# Electronic Supplementary Material (ESI) for Chemical Science # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Chemical Science' _journal_coden_Cambridge 1475 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Che, Chi-Ming' _publ_contact_author_email cmche@hku.hk _publ_section_title ; Nanostructures of tetranuclear copper(I) complexes with short Cu(I)...Cu(I) contacts: crystallization induced emission enhancement ; _publ_author_name 'Chi-Ming Che' # Attachment '- copper.cif' data_040727e_Complex1 _database_code_depnum_ccdc_archive 'CCDC 793442' #TrackingRef '- copper.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C91 H130 B2 Cl2 Cu4 F8 N10 P4' _chemical_formula_weight 1986.61 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 27.568(7) _cell_length_b 15.989(4) _cell_length_c 25.240(6) _cell_angle_alpha 90.00 _cell_angle_beta 106.726(5) _cell_angle_gamma 90.00 _cell_volume 10655(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 769 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 18.33 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.238 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4152 _exptl_absorpt_coefficient_mu 0.956 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.529454 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 27424 _diffrn_reflns_av_R_equivalents 0.1014 _diffrn_reflns_av_sigmaI/netI 0.1327 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 30 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9375 _reflns_number_gt 4415 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.1635P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9375 _refine_ls_number_parameters 692 _refine_ls_number_restraints 271 _refine_ls_R_factor_all 0.1807 _refine_ls_R_factor_gt 0.0820 _refine_ls_wR_factor_ref 0.2879 _refine_ls_wR_factor_gt 0.2251 _refine_ls_goodness_of_fit_ref 1.001 _refine_ls_restrained_S_all 1.001 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.248010(7) 0.834842(12) 0.469609(8) 0.04479(6) Uani 1 1 d . . . Cu2 Cu 0.179101(8) 0.950883(13) 0.458265(8) 0.04958(7) Uani 1 1 d . . . P1 P 0.293275(17) 0.89886(3) 0.422693(19) 0.05067(15) Uani 1 1 d . . . P2 P 0.194338(18) 1.00411(3) 0.383332(19) 0.05230(16) Uani 1 1 d . . . N1 N 0.19217(5) 0.75153(8) 0.44498(5) 0.0471(5) Uani 1 1 d . . . N2 N 0.13107(5) 0.84937(8) 0.44562(5) 0.0481(5) Uani 1 1 d . . . N3 N 0.07451(5) 0.95535(10) 0.44069(7) 0.0671(6) Uani 1 1 d . . . N4 N 0.24139(5) 0.63446(8) 0.44845(5) 0.0432(4) Uani 1 1 d . . . N5 N 0.29579(5) 0.52118(8) 0.45975(5) 0.0495(5) Uani 1 1 d . . . C1 C 0.14249(6) 0.77072(10) 0.43768(6) 0.0474(6) Uani 1 1 d . A . C2 C 0.10314(7) 0.70843(12) 0.42358(8) 0.0641(7) Uani 1 1 d . . . H2 H 0.1109 0.6535 0.4169 0.077 Uiso 1 1 calc R A . C3 C 0.05508(7) 0.72990(13) 0.42003(9) 0.0778(8) Uani 1 1 d . A . H3 H 0.0301 0.6889 0.4136 0.093 Uiso 1 1 calc R . . C4 C 0.04263(7) 0.81250(13) 0.42595(8) 0.0677(7) Uani 1 1 d . . . C5 C 0.08226(6) 0.87203(12) 0.43844(7) 0.0574(6) Uani 1 1 d . A . C6 C 0.02687(8) 0.98243(16) 0.43172(10) 0.0932(9) Uani 1 1 d . A . C7 C -0.01335(8) 0.92724(16) 0.42435(10) 0.1022(10) Uani 1 1 d . . . H7 H -0.0452 0.9488 0.4223 0.123 Uiso 1 1 calc R A . C8 C -0.00846(7) 0.84382(16) 0.42003(9) 0.0908(9) Uani 1 1 d . A . C9 C 0.01710(9) 1.07609(14) 0.43074(11) 0.1153(11) Uani 1 1 d . . . H9A H 0.0465 1.1040 0.4538 0.173 Uiso 1 1 calc R A . H9B H -0.0114 1.0870 0.4443 0.173 Uiso 1 1 calc R . . H9C H 0.0101 1.0964 0.3935 0.173 Uiso 1 1 calc R . . C10 C -0.05128(9) 0.78654(19) 0.40853(13) 0.1388(14) Uani 1 1 d . . . H10A H -0.0507 0.7563 0.4416 0.208 Uiso 1 1 calc R A . H10B H -0.0491 0.7478 0.3802 0.208 Uiso 1 1 calc R . . H10C H -0.0823 0.8177 0.3962 0.208 Uiso 1 1 calc R . . C11 C 0.20417(6) 0.68185(10) 0.41880(7) 0.0503(6) Uani 1 1 d . . . C12 C 0.18046(8) 0.66278(12) 0.36111(7) 0.0684(8) Uani 1 1 d . . . H12 H 0.1535 0.6949 0.3404 0.082 Uiso 1 1 calc R . . C13 C 0.19788(8) 0.59788(11) 0.33763(7) 0.0702(8) Uani 1 1 d . . . H13 H 0.1832 0.5862 0.3003 0.084 Uiso 1 1 calc R . . C14 C 0.23699(7) 0.54873(10) 0.36797(6) 0.0496(6) Uani 1 1 d . . . C15 C 0.25808(6) 0.56856(10) 0.42415(7) 0.0500(6) Uani 1 1 d . . . C16 C 0.31348(7) 0.45692(11) 0.43727(7) 0.0566(6) Uani 1 1 d . . . C17 C 0.29523(8) 0.43828(11) 0.38041(8) 0.0696(7) Uani 1 1 d . . . H17 H 0.3099 0.3945 0.3663 0.084 Uiso 1 1 calc R . . C18 C 0.25712(8) 0.48188(11) 0.34568(8) 0.0706(8) Uani 1 1 d . . . C19 C 0.35440(7) 0.40403(13) 0.47608(9) 0.0826(8) Uani 1 1 d . . . H19A H 0.3592 0.4221 0.5135 0.124 Uiso 1 1 calc R . . H19B H 0.3855 0.4102 0.4666 0.124 Uiso 1 1 calc R . . H19C H 0.3443 0.3464 0.4726 0.124 Uiso 1 1 calc R . . C20 C 0.23630(11) 0.45726(14) 0.28606(9) 0.1081(11) Uani 1 1 d . . . H20A H 0.2549 0.4102 0.2785 0.162 Uiso 1 1 calc R . . H20B H 0.2395 0.5033 0.2629 0.162 Uiso 1 1 calc R . . H20C H 0.2012 0.4425 0.2786 0.162 Uiso 1 1 calc R . . C21 C 0.32478(5) 0.83004(8) 0.38343(5) 0.0646(7) Uani 1 1 d D . . H21 H 0.3444 0.8655 0.3655 0.078 Uiso 1 1 calc R . . C22 C 0.36180(6) 0.77207(10) 0.42415(6) 0.1175(10) Uani 1 1 d D . . H22A H 0.3433 0.7367 0.4428 0.141 Uiso 1 1 calc R . . H22B H 0.3858 0.8052 0.4519 0.141 Uiso 1 1 calc R . . C23 C 0.39063(6) 0.71705(11) 0.39276(7) 0.1581(13) Uani 1 1 d D . . H23A H 0.4113 0.7522 0.3766 0.190 Uiso 1 1 calc R . . H23B H 0.4129 0.6788 0.4184 0.190 Uiso 1 1 calc R . . C24 C 0.35348(7) 0.66764(9) 0.34746(7) 0.1357(12) Uani 1 1 d D . . H24A H 0.3347 0.6293 0.3640 0.163 Uiso 1 1 calc R . . H24B H 0.3720 0.6348 0.3274 0.163 Uiso 1 1 calc R . . C25 C 0.31635(6) 0.72559(10) 0.30708(6) 0.1344(12) Uani 1 1 d D . . H25A H 0.2925 0.6925 0.2792 0.161 Uiso 1 1 calc R . . H25B H 0.3347 0.7614 0.2885 0.161 Uiso 1 1 calc R . . C26 C 0.28736(5) 0.78002(10) 0.33861(6) 0.0960(10) Uani 1 1 d D . . H26A H 0.2647 0.8178 0.3130 0.115 Uiso 1 1 calc R . . H26B H 0.2672 0.7445 0.3552 0.115 Uiso 1 1 calc R . . C27 C 0.34831(5) 0.96054(9) 0.46390(5) 0.0737(8) Uani 1 1 d D . . H27 H 0.3736 0.9187 0.4822 0.088 Uiso 1 1 calc R . . C28 C 0.33842(5) 1.01071(11) 0.51064(5) 0.0891(9) Uani 1 1 d D . . H28A H 0.3234 0.9747 0.5325 0.107 Uiso 1 1 calc R . . H28B H 0.3145 1.0551 0.4953 0.107 Uiso 1 1 calc R . . C29 C 0.38749(6) 1.04873(11) 0.54798(6) 0.1177(12) Uani 1 1 d D . . H29A H 0.4102 1.0042 0.5659 0.141 Uiso 1 1 calc R . . H29B H 0.3798 1.0824 0.5765 0.141 Uiso 1 1 calc R . . C30 C 0.41371(6) 1.10360(10) 0.51414(6) 0.1383(13) Uani 1 1 d D . . H30A H 0.3922 1.1507 0.4985 0.166 Uiso 1 1 calc R . . H30B H 0.4453 1.1252 0.5381 0.166 Uiso 1 1 calc R . . C31 C 0.42411(5) 1.05186(12) 0.46788(6) 0.1544(15) Uani 1 1 d D . . H31A H 0.4474 1.0069 0.4838 0.185 Uiso 1 1 calc R . . H31B H 0.4400 1.0869 0.4462 0.185 Uiso 1 1 calc R . . C32 C 0.37511(5) 1.01496(11) 0.43014(6) 0.1142(11) Uani 1 1 d D . . H32A H 0.3828 0.9811 0.4017 0.137 Uiso 1 1 calc R . . H32B H 0.3527 1.0599 0.4121 0.137 Uiso 1 1 calc R . . C33 C 0.25339(6) 0.97027(12) 0.37000(8) 0.0650(7) Uani 1 1 d . A . H33A H 0.2732 1.0195 0.3675 0.078 Uiso 1 1 calc R . . H33B H 0.2450 0.9425 0.3343 0.078 Uiso 1 1 calc R . . C34 C 0.19554(6) 1.11781(9) 0.37301(9) 0.0598(8) Uani 0.6980(14) 1 d PDU A 1 H34A H 0.2038 1.1288 0.3384 0.072 Uiso 0.6980(14) 1 calc PR A 1 C35 C 0.14395(6) 1.15843(9) 0.36956(12) 0.0874(11) Uani 0.6980(14) 1 d PDU A 1 H35A H 0.1179 1.1340 0.3391 0.105 Uiso 0.6980(14) 1 calc PR A 1 H35B H 0.1352 1.1477 0.4035 0.105 Uiso 0.6980(14) 1 calc PR A 1 C36 C 0.14650(6) 1.25332(9) 0.36068(11) 0.0994(11) Uani 0.6980(14) 1 d PDU A 1 H36A H 0.1511 1.2636 0.3246 0.119 Uiso 0.6980(14) 1 calc PR A 1 H36B H 0.1146 1.2785 0.3612 0.119 Uiso 0.6980(14) 1 calc PR A 1 C37 C 0.18936(6) 1.29422(9) 0.40465(12) 0.1142(12) Uani 0.6980(14) 1 d PDU A 1 H37A H 0.1822 1.2910 0.4400 0.137 Uiso 0.6980(14) 1 calc PR A 1 H37B H 0.1914 1.3528 0.3956 0.137 Uiso 0.6980(14) 1 calc PR A 1 C38 C 0.24024(6) 1.25231(9) 0.40942(13) 0.1129(12) Uani 0.6980(14) 1 d PDU A 1 H38A H 0.2664 1.2779 0.4392 0.136 Uiso 0.6980(14) 1 calc PR A 1 H38B H 0.2492 1.2599 0.3753 0.136 Uiso 0.6980(14) 1 calc PR A 1 C39 C 0.23672(6) 1.15732(9) 0.42123(9) 0.0647(9) Uani 0.6980(14) 1 d PDU A 1 H39A H 0.2691 1.1306 0.4248 0.078 Uiso 0.6980(14) 1 calc PR A 1 H39B H 0.2282 1.1495 0.4556 0.078 Uiso 0.6980(14) 1 calc PR A 1 C40 C 0.14436(9) 0.97030(9) 0.32153(6) 0.0437(8) Uani 0.5896(14) 1 d PDU A 1 H40A H 0.1126 0.9868 0.3286 0.052 Uiso 0.5896(14) 1 calc PR A 1 C41 C 0.14075(8) 0.87509(9) 0.31444(7) 0.0521(9) Uani 0.5896(14) 1 d PDU A 1 H41A H 0.1434 0.8489 0.3498 0.063 Uiso 0.5896(14) 1 calc PR A 1 H41B H 0.1685 0.8551 0.3014 0.063 Uiso 0.5896(14) 1 calc PR A 1 C42 C 0.08985(8) 0.85122(10) 0.27254(7) 0.0988(13) Uani 0.5896(14) 1 d PDU A 1 H42A H 0.0879 0.7910 0.2678 0.119 Uiso 0.5896(14) 1 calc PR A 1 H42B H 0.0621 0.8688 0.2865 0.119 Uiso 0.5896(14) 1 calc PR A 1 C43 C 0.08492(10) 0.89332(10) 0.21658(7) 0.1026(13) Uani 0.5896(14) 1 d PDU A 1 H43A H 0.1103 0.8706 0.2008 0.123 Uiso 0.5896(14) 1 calc PR A 1 H43B H 0.0518 0.8810 0.1914 0.123 Uiso 0.5896(14) 1 calc PR A 1 C44 C 0.09164(9) 0.98737(10) 0.22252(8) 0.1170(14) Uani 0.5896(14) 1 d PDU A 1 H44A H 0.0639 1.0110 0.2341 0.140 Uiso 0.5896(14) 1 calc PR A 1 H44B H 0.0906 1.0114 0.1869 0.140 Uiso 0.5896(14) 1 calc PR A 1 C45 C 0.14223(8) 1.01030(10) 0.26515(7) 0.0725(10) Uani 0.5896(14) 1 d PDU A 1 H45A H 0.1452 1.0706 0.2690 0.087 Uiso 0.5896(14) 1 calc PR A 1 H45B H 0.1702 0.9901 0.2526 0.087 Uiso 0.5896(14) 1 calc PR A 1 C34' C 0.18885(13) 1.12455(10) 0.38886(7) 0.0768(15) Uani 0.3020(14) 1 d PDU A 2 H34B H 0.1540 1.1365 0.3891 0.092 Uiso 0.3020(14) 1 calc PR A 2 C35' C 0.19556(15) 1.16375(10) 0.33561(6) 0.0720(14) Uani 0.3020(14) 1 d PDU A 2 H35C H 0.2301 1.1555 0.3345 0.086 Uiso 0.3020(14) 1 calc PR A 2 H35D H 0.1731 1.1365 0.3035 0.086 Uiso 0.3020(14) 1 calc PR A 2 C36' C 0.18364(18) 1.25779(10) 0.33396(7) 0.2044(17) Uani 0.3020(14) 1 d PDU A 2 H36C H 0.1888 1.2822 0.3008 0.245 Uiso 0.3020(14) 1 calc PR A 2 H36D H 0.1484 1.2658 0.3327 0.245 Uiso 0.3020(14) 1 calc PR A 2 C37' C 0.21779(14) 1.30175(10) 0.38505(7) 0.1427(17) Uani 0.3020(14) 1 d PDU A 2 H37C H 0.2091 1.3607 0.3839 0.171 Uiso 0.3020(14) 1 calc PR A 2 H37D H 0.2529 1.2971 0.3850 0.171 Uiso 0.3020(14) 1 calc PR A 2 C38' C 0.21145(16) 1.26238(10) 0.43818(6) 0.0915(16) Uani 0.3020(14) 1 d PDU A 2 H38C H 0.1769 1.2699 0.4394 0.110 Uiso 0.3020(14) 1 calc PR A 2 H38D H 0.2338 1.2900 0.4702 0.110 Uiso 0.3020(14) 1 calc PR A 2 C39' C 0.22412(18) 1.16836(11) 0.43983(7) 2.00(16) Uiso 0.3020(14) 1 d PD A 2 H39C H 0.2592 1.1609 0.4403 2.400 Uiso 0.3020(14) 1 d PR A 2 H39D H 0.2198 1.1437 0.4733 2.400 Uiso 0.3020(14) 1 d PR A 2 C40' C 0.14633(6) 0.98646(11) 0.31427(13) 0.1179(15) Uani 0.4104(14) 1 d PDU A 2 H40B H 0.1564 1.0162 0.2851 0.141 Uiso 0.4104(14) 1 calc PR A 2 C41' C 0.14675(7) 0.89201(11) 0.30487(11) 0.1551(16) Uani 0.4104(14) 1 d PDU A 2 H41C H 0.1400 0.8631 0.3358 0.186 Uiso 0.4104(14) 1 calc PR A 2 H41D H 0.1800 0.8750 0.3029 0.186 Uiso 0.4104(14) 1 calc PR A 2 C42' C 0.10643(6) 0.86768(12) 0.25082(9) 0.1426(16) Uani 0.4104(14) 1 d PDU A 2 H42C H 0.1145 0.8936 0.2196 0.171 Uiso 0.4104(14) 1 calc PR A 2 H42D H 0.1065 0.8075 0.2460 0.171 Uiso 0.4104(14) 1 calc PR A 2 C43' C 0.05362(6) 0.89650(11) 0.25268(13) 0.1289(16) Uani 0.4104(14) 1 d PDU A 2 H43C H 0.0285 0.8818 0.2183 0.155 Uiso 0.4104(14) 1 calc PR A 2 H43D H 0.0448 0.8685 0.2827 0.155 Uiso 0.4104(14) 1 calc PR A 2 C44' C 0.05359(7) 0.99154(11) 0.26124(11) 0.1384(16) Uani 0.4104(14) 1 d PDU A 2 H44C H 0.0203 1.0095 0.2625 0.166 Uiso 0.4104(14) 1 calc PR A 2 H44D H 0.0612 1.0196 0.2305 0.166 Uiso 0.4104(14) 1 calc PR A 2 C45' C 0.09359(6) 1.01535(12) 0.31582(9) 0.1122(15) Uani 0.4104(14) 1 d PDU A 2 H45C H 0.0936 1.0755 0.3210 0.135 Uiso 0.4104(14) 1 calc PR A 2 H45D H 0.0852 0.9892 0.3467 0.135 Uiso 0.4104(14) 1 calc PR A 2 B1 B 0.17554(6) 0.69217(11) 0.18982(7) 0.1112(13) Uani 1 1 d D . . F1 F 0.19737(7) 0.75982(9) 0.21928(8) 0.2018(11) Uani 1 1 d D . . F2 F 0.13400(5) 0.67251(12) 0.20546(7) 0.2004(10) Uani 1 1 d D . . F3 F 0.16227(6) 0.71185(12) 0.13517(5) 0.1627(9) Uani 1 1 d D . . F4 F 0.20824(6) 0.62780(8) 0.19980(6) 0.1644(8) Uani 1 1 d D . . Cl1 Cl 0.47657(12) -0.0224(2) 0.35289(8) 0.2106(14) Uani 0.25 1 d PDU . . Cl2 Cl 0.40843(12) -0.06059(16) 0.24910(10) 0.2217(15) Uani 0.25 1 d PDU . . C46 C 0.44239(17) 0.01718(18) 0.29029(10) 0.1553(17) Uani 0.25 1 d PDU . . H46A H 0.4652 0.0429 0.2721 0.186 Uiso 0.25 1 calc PR . . H46B H 0.4194 0.0599 0.2959 0.186 Uiso 0.25 1 calc PR . . Cl3 Cl 0.02721(9) 0.20212(17) 0.22158(8) 0.2530(16) Uani 0.25 1 d PDU . . Cl4 Cl -0.00460(12) 0.2497(3) 0.31373(7) 0.3287(17) Uani 0.25 1 d PDU . . C47 C 0.0000 0.27909(18) 0.2500 0.2437(17) Uani 0.50 2 d SPDU . . H47A H -0.0329 0.2924 0.2259 0.292 Uiso 0.25 1 d PR . . H47B H 0.0207 0.3284 0.2542 0.292 Uiso 0.25 1 d PR . . 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 0.05226(10) 0.03782(10) 0.04628(10) -0.00081(9) 0.01734(8) 0.00234(9) Cu2 0.05675(11) 0.04350(11) 0.05161(11) 0.00141(10) 0.02054(9) 0.00698(10) P1 0.0579(2) 0.0473(3) 0.0520(2) 0.0035(2) 0.02401(19) 0.0036(2) P2 0.0679(3) 0.0404(2) 0.0515(2) 0.0057(2) 0.0219(2) 0.0071(2) N1 0.0546(8) 0.0351(7) 0.0503(8) -0.0036(6) 0.0127(6) 0.0030(6) N2 0.0431(7) 0.0501(8) 0.0506(8) 0.0019(7) 0.0125(6) 0.0047(6) N3 0.0564(8) 0.0692(10) 0.0747(10) -0.0053(9) 0.0172(7) 0.0151(8) N4 0.0604(8) 0.0340(7) 0.0375(7) 0.0042(6) 0.0176(6) -0.0015(6) N5 0.0619(8) 0.0438(8) 0.0470(7) -0.0025(7) 0.0225(6) 0.0038(7) C1 0.0463(9) 0.0519(10) 0.0398(9) -0.0031(8) 0.0057(7) -0.0051(8) C2 0.0696(11) 0.0493(10) 0.0684(12) 0.0107(10) 0.0121(9) -0.0090(10) C3 0.0676(12) 0.0714(13) 0.0943(15) 0.0009(12) 0.0231(10) -0.0165(11) C4 0.0439(10) 0.0919(14) 0.0663(12) 0.0034(11) 0.0143(8) -0.0032(10) C5 0.0480(9) 0.0728(12) 0.0540(10) -0.0018(10) 0.0191(7) 0.0013(9) C6 0.0777(13) 0.1185(18) 0.0803(14) -0.0126(14) 0.0181(11) 0.0279(13) C7 0.0560(11) 0.139(2) 0.1111(17) -0.0146(16) 0.0240(11) 0.0217(13) C8 0.0544(11) 0.132(2) 0.0880(15) -0.0115(14) 0.0237(10) -0.0078(13) C9 0.1002(15) 0.0933(15) 0.134(2) -0.0149(15) 0.0049(15) 0.0559(12) C10 0.0648(14) 0.168(3) 0.180(3) -0.029(2) 0.0300(16) -0.0196(17) C11 0.0592(10) 0.0367(9) 0.0561(10) -0.0017(8) 0.0182(8) -0.0075(8) C12 0.0930(14) 0.0555(11) 0.0486(10) 0.0094(9) 0.0074(10) -0.0017(11) C13 0.1124(15) 0.0451(10) 0.0435(10) -0.0121(9) 0.0071(10) 0.0022(11) C14 0.0805(11) 0.0318(9) 0.0396(8) -0.0021(7) 0.0224(7) -0.0021(8) C15 0.0726(10) 0.0349(9) 0.0485(9) -0.0052(8) 0.0268(7) -0.0088(8) C16 0.0732(10) 0.0434(10) 0.0619(10) -0.0045(9) 0.0332(8) 0.0024(9) C17 0.1012(13) 0.0433(10) 0.0735(11) -0.0152(9) 0.0397(9) 0.0014(10) C18 0.1190(15) 0.0408(10) 0.0480(10) -0.0110(9) 0.0176(10) 0.0005(11) C19 0.0847(12) 0.0808(13) 0.0887(13) -0.0017(12) 0.0353(10) 0.0357(11) C20 0.177(2) 0.0749(14) 0.0681(13) -0.0244(11) 0.0281(14) 0.0192(15) C21 0.0806(11) 0.0683(12) 0.0568(9) 0.0033(9) 0.0388(8) 0.0200(10) C22 0.1411(17) 0.1310(17) 0.0764(15) -0.0022(14) 0.0251(13) 0.0838(13) C23 0.1509(19) 0.173(2) 0.143(2) -0.0168(19) 0.0307(17) 0.1088(15) C24 0.157(2) 0.1008(18) 0.168(2) -0.0473(15) 0.0777(15) 0.0200(16) C25 0.189(2) 0.1109(18) 0.1269(16) -0.0441(14) 0.0829(14) 0.0242(17) C26 0.1123(16) 0.0784(15) 0.1021(15) -0.0249(13) 0.0385(12) 0.0137(13) C27 0.0668(11) 0.0695(13) 0.0909(13) -0.0055(11) 0.0323(9) -0.0138(10) C28 0.1017(15) 0.0972(16) 0.0683(13) -0.0144(13) 0.0244(11) -0.0325(13) C29 0.137(2) 0.0972(17) 0.1072(19) -0.0388(15) 0.0162(17) -0.0378(16) C30 0.1194(16) 0.1163(19) 0.192(3) -0.0310(19) 0.0657(16) -0.0713(14) C31 0.1299(18) 0.145(2) 0.205(3) -0.013(2) 0.0758(17) -0.0659(17) C32 0.1079(14) 0.1172(18) 0.1327(19) -0.0185(16) 0.0589(12) -0.0558(13) C33 0.0610(10) 0.0708(12) 0.0714(11) 0.0164(10) 0.0322(8) 0.0110(10) C34 0.0790(14) 0.0448(13) 0.0609(13) 0.0058(11) 0.0285(10) 0.0024(11) C35 0.0847(16) 0.0723(16) 0.0984(18) 0.0052(14) 0.0154(13) 0.0189(14) C36 0.1044(17) 0.0769(16) 0.1150(19) 0.0025(15) 0.0286(14) 0.0368(14) C37 0.1189(19) 0.0901(18) 0.131(2) 0.0049(17) 0.0312(15) 0.0124(16) C38 0.1136(19) 0.0908(18) 0.128(2) -0.0106(16) 0.0248(15) -0.0182(16) C39 0.0695(14) 0.0421(13) 0.0764(15) -0.0041(12) 0.0111(12) -0.0005(11) C40 0.0613(14) 0.0303(12) 0.0369(12) 0.0065(11) 0.0101(10) 0.0095(11) C41 0.0693(15) 0.0430(14) 0.0400(13) 0.0017(12) 0.0093(11) 0.0012(13) C42 0.112(2) 0.0864(19) 0.089(2) -0.0024(16) 0.0133(16) -0.0109(17) C43 0.108(2) 0.101(2) 0.0851(19) 0.0063(17) 0.0063(16) -0.0078(17) C44 0.127(2) 0.104(2) 0.108(2) 0.0089(18) 0.0152(17) 0.0060(18) C45 0.0901(18) 0.0700(17) 0.0448(15) 0.0123(14) -0.0004(13) -0.0163(15) C34' 0.083(2) 0.069(2) 0.077(2) 0.0066(19) 0.0204(18) 0.004(2) C35' 0.082(2) 0.066(2) 0.069(2) -0.0014(19) 0.0240(17) 0.0104(19) C36' 0.207(3) 0.200(3) 0.205(3) 0.007(2) 0.057(2) -0.001(2) C37' 0.144(3) 0.142(3) 0.143(3) 0.005(2) 0.0425(19) 0.003(2) C38' 0.096(2) 0.083(2) 0.089(2) -0.014(2) 0.0157(18) -0.006(2) C40' 0.122(2) 0.115(2) 0.118(2) -0.002(2) 0.0358(18) -0.001(2) C41' 0.163(3) 0.155(3) 0.146(3) 0.010(2) 0.0409(19) 0.002(2) C42' 0.141(2) 0.140(3) 0.146(3) -0.012(2) 0.0378(19) -0.006(2) C43' 0.128(2) 0.125(2) 0.130(2) -0.013(2) 0.0326(18) 0.004(2) C44' 0.138(2) 0.136(3) 0.137(3) 0.009(2) 0.0334(19) 0.003(2) C45' 0.112(2) 0.120(2) 0.104(2) 0.001(2) 0.0307(18) 0.003(2) B1 0.0898(17) 0.159(3) 0.0906(18) 0.025(2) 0.0354(14) 0.0317(19) F1 0.2075(19) 0.1437(14) 0.232(2) -0.0722(14) 0.0283(16) -0.0067(14) F2 0.1611(13) 0.2119(18) 0.2602(17) 0.0913(14) 0.1118(11) 0.0224(13) F3 0.1350(12) 0.2252(18) 0.1249(12) 0.0525(12) 0.0327(10) 0.0410(13) F4 0.2267(14) 0.1399(11) 0.1288(12) 0.0131(10) 0.0545(10) 0.1054(10) Cl1 0.197(2) 0.241(2) 0.206(2) -0.0075(19) 0.0761(17) 0.0240(19) Cl2 0.197(2) 0.217(2) 0.249(2) -0.021(2) 0.0613(17) 0.0257(19) C46 0.155(3) 0.154(3) 0.157(3) 0.001(2) 0.043(2) 0.014(2) Cl3 0.258(2) 0.240(2) 0.252(2) 0.010(2) 0.0599(18) 0.015(2) Cl4 0.328(3) 0.326(3) 0.333(3) 0.017(2) 0.0969(19) -0.010(2) C47 0.245(3) 0.242(3) 0.242(3) 0.000 0.068(2) 0.000 _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.9949(13) . ? Cu1 N4 2.0631(14) 7_566 ? Cu1 P1 2.2040(7) . ? Cu1 Cu2 2.6116(5) . ? Cu2 N5 2.0338(14) 7_566 ? Cu2 N2 2.0608(14) . ? Cu2 P2 2.2215(7) . ? P1 C33 1.8546(18) . ? P1 C21 1.8554(16) . ? P1 C27 1.8569(14) . ? P2 C33 1.836(2) . ? P2 C34 1.8382(16) . ? P2 C40 1.8404(17) . ? P2 C40' 1.882(2) . ? P2 C34' 1.9399(18) . ? N1 C1 1.363(2) . ? N1 C11 1.383(2) . ? N2 C1 1.326(2) . ? N2 C5 1.354(2) . ? N3 C6 1.339(3) . ? N3 C5 1.353(2) . ? N4 C11 1.3211(19) . ? N4 C15 1.364(2) . ? N4 Cu1 2.0630(14) 7_566 ? N5 C16 1.332(2) . ? N5 C15 1.3873(19) . ? N5 Cu2 2.0338(14) 7_566 ? C1 C2 1.440(2) . ? C2 C3 1.346(3) . ? C2 H2 0.9300 . ? C3 C4 1.383(3) . ? C3 H3 0.9300 . ? C4 C5 1.415(3) . ? C4 C8 1.462(3) . ? C6 C7 1.387(3) . ? C6 C9 1.521(3) . ? C7 C8 1.348(4) . ? C7 H7 0.9300 . ? C8 C10 1.456(3) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.447(2) . ? C12 C13 1.350(3) . ? C12 H12 0.9300 . ? C13 C14 1.375(2) . ? C13 H13 0.9300 . ? C14 C18 1.395(3) . ? C14 C15 1.405(2) . ? C16 C17 1.409(3) . ? C16 C19 1.520(2) . ? C17 C18 1.352(3) . ? C17 H17 0.9300 . ? C18 C20 1.501(3) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C26 1.5205(18) . ? C21 C22 1.5341(19) . ? C21 H21 0.9800 . ? C22 C23 1.548(2) . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.519(2) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 C25 1.531(2) . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.548(2) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.515(2) . ? C27 C32 1.546(2) . ? C27 H27 0.9800 . ? C28 C29 1.5342(19) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.542(2) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 C31 1.524(2) . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.5295(19) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 C39 1.541(2) . ? C34 C35 1.543(2) . ? C34 H34A 0.9800 . ? C35 C36 1.538(2) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C36 C37 1.517(3) . ? C36 H36A 0.9700 . ? C36 H36B 0.9700 . ? C37 C38 1.528(2) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.556(2) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C39 H39C 0.6674 . ? C39 H39D 1.5311 . ? C40 C41 1.533(2) . ? C40 C45 1.546(2) . ? C40 H40A 0.9800 . ? C41 C42 1.542(2) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 C43 1.535(2) . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C43 C44 1.517(2) . ? C43 H43A 0.9700 . ? C43 H43B 0.9700 . ? C44 C45 1.541(3) . ? C44 H44A 0.9700 . ? C44 H44B 0.9700 . ? C45 H45A 0.9700 . ? C45 H45B 0.9700 . ? C34' C39' 1.540(3) . ? C34' C35' 1.542(3) . ? C34' H34B 0.9800 . ? C35' C36' 1.537(3) . ? C35' H35C 0.9700 . ? C35' H35D 0.9700 . ? C36' C37' 1.531(3) . ? C36' H36C 0.9700 . ? C36' H36D 0.9700 . ? C37' C38' 1.536(3) . ? C37' H37C 0.9700 . ? C37' H37D 0.9700 . ? C38' C39' 1.541(3) . ? C38' H38C 0.9700 . ? C38' H38D 0.9700 . ? C39' H39C 0.9700 . ? C39' H39D 0.9700 . ? C40' C41' 1.529(2) . ? C40' C45' 1.537(3) . ? C40' H40B 0.9800 . ? C41' C42' 1.541(3) . ? C41' H41C 0.9700 . ? C41' H41D 0.9700 . ? C42' C43' 1.541(3) . ? C42' H42C 0.9700 . ? C42' H42D 0.9700 . ? C43' C44' 1.535(2) . ? C43' H43C 0.9700 . ? C43' H43D 0.9700 . ? C44' C45' 1.544(3) . ? C44' H44C 0.9700 . ? C44' H44D 0.9700 . ? C45' H45C 0.9700 . ? C45' H45D 0.9700 . ? B1 F4 1.343(2) . ? B1 F2 1.351(2) . ? B1 F1 1.352(2) . ? B1 F3 1.358(2) . ? Cl1 C46 1.711(3) . ? Cl2 C46 1.716(4) . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? Cl3 Cl4 1.201(4) 2 ? Cl3 C47 1.703(3) . ? Cl3 Cl3 2.355(5) 2 ? Cl4 Cl3 1.201(4) 2 ? Cl4 C47 1.715(3) . ? C47 Cl3 1.703(3) 2 ? C47 Cl4 1.715(3) 2 ? C47 H47A 0.9600 . ? C47 H47B 0.9599 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N4 110.19(6) . 7_566 ? N1 Cu1 P1 130.40(5) . . ? N4 Cu1 P1 119.30(4) 7_566 . ? N1 Cu1 Cu2 88.20(4) . . ? N4 Cu1 Cu2 80.19(4) 7_566 . ? P1 Cu1 Cu2 96.75(2) . . ? N5 Cu2 N2 110.24(6) 7_566 . ? N5 Cu2 P2 133.61(4) 7_566 . ? N2 Cu2 P2 116.13(4) . . ? N5 Cu2 Cu1 91.18(4) 7_566 . ? N2 Cu2 Cu1 82.65(4) . . ? P2 Cu2 Cu1 93.195(19) . . ? C33 P1 C21 104.72(8) . . ? C33 P1 C27 107.15(8) . . ? C21 P1 C27 100.45(7) . . ? C33 P1 Cu1 111.15(7) . . ? C21 P1 Cu1 115.85(5) . . ? C27 P1 Cu1 116.32(5) . . ? C33 P2 C34 102.26(9) . . ? C33 P2 C40 104.19(9) . . ? C34 P2 C40 102.13(7) . . ? C33 P2 C40' 102.14(10) . . ? C34 P2 C40' 93.07(8) . . ? C40 P2 C40' 10.10(8) . . ? C33 P2 C34' 113.41(12) . . ? C34 P2 C34' 14.83(10) . . ? C40 P2 C34' 107.32(8) . . ? C40' P2 C34' 99.60(8) . . ? C33 P2 Cu2 115.97(6) . . ? C34 P2 Cu2 121.00(7) . . ? C40 P2 Cu2 109.28(7) . . ? C40' P2 Cu2 118.44(8) . . ? C34' P2 Cu2 106.34(7) . . ? C1 N1 C11 119.06(13) . . ? C1 N1 Cu1 123.15(11) . . ? C11 N1 Cu1 114.68(11) . . ? C1 N2 C5 120.25(14) . . ? C1 N2 Cu2 126.91(11) . . ? C5 N2 Cu2 112.29(11) . . ? C6 N3 C5 118.07(17) . . ? C11 N4 C15 119.73(13) . . ? C11 N4 Cu1 107.11(11) . 7_566 ? C15 N4 Cu1 131.74(10) . 7_566 ? C16 N5 C15 116.32(13) . . ? C16 N5 Cu2 122.93(10) . 7_566 ? C15 N5 Cu2 120.75(11) . 7_566 ? N2 C1 N1 117.80(14) . . ? N2 C1 C2 119.91(15) . . ? N1 C1 C2 122.26(15) . . ? C3 C2 C1 119.79(18) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? C2 C3 C4 120.41(18) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C3 C4 C5 117.83(17) . . ? C3 C4 C8 125.30(19) . . ? C5 C4 C8 116.87(19) . . ? N3 C5 N2 114.88(15) . . ? N3 C5 C4 123.42(16) . . ? N2 C5 C4 121.57(17) . . ? N3 C6 C7 121.6(2) . . ? N3 C6 C9 118.8(2) . . ? C7 C6 C9 119.6(2) . . ? C8 C7 C6 123.1(2) . . ? C8 C7 H7 118.5 . . ? C6 C7 H7 118.5 . . ? C7 C8 C10 123.0(2) . . ? C7 C8 C4 116.5(2) . . ? C10 C8 C4 120.5(2) . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N4 C11 N1 116.42(14) . . ? N4 C11 C12 120.10(16) . . ? N1 C11 C12 123.36(14) . . ? C13 C12 C11 119.29(16) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 C14 121.04(16) . . ? C12 C13 H13 119.5 . . ? C14 C13 H13 119.5 . . ? C13 C14 C18 123.53(15) . . ? C13 C14 C15 117.60(16) . . ? C18 C14 C15 118.86(15) . . ? N4 C15 N5 114.68(13) . . ? N4 C15 C14 122.21(14) . . ? N5 C15 C14 123.07(15) . . ? N5 C16 C17 121.99(15) . . ? N5 C16 C19 116.70(15) . . ? C17 C16 C19 121.31(17) . . ? C18 C17 C16 122.28(18) . . ? C18 C17 H17 118.9 . . ? C16 C17 H17 118.9 . . ? C17 C18 C14 117.31(17) . . ? C17 C18 C20 121.08(19) . . ? C14 C18 C20 121.58(17) . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C26 C21 C22 111.02(11) . . ? C26 C21 P1 112.81(11) . . ? C22 C21 P1 108.90(10) . . ? C26 C21 H21 108.0 . . ? C22 C21 H21 108.0 . . ? P1 C21 H21 108.0 . . ? C21 C22 C23 109.95(12) . . ? C21 C22 H22A 109.7 . . ? C23 C22 H22A 109.7 . . ? C21 C22 H22B 109.7 . . ? C23 C22 H22B 109.7 . . ? H22A C22 H22B 108.2 . . ? C24 C23 C22 110.29(13) . . ? C24 C23 H23A 109.6 . . ? C22 C23 H23A 109.6 . . ? C24 C23 H23B 109.6 . . ? C22 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? C23 C24 C25 111.29(13) . . ? C23 C24 H24A 109.4 . . ? C25 C24 H24A 109.4 . . ? C23 C24 H24B 109.4 . . ? C25 C24 H24B 109.4 . . ? H24A C24 H24B 108.0 . . ? C24 C25 C26 110.07(13) . . ? C24 C25 H25A 109.6 . . ? C26 C25 H25A 109.6 . . ? C24 C25 H25B 109.6 . . ? C26 C25 H25B 109.6 . . ? H25A C25 H25B 108.2 . . ? C21 C26 C25 109.76(12) . . ? C21 C26 H26A 109.7 . . ? C25 C26 H26A 109.7 . . ? C21 C26 H26B 109.7 . . ? C25 C26 H26B 109.7 . . ? H26A C26 H26B 108.2 . . ? C28 C27 C32 110.65(12) . . ? C28 C27 P1 114.59(10) . . ? C32 C27 P1 115.67(9) . . ? C28 C27 H27 104.9 . . ? C32 C27 H27 104.9 . . ? P1 C27 H27 104.9 . . ? C27 C28 C29 111.32(12) . . ? C27 C28 H28A 109.4 . . ? C29 C28 H28A 109.4 . . ? C27 C28 H28B 109.4 . . ? C29 C28 H28B 109.4 . . ? H28A C28 H28B 108.0 . . ? C28 C29 C30 110.87(11) . . ? C28 C29 H29A 109.5 . . ? C30 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? C30 C29 H29B 109.5 . . ? H29A C29 H29B 108.1 . . ? C31 C30 C29 109.69(14) . . ? C31 C30 H30A 109.7 . . ? C29 C30 H30A 109.7 . . ? C31 C30 H30B 109.7 . . ? C29 C30 H30B 109.7 . . ? H30A C30 H30B 108.2 . . ? C30 C31 C32 111.06(13) . . ? C30 C31 H31A 109.4 . . ? C32 C31 H31A 109.4 . . ? C30 C31 H31B 109.4 . . ? C32 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? C31 C32 C27 110.51(11) . . ? C31 C32 H32A 109.5 . . ? C27 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 108.1 . . ? P2 C33 P1 115.08(11) . . ? P2 C33 H33A 108.5 . . ? P1 C33 H33A 108.5 . . ? P2 C33 H33B 108.5 . . ? P1 C33 H33B 108.5 . . ? H33A C33 H33B 107.5 . . ? C39 C34 C35 109.25(16) . . ? C39 C34 P2 109.44(11) . . ? C35 C34 P2 111.74(11) . . ? C39 C34 H34A 108.8 . . ? C35 C34 H34A 108.8 . . ? P2 C34 H34A 108.8 . . ? C36 C35 C34 110.08(14) . . ? C36 C35 H35A 109.6 . . ? C34 C35 H35A 109.6 . . ? C36 C35 H35B 109.6 . . ? C34 C35 H35B 109.6 . . ? H35A C35 H35B 108.2 . . ? C37 C36 C35 112.17(16) . . ? C37 C36 H36A 109.2 . . ? C35 C36 H36A 109.2 . . ? C37 C36 H36B 109.2 . . ? C35 C36 H36B 109.2 . . ? H36A C36 H36B 107.9 . . ? C36 C37 C38 111.90(18) . . ? C36 C37 H37A 109.2 . . ? C38 C37 H37A 109.2 . . ? C36 C37 H37B 109.2 . . ? C38 C37 H37B 109.2 . . ? H37A C37 H37B 107.9 . . ? C37 C38 C39 109.67(15) . . ? C37 C38 H38A 109.7 . . ? C39 C38 H38A 109.7 . . ? C37 C38 H38B 109.7 . . ? C39 C38 H38B 109.7 . . ? H38A C38 H38B 108.2 . . ? C34 C39 C38 108.74(15) . . ? C34 C39 H39A 109.9 . . ? C38 C39 H39A 109.9 . . ? C34 C39 H39B 109.9 . . ? C38 C39 H39B 109.9 . . ? H39A C39 H39B 108.3 . . ? C34 C39 H39C 157.4 . . ? C38 C39 H39C 87.6 . . ? H39A C39 H39C 48.3 . . ? H39B C39 H39C 77.3 . . ? C34 C39 H39D 106.4 . . ? C38 C39 H39D 110.8 . . ? H39A C39 H39D 111.0 . . ? H39B C39 H39D 3.7 . . ? H39C C39 H39D 81.0 . . ? C41 C40 C45 108.64(13) . . ? C41 C40 P2 113.48(11) . . ? C45 C40 P2 118.65(14) . . ? C41 C40 H40A 104.9 . . ? C45 C40 H40A 104.9 . . ? P2 C40 H40A 104.9 . . ? C40 C41 C42 109.97(14) . . ? C40 C41 H41A 109.7 . . ? C42 C41 H41A 109.7 . . ? C40 C41 H41B 109.7 . . ? C42 C41 H41B 109.7 . . ? H41A C41 H41B 108.2 . . ? C43 C42 C41 110.15(17) . . ? C43 C42 H42A 109.6 . . ? C41 C42 H42A 109.6 . . ? C43 C42 H42B 109.6 . . ? C41 C42 H42B 109.6 . . ? H42A C42 H42B 108.1 . . ? C44 C43 C42 111.58(14) . . ? C44 C43 H43A 109.3 . . ? C42 C43 H43A 109.3 . . ? C44 C43 H43B 109.3 . . ? C42 C43 H43B 109.3 . . ? H43A C43 H43B 108.0 . . ? C43 C44 C45 111.41(15) . . ? C43 C44 H44A 109.3 . . ? C45 C44 H44A 109.3 . . ? C43 C44 H44B 109.3 . . ? C45 C44 H44B 109.3 . . ? H44A C44 H44B 108.0 . . ? C44 C45 C40 109.34(17) . . ? C44 C45 H45A 109.8 . . ? C40 C45 H45A 109.8 . . ? C44 C45 H45B 109.8 . . ? C40 C45 H45B 109.8 . . ? H45A C45 H45B 108.3 . . ? C39' C34' C35' 109.8(2) . . ? C39' C34' P2 117.91(15) . . ? C35' C34' P2 108.03(14) . . ? C39' C34' H34B 106.9 . . ? C35' C34' H34B 106.9 . . ? P2 C34' H34B 106.9 . . ? C36' C35' C34' 110.1(2) . . ? C36' C35' H35C 109.6 . . ? C34' C35' H35C 109.6 . . ? C36' C35' H35D 109.6 . . ? C34' C35' H35D 109.6 . . ? H35C C35' H35D 108.2 . . ? C37' C36' C35' 110.6(2) . . ? C37' C36' H36C 109.5 . . ? C35' C36' H36C 109.5 . . ? C37' C36' H36D 109.5 . . ? C35' C36' H36D 109.5 . . ? H36C C36' H36D 108.1 . . ? C36' C37' C38' 110.5(2) . . ? C36' C37' H37C 109.6 . . ? C38' C37' H37C 109.6 . . ? C36' C37' H37D 109.6 . . ? C38' C37' H37D 109.6 . . ? H37C C37' H37D 108.1 . . ? C37' C38' C39' 110.0(2) . . ? C37' C38' H38C 109.7 . . ? C39' C38' H38C 109.7 . . ? C37' C38' H38D 109.7 . . ? C39' C38' H38D 109.7 . . ? H38C C38' H38D 108.2 . . ? C34' C39' C38' 109.7(2) . . ? C34' C39' H39C 109.9 . . ? C38' C39' H39C 109.7 . . ? C34' C39' H39D 109.6 . . ? C38' C39' H39D 109.7 . . ? H39C C39' H39D 108.2 . . ? C41' C40' C45' 110.51(15) . . ? C41' C40' P2 104.89(14) . . ? C45' C40' P2 110.46(19) . . ? C41' C40' H40B 110.3 . . ? C45' C40' H40B 110.3 . . ? P2 C40' H40B 110.3 . . ? C40' C41' C42' 110.54(16) . . ? C40' C41' H41C 109.5 . . ? C42' C41' H41C 109.5 . . ? C40' C41' H41D 109.5 . . ? C42' C41' H41D 109.5 . . ? H41C C41' H41D 108.1 . . ? C43' C42' C41' 110.16(19) . . ? C43' C42' H42C 109.6 . . ? C41' C42' H42C 109.6 . . ? C43' C42' H42D 109.6 . . ? C41' C42' H42D 109.6 . . ? H42C C42' H42D 108.1 . . ? C44' C43' C42' 109.83(15) . . ? C44' C43' H43C 109.7 . . ? C42' C43' H43C 109.7 . . ? C44' C43' H43D 109.7 . . ? C42' C43' H43D 109.7 . . ? H43C C43' H43D 108.2 . . ? C43' C44' C45' 109.91(16) . . ? C43' C44' H44C 109.7 . . ? C45' C44' H44C 109.7 . . ? C43' C44' H44D 109.7 . . ? C45' C44' H44D 109.7 . . ? H44C C44' H44D 108.2 . . ? C40' C45' C44' 109.94(19) . . ? C40' C45' H45C 109.7 . . ? C44' C45' H45C 109.7 . . ? C40' C45' H45D 109.7 . . ? C44' C45' H45D 109.7 . . ? H45C C45' H45D 108.2 . . ? F4 B1 F2 110.26(16) . . ? F4 B1 F1 109.96(14) . . ? F2 B1 F1 107.82(17) . . ? F4 B1 F3 109.75(16) . . ? F2 B1 F3 110.32(14) . . ? F1 B1 F3 108.68(16) . . ? Cl1 C46 Cl2 110.5(2) . . ? Cl1 C46 H46A 109.5 . . ? Cl2 C46 H46A 109.5 . . ? Cl1 C46 H46B 109.5 . . ? Cl2 C46 H46B 109.5 . . ? H46A C46 H46B 108.1 . . ? Cl4 Cl3 C47 70.0(2) 2 . ? Cl4 Cl3 Cl3 99.6(2) 2 2 ? C47 Cl3 Cl3 46.26(11) . 2 ? Cl3 Cl4 C47 68.91(17) 2 . ? Cl3 C47 Cl3 87.5(2) . 2 ? Cl3 C47 Cl4 41.13(16) . 2 ? Cl3 C47 Cl4 110.9(2) 2 2 ? Cl3 C47 Cl4 110.9(2) . . ? Cl3 C47 Cl4 41.13(16) 2 . ? Cl4 C47 Cl4 148.2(4) 2 . ? Cl3 C47 H47A 110.1 . . ? Cl3 C47 H47A 88.7 2 . ? Cl4 C47 H47A 77.1 2 . ? Cl4 C47 H47A 110.2 . . ? Cl3 C47 H47B 108.7 . . ? Cl3 C47 H47B 149.9 2 . ? Cl4 C47 H47B 97.3 2 . ? Cl4 C47 H47B 108.8 . . ? H47A C47 H47B 108.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 Cu1 Cu2 N5 118.09(6) . . . 7_566 ? N4 Cu1 Cu2 N5 7.24(5) 7_566 . . 7_566 ? P1 Cu1 Cu2 N5 -111.43(4) . . . 7_566 ? N1 Cu1 Cu2 N2 7.84(6) . . . . ? N4 Cu1 Cu2 N2 -103.02(5) 7_566 . . . ? P1 Cu1 Cu2 N2 138.32(4) . . . . ? N1 Cu1 Cu2 P2 -108.12(4) . . . . ? N4 Cu1 Cu2 P2 141.03(4) 7_566 . . . ? P1 Cu1 Cu2 P2 22.370(18) . . . . ? N1 Cu1 P1 C33 65.80(9) . . . . ? N4 Cu1 P1 C33 -110.10(8) 7_566 . . . ? Cu2 Cu1 P1 C33 -27.60(7) . . . . ? N1 Cu1 P1 C21 -53.55(7) . . . . ? N4 Cu1 P1 C21 130.55(6) 7_566 . . . ? Cu2 Cu1 P1 C21 -146.94(5) . . . . ? N1 Cu1 P1 C27 -171.24(7) . . . . ? N4 Cu1 P1 C27 12.86(7) 7_566 . . . ? Cu2 Cu1 P1 C27 95.37(6) . . . . ? N5 Cu2 P2 C33 80.18(9) 7_566 . . . ? N2 Cu2 P2 C33 -97.89(8) . . . . ? Cu1 Cu2 P2 C33 -14.51(7) . . . . ? N5 Cu2 P2 C34 -44.45(8) 7_566 . . . ? N2 Cu2 P2 C34 137.48(7) . . . . ? Cu1 Cu2 P2 C34 -139.14(6) . . . . ? N5 Cu2 P2 C40 -162.48(8) 7_566 . . . ? N2 Cu2 P2 C40 19.45(8) . . . . ? Cu1 Cu2 P2 C40 102.83(7) . . . . ? N5 Cu2 P2 C40' -157.81(8) 7_566 . . . ? N2 Cu2 P2 C40' 24.12(8) . . . . ? Cu1 Cu2 P2 C40' 107.50(7) . . . . ? N5 Cu2 P2 C34' -46.93(11) 7_566 . . . ? N2 Cu2 P2 C34' 135.00(11) . . . . ? Cu1 Cu2 P2 C34' -141.62(10) . . . . ? N4 Cu1 N1 C1 70.68(13) 7_566 . . . ? P1 Cu1 N1 C1 -105.51(13) . . . . ? Cu2 Cu1 N1 C1 -8.18(13) . . . . ? N4 Cu1 N1 C11 -129.47(11) 7_566 . . . ? P1 Cu1 N1 C11 54.34(12) . . . . ? Cu2 Cu1 N1 C11 151.67(11) . . . . ? N5 Cu2 N2 C1 -99.85(14) 7_566 . . . ? P2 Cu2 N2 C1 78.66(13) . . . . ? Cu1 Cu2 N2 C1 -11.30(13) . . . . ? N5 Cu2 N2 C5 88.70(12) 7_566 . . . ? P2 Cu2 N2 C5 -92.79(12) . . . . ? Cu1 Cu2 N2 C5 177.25(12) . . . . ? C5 N2 C1 N1 179.39(15) . . . . ? Cu2 N2 C1 N1 8.6(2) . . . . ? C5 N2 C1 C2 -2.5(2) . . . . ? Cu2 N2 C1 C2 -173.38(12) . . . . ? C11 N1 C1 N2 -156.62(15) . . . . ? Cu1 N1 C1 N2 2.4(2) . . . . ? C11 N1 C1 C2 25.4(2) . . . . ? Cu1 N1 C1 C2 -175.62(13) . . . . ? N2 C1 C2 C3 -1.9(3) . . . . ? N1 C1 C2 C3 176.12(18) . . . . ? C1 C2 C3 C4 4.6(3) . . . . ? C2 C3 C4 C5 -3.1(3) . . . . ? C2 C3 C4 C8 176.6(2) . . . . ? C6 N3 C5 N2 177.37(18) . . . . ? C6 N3 C5 C4 1.4(3) . . . . ? C1 N2 C5 N3 -171.86(16) . . . . ? Cu2 N2 C5 N3 0.23(19) . . . . ? C1 N2 C5 C4 4.2(3) . . . . ? Cu2 N2 C5 C4 176.25(14) . . . . ? C3 C4 C5 N3 174.31(19) . . . . ? C8 C4 C5 N3 -5.4(3) . . . . ? C3 C4 C5 N2 -1.4(3) . . . . ? C8 C4 C5 N2 178.96(18) . . . . ? C5 N3 C6 C7 4.7(3) . . . . ? C5 N3 C6 C9 -176.5(2) . . . . ? N3 C6 C7 C8 -6.9(4) . . . . ? C9 C6 C7 C8 174.3(2) . . . . ? C6 C7 C8 C10 -175.7(3) . . . . ? C6 C7 C8 C4 2.6(4) . . . . ? C3 C4 C8 C7 -176.5(2) . . . . ? C5 C4 C8 C7 3.2(3) . . . . ? C3 C4 C8 C10 1.9(4) . . . . ? C5 C4 C8 C10 -178.5(2) . . . . ? C15 N4 C11 N1 -174.73(15) . . . . ? Cu1 N4 C11 N1 17.30(18) 7_566 . . . ? C15 N4 C11 C12 1.4(3) . . . . ? Cu1 N4 C11 C12 -166.60(15) 7_566 . . . ? C1 N1 C11 N4 -137.36(16) . . . . ? Cu1 N1 C11 N4 61.90(18) . . . . ? C1 N1 C11 C12 46.7(3) . . . . ? Cu1 N1 C11 C12 -114.05(17) . . . . ? N4 C11 C12 C13 -2.1(3) . . . . ? N1 C11 C12 C13 173.70(19) . . . . ? C11 C12 C13 C14 1.4(3) . . . . ? C12 C13 C14 C18 -178.8(2) . . . . ? C12 C13 C14 C15 0.0(3) . . . . ? C11 N4 C15 N5 -177.41(15) . . . . ? Cu1 N4 C15 N5 -12.9(2) 7_566 . . . ? C11 N4 C15 C14 0.1(3) . . . . ? Cu1 N4 C15 C14 164.56(13) 7_566 . . . ? C16 N5 C15 N4 -179.13(15) . . . . ? Cu2 N5 C15 N4 1.8(2) 7_566 . . . ? C16 N5 C15 C14 3.4(3) . . . . ? Cu2 N5 C15 C14 -175.61(14) 7_566 . . . ? C13 C14 C15 N4 -0.8(3) . . . . ? C18 C14 C15 N4 178.07(18) . . . . ? C13 C14 C15 N5 176.49(18) . . . . ? C18 C14 C15 N5 -4.7(3) . . . . ? C15 N5 C16 C17 0.4(3) . . . . ? Cu2 N5 C16 C17 179.46(14) 7_566 . . . ? C15 N5 C16 C19 -179.32(16) . . . . ? Cu2 N5 C16 C19 -0.3(2) 7_566 . . . ? N5 C16 C17 C18 -3.1(3) . . . . ? C19 C16 C17 C18 176.6(2) . . . . ? C16 C17 C18 C14 1.8(3) . . . . ? C16 C17 C18 C20 -176.2(2) . . . . ? C13 C14 C18 C17 -179.4(2) . . . . ? C15 C14 C18 C17 1.9(3) . . . . ? C13 C14 C18 C20 -1.4(3) . . . . ? C15 C14 C18 C20 179.9(2) . . . . ? C33 P1 C21 C26 -60.18(12) . . . . ? C27 P1 C21 C26 -171.19(10) . . . . ? Cu1 P1 C21 C26 62.62(11) . . . . ? C33 P1 C21 C22 176.10(11) . . . . ? C27 P1 C21 C22 65.09(11) . . . . ? Cu1 P1 C21 C22 -61.10(11) . . . . ? C26 C21 C22 C23 58.09(18) . . . . ? P1 C21 C22 C23 -177.12(10) . . . . ? C21 C22 C23 C24 -56.79(18) . . . . ? C22 C23 C24 C25 57.3(2) . . . . ? C23 C24 C25 C26 -57.7(2) . . . . ? C22 C21 C26 C25 -58.51(17) . . . . ? P1 C21 C26 C25 178.95(10) . . . . ? C24 C25 C26 C21 57.63(17) . . . . ? C33 P1 C27 C28 83.87(12) . . . . ? C21 P1 C27 C28 -167.01(10) . . . . ? Cu1 P1 C27 C28 -41.15(12) . . . . ? C33 P1 C27 C32 -46.69(14) . . . . ? C21 P1 C27 C32 62.42(12) . . . . ? Cu1 P1 C27 C32 -171.72(9) . . . . ? C32 C27 C28 C29 -55.84(15) . . . . ? P1 C27 C28 C29 171.18(10) . . . . ? C27 C28 C29 C30 56.70(18) . . . . ? C28 C29 C30 C31 -57.03(17) . . . . ? C29 C30 C31 C32 57.93(17) . . . . ? C30 C31 C32 C27 -57.67(18) . . . . ? C28 C27 C32 C31 56.16(16) . . . . ? P1 C27 C32 C31 -171.42(11) . . . . ? C34 P2 C33 P1 131.75(10) . . . . ? C40 P2 C33 P1 -122.19(10) . . . . ? C40' P2 C33 P1 -132.35(10) . . . . ? C34' P2 C33 P1 121.45(10) . . . . ? Cu2 P2 C33 P1 -2.05(12) . . . . ? C21 P1 C33 P2 147.76(9) . . . . ? C27 P1 C33 P2 -106.14(10) . . . . ? Cu1 P1 C33 P2 21.96(11) . . . . ? C33 P2 C34 C39 -71.28(16) . . . . ? C40 P2 C34 C39 -178.94(15) . . . . ? C40' P2 C34 C39 -174.42(16) . . . . ? C34' P2 C34 C39 68.9(4) . . . . ? Cu2 P2 C34 C39 59.52(15) . . . . ? C33 P2 C34 C35 167.57(16) . . . . ? C40 P2 C34 C35 59.92(18) . . . . ? C40' P2 C34 C35 64.44(18) . . . . ? C34' P2 C34 C35 -52.3(4) . . . . ? Cu2 P2 C34 C35 -61.62(17) . . . . ? C39 C34 C35 C36 59.0(3) . . . . ? P2 C34 C35 C36 -179.76(17) . . . . ? C34 C35 C36 C37 -54.8(3) . . . . ? C35 C36 C37 C38 54.0(3) . . . . ? C36 C37 C38 C39 -56.3(3) . . . . ? C35 C34 C39 C38 -62.0(2) . . . . ? P2 C34 C39 C38 175.40(15) . . . . ? C37 C38 C39 C34 60.3(3) . . . . ? C33 P2 C40 C41 64.66(17) . . . . ? C34 P2 C40 C41 170.83(16) . . . . ? C40' P2 C40 C41 144.2(6) . . . . ? C34' P2 C40 C41 -174.80(17) . . . . ? Cu2 P2 C40 C41 -59.88(17) . . . . ? C33 P2 C40 C45 -64.70(16) . . . . ? C34 P2 C40 C45 41.47(17) . . . . ? C40' P2 C40 C45 14.8(5) . . . . ? C34' P2 C40 C45 55.84(19) . . . . ? Cu2 P2 C40 C45 170.76(13) . . . . ? C45 C40 C41 C42 -61.6(2) . . . . ? P2 C40 C41 C42 164.15(15) . . . . ? C40 C41 C42 C43 58.6(2) . . . . ? C41 C42 C43 C44 -55.0(3) . . . . ? C42 C43 C44 C45 55.1(3) . . . . ? C43 C44 C45 C40 -57.7(2) . . . . ? C41 C40 C45 C44 60.6(2) . . . . ? P2 C40 C45 C44 -167.86(13) . . . . ? C33 P2 C34' C39' -69.9(3) . . . . ? C34 P2 C34' C39' -112.9(6) . . . . ? C40 P2 C34' C39' 175.6(3) . . . . ? C40' P2 C34' C39' -177.7(3) . . . . ? Cu2 P2 C34' C39' 58.7(3) . . . . ? C33 P2 C34' C35' 55.2(2) . . . . ? C34 P2 C34' C35' 12.1(3) . . . . ? C40 P2 C34' C35' -59.3(2) . . . . ? C40' P2 C34' C35' -52.6(2) . . . . ? Cu2 P2 C34' C35' -176.2(2) . . . . ? C39' C34' C35' C36' -58.7(4) . . . . ? P2 C34' C35' C36' 171.5(2) . . . . ? C34' C35' C36' C37' 57.8(4) . . . . ? C35' C36' C37' C38' -57.6(4) . . . . ? C36' C37' C38' C39' 58.1(4) . . . . ? C35' C34' C39' C38' 59.4(4) . . . . ? P2 C34' C39' C38' -176.4(3) . . . . ? C37' C38' C39' C34' -59.1(4) . . . . ? C33 P2 C40' C41' 63.59(18) . . . . ? C34 P2 C40' C41' 166.83(17) . . . . ? C40 P2 C40' C41' -39.2(5) . . . . ? C34' P2 C40' C41' -179.76(18) . . . . ? Cu2 P2 C40' C41' -65.17(18) . . . . ? C33 P2 C40' C45' -177.32(14) . . . . ? C34 P2 C40' C45' -74.08(15) . . . . ? C40 P2 C40' C45' 79.9(6) . . . . ? C34' P2 C40' C45' -60.67(17) . . . . ? Cu2 P2 C40' C45' 53.92(14) . . . . ? C45' C40' C41' C42' 57.5(3) . . . . ? P2 C40' C41' C42' 176.57(17) . . . . ? C40' C41' C42' C43' -57.6(3) . . . . ? C41' C42' C43' C44' 58.5(3) . . . . ? C42' C43' C44' C45' -59.2(3) . . . . ? C41' C40' C45' C44' -58.0(3) . . . . ? P2 C40' C45' C44' -173.67(13) . . . . ? C43' C44' C45' C40' 58.9(2) . . . . ? Cl4 Cl3 C47 Cl3 126.5(2) 2 . . 2 ? Cl3 Cl3 C47 Cl4 -126.5(2) 2 . . 2 ? Cl4 Cl3 C47 Cl4 161.0(2) 2 . . . ? Cl3 Cl3 C47 Cl4 34.50(16) 2 . . . ? Cl3 Cl4 C47 Cl3 -59.4(3) 2 . . . ? Cl3 Cl4 C47 Cl4 -35.32(19) 2 . . 2 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.948 _refine_diff_density_min -0.532 _refine_diff_density_rms 0.165 #===END data_061008c_Complex2 _database_code_depnum_ccdc_archive 'CCDC 793443' #TrackingRef '- copper.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C92 H84 B2 Cl4 Cu4 F8 N10 P4' _chemical_formula_weight 2023.15 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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.238(2) _cell_length_b 18.531(3) _cell_length_c 20.929(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.246(3) _cell_angle_gamma 90.00 _cell_volume 4620.2(12) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4939 _cell_measurement_theta_min 2.282 _cell_measurement_theta_max 22.515 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.21 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2064 _exptl_absorpt_coefficient_mu 1.160 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7927 _exptl_absorpt_correction_T_max 0.8544 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 23854 _diffrn_reflns_av_R_equivalents 0.0452 _diffrn_reflns_av_sigmaI/netI 0.0587 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8143 _reflns_number_gt 4991 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0644P)^2^+5.1734P] 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 8143 _refine_ls_number_parameters 559 _refine_ls_number_restraints 99 _refine_ls_R_factor_all 0.1001 _refine_ls_R_factor_gt 0.0477 _refine_ls_wR_factor_ref 0.1526 _refine_ls_wR_factor_gt 0.1142 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.077 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.54065(5) 0.63331(3) 0.63302(3) 0.04066(19) Uani 1 1 d . . . Cu2 Cu 0.50289(5) 0.57379(3) 0.51696(3) 0.03825(18) Uani 1 1 d . . . B1 B 0.9557(9) 0.6805(7) 0.4770(6) 0.101(3) Uani 1 1 d U . . Cl1 Cl 0.8965(4) 0.9284(3) 0.52690(18) 0.254(3) Uani 1 1 d DU . . Cl2 Cl 0.9120(3) 0.8587(3) 0.65107(17) 0.2076(18) Uani 1 1 d DU . . F1 F 1.0370(4) 0.6401(3) 0.5131(3) 0.1251(17) Uani 1 1 d U . . F2 F 0.9214(6) 0.6451(4) 0.4177(3) 0.181(3) Uani 1 1 d U . . F3 F 0.8703(5) 0.6855(3) 0.5052(3) 0.168(3) Uani 1 1 d U . . F4 F 0.9975(6) 0.7440(3) 0.4662(4) 0.184(3) Uani 1 1 d U . . N1 N 0.4499(3) 0.5492(2) 0.65513(19) 0.0408(10) Uani 1 1 d . . . N2 N 0.5157(4) 0.5922(3) 0.7593(2) 0.0584(13) Uani 1 1 d . . . N3 N 0.3922(3) 0.5096(2) 0.54879(18) 0.0385(10) Uani 1 1 d . . . N4 N 0.6656(3) 0.5528(2) 0.54711(18) 0.0363(9) Uani 1 1 d . . . N5 N 0.7064(3) 0.6194(2) 0.64252(19) 0.0411(10) Uani 1 1 d . . . P1 P 0.42204(11) 0.72276(7) 0.59783(6) 0.0418(3) Uani 1 1 d . . . P2 P 0.41053(11) 0.66448(7) 0.46228(6) 0.0423(3) Uani 1 1 d . . . C1 C 0.4444(4) 0.5467(3) 0.7200(2) 0.0462(13) Uani 1 1 d . . . C2 C 0.5105(6) 0.5948(4) 0.8215(3) 0.0744(19) Uani 1 1 d . . . C3 C 0.4358(6) 0.5539(4) 0.8472(3) 0.082(2) Uani 1 1 d . . . H3 H 0.4341 0.5593 0.8912 0.099 Uiso 1 1 calc R . . C4 C 0.3651(6) 0.5063(4) 0.8093(3) 0.0686(18) Uani 1 1 d . . . C5 C 0.3689(5) 0.5013(3) 0.7422(3) 0.0506(14) Uani 1 1 d . . . C6 C 0.3022(5) 0.4546(3) 0.6960(3) 0.0535(14) Uani 1 1 d . . . H6 H 0.2541 0.4221 0.7096 0.064 Uiso 1 1 calc R . . C7 C 0.3075(4) 0.4564(3) 0.6324(3) 0.0481(13) Uani 1 1 d . . . H7 H 0.2629 0.4257 0.6021 0.058 Uiso 1 1 calc R . . C8 C 0.3820(4) 0.5060(3) 0.6117(2) 0.0405(12) Uani 1 1 d . . . C9 C 0.5904(8) 0.6454(5) 0.8662(3) 0.120(3) Uani 1 1 d . . . H9A H 0.6641 0.6245 0.8769 0.180 Uiso 1 1 calc R . . H9B H 0.5649 0.6531 0.9058 0.180 Uiso 1 1 calc R . . H9C H 0.5928 0.6907 0.8444 0.180 Uiso 1 1 calc R . . C10 C 0.2862(7) 0.4601(5) 0.8366(3) 0.100(3) Uani 1 1 d . . . H10A H 0.2961 0.4696 0.8827 0.149 Uiso 1 1 calc R . . H10B H 0.3017 0.4101 0.8303 0.149 Uiso 1 1 calc R . . H10C H 0.2102 0.4708 0.8144 0.149 Uiso 1 1 calc R . . C11 C 0.7445(4) 0.5758(3) 0.5999(2) 0.0365(11) Uani 1 1 d . . . C12 C 0.7827(5) 0.6473(3) 0.6930(2) 0.0508(14) Uani 1 1 d . . . C13 C 0.8956(5) 0.6285(4) 0.7051(3) 0.0610(16) Uani 1 1 d . . . H13 H 0.9453 0.6482 0.7413 0.073 Uiso 1 1 calc R . . C14 C 0.9353(4) 0.5818(3) 0.6652(3) 0.0559(15) Uani 1 1 d . . . C15 C 0.8577(4) 0.5553(3) 0.6090(2) 0.0447(13) Uani 1 1 d . . . C16 C 0.8866(4) 0.5114(3) 0.5607(3) 0.0520(14) Uani 1 1 d . . . H16 H 0.9603 0.4957 0.5661 0.062 Uiso 1 1 calc R . . C17 C 0.8090(4) 0.4916(3) 0.5066(3) 0.0498(14) Uani 1 1 d . . . H17 H 0.8292 0.4645 0.4737 0.060 Uiso 1 1 calc R . . C18 C 0.6952(4) 0.5131(3) 0.5011(2) 0.0404(12) Uani 1 1 d . . . C19 C 0.7414(5) 0.6997(4) 0.7359(3) 0.0699(18) Uani 1 1 d . . . H19A H 0.7133 0.7420 0.7110 0.105 Uiso 1 1 calc R . . H19B H 0.8019 0.7129 0.7719 0.105 Uiso 1 1 calc R . . H19C H 0.6822 0.6780 0.7525 0.105 Uiso 1 1 calc R . . C20 C 1.0578(5) 0.5597(4) 0.6785(3) 0.085(2) Uani 1 1 d . . . H20A H 1.0983 0.5827 0.7180 0.128 Uiso 1 1 calc R . . H20B H 1.0889 0.5742 0.6424 0.128 Uiso 1 1 calc R . . H20C H 1.0636 0.5083 0.6837 0.128 Uiso 1 1 calc R . . C21 C 0.3294(4) 0.7054(3) 0.5166(2) 0.0467(13) Uani 1 1 d . . . H21A H 0.2693 0.6731 0.5212 0.056 Uiso 1 1 calc R . . H21B H 0.2962 0.7503 0.4977 0.056 Uiso 1 1 calc R . . C22 C 0.3270(4) 0.7371(3) 0.6518(2) 0.0472(13) Uani 1 1 d . . . C23 C 0.3747(6) 0.7519(4) 0.7171(3) 0.0689(18) Uani 1 1 d . . . H23 H 0.4524 0.7556 0.7307 0.083 Uiso 1 1 calc R . . C24 C 0.3101(7) 0.7613(4) 0.7626(3) 0.084(2) Uani 1 1 d . . . H24 H 0.3442 0.7712 0.8062 0.101 Uiso 1 1 calc R . . C25 C 0.1969(7) 0.7562(4) 0.7434(4) 0.088(2) Uani 1 1 d . . . H25 H 0.1525 0.7630 0.7735 0.106 Uiso 1 1 calc R . . C26 C 0.1490(6) 0.7408(4) 0.6796(4) 0.093(2) Uani 1 1 d . . . H26 H 0.0713 0.7366 0.6665 0.112 Uiso 1 1 calc R . . C27 C 0.2135(5) 0.7312(4) 0.6338(3) 0.0718(19) Uani 1 1 d . . . H27 H 0.1788 0.7207 0.5904 0.086 Uiso 1 1 calc R . . C28 C 0.4716(5) 0.8138(3) 0.5886(3) 0.0520(14) Uani 1 1 d . . . C29 C 0.5828(6) 0.8250(4) 0.5900(3) 0.0724(18) Uani 1 1 d . . . H29 H 0.6327 0.7864 0.5962 0.087 Uiso 1 1 calc R . . C30 C 0.6209(8) 0.8954(5) 0.5821(4) 0.101(3) Uani 1 1 d . . . H30 H 0.6963 0.9033 0.5830 0.121 Uiso 1 1 calc R . . C31 C 0.5490(11) 0.9512(5) 0.5731(4) 0.111(3) Uani 1 1 d . . . H31 H 0.5751 0.9976 0.5686 0.134 Uiso 1 1 calc R . . C32 C 0.4397(10) 0.9403(4) 0.5707(4) 0.112(3) Uani 1 1 d . . . H32 H 0.3899 0.9790 0.5635 0.134 Uiso 1 1 calc R . . C33 C 0.4014(7) 0.8720(3) 0.5787(4) 0.087(2) Uani 1 1 d . . . H33 H 0.3256 0.8653 0.5775 0.104 Uiso 1 1 calc R . . C34 C 0.4881(5) 0.7385(3) 0.4360(2) 0.0445(13) Uani 1 1 d . . . C35 C 0.6017(5) 0.7313(3) 0.4413(3) 0.0597(16) Uani 1 1 d . . . H35 H 0.6381 0.6897 0.4597 0.072 Uiso 1 1 calc R . . C36 C 0.6622(6) 0.7851(4) 0.4195(3) 0.0761(19) Uani 1 1 d . . . H36 H 0.7389 0.7796 0.4229 0.091 Uiso 1 1 calc R . . C37 C 0.6083(8) 0.8467(4) 0.3927(3) 0.083(2) Uani 1 1 d . . . H37 H 0.6488 0.8831 0.3779 0.100 Uiso 1 1 calc R . . C38 C 0.4968(7) 0.8550(4) 0.3878(3) 0.076(2) Uani 1 1 d . . . H38 H 0.4615 0.8973 0.3701 0.091 Uiso 1 1 calc R . . C39 C 0.4346(5) 0.8010(3) 0.4088(3) 0.0608(16) Uani 1 1 d . . . H39 H 0.3578 0.8067 0.4047 0.073 Uiso 1 1 calc R . . C40 C 0.3061(5) 0.6410(3) 0.3878(2) 0.0465(13) Uani 1 1 d . . . C41 C 0.3459(6) 0.6025(4) 0.3406(3) 0.0708(18) Uani 1 1 d . . . H41 H 0.4217 0.5913 0.3475 0.085 Uiso 1 1 calc R . . C42 C 0.2707(7) 0.5809(4) 0.2825(3) 0.090(2) Uani 1 1 d . . . H42 H 0.2968 0.5557 0.2506 0.108 Uiso 1 1 calc R . . C43 C 0.1581(7) 0.5971(4) 0.2729(3) 0.082(2) Uani 1 1 d . . . H43 H 0.1082 0.5835 0.2342 0.099 Uiso 1 1 calc R . . C44 C 0.1202(6) 0.6330(4) 0.3200(3) 0.078(2) Uani 1 1 d . . . H44 H 0.0440 0.6427 0.3140 0.093 Uiso 1 1 calc R . . C45 C 0.1939(5) 0.6553(3) 0.3770(3) 0.0612(16) Uani 1 1 d . . . H45 H 0.1666 0.6805 0.4085 0.073 Uiso 1 1 calc R . . C46 C 0.9237(12) 0.8489(7) 0.5721(5) 0.198(5) Uani 1 1 d DU . . H46A H 0.8716 0.8120 0.5510 0.237 Uiso 1 1 calc R . . H46B H 0.9990 0.8326 0.5721 0.237 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0451(4) 0.0391(4) 0.0376(3) -0.0035(3) 0.0091(3) -0.0002(3) Cu2 0.0403(4) 0.0369(3) 0.0376(3) -0.0019(3) 0.0088(3) 0.0013(3) B1 0.084(6) 0.116(8) 0.118(7) 0.023(7) 0.052(6) 0.009(6) Cl1 0.304(5) 0.350(6) 0.125(3) -0.018(3) 0.082(3) -0.150(5) Cl2 0.173(3) 0.319(5) 0.139(3) 0.014(3) 0.052(2) 0.061(3) F1 0.087(3) 0.138(4) 0.140(4) -0.014(3) 0.003(3) 0.030(3) F2 0.157(5) 0.255(8) 0.113(4) -0.002(5) -0.009(4) -0.057(5) F3 0.132(4) 0.166(5) 0.244(6) 0.092(5) 0.118(4) 0.069(4) F4 0.232(7) 0.123(5) 0.232(6) 0.029(5) 0.128(6) -0.038(5) N1 0.051(3) 0.038(2) 0.036(2) 0.0007(19) 0.0155(19) -0.001(2) N2 0.074(3) 0.055(3) 0.049(3) -0.011(2) 0.019(2) -0.015(3) N3 0.040(2) 0.042(2) 0.035(2) -0.0057(19) 0.0106(19) -0.0047(19) N4 0.039(2) 0.035(2) 0.037(2) 0.0018(18) 0.0121(18) 0.0009(18) N5 0.043(2) 0.043(3) 0.037(2) 0.000(2) 0.0088(19) 0.001(2) P1 0.0475(8) 0.0380(8) 0.0401(7) -0.0033(6) 0.0104(6) 0.0027(6) P2 0.0473(8) 0.0419(8) 0.0367(7) 0.0008(6) 0.0075(6) 0.0074(6) C1 0.055(3) 0.041(3) 0.045(3) 0.003(3) 0.016(3) 0.005(3) C2 0.094(5) 0.083(5) 0.049(4) -0.009(3) 0.021(4) -0.016(4) C3 0.115(6) 0.094(6) 0.043(4) -0.008(4) 0.028(4) -0.015(5) C4 0.084(5) 0.076(5) 0.053(4) 0.007(3) 0.032(3) -0.007(4) C5 0.058(4) 0.051(3) 0.048(3) 0.002(3) 0.023(3) -0.001(3) C6 0.055(3) 0.052(3) 0.059(4) 0.008(3) 0.025(3) -0.009(3) C7 0.050(3) 0.045(3) 0.051(3) -0.001(3) 0.016(3) -0.006(3) C8 0.043(3) 0.038(3) 0.044(3) 0.000(2) 0.017(2) 0.004(2) C9 0.167(9) 0.142(8) 0.054(4) -0.039(5) 0.032(5) -0.067(7) C10 0.127(7) 0.121(7) 0.064(4) 0.008(4) 0.051(4) -0.036(6) C11 0.041(3) 0.035(3) 0.033(3) 0.005(2) 0.006(2) -0.001(2) C12 0.049(3) 0.059(4) 0.043(3) -0.003(3) 0.009(3) -0.007(3) C13 0.047(4) 0.087(5) 0.045(3) -0.005(3) 0.001(3) -0.007(3) C14 0.039(3) 0.074(4) 0.051(3) 0.005(3) 0.002(3) -0.005(3) C15 0.037(3) 0.053(3) 0.044(3) 0.006(3) 0.010(2) 0.002(2) C16 0.035(3) 0.057(4) 0.065(4) 0.006(3) 0.013(3) 0.004(3) C17 0.047(3) 0.043(3) 0.063(4) 0.000(3) 0.020(3) 0.003(3) C18 0.046(3) 0.034(3) 0.044(3) 0.003(2) 0.016(2) -0.003(2) C19 0.064(4) 0.087(5) 0.057(4) -0.022(3) 0.008(3) -0.004(4) C20 0.042(4) 0.118(6) 0.087(5) -0.008(5) -0.005(3) 0.008(4) C21 0.046(3) 0.049(3) 0.044(3) 0.002(3) 0.007(2) 0.007(3) C22 0.052(3) 0.044(3) 0.047(3) -0.003(3) 0.014(3) 0.000(3) C23 0.073(4) 0.085(5) 0.048(3) -0.012(3) 0.014(3) 0.008(4) C24 0.098(6) 0.110(6) 0.047(4) -0.006(4) 0.024(4) 0.010(5) C25 0.101(6) 0.097(6) 0.083(5) 0.001(4) 0.056(5) -0.001(5) C26 0.064(5) 0.130(7) 0.096(6) -0.014(5) 0.042(4) -0.014(5) C27 0.058(4) 0.100(5) 0.061(4) -0.015(4) 0.021(3) -0.007(4) C28 0.074(4) 0.040(3) 0.046(3) -0.007(3) 0.022(3) -0.002(3) C29 0.081(5) 0.068(5) 0.069(4) 0.004(4) 0.018(4) -0.011(4) C30 0.103(7) 0.101(7) 0.101(6) -0.004(5) 0.027(5) -0.048(6) C31 0.195(11) 0.053(5) 0.106(6) -0.012(5) 0.076(7) -0.023(7) C32 0.168(9) 0.057(5) 0.139(8) 0.010(5) 0.094(7) 0.022(6) C33 0.118(6) 0.042(4) 0.124(6) 0.007(4) 0.074(5) 0.015(4) C34 0.063(4) 0.036(3) 0.033(3) -0.002(2) 0.009(2) 0.005(3) C35 0.070(4) 0.054(4) 0.059(4) 0.006(3) 0.023(3) 0.009(3) C36 0.076(5) 0.074(5) 0.083(5) 0.005(4) 0.028(4) -0.011(4) C37 0.115(7) 0.065(5) 0.075(5) 0.002(4) 0.033(5) -0.027(5) C38 0.119(6) 0.049(4) 0.055(4) 0.010(3) 0.012(4) 0.001(4) C39 0.071(4) 0.055(4) 0.054(3) 0.004(3) 0.007(3) 0.010(3) C40 0.056(3) 0.043(3) 0.038(3) 0.005(2) 0.006(2) 0.004(3) C41 0.074(4) 0.084(5) 0.050(4) -0.014(3) 0.005(3) 0.013(4) C42 0.114(7) 0.101(6) 0.047(4) -0.016(4) 0.004(4) -0.001(5) C43 0.096(6) 0.090(5) 0.045(4) 0.010(4) -0.017(4) -0.016(5) C44 0.071(5) 0.090(5) 0.061(4) 0.013(4) -0.007(4) -0.002(4) C45 0.064(4) 0.069(4) 0.047(3) 0.001(3) 0.005(3) 0.003(3) C46 0.209(10) 0.253(11) 0.152(9) 0.018(9) 0.085(8) 0.038(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N5 2.009(4) . ? Cu1 N1 2.029(4) . ? Cu1 P1 2.2152(15) . ? Cu1 Cu2 2.6107(9) . ? Cu2 N4 1.985(4) . ? Cu2 N3 2.027(4) . ? Cu2 P2 2.1953(15) . ? Cu2 Cu2 2.8223(12) 3_666 ? B1 F3 1.315(10) . ? B1 F4 1.323(12) . ? B1 F1 1.334(11) . ? B1 F2 1.381(13) . ? Cl1 C46 1.741(11) . ? Cl2 C46 1.700(10) . ? N1 C8 1.345(6) . ? N1 C1 1.375(6) . ? N2 C2 1.319(7) . ? N2 C1 1.350(7) . ? N3 C8 1.353(6) . ? N3 C18 1.378(6) 3_666 ? N4 C18 1.327(6) . ? N4 C11 1.358(6) . ? N5 C12 1.343(6) . ? N5 C11 1.362(6) . ? P1 C22 1.818(5) . ? P1 C28 1.818(6) . ? P1 C21 1.842(5) . ? P2 C34 1.823(5) . ? P2 C40 1.827(5) . ? P2 C21 1.836(5) . ? C1 C5 1.405(7) . ? C2 C3 1.386(9) . ? C2 C9 1.514(9) . ? C3 C4 1.358(9) . ? C3 H3 0.9300 . ? C4 C5 1.419(8) . ? C4 C10 1.499(8) . ? C5 C6 1.409(7) . ? C6 C7 1.349(7) . ? C6 H6 0.9300 . ? C7 C8 1.429(7) . ? C7 H7 0.9300 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C15 1.407(7) . ? C12 C13 1.390(8) . ? C12 C19 1.487(8) . ? C13 C14 1.368(8) . ? C13 H13 0.9300 . ? C14 C15 1.419(7) . ? C14 C20 1.517(8) . ? C15 C16 1.404(7) . ? C16 C17 1.352(7) . ? C16 H16 0.9300 . ? C17 C18 1.427(7) . ? C17 H17 0.9300 . ? C18 N3 1.378(6) 3_666 ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 C27 1.358(8) . ? C22 C23 1.385(7) . ? C23 C24 1.380(8) . ? C23 H23 0.9300 . ? C24 C25 1.355(10) . ? C24 H24 0.9300 . ? C25 C26 1.359(10) . ? C25 H25 0.9300 . ? C26 C27 1.387(8) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C33 1.365(8) . ? C28 C29 1.370(8) . ? C29 C30 1.408(10) . ? C29 H29 0.9300 . ? C30 C31 1.342(12) . ? C30 H30 0.9300 . ? C31 C32 1.343(12) . ? C31 H31 0.9300 . ? C32 C33 1.373(10) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C35 1.376(7) . ? C34 C39 1.386(7) . ? C35 C36 1.380(8) . ? C35 H35 0.9300 . ? C36 C37 1.373(9) . ? C36 H36 0.9300 . ? C37 C38 1.353(10) . ? C37 H37 0.9300 . ? C38 C39 1.390(9) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 C45 1.366(8) . ? C40 C41 1.393(8) . ? C41 C42 1.405(9) . ? C41 H41 0.9300 . ? C42 C43 1.381(10) . ? C42 H42 0.9300 . ? C43 C44 1.356(10) . ? C43 H43 0.9300 . ? C44 C45 1.383(8) . ? C44 H44 0.9300 . ? C45 H45 0.9300 . ? C46 H46A 0.9700 . ? C46 H46B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Cu1 N1 118.15(16) . . ? N5 Cu1 P1 134.34(12) . . ? N1 Cu1 P1 107.44(12) . . ? N5 Cu1 Cu2 89.84(11) . . ? N1 Cu1 Cu2 84.14(11) . . ? P1 Cu1 Cu2 92.52(4) . . ? N4 Cu2 N3 118.58(16) . . ? N4 Cu2 P2 132.44(12) . . ? N3 Cu2 P2 108.51(12) . . ? N4 Cu2 Cu1 80.58(11) . . ? N3 Cu2 Cu1 86.07(11) . . ? P2 Cu2 Cu1 96.99(4) . . ? N4 Cu2 Cu2 81.70(11) . 3_666 ? N3 Cu2 Cu2 62.22(11) . 3_666 ? P2 Cu2 Cu2 129.09(5) . 3_666 ? Cu1 Cu2 Cu2 129.23(4) . 3_666 ? F3 B1 F4 113.0(10) . . ? F3 B1 F1 110.6(9) . . ? F4 B1 F1 109.1(10) . . ? F3 B1 F2 109.1(10) . . ? F4 B1 F2 108.7(9) . . ? F1 B1 F2 106.1(9) . . ? C8 N1 C1 119.0(4) . . ? C8 N1 Cu1 126.1(3) . . ? C1 N1 Cu1 113.8(3) . . ? C2 N2 C1 117.0(5) . . ? C8 N3 C18 119.6(4) . 3_666 ? C8 N3 Cu2 124.5(3) . . ? C18 N3 Cu2 113.0(3) 3_666 . ? C18 N4 C11 120.2(4) . . ? C18 N4 Cu2 107.4(3) . . ? C11 N4 Cu2 132.2(3) . . ? C12 N5 C11 117.6(4) . . ? C12 N5 Cu1 122.2(3) . . ? C11 N5 Cu1 120.0(3) . . ? C22 P1 C28 101.9(2) . . ? C22 P1 C21 104.7(2) . . ? C28 P1 C21 102.4(3) . . ? C22 P1 Cu1 111.53(18) . . ? C28 P1 Cu1 121.4(2) . . ? C21 P1 Cu1 113.17(17) . . ? C34 P2 C40 103.5(2) . . ? C34 P2 C21 105.6(2) . . ? C40 P2 C21 104.8(2) . . ? C34 P2 Cu2 119.46(18) . . ? C40 P2 Cu2 115.98(18) . . ? C21 P2 Cu2 106.25(17) . . ? N2 C1 N1 114.2(5) . . ? N2 C1 C5 123.7(5) . . ? N1 C1 C5 122.0(5) . . ? N2 C2 C3 123.3(6) . . ? N2 C2 C9 117.5(6) . . ? C3 C2 C9 119.3(6) . . ? C4 C3 C2 121.1(6) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 117.4(6) . . ? C3 C4 C10 121.9(6) . . ? C5 C4 C10 120.6(6) . . ? C1 C5 C6 117.6(5) . . ? C1 C5 C4 117.4(5) . . ? C6 C5 C4 125.0(5) . . ? C7 C6 C5 120.7(5) . . ? C7 C6 H6 119.7 . . ? C5 C6 H6 119.7 . . ? C6 C7 C8 119.6(5) . . ? C6 C7 H7 120.2 . . ? C8 C7 H7 120.2 . . ? N1 C8 N3 116.6(4) . . ? N1 C8 C7 121.1(4) . . ? N3 C8 C7 122.2(5) . . ? C2 C9 H9A 109.5 . . ? C2 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C2 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C4 C10 H10A 109.5 . . ? C4 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C4 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N4 C11 N5 115.6(4) . . ? N4 C11 C15 121.3(4) . . ? N5 C11 C15 123.0(4) . . ? N5 C12 C13 122.0(5) . . ? N5 C12 C19 117.1(5) . . ? C13 C12 C19 120.9(5) . . ? C14 C13 C12 121.6(5) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C13 C14 C15 117.5(5) . . ? C13 C14 C20 122.2(5) . . ? C15 C14 C20 120.3(5) . . ? C16 C15 C11 117.5(5) . . ? C16 C15 C14 124.5(5) . . ? C11 C15 C14 118.0(5) . . ? C17 C16 C15 121.1(5) . . ? C17 C16 H16 119.5 . . ? C15 C16 H16 119.5 . . ? C16 C17 C18 118.5(5) . . ? C16 C17 H17 120.8 . . ? C18 C17 H17 120.8 . . ? N4 C18 N3 115.2(4) . 3_666 ? N4 C18 C17 121.3(5) . . ? N3 C18 C17 123.3(5) 3_666 . ? C12 C19 H19A 109.5 . . ? C12 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C12 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C14 C20 H20A 109.5 . . ? C14 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C14 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? P2 C21 P1 109.8(3) . . ? P2 C21 H21A 109.7 . . ? P1 C21 H21A 109.7 . . ? P2 C21 H21B 109.7 . . ? P1 C21 H21B 109.7 . . ? H21A C21 H21B 108.2 . . ? C27 C22 C23 117.6(5) . . ? C27 C22 P1 125.1(4) . . ? C23 C22 P1 117.2(4) . . ? C24 C23 C22 121.8(6) . . ? C24 C23 H23 119.1 . . ? C22 C23 H23 119.1 . . ? C25 C24 C23 119.6(6) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C24 C25 C26 119.2(6) . . ? C24 C25 H25 120.4 . . ? C26 C25 H25 120.4 . . ? C25 C26 C27 121.3(7) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C22 C27 C26 120.4(6) . . ? C22 C27 H27 119.8 . . ? C26 C27 H27 119.8 . . ? C33 C28 C29 118.1(6) . . ? C33 C28 P1 122.4(5) . . ? C29 C28 P1 119.4(5) . . ? C28 C29 C30 119.4(7) . . ? C28 C29 H29 120.3 . . ? C30 C29 H29 120.3 . . ? C31 C30 C29 120.4(8) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C30 C31 C32 120.4(8) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C31 C32 C33 119.9(8) . . ? C31 C32 H32 120.1 . . ? C33 C32 H32 120.1 . . ? C28 C33 C32 121.7(8) . . ? C28 C33 H33 119.1 . . ? C32 C33 H33 119.1 . . ? C35 C34 C39 119.1(5) . . ? C35 C34 P2 119.3(4) . . ? C39 C34 P2 121.5(5) . . ? C34 C35 C36 120.9(6) . . ? C34 C35 H35 119.6 . . ? C36 C35 H35 119.6 . . ? C37 C36 C35 119.4(7) . . ? C37 C36 H36 120.3 . . ? C35 C36 H36 120.3 . . ? C38 C37 C36 120.5(7) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C37 C38 C39 120.7(6) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C34 C39 C38 119.4(6) . . ? C34 C39 H39 120.3 . . ? C38 C39 H39 120.3 . . ? C45 C40 C41 118.9(5) . . ? C45 C40 P2 125.1(4) . . ? C41 C40 P2 115.9(4) . . ? C40 C41 C42 119.6(6) . . ? C40 C41 H41 120.2 . . ? C42 C41 H41 120.2 . . ? C43 C42 C41 119.9(7) . . ? C43 C42 H42 120.1 . . ? C41 C42 H42 120.1 . . ? C44 C43 C42 119.8(6) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C43 C44 C45 120.7(7) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C40 C45 C44 121.1(6) . . ? C40 C45 H45 119.4 . . ? C44 C45 H45 119.4 . . ? Cl2 C46 Cl1 112.9(7) . . ? Cl2 C46 H46A 109.0 . . ? Cl1 C46 H46A 109.0 . . ? Cl2 C46 H46B 109.0 . . ? Cl1 C46 H46B 109.0 . . ? H46A C46 H46B 107.8 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.527 _refine_diff_density_min -0.610 _refine_diff_density_rms 0.076 #===END data_061230c_Complex3 _database_code_depnum_ccdc_archive 'CCDC 793444' #TrackingRef '- copper.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H34 B Cu F4 N5 P' _chemical_formula_weight 742.02 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' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 '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 8.485(2) _cell_length_b 13.769(2) _cell_length_c 15.231(3) _cell_angle_alpha 91.110(2) _cell_angle_beta 100.453(3) _cell_angle_gamma 91.010(2) _cell_volume 1749.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2931 _cell_measurement_theta_min 2.442 _cell_measurement_theta_max 24.708 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 764 _exptl_absorpt_coefficient_mu 0.727 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7798 _exptl_absorpt_correction_T_max 0.8742 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '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 9117 _diffrn_reflns_av_R_equivalents 0.0193 _diffrn_reflns_av_sigmaI/netI 0.0470 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6063 _reflns_number_gt 4172 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0688P)^2^+1.8331P] 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 6063 _refine_ls_number_parameters 474 _refine_ls_number_restraints 150 _refine_ls_R_factor_all 0.0824 _refine_ls_R_factor_gt 0.0513 _refine_ls_wR_factor_ref 0.1520 _refine_ls_wR_factor_gt 0.1270 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.154 _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 1.02955(7) 0.84125(4) 0.26537(4) 0.0457(2) Uani 1 1 d . . . P1 P 0.94426(14) 0.69086(8) 0.26156(7) 0.0386(3) Uani 1 1 d . . . B1 B 0.7196(7) 0.3000(4) 0.2474(4) 0.0737(18) Uani 1 1 d DU . . F1 F 0.6902(5) 0.3788(3) 0.1991(3) 0.1257(15) Uani 1 1 d DU A . F2 F 0.8682(6) 0.2697(4) 0.2420(4) 0.1513(19) Uani 1 1 d DU A . F3 F 0.6219(10) 0.2246(5) 0.2363(7) 0.158(3) Uani 0.734(8) 1 d PDU A 1 F4 F 0.7494(10) 0.3291(5) 0.3331(4) 0.144(3) Uani 0.734(8) 1 d PDU A 1 F3' F 0.647(2) 0.2418(12) 0.1771(12) 0.144(5) Uani 0.266(8) 1 d PDU A 2 F4' F 0.602(2) 0.2981(15) 0.2929(13) 0.143(5) Uani 0.266(8) 1 d PDU A 2 N1 N 0.9248(5) 1.0625(3) 0.2516(3) 0.0537(10) Uani 1 1 d . . . H1 H 0.8714 1.1148 0.2532 0.064 Uiso 1 1 calc R . . N2 N 1.2652(5) 0.8567(3) 0.4290(3) 0.0496(10) Uani 1 1 d . . . N3 N 1.0941(4) 0.9586(3) 0.3444(2) 0.0436(9) Uani 1 1 d . . . N4 N 1.0137(5) 0.8051(3) 0.0661(2) 0.0489(10) Uani 1 1 d . . . N5 N 0.9609(4) 0.9307(3) 0.1576(2) 0.0445(9) Uani 1 1 d . . . C1 C 1.1978(5) 0.9442(3) 0.4231(3) 0.0424(10) Uani 1 1 d . . . C2 C 1.0262(6) 1.0442(3) 0.3308(3) 0.0459(11) Uani 1 1 d . . . C3 C 1.0541(6) 1.1204(3) 0.3964(3) 0.0555(13) Uani 1 1 d . . . H3 H 1.0056 1.1800 0.3849 0.067 Uiso 1 1 calc R . . C4 C 1.1505(6) 1.1060(4) 0.4747(3) 0.0558(13) Uani 1 1 d . . . H4 H 1.1662 1.1552 0.5183 0.067 Uiso 1 1 calc R . . C5 C 1.2283(5) 1.0168(3) 0.4917(3) 0.0459(11) Uani 1 1 d . . . C6 C 1.3332(6) 0.9938(4) 0.5713(3) 0.0548(13) Uani 1 1 d . . . C7 C 1.3984(6) 0.9037(4) 0.5760(4) 0.0621(14) Uani 1 1 d . . . H7 H 1.4666 0.8863 0.6279 0.075 Uiso 1 1 calc R . . C8 C 1.3645(6) 0.8370(4) 0.5041(4) 0.0562(13) Uani 1 1 d . . . C9 C 1.3707(7) 1.0661(5) 0.6487(4) 0.0722(16) Uani 1 1 d . . . H9A H 1.4404 1.0372 0.6975 0.108 Uiso 1 1 calc R . . H9B H 1.2730 1.0843 0.6674 0.108 Uiso 1 1 calc R . . H9C H 1.4224 1.1228 0.6303 0.108 Uiso 1 1 calc R . . C10 C 1.4412(8) 0.7393(4) 0.5080(4) 0.0811(18) Uani 1 1 d . . . H10A H 1.4334 0.7128 0.4486 0.122 Uiso 1 1 calc R . . H10B H 1.3873 0.6965 0.5424 0.122 Uiso 1 1 calc R . . H10C H 1.5521 0.7463 0.5356 0.122 Uiso 1 1 calc R . . C11 C 0.9315(6) 0.8886(3) 0.0736(3) 0.0464(11) Uani 1 1 d . . . C12 C 0.8923(6) 1.0135(3) 0.1703(3) 0.0467(11) Uani 1 1 d . . . C13 C 0.7838(6) 1.0588(4) 0.1019(4) 0.0595(14) Uani 1 1 d . . . H13 H 0.7361 1.1169 0.1133 0.071 Uiso 1 1 calc R . . C14 C 0.7517(6) 1.0159(4) 0.0206(4) 0.0615(14) Uani 1 1 d . . . H14 H 0.6796 1.0443 -0.0245 0.074 Uiso 1 1 calc R . . C15 C 0.8253(6) 0.9284(4) 0.0023(3) 0.0497(12) Uani 1 1 d . . . C16 C 0.8002(6) 0.8782(4) -0.0818(3) 0.0582(14) Uani 1 1 d . . . C17 C 0.8807(7) 0.7945(4) -0.0869(3) 0.0622(14) Uani 1 1 d . . . H17 H 0.8655 0.7595 -0.1407 0.075 Uiso 1 1 calc R . . C18 C 0.9863(6) 0.7594(4) -0.0129(3) 0.0553(13) Uani 1 1 d . . . C19 C 0.6878(7) 0.9166(5) -0.1614(4) 0.0802(18) Uani 1 1 d . . . H19A H 0.6841 0.8728 -0.2116 0.120 Uiso 1 1 calc R . . H19B H 0.7256 0.9794 -0.1758 0.120 Uiso 1 1 calc R . . H19C H 0.5824 0.9219 -0.1474 0.120 Uiso 1 1 calc R . . C20 C 1.0728(8) 0.6674(4) -0.0221(4) 0.0752(17) Uani 1 1 d . . . H20A H 1.1583 0.6616 0.0282 0.113 Uiso 1 1 calc R . . H20B H 1.1164 0.6682 -0.0760 0.113 Uiso 1 1 calc R . . H20C H 0.9996 0.6130 -0.0243 0.113 Uiso 1 1 calc R . . C21 C 0.7810(5) 0.6718(3) 0.1663(3) 0.0432(11) Uani 1 1 d . . . C22 C 0.6681(6) 0.7434(4) 0.1482(4) 0.0641(15) Uani 1 1 d . . . H22 H 0.6698 0.7959 0.1877 0.077 Uiso 1 1 calc R . . C23 C 0.5517(7) 0.7371(5) 0.0707(5) 0.084(2) Uani 1 1 d . . . H23 H 0.4757 0.7852 0.0585 0.101 Uiso 1 1 calc R . . C24 C 0.5500(8) 0.6597(6) 0.0127(4) 0.086(2) Uani 1 1 d . . . H24 H 0.4736 0.6559 -0.0394 0.103 Uiso 1 1 calc R . . C25 C 0.6581(8) 0.5888(6) 0.0305(4) 0.0800(19) Uani 1 1 d . . . H25 H 0.6546 0.5361 -0.0090 0.096 Uiso 1 1 calc R . . C26 C 0.7743(6) 0.5940(4) 0.1071(3) 0.0603(14) Uani 1 1 d . . . H26 H 0.8483 0.5447 0.1188 0.072 Uiso 1 1 calc R . . C27 C 1.0914(5) 0.6005(3) 0.2463(3) 0.0405(10) Uani 1 1 d . . . C28 C 1.0729(6) 0.5036(3) 0.2652(3) 0.0512(12) Uani 1 1 d . . . H28 H 0.9827 0.4832 0.2871 0.061 Uiso 1 1 calc R . . C29 C 1.1854(7) 0.4366(4) 0.2522(4) 0.0639(15) Uani 1 1 d . . . H29 H 1.1715 0.3717 0.2655 0.077 Uiso 1 1 calc R . . C30 C 1.3187(7) 0.4662(5) 0.2192(4) 0.0749(18) Uani 1 1 d . . . H30 H 1.3949 0.4212 0.2101 0.090 Uiso 1 1 calc R . . C31 C 1.3395(7) 0.5621(5) 0.1999(4) 0.0738(17) Uani 1 1 d . . . H31 H 1.4289 0.5819 0.1769 0.089 Uiso 1 1 calc R . . C32 C 1.2279(6) 0.6286(4) 0.2145(3) 0.0564(13) Uani 1 1 d . . . H32 H 1.2441 0.6937 0.2028 0.068 Uiso 1 1 calc R . . C33 C 0.8662(5) 0.6447(3) 0.3568(3) 0.0391(10) Uani 1 1 d . . . C34 C 0.9558(6) 0.6602(3) 0.4409(3) 0.0491(12) Uani 1 1 d . . . H34 H 1.0491 0.6982 0.4485 0.059 Uiso 1 1 calc R . . C35 C 0.9072(7) 0.6192(4) 0.5143(3) 0.0608(14) Uani 1 1 d . . . H35 H 0.9691 0.6294 0.5708 0.073 Uiso 1 1 calc R . . C36 C 0.7690(7) 0.5639(4) 0.5045(4) 0.0640(15) Uani 1 1 d . . . H36 H 0.7372 0.5368 0.5541 0.077 Uiso 1 1 calc R . . C37 C 0.6784(7) 0.5489(4) 0.4216(4) 0.0671(15) Uani 1 1 d . . . H37 H 0.5839 0.5120 0.4146 0.081 Uiso 1 1 calc R . . C38 C 0.7270(6) 0.5887(4) 0.3479(3) 0.0571(13) Uani 1 1 d . . . H38 H 0.6652 0.5776 0.2915 0.068 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 0.0582(4) 0.0338(3) 0.0433(3) 0.0034(2) 0.0046(3) -0.0026(2) P1 0.0468(7) 0.0336(6) 0.0337(6) 0.0024(5) 0.0032(5) -0.0018(5) B1 0.087(5) 0.054(4) 0.087(5) -0.005(3) 0.034(4) 0.010(3) F1 0.111(3) 0.111(3) 0.154(4) 0.048(3) 0.015(3) 0.030(3) F2 0.144(4) 0.107(3) 0.208(5) 0.029(3) 0.038(4) 0.043(3) F3 0.177(6) 0.132(5) 0.164(6) -0.020(5) 0.042(5) -0.092(4) F4 0.179(6) 0.165(6) 0.087(4) -0.041(4) 0.030(4) -0.044(5) F3' 0.168(9) 0.124(8) 0.138(9) -0.027(8) 0.030(8) -0.013(8) F4' 0.170(9) 0.130(9) 0.140(9) 0.013(8) 0.054(8) 0.016(8) N1 0.063(3) 0.038(2) 0.057(3) 0.0031(19) 0.002(2) 0.0108(19) N2 0.054(2) 0.045(2) 0.050(2) 0.0039(18) 0.008(2) 0.0065(18) N3 0.049(2) 0.034(2) 0.046(2) 0.0005(16) 0.0072(18) -0.0023(16) N4 0.059(2) 0.049(2) 0.040(2) 0.0077(18) 0.0113(19) -0.0003(19) N5 0.052(2) 0.041(2) 0.038(2) 0.0082(17) 0.0018(17) -0.0029(17) C1 0.042(3) 0.043(3) 0.043(3) 0.001(2) 0.008(2) -0.003(2) C2 0.049(3) 0.038(3) 0.051(3) 0.001(2) 0.010(2) -0.004(2) C3 0.066(3) 0.037(3) 0.062(3) -0.006(2) 0.009(3) 0.003(2) C4 0.062(3) 0.051(3) 0.055(3) -0.014(2) 0.012(3) -0.004(2) C5 0.045(3) 0.048(3) 0.046(3) -0.004(2) 0.012(2) -0.007(2) C6 0.048(3) 0.071(4) 0.045(3) 0.000(2) 0.008(2) -0.009(3) C7 0.060(3) 0.078(4) 0.046(3) 0.008(3) 0.003(3) 0.002(3) C8 0.054(3) 0.059(3) 0.058(3) 0.013(3) 0.012(3) 0.008(2) C9 0.070(4) 0.095(5) 0.048(3) -0.016(3) 0.005(3) -0.012(3) C10 0.086(4) 0.076(4) 0.082(4) 0.021(3) 0.012(4) 0.028(3) C11 0.053(3) 0.047(3) 0.039(3) 0.013(2) 0.007(2) -0.011(2) C12 0.051(3) 0.039(3) 0.048(3) 0.009(2) 0.005(2) -0.004(2) C13 0.062(3) 0.046(3) 0.067(4) 0.012(3) 0.000(3) 0.006(2) C14 0.055(3) 0.065(4) 0.060(3) 0.023(3) -0.003(3) 0.001(3) C15 0.047(3) 0.052(3) 0.049(3) 0.016(2) 0.004(2) -0.010(2) C16 0.053(3) 0.076(4) 0.044(3) 0.011(3) 0.004(2) -0.018(3) C17 0.068(4) 0.074(4) 0.043(3) 0.001(3) 0.010(3) -0.012(3) C18 0.064(3) 0.062(3) 0.042(3) 0.000(2) 0.015(2) -0.009(3) C19 0.071(4) 0.109(5) 0.053(3) 0.014(3) -0.012(3) -0.006(3) C20 0.090(4) 0.081(4) 0.058(4) -0.008(3) 0.023(3) 0.012(3) C21 0.047(3) 0.043(3) 0.038(2) 0.006(2) 0.002(2) -0.009(2) C22 0.062(3) 0.050(3) 0.073(4) 0.009(3) -0.010(3) 0.000(3) C23 0.069(4) 0.079(5) 0.093(5) 0.030(4) -0.017(4) -0.004(3) C24 0.065(4) 0.126(6) 0.057(4) 0.025(4) -0.015(3) -0.031(4) C25 0.067(4) 0.118(6) 0.050(3) -0.016(3) 0.002(3) -0.021(4) C26 0.057(3) 0.071(4) 0.050(3) -0.011(3) 0.005(2) -0.009(3) C27 0.044(3) 0.045(3) 0.032(2) 0.0028(19) 0.0047(19) 0.001(2) C28 0.060(3) 0.049(3) 0.047(3) 0.004(2) 0.017(2) 0.008(2) C29 0.084(4) 0.055(3) 0.055(3) 0.000(3) 0.017(3) 0.021(3) C30 0.071(4) 0.102(5) 0.051(3) -0.003(3) 0.007(3) 0.038(4) C31 0.047(3) 0.111(5) 0.066(4) 0.011(4) 0.015(3) 0.011(3) C32 0.047(3) 0.070(3) 0.052(3) 0.008(3) 0.007(2) -0.002(3) C33 0.047(3) 0.033(2) 0.037(2) -0.0001(18) 0.008(2) 0.0066(19) C34 0.060(3) 0.044(3) 0.043(3) 0.004(2) 0.006(2) -0.001(2) C35 0.083(4) 0.059(3) 0.038(3) 0.002(2) 0.006(3) 0.005(3) C36 0.081(4) 0.065(4) 0.053(3) 0.012(3) 0.028(3) 0.006(3) C37 0.062(3) 0.078(4) 0.064(4) 0.011(3) 0.021(3) -0.010(3) C38 0.057(3) 0.069(3) 0.046(3) 0.004(2) 0.010(2) -0.008(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N3 2.003(4) . ? Cu1 N5 2.075(4) . ? Cu1 P1 2.1776(13) . ? P1 C27 1.819(5) . ? P1 C33 1.822(4) . ? P1 C21 1.826(4) . ? B1 F3 1.305(6) . ? B1 F4' 1.312(8) . ? B1 F1 1.325(6) . ? B1 F4 1.337(6) . ? B1 F2 1.351(6) . ? B1 F3' 1.370(8) . ? N1 C12 1.378(6) . ? N1 C2 1.378(6) . ? N1 H1 0.8600 . ? N2 C8 1.328(6) . ? N2 C1 1.341(6) . ? N3 C2 1.325(6) . ? N3 C1 1.372(6) . ? N4 C18 1.328(6) . ? N4 C11 1.368(6) . ? N5 C12 1.317(6) . ? N5 C11 1.374(6) . ? C1 C5 1.417(6) . ? C2 C3 1.420(6) . ? C3 C4 1.340(7) . ? C3 H3 0.9300 . ? C4 C5 1.411(7) . ? C4 H4 0.9300 . ? C5 C6 1.412(7) . ? C6 C7 1.365(7) . ? C6 C9 1.513(7) . ? C7 C8 1.401(7) . ? C7 H7 0.9300 . ? C8 C10 1.502(7) . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C15 1.407(6) . ? C12 C13 1.421(7) . ? C13 C14 1.342(7) . ? C13 H13 0.9300 . ? C14 C15 1.413(7) . ? C14 H14 0.9300 . ? C15 C16 1.423(7) . ? C16 C17 1.358(8) . ? C16 C19 1.510(7) . ? C17 C18 1.405(7) . ? C17 H17 0.9300 . ? C18 C20 1.493(8) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 C26 1.381(6) . ? C21 C22 1.383(7) . ? C22 C23 1.395(8) . ? C22 H22 0.9300 . ? C23 C24 1.369(9) . ? C23 H23 0.9300 . ? C24 C25 1.348(10) . ? C24 H24 0.9300 . ? C25 C26 1.384(7) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 C28 1.383(6) . ? C27 C32 1.386(6) . ? C28 C29 1.376(7) . ? C28 H28 0.9300 . ? C29 C30 1.376(8) . ? C29 H29 0.9300 . ? C30 C31 1.374(9) . ? C30 H30 0.9300 . ? C31 C32 1.373(8) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.376(6) . ? C33 C38 1.383(6) . ? C34 C35 1.385(7) . ? C34 H34 0.9300 . ? C35 C36 1.370(8) . ? C35 H35 0.9300 . ? C36 C37 1.364(8) . ? C36 H36 0.9300 . ? C37 C38 1.383(7) . ? C37 H37 0.9300 . ? C38 H38 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 N3 Cu1 N5 89.83(15) . . ? N3 Cu1 P1 144.62(12) . . ? N5 Cu1 P1 120.96(11) . . ? C27 P1 C33 102.15(19) . . ? C27 P1 C21 105.0(2) . . ? C33 P1 C21 105.0(2) . . ? C27 P1 Cu1 115.21(15) . . ? C33 P1 Cu1 118.96(14) . . ? C21 P1 Cu1 109.26(15) . . ? F3 B1 F4' 62.1(10) . . ? F3 B1 F1 121.9(7) . . ? F4' B1 F1 102.9(9) . . ? F3 B1 F4 110.3(7) . . ? F4' B1 F4 61.0(10) . . ? F1 B1 F4 107.1(6) . . ? F3 B1 F2 108.5(6) . . ? F4' B1 F2 146.4(10) . . ? F1 B1 F2 108.6(5) . . ? F4 B1 F2 97.8(6) . . ? F3 B1 F3' 43.6(9) . . ? F4' B1 F3' 97.4(11) . . ? F1 B1 F3' 91.2(9) . . ? F4 B1 F3' 153.9(11) . . ? F2 B1 F3' 93.6(9) . . ? C12 N1 C2 132.7(4) . . ? C12 N1 H1 113.6 . . ? C2 N1 H1 113.6 . . ? C8 N2 C1 117.7(4) . . ? C2 N3 C1 118.9(4) . . ? C2 N3 Cu1 123.6(3) . . ? C1 N3 Cu1 116.8(3) . . ? C18 N4 C11 116.8(4) . . ? C12 N5 C11 118.4(4) . . ? C12 N5 Cu1 119.1(3) . . ? C11 N5 Cu1 117.9(3) . . ? N2 C1 N3 114.4(4) . . ? N2 C1 C5 123.8(4) . . ? N3 C1 C5 121.9(4) . . ? N3 C2 N1 120.7(4) . . ? N3 C2 C3 121.8(4) . . ? N1 C2 C3 117.5(4) . . ? C4 C3 C2 119.8(5) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 120.5(4) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C4 C5 C6 125.4(4) . . ? C4 C5 C1 117.1(4) . . ? C6 C5 C1 117.5(4) . . ? C7 C6 C5 117.5(5) . . ? C7 C6 C9 121.3(5) . . ? C5 C6 C9 121.2(5) . . ? C6 C7 C8 121.3(5) . . ? C6 C7 H7 119.4 . . ? C8 C7 H7 119.4 . . ? N2 C8 C7 122.2(5) . . ? N2 C8 C10 116.5(5) . . ? C7 C8 C10 121.2(5) . . ? C6 C9 H9A 109.5 . . ? C6 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C6 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N4 C11 N5 114.1(4) . . ? N4 C11 C15 123.6(4) . . ? N5 C11 C15 122.4(5) . . ? N5 C12 N1 121.2(4) . . ? N5 C12 C13 122.8(5) . . ? N1 C12 C13 116.0(4) . . ? C14 C13 C12 118.6(5) . . ? C14 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? C13 C14 C15 121.2(5) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C11 C15 C14 116.6(5) . . ? C11 C15 C16 118.1(5) . . ? C14 C15 C16 125.3(5) . . ? C17 C16 C15 117.1(5) . . ? C17 C16 C19 121.8(5) . . ? C15 C16 C19 121.1(5) . . ? C16 C17 C18 121.8(5) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? N4 C18 C17 122.6(5) . . ? N4 C18 C20 117.7(5) . . ? C17 C18 C20 119.7(5) . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C26 C21 C22 118.7(5) . . ? C26 C21 P1 122.8(4) . . ? C22 C21 P1 118.2(4) . . ? C21 C22 C23 120.2(6) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C24 C23 C22 119.6(6) . . ? C24 C23 H23 120.2 . . ? C22 C23 H23 120.2 . . ? C25 C24 C23 120.7(6) . . ? C25 C24 H24 119.7 . . ? C23 C24 H24 119.7 . . ? C24 C25 C26 120.4(6) . . ? C24 C25 H25 119.8 . . ? C26 C25 H25 119.8 . . ? C21 C26 C25 120.4(6) . . ? C21 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C28 C27 C32 117.9(4) . . ? C28 C27 P1 122.5(4) . . ? C32 C27 P1 119.6(4) . . ? C29 C28 C27 121.3(5) . . ? C29 C28 H28 119.3 . . ? C27 C28 H28 119.3 . . ? C30 C29 C28 119.5(6) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C31 C30 C29 120.2(5) . . ? C31 C30 H30 119.9 . . ? C29 C30 H30 119.9 . . ? C32 C31 C30 119.8(6) . . ? C32 C31 H31 120.1 . . ? C30 C31 H31 120.1 . . ? C31 C32 C27 121.2(5) . . ? C31 C32 H32 119.4 . . ? C27 C32 H32 119.4 . . ? C34 C33 C38 118.5(4) . . ? C34 C33 P1 118.4(3) . . ? C38 C33 P1 122.9(3) . . ? C33 C34 C35 120.2(5) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C36 C35 C34 120.7(5) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C37 C36 C35 119.7(5) . . ? C37 C36 H36 120.2 . . ? C35 C36 H36 120.2 . . ? C36 C37 C38 119.9(5) . . ? C36 C37 H37 120.0 . . ? C38 C37 H37 120.0 . . ? C37 C38 C33 121.0(5) . . ? C37 C38 H38 119.5 . . ? C33 C38 H38 119.5 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.832 _refine_diff_density_min -0.658 _refine_diff_density_rms 0.064 #===END