# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _publ_contact_author_name 'Fumiyuki Ozawa' _publ_contact_author_address ; International Research Center for Elements Science (IRCELS) Institute for Chemical Research Kyoto University Gokasho Uji, Kyoto 611-0011 Japan ; _publ_contact_author_email ozawa@scl.kyoto-u.ac.jp _publ_section_title ; Synthesis and coordination behavior of Cy(I) bis(phosphaethenyl)pyridine complexes. ; loop_ _publ_author_name 'Yumiko Nakajima' 'Yu Shiraishi' 'Takahiro Tsuchimoto' 'Fumiyuki Ozawa' data_1 _database_code_depnum_ccdc_archive 'CCDC 812261' #TrackingRef '1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55.50 H72 Br Cl Cu N P2' _chemical_formula_weight 993.98 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' 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' Br Br -0.2901 2.4595 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.9441(2) _cell_length_b 9.64940(10) _cell_length_c 35.0720(7) _cell_angle_alpha 90.00 _cell_angle_beta 96.2821(8) _cell_angle_gamma 90.00 _cell_volume 5363.46(14) _cell_formula_units_Z 4 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.231 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2092 _exptl_absorpt_coefficient_mu 1.296 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8293 _exptl_absorpt_correction_T_max 0.9380 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type '4-circle diffractometer' _diffrn_measurement_method 'scintillation counter' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 52478 _diffrn_reflns_av_R_equivalents 0.0715 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 41 _diffrn_reflns_theta_min 2.19 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9450 _reflns_number_gt 7829 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius CAD4 software' _computing_cell_refinement 'Nonius CAD4 software' _computing_data_reduction 'XCAD (P.McArdle, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.0001P)^2^+43.1302P] 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 9450 _refine_ls_number_parameters 625 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0969 _refine_ls_R_factor_gt 0.0818 _refine_ls_wR_factor_ref 0.1902 _refine_ls_wR_factor_gt 0.1827 _refine_ls_goodness_of_fit_ref 1.241 _refine_ls_restrained_S_all 1.241 _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 0.38520(5) 0.24650(9) 0.14730(2) 0.0284(2) Uani 1 1 d . . . Br1 Br 0.33950(5) 0.03549(8) 0.17047(3) 0.0482(2) Uani 1 1 d . . . P1 P 0.26947(10) 0.34326(18) 0.11639(5) 0.0284(4) Uani 1 1 d . . . C1 C 0.2792(4) 0.5143(7) 0.12736(17) 0.0267(14) Uani 1 1 d . . . C2 C 0.3665(4) 0.5551(7) 0.14089(18) 0.0293(15) Uani 1 1 d . . . C3 C 0.3955(4) 0.6950(8) 0.13815(19) 0.0377(17) Uani 1 1 d . . . H1 H 0.3574 0.7662 0.1289 0.045 Uiso 1 1 calc R . . C4 C 0.4780(4) 0.7245(7) 0.14885(19) 0.0320(15) Uani 1 1 d . . . H2 H 0.4964 0.8181 0.1494 0.038 Uiso 1 1 calc R . . C5 C 0.5353(4) 0.6206(7) 0.15898(18) 0.0295(15) Uani 1 1 d . . . H3 H 0.5934 0.6421 0.1650 0.035 Uiso 1 1 calc R . . C6 C 0.5073(4) 0.4815(7) 0.16048(17) 0.0263(14) Uani 1 1 d . . . N1 N 0.4219(3) 0.4515(6) 0.15434(14) 0.0269(12) Uani 1 1 d . . . C7 C 0.5663(4) 0.3664(7) 0.16527(18) 0.0278(14) Uani 1 1 d . . . P2 P 0.52412(10) 0.21665(18) 0.14587(5) 0.0270(4) Uani 1 1 d . . . C8 C 0.1575(4) 0.3020(7) 0.10415(18) 0.0277(14) Uani 1 1 d . . . C9 C 0.1334(4) 0.2601(8) 0.06506(19) 0.0355(16) Uani 1 1 d . . . C10 C 0.0488(4) 0.2689(8) 0.05110(19) 0.0389(17) Uani 1 1 d . . . H4 H 0.0330 0.2475 0.0249 0.047 Uiso 1 1 calc R . . C11 C -0.0140(4) 0.3075(7) 0.07345(19) 0.0314(15) Uani 1 1 d . A . C12 C 0.0100(4) 0.3291(6) 0.11202(18) 0.0275(14) Uani 1 1 d . . . H5 H -0.0327 0.3476 0.1282 0.033 Uiso 1 1 calc R . . C13 C 0.0937(4) 0.3253(7) 0.12850(18) 0.0282(14) Uani 1 1 d . . . C14 C 0.1958(5) 0.1976(10) 0.0385(2) 0.052(2) Uani 1 1 d . . . C15 C -0.1063(4) 0.3211(8) 0.0565(2) 0.0365(16) Uani 1 1 d . . . C16 C 0.1036(4) 0.3347(7) 0.17308(19) 0.0305(15) Uani 1 1 d . . . C17 C 0.2427(5) 0.0742(10) 0.0585(3) 0.062(3) Uani 1 1 d . . . H6 H 0.2817 0.0349 0.0416 0.093 Uiso 1 1 calc R . . H7 H 0.2019 0.0034 0.0642 0.093 Uiso 1 1 calc R . . H8 H 0.2746 0.1056 0.0824 0.093 Uiso 1 1 calc R . . C18 C 0.2582(6) 0.3080(12) 0.0258(2) 0.074(3) Uani 1 1 d . . . H9 H 0.2263 0.3847 0.0130 0.111 Uiso 1 1 calc R . . H10 H 0.2942 0.2657 0.0081 0.111 Uiso 1 1 calc R . . H11 H 0.2934 0.3431 0.0484 0.111 Uiso 1 1 calc R . . C19 C 0.1480(6) 0.1402(12) 0.0009(3) 0.075(3) Uani 1 1 d . . . H12 H 0.1175 0.2158 -0.0132 0.112 Uiso 1 1 calc R . . H13 H 0.1078 0.0690 0.0071 0.112 Uiso 1 1 calc R . . H14 H 0.1885 0.0995 -0.0150 0.112 Uiso 1 1 calc R . . C20 C -0.1531(8) 0.1898(13) 0.0723(4) 0.040(3) Uani 0.579(12) 1 d P A 1 H15 H -0.1272 0.1045 0.0639 0.060 Uiso 0.579(12) 1 calc PR A 1 H16 H -0.2130 0.1916 0.0622 0.060 Uiso 0.579(12) 1 calc PR A 1 H17 H -0.1479 0.1927 0.1004 0.060 Uiso 0.579(12) 1 calc PR A 1 C21 C -0.1183(8) 0.3094(16) 0.0131(4) 0.048(4) Uani 0.579(12) 1 d P A 1 H18 H -0.0927 0.2230 0.0053 0.073 Uiso 0.579(12) 1 calc PR A 1 H19 H -0.0912 0.3883 0.0018 0.073 Uiso 0.579(12) 1 calc PR A 1 H20 H -0.1787 0.3092 0.0041 0.073 Uiso 0.579(12) 1 calc PR A 1 C22 C -0.1447(9) 0.4483(16) 0.0693(4) 0.049(4) Uani 0.579(12) 1 d P A 1 H21 H -0.2037 0.4534 0.0580 0.074 Uiso 0.579(12) 1 calc PR A 1 H22 H -0.1138 0.5288 0.0610 0.074 Uiso 0.579(12) 1 calc PR A 1 H23 H -0.1423 0.4480 0.0973 0.074 Uiso 0.579(12) 1 calc PR A 1 C23 C -0.1365(11) 0.1964(19) 0.0345(5) 0.044(5) Uani 0.421(12) 1 d P A 2 H24 H -0.1957 0.2091 0.0242 0.066 Uiso 0.421(12) 1 calc PR A 2 H25 H -0.1315 0.1152 0.0514 0.066 Uiso 0.421(12) 1 calc PR A 2 H26 H -0.1023 0.1822 0.0132 0.066 Uiso 0.421(12) 1 calc PR A 2 C24 C -0.1671(12) 0.362(2) 0.0858(6) 0.046(5) Uani 0.421(12) 1 d P A 2 H27 H -0.1452 0.4444 0.1000 0.069 Uiso 0.421(12) 1 calc PR A 2 H28 H -0.1720 0.2856 0.1037 0.069 Uiso 0.421(12) 1 calc PR A 2 H29 H -0.2228 0.3832 0.0723 0.069 Uiso 0.421(12) 1 calc PR A 2 C25 C -0.1078(12) 0.4537(19) 0.0287(6) 0.054(6) Uani 0.421(12) 1 d P A 2 H30 H -0.0862 0.5347 0.0436 0.081 Uiso 0.421(12) 1 calc PR A 2 H31 H -0.1658 0.4716 0.0175 0.081 Uiso 0.421(12) 1 calc PR A 2 H32 H -0.0722 0.4357 0.0082 0.081 Uiso 0.421(12) 1 calc PR A 2 C26 C 0.0568(4) 0.2085(7) 0.1877(2) 0.0374(17) Uani 1 1 d . . . H33 H -0.0017 0.2082 0.1758 0.056 Uiso 1 1 calc R . . H34 H 0.0575 0.2143 0.2156 0.056 Uiso 1 1 calc R . . H35 H 0.0849 0.1230 0.1809 0.056 Uiso 1 1 calc R . . C27 C 0.0628(4) 0.4686(8) 0.1861(2) 0.0380(17) Uani 1 1 d . . . H36 H 0.0050 0.4758 0.1735 0.057 Uiso 1 1 calc R . . H37 H 0.0957 0.5487 0.1791 0.057 Uiso 1 1 calc R . . H38 H 0.0616 0.4665 0.2140 0.057 Uiso 1 1 calc R . . C28 C 0.1929(4) 0.3268(9) 0.19325(19) 0.0403(18) Uani 1 1 d . . . H39 H 0.2202 0.2419 0.1854 0.060 Uiso 1 1 calc R . . H40 H 0.1909 0.3257 0.2211 0.060 Uiso 1 1 calc R . . H41 H 0.2251 0.4076 0.1862 0.060 Uiso 1 1 calc R . . C29 C 0.2128(4) 0.6234(7) 0.1221(2) 0.0334(16) Uani 1 1 d . . . C30 C 0.1551(5) 0.6277(8) 0.0889(2) 0.0429(18) Uani 1 1 d . . . H42 H 0.1579 0.5602 0.0693 0.051 Uiso 1 1 calc R . . C31 C 0.0938(5) 0.7309(9) 0.0845(3) 0.056(2) Uani 1 1 d . . . H43 H 0.0541 0.7316 0.0622 0.068 Uiso 1 1 calc R . . C32 C 0.0895(5) 0.8324(8) 0.1120(3) 0.061(3) Uani 1 1 d . . . H44 H 0.0478 0.9029 0.1086 0.074 Uiso 1 1 calc R . . C33 C 0.1459(5) 0.8298(8) 0.1442(3) 0.054(2) Uani 1 1 d . . . H45 H 0.1441 0.9001 0.1631 0.065 Uiso 1 1 calc R . . C34 C 0.2063(5) 0.7246(7) 0.1497(2) 0.0398(17) Uani 1 1 d . . . H46 H 0.2436 0.7225 0.1727 0.048 Uiso 1 1 calc R . . C35 C 0.6538(4) 0.3872(7) 0.18406(19) 0.0311(15) Uani 1 1 d . . . C36 C 0.6680(4) 0.4611(8) 0.2189(2) 0.0366(16) Uani 1 1 d . . . H47 H 0.6219 0.5035 0.2294 0.044 Uiso 1 1 calc R . . C37 C 0.7487(5) 0.4719(9) 0.2377(2) 0.0470(19) Uani 1 1 d . . . H48 H 0.7574 0.5201 0.2615 0.056 Uiso 1 1 calc R . . C38 C 0.8161(5) 0.4137(9) 0.2225(3) 0.052(2) Uani 1 1 d . . . H49 H 0.8713 0.4219 0.2356 0.063 Uiso 1 1 calc R . . C39 C 0.8038(4) 0.3429(8) 0.1878(2) 0.0454(19) Uani 1 1 d . . . H50 H 0.8505 0.3029 0.1773 0.054 Uiso 1 1 calc R . . C40 C 0.7236(4) 0.3308(8) 0.1688(2) 0.0371(17) Uani 1 1 d . . . H51 H 0.7158 0.2834 0.1449 0.045 Uiso 1 1 calc R . . C41 C 0.6015(4) 0.0768(7) 0.15026(19) 0.0288(14) Uani 1 1 d . . . C42 C 0.6432(4) 0.0264(7) 0.18514(18) 0.0294(14) Uani 1 1 d . . . C43 C 0.7154(4) -0.0537(7) 0.1834(2) 0.0327(15) Uani 1 1 d . . . H52 H 0.7438 -0.0876 0.2068 0.039 Uiso 1 1 calc R . . C44 C 0.7479(4) -0.0866(7) 0.1497(2) 0.0327(15) Uani 1 1 d . B . C45 C 0.7010(4) -0.0499(7) 0.1157(2) 0.0327(15) Uani 1 1 d . . . H53 H 0.7200 -0.0791 0.0923 0.039 Uiso 1 1 calc R . . C46 C 0.6269(4) 0.0283(7) 0.11436(18) 0.0300(15) Uani 1 1 d . . . C47 C 0.6168(4) 0.0393(8) 0.22648(19) 0.0352(16) Uani 1 1 d . . . C48 C 0.8319(5) -0.1657(8) 0.1507(2) 0.0407(18) Uani 1 1 d . . . C49 C 0.5779(4) 0.0561(9) 0.0744(2) 0.0408(18) Uani 1 1 d . . . C50 C 0.5985(5) -0.1084(8) 0.2399(2) 0.0421(18) Uani 1 1 d . . . H54 H 0.5520 -0.1483 0.2227 0.063 Uiso 1 1 calc R . . H55 H 0.5826 -0.1051 0.2661 0.063 Uiso 1 1 calc R . . H56 H 0.6490 -0.1658 0.2393 0.063 Uiso 1 1 calc R . . C51 C 0.6897(5) 0.1029(9) 0.2536(2) 0.0450(19) Uani 1 1 d . . . H57 H 0.7015 0.1967 0.2449 0.067 Uiso 1 1 calc R . . H58 H 0.7403 0.0454 0.2533 0.067 Uiso 1 1 calc R . . H59 H 0.6735 0.1069 0.2797 0.067 Uiso 1 1 calc R . . C52 C 0.5388(5) 0.1276(9) 0.2313(2) 0.0453(19) Uani 1 1 d . . . H60 H 0.5483 0.2227 0.2229 0.068 Uiso 1 1 calc R . . H61 H 0.5284 0.1282 0.2583 0.068 Uiso 1 1 calc R . . H62 H 0.4897 0.0885 0.2157 0.068 Uiso 1 1 calc R . . C53 C 0.8219(8) -0.3050(13) 0.1712(4) 0.068(5) Uani 0.716(14) 1 d P B 1 H63 H 0.7743 -0.3564 0.1580 0.103 Uiso 0.716(14) 1 calc PR B 1 H64 H 0.8114 -0.2876 0.1978 0.103 Uiso 0.716(14) 1 calc PR B 1 H65 H 0.8737 -0.3595 0.1710 0.103 Uiso 0.716(14) 1 calc PR B 1 C54 C 0.9016(7) -0.0826(15) 0.1688(4) 0.057(4) Uani 0.716(14) 1 d P B 1 H66 H 0.9544 -0.1351 0.1692 0.086 Uiso 0.716(14) 1 calc PR B 1 H67 H 0.8913 -0.0604 0.1952 0.086 Uiso 0.716(14) 1 calc PR B 1 H68 H 0.9061 0.0034 0.1543 0.086 Uiso 0.716(14) 1 calc PR B 1 C55 C 0.8516(7) -0.2051(13) 0.1087(3) 0.047(3) Uani 0.716(14) 1 d P B 1 H69 H 0.8054 -0.2615 0.0962 0.070 Uiso 0.716(14) 1 calc PR B 1 H70 H 0.9044 -0.2579 0.1101 0.070 Uiso 0.716(14) 1 calc PR B 1 H71 H 0.8572 -0.1203 0.0938 0.070 Uiso 0.716(14) 1 calc PR B 1 C56 C 0.826(2) -0.288(5) 0.1331(9) 0.084(16) Uani 0.284(14) 1 d P B 2 H72 H 0.8821 -0.3317 0.1353 0.127 Uiso 0.284(14) 1 calc PR B 2 H73 H 0.8061 -0.2745 0.1059 0.127 Uiso 0.284(14) 1 calc PR B 2 H74 H 0.7868 -0.3471 0.1451 0.127 Uiso 0.284(14) 1 calc PR B 2 C57 C 0.8818(15) -0.175(3) 0.1933(8) 0.044(8) Uani 0.284(14) 1 d P B 2 H75 H 0.8949 -0.0811 0.2029 0.066 Uiso 0.284(14) 1 calc PR B 2 H76 H 0.9343 -0.2269 0.1924 0.066 Uiso 0.284(14) 1 calc PR B 2 H77 H 0.8464 -0.2221 0.2104 0.066 Uiso 0.284(14) 1 calc PR B 2 C58 C 0.8939(17) -0.049(4) 0.1335(10) 0.068(12) Uani 0.284(14) 1 d P B 2 H78 H 0.8960 0.0340 0.1495 0.102 Uiso 0.284(14) 1 calc PR B 2 H79 H 0.8715 -0.0255 0.1072 0.102 Uiso 0.284(14) 1 calc PR B 2 H80 H 0.9508 -0.0877 0.1336 0.102 Uiso 0.284(14) 1 calc PR B 2 C59 C 0.4856(4) 0.0049(8) 0.0737(2) 0.0420(18) Uani 1 1 d . . . H81 H 0.4550 0.0230 0.0484 0.063 Uiso 1 1 calc R . . H82 H 0.4580 0.0542 0.0934 0.063 Uiso 1 1 calc R . . H83 H 0.4853 -0.0948 0.0790 0.063 Uiso 1 1 calc R . . C60 C 0.5802(5) 0.2079(10) 0.0620(2) 0.052(2) Uani 1 1 d . . . H84 H 0.5478 0.2188 0.0367 0.078 Uiso 1 1 calc R . . H85 H 0.6388 0.2360 0.0605 0.078 Uiso 1 1 calc R . . H86 H 0.5554 0.2660 0.0807 0.078 Uiso 1 1 calc R . . C61 C 0.6143(5) -0.0259(12) 0.0426(2) 0.067(3) Uani 1 1 d . . . H87 H 0.5814 -0.0062 0.0180 0.07(3) Uiso 1 1 calc R . . H88 H 0.6116 -0.1252 0.0482 0.107 Uiso 1 1 calc R . . H89 H 0.6732 0.0013 0.0415 0.107 Uiso 1 1 calc R . . C62 C 0.4524(11) 0.5487(19) 0.0468(5) 0.060(5) Uani 0.50 1 d P . . Cl1 Cl 0.3667(4) 0.6598(7) 0.03660(16) 0.095(2) Uani 0.50 1 d P C . Cl2 Cl 0.5463(6) 0.6023(10) 0.0464(3) 0.080(4) Uiso 0.323(10) 1 d P C 1 H90 H 0.4477 0.5112 0.0721 0.120 Uiso 0.323(10) 1 d PR C 1 H91 H 0.4440 0.4749 0.0278 0.120 Uiso 0.323(10) 1 d PR C 1 Cl3 Cl 0.541(2) 0.531(4) 0.0166(12) 0.190(17) Uiso 0.177(10) 1 d P . 2 H92 H 0.4326 0.4576 0.0502 0.285 Uiso 0.177(10) 1 d PR C 2 H93 H 0.4837 0.5785 0.0728 0.285 Uiso 0.177(10) 1 d PR C 2 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 0.0247(4) 0.0261(4) 0.0358(4) -0.0026(4) 0.0088(3) -0.0002(3) Br1 0.0481(5) 0.0261(4) 0.0730(6) 0.0027(4) 0.0188(4) -0.0035(3) P1 0.0245(8) 0.0288(9) 0.0326(9) -0.0053(7) 0.0067(7) -0.0002(7) C1 0.029(3) 0.028(3) 0.024(3) 0.000(3) 0.006(3) 0.001(3) C2 0.029(3) 0.038(4) 0.022(3) 0.000(3) 0.009(3) 0.005(3) C3 0.034(4) 0.053(5) 0.026(4) 0.005(3) 0.004(3) -0.008(3) C4 0.030(3) 0.029(4) 0.037(4) -0.005(3) 0.007(3) 0.001(3) C5 0.028(3) 0.030(4) 0.031(3) -0.008(3) 0.007(3) -0.001(3) C6 0.023(3) 0.034(4) 0.023(3) -0.007(3) 0.006(3) 0.003(3) N1 0.028(3) 0.031(3) 0.023(3) 0.001(2) 0.007(2) -0.004(2) C7 0.029(3) 0.031(4) 0.024(3) 0.001(3) 0.008(3) -0.001(3) P2 0.0240(8) 0.0264(9) 0.0315(9) -0.0033(7) 0.0068(7) 0.0014(7) C8 0.029(3) 0.029(3) 0.025(3) -0.007(3) 0.006(3) -0.002(3) C9 0.032(4) 0.042(4) 0.033(4) -0.008(3) 0.009(3) -0.004(3) C10 0.045(4) 0.046(4) 0.026(3) -0.006(3) 0.003(3) -0.009(4) C11 0.030(4) 0.033(4) 0.032(4) -0.001(3) 0.005(3) -0.001(3) C12 0.028(3) 0.022(3) 0.032(4) -0.003(3) 0.008(3) -0.001(3) C13 0.025(3) 0.028(4) 0.032(3) -0.002(3) 0.004(3) 0.001(3) C14 0.040(4) 0.076(6) 0.041(4) -0.029(4) 0.017(4) -0.014(4) C15 0.034(4) 0.041(4) 0.034(4) 0.003(3) 0.000(3) 0.001(3) C16 0.028(3) 0.034(4) 0.031(3) -0.007(3) 0.005(3) -0.004(3) C17 0.042(5) 0.074(7) 0.071(6) -0.045(5) 0.016(4) 0.003(4) C18 0.060(6) 0.124(10) 0.042(5) -0.027(6) 0.024(4) -0.036(6) C19 0.059(6) 0.115(9) 0.053(6) -0.043(6) 0.023(5) -0.018(6) C20 0.039(7) 0.038(7) 0.042(8) 0.006(6) -0.001(6) -0.005(6) C21 0.041(8) 0.062(10) 0.039(8) 0.002(7) -0.010(6) 0.010(7) C22 0.048(8) 0.038(8) 0.060(10) -0.001(7) -0.008(7) 0.013(7) C23 0.044(11) 0.039(10) 0.045(11) -0.003(9) -0.011(9) -0.010(8) C24 0.040(11) 0.042(12) 0.053(12) -0.009(10) -0.008(9) 0.003(9) C25 0.049(12) 0.032(10) 0.075(15) -0.003(10) -0.016(10) 0.009(9) C26 0.041(4) 0.035(4) 0.036(4) 0.001(3) 0.005(3) 0.004(3) C27 0.038(4) 0.037(4) 0.041(4) -0.010(3) 0.012(3) 0.000(3) C28 0.031(4) 0.065(5) 0.026(3) -0.005(4) 0.006(3) 0.001(4) C29 0.026(3) 0.029(4) 0.046(4) 0.014(3) 0.006(3) 0.002(3) C30 0.040(4) 0.035(4) 0.051(5) 0.009(4) -0.003(4) -0.002(3) C31 0.034(4) 0.049(5) 0.081(6) 0.031(5) -0.015(4) 0.002(4) C32 0.042(5) 0.025(4) 0.117(8) 0.012(5) 0.009(5) 0.005(4) C33 0.038(4) 0.031(4) 0.095(7) 0.001(4) 0.012(5) 0.008(4) C34 0.038(4) 0.026(4) 0.057(5) 0.003(3) 0.012(3) 0.004(3) C35 0.025(3) 0.034(4) 0.034(4) -0.001(3) 0.003(3) 0.002(3) C36 0.033(4) 0.035(4) 0.042(4) -0.003(3) 0.004(3) 0.003(3) C37 0.039(4) 0.050(5) 0.049(5) -0.012(4) -0.005(4) 0.002(4) C38 0.027(4) 0.059(5) 0.068(6) -0.014(5) -0.009(4) 0.004(4) C39 0.026(4) 0.044(5) 0.067(5) -0.014(4) 0.009(4) 0.006(3) C40 0.029(4) 0.041(4) 0.043(4) -0.014(3) 0.009(3) -0.002(3) C41 0.024(3) 0.032(4) 0.032(4) -0.003(3) 0.007(3) 0.003(3) C42 0.028(3) 0.032(4) 0.030(3) 0.000(3) 0.007(3) 0.002(3) C43 0.036(4) 0.027(4) 0.035(4) 0.008(3) 0.004(3) 0.001(3) C44 0.031(4) 0.023(3) 0.046(4) 0.004(3) 0.010(3) 0.003(3) C45 0.035(4) 0.031(4) 0.035(4) -0.007(3) 0.013(3) 0.002(3) C46 0.029(3) 0.034(4) 0.028(3) -0.004(3) 0.008(3) 0.001(3) C47 0.040(4) 0.036(4) 0.031(4) -0.003(3) 0.010(3) 0.002(3) C48 0.037(4) 0.037(4) 0.050(5) 0.006(4) 0.019(4) 0.009(3) C49 0.031(4) 0.064(5) 0.028(4) -0.004(4) 0.007(3) 0.012(4) C50 0.052(5) 0.050(5) 0.027(4) 0.000(3) 0.013(3) -0.010(4) C51 0.056(5) 0.051(5) 0.027(4) 0.000(3) 0.001(3) -0.004(4) C52 0.050(5) 0.059(5) 0.030(4) -0.004(4) 0.016(3) 0.010(4) C53 0.052(8) 0.054(8) 0.104(12) 0.017(8) 0.031(8) 0.028(6) C54 0.034(6) 0.090(11) 0.050(8) -0.008(7) 0.011(5) 0.016(6) C55 0.035(6) 0.057(8) 0.051(7) -0.010(6) 0.015(5) 0.016(5) C56 0.07(2) 0.14(4) 0.036(19) -0.01(2) -0.006(17) 0.07(3) C57 0.027(13) 0.039(16) 0.064(19) -0.010(14) -0.001(13) 0.017(12) C58 0.029(15) 0.10(3) 0.08(3) 0.05(2) 0.029(15) 0.025(17) C59 0.039(4) 0.052(5) 0.035(4) -0.012(3) 0.002(3) 0.007(4) C60 0.040(4) 0.081(7) 0.036(4) 0.016(4) 0.011(3) 0.010(4) C61 0.041(5) 0.130(9) 0.030(4) -0.021(5) 0.006(4) 0.016(5) C62 0.059(11) 0.054(11) 0.067(12) -0.008(9) 0.014(9) 0.014(9) Cl1 0.117(5) 0.103(5) 0.064(3) 0.020(3) 0.003(3) -0.034(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.070(5) . ? Cu1 P1 2.2390(19) . ? Cu1 P2 2.2396(18) . ? Cu1 Br1 2.3381(11) . ? P1 C1 1.698(7) . ? P1 C8 1.833(6) . ? C1 C2 1.474(9) . ? C1 C29 1.491(9) . ? C2 N1 1.383(8) . ? C2 C3 1.433(10) . ? C3 C4 1.358(9) . ? C3 H1 0.9500 . ? C4 C5 1.376(9) . ? C4 H2 0.9500 . ? C5 C6 1.417(9) . ? C5 H3 0.9500 . ? C6 N1 1.385(8) . ? C6 C7 1.453(9) . ? C7 C35 1.491(9) . ? C7 P2 1.704(7) . ? P2 C41 1.824(7) . ? C8 C13 1.417(9) . ? C8 C9 1.441(9) . ? C9 C10 1.386(10) . ? C9 C14 1.557(10) . ? C10 C11 1.389(9) . ? C10 H4 0.9500 . ? C11 C12 1.381(9) . ? C11 C15 1.532(9) . ? C12 C13 1.395(9) . ? C12 H5 0.9500 . ? C13 C16 1.557(9) . ? C14 C17 1.534(13) . ? C14 C19 1.551(11) . ? C14 C18 1.556(12) . ? C15 C22 1.464(15) . ? C15 C23 1.482(18) . ? C15 C21 1.517(14) . ? C15 C24 1.54(2) . ? C15 C20 1.600(14) . ? C15 C25 1.61(2) . ? C16 C28 1.520(9) . ? C16 C27 1.539(9) . ? C16 C26 1.544(9) . ? C17 H6 0.9800 . ? C17 H7 0.9800 . ? C17 H8 0.9800 . ? C18 H9 0.9800 . ? C18 H10 0.9800 . ? C18 H11 0.9800 . ? C19 H12 0.9800 . ? C19 H13 0.9800 . ? C19 H14 0.9800 . ? C20 H15 0.9800 . ? C20 H16 0.9800 . ? C20 H17 0.9800 . ? C21 H18 0.9800 . ? C21 H19 0.9800 . ? C21 H20 0.9800 . ? C22 H21 0.9800 . ? C22 H22 0.9800 . ? C22 H23 0.9800 . ? C23 H24 0.9800 . ? C23 H25 0.9800 . ? C23 H26 0.9800 . ? C24 H27 0.9800 . ? C24 H28 0.9800 . ? C24 H29 0.9800 . ? C25 H30 0.9800 . ? C25 H31 0.9800 . ? C25 H32 0.9800 . ? C26 H33 0.9800 . ? C26 H34 0.9800 . ? C26 H35 0.9800 . ? C27 H36 0.9800 . ? C27 H37 0.9800 . ? C27 H38 0.9800 . ? C28 H39 0.9800 . ? C28 H40 0.9800 . ? C28 H41 0.9800 . ? C29 C34 1.386(10) . ? C29 C30 1.404(10) . ? C30 C31 1.392(11) . ? C30 H42 0.9500 . ? C31 C32 1.382(13) . ? C31 H43 0.9500 . ? C32 C33 1.364(13) . ? C32 H44 0.9500 . ? C33 C34 1.398(10) . ? C33 H45 0.9500 . ? C34 H46 0.9500 . ? C35 C40 1.398(9) . ? C35 C36 1.410(9) . ? C36 C37 1.385(10) . ? C36 H47 0.9500 . ? C37 C38 1.373(11) . ? C37 H48 0.9500 . ? C38 C39 1.389(11) . ? C38 H49 0.9500 . ? C39 C40 1.382(10) . ? C39 H50 0.9500 . ? C40 H51 0.9500 . ? C41 C42 1.413(9) . ? C41 C46 1.442(9) . ? C42 C43 1.394(9) . ? C42 C47 1.558(9) . ? C43 C44 1.379(9) . ? C43 H52 0.9500 . ? C44 C45 1.381(10) . ? C44 C48 1.539(9) . ? C45 C46 1.399(9) . ? C45 H53 0.9500 . ? C46 C49 1.553(9) . ? C47 C52 1.533(10) . ? C47 C50 1.538(10) . ? C47 C51 1.545(10) . ? C48 C56 1.33(4) . ? C48 C54 1.460(14) . ? C48 C53 1.542(14) . ? C48 C55 1.585(13) . ? C48 C57 1.62(3) . ? C48 C58 1.65(3) . ? C49 C60 1.529(12) . ? C49 C61 1.531(10) . ? C49 C59 1.550(10) . ? C50 H54 0.9800 . ? C50 H55 0.9800 . ? C50 H56 0.9800 . ? C51 H57 0.9800 . ? C51 H58 0.9800 . ? C51 H59 0.9800 . ? C52 H60 0.9800 . ? C52 H61 0.9800 . ? C52 H62 0.9800 . ? C53 H63 0.9800 . ? C53 H64 0.9800 . ? C53 H65 0.9800 . ? C54 H66 0.9800 . ? C54 H67 0.9800 . ? C54 H68 0.9800 . ? C55 H69 0.9800 . ? C55 H70 0.9800 . ? C55 H71 0.9800 . ? C56 H72 0.9800 . ? C56 H73 0.9800 . ? C56 H74 0.9800 . ? C57 H75 0.9800 . ? C57 H76 0.9800 . ? C57 H77 0.9800 . ? C58 H78 0.9800 . ? C58 H79 0.9800 . ? C58 H80 0.9800 . ? C59 H81 0.9800 . ? C59 H82 0.9800 . ? C59 H83 0.9800 . ? C60 H84 0.9800 . ? C60 H85 0.9800 . ? C60 H86 0.9800 . ? C61 H87 0.9800 . ? C61 H88 0.9800 . ? C61 H89 0.9800 . ? C62 Cl2 1.59(2) . ? C62 Cl1 1.743(19) . ? C62 Cl3 1.86(4) . ? C62 H90 0.9707 . ? C62 H91 0.9732 . ? C62 H92 0.9456 . ? C62 H93 1.0311 . ? Cl2 H93 1.4507 . ? Cl3 Cl3 1.76(7) 3_665 ? Cl3 H91 1.7263 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 P1 82.34(15) . . ? N1 Cu1 P2 81.83(15) . . ? P1 Cu1 P2 143.84(7) . . ? N1 Cu1 Br1 152.32(14) . . ? P1 Cu1 Br1 105.06(6) . . ? P2 Cu1 Br1 104.03(6) . . ? C1 P1 C8 109.1(3) . . ? C1 P1 Cu1 104.2(2) . . ? C8 P1 Cu1 138.8(2) . . ? C2 C1 C29 119.0(6) . . ? C2 C1 P1 113.1(5) . . ? C29 C1 P1 127.7(5) . . ? N1 C2 C3 120.4(6) . . ? N1 C2 C1 117.5(6) . . ? C3 C2 C1 122.0(6) . . ? C4 C3 C2 119.2(7) . . ? C4 C3 H1 120.4 . . ? C2 C3 H1 120.4 . . ? C3 C4 C5 120.9(7) . . ? C3 C4 H2 119.5 . . ? C5 C4 H2 119.5 . . ? C4 C5 C6 119.8(6) . . ? C4 C5 H3 120.1 . . ? C6 C5 H3 120.1 . . ? N1 C6 C5 120.1(6) . . ? N1 C6 C7 118.0(6) . . ? C5 C6 C7 121.7(6) . . ? C2 N1 C6 118.8(6) . . ? C2 N1 Cu1 119.3(4) . . ? C6 N1 Cu1 118.6(4) . . ? C6 C7 C35 120.7(6) . . ? C6 C7 P2 112.4(5) . . ? C35 C7 P2 126.9(5) . . ? C7 P2 C41 111.1(3) . . ? C7 P2 Cu1 103.3(2) . . ? C41 P2 Cu1 139.0(2) . . ? C13 C8 C9 118.9(6) . . ? C13 C8 P1 124.8(5) . . ? C9 C8 P1 115.8(5) . . ? C10 C9 C8 117.8(6) . . ? C10 C9 C14 118.2(6) . . ? C8 C9 C14 123.8(6) . . ? C9 C10 C11 123.5(6) . . ? C9 C10 H4 118.3 . . ? C11 C10 H4 118.3 . . ? C12 C11 C10 117.0(6) . . ? C12 C11 C15 121.3(6) . . ? C10 C11 C15 121.7(6) . . ? C11 C12 C13 123.5(6) . . ? C11 C12 H5 118.2 . . ? C13 C12 H5 118.2 . . ? C12 C13 C8 118.2(6) . . ? C12 C13 C16 113.7(5) . . ? C8 C13 C16 127.9(6) . . ? C17 C14 C19 106.3(8) . . ? C17 C14 C9 109.8(7) . . ? C19 C14 C9 111.1(6) . . ? C17 C14 C18 111.5(7) . . ? C19 C14 C18 105.8(7) . . ? C9 C14 C18 112.1(7) . . ? C22 C15 C23 135.9(11) . . ? C22 C15 C21 111.1(9) . . ? C23 C15 C21 54.5(9) . . ? C22 C15 C11 111.7(8) . . ? C23 C15 C11 112.1(9) . . ? C21 C15 C11 113.2(7) . . ? C22 C15 C24 42.6(9) . . ? C23 C15 C24 111.4(12) . . ? C21 C15 C24 132.0(10) . . ? C11 C15 C24 114.3(8) . . ? C22 C15 C20 109.4(9) . . ? C23 C15 C20 53.1(9) . . ? C21 C15 C20 106.0(9) . . ? C11 C15 C20 105.2(7) . . ? C24 C15 C20 67.8(10) . . ? C22 C15 C25 62.5(10) . . ? C23 C15 C25 110.5(11) . . ? C21 C15 C25 57.3(9) . . ? C11 C15 C25 104.7(9) . . ? C24 C15 C25 103.3(12) . . ? C20 C15 C25 149.8(10) . . ? C28 C16 C27 108.0(6) . . ? C28 C16 C26 105.6(6) . . ? C27 C16 C26 109.1(5) . . ? C28 C16 C13 116.9(5) . . ? C27 C16 C13 110.3(6) . . ? C26 C16 C13 106.7(5) . . ? C14 C17 H6 109.5 . . ? C14 C17 H7 109.5 . . ? H6 C17 H7 109.5 . . ? C14 C17 H8 109.5 . . ? H6 C17 H8 109.5 . . ? H7 C17 H8 109.5 . . ? C14 C18 H9 109.5 . . ? C14 C18 H10 109.5 . . ? H9 C18 H10 109.5 . . ? C14 C18 H11 109.5 . . ? H9 C18 H11 109.5 . . ? H10 C18 H11 109.5 . . ? C14 C19 H12 109.5 . . ? C14 C19 H13 109.5 . . ? H12 C19 H13 109.5 . . ? C14 C19 H14 109.5 . . ? H12 C19 H14 109.5 . . ? H13 C19 H14 109.5 . . ? C15 C20 H15 109.5 . . ? C15 C20 H16 109.5 . . ? H15 C20 H16 109.5 . . ? C15 C20 H17 109.5 . . ? H15 C20 H17 109.5 . . ? H16 C20 H17 109.5 . . ? C15 C21 H18 109.5 . . ? C15 C21 H19 109.5 . . ? H18 C21 H19 109.5 . . ? C15 C21 H20 109.5 . . ? H18 C21 H20 109.5 . . ? H19 C21 H20 109.5 . . ? C15 C22 H21 109.5 . . ? C15 C22 H22 109.5 . . ? H21 C22 H22 109.5 . . ? C15 C22 H23 109.5 . . ? H21 C22 H23 109.5 . . ? H22 C22 H23 109.5 . . ? C15 C23 H24 109.5 . . ? C15 C23 H25 109.5 . . ? H24 C23 H25 109.5 . . ? C15 C23 H26 109.5 . . ? H24 C23 H26 109.5 . . ? H25 C23 H26 109.5 . . ? C15 C24 H27 109.5 . . ? C15 C24 H28 109.5 . . ? H27 C24 H28 109.5 . . ? C15 C24 H29 109.5 . . ? H27 C24 H29 109.5 . . ? H28 C24 H29 109.5 . . ? C15 C25 H30 109.5 . . ? C15 C25 H31 109.5 . . ? H30 C25 H31 109.5 . . ? C15 C25 H32 109.5 . . ? H30 C25 H32 109.5 . . ? H31 C25 H32 109.5 . . ? C16 C26 H33 109.5 . . ? C16 C26 H34 109.5 . . ? H33 C26 H34 109.5 . . ? C16 C26 H35 109.5 . . ? H33 C26 H35 109.5 . . ? H34 C26 H35 109.5 . . ? C16 C27 H36 109.5 . . ? C16 C27 H37 109.5 . . ? H36 C27 H37 109.5 . . ? C16 C27 H38 109.5 . . ? H36 C27 H38 109.5 . . ? H37 C27 H38 109.5 . . ? C16 C28 H39 109.5 . . ? C16 C28 H40 109.5 . . ? H39 C28 H40 109.5 . . ? C16 C28 H41 109.5 . . ? H39 C28 H41 109.5 . . ? H40 C28 H41 109.5 . . ? C34 C29 C30 117.7(7) . . ? C34 C29 C1 121.2(6) . . ? C30 C29 C1 121.0(7) . . ? C31 C30 C29 120.0(8) . . ? C31 C30 H42 120.0 . . ? C29 C30 H42 120.0 . . ? C32 C31 C30 121.2(8) . . ? C32 C31 H43 119.4 . . ? C30 C31 H43 119.4 . . ? C33 C32 C31 119.1(8) . . ? C33 C32 H44 120.4 . . ? C31 C32 H44 120.4 . . ? C32 C33 C34 120.5(8) . . ? C32 C33 H45 119.7 . . ? C34 C33 H45 119.7 . . ? C29 C34 C33 121.3(8) . . ? C29 C34 H46 119.3 . . ? C33 C34 H46 119.3 . . ? C40 C35 C36 118.0(6) . . ? C40 C35 C7 121.6(6) . . ? C36 C35 C7 120.3(6) . . ? C37 C36 C35 120.3(7) . . ? C37 C36 H47 119.9 . . ? C35 C36 H47 119.9 . . ? C38 C37 C36 120.6(7) . . ? C38 C37 H48 119.7 . . ? C36 C37 H48 119.7 . . ? C37 C38 C39 120.0(7) . . ? C37 C38 H49 120.0 . . ? C39 C38 H49 120.0 . . ? C40 C39 C38 120.0(7) . . ? C40 C39 H50 120.0 . . ? C38 C39 H50 120.0 . . ? C39 C40 C35 121.0(7) . . ? C39 C40 H51 119.5 . . ? C35 C40 H51 119.5 . . ? C42 C41 C46 119.6(6) . . ? C42 C41 P2 125.3(5) . . ? C46 C41 P2 114.7(5) . . ? C43 C42 C41 117.8(6) . . ? C43 C42 C47 113.1(6) . . ? C41 C42 C47 129.0(6) . . ? C44 C43 C42 123.6(6) . . ? C44 C43 H52 118.2 . . ? C42 C43 H52 118.2 . . ? C43 C44 C45 117.5(6) . . ? C43 C44 C48 120.2(6) . . ? C45 C44 C48 122.3(6) . . ? C44 C45 C46 122.9(6) . . ? C44 C45 H53 118.5 . . ? C46 C45 H53 118.5 . . ? C45 C46 C41 117.5(6) . . ? C45 C46 C49 117.7(6) . . ? C41 C46 C49 124.8(6) . . ? C52 C47 C50 107.3(6) . . ? C52 C47 C51 106.1(6) . . ? C50 C47 C51 109.6(6) . . ? C52 C47 C42 116.8(6) . . ? C50 C47 C42 106.8(6) . . ? C51 C47 C42 110.0(6) . . ? C56 C48 C54 134.3(17) . . ? C56 C48 C44 114.6(16) . . ? C54 C48 C44 110.9(7) . . ? C56 C48 C53 55.9(18) . . ? C54 C48 C53 112.8(10) . . ? C44 C48 C53 108.0(7) . . ? C56 C48 C55 50.7(18) . . ? C54 C48 C55 108.6(8) . . ? C44 C48 C55 111.0(7) . . ? C53 C48 C55 105.5(9) . . ? C56 C48 C57 112.4(18) . . ? C54 C48 C57 49.6(12) . . ? C44 C48 C57 112.7(10) . . ? C53 C48 C57 65.5(12) . . ? C55 C48 C57 135.9(11) . . ? C56 C48 C58 116(2) . . ? C54 C48 C58 47.8(14) . . ? C44 C48 C58 102.1(11) . . ? C53 C48 C58 149.2(12) . . ? C55 C48 C58 68.7(15) . . ? C57 C48 C58 96.9(17) . . ? C60 C49 C61 105.4(7) . . ? C60 C49 C46 113.4(6) . . ? C61 C49 C46 111.9(6) . . ? C60 C49 C59 110.7(6) . . ? C61 C49 C59 105.1(6) . . ? C46 C49 C59 109.9(6) . . ? C47 C50 H54 109.5 . . ? C47 C50 H55 109.5 . . ? H54 C50 H55 109.5 . . ? C47 C50 H56 109.5 . . ? H54 C50 H56 109.5 . . ? H55 C50 H56 109.5 . . ? C47 C51 H57 109.5 . . ? C47 C51 H58 109.5 . . ? H57 C51 H58 109.5 . . ? C47 C51 H59 109.5 . . ? H57 C51 H59 109.5 . . ? H58 C51 H59 109.5 . . ? C47 C52 H60 109.5 . . ? C47 C52 H61 109.5 . . ? H60 C52 H61 109.5 . . ? C47 C52 H62 109.5 . . ? H60 C52 H62 109.5 . . ? H61 C52 H62 109.5 . . ? C48 C53 H63 109.5 . . ? C48 C53 H64 109.5 . . ? H63 C53 H64 109.5 . . ? C48 C53 H65 109.5 . . ? H63 C53 H65 109.5 . . ? H64 C53 H65 109.5 . . ? C48 C54 H66 109.5 . . ? C48 C54 H67 109.5 . . ? H66 C54 H67 109.5 . . ? C48 C54 H68 109.5 . . ? H66 C54 H68 109.5 . . ? H67 C54 H68 109.5 . . ? C48 C55 H69 109.5 . . ? C48 C55 H70 109.5 . . ? H69 C55 H70 109.5 . . ? C48 C55 H71 109.5 . . ? H69 C55 H71 109.5 . . ? H70 C55 H71 109.5 . . ? C48 C56 H72 109.5 . . ? C48 C56 H73 109.5 . . ? H72 C56 H73 109.5 . . ? C48 C56 H74 109.5 . . ? H72 C56 H74 109.5 . . ? H73 C56 H74 109.5 . . ? C48 C57 H75 109.5 . . ? C48 C57 H76 109.5 . . ? H75 C57 H76 109.5 . . ? C48 C57 H77 109.5 . . ? H75 C57 H77 109.5 . . ? H76 C57 H77 109.5 . . ? C48 C58 H78 109.5 . . ? C48 C58 H79 109.5 . . ? H78 C58 H79 109.5 . . ? C48 C58 H80 109.5 . . ? H78 C58 H80 109.5 . . ? H79 C58 H80 109.5 . . ? C49 C59 H81 109.5 . . ? C49 C59 H82 109.5 . . ? H81 C59 H82 109.5 . . ? C49 C59 H83 109.5 . . ? H81 C59 H83 109.5 . . ? H82 C59 H83 109.5 . . ? C49 C60 H84 109.5 . . ? C49 C60 H85 109.5 . . ? H84 C60 H85 109.5 . . ? C49 C60 H86 109.5 . . ? H84 C60 H86 109.5 . . ? H85 C60 H86 109.5 . . ? C49 C61 H87 109.5 . . ? C49 C61 H88 109.5 . . ? H87 C61 H88 109.5 . . ? C49 C61 H89 109.5 . . ? H87 C61 H89 109.5 . . ? H88 C61 H89 109.5 . . ? Cl2 C62 Cl1 121.2(12) . . ? Cl2 C62 Cl3 41.4(12) . . ? Cl1 C62 Cl3 124.5(16) . . ? Cl2 C62 H90 107.2 . . ? Cl1 C62 H90 106.2 . . ? Cl3 C62 H90 128.7 . . ? Cl2 C62 H91 107.1 . . ? Cl1 C62 H91 105.3 . . ? Cl3 C62 H91 66.6 . . ? H90 C62 H91 109.5 . . ? Cl2 C62 H92 129.3 . . ? Cl1 C62 H92 109.4 . . ? Cl3 C62 H92 105.7 . . ? H90 C62 H92 58.5 . . ? H91 C62 H92 51.9 . . ? Cl2 C62 H93 63.2 . . ? Cl1 C62 H93 107.6 . . ? Cl3 C62 H93 101.8 . . ? H90 C62 H93 51.1 . . ? H91 C62 H93 145.6 . . ? H92 C62 H93 106.5 . . ? C62 Cl2 H93 39.4 . . ? C62 Cl3 Cl3 81(3) . 3_665 ? C62 Cl3 H91 31.1 . . ? Cl3 Cl3 H91 54.7 3_665 . ? 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 P1 C1 -11.7(3) . . . . ? P2 Cu1 P1 C1 -76.4(3) . . . . ? Br1 Cu1 P1 C1 141.1(2) . . . . ? N1 Cu1 P1 C8 -154.9(3) . . . . ? P2 Cu1 P1 C8 140.4(3) . . . . ? Br1 Cu1 P1 C8 -2.2(3) . . . . ? C8 P1 C1 C2 175.0(4) . . . . ? Cu1 P1 C1 C2 19.6(5) . . . . ? C8 P1 C1 C29 -9.8(7) . . . . ? Cu1 P1 C1 C29 -165.2(5) . . . . ? C29 C1 C2 N1 164.6(6) . . . . ? P1 C1 C2 N1 -19.7(7) . . . . ? C29 C1 C2 C3 -19.3(9) . . . . ? P1 C1 C2 C3 156.3(5) . . . . ? N1 C2 C3 C4 0.1(10) . . . . ? C1 C2 C3 C4 -175.8(6) . . . . ? C2 C3 C4 C5 5.8(10) . . . . ? C3 C4 C5 C6 -3.7(10) . . . . ? C4 C5 C6 N1 -4.4(9) . . . . ? C4 C5 C6 C7 170.5(6) . . . . ? C3 C2 N1 C6 -8.0(9) . . . . ? C1 C2 N1 C6 168.1(5) . . . . ? C3 C2 N1 Cu1 -167.1(5) . . . . ? C1 C2 N1 Cu1 9.0(7) . . . . ? C5 C6 N1 C2 10.1(9) . . . . ? C7 C6 N1 C2 -165.0(5) . . . . ? C5 C6 N1 Cu1 169.4(4) . . . . ? C7 C6 N1 Cu1 -5.7(7) . . . . ? P1 Cu1 N1 C2 3.1(4) . . . . ? P2 Cu1 N1 C2 150.4(4) . . . . ? Br1 Cu1 N1 C2 -104.9(5) . . . . ? P1 Cu1 N1 C6 -156.1(4) . . . . ? P2 Cu1 N1 C6 -8.7(4) . . . . ? Br1 Cu1 N1 C6 96.0(5) . . . . ? N1 C6 C7 C35 -160.1(6) . . . . ? C5 C6 C7 C35 24.9(9) . . . . ? N1 C6 C7 P2 22.1(7) . . . . ? C5 C6 C7 P2 -152.9(5) . . . . ? C6 C7 P2 C41 177.1(4) . . . . ? C35 C7 P2 C41 -0.5(7) . . . . ? C6 C7 P2 Cu1 -25.6(5) . . . . ? C35 C7 P2 Cu1 156.8(5) . . . . ? N1 Cu1 P2 C7 17.3(3) . . . . ? P1 Cu1 P2 C7 82.2(3) . . . . ? Br1 Cu1 P2 C7 -135.1(2) . . . . ? N1 Cu1 P2 C41 164.1(4) . . . . ? P1 Cu1 P2 C41 -131.0(3) . . . . ? Br1 Cu1 P2 C41 11.7(3) . . . . ? C1 P1 C8 C13 -57.0(7) . . . . ? Cu1 P1 C8 C13 85.1(6) . . . . ? C1 P1 C8 C9 114.6(6) . . . . ? Cu1 P1 C8 C9 -103.2(5) . . . . ? C13 C8 C9 C10 11.6(10) . . . . ? P1 C8 C9 C10 -160.6(6) . . . . ? C13 C8 C9 C14 -164.7(7) . . . . ? P1 C8 C9 C14 23.1(10) . . . . ? C8 C9 C10 C11 -4.3(11) . . . . ? C14 C9 C10 C11 172.3(7) . . . . ? C9 C10 C11 C12 -4.1(11) . . . . ? C9 C10 C11 C15 177.7(7) . . . . ? C10 C11 C12 C13 5.4(10) . . . . ? C15 C11 C12 C13 -176.4(6) . . . . ? C11 C12 C13 C8 2.0(10) . . . . ? C11 C12 C13 C16 -172.8(6) . . . . ? C9 C8 C13 C12 -10.5(10) . . . . ? P1 C8 C13 C12 160.9(5) . . . . ? C9 C8 C13 C16 163.5(7) . . . . ? P1 C8 C13 C16 -25.1(10) . . . . ? C10 C9 C14 C17 -123.4(8) . . . . ? C8 C9 C14 C17 52.9(10) . . . . ? C10 C9 C14 C19 -6.0(11) . . . . ? C8 C9 C14 C19 170.3(8) . . . . ? C10 C9 C14 C18 112.1(8) . . . . ? C8 C9 C14 C18 -71.6(10) . . . . ? C12 C11 C15 C22 47.3(11) . . . . ? C10 C11 C15 C22 -134.6(10) . . . . ? C12 C11 C15 C23 -127.1(10) . . . . ? C10 C11 C15 C23 51.0(12) . . . . ? C12 C11 C15 C21 173.5(9) . . . . ? C10 C11 C15 C21 -8.4(11) . . . . ? C12 C11 C15 C24 0.9(13) . . . . ? C10 C11 C15 C24 179.0(11) . . . . ? C12 C11 C15 C20 -71.2(9) . . . . ? C10 C11 C15 C20 106.9(9) . . . . ? C12 C11 C15 C25 113.2(10) . . . . ? C10 C11 C15 C25 -68.7(11) . . . . ? C12 C13 C16 C28 178.2(6) . . . . ? C8 C13 C16 C28 4.0(10) . . . . ? C12 C13 C16 C27 -57.9(7) . . . . ? C8 C13 C16 C27 127.9(7) . . . . ? C12 C13 C16 C26 60.5(7) . . . . ? C8 C13 C16 C26 -113.8(7) . . . . ? C2 C1 C29 C34 -45.5(9) . . . . ? P1 C1 C29 C34 139.5(6) . . . . ? C2 C1 C29 C30 133.8(7) . . . . ? P1 C1 C29 C30 -41.2(9) . . . . ? C34 C29 C30 C31 -0.3(11) . . . . ? C1 C29 C30 C31 -179.7(7) . . . . ? C29 C30 C31 C32 1.6(12) . . . . ? C30 C31 C32 C33 -0.8(13) . . . . ? C31 C32 C33 C34 -1.2(13) . . . . ? C30 C29 C34 C33 -1.6(11) . . . . ? C1 C29 C34 C33 177.8(7) . . . . ? C32 C33 C34 C29 2.4(12) . . . . ? C6 C7 C35 C40 -135.0(7) . . . . ? P2 C7 C35 C40 42.4(9) . . . . ? C6 C7 C35 C36 47.3(9) . . . . ? P2 C7 C35 C36 -135.2(6) . . . . ? C40 C35 C36 C37 -2.4(11) . . . . ? C7 C35 C36 C37 175.4(7) . . . . ? C35 C36 C37 C38 1.4(12) . . . . ? C36 C37 C38 C39 -0.1(14) . . . . ? C37 C38 C39 C40 -0.1(13) . . . . ? C38 C39 C40 C35 -0.9(12) . . . . ? C36 C35 C40 C39 2.2(11) . . . . ? C7 C35 C40 C39 -175.6(7) . . . . ? C7 P2 C41 C42 59.2(7) . . . . ? Cu1 P2 C41 C42 -85.9(7) . . . . ? C7 P2 C41 C46 -113.4(5) . . . . ? Cu1 P2 C41 C46 101.5(5) . . . . ? C46 C41 C42 C43 8.9(10) . . . . ? P2 C41 C42 C43 -163.4(5) . . . . ? C46 C41 C42 C47 -166.7(7) . . . . ? P2 C41 C42 C47 21.0(10) . . . . ? C41 C42 C43 C44 -0.2(10) . . . . ? C47 C42 C43 C44 176.0(6) . . . . ? C42 C43 C44 C45 -7.0(10) . . . . ? C42 C43 C44 C48 175.0(7) . . . . ? C43 C44 C45 C46 5.6(10) . . . . ? C48 C44 C45 C46 -176.5(7) . . . . ? C44 C45 C46 C41 2.8(10) . . . . ? C44 C45 C46 C49 -177.0(7) . . . . ? C42 C41 C46 C45 -10.1(10) . . . . ? P2 C41 C46 C45 163.0(5) . . . . ? C42 C41 C46 C49 169.6(7) . . . . ? P2 C41 C46 C49 -17.2(9) . . . . ? C43 C42 C47 C52 179.0(6) . . . . ? C41 C42 C47 C52 -5.2(11) . . . . ? C43 C42 C47 C50 -60.9(8) . . . . ? C41 C42 C47 C50 114.9(8) . . . . ? C43 C42 C47 C51 58.1(8) . . . . ? C41 C42 C47 C51 -126.2(8) . . . . ? C43 C44 C48 C56 119(2) . . . . ? C45 C44 C48 C56 -59(2) . . . . ? C43 C44 C48 C54 -65.0(10) . . . . ? C45 C44 C48 C54 117.1(9) . . . . ? C43 C44 C48 C53 59.0(11) . . . . ? C45 C44 C48 C53 -118.9(9) . . . . ? C43 C44 C48 C55 174.1(8) . . . . ? C45 C44 C48 C55 -3.7(10) . . . . ? C43 C44 C48 C57 -11.3(15) . . . . ? C45 C44 C48 C57 170.8(13) . . . . ? C43 C44 C48 C58 -114.3(16) . . . . ? C45 C44 C48 C58 67.9(16) . . . . ? C45 C46 C49 C60 -111.3(7) . . . . ? C41 C46 C49 C60 68.9(9) . . . . ? C45 C46 C49 C61 7.8(10) . . . . ? C41 C46 C49 C61 -172.0(7) . . . . ? C45 C46 C49 C59 124.1(7) . . . . ? C41 C46 C49 C59 -55.6(9) . . . . ? Cl2 C62 Cl3 Cl3 -164(4) . . . 3_665 ? Cl1 C62 Cl3 Cl3 -64(3) . . . 3_665 ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.012 _refine_diff_density_min -0.879 _refine_diff_density_rms 0.101 # Attachment '2b.CIF' data_2b _database_code_depnum_ccdc_archive 'CCDC 812262' #TrackingRef '2b.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H71 Cu F6 N P2 Sb' _chemical_formula_weight 1107.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.715(2) _cell_length_b 24.683(5) _cell_length_c 19.400(4) _cell_angle_alpha 90.00 _cell_angle_beta 106.209(3) _cell_angle_gamma 90.00 _cell_volume 5386.7(18) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour dark-red _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.31 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2288 _exptl_absorpt_coefficient_mu 1.012 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.7248 _exptl_absorpt_correction_T_max 0.7444 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _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 51160 _diffrn_reflns_av_R_equivalents 0.0565 _diffrn_reflns_av_sigmaI/netI 0.0585 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 31.62 _reflns_number_total 16150 _reflns_number_gt 13650 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rigaku AFC10/Saturn 70 CCD' _computing_cell_refinement 'Rigaku AFC10/Saturn 70 CCD' _computing_data_reduction 'Rigaku AFC10/Saturn 70 CCD' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'ORTEP3 for windows' _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^)+(0.1000P)^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 16150 _refine_ls_number_parameters 610 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1036 _refine_ls_R_factor_gt 0.0875 _refine_ls_wR_factor_ref 0.2367 _refine_ls_wR_factor_gt 0.2270 _refine_ls_goodness_of_fit_ref 1.396 _refine_ls_restrained_S_all 1.396 _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 -0.20092(4) -0.13953(2) -0.08612(3) 0.02757(13) Uani 1 1 d . . . P1 P -0.07510(8) -0.16632(4) 0.01935(5) 0.0259(2) Uani 1 1 d . . . P2 P -0.30491(8) -0.08004(4) -0.16783(5) 0.0257(2) Uani 1 1 d . . . N1 N -0.0587(3) -0.08808(14) -0.08871(17) 0.0239(6) Uani 1 1 d . . . C1 C 0.0400(3) -0.08960(16) -0.0316(2) 0.0243(7) Uani 1 1 d . . . C2 C 0.1225(3) -0.04733(17) -0.0172(2) 0.0287(8) Uani 1 1 d . . . H1 H 0.1931 -0.0498 0.0214 0.034 Uiso 1 1 calc R . . C3 C 0.0991(4) -0.00153(18) -0.0607(2) 0.0317(9) Uani 1 1 d . . . H2 H 0.1541 0.0277 -0.0523 0.038 Uiso 1 1 calc R . . C4 C -0.0049(4) 0.00132(18) -0.1162(2) 0.0313(8) Uani 1 1 d . . . H3 H -0.0226 0.0328 -0.1454 0.038 Uiso 1 1 calc R . . C5 C -0.0835(3) -0.04255(17) -0.1292(2) 0.0248(7) Uani 1 1 d . . . C6 C 0.0559(3) -0.13655(16) 0.0181(2) 0.0243(7) Uani 1 1 d . . . C7 C 0.1767(3) -0.15079(17) 0.0610(2) 0.0262(7) Uani 1 1 d . . . C8 C 0.2048(4) -0.16035(19) 0.1349(2) 0.0318(9) Uani 1 1 d . . . H4 H 0.1451 -0.1566 0.1591 0.038 Uiso 1 1 calc R . . C9 C 0.3197(4) -0.1754(2) 0.1734(3) 0.0383(10) Uani 1 1 d . . . H5 H 0.3378 -0.1816 0.2236 0.046 Uiso 1 1 calc R . . C10 C 0.4080(4) -0.1813(2) 0.1386(3) 0.0397(11) Uani 1 1 d . . . H6 H 0.4860 -0.1919 0.1648 0.048 Uiso 1 1 calc R . . C11 C 0.3811(4) -0.1715(2) 0.0647(3) 0.0388(10) Uani 1 1 d . . . H7 H 0.4407 -0.1758 0.0404 0.047 Uiso 1 1 calc R . . C12 C 0.2672(4) -0.15557(19) 0.0269(2) 0.0319(9) Uani 1 1 d . . . H8 H 0.2502 -0.1478 -0.0229 0.038 Uiso 1 1 calc R . . C13 C -0.1994(3) -0.03872(16) -0.1842(2) 0.0251(7) Uani 1 1 d . . . C14 C -0.2136(4) 0.00151(18) -0.2427(2) 0.0311(8) Uani 1 1 d . . . C15 C -0.1301(4) 0.0025(2) -0.2821(3) 0.0423(11) Uani 1 1 d . . . H9 H -0.0650 -0.0220 -0.2709 0.051 Uiso 1 1 calc R . . C16 C -0.1427(6) 0.0399(3) -0.3381(3) 0.0597(17) Uani 1 1 d . . . H10 H -0.0860 0.0404 -0.3648 0.072 Uiso 1 1 calc R . . C17 C -0.2358(6) 0.0757(3) -0.3548(3) 0.0620(17) Uani 1 1 d . . . H11 H -0.2430 0.1009 -0.3928 0.074 Uiso 1 1 calc R . . C18 C -0.3180(5) 0.0752(2) -0.3172(3) 0.0506(14) Uani 1 1 d . . . H12 H -0.3820 0.1003 -0.3289 0.061 Uiso 1 1 calc R . . C19 C -0.3090(4) 0.03785(19) -0.2612(3) 0.0363(10) Uani 1 1 d . . . H13 H -0.3677 0.0373 -0.2358 0.044 Uiso 1 1 calc R . . C20 C -0.0399(3) -0.22360(17) 0.0806(2) 0.0254(7) Uani 1 1 d . . . C21 C -0.0671(3) -0.21889(17) 0.1484(2) 0.0268(7) Uani 1 1 d . . . C22 C -0.0071(4) -0.25278(19) 0.2038(2) 0.0311(8) Uani 1 1 d . . . H14 H -0.0222 -0.2492 0.2492 0.037 Uiso 1 1 calc R . . C23 C 0.0745(4) -0.29197(19) 0.1958(2) 0.0336(9) Uani 1 1 d . A . C24 C 0.0853(4) -0.30024(18) 0.1274(2) 0.0320(8) Uani 1 1 d . . . H15 H 0.1338 -0.3293 0.1202 0.038 Uiso 1 1 calc R . . C25 C 0.0284(4) -0.26806(17) 0.0680(2) 0.0279(8) Uani 1 1 d . . . C26 C -0.1566(4) -0.17744(17) 0.1638(2) 0.0287(8) Uani 1 1 d . . . C27 C -0.1051(4) -0.12015(19) 0.1711(3) 0.0362(9) Uani 1 1 d . . . H18 H -0.1622 -0.0949 0.1819 0.054 Uiso 1 1 calc R . . H19 H -0.0890 -0.1095 0.1260 0.054 Uiso 1 1 calc R . . H20 H -0.0309 -0.1193 0.2101 0.054 Uiso 1 1 calc R . . C28 C -0.2764(4) -0.1797(2) 0.1046(3) 0.0373(10) Uani 1 1 d . . . H21 H -0.3323 -0.1540 0.1162 0.056 Uiso 1 1 calc R . . H22 H -0.3091 -0.2164 0.1019 0.056 Uiso 1 1 calc R . . H23 H -0.2638 -0.1699 0.0583 0.056 Uiso 1 1 calc R . . C29 C -0.1847(5) -0.1891(2) 0.2351(3) 0.0386(10) Uani 1 1 d . . . H24 H -0.1169 -0.1785 0.2752 0.058 Uiso 1 1 calc R . . H25 H -0.2002 -0.2279 0.2385 0.058 Uiso 1 1 calc R . . H26 H -0.2551 -0.1684 0.2372 0.058 Uiso 1 1 calc R . . C30 C 0.1465(5) -0.3243(2) 0.2605(3) 0.0447(12) Uani 1 1 d . . . C31 C 0.0624(7) -0.3568(3) 0.2919(3) 0.0641(18) Uani 1 1 d . A . H54 H 0.0062 -0.3322 0.3050 0.096 Uiso 1 1 calc R . . H55 H 0.1083 -0.3762 0.3348 0.096 Uiso 1 1 calc R . . H56 H 0.0186 -0.3829 0.2562 0.096 Uiso 1 1 calc R . . C32 C 0.2155(5) -0.2837(3) 0.3189(3) 0.0539(15) Uani 1 1 d . A . H57 H 0.2689 -0.2618 0.2994 0.081 Uiso 1 1 calc R . . H58 H 0.2621 -0.3039 0.3609 0.081 Uiso 1 1 calc R . . H59 H 0.1589 -0.2600 0.3331 0.081 Uiso 1 1 calc R . . C33A C 0.2622(16) -0.3492(8) 0.2464(8) 0.044(4) Uiso 0.42(3) 1 d P A 3 H60 H 0.2397 -0.3780 0.2104 0.067 Uiso 0.42(3) 1 calc PR A 3 H61 H 0.3131 -0.3643 0.2912 0.067 Uiso 0.42(3) 1 calc PR A 3 H62 H 0.3055 -0.3208 0.2290 0.067 Uiso 0.42(3) 1 calc PR A 3 C33B C 0.2242(13) -0.3683(6) 0.2400(6) 0.048(3) Uiso 0.58(3) 1 d P A 4 H63 H 0.1740 -0.3926 0.2042 0.073 Uiso 0.58(3) 1 calc PR A 4 H64 H 0.2649 -0.3891 0.2828 0.073 Uiso 0.58(3) 1 calc PR A 4 H65 H 0.2834 -0.3512 0.2200 0.073 Uiso 0.58(3) 1 calc PR A 4 C34 C 0.0435(4) -0.28954(19) -0.0043(2) 0.0325(9) Uani 1 1 d . . . C35 C -0.0244(5) -0.3437(2) -0.0193(3) 0.0476(12) Uani 1 1 d . . . H27 H 0.0022 -0.3674 0.0227 0.071 Uiso 1 1 calc R . . H28 H -0.0088 -0.3613 -0.0610 0.071 Uiso 1 1 calc R . . H29 H -0.1099 -0.3369 -0.0290 0.071 Uiso 1 1 calc R . . C36 C 0.1760(5) -0.2986(2) 0.0007(3) 0.0415(11) Uani 1 1 d . . . H30 H 0.2197 -0.2646 0.0141 0.062 Uiso 1 1 calc R . . H31 H 0.1834 -0.3108 -0.0459 0.062 Uiso 1 1 calc R . . H32 H 0.2090 -0.3262 0.0371 0.062 Uiso 1 1 calc R . . C37 C -0.0077(5) -0.2537(2) -0.0715(2) 0.0422(11) Uani 1 1 d . . . H33 H -0.0901 -0.2441 -0.0746 0.063 Uiso 1 1 calc R . . H34 H -0.0053 -0.2738 -0.1147 0.063 Uiso 1 1 calc R . . H35 H 0.0399 -0.2207 -0.0677 0.063 Uiso 1 1 calc R . . C38 C -0.4460(3) -0.06798(16) -0.2355(2) 0.0250(7) Uani 1 1 d . . . C39 C -0.4663(4) -0.08306(18) -0.3088(2) 0.0277(8) Uani 1 1 d . . . C40 C -0.5613(4) -0.0582(2) -0.3591(2) 0.0332(9) Uani 1 1 d . . . H16 H -0.5741 -0.0667 -0.4084 0.040 Uiso 1 1 calc R . . C41 C -0.6377(4) -0.02172(18) -0.3403(2) 0.0323(9) Uani 1 1 d . B . C42 C -0.6225(3) -0.01236(18) -0.2680(2) 0.0311(8) Uani 1 1 d . . . H17 H -0.6775 0.0108 -0.2545 0.037 Uiso 1 1 calc R . . C43 C -0.5305(3) -0.03512(17) -0.2136(2) 0.0278(8) Uani 1 1 d . . . C44 C -0.3988(4) -0.12603(19) -0.3410(2) 0.0346(9) Uani 1 1 d . . . C45 C -0.2968(6) -0.1550(3) -0.2878(3) 0.0547(15) Uani 1 1 d . . . H36 H -0.2647 -0.1831 -0.3128 0.082 Uiso 1 1 calc R . . H37 H -0.3259 -0.1717 -0.2501 0.082 Uiso 1 1 calc R . . H38 H -0.2341 -0.1288 -0.2661 0.082 Uiso 1 1 calc R . . C46 C -0.3492(6) -0.1004(3) -0.3979(3) 0.0572(15) Uani 1 1 d . . . H39 H -0.2941 -0.0712 -0.3763 0.086 Uiso 1 1 calc R . . H40 H -0.4145 -0.0856 -0.4365 0.086 Uiso 1 1 calc R . . H41 H -0.3068 -0.1279 -0.4177 0.086 Uiso 1 1 calc R . . C47 C -0.4911(6) -0.1699(3) -0.3760(4) 0.0573(16) Uani 1 1 d . . . H42 H -0.4535 -0.1972 -0.3992 0.086 Uiso 1 1 calc R . . H43 H -0.5574 -0.1530 -0.4119 0.086 Uiso 1 1 calc R . . H44 H -0.5209 -0.1873 -0.3390 0.086 Uiso 1 1 calc R . . C48 C -0.7356(5) 0.0074(2) -0.3979(3) 0.0423(11) Uiso 1 1 d . . . C49 C -0.8152(10) 0.0453(5) -0.3636(6) 0.055(3) Uiso 0.558(11) 1 d P B 1 H66 H -0.8812 0.0600 -0.4019 0.082 Uiso 0.558(11) 1 calc PR B 1 H67 H -0.7667 0.0751 -0.3375 0.082 Uiso 0.558(11) 1 calc PR B 1 H68 H -0.8468 0.0240 -0.3304 0.082 Uiso 0.558(11) 1 calc PR B 1 C50 C -0.8203(11) -0.0358(5) -0.4407(7) 0.062(3) Uiso 0.558(11) 1 d P B 1 H69 H -0.8545 -0.0565 -0.4083 0.093 Uiso 0.558(11) 1 calc PR B 1 H70 H -0.7764 -0.0602 -0.4638 0.093 Uiso 0.558(11) 1 calc PR B 1 H71 H -0.8843 -0.0181 -0.4775 0.093 Uiso 0.558(11) 1 calc PR B 1 C51 C -0.6826(11) 0.0417(5) -0.4445(7) 0.058(3) Uiso 0.558(11) 1 d P B 1 H72 H -0.7462 0.0600 -0.4808 0.087 Uiso 0.558(11) 1 calc PR B 1 H73 H -0.6369 0.0187 -0.4684 0.087 Uiso 0.558(11) 1 calc PR B 1 H74 H -0.6298 0.0688 -0.4150 0.087 Uiso 0.558(11) 1 calc PR B 1 C52 C -0.7504(15) -0.0162(7) -0.4758(9) 0.067(4) Uiso 0.442(11) 1 d P B 2 H75 H -0.7730 -0.0545 -0.4769 0.101 Uiso 0.442(11) 1 calc PR B 2 H76 H -0.6751 -0.0127 -0.4881 0.101 Uiso 0.442(11) 1 calc PR B 2 H77 H -0.8125 0.0041 -0.5106 0.101 Uiso 0.442(11) 1 calc PR B 2 C53 C -0.6831(18) 0.0649(8) -0.4049(11) 0.079(5) Uiso 0.442(11) 1 d P B 2 H78 H -0.7457 0.0881 -0.4343 0.118 Uiso 0.442(11) 1 calc PR B 2 H79 H -0.6185 0.0615 -0.4276 0.118 Uiso 0.442(11) 1 calc PR B 2 H80 H -0.6523 0.0809 -0.3570 0.118 Uiso 0.442(11) 1 calc PR B 2 C54 C -0.8482(19) 0.0078(9) -0.3822(11) 0.084(6) Uiso 0.442(11) 1 d P B 2 H81 H -0.8390 0.0244 -0.3351 0.126 Uiso 0.442(11) 1 calc PR B 2 H82 H -0.8769 -0.0294 -0.3818 0.126 Uiso 0.442(11) 1 calc PR B 2 H83 H -0.9055 0.0288 -0.4190 0.126 Uiso 0.442(11) 1 calc PR B 2 C55 C -0.5273(4) -0.0240(2) -0.1344(2) 0.0336(9) Uani 1 1 d . . . C56 C -0.5148(4) -0.0766(2) -0.0909(2) 0.0394(10) Uani 1 1 d . . . H45 H -0.4400 -0.0945 -0.0905 0.059 Uiso 1 1 calc R . . H46 H -0.5816 -0.1007 -0.1128 0.059 Uiso 1 1 calc R . . H47 H -0.5149 -0.0682 -0.0415 0.059 Uiso 1 1 calc R . . C57 C -0.4266(5) 0.0150(2) -0.0982(3) 0.0449(12) Uani 1 1 d . . . H48 H -0.4343 0.0484 -0.1264 0.067 Uiso 1 1 calc R . . H49 H -0.3498 -0.0020 -0.0953 0.067 Uiso 1 1 calc R . . H50 H -0.4312 0.0236 -0.0497 0.067 Uiso 1 1 calc R . . C58 C -0.6418(5) 0.0030(3) -0.1295(3) 0.0517(14) Uani 1 1 d . . . H51 H -0.6386 0.0084 -0.0789 0.078 Uiso 1 1 calc R . . H52 H -0.7097 -0.0202 -0.1524 0.078 Uiso 1 1 calc R . . H53 H -0.6507 0.0381 -0.1540 0.078 Uiso 1 1 calc R . . Sb1 Sb -0.41587(3) -0.263461(14) -0.112910(19) 0.04175(12) Uani 1 1 d . . . F1 F -0.2929(3) -0.21579(14) -0.1235(2) 0.0563(9) Uani 1 1 d . C . F2 F -0.5365(5) -0.3090(2) -0.1054(3) 0.0965(18) Uani 1 1 d . C . F3 F -0.3164(5) -0.2852(2) -0.0248(3) 0.0905(15) Uani 1 1 d . C . F4 F -0.4724(4) -0.20842(17) -0.0670(3) 0.0767(12) Uani 1 1 d . C . F5 F -0.5060(4) -0.2385(3) -0.2013(2) 0.1006(19) Uani 1 1 d . C . F6A F -0.3331(10) -0.3196(3) -0.1457(6) 0.057(3) Uiso 0.53(3) 1 d P C 1 F6B F -0.3747(13) -0.3124(4) -0.1742(8) 0.065(4) Uiso 0.47(3) 1 d P C 2 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 0.0225(2) 0.0289(3) 0.0270(2) 0.00677(19) -0.00012(17) -0.00074(17) P1 0.0207(4) 0.0281(5) 0.0257(4) 0.0066(4) 0.0013(3) -0.0013(3) P2 0.0208(4) 0.0276(5) 0.0257(4) 0.0055(4) 0.0016(3) 0.0001(3) N1 0.0209(13) 0.0232(16) 0.0251(14) 0.0023(12) 0.0022(11) -0.0001(11) C1 0.0213(15) 0.0253(19) 0.0250(16) 0.0015(14) 0.0042(13) 0.0019(13) C2 0.0251(17) 0.028(2) 0.0298(18) 0.0016(15) 0.0023(14) 0.0004(14) C3 0.0293(19) 0.024(2) 0.039(2) 0.0017(16) 0.0044(16) -0.0071(15) C4 0.0307(19) 0.026(2) 0.035(2) 0.0057(16) 0.0050(16) -0.0005(15) C5 0.0246(16) 0.027(2) 0.0219(15) 0.0018(14) 0.0053(13) 0.0029(14) C6 0.0231(16) 0.0228(19) 0.0237(16) 0.0026(14) 0.0013(13) 0.0001(13) C7 0.0201(15) 0.026(2) 0.0280(17) 0.0012(15) -0.0006(13) -0.0008(13) C8 0.0234(17) 0.040(3) 0.0277(18) -0.0004(17) 0.0004(14) -0.0013(16) C9 0.031(2) 0.043(3) 0.032(2) 0.0123(19) -0.0042(16) -0.0010(18) C10 0.0253(19) 0.038(3) 0.047(3) 0.005(2) -0.0045(17) 0.0012(17) C11 0.0217(18) 0.045(3) 0.046(2) -0.002(2) 0.0026(17) 0.0021(17) C12 0.0250(18) 0.032(2) 0.037(2) 0.0012(17) 0.0052(15) -0.0006(15) C13 0.0250(16) 0.025(2) 0.0226(16) 0.0027(14) 0.0027(13) 0.0024(14) C14 0.034(2) 0.028(2) 0.0291(18) 0.0057(16) 0.0051(15) -0.0007(16) C15 0.038(2) 0.051(3) 0.040(2) 0.016(2) 0.0131(19) 0.006(2) C16 0.057(3) 0.078(5) 0.045(3) 0.027(3) 0.016(3) -0.005(3) C17 0.066(4) 0.060(4) 0.053(3) 0.031(3) 0.005(3) -0.008(3) C18 0.048(3) 0.041(3) 0.054(3) 0.024(2) 0.000(2) 0.003(2) C19 0.038(2) 0.031(2) 0.036(2) 0.0123(18) 0.0039(17) 0.0021(17) C20 0.0221(15) 0.0243(19) 0.0270(17) 0.0032(14) 0.0022(13) -0.0034(13) C21 0.0259(17) 0.024(2) 0.0294(18) 0.0038(15) 0.0065(14) -0.0021(14) C22 0.034(2) 0.031(2) 0.0274(18) 0.0065(16) 0.0071(15) 0.0039(16) C23 0.038(2) 0.031(2) 0.031(2) 0.0092(17) 0.0083(16) 0.0086(17) C24 0.039(2) 0.027(2) 0.0302(19) 0.0032(16) 0.0092(16) 0.0063(17) C25 0.0254(17) 0.027(2) 0.0291(18) 0.0025(15) 0.0043(14) -0.0033(14) C26 0.0265(17) 0.025(2) 0.036(2) 0.0043(16) 0.0107(15) 0.0022(14) C27 0.039(2) 0.025(2) 0.046(2) 0.0000(18) 0.0138(19) 0.0015(17) C28 0.0233(18) 0.048(3) 0.040(2) 0.003(2) 0.0064(16) 0.0020(17) C29 0.047(3) 0.035(3) 0.039(2) 0.0055(19) 0.021(2) 0.005(2) C30 0.049(3) 0.051(3) 0.033(2) 0.014(2) 0.010(2) 0.020(2) C31 0.088(5) 0.050(4) 0.047(3) 0.021(3) 0.005(3) -0.003(3) C32 0.039(3) 0.074(4) 0.042(3) 0.018(3) -0.001(2) -0.002(3) C34 0.036(2) 0.031(2) 0.0292(19) -0.0034(16) 0.0065(16) -0.0042(17) C35 0.057(3) 0.039(3) 0.043(3) -0.008(2) 0.008(2) -0.007(2) C36 0.042(2) 0.044(3) 0.040(2) -0.004(2) 0.015(2) 0.005(2) C37 0.052(3) 0.046(3) 0.0251(19) -0.0044(19) 0.0047(19) 0.004(2) C38 0.0220(15) 0.0237(19) 0.0270(17) 0.0021(14) 0.0032(13) 0.0005(13) C39 0.0284(18) 0.031(2) 0.0211(16) -0.0006(14) 0.0029(13) -0.0013(15) C40 0.034(2) 0.038(2) 0.0248(17) 0.0012(17) 0.0028(15) 0.0044(17) C41 0.0279(18) 0.030(2) 0.0332(19) 0.0048(17) -0.0016(15) 0.0003(15) C42 0.0223(17) 0.030(2) 0.037(2) 0.0002(17) 0.0006(15) 0.0057(15) C43 0.0231(16) 0.026(2) 0.0294(18) -0.0027(15) 0.0000(14) -0.0007(14) C44 0.037(2) 0.033(2) 0.033(2) -0.0044(17) 0.0085(17) 0.0036(17) C45 0.063(4) 0.049(3) 0.046(3) -0.008(2) 0.006(3) 0.027(3) C46 0.066(4) 0.061(4) 0.054(3) -0.001(3) 0.032(3) 0.010(3) C47 0.054(3) 0.046(3) 0.070(4) -0.027(3) 0.016(3) -0.003(3) C55 0.032(2) 0.035(2) 0.0311(19) -0.0062(17) 0.0046(16) -0.0007(17) C56 0.040(2) 0.052(3) 0.0278(19) -0.0006(19) 0.0111(17) -0.003(2) C57 0.049(3) 0.048(3) 0.036(2) -0.018(2) 0.010(2) -0.012(2) C58 0.041(3) 0.070(4) 0.044(3) -0.011(3) 0.011(2) 0.016(3) Sb1 0.03876(18) 0.0372(2) 0.0474(2) -0.01035(14) 0.00886(14) -0.01095(13) F1 0.0437(17) 0.0466(19) 0.067(2) 0.0097(16) -0.0038(15) -0.0178(14) F2 0.088(3) 0.098(4) 0.125(4) -0.032(3) 0.064(3) -0.053(3) F3 0.083(3) 0.098(4) 0.087(3) 0.050(3) 0.018(3) 0.020(3) F4 0.094(3) 0.059(2) 0.079(3) -0.016(2) 0.027(2) 0.020(2) F5 0.048(2) 0.186(6) 0.055(2) 0.010(3) -0.0089(19) -0.026(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 N1 2.107(3) . ? Cu1 F1 2.189(3) . ? Cu1 P2 2.2526(11) . ? Cu1 P1 2.2612(11) . ? P1 C6 1.708(4) . ? P1 C20 1.818(4) . ? P2 C13 1.699(4) . ? P2 C38 1.825(4) . ? N1 C5 1.355(5) . ? N1 C1 1.360(4) . ? C1 C2 1.397(6) . ? C1 C6 1.486(5) . ? C2 C3 1.391(6) . ? C2 H1 0.9500 . ? C3 C4 1.384(6) . ? C3 H2 0.9500 . ? C4 C5 1.399(6) . ? C4 H3 0.9500 . ? C5 C13 1.478(5) . ? C6 C7 1.470(5) . ? C7 C8 1.399(6) . ? C7 C12 1.402(6) . ? C8 C9 1.395(6) . ? C8 H4 0.9500 . ? C9 C10 1.392(7) . ? C9 H5 0.9500 . ? C10 C11 1.402(7) . ? C10 H6 0.9500 . ? C11 C12 1.388(6) . ? C11 H7 0.9500 . ? C12 H8 0.9500 . ? C13 C14 1.482(6) . ? C14 C19 1.399(6) . ? C14 C15 1.400(6) . ? C15 C16 1.401(7) . ? C15 H9 0.9500 . ? C16 C17 1.370(10) . ? C16 H10 0.9500 . ? C17 C18 1.361(9) . ? C17 H11 0.9500 . ? C18 C19 1.408(7) . ? C18 H12 0.9500 . ? C19 H13 0.9500 . ? C20 C25 1.418(6) . ? C20 C21 1.442(6) . ? C21 C22 1.389(6) . ? C21 C26 1.552(6) . ? C22 C23 1.399(6) . ? C22 H14 0.9500 . ? C23 C24 1.381(6) . ? C23 C30 1.529(6) . ? C24 C25 1.405(6) . ? C24 H15 0.9500 . ? C25 C34 1.555(6) . ? C26 C27 1.529(6) . ? C26 C29 1.536(6) . ? C26 C28 1.546(6) . ? C27 H18 0.9800 . ? C27 H19 0.9800 . ? C27 H20 0.9800 . ? C28 H21 0.9800 . ? C28 H22 0.9800 . ? C28 H23 0.9800 . ? C29 H24 0.9800 . ? C29 H25 0.9800 . ? C29 H26 0.9800 . ? C30 C31 1.522(9) . ? C30 C33B 1.539(12) . ? C30 C32 1.558(9) . ? C30 C33A 1.580(15) . ? C31 H54 0.9800 . ? C31 H55 0.9800 . ? C31 H56 0.9800 . ? C32 H57 0.9800 . ? C32 H58 0.9800 . ? C32 H59 0.9800 . ? C33A H60 0.9800 . ? C33A H61 0.9800 . ? C33A H62 0.9800 . ? C33B H63 0.9800 . ? C33B H64 0.9800 . ? C33B H65 0.9800 . ? C34 C35 1.542(7) . ? C34 C36 1.545(7) . ? C34 C37 1.550(7) . ? C35 H27 0.9800 . ? C35 H28 0.9800 . ? C35 H29 0.9800 . ? C36 H30 0.9800 . ? C36 H31 0.9800 . ? C36 H32 0.9800 . ? C37 H33 0.9800 . ? C37 H34 0.9800 . ? C37 H35 0.9800 . ? C38 C39 1.425(5) . ? C38 C43 1.433(6) . ? C39 C40 1.400(6) . ? C39 C44 1.554(6) . ? C40 C41 1.388(6) . ? C40 H16 0.9500 . ? C41 C42 1.384(6) . ? C41 C48 1.537(7) . ? C42 C43 1.399(5) . ? C42 H17 0.9500 . ? C43 C55 1.551(6) . ? C44 C45 1.522(7) . ? C44 C46 1.523(8) . ? C44 C47 1.547(7) . ? C45 H36 0.9800 . ? C45 H37 0.9800 . ? C45 H38 0.9800 . ? C46 H39 0.9800 . ? C46 H40 0.9800 . ? C46 H41 0.9800 . ? C47 H42 0.9800 . ? C47 H43 0.9800 . ? C47 H44 0.9800 . ? C48 C54 1.43(2) . ? C48 C51 1.495(13) . ? C48 C50 1.533(14) . ? C48 C53 1.57(2) . ? C48 C52 1.583(17) . ? C48 C49 1.590(13) . ? C49 H66 0.9800 . ? C49 H67 0.9800 . ? C49 H68 0.9800 . ? C50 H69 0.9800 . ? C50 H70 0.9800 . ? C50 H71 0.9800 . ? C51 H72 0.9800 . ? C51 H73 0.9800 . ? C51 H74 0.9800 . ? C52 H75 0.9800 . ? C52 H76 0.9800 . ? C52 H77 0.9800 . ? C53 H78 0.9800 . ? C53 H79 0.9800 . ? C53 H80 0.9800 . ? C54 H81 0.9800 . ? C54 H82 0.9800 . ? C54 H83 0.9800 . ? C55 C58 1.525(7) . ? C55 C57 1.533(6) . ? C55 C56 1.534(7) . ? C56 H45 0.9800 . ? C56 H46 0.9800 . ? C56 H47 0.9800 . ? C57 H48 0.9800 . ? C57 H49 0.9800 . ? C57 H50 0.9800 . ? C58 H51 0.9800 . ? C58 H52 0.9800 . ? C58 H53 0.9800 . ? Sb1 F2 1.843(4) . ? Sb1 F4 1.846(4) . ? Sb1 F5 1.850(5) . ? Sb1 F6B 1.851(10) . ? Sb1 F3 1.859(5) . ? Sb1 F6A 1.901(8) . ? Sb1 F1 1.916(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 F1 146.05(15) . . ? N1 Cu1 P2 82.32(9) . . ? F1 Cu1 P2 101.99(10) . . ? N1 Cu1 P1 82.98(9) . . ? F1 Cu1 P1 100.63(10) . . ? P2 Cu1 P1 156.25(5) . . ? C6 P1 C20 107.65(18) . . ? C6 P1 Cu1 102.85(13) . . ? C20 P1 Cu1 142.20(13) . . ? C13 P2 C38 109.12(18) . . ? C13 P2 Cu1 104.14(13) . . ? C38 P2 Cu1 144.63(14) . . ? C5 N1 C1 119.4(3) . . ? C5 N1 Cu1 118.0(2) . . ? C1 N1 Cu1 117.5(3) . . ? N1 C1 C2 121.7(4) . . ? N1 C1 C6 118.3(3) . . ? C2 C1 C6 119.9(3) . . ? C3 C2 C1 118.5(4) . . ? C3 C2 H1 120.8 . . ? C1 C2 H1 120.8 . . ? C4 C3 C2 119.7(4) . . ? C4 C3 H2 120.2 . . ? C2 C3 H2 120.2 . . ? C3 C4 C5 119.5(4) . . ? C3 C4 H3 120.2 . . ? C5 C4 H3 120.2 . . ? N1 C5 C4 120.9(3) . . ? N1 C5 C13 118.5(3) . . ? C4 C5 C13 120.4(4) . . ? C7 C6 C1 118.7(3) . . ? C7 C6 P1 128.0(3) . . ? C1 C6 P1 113.2(3) . . ? C8 C7 C12 118.5(4) . . ? C8 C7 C6 122.3(4) . . ? C12 C7 C6 119.2(4) . . ? C9 C8 C7 120.6(4) . . ? C9 C8 H4 119.7 . . ? C7 C8 H4 119.7 . . ? C10 C9 C8 120.4(4) . . ? C10 C9 H5 119.8 . . ? C8 C9 H5 119.8 . . ? C9 C10 C11 119.5(4) . . ? C9 C10 H6 120.2 . . ? C11 C10 H6 120.2 . . ? C12 C11 C10 119.9(5) . . ? C12 C11 H7 120.1 . . ? C10 C11 H7 120.1 . . ? C11 C12 C7 121.1(4) . . ? C11 C12 H8 119.5 . . ? C7 C12 H8 119.5 . . ? C5 C13 C14 118.7(4) . . ? C5 C13 P2 113.3(3) . . ? C14 C13 P2 127.9(3) . . ? C19 C14 C15 118.6(4) . . ? C19 C14 C13 122.4(4) . . ? C15 C14 C13 119.0(4) . . ? C14 C15 C16 119.8(5) . . ? C14 C15 H9 120.1 . . ? C16 C15 H9 120.1 . . ? C17 C16 C15 120.9(6) . . ? C17 C16 H10 119.6 . . ? C15 C16 H10 119.6 . . ? C18 C17 C16 120.2(5) . . ? C18 C17 H11 119.9 . . ? C16 C17 H11 119.9 . . ? C17 C18 C19 120.5(5) . . ? C17 C18 H12 119.7 . . ? C19 C18 H12 119.7 . . ? C14 C19 C18 120.0(5) . . ? C14 C19 H13 120.0 . . ? C18 C19 H13 120.0 . . ? C25 C20 C21 119.9(4) . . ? C25 C20 P1 121.7(3) . . ? C21 C20 P1 117.7(3) . . ? C22 C21 C20 117.7(4) . . ? C22 C21 C26 118.1(4) . . ? C20 C21 C26 124.2(4) . . ? C21 C22 C23 123.0(4) . . ? C21 C22 H14 118.5 . . ? C23 C22 H14 118.5 . . ? C24 C23 C22 117.2(4) . . ? C24 C23 C30 122.3(4) . . ? C22 C23 C30 120.5(4) . . ? C23 C24 C25 123.7(4) . . ? C23 C24 H15 118.2 . . ? C25 C24 H15 118.2 . . ? C24 C25 C20 117.2(4) . . ? C24 C25 C34 113.6(4) . . ? C20 C25 C34 129.1(4) . . ? C27 C26 C29 105.6(4) . . ? C27 C26 C28 110.8(4) . . ? C29 C26 C28 106.4(4) . . ? C27 C26 C21 110.9(3) . . ? C29 C26 C21 112.1(4) . . ? C28 C26 C21 110.8(4) . . ? C26 C27 H18 109.5 . . ? C26 C27 H19 109.5 . . ? H18 C27 H19 109.5 . . ? C26 C27 H20 109.5 . . ? H18 C27 H20 109.5 . . ? H19 C27 H20 109.5 . . ? C26 C28 H21 109.5 . . ? C26 C28 H22 109.5 . . ? H21 C28 H22 109.5 . . ? C26 C28 H23 109.5 . . ? H21 C28 H23 109.5 . . ? H22 C28 H23 109.5 . . ? C26 C29 H24 109.5 . . ? C26 C29 H25 109.5 . . ? H24 C29 H25 109.5 . . ? C26 C29 H26 109.5 . . ? H24 C29 H26 109.5 . . ? H25 C29 H26 109.5 . . ? C31 C30 C23 109.5(5) . . ? C31 C30 C33B 103.2(8) . . ? C23 C30 C33B 112.7(5) . . ? C31 C30 C32 108.1(5) . . ? C23 C30 C32 108.4(4) . . ? C33B C30 C32 114.6(7) . . ? C31 C30 C33A 123.1(9) . . ? C23 C30 C33A 111.3(6) . . ? C33B C30 C33A 23.5(6) . . ? C32 C30 C33A 94.6(8) . . ? C30 C31 H54 109.5 . . ? C30 C31 H55 109.5 . . ? H54 C31 H55 109.5 . . ? C30 C31 H56 109.5 . . ? H54 C31 H56 109.5 . . ? H55 C31 H56 109.5 . . ? C30 C32 H57 109.5 . . ? C30 C32 H58 109.5 . . ? H57 C32 H58 109.5 . . ? C30 C32 H59 109.5 . . ? H57 C32 H59 109.5 . . ? H58 C32 H59 109.5 . . ? C30 C33A H60 109.5 . . ? C30 C33A H61 109.5 . . ? C30 C33A H62 109.5 . . ? C30 C33B H63 109.5 . . ? C30 C33B H64 109.5 . . ? C30 C33B H65 109.5 . . ? C35 C34 C36 110.0(4) . . ? C35 C34 C37 106.1(4) . . ? C36 C34 C37 106.4(4) . . ? C35 C34 C25 106.4(4) . . ? C36 C34 C25 111.0(4) . . ? C37 C34 C25 116.7(4) . . ? C34 C35 H27 109.5 . . ? C34 C35 H28 109.5 . . ? H27 C35 H28 109.5 . . ? C34 C35 H29 109.5 . . ? H27 C35 H29 109.5 . . ? H28 C35 H29 109.5 . . ? C34 C36 H30 109.5 . . ? C34 C36 H31 109.5 . . ? H30 C36 H31 109.5 . . ? C34 C36 H32 109.5 . . ? H30 C36 H32 109.5 . . ? H31 C36 H32 109.5 . . ? C34 C37 H33 109.5 . . ? C34 C37 H34 109.5 . . ? H33 C37 H34 109.5 . . ? C34 C37 H35 109.5 . . ? H33 C37 H35 109.5 . . ? H34 C37 H35 109.5 . . ? C39 C38 C43 120.5(3) . . ? C39 C38 P2 122.7(3) . . ? C43 C38 P2 116.2(3) . . ? C40 C39 C38 117.4(4) . . ? C40 C39 C44 114.5(4) . . ? C38 C39 C44 128.1(4) . . ? C41 C40 C39 123.2(4) . . ? C41 C40 H16 118.4 . . ? C39 C40 H16 118.4 . . ? C42 C41 C40 117.6(4) . . ? C42 C41 C48 121.2(4) . . ? C40 C41 C48 121.2(4) . . ? C41 C42 C43 123.5(4) . . ? C41 C42 H17 118.2 . . ? C43 C42 H17 118.2 . . ? C42 C43 C38 117.0(4) . . ? C42 C43 C55 118.5(4) . . ? C38 C43 C55 124.5(4) . . ? C45 C44 C46 107.5(5) . . ? C45 C44 C47 106.8(5) . . ? C46 C44 C47 109.5(5) . . ? C45 C44 C39 116.1(4) . . ? C46 C44 C39 110.4(4) . . ? C47 C44 C39 106.4(4) . . ? C44 C45 H36 109.5 . . ? C44 C45 H37 109.5 . . ? H36 C45 H37 109.5 . . ? C44 C45 H38 109.5 . . ? H36 C45 H38 109.5 . . ? H37 C45 H38 109.5 . . ? C44 C46 H39 109.5 . . ? C44 C46 H40 109.5 . . ? H39 C46 H40 109.5 . . ? C44 C46 H41 109.5 . . ? H39 C46 H41 109.5 . . ? H40 C46 H41 109.5 . . ? C44 C47 H42 109.5 . . ? C44 C47 H43 109.5 . . ? H42 C47 H43 109.5 . . ? C44 C47 H44 109.5 . . ? H42 C47 H44 109.5 . . ? H43 C47 H44 109.5 . . ? C54 C48 C51 133.4(11) . . ? C54 C48 C50 68.0(10) . . ? C51 C48 C50 112.4(8) . . ? C54 C48 C41 113.1(10) . . ? C51 C48 C41 110.6(6) . . ? C50 C48 C41 107.9(6) . . ? C54 C48 C53 114.7(12) . . ? C51 C48 C53 36.5(8) . . ? C50 C48 C53 142.4(10) . . ? C41 C48 C53 104.8(8) . . ? C54 C48 C52 110.0(11) . . ? C51 C48 C52 65.4(8) . . ? C50 C48 C52 49.1(8) . . ? C41 C48 C52 112.5(7) . . ? C53 C48 C52 101.0(11) . . ? C54 C48 C49 39.3(9) . . ? C51 C48 C49 108.2(7) . . ? C50 C48 C49 105.6(7) . . ? C41 C48 C49 112.1(6) . . ? C53 C48 C49 78.2(9) . . ? C52 C48 C49 133.9(8) . . ? C48 C49 H66 109.5 . . ? C48 C49 H67 109.5 . . ? C48 C49 H68 109.5 . . ? C48 C50 H69 109.5 . . ? C48 C50 H70 109.5 . . ? C48 C50 H71 109.5 . . ? C48 C51 H72 109.5 . . ? C48 C51 H73 109.5 . . ? C48 C51 H74 109.5 . . ? C48 C52 H75 109.5 . . ? C48 C52 H76 109.5 . . ? H75 C52 H76 109.5 . . ? C48 C52 H77 109.5 . . ? H75 C52 H77 109.5 . . ? H76 C52 H77 109.5 . . ? C48 C53 H78 109.5 . . ? C48 C53 H79 109.5 . . ? H78 C53 H79 109.5 . . ? C48 C53 H80 109.5 . . ? H78 C53 H80 109.5 . . ? H79 C53 H80 109.5 . . ? C48 C54 H81 109.5 . . ? C48 C54 H82 109.5 . . ? H81 C54 H82 109.5 . . ? C48 C54 H83 109.5 . . ? H81 C54 H83 109.5 . . ? H82 C54 H83 109.5 . . ? C58 C55 C57 106.0(4) . . ? C58 C55 C56 106.6(4) . . ? C57 C55 C56 109.7(4) . . ? C58 C55 C43 111.1(4) . . ? C57 C55 C43 111.6(4) . . ? C56 C55 C43 111.6(4) . . ? C55 C56 H45 109.5 . . ? C55 C56 H46 109.5 . . ? H45 C56 H46 109.5 . . ? C55 C56 H47 109.5 . . ? H45 C56 H47 109.5 . . ? H46 C56 H47 109.5 . . ? C55 C57 H48 109.5 . . ? C55 C57 H49 109.5 . . ? H48 C57 H49 109.5 . . ? C55 C57 H50 109.5 . . ? H48 C57 H50 109.5 . . ? H49 C57 H50 109.5 . . ? C55 C58 H51 109.5 . . ? C55 C58 H52 109.5 . . ? H51 C58 H52 109.5 . . ? C55 C58 H53 109.5 . . ? H51 C58 H53 109.5 . . ? H52 C58 H53 109.5 . . ? F2 Sb1 F4 91.4(2) . . ? F2 Sb1 F5 91.4(3) . . ? F4 Sb1 F5 90.8(3) . . ? F2 Sb1 F6B 89.8(3) . . ? F4 Sb1 F6B 169.5(5) . . ? F5 Sb1 F6B 78.8(6) . . ? F2 Sb1 F3 92.8(3) . . ? F4 Sb1 F3 89.2(2) . . ? F5 Sb1 F3 175.8(2) . . ? F6B Sb1 F3 101.1(6) . . ? F2 Sb1 F6A 93.2(3) . . ? F4 Sb1 F6A 169.7(4) . . ? F5 Sb1 F6A 98.3(4) . . ? F6B Sb1 F6A 19.9(3) . . ? F3 Sb1 F6A 81.4(4) . . ? F2 Sb1 F1 178.4(2) . . ? F4 Sb1 F1 89.0(2) . . ? F5 Sb1 F1 87.01(19) . . ? F6B Sb1 F1 89.6(3) . . ? F3 Sb1 F1 88.8(2) . . ? F6A Sb1 F1 86.7(3) . . ? Sb1 F1 Cu1 143.9(2) . . ? 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 P1 C6 -10.19(17) . . . . ? F1 Cu1 P1 C6 135.63(18) . . . . ? P2 Cu1 P1 C6 -62.29(19) . . . . ? N1 Cu1 P1 C20 -153.5(3) . . . . ? F1 Cu1 P1 C20 -7.6(3) . . . . ? P2 Cu1 P1 C20 154.4(2) . . . . ? N1 Cu1 P2 C13 6.46(17) . . . . ? F1 Cu1 P2 C13 -139.33(18) . . . . ? P1 Cu1 P2 C13 58.67(19) . . . . ? N1 Cu1 P2 C38 166.2(3) . . . . ? F1 Cu1 P2 C38 20.5(3) . . . . ? P1 Cu1 P2 C38 -141.5(2) . . . . ? F1 Cu1 N1 C5 104.7(3) . . . . ? P2 Cu1 N1 C5 4.6(3) . . . . ? P1 Cu1 N1 C5 -156.7(3) . . . . ? F1 Cu1 N1 C1 -100.5(3) . . . . ? P2 Cu1 N1 C1 159.4(3) . . . . ? P1 Cu1 N1 C1 -1.9(3) . . . . ? C5 N1 C1 C2 -5.9(6) . . . . ? Cu1 N1 C1 C2 -160.4(3) . . . . ? C5 N1 C1 C6 171.1(3) . . . . ? Cu1 N1 C1 C6 16.7(5) . . . . ? N1 C1 C2 C3 3.3(6) . . . . ? C6 C1 C2 C3 -173.7(4) . . . . ? C1 C2 C3 C4 0.5(7) . . . . ? C2 C3 C4 C5 -1.7(7) . . . . ? C1 N1 C5 C4 4.7(6) . . . . ? Cu1 N1 C5 C4 159.0(3) . . . . ? C1 N1 C5 C13 -171.2(3) . . . . ? Cu1 N1 C5 C13 -16.9(5) . . . . ? C3 C4 C5 N1 -0.9(6) . . . . ? C3 C4 C5 C13 174.9(4) . . . . ? N1 C1 C6 C7 155.9(4) . . . . ? C2 C1 C6 C7 -27.0(6) . . . . ? N1 C1 C6 P1 -26.1(5) . . . . ? C2 C1 C6 P1 151.0(3) . . . . ? C20 P1 C6 C7 -3.7(4) . . . . ? Cu1 P1 C6 C7 -161.0(3) . . . . ? C20 P1 C6 C1 178.6(3) . . . . ? Cu1 P1 C6 C1 21.2(3) . . . . ? C1 C6 C7 C8 131.5(4) . . . . ? P1 C6 C7 C8 -46.2(6) . . . . ? C1 C6 C7 C12 -49.2(5) . . . . ? P1 C6 C7 C12 133.2(4) . . . . ? C12 C7 C8 C9 -1.3(7) . . . . ? C6 C7 C8 C9 178.1(4) . . . . ? C7 C8 C9 C10 -0.3(7) . . . . ? C8 C9 C10 C11 0.7(8) . . . . ? C9 C10 C11 C12 0.5(8) . . . . ? C10 C11 C12 C7 -2.2(7) . . . . ? C8 C7 C12 C11 2.5(7) . . . . ? C6 C7 C12 C11 -176.8(4) . . . . ? N1 C5 C13 C14 -161.3(4) . . . . ? C4 C5 C13 C14 22.8(6) . . . . ? N1 C5 C13 P2 22.6(5) . . . . ? C4 C5 C13 P2 -153.4(3) . . . . ? C38 P2 C13 C5 175.8(3) . . . . ? Cu1 P2 C13 C5 -16.4(3) . . . . ? C38 P2 C13 C14 0.1(4) . . . . ? Cu1 P2 C13 C14 167.9(4) . . . . ? C5 C13 C14 C19 -130.0(5) . . . . ? P2 C13 C14 C19 45.5(6) . . . . ? C5 C13 C14 C15 51.4(6) . . . . ? P2 C13 C14 C15 -133.0(4) . . . . ? C19 C14 C15 C16 0.7(8) . . . . ? C13 C14 C15 C16 179.3(5) . . . . ? C14 C15 C16 C17 0.2(10) . . . . ? C15 C16 C17 C18 -0.3(11) . . . . ? C16 C17 C18 C19 -0.4(10) . . . . ? C15 C14 C19 C18 -1.4(7) . . . . ? C13 C14 C19 C18 -180.0(5) . . . . ? C17 C18 C19 C14 1.3(9) . . . . ? C6 P1 C20 C25 -62.0(4) . . . . ? Cu1 P1 C20 C25 80.3(4) . . . . ? C6 P1 C20 C21 108.4(3) . . . . ? Cu1 P1 C20 C21 -109.4(3) . . . . ? C25 C20 C21 C22 11.6(6) . . . . ? P1 C20 C21 C22 -159.0(3) . . . . ? C25 C20 C21 C26 -170.1(4) . . . . ? P1 C20 C21 C26 19.4(5) . . . . ? C20 C21 C22 C23 -2.2(7) . . . . ? C26 C21 C22 C23 179.3(4) . . . . ? C21 C22 C23 C24 -6.7(7) . . . . ? C21 C22 C23 C30 174.1(5) . . . . ? C22 C23 C24 C25 6.6(7) . . . . ? C30 C23 C24 C25 -174.2(5) . . . . ? C23 C24 C25 C20 2.4(7) . . . . ? C23 C24 C25 C34 -173.6(4) . . . . ? C21 C20 C25 C24 -11.6(6) . . . . ? P1 C20 C25 C24 158.5(3) . . . . ? C21 C20 C25 C34 163.7(4) . . . . ? P1 C20 C25 C34 -26.2(6) . . . . ? C22 C21 C26 C27 105.2(5) . . . . ? C20 C21 C26 C27 -73.2(5) . . . . ? C22 C21 C26 C29 -12.5(6) . . . . ? C20 C21 C26 C29 169.1(4) . . . . ? C22 C21 C26 C28 -131.3(4) . . . . ? C20 C21 C26 C28 50.3(5) . . . . ? C24 C23 C30 C31 -117.7(6) . . . . ? C22 C23 C30 C31 61.5(7) . . . . ? C24 C23 C30 C33B -3.4(10) . . . . ? C22 C23 C30 C33B 175.7(8) . . . . ? C24 C23 C30 C32 124.6(5) . . . . ? C22 C23 C30 C32 -56.3(6) . . . . ? C24 C23 C30 C33A 21.8(11) . . . . ? C22 C23 C30 C33A -159.0(9) . . . . ? C24 C25 C34 C35 66.7(5) . . . . ? C20 C25 C34 C35 -108.7(5) . . . . ? C24 C25 C34 C36 -53.0(5) . . . . ? C20 C25 C34 C36 131.6(5) . . . . ? C24 C25 C34 C37 -175.1(4) . . . . ? C20 C25 C34 C37 9.5(6) . . . . ? C13 P2 C38 C39 69.4(4) . . . . ? Cu1 P2 C38 C39 -89.8(4) . . . . ? C13 P2 C38 C43 -101.5(3) . . . . ? Cu1 P2 C38 C43 99.2(4) . . . . ? C43 C38 C39 C40 9.2(6) . . . . ? P2 C38 C39 C40 -161.4(3) . . . . ? C43 C38 C39 C44 -168.1(4) . . . . ? P2 C38 C39 C44 21.4(6) . . . . ? C38 C39 C40 C41 -2.5(7) . . . . ? C44 C39 C40 C41 175.2(4) . . . . ? C39 C40 C41 C42 -4.0(7) . . . . ? C39 C40 C41 C48 175.8(4) . . . . ? C40 C41 C42 C43 3.9(7) . . . . ? C48 C41 C42 C43 -175.9(4) . . . . ? C41 C42 C43 C38 2.6(7) . . . . ? C41 C42 C43 C55 -176.6(4) . . . . ? C39 C38 C43 C42 -9.3(6) . . . . ? P2 C38 C43 C42 161.9(3) . . . . ? C39 C38 C43 C55 169.9(4) . . . . ? P2 C38 C43 C55 -18.9(5) . . . . ? C40 C39 C44 C45 -178.5(5) . . . . ? C38 C39 C44 C45 -1.2(7) . . . . ? C40 C39 C44 C46 58.9(6) . . . . ? C38 C39 C44 C46 -123.8(5) . . . . ? C40 C39 C44 C47 -59.9(6) . . . . ? C38 C39 C44 C47 117.5(5) . . . . ? C42 C41 C48 C54 -45.3(12) . . . . ? C40 C41 C48 C54 134.9(11) . . . . ? C42 C41 C48 C51 118.3(7) . . . . ? C40 C41 C48 C51 -61.5(8) . . . . ? C42 C41 C48 C50 -118.4(7) . . . . ? C40 C41 C48 C50 61.8(7) . . . . ? C42 C41 C48 C53 80.4(10) . . . . ? C40 C41 C48 C53 -99.4(9) . . . . ? C42 C41 C48 C52 -170.7(8) . . . . ? C40 C41 C48 C52 9.5(9) . . . . ? C42 C41 C48 C49 -2.6(8) . . . . ? C40 C41 C48 C49 177.6(6) . . . . ? C42 C43 C55 C58 10.2(6) . . . . ? C38 C43 C55 C58 -168.9(4) . . . . ? C42 C43 C55 C57 -107.8(5) . . . . ? C38 C43 C55 C57 73.0(6) . . . . ? C42 C43 C55 C56 129.0(4) . . . . ? C38 C43 C55 C56 -50.1(6) . . . . ? F2 Sb1 F1 Cu1 117(7) . . . . ? F4 Sb1 F1 Cu1 15.3(3) . . . . ? F5 Sb1 F1 Cu1 106.2(4) . . . . ? F6B Sb1 F1 Cu1 -175.0(6) . . . . ? F3 Sb1 F1 Cu1 -73.9(3) . . . . ? F6A Sb1 F1 Cu1 -155.3(5) . . . . ? N1 Cu1 F1 Sb1 172.7(2) . . . . ? P2 Cu1 F1 Sb1 -93.3(3) . . . . ? P1 Cu1 F1 Sb1 79.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.891 _diffrn_reflns_theta_full 31.62 _diffrn_measured_fraction_theta_full 0.891 _refine_diff_density_max 0.629 _refine_diff_density_min -1.468 _refine_diff_density_rms 0.110 # Attachment '3a.cif' data_3a _database_code_depnum_ccdc_archive 'CCDC 812263' #TrackingRef '3a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C67.50 H86 Cu F6 N2 P2 Sb' _chemical_formula_weight 1286.61 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' 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.075(3) _cell_length_b 17.639(4) _cell_length_c 17.853(4) _cell_angle_alpha 111.242(3) _cell_angle_beta 101.392(2) _cell_angle_gamma 105.3822(15) _cell_volume 3229.7(13) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 12 _cell_measurement_theta_max 18 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.323 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1338 _exptl_absorpt_coefficient_mu 0.854 _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 173(2) _diffrn_radiation_wavelength 0.71070 _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 31379 _diffrn_reflns_av_R_equivalents 0.0391 _diffrn_reflns_av_sigmaI/netI 0.0742 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 31.59 _reflns_number_total 17862 _reflns_number_gt 13717 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rigaku AFC10/Saturn 70 CCD' _computing_cell_refinement 'Rigaku AFC10/Saturn 70 CCD' _computing_data_reduction 'Rigaku AFC10/Saturn 70 CCD' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for windows' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0673P)^2^+5.9928P] 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 17862 _refine_ls_number_parameters 691 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1069 _refine_ls_R_factor_gt 0.0833 _refine_ls_wR_factor_ref 0.2033 _refine_ls_wR_factor_gt 0.1860 _refine_ls_goodness_of_fit_ref 1.124 _refine_ls_restrained_S_all 1.124 _refine_ls_shift/su_max 6.845 _refine_ls_shift/su_mean 0.044 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 0.26734(4) 0.47898(3) 0.18146(3) 0.02956(13) Uani 1 1 d . . . N1 N 0.1707(3) 0.4947(2) 0.2559(2) 0.0369(8) Uani 1 1 d . . . C1 C 0.1209(4) 0.5098(3) 0.3040(3) 0.0379(10) Uani 1 1 d . . . C2 C 0.0585(6) 0.5320(4) 0.3663(4) 0.0576(15) Uani 1 1 d . . . H110 H 0.0750 0.5949 0.3904 0.086 Uiso 1 1 calc R . . H111 H 0.0877 0.5164 0.4118 0.086 Uiso 1 1 calc R . . H112 H -0.0292 0.4995 0.3385 0.086 Uiso 1 1 calc R . . P1 P 0.43741(10) 0.60256(7) 0.23645(7) 0.0291(2) Uani 1 1 d . . . P2 P 0.15818(9) 0.36085(7) 0.05258(7) 0.0279(2) Uani 1 1 d . . . N2 N 0.3950(3) 0.4215(2) 0.1734(2) 0.0266(7) Uani 1 1 d . . . C3 C 0.5506(4) 0.5670(3) 0.2630(3) 0.0299(8) Uani 1 1 d . . . C4 C 0.2332(4) 0.2932(3) 0.0582(3) 0.0303(8) Uani 1 1 d . . . C5 C 0.5159(4) 0.4713(3) 0.2145(3) 0.0301(8) Uani 1 1 d . . . C6 C 0.6032(4) 0.4334(3) 0.2041(3) 0.0368(10) Uani 1 1 d . . . H1 H 0.6870 0.4682 0.2329 0.044 Uiso 1 1 calc R . . C7 C 0.5674(4) 0.3449(3) 0.1517(3) 0.0376(10) Uani 1 1 d . . . H2 H 0.6256 0.3178 0.1475 0.045 Uiso 1 1 calc R . . C8 C 0.4453(4) 0.2966(3) 0.1057(3) 0.0348(9) Uani 1 1 d . . . H3 H 0.4194 0.2364 0.0678 0.042 Uiso 1 1 calc R . . C9 C 0.3607(4) 0.3369(3) 0.1154(3) 0.0301(8) Uani 1 1 d . . . C10 C 0.6760(4) 0.6188(3) 0.3238(3) 0.0328(9) Uani 1 1 d . . . C11 C 0.7466(4) 0.6977(3) 0.3283(3) 0.0371(10) Uani 1 1 d . . . H4 H 0.7156 0.7195 0.2907 0.045 Uiso 1 1 calc R . . C12 C 0.8630(4) 0.7449(3) 0.3880(3) 0.0488(13) Uani 1 1 d . . . H5 H 0.9099 0.7994 0.3915 0.059 Uiso 1 1 calc R . . C13 C 0.9110(4) 0.7138(4) 0.4417(3) 0.0529(14) Uani 1 1 d . . . H6 H 0.9908 0.7461 0.4814 0.063 Uiso 1 1 calc R . . C14 C 0.8423(5) 0.6351(4) 0.4374(3) 0.0504(13) Uani 1 1 d . . . H7 H 0.8752 0.6131 0.4742 0.060 Uiso 1 1 calc R . . C15 C 0.7257(4) 0.5882(3) 0.3799(3) 0.0415(11) Uani 1 1 d . . . H8 H 0.6788 0.5346 0.3782 0.050 Uiso 1 1 calc R . . C16 C 0.1888(4) 0.1963(3) 0.0088(3) 0.0347(9) Uani 1 1 d . . . C17 C 0.1902(4) 0.1449(3) 0.0525(3) 0.0386(10) Uani 1 1 d . . . H9 H 0.2202 0.1722 0.1129 0.046 Uiso 1 1 calc R . . C18 C 0.1483(5) 0.0544(3) 0.0086(4) 0.0477(12) Uani 1 1 d . . . H10 H 0.1473 0.0199 0.0390 0.057 Uiso 1 1 calc R . . C19 C 0.1078(5) 0.0143(3) -0.0795(4) 0.0540(14) Uani 1 1 d . . . H11 H 0.0806 -0.0476 -0.1095 0.065 Uiso 1 1 calc R . . C20 C 0.1072(5) 0.0643(3) -0.1237(4) 0.0498(13) Uani 1 1 d . . . H12 H 0.0789 0.0366 -0.1841 0.060 Uiso 1 1 calc R . . C21 C 0.1477(4) 0.1553(3) -0.0803(3) 0.0404(11) Uani 1 1 d . . . H13 H 0.1474 0.1893 -0.1111 0.048 Uiso 1 1 calc R . . C22 C 0.4989(4) 0.7219(3) 0.2853(3) 0.0279(8) Uani 1 1 d . . . C23 C 0.5230(4) 0.7599(3) 0.2289(3) 0.0307(8) Uani 1 1 d . . . C24 C 0.6086(4) 0.8445(3) 0.2643(3) 0.0366(10) Uani 1 1 d . . . H14 H 0.6295 0.8691 0.2273 0.044 Uiso 1 1 calc R . . C25 C 0.6651(4) 0.8950(3) 0.3520(3) 0.0374(10) Uani 1 1 d . A . C26 C 0.6231(4) 0.8609(3) 0.4041(3) 0.0368(10) Uani 1 1 d . . . H15 H 0.6526 0.8971 0.4637 0.044 Uiso 1 1 calc R . . C27 C 0.5391(4) 0.7756(3) 0.3734(3) 0.0330(9) Uani 1 1 d . B . C28 C 0.4553(4) 0.7131(3) 0.1307(3) 0.0368(10) Uani 1 1 d . . . C29 C 0.3173(4) 0.6779(3) 0.1138(3) 0.0402(10) Uani 1 1 d . . . H23 H 0.2932 0.7255 0.1454 0.060 Uiso 1 1 calc R . . H24 H 0.2965 0.6316 0.1324 0.060 Uiso 1 1 calc R . . H25 H 0.2744 0.6541 0.0529 0.060 Uiso 1 1 calc R . . C30 C 0.4952(5) 0.6396(4) 0.0817(3) 0.0518(13) Uani 1 1 d . . . H26 H 0.5832 0.6630 0.0931 0.078 Uiso 1 1 calc R . . H27 H 0.4530 0.6158 0.0206 0.078 Uiso 1 1 calc R . . H28 H 0.4750 0.5930 0.0999 0.078 Uiso 1 1 calc R . . C31 C 0.4768(5) 0.7791(4) 0.0919(3) 0.0480(12) Uani 1 1 d . . . H29 H 0.4524 0.8274 0.1215 0.072 Uiso 1 1 calc R . . H30 H 0.4284 0.7495 0.0315 0.072 Uiso 1 1 calc R . . H31 H 0.5631 0.8020 0.0982 0.072 Uiso 1 1 calc R . . C32 C 0.7631(5) 0.9871(3) 0.3879(4) 0.0535(14) Uani 1 1 d . . . C33 C 0.8836(15) 0.9725(11) 0.3759(12) 0.085(5) Uiso 0.536(16) 1 d P A 1 H32 H 0.8689 0.9368 0.3156 0.128 Uiso 0.536(16) 1 calc PR A 1 H33 H 0.9080 0.9425 0.4091 0.128 Uiso 0.536(16) 1 calc PR A 1 H34 H 0.9485 1.0293 0.3955 0.128 Uiso 0.536(16) 1 calc PR A 1 C34 C 0.7382(14) 1.0329(10) 0.3310(10) 0.079(5) Uiso 0.536(16) 1 d P A 1 H35 H 0.7259 0.9942 0.2720 0.119 Uiso 0.536(16) 1 calc PR A 1 H36 H 0.8077 1.0873 0.3505 0.119 Uiso 0.536(16) 1 calc PR A 1 H37 H 0.6651 1.0464 0.3342 0.119 Uiso 0.536(16) 1 calc PR A 1 C35 C 0.7857(16) 1.0441(11) 0.4788(10) 0.084(5) Uiso 0.536(16) 1 d P A 1 H38 H 0.8490 1.1010 0.4965 0.127 Uiso 0.536(16) 1 calc PR A 1 H39 H 0.8124 1.0164 0.5140 0.127 Uiso 0.536(16) 1 calc PR A 1 H40 H 0.7106 1.0523 0.4859 0.127 Uiso 0.536(16) 1 calc PR A 1 C36 C 0.8528(19) 0.9858(13) 0.3422(14) 0.089(6) Uiso 0.464(16) 1 d P A 2 H41 H 0.9142 1.0448 0.3658 0.133 Uiso 0.464(16) 1 calc PR A 2 H42 H 0.8114 0.9662 0.2817 0.133 Uiso 0.464(16) 1 calc PR A 2 H43 H 0.8922 0.9457 0.3489 0.133 Uiso 0.464(16) 1 calc PR A 2 C37 C 0.7035(18) 1.0505(13) 0.3802(14) 0.094(7) Uiso 0.464(16) 1 d P A 2 H44 H 0.6444 1.0507 0.4107 0.141 Uiso 0.464(16) 1 calc PR A 2 H45 H 0.6619 1.0324 0.3200 0.141 Uiso 0.464(16) 1 calc PR A 2 H46 H 0.7656 1.1094 0.4048 0.141 Uiso 0.464(16) 1 calc PR A 2 C38 C 0.8382(17) 1.0156(12) 0.4815(11) 0.081(5) Uiso 0.464(16) 1 d P A 2 H47 H 0.7852 1.0206 0.5166 0.121 Uiso 0.464(16) 1 calc PR A 2 H48 H 0.9040 1.0724 0.5028 0.121 Uiso 0.464(16) 1 calc PR A 2 H49 H 0.8727 0.9719 0.4840 0.121 Uiso 0.464(16) 1 calc PR A 2 C39 C 0.4920(6) 0.7517(3) 0.4396(3) 0.0509(14) Uani 1 1 d . . . C40 C 0.6115(9) 0.7558(6) 0.5052(6) 0.057(3) Uiso 0.628(8) 1 d P B 1 H50 H 0.6765 0.8131 0.5275 0.085 Uiso 0.628(8) 1 calc PR B 1 H51 H 0.6394 0.7098 0.4750 0.085 Uiso 0.628(8) 1 calc PR B 1 H52 H 0.5903 0.7468 0.5523 0.085 Uiso 0.628(8) 1 calc PR B 1 C41 C 0.4583(8) 0.8260(5) 0.4927(6) 0.044(2) Uiso 0.628(8) 1 d P B 1 H53 H 0.5251 0.8819 0.5125 0.067 Uiso 0.628(8) 1 calc PR B 1 H54 H 0.4435 0.8178 0.5417 0.067 Uiso 0.628(8) 1 calc PR B 1 H55 H 0.3847 0.8261 0.4579 0.067 Uiso 0.628(8) 1 calc PR B 1 C42 C 0.3979(9) 0.6680(6) 0.4087(6) 0.056(2) Uiso 0.628(8) 1 d P B 1 H56 H 0.4234 0.6222 0.3751 0.084 Uiso 0.628(8) 1 calc PR B 1 H57 H 0.3236 0.6663 0.3729 0.084 Uiso 0.628(8) 1 calc PR B 1 H58 H 0.3823 0.6581 0.4568 0.084 Uiso 0.628(8) 1 calc PR B 1 C43 C 0.4896(16) 0.6664(11) 0.4426(11) 0.058(4) Uiso 0.372(8) 1 d P B 2 H59 H 0.4774 0.6230 0.3856 0.087 Uiso 0.372(8) 1 calc PR B 2 H60 H 0.4229 0.6450 0.4622 0.087 Uiso 0.372(8) 1 calc PR B 2 H61 H 0.5669 0.6763 0.4818 0.087 Uiso 0.372(8) 1 calc PR B 2 C44 C 0.5120(16) 0.8198(11) 0.5222(11) 0.056(4) Uiso 0.372(8) 1 d P B 2 H62 H 0.5138 0.8735 0.5171 0.084 Uiso 0.372(8) 1 calc PR B 2 H63 H 0.5897 0.8308 0.5618 0.084 Uiso 0.372(8) 1 calc PR B 2 H64 H 0.4460 0.8011 0.5436 0.084 Uiso 0.372(8) 1 calc PR B 2 C45 C 0.3331(14) 0.7205(11) 0.3937(10) 0.057(4) Uiso 0.372(8) 1 d P B 2 H65 H 0.3052 0.6733 0.3360 0.085 Uiso 0.372(8) 1 calc PR B 2 H66 H 0.3156 0.7709 0.3914 0.085 Uiso 0.372(8) 1 calc PR B 2 H67 H 0.2909 0.7001 0.4283 0.085 Uiso 0.372(8) 1 calc PR B 2 C46 C 0.0092(4) 0.2903(3) -0.0292(3) 0.0275(8) Uani 1 1 d . . . C47 C -0.0057(4) 0.2859(3) -0.1127(3) 0.0305(9) Uani 1 1 d . . . C48 C -0.0956(4) 0.2119(3) -0.1797(3) 0.0368(10) Uani 1 1 d . . . H16 H -0.1051 0.2068 -0.2356 0.044 Uiso 1 1 calc R . . C49 C -0.1726(4) 0.1449(3) -0.1700(3) 0.0362(10) Uani 1 1 d . C . C50 C -0.1691(4) 0.1586(3) -0.0878(3) 0.0345(9) Uani 1 1 d . . . H17 H -0.2279 0.1167 -0.0800 0.041 Uiso 1 1 calc R . . C51 C -0.0819(4) 0.2321(3) -0.0155(3) 0.0302(8) Uani 1 1 d . . . C52 C -0.0983(4) 0.2514(3) 0.0725(3) 0.0313(9) Uani 1 1 d . . . C53 C 0.0021(4) 0.2473(3) 0.1377(3) 0.0389(10) Uani 1 1 d . . . H68 H 0.0814 0.2877 0.1450 0.058 Uiso 1 1 calc R . . H69 H 0.0018 0.1876 0.1170 0.058 Uiso 1 1 calc R . . H70 H -0.0129 0.2641 0.1923 0.058 Uiso 1 1 calc R . . C54 C -0.1050(4) 0.3427(3) 0.1089(3) 0.0348(9) Uani 1 1 d . . . H71 H -0.0299 0.3862 0.1145 0.052 Uiso 1 1 calc R . . H72 H -0.1151 0.3566 0.1649 0.052 Uiso 1 1 calc R . . H73 H -0.1744 0.3437 0.0706 0.052 Uiso 1 1 calc R . . C55 C -0.2184(4) 0.1864(3) 0.0651(3) 0.0421(11) Uani 1 1 d . . . H74 H -0.2177 0.1270 0.0421 0.063 Uiso 1 1 calc R . . H75 H -0.2865 0.1890 0.0271 0.063 Uiso 1 1 calc R . . H76 H -0.2275 0.2018 0.1215 0.063 Uiso 1 1 calc R . . C56 C -0.2621(5) 0.0610(3) -0.2494(3) 0.0471(12) Uani 1 1 d . . . C57 C -0.1919(9) 0.0137(7) -0.2940(7) 0.046(3) Uiso 0.61(3) 1 d P C 1 H77 H -0.1345 0.0527 -0.3082 0.069 Uiso 0.61(3) 1 calc PR C 1 H78 H -0.2478 -0.0376 -0.3463 0.069 Uiso 0.61(3) 1 calc PR C 1 H79 H -0.1470 -0.0053 -0.2569 0.069 Uiso 0.61(3) 1 calc PR C 1 C58 C -0.3600(15) 0.0747(11) -0.2937(11) 0.043(4) Uiso 0.39(3) 1 d P C 2 H80 H -0.4135 0.0199 -0.3434 0.065 Uiso 0.39(3) 1 calc PR C 2 H81 H -0.3284 0.1195 -0.3123 0.065 Uiso 0.39(3) 1 calc PR C 2 H82 H -0.4059 0.0943 -0.2560 0.065 Uiso 0.39(3) 1 calc PR C 2 C59 C -0.3151(17) -0.0147(11) -0.2228(10) 0.047(4) Uiso 0.39(3) 1 d P C 2 H83 H -0.2478 -0.0244 -0.1918 0.03(3) Uiso 0.39(3) 1 calc PR C 2 H84 H -0.3667 -0.0688 -0.2739 0.045 Uiso 0.39(3) 1 calc PR C 2 H85 H -0.3634 0.0027 -0.1862 0.045 Uiso 0.39(3) 1 calc PR C 2 C60 C -0.1843(13) 0.0293(11) -0.3109(11) 0.039(4) Uiso 0.39(3) 1 d P C 2 H86 H -0.1181 0.0184 -0.2803 0.059 Uiso 0.39(3) 1 calc PR C 2 H87 H -0.1504 0.0750 -0.3279 0.059 Uiso 0.39(3) 1 calc PR C 2 H88 H -0.2376 -0.0246 -0.3617 0.059 Uiso 0.39(3) 1 calc PR C 2 C61 C -0.3384(9) 0.0908(7) -0.3114(7) 0.044(2) Uiso 0.61(3) 1 d P C 1 H89 H -0.3855 0.1213 -0.2823 0.066 Uiso 0.61(3) 1 calc PR C 1 H90 H -0.3937 0.0390 -0.3634 0.066 Uiso 0.61(3) 1 calc PR C 1 H91 H -0.2821 0.1301 -0.3260 0.066 Uiso 0.61(3) 1 calc PR C 1 C62 C -0.3511(12) 0.0024(8) -0.2292(7) 0.055(3) Uiso 0.61(3) 1 d P C 1 H92 H -0.3967 0.0342 -0.1998 0.082 Uiso 0.61(3) 1 calc PR C 1 H93 H -0.3080 -0.0178 -0.1925 0.082 Uiso 0.61(3) 1 calc PR C 1 H94 H -0.4074 -0.0481 -0.2819 0.082 Uiso 0.61(3) 1 calc PR C 1 C63 C 0.0683(4) 0.3595(3) -0.1311(3) 0.0377(10) Uani 1 1 d . . . C64 C 0.1975(5) 0.3617(4) -0.1256(4) 0.0511(13) Uani 1 1 d . . . H95 H 0.1937 0.3046 -0.1648 0.077 Uiso 1 1 calc R . . H96 H 0.2425 0.3753 -0.0674 0.077 Uiso 1 1 calc R . . H97 H 0.2389 0.4068 -0.1411 0.077 Uiso 1 1 calc R . . C65 C 0.0717(6) 0.4484(3) -0.0702(4) 0.0510(13) Uani 1 1 d . . . H98 H -0.0115 0.4460 -0.0747 0.077 Uiso 1 1 calc R . . H99 H 0.1129 0.4939 -0.0853 0.077 Uiso 1 1 calc R . . H100 H 0.1159 0.4622 -0.0117 0.077 Uiso 1 1 calc R . . C66 C 0.0061(5) 0.3477(4) -0.2210(3) 0.0539(14) Uani 1 1 d . . . H101 H -0.0769 0.3461 -0.2267 0.081 Uiso 1 1 calc R . . H102 H 0.0038 0.2927 -0.2635 0.081 Uiso 1 1 calc R . . H103 H 0.0521 0.3967 -0.2299 0.081 Uiso 1 1 calc R . . Sb1 Sb 0.21156(3) -0.31319(2) -0.36582(2) 0.04480(11) Uani 1 1 d . . . F1 F 0.2607(4) -0.3994(3) -0.4296(3) 0.0910(14) Uani 1 1 d . . . F2 F 0.1594(4) -0.2291(3) -0.3030(3) 0.0981(15) Uani 1 1 d . . . F3 F 0.0507(3) -0.3867(3) -0.4291(2) 0.0662(10) Uani 1 1 d . . . F4 F 0.3721(4) -0.2411(3) -0.3028(3) 0.1012(16) Uani 1 1 d . . . F5 F 0.2101(4) -0.2682(3) -0.4457(3) 0.0936(14) Uani 1 1 d . . . F6 F 0.2055(4) -0.3615(3) -0.2891(3) 0.0940(15) Uani 1 1 d . . . C71 C 0.2206(7) 0.2676(5) 0.3251(4) 0.0658(18) Uani 1 1 d . . . C72 C 0.2134(6) 0.3462(4) 0.3697(4) 0.0566(14) Uani 1 1 d . . . H18 H 0.1395 0.3470 0.3801 0.068 Uiso 1 1 calc R . . C73 C 0.3085(7) 0.4246(5) 0.4002(5) 0.0705(18) Uani 1 1 d . . . H19 H 0.2999 0.4776 0.4325 0.085 Uiso 1 1 calc R . . C74 C 0.4136(7) 0.4269(6) 0.3845(5) 0.081(2) Uani 1 1 d . . . H20 H 0.4795 0.4812 0.4068 0.097 Uiso 1 1 calc R . . C75 C 0.4255(7) 0.3512(7) 0.3367(5) 0.083(2) Uani 1 1 d . . . H21 H 0.4985 0.3533 0.3237 0.099 Uiso 1 1 calc R . . C76 C 0.3329(9) 0.2720(7) 0.3071(5) 0.090(3) Uani 1 1 d . . . H22 H 0.3428 0.2196 0.2745 0.108 Uiso 1 1 calc R . . C77 C 0.1175(4) 0.1842(3) 0.2960(3) 0.129(5) Uani 1 1 d . . . H107 H 0.1394 0.1350 0.2650 0.194 Uiso 1 1 calc R . . H108 H 0.0460 0.1837 0.2583 0.194 Uiso 1 1 calc R . . H109 H 0.0991 0.1789 0.3453 0.194 Uiso 1 1 calc R . . C68 C 0.4379(4) 0.0497(3) -0.0053(3) 0.092(2) Uiso 1 1 d RD D . H113 H 0.3926 0.0848 -0.0119 0.110 Uiso 1 1 calc R . . C67 C 0.4377(4) -0.0131(3) -0.0728(3) 0.102(3) Uiso 1 1 d RD . . C69 C 0.4912(4) 0.0631(3) 0.0613(3) 0.116(3) Uiso 1 1 d RD . . C70 C 0.4971(4) 0.1229(3) 0.1237(3) 0.27(12) Uiso 0.25 1 d PRD D 1 H70A H 0.5471 0.1230 0.1742 0.409 Uiso 0.25 1 calc PR E 1 H70B H 0.4153 0.1164 0.1268 0.409 Uiso 0.25 1 calc PR F 1 H70C H 0.5340 0.1781 0.1211 0.409 Uiso 0.25 1 calc PR G 1 H120 H 0.4971 0.1229 0.1237 0.0(3) Uiso 0.75 1 d PR H 2 C70A C 0.3814(4) -0.0405(3) -0.1481(3) 0.051(6) Uiso 0.25 1 d PRD I 1 H122 H 0.2957 -0.0733 -0.1595 0.077 Uiso 0.25 1 calc PR J 1 H123 H 0.4155 -0.0790 -0.1829 0.077 Uiso 0.25 1 calc PR K 1 H124 H 0.3879 0.0089 -0.1623 0.077 Uiso 0.25 1 calc PR L 1 H121 H 0.3814 -0.0405 -0.1481 0.00(3) Uiso 0.75 1 d PR M 2 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 0.0261(2) 0.0277(2) 0.0273(3) 0.0070(2) 0.0045(2) 0.00907(19) N1 0.0339(19) 0.0356(19) 0.033(2) 0.0097(16) 0.0092(16) 0.0103(16) C1 0.038(2) 0.033(2) 0.030(2) 0.0077(18) 0.0061(19) 0.0063(18) C2 0.060(3) 0.064(4) 0.044(3) 0.017(3) 0.028(3) 0.015(3) P1 0.0265(5) 0.0267(5) 0.0256(5) 0.0074(4) 0.0024(4) 0.0077(4) P2 0.0267(5) 0.0253(5) 0.0258(5) 0.0082(4) 0.0036(4) 0.0085(4) N2 0.0258(15) 0.0277(16) 0.0239(16) 0.0096(13) 0.0047(13) 0.0112(13) C3 0.0281(19) 0.030(2) 0.026(2) 0.0091(16) 0.0064(16) 0.0081(16) C4 0.0295(19) 0.0275(19) 0.025(2) 0.0075(16) 0.0030(16) 0.0073(16) C5 0.0302(19) 0.032(2) 0.0238(19) 0.0107(16) 0.0020(16) 0.0129(16) C6 0.031(2) 0.042(2) 0.033(2) 0.014(2) 0.0029(18) 0.0156(19) C7 0.035(2) 0.041(2) 0.037(2) 0.014(2) 0.0084(19) 0.0211(19) C8 0.038(2) 0.033(2) 0.030(2) 0.0107(18) 0.0083(18) 0.0153(18) C9 0.030(2) 0.033(2) 0.025(2) 0.0122(17) 0.0062(16) 0.0125(17) C10 0.0269(19) 0.039(2) 0.024(2) 0.0082(17) 0.0031(16) 0.0099(17) C11 0.029(2) 0.038(2) 0.036(2) 0.0096(19) 0.0078(18) 0.0115(18) C12 0.023(2) 0.045(3) 0.051(3) 0.005(2) 0.005(2) 0.0009(19) C13 0.028(2) 0.062(3) 0.040(3) 0.004(3) -0.005(2) 0.012(2) C14 0.039(3) 0.071(4) 0.032(3) 0.014(3) 0.000(2) 0.027(3) C15 0.036(2) 0.048(3) 0.032(2) 0.015(2) 0.0024(19) 0.014(2) C16 0.029(2) 0.029(2) 0.035(2) 0.0053(18) 0.0050(17) 0.0103(17) C17 0.044(3) 0.032(2) 0.039(3) 0.016(2) 0.010(2) 0.0128(19) C18 0.048(3) 0.036(3) 0.062(4) 0.024(2) 0.017(3) 0.018(2) C19 0.050(3) 0.031(2) 0.066(4) 0.008(2) 0.010(3) 0.018(2) C20 0.045(3) 0.035(2) 0.044(3) -0.001(2) -0.002(2) 0.014(2) C21 0.041(2) 0.036(2) 0.036(2) 0.008(2) 0.004(2) 0.018(2) C22 0.0248(18) 0.0275(19) 0.0250(19) 0.0089(16) 0.0040(15) 0.0071(15) C23 0.0266(19) 0.033(2) 0.030(2) 0.0140(17) 0.0073(16) 0.0088(16) C24 0.033(2) 0.038(2) 0.039(2) 0.022(2) 0.0075(19) 0.0092(18) C25 0.028(2) 0.029(2) 0.043(3) 0.0122(19) 0.0042(19) 0.0034(17) C26 0.033(2) 0.031(2) 0.032(2) 0.0081(18) -0.0002(18) 0.0049(17) C27 0.033(2) 0.034(2) 0.027(2) 0.0120(18) 0.0054(17) 0.0097(17) C28 0.037(2) 0.045(3) 0.029(2) 0.017(2) 0.0072(18) 0.019(2) C29 0.036(2) 0.041(2) 0.034(2) 0.013(2) -0.0012(19) 0.014(2) C30 0.060(3) 0.065(4) 0.035(3) 0.017(3) 0.020(2) 0.035(3) C31 0.055(3) 0.059(3) 0.036(3) 0.028(2) 0.014(2) 0.020(3) C32 0.041(3) 0.039(3) 0.056(3) 0.017(3) -0.001(2) -0.004(2) C39 0.082(4) 0.038(3) 0.030(2) 0.013(2) 0.021(3) 0.017(3) C46 0.0262(18) 0.0258(18) 0.0242(19) 0.0080(15) 0.0026(15) 0.0085(15) C47 0.0292(19) 0.038(2) 0.0218(19) 0.0096(17) 0.0037(16) 0.0172(17) C48 0.039(2) 0.045(3) 0.025(2) 0.0114(19) 0.0079(18) 0.021(2) C49 0.035(2) 0.033(2) 0.028(2) 0.0026(18) 0.0032(18) 0.0153(18) C50 0.028(2) 0.027(2) 0.037(2) 0.0085(18) 0.0012(18) 0.0077(16) C51 0.0278(19) 0.0275(19) 0.026(2) 0.0058(16) 0.0018(16) 0.0100(16) C52 0.034(2) 0.029(2) 0.028(2) 0.0123(17) 0.0075(17) 0.0103(17) C53 0.037(2) 0.049(3) 0.038(3) 0.025(2) 0.013(2) 0.018(2) C54 0.037(2) 0.036(2) 0.028(2) 0.0130(18) 0.0084(18) 0.0126(18) C55 0.040(2) 0.040(3) 0.039(3) 0.016(2) 0.011(2) 0.006(2) C56 0.040(3) 0.044(3) 0.034(3) -0.001(2) 0.003(2) 0.013(2) C63 0.040(2) 0.046(3) 0.034(2) 0.023(2) 0.0113(19) 0.017(2) C64 0.042(3) 0.075(4) 0.048(3) 0.034(3) 0.021(2) 0.024(3) C65 0.067(4) 0.043(3) 0.048(3) 0.027(2) 0.016(3) 0.020(3) C66 0.058(3) 0.068(4) 0.040(3) 0.028(3) 0.013(3) 0.027(3) Sb1 0.03843(18) 0.0528(2) 0.0400(2) 0.01642(16) 0.01190(14) 0.01814(15) F1 0.081(3) 0.083(3) 0.093(3) 0.009(2) 0.028(2) 0.047(2) F2 0.107(4) 0.096(3) 0.091(3) 0.018(3) 0.042(3) 0.061(3) F3 0.0422(17) 0.084(3) 0.065(2) 0.042(2) 0.0008(16) 0.0119(17) F4 0.048(2) 0.084(3) 0.111(4) 0.002(3) 0.004(2) 0.007(2) F5 0.102(3) 0.099(3) 0.092(3) 0.062(3) 0.039(3) 0.021(3) F6 0.084(3) 0.134(4) 0.068(3) 0.065(3) 0.003(2) 0.035(3) C71 0.081(5) 0.067(4) 0.048(3) 0.025(3) 0.002(3) 0.040(4) C72 0.057(3) 0.072(4) 0.052(3) 0.035(3) 0.017(3) 0.030(3) C73 0.079(5) 0.074(5) 0.067(4) 0.038(4) 0.021(4) 0.033(4) C74 0.068(5) 0.115(7) 0.081(5) 0.063(5) 0.022(4) 0.036(5) C75 0.068(5) 0.143(8) 0.078(5) 0.072(6) 0.038(4) 0.057(5) C76 0.129(8) 0.118(7) 0.050(4) 0.039(5) 0.026(5) 0.086(7) C77 0.145(9) 0.063(5) 0.120(8) 0.044(5) -0.048(7) 0.009(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 1.928(4) . ? Cu1 N2 2.059(3) . ? Cu1 P1 2.2828(12) . ? Cu1 P2 2.2900(12) . ? N1 C1 1.138(6) . ? C1 C2 1.460(7) . ? C2 H110 0.9800 . ? C2 H111 0.9800 . ? C2 H112 0.9800 . ? P1 C3 1.704(4) . ? P1 C22 1.824(4) . ? P2 C4 1.697(4) . ? P2 C46 1.837(4) . ? N2 C9 1.361(5) . ? N2 C5 1.368(5) . ? C3 C5 1.481(6) . ? C3 C10 1.485(6) . ? C4 C9 1.478(6) . ? C4 C16 1.490(6) . ? C5 C6 1.398(6) . ? C6 C7 1.386(6) . ? C6 H1 0.9500 . ? C7 C8 1.387(6) . ? C7 H2 0.9500 . ? C8 C9 1.395(6) . ? C8 H3 0.9500 . ? C10 C11 1.390(6) . ? C10 C15 1.408(7) . ? C11 C12 1.397(6) . ? C11 H4 0.9500 . ? C12 C13 1.373(8) . ? C12 H5 0.9500 . ? C13 C14 1.381(8) . ? C13 H6 0.9500 . ? C14 C15 1.384(7) . ? C14 H7 0.9500 . ? C15 H8 0.9500 . ? C16 C17 1.395(7) . ? C16 C21 1.400(6) . ? C17 C18 1.389(6) . ? C17 H9 0.9500 . ? C18 C19 1.385(8) . ? C18 H10 0.9500 . ? C19 C20 1.381(8) . ? C19 H11 0.9500 . ? C20 C21 1.395(6) . ? C20 H12 0.9500 . ? C21 H13 0.9500 . ? C22 C27 1.408(6) . ? C22 C23 1.432(6) . ? C23 C24 1.391(6) . ? C23 C28 1.565(6) . ? C24 C25 1.398(7) . ? C24 H14 0.9500 . ? C25 C26 1.385(7) . ? C25 C32 1.541(6) . ? C26 C27 1.403(6) . ? C26 H15 0.9500 . ? C27 C39 1.548(7) . ? C28 C30 1.536(7) . ? C28 C29 1.539(6) . ? C28 C31 1.548(7) . ? C29 H23 0.9800 . ? C29 H24 0.9800 . ? C29 H25 0.9800 . ? C30 H26 0.9800 . ? C30 H27 0.9800 . ? C30 H28 0.9800 . ? C31 H29 0.9800 . ? C31 H30 0.9800 . ? C31 H31 0.9800 . ? C32 C36 1.48(2) . ? C32 C35 1.489(16) . ? C32 C37 1.512(19) . ? C32 C34 1.543(15) . ? C32 C38 1.554(18) . ? C32 C33 1.585(17) . ? C33 H32 0.9800 . ? C33 H33 0.9800 . ? C33 H34 0.9800 . ? C34 H35 0.9800 . ? C34 H36 0.9800 . ? C34 H37 0.9800 . ? C35 H38 0.9800 . ? C35 H39 0.9800 . ? C35 H40 0.9800 . ? C36 H41 0.9800 . ? C36 H42 0.9800 . ? C36 H43 0.9800 . ? C37 H44 0.9800 . ? C37 H45 0.9800 . ? C37 H46 0.9800 . ? C38 H47 0.9800 . ? C38 H48 0.9800 . ? C38 H49 0.9800 . ? C39 C42 1.430(10) . ? C39 C44 1.448(16) . ? C39 C43 1.516(17) . ? C39 C41 1.522(10) . ? C39 C40 1.635(11) . ? C39 C45 1.775(17) . ? C40 H50 0.9800 . ? C40 H51 0.9800 . ? C40 H52 0.9800 . ? C41 H53 0.9800 . ? C41 H54 0.9800 . ? C41 H55 0.9800 . ? C42 H56 0.9800 . ? C42 H57 0.9800 . ? C42 H58 0.9800 . ? C43 H59 0.9800 . ? C43 H60 0.9800 . ? C43 H61 0.9800 . ? C44 H62 0.9800 . ? C44 H63 0.9800 . ? C44 H64 0.9800 . ? C45 H65 0.9800 . ? C45 H66 0.9800 . ? C45 H67 0.9800 . ? C46 C51 1.420(6) . ? C46 C47 1.436(6) . ? C47 C48 1.385(6) . ? C47 C63 1.550(6) . ? C48 C49 1.386(7) . ? C48 H16 0.9500 . ? C49 C50 1.389(7) . ? C49 C56 1.547(6) . ? C50 C51 1.408(5) . ? C50 H17 0.9500 . ? C51 C52 1.547(6) . ? C52 C54 1.535(6) . ? C52 C55 1.539(6) . ? C52 C53 1.542(6) . ? C53 H68 0.9800 . ? C53 H69 0.9800 . ? C53 H70 0.9800 . ? C54 H71 0.9800 . ? C54 H72 0.9800 . ? C54 H73 0.9800 . ? C55 H74 0.9800 . ? C55 H75 0.9800 . ? C55 H76 0.9800 . ? C56 C58 1.414(16) . ? C56 C62 1.480(11) . ? C56 C57 1.487(11) . ? C56 C59 1.596(16) . ? C56 C61 1.618(12) . ? C56 C60 1.626(16) . ? C57 H77 0.9800 . ? C57 H78 0.9800 . ? C57 H79 0.9800 . ? C58 H80 0.9800 . ? C58 H81 0.9800 . ? C58 H82 0.9800 . ? C59 H83 0.9800 . ? C59 H84 0.9800 . ? C59 H85 0.9800 . ? C60 H86 0.9800 . ? C60 H87 0.9800 . ? C60 H88 0.9800 . ? C61 H89 0.9800 . ? C61 H90 0.9800 . ? C61 H91 0.9800 . ? C62 H92 0.9800 . ? C62 H93 0.9800 . ? C62 H94 0.9800 . ? C63 C64 1.532(7) . ? C63 C65 1.536(7) . ? C63 C66 1.543(7) . ? C64 H95 0.9800 . ? C64 H96 0.9800 . ? C64 H97 0.9800 . ? C65 H98 0.9800 . ? C65 H99 0.9800 . ? C65 H100 0.9800 . ? C66 H101 0.9800 . ? C66 H102 0.9800 . ? C66 H103 0.9800 . ? Sb1 F2 1.850(4) . ? Sb1 F4 1.853(4) . ? Sb1 F1 1.858(4) . ? Sb1 F6 1.860(4) . ? Sb1 F3 1.862(3) . ? Sb1 F5 1.866(4) . ? C71 C72 1.363(9) . ? C71 C76 1.442(11) . ? C71 C77 1.484(8) . ? C72 C73 1.375(9) . ? C72 H18 0.9500 . ? C73 C74 1.347(10) . ? C73 H19 0.9500 . ? C74 C75 1.362(11) . ? C74 H20 0.9500 . ? C75 C76 1.373(12) . ? C75 H21 0.9500 . ? C76 H22 0.9500 . ? C77 H107 0.9800 . ? C77 H108 0.9800 . ? C77 H109 0.9800 . ? C68 C69 1.1384 . ? C68 C67 1.3065 . ? C68 H113 0.9500 . ? C67 C70A 1.2239 . ? C67 C69 1.423(8) 2_655 ? C67 H121 1.2239 . ? C69 C70 1.1982 . ? C69 C67 1.423(8) 2_655 ? C69 H120 1.1982 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C70 H120 0.0000 . ? C70A H122 0.9802 . ? C70A H123 0.9798 . ? C70A H124 0.9805 . ? C70A H121 0.0000 . ? 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 N2 131.57(16) . . ? N1 Cu1 P1 108.87(12) . . ? N2 Cu1 P1 81.32(10) . . ? N1 Cu1 P2 111.17(12) . . ? N2 Cu1 P2 82.45(10) . . ? P1 Cu1 P2 137.65(5) . . ? C1 N1 Cu1 174.8(4) . . ? N1 C1 C2 178.2(5) . . ? C1 C2 H110 109.5 . . ? C1 C2 H111 109.5 . . ? H110 C2 H111 109.5 . . ? C1 C2 H112 109.5 . . ? H110 C2 H112 109.5 . . ? H111 C2 H112 109.5 . . ? C3 P1 C22 108.79(19) . . ? C3 P1 Cu1 102.58(15) . . ? C22 P1 Cu1 146.15(14) . . ? C4 P2 C46 105.84(19) . . ? C4 P2 Cu1 99.83(14) . . ? C46 P2 Cu1 147.73(14) . . ? C9 N2 C5 119.5(3) . . ? C9 N2 Cu1 119.2(3) . . ? C5 N2 Cu1 120.3(3) . . ? C5 C3 C10 118.2(4) . . ? C5 C3 P1 112.9(3) . . ? C10 C3 P1 128.8(3) . . ? C9 C4 C16 116.5(4) . . ? C9 C4 P2 115.5(3) . . ? C16 C4 P2 127.9(3) . . ? N2 C5 C6 120.3(4) . . ? N2 C5 C3 117.8(4) . . ? C6 C5 C3 121.7(4) . . ? C7 C6 C5 120.0(4) . . ? C7 C6 H1 120.0 . . ? C5 C6 H1 120.0 . . ? C6 C7 C8 119.0(4) . . ? C6 C7 H2 120.5 . . ? C8 C7 H2 120.5 . . ? C7 C8 C9 119.6(4) . . ? C7 C8 H3 120.2 . . ? C9 C8 H3 120.2 . . ? N2 C9 C8 121.0(4) . . ? N2 C9 C4 117.0(4) . . ? C8 C9 C4 121.8(4) . . ? C11 C10 C15 118.3(4) . . ? C11 C10 C3 122.3(4) . . ? C15 C10 C3 119.4(4) . . ? C10 C11 C12 120.0(5) . . ? C10 C11 H4 120.0 . . ? C12 C11 H4 120.0 . . ? C13 C12 C11 121.1(5) . . ? C13 C12 H5 119.4 . . ? C11 C12 H5 119.4 . . ? C12 C13 C14 119.5(5) . . ? C12 C13 H6 120.3 . . ? C14 C13 H6 120.3 . . ? C13 C14 C15 120.3(5) . . ? C13 C14 H7 119.8 . . ? C15 C14 H7 119.8 . . ? C14 C15 C10 120.8(5) . . ? C14 C15 H8 119.6 . . ? C10 C15 H8 119.6 . . ? C17 C16 C21 118.9(4) . . ? C17 C16 C4 119.0(4) . . ? C21 C16 C4 122.1(4) . . ? C18 C17 C16 120.7(5) . . ? C18 C17 H9 119.7 . . ? C16 C17 H9 119.7 . . ? C19 C18 C17 120.0(5) . . ? C19 C18 H10 120.0 . . ? C17 C18 H10 120.0 . . ? C20 C19 C18 120.0(5) . . ? C20 C19 H11 120.0 . . ? C18 C19 H11 120.0 . . ? C19 C20 C21 120.5(5) . . ? C19 C20 H12 119.8 . . ? C21 C20 H12 119.8 . . ? C20 C21 C16 119.9(5) . . ? C20 C21 H13 120.0 . . ? C16 C21 H13 120.0 . . ? C27 C22 C23 119.7(4) . . ? C27 C22 P1 124.5(3) . . ? C23 C22 P1 115.1(3) . . ? C24 C23 C22 117.7(4) . . ? C24 C23 C28 118.5(4) . . ? C22 C23 C28 123.7(4) . . ? C23 C24 C25 122.8(4) . . ? C23 C24 H14 118.6 . . ? C25 C24 H14 118.6 . . ? C26 C25 C24 116.9(4) . . ? C26 C25 C32 122.1(4) . . ? C24 C25 C32 120.8(5) . . ? C25 C26 C27 123.3(4) . . ? C25 C26 H15 118.3 . . ? C27 C26 H15 118.4 . . ? C26 C27 C22 117.7(4) . . ? C26 C27 C39 116.2(4) . . ? C22 C27 C39 126.0(4) . . ? C30 C28 C29 110.5(4) . . ? C30 C28 C31 106.6(4) . . ? C29 C28 C31 105.3(4) . . ? C30 C28 C23 114.0(4) . . ? C29 C28 C23 109.3(4) . . ? C31 C28 C23 110.8(4) . . ? C28 C29 H23 109.5 . . ? C28 C29 H24 109.5 . . ? H23 C29 H24 109.5 . . ? C28 C29 H25 109.5 . . ? H23 C29 H25 109.5 . . ? H24 C29 H25 109.5 . . ? C28 C30 H26 109.5 . . ? C28 C30 H27 109.5 . . ? H26 C30 H27 109.5 . . ? C28 C30 H28 109.5 . . ? H26 C30 H28 109.5 . . ? H27 C30 H28 109.5 . . ? C28 C31 H29 109.5 . . ? C28 C31 H30 109.5 . . ? H29 C31 H30 109.5 . . ? C28 C31 H31 109.5 . . ? H29 C31 H31 109.5 . . ? H30 C31 H31 109.5 . . ? C36 C32 C35 127.2(11) . . ? C36 C32 C37 110.3(12) . . ? C35 C32 C37 78.6(10) . . ? C36 C32 C25 110.6(9) . . ? C35 C32 C25 114.8(8) . . ? C37 C32 C25 109.5(9) . . ? C36 C32 C34 73.4(10) . . ? C35 C32 C34 111.7(9) . . ? C37 C32 C34 39.4(8) . . ? C25 C32 C34 111.3(7) . . ? C36 C32 C38 104.6(11) . . ? C35 C32 C38 34.8(8) . . ? C37 C32 C38 112.1(11) . . ? C25 C32 C38 109.7(8) . . ? C34 C32 C38 136.5(10) . . ? C36 C32 C33 29.4(9) . . ? C35 C32 C33 110.0(10) . . ? C37 C32 C33 135.3(11) . . ? C25 C32 C33 106.0(7) . . ? C34 C32 C33 102.1(9) . . ? C38 C32 C33 79.4(9) . . ? C32 C33 H32 109.5 . . ? C32 C33 H33 109.4 . . ? H32 C33 H33 109.5 . . ? C32 C33 H34 109.5 . . ? H32 C33 H34 109.5 . . ? H33 C33 H34 109.5 . . ? C32 C34 H35 109.5 . . ? C32 C34 H36 109.5 . . ? H35 C34 H36 109.5 . . ? C32 C34 H37 109.5 . . ? H35 C34 H37 109.5 . . ? H36 C34 H37 109.5 . . ? C32 C35 H38 109.5 . . ? C32 C35 H39 109.5 . . ? H38 C35 H39 109.5 . . ? C32 C35 H40 109.4 . . ? H38 C35 H40 109.5 . . ? H39 C35 H40 109.5 . . ? C32 C36 H41 109.5 . . ? C32 C36 H42 109.4 . . ? H41 C36 H42 109.5 . . ? C32 C36 H43 109.5 . . ? H41 C36 H43 109.5 . . ? H42 C36 H43 109.5 . . ? C32 C37 H44 109.4 . . ? C32 C37 H45 109.5 . . ? H44 C37 H45 109.5 . . ? C32 C37 H46 109.5 . . ? H44 C37 H46 109.5 . . ? H45 C37 H46 109.5 . . ? C32 C38 H47 109.5 . . ? C32 C38 H48 109.5 . . ? H47 C38 H48 109.5 . . ? C32 C38 H49 109.4 . . ? H47 C38 H49 109.5 . . ? H48 C38 H49 109.5 . . ? C42 C39 C44 119.5(9) . . ? C42 C39 C43 46.4(7) . . ? C44 C39 C43 112.6(10) . . ? C42 C39 C41 112.2(7) . . ? C44 C39 C41 31.5(7) . . ? C43 C39 C41 132.6(8) . . ? C42 C39 C27 117.3(5) . . ? C44 C39 C27 120.2(8) . . ? C43 C39 C27 119.2(8) . . ? C41 C39 C27 108.2(5) . . ? C42 C39 C40 108.6(6) . . ? C44 C39 C40 73.5(8) . . ? C43 C39 C40 63.3(8) . . ? C41 C39 C40 104.8(6) . . ? C27 C39 C40 104.8(5) . . ? C42 C39 C45 51.3(7) . . ? C44 C39 C45 99.8(10) . . ? C43 C39 C45 97.5(9) . . ? C41 C39 C45 73.6(7) . . ? C27 C39 C45 100.9(6) . . ? C40 C39 C45 153.2(7) . . ? C39 C40 H50 109.5 . . ? C39 C40 H51 109.5 . . ? H50 C40 H51 109.5 . . ? C39 C40 H52 109.5 . . ? H50 C40 H52 109.5 . . ? H51 C40 H52 109.5 . . ? C39 C41 H53 109.5 . . ? C39 C41 H54 109.4 . . ? H53 C41 H54 109.5 . . ? C39 C41 H55 109.5 . . ? H53 C41 H55 109.5 . . ? H54 C41 H55 109.5 . . ? C39 C42 H56 109.4 . . ? C39 C42 H57 109.6 . . ? H56 C42 H57 109.5 . . ? C39 C42 H58 109.4 . . ? H56 C42 H58 109.5 . . ? H57 C42 H58 109.5 . . ? C39 C43 H59 109.5 . . ? C39 C43 H60 109.5 . . ? H59 C43 H60 109.5 . . ? C39 C43 H61 109.4 . . ? H59 C43 H61 109.5 . . ? H60 C43 H61 109.5 . . ? C39 C44 H62 109.5 . . ? C39 C44 H63 109.5 . . ? H62 C44 H63 109.5 . . ? C39 C44 H64 109.5 . . ? H62 C44 H64 109.5 . . ? H63 C44 H64 109.5 . . ? C39 C45 H65 109.5 . . ? C39 C45 H66 109.5 . . ? H65 C45 H66 109.5 . . ? C39 C45 H67 109.5 . . ? H65 C45 H67 109.5 . . ? H66 C45 H67 109.5 . . ? C51 C46 C47 120.1(4) . . ? C51 C46 P2 122.0(3) . . ? C47 C46 P2 117.2(3) . . ? C48 C47 C46 116.7(4) . . ? C48 C47 C63 119.0(4) . . ? C46 C47 C63 124.2(4) . . ? C47 C48 C49 123.9(4) . . ? C47 C48 H16 118.0 . . ? C49 C48 H16 118.0 . . ? C48 C49 C50 117.3(4) . . ? C48 C49 C56 119.8(4) . . ? C50 C49 C56 122.8(4) . . ? C49 C50 C51 122.6(4) . . ? C49 C50 H17 118.7 . . ? C51 C50 H17 118.7 . . ? C50 C51 C46 117.2(4) . . ? C50 C51 C52 119.1(4) . . ? C46 C51 C52 123.2(3) . . ? C54 C52 C55 106.9(4) . . ? C54 C52 C53 109.2(4) . . ? C55 C52 C53 105.8(4) . . ? C54 C52 C51 107.9(3) . . ? C55 C52 C51 111.5(4) . . ? C53 C52 C51 115.2(4) . . ? C52 C53 H68 109.5 . . ? C52 C53 H69 109.5 . . ? H68 C53 H69 109.5 . . ? C52 C53 H70 109.5 . . ? H68 C53 H70 109.5 . . ? H69 C53 H70 109.5 . . ? C52 C54 H71 109.5 . . ? C52 C54 H72 109.4 . . ? H71 C54 H72 109.5 . . ? C52 C54 H73 109.5 . . ? H71 C54 H73 109.5 . . ? H72 C54 H73 109.5 . . ? C52 C55 H74 109.5 . . ? C52 C55 H75 109.5 . . ? H74 C55 H75 109.5 . . ? C52 C55 H76 109.5 . . ? H74 C55 H76 109.5 . . ? H75 C55 H76 109.5 . . ? C58 C56 C62 88.1(8) . . ? C58 C56 C57 122.1(8) . . ? C62 C56 C57 110.1(7) . . ? C58 C56 C49 112.8(7) . . ? C62 C56 C49 113.1(6) . . ? C57 C56 C49 109.1(5) . . ? C58 C56 C59 108.9(9) . . ? C62 C56 C59 22.3(6) . . ? C57 C56 C59 91.7(8) . . ? C49 C56 C59 110.1(7) . . ? C58 C56 C61 19.6(7) . . ? C62 C56 C61 107.2(6) . . ? C57 C56 C61 109.5(6) . . ? C49 C56 C61 107.7(5) . . ? C59 C56 C61 127.0(8) . . ? C58 C56 C60 110.1(9) . . ? C62 C56 C60 124.6(8) . . ? C57 C56 C60 17.1(6) . . ? C49 C56 C60 106.9(6) . . ? C59 C56 C60 108.0(9) . . ? C61 C56 C60 94.8(7) . . ? C56 C57 H77 109.5 . . ? C56 C57 H78 109.5 . . ? H77 C57 H78 109.5 . . ? C56 C57 H79 109.5 . . ? H77 C57 H79 109.5 . . ? H78 C57 H79 109.5 . . ? C56 C58 H80 109.4 . . ? C56 C58 H81 109.5 . . ? H80 C58 H81 109.5 . . ? C56 C58 H82 109.5 . . ? H80 C58 H82 109.5 . . ? H81 C58 H82 109.5 . . ? C56 C59 H83 109.5 . . ? C56 C59 H84 109.4 . . ? H83 C59 H84 109.5 . . ? C56 C59 H85 109.5 . . ? H83 C59 H85 109.5 . . ? H84 C59 H85 109.5 . . ? C56 C60 H86 109.5 . . ? C56 C60 H87 109.5 . . ? H86 C60 H87 109.5 . . ? C56 C60 H88 109.5 . . ? H86 C60 H88 109.5 . . ? H87 C60 H88 109.5 . . ? C56 C61 H89 109.5 . . ? C56 C61 H90 109.5 . . ? H89 C61 H90 109.5 . . ? C56 C61 H91 109.5 . . ? H89 C61 H91 109.5 . . ? H90 C61 H91 109.5 . . ? C56 C62 H92 109.5 . . ? C56 C62 H93 109.5 . . ? H92 C62 H93 109.5 . . ? C56 C62 H94 109.5 . . ? H92 C62 H94 109.5 . . ? H93 C62 H94 109.5 . . ? C64 C63 C65 110.5(4) . . ? C64 C63 C66 107.3(4) . . ? C65 C63 C66 105.2(4) . . ? C64 C63 C47 112.5(4) . . ? C65 C63 C47 110.0(4) . . ? C66 C63 C47 111.0(4) . . ? C63 C64 H95 109.5 . . ? C63 C64 H96 109.5 . . ? H95 C64 H96 109.5 . . ? C63 C64 H97 109.5 . . ? H95 C64 H97 109.5 . . ? H96 C64 H97 109.5 . . ? C63 C65 H98 109.5 . . ? C63 C65 H99 109.5 . . ? H98 C65 H99 109.5 . . ? C63 C65 H100 109.5 . . ? H98 C65 H100 109.5 . . ? H99 C65 H100 109.5 . . ? C63 C66 H101 109.5 . . ? C63 C66 H102 109.5 . . ? H101 C66 H102 109.5 . . ? C63 C66 H103 109.5 . . ? H101 C66 H103 109.5 . . ? H102 C66 H103 109.5 . . ? F2 Sb1 F4 90.6(2) . . ? F2 Sb1 F1 178.8(2) . . ? F4 Sb1 F1 90.6(2) . . ? F2 Sb1 F6 90.0(2) . . ? F4 Sb1 F6 90.2(2) . . ? F1 Sb1 F6 89.6(2) . . ? F2 Sb1 F3 89.9(2) . . ? F4 Sb1 F3 179.3(2) . . ? F1 Sb1 F3 88.93(19) . . ? F6 Sb1 F3 89.34(17) . . ? F2 Sb1 F5 90.0(2) . . ? F4 Sb1 F5 92.4(2) . . ? F1 Sb1 F5 90.4(2) . . ? F6 Sb1 F5 177.3(2) . . ? F3 Sb1 F5 87.99(18) . . ? C72 C71 C76 115.4(7) . . ? C72 C71 C77 121.2(7) . . ? C76 C71 C77 123.4(7) . . ? C71 C72 C73 122.9(7) . . ? C71 C72 H18 118.6 . . ? C73 C72 H18 118.6 . . ? C74 C73 C72 120.6(8) . . ? C74 C73 H19 119.7 . . ? C72 C73 H19 119.7 . . ? C73 C74 C75 119.9(8) . . ? C73 C74 H20 120.1 . . ? C75 C74 H20 120.1 . . ? C74 C75 C76 120.6(8) . . ? C74 C75 H21 119.7 . . ? C76 C75 H21 119.7 . . ? C75 C76 C71 120.5(7) . . ? C75 C76 H22 119.7 . . ? C71 C76 H22 119.7 . . ? C71 C77 H107 109.5 . . ? C71 C77 H108 109.5 . . ? H107 C77 H108 109.5 . . ? C71 C77 H109 109.4 . . ? H107 C77 H109 109.5 . . ? H108 C77 H109 109.5 . . ? C69 C68 C67 121.3 . . ? C69 C68 H113 119.3 . . ? C67 C68 H113 119.3 . . ? C70A C67 C68 130.8 . . ? C70A C67 C69 110.9(4) . 2_655 ? C68 C67 C69 118.2(4) . 2_655 ? C70A C67 H121 0.0 . . ? C68 C67 H121 130.8 . . ? C69 C67 H121 110.9 2_655 . ? C68 C69 C70 122.3 . . ? C68 C69 C67 120.4(4) . 2_655 ? C70 C69 C67 117.1(4) . 2_655 ? C68 C69 H120 122.3 . . ? C70 C69 H120 0.0 . . ? C67 C69 H120 117.1 2_655 . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C69 C70 H120 0.0 . . ? H70A C70 H120 0.0 . . ? H70B C70 H120 0.0 . . ? H70C C70 H120 0.0 . . ? C67 C70A H122 109.5 . . ? C67 C70A H123 109.5 . . ? C67 C70A H124 109.5 . . ? C67 C70A H121 0.0 . . ? H122 C70A H121 0.0 . . ? H123 C70A H121 0.0 . . ? H124 C70A H121 0.0 . . ? 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 N2 Cu1 N1 C1 88(5) . . . . ? P1 Cu1 N1 C1 -7(5) . . . . ? P2 Cu1 N1 C1 -173(5) . . . . ? Cu1 N1 C1 C2 39(22) . . . . ? N1 Cu1 P1 C3 113.2(2) . . . . ? N2 Cu1 P1 C3 -17.85(18) . . . . ? P2 Cu1 P1 C3 -86.46(16) . . . . ? N1 Cu1 P1 C22 -44.5(3) . . . . ? N2 Cu1 P1 C22 -175.5(3) . . . . ? P2 Cu1 P1 C22 115.8(3) . . . . ? N1 Cu1 P2 C4 -112.3(2) . . . . ? N2 Cu1 P2 C4 19.51(18) . . . . ? P1 Cu1 P2 C4 87.71(17) . . . . ? N1 Cu1 P2 C46 30.2(3) . . . . ? N2 Cu1 P2 C46 162.0(3) . . . . ? P1 Cu1 P2 C46 -129.8(3) . . . . ? N1 Cu1 N2 C9 96.5(3) . . . . ? P1 Cu1 N2 C9 -155.9(3) . . . . ? P2 Cu1 N2 C9 -15.2(3) . . . . ? N1 Cu1 N2 C5 -95.0(3) . . . . ? P1 Cu1 N2 C5 12.6(3) . . . . ? P2 Cu1 N2 C5 153.3(3) . . . . ? C22 P1 C3 C5 -169.8(3) . . . . ? Cu1 P1 C3 C5 23.1(3) . . . . ? C22 P1 C3 C10 7.4(5) . . . . ? Cu1 P1 C3 C10 -159.6(4) . . . . ? C46 P2 C4 C9 175.0(3) . . . . ? Cu1 P2 C4 C9 -24.7(3) . . . . ? C46 P2 C4 C16 -0.9(5) . . . . ? Cu1 P2 C4 C16 159.3(4) . . . . ? C9 N2 C5 C6 -6.9(6) . . . . ? Cu1 N2 C5 C6 -175.4(3) . . . . ? C9 N2 C5 C3 167.5(4) . . . . ? Cu1 N2 C5 C3 -0.9(5) . . . . ? C10 C3 C5 N2 165.8(4) . . . . ? P1 C3 C5 N2 -16.6(5) . . . . ? C10 C3 C5 C6 -19.8(6) . . . . ? P1 C3 C5 C6 157.8(4) . . . . ? N2 C5 C6 C7 0.2(7) . . . . ? C3 C5 C6 C7 -174.0(4) . . . . ? C5 C6 C7 C8 4.4(7) . . . . ? C6 C7 C8 C9 -2.5(7) . . . . ? C5 N2 C9 C8 9.0(6) . . . . ? Cu1 N2 C9 C8 177.6(3) . . . . ? C5 N2 C9 C4 -165.3(4) . . . . ? Cu1 N2 C9 C4 3.3(5) . . . . ? C7 C8 C9 N2 -4.3(7) . . . . ? C7 C8 C9 C4 169.7(4) . . . . ? C16 C4 C9 N2 -166.8(4) . . . . ? P2 C4 C9 N2 16.8(5) . . . . ? C16 C4 C9 C8 19.0(6) . . . . ? P2 C4 C9 C8 -157.4(4) . . . . ? C5 C3 C10 C11 134.7(4) . . . . ? P1 C3 C10 C11 -42.5(6) . . . . ? C5 C3 C10 C15 -46.0(6) . . . . ? P1 C3 C10 C15 136.8(4) . . . . ? C15 C10 C11 C12 -0.8(7) . . . . ? C3 C10 C11 C12 178.5(4) . . . . ? C10 C11 C12 C13 1.5(8) . . . . ? C11 C12 C13 C14 -1.0(8) . . . . ? C12 C13 C14 C15 -0.3(8) . . . . ? C13 C14 C15 C10 1.1(8) . . . . ? C11 C10 C15 C14 -0.5(7) . . . . ? C3 C10 C15 C14 -179.8(4) . . . . ? C9 C4 C16 C17 59.7(6) . . . . ? P2 C4 C16 C17 -124.4(4) . . . . ? C9 C4 C16 C21 -119.1(5) . . . . ? P2 C4 C16 C21 56.8(6) . . . . ? C21 C16 C17 C18 -1.9(7) . . . . ? C4 C16 C17 C18 179.3(4) . . . . ? C16 C17 C18 C19 1.9(8) . . . . ? C17 C18 C19 C20 -1.2(8) . . . . ? C18 C19 C20 C21 0.4(8) . . . . ? C19 C20 C21 C16 -0.3(8) . . . . ? C17 C16 C21 C20 1.1(7) . . . . ? C4 C16 C21 C20 179.9(4) . . . . ? C3 P1 C22 C27 -67.5(4) . . . . ? Cu1 P1 C22 C27 89.5(4) . . . . ? C3 P1 C22 C23 102.7(3) . . . . ? Cu1 P1 C22 C23 -100.3(3) . . . . ? C27 C22 C23 C24 14.3(6) . . . . ? P1 C22 C23 C24 -156.4(3) . . . . ? C27 C22 C23 C28 -163.2(4) . . . . ? P1 C22 C23 C28 26.0(5) . . . . ? C22 C23 C24 C25 -4.2(7) . . . . ? C28 C23 C24 C25 173.5(4) . . . . ? C23 C24 C25 C26 -6.7(7) . . . . ? C23 C24 C25 C32 177.5(5) . . . . ? C24 C25 C26 C27 8.0(7) . . . . ? C32 C25 C26 C27 -176.2(5) . . . . ? C25 C26 C27 C22 1.8(7) . . . . ? C25 C26 C27 C39 -173.8(5) . . . . ? C23 C22 C27 C26 -13.1(6) . . . . ? P1 C22 C27 C26 156.7(4) . . . . ? C23 C22 C27 C39 161.9(5) . . . . ? P1 C22 C27 C39 -28.2(7) . . . . ? C24 C23 C28 C30 107.8(5) . . . . ? C22 C23 C28 C30 -74.7(6) . . . . ? C24 C23 C28 C29 -128.1(4) . . . . ? C22 C23 C28 C29 49.4(6) . . . . ? C24 C23 C28 C31 -12.5(6) . . . . ? C22 C23 C28 C31 165.1(4) . . . . ? C26 C25 C32 C36 137.3(11) . . . . ? C24 C25 C32 C36 -47.1(12) . . . . ? C26 C25 C32 C35 -14.9(11) . . . . ? C24 C25 C32 C35 160.7(9) . . . . ? C26 C25 C32 C37 -101.0(11) . . . . ? C24 C25 C32 C37 74.6(11) . . . . ? C26 C25 C32 C34 -143.0(8) . . . . ? C24 C25 C32 C34 32.5(10) . . . . ? C26 C25 C32 C38 22.4(11) . . . . ? C24 C25 C32 C38 -162.0(9) . . . . ? C26 C25 C32 C33 106.7(9) . . . . ? C24 C25 C32 C33 -77.7(9) . . . . ? C26 C27 C39 C42 174.2(6) . . . . ? C22 C27 C39 C42 -0.9(9) . . . . ? C26 C27 C39 C44 14.0(11) . . . . ? C22 C27 C39 C44 -161.1(10) . . . . ? C26 C27 C39 C43 -132.6(9) . . . . ? C22 C27 C39 C43 52.3(10) . . . . ? C26 C27 C39 C41 46.1(7) . . . . ? C22 C27 C39 C41 -129.0(6) . . . . ? C26 C27 C39 C40 -65.3(6) . . . . ? C22 C27 C39 C40 119.6(6) . . . . ? C26 C27 C39 C45 122.3(7) . . . . ? C22 C27 C39 C45 -52.8(8) . . . . ? C4 P2 C46 C51 71.6(4) . . . . ? Cu1 P2 C46 C51 -69.9(4) . . . . ? C4 P2 C46 C47 -99.0(3) . . . . ? Cu1 P2 C46 C47 119.6(3) . . . . ? C51 C46 C47 C48 -14.3(6) . . . . ? P2 C46 C47 C48 156.4(3) . . . . ? C51 C46 C47 C63 163.2(4) . . . . ? P2 C46 C47 C63 -26.0(5) . . . . ? C46 C47 C48 C49 2.2(6) . . . . ? C63 C47 C48 C49 -175.5(4) . . . . ? C47 C48 C49 C50 8.7(7) . . . . ? C47 C48 C49 C56 -174.3(4) . . . . ? C48 C49 C50 C51 -7.7(7) . . . . ? C56 C49 C50 C51 175.4(4) . . . . ? C49 C50 C51 C46 -4.0(6) . . . . ? C49 C50 C51 C52 168.8(4) . . . . ? C47 C46 C51 C50 15.2(6) . . . . ? P2 C46 C51 C50 -155.1(3) . . . . ? C47 C46 C51 C52 -157.3(4) . . . . ? P2 C46 C51 C52 32.4(6) . . . . ? C50 C51 C52 C54 -120.9(4) . . . . ? C46 C51 C52 C54 51.5(5) . . . . ? C50 C51 C52 C55 -3.7(6) . . . . ? C46 C51 C52 C55 168.6(4) . . . . ? C50 C51 C52 C53 116.8(4) . . . . ? C46 C51 C52 C53 -70.8(5) . . . . ? C48 C49 C56 C58 -72.6(11) . . . . ? C50 C49 C56 C58 104.3(11) . . . . ? C48 C49 C56 C62 -170.7(8) . . . . ? C50 C49 C56 C62 6.1(9) . . . . ? C48 C49 C56 C57 66.4(8) . . . . ? C50 C49 C56 C57 -116.8(8) . . . . ? C48 C49 C56 C59 165.5(9) . . . . ? C50 C49 C56 C59 -17.6(10) . . . . ? C48 C49 C56 C61 -52.4(7) . . . . ? C50 C49 C56 C61 124.5(6) . . . . ? C48 C49 C56 C60 48.5(9) . . . . ? C50 C49 C56 C60 -134.7(8) . . . . ? C48 C47 C63 C64 -105.7(5) . . . . ? C46 C47 C63 C64 76.8(5) . . . . ? C48 C47 C63 C65 130.6(4) . . . . ? C46 C47 C63 C65 -46.9(6) . . . . ? C48 C47 C63 C66 14.6(6) . . . . ? C46 C47 C63 C66 -162.9(4) . . . . ? C76 C71 C72 C73 -3.8(9) . . . . ? C77 C71 C72 C73 177.8(6) . . . . ? C71 C72 C73 C74 2.1(10) . . . . ? C72 C73 C74 C75 1.3(11) . . . . ? C73 C74 C75 C76 -2.8(11) . . . . ? C74 C75 C76 C71 0.9(11) . . . . ? C72 C71 C76 C75 2.3(10) . . . . ? C77 C71 C76 C75 -179.3(6) . . . . ? C69 C68 C67 C70A 175.2 . . . . ? C69 C68 C67 C69 -1.7(4) . . . 2_655 ? C67 C68 C69 C70 176.4 . . . . ? C67 C68 C69 C67 1.7(4) . . . 2_655 ? _diffrn_measured_fraction_theta_max 0.824 _diffrn_reflns_theta_full 31.59 _diffrn_measured_fraction_theta_full 0.824 _refine_diff_density_max 1.745 _refine_diff_density_min -1.246 _refine_diff_density_rms 0.109 # Attachment '3b.CIF' data_3b _database_code_depnum_ccdc_archive 'CCDC 812264' #TrackingRef '3b.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C57 H73 Cl2 Cu F6 N O P2 Sb' _chemical_formula_weight 1220.29 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' 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sb Sb -0.5866 1.5461 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z' '-x, -y, -z' 'x-1/2, -y-1/2, z' _cell_length_a 18.330(7) _cell_length_b 18.284(6) _cell_length_c 18.673(7) _cell_angle_alpha 90.00 _cell_angle_beta 110.230(4) _cell_angle_gamma 90.00 _cell_volume 5872(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.380 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2512 _exptl_absorpt_coefficient_mu 1.024 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.9506 _exptl_absorpt_correction_T_max 0.9798 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ' 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 47440 _diffrn_reflns_av_R_equivalents 0.0557 _diffrn_reflns_av_sigmaI/netI 0.0570 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.14 _diffrn_reflns_theta_max 27.48 _reflns_number_total 13047 _reflns_number_gt 11612 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rigaku AFC10/Saturn 70 CCD' _computing_cell_refinement 'Rigaku AFC10/Saturn 70 CCD' _computing_data_reduction 'Rigaku AFC10/Saturn 70 CCD' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for windows' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.1000P)^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 13047 _refine_ls_number_parameters 661 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1099 _refine_ls_R_factor_gt 0.1005 _refine_ls_wR_factor_ref 0.3193 _refine_ls_wR_factor_gt 0.3153 _refine_ls_goodness_of_fit_ref 1.992 _refine_ls_restrained_S_all 1.992 _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 -0.24077(4) 0.18757(4) -0.27452(4) 0.0307(2) Uani 1 1 d . A . P1 P -0.32455(9) 0.22348(8) -0.39429(9) 0.0270(3) Uani 1 1 d . . . P2 P -0.12159(9) 0.22738(9) -0.19140(9) 0.0301(4) Uani 1 1 d . . . N1 N -0.1753(3) 0.1565(3) -0.3359(3) 0.0290(11) Uani 1 1 d . . . C1 C -0.2948(4) 0.1286(5) -0.2290(4) 0.0503(19) Uani 1 1 d . . . O1 O -0.3306(5) 0.0956(5) -0.2028(4) 0.093(3) Uani 1 1 d . A 1 C2 C -0.2077(4) 0.1489(3) -0.4131(4) 0.0289(12) Uani 1 1 d . . . C3 C -0.1630(4) 0.1312(3) -0.4586(4) 0.0333(14) Uani 1 1 d . . . H1 H -0.1866 0.1255 -0.5122 0.040 Uiso 1 1 calc R . . C4 C -0.0840(4) 0.1223(4) -0.4233(4) 0.0376(15) Uani 1 1 d . . . H2 H -0.0529 0.1080 -0.4525 0.045 Uiso 1 1 calc R . . C5 C -0.0502(4) 0.1337(4) -0.3468(4) 0.0354(14) Uani 1 1 d . . . H3 H 0.0045 0.1286 -0.3230 0.042 Uiso 1 1 calc R . . C6 C -0.0956(4) 0.1529(3) -0.3037(4) 0.0305(13) Uani 1 1 d . . . C7 C -0.2898(4) 0.1708(3) -0.4483(4) 0.0302(13) Uani 1 1 d . . . C8 C -0.3302(4) 0.1484(3) -0.5287(4) 0.0314(13) Uani 1 1 d . . . C9 C -0.3417(4) 0.0732(4) -0.5456(4) 0.0383(15) Uani 1 1 d . . . H4 H -0.3226 0.0382 -0.5059 0.046 Uiso 1 1 calc R . . C10 C -0.3802(5) 0.0502(5) -0.6188(4) 0.0495(19) Uani 1 1 d . . . H5 H -0.3886 -0.0006 -0.6294 0.059 Uiso 1 1 calc R . . C11 C -0.4068(6) 0.1006(5) -0.6772(4) 0.058(2) Uani 1 1 d . . . H6 H -0.4340 0.0845 -0.7278 0.070 Uiso 1 1 calc R . . C12 C -0.3940(6) 0.1740(5) -0.6622(4) 0.060(2) Uani 1 1 d . . . H7 H -0.4109 0.2084 -0.7028 0.072 Uiso 1 1 calc R . . C13 C -0.3567(5) 0.1980(4) -0.5883(4) 0.0462(18) Uani 1 1 d . . . H8 H -0.3492 0.2489 -0.5782 0.055 Uiso 1 1 calc R . . C14 C -0.0629(4) 0.1777(4) -0.2239(4) 0.0349(14) Uani 1 1 d . . . C15 C 0.0216(4) 0.1613(4) -0.1836(4) 0.0372(15) Uani 1 1 d . . . C16 C 0.0758(4) 0.2174(5) -0.1602(4) 0.0479(18) Uani 1 1 d . . . H9 H 0.0591 0.2668 -0.1695 0.057 Uiso 1 1 calc R . . C17 C 0.1531(5) 0.2023(6) -0.1237(5) 0.059(2) Uani 1 1 d . . . H10 H 0.1900 0.2408 -0.1079 0.070 Uiso 1 1 calc R . . C18 C 0.1769(5) 0.1290(8) -0.1100(6) 0.079(4) Uani 1 1 d . . . H11 H 0.2300 0.1184 -0.0827 0.095 Uiso 1 1 calc R . . C19 C 0.1241(6) 0.0715(6) -0.1356(6) 0.070(3) Uani 1 1 d . . . H12 H 0.1409 0.0220 -0.1282 0.084 Uiso 1 1 calc R . . C20 C 0.0467(5) 0.0890(5) -0.1721(5) 0.054(2) Uani 1 1 d . . . H13 H 0.0097 0.0507 -0.1898 0.064 Uiso 1 1 calc R . . C21 C -0.4153(3) 0.2627(3) -0.4564(3) 0.0257(12) Uani 1 1 d . . . C22 C -0.4844(4) 0.2239(3) -0.4947(4) 0.0321(13) Uani 1 1 d . . . C23 C -0.5367(4) 0.2528(4) -0.5614(4) 0.0348(14) Uani 1 1 d . . . H14 H -0.5831 0.2266 -0.5872 0.042 Uiso 1 1 calc R . . C24 C -0.5237(4) 0.3189(4) -0.5919(4) 0.0347(14) Uani 1 1 d . B . C25 C -0.4612(3) 0.3607(4) -0.5494(3) 0.0298(13) Uani 1 1 d . . . H15 H -0.4546 0.4081 -0.5672 0.036 Uiso 1 1 calc R . . C26 C -0.4072(3) 0.3357(3) -0.4808(4) 0.0289(12) Uani 1 1 d . . . C27 C -0.5112(4) 0.1529(4) -0.4650(4) 0.0360(14) Uani 1 1 d . . . C28 C -0.5368(5) 0.0945(4) -0.5271(5) 0.056(2) Uani 1 1 d . . . H18 H -0.4929 0.0814 -0.5431 0.084 Uiso 1 1 calc R . . H19 H -0.5794 0.1135 -0.5710 0.084 Uiso 1 1 calc R . . H20 H -0.5545 0.0510 -0.5071 0.084 Uiso 1 1 calc R . . C29 C -0.5830(5) 0.1742(4) -0.4423(6) 0.054(2) Uani 1 1 d . . . H21 H -0.6071 0.1298 -0.4314 0.080 Uiso 1 1 calc R . . H22 H -0.6208 0.2008 -0.4845 0.080 Uiso 1 1 calc R . . H23 H -0.5659 0.2053 -0.3968 0.080 Uiso 1 1 calc R . . C30 C -0.4522(4) 0.1188(5) -0.3956(5) 0.053(2) Uani 1 1 d . . . H24 H -0.4771 0.0801 -0.3759 0.079 Uiso 1 1 calc R . . H25 H -0.4315 0.1562 -0.3562 0.079 Uiso 1 1 calc R . . H26 H -0.4097 0.0980 -0.4095 0.079 Uiso 1 1 calc R . . C31 C -0.5796(4) 0.3439(5) -0.6712(4) 0.0461(18) Uani 1 1 d . . . C32 C -0.5570(6) 0.4170(6) -0.6955(6) 0.074(3) Uani 1 1 d . B . H54 H -0.5033 0.4147 -0.6945 0.111 Uiso 1 1 calc R . . H55 H -0.5614 0.4551 -0.6602 0.111 Uiso 1 1 calc R . . H56 H -0.5918 0.4285 -0.7473 0.111 Uiso 1 1 calc R . . C33A C -0.602(3) 0.272(2) -0.7261(17) 0.066(9) Uiso 0.38(6) 1 d P B 1 H57 H -0.6570 0.2729 -0.7568 0.099 Uiso 0.38(6) 1 calc PR B 1 H58 H -0.5900 0.2276 -0.6945 0.099 Uiso 0.38(6) 1 calc PR B 1 H59 H -0.5708 0.2718 -0.7599 0.099 Uiso 0.38(6) 1 calc PR B 1 C34A C -0.656(2) 0.365(2) -0.6678(19) 0.056(9) Uiso 0.38(6) 1 d P B 1 H60 H -0.6912 0.3764 -0.7194 0.083 Uiso 0.38(6) 1 calc PR B 1 H61 H -0.6495 0.4081 -0.6352 0.083 Uiso 0.38(6) 1 calc PR B 1 H62 H -0.6768 0.3244 -0.6468 0.083 Uiso 0.38(6) 1 calc PR B 1 C35 C -0.3423(4) 0.3899(3) -0.4347(4) 0.0337(14) Uani 1 1 d . . . C36 C -0.2625(4) 0.3737(4) -0.4371(5) 0.0450(17) Uani 1 1 d . . . H27 H -0.2297 0.4173 -0.4215 0.067 Uiso 1 1 calc R . . H28 H -0.2668 0.3600 -0.4892 0.067 Uiso 1 1 calc R . . H29 H -0.2391 0.3333 -0.4022 0.067 Uiso 1 1 calc R . . C37 C -0.3407(4) 0.3934(4) -0.3514(4) 0.0408(16) Uani 1 1 d . . . H30 H -0.3291 0.3448 -0.3282 0.061 Uiso 1 1 calc R . . H31 H -0.3915 0.4097 -0.3510 0.061 Uiso 1 1 calc R . . H32 H -0.3006 0.4280 -0.3224 0.061 Uiso 1 1 calc R . . C38 C -0.3606(5) 0.4680(4) -0.4665(5) 0.0499(19) Uani 1 1 d . . . H33 H -0.3238 0.5023 -0.4322 0.075 Uiso 1 1 calc R . . H34 H -0.4137 0.4811 -0.4703 0.075 Uiso 1 1 calc R . . H35 H -0.3560 0.4704 -0.5172 0.075 Uiso 1 1 calc R . . C39 C -0.0617(4) 0.2604(4) -0.0970(4) 0.0352(14) Uani 1 1 d . . . C40 C -0.0276(4) 0.3303(3) -0.0929(3) 0.0303(13) Uani 1 1 d . C . C41 C 0.0397(4) 0.3446(3) -0.0309(3) 0.0308(13) Uani 1 1 d . . . H16 H 0.0636 0.3912 -0.0275 0.037 Uiso 1 1 calc R . . C42 C 0.0734(4) 0.2937(4) 0.0260(4) 0.0362(14) Uani 1 1 d . . . C43 C 0.0312(4) 0.2292(4) 0.0248(4) 0.0352(14) Uani 1 1 d . . . H17 H 0.0506 0.1961 0.0662 0.042 Uiso 1 1 calc R . . C44 C -0.0361(4) 0.2117(4) -0.0327(4) 0.0328(13) Uani 1 1 d . . . C45 C -0.0636(4) 0.3937(4) -0.1490(4) 0.0366(15) Uani 1 1 d . . . C46A C -0.0556(10) 0.3847(7) -0.2293(8) 0.047(4) Uiso 0.68(4) 1 d P C 1 H63 H -0.0853 0.3418 -0.2550 0.070 Uiso 0.68(4) 1 calc PR C 1 H64 H -0.0007 0.3782 -0.2232 0.070 Uiso 0.68(4) 1 calc PR C 1 H65 H -0.0759 0.4285 -0.2600 0.070 Uiso 0.68(4) 1 calc PR C 1 C47A C -0.1536(9) 0.3978(10) -0.1533(12) 0.057(4) Uiso 0.68(4) 1 d P C 1 H66 H -0.1806 0.4365 -0.1888 0.086 Uiso 0.68(4) 1 calc PR C 1 H67 H -0.1553 0.4085 -0.1025 0.086 Uiso 0.68(4) 1 calc PR C 1 H68 H -0.1791 0.3508 -0.1711 0.086 Uiso 0.68(4) 1 calc PR C 1 C48A C -0.0217(10) 0.4666(8) -0.1236(10) 0.053(4) Uiso 0.68(4) 1 d P C 1 H69 H -0.0445 0.5037 -0.1628 0.079 Uiso 0.68(4) 1 calc PR C 1 H70 H 0.0336 0.4608 -0.1162 0.079 Uiso 0.68(4) 1 calc PR C 1 H71 H -0.0273 0.4819 -0.0755 0.079 Uiso 0.68(4) 1 calc PR C 1 C49 C 0.1507(4) 0.3070(4) 0.0905(4) 0.0429(17) Uani 1 1 d . . . C50 C 0.2065(5) 0.2420(5) 0.0953(5) 0.057(2) Uani 1 1 d . . . H36 H 0.1808 0.1962 0.1000 0.085 Uiso 1 1 calc R . . H37 H 0.2538 0.2482 0.1400 0.085 Uiso 1 1 calc R . . H38 H 0.2201 0.2407 0.0490 0.085 Uiso 1 1 calc R . . C51 C 0.1343(5) 0.3105(6) 0.1664(5) 0.063(3) Uani 1 1 d . . . H39 H 0.1026 0.3537 0.1662 0.095 Uiso 1 1 calc R . . H40 H 0.1836 0.3137 0.2092 0.095 Uiso 1 1 calc R . . H41 H 0.1064 0.2663 0.1717 0.095 Uiso 1 1 calc R . . C52 C 0.1904(5) 0.3778(5) 0.0797(5) 0.058(2) Uani 1 1 d . . . H42 H 0.2020 0.3749 0.0324 0.087 Uiso 1 1 calc R . . H43 H 0.2388 0.3845 0.1230 0.087 Uiso 1 1 calc R . . H44 H 0.1557 0.4193 0.0769 0.087 Uiso 1 1 calc R . . C53 C -0.0833(4) 0.1446(4) -0.0207(4) 0.0444(17) Uani 1 1 d . . . C54 C -0.0791(7) 0.0777(5) -0.0701(6) 0.075(3) Uani 1 1 d . . . H45 H -0.0246 0.0642 -0.0593 0.113 Uiso 1 1 calc R . . H46 H -0.1031 0.0903 -0.1243 0.113 Uiso 1 1 calc R . . H47 H -0.1071 0.0365 -0.0581 0.113 Uiso 1 1 calc R . . C55 C -0.1686(5) 0.1673(6) -0.0449(5) 0.056(2) Uani 1 1 d . . . H48 H -0.2005 0.1245 -0.0439 0.084 Uiso 1 1 calc R . . H49 H -0.1853 0.1874 -0.0967 0.084 Uiso 1 1 calc R . . H50 H -0.1747 0.2045 -0.0096 0.084 Uiso 1 1 calc R . . C56 C -0.0560(6) 0.1218(6) 0.0622(5) 0.065(3) Uani 1 1 d . . . H51 H 0.0000 0.1119 0.0798 0.098 Uiso 1 1 calc R . . H52 H -0.0837 0.0775 0.0676 0.098 Uiso 1 1 calc R . . H53 H -0.0664 0.1612 0.0928 0.098 Uiso 1 1 calc R . . Sb1 Sb 0.20627(3) 0.07250(3) 0.29430(3) 0.0483(2) Uani 1 1 d . . . F1A F 0.1436(11) 0.1198(12) 0.2063(11) 0.119(6) Uiso 0.487(12) 1 d P D 1 F2A F 0.2823(8) 0.0034(8) 0.3471(8) 0.084(4) Uiso 0.487(12) 1 d P D 1 F3A F 0.1377(14) 0.0304(15) 0.3458(15) 0.163(9) Uiso 0.487(12) 1 d P D 1 F4A F 0.1581(17) 0.1366(19) 0.3397(18) 0.214(13) Uiso 0.487(12) 1 d P D 1 F5A F 0.1639(13) -0.0084(12) 0.2316(11) 0.128(7) Uiso 0.487(12) 1 d P D 1 F6A F 0.2812(10) 0.1467(11) 0.3115(11) 0.118(6) Uiso 0.487(12) 1 d P D 1 C57 C 0.3457(9) 0.0880(7) 0.1298(8) 0.097(4) Uani 1 1 d . . . H57A H 0.3041 0.1176 0.1379 0.117 Uiso 1 1 calc R E 1 H57B H 0.3753 0.0637 0.1787 0.117 Uiso 1 1 calc R E 1 Cl1A Cl 0.3018(8) 0.0178(7) 0.0566(8) 0.061(3) Uiso 0.33 1 d P F 1 Cl2A Cl 0.4113(8) 0.1483(6) 0.1011(10) 0.061(3) Uiso 0.33 1 d P F 1 C33B C -0.5774(10) 0.2910(9) -0.7309(7) 0.041(5) Uiso 0.62(6) 1 d P B 2 H72 H -0.5913 0.2422 -0.7181 0.061 Uiso 0.62(6) 1 calc PR B 2 H73 H -0.5249 0.2897 -0.7334 0.061 Uiso 0.62(6) 1 calc PR B 2 H74 H -0.6146 0.3061 -0.7804 0.061 Uiso 0.62(6) 1 calc PR B 2 C34B C -0.6635(10) 0.3471(13) -0.6686(10) 0.044(4) Uiso 0.62(6) 1 d P B 2 H75 H -0.6651 0.3821 -0.6294 0.066 Uiso 0.62(6) 1 calc PR B 2 H76 H -0.6785 0.2985 -0.6563 0.066 Uiso 0.62(6) 1 calc PR B 2 H77 H -0.6997 0.3627 -0.7184 0.066 Uiso 0.62(6) 1 calc PR B 2 C46B C -0.021(3) 0.398(2) -0.210(2) 0.070(11) Uiso 0.32(4) 1 d P C 2 H78 H -0.0285 0.3515 -0.2389 0.105 Uiso 0.32(4) 1 calc PR C 2 H79 H 0.0351 0.4056 -0.1842 0.105 Uiso 0.32(4) 1 calc PR C 2 H80 H -0.0423 0.4380 -0.2459 0.105 Uiso 0.32(4) 1 calc PR C 2 C47B C -0.1478(14) 0.4013(13) -0.1739(17) 0.029(6) Uiso 0.32(4) 1 d P C 2 H81 H -0.1642 0.4027 -0.1292 0.044 Uiso 0.32(4) 1 calc PR C 2 H82 H -0.1724 0.3596 -0.2062 0.044 Uiso 0.32(4) 1 calc PR C 2 H83 H -0.1635 0.4467 -0.2031 0.044 Uiso 0.32(4) 1 calc PR C 2 C48B C -0.0399(13) 0.4708(9) -0.1077(12) 0.018(5) Uiso 0.32(4) 1 d P C 2 H84 H -0.0598 0.5102 -0.1450 0.028 Uiso 0.32(4) 1 calc PR C 2 H85 H 0.0169 0.4743 -0.0855 0.028 Uiso 0.32(4) 1 calc PR C 2 H86 H -0.0622 0.4754 -0.0672 0.028 Uiso 0.32(4) 1 calc PR C 2 F4B F 0.2777(13) 0.1064(15) 0.2549(14) 0.162(9) Uiso 0.513(12) 1 d P D 2 F3B F 0.2619(12) 0.0288(12) 0.3830(12) 0.136(7) Uiso 0.513(12) 1 d P D 2 F2B F 0.1248(9) 0.0076(9) 0.2700(9) 0.098(5) Uiso 0.513(12) 1 d P D 2 F1B F 0.1293(9) 0.1421(10) 0.2474(10) 0.107(5) Uiso 0.513(12) 1 d P D 2 F5B F 0.236(2) 0.006(2) 0.237(2) 0.242(15) Uiso 0.513(12) 1 d P D 2 F6B F 0.2575(12) 0.1467(12) 0.3659(12) 0.143(8) Uiso 0.513(12) 1 d P D 2 Cl1B Cl 0.3918(7) 0.1464(6) 0.0785(6) 0.079(4) Uiso 0.33 1 d P F 2 Cl2B Cl 0.2891(8) 0.0378(9) 0.0692(8) 0.108(5) Uiso 0.33 1 d P F 2 Cl1C Cl 0.4148(9) 0.1446(8) 0.1220(8) 0.089(5) Uiso 0.33 1 d P F 3 Cl2C Cl 0.3167(7) 0.0218(8) 0.0506(7) 0.073(4) Uiso 0.33 1 d P F 3 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 0.0296(5) 0.0327(4) 0.0321(4) -0.0006(3) 0.0137(3) 0.0007(3) P1 0.0265(8) 0.0238(7) 0.0300(7) -0.0029(5) 0.0087(6) 0.0020(6) P2 0.0280(8) 0.0313(8) 0.0301(8) -0.0046(6) 0.0087(6) 0.0003(6) N1 0.025(3) 0.028(2) 0.029(2) 0.0048(19) 0.002(2) -0.0016(19) C1 0.040(4) 0.065(5) 0.041(4) 0.003(4) 0.007(3) -0.006(4) O1 0.081(5) 0.117(7) 0.082(5) 0.040(5) 0.030(4) -0.036(5) C2 0.032(3) 0.021(3) 0.035(3) -0.002(2) 0.013(3) 0.002(2) C3 0.038(4) 0.030(3) 0.035(3) -0.006(2) 0.017(3) -0.002(3) C4 0.040(4) 0.035(3) 0.046(4) -0.010(3) 0.025(3) 0.002(3) C5 0.030(3) 0.030(3) 0.050(4) 0.000(3) 0.020(3) 0.002(2) C6 0.033(3) 0.022(3) 0.040(3) -0.002(2) 0.018(3) -0.002(2) C7 0.031(3) 0.021(3) 0.038(3) 0.002(2) 0.012(3) -0.002(2) C8 0.034(3) 0.031(3) 0.034(3) -0.002(2) 0.017(3) 0.006(2) C9 0.038(4) 0.036(3) 0.037(3) -0.002(3) 0.008(3) 0.003(3) C10 0.047(4) 0.048(4) 0.046(4) -0.014(3) 0.007(3) 0.000(3) C11 0.072(6) 0.064(5) 0.035(4) -0.008(4) 0.013(4) 0.015(4) C12 0.085(6) 0.062(5) 0.034(4) 0.006(3) 0.023(4) 0.032(5) C13 0.065(5) 0.038(4) 0.037(3) -0.004(3) 0.020(3) 0.016(3) C14 0.033(4) 0.035(3) 0.037(3) 0.004(3) 0.013(3) -0.002(3) C15 0.034(4) 0.043(4) 0.036(3) -0.001(3) 0.014(3) 0.002(3) C16 0.035(4) 0.063(5) 0.047(4) -0.004(4) 0.016(3) 0.000(3) C17 0.034(4) 0.089(7) 0.052(5) -0.009(5) 0.014(4) -0.004(4) C18 0.032(5) 0.142(12) 0.057(5) 0.019(6) 0.009(4) 0.014(6) C19 0.055(6) 0.084(7) 0.073(6) 0.023(5) 0.027(5) 0.035(5) C20 0.040(4) 0.056(5) 0.068(5) 0.008(4) 0.023(4) 0.010(4) C21 0.029(3) 0.019(3) 0.030(3) -0.002(2) 0.011(2) -0.001(2) C22 0.032(3) 0.025(3) 0.040(3) -0.005(2) 0.014(3) -0.001(2) C23 0.034(4) 0.033(3) 0.036(3) -0.006(3) 0.010(3) -0.003(3) C24 0.033(4) 0.043(4) 0.030(3) 0.001(3) 0.013(3) 0.007(3) C25 0.029(3) 0.031(3) 0.033(3) 0.003(2) 0.016(3) 0.003(2) C26 0.028(3) 0.023(3) 0.038(3) -0.002(2) 0.013(3) 0.002(2) C27 0.034(3) 0.027(3) 0.050(4) 0.001(3) 0.017(3) -0.004(2) C28 0.049(5) 0.031(4) 0.080(6) -0.013(4) 0.012(4) -0.008(3) C29 0.050(5) 0.034(4) 0.091(6) 0.016(4) 0.041(5) 0.003(3) C30 0.038(4) 0.049(5) 0.071(5) 0.025(4) 0.019(4) -0.002(3) C31 0.044(4) 0.054(5) 0.033(3) 0.003(3) 0.004(3) 0.009(3) C32 0.071(6) 0.073(7) 0.057(5) 0.031(5) -0.003(5) 0.000(5) C35 0.028(3) 0.026(3) 0.043(3) -0.002(2) 0.008(3) -0.005(2) C36 0.034(4) 0.036(4) 0.071(5) -0.008(3) 0.027(4) -0.007(3) C37 0.042(4) 0.034(3) 0.045(4) -0.010(3) 0.014(3) -0.009(3) C38 0.053(5) 0.029(4) 0.063(5) -0.005(3) 0.015(4) -0.011(3) C39 0.038(4) 0.035(3) 0.032(3) -0.005(3) 0.013(3) 0.000(3) C40 0.031(3) 0.030(3) 0.030(3) 0.002(2) 0.012(3) 0.004(2) C41 0.030(3) 0.029(3) 0.033(3) -0.002(2) 0.010(3) -0.001(2) C42 0.035(4) 0.043(4) 0.030(3) -0.001(3) 0.011(3) -0.002(3) C43 0.036(4) 0.040(4) 0.030(3) 0.010(3) 0.011(3) 0.006(3) C44 0.037(4) 0.029(3) 0.037(3) 0.004(2) 0.020(3) -0.001(3) C45 0.039(4) 0.033(3) 0.032(3) 0.003(3) 0.007(3) 0.003(3) C49 0.033(4) 0.050(4) 0.038(4) 0.003(3) 0.004(3) -0.001(3) C50 0.037(4) 0.067(6) 0.058(5) 0.009(4) 0.006(4) 0.005(4) C51 0.053(5) 0.086(7) 0.042(4) -0.008(4) 0.006(4) -0.016(5) C52 0.036(4) 0.074(6) 0.051(4) 0.005(4) 0.001(4) -0.016(4) C53 0.043(4) 0.044(4) 0.052(4) 0.005(3) 0.023(3) -0.009(3) C54 0.116(9) 0.039(5) 0.086(7) -0.002(4) 0.055(7) -0.012(5) C55 0.049(5) 0.074(6) 0.054(5) 0.004(4) 0.029(4) -0.013(4) C56 0.065(6) 0.067(6) 0.064(5) 0.018(5) 0.022(5) -0.014(5) Sb1 0.0581(4) 0.0371(3) 0.0550(4) 0.0023(2) 0.0263(3) -0.0004(2) C57 0.128(11) 0.069(8) 0.121(11) -0.001(7) 0.076(9) 0.026(7) _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 C1 1.857(9) . ? Cu1 N1 2.007(6) . ? Cu1 P2 2.3164(18) . ? Cu1 P1 2.3272(18) . ? P1 C7 1.672(7) . ? P1 C21 1.815(6) . ? P2 C14 1.674(7) . ? P2 C39 1.827(7) . ? N1 C2 1.364(8) . ? N1 C6 1.377(8) . ? C1 O1 1.121(11) . ? C2 C3 1.406(9) . ? C2 C7 1.475(9) . ? C3 C4 1.377(10) . ? C3 H1 0.9500 . ? C4 C5 1.362(10) . ? C4 H2 0.9500 . ? C5 C6 1.389(9) . ? C5 H3 0.9500 . ? C6 C14 1.471(9) . ? C7 C8 1.483(9) . ? C8 C13 1.388(9) . ? C8 C9 1.410(9) . ? C9 C10 1.370(10) . ? C9 H4 0.9500 . ? C10 C11 1.383(12) . ? C10 H5 0.9500 . ? C11 C12 1.375(13) . ? C11 H6 0.9500 . ? C12 C13 1.383(11) . ? C12 H7 0.9500 . ? C13 H8 0.9500 . ? C14 C15 1.500(10) . ? C15 C16 1.388(11) . ? C15 C20 1.393(11) . ? C16 C17 1.371(11) . ? C16 H9 0.9500 . ? C17 C18 1.405(16) . ? C17 H10 0.9500 . ? C18 C19 1.397(16) . ? C18 H11 0.9500 . ? C19 C20 1.383(12) . ? C19 H12 0.9500 . ? C20 H13 0.9500 . ? C21 C22 1.412(8) . ? C21 C26 1.435(8) . ? C22 C23 1.388(9) . ? C22 C27 1.555(9) . ? C23 C24 1.391(10) . ? C23 H14 0.9500 . ? C24 C25 1.378(9) . ? C24 C31 1.549(9) . ? C25 C26 1.397(8) . ? C25 H15 0.9500 . ? C26 C35 1.557(8) . ? C27 C30 1.506(10) . ? C27 C28 1.527(10) . ? C27 C29 1.563(10) . ? C28 H18 0.9800 . ? C28 H19 0.9800 . ? C28 H20 0.9800 . ? C29 H21 0.9800 . ? C29 H22 0.9800 . ? C29 H23 0.9800 . ? C30 H24 0.9800 . ? C30 H25 0.9800 . ? C30 H26 0.9800 . ? C31 C34A 1.47(3) . ? C31 C33B 1.485(15) . ? C31 C32 1.514(12) . ? C31 C34B 1.56(2) . ? C31 C33A 1.63(4) . ? C32 H54 0.9800 . ? C32 H55 0.9800 . ? C32 H56 0.9800 . ? C33A H57 0.9800 . ? C33A H58 0.9800 . ? C33A H59 0.9800 . ? C34A H60 0.9800 . ? C34A H61 0.9800 . ? C34A H62 0.9800 . ? C35 C36 1.509(10) . ? C35 C38 1.539(10) . ? C35 C37 1.547(10) . ? C36 H27 0.9800 . ? C36 H28 0.9800 . ? C36 H29 0.9800 . ? C37 H30 0.9800 . ? C37 H31 0.9800 . ? C37 H32 0.9800 . ? C38 H33 0.9800 . ? C38 H34 0.9800 . ? C38 H35 0.9800 . ? C39 C40 1.413(9) . ? C39 C44 1.437(9) . ? C40 C41 1.394(8) . ? C40 C45 1.548(9) . ? C41 C42 1.387(9) . ? C41 H16 0.9500 . ? C42 C43 1.405(10) . ? C42 C49 1.529(9) . ? C43 C44 1.364(9) . ? C43 H17 0.9500 . ? C44 C53 1.563(9) . ? C45 C47B 1.46(3) . ? C45 C48A 1.529(15) . ? C45 C46A 1.564(14) . ? C45 C48B 1.594(19) . ? C45 C46B 1.60(4) . ? C45 C47A 1.626(18) . ? C46A H63 0.9800 . ? C46A H64 0.9800 . ? C46A H65 0.9800 . ? C47A H66 0.9800 . ? C47A H67 0.9800 . ? C47A H68 0.9800 . ? C48A H69 0.9800 . ? C48A H70 0.9800 . ? C48A H71 0.9800 . ? C49 C52 1.532(11) . ? C49 C51 1.548(12) . ? C49 C50 1.549(12) . ? C50 H36 0.9800 . ? C50 H37 0.9800 . ? C50 H38 0.9800 . ? C51 H39 0.9800 . ? C51 H40 0.9800 . ? C51 H41 0.9800 . ? C52 H42 0.9800 . ? C52 H43 0.9800 . ? C52 H44 0.9800 . ? C53 C56 1.510(11) . ? C53 C55 1.527(11) . ? C53 C54 1.549(12) . ? C54 H45 0.9800 . ? C54 H46 0.9800 . ? C54 H47 0.9800 . ? C55 H48 0.9800 . ? C55 H49 0.9800 . ? C55 H50 0.9800 . ? C56 H51 0.9800 . ? C56 H52 0.9800 . ? C56 H53 0.9800 . ? Sb1 F3B 1.80(2) . ? Sb1 F4B 1.82(2) . ? Sb1 F5B 1.82(4) . ? Sb1 F4A 1.84(3) . ? Sb1 F2B 1.837(15) . ? Sb1 F1A 1.861(19) . ? Sb1 F1B 1.877(17) . ? Sb1 F6A 1.88(2) . ? Sb1 F5A 1.88(2) . ? Sb1 F2A 1.887(14) . ? Sb1 F6B 1.91(2) . ? Sb1 F3A 1.98(3) . ? C57 Cl2B 1.55(2) . ? C57 Cl1C 1.68(2) . ? C57 Cl2C 1.841(19) . ? C57 Cl1B 1.826(18) . ? C57 Cl2A 1.843(19) . ? C57 Cl1A 1.845(19) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C33B H72 0.9800 . ? C33B H73 0.9800 . ? C33B H74 0.9800 . ? C34B H75 0.9800 . ? C34B H76 0.9800 . ? C34B H77 0.9800 . ? C46B H78 0.9800 . ? C46B H79 0.9800 . ? C46B H80 0.9800 . ? C47B H81 0.9800 . ? C47B H82 0.9800 . ? C47B H83 0.9800 . ? C48B H84 0.9800 . ? C48B H85 0.9800 . ? C48B H86 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Cu1 N1 128.0(3) . . ? C1 Cu1 P2 113.9(2) . . ? N1 Cu1 P2 81.96(15) . . ? C1 Cu1 P1 108.9(2) . . ? N1 Cu1 P1 81.78(14) . . ? P2 Cu1 P1 135.33(7) . . ? C7 P1 C21 107.3(3) . . ? C7 P1 Cu1 98.9(2) . . ? C21 P1 Cu1 151.7(2) . . ? C14 P2 C39 106.4(3) . . ? C14 P2 Cu1 99.3(2) . . ? C39 P2 Cu1 149.7(2) . . ? C2 N1 C6 117.7(6) . . ? C2 N1 Cu1 120.4(4) . . ? C6 N1 Cu1 121.2(4) . . ? O1 C1 Cu1 176.3(9) . . ? N1 C2 C3 122.0(6) . . ? N1 C2 C7 116.6(6) . . ? C3 C2 C7 120.8(6) . . ? C4 C3 C2 118.4(6) . . ? C4 C3 H1 120.8 . . ? C2 C3 H1 120.8 . . ? C5 C4 C3 120.3(6) . . ? C5 C4 H2 119.8 . . ? C3 C4 H2 119.8 . . ? C4 C5 C6 120.1(6) . . ? C4 C5 H3 120.0 . . ? C6 C5 H3 120.0 . . ? N1 C6 C5 121.1(6) . . ? N1 C6 C14 115.3(6) . . ? C5 C6 C14 123.3(6) . . ? C2 C7 C8 116.8(6) . . ? C2 C7 P1 115.5(5) . . ? C8 C7 P1 127.5(5) . . ? C13 C8 C9 118.3(6) . . ? C13 C8 C7 123.0(6) . . ? C9 C8 C7 118.7(6) . . ? C10 C9 C8 120.6(7) . . ? C10 C9 H4 119.7 . . ? C8 C9 H4 119.7 . . ? C9 C10 C11 120.1(8) . . ? C9 C10 H5 120.0 . . ? C11 C10 H5 120.0 . . ? C12 C11 C10 120.1(7) . . ? C12 C11 H6 119.9 . . ? C10 C11 H6 119.9 . . ? C11 C12 C13 120.3(8) . . ? C11 C12 H7 119.9 . . ? C13 C12 H7 119.9 . . ? C12 C13 C8 120.6(7) . . ? C12 C13 H8 119.7 . . ? C8 C13 H8 119.7 . . ? C6 C14 C15 115.8(6) . . ? C6 C14 P2 116.5(5) . . ? C15 C14 P2 127.5(5) . . ? C16 C15 C20 119.4(7) . . ? C16 C15 C14 120.8(7) . . ? C20 C15 C14 119.7(7) . . ? C17 C16 C15 120.8(9) . . ? C17 C16 H9 119.6 . . ? C15 C16 H9 119.6 . . ? C16 C17 C18 119.0(9) . . ? C16 C17 H10 120.5 . . ? C18 C17 H10 120.5 . . ? C19 C18 C17 121.4(8) . . ? C19 C18 H11 119.3 . . ? C17 C18 H11 119.3 . . ? C20 C19 C18 117.7(10) . . ? C20 C19 H12 121.1 . . ? C18 C19 H12 121.1 . . ? C19 C20 C15 121.6(9) . . ? C19 C20 H13 119.2 . . ? C15 C20 H13 119.2 . . ? C22 C21 C26 118.8(5) . . ? C22 C21 P1 126.0(4) . . ? C26 C21 P1 113.4(4) . . ? C23 C22 C21 118.8(6) . . ? C23 C22 C27 115.6(6) . . ? C21 C22 C27 125.3(6) . . ? C22 C23 C24 122.4(6) . . ? C22 C23 H14 118.8 . . ? C24 C23 H14 118.8 . . ? C25 C24 C23 118.1(6) . . ? C25 C24 C31 122.1(6) . . ? C23 C24 C31 119.8(6) . . ? C24 C25 C26 122.1(6) . . ? C24 C25 H15 118.9 . . ? C26 C25 H15 118.9 . . ? C25 C26 C21 118.4(5) . . ? C25 C26 C35 117.5(5) . . ? C21 C26 C35 124.0(5) . . ? C30 C27 C28 107.7(7) . . ? C30 C27 C22 115.5(6) . . ? C28 C27 C22 111.4(6) . . ? C30 C27 C29 106.9(6) . . ? C28 C27 C29 108.3(6) . . ? C22 C27 C29 106.8(5) . . ? C27 C28 H18 109.5 . . ? C27 C28 H19 109.5 . . ? H18 C28 H19 109.5 . . ? C27 C28 H20 109.5 . . ? H18 C28 H20 109.5 . . ? H19 C28 H20 109.5 . . ? C27 C29 H21 109.5 . . ? C27 C29 H22 109.5 . . ? H21 C29 H22 109.5 . . ? C27 C29 H23 109.5 . . ? H21 C29 H23 109.5 . . ? H22 C29 H23 109.5 . . ? C27 C30 H24 109.5 . . ? C27 C30 H25 109.5 . . ? H24 C30 H25 109.5 . . ? C27 C30 H26 109.5 . . ? H24 C30 H26 109.5 . . ? H25 C30 H26 109.5 . . ? C34A C31 C33B 118.4(15) . . ? C34A C31 C32 98.2(19) . . ? C33B C31 C32 105.7(10) . . ? C34A C31 C24 111.1(14) . . ? C33B C31 C24 110.2(7) . . ? C32 C31 C24 112.7(7) . . ? C34A C31 C34B 13.1(16) . . ? C33B C31 C34B 109.4(10) . . ? C32 C31 C34B 110.5(11) . . ? C24 C31 C34B 108.3(8) . . ? C34A C31 C33A 102.0(18) . . ? C33B C31 C33A 21.3(14) . . ? C32 C31 C33A 124.0(17) . . ? C24 C31 C33A 107.5(12) . . ? C34B C31 C33A 91.1(16) . . ? C31 C32 H54 109.5 . . ? C31 C32 H55 109.5 . . ? H54 C32 H55 109.5 . . ? C31 C32 H56 109.5 . . ? H54 C32 H56 109.5 . . ? H55 C32 H56 109.5 . . ? C31 C33A H57 109.5 . . ? C31 C33A H58 109.5 . . ? C31 C33A H59 109.5 . . ? C31 C34A H60 109.5 . . ? C31 C34A H61 109.5 . . ? C31 C34A H62 109.5 . . ? C36 C35 C38 104.7(6) . . ? C36 C35 C37 110.9(6) . . ? C38 C35 C37 105.9(6) . . ? C36 C35 C26 115.0(6) . . ? C38 C35 C26 110.7(5) . . ? C37 C35 C26 109.1(5) . . ? C35 C36 H27 109.5 . . ? C35 C36 H28 109.5 . . ? H27 C36 H28 109.5 . . ? C35 C36 H29 109.5 . . ? H27 C36 H29 109.5 . . ? H28 C36 H29 109.5 . . ? C35 C37 H30 109.5 . . ? C35 C37 H31 109.5 . . ? H30 C37 H31 109.5 . . ? C35 C37 H32 109.5 . . ? H30 C37 H32 109.5 . . ? H31 C37 H32 109.5 . . ? C35 C38 H33 109.5 . . ? C35 C38 H34 109.5 . . ? H33 C38 H34 109.5 . . ? C35 C38 H35 109.5 . . ? H33 C38 H35 109.5 . . ? H34 C38 H35 109.5 . . ? C40 C39 C44 120.3(6) . . ? C40 C39 P2 117.2(5) . . ? C44 C39 P2 121.0(5) . . ? C41 C40 C39 117.5(6) . . ? C41 C40 C45 118.0(6) . . ? C39 C40 C45 124.3(6) . . ? C42 C41 C40 122.9(6) . . ? C42 C41 H16 118.6 . . ? C40 C41 H16 118.6 . . ? C41 C42 C43 117.0(6) . . ? C41 C42 C49 122.9(6) . . ? C43 C42 C49 120.0(6) . . ? C44 C43 C42 123.5(6) . . ? C44 C43 H17 118.3 . . ? C42 C43 H17 118.3 . . ? C43 C44 C39 117.3(6) . . ? C43 C44 C53 117.8(6) . . ? C39 C44 C53 124.7(6) . . ? C47B C45 C48A 112.2(12) . . ? C47B C45 C40 116.3(12) . . ? C48A C45 C40 113.1(7) . . ? C47B C45 C46A 98.2(12) . . ? C48A C45 C46A 100.7(9) . . ? C40 C45 C46A 114.2(7) . . ? C47B C45 C48B 98.7(13) . . ? C48A C45 C48B 19.1(8) . . ? C40 C45 C48B 110.7(8) . . ? C46A C45 C48B 117.2(10) . . ? C47B C45 C46B 119.7(18) . . ? C48A C45 C46B 82.3(16) . . ? C40 C45 C46B 108.5(14) . . ? C46A C45 C46B 24.0(15) . . ? C48B C45 C46B 100.9(17) . . ? C47B C45 C47A 15.1(11) . . ? C48A C45 C47A 111.5(11) . . ? C40 C45 C47A 104.8(9) . . ? C46A C45 C47A 112.7(9) . . ? C48B C45 C47A 94.9(12) . . ? C46B C45 C47A 134.8(17) . . ? C45 C46A H63 109.5 . . ? C45 C46A H64 109.5 . . ? C45 C46A H65 109.5 . . ? C45 C47A H66 109.5 . . ? C45 C47A H67 109.5 . . ? C45 C47A H68 109.5 . . ? C45 C48A H69 109.5 . . ? C45 C48A H70 109.5 . . ? C45 C48A H71 109.5 . . ? C42 C49 C52 112.6(6) . . ? C42 C49 C51 107.9(6) . . ? C52 C49 C51 109.6(7) . . ? C42 C49 C50 109.7(6) . . ? C52 C49 C50 108.8(7) . . ? C51 C49 C50 108.2(7) . . ? C49 C50 H36 109.5 . . ? C49 C50 H37 109.5 . . ? H36 C50 H37 109.5 . . ? C49 C50 H38 109.5 . . ? H36 C50 H38 109.5 . . ? H37 C50 H38 109.5 . . ? C49 C51 H39 109.5 . . ? C49 C51 H40 109.5 . . ? H39 C51 H40 109.5 . . ? C49 C51 H41 109.5 . . ? H39 C51 H41 109.5 . . ? H40 C51 H41 109.5 . . ? C49 C52 H42 109.5 . . ? C49 C52 H43 109.5 . . ? H42 C52 H43 109.5 . . ? C49 C52 H44 109.5 . . ? H42 C52 H44 109.5 . . ? H43 C52 H44 109.5 . . ? C56 C53 C55 108.8(7) . . ? C56 C53 C54 109.0(8) . . ? C55 C53 C54 107.1(8) . . ? C56 C53 C44 111.1(6) . . ? C55 C53 C44 107.7(6) . . ? C54 C53 C44 112.9(7) . . ? C53 C54 H45 109.5 . . ? C53 C54 H46 109.5 . . ? H45 C54 H46 109.5 . . ? C53 C54 H47 109.5 . . ? H45 C54 H47 109.5 . . ? H46 C54 H47 109.5 . . ? C53 C55 H48 109.5 . . ? C53 C55 H49 109.5 . . ? H48 C55 H49 109.5 . . ? C53 C55 H50 109.5 . . ? H48 C55 H50 109.5 . . ? H49 C55 H50 109.5 . . ? C53 C56 H51 109.5 . . ? C53 C56 H52 109.5 . . ? H51 C56 H52 109.5 . . ? C53 C56 H53 109.5 . . ? H51 C56 H53 109.5 . . ? H52 C56 H53 109.5 . . ? F3B Sb1 F4B 105.3(10) . . ? F3B Sb1 F5B 93.4(13) . . ? F4B Sb1 F5B 65.6(15) . . ? F3B Sb1 F4A 93.9(13) . . ? F4B Sb1 F4A 119.7(14) . . ? F5B Sb1 F4A 169.2(14) . . ? F3B Sb1 F2B 95.4(8) . . ? F4B Sb1 F2B 139.3(10) . . ? F5B Sb1 F2B 78.7(13) . . ? F4A Sb1 F2B 92.7(11) . . ? F3B Sb1 F1A 175.7(10) . . ? F4B Sb1 F1A 78.2(9) . . ? F5B Sb1 F1A 90.3(13) . . ? F4A Sb1 F1A 82.1(12) . . ? F2B Sb1 F1A 83.2(8) . . ? F3B Sb1 F1B 145.5(10) . . ? F4B Sb1 F1B 96.4(9) . . ? F5B Sb1 F1B 120.2(12) . . ? F4A Sb1 F1B 51.7(10) . . ? F2B Sb1 F1B 84.7(7) . . ? F1A Sb1 F1B 30.5(7) . . ? F3B Sb1 F6A 90.8(9) . . ? F4B Sb1 F6A 40.2(9) . . ? F5B Sb1 F6A 103.6(14) . . ? F4A Sb1 F6A 84.3(12) . . ? F2B Sb1 F6A 173.2(7) . . ? F1A Sb1 F6A 90.4(8) . . ? F1B Sb1 F6A 88.7(8) . . ? F3B Sb1 F5A 101.8(9) . . ? F4B Sb1 F5A 102.5(11) . . ? F5B Sb1 F5A 41.5(12) . . ? F4A Sb1 F5A 128.9(12) . . ? F2B Sb1 F5A 38.0(7) . . ? F1A Sb1 F5A 79.6(9) . . ? F1B Sb1 F5A 99.3(8) . . ? F6A Sb1 F5A 142.7(9) . . ? F3B Sb1 F2A 30.9(7) . . ? F4B Sb1 F2A 86.2(9) . . ? F5B Sb1 F2A 63.2(12) . . ? F4A Sb1 F2A 124.8(11) . . ? F2B Sb1 F2A 95.0(7) . . ? F1A Sb1 F2A 153.1(8) . . ? F1B Sb1 F2A 176.4(7) . . ? F6A Sb1 F2A 91.7(7) . . ? F5A Sb1 F2A 82.5(8) . . ? F3B Sb1 F6B 71.7(10) . . ? F4B Sb1 F6B 78.0(10) . . ? F5B Sb1 F6B 135.5(14) . . ? F4A Sb1 F6B 54.7(11) . . ? F2B Sb1 F6B 142.5(9) . . ? F1A Sb1 F6B 107.0(9) . . ? F1B Sb1 F6B 87.3(8) . . ? F6A Sb1 F6B 38.1(8) . . ? F5A Sb1 F6B 173.3(9) . . ? F2A Sb1 F6B 90.8(8) . . ? F3B Sb1 F3A 68.6(10) . . ? F4B Sb1 F3A 173.9(10) . . ? F5B Sb1 F3A 113.2(15) . . ? F4A Sb1 F3A 62.5(13) . . ? F2B Sb1 F3A 43.3(8) . . ? F1A Sb1 F3A 107.9(10) . . ? F1B Sb1 F3A 89.4(9) . . ? F6A Sb1 F3A 138.3(10) . . ? F5A Sb1 F3A 78.6(10) . . ? F2A Sb1 F3A 87.9(9) . . ? F6B Sb1 F3A 100.2(10) . . ? Cl2B C57 Cl1C 129.6(12) . . ? Cl2B C57 Cl2C 24.1(7) . . ? Cl1C C57 Cl2C 110.6(10) . . ? Cl2B C57 Cl1B 106.1(10) . . ? Cl1C C57 Cl1B 25.1(6) . . ? Cl2C C57 Cl1B 91.1(8) . . ? Cl2B C57 Cl2A 118.8(11) . . ? Cl1C C57 Cl2A 11.2(7) . . ? Cl2C C57 Cl2A 101.2(9) . . ? Cl1B C57 Cl2A 14.1(6) . . ? Cl2B C57 Cl1A 14.9(8) . . ? Cl1C C57 Cl1A 120.8(10) . . ? Cl2C C57 Cl1A 10.5(6) . . ? Cl1B C57 Cl1A 100.3(9) . . ? Cl2A C57 Cl1A 111.2(10) . . ? Cl2B C57 H57A 94.5 . . ? Cl1C C57 H57A 108.6 . . ? Cl2C C57 H57A 117.3 . . ? Cl1B C57 H57A 106.3 . . ? Cl2A C57 H57A 109.4 . . ? Cl1A C57 H57A 109.4 . . ? Cl2B C57 H57B 115.2 . . ? Cl1C C57 H57B 99.7 . . ? Cl2C C57 H57B 111.2 . . ? Cl1B C57 H57B 122.7 . . ? Cl2A C57 H57B 109.4 . . ? Cl1A C57 H57B 109.4 . . ? H57A C57 H57B 108.0 . . ? C31 C33B H72 109.5 . . ? C31 C33B H73 109.5 . . ? H72 C33B H73 109.5 . . ? C31 C33B H74 109.5 . . ? H72 C33B H74 109.5 . . ? H73 C33B H74 109.5 . . ? C31 C34B H75 109.5 . . ? C31 C34B H76 109.5 . . ? H75 C34B H76 109.5 . . ? C31 C34B H77 109.5 . . ? H75 C34B H77 109.5 . . ? H76 C34B H77 109.5 . . ? C45 C46B H78 109.5 . . ? C45 C46B H79 109.5 . . ? H78 C46B H79 109.5 . . ? C45 C46B H80 109.5 . . ? H78 C46B H80 109.5 . . ? H79 C46B H80 109.5 . . ? C45 C47B H81 109.5 . . ? C45 C47B H82 109.5 . . ? H81 C47B H82 109.5 . . ? C45 C47B H83 109.5 . . ? H81 C47B H83 109.5 . . ? H82 C47B H83 109.5 . . ? C45 C48B H84 109.5 . . ? C45 C48B H85 109.5 . . ? H84 C48B H85 109.5 . . ? C45 C48B H86 109.5 . . ? H84 C48B H86 109.5 . . ? H85 C48B H86 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Cu1 P1 C7 -106.6(4) . . . . ? N1 Cu1 P1 C7 20.9(3) . . . . ? P2 Cu1 P1 C7 90.6(2) . . . . ? C1 Cu1 P1 C21 51.4(5) . . . . ? N1 Cu1 P1 C21 178.9(4) . . . . ? P2 Cu1 P1 C21 -111.4(4) . . . . ? C1 Cu1 P2 C14 109.2(4) . . . . ? N1 Cu1 P2 C14 -18.9(3) . . . . ? P1 Cu1 P2 C14 -88.5(2) . . . . ? C1 Cu1 P2 C39 -38.6(6) . . . . ? N1 Cu1 P2 C39 -166.8(5) . . . . ? P1 Cu1 P2 C39 123.6(5) . . . . ? C1 Cu1 N1 C2 90.7(5) . . . . ? P2 Cu1 N1 C2 -155.2(5) . . . . ? P1 Cu1 N1 C2 -17.0(4) . . . . ? C1 Cu1 N1 C6 -99.1(5) . . . . ? P2 Cu1 N1 C6 15.0(4) . . . . ? P1 Cu1 N1 C6 153.2(5) . . . . ? N1 Cu1 C1 O1 -138(13) . . . . ? P2 Cu1 C1 O1 123(13) . . . . ? P1 Cu1 C1 O1 -43(13) . . . . ? C6 N1 C2 C3 5.9(9) . . . . ? Cu1 N1 C2 C3 176.5(5) . . . . ? C6 N1 C2 C7 -165.4(5) . . . . ? Cu1 N1 C2 C7 5.2(7) . . . . ? N1 C2 C3 C4 -0.9(9) . . . . ? C7 C2 C3 C4 170.1(6) . . . . ? C2 C3 C4 C5 -2.9(10) . . . . ? C3 C4 C5 C6 1.5(10) . . . . ? C2 N1 C6 C5 -7.4(9) . . . . ? Cu1 N1 C6 C5 -177.8(5) . . . . ? C2 N1 C6 C14 166.6(5) . . . . ? Cu1 N1 C6 C14 -3.8(7) . . . . ? C4 C5 C6 N1 3.8(10) . . . . ? C4 C5 C6 C14 -169.7(6) . . . . ? N1 C2 C7 C8 -167.3(5) . . . . ? C3 C2 C7 C8 21.3(8) . . . . ? N1 C2 C7 P1 16.9(7) . . . . ? C3 C2 C7 P1 -154.5(5) . . . . ? C21 P1 C7 C2 165.1(4) . . . . ? Cu1 P1 C7 C2 -25.6(5) . . . . ? C21 P1 C7 C8 -10.1(6) . . . . ? Cu1 P1 C7 C8 159.2(5) . . . . ? C2 C7 C8 C13 -114.4(7) . . . . ? P1 C7 C8 C13 60.8(9) . . . . ? C2 C7 C8 C9 65.0(8) . . . . ? P1 C7 C8 C9 -119.9(6) . . . . ? C13 C8 C9 C10 -2.0(11) . . . . ? C7 C8 C9 C10 178.6(7) . . . . ? C8 C9 C10 C11 1.3(12) . . . . ? C9 C10 C11 C12 0.7(14) . . . . ? C10 C11 C12 C13 -2.1(15) . . . . ? C11 C12 C13 C8 1.4(14) . . . . ? C9 C8 C13 C12 0.6(12) . . . . ? C7 C8 C13 C12 180.0(7) . . . . ? N1 C6 C14 C15 169.1(6) . . . . ? C5 C6 C14 C15 -17.0(9) . . . . ? N1 C6 C14 P2 -16.3(7) . . . . ? C5 C6 C14 P2 157.6(5) . . . . ? C39 P2 C14 C6 -172.4(5) . . . . ? Cu1 P2 C14 C6 23.9(5) . . . . ? C39 P2 C14 C15 1.5(7) . . . . ? Cu1 P2 C14 C15 -162.2(6) . . . . ? C6 C14 C15 C16 114.5(8) . . . . ? P2 C14 C15 C16 -59.4(9) . . . . ? C6 C14 C15 C20 -62.9(9) . . . . ? P2 C14 C15 C20 123.1(7) . . . . ? C20 C15 C16 C17 -2.2(12) . . . . ? C14 C15 C16 C17 -179.7(7) . . . . ? C15 C16 C17 C18 -0.2(13) . . . . ? C16 C17 C18 C19 2.8(15) . . . . ? C17 C18 C19 C20 -2.8(15) . . . . ? C18 C19 C20 C15 0.3(14) . . . . ? C16 C15 C20 C19 2.1(13) . . . . ? C14 C15 C20 C19 179.6(8) . . . . ? C7 P1 C21 C22 66.4(6) . . . . ? Cu1 P1 C21 C22 -90.7(6) . . . . ? C7 P1 C21 C26 -98.1(5) . . . . ? Cu1 P1 C21 C26 104.7(5) . . . . ? C26 C21 C22 C23 9.7(9) . . . . ? P1 C21 C22 C23 -154.1(5) . . . . ? C26 C21 C22 C27 -165.0(6) . . . . ? P1 C21 C22 C27 31.2(9) . . . . ? C21 C22 C23 C24 -0.2(10) . . . . ? C27 C22 C23 C24 175.0(6) . . . . ? C22 C23 C24 C25 -7.8(10) . . . . ? C22 C23 C24 C31 173.0(6) . . . . ? C23 C24 C25 C26 6.1(10) . . . . ? C31 C24 C25 C26 -174.7(6) . . . . ? C24 C25 C26 C21 3.3(9) . . . . ? C24 C25 C26 C35 -175.7(6) . . . . ? C22 C21 C26 C25 -11.2(9) . . . . ? P1 C21 C26 C25 154.5(5) . . . . ? C22 C21 C26 C35 167.7(6) . . . . ? P1 C21 C26 C35 -26.6(8) . . . . ? C23 C22 C27 C30 176.0(7) . . . . ? C21 C22 C27 C30 -9.1(10) . . . . ? C23 C22 C27 C28 52.8(8) . . . . ? C21 C22 C27 C28 -132.4(7) . . . . ? C23 C22 C27 C29 -65.3(8) . . . . ? C21 C22 C27 C29 109.6(8) . . . . ? C25 C24 C31 C34A -108(2) . . . . ? C23 C24 C31 C34A 71(2) . . . . ? C25 C24 C31 C33B 118.4(11) . . . . ? C23 C24 C31 C33B -62.5(12) . . . . ? C25 C24 C31 C32 0.6(11) . . . . ? C23 C24 C31 C32 179.8(8) . . . . ? C25 C24 C31 C34B -122.1(11) . . . . ? C23 C24 C31 C34B 57.1(12) . . . . ? C25 C24 C31 C33A 141(2) . . . . ? C23 C24 C31 C33A -40(2) . . . . ? C25 C26 C35 C36 -106.6(7) . . . . ? C21 C26 C35 C36 74.5(8) . . . . ? C25 C26 C35 C38 11.9(8) . . . . ? C21 C26 C35 C38 -167.0(6) . . . . ? C25 C26 C35 C37 128.1(6) . . . . ? C21 C26 C35 C37 -50.8(8) . . . . ? C14 P2 C39 C40 93.5(6) . . . . ? Cu1 P2 C39 C40 -119.6(5) . . . . ? C14 P2 C39 C44 -72.8(6) . . . . ? Cu1 P2 C39 C44 74.0(7) . . . . ? C44 C39 C40 C41 11.3(10) . . . . ? P2 C39 C40 C41 -155.2(5) . . . . ? C44 C39 C40 C45 -163.6(6) . . . . ? P2 C39 C40 C45 29.9(9) . . . . ? C39 C40 C41 C42 -0.4(10) . . . . ? C45 C40 C41 C42 174.8(6) . . . . ? C40 C41 C42 C43 -8.4(10) . . . . ? C40 C41 C42 C49 174.9(6) . . . . ? C41 C42 C43 C44 6.6(11) . . . . ? C49 C42 C43 C44 -176.6(7) . . . . ? C42 C43 C44 C39 3.8(10) . . . . ? C42 C43 C44 C53 -170.8(7) . . . . ? C40 C39 C44 C43 -12.9(10) . . . . ? P2 C39 C44 C43 153.0(5) . . . . ? C40 C39 C44 C53 161.3(7) . . . . ? P2 C39 C44 C53 -32.8(9) . . . . ? C41 C40 C45 C47B -136.6(13) . . . . ? C39 C40 C45 C47B 38.3(15) . . . . ? C41 C40 C45 C48A -4.5(13) . . . . ? C39 C40 C45 C48A 170.3(11) . . . . ? C41 C40 C45 C46A 109.9(10) . . . . ? C39 C40 C45 C46A -75.2(11) . . . . ? C41 C40 C45 C48B -25.0(14) . . . . ? C39 C40 C45 C48B 149.8(12) . . . . ? C41 C40 C45 C46B 85(2) . . . . ? C39 C40 C45 C46B -100(2) . . . . ? C41 C40 C45 C47A -126.2(9) . . . . ? C39 C40 C45 C47A 48.7(10) . . . . ? C41 C42 C49 C52 -6.6(11) . . . . ? C43 C42 C49 C52 176.7(7) . . . . ? C41 C42 C49 C51 114.5(8) . . . . ? C43 C42 C49 C51 -62.2(9) . . . . ? C41 C42 C49 C50 -127.9(8) . . . . ? C43 C42 C49 C50 55.4(9) . . . . ? C43 C44 C53 C56 14.6(10) . . . . ? C39 C44 C53 C56 -159.6(8) . . . . ? C43 C44 C53 C55 133.7(7) . . . . ? C39 C44 C53 C55 -40.5(10) . . . . ? C43 C44 C53 C54 -108.2(9) . . . . ? C39 C44 C53 C54 77.6(10) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 2.107 _refine_diff_density_min -1.335 _refine_diff_density_rms 0.151 # Attachment '4a.CIF' data_4a _database_code_depnum_ccdc_archive 'CCDC 812265' #TrackingRef '4a.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C55 H71 Cu F6 N P3' _chemical_formula_weight 1016.58 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.5918(16) _cell_length_b 13.059(2) _cell_length_c 19.304(3) _cell_angle_alpha 71.143(7) _cell_angle_beta 73.149(8) _cell_angle_gamma 76.891(8) _cell_volume 2618.0(7) _cell_formula_units_Z 2 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour purple _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.290 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 0.566 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8760 _exptl_absorpt_correction_T_max 0.9455 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71070 _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 21606 _diffrn_reflns_av_R_equivalents 0.0331 _diffrn_reflns_av_sigmaI/netI 0.0648 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 27.48 _reflns_number_total 11509 _reflns_number_gt 9502 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius CAD4 software' _computing_cell_refinement 'Nonius CAD4 software' _computing_data_reduction 'XCAD (P.McArdle, 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEX (P.McArdle, 1995)' _computing_publication_material 'SHELXL-97/2 (Sheldrick,1997)' _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^)+(0.1000P)^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 11509 _refine_ls_number_parameters 599 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0853 _refine_ls_R_factor_gt 0.0719 _refine_ls_wR_factor_ref 0.2095 _refine_ls_wR_factor_gt 0.1985 _refine_ls_goodness_of_fit_ref 1.284 _refine_ls_restrained_S_all 1.284 _refine_ls_shift/su_max 0.022 _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 0.25262(3) 0.29478(3) 0.01858(2) 0.02599(14) Uani 1 1 d . . . P1 P 0.37004(7) 0.34362(7) -0.09955(5) 0.0268(2) Uani 1 1 d . . . P2 P 0.16689(7) 0.18087(6) 0.12876(4) 0.02333(19) Uani 1 1 d . . . N1 N 0.4155(2) 0.1982(2) 0.04154(16) 0.0273(6) Uani 1 1 d . . . C1 C 0.5139(3) 0.1969(3) -0.01712(19) 0.0287(7) Uani 1 1 d . . . C2 C 0.6089(3) 0.1098(3) -0.0144(2) 0.0360(8) Uani 1 1 d . . . H1 H 0.6775 0.1107 -0.0559 0.043 Uiso 1 1 calc R . . C3 C 0.6022(3) 0.0217(3) 0.0496(2) 0.0382(8) Uani 1 1 d . . . H2 H 0.6673 -0.0375 0.0532 0.046 Uiso 1 1 calc R . . C4 C 0.4996(3) 0.0208(3) 0.1084(2) 0.0349(8) Uani 1 1 d . . . H3 H 0.4929 -0.0398 0.1521 0.042 Uiso 1 1 calc R . . C5 C 0.4064(3) 0.1092(3) 0.10296(19) 0.0296(7) Uani 1 1 d . . . C6 C 0.5124(3) 0.2873(3) -0.0877(2) 0.0301(7) Uani 1 1 d . . . C7 C 0.6323(3) 0.3128(3) -0.1388(2) 0.0307(7) Uani 1 1 d . . . C8 C 0.7251(3) 0.3191(3) -0.1084(2) 0.0361(8) Uani 1 1 d . . . H4 H 0.7117 0.3043 -0.0554 0.043 Uiso 1 1 calc R . . C9 C 0.8367(3) 0.3467(3) -0.1541(2) 0.0381(8) Uani 1 1 d . . . H5 H 0.8983 0.3518 -0.1325 0.046 Uiso 1 1 calc R . . C10 C 0.8581(3) 0.3668(3) -0.2315(2) 0.0387(8) Uani 1 1 d . . . H6 H 0.9344 0.3856 -0.2629 0.046 Uiso 1 1 calc R . . C11 C 0.7679(3) 0.3594(3) -0.2632(2) 0.0359(8) Uani 1 1 d . . . H7 H 0.7829 0.3725 -0.3162 0.043 Uiso 1 1 calc R . . C12 C 0.6554(3) 0.3328(3) -0.2172(2) 0.0338(8) Uani 1 1 d . . . H8 H 0.5938 0.3282 -0.2391 0.041 Uiso 1 1 calc R . . C13 C 0.2894(3) 0.1035(3) 0.16034(18) 0.0271(7) Uani 1 1 d . . . C14 C 0.2913(3) 0.0245(3) 0.2354(2) 0.0326(7) Uani 1 1 d . . . C15 C 0.2174(4) -0.0579(3) 0.2670(2) 0.0383(8) Uani 1 1 d . . . H9 H 0.1629 -0.0637 0.2405 0.046 Uiso 1 1 calc R . . C16 C 0.2232(4) -0.1314(3) 0.3369(2) 0.0506(11) Uani 1 1 d . . . H10 H 0.1725 -0.1870 0.3578 0.061 Uiso 1 1 calc R . . C17 C 0.3018(5) -0.1244(4) 0.3761(3) 0.0597(13) Uani 1 1 d . . . H11 H 0.3050 -0.1747 0.4239 0.072 Uiso 1 1 calc R . . C18 C 0.3755(4) -0.0444(4) 0.3458(2) 0.0560(12) Uani 1 1 d . . . H12 H 0.4295 -0.0397 0.3731 0.067 Uiso 1 1 calc R . . C19 C 0.3723(4) 0.0306(3) 0.2754(2) 0.0419(9) Uani 1 1 d . . . H13 H 0.4245 0.0850 0.2547 0.050 Uiso 1 1 calc R . . C20 C 0.3837(3) 0.4494(3) -0.1888(2) 0.0334(8) Uani 1 1 d . A . C21 C 0.4348(3) 0.5454(3) -0.2022(3) 0.0488(11) Uani 1 1 d . A . C22 C 0.4808(4) 0.6000(3) -0.2772(3) 0.0642(16) Uani 1 1 d . A . H14 H 0.5207 0.6609 -0.2868 0.077 Uiso 1 1 calc R . . C23 C 0.4726(4) 0.5723(4) -0.3371(3) 0.075(2) Uani 1 1 d . . . C24 C 0.4066(3) 0.4873(3) -0.3233(2) 0.0517(12) Uani 1 1 d . B . H15 H 0.3927 0.4716 -0.3648 0.062 Uiso 1 1 calc R . . C25 C 0.3609(3) 0.4255(3) -0.2508(2) 0.0334(8) Uani 1 1 d . . . C26 C 0.4402(4) 0.6005(4) -0.1432(4) 0.0733(18) Uani 1 1 d . . . C27 C 0.4074(8) 0.5238(7) -0.0457(5) 0.034(2) Uiso 0.422(10) 1 d P A 1 H72 H 0.4046 0.5706 -0.0143 0.051 Uiso 0.422(10) 1 calc PR A 1 H73 H 0.4713 0.4607 -0.0372 0.051 Uiso 0.422(10) 1 calc PR A 1 H74 H 0.3285 0.4984 -0.0325 0.051 Uiso 0.422(10) 1 calc PR A 1 C28 C 0.3707(9) 0.7032(8) -0.1383(6) 0.046(3) Uiso 0.422(10) 1 d P A 1 H75 H 0.2888 0.6925 -0.1070 0.068 Uiso 0.422(10) 1 calc PR A 1 H76 H 0.3650 0.7494 -0.1889 0.068 Uiso 0.422(10) 1 calc PR A 1 H77 H 0.4103 0.7387 -0.1157 0.068 Uiso 0.422(10) 1 calc PR A 1 C29 C 0.5631(8) 0.6251(7) -0.1661(5) 0.0286(19) Uiso 0.422(10) 1 d P A 1 H78 H 0.5740 0.6633 -0.1329 0.043 Uiso 0.422(10) 1 calc PR A 1 H79 H 0.5783 0.6717 -0.2181 0.043 Uiso 0.422(10) 1 calc PR A 1 H80 H 0.6206 0.5569 -0.1629 0.043 Uiso 0.422(10) 1 calc PR A 1 C27A C 0.3721(7) 0.5619(6) -0.0740(4) 0.0406(18) Uiso 0.578(10) 1 d P A 2 H81 H 0.3449 0.6199 -0.0485 0.061 Uiso 0.578(10) 1 calc PR A 2 H82 H 0.4205 0.5003 -0.0452 0.061 Uiso 0.578(10) 1 calc PR A 2 H83 H 0.3009 0.5372 -0.0779 0.061 Uiso 0.578(10) 1 calc PR A 2 C28A C 0.3669(8) 0.7267(7) -0.1812(5) 0.057(2) Uiso 0.578(10) 1 d P A 2 H84 H 0.2799 0.7233 -0.1717 0.085 Uiso 0.578(10) 1 calc PR A 2 H85 H 0.4013 0.7495 -0.2357 0.085 Uiso 0.578(10) 1 calc PR A 2 H86 H 0.3775 0.7797 -0.1582 0.085 Uiso 0.578(10) 1 calc PR A 2 C29A C 0.5793(6) 0.6022(5) -0.1413(4) 0.0289(14) Uiso 0.578(10) 1 d P A 2 H87 H 0.5778 0.6379 -0.1034 0.043 Uiso 0.578(10) 1 calc PR A 2 H88 H 0.6223 0.6428 -0.1909 0.043 Uiso 0.578(10) 1 calc PR A 2 H89 H 0.6216 0.5271 -0.1283 0.043 Uiso 0.578(10) 1 calc PR A 2 C30 C 0.5463(7) 0.6122(6) -0.4289(4) 0.0407(17) Uiso 0.558(8) 1 d P B 1 C31 C 0.4465(8) 0.6686(8) -0.4724(5) 0.058(2) Uiso 0.558(8) 1 d P B 1 H90 H 0.4844 0.6993 -0.5256 0.087 Uiso 0.558(8) 1 calc PR B 1 H91 H 0.3956 0.7275 -0.4514 0.087 Uiso 0.558(8) 1 calc PR B 1 H92 H 0.3958 0.6150 -0.4680 0.087 Uiso 0.558(8) 1 calc PR B 1 C32 C 0.6267(9) 0.6908(8) -0.4359(6) 0.064(3) Uiso 0.558(8) 1 d P B 1 H93 H 0.6969 0.6511 -0.4149 0.096 Uiso 0.558(8) 1 calc PR B 1 H94 H 0.5810 0.7442 -0.4083 0.096 Uiso 0.558(8) 1 calc PR B 1 H95 H 0.6551 0.7289 -0.4892 0.096 Uiso 0.558(8) 1 calc PR B 1 C33 C 0.6227(7) 0.5177(7) -0.4608(4) 0.0454(19) Uiso 0.558(8) 1 d P B 1 H96 H 0.6629 0.5470 -0.5138 0.068 Uiso 0.558(8) 1 calc PR B 1 H97 H 0.5695 0.4666 -0.4570 0.068 Uiso 0.558(8) 1 calc PR B 1 H98 H 0.6845 0.4793 -0.4320 0.068 Uiso 0.558(8) 1 calc PR B 1 C30A C 0.5165(9) 0.6511(8) -0.4056(5) 0.043(2) Uiso 0.442(8) 1 d P B 2 C31A C 0.4125(10) 0.7114(9) -0.4452(6) 0.053(3) Uiso 0.442(8) 1 d P B 2 H99 H 0.3704 0.6578 -0.4501 0.079 Uiso 0.442(8) 1 calc PR B 2 H100 H 0.4463 0.7572 -0.4953 0.079 Uiso 0.442(8) 1 calc PR B 2 H101 H 0.3547 0.7575 -0.4154 0.079 Uiso 0.442(8) 1 calc PR B 2 C32A C 0.5868(11) 0.7390(10) -0.4076(7) 0.062(3) Uiso 0.442(8) 1 d P B 2 H102 H 0.5357 0.7837 -0.3746 0.093 Uiso 0.442(8) 1 calc PR B 2 H103 H 0.6082 0.7857 -0.4592 0.093 Uiso 0.442(8) 1 calc PR B 2 H104 H 0.6613 0.7036 -0.3901 0.093 Uiso 0.442(8) 1 calc PR B 2 C33A C 0.6051(9) 0.5749(9) -0.4503(5) 0.043(2) Uiso 0.442(8) 1 d P B 2 H105 H 0.6663 0.5315 -0.4222 0.065 Uiso 0.442(8) 1 calc PR B 2 H106 H 0.6456 0.6187 -0.4994 0.065 Uiso 0.442(8) 1 calc PR B 2 H107 H 0.5598 0.5259 -0.4576 0.065 Uiso 0.442(8) 1 calc PR B 2 C34 C 0.2898(3) 0.3326(3) -0.24254(18) 0.0282(7) Uani 1 1 d . B . C35 C 0.2577(4) 0.3430(4) -0.3169(2) 0.0473(10) Uani 1 1 d . . . H34 H 0.2041 0.2896 -0.3081 0.071 Uiso 1 1 calc R B . H35 H 0.3326 0.3291 -0.3545 0.071 Uiso 1 1 calc R . . H36 H 0.2160 0.4170 -0.3354 0.071 Uiso 1 1 calc R . . C36 C 0.3675(3) 0.2209(3) -0.22213(19) 0.0313(7) Uani 1 1 d . . . H37 H 0.3792 0.2056 -0.1713 0.047 Uiso 1 1 calc R B . H38 H 0.4470 0.2211 -0.2582 0.047 Uiso 1 1 calc R . . H39 H 0.3263 0.1644 -0.2238 0.047 Uiso 1 1 calc R . . C37 C 0.1687(3) 0.3375(3) -0.18359(18) 0.0291(7) Uani 1 1 d . . . H40 H 0.1215 0.2839 -0.1835 0.044 Uiso 1 1 calc R B . H41 H 0.1222 0.4110 -0.1959 0.044 Uiso 1 1 calc R . . H42 H 0.1848 0.3208 -0.1337 0.044 Uiso 1 1 calc R . . C38 C 0.0307(3) 0.1505(2) 0.20366(16) 0.0215(6) Uani 1 1 d . C . C39 C -0.0379(3) 0.0761(2) 0.19804(16) 0.0241(6) Uani 1 1 d . . . C40 C -0.1128(3) 0.0223(3) 0.26377(18) 0.0336(8) Uani 1 1 d . C . H43 H -0.1583 -0.0276 0.2609 0.040 Uiso 1 1 calc R . . C41 C -0.1248(4) 0.0376(3) 0.33340(19) 0.0424(9) Uani 1 1 d . . . C42 C -0.0714(4) 0.1207(3) 0.33471(18) 0.0369(8) Uani 1 1 d . C . H44 H -0.0873 0.1383 0.3810 0.044 Uiso 1 1 calc R . . C43 C 0.0048(3) 0.1805(2) 0.27161(17) 0.0253(6) Uani 1 1 d . . . C44 C -0.0340(3) 0.0532(2) 0.12323(17) 0.0246(6) Uani 1 1 d . . . C45 C -0.0473(3) 0.1596(3) 0.06116(17) 0.0276(7) Uani 1 1 d . . . H45 H -0.0522 0.1434 0.0160 0.041 Uiso 1 1 calc R . . H46 H 0.0234 0.1968 0.0493 0.041 Uiso 1 1 calc R . . H47 H -0.1218 0.2070 0.0782 0.041 Uiso 1 1 calc R . . C46 C 0.0838(3) -0.0214(3) 0.09852(18) 0.0306(7) Uani 1 1 d . . . H48 H 0.0921 -0.0886 0.1394 0.046 Uiso 1 1 calc R . . H49 H 0.1539 0.0166 0.0866 0.046 Uiso 1 1 calc R . . H50 H 0.0807 -0.0399 0.0538 0.046 Uiso 1 1 calc R . . C47 C -0.1401(3) -0.0065(3) 0.13274(19) 0.0359(8) Uani 1 1 d . . . H51 H -0.1440 -0.0092 0.0834 0.054 Uiso 1 1 calc R . . H52 H -0.2168 0.0329 0.1556 0.054 Uiso 1 1 calc R . . H53 H -0.1272 -0.0811 0.1654 0.054 Uiso 1 1 calc R . . C48 C -0.1880(5) -0.0383(4) 0.4048(3) 0.0387(11) Uiso 0.783(6) 1 d P C 1 C49 C -0.1273(5) -0.1546(5) 0.4154(3) 0.0537(15) Uiso 0.783(6) 1 d P C 1 H49A H -0.1715 -0.2007 0.4622 0.081 Uiso 0.783(6) 1 calc PR C 1 H49B H -0.0430 -0.1596 0.4181 0.081 Uiso 0.783(6) 1 calc PR C 1 H49C H -0.1277 -0.1796 0.3727 0.081 Uiso 0.783(6) 1 calc PR C 1 C50 C -0.3210(5) -0.0289(5) 0.3967(3) 0.0540(15) Uiso 0.783(6) 1 d P C 1 H50A H -0.3669 -0.0768 0.4418 0.081 Uiso 0.783(6) 1 calc PR C 1 H50B H -0.3182 -0.0511 0.3523 0.081 Uiso 0.783(6) 1 calc PR C 1 H50C H -0.3612 0.0469 0.3910 0.081 Uiso 0.783(6) 1 calc PR C 1 C51 C -0.2027(4) -0.0037(4) 0.4764(3) 0.0516(14) Uiso 0.783(6) 1 d P C 1 H51A H -0.2446 -0.0561 0.5203 0.077 Uiso 0.783(6) 1 calc PR C 1 H51B H -0.2508 0.0693 0.4718 0.077 Uiso 0.783(6) 1 calc PR C 1 H51C H -0.1222 -0.0022 0.4826 0.077 Uiso 0.783(6) 1 calc PR C 1 C48A C -0.2411(4) -0.0192(4) 0.3997(3) 0.008(2) Uiso 0.217(6) 1 d PR C 2 C49A C -0.1736(4) -0.0862(4) 0.4655(3) 0.064(6) Uiso 0.217(6) 1 d PR C 2 H49D H -0.1335 -0.0370 0.4767 0.095 Uiso 0.217(6) 1 calc PR C 2 H49E H -0.1125 -0.1448 0.4495 0.095 Uiso 0.217(6) 1 calc PR C 2 H49F H -0.2334 -0.1182 0.5107 0.095 Uiso 0.217(6) 1 calc PR C 2 C50A C -0.3004(4) -0.0881(4) 0.3819(3) 0.053(5) Uiso 0.217(6) 1 d PR C 2 H50D H -0.2394 -0.1429 0.3613 0.080 Uiso 0.217(6) 1 calc PR C 2 H50E H -0.3469 -0.0440 0.3444 0.080 Uiso 0.217(6) 1 calc PR C 2 H50F H -0.3558 -0.1251 0.4275 0.080 Uiso 0.217(6) 1 calc PR C 2 C51A C -0.3342(4) 0.0691(4) 0.4325(3) 0.084(8) Uiso 0.217(6) 1 d PR C 2 H51D H -0.2906 0.1152 0.4442 0.125 Uiso 0.217(6) 1 calc PR C 2 H51E H -0.3898 0.0334 0.4786 0.125 Uiso 0.217(6) 1 calc PR C 2 H51F H -0.3810 0.1145 0.3955 0.125 Uiso 0.217(6) 1 calc PR C 2 C52 C 0.0444(3) 0.2788(3) 0.28212(19) 0.0308(7) Uani 1 1 d . C . C53 C -0.0714(3) 0.3500(3) 0.3128(2) 0.0435(9) Uani 1 1 d . . . H63 H -0.0492 0.4110 0.3228 0.065 Uiso 1 1 calc R C . H64 H -0.1178 0.3059 0.3597 0.065 Uiso 1 1 calc R . . H65 H -0.1215 0.3787 0.2756 0.065 Uiso 1 1 calc R . . C54 C 0.1266(6) 0.2396(4) 0.3377(3) 0.083(2) Uani 1 1 d . . . H66 H 0.1999 0.1931 0.3183 0.124 Uiso 1 1 calc R C . H67 H 0.0825 0.1977 0.3865 0.124 Uiso 1 1 calc R . . H68 H 0.1500 0.3030 0.3441 0.124 Uiso 1 1 calc R . . C55 C 0.1073(4) 0.3543(3) 0.2103(2) 0.0550(12) Uani 1 1 d . . . H69 H 0.1865 0.3159 0.1897 0.083 Uiso 1 1 calc R C . H70 H 0.1193 0.4190 0.2210 0.083 Uiso 1 1 calc R . . H71 H 0.0568 0.3769 0.1735 0.083 Uiso 1 1 calc R . . P3 P 0.0000 0.5000 0.0000 0.0377(3) Uani 1 2 d S . . F1 F 0.12633(18) 0.44978(16) 0.02862(12) 0.0432(5) Uani 1 1 d . . . F2 F 0.0174(2) 0.39990(17) -0.03342(13) 0.0481(6) Uani 1 1 d . . . F3 F -0.07484(19) 0.43316(18) 0.07811(13) 0.0494(6) Uani 1 1 d . . . P4 P 1.0000 0.5000 0.5000 0.0594(5) Uani 1 2 d S . . F4 F 1.0887(3) 0.4371(3) 0.4431(2) 0.1031(12) Uani 1 1 d . . . F5 F 1.0824(3) 0.4435(3) 0.5569(2) 0.1003(12) Uani 1 1 d . . . F6 F 0.9193(3) 0.4034(3) 0.5366(2) 0.0967(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0161(2) 0.0247(2) 0.0353(2) -0.00906(17) -0.00355(16) -0.00140(16) P1 0.0144(4) 0.0287(4) 0.0389(5) -0.0150(3) -0.0027(3) -0.0026(3) P2 0.0193(4) 0.0226(4) 0.0287(4) -0.0074(3) -0.0083(3) -0.0005(3) N1 0.0166(12) 0.0336(14) 0.0386(15) -0.0183(12) -0.0095(11) -0.0009(11) C1 0.0155(14) 0.0350(17) 0.0451(19) -0.0253(15) -0.0088(13) 0.0006(13) C2 0.0218(16) 0.043(2) 0.056(2) -0.0302(18) -0.0132(15) 0.0016(15) C3 0.0271(18) 0.039(2) 0.057(2) -0.0259(18) -0.0224(17) 0.0120(15) C4 0.0287(18) 0.0347(18) 0.050(2) -0.0219(16) -0.0220(16) 0.0098(15) C5 0.0276(16) 0.0305(17) 0.0407(18) -0.0208(14) -0.0169(14) 0.0037(14) C6 0.0170(14) 0.0378(18) 0.0435(19) -0.0250(15) -0.0025(13) -0.0051(13) C7 0.0136(14) 0.0314(17) 0.054(2) -0.0277(16) -0.0023(13) -0.0003(13) C8 0.0221(16) 0.044(2) 0.052(2) -0.0291(17) -0.0046(15) -0.0063(15) C9 0.0183(16) 0.044(2) 0.061(2) -0.0320(18) -0.0043(15) -0.0024(15) C10 0.0172(15) 0.040(2) 0.061(2) -0.0253(18) 0.0016(15) -0.0039(14) C11 0.0238(17) 0.0365(19) 0.046(2) -0.0175(16) -0.0016(15) -0.0019(14) C12 0.0187(15) 0.0374(18) 0.051(2) -0.0234(16) -0.0059(14) -0.0014(14) C13 0.0272(16) 0.0258(15) 0.0347(17) -0.0127(13) -0.0151(13) 0.0001(13) C14 0.0339(18) 0.0299(17) 0.0390(18) -0.0148(14) -0.0213(15) 0.0096(14) C15 0.049(2) 0.0266(17) 0.044(2) -0.0096(15) -0.0273(18) 0.0059(16) C16 0.074(3) 0.032(2) 0.042(2) -0.0034(16) -0.028(2) 0.006(2) C17 0.093(4) 0.040(2) 0.052(3) -0.0107(19) -0.046(3) 0.015(2) C18 0.063(3) 0.061(3) 0.054(3) -0.026(2) -0.043(2) 0.025(2) C19 0.044(2) 0.046(2) 0.045(2) -0.0244(18) -0.0240(18) 0.0101(18) C20 0.0154(15) 0.0215(15) 0.055(2) -0.0074(14) 0.0015(14) -0.0045(12) C21 0.0175(16) 0.0203(17) 0.101(3) -0.0185(19) -0.0019(18) -0.0015(13) C22 0.023(2) 0.027(2) 0.118(4) 0.021(2) -0.019(2) -0.0121(16) C23 0.026(2) 0.062(3) 0.097(4) 0.056(3) -0.031(2) -0.021(2) C24 0.0270(19) 0.055(2) 0.052(2) 0.0256(19) -0.0164(17) -0.0142(18) C25 0.0173(15) 0.0238(16) 0.0447(19) 0.0069(14) -0.0044(13) -0.0029(12) C26 0.029(2) 0.050(3) 0.146(5) -0.067(3) 0.027(2) -0.0197(19) C34 0.0222(15) 0.0285(16) 0.0294(16) -0.0017(12) -0.0049(12) -0.0059(13) C35 0.040(2) 0.069(3) 0.0301(18) -0.0044(18) -0.0079(16) -0.016(2) C36 0.0248(16) 0.0298(17) 0.0380(18) -0.0119(14) -0.0040(13) -0.0019(14) C37 0.0204(15) 0.0277(16) 0.0363(17) -0.0041(13) -0.0059(13) -0.0058(13) C38 0.0211(14) 0.0208(14) 0.0224(14) -0.0038(11) -0.0082(11) -0.0016(12) C39 0.0283(16) 0.0196(14) 0.0226(14) -0.0058(11) -0.0043(12) -0.0019(12) C40 0.047(2) 0.0267(16) 0.0254(16) -0.0059(13) -0.0005(14) -0.0155(15) C41 0.067(3) 0.0319(18) 0.0224(16) -0.0051(13) 0.0037(16) -0.0187(18) C42 0.063(2) 0.0253(16) 0.0222(15) -0.0045(12) -0.0101(16) -0.0093(16) C43 0.0308(16) 0.0202(14) 0.0264(15) -0.0053(11) -0.0130(13) 0.0000(12) C44 0.0235(15) 0.0266(15) 0.0263(15) -0.0093(12) -0.0044(12) -0.0074(12) C45 0.0295(16) 0.0304(16) 0.0259(15) -0.0079(12) -0.0090(12) -0.0065(13) C46 0.0294(17) 0.0344(17) 0.0320(16) -0.0174(14) -0.0063(13) -0.0019(14) C47 0.0373(19) 0.042(2) 0.0343(18) -0.0140(15) -0.0040(14) -0.0179(16) C52 0.0340(18) 0.0264(16) 0.0383(18) -0.0150(14) -0.0142(14) -0.0005(14) C53 0.045(2) 0.0274(18) 0.053(2) -0.0182(16) 0.0077(18) -0.0094(16) C54 0.116(5) 0.056(3) 0.124(5) -0.054(3) -0.100(4) 0.030(3) C55 0.052(2) 0.054(2) 0.068(3) -0.042(2) 0.021(2) -0.035(2) P3 0.0274(6) 0.0207(6) 0.0438(7) -0.0022(5) 0.0133(5) 0.0001(5) F1 0.0307(11) 0.0290(11) 0.0498(13) -0.0032(9) 0.0073(9) 0.0018(9) F2 0.0437(12) 0.0266(11) 0.0624(15) -0.0157(10) 0.0012(11) 0.0045(9) F3 0.0380(12) 0.0414(12) 0.0440(12) 0.0039(10) 0.0126(9) -0.0097(10) P4 0.0512(10) 0.0679(12) 0.0609(11) -0.0198(9) -0.0264(8) 0.0078(9) F4 0.068(2) 0.137(3) 0.122(3) -0.083(3) -0.009(2) 0.001(2) F5 0.085(2) 0.116(3) 0.099(3) -0.008(2) -0.061(2) 0.004(2) F6 0.080(2) 0.077(2) 0.126(3) -0.016(2) -0.024(2) -0.0171(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.097(3) . ? Cu1 F1 2.241(2) . ? Cu1 P1 2.2613(10) . ? Cu1 P2 2.2638(9) . ? P1 C6 1.696(3) . ? P1 C20 1.817(4) . ? P2 C13 1.692(3) . ? P2 C38 1.825(3) . ? N1 C1 1.356(4) . ? N1 C5 1.363(4) . ? C1 C2 1.392(5) . ? C1 C6 1.488(5) . ? C2 C3 1.387(5) . ? C2 H1 0.9500 . ? C3 C4 1.384(5) . ? C3 H2 0.9500 . ? C4 C5 1.390(5) . ? C4 H3 0.9500 . ? C5 C13 1.481(5) . ? C6 C7 1.490(4) . ? C7 C8 1.396(5) . ? C7 C12 1.404(5) . ? C8 C9 1.387(5) . ? C8 H4 0.9500 . ? C9 C10 1.387(5) . ? C9 H5 0.9500 . ? C10 C11 1.390(5) . ? C10 H6 0.9500 . ? C11 C12 1.395(4) . ? C11 H7 0.9500 . ? C12 H8 0.9500 . ? C13 C14 1.486(5) . ? C14 C15 1.398(5) . ? C14 C19 1.406(5) . ? C15 C16 1.391(5) . ? C15 H9 0.9500 . ? C16 C17 1.375(6) . ? C16 H10 0.9500 . ? C17 C18 1.373(7) . ? C17 H11 0.9500 . ? C18 C19 1.401(6) . ? C18 H12 0.9500 . ? C19 H13 0.9500 . ? C20 C21 1.424(4) . ? C20 C25 1.436(5) . ? C21 C22 1.394(7) . ? C21 C26 1.553(7) . ? C22 C23 1.352(8) . ? C22 H14 0.9500 . ? C23 C24 1.402(6) . ? C23 C30A 1.427(10) . ? C23 C30 1.694(9) . ? C24 C25 1.388(5) . ? C24 H15 0.9500 . ? C25 C34 1.559(4) . ? C26 C27A 1.340(8) . ? C26 C28 1.415(10) . ? C26 C29 1.441(9) . ? C26 C29A 1.629(7) . ? C26 C28A 1.710(10) . ? C26 C27 1.797(11) . ? C27 H72 0.9800 . ? C27 H73 0.9800 . ? C27 H74 0.9800 . ? C28 H75 0.9800 . ? C28 H76 0.9800 . ? C28 H77 0.9800 . ? C29 H78 0.9800 . ? C29 H79 0.9800 . ? C29 H80 0.9800 . ? C27A H81 0.9800 . ? C27A H82 0.9800 . ? C27A H83 0.9800 . ? C28A H84 0.9800 . ? C28A H85 0.9800 . ? C28A H86 0.9800 . ? C29A H87 0.9800 . ? C29A H88 0.9800 . ? C29A H89 0.9800 . ? C30 C32 1.487(11) . ? C30 C31 1.538(11) . ? C30 C33 1.538(11) . ? C31 H90 0.9800 . ? C31 H91 0.9800 . ? C31 H92 0.9800 . ? C32 H93 0.9800 . ? C32 H94 0.9800 . ? C32 H95 0.9800 . ? C33 H96 0.9800 . ? C33 H97 0.9800 . ? C33 H98 0.9800 . ? C30A C32A 1.537(14) . ? C30A C33A 1.538(13) . ? C30A C31A 1.539(13) . ? C31A H99 0.9800 . ? C31A H100 0.9800 . ? C31A H101 0.9800 . ? C32A H102 0.9800 . ? C32A H103 0.9800 . ? C32A H104 0.9800 . ? C33A H105 0.9800 . ? C33A H106 0.9800 . ? C33A H107 0.9800 . ? C34 C36 1.527(4) . ? C34 C37 1.534(4) . ? C34 C35 1.543(5) . ? C35 H34 0.9800 . ? C35 H35 0.9800 . ? C35 H36 0.9800 . ? C36 H37 0.9800 . ? C36 H38 0.9800 . ? C36 H39 0.9800 . ? C37 H40 0.9800 . ? C37 H41 0.9800 . ? C37 H42 0.9800 . ? C38 C43 1.420(4) . ? C38 C39 1.434(4) . ? C39 C40 1.385(4) . ? C39 C44 1.553(4) . ? C40 C41 1.385(4) . ? C40 H43 0.9500 . ? C41 C42 1.376(5) . ? C41 C48 1.509(6) . ? C41 C48A 1.686(6) . ? C42 C43 1.396(4) . ? C42 H44 0.9500 . ? C43 C52 1.545(4) . ? C44 C45 1.524(4) . ? C44 C46 1.537(4) . ? C44 C47 1.538(4) . ? C45 H45 0.9800 . ? C45 H46 0.9800 . ? C45 H47 0.9800 . ? C46 H48 0.9800 . ? C46 H49 0.9800 . ? C46 H50 0.9800 . ? C47 H51 0.9800 . ? C47 H52 0.9800 . ? C47 H53 0.9800 . ? C48 C49 1.497(7) . ? C48 C51 1.541(7) . ? C48 C50 1.569(7) . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C48A C50A 1.4207 . ? C48A C51A 1.5527 . ? C48A C49A 1.5929 . ? C49A H49D 0.9800 . ? C49A H49E 0.9800 . ? C49A H49F 0.9800 . ? C50A H50D 0.9800 . ? C50A H50E 0.9800 . ? C50A H50F 0.9800 . ? C51A H51D 0.9800 . ? C51A H51E 0.9800 . ? C51A H51F 0.9800 . ? C52 C55 1.511(5) . ? C52 C54 1.530(5) . ? C52 C53 1.532(5) . ? C53 H63 0.9800 . ? C53 H64 0.9800 . ? C53 H65 0.9800 . ? C54 H66 0.9800 . ? C54 H67 0.9800 . ? C54 H68 0.9800 . ? C55 H69 0.9800 . ? C55 H70 0.9800 . ? C55 H71 0.9800 . ? P3 F2 1.586(2) . ? P3 F2 1.586(2) 2_565 ? P3 F3 1.588(2) . ? P3 F3 1.588(2) 2_565 ? P3 F1 1.637(2) 2_565 ? P3 F1 1.637(2) . ? P4 F5 1.558(3) 2_766 ? P4 F5 1.558(3) . ? P4 F4 1.576(3) 2_766 ? P4 F4 1.576(3) . ? P4 F6 1.594(3) 2_766 ? P4 F6 1.594(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 F1 144.32(9) . . ? N1 Cu1 P1 82.90(8) . . ? F1 Cu1 P1 102.98(6) . . ? N1 Cu1 P2 83.39(8) . . ? F1 Cu1 P2 98.69(6) . . ? P1 Cu1 P2 157.34(4) . . ? C6 P1 C20 108.16(16) . . ? C6 P1 Cu1 102.89(13) . . ? C20 P1 Cu1 143.79(11) . . ? C13 P2 C38 108.12(15) . . ? C13 P2 Cu1 102.80(12) . . ? C38 P2 Cu1 147.88(10) . . ? C1 N1 C5 119.1(3) . . ? C1 N1 Cu1 117.8(2) . . ? C5 N1 Cu1 117.3(2) . . ? N1 C1 C2 121.6(3) . . ? N1 C1 C6 117.8(3) . . ? C2 C1 C6 120.4(3) . . ? C3 C2 C1 119.1(3) . . ? C3 C2 H1 120.4 . . ? C1 C2 H1 120.4 . . ? C4 C3 C2 119.3(3) . . ? C4 C3 H2 120.4 . . ? C2 C3 H2 120.4 . . ? C3 C4 C5 119.6(4) . . ? C3 C4 H3 120.2 . . ? C5 C4 H3 120.2 . . ? N1 C5 C4 121.2(3) . . ? N1 C5 C13 118.3(3) . . ? C4 C5 C13 120.2(3) . . ? C1 C6 C7 117.3(3) . . ? C1 C6 P1 113.5(2) . . ? C7 C6 P1 129.2(3) . . ? C8 C7 C12 118.3(3) . . ? C8 C7 C6 119.3(3) . . ? C12 C7 C6 122.4(3) . . ? C9 C8 C7 121.2(4) . . ? C9 C8 H4 119.4 . . ? C7 C8 H4 119.4 . . ? C10 C9 C8 119.9(3) . . ? C10 C9 H5 120.0 . . ? C8 C9 H5 120.0 . . ? C9 C10 C11 120.1(3) . . ? C9 C10 H6 120.0 . . ? C11 C10 H6 120.0 . . ? C10 C11 C12 119.9(4) . . ? C10 C11 H7 120.0 . . ? C12 C11 H7 120.0 . . ? C11 C12 C7 120.6(3) . . ? C11 C12 H8 119.7 . . ? C7 C12 H8 119.7 . . ? C5 C13 C14 117.1(3) . . ? C5 C13 P2 114.7(2) . . ? C14 C13 P2 127.9(3) . . ? C15 C14 C19 118.7(3) . . ? C15 C14 C13 122.2(3) . . ? C19 C14 C13 119.1(3) . . ? C16 C15 C14 120.5(4) . . ? C16 C15 H9 119.8 . . ? C14 C15 H9 119.8 . . ? C17 C16 C15 120.6(4) . . ? C17 C16 H10 119.7 . . ? C15 C16 H10 119.7 . . ? C18 C17 C16 119.8(4) . . ? C18 C17 H11 120.1 . . ? C16 C17 H11 120.1 . . ? C17 C18 C19 121.1(4) . . ? C17 C18 H12 119.5 . . ? C19 C18 H12 119.5 . . ? C18 C19 C14 119.4(4) . . ? C18 C19 H13 120.3 . . ? C14 C19 H13 120.3 . . ? C21 C20 C25 119.2(3) . . ? C21 C20 P1 122.3(3) . . ? C25 C20 P1 117.7(2) . . ? C22 C21 C20 116.9(4) . . ? C22 C21 C26 115.4(4) . . ? C20 C21 C26 127.6(4) . . ? C23 C22 C21 124.6(4) . . ? C23 C22 H14 117.7 . . ? C21 C22 H14 117.7 . . ? C22 C23 C24 117.9(4) . . ? C22 C23 C30A 110.7(6) . . ? C24 C23 C30A 130.3(7) . . ? C22 C23 C30 130.1(4) . . ? C24 C23 C30 111.4(6) . . ? C30A C23 C30 25.9(4) . . ? C25 C24 C23 121.7(5) . . ? C25 C24 H15 119.1 . . ? C23 C24 H15 119.1 . . ? C24 C25 C20 118.5(3) . . ? C24 C25 C34 117.1(3) . . ? C20 C25 C34 124.4(3) . . ? C27A C26 C28 84.9(6) . . ? C27A C26 C29 129.7(7) . . ? C28 C26 C29 102.0(6) . . ? C27A C26 C21 114.4(4) . . ? C28 C26 C21 121.8(7) . . ? C29 C26 C21 103.8(5) . . ? C27A C26 C29A 111.6(6) . . ? C28 C26 C29A 108.4(5) . . ? C29 C26 C29A 18.9(4) . . ? C21 C26 C29A 112.7(3) . . ? C27A C26 C28A 106.9(5) . . ? C28 C26 C28A 27.5(5) . . ? C29 C26 C28A 99.2(6) . . ? C21 C26 C28A 97.0(5) . . ? C29A C26 C28A 113.3(5) . . ? C27A C26 C27 22.5(4) . . ? C28 C26 C27 100.3(6) . . ? C29 C26 C27 109.9(6) . . ? C21 C26 C27 117.8(4) . . ? C29A C26 C27 91.1(5) . . ? C28A C26 C27 125.9(5) . . ? C26 C27 H72 109.5 . . ? C26 C27 H73 109.5 . . ? C26 C27 H74 109.5 . . ? C26 C28 H75 109.5 . . ? C26 C28 H76 109.5 . . ? C26 C28 H77 109.5 . . ? C26 C29 H78 109.5 . . ? C26 C29 H79 109.5 . . ? C26 C29 H80 109.5 . . ? C26 C27A H81 109.5 . . ? C26 C27A H82 109.5 . . ? H81 C27A H82 109.5 . . ? C26 C27A H83 109.5 . . ? H81 C27A H83 109.5 . . ? H82 C27A H83 109.5 . . ? C26 C28A H84 109.5 . . ? C26 C28A H85 109.5 . . ? H84 C28A H85 109.5 . . ? C26 C28A H86 109.5 . . ? H84 C28A H86 109.5 . . ? H85 C28A H86 109.5 . . ? C26 C29A H87 109.5 . . ? C26 C29A H88 109.5 . . ? H87 C29A H88 109.5 . . ? C26 C29A H89 109.5 . . ? H87 C29A H89 109.5 . . ? H88 C29A H89 109.5 . . ? C32 C30 C31 110.8(7) . . ? C32 C30 C33 109.5(7) . . ? C31 C30 C33 108.9(6) . . ? C32 C30 C23 107.4(6) . . ? C31 C30 C23 105.9(6) . . ? C33 C30 C23 114.2(6) . . ? C23 C30A C32A 121.5(9) . . ? C23 C30A C33A 100.0(7) . . ? C32A C30A C33A 107.5(8) . . ? C23 C30A C31A 110.7(8) . . ? C32A C30A C31A 106.7(9) . . ? C33A C30A C31A 109.9(8) . . ? C30A C31A H99 109.5 . . ? C30A C31A H100 109.5 . . ? H99 C31A H100 109.5 . . ? C30A C31A H101 109.5 . . ? H99 C31A H101 109.5 . . ? H100 C31A H101 109.5 . . ? C30A C32A H102 109.5 . . ? C30A C32A H103 109.5 . . ? H102 C32A H103 109.5 . . ? C30A C32A H104 109.5 . . ? H102 C32A H104 109.5 . . ? H103 C32A H104 109.5 . . ? C30A C33A H105 109.5 . . ? C30A C33A H106 109.5 . . ? H105 C33A H106 109.5 . . ? C30A C33A H107 109.5 . . ? H105 C33A H107 109.5 . . ? H106 C33A H107 109.5 . . ? C36 C34 C37 110.6(3) . . ? C36 C34 C35 106.6(3) . . ? C37 C34 C35 106.4(3) . . ? C36 C34 C25 110.5(3) . . ? C37 C34 C25 110.9(3) . . ? C35 C34 C25 111.6(3) . . ? C34 C35 H34 109.5 . . ? C34 C35 H35 109.5 . . ? H34 C35 H35 109.5 . . ? C34 C35 H36 109.5 . . ? H34 C35 H36 109.5 . . ? H35 C35 H36 109.5 . . ? C34 C36 H37 109.5 . . ? C34 C36 H38 109.5 . . ? H37 C36 H38 109.5 . . ? C34 C36 H39 109.5 . . ? H37 C36 H39 109.5 . . ? H38 C36 H39 109.5 . . ? C34 C37 H40 109.5 . . ? C34 C37 H41 109.5 . . ? H40 C37 H41 109.5 . . ? C34 C37 H42 109.5 . . ? H40 C37 H42 109.5 . . ? H41 C37 H42 109.5 . . ? C43 C38 C39 119.7(3) . . ? C43 C38 P2 122.5(2) . . ? C39 C38 P2 116.8(2) . . ? C40 C39 C38 117.4(3) . . ? C40 C39 C44 118.5(3) . . ? C38 C39 C44 124.1(3) . . ? C41 C40 C39 123.5(3) . . ? C41 C40 H43 118.3 . . ? C39 C40 H43 118.3 . . ? C42 C41 C40 117.2(3) . . ? C42 C41 C48 121.8(3) . . ? C40 C41 C48 120.9(3) . . ? C42 C41 C48A 126.5(3) . . ? C40 C41 C48A 112.8(3) . . ? C48 C41 C48A 22.0(2) . . ? C41 C42 C43 123.4(3) . . ? C41 C42 H44 118.3 . . ? C43 C42 H44 118.3 . . ? C42 C43 C38 117.4(3) . . ? C42 C43 C52 115.7(3) . . ? C38 C43 C52 126.7(3) . . ? C45 C44 C46 110.5(3) . . ? C45 C44 C47 106.6(3) . . ? C46 C44 C47 106.5(3) . . ? C45 C44 C39 111.0(2) . . ? C46 C44 C39 111.2(2) . . ? C47 C44 C39 110.9(2) . . ? C44 C45 H45 109.5 . . ? C44 C45 H46 109.5 . . ? H45 C45 H46 109.5 . . ? C44 C45 H47 109.5 . . ? H45 C45 H47 109.5 . . ? H46 C45 H47 109.5 . . ? C44 C46 H48 109.5 . . ? C44 C46 H49 109.5 . . ? H48 C46 H49 109.5 . . ? C44 C46 H50 109.5 . . ? H48 C46 H50 109.5 . . ? H49 C46 H50 109.5 . . ? C44 C47 H51 109.5 . . ? C44 C47 H52 109.5 . . ? H51 C47 H52 109.5 . . ? C44 C47 H53 109.5 . . ? H51 C47 H53 109.5 . . ? H52 C47 H53 109.5 . . ? C49 C48 C41 112.4(4) . . ? C49 C48 C51 109.5(4) . . ? C41 C48 C51 113.9(4) . . ? C49 C48 C50 109.6(4) . . ? C41 C48 C50 105.7(4) . . ? C51 C48 C50 105.3(4) . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C48 C51 H51A 109.5 . . ? C48 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C48 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C50A C48A C51A 111.4 . . ? C50A C48A C49A 111.1 . . ? C51A C48A C49A 103.7 . . ? C50A C48A C41 118.3(2) . . ? C51A C48A C41 110.5(2) . . ? C49A C48A C41 100.4(2) . . ? C48A C49A H49D 109.5 . . ? C48A C49A H49E 109.5 . . ? H49D C49A H49E 109.5 . . ? C48A C49A H49F 109.5 . . ? H49D C49A H49F 109.5 . . ? H49E C49A H49F 109.5 . . ? C48A C50A H50D 109.5 . . ? C48A C50A H50E 109.5 . . ? H50D C50A H50E 109.5 . . ? C48A C50A H50F 109.5 . . ? H50D C50A H50F 109.5 . . ? H50E C50A H50F 109.5 . . ? C48A C51A H51D 109.5 . . ? C48A C51A H51E 109.5 . . ? H51D C51A H51E 109.5 . . ? C48A C51A H51F 109.5 . . ? H51D C51A H51F 109.5 . . ? H51E C51A H51F 109.5 . . ? C55 C52 C54 109.1(4) . . ? C55 C52 C53 104.9(3) . . ? C54 C52 C53 109.7(3) . . ? C55 C52 C43 114.8(3) . . ? C54 C52 C43 110.7(3) . . ? C53 C52 C43 107.5(3) . . ? C52 C53 H63 109.5 . . ? C52 C53 H64 109.5 . . ? H63 C53 H64 109.5 . . ? C52 C53 H65 109.5 . . ? H63 C53 H65 109.5 . . ? H64 C53 H65 109.5 . . ? C52 C54 H66 109.5 . . ? C52 C54 H67 109.5 . . ? H66 C54 H67 109.5 . . ? C52 C54 H68 109.5 . . ? H66 C54 H68 109.5 . . ? H67 C54 H68 109.5 . . ? C52 C55 H69 109.5 . . ? C52 C55 H70 109.5 . . ? H69 C55 H70 109.5 . . ? C52 C55 H71 109.5 . . ? H69 C55 H71 109.5 . . ? H70 C55 H71 109.5 . . ? F2 P3 F2 180.00(14) . 2_565 ? F2 P3 F3 89.88(12) . . ? F2 P3 F3 90.12(12) 2_565 . ? F2 P3 F3 90.12(12) . 2_565 ? F2 P3 F3 89.88(12) 2_565 2_565 ? F3 P3 F3 180.0(2) . 2_565 ? F2 P3 F1 89.88(11) . 2_565 ? F2 P3 F1 90.12(11) 2_565 2_565 ? F3 P3 F1 90.00(11) . 2_565 ? F3 P3 F1 90.00(11) 2_565 2_565 ? F2 P3 F1 90.12(11) . . ? F2 P3 F1 89.88(11) 2_565 . ? F3 P3 F1 90.00(11) . . ? F3 P3 F1 90.00(11) 2_565 . ? F1 P3 F1 180.0(2) 2_565 . ? P3 F1 Cu1 128.95(13) . . ? F5 P4 F5 180.0(2) 2_766 . ? F5 P4 F4 89.4(2) 2_766 2_766 ? F5 P4 F4 90.6(2) . 2_766 ? F5 P4 F4 90.6(2) 2_766 . ? F5 P4 F4 89.4(2) . . ? F4 P4 F4 180.0(2) 2_766 . ? F5 P4 F6 90.55(19) 2_766 2_766 ? F5 P4 F6 89.4(2) . 2_766 ? F4 P4 F6 91.2(2) 2_766 2_766 ? F4 P4 F6 88.8(2) . 2_766 ? F5 P4 F6 89.4(2) 2_766 . ? F5 P4 F6 90.55(19) . . ? F4 P4 F6 88.8(2) 2_766 . ? F4 P4 F6 91.2(2) . . ? F6 P4 F6 180.0(3) 2_766 . ? 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 P1 C6 -8.85(13) . . . . ? F1 Cu1 P1 C6 135.38(13) . . . . ? P2 Cu1 P1 C6 -62.01(14) . . . . ? N1 Cu1 P1 C20 -157.5(2) . . . . ? F1 Cu1 P1 C20 -13.3(2) . . . . ? P2 Cu1 P1 C20 149.3(2) . . . . ? N1 Cu1 P2 C13 5.61(13) . . . . ? F1 Cu1 P2 C13 -138.44(12) . . . . ? P1 Cu1 P2 C13 58.69(14) . . . . ? N1 Cu1 P2 C38 169.7(2) . . . . ? F1 Cu1 P2 C38 25.7(2) . . . . ? P1 Cu1 P2 C38 -137.17(19) . . . . ? F1 Cu1 N1 C1 -106.3(2) . . . . ? P1 Cu1 N1 C1 -3.9(2) . . . . ? P2 Cu1 N1 C1 158.0(2) . . . . ? F1 Cu1 N1 C5 100.8(2) . . . . ? P1 Cu1 N1 C5 -156.8(2) . . . . ? P2 Cu1 N1 C5 5.2(2) . . . . ? C5 N1 C1 C2 -3.7(4) . . . . ? Cu1 N1 C1 C2 -156.0(2) . . . . ? C5 N1 C1 C6 170.9(3) . . . . ? Cu1 N1 C1 C6 18.6(3) . . . . ? N1 C1 C2 C3 0.6(5) . . . . ? C6 C1 C2 C3 -173.8(3) . . . . ? C1 C2 C3 C4 2.0(5) . . . . ? C2 C3 C4 C5 -1.5(5) . . . . ? C1 N1 C5 C4 4.2(4) . . . . ? Cu1 N1 C5 C4 156.7(2) . . . . ? C1 N1 C5 C13 -169.4(3) . . . . ? Cu1 N1 C5 C13 -16.9(3) . . . . ? C3 C4 C5 N1 -1.6(5) . . . . ? C3 C4 C5 C13 171.8(3) . . . . ? N1 C1 C6 C7 155.7(3) . . . . ? C2 C1 C6 C7 -29.6(4) . . . . ? N1 C1 C6 P1 -26.7(4) . . . . ? C2 C1 C6 P1 148.0(3) . . . . ? C20 P1 C6 C1 -178.5(2) . . . . ? Cu1 P1 C6 C1 20.4(2) . . . . ? C20 P1 C6 C7 -1.2(3) . . . . ? Cu1 P1 C6 C7 -162.3(3) . . . . ? C1 C6 C7 C8 -44.9(4) . . . . ? P1 C6 C7 C8 137.9(3) . . . . ? C1 C6 C7 C12 136.2(3) . . . . ? P1 C6 C7 C12 -41.0(5) . . . . ? C12 C7 C8 C9 1.4(5) . . . . ? C6 C7 C8 C9 -177.6(3) . . . . ? C7 C8 C9 C10 -1.1(5) . . . . ? C8 C9 C10 C11 0.1(5) . . . . ? C9 C10 C11 C12 0.6(5) . . . . ? C10 C11 C12 C7 -0.3(5) . . . . ? C8 C7 C12 C11 -0.7(5) . . . . ? C6 C7 C12 C11 178.2(3) . . . . ? N1 C5 C13 C14 -163.2(3) . . . . ? C4 C5 C13 C14 23.2(4) . . . . ? N1 C5 C13 P2 22.2(4) . . . . ? C4 C5 C13 P2 -151.5(3) . . . . ? C38 P2 C13 C5 173.3(2) . . . . ? Cu1 P2 C13 C5 -15.5(2) . . . . ? C38 P2 C13 C14 -0.6(3) . . . . ? Cu1 P2 C13 C14 170.6(3) . . . . ? C5 C13 C14 C15 -122.8(4) . . . . ? P2 C13 C14 C15 51.0(4) . . . . ? C5 C13 C14 C19 55.4(4) . . . . ? P2 C13 C14 C19 -130.8(3) . . . . ? C19 C14 C15 C16 0.8(6) . . . . ? C13 C14 C15 C16 178.9(3) . . . . ? C14 C15 C16 C17 -0.1(6) . . . . ? C15 C16 C17 C18 -0.2(7) . . . . ? C16 C17 C18 C19 -0.1(7) . . . . ? C17 C18 C19 C14 0.8(6) . . . . ? C15 C14 C19 C18 -1.1(5) . . . . ? C13 C14 C19 C18 -179.3(3) . . . . ? C6 P1 C20 C21 -64.4(3) . . . . ? Cu1 P1 C20 C21 83.3(3) . . . . ? C6 P1 C20 C25 104.9(3) . . . . ? Cu1 P1 C20 C25 -107.3(3) . . . . ? C25 C20 C21 C22 -11.7(5) . . . . ? P1 C20 C21 C22 157.5(3) . . . . ? C25 C20 C21 C26 165.2(4) . . . . ? P1 C20 C21 C26 -25.6(5) . . . . ? C20 C21 C22 C23 4.7(6) . . . . ? C26 C21 C22 C23 -172.6(4) . . . . ? C21 C22 C23 C24 4.3(7) . . . . ? C21 C22 C23 C30A 173.6(5) . . . . ? C21 C22 C23 C30 -166.2(5) . . . . ? C22 C23 C24 C25 -6.3(6) . . . . ? C30A C23 C24 C25 -173.2(7) . . . . ? C30 C23 C24 C25 165.8(4) . . . . ? C23 C24 C25 C20 -0.7(6) . . . . ? C23 C24 C25 C34 -179.5(4) . . . . ? C21 C20 C25 C24 9.9(5) . . . . ? P1 C20 C25 C24 -159.9(3) . . . . ? C21 C20 C25 C34 -171.4(3) . . . . ? P1 C20 C25 C34 18.8(4) . . . . ? C22 C21 C26 C27A 165.7(5) . . . . ? C20 C21 C26 C27A -11.3(7) . . . . ? C22 C21 C26 C28 66.0(7) . . . . ? C20 C21 C26 C28 -110.9(7) . . . . ? C22 C21 C26 C29 -47.8(6) . . . . ? C20 C21 C26 C29 135.3(5) . . . . ? C22 C21 C26 C29A -65.4(6) . . . . ? C20 C21 C26 C29A 117.7(5) . . . . ? C22 C21 C26 C28A 53.5(5) . . . . ? C20 C21 C26 C28A -123.5(5) . . . . ? C22 C21 C26 C27 -169.5(4) . . . . ? C20 C21 C26 C27 13.6(6) . . . . ? C22 C23 C30 C32 -1.3(9) . . . . ? C24 C23 C30 C32 -172.3(6) . . . . ? C30A C23 C30 C32 46.3(11) . . . . ? C22 C23 C30 C31 -119.8(6) . . . . ? C24 C23 C30 C31 69.2(6) . . . . ? C30A C23 C30 C31 -72.2(12) . . . . ? C22 C23 C30 C33 120.3(7) . . . . ? C24 C23 C30 C33 -50.6(6) . . . . ? C30A C23 C30 C33 168.0(14) . . . . ? C22 C23 C30A C32A 11.8(11) . . . . ? C24 C23 C30A C32A 179.4(8) . . . . ? C30 C23 C30A C32A -131.0(16) . . . . ? C22 C23 C30A C33A 129.6(6) . . . . ? C24 C23 C30A C33A -62.8(9) . . . . ? C30 C23 C30A C33A -13.2(8) . . . . ? C22 C23 C30A C31A -114.5(7) . . . . ? C24 C23 C30A C31A 53.1(11) . . . . ? C30 C23 C30A C31A 102.7(13) . . . . ? C24 C25 C34 C36 105.3(3) . . . . ? C20 C25 C34 C36 -73.4(4) . . . . ? C24 C25 C34 C37 -131.6(3) . . . . ? C20 C25 C34 C37 49.6(4) . . . . ? C24 C25 C34 C35 -13.1(4) . . . . ? C20 C25 C34 C35 168.1(3) . . . . ? C13 P2 C38 C43 68.4(3) . . . . ? Cu1 P2 C38 C43 -95.3(3) . . . . ? C13 P2 C38 C39 -99.7(2) . . . . ? Cu1 P2 C38 C39 96.6(3) . . . . ? C43 C38 C39 C40 -10.7(4) . . . . ? P2 C38 C39 C40 157.7(2) . . . . ? C43 C38 C39 C44 168.7(3) . . . . ? P2 C38 C39 C44 -22.8(4) . . . . ? C38 C39 C40 C41 0.5(5) . . . . ? C44 C39 C40 C41 -179.0(3) . . . . ? C39 C40 C41 C42 8.6(6) . . . . ? C39 C40 C41 C48 -168.1(4) . . . . ? C39 C40 C41 C48A 169.0(3) . . . . ? C40 C41 C42 C43 -7.8(6) . . . . ? C48 C41 C42 C43 168.9(4) . . . . ? C48A C41 C42 C43 -165.1(4) . . . . ? C41 C42 C43 C38 -2.1(5) . . . . ? C41 C42 C43 C52 173.5(4) . . . . ? C39 C38 C43 C42 11.5(4) . . . . ? P2 C38 C43 C42 -156.3(3) . . . . ? C39 C38 C43 C52 -163.5(3) . . . . ? P2 C38 C43 C52 28.7(4) . . . . ? C40 C39 C44 C45 132.2(3) . . . . ? C38 C39 C44 C45 -47.3(4) . . . . ? C40 C39 C44 C46 -104.4(3) . . . . ? C38 C39 C44 C46 76.1(4) . . . . ? C40 C39 C44 C47 13.9(4) . . . . ? C38 C39 C44 C47 -165.6(3) . . . . ? C42 C41 C48 C49 -117.0(5) . . . . ? C40 C41 C48 C49 59.6(6) . . . . ? C48A C41 C48 C49 133.6(9) . . . . ? C42 C41 C48 C51 8.4(6) . . . . ? C40 C41 C48 C51 -175.1(4) . . . . ? C48A C41 C48 C51 -101.1(8) . . . . ? C42 C41 C48 C50 123.5(5) . . . . ? C40 C41 C48 C50 -60.0(5) . . . . ? C48A C41 C48 C50 14.0(5) . . . . ? C42 C41 C48A C50A 167.4(3) . . . . ? C40 C41 C48A C50A 9.2(4) . . . . ? C48 C41 C48A C50A -107.3(7) . . . . ? C42 C41 C48A C51A 37.3(5) . . . . ? C40 C41 C48A C51A -120.9(3) . . . . ? C48 C41 C48A C51A 122.6(7) . . . . ? C42 C41 C48A C49A -71.7(4) . . . . ? C40 C41 C48A C49A 130.1(3) . . . . ? C48 C41 C48A C49A 13.6(6) . . . . ? C42 C43 C52 C55 -169.4(3) . . . . ? C38 C43 C52 C55 5.7(5) . . . . ? C42 C43 C52 C54 66.6(5) . . . . ? C38 C43 C52 C54 -118.3(4) . . . . ? C42 C43 C52 C53 -53.2(4) . . . . ? C38 C43 C52 C53 122.0(3) . . . . ? F2 P3 F1 Cu1 -1.32(14) . . . . ? F2 P3 F1 Cu1 178.68(14) 2_565 . . . ? F3 P3 F1 Cu1 88.55(15) . . . . ? F3 P3 F1 Cu1 -91.45(15) 2_565 . . . ? F1 P3 F1 Cu1 -115(100) 2_565 . . . ? N1 Cu1 F1 P3 178.75(15) . . . . ? P1 Cu1 F1 P3 82.81(13) . . . . ? P2 Cu1 F1 P3 -90.50(13) . . . . ? _diffrn_measured_fraction_theta_max 0.961 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.961 _refine_diff_density_max 0.848 _refine_diff_density_min -0.812 _refine_diff_density_rms 0.084