# Electronic Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and The Centre National de la Recherche Scientifique 2011 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Prof. Xiu-Jian Wang' _publ_contact_author_email 'wang1 xj@yahoo.com.cn' _publ_author_name 'Xiu-Jian Wang' data_1 _database_code_depnum_ccdc_archive 'CCDC 822790' #TrackingRef '- complex 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H49 Cl2 Cu2 N6 O8.50 P2' _chemical_formula_weight 1249.96 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' 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 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.844(1) _cell_length_b 15.520(1) _cell_length_c 17.594(2) _cell_angle_alpha 90.00 _cell_angle_beta 100.868(1) _cell_angle_gamma 90.00 _cell_volume 2908.00(15) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 15175 _cell_measurement_theta_min 6.08 _cell_measurement_theta_max 54.97 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 0.939 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8272 _exptl_absorpt_correction_T_max 0.9287 _exptl_absorpt_process_details ? _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 RAXIS-RAPID _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22466 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5112 _reflns_number_gt 3535 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1513P)^2^+1.1688P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.013(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 5112 _refine_ls_number_parameters 363 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0974 _refine_ls_R_factor_gt 0.0693 _refine_ls_wR_factor_ref 0.2513 _refine_ls_wR_factor_gt 0.2046 _refine_ls_goodness_of_fit_ref 1.178 _refine_ls_restrained_S_all 1.178 _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 0.17084(6) 0.06373(4) 0.37235(4) 0.0496(3) Uani 1 1 d . . . P1 P 0.22003(12) 0.14081(8) 0.28101(8) 0.0419(4) Uani 1 1 d . . . N1 N 0.4612(4) 0.1075(3) 0.3520(3) 0.0507(12) Uani 1 1 d . . . H1B H 0.5153 0.1464 0.3701 0.061 Uiso 1 1 calc R . . N3 N 0.1022(4) -0.0381(3) 0.4200(3) 0.0488(11) Uani 1 1 d . . . N2 N 0.2199(4) 0.1029(3) 0.4857(3) 0.0499(11) Uani 1 1 d . . . C1 C 0.3845(5) -0.0366(3) 0.3651(4) 0.0492(13) Uani 1 1 d . . . H1A H 0.3472 -0.0372 0.3130 0.059 Uiso 1 1 calc R . . C2 C 0.4497(5) 0.0363(3) 0.3968(3) 0.0467(13) Uani 1 1 d . . . C3 C 0.5071(4) 0.0365(3) 0.4776(3) 0.0417(12) Uani 1 1 d . . . C4 C 0.5726(5) 0.1099(3) 0.5133(3) 0.0467(13) Uani 1 1 d . . . H4A H 0.5790 0.1592 0.4843 0.056 Uiso 1 1 calc R . . C5 C 0.6251(5) 0.1083(3) 0.5889(3) 0.0461(13) Uani 1 1 d . . . H5A H 0.6690 0.1564 0.6111 0.055 Uiso 1 1 calc R . . C6 C 0.3863(5) 0.1196(3) 0.2760(3) 0.0498(13) Uani 1 1 d . . . H6A H 0.3915 0.0684 0.2451 0.060 Uiso 1 1 calc R . . H6B H 0.4194 0.1676 0.2508 0.060 Uiso 1 1 calc R . . C7 C 0.1426(7) 0.1334(3) 0.1816(4) 0.067(2) Uani 1 1 d . . . C8 C 0.2009(11) 0.1653(4) 0.1217(4) 0.105(3) Uani 1 1 d . . . H8A H 0.2777 0.1928 0.1375 0.126 Uiso 1 1 calc R . . C9 C 0.1591(14) 0.1608(6) 0.0444(5) 0.118(4) Uani 1 1 d . . . H9A H 0.2041 0.1797 0.0075 0.141 Uiso 1 1 calc R . . C10 C 0.0484(13) 0.1269(7) 0.0284(8) 0.127(5) Uani 1 1 d . . . H10A H 0.0137 0.1262 -0.0241 0.152 Uiso 1 1 calc R . . C11 C -0.0318(13) 0.0898(7) 0.0770(9) 0.149(6) Uani 1 1 d . . . H11A H -0.1104 0.0659 0.0584 0.179 Uiso 1 1 calc R . . C12 C 0.0287(9) 0.0948(5) 0.1625(6) 0.112(4) Uani 1 1 d . . . H12A H -0.0112 0.0722 0.2004 0.134 Uiso 1 1 calc R . . C13 C 0.2158(5) 0.2557(3) 0.3053(3) 0.0396(11) Uani 1 1 d . . . C14 C 0.1060(6) 0.2857(4) 0.3237(4) 0.0585(15) Uani 1 1 d . . . H14A H 0.0363 0.2497 0.3185 0.070 Uiso 1 1 calc R . . C15 C 0.0985(7) 0.3695(4) 0.3500(4) 0.0678(18) Uani 1 1 d . . . H15A H 0.0245 0.3898 0.3630 0.081 Uiso 1 1 calc R . . C16 C 0.2034(7) 0.4228(3) 0.3565(4) 0.0585(16) Uani 1 1 d . . . H16A H 0.2006 0.4787 0.3754 0.070 Uiso 1 1 calc R . . C17 C 0.3086(6) 0.3934(4) 0.3357(4) 0.0613(17) Uani 1 1 d . . . H17A H 0.3777 0.4297 0.3389 0.074 Uiso 1 1 calc R . . C18 C 0.3152(5) 0.3101(3) 0.3095(4) 0.0550(15) Uani 1 1 d . . . H18A H 0.3884 0.2909 0.2946 0.066 Uiso 1 1 calc R . . C19 C 0.2779(5) 0.1722(4) 0.5168(4) 0.0558(14) Uani 1 1 d . . . H19A H 0.2898 0.2176 0.4845 0.067 Uiso 1 1 calc R . . C20 C 0.3231(6) 0.1811(4) 0.5969(4) 0.0656(17) Uani 1 1 d . . . H20A H 0.3649 0.2309 0.6165 0.079 Uiso 1 1 calc R . . C21 C 0.3048(6) 0.1159(5) 0.6453(4) 0.0678(18) Uani 1 1 d . . . H21A H 0.3328 0.1213 0.6984 0.081 Uiso 1 1 calc R . . C22 C 0.2436(6) 0.0404(4) 0.6148(4) 0.0591(16) Uani 1 1 d . . . C23 C 0.2023(5) 0.0365(4) 0.5335(4) 0.0522(14) Uani 1 1 d . . . C24 C 0.2215(6) -0.0327(5) 0.6590(4) 0.0674(18) Uani 1 1 d . . . H24A H 0.2477 -0.0312 0.7125 0.081 Uiso 1 1 calc R . . C25 C 0.1645(6) -0.1031(5) 0.6266(4) 0.0669(18) Uani 1 1 d . . . H25A H 0.1510 -0.1493 0.6577 0.080 Uiso 1 1 calc R . . C26 C 0.1239(6) -0.1089(4) 0.5452(4) 0.0567(15) Uani 1 1 d . . . C27 C 0.1403(5) -0.0376(3) 0.4982(4) 0.0523(15) Uani 1 1 d . . . C28 C 0.0660(6) -0.1824(4) 0.5073(5) 0.0685(19) Uani 1 1 d . . . H28A H 0.0547 -0.2313 0.5358 0.082 Uiso 1 1 calc R . . C29 C 0.0264(6) -0.1822(4) 0.4293(4) 0.0608(17) Uani 1 1 d . . . H29A H -0.0134 -0.2303 0.4044 0.073 Uiso 1 1 calc R . . C30 C 0.0462(5) -0.1083(3) 0.3864(4) 0.0558(15) Uani 1 1 d . . . H30A H 0.0192 -0.1088 0.3330 0.067 Uiso 1 1 calc R . . Cl1 Cl 0.17000(14) 0.18979(9) 0.81462(10) 0.0625(5) Uani 1 1 d . . . O1 O 0.1243(5) 0.2381(3) 0.7448(3) 0.0877(15) Uani 1 1 d . . . O2 O 0.1182(4) 0.1053(3) 0.8054(4) 0.0866(16) Uani 1 1 d . . . O3 O 0.3039(4) 0.1837(3) 0.8297(3) 0.0903(17) Uani 1 1 d . . . O4 O 0.1300(4) 0.2336(3) 0.8773(3) 0.0702(12) Uani 1 1 d . . . O5 O 0.5000 0.0000 0.0000 0.214(12) Uiso 0.50 2 d SP . . 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 0.0490(5) 0.0406(5) 0.0613(5) 0.0098(3) 0.0163(3) -0.0006(3) P1 0.0441(8) 0.0348(7) 0.0451(8) 0.0047(5) 0.0038(6) 0.0007(5) N1 0.039(2) 0.045(2) 0.067(3) 0.014(2) 0.007(2) -0.0049(19) N3 0.044(2) 0.042(2) 0.063(3) 0.010(2) 0.017(2) 0.0078(19) N2 0.041(2) 0.045(2) 0.068(3) 0.003(2) 0.021(2) 0.001(2) C1 0.041(3) 0.042(3) 0.065(4) 0.006(3) 0.009(3) 0.005(2) C2 0.037(3) 0.039(3) 0.067(4) 0.009(2) 0.014(2) 0.001(2) C3 0.027(2) 0.037(2) 0.062(3) 0.008(2) 0.008(2) 0.0036(19) C4 0.037(3) 0.033(2) 0.070(4) 0.012(2) 0.009(3) 0.004(2) C5 0.036(3) 0.033(2) 0.068(4) 0.005(2) 0.006(2) 0.004(2) C6 0.055(3) 0.043(3) 0.055(3) 0.005(2) 0.020(3) 0.002(2) C7 0.104(5) 0.032(3) 0.055(4) -0.004(3) -0.015(4) 0.019(3) C8 0.202(10) 0.046(4) 0.053(4) -0.001(3) -0.010(5) 0.035(5) C9 0.202(13) 0.072(5) 0.067(5) -0.002(4) -0.005(6) 0.029(7) C10 0.124(10) 0.069(6) 0.158(12) -0.002(6) -0.047(9) 0.024(6) C11 0.144(10) 0.062(5) 0.198(13) -0.062(7) -0.080(10) 0.031(6) C12 0.111(7) 0.060(4) 0.132(7) -0.034(5) -0.059(6) 0.031(4) C13 0.046(3) 0.037(2) 0.035(3) 0.007(2) 0.006(2) -0.002(2) C14 0.056(4) 0.049(3) 0.078(4) -0.011(3) 0.031(3) -0.014(3) C15 0.079(5) 0.047(3) 0.087(5) -0.010(3) 0.039(4) -0.001(3) C16 0.081(4) 0.034(3) 0.059(4) -0.007(2) 0.009(3) -0.007(3) C17 0.047(3) 0.041(3) 0.091(5) 0.003(3) 0.000(3) -0.005(2) C18 0.041(3) 0.042(3) 0.082(4) 0.010(3) 0.012(3) -0.003(2) C19 0.047(3) 0.059(3) 0.067(4) -0.001(3) 0.025(3) 0.004(3) C20 0.047(3) 0.071(4) 0.083(5) -0.017(4) 0.024(3) -0.001(3) C21 0.049(4) 0.094(5) 0.061(4) 0.000(4) 0.013(3) 0.009(3) C22 0.047(3) 0.079(4) 0.056(4) 0.015(3) 0.022(3) 0.022(3) C23 0.036(3) 0.050(3) 0.076(4) 0.014(3) 0.025(3) 0.011(2) C24 0.057(4) 0.093(5) 0.058(4) 0.023(4) 0.025(3) 0.027(4) C25 0.063(4) 0.074(4) 0.071(4) 0.030(4) 0.032(3) 0.026(3) C26 0.050(3) 0.048(3) 0.077(4) 0.019(3) 0.025(3) 0.013(3) C27 0.034(3) 0.045(3) 0.083(5) 0.014(3) 0.025(3) 0.009(2) C28 0.070(4) 0.049(3) 0.096(6) 0.024(3) 0.040(4) 0.015(3) C29 0.050(3) 0.041(3) 0.098(5) 0.008(3) 0.031(3) -0.001(2) C30 0.042(3) 0.041(3) 0.088(4) 0.005(3) 0.024(3) 0.005(2) Cl1 0.0495(9) 0.0558(9) 0.0841(11) -0.0233(8) 0.0174(8) -0.0022(6) O1 0.105(4) 0.085(3) 0.073(3) -0.001(3) 0.018(3) 0.008(3) O2 0.067(3) 0.054(3) 0.139(5) -0.032(3) 0.018(3) -0.008(2) O3 0.043(2) 0.104(4) 0.125(4) -0.055(3) 0.017(3) 0.000(2) O4 0.077(3) 0.062(3) 0.077(3) -0.019(2) 0.029(2) 0.010(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 N3 1.998(4) . ? Cu1 N2 2.057(5) . ? Cu1 P1 2.1498(15) . ? P1 C7 1.796(6) . ? P1 C13 1.836(5) . ? P1 C6 1.852(6) . ? N1 C2 1.378(7) . ? N1 C6 1.439(7) . ? N1 H1B 0.8600 . ? N3 C30 1.331(8) . ? N3 C27 1.361(8) . ? N2 C19 1.312(7) . ? N2 C23 1.367(7) . ? C1 C5 1.391(8) 3_656 ? C1 C2 1.393(8) . ? C1 H1A 0.9300 . ? C2 C3 1.440(8) . ? C3 C3 1.407(10) 3_656 ? C3 C4 1.424(7) . ? C4 C5 1.345(8) . ? C4 H4A 0.9300 . ? C5 C1 1.391(8) 3_656 ? C5 H5A 0.9300 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C12 1.356(11) . ? C7 C8 1.417(12) . ? C8 C9 1.351(11) . ? C8 H8A 0.9300 . ? C9 C10 1.292(15) . ? C9 H9A 0.9300 . ? C10 C11 1.450(19) . ? C10 H10A 0.9300 . ? C11 C12 1.526(15) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C18 1.360(7) . ? C13 C14 1.373(8) . ? C14 C15 1.388(8) . ? C14 H14A 0.9300 . ? C15 C16 1.395(9) . ? C15 H15A 0.9300 . ? C16 C17 1.342(9) . ? C16 H16A 0.9300 . ? C17 C18 1.380(8) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 C20 1.408(9) . ? C19 H19A 0.9300 . ? C20 C21 1.361(10) . ? C20 H20A 0.9300 . ? C21 C22 1.403(10) . ? C21 H21A 0.9300 . ? C22 C23 1.417(9) . ? C22 C24 1.420(9) . ? C23 C27 1.414(8) . ? C24 C25 1.330(10) . ? C24 H24A 0.9300 . ? C25 C26 1.420(10) . ? C25 H25A 0.9300 . ? C26 C28 1.409(9) . ? C26 C27 1.412(8) . ? C28 C29 1.357(10) . ? C28 H28A 0.9300 . ? C29 C30 1.411(8) . ? C29 H29A 0.9300 . ? C30 H30A 0.9300 . ? Cl1 O2 1.423(5) . ? Cl1 O3 1.429(5) . ? Cl1 O4 1.431(4) . ? Cl1 O1 1.444(5) . ? 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 N3 Cu1 N2 82.88(19) . . ? N3 Cu1 P1 156.72(15) . . ? N2 Cu1 P1 120.32(13) . . ? C7 P1 C13 105.1(2) . . ? C7 P1 C6 102.9(3) . . ? C13 P1 C6 104.5(2) . . ? C7 P1 Cu1 123.8(3) . . ? C13 P1 Cu1 110.26(17) . . ? C6 P1 Cu1 108.53(18) . . ? C2 N1 C6 122.7(4) . . ? C2 N1 H1B 118.6 . . ? C6 N1 H1B 118.6 . . ? C30 N3 C27 118.7(5) . . ? C30 N3 Cu1 129.6(4) . . ? C27 N3 Cu1 110.7(4) . . ? C19 N2 C23 118.2(5) . . ? C19 N2 Cu1 131.5(4) . . ? C23 N2 Cu1 109.4(4) . . ? C5 C1 C2 120.3(5) 3_656 . ? C5 C1 H1A 119.8 3_656 . ? C2 C1 H1A 119.8 . . ? N1 C2 C1 121.1(5) . . ? N1 C2 C3 119.6(5) . . ? C1 C2 C3 119.3(5) . . ? C3 C3 C4 119.7(6) 3_656 . ? C3 C3 C2 118.6(6) 3_656 . ? C4 C3 C2 121.7(5) . . ? C5 C4 C3 120.4(5) . . ? C5 C4 H4A 119.8 . . ? C3 C4 H4A 119.8 . . ? C4 C5 C1 121.6(5) . 3_656 ? C4 C5 H5A 119.2 . . ? C1 C5 H5A 119.2 3_656 . ? N1 C6 P1 111.2(4) . . ? N1 C6 H6A 109.4 . . ? P1 C6 H6A 109.4 . . ? N1 C6 H6B 109.4 . . ? P1 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? C12 C7 C8 118.9(8) . . ? C12 C7 P1 120.4(7) . . ? C8 C7 P1 120.7(6) . . ? C9 C8 C7 128.2(11) . . ? C9 C8 H8A 115.9 . . ? C7 C8 H8A 115.9 . . ? C10 C9 C8 111.2(13) . . ? C10 C9 H9A 124.4 . . ? C8 C9 H9A 124.4 . . ? C9 C10 C11 132.0(12) . . ? C9 C10 H10A 114.0 . . ? C11 C10 H10A 114.0 . . ? C10 C11 C12 111.5(10) . . ? C10 C11 H11A 124.3 . . ? C12 C11 H11A 124.3 . . ? C7 C12 C11 118.0(12) . . ? C7 C12 H12A 121.0 . . ? C11 C12 H12A 121.0 . . ? C18 C13 C14 119.4(5) . . ? C18 C13 P1 124.1(4) . . ? C14 C13 P1 116.4(4) . . ? C13 C14 C15 120.3(5) . . ? C13 C14 H14A 119.9 . . ? C15 C14 H14A 119.9 . . ? C14 C15 C16 119.1(6) . . ? C14 C15 H15A 120.5 . . ? C16 C15 H15A 120.5 . . ? C17 C16 C15 119.8(5) . . ? C17 C16 H16A 120.1 . . ? C15 C16 H16A 120.1 . . ? C16 C17 C18 120.7(6) . . ? C16 C17 H17A 119.6 . . ? C18 C17 H17A 119.6 . . ? C13 C18 C17 120.6(6) . . ? C13 C18 H18A 119.7 . . ? C17 C18 H18A 119.7 . . ? N2 C19 C20 123.1(6) . . ? N2 C19 H19A 118.4 . . ? C20 C19 H19A 118.4 . . ? C21 C20 C19 119.3(6) . . ? C21 C20 H20A 120.4 . . ? C19 C20 H20A 120.4 . . ? C20 C21 C22 119.7(6) . . ? C20 C21 H21A 120.1 . . ? C22 C21 H21A 120.1 . . ? C21 C22 C23 117.3(6) . . ? C21 C22 C24 125.0(6) . . ? C23 C22 C24 117.7(6) . . ? N2 C23 C27 116.9(6) . . ? N2 C23 C22 122.3(6) . . ? C27 C23 C22 120.7(5) . . ? C25 C24 C22 122.2(6) . . ? C25 C24 H24A 118.9 . . ? C22 C24 H24A 118.9 . . ? C24 C25 C26 121.0(6) . . ? C24 C25 H25A 119.5 . . ? C26 C25 H25A 119.5 . . ? C28 C26 C27 116.9(6) . . ? C28 C26 C25 123.7(6) . . ? C27 C26 C25 119.4(6) . . ? N3 C27 C26 122.6(6) . . ? N3 C27 C23 118.5(5) . . ? C26 C27 C23 118.8(6) . . ? C29 C28 C26 120.2(6) . . ? C29 C28 H28A 119.9 . . ? C26 C28 H28A 119.9 . . ? C28 C29 C30 119.5(6) . . ? C28 C29 H29A 120.3 . . ? C30 C29 H29A 120.3 . . ? N3 C30 C29 122.0(6) . . ? N3 C30 H30A 119.0 . . ? C29 C30 H30A 119.0 . . ? O2 Cl1 O3 109.0(3) . . ? O2 Cl1 O4 110.7(3) . . ? O3 Cl1 O4 109.5(3) . . ? O2 Cl1 O1 108.5(3) . . ? O3 Cl1 O1 111.4(4) . . ? O4 Cl1 O1 107.7(3) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.818 _refine_diff_density_min -0.738 _refine_diff_density_rms 0.125 # Attachment '- complex 2.CIF' data_2 _database_code_depnum_ccdc_archive 'CCDC 822791' #TrackingRef '- complex 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H70 Cl2 Cu2 N8 O10 P2' _chemical_formula_weight 1443.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 11.155(2) _cell_length_b 11.249(2) _cell_length_c 15.696(1) _cell_angle_alpha 84.503(1) _cell_angle_beta 75.887(6) _cell_angle_gamma 60.284(4) _cell_volume 1658.2(3) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2669 _cell_measurement_theta_min 3.0227 _cell_measurement_theta_max 29.7387 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.445 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 0.836 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.96092 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_process_details ? _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 'Bruker APEX CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10120 _diffrn_reflns_av_R_equivalents 0.0801 _diffrn_reflns_av_sigmaI/netI 0.1759 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5607 _reflns_number_gt 3112 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0868P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5607 _refine_ls_number_parameters 428 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1825 _refine_ls_R_factor_gt 0.0956 _refine_ls_wR_factor_ref 0.2136 _refine_ls_wR_factor_gt 0.1825 _refine_ls_goodness_of_fit_ref 1.073 _refine_ls_restrained_S_all 1.073 _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 0.32993(10) 0.77698(10) 0.12423(7) 0.0257(3) Uani 1 1 d . . . P1 P 0.1817(2) 0.9010(2) 0.23912(15) 0.0280(6) Uani 1 1 d . . . N1 N 0.2801(6) 1.0774(7) 0.1748(5) 0.0327(17) Uani 1 1 d . . . H1B H 0.3252 1.0995 0.2016 0.039 Uiso 1 1 calc R . . N2 N 0.3335(7) 0.6981(6) 0.0104(4) 0.0235(16) Uani 1 1 d . . . N3 N 0.5431(6) 0.6942(6) 0.0705(4) 0.0217(16) Uani 1 1 d . . . N4 N 0.2987(9) 0.2754(12) 0.4157(6) 0.083(4) Uani 1 1 d . . . C1 C 0.2570(7) 1.0238(7) 0.0371(6) 0.026(2) Uani 1 1 d . . . H1A H 0.1675 1.0354 0.0636 0.031 Uiso 1 1 calc R . . C2 C 0.3330(8) 1.0411(7) 0.0873(6) 0.024(2) Uani 1 1 d . . . C3 C 0.4753(8) 1.0174(7) 0.0448(5) 0.027(2) Uani 1 1 d . . . C4 C 0.5600(8) 1.0330(7) 0.0927(6) 0.028(2) Uani 1 1 d . . . H4A H 0.5255 1.0587 0.1520 0.033 Uiso 1 1 calc R . . C5 C 0.6906(8) 1.0103(8) 0.0510(6) 0.026(2) Uani 1 1 d . . . H5A H 0.7469 1.0178 0.0828 0.031 Uiso 1 1 calc R . . C6 C 0.1532(8) 1.0798(8) 0.2228(6) 0.034(2) Uani 1 1 d . . . H6A H 0.0787 1.1309 0.1912 0.041 Uiso 1 1 calc R . . H6B H 0.1235 1.1254 0.2796 0.041 Uiso 1 1 calc R . . C7 C 0.2315(9) 0.8536(10) 0.3437(6) 0.035(2) Uani 1 1 d . . . C8 C 0.1685(11) 0.9424(14) 0.4150(7) 0.068(4) Uani 1 1 d . . . H8A H 0.0990 1.0316 0.4089 0.082 Uiso 1 1 calc R . . C9 C 0.2034(13) 0.9053(16) 0.4947(8) 0.080(4) Uani 1 1 d . . . H9A H 0.1644 0.9694 0.5406 0.097 Uiso 1 1 calc R . . C10 C 0.2987(16) 0.7694(18) 0.5050(8) 0.084(4) Uani 1 1 d . . . H10A H 0.3143 0.7399 0.5607 0.100 Uiso 1 1 calc R . . C11 C 0.3712(15) 0.6763(14) 0.4347(9) 0.082(4) Uani 1 1 d . . . H11A H 0.4415 0.5875 0.4411 0.098 Uiso 1 1 calc R . . C12 C 0.3348(12) 0.7206(12) 0.3528(7) 0.060(3) Uani 1 1 d . . . H12A H 0.3807 0.6598 0.3046 0.072 Uiso 1 1 calc R . . C13 C 0.0030(8) 0.9197(9) 0.2642(5) 0.030(2) Uani 1 1 d . . . C14 C -0.1161(9) 1.0398(10) 0.2569(6) 0.040(2) Uani 1 1 d . . . H14A H -0.1110 1.1191 0.2404 0.048 Uiso 1 1 calc R . . C15 C -0.2471(9) 1.0410(10) 0.2751(6) 0.041(2) Uani 1 1 d . . . H15A H -0.3279 1.1225 0.2695 0.049 Uiso 1 1 calc R . . C16 C -0.2601(10) 0.9302(11) 0.2999(6) 0.044(3) Uani 1 1 d . . . H16A H -0.3479 0.9342 0.3126 0.053 Uiso 1 1 calc R . . C17 C -0.1389(11) 0.8099(11) 0.3060(8) 0.064(3) Uani 1 1 d . . . H17A H -0.1441 0.7305 0.3221 0.076 Uiso 1 1 calc R . . C18 C -0.0099(10) 0.8062(10) 0.2885(7) 0.056(3) Uani 1 1 d . . . H18A H 0.0706 0.7239 0.2933 0.068 Uiso 1 1 calc R . . C19 C 0.6436(8) 0.6920(8) 0.1010(6) 0.033(2) Uani 1 1 d . . . C20 C 0.7795(9) 0.6508(8) 0.0467(7) 0.038(2) Uani 1 1 d . . . H20A H 0.8483 0.6522 0.0696 0.045 Uiso 1 1 calc R . . C21 C 0.8119(9) 0.6097(8) -0.0371(7) 0.044(3) Uani 1 1 d . . . H21A H 0.9016 0.5837 -0.0725 0.052 Uiso 1 1 calc R . . C22 C 0.7058(8) 0.6067(8) -0.0709(6) 0.029(2) Uani 1 1 d . . . C23 C 0.7293(9) 0.5666(9) -0.1598(6) 0.041(2) Uani 1 1 d . . . H23A H 0.8164 0.5415 -0.1983 0.049 Uiso 1 1 calc R . . C24 C 0.6240(10) 0.5651(9) -0.1877(6) 0.041(2) Uani 1 1 d . . . H24A H 0.6418 0.5340 -0.2446 0.049 Uiso 1 1 calc R . . C25 C 0.4867(8) 0.6100(8) -0.1317(6) 0.027(2) Uani 1 1 d . . . C26 C 0.3712(10) 0.6158(8) -0.1585(6) 0.038(2) Uani 1 1 d . . . H26A H 0.3834 0.5868 -0.2151 0.045 Uiso 1 1 calc R . . C27 C 0.2461(9) 0.6625(8) -0.1026(6) 0.035(2) Uani 1 1 d . . . H27A H 0.1701 0.6695 -0.1215 0.042 Uiso 1 1 calc R . . C28 C 0.2252(8) 0.7021(7) -0.0149(6) 0.025(2) Uani 1 1 d . . . C29 C 0.4601(8) 0.6529(7) -0.0452(6) 0.025(2) Uani 1 1 d . . . C30 C 0.5735(8) 0.6506(7) -0.0146(6) 0.025(2) Uani 1 1 d . . . C31 C 0.6107(10) 0.7373(10) 0.1949(6) 0.046(3) Uani 1 1 d . . . H31A H 0.6769 0.7648 0.2017 0.069 Uiso 1 1 calc R . . H31B H 0.6182 0.6630 0.2328 0.069 Uiso 1 1 calc R . . H31C H 0.5162 0.8132 0.2100 0.069 Uiso 1 1 calc R . . C32 C 0.0852(8) 0.7608(9) 0.0471(7) 0.043(3) Uani 1 1 d . . . H32A H 0.0952 0.7183 0.1029 0.065 Uiso 1 1 calc R . . H32B H 0.0219 0.7446 0.0243 0.065 Uiso 1 1 calc R . . H32C H 0.0474 0.8576 0.0544 0.065 Uiso 1 1 calc R . . C33 C 0.1833(15) 0.4102(17) 0.4479(11) 0.132(7) Uani 1 1 d . . . H33A H 0.1409 0.4600 0.4004 0.199 Uiso 1 1 calc R . . H33B H 0.2192 0.4588 0.4713 0.199 Uiso 1 1 calc R . . H33C H 0.1134 0.4009 0.4932 0.199 Uiso 1 1 calc R . . C34 C 0.4038(13) 0.201(2) 0.4655(10) 0.167(11) Uani 1 1 d . . . H34A H 0.3653 0.1663 0.5167 0.250 Uiso 1 1 calc R . . H34B H 0.4324 0.2609 0.4832 0.250 Uiso 1 1 calc R . . H34C H 0.4844 0.1263 0.4302 0.250 Uiso 1 1 calc R . . C35 C 0.3032(12) 0.2177(13) 0.3455(7) 0.056(3) Uani 1 1 d . . . H35A H 0.2276 0.2661 0.3184 0.067 Uiso 1 1 calc R . . Cl1 Cl 0.1336(2) 0.5688(2) 0.68405(17) 0.0436(7) Uani 1 1 d . . . O1 O 0.0628(11) 0.5504(12) 0.7616(8) 0.169(6) Uani 1 1 d . . . O2 O 0.1997(12) 0.6323(10) 0.7085(7) 0.120(4) Uani 1 1 d . . . O3 O 0.0489(8) 0.6622(9) 0.6283(6) 0.110(4) Uani 1 1 d . . . O4 O 0.2381(8) 0.4487(8) 0.6382(5) 0.081(3) Uani 1 1 d . . . O5 O 0.3960(7) 0.1076(8) 0.3125(5) 0.064(2) 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 0.0217(5) 0.0270(6) 0.0285(7) -0.0019(5) -0.0050(4) -0.0118(5) P1 0.0287(12) 0.0334(13) 0.0261(14) -0.0026(10) -0.0016(10) -0.0198(11) N1 0.029(4) 0.030(4) 0.047(5) -0.006(3) 0.004(3) -0.025(3) N2 0.031(4) 0.015(3) 0.031(4) 0.014(3) -0.011(3) -0.017(3) N3 0.013(3) 0.018(3) 0.038(5) 0.013(3) -0.015(3) -0.009(3) N4 0.046(5) 0.127(10) 0.051(7) -0.043(6) -0.006(5) -0.018(6) C1 0.010(4) 0.018(4) 0.051(6) 0.003(4) -0.010(4) -0.006(3) C2 0.021(4) 0.004(4) 0.046(6) 0.009(4) -0.011(4) -0.005(3) C3 0.023(4) 0.013(4) 0.042(5) 0.005(4) -0.014(4) -0.005(3) C4 0.025(4) 0.016(4) 0.044(6) 0.003(4) -0.008(4) -0.013(4) C5 0.026(4) 0.023(4) 0.040(6) 0.010(4) -0.014(4) -0.018(4) C6 0.028(4) 0.026(5) 0.047(6) -0.009(4) 0.008(4) -0.017(4) C7 0.039(5) 0.051(6) 0.026(6) 0.004(4) -0.004(4) -0.033(5) C8 0.049(6) 0.120(11) 0.020(7) -0.005(6) -0.002(5) -0.032(7) C9 0.068(8) 0.116(12) 0.058(10) -0.016(8) -0.007(7) -0.045(8) C10 0.105(11) 0.146(14) 0.032(8) 0.011(9) -0.014(8) -0.087(11) C11 0.106(10) 0.087(10) 0.084(11) 0.039(9) -0.047(9) -0.066(9) C12 0.087(8) 0.067(8) 0.044(7) 0.019(6) -0.028(6) -0.048(7) C13 0.029(5) 0.034(5) 0.026(5) -0.001(4) 0.002(4) -0.019(4) C14 0.037(5) 0.056(6) 0.042(6) 0.012(5) -0.013(5) -0.035(5) C15 0.040(5) 0.052(6) 0.034(6) 0.014(5) -0.018(5) -0.024(5) C16 0.035(5) 0.070(8) 0.033(6) -0.011(5) 0.001(4) -0.032(6) C17 0.052(7) 0.035(6) 0.102(10) -0.002(6) 0.001(6) -0.028(6) C18 0.039(6) 0.037(6) 0.090(9) 0.007(6) 0.002(6) -0.025(5) C19 0.020(4) 0.010(4) 0.069(7) 0.014(4) -0.017(5) -0.005(4) C20 0.027(5) 0.026(5) 0.063(7) 0.015(5) -0.023(5) -0.011(4) C21 0.019(5) 0.021(5) 0.077(8) 0.004(5) 0.006(5) -0.008(4) C22 0.029(5) 0.017(4) 0.045(6) 0.012(4) -0.008(4) -0.018(4) C23 0.025(5) 0.033(5) 0.051(7) 0.001(5) 0.009(4) -0.014(4) C24 0.054(6) 0.034(5) 0.029(6) -0.003(4) 0.004(5) -0.022(5) C25 0.029(5) 0.020(4) 0.033(6) 0.009(4) -0.006(4) -0.016(4) C26 0.065(7) 0.027(5) 0.027(6) 0.011(4) -0.024(5) -0.023(5) C27 0.034(5) 0.029(5) 0.052(7) 0.013(4) -0.021(5) -0.019(4) C28 0.022(4) 0.009(4) 0.040(6) 0.000(4) -0.013(4) -0.002(3) C29 0.023(4) 0.014(4) 0.030(5) -0.002(4) -0.009(4) -0.001(4) C30 0.019(4) 0.011(4) 0.039(6) 0.001(4) -0.001(4) -0.004(3) C31 0.049(6) 0.049(6) 0.049(7) -0.003(5) -0.021(5) -0.026(5) C32 0.026(5) 0.037(6) 0.074(8) 0.003(5) -0.023(5) -0.016(4) C33 0.107(12) 0.170(17) 0.118(14) -0.078(13) 0.003(10) -0.064(12) C34 0.062(9) 0.30(3) 0.097(13) -0.085(15) -0.032(9) -0.037(12) C35 0.058(7) 0.095(9) 0.031(7) -0.003(6) -0.001(5) -0.051(7) Cl1 0.0371(13) 0.0358(14) 0.0542(17) -0.0092(12) -0.0092(12) -0.0138(11) O1 0.101(8) 0.132(10) 0.175(12) 0.027(9) 0.072(8) -0.034(7) O2 0.193(10) 0.126(8) 0.112(9) 0.021(6) -0.098(8) -0.106(8) O3 0.055(5) 0.107(8) 0.110(8) -0.033(6) -0.047(5) 0.022(5) O4 0.073(5) 0.060(5) 0.070(6) -0.009(4) -0.004(4) -0.006(4) O5 0.047(4) 0.084(6) 0.055(5) -0.022(4) -0.002(4) -0.028(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 2.052(6) . ? Cu1 N2 2.053(7) . ? Cu1 P1 2.162(2) . ? P1 C7 1.808(9) . ? P1 C13 1.842(8) . ? P1 C6 1.875(8) . ? N1 C2 1.370(10) . ? N1 C6 1.420(10) . ? N1 H1B 0.8600 . ? N2 C29 1.337(10) . ? N2 C28 1.340(9) . ? N3 C19 1.311(9) . ? N3 C30 1.370(10) . ? N4 C35 1.310(12) . ? N4 C34 1.427(14) . ? N4 C33 1.451(15) . ? C1 C5 1.372(11) 2_675 ? C1 C2 1.378(10) . ? C1 H1A 0.9300 . ? C2 C3 1.460(11) . ? C3 C3 1.395(16) 2_675 ? C3 C4 1.423(10) . ? C4 C5 1.347(11) . ? C4 H4A 0.9300 . ? C5 C1 1.372(11) 2_675 ? C5 H5A 0.9300 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C8 1.372(13) . ? C7 C12 1.385(13) . ? C8 C9 1.366(14) . ? C8 H8A 0.9300 . ? C9 C10 1.386(17) . ? C9 H9A 0.9300 . ? C10 C11 1.384(17) . ? C10 H10A 0.9300 . ? C11 C12 1.414(15) . ? C11 H11A 0.9300 . ? C12 H12A 0.9300 . ? C13 C18 1.363(13) . ? C13 C14 1.367(11) . ? C14 C15 1.413(12) . ? C14 H14A 0.9300 . ? C15 C16 1.336(13) . ? C15 H15A 0.9300 . ? C16 C17 1.376(12) . ? C16 H16A 0.9300 . ? C17 C18 1.378(13) . ? C17 H17A 0.9300 . ? C18 H18A 0.9300 . ? C19 C20 1.411(12) . ? C19 C31 1.504(12) . ? C20 C21 1.340(12) . ? C20 H20A 0.9300 . ? C21 C22 1.425(12) . ? C21 H21A 0.9300 . ? C22 C30 1.388(11) . ? C22 C23 1.429(12) . ? C23 C24 1.358(12) . ? C23 H23A 0.9300 . ? C24 C25 1.426(12) . ? C24 H24A 0.9300 . ? C25 C29 1.397(11) . ? C25 C26 1.420(11) . ? C26 C27 1.326(12) . ? C26 H26A 0.9300 . ? C27 C28 1.416(12) . ? C27 H27A 0.9300 . ? C28 C32 1.477(11) . ? C29 C30 1.447(11) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 O5 1.211(12) . ? C35 H35A 0.9300 . ? Cl1 O1 1.339(11) . ? Cl1 O2 1.383(10) . ? Cl1 O4 1.385(7) . ? Cl1 O3 1.415(8) . ? 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 N3 Cu1 N2 82.5(3) . . ? N3 Cu1 P1 136.78(19) . . ? N2 Cu1 P1 140.51(19) . . ? C7 P1 C13 102.4(4) . . ? C7 P1 C6 104.8(4) . . ? C13 P1 C6 105.1(4) . . ? C7 P1 Cu1 117.9(3) . . ? C13 P1 Cu1 116.9(3) . . ? C6 P1 Cu1 108.4(3) . . ? C2 N1 C6 122.3(7) . . ? C2 N1 H1B 118.9 . . ? C6 N1 H1B 118.9 . . ? C29 N2 C28 120.6(7) . . ? C29 N2 Cu1 110.7(5) . . ? C28 N2 Cu1 128.2(6) . . ? C19 N3 C30 118.9(7) . . ? C19 N3 Cu1 130.4(6) . . ? C30 N3 Cu1 110.2(4) . . ? C35 N4 C34 119.7(11) . . ? C35 N4 C33 121.5(11) . . ? C34 N4 C33 118.7(11) . . ? C5 C1 C2 121.9(8) 2_675 . ? C5 C1 H1A 119.0 2_675 . ? C2 C1 H1A 119.0 . . ? N1 C2 C1 122.1(8) . . ? N1 C2 C3 119.9(7) . . ? C1 C2 C3 118.0(8) . . ? C3 C3 C4 120.7(9) 2_675 . ? C3 C3 C2 118.2(9) 2_675 . ? C4 C3 C2 121.0(7) . . ? C5 C4 C3 119.1(8) . . ? C5 C4 H4A 120.4 . . ? C3 C4 H4A 120.4 . . ? C4 C5 C1 121.9(7) . 2_675 ? C4 C5 H5A 119.0 . . ? C1 C5 H5A 119.0 2_675 . ? N1 C6 P1 110.4(5) . . ? N1 C6 H6A 109.6 . . ? P1 C6 H6A 109.6 . . ? N1 C6 H6B 109.6 . . ? P1 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? C8 C7 C12 118.6(9) . . ? C8 C7 P1 122.9(8) . . ? C12 C7 P1 118.5(7) . . ? C9 C8 C7 122.8(11) . . ? C9 C8 H8A 118.6 . . ? C7 C8 H8A 118.6 . . ? C8 C9 C10 118.0(12) . . ? C8 C9 H9A 121.0 . . ? C10 C9 H9A 121.0 . . ? C11 C10 C9 121.7(12) . . ? C11 C10 H10A 119.1 . . ? C9 C10 H10A 119.1 . . ? C10 C11 C12 117.8(12) . . ? C10 C11 H11A 121.1 . . ? C12 C11 H11A 121.1 . . ? C7 C12 C11 120.6(11) . . ? C7 C12 H12A 119.7 . . ? C11 C12 H12A 119.7 . . ? C18 C13 C14 118.5(8) . . ? C18 C13 P1 118.0(7) . . ? C14 C13 P1 123.5(7) . . ? C13 C14 C15 118.6(9) . . ? C13 C14 H14A 120.7 . . ? C15 C14 H14A 120.7 . . ? C16 C15 C14 122.9(9) . . ? C16 C15 H15A 118.5 . . ? C14 C15 H15A 118.5 . . ? C15 C16 C17 117.7(9) . . ? C15 C16 H16A 121.2 . . ? C17 C16 H16A 121.2 . . ? C16 C17 C18 120.4(10) . . ? C16 C17 H17A 119.8 . . ? C18 C17 H17A 119.8 . . ? C13 C18 C17 121.9(9) . . ? C13 C18 H18A 119.1 . . ? C17 C18 H18A 119.1 . . ? N3 C19 C20 121.0(9) . . ? N3 C19 C31 118.8(8) . . ? C20 C19 C31 120.1(8) . . ? C21 C20 C19 121.4(8) . . ? C21 C20 H20A 119.3 . . ? C19 C20 H20A 119.3 . . ? C20 C21 C22 118.6(8) . . ? C20 C21 H21A 120.7 . . ? C22 C21 H21A 120.7 . . ? C30 C22 C21 117.2(8) . . ? C30 C22 C23 120.1(8) . . ? C21 C22 C23 122.7(8) . . ? C24 C23 C22 119.8(8) . . ? C24 C23 H23A 120.1 . . ? C22 C23 H23A 120.1 . . ? C23 C24 C25 121.5(9) . . ? C23 C24 H24A 119.2 . . ? C25 C24 H24A 119.2 . . ? C29 C25 C26 116.4(8) . . ? C29 C25 C24 119.7(8) . . ? C26 C25 C24 123.9(8) . . ? C27 C26 C25 119.7(8) . . ? C27 C26 H26A 120.1 . . ? C25 C26 H26A 120.1 . . ? C26 C27 C28 121.7(8) . . ? C26 C27 H27A 119.1 . . ? C28 C27 H27A 119.1 . . ? N2 C28 C27 118.7(8) . . ? N2 C28 C32 118.4(7) . . ? C27 C28 C32 122.6(7) . . ? N2 C29 C25 122.8(7) . . ? N2 C29 C30 118.4(7) . . ? C25 C29 C30 118.8(8) . . ? N3 C30 C22 122.9(7) . . ? N3 C30 C29 117.1(7) . . ? C22 C30 C29 120.0(8) . . ? C19 C31 H31A 109.5 . . ? C19 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C19 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C28 C32 H32A 109.5 . . ? C28 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C28 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N4 C33 H33A 109.5 . . ? N4 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N4 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N4 C34 H34A 109.5 . . ? N4 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N4 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? O5 C35 N4 126.4(11) . . ? O5 C35 H35A 116.8 . . ? N4 C35 H35A 116.8 . . ? O1 Cl1 O2 102.4(8) . . ? O1 Cl1 O4 114.4(7) . . ? O2 Cl1 O4 107.7(6) . . ? O1 Cl1 O3 115.7(7) . . ? O2 Cl1 O3 104.7(6) . . ? O4 Cl1 O3 110.7(5) . . ? _diffrn_measured_fraction_theta_max 0.959 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.959 _refine_diff_density_max 0.931 _refine_diff_density_min -0.469 _refine_diff_density_rms 0.105 # Attachment '- complex 3.CIF' data_3 _database_code_depnum_ccdc_archive 'CCDC 822792' #TrackingRef '- complex 3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H47 Cl Cu N5 O5 P2' _chemical_formula_weight 970.87 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting ORTHORHOMBIC _symmetry_space_group_name_H-M P212121 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' _cell_length_a 13.523(2) _cell_length_b 18.277(3) _cell_length_c 18.648(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4609.0(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 27.43 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 0.656 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8078 _exptl_absorpt_correction_T_max 0.9255 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEX CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 14425 _diffrn_reflns_av_R_equivalents 0.0416 _diffrn_reflns_av_sigmaI/netI 0.0695 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.56 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7308 _reflns_number_gt 5342 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0850P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.572(19) _refine_ls_number_reflns 7308 _refine_ls_number_parameters 589 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0866 _refine_ls_R_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.1540 _refine_ls_wR_factor_gt 0.1362 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 0.18414(5) -0.32971(4) -0.69058(4) 0.0345(2) Uani 1 1 d . . . P1 P 0.05750(11) -0.39101(8) -0.73991(9) 0.0349(4) Uani 1 1 d . . . P2 P -0.16849(11) -0.14385(8) -0.25687(9) 0.0361(4) Uani 1 1 d . . . N1 N -0.0703(4) -0.3910(3) -0.6255(3) 0.0403(12) Uani 1 1 d . . . H1A H -0.0749 -0.4339 -0.6043 0.048 Uiso 1 1 calc R . . N2 N -0.0538(4) -0.2241(3) -0.3429(3) 0.0495(14) Uani 1 1 d . . . H2B H -0.0320 -0.1837 -0.3630 0.059 Uiso 1 1 calc R . . N4 N 0.1869(3) -0.3312(2) -0.5794(2) 0.0325(10) Uani 1 1 d . . . N3 N 0.1825(3) -0.2176(2) -0.6706(2) 0.0308(10) Uani 1 1 d . . . C10 C -0.0586(4) -0.2863(3) -0.3856(3) 0.0339(14) Uani 1 1 d . . . C9 C -0.0602(4) -0.3552(3) -0.3573(4) 0.0413(15) Uani 1 1 d . . . H9A H -0.0584 -0.3617 -0.3067 0.050 Uiso 1 1 calc R . . C8 C -0.0646(4) -0.4160(3) -0.4023(3) 0.0373(15) Uani 1 1 d . . . H8A H -0.0668 -0.4636 -0.3818 0.045 Uiso 1 1 calc R . . C7 C -0.0659(4) -0.4089(3) -0.4739(3) 0.0353(14) Uani 1 1 d . . . H7A H -0.0688 -0.4513 -0.5032 0.042 Uiso 1 1 calc R . . C6 C -0.0629(4) -0.3392(3) -0.5063(3) 0.0322(13) Uani 1 1 d . . . C5 C -0.0597(4) -0.2758(3) -0.4621(3) 0.0332(14) Uani 1 1 d . . . C4 C -0.0575(4) -0.2060(3) -0.4949(4) 0.0395(15) Uani 1 1 d . . . H4A H -0.0580 -0.1633 -0.4659 0.047 Uiso 1 1 calc R . . C3 C -0.0546(4) -0.1996(3) -0.5672(4) 0.0385(15) Uani 1 1 d . . . H3A H -0.0513 -0.1522 -0.5879 0.046 Uiso 1 1 calc R . . C2 C -0.0563(4) -0.2608(3) -0.6121(4) 0.0365(14) Uani 1 1 d . . . H2A H -0.0523 -0.2547 -0.6626 0.044 Uiso 1 1 calc R . . C1 C -0.0636(4) -0.3296(3) -0.5836(3) 0.0335(13) Uani 1 1 d . . . C11 C -0.0702(4) -0.3884(3) -0.7025(3) 0.0381(14) Uani 1 1 d . . . H11A H -0.1035 -0.3430 -0.7186 0.046 Uiso 1 1 calc R . . H11B H -0.1083 -0.4305 -0.7214 0.046 Uiso 1 1 calc R . . C12 C 0.0282(4) -0.3717(3) -0.8329(3) 0.0385(15) Uani 1 1 d . . . C13 C 0.0347(5) -0.3013(4) -0.8570(4) 0.0532(19) Uani 1 1 d . . . H13A H 0.0603 -0.2645 -0.8261 0.064 Uiso 1 1 calc R . . C14 C 0.0046(6) -0.2824(4) -0.9255(4) 0.065(2) Uani 1 1 d . . . H14A H 0.0089 -0.2330 -0.9411 0.078 Uiso 1 1 calc R . . C15 C -0.0317(6) -0.3353(5) -0.9711(4) 0.065(2) Uani 1 1 d . . . H15A H -0.0542 -0.3223 -1.0176 0.078 Uiso 1 1 calc R . . C16 C -0.0350(6) -0.4066(5) -0.9492(4) 0.064(2) Uani 1 1 d . . . H16A H -0.0577 -0.4437 -0.9808 0.077 Uiso 1 1 calc R . . C17 C -0.0054(5) -0.4239(4) -0.8810(4) 0.056(2) Uani 1 1 d . . . H17A H -0.0080 -0.4735 -0.8661 0.067 Uiso 1 1 calc R . . C18 C 0.0873(4) -0.4889(3) -0.7387(3) 0.0361(14) Uani 1 1 d . . . C19 C 0.0447(5) -0.5358(3) -0.6910(4) 0.0462(15) Uani 1 1 d . . . H19A H -0.0035 -0.5183 -0.6582 0.055 Uiso 1 1 calc R . . C20 C 0.0713(6) -0.6088(3) -0.6903(4) 0.0584(19) Uani 1 1 d . . . H20A H 0.0395 -0.6413 -0.6579 0.070 Uiso 1 1 calc R . . C21 C 0.1408(6) -0.6342(4) -0.7340(4) 0.061(2) Uani 1 1 d . . . H21A H 0.1616 -0.6837 -0.7311 0.073 Uiso 1 1 calc R . . C22 C 0.1817(7) -0.5881(4) -0.7831(5) 0.078(2) Uani 1 1 d . . . H22A H 0.2285 -0.6064 -0.8165 0.094 Uiso 1 1 calc R . . C23 C 0.1561(5) -0.5159(4) -0.7847(4) 0.061(2) Uani 1 1 d . . . H23A H 0.1867 -0.4841 -0.8183 0.073 Uiso 1 1 calc R . . C24 C -0.0813(5) -0.2203(3) -0.2691(4) 0.0447(16) Uani 1 1 d . . . H24A H -0.0219 -0.2125 -0.2391 0.054 Uiso 1 1 calc R . . H24B H -0.1128 -0.2668 -0.2543 0.054 Uiso 1 1 calc R . . C25 C -0.1617(4) -0.1338(3) -0.1597(3) 0.0377(15) Uani 1 1 d . . . C26 C -0.1166(5) -0.0762(4) -0.1242(4) 0.0457(17) Uani 1 1 d . . . H26A H -0.0872 -0.0380 -0.1513 0.055 Uiso 1 1 calc R . . C27 C -0.1135(5) -0.0732(4) -0.0499(4) 0.0528(18) Uani 1 1 d . . . H27A H -0.0814 -0.0338 -0.0263 0.063 Uiso 1 1 calc R . . C28 C -0.1574(6) -0.1278(4) -0.0112(4) 0.061(2) Uani 1 1 d . . . H28A H -0.1574 -0.1256 0.0397 0.073 Uiso 1 1 calc R . . C29 C -0.2018(7) -0.1860(4) -0.0458(4) 0.071(2) Uani 1 1 d . . . H29A H -0.2301 -0.2247 -0.0186 0.086 Uiso 1 1 calc R . . C30 C -0.2051(6) -0.1883(4) -0.1193(4) 0.057(2) Uani 1 1 d . . . H30A H -0.2375 -0.2278 -0.1427 0.068 Uiso 1 1 calc R . . C31 C -0.0962(5) -0.0674(3) -0.2921(3) 0.0428(16) Uani 1 1 d . . . C32 C 0.0048(5) -0.0605(4) -0.2840(4) 0.057(2) Uani 1 1 d . . . H32A H 0.0403 -0.0964 -0.2577 0.068 Uiso 1 1 calc R . . C33 C 0.0542(7) -0.0030(5) -0.3133(5) 0.073(2) Uani 1 1 d . . . H33A H 0.1240 0.0000 -0.3080 0.088 Uiso 1 1 calc R . . C34 C 0.0066(8) 0.0494(5) -0.3494(5) 0.092(3) Uani 1 1 d . . . H34A H 0.0422 0.0903 -0.3675 0.110 Uiso 1 1 calc R . . C35 C -0.0938(9) 0.0444(5) -0.3605(5) 0.093(3) Uani 1 1 d . . . H35A H -0.1273 0.0806 -0.3878 0.112 Uiso 1 1 calc R . . C36 C -0.1456(6) -0.0139(4) -0.3315(4) 0.063(2) Uani 1 1 d . . . H36A H -0.2151 -0.0174 -0.3385 0.076 Uiso 1 1 calc R . . C37 C 0.1814(4) -0.1615(3) -0.7154(3) 0.0388(14) Uani 1 1 d . . . H37A H 0.1786 -0.1710 -0.7654 0.047 Uiso 1 1 calc R . . C38 C 0.1842(4) -0.0884(3) -0.6922(4) 0.0434(15) Uani 1 1 d . . . H38A H 0.1835 -0.0497 -0.7263 0.052 Uiso 1 1 calc R . . C39 C 0.1880(4) -0.0732(3) -0.6218(4) 0.0403(15) Uani 1 1 d . . . H39A H 0.1908 -0.0239 -0.6059 0.048 Uiso 1 1 calc R . . C40 C 0.1876(4) -0.1302(3) -0.5720(3) 0.0300(12) Uani 1 1 d . . . C41 C 0.1864(4) -0.2022(3) -0.5997(3) 0.0312(13) Uani 1 1 d . . . C42 C 0.1900(4) -0.1190(3) -0.4957(3) 0.0399(15) Uani 1 1 d . . . H42A H 0.1917 -0.0707 -0.4771 0.048 Uiso 1 1 calc R . . C43 C 0.1898(4) -0.1765(3) -0.4504(3) 0.0355(13) Uani 1 1 d . . . H43A H 0.1909 -0.1678 -0.4002 0.043 Uiso 1 1 calc R . . C44 C 0.1881(4) -0.2505(3) -0.4759(3) 0.0319(13) Uani 1 1 d . . . C45 C 0.1872(4) -0.2622(3) -0.5505(3) 0.0283(12) Uani 1 1 d . . . C46 C 0.1870(4) -0.3112(3) -0.4305(3) 0.0380(14) Uani 1 1 d . . . H46A H 0.1867 -0.3051 -0.3799 0.046 Uiso 1 1 calc R . . C47 C 0.1864(5) -0.3795(3) -0.4600(3) 0.0393(14) Uani 1 1 d . . . H47A H 0.1862 -0.4215 -0.4300 0.047 Uiso 1 1 calc R . . C48 C 0.1860(5) -0.3874(3) -0.5347(3) 0.0370(13) Uani 1 1 d . . . H48A H 0.1851 -0.4354 -0.5542 0.044 Uiso 1 1 calc R . . N5 N -0.3355(6) -0.3069(4) -0.8415(5) 0.088(2) Uani 1 1 d . . . C49 C -0.3934(10) -0.2823(8) -0.9037(7) 0.148(6) Uani 1 1 d . . . H49A H -0.3974 -0.2288 -0.9036 0.223 Uiso 1 1 calc R . . H49B H -0.4601 -0.3030 -0.9011 0.223 Uiso 1 1 calc R . . H49C H -0.3611 -0.2988 -0.9479 0.223 Uiso 1 1 calc R . . C50 C -0.2905(11) -0.3740(8) -0.8503(8) 0.164(6) Uani 1 1 d . . . H50A H -0.2713 -0.3934 -0.8034 0.246 Uiso 1 1 calc R . . H50B H -0.2315 -0.3683 -0.8804 0.246 Uiso 1 1 calc R . . H50C H -0.3367 -0.4079 -0.8735 0.246 Uiso 1 1 calc R . . C51 C -0.3283(8) -0.2676(7) -0.7845(6) 0.099(3) Uani 1 1 d . . . H51A H -0.3605 -0.2214 -0.7845 0.118 Uiso 1 1 calc R . . Cl1 Cl -0.20209(14) -0.58520(8) -0.57959(10) 0.0560(5) Uani 1 1 d . . . O1 O -0.2513(12) -0.6396(4) -0.6089(5) 0.229(8) Uani 1 1 d . . . O2 O -0.2501(6) -0.5667(4) -0.5177(4) 0.114(3) Uani 1 1 d . . . O3 O -0.1991(4) -0.5243(2) -0.6273(3) 0.0633(13) Uani 1 1 d . . . O4 O -0.1119(7) -0.6073(8) -0.5667(8) 0.287(10) Uani 1 1 d . . . O5 O -0.2848(6) -0.2843(5) -0.7324(5) 0.118(3) 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 0.0410(4) 0.0331(4) 0.0295(4) -0.0030(3) 0.0008(3) -0.0031(3) P1 0.0393(8) 0.0351(8) 0.0302(9) -0.0045(7) 0.0018(7) -0.0080(7) P2 0.0426(9) 0.0349(8) 0.0309(9) -0.0027(7) -0.0019(7) -0.0010(7) N1 0.043(3) 0.036(3) 0.042(3) -0.003(3) 0.007(3) -0.001(2) N2 0.072(4) 0.043(3) 0.033(3) -0.006(3) 0.011(3) -0.004(3) N4 0.030(2) 0.030(2) 0.037(3) 0.000(2) -0.001(2) -0.001(2) N3 0.034(2) 0.030(2) 0.028(3) -0.001(2) -0.001(2) 0.002(2) C10 0.029(3) 0.034(3) 0.038(4) -0.004(3) 0.008(3) 0.002(3) C9 0.038(3) 0.049(4) 0.037(4) -0.005(3) 0.003(3) 0.008(3) C8 0.037(3) 0.032(3) 0.043(4) 0.002(3) 0.009(3) 0.008(3) C7 0.028(3) 0.038(3) 0.040(4) 0.000(3) 0.006(3) 0.004(3) C6 0.024(3) 0.036(3) 0.037(4) -0.002(3) 0.002(2) 0.004(3) C5 0.022(3) 0.034(3) 0.043(4) -0.005(3) 0.003(3) 0.004(2) C4 0.033(3) 0.037(3) 0.049(4) -0.005(3) -0.001(3) 0.002(3) C3 0.034(3) 0.035(3) 0.046(5) -0.003(3) 0.003(3) 0.006(3) C2 0.029(3) 0.042(3) 0.038(4) 0.005(3) 0.005(3) -0.001(3) C1 0.027(3) 0.035(3) 0.039(4) -0.011(3) 0.004(3) 0.004(3) C11 0.041(3) 0.045(3) 0.029(4) -0.006(3) -0.004(3) -0.005(3) C12 0.038(3) 0.045(4) 0.033(4) -0.007(3) 0.002(3) -0.007(3) C13 0.072(5) 0.053(4) 0.035(4) -0.016(3) -0.013(4) -0.001(4) C14 0.099(6) 0.055(4) 0.043(5) 0.006(4) -0.003(4) 0.000(4) C15 0.087(5) 0.078(5) 0.029(4) 0.006(4) -0.003(4) -0.011(5) C16 0.073(5) 0.080(5) 0.038(5) -0.002(4) -0.003(4) -0.034(4) C17 0.075(5) 0.057(4) 0.036(5) -0.008(4) -0.002(4) -0.030(4) C18 0.039(3) 0.036(3) 0.033(4) -0.008(3) -0.005(3) -0.007(3) C19 0.054(4) 0.050(4) 0.035(4) 0.005(3) 0.004(3) 0.005(3) C20 0.074(5) 0.048(4) 0.053(5) 0.007(4) -0.012(4) 0.002(4) C21 0.079(5) 0.040(4) 0.064(6) -0.010(4) -0.003(4) 0.007(4) C22 0.099(6) 0.052(4) 0.083(6) -0.012(4) 0.028(6) 0.008(5) C23 0.077(5) 0.050(4) 0.055(5) -0.011(4) 0.030(4) -0.011(4) C24 0.046(4) 0.048(4) 0.041(4) -0.006(3) 0.002(3) -0.003(3) C25 0.040(3) 0.029(3) 0.044(4) -0.007(3) -0.007(3) 0.006(3) C26 0.057(4) 0.044(4) 0.036(5) -0.004(3) -0.003(3) -0.013(3) C27 0.064(4) 0.047(4) 0.048(5) -0.004(4) -0.010(4) 0.000(3) C28 0.085(6) 0.075(5) 0.022(4) 0.002(4) -0.016(4) -0.002(4) C29 0.108(7) 0.069(5) 0.038(5) 0.003(4) 0.002(5) -0.028(5) C30 0.078(5) 0.046(4) 0.045(5) 0.001(3) -0.008(4) -0.024(4) C31 0.051(4) 0.045(4) 0.032(4) 0.003(3) 0.007(3) -0.011(3) C32 0.057(4) 0.055(4) 0.059(5) 0.003(4) 0.006(4) -0.013(4) C33 0.076(5) 0.081(5) 0.063(6) -0.007(5) 0.016(5) -0.030(5) C34 0.128(9) 0.085(7) 0.062(7) 0.023(5) 0.014(6) -0.044(6) C35 0.125(9) 0.080(6) 0.075(7) 0.034(5) -0.018(6) -0.026(6) C36 0.080(5) 0.054(4) 0.057(5) 0.008(4) -0.003(4) -0.009(4) C37 0.042(3) 0.034(3) 0.040(4) 0.004(3) -0.001(3) -0.001(3) C38 0.041(3) 0.033(3) 0.056(4) 0.008(3) -0.013(4) 0.005(3) C39 0.033(3) 0.034(3) 0.054(5) 0.003(3) -0.002(3) -0.003(3) C40 0.027(3) 0.032(3) 0.032(3) -0.001(2) 0.003(3) -0.003(2) C41 0.019(2) 0.033(3) 0.042(4) -0.004(3) 0.001(3) -0.004(2) C42 0.028(3) 0.039(3) 0.053(4) -0.013(3) -0.002(3) -0.001(3) C43 0.032(3) 0.044(3) 0.031(3) -0.013(3) -0.004(3) 0.000(3) C44 0.022(2) 0.043(3) 0.032(3) 0.008(3) -0.003(3) -0.002(3) C45 0.016(2) 0.035(3) 0.034(3) -0.001(3) -0.001(3) 0.002(2) C46 0.033(3) 0.052(4) 0.029(3) 0.003(3) -0.004(3) -0.001(3) C47 0.038(3) 0.040(3) 0.040(4) 0.012(3) -0.003(3) 0.003(3) C48 0.040(3) 0.034(3) 0.037(4) 0.005(3) 0.002(3) 0.000(3) N5 0.089(6) 0.089(5) 0.086(6) -0.028(5) 0.021(5) -0.017(5) C49 0.156(12) 0.199(15) 0.090(9) 0.042(10) -0.039(9) -0.035(10) C50 0.132(12) 0.180(14) 0.179(15) -0.065(12) 0.008(10) 0.032(10) C51 0.078(7) 0.126(9) 0.092(8) 0.001(8) -0.004(6) -0.036(7) Cl1 0.0701(12) 0.0355(8) 0.0625(12) 0.0060(8) 0.0241(10) 0.0037(8) O1 0.51(2) 0.068(4) 0.108(7) -0.023(5) 0.054(10) -0.128(8) O2 0.163(7) 0.099(5) 0.080(5) 0.013(4) 0.057(5) 0.026(5) O3 0.060(3) 0.057(3) 0.073(4) 0.019(3) -0.003(3) -0.012(2) O4 0.146(8) 0.340(15) 0.374(19) 0.300(15) 0.158(11) 0.154(10) O5 0.109(6) 0.146(7) 0.098(6) 0.016(5) -0.007(5) 0.004(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 N4 2.073(5) . ? Cu1 N3 2.083(4) . ? Cu1 P1 2.2437(16) . ? Cu1 P2 2.2729(17) 3_544 ? P1 C12 1.813(7) . ? P1 C18 1.834(6) . ? P1 C11 1.864(6) . ? P2 C25 1.824(7) . ? P2 C31 1.827(6) . ? P2 C24 1.842(6) . ? P2 Cu1 2.2729(17) 3_444 ? N1 C1 1.370(7) . ? N1 C11 1.437(7) . ? N1 H1A 0.8800 . ? N2 C10 1.390(7) . ? N2 C24 1.426(8) . ? N2 H2B 0.8800 . ? N4 C48 1.323(7) . ? N4 C45 1.371(7) . ? N3 C37 1.322(7) . ? N3 C41 1.352(7) . ? C10 C9 1.366(8) . ? C10 C5 1.439(9) . ? C9 C8 1.393(8) . ? C9 H9A 0.9500 . ? C8 C7 1.342(9) . ? C8 H8A 0.9500 . ? C7 C6 1.410(8) . ? C7 H7A 0.9500 . ? C6 C5 1.423(8) . ? C6 C1 1.452(8) . ? C5 C4 1.415(8) . ? C4 C3 1.354(8) . ? C4 H4A 0.9500 . ? C3 C2 1.398(8) . ? C3 H3A 0.9500 . ? C2 C1 1.369(8) . ? C2 H2A 0.9500 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.366(9) . ? C12 C17 1.386(8) . ? C13 C14 1.385(10) . ? C13 H13A 0.9500 . ? C14 C15 1.377(10) . ? C14 H14A 0.9500 . ? C15 C16 1.366(11) . ? C15 H15A 0.9500 . ? C16 C17 1.370(10) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C23 1.357(9) . ? C18 C19 1.364(8) . ? C19 C20 1.381(8) . ? C19 H19A 0.9500 . ? C20 C21 1.327(10) . ? C20 H20A 0.9500 . ? C21 C22 1.361(10) . ? C21 H21A 0.9500 . ? C22 C23 1.365(10) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C30 1.379(9) . ? C25 C26 1.385(8) . ? C26 C27 1.387(9) . ? C26 H26A 0.9500 . ? C27 C28 1.366(10) . ? C27 H27A 0.9500 . ? C28 C29 1.383(10) . ? C28 H28A 0.9500 . ? C29 C30 1.373(10) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C32 1.381(9) . ? C31 C36 1.394(9) . ? C32 C33 1.360(10) . ? C32 H32A 0.9500 . ? C33 C34 1.337(12) . ? C33 H33A 0.9500 . ? C34 C35 1.377(13) . ? C34 H34A 0.9500 . ? C35 C36 1.384(11) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C38 1.405(8) . ? C37 H37A 0.9500 . ? C38 C39 1.343(9) . ? C38 H38A 0.9500 . ? C39 C40 1.395(8) . ? C39 H39A 0.9500 . ? C40 C41 1.414(7) . ? C40 C42 1.437(8) . ? C41 C45 1.431(7) . ? C42 C43 1.348(8) . ? C42 H42A 0.9500 . ? C43 C44 1.433(8) . ? C43 H43A 0.9500 . ? C44 C46 1.396(8) . ? C44 C45 1.408(7) . ? C46 C47 1.363(8) . ? C46 H46A 0.9500 . ? C47 C48 1.401(8) . ? C47 H47A 0.9500 . ? C48 H48A 0.9500 . ? N5 C51 1.287(12) . ? N5 C50 1.380(14) . ? N5 C49 1.468(13) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 O5 1.175(11) . ? C51 H51A 0.9500 . ? Cl1 O4 1.307(9) . ? Cl1 O1 1.315(9) . ? Cl1 O2 1.368(6) . ? Cl1 O3 1.426(5) . ? 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 N4 Cu1 N3 80.47(17) . . ? N4 Cu1 P1 114.64(13) . . ? N3 Cu1 P1 123.80(14) . . ? N4 Cu1 P2 114.38(13) . 3_544 ? N3 Cu1 P2 107.20(14) . 3_544 ? P1 Cu1 P2 112.72(6) . 3_544 ? C12 P1 C18 104.4(3) . . ? C12 P1 C11 98.6(3) . . ? C18 P1 C11 103.0(3) . . ? C12 P1 Cu1 117.5(2) . . ? C18 P1 Cu1 108.32(19) . . ? C11 P1 Cu1 122.78(19) . . ? C25 P2 C31 104.7(3) . . ? C25 P2 C24 99.6(3) . . ? C31 P2 C24 101.1(3) . . ? C25 P2 Cu1 119.6(2) . 3_444 ? C31 P2 Cu1 118.4(2) . 3_444 ? C24 P2 Cu1 110.3(2) . 3_444 ? C1 N1 C11 122.9(5) . . ? C1 N1 H1A 118.5 . . ? C11 N1 H1A 118.5 . . ? C10 N2 C24 125.5(5) . . ? C10 N2 H2B 117.3 . . ? C24 N2 H2B 117.3 . . ? C48 N4 C45 117.8(5) . . ? C48 N4 Cu1 129.8(4) . . ? C45 N4 Cu1 112.4(3) . . ? C37 N3 C41 117.1(5) . . ? C37 N3 Cu1 130.6(4) . . ? C41 N3 Cu1 112.3(3) . . ? C9 C10 N2 122.2(6) . . ? C9 C10 C5 120.4(5) . . ? N2 C10 C5 117.3(5) . . ? C10 C9 C8 120.2(6) . . ? C10 C9 H9A 119.9 . . ? C8 C9 H9A 119.9 . . ? C7 C8 C9 121.5(6) . . ? C7 C8 H8A 119.2 . . ? C9 C8 H8A 119.2 . . ? C8 C7 C6 120.9(6) . . ? C8 C7 H7A 119.5 . . ? C6 C7 H7A 119.5 . . ? C7 C6 C5 119.2(5) . . ? C7 C6 C1 122.3(5) . . ? C5 C6 C1 118.5(5) . . ? C4 C5 C6 118.9(6) . . ? C4 C5 C10 123.3(6) . . ? C6 C5 C10 117.8(5) . . ? C3 C4 C5 120.6(6) . . ? C3 C4 H4A 119.7 . . ? C5 C4 H4A 119.7 . . ? C4 C3 C2 121.8(6) . . ? C4 C3 H3A 119.1 . . ? C2 C3 H3A 119.1 . . ? C1 C2 C3 120.2(6) . . ? C1 C2 H2A 119.9 . . ? C3 C2 H2A 119.9 . . ? C2 C1 N1 122.3(6) . . ? C2 C1 C6 119.8(5) . . ? N1 C1 C6 117.9(5) . . ? N1 C11 P1 111.9(4) . . ? N1 C11 H11A 109.2 . . ? P1 C11 H11A 109.2 . . ? N1 C11 H11B 109.2 . . ? P1 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? C13 C12 C17 117.1(6) . . ? C13 C12 P1 118.9(5) . . ? C17 C12 P1 123.8(5) . . ? C12 C13 C14 121.3(6) . . ? C12 C13 H13A 119.4 . . ? C14 C13 H13A 119.4 . . ? C15 C14 C13 120.0(7) . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C16 C15 C14 119.8(7) . . ? C16 C15 H15A 120.1 . . ? C14 C15 H15A 120.1 . . ? C15 C16 C17 119.2(7) . . ? C15 C16 H16A 120.4 . . ? C17 C16 H16A 120.4 . . ? C16 C17 C12 122.5(7) . . ? C16 C17 H17A 118.7 . . ? C12 C17 H17A 118.7 . . ? C23 C18 C19 118.2(6) . . ? C23 C18 P1 119.8(5) . . ? C19 C18 P1 121.9(5) . . ? C18 C19 C20 120.3(7) . . ? C18 C19 H19A 119.9 . . ? C20 C19 H19A 119.9 . . ? C21 C20 C19 121.0(7) . . ? C21 C20 H20A 119.5 . . ? C19 C20 H20A 119.5 . . ? C20 C21 C22 119.0(7) . . ? C20 C21 H21A 120.5 . . ? C22 C21 H21A 120.5 . . ? C21 C22 C23 120.7(8) . . ? C21 C22 H22A 119.7 . . ? C23 C22 H22A 119.7 . . ? C18 C23 C22 120.8(7) . . ? C18 C23 H23A 119.6 . . ? C22 C23 H23A 119.6 . . ? N2 C24 P2 108.9(5) . . ? N2 C24 H24A 109.9 . . ? P2 C24 H24A 109.9 . . ? N2 C24 H24B 109.9 . . ? P2 C24 H24B 109.9 . . ? H24A C24 H24B 108.3 . . ? C30 C25 C26 118.4(6) . . ? C30 C25 P2 116.6(5) . . ? C26 C25 P2 125.0(5) . . ? C25 C26 C27 121.4(6) . . ? C25 C26 H26A 119.3 . . ? C27 C26 H26A 119.3 . . ? C28 C27 C26 119.1(7) . . ? C28 C27 H27A 120.5 . . ? C26 C27 H27A 120.5 . . ? C27 C28 C29 120.2(7) . . ? C27 C28 H28A 119.9 . . ? C29 C28 H28A 119.9 . . ? C30 C29 C28 120.3(7) . . ? C30 C29 H29A 119.9 . . ? C28 C29 H29A 119.9 . . ? C29 C30 C25 120.6(6) . . ? C29 C30 H30A 119.7 . . ? C25 C30 H30A 119.7 . . ? C32 C31 C36 117.9(6) . . ? C32 C31 P2 124.0(6) . . ? C36 C31 P2 118.0(5) . . ? C33 C32 C31 120.8(8) . . ? C33 C32 H32A 119.6 . . ? C31 C32 H32A 119.6 . . ? C34 C33 C32 121.4(9) . . ? C34 C33 H33A 119.3 . . ? C32 C33 H33A 119.3 . . ? C33 C34 C35 120.1(8) . . ? C33 C34 H34A 119.9 . . ? C35 C34 H34A 119.9 . . ? C34 C35 C36 119.6(9) . . ? C34 C35 H35A 120.2 . . ? C36 C35 H35A 120.2 . . ? C35 C36 C31 120.2(8) . . ? C35 C36 H36A 119.9 . . ? C31 C36 H36A 119.9 . . ? N3 C37 C38 122.9(6) . . ? N3 C37 H37A 118.6 . . ? C38 C37 H37A 118.6 . . ? C39 C38 C37 119.9(6) . . ? C39 C38 H38A 120.1 . . ? C37 C38 H38A 120.1 . . ? C38 C39 C40 119.8(5) . . ? C38 C39 H39A 120.1 . . ? C40 C39 H39A 120.1 . . ? C39 C40 C41 116.8(5) . . ? C39 C40 C42 123.5(5) . . ? C41 C40 C42 119.6(5) . . ? N3 C41 C40 123.5(5) . . ? N3 C41 C45 117.9(5) . . ? C40 C41 C45 118.6(5) . . ? C43 C42 C40 120.6(5) . . ? C43 C42 H42A 119.7 . . ? C40 C42 H42A 119.7 . . ? C42 C43 C44 121.8(5) . . ? C42 C43 H43A 119.1 . . ? C44 C43 H43A 119.1 . . ? C46 C44 C45 118.5(5) . . ? C46 C44 C43 123.3(5) . . ? C45 C44 C43 118.1(5) . . ? N4 C45 C44 122.0(5) . . ? N4 C45 C41 116.9(5) . . ? C44 C45 C41 121.1(5) . . ? C47 C46 C44 118.9(5) . . ? C47 C46 H46A 120.6 . . ? C44 C46 H46A 120.6 . . ? C46 C47 C48 119.7(5) . . ? C46 C47 H47A 120.1 . . ? C48 C47 H47A 120.1 . . ? N4 C48 C47 123.2(5) . . ? N4 C48 H48A 118.4 . . ? C47 C48 H48A 118.4 . . ? C51 N5 C50 124.1(12) . . ? C51 N5 C49 121.5(11) . . ? C50 N5 C49 114.4(11) . . ? N5 C49 H49A 109.5 . . ? N5 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? N5 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? N5 C50 H50A 109.5 . . ? N5 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? N5 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? O5 C51 N5 125.2(13) . . ? O5 C51 H51A 117.4 . . ? N5 C51 H51A 117.4 . . ? O4 Cl1 O1 108.3(9) . . ? O4 Cl1 O2 111.4(8) . . ? O1 Cl1 O2 107.3(6) . . ? O4 Cl1 O3 109.2(4) . . ? O1 Cl1 O3 110.2(5) . . ? O2 Cl1 O3 110.3(4) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 0.695 _refine_diff_density_min -0.460 _refine_diff_density_rms 0.092 # Attachment '- complex 4.CIF' data_4 _database_code_depnum_ccdc_archive 'CCDC 822793' #TrackingRef '- complex 4.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H45 Cl2 Cu2 N7 O8 P2, 0.68C4H10O' _chemical_formula_sum 'C48.72 H51.8 Cl2 Cu2 N7 O8.68 P2' _chemical_formula_weight 1134.24 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' 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 'P 21/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 11.357(3) _cell_length_b 37.356(6) _cell_length_c 12.909(2) _cell_angle_alpha 90.00 _cell_angle_beta 112.442(3) _cell_angle_gamma 90.00 _cell_volume 5062.3(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 2.87 _cell_measurement_theta_max 27.48 _exptl_crystal_description block _exptl_crystal_colour orange-red _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.52 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2224 _exptl_absorpt_coefficient_mu 1.066 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.663027 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker APEX CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30108 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0500 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -37 _diffrn_reflns_limit_k_max 47 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 27.06 _reflns_number_total 11006 _reflns_number_gt 7799 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1013P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11006 _refine_ls_number_parameters 607 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0781 _refine_ls_R_factor_gt 0.0549 _refine_ls_wR_factor_ref 0.1680 _refine_ls_wR_factor_gt 0.1560 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.079 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 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 0.74556(4) 0.128657(11) 0.43269(4) 0.02839(14) Uani 1 1 d . . . Cu2 Cu 0.79069(4) 0.311556(12) 0.44408(4) 0.03209(14) Uani 1 1 d . . . P1 P 0.85427(8) 0.10109(2) 0.34654(8) 0.0241(2) Uani 1 1 d . . . P2 P 0.64590(9) 0.34969(2) 0.34329(8) 0.0253(2) Uani 1 1 d . . . N1 N 0.9049(3) 0.16464(8) 0.2576(2) 0.0262(6) Uani 1 1 d . . . H1A H 0.9774 0.1753 0.2968 0.031 Uiso 1 1 calc R . . N2 N 0.6033(3) 0.30390(8) 0.1649(3) 0.0308(7) Uani 1 1 d . . . H2B H 0.5294 0.2939 0.1259 0.037 Uiso 1 1 calc R . . N3 N 0.7523(3) 0.18329(8) 0.4493(2) 0.0253(6) Uani 1 1 d . . . N4 N 0.7697(3) 0.25796(8) 0.4588(2) 0.0242(6) Uani 1 1 d . . . N5 N 0.5661(3) 0.11806(10) 0.4100(3) 0.0434(8) Uani 1 1 d . . . N6 N 0.8416(3) 0.11420(9) 0.6017(3) 0.0398(8) Uani 1 1 d . . . N7 N 0.9759(3) 0.31756(8) 0.5330(3) 0.0358(7) Uani 1 1 d . . . C1 C 0.7979(3) 0.18532(9) 0.2119(3) 0.0238(7) Uani 1 1 d . . . C2 C 0.6780(3) 0.17055(10) 0.1591(3) 0.0282(8) Uani 1 1 d . . . H2A H 0.6695 0.1454 0.1487 0.034 Uiso 1 1 calc R . . C3 C 0.5695(3) 0.19200(10) 0.1210(3) 0.0306(8) Uani 1 1 d . . . H3A H 0.4883 0.1812 0.0857 0.037 Uiso 1 1 calc R . . C4 C 0.5776(3) 0.22794(10) 0.1333(3) 0.0277(8) Uani 1 1 d . . . H4A H 0.5020 0.2420 0.1078 0.033 Uiso 1 1 calc R . . C5 C 0.6982(3) 0.24498(9) 0.1841(3) 0.0225(7) Uani 1 1 d . . . C6 C 0.8102(3) 0.22341(9) 0.2223(3) 0.0221(7) Uani 1 1 d . . . C7 C 0.9310(3) 0.24015(9) 0.2708(3) 0.0242(7) Uani 1 1 d . . . H7A H 1.0062 0.2260 0.2953 0.029 Uiso 1 1 calc R . . C8 C 0.9403(3) 0.27629(9) 0.2826(3) 0.0261(7) Uani 1 1 d . . . H8A H 1.0223 0.2870 0.3146 0.031 Uiso 1 1 calc R . . C9 C 0.8313(3) 0.29833(9) 0.2484(3) 0.0257(7) Uani 1 1 d . . . H9A H 0.8398 0.3235 0.2595 0.031 Uiso 1 1 calc R . . C10 C 0.7116(3) 0.28305(9) 0.1984(3) 0.0235(7) Uani 1 1 d . . . C11 C 0.9049(4) 0.12629(9) 0.2446(3) 0.0290(8) Uani 1 1 d . . . H11A H 0.9917 0.1185 0.2542 0.035 Uiso 1 1 calc R . . H11B H 0.8469 0.1200 0.1675 0.035 Uiso 1 1 calc R . . C12 C 1.0053(3) 0.08711(9) 0.4554(3) 0.0258(7) Uani 1 1 d . . . C13 C 1.0281(4) 0.05280(10) 0.4975(3) 0.0352(9) Uani 1 1 d . . . H13A H 0.9684 0.0344 0.4622 0.042 Uiso 1 1 calc R . . C14 C 1.1358(4) 0.04460(11) 0.5897(3) 0.0417(10) Uani 1 1 d . . . H14A H 1.1496 0.0207 0.6172 0.050 Uiso 1 1 calc R . . C15 C 1.2236(4) 0.07084(12) 0.6424(3) 0.0400(9) Uani 1 1 d . . . H15A H 1.2978 0.0652 0.7061 0.048 Uiso 1 1 calc R . . C16 C 1.2027(3) 0.10529(11) 0.6019(3) 0.0349(9) Uani 1 1 d . . . H16A H 1.2626 0.1236 0.6378 0.042 Uiso 1 1 calc R . . C17 C 1.0935(3) 0.11348(10) 0.5078(3) 0.0314(8) Uani 1 1 d . . . H17A H 1.0798 0.1373 0.4797 0.038 Uiso 1 1 calc R . . C18 C 0.7868(4) 0.06113(9) 0.2646(3) 0.0294(8) Uani 1 1 d . . . C19 C 0.6588(4) 0.05428(12) 0.2341(3) 0.0449(10) Uani 1 1 d . . . H19A H 0.6087 0.0693 0.2604 0.054 Uiso 1 1 calc R . . C20 C 0.6029(5) 0.02543(14) 0.1651(4) 0.0579(13) Uani 1 1 d . . . H20A H 0.5141 0.0213 0.1433 0.069 Uiso 1 1 calc R . . C21 C 0.6726(6) 0.00311(13) 0.1282(4) 0.0627(15) Uani 1 1 d . . . H21A H 0.6336 -0.0170 0.0829 0.075 Uiso 1 1 calc R . . C22 C 0.8004(5) 0.00979(11) 0.1569(4) 0.0527(13) Uani 1 1 d . . . H22A H 0.8492 -0.0055 0.1300 0.063 Uiso 1 1 calc R . . C23 C 0.8586(4) 0.03876(10) 0.2251(3) 0.0388(9) Uani 1 1 d . . . H23A H 0.9468 0.0432 0.2445 0.047 Uiso 1 1 calc R . . C24 C 0.6065(4) 0.34130(10) 0.1913(3) 0.0311(8) Uani 1 1 d . . . H24A H 0.5224 0.3520 0.1474 0.037 Uiso 1 1 calc R . . H24B H 0.6706 0.3533 0.1687 0.037 Uiso 1 1 calc R . . C25 C 0.6835(4) 0.39676(9) 0.3509(3) 0.0309(8) Uani 1 1 d . . . C26 C 0.6002(4) 0.42113(10) 0.2769(4) 0.0407(10) Uani 1 1 d . . . H26A H 0.5225 0.4128 0.2216 0.049 Uiso 1 1 calc R . . C27 C 0.6292(5) 0.45715(12) 0.2830(4) 0.0535(12) Uani 1 1 d . . . H27A H 0.5720 0.4735 0.2320 0.064 Uiso 1 1 calc R . . C28 C 0.7424(6) 0.46934(12) 0.3643(5) 0.0605(14) Uani 1 1 d . . . H28A H 0.7621 0.4941 0.3692 0.073 Uiso 1 1 calc R . . C29 C 0.8259(5) 0.44579(13) 0.4375(4) 0.0537(13) Uani 1 1 d . . . H29A H 0.9031 0.4544 0.4926 0.064 Uiso 1 1 calc R . . C30 C 0.7979(4) 0.40922(11) 0.4314(4) 0.0403(10) Uani 1 1 d . . . H30A H 0.8563 0.3929 0.4817 0.048 Uiso 1 1 calc R . . C31 C 0.4901(3) 0.34858(10) 0.3539(3) 0.0294(8) Uani 1 1 d . . . C32 C 0.4089(4) 0.31987(11) 0.3096(3) 0.0358(9) Uani 1 1 d . . . H32A H 0.4329 0.3013 0.2711 0.043 Uiso 1 1 calc R . . C33 C 0.2923(4) 0.31818(12) 0.3214(4) 0.0473(11) Uani 1 1 d . . . H33A H 0.2372 0.2984 0.2918 0.057 Uiso 1 1 calc R . . C34 C 0.2567(4) 0.34532(14) 0.3762(4) 0.0543(13) Uani 1 1 d . . . H34A H 0.1760 0.3445 0.3824 0.065 Uiso 1 1 calc R . . C35 C 0.3377(4) 0.37351(12) 0.4218(4) 0.0485(12) Uani 1 1 d . . . H35A H 0.3137 0.3917 0.4612 0.058 Uiso 1 1 calc R . . C36 C 0.4540(4) 0.37559(11) 0.4106(3) 0.0371(9) Uani 1 1 d . . . H36A H 0.5091 0.3953 0.4414 0.044 Uiso 1 1 calc R . . C37 C 0.6493(3) 0.20442(10) 0.4135(3) 0.0263(7) Uani 1 1 d . . . H37A H 0.5674 0.1937 0.3837 0.032 Uiso 1 1 calc R . . C38 C 0.6580(3) 0.24093(9) 0.4183(3) 0.0265(7) Uani 1 1 d . . . H38A H 0.5818 0.2547 0.3919 0.032 Uiso 1 1 calc R . . C39 C 0.8739(3) 0.23684(9) 0.4967(3) 0.0263(7) Uani 1 1 d . . . H39A H 0.9558 0.2476 0.5274 0.032 Uiso 1 1 calc R . . C40 C 0.8643(3) 0.20044(10) 0.4921(3) 0.0266(7) Uani 1 1 d . . . H40A H 0.9402 0.1866 0.5204 0.032 Uiso 1 1 calc R . . C41 C 0.4692(5) 0.11083(17) 0.4082(4) 0.0667(16) Uani 1 1 d . . . C42 C 0.3457(6) 0.1007(3) 0.4088(6) 0.147(4) Uani 1 1 d . . . H42A H 0.3160 0.0788 0.3646 0.220 Uiso 1 1 calc R . . H42B H 0.2844 0.1200 0.3761 0.220 Uiso 1 1 calc R . . H42C H 0.3536 0.0964 0.4861 0.220 Uiso 1 1 calc R . . C43 C 0.9101(4) 0.10086(11) 0.6791(4) 0.0365(9) Uani 1 1 d . . . C44 C 1.0001(5) 0.08343(15) 0.7801(4) 0.0598(13) Uani 1 1 d . . . H44A H 1.0021 0.0965 0.8466 0.090 Uiso 1 1 calc R . . H44B H 1.0854 0.0835 0.7778 0.090 Uiso 1 1 calc R . . H44C H 0.9730 0.0587 0.7834 0.090 Uiso 1 1 calc R . . C45 C 1.0818(4) 0.31611(10) 0.5756(3) 0.0329(8) Uani 1 1 d . . . C46 C 1.2200(4) 0.31294(13) 0.6296(4) 0.0532(12) Uani 1 1 d . . . H46A H 1.2429 0.3034 0.7054 0.080 Uiso 1 1 calc R . . H46B H 1.2589 0.3366 0.6337 0.080 Uiso 1 1 calc R . . H46C H 1.2511 0.2968 0.5859 0.080 Uiso 1 1 calc R . . Cl1 Cl 0.19171(11) 0.07514(3) 0.10882(9) 0.0461(3) Uani 1 1 d . . . O1 O 0.3207(4) 0.08463(16) 0.1657(3) 0.1050(18) Uani 1 1 d . . . O2 O 0.1440(4) 0.05783(12) 0.1821(3) 0.0820(12) Uani 1 1 d . . . O3 O 0.1791(5) 0.05333(10) 0.0163(3) 0.0841(13) Uani 1 1 d . . . O4 O 0.1196(4) 0.10664(10) 0.0633(4) 0.0952(14) Uani 1 1 d . . . Cl2 Cl 1.26422(11) 0.20759(4) 0.45055(11) 0.0623(4) Uani 1 1 d . . . O5 O 1.3691(6) 0.2138(3) 0.4178(7) 0.200(4) Uani 1 1 d . . . O6 O 1.2282(6) 0.24038(18) 0.4425(8) 0.211(5) Uani 1 1 d . . . O7 O 1.3324(7) 0.1890(2) 0.5446(6) 0.175(3) Uani 1 1 d . . . O8 O 1.1778(3) 0.18498(9) 0.3690(4) 0.0711(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 0.0292(3) 0.0268(2) 0.0328(3) -0.00300(18) 0.0160(2) -0.00092(18) Cu2 0.0303(3) 0.0257(2) 0.0359(3) 0.00566(18) 0.0077(2) 0.00231(18) P1 0.0263(5) 0.0227(4) 0.0248(5) -0.0036(3) 0.0113(4) -0.0018(3) P2 0.0276(5) 0.0235(4) 0.0269(5) 0.0039(4) 0.0127(4) 0.0031(3) N1 0.0221(15) 0.0259(15) 0.0273(16) 0.0024(12) 0.0058(12) -0.0009(12) N2 0.0277(16) 0.0302(16) 0.0295(17) -0.0030(13) 0.0052(13) 0.0064(12) N3 0.0297(16) 0.0264(15) 0.0227(15) 0.0004(11) 0.0132(13) -0.0004(12) N4 0.0307(16) 0.0277(15) 0.0158(14) 0.0044(11) 0.0107(12) 0.0038(12) N5 0.037(2) 0.050(2) 0.048(2) -0.0125(17) 0.0216(17) -0.0059(16) N6 0.051(2) 0.0391(19) 0.036(2) 0.0037(16) 0.0239(18) 0.0095(16) N7 0.0372(19) 0.0314(18) 0.0375(19) 0.0001(14) 0.0130(16) -0.0033(14) C1 0.0290(18) 0.0301(18) 0.0133(16) -0.0006(13) 0.0092(14) 0.0010(14) C2 0.0310(19) 0.0260(18) 0.0253(19) -0.0069(14) 0.0084(16) -0.0041(15) C3 0.0229(18) 0.039(2) 0.0249(19) -0.0054(15) 0.0029(15) -0.0045(15) C4 0.0243(18) 0.034(2) 0.0227(18) -0.0059(14) 0.0068(15) 0.0034(15) C5 0.0227(17) 0.0318(18) 0.0146(16) -0.0011(13) 0.0089(13) 0.0018(13) C6 0.0260(17) 0.0280(18) 0.0147(16) 0.0010(13) 0.0104(14) -0.0014(13) C7 0.0222(17) 0.0297(18) 0.0218(17) 0.0061(14) 0.0096(14) 0.0030(14) C8 0.0222(17) 0.0304(19) 0.0271(19) 0.0029(14) 0.0110(15) -0.0042(14) C9 0.0346(19) 0.0232(17) 0.0247(18) 0.0001(14) 0.0172(16) -0.0017(14) C10 0.0233(17) 0.0345(19) 0.0144(16) 0.0033(13) 0.0091(14) 0.0043(14) C11 0.0313(19) 0.0308(19) 0.0268(19) 0.0001(15) 0.0132(16) 0.0014(15) C12 0.0280(18) 0.0306(19) 0.0231(18) -0.0026(14) 0.0147(15) -0.0010(14) C13 0.042(2) 0.0257(19) 0.035(2) -0.0022(16) 0.0111(18) -0.0056(16) C14 0.052(3) 0.031(2) 0.036(2) 0.0043(17) 0.009(2) 0.0009(18) C15 0.035(2) 0.051(3) 0.033(2) 0.0035(18) 0.0110(18) 0.0048(18) C16 0.0246(19) 0.044(2) 0.036(2) -0.0071(17) 0.0109(17) -0.0080(16) C17 0.031(2) 0.0302(19) 0.037(2) -0.0030(16) 0.0177(17) -0.0052(15) C18 0.039(2) 0.0254(18) 0.0236(19) -0.0025(14) 0.0118(16) -0.0071(15) C19 0.048(3) 0.053(3) 0.034(2) -0.0068(19) 0.016(2) -0.014(2) C20 0.072(3) 0.059(3) 0.043(3) -0.015(2) 0.022(3) -0.033(3) C21 0.102(4) 0.045(3) 0.034(3) -0.010(2) 0.016(3) -0.030(3) C22 0.098(4) 0.029(2) 0.030(2) -0.0049(17) 0.023(2) 0.005(2) C23 0.060(3) 0.0249(19) 0.033(2) -0.0041(16) 0.020(2) -0.0013(18) C24 0.037(2) 0.032(2) 0.029(2) 0.0066(15) 0.0180(17) 0.0107(16) C25 0.044(2) 0.0233(18) 0.033(2) -0.0017(15) 0.0228(18) 0.0009(15) C26 0.050(3) 0.030(2) 0.044(2) 0.0066(17) 0.020(2) 0.0052(18) C27 0.080(3) 0.032(2) 0.061(3) 0.011(2) 0.041(3) 0.013(2) C28 0.100(4) 0.025(2) 0.077(4) -0.010(2) 0.056(3) -0.012(2) C29 0.067(3) 0.046(3) 0.060(3) -0.024(2) 0.037(3) -0.017(2) C30 0.048(2) 0.040(2) 0.042(2) -0.0058(18) 0.028(2) -0.0028(18) C31 0.0295(19) 0.033(2) 0.029(2) 0.0115(15) 0.0152(16) 0.0113(15) C32 0.032(2) 0.037(2) 0.042(2) 0.0046(17) 0.0185(18) 0.0013(16) C33 0.036(2) 0.051(3) 0.054(3) 0.010(2) 0.016(2) -0.0051(19) C34 0.042(3) 0.068(3) 0.066(3) 0.022(3) 0.036(2) 0.011(2) C35 0.053(3) 0.052(3) 0.056(3) 0.019(2) 0.038(2) 0.025(2) C36 0.042(2) 0.037(2) 0.036(2) 0.0085(17) 0.0194(19) 0.0097(17) C37 0.0242(18) 0.037(2) 0.0194(17) -0.0017(14) 0.0102(14) -0.0041(15) C38 0.0303(19) 0.0290(18) 0.0239(18) 0.0021(14) 0.0144(15) 0.0023(15) C39 0.0299(18) 0.0289(18) 0.0215(18) 0.0006(14) 0.0112(15) -0.0009(14) C40 0.0257(18) 0.0319(19) 0.0210(18) 0.0030(14) 0.0077(14) 0.0053(14) C41 0.046(3) 0.113(5) 0.050(3) -0.042(3) 0.027(2) -0.035(3) C42 0.071(4) 0.298(12) 0.100(6) -0.102(7) 0.065(4) -0.102(6) C43 0.044(2) 0.039(2) 0.038(2) 0.0014(18) 0.028(2) 0.0011(18) C44 0.057(3) 0.084(4) 0.039(3) 0.017(2) 0.018(2) 0.014(3) C45 0.036(2) 0.035(2) 0.026(2) 0.0023(15) 0.0095(17) -0.0033(16) C46 0.035(2) 0.063(3) 0.055(3) 0.007(2) 0.010(2) -0.001(2) Cl1 0.0554(7) 0.0437(6) 0.0399(6) -0.0024(4) 0.0191(5) 0.0065(5) O1 0.049(2) 0.214(6) 0.052(3) -0.001(3) 0.019(2) -0.012(3) O2 0.096(3) 0.098(3) 0.060(3) -0.001(2) 0.039(2) -0.032(2) O3 0.148(4) 0.052(2) 0.052(2) -0.0064(17) 0.038(2) 0.027(2) O4 0.111(3) 0.045(2) 0.134(4) 0.001(2) 0.050(3) 0.025(2) Cl2 0.0396(6) 0.0545(7) 0.0624(8) -0.0005(6) -0.0146(6) 0.0022(5) O5 0.104(5) 0.325(11) 0.187(8) -0.113(7) 0.075(5) -0.104(6) O6 0.122(5) 0.095(5) 0.297(11) -0.032(5) -0.056(6) 0.006(4) O7 0.140(5) 0.212(8) 0.105(5) 0.065(5) -0.029(4) -0.041(5) O8 0.0320(17) 0.060(2) 0.095(3) -0.0066(19) -0.0054(18) -0.0042(15) _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 N5 1.985(3) . ? Cu1 N3 2.051(3) . ? Cu1 N6 2.104(4) . ? Cu1 P1 2.2070(10) . ? Cu2 N7 1.988(4) . ? Cu2 N4 2.034(3) . ? Cu2 P2 2.1893(10) . ? P1 C18 1.821(4) . ? P1 C12 1.830(4) . ? P1 C11 1.877(4) . ? P2 C25 1.803(4) . ? P2 C31 1.826(3) . ? P2 C24 1.865(4) . ? N1 C1 1.369(4) . ? N1 C11 1.443(4) . ? N1 H1A 0.8800 . ? N2 C10 1.379(4) . ? N2 C24 1.435(4) . ? N2 H2B 0.8800 . ? N3 C37 1.338(4) . ? N3 C40 1.341(4) . ? N4 C38 1.335(4) . ? N4 C39 1.349(4) . ? N5 C41 1.125(5) . ? N6 C43 1.122(5) . ? N7 C45 1.116(5) . ? C1 C2 1.384(5) . ? C1 C6 1.431(5) . ? C2 C3 1.393(5) . ? C2 H2A 0.9500 . ? C3 C4 1.351(5) . ? C3 H3A 0.9500 . ? C4 C5 1.423(5) . ? C4 H4A 0.9500 . ? C5 C6 1.426(4) . ? C5 C10 1.434(5) . ? C6 C7 1.417(5) . ? C7 C8 1.358(5) . ? C7 H7A 0.9500 . ? C8 C9 1.410(5) . ? C8 H8A 0.9500 . ? C9 C10 1.386(5) . ? C9 H9A 0.9500 . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.378(5) . ? C12 C17 1.383(5) . ? C13 C14 1.377(6) . ? C13 H13A 0.9500 . ? C14 C15 1.379(6) . ? C14 H14A 0.9500 . ? C15 C16 1.375(6) . ? C15 H15A 0.9500 . ? C16 C17 1.399(5) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? C18 C19 1.378(5) . ? C18 C23 1.393(5) . ? C19 C20 1.388(6) . ? C19 H19A 0.9500 . ? C20 C21 1.355(7) . ? C20 H20A 0.9500 . ? C21 C22 1.377(7) . ? C21 H21A 0.9500 . ? C22 C23 1.392(6) . ? C22 H22A 0.9500 . ? C23 H23A 0.9500 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? C25 C26 1.395(5) . ? C25 C30 1.398(5) . ? C26 C27 1.381(6) . ? C26 H26A 0.9500 . ? C27 C28 1.390(7) . ? C27 H27A 0.9500 . ? C28 C29 1.371(7) . ? C28 H28A 0.9500 . ? C29 C30 1.398(6) . ? C29 H29A 0.9500 . ? C30 H30A 0.9500 . ? C31 C32 1.388(5) . ? C31 C36 1.397(5) . ? C32 C33 1.391(5) . ? C32 H32A 0.9500 . ? C33 C34 1.382(7) . ? C33 H33A 0.9500 . ? C34 C35 1.374(7) . ? C34 H34A 0.9500 . ? C35 C36 1.385(6) . ? C35 H35A 0.9500 . ? C36 H36A 0.9500 . ? C37 C38 1.367(5) . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C40 1.364(5) . ? C39 H39A 0.9500 . ? C40 H40A 0.9500 . ? C41 C42 1.455(6) . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.467(6) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 C46 1.459(6) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? Cl1 O3 1.407(4) . ? Cl1 O1 1.410(4) . ? Cl1 O2 1.413(4) . ? Cl1 O4 1.426(4) . ? Cl2 O6 1.283(7) . ? Cl2 O7 1.356(6) . ? Cl2 O8 1.413(4) . ? Cl2 O5 1.427(6) . ? 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 N5 Cu1 N3 102.08(13) . . ? N5 Cu1 N6 101.45(15) . . ? N3 Cu1 N6 99.41(12) . . ? N5 Cu1 P1 124.95(10) . . ? N3 Cu1 P1 120.76(8) . . ? N6 Cu1 P1 103.57(9) . . ? N7 Cu2 N4 101.13(12) . . ? N7 Cu2 P2 131.24(10) . . ? N4 Cu2 P2 127.44(9) . . ? C18 P1 C12 105.99(17) . . ? C18 P1 C11 100.22(16) . . ? C12 P1 C11 103.47(16) . . ? C18 P1 Cu1 118.89(12) . . ? C12 P1 Cu1 106.68(11) . . ? C11 P1 Cu1 119.93(12) . . ? C25 P2 C31 103.53(17) . . ? C25 P2 C24 100.26(16) . . ? C31 P2 C24 102.98(17) . . ? C25 P2 Cu2 119.58(13) . . ? C31 P2 Cu2 118.04(11) . . ? C24 P2 Cu2 109.89(11) . . ? C1 N1 C11 123.3(3) . . ? C1 N1 H1A 118.3 . . ? C11 N1 H1A 118.3 . . ? C10 N2 C24 122.5(3) . . ? C10 N2 H2B 118.8 . . ? C24 N2 H2B 118.8 . . ? C37 N3 C40 115.3(3) . . ? C37 N3 Cu1 123.9(2) . . ? C40 N3 Cu1 120.7(2) . . ? C38 N4 C39 115.7(3) . . ? C38 N4 Cu2 124.1(2) . . ? C39 N4 Cu2 119.5(2) . . ? C41 N5 Cu1 172.8(4) . . ? C43 N6 Cu1 161.1(3) . . ? C45 N7 Cu2 169.3(3) . . ? N1 C1 C2 122.2(3) . . ? N1 C1 C6 118.8(3) . . ? C2 C1 C6 119.0(3) . . ? C1 C2 C3 121.1(3) . . ? C1 C2 H2A 119.5 . . ? C3 C2 H2A 119.5 . . ? C4 C3 C2 121.3(3) . . ? C4 C3 H3A 119.3 . . ? C2 C3 H3A 119.3 . . ? C3 C4 C5 120.6(3) . . ? C3 C4 H4A 119.7 . . ? C5 C4 H4A 119.7 . . ? C4 C5 C6 118.8(3) . . ? C4 C5 C10 122.6(3) . . ? C6 C5 C10 118.6(3) . . ? C7 C6 C5 119.3(3) . . ? C7 C6 C1 121.6(3) . . ? C5 C6 C1 119.2(3) . . ? C8 C7 C6 120.6(3) . . ? C8 C7 H7A 119.7 . . ? C6 C7 H7A 119.7 . . ? C7 C8 C9 121.6(3) . . ? C7 C8 H8A 119.2 . . ? C9 C8 H8A 119.2 . . ? C10 C9 C8 119.6(3) . . ? C10 C9 H9A 120.2 . . ? C8 C9 H9A 120.2 . . ? N2 C10 C9 120.8(3) . . ? N2 C10 C5 118.8(3) . . ? C9 C10 C5 120.4(3) . . ? N1 C11 P1 113.8(2) . . ? N1 C11 H11A 108.8 . . ? P1 C11 H11A 108.8 . . ? N1 C11 H11B 108.8 . . ? P1 C11 H11B 108.8 . . ? H11A C11 H11B 107.7 . . ? C13 C12 C17 118.6(3) . . ? C13 C12 P1 123.2(3) . . ? C17 C12 P1 117.6(3) . . ? C14 C13 C12 121.3(4) . . ? C14 C13 H13A 119.4 . . ? C12 C13 H13A 119.4 . . ? C13 C14 C15 120.3(4) . . ? C13 C14 H14A 119.8 . . ? C15 C14 H14A 119.8 . . ? C16 C15 C14 119.4(4) . . ? C16 C15 H15A 120.3 . . ? C14 C15 H15A 120.3 . . ? C15 C16 C17 120.1(4) . . ? C15 C16 H16A 119.9 . . ? C17 C16 H16A 119.9 . . ? C12 C17 C16 120.3(4) . . ? C12 C17 H17A 119.8 . . ? C16 C17 H17A 119.8 . . ? C19 C18 C23 119.1(4) . . ? C19 C18 P1 118.8(3) . . ? C23 C18 P1 121.9(3) . . ? C18 C19 C20 120.1(4) . . ? C18 C19 H19A 119.9 . . ? C20 C19 H19A 119.9 . . ? C21 C20 C19 121.2(5) . . ? C21 C20 H20A 119.4 . . ? C19 C20 H20A 119.4 . . ? C20 C21 C22 119.4(4) . . ? C20 C21 H21A 120.3 . . ? C22 C21 H21A 120.3 . . ? C21 C22 C23 120.6(4) . . ? C21 C22 H22A 119.7 . . ? C23 C22 H22A 119.7 . . ? C22 C23 C18 119.6(4) . . ? C22 C23 H23A 120.2 . . ? C18 C23 H23A 120.2 . . ? N2 C24 P2 112.8(2) . . ? N2 C24 H24A 109.0 . . ? P2 C24 H24A 109.0 . . ? N2 C24 H24B 109.0 . . ? P2 C24 H24B 109.0 . . ? H24A C24 H24B 107.8 . . ? C26 C25 C30 119.1(4) . . ? C26 C25 P2 120.9(3) . . ? C30 C25 P2 119.9(3) . . ? C27 C26 C25 120.8(4) . . ? C27 C26 H26A 119.6 . . ? C25 C26 H26A 119.6 . . ? C26 C27 C28 119.6(4) . . ? C26 C27 H27A 120.2 . . ? C28 C27 H27A 120.2 . . ? C29 C28 C27 120.5(4) . . ? C29 C28 H28A 119.8 . . ? C27 C28 H28A 119.8 . . ? C28 C29 C30 120.4(5) . . ? C28 C29 H29A 119.8 . . ? C30 C29 H29A 119.8 . . ? C25 C30 C29 119.6(4) . . ? C25 C30 H30A 120.2 . . ? C29 C30 H30A 120.2 . . ? C32 C31 C36 119.5(3) . . ? C32 C31 P2 119.8(3) . . ? C36 C31 P2 120.6(3) . . ? C31 C32 C33 120.0(4) . . ? C31 C32 H32A 120.0 . . ? C33 C32 H32A 120.0 . . ? C34 C33 C32 120.0(4) . . ? C34 C33 H33A 120.0 . . ? C32 C33 H33A 120.0 . . ? C35 C34 C33 120.1(4) . . ? C35 C34 H34A 119.9 . . ? C33 C34 H34A 119.9 . . ? C34 C35 C36 120.5(4) . . ? C34 C35 H35A 119.7 . . ? C36 C35 H35A 119.7 . . ? C35 C36 C31 119.8(4) . . ? C35 C36 H36A 120.1 . . ? C31 C36 H36A 120.1 . . ? N3 C37 C38 122.3(3) . . ? N3 C37 H37A 118.8 . . ? C38 C37 H37A 118.8 . . ? N4 C38 C37 122.3(3) . . ? N4 C38 H38A 118.9 . . ? C37 C38 H38A 118.9 . . ? N4 C39 C40 121.5(3) . . ? N4 C39 H39A 119.2 . . ? C40 C39 H39A 119.2 . . ? N3 C40 C39 122.8(3) . . ? N3 C40 H40A 118.6 . . ? C39 C40 H40A 118.6 . . ? N5 C41 C42 178.2(8) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N6 C43 C44 179.8(5) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N7 C45 C46 178.0(4) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O3 Cl1 O1 109.6(3) . . ? O3 Cl1 O2 111.2(3) . . ? O1 Cl1 O2 110.8(3) . . ? O3 Cl1 O4 105.8(3) . . ? O1 Cl1 O4 109.0(3) . . ? O2 Cl1 O4 110.3(3) . . ? O6 Cl2 O7 128.1(6) . . ? O6 Cl2 O8 113.6(3) . . ? O7 Cl2 O8 111.0(4) . . ? O6 Cl2 O5 95.6(6) . . ? O7 Cl2 O5 95.3(5) . . ? O8 Cl2 O5 107.3(3) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.06 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 1.616 _refine_diff_density_min -1.153 _refine_diff_density_rms 0.108 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.500 1.000 174 57 ' ' 2 0.500 1.000 0.500 174 57 ' ' _platon_squeeze_details ; ; # start Validation Reply Form _vrf_CHEMW)3 ; PROBLEM: The ratio of given/expected molecular weight as calculated from the _atom_site* data lies outside the range 0.95 <> 1.05 From the CIF: _cell_formula_units_Z 4 From the CIF: _chemical_formula_weight 1157.93 TEST: Calculate formula weight from _atom_site_* atom mass num sum C 12.01 46.00 552.51 H 1.01 45.00 45.36 N 14.01 7.00 98.05 O 16.00 8.00 127.99 P 30.97 2.00 61.95 Cl 35.45 2.00 70.91 Cu 63.55 2.00 127.09 Calculated formula weight 1083.85 _vrf_PLAT043_1 PROBLEM: Check Reported Molecular Weight ................ 1157.93 RESPONSE: due to the solvent ethyl ether being removed by the SQUEEZE process, so the reported molecular formula, formula weight, etc., are inconsistent with those calculated by CIF. ; # end Validation Reply Form # Attachment '- complex 5.CIF' data_5 _database_code_depnum_ccdc_archive 'CCDC 822794' #TrackingRef '- complex 5.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C87 H91 Cl2 Cu2 N7 O12 P4' _chemical_formula_weight 1748.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _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 10.913(1) _cell_length_b 17.535(1) _cell_length_c 22.068(1) _cell_angle_alpha 86.442(1) _cell_angle_beta 84.066(1) _cell_angle_gamma 77.951(1) _cell_volume 4104.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 3.25 _cell_measurement_theta_max 27.9 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.415 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1820 _exptl_absorpt_coefficient_mu 0.728 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8504 _exptl_absorpt_correction_T_max 0.9308 _exptl_absorpt_process_details ? _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31620 _diffrn_reflns_av_R_equivalents 0.0593 _diffrn_reflns_av_sigmaI/netI 0.0842 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.00 _diffrn_reflns_theta_max 25.01 _reflns_number_total 14162 _reflns_number_gt 7978 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1636P)^2^+6.5886P] 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 constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0134(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 14162 _refine_ls_number_parameters 1033 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1547 _refine_ls_R_factor_gt 0.0870 _refine_ls_wR_factor_ref 0.3121 _refine_ls_wR_factor_gt 0.2211 _refine_ls_goodness_of_fit_ref 1.149 _refine_ls_restrained_S_all 1.149 _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 -0.04723(9) 0.53310(6) 0.30369(4) 0.0393(3) Uani 1 1 d . . . Cu2 Cu 0.18841(9) 0.84522(6) 0.17859(4) 0.0401(3) Uani 1 1 d . . . P1 P 0.07362(19) 0.41405(12) 0.28619(9) 0.0397(5) Uani 1 1 d . . . P2 P 0.2533(2) 0.91948(12) 0.24356(9) 0.0420(5) Uani 1 1 d . . . P3 P 0.20968(19) 0.86406(13) 0.07717(9) 0.0402(5) Uani 1 1 d . . . P4 P -0.23879(19) 0.57171(12) 0.35489(9) 0.0394(5) Uani 1 1 d . . . N1 N 0.0242(6) 0.6257(4) 0.2698(3) 0.0419(15) Uani 1 1 d . . . N2 N 0.1137(5) 0.7571(4) 0.2169(3) 0.0381(15) Uani 1 1 d . . . N4 N 0.3417(6) 0.7968(4) 0.3203(3) 0.0458(16) Uani 1 1 d . . . H3B H 0.3107 0.7966 0.3577 0.055 Uiso 1 1 calc R . . N3 N 0.2968(6) 0.4635(4) 0.2802(3) 0.0444(16) Uani 1 1 d . . . H4B H 0.3387 0.4616 0.2449 0.053 Uiso 1 1 calc R . . N5 N 0.0193(6) 0.7887(4) 0.0539(3) 0.0428(16) Uani 1 1 d . . . H5A H 0.0306 0.7442 0.0376 0.051 Uiso 1 1 calc R . . N6 N -0.3058(6) 0.7022(4) 0.2793(3) 0.0420(15) Uani 1 1 d . . . H6A H -0.3159 0.7473 0.2947 0.050 Uiso 1 1 calc R . . C1 C 0.0024(7) 0.6955(5) 0.2976(3) 0.0382(17) Uani 1 1 d . . . H1A H -0.0439 0.7002 0.3355 0.046 Uiso 1 1 calc R . . C2 C 0.0459(7) 0.7575(4) 0.2719(3) 0.0370(17) Uani 1 1 d . . . H2A H 0.0283 0.8033 0.2931 0.044 Uiso 1 1 calc R . . C3 C 0.0914(6) 0.6259(4) 0.2149(3) 0.0333(16) Uani 1 1 d . . . H3A H 0.1085 0.5802 0.1934 0.040 Uiso 1 1 calc R . . C4 C 0.1355(7) 0.6877(5) 0.1890(3) 0.0386(17) Uani 1 1 d . . . H4A H 0.1820 0.6829 0.1512 0.046 Uiso 1 1 calc R . . C5 C 0.3380(7) 0.5919(5) 0.2862(3) 0.0383(17) Uani 1 1 d . . . C6 C 0.2874(7) 0.5280(5) 0.3141(3) 0.0402(18) Uani 1 1 d . . . C7 C 0.2280(7) 0.5336(5) 0.3730(3) 0.0422(18) Uani 1 1 d . . . H7A H 0.1939 0.4924 0.3910 0.051 Uiso 1 1 calc R . . C8 C 0.2193(8) 0.6014(5) 0.4055(3) 0.047(2) Uani 1 1 d . . . H8A H 0.1835 0.6033 0.4456 0.057 Uiso 1 1 calc R . . C9 C 0.2621(8) 0.6637(5) 0.3795(3) 0.046(2) Uani 1 1 d . . . H9A H 0.2526 0.7084 0.4015 0.056 Uiso 1 1 calc R . . C10 C 0.3208(7) 0.6623(5) 0.3195(3) 0.0396(17) Uani 1 1 d . . . C11 C 0.3609(7) 0.7283(5) 0.2892(3) 0.0387(17) Uani 1 1 d . . . C12 C 0.4177(7) 0.7242(5) 0.2297(3) 0.0396(18) Uani 1 1 d . . . H12A H 0.4416 0.7680 0.2100 0.047 Uiso 1 1 calc R . . C13 C 0.4388(7) 0.6542(5) 0.1996(3) 0.0415(18) Uani 1 1 d . . . H13A H 0.4809 0.6513 0.1607 0.050 Uiso 1 1 calc R . . C14 C 0.3990(7) 0.5899(5) 0.2259(3) 0.0412(18) Uani 1 1 d . . . H14A H 0.4119 0.5446 0.2043 0.049 Uiso 1 1 calc R . . C15 C 0.2382(8) 0.3988(5) 0.3020(4) 0.0444(19) Uani 1 1 d . . . H15A H 0.2431 0.3910 0.3457 0.053 Uiso 1 1 calc R . . H15B H 0.2847 0.3517 0.2830 0.053 Uiso 1 1 calc R . . C16 C 0.0803(8) 0.3872(4) 0.2071(3) 0.0387(17) Uani 1 1 d . . . C17 C 0.1924(8) 0.3612(6) 0.1714(4) 0.052(2) Uani 1 1 d . . . H17A H 0.2689 0.3611 0.1864 0.062 Uiso 1 1 calc R . . C18 C 0.1901(10) 0.3350(6) 0.1129(4) 0.070(3) Uani 1 1 d . . . H18A H 0.2651 0.3172 0.0893 0.084 Uiso 1 1 calc R . . C19 C 0.0762(10) 0.3357(6) 0.0904(4) 0.060(2) Uani 1 1 d . . . H19A H 0.0740 0.3179 0.0518 0.072 Uiso 1 1 calc R . . C20 C -0.0333(9) 0.3630(6) 0.1255(4) 0.061(2) Uani 1 1 d . . . H20A H -0.1102 0.3640 0.1106 0.073 Uiso 1 1 calc R . . C21 C -0.0302(8) 0.3888(6) 0.1826(4) 0.055(2) Uani 1 1 d . . . H21A H -0.1058 0.4079 0.2054 0.067 Uiso 1 1 calc R . . C22 C 0.0204(7) 0.3332(4) 0.3267(3) 0.0395(17) Uani 1 1 d . . . C23 C 0.0878(9) 0.2555(5) 0.3177(4) 0.058(2) Uani 1 1 d . . . H23A H 0.1589 0.2468 0.2900 0.070 Uiso 1 1 calc R . . C24 C 0.0499(11) 0.1924(5) 0.3494(4) 0.067(3) Uani 1 1 d . . . H24A H 0.0941 0.1418 0.3427 0.080 Uiso 1 1 calc R . . C25 C -0.0560(10) 0.2062(6) 0.3918(4) 0.066(3) Uani 1 1 d . . . H25A H -0.0846 0.1643 0.4123 0.079 Uiso 1 1 calc R . . C26 C -0.1179(9) 0.2808(6) 0.4033(4) 0.059(2) Uani 1 1 d . . . H26A H -0.1864 0.2899 0.4325 0.071 Uiso 1 1 calc R . . C27 C -0.0776(8) 0.3425(5) 0.3711(4) 0.0467(19) Uani 1 1 d . . . H27A H -0.1194 0.3929 0.3802 0.056 Uiso 1 1 calc R . . C28 C 0.3710(7) 0.8673(5) 0.2930(3) 0.0397(18) Uani 1 1 d . . . H28A H 0.4520 0.8553 0.2693 0.048 Uiso 1 1 calc R . . H28B H 0.3783 0.9012 0.3250 0.048 Uiso 1 1 calc R . . C29 C 0.1180(9) 0.9586(5) 0.2947(4) 0.050(2) Uani 1 1 d . . . C30 C 0.1242(10) 0.9715(5) 0.3566(4) 0.056(2) Uani 1 1 d . . . H30A H 0.2010 0.9610 0.3734 0.067 Uiso 1 1 calc R . . C31 C 0.0112(10) 1.0007(6) 0.3926(4) 0.062(3) Uani 1 1 d . . . H31A H 0.0136 1.0092 0.4336 0.075 Uiso 1 1 calc R . . C32 C -0.1009(10) 1.0165(6) 0.3679(4) 0.063(3) Uani 1 1 d . . . H32A H -0.1741 1.0360 0.3923 0.075 Uiso 1 1 calc R . . C33 C -0.1079(9) 1.0044(6) 0.3081(4) 0.061(2) Uani 1 1 d . . . H33A H -0.1852 1.0156 0.2918 0.073 Uiso 1 1 calc R . . C34 C 0.0003(9) 0.9755(6) 0.2721(4) 0.057(2) Uani 1 1 d . . . H34A H -0.0053 0.9670 0.2314 0.068 Uiso 1 1 calc R . . C35 C 0.3229(8) 1.0009(5) 0.2144(3) 0.0459(19) Uani 1 1 d . . . C36 C 0.2581(9) 1.0778(5) 0.2169(4) 0.056(2) Uani 1 1 d . . . H36A H 0.1760 1.0883 0.2352 0.067 Uiso 1 1 calc R . . C37 C 0.3114(11) 1.1391(6) 0.1932(4) 0.065(3) Uani 1 1 d . . . H37A H 0.2651 1.1900 0.1950 0.078 Uiso 1 1 calc R . . C38 C 0.4326(11) 1.1249(6) 0.1669(4) 0.067(3) Uani 1 1 d . . . H38A H 0.4691 1.1665 0.1518 0.080 Uiso 1 1 calc R . . C39 C 0.5009(10) 1.0500(6) 0.1624(4) 0.062(3) Uani 1 1 d . . . H39A H 0.5827 1.0405 0.1436 0.074 Uiso 1 1 calc R . . C40 C 0.4462(9) 0.9887(5) 0.1864(4) 0.053(2) Uani 1 1 d . . . H40A H 0.4928 0.9380 0.1837 0.063 Uiso 1 1 calc R . . C41 C -0.1226(7) 0.7419(4) 0.1333(3) 0.0371(17) Uani 1 1 d . . . C42 C -0.0677(7) 0.8044(4) 0.1044(3) 0.0373(17) Uani 1 1 d . . . C43 C -0.1061(7) 0.8794(5) 0.1258(4) 0.0419(18) Uani 1 1 d . . . H43A H -0.0770 0.9209 0.1051 0.050 Uiso 1 1 calc R . . C44 C -0.1890(7) 0.8919(5) 0.1787(3) 0.0446(19) Uani 1 1 d . . . H44A H -0.2148 0.9423 0.1924 0.054 Uiso 1 1 calc R . . C45 C -0.2331(8) 0.8328(5) 0.2107(4) 0.0446(19) Uani 1 1 d . . . H45A H -0.2853 0.8429 0.2466 0.054 Uiso 1 1 calc R . . C46 C -0.1993(7) 0.7552(4) 0.1893(3) 0.0360(16) Uani 1 1 d . . . C47 C -0.2422(7) 0.6914(5) 0.2218(3) 0.0398(18) Uani 1 1 d . . . C48 C -0.2213(7) 0.6199(5) 0.1953(4) 0.0434(19) Uani 1 1 d . . . H48A H -0.2538 0.5790 0.2150 0.052 Uiso 1 1 calc R . . C49 C -0.1508(7) 0.6094(5) 0.1384(3) 0.0427(19) Uani 1 1 d . . . H49A H -0.1379 0.5612 0.1208 0.051 Uiso 1 1 calc R . . C50 C -0.1010(7) 0.6672(5) 0.1083(3) 0.0413(18) Uani 1 1 d . . . H50A H -0.0527 0.6578 0.0713 0.050 Uiso 1 1 calc R . . C51 C 0.0908(8) 0.8449(5) 0.0281(4) 0.048(2) Uani 1 1 d . . . H51A H 0.0331 0.8936 0.0199 0.058 Uiso 1 1 calc R . . H51B H 0.1338 0.8266 -0.0106 0.058 Uiso 1 1 calc R . . C52 C 0.3588(7) 0.8027(5) 0.0519(3) 0.0428(18) Uani 1 1 d . . . C53 C 0.4623(7) 0.8101(5) 0.0829(3) 0.0430(19) Uani 1 1 d . . . H53A H 0.4524 0.8480 0.1117 0.052 Uiso 1 1 calc R . . C54 C 0.5772(8) 0.7618(5) 0.0708(4) 0.049(2) Uani 1 1 d . . . H54A H 0.6441 0.7672 0.0919 0.059 Uiso 1 1 calc R . . C55 C 0.5954(9) 0.7067(6) 0.0292(4) 0.058(2) Uani 1 1 d . . . H55A H 0.6741 0.6742 0.0219 0.070 Uiso 1 1 calc R . . C56 C 0.4969(8) 0.6985(6) -0.0027(5) 0.067(3) Uani 1 1 d . . . H56A H 0.5093 0.6609 -0.0319 0.080 Uiso 1 1 calc R . . C57 C 0.3795(9) 0.7463(6) 0.0088(4) 0.061(3) Uani 1 1 d . . . H57A H 0.3135 0.7403 -0.0127 0.073 Uiso 1 1 calc R . . C58 C 0.2276(8) 0.9610(5) 0.0519(3) 0.0428(18) Uani 1 1 d . . . C59 C 0.1469(8) 1.0245(5) 0.0806(4) 0.049(2) Uani 1 1 d . . . H59A H 0.0861 1.0154 0.1113 0.059 Uiso 1 1 calc R . . C60 C 0.1571(10) 1.1011(5) 0.0634(4) 0.057(2) Uani 1 1 d . . . H60A H 0.1039 1.1427 0.0829 0.068 Uiso 1 1 calc R . . C61 C 0.2456(9) 1.1147(6) 0.0177(4) 0.056(2) Uani 1 1 d . . . H61A H 0.2528 1.1657 0.0064 0.067 Uiso 1 1 calc R . . C62 C 0.3238(9) 1.0534(6) -0.0115(4) 0.061(2) Uani 1 1 d . . . H62A H 0.3829 1.0632 -0.0430 0.073 Uiso 1 1 calc R . . C63 C 0.3151(9) 0.9771(5) 0.0055(4) 0.055(2) Uani 1 1 d . . . H63A H 0.3689 0.9362 -0.0145 0.067 Uiso 1 1 calc R . . C64 C -0.3549(8) 0.6431(5) 0.3142(4) 0.0456(19) Uani 1 1 d . . . H64A H -0.3932 0.6151 0.2872 0.055 Uiso 1 1 calc R . . H64B H -0.4209 0.6676 0.3439 0.055 Uiso 1 1 calc R . . C65 C -0.3297(7) 0.4984(5) 0.3777(3) 0.0408(18) Uani 1 1 d . . . C66 C -0.3662(8) 0.4580(5) 0.3326(4) 0.054(2) Uani 1 1 d . . . H66A H -0.3497 0.4724 0.2918 0.064 Uiso 1 1 calc R . . C67 C -0.4263(8) 0.3968(5) 0.3478(5) 0.058(2) Uani 1 1 d . . . H67A H -0.4494 0.3705 0.3169 0.069 Uiso 1 1 calc R . . C68 C -0.4531(9) 0.3737(6) 0.4074(5) 0.066(3) Uani 1 1 d . . . H68A H -0.4934 0.3321 0.4166 0.079 Uiso 1 1 calc R . . C69 C -0.4200(9) 0.4126(6) 0.4536(5) 0.067(3) Uani 1 1 d . . . H69A H -0.4384 0.3980 0.4942 0.081 Uiso 1 1 calc R . . C70 C -0.3573(8) 0.4751(5) 0.4380(4) 0.053(2) Uani 1 1 d . . . H70A H -0.3340 0.5012 0.4690 0.064 Uiso 1 1 calc R . . C71 C -0.2255(7) 0.6159(5) 0.4254(3) 0.0436(19) Uani 1 1 d . . . C72 C -0.1138(8) 0.5945(5) 0.4519(4) 0.051(2) Uani 1 1 d . . . H72A H -0.0490 0.5578 0.4333 0.061 Uiso 1 1 calc R . . C73 C -0.0951(10) 0.6265(6) 0.5059(4) 0.064(3) Uani 1 1 d . . . H73A H -0.0198 0.6105 0.5238 0.077 Uiso 1 1 calc R . . C74 C -0.1899(10) 0.6820(6) 0.5319(4) 0.058(2) Uani 1 1 d . . . H74A H -0.1782 0.7045 0.5674 0.070 Uiso 1 1 calc R . . C75 C -0.3026(9) 0.7052(6) 0.5063(4) 0.057(2) Uani 1 1 d . . . H75A H -0.3670 0.7422 0.5248 0.068 Uiso 1 1 calc R . . C76 C -0.3188(8) 0.6728(5) 0.4530(4) 0.047(2) Uani 1 1 d . . . H76A H -0.3940 0.6895 0.4352 0.056 Uiso 1 1 calc R . . O9 O -0.1581(10) 0.8266(6) 0.3927(5) 0.117(3) Uani 1 1 d . . . C77 C -0.1191(15) 0.8401(8) 0.4429(6) 0.095(4) Uani 1 1 d . . . C78 C -0.240(2) 0.8915(10) 0.4812(8) 0.208(13) Uani 1 1 d . . . H78A H -0.3128 0.8964 0.4593 0.313 Uiso 1 1 calc R . . H78B H -0.2241 0.9424 0.4867 0.313 Uiso 1 1 calc R . . H78C H -0.2540 0.8660 0.5203 0.313 Uiso 1 1 calc R . . C79 C 0.0101(16) 0.8165(11) 0.4564(8) 0.136(6) Uani 1 1 d . . . H79A H 0.0578 0.7861 0.4240 0.205 Uiso 1 1 calc R . . H79B H 0.0142 0.7857 0.4939 0.205 Uiso 1 1 calc R . . H79C H 0.0443 0.8620 0.4602 0.205 Uiso 1 1 calc R . . O10 O 0.3787(10) 0.2132(7) 0.3539(5) 0.128(4) Uani 1 1 d . . . C80 C 0.4610(13) 0.1585(8) 0.3413(5) 0.085(4) Uani 1 1 d . . . C81 C 0.4576(15) 0.0741(8) 0.3574(6) 0.109(5) Uani 1 1 d . . . H81A H 0.5253 0.0519 0.3817 0.163 Uiso 1 1 calc R . . H81B H 0.4664 0.0460 0.3207 0.163 Uiso 1 1 calc R . . H81C H 0.3788 0.0708 0.3801 0.163 Uiso 1 1 calc R . . C82 C 0.5797(14) 0.1738(9) 0.3094(6) 0.109(5) Uani 1 1 d . . . H82A H 0.5684 0.2278 0.2962 0.164 Uiso 1 1 calc R . . H82B H 0.6029 0.1418 0.2746 0.164 Uiso 1 1 calc R . . H82C H 0.6449 0.1617 0.3366 0.164 Uiso 1 1 calc R . . O11 O 0.1725(8) 0.6319(5) 0.0298(4) 0.103(3) Uani 1 1 d . . . C83 C 0.2296(11) 0.5669(7) 0.0276(5) 0.076(3) Uani 1 1 d . . . C84 C 0.189(2) 0.5090(9) -0.0044(8) 0.170(9) Uani 1 1 d . . . H84A H 0.1133 0.5322 -0.0226 0.255 Uiso 1 1 calc R . . H84B H 0.1735 0.4673 0.0238 0.255 Uiso 1 1 calc R . . H84C H 0.2536 0.4886 -0.0356 0.255 Uiso 1 1 calc R . . C85 C 0.3454(18) 0.5365(13) 0.0588(9) 0.173(9) Uani 1 1 d . . . H85A H 0.3812 0.5794 0.0685 0.260 Uiso 1 1 calc R . . H85B H 0.4052 0.5025 0.0325 0.260 Uiso 1 1 calc R . . H85C H 0.3247 0.5081 0.0957 0.260 Uiso 1 1 calc R . . N7 N 0.8300(13) 0.0926(8) 0.1467(7) 0.125(5) Uani 1 1 d . . . C86 C 0.8402(12) 0.1420(8) 0.1732(7) 0.088(4) Uani 1 1 d . . . C87 C 0.8705(16) 0.1968(9) 0.2131(7) 0.119(5) Uani 1 1 d . . . H87A H 0.8951 0.1700 0.2506 0.178 Uiso 1 1 calc R . . H87B H 0.7981 0.2376 0.2216 0.178 Uiso 1 1 calc R . . H87C H 0.9385 0.2190 0.1936 0.178 Uiso 1 1 calc R . . Cl1 Cl 0.6573(2) 0.13485(14) 0.51344(9) 0.0563(6) Uani 1 1 d . . . O1 O 0.5980(11) 0.1445(6) 0.4596(4) 0.130(4) Uani 1 1 d . . . O2 O 0.5973(9) 0.0891(6) 0.5598(4) 0.108(3) Uani 1 1 d . . . O3 O 0.7798(8) 0.0893(6) 0.5009(4) 0.103(3) Uani 1 1 d . . . O4 O 0.6598(11) 0.2048(5) 0.5386(4) 0.116(3) Uani 1 1 d . . . Cl2 Cl 0.5958(3) 0.3882(3) 0.15477(15) 0.0985(12) Uani 1 1 d . . . O5 O 0.575(4) 0.441(2) 0.1095(15) 0.47(3) Uani 1 1 d . . . O6 O 0.6511(10) 0.3347(14) 0.1176(8) 0.274(13) Uani 1 1 d . . . O7 O 0.6637(10) 0.4136(15) 0.1898(7) 0.329(16) Uani 1 1 d . . . O8 O 0.4762(8) 0.3960(7) 0.1730(6) 0.155(6) Uani 1 1 d . . . O12 O -0.3783(9) 0.8399(6) 0.3539(4) 0.112(3) Uani 1 1 d . . . H12B H -0.3083 0.8367 0.3685 0.135 Uiso 1 1 d R . . H12C H -0.4369 0.8603 0.3800 0.135 Uiso 1 1 d 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 0.0367(6) 0.0352(6) 0.0450(5) -0.0005(4) 0.0018(4) -0.0076(4) Cu2 0.0426(6) 0.0375(6) 0.0396(5) 0.0005(4) 0.0003(4) -0.0092(4) P1 0.0377(11) 0.0308(11) 0.0493(11) -0.0018(9) 0.0019(8) -0.0067(9) P2 0.0480(13) 0.0357(12) 0.0420(11) -0.0025(9) -0.0017(9) -0.0090(10) P3 0.0397(12) 0.0408(12) 0.0392(10) 0.0031(9) -0.0009(8) -0.0090(9) P4 0.0335(11) 0.0397(12) 0.0439(11) 0.0002(9) 0.0002(8) -0.0073(9) N1 0.032(3) 0.051(4) 0.042(3) -0.001(3) -0.006(3) -0.005(3) N2 0.032(3) 0.047(4) 0.036(3) -0.005(3) -0.008(3) -0.006(3) N4 0.055(4) 0.042(4) 0.041(3) 0.002(3) 0.005(3) -0.016(3) N3 0.046(4) 0.042(4) 0.047(4) -0.003(3) 0.002(3) -0.014(3) N5 0.034(4) 0.049(4) 0.046(4) -0.003(3) 0.002(3) -0.012(3) N6 0.040(4) 0.043(4) 0.043(3) -0.002(3) 0.000(3) -0.011(3) C1 0.033(4) 0.041(5) 0.038(4) -0.007(3) 0.000(3) -0.002(3) C2 0.040(4) 0.035(4) 0.039(4) 0.001(3) -0.006(3) -0.014(3) C3 0.028(4) 0.030(4) 0.041(4) -0.002(3) -0.006(3) -0.004(3) C4 0.034(4) 0.043(5) 0.038(4) 0.002(3) 0.004(3) -0.010(4) C5 0.028(4) 0.040(5) 0.046(4) 0.001(3) -0.005(3) -0.005(3) C6 0.041(4) 0.042(5) 0.040(4) 0.008(3) -0.011(3) -0.013(4) C7 0.034(4) 0.051(5) 0.041(4) 0.014(4) -0.005(3) -0.011(4) C8 0.061(5) 0.046(5) 0.037(4) -0.002(4) -0.004(4) -0.016(4) C9 0.054(5) 0.044(5) 0.040(4) -0.001(4) -0.005(4) -0.010(4) C10 0.028(4) 0.042(5) 0.047(4) 0.004(3) -0.003(3) -0.006(3) C11 0.034(4) 0.036(4) 0.044(4) 0.010(3) -0.012(3) -0.003(3) C12 0.032(4) 0.048(5) 0.038(4) 0.004(3) -0.006(3) -0.008(4) C13 0.036(4) 0.050(5) 0.038(4) -0.001(4) 0.002(3) -0.011(4) C14 0.033(4) 0.050(5) 0.041(4) 0.003(4) -0.006(3) -0.008(4) C15 0.048(5) 0.032(4) 0.053(5) -0.002(4) 0.000(4) -0.010(4) C16 0.053(5) 0.025(4) 0.038(4) 0.005(3) 0.002(3) -0.012(4) C17 0.043(5) 0.063(6) 0.046(5) -0.003(4) 0.000(4) -0.003(4) C18 0.072(7) 0.075(7) 0.051(5) 0.000(5) 0.016(5) -0.002(6) C19 0.069(7) 0.062(6) 0.045(5) -0.004(4) -0.003(4) -0.007(5) C20 0.062(6) 0.064(7) 0.058(5) -0.012(5) -0.007(4) -0.014(5) C21 0.036(5) 0.071(7) 0.061(5) -0.004(5) -0.009(4) -0.012(4) C22 0.043(5) 0.023(4) 0.052(4) 0.003(3) -0.002(3) -0.007(3) C23 0.063(6) 0.053(6) 0.055(5) -0.011(4) 0.020(4) -0.011(5) C24 0.099(8) 0.029(5) 0.069(6) -0.006(4) 0.019(6) -0.015(5) C25 0.089(8) 0.042(6) 0.068(6) 0.010(5) 0.008(5) -0.025(5) C26 0.048(5) 0.057(6) 0.066(6) 0.015(5) 0.015(4) -0.013(5) C27 0.041(5) 0.040(5) 0.055(5) -0.003(4) 0.003(4) -0.002(4) C28 0.039(4) 0.043(5) 0.039(4) 0.005(3) -0.006(3) -0.014(4) C29 0.070(6) 0.030(4) 0.051(5) -0.015(4) 0.008(4) -0.011(4) C30 0.075(7) 0.038(5) 0.052(5) -0.002(4) -0.003(4) -0.007(5) C31 0.079(7) 0.055(6) 0.047(5) -0.007(4) 0.009(5) -0.008(5) C32 0.072(7) 0.053(6) 0.058(6) -0.006(5) 0.020(5) -0.014(5) C33 0.054(6) 0.050(6) 0.073(6) -0.004(5) 0.001(5) 0.000(5) C34 0.054(6) 0.061(6) 0.052(5) -0.011(4) -0.005(4) -0.004(5) C35 0.059(5) 0.033(5) 0.043(4) -0.001(3) -0.003(4) -0.003(4) C36 0.062(6) 0.049(6) 0.052(5) -0.003(4) 0.008(4) -0.007(5) C37 0.094(8) 0.037(5) 0.061(5) 0.001(4) 0.020(5) -0.021(5) C38 0.105(9) 0.040(6) 0.059(6) 0.002(4) -0.002(6) -0.028(6) C39 0.068(6) 0.063(7) 0.057(5) 0.003(5) 0.010(4) -0.031(5) C40 0.065(6) 0.046(5) 0.050(5) -0.007(4) 0.003(4) -0.021(5) C41 0.038(4) 0.036(4) 0.037(4) 0.003(3) -0.003(3) -0.009(3) C42 0.032(4) 0.036(4) 0.042(4) 0.002(3) 0.000(3) -0.004(3) C43 0.034(4) 0.036(4) 0.054(5) 0.007(4) -0.005(3) -0.005(3) C44 0.044(5) 0.035(5) 0.049(4) 0.005(4) -0.001(4) 0.001(4) C45 0.046(5) 0.043(5) 0.043(4) -0.005(4) -0.001(3) -0.007(4) C46 0.028(4) 0.034(4) 0.046(4) -0.002(3) -0.003(3) -0.007(3) C47 0.032(4) 0.046(5) 0.041(4) -0.001(3) -0.001(3) -0.011(4) C48 0.036(4) 0.043(5) 0.052(4) 0.000(4) 0.004(3) -0.014(4) C49 0.042(5) 0.048(5) 0.043(4) -0.006(4) -0.003(3) -0.020(4) C50 0.041(4) 0.043(5) 0.041(4) -0.006(3) -0.003(3) -0.011(4) C51 0.051(5) 0.050(5) 0.044(4) -0.002(4) 0.003(4) -0.013(4) C52 0.040(5) 0.041(5) 0.047(4) 0.008(4) 0.002(3) -0.012(4) C53 0.037(5) 0.049(5) 0.042(4) 0.009(4) -0.001(3) -0.011(4) C54 0.045(5) 0.058(6) 0.045(4) 0.002(4) -0.002(4) -0.013(4) C55 0.044(5) 0.060(6) 0.067(6) -0.004(5) -0.003(4) -0.004(4) C56 0.040(5) 0.073(7) 0.082(7) -0.029(6) 0.000(5) 0.005(5) C57 0.047(5) 0.070(7) 0.069(6) -0.025(5) -0.007(4) -0.009(5) C58 0.044(5) 0.047(5) 0.036(4) 0.004(3) 0.001(3) -0.009(4) C59 0.046(5) 0.061(6) 0.039(4) 0.000(4) 0.005(4) -0.011(4) C60 0.077(7) 0.032(5) 0.058(5) 0.002(4) -0.006(5) -0.007(4) C61 0.060(6) 0.056(6) 0.054(5) 0.016(4) -0.005(4) -0.023(5) C62 0.062(6) 0.059(6) 0.059(5) 0.011(5) 0.009(5) -0.022(5) C63 0.063(6) 0.046(5) 0.055(5) 0.004(4) 0.004(4) -0.011(5) C64 0.040(5) 0.046(5) 0.049(4) 0.007(4) 0.008(3) -0.012(4) C65 0.031(4) 0.036(4) 0.051(4) 0.001(3) 0.010(3) -0.006(3) C66 0.050(5) 0.056(6) 0.059(5) -0.010(4) -0.009(4) -0.017(5) C67 0.037(5) 0.040(5) 0.098(7) -0.002(5) -0.016(5) -0.008(4) C68 0.053(6) 0.051(6) 0.095(8) 0.001(5) 0.011(5) -0.026(5) C69 0.065(7) 0.056(6) 0.078(7) 0.002(5) 0.023(5) -0.021(5) C70 0.048(5) 0.047(5) 0.061(5) -0.003(4) 0.002(4) -0.006(4) C71 0.037(4) 0.052(5) 0.042(4) 0.008(4) 0.001(3) -0.016(4) C72 0.043(5) 0.058(6) 0.048(5) -0.001(4) 0.000(4) -0.002(4) C73 0.070(7) 0.070(7) 0.055(5) -0.005(5) -0.015(5) -0.016(6) C74 0.080(7) 0.056(6) 0.045(5) 0.001(4) -0.002(5) -0.034(5) C75 0.065(6) 0.054(6) 0.050(5) -0.010(4) 0.017(4) -0.019(5) C76 0.044(5) 0.039(5) 0.058(5) -0.003(4) 0.001(4) -0.014(4) O9 0.132(8) 0.097(8) 0.116(7) 0.004(6) 0.009(6) -0.021(6) C77 0.136(13) 0.095(10) 0.066(7) -0.004(7) -0.010(8) -0.050(9) C78 0.38(3) 0.086(12) 0.146(14) -0.052(11) 0.160(19) -0.095(17) C79 0.115(13) 0.138(16) 0.162(16) 0.010(12) -0.055(11) -0.023(11) O10 0.106(8) 0.134(9) 0.125(8) -0.044(7) -0.037(6) 0.042(7) C80 0.081(9) 0.094(10) 0.070(7) -0.015(7) -0.016(6) 0.011(8) C81 0.154(14) 0.095(11) 0.092(9) 0.005(8) -0.028(9) -0.050(10) C82 0.116(12) 0.100(11) 0.105(10) -0.012(8) -0.017(9) -0.003(9) O11 0.079(6) 0.060(5) 0.155(8) -0.017(5) 0.047(5) -0.002(4) C83 0.078(8) 0.057(7) 0.082(7) -0.016(6) 0.017(6) 0.001(6) C84 0.34(3) 0.081(11) 0.120(13) 0.016(9) -0.088(16) -0.076(15) C85 0.138(17) 0.19(2) 0.178(19) 0.026(16) -0.052(14) 0.015(15) N7 0.127(11) 0.096(10) 0.154(12) -0.027(9) 0.031(9) -0.041(9) C86 0.079(9) 0.067(8) 0.115(10) 0.019(8) 0.006(7) -0.017(7) C87 0.141(14) 0.100(12) 0.129(12) 0.018(9) -0.039(10) -0.049(10) Cl1 0.0604(14) 0.0630(15) 0.0448(11) -0.0047(10) 0.0015(9) -0.0136(12) O1 0.170(10) 0.146(10) 0.080(6) -0.007(6) -0.071(6) -0.012(8) O2 0.113(7) 0.133(9) 0.084(5) 0.014(5) 0.009(5) -0.049(6) O3 0.079(6) 0.108(7) 0.108(6) -0.008(5) 0.015(5) 0.005(5) O4 0.193(10) 0.079(6) 0.088(6) -0.038(5) -0.015(6) -0.042(6) Cl2 0.0615(18) 0.143(3) 0.0789(19) -0.040(2) -0.0026(14) 0.0158(19) O5 0.55(6) 0.45(5) 0.30(3) 0.20(3) 0.05(4) 0.04(4) O6 0.068(7) 0.49(3) 0.274(17) -0.32(2) 0.005(8) -0.008(11) O7 0.067(7) 0.72(4) 0.239(15) -0.36(2) 0.020(8) -0.100(13) O8 0.062(6) 0.175(11) 0.238(13) -0.127(10) 0.062(7) -0.049(6) O12 0.125(8) 0.108(8) 0.091(6) -0.014(5) 0.008(5) 0.002(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.015(7) . ? Cu1 P1 2.257(2) . ? Cu1 P4 2.263(2) . ? Cu2 N2 1.997(7) . ? Cu2 P3 2.237(2) . ? Cu2 P2 2.254(2) . ? P1 C22 1.796(8) . ? P1 C16 1.825(7) . ? P1 C15 1.827(8) . ? P2 C29 1.803(8) . ? P2 C35 1.807(9) . ? P2 C28 1.831(8) . ? P3 C58 1.799(8) . ? P3 C52 1.809(8) . ? P3 C51 1.867(8) . ? P4 C65 1.800(8) . ? P4 C71 1.812(8) . ? P4 C64 1.847(9) . ? N1 C3 1.351(9) . ? N1 C1 1.368(10) . ? N2 C2 1.354(9) . ? N2 C4 1.362(10) . ? N4 C11 1.386(10) . ? N4 C28 1.423(10) . ? N4 H3B 0.8600 . ? N3 C6 1.375(10) . ? N3 C15 1.451(10) . ? N3 H4B 0.8600 . ? N5 C42 1.389(9) . ? N5 C51 1.435(10) . ? N5 H5A 0.8600 . ? N6 C47 1.387(9) . ? N6 C64 1.415(10) . ? N6 H6A 0.8600 . ? C1 C2 1.347(10) . ? C1 H1A 0.9300 . ? C2 H2A 0.9300 . ? C3 C4 1.348(10) . ? C3 H3A 0.9300 . ? C4 H4A 0.9300 . ? C5 C14 1.424(10) . ? C5 C6 1.429(11) . ? C5 C10 1.444(10) . ? C6 C7 1.390(10) . ? C7 C8 1.408(11) . ? C7 H7A 0.9300 . ? C8 C9 1.348(11) . ? C8 H8A 0.9300 . ? C9 C10 1.410(10) . ? C9 H9A 0.9300 . ? C10 C11 1.426(11) . ? C11 C12 1.393(10) . ? C12 C13 1.397(11) . ? C12 H12A 0.9300 . ? C13 C14 1.367(11) . ? C13 H13A 0.9300 . ? C14 H14A 0.9300 . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 C21 1.367(11) . ? C16 C17 1.393(11) . ? C17 C18 1.400(12) . ? C17 H17A 0.9300 . ? C18 C19 1.383(14) . ? C18 H18A 0.9300 . ? C19 C20 1.368(13) . ? C19 H19A 0.9300 . ? C20 C21 1.371(12) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C27 1.365(11) . ? C22 C23 1.422(12) . ? C23 C24 1.386(12) . ? C23 H23A 0.9300 . ? C24 C25 1.399(13) . ? C24 H24A 0.9300 . ? C25 C26 1.367(13) . ? C25 H25A 0.9300 . ? C26 C27 1.381(12) . ? C26 H26A 0.9300 . ? C27 H27A 0.9300 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C34 1.393(12) . ? C29 C30 1.410(11) . ? C30 C31 1.414(13) . ? C30 H30A 0.9300 . ? C31 C32 1.359(14) . ? C31 H31A 0.9300 . ? C32 C33 1.363(13) . ? C32 H32A 0.9300 . ? C33 C34 1.374(12) . ? C33 H33A 0.9300 . ? C34 H34A 0.9300 . ? C35 C36 1.388(12) . ? C35 C40 1.402(12) . ? C36 C37 1.378(12) . ? C36 H36A 0.9300 . ? C37 C38 1.368(14) . ? C37 H37A 0.9300 . ? C38 C39 1.372(14) . ? C38 H38A 0.9300 . ? C39 C40 1.387(12) . ? C39 H39A 0.9300 . ? C40 H40A 0.9300 . ? C41 C50 1.418(10) . ? C41 C46 1.422(10) . ? C41 C42 1.441(10) . ? C42 C43 1.391(11) . ? C43 C44 1.400(11) . ? C43 H43A 0.9300 . ? C44 C45 1.361(11) . ? C44 H44A 0.9300 . ? C45 C46 1.430(11) . ? C45 H45A 0.9300 . ? C46 C47 1.428(11) . ? C47 C48 1.383(11) . ? C48 C49 1.403(11) . ? C48 H48A 0.9300 . ? C49 C50 1.355(11) . ? C49 H49A 0.9300 . ? C50 H50A 0.9300 . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C57 1.383(11) . ? C52 C53 1.412(11) . ? C53 C54 1.369(12) . ? C53 H53A 0.9300 . ? C54 C55 1.346(12) . ? C54 H54A 0.9300 . ? C55 C56 1.380(12) . ? C55 H55A 0.9300 . ? C56 C57 1.386(12) . ? C56 H56A 0.9300 . ? C57 H57A 0.9300 . ? C58 C63 1.384(11) . ? C58 C59 1.406(12) . ? C59 C60 1.396(12) . ? C59 H59A 0.9300 . ? C60 C61 1.367(12) . ? C60 H60A 0.9300 . ? C61 C62 1.375(13) . ? C61 H61A 0.9300 . ? C62 C63 1.387(13) . ? C62 H62A 0.9300 . ? C63 H63A 0.9300 . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 C70 1.390(11) . ? C65 C66 1.393(11) . ? C66 C67 1.377(12) . ? C66 H66A 0.9300 . ? C67 C68 1.372(14) . ? C67 H67A 0.9300 . ? C68 C69 1.377(14) . ? C68 H68A 0.9300 . ? C69 C70 1.416(13) . ? C69 H69A 0.9300 . ? C70 H70A 0.9300 . ? C71 C72 1.378(11) . ? C71 C76 1.389(11) . ? C72 C73 1.401(12) . ? C72 H72A 0.9300 . ? C73 C74 1.369(14) . ? C73 H73A 0.9300 . ? C74 C75 1.380(13) . ? C74 H74A 0.9300 . ? C75 C76 1.380(11) . ? C75 H75A 0.9300 . ? C76 H76A 0.9300 . ? O9 C77 1.279(14) . ? C77 C79 1.44(2) . ? C77 C78 1.62(2) . ? C78 H78A 0.9600 . ? C78 H78B 0.9600 . ? C78 H78C 0.9600 . ? C79 H79A 0.9600 . ? C79 H79B 0.9600 . ? C79 H79C 0.9600 . ? O10 C80 1.194(14) . ? C80 C82 1.476(18) . ? C80 C81 1.507(18) . ? C81 H81A 0.9600 . ? C81 H81B 0.9600 . ? C81 H81C 0.9600 . ? C82 H82A 0.9600 . ? C82 H82B 0.9600 . ? C82 H82C 0.9600 . ? O11 C83 1.182(13) . ? C83 C84 1.437(17) . ? C83 C85 1.49(2) . ? C84 H84A 0.9600 . ? C84 H84B 0.9600 . ? C84 H84C 0.9600 . ? C85 H85A 0.9600 . ? C85 H85B 0.9600 . ? C85 H85C 0.9600 . ? N7 C86 1.105(16) . ? C86 C87 1.452(19) . ? C87 H87A 0.9600 . ? C87 H87B 0.9600 . ? C87 H87C 0.9600 . ? Cl1 O4 1.385(7) . ? Cl1 O1 1.395(8) . ? Cl1 O3 1.418(8) . ? Cl1 O2 1.448(9) . ? Cl2 O7 1.282(9) . ? Cl2 O6 1.294(11) . ? Cl2 O8 1.307(8) . ? Cl2 O5 1.32(3) . ? O12 H12B 0.8500 . ? O12 H12C 0.8500 . ? 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 N1 Cu1 P1 116.68(19) . . ? N1 Cu1 P4 111.05(19) . . ? P1 Cu1 P4 132.26(9) . . ? N2 Cu2 P3 120.69(17) . . ? N2 Cu2 P2 115.78(17) . . ? P3 Cu2 P2 123.50(9) . . ? C22 P1 C16 101.6(3) . . ? C22 P1 C15 103.2(4) . . ? C16 P1 C15 104.5(4) . . ? C22 P1 Cu1 116.0(3) . . ? C16 P1 Cu1 112.7(3) . . ? C15 P1 Cu1 117.0(3) . . ? C29 P2 C35 106.7(4) . . ? C29 P2 C28 105.1(4) . . ? C35 P2 C28 101.5(4) . . ? C29 P2 Cu2 106.9(3) . . ? C35 P2 Cu2 120.0(3) . . ? C28 P2 Cu2 115.5(3) . . ? C58 P3 C52 104.1(4) . . ? C58 P3 C51 102.9(4) . . ? C52 P3 C51 107.1(4) . . ? C58 P3 Cu2 114.1(2) . . ? C52 P3 Cu2 105.5(3) . . ? C51 P3 Cu2 121.8(3) . . ? C65 P4 C71 104.3(4) . . ? C65 P4 C64 100.1(4) . . ? C71 P4 C64 105.9(4) . . ? C65 P4 Cu1 117.8(3) . . ? C71 P4 Cu1 110.9(3) . . ? C64 P4 Cu1 116.3(3) . . ? C3 N1 C1 113.7(7) . . ? C3 N1 Cu1 122.3(5) . . ? C1 N1 Cu1 123.9(5) . . ? C2 N2 C4 114.2(6) . . ? C2 N2 Cu2 125.5(5) . . ? C4 N2 Cu2 120.1(5) . . ? C11 N4 C28 123.0(6) . . ? C11 N4 H3B 118.5 . . ? C28 N4 H3B 118.5 . . ? C6 N3 C15 122.0(6) . . ? C6 N3 H4B 119.0 . . ? C15 N3 H4B 119.0 . . ? C42 N5 C51 121.8(7) . . ? C42 N5 H5A 119.1 . . ? C51 N5 H5A 119.1 . . ? C47 N6 C64 123.4(7) . . ? C47 N6 H6A 118.3 . . ? C64 N6 H6A 118.3 . . ? C2 C1 N1 122.2(7) . . ? C2 C1 H1A 118.9 . . ? N1 C1 H1A 118.9 . . ? C1 C2 N2 123.8(7) . . ? C1 C2 H2A 118.1 . . ? N2 C2 H2A 118.1 . . ? C4 C3 N1 124.4(7) . . ? C4 C3 H3A 117.8 . . ? N1 C3 H3A 117.8 . . ? C3 C4 N2 121.8(7) . . ? C3 C4 H4A 119.1 . . ? N2 C4 H4A 119.1 . . ? C14 C5 C6 122.5(7) . . ? C14 C5 C10 119.0(7) . . ? C6 C5 C10 118.5(7) . . ? N3 C6 C7 122.6(7) . . ? N3 C6 C5 117.6(7) . . ? C7 C6 C5 119.8(7) . . ? C6 C7 C8 120.3(7) . . ? C6 C7 H7A 119.8 . . ? C8 C7 H7A 119.8 . . ? C9 C8 C7 121.2(7) . . ? C9 C8 H8A 119.4 . . ? C7 C8 H8A 119.4 . . ? C8 C9 C10 121.2(8) . . ? C8 C9 H9A 119.4 . . ? C10 C9 H9A 119.4 . . ? C9 C10 C11 122.8(7) . . ? C9 C10 C5 119.0(7) . . ? C11 C10 C5 118.2(7) . . ? N4 C11 C12 120.7(7) . . ? N4 C11 C10 118.6(7) . . ? C12 C11 C10 120.7(7) . . ? C11 C12 C13 119.9(8) . . ? C11 C12 H12A 120.1 . . ? C13 C12 H12A 120.1 . . ? C14 C13 C12 121.7(7) . . ? C14 C13 H13A 119.2 . . ? C12 C13 H13A 119.2 . . ? C13 C14 C5 120.4(7) . . ? C13 C14 H14A 119.8 . . ? C5 C14 H14A 119.8 . . ? N3 C15 P1 112.9(6) . . ? N3 C15 H15A 109.0 . . ? P1 C15 H15A 109.0 . . ? N3 C15 H15B 109.0 . . ? P1 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C21 C16 C17 118.0(7) . . ? C21 C16 P1 118.5(6) . . ? C17 C16 P1 123.4(6) . . ? C16 C17 C18 120.2(8) . . ? C16 C17 H17A 119.9 . . ? C18 C17 H17A 119.9 . . ? C19 C18 C17 119.9(9) . . ? C19 C18 H18A 120.0 . . ? C17 C18 H18A 120.0 . . ? C20 C19 C18 119.3(8) . . ? C20 C19 H19A 120.4 . . ? C18 C19 H19A 120.4 . . ? C19 C20 C21 120.4(9) . . ? C19 C20 H20A 119.8 . . ? C21 C20 H20A 119.8 . . ? C16 C21 C20 122.1(8) . . ? C16 C21 H21A 118.9 . . ? C20 C21 H21A 118.9 . . ? C27 C22 C23 116.4(7) . . ? C27 C22 P1 122.8(6) . . ? C23 C22 P1 120.5(6) . . ? C24 C23 C22 121.5(8) . . ? C24 C23 H23A 119.3 . . ? C22 C23 H23A 119.3 . . ? C23 C24 C25 118.8(9) . . ? C23 C24 H24A 120.6 . . ? C25 C24 H24A 120.6 . . ? C26 C25 C24 120.4(8) . . ? C26 C25 H25A 119.8 . . ? C24 C25 H25A 119.8 . . ? C25 C26 C27 119.4(8) . . ? C25 C26 H26A 120.3 . . ? C27 C26 H26A 120.3 . . ? C22 C27 C26 123.3(8) . . ? C22 C27 H27A 118.4 . . ? C26 C27 H27A 118.4 . . ? N4 C28 P2 113.4(5) . . ? N4 C28 H28A 108.9 . . ? P2 C28 H28A 108.9 . . ? N4 C28 H28B 108.9 . . ? P2 C28 H28B 108.9 . . ? H28A C28 H28B 107.7 . . ? C34 C29 C30 118.1(8) . . ? C34 C29 P2 118.3(6) . . ? C30 C29 P2 123.7(8) . . ? C29 C30 C31 118.6(9) . . ? C29 C30 H30A 120.7 . . ? C31 C30 H30A 120.7 . . ? C32 C31 C30 120.7(9) . . ? C32 C31 H31A 119.7 . . ? C30 C31 H31A 119.7 . . ? C31 C32 C33 121.2(9) . . ? C31 C32 H32A 119.4 . . ? C33 C32 H32A 119.4 . . ? C32 C33 C34 119.4(10) . . ? C32 C33 H33A 120.3 . . ? C34 C33 H33A 120.3 . . ? C33 C34 C29 122.1(8) . . ? C33 C34 H34A 119.0 . . ? C29 C34 H34A 119.0 . . ? C36 C35 C40 116.4(8) . . ? C36 C35 P2 122.8(7) . . ? C40 C35 P2 120.8(6) . . ? C37 C36 C35 122.1(9) . . ? C37 C36 H36A 118.9 . . ? C35 C36 H36A 118.9 . . ? C38 C37 C36 119.8(9) . . ? C38 C37 H37A 120.1 . . ? C36 C37 H37A 120.1 . . ? C37 C38 C39 120.8(9) . . ? C37 C38 H38A 119.6 . . ? C39 C38 H38A 119.6 . . ? C38 C39 C40 119.0(9) . . ? C38 C39 H39A 120.5 . . ? C40 C39 H39A 120.5 . . ? C39 C40 C35 122.0(9) . . ? C39 C40 H40A 119.0 . . ? C35 C40 H40A 119.0 . . ? C50 C41 C46 119.0(7) . . ? C50 C41 C42 122.2(7) . . ? C46 C41 C42 118.8(7) . . ? N5 C42 C43 121.3(7) . . ? N5 C42 C41 118.8(7) . . ? C43 C42 C41 119.8(7) . . ? C42 C43 C44 119.5(7) . . ? C42 C43 H43A 120.3 . . ? C44 C43 H43A 120.3 . . ? C45 C44 C43 122.3(8) . . ? C45 C44 H44A 118.8 . . ? C43 C44 H44A 118.8 . . ? C44 C45 C46 120.0(7) . . ? C44 C45 H45A 120.0 . . ? C46 C45 H45A 120.0 . . ? C41 C46 C47 119.2(7) . . ? C41 C46 C45 118.8(7) . . ? C47 C46 C45 121.9(7) . . ? C48 C47 N6 120.9(7) . . ? C48 C47 C46 119.6(7) . . ? N6 C47 C46 119.5(7) . . ? C47 C48 C49 119.6(7) . . ? C47 C48 H48A 120.2 . . ? C49 C48 H48A 120.2 . . ? C50 C49 C48 122.2(7) . . ? C50 C49 H49A 118.9 . . ? C48 C49 H49A 118.9 . . ? C49 C50 C41 119.9(7) . . ? C49 C50 H50A 120.0 . . ? C41 C50 H50A 120.0 . . ? N5 C51 P3 114.6(6) . . ? N5 C51 H51A 108.6 . . ? P3 C51 H51A 108.6 . . ? N5 C51 H51B 108.6 . . ? P3 C51 H51B 108.6 . . ? H51A C51 H51B 107.6 . . ? C57 C52 C53 117.3(8) . . ? C57 C52 P3 126.9(6) . . ? C53 C52 P3 115.7(6) . . ? C54 C53 C52 120.4(8) . . ? C54 C53 H53A 119.8 . . ? C52 C53 H53A 119.8 . . ? C55 C54 C53 121.6(8) . . ? C55 C54 H54A 119.2 . . ? C53 C54 H54A 119.2 . . ? C54 C55 C56 119.7(9) . . ? C54 C55 H55A 120.2 . . ? C56 C55 H55A 120.2 . . ? C55 C56 C57 119.9(9) . . ? C55 C56 H56A 120.0 . . ? C57 C56 H56A 120.0 . . ? C52 C57 C56 121.1(8) . . ? C52 C57 H57A 119.4 . . ? C56 C57 H57A 119.4 . . ? C63 C58 C59 117.8(8) . . ? C63 C58 P3 124.0(7) . . ? C59 C58 P3 118.2(6) . . ? C60 C59 C58 120.8(8) . . ? C60 C59 H59A 119.6 . . ? C58 C59 H59A 119.6 . . ? C61 C60 C59 119.7(9) . . ? C61 C60 H60A 120.1 . . ? C59 C60 H60A 120.1 . . ? C60 C61 C62 120.3(9) . . ? C60 C61 H61A 119.8 . . ? C62 C61 H61A 119.8 . . ? C61 C62 C63 120.4(8) . . ? C61 C62 H62A 119.8 . . ? C63 C62 H62A 119.8 . . ? C58 C63 C62 120.9(9) . . ? C58 C63 H63A 119.5 . . ? C62 C63 H63A 119.5 . . ? N6 C64 P4 115.1(5) . . ? N6 C64 H64A 108.5 . . ? P4 C64 H64A 108.5 . . ? N6 C64 H64B 108.5 . . ? P4 C64 H64B 108.5 . . ? H64A C64 H64B 107.5 . . ? C70 C65 C66 117.5(8) . . ? C70 C65 P4 123.8(6) . . ? C66 C65 P4 118.5(6) . . ? C67 C66 C65 120.6(9) . . ? C67 C66 H66A 119.7 . . ? C65 C66 H66A 119.7 . . ? C68 C67 C66 121.7(9) . . ? C68 C67 H67A 119.1 . . ? C66 C67 H67A 119.1 . . ? C67 C68 C69 119.6(9) . . ? C67 C68 H68A 120.2 . . ? C69 C68 H68A 120.2 . . ? C68 C69 C70 118.8(9) . . ? C68 C69 H69A 120.6 . . ? C70 C69 H69A 120.6 . . ? C65 C70 C69 121.7(8) . . ? C65 C70 H70A 119.1 . . ? C69 C70 H70A 119.1 . . ? C72 C71 C76 117.6(7) . . ? C72 C71 P4 118.2(6) . . ? C76 C71 P4 124.1(6) . . ? C71 C72 C73 121.9(8) . . ? C71 C72 H72A 119.1 . . ? C73 C72 H72A 119.1 . . ? C74 C73 C72 118.5(9) . . ? C74 C73 H73A 120.7 . . ? C72 C73 H73A 120.7 . . ? C73 C74 C75 121.1(8) . . ? C73 C74 H74A 119.5 . . ? C75 C74 H74A 119.5 . . ? C76 C75 C74 119.3(9) . . ? C76 C75 H75A 120.3 . . ? C74 C75 H75A 120.3 . . ? C75 C76 C71 121.5(8) . . ? C75 C76 H76A 119.2 . . ? C71 C76 H76A 119.2 . . ? O9 C77 C79 123.4(14) . . ? O9 C77 C78 105.8(15) . . ? C79 C77 C78 130.7(15) . . ? C77 C78 H78A 109.5 . . ? C77 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C77 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C77 C79 H79A 109.5 . . ? C77 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? C77 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? O10 C80 C82 118.0(15) . . ? O10 C80 C81 125.9(15) . . ? C82 C80 C81 116.0(12) . . ? C80 C81 H81A 109.5 . . ? C80 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C80 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C80 C82 H82A 109.5 . . ? C80 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C80 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? O11 C83 C84 122.0(14) . . ? O11 C83 C85 124.0(14) . . ? C84 C83 C85 114.0(15) . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C83 C85 H85A 109.5 . . ? C83 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C83 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? N7 C86 C87 169.8(17) . . ? C86 C87 H87A 109.5 . . ? C86 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C86 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? O4 Cl1 O1 113.1(7) . . ? O4 Cl1 O3 111.9(6) . . ? O1 Cl1 O3 107.8(6) . . ? O4 Cl1 O2 107.2(6) . . ? O1 Cl1 O2 112.1(6) . . ? O3 Cl1 O2 104.3(6) . . ? O7 Cl2 O6 117.8(8) . . ? O7 Cl2 O8 116.7(7) . . ? O6 Cl2 O8 120.9(8) . . ? O7 Cl2 O5 106(2) . . ? O6 Cl2 O5 91.9(19) . . ? O8 Cl2 O5 93.5(19) . . ? H12B O12 H12C 108.5 . . ? _diffrn_measured_fraction_theta_max 0.979 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.979 _refine_diff_density_max 1.058 _refine_diff_density_min -1.388 _refine_diff_density_rms 0.156