# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Hongjian Sun ' _publ_contact_author_email hjsun@sdu.edu.cn _publ_author_name 'Hongjian Sun' data_test _database_code_depnum_ccdc_archive 'CCDC 806080' #TrackingRef '- 6.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H26 Cl1 N1 Ni1 O1 P2' _chemical_formula_sum 'C14 H26 Cl1 N1 Ni1 O1 P2' _chemical_formula_weight 380.44 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 13.607(2) _cell_length_b 24.405(4) _cell_length_c 16.845(3) _cell_angle_alpha 90.00 _cell_angle_beta 91.232(3) _cell_angle_gamma 90.00 _cell_volume 5592.9(16) _cell_formula_units_Z 12 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 3677 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 23.96 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.355 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2400 _exptl_absorpt_coefficient_mu 1.351 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.850 _exptl_absorpt_correction_T_max 0.8747 _exptl_absorpt_process_details '(SADABS; Bruker, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(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 26057 _diffrn_reflns_av_R_equivalents 0.0633 _diffrn_reflns_av_sigmaI/netI 0.0749 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 24.45 _reflns_number_total 9255 _reflns_number_gt 6111 _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^)+(0.0888P)^2^+9.1503P] 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 9203 _refine_ls_number_parameters 541 _refine_ls_number_restraints 252 _refine_ls_R_factor_all 0.0990 _refine_ls_R_factor_gt 0.0628 _refine_ls_wR_factor_ref 0.1807 _refine_ls_wR_factor_gt 0.1583 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.020 _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 P2 P 0.58445(12) 0.26029(7) 0.36517(11) 0.0371(4) Uani 1 1 d . . . P4 P 0.89257(13) 0.91095(8) 0.36205(11) 0.0440(5) Uani 1 1 d . . . C32 C 0.9743(5) 0.9155(3) 0.4480(5) 0.055(2) Uani 1 1 d U . . H32A H 0.9546 0.8893 0.4872 0.082 Uiso 1 1 calc R . . H32B H 0.9713 0.9517 0.4699 0.082 Uiso 1 1 calc R . . H32C H 1.0404 0.9077 0.4325 0.082 Uiso 1 1 calc R . . C31 C 0.5024(6) 0.2428(4) 0.4431(5) 0.072(3) Uani 1 1 d U . . H31A H 0.5152 0.2060 0.4604 0.108 Uiso 1 1 calc R . . H31B H 0.4357 0.2456 0.4237 0.108 Uiso 1 1 calc R . . H31C H 0.5123 0.2676 0.4869 0.108 Uiso 1 1 calc R . . C30 C 0.5466(5) 0.3307(3) 0.3430(5) 0.0505(19) Uani 1 1 d U . . H30A H 0.5860 0.3450 0.3011 0.076 Uiso 1 1 calc R . . H30B H 0.5555 0.3529 0.3896 0.076 Uiso 1 1 calc R . . H30C H 0.4787 0.3311 0.3265 0.076 Uiso 1 1 calc R . . C36 C 0.9784(6) 0.8934(3) 1.0024(4) 0.059(2) Uani 1 1 d U . . H36A H 0.9438 0.8628 1.0244 0.089 Uiso 1 1 calc R . . H36B H 0.9681 0.9253 1.0344 0.089 Uiso 1 1 calc R . . H36C H 1.0473 0.8852 1.0014 0.089 Uiso 1 1 calc R . . C35 C 0.5804(6) 1.0111(3) 0.8760(5) 0.067(2) Uani 1 1 d U . . H35A H 0.6171 1.0329 0.8395 0.100 Uiso 1 1 calc R . . H35B H 0.5926 1.0240 0.9291 0.100 Uiso 1 1 calc R . . H35C H 0.5115 1.0141 0.8631 0.100 Uiso 1 1 calc R . . C33 C 0.5414(6) 0.9054(4) 0.9391(6) 0.083(3) Uani 1 1 d U . . H33A H 0.5566 0.8670 0.9391 0.125 Uiso 1 1 calc R . . H33B H 0.4735 0.9105 0.9244 0.125 Uiso 1 1 calc R . . H33C H 0.5535 0.9202 0.9913 0.125 Uiso 1 1 calc R . . C34 C 0.5607(6) 0.9216(4) 0.7742(5) 0.074(3) Uani 1 1 d U . . H34A H 0.5958 0.9385 0.7318 0.111 Uiso 1 1 calc R . . H34B H 0.4937 0.9339 0.7727 0.111 Uiso 1 1 calc R . . H34C H 0.5624 0.8825 0.7681 0.111 Uiso 1 1 calc R . . C38 C 1.0051(6) 0.9640(4) 0.8691(6) 0.087(3) Uani 1 1 d U . . H38A H 0.9828 0.9967 0.8948 0.131 Uiso 1 1 calc R . . H38B H 0.9978 0.9681 0.8126 0.131 Uiso 1 1 calc R . . H38C H 1.0730 0.9578 0.8829 0.131 Uiso 1 1 calc R . . C37 C 0.9856(6) 0.8486(4) 0.8476(5) 0.081(3) Uani 1 1 d U . . H37A H 0.9512 0.8156 0.8606 0.122 Uiso 1 1 calc R . . H37B H 1.0538 0.8449 0.8624 0.122 Uiso 1 1 calc R . . H37C H 0.9796 0.8552 0.7915 0.122 Uiso 1 1 calc R . . C39 C 0.7913(6) 0.9767(3) 0.5825(4) 0.0461(18) Uani 1 1 d U . . H39A H 0.7850 0.9711 0.5262 0.069 Uiso 1 1 calc R . . H39B H 0.8542 0.9927 0.5950 0.069 Uiso 1 1 calc R . . H39C H 0.7401 1.0008 0.5996 0.069 Uiso 1 1 calc R . . Ni1 Ni 0.74140(5) 0.24063(3) 0.38338(4) 0.0268(2) Uani 1 1 d . . . Ni2 Ni 0.73451(6) 0.90819(3) 0.38446(4) 0.0282(2) Uani 1 1 d . . . Ni3 Ni 0.77549(6) 0.92504(3) 0.88679(4) 0.0277(2) Uani 1 1 d . . . Cl1 Cl 0.71089(12) 0.17157(6) 0.46853(9) 0.0340(4) Uani 1 1 d . . . Cl2 Cl 0.75867(13) 0.83849(6) 0.47078(9) 0.0403(4) Uani 1 1 d . . . Cl3 Cl 0.79152(14) 0.99357(6) 0.97576(9) 0.0419(4) Uani 1 1 d . . . P5 P 0.93256(13) 0.90619(8) 0.90140(11) 0.0427(5) Uani 1 1 d . . . P1 P 0.89906(12) 0.22268(7) 0.39220(10) 0.0342(4) Uani 1 1 d . . . P3 P 0.57626(13) 0.90370(7) 0.40204(10) 0.0366(4) Uani 1 1 d . . . P6 P 0.61787(13) 0.94037(7) 0.86875(11) 0.0374(4) Uani 1 1 d . . . O1 O 0.7638(4) 0.20149(17) 0.2358(3) 0.0453(12) Uani 1 1 d . . . O3 O 0.8051(4) 0.96211(18) 0.7426(3) 0.0456(12) Uani 1 1 d . . . N3 N 0.7830(4) 0.9247(2) 0.6227(3) 0.0385(13) Uani 1 1 d . . . H23 H 0.7742 0.8954 0.5950 0.046 Uiso 1 1 calc R . . N2 N 0.7326(4) 0.9081(2) 0.1206(3) 0.0390(14) Uani 1 1 d . . . H12 H 0.7428 0.9378 0.0945 0.047 Uiso 1 1 calc R . . C29 C 0.7885(4) 0.9209(2) 0.7018(4) 0.0303(14) Uani 1 1 d U . . O2 O 0.6957(3) 0.86946(16) 0.2367(2) 0.0383(11) Uani 1 1 d . . . C13 C 0.7113(4) 0.9669(2) 0.2358(3) 0.0260(13) Uani 1 1 d U . . C7 C 0.7555(4) 0.2438(3) 0.1975(4) 0.0318(14) Uani 1 1 d U . . C12 C 0.7170(4) 0.9703(2) 0.3191(3) 0.0260(13) Uani 1 1 d U . . C18 C 0.7115(4) 0.9112(2) 0.1985(4) 0.0298(14) Uani 1 1 d U . . C1 C 0.7683(4) 0.3017(2) 0.3190(4) 0.0280(14) Uani 1 1 d U . . C28 C 0.7718(4) 0.8661(2) 0.7382(3) 0.0283(14) Uani 1 1 d U . . C24 C 0.7428(4) 0.8111(2) 0.8537(4) 0.0354(15) Uani 1 1 d U . . H24 H 0.7350 0.8081 0.9082 0.042 Uiso 1 1 calc R . . N1 N 0.7338(4) 0.2423(2) 0.1191(3) 0.0393(14) Uani 1 1 d . . . H1 H 0.7270 0.2726 0.0934 0.047 Uiso 1 1 calc R . . C23 C 0.7620(4) 0.8630(2) 0.8216(3) 0.0277(13) Uani 1 1 d U . . C2 C 0.7847(4) 0.3534(2) 0.3540(4) 0.0321(14) Uani 1 1 d U . . H2 H 0.7866 0.3562 0.4091 0.038 Uiso 1 1 calc R . . C17 C 0.7161(5) 1.0231(3) 0.3524(4) 0.0370(15) Uani 1 1 d U . . H17 H 0.7181 1.0268 0.4074 0.044 Uiso 1 1 calc R . . C16 C 0.7122(5) 1.0697(3) 0.3057(4) 0.0401(16) Uani 1 1 d U . . H16 H 0.7117 1.1041 0.3296 0.048 Uiso 1 1 calc R . . C27 C 0.7643(4) 0.8177(2) 0.6917(4) 0.0338(15) Uani 1 1 d U . . H27 H 0.7717 0.8198 0.6370 0.041 Uiso 1 1 calc R . . C6 C 0.7680(4) 0.2990(2) 0.2355(4) 0.0294(14) Uani 1 1 d U . . C14 C 0.7080(4) 1.0146(2) 0.1892(4) 0.0315(14) Uani 1 1 d U . . H14 H 0.7052 1.0117 0.1342 0.038 Uiso 1 1 calc R . . C15 C 0.7089(4) 1.0655(2) 0.2241(4) 0.0355(15) Uani 1 1 d U . . H15 H 0.7073 1.0969 0.1929 0.043 Uiso 1 1 calc R . . C25 C 0.7348(5) 0.7640(3) 0.8080(4) 0.0372(16) Uani 1 1 d U . . H25 H 0.7219 0.7303 0.8316 0.045 Uiso 1 1 calc R . . C4 C 0.7939(5) 0.3971(3) 0.2268(4) 0.0371(16) Uani 1 1 d U . . H4 H 0.8011 0.4286 0.1962 0.045 Uiso 1 1 calc R . . C5 C 0.7790(5) 0.3468(3) 0.1901(4) 0.0356(15) Uani 1 1 d U . . H5 H 0.7763 0.3447 0.1350 0.043 Uiso 1 1 calc R . . C8 C 0.7216(6) 0.1911(3) 0.0773(4) 0.0458(18) Uani 1 1 d U . . H8A H 0.7062 0.1982 0.0224 0.069 Uiso 1 1 calc R . . H8B H 0.6692 0.1706 0.1002 0.069 Uiso 1 1 calc R . . H8C H 0.7815 0.1704 0.0814 0.069 Uiso 1 1 calc R . . C26 C 0.7464(5) 0.7677(2) 0.7266(4) 0.0375(16) Uani 1 1 d U . . H26 H 0.7419 0.7364 0.6954 0.045 Uiso 1 1 calc R . . C19 C 0.7384(6) 0.8564(3) 0.0804(4) 0.0477(18) Uani 1 1 d U . . H19A H 0.7541 0.8623 0.0258 0.072 Uiso 1 1 calc R . . H19B H 0.6764 0.8378 0.0833 0.072 Uiso 1 1 calc R . . H19C H 0.7887 0.8343 0.1053 0.072 Uiso 1 1 calc R . . C3 C 0.7982(5) 0.4007(2) 0.3084(4) 0.0362(15) Uani 1 1 d U . . H3 H 0.8099 0.4342 0.3330 0.043 Uiso 1 1 calc R . . C11 C 0.9277(5) 0.1518(3) 0.3683(4) 0.0429(17) Uani 1 1 d U . . H11A H 0.8861 0.1278 0.3978 0.064 Uiso 1 1 calc R . . H11B H 0.9952 0.1444 0.3821 0.064 Uiso 1 1 calc R . . H11C H 0.9168 0.1458 0.3125 0.064 Uiso 1 1 calc R . . C21 C 0.5284(5) 0.8360(3) 0.3781(4) 0.0504(19) Uani 1 1 d U . . H21A H 0.5450 0.8268 0.3246 0.076 Uiso 1 1 calc R . . H21B H 0.4583 0.8360 0.3829 0.076 Uiso 1 1 calc R . . H21C H 0.5568 0.8096 0.4140 0.076 Uiso 1 1 calc R . . C22 C 0.5396(6) 0.9161(3) 0.5042(4) 0.057(2) Uani 1 1 d U . . H22A H 0.5626 0.9515 0.5210 0.085 Uiso 1 1 calc R . . H22B H 0.5676 0.8884 0.5382 0.085 Uiso 1 1 calc R . . H22C H 0.4692 0.9148 0.5069 0.085 Uiso 1 1 calc R . . C9 C 0.9516(5) 0.2319(3) 0.4913(4) 0.055(2) Uani 1 1 d U . . H9A H 0.9400 0.2687 0.5088 0.082 Uiso 1 1 calc R . . H9B H 1.0210 0.2251 0.4905 0.082 Uiso 1 1 calc R . . H9C H 0.9214 0.2066 0.5271 0.082 Uiso 1 1 calc R . . C10 C 0.9842(5) 0.2606(3) 0.3313(5) 0.055(2) Uani 1 1 d U . . H10A H 0.9753 0.2991 0.3396 0.083 Uiso 1 1 calc R . . H10B H 0.9718 0.2520 0.2764 0.083 Uiso 1 1 calc R . . H10C H 1.0504 0.2505 0.3458 0.083 Uiso 1 1 calc R . . C20 C 0.4929(5) 0.9484(3) 0.3446(5) 0.058(2) Uani 1 1 d U . . H20A H 0.5116 0.9860 0.3527 0.088 Uiso 1 1 calc R . . H20B H 0.4267 0.9431 0.3618 0.088 Uiso 1 1 calc R . . H20C H 0.4966 0.9396 0.2892 0.088 Uiso 1 1 calc R . . C40 C 0.5345(6) 0.2221(4) 0.2799(5) 0.076(3) Uani 1 1 d U . . H40A H 0.5741 0.2289 0.2344 0.115 Uiso 1 1 calc R . . H40B H 0.4683 0.2338 0.2687 0.115 Uiso 1 1 calc R . . H40C H 0.5349 0.1837 0.2917 0.115 Uiso 1 1 calc R . . C42 C 0.9314(7) 0.8463(4) 0.3186(6) 0.096(3) Uani 1 1 d U . . H42A H 0.9072 0.8164 0.3497 0.144 Uiso 1 1 calc R . . H42B H 1.0019 0.8449 0.3181 0.144 Uiso 1 1 calc R . . H42C H 0.9056 0.8436 0.2653 0.144 Uiso 1 1 calc R . . C41 C 0.9428(7) 0.9607(5) 0.2983(6) 0.102(4) Uani 1 1 d U . . H41A H 0.9046 0.9622 0.2498 0.154 Uiso 1 1 calc R . . H41B H 1.0094 0.9510 0.2868 0.154 Uiso 1 1 calc R . . H41C H 0.9417 0.9959 0.3237 0.154 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 P2 0.0362(9) 0.0300(10) 0.0452(11) 0.0086(8) 0.0029(8) -0.0008(7) P4 0.0373(10) 0.0610(13) 0.0337(10) 0.0042(9) -0.0008(8) 0.0062(9) C32 0.056(4) 0.051(4) 0.057(5) 0.009(4) -0.008(4) -0.007(4) C31 0.062(5) 0.080(6) 0.074(5) 0.027(5) 0.021(4) 0.015(4) C30 0.049(4) 0.046(4) 0.057(4) 0.009(3) 0.005(3) 0.009(3) C36 0.071(5) 0.058(5) 0.048(4) 0.006(4) -0.014(4) 0.011(4) C35 0.065(5) 0.043(4) 0.093(6) -0.012(4) -0.006(4) 0.010(4) C33 0.068(5) 0.085(6) 0.099(6) 0.041(5) 0.021(5) 0.001(4) C34 0.058(5) 0.089(6) 0.075(5) -0.031(5) -0.016(4) 0.017(4) C38 0.066(5) 0.098(6) 0.098(6) 0.041(5) -0.005(5) -0.034(5) C37 0.062(5) 0.104(6) 0.078(6) -0.027(5) -0.011(4) 0.033(5) C39 0.076(5) 0.031(4) 0.032(4) 0.000(3) 0.000(3) -0.003(3) Ni1 0.0371(4) 0.0205(4) 0.0227(4) 0.0030(3) 0.0002(3) -0.0013(3) Ni2 0.0403(5) 0.0213(4) 0.0229(4) 0.0013(3) 0.0013(3) 0.0001(3) Ni3 0.0380(4) 0.0211(4) 0.0240(4) -0.0019(3) 0.0006(3) -0.0032(3) Cl1 0.0530(10) 0.0233(8) 0.0257(8) 0.0033(6) 0.0024(7) -0.0037(7) Cl2 0.0690(11) 0.0237(8) 0.0279(9) 0.0010(6) -0.0043(8) 0.0008(8) Cl3 0.0739(12) 0.0247(8) 0.0269(9) -0.0018(7) -0.0022(8) -0.0088(8) P5 0.0358(10) 0.0570(13) 0.0350(10) 0.0010(9) -0.0030(8) -0.0039(8) P1 0.0381(9) 0.0257(9) 0.0388(10) 0.0074(8) 0.0008(8) 0.0010(7) P3 0.0394(10) 0.0358(10) 0.0348(10) 0.0030(8) 0.0057(8) -0.0039(8) P6 0.0377(10) 0.0299(10) 0.0446(11) -0.0002(8) 0.0051(8) 0.0011(7) O1 0.083(4) 0.016(2) 0.036(3) 0.005(2) -0.012(2) -0.001(2) O3 0.078(3) 0.026(3) 0.032(3) -0.006(2) -0.004(2) -0.007(2) N3 0.067(4) 0.017(3) 0.031(3) -0.001(2) -0.003(3) -0.008(3) N2 0.068(4) 0.023(3) 0.027(3) 0.000(2) 0.007(3) -0.009(3) C29 0.043(4) 0.023(3) 0.025(3) -0.002(3) -0.003(3) 0.003(3) O2 0.069(3) 0.018(2) 0.029(2) 0.0016(19) 0.008(2) -0.004(2) C13 0.032(3) 0.018(3) 0.028(3) 0.004(3) 0.002(3) 0.001(2) C7 0.040(4) 0.029(4) 0.026(4) 0.003(3) 0.006(3) -0.004(3) C12 0.029(3) 0.017(3) 0.032(3) 0.002(3) 0.001(3) 0.000(2) C18 0.032(3) 0.025(3) 0.032(4) 0.003(3) 0.000(3) -0.004(3) C1 0.027(3) 0.025(3) 0.032(4) 0.003(3) -0.004(3) -0.001(3) C28 0.029(3) 0.026(3) 0.030(3) -0.006(3) -0.003(3) 0.000(3) C24 0.048(4) 0.029(4) 0.029(4) 0.005(3) 0.003(3) 0.001(3) N1 0.069(4) 0.022(3) 0.027(3) 0.003(2) -0.005(3) 0.000(3) C23 0.032(3) 0.024(3) 0.027(3) -0.004(3) -0.003(3) 0.003(3) C2 0.040(4) 0.023(3) 0.033(4) -0.001(3) -0.007(3) 0.001(3) C17 0.049(4) 0.030(4) 0.031(4) -0.001(3) 0.001(3) -0.001(3) C16 0.049(4) 0.029(4) 0.043(4) -0.007(3) -0.006(3) -0.003(3) C27 0.046(4) 0.031(4) 0.025(3) -0.006(3) -0.001(3) 0.004(3) C6 0.027(3) 0.027(3) 0.034(4) 0.001(3) 0.000(3) 0.002(3) C14 0.035(3) 0.029(4) 0.031(3) 0.004(3) -0.004(3) -0.001(3) C15 0.043(4) 0.018(3) 0.045(4) 0.007(3) 0.000(3) -0.001(3) C25 0.049(4) 0.022(3) 0.040(4) 0.001(3) 0.001(3) -0.001(3) C4 0.043(4) 0.024(3) 0.045(4) 0.010(3) 0.001(3) 0.000(3) C5 0.049(4) 0.028(4) 0.029(4) 0.008(3) -0.001(3) -0.001(3) C8 0.077(5) 0.024(3) 0.036(4) -0.004(3) -0.006(3) 0.000(3) C26 0.055(4) 0.016(3) 0.042(4) -0.004(3) -0.002(3) 0.002(3) C19 0.073(5) 0.032(4) 0.039(4) -0.001(3) 0.012(3) -0.006(3) C3 0.040(4) 0.021(3) 0.048(4) -0.001(3) 0.000(3) -0.005(3) C11 0.046(4) 0.035(4) 0.047(4) 0.002(3) 0.002(3) 0.011(3) C21 0.056(4) 0.051(4) 0.045(4) -0.004(3) 0.004(3) -0.021(3) C22 0.063(5) 0.063(5) 0.045(4) -0.005(4) 0.014(4) -0.003(4) C9 0.049(4) 0.062(5) 0.053(4) 0.000(4) -0.009(3) -0.006(4) C10 0.046(4) 0.047(4) 0.072(5) 0.022(4) 0.008(4) 0.004(3) C20 0.048(4) 0.058(5) 0.069(5) 0.016(4) 0.001(4) 0.006(4) C40 0.054(5) 0.080(6) 0.094(6) -0.023(5) -0.022(4) -0.006(4) C42 0.071(5) 0.116(7) 0.101(7) -0.053(6) 0.003(5) 0.010(5) C41 0.059(5) 0.131(7) 0.118(7) 0.068(6) 0.009(5) -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 P2 C31 1.793(7) . ? P2 C30 1.830(7) . ? P2 C40 1.831(8) . ? P2 Ni1 2.2040(19) . ? P4 C41 1.768(9) . ? P4 C32 1.810(7) . ? P4 C42 1.822(9) . ? P4 Ni2 2.193(2) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C36 P5 1.826(7) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C35 P6 1.805(7) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C33 P6 1.808(8) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 P6 1.816(8) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C38 P5 1.812(8) . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C37 P5 1.829(8) . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C39 N3 1.442(8) . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? Ni1 C1 1.882(6) . ? Ni1 P1 2.1915(18) . ? Ni1 Cl1 2.2574(16) . ? Ni2 C12 1.885(6) . ? Ni2 P3 2.1827(19) . ? Ni2 Cl2 2.2573(17) . ? Ni3 C23 1.877(6) . ? Ni3 P6 2.1920(19) . ? Ni3 P5 2.195(2) . ? Ni3 Cl3 2.2533(17) . ? P1 C9 1.816(7) . ? P1 C10 1.817(7) . ? P1 C11 1.820(7) . ? P3 C21 1.817(7) . ? P3 C22 1.827(7) . ? P3 C20 1.836(7) . ? O1 C7 1.222(7) . ? O3 C29 1.235(7) . ? N3 C29 1.337(8) . ? N3 H23 0.8600 . ? N2 C18 1.352(8) . ? N2 C19 1.437(8) . ? N2 H12 0.8600 . ? C29 C28 1.492(8) . ? O2 C18 1.226(7) . ? C13 C14 1.404(8) . ? C13 C12 1.407(8) . ? C13 C18 1.498(8) . ? C7 N1 1.349(8) . ? C7 C6 1.499(8) . ? C12 C17 1.405(8) . ? C1 C2 1.409(8) . ? C1 C6 1.409(8) . ? C28 C23 1.416(8) . ? C28 C27 1.420(8) . ? C24 C25 1.386(9) . ? C24 C23 1.405(8) . ? C24 H24 0.9300 . ? N1 C8 1.442(8) . ? N1 H1 0.8600 . ? C2 C3 1.401(8) . ? C2 H2 0.9300 . ? C17 C16 1.383(9) . ? C17 H17 0.9300 . ? C16 C15 1.378(9) . ? C16 H16 0.9300 . ? C27 C26 1.379(8) . ? C27 H27 0.9300 . ? C6 C5 1.404(8) . ? C14 C15 1.375(8) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C25 C26 1.386(9) . ? C25 H25 0.9300 . ? C4 C3 1.377(9) . ? C4 C5 1.388(9) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C26 H26 0.9300 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C3 H3 0.9300 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 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 C31 P2 C30 101.3(4) . . ? C31 P2 C40 103.1(4) . . ? C30 P2 C40 102.7(4) . . ? C31 P2 Ni1 117.6(3) . . ? C30 P2 Ni1 120.0(2) . . ? C40 P2 Ni1 109.9(3) . . ? C41 P4 C32 101.8(4) . . ? C41 P4 C42 103.4(5) . . ? C32 P4 C42 101.3(4) . . ? C41 P4 Ni2 121.3(3) . . ? C32 P4 Ni2 116.9(3) . . ? C42 P4 Ni2 109.7(3) . . ? P4 C32 H32A 109.5 . . ? P4 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? P4 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? P2 C31 H31A 109.5 . . ? P2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? P2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? P2 C30 H30A 109.5 . . ? P2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? P2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 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 . . ? P6 C35 H35A 109.5 . . ? P6 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? P6 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 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 . . ? P5 C38 H38A 109.5 . . ? P5 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? P5 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 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 . . ? N3 C39 H39A 109.5 . . ? N3 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N3 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C1 Ni1 P1 89.70(18) . . ? C1 Ni1 P2 87.01(18) . . ? P1 Ni1 P2 175.74(7) . . ? C1 Ni1 Cl1 175.70(19) . . ? P1 Ni1 Cl1 90.04(7) . . ? P2 Ni1 Cl1 93.44(7) . . ? C12 Ni2 P3 90.39(18) . . ? C12 Ni2 P4 89.26(18) . . ? P3 Ni2 P4 177.61(8) . . ? C12 Ni2 Cl2 175.38(19) . . ? P3 Ni2 Cl2 90.30(7) . . ? P4 Ni2 Cl2 90.24(7) . . ? C23 Ni3 P6 88.48(18) . . ? C23 Ni3 P5 88.82(18) . . ? P6 Ni3 P5 177.30(8) . . ? C23 Ni3 Cl3 174.10(19) . . ? P6 Ni3 Cl3 92.63(7) . . ? P5 Ni3 Cl3 90.05(7) . . ? C38 P5 C36 103.6(4) . . ? C38 P5 C37 103.1(5) . . ? C36 P5 C37 101.5(4) . . ? C38 P5 Ni3 109.8(3) . . ? C36 P5 Ni3 116.9(3) . . ? C37 P5 Ni3 119.9(3) . . ? C9 P1 C10 102.3(4) . . ? C9 P1 C11 103.8(3) . . ? C10 P1 C11 102.5(3) . . ? C9 P1 Ni1 113.8(3) . . ? C10 P1 Ni1 119.7(2) . . ? C11 P1 Ni1 112.9(2) . . ? C21 P3 C22 104.8(3) . . ? C21 P3 C20 102.1(4) . . ? C22 P3 C20 102.7(4) . . ? C21 P3 Ni2 111.4(3) . . ? C22 P3 Ni2 114.2(3) . . ? C20 P3 Ni2 119.9(3) . . ? C35 P6 C33 103.9(4) . . ? C35 P6 C34 100.6(4) . . ? C33 P6 C34 102.4(5) . . ? C35 P6 Ni3 115.5(3) . . ? C33 P6 Ni3 113.8(3) . . ? C34 P6 Ni3 118.5(3) . . ? C29 N3 C39 121.7(5) . . ? C29 N3 H23 119.2 . . ? C39 N3 H23 119.2 . . ? C18 N2 C19 121.3(5) . . ? C18 N2 H12 119.3 . . ? C19 N2 H12 119.3 . . ? O3 C29 N3 120.3(6) . . ? O3 C29 C28 121.9(5) . . ? N3 C29 C28 117.8(5) . . ? C14 C13 C12 120.6(5) . . ? C14 C13 C18 121.2(5) . . ? C12 C13 C18 118.1(5) . . ? O1 C7 N1 120.6(6) . . ? O1 C7 C6 121.8(6) . . ? N1 C7 C6 117.6(5) . . ? C17 C12 C13 116.8(5) . . ? C17 C12 Ni2 120.4(5) . . ? C13 C12 Ni2 122.6(4) . . ? O2 C18 N2 120.5(6) . . ? O2 C18 C13 122.1(5) . . ? N2 C18 C13 117.3(5) . . ? C2 C1 C6 117.1(5) . . ? C2 C1 Ni1 120.0(5) . . ? C6 C1 Ni1 122.9(4) . . ? C23 C28 C27 119.8(5) . . ? C23 C28 C29 118.3(5) . . ? C27 C28 C29 121.9(5) . . ? C25 C24 C23 123.2(6) . . ? C25 C24 H24 118.4 . . ? C23 C24 H24 118.4 . . ? C7 N1 C8 121.5(5) . . ? C7 N1 H1 119.2 . . ? C8 N1 H1 119.2 . . ? C24 C23 C28 116.9(5) . . ? C24 C23 Ni3 121.3(5) . . ? C28 C23 Ni3 121.8(4) . . ? C3 C2 C1 122.1(6) . . ? C3 C2 H2 119.0 . . ? C1 C2 H2 119.0 . . ? C16 C17 C12 121.9(6) . . ? C16 C17 H17 119.1 . . ? C12 C17 H17 119.1 . . ? C15 C16 C17 120.4(6) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C26 C27 C28 120.8(6) . . ? C26 C27 H27 119.6 . . ? C28 C27 H27 119.6 . . ? C5 C6 C1 120.5(6) . . ? C5 C6 C7 121.8(6) . . ? C1 C6 C7 117.7(5) . . ? C15 C14 C13 120.7(6) . . ? C15 C14 H14 119.7 . . ? C13 C14 H14 119.7 . . ? C14 C15 C16 119.6(6) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? C26 C25 C24 119.0(6) . . ? C26 C25 H25 120.5 . . ? C24 C25 H25 120.5 . . ? C3 C4 C5 120.2(6) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C6 120.6(6) . . ? C4 C5 H5 119.7 . . ? C6 C5 H5 119.7 . . ? N1 C8 H8A 109.5 . . ? N1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C27 C26 C25 120.4(6) . . ? C27 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? N2 C19 H19A 109.5 . . ? N2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C4 C3 C2 119.5(6) . . ? C4 C3 H3 120.3 . . ? C2 C3 H3 120.3 . . ? P1 C11 H11A 109.5 . . ? P1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? P1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? P3 C21 H21A 109.5 . . ? P3 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? P3 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? P3 C22 H22A 109.5 . . ? P3 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? P3 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? P1 C9 H9A 109.5 . . ? P1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? P1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? P1 C10 H10A 109.5 . . ? P1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? P1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? P3 C20 H20A 109.5 . . ? P3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? P3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? P2 C40 H40A 109.5 . . ? P2 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? P2 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? P4 C42 H42A 109.5 . . ? P4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? P4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? P4 C41 H41A 109.5 . . ? P4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? P4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 24.45 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.566 _refine_diff_density_min -0.568 _refine_diff_density_rms 0.113 # Attachment '- 7.cif' data_sun13a _database_code_depnum_ccdc_archive 'CCDC 806081' #TrackingRef '- 7.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H32 Cl N Ni O P2' _chemical_formula_sum 'C17 H32 Cl N Ni O P2' _chemical_formula_weight 422.52 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ni Ni 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M pbca _symmetry_space_group_name_hall -P2ac2ab loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.6040(19) _cell_length_b 19.709(4) _cell_length_c 22.573(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4272.7(15) _cell_formula_units_Z 8 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 1.186 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8707 _exptl_absorpt_correction_T_max 0.9216 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15728 _diffrn_reflns_av_R_equivalents 0.0592 _diffrn_reflns_av_sigmaI/netI 0.0409 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3672 _reflns_number_gt 3125 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0672P)^2^+11.2785P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3672 _refine_ls_number_parameters 243 _refine_ls_number_restraints 162 _refine_ls_R_factor_all 0.0610 _refine_ls_R_factor_gt 0.0515 _refine_ls_wR_factor_ref 0.1342 _refine_ls_wR_factor_gt 0.1290 _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_restrained_S_all 1.026 _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 O1 O 0.8114(3) 0.11763(16) 0.70021(14) 0.0376(7) Uani 1 1 d . . . N1 N 1.0022(5) 0.13835(19) 0.75547(18) 0.0374(9) Uani 1 1 d . . . Ni1 Ni 0.83970(5) 0.09095(2) 0.57644(2) 0.02370(17) Uani 1 1 d . . . Cl1 Cl 0.66967(11) 0.13797(5) 0.52218(5) 0.0364(3) Uani 1 1 d . . . P1 P 0.97318(11) 0.17776(5) 0.55592(5) 0.0258(2) Uani 1 1 d . . . P2 P 0.70767(11) 0.00264(5) 0.59330(5) 0.0249(2) Uani 1 1 d . . . C1 C 1.1487(5) 0.1835(2) 0.5855(2) 0.0379(10) Uani 1 1 d U . . H1A H 1.1933 0.2234 0.5702 0.057 Uiso 1 1 calc R . . H1B H 1.2007 0.1441 0.5740 0.057 Uiso 1 1 calc R . . H1C H 1.1447 0.1861 0.6279 0.057 Uiso 1 1 calc R . . C2 C 0.8992(6) 0.2582(2) 0.5783(2) 0.0432(11) Uani 1 1 d U . . H2A H 0.8851 0.2584 0.6204 0.065 Uiso 1 1 calc R . . H2B H 0.8115 0.2648 0.5586 0.065 Uiso 1 1 calc R . . H2C H 0.9616 0.2943 0.5677 0.065 Uiso 1 1 calc R . . C3 C 1.0000(5) 0.1892(2) 0.4770(2) 0.0370(10) Uani 1 1 d U . . H3A H 0.9116 0.1896 0.4572 0.056 Uiso 1 1 calc R . . H3B H 1.0557 0.1526 0.4620 0.056 Uiso 1 1 calc R . . H3C H 1.0469 0.2315 0.4701 0.056 Uiso 1 1 calc R . . C4 C 0.7619(5) -0.0628(2) 0.64530(19) 0.0349(9) Uani 1 1 d U . . H4A H 0.7755 -0.0429 0.6837 0.052 Uiso 1 1 calc R . . H4B H 0.8475 -0.0827 0.6320 0.052 Uiso 1 1 calc R . . H4C H 0.6913 -0.0971 0.6477 0.052 Uiso 1 1 calc R . . C5 C 0.5340(5) 0.0228(2) 0.6190(2) 0.0389(10) Uani 1 1 d U . . H5A H 0.4909 0.0539 0.5919 0.058 Uiso 1 1 calc R . . H5B H 0.5394 0.0432 0.6576 0.058 Uiso 1 1 calc R . . H5C H 0.4797 -0.0180 0.6213 0.058 Uiso 1 1 calc R . . C6 C 0.6756(5) -0.0451(2) 0.5258(2) 0.0360(10) Uani 1 1 d U . . H6A H 0.6080 -0.0799 0.5335 0.054 Uiso 1 1 calc R . . H6B H 0.7609 -0.0655 0.5126 0.054 Uiso 1 1 calc R . . H6C H 0.6410 -0.0151 0.4957 0.054 Uiso 1 1 calc R . . C7 C 0.9862(4) 0.04576(17) 0.61559(17) 0.0239(8) Uani 1 1 d U . . C8 C 1.0191(4) 0.05686(17) 0.67560(17) 0.0234(7) Uani 1 1 d U . . C9 C 1.1259(5) 0.02041(19) 0.70313(19) 0.0289(8) Uani 1 1 d U . . C10 C 1.2019(5) -0.0274(2) 0.6719(2) 0.0311(9) Uani 1 1 d U . . C11 C 1.1720(5) -0.0387(2) 0.61254(19) 0.0304(9) Uani 1 1 d U . . C12 C 1.0672(5) -0.00219(19) 0.58542(18) 0.0285(8) Uani 1 1 d U . . C13 C 0.9352(4) 0.10639(19) 0.71107(18) 0.0268(8) Uani 1 1 d U . . C14 C 0.9323(7) 0.1841(3) 0.7963(3) 0.0556(13) Uani 1 1 d U . . C15 C 1.0318(10) 0.2383(4) 0.8180(4) 0.097(2) Uani 1 1 d U . . H15A H 0.9818 0.2661 0.8464 0.116 Uiso 1 1 calc R . . H15B H 1.1058 0.2157 0.8395 0.116 Uiso 1 1 calc R . . C16 C 1.0930(11) 0.2812(5) 0.7780(5) 0.107(2) Uani 1 1 d U . . H16A H 1.1391 0.2533 0.7486 0.129 Uiso 1 1 calc R . . H16B H 1.1654 0.3058 0.7989 0.129 Uiso 1 1 calc R . . C17 C 1.0078(12) 0.3324(5) 0.7453(5) 0.116(3) Uani 1 1 d U . . H17A H 0.9360 0.3096 0.7234 0.174 Uiso 1 1 calc R . . H17B H 1.0664 0.3572 0.7186 0.174 Uiso 1 1 calc R . . H17C H 0.9661 0.3632 0.7731 0.174 Uiso 1 1 calc R . . H11 H 1.219(5) -0.075(2) 0.591(2) 0.034(12) Uiso 1 1 d . . . H12 H 1.049(5) -0.011(2) 0.542(2) 0.034(12) Uiso 1 1 d . . . H10 H 1.278(6) -0.057(3) 0.691(2) 0.050(14) Uiso 1 1 d . . . H1 H 1.081(6) 0.130(2) 0.761(2) 0.030(13) Uiso 1 1 d . . . H9 H 1.145(5) 0.028(2) 0.745(2) 0.034(12) Uiso 1 1 d . . . H14A H 0.885(7) 0.224(3) 0.776(3) 0.071(18) Uiso 1 1 d . . . H14B H 0.891(7) 0.156(3) 0.817(3) 0.059(17) Uiso 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 O1 0.0247(16) 0.0529(18) 0.0352(17) 0.0020(14) 0.0020(14) 0.0093(13) N1 0.031(2) 0.047(2) 0.034(2) -0.0102(16) 0.0007(19) 0.0070(17) Ni1 0.0194(3) 0.0251(3) 0.0266(3) 0.00299(19) -0.0057(2) -0.00179(18) Cl1 0.0289(6) 0.0329(5) 0.0473(6) 0.0060(4) -0.0147(5) 0.0020(4) P1 0.0257(5) 0.0246(5) 0.0271(5) 0.0006(4) -0.0025(4) -0.0032(4) P2 0.0202(5) 0.0301(5) 0.0243(5) 0.0019(4) -0.0016(4) -0.0038(4) C1 0.0367(13) 0.0385(12) 0.0385(13) 0.0006(9) -0.0011(9) -0.0026(9) C2 0.0430(14) 0.0420(13) 0.0446(14) -0.0021(9) 0.0008(9) 0.0000(9) C3 0.0376(13) 0.0375(12) 0.0361(12) 0.0013(9) -0.0002(9) -0.0013(9) C4 0.0347(13) 0.0351(12) 0.0348(12) 0.0025(9) 0.0004(9) -0.0011(9) C5 0.0372(13) 0.0413(12) 0.0383(13) 0.0003(9) -0.0003(9) 0.0000(9) C6 0.0364(13) 0.0357(12) 0.0360(13) -0.0007(9) -0.0006(9) -0.0018(9) C7 0.0230(11) 0.0245(10) 0.0242(11) 0.0013(8) -0.0005(9) -0.0018(8) C8 0.0224(11) 0.0245(10) 0.0231(11) 0.0005(8) 0.0002(9) -0.0016(8) C9 0.0283(12) 0.0306(11) 0.0277(12) 0.0004(9) -0.0004(9) -0.0002(9) C10 0.0299(12) 0.0327(11) 0.0308(12) 0.0006(9) -0.0003(9) 0.0015(9) C11 0.0296(12) 0.0312(11) 0.0304(12) -0.0008(9) 0.0004(9) 0.0011(9) C12 0.0282(12) 0.0293(11) 0.0279(11) -0.0003(9) -0.0005(9) -0.0012(9) C13 0.0266(12) 0.0278(11) 0.0260(11) 0.0019(9) 0.0010(9) 0.0008(9) C14 0.0566(16) 0.0559(15) 0.0544(16) -0.0019(10) 0.0020(10) 0.0025(10) C15 0.097(2) 0.097(2) 0.097(2) -0.0037(10) -0.0012(10) 0.0034(10) C16 0.106(3) 0.106(3) 0.109(3) -0.0036(10) -0.0004(10) 0.0004(10) C17 0.116(3) 0.116(3) 0.116(3) -0.0010(10) -0.0002(10) 0.0006(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 O1 C13 1.234(5) . ? N1 C13 1.347(6) . ? N1 C14 1.453(7) . ? Ni1 C7 1.885(4) . ? Ni1 P2 2.1868(11) . ? Ni1 P1 2.1876(11) . ? Ni1 Cl1 2.2418(11) . ? P1 C2 1.810(5) . ? P1 C3 1.814(5) . ? P1 C1 1.816(5) . ? P2 C5 1.810(5) . ? P2 C6 1.817(5) . ? P2 C4 1.819(4) . ? C7 C12 1.401(6) . ? C7 C8 1.408(5) . ? C8 C9 1.398(6) . ? C8 C13 1.498(5) . ? C9 C10 1.384(6) . ? C10 C11 1.389(6) . ? C11 C12 1.380(6) . ? C14 C15 1.515(11) . ? C15 C16 1.370(12) . ? C16 C17 1.493(13) . ? 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 C13 N1 C14 122.8(4) . . ? C7 Ni1 P2 88.57(12) . . ? C7 Ni1 P1 91.80(12) . . ? P2 Ni1 P1 177.67(5) . . ? C7 Ni1 Cl1 174.32(12) . . ? P2 Ni1 Cl1 90.10(4) . . ? P1 Ni1 Cl1 89.30(4) . . ? C2 P1 C3 102.7(2) . . ? C2 P1 C1 102.0(2) . . ? C3 P1 C1 102.8(2) . . ? C2 P1 Ni1 113.35(17) . . ? C3 P1 Ni1 112.87(15) . . ? C1 P1 Ni1 120.98(15) . . ? C5 P2 C6 103.1(2) . . ? C5 P2 C4 102.3(2) . . ? C6 P2 C4 102.9(2) . . ? C5 P2 Ni1 114.54(15) . . ? C6 P2 Ni1 111.39(15) . . ? C4 P2 Ni1 120.67(15) . . ? C12 C7 C8 116.6(4) . . ? C12 C7 Ni1 120.4(3) . . ? C8 C7 Ni1 123.0(3) . . ? C9 C8 C7 120.8(4) . . ? C9 C8 C13 119.5(3) . . ? C7 C8 C13 119.6(3) . . ? C10 C9 C8 120.7(4) . . ? C9 C10 C11 119.4(4) . . ? C12 C11 C10 119.7(4) . . ? C11 C12 C7 122.7(4) . . ? O1 C13 N1 121.6(4) . . ? O1 C13 C8 122.0(4) . . ? N1 C13 C8 116.5(4) . . ? N1 C14 C15 110.6(6) . . ? C16 C15 C14 119.5(9) . . ? C15 C16 C17 120.5(10) . . ? _diffrn_measured_fraction_theta_max 0.974 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.974 _refine_diff_density_max 1.354 _refine_diff_density_min -0.706 _refine_diff_density_rms 0.091 # Attachment '- 10.cif' data_10 _database_code_depnum_ccdc_archive 'CCDC 806082' #TrackingRef '- 10.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H41 Cl Co N O P3' _chemical_formula_weight 498.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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)/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 16.4434(11) _cell_length_b 9.1090(6) _cell_length_c 18.6041(13) _cell_angle_alpha 90.00 _cell_angle_beta 108.4460(10) _cell_angle_gamma 90.00 _cell_volume 2643.4(3) _cell_formula_units_Z 4 _cell_measurement_temperature 273(2) _cell_measurement_reflns_used 2747 _cell_measurement_theta_min 2.31 _cell_measurement_theta_max 21.73 _exptl_crystal_description ? _exptl_crystal_colour ? _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 1.253 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1060 _exptl_absorpt_coefficient_mu 0.942 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8716 _exptl_absorpt_correction_T_max 0.9117 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 273(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source '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 14855 _diffrn_reflns_av_R_equivalents 0.0414 _diffrn_reflns_av_sigmaI/netI 0.0555 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.31 _diffrn_reflns_theta_max 27.12 _reflns_number_total 5754 _reflns_number_gt 3856 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _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^)+(0.0650P)^2^+0.3118P] 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 5754 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0804 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.1318 _refine_ls_wR_factor_gt 0.1143 _refine_ls_goodness_of_fit_ref 1.015 _refine_ls_restrained_S_all 1.015 _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 C18 C 0.0392(3) -0.0639(4) 0.4030(3) 0.0696(12) Uani 1 1 d . . . H18A H 0.0563 -0.0552 0.4572 0.104 Uiso 1 1 calc R . . H18B H 0.0643 -0.1506 0.3896 0.104 Uiso 1 1 calc R . . H18C H -0.0222 -0.0708 0.3832 0.104 Uiso 1 1 calc R . . C20 C 0.0376(3) 0.0648(5) 0.2618(2) 0.0674(11) Uani 1 1 d . . . H20A H 0.0754 -0.0027 0.2486 0.101 Uiso 1 1 calc R . . H20B H 0.0364 0.1559 0.2356 0.101 Uiso 1 1 calc R . . H20C H -0.0192 0.0240 0.2475 0.101 Uiso 1 1 calc R . . C12 C 0.4038(2) 0.2199(5) 0.5546(2) 0.0727(12) Uani 1 1 d . . . H12A H 0.4105 0.1151 0.5564 0.109 Uiso 1 1 calc R . . H12B H 0.3759 0.2499 0.5903 0.109 Uiso 1 1 calc R . . H12C H 0.4592 0.2656 0.5671 0.109 Uiso 1 1 calc R . . C16 C 0.3635(3) -0.1117(5) 0.4299(2) 0.0719(12) Uani 1 1 d . . . H16A H 0.3557 -0.1308 0.4780 0.108 Uiso 1 1 calc R . . H16B H 0.4099 -0.0437 0.4364 0.108 Uiso 1 1 calc R . . H16C H 0.3765 -0.2018 0.4091 0.108 Uiso 1 1 calc R . . C19 C -0.0062(2) 0.2252(5) 0.3704(3) 0.0718(12) Uani 1 1 d . . . H19A H 0.0050 0.2529 0.4224 0.108 Uiso 1 1 calc R . . H19B H -0.0615 0.1795 0.3518 0.108 Uiso 1 1 calc R . . H19C H -0.0051 0.3109 0.3407 0.108 Uiso 1 1 calc R . . C15 C 0.2900(3) -0.0078(5) 0.2774(2) 0.0786(13) Uani 1 1 d . . . H15A H 0.3217 0.0817 0.2801 0.118 Uiso 1 1 calc R . . H15B H 0.2377 -0.0026 0.2356 0.118 Uiso 1 1 calc R . . H15C H 0.3237 -0.0890 0.2701 0.118 Uiso 1 1 calc R . . C13 C 0.4179(3) 0.2669(6) 0.4087(3) 0.0829(14) Uani 1 1 d . . . H13A H 0.3905 0.2939 0.3568 0.124 Uiso 1 1 calc R . . H13B H 0.4401 0.1689 0.4110 0.124 Uiso 1 1 calc R . . H13C H 0.4640 0.3337 0.4314 0.124 Uiso 1 1 calc R . . C17 C 0.2052(3) -0.2053(4) 0.3461(3) 0.0787(14) Uani 1 1 d . . . H17A H 0.1876 -0.2309 0.3891 0.118 Uiso 1 1 calc R . . H17B H 0.2410 -0.2816 0.3370 0.118 Uiso 1 1 calc R . . H17C H 0.1554 -0.1938 0.3023 0.118 Uiso 1 1 calc R . . C14 C 0.3381(3) 0.4724(4) 0.4726(3) 0.0917(16) Uani 1 1 d . . . H14A H 0.3048 0.5173 0.4259 0.138 Uiso 1 1 calc R . . H14B H 0.3957 0.5096 0.4871 0.138 Uiso 1 1 calc R . . H14C H 0.3131 0.4949 0.5114 0.138 Uiso 1 1 calc R . . Co Co 0.21365(3) 0.15914(4) 0.41410(2) 0.03534(14) Uani 1 1 d . . . P2 P 0.07530(5) 0.09709(10) 0.36327(5) 0.0406(2) Uani 1 1 d . . . Cl Cl 0.19252(7) 0.35113(10) 0.29076(5) 0.0589(3) Uani 1 1 d . . . P1 P 0.33960(6) 0.27465(11) 0.46023(5) 0.0502(2) Uani 1 1 d . . . P3 P 0.26499(6) -0.03310(10) 0.36514(5) 0.0470(2) Uani 1 1 d . . . O1 O 0.23151(14) 0.0193(2) 0.51618(12) 0.0440(5) Uani 1 1 d . . . N N 0.21909(18) 0.0282(3) 0.63258(15) 0.0487(7) Uani 1 1 d . . . H0 H 0.2052 0.0781 0.6661 0.058 Uiso 1 1 calc R . . C7 C 0.2114(2) 0.0894(3) 0.56556(17) 0.0385(7) Uani 1 1 d . . . C6 C 0.17811(19) 0.2412(3) 0.54865(17) 0.0373(7) Uani 1 1 d . . . C2 C 0.1428(2) 0.4379(3) 0.45932(19) 0.0467(8) Uani 1 1 d . . . H2 H 0.1387 0.4768 0.4121 0.056 Uiso 1 1 calc R . . C1 C 0.1757(2) 0.2965(3) 0.47769(17) 0.0371(7) Uani 1 1 d . . . C5 C 0.1507(2) 0.3248(4) 0.5993(2) 0.0518(9) Uani 1 1 d . . . H5 H 0.1531 0.2863 0.6462 0.062 Uiso 1 1 calc R . . C4 C 0.1202(3) 0.4645(4) 0.5795(2) 0.0625(11) Uani 1 1 d . . . H4 H 0.1021 0.5211 0.6131 0.075 Uiso 1 1 calc R . . C3 C 0.1166(3) 0.5207(4) 0.5096(2) 0.0586(10) Uani 1 1 d . . . H3 H 0.0961 0.6154 0.4964 0.070 Uiso 1 1 calc R . . C9 C 0.3473(3) -0.1349(5) 0.6695(3) 0.0747(13) Uani 1 1 d . . . H9A H 0.3630 -0.2378 0.6760 0.090 Uiso 1 1 calc R . . H9B H 0.3638 -0.0981 0.6272 0.090 Uiso 1 1 calc R . . C8 C 0.2507(3) -0.1219(4) 0.6502(2) 0.0609(10) Uani 1 1 d . . . H8A H 0.2235 -0.1843 0.6070 0.073 Uiso 1 1 calc R . . H8B H 0.2341 -0.1575 0.6927 0.073 Uiso 1 1 calc R . . C10 C 0.3961(3) -0.0532(6) 0.7394(3) 0.0936(15) Uani 1 1 d . . . H10A H 0.3836 -0.0969 0.7823 0.112 Uiso 1 1 calc R . . H10B H 0.3756 0.0473 0.7348 0.112 Uiso 1 1 calc R . . C11 C 0.4917(4) -0.0509(8) 0.7561(4) 0.138(2) Uani 1 1 d . . . H11A H 0.5175 0.0055 0.8012 0.207 Uiso 1 1 calc R . . H11B H 0.5052 -0.0072 0.7143 0.207 Uiso 1 1 calc R . . H11C H 0.5133 -0.1495 0.7635 0.207 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 C18 0.064(3) 0.074(3) 0.077(3) 0.014(2) 0.032(2) -0.008(2) C20 0.063(2) 0.087(3) 0.042(2) -0.008(2) 0.0037(19) -0.003(2) C12 0.049(2) 0.092(3) 0.066(3) 0.006(2) 0.001(2) 0.000(2) C16 0.065(3) 0.068(3) 0.076(3) -0.003(2) 0.012(2) 0.025(2) C19 0.049(2) 0.078(3) 0.083(3) -0.008(2) 0.013(2) 0.021(2) C15 0.103(4) 0.085(3) 0.062(3) -0.005(2) 0.046(3) 0.018(3) C13 0.062(3) 0.105(4) 0.089(4) -0.002(3) 0.036(3) -0.021(3) C17 0.086(3) 0.045(2) 0.105(4) -0.014(2) 0.029(3) 0.009(2) C14 0.069(3) 0.056(3) 0.132(5) -0.004(3) 0.006(3) -0.016(2) Co 0.0391(3) 0.0378(2) 0.0303(2) -0.00110(18) 0.01258(18) 0.00431(19) P2 0.0403(5) 0.0432(5) 0.0379(5) 0.0005(4) 0.0117(4) 0.0032(4) Cl 0.0743(6) 0.0681(6) 0.0394(5) 0.0035(4) 0.0253(5) -0.0008(5) P1 0.0446(5) 0.0547(6) 0.0479(6) 0.0002(4) 0.0098(4) -0.0047(4) P3 0.0496(5) 0.0497(5) 0.0433(5) -0.0048(4) 0.0171(4) 0.0124(4) O1 0.0587(14) 0.0393(12) 0.0367(12) 0.0036(10) 0.0187(11) 0.0120(11) N 0.0639(18) 0.0514(17) 0.0358(15) 0.0123(13) 0.0228(14) 0.0154(15) C7 0.0419(18) 0.0433(18) 0.0313(17) 0.0040(14) 0.0132(14) 0.0031(15) C6 0.0416(18) 0.0373(17) 0.0324(17) -0.0009(13) 0.0110(14) 0.0073(14) C2 0.063(2) 0.0408(18) 0.0366(19) 0.0022(15) 0.0161(16) 0.0076(16) C1 0.0431(18) 0.0377(17) 0.0312(17) 0.0036(13) 0.0129(14) 0.0062(14) C5 0.068(2) 0.055(2) 0.0364(19) 0.0036(16) 0.0218(18) 0.0157(18) C4 0.087(3) 0.057(2) 0.047(2) -0.0025(18) 0.026(2) 0.029(2) C3 0.077(3) 0.043(2) 0.054(2) -0.0021(17) 0.018(2) 0.0229(19) C9 0.085(3) 0.074(3) 0.071(3) 0.025(2) 0.034(3) 0.031(2) C8 0.082(3) 0.053(2) 0.052(2) 0.0210(18) 0.028(2) 0.013(2) C10 0.087(4) 0.111(4) 0.080(4) 0.008(3) 0.021(3) 0.015(3) C11 0.084(4) 0.182(7) 0.138(6) 0.021(5) 0.022(4) 0.012(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 C18 P2 1.825(4) . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C20 P2 1.815(4) . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C12 P1 1.809(4) . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C16 P3 1.831(4) . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C19 P2 1.813(4) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C15 P3 1.820(4) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C13 P1 1.833(4) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C17 P3 1.825(4) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C14 P1 1.817(4) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? Co C1 1.955(3) . ? Co O1 2.228(2) . ? Co P1 2.2379(10) . ? Co P2 2.2422(10) . ? Co P3 2.2574(9) . ? Co Cl 2.8178(10) . ? O1 C7 1.246(4) . ? N C7 1.335(4) . ? N C8 1.462(4) . ? N H0 0.8600 . ? C7 C6 1.484(4) . ? C6 C5 1.392(4) . ? C6 C1 1.402(4) . ? C2 C3 1.373(5) . ? C2 C1 1.397(4) . ? C2 H2 0.9300 . ? C5 C4 1.375(5) . ? C5 H5 0.9300 . ? C4 C3 1.381(5) . ? C4 H4 0.9300 . ? C3 H3 0.9300 . ? C9 C10 1.494(7) . ? C9 C8 1.518(6) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C10 C11 1.502(7) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 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 P2 C18 H18A 109.5 . . ? P2 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? P2 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? P2 C20 H20A 109.5 . . ? P2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? P2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? P1 C12 H12A 109.5 . . ? P1 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? P1 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? P3 C16 H16A 109.5 . . ? P3 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? P3 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? P2 C19 H19A 109.5 . . ? P2 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? P2 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? P3 C15 H15A 109.5 . . ? P3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? P3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? P1 C13 H13A 109.5 . . ? P1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? P1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? P3 C17 H17A 109.5 . . ? P3 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? P3 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? P1 C14 H14A 109.5 . . ? P1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? P1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C1 Co O1 80.30(10) . . ? C1 Co P1 84.32(10) . . ? O1 Co P1 94.91(7) . . ? C1 Co P2 86.62(10) . . ? O1 Co P2 93.32(6) . . ? P1 Co P2 166.56(4) . . ? C1 Co P3 166.53(9) . . ? O1 Co P3 86.28(6) . . ? P1 Co P3 95.77(4) . . ? P2 Co P3 95.36(4) . . ? C1 Co Cl 96.59(9) . . ? O1 Co Cl 176.52(6) . . ? P1 Co Cl 83.17(3) . . ? P2 Co Cl 88.04(3) . . ? P3 Co Cl 96.80(3) . . ? C19 P2 C20 99.4(2) . . ? C19 P2 C18 98.3(2) . . ? C20 P2 C18 104.1(2) . . ? C19 P2 Co 118.79(15) . . ? C20 P2 Co 116.55(14) . . ? C18 P2 Co 116.67(14) . . ? C12 P1 C14 100.2(2) . . ? C12 P1 C13 101.8(2) . . ? C14 P1 C13 98.3(2) . . ? C12 P1 Co 115.34(14) . . ? C14 P1 Co 117.83(15) . . ? C13 P1 Co 119.94(16) . . ? C15 P3 C17 101.3(2) . . ? C15 P3 C16 103.7(2) . . ? C17 P3 C16 95.8(2) . . ? C15 P3 Co 118.89(15) . . ? C17 P3 Co 119.82(14) . . ? C16 P3 Co 113.82(14) . . ? C7 O1 Co 109.95(19) . . ? C7 N C8 121.5(3) . . ? C7 N H0 119.3 . . ? C8 N H0 119.3 . . ? O1 C7 N 120.4(3) . . ? O1 C7 C6 119.2(3) . . ? N C7 C6 120.5(3) . . ? C5 C6 C1 121.5(3) . . ? C5 C6 C7 122.8(3) . . ? C1 C6 C7 115.7(3) . . ? C3 C2 C1 121.4(3) . . ? C3 C2 H2 119.3 . . ? C1 C2 H2 119.3 . . ? C2 C1 C6 117.1(3) . . ? C2 C1 Co 128.0(2) . . ? C6 C1 Co 114.9(2) . . ? C4 C5 C6 119.5(3) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C5 C4 C3 120.0(3) . . ? C5 C4 H4 120.0 . . ? C3 C4 H4 120.0 . . ? C2 C3 C4 120.6(3) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C10 C9 C8 113.6(4) . . ? C10 C9 H9A 108.8 . . ? C8 C9 H9A 108.8 . . ? C10 C9 H9B 108.8 . . ? C8 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? N C8 C9 113.4(3) . . ? N C8 H8A 108.9 . . ? C9 C8 H8A 108.9 . . ? N C8 H8B 108.9 . . ? C9 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? C9 C10 C11 115.2(5) . . ? C9 C10 H10A 108.5 . . ? C11 C10 H10A 108.5 . . ? C9 C10 H10B 108.5 . . ? C11 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.12 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.052 _refine_diff_density_min -0.272 _refine_diff_density_rms 0.073 # Attachment '- 11.cif' data_sun-7 _database_code_depnum_ccdc_archive 'CCDC 806083' #TrackingRef '- 11.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H36 Cl Co N2 O2 P2' _chemical_formula_sum 'C32 H36 Cl Co N2 O2 P2' _chemical_formula_weight 636.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _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 10.990(2) _cell_length_b 14.336(3) _cell_length_c 19.780(4) _cell_angle_alpha 90.00 _cell_angle_beta 93.90(3) _cell_angle_gamma 90.00 _cell_volume 3109.0(11) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1328 _exptl_absorpt_coefficient_mu 0.772 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19749 _diffrn_reflns_av_R_equivalents 0.0224 _diffrn_reflns_av_sigmaI/netI 0.0166 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.76 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5256 _reflns_number_gt 4816 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0514P)^2^+2.2235P] 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 5256 _refine_ls_number_parameters 367 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0383 _refine_ls_R_factor_gt 0.0338 _refine_ls_wR_factor_ref 0.0945 _refine_ls_wR_factor_gt 0.0892 _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_restrained_S_all 1.085 _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 Co1 Co 0.47585(2) 0.228040(18) 0.291714(14) 0.02011(10) Uani 1 1 d . . . P1 P 0.33308(6) 0.11606(4) 0.28101(3) 0.03053(15) Uani 1 1 d . . . P2 P 0.61066(5) 0.34628(4) 0.28939(3) 0.02189(14) Uani 1 1 d . . . Cl1 Cl 0.07434(6) 0.31185(6) 0.36808(4) 0.0509(2) Uani 1 1 d . . . N1 N 0.60779(18) 0.13972(13) 0.28375(10) 0.0279(4) Uani 1 1 d . . . N2 N 0.43658(16) 0.25901(12) 0.39264(9) 0.0223(4) Uani 1 1 d . . . O1 O 0.71110(18) 0.05885(13) 0.20398(10) 0.0435(5) Uani 1 1 d . . . O2 O 0.34211(13) 0.31766(10) 0.30135(8) 0.0253(3) Uani 1 1 d . . . C1 C 0.4768(2) 0.23274(14) 0.19577(12) 0.0240(5) Uani 1 1 d . . . C2 C 0.4099(2) 0.29303(16) 0.15188(12) 0.0275(5) Uani 1 1 d . . . H2A H 0.3490 0.3322 0.1686 0.033 Uiso 1 1 calc R . . C3 C 0.4331(2) 0.29531(17) 0.08355(12) 0.0313(5) Uani 1 1 d . . . H3A H 0.3894 0.3378 0.0541 0.038 Uiso 1 1 calc R . . C4 C 0.5189(2) 0.23663(17) 0.05765(13) 0.0340(5) Uani 1 1 d . . . H4A H 0.5334 0.2388 0.0109 0.041 Uiso 1 1 calc R . . C5 C 0.5833(2) 0.17477(16) 0.10046(12) 0.0306(5) Uani 1 1 d . . . H5A H 0.6410 0.1333 0.0831 0.037 Uiso 1 1 calc R . . C6 C 0.5626(2) 0.17397(15) 0.16908(12) 0.0260(5) Uani 1 1 d . . . C7 C 0.6353(2) 0.11788(16) 0.21974(12) 0.0303(5) Uani 1 1 d . . . C8 C 0.6767(2) 0.09754(16) 0.33871(13) 0.0340(6) Uani 1 1 d . . . C9 C 0.8036(3) 0.1075(2) 0.34591(15) 0.0444(7) Uani 1 1 d . . . H9A H 0.8445 0.1424 0.3135 0.053 Uiso 1 1 calc R . . C10 C 0.8698(3) 0.0664(2) 0.40033(18) 0.0578(8) Uani 1 1 d . . . H10A H 0.9558 0.0739 0.4050 0.069 Uiso 1 1 calc R . . C11 C 0.8125(3) 0.0148(2) 0.44759(17) 0.0592(9) Uani 1 1 d . . . H11A H 0.8587 -0.0138 0.4843 0.071 Uiso 1 1 calc R . . C12 C 0.6879(3) 0.0052(2) 0.44116(15) 0.0549(8) Uani 1 1 d . . . H12A H 0.6478 -0.0300 0.4737 0.066 Uiso 1 1 calc R . . C13 C 0.6200(3) 0.04658(19) 0.38738(14) 0.0439(7) Uani 1 1 d . . . H13A H 0.5338 0.0399 0.3839 0.053 Uiso 1 1 calc R . . C14 C 0.1663(3) 0.3992(2) 0.40409(14) 0.0422(7) Uani 1 1 d . . . C15 C 0.1111(3) 0.4751(2) 0.43395(15) 0.0560(9) Uani 1 1 d . . . H15A H 0.0248 0.4782 0.4349 0.067 Uiso 1 1 calc R . . C16 C 0.1833(4) 0.5453(2) 0.46200(16) 0.0619(10) Uani 1 1 d . . . H16A H 0.1462 0.5974 0.4820 0.074 Uiso 1 1 calc R . . C17 C 0.3094(3) 0.5414(2) 0.46156(15) 0.0558(8) Uani 1 1 d . . . H17A H 0.3574 0.5914 0.4803 0.067 Uiso 1 1 calc R . . C18 C 0.3652(3) 0.46605(18) 0.43430(14) 0.0425(7) Uani 1 1 d . . . H18A H 0.4517 0.4623 0.4358 0.051 Uiso 1 1 calc R . . C19 C 0.2915(2) 0.39290(17) 0.40343(12) 0.0338(6) Uani 1 1 d . . . C20 C 0.35571(19) 0.31770(15) 0.36664(11) 0.0235(4) Uani 1 1 d . . . C21 C 0.4561(2) 0.24262(14) 0.46299(11) 0.0228(4) Uani 1 1 d . . . C22 C 0.5724(2) 0.21984(16) 0.49040(13) 0.0301(5) Uani 1 1 d . . . H22A H 0.6381 0.2157 0.4617 0.036 Uiso 1 1 calc R . . C23 C 0.5929(2) 0.20323(19) 0.55898(13) 0.0373(6) Uani 1 1 d . . . H23A H 0.6727 0.1873 0.5768 0.045 Uiso 1 1 calc R . . C24 C 0.4997(3) 0.20931(19) 0.60203(14) 0.0407(6) Uani 1 1 d . . . H24A H 0.5150 0.1996 0.6494 0.049 Uiso 1 1 calc R . . C25 C 0.3842(3) 0.2297(2) 0.57495(15) 0.0479(7) Uani 1 1 d . . . H25A H 0.3189 0.2334 0.6039 0.057 Uiso 1 1 calc R . . C26 C 0.3619(2) 0.2447(2) 0.50681(14) 0.0391(6) Uani 1 1 d . . . H26A H 0.2809 0.2567 0.4891 0.047 Uiso 1 1 calc R . . C27 C 0.3807(3) 0.00497(18) 0.24845(15) 0.0489(8) Uani 1 1 d . . . H27A H 0.4419 -0.0231 0.2806 0.059 Uiso 1 1 calc R . . H27B H 0.4160 0.0144 0.2048 0.059 Uiso 1 1 calc R . . H27C H 0.3100 -0.0366 0.2423 0.059 Uiso 1 1 calc R . . C28 C 0.2610(2) 0.08271(18) 0.35780(14) 0.0381(6) Uani 1 1 d . . . H28A H 0.2215 0.1373 0.3765 0.046 Uiso 1 1 calc R . . H28B H 0.3231 0.0586 0.3913 0.046 Uiso 1 1 calc R . . H28C H 0.1999 0.0343 0.3469 0.046 Uiso 1 1 calc R . . C29 C 0.2036(3) 0.1495(2) 0.22489(16) 0.0499(8) Uani 1 1 d . . . H29A H 0.2283 0.1531 0.1783 0.060 Uiso 1 1 calc R . . H29B H 0.1736 0.2106 0.2385 0.060 Uiso 1 1 calc R . . H29C H 0.1386 0.1031 0.2274 0.060 Uiso 1 1 calc R . . C30 C 0.7224(2) 0.34446(17) 0.22609(13) 0.0319(5) Uani 1 1 d . . . H30A H 0.6805 0.3460 0.1808 0.038 Uiso 1 1 calc R . . H30B H 0.7713 0.2874 0.2312 0.038 Uiso 1 1 calc R . . H30C H 0.7759 0.3990 0.2321 0.038 Uiso 1 1 calc R . . C31 C 0.7054(2) 0.36494(17) 0.36684(12) 0.0308(5) Uani 1 1 d . . . H31A H 0.7577 0.3104 0.3759 0.037 Uiso 1 1 calc R . . H31B H 0.6534 0.3742 0.4046 0.037 Uiso 1 1 calc R . . H31C H 0.7563 0.4203 0.3618 0.037 Uiso 1 1 calc R . . C32 C 0.5364(2) 0.45771(15) 0.27399(14) 0.0320(5) Uani 1 1 d . . . H32A H 0.4801 0.4697 0.3094 0.038 Uiso 1 1 calc R . . H32B H 0.4909 0.4566 0.2296 0.038 Uiso 1 1 calc R . . H32C H 0.5980 0.5072 0.2746 0.038 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 0.02323(16) 0.01790(16) 0.01935(17) -0.00109(10) 0.00246(12) -0.00037(10) P1 0.0405(3) 0.0278(3) 0.0231(3) 0.0000(2) -0.0001(3) -0.0134(2) P2 0.0221(3) 0.0196(3) 0.0244(3) -0.0007(2) 0.0048(2) -0.0011(2) Cl1 0.0322(3) 0.0682(5) 0.0535(5) 0.0156(4) 0.0104(3) 0.0047(3) N1 0.0374(10) 0.0221(9) 0.0242(10) -0.0013(7) 0.0024(8) 0.0085(8) N2 0.0221(9) 0.0204(8) 0.0247(10) 0.0001(7) 0.0041(8) -0.0006(7) O1 0.0548(11) 0.0405(10) 0.0356(11) -0.0085(8) 0.0055(9) 0.0243(9) O2 0.0236(7) 0.0278(8) 0.0248(9) 0.0023(6) 0.0025(6) 0.0031(6) C1 0.0251(10) 0.0225(10) 0.0245(12) -0.0018(8) 0.0021(9) -0.0046(8) C2 0.0260(11) 0.0275(11) 0.0291(13) 0.0011(9) 0.0023(10) -0.0011(9) C3 0.0330(12) 0.0371(13) 0.0235(13) 0.0084(10) -0.0006(10) -0.0055(10) C4 0.0370(13) 0.0405(13) 0.0253(13) -0.0008(10) 0.0076(11) -0.0092(10) C5 0.0316(12) 0.0315(12) 0.0296(13) -0.0072(10) 0.0084(10) -0.0041(9) C6 0.0302(11) 0.0240(11) 0.0235(12) -0.0032(9) 0.0005(9) -0.0032(9) C7 0.0363(12) 0.0268(11) 0.0279(13) -0.0041(9) 0.0032(10) 0.0063(10) C8 0.0468(14) 0.0258(11) 0.0288(13) -0.0070(9) -0.0013(11) 0.0144(10) C9 0.0487(16) 0.0433(15) 0.0400(16) -0.0060(12) -0.0068(13) 0.0116(12) C10 0.0568(19) 0.063(2) 0.050(2) -0.0112(16) -0.0195(16) 0.0224(16) C11 0.084(2) 0.0515(18) 0.0385(18) -0.0047(14) -0.0185(17) 0.0329(17) C12 0.084(2) 0.0463(16) 0.0336(17) 0.0060(12) -0.0006(16) 0.0244(16) C13 0.0564(17) 0.0418(15) 0.0333(15) 0.0041(11) 0.0023(13) 0.0148(12) C14 0.0440(15) 0.0535(16) 0.0301(14) 0.0119(12) 0.0102(12) 0.0206(13) C15 0.0645(19) 0.076(2) 0.0294(16) 0.0102(15) 0.0150(15) 0.0420(18) C16 0.087(2) 0.068(2) 0.0315(17) -0.0047(15) 0.0046(17) 0.047(2) C17 0.085(2) 0.0476(17) 0.0339(17) -0.0090(13) -0.0038(16) 0.0258(16) C18 0.0618(17) 0.0349(13) 0.0320(15) 0.0012(11) 0.0124(13) 0.0213(12) C19 0.0416(13) 0.0362(13) 0.0245(13) 0.0058(10) 0.0083(11) 0.0146(11) C20 0.0224(10) 0.0267(11) 0.0220(12) 0.0007(9) 0.0052(9) -0.0010(8) C21 0.0277(11) 0.0209(10) 0.0199(11) -0.0007(8) 0.0011(9) -0.0006(8) C22 0.0258(11) 0.0317(12) 0.0329(14) 0.0018(9) 0.0035(10) -0.0008(9) C23 0.0333(13) 0.0490(15) 0.0284(14) 0.0068(11) -0.0069(11) -0.0033(11) C24 0.0528(16) 0.0471(15) 0.0215(13) 0.0046(11) -0.0015(12) 0.0010(12) C25 0.0475(16) 0.0660(19) 0.0319(15) 0.0157(13) 0.0157(13) 0.0157(14) C26 0.0290(12) 0.0529(15) 0.0363(15) 0.0147(12) 0.0080(11) 0.0101(11) C27 0.082(2) 0.0299(13) 0.0356(16) -0.0105(11) 0.0124(15) -0.0187(13) C28 0.0434(14) 0.0362(13) 0.0350(14) 0.0018(11) 0.0048(12) -0.0156(11) C29 0.0447(15) 0.0587(18) 0.0443(18) 0.0118(14) -0.0113(13) -0.0276(14) C30 0.0294(12) 0.0344(12) 0.0332(14) -0.0023(10) 0.0116(10) -0.0068(10) C31 0.0316(12) 0.0318(12) 0.0288(13) -0.0022(10) 0.0011(10) -0.0090(9) C32 0.0353(12) 0.0210(11) 0.0402(15) 0.0030(10) 0.0056(11) -0.0008(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Co1 C1 1.900(2) . ? Co1 N1 1.9394(18) . ? Co1 O2 1.9711(15) . ? Co1 N2 2.1180(19) . ? Co1 P1 2.2446(7) . ? Co1 P2 2.2538(7) . ? Co1 C20 2.420(2) . ? P1 C27 1.808(3) . ? P1 C29 1.809(3) . ? P1 C28 1.824(3) . ? P2 C32 1.810(2) . ? P2 C31 1.813(3) . ? P2 C30 1.813(2) . ? Cl1 C14 1.732(3) . ? N1 C7 1.358(3) . ? N1 C8 1.417(3) . ? N2 C20 1.304(3) . ? N2 C21 1.413(3) . ? O1 C7 1.242(3) . ? O2 C20 1.290(3) . ? C1 C6 1.395(3) . ? C1 C2 1.398(3) . ? C2 C3 1.393(3) . ? C3 C4 1.387(4) . ? C4 C5 1.387(4) . ? C5 C6 1.391(3) . ? C6 C7 1.476(3) . ? C8 C13 1.389(4) . ? C8 C9 1.399(4) . ? C9 C10 1.389(4) . ? C10 C11 1.377(5) . ? C11 C12 1.373(5) . ? C12 C13 1.390(4) . ? C14 C19 1.380(4) . ? C14 C15 1.396(4) . ? C15 C16 1.374(5) . ? C16 C17 1.388(5) . ? C17 C18 1.371(4) . ? C18 C19 1.436(4) . ? C19 C20 1.503(3) . ? C21 C22 1.394(3) . ? C21 C26 1.395(3) . ? C22 C23 1.380(4) . ? C23 C24 1.379(4) . ? C24 C25 1.375(4) . ? C25 C26 1.370(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 C1 Co1 N1 83.52(9) . . ? C1 Co1 O2 97.37(8) . . ? N1 Co1 O2 179.11(7) . . ? C1 Co1 N2 161.71(8) . . ? N1 Co1 N2 114.51(8) . . ? O2 Co1 N2 64.60(7) . . ? C1 Co1 P1 88.99(7) . . ? N1 Co1 P1 92.70(6) . . ? O2 Co1 P1 87.38(5) . . ? N2 Co1 P1 93.03(5) . . ? C1 Co1 P2 84.53(7) . . ? N1 Co1 P2 89.61(6) . . ? O2 Co1 P2 90.41(5) . . ? N2 Co1 P2 92.18(5) . . ? P1 Co1 P2 172.84(3) . . ? C1 Co1 C20 129.28(9) . . ? N1 Co1 C20 146.98(8) . . ? O2 Co1 C20 32.13(7) . . ? N2 Co1 C20 32.53(7) . . ? P1 Co1 C20 91.76(6) . . ? P2 Co1 C20 89.99(5) . . ? C27 P1 C29 104.46(16) . . ? C27 P1 C28 102.61(13) . . ? C29 P1 C28 102.28(14) . . ? C27 P1 Co1 116.50(11) . . ? C29 P1 Co1 112.57(9) . . ? C28 P1 Co1 116.69(9) . . ? C32 P2 C31 103.80(12) . . ? C32 P2 C30 102.44(12) . . ? C31 P2 C30 102.03(12) . . ? C32 P2 Co1 112.20(8) . . ? C31 P2 Co1 115.75(8) . . ? C30 P2 Co1 118.72(8) . . ? C7 N1 C8 118.38(19) . . ? C7 N1 Co1 116.19(16) . . ? C8 N1 Co1 125.43(15) . . ? C20 N2 C21 123.31(18) . . ? C20 N2 Co1 86.60(14) . . ? C21 N2 Co1 150.05(14) . . ? C20 O2 Co1 93.48(13) . . ? C6 C1 C2 118.6(2) . . ? C6 C1 Co1 113.98(17) . . ? C2 C1 Co1 127.17(17) . . ? C3 C2 C1 119.6(2) . . ? C4 C3 C2 121.2(2) . . ? C5 C4 C3 119.6(2) . . ? C4 C5 C6 119.4(2) . . ? C5 C6 C1 121.6(2) . . ? C5 C6 C7 123.4(2) . . ? C1 C6 C7 114.9(2) . . ? O1 C7 N1 125.9(2) . . ? O1 C7 C6 122.8(2) . . ? N1 C7 C6 111.26(19) . . ? C13 C8 C9 118.3(3) . . ? C13 C8 N1 121.0(2) . . ? C9 C8 N1 120.8(2) . . ? C10 C9 C8 120.1(3) . . ? C11 C10 C9 120.9(3) . . ? C12 C11 C10 119.3(3) . . ? C11 C12 C13 120.5(3) . . ? C8 C13 C12 120.8(3) . . ? C19 C14 C15 121.1(3) . . ? C19 C14 Cl1 120.2(2) . . ? C15 C14 Cl1 118.7(2) . . ? C16 C15 C14 119.1(3) . . ? C15 C16 C17 121.1(3) . . ? C18 C17 C16 120.5(3) . . ? C17 C18 C19 119.2(3) . . ? C14 C19 C18 118.8(2) . . ? C14 C19 C20 123.6(3) . . ? C18 C19 C20 117.3(2) . . ? O2 C20 N2 115.09(19) . . ? O2 C20 C19 117.30(19) . . ? N2 C20 C19 127.0(2) . . ? O2 C20 Co1 54.38(10) . . ? N2 C20 Co1 60.87(12) . . ? C19 C20 Co1 166.15(16) . . ? C22 C21 C26 117.6(2) . . ? C22 C21 N2 119.7(2) . . ? C26 C21 N2 122.6(2) . . ? C23 C22 C21 120.4(2) . . ? C24 C23 C22 121.2(2) . . ? C25 C24 C23 118.5(3) . . ? C26 C25 C24 121.0(3) . . ? C25 C26 C21 121.1(2) . . ? _diffrn_measured_fraction_theta_max 0.963 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.963 _refine_diff_density_max 0.595 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.054 # Attachment '- 9.cif' data_sun12a _database_code_depnum_ccdc_archive 'CCDC 806084' #TrackingRef '- 9.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H30 Cl N Ni O P2' _chemical_formula_sum 'C20 H30 Cl N Ni O P2' _chemical_formula_weight 456.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 13.506(3) _cell_length_b 14.564(3) _cell_length_c 12.115(2) _cell_angle_alpha 90.00 _cell_angle_beta 106.80(3) _cell_angle_gamma 90.00 _cell_volume 2281.3(8) _cell_formula_units_Z 4 _cell_measurement_temperature 423(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 960 _exptl_absorpt_coefficient_mu 1.117 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 423(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10503 _diffrn_reflns_av_R_equivalents 0.0606 _diffrn_reflns_av_sigmaI/netI 0.0510 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 26.70 _reflns_number_total 4832 _reflns_number_gt 3752 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4562 _refine_ls_number_parameters 278 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0517 _refine_ls_R_factor_gt 0.0424 _refine_ls_wR_factor_ref 0.1174 _refine_ls_wR_factor_gt 0.1107 _refine_ls_goodness_of_fit_ref 0.825 _refine_ls_restrained_S_all 0.825 _refine_ls_shift/su_max 0.144 _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 Ni1 Ni -0.279430(18) 0.357029(18) -0.15180(2) 0.02212(12) Uani 1 1 d . . . P1 P -0.44408(4) 0.35874(4) -0.15934(6) 0.02924(17) Uani 1 1 d . . . P2 P -0.11716(4) 0.35873(4) -0.15445(6) 0.02433(16) Uani 1 1 d . . . Cl1 Cl -0.25208(5) 0.22761(4) -0.05238(6) 0.03922(18) Uani 1 1 d . . . O1 O -0.26340(15) 0.67872(11) -0.09634(17) 0.0395(4) Uani 1 1 d . . . N1 N -0.25536(15) 0.53553(13) -0.02109(18) 0.0270(4) Uani 1 1 d . . . C1 C -0.4761(2) 0.3184(2) -0.0323(3) 0.0446(7) Uani 1 1 d . . . H1A H -0.4423 0.3563 0.0324 0.067 Uiso 1 1 calc R . . H1B H -0.4534 0.2560 -0.0167 0.067 Uiso 1 1 calc R . . H1C H -0.5496 0.3215 -0.0455 0.067 Uiso 1 1 calc R . . C2 C -0.5119(2) 0.2805(3) -0.2720(3) 0.0603(9) Uani 1 1 d . . . H2A H -0.4855 0.2195 -0.2534 0.090 Uiso 1 1 calc R . . H2B H -0.5018 0.2991 -0.3440 0.090 Uiso 1 1 calc R . . H2C H -0.5844 0.2814 -0.2783 0.090 Uiso 1 1 calc R . . C3 C -0.5180(2) 0.4640(2) -0.1952(3) 0.0559(9) Uani 1 1 d . . . H3A H -0.5891 0.4520 -0.2005 0.084 Uiso 1 1 calc R . . H3B H -0.5132 0.4868 -0.2678 0.084 Uiso 1 1 calc R . . H3C H -0.4909 0.5089 -0.1362 0.084 Uiso 1 1 calc R . . C4 C -0.07144(18) 0.45274(19) -0.2244(3) 0.0417(7) Uani 1 1 d . . . H4A H 0.0012 0.4454 -0.2148 0.062 Uiso 1 1 calc R . . H4B H -0.0831 0.5098 -0.1905 0.062 Uiso 1 1 calc R . . H4C H -0.1082 0.4529 -0.3051 0.062 Uiso 1 1 calc R . . C5 C -0.0843(2) 0.25950(19) -0.2264(3) 0.0420(7) Uani 1 1 d . . . H5A H -0.1264 0.2586 -0.3052 0.063 Uiso 1 1 calc R . . H5B H -0.0964 0.2047 -0.1882 0.063 Uiso 1 1 calc R . . H5C H -0.0127 0.2626 -0.2239 0.063 Uiso 1 1 calc R . . C6 C -0.02649(19) 0.3566(2) -0.0112(3) 0.0473(8) Uani 1 1 d . . . H6A H -0.0368 0.3018 0.0280 0.071 Uiso 1 1 calc R . . H6B H -0.0376 0.4094 0.0313 0.071 Uiso 1 1 calc R . . H6C H 0.0429 0.3577 -0.0170 0.071 Uiso 1 1 calc R . . C7 C -0.30558(15) 0.45883(15) -0.2535(2) 0.0239(5) Uani 1 1 d . . . C8 C -0.33226(17) 0.43249(18) -0.3699(2) 0.0306(5) Uani 1 1 d . . . C9 C -0.35233(19) 0.4960(2) -0.4586(3) 0.0392(6) Uani 1 1 d . . . C10 C -0.3461(2) 0.5891(2) -0.4336(2) 0.0414(6) Uani 1 1 d . . . C11 C -0.31983(18) 0.61742(18) -0.3201(2) 0.0326(5) Uani 1 1 d . . . C12 C -0.29981(15) 0.55365(15) -0.2294(2) 0.0256(5) Uani 1 1 d . . . C13 C -0.27154(15) 0.59559(15) -0.1108(2) 0.0247(5) Uani 1 1 d . . . C14 C -0.22661(15) 0.55410(14) 0.0988(2) 0.0239(4) Uani 1 1 d . . . C15 C -0.20974(17) 0.64166(15) 0.1457(2) 0.0269(5) Uani 1 1 d . . . C16 C -0.17789(17) 0.65278(16) 0.2646(2) 0.0297(5) Uani 1 1 d . . . C17 C -0.16165(16) 0.57819(17) 0.3393(2) 0.0294(5) Uani 1 1 d . . . C18 C -0.18224(17) 0.49086(17) 0.2910(2) 0.0298(5) Uani 1 1 d . . . C19 C -0.21372(16) 0.47846(16) 0.1725(2) 0.0267(5) Uani 1 1 d . . . C20 C -0.1204(2) 0.5923(2) 0.4677(2) 0.0436(6) Uani 1 1 d . . . H20A H -0.1371 0.5399 0.5069 0.065 Uiso 1 1 calc R . . H20B H -0.1511 0.6462 0.4893 0.065 Uiso 1 1 calc R . . H20C H -0.0467 0.5997 0.4885 0.065 Uiso 1 1 calc R . . H19 H -0.2267(19) 0.420(2) 0.141(2) 0.030(7) Uiso 1 1 d . . . H11 H -0.312(2) 0.677(2) -0.300(3) 0.044(8) Uiso 1 1 d . . . H16 H -0.167(2) 0.7121(18) 0.298(2) 0.029(6) Uiso 1 1 d . . . H10 H -0.360(3) 0.632(2) -0.495(3) 0.055(10) Uiso 1 1 d . . . H18 H -0.175(2) 0.4387(18) 0.339(2) 0.029(7) Uiso 1 1 d . . . H8 H -0.334(2) 0.3716(19) -0.388(3) 0.032(7) Uiso 1 1 d . . . H15 H -0.217(2) 0.690(2) 0.103(3) 0.033(7) Uiso 1 1 d . . . H1 H -0.269(2) 0.479(2) -0.042(3) 0.038(8) Uiso 1 1 d . . . H9 H -0.367(2) 0.476(2) -0.535(3) 0.047(9) Uiso 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 Ni1 0.01705(16) 0.02664(17) 0.0234(2) -0.00099(10) 0.00690(12) -0.00147(9) P1 0.0181(3) 0.0439(4) 0.0268(4) -0.0004(2) 0.0081(2) -0.0035(2) P2 0.0170(3) 0.0301(3) 0.0261(4) 0.0002(2) 0.0065(2) -0.00034(18) Cl1 0.0382(3) 0.0358(3) 0.0492(4) 0.0135(3) 0.0215(3) 0.0040(2) O1 0.0531(11) 0.0283(8) 0.0313(11) 0.0019(7) 0.0031(8) -0.0009(8) N1 0.0325(9) 0.0234(9) 0.0233(11) -0.0003(7) 0.0050(8) 0.0004(7) C1 0.0325(12) 0.0728(19) 0.0333(17) 0.0043(13) 0.0170(11) 0.0021(12) C2 0.0395(15) 0.099(3) 0.043(2) -0.0207(17) 0.0121(13) -0.0333(16) C3 0.0284(13) 0.0682(19) 0.076(2) 0.0196(17) 0.0235(14) 0.0144(13) C4 0.0235(11) 0.0457(14) 0.059(2) 0.0163(13) 0.0166(11) 0.0011(10) C5 0.0346(12) 0.0434(14) 0.0536(19) -0.0127(12) 0.0218(12) -0.0022(11) C6 0.0242(12) 0.080(2) 0.0351(17) -0.0015(13) 0.0041(11) -0.0034(11) C7 0.0152(9) 0.0339(11) 0.0228(12) 0.0020(8) 0.0055(8) 0.0003(7) C8 0.0246(10) 0.0412(13) 0.0258(13) -0.0033(10) 0.0067(9) -0.0018(9) C9 0.0337(12) 0.0597(16) 0.0221(15) 0.0003(11) 0.0047(10) 0.0039(11) C10 0.0438(14) 0.0523(15) 0.0261(15) 0.0135(12) 0.0071(11) 0.0104(12) C11 0.0295(11) 0.0371(12) 0.0302(14) 0.0089(10) 0.0068(9) 0.0069(10) C12 0.0185(9) 0.0346(11) 0.0228(12) 0.0033(9) 0.0042(8) 0.0025(8) C13 0.0187(9) 0.0285(10) 0.0257(13) 0.0030(9) 0.0043(8) 0.0015(8) C14 0.0179(9) 0.0314(10) 0.0221(12) 0.0007(9) 0.0055(8) 0.0018(8) C15 0.0257(10) 0.0297(12) 0.0253(14) 0.0013(9) 0.0075(9) 0.0039(8) C16 0.0258(11) 0.0336(12) 0.0310(14) -0.0074(10) 0.0102(9) 0.0008(8) C17 0.0233(10) 0.0435(12) 0.0235(13) -0.0008(9) 0.0100(8) 0.0044(9) C18 0.0269(10) 0.0372(12) 0.0257(14) 0.0074(10) 0.0083(9) 0.0028(9) C19 0.0237(10) 0.0279(11) 0.0288(13) 0.0013(9) 0.0081(8) -0.0008(8) C20 0.0440(14) 0.0562(16) 0.0294(16) -0.0031(12) 0.0083(11) 0.0028(12) _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 C7 1.895(2) . ? Ni1 P1 2.1992(8) . ? Ni1 P2 2.2012(7) . ? Ni1 Cl1 2.2096(7) . ? P1 C3 1.812(3) . ? P1 C1 1.812(3) . ? P1 C2 1.811(3) . ? P2 C5 1.808(3) . ? P2 C6 1.812(3) . ? P2 C4 1.810(3) . ? O1 C13 1.224(3) . ? N1 C13 1.363(3) . ? N1 C14 1.417(3) . ? C7 C8 1.403(3) . ? C7 C12 1.409(3) . ? C8 C9 1.385(4) . ? C9 C10 1.386(4) . ? C10 C11 1.379(4) . ? C11 C12 1.404(3) . ? C12 C13 1.505(3) . ? C14 C19 1.397(3) . ? C14 C15 1.388(3) . ? C15 C16 1.389(4) . ? C16 C17 1.390(4) . ? C17 C18 1.394(4) . ? C17 C20 1.507(4) . ? C18 C19 1.386(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 C7 Ni1 P1 88.17(7) . . ? C7 Ni1 P2 88.91(7) . . ? P1 Ni1 P2 176.66(3) . . ? C7 Ni1 Cl1 172.91(7) . . ? P1 Ni1 Cl1 92.29(3) . . ? P2 Ni1 Cl1 90.42(3) . . ? C3 P1 C1 103.13(16) . . ? C3 P1 C2 103.17(18) . . ? C1 P1 C2 104.05(16) . . ? C3 P1 Ni1 120.01(10) . . ? C1 P1 Ni1 116.61(9) . . ? C2 P1 Ni1 108.04(11) . . ? C5 P2 C6 104.85(15) . . ? C5 P2 C4 102.39(15) . . ? C6 P2 C4 103.51(14) . . ? C5 P2 Ni1 112.46(9) . . ? C6 P2 Ni1 112.70(10) . . ? C4 P2 Ni1 119.42(8) . . ? C13 N1 C14 128.93(19) . . ? C8 C7 C12 117.3(2) . . ? C8 C7 Ni1 112.63(17) . . ? C12 C7 Ni1 130.03(18) . . ? C9 C8 C7 122.2(2) . . ? C10 C9 C8 119.8(3) . . ? C9 C10 C11 119.5(3) . . ? C10 C11 C12 121.2(2) . . ? C11 C12 C7 120.0(2) . . ? C11 C12 C13 114.6(2) . . ? C7 C12 C13 125.4(2) . . ? O1 C13 N1 122.2(2) . . ? O1 C13 C12 121.7(2) . . ? N1 C13 C12 116.04(19) . . ? C19 C14 C15 119.2(2) . . ? C19 C14 N1 116.8(2) . . ? C15 C14 N1 124.0(2) . . ? C14 C15 C16 119.8(2) . . ? C17 C16 C15 121.8(2) . . ? C16 C17 C18 117.7(2) . . ? C16 C17 C20 120.5(2) . . ? C18 C17 C20 121.8(2) . . ? C19 C18 C17 121.2(2) . . ? C18 C19 C14 120.2(2) . . ? _diffrn_measured_fraction_theta_max 0.945 _diffrn_reflns_theta_full 26.70 _diffrn_measured_fraction_theta_full 0.945 _refine_diff_density_max 0.728 _refine_diff_density_min -1.110 _refine_diff_density_rms 0.089 # Attachment '- 12.cif' data_12 _database_code_depnum_ccdc_archive 'CCDC 806085' #TrackingRef '- 12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C34 H40 Cl Co N2 O2 P2' _chemical_formula_weight 665.00 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' Co Co 0.3494 0.9721 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 9.9389(6) _cell_length_b 28.7709(17) _cell_length_c 11.8115(7) _cell_angle_alpha 90.00 _cell_angle_beta 98.1320(10) _cell_angle_gamma 90.00 _cell_volume 3343.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.721 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min 0.8872 _exptl_absorpt_correction_T_max 0.9249 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17944 _diffrn_reflns_av_R_equivalents 0.0400 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6570 _reflns_number_gt 4917 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1181P)^2^+9.4235P] 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 6570 _refine_ls_number_parameters 387 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0897 _refine_ls_R_factor_gt 0.0675 _refine_ls_wR_factor_ref 0.2143 _refine_ls_wR_factor_gt 0.1945 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.5053(4) 0.12277(15) 0.9676(4) 0.0212(9) Uani 1 1 d . . . C2 C 0.3972(5) 0.10348(16) 0.8936(4) 0.0266(10) Uani 1 1 d . . . H2 H 0.4136 0.0897 0.8256 0.032 Uiso 1 1 calc R . . C3 C 0.2657(5) 0.10469(17) 0.9208(4) 0.0311(11) Uani 1 1 d . . . H3 H 0.1953 0.0914 0.8710 0.037 Uiso 1 1 calc R . . C4 C 0.2377(5) 0.12531(18) 1.0209(5) 0.0331(11) Uani 1 1 d . . . H4 H 0.1490 0.1269 1.0373 0.040 Uiso 1 1 calc R . . C5 C 0.3445(5) 0.14360(17) 1.0963(4) 0.0291(10) Uani 1 1 d . . . H5 H 0.3275 0.1572 1.1644 0.035 Uiso 1 1 calc R . . C6 C 0.4760(5) 0.14179(15) 1.0709(4) 0.0234(9) Uani 1 1 d . . . C7 C 0.5936(5) 0.15972(15) 1.1486(4) 0.0231(9) Uani 1 1 d . . . C8 C 0.8358(4) 0.16778(15) 1.1684(4) 0.0238(9) Uani 1 1 d . . . C9 C 0.8684(5) 0.15588(18) 1.2834(4) 0.0321(11) Uani 1 1 d . . . H9 H 0.8079 0.1381 1.3183 0.038 Uiso 1 1 calc R . . C10 C 0.9892(6) 0.1701(2) 1.3463(5) 0.0401(13) Uani 1 1 d . . . H10 H 1.0081 0.1617 1.4229 0.048 Uiso 1 1 calc R . . C11 C 1.0834(5) 0.1967(2) 1.2981(5) 0.0396(13) Uani 1 1 d . . . C12 C 1.0520(5) 0.20768(19) 1.1830(5) 0.0361(12) Uani 1 1 d . . . H12 H 1.1139 0.2249 1.1482 0.043 Uiso 1 1 calc R . . C13 C 0.9316(5) 0.19376(17) 1.1182(4) 0.0286(10) Uani 1 1 d . . . H13 H 0.9141 0.2016 1.0411 0.034 Uiso 1 1 calc R . . C14 C 1.2128(6) 0.2132(3) 1.3687(6) 0.0593(18) Uani 1 1 d . . . H14A H 1.2670 0.2296 1.3206 0.089 Uiso 1 1 calc R . . H14B H 1.2628 0.1869 1.4026 0.089 Uiso 1 1 calc R . . H14C H 1.1912 0.2336 1.4279 0.089 Uiso 1 1 calc R . . C15 C 0.9465(6) 0.1129(3) 0.7257(5) 0.0539(18) Uani 1 1 d . . . C16 C 1.0366(6) 0.1565(3) 0.7165(5) 0.059(2) Uani 1 1 d . . . H16 H 1.0211 0.1840 0.7540 0.071 Uiso 1 1 calc R . . C17 C 1.1359(8) 0.1531(4) 0.6536(7) 0.081(3) Uani 1 1 d . . . H17 H 1.1907 0.1787 0.6456 0.097 Uiso 1 1 calc R . . C18 C 1.1593(10) 0.1122(5) 0.5999(7) 0.090(3) Uani 1 1 d . . . H18 H 1.2307 0.1115 0.5569 0.108 Uiso 1 1 calc R . . C19 C 1.0888(10) 0.0744(5) 0.6048(7) 0.089(3) Uani 1 1 d . . . H19 H 1.1100 0.0472 0.5687 0.107 Uiso 1 1 calc R . . C20 C 0.9735(9) 0.0768(3) 0.6706(7) 0.072(2) Uani 1 1 d . . . C21 C 0.8429(5) 0.11740(17) 0.8072(4) 0.0285(10) Uani 1 1 d . . . C22 C 0.6382(5) 0.09685(16) 0.6804(4) 0.0266(10) Uani 1 1 d . . . C23 C 0.6476(5) 0.12395(17) 0.5847(4) 0.0308(11) Uani 1 1 d . . . H23 H 0.7092 0.1485 0.5896 0.037 Uiso 1 1 calc R . . C24 C 0.5658(6) 0.11475(19) 0.4814(4) 0.0347(12) Uani 1 1 d . . . H24 H 0.5741 0.1334 0.4184 0.042 Uiso 1 1 calc R . . C25 C 0.4727(5) 0.07874(19) 0.4696(4) 0.0335(11) Uani 1 1 d . . . C26 C 0.4666(5) 0.05107(18) 0.5656(4) 0.0327(11) Uani 1 1 d . . . H26 H 0.4068 0.0260 0.5598 0.039 Uiso 1 1 calc R . . C27 C 0.5457(5) 0.05951(16) 0.6686(4) 0.0275(10) Uani 1 1 d . . . H27 H 0.5382 0.0404 0.7309 0.033 Uiso 1 1 calc R . . C28 C 0.3811(7) 0.0705(2) 0.3590(5) 0.0487(15) Uani 1 1 d . . . H28A H 0.3002 0.0889 0.3574 0.073 Uiso 1 1 calc R . . H28B H 0.3571 0.0382 0.3527 0.073 Uiso 1 1 calc R . . H28C H 0.4274 0.0792 0.2962 0.073 Uiso 1 1 calc R . . C29 C 0.5974(6) 0.24482(17) 0.9721(4) 0.0360(12) Uani 1 1 d . . . H29A H 0.5765 0.2734 0.9314 0.054 Uiso 1 1 calc R . . H29B H 0.6757 0.2492 1.0288 0.054 Uiso 1 1 calc R . . H29C H 0.5213 0.2357 1.0089 0.054 Uiso 1 1 calc R . . C30 C 0.4818(5) 0.20212(17) 0.7659(4) 0.0317(11) Uani 1 1 d . . . H30A H 0.4737 0.2325 0.7321 0.048 Uiso 1 1 calc R . . H30B H 0.4029 0.1957 0.8017 0.048 Uiso 1 1 calc R . . H30C H 0.4890 0.1794 0.7076 0.048 Uiso 1 1 calc R . . C31 C 0.7596(5) 0.22713(18) 0.7969(5) 0.0342(11) Uani 1 1 d . . . H31A H 0.7730 0.2085 0.7320 0.051 Uiso 1 1 calc R . . H31B H 0.8439 0.2298 0.8474 0.051 Uiso 1 1 calc R . . H31C H 0.7287 0.2575 0.7715 0.051 Uiso 1 1 calc R . . C32 C 0.6670(6) 0.04721(19) 1.1581(5) 0.0400(13) Uani 1 1 d . . . H32A H 0.5707 0.0525 1.1440 0.060 Uiso 1 1 calc R . . H32B H 0.7069 0.0670 1.2193 0.060 Uiso 1 1 calc R . . H32C H 0.6844 0.0153 1.1790 0.060 Uiso 1 1 calc R . . C33 C 0.9216(6) 0.0518(2) 1.0769(6) 0.0439(14) Uani 1 1 d . . . H33A H 0.9359 0.0220 1.1130 0.066 Uiso 1 1 calc R . . H33B H 0.9543 0.0757 1.1304 0.066 Uiso 1 1 calc R . . H33C H 0.9699 0.0532 1.0121 0.066 Uiso 1 1 calc R . . C34 C 0.6942(7) 0.01008(19) 0.9420(5) 0.0483(16) Uani 1 1 d . . . H34A H 0.7184 -0.0176 0.9855 0.072 Uiso 1 1 calc R . . H34B H 0.7413 0.0107 0.8765 0.072 Uiso 1 1 calc R . . H34C H 0.5979 0.0104 0.9173 0.072 Uiso 1 1 calc R . . Cl1 Cl 0.8967(4) 0.02741(13) 0.6796(3) 0.1277(11) Uani 1 1 d . . . Co Co 0.69192(6) 0.129701(19) 0.94792(5) 0.01877(19) Uani 1 1 d . . . N1 N 0.7104(4) 0.15483(12) 1.1030(3) 0.0214(8) Uani 1 1 d . . . N2 N 0.7127(4) 0.10732(13) 0.7891(3) 0.0241(8) Uani 1 1 d . . . O1 O 0.5818(3) 0.17718(12) 1.2441(3) 0.0314(8) Uani 1 1 d . . . O2 O 0.8855(3) 0.13368(12) 0.9064(3) 0.0274(7) Uani 1 1 d . . . P1 P 0.74092(12) 0.06025(4) 1.02976(10) 0.0242(3) Uani 1 1 d . . . P2 P 0.63274(12) 0.19978(4) 0.87245(10) 0.0229(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 0.022(2) 0.019(2) 0.023(2) 0.0036(17) 0.0032(18) 0.0021(16) C2 0.027(2) 0.026(2) 0.026(2) 0.0023(19) 0.0012(19) -0.0028(19) C3 0.023(2) 0.033(3) 0.036(3) 0.004(2) -0.001(2) -0.003(2) C4 0.017(2) 0.038(3) 0.046(3) 0.006(2) 0.009(2) 0.0007(19) C5 0.026(2) 0.032(3) 0.031(2) 0.001(2) 0.008(2) 0.004(2) C6 0.026(2) 0.021(2) 0.024(2) 0.0044(17) 0.0052(18) 0.0006(17) C7 0.025(2) 0.020(2) 0.025(2) 0.0018(17) 0.0060(18) 0.0012(17) C8 0.022(2) 0.022(2) 0.027(2) -0.0041(18) 0.0017(18) 0.0016(17) C9 0.030(3) 0.035(3) 0.031(3) 0.002(2) 0.004(2) -0.004(2) C10 0.038(3) 0.049(3) 0.030(3) 0.002(2) -0.006(2) -0.002(2) C11 0.030(3) 0.044(3) 0.043(3) -0.009(3) -0.002(2) -0.006(2) C12 0.030(3) 0.039(3) 0.041(3) -0.007(2) 0.009(2) -0.007(2) C13 0.027(2) 0.032(3) 0.027(2) -0.003(2) 0.0039(19) -0.005(2) C14 0.037(3) 0.083(5) 0.054(4) -0.010(4) -0.006(3) -0.021(3) C15 0.031(3) 0.109(6) 0.023(3) 0.005(3) 0.006(2) 0.030(3) C16 0.023(3) 0.121(6) 0.033(3) 0.005(3) -0.001(2) 0.015(3) C17 0.045(4) 0.138(8) 0.060(5) 0.033(5) 0.010(4) 0.014(5) C18 0.071(6) 0.143(10) 0.057(5) 0.019(6) 0.018(4) 0.054(6) C19 0.075(6) 0.145(10) 0.049(4) 0.017(5) 0.017(4) 0.054(6) C20 0.084(6) 0.070(5) 0.064(5) 0.000(4) 0.012(4) 0.023(4) C21 0.029(3) 0.033(3) 0.025(2) 0.005(2) 0.008(2) 0.007(2) C22 0.029(2) 0.028(2) 0.022(2) -0.0048(19) 0.0036(19) 0.0054(19) C23 0.033(3) 0.030(3) 0.030(3) -0.001(2) 0.006(2) 0.001(2) C24 0.043(3) 0.037(3) 0.025(2) 0.001(2) 0.007(2) 0.008(2) C25 0.037(3) 0.039(3) 0.024(2) -0.006(2) 0.003(2) 0.009(2) C26 0.033(3) 0.033(3) 0.033(3) -0.007(2) 0.005(2) 0.003(2) C27 0.033(3) 0.025(2) 0.025(2) 0.0008(18) 0.0052(19) 0.0065(19) C28 0.057(4) 0.054(4) 0.032(3) -0.008(3) -0.004(3) 0.004(3) C29 0.050(3) 0.023(2) 0.035(3) -0.001(2) 0.005(2) 0.007(2) C30 0.034(3) 0.028(2) 0.033(3) 0.009(2) 0.002(2) 0.007(2) C31 0.034(3) 0.030(3) 0.040(3) 0.010(2) 0.009(2) -0.001(2) C32 0.052(3) 0.032(3) 0.038(3) 0.012(2) 0.011(3) 0.001(2) C33 0.032(3) 0.040(3) 0.058(4) 0.015(3) 0.002(3) 0.011(2) C34 0.081(5) 0.024(3) 0.036(3) 0.001(2) -0.003(3) 0.001(3) Cl1 0.121(3) 0.129(3) 0.136(3) -0.004(2) 0.031(2) 0.018(2) Co 0.0183(3) 0.0182(3) 0.0202(3) 0.0011(2) 0.0040(2) 0.0003(2) N1 0.0219(19) 0.0212(18) 0.0214(18) -0.0013(14) 0.0044(15) -0.0006(14) N2 0.025(2) 0.026(2) 0.0216(19) -0.0007(15) 0.0045(15) 0.0024(16) O1 0.0304(18) 0.0374(19) 0.0279(18) -0.0062(15) 0.0099(14) -0.0038(14) O2 0.0208(16) 0.0375(19) 0.0246(17) 0.0044(14) 0.0060(13) -0.0010(13) P1 0.0257(6) 0.0200(6) 0.0268(6) 0.0034(5) 0.0034(5) 0.0013(4) P2 0.0259(6) 0.0190(6) 0.0245(6) 0.0030(4) 0.0055(5) 0.0020(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 C1 C2 1.399(6) . ? C1 C6 1.405(6) . ? C1 Co 1.912(4) . ? C2 C3 1.390(7) . ? C2 H2 0.9300 . ? C3 C4 1.385(7) . ? C3 H3 0.9300 . ? C4 C5 1.389(7) . ? C4 H4 0.9300 . ? C5 C6 1.383(6) . ? C5 H5 0.9300 . ? C6 C7 1.473(6) . ? C7 O1 1.255(5) . ? C7 N1 1.355(6) . ? C8 C9 1.393(7) . ? C8 C13 1.406(7) . ? C8 N1 1.420(6) . ? C9 C10 1.381(7) . ? C9 H9 0.9300 . ? C10 C11 1.391(8) . ? C10 H10 0.9300 . ? C11 C12 1.388(8) . ? C11 C14 1.507(7) . ? C12 C13 1.385(7) . ? C12 H12 0.9300 . ? C13 H13 0.9300 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 C20 1.273(10) . ? C15 C21 1.511(7) . ? C15 C16 1.555(11) . ? C16 C17 1.320(9) . ? C16 H16 0.9300 . ? C17 C18 1.371(14) . ? C17 H17 0.9300 . ? C18 C19 1.300(14) . ? C18 H18 0.9300 . ? C19 C20 1.474(12) . ? C19 H19 0.9300 . ? C20 Cl1 1.624(10) . ? C21 O2 1.278(6) . ? C21 N2 1.314(6) . ? C22 C23 1.388(7) . ? C22 C27 1.408(7) . ? C22 N2 1.420(6) . ? C23 C24 1.392(7) . ? C23 H23 0.9300 . ? C24 C25 1.383(8) . ? C24 H24 0.9300 . ? C25 C26 1.394(7) . ? C25 C28 1.502(7) . ? C26 C27 1.374(7) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 P2 1.818(5) . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 P2 1.818(5) . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 P2 1.823(5) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 P1 1.815(5) . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 P1 1.820(5) . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 P1 1.799(6) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? Co N1 1.953(4) . ? Co N2 2.021(4) . ? Co O2 2.055(3) . ? Co P1 2.2430(13) . ? Co P2 2.2489(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 C2 C1 C6 117.5(4) . . ? C2 C1 Co 129.6(3) . . ? C6 C1 Co 112.8(3) . . ? C3 C2 C1 120.6(4) . . ? C3 C2 H2 119.7 . . ? C1 C2 H2 119.7 . . ? C4 C3 C2 121.1(5) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 118.8(4) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C6 C5 C4 120.4(5) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C1 121.4(4) . . ? C5 C6 C7 122.8(4) . . ? C1 C6 C7 115.8(4) . . ? O1 C7 N1 126.4(4) . . ? O1 C7 C6 122.3(4) . . ? N1 C7 C6 111.4(4) . . ? C9 C8 C13 117.6(4) . . ? C9 C8 N1 122.1(4) . . ? C13 C8 N1 120.3(4) . . ? C10 C9 C8 121.1(5) . . ? C10 C9 H9 119.5 . . ? C8 C9 H9 119.5 . . ? C9 C10 C11 121.8(5) . . ? C9 C10 H10 119.1 . . ? C11 C10 H10 119.1 . . ? C12 C11 C10 117.1(5) . . ? C12 C11 C14 121.7(5) . . ? C10 C11 C14 121.2(5) . . ? C13 C12 C11 122.2(5) . . ? C13 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C12 C13 C8 120.3(5) . . ? C12 C13 H13 119.9 . . ? C8 C13 H13 119.9 . . ? C11 C14 H14A 109.5 . . ? C11 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C11 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C20 C15 C21 127.5(8) . . ? C20 C15 C16 117.2(6) . . ? C21 C15 C16 115.2(6) . . ? C17 C16 C15 117.6(8) . . ? C17 C16 H16 121.2 . . ? C15 C16 H16 121.2 . . ? C16 C17 C18 120.9(10) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C19 C18 C17 124.7(9) . . ? C19 C18 H18 117.6 . . ? C17 C18 H18 117.6 . . ? C18 C19 C20 116.6(10) . . ? C18 C19 H19 121.7 . . ? C20 C19 H19 121.7 . . ? C15 C20 C19 122.9(9) . . ? C15 C20 Cl1 123.0(7) . . ? C19 C20 Cl1 113.7(7) . . ? O2 C21 N2 114.9(4) . . ? O2 C21 C15 116.7(5) . . ? N2 C21 C15 128.5(5) . . ? C23 C22 C27 117.8(4) . . ? C23 C22 N2 122.0(4) . . ? C27 C22 N2 120.1(4) . . ? C22 C23 C24 120.6(5) . . ? C22 C23 H23 119.7 . . ? C24 C23 H23 119.7 . . ? C25 C24 C23 122.0(5) . . ? C25 C24 H24 119.0 . . ? C23 C24 H24 119.0 . . ? C24 C25 C26 116.8(5) . . ? C24 C25 C28 121.4(5) . . ? C26 C25 C28 121.8(5) . . ? C27 C26 C25 122.3(5) . . ? C27 C26 H26 118.9 . . ? C25 C26 H26 118.9 . . ? C26 C27 C22 120.5(5) . . ? C26 C27 H27 119.8 . . ? C22 C27 H27 119.8 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? P2 C29 H29A 109.5 . . ? P2 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? P2 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? P2 C30 H30A 109.5 . . ? P2 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? P2 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? P2 C31 H31A 109.5 . . ? P2 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? P2 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? P1 C32 H32A 109.5 . . ? P1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? P1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? P1 C33 H33A 109.5 . . ? P1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? P1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? P1 C34 H34A 109.5 . . ? P1 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? P1 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C1 Co N1 83.64(17) . . ? C1 Co N2 107.91(17) . . ? N1 Co N2 168.41(16) . . ? C1 Co O2 172.71(16) . . ? N1 Co O2 103.65(14) . . ? N2 Co O2 64.80(14) . . ? C1 Co P1 90.58(13) . . ? N1 Co P1 86.54(11) . . ? N2 Co P1 94.11(11) . . ? O2 Co P1 89.93(10) . . ? C1 Co P2 86.43(13) . . ? N1 Co P2 91.41(11) . . ? N2 Co P2 88.45(11) . . ? O2 Co P2 93.25(10) . . ? P1 Co P2 176.55(5) . . ? C7 N1 C8 119.5(4) . . ? C7 N1 Co 116.0(3) . . ? C8 N1 Co 124.5(3) . . ? C21 N2 C22 124.7(4) . . ? C21 N2 Co 90.4(3) . . ? C22 N2 Co 142.9(3) . . ? C21 O2 Co 89.9(3) . . ? C34 P1 C32 102.3(3) . . ? C34 P1 C33 103.4(3) . . ? C32 P1 C33 102.4(3) . . ? C34 P1 Co 116.35(19) . . ? C32 P1 Co 117.09(19) . . ? C33 P1 Co 113.31(19) . . ? C30 P2 C29 101.9(2) . . ? C30 P2 C31 101.8(2) . . ? C29 P2 C31 102.7(3) . . ? C30 P2 Co 116.85(17) . . ? C29 P2 Co 116.48(17) . . ? C31 P2 Co 114.89(17) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.386 _refine_diff_density_min -1.869 _refine_diff_density_rms 0.121