data_1100816 _chemical_formula_sum 'C46 H43 F3 N Ni O P' _chemical_formula_weight 772.49 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'P' 'P' 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ni' 'Ni' 0.3393 1.1124 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.611(3) _cell_length_b 12.665(2) _cell_length_c 14.887(2) _cell_angle_alpha 72.302(12) _cell_angle_beta 70.461(13) _cell_angle_gamma 68.172(15) _cell_volume 2035.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min 5.20 _cell_measurement_theta_max 9.31 _exptl_crystal_description 'rod-like' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.260 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 808 _exptl_absorpt_coefficient_mu 0.564 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.49629 _exptl_absorpt_correction_T_max 0.54954 _exptl_absorpt_process_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 'Siemens P4' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 8418 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0889 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 24.98 _reflns_number_total 7098 _reflns_number_gt 4218 _reflns_threshold_expression >2sigma(I) _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^)+(0.0100P)^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 7098 _refine_ls_number_parameters 482 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0781 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.0696 _refine_ls_wR_factor_gt 0.0643 _refine_ls_goodness_of_fit_ref 0.872 _refine_ls_restrained_S_all 0.872 _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 Ni Ni 0.82357(3) 0.81734(3) 0.73541(3) 0.04088(11) Uani 1 1 d . . . P P 0.68644(7) 0.73837(6) 0.75567(5) 0.0431(2) Uani 1 1 d . . . O O 0.70004(15) 0.96034(15) 0.74550(13) 0.0489(5) Uani 1 1 d . . . N N 0.93982(19) 0.87770(17) 0.74653(15) 0.0420(6) Uani 1 1 d . . . F1 F 1.11005(17) 0.96791(16) 0.76664(17) 0.1017(7) Uani 1 1 d . . . F2 F 1.00778(19) 1.13373(17) 0.7100(2) 0.1279(10) Uani 1 1 d . . . F3 F 0.9557(2) 1.0592(2) 0.8594(2) 0.1350(11) Uani 1 1 d . . . C1 C 0.9342(2) 0.6816(2) 0.6910(2) 0.0478(8) Uani 1 1 d . . . C2 C 0.9955(3) 0.5804(3) 0.7451(2) 0.0634(9) Uani 1 1 d . . . H2 H 0.9850 0.5755 0.8109 0.063 Uiso 1 1 calc R . . C3 C 1.0714(3) 0.4870(3) 0.7033(3) 0.0893(13) Uani 1 1 d . . . H3 H 1.1103 0.4203 0.7415 0.089 Uiso 1 1 calc R . . C4 C 1.0903(3) 0.4915(4) 0.6064(4) 0.1083(17) Uani 1 1 d . . . H4 H 1.1421 0.4284 0.5788 0.108 Uiso 1 1 calc R . . C5 C 1.0321(3) 0.5899(4) 0.5501(3) 0.0915(13) Uani 1 1 d . . . H5 H 1.0446 0.5940 0.4841 0.091 Uiso 1 1 calc R . . C6 C 0.9545(3) 0.6833(3) 0.5925(2) 0.0613(9) Uani 1 1 d . . . H6 H 0.9148 0.7490 0.5540 0.061 Uiso 1 1 calc R . . C7 C 0.5488(2) 0.8067(2) 0.8375(2) 0.0442(7) Uani 1 1 d . . . C8 C 0.4387(3) 0.8336(3) 0.8212(2) 0.0611(9) Uani 1 1 d . . . H8 H 0.4324 0.8164 0.7671 0.061 Uiso 1 1 calc R . . C9 C 0.3381(3) 0.8860(3) 0.8859(3) 0.0784(11) Uani 1 1 d . . . H9 H 0.2647 0.9046 0.8742 0.078 Uiso 1 1 calc R . . C10 C 0.3450(3) 0.9110(3) 0.9663(3) 0.0773(11) Uani 1 1 d . . . H10 H 0.2768 0.9464 1.0090 0.077 Uiso 1 1 calc R . . C11 C 0.4528(3) 0.8836(3) 0.9839(2) 0.0696(10) Uani 1 1 d . . . H11 H 0.4580 0.8995 1.0390 0.070 Uiso 1 1 calc R . . C12 C 0.5542(3) 0.8324(2) 0.9198(2) 0.0566(8) Uani 1 1 d . . . H12 H 0.6272 0.8148 0.9320 0.057 Uiso 1 1 calc R . . C13 C 0.6450(2) 0.7594(3) 0.6442(2) 0.0524(8) Uani 1 1 d . . . C14 C 0.6544(3) 0.8569(3) 0.5730(3) 0.0860(12) Uani 1 1 d . . . H14 H 0.6824 0.9101 0.5823 0.086 Uiso 1 1 calc R . . C15 C 0.6229(4) 0.8765(4) 0.4882(3) 0.1312(19) Uani 1 1 d . . . H15 H 0.6286 0.9434 0.4411 0.131 Uiso 1 1 calc R . . C16 C 0.5832(4) 0.7982(5) 0.4724(3) 0.126(2) Uani 1 1 d . . . H16 H 0.5628 0.8114 0.4145 0.126 Uiso 1 1 calc R . . C17 C 0.5739(4) 0.7020(5) 0.5413(3) 0.1097(16) Uani 1 1 d . . . H17 H 0.5473 0.6484 0.5309 0.110 Uiso 1 1 calc R . . C18 C 0.6035(3) 0.6830(3) 0.6263(3) 0.0787(11) Uani 1 1 d . . . H18 H 0.5955 0.6168 0.6735 0.079 Uiso 1 1 calc R . . C19 C 0.7090(3) 0.5833(2) 0.8072(2) 0.0498(8) Uani 1 1 d . . . C20 C 0.7856(3) 0.5024(3) 0.7507(2) 0.0668(10) Uani 1 1 d . . . H20 H 0.8245 0.5282 0.6870 0.067 Uiso 1 1 calc R . . C21 C 0.8050(3) 0.3847(3) 0.7872(3) 0.0862(12) Uani 1 1 d . . . H21 H 0.8570 0.3318 0.7485 0.086 Uiso 1 1 calc R . . C22 C 0.7478(3) 0.3462(3) 0.8799(3) 0.0860(12) Uani 1 1 d . . . H22 H 0.7607 0.2669 0.9042 0.086 Uiso 1 1 calc R . . C23 C 0.6709(3) 0.4236(3) 0.9382(3) 0.0759(10) Uani 1 1 d . . . H23 H 0.6317 0.3967 1.0014 0.076 Uiso 1 1 calc R . . C24 C 0.6524(3) 0.5422(3) 0.9016(2) 0.0613(9) Uani 1 1 d . . . H24 H 0.6014 0.5946 0.9411 0.061 Uiso 1 1 calc R . . C25 C 1.0462(2) 0.7931(2) 0.7719(2) 0.0429(7) Uani 1 1 d . . . C26 C 1.0416(3) 0.7423(2) 0.8699(2) 0.0482(7) Uani 1 1 d . . . C27 C 1.1441(3) 0.6614(3) 0.8926(2) 0.0657(9) Uani 1 1 d . . . H27 H 1.1438 0.6259 0.9573 0.066 Uiso 1 1 calc R . . C28 C 1.2461(3) 0.6329(3) 0.8211(3) 0.0732(10) Uani 1 1 d . . . H28 H 1.3140 0.5793 0.8380 0.073 Uiso 1 1 calc R . . C29 C 1.2484(3) 0.6830(3) 0.7251(3) 0.0673(9) Uani 1 1 d . . . H29 H 1.3181 0.6627 0.6776 0.067 Uiso 1 1 calc R . . C30 C 1.1489(3) 0.7632(2) 0.6976(2) 0.0509(8) Uani 1 1 d . . . C31 C 0.9304(3) 0.7726(3) 0.9516(2) 0.0610(9) Uani 1 1 d . . . H31 H 0.8739 0.8414 0.9233 0.061 Uiso 1 1 calc R . . C32 C 0.8730(3) 0.6750(3) 0.9917(2) 0.0927(12) Uani 1 1 d . . . H32A H 0.8566 0.6589 0.9395 0.093 Uiso 1 1 calc R . . H32B H 0.8007 0.6985 1.0396 0.093 Uiso 1 1 calc R . . H32C H 0.9256 0.6064 1.0211 0.093 Uiso 1 1 calc R . . C33 C 0.9523(3) 0.8034(3) 1.0338(2) 0.1060(14) Uani 1 1 d . . . H33A H 1.0031 0.7360 1.0662 0.106 Uiso 1 1 calc R . . H33B H 0.8785 0.8294 1.0794 0.106 Uiso 1 1 calc R . . H33C H 0.9891 0.8641 1.0074 0.106 Uiso 1 1 calc R . . C34 C 1.1521(3) 0.8145(3) 0.5902(2) 0.0725(10) Uani 1 1 d . . . H34 H 1.0723 0.8320 0.5835 0.073 Uiso 1 1 calc R . . C35 C 1.1834(4) 0.9276(3) 0.5523(3) 0.1392(18) Uani 1 1 d . . . H35A H 1.1207 0.9875 0.5821 0.139 Uiso 1 1 calc R . . H35B H 1.1943 0.9493 0.4829 0.139 Uiso 1 1 calc R . . H35C H 1.2550 0.9174 0.5679 0.139 Uiso 1 1 calc R . . C36 C 1.2346(3) 0.7296(3) 0.5241(2) 0.1039(14) Uani 1 1 d . . . H36A H 1.3148 0.7262 0.5148 0.104 Uiso 1 1 calc R . . H36B H 1.2154 0.7555 0.4622 0.104 Uiso 1 1 calc R . . H36C H 1.2254 0.6537 0.5536 0.104 Uiso 1 1 calc R . . C37 C 0.9152(3) 0.9880(2) 0.7501(2) 0.0509(8) Uani 1 1 d . . . C38 C 0.8090(3) 1.0758(2) 0.7421(2) 0.0551(8) Uani 1 1 d . . . H38 H 0.8074 1.1517 0.7360 0.055 Uiso 1 1 calc R . . C39 C 0.7071(3) 1.0594(2) 0.74253(18) 0.0425(7) Uani 1 1 d . . . C40 C 0.9992(3) 1.0333(3) 0.7730(3) 0.0819(12) Uani 1 1 d . . . C41 C 0.5952(3) 1.1582(2) 0.74503(19) 0.0449(7) Uani 1 1 d . . . C42 C 0.5928(3) 1.2729(2) 0.7266(2) 0.0717(10) Uani 1 1 d . . . H42 H 0.6629 1.2906 0.7113 0.072 Uiso 1 1 calc R . . C43 C 0.4872(3) 1.3614(3) 0.7308(3) 0.0912(13) Uani 1 1 d . . . H43 H 0.4872 1.4381 0.7173 0.091 Uiso 1 1 calc R . . C44 C 0.3818(3) 1.3375(3) 0.7546(3) 0.0808(11) Uani 1 1 d . . . H44 H 0.3108 1.3972 0.7584 0.081 Uiso 1 1 calc R . . C45 C 0.3837(3) 1.2246(3) 0.7724(2) 0.0700(10) Uani 1 1 d . . . H45 H 0.3134 1.2071 0.7884 0.070 Uiso 1 1 calc R . . C46 C 0.4894(3) 1.1361(3) 0.7669(2) 0.0541(8) Uani 1 1 d . . . H46 H 0.4890 1.0598 0.7783 0.054 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 Ni 0.0406(2) 0.0370(2) 0.0500(2) -0.01385(17) -0.01054(19) -0.01383(18) P 0.0433(5) 0.0421(4) 0.0500(5) -0.0141(4) -0.0115(4) -0.0161(4) O 0.0397(12) 0.0370(11) 0.0709(14) -0.0164(10) -0.0129(11) -0.0092(10) N 0.0400(15) 0.0349(13) 0.0543(15) -0.0122(11) -0.0144(12) -0.0100(12) F1 0.0665(14) 0.0660(13) 0.205(2) -0.0483(14) -0.0661(15) -0.0111(11) F2 0.0953(18) 0.0587(14) 0.255(3) -0.0174(16) -0.0739(19) -0.0359(13) F3 0.113(2) 0.172(2) 0.188(3) -0.117(2) -0.0511(19) -0.0410(18) C1 0.0416(19) 0.0463(18) 0.067(2) -0.0223(16) -0.0132(17) -0.0173(15) C2 0.058(2) 0.053(2) 0.092(3) -0.0304(19) -0.027(2) -0.0109(18) C3 0.061(3) 0.056(2) 0.162(4) -0.046(3) -0.042(3) 0.002(2) C4 0.062(3) 0.098(3) 0.179(5) -0.103(4) -0.001(3) -0.005(3) C5 0.077(3) 0.111(3) 0.107(3) -0.077(3) 0.006(3) -0.033(3) C6 0.053(2) 0.069(2) 0.073(2) -0.0341(19) -0.0041(18) -0.0241(18) C7 0.0427(19) 0.0444(17) 0.0477(19) -0.0104(14) -0.0064(15) -0.0192(15) C8 0.052(2) 0.070(2) 0.066(2) -0.0230(18) -0.0123(19) -0.0182(19) C9 0.044(2) 0.087(3) 0.101(3) -0.030(2) -0.013(2) -0.012(2) C10 0.065(3) 0.068(2) 0.077(3) -0.023(2) 0.014(2) -0.019(2) C11 0.086(3) 0.073(2) 0.050(2) -0.0202(18) -0.001(2) -0.033(2) C12 0.055(2) 0.063(2) 0.055(2) -0.0179(17) -0.0088(18) -0.0214(18) C13 0.0418(19) 0.068(2) 0.0517(19) -0.0213(17) -0.0106(16) -0.0145(17) C14 0.104(3) 0.093(3) 0.074(3) 0.006(2) -0.047(2) -0.041(3) C15 0.157(5) 0.167(5) 0.079(3) 0.020(3) -0.066(3) -0.062(4) C16 0.118(4) 0.212(7) 0.065(3) -0.042(4) -0.041(3) -0.042(4) C17 0.093(3) 0.182(5) 0.095(3) -0.071(3) -0.031(3) -0.046(4) C18 0.084(3) 0.101(3) 0.078(3) -0.036(2) -0.023(2) -0.041(2) C19 0.047(2) 0.0453(18) 0.065(2) -0.0138(16) -0.0134(17) -0.0209(16) C20 0.071(2) 0.051(2) 0.085(3) -0.0221(19) -0.007(2) -0.0301(19) C21 0.081(3) 0.048(2) 0.131(4) -0.032(2) -0.010(3) -0.025(2) C22 0.087(3) 0.046(2) 0.132(4) -0.007(2) -0.037(3) -0.028(2) C23 0.084(3) 0.064(2) 0.079(3) 0.009(2) -0.025(2) -0.037(2) C24 0.060(2) 0.051(2) 0.074(2) -0.0104(18) -0.019(2) -0.0184(18) C25 0.0382(18) 0.0405(16) 0.058(2) -0.0173(15) -0.0169(16) -0.0107(14) C26 0.0435(19) 0.0501(18) 0.055(2) -0.0235(16) -0.0155(17) -0.0058(16) C27 0.064(2) 0.063(2) 0.067(2) -0.0197(18) -0.028(2) -0.0019(19) C28 0.054(2) 0.067(2) 0.097(3) -0.034(2) -0.038(2) 0.0142(19) C29 0.043(2) 0.077(2) 0.084(3) -0.036(2) -0.009(2) -0.0112(19) C30 0.043(2) 0.0542(19) 0.060(2) -0.0172(17) -0.0096(18) -0.0177(17) C31 0.052(2) 0.069(2) 0.056(2) -0.0237(18) -0.0161(18) -0.0008(18) C32 0.084(3) 0.112(3) 0.078(3) -0.032(2) 0.004(2) -0.036(3) C33 0.093(3) 0.152(4) 0.087(3) -0.073(3) -0.010(2) -0.025(3) C34 0.058(2) 0.088(3) 0.067(2) -0.011(2) -0.003(2) -0.034(2) C35 0.190(5) 0.132(4) 0.098(3) 0.004(3) 0.001(3) -0.106(4) C36 0.077(3) 0.158(4) 0.076(3) -0.043(3) 0.006(2) -0.042(3) C37 0.048(2) 0.0408(18) 0.075(2) -0.0167(16) -0.0226(17) -0.0159(16) C38 0.053(2) 0.0303(17) 0.089(2) -0.0133(16) -0.0305(19) -0.0086(16) C39 0.050(2) 0.0386(17) 0.0395(17) -0.0102(14) -0.0096(15) -0.0133(15) C40 0.073(3) 0.049(2) 0.151(4) -0.030(3) -0.054(3) -0.017(2) C41 0.0435(19) 0.0407(17) 0.0453(18) -0.0122(14) -0.0097(15) -0.0055(15) C42 0.054(2) 0.0433(19) 0.107(3) -0.0202(19) -0.008(2) -0.0087(18) C43 0.071(3) 0.044(2) 0.146(4) -0.032(2) -0.017(3) -0.002(2) C44 0.054(2) 0.063(2) 0.110(3) -0.036(2) -0.021(2) 0.013(2) C45 0.044(2) 0.070(2) 0.088(3) -0.025(2) -0.0115(19) -0.0056(19) C46 0.049(2) 0.0504(19) 0.059(2) -0.0123(16) -0.0126(17) -0.0109(17)