26 C25 C24 123.8(7) . . ? C27 C26 C25 121.5(8) . . ? C26 C27 C28 119.2(7) . . ? N2 C28 C23 110.0(4) . . ? N2 C28 C27 127.9(4) . . ? C23 C28 C27 122.1(5) . . ? O1 C29A N3 121.0(5) . . ? O1 C29B N3 104.9(10) . . ? O6 C32 N4 124.1(7) . . ? 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 O3 Cu1 O1 C29B 17(4) . . . . ? O4 Cu1 O1 C29B -73(4) . . . . ? O2 Cu1 O1 C29B 107(4) . . . . ? O5 Cu1 O1 C29B -164(4) . . . . ? Cu1 Cu1 O1 C29B 170(3) 3_666 . . . ? O3 Cu1 O1 C29A -146.3(5) . . . . ? O4 Cu1 O1 C29A 124.0(5) . . . . ? O2 Cu1 O1 C29A -56.0(5) . . . . ? O5 Cu1 O1 C29A 33.6(5) . . . . ? Cu1 Cu1 O1 C29A 7.3(14) 3_666 . . . ? O3 Cu1 O2 C1 -87.6(3) . . . 3_666 ? O4 Cu1 O2 C1 -6.7(7) . . . 3_666 ? O5 Cu1 O2 C1 80.2(3) . . . 3_666 ? O1 Cu1 O2 C1 173.3(3) . . . 3_666 ? Cu1 Cu1 O2 C1 -1.5(3) 3_666 . . 3_666 ? O4 Cu1 O3 C15 -83.1(3) . . . 3_666 ? O2 Cu1 O3 C15 84.6(3) . . . 3_666 ? O5 Cu1 O3 C15 -1.2(7) . . . 3_666 ? O1 Cu1 O3 C15 178.4(3) . . . 3_666 ? Cu1 Cu1 O3 C15 1.0(3) 3_666 . . 3_666 ? O3 Cu1 O4 C1 87.5(3) . . . . ? O2 Cu1 O4 C1 6.5(7) . . . . ? O5 Cu1 O4 C1 -80.4(3) . . . . ? O1 Cu1 O4 C1 -173.5(3) . . . . ? Cu1 Cu1 O4 C1 1.2(3) 3_666 . . . ? O3 Cu1 O5 C15 4.5(8) . . . . ? O4 Cu1 O5 C15 86.2(3) . . . . ? O2 Cu1 O5 C15 -81.3(3) . . . . ? O1 Cu1 O5 C15 -175.1(3) . . . . ? Cu1 Cu1 O5 C15 2.2(3) 3_666 . . . ? Cu1 O4 C1 O2 -0.5(5) . . . 3_666 ? Cu1 O4 C1 C2 -178.0(2) . . . . ? C14 N1 C2 C1 79.5(5) . . . . ? C3 N1 C2 C1 -90.4(4) . . . . ? O2 C1 C2 N1 29.5(5) 3_666 . . . ? O4 C1 C2 N1 -152.8(3) . . . . ? C14 N1 C3 C4 -176.8(4) . . . . ? C2 N1 C3 C4 -5.6(7) . . . . ? C14 N1 C3 C8 2.3(4) . . . . ? C2 N1 C3 C8 173.5(4) . . . . ? N1 C3 C4 C5 -178.7(4) . . . . ? C8 C3 C4 C5 2.2(7) . . . . ? C3 C4 C5 C6 -0.6(8) . . . . ? C4 C5 C6 C7 -1.1(9) . . . . ? C5 C6 C7 C8 1.3(8) . . . . ? C6 C7 C8 C3 0.2(7) . . . . ? C6 C7 C8 C9 -179.6(5) . . . . ? C4 C3 C8 C7 -2.1(6) . . . . ? N1 C3 C8 C7 178.7(4) . . . . ? C4 C3 C8 C9 177.8(4) . . . . ? N1 C3 C8 C9 -1.4(4) . . . . ? C7 C8 C9 C10 1.1(9) . . . . ? C3 C8 C9 C10 -178.8(5) . . . . ? C7 C8 C9 C14 179.8(5) . . . . ? C3 C8 C9 C14 0.0(4) . . . . ? C14 C9 C10 C11 0.6(7) . . . . ? C8 C9 C10 C11 179.3(5) . . . . ? C9 C10 C11 C12 -0.8(8) . . . . ? C10 C11 C12 C13 0.7(8) . . . . ? C11 C12 C13 C14 -0.4(7) . . . . ? C3 N1 C14 C13 178.4(4) . . . . ? C2 N1 C14 C13 6.9(6) . . . . ? C3 N1 C14 C9 -2.3(4) . . . . ? C2 N1 C14 C9 -173.8(4) . . . . ? C12 C13 C14 N1 179.3(4) . . . . ? C12 C13 C14 C9 0.1(6) . . . . ? C10 C9 C14 N1 -179.6(4) . . . . ? C8 C9 C14 N1 1.4(4) . . . . ? C10 C9 C14 C13 -0.3(6) . . . . ? C8 C9 C14 C13 -179.3(4) . . . . ? Cu1 O5 C15 O3 -4.0(6) . . . 3_666 ? Cu1 O5 C15 C16 177.3(3) . . . . ? C28 N2 C16 C15 91.6(5) . . . . ? C17 N2 C16 C15 -82.5(5) . . . . ? O5 C15 C16 N2 -9.2(7) . . . . ? O3 C15 C16 N2 172.0(4) 3_666 . . . ? C28 N2 C17 C18 -179.5(4) . . . . ? C16 N2 C17 C18 -4.6(6) . . . . ? C28 N2 C17 C22 1.9(4) . . . . ? C16 N2 C17 C22 176.9(3) . . . . ? N2 C17 C18 C19 -179.1(4) . . . . ? C22 C17 C18 C19 -0.8(7) . . . . ? C17 C18 C19 C20 0.5(9) . . . . ? C18 C19 C20 C21 -0.5(14) . . . . ? C19 C20 C21 C22 0.6(13) . . . . ? C20 C21 C22 C17 -0.7(8) . . . . ? C20 C21 C22 C23 -179.2(6) . . . . ? N2 C17 C22 C21 179.5(4) . . . . ? C18 C17 C22 C21 0.9(7) . . . . ? N2 C17 C22 C23 -1.7(4) . . . . ? C18 C17 C22 C23 179.7(4) . . . . ? C21 C22 C23 C28 179.4(5) . . . . ? C17 C22 C23 C28 0.8(4) . . . . ? C21 C22 C23 C24 -1.2(9) . . . . ? C17 C22 C23 C24 -179.8(5) . . . . ? C28 C23 C24 C25 0.3(7) . . . . ? C22 C23 C24 C25 -179.1(5) . . . . ? C23 C24 C25 C26 -0.5(9) . . . . ? C24 C25 C26 C27 0.0(11) . . . . ? C25 C26 C27 C28 0.7(9) . . . . ? C17 N2 C28 C23 -1.5(4) . . . . ? C16 N2 C28 C23 -176.3(4) . . . . ? C17 N2 C28 C27 179.1(4) . . . . ? C16 N2 C28 C27 4.2(6) . . . . ? C22 C23 C28 N2 0.4(4) . . . . ? C24 C23 C28 N2 -179.1(4) . . . . ? C22 C23 C28 C27 179.9(4) . . . . ? C24 C23 C28 C27 0.4(6) . . . . ? C26 C27 C28 N2 178.5(5) . . . . ? C26 C27 C28 C23 -0.9(7) . . . . ? C29B O1 C29A N3 -0.7(13) . . . . ? Cu1 O1 C29A N3 174.2(5) . . . . ? C30 N3 C29A O1 -5.3(14) . . . . ? C31 N3 C29A O1 -175.4(9) . . . . ? C29B N3 C29A O1 0.4(8) . . . . ? C29A O1 C29B N3 0.4(8) . . . . ? Cu1 O1 C29B N3 -164(3) . . . . ? C29A N3 C29B O1 -0.5(10) . . . . ? C30 N3 C29B O1 175.9(13) . . . . ? C31 N3 C29B O1 12(4) . . . . ? C34 N4 C32 O6 -175.5(7) . . . . ? C33 N4 C32 O6 -0.2(10) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 28.20 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.718 _refine_diff_density_min -0.602 _refine_diff_density_rms 0.086 data_tian27m _database_code_CSD 181845 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H28 Cu N4 O4' _chemical_formula_weight 692.20 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 16.1794(1) _cell_length_b 24.1843(1) _cell_length_c 16.4207(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6425.21(9) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.68 _cell_measurement_theta_max 28.36 _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.48 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2856 _exptl_absorpt_coefficient_mu 0.730 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7207 _exptl_absorpt_correction_T_max 0.7588 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Siemens SMART CCD area detector diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% negligible _diffrn_reflns_number 42835 _diffrn_reflns_av_R_equivalents 0.0841 _diffrn_reflns_av_sigmaI/netI 0.0567 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 28.29 _reflns_number_total 7933 _reflns_number_gt 4953 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 1997)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material ; SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990) ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0635P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0027(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 7933 _refine_ls_number_parameters 444 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0715 _refine_ls_R_factor_gt 0.0402 _refine_ls_wR_factor_ref 0.1126 _refine_ls_wR_factor_gt 0.1000 _refine_ls_goodness_of_fit_ref 0.904 _refine_ls_restrained_S_all 0.904 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu5 Cu -0.317075(14) -0.442261(9) -0.499973(12) 0.03717(9) Uani 1 1 d . . . O1 O -0.23818(9) -0.45469(6) -0.41584(8) 0.0568(4) Uani 1 1 d . . . O2 O -0.14126(10) -0.39053(8) -0.43881(11) 0.0840(6) Uani 1 1 d . . . O3 O -0.30804(9) -0.36408(6) -0.51104(7) 0.0519(4) Uani 1 1 d . . . O4 O -0.32088(11) -0.34565(7) -0.37832(9) 0.0795(5) Uani 1 1 d . . . N1 N -0.41562(9) -0.44244(6) -0.57521(9) 0.0403(4) Uani 1 1 d . . . N2 N -0.33445(9) -0.52458(7) -0.50715(9) 0.0394(4) Uani 1 1 d . . . N3 N -0.17284(11) -0.48453(7) -0.27081(10) 0.0513(4) Uani 1 1 d . . . N4 N -0.27135(11) -0.25580(6) -0.54382(9) 0.0478(4) Uani 1 1 d . . . C1 C -0.44340(11) -0.49436(8) -0.59176(10) 0.0397(4) Uani 1 1 d . . . C2 C -0.45477(13) -0.39995(9) -0.60853(12) 0.0547(5) Uani 1 1 d . . . H2A H -0.4363 -0.3643 -0.5978 0.066 Uiso 1 1 calc R . . C3 C -0.52341(15) -0.40749(12) -0.65960(13) 0.0675(7) Uani 1 1 d . . . H3A H -0.5497 -0.3771 -0.6826 0.081 Uiso 1 1 calc R . . C4 C -0.55132(14) -0.45953(13) -0.67537(13) 0.0712(7) Uani 1 1 d . . . H4A H -0.5970 -0.4646 -0.7089 0.085 Uiso 1 1 calc R . . C5 C -0.51158(12) -0.50544(9) -0.64147(12) 0.0536(6) Uani 1 1 d . . . C6 C -0.53534(16) -0.56200(12) -0.65373(14) 0.0719(7) Uani 1 1 d . . . H6A H -0.5814 -0.5700 -0.6856 0.086 Uiso 1 1 calc R . . C7 C -0.49257(16) -0.60339(11) -0.62024(15) 0.0713(7) Uani 1 1 d . . . H7A H -0.5095 -0.6396 -0.6296 0.086 Uiso 1 1 calc R . . C8 C -0.42190(13) -0.59377(9) -0.57070(13) 0.0543(5) Uani 1 1 d . . . C9 C -0.37414(16) -0.63491(9) -0.53323(17) 0.0709(7) Uani 1 1 d . . . H9A H -0.3872 -0.6720 -0.5407 0.085 Uiso 1 1 calc R . . C10 C -0.30909(16) -0.62045(10) -0.48615(16) 0.0708(7) Uani 1 1 d . . . H10A H -0.2765 -0.6477 -0.4624 0.085 Uiso 1 1 calc R . . C11 C -0.29083(14) -0.56488(8) -0.47319(15) 0.0539(5) Uani 1 1 d . . . H11A H -0.2466 -0.5557 -0.4396 0.065 Uiso 1 1 calc R . . C12 C -0.39904(11) -0.53872(8) -0.55560(11) 0.0398(4) Uani 1 1 d . . . C13 C -0.23676(13) -0.48574(8) -0.21563(13) 0.0495(5) Uani 1 1 d . . . C14 C -0.28097(16) -0.44187(10) -0.18153(15) 0.0680(7) Uani 1 1 d . . . H14A H -0.2698 -0.4055 -0.1961 0.082 Uiso 1 1 calc R . . C15 C -0.34112(19) -0.45422(13) -0.12605(18) 0.0863(8) Uani 1 1 d . . . H15A H -0.3717 -0.4255 -0.1034 0.104 Uiso 1 1 calc R . . C16 C -0.35825(17) -0.50831(14) -0.10222(16) 0.0819(8) Uani 1 1 d . . . H16A H -0.3987 -0.5151 -0.0632 0.098 Uiso 1 1 calc R . . C17 C -0.31500(15) -0.55198(11) -0.13663(16) 0.0678(7) Uani 1 1 d . . . H17A H -0.3260 -0.5882 -0.1210 0.081 Uiso 1 1 calc R . . C18 C -0.25512(13) -0.54084(9) -0.19465(13) 0.0521(5) Uani 1 1 d . . . C19 C -0.20148(13) -0.57486(8) -0.24384(13) 0.0524(5) Uani 1 1 d . . . C20 C -0.19141(16) -0.63171(9) -0.25349(16) 0.0696(7) Uani 1 1 d . . . H20A H -0.2230 -0.6564 -0.2232 0.084 Uiso 1 1 calc R . . C21 C -0.1343(2) -0.65077(12) -0.30827(19) 0.0868(9) Uani 1 1 d . . . H21A H -0.1269 -0.6887 -0.3145 0.104 Uiso 1 1 calc R . . C22 C -0.08738(19) -0.61465(13) -0.35452(17) 0.0844(8) Uani 1 1 d . . . H22A H -0.0499 -0.6289 -0.3920 0.101 Uiso 1 1 calc R . . C23 C -0.09496(16) -0.55765(11) -0.34631(15) 0.0697(7) Uani 1 1 d . . . H23A H -0.0630 -0.5335 -0.3771 0.084 Uiso 1 1 calc R . . C24 C -0.15218(13) -0.53841(9) -0.29036(13) 0.0516(5) Uani 1 1 d . . . C25 C -0.14015(14) -0.43632(9) -0.31252(13) 0.0592(6) Uani 1 1 d . . . H25A H -0.0807 -0.4405 -0.3174 0.071 Uiso 1 1 calc R . . H25B H -0.1503 -0.4041 -0.2789 0.071 Uiso 1 1 calc R . . C26 C -0.17561(13) -0.42542(9) -0.39717(13) 0.0535(6) Uani 1 1 d . . . C27 C -0.21372(12) -0.25941(7) -0.60576(11) 0.0436(4) Uani 1 1 d . . . C28 C -0.13673(15) -0.28438(9) -0.60681(16) 0.0675(7) Uani 1 1 d . . . H28A H -0.1166 -0.3032 -0.5616 0.081 Uiso 1 1 calc R . . C29 C -0.09149(16) -0.28027(12) -0.6769(2) 0.0873(9) Uani 1 1 d . . . H29A H -0.0396 -0.2968 -0.6790 0.105 Uiso 1 1 calc R . . C30 C -0.12028(17) -0.25237(11) -0.74492(17) 0.0812(8) Uani 1 1 d . . . H30A H -0.0873 -0.2500 -0.7912 0.097 Uiso 1 1 calc R . . C31 C -0.19672(14) -0.22828(10) -0.74464(13) 0.0581(5) Uani 1 1 d . . . H31A H -0.2159 -0.2096 -0.7904 0.070 Uiso 1 1 calc R . . C32 C -0.24543(11) -0.23199(7) -0.67500(11) 0.0403(4) Uani 1 1 d . . . C33 C -0.32739(11) -0.21340(7) -0.65421(11) 0.0399(4) Uani 1 1 d . . . C34 C -0.38926(13) -0.18578(8) -0.69657(13) 0.0532(5) Uani 1 1 d . . . H34A H -0.3816 -0.1754 -0.7506 0.064 Uiso 1 1 calc R . . C35 C -0.46227(14) -0.17406(10) -0.65677(17) 0.0721(7) Uani 1 1 d . . . H35A H -0.5041 -0.1555 -0.6844 0.086 Uiso 1 1 calc R . . C36 C -0.47434(16) -0.18924(11) -0.57710(18) 0.0803(8) Uani 1 1 d . . . H36A H -0.5239 -0.1801 -0.5517 0.096 Uiso 1 1 calc R . . C37 C -0.41494(16) -0.21776(10) -0.53356(15) 0.0678(7) Uani 1 1 d . . . H37A H -0.4242 -0.2290 -0.4802 0.081 Uiso 1 1 calc R . . C38 C -0.34083(13) -0.22898(7) -0.57291(11) 0.0448(4) Uani 1 1 d . . . C39 C -0.26263(15) -0.27742(8) -0.46234(12) 0.0559(6) Uani 1 1 d . . . H39A H -0.2868 -0.2512 -0.4246 0.067 Uiso 1 1 calc R . . H39B H -0.2042 -0.2801 -0.4498 0.067 Uiso 1 1 calc R . . C40 C -0.30200(13) -0.33362(8) -0.44790(12) 0.0476(5) Uani 1 1 d . . . 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 Cu5 0.04069(15) 0.03669(14) 0.03411(14) 0.00098(9) -0.00928(9) -0.00645(9) O1 0.0610(9) 0.0487(8) 0.0607(9) 0.0164(6) -0.0310(7) -0.0185(7) O2 0.0662(11) 0.0963(12) 0.0894(13) 0.0437(11) -0.0237(9) -0.0365(9) O3 0.0786(11) 0.0369(7) 0.0401(8) -0.0017(5) -0.0180(6) -0.0043(7) O4 0.1158(15) 0.0748(11) 0.0477(9) -0.0060(8) 0.0248(9) -0.0348(10) N1 0.0347(8) 0.0538(9) 0.0325(8) -0.0027(7) -0.0007(6) 0.0037(7) N2 0.0310(8) 0.0404(8) 0.0469(9) -0.0048(7) -0.0010(7) -0.0039(6) N3 0.0568(11) 0.0426(9) 0.0543(11) 0.0113(8) -0.0206(9) -0.0051(8) N4 0.0659(12) 0.0420(9) 0.0355(9) 0.0052(7) -0.0074(8) 0.0010(8) C1 0.0295(9) 0.0597(12) 0.0299(9) -0.0105(8) 0.0047(7) -0.0069(8) C2 0.0561(14) 0.0661(13) 0.0419(11) 0.0027(10) -0.0026(10) 0.0124(11) C3 0.0551(14) 0.0954(19) 0.0519(13) 0.0143(12) -0.0109(11) 0.0190(14) C4 0.0445(13) 0.123(2) 0.0464(13) -0.0048(14) -0.0135(10) -0.0031(14) C5 0.0379(12) 0.0866(17) 0.0361(11) -0.0093(10) -0.0005(8) -0.0066(11) C6 0.0516(15) 0.107(2) 0.0568(15) -0.0252(14) -0.0067(11) -0.0335(14) C7 0.0650(17) 0.0773(17) 0.0718(16) -0.0305(14) 0.0013(13) -0.0332(14) C8 0.0468(12) 0.0549(12) 0.0611(13) -0.0205(10) 0.0130(10) -0.0147(10) C9 0.0671(16) 0.0444(13) 0.1011(19) -0.0199(13) 0.0161(15) -0.0080(12) C10 0.0654(17) 0.0434(13) 0.104(2) 0.0041(12) 0.0062(14) 0.0081(11) C11 0.0444(12) 0.0461(12) 0.0711(14) 0.0012(10) -0.0028(11) -0.0011(9) C12 0.0306(9) 0.0499(10) 0.0389(10) -0.0118(8) 0.0079(7) -0.0074(8) C13 0.0507(13) 0.0457(11) 0.0521(12) 0.0044(9) -0.0269(10) 0.0015(9) C14 0.0755(18) 0.0652(15) 0.0634(16) -0.0008(12) -0.0245(13) 0.0152(13) C15 0.087(2) 0.100(2) 0.0716(19) -0.0089(16) -0.0226(16) 0.0305(18) C16 0.0617(17) 0.119(2) 0.0647(17) 0.0100(17) -0.0082(13) 0.0080(17) C17 0.0631(17) 0.0791(18) 0.0612(16) 0.0135(13) -0.0192(12) -0.0095(13) C18 0.0491(12) 0.0542(12) 0.0530(13) 0.0083(10) -0.0229(10) -0.0049(10) C19 0.0566(13) 0.0445(11) 0.0562(13) 0.0069(10) -0.0239(10) -0.0023(10) C20 0.0847(18) 0.0449(12) 0.0792(17) 0.0046(12) -0.0222(14) -0.0022(12) C21 0.102(2) 0.0590(16) 0.099(2) -0.0123(15) -0.0273(18) 0.0121(16) C22 0.085(2) 0.093(2) 0.0757(19) -0.0151(16) -0.0130(15) 0.0285(17) C23 0.0638(16) 0.0795(18) 0.0657(16) 0.0062(13) -0.0115(12) 0.0064(13) C24 0.0525(13) 0.0503(12) 0.0520(12) 0.0049(10) -0.0228(10) 0.0017(10) C25 0.0611(15) 0.0533(12) 0.0631(14) 0.0128(10) -0.0278(11) -0.0192(11) C26 0.0533(14) 0.0478(11) 0.0595(14) 0.0113(10) -0.0192(10) -0.0113(10) C27 0.0497(12) 0.0354(9) 0.0458(11) -0.0014(8) -0.0107(9) -0.0003(8) C28 0.0640(16) 0.0581(14) 0.0803(17) -0.0001(12) -0.0212(13) 0.0158(12) C29 0.0519(16) 0.089(2) 0.121(3) -0.0065(18) 0.0033(16) 0.0192(14) C30 0.0650(17) 0.0867(19) 0.092(2) 0.0054(16) 0.0275(15) 0.0106(14) C31 0.0630(15) 0.0594(12) 0.0520(13) 0.0045(10) 0.0081(11) 0.0020(11) C32 0.0444(11) 0.0360(9) 0.0406(10) 0.0001(7) -0.0032(8) -0.0021(8) C33 0.0439(11) 0.0355(9) 0.0404(10) 0.0009(7) -0.0018(8) -0.0008(8) C34 0.0524(13) 0.0517(12) 0.0556(13) 0.0080(9) -0.0081(10) 0.0036(10) C35 0.0494(14) 0.0731(16) 0.0937(19) 0.0096(14) -0.0068(13) 0.0144(12) C36 0.0582(16) 0.0842(18) 0.098(2) 0.0003(16) 0.0229(14) 0.0110(14) C37 0.0783(18) 0.0657(15) 0.0593(14) -0.0005(12) 0.0228(13) -0.0008(13) C38 0.0525(12) 0.0388(10) 0.0430(11) -0.0018(8) 0.0015(9) -0.0022(9) C39 0.0914(17) 0.0420(11) 0.0343(11) 0.0018(8) -0.0132(10) -0.0104(11) C40 0.0589(13) 0.0443(11) 0.0398(11) -0.0029(9) -0.0071(9) -0.0070(9) _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 Cu5 O3 1.9050(14) . ? Cu5 O1 1.9049(12) . ? Cu5 N2 2.0141(16) . ? Cu5 N1 2.0171(15) . ? O1 C26 1.273(2) . ? O2 C26 1.220(2) . ? O3 C40 1.276(2) . ? O4 C40 1.218(2) . ? N1 C2 1.325(2) . ? N1 C1 1.361(2) . ? N2 C11 1.326(3) . ? N2 C12 1.357(2) . ? N3 C13 1.375(3) . ? N3 C24 1.383(3) . ? N3 C25 1.452(2) . ? N4 C27 1.383(2) . ? N4 C38 1.383(2) . ? N4 C39 1.443(2) . ? C1 C5 1.398(3) . ? C1 C12 1.421(3) . ? C2 C3 1.403(3) . ? C3 C4 1.362(4) . ? C4 C5 1.399(3) . ? C5 C6 1.435(3) . ? C6 C7 1.335(4) . ? C7 C8 1.422(3) . ? C8 C12 1.404(3) . ? C8 C9 1.402(3) . ? C9 C10 1.352(3) . ? C10 C11 1.392(3) . ? C13 C14 1.397(3) . ? C13 C18 1.408(3) . ? C14 C15 1.366(4) . ? C15 C16 1.393(4) . ? C16 C17 1.387(4) . ? C17 C18 1.385(3) . ? C18 C19 1.443(3) . ? C19 C20 1.393(3) . ? C19 C24 1.413(3) . ? C20 C21 1.369(4) . ? C21 C22 1.384(4) . ? C22 C23 1.391(4) . ? C23 C24 1.385(3) . ? C25 C26 1.527(3) . ? C27 C28 1.384(3) . ? C27 C32 1.413(2) . ? C28 C29 1.368(4) . ? C29 C30 1.385(4) . ? C30 C31 1.367(3) . ? C31 C32 1.392(3) . ? C32 C33 1.441(3) . ? C33 C34 1.390(3) . ? C33 C38 1.404(2) . ? C34 C35 1.379(3) . ? C35 C36 1.373(3) . ? C36 C37 1.382(4) . ? C37 C38 1.389(3) . ? C39 C40 1.520(3) . ? 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 O3 Cu5 O1 100.04(5) . . ? O3 Cu5 N2 170.46(6) . . ? O1 Cu5 N2 88.85(6) . . ? O3 Cu5 N1 90.25(6) . . ? O1 Cu5 N1 166.81(6) . . ? N2 Cu5 N1 81.48(6) . . ? C26 O1 Cu5 128.31(13) . . ? C40 O3 Cu5 120.10(12) . . ? C2 N1 C1 118.36(17) . . ? C2 N1 Cu5 128.98(14) . . ? C1 N1 Cu5 112.66(12) . . ? C11 N2 C12 118.10(17) . . ? C11 N2 Cu5 128.87(14) . . ? C12 N2 Cu5 113.00(12) . . ? C13 N3 C24 108.34(17) . . ? C13 N3 C25 127.01(18) . . ? C24 N3 C25 124.0(2) . . ? C27 N4 C38 108.88(15) . . ? C27 N4 C39 126.39(17) . . ? C38 N4 C39 124.71(17) . . ? N1 C1 C5 123.64(19) . . ? N1 C1 C12 116.51(15) . . ? C5 C1 C12 119.86(18) . . ? N1 C2 C3 121.6(2) . . ? C4 C3 C2 119.7(2) . . ? C3 C4 C5 120.4(2) . . ? C1 C5 C4 116.3(2) . . ? C1 C5 C6 118.4(2) . . ? C4 C5 C6 125.3(2) . . ? C7 C6 C5 121.2(2) . . ? C6 C7 C8 122.0(2) . . ? C12 C8 C9 116.8(2) . . ? C12 C8 C7 117.9(2) . . ? C9 C8 C7 125.3(2) . . ? C10 C9 C8 119.8(2) . . ? C9 C10 C11 120.2(2) . . ? N2 C11 C10 122.1(2) . . ? N2 C12 C8 123.05(19) . . ? N2 C12 C1 116.34(16) . . ? C8 C12 C1 120.61(17) . . ? N3 C13 C14 129.3(2) . . ? N3 C13 C18 109.88(19) . . ? C14 C13 C18 120.8(2) . . ? C15 C14 C13 117.8(2) . . ? C14 C15 C16 122.3(3) . . ? C17 C16 C15 120.0(3) . . ? C18 C17 C16 119.0(2) . . ? C17 C18 C13 120.0(2) . . ? C17 C18 C19 134.0(2) . . ? C13 C18 C19 106.0(2) . . ? C20 C19 C24 119.2(2) . . ? C20 C19 C18 134.1(2) . . ? C24 C19 C18 106.64(18) . . ? C21 C20 C19 119.1(2) . . ? C20 C21 C22 121.2(3) . . ? C21 C22 C23 121.6(3) . . ? C24 C23 C22 117.2(3) . . ? N3 C24 C23 129.2(2) . . ? N3 C24 C19 109.0(2) . . ? C23 C24 C19 121.8(2) . . ? N3 C25 C26 115.55(16) . . ? O2 C26 O1 127.7(2) . . ? O2 C26 C25 117.29(18) . . ? O1 C26 C25 114.96(18) . . ? N4 C27 C28 130.04(19) . . ? N4 C27 C32 108.51(17) . . ? C28 C27 C32 121.4(2) . . ? C29 C28 C27 117.4(2) . . ? C28 C29 C30 122.3(2) . . ? C31 C30 C29 120.6(2) . . ? C30 C31 C32 119.2(2) . . ? C31 C32 C27 119.07(19) . . ? C31 C32 C33 134.07(18) . . ? C27 C32 C33 106.86(16) . . ? C34 C33 C38 119.55(18) . . ? C34 C33 C32 133.95(18) . . ? C38 C33 C32 106.50(16) . . ? C35 C34 C33 118.6(2) . . ? C36 C35 C34 121.2(2) . . ? C35 C36 C37 121.8(2) . . ? C36 C37 C38 117.2(2) . . ? N4 C38 C37 129.25(19) . . ? N4 C38 C33 109.17(17) . . ? C37 C38 C33 121.6(2) . . ? N4 C39 C40 115.32(16) . . ? O4 C40 O3 127.25(19) . . ? O4 C40 C39 117.72(18) . . ? O3 C40 C39 114.95(17) . . ? 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 O3 Cu5 O1 C26 -25.4(2) . . . . ? N2 Cu5 O1 C26 151.2(2) . . . . ? N1 Cu5 O1 C26 -166.2(2) . . . . ? O1 Cu5 O3 C40 -41.58(16) . . . . ? N2 Cu5 O3 C40 159.8(3) . . . . ? N1 Cu5 O3 C40 130.12(16) . . . . ? O3 Cu5 N1 C2 -4.55(17) . . . . ? O1 Cu5 N1 C2 136.9(3) . . . . ? N2 Cu5 N1 C2 -179.80(17) . . . . ? O3 Cu5 N1 C1 175.73(12) . . . . ? O1 Cu5 N1 C1 -42.8(3) . . . . ? N2 Cu5 N1 C1 0.49(11) . . . . ? O3 Cu5 N2 C11 148.3(3) . . . . ? O1 Cu5 N2 C11 -10.68(18) . . . . ? N1 Cu5 N2 C11 178.32(18) . . . . ? O3 Cu5 N2 C12 -29.9(4) . . . . ? O1 Cu5 N2 C12 171.11(12) . . . . ? N1 Cu5 N2 C12 0.11(12) . . . . ? C2 N1 C1 C5 -0.6(3) . . . . ? Cu5 N1 C1 C5 179.13(14) . . . . ? C2 N1 C1 C12 179.25(16) . . . . ? Cu5 N1 C1 C12 -1.00(19) . . . . ? C1 N1 C2 C3 0.2(3) . . . . ? Cu5 N1 C2 C3 -179.54(15) . . . . ? N1 C2 C3 C4 0.4(3) . . . . ? C2 C3 C4 C5 -0.5(4) . . . . ? N1 C1 C5 C4 0.5(3) . . . . ? C12 C1 C5 C4 -179.37(18) . . . . ? N1 C1 C5 C6 -179.44(18) . . . . ? C12 C1 C5 C6 0.7(3) . . . . ? C3 C4 C5 C1 0.1(3) . . . . ? C3 C4 C5 C6 180.0(2) . . . . ? C1 C5 C6 C7 -1.5(3) . . . . ? C4 C5 C6 C7 178.5(2) . . . . ? C5 C6 C7 C8 0.3(4) . . . . ? C6 C7 C8 C12 1.8(3) . . . . ? C6 C7 C8 C9 179.7(2) . . . . ? C12 C8 C9 C10 -0.8(3) . . . . ? C7 C8 C9 C10 -178.7(2) . . . . ? C8 C9 C10 C11 1.7(4) . . . . ? C12 N2 C11 C10 0.3(3) . . . . ? Cu5 N2 C11 C10 -177.79(16) . . . . ? C9 C10 C11 N2 -1.4(4) . . . . ? C11 N2 C12 C8 0.5(3) . . . . ? Cu5 N2 C12 C8 178.94(14) . . . . ? C11 N2 C12 C1 -179.10(17) . . . . ? Cu5 N2 C12 C1 -0.68(19) . . . . ? C9 C8 C12 N2 -0.3(3) . . . . ? C7 C8 C12 N2 177.80(19) . . . . ? C9 C8 C12 C1 179.32(18) . . . . ? C7 C8 C12 C1 -2.6(3) . . . . ? N1 C1 C12 N2 1.1(2) . . . . ? C5 C1 C12 N2 -178.99(16) . . . . ? N1 C1 C12 C8 -178.50(16) . . . . ? C5 C1 C12 C8 1.4(3) . . . . ? C24 N3 C13 C14 -176.4(2) . . . . ? C25 N3 C13 C14 -5.6(3) . . . . ? C24 N3 C13 C18 3.7(2) . . . . ? C25 N3 C13 C18 174.47(16) . . . . ? N3 C13 C14 C15 -178.5(2) . . . . ? C18 C13 C14 C15 1.4(3) . . . . ? C13 C14 C15 C16 1.0(4) . . . . ? C14 C15 C16 C17 -1.7(4) . . . . ? C15 C16 C17 C18 -0.1(4) . . . . ? C16 C17 C18 C13 2.4(3) . . . . ? C16 C17 C18 C19 -177.6(2) . . . . ? N3 C13 C18 C17 176.81(18) . . . . ? C14 C13 C18 C17 -3.1(3) . . . . ? N3 C13 C18 C19 -3.2(2) . . . . ? C14 C13 C18 C19 176.92(18) . . . . ? C17 C18 C19 C20 2.4(4) . . . . ? C13 C18 C19 C20 -177.6(2) . . . . ? C17 C18 C19 C24 -178.5(2) . . . . ? C13 C18 C19 C24 1.4(2) . . . . ? C24 C19 C20 C21 -0.4(3) . . . . ? C18 C19 C20 C21 178.5(2) . . . . ? C19 C20 C21 C22 -0.7(4) . . . . ? C20 C21 C22 C23 1.3(4) . . . . ? C21 C22 C23 C24 -0.6(4) . . . . ? C13 N3 C24 C23 176.1(2) . . . . ? C25 N3 C24 C23 5.0(3) . . . . ? C13 N3 C24 C19 -2.7(2) . . . . ? C25 N3 C24 C19 -173.84(16) . . . . ? C22 C23 C24 N3 -179.2(2) . . . . ? C22 C23 C24 C19 -0.5(3) . . . . ? C20 C19 C24 N3 179.96(17) . . . . ? C18 C19 C24 N3 0.7(2) . . . . ? C20 C19 C24 C23 1.1(3) . . . . ? C18 C19 C24 C23 -178.17(19) . . . . ? C13 N3 C25 C26 -94.9(3) . . . . ? C24 N3 C25 C26 74.6(3) . . . . ? Cu5 O1 C26 O2 -18.1(4) . . . . ? Cu5 O1 C26 C25 162.33(15) . . . . ? N3 C25 C26 O2 -169.3(2) . . . . ? N3 C25 C26 O1 10.3(3) . . . . ? C38 N4 C27 C28 -177.2(2) . . . . ? C39 N4 C27 C28 1.4(3) . . . . ? C38 N4 C27 C32 2.8(2) . . . . ? C39 N4 C27 C32 -178.68(16) . . . . ? N4 C27 C28 C29 -178.4(2) . . . . ? C32 C27 C28 C29 1.6(3) . . . . ? C27 C28 C29 C30 0.1(4) . . . . ? C28 C29 C30 C31 -1.0(4) . . . . ? C29 C30 C31 C32 0.1(4) . . . . ? C30 C31 C32 C27 1.5(3) . . . . ? C30 C31 C32 C33 -178.2(2) . . . . ? N4 C27 C32 C31 177.57(17) . . . . ? C28 C27 C32 C31 -2.5(3) . . . . ? N4 C27 C32 C33 -2.7(2) . . . . ? C28 C27 C32 C33 177.29(18) . . . . ? C31 C32 C33 C34 1.6(4) . . . . ? C27 C32 C33 C34 -178.1(2) . . . . ? C31 C32 C33 C38 -178.7(2) . . . . ? C27 C32 C33 C38 1.6(2) . . . . ? C38 C33 C34 C35 0.5(3) . . . . ? C32 C33 C34 C35 -179.9(2) . . . . ? C33 C34 C35 C36 -0.1(4) . . . . ? C34 C35 C36 C37 -1.3(4) . . . . ? C35 C36 C37 C38 2.1(4) . . . . ? C27 N4 C38 C37 177.6(2) . . . . ? C39 N4 C38 C37 -1.0(3) . . . . ? C27 N4 C38 C33 -1.8(2) . . . . ? C39 N4 C38 C33 179.65(16) . . . . ? C36 C37 C38 N4 179.0(2) . . . . ? C36 C37 C38 C33 -1.7(3) . . . . ? C34 C33 C38 N4 179.81(17) . . . . ? C32 C33 C38 N4 0.1(2) . . . . ? C34 C33 C38 C37 0.4(3) . . . . ? C32 C33 C38 C37 -179.31(19) . . . . ? C27 N4 C39 C40 -96.9(2) . . . . ? C38 N4 C39 C40 81.4(2) . . . . ? Cu5 O3 C40 O4 -19.5(3) . . . . ? Cu5 O3 C40 C39 157.21(15) . . . . ? N4 C39 C40 O4 -156.3(2) . . . . ? N4 C39 C40 O3 26.7(3) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.561 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.066 data_tian33m _database_code_CSD 181846 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C68 H54 Cl Cu2 N7 O12' _chemical_formula_weight 1323.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.2574(4) _cell_length_b 24.8155(7) _cell_length_c 21.5853(5) _cell_angle_alpha 90.00 _cell_angle_beta 129.6300(10) _cell_angle_gamma 90.00 _cell_volume 5881.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 6024 _cell_measurement_theta_min 1.47 _cell_measurement_theta_max 28.52 _exptl_crystal_description block _exptl_crystal_colour 'dark green' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.495 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2728 _exptl_absorpt_coefficient_mu 0.842 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7294 _exptl_absorpt_correction_T_max 0.7863 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Siemens SMART CCD area detector diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% negligible _diffrn_reflns_number 39847 _diffrn_reflns_av_R_equivalents 0.1609 _diffrn_reflns_av_sigmaI/netI 0.2182 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 28.45 _reflns_number_total 14221 _reflns_number_gt 5344 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 1997)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material ; SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990) ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1561P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0025(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 14221 _refine_ls_number_parameters 858 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.2140 _refine_ls_R_factor_gt 0.1057 _refine_ls_wR_factor_ref 0.3068 _refine_ls_wR_factor_gt 0.2616 _refine_ls_goodness_of_fit_ref 0.886 _refine_ls_restrained_S_all 0.886 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu -0.56772(4) 0.18135(2) -0.27410(3) 0.03744(17) Uani 1 1 d . . . Cu2 Cu -0.71016(4) 0.17478(2) -0.46179(3) 0.03933(17) Uani 1 1 d . . . Cl1 Cl 0.0859(2) -0.01471(12) -0.12917(15) 0.1542(12) Uani 1 1 d . . . O1 O -0.9132(3) 0.1514(2) -0.4476(2) 0.0835(16) Uani 1 1 d . . . O2 O -0.7385(2) 0.19602(12) -0.36885(15) 0.0394(9) Uani 1 1 d . . . O3 O -0.5355(2) 0.19197(12) -0.36464(16) 0.0406(9) Uani 1 1 d . . . O4 O -0.6919(3) 0.09941(12) -0.43001(17) 0.0490(11) Uani 1 1 d . . . O5 O -0.5909(3) 0.10450(13) -0.29621(16) 0.0517(11) Uani 1 1 d . . . O6 O -0.5182(3) 0.15383(17) -0.44949(19) 0.0681(13) Uani 1 1 d . . . O7 O 0.0349(6) -0.0235(5) -0.0837(5) 0.287(6) Uani 1 1 d . . . O8 O 0.1740(8) 0.0269(4) -0.0922(6) 0.359(6) Uani 1 1 d . . . O9 O 0.1434(7) -0.0652(3) -0.1277(5) 0.264(5) Uani 1 1 d . . . O10 O -0.0172(11) 0.0002(6) -0.2054(5) 0.517(11) Uani 1 1 d . . . O1W O 0.0134(7) -0.4552(3) -0.0282(5) 0.237(4) Uani 1 1 d . . . H1W1 H 0.0280 -0.4311 -0.0520 0.106 Uiso 1 1 d . . . H2W1 H -0.0625 -0.4640 -0.0474 0.508 Uiso 1 1 d . . . N1 N -0.7647(3) 0.20230(17) -0.2492(2) 0.0557(13) Uani 1 1 d . . . N2 N -0.8563(3) 0.15559(16) -0.5740(2) 0.0421(11) Uani 1 1 d . . . N3 N -0.7461(3) 0.24762(15) -0.50996(19) 0.0384(10) Uani 1 1 d . . . N4 N -0.2744(3) 0.20043(16) -0.2476(2) 0.0447(12) Uani 1 1 d . . . N5 N -0.5725(4) -0.00395(17) -0.2823(3) 0.083(2) Uani 1 1 d . . . N6 N -0.4123(3) 0.16865(14) -0.16378(19) 0.0392(11) Uani 1 1 d . . . N7 N -0.5363(3) 0.25712(13) -0.23681(19) 0.0346(10) Uani 1 1 d . . . C1 C -0.7831(4) 0.2573(2) -0.2464(3) 0.0496(14) Uani 1 1 d . . . C2 C -0.8664(4) 0.2921(2) -0.3088(3) 0.0598(18) Uani 1 1 d . . . H2A H -0.9227 0.2792 -0.3631 0.055(14) Uiso 1 1 d R . . C3 C -0.8655(4) 0.3450(2) -0.2914(3) 0.0601(18) Uani 1 1 d . . . H3A H -0.9231 0.3695 -0.3337 0.10(2) Uiso 1 1 d R . . C4 C -0.7819(4) 0.3635(2) -0.2119(3) 0.0572(16) Uani 1 1 d . . . H4A H -0.7822 0.4007 -0.1997 0.040(13) Uiso 1 1 d R . . C5 C -0.6984(3) 0.32912(19) -0.1503(2) 0.0423(13) Uani 1 1 d . . . H5A H -0.6409 0.3417 -0.0959 0.044(13) Uiso 1 1 d R . . C6 C -0.6971(4) 0.27619(19) -0.1671(2) 0.0403(13) Uani 1 1 d . . . C7 C -0.6242(4) 0.22954(19) -0.1206(2) 0.0449(13) Uani 1 1 d . . . C8 C -0.5246(4) 0.2229(2) -0.0386(3) 0.0532(15) Uani 1 1 d . . . H8A H -0.4931 0.2529 -0.0024 0.084(19) Uiso 1 1 d R . . C9 C -0.4735(5) 0.1722(2) -0.0115(3) 0.071(2) Uani 1 1 d . . . H9A H -0.4036 0.1674 0.0441 0.068(16) Uiso 1 1 d R . . C10 C -0.5196(5) 0.1282(2) -0.0623(3) 0.0730(19) Uani 1 1 d . . . H10A H -0.4830 0.0934 -0.0410 0.080(18) Uiso 1 1 d R . . C11 C -0.6196(4) 0.1335(2) -0.1445(3) 0.0664(17) Uani 1 1 d . . . H11A H -0.6532 0.1035 -0.1809 0.056(14) Uiso 1 1 d R . . C12 C -0.6674(4) 0.1851(2) -0.1709(3) 0.0500(14) Uani 1 1 d . . . C13 C -0.8442(5) 0.1679(2) -0.3195(3) 0.0667(18) Uani 1 1 d . . . H13A H -0.8308 0.1312 -0.3016 0.030(11) Uiso 1 1 d R . . H13B H -0.9268 0.1770 -0.3441 0.058(16) Uiso 1 1 d R . . C14 C -0.8302(4) 0.17236(19) -0.3829(2) 0.0406(14) Uani 1 1 d . . . C15 C -0.9067(4) 0.1076(2) -0.6038(3) 0.0587(17) Uani 1 1 d . . . H15A H -0.8716 0.0769 -0.5686 0.085(19) Uiso 1 1 d R . . C16 C -1.0100(4) 0.1025(3) -0.6846(3) 0.070(2) Uani 1 1 d . . . H16A H -1.0463 0.0677 -0.7052 0.11(2) Uiso 1 1 d R . . C17 C -1.0572(4) 0.1449(3) -0.7348(3) 0.079(2) Uani 1 1 d . . . H17A H -1.1264 0.1405 -0.7907 0.068(16) Uiso 1 1 d R . . C18 C -1.0079(4) 0.1955(2) -0.7058(3) 0.0558(17) Uani 1 1 d . . . C19 C -1.0478(4) 0.2457(3) -0.7512(3) 0.076(2) Uani 1 1 d . . . H19A H -1.1178 0.2447 -0.8074 0.092(19) Uiso 1 1 d R . . C20 C -0.9942(4) 0.2907(3) -0.7196(3) 0.0696(18) Uani 1 1 d . . . H20A H -1.0251 0.3224 -0.7528 0.12(3) Uiso 1 1 d R . . C21 C -0.8893(4) 0.2961(2) -0.6365(3) 0.0616(16) Uani 1 1 d . . . C22 C -0.8249(4) 0.3423(2) -0.5984(3) 0.0693(16) Uani 1 1 d . . . H22A H -0.8474 0.3750 -0.6288 0.12(3) Uiso 1 1 d R . . C23 C -0.7254(4) 0.3417(2) -0.5176(3) 0.0668(18) Uani 1 1 d . . . H23A H -0.6850 0.3748 -0.4902 0.077(17) Uiso 1 1 d R . . C24 C -0.6876(4) 0.2941(2) -0.4755(3) 0.0511(14) Uani 1 1 d . . . H24A H -0.6166 0.2938 -0.4196 0.072(17) Uiso 1 1 d R . . C25 C -0.8461(4) 0.24917(19) -0.5897(2) 0.0423(13) Uani 1 1 d . . . C26 C -0.9045(3) 0.1990(2) -0.6238(2) 0.0405(13) Uani 1 1 d . . . C27 C -0.4724(4) 0.17295(19) -0.3814(2) 0.0428(14) Uani 1 1 d . . . C28 C -0.3370(4) 0.1738(2) -0.3259(3) 0.0607(19) Uani 1 1 d . . . H28A H -0.3121 0.1910 -0.3531 0.057(16) Uiso 1 1 d R . . H28B H -0.3092 0.1372 -0.3156 0.072(17) Uiso 1 1 d R . . C29 C -0.2746(3) 0.25469(18) -0.2367(2) 0.0374(13) Uani 1 1 d . . . C30 C -0.3494(4) 0.2949(2) -0.2926(3) 0.0587(18) Uani 1 1 d . . . H30A H -0.4103 0.2862 -0.3485 0.079(18) Uiso 1 1 d R . . C31 C -0.3334(4) 0.3468(2) -0.2663(3) 0.0598(19) Uani 1 1 d . . . H31A H -0.3830 0.3749 -0.3043 0.11(2) Uiso 1 1 d R . . C32 C -0.2472(4) 0.3591(2) -0.1863(3) 0.0608(18) Uani 1 1 d . . . H32A H -0.2411 0.3954 -0.1687 0.026(11) Uiso 1 1 d R . . C33 C -0.1692(4) 0.32077(19) -0.1297(3) 0.0483(15) Uani 1 1 d . . . H33A H -0.1052 0.3300 -0.0743 0.042(13) Uiso 1 1 d R . . C34 C -0.1842(3) 0.26701(18) -0.1556(2) 0.0387(13) Uani 1 1 d . . . C35 C -0.1186(3) 0.21777(19) -0.1157(2) 0.0391(13) Uani 1 1 d . . . C36 C -0.0165(4) 0.2055(2) -0.0354(3) 0.0479(15) Uani 1 1 d . . . H36A H 0.0239 0.2333 0.0048 0.18(4) Uiso 1 1 d R . . C37 C 0.0229(4) 0.1529(2) -0.0172(3) 0.0593(18) Uani 1 1 d . . . H37A H 0.0923 0.1439 0.0370 0.054(14) Uiso 1 1 d R . . C38 C -0.0364(4) 0.1132(2) -0.0766(3) 0.0635(19) Uani 1 1 d . . . H38A H -0.0073 0.0768 -0.0614 0.064(16) Uiso 1 1 d R . . C39 C -0.1349(4) 0.1244(2) -0.1546(3) 0.0531(17) Uani 1 1 d . . . H39A H -0.1733 0.0973 -0.1957 0.033(11) Uiso 1 1 d R . . C40 C -0.1763(3) 0.17722(18) -0.1732(2) 0.0384(13) Uani 1 1 d . . . C41 C -0.6058(5) -0.0076(2) -0.2316(3) 0.077(3) Uani 1 1 d . . . C42 C -0.7175(5) -0.0009(2) -0.2496(4) 0.089(3) Uani 1 1 d . . . H42A H -0.7886 0.0085 -0.3031 0.081(18) Uiso 1 1 d R . . C43 C -0.7193(6) -0.0081(3) -0.1883(4) 0.090(3) Uani 1 1 d . . . H43A H -0.7956 -0.0040 -0.1992 0.056(16) Uiso 1 1 d R . . C44 C -0.6196(7) -0.0210(3) -0.1131(4) 0.106(3) Uani 1 1 d . . . H44A H -0.6264 -0.0264 -0.0720 0.11(2) Uiso 1 1 d R . . C45 C -0.5048(6) -0.0272(2) -0.0924(4) 0.094(3) Uani 1 1 d . . . H45A H -0.4334 -0.0356 -0.0386 0.087(19) Uiso 1 1 d R . . C46 C -0.4994(5) -0.0206(2) -0.1533(3) 0.072(2) Uani 1 1 d . . . C47 C -0.4034(6) -0.0215(2) -0.1567(3) 0.079(3) Uani 1 1 d . . . C48 C -0.2636(6) -0.0304(2) -0.0997(4) 0.128(4) Uani 1 1 d . . . H48A H -0.2268 -0.0396 -0.0452 0.24(5) Uiso 1 1 d R . . C49 C -0.1900(7) -0.0261(3) -0.1221(5) 0.123(4) Uani 1 1 d . . . H49A H -0.1034 -0.0307 -0.0825 0.23(5) Uiso 1 1 d R . . C50 C -0.2496(6) -0.0146(2) -0.2022(4) 0.099(3) Uani 1 1 d . . . H50A H -0.1994 -0.0127 -0.2174 0.13(3) Uiso 1 1 d R . . C51 C -0.3734(6) -0.0069(2) -0.2604(4) 0.102(3) Uani 1 1 d . . . H51A H -0.4096 0.0014 -0.3150 0.12(3) Uiso 1 1 d R . . C52 C -0.4463(5) -0.0108(2) -0.2369(4) 0.076(2) Uani 1 1 d . . . C53 C -0.6532(5) 0.0186(2) -0.3619(3) 0.079(3) Uani 1 1 d . . . H53A H -0.6359 0.0029 -0.3943 0.11(2) Uiso 1 1 d R . . H53B H -0.7354 0.0095 -0.3856 0.11(2) Uiso 1 1 d R . . C54 C -0.6436(4) 0.08053(18) -0.3620(3) 0.0453(16) Uani 1 1 d . . . C55 C -0.3518(4) 0.1228(2) -0.1286(3) 0.0506(15) Uani 1 1 d . . . H55A H -0.3793 0.0907 -0.1607 0.067(16) Uiso 1 1 d R . . C56 C -0.2511(4) 0.1202(2) -0.0488(3) 0.0587(18) Uani 1 1 d . . . H56A H -0.2124 0.0862 -0.0250 0.10(2) Uiso 1 1 d R . . C57 C -0.2082(4) 0.1654(3) -0.0032(3) 0.0593(18) Uani 1 1 d . . . H57A H -0.1376 0.1634 0.0527 0.10(2) Uiso 1 1 d R . . C58 C -0.2664(4) 0.2153(2) -0.0371(3) 0.0500(16) Uani 1 1 d . . . C59 C -0.2310(5) 0.2654(3) 0.0037(3) 0.068(2) Uani 1 1 d . . . H59A H -0.1580 0.2667 0.0589 0.15(3) Uiso 1 1 d R . . C60 C -0.2935(4) 0.3108(2) -0.0323(3) 0.0675(19) Uani 1 1 d . . . H60A H -0.2710 0.3431 -0.0012 0.055(14) Uiso 1 1 d R . . C61 C -0.3996(4) 0.31172(19) -0.1183(3) 0.0463(15) Uani 1 1 d . . . C62 C -0.4693(4) 0.3569(2) -0.1623(3) 0.0594(17) Uani 1 1 d . . . H62A H -0.4453 0.3916 -0.1368 0.080(18) Uiso 1 1 d R . . C63 C -0.5694(4) 0.35170(18) -0.2402(3) 0.0517(15) Uani 1 1 d . . . H63A H -0.6177 0.3827 -0.2706 0.068(16) Uiso 1 1 d R . . C64 C -0.6023(3) 0.30085(18) -0.2759(2) 0.0395(13) Uani 1 1 d . . . H64A H -0.6757 0.2972 -0.3306 0.018(10) Uiso 1 1 d R . . C65 C -0.4377(3) 0.26217(17) -0.1590(2) 0.0356(12) Uani 1 1 d . . . C66 C -0.3692(3) 0.21451(18) -0.1190(2) 0.0359(13) Uani 1 1 d . . . C67 C -0.1043(3) 0.05943(7) -0.34115(12) 0.0716(19) Uani 1 1 d D . . H67A H -0.1452 0.0440 -0.3227 0.086 Uiso 1 1 calc R . . H67B H -0.0174 0.0531 -0.3013 0.086 Uiso 1 1 calc R . . C68 C -0.1553(7) 0.0384(4) -0.4224(2) 0.55(2) Uani 1 1 d D . . H68A H -0.1240 0.0029 -0.4169 0.826 Uiso 1 1 calc R . . H68B H -0.1320 0.0619 -0.4459 0.826 Uiso 1 1 calc R . . H68C H -0.2425 0.0370 -0.4565 0.826 Uiso 1 1 calc R . . O11 O -0.1323(10) 0.11695(10) -0.3604(5) 0.793(17) Uani 1 1 d D . . H11B H -0.1163 0.1329 -0.3214 1.190 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 0.0398(3) 0.0184(3) 0.0296(2) -0.00025(19) 0.01073(18) -0.0005(2) Cu2 0.0392(3) 0.0243(3) 0.0294(2) 0.0012(2) 0.01022(18) -0.0013(2) Cl1 0.1763(18) 0.116(2) 0.1198(16) -0.0075(15) 0.0710(14) 0.0011(17) O1 0.0561(19) 0.125(4) 0.0409(17) -0.019(2) 0.0175(14) -0.024(2) O2 0.0366(13) 0.0267(16) 0.0378(13) 0.0022(12) 0.0157(10) 0.0024(12) O3 0.0311(13) 0.0311(17) 0.0424(13) -0.0021(12) 0.0154(10) -0.0001(12) O4 0.0626(16) 0.0159(15) 0.0395(14) -0.0056(12) 0.0190(12) -0.0038(13) O5 0.0598(17) 0.0295(18) 0.0316(14) 0.0039(12) 0.0132(12) -0.0032(14) O6 0.0568(17) 0.080(3) 0.0421(16) -0.0115(17) 0.0198(13) 0.0034(19) O7 0.240(4) 0.472(17) 0.259(5) 0.068(7) 0.211(4) 0.021(8) O8 0.498(8) 0.226(7) 0.351(9) -0.155(7) 0.270(7) -0.276(6) O9 0.404(8) 0.102(6) 0.240(7) -0.010(5) 0.185(6) 0.089(6) O10 0.415(13) 0.60(2) 0.100(7) 0.026(10) -0.040(8) 0.278(13) O1W 0.320(6) 0.124(7) 0.348(7) 0.061(5) 0.250(5) 0.050(5) N1 0.082(2) 0.041(2) 0.0447(16) -0.0170(16) 0.0405(14) -0.020(2) N2 0.0383(16) 0.039(2) 0.0382(16) 0.0009(15) 0.0193(12) -0.0038(17) N3 0.0420(15) 0.027(2) 0.0466(15) -0.0003(14) 0.0284(12) 0.0033(15) N4 0.0378(17) 0.038(2) 0.0318(16) 0.0007(15) 0.0098(13) -0.0060(17) N5 0.111(3) 0.019(2) 0.048(2) 0.0025(18) 0.018(2) -0.001(2) N6 0.0450(16) 0.0238(19) 0.0374(15) -0.0042(13) 0.0210(12) 0.0013(15) N7 0.0362(15) 0.0171(17) 0.0444(15) 0.0047(13) 0.0228(12) 0.0015(14) C1 0.058(2) 0.048(3) 0.0478(19) -0.004(2) 0.0361(16) -0.010(2) C2 0.045(2) 0.078(4) 0.038(2) 0.009(2) 0.0176(18) -0.004(3) C3 0.051(2) 0.068(4) 0.054(2) 0.015(2) 0.0302(18) 0.008(3) C4 0.065(2) 0.052(3) 0.067(2) 0.007(2) 0.0477(18) -0.001(2) C5 0.0467(19) 0.041(3) 0.0412(18) 0.0031(18) 0.0289(14) 0.003(2) C6 0.0497(19) 0.039(3) 0.0385(17) 0.0048(17) 0.0312(14) 0.000(2) C7 0.061(2) 0.032(3) 0.0498(19) -0.0036(18) 0.0388(15) -0.008(2) C8 0.067(2) 0.044(3) 0.047(2) 0.008(2) 0.0361(17) 0.010(2) C9 0.083(3) 0.063(4) 0.067(3) 0.013(3) 0.048(2) 0.020(3) C10 0.104(3) 0.049(4) 0.086(3) 0.019(3) 0.070(2) 0.019(3) C11 0.104(3) 0.032(3) 0.087(3) -0.009(2) 0.072(2) -0.009(3) C12 0.071(2) 0.041(3) 0.0498(19) -0.0068(19) 0.0440(16) -0.016(2) C13 0.087(3) 0.050(3) 0.058(2) -0.026(2) 0.044(2) -0.032(3) C14 0.039(2) 0.039(3) 0.0315(18) 0.0006(17) 0.0162(15) 0.003(2) C15 0.064(3) 0.047(3) 0.050(2) -0.013(2) 0.0288(19) -0.012(2) C16 0.060(3) 0.072(4) 0.049(3) -0.018(3) 0.020(2) -0.022(3) C17 0.043(3) 0.128(6) 0.036(2) -0.012(3) 0.011(2) 0.005(3) C18 0.039(2) 0.083(4) 0.0343(19) 0.000(2) 0.0179(16) 0.020(2) C19 0.059(3) 0.122(5) 0.037(2) 0.024(3) 0.0259(18) 0.043(3) C20 0.074(3) 0.081(4) 0.057(2) 0.033(3) 0.0431(19) 0.043(3) C21 0.078(2) 0.060(3) 0.071(2) 0.034(2) 0.0593(17) 0.040(2) C22 0.099(3) 0.038(3) 0.113(3) 0.032(2) 0.086(2) 0.033(2) C23 0.084(3) 0.024(3) 0.108(3) 0.008(2) 0.068(2) 0.011(2) C24 0.063(2) 0.029(3) 0.076(2) -0.001(2) 0.0512(17) 0.002(2) C25 0.0495(19) 0.037(3) 0.0462(18) 0.0107(18) 0.0331(14) 0.013(2) C26 0.0373(18) 0.053(3) 0.0315(16) 0.0067(18) 0.0222(13) 0.007(2) C27 0.036(2) 0.038(3) 0.0341(19) 0.0038(18) 0.0125(16) -0.005(2) C28 0.043(2) 0.064(4) 0.042(2) -0.002(2) 0.011(2) 0.004(3) C29 0.0292(18) 0.035(3) 0.0384(18) 0.0062(17) 0.0171(14) -0.0030(18) C30 0.050(2) 0.050(3) 0.049(2) 0.021(2) 0.0185(19) 0.006(2) C31 0.052(3) 0.031(3) 0.068(3) 0.021(2) 0.025(2) 0.005(2) C32 0.067(3) 0.031(3) 0.085(3) 0.011(2) 0.049(2) 0.003(2) C33 0.050(2) 0.037(3) 0.055(2) 0.002(2) 0.0323(17) -0.001(2) C34 0.0337(18) 0.030(2) 0.050(2) 0.0115(17) 0.0253(15) 0.0039(18) C35 0.0329(18) 0.036(3) 0.0466(19) 0.0048(18) 0.0244(14) -0.0008(18) C36 0.038(2) 0.050(3) 0.039(2) 0.003(2) 0.0172(16) 0.004(2) C37 0.048(2) 0.067(4) 0.042(2) 0.013(2) 0.0197(19) 0.013(3) C38 0.056(3) 0.039(3) 0.080(3) 0.014(2) 0.036(2) 0.015(2) C39 0.050(2) 0.031(3) 0.059(3) -0.003(2) 0.0255(19) 0.001(2) C40 0.0258(18) 0.035(3) 0.0403(19) -0.0041(18) 0.0143(14) -0.0052(18) C41 0.095(4) 0.013(2) 0.056(3) -0.004(2) 0.017(3) -0.009(3) C42 0.083(4) 0.029(3) 0.085(4) -0.004(3) 0.021(3) -0.009(3) C43 0.106(4) 0.047(4) 0.088(4) -0.003(3) 0.048(3) -0.004(3) C44 0.150(5) 0.047(4) 0.092(4) -0.012(3) 0.063(4) -0.004(4) C45 0.142(5) 0.031(3) 0.071(3) -0.002(3) 0.050(3) 0.002(4) C46 0.089(3) 0.031(3) 0.056(3) -0.007(2) 0.027(3) -0.004(3) C47 0.096(4) 0.016(2) 0.049(3) 0.006(2) 0.010(3) 0.000(3) C48 0.118(5) 0.019(3) 0.075(4) 0.008(3) -0.019(4) 0.008(3) C49 0.143(5) 0.043(4) 0.172(6) 0.019(4) 0.096(5) 0.003(4) C50 0.130(5) 0.034(3) 0.107(4) 0.015(3) 0.063(4) 0.015(3) C51 0.144(5) 0.018(3) 0.111(5) 0.008(3) 0.066(4) 0.003(3) C52 0.085(4) 0.015(2) 0.076(4) -0.003(2) 0.029(3) 0.000(3) C53 0.102(4) 0.022(3) 0.049(3) 0.007(2) 0.018(3) 0.002(3) C54 0.048(2) 0.021(2) 0.038(2) -0.0024(17) 0.0135(18) -0.0027(19) C55 0.064(2) 0.030(3) 0.043(2) 0.0057(19) 0.0274(17) 0.012(2) C56 0.048(2) 0.047(3) 0.056(3) 0.015(2) 0.022(2) 0.013(2) C57 0.037(2) 0.087(4) 0.044(2) 0.013(2) 0.0216(17) 0.009(3) C58 0.048(2) 0.052(3) 0.0320(19) -0.002(2) 0.0175(16) -0.009(2) C59 0.062(3) 0.080(4) 0.032(2) -0.016(3) 0.016(2) -0.013(3) C60 0.068(3) 0.061(4) 0.055(3) -0.031(2) 0.031(2) -0.022(3) C61 0.049(2) 0.030(3) 0.054(2) -0.0126(19) 0.0295(17) -0.011(2) C62 0.079(3) 0.026(3) 0.078(3) -0.014(2) 0.052(2) -0.008(2) C63 0.064(2) 0.014(2) 0.080(3) 0.0035(19) 0.0473(19) 0.002(2) C64 0.046(2) 0.022(2) 0.0467(19) 0.0051(17) 0.0278(15) 0.0055(18) C65 0.0395(18) 0.022(2) 0.0434(18) -0.0040(16) 0.0257(14) -0.0038(17) C66 0.0364(19) 0.027(2) 0.0402(18) -0.0048(16) 0.0226(14) 0.0008(18) C67 0.096(3) 0.031(3) 0.111(3) -0.011(2) 0.077(2) 0.004(3) C68 0.93(4) 0.115(13) 0.61(3) -0.135(17) 0.49(3) -0.15(2) O11 0.561(19) 1.12(3) 0.188(9) -0.295(14) 0.000(12) 0.39(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 O5 1.942(3) . ? Cu1 O2 1.972(2) . ? Cu1 N7 1.981(3) . ? Cu1 N6 1.987(3) . ? Cu1 O3 2.290(4) . ? Cu2 O4 1.952(3) . ? Cu2 N3 1.983(4) . ? Cu2 N2 1.999(3) . ? Cu2 O3 2.029(2) . ? Cu2 O2 2.345(4) . ? Cl1 O10 1.386(8) . ? Cl1 O8 1.415(8) . ? Cl1 O9 1.487(8) . ? Cl1 O7 1.565(9) . ? O1 C14 1.230(5) . ? O2 C14 1.281(6) . ? O3 C27 1.257(6) . ? O4 C54 1.248(5) . ? O5 C54 1.255(5) . ? O6 C27 1.260(6) . ? O1W H1W1 0.8948 . ? O1W H2W1 0.9041 . ? N1 C1 1.399(7) . ? N1 C12 1.405(5) . ? N1 C13 1.455(6) . ? N2 C15 1.327(6) . ? N2 C26 1.358(6) . ? N3 C24 1.338(6) . ? N3 C25 1.366(5) . ? N4 C29 1.367(6) . ? N4 C40 1.415(5) . ? N4 C28 1.471(6) . ? N5 C52 1.405(8) . ? N5 C53 1.438(6) . ? N5 C41 1.446(10) . ? N6 C55 1.334(6) . ? N6 C66 1.360(5) . ? N7 C64 1.328(5) . ? N7 C65 1.342(4) . ? C1 C2 1.389(6) . ? C1 C6 1.406(6) . ? C2 C3 1.363(8) . ? C2 H2A 0.9599 . ? C3 C4 1.403(7) . ? C3 H3A 0.9601 . ? C4 C5 1.376(6) . ? C4 H4A 0.9601 . ? C5 C6 1.366(6) . ? C5 H5A 0.9601 . ? C6 C7 1.448(6) . ? C7 C12 1.387(6) . ? C7 C8 1.404(5) . ? C8 C9 1.383(7) . ? C8 H8A 0.9600 . ? C9 C10 1.382(8) . ? C9 H9A 0.9601 . ? C10 C11 1.404(6) . ? C10 H10A 0.9601 . ? C11 C12 1.389(7) . ? C11 H11A 0.9602 . ? C13 C14 1.509(8) . ? C13 H13A 0.9598 . ? C13 H13B 0.9601 . ? C15 C16 1.396(6) . ? C15 H15A 0.9600 . ? C16 C17 1.342(9) . ? C16 H16A 0.9601 . ? C17 C18 1.378(9) . ? C17 H17A 0.9601 . ? C18 C26 1.409(5) . ? C18 C19 1.460(9) . ? C19 C20 1.276(9) . ? C19 H19A 0.9601 . ? C20 C21 1.433(6) . ? C20 H20A 0.9602 . ? C21 C22 1.368(8) . ? C21 C25 1.401(7) . ? C22 C23 1.377(7) . ? C22 H22A 0.9601 . ? C23 C24 1.374(7) . ? C23 H23A 0.9599 . ? C24 H24A 0.9600 . ? C25 C26 1.416(7) . ? C27 C28 1.487(6) . ? C28 H28A 0.9600 . ? C28 H28B 0.9597 . ? C29 C34 1.394(5) . ? C29 C30 1.395(6) . ? C30 C31 1.366(7) . ? C30 H30A 0.9599 . ? C31 C32 1.370(7) . ? C31 H31A 0.9598 . ? C32 C33 1.379(6) . ? C32 H32A 0.9595 . ? C33 C34 1.409(6) . ? C33 H33A 0.9597 . ? C34 C35 1.443(6) . ? C35 C40 1.388(6) . ? C35 C36 1.413(5) . ? C36 C37 1.375(7) . ? C36 H36A 0.9599 . ? C37 C38 1.397(7) . ? C37 H37A 0.9597 . ? C38 C39 1.367(6) . ? C38 H38A 0.9600 . ? C39 C40 1.386(6) . ? C39 H39A 0.9600 . ? C41 C42 1.388(10) . ? C41 C46 1.411(7) . ? C42 C43 1.352(11) . ? C42 H42A 0.9600 . ? C43 C44 1.348(8) . ? C43 H43A 0.9599 . ? C44 C45 1.404(11) . ? C44 H44A 0.9600 . ? C45 C46 1.374(11) . ? C45 H45A 0.9600 . ? C46 C47 1.418(10) . ? C47 C52 1.444(10) . ? C47 C48 1.551(9) . ? C48 C49 1.412(14) . ? C48 H48A 0.9599 . ? C49 C50 1.387(11) . ? C49 H49A 0.9598 . ? C50 C51 1.378(9) . ? C50 H50A 0.9598 . ? C51 C52 1.422(11) . ? C51 H51A 0.9600 . ? C53 C54 1.543(7) . ? C53 H53A 0.9597 . ? C53 H53B 0.9600 . ? C55 C56 1.369(6) . ? C55 H55A 0.9601 . ? C56 C57 1.354(8) . ? C56 H56A 0.9599 . ? C57 C58 1.410(7) . ? C57 H57A 0.9600 . ? C58 C66 1.403(5) . ? C58 C59 1.417(8) . ? C59 C60 1.336(8) . ? C59 H59A 0.9600 . ? C60 C61 1.468(6) . ? C60 H60A 0.9599 . ? C61 C62 1.393(6) . ? C61 C65 1.404(6) . ? C62 C63 1.348(6) . ? C62 H62A 0.9600 . ? C63 C64 1.395(6) . ? C63 H63A 0.9602 . ? C64 H64A 0.9599 . ? C65 C66 1.422(6) . ? C67 O11 1.4690(19) . ? C67 C68 1.500(2) . ? C67 H67A 0.9700 . ? C67 H67B 0.9700 . ? C68 H68A 0.9600 . ? C68 H68B 0.9600 . ? C68 H68C 0.9600 . ? O11 H11B 0.8200 . ? 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 O5 Cu1 O2 91.30(11) . . ? O5 Cu1 N7 172.20(15) . . ? O2 Cu1 N7 93.20(12) . . ? O5 Cu1 N6 91.35(13) . . ? O2 Cu1 N6 165.28(17) . . ? N7 Cu1 N6 82.71(13) . . ? O5 Cu1 O3 89.91(14) . . ? O2 Cu1 O3 83.15(12) . . ? N7 Cu1 O3 96.94(14) . . ? N6 Cu1 O3 111.34(14) . . ? O4 Cu2 N3 171.86(12) . . ? O4 Cu2 N2 89.99(14) . . ? N3 Cu2 N2 82.01(14) . . ? O4 Cu2 O3 92.15(11) . . ? N3 Cu2 O3 94.96(12) . . ? N2 Cu2 O3 161.03(17) . . ? O4 Cu2 O2 88.38(14) . . ? N3 Cu2 O2 96.66(14) . . ? N2 Cu2 O2 118.35(14) . . ? O3 Cu2 O2 80.56(12) . . ? O10 Cl1 O8 111.3(8) . . ? O10 Cl1 O9 113.8(7) . . ? O8 Cl1 O9 108.9(6) . . ? O10 Cl1 O7 102.6(8) . . ? O8 Cl1 O7 110.4(7) . . ? O9 Cl1 O7 109.8(6) . . ? C14 O2 Cu1 124.0(3) . . ? C14 O2 Cu2 113.6(3) . . ? Cu1 O2 Cu2 94.21(13) . . ? C27 O3 Cu2 104.8(2) . . ? C27 O3 Cu1 140.6(3) . . ? Cu2 O3 Cu1 94.35(13) . . ? C54 O4 Cu2 128.5(3) . . ? C54 O5 Cu1 129.0(3) . . ? H1W1 O1W H2W1 123.1 . . ? C1 N1 C12 108.3(4) . . ? C1 N1 C13 125.1(4) . . ? C12 N1 C13 126.2(4) . . ? C15 N2 C26 119.0(4) . . ? C15 N2 Cu2 128.7(3) . . ? C26 N2 Cu2 112.3(3) . . ? C24 N3 C25 117.1(4) . . ? C24 N3 Cu2 129.3(3) . . ? C25 N3 Cu2 113.5(3) . . ? C29 N4 C40 108.3(3) . . ? C29 N4 C28 125.0(4) . . ? C40 N4 C28 123.9(4) . . ? C52 N5 C53 125.0(7) . . ? C52 N5 C41 110.9(5) . . ? C53 N5 C41 121.9(6) . . ? C55 N6 C66 118.3(3) . . ? C55 N6 Cu1 129.8(3) . . ? C66 N6 Cu1 111.9(3) . . ? C64 N7 C65 118.1(4) . . ? C64 N7 Cu1 129.3(3) . . ? C65 N7 Cu1 112.5(3) . . ? C2 C1 N1 129.2(4) . . ? C2 C1 C6 121.1(5) . . ? N1 C1 C6 109.6(4) . . ? C3 C2 C1 118.6(4) . . ? C3 C2 H2A 120.8 . . ? C1 C2 H2A 120.5 . . ? C2 C3 C4 120.3(5) . . ? C2 C3 H3A 119.7 . . ? C4 C3 H3A 120.0 . . ? C5 C4 C3 121.0(5) . . ? C5 C4 H4A 118.9 . . ? C3 C4 H4A 120.0 . . ? C6 C5 C4 119.3(4) . . ? C6 C5 H5A 119.5 . . ? C4 C5 H5A 121.2 . . ? C5 C6 C1 119.6(4) . . ? C5 C6 C7 135.3(4) . . ? C1 C6 C7 105.1(4) . . ? C12 C7 C8 118.7(4) . . ? C12 C7 C6 109.3(4) . . ? C8 C7 C6 132.0(4) . . ? C9 C8 C7 118.5(5) . . ? C9 C8 H8A 121.1 . . ? C7 C8 H8A 120.5 . . ? C10 C9 C8 121.9(5) . . ? C10 C9 H9A 118.9 . . ? C8 C9 H9A 119.2 . . ? C9 C10 C11 120.9(5) . . ? C9 C10 H10A 119.4 . . ? C11 C10 H10A 119.6 . . ? C12 C11 C10 116.3(5) . . ? C12 C11 H11A 121.4 . . ? C10 C11 H11A 122.3 . . ? C7 C12 C11 123.7(4) . . ? C7 C12 N1 107.7(4) . . ? C11 C12 N1 128.6(4) . . ? N1 C13 C14 115.9(5) . . ? N1 C13 H13A 108.3 . . ? C14 C13 H13A 109.1 . . ? N1 C13 H13B 107.7 . . ? C14 C13 H13B 107.8 . . ? H13A C13 H13B 107.7 . . ? O1 C14 O2 124.1(5) . . ? O1 C14 C13 114.3(5) . . ? O2 C14 C13 121.6(4) . . ? N2 C15 C16 119.9(5) . . ? N2 C15 H15A 118.7 . . ? C16 C15 H15A 121.4 . . ? C17 C16 C15 121.7(6) . . ? C17 C16 H16A 119.2 . . ? C15 C16 H16A 119.1 . . ? C16 C17 C18 119.9(4) . . ? C16 C17 H17A 120.7 . . ? C18 C17 H17A 119.4 . . ? C17 C18 C26 116.6(5) . . ? C17 C18 C19 127.3(4) . . ? C26 C18 C19 116.0(5) . . ? C20 C19 C18 123.0(4) . . ? C20 C19 H19A 118.9 . . ? C18 C19 H19A 118.1 . . ? C19 C20 C21 122.8(6) . . ? C19 C20 H20A 118.9 . . ? C21 C20 H20A 118.3 . . ? C22 C21 C25 116.5(4) . . ? C22 C21 C20 126.6(5) . . ? C25 C21 C20 116.9(5) . . ? C21 C22 C23 120.4(5) . . ? C21 C22 H22A 119.5 . . ? C23 C22 H22A 120.0 . . ? C24 C23 C22 120.0(5) . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? N3 C24 C23 122.1(4) . . ? N3 C24 H24A 118.4 . . ? C23 C24 H24A 119.6 . . ? N3 C25 C21 123.8(4) . . ? N3 C25 C26 115.2(4) . . ? C21 C25 C26 121.0(4) . . ? N2 C26 C18 122.8(5) . . ? N2 C26 C25 117.0(3) . . ? C18 C26 C25 120.3(5) . . ? O3 C27 O6 123.0(4) . . ? O3 C27 C28 124.2(4) . . ? O6 C27 C28 112.7(5) . . ? N4 C28 C27 117.2(5) . . ? N4 C28 H28A 108.3 . . ? C27 C28 H28A 108.1 . . ? N4 C28 H28B 107.5 . . ? C27 C28 H28B 107.8 . . ? H28A C28 H28B 107.6 . . ? N4 C29 C34 109.3(3) . . ? N4 C29 C30 129.8(4) . . ? C34 C29 C30 120.9(4) . . ? C31 C30 C29 118.8(4) . . ? C31 C30 H30A 120.7 . . ? C29 C30 H30A 120.5 . . ? C30 C31 C32 120.8(4) . . ? C30 C31 H31A 119.6 . . ? C32 C31 H31A 119.6 . . ? C31 C32 C33 122.1(5) . . ? C31 C32 H32A 119.4 . . ? C33 C32 H32A 118.5 . . ? C32 C33 C34 117.9(4) . . ? C32 C33 H33A 121.8 . . ? C34 C33 H33A 120.2 . . ? C29 C34 C33 119.4(4) . . ? C29 C34 C35 107.0(4) . . ? C33 C34 C35 133.5(4) . . ? C40 C35 C36 120.0(4) . . ? C40 C35 C34 106.9(3) . . ? C36 C35 C34 133.1(4) . . ? C37 C36 C35 117.9(4) . . ? C37 C36 H36A 121.5 . . ? C35 C36 H36A 120.6 . . ? C36 C37 C38 120.7(4) . . ? C36 C37 H37A 119.1 . . ? C38 C37 H37A 120.2 . . ? C39 C38 C37 122.1(5) . . ? C39 C38 H38A 119.6 . . ? C37 C38 H38A 118.3 . . ? C38 C39 C40 117.6(5) . . ? C38 C39 H39A 121.8 . . ? C40 C39 H39A 120.6 . . ? C39 C40 C35 121.7(4) . . ? C39 C40 N4 130.0(4) . . ? C35 C40 N4 108.2(4) . . ? C42 C41 C46 121.8(7) . . ? C42 C41 N5 130.8(5) . . ? C46 C41 N5 107.5(6) . . ? C43 C42 C41 116.5(6) . . ? C43 C42 H42A 123.0 . . ? C41 C42 H42A 120.5 . . ? C44 C43 C42 123.1(9) . . ? C44 C43 H43A 118.8 . . ? C42 C43 H43A 118.1 . . ? C43 C44 C45 121.9(9) . . ? C43 C44 H44A 119.7 . . ? C45 C44 H44A 118.4 . . ? C46 C45 C44 116.6(6) . . ? C46 C45 H45A 121.4 . . ? C44 C45 H45A 122.0 . . ? C45 C46 C41 120.0(7) . . ? C45 C46 C47 133.8(5) . . ? C41 C46 C47 106.0(6) . . ? C46 C47 C52 111.9(5) . . ? C46 C47 C48 139.0(7) . . ? C52 C47 C48 109.1(7) . . ? C49 C48 C47 125.2(7) . . ? C49 C48 H48A 119.4 . . ? C47 C48 H48A 115.4 . . ? C50 C49 C48 116.4(7) . . ? C50 C49 H49A 123.4 . . ? C48 C49 H49A 120.2 . . ? C51 C50 C49 125.1(10) . . ? C51 C50 H50A 118.8 . . ? C49 C50 H50A 116.1 . . ? C50 C51 C52 117.9(8) . . ? C50 C51 H51A 121.4 . . ? C52 C51 H51A 120.6 . . ? N5 C52 C51 130.2(6) . . ? N5 C52 C47 103.5(7) . . ? C51 C52 C47 126.3(6) . . ? N5 C53 C54 112.7(4) . . ? N5 C53 H53A 109.4 . . ? C54 C53 H53A 109.7 . . ? N5 C53 H53B 108.7 . . ? C54 C53 H53B 108.3 . . ? H53A C53 H53B 108.0 . . ? O4 C54 O5 129.5(4) . . ? O4 C54 C53 113.2(4) . . ? O5 C54 C53 117.4(4) . . ? N6 C55 C56 122.3(5) . . ? N6 C55 H55A 118.5 . . ? C56 C55 H55A 119.2 . . ? C57 C56 C55 120.1(5) . . ? C57 C56 H56A 120.0 . . ? C55 C56 H56A 119.9 . . ? C56 C57 C58 120.5(4) . . ? C56 C57 H57A 119.8 . . ? C58 C57 H57A 119.7 . . ? C66 C58 C57 115.9(4) . . ? C66 C58 C59 117.9(4) . . ? C57 C58 C59 126.2(4) . . ? C60 C59 C58 122.5(4) . . ? C60 C59 H59A 119.2 . . ? C58 C59 H59A 118.3 . . ? C59 C60 C61 121.0(5) . . ? C59 C60 H60A 119.8 . . ? C61 C60 H60A 119.2 . . ? C62 C61 C65 117.1(4) . . ? C62 C61 C60 125.8(5) . . ? C65 C61 C60 117.0(4) . . ? C63 C62 C61 120.0(4) . . ? C63 C62 H62A 120.4 . . ? C61 C62 H62A 119.6 . . ? C62 C63 C64 119.4(4) . . ? C62 C63 H63A 120.2 . . ? C64 C63 H63A 120.4 . . ? N7 C64 C63 122.4(3) . . ? N7 C64 H64A 118.7 . . ? C63 C64 H64A 118.9 . . ? N7 C65 C61 122.9(4) . . ? N7 C65 C66 116.6(4) . . ? C61 C65 C66 120.4(3) . . ? N6 C66 C58 122.9(4) . . ? N6 C66 C65 116.1(3) . . ? C58 C66 C65 120.9(4) . . ? O11 C67 C68 99.6(6) . . ? O11 C67 H67A 111.9 . . ? C68 C67 H67A 111.9 . . ? O11 C67 H67B 111.9 . . ? C68 C67 H67B 111.9 . . ? H67A C67 H67B 109.6 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C67 O11 H11B 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 O5 Cu1 O2 C14 52.1(4) . . . . ? N7 Cu1 O2 C14 -121.5(4) . . . . ? N6 Cu1 O2 C14 -48.2(7) . . . . ? O3 Cu1 O2 C14 141.9(4) . . . . ? O5 Cu1 O2 Cu2 -70.21(14) . . . . ? N7 Cu1 O2 Cu2 116.16(15) . . . . ? N6 Cu1 O2 Cu2 -170.5(5) . . . . ? O3 Cu1 O2 Cu2 19.55(11) . . . . ? O4 Cu2 O2 C14 -60.0(3) . . . . ? N3 Cu2 O2 C14 113.6(3) . . . . ? N2 Cu2 O2 C14 29.1(3) . . . . ? O3 Cu2 O2 C14 -152.5(3) . . . . ? O4 Cu2 O2 Cu1 70.12(12) . . . . ? N3 Cu2 O2 Cu1 -116.28(12) . . . . ? N2 Cu2 O2 Cu1 159.23(14) . . . . ? O3 Cu2 O2 Cu1 -22.33(12) . . . . ? O4 Cu2 O3 C27 76.4(3) . . . . ? N3 Cu2 O3 C27 -99.7(3) . . . . ? N2 Cu2 O3 C27 -19.9(6) . . . . ? O2 Cu2 O3 C27 164.4(3) . . . . ? O4 Cu2 O3 Cu1 -68.90(14) . . . . ? N3 Cu2 O3 Cu1 115.05(15) . . . . ? N2 Cu2 O3 Cu1 -165.1(4) . . . . ? O2 Cu2 O3 Cu1 19.11(10) . . . . ? O5 Cu1 O3 C27 -51.2(4) . . . . ? O2 Cu1 O3 C27 -142.5(4) . . . . ? N7 Cu1 O3 C27 125.1(4) . . . . ? N6 Cu1 O3 C27 40.2(4) . . . . ? O5 Cu1 O3 Cu2 68.57(12) . . . . ? O2 Cu1 O3 Cu2 -22.75(12) . . . . ? N7 Cu1 O3 Cu2 -115.16(12) . . . . ? N6 Cu1 O3 Cu2 159.99(13) . . . . ? N3 Cu2 O4 C54 -164.0(10) . . . . ? N2 Cu2 O4 C54 -153.9(5) . . . . ? O3 Cu2 O4 C54 45.0(4) . . . . ? O2 Cu2 O4 C54 -35.5(4) . . . . ? O2 Cu1 O5 C54 44.7(5) . . . . ? N7 Cu1 O5 C54 170.0(9) . . . . ? N6 Cu1 O5 C54 -149.8(5) . . . . ? O3 Cu1 O5 C54 -38.4(4) . . . . ? O4 Cu2 N2 C15 -0.5(5) . . . . ? N3 Cu2 N2 C15 178.1(5) . . . . ? O3 Cu2 N2 C15 96.1(6) . . . . ? O2 Cu2 N2 C15 -88.7(5) . . . . ? O4 Cu2 N2 C26 -178.9(4) . . . . ? N3 Cu2 N2 C26 -0.3(4) . . . . ? O3 Cu2 N2 C26 -82.3(6) . . . . ? O2 Cu2 N2 C26 92.9(4) . . . . ? O4 Cu2 N3 C24 -169.7(10) . . . . ? N2 Cu2 N3 C24 -179.9(5) . . . . ? O3 Cu2 N3 C24 -18.7(5) . . . . ? O2 Cu2 N3 C24 62.3(5) . . . . ? O4 Cu2 N3 C25 11.0(14) . . . . ? N2 Cu2 N3 C25 0.8(4) . . . . ? O3 Cu2 N3 C25 161.9(4) . . . . ? O2 Cu2 N3 C25 -117.0(3) . . . . ? O5 Cu1 N6 C55 5.0(5) . . . . ? O2 Cu1 N6 C55 105.4(7) . . . . ? N7 Cu1 N6 C55 180.0(5) . . . . ? O3 Cu1 N6 C55 -85.4(5) . . . . ? O5 Cu1 N6 C66 -171.0(4) . . . . ? O2 Cu1 N6 C66 -70.7(7) . . . . ? N7 Cu1 N6 C66 4.0(4) . . . . ? O3 Cu1 N6 C66 98.6(4) . . . . ? O5 Cu1 N7 C64 -138.9(10) . . . . ? O2 Cu1 N7 C64 -13.7(5) . . . . ? N6 Cu1 N7 C64 -179.5(5) . . . . ? O3 Cu1 N7 C64 69.8(5) . . . . ? O5 Cu1 N7 C65 36.1(13) . . . . ? O2 Cu1 N7 C65 161.3(4) . . . . ? N6 Cu1 N7 C65 -4.5(4) . . . . ? O3 Cu1 N7 C65 -115.2(3) . . . . ? C12 N1 C1 C2 178.1(6) . . . . ? C13 N1 C1 C2 -9.8(10) . . . . ? C12 N1 C1 C6 1.1(6) . . . . ? C13 N1 C1 C6 173.2(5) . . . . ? N1 C1 C2 C3 -178.5(6) . . . . ? C6 C1 C2 C3 -1.8(9) . . . . ? C1 C2 C3 C4 0.1(9) . . . . ? C2 C3 C4 C5 0.9(9) . . . . ? C3 C4 C5 C6 0.0(8) . . . . ? C4 C5 C6 C1 -1.7(8) . . . . ? C4 C5 C6 C7 178.5(6) . . . . ? C2 C1 C6 C5 2.7(8) . . . . ? N1 C1 C6 C5 -180.0(5) . . . . ? C2 C1 C6 C7 -177.4(5) . . . . ? N1 C1 C6 C7 -0.1(6) . . . . ? C5 C6 C7 C12 179.0(6) . . . . ? C1 C6 C7 C12 -0.9(6) . . . . ? C5 C6 C7 C8 -0.5(11) . . . . ? C1 C6 C7 C8 179.7(6) . . . . ? C12 C7 C8 C9 0.3(8) . . . . ? C6 C7 C8 C9 179.6(6) . . . . ? C7 C8 C9 C10 -1.6(10) . . . . ? C8 C9 C10 C11 1.2(11) . . . . ? C9 C10 C11 C12 0.5(10) . . . . ? C8 C7 C12 C11 1.6(9) . . . . ? C6 C7 C12 C11 -177.9(5) . . . . ? C8 C7 C12 N1 -179.0(5) . . . . ? C6 C7 C12 N1 1.5(6) . . . . ? C10 C11 C12 C7 -1.9(9) . . . . ? C10 C11 C12 N1 178.7(6) . . . . ? C1 N1 C12 C7 -1.6(6) . . . . ? C13 N1 C12 C7 -173.6(5) . . . . ? C1 N1 C12 C11 177.8(6) . . . . ? C13 N1 C12 C11 5.8(10) . . . . ? C1 N1 C13 C14 78.6(7) . . . . ? C12 N1 C13 C14 -110.6(6) . . . . ? Cu1 O2 C14 O1 -130.2(4) . . . . ? Cu2 O2 C14 O1 -17.1(6) . . . . ? Cu1 O2 C14 C13 49.6(6) . . . . ? Cu2 O2 C14 C13 162.7(4) . . . . ? N1 C13 C14 O1 -166.4(5) . . . . ? N1 C13 C14 O2 13.9(7) . . . . ? C26 N2 C15 C16 -2.0(9) . . . . ? Cu2 N2 C15 C16 179.7(5) . . . . ? N2 C15 C16 C17 3.2(10) . . . . ? C15 C16 C17 C18 -3.8(11) . . . . ? C16 C17 C18 C26 3.0(9) . . . . ? C16 C17 C18 C19 -179.6(6) . . . . ? C17 C18 C19 C20 -178.0(7) . . . . ? C26 C18 C19 C20 -0.6(9) . . . . ? C18 C19 C20 C21 0.2(11) . . . . ? C19 C20 C21 C22 178.2(7) . . . . ? C19 C20 C21 C25 0.2(10) . . . . ? C25 C21 C22 C23 -2.0(9) . . . . ? C20 C21 C22 C23 179.9(6) . . . . ? C21 C22 C23 C24 2.4(10) . . . . ? C25 N3 C24 C23 0.0(8) . . . . ? Cu2 N3 C24 C23 -179.3(4) . . . . ? C22 C23 C24 N3 -1.4(10) . . . . ? C24 N3 C25 C21 0.4(8) . . . . ? Cu2 N3 C25 C21 179.8(4) . . . . ? C24 N3 C25 C26 179.5(5) . . . . ? Cu2 N3 C25 C26 -1.1(6) . . . . ? C22 C21 C25 N3 0.6(9) . . . . ? C20 C21 C25 N3 178.9(5) . . . . ? C22 C21 C25 C26 -178.5(5) . . . . ? C20 C21 C25 C26 -0.2(8) . . . . ? C15 N2 C26 C18 1.4(8) . . . . ? Cu2 N2 C26 C18 180.0(4) . . . . ? C15 N2 C26 C25 -178.7(5) . . . . ? Cu2 N2 C26 C25 -0.1(6) . . . . ? C17 C18 C26 N2 -1.9(8) . . . . ? C19 C18 C26 N2 -179.6(5) . . . . ? C17 C18 C26 C25 178.2(5) . . . . ? C19 C18 C26 C25 0.5(8) . . . . ? N3 C25 C26 N2 0.8(7) . . . . ? C21 C25 C26 N2 179.9(5) . . . . ? N3 C25 C26 C18 -179.3(5) . . . . ? C21 C25 C26 C18 -0.2(8) . . . . ? Cu2 O3 C27 O6 7.2(6) . . . . ? Cu1 O3 C27 O6 123.6(4) . . . . ? Cu2 O3 C27 C28 -177.2(4) . . . . ? Cu1 O3 C27 C28 -60.7(7) . . . . ? C29 N4 C28 C27 -69.7(7) . . . . ? C40 N4 C28 C27 131.5(5) . . . . ? O3 C27 C28 N4 -2.2(8) . . . . ? O6 C27 C28 N4 173.9(5) . . . . ? C40 N4 C29 C34 -4.3(6) . . . . ? C28 N4 C29 C34 -165.8(5) . . . . ? C40 N4 C29 C30 176.6(6) . . . . ? C28 N4 C29 C30 15.1(9) . . . . ? N4 C29 C30 C31 178.4(6) . . . . ? C34 C29 C30 C31 -0.6(9) . . . . ? C29 C30 C31 C32 -1.4(9) . . . . ? C30 C31 C32 C33 3.4(10) . . . . ? C31 C32 C33 C34 -3.2(9) . . . . ? N4 C29 C34 C33 -178.6(5) . . . . ? C30 C29 C34 C33 0.6(8) . . . . ? N4 C29 C34 C35 4.8(6) . . . . ? C30 C29 C34 C35 -176.0(5) . . . . ? C32 C33 C34 C29 1.2(8) . . . . ? C32 C33 C34 C35 176.9(6) . . . . ? C29 C34 C35 C40 -3.4(6) . . . . ? C33 C34 C35 C40 -179.4(6) . . . . ? C29 C34 C35 C36 177.4(6) . . . . ? C33 C34 C35 C36 1.4(11) . . . . ? C40 C35 C36 C37 0.4(8) . . . . ? C34 C35 C36 C37 179.4(6) . . . . ? C35 C36 C37 C38 0.2(9) . . . . ? C36 C37 C38 C39 0.1(10) . . . . ? C37 C38 C39 C40 -0.9(10) . . . . ? C38 C39 C40 C35 1.5(9) . . . . ? C38 C39 C40 N4 179.8(6) . . . . ? C36 C35 C40 C39 -1.3(8) . . . . ? C34 C35 C40 C39 179.4(5) . . . . ? C36 C35 C40 N4 -179.8(5) . . . . ? C34 C35 C40 N4 0.9(6) . . . . ? C29 N4 C40 C39 -176.3(6) . . . . ? C28 N4 C40 C39 -14.6(9) . . . . ? C29 N4 C40 C35 2.1(6) . . . . ? C28 N4 C40 C35 163.8(5) . . . . ? C52 N5 C41 C42 176.6(5) . . . . ? C53 N5 C41 C42 12.6(8) . . . . ? C52 N5 C41 C46 -4.0(6) . . . . ? C53 N5 C41 C46 -168.0(4) . . . . ? C46 C41 C42 C43 -0.7(8) . . . . ? N5 C41 C42 C43 178.7(5) . . . . ? C41 C42 C43 C44 0.1(9) . . . . ? C42 C43 C44 C45 1.0(11) . . . . ? C43 C44 C45 C46 -1.5(10) . . . . ? C44 C45 C46 C41 0.9(8) . . . . ? C44 C45 C46 C47 177.2(6) . . . . ? C42 C41 C46 C45 0.1(8) . . . . ? N5 C41 C46 C45 -179.3(5) . . . . ? C42 C41 C46 C47 -177.1(5) . . . . ? N5 C41 C46 C47 3.5(6) . . . . ? C45 C46 C47 C52 -178.5(6) . . . . ? C41 C46 C47 C52 -1.9(6) . . . . ? C45 C46 C47 C48 1.4(12) . . . . ? C41 C46 C47 C48 178.1(6) . . . . ? C46 C47 C48 C49 -177.1(7) . . . . ? C52 C47 C48 C49 2.9(8) . . . . ? C47 C48 C49 C50 -2.1(10) . . . . ? C48 C49 C50 C51 0.3(11) . . . . ? C49 C50 C51 C52 0.2(10) . . . . ? C53 N5 C52 C51 -12.0(9) . . . . ? C41 N5 C52 C51 -175.4(5) . . . . ? C53 N5 C52 C47 166.1(5) . . . . ? C41 N5 C52 C47 2.7(5) . . . . ? C50 C51 C52 N5 178.7(5) . . . . ? C50 C51 C52 C47 1.0(9) . . . . ? C46 C47 C52 N5 -0.5(6) . . . . ? C48 C47 C52 N5 179.5(4) . . . . ? C46 C47 C52 C51 177.7(5) . . . . ? C48 C47 C52 C51 -2.3(7) . . . . ? C52 N5 C53 C54 -76.6(8) . . . . ? C41 N5 C53 C54 85.0(7) . . . . ? Cu2 O4 C54 O5 -2.6(9) . . . . ? Cu2 O4 C54 C53 176.8(4) . . . . ? Cu1 O5 C54 O4 2.2(9) . . . . ? Cu1 O5 C54 C53 -177.1(4) . . . . ? N5 C53 C54 O4 165.2(6) . . . . ? N5 C53 C54 O5 -15.3(9) . . . . ? C66 N6 C55 C56 2.3(8) . . . . ? Cu1 N6 C55 C56 -173.5(5) . . . . ? N6 C55 C56 C57 -1.3(10) . . . . ? C55 C56 C57 C58 -0.1(10) . . . . ? C56 C57 C58 C66 0.4(9) . . . . ? C56 C57 C58 C59 -179.9(6) . . . . ? C66 C58 C59 C60 1.8(10) . . . . ? C57 C58 C59 C60 -177.9(7) . . . . ? C58 C59 C60 C61 -3.4(11) . . . . ? C59 C60 C61 C62 -178.3(7) . . . . ? C59 C60 C61 C65 4.9(10) . . . . ? C65 C61 C62 C63 0.8(9) . . . . ? C60 C61 C62 C63 -176.0(6) . . . . ? C61 C62 C63 C64 0.3(9) . . . . ? C65 N7 C64 C63 3.3(8) . . . . ? Cu1 N7 C64 C63 178.0(4) . . . . ? C62 C63 C64 N7 -2.4(9) . . . . ? C64 N7 C65 C61 -2.1(8) . . . . ? Cu1 N7 C65 C61 -177.7(4) . . . . ? C64 N7 C65 C66 179.9(5) . . . . ? Cu1 N7 C65 C66 4.3(6) . . . . ? C62 C61 C65 N7 0.1(8) . . . . ? C60 C61 C65 N7 177.2(5) . . . . ? C62 C61 C65 C66 178.0(5) . . . . ? C60 C61 C65 C66 -4.9(8) . . . . ? C55 N6 C66 C58 -2.0(8) . . . . ? Cu1 N6 C66 C58 174.5(4) . . . . ? C55 N6 C66 C65 -179.4(5) . . . . ? Cu1 N6 C66 C65 -2.8(6) . . . . ? C57 C58 C66 N6 0.7(8) . . . . ? C59 C58 C66 N6 -179.1(5) . . . . ? C57 C58 C66 C65 177.9(5) . . . . ? C59 C58 C66 C65 -1.8(8) . . . . ? N7 C65 C66 N6 -0.9(7) . . . . ? C61 C65 C66 N6 -179.0(5) . . . . ? N7 C65 C66 C58 -178.4(5) . . . . ? C61 C65 C66 C58 3.6(8) . . . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 28.45 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 1.472 _refine_diff_density_min -1.643 _refine_diff_density_rms 0.186 data_tian34m _database_code_CSD 181847 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C50 H40 Cu N O2 P2' _chemical_formula_weight 812.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2055(1) _cell_length_b 13.5557(2) _cell_length_c 14.4757(1) _cell_angle_alpha 111.532(1) _cell_angle_beta 92.833(1) _cell_angle_gamma 109.639(1) _cell_volume 2057.11(4) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 1.54 _cell_measurement_theta_max 29.50 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.311 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 844 _exptl_absorpt_coefficient_mu 0.650 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.7370 _exptl_absorpt_correction_T_max 0.9145 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1996)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Siemens SMART CCD area detector diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 8.33 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% negligible _diffrn_reflns_number 13175 _diffrn_reflns_av_R_equivalents 0.0972 _diffrn_reflns_av_sigmaI/netI 0.1719 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 26.50 _reflns_number_total 8338 _reflns_number_gt 4699 _reflns_threshold_expression 'I > 2\s(I)' _computing_data_collection 'SMART (Siemens, 1996)' _computing_cell_refinement 'SAINT (Siemens, 1996)' _computing_data_reduction SAINT _computing_structure_solution 'SHELXTL (Sheldrick, 1997)' _computing_structure_refinement SHELXTL _computing_molecular_graphics SHELXTL _computing_publication_material ; SHELXTL, PARST (Nardelli, 1995) and PLATON (Spek, 1990) ; _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0569P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.035(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 8338 _refine_ls_number_parameters 506 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1052 _refine_ls_R_factor_gt 0.0698 _refine_ls_wR_factor_ref 0.1866 _refine_ls_wR_factor_gt 0.1657 _refine_ls_goodness_of_fit_ref 0.871 _refine_ls_restrained_S_all 0.871 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu -0.15241(5) -0.07519(4) -0.27473(4) 0.0385(2) Uani 1 1 d . . . P1 P -0.27869(10) -0.02159(9) -0.34214(8) 0.0365(3) Uani 1 1 d . . . P2 P -0.13487(10) -0.24634(9) -0.32869(8) 0.0356(3) Uani 1 1 d . . . O1 O 0.0271(3) 0.0621(2) -0.19752(19) 0.0439(7) Uani 1 1 d . . . O2 O -0.1068(2) 0.0101(2) -0.1092(2) 0.0432(7) Uani 1 1 d . . . N1 N 0.1954(3) 0.2192(3) -0.0238(2) 0.0358(8) Uani 1 1 d . . . C1 C -0.4331(4) -0.0982(4) -0.3414(3) 0.0411(10) Uani 1 1 d . . . C2 C -0.4610(5) -0.1912(5) -0.3188(5) 0.0808(19) Uani 1 1 d . . . H2A H -0.3999 -0.2128 -0.3038 0.097 Uiso 1 1 calc R . . C3 C -0.5754(6) -0.2559(6) -0.3168(6) 0.104(3) Uani 1 1 d . . . H3A H -0.5910 -0.3166 -0.2973 0.125 Uiso 1 1 calc R . . C4 C -0.6651(5) -0.2261(6) -0.3450(5) 0.087(2) Uani 1 1 d . . . H4A H -0.7433 -0.2688 -0.3465 0.104 Uiso 1 1 calc R . . C5 C -0.6411(6) -0.1369(7) -0.3701(6) 0.096(2) Uani 1 1 d . . . H5A H -0.7024 -0.1184 -0.3901 0.115 Uiso 1 1 calc R . . C6 C -0.5260(5) -0.0727(6) -0.3664(5) 0.084(2) Uani 1 1 d . . . H6A H -0.5106 -0.0090 -0.3816 0.101 Uiso 1 1 calc R . . C7 C -0.2710(4) -0.0479(3) -0.4756(3) 0.0358(9) Uani 1 1 d . . . C8 C -0.3643(4) -0.1290(4) -0.5552(3) 0.0456(11) Uani 1 1 d . . . H8A H -0.4370 -0.1668 -0.5424 0.055 Uiso 1 1 calc R . . C9 C -0.3477(5) -0.1528(4) -0.6535(3) 0.0582(13) Uani 1 1 d . . . H9A H -0.4096 -0.2072 -0.7070 0.070 Uiso 1 1 calc R . . C10 C -0.2410(5) -0.0973(4) -0.6731(4) 0.0607(14) Uani 1 1 d . . . H10A H -0.2308 -0.1129 -0.7395 0.073 Uiso 1 1 calc R . . C11 C -0.1492(5) -0.0181(4) -0.5933(4) 0.0543(12) Uani 1 1 d . . . H11A H -0.0761 0.0191 -0.6061 0.065 Uiso 1 1 calc R . . C12 C -0.1644(4) 0.0063(4) -0.4958(3) 0.0504(12) Uani 1 1 d . . . H12A H -0.1017 0.0603 -0.4426 0.060 Uiso 1 1 calc R . . C13 C -0.2600(4) 0.1300(3) -0.2850(3) 0.0379(9) Uani 1 1 d . . . C14 C -0.2935(5) 0.1838(4) -0.3412(4) 0.0588(13) Uani 1 1 d . . . H14A H -0.3222 0.1438 -0.4107 0.071 Uiso 1 1 calc R . . C15 C -0.2841(5) 0.2966(4) -0.2936(4) 0.0635(14) Uani 1 1 d . . . H15A H -0.3075 0.3320 -0.3306 0.076 Uiso 1 1 calc R . . C16 C -0.2395(5) 0.3557(4) -0.1907(5) 0.0657(15) Uani 1 1 d . . . H16A H -0.2336 0.4310 -0.1584 0.079 Uiso 1 1 calc R . . C17 C -0.2034(5) 0.3042(4) -0.1349(4) 0.0646(15) Uani 1 1 d . . . H17A H -0.1718 0.3455 -0.0660 0.078 Uiso 1 1 calc R . . C18 C -0.2147(4) 0.1912(4) -0.1821(3) 0.0506(12) Uani 1 1 d . . . H18A H -0.1916 0.1562 -0.1445 0.061 Uiso 1 1 calc R . . C19 C -0.2694(4) -0.3616(4) -0.3361(3) 0.0414(10) Uani 1 1 d . . . C20 C -0.3166(5) -0.3446(4) -0.2509(4) 0.0571(13) Uani 1 1 d . . . H20A H -0.2790 -0.2757 -0.1945 0.069 Uiso 1 1 calc R . . C21 C -0.4194(6) -0.4264(5) -0.2448(5) 0.0810(18) Uani 1 1 d . . . H21A H -0.4481 -0.4143 -0.1849 0.097 Uiso 1 1 calc R . . C22 C -0.4764(5) -0.5251(5) -0.3305(6) 0.084(2) Uani 1 1 d . . . H22A H -0.5471 -0.5795 -0.3300 0.100 Uiso 1 1 calc R . . C23 C -0.4305(6) -0.5444(5) -0.4160(5) 0.0797(18) Uani 1 1 d . . . H23A H -0.4685 -0.6129 -0.4728 0.096 Uiso 1 1 calc R . . C24 C -0.3279(5) -0.4631(4) -0.4194(4) 0.0575(13) Uani 1 1 d . . . H24A H -0.2979 -0.4770 -0.4787 0.069 Uiso 1 1 calc R . . C25 C -0.0942(4) -0.2929(3) -0.4538(3) 0.0385(10) Uani 1 1 d . . . C26 C -0.1432(5) -0.2700(4) -0.5261(4) 0.0622(14) Uani 1 1 d . . . H26A H -0.1993 -0.2368 -0.5126 0.075 Uiso 1 1 calc R . . C27 C -0.1101(6) -0.2961(5) -0.6205(4) 0.0733(17) Uani 1 1 d . . . H27A H -0.1444 -0.2810 -0.6699 0.088 Uiso 1 1 calc R . . C28 C -0.0273(6) -0.3439(5) -0.6396(4) 0.0804(18) Uani 1 1 d . . . H28A H -0.0031 -0.3594 -0.7015 0.096 Uiso 1 1 calc R . . C29 C 0.0213(6) -0.3697(6) -0.5666(5) 0.090(2) Uani 1 1 d . . . H29A H 0.0756 -0.4051 -0.5798 0.108 Uiso 1 1 calc R . . C30 C -0.0127(5) -0.3419(5) -0.4761(4) 0.0656(15) Uani 1 1 d . . . H30A H 0.0213 -0.3571 -0.4265 0.079 Uiso 1 1 calc R . . C31 C -0.0254(4) -0.2608(3) -0.2494(3) 0.0391(10) Uani 1 1 d . . . C32 C -0.0482(5) -0.3588(4) -0.2308(4) 0.0563(13) Uani 1 1 d . . . H32A H -0.1217 -0.4190 -0.2592 0.068 Uiso 1 1 calc R . . C33 C 0.0366(6) -0.3687(5) -0.1708(4) 0.0759(18) Uani 1 1 d . . . H33A H 0.0194 -0.4338 -0.1575 0.091 Uiso 1 1 calc R . . C34 C 0.1461(5) -0.2809(5) -0.1316(4) 0.0745(17) Uani 1 1 d . . . H34A H 0.2043 -0.2869 -0.0923 0.089 Uiso 1 1 calc R . . C35 C 0.1699(5) -0.1833(5) -0.1506(4) 0.0654(15) Uani 1 1 d . . . H35A H 0.2445 -0.1245 -0.1243 0.078 Uiso 1 1 calc R . . C36 C 0.0840(4) -0.1720(4) -0.2083(3) 0.0477(11) Uani 1 1 d . . . H36A H 0.1002 -0.1054 -0.2190 0.057 Uiso 1 1 calc R . . C37 C -0.0053(3) 0.0688(3) -0.1148(3) 0.0316(9) Uani 1 1 d . . . C38 C 0.0797(3) 0.1509(3) -0.0145(3) 0.0372(9) Uani 1 1 d . . . H38A H 0.0438 0.2022 0.0251 0.045 Uiso 1 1 calc R . . H38B H 0.0901 0.1069 0.0226 0.045 Uiso 1 1 calc R . . C39 C 0.2959(3) 0.1943(3) -0.0218(3) 0.0355(9) Uani 1 1 d . . . C40 C 0.3159(4) 0.1147(4) 0.0076(4) 0.0493(11) Uani 1 1 d . . . H40A H 0.2571 0.0671 0.0279 0.059 Uiso 1 1 calc R . . C41 C 0.4258(5) 0.1087(5) 0.0058(5) 0.0767(18) Uani 1 1 d . . . H41A H 0.4417 0.0567 0.0264 0.092 Uiso 1 1 calc R . . C42 C 0.5130(5) 0.1768(5) -0.0253(5) 0.0766(17) Uani 1 1 d . . . H42A H 0.5863 0.1699 -0.0252 0.092 Uiso 1 1 calc R . . C43 C 0.4942(4) 0.2560(5) -0.0569(4) 0.0717(17) Uani 1 1 d . . . H43A H 0.5526 0.2997 -0.0805 0.086 Uiso 1 1 calc R . . C44 C 0.3837(4) 0.2684(4) -0.0522(3) 0.0469(11) Uani 1 1 d . . . C45 C 0.3335(4) 0.3407(3) -0.0744(3) 0.0443(11) Uani 1 1 d . . . C46 C 0.3763(6) 0.4289(4) -0.1033(4) 0.0699(16) Uani 1 1 d . . . H46A H 0.4546 0.4541 -0.1114 0.084 Uiso 1 1 calc R . . C47 C 0.3026(7) 0.4804(5) -0.1204(5) 0.087(2) Uani 1 1 d . . . H47A H 0.3294 0.5379 -0.1439 0.105 Uiso 1 1 calc R . . C48 C 0.1869(7) 0.4461(5) -0.1023(4) 0.082(2) Uani 1 1 d . . . H48A H 0.1395 0.4847 -0.1105 0.099 Uiso 1 1 calc R . . C49 C 0.1416(5) 0.3586(4) -0.0733(3) 0.0572(13) Uani 1 1 d . . . H49A H 0.0637 0.3342 -0.0640 0.069 Uiso 1 1 calc R . . C50 C 0.2177(4) 0.3076(3) -0.0583(3) 0.0431(11) Uani 1 1 d . . . 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 0.0425(3) 0.0386(3) 0.0313(3) 0.0093(2) 0.0023(2) 0.0181(3) P1 0.0394(6) 0.0420(6) 0.0313(5) 0.0152(5) 0.0078(4) 0.0188(5) P2 0.0408(6) 0.0347(6) 0.0301(5) 0.0110(4) 0.0056(5) 0.0158(5) O1 0.0431(17) 0.0481(17) 0.0296(15) 0.0120(13) 0.0115(13) 0.0083(15) O2 0.0342(17) 0.0517(17) 0.0398(16) 0.0231(14) 0.0086(13) 0.0067(15) N1 0.034(2) 0.0360(18) 0.0326(18) 0.0154(15) 0.0076(15) 0.0067(16) C1 0.045(3) 0.054(3) 0.034(2) 0.023(2) 0.0159(19) 0.024(2) C2 0.047(3) 0.089(4) 0.137(6) 0.071(4) 0.030(3) 0.034(3) C3 0.059(4) 0.103(5) 0.186(8) 0.094(6) 0.047(5) 0.032(4) C4 0.043(3) 0.099(5) 0.115(5) 0.045(4) 0.034(3) 0.019(3) C5 0.059(4) 0.139(6) 0.140(6) 0.094(6) 0.043(4) 0.055(4) C6 0.051(4) 0.105(5) 0.146(6) 0.093(5) 0.035(4) 0.039(3) C7 0.041(2) 0.041(2) 0.031(2) 0.0175(18) 0.0113(18) 0.019(2) C8 0.051(3) 0.051(3) 0.035(2) 0.023(2) 0.015(2) 0.013(2) C9 0.064(3) 0.064(3) 0.031(2) 0.011(2) 0.003(2) 0.016(3) C10 0.069(4) 0.067(3) 0.042(3) 0.019(2) 0.021(3) 0.024(3) C11 0.054(3) 0.062(3) 0.052(3) 0.028(3) 0.025(2) 0.021(3) C12 0.044(3) 0.054(3) 0.046(3) 0.018(2) 0.007(2) 0.013(2) C13 0.041(2) 0.040(2) 0.038(2) 0.0178(19) 0.0143(19) 0.019(2) C14 0.064(3) 0.051(3) 0.064(3) 0.023(3) 0.007(3) 0.026(3) C15 0.077(4) 0.055(3) 0.078(4) 0.037(3) 0.026(3) 0.035(3) C16 0.069(4) 0.040(3) 0.093(4) 0.022(3) 0.039(3) 0.029(3) C17 0.085(4) 0.054(3) 0.046(3) 0.003(2) 0.012(3) 0.036(3) C18 0.063(3) 0.045(3) 0.045(3) 0.014(2) 0.010(2) 0.027(2) C19 0.046(3) 0.040(2) 0.045(2) 0.023(2) 0.009(2) 0.017(2) C20 0.064(3) 0.053(3) 0.053(3) 0.028(2) 0.019(3) 0.012(3) C21 0.073(4) 0.080(4) 0.107(5) 0.057(4) 0.039(4) 0.024(4) C22 0.054(4) 0.071(4) 0.124(6) 0.056(4) 0.011(4) 0.006(3) C23 0.077(4) 0.058(3) 0.081(4) 0.030(3) -0.004(4) 0.001(3) C24 0.061(3) 0.054(3) 0.048(3) 0.019(2) 0.009(2) 0.012(3) C25 0.046(3) 0.040(2) 0.031(2) 0.0137(18) 0.0102(18) 0.018(2) C26 0.079(4) 0.063(3) 0.044(3) 0.008(2) 0.009(3) 0.043(3) C27 0.118(5) 0.078(4) 0.029(3) 0.013(2) 0.009(3) 0.055(4) C28 0.106(5) 0.095(4) 0.038(3) 0.016(3) 0.026(3) 0.048(4) C29 0.098(5) 0.117(5) 0.065(4) 0.018(4) 0.031(4) 0.071(4) C30 0.080(4) 0.095(4) 0.045(3) 0.030(3) 0.022(3) 0.058(3) C31 0.046(3) 0.042(2) 0.033(2) 0.0137(18) 0.0071(19) 0.022(2) C32 0.062(3) 0.047(3) 0.060(3) 0.021(2) -0.003(3) 0.025(3) C33 0.085(4) 0.067(4) 0.079(4) 0.027(3) -0.012(3) 0.039(3) C34 0.079(4) 0.080(4) 0.068(4) 0.015(3) -0.010(3) 0.055(4) C35 0.051(3) 0.068(3) 0.060(3) 0.005(3) -0.004(2) 0.029(3) C36 0.047(3) 0.046(3) 0.048(3) 0.013(2) 0.006(2) 0.022(2) C37 0.034(2) 0.032(2) 0.032(2) 0.0155(17) 0.0094(17) 0.0131(19) C38 0.033(2) 0.044(2) 0.031(2) 0.0153(18) 0.0102(17) 0.0106(19) C39 0.030(2) 0.037(2) 0.029(2) 0.0106(18) 0.0051(17) 0.0045(18) C40 0.042(3) 0.042(2) 0.063(3) 0.022(2) 0.012(2) 0.013(2) C41 0.052(4) 0.067(4) 0.110(5) 0.031(4) 0.007(3) 0.028(3) C42 0.046(3) 0.085(4) 0.103(5) 0.042(4) 0.023(3) 0.027(3) C43 0.032(3) 0.069(3) 0.080(4) 0.012(3) 0.018(3) -0.002(3) C44 0.035(2) 0.044(2) 0.040(2) 0.008(2) 0.007(2) 0.000(2) C45 0.050(3) 0.033(2) 0.030(2) 0.0117(18) 0.0038(19) -0.005(2) C46 0.077(4) 0.056(3) 0.061(3) 0.030(3) 0.006(3) 0.003(3) C47 0.121(6) 0.048(3) 0.069(4) 0.026(3) -0.005(4) 0.005(4) C48 0.124(6) 0.050(3) 0.060(4) 0.008(3) -0.023(4) 0.039(4) C49 0.074(4) 0.046(3) 0.047(3) 0.014(2) -0.006(2) 0.023(3) C50 0.053(3) 0.032(2) 0.030(2) 0.0064(18) 0.000(2) 0.007(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 O2 2.189(3) . ? Cu1 P1 2.2317(11) . ? Cu1 O1 2.237(3) . ? Cu1 P2 2.2492(11) . ? Cu1 C37 2.512(4) . ? P1 C1 1.823(5) . ? P1 C13 1.837(4) . ? P1 C7 1.845(4) . ? P2 C19 1.812(4) . ? P2 C31 1.826(4) . ? P2 C25 1.840(4) . ? O1 C37 1.261(4) . ? O2 C37 1.253(4) . ? N1 C39 1.380(5) . ? N1 C50 1.411(5) . ? N1 C38 1.450(5) . ? C1 C2 1.356(7) . ? C1 C6 1.361(7) . ? C2 C3 1.385(8) . ? C2 H2A 0.9300 . ? C3 C4 1.379(9) . ? C3 H3A 0.9300 . ? C4 C5 1.332(8) . ? C4 H4A 0.9300 . ? C5 C6 1.367(8) . ? C5 H5A 0.9300 . ? C6 H6A 0.9300 . ? C7 C12 1.369(6) . ? C7 C8 1.390(6) . ? C8 C9 1.380(6) . ? C8 H8A 0.9300 . ? C9 C10 1.370(7) . ? C9 H9A 0.9300 . ? C10 C11 1.377(7) . ? C10 H10A 0.9300 . ? C11 C12 1.364(6) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C18 1.383(6) . ? C13 C14 1.402(6) . ? C14 C15 1.388(7) . ? C14 H14A 0.9300 . ? C15 C16 1.382(7) . ? C15 H15A 0.9300 . ? C16 C17 1.383(7) . ? C16 H16A 0.9300 . ? C17 C18 1.383(6) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 C20 1.362(6) . ? C19 C24 1.376(6) . ? C20 C21 1.400(7) . ? C20 H20A 0.9300 . ? C21 C22 1.372(9) . ? C21 H21A 0.9300 . ? C22 C23 1.358(9) . ? C22 H22A 0.9300 . ? C23 C24 1.379(7) . ? C23 H23A 0.9300 . ? C24 H24A 0.9300 . ? C25 C26 1.360(6) . ? C25 C30 1.363(6) . ? C26 C27 1.396(7) . ? C26 H26A 0.9300 . ? C27 C28 1.362(8) . ? C27 H27A 0.9300 . ? C28 C29 1.391(8) . ? C28 H28A 0.9300 . ? C29 C30 1.352(7) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? C31 C36 1.379(6) . ? C31 C32 1.391(6) . ? C32 C33 1.390(7) . ? C32 H32A 0.9300 . ? C33 C34 1.373(8) . ? C33 H33A 0.9300 . ? C34 C35 1.389(7) . ? C34 H34A 0.9300 . ? C35 C36 1.391(6) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? C37 C38 1.520(5) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.381(6) . ? C39 C44 1.413(6) . ? C40 C41 1.373(7) . ? C40 H40A 0.9300 . ? C41 C42 1.370(8) . ? C41 H41A 0.9300 . ? C42 C43 1.389(8) . ? C42 H42A 0.9300 . ? C43 C44 1.415(7) . ? C43 H43A 0.9300 . ? C44 C45 1.435(7) . ? C45 C46 1.359(6) . ? C45 C50 1.392(6) . ? C46 C47 1.372(9) . ? C46 H46A 0.9300 . ? C47 C48 1.402(9) . ? C47 H47A 0.9300 . ? C48 C49 1.355(7) . ? C48 H48A 0.9300 . ? C49 C50 1.382(6) . ? C49 H49A 0.9300 . ? 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 O2 Cu1 P1 113.03(9) . . ? O2 Cu1 O1 59.99(10) . . ? P1 Cu1 O1 115.24(8) . . ? O2 Cu1 P2 110.38(8) . . ? P1 Cu1 P2 129.30(4) . . ? O1 Cu1 P2 108.40(8) . . ? O2 Cu1 C37 29.91(11) . . ? P1 Cu1 C37 118.68(9) . . ? O1 Cu1 C37 30.09(11) . . ? P2 Cu1 C37 112.01(9) . . ? C1 P1 C13 103.65(19) . . ? C1 P1 C7 106.12(19) . . ? C13 P1 C7 103.04(18) . . ? C1 P1 Cu1 113.10(14) . . ? C13 P1 Cu1 118.09(14) . . ? C7 P1 Cu1 111.65(13) . . ? C19 P2 C31 101.63(19) . . ? C19 P2 C25 106.23(19) . . ? C31 P2 C25 102.89(19) . . ? C19 P2 Cu1 112.91(15) . . ? C31 P2 Cu1 116.96(13) . . ? C25 P2 Cu1 114.74(13) . . ? C37 O1 Cu1 87.1(2) . . ? C37 O2 Cu1 89.5(2) . . ? C39 N1 C50 107.7(3) . . ? C39 N1 C38 126.0(3) . . ? C50 N1 C38 124.9(4) . . ? C2 C1 C6 115.9(5) . . ? C2 C1 P1 119.0(4) . . ? C6 C1 P1 125.1(4) . . ? C1 C2 C3 123.6(5) . . ? C1 C2 H2A 118.2 . . ? C3 C2 H2A 118.2 . . ? C4 C3 C2 117.0(6) . . ? C4 C3 H3A 121.5 . . ? C2 C3 H3A 121.5 . . ? C5 C4 C3 120.9(6) . . ? C5 C4 H4A 119.6 . . ? C3 C4 H4A 119.6 . . ? C4 C5 C6 119.7(6) . . ? C4 C5 H5A 120.1 . . ? C6 C5 H5A 120.1 . . ? C1 C6 C5 122.8(5) . . ? C1 C6 H6A 118.6 . . ? C5 C6 H6A 118.6 . . ? C12 C7 C8 119.6(4) . . ? C12 C7 P1 117.5(3) . . ? C8 C7 P1 122.5(3) . . ? C9 C8 C7 119.2(4) . . ? C9 C8 H8A 120.4 . . ? C7 C8 H8A 120.4 . . ? C10 C9 C8 120.9(4) . . ? C10 C9 H9A 119.6 . . ? C8 C9 H9A 119.6 . . ? C9 C10 C11 119.2(5) . . ? C9 C10 H10A 120.4 . . ? C11 C10 H10A 120.4 . . ? C12 C11 C10 120.6(5) . . ? C12 C11 H11A 119.7 . . ? C10 C11 H11A 119.7 . . ? C11 C12 C7 120.5(4) . . ? C11 C12 H12A 119.7 . . ? C7 C12 H12A 119.7 . . ? C18 C13 C14 119.4(4) . . ? C18 C13 P1 118.3(3) . . ? C14 C13 P1 122.3(3) . . ? C15 C14 C13 120.3(5) . . ? C15 C14 H14A 119.9 . . ? C13 C14 H14A 119.9 . . ? C16 C15 C14 119.2(5) . . ? C16 C15 H15A 120.4 . . ? C14 C15 H15A 120.4 . . ? C15 C16 C17 120.9(4) . . ? C15 C16 H16A 119.5 . . ? C17 C16 H16A 119.5 . . ? C16 C17 C18 119.8(5) . . ? C16 C17 H17A 120.1 . . ? C18 C17 H17A 120.1 . . ? C13 C18 C17 120.4(4) . . ? C13 C18 H18A 119.8 . . ? C17 C18 H18A 119.8 . . ? C20 C19 C24 117.6(4) . . ? C20 C19 P2 116.3(3) . . ? C24 C19 P2 126.1(4) . . ? C19 C20 C21 122.8(5) . . ? C19 C20 H20A 118.6 . . ? C21 C20 H20A 118.6 . . ? C22 C21 C20 117.5(6) . . ? C22 C21 H21A 121.2 . . ? C20 C21 H21A 121.2 . . ? C23 C22 C21 120.7(6) . . ? C23 C22 H22A 119.6 . . ? C21 C22 H22A 119.6 . . ? C22 C23 C24 120.4(6) . . ? C22 C23 H23A 119.8 . . ? C24 C23 H23A 119.8 . . ? C19 C24 C23 120.8(5) . . ? C19 C24 H24A 119.6 . . ? C23 C24 H24A 119.6 . . ? C26 C25 C30 118.3(4) . . ? C26 C25 P2 117.6(3) . . ? C30 C25 P2 123.9(3) . . ? C25 C26 C27 120.5(5) . . ? C25 C26 H26A 119.7 . . ? C27 C26 H26A 119.7 . . ? C28 C27 C26 119.5(5) . . ? C28 C27 H27A 120.2 . . ? C26 C27 H27A 120.2 . . ? C27 C28 C29 120.1(5) . . ? C27 C28 H28A 119.9 . . ? C29 C28 H28A 119.9 . . ? C30 C29 C28 118.2(6) . . ? C30 C29 H29A 120.9 . . ? C28 C29 H29A 120.9 . . ? C29 C30 C25 123.2(5) . . ? C29 C30 H30A 118.4 . . ? C25 C30 H30A 118.4 . . ? C36 C31 C32 119.4(4) . . ? C36 C31 P2 118.4(3) . . ? C32 C31 P2 122.2(3) . . ? C33 C32 C31 121.4(5) . . ? C33 C32 H32A 119.3 . . ? C31 C32 H32A 119.3 . . ? C34 C33 C32 119.0(5) . . ? C34 C33 H33A 120.5 . . ? C32 C33 H33A 120.5 . . ? C33 C34 C35 119.9(5) . . ? C33 C34 H34A 120.1 . . ? C35 C34 H34A 120.1 . . ? C34 C35 C36 121.1(5) . . ? C34 C35 H35A 119.4 . . ? C36 C35 H35A 119.4 . . ? C31 C36 C35 119.2(4) . . ? C31 C36 H36A 120.4 . . ? C35 C36 H36A 120.4 . . ? O2 C37 O1 123.4(4) . . ? O2 C37 C38 116.1(3) . . ? O1 C37 C38 120.6(4) . . ? O2 C37 Cu1 60.61(19) . . ? O1 C37 Cu1 62.8(2) . . ? C38 C37 Cu1 176.2(3) . . ? N1 C38 C37 114.6(3) . . ? N1 C38 H38A 108.6 . . ? C37 C38 H38A 108.6 . . ? N1 C38 H38B 108.6 . . ? C37 C38 H38B 108.6 . . ? H38A C38 H38B 107.6 . . ? N1 C39 C40 128.5(4) . . ? N1 C39 C44 108.9(4) . . ? C40 C39 C44 122.6(4) . . ? C41 C40 C39 117.3(5) . . ? C41 C40 H40A 121.3 . . ? C39 C40 H40A 121.3 . . ? C42 C41 C40 122.3(5) . . ? C42 C41 H41A 118.9 . . ? C40 C41 H41A 118.9 . . ? C41 C42 C43 121.3(5) . . ? C41 C42 H42A 119.3 . . ? C43 C42 H42A 119.3 . . ? C42 C43 C44 118.2(5) . . ? C42 C43 H43A 120.9 . . ? C44 C43 H43A 120.9 . . ? C39 C44 C43 118.1(5) . . ? C39 C44 C45 107.3(4) . . ? C43 C44 C45 134.6(5) . . ? C46 C45 C50 119.6(5) . . ? C46 C45 C44 133.8(5) . . ? C50 C45 C44 106.7(4) . . ? C45 C46 C47 119.2(6) . . ? C45 C46 H46A 120.4 . . ? C47 C46 H46A 120.4 . . ? C46 C47 C48 119.9(5) . . ? C46 C47 H47A 120.1 . . ? C48 C47 H47A 120.1 . . ? C49 C48 C47 122.3(6) . . ? C49 C48 H48A 118.9 . . ? C47 C48 H48A 118.9 . . ? C48 C49 C50 116.2(6) . . ? C48 C49 H49A 121.9 . . ? C50 C49 H49A 121.9 . . ? C49 C50 C45 122.7(4) . . ? C49 C50 N1 127.9(5) . . ? C45 C50 N1 109.4(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 O2 Cu1 P1 C1 -82.43(17) . . . . ? O1 Cu1 P1 C1 -148.82(17) . . . . ? P2 Cu1 P1 C1 64.38(16) . . . . ? C37 Cu1 P1 C1 -115.17(18) . . . . ? O2 Cu1 P1 C13 38.80(18) . . . . ? O1 Cu1 P1 C13 -27.59(17) . . . . ? P2 Cu1 P1 C13 -174.39(15) . . . . ? C37 Cu1 P1 C13 6.06(19) . . . . ? O2 Cu1 P1 C7 157.96(16) . . . . ? O1 Cu1 P1 C7 91.56(16) . . . . ? P2 Cu1 P1 C7 -55.23(16) . . . . ? C37 Cu1 P1 C7 125.21(18) . . . . ? O2 Cu1 P2 C19 88.18(17) . . . . ? P1 Cu1 P2 C19 -59.32(16) . . . . ? O1 Cu1 P2 C19 152.15(17) . . . . ? C37 Cu1 P2 C19 120.26(18) . . . . ? O2 Cu1 P2 C31 -29.24(18) . . . . ? P1 Cu1 P2 C31 -176.73(16) . . . . ? O1 Cu1 P2 C31 34.74(18) . . . . ? C37 Cu1 P2 C31 2.85(19) . . . . ? O2 Cu1 P2 C25 -149.90(17) . . . . ? P1 Cu1 P2 C25 62.61(17) . . . . ? O1 Cu1 P2 C25 -85.92(17) . . . . ? C37 Cu1 P2 C25 -117.81(18) . . . . ? O2 Cu1 O1 C37 1.0(2) . . . . ? P1 Cu1 O1 C37 104.2(2) . . . . ? P2 Cu1 O1 C37 -102.3(2) . . . . ? P1 Cu1 O2 C37 -107.9(2) . . . . ? O1 Cu1 O2 C37 -1.1(2) . . . . ? P2 Cu1 O2 C37 99.0(2) . . . . ? C13 P1 C1 C2 -140.5(4) . . . . ? C7 P1 C1 C2 111.4(4) . . . . ? Cu1 P1 C1 C2 -11.4(5) . . . . ? C13 P1 C1 C6 42.5(5) . . . . ? C7 P1 C1 C6 -65.7(5) . . . . ? Cu1 P1 C1 C6 171.6(5) . . . . ? C6 C1 C2 C3 -2.3(10) . . . . ? P1 C1 C2 C3 -179.6(6) . . . . ? C1 C2 C3 C4 3.6(12) . . . . ? C2 C3 C4 C5 -1.9(12) . . . . ? C3 C4 C5 C6 -1.0(12) . . . . ? C2 C1 C6 C5 -0.8(10) . . . . ? P1 C1 C6 C5 176.2(5) . . . . ? C4 C5 C6 C1 2.5(12) . . . . ? C1 P1 C7 C12 176.4(3) . . . . ? C13 P1 C7 C12 67.8(4) . . . . ? Cu1 P1 C7 C12 -59.9(4) . . . . ? C1 P1 C7 C8 -10.8(4) . . . . ? C13 P1 C7 C8 -119.4(4) . . . . ? Cu1 P1 C7 C8 112.9(3) . . . . ? C12 C7 C8 C9 -0.4(6) . . . . ? P1 C7 C8 C9 -173.0(4) . . . . ? C7 C8 C9 C10 -0.3(7) . . . . ? C8 C9 C10 C11 1.0(8) . . . . ? C9 C10 C11 C12 -1.0(8) . . . . ? C10 C11 C12 C7 0.3(8) . . . . ? C8 C7 C12 C11 0.4(7) . . . . ? P1 C7 C12 C11 173.4(4) . . . . ? C1 P1 C13 C18 94.9(4) . . . . ? C7 P1 C13 C18 -154.6(4) . . . . ? Cu1 P1 C13 C18 -31.0(4) . . . . ? C1 P1 C13 C14 -83.0(4) . . . . ? C7 P1 C13 C14 27.5(4) . . . . ? Cu1 P1 C13 C14 151.1(3) . . . . ? C18 C13 C14 C15 -1.6(7) . . . . ? P1 C13 C14 C15 176.3(4) . . . . ? C13 C14 C15 C16 1.1(8) . . . . ? C14 C15 C16 C17 0.5(8) . . . . ? C15 C16 C17 C18 -1.6(8) . . . . ? C14 C13 C18 C17 0.6(7) . . . . ? P1 C13 C18 C17 -177.4(4) . . . . ? C16 C17 C18 C13 1.0(8) . . . . ? C31 P2 C19 C20 73.4(4) . . . . ? C25 P2 C19 C20 -179.3(4) . . . . ? Cu1 P2 C19 C20 -52.7(4) . . . . ? C31 P2 C19 C24 -107.2(4) . . . . ? C25 P2 C19 C24 0.1(5) . . . . ? Cu1 P2 C19 C24 126.7(4) . . . . ? C24 C19 C20 C21 1.3(8) . . . . ? P2 C19 C20 C21 -179.2(4) . . . . ? C19 C20 C21 C22 -2.8(9) . . . . ? C20 C21 C22 C23 3.3(9) . . . . ? C21 C22 C23 C24 -2.3(10) . . . . ? C20 C19 C24 C23 -0.2(7) . . . . ? P2 C19 C24 C23 -179.6(4) . . . . ? C22 C23 C24 C19 0.7(9) . . . . ? C19 P2 C25 C26 87.0(4) . . . . ? C31 P2 C25 C26 -166.7(4) . . . . ? Cu1 P2 C25 C26 -38.5(4) . . . . ? C19 P2 C25 C30 -97.4(4) . . . . ? C31 P2 C25 C30 9.0(5) . . . . ? Cu1 P2 C25 C30 137.1(4) . . . . ? C30 C25 C26 C27 -0.2(7) . . . . ? P2 C25 C26 C27 175.7(4) . . . . ? C25 C26 C27 C28 -0.6(9) . . . . ? C26 C27 C28 C29 1.9(10) . . . . ? C27 C28 C29 C30 -2.5(10) . . . . ? C28 C29 C30 C25 1.8(10) . . . . ? C26 C25 C30 C29 -0.5(8) . . . . ? P2 C25 C30 C29 -176.1(5) . . . . ? C19 P2 C31 C36 -165.9(3) . . . . ? C25 P2 C31 C36 84.2(4) . . . . ? Cu1 P2 C31 C36 -42.5(4) . . . . ? C19 P2 C31 C32 15.2(4) . . . . ? C25 P2 C31 C32 -94.7(4) . . . . ? Cu1 P2 C31 C32 138.6(3) . . . . ? C36 C31 C32 C33 0.7(7) . . . . ? P2 C31 C32 C33 179.5(4) . . . . ? C31 C32 C33 C34 -1.8(8) . . . . ? C32 C33 C34 C35 1.2(9) . . . . ? C33 C34 C35 C36 0.6(8) . . . . ? C32 C31 C36 C35 1.1(7) . . . . ? P2 C31 C36 C35 -177.8(4) . . . . ? C34 C35 C36 C31 -1.8(7) . . . . ? Cu1 O2 C37 O1 1.9(4) . . . . ? Cu1 O2 C37 C38 -177.9(3) . . . . ? Cu1 O1 C37 O2 -1.9(4) . . . . ? Cu1 O1 C37 C38 178.0(3) . . . . ? P1 Cu1 C37 O2 86.7(2) . . . . ? O1 Cu1 C37 O2 178.2(4) . . . . ? P2 Cu1 C37 O2 -92.9(2) . . . . ? O2 Cu1 C37 O1 -178.2(4) . . . . ? P1 Cu1 C37 O1 -91.4(2) . . . . ? P2 Cu1 C37 O1 88.9(2) . . . . ? O2 Cu1 C37 C38 29(4) . . . . ? P1 Cu1 C37 C38 116(4) . . . . ? O1 Cu1 C37 C38 -153(4) . . . . ? P2 Cu1 C37 C38 -64(4) . . . . ? C39 N1 C38 C37 -96.0(4) . . . . ? C50 N1 C38 C37 69.2(5) . . . . ? O2 C37 C38 N1 -178.8(3) . . . . ? O1 C37 C38 N1 1.3(5) . . . . ? Cu1 C37 C38 N1 153(4) . . . . ? C50 N1 C39 C40 179.3(4) . . . . ? C38 N1 C39 C40 -13.4(7) . . . . ? C50 N1 C39 C44 1.6(4) . . . . ? C38 N1 C39 C44 168.9(3) . . . . ? N1 C39 C40 C41 -177.9(5) . . . . ? C44 C39 C40 C41 -0.5(7) . . . . ? C39 C40 C41 C42 -1.0(8) . . . . ? C40 C41 C42 C43 0.0(10) . . . . ? C41 C42 C43 C44 2.6(9) . . . . ? N1 C39 C44 C43 -179.1(4) . . . . ? C40 C39 C44 C43 3.1(6) . . . . ? N1 C39 C44 C45 -0.6(5) . . . . ? C40 C39 C44 C45 -178.4(4) . . . . ? C42 C43 C44 C39 -4.0(7) . . . . ? C42 C43 C44 C45 177.9(5) . . . . ? C39 C44 C45 C46 177.6(5) . . . . ? C43 C44 C45 C46 -4.2(9) . . . . ? C39 C44 C45 C50 -0.7(4) . . . . ? C43 C44 C45 C50 177.5(5) . . . . ? C50 C45 C46 C47 -2.9(7) . . . . ? C44 C45 C46 C47 179.0(5) . . . . ? C45 C46 C47 C48 3.7(9) . . . . ? C46 C47 C48 C49 -3.7(9) . . . . ? C47 C48 C49 C50 2.6(8) . . . . ? C48 C49 C50 C45 -1.8(7) . . . . ? C48 C49 C50 N1 176.8(4) . . . . ? C46 C45 C50 C49 2.0(7) . . . . ? C44 C45 C50 C49 -179.4(4) . . . . ? C46 C45 C50 N1 -176.9(4) . . . . ? C44 C45 C50 N1 1.8(4) . . . . ? C39 N1 C50 C49 179.1(4) . . . . ? C38 N1 C50 C49 11.6(6) . . . . ? C39 N1 C50 C45 -2.1(4) . . . . ? C38 N1 C50 C45 -169.6(3) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.799 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.144