Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Raphael G. Raptis' _publ_contact_author_address ; Department of Chemistry University of Puerto Rico San Juan Puerto Rico PR 00931-3346 PUERTO RICO ; _publ_contact_author_email RAPHAEL@ADAM.UPRR.PR _publ_section_title ; Trigonal prismatic CuII6-pyrazolato cages: Structural and electrochemical study, evidence of charge-delocalisation ; loop_ _publ_author_name 'Raphael G. Raptis' 'Gellert Mezei' 'Marlyn Rivera-Carrillo' data_PPN[3] _database_code_depnum_ccdc_archive 'CCDC 617268' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C99 H81 Cu6 N19 O2 P2' _chemical_formula_weight 2012.01 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/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 17.977(19) _cell_length_b 25.31(3) _cell_length_c 22.76(2) _cell_angle_alpha 90.00 _cell_angle_beta 109.884(18) _cell_angle_gamma 90.00 _cell_volume 9741(18) _cell_formula_units_Z 4 _cell_measurement_temperature 303(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour brown _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4112 _exptl_absorpt_coefficient_mu 1.377 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 303(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 41689 _diffrn_reflns_av_R_equivalents 0.0819 _diffrn_reflns_av_sigmaI/netI 0.0643 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 23.34 _reflns_number_total 14043 _reflns_number_gt 8551 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0844P)^2^+23.4136P] 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 14043 _refine_ls_number_parameters 1153 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1191 _refine_ls_R_factor_gt 0.0604 _refine_ls_wR_factor_ref 0.2014 _refine_ls_wR_factor_gt 0.1518 _refine_ls_goodness_of_fit_ref 1.113 _refine_ls_restrained_S_all 1.113 _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 0.24346(5) 0.34071(3) 0.23301(4) 0.0371(2) Uani 1 1 d . . . Cu2 Cu 0.25849(5) 0.23133(3) 0.30782(4) 0.0401(2) Uani 1 1 d . . . Cu3 Cu 0.27888(5) 0.34422(3) 0.38233(4) 0.0371(2) Uani 1 1 d . . . Cu4 Cu 0.07491(5) 0.34528(3) 0.22848(4) 0.0360(2) Uani 1 1 d . . . Cu5 Cu 0.09267(5) 0.23527(3) 0.30684(4) 0.0374(2) Uani 1 1 d . . . Cu6 Cu 0.10877(5) 0.34613(3) 0.37828(4) 0.0340(2) Uani 1 1 d . . . P1 P 0.69695(15) 0.27642(10) 0.50175(12) 0.0667(7) Uani 1 1 d . . . P2 P 0.65944(16) 0.21699(12) 0.60633(13) 0.0747(8) Uani 1 1 d . . . O1 O 0.2741(3) 0.30540(18) 0.31039(19) 0.0384(11) Uani 1 1 d . . . O2 O 0.0783(3) 0.30916(17) 0.30199(19) 0.0355(11) Uani 1 1 d . . . N1 N 0.2542(3) 0.2746(2) 0.1914(3) 0.0423(15) Uani 1 1 d . . . N2 N 0.2580(3) 0.2289(3) 0.2228(3) 0.0465(16) Uani 1 1 d . . . N3 N 0.2880(4) 0.2323(2) 0.3982(3) 0.0454(15) Uani 1 1 d . . . N4 N 0.2996(3) 0.2783(2) 0.4294(3) 0.0440(15) Uani 1 1 d . . . N5 N 0.2817(4) 0.4099(2) 0.3388(3) 0.0469(16) Uani 1 1 d . . . N6 N 0.2641(4) 0.4088(2) 0.2763(3) 0.0501(16) Uani 1 1 d . . . N7 N 0.0520(3) 0.2786(2) 0.1835(3) 0.0428(15) Uani 1 1 d . . . N8 N 0.0640(4) 0.2331(2) 0.2160(3) 0.0458(15) Uani 1 1 d . . . N9 N 0.0950(4) 0.2355(2) 0.3928(3) 0.0426(15) Uani 1 1 d . . . N10 N 0.0995(3) 0.2819(2) 0.4223(3) 0.0409(14) Uani 1 1 d . . . N11 N 0.0835(3) 0.4122(2) 0.3316(3) 0.0436(15) Uani 1 1 d . . . N12 N 0.0733(4) 0.4117(2) 0.2705(3) 0.0461(15) Uani 1 1 d . . . N13 N 0.0951(3) 0.3801(2) 0.1539(3) 0.0390(14) Uani 1 1 d . . . N14 N 0.1718(3) 0.3764(2) 0.1549(3) 0.0392(14) Uani 1 1 d . . . N15 N 0.2090(4) 0.1584(2) 0.3055(3) 0.0491(16) Uani 1 1 d . . . N16 N 0.1359(4) 0.1617(2) 0.3117(3) 0.0460(15) Uani 1 1 d . . . N17 N 0.1842(3) 0.3820(2) 0.4550(3) 0.0383(14) Uani 1 1 d . . . N18 N 0.2606(3) 0.3832(2) 0.4552(3) 0.0408(14) Uani 1 1 d . . . N19 N 0.6835(7) 0.2478(4) 0.5577(4) 0.126(4) Uani 1 1 d . . . C1 C 0.2572(5) 0.1898(3) 0.1830(4) 0.053(2) Uani 1 1 d . . . H1 H 0.2590 0.1540 0.1928 0.064 Uiso 1 1 calc R . . C2 C 0.2534(4) 0.2094(3) 0.1262(4) 0.053(2) Uani 1 1 d . . . H2 H 0.2525 0.1908 0.0907 0.064 Uiso 1 1 calc R . . C3 C 0.2514(4) 0.2629(3) 0.1340(4) 0.0484(19) Uani 1 1 d . . . H3 H 0.2485 0.2876 0.1031 0.058 Uiso 1 1 calc R . . C4 C 0.3242(5) 0.2674(3) 0.4906(3) 0.053(2) Uani 1 1 d . . . H4 H 0.3366 0.2925 0.5223 0.064 Uiso 1 1 calc R . . C5 C 0.3287(5) 0.2129(4) 0.4997(4) 0.065(2) Uani 1 1 d . . . H5 H 0.3443 0.1944 0.5372 0.078 Uiso 1 1 calc R . . C6 C 0.3046(5) 0.1931(3) 0.4400(3) 0.058(2) Uani 1 1 d . . . H6 H 0.3004 0.1573 0.4300 0.069 Uiso 1 1 calc R . . C7 C 0.2644(6) 0.4586(4) 0.2561(4) 0.069(3) Uani 1 1 d . . . H7 H 0.2537 0.4686 0.2147 0.083 Uiso 1 1 calc R . . C8 C 0.2833(6) 0.4928(4) 0.3065(4) 0.072(3) Uani 1 1 d . . . H8 H 0.2876 0.5294 0.3062 0.086 Uiso 1 1 calc R . . C9 C 0.2942(5) 0.4603(4) 0.3575(4) 0.065(2) Uani 1 1 d . . . H9 H 0.3082 0.4717 0.3987 0.078 Uiso 1 1 calc R . . C10 C 0.0487(5) 0.1933(3) 0.1751(4) 0.058(2) Uani 1 1 d . . . H10 H 0.0541 0.1577 0.1858 0.070 Uiso 1 1 calc R . . C11 C 0.0238(5) 0.2123(4) 0.1153(3) 0.065(2) Uani 1 1 d . . . H11 H 0.0081 0.1932 0.0782 0.078 Uiso 1 1 calc R . . C12 C 0.0275(5) 0.2667(3) 0.1226(4) 0.055(2) Uani 1 1 d . . . H12 H 0.0148 0.2912 0.0902 0.066 Uiso 1 1 calc R . . C13 C 0.1054(4) 0.2719(3) 0.4813(3) 0.0458(19) Uani 1 1 d . . . H13 H 0.1097 0.2975 0.5115 0.055 Uiso 1 1 calc R . . C14 C 0.1042(5) 0.2182(3) 0.4910(3) 0.052(2) Uani 1 1 d . . . H14 H 0.1072 0.2006 0.5276 0.063 Uiso 1 1 calc R . . C15 C 0.0977(5) 0.1969(3) 0.4345(3) 0.049(2) Uani 1 1 d . . . H15 H 0.0954 0.1610 0.4258 0.059 Uiso 1 1 calc R . . C16 C 0.0593(6) 0.4617(3) 0.2498(4) 0.067(3) Uani 1 1 d . . . H16 H 0.0513 0.4724 0.2090 0.080 Uiso 1 1 calc R . . C17 C 0.0584(6) 0.4950(3) 0.2977(4) 0.070(3) Uani 1 1 d . . . H17 H 0.0489 0.5312 0.2958 0.084 Uiso 1 1 calc R . . C18 C 0.0746(5) 0.4628(3) 0.3479(4) 0.057(2) Uani 1 1 d . . . H18 H 0.0791 0.4738 0.3879 0.068 Uiso 1 1 calc R . . C19 C 0.1765(4) 0.3983(3) 0.1028(3) 0.0414(18) Uani 1 1 d . . . C20 C 0.1028(4) 0.4159(3) 0.0664(3) 0.0434(18) Uani 1 1 d . . . H20 H 0.0891 0.4323 0.0276 0.052 Uiso 1 1 calc R . . C21 C 0.0529(4) 0.4039(3) 0.1003(3) 0.0427(18) Uani 1 1 d . . . C22 C -0.0327(4) 0.4165(3) 0.0826(4) 0.0469(19) Uani 1 1 d . . . C23 C -0.0774(5) 0.4018(4) 0.1183(4) 0.072(3) Uani 1 1 d . . . H23 H -0.0544 0.3818 0.1542 0.086 Uiso 1 1 calc R . . C24 C -0.1549(6) 0.4162(5) 0.1019(6) 0.097(4) Uani 1 1 d . . . H24 H -0.1840 0.4064 0.1269 0.116 Uiso 1 1 calc R . . C25 C -0.1901(5) 0.4452(4) 0.0486(5) 0.084(3) Uani 1 1 d . . . H25 H -0.2430 0.4550 0.0376 0.101 Uiso 1 1 calc R . . C26 C -0.1476(5) 0.4596(4) 0.0123(5) 0.077(3) Uani 1 1 d . . . H26 H -0.1715 0.4788 -0.0240 0.092 Uiso 1 1 calc R . . C27 C -0.0690(5) 0.4457(3) 0.0292(4) 0.061(2) Uani 1 1 d . . . H27 H -0.0400 0.4562 0.0043 0.073 Uiso 1 1 calc R . . C28 C 0.2523(4) 0.4045(3) 0.0902(4) 0.0472(19) Uani 1 1 d . . . C29 C 0.3247(5) 0.4009(4) 0.1383(4) 0.063(2) Uani 1 1 d . . . H29 H 0.3270 0.3921 0.1785 0.075 Uiso 1 1 calc R . . C30 C 0.3947(6) 0.4106(4) 0.1252(6) 0.092(3) Uani 1 1 d . . . H30 H 0.4433 0.4083 0.1573 0.110 Uiso 1 1 calc R . . C31 C 0.3927(7) 0.4234(4) 0.0665(7) 0.090(4) Uani 1 1 d . . . H31 H 0.4392 0.4302 0.0585 0.108 Uiso 1 1 calc R . . C32 C 0.3221(7) 0.4259(4) 0.0202(5) 0.079(3) Uani 1 1 d . . . H32 H 0.3205 0.4343 -0.0200 0.094 Uiso 1 1 calc R . . C33 C 0.2505(5) 0.4163(3) 0.0310(4) 0.060(2) Uani 1 1 d . . . H33 H 0.2025 0.4179 -0.0018 0.072 Uiso 1 1 calc R . . C34 C 0.1079(5) 0.1127(3) 0.3136(4) 0.058(2) Uani 1 1 d . . . C35 C 0.1647(6) 0.0767(4) 0.3101(4) 0.075(3) Uani 1 1 d . . . H35 H 0.1617 0.0400 0.3111 0.090 Uiso 1 1 calc R . . C36 C 0.2267(6) 0.1068(4) 0.3048(4) 0.064(2) Uani 1 1 d . . . C37 C 0.0292(6) 0.1039(3) 0.3193(4) 0.062(2) Uani 1 1 d . . . C38 C 0.0185(7) 0.0626(3) 0.3567(4) 0.072(3) Uani 1 1 d . . . H38 H 0.0610 0.0409 0.3777 0.086 Uiso 1 1 calc R . . C39 C -0.0539(8) 0.0540(5) 0.3625(5) 0.088(3) Uani 1 1 d . . . H39 H -0.0606 0.0262 0.3869 0.105 Uiso 1 1 calc R . . C40 C -0.1157(8) 0.0858(5) 0.3327(6) 0.101(4) Uani 1 1 d . . . H40 H -0.1647 0.0792 0.3365 0.121 Uiso 1 1 calc R . . C41 C -0.1074(7) 0.1282(5) 0.2964(6) 0.093(3) Uani 1 1 d . . . H41 H -0.1497 0.1507 0.2772 0.112 Uiso 1 1 calc R . . C42 C -0.0345(6) 0.1359(4) 0.2897(4) 0.071(3) Uani 1 1 d . . . H42 H -0.0284 0.1634 0.2647 0.085 Uiso 1 1 calc R . . C43 C 0.3006(7) 0.0884(4) 0.2969(5) 0.082(3) Uani 1 1 d . . . C44 C 0.3690(7) 0.1176(5) 0.3193(6) 0.098(4) Uani 1 1 d . . . H44 H 0.3693 0.1484 0.3415 0.118 Uiso 1 1 calc R . . C45 C 0.4383(9) 0.1016(8) 0.3092(8) 0.150(7) Uani 1 1 d . . . H45 H 0.4835 0.1224 0.3236 0.181 Uiso 1 1 calc R . . C46 C 0.4397(13) 0.0564(11) 0.2787(14) 0.208(12) Uani 1 1 d . . . H46 H 0.4865 0.0447 0.2744 0.250 Uiso 1 1 calc R . . C47 C 0.3722(15) 0.0281(9) 0.2543(11) 0.202(10) Uani 1 1 d . . . H47 H 0.3727 -0.0018 0.2305 0.243 Uiso 1 1 calc R . . C48 C 0.3011(9) 0.0426(5) 0.2638(7) 0.143(6) Uani 1 1 d . . . H48 H 0.2559 0.0219 0.2482 0.171 Uiso 1 1 calc R . . C49 C 0.1836(4) 0.4048(3) 0.5080(3) 0.0429(18) Uani 1 1 d . . . C50 C 0.2577(4) 0.4216(3) 0.5420(3) 0.0478(19) Uani 1 1 d . . . H50 H 0.2732 0.4392 0.5802 0.057 Uiso 1 1 calc R . . C51 C 0.3050(4) 0.4071(3) 0.5077(3) 0.0484(19) Uani 1 1 d . . . C52 C 0.3915(4) 0.4177(3) 0.5230(4) 0.054(2) Uani 1 1 d . . . C53 C 0.4351(5) 0.3956(4) 0.4910(4) 0.065(3) Uani 1 1 d . . . H53 H 0.4110 0.3721 0.4587 0.078 Uiso 1 1 calc R . . C54 C 0.5148(5) 0.4073(4) 0.5052(5) 0.081(3) Uani 1 1 d . . . H54 H 0.5432 0.3919 0.4823 0.097 Uiso 1 1 calc R . . C55 C 0.5514(6) 0.4413(4) 0.5525(6) 0.090(3) Uani 1 1 d . . . H55 H 0.6049 0.4490 0.5622 0.108 Uiso 1 1 calc R . . C56 C 0.5086(6) 0.4643(4) 0.5861(6) 0.098(4) Uani 1 1 d . . . H56 H 0.5329 0.4876 0.6185 0.118 Uiso 1 1 calc R . . C57 C 0.4295(5) 0.4522(4) 0.5710(4) 0.076(3) Uani 1 1 d . . . H57 H 0.4009 0.4677 0.5936 0.091 Uiso 1 1 calc R . . C58 C 0.1161(6) 0.4274(4) 0.5831(5) 0.074(3) Uani 1 1 d . . . H58 H 0.1659 0.4317 0.6131 0.089 Uiso 1 1 calc R . . C59 C 0.0488(7) 0.4360(5) 0.5988(6) 0.094(4) Uani 1 1 d . . . H59 H 0.0538 0.4464 0.6391 0.113 Uiso 1 1 calc R . . C60 C -0.0225(7) 0.4294(4) 0.5565(7) 0.093(4) Uani 1 1 d . . . H60 H -0.0672 0.4346 0.5676 0.112 Uiso 1 1 calc R . . C61 C -0.0312(6) 0.4149(4) 0.4961(6) 0.086(3) Uani 1 1 d . . . H61 H -0.0815 0.4112 0.4665 0.103 Uiso 1 1 calc R . . C62 C 0.0355(5) 0.4057(3) 0.4793(4) 0.060(2) Uani 1 1 d . . . H62 H 0.0300 0.3952 0.4389 0.072 Uiso 1 1 calc R . . C63 C 0.1092(5) 0.4124(3) 0.5232(4) 0.052(2) Uani 1 1 d . . . C64 C 0.6130(5) 0.2735(4) 0.4327(5) 0.070(3) Uani 1 1 d . . . C65 C 0.5371(7) 0.2790(4) 0.4358(7) 0.106(4) Uani 1 1 d . . . H65 H 0.5315 0.2849 0.4744 0.127 Uiso 1 1 calc R . . C66 C 0.4711(7) 0.2759(6) 0.3841(9) 0.132(6) Uani 1 1 d . . . H66 H 0.4213 0.2777 0.3880 0.158 Uiso 1 1 calc R . . C67 C 0.4778(9) 0.2701(8) 0.3273(9) 0.162(7) Uani 1 1 d . . . H67 H 0.4327 0.2687 0.2918 0.194 Uiso 1 1 calc R . . C68 C 0.5529(8) 0.2661(9) 0.3216(7) 0.204(10) Uani 1 1 d . . . H68 H 0.5580 0.2625 0.2825 0.245 Uiso 1 1 calc R . . C69 C 0.6187(6) 0.2677(7) 0.3747(6) 0.134(6) Uani 1 1 d . . . H69 H 0.6685 0.2647 0.3710 0.161 Uiso 1 1 calc R . . C70 C 0.7225(6) 0.3442(4) 0.5205(6) 0.077(3) Uani 1 1 d . . . C71 C 0.7051(6) 0.3821(5) 0.4757(8) 0.114(5) Uani 1 1 d . . . H71 H 0.6763 0.3735 0.4345 0.137 Uiso 1 1 calc R . . C72 C 0.7306(9) 0.4345(6) 0.4914(12) 0.157(8) Uani 1 1 d . . . H72 H 0.7201 0.4608 0.4611 0.189 Uiso 1 1 calc R . . C73 C 0.7714(13) 0.4452(10) 0.5529(14) 0.173(14) Uani 1 1 d . . . H73 H 0.7896 0.4795 0.5632 0.208 Uiso 1 1 calc R . . C74 C 0.7866(13) 0.4108(9) 0.5981(12) 0.170(11) Uani 1 1 d . . . H74 H 0.8124 0.4206 0.6395 0.204 Uiso 1 1 calc R . . C75 C 0.7621(7) 0.3579(5) 0.5817(7) 0.108(4) Uani 1 1 d . . . H75 H 0.7731 0.3322 0.6126 0.129 Uiso 1 1 calc R . . C76 C 0.7764(5) 0.2475(4) 0.4818(4) 0.062(2) Uani 1 1 d . . . C77 C 0.8372(5) 0.2776(4) 0.4755(4) 0.073(3) Uani 1 1 d . . . H77 H 0.8394 0.3137 0.4833 0.087 Uiso 1 1 calc R . . C78 C 0.8948(6) 0.2533(6) 0.4574(6) 0.108(4) Uani 1 1 d . . . H78 H 0.9365 0.2732 0.4537 0.130 Uiso 1 1 calc R . . C79 C 0.8912(7) 0.2018(7) 0.4453(6) 0.111(5) Uani 1 1 d . . . H79 H 0.9299 0.1864 0.4322 0.133 Uiso 1 1 calc R . . C80 C 0.8334(11) 0.1716(6) 0.4514(7) 0.134(5) Uani 1 1 d . . . H80 H 0.8320 0.1356 0.4428 0.161 Uiso 1 1 calc R . . C81 C 0.7755(8) 0.1943(5) 0.4709(6) 0.109(4) Uani 1 1 d . . . H81 H 0.7359 0.1734 0.4764 0.131 Uiso 1 1 calc R . . C82 C 0.7411(6) 0.2141(5) 0.6761(5) 0.097(4) Uani 1 1 d . . . C83 C 0.8180(7) 0.2139(5) 0.6769(7) 0.109(4) Uani 1 1 d . . . H83 H 0.8271 0.2158 0.6392 0.130 Uiso 1 1 calc R . . C84 C 0.8820(7) 0.2110(7) 0.7316(9) 0.137(6) Uani 1 1 d . . . H84 H 0.9328 0.2085 0.7297 0.164 Uiso 1 1 calc R . . C85 C 0.8723(9) 0.2117(9) 0.7874(9) 0.180(9) Uani 1 1 d . . . H85 H 0.9162 0.2106 0.8238 0.217 Uiso 1 1 calc R . . C86 C 0.7975(8) 0.2140(9) 0.7909(7) 0.214(11) Uani 1 1 d . . . H86 H 0.7900 0.2156 0.8293 0.257 Uiso 1 1 calc R . . C87 C 0.7329(7) 0.2139(8) 0.7349(6) 0.159(7) Uani 1 1 d . . . H87 H 0.6822 0.2136 0.7371 0.191 Uiso 1 1 calc R . . C88 C 0.6498(7) 0.1083(7) 0.6222(8) 0.126(5) Uani 1 1 d . . . H88 H 0.6785 0.1142 0.6641 0.152 Uiso 1 1 calc R . . C89 C 0.6270(9) 0.0567(7) 0.6012(12) 0.156(8) Uani 1 1 d . . . H89 H 0.6392 0.0283 0.6287 0.187 Uiso 1 1 calc R . . C90 C 0.5860(10) 0.0497(9) 0.5387(13) 0.156(9) Uani 1 1 d . . . H90 H 0.5714 0.0155 0.5242 0.187 Uiso 1 1 calc R . . C91 C 0.5663(11) 0.0889(8) 0.4985(11) 0.150(8) Uani 1 1 d . . . H91 H 0.5389 0.0830 0.4563 0.180 Uiso 1 1 calc R . . C92 C 0.5884(9) 0.1402(6) 0.5221(7) 0.126(5) Uani 1 1 d . . . H92 H 0.5728 0.1685 0.4946 0.152 Uiso 1 1 calc R . . C93 C 0.6303(6) 0.1504(5) 0.5814(6) 0.084(3) Uani 1 1 d . . . C94 C 0.5793(6) 0.2466(4) 0.6245(4) 0.070(3) Uani 1 1 d . . . C95 C 0.5206(5) 0.2183(5) 0.6343(4) 0.083(3) Uani 1 1 d . . . H95 H 0.5179 0.1819 0.6286 0.100 Uiso 1 1 calc R . . C96 C 0.4647(6) 0.2446(7) 0.6527(6) 0.117(5) Uani 1 1 d . . . H96 H 0.4244 0.2252 0.6596 0.141 Uiso 1 1 calc R . . C97 C 0.4668(8) 0.2971(8) 0.6610(6) 0.120(5) Uani 1 1 d . . . H97 H 0.4286 0.3138 0.6736 0.144 Uiso 1 1 calc R . . C98 C 0.5243(11) 0.3254(6) 0.6511(7) 0.130(5) Uani 1 1 d . . . H98 H 0.5258 0.3618 0.6566 0.156 Uiso 1 1 calc R . . C99 C 0.5823(8) 0.3006(5) 0.6325(6) 0.112(4) Uani 1 1 d . . . H99 H 0.6223 0.3203 0.6256 0.135 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0367(5) 0.0399(5) 0.0357(5) 0.0000(4) 0.0136(4) 0.0028(4) Cu2 0.0457(5) 0.0412(6) 0.0334(5) -0.0021(4) 0.0136(4) 0.0011(4) Cu3 0.0331(5) 0.0439(6) 0.0367(5) -0.0062(4) 0.0149(4) 0.0001(4) Cu4 0.0379(5) 0.0374(5) 0.0359(5) 0.0031(4) 0.0167(4) -0.0001(4) Cu5 0.0470(5) 0.0330(5) 0.0328(5) -0.0006(4) 0.0145(4) -0.0027(4) Cu6 0.0337(5) 0.0353(5) 0.0342(5) -0.0009(4) 0.0131(4) -0.0006(4) P1 0.0682(16) 0.0673(17) 0.0821(18) -0.0164(13) 0.0484(14) -0.0174(12) P2 0.0736(17) 0.089(2) 0.0783(18) -0.0134(15) 0.0473(14) -0.0217(14) O1 0.043(3) 0.038(3) 0.034(3) -0.004(2) 0.014(2) 0.002(2) O2 0.045(3) 0.029(3) 0.034(3) -0.001(2) 0.016(2) -0.001(2) N1 0.047(4) 0.045(4) 0.033(3) 0.001(3) 0.011(3) 0.006(3) N2 0.053(4) 0.053(4) 0.034(3) -0.005(3) 0.015(3) 0.003(3) N3 0.056(4) 0.050(4) 0.034(3) 0.001(3) 0.019(3) 0.002(3) N4 0.044(4) 0.053(4) 0.039(4) -0.010(3) 0.020(3) 0.002(3) N5 0.051(4) 0.045(4) 0.045(4) -0.008(3) 0.016(3) 0.004(3) N6 0.055(4) 0.044(4) 0.055(4) -0.003(3) 0.024(3) 0.002(3) N7 0.056(4) 0.040(4) 0.033(4) 0.001(3) 0.017(3) -0.003(3) N8 0.061(4) 0.042(4) 0.037(3) -0.004(3) 0.019(3) -0.003(3) N9 0.059(4) 0.041(4) 0.029(3) 0.000(3) 0.016(3) -0.002(3) N10 0.048(4) 0.041(4) 0.033(3) -0.004(3) 0.014(3) -0.002(3) N11 0.049(4) 0.038(4) 0.044(4) -0.003(3) 0.018(3) 0.002(3) N12 0.061(4) 0.038(4) 0.041(4) 0.003(3) 0.020(3) -0.001(3) N13 0.040(3) 0.038(4) 0.042(3) 0.003(3) 0.017(3) 0.001(3) N14 0.036(3) 0.045(4) 0.040(3) 0.004(3) 0.016(3) 0.006(3) N15 0.061(4) 0.040(4) 0.045(4) 0.001(3) 0.017(3) 0.001(3) N16 0.067(4) 0.034(4) 0.038(3) 0.001(3) 0.019(3) 0.001(3) N17 0.036(3) 0.042(4) 0.042(3) -0.006(3) 0.019(3) -0.001(3) N18 0.033(3) 0.047(4) 0.042(4) -0.005(3) 0.014(3) 0.000(3) N19 0.181(11) 0.133(9) 0.104(8) -0.023(7) 0.101(8) -0.070(8) C1 0.074(6) 0.036(5) 0.049(5) -0.002(4) 0.019(4) 0.013(4) C2 0.056(5) 0.059(6) 0.050(5) -0.017(4) 0.025(4) 0.007(4) C3 0.058(5) 0.048(5) 0.043(5) 0.009(4) 0.023(4) 0.001(4) C4 0.073(6) 0.056(6) 0.033(4) -0.011(4) 0.020(4) -0.004(4) C5 0.076(6) 0.078(7) 0.041(5) 0.012(5) 0.020(4) 0.007(5) C6 0.085(6) 0.047(5) 0.040(5) -0.003(4) 0.020(4) 0.003(4) C7 0.104(7) 0.052(6) 0.058(6) 0.007(5) 0.036(5) 0.003(5) C8 0.095(7) 0.037(5) 0.083(7) -0.006(5) 0.030(6) -0.010(5) C9 0.075(6) 0.055(6) 0.066(6) -0.009(5) 0.025(5) -0.002(5) C10 0.095(7) 0.027(4) 0.058(5) 0.000(4) 0.033(5) -0.006(4) C11 0.097(7) 0.070(7) 0.027(4) -0.011(4) 0.019(4) -0.018(5) C12 0.081(6) 0.050(5) 0.037(5) 0.003(4) 0.025(4) -0.002(4) C13 0.060(5) 0.041(5) 0.037(4) -0.011(3) 0.019(4) -0.005(4) C14 0.060(5) 0.066(6) 0.035(4) 0.015(4) 0.021(4) -0.010(4) C15 0.074(6) 0.027(4) 0.043(5) -0.002(4) 0.015(4) -0.010(4) C16 0.100(7) 0.047(6) 0.055(6) 0.019(4) 0.028(5) 0.006(5) C17 0.102(7) 0.027(5) 0.083(7) 0.009(5) 0.035(6) 0.014(5) C18 0.085(6) 0.039(5) 0.051(5) -0.003(4) 0.029(4) 0.002(4) C19 0.046(4) 0.040(4) 0.041(4) 0.007(3) 0.019(4) -0.001(3) C20 0.048(4) 0.047(5) 0.040(4) 0.013(3) 0.021(4) 0.000(4) C21 0.041(4) 0.041(4) 0.047(5) 0.006(4) 0.017(4) 0.002(3) C22 0.043(4) 0.045(5) 0.052(5) 0.015(4) 0.015(4) 0.001(4) C23 0.048(5) 0.095(8) 0.073(6) 0.031(5) 0.022(5) 0.008(5) C24 0.057(6) 0.121(10) 0.122(10) 0.045(8) 0.043(6) 0.011(6) C25 0.033(5) 0.093(8) 0.122(9) 0.021(7) 0.021(5) 0.010(5) C26 0.047(5) 0.078(7) 0.094(7) 0.029(6) 0.009(5) 0.010(5) C27 0.052(5) 0.056(6) 0.074(6) 0.020(5) 0.020(4) 0.003(4) C28 0.051(5) 0.040(5) 0.061(5) 0.001(4) 0.032(4) -0.001(4) C29 0.049(5) 0.076(7) 0.075(6) 0.011(5) 0.036(5) -0.004(4) C30 0.051(6) 0.102(9) 0.131(10) 0.008(7) 0.042(6) -0.001(5) C31 0.080(8) 0.074(8) 0.151(12) -0.009(7) 0.087(8) -0.007(6) C32 0.103(8) 0.063(7) 0.104(8) 0.008(6) 0.081(7) -0.002(6) C33 0.069(6) 0.053(6) 0.073(6) 0.007(4) 0.043(5) 0.002(4) C34 0.080(6) 0.042(5) 0.054(5) 0.001(4) 0.025(4) -0.003(5) C35 0.111(8) 0.038(5) 0.078(7) 0.006(5) 0.037(6) 0.008(5) C36 0.085(7) 0.047(6) 0.058(6) 0.011(4) 0.024(5) 0.012(5) C37 0.091(7) 0.046(5) 0.053(5) -0.015(4) 0.030(5) -0.022(5) C38 0.120(9) 0.042(5) 0.067(6) -0.009(4) 0.049(6) -0.023(5) C39 0.132(11) 0.062(7) 0.096(8) -0.021(6) 0.073(8) -0.027(7) C40 0.113(10) 0.092(10) 0.130(11) -0.039(8) 0.083(9) -0.046(8) C41 0.087(8) 0.082(8) 0.119(9) -0.016(7) 0.046(7) -0.022(6) C42 0.082(7) 0.060(6) 0.077(7) -0.006(5) 0.033(5) -0.020(5) C43 0.094(8) 0.065(7) 0.100(8) 0.020(6) 0.047(7) 0.035(6) C44 0.079(8) 0.111(10) 0.110(9) 0.020(7) 0.039(7) 0.039(7) C45 0.109(12) 0.171(18) 0.185(17) 0.038(13) 0.067(11) 0.063(12) C46 0.144(18) 0.20(3) 0.32(3) 0.01(2) 0.13(2) 0.085(18) C47 0.23(2) 0.17(2) 0.25(3) -0.025(17) 0.14(2) 0.100(19) C48 0.167(14) 0.085(10) 0.202(16) -0.026(10) 0.097(12) 0.042(9) C49 0.048(5) 0.044(5) 0.042(4) -0.003(4) 0.022(4) -0.001(4) C50 0.056(5) 0.049(5) 0.042(4) -0.017(4) 0.021(4) -0.003(4) C51 0.048(5) 0.049(5) 0.044(5) -0.007(4) 0.011(4) -0.005(4) C52 0.038(4) 0.060(6) 0.060(5) -0.008(4) 0.009(4) 0.002(4) C53 0.041(5) 0.079(7) 0.074(6) -0.027(5) 0.018(4) -0.008(4) C54 0.053(6) 0.084(8) 0.108(8) -0.017(6) 0.030(6) 0.000(5) C55 0.048(6) 0.083(8) 0.126(10) -0.026(7) 0.013(6) -0.013(5) C56 0.062(7) 0.090(9) 0.124(10) -0.049(7) 0.008(6) -0.017(6) C57 0.053(6) 0.086(7) 0.082(7) -0.033(6) 0.013(5) -0.008(5) C58 0.083(7) 0.080(7) 0.076(7) -0.016(5) 0.050(5) -0.003(5) C59 0.100(9) 0.105(9) 0.113(9) -0.036(7) 0.081(8) -0.005(7) C60 0.093(9) 0.073(8) 0.154(12) -0.006(8) 0.094(9) 0.005(6) C61 0.059(6) 0.082(8) 0.128(10) -0.008(7) 0.048(6) -0.004(5) C62 0.047(5) 0.071(6) 0.075(6) -0.007(5) 0.037(5) 0.009(4) C63 0.057(5) 0.044(5) 0.066(6) 0.002(4) 0.034(4) 0.006(4) C64 0.056(5) 0.076(7) 0.092(7) -0.019(5) 0.045(5) -0.015(5) C65 0.078(8) 0.088(9) 0.183(14) -0.048(8) 0.085(9) -0.031(6) C66 0.047(7) 0.138(13) 0.215(18) -0.061(12) 0.050(10) -0.020(7) C67 0.076(10) 0.23(2) 0.160(16) -0.050(15) 0.016(10) -0.002(10) C68 0.069(9) 0.41(3) 0.118(13) -0.055(16) 0.016(9) -0.013(13) C69 0.051(7) 0.260(19) 0.101(10) -0.037(10) 0.037(7) -0.018(8) C70 0.056(6) 0.069(7) 0.126(9) -0.030(7) 0.057(6) -0.013(5) C71 0.069(7) 0.068(9) 0.207(15) 0.007(9) 0.049(8) 0.005(6) C72 0.092(11) 0.068(11) 0.32(3) 0.020(13) 0.079(14) 0.013(8) C73 0.092(13) 0.14(2) 0.33(4) -0.11(2) 0.13(2) -0.034(14) C74 0.120(14) 0.20(3) 0.23(3) -0.14(2) 0.114(18) -0.085(17) C75 0.095(9) 0.112(11) 0.132(11) -0.051(9) 0.060(8) -0.032(7) C76 0.072(6) 0.063(6) 0.055(5) 0.003(4) 0.028(4) 0.007(5) C77 0.051(5) 0.083(7) 0.085(7) -0.023(6) 0.024(5) 0.002(5) C78 0.049(6) 0.149(13) 0.125(10) -0.047(9) 0.027(6) -0.006(7) C79 0.074(8) 0.152(15) 0.101(9) -0.030(10) 0.022(7) 0.040(9) C80 0.171(16) 0.095(11) 0.151(14) 0.001(9) 0.074(12) 0.058(11) C81 0.143(11) 0.073(8) 0.138(11) -0.001(7) 0.083(9) 0.011(8) C82 0.075(7) 0.142(11) 0.095(8) -0.015(8) 0.057(6) 0.002(7) C83 0.069(8) 0.128(11) 0.151(12) -0.050(9) 0.067(9) -0.002(7) C84 0.047(7) 0.168(15) 0.195(17) -0.063(13) 0.040(10) -0.001(8) C85 0.077(11) 0.28(3) 0.166(18) -0.045(17) 0.018(11) 0.010(12) C86 0.052(8) 0.46(4) 0.121(13) 0.001(17) 0.012(8) 0.038(13) C87 0.063(8) 0.31(2) 0.100(10) 0.004(12) 0.021(7) 0.023(10) C88 0.076(8) 0.120(13) 0.182(16) -0.001(12) 0.042(9) -0.008(8) C89 0.089(11) 0.096(13) 0.29(3) 0.006(15) 0.074(14) 0.007(9) C90 0.092(12) 0.142(18) 0.27(3) -0.078(19) 0.105(16) -0.028(13) C91 0.162(17) 0.127(16) 0.20(2) -0.054(14) 0.111(15) -0.053(14) C92 0.163(13) 0.129(13) 0.117(11) -0.034(9) 0.086(10) -0.074(10) C93 0.068(7) 0.095(9) 0.108(9) -0.010(8) 0.054(7) -0.014(6) C94 0.077(7) 0.080(7) 0.056(6) 0.000(5) 0.027(5) -0.001(6) C95 0.051(6) 0.123(10) 0.081(7) -0.024(6) 0.030(5) -0.009(6) C96 0.046(6) 0.190(16) 0.114(10) -0.036(11) 0.025(6) -0.012(8) C97 0.081(9) 0.177(17) 0.095(10) -0.022(11) 0.020(7) 0.034(10) C98 0.171(15) 0.105(11) 0.138(13) 0.020(9) 0.084(12) 0.045(11) C99 0.134(11) 0.098(10) 0.134(11) -0.003(8) 0.082(9) 0.015(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.883(5) . ? Cu1 N6 1.957(7) . ? Cu1 N1 1.964(6) . ? Cu1 N14 2.020(6) . ? Cu1 Cu4 2.999(3) . ? Cu2 O1 1.894(5) . ? Cu2 N2 1.934(6) . ? Cu2 N3 1.942(6) . ? Cu2 N15 2.043(7) . ? Cu2 Cu5 2.975(3) . ? Cu3 O1 1.886(5) . ? Cu3 N5 1.946(7) . ? Cu3 N4 1.949(7) . ? Cu3 N18 2.050(6) . ? Cu3 Cu6 3.028(3) . ? Cu4 O2 1.890(5) . ? Cu4 N12 1.940(6) . ? Cu4 N7 1.943(6) . ? Cu4 N13 2.051(6) . ? Cu5 O2 1.886(5) . ? Cu5 N9 1.943(6) . ? Cu5 N8 1.953(6) . ? Cu5 N16 2.007(6) . ? Cu6 O2 1.883(5) . ? Cu6 N10 1.946(6) . ? Cu6 N11 1.949(6) . ? Cu6 N17 2.026(6) . ? P1 N19 1.554(9) . ? P1 C64 1.772(10) . ? P1 C70 1.789(10) . ? P1 C76 1.795(9) . ? P2 N19 1.532(9) . ? P2 C82 1.760(12) . ? P2 C94 1.793(10) . ? P2 C93 1.799(12) . ? N1 C3 1.324(9) . ? N1 N2 1.349(8) . ? N2 C1 1.339(9) . ? N3 C6 1.337(10) . ? N3 N4 1.343(8) . ? N4 C4 1.338(9) . ? N5 C9 1.339(10) . ? N5 N6 1.348(8) . ? N6 C7 1.343(10) . ? N7 C12 1.337(9) . ? N7 N8 1.348(8) . ? N8 C10 1.336(9) . ? N9 N10 1.342(8) . ? N9 C15 1.349(9) . ? N10 C13 1.335(9) . ? N11 N12 1.341(8) . ? N11 C18 1.358(9) . ? N12 C16 1.345(10) . ? N13 C21 1.340(9) . ? N13 N14 1.376(7) . ? N14 C19 1.336(8) . ? N15 C36 1.345(10) . ? N15 N16 1.370(9) . ? N16 C34 1.345(10) . ? N17 C49 1.341(9) . ? N17 N18 1.371(7) . ? N18 C51 1.335(9) . ? C1 C2 1.365(11) . ? C1 H1 0.9300 . ? C2 C3 1.368(11) . ? C2 H2 0.9300 . ? C3 H3 0.9300 . ? C4 C5 1.393(11) . ? C4 H4 0.9300 . ? C5 C6 1.373(11) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.386(12) . ? C7 H7 0.9300 . ? C8 C9 1.380(12) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C11 1.368(11) . ? C10 H10 0.9300 . ? C11 C12 1.386(11) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.378(10) . ? C13 H13 0.9300 . ? C14 C15 1.363(10) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.381(12) . ? C16 H16 0.9300 . ? C17 C18 1.354(11) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C20 1.376(10) . ? C19 C28 1.492(10) . ? C20 C21 1.402(9) . ? C20 H20 0.9300 . ? C21 C22 1.487(10) . ? C22 C23 1.372(11) . ? C22 C27 1.384(10) . ? C23 C24 1.364(12) . ? C23 H23 0.9300 . ? C24 C25 1.373(13) . ? C24 H24 0.9300 . ? C25 C26 1.352(13) . ? C25 H25 0.9300 . ? C26 C27 1.378(11) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C33 1.371(11) . ? C28 C29 1.390(11) . ? C29 C30 1.411(12) . ? C29 H29 0.9300 . ? C30 C31 1.363(15) . ? C30 H30 0.9300 . ? C31 C32 1.348(14) . ? C31 H31 0.9300 . ? C32 C33 1.412(12) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C35 1.391(12) . ? C34 C37 1.481(12) . ? C35 C36 1.390(13) . ? C35 H35 0.9300 . ? C36 C43 1.475(13) . ? C37 C42 1.378(13) . ? C37 C38 1.400(12) . ? C38 C39 1.370(14) . ? C38 H38 0.9300 . ? C39 C40 1.353(16) . ? C39 H39 0.9300 . ? C40 C41 1.394(16) . ? C40 H40 0.9300 . ? C41 C42 1.383(13) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? C43 C44 1.374(15) . ? C43 C48 1.386(16) . ? C44 C45 1.401(17) . ? C44 H44 0.9300 . ? C45 C46 1.34(3) . ? C45 H45 0.9300 . ? C46 C47 1.35(3) . ? C46 H46 0.9300 . ? C47 C48 1.42(2) . ? C47 H47 0.9300 . ? C48 H48 0.9300 . ? C49 C50 1.362(10) . ? C49 C63 1.503(10) . ? C50 C51 1.387(10) . ? C50 H50 0.9300 . ? C51 C52 1.497(10) . ? C52 C53 1.360(11) . ? C52 C57 1.383(11) . ? C53 C54 1.390(12) . ? C53 H53 0.9300 . ? C54 C55 1.360(13) . ? C54 H54 0.9300 . ? C55 C56 1.384(14) . ? C55 H55 0.9300 . ? C56 C57 1.380(12) . ? C56 H56 0.9300 . ? C57 H57 0.9300 . ? C58 C63 1.379(11) . ? C58 C59 1.391(13) . ? C58 H58 0.9300 . ? C59 C60 1.326(15) . ? C59 H59 0.9300 . ? C60 C61 1.380(15) . ? C60 H60 0.9300 . ? C61 C62 1.396(11) . ? C61 H61 0.9300 . ? C62 C63 1.372(11) . ? C62 H62 0.9300 . ? C64 C69 1.366(14) . ? C64 C65 1.397(13) . ? C65 C66 1.359(18) . ? C65 H65 0.9300 . ? C66 C67 1.35(2) . ? C66 H66 0.9300 . ? C67 C68 1.402(19) . ? C67 H67 0.9300 . ? C68 C69 1.375(17) . ? C68 H68 0.9300 . ? C69 H69 0.9300 . ? C70 C71 1.358(16) . ? C70 C75 1.375(15) . ? C71 C72 1.409(19) . ? C71 H71 0.9300 . ? C72 C73 1.37(3) . ? C72 H72 0.9300 . ? C73 C74 1.30(3) . ? C73 H73 0.9300 . ? C74 C75 1.42(2) . ? C74 H74 0.9300 . ? C75 H75 0.9300 . ? C76 C81 1.369(14) . ? C76 C77 1.379(12) . ? C77 C78 1.381(14) . ? C77 H77 0.9300 . ? C78 C79 1.330(18) . ? C78 H78 0.9300 . ? C79 C80 1.334(19) . ? C79 H79 0.9300 . ? C80 C81 1.387(16) . ? C80 H80 0.9300 . ? C81 H81 0.9300 . ? C82 C83 1.376(13) . ? C82 C87 1.396(16) . ? C83 C84 1.381(18) . ? C83 H83 0.9300 . ? C84 C85 1.34(2) . ? C84 H84 0.9300 . ? C85 C86 1.375(19) . ? C85 H85 0.9300 . ? C86 C87 1.401(17) . ? C86 H86 0.9300 . ? C87 H87 0.9300 . ? C88 C93 1.378(17) . ? C88 C89 1.40(2) . ? C88 H88 0.9300 . ? C89 C90 1.37(2) . ? C89 H89 0.9300 . ? C90 C91 1.32(2) . ? C90 H90 0.9300 . ? C91 C92 1.410(19) . ? C91 H91 0.9300 . ? C92 C93 1.328(16) . ? C92 H92 0.9300 . ? C94 C95 1.354(13) . ? C94 C99 1.379(15) . ? C95 C96 1.385(15) . ? C95 H95 0.9300 . ? C96 C97 1.342(19) . ? C96 H96 0.9300 . ? C97 C98 1.339(19) . ? C97 H97 0.9300 . ? C98 C99 1.400(17) . ? C98 H98 0.9300 . ? C99 H99 0.9300 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N6 90.1(2) . . ? O1 Cu1 N1 90.1(2) . . ? N6 Cu1 N1 163.8(3) . . ? O1 Cu1 N14 158.8(2) . . ? N6 Cu1 N14 90.2(3) . . ? N1 Cu1 N14 95.4(2) . . ? O1 Cu1 Cu4 91.20(14) . . ? N6 Cu1 Cu4 89.96(18) . . ? N1 Cu1 Cu4 106.27(17) . . ? N14 Cu1 Cu4 67.58(16) . . ? O1 Cu2 N2 90.7(2) . . ? O1 Cu2 N3 88.3(2) . . ? N2 Cu2 N3 165.3(3) . . ? O1 Cu2 N15 162.6(2) . . ? N2 Cu2 N15 95.3(3) . . ? N3 Cu2 N15 89.9(3) . . ? O1 Cu2 Cu5 95.99(14) . . ? N2 Cu2 Cu5 109.27(18) . . ? N3 Cu2 Cu5 85.41(18) . . ? N15 Cu2 Cu5 66.6(2) . . ? O1 Cu3 N5 90.3(2) . . ? O1 Cu3 N4 88.6(2) . . ? N5 Cu3 N4 168.1(2) . . ? O1 Cu3 N18 168.6(2) . . ? N5 Cu3 N18 92.3(3) . . ? N4 Cu3 N18 91.1(2) . . ? O1 Cu3 Cu6 103.55(14) . . ? N5 Cu3 Cu6 99.89(18) . . ? N4 Cu3 Cu6 91.85(17) . . ? N18 Cu3 Cu6 65.07(15) . . ? O2 Cu4 N12 89.1(2) . . ? O2 Cu4 N7 89.1(2) . . ? N12 Cu4 N7 167.5(3) . . ? O2 Cu4 N13 168.3(2) . . ? N12 Cu4 N13 94.1(2) . . ? N7 Cu4 N13 90.1(2) . . ? O2 Cu4 Cu1 102.89(13) . . ? N12 Cu4 Cu1 101.59(19) . . ? N7 Cu4 Cu1 90.88(18) . . ? N13 Cu4 Cu1 65.43(16) . . ? O2 Cu5 N9 90.7(2) . . ? O2 Cu5 N8 89.1(2) . . ? N9 Cu5 N8 166.7(3) . . ? O2 Cu5 N16 165.1(2) . . ? N9 Cu5 N16 94.1(2) . . ? N8 Cu5 N16 89.4(2) . . ? O2 Cu5 Cu2 98.67(13) . . ? N9 Cu5 Cu2 108.32(18) . . ? N8 Cu5 Cu2 84.83(18) . . ? N16 Cu5 Cu2 66.42(19) . . ? O2 Cu6 N10 90.6(2) . . ? O2 Cu6 N11 89.0(2) . . ? N10 Cu6 N11 162.1(2) . . ? O2 Cu6 N17 156.6(2) . . ? N10 Cu6 N17 94.6(2) . . ? N11 Cu6 N17 92.8(3) . . ? O2 Cu6 Cu3 89.67(14) . . ? N10 Cu6 Cu3 103.48(17) . . ? N11 Cu6 Cu3 94.38(17) . . ? N17 Cu6 Cu3 66.90(16) . . ? N19 P1 C64 112.6(5) . . ? N19 P1 C70 110.5(6) . . ? C64 P1 C70 108.9(5) . . ? N19 P1 C76 112.1(6) . . ? C64 P1 C76 105.6(4) . . ? C70 P1 C76 106.8(4) . . ? N19 P2 C82 108.7(6) . . ? N19 P2 C94 113.6(6) . . ? C82 P2 C94 107.3(5) . . ? N19 P2 C93 111.8(6) . . ? C82 P2 C93 108.1(6) . . ? C94 P2 C93 107.1(5) . . ? Cu1 O1 Cu3 118.5(3) . . ? Cu1 O1 Cu2 116.6(2) . . ? Cu3 O1 Cu2 120.3(2) . . ? Cu6 O2 Cu5 116.6(2) . . ? Cu6 O2 Cu4 119.2(2) . . ? Cu5 O2 Cu4 119.6(2) . . ? C3 N1 N2 107.9(6) . . ? C3 N1 Cu1 133.7(5) . . ? N2 N1 Cu1 118.1(4) . . ? C1 N2 N1 106.9(6) . . ? C1 N2 Cu2 134.1(6) . . ? N1 N2 Cu2 119.0(5) . . ? C6 N3 N4 108.1(6) . . ? C6 N3 Cu2 131.2(5) . . ? N4 N3 Cu2 120.6(5) . . ? C4 N4 N3 107.9(6) . . ? C4 N4 Cu3 133.1(5) . . ? N3 N4 Cu3 119.0(4) . . ? C9 N5 N6 108.0(7) . . ? C9 N5 Cu3 133.1(6) . . ? N6 N5 Cu3 118.8(5) . . ? C7 N6 N5 108.4(6) . . ? C7 N6 Cu1 132.5(6) . . ? N5 N6 Cu1 119.1(5) . . ? C12 N7 N8 108.1(6) . . ? C12 N7 Cu4 132.7(5) . . ? N8 N7 Cu4 119.1(4) . . ? C10 N8 N7 107.8(6) . . ? C10 N8 Cu5 132.6(5) . . ? N7 N8 Cu5 119.5(4) . . ? N10 N9 C15 107.5(6) . . ? N10 N9 Cu5 118.8(4) . . ? C15 N9 Cu5 133.5(5) . . ? C13 N10 N9 107.9(6) . . ? C13 N10 Cu6 133.2(5) . . ? N9 N10 Cu6 118.4(4) . . ? N12 N11 C18 107.7(6) . . ? N12 N11 Cu6 118.8(4) . . ? C18 N11 Cu6 133.5(5) . . ? N11 N12 C16 107.4(6) . . ? N11 N12 Cu4 120.0(4) . . ? C16 N12 Cu4 132.6(6) . . ? C21 N13 N14 107.4(5) . . ? C21 N13 Cu4 137.9(5) . . ? N14 N13 Cu4 114.6(4) . . ? C19 N14 N13 108.9(5) . . ? C19 N14 Cu1 138.8(5) . . ? N13 N14 Cu1 112.3(4) . . ? C36 N15 N16 107.5(7) . . ? C36 N15 Cu2 140.8(6) . . ? N16 N15 Cu2 111.5(5) . . ? C34 N16 N15 109.2(6) . . ? C34 N16 Cu5 135.7(6) . . ? N15 N16 Cu5 114.7(5) . . ? C49 N17 N18 107.6(5) . . ? C49 N17 Cu6 139.5(5) . . ? N18 N17 Cu6 112.9(4) . . ? C51 N18 N17 107.8(6) . . ? C51 N18 Cu3 136.9(5) . . ? N17 N18 Cu3 115.0(4) . . ? P2 N19 P1 172.2(8) . . ? N2 C1 C2 110.9(7) . . ? N2 C1 H1 124.5 . . ? C2 C1 H1 124.5 . . ? C1 C2 C3 103.4(7) . . ? C1 C2 H2 128.3 . . ? C3 C2 H2 128.3 . . ? N1 C3 C2 110.9(7) . . ? N1 C3 H3 124.5 . . ? C2 C3 H3 124.5 . . ? N4 C4 C5 110.0(7) . . ? N4 C4 H4 125.0 . . ? C5 C4 H4 125.0 . . ? C6 C5 C4 103.4(7) . . ? C6 C5 H5 128.3 . . ? C4 C5 H5 128.3 . . ? N3 C6 C5 110.6(8) . . ? N3 C6 H6 124.7 . . ? C5 C6 H6 124.7 . . ? N6 C7 C8 109.3(8) . . ? N6 C7 H7 125.4 . . ? C8 C7 H7 125.4 . . ? C9 C8 C7 104.4(8) . . ? C9 C8 H8 127.8 . . ? C7 C8 H8 127.8 . . ? N5 C9 C8 109.9(8) . . ? N5 C9 H9 125.1 . . ? C8 C9 H9 125.1 . . ? N8 C10 C11 110.4(7) . . ? N8 C10 H10 124.8 . . ? C11 C10 H10 124.8 . . ? C10 C11 C12 104.1(7) . . ? C10 C11 H11 128.0 . . ? C12 C11 H11 128.0 . . ? N7 C12 C11 109.5(7) . . ? N7 C12 H12 125.2 . . ? C11 C12 H12 125.2 . . ? N10 C13 C14 110.4(6) . . ? N10 C13 H13 124.8 . . ? C14 C13 H13 124.8 . . ? C15 C14 C13 103.8(7) . . ? C15 C14 H14 128.1 . . ? C13 C14 H14 128.1 . . ? N9 C15 C14 110.4(7) . . ? N9 C15 H15 124.8 . . ? C14 C15 H15 124.8 . . ? N12 C16 C17 110.4(7) . . ? N12 C16 H16 124.8 . . ? C17 C16 H16 124.8 . . ? C18 C17 C16 104.0(7) . . ? C18 C17 H17 128.0 . . ? C16 C17 H17 128.0 . . ? C17 C18 N11 110.5(7) . . ? C17 C18 H18 124.7 . . ? N11 C18 H18 124.7 . . ? N14 C19 C20 109.3(6) . . ? N14 C19 C28 123.4(6) . . ? C20 C19 C28 127.2(7) . . ? C19 C20 C21 105.3(6) . . ? C19 C20 H20 127.3 . . ? C21 C20 H20 127.3 . . ? N13 C21 C20 109.2(6) . . ? N13 C21 C22 123.8(6) . . ? C20 C21 C22 127.0(7) . . ? C23 C22 C27 117.9(7) . . ? C23 C22 C21 122.8(7) . . ? C27 C22 C21 119.2(7) . . ? C24 C23 C22 121.0(9) . . ? C24 C23 H23 119.5 . . ? C22 C23 H23 119.5 . . ? C23 C24 C25 120.4(9) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C26 C25 C24 119.7(9) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 120.1(9) . . ? C25 C26 H26 120.0 . . ? C27 C26 H26 120.0 . . ? C26 C27 C22 120.9(8) . . ? C26 C27 H27 119.6 . . ? C22 C27 H27 119.6 . . ? C33 C28 C29 119.4(7) . . ? C33 C28 C19 119.6(7) . . ? C29 C28 C19 120.9(7) . . ? C28 C29 C30 119.1(9) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? C31 C30 C29 121.3(10) . . ? C31 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C32 C31 C30 118.9(9) . . ? C32 C31 H31 120.5 . . ? C30 C31 H31 120.5 . . ? C31 C32 C33 121.8(10) . . ? C31 C32 H32 119.1 . . ? C33 C32 H32 119.1 . . ? C28 C33 C32 119.4(9) . . ? C28 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? N16 C34 C35 108.2(8) . . ? N16 C34 C37 121.4(8) . . ? C35 C34 C37 130.4(8) . . ? C36 C35 C34 105.7(8) . . ? C36 C35 H35 127.1 . . ? C34 C35 H35 127.1 . . ? N15 C36 C35 109.4(8) . . ? N15 C36 C43 122.3(9) . . ? C35 C36 C43 128.3(9) . . ? C42 C37 C38 118.2(9) . . ? C42 C37 C34 121.9(8) . . ? C38 C37 C34 119.8(9) . . ? C39 C38 C37 120.6(11) . . ? C39 C38 H38 119.7 . . ? C37 C38 H38 119.7 . . ? C40 C39 C38 120.1(11) . . ? C40 C39 H39 119.9 . . ? C38 C39 H39 119.9 . . ? C39 C40 C41 121.4(11) . . ? C39 C40 H40 119.3 . . ? C41 C40 H40 119.3 . . ? C42 C41 C40 118.0(12) . . ? C42 C41 H41 121.0 . . ? C40 C41 H41 121.0 . . ? C37 C42 C41 121.7(10) . . ? C37 C42 H42 119.2 . . ? C41 C42 H42 119.2 . . ? C44 C43 C48 118.7(12) . . ? C44 C43 C36 121.1(10) . . ? C48 C43 C36 120.2(12) . . ? C43 C44 C45 121.2(14) . . ? C43 C44 H44 119.4 . . ? C45 C44 H44 119.4 . . ? C46 C45 C44 120.3(19) . . ? C46 C45 H45 119.8 . . ? C44 C45 H45 119.8 . . ? C45 C46 C47 119(2) . . ? C45 C46 H46 120.3 . . ? C47 C46 H46 120.3 . . ? C46 C47 C48 122(2) . . ? C46 C47 H47 119.1 . . ? C48 C47 H47 119.1 . . ? C43 C48 C47 118.3(17) . . ? C43 C48 H48 120.9 . . ? C47 C48 H48 120.9 . . ? N17 C49 C50 109.9(6) . . ? N17 C49 C63 122.9(7) . . ? C50 C49 C63 127.1(7) . . ? C49 C50 C51 105.4(7) . . ? C49 C50 H50 127.3 . . ? C51 C50 H50 127.3 . . ? N18 C51 C50 109.2(6) . . ? N18 C51 C52 123.2(7) . . ? C50 C51 C52 127.5(7) . . ? C53 C52 C57 117.6(8) . . ? C53 C52 C51 122.9(7) . . ? C57 C52 C51 119.5(7) . . ? C52 C53 C54 121.6(8) . . ? C52 C53 H53 119.2 . . ? C54 C53 H53 119.2 . . ? C55 C54 C53 120.2(9) . . ? C55 C54 H54 119.9 . . ? C53 C54 H54 119.9 . . ? C54 C55 C56 119.5(9) . . ? C54 C55 H55 120.2 . . ? C56 C55 H55 120.2 . . ? C57 C56 C55 119.2(9) . . ? C57 C56 H56 120.4 . . ? C55 C56 H56 120.4 . . ? C56 C57 C52 121.9(9) . . ? C56 C57 H57 119.1 . . ? C52 C57 H57 119.1 . . ? C63 C58 C59 120.2(10) . . ? C63 C58 H58 119.9 . . ? C59 C58 H58 119.9 . . ? C60 C59 C58 120.2(11) . . ? C60 C59 H59 119.9 . . ? C58 C59 H59 119.9 . . ? C59 C60 C61 120.8(10) . . ? C59 C60 H60 119.6 . . ? C61 C60 H60 119.6 . . ? C60 C61 C62 120.0(10) . . ? C60 C61 H61 120.0 . . ? C62 C61 H61 120.0 . . ? C63 C62 C61 119.1(9) . . ? C63 C62 H62 120.4 . . ? C61 C62 H62 120.4 . . ? C62 C63 C58 119.6(8) . . ? C62 C63 C49 122.0(7) . . ? C58 C63 C49 118.4(8) . . ? C69 C64 C65 117.0(11) . . ? C69 C64 P1 122.7(7) . . ? C65 C64 P1 120.2(9) . . ? C66 C65 C64 122.1(12) . . ? C66 C65 H65 119.0 . . ? C64 C65 H65 119.0 . . ? C67 C66 C65 120.0(13) . . ? C67 C66 H66 120.0 . . ? C65 C66 H66 120.0 . . ? C66 C67 C68 119.9(15) . . ? C66 C67 H67 120.0 . . ? C68 C67 H67 120.0 . . ? C69 C68 C67 119.0(15) . . ? C69 C68 H68 120.5 . . ? C67 C68 H68 120.5 . . ? C64 C69 C68 121.8(12) . . ? C64 C69 H69 119.1 . . ? C68 C69 H69 119.1 . . ? C71 C70 C75 119.3(12) . . ? C71 C70 P1 121.6(10) . . ? C75 C70 P1 119.1(10) . . ? C70 C71 C72 120.3(16) . . ? C70 C71 H71 119.9 . . ? C72 C71 H71 119.9 . . ? C73 C72 C71 117(2) . . ? C73 C72 H72 121.3 . . ? C71 C72 H72 121.3 . . ? C74 C73 C72 125(3) . . ? C74 C73 H73 117.5 . . ? C72 C73 H73 117.5 . . ? C73 C74 C75 117(3) . . ? C73 C74 H74 121.4 . . ? C75 C74 H74 121.4 . . ? C70 C75 C74 120.9(17) . . ? C70 C75 H75 119.6 . . ? C74 C75 H75 119.6 . . ? C81 C76 C77 119.0(9) . . ? C81 C76 P1 119.0(8) . . ? C77 C76 P1 121.9(8) . . ? C76 C77 C78 119.1(11) . . ? C76 C77 H77 120.4 . . ? C78 C77 H77 120.4 . . ? C79 C78 C77 120.6(12) . . ? C79 C78 H78 119.7 . . ? C77 C78 H78 119.7 . . ? C78 C79 C80 121.6(13) . . ? C78 C79 H79 119.2 . . ? C80 C79 H79 119.2 . . ? C79 C80 C81 119.4(14) . . ? C79 C80 H80 120.3 . . ? C81 C80 H80 120.3 . . ? C76 C81 C80 120.1(13) . . ? C76 C81 H81 119.9 . . ? C80 C81 H81 119.9 . . ? C83 C82 C87 114.9(12) . . ? C83 C82 P2 122.5(9) . . ? C87 C82 P2 122.6(8) . . ? C82 C83 C84 122.5(13) . . ? C82 C83 H83 118.7 . . ? C84 C83 H83 118.7 . . ? C85 C84 C83 121.1(13) . . ? C85 C84 H84 119.5 . . ? C83 C84 H84 119.5 . . ? C84 C85 C86 120.1(16) . . ? C84 C85 H85 119.9 . . ? C86 C85 H85 119.9 . . ? C85 C86 C87 118.1(16) . . ? C85 C86 H86 121.0 . . ? C87 C86 H86 121.0 . . ? C82 C87 C86 123.1(13) . . ? C82 C87 H87 118.4 . . ? C86 C87 H87 118.4 . . ? C93 C88 C89 120.8(17) . . ? C93 C88 H88 119.6 . . ? C89 C88 H88 119.6 . . ? C90 C89 C88 118(2) . . ? C90 C89 H89 121.1 . . ? C88 C89 H89 121.1 . . ? C91 C90 C89 123(2) . . ? C91 C90 H90 118.5 . . ? C89 C90 H90 118.5 . . ? C90 C91 C92 117(2) . . ? C90 C91 H91 121.4 . . ? C92 C91 H91 121.4 . . ? C93 C92 C91 123.7(17) . . ? C93 C92 H92 118.1 . . ? C91 C92 H92 118.1 . . ? C92 C93 C88 117.4(13) . . ? C92 C93 P2 120.5(12) . . ? C88 C93 P2 122.1(12) . . ? C95 C94 C99 120.1(10) . . ? C95 C94 P2 123.3(9) . . ? C99 C94 P2 116.5(8) . . ? C94 C95 C96 118.9(12) . . ? C94 C95 H95 120.6 . . ? C96 C95 H95 120.6 . . ? C97 C96 C95 122.0(14) . . ? C97 C96 H96 119.0 . . ? C95 C96 H96 119.0 . . ? C98 C97 C96 119.5(14) . . ? C98 C97 H97 120.2 . . ? C96 C97 H97 120.2 . . ? C97 C98 C99 120.7(15) . . ? C97 C98 H98 119.7 . . ? C99 C98 H98 119.7 . . ? C94 C99 C98 118.9(13) . . ? C94 C99 H99 120.5 . . ? C98 C99 H99 120.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.34 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.292 _refine_diff_density_min -0.772 _refine_diff_density_rms 0.175 #===END data_PPN[4] _database_code_depnum_ccdc_archive 'CCDC 617269' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C101 H79 Cl10 Cu6 N19 O2 P2' _chemical_formula_weight 2388.51 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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6703(14) _cell_length_b 20.722(2) _cell_length_c 21.286(3) _cell_angle_alpha 97.971(2) _cell_angle_beta 90.476(2) _cell_angle_gamma 90.654(2) _cell_volume 5097.4(11) _cell_formula_units_Z 2 _cell_measurement_temperature 302(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2416 _exptl_absorpt_coefficient_mu 1.582 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 302(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22359 _diffrn_reflns_av_R_equivalents 0.0270 _diffrn_reflns_av_sigmaI/netI 0.0389 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 23.28 _reflns_number_total 14602 _reflns_number_gt 10897 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0921P)^2^+4.9275P] 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 14602 _refine_ls_number_parameters 1261 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0687 _refine_ls_R_factor_gt 0.0483 _refine_ls_wR_factor_ref 0.1493 _refine_ls_wR_factor_gt 0.1353 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 1.08453(5) 0.67981(3) 0.27552(3) 0.03445(16) Uani 1 1 d . . . Cu2 Cu 0.99150(5) 0.82731(3) 0.29804(3) 0.03599(16) Uani 1 1 d . . . Cu3 Cu 0.98406(5) 0.74487(3) 0.15639(3) 0.03680(17) Uani 1 1 d . . . Cu4 Cu 0.85676(5) 0.62051(3) 0.30561(3) 0.03328(16) Uani 1 1 d . . . Cu5 Cu 0.76424(5) 0.76842(3) 0.32430(3) 0.03563(16) Uani 1 1 d . . . Cu6 Cu 0.75809(5) 0.68201(3) 0.18472(3) 0.03543(16) Uani 1 1 d . . . Cl1 Cl 1.16435(16) 0.77481(8) 0.54036(7) 0.0666(4) Uani 1 1 d . . . Cl2 Cl 0.87563(18) 1.01200(8) 0.13009(8) 0.0764(5) Uani 1 1 d . . . Cl3 Cl 1.12505(15) 0.48336(7) 0.05784(8) 0.0646(4) Uani 1 1 d . . . Cl4 Cl 0.85250(16) 0.70743(8) 0.57641(7) 0.0682(4) Uani 1 1 d . . . Cl5 Cl 0.5802(2) 0.93447(8) 0.15419(9) 0.0900(6) Uani 1 1 d . . . Cl6 Cl 0.83921(17) 0.41159(7) 0.09453(8) 0.0728(5) Uani 1 1 d . . . Cl7 Cl 0.1692(4) -0.03667(19) 0.0490(2) 0.215(2) Uani 1 1 d . . . Cl8 Cl 0.2579(3) 0.0831(2) 0.01903(17) 0.1614(13) Uani 1 1 d . . . Cl9 Cl 0.3236(4) 0.7815(3) 0.1512(3) 0.249(3) Uani 1 1 d . . . Cl10 Cl 0.3118(5) 0.8821(4) 0.2536(3) 0.338(4) Uani 1 1 d . . . P1 P 0.46032(14) 0.17206(7) 0.21165(8) 0.0552(4) Uani 1 1 d . . . P2 P 0.52931(15) 0.30751(7) 0.27300(8) 0.0560(4) Uani 1 1 d . . . O1 O 1.0406(3) 0.75478(15) 0.24104(15) 0.0374(8) Uani 1 1 d . . . O2 O 0.7752(3) 0.68689(15) 0.27363(15) 0.0347(7) Uani 1 1 d . . . N1 N 1.1088(4) 0.73192(19) 0.35862(19) 0.0395(10) Uani 1 1 d . . . N2 N 1.0617(4) 0.7915(2) 0.3695(2) 0.0417(10) Uani 1 1 d . . . N3 N 0.9571(4) 0.87280(19) 0.2256(2) 0.0410(10) Uani 1 1 d . . . N4 N 0.9548(4) 0.83918(19) 0.16655(19) 0.0413(10) Uani 1 1 d . . . N5 N 1.0488(4) 0.6568(2) 0.14023(19) 0.0411(10) Uani 1 1 d . . . N6 N 1.0883(4) 0.63031(19) 0.19060(19) 0.0409(10) Uani 1 1 d . . . N7 N 0.8381(3) 0.6661(2) 0.39238(18) 0.0386(10) Uani 1 1 d . . . N8 N 0.8000(4) 0.72813(19) 0.40008(19) 0.0384(10) Uani 1 1 d . . . N9 N 0.6974(4) 0.8061(2) 0.2530(2) 0.0438(11) Uani 1 1 d . . . N10 N 0.6960(4) 0.7705(2) 0.1949(2) 0.0440(11) Uani 1 1 d . . . N11 N 0.7887(4) 0.58857(19) 0.17513(19) 0.0408(10) Uani 1 1 d . . . N12 N 0.8312(4) 0.5623(2) 0.2255(2) 0.0413(10) Uani 1 1 d . . . N13 N 1.0946(3) 0.59736(18) 0.31481(18) 0.0358(9) Uani 1 1 d . . . N14 N 0.9938(3) 0.57061(18) 0.33017(19) 0.0352(9) Uani 1 1 d . . . N15 N 0.8947(4) 0.88676(19) 0.36000(18) 0.0374(10) Uani 1 1 d . . . N16 N 0.7917(4) 0.85892(19) 0.37056(19) 0.0404(10) Uani 1 1 d . . . N17 N 0.8801(4) 0.7216(2) 0.07980(19) 0.0409(10) Uani 1 1 d . . . N18 N 0.7822(3) 0.68900(19) 0.09258(18) 0.0372(10) Uani 1 1 d . . . N19 N 0.4656(5) 0.2470(2) 0.2355(3) 0.0730(16) Uani 1 1 d . . . C1 C 1.0726(5) 0.8141(3) 0.4313(2) 0.0470(13) Uani 1 1 d . . . H1 H 1.0463 0.8540 0.4511 0.056 Uiso 1 1 calc R . . C2 C 1.1288(5) 0.7689(3) 0.4606(2) 0.0440(13) Uani 1 1 d . . . C3 C 1.1501(5) 0.7179(3) 0.4141(2) 0.0478(14) Uani 1 1 d . . . H3 H 1.1871 0.6797 0.4201 0.057 Uiso 1 1 calc R . . C4 C 0.9258(5) 0.8803(3) 0.1265(3) 0.0529(15) Uani 1 1 d . . . H4 H 0.9170 0.8695 0.0828 0.064 Uiso 1 1 calc R . . C5 C 0.9112(5) 0.9409(3) 0.1600(3) 0.0498(14) Uani 1 1 d . . . C6 C 0.9311(5) 0.9348(3) 0.2222(3) 0.0507(14) Uani 1 1 d . . . H6 H 0.9272 0.9680 0.2563 0.061 Uiso 1 1 calc R . . C7 C 1.1188(5) 0.5693(3) 0.1701(3) 0.0490(14) Uani 1 1 d . . . H7 H 1.1483 0.5401 0.1954 0.059 Uiso 1 1 calc R . . C8 C 1.0998(5) 0.5562(3) 0.1061(3) 0.0463(13) Uani 1 1 d . . . C9 C 1.0555(5) 0.6119(3) 0.0881(3) 0.0488(14) Uani 1 1 d . . . H9 H 1.0338 0.6178 0.0471 0.059 Uiso 1 1 calc R . . C10 C 0.8001(5) 0.7504(3) 0.4617(2) 0.0478(14) Uani 1 1 d . . . H10 H 0.7774 0.7917 0.4795 0.057 Uiso 1 1 calc R . . C11 C 0.8387(5) 0.7028(3) 0.4947(2) 0.0437(13) Uani 1 1 d . . . C12 C 0.8614(5) 0.6506(3) 0.4502(3) 0.0470(13) Uani 1 1 d . . . H12 H 0.8886 0.6107 0.4587 0.056 Uiso 1 1 calc R . . C13 C 0.6571(5) 0.8082(3) 0.1534(3) 0.0545(15) Uani 1 1 d . . . H13 H 0.6486 0.7957 0.1099 0.065 Uiso 1 1 calc R . . C14 C 0.6319(5) 0.8684(3) 0.1855(3) 0.0539(15) Uani 1 1 d . . . C15 C 0.6598(5) 0.8654(3) 0.2476(3) 0.0542(15) Uani 1 1 d . . . H15 H 0.6535 0.8994 0.2808 0.065 Uiso 1 1 calc R . . C16 C 0.8539(5) 0.4999(3) 0.2058(3) 0.0474(13) Uani 1 1 d . . . H16 H 0.8843 0.4707 0.2308 0.057 Uiso 1 1 calc R . . C17 C 0.8249(5) 0.4855(2) 0.1422(2) 0.0442(13) Uani 1 1 d . . . C18 C 0.7854(5) 0.5416(3) 0.1250(3) 0.0472(13) Uani 1 1 d . . . H18 H 0.7597 0.5469 0.0846 0.057 Uiso 1 1 calc R . . C19 C 1.0167(4) 0.5194(2) 0.3614(2) 0.0404(12) Uani 1 1 d . . . C20 C 1.1360(5) 0.5132(3) 0.3649(3) 0.0485(14) Uani 1 1 d . . . H20 H 1.1761 0.4821 0.3835 0.058 Uiso 1 1 calc R . . C21 C 1.1822(4) 0.5628(2) 0.3353(2) 0.0376(12) Uani 1 1 d . . . C22 C 1.3033(4) 0.5827(3) 0.3304(3) 0.0445(13) Uani 1 1 d . . . C23 C 1.3394(5) 0.6262(3) 0.2896(3) 0.0583(16) Uani 1 1 d . . . H23 H 1.2860 0.6420 0.2631 0.070 Uiso 1 1 calc R . . C24 C 1.4516(5) 0.6461(3) 0.2879(4) 0.0709(19) Uani 1 1 d . . . H24 H 1.4732 0.6756 0.2608 0.085 Uiso 1 1 calc R . . C25 C 1.5321(6) 0.6225(4) 0.3261(4) 0.076(2) Uani 1 1 d . . . H25 H 1.6082 0.6360 0.3252 0.091 Uiso 1 1 calc R . . C26 C 1.4991(6) 0.5792(4) 0.3650(4) 0.073(2) Uani 1 1 d . . . H26 H 1.5536 0.5626 0.3903 0.088 Uiso 1 1 calc R . . C27 C 1.3848(5) 0.5593(3) 0.3677(3) 0.0583(16) Uani 1 1 d . . . H27 H 1.3638 0.5300 0.3951 0.070 Uiso 1 1 calc R . . C28 C 0.9267(5) 0.4833(2) 0.3907(3) 0.0436(13) Uani 1 1 d . . . C29 C 0.9566(6) 0.4441(3) 0.4358(3) 0.0643(17) Uani 1 1 d . . . H29 H 1.0338 0.4396 0.4454 0.077 Uiso 1 1 calc R . . C30 C 0.8767(6) 0.4119(3) 0.4666(3) 0.076(2) Uani 1 1 d . . . H30 H 0.9000 0.3848 0.4955 0.092 Uiso 1 1 calc R . . C31 C 0.7628(6) 0.4194(3) 0.4552(3) 0.0730(19) Uani 1 1 d . . . H31 H 0.7082 0.3990 0.4775 0.088 Uiso 1 1 calc R . . C32 C 0.7294(5) 0.4576(3) 0.4101(3) 0.0661(18) Uani 1 1 d . . . H32 H 0.6520 0.4622 0.4013 0.079 Uiso 1 1 calc R . . C33 C 0.8107(5) 0.4890(3) 0.3782(3) 0.0553(15) Uani 1 1 d . . . H33 H 0.7873 0.5143 0.3478 0.066 Uiso 1 1 calc R . . C34 C 0.7342(4) 0.8997(2) 0.4141(2) 0.0404(12) Uani 1 1 d . . . C35 C 0.8023(5) 0.9547(2) 0.4321(2) 0.0438(13) Uani 1 1 d . . . H35 H 0.7849 0.9905 0.4618 0.053 Uiso 1 1 calc R . . C36 C 0.9021(4) 0.9453(2) 0.3968(2) 0.0387(12) Uani 1 1 d . . . C37 C 1.0010(5) 0.9895(3) 0.3969(2) 0.0440(13) Uani 1 1 d . . . C38 C 1.1082(5) 0.9686(3) 0.3757(3) 0.0585(16) Uani 1 1 d . . . H38 H 1.1192 0.9248 0.3610 0.070 Uiso 1 1 calc R . . C39 C 1.1999(6) 1.0128(4) 0.3762(3) 0.0727(19) Uani 1 1 d . . . H39 H 1.2711 0.9982 0.3614 0.087 Uiso 1 1 calc R . . C40 C 1.1852(6) 1.0775(3) 0.3984(3) 0.0708(19) Uani 1 1 d . . . H40 H 1.2466 1.1067 0.3994 0.085 Uiso 1 1 calc R . . C41 C 1.0799(6) 1.0987(3) 0.4190(3) 0.0683(18) Uani 1 1 d . . . H41 H 1.0693 1.1426 0.4334 0.082 Uiso 1 1 calc R . . C42 C 0.9891(6) 1.0555(3) 0.4186(3) 0.0569(15) Uani 1 1 d . . . H42 H 0.9183 1.0709 0.4332 0.068 Uiso 1 1 calc R . . C43 C 0.6158(5) 0.8861(3) 0.4335(3) 0.0472(13) Uani 1 1 d . . . C44 C 0.5718(6) 0.9205(3) 0.4877(3) 0.076(2) Uani 1 1 d . . . H44 H 0.6182 0.9506 0.5129 0.091 Uiso 1 1 calc R . . C45 C 0.4600(7) 0.9110(4) 0.5054(4) 0.096(3) Uani 1 1 d . . . H45 H 0.4327 0.9347 0.5424 0.115 Uiso 1 1 calc R . . C46 C 0.3897(7) 0.8684(4) 0.4701(4) 0.091(2) Uani 1 1 d . . . H46 H 0.3138 0.8633 0.4817 0.109 Uiso 1 1 calc R . . C47 C 0.4319(6) 0.8327(4) 0.4169(4) 0.086(2) Uani 1 1 d . . . H47 H 0.3851 0.8019 0.3929 0.104 Uiso 1 1 calc R . . C48 C 0.5428(5) 0.8416(3) 0.3982(3) 0.0647(17) Uani 1 1 d . . . H48 H 0.5693 0.8173 0.3613 0.078 Uiso 1 1 calc R . . C49 C 0.7210(5) 0.6751(2) 0.0384(2) 0.0432(13) Uani 1 1 d . . . C50 C 0.7812(5) 0.6979(3) -0.0101(2) 0.0498(14) Uani 1 1 d . . . H50 H 0.7593 0.6944 -0.0526 0.060 Uiso 1 1 calc R . . C51 C 0.8797(5) 0.7268(3) 0.0170(3) 0.0451(13) Uani 1 1 d . . . C52 C 0.9726(5) 0.7593(3) -0.0125(3) 0.0519(14) Uani 1 1 d . . . C53 C 1.0839(6) 0.7599(3) 0.0096(3) 0.0687(18) Uani 1 1 d . . . H53 H 1.1014 0.7389 0.0443 0.082 Uiso 1 1 calc R . . C54 C 1.1716(7) 0.7920(4) -0.0195(4) 0.094(3) Uani 1 1 d . . . H54 H 1.2464 0.7923 -0.0041 0.113 Uiso 1 1 calc R . . C55 C 1.1461(9) 0.8228(4) -0.0709(4) 0.097(3) Uani 1 1 d . . . H55 H 1.2038 0.8435 -0.0908 0.117 Uiso 1 1 calc R . . C56 C 1.0379(8) 0.8230(4) -0.0922(4) 0.094(3) Uani 1 1 d . . . H56 H 1.0205 0.8448 -0.1264 0.113 Uiso 1 1 calc R . . C57 C 0.9524(7) 0.7912(3) -0.0644(3) 0.0746(19) Uani 1 1 d . . . H57 H 0.8784 0.7912 -0.0809 0.089 Uiso 1 1 calc R . . C58 C 0.6065(5) 0.6434(3) 0.0359(3) 0.0495(14) Uani 1 1 d . . . C59 C 0.5673(7) 0.6077(4) -0.0193(3) 0.093(3) Uani 1 1 d . . . H59 H 0.6151 0.6017 -0.0543 0.111 Uiso 1 1 calc R . . C60 C 0.4592(7) 0.5806(5) -0.0241(4) 0.121(4) Uani 1 1 d . . . H60 H 0.4347 0.5570 -0.0623 0.145 Uiso 1 1 calc R . . C61 C 0.3875(7) 0.5878(5) 0.0264(4) 0.097(3) Uani 1 1 d . . . H61 H 0.3142 0.5695 0.0229 0.116 Uiso 1 1 calc R . . C62 C 0.4248(6) 0.6226(4) 0.0827(3) 0.0719(19) Uani 1 1 d . . . H62 H 0.3770 0.6273 0.1177 0.086 Uiso 1 1 calc R . . C63 C 0.5327(5) 0.6506(3) 0.0873(3) 0.0567(15) Uani 1 1 d . . . H63 H 0.5567 0.6746 0.1254 0.068 Uiso 1 1 calc R . . C64 C 0.3160(5) 0.1442(3) 0.2215(3) 0.0596(16) Uani 1 1 d . . . C65 C 0.2419(7) 0.1828(4) 0.2592(4) 0.082(2) Uani 1 1 d . . . H65 H 0.2649 0.2241 0.2782 0.099 Uiso 1 1 calc R . . C66 C 0.1331(8) 0.1599(5) 0.2688(5) 0.101(3) Uani 1 1 d . . . H66 H 0.0832 0.1866 0.2941 0.122 Uiso 1 1 calc R . . C67 C 0.0968(8) 0.1007(6) 0.2429(5) 0.104(3) Uani 1 1 d . . . H67 H 0.0226 0.0867 0.2499 0.125 Uiso 1 1 calc R . . C68 C 0.1690(8) 0.0613(5) 0.2064(4) 0.106(3) Uani 1 1 d . . . H68 H 0.1446 0.0198 0.1890 0.127 Uiso 1 1 calc R . . C69 C 0.2794(7) 0.0823(4) 0.1946(4) 0.087(2) Uani 1 1 d . . . H69 H 0.3282 0.0552 0.1689 0.105 Uiso 1 1 calc R . . C70 C 0.5541(6) 0.1231(3) 0.2533(3) 0.0612(17) Uani 1 1 d . . . C71 C 0.6710(6) 0.1342(4) 0.2501(4) 0.082(2) Uani 1 1 d . . . H71 H 0.7000 0.1648 0.2261 0.099 Uiso 1 1 calc R . . C72 C 0.7447(8) 0.0983(5) 0.2838(5) 0.107(3) Uani 1 1 d . . . H72 H 0.8235 0.1052 0.2827 0.128 Uiso 1 1 calc R . . C73 C 0.7001(10) 0.0527(5) 0.3188(4) 0.107(3) Uani 1 1 d . . . H73 H 0.7494 0.0294 0.3415 0.128 Uiso 1 1 calc R . . C74 C 0.5880(10) 0.0415(4) 0.3205(4) 0.103(3) Uani 1 1 d . . . H74 H 0.5595 0.0098 0.3434 0.124 Uiso 1 1 calc R . . C75 C 0.5133(7) 0.0770(3) 0.2880(3) 0.077(2) Uani 1 1 d . . . H75 H 0.4348 0.0694 0.2899 0.092 Uiso 1 1 calc R . . C76 C 0.4955(5) 0.1565(3) 0.1292(3) 0.0591(16) Uani 1 1 d . . . C77 C 0.4765(6) 0.2043(4) 0.0908(4) 0.081(2) Uani 1 1 d . . . H77 H 0.4480 0.2445 0.1084 0.098 Uiso 1 1 calc R . . C78 C 0.4993(8) 0.1931(6) 0.0269(5) 0.113(3) Uani 1 1 d . . . H78 H 0.4853 0.2253 0.0015 0.135 Uiso 1 1 calc R . . C79 C 0.5428(8) 0.1343(7) 0.0007(4) 0.109(3) Uani 1 1 d . . . H79 H 0.5584 0.1267 -0.0425 0.131 Uiso 1 1 calc R . . C80 C 0.5635(7) 0.0864(5) 0.0382(4) 0.098(3) Uani 1 1 d . . . H80 H 0.5928 0.0466 0.0204 0.117 Uiso 1 1 calc R . . C81 C 0.5405(6) 0.0979(4) 0.1026(4) 0.076(2) Uani 1 1 d . . . H81 H 0.5556 0.0658 0.1279 0.091 Uiso 1 1 calc R . . C82 C 0.4820(6) 0.3780(3) 0.2399(3) 0.0574(16) Uani 1 1 d . . . C83 C 0.5544(7) 0.4304(3) 0.2352(3) 0.0713(19) Uani 1 1 d . . . H83 H 0.6290 0.4309 0.2509 0.086 Uiso 1 1 calc R . . C84 C 0.5143(9) 0.4824(4) 0.2067(4) 0.092(3) Uani 1 1 d . . . H84 H 0.5627 0.5175 0.2026 0.110 Uiso 1 1 calc R . . C85 C 0.4048(10) 0.4819(4) 0.1850(4) 0.095(3) Uani 1 1 d . . . H85 H 0.3787 0.5169 0.1661 0.114 Uiso 1 1 calc R . . C86 C 0.3333(8) 0.4317(4) 0.1905(4) 0.095(3) Uani 1 1 d . . . H86 H 0.2579 0.4330 0.1763 0.114 Uiso 1 1 calc R . . C87 C 0.3700(6) 0.3784(3) 0.2169(3) 0.076(2) Uani 1 1 d . . . H87 H 0.3208 0.3432 0.2194 0.092 Uiso 1 1 calc R . . C88 C 0.4924(5) 0.3169(3) 0.3551(3) 0.0579(15) Uani 1 1 d . . . C89 C 0.4537(6) 0.3746(3) 0.3865(4) 0.0721(19) Uani 1 1 d . . . H89 H 0.4439 0.4100 0.3647 0.087 Uiso 1 1 calc R . . C90 C 0.4291(7) 0.3804(4) 0.4506(4) 0.087(2) Uani 1 1 d . . . H90 H 0.4038 0.4199 0.4716 0.105 Uiso 1 1 calc R . . C91 C 0.4415(7) 0.3291(5) 0.4828(4) 0.096(3) Uani 1 1 d . . . H91 H 0.4253 0.3334 0.5259 0.116 Uiso 1 1 calc R . . C92 C 0.4779(8) 0.2710(5) 0.4519(4) 0.099(3) Uani 1 1 d . . . H92 H 0.4862 0.2354 0.4738 0.119 Uiso 1 1 calc R . . C93 C 0.5023(7) 0.2652(4) 0.3885(4) 0.085(2) Uani 1 1 d . . . H93 H 0.5261 0.2252 0.3677 0.102 Uiso 1 1 calc R . . C94 C 0.6824(6) 0.3052(3) 0.2679(3) 0.0588(16) Uani 1 1 d . . . C95 C 0.7325(7) 0.3034(4) 0.2095(4) 0.082(2) Uani 1 1 d . . . H95 H 0.6862 0.3041 0.1738 0.098 Uiso 1 1 calc R . . C96 C 0.8505(8) 0.3008(4) 0.2025(4) 0.100(3) Uani 1 1 d . . . H96 H 0.8833 0.2995 0.1627 0.120 Uiso 1 1 calc R . . C97 C 0.9183(8) 0.3001(5) 0.2558(5) 0.105(3) Uani 1 1 d . . . H97 H 0.9975 0.2995 0.2517 0.126 Uiso 1 1 calc R . . C98 C 0.8719(7) 0.3002(4) 0.3134(4) 0.096(3) Uani 1 1 d . . . H98 H 0.9188 0.2982 0.3486 0.115 Uiso 1 1 calc R . . C99 C 0.7535(6) 0.3035(3) 0.3204(3) 0.0725(19) Uani 1 1 d . . . H99 H 0.7217 0.3046 0.3604 0.087 Uiso 1 1 calc R . . C100 C 0.1398(10) 0.0442(5) 0.0377(5) 0.134(4) Uani 1 1 d . . . H10A H 0.0833 0.0439 0.0040 0.161 Uiso 1 1 calc R . . H10B H 0.1078 0.0672 0.0762 0.161 Uiso 1 1 calc R . . C101 C 0.2779(15) 0.8322(10) 0.2018(11) 0.46(3) Uani 1 1 d . . . H10C H 0.2293 0.8568 0.1769 0.552 Uiso 1 1 calc R . . H10D H 0.2249 0.8063 0.2231 0.552 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0368(3) 0.0342(3) 0.0337(3) 0.0093(3) 0.0002(3) 0.0011(3) Cu2 0.0425(4) 0.0346(3) 0.0318(3) 0.0077(3) 0.0000(3) 0.0022(3) Cu3 0.0440(4) 0.0351(3) 0.0323(3) 0.0082(3) -0.0028(3) -0.0003(3) Cu4 0.0318(3) 0.0363(3) 0.0330(3) 0.0094(3) -0.0023(2) 0.0017(2) Cu5 0.0423(4) 0.0335(3) 0.0318(3) 0.0071(3) -0.0007(3) 0.0004(3) Cu6 0.0421(4) 0.0354(3) 0.0298(3) 0.0083(3) -0.0028(3) -0.0001(3) Cl1 0.0928(12) 0.0720(10) 0.0365(8) 0.0138(7) -0.0149(8) 0.0022(9) Cl2 0.1177(15) 0.0482(9) 0.0682(11) 0.0251(8) -0.0129(10) 0.0120(9) Cl3 0.0773(11) 0.0522(8) 0.0595(10) -0.0094(7) -0.0008(8) 0.0122(8) Cl4 0.0908(12) 0.0807(11) 0.0340(8) 0.0114(7) -0.0078(8) 0.0075(9) Cl5 0.1436(18) 0.0550(10) 0.0748(12) 0.0202(9) -0.0294(12) 0.0309(11) Cl6 0.1124(14) 0.0438(8) 0.0590(10) -0.0044(7) -0.0033(9) 0.0074(8) Cl7 0.232(4) 0.147(3) 0.248(5) -0.041(3) 0.126(4) -0.029(3) Cl8 0.108(2) 0.216(4) 0.156(3) 0.017(3) -0.0022(19) -0.013(2) Cl9 0.207(4) 0.257(5) 0.255(6) -0.067(4) 0.085(4) -0.046(4) Cl10 0.237(6) 0.369(8) 0.345(8) -0.176(7) 0.104(5) -0.076(6) P1 0.0630(10) 0.0445(8) 0.0587(10) 0.0092(7) -0.0119(8) 0.0064(7) P2 0.0679(10) 0.0446(8) 0.0560(10) 0.0087(7) -0.0128(8) 0.0063(7) O1 0.042(2) 0.0357(18) 0.0356(19) 0.0103(15) -0.0025(15) 0.0007(15) O2 0.0396(19) 0.0336(17) 0.0313(18) 0.0063(14) -0.0017(14) 0.0016(14) N1 0.046(3) 0.039(2) 0.035(2) 0.0094(19) -0.0027(19) 0.0018(19) N2 0.049(3) 0.038(2) 0.038(3) 0.0061(19) 0.000(2) 0.005(2) N3 0.049(3) 0.037(2) 0.038(3) 0.011(2) 0.001(2) 0.0044(19) N4 0.053(3) 0.038(2) 0.034(2) 0.010(2) -0.005(2) 0.000(2) N5 0.048(3) 0.042(2) 0.034(2) 0.008(2) -0.002(2) 0.004(2) N6 0.049(3) 0.039(2) 0.036(2) 0.0061(19) -0.002(2) 0.003(2) N7 0.042(2) 0.044(2) 0.030(2) 0.0062(19) -0.0060(18) 0.0038(19) N8 0.047(3) 0.040(2) 0.030(2) 0.0094(19) -0.0021(19) -0.0001(19) N9 0.054(3) 0.038(2) 0.040(3) 0.007(2) -0.006(2) 0.004(2) N10 0.057(3) 0.039(2) 0.037(3) 0.009(2) -0.005(2) 0.005(2) N11 0.050(3) 0.038(2) 0.034(2) 0.005(2) -0.003(2) 0.001(2) N12 0.044(3) 0.041(2) 0.040(3) 0.008(2) -0.005(2) 0.0020(19) N13 0.038(2) 0.036(2) 0.035(2) 0.0089(18) -0.0012(18) -0.0022(19) N14 0.032(2) 0.038(2) 0.038(2) 0.0101(19) -0.0013(18) 0.0038(18) N15 0.044(3) 0.038(2) 0.032(2) 0.0099(19) 0.0001(19) 0.0002(19) N16 0.048(3) 0.039(2) 0.035(2) 0.0076(19) -0.002(2) 0.000(2) N17 0.046(3) 0.043(2) 0.035(2) 0.0098(19) -0.0038(19) -0.002(2) N18 0.042(2) 0.040(2) 0.030(2) 0.0079(18) -0.0014(19) -0.0016(19) N19 0.084(4) 0.047(3) 0.087(4) 0.007(3) -0.031(3) 0.012(3) C1 0.062(4) 0.045(3) 0.035(3) 0.007(2) -0.002(3) 0.005(3) C2 0.054(3) 0.049(3) 0.030(3) 0.010(2) -0.004(2) -0.006(3) C3 0.058(4) 0.047(3) 0.041(3) 0.014(3) -0.004(3) 0.008(3) C4 0.072(4) 0.049(3) 0.039(3) 0.014(3) -0.015(3) 0.000(3) C5 0.065(4) 0.041(3) 0.046(3) 0.018(3) -0.008(3) -0.002(3) C6 0.063(4) 0.037(3) 0.053(4) 0.010(3) 0.000(3) 0.004(3) C7 0.057(4) 0.044(3) 0.046(3) 0.007(3) -0.003(3) 0.015(3) C8 0.046(3) 0.044(3) 0.048(3) 0.004(3) 0.003(3) 0.000(2) C9 0.055(4) 0.050(3) 0.040(3) 0.002(3) -0.004(3) 0.007(3) C10 0.061(4) 0.048(3) 0.033(3) 0.003(3) -0.002(3) 0.003(3) C11 0.049(3) 0.053(3) 0.030(3) 0.010(3) -0.006(2) 0.001(3) C12 0.056(3) 0.044(3) 0.044(3) 0.014(3) -0.007(3) 0.004(3) C13 0.074(4) 0.052(3) 0.038(3) 0.008(3) -0.012(3) 0.009(3) C14 0.069(4) 0.044(3) 0.050(4) 0.012(3) -0.008(3) 0.007(3) C15 0.076(4) 0.041(3) 0.046(4) 0.008(3) -0.007(3) 0.016(3) C16 0.056(3) 0.038(3) 0.050(3) 0.011(3) -0.006(3) 0.004(3) C17 0.053(3) 0.037(3) 0.042(3) 0.001(2) 0.003(3) 0.000(2) C18 0.060(4) 0.047(3) 0.035(3) 0.005(3) -0.004(3) 0.000(3) C19 0.039(3) 0.039(3) 0.044(3) 0.010(2) -0.003(2) 0.001(2) C20 0.045(3) 0.048(3) 0.057(4) 0.022(3) -0.004(3) 0.012(3) C21 0.037(3) 0.040(3) 0.037(3) 0.008(2) -0.001(2) 0.004(2) C22 0.036(3) 0.048(3) 0.049(3) 0.004(3) 0.003(2) 0.004(2) C23 0.044(4) 0.067(4) 0.067(4) 0.018(3) 0.000(3) -0.001(3) C24 0.051(4) 0.070(4) 0.092(5) 0.013(4) 0.017(4) -0.008(3) C25 0.043(4) 0.079(5) 0.101(6) 0.000(4) 0.000(4) -0.005(3) C26 0.049(4) 0.082(5) 0.088(5) 0.005(4) -0.015(4) 0.010(4) C27 0.048(4) 0.062(4) 0.067(4) 0.014(3) -0.005(3) 0.006(3) C28 0.046(3) 0.037(3) 0.049(3) 0.012(2) -0.003(3) 0.000(2) C29 0.062(4) 0.066(4) 0.070(4) 0.031(3) -0.015(3) -0.011(3) C30 0.084(5) 0.086(5) 0.069(5) 0.046(4) -0.009(4) -0.027(4) C31 0.076(5) 0.068(4) 0.077(5) 0.021(4) 0.015(4) -0.022(4) C32 0.049(4) 0.061(4) 0.091(5) 0.021(4) 0.005(3) -0.006(3) C33 0.044(3) 0.049(3) 0.077(4) 0.025(3) -0.003(3) 0.000(3) C34 0.046(3) 0.041(3) 0.036(3) 0.010(2) 0.002(2) 0.005(2) C35 0.051(3) 0.040(3) 0.040(3) 0.002(2) 0.002(3) 0.006(2) C36 0.051(3) 0.033(3) 0.032(3) 0.005(2) -0.006(2) 0.005(2) C37 0.050(3) 0.044(3) 0.038(3) 0.007(2) -0.004(2) -0.004(3) C38 0.062(4) 0.048(3) 0.066(4) 0.009(3) 0.002(3) -0.007(3) C39 0.058(4) 0.083(5) 0.078(5) 0.016(4) 0.003(3) -0.017(4) C40 0.075(5) 0.070(5) 0.068(4) 0.014(4) -0.006(4) -0.033(4) C41 0.087(5) 0.047(4) 0.069(4) 0.001(3) -0.005(4) -0.014(4) C42 0.070(4) 0.046(3) 0.053(4) 0.001(3) -0.002(3) -0.009(3) C43 0.048(3) 0.046(3) 0.051(3) 0.017(3) 0.003(3) 0.008(3) C44 0.063(4) 0.084(5) 0.075(5) -0.014(4) 0.019(4) -0.006(4) C45 0.078(6) 0.111(6) 0.090(6) -0.012(5) 0.034(5) 0.000(5) C46 0.061(5) 0.108(6) 0.104(7) 0.017(5) 0.028(5) -0.007(5) C47 0.065(5) 0.100(6) 0.092(6) 0.009(5) 0.003(4) -0.025(4) C48 0.054(4) 0.077(4) 0.059(4) -0.003(3) 0.009(3) -0.011(3) C49 0.051(3) 0.045(3) 0.034(3) 0.006(2) -0.006(2) -0.001(2) C50 0.059(4) 0.063(4) 0.028(3) 0.009(3) -0.010(3) -0.004(3) C51 0.052(3) 0.044(3) 0.042(3) 0.012(2) 0.003(3) 0.003(3) C52 0.058(4) 0.050(3) 0.048(3) 0.009(3) 0.012(3) 0.000(3) C53 0.068(5) 0.084(5) 0.054(4) 0.014(3) 0.006(3) -0.021(4) C54 0.068(5) 0.118(7) 0.095(6) 0.010(5) 0.008(4) -0.034(5) C55 0.109(7) 0.103(6) 0.082(6) 0.025(5) 0.025(5) -0.039(5) C56 0.115(7) 0.094(6) 0.081(6) 0.040(5) 0.010(5) -0.021(5) C57 0.083(5) 0.084(5) 0.063(4) 0.032(4) 0.006(4) -0.006(4) C58 0.052(3) 0.056(3) 0.041(3) 0.010(3) -0.009(3) -0.003(3) C59 0.075(5) 0.137(7) 0.056(4) -0.018(5) 0.004(4) -0.031(5) C60 0.080(6) 0.193(10) 0.075(6) -0.029(6) -0.004(5) -0.065(6) C61 0.060(5) 0.138(7) 0.086(6) -0.004(5) -0.003(4) -0.037(5) C62 0.062(4) 0.097(5) 0.059(4) 0.019(4) 0.005(3) -0.015(4) C63 0.055(4) 0.069(4) 0.047(4) 0.011(3) 0.000(3) -0.011(3) C64 0.063(4) 0.057(4) 0.058(4) 0.008(3) -0.008(3) 0.005(3) C65 0.091(6) 0.074(5) 0.086(6) 0.023(4) 0.004(4) 0.017(4) C66 0.088(7) 0.113(7) 0.110(7) 0.035(6) 0.021(5) 0.030(6) C67 0.079(6) 0.147(9) 0.090(7) 0.027(6) 0.002(5) -0.007(6) C68 0.105(7) 0.123(8) 0.086(6) 0.004(6) -0.003(5) -0.045(6) C69 0.073(5) 0.102(6) 0.082(5) -0.001(5) -0.002(4) -0.021(4) C70 0.078(5) 0.048(3) 0.058(4) 0.007(3) -0.011(3) 0.016(3) C71 0.070(5) 0.079(5) 0.102(6) 0.022(4) -0.016(4) 0.024(4) C72 0.087(6) 0.110(7) 0.124(8) 0.017(6) -0.019(5) 0.045(5) C73 0.142(9) 0.105(7) 0.075(6) 0.015(5) -0.021(6) 0.065(7) C74 0.150(9) 0.087(6) 0.080(6) 0.034(5) 0.000(6) 0.044(6) C75 0.103(6) 0.067(4) 0.064(4) 0.019(4) -0.005(4) 0.017(4) C76 0.056(4) 0.062(4) 0.060(4) 0.014(3) -0.010(3) -0.007(3) C77 0.078(5) 0.091(5) 0.080(6) 0.032(4) -0.017(4) 0.005(4) C78 0.087(6) 0.185(11) 0.079(7) 0.068(7) -0.021(5) -0.019(7) C79 0.082(6) 0.177(11) 0.066(6) 0.011(7) 0.000(5) -0.025(7) C80 0.080(6) 0.119(7) 0.086(6) -0.015(6) 0.020(5) -0.017(5) C81 0.071(5) 0.075(5) 0.078(5) 0.000(4) 0.006(4) -0.001(4) C82 0.079(5) 0.043(3) 0.050(4) 0.004(3) -0.004(3) 0.011(3) C83 0.085(5) 0.058(4) 0.073(5) 0.015(3) 0.012(4) 0.014(4) C84 0.135(8) 0.054(4) 0.091(6) 0.020(4) 0.047(6) 0.019(5) C85 0.150(9) 0.071(5) 0.073(5) 0.031(4) 0.024(6) 0.057(6) C86 0.113(7) 0.079(5) 0.095(6) 0.014(5) -0.026(5) 0.037(5) C87 0.084(5) 0.057(4) 0.088(5) 0.010(4) -0.016(4) 0.015(4) C88 0.057(4) 0.062(4) 0.055(4) 0.009(3) -0.003(3) -0.003(3) C89 0.066(4) 0.067(4) 0.083(5) 0.009(4) 0.004(4) -0.006(3) C90 0.097(6) 0.092(6) 0.070(5) -0.001(5) 0.019(4) -0.004(5) C91 0.085(6) 0.138(8) 0.068(5) 0.020(6) 0.008(4) -0.034(6) C92 0.123(8) 0.107(7) 0.073(6) 0.035(5) 0.002(5) -0.010(6) C93 0.106(6) 0.082(5) 0.071(5) 0.027(4) 0.000(4) 0.010(4) C94 0.073(4) 0.055(4) 0.050(4) 0.012(3) -0.006(3) 0.012(3) C95 0.089(6) 0.087(5) 0.073(5) 0.022(4) -0.005(4) 0.026(4) C96 0.111(7) 0.101(6) 0.093(7) 0.031(5) 0.037(6) 0.040(5) C97 0.079(6) 0.126(8) 0.120(8) 0.052(6) 0.013(6) 0.032(5) C98 0.068(5) 0.124(7) 0.102(7) 0.040(6) -0.011(5) 0.015(5) C99 0.071(5) 0.083(5) 0.063(4) 0.011(4) -0.005(4) 0.008(4) C100 0.163(11) 0.133(9) 0.098(7) -0.005(6) -0.003(7) -0.039(8) C101 0.237(19) 0.45(3) 0.55(4) -0.43(3) 0.28(2) -0.24(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 O1 1.882(3) . ? Cu1 N6 1.952(4) . ? Cu1 N1 1.957(4) . ? Cu1 N13 2.008(4) . ? Cu1 Cu4 3.0262(9) . ? Cu2 O1 1.893(3) . ? Cu2 N3 1.956(4) . ? Cu2 N2 1.961(4) . ? Cu2 N15 2.034(4) . ? Cu2 Cu5 2.9960(9) . ? Cu3 O1 1.897(3) . ? Cu3 N4 1.970(4) . ? Cu3 N5 1.971(4) . ? Cu3 N17 2.024(4) . ? Cu3 Cu6 3.0299(9) . ? Cu4 O2 1.882(3) . ? Cu4 N12 1.966(4) . ? Cu4 N7 1.969(4) . ? Cu4 N14 2.018(4) . ? Cu5 O2 1.880(3) . ? Cu5 N9 1.960(4) . ? Cu5 N8 1.961(4) . ? Cu5 N16 2.015(4) . ? Cu6 O2 1.890(3) . ? Cu6 N11 1.956(4) . ? Cu6 N10 1.964(4) . ? Cu6 N18 2.008(4) . ? Cl1 C2 1.732(5) . ? Cl2 C5 1.736(5) . ? Cl3 C8 1.734(5) . ? Cl4 C11 1.735(5) . ? Cl5 C14 1.717(5) . ? Cl6 C17 1.727(5) . ? Cl7 C100 1.762(11) . ? Cl8 C100 1.668(11) . ? Cl9 C101 1.502(12) . ? Cl10 C101 1.452(13) . ? P1 N19 1.566(5) . ? P1 C76 1.792(7) . ? P1 C64 1.798(7) . ? P1 C70 1.809(6) . ? P2 N19 1.566(5) . ? P2 C88 1.788(6) . ? P2 C94 1.792(7) . ? P2 C82 1.798(6) . ? N1 C3 1.342(6) . ? N1 N2 1.348(6) . ? N2 C1 1.339(6) . ? N3 C6 1.335(6) . ? N3 N4 1.351(6) . ? N4 C4 1.330(6) . ? N5 C9 1.349(6) . ? N5 N6 1.350(6) . ? N6 C7 1.332(6) . ? N7 C12 1.341(6) . ? N7 N8 1.354(6) . ? N8 C10 1.328(6) . ? N9 C15 1.330(7) . ? N9 N10 1.348(6) . ? N10 C13 1.338(7) . ? N11 C18 1.340(6) . ? N11 N12 1.360(6) . ? N12 C16 1.334(6) . ? N13 N14 1.356(5) . ? N13 C21 1.359(6) . ? N14 C19 1.357(6) . ? N15 C36 1.352(6) . ? N15 N16 1.361(6) . ? N16 C34 1.353(6) . ? N17 C51 1.356(6) . ? N17 N18 1.369(6) . ? N18 C49 1.346(6) . ? C1 C2 1.365(7) . ? C2 C3 1.370(7) . ? C4 C5 1.370(8) . ? C5 C6 1.367(8) . ? C7 C8 1.368(8) . ? C8 C9 1.371(7) . ? C10 C11 1.366(7) . ? C11 C12 1.364(7) . ? C13 C14 1.373(8) . ? C14 C15 1.369(8) . ? C16 C17 1.384(7) . ? C17 C18 1.352(7) . ? C19 C20 1.402(7) . ? C19 C28 1.473(7) . ? C20 C21 1.384(7) . ? C21 C22 1.476(7) . ? C22 C27 1.370(8) . ? C22 C23 1.400(8) . ? C23 C24 1.370(8) . ? C24 C25 1.375(10) . ? C25 C26 1.358(10) . ? C26 C27 1.396(9) . ? C28 C29 1.387(8) . ? C28 C33 1.387(7) . ? C29 C30 1.364(9) . ? C30 C31 1.364(10) . ? C31 C32 1.383(9) . ? C32 C33 1.379(8) . ? C34 C35 1.390(7) . ? C34 C43 1.481(8) . ? C35 C36 1.392(7) . ? C36 C37 1.465(7) . ? C37 C38 1.387(8) . ? C37 C42 1.390(7) . ? C38 C39 1.399(9) . ? C39 C40 1.371(9) . ? C40 C41 1.365(9) . ? C41 C42 1.378(9) . ? C43 C44 1.376(8) . ? C43 C48 1.385(8) . ? C44 C45 1.380(10) . ? C45 C46 1.345(11) . ? C46 C47 1.362(11) . ? C47 C48 1.375(9) . ? C49 C50 1.387(7) . ? C49 C58 1.481(8) . ? C50 C51 1.376(7) . ? C51 C52 1.461(8) . ? C52 C53 1.376(9) . ? C52 C57 1.385(8) . ? C53 C54 1.409(9) . ? C54 C55 1.372(11) . ? C55 C56 1.338(11) . ? C56 C57 1.372(10) . ? C58 C59 1.372(8) . ? C58 C63 1.390(8) . ? C59 C60 1.372(10) . ? C60 C61 1.361(11) . ? C61 C62 1.374(10) . ? C62 C63 1.377(8) . ? C64 C65 1.372(9) . ? C64 C69 1.392(9) . ? C65 C66 1.377(11) . ? C66 C67 1.335(12) . ? C67 C68 1.353(12) . ? C68 C69 1.391(11) . ? C70 C75 1.370(9) . ? C70 C71 1.385(10) . ? C71 C72 1.400(10) . ? C72 C73 1.382(13) . ? C73 C74 1.328(13) . ? C74 C75 1.387(10) . ? C76 C81 1.379(9) . ? C76 C77 1.388(9) . ? C77 C78 1.376(12) . ? C78 C79 1.373(13) . ? C79 C80 1.378(13) . ? C80 C81 1.386(11) . ? C82 C83 1.384(9) . ? C82 C87 1.391(9) . ? C83 C84 1.391(10) . ? C84 C85 1.354(12) . ? C85 C86 1.345(12) . ? C86 C87 1.378(10) . ? C88 C89 1.368(9) . ? C88 C93 1.372(9) . ? C89 C90 1.386(10) . ? C90 C91 1.351(11) . ? C91 C92 1.364(12) . ? C92 C93 1.370(11) . ? C94 C95 1.375(9) . ? C94 C99 1.390(9) . ? C95 C96 1.387(11) . ? C96 C97 1.379(12) . ? C97 C98 1.345(11) . ? C98 C99 1.392(10) . ? 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 O1 Cu1 N6 90.30(15) . . ? O1 Cu1 N1 90.42(15) . . ? N6 Cu1 N1 170.15(18) . . ? O1 Cu1 N13 167.52(16) . . ? N6 Cu1 N13 90.87(16) . . ? N1 Cu1 N13 90.56(16) . . ? O1 Cu1 Cu4 102.72(10) . . ? N6 Cu1 Cu4 92.94(13) . . ? N1 Cu1 Cu4 96.48(13) . . ? N13 Cu1 Cu4 64.81(11) . . ? O1 Cu2 N3 89.22(15) . . ? O1 Cu2 N2 90.73(15) . . ? N3 Cu2 N2 166.41(18) . . ? O1 Cu2 N15 161.93(16) . . ? N3 Cu2 N15 94.61(16) . . ? N2 Cu2 N15 89.63(16) . . ? O1 Cu2 Cu5 95.26(10) . . ? N3 Cu2 Cu5 102.73(13) . . ? N2 Cu2 Cu5 90.81(13) . . ? N15 Cu2 Cu5 66.67(12) . . ? O1 Cu3 N4 89.07(15) . . ? O1 Cu3 N5 90.42(15) . . ? N4 Cu3 N5 166.69(19) . . ? O1 Cu3 N17 161.27(16) . . ? N4 Cu3 N17 95.78(17) . . ? N5 Cu3 N17 88.93(17) . . ? O1 Cu3 Cu6 95.61(10) . . ? N4 Cu3 Cu6 105.33(13) . . ? N5 Cu3 Cu6 87.96(13) . . ? N17 Cu3 Cu6 65.67(12) . . ? O2 Cu4 N12 90.41(15) . . ? O2 Cu4 N7 89.80(15) . . ? N12 Cu4 N7 162.39(18) . . ? O2 Cu4 N14 158.00(15) . . ? N12 Cu4 N14 93.40(16) . . ? N7 Cu4 N14 92.97(16) . . ? O2 Cu4 Cu1 91.85(10) . . ? N12 Cu4 Cu1 98.91(13) . . ? N7 Cu4 Cu1 98.68(12) . . ? N14 Cu4 Cu1 66.15(11) . . ? O2 Cu5 N9 90.64(15) . . ? O2 Cu5 N8 90.18(15) . . ? N9 Cu5 N8 168.86(19) . . ? O2 Cu5 N16 165.83(16) . . ? N9 Cu5 N16 89.55(17) . . ? N8 Cu5 N16 92.36(16) . . ? O2 Cu5 Cu2 100.17(10) . . ? N9 Cu5 Cu2 89.36(13) . . ? N8 Cu5 Cu2 101.43(12) . . ? N16 Cu5 Cu2 65.67(12) . . ? O2 Cu6 N11 90.02(15) . . ? O2 Cu6 N10 90.37(15) . . ? N11 Cu6 N10 168.85(19) . . ? O2 Cu6 N18 164.26(15) . . ? N11 Cu6 N18 94.23(17) . . ? N10 Cu6 N18 88.37(17) . . ? O2 Cu6 Cu3 98.67(10) . . ? N11 Cu6 Cu3 104.88(13) . . ? N10 Cu6 Cu3 86.07(13) . . ? N18 Cu6 Cu3 65.59(12) . . ? N19 P1 C76 110.3(3) . . ? N19 P1 C64 107.8(3) . . ? C76 P1 C64 108.7(3) . . ? N19 P1 C70 115.1(3) . . ? C76 P1 C70 107.3(3) . . ? C64 P1 C70 107.4(3) . . ? N19 P2 C88 110.7(3) . . ? N19 P2 C94 114.6(3) . . ? C88 P2 C94 107.9(3) . . ? N19 P2 C82 106.9(3) . . ? C88 P2 C82 108.7(3) . . ? C94 P2 C82 107.8(3) . . ? Cu1 O1 Cu2 117.59(17) . . ? Cu1 O1 Cu3 118.57(17) . . ? Cu2 O1 Cu3 118.22(16) . . ? Cu5 O2 Cu4 118.59(16) . . ? Cu5 O2 Cu6 119.04(16) . . ? Cu4 O2 Cu6 118.13(16) . . ? C3 N1 N2 107.6(4) . . ? C3 N1 Cu1 133.0(4) . . ? N2 N1 Cu1 118.5(3) . . ? C1 N2 N1 108.8(4) . . ? C1 N2 Cu2 132.7(4) . . ? N1 N2 Cu2 118.5(3) . . ? C6 N3 N4 108.9(4) . . ? C6 N3 Cu2 131.6(4) . . ? N4 N3 Cu2 119.5(3) . . ? C4 N4 N3 107.8(4) . . ? C4 N4 Cu3 133.7(4) . . ? N3 N4 Cu3 118.4(3) . . ? C9 N5 N6 108.7(4) . . ? C9 N5 Cu3 133.5(4) . . ? N6 N5 Cu3 117.6(3) . . ? C7 N6 N5 107.8(4) . . ? C7 N6 Cu1 131.8(4) . . ? N5 N6 Cu1 120.3(3) . . ? C12 N7 N8 107.4(4) . . ? C12 N7 Cu4 133.8(4) . . ? N8 N7 Cu4 118.6(3) . . ? C10 N8 N7 108.5(4) . . ? C10 N8 Cu5 132.9(4) . . ? N7 N8 Cu5 118.5(3) . . ? C15 N9 N10 108.4(4) . . ? C15 N9 Cu5 132.3(4) . . ? N10 N9 Cu5 118.9(3) . . ? C13 N10 N9 108.1(4) . . ? C13 N10 Cu6 132.7(4) . . ? N9 N10 Cu6 119.0(3) . . ? C18 N11 N12 107.9(4) . . ? C18 N11 Cu6 132.7(4) . . ? N12 N11 Cu6 119.1(3) . . ? C16 N12 N11 107.9(4) . . ? C16 N12 Cu4 134.0(4) . . ? N11 N12 Cu4 118.0(3) . . ? N14 N13 C21 109.0(4) . . ? N14 N13 Cu1 116.4(3) . . ? C21 N13 Cu1 134.4(3) . . ? N13 N14 C19 108.5(4) . . ? N13 N14 Cu4 112.6(3) . . ? C19 N14 Cu4 138.7(3) . . ? C36 N15 N16 108.3(4) . . ? C36 N15 Cu2 139.7(4) . . ? N16 N15 Cu2 112.0(3) . . ? C34 N16 N15 108.8(4) . . ? C34 N16 Cu5 135.4(4) . . ? N15 N16 Cu5 115.7(3) . . ? C51 N17 N18 108.0(4) . . ? C51 N17 Cu3 138.5(4) . . ? N18 N17 Cu3 113.5(3) . . ? C49 N18 N17 108.4(4) . . ? C49 N18 Cu6 136.4(4) . . ? N17 N18 Cu6 114.9(3) . . ? P1 N19 P2 149.8(4) . . ? N2 C1 C2 108.6(5) . . ? C1 C2 C3 106.0(5) . . ? C1 C2 Cl1 126.8(4) . . ? C3 C2 Cl1 127.2(4) . . ? N1 C3 C2 109.1(5) . . ? N4 C4 C5 109.0(5) . . ? C6 C5 C4 106.2(5) . . ? C6 C5 Cl2 126.4(4) . . ? C4 C5 Cl2 127.4(4) . . ? N3 C6 C5 108.1(5) . . ? N6 C7 C8 109.4(5) . . ? C7 C8 C9 106.2(5) . . ? C7 C8 Cl3 126.7(4) . . ? C9 C8 Cl3 127.1(4) . . ? N5 C9 C8 107.9(5) . . ? N8 C10 C11 109.1(5) . . ? C12 C11 C10 105.7(5) . . ? C12 C11 Cl4 127.4(4) . . ? C10 C11 Cl4 126.9(4) . . ? N7 C12 C11 109.2(5) . . ? N10 C13 C14 108.8(5) . . ? C15 C14 C13 105.6(5) . . ? C15 C14 Cl5 127.1(5) . . ? C13 C14 Cl5 127.3(5) . . ? N9 C15 C14 109.1(5) . . ? N12 C16 C17 108.9(5) . . ? C18 C17 C16 105.7(5) . . ? C18 C17 Cl6 127.3(4) . . ? C16 C17 Cl6 127.0(4) . . ? N11 C18 C17 109.6(5) . . ? N14 C19 C20 108.1(4) . . ? N14 C19 C28 122.8(4) . . ? C20 C19 C28 128.9(5) . . ? C21 C20 C19 106.2(4) . . ? N13 C21 C20 108.2(4) . . ? N13 C21 C22 122.3(4) . . ? C20 C21 C22 129.2(5) . . ? C27 C22 C23 117.5(5) . . ? C27 C22 C21 119.8(5) . . ? C23 C22 C21 122.7(5) . . ? C24 C23 C22 121.6(6) . . ? C23 C24 C25 120.0(7) . . ? C26 C25 C24 119.3(6) . . ? C25 C26 C27 121.2(6) . . ? C22 C27 C26 120.4(6) . . ? C29 C28 C33 116.9(5) . . ? C29 C28 C19 119.6(5) . . ? C33 C28 C19 123.4(5) . . ? C30 C29 C28 122.2(6) . . ? C29 C30 C31 120.3(6) . . ? C30 C31 C32 119.3(6) . . ? C33 C32 C31 120.1(6) . . ? C32 C33 C28 121.2(6) . . ? N16 C34 C35 108.3(5) . . ? N16 C34 C43 122.8(5) . . ? C35 C34 C43 128.8(5) . . ? C34 C35 C36 106.0(5) . . ? N15 C36 C35 108.6(5) . . ? N15 C36 C37 123.3(5) . . ? C35 C36 C37 128.1(5) . . ? C38 C37 C42 117.3(5) . . ? C38 C37 C36 122.8(5) . . ? C42 C37 C36 119.8(5) . . ? C37 C38 C39 120.8(6) . . ? C40 C39 C38 120.3(7) . . ? C41 C40 C39 119.5(6) . . ? C40 C41 C42 120.6(6) . . ? C41 C42 C37 121.6(6) . . ? C44 C43 C48 116.8(6) . . ? C44 C43 C34 119.8(5) . . ? C48 C43 C34 123.4(5) . . ? C43 C44 C45 121.1(7) . . ? C46 C45 C44 121.4(7) . . ? C45 C46 C47 118.6(7) . . ? C46 C47 C48 121.0(7) . . ? C47 C48 C43 121.1(6) . . ? N18 C49 C50 108.6(5) . . ? N18 C49 C58 122.6(5) . . ? C50 C49 C58 128.7(5) . . ? C51 C50 C49 106.3(5) . . ? N17 C51 C50 108.7(5) . . ? N17 C51 C52 122.1(5) . . ? C50 C51 C52 129.2(5) . . ? C53 C52 C57 116.7(6) . . ? C53 C52 C51 122.2(5) . . ? C57 C52 C51 121.1(6) . . ? C52 C53 C54 121.0(7) . . ? C55 C54 C53 119.6(8) . . ? C56 C55 C54 119.8(7) . . ? C55 C56 C57 120.8(8) . . ? C56 C57 C52 122.2(7) . . ? C59 C58 C63 117.4(6) . . ? C59 C58 C49 120.2(6) . . ? C63 C58 C49 122.4(5) . . ? C58 C59 C60 121.5(7) . . ? C61 C60 C59 120.8(7) . . ? C60 C61 C62 119.1(7) . . ? C61 C62 C63 120.2(7) . . ? C62 C63 C58 121.0(6) . . ? C65 C64 C69 118.8(7) . . ? C65 C64 P1 119.8(6) . . ? C69 C64 P1 121.2(6) . . ? C64 C65 C66 119.4(8) . . ? C67 C66 C65 122.3(9) . . ? C66 C67 C68 119.4(9) . . ? C67 C68 C69 120.8(9) . . ? C64 C69 C68 119.3(8) . . ? C75 C70 C71 119.9(6) . . ? C75 C70 P1 122.4(6) . . ? C71 C70 P1 117.7(5) . . ? C70 C71 C72 118.5(8) . . ? C73 C72 C71 119.9(9) . . ? C74 C73 C72 121.1(8) . . ? C73 C74 C75 120.0(9) . . ? C70 C75 C74 120.6(8) . . ? C81 C76 C77 118.8(7) . . ? C81 C76 P1 121.7(5) . . ? C77 C76 P1 119.5(6) . . ? C78 C77 C76 120.8(8) . . ? C79 C78 C77 119.9(9) . . ? C78 C79 C80 120.1(9) . . ? C79 C80 C81 119.9(9) . . ? C76 C81 C80 120.4(8) . . ? C83 C82 C87 119.7(6) . . ? C83 C82 P2 121.9(5) . . ? C87 C82 P2 118.4(5) . . ? C82 C83 C84 119.3(7) . . ? C85 C84 C83 120.0(8) . . ? C86 C85 C84 121.1(7) . . ? C85 C86 C87 121.0(8) . . ? C86 C87 C82 118.9(8) . . ? C89 C88 C93 118.0(7) . . ? C89 C88 P2 122.2(5) . . ? C93 C88 P2 119.8(5) . . ? C88 C89 C90 120.4(7) . . ? C91 C90 C89 120.6(8) . . ? C90 C91 C92 119.7(8) . . ? C91 C92 C93 119.8(8) . . ? C92 C93 C88 121.5(8) . . ? C95 C94 C99 118.1(7) . . ? C95 C94 P2 119.0(5) . . ? C99 C94 P2 122.9(5) . . ? C94 C95 C96 121.5(7) . . ? C97 C96 C95 118.7(8) . . ? C98 C97 C96 121.3(8) . . ? C97 C98 C99 119.9(8) . . ? C94 C99 C98 120.5(7) . . ? Cl8 C100 Cl7 111.4(7) . . ? Cl10 C101 Cl9 143.4(14) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.281 _refine_diff_density_min -1.262 _refine_diff_density_rms 0.079 #===END data_PPN[6] _database_code_depnum_ccdc_archive 'CCDC 617270' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C105 H86 Cl13 Cu6 N19 O3 P2' _chemical_formula_weight 2565.96 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 19.588(2) _cell_length_b 20.268(2) _cell_length_c 27.541(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 10934(2) _cell_formula_units_Z 4 _cell_measurement_temperature 299(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description polyhedron _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.559 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5192 _exptl_absorpt_coefficient_mu 1.553 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 299(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48230 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_sigmaI/netI 0.0749 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 23.28 _reflns_number_total 15738 _reflns_number_gt 11239 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0513P)^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 0.002(11) _refine_ls_number_reflns 15738 _refine_ls_number_parameters 1335 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0723 _refine_ls_R_factor_gt 0.0392 _refine_ls_wR_factor_ref 0.1012 _refine_ls_wR_factor_gt 0.0796 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.979 _refine_ls_shift/su_max 0.003 _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 0.62157(4) 0.94441(4) 0.94036(3) 0.0304(2) Uani 1 1 d . . . Cu2 Cu 0.45897(4) 0.94447(4) 0.94159(3) 0.03169(19) Uani 1 1 d . . . Cu3 Cu 0.54234(4) 1.04882(4) 0.87268(3) 0.0331(2) Uani 1 1 d . . . Cu4 Cu 0.61353(4) 0.85879(4) 0.84946(3) 0.0303(2) Uani 1 1 d . . . Cu5 Cu 0.44649(4) 0.85573(4) 0.85368(3) 0.0323(2) Uani 1 1 d . . . Cu6 Cu 0.52076(4) 0.96064(4) 0.78489(3) 0.0343(2) Uani 1 1 d . . . P1 P 0.48602(10) 0.22472(10) 0.17182(7) 0.0465(5) Uani 1 1 d . . . P2 P 0.53704(11) 0.14742(10) 0.08787(6) 0.0453(5) Uani 1 1 d . . . Cl1 Cl 0.54132(11) 0.77555(10) 1.09947(7) 0.0586(5) Uani 1 1 d . . . Cl2 Cl 0.25787(11) 1.09679(14) 0.83804(10) 0.0918(9) Uani 1 1 d . . . Cl3 Cl 0.82447(10) 1.06966(12) 0.82034(9) 0.0709(7) Uani 1 1 d . . . Cl4 Cl 0.53884(11) 0.66106(9) 0.99074(7) 0.0587(5) Uani 1 1 d . . . Cl5 Cl 0.23171(11) 0.96711(14) 0.73749(9) 0.0855(8) Uani 1 1 d . . . Cl6 Cl 0.79262(11) 0.97347(13) 0.70531(9) 0.0809(8) Uani 1 1 d . . . Cl7 Cl 0.87820(10) 0.79876(12) 0.94224(9) 0.0701(7) Uani 1 1 d . . . Cl8 Cl 0.21170(10) 0.78686(11) 0.97678(8) 0.0580(6) Uani 1 1 d . . . Cl9 Cl 0.48606(11) 1.23466(10) 0.71693(7) 0.0617(6) Uani 1 1 d . . . Cl10 Cl 0.6607(2) 0.7560(2) 0.67782(15) 0.1656(17) Uani 1 1 d . . . Cl11 Cl 0.6185(2) 0.87139(19) 0.62989(14) 0.1519(15) Uani 1 1 d . . . Cl12 Cl 0.4286(3) 0.5011(4) 0.0774(2) 0.295(4) Uani 1 1 d . . . Cl13 Cl 0.4453(4) 0.4214(3) -0.0028(2) 0.271(3) Uani 1 1 d . . . O1 O 0.5399(2) 0.99027(19) 0.92589(14) 0.0327(10) Uani 1 1 d . . . O2 O 0.5278(2) 0.88460(19) 0.82374(14) 0.0303(10) Uani 1 1 d . . . O3 O 0.6524(7) 0.4671(6) 0.0549(4) 0.179(5) Uani 1 1 d . . . N1 N 0.5752(3) 0.8964(3) 0.99262(19) 0.0348(15) Uani 1 1 d . . . N2 N 0.5059(3) 0.8975(3) 0.99350(18) 0.0328(14) Uani 1 1 d . . . N3 N 0.4080(3) 1.0033(3) 0.8978(2) 0.0339(15) Uani 1 1 d . . . N4 N 0.4428(3) 1.0506(3) 0.87308(19) 0.0403(15) Uani 1 1 d . . . N5 N 0.6412(3) 1.0524(3) 0.87307(19) 0.0379(15) Uani 1 1 d . . . N6 N 0.6747(3) 1.0052(3) 0.8987(2) 0.0346(14) Uani 1 1 d . . . N7 N 0.5687(3) 0.7961(3) 0.89278(18) 0.0301(14) Uani 1 1 d . . . N8 N 0.4991(3) 0.7969(3) 0.89536(19) 0.0339(14) Uani 1 1 d . . . N9 N 0.3920(3) 0.8985(3) 0.8030(2) 0.0411(15) Uani 1 1 d . . . N10 N 0.4213(3) 0.9469(3) 0.7766(2) 0.0388(15) Uani 1 1 d . . . N11 N 0.6196(3) 0.9560(3) 0.7734(2) 0.0352(14) Uani 1 1 d . . . N12 N 0.6575(3) 0.9089(3) 0.7969(2) 0.0372(15) Uani 1 1 d . . . N13 N 0.6994(3) 0.8802(3) 0.93400(19) 0.0310(14) Uani 1 1 d . . . N14 N 0.6996(3) 0.8469(3) 0.89037(19) 0.0316(13) Uani 1 1 d . . . N15 N 0.3757(2) 0.8836(3) 0.94190(19) 0.0327(13) Uani 1 1 d . . . N16 N 0.3681(3) 0.8465(3) 0.90112(19) 0.0334(14) Uani 1 1 d . . . N17 N 0.5387(3) 1.0974(3) 0.80748(19) 0.0384(14) Uani 1 1 d . . . N18 N 0.5193(2) 1.0593(3) 0.76915(18) 0.0340(13) Uani 1 1 d . . . N19 N 0.5352(3) 0.1988(3) 0.13086(19) 0.0500(16) Uani 1 1 d . . . C1 C 0.4861(3) 0.8569(3) 1.0292(2) 0.0374(18) Uani 1 1 d . . . H1 H 0.4410 0.8479 1.0375 0.045 Uiso 1 1 calc R . . C2 C 0.5417(4) 0.8306(3) 1.0514(2) 0.0377(17) Uani 1 1 d . . . C3 C 0.5972(4) 0.8560(4) 1.0278(2) 0.0408(19) Uani 1 1 d . . . H3 H 0.6426 0.8467 1.0350 0.049 Uiso 1 1 calc R . . C4 C 0.3973(4) 1.0881(4) 0.8501(3) 0.050(2) Uani 1 1 d . . . H4 H 0.4078 1.1243 0.8308 0.059 Uiso 1 1 calc R . . C5 C 0.3330(4) 1.0656(4) 0.8592(3) 0.047(2) Uani 1 1 d . . . C6 C 0.3421(4) 1.0114(4) 0.8892(3) 0.046(2) Uani 1 1 d . . . H6 H 0.3074 0.9848 0.9014 0.055 Uiso 1 1 calc R . . C7 C 0.7403(4) 1.0061(4) 0.8850(3) 0.045(2) Uani 1 1 d . . . H7 H 0.7744 0.9785 0.8969 0.054 Uiso 1 1 calc R . . C8 C 0.7491(4) 1.0540(4) 0.8505(3) 0.051(2) Uani 1 1 d . . . C9 C 0.6857(4) 1.0821(4) 0.8436(3) 0.049(2) Uani 1 1 d . . . H9 H 0.6757 1.1160 0.8221 0.059 Uiso 1 1 calc R . . C10 C 0.4799(4) 0.7508(3) 0.9275(2) 0.0380(18) Uani 1 1 d . . . H10 H 0.4351 0.7404 0.9356 0.046 Uiso 1 1 calc R . . C11 C 0.5373(4) 0.7215(3) 0.9464(2) 0.0384(16) Uani 1 1 d . . . C12 C 0.5910(3) 0.7512(4) 0.9242(2) 0.0376(19) Uani 1 1 d . . . H12 H 0.6366 0.7416 0.9302 0.045 Uiso 1 1 calc R . . C13 C 0.3718(4) 0.9760(4) 0.7501(3) 0.062(3) Uani 1 1 d . . . H13 H 0.3782 1.0107 0.7285 0.074 Uiso 1 1 calc R . . C14 C 0.3107(4) 0.9463(4) 0.7600(3) 0.047(2) Uani 1 1 d . . . C15 C 0.3244(4) 0.8994(4) 0.7934(3) 0.051(2) Uani 1 1 d . . . H15 H 0.2921 0.8719 0.8077 0.062 Uiso 1 1 calc R . . C16 C 0.7206(4) 0.9095(4) 0.7778(2) 0.050(2) Uani 1 1 d . . . H16 H 0.7564 0.8825 0.7876 0.060 Uiso 1 1 calc R . . C17 C 0.7244(4) 0.9552(4) 0.7422(3) 0.045(2) Uani 1 1 d . . . C18 C 0.6599(4) 0.9848(4) 0.7409(2) 0.043(2) Uani 1 1 d . . . H18 H 0.6472 1.0192 0.7205 0.052 Uiso 1 1 calc R . . C19 C 0.7595(3) 0.8130(3) 0.8874(2) 0.0340(17) Uani 1 1 d . . . C20 C 0.7979(3) 0.8272(3) 0.9284(3) 0.0386(19) Uani 1 1 d . . . C21 C 0.7585(3) 0.8685(3) 0.9568(2) 0.0343(17) Uani 1 1 d . . . C22 C 0.7745(3) 0.9008(4) 1.0040(2) 0.0384(18) Uani 1 1 d . . . C23 C 0.7516(4) 0.9643(4) 1.0145(3) 0.050(2) Uani 1 1 d . . . H23 H 0.7248 0.9867 0.9920 0.060 Uiso 1 1 calc R . . C24 C 0.7684(4) 0.9951(4) 1.0587(3) 0.062(2) Uani 1 1 d . . . H24 H 0.7519 1.0372 1.0653 0.075 Uiso 1 1 calc R . . C25 C 0.8089(5) 0.9637(5) 1.0919(3) 0.071(3) Uani 1 1 d . . . H25 H 0.8209 0.9846 1.1208 0.085 Uiso 1 1 calc R . . C26 C 0.8312(6) 0.9016(5) 1.0824(3) 0.086(3) Uani 1 1 d . . . H26 H 0.8583 0.8798 1.1050 0.103 Uiso 1 1 calc R . . C27 C 0.8142(5) 0.8703(4) 1.0391(3) 0.063(3) Uani 1 1 d . . . H27 H 0.8299 0.8276 1.0335 0.075 Uiso 1 1 calc R . . C28 C 0.7745(3) 0.7696(3) 0.8464(3) 0.0379(18) Uani 1 1 d . . . C29 C 0.8411(4) 0.7592(4) 0.8296(3) 0.059(2) Uani 1 1 d . . . H29 H 0.8773 0.7816 0.8439 0.071 Uiso 1 1 calc R . . C30 C 0.8537(5) 0.7154(5) 0.7913(3) 0.082(3) Uani 1 1 d . . . H30 H 0.8983 0.7091 0.7808 0.098 Uiso 1 1 calc R . . C31 C 0.8036(6) 0.6825(5) 0.7693(3) 0.080(3) Uani 1 1 d . . . H31 H 0.8131 0.6533 0.7442 0.096 Uiso 1 1 calc R . . C32 C 0.7380(5) 0.6924(4) 0.7845(3) 0.067(3) Uani 1 1 d . . . H32 H 0.7028 0.6698 0.7691 0.080 Uiso 1 1 calc R . . C33 C 0.7228(4) 0.7343(4) 0.8213(3) 0.048(2) Uani 1 1 d . . . H33 H 0.6774 0.7401 0.8304 0.058 Uiso 1 1 calc R . . C34 C 0.3121(3) 0.8073(4) 0.9050(3) 0.0349(18) Uani 1 1 d . . . C35 C 0.2844(3) 0.8219(3) 0.9509(3) 0.0360(18) Uani 1 1 d . . . C36 C 0.3239(3) 0.8689(3) 0.9726(2) 0.0334(17) Uani 1 1 d . . . C37 C 0.3132(3) 0.9059(4) 1.0195(3) 0.0405(19) Uani 1 1 d . . . C38 C 0.2947(4) 0.8737(4) 1.0622(3) 0.055(2) Uani 1 1 d . . . H38 H 0.2908 0.8280 1.0623 0.067 Uiso 1 1 calc R . . C39 C 0.2820(5) 0.9086(6) 1.1044(3) 0.072(3) Uani 1 1 d . . . H39 H 0.2696 0.8862 1.1325 0.087 Uiso 1 1 calc R . . C40 C 0.2874(5) 0.9747(6) 1.1050(3) 0.077(3) Uani 1 1 d . . . H40 H 0.2780 0.9981 1.1333 0.092 Uiso 1 1 calc R . . C41 C 0.3068(4) 1.0070(5) 1.0641(4) 0.072(3) Uani 1 1 d . . . H41 H 0.3116 1.0526 1.0650 0.086 Uiso 1 1 calc R . . C42 C 0.3199(4) 0.9736(4) 1.0206(3) 0.057(2) Uani 1 1 d . . . H42 H 0.3329 0.9967 0.9929 0.068 Uiso 1 1 calc R . . C43 C 0.2909(4) 0.7613(3) 0.8665(2) 0.0392(19) Uani 1 1 d . . . C44 C 0.3386(4) 0.7320(4) 0.8361(3) 0.047(2) Uani 1 1 d . . . H44 H 0.3848 0.7402 0.8408 0.057 Uiso 1 1 calc R . . C45 C 0.3182(5) 0.6910(4) 0.7992(3) 0.065(3) Uani 1 1 d . . . H45 H 0.3505 0.6737 0.7780 0.078 Uiso 1 1 calc R . . C46 C 0.2498(5) 0.6753(4) 0.7931(3) 0.074(3) Uani 1 1 d . . . H46 H 0.2362 0.6461 0.7689 0.089 Uiso 1 1 calc R . . C47 C 0.2023(5) 0.7038(5) 0.8236(3) 0.070(3) Uani 1 1 d . . . H47 H 0.1562 0.6943 0.8197 0.084 Uiso 1 1 calc R . . C48 C 0.2229(4) 0.7460(4) 0.8595(3) 0.055(2) Uani 1 1 d . . . H48 H 0.1902 0.7648 0.8797 0.066 Uiso 1 1 calc R . . C49 C 0.4994(3) 1.0992(4) 0.7331(2) 0.0410(19) Uani 1 1 d . . . C50 C 0.5066(3) 1.1633(4) 0.7485(3) 0.0392(18) Uani 1 1 d . . . C51 C 0.5323(4) 1.1612(3) 0.7959(2) 0.0382(17) Uani 1 1 d . . . C52 C 0.5518(4) 1.2156(4) 0.8287(3) 0.047(2) Uani 1 1 d . . . C53 C 0.5789(4) 1.2738(4) 0.8107(3) 0.061(2) Uani 1 1 d . . . H53 H 0.5864 1.2774 0.7774 0.074 Uiso 1 1 calc R . . C54 C 0.5950(5) 1.3258(5) 0.8394(4) 0.072(3) Uani 1 1 d . . . H54 H 0.6118 1.3645 0.8257 0.086 Uiso 1 1 calc R . . C55 C 0.5866(5) 1.3212(5) 0.8888(4) 0.082(3) Uani 1 1 d . . . H55 H 0.5975 1.3566 0.9089 0.098 Uiso 1 1 calc R . . C56 C 0.5616(4) 1.2634(5) 0.9079(3) 0.072(3) Uani 1 1 d . . . H56 H 0.5569 1.2594 0.9413 0.087 Uiso 1 1 calc R . . C57 C 0.5435(4) 1.2114(4) 0.8785(3) 0.058(2) Uani 1 1 d . . . H57 H 0.5255 1.1732 0.8922 0.070 Uiso 1 1 calc R . . C58 C 0.4778(4) 1.0732(4) 0.6866(3) 0.0426(19) Uani 1 1 d . . . C59 C 0.5036(4) 1.0167(4) 0.6671(3) 0.057(2) Uani 1 1 d . . . H59 H 0.5384 0.9950 0.6836 0.068 Uiso 1 1 calc R . . C60 C 0.4806(5) 0.9902(4) 0.6241(3) 0.072(3) Uani 1 1 d . . . H60 H 0.4995 0.9517 0.6116 0.087 Uiso 1 1 calc R . . C61 C 0.4289(6) 1.0222(6) 0.6004(4) 0.090(3) Uani 1 1 d . . . H61 H 0.4126 1.0048 0.5713 0.108 Uiso 1 1 calc R . . C62 C 0.4009(5) 1.0786(5) 0.6179(4) 0.081(3) Uani 1 1 d . . . H62 H 0.3655 1.0994 0.6015 0.097 Uiso 1 1 calc R . . C63 C 0.4258(4) 1.1042(4) 0.6605(3) 0.059(2) Uani 1 1 d . . . H63 H 0.4075 1.1434 0.6723 0.071 Uiso 1 1 calc R . . C64 C 0.5289(4) 0.0634(4) 0.1078(2) 0.051(2) Uani 1 1 d . . . C65 C 0.5836(5) 0.0218(5) 0.1103(3) 0.064(2) Uani 1 1 d . . . H65 H 0.6259 0.0356 0.0988 0.076 Uiso 1 1 calc R . . C66 C 0.5768(6) -0.0404(5) 0.1299(3) 0.083(3) Uani 1 1 d . . . H66 H 0.6142 -0.0688 0.1307 0.099 Uiso 1 1 calc R . . C67 C 0.5160(7) -0.0604(5) 0.1478(4) 0.089(4) Uani 1 1 d . . . H67 H 0.5121 -0.1024 0.1612 0.107 Uiso 1 1 calc R . . C68 C 0.4609(6) -0.0207(6) 0.1466(4) 0.093(3) Uani 1 1 d . . . H68 H 0.4196 -0.0350 0.1595 0.112 Uiso 1 1 calc R . . C69 C 0.4660(5) 0.0418(5) 0.1259(3) 0.077(3) Uani 1 1 d . . . H69 H 0.4279 0.0690 0.1242 0.093 Uiso 1 1 calc R . . C70 C 0.4744(4) 0.1645(4) 0.0419(2) 0.0445(19) Uani 1 1 d . . . C71 C 0.4614(5) 0.2291(4) 0.0299(3) 0.058(2) Uani 1 1 d . . . H71 H 0.4816 0.2629 0.0476 0.070 Uiso 1 1 calc R . . C72 C 0.4187(5) 0.2443(5) -0.0085(3) 0.072(3) Uani 1 1 d . . . H72 H 0.4103 0.2882 -0.0164 0.086 Uiso 1 1 calc R . . C73 C 0.3889(5) 0.1955(5) -0.0345(3) 0.071(3) Uani 1 1 d . . . H73 H 0.3603 0.2060 -0.0603 0.085 Uiso 1 1 calc R . . C74 C 0.4007(5) 0.1306(5) -0.0230(3) 0.068(3) Uani 1 1 d . . . H74 H 0.3803 0.0973 -0.0412 0.082 Uiso 1 1 calc R . . C75 C 0.4429(4) 0.1146(4) 0.0157(3) 0.057(2) Uani 1 1 d . . . H75 H 0.4501 0.0707 0.0240 0.069 Uiso 1 1 calc R . . C76 C 0.6186(4) 0.1553(4) 0.0591(3) 0.052(2) Uani 1 1 d . . . C77 C 0.6721(4) 0.1850(4) 0.0827(3) 0.062(2) Uani 1 1 d . . . H77 H 0.6663 0.2013 0.1140 0.074 Uiso 1 1 calc R . . C78 C 0.7336(5) 0.1904(5) 0.0601(4) 0.077(3) Uani 1 1 d . . . H78 H 0.7703 0.2087 0.0767 0.092 Uiso 1 1 calc R . . C79 C 0.7424(5) 0.1691(5) 0.0124(4) 0.082(3) Uani 1 1 d . . . H79 H 0.7843 0.1750 -0.0028 0.098 Uiso 1 1 calc R . . C80 C 0.6907(5) 0.1401(5) -0.0117(3) 0.069(3) Uani 1 1 d . . . H80 H 0.6970 0.1250 -0.0432 0.083 Uiso 1 1 calc R . . C81 C 0.6267(4) 0.1329(4) 0.0114(3) 0.061(2) Uani 1 1 d . . . H81 H 0.5904 0.1135 -0.0049 0.074 Uiso 1 1 calc R . . C82 C 0.4950(4) 0.1783(4) 0.2270(3) 0.053(2) Uani 1 1 d . . . C83 C 0.5505(5) 0.1359(4) 0.2320(3) 0.064(2) Uani 1 1 d . . . H83 H 0.5814 0.1306 0.2067 0.077 Uiso 1 1 calc R . . C84 C 0.5592(5) 0.1019(5) 0.2748(4) 0.085(3) Uani 1 1 d . . . H84 H 0.5956 0.0729 0.2783 0.102 Uiso 1 1 calc R . . C85 C 0.5139(7) 0.1110(6) 0.3122(4) 0.099(4) Uani 1 1 d . . . H85 H 0.5201 0.0884 0.3412 0.119 Uiso 1 1 calc R . . C86 C 0.4598(7) 0.1528(5) 0.3073(4) 0.100(4) Uani 1 1 d . . . H86 H 0.4300 0.1590 0.3332 0.120 Uiso 1 1 calc R . . C87 C 0.4493(6) 0.1858(4) 0.2646(3) 0.077(3) Uani 1 1 d . . . H87 H 0.4115 0.2131 0.2610 0.093 Uiso 1 1 calc R . . C88 C 0.5095(4) 0.3079(4) 0.1848(3) 0.048(2) Uani 1 1 d . . . C89 C 0.4742(5) 0.3452(4) 0.2188(3) 0.065(2) Uani 1 1 d . . . H89 H 0.4387 0.3262 0.2363 0.078 Uiso 1 1 calc R . . C90 C 0.4916(6) 0.4108(5) 0.2267(3) 0.082(3) Uani 1 1 d . . . H90 H 0.4674 0.4358 0.2492 0.098 Uiso 1 1 calc R . . C91 C 0.5448(6) 0.4387(5) 0.2011(5) 0.099(4) Uani 1 1 d . . . H91 H 0.5562 0.4827 0.2062 0.118 Uiso 1 1 calc R . . C92 C 0.5793(5) 0.4035(6) 0.1697(5) 0.105(4) Uani 1 1 d . . . H92 H 0.6157 0.4226 0.1532 0.126 Uiso 1 1 calc R . . C93 C 0.5627(4) 0.3383(5) 0.1605(4) 0.074(3) Uani 1 1 d . . . H93 H 0.5877 0.3146 0.1377 0.088 Uiso 1 1 calc R . . C94 C 0.3969(4) 0.2257(5) 0.1568(3) 0.060(2) Uani 1 1 d . . . C95 C 0.3742(4) 0.2792(5) 0.1296(3) 0.073(3) Uani 1 1 d . . . H95 H 0.4038 0.3135 0.1219 0.088 Uiso 1 1 calc R . . C96 C 0.3054(6) 0.2806(7) 0.1139(4) 0.104(4) Uani 1 1 d . . . H96 H 0.2886 0.3151 0.0950 0.125 Uiso 1 1 calc R . . C97 C 0.2645(6) 0.2291(8) 0.1276(5) 0.128(5) Uani 1 1 d . . . H97 H 0.2190 0.2294 0.1180 0.154 Uiso 1 1 calc R . . C98 C 0.2873(7) 0.1778(7) 0.1546(6) 0.145(6) Uani 1 1 d . . . H98 H 0.2574 0.1443 0.1635 0.174 Uiso 1 1 calc R . . C99 C 0.3539(5) 0.1750(5) 0.1686(4) 0.094(4) Uani 1 1 d . . . H99 H 0.3700 0.1390 0.1862 0.113 Uiso 1 1 calc R . . C100 C 0.6118(6) 0.8251(5) 0.6811(4) 0.113(4) Uani 1 1 d . . . H10A H 0.5645 0.8126 0.6858 0.135 Uiso 1 1 calc R . . H10B H 0.6259 0.8512 0.7088 0.135 Uiso 1 1 calc R . . C101 C 0.4389(8) 0.4987(7) 0.0211(6) 0.172(7) Uani 1 1 d . . . H10C H 0.4800 0.5230 0.0130 0.206 Uiso 1 1 calc R . . H10D H 0.4008 0.5211 0.0058 0.206 Uiso 1 1 calc R . . C102 C 0.6490(6) 0.5330(7) 0.0561(8) 0.172(9) Uani 1 1 d . . . H10H H 0.6114 0.5465 0.0354 0.206 Uiso 1 1 calc R . . H10I H 0.6905 0.5501 0.0416 0.206 Uiso 1 1 calc R . . C103 C 0.6403(9) 0.5640(8) 0.1017(6) 0.219(12) Uani 1 1 d . . . H10E H 0.6712 0.5449 0.1248 0.329 Uiso 1 1 calc R . . H10F H 0.5942 0.5578 0.1127 0.329 Uiso 1 1 calc R . . H10G H 0.6495 0.6103 0.0987 0.329 Uiso 1 1 calc R . . C104 C 0.6631(9) 0.4201(9) 0.0229(6) 0.154(6) Uani 1 1 d . . . H10J H 0.6311 0.4291 -0.0032 0.185 Uiso 1 1 calc R . . H10K H 0.7080 0.4294 0.0096 0.185 Uiso 1 1 calc R . . C105 C 0.6616(13) 0.3565(9) 0.0283(7) 0.286(15) Uani 1 1 d . . . H10L H 0.6154 0.3424 0.0335 0.429 Uiso 1 1 calc R . . H10M H 0.6889 0.3443 0.0558 0.429 Uiso 1 1 calc R . . H10N H 0.6794 0.3356 -0.0003 0.429 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0263(4) 0.0323(5) 0.0327(5) 0.0056(4) 0.0005(4) 0.0016(4) Cu2 0.0268(4) 0.0360(5) 0.0323(4) 0.0073(4) -0.0007(4) -0.0019(4) Cu3 0.0290(4) 0.0348(5) 0.0356(4) 0.0099(4) 0.0008(4) 0.0004(4) Cu4 0.0258(4) 0.0342(5) 0.0308(5) 0.0044(4) 0.0003(4) 0.0000(4) Cu5 0.0265(5) 0.0390(5) 0.0313(4) 0.0064(4) -0.0008(4) -0.0022(4) Cu6 0.0297(5) 0.0375(5) 0.0359(5) 0.0087(4) 0.0007(4) 0.0017(4) P1 0.0412(12) 0.0490(13) 0.0492(12) -0.0061(10) 0.0002(10) 0.0014(10) P2 0.0420(12) 0.0511(12) 0.0429(10) -0.0010(10) -0.0022(10) 0.0001(11) Cl1 0.0559(13) 0.0679(14) 0.0521(11) 0.0321(10) -0.0041(11) -0.0023(12) Cl2 0.0367(13) 0.135(2) 0.103(2) 0.0591(18) -0.0114(12) 0.0151(14) Cl3 0.0416(13) 0.0853(18) 0.0858(16) 0.0273(14) 0.0193(12) -0.0090(11) Cl4 0.0563(13) 0.0577(13) 0.0621(12) 0.0312(10) 0.0012(11) 0.0020(11) Cl5 0.0425(13) 0.130(2) 0.0841(17) 0.0387(17) -0.0225(12) 0.0052(14) Cl6 0.0465(13) 0.116(2) 0.0800(16) 0.0446(15) 0.0274(12) 0.0057(13) Cl7 0.0407(12) 0.0836(17) 0.0859(16) -0.0171(14) -0.0222(12) 0.0251(11) Cl8 0.0424(12) 0.0678(15) 0.0637(13) 0.0026(11) 0.0185(10) -0.0206(10) Cl9 0.0672(14) 0.0566(13) 0.0614(12) 0.0284(11) 0.0000(11) 0.0069(11) Cl10 0.234(5) 0.113(3) 0.150(3) 0.041(3) -0.007(3) 0.031(3) Cl11 0.174(4) 0.133(3) 0.149(3) 0.037(3) 0.017(3) 0.051(3) Cl12 0.185(5) 0.536(13) 0.164(5) -0.132(6) 0.020(4) 0.004(6) Cl13 0.363(9) 0.153(5) 0.295(7) -0.061(5) -0.050(7) -0.040(5) O1 0.026(2) 0.034(3) 0.038(3) 0.009(2) 0.000(2) 0.005(2) O2 0.022(2) 0.035(3) 0.035(2) 0.013(2) 0.002(2) -0.001(2) O3 0.297(15) 0.129(10) 0.111(8) -0.001(7) 0.050(9) 0.024(9) N1 0.036(4) 0.033(4) 0.035(4) 0.003(3) 0.003(3) 0.001(3) N2 0.025(3) 0.042(4) 0.032(3) 0.009(3) -0.006(3) -0.004(3) N3 0.025(3) 0.041(4) 0.035(4) 0.016(3) -0.003(3) -0.001(3) N4 0.026(3) 0.049(4) 0.046(4) 0.016(3) -0.002(3) 0.001(3) N5 0.032(3) 0.041(4) 0.040(3) 0.019(3) 0.004(3) 0.005(3) N6 0.031(4) 0.036(4) 0.037(3) 0.008(3) 0.004(3) -0.006(3) N7 0.029(4) 0.037(4) 0.024(3) 0.003(3) -0.002(3) 0.000(3) N8 0.028(4) 0.038(4) 0.035(3) 0.008(3) 0.003(3) -0.004(3) N9 0.037(4) 0.046(4) 0.041(4) 0.007(3) -0.004(3) -0.001(3) N10 0.030(3) 0.045(4) 0.042(4) 0.016(3) -0.004(3) 0.004(3) N11 0.028(3) 0.031(3) 0.047(4) 0.012(3) 0.000(3) 0.001(3) N12 0.031(4) 0.041(4) 0.040(4) 0.008(3) 0.004(3) -0.001(3) N13 0.025(3) 0.037(4) 0.032(3) 0.006(3) -0.002(3) 0.000(2) N14 0.030(3) 0.029(3) 0.035(3) 0.008(3) -0.005(3) 0.004(3) N15 0.026(3) 0.042(4) 0.030(3) 0.005(3) -0.003(3) -0.002(3) N16 0.024(3) 0.047(4) 0.029(3) 0.004(3) 0.001(2) -0.004(3) N17 0.033(3) 0.044(4) 0.038(3) 0.016(3) 0.000(3) 0.004(3) N18 0.025(3) 0.041(3) 0.036(3) 0.011(3) -0.001(2) 0.001(3) N19 0.046(4) 0.063(4) 0.041(3) -0.008(3) 0.000(3) -0.002(3) C1 0.030(4) 0.041(5) 0.041(4) 0.014(4) 0.005(3) -0.007(4) C2 0.048(5) 0.036(4) 0.029(4) 0.013(3) -0.003(4) 0.001(4) C3 0.034(4) 0.048(5) 0.040(4) 0.012(4) -0.003(4) 0.007(4) C4 0.037(5) 0.065(6) 0.046(5) 0.032(4) 0.004(4) -0.001(4) C5 0.036(5) 0.060(6) 0.045(5) 0.021(4) 0.001(4) 0.011(4) C6 0.031(5) 0.065(6) 0.041(5) 0.006(4) 0.008(4) -0.006(4) C7 0.025(4) 0.047(5) 0.064(6) 0.005(4) 0.000(4) 0.009(4) C8 0.040(5) 0.053(5) 0.060(5) 0.020(5) 0.008(4) -0.009(4) C9 0.038(5) 0.045(5) 0.065(6) 0.021(4) 0.002(4) -0.004(4) C10 0.035(5) 0.039(5) 0.040(4) 0.006(4) 0.005(4) -0.006(4) C11 0.042(4) 0.033(4) 0.040(4) 0.013(3) 0.000(4) -0.001(4) C12 0.025(4) 0.041(5) 0.047(5) 0.009(4) 0.004(3) 0.005(3) C13 0.048(6) 0.072(7) 0.066(6) 0.033(5) -0.004(5) 0.004(5) C14 0.029(4) 0.078(6) 0.033(4) 0.014(5) -0.011(3) -0.005(4) C15 0.033(5) 0.076(6) 0.044(5) 0.009(5) -0.004(4) -0.011(4) C16 0.036(5) 0.070(6) 0.044(5) 0.017(4) 0.005(4) 0.010(4) C17 0.034(4) 0.055(5) 0.046(5) 0.025(4) 0.009(3) -0.001(4) C18 0.047(5) 0.051(5) 0.031(4) 0.014(4) -0.001(4) 0.004(4) C19 0.028(4) 0.034(4) 0.040(4) 0.004(3) 0.003(3) -0.002(3) C20 0.024(4) 0.039(5) 0.053(5) 0.004(4) -0.003(4) 0.006(3) C21 0.034(4) 0.037(5) 0.032(4) 0.005(3) -0.007(3) -0.005(3) C22 0.036(4) 0.041(5) 0.039(4) 0.005(4) -0.009(4) -0.002(4) C23 0.044(5) 0.050(6) 0.056(5) -0.001(4) -0.004(4) 0.007(4) C24 0.077(6) 0.057(6) 0.052(5) -0.028(5) -0.005(5) 0.011(5) C25 0.100(8) 0.067(7) 0.045(5) -0.008(5) -0.013(5) -0.007(6) C26 0.132(10) 0.068(8) 0.058(6) 0.002(6) -0.058(6) 0.003(6) C27 0.094(7) 0.035(5) 0.059(5) 0.003(4) -0.029(5) 0.017(5) C28 0.034(4) 0.034(4) 0.046(5) 0.002(4) 0.006(4) 0.000(3) C29 0.048(5) 0.071(6) 0.059(6) -0.004(5) 0.004(4) 0.006(4) C30 0.066(7) 0.109(9) 0.070(7) -0.024(6) 0.027(6) 0.022(6) C31 0.086(8) 0.091(8) 0.062(6) -0.029(6) 0.000(6) -0.001(6) C32 0.069(7) 0.072(7) 0.059(6) -0.023(5) 0.004(5) -0.003(5) C33 0.041(5) 0.056(6) 0.048(5) -0.001(4) -0.001(4) 0.002(4) C34 0.022(4) 0.039(5) 0.044(5) 0.007(4) 0.000(3) 0.000(3) C35 0.023(4) 0.035(4) 0.050(5) 0.008(4) 0.007(4) -0.010(3) C36 0.029(4) 0.038(5) 0.033(4) 0.008(4) 0.007(3) 0.002(3) C37 0.030(4) 0.055(6) 0.036(5) 0.002(4) 0.000(3) 0.000(4) C38 0.053(5) 0.065(6) 0.048(5) 0.010(5) 0.003(4) -0.008(4) C39 0.079(7) 0.100(9) 0.039(5) 0.001(6) 0.020(5) -0.024(6) C40 0.088(8) 0.102(9) 0.040(6) -0.014(6) 0.021(5) -0.023(6) C41 0.073(7) 0.066(7) 0.076(7) -0.026(6) 0.003(6) -0.011(5) C42 0.065(6) 0.056(6) 0.049(5) -0.008(5) 0.012(4) -0.022(4) C43 0.040(5) 0.040(5) 0.038(4) 0.010(4) 0.001(4) -0.013(4) C44 0.038(5) 0.057(5) 0.047(5) -0.007(4) 0.008(4) -0.001(4) C45 0.067(7) 0.067(6) 0.061(6) -0.015(5) 0.015(5) -0.009(5) C46 0.077(7) 0.070(7) 0.076(7) -0.028(5) -0.004(6) -0.024(5) C47 0.053(6) 0.085(7) 0.071(6) -0.016(6) -0.005(5) -0.015(5) C48 0.036(5) 0.066(6) 0.063(6) -0.010(5) 0.005(4) -0.007(4) C49 0.044(5) 0.046(5) 0.032(4) 0.014(4) -0.005(4) 0.001(4) C50 0.036(4) 0.036(5) 0.046(4) 0.014(4) 0.010(3) 0.012(3) C51 0.030(4) 0.040(5) 0.045(4) 0.011(3) 0.015(4) 0.005(4) C52 0.037(5) 0.047(5) 0.057(5) 0.013(4) 0.008(4) 0.009(4) C53 0.065(6) 0.049(6) 0.070(6) -0.001(5) 0.002(5) -0.006(5) C54 0.078(7) 0.055(7) 0.082(7) 0.014(6) 0.002(6) -0.007(5) C55 0.075(7) 0.055(7) 0.116(10) -0.017(6) -0.004(7) 0.001(5) C56 0.077(7) 0.078(7) 0.062(6) -0.011(6) 0.007(5) -0.002(6) C57 0.065(6) 0.057(6) 0.053(5) 0.004(4) 0.001(5) 0.002(5) C58 0.038(5) 0.042(5) 0.047(5) 0.016(4) 0.009(4) 0.006(4) C59 0.060(6) 0.067(6) 0.044(5) 0.007(5) -0.007(4) 0.004(5) C60 0.081(7) 0.065(6) 0.071(6) -0.002(5) -0.009(6) 0.009(5) C61 0.098(9) 0.102(10) 0.070(7) 0.009(7) -0.038(6) -0.015(7) C62 0.077(7) 0.074(8) 0.092(8) 0.032(6) -0.026(6) 0.005(6) C63 0.063(6) 0.067(6) 0.047(5) 0.010(5) -0.008(4) 0.001(5) C64 0.048(5) 0.060(5) 0.045(4) -0.006(4) -0.012(4) 0.001(5) C65 0.064(6) 0.067(7) 0.060(6) 0.000(5) -0.001(5) 0.008(5) C66 0.139(11) 0.055(7) 0.054(6) 0.003(5) -0.027(6) 0.024(7) C67 0.142(11) 0.059(7) 0.067(7) 0.005(5) -0.020(8) -0.027(8) C68 0.102(9) 0.086(8) 0.092(7) 0.022(6) -0.003(8) -0.023(7) C69 0.066(6) 0.073(7) 0.093(7) 0.008(6) -0.011(6) 0.002(6) C70 0.045(5) 0.045(5) 0.043(4) -0.004(4) -0.003(4) 0.000(4) C71 0.062(6) 0.050(5) 0.063(5) -0.010(4) -0.001(5) 0.002(5) C72 0.081(7) 0.051(6) 0.083(7) 0.000(5) -0.010(6) 0.021(5) C73 0.076(7) 0.075(7) 0.061(6) 0.005(6) -0.017(5) 0.009(6) C74 0.074(7) 0.069(7) 0.062(6) 0.000(5) -0.019(5) 0.000(5) C75 0.062(6) 0.048(5) 0.061(5) 0.001(4) -0.008(5) 0.005(4) C76 0.048(5) 0.052(5) 0.057(5) -0.003(5) -0.001(4) 0.009(4) C77 0.049(6) 0.083(7) 0.053(5) -0.004(5) 0.000(5) -0.004(5) C78 0.056(6) 0.100(8) 0.075(7) -0.019(6) 0.002(6) -0.014(5) C79 0.045(6) 0.101(9) 0.100(8) 0.011(7) 0.013(6) -0.012(6) C80 0.066(6) 0.073(7) 0.068(6) 0.004(6) 0.024(5) 0.011(6) C81 0.046(5) 0.069(6) 0.069(6) -0.002(5) -0.003(5) 0.001(4) C82 0.067(6) 0.045(5) 0.047(5) -0.003(4) 0.008(4) -0.011(4) C83 0.071(6) 0.067(6) 0.056(5) 0.004(5) -0.005(5) 0.001(5) C84 0.095(9) 0.081(7) 0.080(7) 0.019(6) -0.016(6) -0.009(6) C85 0.169(13) 0.078(8) 0.050(6) 0.016(6) -0.022(8) -0.032(8) C86 0.168(13) 0.067(8) 0.066(7) -0.005(6) 0.038(8) -0.013(9) C87 0.108(9) 0.051(6) 0.072(6) 0.007(5) 0.023(6) 0.005(5) C88 0.040(5) 0.053(5) 0.050(5) -0.001(4) -0.006(4) 0.010(4) C89 0.093(7) 0.056(6) 0.047(5) -0.003(4) -0.006(5) 0.002(5) C90 0.126(10) 0.054(7) 0.065(6) -0.017(5) -0.024(6) 0.022(6) C91 0.085(8) 0.052(7) 0.159(12) -0.014(8) -0.056(8) 0.013(7) C92 0.059(7) 0.057(8) 0.199(14) 0.027(9) 0.004(8) -0.010(6) C93 0.058(6) 0.061(7) 0.102(8) -0.010(6) 0.003(5) 0.002(5) C94 0.040(5) 0.070(7) 0.071(6) -0.013(5) 0.002(5) 0.005(5) C95 0.047(6) 0.094(8) 0.079(7) -0.015(6) -0.005(5) 0.004(5) C96 0.072(8) 0.144(12) 0.096(8) -0.003(8) -0.017(7) 0.039(8) C97 0.056(8) 0.176(15) 0.152(13) -0.024(12) -0.004(8) -0.045(10) C98 0.080(11) 0.123(13) 0.234(19) 0.046(12) -0.001(11) -0.011(8) C99 0.051(7) 0.086(8) 0.144(11) -0.011(7) 0.001(7) -0.010(6) C100 0.149(11) 0.089(9) 0.100(9) 0.002(7) 0.044(8) -0.018(8) C101 0.177(17) 0.132(13) 0.207(17) 0.073(13) 0.008(14) -0.003(11) C102 0.076(9) 0.094(12) 0.35(3) 0.119(15) -0.016(12) 0.004(8) C103 0.28(2) 0.090(12) 0.29(2) -0.040(14) 0.171(19) 0.013(12) C104 0.158(15) 0.150(17) 0.155(15) -0.018(14) 0.005(12) -0.010(12) C105 0.60(5) 0.085(13) 0.175(18) 0.001(14) 0.00(2) 0.05(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 O1 1.893(4) . ? Cu1 N1 1.960(5) . ? Cu1 N6 1.979(5) . ? Cu1 N13 2.012(5) . ? Cu1 Cu4 3.0502(12) . ? Cu2 O1 1.887(4) . ? Cu2 N2 1.948(5) . ? Cu2 N3 1.968(5) . ? Cu2 N15 2.045(5) . ? Cu2 Cu5 3.0258(11) . ? Cu3 O1 1.886(4) . ? Cu3 N5 1.938(5) . ? Cu3 N4 1.951(5) . ? Cu3 N17 2.049(5) . ? Cu3 Cu6 3.0364(12) . ? Cu4 O2 1.896(4) . ? Cu4 N7 1.951(5) . ? Cu4 N12 1.967(5) . ? Cu4 N14 2.042(5) . ? Cu5 O2 1.887(4) . ? Cu5 N8 1.950(5) . ? Cu5 N9 1.960(6) . ? Cu5 N16 2.026(5) . ? Cu6 O2 1.881(4) . ? Cu6 N11 1.965(5) . ? Cu6 N10 1.982(5) . ? Cu6 N18 2.047(5) . ? P1 N19 1.573(6) . ? P1 C88 1.784(8) . ? P1 C94 1.795(8) . ? P1 C82 1.796(8) . ? P2 N19 1.578(6) . ? P2 C76 1.790(8) . ? P2 C64 1.795(8) . ? P2 C70 1.795(7) . ? Cl1 C2 1.732(6) . ? Cl2 C5 1.704(7) . ? Cl3 C8 1.723(7) . ? Cl4 C11 1.730(6) . ? Cl5 C14 1.720(7) . ? Cl6 C17 1.719(7) . ? Cl7 C20 1.718(7) . ? Cl8 C35 1.744(6) . ? Cl9 C50 1.735(7) . ? Cl10 C100 1.700(11) . ? Cl11 C100 1.698(11) . ? Cl12 C101 1.566(15) . ? Cl13 C101 1.705(16) . ? O3 C104 1.315(16) . ? O3 C102 1.337(15) . ? N1 C3 1.340(8) . ? N1 N2 1.359(6) . ? N2 C1 1.340(8) . ? N3 C6 1.322(8) . ? N3 N4 1.359(7) . ? N4 C4 1.331(8) . ? N5 C9 1.334(8) . ? N5 N6 1.357(7) . ? N6 C7 1.340(8) . ? N7 C12 1.331(8) . ? N7 N8 1.365(6) . ? N8 C10 1.339(8) . ? N9 N10 1.349(7) . ? N9 C15 1.350(8) . ? N10 C13 1.349(9) . ? N11 C18 1.327(8) . ? N11 N12 1.371(7) . ? N12 C16 1.344(8) . ? N13 C21 1.338(8) . ? N13 N14 1.378(7) . ? N14 C19 1.363(8) . ? N15 C36 1.354(8) . ? N15 N16 1.360(7) . ? N16 C34 1.358(8) . ? N17 C51 1.338(8) . ? N17 N18 1.362(7) . ? N18 C49 1.337(8) . ? C1 C2 1.358(9) . ? C2 C3 1.367(9) . ? C4 C5 1.362(10) . ? C5 C6 1.388(10) . ? C7 C8 1.368(10) . ? C8 C9 1.379(10) . ? C10 C11 1.373(9) . ? C11 C12 1.357(9) . ? C13 C14 1.367(10) . ? C14 C15 1.349(10) . ? C16 C17 1.350(9) . ? C17 C18 1.399(9) . ? C19 C20 1.388(9) . ? C19 C28 1.462(9) . ? C20 C21 1.381(9) . ? C21 C22 1.488(9) . ? C22 C27 1.386(9) . ? C22 C23 1.394(10) . ? C23 C24 1.405(10) . ? C24 C25 1.369(11) . ? C25 C26 1.358(12) . ? C26 C27 1.392(11) . ? C28 C29 1.400(9) . ? C28 C33 1.419(10) . ? C29 C30 1.401(11) . ? C30 C31 1.331(12) . ? C31 C32 1.365(12) . ? C32 C33 1.356(10) . ? C34 C35 1.408(9) . ? C34 C43 1.471(10) . ? C35 C36 1.364(9) . ? C36 C37 1.508(9) . ? C37 C42 1.378(10) . ? C37 C38 1.394(10) . ? C38 C39 1.382(11) . ? C39 C40 1.343(12) . ? C40 C41 1.359(12) . ? C41 C42 1.399(11) . ? C43 C48 1.382(9) . ? C43 C44 1.388(9) . ? C44 C45 1.372(10) . ? C45 C46 1.387(11) . ? C46 C47 1.379(11) . ? C47 C48 1.368(11) . ? C49 C50 1.375(9) . ? C49 C58 1.449(10) . ? C50 C51 1.399(9) . ? C51 C52 1.476(10) . ? C52 C57 1.382(10) . ? C52 C53 1.387(10) . ? C53 C54 1.354(12) . ? C54 C55 1.373(13) . ? C55 C56 1.374(12) . ? C56 C57 1.375(11) . ? C58 C59 1.362(10) . ? C58 C63 1.395(10) . ? C59 C60 1.376(11) . ? C60 C61 1.368(12) . ? C61 C62 1.357(13) . ? C62 C63 1.372(12) . ? C64 C65 1.365(10) . ? C64 C69 1.401(11) . ? C65 C66 1.377(12) . ? C66 C67 1.353(13) . ? C67 C68 1.346(14) . ? C68 C69 1.392(12) . ? C70 C71 1.376(10) . ? C70 C75 1.387(10) . ? C71 C72 1.382(11) . ? C72 C73 1.354(12) . ? C73 C74 1.372(12) . ? C74 C75 1.389(11) . ? C76 C77 1.372(10) . ? C76 C81 1.398(10) . ? C77 C78 1.362(11) . ? C78 C79 1.391(12) . ? C79 C80 1.346(12) . ? C80 C81 1.413(11) . ? C82 C87 1.377(11) . ? C82 C83 1.392(11) . ? C83 C84 1.374(11) . ? C84 C85 1.372(14) . ? C85 C86 1.362(15) . ? C86 C87 1.369(13) . ? C88 C93 1.382(11) . ? C88 C89 1.388(10) . ? C89 C90 1.390(11) . ? C90 C91 1.380(14) . ? C91 C92 1.309(15) . ? C92 C93 1.384(13) . ? C94 C99 1.368(12) . ? C94 C95 1.390(12) . ? C95 C96 1.418(12) . ? C96 C97 1.367(16) . ? C97 C98 1.354(17) . ? C98 C99 1.362(14) . ? C102 C103 1.42(2) . ? C104 C105 1.300(18) . ? 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 O1 Cu1 N1 90.4(2) . . ? O1 Cu1 N6 90.9(2) . . ? N1 Cu1 N6 168.0(2) . . ? O1 Cu1 N13 160.0(2) . . ? N1 Cu1 N13 95.4(2) . . ? N6 Cu1 N13 87.4(2) . . ? O1 Cu1 Cu4 93.61(13) . . ? N1 Cu1 Cu4 107.23(16) . . ? N6 Cu1 Cu4 84.61(16) . . ? N13 Cu1 Cu4 66.41(16) . . ? O1 Cu2 N2 90.70(19) . . ? O1 Cu2 N3 89.3(2) . . ? N2 Cu2 N3 170.1(2) . . ? O1 Cu2 N15 165.4(2) . . ? N2 Cu2 N15 94.5(2) . . ? N3 Cu2 N15 87.9(2) . . ? O1 Cu2 Cu5 100.19(13) . . ? N2 Cu2 Cu5 109.58(16) . . ? N3 Cu2 Cu5 80.15(17) . . ? N15 Cu2 Cu5 65.20(15) . . ? O1 Cu3 N5 92.6(2) . . ? O1 Cu3 N4 89.0(2) . . ? N5 Cu3 N4 176.7(2) . . ? O1 Cu3 N17 169.2(2) . . ? N5 Cu3 N17 91.2(2) . . ? N4 Cu3 N17 87.8(2) . . ? O1 Cu3 Cu6 104.17(13) . . ? N5 Cu3 Cu6 99.52(17) . . ? N4 Cu3 Cu6 82.90(17) . . ? N17 Cu3 Cu6 65.16(16) . . ? O2 Cu4 N7 90.5(2) . . ? O2 Cu4 N12 88.3(2) . . ? N7 Cu4 N12 169.5(2) . . ? O2 Cu4 N14 165.9(2) . . ? N7 Cu4 N14 87.6(2) . . ? N12 Cu4 N14 96.0(2) . . ? O2 Cu4 Cu1 101.27(13) . . ? N7 Cu4 Cu1 83.78(16) . . ? N12 Cu4 Cu1 106.67(17) . . ? N14 Cu4 Cu1 64.63(16) . . ? O2 Cu5 N8 90.06(19) . . ? O2 Cu5 N9 90.7(2) . . ? N8 Cu5 N9 167.9(2) . . ? O2 Cu5 N16 162.0(2) . . ? N8 Cu5 N16 87.9(2) . . ? N9 Cu5 N16 95.0(2) . . ? O2 Cu5 Cu2 95.58(13) . . ? N8 Cu5 Cu2 81.37(16) . . ? N9 Cu5 Cu2 110.52(17) . . ? N16 Cu5 Cu2 66.44(16) . . ? O2 Cu6 N11 88.9(2) . . ? O2 Cu6 N10 91.3(2) . . ? N11 Cu6 N10 160.7(2) . . ? O2 Cu6 N18 157.2(2) . . ? N11 Cu6 N18 91.5(2) . . ? N10 Cu6 N18 95.7(2) . . ? O2 Cu6 Cu3 91.09(13) . . ? N11 Cu6 Cu3 91.13(17) . . ? N10 Cu6 Cu3 108.13(17) . . ? N18 Cu6 Cu3 66.14(15) . . ? N19 P1 C88 107.5(4) . . ? N19 P1 C94 115.7(4) . . ? C88 P1 C94 106.6(4) . . ? N19 P1 C82 111.9(4) . . ? C88 P1 C82 107.5(3) . . ? C94 P1 C82 107.2(4) . . ? N19 P2 C76 107.1(4) . . ? N19 P2 C64 113.3(3) . . ? C76 P2 C64 107.4(4) . . ? N19 P2 C70 112.7(3) . . ? C76 P2 C70 106.3(4) . . ? C64 P2 C70 109.7(3) . . ? Cu3 O1 Cu2 120.6(2) . . ? Cu3 O1 Cu1 116.8(2) . . ? Cu2 O1 Cu1 114.84(19) . . ? Cu6 O2 Cu5 116.1(2) . . ? Cu6 O2 Cu4 120.2(2) . . ? Cu5 O2 Cu4 119.93(19) . . ? C104 O3 C102 138.3(15) . . ? C3 N1 N2 108.5(6) . . ? C3 N1 Cu1 133.3(5) . . ? N2 N1 Cu1 117.9(4) . . ? C1 N2 N1 107.0(5) . . ? C1 N2 Cu2 134.6(5) . . ? N1 N2 Cu2 117.8(4) . . ? C6 N3 N4 108.2(5) . . ? C6 N3 Cu2 132.8(5) . . ? N4 N3 Cu2 118.7(4) . . ? C4 N4 N3 107.8(5) . . ? C4 N4 Cu3 132.6(5) . . ? N3 N4 Cu3 119.4(4) . . ? C9 N5 N6 108.6(6) . . ? C9 N5 Cu3 131.8(5) . . ? N6 N5 Cu3 117.3(4) . . ? C7 N6 N5 107.9(5) . . ? C7 N6 Cu1 132.5(5) . . ? N5 N6 Cu1 119.1(4) . . ? C12 N7 N8 107.5(5) . . ? C12 N7 Cu4 134.0(5) . . ? N8 N7 Cu4 118.3(4) . . ? C10 N8 N7 107.8(6) . . ? C10 N8 Cu5 131.9(5) . . ? N7 N8 Cu5 120.2(4) . . ? N10 N9 C15 107.6(6) . . ? N10 N9 Cu5 118.3(4) . . ? C15 N9 Cu5 132.8(5) . . ? C13 N10 N9 107.6(6) . . ? C13 N10 Cu6 135.1(5) . . ? N9 N10 Cu6 117.3(4) . . ? C18 N11 N12 107.7(5) . . ? C18 N11 Cu6 132.3(5) . . ? N12 N11 Cu6 119.3(4) . . ? C16 N12 N11 107.8(5) . . ? C16 N12 Cu4 134.1(5) . . ? N11 N12 Cu4 118.1(4) . . ? C21 N13 N14 108.7(5) . . ? C21 N13 Cu1 136.8(5) . . ? N14 N13 Cu1 113.2(4) . . ? C19 N14 N13 107.6(5) . . ? C19 N14 Cu4 137.5(5) . . ? N13 N14 Cu4 114.9(4) . . ? C36 N15 N16 108.1(5) . . ? C36 N15 Cu2 137.2(5) . . ? N16 N15 Cu2 114.7(4) . . ? C34 N16 N15 110.3(5) . . ? C34 N16 Cu5 135.8(5) . . ? N15 N16 Cu5 113.5(4) . . ? C51 N17 N18 109.7(5) . . ? C51 N17 Cu3 132.6(5) . . ? N18 N17 Cu3 114.7(4) . . ? C49 N18 N17 108.3(5) . . ? C49 N18 Cu6 138.7(5) . . ? N17 N18 Cu6 112.7(4) . . ? P1 N19 P2 140.6(4) . . ? N2 C1 C2 109.8(6) . . ? C1 C2 C3 106.0(5) . . ? C1 C2 Cl1 126.4(6) . . ? C3 C2 Cl1 127.5(6) . . ? N1 C3 C2 108.6(6) . . ? N4 C4 C5 109.9(7) . . ? C4 C5 C6 104.8(6) . . ? C4 C5 Cl2 127.7(6) . . ? C6 C5 Cl2 127.5(6) . . ? N3 C6 C5 109.2(6) . . ? N6 C7 C8 109.0(6) . . ? C7 C8 C9 105.9(6) . . ? C7 C8 Cl3 125.0(6) . . ? C9 C8 Cl3 128.9(6) . . ? N5 C9 C8 108.6(7) . . ? N8 C10 C11 108.9(6) . . ? C12 C11 C10 105.8(6) . . ? C12 C11 Cl4 128.1(6) . . ? C10 C11 Cl4 126.1(6) . . ? N7 C12 C11 110.0(6) . . ? N10 C13 C14 109.2(7) . . ? C15 C14 C13 105.8(7) . . ? C15 C14 Cl5 126.7(6) . . ? C13 C14 Cl5 127.4(7) . . ? C14 C15 N9 109.7(7) . . ? N12 C16 C17 110.0(6) . . ? C16 C17 C18 105.2(6) . . ? C16 C17 Cl6 128.3(6) . . ? C18 C17 Cl6 126.5(6) . . ? N11 C18 C17 109.3(6) . . ? N14 C19 C20 108.2(6) . . ? N14 C19 C28 121.6(6) . . ? C20 C19 C28 130.2(6) . . ? C21 C20 C19 106.5(6) . . ? C21 C20 Cl7 126.1(6) . . ? C19 C20 Cl7 127.3(6) . . ? N13 C21 C20 109.0(6) . . ? N13 C21 C22 120.9(6) . . ? C20 C21 C22 130.0(6) . . ? C27 C22 C23 116.6(7) . . ? C27 C22 C21 122.0(7) . . ? C23 C22 C21 121.4(6) . . ? C22 C23 C24 121.0(7) . . ? C25 C24 C23 120.5(8) . . ? C26 C25 C24 119.2(8) . . ? C25 C26 C27 120.8(8) . . ? C22 C27 C26 121.8(8) . . ? C29 C28 C33 115.5(7) . . ? C29 C28 C19 122.2(7) . . ? C33 C28 C19 122.3(6) . . ? C28 C29 C30 120.4(8) . . ? C31 C30 C29 122.0(9) . . ? C30 C31 C32 118.8(9) . . ? C33 C32 C31 121.9(9) . . ? C32 C33 C28 121.4(8) . . ? N16 C34 C35 105.0(6) . . ? N16 C34 C43 122.8(6) . . ? C35 C34 C43 132.3(6) . . ? C36 C35 C34 108.8(6) . . ? C36 C35 Cl8 124.7(5) . . ? C34 C35 Cl8 126.5(5) . . ? N15 C36 C35 107.8(6) . . ? N15 C36 C37 121.9(6) . . ? C35 C36 C37 130.0(6) . . ? C42 C37 C38 118.2(7) . . ? C42 C37 C36 120.1(7) . . ? C38 C37 C36 121.7(7) . . ? C39 C38 C37 121.1(8) . . ? C40 C39 C38 120.4(9) . . ? C39 C40 C41 119.5(9) . . ? C40 C41 C42 121.9(9) . . ? C37 C42 C41 118.9(8) . . ? C48 C43 C44 117.9(7) . . ? C48 C43 C34 121.0(7) . . ? C44 C43 C34 121.1(6) . . ? C45 C44 C43 120.7(7) . . ? C44 C45 C46 120.7(8) . . ? C47 C46 C45 118.7(8) . . ? C48 C47 C46 120.3(8) . . ? C47 C48 C43 121.7(8) . . ? N18 C49 C50 108.2(6) . . ? N18 C49 C58 121.5(7) . . ? C50 C49 C58 130.2(6) . . ? C49 C50 C51 107.2(6) . . ? C49 C50 Cl9 127.6(6) . . ? C51 C50 Cl9 125.2(6) . . ? N17 C51 C50 106.6(6) . . ? N17 C51 C52 123.4(6) . . ? C50 C51 C52 129.9(7) . . ? C57 C52 C53 116.9(8) . . ? C57 C52 C51 122.1(7) . . ? C53 C52 C51 121.0(7) . . ? C54 C53 C52 122.8(9) . . ? C53 C54 C55 119.9(9) . . ? C54 C55 C56 118.6(9) . . ? C55 C56 C57 121.4(9) . . ? C56 C57 C52 120.4(8) . . ? C59 C58 C63 116.5(8) . . ? C59 C58 C49 123.1(7) . . ? C63 C58 C49 120.4(7) . . ? C58 C59 C60 123.1(8) . . ? C61 C60 C59 117.9(9) . . ? C62 C61 C60 121.8(10) . . ? C61 C62 C63 118.7(9) . . ? C62 C63 C58 122.0(9) . . ? C65 C64 C69 118.5(8) . . ? C65 C64 P2 122.2(7) . . ? C69 C64 P2 119.0(7) . . ? C64 C65 C66 120.8(9) . . ? C67 C66 C65 120.1(10) . . ? C68 C67 C66 121.2(11) . . ? C67 C68 C69 119.8(11) . . ? C68 C69 C64 119.6(9) . . ? C71 C70 C75 119.1(7) . . ? C71 C70 P2 118.7(6) . . ? C75 C70 P2 122.0(6) . . ? C70 C71 C72 120.6(8) . . ? C73 C72 C71 120.2(9) . . ? C72 C73 C74 120.5(9) . . ? C73 C74 C75 120.0(9) . . ? C70 C75 C74 119.7(8) . . ? C77 C76 C81 120.0(8) . . ? C77 C76 P2 120.7(7) . . ? C81 C76 P2 119.3(6) . . ? C78 C77 C76 119.7(8) . . ? C77 C78 C79 121.1(9) . . ? C80 C79 C78 120.5(9) . . ? C79 C80 C81 119.4(9) . . ? C76 C81 C80 119.4(8) . . ? C87 C82 C83 120.1(8) . . ? C87 C82 P1 121.0(7) . . ? C83 C82 P1 118.9(6) . . ? C84 C83 C82 119.4(9) . . ? C85 C84 C83 119.7(10) . . ? C86 C85 C84 120.8(10) . . ? C85 C86 C87 120.4(11) . . ? C86 C87 C82 119.6(10) . . ? C93 C88 C89 117.3(8) . . ? C93 C88 P1 121.2(7) . . ? C89 C88 P1 121.4(7) . . ? C88 C89 C90 120.3(9) . . ? C91 C90 C89 119.8(10) . . ? C92 C91 C90 120.3(11) . . ? C91 C92 C93 121.3(11) . . ? C88 C93 C92 120.9(10) . . ? C99 C94 C95 121.2(9) . . ? C99 C94 P1 122.4(8) . . ? C95 C94 P1 116.3(7) . . ? C94 C95 C96 118.9(10) . . ? C97 C96 C95 117.2(12) . . ? C98 C97 C96 123.0(13) . . ? C97 C98 C99 120.3(13) . . ? C98 C99 C94 119.3(12) . . ? Cl11 C100 Cl10 111.6(6) . . ? Cl12 C101 Cl13 115.0(9) . . ? O3 C102 C103 118.1(16) . . ? C105 C104 O3 129.6(18) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.445 _refine_diff_density_min -0.450 _refine_diff_density_rms 0.134