# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Nazhen Liu' _publ_contact_author_email nazhen0106@163.com loop_ _publ_author_name 'Nazhen Liu' 'Xiaoyan Li' 'Hongjian Sun' # Attachment '- 2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 780554' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H46 Co Ni P4' _chemical_formula_sum 'C40 H46 Co Ni P4' _chemical_formula_weight 768.29 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 25.604(5) _cell_length_b 18.385(4) _cell_length_c 17.539(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.91(3) _cell_angle_gamma 90.00 _cell_volume 8156(3) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5952 _cell_measurement_theta_min 1.61 _cell_measurement_theta_max 25.66 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.27 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3208 _exptl_absorpt_coefficient_mu 1.050 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7366 _exptl_absorpt_correction_T_max 0.7646 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23945 _diffrn_reflns_av_R_equivalents 0.1434 _diffrn_reflns_av_sigmaI/netI 0.2263 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.37 _diffrn_reflns_theta_max 25.66 _reflns_number_total 13110 _reflns_number_gt 5739 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Restrains were used for 'Large Non-Solvent C Ueq(max)/Ueq(min) 8.63 Ratio' and 'Check Low Ueq as Compared to Neighbors for P3'. ; _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^)+(0.0782P)^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 13110 _refine_ls_number_parameters 841 _refine_ls_number_restraints 1626 _refine_ls_R_factor_all 0.2057 _refine_ls_R_factor_gt 0.1016 _refine_ls_wR_factor_ref 0.2367 _refine_ls_wR_factor_gt 0.1963 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 0.912 _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 Ni1 Ni -0.00079(7) 0.68908(7) 0.43054(7) 0.0340(4) Uani 1 1 d . . . Ni2 Ni 0.52579(7) 0.68720(7) 0.48048(8) 0.0368(4) Uani 1 1 d . . . Co1 Co 0.13369(7) 0.81099(7) 0.54593(8) 0.0348(4) Uani 1 1 d . . . Co2 Co 0.64809(7) 0.83805(7) 0.57859(8) 0.0344(4) Uani 1 1 d . . . P1 P -0.08204(14) 0.67066(13) 0.43675(16) 0.0362(7) Uani 1 1 d . . . P2 P 0.00309(12) 0.80358(12) 0.44707(14) 0.0282(6) Uani 1 1 d . . . P3 P 0.17559(17) 0.82072(15) 0.66090(19) 0.0525(11) Uani 1 1 d . . . P4 P 0.13233(13) 0.69646(13) 0.52984(15) 0.0330(7) Uani 1 1 d . . . P5 P 0.51544(13) 0.80023(12) 0.49358(14) 0.0301(7) Uani 1 1 d . . . P6 P 0.47480(16) 0.66872(14) 0.37390(17) 0.0465(9) Uani 1 1 d . . . P7 P 0.65854(14) 0.72424(14) 0.56461(15) 0.0353(8) Uani 1 1 d . . . P8 P 0.72106(15) 0.88026(16) 0.5534(2) 0.0475(9) Uani 1 1 d . . . C1 C -0.1289(6) 0.7411(6) 0.4502(7) 0.054(3) Uani 1 1 d U . . H1A H -0.1641 0.7219 0.4392 0.080 Uiso 1 1 calc R . . H1B H -0.1252 0.7808 0.4159 0.080 Uiso 1 1 calc R . . H1C H -0.1222 0.7580 0.5026 0.080 Uiso 1 1 calc R . . C2 C -0.1193(7) 0.6285(6) 0.3503(7) 0.059(3) Uani 1 1 d U . . H2A H -0.1026 0.5837 0.3397 0.089 Uiso 1 1 calc R . . H2B H -0.1200 0.6609 0.3072 0.089 Uiso 1 1 calc R . . H2C H -0.1548 0.6189 0.3589 0.089 Uiso 1 1 calc R . . C3 C -0.0949(8) 0.6056(7) 0.5082(8) 0.065(3) Uani 1 1 d U . . H3A H -0.0794 0.6222 0.5585 0.097 Uiso 1 1 calc R . . H3B H -0.0799 0.5595 0.4978 0.097 Uiso 1 1 calc R . . H3C H -0.1324 0.6003 0.5063 0.097 Uiso 1 1 calc R . . C4 C -0.0302(5) 0.8396(5) 0.5250(6) 0.0363(16) Uani 1 1 d U . . C5 C -0.0240(6) 0.7996(5) 0.5943(6) 0.0413(18) Uani 1 1 d U . . H5 H -0.0032 0.7579 0.5996 0.050 Uiso 1 1 calc R . . C6 C -0.0488(6) 0.8225(5) 0.6541(6) 0.045(2) Uani 1 1 d U . . H6 H -0.0437 0.7965 0.7002 0.053 Uiso 1 1 calc R . . C7 C -0.0806(6) 0.8823(5) 0.6478(6) 0.042(2) Uani 1 1 d U . . H7 H -0.0981 0.8959 0.6883 0.050 Uiso 1 1 calc R . . C8 C -0.0866(6) 0.9220(5) 0.5812(6) 0.041(2) Uani 1 1 d U . . H8 H -0.1075 0.9636 0.5772 0.049 Uiso 1 1 calc R . . C9 C -0.0626(6) 0.9019(5) 0.5208(6) 0.0387(17) Uani 1 1 d U . . H9 H -0.0677 0.9296 0.4759 0.046 Uiso 1 1 calc R . . C10 C -0.0251(5) 0.8626(5) 0.3642(6) 0.0354(16) Uani 1 1 d U . . C11 C -0.0126(6) 0.9356(5) 0.3602(6) 0.0407(16) Uani 1 1 d U . . H11 H 0.0102 0.9571 0.4004 0.049 Uiso 1 1 calc R . . C12 C -0.0338(6) 0.9770(5) 0.2965(6) 0.041(2) Uani 1 1 d U . . H12 H -0.0248 1.0258 0.2933 0.049 Uiso 1 1 calc R . . C13 C -0.0682(6) 0.9447(6) 0.2387(6) 0.045(2) Uani 1 1 d U . . H13 H -0.0835 0.9729 0.1971 0.054 Uiso 1 1 calc R . . C14 C -0.0804(6) 0.8738(6) 0.2400(6) 0.045(2) Uani 1 1 d U . . H14 H -0.1028 0.8528 0.1991 0.054 Uiso 1 1 calc R . . C15 C -0.0593(6) 0.8319(5) 0.3035(6) 0.041(2) Uani 1 1 d U . . H15 H -0.0681 0.7829 0.3053 0.049 Uiso 1 1 calc R . . C16 C 0.0675(5) 0.8474(5) 0.4717(6) 0.0372(15) Uani 1 1 d U . . C17 C 0.0820(5) 0.8991(5) 0.5304(6) 0.0390(17) Uani 1 1 d U . . H17 H 0.0595 0.9153 0.5676 0.047 Uiso 1 1 calc R . . C18 C 0.1339(6) 0.9222(6) 0.5293(7) 0.048(2) Uani 1 1 d U . . H18 H 0.1534 0.9579 0.5642 0.057 Uiso 1 1 calc R . . C19 C 0.1526(6) 0.8874(5) 0.4642(7) 0.045(2) Uani 1 1 d U . . H19 H 0.1871 0.8944 0.4474 0.055 Uiso 1 1 calc R . . C20 C 0.1117(5) 0.8403(5) 0.4311(6) 0.0406(17) Uani 1 1 d U . . H20 H 0.1130 0.8084 0.3867 0.049 Uiso 1 1 calc R . . C21 C 0.0666(6) 0.6710(5) 0.3822(6) 0.0420(18) Uani 1 1 d U . . H21 H 0.0849 0.7074 0.3553 0.050 Uiso 1 1 calc R . . C22 C 0.0768(6) 0.6561(5) 0.4648(6) 0.0423(16) Uani 1 1 d U . . C23 C 0.0434(6) 0.5987(5) 0.4772(7) 0.0450(19) Uani 1 1 d U . . H23 H 0.0412 0.5763 0.5273 0.054 Uiso 1 1 calc R . . C24 C 0.0100(6) 0.5816(5) 0.4062(6) 0.045(2) Uani 1 1 d U . . H24 H -0.0176 0.5442 0.3993 0.054 Uiso 1 1 calc R . . C25 C 0.0269(6) 0.6225(6) 0.3466(7) 0.048(2) Uani 1 1 d U . . H25 H 0.0125 0.6201 0.2915 0.057 Uiso 1 1 calc R . . C26 C 0.1304(6) 0.6380(6) 0.6141(7) 0.0479(18) Uani 1 1 d U . . C27 C 0.0880(7) 0.6481(6) 0.6535(7) 0.053(2) Uani 1 1 d U . . H27 H 0.0620 0.6814 0.6341 0.064 Uiso 1 1 calc R . . C28 C 0.0827(7) 0.6110(7) 0.7203(7) 0.060(2) Uani 1 1 d U . . H28 H 0.0539 0.6191 0.7457 0.072 Uiso 1 1 calc R . . C29 C 0.1208(7) 0.5622(6) 0.7477(7) 0.054(2) Uani 1 1 d U . . H29 H 0.1179 0.5361 0.7923 0.065 Uiso 1 1 calc R . . C30 C 0.1631(7) 0.5509(6) 0.7113(7) 0.054(2) Uani 1 1 d U . . H30 H 0.1892 0.5183 0.7322 0.064 Uiso 1 1 calc R . . C31 C 0.1681(6) 0.5880(6) 0.6415(7) 0.0499(19) Uani 1 1 d U . . H31 H 0.1962 0.5784 0.6153 0.060 Uiso 1 1 calc R . . C32 C 0.1876(6) 0.6556(6) 0.4857(6) 0.0460(18) Uani 1 1 d U . . C33 C 0.1843(6) 0.5845(6) 0.4557(7) 0.0491(18) Uani 1 1 d U . . H33 H 0.1549 0.5560 0.4603 0.059 Uiso 1 1 calc R . . C34 C 0.2238(7) 0.5566(7) 0.4197(7) 0.054(2) Uani 1 1 d U . . H34 H 0.2201 0.5107 0.3971 0.065 Uiso 1 1 calc R . . C35 C 0.2685(7) 0.5965(6) 0.4173(7) 0.056(2) Uani 1 1 d U . . H35 H 0.2965 0.5757 0.3970 0.067 Uiso 1 1 calc R . . C36 C 0.2730(7) 0.6684(6) 0.4448(7) 0.056(2) Uani 1 1 d U . . H36 H 0.3024 0.6969 0.4401 0.068 Uiso 1 1 calc R . . C37 C 0.2307(6) 0.6955(7) 0.4801(7) 0.052(2) Uani 1 1 d U . . H37 H 0.2329 0.7424 0.5000 0.062 Uiso 1 1 calc R . . C38 C 0.1804(10) 0.7552(9) 0.7364(10) 0.094(4) Uani 1 1 d U . . H38A H 0.2117 0.7643 0.7729 0.142 Uiso 1 1 calc R . . H38B H 0.1822 0.7073 0.7151 0.142 Uiso 1 1 calc R . . H38C H 0.1499 0.7587 0.7618 0.142 Uiso 1 1 calc R . . C39 C 0.1441(10) 0.8899(10) 0.7205(11) 0.103(5) Uani 1 1 d U . . H39A H 0.1101 0.8725 0.7290 0.155 Uiso 1 1 calc R . . H39B H 0.1399 0.9354 0.6933 0.155 Uiso 1 1 calc R . . H39C H 0.1664 0.8968 0.7692 0.155 Uiso 1 1 calc R . . C40 C 0.2295(11) 0.8812(12) 0.6742(12) 0.119(5) Uani 1 1 d U . . H40A H 0.2223 0.9215 0.6393 0.178 Uiso 1 1 calc R . . H40B H 0.2607 0.8564 0.6643 0.178 Uiso 1 1 calc R . . H40C H 0.2348 0.8988 0.7264 0.178 Uiso 1 1 calc R . . C41 C 0.4221(7) 0.6010(6) 0.3783(8) 0.061(3) Uani 1 1 d U . . H41A H 0.4065 0.5876 0.3269 0.092 Uiso 1 1 calc R . . H41B H 0.3955 0.6216 0.4049 0.092 Uiso 1 1 calc R . . H41C H 0.4369 0.5586 0.4055 0.092 Uiso 1 1 calc R . . C42 C 0.4344(8) 0.7398(7) 0.3170(9) 0.068(3) Uani 1 1 d U . . H42A H 0.4573 0.7767 0.3018 0.102 Uiso 1 1 calc R . . H42B H 0.4107 0.7612 0.3479 0.102 Uiso 1 1 calc R . . H42C H 0.4145 0.7181 0.2718 0.102 Uiso 1 1 calc R . . C43 C 0.5076(7) 0.6326(7) 0.2997(7) 0.066(3) Uani 1 1 d U . . H43A H 0.5305 0.5936 0.3203 0.099 Uiso 1 1 calc R . . H43B H 0.5282 0.6702 0.2805 0.099 Uiso 1 1 calc R . . H43C H 0.4819 0.6145 0.2584 0.099 Uiso 1 1 calc R . . C44 C 0.7614(7) 0.9249(7) 0.6345(9) 0.064(4) Uani 1 1 d U . . H44A H 0.7760 0.8891 0.6716 0.096 Uiso 1 1 calc R . . H44B H 0.7400 0.9583 0.6583 0.096 Uiso 1 1 calc R . . H44C H 0.7896 0.9510 0.6166 0.096 Uiso 1 1 calc R . . C45 C 0.7147(8) 0.9536(7) 0.4831(8) 0.067(4) Uani 1 1 d U . . H45A H 0.7485 0.9765 0.4836 0.100 Uiso 1 1 calc R . . H45B H 0.6898 0.9888 0.4959 0.100 Uiso 1 1 calc R . . H45C H 0.7026 0.9343 0.4326 0.100 Uiso 1 1 calc R . . C46 C 0.7716(8) 0.8271(7) 0.5211(9) 0.070(4) Uani 1 1 d U . . H46A H 0.7590 0.8084 0.4705 0.105 Uiso 1 1 calc R . . H46B H 0.7809 0.7874 0.5561 0.105 Uiso 1 1 calc R . . H46C H 0.8022 0.8570 0.5192 0.105 Uiso 1 1 calc R . . C47 C 0.5162(6) 0.8572(5) 0.4060(6) 0.0429(17) Uani 1 1 d U . . C48 C 0.5502(6) 0.8411(6) 0.3610(6) 0.0452(19) Uani 1 1 d U . . H48 H 0.5717 0.8007 0.3731 0.054 Uiso 1 1 calc R . . C49 C 0.5562(6) 0.8813(6) 0.2952(6) 0.046(2) Uani 1 1 d U . . H49 H 0.5827 0.8707 0.2661 0.055 Uiso 1 1 calc R . . C50 C 0.5216(6) 0.9363(6) 0.2759(7) 0.047(2) Uani 1 1 d U . . H50 H 0.5242 0.9635 0.2319 0.056 Uiso 1 1 calc R . . C51 C 0.4843(6) 0.9529(6) 0.3173(6) 0.045(2) Uani 1 1 d U . . H51 H 0.4607 0.9904 0.3013 0.054 Uiso 1 1 calc R . . C52 C 0.4799(6) 0.9143(5) 0.3852(6) 0.0411(17) Uani 1 1 d U . . H52 H 0.4541 0.9259 0.4153 0.049 Uiso 1 1 calc R . . C53 C 0.4571(6) 0.8316(5) 0.5331(6) 0.0403(17) Uani 1 1 d U . . C54 C 0.4161(6) 0.7815(6) 0.5378(7) 0.047(2) Uani 1 1 d U . . H54 H 0.4187 0.7347 0.5186 0.056 Uiso 1 1 calc R . . C55 C 0.3721(6) 0.8004(6) 0.5703(7) 0.053(2) Uani 1 1 d U . . H55 H 0.3452 0.7667 0.5721 0.064 Uiso 1 1 calc R . . C56 C 0.3681(6) 0.8697(6) 0.6001(7) 0.051(2) Uani 1 1 d U . . H56 H 0.3385 0.8831 0.6214 0.061 Uiso 1 1 calc R . . C57 C 0.4079(6) 0.9175(6) 0.5978(7) 0.048(2) Uani 1 1 d U . . H57 H 0.4055 0.9637 0.6186 0.057 Uiso 1 1 calc R . . C58 C 0.4530(6) 0.8991(6) 0.5647(6) 0.0433(17) Uani 1 1 d U . . H58 H 0.4799 0.9329 0.5643 0.052 Uiso 1 1 calc R . . C59 C 0.5894(6) 0.6139(6) 0.4876(7) 0.0455(17) Uani 1 1 d U . . H59 H 0.6105 0.6044 0.4466 0.055 Uiso 1 1 calc R . . C60 C 0.6010(6) 0.6675(5) 0.5470(6) 0.0424(16) Uani 1 1 d U . . C61 C 0.5576(6) 0.6600(6) 0.5914(7) 0.0448(18) Uani 1 1 d U . . H61 H 0.5536 0.6890 0.6371 0.054 Uiso 1 1 calc R . . C62 C 0.5231(6) 0.6050(6) 0.5611(7) 0.049(2) Uani 1 1 d U . . H62 H 0.4918 0.5881 0.5817 0.058 Uiso 1 1 calc R . . C63 C 0.5422(6) 0.5778(6) 0.4968(7) 0.046(2) Uani 1 1 d U . . H63 H 0.5258 0.5386 0.4636 0.055 Uiso 1 1 calc R . . C64 C 0.5649(5) 0.8501(5) 0.5582(6) 0.0396(16) Uani 1 1 d U . . C65 C 0.5855(5) 0.8366(5) 0.6381(6) 0.0395(17) Uani 1 1 d U . . H65 H 0.5758 0.7948 0.6676 0.047 Uiso 1 1 calc R . . C66 C 0.6181(6) 0.8926(5) 0.6688(6) 0.040(2) Uani 1 1 d U . . H66 H 0.6355 0.8966 0.7225 0.048 Uiso 1 1 calc R . . C67 C 0.6247(5) 0.9397(5) 0.6087(6) 0.041(2) Uani 1 1 d U . . H67 H 0.6467 0.9835 0.6135 0.049 Uiso 1 1 calc R . . C68 C 0.5908(5) 0.9164(5) 0.5401(6) 0.0380(17) Uani 1 1 d U . . H68 H 0.5861 0.9410 0.4899 0.046 Uiso 1 1 calc R . . C69 C 0.6919(6) 0.6894(6) 0.4843(7) 0.0486(17) Uani 1 1 d U . . C70 C 0.6785(6) 0.7270(6) 0.4142(7) 0.049(2) Uani 1 1 d U . . H70 H 0.6589 0.7697 0.4123 0.059 Uiso 1 1 calc R . . C71 C 0.6941(6) 0.7007(7) 0.3499(7) 0.056(2) Uani 1 1 d U . . H71 H 0.6834 0.7236 0.3028 0.067 Uiso 1 1 calc R . . C72 C 0.7270(6) 0.6373(7) 0.3534(7) 0.054(2) Uani 1 1 d U . . H72 H 0.7386 0.6194 0.3093 0.065 Uiso 1 1 calc R . . C73 C 0.7410(6) 0.6042(7) 0.4228(7) 0.055(2) Uani 1 1 d U . . H73 H 0.7624 0.5632 0.4259 0.065 Uiso 1 1 calc R . . C74 C 0.7243(6) 0.6297(6) 0.4882(7) 0.0513(18) Uani 1 1 d U . . H74 H 0.7348 0.6065 0.5352 0.062 Uiso 1 1 calc R . . C75 C 0.6959(6) 0.6743(6) 0.6477(7) 0.0534(18) Uani 1 1 d U . . C76 C 0.6841(7) 0.6045(7) 0.6681(7) 0.0557(18) Uani 1 1 d U . . H76 H 0.6552 0.5803 0.6407 0.067 Uiso 1 1 calc R . . C77 C 0.7160(7) 0.5695(8) 0.7310(8) 0.065(2) Uani 1 1 d U . . H77 H 0.7086 0.5220 0.7443 0.079 Uiso 1 1 calc R . . C78 C 0.7559(8) 0.6045(8) 0.7700(9) 0.068(2) Uani 1 1 d U . . H78 H 0.7753 0.5820 0.8128 0.082 Uiso 1 1 calc R . . C79 C 0.7701(7) 0.6712(8) 0.7510(8) 0.068(2) Uani 1 1 d U . . H79 H 0.8000 0.6925 0.7792 0.082 Uiso 1 1 calc R . . C80 C 0.7412(7) 0.7103(7) 0.6895(8) 0.060(2) Uani 1 1 d U . . H80 H 0.7510 0.7569 0.6767 0.072 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ni1 0.0462(11) 0.0269(6) 0.0298(6) -0.0006(5) 0.0087(6) 0.0054(6) Ni2 0.0472(11) 0.0278(6) 0.0371(7) -0.0005(5) 0.0121(7) -0.0009(6) Co1 0.0443(11) 0.0272(6) 0.0328(7) 0.0026(6) 0.0061(7) 0.0009(6) Co2 0.0368(11) 0.0351(7) 0.0316(7) -0.0081(6) 0.0060(7) 0.0046(6) P1 0.042(2) 0.0296(13) 0.0381(14) -0.0066(10) 0.0109(13) -0.0019(11) P2 0.0358(19) 0.0238(11) 0.0265(12) 0.0022(9) 0.0097(11) 0.0050(11) P3 0.067(3) 0.0369(15) 0.0476(17) 0.0005(13) -0.0112(18) -0.0065(14) P4 0.039(2) 0.0323(13) 0.0288(13) 0.0055(10) 0.0094(12) 0.0038(12) P5 0.040(2) 0.0226(11) 0.0279(12) -0.0020(9) 0.0041(12) -0.0011(11) P6 0.062(3) 0.0356(14) 0.0406(16) -0.0102(12) 0.0024(16) -0.0009(13) P7 0.039(2) 0.0377(13) 0.0302(13) -0.0007(11) 0.0073(13) 0.0104(12) P8 0.036(2) 0.0504(16) 0.0570(19) -0.0210(14) 0.0111(17) -0.0013(14) C1 0.057(7) 0.047(5) 0.056(5) -0.015(5) 0.007(5) -0.002(5) C2 0.072(8) 0.051(5) 0.051(6) -0.023(5) 0.000(6) -0.005(5) C3 0.078(8) 0.055(6) 0.061(6) 0.001(5) 0.012(7) 0.001(6) C4 0.052(4) 0.031(3) 0.027(3) -0.001(3) 0.011(3) 0.003(3) C5 0.057(4) 0.035(3) 0.032(3) 0.002(3) 0.006(3) 0.002(3) C6 0.061(5) 0.039(4) 0.035(4) 0.003(3) 0.013(4) 0.006(4) C7 0.060(5) 0.042(4) 0.028(3) 0.000(3) 0.017(4) 0.002(4) C8 0.055(5) 0.036(3) 0.033(4) 0.004(3) 0.014(4) 0.003(3) C9 0.054(4) 0.032(3) 0.030(3) 0.007(3) 0.010(3) 0.002(3) C10 0.049(4) 0.032(3) 0.027(3) 0.003(3) 0.008(3) 0.001(3) C11 0.054(4) 0.036(3) 0.033(3) 0.006(3) 0.008(3) 0.002(3) C12 0.053(5) 0.037(3) 0.034(4) 0.009(3) 0.009(4) 0.003(3) C13 0.056(5) 0.042(4) 0.036(4) 0.009(3) 0.006(4) 0.009(4) C14 0.053(5) 0.046(4) 0.035(4) 0.006(3) 0.002(4) 0.002(4) C15 0.049(4) 0.039(3) 0.033(3) 0.002(3) 0.002(4) 0.002(3) C16 0.053(3) 0.030(3) 0.030(3) 0.004(2) 0.009(3) 0.001(3) C17 0.051(4) 0.032(3) 0.033(3) 0.001(3) 0.005(3) 0.004(3) C18 0.057(5) 0.044(4) 0.041(4) 0.008(3) 0.007(4) -0.003(4) C19 0.052(5) 0.042(4) 0.043(4) 0.009(4) 0.010(4) -0.008(4) C20 0.051(4) 0.036(3) 0.035(3) 0.008(3) 0.010(3) 0.002(3) C21 0.055(4) 0.039(3) 0.032(3) -0.004(3) 0.009(3) 0.007(3) C22 0.057(3) 0.036(3) 0.033(3) 0.002(3) 0.006(3) 0.008(3) C23 0.059(4) 0.037(3) 0.039(3) 0.003(3) 0.009(3) 0.008(3) C24 0.062(5) 0.034(4) 0.040(4) -0.005(3) 0.008(4) 0.006(4) C25 0.059(5) 0.041(4) 0.041(4) -0.005(3) 0.006(4) 0.008(4) C26 0.063(4) 0.045(3) 0.036(3) 0.007(3) 0.008(3) 0.002(3) C27 0.067(4) 0.055(4) 0.037(3) 0.008(3) 0.005(3) 0.004(3) C28 0.073(5) 0.066(4) 0.041(4) 0.012(4) 0.010(4) -0.001(4) C29 0.073(5) 0.056(4) 0.035(4) 0.010(4) 0.011(4) -0.005(4) C30 0.069(5) 0.049(4) 0.040(4) 0.009(4) 0.003(4) 0.002(4) C31 0.066(4) 0.046(3) 0.037(3) 0.009(3) 0.006(3) 0.005(3) C32 0.060(4) 0.042(3) 0.036(3) 0.004(3) 0.008(3) 0.004(3) C33 0.060(4) 0.045(3) 0.043(3) 0.003(3) 0.011(3) 0.005(3) C34 0.062(5) 0.051(4) 0.049(4) 0.000(4) 0.014(4) 0.009(4) C35 0.062(5) 0.057(4) 0.051(4) 0.005(4) 0.013(4) 0.009(4) C36 0.064(5) 0.052(4) 0.056(4) 0.001(4) 0.018(4) 0.001(4) C37 0.060(5) 0.049(4) 0.048(4) -0.004(4) 0.014(4) 0.002(4) C38 0.103(8) 0.107(7) 0.070(6) -0.004(6) 0.002(7) -0.010(7) C39 0.099(10) 0.132(9) 0.078(8) -0.003(8) 0.008(8) -0.004(8) C40 0.111(11) 0.159(10) 0.081(9) -0.005(9) 0.001(9) -0.029(9) C41 0.077(8) 0.055(6) 0.052(6) -0.018(5) 0.011(6) -0.012(6) C42 0.077(8) 0.057(6) 0.060(6) -0.007(5) -0.015(6) 0.002(6) C43 0.087(9) 0.066(6) 0.045(6) -0.025(5) 0.010(6) -0.001(6) C44 0.049(8) 0.066(7) 0.078(7) -0.013(6) 0.016(7) -0.018(6) C45 0.064(8) 0.070(6) 0.069(7) -0.009(6) 0.020(7) -0.019(6) C46 0.065(8) 0.071(7) 0.078(7) -0.020(6) 0.023(7) -0.010(6) C47 0.051(4) 0.040(3) 0.039(3) -0.003(3) 0.010(3) -0.002(3) C48 0.053(4) 0.044(3) 0.039(3) -0.001(3) 0.008(3) -0.001(3) C49 0.055(5) 0.048(4) 0.036(4) 0.004(3) 0.012(4) -0.003(4) C50 0.057(5) 0.044(4) 0.041(4) 0.004(3) 0.011(4) -0.004(4) C51 0.054(5) 0.041(4) 0.040(4) 0.000(3) 0.010(4) -0.002(4) C52 0.050(4) 0.039(3) 0.036(3) 0.003(3) 0.008(3) -0.001(3) C53 0.046(4) 0.038(3) 0.038(3) 0.002(3) 0.011(3) 0.002(3) C54 0.048(5) 0.047(4) 0.049(4) -0.004(4) 0.020(4) -0.008(4) C55 0.053(5) 0.053(4) 0.056(4) -0.004(4) 0.016(4) -0.001(4) C56 0.051(5) 0.053(4) 0.051(4) -0.002(4) 0.017(4) 0.000(4) C57 0.052(5) 0.048(4) 0.046(4) -0.003(4) 0.016(4) -0.001(4) C58 0.049(4) 0.041(3) 0.041(3) -0.002(3) 0.011(3) 0.000(3) C59 0.052(4) 0.046(3) 0.039(3) 0.000(3) 0.010(3) 0.009(3) C60 0.050(3) 0.041(3) 0.037(3) -0.003(3) 0.010(3) 0.010(3) C61 0.053(4) 0.040(3) 0.042(3) 0.003(3) 0.009(3) 0.009(3) C62 0.054(5) 0.045(4) 0.049(4) 0.006(4) 0.014(4) 0.005(4) C63 0.051(5) 0.041(4) 0.046(4) 0.003(3) 0.011(4) 0.005(4) C64 0.047(3) 0.037(3) 0.035(3) -0.002(3) 0.009(3) 0.004(3) C65 0.047(4) 0.038(3) 0.034(3) -0.003(3) 0.009(3) 0.003(3) C66 0.046(5) 0.040(4) 0.034(4) -0.008(3) 0.009(4) -0.001(4) C67 0.045(5) 0.035(4) 0.043(4) -0.010(3) 0.008(4) -0.001(3) C68 0.044(4) 0.034(3) 0.036(3) -0.001(3) 0.009(3) 0.000(3) C69 0.053(4) 0.051(3) 0.042(3) -0.005(3) 0.010(3) 0.009(3) C70 0.054(4) 0.056(4) 0.040(3) -0.010(3) 0.013(3) 0.004(3) C71 0.057(5) 0.066(4) 0.046(4) -0.009(4) 0.015(4) 0.004(4) C72 0.051(5) 0.066(4) 0.047(4) -0.014(4) 0.014(4) -0.001(4) C73 0.055(5) 0.061(4) 0.049(4) -0.015(4) 0.013(4) 0.008(4) C74 0.054(4) 0.057(3) 0.043(3) -0.006(3) 0.010(3) 0.010(3) C75 0.057(4) 0.058(3) 0.045(3) -0.002(3) 0.007(3) 0.016(3) C76 0.058(4) 0.059(3) 0.049(3) 0.003(3) 0.006(3) 0.018(3) C77 0.066(5) 0.072(4) 0.057(4) 0.007(4) 0.005(4) 0.026(4) C78 0.067(5) 0.078(4) 0.058(4) 0.002(4) 0.004(4) 0.023(4) C79 0.065(5) 0.079(4) 0.059(4) -0.006(4) 0.002(4) 0.022(4) C80 0.058(4) 0.069(4) 0.050(4) -0.004(3) 0.002(4) 0.019(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 Ni1 C24 2.050(10) . ? Ni1 C21 2.063(15) . ? Ni1 C22 2.074(13) . ? Ni1 C23 2.103(11) . ? Ni1 C25 2.120(13) . ? Ni1 P2 2.125(3) . ? Ni1 P1 2.127(4) . ? Ni2 C61 2.052(11) . ? Ni2 C63 2.066(11) . ? Ni2 C62 2.078(12) . ? Ni2 C59 2.103(13) . ? Ni2 P5 2.112(3) . ? Ni2 C60 2.123(12) . ? Ni2 P6 2.135(3) . ? Co1 C18 2.065(11) . ? Co1 C20 2.076(10) . ? Co1 C16 2.081(11) . ? Co1 C17 2.084(11) . ? Co1 C19 2.116(12) . ? Co1 P4 2.124(3) . ? Co1 P3 2.140(3) . ? Co2 C65 2.043(15) . ? Co2 C67 2.057(10) . ? Co2 C68 2.092(11) . ? Co2 C66 2.117(12) . ? Co2 C64 2.117(14) . ? Co2 P7 2.128(3) . ? Co2 P8 2.132(5) . ? P1 C3 1.799(15) . ? P1 C1 1.804(14) . ? P1 C2 1.833(11) . ? P2 C16 1.826(13) . ? P2 C4 1.842(12) . ? P2 C10 1.867(9) . ? P3 C40 1.76(2) . ? P3 C38 1.779(17) . ? P3 C39 1.90(2) . ? P4 C26 1.834(12) . ? P4 C22 1.836(12) . ? P4 C32 1.872(16) . ? P5 C64 1.811(11) . ? P5 C53 1.836(15) . ? P5 C47 1.862(12) . ? P6 C43 1.783(16) . ? P6 C41 1.846(16) . ? P6 C42 1.858(12) . ? P7 C60 1.792(14) . ? P7 C75 1.858(11) . ? P7 C69 1.870(14) . ? P8 C46 1.783(19) . ? P8 C45 1.818(14) . ? P8 C44 1.820(12) . ? C4 C5 1.408(14) . ? C4 C9 1.410(16) . ? C5 C6 1.374(18) . ? C6 C7 1.363(17) . ? C7 C8 1.365(14) . ? C8 C9 1.354(18) . ? C10 C11 1.386(14) . ? C10 C15 1.387(14) . ? C11 C12 1.390(13) . ? C12 C13 1.371(15) . ? C13 C14 1.343(15) . ? C14 C15 1.393(13) . ? C16 C17 1.409(13) . ? C16 C20 1.432(19) . ? C17 C18 1.40(2) . ? C18 C19 1.45(2) . ? C19 C20 1.414(17) . ? C21 C25 1.420(17) . ? C21 C22 1.458(14) . ? C22 C23 1.396(19) . ? C23 C24 1.433(15) . ? C24 C25 1.409(19) . ? C26 C31 1.365(17) . ? C26 C27 1.39(2) . ? C27 C28 1.380(18) . ? C28 C29 1.36(2) . ? C29 C30 1.35(2) . ? C30 C31 1.425(17) . ? C32 C37 1.34(2) . ? C32 C33 1.406(15) . ? C33 C34 1.37(2) . ? C34 C35 1.37(2) . ? C35 C36 1.406(16) . ? C36 C37 1.42(2) . ? C47 C48 1.29(2) . ? C47 C52 1.413(17) . ? C48 C49 1.399(16) . ? C49 C50 1.352(18) . ? C50 C51 1.32(2) . ? C51 C52 1.407(16) . ? C53 C58 1.369(14) . ? C53 C54 1.409(18) . ? C54 C55 1.38(2) . ? C55 C56 1.388(16) . ? C56 C57 1.35(2) . ? C57 C58 1.41(2) . ? C59 C63 1.41(2) . ? C59 C60 1.433(14) . ? C60 C61 1.46(2) . ? C61 C62 1.392(17) . ? C62 C63 1.39(2) . ? C64 C65 1.441(14) . ? C64 C68 1.448(16) . ? C65 C66 1.382(15) . ? C66 C67 1.394(16) . ? C67 C68 1.435(14) . ? C69 C74 1.372(18) . ? C69 C70 1.406(16) . ? C70 C71 1.343(19) . ? C71 C72 1.434(19) . ? C72 C73 1.358(17) . ? C73 C74 1.37(2) . ? C75 C76 1.379(18) . ? C75 C80 1.43(2) . ? C76 C77 1.421(16) . ? C77 C78 1.31(2) . ? C78 C79 1.34(2) . ? C79 C80 1.406(17) . ? 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 C24 Ni1 C21 67.1(5) . . ? C24 Ni1 C22 68.0(5) . . ? C21 Ni1 C22 41.3(4) . . ? C24 Ni1 C23 40.3(4) . . ? C21 Ni1 C23 66.4(5) . . ? C22 Ni1 C23 39.0(5) . . ? C24 Ni1 C25 39.5(5) . . ? C21 Ni1 C25 39.7(5) . . ? C22 Ni1 C25 67.9(5) . . ? C23 Ni1 C25 66.2(5) . . ? C24 Ni1 P2 168.1(5) . . ? C21 Ni1 P2 101.0(3) . . ? C22 Ni1 P2 103.2(3) . . ? C23 Ni1 P2 135.9(3) . . ? C25 Ni1 P2 130.8(4) . . ? C24 Ni1 P1 91.2(4) . . ? C21 Ni1 P1 151.8(3) . . ? C22 Ni1 P1 147.0(3) . . ? C23 Ni1 P1 109.0(4) . . ? C25 Ni1 P1 112.3(4) . . ? P2 Ni1 P1 100.14(13) . . ? C61 Ni2 C63 65.7(4) . . ? C61 Ni2 C62 39.4(5) . . ? C63 Ni2 C62 39.2(5) . . ? C61 Ni2 C59 66.3(5) . . ? C63 Ni2 C59 39.5(6) . . ? C62 Ni2 C59 66.4(6) . . ? C61 Ni2 P5 100.0(3) . . ? C63 Ni2 P5 165.8(3) . . ? C62 Ni2 P5 128.6(4) . . ? C59 Ni2 P5 137.2(4) . . ? C61 Ni2 C60 40.9(5) . . ? C63 Ni2 C60 67.1(5) . . ? C62 Ni2 C60 68.0(5) . . ? C59 Ni2 C60 39.6(4) . . ? P5 Ni2 C60 103.1(3) . . ? C61 Ni2 P6 153.0(4) . . ? C63 Ni2 P6 92.9(3) . . ? C62 Ni2 P6 113.6(4) . . ? C59 Ni2 P6 108.2(3) . . ? P5 Ni2 P6 100.47(11) . . ? C60 Ni2 P6 146.5(3) . . ? C18 Co1 C20 67.2(4) . . ? C18 Co1 C16 67.2(5) . . ? C20 Co1 C16 40.3(5) . . ? C18 Co1 C17 39.4(5) . . ? C20 Co1 C17 66.4(5) . . ? C16 Co1 C17 39.6(4) . . ? C18 Co1 C19 40.6(5) . . ? C20 Co1 C19 39.4(5) . . ? C16 Co1 C19 67.2(5) . . ? C17 Co1 C19 66.6(5) . . ? C18 Co1 P4 164.3(4) . . ? C20 Co1 P4 97.6(3) . . ? C16 Co1 P4 103.9(3) . . ? C17 Co1 P4 139.2(3) . . ? C19 Co1 P4 124.7(4) . . ? C18 Co1 P3 92.2(3) . . ? C20 Co1 P3 156.0(3) . . ? C16 Co1 P3 143.5(3) . . ? C17 Co1 P3 105.9(3) . . ? C19 Co1 P3 116.6(3) . . ? P4 Co1 P3 101.75(11) . . ? C65 Co2 C67 66.3(5) . . ? C65 Co2 C68 66.9(5) . . ? C67 Co2 C68 40.5(4) . . ? C65 Co2 C66 38.8(4) . . ? C67 Co2 C66 39.0(4) . . ? C68 Co2 C66 66.3(4) . . ? C65 Co2 C64 40.5(4) . . ? C67 Co2 C64 67.8(5) . . ? C68 Co2 C64 40.2(4) . . ? C66 Co2 C64 66.7(4) . . ? C65 Co2 P7 99.7(3) . . ? C67 Co2 P7 165.9(4) . . ? C68 Co2 P7 137.2(3) . . ? C66 Co2 P7 128.2(3) . . ? C64 Co2 P7 103.0(3) . . ? C65 Co2 P8 153.2(3) . . ? C67 Co2 P8 91.3(4) . . ? C68 Co2 P8 106.0(4) . . ? C66 Co2 P8 114.4(4) . . ? C64 Co2 P8 144.9(3) . . ? P7 Co2 P8 101.78(15) . . ? C3 P1 C1 100.9(8) . . ? C3 P1 C2 99.6(7) . . ? C1 P1 C2 98.0(7) . . ? C3 P1 Ni1 115.3(6) . . ? C1 P1 Ni1 124.6(5) . . ? C2 P1 Ni1 114.4(6) . . ? C16 P2 C4 99.8(5) . . ? C16 P2 C10 98.9(5) . . ? C4 P2 C10 101.6(5) . . ? C16 P2 Ni1 119.4(4) . . ? C4 P2 Ni1 116.1(3) . . ? C10 P2 Ni1 117.7(3) . . ? C40 P3 C38 111.5(9) . . ? C40 P3 C39 83.9(12) . . ? C38 P3 C39 91.7(10) . . ? C40 P3 Co1 116.5(7) . . ? C38 P3 Co1 127.7(6) . . ? C39 P3 Co1 112.4(6) . . ? C26 P4 C22 98.6(5) . . ? C26 P4 C32 102.4(6) . . ? C22 P4 C32 98.2(6) . . ? C26 P4 Co1 118.4(4) . . ? C22 P4 Co1 118.6(3) . . ? C32 P4 Co1 117.1(4) . . ? C64 P5 C53 97.8(5) . . ? C64 P5 C47 97.8(5) . . ? C53 P5 C47 104.4(6) . . ? C64 P5 Ni2 118.6(4) . . ? C53 P5 Ni2 118.3(4) . . ? C47 P5 Ni2 116.5(4) . . ? C43 P6 C41 102.1(7) . . ? C43 P6 C42 99.0(8) . . ? C41 P6 C42 98.5(8) . . ? C43 P6 Ni2 113.9(5) . . ? C41 P6 Ni2 115.0(4) . . ? C42 P6 Ni2 124.9(4) . . ? C60 P7 C75 99.0(6) . . ? C60 P7 C69 97.5(6) . . ? C75 P7 C69 100.5(6) . . ? C60 P7 Co2 118.5(4) . . ? C75 P7 Co2 117.0(4) . . ? C69 P7 Co2 120.2(4) . . ? C46 P8 C45 100.6(9) . . ? C46 P8 C44 98.3(8) . . ? C45 P8 C44 100.1(7) . . ? C46 P8 Co2 124.7(5) . . ? C45 P8 Co2 114.9(6) . . ? C44 P8 Co2 114.3(7) . . ? C5 C4 C9 117.2(11) . . ? C5 C4 P2 116.7(8) . . ? C9 C4 P2 126.1(8) . . ? C6 C5 C4 119.6(10) . . ? C7 C6 C5 121.8(10) . . ? C6 C7 C8 119.2(13) . . ? C9 C8 C7 121.2(11) . . ? C8 C9 C4 121.0(10) . . ? C11 C10 C15 118.7(9) . . ? C11 C10 P2 122.5(8) . . ? C15 C10 P2 118.9(7) . . ? C10 C11 C12 120.4(10) . . ? C13 C12 C11 119.0(10) . . ? C14 C13 C12 122.1(10) . . ? C13 C14 C15 119.3(10) . . ? C10 C15 C14 120.6(9) . . ? C17 C16 C20 106.6(11) . . ? C17 C16 P2 126.6(11) . . ? C20 C16 P2 126.6(8) . . ? C17 C16 Co1 70.3(6) . . ? C20 C16 Co1 69.7(7) . . ? P2 C16 Co1 128.7(5) . . ? C18 C17 C16 109.7(12) . . ? C18 C17 Co1 69.6(7) . . ? C16 C17 Co1 70.1(6) . . ? C17 C18 C19 108.0(11) . . ? C17 C18 Co1 71.0(6) . . ? C19 C18 Co1 71.6(6) . . ? C20 C19 C18 106.1(14) . . ? C20 C19 Co1 68.8(6) . . ? C18 C19 Co1 67.8(7) . . ? C19 C20 C16 109.5(11) . . ? C19 C20 Co1 71.8(6) . . ? C16 C20 Co1 70.0(6) . . ? C25 C21 C22 109.0(11) . . ? C25 C21 Ni1 72.3(9) . . ? C22 C21 Ni1 69.8(8) . . ? C23 C22 C21 106.1(10) . . ? C23 C22 P4 130.0(8) . . ? C21 C22 P4 122.9(10) . . ? C23 C22 Ni1 71.6(8) . . ? C21 C22 Ni1 69.0(7) . . ? P4 C22 Ni1 132.6(6) . . ? C22 C23 C24 109.2(10) . . ? C22 C23 Ni1 69.4(6) . . ? C24 C23 Ni1 67.8(6) . . ? C25 C24 C23 108.5(12) . . ? C25 C24 Ni1 72.9(6) . . ? C23 C24 Ni1 71.8(6) . . ? C24 C25 C21 106.9(10) . . ? C24 C25 Ni1 67.6(7) . . ? C21 C25 Ni1 68.0(7) . . ? C31 C26 C27 118.6(12) . . ? C31 C26 P4 125.0(13) . . ? C27 C26 P4 116.4(9) . . ? C28 C27 C26 123.0(13) . . ? C29 C28 C27 117.9(17) . . ? C30 C29 C28 121.2(13) . . ? C29 C30 C31 121.1(13) . . ? C26 C31 C30 118.2(15) . . ? C37 C32 C33 118.9(14) . . ? C37 C32 P4 119.6(9) . . ? C33 C32 P4 121.5(11) . . ? C34 C33 C32 120.9(14) . . ? C35 C34 C33 119.6(13) . . ? C34 C35 C36 121.3(15) . . ? C35 C36 C37 116.8(14) . . ? C32 C37 C36 122.2(12) . . ? C48 C47 C52 119.3(11) . . ? C48 C47 P5 118.0(9) . . ? C52 C47 P5 122.6(11) . . ? C47 C48 C49 123.6(12) . . ? C50 C49 C48 116.7(15) . . ? C51 C50 C49 122.4(12) . . ? C50 C51 C52 120.6(12) . . ? C51 C52 C47 117.2(14) . . ? C58 C53 C54 117.7(13) . . ? C58 C53 P5 123.8(10) . . ? C54 C53 P5 118.3(9) . . ? C55 C54 C53 121.4(12) . . ? C54 C55 C56 119.8(13) . . ? C57 C56 C55 119.2(15) . . ? C56 C57 C58 121.6(12) . . ? C53 C58 C57 120.2(12) . . ? C63 C59 C60 109.0(13) . . ? C63 C59 Ni2 68.8(8) . . ? C60 C59 Ni2 70.9(7) . . ? C59 C60 C61 103.5(11) . . ? C59 C60 P7 126.7(11) . . ? C61 C60 P7 129.6(8) . . ? C59 C60 Ni2 69.4(7) . . ? C61 C60 Ni2 66.9(7) . . ? P7 C60 Ni2 130.3(5) . . ? C62 C61 C60 110.8(11) . . ? C62 C61 Ni2 71.3(6) . . ? C60 C61 Ni2 72.2(7) . . ? C63 C62 C61 106.8(14) . . ? C63 C62 Ni2 69.9(7) . . ? C61 C62 Ni2 69.3(7) . . ? C62 C63 C59 109.8(11) . . ? C62 C63 Ni2 70.9(6) . . ? C59 C63 Ni2 71.7(7) . . ? C65 C64 C68 104.3(9) . . ? C65 C64 P5 129.6(9) . . ? C68 C64 P5 126.1(8) . . ? C65 C64 Co2 67.0(7) . . ? C68 C64 Co2 69.0(8) . . ? P5 C64 Co2 129.9(6) . . ? C66 C65 C64 111.1(10) . . ? C66 C65 Co2 73.5(9) . . ? C64 C65 Co2 72.5(8) . . ? C65 C66 C67 107.7(9) . . ? C65 C66 Co2 67.7(7) . . ? C67 C66 Co2 68.2(7) . . ? C66 C67 C68 108.8(10) . . ? C66 C67 Co2 72.8(6) . . ? C68 C67 Co2 71.1(6) . . ? C67 C68 C64 107.8(9) . . ? C67 C68 Co2 68.4(6) . . ? C64 C68 Co2 70.8(6) . . ? C74 C69 C70 120.1(13) . . ? C74 C69 P7 125.4(10) . . ? C70 C69 P7 114.4(9) . . ? C71 C70 C69 119.6(12) . . ? C70 C71 C72 120.4(12) . . ? C73 C72 C71 118.3(13) . . ? C72 C73 C74 121.6(13) . . ? C73 C74 C69 119.9(12) . . ? C76 C75 C80 119.3(11) . . ? C76 C75 P7 123.8(10) . . ? C80 C75 P7 116.7(10) . . ? C75 C76 C77 120.0(14) . . ? C78 C77 C76 119.5(15) . . ? C77 C78 C79 122.8(13) . . ? C78 C79 C80 122.0(15) . . ? C79 C80 C75 116.3(14) . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.333 0.877 0.227 225 29 ' ' 2 0.667 0.377 0.272 225 29 ' ' 3 0.826 0.823 0.095 7 1 ' ' 4 0.849 0.733 0.180 8 -1 ' ' 5 0.152 0.235 0.321 9 -1 ' ' 6 0.175 0.325 0.406 7 1 ' ' 7 0.333 0.623 0.727 225 30 ' ' 8 0.667 0.123 0.772 225 30 ' ' 9 0.826 0.677 0.595 7 1 ' ' 10 0.849 0.766 0.680 9 -1 ' ' 11 0.152 0.265 0.821 9 -1 ' ' 12 0.175 0.175 0.906 7 1 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.848 _diffrn_reflns_theta_full 25.66 _diffrn_measured_fraction_theta_full 0.848 _refine_diff_density_max 0.654 _refine_diff_density_min -0.578 _refine_diff_density_rms 0.101 # Attachment '- 6.cif' data_6 _database_code_depnum_ccdc_archive 'CCDC 780555' #TrackingRef '- 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H52 Co Fe P4' _chemical_formula_sum 'C42 H52 Co Fe P4' _chemical_formula_weight 795.50 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.816(6) _cell_length_b 16.502(9) _cell_length_c 20.416(11) _cell_angle_alpha 90.00 _cell_angle_beta 103.579(11) _cell_angle_gamma 90.00 _cell_volume 3870(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 553 _cell_measurement_theta_min 2.21 _cell_measurement_theta_max 16.51 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.365 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1668 _exptl_absorpt_coefficient_mu 0.998 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7472 _exptl_absorpt_correction_T_max 0.7814 _exptl_absorpt_process_details ? _exptl_special_details ; Theta(max) is low. The reason is that the quality of the crystal is not very good, and the diffraction data is relatively weak. ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16369 _diffrn_reflns_av_R_equivalents 0.2145 _diffrn_reflns_av_sigmaI/netI 0.2450 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.60 _diffrn_reflns_theta_max 23.32 _reflns_number_total 5590 _reflns_number_gt 2128 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. 252 restrains were used for ' Large Non-Solvent C Ueq(max)/Ueq(min)' ; _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^)+(0.1102P)^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 5590 _refine_ls_number_parameters 436 _refine_ls_number_restraints 252 _refine_ls_R_factor_all 0.2410 _refine_ls_R_factor_gt 0.0970 _refine_ls_wR_factor_ref 0.2803 _refine_ls_wR_factor_gt 0.2087 _refine_ls_goodness_of_fit_ref 0.985 _refine_ls_restrained_S_all 0.984 _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 C1 C 0.7996(12) 0.4232(8) 0.3414(7) 0.045(4) Uani 1 1 d U . . C2 C 0.8605(12) 0.4026(8) 0.4056(7) 0.054(4) Uani 1 1 d U . . H2 H 0.8228 0.3757 0.4344 0.065 Uiso 1 1 calc R . . C3 C 0.9784(14) 0.4219(9) 0.4273(9) 0.071(5) Uani 1 1 d U . . H3 H 1.0190 0.4071 0.4704 0.085 Uiso 1 1 calc R . . C4 C 1.0349(14) 0.4626(9) 0.3858(9) 0.071(5) Uani 1 1 d U . . H4 H 1.1122 0.4780 0.4015 0.085 Uiso 1 1 calc R . . C5 C 0.9770(13) 0.4803(9) 0.3212(8) 0.069(5) Uani 1 1 d U . . H5 H 1.0162 0.5049 0.2920 0.083 Uiso 1 1 calc R . . C6 C 0.8596(12) 0.4616(8) 0.2992(8) 0.056(4) Uani 1 1 d U . . H6 H 0.8205 0.4749 0.2554 0.067 Uiso 1 1 calc R . . C7 C 0.3419(12) 0.5669(8) 0.1448(7) 0.046(4) Uani 1 1 d U . . C8 C 0.4174(13) 0.5995(9) 0.1119(7) 0.065(5) Uani 1 1 d U . . H8 H 0.4762 0.5670 0.1028 0.077 Uiso 1 1 calc R . . C9 C 0.4105(15) 0.6803(11) 0.0910(9) 0.086(6) Uani 1 1 d U . . H9 H 0.4594 0.6994 0.0648 0.103 Uiso 1 1 calc R . . C10 C 0.3316(16) 0.7319(11) 0.1092(9) 0.088(6) Uani 1 1 d U . . H10 H 0.3317 0.7868 0.0989 0.105 Uiso 1 1 calc R . . C11 C 0.2523(15) 0.7014(10) 0.1429(8) 0.077(5) Uani 1 1 d U . . H11 H 0.1973 0.7354 0.1545 0.092 Uiso 1 1 calc R . . C12 C 0.2551(13) 0.6194(9) 0.1595(7) 0.063(4) Uani 1 1 d U . . H12 H 0.1996 0.5985 0.1805 0.075 Uiso 1 1 calc R . . C13 C 0.1909(11) 0.4366(7) 0.1472(7) 0.042(4) Uani 1 1 d U . . C14 C 0.1340(13) 0.4036(9) 0.1927(8) 0.061(4) Uani 1 1 d U . . H14 H 0.1738 0.3945 0.2371 0.074 Uiso 1 1 calc R . . C15 C 0.0139(15) 0.3837(10) 0.1711(10) 0.081(5) Uani 1 1 d U . . H15 H -0.0258 0.3643 0.2022 0.097 Uiso 1 1 calc R . . C16 C -0.0425(15) 0.3925(10) 0.1066(10) 0.075(5) Uani 1 1 d U . . H16 H -0.1208 0.3784 0.0932 0.091 Uiso 1 1 calc R . . C17 C 0.0119(15) 0.4214(10) 0.0609(9) 0.076(5) Uani 1 1 d U . . H17 H -0.0279 0.4240 0.0159 0.091 Uiso 1 1 calc R . . C18 C 0.1296(14) 0.4484(9) 0.0799(9) 0.071(5) Uani 1 1 d U . . H18 H 0.1649 0.4729 0.0488 0.085 Uiso 1 1 calc R . . C19 C 0.6207(11) 0.4411(8) 0.1189(7) 0.045(4) Uani 1 1 d U . . H19 H 0.6179 0.4784 0.0813 0.055 Uiso 1 1 calc R . . C20 C 0.6112(10) 0.4630(7) 0.1840(6) 0.036(3) Uani 1 1 d U . . H20 H 0.6007 0.5184 0.1988 0.044 Uiso 1 1 calc R . . C21 C 0.6216(10) 0.3934(7) 0.2253(6) 0.032(3) Uani 1 1 d U . . C22 C 0.6376(10) 0.3267(8) 0.1828(7) 0.044(4) Uani 1 1 d U . . H22 H 0.6473 0.2698 0.1968 0.052 Uiso 1 1 calc R . . C23 C 0.6372(11) 0.3568(8) 0.1174(7) 0.049(4) Uani 1 1 d U . . H23 H 0.6473 0.3248 0.0787 0.059 Uiso 1 1 calc R . . C24 C 0.3681(10) 0.4703(7) 0.2616(6) 0.034(3) Uani 1 1 d U . . C25 C 0.3582(11) 0.5377(8) 0.3059(7) 0.046(4) Uani 1 1 d U . . H25 H 0.3510 0.5948 0.2922 0.055 Uiso 1 1 calc R . . C26 C 0.3593(11) 0.5093(9) 0.3704(8) 0.056(4) Uani 1 1 d U . . H26 H 0.3512 0.5422 0.4090 0.068 Uiso 1 1 calc R . . C27 C 0.3708(11) 0.4242(9) 0.3693(7) 0.052(4) Uani 1 1 d U . . H27 H 0.3733 0.3881 0.4077 0.062 Uiso 1 1 calc R . . C28 C 0.3815(11) 0.3995(8) 0.3052(7) 0.044(4) Uani 1 1 d U . . H28 H 0.3906 0.3435 0.2914 0.053 Uiso 1 1 calc R . . C29 C 0.3809(18) 0.2083(12) 0.1981(9) 0.118(7) Uani 1 1 d U . . H29A H 0.4559 0.2079 0.2290 0.177 Uiso 1 1 calc R . . H29B H 0.3591 0.1538 0.1839 0.177 Uiso 1 1 calc R . . H29C H 0.3243 0.2308 0.2198 0.177 Uiso 1 1 calc R . . C30 C 0.4582(13) 0.1992(9) 0.0793(8) 0.072(5) Uani 1 1 d U . . H30A H 0.4678 0.2239 0.0384 0.109 Uiso 1 1 calc R . . H30B H 0.4113 0.1513 0.0687 0.109 Uiso 1 1 calc R . . H30C H 0.5332 0.1848 0.1068 0.109 Uiso 1 1 calc R . . C31 C 0.2392(16) 0.2595(12) 0.0772(10) 0.138(8) Uani 1 1 d U . . H31A H 0.2287 0.2892 0.0358 0.208 Uiso 1 1 calc R . . H31B H 0.1877 0.2806 0.1031 0.208 Uiso 1 1 calc R . . H31C H 0.2220 0.2033 0.0675 0.208 Uiso 1 1 calc R . . C32 C 0.627(2) 0.6560(14) 0.3038(11) 0.155(9) Uani 1 1 d U . . H32A H 0.5553 0.6583 0.2700 0.233 Uiso 1 1 calc R . . H32B H 0.6878 0.6359 0.2841 0.233 Uiso 1 1 calc R . . H32C H 0.6470 0.7093 0.3216 0.233 Uiso 1 1 calc R . . C33 C 0.7521(18) 0.5952(14) 0.4260(11) 0.156(9) Uani 1 1 d U . . H33A H 0.8070 0.5680 0.4056 0.235 Uiso 1 1 calc R . . H33B H 0.7518 0.5700 0.4683 0.235 Uiso 1 1 calc R . . H33C H 0.7739 0.6511 0.4333 0.235 Uiso 1 1 calc R . . C34 C 0.5411(15) 0.6624(10) 0.4170(9) 0.096(6) Uani 1 1 d U . . H34A H 0.5219 0.6365 0.4550 0.145 Uiso 1 1 calc R . . H34B H 0.4715 0.6829 0.3875 0.145 Uiso 1 1 calc R . . H34C H 0.5940 0.7063 0.4322 0.145 Uiso 1 1 calc R . . C35 C 0.6499(12) 0.2918(8) 0.3421(6) 0.041(4) Uani 1 1 d U . . C36 C 0.7331(13) 0.2418(8) 0.3265(7) 0.057(4) Uani 1 1 d U . . H36 H 0.7868 0.2617 0.3037 0.068 Uiso 1 1 calc R . . C37 C 0.5747(12) 0.2613(9) 0.3785(7) 0.058(4) Uani 1 1 d U . . H37 H 0.5232 0.2964 0.3923 0.070 Uiso 1 1 calc R . . C38 C 0.7353(15) 0.1599(10) 0.3458(8) 0.070(5) Uani 1 1 d U . . H38 H 0.7926 0.1262 0.3365 0.083 Uiso 1 1 calc R . . C39 C 0.6564(15) 0.1286(9) 0.3776(8) 0.074(5) Uani 1 1 d U . . H39 H 0.6580 0.0735 0.3874 0.089 Uiso 1 1 calc R . . C40 C 0.5737(15) 0.1775(10) 0.3954(9) 0.081(5) Uani 1 1 d U . . H40 H 0.5196 0.1567 0.4175 0.097 Uiso 1 1 calc R . . C50 C 0.3974(17) 0.4047(12) 0.0403(9) 0.119(7) Uani 1 1 d U . . H50A H 0.3786 0.4612 0.0336 0.179 Uiso 1 1 calc R . . H50B H 0.3274 0.3732 0.0280 0.179 Uiso 1 1 calc R . . H50C H 0.4495 0.3892 0.0129 0.179 Uiso 1 1 calc R . . C51 C 0.5993(19) 0.4535(15) 0.4478(11) 0.160(10) Uani 1 1 d U . . H51A H 0.5505 0.4713 0.4766 0.240 Uiso 1 1 calc R . . H51B H 0.6722 0.4819 0.4595 0.240 Uiso 1 1 calc R . . H51C H 0.6130 0.3964 0.4536 0.240 Uiso 1 1 calc R . . Co1 Co 0.51522(16) 0.47822(11) 0.34531(10) 0.0471(6) Uani 1 1 d . . . Fe1 Fe 0.47784(16) 0.38419(11) 0.14241(10) 0.0395(6) Uani 1 1 d . . . P3 P 0.6426(3) 0.4005(2) 0.31623(18) 0.0380(10) Uani 1 1 d . . . P4 P 0.3501(3) 0.4609(2) 0.17276(19) 0.0391(10) Uani 1 1 d . . . P5 P 0.3875(3) 0.2697(2) 0.1246(2) 0.0548(12) Uani 1 1 d . . . P6 P 0.6100(4) 0.5887(2) 0.3714(2) 0.0640(14) 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 C1 0.044(7) 0.043(7) 0.045(8) -0.006(6) 0.002(6) 0.005(6) C2 0.043(7) 0.060(8) 0.057(8) 0.003(6) 0.009(6) -0.005(6) C3 0.069(8) 0.067(8) 0.070(9) 0.002(7) 0.000(7) -0.001(7) C4 0.056(8) 0.071(8) 0.080(9) -0.005(7) 0.007(7) -0.014(7) C5 0.064(8) 0.075(8) 0.073(9) 0.000(7) 0.026(7) -0.011(7) C6 0.046(7) 0.061(8) 0.060(8) 0.004(6) 0.013(7) -0.010(6) C7 0.042(7) 0.043(7) 0.053(8) 0.006(6) 0.013(6) -0.003(6) C8 0.066(8) 0.056(8) 0.079(9) 0.020(7) 0.032(7) 0.013(7) C9 0.084(9) 0.083(9) 0.098(9) 0.016(8) 0.035(8) 0.017(8) C10 0.097(9) 0.071(9) 0.099(9) 0.020(7) 0.031(8) 0.010(8) C11 0.078(8) 0.065(8) 0.093(9) 0.002(7) 0.032(7) 0.024(7) C12 0.066(8) 0.058(8) 0.070(8) 0.012(7) 0.028(7) 0.013(7) C13 0.033(7) 0.036(6) 0.054(8) 0.001(6) 0.007(6) 0.001(5) C14 0.057(8) 0.072(8) 0.059(8) -0.013(7) 0.020(7) -0.009(7) C15 0.077(9) 0.081(9) 0.089(9) -0.002(7) 0.030(8) -0.012(7) C16 0.065(8) 0.076(9) 0.083(9) -0.012(8) 0.015(8) -0.001(7) C17 0.067(8) 0.077(9) 0.076(9) -0.004(7) 0.003(7) 0.004(7) C18 0.062(8) 0.072(8) 0.071(9) -0.001(7) 0.000(7) -0.004(7) C19 0.044(7) 0.047(7) 0.050(8) 0.006(6) 0.020(6) 0.001(6) C20 0.036(6) 0.032(6) 0.038(7) -0.004(5) 0.001(6) -0.003(5) C21 0.027(6) 0.026(6) 0.041(7) 0.006(5) 0.004(5) 0.003(5) C22 0.038(7) 0.048(7) 0.041(7) 0.003(6) 0.002(6) 0.010(6) C23 0.042(7) 0.058(7) 0.049(8) 0.000(6) 0.014(6) 0.006(6) C24 0.027(6) 0.028(6) 0.045(7) 0.006(5) 0.005(5) -0.001(5) C25 0.039(7) 0.049(7) 0.049(8) -0.009(6) 0.009(6) 0.007(6) C26 0.045(7) 0.072(8) 0.055(8) -0.002(7) 0.018(6) 0.006(6) C27 0.043(7) 0.065(8) 0.050(8) 0.009(6) 0.016(6) -0.006(6) C28 0.040(7) 0.038(7) 0.056(8) -0.004(6) 0.015(6) -0.006(6) C29 0.140(11) 0.107(10) 0.114(10) 0.003(8) 0.044(8) -0.028(8) C30 0.068(8) 0.065(8) 0.083(9) -0.017(7) 0.014(7) -0.012(7) C31 0.121(11) 0.122(11) 0.163(12) -0.015(9) 0.016(9) -0.006(9) C32 0.176(13) 0.144(12) 0.159(12) -0.008(9) 0.066(9) -0.023(9) C33 0.143(12) 0.138(12) 0.177(13) -0.032(9) 0.015(9) -0.002(9) C34 0.097(9) 0.100(9) 0.097(9) -0.020(8) 0.030(8) -0.001(8) C35 0.047(7) 0.040(7) 0.035(7) 0.001(6) 0.006(6) -0.008(6) C36 0.069(8) 0.044(7) 0.054(8) 0.010(6) 0.005(7) 0.008(7) C37 0.050(7) 0.061(8) 0.063(8) 0.010(7) 0.011(7) 0.005(6) C38 0.076(8) 0.061(8) 0.070(8) -0.003(7) 0.015(7) 0.029(7) C39 0.081(9) 0.045(8) 0.091(9) 0.005(7) 0.009(7) -0.001(7) C40 0.076(9) 0.073(9) 0.096(9) 0.027(7) 0.027(7) -0.015(7) C50 0.115(10) 0.126(11) 0.117(11) -0.001(8) 0.030(8) -0.004(8) C51 0.158(13) 0.169(13) 0.157(13) -0.005(9) 0.045(9) -0.012(9) Co1 0.0399(12) 0.0407(12) 0.0624(16) -0.0040(10) 0.0152(11) 0.0004(10) Fe1 0.0315(12) 0.0329(11) 0.0540(15) -0.0014(10) 0.0101(10) 0.0004(9) P3 0.036(2) 0.031(2) 0.047(3) 0.0003(17) 0.0093(19) -0.0039(17) P4 0.033(2) 0.039(2) 0.045(3) 0.0051(18) 0.0083(19) 0.0013(17) P5 0.050(3) 0.044(3) 0.071(3) -0.012(2) 0.017(2) -0.006(2) P6 0.046(3) 0.053(3) 0.095(4) -0.024(2) 0.021(3) -0.010(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.382(17) . ? C1 C6 1.390(18) . ? C1 P3 1.843(14) . ? C2 C3 1.396(18) . ? C2 H2 0.9300 . ? C3 C4 1.37(2) . ? C3 H3 0.9300 . ? C4 C5 1.368(19) . ? C4 H4 0.9300 . ? C5 C6 1.389(18) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C8 1.348(17) . ? C7 C12 1.427(18) . ? C7 P4 1.835(13) . ? C8 C9 1.40(2) . ? C8 H8 0.9300 . ? C9 C10 1.38(2) . ? C9 H9 0.9300 . ? C10 C11 1.38(2) . ? C10 H10 0.9300 . ? C11 C12 1.395(19) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.380(18) . ? C13 C18 1.409(18) . ? C13 P4 1.874(13) . ? C14 C15 1.422(19) . ? C14 H14 0.9300 . ? C15 C16 1.337(19) . ? C15 H15 0.9300 . ? C16 C17 1.34(2) . ? C16 H16 0.9300 . ? C17 C18 1.42(2) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C23 1.406(17) . ? C19 C20 1.407(16) . ? C19 Fe1 2.083(13) . ? C19 H19 0.9800 . ? C20 C21 1.413(15) . ? C20 Fe1 2.066(12) . ? C20 H20 0.9800 . ? C21 C22 1.440(16) . ? C21 P3 1.817(12) . ? C21 Fe1 2.103(12) . ? C22 C23 1.425(17) . ? C22 Fe1 2.100(12) . ? C22 H22 0.9800 . ? C23 Fe1 2.112(13) . ? C23 H23 0.9800 . ? C24 C28 1.455(16) . ? C24 C25 1.455(16) . ? C24 P4 1.782(13) . ? C24 Co1 2.137(12) . ? C25 C26 1.396(18) . ? C25 Co1 2.086(13) . ? C25 H25 0.9800 . ? C26 C27 1.412(18) . ? C26 Co1 2.089(14) . ? C26 H26 0.9800 . ? C27 C28 1.403(17) . ? C27 Co1 2.082(14) . ? C27 H27 0.9800 . ? C28 Co1 2.060(12) . ? C28 H28 0.9800 . ? C29 P5 1.827(18) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 P5 1.809(15) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 P5 1.800(18) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 P6 1.82(2) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 P6 1.79(2) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 P6 1.832(16) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.378(17) . ? C35 C37 1.380(17) . ? C35 P3 1.866(13) . ? C36 C38 1.406(19) . ? C36 H36 0.9300 . ? C37 C40 1.426(19) . ? C37 H37 0.9300 . ? C38 C39 1.36(2) . ? C38 H38 0.9300 . ? C39 C40 1.38(2) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? C50 Fe1 2.105(18) . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 Co1 2.13(2) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? Co1 P6 2.141(4) . ? Co1 P3 2.165(4) . ? Fe1 P5 2.158(4) . ? Fe1 P4 2.169(4) . ? 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 C2 C1 C6 118.2(13) . . ? C2 C1 P3 118.6(11) . . ? C6 C1 P3 123.1(11) . . ? C1 C2 C3 120.2(15) . . ? C1 C2 H2 119.9 . . ? C3 C2 H2 119.9 . . ? C4 C3 C2 120.7(16) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C5 C4 C3 119.6(16) . . ? C5 C4 H4 120.2 . . ? C3 C4 H4 120.2 . . ? C4 C5 C6 120.0(16) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C5 C6 C1 121.1(15) . . ? C5 C6 H6 119.5 . . ? C1 C6 H6 119.5 . . ? C8 C7 C12 117.0(14) . . ? C8 C7 P4 122.9(12) . . ? C12 C7 P4 120.0(11) . . ? C7 C8 C9 122.3(16) . . ? C7 C8 H8 118.8 . . ? C9 C8 H8 118.8 . . ? C10 C9 C8 120.2(17) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C9 C10 C11 119.4(17) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C10 C11 C12 119.6(16) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C11 C12 C7 121.1(15) . . ? C11 C12 H12 119.5 . . ? C7 C12 H12 119.5 . . ? C14 C13 C18 119.4(13) . . ? C14 C13 P4 120.9(11) . . ? C18 C13 P4 119.7(11) . . ? C13 C14 C15 119.4(15) . . ? C13 C14 H14 120.3 . . ? C15 C14 H14 120.3 . . ? C16 C15 C14 120.7(17) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C17 121.0(18) . . ? C15 C16 H16 119.5 . . ? C17 C16 H16 119.5 . . ? C16 C17 C18 121.4(18) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C13 C18 C17 117.9(16) . . ? C13 C18 H18 121.0 . . ? C17 C18 H18 121.0 . . ? C23 C19 C20 108.5(12) . . ? C23 C19 Fe1 71.6(8) . . ? C20 C19 Fe1 69.5(7) . . ? C23 C19 H19 125.7 . . ? C20 C19 H19 125.7 . . ? Fe1 C19 H19 125.7 . . ? C19 C20 C21 109.9(11) . . ? C19 C20 Fe1 70.8(7) . . ? C21 C20 Fe1 71.6(7) . . ? C19 C20 H20 125.1 . . ? C21 C20 H20 125.1 . . ? Fe1 C20 H20 125.1 . . ? C20 C21 C22 105.5(11) . . ? C20 C21 P3 121.9(9) . . ? C22 C21 P3 131.2(9) . . ? C20 C21 Fe1 68.8(7) . . ? C22 C21 Fe1 69.8(7) . . ? P3 C21 Fe1 135.8(7) . . ? C23 C22 C21 109.1(12) . . ? C23 C22 Fe1 70.7(7) . . ? C21 C22 Fe1 70.1(7) . . ? C23 C22 H22 125.5 . . ? C21 C22 H22 125.5 . . ? Fe1 C22 H22 125.5 . . ? C19 C23 C22 107.1(13) . . ? C19 C23 Fe1 69.3(8) . . ? C22 C23 Fe1 69.8(8) . . ? C19 C23 H23 126.5 . . ? C22 C23 H23 126.5 . . ? Fe1 C23 H23 126.5 . . ? C28 C24 C25 104.2(11) . . ? C28 C24 P4 121.6(9) . . ? C25 C24 P4 133.7(10) . . ? C28 C24 Co1 66.9(7) . . ? C25 C24 Co1 68.0(7) . . ? P4 C24 Co1 134.4(7) . . ? C26 C25 C24 110.2(13) . . ? C26 C25 Co1 70.6(8) . . ? C24 C25 Co1 71.7(7) . . ? C26 C25 H25 124.9 . . ? C24 C25 H25 124.9 . . ? Co1 C25 H25 124.9 . . ? C25 C26 C27 107.3(14) . . ? C25 C26 Co1 70.4(8) . . ? C27 C26 Co1 70.0(8) . . ? C25 C26 H26 126.3 . . ? C27 C26 H26 126.3 . . ? Co1 C26 H26 126.3 . . ? C28 C27 C26 109.5(13) . . ? C28 C27 Co1 69.4(8) . . ? C26 C27 Co1 70.5(8) . . ? C28 C27 H27 125.2 . . ? C26 C27 H27 125.2 . . ? Co1 C27 H27 125.2 . . ? C27 C28 C24 108.5(12) . . ? C27 C28 Co1 71.1(8) . . ? C24 C28 Co1 72.6(7) . . ? C27 C28 H28 125.7 . . ? C24 C28 H28 125.7 . . ? Co1 C28 H28 125.7 . . ? P5 C29 H29A 109.5 . . ? P5 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? P5 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? P5 C30 H30A 109.5 . . ? P5 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? P5 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? P5 C31 H31A 109.5 . . ? P5 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? P5 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? P6 C32 H32A 109.5 . . ? P6 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? P6 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? P6 C33 H33A 109.5 . . ? P6 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? P6 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? P6 C34 H34A 109.5 . . ? P6 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? P6 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C37 119.4(13) . . ? C36 C35 P3 119.9(11) . . ? C37 C35 P3 120.7(11) . . ? C35 C36 C38 118.5(15) . . ? C35 C36 H36 120.7 . . ? C38 C36 H36 120.7 . . ? C35 C37 C40 121.8(15) . . ? C35 C37 H37 119.1 . . ? C40 C37 H37 119.1 . . ? C39 C38 C36 122.1(16) . . ? C39 C38 H38 118.9 . . ? C36 C38 H38 118.9 . . ? C38 C39 C40 120.7(16) . . ? C38 C39 H39 119.6 . . ? C40 C39 H39 119.6 . . ? C39 C40 C37 117.2(16) . . ? C39 C40 H40 121.4 . . ? C37 C40 H40 121.4 . . ? Fe1 C50 H50A 109.5 . . ? Fe1 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? Fe1 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? Co1 C51 H51A 109.5 . . ? Co1 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? Co1 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C28 Co1 C27 39.6(5) . . ? C28 Co1 C25 67.3(5) . . ? C27 Co1 C25 65.7(6) . . ? C28 Co1 C26 67.3(6) . . ? C27 Co1 C26 39.6(5) . . ? C25 Co1 C26 39.1(5) . . ? C28 Co1 C51 114.0(7) . . ? C27 Co1 C51 84.6(7) . . ? C25 Co1 C51 129.4(7) . . ? C26 Co1 C51 92.3(7) . . ? C28 Co1 C24 40.5(4) . . ? C27 Co1 C24 66.7(5) . . ? C25 Co1 C24 40.3(4) . . ? C26 Co1 C24 67.2(5) . . ? C51 Co1 C24 151.2(7) . . ? C28 Co1 P6 160.6(4) . . ? C27 Co1 P6 135.7(4) . . ? C25 Co1 P6 93.5(4) . . ? C26 Co1 P6 99.7(4) . . ? C51 Co1 P6 79.8(7) . . ? C24 Co1 P6 122.1(3) . . ? C28 Co1 P3 92.0(4) . . ? C27 Co1 P3 118.1(4) . . ? C25 Co1 P3 141.8(4) . . ? C26 Co1 P3 157.4(4) . . ? C51 Co1 P3 87.8(7) . . ? C24 Co1 P3 103.4(4) . . ? P6 Co1 P3 102.51(17) . . ? C20 Fe1 C19 39.7(5) . . ? C20 Fe1 C22 66.1(5) . . ? C19 Fe1 C22 65.9(5) . . ? C20 Fe1 C21 39.6(4) . . ? C19 Fe1 C21 66.9(5) . . ? C22 Fe1 C21 40.1(4) . . ? C20 Fe1 C50 115.4(6) . . ? C19 Fe1 C50 84.3(7) . . ? C22 Fe1 C50 128.1(7) . . ? C21 Fe1 C50 151.3(6) . . ? C20 Fe1 C23 66.2(5) . . ? C19 Fe1 C23 39.1(5) . . ? C22 Fe1 C23 39.5(5) . . ? C21 Fe1 C23 67.2(5) . . ? C50 Fe1 C23 90.9(7) . . ? C20 Fe1 P5 156.9(4) . . ? C19 Fe1 P5 138.7(4) . . ? C22 Fe1 P5 92.0(4) . . ? C21 Fe1 P5 118.2(3) . . ? C50 Fe1 P5 83.3(6) . . ? C23 Fe1 P5 101.9(4) . . ? C20 Fe1 P4 91.7(4) . . ? C19 Fe1 P4 117.3(4) . . ? C22 Fe1 P4 140.6(4) . . ? C21 Fe1 P4 102.3(4) . . ? C50 Fe1 P4 90.3(6) . . ? C23 Fe1 P4 156.0(4) . . ? P5 Fe1 P4 102.08(16) . . ? C21 P3 C1 100.7(6) . . ? C21 P3 C35 102.3(6) . . ? C1 P3 C35 98.1(6) . . ? C21 P3 Co1 112.4(4) . . ? C1 P3 Co1 121.5(4) . . ? C35 P3 Co1 118.7(5) . . ? C24 P4 C7 102.7(6) . . ? C24 P4 C13 100.0(6) . . ? C7 P4 C13 98.1(6) . . ? C24 P4 Fe1 114.6(4) . . ? C7 P4 Fe1 117.2(5) . . ? C13 P4 Fe1 121.1(4) . . ? C31 P5 C30 100.0(8) . . ? C31 P5 C29 99.5(10) . . ? C30 P5 C29 100.1(8) . . ? C31 P5 Fe1 123.6(7) . . ? C30 P5 Fe1 112.3(5) . . ? C29 P5 Fe1 117.6(6) . . ? C33 P6 C32 100.4(11) . . ? C33 P6 C34 96.2(9) . . ? C32 P6 C34 97.0(10) . . ? C33 P6 Co1 124.5(8) . . ? C32 P6 Co1 118.4(8) . . ? C34 P6 Co1 115.0(6) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 23.32 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.703 _refine_diff_density_min -0.483 _refine_diff_density_rms 0.109 # Attachment '- 5.cif' data_5 _database_code_depnum_ccdc_archive 'CCDC 780556' #TrackingRef '- 5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H46 Co Ni P4' _chemical_formula_weight 768.29 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5071(14) _cell_length_b 19.009(3) _cell_length_c 20.070(3) _cell_angle_alpha 69.582(2) _cell_angle_beta 87.254(2) _cell_angle_gamma 86.414(2) _cell_volume 3747.9(9) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4937 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 24.64 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.362 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1604 _exptl_absorpt_coefficient_mu 1.143 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7112 _exptl_absorpt_correction_T_max 0.7632 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 18803 _diffrn_reflns_av_R_equivalents 0.0233 _diffrn_reflns_av_sigmaI/netI 0.0553 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 25.12 _reflns_number_total 13215 _reflns_number_gt 9351 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0762P)^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 13215 _refine_ls_number_parameters 841 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0730 _refine_ls_R_factor_gt 0.0449 _refine_ls_wR_factor_ref 0.1405 _refine_ls_wR_factor_gt 0.1156 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _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 C1 C 0.6461(4) 1.0006(2) 0.0731(2) 0.0539(12) Uani 1 1 d . . . H1 H 0.5681 1.0331 0.0633 0.065 Uiso 1 1 calc R . . C2 C 0.7290(4) 0.9896(2) 0.1294(2) 0.0439(10) Uani 1 1 d . . . H2 H 0.7185 1.0138 0.1653 0.053 Uiso 1 1 calc R . . C3 C 0.8322(4) 0.9397(2) 0.1245(2) 0.0375(9) Uani 1 1 d . . . C4 C 0.8099(4) 0.9196(3) 0.0643(2) 0.0451(10) Uani 1 1 d . . . H4 H 0.8654 0.8859 0.0469 0.054 Uiso 1 1 calc R . . C5 C 0.6957(5) 0.9566(3) 0.0332(2) 0.0563(12) Uani 1 1 d . . . H5 H 0.6582 0.9532 -0.0093 0.068 Uiso 1 1 calc R . . C6 C 0.5926(5) 0.7810(3) 0.1488(3) 0.0620(14) Uani 1 1 d . . . H6 H 0.6003 0.7572 0.1125 0.074 Uiso 1 1 calc R . . C7 C 0.4907(5) 0.8280(3) 0.1579(3) 0.0653(15) Uani 1 1 d . . . H7 H 0.4150 0.8430 0.1286 0.078 Uiso 1 1 calc R . . C8 C 0.5127(4) 0.8492(3) 0.2162(2) 0.0518(12) Uani 1 1 d . . . H8 H 0.4551 0.8812 0.2345 0.062 Uiso 1 1 calc R . . C9 C 0.6335(4) 0.8167(2) 0.2444(2) 0.0406(10) Uani 1 1 d . . . C10 C 0.6833(5) 0.7739(2) 0.2014(2) 0.0490(11) Uani 1 1 d . . . H10 H 0.7638 0.7436 0.2085 0.059 Uiso 1 1 calc R . . C11 C 1.0541(4) 0.8481(2) 0.1421(2) 0.0395(10) Uani 1 1 d . . . C12 C 1.1251(4) 0.8798(3) 0.0802(2) 0.0528(12) Uani 1 1 d . . . H12 H 1.1286 0.9318 0.0604 0.063 Uiso 1 1 calc R . . C13 C 1.1911(5) 0.8348(3) 0.0476(3) 0.0615(13) Uani 1 1 d . . . H13 H 1.2378 0.8570 0.0056 0.074 Uiso 1 1 calc R . . C14 C 1.1888(5) 0.7583(3) 0.0760(3) 0.0650(14) Uani 1 1 d . . . H14 H 1.2336 0.7285 0.0538 0.078 Uiso 1 1 calc R . . C15 C 1.1198(5) 0.7262(3) 0.1375(3) 0.0660(14) Uani 1 1 d . . . H15 H 1.1194 0.6741 0.1579 0.079 Uiso 1 1 calc R . . C16 C 1.0505(4) 0.7706(2) 0.1697(2) 0.0504(11) Uani 1 1 d . . . H16 H 1.0010 0.7480 0.2104 0.060 Uiso 1 1 calc R . . C17 C 1.0611(4) 0.9868(2) 0.1613(2) 0.0388(9) Uani 1 1 d . . . C18 C 1.1812(5) 0.9775(3) 0.1898(3) 0.0649(14) Uani 1 1 d . . . H18 H 1.2088 0.9306 0.2207 0.078 Uiso 1 1 calc R . . C19 C 1.2608(5) 1.0371(4) 0.1727(3) 0.0760(17) Uani 1 1 d . . . H19 H 1.3410 1.0299 0.1924 0.091 Uiso 1 1 calc R . . C20 C 1.2223(6) 1.1062(3) 0.1274(3) 0.0751(17) Uani 1 1 d . . . H20 H 1.2756 1.1462 0.1163 0.090 Uiso 1 1 calc R . . C21 C 1.1022(5) 1.1165(3) 0.0979(3) 0.0606(13) Uani 1 1 d . . . H21 H 1.0747 1.1635 0.0669 0.073 Uiso 1 1 calc R . . C22 C 1.0244(4) 1.0566(2) 0.1150(2) 0.0495(11) Uani 1 1 d . . . H22 H 0.9449 1.0637 0.0945 0.059 Uiso 1 1 calc R . . C23 C 0.6737(4) 0.7304(2) 0.3860(2) 0.0455(10) Uani 1 1 d . . . C24 C 0.5874(5) 0.6847(3) 0.3742(3) 0.0672(15) Uani 1 1 d . . . H24 H 0.5519 0.6978 0.3297 0.081 Uiso 1 1 calc R . . C25 C 0.5532(7) 0.6196(3) 0.4279(3) 0.0868(19) Uani 1 1 d . . . H25 H 0.4945 0.5895 0.4189 0.104 Uiso 1 1 calc R . . C26 C 0.6030(6) 0.5989(3) 0.4928(3) 0.0741(16) Uani 1 1 d . . . H26 H 0.5776 0.5555 0.5287 0.089 Uiso 1 1 calc R . . C27 C 0.6920(5) 0.6425(3) 0.5059(3) 0.0655(14) Uani 1 1 d . . . H27 H 0.7277 0.6283 0.5505 0.079 Uiso 1 1 calc R . . C28 C 0.7281(5) 0.7077(3) 0.4521(2) 0.0569(12) Uani 1 1 d . . . H28 H 0.7895 0.7365 0.4606 0.068 Uiso 1 1 calc R . . C29 C 0.6033(4) 0.8846(2) 0.3484(2) 0.0455(10) Uani 1 1 d . . . C30 C 0.5306(6) 0.8633(3) 0.4094(3) 0.092(2) Uani 1 1 d . . . H30 H 0.5294 0.8127 0.4375 0.110 Uiso 1 1 calc R . . C31 C 0.4585(8) 0.9158(4) 0.4300(4) 0.135(4) Uani 1 1 d . . . H31 H 0.4141 0.9000 0.4734 0.162 Uiso 1 1 calc R . . C32 C 0.4499(6) 0.9890(4) 0.3896(4) 0.0880(19) Uani 1 1 d . . . H32 H 0.3989 1.0233 0.4038 0.106 Uiso 1 1 calc R . . C33 C 0.5163(6) 1.0105(3) 0.3289(3) 0.0758(16) Uani 1 1 d . . . H33 H 0.5103 1.0605 0.2991 0.091 Uiso 1 1 calc R . . C34 C 0.5950(6) 0.9592(3) 0.3095(3) 0.0721(16) Uani 1 1 d . . . H34 H 0.6444 0.9767 0.2679 0.087 Uiso 1 1 calc R . . C35 C 0.9116(6) 1.0320(3) 0.3106(3) 0.0842(19) Uani 1 1 d . . . H35A H 0.8239 1.0387 0.2972 0.126 Uiso 1 1 calc R . . H35B H 0.9653 1.0514 0.2688 0.126 Uiso 1 1 calc R . . H35C H 0.9243 1.0585 0.3424 0.126 Uiso 1 1 calc R . . C36 C 0.8753(6) 0.9176(4) 0.4419(3) 0.0867(19) Uani 1 1 d . . . H36A H 0.9032 0.9541 0.4605 0.130 Uiso 1 1 calc R . . H36B H 0.8980 0.8680 0.4739 0.130 Uiso 1 1 calc R . . H36C H 0.7844 0.9233 0.4372 0.130 Uiso 1 1 calc R . . C37 C 1.1170(6) 0.9408(4) 0.3785(4) 0.096(2) Uani 1 1 d . . . H37A H 1.1162 0.9753 0.4039 0.143 Uiso 1 1 calc R . . H37B H 1.1689 0.9593 0.3359 0.143 Uiso 1 1 calc R . . H37C H 1.1513 0.8925 0.4080 0.143 Uiso 1 1 calc R . . C38 C 1.0759(6) 0.7331(3) 0.4496(3) 0.090(2) Uani 1 1 d . . . H38A H 1.1387 0.6923 0.4651 0.134 Uiso 1 1 calc R . . H38B H 0.9976 0.7188 0.4763 0.134 Uiso 1 1 calc R . . H38C H 1.1057 0.7764 0.4570 0.134 Uiso 1 1 calc R . . C39 C 1.2175(5) 0.7620(3) 0.3228(3) 0.0815(18) Uani 1 1 d . . . H39A H 1.2641 0.7161 0.3485 0.122 Uiso 1 1 calc R . . H39B H 1.2533 0.8033 0.3311 0.122 Uiso 1 1 calc R . . H39C H 1.2228 0.7697 0.2729 0.122 Uiso 1 1 calc R . . C40 C 1.0181(5) 0.6604(3) 0.3575(3) 0.0785(17) Uani 1 1 d . . . H40A H 1.0391 0.6558 0.3121 0.118 Uiso 1 1 calc R . . H40B H 0.9296 0.6509 0.3692 0.118 Uiso 1 1 calc R . . H40C H 1.0698 0.6247 0.3932 0.118 Uiso 1 1 calc R . . C41 C 0.6143(4) 0.5795(2) 0.8346(2) 0.0365(9) Uani 1 1 d . . . C42 C 0.5763(5) 0.5121(2) 0.8893(2) 0.0488(11) Uani 1 1 d . . . H42 H 0.4954 0.5051 0.9167 0.059 Uiso 1 1 calc R . . C43 C 0.6819(5) 0.4586(3) 0.8995(3) 0.0612(14) Uani 1 1 d . . . H43 H 0.6848 0.4076 0.9346 0.073 Uiso 1 1 calc R . . C44 C 0.7795(5) 0.4906(3) 0.8522(3) 0.0610(14) Uani 1 1 d . . . H44 H 0.8629 0.4662 0.8481 0.073 Uiso 1 1 calc R . . C45 C 0.7392(4) 0.5650(2) 0.8115(2) 0.0456(11) Uani 1 1 d . . . H45 H 0.7901 0.6010 0.7744 0.055 Uiso 1 1 calc R . . C46 C 0.4449(4) 0.4906(2) 0.7453(2) 0.0381(9) Uani 1 1 d . . . C47 C 0.5418(4) 0.5232(2) 0.6941(2) 0.0462(11) Uani 1 1 d . . . H47 H 0.5383 0.5748 0.6599 0.055 Uiso 1 1 calc R . . C48 C 0.6432(5) 0.4686(3) 0.6988(3) 0.0580(13) Uani 1 1 d . . . H48 H 0.7215 0.4760 0.6690 0.070 Uiso 1 1 calc R . . C49 C 0.6101(5) 0.4020(3) 0.7526(3) 0.0599(13) Uani 1 1 d . . . H49 H 0.6623 0.3549 0.7677 0.072 Uiso 1 1 calc R . . C50 C 0.4882(4) 0.4139(2) 0.7821(3) 0.0498(11) Uani 1 1 d . . . H50 H 0.4414 0.3764 0.8201 0.060 Uiso 1 1 calc R . . C51 C 0.2350(4) 0.4692(2) 0.8419(2) 0.0456(11) Uani 1 1 d . . . C52 C 0.2316(4) 0.4816(3) 0.9056(2) 0.0525(12) Uani 1 1 d . . . H52 H 0.2619 0.5258 0.9074 0.063 Uiso 1 1 calc R . . C53 C 0.1834(5) 0.4288(3) 0.9672(3) 0.0748(16) Uani 1 1 d . . . H53 H 0.1808 0.4378 1.0100 0.090 Uiso 1 1 calc R . . C54 C 0.1402(5) 0.3642(3) 0.9647(3) 0.0803(18) Uani 1 1 d . . . H54 H 0.1058 0.3294 1.0056 0.096 Uiso 1 1 calc R . . C55 C 0.1465(5) 0.3494(3) 0.9027(3) 0.0762(17) Uani 1 1 d . . . H55 H 0.1220 0.3034 0.9023 0.091 Uiso 1 1 calc R . . C56 C 0.1893(4) 0.4029(3) 0.8406(3) 0.0588(13) Uani 1 1 d . . . H56 H 0.1874 0.3944 0.7978 0.071 Uiso 1 1 calc R . . C57 C 0.1967(4) 0.5338(2) 0.6945(2) 0.0426(10) Uani 1 1 d . . . C58 C 0.2374(5) 0.5152(3) 0.6364(3) 0.0602(13) Uani 1 1 d . . . H58 H 0.3228 0.5011 0.6318 0.072 Uiso 1 1 calc R . . C59 C 0.1516(6) 0.5172(3) 0.5836(3) 0.0746(16) Uani 1 1 d . . . H59 H 0.1812 0.5047 0.5445 0.090 Uiso 1 1 calc R . . C60 C 0.0277(6) 0.5368(3) 0.5894(3) 0.0746(16) Uani 1 1 d . . . H60 H -0.0285 0.5384 0.5545 0.090 Uiso 1 1 calc R . . C61 C -0.0143(5) 0.5543(4) 0.6467(3) 0.0814(18) Uani 1 1 d . . . H61 H -0.1002 0.5677 0.6508 0.098 Uiso 1 1 calc R . . C62 C 0.0667(5) 0.5527(3) 0.6992(3) 0.0687(15) Uani 1 1 d . . . H62 H 0.0345 0.5644 0.7382 0.082 Uiso 1 1 calc R . . C63 C 0.6287(4) 0.7257(2) 0.7360(2) 0.0354(9) Uani 1 1 d . . . C64 C 0.6381(5) 0.7284(3) 0.6668(2) 0.0597(13) Uani 1 1 d . . . H64 H 0.5875 0.6985 0.6520 0.072 Uiso 1 1 calc R . . C65 C 0.7220(5) 0.7751(3) 0.6187(3) 0.0762(17) Uani 1 1 d . . . H65 H 0.7316 0.7736 0.5729 0.091 Uiso 1 1 calc R . . C66 C 0.7899(5) 0.8225(3) 0.6373(3) 0.0643(14) Uani 1 1 d . . . H66 H 0.8413 0.8563 0.6038 0.077 Uiso 1 1 calc R . . C67 C 0.7828(5) 0.8207(3) 0.7052(3) 0.0685(15) Uani 1 1 d . . . H67 H 0.8318 0.8523 0.7187 0.082 Uiso 1 1 calc R . . C68 C 0.7033(4) 0.7724(3) 0.7548(3) 0.0521(12) Uani 1 1 d . . . H68 H 0.7002 0.7715 0.8015 0.063 Uiso 1 1 calc R . . C69 C 0.5079(4) 0.7056(2) 0.8679(2) 0.0380(9) Uani 1 1 d . . . C70 C 0.4551(4) 0.7779(2) 0.8521(2) 0.0482(11) Uani 1 1 d . . . H70 H 0.4250 0.8034 0.8067 0.058 Uiso 1 1 calc R . . C71 C 0.4460(5) 0.8129(3) 0.9016(3) 0.0612(13) Uani 1 1 d . . . H71 H 0.4117 0.8619 0.8895 0.073 Uiso 1 1 calc R . . C72 C 0.4880(5) 0.7749(3) 0.9696(3) 0.0646(14) Uani 1 1 d . . . H72 H 0.4818 0.7983 1.0034 0.078 Uiso 1 1 calc R . . C73 C 0.5385(5) 0.7033(3) 0.9871(3) 0.0634(14) Uani 1 1 d . . . H73 H 0.5658 0.6776 1.0331 0.076 Uiso 1 1 calc R . . C74 C 0.5494(4) 0.6687(3) 0.9370(2) 0.0496(11) Uani 1 1 d . . . H74 H 0.5850 0.6200 0.9494 0.060 Uiso 1 1 calc R . . C75 C 0.3467(5) 0.7149(3) 0.5757(2) 0.0652(14) Uani 1 1 d . . . H75A H 0.3203 0.7557 0.5341 0.098 Uiso 1 1 calc R . . H75B H 0.3142 0.6691 0.5751 0.098 Uiso 1 1 calc R . . H75C H 0.4382 0.7103 0.5764 0.098 Uiso 1 1 calc R . . C76 C 0.3363(6) 0.8294(3) 0.6349(3) 0.0704(15) Uani 1 1 d . . . H76A H 0.3037 0.8610 0.5898 0.106 Uiso 1 1 calc R . . H76B H 0.4278 0.8289 0.6328 0.106 Uiso 1 1 calc R . . H76C H 0.3045 0.8485 0.6713 0.106 Uiso 1 1 calc R . . C77 C 0.1182(5) 0.7545(3) 0.6297(3) 0.0767(17) Uani 1 1 d . . . H77A H 0.0707 0.7708 0.6642 0.115 Uiso 1 1 calc R . . H77B H 0.0825 0.7101 0.6274 0.115 Uiso 1 1 calc R . . H77C H 0.1141 0.7935 0.5839 0.115 Uiso 1 1 calc R . . C78 C 0.1285(5) 0.7860(3) 0.8065(3) 0.0690(15) Uani 1 1 d . . . H78A H 0.0544 0.7918 0.8344 0.103 Uiso 1 1 calc R . . H78B H 0.1095 0.8068 0.7569 0.103 Uiso 1 1 calc R . . H78C H 0.1973 0.8118 0.8159 0.103 Uiso 1 1 calc R . . C79 C 0.1933(4) 0.6643(3) 0.9257(2) 0.0586(13) Uani 1 1 d . . . H79A H 0.2745 0.6800 0.9337 0.088 Uiso 1 1 calc R . . H79B H 0.1885 0.6111 0.9501 0.088 Uiso 1 1 calc R . . H79C H 0.1265 0.6904 0.9435 0.088 Uiso 1 1 calc R . . C80 C 0.0164(4) 0.6498(3) 0.8334(3) 0.0650(14) Uani 1 1 d . . . H80A H 0.0222 0.5959 0.8527 0.097 Uiso 1 1 calc R . . H80B H -0.0161 0.6659 0.7863 0.097 Uiso 1 1 calc R . . H80C H -0.0400 0.6686 0.8630 0.097 Uiso 1 1 calc R . . Co1 Co 0.65925(5) 0.88667(3) 0.13869(3) 0.04049(15) Uani 1 1 d . . . Co2 Co 0.61569(5) 0.48944(3) 0.79566(3) 0.04145(16) Uani 1 1 d . . . Ni1 Ni 0.91683(5) 0.85205(3) 0.30212(3) 0.03534(14) Uani 1 1 d . . . Ni2 Ni 0.32224(4) 0.65443(3) 0.76256(3) 0.03248(14) Uani 1 1 d . . . P1 P 0.96058(10) 0.90365(6) 0.18896(5) 0.0343(2) Uani 1 1 d . . . P2 P 0.71877(10) 0.82175(6) 0.31935(6) 0.0379(3) Uani 1 1 d . . . P3 P 1.04797(12) 0.75563(7) 0.35368(7) 0.0519(3) Uani 1 1 d . . . P4 P 0.95210(13) 0.93177(7) 0.35494(6) 0.0523(3) Uani 1 1 d . . . P5 P 0.50941(9) 0.66408(5) 0.79737(5) 0.0316(2) Uani 1 1 d . . . P6 P 0.30197(10) 0.54225(6) 0.76206(6) 0.0364(2) Uani 1 1 d . . . P7 P 0.17502(10) 0.68597(7) 0.83006(6) 0.0426(3) Uani 1 1 d . . . P8 P 0.28437(11) 0.73335(6) 0.65565(6) 0.0444(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.048(3) 0.045(3) 0.058(3) -0.004(2) -0.008(2) 0.000(2) C2 0.045(2) 0.038(2) 0.047(3) -0.0118(19) -0.004(2) -0.0027(19) C3 0.045(2) 0.035(2) 0.030(2) -0.0069(17) -0.0009(18) -0.0093(18) C4 0.044(2) 0.060(3) 0.028(2) -0.011(2) -0.0002(19) -0.004(2) C5 0.067(3) 0.063(3) 0.032(2) -0.005(2) -0.008(2) -0.010(3) C6 0.083(4) 0.051(3) 0.057(3) -0.020(2) -0.020(3) -0.017(3) C7 0.056(3) 0.077(4) 0.061(3) -0.016(3) -0.018(3) -0.026(3) C8 0.035(2) 0.068(3) 0.050(3) -0.015(2) -0.002(2) -0.013(2) C9 0.040(2) 0.043(2) 0.035(2) -0.0068(18) 0.0004(18) -0.0121(19) C10 0.064(3) 0.038(2) 0.047(3) -0.014(2) -0.006(2) -0.010(2) C11 0.038(2) 0.043(2) 0.038(2) -0.0154(19) -0.0032(19) 0.0012(19) C12 0.049(3) 0.053(3) 0.053(3) -0.017(2) 0.007(2) 0.006(2) C13 0.051(3) 0.081(4) 0.052(3) -0.026(3) 0.004(2) 0.011(3) C14 0.054(3) 0.082(4) 0.076(4) -0.051(3) -0.003(3) 0.012(3) C15 0.071(4) 0.053(3) 0.084(4) -0.037(3) -0.009(3) 0.006(3) C16 0.052(3) 0.049(3) 0.053(3) -0.021(2) -0.001(2) -0.003(2) C17 0.036(2) 0.047(2) 0.037(2) -0.0199(19) 0.0073(18) -0.0084(19) C18 0.058(3) 0.071(3) 0.062(3) -0.016(3) -0.004(3) -0.017(3) C19 0.051(3) 0.094(5) 0.089(4) -0.034(4) -0.008(3) -0.031(3) C20 0.083(4) 0.079(4) 0.081(4) -0.047(3) 0.030(3) -0.050(3) C21 0.077(4) 0.049(3) 0.060(3) -0.024(2) 0.020(3) -0.017(3) C22 0.053(3) 0.042(3) 0.052(3) -0.015(2) 0.010(2) -0.011(2) C23 0.051(3) 0.043(2) 0.041(3) -0.013(2) 0.007(2) -0.007(2) C24 0.082(4) 0.061(3) 0.052(3) -0.006(3) -0.002(3) -0.030(3) C25 0.119(5) 0.063(4) 0.075(4) -0.015(3) 0.013(4) -0.041(4) C26 0.096(4) 0.052(3) 0.061(4) -0.004(3) 0.018(3) -0.015(3) C27 0.076(4) 0.064(3) 0.042(3) -0.003(2) 0.003(3) 0.004(3) C28 0.058(3) 0.059(3) 0.045(3) -0.006(2) -0.002(2) -0.009(2) C29 0.039(2) 0.052(3) 0.046(3) -0.018(2) 0.001(2) -0.005(2) C30 0.086(4) 0.074(4) 0.088(4) -0.003(3) 0.050(4) 0.013(3) C31 0.150(7) 0.106(6) 0.119(6) -0.018(5) 0.091(6) 0.024(5) C32 0.084(4) 0.076(4) 0.104(5) -0.039(4) 0.024(4) 0.015(3) C33 0.093(4) 0.059(3) 0.076(4) -0.027(3) 0.006(3) 0.002(3) C34 0.095(4) 0.056(3) 0.063(3) -0.020(3) 0.028(3) -0.010(3) C35 0.125(5) 0.053(3) 0.082(4) -0.033(3) 0.017(4) -0.018(3) C36 0.106(5) 0.113(5) 0.058(4) -0.046(3) 0.020(3) -0.052(4) C37 0.083(4) 0.120(5) 0.107(5) -0.063(4) -0.011(4) -0.037(4) C38 0.104(5) 0.091(4) 0.055(3) 0.002(3) -0.032(3) 0.002(4) C39 0.049(3) 0.087(4) 0.095(5) -0.015(3) -0.010(3) 0.002(3) C40 0.086(4) 0.045(3) 0.093(4) -0.009(3) -0.012(3) 0.000(3) C41 0.037(2) 0.035(2) 0.041(2) -0.0175(18) -0.0063(18) -0.0005(17) C42 0.063(3) 0.042(2) 0.041(3) -0.012(2) -0.009(2) -0.003(2) C43 0.076(4) 0.043(3) 0.062(3) -0.012(2) -0.033(3) 0.003(3) C44 0.045(3) 0.056(3) 0.090(4) -0.033(3) -0.025(3) 0.007(2) C45 0.031(2) 0.045(2) 0.065(3) -0.022(2) -0.010(2) -0.0027(19) C46 0.034(2) 0.038(2) 0.048(3) -0.0213(19) -0.0034(19) -0.0042(18) C47 0.048(3) 0.048(3) 0.046(3) -0.022(2) 0.001(2) -0.003(2) C48 0.050(3) 0.074(3) 0.065(3) -0.043(3) 0.006(2) -0.002(3) C49 0.058(3) 0.049(3) 0.084(4) -0.038(3) -0.011(3) 0.009(2) C50 0.057(3) 0.033(2) 0.060(3) -0.016(2) -0.006(2) -0.006(2) C51 0.040(2) 0.042(2) 0.053(3) -0.014(2) 0.005(2) -0.0085(19) C52 0.053(3) 0.052(3) 0.049(3) -0.012(2) 0.003(2) -0.008(2) C53 0.084(4) 0.074(4) 0.056(3) -0.013(3) 0.015(3) 0.000(3) C54 0.072(4) 0.079(4) 0.072(4) -0.004(3) 0.021(3) -0.024(3) C55 0.067(4) 0.065(4) 0.090(5) -0.013(3) 0.002(3) -0.033(3) C56 0.057(3) 0.058(3) 0.059(3) -0.014(2) -0.004(2) -0.023(2) C57 0.044(2) 0.042(2) 0.047(3) -0.020(2) -0.008(2) -0.0068(19) C58 0.055(3) 0.077(3) 0.061(3) -0.040(3) -0.009(2) 0.000(3) C59 0.086(4) 0.092(4) 0.061(4) -0.045(3) -0.020(3) 0.002(3) C60 0.084(4) 0.075(4) 0.071(4) -0.028(3) -0.035(3) -0.006(3) C61 0.052(3) 0.104(5) 0.096(5) -0.043(4) -0.025(3) 0.000(3) C62 0.050(3) 0.096(4) 0.077(4) -0.051(3) -0.011(3) -0.001(3) C63 0.035(2) 0.033(2) 0.037(2) -0.0116(17) 0.0055(18) -0.0025(17) C64 0.070(3) 0.070(3) 0.046(3) -0.026(2) 0.010(2) -0.028(3) C65 0.085(4) 0.094(4) 0.053(3) -0.027(3) 0.028(3) -0.038(3) C66 0.049(3) 0.069(3) 0.067(4) -0.012(3) 0.016(3) -0.021(3) C67 0.064(3) 0.065(3) 0.084(4) -0.032(3) 0.016(3) -0.032(3) C68 0.050(3) 0.063(3) 0.051(3) -0.027(2) 0.004(2) -0.022(2) C69 0.035(2) 0.043(2) 0.041(2) -0.0218(19) 0.0063(18) -0.0089(18) C70 0.051(3) 0.050(3) 0.051(3) -0.026(2) -0.003(2) 0.000(2) C71 0.061(3) 0.063(3) 0.074(4) -0.044(3) -0.003(3) 0.005(3) C72 0.058(3) 0.093(4) 0.065(3) -0.054(3) 0.000(3) -0.003(3) C73 0.064(3) 0.088(4) 0.047(3) -0.034(3) -0.009(2) 0.001(3) C74 0.052(3) 0.058(3) 0.040(3) -0.019(2) -0.007(2) 0.002(2) C75 0.091(4) 0.063(3) 0.041(3) -0.019(2) 0.006(3) 0.004(3) C76 0.099(4) 0.044(3) 0.059(3) -0.008(2) 0.006(3) -0.002(3) C77 0.066(4) 0.099(4) 0.051(3) -0.011(3) -0.014(3) 0.015(3) C78 0.068(3) 0.060(3) 0.083(4) -0.033(3) 0.006(3) 0.015(3) C79 0.050(3) 0.085(4) 0.046(3) -0.029(3) 0.006(2) -0.005(3) C80 0.038(3) 0.099(4) 0.068(3) -0.041(3) 0.006(2) -0.009(3) Co1 0.0414(3) 0.0420(3) 0.0376(3) -0.0121(3) -0.0046(3) -0.0056(3) Co2 0.0389(3) 0.0370(3) 0.0509(4) -0.0180(3) -0.0052(3) -0.0005(2) Ni1 0.0384(3) 0.0348(3) 0.0314(3) -0.0089(2) -0.0018(2) -0.0062(2) Ni2 0.0313(3) 0.0357(3) 0.0319(3) -0.0135(2) 0.0003(2) -0.0028(2) P1 0.0334(6) 0.0351(5) 0.0332(6) -0.0102(4) 0.0007(4) -0.0031(4) P2 0.0402(6) 0.0393(6) 0.0326(6) -0.0097(5) 0.0019(5) -0.0081(5) P3 0.0491(7) 0.0471(7) 0.0497(7) -0.0038(5) -0.0107(6) 0.0011(6) P4 0.0665(8) 0.0539(7) 0.0423(7) -0.0215(6) 0.0030(6) -0.0197(6) P5 0.0310(5) 0.0331(5) 0.0325(5) -0.0132(4) 0.0008(4) -0.0046(4) P6 0.0357(6) 0.0386(6) 0.0378(6) -0.0164(5) -0.0004(5) -0.0066(5) P7 0.0353(6) 0.0549(7) 0.0418(6) -0.0228(5) 0.0034(5) -0.0008(5) P8 0.0498(7) 0.0446(6) 0.0356(6) -0.0106(5) -0.0020(5) 0.0016(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 C1 C5 1.408(7) . ? C1 C2 1.410(6) . ? C1 Co1 2.105(4) . ? C1 H1 0.9800 . ? C2 C3 1.418(6) . ? C2 Co1 2.077(4) . ? C2 H2 0.9800 . ? C3 C4 1.421(6) . ? C3 P1 1.843(4) . ? C3 Co1 2.092(4) . ? C4 C5 1.409(6) . ? C4 Co1 2.091(4) . ? C4 H4 0.9800 . ? C5 Co1 2.102(4) . ? C5 H5 0.9800 . ? C6 C7 1.398(7) . ? C6 C10 1.423(6) . ? C6 Co1 2.108(5) . ? C6 H6 0.9800 . ? C7 C8 1.397(7) . ? C7 Co1 2.100(5) . ? C7 H7 0.9800 . ? C8 C9 1.429(6) . ? C8 Co1 2.106(4) . ? C8 H8 0.9800 . ? C9 C10 1.439(6) . ? C9 P2 1.821(4) . ? C9 Co1 2.089(4) . ? C10 Co1 2.079(4) . ? C10 H10 0.9800 . ? C11 C12 1.380(6) . ? C11 C16 1.383(6) . ? C11 P1 1.856(4) . ? C12 C13 1.384(6) . ? C12 H12 0.9300 . ? C13 C14 1.366(7) . ? C13 H13 0.9300 . ? C14 C15 1.366(7) . ? C14 H14 0.9300 . ? C15 C16 1.385(6) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C22 1.372(6) . ? C17 C18 1.386(6) . ? C17 P1 1.861(4) . ? C18 C19 1.386(7) . ? C18 H18 0.9300 . ? C19 C20 1.360(8) . ? C19 H19 0.9300 . ? C20 C21 1.393(8) . ? C20 H20 0.9300 . ? C21 C22 1.378(6) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.376(6) . ? C23 C28 1.385(6) . ? C23 P2 1.858(4) . ? C24 C25 1.382(7) . ? C24 H24 0.9300 . ? C25 C26 1.345(8) . ? C25 H25 0.9300 . ? C26 C27 1.379(8) . ? C26 H26 0.9300 . ? C27 C28 1.391(6) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.359(6) . ? C29 C34 1.359(6) . ? C29 P2 1.865(4) . ? C30 C31 1.381(8) . ? C30 H30 0.9300 . ? C31 C32 1.343(8) . ? C31 H31 0.9300 . ? C32 C33 1.319(7) . ? C32 H32 0.9300 . ? C33 C34 1.385(7) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 P4 1.832(5) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 P4 1.827(5) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 P4 1.851(6) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 P3 1.853(5) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 P3 1.854(5) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 P3 1.830(5) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C45 1.413(6) . ? C41 C42 1.430(6) . ? C41 P5 1.838(4) . ? C41 Co2 2.114(4) . ? C42 C43 1.430(6) . ? C42 Co2 2.088(4) . ? C42 H42 0.9800 . ? C43 C44 1.379(7) . ? C43 Co2 2.098(5) . ? C43 H43 0.9800 . ? C44 C45 1.415(6) . ? C44 Co2 2.112(5) . ? C44 H44 0.9800 . ? C45 Co2 2.107(4) . ? C45 H45 0.9800 . ? C46 C47 1.419(6) . ? C46 C50 1.440(6) . ? C46 P6 1.825(4) . ? C46 Co2 2.096(4) . ? C47 C48 1.423(6) . ? C47 Co2 2.085(4) . ? C47 H47 0.9800 . ? C48 C49 1.399(7) . ? C48 Co2 2.120(5) . ? C48 H48 0.9800 . ? C49 C50 1.423(6) . ? C49 Co2 2.128(5) . ? C49 H49 0.9800 . ? C50 Co2 2.117(4) . ? C50 H50 0.9800 . ? C51 C52 1.377(6) . ? C51 C56 1.386(6) . ? C51 P6 1.858(4) . ? C52 C53 1.390(7) . ? C52 H52 0.9300 . ? C53 C54 1.354(8) . ? C53 H53 0.9300 . ? C54 C55 1.365(8) . ? C54 H54 0.9300 . ? C55 C56 1.381(7) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C57 C58 1.374(6) . ? C57 C62 1.398(6) . ? C57 P6 1.846(4) . ? C58 C59 1.414(7) . ? C58 H58 0.9300 . ? C59 C60 1.343(8) . ? C59 H59 0.9300 . ? C60 C61 1.351(8) . ? C60 H60 0.9300 . ? C61 C62 1.377(7) . ? C61 H61 0.9300 . ? C62 H62 0.9300 . ? C63 C64 1.372(6) . ? C63 C68 1.377(6) . ? C63 P5 1.868(4) . ? C64 C65 1.385(6) . ? C64 H64 0.9300 . ? C65 C66 1.342(7) . ? C65 H65 0.9300 . ? C66 C67 1.350(7) . ? C66 H66 0.9300 . ? C67 C68 1.382(6) . ? C67 H67 0.9300 . ? C68 H68 0.9300 . ? C69 C70 1.384(6) . ? C69 C74 1.394(6) . ? C69 P5 1.845(4) . ? C70 C71 1.372(6) . ? C70 H70 0.9300 . ? C71 C72 1.382(7) . ? C71 H71 0.9300 . ? C72 C73 1.360(7) . ? C72 H72 0.9300 . ? C73 C74 1.378(6) . ? C73 H73 0.9300 . ? C74 H74 0.9300 . ? C75 P8 1.841(5) . ? C75 H75A 0.9600 . ? C75 H75B 0.9600 . ? C75 H75C 0.9600 . ? C76 P8 1.837(5) . ? C76 H76A 0.9600 . ? C76 H76B 0.9600 . ? C76 H76C 0.9600 . ? C77 P8 1.826(5) . ? C77 H77A 0.9600 . ? C77 H77B 0.9600 . ? C77 H77C 0.9600 . ? C78 P7 1.832(5) . ? C78 H78A 0.9600 . ? C78 H78B 0.9600 . ? C78 H78C 0.9600 . ? C79 P7 1.835(5) . ? C79 H79A 0.9600 . ? C79 H79B 0.9600 . ? C79 H79C 0.9600 . ? C80 P7 1.832(5) . ? C80 H80A 0.9600 . ? C80 H80B 0.9600 . ? C80 H80C 0.9600 . ? Ni1 P2 2.1735(12) . ? Ni1 P1 2.1758(12) . ? Ni1 P4 2.1878(13) . ? Ni1 P3 2.1969(13) . ? Ni2 P5 2.1577(11) . ? Ni2 P6 2.1598(12) . ? Ni2 P8 2.1849(12) . ? Ni2 P7 2.1993(12) . ? 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 C5 C1 C2 107.8(4) . . ? C5 C1 Co1 70.3(3) . . ? C2 C1 Co1 69.2(2) . . ? C5 C1 H1 126.1 . . ? C2 C1 H1 126.1 . . ? Co1 C1 H1 126.1 . . ? C1 C2 C3 109.0(4) . . ? C1 C2 Co1 71.4(2) . . ? C3 C2 Co1 70.7(2) . . ? C1 C2 H2 125.5 . . ? C3 C2 H2 125.5 . . ? Co1 C2 H2 125.5 . . ? C2 C3 C4 106.4(4) . . ? C2 C3 P1 125.4(3) . . ? C4 C3 P1 128.1(3) . . ? C2 C3 Co1 69.5(2) . . ? C4 C3 Co1 70.1(2) . . ? P1 C3 Co1 121.50(19) . . ? C5 C4 C3 108.8(4) . . ? C5 C4 Co1 70.8(2) . . ? C3 C4 Co1 70.2(2) . . ? C5 C4 H4 125.6 . . ? C3 C4 H4 125.6 . . ? Co1 C4 H4 125.6 . . ? C1 C5 C4 108.0(4) . . ? C1 C5 Co1 70.6(3) . . ? C4 C5 Co1 69.9(2) . . ? C1 C5 H5 126.0 . . ? C4 C5 H5 126.0 . . ? Co1 C5 H5 126.0 . . ? C7 C6 C10 107.8(4) . . ? C7 C6 Co1 70.3(3) . . ? C10 C6 Co1 69.0(2) . . ? C7 C6 H6 126.1 . . ? C10 C6 H6 126.1 . . ? Co1 C6 H6 126.1 . . ? C8 C7 C6 109.3(4) . . ? C8 C7 Co1 70.8(3) . . ? C6 C7 Co1 70.9(3) . . ? C8 C7 H7 125.3 . . ? C6 C7 H7 125.3 . . ? Co1 C7 H7 125.3 . . ? C7 C8 C9 108.5(5) . . ? C7 C8 Co1 70.4(3) . . ? C9 C8 Co1 69.5(2) . . ? C7 C8 H8 125.7 . . ? C9 C8 H8 125.7 . . ? Co1 C8 H8 125.7 . . ? C8 C9 C10 106.4(4) . . ? C8 C9 P2 131.2(4) . . ? C10 C9 P2 122.4(3) . . ? C8 C9 Co1 70.7(2) . . ? C10 C9 Co1 69.4(2) . . ? P2 C9 Co1 125.1(2) . . ? C6 C10 C9 107.9(4) . . ? C6 C10 Co1 71.3(3) . . ? C9 C10 Co1 70.2(2) . . ? C6 C10 H10 126.0 . . ? C9 C10 H10 126.0 . . ? Co1 C10 H10 126.0 . . ? C12 C11 C16 118.1(4) . . ? C12 C11 P1 123.6(3) . . ? C16 C11 P1 118.3(3) . . ? C11 C12 C13 120.4(4) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 121.0(5) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C15 119.2(5) . . ? C13 C14 H14 120.4 . . ? C15 C14 H14 120.4 . . ? C14 C15 C16 120.4(5) . . ? C14 C15 H15 119.8 . . ? C16 C15 H15 119.8 . . ? C11 C16 C15 120.8(4) . . ? C11 C16 H16 119.6 . . ? C15 C16 H16 119.6 . . ? C22 C17 C18 117.9(4) . . ? C22 C17 P1 124.6(3) . . ? C18 C17 P1 117.6(3) . . ? C17 C18 C19 121.0(5) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C20 C19 C18 120.4(5) . . ? C20 C19 H19 119.8 . . ? C18 C19 H19 119.8 . . ? C19 C20 C21 119.5(5) . . ? C19 C20 H20 120.3 . . ? C21 C20 H20 120.3 . . ? C22 C21 C20 119.5(5) . . ? C22 C21 H21 120.2 . . ? C20 C21 H21 120.2 . . ? C17 C22 C21 121.8(5) . . ? C17 C22 H22 119.1 . . ? C21 C22 H22 119.1 . . ? C24 C23 C28 118.0(4) . . ? C24 C23 P2 124.0(4) . . ? C28 C23 P2 117.9(3) . . ? C23 C24 C25 120.6(5) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C26 C25 C24 121.3(6) . . ? C26 C25 H25 119.4 . . ? C24 C25 H25 119.4 . . ? C25 C26 C27 119.6(5) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C26 C27 C28 119.6(5) . . ? C26 C27 H27 120.2 . . ? C28 C27 H27 120.2 . . ? C23 C28 C27 120.8(5) . . ? C23 C28 H28 119.6 . . ? C27 C28 H28 119.6 . . ? C30 C29 C34 115.3(5) . . ? C30 C29 P2 125.3(4) . . ? C34 C29 P2 119.2(3) . . ? C29 C30 C31 120.7(6) . . ? C29 C30 H30 119.6 . . ? C31 C30 H30 119.6 . . ? C32 C31 C30 122.5(6) . . ? C32 C31 H31 118.8 . . ? C30 C31 H31 118.8 . . ? C33 C32 C31 117.7(6) . . ? C33 C32 H32 121.1 . . ? C31 C32 H32 121.1 . . ? C32 C33 C34 120.5(6) . . ? C32 C33 H33 119.8 . . ? C34 C33 H33 119.8 . . ? C29 C34 C33 123.1(5) . . ? C29 C34 H34 118.4 . . ? C33 C34 H34 118.4 . . ? P4 C35 H35A 109.5 . . ? P4 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? P4 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? P4 C36 H36A 109.5 . . ? P4 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? P4 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? P4 C37 H37A 109.5 . . ? P4 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? P4 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? P3 C38 H38A 109.5 . . ? P3 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? P3 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? P3 C39 H39A 109.5 . . ? P3 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? P3 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? P3 C40 H40A 109.5 . . ? P3 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? P3 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C45 C41 C42 107.3(4) . . ? C45 C41 P5 128.1(3) . . ? C42 C41 P5 124.4(3) . . ? C45 C41 Co2 70.2(2) . . ? C42 C41 Co2 69.1(2) . . ? P5 C41 Co2 121.3(2) . . ? C43 C42 C41 106.9(4) . . ? C43 C42 Co2 70.4(3) . . ? C41 C42 Co2 71.1(2) . . ? C43 C42 H42 126.5 . . ? C41 C42 H42 126.5 . . ? Co2 C42 H42 126.5 . . ? C44 C43 C42 109.0(4) . . ? C44 C43 Co2 71.4(3) . . ? C42 C43 Co2 69.6(3) . . ? C44 C43 H43 125.5 . . ? C42 C43 H43 125.5 . . ? Co2 C43 H43 125.5 . . ? C43 C44 C45 108.3(4) . . ? C43 C44 Co2 70.4(3) . . ? C45 C44 Co2 70.2(2) . . ? C43 C44 H44 125.8 . . ? C45 C44 H44 125.8 . . ? Co2 C44 H44 125.8 . . ? C41 C45 C44 108.5(4) . . ? C41 C45 Co2 70.7(2) . . ? C44 C45 Co2 70.6(3) . . ? C41 C45 H45 125.7 . . ? C44 C45 H45 125.7 . . ? Co2 C45 H45 125.7 . . ? C47 C46 C50 106.5(4) . . ? C47 C46 P6 124.1(3) . . ? C50 C46 P6 129.4(3) . . ? C47 C46 Co2 69.8(2) . . ? C50 C46 Co2 70.8(2) . . ? P6 C46 Co2 120.9(2) . . ? C46 C47 C48 109.2(4) . . ? C46 C47 Co2 70.6(2) . . ? C48 C47 Co2 71.5(3) . . ? C46 C47 H47 125.4 . . ? C48 C47 H47 125.4 . . ? Co2 C47 H47 125.4 . . ? C49 C48 C47 107.6(4) . . ? C49 C48 Co2 71.1(3) . . ? C47 C48 Co2 68.9(2) . . ? C49 C48 H48 126.2 . . ? C47 C48 H48 126.2 . . ? Co2 C48 H48 126.2 . . ? C48 C49 C50 108.9(4) . . ? C48 C49 Co2 70.4(3) . . ? C50 C49 Co2 70.0(3) . . ? C48 C49 H49 125.6 . . ? C50 C49 H49 125.6 . . ? Co2 C49 H49 125.6 . . ? C49 C50 C46 107.8(4) . . ? C49 C50 Co2 70.9(3) . . ? C46 C50 Co2 69.2(2) . . ? C49 C50 H50 126.1 . . ? C46 C50 H50 126.1 . . ? Co2 C50 H50 126.1 . . ? C52 C51 C56 118.5(4) . . ? C52 C51 P6 118.1(3) . . ? C56 C51 P6 123.4(4) . . ? C51 C52 C53 120.7(5) . . ? C51 C52 H52 119.6 . . ? C53 C52 H52 119.6 . . ? C54 C53 C52 119.6(6) . . ? C54 C53 H53 120.2 . . ? C52 C53 H53 120.2 . . ? C53 C54 C55 120.8(5) . . ? C53 C54 H54 119.6 . . ? C55 C54 H54 119.6 . . ? C54 C55 C56 119.9(5) . . ? C54 C55 H55 120.0 . . ? C56 C55 H55 120.0 . . ? C55 C56 C51 120.3(5) . . ? C55 C56 H56 119.9 . . ? C51 C56 H56 119.9 . . ? C58 C57 C62 116.7(4) . . ? C58 C57 P6 124.9(3) . . ? C62 C57 P6 118.3(3) . . ? C57 C58 C59 121.1(5) . . ? C57 C58 H58 119.5 . . ? C59 C58 H58 119.5 . . ? C60 C59 C58 120.5(5) . . ? C60 C59 H59 119.8 . . ? C58 C59 H59 119.8 . . ? C59 C60 C61 119.2(5) . . ? C59 C60 H60 120.4 . . ? C61 C60 H60 120.4 . . ? C60 C61 C62 121.8(5) . . ? C60 C61 H61 119.1 . . ? C62 C61 H61 119.1 . . ? C61 C62 C57 120.8(5) . . ? C61 C62 H62 119.6 . . ? C57 C62 H62 119.6 . . ? C64 C63 C68 117.4(4) . . ? C64 C63 P5 118.6(3) . . ? C68 C63 P5 123.9(3) . . ? C63 C64 C65 120.8(5) . . ? C63 C64 H64 119.6 . . ? C65 C64 H64 119.6 . . ? C66 C65 C64 120.8(5) . . ? C66 C65 H65 119.6 . . ? C64 C65 H65 119.6 . . ? C65 C66 C67 119.4(5) . . ? C65 C66 H66 120.3 . . ? C67 C66 H66 120.3 . . ? C66 C67 C68 120.6(5) . . ? C66 C67 H67 119.7 . . ? C68 C67 H67 119.7 . . ? C63 C68 C67 120.9(5) . . ? C63 C68 H68 119.6 . . ? C67 C68 H68 119.6 . . ? C70 C69 C74 117.3(4) . . ? C70 C69 P5 117.2(3) . . ? C74 C69 P5 125.4(3) . . ? C71 C70 C69 121.7(4) . . ? C71 C70 H70 119.2 . . ? C69 C70 H70 119.2 . . ? C70 C71 C72 119.6(5) . . ? C70 C71 H71 120.2 . . ? C72 C71 H71 120.2 . . ? C73 C72 C71 120.1(5) . . ? C73 C72 H72 120.0 . . ? C71 C72 H72 120.0 . . ? C72 C73 C74 120.2(5) . . ? C72 C73 H73 119.9 . . ? C74 C73 H73 119.9 . . ? C73 C74 C69 121.1(4) . . ? C73 C74 H74 119.5 . . ? C69 C74 H74 119.5 . . ? P8 C75 H75A 109.5 . . ? P8 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? P8 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? P8 C76 H76A 109.5 . . ? P8 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? P8 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? P8 C77 H77A 109.5 . . ? P8 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? P8 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? P7 C78 H78A 109.5 . . ? P7 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? P7 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? P7 C79 H79A 109.5 . . ? P7 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? P7 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? P7 C80 H80A 109.5 . . ? P7 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? P7 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C2 Co1 C10 139.20(17) . . ? C2 Co1 C9 112.76(17) . . ? C10 Co1 C9 40.39(16) . . ? C2 Co1 C4 66.12(18) . . ? C10 Co1 C4 110.95(18) . . ? C9 Co1 C4 137.77(16) . . ? C2 Co1 C3 39.76(15) . . ? C10 Co1 C3 110.53(17) . . ? C9 Co1 C3 110.63(15) . . ? C4 Co1 C3 39.73(16) . . ? C2 Co1 C7 142.4(2) . . ? C10 Co1 C7 66.1(2) . . ? C9 Co1 C7 66.38(18) . . ? C4 Co1 C7 141.5(2) . . ? C3 Co1 C7 176.56(19) . . ? C2 Co1 C5 66.01(18) . . ? C10 Co1 C5 138.73(19) . . ? C9 Co1 C5 176.95(18) . . ? C4 Co1 C5 39.27(17) . . ? C3 Co1 C5 66.57(17) . . ? C7 Co1 C5 116.4(2) . . ? C2 Co1 C1 39.40(17) . . ? C10 Co1 C1 176.64(19) . . ? C9 Co1 C1 141.56(18) . . ? C4 Co1 C1 65.79(18) . . ? C3 Co1 C1 66.54(16) . . ? C7 Co1 C1 116.8(2) . . ? C5 Co1 C1 39.11(18) . . ? C2 Co1 C8 115.13(18) . . ? C10 Co1 C8 66.57(19) . . ? C9 Co1 C8 39.82(16) . . ? C4 Co1 C8 177.41(18) . . ? C3 Co1 C8 139.78(17) . . ? C7 Co1 C8 38.79(18) . . ? C5 Co1 C8 143.16(19) . . ? C1 Co1 C8 116.68(19) . . ? C2 Co1 C6 178.69(19) . . ? C10 Co1 C6 39.74(17) . . ? C9 Co1 C6 66.89(18) . . ? C4 Co1 C6 113.2(2) . . ? C3 Co1 C6 139.0(2) . . ? C7 Co1 C6 38.8(2) . . ? C5 Co1 C6 114.3(2) . . ? C1 Co1 C6 141.59(19) . . ? C8 Co1 C6 65.5(2) . . ? C47 Co2 C42 137.05(17) . . ? C47 Co2 C46 39.68(16) . . ? C42 Co2 C46 109.68(17) . . ? C47 Co2 C43 176.96(19) . . ? C42 Co2 C43 39.93(18) . . ? C46 Co2 C43 138.4(2) . . ? C47 Co2 C45 114.76(18) . . ? C42 Co2 C45 66.15(18) . . ? C46 Co2 C45 139.76(16) . . ? C43 Co2 C45 65.16(19) . . ? C47 Co2 C44 143.5(2) . . ? C42 Co2 C44 66.0(2) . . ? C46 Co2 C44 175.66(19) . . ? C43 Co2 C44 38.24(19) . . ? C45 Co2 C44 39.18(17) . . ? C47 Co2 C41 111.80(16) . . ? C42 Co2 C41 39.79(15) . . ? C46 Co2 C41 110.91(15) . . ? C43 Co2 C41 66.08(17) . . ? C45 Co2 C41 39.11(15) . . ? C44 Co2 C41 65.78(17) . . ? C47 Co2 C50 66.05(17) . . ? C42 Co2 C50 112.26(18) . . ? C46 Co2 C50 39.98(15) . . ? C43 Co2 C50 113.94(19) . . ? C45 Co2 C50 178.37(18) . . ? C44 Co2 C50 140.90(18) . . ? C41 Co2 C50 139.41(17) . . ? C47 Co2 C48 39.56(17) . . ? C42 Co2 C48 176.27(19) . . ? C46 Co2 C48 66.67(17) . . ? C43 Co2 C48 143.4(2) . . ? C45 Co2 C48 115.95(19) . . ? C44 Co2 C48 117.7(2) . . ? C41 Co2 C48 139.92(18) . . ? C50 Co2 C48 65.61(19) . . ? C47 Co2 C49 65.44(19) . . ? C42 Co2 C49 141.59(19) . . ? C46 Co2 C49 66.42(17) . . ? C43 Co2 C49 116.64(19) . . ? C45 Co2 C49 142.36(18) . . ? C44 Co2 C49 116.94(19) . . ? C41 Co2 C49 177.08(17) . . ? C50 Co2 C49 39.17(17) . . ? C48 Co2 C49 38.45(18) . . ? P2 Ni1 P1 110.32(4) . . ? P2 Ni1 P4 109.89(5) . . ? P1 Ni1 P4 108.87(5) . . ? P2 Ni1 P3 111.82(5) . . ? P1 Ni1 P3 112.17(5) . . ? P4 Ni1 P3 103.52(6) . . ? P5 Ni2 P6 110.21(4) . . ? P5 Ni2 P8 112.63(5) . . ? P6 Ni2 P8 107.85(5) . . ? P5 Ni2 P7 109.97(5) . . ? P6 Ni2 P7 112.10(5) . . ? P8 Ni2 P7 103.95(5) . . ? C3 P1 C11 97.54(18) . . ? C3 P1 C17 99.86(18) . . ? C11 P1 C17 97.83(18) . . ? C3 P1 Ni1 120.93(13) . . ? C11 P1 Ni1 119.22(13) . . ? C17 P1 Ni1 116.98(13) . . ? C9 P2 C23 98.09(19) . . ? C9 P2 C29 99.3(2) . . ? C23 P2 C29 98.48(19) . . ? C9 P2 Ni1 118.20(13) . . ? C23 P2 Ni1 120.89(15) . . ? C29 P2 Ni1 117.55(14) . . ? C40 P3 C38 97.6(3) . . ? C40 P3 C39 100.5(3) . . ? C38 P3 C39 97.3(3) . . ? C40 P3 Ni1 121.99(19) . . ? C38 P3 Ni1 117.3(2) . . ? C39 P3 Ni1 117.57(19) . . ? C36 P4 C35 99.8(3) . . ? C36 P4 C37 98.0(3) . . ? C35 P4 C37 97.7(3) . . ? C36 P4 Ni1 117.97(18) . . ? C35 P4 Ni1 119.7(2) . . ? C37 P4 Ni1 119.3(2) . . ? C41 P5 C69 101.68(18) . . ? C41 P5 C63 98.24(18) . . ? C69 P5 C63 97.54(17) . . ? C41 P5 Ni2 119.83(13) . . ? C69 P5 Ni2 113.96(13) . . ? C63 P5 Ni2 121.58(13) . . ? C46 P6 C57 100.12(19) . . ? C46 P6 C51 99.82(19) . . ? C57 P6 C51 99.1(2) . . ? C46 P6 Ni2 117.94(13) . . ? C57 P6 Ni2 116.29(14) . . ? C51 P6 Ni2 119.93(15) . . ? C80 P7 C78 98.7(3) . . ? C80 P7 C79 98.5(2) . . ? C78 P7 C79 97.8(2) . . ? C80 P7 Ni2 117.13(17) . . ? C78 P7 Ni2 117.43(17) . . ? C79 P7 Ni2 122.71(16) . . ? C77 P8 C76 99.6(3) . . ? C77 P8 C75 97.5(3) . . ? C76 P8 C75 99.8(2) . . ? C77 P8 Ni2 117.74(17) . . ? C76 P8 Ni2 116.45(18) . . ? C75 P8 Ni2 121.66(17) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 25.12 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.506 _refine_diff_density_min -0.433 _refine_diff_density_rms 0.107 data_1 _database_code_depnum_ccdc_archive 'CCDC 780557' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H46 Co2 P4' _chemical_formula_sum 'C40 H46 Co2 P4' _chemical_formula_weight 768.51 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.649(11) _cell_length_b 17.258(15) _cell_length_c 18.330(15) _cell_angle_alpha 90.00 _cell_angle_beta 103.868(14) _cell_angle_gamma 90.00 _cell_volume 3885(6) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 2492 _cell_measurement_theta_min 2.23 _cell_measurement_theta_max 21.40 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 1.045 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8590 _exptl_absorpt_correction_T_max 0.9027 _exptl_absorpt_process_details ? _exptl_special_details ; Theta(max) is low. The reason is that the quality of the crystal is not very good, and the diffraction data is relatively weak. ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13201 _diffrn_reflns_av_R_equivalents 0.0672 _diffrn_reflns_av_sigmaI/netI 0.0777 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 21.63 _reflns_number_total 4467 _reflns_number_gt 2946 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1105P)^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 4467 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0905 _refine_ls_R_factor_gt 0.0637 _refine_ls_wR_factor_ref 0.1841 _refine_ls_wR_factor_gt 0.1690 _refine_ls_goodness_of_fit_ref 1.003 _refine_ls_restrained_S_all 1.003 _refine_ls_shift/su_max 0.090 _refine_ls_shift/su_mean 0.014 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 C40 C 0.8255(6) 0.7743(5) -0.0210(5) 0.069(2) Uani 1 1 d . . . H40A H 0.7987 0.8212 -0.0471 0.103 Uiso 1 1 calc R . . H40B H 0.8605 0.7433 -0.0518 0.103 Uiso 1 1 calc R . . H40C H 0.8769 0.7868 0.0252 0.103 Uiso 1 1 calc R . . C38 C 0.6561(6) 0.6754(6) -0.0933(4) 0.076(3) Uani 1 1 d . . . H38A H 0.6150 0.7133 -0.1267 0.114 Uiso 1 1 calc R . . H38B H 0.6096 0.6327 -0.0885 0.114 Uiso 1 1 calc R . . H38C H 0.7151 0.6571 -0.1132 0.114 Uiso 1 1 calc R . . C37 C 0.0761(6) 0.8012(5) 0.1813(5) 0.078(3) Uani 1 1 d . . . H37A H 0.0433 0.8291 0.1363 0.117 Uiso 1 1 calc R . . H37B H 0.1048 0.8372 0.2210 0.117 Uiso 1 1 calc R . . H37C H 0.0224 0.7690 0.1954 0.117 Uiso 1 1 calc R . . C35 C 0.2331(7) 0.6963(5) 0.2577(4) 0.075(3) Uani 1 1 d . . . H35A H 0.2752 0.7334 0.2917 0.113 Uiso 1 1 calc R . . H35B H 0.2772 0.6517 0.2547 0.113 Uiso 1 1 calc R . . H35C H 0.1709 0.6810 0.2757 0.113 Uiso 1 1 calc R . . C39 C 0.7828(7) 0.6360(5) 0.0479(5) 0.085(3) Uani 1 1 d . . . H39A H 0.7318 0.6016 0.0624 0.128 Uiso 1 1 calc R . . H39B H 0.8356 0.6529 0.0918 0.128 Uiso 1 1 calc R . . H39C H 0.8190 0.6094 0.0149 0.128 Uiso 1 1 calc R . . C36 C 0.1099(7) 0.6589(5) 0.1126(5) 0.086(3) Uani 1 1 d . . . H36A H 0.0802 0.6740 0.0614 0.129 Uiso 1 1 calc R . . H36B H 0.0517 0.6451 0.1355 0.129 Uiso 1 1 calc R . . H36C H 0.1572 0.6151 0.1139 0.129 Uiso 1 1 calc R . . Co1 Co 0.61523(7) 0.78308(6) 0.06033(5) 0.0412(3) Uani 1 1 d . . . Co2 Co 0.29266(7) 0.79652(5) 0.10609(5) 0.0388(3) Uani 1 1 d . . . P2 P 0.44206(14) 0.78237(10) 0.18791(10) 0.0368(5) Uani 1 1 d . . . P1 P 0.46444(14) 0.78658(10) -0.02158(9) 0.0366(5) Uani 1 1 d . . . P3 P 0.71081(15) 0.71957(13) -0.00021(11) 0.0507(6) Uani 1 1 d . . . P4 P 0.18753(15) 0.73995(13) 0.16445(11) 0.0532(6) Uani 1 1 d . . . C9 C 0.7440(6) 0.7986(6) 0.1495(4) 0.061(2) Uani 1 1 d . . . H9 H 0.8132 0.7803 0.1495 0.073 Uiso 1 1 calc R . . C29 C 0.4623(5) 0.8452(4) 0.2719(3) 0.0398(17) Uani 1 1 d . . . C4 C 0.1666(6) 0.8242(5) 0.0172(4) 0.052(2) Uani 1 1 d . . . H4 H 0.0950 0.8109 0.0163 0.063 Uiso 1 1 calc R . . C11 C 0.4168(5) 0.6931(4) -0.0671(4) 0.0383(17) Uani 1 1 d . . . C16 C 0.3726(6) 0.6816(4) -0.1429(4) 0.0489(19) Uani 1 1 d . . . H16 H 0.3638 0.7236 -0.1756 0.059 Uiso 1 1 calc R . . C34 C 0.3741(6) 0.8892(4) 0.2828(4) 0.050(2) Uani 1 1 d . . . H34 H 0.3070 0.8848 0.2485 0.060 Uiso 1 1 calc R . . C17 C 0.4517(6) 0.8539(4) -0.1026(4) 0.0428(18) Uani 1 1 d . . . C12 C 0.4269(6) 0.6294(4) -0.0200(4) 0.0484(19) Uani 1 1 d . . . H12 H 0.4573 0.6358 0.0311 0.058 Uiso 1 1 calc R . . C5 C 0.2387(6) 0.7769(4) -0.0094(4) 0.0474(19) Uani 1 1 d . . . H5 H 0.2224 0.7295 -0.0336 0.057 Uiso 1 1 calc R . . C1 C 0.3426(5) 0.8151(4) 0.0074(3) 0.0366(17) Uani 1 1 d . . . C6 C 0.5700(5) 0.8018(4) 0.1622(3) 0.0403(18) Uani 1 1 d . . . C28 C 0.4347(6) 0.6217(5) 0.1831(5) 0.063(2) Uani 1 1 d . . . H28 H 0.3962 0.6311 0.1340 0.076 Uiso 1 1 calc R . . C22 C 0.5449(6) 0.8874(4) -0.1162(5) 0.057(2) Uani 1 1 d . . . H22 H 0.6124 0.8769 -0.0842 0.068 Uiso 1 1 calc R . . C23 C 0.4714(5) 0.6836(4) 0.2281(4) 0.0441(18) Uani 1 1 d . . . C18 C 0.3517(7) 0.8717(4) -0.1512(4) 0.060(2) Uani 1 1 d . . . H18 H 0.2882 0.8504 -0.1427 0.072 Uiso 1 1 calc R . . C30 C 0.5601(6) 0.8559(4) 0.3236(4) 0.053(2) Uani 1 1 d . . . H30 H 0.6213 0.8295 0.3170 0.063 Uiso 1 1 calc R . . C7 C 0.5951(5) 0.8754(4) 0.1306(4) 0.0471(19) Uani 1 1 d . . . H7 H 0.5477 0.9170 0.1169 0.056 Uiso 1 1 calc R . . C33 C 0.3842(7) 0.9384(5) 0.3427(5) 0.065(2) Uani 1 1 d . . . H33 H 0.3247 0.9677 0.3478 0.079 Uiso 1 1 calc R . . C2 C 0.3261(6) 0.8887(4) 0.0409(4) 0.0479(19) Uani 1 1 d . . . H2 H 0.3793 0.9263 0.0569 0.057 Uiso 1 1 calc R . . C24 C 0.5266(6) 0.6671(5) 0.3021(4) 0.063(2) Uani 1 1 d . . . H24 H 0.5522 0.7073 0.3354 0.076 Uiso 1 1 calc R . . C14 C 0.3511(7) 0.5450(5) -0.1228(5) 0.068(2) Uani 1 1 d . . . H14 H 0.3297 0.4958 -0.1411 0.082 Uiso 1 1 calc R . . C10 C 0.6642(6) 0.7560(5) 0.1749(4) 0.053(2) Uani 1 1 d . . . H10 H 0.6726 0.7067 0.1961 0.064 Uiso 1 1 calc R . . C19 C 0.3453(9) 0.9204(5) -0.2115(5) 0.076(3) Uani 1 1 d . . . H19 H 0.2780 0.9322 -0.2430 0.091 Uiso 1 1 calc R . . C21 C 0.5381(9) 0.9361(5) -0.1768(6) 0.077(3) Uani 1 1 d . . . H21 H 0.6009 0.9587 -0.1852 0.093 Uiso 1 1 calc R . . C3 C 0.2158(6) 0.8943(5) 0.0455(4) 0.057(2) Uani 1 1 d . . . H3 H 0.1830 0.9359 0.0637 0.069 Uiso 1 1 calc R . . C32 C 0.4811(9) 0.9449(5) 0.3949(5) 0.072(3) Uani 1 1 d . . . H32 H 0.4867 0.9764 0.4368 0.086 Uiso 1 1 calc R . . C8 C 0.7048(6) 0.8722(6) 0.1244(4) 0.060(2) Uani 1 1 d . . . H8 H 0.7431 0.9113 0.1071 0.072 Uiso 1 1 calc R . . C31 C 0.5704(7) 0.9042(5) 0.3847(4) 0.063(2) Uani 1 1 d . . . H31 H 0.6373 0.9094 0.4189 0.076 Uiso 1 1 calc R . . C25 C 0.5430(8) 0.5915(5) 0.3258(5) 0.080(3) Uani 1 1 d . . . H25 H 0.5799 0.5815 0.3752 0.096 Uiso 1 1 calc R . . C13 C 0.3935(6) 0.5573(5) -0.0468(4) 0.061(2) Uani 1 1 d . . . H13 H 0.3993 0.5159 -0.0135 0.073 Uiso 1 1 calc R . . C15 C 0.3413(6) 0.6081(5) -0.1709(4) 0.058(2) Uani 1 1 d . . . H15 H 0.3136 0.6011 -0.2222 0.070 Uiso 1 1 calc R . . C20 C 0.4387(11) 0.9516(5) -0.2252(5) 0.088(3) Uani 1 1 d . . . H20 H 0.4349 0.9831 -0.2669 0.105 Uiso 1 1 calc R . . C26 C 0.5071(8) 0.5311(5) 0.2792(6) 0.088(3) Uani 1 1 d . . . H26 H 0.5199 0.4804 0.2963 0.105 Uiso 1 1 calc R . . C27 C 0.4517(8) 0.5455(5) 0.2067(6) 0.076(3) Uani 1 1 d . . . H27 H 0.4260 0.5049 0.1739 0.091 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C40 0.036(5) 0.112(7) 0.067(6) -0.006(5) 0.032(4) -0.010(5) C38 0.047(5) 0.123(8) 0.064(6) -0.035(5) 0.027(4) 0.002(5) C37 0.037(5) 0.135(8) 0.071(6) 0.008(5) 0.028(5) 0.013(5) C35 0.056(6) 0.118(7) 0.059(6) 0.021(5) 0.028(5) -0.004(5) C39 0.058(6) 0.114(8) 0.092(7) 0.015(6) 0.034(5) 0.018(6) C36 0.063(6) 0.119(8) 0.077(7) -0.004(6) 0.016(5) -0.025(6) Co1 0.0247(6) 0.0757(7) 0.0242(6) -0.0063(5) 0.0076(4) -0.0042(5) Co2 0.0238(6) 0.0670(7) 0.0262(6) 0.0002(4) 0.0070(4) 0.0003(5) P2 0.0288(10) 0.0607(12) 0.0215(10) -0.0006(8) 0.0074(8) 0.0016(9) P1 0.0329(11) 0.0570(12) 0.0200(10) -0.0009(8) 0.0067(8) -0.0030(9) P3 0.0310(11) 0.0864(16) 0.0382(13) -0.0057(10) 0.0151(9) 0.0005(10) P4 0.0293(11) 0.0906(16) 0.0415(13) 0.0009(11) 0.0121(9) -0.0058(11) C9 0.024(4) 0.135(8) 0.028(5) -0.020(5) 0.015(4) -0.002(5) C29 0.035(4) 0.061(5) 0.028(4) 0.002(3) 0.017(3) -0.005(4) C4 0.032(4) 0.094(6) 0.035(5) 0.000(4) 0.015(4) 0.010(5) C11 0.026(4) 0.061(5) 0.028(4) -0.003(4) 0.006(3) 0.000(3) C16 0.051(5) 0.061(5) 0.031(5) -0.007(4) 0.002(4) 0.006(4) C34 0.046(5) 0.068(5) 0.044(5) -0.011(4) 0.027(4) -0.018(4) C17 0.048(5) 0.059(5) 0.024(4) 0.000(3) 0.015(4) 0.002(4) C12 0.055(5) 0.060(5) 0.030(4) 0.002(4) 0.010(4) 0.001(4) C5 0.037(5) 0.068(5) 0.031(4) -0.001(4) -0.005(4) -0.005(4) C1 0.033(4) 0.053(4) 0.022(4) 0.001(3) 0.001(3) -0.003(4) C6 0.031(4) 0.070(5) 0.017(4) -0.008(3) 0.002(3) -0.006(4) C28 0.065(6) 0.077(6) 0.046(5) -0.004(5) 0.011(4) 0.010(5) C22 0.058(5) 0.061(5) 0.064(6) -0.001(4) 0.039(4) 0.002(4) C23 0.032(4) 0.063(5) 0.041(5) -0.008(4) 0.018(4) -0.002(4) C18 0.068(6) 0.074(5) 0.034(5) 0.012(4) 0.005(4) -0.004(5) C30 0.054(5) 0.064(5) 0.035(5) 0.001(4) 0.002(4) -0.001(4) C7 0.039(5) 0.071(5) 0.032(4) -0.016(4) 0.010(3) -0.008(4) C33 0.069(6) 0.073(6) 0.064(6) -0.022(5) 0.033(5) -0.012(5) C2 0.042(5) 0.060(5) 0.041(5) 0.007(4) 0.008(4) 0.001(4) C24 0.062(6) 0.068(6) 0.047(5) 0.005(4) -0.013(4) 0.000(5) C14 0.078(6) 0.061(6) 0.060(6) -0.012(5) 0.005(5) -0.001(5) C10 0.028(4) 0.102(6) 0.027(4) 0.004(4) -0.001(3) 0.014(4) C19 0.102(8) 0.071(6) 0.050(6) 0.015(5) 0.008(5) -0.003(6) C21 0.124(9) 0.051(5) 0.081(7) 0.004(5) 0.073(7) -0.004(6) C3 0.055(5) 0.073(6) 0.050(5) 0.005(4) 0.025(4) 0.023(5) C32 0.104(8) 0.074(6) 0.049(6) -0.018(5) 0.042(6) -0.021(6) C8 0.045(5) 0.101(7) 0.037(5) -0.030(5) 0.017(4) -0.022(5) C31 0.084(7) 0.074(6) 0.024(5) -0.002(4) -0.003(4) -0.010(5) C25 0.088(7) 0.076(7) 0.065(6) 0.019(6) -0.002(5) 0.004(6) C13 0.067(6) 0.060(5) 0.050(6) 0.017(4) 0.005(4) 0.004(5) C15 0.061(5) 0.077(6) 0.028(4) -0.007(4) -0.005(4) 0.003(5) C20 0.147(11) 0.072(7) 0.050(6) 0.011(5) 0.036(7) 0.006(7) C26 0.105(8) 0.059(6) 0.091(8) 0.011(6) 0.006(6) 0.006(6) C27 0.088(7) 0.059(6) 0.086(8) -0.009(5) 0.032(6) 0.001(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 C40 P3 1.845(7) . ? C38 P3 1.846(8) . ? C37 P4 1.845(8) . ? C35 P4 1.831(8) . ? C39 P3 1.817(8) . ? C36 P4 1.838(8) . ? Co1 C9 2.030(7) . ? Co1 C10 2.095(7) . ? Co1 C8 2.095(7) . ? Co1 C7 2.103(7) . ? Co1 C6 2.106(6) . ? Co1 P1 2.127(2) . ? Co1 P3 2.130(2) . ? Co2 C4 2.044(7) . ? Co2 C1 2.080(6) . ? Co2 C5 2.091(7) . ? Co2 C2 2.093(7) . ? Co2 C3 2.123(7) . ? Co2 P2 2.126(2) . ? Co2 P4 2.133(2) . ? P2 C6 1.822(7) . ? P2 C29 1.850(7) . ? P2 C23 1.859(8) . ? P1 C1 1.814(7) . ? P1 C11 1.849(7) . ? P1 C17 1.861(7) . ? C9 C8 1.400(11) . ? C9 C10 1.416(10) . ? C29 C30 1.378(9) . ? C29 C34 1.404(9) . ? C4 C5 1.396(10) . ? C4 C3 1.402(10) . ? C11 C12 1.384(9) . ? C11 C16 1.383(9) . ? C16 C15 1.390(10) . ? C34 C33 1.369(10) . ? C17 C22 1.388(9) . ? C17 C18 1.397(10) . ? C12 C13 1.367(9) . ? C5 C1 1.437(9) . ? C1 C2 1.447(9) . ? C6 C10 1.402(9) . ? C6 C7 1.463(9) . ? C28 C23 1.360(10) . ? C28 C27 1.385(11) . ? C22 C21 1.380(11) . ? C23 C24 1.398(9) . ? C18 C19 1.374(10) . ? C30 C31 1.377(10) . ? C7 C8 1.420(9) . ? C33 C32 1.366(11) . ? C2 C3 1.422(10) . ? C24 C25 1.376(10) . ? C14 C13 1.384(10) . ? C14 C15 1.388(10) . ? C19 C20 1.375(13) . ? C21 C20 1.380(13) . ? C32 C31 1.381(11) . ? C25 C26 1.355(11) . ? C26 C27 1.367(11) . ? 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 C9 Co1 C10 40.1(3) . . ? C9 Co1 C8 39.6(3) . . ? C10 Co1 C8 67.2(3) . . ? C9 Co1 C7 66.3(3) . . ? C10 Co1 C7 66.8(3) . . ? C8 Co1 C7 39.5(3) . . ? C9 Co1 C6 66.5(3) . . ? C10 Co1 C6 39.0(3) . . ? C8 Co1 C6 67.4(3) . . ? C7 Co1 C6 40.7(2) . . ? C9 Co1 P1 167.3(2) . . ? C10 Co1 P1 135.5(2) . . ? C8 Co1 P1 130.4(3) . . ? C7 Co1 P1 101.0(2) . . ? C6 Co1 P1 103.51(19) . . ? C9 Co1 P3 92.4(2) . . ? C10 Co1 P3 109.8(2) . . ? C8 Co1 P3 111.8(2) . . ? C7 Co1 P3 151.2(2) . . ? C6 Co1 P3 148.2(2) . . ? P1 Co1 P3 99.89(10) . . ? C4 Co2 C1 67.2(3) . . ? C4 Co2 C5 39.4(3) . . ? C1 Co2 C5 40.3(3) . . ? C4 Co2 C2 66.0(3) . . ? C1 Co2 C2 40.6(2) . . ? C5 Co2 C2 66.8(3) . . ? C4 Co2 C3 39.3(3) . . ? C1 Co2 C3 67.6(3) . . ? C5 Co2 C3 66.5(3) . . ? C2 Co2 C3 39.4(3) . . ? C4 Co2 P2 168.7(2) . . ? C1 Co2 P2 103.16(19) . . ? C5 Co2 P2 135.7(2) . . ? C2 Co2 P2 102.9(2) . . ? C3 Co2 P2 132.7(2) . . ? C4 Co2 P4 92.6(2) . . ? C1 Co2 P4 149.68(19) . . ? C5 Co2 P4 110.0(2) . . ? C2 Co2 P4 150.5(2) . . ? C3 Co2 P4 111.3(2) . . ? P2 Co2 P4 98.58(10) . . ? C6 P2 C29 98.8(3) . . ? C6 P2 C23 99.6(3) . . ? C29 P2 C23 103.5(3) . . ? C6 P2 Co2 119.4(2) . . ? C29 P2 Co2 116.2(2) . . ? C23 P2 Co2 116.4(2) . . ? C1 P1 C11 99.2(3) . . ? C1 P1 C17 98.4(3) . . ? C11 P1 C17 103.2(3) . . ? C1 P1 Co1 118.8(2) . . ? C11 P1 Co1 115.7(2) . . ? C17 P1 Co1 118.2(2) . . ? C39 P3 C38 98.9(4) . . ? C39 P3 C40 100.3(4) . . ? C38 P3 C40 99.2(4) . . ? C39 P3 Co1 115.9(3) . . ? C38 P3 Co1 124.1(3) . . ? C40 P3 Co1 114.6(3) . . ? C35 P4 C36 100.3(4) . . ? C35 P4 C37 99.3(4) . . ? C36 P4 C37 100.8(4) . . ? C35 P4 Co2 124.2(3) . . ? C36 P4 Co2 114.2(3) . . ? C37 P4 Co2 114.5(3) . . ? C8 C9 C10 110.8(7) . . ? C8 C9 Co1 72.7(4) . . ? C10 C9 Co1 72.4(4) . . ? C30 C29 C34 116.3(6) . . ? C30 C29 P2 124.9(6) . . ? C34 C29 P2 118.7(5) . . ? C5 C4 C3 111.4(7) . . ? C5 C4 Co2 72.1(4) . . ? C3 C4 Co2 73.4(4) . . ? C12 C11 C16 117.8(7) . . ? C12 C11 P1 116.1(5) . . ? C16 C11 P1 126.0(6) . . ? C11 C16 C15 120.8(7) . . ? C33 C34 C29 121.7(7) . . ? C22 C17 C18 118.2(7) . . ? C22 C17 P1 119.2(6) . . ? C18 C17 P1 122.6(6) . . ? C13 C12 C11 121.7(7) . . ? C4 C5 C1 107.3(6) . . ? C4 C5 Co2 68.5(4) . . ? C1 C5 Co2 69.4(4) . . ? C5 C1 C2 106.1(6) . . ? C5 C1 P1 127.6(5) . . ? C2 C1 P1 125.5(5) . . ? C5 C1 Co2 70.3(4) . . ? C2 C1 Co2 70.2(4) . . ? P1 C1 Co2 132.0(3) . . ? C10 C6 C7 107.4(6) . . ? C10 C6 P2 128.7(6) . . ? C7 C6 P2 123.6(5) . . ? C10 C6 Co1 70.1(4) . . ? C7 C6 Co1 69.6(4) . . ? P2 C6 Co1 130.4(3) . . ? C23 C28 C27 123.5(8) . . ? C21 C22 C17 120.4(8) . . ? C28 C23 C24 116.5(7) . . ? C28 C23 P2 118.2(6) . . ? C24 C23 P2 125.2(6) . . ? C19 C18 C17 121.2(8) . . ? C31 C30 C29 122.2(8) . . ? C8 C7 C6 107.8(7) . . ? C8 C7 Co1 70.0(4) . . ? C6 C7 Co1 69.8(4) . . ? C32 C33 C34 120.6(8) . . ? C3 C2 C1 109.2(7) . . ? C3 C2 Co2 71.4(4) . . ? C1 C2 Co2 69.2(4) . . ? C25 C24 C23 120.2(8) . . ? C13 C14 C15 118.3(7) . . ? C6 C10 C9 107.2(7) . . ? C6 C10 Co1 70.9(4) . . ? C9 C10 Co1 67.5(4) . . ? C20 C19 C18 119.9(9) . . ? C20 C21 C22 120.5(9) . . ? C4 C3 C2 105.9(7) . . ? C4 C3 Co2 67.3(4) . . ? C2 C3 Co2 69.1(4) . . ? C33 C32 C31 119.3(7) . . ? C9 C8 C7 106.6(7) . . ? C9 C8 Co1 67.7(4) . . ? C7 C8 Co1 70.5(4) . . ? C30 C31 C32 119.8(8) . . ? C26 C25 C24 121.8(8) . . ? C12 C13 C14 120.8(7) . . ? C14 C15 C16 120.5(7) . . ? C19 C20 C21 119.8(9) . . ? C25 C26 C27 119.3(8) . . ? C26 C27 C28 118.7(8) . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.000 0.000 111 4 ' ' 2 0.000 0.500 0.500 12 0 ' ' 3 0.250 0.024 0.448 9 0 ' ' 4 0.250 0.524 0.052 9 0 ' ' 5 0.500 0.500 0.500 111 4 ' ' 6 0.500 0.000 1.000 12 0 ' ' 7 0.750 0.476 0.948 9 0 ' ' 8 0.750 0.976 0.552 9 0 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 21.63 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.843 _refine_diff_density_min -0.600 _refine_diff_density_rms 0.119 # Attachment '- 4.cif' data_4 _database_code_depnum_ccdc_archive 'CCDC 780558' #TrackingRef '- 4.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H40 Co Ni P2' _chemical_formula_sum 'C42 H40 Co Ni P2' _chemical_formula_weight 724.32 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 '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 8.994(4) _cell_length_b 9.975(5) _cell_length_c 20.652(11) _cell_angle_alpha 87.715(12) _cell_angle_beta 83.420(12) _cell_angle_gamma 65.95(2) _cell_volume 1680.8(14) _cell_formula_units_Z 2 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 329 _cell_measurement_theta_min 1.99 _cell_measurement_theta_max 23.41 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.431 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 754 _exptl_absorpt_coefficient_mu 1.179 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7337 _exptl_absorpt_correction_T_max 0.7732 _exptl_absorpt_process_details ? _exptl_special_details ; Theta(max) is low. The reason is that the quality of the crystal is not very good, and the diffraction data is relatively weak. ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7239 _diffrn_reflns_av_R_equivalents 0.1219 _diffrn_reflns_av_sigmaI/netI 0.3111 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 23.41 _reflns_number_total 4817 _reflns_number_gt 1679 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The restrains 'Delu' were used for 'Large Hirshfeld Difference C24 -- C25'. ; _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^)+(0.0861P)^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 4817 _refine_ls_number_parameters 415 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.2495 _refine_ls_R_factor_gt 0.0921 _refine_ls_wR_factor_ref 0.2491 _refine_ls_wR_factor_gt 0.1630 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.936 _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 Co1 Co 0.6062(3) -0.1020(2) 0.31221(10) 0.0511(7) Uani 1 1 d . . . Ni1 Ni 0.8003(2) 0.1885(2) 0.21967(9) 0.0436(7) Uani 1 1 d . . . P5 P 0.7356(5) 0.0304(4) 0.17180(18) 0.0434(12) Uani 1 1 d . . . P7 P 0.7446(5) 0.1666(4) 0.32443(19) 0.0430(12) Uani 1 1 d . . . C1 C 0.6552(19) 0.0836(15) 0.0926(7) 0.046(4) Uani 1 1 d . . . C2 C 0.486(2) 0.1456(17) 0.0880(7) 0.062(5) Uani 1 1 d . . . H2 H 0.4131 0.1495 0.1245 0.075 Uiso 1 1 calc R . . C3 C 0.426(2) 0.2018(17) 0.0283(9) 0.077(6) Uani 1 1 d . . . H3 H 0.3133 0.2469 0.0269 0.093 Uiso 1 1 calc R . . C4 C 0.523(3) 0.1933(18) -0.0261(8) 0.080(7) Uani 1 1 d . . . H4 H 0.4806 0.2259 -0.0655 0.096 Uiso 1 1 calc R . . C5 C 0.690(2) 0.1345(19) -0.0226(8) 0.068(5) Uani 1 1 d . . . H5 H 0.7621 0.1299 -0.0595 0.081 Uiso 1 1 calc R . . C6 C 0.7494(19) 0.0831(15) 0.0358(7) 0.051(5) Uani 1 1 d . . . H6 H 0.8622 0.0449 0.0369 0.061 Uiso 1 1 calc R . . C7 C 0.9098(19) -0.1511(16) 0.1478(7) 0.049(5) Uani 1 1 d . . . C8 C 1.0484(19) -0.1875(16) 0.1803(7) 0.052(5) Uani 1 1 d . . . H8 H 1.0498 -0.1240 0.2118 0.063 Uiso 1 1 calc R . . C9 C 1.184(2) -0.3171(18) 0.1661(8) 0.066(6) Uani 1 1 d . . . H9 H 1.2746 -0.3443 0.1890 0.079 Uiso 1 1 calc R . . C10 C 1.180(2) -0.4010(17) 0.1194(9) 0.067(6) Uani 1 1 d . . . H10 H 1.2715 -0.4882 0.1094 0.080 Uiso 1 1 calc R . . C11 C 1.049(2) -0.3658(16) 0.0850(7) 0.057(5) Uani 1 1 d . . . H11 H 1.0527 -0.4279 0.0520 0.068 Uiso 1 1 calc R . . C12 C 0.9110(18) -0.2374(17) 0.0993(7) 0.050(4) Uani 1 1 d . . . H12 H 0.8212 -0.2117 0.0758 0.060 Uiso 1 1 calc R . . C13 C 0.5961(19) -0.0392(18) 0.2132(7) 0.052(5) Uani 1 1 d . . . C14 C 0.4479(18) 0.0440(18) 0.2541(7) 0.052(5) Uani 1 1 d . . . H14 H 0.4066 0.1448 0.2611 0.063 Uiso 1 1 calc R . . C15 C 0.3726(19) -0.049(2) 0.2827(8) 0.071(6) Uani 1 1 d . . . H15 H 0.2759 -0.0207 0.3106 0.085 Uiso 1 1 calc R . . C16 C 0.475(2) -0.1938(19) 0.2601(8) 0.066(5) Uani 1 1 d . . . H16 H 0.4570 -0.2781 0.2703 0.079 Uiso 1 1 calc R . . C17 C 0.612(2) -0.1863(19) 0.2181(8) 0.058(5) Uani 1 1 d . . . H17 H 0.6982 -0.2663 0.1975 0.070 Uiso 1 1 calc R . . C18 C 0.7227(18) 0.0026(15) 0.3606(7) 0.040(4) Uani 1 1 d . . . C19 C 0.8395(18) -0.1464(17) 0.3415(7) 0.055(5) Uani 1 1 d . . . H19 H 0.9368 -0.1733 0.3141 0.066 Uiso 1 1 calc R . . C20 C 0.771(2) -0.2433(18) 0.3746(8) 0.065(5) Uani 1 1 d . . . H20 H 0.8158 -0.3453 0.3721 0.078 Uiso 1 1 calc R . . C21 C 0.622(2) -0.152(2) 0.4116(7) 0.061(5) Uani 1 1 d . . . H21 H 0.5551 -0.1870 0.4378 0.073 Uiso 1 1 calc R . . C22 C 0.590(2) -0.0056(18) 0.4040(7) 0.052(4) Uani 1 1 d . . . H22 H 0.5000 0.0730 0.4232 0.063 Uiso 1 1 calc R . . C23 C 0.5499(18) 0.3079(15) 0.3578(7) 0.039(4) Uani 1 1 d . . . C24 C 0.5172(17) 0.3409(15) 0.4224(8) 0.051(5) Uani 1 1 d U . . H24 H 0.5932 0.2870 0.4507 0.062 Uiso 1 1 calc R . . C25 C 0.368(2) 0.457(2) 0.4475(8) 0.074(6) Uani 1 1 d U . . H25 H 0.3470 0.4799 0.4917 0.088 Uiso 1 1 calc R . . C26 C 0.256(2) 0.5346(18) 0.4052(11) 0.075(6) Uani 1 1 d . . . H26 H 0.1612 0.6141 0.4207 0.090 Uiso 1 1 calc R . . C27 C 0.282(2) 0.4963(19) 0.3400(9) 0.064(5) Uani 1 1 d . . . H27 H 0.2021 0.5423 0.3120 0.077 Uiso 1 1 calc R . . C28 C 0.4303(18) 0.3871(17) 0.3185(8) 0.051(4) Uani 1 1 d . . . H28 H 0.4517 0.3650 0.2742 0.062 Uiso 1 1 calc R . . C29 C 0.8810(18) 0.1875(18) 0.3797(7) 0.045(4) Uani 1 1 d . . . C30 C 0.879(2) 0.321(2) 0.3892(8) 0.066(5) Uani 1 1 d . . . H30 H 0.8035 0.4026 0.3703 0.079 Uiso 1 1 calc R . . C31 C 0.990(3) 0.336(2) 0.4278(8) 0.071(6) Uani 1 1 d . . . H31 H 0.9840 0.4294 0.4357 0.085 Uiso 1 1 calc R . . C32 C 1.103(2) 0.220(3) 0.4529(8) 0.072(6) Uani 1 1 d . . . H32 H 1.1802 0.2314 0.4759 0.086 Uiso 1 1 calc R . . C33 C 1.106(2) 0.087(2) 0.4452(9) 0.076(6) Uani 1 1 d . . . H33 H 1.1788 0.0060 0.4660 0.092 Uiso 1 1 calc R . . C34 C 1.001(2) 0.0705(19) 0.4060(8) 0.059(5) Uani 1 1 d . . . H34 H 1.0108 -0.0237 0.3971 0.071 Uiso 1 1 calc R . . C35 C 1.040(2) 0.1775(19) 0.2064(9) 0.066(5) Uani 1 1 d . . . H35 H 1.0649 0.0961 0.2335 0.079 Uiso 1 1 calc R . . C36 C 0.9962(19) 0.1628(16) 0.1458(8) 0.056(5) Uani 1 1 d . . . H36 H 0.9945 0.0741 0.1344 0.067 Uiso 1 1 calc R . . C37 C 0.952(2) 0.2851(19) 0.0985(8) 0.072(6) Uani 1 1 d . . . H37A H 0.9861 0.2442 0.0548 0.087 Uiso 1 1 calc R . . H37B H 1.0133 0.3434 0.1050 0.087 Uiso 1 1 calc R . . C38 C 0.768(2) 0.3873(17) 0.1037(8) 0.074(6) Uani 1 1 d . . . H38A H 0.7145 0.3515 0.0747 0.088 Uiso 1 1 calc R . . H38B H 0.7553 0.4850 0.0897 0.088 Uiso 1 1 calc R . . C39 C 0.6839(19) 0.3957(15) 0.1742(8) 0.058(5) Uani 1 1 d . . . H39 H 0.5851 0.3853 0.1803 0.070 Uiso 1 1 calc R . . C40 C 0.746(2) 0.4170(14) 0.2267(7) 0.042(4) Uani 1 1 d . . . H40 H 0.6917 0.4131 0.2673 0.050 Uiso 1 1 calc R . . C41 C 0.896(2) 0.4465(18) 0.2253(8) 0.070(6) Uani 1 1 d . . . H41A H 0.8812 0.5146 0.2603 0.084 Uiso 1 1 calc R . . H41B H 0.9114 0.4930 0.1844 0.084 Uiso 1 1 calc R . . C42 C 1.0500(19) 0.3080(18) 0.2328(8) 0.063(5) Uani 1 1 d . . . H42A H 1.1441 0.3206 0.2102 0.076 Uiso 1 1 calc R . . H42B H 1.0662 0.2930 0.2786 0.076 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0577(16) 0.0430(15) 0.0454(15) 0.0051(11) -0.0074(12) -0.0131(12) Ni1 0.0494(13) 0.0328(12) 0.0375(13) 0.0011(9) -0.0035(10) -0.0056(10) P5 0.049(3) 0.040(3) 0.032(3) 0.002(2) -0.005(2) -0.008(2) P7 0.042(3) 0.035(3) 0.045(3) -0.002(2) -0.003(2) -0.009(2) C1 0.044(11) 0.034(9) 0.051(11) 0.008(8) -0.012(9) -0.005(8) C2 0.052(12) 0.074(13) 0.039(11) -0.017(9) 0.004(9) -0.004(10) C3 0.083(15) 0.057(13) 0.070(14) 0.006(11) -0.047(13) 0.004(10) C4 0.14(2) 0.052(12) 0.017(10) 0.008(9) -0.002(12) -0.012(13) C5 0.085(15) 0.072(14) 0.035(12) 0.004(9) -0.009(11) -0.020(12) C6 0.052(11) 0.046(10) 0.035(10) 0.006(8) -0.001(9) -0.002(8) C7 0.048(11) 0.042(10) 0.034(10) 0.000(8) 0.019(9) 0.000(8) C8 0.048(11) 0.039(10) 0.052(11) -0.006(8) -0.005(9) 0.001(9) C9 0.080(14) 0.045(12) 0.048(12) -0.008(9) -0.012(10) 0.003(10) C10 0.063(13) 0.029(11) 0.076(15) 0.025(10) 0.006(11) 0.008(10) C11 0.085(14) 0.033(11) 0.039(11) -0.019(8) 0.015(10) -0.015(10) C12 0.054(11) 0.046(11) 0.031(10) -0.004(8) 0.004(8) -0.003(9) C13 0.063(12) 0.056(12) 0.029(10) 0.002(8) -0.003(9) -0.018(10) C14 0.039(10) 0.057(11) 0.044(11) 0.009(9) -0.006(9) -0.002(9) C15 0.038(11) 0.103(17) 0.063(13) 0.022(12) 0.007(10) -0.026(11) C16 0.082(14) 0.050(13) 0.081(14) -0.003(10) -0.015(12) -0.040(12) C17 0.054(12) 0.061(13) 0.072(13) 0.033(10) -0.030(10) -0.033(10) C18 0.043(10) 0.029(9) 0.052(11) 0.018(8) -0.025(9) -0.015(8) C19 0.050(11) 0.044(11) 0.064(12) 0.002(9) 0.003(9) -0.015(9) C20 0.075(14) 0.045(12) 0.080(14) 0.027(10) -0.032(11) -0.025(11) C21 0.077(14) 0.074(14) 0.035(11) 0.003(10) -0.012(10) -0.032(12) C22 0.060(12) 0.043(11) 0.054(12) 0.004(9) -0.013(10) -0.019(9) C23 0.058(11) 0.030(9) 0.022(9) -0.008(7) 0.007(8) -0.013(8) C24 0.039(10) 0.026(9) 0.070(13) -0.010(9) 0.002(9) 0.004(8) C25 0.108(17) 0.079(15) 0.052(13) -0.008(11) -0.007(12) -0.056(13) C26 0.050(13) 0.042(12) 0.107(17) -0.001(12) -0.005(13) 0.006(9) C27 0.052(13) 0.070(14) 0.064(14) 0.006(10) -0.011(11) -0.018(11) C28 0.044(11) 0.048(11) 0.056(11) -0.007(9) -0.007(9) -0.010(9) C29 0.044(10) 0.043(11) 0.042(10) -0.001(8) -0.005(8) -0.013(9) C30 0.071(14) 0.068(14) 0.058(12) 0.003(10) -0.021(10) -0.025(11) C31 0.088(16) 0.064(14) 0.064(13) -0.013(11) -0.001(12) -0.033(13) C32 0.062(14) 0.110(18) 0.046(12) -0.007(13) -0.010(10) -0.035(14) C33 0.066(15) 0.087(17) 0.071(15) 0.013(12) -0.016(12) -0.024(13) C34 0.057(12) 0.061(13) 0.051(12) -0.015(9) -0.001(10) -0.016(10) C35 0.067(13) 0.058(13) 0.075(14) 0.010(11) -0.013(11) -0.028(10) C36 0.069(12) 0.027(10) 0.068(13) 0.017(9) -0.002(10) -0.020(9) C37 0.086(15) 0.070(13) 0.055(12) 0.001(10) 0.016(11) -0.031(12) C38 0.095(15) 0.045(11) 0.062(13) 0.019(9) -0.011(11) -0.010(11) C39 0.049(11) 0.032(10) 0.073(14) 0.016(9) 0.002(11) 0.000(8) C40 0.074(13) 0.014(8) 0.033(10) 0.005(7) -0.008(9) -0.012(8) C41 0.110(16) 0.051(12) 0.070(13) -0.015(10) 0.027(12) -0.064(13) C42 0.053(12) 0.059(13) 0.081(13) -0.010(10) -0.004(10) -0.026(10) _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 Co1 C14 2.037(14) . ? Co1 C18 2.097(14) . ? Co1 C21 2.100(15) . ? Co1 C15 2.104(16) . ? Co1 C20 2.107(15) . ? Co1 C13 2.115(14) . ? Co1 C19 2.117(15) . ? Co1 C22 2.123(15) . ? Co1 C17 2.135(17) . ? Co1 C16 2.155(16) . ? Ni1 C35 2.096(17) . ? Ni1 C36 2.132(15) . ? Ni1 C39 2.134(14) . ? Ni1 C40 2.136(13) . ? Ni1 P7 2.187(5) . ? Ni1 P5 2.192(5) . ? P5 C13 1.790(17) . ? P5 C1 1.836(15) . ? P5 C7 1.887(14) . ? P7 C23 1.821(14) . ? P7 C29 1.844(16) . ? P7 C18 1.845(14) . ? C1 C6 1.364(18) . ? C1 C2 1.406(19) . ? C2 C3 1.405(19) . ? C2 H2 0.9300 . ? C3 C4 1.33(2) . ? C3 H3 0.9300 . ? C4 C5 1.38(2) . ? C4 H4 0.9300 . ? C5 C6 1.368(18) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.343(19) . ? C7 C8 1.392(19) . ? C8 C9 1.380(18) . ? C8 H8 0.9300 . ? C9 C10 1.31(2) . ? C9 H9 0.9300 . ? C10 C11 1.36(2) . ? C10 H10 0.9300 . ? C11 C12 1.387(18) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C17 1.41(2) . ? C13 C14 1.441(18) . ? C14 C15 1.43(2) . ? C14 H14 0.9300 . ? C15 C16 1.42(2) . ? C15 H15 0.9300 . ? C16 C17 1.45(2) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C22 1.434(18) . ? C18 C19 1.465(17) . ? C19 C20 1.454(19) . ? C19 H19 0.9300 . ? C20 C21 1.43(2) . ? C20 H20 0.9300 . ? C21 C22 1.37(2) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.356(17) . ? C23 C28 1.376(18) . ? C24 C25 1.43(2) . ? C24 H24 0.9300 . ? C25 C26 1.37(2) . ? C25 H25 0.9300 . ? C26 C27 1.38(2) . ? C26 H26 0.9300 . ? C27 C28 1.373(19) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.34(2) . ? C29 C34 1.370(19) . ? C30 C31 1.41(2) . ? C30 H30 0.9300 . ? C31 C32 1.33(2) . ? C31 H31 0.9300 . ? C32 C33 1.33(2) . ? C32 H32 0.9300 . ? C33 C34 1.38(2) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 C36 1.385(19) . ? C35 C42 1.47(2) . ? C35 H35 0.9300 . ? C36 C37 1.483(19) . ? C36 H36 0.9300 . ? C37 C38 1.54(2) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.551(19) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.338(18) . ? C39 H39 0.9300 . ? C40 C41 1.49(2) . ? C40 H40 0.9300 . ? C41 C42 1.52(2) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C14 Co1 C18 109.9(6) . . ? C14 Co1 C21 139.0(7) . . ? C18 Co1 C21 65.0(6) . . ? C14 Co1 C15 40.4(6) . . ? C18 Co1 C15 137.4(7) . . ? C21 Co1 C15 114.2(7) . . ? C14 Co1 C20 176.9(7) . . ? C18 Co1 C20 67.1(6) . . ? C21 Co1 C20 39.6(6) . . ? C15 Co1 C20 141.5(7) . . ? C14 Co1 C13 40.6(5) . . ? C18 Co1 C13 110.7(6) . . ? C21 Co1 C13 175.6(7) . . ? C15 Co1 C13 68.3(6) . . ? C20 Co1 C13 140.4(7) . . ? C14 Co1 C19 137.7(7) . . ? C18 Co1 C19 40.7(5) . . ? C21 Co1 C19 66.5(6) . . ? C15 Co1 C19 177.8(7) . . ? C20 Co1 C19 40.3(5) . . ? C13 Co1 C19 111.0(6) . . ? C14 Co1 C22 110.8(6) . . ? C18 Co1 C22 39.7(5) . . ? C21 Co1 C22 37.9(5) . . ? C15 Co1 C22 111.4(7) . . ? C20 Co1 C22 66.5(6) . . ? C13 Co1 C22 138.2(6) . . ? C19 Co1 C22 67.7(6) . . ? C14 Co1 C17 65.7(6) . . ? C18 Co1 C17 140.2(6) . . ? C21 Co1 C17 145.1(7) . . ? C15 Co1 C17 66.4(6) . . ? C20 Co1 C17 116.9(7) . . ? C13 Co1 C17 38.9(5) . . ? C19 Co1 C17 114.4(6) . . ? C22 Co1 C17 176.5(6) . . ? C14 Co1 C16 65.9(7) . . ? C18 Co1 C16 175.8(6) . . ? C21 Co1 C16 117.5(7) . . ? C15 Co1 C16 39.0(6) . . ? C20 Co1 C16 117.1(7) . . ? C13 Co1 C16 66.7(6) . . ? C19 Co1 C16 142.9(7) . . ? C22 Co1 C16 140.1(7) . . ? C17 Co1 C16 39.6(5) . . ? C35 Ni1 C36 38.2(5) . . ? C35 Ni1 C39 97.5(7) . . ? C36 Ni1 C39 83.3(6) . . ? C35 Ni1 C40 80.8(6) . . ? C36 Ni1 C40 90.0(6) . . ? C39 Ni1 C40 36.5(5) . . ? C35 Ni1 P7 106.1(5) . . ? C36 Ni1 P7 142.9(5) . . ? C39 Ni1 P7 119.6(5) . . ? C40 Ni1 P7 93.6(4) . . ? C35 Ni1 P5 121.1(5) . . ? C36 Ni1 P5 92.1(5) . . ? C39 Ni1 P5 107.2(5) . . ? C40 Ni1 P5 143.0(5) . . ? P7 Ni1 P5 106.28(18) . . ? C13 P5 C1 102.3(7) . . ? C13 P5 C7 98.0(7) . . ? C1 P5 C7 99.2(7) . . ? C13 P5 Ni1 120.8(5) . . ? C1 P5 Ni1 116.8(5) . . ? C7 P5 Ni1 116.0(6) . . ? C23 P7 C29 99.8(7) . . ? C23 P7 C18 99.6(7) . . ? C29 P7 C18 99.4(7) . . ? C23 P7 Ni1 113.2(5) . . ? C29 P7 Ni1 118.2(5) . . ? C18 P7 Ni1 122.8(5) . . ? C6 C1 C2 114.7(14) . . ? C6 C1 P5 124.0(12) . . ? C2 C1 P5 120.8(12) . . ? C3 C2 C1 119.9(16) . . ? C3 C2 H2 120.0 . . ? C1 C2 H2 120.0 . . ? C4 C3 C2 122.9(18) . . ? C4 C3 H3 118.6 . . ? C2 C3 H3 118.6 . . ? C3 C4 C5 118.0(17) . . ? C3 C4 H4 121.0 . . ? C5 C4 H4 121.0 . . ? C6 C5 C4 119.4(17) . . ? C6 C5 H5 120.3 . . ? C4 C5 H5 120.3 . . ? C1 C6 C5 125.0(16) . . ? C1 C6 H6 117.5 . . ? C5 C6 H6 117.5 . . ? C12 C7 C8 120.1(14) . . ? C12 C7 P5 124.1(13) . . ? C8 C7 P5 115.6(12) . . ? C9 C8 C7 120.4(15) . . ? C9 C8 H8 119.8 . . ? C7 C8 H8 119.8 . . ? C10 C9 C8 118.3(17) . . ? C10 C9 H9 120.9 . . ? C8 C9 H9 120.9 . . ? C9 C10 C11 122.7(16) . . ? C9 C10 H10 118.6 . . ? C11 C10 H10 118.6 . . ? C10 C11 C12 120.1(15) . . ? C10 C11 H11 120.0 . . ? C12 C11 H11 120.0 . . ? C7 C12 C11 118.4(15) . . ? C7 C12 H12 120.8 . . ? C11 C12 H12 120.8 . . ? C17 C13 C14 105.0(15) . . ? C17 C13 P5 128.5(13) . . ? C14 C13 P5 126.2(13) . . ? C17 C13 Co1 71.3(9) . . ? C14 C13 Co1 66.8(8) . . ? P5 C13 Co1 121.9(8) . . ? C15 C14 C13 111.0(15) . . ? C15 C14 Co1 72.3(9) . . ? C13 C14 Co1 72.6(8) . . ? C15 C14 H14 124.5 . . ? C13 C14 H14 124.5 . . ? Co1 C14 H14 122.1 . . ? C16 C15 C14 106.4(15) . . ? C16 C15 Co1 72.5(9) . . ? C14 C15 Co1 67.3(8) . . ? C16 C15 H15 126.8 . . ? C14 C15 H15 126.8 . . ? Co1 C15 H15 125.0 . . ? C15 C16 C17 107.7(15) . . ? C15 C16 Co1 68.6(9) . . ? C17 C16 Co1 69.4(9) . . ? C15 C16 H16 126.2 . . ? C17 C16 H16 126.2 . . ? Co1 C16 H16 127.4 . . ? C13 C17 C16 110.0(15) . . ? C13 C17 Co1 69.8(9) . . ? C16 C17 Co1 71.0(9) . . ? C13 C17 H17 125.0 . . ? C16 C17 H17 125.0 . . ? Co1 C17 H17 125.8 . . ? C22 C18 C19 109.0(13) . . ? C22 C18 P7 128.7(12) . . ? C19 C18 P7 121.9(12) . . ? C22 C18 Co1 71.1(9) . . ? C19 C18 Co1 70.4(8) . . ? P7 C18 Co1 119.7(7) . . ? C20 C19 C18 105.4(13) . . ? C20 C19 Co1 69.5(8) . . ? C18 C19 Co1 69.0(8) . . ? C20 C19 H19 127.3 . . ? C18 C19 H19 127.3 . . ? Co1 C19 H19 125.8 . . ? C21 C20 C19 106.7(15) . . ? C21 C20 Co1 69.9(9) . . ? C19 C20 Co1 70.2(8) . . ? C21 C20 H20 126.6 . . ? C19 C20 H20 126.6 . . ? Co1 C20 H20 124.8 . . ? C22 C21 C20 112.0(16) . . ? C22 C21 Co1 72.0(9) . . ? C20 C21 Co1 70.4(8) . . ? C22 C21 H21 124.0 . . ? C20 C21 H21 124.0 . . ? Co1 C21 H21 125.2 . . ? C21 C22 C18 106.8(15) . . ? C21 C22 Co1 70.1(9) . . ? C18 C22 Co1 69.2(8) . . ? C21 C22 H22 126.6 . . ? C18 C22 H22 126.6 . . ? Co1 C22 H22 125.7 . . ? C24 C23 C28 117.1(13) . . ? C24 C23 P7 121.4(12) . . ? C28 C23 P7 121.5(11) . . ? C23 C24 C25 121.0(15) . . ? C23 C24 H24 119.5 . . ? C25 C24 H24 119.5 . . ? C26 C25 C24 118.9(16) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? C25 C26 C27 121.1(16) . . ? C25 C26 H26 119.5 . . ? C27 C26 H26 119.5 . . ? C28 C27 C26 117.0(16) . . ? C28 C27 H27 121.5 . . ? C26 C27 H27 121.5 . . ? C27 C28 C23 124.7(15) . . ? C27 C28 H28 117.6 . . ? C23 C28 H28 117.6 . . ? C30 C29 C34 116.9(16) . . ? C30 C29 P7 119.7(13) . . ? C34 C29 P7 122.9(14) . . ? C29 C30 C31 120.1(17) . . ? C29 C30 H30 119.9 . . ? C31 C30 H30 119.9 . . ? C32 C31 C30 121.0(19) . . ? C32 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C31 C32 C33 120(2) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C32 C33 C34 118.9(18) . . ? C32 C33 H33 120.5 . . ? C34 C33 H33 120.5 . . ? C29 C34 C33 122.6(17) . . ? C29 C34 H34 118.7 . . ? C33 C34 H34 118.7 . . ? C36 C35 C42 127.1(16) . . ? C36 C35 Ni1 72.3(10) . . ? C42 C35 Ni1 112.1(11) . . ? C36 C35 H35 116.5 . . ? C42 C35 H35 116.5 . . ? Ni1 C35 H35 85.3 . . ? C35 C36 C37 121.5(16) . . ? C35 C36 Ni1 69.5(10) . . ? C37 C36 Ni1 112.4(10) . . ? C35 C36 H36 119.3 . . ? C37 C36 H36 119.3 . . ? Ni1 C36 H36 88.2 . . ? C36 C37 C38 114.5(14) . . ? C36 C37 H37A 108.6 . . ? C38 C37 H37A 108.6 . . ? C36 C37 H37B 108.6 . . ? C38 C37 H37B 108.6 . . ? H37A C37 H37B 107.6 . . ? C37 C38 C39 112.0(13) . . ? C37 C38 H38A 109.2 . . ? C39 C38 H38A 109.2 . . ? C37 C38 H38B 109.2 . . ? C39 C38 H38B 109.2 . . ? H38A C38 H38B 107.9 . . ? C40 C39 C38 123.3(16) . . ? C40 C39 Ni1 71.8(8) . . ? C38 C39 Ni1 108.5(9) . . ? C40 C39 H39 118.3 . . ? C38 C39 H39 118.3 . . ? Ni1 C39 H39 89.7 . . ? C39 C40 C41 125.3(16) . . ? C39 C40 Ni1 71.7(9) . . ? C41 C40 Ni1 112.7(10) . . ? C39 C40 H40 117.3 . . ? C41 C40 H40 117.3 . . ? Ni1 C40 H40 85.5 . . ? C40 C41 C42 112.9(13) . . ? C40 C41 H41A 109.0 . . ? C42 C41 H41A 109.0 . . ? C40 C41 H41B 109.0 . . ? C42 C41 H41B 109.0 . . ? H41A C41 H41B 107.8 . . ? C35 C42 C41 112.0(14) . . ? C35 C42 H42A 109.2 . . ? C41 C42 H42A 109.2 . . ? C35 C42 H42B 109.2 . . ? C41 C42 H42B 109.2 . . ? H42A C42 H42B 107.9 . . ? 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 C35 Ni1 P5 C13 141.6(8) . . . . ? C36 Ni1 P5 C13 168.1(7) . . . . ? C39 Ni1 P5 C13 -108.2(8) . . . . ? C40 Ni1 P5 C13 -99.0(9) . . . . ? P7 Ni1 P5 C13 20.7(6) . . . . ? C35 Ni1 P5 C1 -93.0(8) . . . . ? C36 Ni1 P5 C1 -66.5(7) . . . . ? C39 Ni1 P5 C1 17.1(8) . . . . ? C40 Ni1 P5 C1 26.3(10) . . . . ? P7 Ni1 P5 C1 146.1(6) . . . . ? C35 Ni1 P5 C7 23.5(8) . . . . ? C36 Ni1 P5 C7 50.0(7) . . . . ? C39 Ni1 P5 C7 133.6(7) . . . . ? C40 Ni1 P5 C7 142.8(9) . . . . ? P7 Ni1 P5 C7 -97.4(5) . . . . ? C35 Ni1 P7 C23 130.1(7) . . . . ? C36 Ni1 P7 C23 143.4(9) . . . . ? C39 Ni1 P7 C23 21.5(8) . . . . ? C40 Ni1 P7 C23 48.6(7) . . . . ? P5 Ni1 P7 C23 -99.8(6) . . . . ? C35 Ni1 P7 C29 14.0(8) . . . . ? C36 Ni1 P7 C29 27.3(10) . . . . ? C39 Ni1 P7 C29 -94.7(8) . . . . ? C40 Ni1 P7 C29 -67.5(8) . . . . ? P5 Ni1 P7 C29 144.1(6) . . . . ? C35 Ni1 P7 C18 -110.4(7) . . . . ? C36 Ni1 P7 C18 -97.1(9) . . . . ? C39 Ni1 P7 C18 141.0(8) . . . . ? C40 Ni1 P7 C18 168.1(7) . . . . ? P5 Ni1 P7 C18 19.7(6) . . . . ? C13 P5 C1 C6 -150.7(13) . . . . ? C7 P5 C1 C6 -50.3(14) . . . . ? Ni1 P5 C1 C6 75.2(13) . . . . ? C13 P5 C1 C2 37.2(14) . . . . ? C7 P5 C1 C2 137.6(13) . . . . ? Ni1 P5 C1 C2 -96.9(13) . . . . ? C6 C1 C2 C3 0(2) . . . . ? P5 C1 C2 C3 172.3(12) . . . . ? C1 C2 C3 C4 3(3) . . . . ? C2 C3 C4 C5 -4(3) . . . . ? C3 C4 C5 C6 2(3) . . . . ? C2 C1 C6 C5 -1(2) . . . . ? P5 C1 C6 C5 -173.9(13) . . . . ? C4 C5 C6 C1 1(3) . . . . ? C13 P5 C7 C12 75.4(15) . . . . ? C1 P5 C7 C12 -28.5(15) . . . . ? Ni1 P5 C7 C12 -154.5(12) . . . . ? C13 P5 C7 C8 -109.9(12) . . . . ? C1 P5 C7 C8 146.1(12) . . . . ? Ni1 P5 C7 C8 20.1(13) . . . . ? C12 C7 C8 C9 -5(2) . . . . ? P5 C7 C8 C9 -179.4(12) . . . . ? C7 C8 C9 C10 3(3) . . . . ? C8 C9 C10 C11 0(3) . . . . ? C9 C10 C11 C12 -1(3) . . . . ? C8 C7 C12 C11 3(2) . . . . ? P5 C7 C12 C11 177.7(11) . . . . ? C10 C11 C12 C7 -1(2) . . . . ? C1 P5 C13 C17 95.1(14) . . . . ? C7 P5 C13 C17 -6.2(16) . . . . ? Ni1 P5 C13 C17 -133.1(12) . . . . ? C1 P5 C13 C14 -90.9(13) . . . . ? C7 P5 C13 C14 167.7(13) . . . . ? Ni1 P5 C13 C14 40.9(15) . . . . ? C1 P5 C13 Co1 -174.1(8) . . . . ? C7 P5 C13 Co1 84.6(10) . . . . ? Ni1 P5 C13 Co1 -42.3(11) . . . . ? C14 Co1 C13 C17 -116.3(14) . . . . ? C18 Co1 C13 C17 147.0(10) . . . . ? C21 Co1 C13 C17 156(8) . . . . ? C15 Co1 C13 C17 -78.9(10) . . . . ? C20 Co1 C13 C17 68.3(14) . . . . ? C19 Co1 C13 C17 103.3(10) . . . . ? C22 Co1 C13 C17 -177.1(10) . . . . ? C16 Co1 C13 C17 -36.6(9) . . . . ? C18 Co1 C13 C14 -96.7(10) . . . . ? C21 Co1 C13 C14 -87(9) . . . . ? C15 Co1 C13 C14 37.4(10) . . . . ? C20 Co1 C13 C14 -175.4(11) . . . . ? C19 Co1 C13 C14 -140.4(10) . . . . ? C22 Co1 C13 C14 -60.9(14) . . . . ? C17 Co1 C13 C14 116.3(14) . . . . ? C16 Co1 C13 C14 79.6(10) . . . . ? C14 Co1 C13 P5 119.4(15) . . . . ? C18 Co1 C13 P5 22.7(11) . . . . ? C21 Co1 C13 P5 32(9) . . . . ? C15 Co1 C13 P5 156.7(13) . . . . ? C20 Co1 C13 P5 -56.0(15) . . . . ? C19 Co1 C13 P5 -21.0(11) . . . . ? C22 Co1 C13 P5 58.5(14) . . . . ? C17 Co1 C13 P5 -124.4(15) . . . . ? C16 Co1 C13 P5 -161.0(12) . . . . ? C17 C13 C14 C15 -1.0(17) . . . . ? P5 C13 C14 C15 -176.1(11) . . . . ? Co1 C13 C14 C15 -62.6(11) . . . . ? C17 C13 C14 Co1 61.6(10) . . . . ? P5 C13 C14 Co1 -113.5(12) . . . . ? C18 Co1 C14 C15 -141.4(11) . . . . ? C21 Co1 C14 C15 -67.1(15) . . . . ? C20 Co1 C14 C15 -130(13) . . . . ? C13 Co1 C14 C15 119.6(15) . . . . ? C19 Co1 C14 C15 -178.3(10) . . . . ? C22 Co1 C14 C15 -98.9(11) . . . . ? C17 Co1 C14 C15 81.5(11) . . . . ? C16 Co1 C14 C15 37.9(10) . . . . ? C18 Co1 C14 C13 99.0(10) . . . . ? C21 Co1 C14 C13 173.3(11) . . . . ? C15 Co1 C14 C13 -119.6(15) . . . . ? C20 Co1 C14 C13 110(13) . . . . ? C19 Co1 C14 C13 62.2(13) . . . . ? C22 Co1 C14 C13 141.5(10) . . . . ? C17 Co1 C14 C13 -38.1(9) . . . . ? C16 Co1 C14 C13 -81.7(10) . . . . ? C13 C14 C15 C16 0.4(18) . . . . ? Co1 C14 C15 C16 -62.4(11) . . . . ? C13 C14 C15 Co1 62.8(10) . . . . ? C14 Co1 C15 C16 116.9(14) . . . . ? C18 Co1 C15 C16 176.9(10) . . . . ? C21 Co1 C15 C16 -104.5(11) . . . . ? C20 Co1 C15 C16 -66.9(15) . . . . ? C13 Co1 C15 C16 79.4(10) . . . . ? C19 Co1 C15 C16 149(16) . . . . ? C22 Co1 C15 C16 -145.7(10) . . . . ? C17 Co1 C15 C16 37.2(9) . . . . ? C18 Co1 C15 C14 59.9(13) . . . . ? C21 Co1 C15 C14 138.6(10) . . . . ? C20 Co1 C15 C14 176.2(11) . . . . ? C13 Co1 C15 C14 -37.5(9) . . . . ? C19 Co1 C15 C14 32(17) . . . . ? C22 Co1 C15 C14 97.4(10) . . . . ? C17 Co1 C15 C14 -79.7(10) . . . . ? C16 Co1 C15 C14 -116.9(14) . . . . ? C14 C15 C16 C17 0.4(19) . . . . ? Co1 C15 C16 C17 -58.6(11) . . . . ? C14 C15 C16 Co1 59.0(11) . . . . ? C14 Co1 C16 C15 -39.3(9) . . . . ? C18 Co1 C16 C15 -30(10) . . . . ? C21 Co1 C16 C15 95.2(11) . . . . ? C20 Co1 C16 C15 140.0(11) . . . . ? C13 Co1 C16 C15 -83.7(10) . . . . ? C19 Co1 C16 C15 -178.1(10) . . . . ? C22 Co1 C16 C15 54.9(14) . . . . ? C17 Co1 C16 C15 -119.7(14) . . . . ? C14 Co1 C16 C17 80.4(10) . . . . ? C18 Co1 C16 C17 89(9) . . . . ? C21 Co1 C16 C17 -145.2(10) . . . . ? C15 Co1 C16 C17 119.7(14) . . . . ? C20 Co1 C16 C17 -100.3(11) . . . . ? C13 Co1 C16 C17 36.0(9) . . . . ? C19 Co1 C16 C17 -58.4(14) . . . . ? C22 Co1 C16 C17 174.6(10) . . . . ? C14 C13 C17 C16 1.2(17) . . . . ? P5 C13 C17 C16 176.2(11) . . . . ? Co1 C13 C17 C16 59.8(11) . . . . ? C14 C13 C17 Co1 -58.6(9) . . . . ? P5 C13 C17 Co1 116.4(13) . . . . ? C15 C16 C17 C13 -1.0(19) . . . . ? Co1 C16 C17 C13 -59.1(11) . . . . ? C15 C16 C17 Co1 58.1(11) . . . . ? C14 Co1 C17 C13 39.8(9) . . . . ? C18 Co1 C17 C13 -52.7(13) . . . . ? C21 Co1 C17 C13 -177.0(11) . . . . ? C15 Co1 C17 C13 84.2(10) . . . . ? C20 Co1 C17 C13 -138.4(10) . . . . ? C19 Co1 C17 C13 -93.6(10) . . . . ? C22 Co1 C17 C13 34(12) . . . . ? C16 Co1 C17 C13 120.8(14) . . . . ? C14 Co1 C17 C16 -81.0(10) . . . . ? C18 Co1 C17 C16 -173.4(9) . . . . ? C21 Co1 C17 C16 62.3(15) . . . . ? C15 Co1 C17 C16 -36.6(9) . . . . ? C20 Co1 C17 C16 100.8(11) . . . . ? C13 Co1 C17 C16 -120.8(14) . . . . ? C19 Co1 C17 C16 145.7(10) . . . . ? C22 Co1 C17 C16 -87(11) . . . . ? C23 P7 C18 C22 -1.7(15) . . . . ? C29 P7 C18 C22 100.0(14) . . . . ? Ni1 P7 C18 C22 -127.5(12) . . . . ? C23 P7 C18 C19 171.3(12) . . . . ? C29 P7 C18 C19 -87.0(12) . . . . ? Ni1 P7 C18 C19 45.5(13) . . . . ? C23 P7 C18 Co1 87.1(9) . . . . ? C29 P7 C18 Co1 -171.2(8) . . . . ? Ni1 P7 C18 Co1 -38.7(10) . . . . ? C14 Co1 C18 C22 99.0(9) . . . . ? C21 Co1 C18 C22 -36.8(8) . . . . ? C15 Co1 C18 C22 62.4(12) . . . . ? C20 Co1 C18 C22 -80.3(9) . . . . ? C13 Co1 C18 C22 142.4(9) . . . . ? C19 Co1 C18 C22 -119.2(12) . . . . ? C17 Co1 C18 C22 174.6(10) . . . . ? C16 Co1 C18 C22 90(9) . . . . ? C14 Co1 C18 C19 -141.8(9) . . . . ? C21 Co1 C18 C19 82.4(9) . . . . ? C15 Co1 C18 C19 -178.4(10) . . . . ? C20 Co1 C18 C19 38.9(8) . . . . ? C13 Co1 C18 C19 -98.4(9) . . . . ? C22 Co1 C18 C19 119.2(12) . . . . ? C17 Co1 C18 C19 -66.2(12) . . . . ? C16 Co1 C18 C19 -150(9) . . . . ? C14 Co1 C18 P7 -25.5(11) . . . . ? C21 Co1 C18 P7 -161.3(12) . . . . ? C15 Co1 C18 P7 -62.1(13) . . . . ? C20 Co1 C18 P7 155.2(12) . . . . ? C13 Co1 C18 P7 17.9(10) . . . . ? C19 Co1 C18 P7 116.3(13) . . . . ? C22 Co1 C18 P7 -124.5(13) . . . . ? C17 Co1 C18 P7 50.1(13) . . . . ? C16 Co1 C18 P7 -34(10) . . . . ? C22 C18 C19 C20 0.5(16) . . . . ? P7 C18 C19 C20 -173.7(10) . . . . ? Co1 C18 C19 C20 -60.3(10) . . . . ? C22 C18 C19 Co1 60.9(10) . . . . ? P7 C18 C19 Co1 -113.4(10) . . . . ? C14 Co1 C19 C20 176.4(10) . . . . ? C18 Co1 C19 C20 116.6(13) . . . . ? C21 Co1 C19 C20 38.2(9) . . . . ? C15 Co1 C19 C20 146(16) . . . . ? C13 Co1 C19 C20 -145.6(10) . . . . ? C22 Co1 C19 C20 79.5(10) . . . . ? C17 Co1 C19 C20 -103.4(11) . . . . ? C16 Co1 C19 C20 -66.9(14) . . . . ? C14 Co1 C19 C18 59.8(12) . . . . ? C21 Co1 C19 C18 -78.4(9) . . . . ? C15 Co1 C19 C18 29(16) . . . . ? C20 Co1 C19 C18 -116.6(13) . . . . ? C13 Co1 C19 C18 97.8(9) . . . . ? C22 Co1 C19 C18 -37.1(8) . . . . ? C17 Co1 C19 C18 140.0(9) . . . . ? C16 Co1 C19 C18 176.6(10) . . . . ? C18 C19 C20 C21 -0.8(16) . . . . ? Co1 C19 C20 C21 -60.7(10) . . . . ? C18 C19 C20 Co1 60.0(10) . . . . ? C14 Co1 C20 C21 66(13) . . . . ? C18 Co1 C20 C21 77.9(11) . . . . ? C15 Co1 C20 C21 -60.8(15) . . . . ? C13 Co1 C20 C21 173.2(11) . . . . ? C19 Co1 C20 C21 117.2(14) . . . . ? C22 Co1 C20 C21 34.5(10) . . . . ? C17 Co1 C20 C21 -146.0(10) . . . . ? C16 Co1 C20 C21 -101.3(11) . . . . ? C14 Co1 C20 C19 -51(13) . . . . ? C18 Co1 C20 C19 -39.3(9) . . . . ? C21 Co1 C20 C19 -117.2(14) . . . . ? C15 Co1 C20 C19 -178.0(11) . . . . ? C13 Co1 C20 C19 56.0(14) . . . . ? C22 Co1 C20 C19 -82.7(10) . . . . ? C17 Co1 C20 C19 96.8(10) . . . . ? C16 Co1 C20 C19 141.5(10) . . . . ? C19 C20 C21 C22 0.8(18) . . . . ? Co1 C20 C21 C22 -60.1(11) . . . . ? C19 C20 C21 Co1 60.9(10) . . . . ? C14 Co1 C21 C22 -53.4(15) . . . . ? C18 Co1 C21 C22 38.6(9) . . . . ? C15 Co1 C21 C22 -94.3(12) . . . . ? C20 Co1 C21 C22 122.3(15) . . . . ? C13 Co1 C21 C22 29(9) . . . . ? C19 Co1 C21 C22 83.4(11) . . . . ? C17 Co1 C21 C22 -177.1(11) . . . . ? C16 Co1 C21 C22 -137.6(11) . . . . ? C14 Co1 C21 C20 -175.7(11) . . . . ? C18 Co1 C21 C20 -83.7(10) . . . . ? C15 Co1 C21 C20 143.5(11) . . . . ? C13 Co1 C21 C20 -93(9) . . . . ? C19 Co1 C21 C20 -38.8(9) . . . . ? C22 Co1 C21 C20 -122.3(15) . . . . ? C17 Co1 C21 C20 60.6(16) . . . . ? C16 Co1 C21 C20 100.1(11) . . . . ? C20 C21 C22 C18 -0.5(18) . . . . ? Co1 C21 C22 C18 -59.7(10) . . . . ? C20 C21 C22 Co1 59.2(11) . . . . ? C19 C18 C22 C21 -0.1(17) . . . . ? P7 C18 C22 C21 173.7(11) . . . . ? Co1 C18 C22 C21 60.3(10) . . . . ? C19 C18 C22 Co1 -60.4(10) . . . . ? P7 C18 C22 Co1 113.4(12) . . . . ? C14 Co1 C22 C21 145.7(11) . . . . ? C18 Co1 C22 C21 -117.8(14) . . . . ? C15 Co1 C22 C21 102.3(11) . . . . ? C20 Co1 C22 C21 -36.0(10) . . . . ? C13 Co1 C22 C21 -176.8(10) . . . . ? C19 Co1 C22 C21 -79.9(11) . . . . ? C17 Co1 C22 C21 152(11) . . . . ? C16 Co1 C22 C21 68.7(14) . . . . ? C14 Co1 C22 C18 -96.4(9) . . . . ? C21 Co1 C22 C18 117.8(14) . . . . ? C15 Co1 C22 C18 -139.9(9) . . . . ? C20 Co1 C22 C18 81.8(9) . . . . ? C13 Co1 C22 C18 -59.0(13) . . . . ? C19 Co1 C22 C18 38.0(8) . . . . ? C17 Co1 C22 C18 -91(11) . . . . ? C16 Co1 C22 C18 -173.4(9) . . . . ? C29 P7 C23 C24 -32.8(14) . . . . ? C18 P7 C23 C24 68.6(14) . . . . ? Ni1 P7 C23 C24 -159.4(11) . . . . ? C29 P7 C23 C28 146.4(13) . . . . ? C18 P7 C23 C28 -112.3(13) . . . . ? Ni1 P7 C23 C28 19.8(14) . . . . ? C28 C23 C24 C25 -3(2) . . . . ? P7 C23 C24 C25 176.6(12) . . . . ? C23 C24 C25 C26 1(2) . . . . ? C24 C25 C26 C27 4(3) . . . . ? C25 C26 C27 C28 -6(3) . . . . ? C26 C27 C28 C23 4(3) . . . . ? C24 C23 C28 C27 0(2) . . . . ? P7 C23 C28 C27 -179.1(13) . . . . ? C23 P7 C29 C30 -51.7(14) . . . . ? C18 P7 C29 C30 -153.3(13) . . . . ? Ni1 P7 C29 C30 71.5(14) . . . . ? C23 P7 C29 C34 136.6(13) . . . . ? C18 P7 C29 C34 35.0(14) . . . . ? Ni1 P7 C29 C34 -100.3(13) . . . . ? C34 C29 C30 C31 -3(2) . . . . ? P7 C29 C30 C31 -175.7(12) . . . . ? C29 C30 C31 C32 3(3) . . . . ? C30 C31 C32 C33 -4(3) . . . . ? C31 C32 C33 C34 6(3) . . . . ? C30 C29 C34 C33 5(2) . . . . ? P7 C29 C34 C33 177.3(12) . . . . ? C32 C33 C34 C29 -7(3) . . . . ? C39 Ni1 C35 C36 -69.2(10) . . . . ? C40 Ni1 C35 C36 -101.8(10) . . . . ? P7 Ni1 C35 C36 167.0(8) . . . . ? P5 Ni1 C35 C36 46.0(11) . . . . ? C36 Ni1 C35 C42 123.6(17) . . . . ? C39 Ni1 C35 C42 54.4(13) . . . . ? C40 Ni1 C35 C42 21.8(12) . . . . ? P7 Ni1 C35 C42 -69.4(13) . . . . ? P5 Ni1 C35 C42 169.6(10) . . . . ? C42 C35 C36 C37 0(3) . . . . ? Ni1 C35 C36 C37 104.4(15) . . . . ? C42 C35 C36 Ni1 -104.8(17) . . . . ? C39 Ni1 C36 C35 111.1(11) . . . . ? C40 Ni1 C36 C35 75.1(10) . . . . ? P7 Ni1 C36 C35 -20.9(13) . . . . ? P5 Ni1 C36 C35 -141.9(9) . . . . ? C35 Ni1 C36 C37 -116.6(17) . . . . ? C39 Ni1 C36 C37 -5.6(13) . . . . ? C40 Ni1 C36 C37 -41.6(13) . . . . ? P7 Ni1 C36 C37 -137.6(10) . . . . ? P5 Ni1 C36 C37 101.5(12) . . . . ? C35 C36 C37 C38 -91(2) . . . . ? Ni1 C36 C37 C38 -12(2) . . . . ? C36 C37 C38 C39 30(2) . . . . ? C37 C38 C39 C40 47(2) . . . . ? C37 C38 C39 Ni1 -32.7(17) . . . . ? C35 Ni1 C39 C40 -63.5(11) . . . . ? C36 Ni1 C39 C40 -99.1(11) . . . . ? P7 Ni1 C39 C40 49.9(12) . . . . ? P5 Ni1 C39 C40 170.7(9) . . . . ? C35 Ni1 C39 C38 56.5(13) . . . . ? C36 Ni1 C39 C38 20.9(12) . . . . ? C40 Ni1 C39 C38 120.0(17) . . . . ? P7 Ni1 C39 C38 169.9(9) . . . . ? P5 Ni1 C39 C38 -69.3(12) . . . . ? C38 C39 C40 C41 5(2) . . . . ? Ni1 C39 C40 C41 105.3(14) . . . . ? C38 C39 C40 Ni1 -100.6(13) . . . . ? C35 Ni1 C40 C39 116.0(11) . . . . ? C36 Ni1 C40 C39 78.7(11) . . . . ? P7 Ni1 C40 C39 -138.2(10) . . . . ? P5 Ni1 C40 C39 -14.8(14) . . . . ? C35 Ni1 C40 C41 -5.4(11) . . . . ? C36 Ni1 C40 C41 -42.7(12) . . . . ? C39 Ni1 C40 C41 -121.4(17) . . . . ? P7 Ni1 C40 C41 100.3(11) . . . . ? P5 Ni1 C40 C41 -136.2(9) . . . . ? C39 C40 C41 C42 -94.4(18) . . . . ? Ni1 C40 C41 C42 -11.3(17) . . . . ? C36 C35 C42 C41 50(2) . . . . ? Ni1 C35 C42 C41 -34.1(17) . . . . ? C40 C41 C42 C35 30(2) . . . . ? _diffrn_measured_fraction_theta_max 0.981 _diffrn_reflns_theta_full 23.41 _diffrn_measured_fraction_theta_full 0.981 _refine_diff_density_max 0.484 _refine_diff_density_min -0.522 _refine_diff_density_rms 0.108 # Attachment '- 3.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 780559' #TrackingRef '- 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C40 H46 Co Fe P4' _chemical_formula_weight 765.43 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 '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 Monoclinic _symmetry_space_group_name_H-M Cc loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x, -y, z+1/2' 'x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 13.2681(19) _cell_length_b 15.846(2) _cell_length_c 17.926(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.362(2) _cell_angle_gamma 90.00 _cell_volume 3762.4(10) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4943 _cell_measurement_theta_min 2.00 _cell_measurement_theta_max 27.52 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1596 _exptl_absorpt_coefficient_mu 1.024 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8372 _exptl_absorpt_correction_T_max 0.8870 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10802 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0414 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 27.52 _reflns_number_total 6063 _reflns_number_gt 4943 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. No Obvious Spacegroup Change Needed/Suggested SpaceGroup = Cc ; _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^)+(0.0467P)^2^+14.7289P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.20(4) _refine_ls_number_reflns 6063 _refine_ls_number_parameters 421 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0581 _refine_ls_R_factor_gt 0.0450 _refine_ls_wR_factor_ref 0.1243 _refine_ls_wR_factor_gt 0.1161 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.029 _refine_ls_shift/su_mean 0.006 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 Co1 Co 0.80024(7) 0.29055(9) 0.34302(5) 0.0326(3) Uani 1 1 d . . . Fe2 Fe 0.59496(7) 0.29029(9) 0.39531(5) 0.0297(3) Uani 1 1 d . . . P3 P 0.7101(2) 0.22796(18) 0.25498(16) 0.0290(6) Uani 1 1 d . . . P4 P 0.6853(2) 0.22687(17) 0.48155(15) 0.0270(6) Uani 1 1 d . . . P5 P 0.8145(3) 0.4124(2) 0.2874(2) 0.0450(9) Uani 1 1 d . . . P6 P 0.5810(3) 0.4111(2) 0.4513(2) 0.0484(9) Uani 1 1 d . . . C1 C 0.6949(9) 0.2591(7) 0.1557(6) 0.036(3) Uani 1 1 d . . . C2 C 0.5975(10) 0.2730(8) 0.1217(7) 0.039(3) Uani 1 1 d . . . H2 H 0.5398 0.2685 0.1485 0.047 Uiso 1 1 calc R . . C3 C 0.5917(13) 0.2948(8) 0.0416(8) 0.060(4) Uani 1 1 d . . . H3 H 0.5299 0.3060 0.0163 0.072 Uiso 1 1 calc R . . C4 C 0.6831(14) 0.2983(9) 0.0040(7) 0.067(5) Uani 1 1 d . . . H4 H 0.6811 0.3162 -0.0455 0.081 Uiso 1 1 calc R . . C5 C 0.7705(11) 0.2769(9) 0.0373(8) 0.069(4) Uani 1 1 d . . . H5 H 0.8286 0.2742 0.0107 0.083 Uiso 1 1 calc R . . C6 C 0.7738(10) 0.2577(9) 0.1159(7) 0.058(4) Uani 1 1 d . . . H6 H 0.8357 0.2435 0.1396 0.070 Uiso 1 1 calc R . . C7 C 0.7317(10) 0.1153(8) 0.2389(7) 0.043(3) Uani 1 1 d . . . C8 C 0.8373(10) 0.0932(8) 0.2283(8) 0.042(3) Uani 1 1 d . . . H8 H 0.8876 0.1342 0.2297 0.051 Uiso 1 1 calc R . . C9 C 0.8597(12) 0.0072(10) 0.2159(8) 0.071(5) Uani 1 1 d . . . H9 H 0.9264 -0.0100 0.2132 0.085 Uiso 1 1 calc R . . C10 C 0.7797(14) -0.0536(7) 0.2074(9) 0.070(4) Uani 1 1 d . . . H10 H 0.7916 -0.1100 0.1965 0.084 Uiso 1 1 calc R . . C11 C 0.6963(14) -0.0269(9) 0.2153(10) 0.077(5) Uani 1 1 d . . . H11 H 0.6450 -0.0667 0.2089 0.092 Uiso 1 1 calc R . . C12 C 0.6642(10) 0.0534(9) 0.2324(9) 0.055(3) Uani 1 1 d . . . H12 H 0.5964 0.0639 0.2393 0.066 Uiso 1 1 calc R . . C13 C 0.6579(8) 0.1135(7) 0.4994(6) 0.028(2) Uani 1 1 d . . . C14 C 0.5638(11) 0.0881(9) 0.5067(9) 0.058(4) Uani 1 1 d . . . H14 H 0.5128 0.1274 0.4966 0.069 Uiso 1 1 calc R . . C15 C 0.5358(11) 0.0101(9) 0.5273(9) 0.062(4) Uani 1 1 d . . . H15 H 0.4695 -0.0008 0.5387 0.075 Uiso 1 1 calc R . . C16 C 0.6012(13) -0.0475(9) 0.5309(10) 0.081(5) Uani 1 1 d . . . H16 H 0.5798 -0.1028 0.5376 0.097 Uiso 1 1 calc R . . C17 C 0.7143(13) -0.0313(8) 0.5248(9) 0.070(4) Uani 1 1 d . . . H17 H 0.7631 -0.0733 0.5297 0.084 Uiso 1 1 calc R . . C18 C 0.7367(10) 0.0539(7) 0.5110(8) 0.050(3) Uani 1 1 d . . . H18 H 0.8035 0.0711 0.5096 0.060 Uiso 1 1 calc R . . C19 C 0.7043(8) 0.2574(6) 0.5816(6) 0.034(3) Uani 1 1 d . . . C20 C 0.6159(10) 0.2629(9) 0.6242(7) 0.052(3) Uani 1 1 d . . . H20 H 0.5518 0.2536 0.6019 0.063 Uiso 1 1 calc R . . C21 C 0.6289(15) 0.2821(10) 0.6982(9) 0.087(6) Uani 1 1 d . . . H21 H 0.5727 0.2866 0.7267 0.105 Uiso 1 1 calc R . . C22 C 0.7262(13) 0.2955(9) 0.7326(8) 0.067(5) Uani 1 1 d . . . H22 H 0.7346 0.3057 0.7837 0.080 Uiso 1 1 calc R . . C23 C 0.8045(12) 0.2933(8) 0.6913(8) 0.053(4) Uani 1 1 d . . . H23 H 0.8685 0.3047 0.7129 0.064 Uiso 1 1 calc R . . C24 C 0.7940(10) 0.2755(7) 0.6212(7) 0.041(3) Uani 1 1 d . . . H24 H 0.8522 0.2749 0.5948 0.049 Uiso 1 1 calc R . . C25 C 0.5870(7) 0.2351(6) 0.2885(6) 0.031(2) Uani 1 1 d . . . C26 C 0.5417(10) 0.1801(8) 0.3427(6) 0.045(3) Uani 1 1 d . . . H26 H 0.5642 0.1228 0.3556 0.053 Uiso 1 1 d R . . C27 C 0.4631(9) 0.2207(7) 0.3719(7) 0.051(3) Uani 1 1 d . . . H27 H 0.4187 0.1978 0.4087 0.061 Uiso 1 1 d R . . C28 C 0.4568(8) 0.3029(8) 0.3399(8) 0.054(4) Uani 1 1 d . . . H28 H 0.4066 0.3454 0.3519 0.065 Uiso 1 1 d R . . C29 C 0.5300(9) 0.3148(7) 0.2895(5) 0.038(3) Uani 1 1 d . . . H29 H 0.5399 0.3650 0.2588 0.045 Uiso 1 1 d R . . C30 C 0.8522(7) 0.1802(5) 0.3966(6) 0.026(2) Uani 1 1 d . . . H30 H 0.8291 0.1227 0.3850 0.031 Uiso 1 1 d R . . C31 C 0.9375(7) 0.2232(7) 0.3650(6) 0.042(3) Uani 1 1 d . . . H31 H 0.9801 0.1999 0.3272 0.050 Uiso 1 1 d R . . C32 C 0.9469(8) 0.3022(8) 0.3966(5) 0.038(3) Uani 1 1 d . . . H32 H 0.9977 0.3448 0.3860 0.046 Uiso 1 1 d R . . C33 C 0.8684(8) 0.3106(6) 0.4478(7) 0.037(3) Uani 1 1 d . . . H33 H 0.8577 0.3601 0.4791 0.045 Uiso 1 1 d R . . C34 C 0.8132(7) 0.2343(6) 0.4498(6) 0.029(2) Uani 1 1 d . . . C35 C 0.8538(12) 0.5013(9) 0.3477(9) 0.075(4) Uani 1 1 d . . . H35A H 0.8627 0.5506 0.3175 0.112 Uiso 1 1 calc R . . H35B H 0.9164 0.4878 0.3746 0.112 Uiso 1 1 calc R . . H35C H 0.8030 0.5122 0.3824 0.112 Uiso 1 1 calc R . . C36 C 0.9159(12) 0.4257(9) 0.2332(8) 0.069(3) Uani 1 1 d . . . H36A H 0.9145 0.3832 0.1951 0.103 Uiso 1 1 calc R . . H36B H 0.9773 0.4210 0.2639 0.103 Uiso 1 1 calc R . . H36C H 0.9124 0.4805 0.2103 0.103 Uiso 1 1 calc R . . C37 C 0.7235(12) 0.4586(8) 0.2251(8) 0.066(4) Uani 1 1 d . . . H37A H 0.7520 0.5072 0.2022 0.099 Uiso 1 1 calc R . . H37B H 0.6662 0.4754 0.2518 0.099 Uiso 1 1 calc R . . H37C H 0.7026 0.4184 0.1872 0.099 Uiso 1 1 calc R . . C38 C 0.6831(12) 0.4621(6) 0.5129(7) 0.062(4) Uani 1 1 d . . . H38A H 0.7465 0.4574 0.4900 0.093 Uiso 1 1 calc R . . H38B H 0.6878 0.4344 0.5606 0.093 Uiso 1 1 calc R . . H38C H 0.6673 0.5206 0.5197 0.093 Uiso 1 1 calc R . . C39 C 0.5528(13) 0.5045(8) 0.3910(8) 0.080(5) Uani 1 1 d . . . H39A H 0.5251 0.5487 0.4202 0.119 Uiso 1 1 calc R . . H39B H 0.5049 0.4891 0.3511 0.119 Uiso 1 1 calc R . . H39C H 0.6139 0.5240 0.3705 0.119 Uiso 1 1 calc R . . C40 C 0.4717(12) 0.4083(9) 0.5202(9) 0.073(4) Uani 1 1 d . . . H40A H 0.4578 0.4646 0.5365 0.109 Uiso 1 1 calc R . . H40B H 0.4916 0.3740 0.5627 0.109 Uiso 1 1 calc R . . H40C H 0.4121 0.3849 0.4951 0.109 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Co1 0.0355(8) 0.0307(7) 0.0312(8) 0.0059(6) -0.0018(6) -0.0025(6) Fe2 0.0257(7) 0.0320(8) 0.0304(8) -0.0030(6) -0.0061(6) 0.0063(6) P3 0.0311(14) 0.0282(13) 0.0275(15) 0.0007(11) 0.0000(12) -0.0012(12) P4 0.0301(14) 0.0265(13) 0.0243(14) -0.0014(10) 0.0003(11) 0.0012(11) P5 0.054(2) 0.0371(17) 0.0424(19) 0.0150(14) -0.0117(16) -0.0209(15) P6 0.061(2) 0.0371(18) 0.046(2) -0.0089(14) -0.0100(17) 0.0159(16) C1 0.043(6) 0.041(6) 0.023(5) -0.006(4) -0.016(4) 0.003(5) C2 0.044(6) 0.053(6) 0.019(4) 0.000(4) -0.012(4) -0.013(5) C3 0.088(10) 0.048(7) 0.043(7) 0.024(5) -0.012(7) -0.024(6) C4 0.117(12) 0.065(8) 0.025(6) 0.003(5) 0.032(7) -0.004(7) C5 0.065(8) 0.090(9) 0.053(9) 0.032(7) 0.017(6) -0.029(7) C6 0.059(7) 0.068(8) 0.044(7) 0.007(6) -0.021(6) -0.007(6) C7 0.050(6) 0.040(6) 0.038(7) -0.001(5) -0.006(5) 0.011(5) C8 0.040(6) 0.043(6) 0.045(7) -0.009(5) 0.006(5) 0.016(5) C9 0.091(10) 0.073(9) 0.045(7) -0.015(6) -0.035(7) 0.046(8) C10 0.111(11) 0.023(5) 0.074(9) 0.002(5) -0.007(8) -0.005(6) C11 0.085(9) 0.051(8) 0.092(11) -0.005(7) -0.014(8) -0.012(7) C12 0.048(7) 0.060(8) 0.057(8) -0.009(6) 0.010(6) 0.004(6) C13 0.037(5) 0.026(5) 0.021(5) 0.001(4) 0.004(4) 0.002(4) C14 0.052(7) 0.061(8) 0.059(9) 0.008(6) -0.007(6) -0.002(6) C15 0.060(8) 0.053(7) 0.075(9) 0.018(6) 0.009(6) -0.015(6) C16 0.103(11) 0.060(8) 0.080(11) 0.027(7) 0.006(8) -0.048(8) C17 0.083(8) 0.037(6) 0.095(10) 0.034(6) 0.038(7) 0.022(5) C18 0.066(8) 0.027(5) 0.058(7) 0.020(5) 0.020(6) 0.019(5) C19 0.047(6) 0.023(5) 0.034(5) -0.004(4) 0.024(5) 0.012(4) C20 0.052(6) 0.064(7) 0.046(6) -0.013(5) 0.039(5) 0.002(5) C21 0.116(14) 0.103(11) 0.047(9) -0.002(7) 0.039(9) -0.030(9) C22 0.097(10) 0.061(8) 0.039(7) -0.020(5) -0.030(7) 0.023(7) C23 0.068(8) 0.055(7) 0.033(6) 0.009(5) -0.018(6) -0.018(6) C24 0.054(7) 0.028(5) 0.043(7) 0.001(4) 0.006(5) 0.009(4) C25 0.026(4) 0.041(5) 0.024(5) -0.001(4) -0.011(4) -0.020(4) C26 0.057(7) 0.054(7) 0.021(5) 0.004(5) -0.008(5) -0.018(6) C27 0.055(7) 0.063(7) 0.035(6) 0.001(5) -0.004(5) -0.040(5) C28 0.021(5) 0.057(7) 0.082(9) -0.027(6) -0.023(5) 0.022(4) C29 0.040(6) 0.057(6) 0.015(4) 0.006(4) -0.010(4) -0.007(5) C30 0.018(4) 0.020(4) 0.040(5) 0.014(4) 0.015(4) 0.001(3) C31 0.017(4) 0.071(7) 0.038(6) 0.023(5) 0.001(4) -0.017(4) C32 0.036(5) 0.063(7) 0.016(4) 0.007(4) 0.000(3) 0.000(4) C33 0.033(5) 0.025(4) 0.053(7) 0.010(4) -0.009(5) -0.018(4) C34 0.030(4) 0.024(4) 0.035(6) 0.003(4) 0.008(4) -0.016(3) C35 0.086(9) 0.051(8) 0.087(11) 0.019(7) 0.000(7) -0.027(7) C36 0.074(7) 0.070(7) 0.063(7) 0.010(6) 0.021(6) -0.010(5) C37 0.078(8) 0.056(7) 0.063(8) -0.005(6) -0.001(7) -0.020(6) C38 0.093(9) 0.024(5) 0.062(8) -0.025(5) -0.051(7) 0.008(5) C39 0.126(12) 0.034(6) 0.070(9) -0.005(5) -0.067(8) 0.031(6) C40 0.079(8) 0.071(7) 0.072(8) -0.001(5) 0.035(6) 0.033(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C33 2.061(11) . ? Co1 C30 2.092(9) . ? Co1 C34 2.109(10) . ? Co1 C31 2.128(10) . ? Co1 C32 2.127(11) . ? Co1 P3 2.164(3) . ? Co1 P5 2.186(3) . ? Co1 Fe2 2.9319(9) . ? Fe2 C28 2.043(10) . ? Fe2 C29 2.073(10) . ? Fe2 C26 2.087(12) . ? Fe2 C27 2.090(10) . ? Fe2 C25 2.102(10) . ? Fe2 P4 2.149(3) . ? Fe2 P6 2.175(4) . ? P3 C25 1.776(11) . ? P3 C7 1.834(13) . ? P3 C1 1.846(11) . ? P4 C34 1.825(10) . ? P4 C19 1.861(11) . ? P4 C13 1.864(11) . ? P5 C36 1.717(14) . ? P5 C37 1.756(14) . ? P5 C35 1.833(15) . ? P6 C39 1.858(12) . ? P6 C38 1.879(11) . ? P6 C40 1.960(14) . ? C1 C6 1.301(16) . ? C1 C2 1.414(15) . ? C2 C3 1.475(18) . ? C2 H2 0.9300 . ? C3 C4 1.42(2) . ? C3 H3 0.9300 . ? C4 C5 1.32(2) . ? C4 H4 0.9300 . ? C5 C6 1.440(19) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.328(18) . ? C7 C8 1.467(18) . ? C8 C9 1.416(18) . ? C8 H8 0.9300 . ? C9 C10 1.43(2) . ? C9 H9 0.9300 . ? C10 C11 1.20(2) . ? C10 H10 0.9300 . ? C11 C12 1.382(19) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.325(18) . ? C13 C18 1.415(15) . ? C14 C15 1.348(19) . ? C14 H14 0.9300 . ? C15 C16 1.26(2) . ? C15 H15 0.9300 . ? C16 C17 1.53(2) . ? C16 H16 0.9300 . ? C17 C18 1.407(15) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 C24 1.378(16) . ? C19 C20 1.440(13) . ? C20 C21 1.36(2) . ? C20 H20 0.9300 . ? C21 C22 1.41(2) . ? C21 H21 0.9300 . ? C22 C23 1.31(2) . ? C22 H22 0.9300 . ? C23 C24 1.287(18) . ? C23 H23 0.9300 . ? C24 H24 0.9300 . ? C25 C29 1.472(14) . ? C25 C26 1.461(15) . ? C26 C27 1.356(17) . ? C26 H26 0.9800 . ? C27 C28 1.424(17) . ? C27 H27 0.9800 . ? C28 C29 1.377(18) . ? C28 H28 0.9799 . ? C29 H29 0.9800 . ? C30 C34 1.403(14) . ? C30 C31 1.463(11) . ? C30 H30 0.9800 . ? C31 C32 1.377(16) . ? C31 H31 0.9799 . ? C32 C33 1.434(16) . ? C32 H32 0.9800 . ? C33 C34 1.416(11) . ? C33 H33 0.9800 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? 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 C33 Co1 C30 66.2(4) . . ? C33 Co1 C34 39.7(3) . . ? C30 Co1 C34 39.0(4) . . ? C33 Co1 C31 65.4(5) . . ? C30 Co1 C31 40.6(3) . . ? C34 Co1 C31 66.2(4) . . ? C33 Co1 C32 40.0(4) . . ? C30 Co1 C32 66.3(4) . . ? C34 Co1 C32 66.6(4) . . ? C31 Co1 C32 37.8(4) . . ? C33 Co1 P3 158.4(3) . . ? C30 Co1 P3 96.0(3) . . ? C34 Co1 P3 118.7(3) . . ? C31 Co1 P3 109.6(4) . . ? C32 Co1 P3 145.2(3) . . ? C33 Co1 P5 103.5(3) . . ? C30 Co1 P5 155.9(3) . . ? C34 Co1 P5 141.5(3) . . ? C31 Co1 P5 115.6(3) . . ? C32 Co1 P5 91.6(3) . . ? P3 Co1 P5 97.52(13) . . ? C33 Co1 Fe2 94.3(3) . . ? C30 Co1 Fe2 98.0(2) . . ? C34 Co1 Fe2 74.8(3) . . ? C31 Co1 Fe2 137.8(3) . . ? C32 Co1 Fe2 134.3(3) . . ? P3 Co1 Fe2 75.42(9) . . ? P5 Co1 Fe2 104.71(12) . . ? C28 Fe2 C29 39.1(5) . . ? C28 Fe2 C26 65.9(5) . . ? C29 Fe2 C26 68.4(4) . . ? C28 Fe2 C27 40.3(5) . . ? C29 Fe2 C27 67.5(5) . . ? C26 Fe2 C27 37.9(5) . . ? C28 Fe2 C25 66.5(4) . . ? C29 Fe2 C25 41.3(4) . . ? C26 Fe2 C25 40.8(4) . . ? C27 Fe2 C25 66.5(4) . . ? C28 Fe2 P4 147.4(4) . . ? C29 Fe2 P4 158.4(3) . . ? C26 Fe2 P4 95.4(3) . . ? C27 Fe2 P4 108.8(4) . . ? C25 Fe2 P4 117.2(3) . . ? C28 Fe2 P6 92.3(4) . . ? C29 Fe2 P6 102.4(4) . . ? C26 Fe2 P6 155.4(4) . . ? C27 Fe2 P6 117.7(4) . . ? C25 Fe2 P6 141.8(3) . . ? P4 Fe2 P6 97.97(13) . . ? C28 Fe2 Co1 131.9(4) . . ? C29 Fe2 Co1 92.9(3) . . ? C26 Fe2 Co1 98.8(4) . . ? C27 Fe2 Co1 136.0(4) . . ? C25 Fe2 Co1 73.0(3) . . ? P4 Fe2 Co1 75.00(9) . . ? P6 Fe2 Co1 104.59(13) . . ? C25 P3 C7 105.7(6) . . ? C25 P3 C1 105.0(5) . . ? C7 P3 C1 96.8(6) . . ? C25 P3 Co1 101.8(3) . . ? C7 P3 Co1 118.4(4) . . ? C1 P3 Co1 127.2(4) . . ? C34 P4 C19 102.0(5) . . ? C34 P4 C13 108.1(5) . . ? C19 P4 C13 95.8(5) . . ? C34 P4 Fe2 103.6(3) . . ? C19 P4 Fe2 127.6(3) . . ? C13 P4 Fe2 117.9(4) . . ? C36 P5 C37 96.9(8) . . ? C36 P5 C35 91.9(7) . . ? C37 P5 C35 102.5(7) . . ? C36 P5 Co1 117.3(5) . . ? C37 P5 Co1 125.7(5) . . ? C35 P5 Co1 116.1(5) . . ? C39 P6 C38 96.5(6) . . ? C39 P6 C40 104.7(7) . . ? C38 P6 C40 100.0(8) . . ? C39 P6 Fe2 116.9(5) . . ? C38 P6 Fe2 124.9(4) . . ? C40 P6 Fe2 110.9(5) . . ? C6 C1 C2 120.7(11) . . ? C6 C1 P3 118.6(8) . . ? C2 C1 P3 120.2(9) . . ? C1 C2 C3 116.8(13) . . ? C1 C2 H2 121.6 . . ? C3 C2 H2 121.6 . . ? C4 C3 C2 118.2(14) . . ? C4 C3 H3 120.9 . . ? C2 C3 H3 120.9 . . ? C5 C4 C3 121.9(12) . . ? C5 C4 H4 119.0 . . ? C3 C4 H4 119.1 . . ? C4 C5 C6 118.2(12) . . ? C4 C5 H5 120.9 . . ? C6 C5 H5 120.9 . . ? C1 C6 C5 123.7(12) . . ? C1 C6 H6 118.2 . . ? C5 C6 H6 118.2 . . ? C12 C7 C8 117.2(12) . . ? C12 C7 P3 128.4(11) . . ? C8 C7 P3 114.3(10) . . ? C9 C8 C7 117.4(13) . . ? C9 C8 H8 121.3 . . ? C7 C8 H8 121.3 . . ? C10 C9 C8 120.1(14) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C11 C10 C9 115.6(13) . . ? C11 C10 H10 122.2 . . ? C9 C10 H10 122.2 . . ? C10 C11 C12 130.5(16) . . ? C10 C11 H11 114.8 . . ? C12 C11 H11 114.7 . . ? C7 C12 C11 118.9(14) . . ? C7 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C14 C13 C18 118.3(12) . . ? C14 C13 P4 120.3(10) . . ? C18 C13 P4 121.2(9) . . ? C13 C14 C15 125.6(14) . . ? C13 C14 H14 117.2 . . ? C15 C14 H14 117.2 . . ? C16 C15 C14 118.6(14) . . ? C16 C15 H15 120.7 . . ? C14 C15 H15 120.7 . . ? C15 C16 C17 123.3(12) . . ? C15 C16 H16 118.3 . . ? C17 C16 H16 118.4 . . ? C18 C17 C16 113.0(12) . . ? C18 C17 H17 123.5 . . ? C16 C17 H17 123.5 . . ? C17 C18 C13 120.3(13) . . ? C17 C18 H18 119.8 . . ? C13 C18 H18 119.9 . . ? C24 C19 C20 114.8(11) . . ? C24 C19 P4 127.9(8) . . ? C20 C19 P4 117.3(9) . . ? C21 C20 C19 118.0(14) . . ? C21 C20 H20 121.0 . . ? C19 C20 H20 121.0 . . ? C20 C21 C22 121.2(14) . . ? C20 C21 H21 119.4 . . ? C22 C21 H21 119.4 . . ? C23 C22 C21 118.9(13) . . ? C23 C22 H22 120.5 . . ? C21 C22 H22 120.5 . . ? C24 C23 C22 120.9(14) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C19 126.0(14) . . ? C23 C24 H24 117.0 . . ? C19 C24 H24 117.0 . . ? C29 C25 C26 105.8(10) . . ? C29 C25 P3 122.8(8) . . ? C26 C25 P3 127.5(9) . . ? C29 C25 Fe2 68.3(5) . . ? C26 C25 Fe2 69.0(6) . . ? P3 C25 Fe2 109.7(4) . . ? C27 C26 C25 109.2(11) . . ? C27 C26 Fe2 71.2(7) . . ? C25 C26 Fe2 70.1(6) . . ? C27 C26 H26 125.4 . . ? C25 C26 H26 125.4 . . ? Fe2 C26 H26 125.4 . . ? C26 C27 C28 107.8(11) . . ? C26 C27 Fe2 70.9(7) . . ? C28 C27 Fe2 68.1(6) . . ? C26 C27 H27 126.2 . . ? C28 C27 H27 126.0 . . ? Fe2 C27 H27 126.1 . . ? C29 C28 C27 111.3(11) . . ? C29 C28 Fe2 71.6(6) . . ? C27 C28 Fe2 71.7(7) . . ? C29 C28 H28 124.4 . . ? C27 C28 H28 124.4 . . ? Fe2 C28 H28 124.3 . . ? C28 C29 C25 105.9(10) . . ? C28 C29 Fe2 69.3(6) . . ? C25 C29 Fe2 70.4(5) . . ? C28 C29 H29 127.0 . . ? C25 C29 H29 127.1 . . ? Fe2 C29 H29 127.1 . . ? C34 C30 C31 107.6(8) . . ? C34 C30 Co1 71.1(5) . . ? C31 C30 Co1 71.0(5) . . ? C34 C30 H30 126.2 . . ? C31 C30 H30 126.1 . . ? Co1 C30 H30 126.2 . . ? C32 C31 C30 108.5(10) . . ? C32 C31 Co1 71.1(7) . . ? C30 C31 Co1 68.4(5) . . ? C32 C31 H31 125.7 . . ? C30 C31 H31 125.7 . . ? Co1 C31 H31 125.7 . . ? C31 C32 C33 107.2(10) . . ? C31 C32 Co1 71.1(6) . . ? C33 C32 Co1 67.5(6) . . ? C31 C32 H32 126.4 . . ? C33 C32 H32 126.4 . . ? Co1 C32 H32 126.4 . . ? C34 C33 C32 109.5(10) . . ? C34 C33 Co1 72.0(6) . . ? C32 C33 Co1 72.5(7) . . ? C34 C33 H33 125.2 . . ? C32 C33 H33 125.3 . . ? Co1 C33 H33 125.1 . . ? C30 C34 C33 107.0(9) . . ? C30 C34 P4 124.0(7) . . ? C33 C34 P4 123.7(8) . . ? C30 C34 Co1 69.9(6) . . ? C33 C34 Co1 68.3(6) . . ? P4 C34 Co1 106.4(5) . . ? P5 C35 H35A 109.5 . . ? P5 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? P5 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? P5 C36 H36A 109.5 . . ? P5 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? P5 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? P5 C37 H37A 109.5 . . ? P5 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? P5 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? P6 C38 H38A 109.5 . . ? P6 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? P6 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? P6 C39 H39A 109.5 . . ? P6 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? P6 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? P6 C40 H40A 109.5 . . ? P6 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? P6 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 27.52 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.726 _refine_diff_density_min -0.362 _refine_diff_density_rms 0.082 # Attachment '- 7.cif' data_7 _database_code_depnum_ccdc_archive 'CCDC 780560' #TrackingRef '- 7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H46 Fe Ni P4' _chemical_formula_sum 'C40 H46 Fe Ni P4' _chemical_formula_weight 765.21 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.468(8) _cell_length_b 18.923(13) _cell_length_c 20.003(14) _cell_angle_alpha 69.728(14) _cell_angle_beta 87.192(14) _cell_angle_gamma 86.672(14) _cell_volume 3709(5) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 1521 _cell_measurement_theta_min 1.09 _cell_measurement_theta_max 23.34 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1600 _exptl_absorpt_coefficient_mu 1.099 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8102 _exptl_absorpt_correction_T_max 0.8438 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15871 _diffrn_reflns_av_R_equivalents 0.0779 _diffrn_reflns_av_sigmaI/netI 0.1632 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.09 _diffrn_reflns_theta_max 23.34 _reflns_number_total 10631 _reflns_number_gt 5409 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1007P)^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 10631 _refine_ls_number_parameters 841 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1480 _refine_ls_R_factor_gt 0.0697 _refine_ls_wR_factor_ref 0.2160 _refine_ls_wR_factor_gt 0.1660 _refine_ls_goodness_of_fit_ref 0.943 _refine_ls_restrained_S_all 0.943 _refine_ls_shift/su_max 0.002 _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 Fe1 Fe -0.11545(14) 0.51013(7) 0.20534(8) 0.0388(4) Uani 1 1 d . . . Fe2 Fe 0.16167(14) 0.88633(8) 0.13977(7) 0.0368(4) Uani 1 1 d . . . Ni1 Ni 0.17927(11) 0.34624(6) 0.23708(6) 0.0314(3) Uani 1 1 d . . . Ni2 Ni 0.41952(12) 0.85254(6) 0.30260(6) 0.0328(3) Uani 1 1 d . . . P1 P 0.1975(2) 0.45861(14) 0.23753(13) 0.0338(6) Uani 1 1 d . . . P2 P -0.0095(2) 0.33677(14) 0.20373(13) 0.0317(6) Uani 1 1 d . . . P3 P 0.2189(3) 0.26682(15) 0.34359(14) 0.0416(7) Uani 1 1 d . . . P4 P 0.3251(3) 0.31540(15) 0.16843(14) 0.0402(7) Uani 1 1 d . . . P5 P 0.4615(2) 0.90415(14) 0.18933(13) 0.0326(6) Uani 1 1 d . . . P6 P 0.2209(3) 0.82330(14) 0.31957(13) 0.0360(7) Uani 1 1 d . . . P7 P 0.4562(3) 0.93280(16) 0.35535(15) 0.0485(8) Uani 1 1 d . . . P8 P 0.5500(3) 0.75606(16) 0.35318(15) 0.0483(8) Uani 1 1 d . . . C1 C 0.2645(9) 0.5320(5) 0.1576(5) 0.041(3) Uani 1 1 d . . . C2 C 0.3072(10) 0.6012(6) 0.1585(6) 0.049(3) Uani 1 1 d . . . H2 H 0.3063 0.6110 0.2010 0.059 Uiso 1 1 calc R . . C3 C 0.3503(11) 0.6542(6) 0.0956(7) 0.065(4) Uani 1 1 d . . . H3 H 0.3732 0.7007 0.0963 0.078 Uiso 1 1 calc R . . C4 C 0.3604(12) 0.6413(7) 0.0333(8) 0.074(4) Uani 1 1 d . . . H4 H 0.3929 0.6771 -0.0079 0.089 Uiso 1 1 calc R . . C5 C 0.3201(11) 0.5718(7) 0.0325(6) 0.066(4) Uani 1 1 d . . . H5 H 0.3261 0.5613 -0.0097 0.079 Uiso 1 1 calc R . . C6 C 0.2720(10) 0.5194(6) 0.0939(6) 0.050(3) Uani 1 1 d . . . H6 H 0.2438 0.4744 0.0922 0.059 Uiso 1 1 calc R . . C7 C 0.3027(11) 0.4677(5) 0.3045(5) 0.041(3) Uani 1 1 d . . . C8 C 0.4308(11) 0.4483(7) 0.3024(6) 0.065(4) Uani 1 1 d . . . H8 H 0.4644 0.4368 0.2633 0.078 Uiso 1 1 calc R . . C9 C 0.5104(13) 0.4451(7) 0.3549(7) 0.076(4) Uani 1 1 d . . . H9 H 0.5961 0.4303 0.3516 0.091 Uiso 1 1 calc R . . C10 C 0.4672(14) 0.4631(6) 0.4121(7) 0.064(4) Uani 1 1 d . . . H10 H 0.5219 0.4606 0.4482 0.077 Uiso 1 1 calc R . . C11 C 0.3434(14) 0.4848(7) 0.4153(6) 0.070(4) Uani 1 1 d . . . H11 H 0.3126 0.4984 0.4538 0.084 Uiso 1 1 calc R . . C12 C 0.2598(11) 0.4873(6) 0.3621(6) 0.050(3) Uani 1 1 d . . . H12 H 0.1743 0.5023 0.3657 0.060 Uiso 1 1 calc R . . C13 C -0.0100(8) 0.2962(5) 0.1326(5) 0.030(2) Uani 1 1 d . . . C14 C -0.0514(10) 0.3338(6) 0.0653(5) 0.041(3) Uani 1 1 d . . . H14 H -0.0864 0.3827 0.0541 0.050 Uiso 1 1 calc R . . C15 C -0.0420(11) 0.3001(7) 0.0130(6) 0.056(3) Uani 1 1 d . . . H15 H -0.0708 0.3259 -0.0327 0.068 Uiso 1 1 calc R . . C16 C 0.0101(11) 0.2288(7) 0.0303(6) 0.057(3) Uani 1 1 d . . . H16 H 0.0175 0.2062 -0.0043 0.069 Uiso 1 1 calc R . . C17 C 0.0523(10) 0.1889(6) 0.0980(6) 0.052(3) Uani 1 1 d . . . H17 H 0.0877 0.1402 0.1088 0.062 Uiso 1 1 calc R . . C18 C 0.0412(10) 0.2222(6) 0.1485(5) 0.049(3) Uani 1 1 d . . . H18 H 0.0680 0.1954 0.1943 0.059 Uiso 1 1 calc R . . C19 C -0.1286(9) 0.2743(5) 0.2644(5) 0.034(2) Uani 1 1 d . . . C20 C -0.1371(11) 0.2714(6) 0.3348(5) 0.052(3) Uani 1 1 d . . . H20 H -0.0887 0.3027 0.3496 0.063 Uiso 1 1 calc R . . C21 C -0.2191(11) 0.2210(7) 0.3835(6) 0.067(4) Uani 1 1 d . . . H21 H -0.2237 0.2192 0.4306 0.081 Uiso 1 1 calc R . . C22 C -0.2920(11) 0.1746(6) 0.3641(6) 0.060(3) Uani 1 1 d . . . H22 H -0.3455 0.1412 0.3971 0.072 Uiso 1 1 calc R . . C23 C -0.2842(11) 0.1787(6) 0.2945(6) 0.059(3) Uani 1 1 d . . . H23 H -0.3321 0.1470 0.2801 0.071 Uiso 1 1 calc R . . C24 C -0.2060(9) 0.2292(6) 0.2451(5) 0.044(3) Uani 1 1 d . . . H24 H -0.2061 0.2325 0.1976 0.053 Uiso 1 1 calc R . . C25 C 0.1554(11) 0.2848(6) 0.4231(5) 0.057(3) Uani 1 1 d . . . H25A H 0.1781 0.2427 0.4648 0.086 Uiso 1 1 calc R . . H25B H 0.0639 0.2914 0.4211 0.086 Uiso 1 1 calc R . . H25C H 0.1908 0.3296 0.4252 0.086 Uiso 1 1 calc R . . C26 C 0.1672(12) 0.1709(5) 0.3655(6) 0.063(3) Uani 1 1 d . . . H26A H 0.1979 0.1514 0.3290 0.095 Uiso 1 1 calc R . . H26B H 0.0753 0.1710 0.3685 0.095 Uiso 1 1 calc R . . H26C H 0.2010 0.1397 0.4104 0.095 Uiso 1 1 calc R . . C27 C 0.3852(10) 0.2461(6) 0.3678(6) 0.063(3) Uani 1 1 d . . . H27A H 0.3905 0.2057 0.4128 0.095 Uiso 1 1 calc R . . H27B H 0.4210 0.2901 0.3714 0.095 Uiso 1 1 calc R . . H27C H 0.4322 0.2314 0.3319 0.095 Uiso 1 1 calc R . . C28 C 0.3052(11) 0.3371(7) 0.0720(5) 0.060(3) Uani 1 1 d . . . H28A H 0.3174 0.3897 0.0470 0.090 Uiso 1 1 calc R . . H28B H 0.2206 0.3252 0.0641 0.090 Uiso 1 1 calc R . . H28C H 0.3672 0.3077 0.0547 0.090 Uiso 1 1 calc R . . C29 C 0.3712(11) 0.2141(6) 0.1920(6) 0.060(3) Uani 1 1 d . . . H29A H 0.4404 0.2079 0.1609 0.091 Uiso 1 1 calc R . . H29B H 0.2992 0.1874 0.1869 0.091 Uiso 1 1 calc R . . H29C H 0.3980 0.1943 0.2405 0.091 Uiso 1 1 calc R . . C30 C 0.4868(10) 0.3508(7) 0.1642(6) 0.061(3) Uani 1 1 d . . . H30A H 0.5416 0.3323 0.1334 0.092 Uiso 1 1 calc R . . H30B H 0.5208 0.3336 0.2111 0.092 Uiso 1 1 calc R . . H30C H 0.4823 0.4049 0.1458 0.092 Uiso 1 1 calc R . . C31 C 0.0535(9) 0.5093(5) 0.2528(5) 0.038(3) Uani 1 1 d . . . C32 C 0.0051(11) 0.5858(5) 0.2169(6) 0.049(3) Uani 1 1 d . . . H32 H 0.0481 0.6223 0.1805 0.058 Uiso 1 1 calc R . . C33 C -0.1173(12) 0.5966(6) 0.2456(6) 0.054(3) Uani 1 1 d . . . H33 H -0.1686 0.6407 0.2312 0.065 Uiso 1 1 calc R . . C34 C -0.1481(10) 0.5287(7) 0.2999(6) 0.053(3) Uani 1 1 d . . . H34 H -0.2234 0.5204 0.3276 0.064 Uiso 1 1 calc R . . C35 C -0.0442(9) 0.4746(6) 0.3054(5) 0.039(3) Uani 1 1 d . . . H35 H -0.0405 0.4254 0.3374 0.046 Uiso 1 1 calc R . . C36 C -0.1110(9) 0.4205(5) 0.1684(5) 0.035(2) Uani 1 1 d . . . C37 C -0.0740(10) 0.4879(6) 0.1136(5) 0.046(3) Uani 1 1 d . . . H37 H 0.0040 0.4952 0.0884 0.055 Uiso 1 1 calc R . . C38 C -0.1796(12) 0.5430(6) 0.1043(6) 0.053(3) Uani 1 1 d . . . H38 H -0.1805 0.5919 0.0716 0.064 Uiso 1 1 calc R . . C39 C -0.2789(11) 0.5116(6) 0.1514(6) 0.054(3) Uani 1 1 d . . . H39 H -0.3577 0.5351 0.1561 0.065 Uiso 1 1 calc R . . C40 C -0.2374(10) 0.4356(6) 0.1919(6) 0.048(3) Uani 1 1 d . . . H40 H -0.2854 0.4016 0.2278 0.057 Uiso 1 1 calc R . . C41 C 0.5598(9) 0.9879(5) 0.1614(5) 0.036(2) Uani 1 1 d . . . C42 C 0.6792(10) 0.9823(6) 0.1883(6) 0.054(3) Uani 1 1 d . . . H42 H 0.7071 0.9360 0.2204 0.064 Uiso 1 1 calc R . . C43 C 0.7613(12) 1.0415(8) 0.1708(7) 0.071(4) Uani 1 1 d . . . H43 H 0.8425 1.0345 0.1896 0.085 Uiso 1 1 calc R . . C44 C 0.7192(13) 1.1107(8) 0.1249(7) 0.074(4) Uani 1 1 d . . . H44 H 0.7713 1.1517 0.1136 0.088 Uiso 1 1 calc R . . C45 C 0.6017(13) 1.1198(6) 0.0959(6) 0.058(3) Uani 1 1 d . . . H45 H 0.5738 1.1667 0.0648 0.069 Uiso 1 1 calc R . . C46 C 0.5208(10) 1.0564(5) 0.1136(5) 0.046(3) Uani 1 1 d . . . H46 H 0.4418 1.0620 0.0926 0.055 Uiso 1 1 calc R . . C47 C 0.5536(9) 0.8494(5) 0.1428(5) 0.035(2) Uani 1 1 d . . . C48 C 0.6264(11) 0.8817(6) 0.0793(5) 0.050(3) Uani 1 1 d . . . H48 H 0.6300 0.9339 0.0596 0.060 Uiso 1 1 calc R . . C49 C 0.6928(12) 0.8370(7) 0.0459(6) 0.063(3) Uani 1 1 d . . . H49 H 0.7402 0.8594 0.0040 0.076 Uiso 1 1 calc R . . C50 C 0.6888(11) 0.7608(7) 0.0741(7) 0.059(3) Uani 1 1 d . . . H50 H 0.7339 0.7313 0.0514 0.071 Uiso 1 1 calc R . . C51 C 0.6202(12) 0.7271(6) 0.1348(7) 0.061(3) Uani 1 1 d . . . H51 H 0.6175 0.6749 0.1537 0.073 Uiso 1 1 calc R . . C52 C 0.5545(10) 0.7710(6) 0.1682(5) 0.043(3) Uani 1 1 d . . . H52 H 0.5080 0.7470 0.2100 0.052 Uiso 1 1 calc R . . C53 C 0.1057(10) 0.8855(6) 0.3506(5) 0.043(3) Uani 1 1 d . . . C54 C 0.0363(13) 0.8638(7) 0.4130(7) 0.090(5) Uani 1 1 d . . . H54 H 0.0401 0.8135 0.4425 0.108 Uiso 1 1 calc R . . C55 C -0.0387(16) 0.9145(8) 0.4332(9) 0.125(7) Uani 1 1 d . . . H55 H -0.0850 0.8976 0.4762 0.150 Uiso 1 1 calc R . . C56 C -0.0487(13) 0.9889(8) 0.3930(8) 0.081(4) Uani 1 1 d . . . H56 H -0.0985 1.0227 0.4087 0.097 Uiso 1 1 calc R . . C57 C 0.0157(15) 1.0120(7) 0.3297(7) 0.079(4) Uani 1 1 d . . . H57 H 0.0082 1.0619 0.2993 0.095 Uiso 1 1 calc R . . C58 C 0.0926(13) 0.9602(6) 0.3113(6) 0.071(4) Uani 1 1 d . . . H58 H 0.1397 0.9774 0.2685 0.085 Uiso 1 1 calc R . . C59 C 0.1736(10) 0.7312(5) 0.3859(5) 0.041(3) Uani 1 1 d . . . C60 C 0.0842(11) 0.6866(6) 0.3742(6) 0.062(3) Uani 1 1 d . . . H60 H 0.0475 0.7009 0.3298 0.074 Uiso 1 1 calc R . . C61 C 0.0478(13) 0.6215(6) 0.4270(7) 0.073(4) Uani 1 1 d . . . H61 H -0.0120 0.5919 0.4177 0.088 Uiso 1 1 calc R . . C62 C 0.0986(12) 0.6003(6) 0.4924(7) 0.066(4) Uani 1 1 d . . . H62 H 0.0724 0.5570 0.5285 0.079 Uiso 1 1 calc R . . C63 C 0.1891(12) 0.6435(7) 0.5048(6) 0.063(3) Uani 1 1 d . . . H63 H 0.2247 0.6291 0.5495 0.076 Uiso 1 1 calc R . . C64 C 0.2274(11) 0.7074(6) 0.4521(5) 0.050(3) Uani 1 1 d . . . H64 H 0.2906 0.7353 0.4610 0.060 Uiso 1 1 calc R . . C65 C 0.4166(14) 1.0332(6) 0.3126(6) 0.079(4) Uani 1 1 d . . . H65A H 0.4445 1.0603 0.3414 0.118 Uiso 1 1 calc R . . H65B H 0.3256 1.0409 0.3074 0.118 Uiso 1 1 calc R . . H65C H 0.4587 1.0511 0.2664 0.118 Uiso 1 1 calc R . . C66 C 0.3768(13) 0.9212(7) 0.4422(6) 0.082(4) Uani 1 1 d . . . H66A H 0.3977 0.9617 0.4576 0.123 Uiso 1 1 calc R . . H66B H 0.4054 0.8740 0.4765 0.123 Uiso 1 1 calc R . . H66C H 0.2858 0.9217 0.4379 0.123 Uiso 1 1 calc R . . C67 C 0.6193(12) 0.9435(8) 0.3785(7) 0.089(5) Uani 1 1 d . . . H67A H 0.6741 0.9554 0.3365 0.134 Uiso 1 1 calc R . . H67B H 0.6501 0.8972 0.4133 0.134 Uiso 1 1 calc R . . H67C H 0.6193 0.9834 0.3978 0.134 Uiso 1 1 calc R . . C68 C 0.5181(12) 0.6598(6) 0.3568(7) 0.073(4) Uani 1 1 d . . . H68A H 0.5424 0.6544 0.3119 0.109 Uiso 1 1 calc R . . H68B H 0.4285 0.6512 0.3666 0.109 Uiso 1 1 calc R . . H68C H 0.5667 0.6237 0.3939 0.109 Uiso 1 1 calc R . . C69 C 0.5764(13) 0.7322(7) 0.4486(6) 0.084(4) Uani 1 1 d . . . H69A H 0.6299 0.6870 0.4652 0.126 Uiso 1 1 calc R . . H69B H 0.4956 0.7243 0.4744 0.126 Uiso 1 1 calc R . . H69C H 0.6174 0.7728 0.4561 0.126 Uiso 1 1 calc R . . C70 C 0.7164(11) 0.7650(7) 0.3233(7) 0.077(4) Uani 1 1 d . . . H70A H 0.7540 0.8014 0.3390 0.115 Uiso 1 1 calc R . . H70B H 0.7217 0.7813 0.2722 0.115 Uiso 1 1 calc R . . H70C H 0.7615 0.7171 0.3429 0.115 Uiso 1 1 calc R . . C71 C 0.3315(9) 0.9387(5) 0.1260(5) 0.035(2) Uani 1 1 d . . . C72 C 0.3087(10) 0.9173(6) 0.0649(5) 0.041(3) Uani 1 1 d . . . H72 H 0.3620 0.8859 0.0478 0.049 Uiso 1 1 calc R . . C73 C 0.1931(11) 0.9520(6) 0.0362(6) 0.055(3) Uani 1 1 d . . . H73 H 0.1560 0.9471 -0.0031 0.066 Uiso 1 1 calc R . . C74 C 0.1421(11) 0.9952(6) 0.0756(6) 0.057(3) Uani 1 1 d . . . H74 H 0.0659 1.0242 0.0670 0.068 Uiso 1 1 calc R . . C75 C 0.2275(10) 0.9872(5) 0.1321(5) 0.040(3) Uani 1 1 d . . . H75 H 0.2162 1.0100 0.1665 0.048 Uiso 1 1 calc R . . C76 C 0.1358(9) 0.8193(5) 0.2433(5) 0.037(2) Uani 1 1 d . . . C77 C 0.1879(10) 0.7763(6) 0.2012(5) 0.045(3) Uani 1 1 d . . . H77 H 0.2659 0.7490 0.2077 0.054 Uiso 1 1 calc R . . C78 C 0.0998(12) 0.7829(6) 0.1481(6) 0.055(3) Uani 1 1 d . . . H78 H 0.1083 0.7597 0.1139 0.066 Uiso 1 1 calc R . . C79 C -0.0042(12) 0.8311(7) 0.1561(6) 0.062(3) Uani 1 1 d . . . H79 H -0.0743 0.8464 0.1268 0.074 Uiso 1 1 calc R . . C80 C 0.0158(10) 0.8518(6) 0.2148(5) 0.048(3) Uani 1 1 d . . . H80 H -0.0398 0.8818 0.2324 0.058 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Fe1 0.0387(9) 0.0340(8) 0.0467(9) -0.0166(7) -0.0059(7) -0.0043(7) Fe2 0.0373(9) 0.0404(9) 0.0335(8) -0.0117(7) -0.0069(7) -0.0089(7) Ni1 0.0320(8) 0.0338(7) 0.0306(7) -0.0130(6) -0.0006(6) -0.0072(6) Ni2 0.0362(8) 0.0316(7) 0.0301(7) -0.0087(6) -0.0030(6) -0.0081(6) P1 0.0321(16) 0.0374(15) 0.0368(15) -0.0175(13) -0.0028(12) -0.0087(12) P2 0.0323(16) 0.0336(15) 0.0318(14) -0.0136(12) -0.0001(11) -0.0089(12) P3 0.0460(18) 0.0436(17) 0.0343(16) -0.0121(14) -0.0043(13) -0.0007(14) P4 0.0387(17) 0.0491(17) 0.0361(16) -0.0186(14) 0.0035(13) -0.0087(13) P5 0.0331(16) 0.0327(15) 0.0323(15) -0.0101(12) -0.0042(12) -0.0068(12) P6 0.0390(17) 0.0364(15) 0.0318(15) -0.0093(13) 0.0000(12) -0.0105(12) P7 0.065(2) 0.0450(17) 0.0402(17) -0.0184(15) 0.0032(15) -0.0209(15) P8 0.0491(19) 0.0423(17) 0.0469(18) -0.0050(15) -0.0126(14) -0.0059(14) C1 0.034(6) 0.046(6) 0.046(7) -0.020(6) 0.000(5) -0.007(5) C2 0.041(7) 0.046(7) 0.067(8) -0.024(6) -0.014(6) -0.014(5) C3 0.057(9) 0.045(7) 0.080(10) -0.001(7) 0.004(7) -0.026(6) C4 0.075(10) 0.062(9) 0.075(10) -0.012(8) 0.033(8) -0.016(7) C5 0.061(9) 0.072(9) 0.055(8) -0.013(7) 0.014(7) 0.005(7) C6 0.045(7) 0.056(7) 0.048(7) -0.019(6) 0.005(6) -0.001(6) C7 0.055(8) 0.036(6) 0.039(6) -0.018(5) 0.002(5) -0.015(5) C8 0.026(7) 0.116(11) 0.068(8) -0.049(8) 0.000(6) -0.009(7) C9 0.057(9) 0.095(10) 0.077(10) -0.028(9) -0.018(8) -0.006(8) C10 0.070(10) 0.062(8) 0.068(9) -0.029(7) -0.034(8) -0.002(7) C11 0.092(11) 0.087(10) 0.040(7) -0.033(7) -0.023(7) -0.002(8) C12 0.044(7) 0.053(7) 0.056(7) -0.022(6) -0.002(6) -0.004(6) C13 0.023(5) 0.036(6) 0.038(6) -0.020(5) 0.005(4) -0.009(4) C14 0.050(7) 0.043(6) 0.032(6) -0.015(5) -0.005(5) 0.004(5) C15 0.062(9) 0.076(9) 0.034(7) -0.022(7) -0.001(6) -0.001(7) C16 0.047(8) 0.089(10) 0.060(8) -0.056(8) 0.010(6) -0.015(7) C17 0.049(8) 0.056(7) 0.068(8) -0.045(7) -0.002(6) 0.005(6) C18 0.053(8) 0.060(8) 0.043(7) -0.027(6) 0.001(5) -0.016(6) C19 0.032(6) 0.025(5) 0.050(6) -0.019(5) -0.002(5) -0.004(4) C20 0.062(8) 0.067(8) 0.034(6) -0.022(6) 0.006(6) -0.024(6) C21 0.064(9) 0.102(10) 0.042(7) -0.031(7) 0.019(6) -0.038(8) C22 0.060(9) 0.063(8) 0.055(8) -0.018(7) 0.017(6) -0.022(6) C23 0.056(8) 0.061(8) 0.068(8) -0.028(7) 0.007(7) -0.036(6) C24 0.036(7) 0.058(7) 0.047(6) -0.029(6) 0.008(5) -0.010(5) C25 0.074(9) 0.064(8) 0.039(7) -0.024(6) -0.013(6) 0.000(6) C26 0.095(10) 0.038(7) 0.049(7) -0.005(6) 0.005(7) -0.006(6) C27 0.054(8) 0.070(8) 0.056(8) -0.008(7) -0.014(6) 0.005(6) C28 0.048(8) 0.093(9) 0.048(7) -0.036(7) 0.010(6) -0.007(7) C29 0.056(8) 0.062(8) 0.069(8) -0.032(7) 0.002(6) 0.011(6) C30 0.039(7) 0.097(10) 0.057(8) -0.038(7) 0.010(6) -0.011(7) C31 0.042(7) 0.036(6) 0.044(6) -0.021(5) -0.005(5) -0.010(5) C32 0.055(8) 0.033(6) 0.056(7) -0.010(6) -0.013(6) -0.012(6) C33 0.059(9) 0.038(7) 0.071(8) -0.027(7) -0.006(7) 0.011(6) C34 0.036(7) 0.073(8) 0.063(8) -0.041(7) 0.002(6) 0.003(6) C35 0.032(6) 0.048(6) 0.037(6) -0.017(5) -0.003(5) 0.002(5) C36 0.036(6) 0.035(6) 0.041(6) -0.019(5) 0.001(5) -0.015(5) C37 0.048(7) 0.047(7) 0.047(7) -0.021(6) -0.008(5) 0.002(6) C38 0.070(9) 0.038(6) 0.043(7) -0.002(6) -0.035(6) 0.014(6) C39 0.041(7) 0.051(7) 0.073(9) -0.024(7) -0.022(7) 0.005(6) C40 0.044(7) 0.045(7) 0.054(7) -0.013(6) -0.018(6) -0.010(6) C41 0.037(6) 0.041(6) 0.027(6) -0.006(5) 0.005(5) -0.016(5) C42 0.044(7) 0.058(7) 0.054(7) -0.010(6) -0.007(6) -0.018(6) C43 0.048(8) 0.083(10) 0.083(10) -0.025(8) -0.014(7) -0.023(8) C44 0.067(10) 0.079(10) 0.093(11) -0.050(9) 0.021(8) -0.045(8) C45 0.085(10) 0.037(7) 0.056(8) -0.023(6) 0.025(7) -0.020(6) C46 0.056(8) 0.041(6) 0.044(7) -0.015(6) 0.002(5) -0.022(6) C47 0.032(6) 0.042(6) 0.033(6) -0.014(5) -0.003(5) -0.009(5) C48 0.057(8) 0.052(7) 0.050(7) -0.025(6) -0.014(6) -0.006(6) C49 0.068(9) 0.078(9) 0.052(8) -0.036(7) 0.004(6) 0.008(7) C50 0.043(8) 0.070(9) 0.079(10) -0.047(8) -0.013(7) 0.013(7) C51 0.074(10) 0.039(7) 0.072(9) -0.020(7) -0.006(7) -0.009(7) C52 0.041(7) 0.042(7) 0.047(7) -0.014(6) -0.008(5) -0.003(5) C53 0.042(7) 0.043(7) 0.042(7) -0.011(6) -0.005(5) -0.007(5) C54 0.088(11) 0.067(9) 0.080(10) 0.006(8) 0.048(9) 0.032(8) C55 0.145(16) 0.068(10) 0.118(14) 0.006(10) 0.082(12) 0.033(10) C56 0.068(10) 0.085(11) 0.104(12) -0.051(10) 0.004(9) 0.001(8) C57 0.118(13) 0.057(9) 0.065(9) -0.024(8) -0.004(9) 0.002(8) C58 0.116(12) 0.047(8) 0.050(8) -0.023(7) 0.034(7) -0.006(7) C59 0.044(7) 0.041(6) 0.032(6) -0.007(5) 0.005(5) -0.004(5) C60 0.076(9) 0.057(8) 0.053(8) -0.015(7) -0.015(6) -0.025(7) C61 0.097(11) 0.046(8) 0.070(9) -0.007(7) 0.003(8) -0.035(7) C62 0.075(10) 0.044(7) 0.062(9) 0.004(7) 0.003(7) -0.016(7) C63 0.070(9) 0.064(8) 0.043(7) -0.004(7) 0.001(6) 0.005(7) C64 0.060(8) 0.051(7) 0.037(7) -0.009(6) 0.003(6) -0.016(6) C65 0.125(13) 0.051(8) 0.069(9) -0.035(7) 0.026(8) -0.010(8) C66 0.117(12) 0.096(10) 0.049(8) -0.043(8) 0.026(7) -0.047(9) C67 0.063(10) 0.135(12) 0.097(11) -0.070(10) 0.013(8) -0.046(9) C68 0.077(10) 0.038(7) 0.094(10) -0.010(7) -0.023(8) 0.004(6) C69 0.091(11) 0.082(10) 0.062(9) 0.000(8) -0.036(8) 0.005(8) C70 0.046(8) 0.069(9) 0.102(11) -0.014(8) -0.023(7) 0.014(7) C71 0.037(6) 0.035(6) 0.027(5) -0.002(5) 0.000(4) -0.010(5) C72 0.037(7) 0.051(7) 0.035(6) -0.014(5) -0.006(5) -0.004(5) C73 0.047(8) 0.078(9) 0.042(7) -0.020(7) -0.006(6) -0.018(6) C74 0.049(8) 0.049(7) 0.062(8) -0.004(7) -0.022(6) 0.009(6) C75 0.047(7) 0.032(6) 0.042(6) -0.013(5) 0.001(5) -0.005(5) C76 0.034(6) 0.038(6) 0.039(6) -0.010(5) -0.011(5) -0.012(5) C77 0.052(7) 0.043(6) 0.034(6) -0.004(5) -0.005(5) -0.015(5) C78 0.069(9) 0.053(7) 0.050(7) -0.022(6) -0.017(6) -0.020(7) C79 0.045(8) 0.071(8) 0.067(9) -0.014(7) -0.018(6) -0.018(7) C80 0.033(7) 0.070(8) 0.043(7) -0.020(6) 0.000(5) -0.016(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Fe1 C38 2.034(10) . ? Fe1 C32 2.041(10) . ? Fe1 C35 2.041(9) . ? Fe1 C37 2.041(10) . ? Fe1 C31 2.045(10) . ? Fe1 C40 2.049(10) . ? Fe1 C34 2.050(10) . ? Fe1 C33 2.058(10) . ? Fe1 C39 2.061(11) . ? Fe1 C36 2.070(9) . ? Fe2 C74 2.019(10) . ? Fe2 C75 2.020(9) . ? Fe2 C77 2.028(10) . ? Fe2 C79 2.033(11) . ? Fe2 C76 2.034(9) . ? Fe2 C73 2.035(10) . ? Fe2 C71 2.046(9) . ? Fe2 C78 2.047(10) . ? Fe2 C80 2.055(10) . ? Fe2 C72 2.056(10) . ? Ni1 P1 2.149(3) . ? Ni1 P2 2.153(3) . ? Ni1 P3 2.183(3) . ? Ni1 P4 2.191(3) . ? Ni2 P6 2.164(3) . ? Ni2 P5 2.168(3) . ? Ni2 P7 2.188(3) . ? Ni2 P8 2.188(3) . ? P1 C31 1.809(10) . ? P1 C7 1.833(10) . ? P1 C1 1.856(10) . ? P2 C36 1.800(10) . ? P2 C13 1.837(9) . ? P2 C19 1.858(9) . ? P3 C27 1.815(11) . ? P3 C26 1.822(10) . ? P3 C25 1.825(10) . ? P4 C30 1.844(11) . ? P4 C28 1.848(10) . ? P4 C29 1.850(10) . ? P5 C47 1.826(10) . ? P5 C71 1.837(10) . ? P5 C41 1.844(9) . ? P6 C76 1.830(9) . ? P6 C59 1.865(10) . ? P6 C53 1.869(11) . ? P7 C65 1.825(11) . ? P7 C67 1.831(12) . ? P7 C66 1.837(11) . ? P8 C70 1.812(12) . ? P8 C69 1.833(11) . ? P8 C68 1.848(11) . ? C1 C6 1.373(13) . ? C1 C2 1.413(13) . ? C2 C3 1.384(14) . ? C3 C4 1.349(16) . ? C4 C5 1.409(16) . ? C5 C6 1.379(14) . ? C7 C8 1.372(14) . ? C7 C12 1.376(13) . ? C8 C9 1.356(15) . ? C9 C10 1.353(16) . ? C10 C11 1.342(16) . ? C11 C12 1.398(14) . ? C13 C14 1.364(12) . ? C13 C18 1.403(13) . ? C14 C15 1.399(13) . ? C15 C16 1.358(14) . ? C16 C17 1.381(14) . ? C17 C18 1.360(13) . ? C19 C24 1.369(12) . ? C19 C20 1.390(13) . ? C20 C21 1.401(14) . ? C21 C22 1.359(15) . ? C22 C23 1.366(14) . ? C23 C24 1.384(13) . ? C31 C35 1.441(13) . ? C31 C32 1.450(13) . ? C32 C33 1.411(14) . ? C33 C34 1.407(14) . ? C34 C35 1.430(13) . ? C36 C37 1.423(13) . ? C36 C40 1.429(13) . ? C37 C38 1.448(14) . ? C38 C39 1.383(15) . ? C39 C40 1.437(13) . ? C41 C42 1.370(13) . ? C41 C46 1.371(12) . ? C42 C43 1.387(15) . ? C43 C44 1.376(16) . ? C44 C45 1.362(16) . ? C45 C46 1.440(14) . ? C47 C52 1.392(13) . ? C47 C48 1.410(13) . ? C48 C49 1.387(14) . ? C49 C50 1.356(15) . ? C50 C51 1.353(15) . ? C51 C52 1.370(14) . ? C53 C54 1.358(14) . ? C53 C58 1.361(13) . ? C54 C55 1.360(17) . ? C55 C56 1.357(17) . ? C56 C57 1.348(17) . ? C57 C58 1.370(16) . ? C59 C60 1.374(14) . ? C59 C64 1.380(13) . ? C60 C61 1.375(14) . ? C61 C62 1.355(16) . ? C62 C63 1.371(16) . ? C63 C64 1.366(14) . ? C71 C75 1.412(13) . ? C71 C72 1.448(13) . ? C72 C73 1.393(13) . ? C73 C74 1.388(15) . ? C74 C75 1.436(13) . ? C76 C80 1.421(13) . ? C76 C77 1.431(13) . ? C77 C78 1.410(13) . ? C78 C79 1.419(15) . ? C79 C80 1.389(14) . ? 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 C38 Fe1 C32 111.5(5) . . ? C38 Fe1 C35 177.4(4) . . ? C32 Fe1 C35 68.5(4) . . ? C38 Fe1 C37 41.6(4) . . ? C32 Fe1 C37 111.5(5) . . ? C35 Fe1 C37 135.8(4) . . ? C38 Fe1 C31 137.0(5) . . ? C32 Fe1 C31 41.6(4) . . ? C35 Fe1 C31 41.3(4) . . ? C37 Fe1 C31 107.8(4) . . ? C38 Fe1 C40 67.4(4) . . ? C32 Fe1 C40 178.9(4) . . ? C35 Fe1 C40 112.6(4) . . ? C37 Fe1 C40 67.9(4) . . ? C31 Fe1 C40 139.4(4) . . ? C38 Fe1 C34 141.6(5) . . ? C32 Fe1 C34 67.7(5) . . ? C35 Fe1 C34 40.9(4) . . ? C37 Fe1 C34 176.7(4) . . ? C31 Fe1 C34 69.4(4) . . ? C40 Fe1 C34 113.0(5) . . ? C38 Fe1 C33 113.4(4) . . ? C32 Fe1 C33 40.3(4) . . ? C35 Fe1 C33 68.4(4) . . ? C37 Fe1 C33 141.2(5) . . ? C31 Fe1 C33 69.5(4) . . ? C40 Fe1 C33 139.7(5) . . ? C34 Fe1 C33 40.1(4) . . ? C38 Fe1 C39 39.5(4) . . ? C32 Fe1 C39 138.1(4) . . ? C35 Fe1 C39 142.1(5) . . ? C37 Fe1 C39 68.6(5) . . ? C31 Fe1 C39 176.2(5) . . ? C40 Fe1 C39 40.9(4) . . ? C34 Fe1 C39 114.3(5) . . ? C33 Fe1 C39 112.5(5) . . ? C38 Fe1 C36 68.8(4) . . ? C32 Fe1 C36 139.5(4) . . ? C35 Fe1 C36 109.5(4) . . ? C37 Fe1 C36 40.5(4) . . ? C31 Fe1 C36 109.1(4) . . ? C40 Fe1 C36 40.6(4) . . ? C34 Fe1 C36 138.2(4) . . ? C33 Fe1 C36 177.9(4) . . ? C39 Fe1 C36 69.0(4) . . ? C74 Fe2 C75 41.7(4) . . ? C74 Fe2 C77 177.4(5) . . ? C75 Fe2 C77 138.4(4) . . ? C74 Fe2 C79 113.0(5) . . ? C75 Fe2 C79 140.7(5) . . ? C77 Fe2 C79 68.5(5) . . ? C74 Fe2 C76 141.1(5) . . ? C75 Fe2 C76 111.4(4) . . ? C77 Fe2 C76 41.3(4) . . ? C79 Fe2 C76 68.1(4) . . ? C74 Fe2 C73 40.0(4) . . ? C75 Fe2 C73 68.6(4) . . ? C77 Fe2 C73 137.6(5) . . ? C79 Fe2 C73 113.1(4) . . ? C76 Fe2 C73 178.3(5) . . ? C74 Fe2 C71 69.0(4) . . ? C75 Fe2 C71 40.6(4) . . ? C77 Fe2 C71 109.5(4) . . ? C79 Fe2 C71 178.0(4) . . ? C76 Fe2 C71 110.2(4) . . ? C73 Fe2 C71 68.6(4) . . ? C74 Fe2 C78 139.4(4) . . ? C75 Fe2 C78 178.5(5) . . ? C77 Fe2 C78 40.5(4) . . ? C79 Fe2 C78 40.7(4) . . ? C76 Fe2 C78 68.4(4) . . ? C73 Fe2 C78 111.6(4) . . ? C71 Fe2 C78 137.9(5) . . ? C74 Fe2 C80 114.0(5) . . ? C75 Fe2 C80 113.2(4) . . ? C77 Fe2 C80 68.5(4) . . ? C79 Fe2 C80 39.7(4) . . ? C76 Fe2 C80 40.7(4) . . ? C73 Fe2 C80 141.0(4) . . ? C71 Fe2 C80 139.6(4) . . ? C78 Fe2 C80 67.7(5) . . ? C74 Fe2 C72 67.6(4) . . ? C75 Fe2 C72 68.5(4) . . ? C77 Fe2 C72 109.8(4) . . ? C79 Fe2 C72 139.3(4) . . ? C76 Fe2 C72 138.5(4) . . ? C73 Fe2 C72 39.8(4) . . ? C71 Fe2 C72 41.4(4) . . ? C78 Fe2 C72 110.6(5) . . ? C80 Fe2 C72 178.2(4) . . ? P1 Ni1 P2 109.04(11) . . ? P1 Ni1 P3 108.37(11) . . ? P2 Ni1 P3 112.61(11) . . ? P1 Ni1 P4 112.55(11) . . ? P2 Ni1 P4 110.35(12) . . ? P3 Ni1 P4 103.88(12) . . ? P6 Ni2 P5 109.53(11) . . ? P6 Ni2 P7 109.79(12) . . ? P5 Ni2 P7 108.86(12) . . ? P6 Ni2 P8 112.33(12) . . ? P5 Ni2 P8 112.28(12) . . ? P7 Ni2 P8 103.85(13) . . ? C31 P1 C7 101.5(5) . . ? C31 P1 C1 99.5(4) . . ? C7 P1 C1 98.8(4) . . ? C31 P1 Ni1 117.7(3) . . ? C7 P1 Ni1 116.0(3) . . ? C1 P1 Ni1 119.9(3) . . ? C36 P2 C13 101.8(4) . . ? C36 P2 C19 98.8(4) . . ? C13 P2 C19 96.9(4) . . ? C36 P2 Ni1 119.3(3) . . ? C13 P2 Ni1 113.7(3) . . ? C19 P2 Ni1 122.3(3) . . ? C27 P3 C26 99.2(6) . . ? C27 P3 C25 98.9(5) . . ? C26 P3 C25 98.8(5) . . ? C27 P3 Ni1 117.5(4) . . ? C26 P3 Ni1 117.3(4) . . ? C25 P3 Ni1 121.1(4) . . ? C30 P4 C28 98.4(5) . . ? C30 P4 C29 98.0(5) . . ? C28 P4 C29 97.8(5) . . ? C30 P4 Ni1 117.9(4) . . ? C28 P4 Ni1 122.9(4) . . ? C29 P4 Ni1 117.0(4) . . ? C47 P5 C71 97.6(4) . . ? C47 P5 C41 98.3(4) . . ? C71 P5 C41 100.1(4) . . ? C47 P5 Ni2 119.0(3) . . ? C71 P5 Ni2 120.7(3) . . ? C41 P5 Ni2 116.8(3) . . ? C76 P6 C59 98.3(4) . . ? C76 P6 C53 100.0(5) . . ? C59 P6 C53 97.8(5) . . ? C76 P6 Ni2 117.7(3) . . ? C59 P6 Ni2 120.8(3) . . ? C53 P6 Ni2 118.0(3) . . ? C65 P7 C67 96.4(7) . . ? C65 P7 C66 97.5(6) . . ? C67 P7 C66 98.2(6) . . ? C65 P7 Ni2 120.6(4) . . ? C67 P7 Ni2 120.3(5) . . ? C66 P7 Ni2 118.6(4) . . ? C70 P8 C69 97.2(6) . . ? C70 P8 C68 102.5(6) . . ? C69 P8 C68 96.7(6) . . ? C70 P8 Ni2 116.7(4) . . ? C69 P8 Ni2 117.4(4) . . ? C68 P8 Ni2 121.9(4) . . ? C6 C1 C2 117.9(10) . . ? C6 C1 P1 118.7(8) . . ? C2 C1 P1 123.3(8) . . ? C3 C2 C1 119.4(10) . . ? C4 C3 C2 122.7(12) . . ? C3 C4 C5 117.9(12) . . ? C6 C5 C4 120.3(12) . . ? C1 C6 C5 121.7(11) . . ? C8 C7 C12 115.8(10) . . ? C8 C7 P1 120.1(8) . . ? C12 C7 P1 123.9(9) . . ? C9 C8 C7 122.8(12) . . ? C10 C9 C8 121.1(13) . . ? C11 C10 C9 118.3(12) . . ? C10 C11 C12 121.3(12) . . ? C7 C12 C11 120.7(11) . . ? C14 C13 C18 118.4(9) . . ? C14 C13 P2 124.7(7) . . ? C18 C13 P2 116.9(7) . . ? C13 C14 C15 121.1(10) . . ? C16 C15 C14 118.6(10) . . ? C15 C16 C17 121.8(10) . . ? C18 C17 C16 118.9(11) . . ? C17 C18 C13 121.2(10) . . ? C24 C19 C20 117.6(9) . . ? C24 C19 P2 124.6(8) . . ? C20 C19 P2 117.8(7) . . ? C19 C20 C21 119.5(10) . . ? C22 C21 C20 122.1(11) . . ? C21 C22 C23 117.8(10) . . ? C22 C23 C24 121.1(10) . . ? C19 C24 C23 121.7(10) . . ? C35 C31 C32 105.3(9) . . ? C35 C31 P1 123.1(7) . . ? C32 C31 P1 131.5(8) . . ? C35 C31 Fe1 69.2(5) . . ? C32 C31 Fe1 69.1(5) . . ? P1 C31 Fe1 123.1(5) . . ? C33 C32 C31 109.6(9) . . ? C33 C32 Fe1 70.5(6) . . ? C31 C32 Fe1 69.4(5) . . ? C34 C33 C32 107.9(9) . . ? C34 C33 Fe1 69.7(6) . . ? C32 C33 Fe1 69.2(6) . . ? C33 C34 C35 108.7(10) . . ? C33 C34 Fe1 70.3(6) . . ? C35 C34 Fe1 69.2(6) . . ? C34 C35 C31 108.5(9) . . ? C34 C35 Fe1 69.9(6) . . ? C31 C35 Fe1 69.5(5) . . ? C37 C36 C40 106.4(9) . . ? C37 C36 P2 125.0(8) . . ? C40 C36 P2 128.4(7) . . ? C37 C36 Fe1 68.7(5) . . ? C40 C36 Fe1 68.9(5) . . ? P2 C36 Fe1 123.5(5) . . ? C36 C37 C38 107.7(10) . . ? C36 C37 Fe1 70.8(6) . . ? C38 C37 Fe1 68.9(6) . . ? C39 C38 C37 109.4(10) . . ? C39 C38 Fe1 71.3(6) . . ? C37 C38 Fe1 69.4(5) . . ? C38 C39 C40 107.0(10) . . ? C38 C39 Fe1 69.2(6) . . ? C40 C39 Fe1 69.1(6) . . ? C36 C40 C39 109.5(10) . . ? C36 C40 Fe1 70.5(5) . . ? C39 C40 Fe1 70.0(6) . . ? C42 C41 C46 117.1(9) . . ? C42 C41 P5 119.3(8) . . ? C46 C41 P5 123.5(7) . . ? C41 C42 C43 124.1(11) . . ? C44 C43 C42 118.2(11) . . ? C45 C44 C43 120.5(11) . . ? C44 C45 C46 119.7(11) . . ? C41 C46 C45 120.3(10) . . ? C52 C47 C48 115.1(9) . . ? C52 C47 P5 121.1(8) . . ? C48 C47 P5 123.9(8) . . ? C49 C48 C47 121.1(11) . . ? C50 C49 C48 120.2(12) . . ? C51 C50 C49 120.9(11) . . ? C50 C51 C52 119.2(11) . . ? C51 C52 C47 123.5(10) . . ? C54 C53 C58 114.8(11) . . ? C54 C53 P6 125.5(9) . . ? C58 C53 P6 119.6(8) . . ? C53 C54 C55 121.1(12) . . ? C56 C55 C54 122.7(14) . . ? C57 C56 C55 117.9(14) . . ? C56 C57 C58 118.2(13) . . ? C53 C58 C57 125.2(11) . . ? C60 C59 C64 117.5(10) . . ? C60 C59 P6 124.2(8) . . ? C64 C59 P6 118.2(8) . . ? C59 C60 C61 121.3(11) . . ? C62 C61 C60 120.3(12) . . ? C61 C62 C63 119.2(11) . . ? C64 C63 C62 120.6(11) . . ? C63 C64 C59 120.9(11) . . ? C75 C71 C72 106.7(8) . . ? C75 C71 P5 125.3(7) . . ? C72 C71 P5 127.7(8) . . ? C75 C71 Fe2 68.7(5) . . ? C72 C71 Fe2 69.7(5) . . ? P5 C71 Fe2 122.6(5) . . ? C73 C72 C71 108.0(9) . . ? C73 C72 Fe2 69.3(6) . . ? C71 C72 Fe2 68.9(5) . . ? C74 C73 C72 109.3(10) . . ? C74 C73 Fe2 69.4(6) . . ? C72 C73 Fe2 70.9(6) . . ? C73 C74 C75 108.1(10) . . ? C73 C74 Fe2 70.6(6) . . ? C75 C74 Fe2 69.2(5) . . ? C71 C75 C74 107.8(9) . . ? C71 C75 Fe2 70.7(5) . . ? C74 C75 Fe2 69.1(6) . . ? C80 C76 C77 107.5(9) . . ? C80 C76 P6 131.5(8) . . ? C77 C76 P6 121.0(8) . . ? C80 C76 Fe2 70.5(5) . . ? C77 C76 Fe2 69.2(5) . . ? P6 C76 Fe2 126.4(5) . . ? C78 C77 C76 107.6(10) . . ? C78 C77 Fe2 70.5(6) . . ? C76 C77 Fe2 69.6(6) . . ? C77 C78 C79 107.8(10) . . ? C77 C78 Fe2 69.0(6) . . ? C79 C78 Fe2 69.1(6) . . ? C80 C79 C78 108.9(10) . . ? C80 C79 Fe2 71.0(6) . . ? C78 C79 Fe2 70.2(6) . . ? C79 C80 C76 108.2(10) . . ? C79 C80 Fe2 69.3(6) . . ? C76 C80 Fe2 68.9(6) . . ? _diffrn_measured_fraction_theta_max 0.986 _diffrn_reflns_theta_full 23.34 _diffrn_measured_fraction_theta_full 0.986 _refine_diff_density_max 0.709 _refine_diff_density_min -0.586 _refine_diff_density_rms 0.188 # Attachment '- 8.cif' data_8 _database_code_depnum_ccdc_archive 'CCDC 780561' #TrackingRef '- 8.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H46 Co Fe P4' _chemical_formula_sum 'C40 H46 Co Fe P4' _chemical_formula_weight 765.43 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Fe Fe 0.3463 0.8444 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.524(3) _cell_length_b 18.946(6) _cell_length_c 20.071(6) _cell_angle_alpha 69.857(6) _cell_angle_beta 87.349(6) _cell_angle_gamma 87.141(6) _cell_volume 3750.7(19) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 5688 _cell_measurement_theta_min 1.08 _cell_measurement_theta_max 24.00 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.36 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.356 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1596 _exptl_absorpt_coefficient_mu 1.027 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7088 _exptl_absorpt_correction_T_max 0.7619 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17348 _diffrn_reflns_av_R_equivalents 0.0646 _diffrn_reflns_av_sigmaI/netI 0.1511 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.08 _diffrn_reflns_theta_max 24.00 _reflns_number_total 11701 _reflns_number_gt 5688 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1147P)^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 11701 _refine_ls_number_parameters 841 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1588 _refine_ls_R_factor_gt 0.0693 _refine_ls_wR_factor_ref 0.2500 _refine_ls_wR_factor_gt 0.1625 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.005 _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 C1 C 0.1699(9) 0.0602(5) 0.3745(5) 0.038(2) Uani 1 1 d . . . C2 C 0.2727(9) 0.0113(5) 0.3675(5) 0.042(2) Uani 1 1 d . . . H2 H 0.2828 -0.0122 0.3310 0.050 Uiso 1 1 calc R . . C3 C 0.3586(11) 0.0025(6) 0.4231(6) 0.059(3) Uani 1 1 d . . . H3 H 0.4385 -0.0277 0.4310 0.071 Uiso 1 1 calc R . . C4 C 0.3098(10) 0.0454(6) 0.4637(5) 0.054(3) Uani 1 1 d . . . H4 H 0.3496 0.0504 0.5050 0.065 Uiso 1 1 calc R . . C5 C 0.1943(11) 0.0808(6) 0.4345(5) 0.054(3) Uani 1 1 d . . . H5 H 0.1400 0.1144 0.4522 0.065 Uiso 1 1 calc R . . C6 C 0.3671(10) 0.1798(5) 0.2572(5) 0.044(3) Uani 1 1 d . . . C7 C 0.4829(9) 0.1486(6) 0.2861(6) 0.051(3) Uani 1 1 d . . . H7 H 0.5394 0.1155 0.2688 0.061 Uiso 1 1 calc R . . C8 C 0.5053(10) 0.1693(6) 0.3449(6) 0.060(3) Uani 1 1 d . . . H8 H 0.5796 0.1543 0.3749 0.072 Uiso 1 1 calc R . . C9 C 0.4006(14) 0.2155(6) 0.3532(6) 0.071(4) Uani 1 1 d . . . H9 H 0.3903 0.2380 0.3905 0.085 Uiso 1 1 calc R . . C10 C 0.3113(10) 0.2231(5) 0.2997(5) 0.047(3) Uani 1 1 d . . . H10 H 0.2309 0.2528 0.2919 0.056 Uiso 1 1 calc R . . C11 C 0.3328(10) 0.2674(5) 0.1150(5) 0.049(3) Uani 1 1 d . . . C12 C 0.4207(11) 0.3123(6) 0.1263(6) 0.066(3) Uani 1 1 d . . . H12 H 0.4600 0.2976 0.1697 0.079 Uiso 1 1 calc R . . C13 C 0.4523(13) 0.3794(7) 0.0740(7) 0.079(4) Uani 1 1 d . . . H13 H 0.5099 0.4103 0.0833 0.094 Uiso 1 1 calc R . . C14 C 0.3994(14) 0.4003(7) 0.0092(7) 0.076(4) Uani 1 1 d . . . H14 H 0.4231 0.4445 -0.0263 0.091 Uiso 1 1 calc R . . C15 C 0.3121(12) 0.3567(7) -0.0036(7) 0.072(4) Uani 1 1 d . . . H15 H 0.2775 0.3702 -0.0483 0.087 Uiso 1 1 calc R . . C16 C 0.2747(11) 0.2925(6) 0.0497(6) 0.064(3) Uani 1 1 d . . . H16 H 0.2092 0.2653 0.0419 0.077 Uiso 1 1 calc R . . C17 C -0.0532(9) 0.1492(5) 0.3591(5) 0.040(2) Uani 1 1 d . . . C18 C -0.0557(10) 0.2271(6) 0.3312(6) 0.052(3) Uani 1 1 d . . . H18 H -0.0117 0.2500 0.2884 0.062 Uiso 1 1 calc R . . C19 C -0.1188(10) 0.2716(6) 0.3630(7) 0.060(3) Uani 1 1 d . . . H19 H -0.1165 0.3237 0.3428 0.072 Uiso 1 1 calc R . . C20 C -0.1833(12) 0.2401(7) 0.4229(7) 0.069(4) Uani 1 1 d . . . H20 H -0.2281 0.2704 0.4446 0.083 Uiso 1 1 calc R . . C21 C -0.1858(11) 0.1626(7) 0.4543(6) 0.066(3) Uani 1 1 d . . . H21 H -0.2303 0.1409 0.4971 0.079 Uiso 1 1 calc R . . C22 C -0.1207(9) 0.1176(6) 0.4209(6) 0.052(3) Uani 1 1 d . . . H22 H -0.1233 0.0655 0.4410 0.063 Uiso 1 1 calc R . . C23 C 0.3970(9) 0.1131(6) 0.1512(5) 0.042(2) Uani 1 1 d . . . C24 C 0.4140(13) 0.0394(7) 0.1904(7) 0.083(4) Uani 1 1 d . . . H24 H 0.3719 0.0231 0.2345 0.100 Uiso 1 1 calc R . . C25 C 0.4850(15) -0.0128(7) 0.1729(8) 0.090(5) Uani 1 1 d . . . H25 H 0.4903 -0.0624 0.2034 0.108 Uiso 1 1 calc R . . C26 C 0.5483(14) 0.0091(8) 0.1095(10) 0.101(5) Uani 1 1 d . . . H26 H 0.5998 -0.0250 0.0956 0.121 Uiso 1 1 calc R . . C27 C 0.5351(18) 0.0817(9) 0.0667(9) 0.144(8) Uani 1 1 d . . . H27 H 0.5760 0.0979 0.0222 0.173 Uiso 1 1 calc R . . C28 C 0.4592(13) 0.1327(7) 0.0896(8) 0.098(5) Uani 1 1 d . . . H28 H 0.4528 0.1826 0.0598 0.118 Uiso 1 1 calc R . . C29 C -0.0627(9) 0.0108(5) 0.3414(5) 0.042(2) Uani 1 1 d . . . C30 C -0.1764(11) 0.0170(7) 0.3135(6) 0.064(3) Uani 1 1 d . . . H30 H -0.2035 0.0627 0.2806 0.077 Uiso 1 1 calc R . . C31 C -0.2558(13) -0.0440(10) 0.3326(7) 0.095(5) Uani 1 1 d . . . H31 H -0.3367 -0.0387 0.3143 0.114 Uiso 1 1 calc R . . C32 C -0.2126(17) -0.1126(8) 0.3793(8) 0.086(5) Uani 1 1 d . . . H32 H -0.2644 -0.1538 0.3920 0.103 Uiso 1 1 calc R . . C33 C -0.0994(12) -0.1199(7) 0.4058(6) 0.061(3) Uani 1 1 d . . . H33 H -0.0712 -0.1659 0.4377 0.073 Uiso 1 1 calc R . . C34 C -0.0221(11) -0.0589(5) 0.3861(5) 0.052(3) Uani 1 1 d . . . H34 H 0.0595 -0.0650 0.4036 0.062 Uiso 1 1 calc R . . C35 C -0.2171(10) 0.2355(7) 0.1749(7) 0.087(4) Uani 1 1 d . . . H35A H -0.2224 0.2221 0.2256 0.130 Uiso 1 1 calc R . . H35B H -0.2545 0.1973 0.1616 0.130 Uiso 1 1 calc R . . H35C H -0.2619 0.2827 0.1534 0.130 Uiso 1 1 calc R . . C36 C -0.0282(13) 0.3391(6) 0.1424(8) 0.101(5) Uani 1 1 d . . . H36A H -0.0788 0.3739 0.1059 0.151 Uiso 1 1 calc R . . H36B H 0.0600 0.3503 0.1322 0.151 Uiso 1 1 calc R . . H36C H -0.0532 0.3436 0.1874 0.151 Uiso 1 1 calc R . . C37 C -0.0839(14) 0.2656(8) 0.0500(6) 0.098(5) Uani 1 1 d . . . H37A H -0.1205 0.2231 0.0435 0.147 Uiso 1 1 calc R . . H37B H -0.0055 0.2768 0.0227 0.147 Uiso 1 1 calc R . . H37C H -0.1421 0.3083 0.0344 0.147 Uiso 1 1 calc R . . C38 C 0.1273(12) 0.0808(8) 0.0596(6) 0.087(4) Uani 1 1 d . . . H38A H 0.1999 0.1112 0.0547 0.130 Uiso 1 1 calc R . . H38B H 0.0694 0.1057 0.0224 0.130 Uiso 1 1 calc R . . H38C H 0.1546 0.0329 0.0565 0.130 Uiso 1 1 calc R . . C39 C -0.1208(12) 0.0536(8) 0.1266(7) 0.096(5) Uani 1 1 d . . . H39A H -0.1632 0.1018 0.1060 0.144 Uiso 1 1 calc R . . H39B H -0.1655 0.0253 0.1696 0.144 Uiso 1 1 calc R . . H39C H -0.1196 0.0268 0.0937 0.144 Uiso 1 1 calc R . . C40 C 0.0961(17) -0.0327(6) 0.1907(7) 0.116(6) Uani 1 1 d . . . H40A H 0.0864 -0.0599 0.1589 0.174 Uiso 1 1 calc R . . H40B H 0.0442 -0.0542 0.2329 0.174 Uiso 1 1 calc R . . H40C H 0.1837 -0.0358 0.2032 0.174 Uiso 1 1 calc R . . C41 C 0.4491(8) 0.4899(5) 0.2465(5) 0.038(2) Uani 1 1 d . . . C42 C 0.5426(10) 0.5235(6) 0.1952(5) 0.050(3) Uani 1 1 d . . . H42 H 0.5387 0.5755 0.1621 0.060 Uiso 1 1 calc R . . C43 C 0.6485(11) 0.4690(7) 0.2002(7) 0.065(3) Uani 1 1 d . . . H43 H 0.7273 0.4765 0.1710 0.078 Uiso 1 1 calc R . . C44 C 0.6105(11) 0.4020(6) 0.2550(6) 0.060(3) Uani 1 1 d . . . H44 H 0.6630 0.3555 0.2717 0.072 Uiso 1 1 calc R . . C45 C 0.4920(9) 0.4129(5) 0.2843(6) 0.049(3) Uani 1 1 d . . . H45 H 0.4458 0.3756 0.3230 0.059 Uiso 1 1 calc R . . C46 C 0.6118(9) 0.5776(5) 0.3316(5) 0.039(2) Uani 1 1 d . . . C47 C 0.7421(9) 0.5635(5) 0.3067(6) 0.048(3) Uani 1 1 d . . . H47 H 0.7912 0.5993 0.2683 0.057 Uiso 1 1 calc R . . C48 C 0.7835(11) 0.4889(6) 0.3469(6) 0.061(3) Uani 1 1 d . . . H48 H 0.8653 0.4640 0.3417 0.073 Uiso 1 1 calc R . . C49 C 0.6770(11) 0.4560(6) 0.3969(6) 0.061(3) Uani 1 1 d . . . H49 H 0.6763 0.4047 0.4313 0.073 Uiso 1 1 calc R . . C50 C 0.5746(10) 0.5104(5) 0.3859(5) 0.048(3) Uani 1 1 d . . . H50 H 0.4925 0.5030 0.4120 0.057 Uiso 1 1 calc R . . C51 C 0.5087(9) 0.7044(5) 0.3650(5) 0.039(2) Uani 1 1 d . . . C52 C 0.5483(10) 0.6670(6) 0.4344(5) 0.054(3) Uani 1 1 d . . . H52 H 0.5822 0.6181 0.4464 0.064 Uiso 1 1 calc R . . C53 C 0.5382(11) 0.7013(7) 0.4864(6) 0.066(3) Uani 1 1 d . . . H53 H 0.5652 0.6756 0.5322 0.079 Uiso 1 1 calc R . . C54 C 0.4879(10) 0.7735(8) 0.4686(7) 0.065(4) Uani 1 1 d . . . H54 H 0.4810 0.7969 0.5025 0.078 Uiso 1 1 calc R . . C55 C 0.4481(10) 0.8109(6) 0.4017(6) 0.060(3) Uani 1 1 d . . . H55 H 0.4127 0.8595 0.3900 0.072 Uiso 1 1 calc R . . C56 C 0.4604(9) 0.7767(5) 0.3515(6) 0.047(3) Uani 1 1 d . . . H56 H 0.4347 0.8039 0.3058 0.056 Uiso 1 1 calc R . . C57 C 0.6287(9) 0.7252(5) 0.2352(5) 0.040(2) Uani 1 1 d . . . C58 C 0.7086(10) 0.7704(6) 0.2538(6) 0.060(3) Uani 1 1 d . . . H58 H 0.7082 0.7672 0.3011 0.072 Uiso 1 1 calc R . . C59 C 0.7905(10) 0.8208(6) 0.2056(6) 0.061(3) Uani 1 1 d . . . H59 H 0.8392 0.8518 0.2205 0.073 Uiso 1 1 calc R . . C60 C 0.7982(11) 0.8240(7) 0.1383(7) 0.064(3) Uani 1 1 d . . . H60 H 0.8522 0.8576 0.1061 0.077 Uiso 1 1 calc R . . C61 C 0.7274(13) 0.7784(7) 0.1165(6) 0.081(4) Uani 1 1 d . . . H61 H 0.7352 0.7794 0.0699 0.097 Uiso 1 1 calc R . . C62 C 0.6429(11) 0.7298(6) 0.1644(6) 0.063(3) Uani 1 1 d . . . H62 H 0.5943 0.6995 0.1485 0.075 Uiso 1 1 calc R . . C63 C 0.2390(9) 0.4661(6) 0.3421(5) 0.045(3) Uani 1 1 d . . . C64 C 0.2311(9) 0.4779(6) 0.4074(6) 0.054(3) Uani 1 1 d . . . H64 H 0.2630 0.5214 0.4108 0.064 Uiso 1 1 calc R . . C65 C 0.1747(13) 0.4240(8) 0.4688(6) 0.084(4) Uani 1 1 d . . . H65 H 0.1663 0.4340 0.5110 0.101 Uiso 1 1 calc R . . C66 C 0.1328(13) 0.3578(7) 0.4660(8) 0.083(4) Uani 1 1 d . . . H66 H 0.0973 0.3223 0.5061 0.099 Uiso 1 1 calc R . . C67 C 0.1446(12) 0.3452(7) 0.4025(8) 0.078(4) Uani 1 1 d . . . H67 H 0.1163 0.3004 0.4001 0.094 Uiso 1 1 calc R . . C68 C 0.1984(10) 0.3982(6) 0.3405(7) 0.063(3) Uani 1 1 d . . . H68 H 0.2065 0.3874 0.2986 0.076 Uiso 1 1 calc R . . C69 C 0.1993(9) 0.5320(5) 0.1953(5) 0.041(2) Uani 1 1 d . . . C70 C 0.0679(12) 0.5517(7) 0.1998(7) 0.077(4) Uani 1 1 d . . . H70 H 0.0368 0.5630 0.2392 0.092 Uiso 1 1 calc R . . C71 C -0.0165(12) 0.5545(7) 0.1466(7) 0.076(4) Uani 1 1 d . . . H71 H -0.1020 0.5684 0.1494 0.092 Uiso 1 1 calc R . . C72 C 0.0334(15) 0.5359(7) 0.0903(7) 0.084(4) Uani 1 1 d . . . H72 H -0.0198 0.5367 0.0543 0.101 Uiso 1 1 calc R . . C73 C 0.1613(12) 0.5158(8) 0.0857(7) 0.083(4) Uani 1 1 d . . . H73 H 0.1934 0.5033 0.0471 0.099 Uiso 1 1 calc R . . C74 C 0.2377(11) 0.5145(7) 0.1375(6) 0.067(3) Uani 1 1 d . . . H74 H 0.3230 0.5007 0.1335 0.080 Uiso 1 1 calc R . . C75 C 0.0137(9) 0.6482(7) 0.3350(6) 0.062(3) Uani 1 1 d . . . H75A H -0.0428 0.6677 0.3641 0.093 Uiso 1 1 calc R . . H75B H 0.0179 0.5943 0.3546 0.093 Uiso 1 1 calc R . . H75C H -0.0175 0.6639 0.2878 0.093 Uiso 1 1 calc R . . C76 C 0.1958(11) 0.6635(6) 0.4283(5) 0.066(3) Uani 1 1 d . . . H76A H 0.1165 0.6730 0.4499 0.099 Uiso 1 1 calc R . . H76B H 0.2595 0.6947 0.4351 0.099 Uiso 1 1 calc R . . H76C H 0.2218 0.6115 0.4499 0.099 Uiso 1 1 calc R . . C77 C 0.1308(12) 0.7859(6) 0.3103(7) 0.076(4) Uani 1 1 d . . . H77A H 0.1004 0.8056 0.2628 0.114 Uiso 1 1 calc R . . H77B H 0.2038 0.8127 0.3137 0.114 Uiso 1 1 calc R . . H77C H 0.0649 0.7917 0.3430 0.114 Uiso 1 1 calc R . . C78 C 0.3389(13) 0.8306(5) 0.1347(6) 0.078(4) Uani 1 1 d . . . H78A H 0.3505 0.8546 0.0843 0.117 Uiso 1 1 calc R . . H78B H 0.4180 0.8289 0.1573 0.117 Uiso 1 1 calc R . . H78C H 0.2758 0.8586 0.1524 0.117 Uiso 1 1 calc R . . C79 C 0.3518(11) 0.7164(7) 0.0738(5) 0.066(3) Uani 1 1 d . . . H79A H 0.3150 0.6727 0.0698 0.100 Uiso 1 1 calc R . . H79B H 0.4424 0.7085 0.0771 0.100 Uiso 1 1 calc R . . H79C H 0.3323 0.7593 0.0326 0.100 Uiso 1 1 calc R . . C80 C 0.1250(12) 0.7554(8) 0.1283(7) 0.088(4) Uani 1 1 d . . . H80A H 0.1231 0.7941 0.0824 0.132 Uiso 1 1 calc R . . H80B H 0.0786 0.7728 0.1623 0.132 Uiso 1 1 calc R . . H80C H 0.0867 0.7113 0.1261 0.132 Uiso 1 1 calc R . . Co1 Co 0.08022(12) 0.14936(7) 0.19822(7) 0.0397(4) Uani 1 1 d . . . Co2 Co 0.31947(12) 0.65468(7) 0.26214(7) 0.0379(4) Uani 1 1 d . . . Fe1 Fe 0.33784(13) 0.11315(8) 0.36031(7) 0.0407(4) Uani 1 1 d . . . Fe2 Fe 0.61550(13) 0.48888(7) 0.29453(8) 0.0422(4) Uani 1 1 d . . . P1 P 0.2811(3) 0.17618(15) 0.18035(13) 0.0423(7) Uani 1 1 d . . . P2 P 0.0382(2) 0.09420(14) 0.31146(13) 0.0370(6) Uani 1 1 d . . . P3 P 0.0462(3) 0.06672(17) 0.14695(16) 0.0586(8) Uani 1 1 d . . . P4 P -0.0526(3) 0.24361(17) 0.14525(17) 0.0597(8) Uani 1 1 d . . . P5 P 0.5102(2) 0.66245(13) 0.29590(13) 0.0348(6) Uani 1 1 d . . . P6 P 0.3043(2) 0.54029(14) 0.26380(14) 0.0400(6) Uani 1 1 d . . . P7 P 0.2856(3) 0.73307(16) 0.15427(15) 0.0513(8) Uani 1 1 d . . . P8 P 0.1754(3) 0.68485(16) 0.33247(15) 0.0471(7) 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 C1 0.052(6) 0.024(5) 0.035(6) -0.007(4) 0.001(5) -0.011(5) C2 0.035(6) 0.030(5) 0.058(7) -0.014(5) 0.011(5) -0.004(5) C3 0.078(9) 0.042(6) 0.050(7) -0.006(6) -0.018(6) 0.008(6) C4 0.047(7) 0.073(8) 0.032(6) 0.000(6) -0.013(5) -0.020(6) C5 0.078(8) 0.051(7) 0.035(6) -0.014(5) -0.010(6) -0.012(6) C6 0.052(7) 0.042(6) 0.032(6) -0.003(5) 0.001(5) -0.023(5) C7 0.028(6) 0.062(7) 0.059(7) -0.016(6) -0.002(5) -0.016(5) C8 0.043(7) 0.064(8) 0.066(8) -0.012(7) -0.016(6) -0.012(6) C9 0.125(12) 0.048(7) 0.045(7) -0.018(6) -0.018(7) -0.024(8) C10 0.062(7) 0.039(6) 0.039(6) -0.010(5) -0.003(5) -0.014(5) C11 0.064(7) 0.036(6) 0.040(6) -0.003(5) -0.005(5) -0.009(5) C12 0.070(8) 0.059(8) 0.065(8) -0.012(7) -0.005(6) -0.021(7) C13 0.106(11) 0.052(8) 0.072(10) -0.011(7) 0.009(8) -0.042(8) C14 0.113(12) 0.043(7) 0.052(8) 0.004(6) 0.026(8) -0.004(8) C15 0.088(10) 0.057(8) 0.063(9) -0.010(7) -0.009(7) -0.001(7) C16 0.077(9) 0.054(7) 0.052(8) -0.004(6) 0.004(7) -0.010(6) C17 0.047(6) 0.036(6) 0.035(6) -0.012(5) -0.002(5) 0.001(5) C18 0.054(7) 0.051(7) 0.057(7) -0.030(6) 0.001(5) -0.002(6) C19 0.049(7) 0.054(7) 0.078(9) -0.024(7) 0.008(6) 0.000(6) C20 0.069(9) 0.075(9) 0.087(10) -0.060(8) -0.022(7) 0.021(7) C21 0.072(8) 0.076(9) 0.046(7) -0.020(7) 0.003(6) 0.012(7) C22 0.028(6) 0.058(7) 0.074(8) -0.028(6) 0.003(5) 0.005(5) C23 0.037(6) 0.052(7) 0.038(6) -0.017(5) 0.007(5) -0.004(5) C24 0.121(12) 0.055(8) 0.064(9) -0.014(7) 0.037(8) 0.006(8) C25 0.131(13) 0.054(8) 0.078(10) -0.020(7) 0.027(9) 0.005(8) C26 0.099(12) 0.067(10) 0.135(15) -0.036(10) 0.000(11) 0.026(9) C27 0.183(19) 0.103(13) 0.112(14) -0.010(11) 0.087(13) 0.045(13) C28 0.108(12) 0.063(8) 0.105(12) -0.015(8) 0.060(10) 0.012(8) C29 0.044(6) 0.045(6) 0.045(6) -0.024(5) 0.003(5) -0.015(5) C30 0.057(8) 0.071(8) 0.057(8) -0.010(6) -0.006(6) -0.021(7) C31 0.076(10) 0.144(15) 0.078(10) -0.049(11) -0.008(8) -0.051(11) C32 0.141(15) 0.054(9) 0.070(10) -0.029(8) 0.031(10) -0.051(10) C33 0.053(8) 0.068(8) 0.063(8) -0.027(7) 0.012(7) -0.008(7) C34 0.062(7) 0.039(6) 0.052(7) -0.013(6) 0.014(6) -0.016(6) C35 0.057(8) 0.095(10) 0.086(10) -0.006(8) -0.006(7) 0.015(7) C36 0.115(12) 0.036(7) 0.132(13) -0.009(8) 0.020(10) 0.002(7) C37 0.112(12) 0.104(11) 0.060(9) -0.004(8) -0.023(8) 0.003(9) C38 0.104(11) 0.112(11) 0.060(8) -0.048(8) 0.024(8) -0.051(9) C39 0.080(10) 0.124(12) 0.105(12) -0.062(10) 0.007(8) -0.044(9) C40 0.24(2) 0.042(8) 0.078(10) -0.031(7) 0.018(11) -0.026(10) C41 0.027(5) 0.052(6) 0.043(6) -0.027(5) 0.001(4) -0.004(5) C42 0.055(7) 0.056(7) 0.049(7) -0.028(6) 0.002(5) -0.020(6) C43 0.060(8) 0.076(9) 0.077(9) -0.051(8) -0.004(6) 0.010(7) C44 0.079(9) 0.036(6) 0.073(9) -0.027(6) -0.021(7) 0.011(6) C45 0.038(6) 0.040(6) 0.078(8) -0.032(6) 0.003(6) -0.004(5) C46 0.045(6) 0.030(5) 0.044(6) -0.015(5) -0.006(5) -0.010(5) C47 0.049(7) 0.039(6) 0.062(7) -0.025(5) -0.005(5) -0.010(5) C48 0.065(8) 0.053(7) 0.076(9) -0.037(7) -0.014(7) 0.007(6) C49 0.080(9) 0.045(7) 0.053(7) -0.009(6) -0.033(7) 0.005(6) C50 0.054(7) 0.039(6) 0.051(7) -0.016(5) -0.009(5) -0.001(5) C51 0.039(6) 0.044(6) 0.041(6) -0.021(5) 0.010(5) -0.014(5) C52 0.063(7) 0.058(7) 0.039(7) -0.016(6) 0.006(5) -0.008(6) C53 0.080(9) 0.075(9) 0.048(7) -0.028(7) -0.003(6) 0.004(7) C54 0.041(7) 0.104(11) 0.074(9) -0.060(8) 0.010(6) -0.020(7) C55 0.062(8) 0.066(8) 0.071(9) -0.049(7) -0.005(6) 0.005(6) C56 0.048(6) 0.046(6) 0.053(7) -0.026(5) -0.005(5) 0.000(5) C57 0.045(6) 0.032(5) 0.044(6) -0.015(5) 0.001(5) 0.002(5) C58 0.067(8) 0.076(8) 0.046(7) -0.031(6) 0.005(6) -0.031(7) C59 0.058(8) 0.068(8) 0.066(8) -0.033(7) 0.019(6) -0.038(6) C60 0.049(7) 0.076(9) 0.063(9) -0.021(7) 0.017(6) -0.014(6) C61 0.102(11) 0.093(10) 0.039(7) -0.013(7) 0.044(7) -0.029(9) C62 0.076(8) 0.071(8) 0.053(8) -0.033(7) 0.002(6) -0.031(7) C63 0.029(5) 0.054(7) 0.053(7) -0.019(6) 0.000(5) -0.013(5) C64 0.043(6) 0.061(7) 0.058(8) -0.021(6) 0.004(5) -0.002(6) C65 0.115(12) 0.088(10) 0.033(7) -0.004(7) 0.011(7) 0.021(9) C66 0.089(10) 0.056(9) 0.094(12) -0.013(8) 0.027(9) -0.021(8) C67 0.074(9) 0.058(8) 0.099(11) -0.019(8) 0.001(8) -0.026(7) C68 0.056(7) 0.055(7) 0.077(9) -0.018(7) -0.001(6) -0.024(6) C69 0.027(5) 0.043(6) 0.060(7) -0.024(5) 0.005(5) -0.016(5) C70 0.077(9) 0.093(10) 0.075(9) -0.046(8) -0.009(7) -0.004(8) C71 0.061(8) 0.092(10) 0.089(10) -0.044(9) -0.034(7) 0.009(7) C72 0.117(13) 0.071(9) 0.074(10) -0.029(8) -0.052(9) -0.020(9) C73 0.054(8) 0.133(13) 0.082(10) -0.062(9) -0.010(7) -0.002(8) C74 0.057(8) 0.090(9) 0.075(9) -0.054(8) -0.009(7) -0.005(7) C75 0.035(6) 0.098(9) 0.063(8) -0.041(7) 0.012(5) -0.009(6) C76 0.095(9) 0.066(8) 0.043(7) -0.028(6) 0.008(6) -0.014(7) C77 0.094(10) 0.046(7) 0.094(10) -0.034(7) -0.005(8) 0.018(7) C78 0.143(12) 0.028(6) 0.054(8) -0.005(5) 0.013(8) 0.004(7) C79 0.077(9) 0.086(9) 0.041(7) -0.029(6) 0.001(6) 0.002(7) C80 0.089(10) 0.101(11) 0.061(9) -0.015(8) -0.007(7) 0.022(8) Co1 0.0421(8) 0.0390(8) 0.0367(8) -0.0103(6) -0.0035(6) -0.0053(6) Co2 0.0382(8) 0.0395(8) 0.0378(8) -0.0157(6) 0.0003(6) -0.0026(6) Fe1 0.0426(9) 0.0424(8) 0.0375(9) -0.0133(7) -0.0051(7) -0.0055(7) Fe2 0.0425(9) 0.0359(8) 0.0513(9) -0.0188(7) -0.0027(7) -0.0015(7) P1 0.0503(17) 0.0417(15) 0.0338(15) -0.0105(12) -0.0016(12) -0.0085(13) P2 0.0358(15) 0.0365(14) 0.0376(15) -0.0111(12) 0.0001(11) -0.0057(12) P3 0.075(2) 0.0540(18) 0.0513(19) -0.0228(15) 0.0064(16) -0.0196(16) P4 0.0582(19) 0.0539(18) 0.055(2) -0.0031(15) -0.0109(15) 0.0037(16) P5 0.0393(15) 0.0331(14) 0.0341(14) -0.0136(12) 0.0004(11) -0.0070(11) P6 0.0399(15) 0.0428(15) 0.0414(16) -0.0190(13) -0.0015(12) -0.0066(12) P7 0.0631(19) 0.0470(17) 0.0409(17) -0.0124(14) -0.0026(14) 0.0048(15) P8 0.0422(16) 0.0553(18) 0.0467(17) -0.0214(14) 0.0023(13) -0.0027(14) _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 C1 C5 1.424(13) . ? C1 C2 1.422(12) . ? C1 P2 1.857(10) . ? C1 Fe1 2.035(9) . ? C2 C3 1.428(14) . ? C2 Fe1 2.036(9) . ? C2 H2 0.9800 . ? C3 C4 1.401(14) . ? C3 Fe1 2.047(10) . ? C3 H3 0.9800 . ? C4 C5 1.408(14) . ? C4 Fe1 2.046(10) . ? C4 H4 0.9800 . ? C5 Fe1 2.032(11) . ? C5 H5 0.9800 . ? C6 C7 1.388(13) . ? C6 C10 1.462(13) . ? C6 P1 1.847(10) . ? C6 Fe1 2.037(9) . ? C7 C8 1.397(14) . ? C7 Fe1 2.051(10) . ? C7 H7 0.9800 . ? C8 C9 1.413(16) . ? C8 Fe1 2.060(10) . ? C8 H8 0.9800 . ? C9 C10 1.424(14) . ? C9 Fe1 2.036(10) . ? C9 H9 0.9800 . ? C10 Fe1 2.032(10) . ? C10 H10 0.9800 . ? C11 C12 1.365(13) . ? C11 C16 1.390(14) . ? C11 P1 1.863(10) . ? C12 C13 1.386(14) . ? C12 H12 0.9300 . ? C13 C14 1.360(17) . ? C13 H13 0.9300 . ? C14 C15 1.355(16) . ? C14 H14 0.9300 . ? C15 C16 1.376(14) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 C22 1.360(13) . ? C17 C18 1.386(13) . ? C17 P2 1.851(9) . ? C18 C19 1.355(13) . ? C18 H18 0.9300 . ? C19 C20 1.317(15) . ? C19 H19 0.9300 . ? C20 C21 1.386(15) . ? C20 H20 0.9300 . ? C21 C22 1.392(14) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C28 1.314(14) . ? C23 C24 1.355(14) . ? C23 P1 1.878(10) . ? C24 C25 1.342(15) . ? C24 H24 0.9300 . ? C25 C26 1.348(17) . ? C25 H25 0.9300 . ? C26 C27 1.352(18) . ? C26 H26 0.9300 . ? C27 C28 1.407(17) . ? C27 H27 0.9300 . ? C28 H28 0.9300 . ? C29 C30 1.327(14) . ? C29 C34 1.376(13) . ? C29 P2 1.855(9) . ? C30 C31 1.393(16) . ? C30 H30 0.9300 . ? C31 C32 1.384(19) . ? C31 H31 0.9300 . ? C32 C33 1.309(18) . ? C32 H32 0.9300 . ? C33 C34 1.379(13) . ? C33 H33 0.9300 . ? C34 H34 0.9300 . ? C35 P4 1.801(11) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 P4 1.821(12) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 P4 1.853(13) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 P3 1.853(11) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 P3 1.871(12) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 P3 1.844(13) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 C42 1.396(12) . ? C41 C45 1.452(13) . ? C41 P6 1.842(9) . ? C41 Fe2 2.034(9) . ? C42 C43 1.464(14) . ? C42 Fe2 2.045(11) . ? C42 H42 0.9800 . ? C43 C44 1.425(15) . ? C43 Fe2 2.066(11) . ? C43 H43 0.9800 . ? C44 C45 1.391(14) . ? C44 Fe2 2.061(10) . ? C44 H44 0.9800 . ? C45 Fe2 2.053(9) . ? C45 H45 0.9800 . ? C46 C50 1.420(13) . ? C46 C47 1.481(13) . ? C46 P5 1.830(10) . ? C46 Fe2 2.057(9) . ? C47 C48 1.422(14) . ? C47 Fe2 2.071(9) . ? C47 H47 0.9800 . ? C48 C49 1.479(15) . ? C48 Fe2 2.098(11) . ? C48 H48 0.9800 . ? C49 C50 1.424(14) . ? C49 Fe2 2.057(11) . ? C49 H49 0.9800 . ? C50 Fe2 2.034(10) . ? C50 H50 0.9800 . ? C51 C56 1.376(13) . ? C51 C52 1.400(13) . ? C51 P5 1.821(9) . ? C52 C53 1.405(14) . ? C52 H52 0.9300 . ? C53 C54 1.374(15) . ? C53 H53 0.9300 . ? C54 C55 1.359(15) . ? C54 H54 0.9300 . ? C55 C56 1.372(13) . ? C55 H55 0.9300 . ? C56 H56 0.9300 . ? C57 C58 1.378(13) . ? C57 C62 1.395(13) . ? C57 P5 1.861(9) . ? C58 C59 1.400(13) . ? C58 H58 0.9300 . ? C59 C60 1.329(15) . ? C59 H59 0.9300 . ? C60 C61 1.360(16) . ? C60 H60 0.9300 . ? C61 C62 1.398(14) . ? C61 H61 0.9300 . ? C62 H62 0.9300 . ? C63 C68 1.388(13) . ? C63 C64 1.401(14) . ? C63 P6 1.841(10) . ? C64 C65 1.428(15) . ? C64 H64 0.9300 . ? C65 C66 1.370(17) . ? C65 H65 0.9300 . ? C66 C67 1.374(17) . ? C66 H66 0.9300 . ? C67 C68 1.417(15) . ? C67 H67 0.9300 . ? C68 H68 0.9300 . ? C69 C74 1.351(13) . ? C69 C70 1.421(14) . ? C69 P6 1.856(10) . ? C70 C71 1.405(15) . ? C70 H70 0.9300 . ? C71 C72 1.370(17) . ? C71 H71 0.9300 . ? C72 C73 1.388(17) . ? C72 H72 0.9300 . ? C73 C74 1.336(15) . ? C73 H73 0.9300 . ? C74 H74 0.9300 . ? C75 P8 1.862(10) . ? C75 H75A 0.9600 . ? C75 H75B 0.9600 . ? C75 H75C 0.9600 . ? C76 P8 1.845(10) . ? C76 H76A 0.9600 . ? C76 H76B 0.9600 . ? C76 H76C 0.9600 . ? C77 P8 1.851(10) . ? C77 H77A 0.9600 . ? C77 H77B 0.9600 . ? C77 H77C 0.9600 . ? C78 P7 1.863(10) . ? C78 H78A 0.9600 . ? C78 H78B 0.9600 . ? C78 H78C 0.9600 . ? C79 P7 1.849(10) . ? C79 H79A 0.9600 . ? C79 H79B 0.9600 . ? C79 H79C 0.9600 . ? C80 P7 1.779(12) . ? C80 H80A 0.9600 . ? C80 H80B 0.9600 . ? C80 H80C 0.9600 . ? Co1 P2 2.184(3) . ? Co1 P1 2.184(3) . ? Co1 P3 2.200(3) . ? Co1 P4 2.203(3) . ? Co2 P6 2.170(3) . ? Co2 P5 2.176(3) . ? Co2 P7 2.197(3) . ? Co2 P8 2.211(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 C5 C1 C2 106.8(9) . . ? C5 C1 P2 128.4(8) . . ? C2 C1 P2 124.7(7) . . ? C5 C1 Fe1 69.4(6) . . ? C2 C1 Fe1 69.6(5) . . ? P2 C1 Fe1 122.7(4) . . ? C1 C2 C3 108.0(9) . . ? C1 C2 Fe1 69.5(5) . . ? C3 C2 Fe1 69.9(6) . . ? C1 C2 H2 126.0 . . ? C3 C2 H2 126.0 . . ? Fe1 C2 H2 126.0 . . ? C4 C3 C2 108.1(10) . . ? C4 C3 Fe1 70.0(6) . . ? C2 C3 Fe1 69.1(5) . . ? C4 C3 H3 125.9 . . ? C2 C3 H3 125.9 . . ? Fe1 C3 H3 125.9 . . ? C3 C4 C5 108.2(9) . . ? C3 C4 Fe1 70.0(6) . . ? C5 C4 Fe1 69.2(6) . . ? C3 C4 H4 125.9 . . ? C5 C4 H4 125.9 . . ? Fe1 C4 H4 125.9 . . ? C4 C5 C1 108.8(10) . . ? C4 C5 Fe1 70.3(6) . . ? C1 C5 Fe1 69.6(6) . . ? C4 C5 H5 125.6 . . ? C1 C5 H5 125.6 . . ? Fe1 C5 H5 125.6 . . ? C7 C6 C10 107.7(9) . . ? C7 C6 P1 132.9(8) . . ? C10 C6 P1 119.4(8) . . ? C7 C6 Fe1 70.7(6) . . ? C10 C6 Fe1 68.8(5) . . ? P1 C6 Fe1 126.0(5) . . ? C6 C7 C8 110.1(10) . . ? C6 C7 Fe1 69.6(5) . . ? C8 C7 Fe1 70.5(6) . . ? C6 C7 H7 124.9 . . ? C8 C7 H7 124.9 . . ? Fe1 C7 H7 124.9 . . ? C7 C8 C9 107.4(10) . . ? C7 C8 Fe1 69.8(6) . . ? C9 C8 Fe1 68.9(6) . . ? C7 C8 H8 126.3 . . ? C9 C8 H8 126.3 . . ? Fe1 C8 H8 126.3 . . ? C8 C9 C10 109.3(10) . . ? C8 C9 Fe1 70.7(6) . . ? C10 C9 Fe1 69.3(6) . . ? C8 C9 H9 125.3 . . ? C10 C9 H9 125.3 . . ? Fe1 C9 H9 125.3 . . ? C9 C10 C6 105.5(10) . . ? C9 C10 Fe1 69.7(6) . . ? C6 C10 Fe1 69.1(5) . . ? C9 C10 H10 127.2 . . ? C6 C10 H10 127.2 . . ? Fe1 C10 H10 127.2 . . ? C12 C11 C16 117.3(10) . . ? C12 C11 P1 125.6(8) . . ? C16 C11 P1 117.1(8) . . ? C11 C12 C13 121.1(12) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C14 C13 C12 120.2(12) . . ? C14 C13 H13 119.9 . . ? C12 C13 H13 119.9 . . ? C15 C14 C13 120.0(11) . . ? C15 C14 H14 120.0 . . ? C13 C14 H14 120.0 . . ? C14 C15 C16 119.8(12) . . ? C14 C15 H15 120.1 . . ? C16 C15 H15 120.1 . . ? C15 C16 C11 121.3(12) . . ? C15 C16 H16 119.3 . . ? C11 C16 H16 119.3 . . ? C22 C17 C18 116.8(9) . . ? C22 C17 P2 123.7(7) . . ? C18 C17 P2 119.6(7) . . ? C19 C18 C17 123.4(10) . . ? C19 C18 H18 118.3 . . ? C17 C18 H18 118.3 . . ? C20 C19 C18 119.1(11) . . ? C20 C19 H19 120.5 . . ? C18 C19 H19 120.5 . . ? C19 C20 C21 121.1(11) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C20 C21 C22 119.1(11) . . ? C20 C21 H21 120.5 . . ? C22 C21 H21 120.5 . . ? C17 C22 C21 120.6(10) . . ? C17 C22 H22 119.7 . . ? C21 C22 H22 119.7 . . ? C28 C23 C24 113.4(10) . . ? C28 C23 P1 124.8(9) . . ? C24 C23 P1 121.5(8) . . ? C25 C24 C23 127.3(12) . . ? C25 C24 H24 116.3 . . ? C23 C24 H24 116.3 . . ? C24 C25 C26 117.9(13) . . ? C24 C25 H25 121.0 . . ? C26 C25 H25 121.0 . . ? C25 C26 C27 118.5(14) . . ? C25 C26 H26 120.8 . . ? C27 C26 H26 120.8 . . ? C26 C27 C28 119.8(14) . . ? C26 C27 H27 120.1 . . ? C28 C27 H27 120.1 . . ? C23 C28 C27 123.1(13) . . ? C23 C28 H28 118.5 . . ? C27 C28 H28 118.5 . . ? C30 C29 C34 118.0(10) . . ? C30 C29 P2 118.1(9) . . ? C34 C29 P2 123.6(8) . . ? C29 C30 C31 121.0(12) . . ? C29 C30 H30 119.5 . . ? C31 C30 H30 119.5 . . ? C32 C31 C30 119.0(13) . . ? C32 C31 H31 120.5 . . ? C30 C31 H31 120.5 . . ? C33 C32 C31 120.5(13) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C32 C33 C34 119.5(13) . . ? C32 C33 H33 120.2 . . ? C34 C33 H33 120.2 . . ? C29 C34 C33 121.8(11) . . ? C29 C34 H34 119.1 . . ? C33 C34 H34 119.1 . . ? P4 C35 H35A 109.5 . . ? P4 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? P4 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? P4 C36 H36A 109.5 . . ? P4 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? P4 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? P4 C37 H37A 109.5 . . ? P4 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? P4 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? P3 C38 H38A 109.5 . . ? P3 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? P3 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? P3 C39 H39A 109.5 . . ? P3 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? P3 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? P3 C40 H40A 109.5 . . ? P3 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? P3 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C45 108.1(9) . . ? C42 C41 P6 123.6(8) . . ? C45 C41 P6 128.2(7) . . ? C42 C41 Fe2 70.4(6) . . ? C45 C41 Fe2 69.9(5) . . ? P6 C41 Fe2 122.1(5) . . ? C41 C42 C43 108.8(10) . . ? C41 C42 Fe2 69.6(6) . . ? C43 C42 Fe2 69.9(6) . . ? C41 C42 H42 125.6 . . ? C43 C42 H42 125.6 . . ? Fe2 C42 H42 125.6 . . ? C44 C43 C42 105.1(10) . . ? C44 C43 Fe2 69.6(6) . . ? C42 C43 Fe2 68.4(6) . . ? C44 C43 H43 127.4 . . ? C42 C43 H43 127.4 . . ? Fe2 C43 H43 127.4 . . ? C45 C44 C43 110.9(10) . . ? C45 C44 Fe2 69.9(6) . . ? C43 C44 Fe2 70.0(6) . . ? C45 C44 H44 124.5 . . ? C43 C44 H44 124.5 . . ? Fe2 C44 H44 124.5 . . ? C44 C45 C41 107.1(9) . . ? C44 C45 Fe2 70.6(6) . . ? C41 C45 Fe2 68.5(5) . . ? C44 C45 H45 126.4 . . ? C41 C45 H45 126.4 . . ? Fe2 C45 H45 126.4 . . ? C50 C46 C47 107.3(8) . . ? C50 C46 P5 125.1(7) . . ? C47 C46 P5 127.4(7) . . ? C50 C46 Fe2 68.9(5) . . ? C47 C46 Fe2 69.5(5) . . ? P5 C46 Fe2 123.5(5) . . ? C48 C47 C46 108.9(9) . . ? C48 C47 Fe2 71.1(6) . . ? C46 C47 Fe2 68.5(5) . . ? C48 C47 H47 125.6 . . ? C46 C47 H47 125.6 . . ? Fe2 C47 H47 125.6 . . ? C47 C48 C49 106.1(10) . . ? C47 C48 Fe2 69.0(6) . . ? C49 C48 Fe2 67.7(6) . . ? C47 C48 H48 126.9 . . ? C49 C48 H48 126.9 . . ? Fe2 C48 H48 126.9 . . ? C50 C49 C48 109.0(9) . . ? C50 C49 Fe2 68.8(6) . . ? C48 C49 Fe2 70.6(6) . . ? C50 C49 H49 125.5 . . ? C48 C49 H49 125.5 . . ? Fe2 C49 H49 125.5 . . ? C46 C50 C49 108.7(9) . . ? C46 C50 Fe2 70.5(6) . . ? C49 C50 Fe2 70.5(6) . . ? C46 C50 H50 125.6 . . ? C49 C50 H50 125.6 . . ? Fe2 C50 H50 125.6 . . ? C56 C51 C52 115.5(9) . . ? C56 C51 P5 119.8(8) . . ? C52 C51 P5 124.6(8) . . ? C51 C52 C53 121.8(10) . . ? C51 C52 H52 119.1 . . ? C53 C52 H52 119.1 . . ? C54 C53 C52 119.0(11) . . ? C54 C53 H53 120.5 . . ? C52 C53 H53 120.5 . . ? C55 C54 C53 120.4(11) . . ? C55 C54 H54 119.8 . . ? C53 C54 H54 119.8 . . ? C54 C55 C56 119.7(11) . . ? C54 C55 H55 120.2 . . ? C56 C55 H55 120.2 . . ? C55 C56 C51 123.7(11) . . ? C55 C56 H56 118.2 . . ? C51 C56 H56 118.2 . . ? C58 C57 C62 114.0(9) . . ? C58 C57 P5 125.3(8) . . ? C62 C57 P5 120.7(8) . . ? C57 C58 C59 123.7(10) . . ? C57 C58 H58 118.1 . . ? C59 C58 H58 118.1 . . ? C60 C59 C58 119.7(11) . . ? C60 C59 H59 120.2 . . ? C58 C59 H59 120.2 . . ? C59 C60 C61 120.2(11) . . ? C59 C60 H60 119.9 . . ? C61 C60 H60 119.9 . . ? C60 C61 C62 119.9(11) . . ? C60 C61 H61 120.0 . . ? C62 C61 H61 120.0 . . ? C57 C62 C61 122.4(11) . . ? C57 C62 H62 118.8 . . ? C61 C62 H62 118.8 . . ? C68 C63 C64 117.6(10) . . ? C68 C63 P6 123.6(8) . . ? C64 C63 P6 118.8(8) . . ? C63 C64 C65 121.0(11) . . ? C63 C64 H64 119.5 . . ? C65 C64 H64 119.5 . . ? C66 C65 C64 120.6(12) . . ? C66 C65 H65 119.7 . . ? C64 C65 H65 119.7 . . ? C65 C66 C67 118.3(12) . . ? C65 C66 H66 120.8 . . ? C67 C66 H66 120.8 . . ? C66 C67 C68 122.2(12) . . ? C66 C67 H67 118.9 . . ? C68 C67 H67 118.9 . . ? C63 C68 C67 120.2(12) . . ? C63 C68 H68 119.9 . . ? C67 C68 H68 119.9 . . ? C74 C69 C70 116.0(10) . . ? C74 C69 P6 125.8(8) . . ? C70 C69 P6 117.9(8) . . ? C71 C70 C69 122.1(12) . . ? C71 C70 H70 119.0 . . ? C69 C70 H70 119.0 . . ? C72 C71 C70 116.7(12) . . ? C72 C71 H71 121.6 . . ? C70 C71 H71 121.6 . . ? C71 C72 C73 121.7(12) . . ? C71 C72 H72 119.1 . . ? C73 C72 H72 119.1 . . ? C74 C73 C72 119.1(12) . . ? C74 C73 H73 120.4 . . ? C72 C73 H73 120.4 . . ? C73 C74 C69 124.3(12) . . ? C73 C74 H74 117.8 . . ? C69 C74 H74 117.8 . . ? P8 C75 H75A 109.5 . . ? P8 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? P8 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? P8 C76 H76A 109.5 . . ? P8 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? P8 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? P8 C77 H77A 109.5 . . ? P8 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? P8 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? P7 C78 H78A 109.5 . . ? P7 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? P7 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? P7 C79 H79A 109.5 . . ? P7 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? P7 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? P7 C80 H80A 109.5 . . ? P7 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? P7 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? P2 Co1 P1 110.19(11) . . ? P2 Co1 P3 106.47(12) . . ? P1 Co1 P3 107.43(12) . . ? P2 Co1 P4 114.25(12) . . ? P1 Co1 P4 114.58(12) . . ? P3 Co1 P4 103.12(14) . . ? P6 Co2 P5 106.51(11) . . ? P6 Co2 P7 109.09(12) . . ? P5 Co2 P7 112.05(11) . . ? P6 Co2 P8 112.68(11) . . ? P5 Co2 P8 110.28(11) . . ? P7 Co2 P8 106.32(12) . . ? C10 Fe1 C5 110.2(4) . . ? C10 Fe1 C2 138.6(4) . . ? C5 Fe1 C2 68.4(4) . . ? C10 Fe1 C9 41.0(4) . . ? C5 Fe1 C9 111.0(5) . . ? C2 Fe1 C9 179.2(5) . . ? C10 Fe1 C6 42.1(4) . . ? C5 Fe1 C6 140.1(4) . . ? C2 Fe1 C6 111.4(4) . . ? C9 Fe1 C6 68.7(4) . . ? C10 Fe1 C1 109.7(4) . . ? C5 Fe1 C1 41.0(4) . . ? C2 Fe1 C1 40.9(3) . . ? C9 Fe1 C1 138.3(5) . . ? C6 Fe1 C1 111.4(4) . . ? C10 Fe1 C4 138.5(5) . . ? C5 Fe1 C4 40.4(4) . . ? C2 Fe1 C4 68.3(4) . . ? C9 Fe1 C4 111.6(5) . . ? C6 Fe1 C4 179.4(5) . . ? C1 Fe1 C4 68.7(4) . . ? C10 Fe1 C3 178.0(5) . . ? C5 Fe1 C3 67.8(5) . . ? C2 Fe1 C3 41.0(4) . . ? C9 Fe1 C3 139.4(5) . . ? C6 Fe1 C3 139.4(4) . . ? C1 Fe1 C3 68.8(4) . . ? C4 Fe1 C3 40.0(4) . . ? C10 Fe1 C7 68.6(4) . . ? C5 Fe1 C7 178.4(4) . . ? C2 Fe1 C7 113.3(4) . . ? C9 Fe1 C7 67.3(5) . . ? C6 Fe1 C7 39.7(4) . . ? C1 Fe1 C7 140.3(4) . . ? C4 Fe1 C7 139.8(4) . . ? C3 Fe1 C7 113.3(5) . . ? C10 Fe1 C8 68.9(4) . . ? C5 Fe1 C8 138.9(4) . . ? C2 Fe1 C8 140.4(4) . . ? C9 Fe1 C8 40.4(4) . . ? C6 Fe1 C8 67.8(4) . . ? C1 Fe1 C8 178.5(4) . . ? C4 Fe1 C8 112.1(4) . . ? C3 Fe1 C8 112.6(5) . . ? C7 Fe1 C8 39.7(4) . . ? C41 Fe2 C50 108.2(4) . . ? C41 Fe2 C42 40.0(3) . . ? C50 Fe2 C42 135.7(4) . . ? C41 Fe2 C45 41.6(4) . . ? C50 Fe2 C45 110.2(4) . . ? C42 Fe2 C45 68.5(4) . . ? C41 Fe2 C46 109.2(4) . . ? C50 Fe2 C46 40.6(4) . . ? C42 Fe2 C46 109.8(4) . . ? C45 Fe2 C46 138.4(4) . . ? C41 Fe2 C49 136.7(4) . . ? C50 Fe2 C49 40.7(4) . . ? C42 Fe2 C49 176.1(5) . . ? C45 Fe2 C49 110.5(5) . . ? C46 Fe2 C49 68.3(4) . . ? C41 Fe2 C44 67.9(4) . . ? C50 Fe2 C44 139.9(4) . . ? C42 Fe2 C44 67.9(4) . . ? C45 Fe2 C44 39.5(4) . . ? C46 Fe2 C44 177.1(4) . . ? C49 Fe2 C44 113.8(4) . . ? C41 Fe2 C43 69.1(4) . . ? C50 Fe2 C43 177.3(4) . . ? C42 Fe2 C43 41.7(4) . . ? C45 Fe2 C43 68.5(4) . . ? C46 Fe2 C43 138.9(4) . . ? C49 Fe2 C43 141.8(5) . . ? C44 Fe2 C43 40.4(4) . . ? C41 Fe2 C47 139.7(4) . . ? C50 Fe2 C47 69.4(4) . . ? C42 Fe2 C47 112.8(4) . . ? C45 Fe2 C47 178.6(4) . . ? C46 Fe2 C47 42.0(4) . . ? C49 Fe2 C47 68.3(4) . . ? C44 Fe2 C47 140.1(4) . . ? C43 Fe2 C47 112.0(4) . . ? C41 Fe2 C48 178.0(4) . . ? C50 Fe2 C48 69.7(4) . . ? C42 Fe2 C48 141.5(4) . . ? C45 Fe2 C48 138.8(4) . . ? C46 Fe2 C48 69.3(4) . . ? C49 Fe2 C48 41.7(4) . . ? C44 Fe2 C48 113.6(4) . . ? C43 Fe2 C48 112.9(5) . . ? C47 Fe2 C48 39.9(4) . . ? C6 P1 C11 97.8(4) . . ? C6 P1 C23 98.6(5) . . ? C11 P1 C23 97.5(5) . . ? C6 P1 Co1 116.9(3) . . ? C11 P1 Co1 121.3(4) . . ? C23 P1 Co1 120.1(3) . . ? C17 P2 C29 96.9(4) . . ? C17 P2 C1 97.5(4) . . ? C29 P2 C1 100.3(4) . . ? C17 P2 Co1 117.8(3) . . ? C29 P2 Co1 119.6(3) . . ? C1 P2 Co1 120.1(3) . . ? C40 P3 C38 97.7(6) . . ? C40 P3 C39 99.1(7) . . ? C38 P3 C39 100.7(6) . . ? C40 P3 Co1 119.6(5) . . ? C38 P3 Co1 116.9(4) . . ? C39 P3 Co1 118.8(5) . . ? C35 P4 C36 99.3(6) . . ? C35 P4 C37 95.7(6) . . ? C36 P4 C37 97.9(7) . . ? C35 P4 Co1 117.6(4) . . ? C36 P4 Co1 122.0(5) . . ? C37 P4 Co1 119.2(5) . . ? C51 P5 C46 103.2(5) . . ? C51 P5 C57 96.8(4) . . ? C46 P5 C57 99.1(4) . . ? C51 P5 Co2 112.1(3) . . ? C46 P5 Co2 120.2(3) . . ? C57 P5 Co2 121.6(3) . . ? C41 P6 C63 99.4(4) . . ? C41 P6 C69 100.5(4) . . ? C63 P6 C69 99.3(4) . . ? C41 P6 Co2 118.6(3) . . ? C63 P6 Co2 121.6(3) . . ? C69 P6 Co2 113.8(3) . . ? C80 P7 C79 98.7(6) . . ? C80 P7 C78 98.3(6) . . ? C79 P7 C78 99.1(5) . . ? C80 P7 Co2 117.8(4) . . ? C79 P7 Co2 122.9(4) . . ? C78 P7 Co2 115.7(4) . . ? C76 P8 C77 97.0(5) . . ? C76 P8 C75 99.6(5) . . ? C77 P8 C75 98.7(6) . . ? C76 P8 Co2 123.6(4) . . ? C77 P8 Co2 117.1(4) . . ? C75 P8 Co2 116.2(3) . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.567 _refine_diff_density_min -0.589 _refine_diff_density_rms 0.152