data_1100817 _chemical_formula_sum 'C46 H46 N Ni O P' _chemical_formula_weight 718.52 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' '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 10.782(3) _cell_length_b 38.013(11) _cell_length_c 10.424(3) _cell_angle_alpha 90.00 _cell_angle_beta 114.18(2) _cell_angle_gamma 90.00 _cell_volume 3897.5(19) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 45 _cell_measurement_theta_min 4.98 _cell_measurement_theta_max 11.69 _exptl_crystal_description 'block' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.225 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 0.574 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.5631 _exptl_absorpt_correction_T_max 0.7205 _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 9536 _diffrn_reflns_av_R_equivalents 0.0277 _diffrn_reflns_av_sigmaI/netI 0.1180 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -46 _diffrn_reflns_limit_k_max 1 _diffrn_reflns_limit_l_min -1 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.98 _reflns_number_total 7656 _reflns_number_gt 4019 _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 7656 _refine_ls_number_parameters 456 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0998 _refine_ls_R_factor_gt 0.0438 _refine_ls_wR_factor_ref 0.0790 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 0.915 _refine_ls_restrained_S_all 0.915 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ni Ni 0.57075(4) 0.871396(10) 0.38721(4) 0.03179(11) Uani 1 1 d . . . P P 0.76716(8) 0.86565(2) 0.56788(9) 0.0355(2) Uani 1 1 d . . . O O 0.52279(19) 0.82689(5) 0.4354(2) 0.0458(6) Uani 1 1 d . . . N N 0.3859(2) 0.88322(6) 0.2610(3) 0.0317(6) Uani 1 1 d . . . C1 C 0.6577(3) 0.90515(8) 0.3166(3) 0.0348(8) Uani 1 1 d . . . C2 C 0.6593(3) 0.94169(9) 0.3264(4) 0.0459(9) Uani 1 1 d . . . H2 H 0.6121 0.9526 0.3727 0.046 Uiso 1 1 calc R . . C3 C 0.7302(4) 0.96236(10) 0.2683(4) 0.0617(12) Uani 1 1 d . . . H3 H 0.7303 0.9867 0.2770 0.062 Uiso 1 1 calc R . . C4 C 0.7997(4) 0.94693(12) 0.1985(5) 0.0744(14) Uani 1 1 d . . . H4 H 0.8468 0.9608 0.1601 0.074 Uiso 1 1 calc R . . C5 C 0.7998(3) 0.91059(12) 0.1850(4) 0.0667(12) Uani 1 1 d . . . H5 H 0.8462 0.9000 0.1372 0.067 Uiso 1 1 calc R . . C6 C 0.7300(3) 0.89031(9) 0.2437(3) 0.0476(9) Uani 1 1 d . . . H6 H 0.7307 0.8660 0.2347 0.048 Uiso 1 1 calc R . . C7 C 0.8851(3) 0.83909(9) 0.5239(4) 0.0414(9) Uani 1 1 d . . . C8 C 0.8320(4) 0.80865(9) 0.4487(4) 0.0637(12) Uani 1 1 d . . . H8 H 0.7418 0.8027 0.4265 0.064 Uiso 1 1 calc R . . C9 C 0.9115(5) 0.78674(11) 0.4057(5) 0.0852(15) Uani 1 1 d . . . H9 H 0.8740 0.7668 0.3524 0.085 Uiso 1 1 calc R . . C10 C 1.0465(5) 0.79509(12) 0.4433(5) 0.0883(16) Uani 1 1 d . . . H10 H 1.1020 0.7801 0.4194 0.088 Uiso 1 1 calc R . . C11 C 1.0977(4) 0.82531(13) 0.5153(5) 0.0820(15) Uani 1 1 d . . . H11 H 1.1875 0.8314 0.5366 0.082 Uiso 1 1 calc R . . C12 C 1.0186(3) 0.84706(10) 0.5573(4) 0.0596(11) Uani 1 1 d . . . H12 H 1.0563 0.8673 0.6088 0.060 Uiso 1 1 calc R . . C13 C 0.8620(3) 0.90515(8) 0.6577(4) 0.0383(8) Uani 1 1 d . . . C14 C 0.9214(3) 0.92720(8) 0.5930(4) 0.0478(9) Uani 1 1 d . . . H14 H 0.9179 0.9214 0.5049 0.048 Uiso 1 1 calc R . . C15 C 0.9859(3) 0.95781(9) 0.6591(5) 0.0577(11) Uani 1 1 d . . . H15 H 1.0247 0.9726 0.6146 0.058 Uiso 1 1 calc R . . C16 C 0.9930(4) 0.96658(10) 0.7895(5) 0.0674(13) Uani 1 1 d . . . H16 H 1.0365 0.9871 0.8335 0.067 Uiso 1 1 calc R . . C17 C 0.9352(3) 0.94467(10) 0.8547(4) 0.0601(11) Uani 1 1 d . . . H17 H 0.9409 0.9502 0.9439 0.060 Uiso 1 1 calc R . . C18 C 0.8685(3) 0.91437(9) 0.7884(4) 0.0493(10) Uani 1 1 d . . . H18 H 0.8276 0.9001 0.8323 0.049 Uiso 1 1 calc R . . C19 C 0.7553(3) 0.84206(8) 0.7157(3) 0.0431(9) Uani 1 1 d . . . C20 C 0.6424(4) 0.84596(10) 0.7436(4) 0.0601(11) Uani 1 1 d . . . H20 H 0.5691 0.8590 0.6821 0.060 Uiso 1 1 calc R . . C21 C 0.6350(5) 0.83090(13) 0.8618(5) 0.0923(16) Uani 1 1 d . . . H21 H 0.5583 0.8340 0.8803 0.092 Uiso 1 1 calc R . . C22 C 0.7437(7) 0.81135(12) 0.9509(5) 0.102(2) Uani 1 1 d . . . H22 H 0.7401 0.8010 1.0301 0.102 Uiso 1 1 calc R . . C23 C 0.8556(5) 0.80708(12) 0.9247(5) 0.0853(15) Uani 1 1 d . . . H23 H 0.9284 0.7939 0.9862 0.085 Uiso 1 1 calc R . . C24 C 0.8629(4) 0.82218(10) 0.8069(4) 0.0609(11) Uani 1 1 d . . . H24 H 0.9399 0.8190 0.7892 0.061 Uiso 1 1 calc R . . C25 C 0.3560(3) 0.91921(8) 0.2158(3) 0.0321(8) Uani 1 1 d . . . C26 C 0.3303(3) 0.94292(9) 0.3042(4) 0.0387(8) Uani 1 1 d . . . C27 C 0.3060(3) 0.97804(9) 0.2639(4) 0.0485(10) Uani 1 1 d . . . H27 H 0.2882 0.9941 0.3215 0.049 Uiso 1 1 calc R . . C28 C 0.3084(3) 0.98911(9) 0.1388(4) 0.0539(10) Uani 1 1 d . . . H28 H 0.2924 1.0126 0.1124 0.054 Uiso 1 1 calc R . . C29 C 0.3343(3) 0.96553(9) 0.0533(4) 0.0475(9) Uani 1 1 d . . . H29 H 0.3361 0.9734 -0.0304 0.048 Uiso 1 1 calc R . . C30 C 0.3582(3) 0.92987(8) 0.0885(3) 0.0353(8) Uani 1 1 d . . . C31 C 0.3344(3) 0.93227(10) 0.4469(4) 0.0509(10) Uani 1 1 d . . . H31 H 0.3361 0.9065 0.4511 0.051 Uiso 1 1 calc R . . C32 C 0.2116(4) 0.94454(12) 0.4713(4) 0.1003(17) Uani 1 1 d . . . H32A H 0.2168 0.9695 0.4862 0.100 Uiso 1 1 calc R . . H32B H 0.2105 0.9329 0.5526 0.100 Uiso 1 1 calc R . . H32C H 0.1300 0.9389 0.3905 0.100 Uiso 1 1 calc R . . C33 C 0.4648(4) 0.94554(12) 0.5642(4) 0.0859(15) Uani 1 1 d . . . H33A H 0.5415 0.9379 0.5473 0.086 Uiso 1 1 calc R . . H33B H 0.4716 0.9364 0.6527 0.086 Uiso 1 1 calc R . . H33C H 0.4634 0.9708 0.5667 0.086 Uiso 1 1 calc R . . C34 C 0.3879(3) 0.90436(9) -0.0070(3) 0.0457(9) Uani 1 1 d . . . H34 H 0.4464 0.8858 0.0529 0.046 Uiso 1 1 calc R . . C35 C 0.2607(4) 0.88672(10) -0.1104(4) 0.0788(14) Uani 1 1 d . . . H35A H 0.2219 0.8724 -0.0603 0.079 Uiso 1 1 calc R . . H35B H 0.2832 0.8722 -0.1732 0.079 Uiso 1 1 calc R . . H35C H 0.1962 0.9043 -0.1634 0.079 Uiso 1 1 calc R . . C36 C 0.4655(4) 0.92162(11) -0.0842(4) 0.0838(14) Uani 1 1 d . . . H36A H 0.4115 0.9402 -0.1429 0.084 Uiso 1 1 calc R . . H36B H 0.4841 0.9044 -0.1413 0.084 Uiso 1 1 calc R . . H36C H 0.5495 0.9311 -0.0170 0.084 Uiso 1 1 calc R . . C37 C 0.2807(3) 0.86208(8) 0.2350(3) 0.0396(9) Uani 1 1 d . . . C38 C 0.2912(3) 0.82697(8) 0.2801(4) 0.0436(9) Uani 1 1 d . . . H38 H 0.2132 0.8132 0.2419 0.044 Uiso 1 1 calc R . . C39 C 0.4070(3) 0.81102(8) 0.3759(4) 0.0372(8) Uani 1 1 d . . . C40 C 0.1366(3) 0.87537(9) 0.1591(4) 0.0622(11) Uani 1 1 d . . . H40A H 0.1031 0.8831 0.2267 0.062 Uiso 1 1 calc R . . H40B H 0.0799 0.8568 0.1032 0.062 Uiso 1 1 calc R . . H40C H 0.1353 0.8947 0.0993 0.062 Uiso 1 1 calc R . . C41 C 0.4042(3) 0.77390(8) 0.4226(4) 0.0402(9) Uani 1 1 d . . . C42 C 0.3124(4) 0.74915(9) 0.3388(4) 0.0599(11) Uani 1 1 d . . . H42 H 0.2517 0.7552 0.2483 0.060 Uiso 1 1 calc R . . C43 C 0.3102(4) 0.71551(10) 0.3882(5) 0.0732(14) Uani 1 1 d . . . H43 H 0.2466 0.6994 0.3311 0.073 Uiso 1 1 calc R . . C44 C 0.3990(5) 0.70560(11) 0.5180(5) 0.0791(15) Uani 1 1 d . . . H44 H 0.3969 0.6828 0.5497 0.079 Uiso 1 1 calc R . . C45 C 0.4922(4) 0.72944(10) 0.6024(5) 0.0759(13) Uani 1 1 d . . . H45 H 0.5533 0.7228 0.6919 0.076 Uiso 1 1 calc R . . C46 C 0.4960(4) 0.76331(9) 0.5551(4) 0.0632(11) Uani 1 1 d . . . H46 H 0.5606 0.7791 0.6127 0.063 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 0.02706(19) 0.0327(2) 0.0321(2) 0.0065(2) 0.00852(17) -0.0007(2) P 0.0306(4) 0.0365(5) 0.0360(5) 0.0057(5) 0.0101(4) 0.0010(4) O 0.0371(12) 0.0403(13) 0.0526(17) 0.0145(13) 0.0108(12) -0.0055(11) N 0.0277(13) 0.0326(15) 0.0316(16) 0.0033(13) 0.0090(13) 0.0025(11) C1 0.0275(16) 0.040(2) 0.032(2) 0.0110(17) 0.0076(16) -0.0012(15) C2 0.0391(19) 0.043(2) 0.049(2) 0.0133(19) 0.0118(18) -0.0017(16) C3 0.059(2) 0.051(2) 0.062(3) 0.017(2) 0.013(2) -0.013(2) C4 0.066(3) 0.088(4) 0.075(3) 0.029(3) 0.035(3) -0.015(3) C5 0.059(3) 0.088(3) 0.065(3) 0.019(3) 0.038(2) 0.004(2) C6 0.044(2) 0.051(2) 0.046(2) 0.010(2) 0.0167(19) 0.0035(18) C7 0.0384(19) 0.044(2) 0.037(2) 0.0057(19) 0.0107(18) 0.0044(17) C8 0.052(2) 0.052(2) 0.089(3) -0.008(3) 0.030(2) 0.002(2) C9 0.102(4) 0.051(3) 0.112(4) -0.014(3) 0.053(3) 0.009(3) C10 0.087(4) 0.082(3) 0.121(5) 0.004(3) 0.068(4) 0.029(3) C11 0.051(3) 0.100(4) 0.101(4) -0.004(3) 0.037(3) 0.010(3) C12 0.044(2) 0.067(3) 0.063(3) -0.015(2) 0.017(2) 0.000(2) C13 0.0259(17) 0.0387(19) 0.042(2) 0.0053(18) 0.0050(16) 0.0013(15) C14 0.0335(17) 0.056(2) 0.043(2) 0.007(2) 0.0044(18) -0.0028(18) C15 0.042(2) 0.042(2) 0.075(3) 0.012(2) 0.011(2) -0.0057(18) C16 0.049(2) 0.040(2) 0.092(4) -0.018(3) 0.007(3) -0.0057(19) C17 0.061(3) 0.051(3) 0.056(3) -0.015(2) 0.012(2) 0.007(2) C18 0.051(2) 0.040(2) 0.054(3) 0.001(2) 0.018(2) 0.0032(18) C19 0.058(2) 0.037(2) 0.031(2) 0.0022(18) 0.0151(19) -0.0032(18) C20 0.069(3) 0.067(3) 0.054(3) 0.009(2) 0.034(2) 0.000(2) C21 0.130(5) 0.098(4) 0.082(4) -0.005(3) 0.076(4) -0.029(3) C22 0.195(6) 0.065(3) 0.055(4) 0.020(3) 0.059(4) -0.010(4) C23 0.128(4) 0.064(3) 0.050(3) 0.014(3) 0.022(3) 0.012(3) C24 0.076(3) 0.056(3) 0.043(3) 0.018(2) 0.017(2) 0.008(2) C25 0.0239(15) 0.0339(19) 0.032(2) 0.0034(17) 0.0053(15) 0.0054(14) C26 0.0333(18) 0.040(2) 0.039(2) 0.0019(18) 0.0114(17) 0.0030(15) C27 0.052(2) 0.040(2) 0.051(3) -0.005(2) 0.018(2) 0.0113(17) C28 0.062(2) 0.035(2) 0.053(3) 0.010(2) 0.012(2) 0.0135(18) C29 0.054(2) 0.047(2) 0.033(2) 0.0118(19) 0.0093(19) 0.0071(19) C30 0.0328(17) 0.0376(19) 0.0266(19) 0.0033(17) 0.0031(16) 0.0034(15) C31 0.059(2) 0.055(2) 0.046(2) -0.004(2) 0.028(2) 0.0029(19) C32 0.087(3) 0.151(5) 0.090(4) 0.003(4) 0.063(3) 0.013(3) C33 0.087(3) 0.133(4) 0.036(3) 0.010(3) 0.024(2) -0.012(3) C34 0.054(2) 0.049(2) 0.027(2) 0.0082(18) 0.0100(18) 0.0175(18) C35 0.079(3) 0.077(3) 0.056(3) -0.032(3) 0.004(2) 0.022(2) C36 0.116(4) 0.096(4) 0.057(3) 0.014(3) 0.053(3) 0.022(3) C37 0.0316(17) 0.041(2) 0.042(2) 0.0005(18) 0.0107(16) -0.0029(15) C38 0.0286(17) 0.039(2) 0.058(3) 0.000(2) 0.0122(18) -0.0066(15) C39 0.0420(19) 0.0332(18) 0.044(2) -0.0024(18) 0.0260(18) -0.0059(16) C40 0.0318(18) 0.062(2) 0.072(3) 0.012(2) 0.0003(19) -0.0019(18) C41 0.0414(19) 0.034(2) 0.051(2) 0.0040(19) 0.0255(19) -0.0026(16) C42 0.068(3) 0.041(2) 0.074(3) -0.003(2) 0.032(2) -0.0081(19) C43 0.090(3) 0.035(2) 0.105(4) -0.011(3) 0.051(3) -0.019(2) C44 0.125(4) 0.038(2) 0.103(4) 0.011(3) 0.076(4) -0.001(3) C45 0.117(4) 0.049(3) 0.067(3) 0.018(3) 0.042(3) 0.006(3) C46 0.082(3) 0.046(2) 0.066(3) 0.001(2) 0.035(3) -0.011(2)