#------------------------------------------------------------------------------ #$Date: 2008-01-26 13:05:32 +0000 (Sat, 26 Jan 2008) $ #$Revision: 19 $ #$URL: svn://www.crystallography.net/cod/cif/1/1100818.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100818 _chemical_formula_sum 'C41 H41 F3 N Ni O P' _chemical_formula_weight 710.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' 'F' 'F' 0.0171 0.0103 '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 9.299(3) _cell_length_b 21.609(6) _cell_length_c 18.370(13) _cell_angle_alpha 90.00 _cell_angle_beta 96.70(3) _cell_angle_gamma 90.00 _cell_volume 3666(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 34 _cell_measurement_theta_min 5.21 _cell_measurement_theta_max 12.30 _exptl_crystal_description 'tabular' _exptl_crystal_colour 'brown' _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.51 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.287 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1488 _exptl_absorpt_coefficient_mu 0.620 _exptl_absorpt_correction_type psi-scan _exptl_absorpt_correction_T_min 0.4412 _exptl_absorpt_correction_T_max 0.5419 _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 8303 _diffrn_reflns_av_R_equivalents 0.0377 _diffrn_reflns_av_sigmaI/netI 0.0867 _diffrn_reflns_limit_h_min -1 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -1 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 24.99 _reflns_number_total 6407 _reflns_number_gt 3724 _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^)+(0.1000P)^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 6407 _refine_ls_number_parameters 438 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1164 _refine_ls_R_factor_gt 0.0677 _refine_ls_wR_factor_ref 0.1924 _refine_ls_wR_factor_gt 0.1763 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.020 _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 Ni Ni 0.33418(6) 0.45323(3) 0.26059(4) 0.0408(2) Uani 1 1 d . . . P P 0.17835(13) 0.52612(6) 0.22702(8) 0.0410(3) Uani 1 1 d . . . O O 0.4340(4) 0.51268(16) 0.3237(2) 0.0535(10) Uani 1 1 d . . . N N 0.4353(4) 0.38306(18) 0.3099(2) 0.0409(10) Uani 1 1 d . . . C1 C 0.2648(6) 0.4123(2) 0.1710(3) 0.0480(13) Uani 1 1 d . . . C2 C 0.3271(6) 0.4333(3) 0.1114(3) 0.0573(15) Uani 1 1 d . . . H2 H 0.3947 0.4651 0.1176 0.057 Uiso 1 1 calc R . . C3 C 0.2919(8) 0.4082(3) 0.0423(4) 0.079(2) Uani 1 1 d . . . H3 H 0.3352 0.4232 0.0027 0.079 Uiso 1 1 calc R . . C4 C 0.1922(10) 0.3611(3) 0.0327(4) 0.093(3) Uani 1 1 d . . . H4 H 0.1695 0.3434 -0.0133 0.093 Uiso 1 1 calc R . . C5 C 0.1266(9) 0.3402(3) 0.0908(5) 0.089(2) Uani 1 1 d . . . H5 H 0.0575 0.3090 0.0837 0.089 Uiso 1 1 calc R . . C6 C 0.1615(7) 0.3648(3) 0.1595(4) 0.0653(17) Uani 1 1 d . . . H6 H 0.1166 0.3499 0.1987 0.065 Uiso 1 1 calc R . . C7 C 0.2418(6) 0.5831(2) 0.1634(3) 0.0505(14) Uani 1 1 d . . . C8 C 0.3889(7) 0.5929(3) 0.1683(4) 0.0676(17) Uani 1 1 d . . . H8 H 0.4509 0.5718 0.2031 0.068 Uiso 1 1 calc R . . C9 C 0.4449(9) 0.6347(4) 0.1208(5) 0.093(3) Uani 1 1 d . . . H9 H 0.5443 0.6410 0.1235 0.093 Uiso 1 1 calc R . . C10 C 0.3543(12) 0.6657(3) 0.0712(4) 0.099(3) Uani 1 1 d . . . H10 H 0.3920 0.6932 0.0394 0.099 Uiso 1 1 calc R . . C11 C 0.2081(11) 0.6575(3) 0.0668(4) 0.096(3) Uani 1 1 d . . . H11 H 0.1464 0.6796 0.0327 0.096 Uiso 1 1 calc R . . C12 C 0.1530(7) 0.6164(3) 0.1134(4) 0.0687(18) Uani 1 1 d . . . H12 H 0.0532 0.6111 0.1109 0.069 Uiso 1 1 calc R . . C13 C 0.1419(5) 0.5718(3) 0.3067(3) 0.0475(13) Uani 1 1 d . . . C14 C 0.1385(7) 0.5439(3) 0.3738(3) 0.0677(17) Uani 1 1 d . . . H14 H 0.1582 0.5018 0.3781 0.068 Uiso 1 1 calc R . . C15 C 0.1075(7) 0.5755(4) 0.4345(4) 0.086(2) Uani 1 1 d . . . H15 H 0.1021 0.5552 0.4787 0.086 Uiso 1 1 calc R . . C16 C 0.0847(8) 0.6380(5) 0.4284(5) 0.099(3) Uani 1 1 d . . . H16 H 0.0650 0.6605 0.4693 0.099 Uiso 1 1 calc R . . C17 C 0.0902(9) 0.6667(4) 0.3652(5) 0.101(3) Uani 1 1 d . . . H17 H 0.0769 0.7093 0.3626 0.101 Uiso 1 1 calc R . . C18 C 0.1157(7) 0.6340(3) 0.3020(4) 0.0723(18) Uani 1 1 d . . . H18 H 0.1148 0.6544 0.2573 0.072 Uiso 1 1 calc R . . C19 C -0.0034(5) 0.5044(2) 0.1847(3) 0.0468(13) Uani 1 1 d . . . C20 C -0.1188(6) 0.5003(3) 0.2263(3) 0.0633(16) Uani 1 1 d . . . H20 H -0.1063 0.5118 0.2755 0.063 Uiso 1 1 calc R . . C21 C -0.2517(7) 0.4794(4) 0.1949(5) 0.084(2) Uani 1 1 d . . . H21 H -0.3285 0.4770 0.2230 0.084 Uiso 1 1 calc R . . C22 C -0.2718(7) 0.4622(3) 0.1230(5) 0.081(2) Uani 1 1 d . . . H22 H -0.3617 0.4477 0.1026 0.081 Uiso 1 1 calc R . . C23 C -0.1599(6) 0.4660(3) 0.0807(3) 0.0602(16) Uani 1 1 d . . . H23 H -0.1741 0.4549 0.0314 0.060 Uiso 1 1 calc R . . C24 C -0.0258(6) 0.4864(3) 0.1120(3) 0.0546(15) Uani 1 1 d . . . H24 H 0.0507 0.4880 0.0837 0.055 Uiso 1 1 calc R . . C25 C 0.3780(6) 0.3209(2) 0.2926(3) 0.0510(14) Uani 1 1 d . . . C26 C 0.4368(6) 0.2857(3) 0.2379(4) 0.0603(16) Uani 1 1 d . . . C27 C 0.3755(7) 0.2290(3) 0.2222(4) 0.0734(19) Uani 1 1 d . . . H27 H 0.4120 0.2044 0.1871 0.073 Uiso 1 1 calc R . . C28 C 0.2611(8) 0.2067(3) 0.2566(4) 0.079(2) Uani 1 1 d . . . H28 H 0.2211 0.1681 0.2442 0.079 Uiso 1 1 calc R . . C29 C 0.2073(7) 0.2425(3) 0.3093(4) 0.0715(19) Uani 1 1 d . . . H29 H 0.1304 0.2274 0.3322 0.072 Uiso 1 1 calc R . . C30 C 0.2640(6) 0.3003(2) 0.3294(3) 0.0524(14) Uani 1 1 d . . . C31 C 0.5601(7) 0.3105(3) 0.1989(4) 0.0670(17) Uani 1 1 d . . . H31 H 0.5514 0.3557 0.1972 0.067 Uiso 1 1 calc R . . C32 C 0.7059(7) 0.2950(5) 0.2397(4) 0.114(3) Uani 1 1 d . . . H32A H 0.7144 0.3138 0.2874 0.114 Uiso 1 1 calc R . . H32B H 0.7811 0.3105 0.2129 0.114 Uiso 1 1 calc R . . H32C H 0.7152 0.2509 0.2448 0.114 Uiso 1 1 calc R . . C33 C 0.5532(8) 0.2873(4) 0.1195(4) 0.093(2) Uani 1 1 d . . . H33A H 0.5775 0.2441 0.1196 0.093 Uiso 1 1 calc R . . H33B H 0.6208 0.3101 0.0943 0.093 Uiso 1 1 calc R . . H33C H 0.4571 0.2931 0.0951 0.093 Uiso 1 1 calc R . . C34 C 0.2023(7) 0.3371(3) 0.3866(4) 0.0634(17) Uani 1 1 d . . . H34 H 0.2642 0.3736 0.3961 0.063 Uiso 1 1 calc R . . C35 C 0.0517(8) 0.3602(4) 0.3637(5) 0.097(3) Uani 1 1 d . . . H35A H 0.0485 0.3804 0.3170 0.097 Uiso 1 1 calc R . . H35B H 0.0248 0.3891 0.3995 0.097 Uiso 1 1 calc R . . H35C H -0.0145 0.3260 0.3599 0.097 Uiso 1 1 calc R . . C36 C 0.2061(9) 0.3020(4) 0.4590(4) 0.102(3) Uani 1 1 d . . . H36A H 0.1504 0.2647 0.4514 0.102 Uiso 1 1 calc R . . H36B H 0.1658 0.3275 0.4943 0.102 Uiso 1 1 calc R . . H36C H 0.3044 0.2918 0.4767 0.102 Uiso 1 1 calc R . . C37 C 0.5337(6) 0.3869(3) 0.3656(4) 0.0556(15) Uani 1 1 d . . . C38 C 0.5926(6) 0.4444(2) 0.3936(3) 0.0572(15) Uani 1 1 d . . . H38 H 0.6720 0.4432 0.4295 0.057 Uiso 1 1 calc R . . C39 C 0.5406(6) 0.5004(2) 0.3715(3) 0.0476(13) Uani 1 1 d . . . C40 C 0.5918(7) 0.3313(2) 0.4103(4) 0.0722(19) Uani 1 1 d . . . H40A H 0.5530 0.3312 0.4565 0.072 Uiso 1 1 calc R . . H40B H 0.6956 0.3335 0.4187 0.072 Uiso 1 1 calc R . . H40C H 0.5636 0.2940 0.3841 0.072 Uiso 1 1 calc R . . C41 C 0.6130(7) 0.5582(3) 0.4071(4) 0.0638(17) Uani 1 1 d . . . F1 F 0.5180(5) 0.5991(2) 0.4256(3) 0.1241(19) Uani 1 1 d . . . F2 F 0.7022(6) 0.54837(18) 0.4664(3) 0.126(2) Uani 1 1 d . . . F3 F 0.6850(6) 0.5879(2) 0.3610(3) 0.1164(17) 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 Ni 0.0352(3) 0.0333(3) 0.0540(4) -0.0013(3) 0.0059(3) 0.0026(3) P 0.0367(7) 0.0369(7) 0.0504(9) 0.0021(6) 0.0092(6) 0.0050(6) O 0.048(2) 0.038(2) 0.071(3) -0.0106(18) -0.006(2) -0.0019(17) N 0.035(2) 0.033(2) 0.053(3) 0.0011(19) -0.001(2) 0.0026(18) C1 0.048(3) 0.037(3) 0.058(4) -0.004(3) -0.002(3) 0.008(2) C2 0.052(3) 0.056(3) 0.065(4) -0.009(3) 0.013(3) 0.011(3) C3 0.098(5) 0.076(5) 0.061(4) -0.002(4) 0.004(4) 0.029(4) C4 0.139(7) 0.064(5) 0.066(5) -0.013(4) -0.034(5) 0.023(5) C5 0.119(6) 0.046(4) 0.087(6) -0.009(4) -0.043(5) -0.009(4) C6 0.070(4) 0.049(3) 0.071(4) 0.004(3) -0.019(3) -0.004(3) C7 0.056(3) 0.036(3) 0.061(4) -0.002(3) 0.015(3) -0.007(3) C8 0.066(4) 0.068(4) 0.070(4) 0.000(3) 0.013(3) -0.016(3) C9 0.094(5) 0.106(6) 0.084(6) -0.015(5) 0.030(5) -0.059(5) C10 0.166(9) 0.072(5) 0.060(5) -0.001(4) 0.023(6) -0.055(6) C11 0.147(8) 0.059(4) 0.079(6) 0.011(4) 0.000(5) -0.022(5) C12 0.072(4) 0.052(4) 0.077(5) 0.017(3) -0.011(3) -0.010(3) C13 0.037(3) 0.052(3) 0.054(4) -0.011(3) 0.009(2) 0.007(2) C14 0.069(4) 0.074(4) 0.063(4) 0.007(4) 0.019(3) 0.010(4) C15 0.072(5) 0.125(7) 0.065(5) -0.006(5) 0.020(4) 0.010(5) C16 0.074(5) 0.146(9) 0.083(6) -0.050(6) 0.029(4) 0.002(5) C17 0.109(6) 0.077(5) 0.123(8) -0.039(5) 0.036(6) 0.016(5) C18 0.082(4) 0.063(4) 0.076(5) -0.009(4) 0.024(4) 0.010(4) C19 0.035(3) 0.040(3) 0.067(4) 0.001(3) 0.012(3) 0.008(2) C20 0.052(3) 0.086(4) 0.054(4) 0.002(3) 0.012(3) 0.003(3) C21 0.042(3) 0.117(6) 0.096(6) 0.002(5) 0.024(4) -0.005(4) C22 0.040(3) 0.095(5) 0.106(6) 0.000(5) 0.010(4) -0.006(4) C23 0.048(3) 0.073(4) 0.057(4) -0.005(3) -0.007(3) 0.001(3) C24 0.038(3) 0.061(4) 0.065(4) 0.001(3) 0.009(3) 0.003(3) C25 0.046(3) 0.030(3) 0.076(4) -0.001(3) 0.002(3) 0.001(2) C26 0.056(3) 0.040(3) 0.086(5) 0.000(3) 0.012(3) 0.012(3) C27 0.082(5) 0.049(4) 0.089(5) -0.018(4) 0.010(4) 0.009(4) C28 0.082(5) 0.038(3) 0.116(6) -0.011(4) 0.003(4) -0.009(3) C29 0.069(4) 0.044(3) 0.102(5) 0.010(4) 0.015(4) -0.009(3) C30 0.052(3) 0.037(3) 0.067(4) 0.006(3) 0.004(3) -0.005(3) C31 0.066(4) 0.061(4) 0.078(5) -0.007(3) 0.024(3) 0.012(3) C32 0.067(5) 0.178(10) 0.096(7) 0.002(6) 0.013(5) 0.015(6) C33 0.104(6) 0.107(6) 0.071(5) 0.003(4) 0.024(4) 0.030(5) C34 0.066(4) 0.052(4) 0.076(5) 0.003(3) 0.025(3) -0.013(3) C35 0.091(5) 0.091(6) 0.112(7) 0.002(5) 0.027(5) 0.028(5) C36 0.107(6) 0.096(6) 0.108(7) 0.020(5) 0.039(5) 0.009(5) C37 0.051(3) 0.042(3) 0.074(4) 0.006(3) 0.009(3) 0.009(3) C38 0.056(3) 0.050(4) 0.061(4) -0.002(3) -0.015(3) -0.003(3) C39 0.051(3) 0.035(3) 0.058(4) -0.003(3) 0.009(3) -0.008(2) C40 0.077(4) 0.042(3) 0.093(5) 0.003(3) -0.013(4) 0.006(3) C41 0.068(4) 0.040(3) 0.080(5) -0.001(3) -0.008(4) -0.008(3) F1 0.117(4) 0.080(3) 0.172(5) -0.069(3) 0.003(3) 0.003(3) F2 0.165(5) 0.062(3) 0.126(4) 0.007(3) -0.085(4) -0.022(3) F3 0.142(4) 0.079(3) 0.130(4) -0.002(3) 0.023(3) -0.058(3)