#------------------------------------------------------------------------------ #$Date: 2010-01-30 15:59:17 +0200 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100797.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_1100797 _chemical_formula_sum 'C21 H55 B8 N2 Ni Si4' _chemical_formula_weight 593.22 _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_space_group_name_H-M 'P 1 21/c 1' _[local]_cod_cif_authors_sg_H-M P2(1)/c 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' 'B' 'B' 0.0013 0.0007 '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' 'Si' 'Si' 0.0817 0.0704 '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 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 17.788(5) _cell_length_b 10.130(2) _cell_length_c 21.049(5) _cell_angle_alpha 90.00 _cell_angle_beta 112.33(2) _cell_angle_gamma 90.00 _cell_volume 3508.4(15) _cell_formula_units_Z 4 _cell_measurement_temperature 230(2) _cell_measurement_reflns_used 30 _cell_measurement_theta_min 10.0 _cell_measurement_theta_max 15.0 _exptl_crystal_description plates _exptl_crystal_colour brown _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.123 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1276 _exptl_absorpt_coefficient_mu 0.704 _exptl_absorpt_correction_type 'psi scan' _exptl_absorpt_correction_T_min 0.802 _exptl_absorpt_correction_T_max 0.899 _exptl_absorpt_process_details 'Siemens XEMP' _diffrn_ambient_temperature 230(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 P3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 200 _diffrn_standards_interval_time ? _diffrn_standards_decay_% n/a _diffrn_reflns_number 4475 _diffrn_reflns_av_R_equivalents 0.017 _diffrn_reflns_av_sigmaI/netI 0.032 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -2 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 22.00 _reflns_number_total 4308 _reflns_number_gt 3488 _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^)+(0.0407P)^2^+2.5132P] 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 4308 _refine_ls_number_parameters 340 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.051 _refine_ls_R_factor_gt 0.034 _refine_ls_wR_factor_ref 0.089 _refine_ls_wR_factor_gt 0.080 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _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 0.72816(2) 0.13974(4) 0.261017(19) 0.02664(14) Uani 1 1 d . . . Si1 Si 0.81991(7) -0.10587(10) 0.41327(5) 0.0457(3) Uani 1 1 d . . . Si2 Si 0.72475(6) -0.07295(10) 0.11620(5) 0.0425(3) Uani 1 1 d . . . Si3 Si 0.92885(6) 0.33543(10) 0.30213(6) 0.0472(3) Uani 1 1 d . . . Si4 Si 0.59347(6) 0.37828(10) 0.12039(5) 0.0413(3) Uani 1 1 d . . . C1 C 0.76194(19) -0.0412(3) 0.32575(16) 0.0319(8) Uani 1 1 d . . . B2 B 0.7933(2) -0.0416(4) 0.26692(19) 0.0327(9) Uani 1 1 d . . . H2 H 0.8565 -0.0599 0.2724 0.039 Uiso 1 1 calc R . . C3 C 0.71535(18) -0.0286(3) 0.19823(15) 0.0310(7) Uani 1 1 d . . . B4 B 0.6370(2) -0.0038(4) 0.2114(2) 0.0348(9) Uani 1 1 d . . . H4 H 0.5747 0.0048 0.1730 0.042 Uiso 1 1 calc R . . B5 B 0.6701(2) -0.0032(4) 0.2990(2) 0.0353(9) Uani 1 1 d . . . H5 H 0.6341 0.0091 0.3311 0.042 Uiso 1 1 calc R . . B6 B 0.7015(2) -0.1298(4) 0.25772(19) 0.0364(9) Uani 1 1 d . . . H6 H 0.6877 -0.2360 0.2551 0.044 Uiso 1 1 calc R . . C11 C 0.81980(18) 0.3009(3) 0.28530(16) 0.0311(8) Uani 1 1 d . . . B12 B 0.7594(2) 0.2907(4) 0.20744(19) 0.0323(9) Uani 1 1 d . . . H12 H 0.7772 0.2798 0.1631 0.039 Uiso 1 1 calc R . . C13 C 0.67107(18) 0.3235(3) 0.20407(15) 0.0304(7) Uani 1 1 d . . . B14 B 0.6746(2) 0.3105(3) 0.27791(18) 0.0281(8) Uani 1 1 d . . . B15 B 0.7734(2) 0.3061(3) 0.33382(19) 0.0310(9) Uani 1 1 d . . . B16 B 0.7442(2) 0.4166(4) 0.26126(19) 0.0321(9) Uani 1 1 d . . . H16 H 0.7490 0.5248 0.2613 0.038 Uiso 1 1 calc R . . C21 C 0.9290(3) -0.1234(5) 0.4285(2) 0.0928(17) Uani 1 1 d . . . H21A H 0.9523 -0.0376 0.4296 0.139 Uiso 1 1 calc R . . H21B H 0.9346 -0.1747 0.3922 0.139 Uiso 1 1 calc R . . H21C H 0.9565 -0.1670 0.4716 0.139 Uiso 1 1 calc R . . C22 C 0.8071(4) -0.0006(4) 0.4800(2) 0.0933(18) Uani 1 1 d . . . H22A H 0.8383 -0.0362 0.5246 0.140 Uiso 1 1 calc R . . H22B H 0.7507 0.0020 0.4736 0.140 Uiso 1 1 calc R . . H22C H 0.8256 0.0872 0.4766 0.140 Uiso 1 1 calc R . . C23 C 0.7799(3) -0.2726(4) 0.4201(2) 0.0769(14) Uani 1 1 d . . . H23A H 0.8091 -0.3076 0.4652 0.115 Uiso 1 1 calc R . . H23B H 0.7868 -0.3301 0.3864 0.115 Uiso 1 1 calc R . . H23C H 0.7232 -0.2663 0.4122 0.115 Uiso 1 1 calc R . . C24 C 0.6322(2) -0.0242(5) 0.04144(19) 0.0743(14) Uani 1 1 d . . . H24A H 0.6381 -0.0499 -0.0003 0.111 Uiso 1 1 calc R . . H24B H 0.6252 0.0697 0.0417 0.111 Uiso 1 1 calc R . . H24C H 0.5856 -0.0673 0.0444 0.111 Uiso 1 1 calc R . . C25 C 0.8145(2) 0.0097(4) 0.10985(18) 0.0555(10) Uani 1 1 d . . . H25A H 0.8617 -0.0096 0.1502 0.083 Uiso 1 1 calc R . . H25B H 0.8057 0.1033 0.1062 0.083 Uiso 1 1 calc R . . H25C H 0.8227 -0.0219 0.0699 0.083 Uiso 1 1 calc R . . C26 C 0.7398(4) -0.2533(4) 0.1151(3) 0.0953(18) Uani 1 1 d . . . H26A H 0.7881 -0.2778 0.1533 0.143 Uiso 1 1 calc R . . H26B H 0.7454 -0.2778 0.0730 0.143 Uiso 1 1 calc R . . H26C H 0.6938 -0.2979 0.1184 0.143 Uiso 1 1 calc R . . C27 C 0.9538(3) 0.4995(4) 0.3446(3) 0.0913(17) Uani 1 1 d . . . H27A H 0.9469 0.4965 0.3876 0.137 Uiso 1 1 calc R . . H27B H 0.9183 0.5651 0.3155 0.137 Uiso 1 1 calc R . . H27C H 1.0092 0.5215 0.3525 0.137 Uiso 1 1 calc R . . C28 C 0.9468(3) 0.3448(5) 0.2212(2) 0.0902(16) Uani 1 1 d . . . H28A H 1.0028 0.3658 0.2313 0.135 Uiso 1 1 calc R . . H28B H 0.9129 0.4121 0.1922 0.135 Uiso 1 1 calc R . . H28C H 0.9341 0.2613 0.1979 0.135 Uiso 1 1 calc R . . C29 C 0.9963(2) 0.2045(5) 0.3553(3) 0.0835(15) Uani 1 1 d . . . H29A H 0.9765 0.1197 0.3357 0.125 Uiso 1 1 calc R . . H29B H 0.9972 0.2087 0.4011 0.125 Uiso 1 1 calc R . . H29C H 1.0504 0.2171 0.3565 0.125 Uiso 1 1 calc R . . C30 C 0.5047(2) 0.2642(4) 0.0876(2) 0.0656(12) Uani 1 1 d . . . H30A H 0.4708 0.2885 0.0415 0.098 Uiso 1 1 calc R . . H30B H 0.4739 0.2702 0.1164 0.098 Uiso 1 1 calc R . . H30C H 0.5235 0.1753 0.0881 0.098 Uiso 1 1 calc R . . C31 C 0.5531(2) 0.5449(4) 0.12811(19) 0.0595(11) Uani 1 1 d . . . H31A H 0.5964 0.5989 0.1581 0.089 Uiso 1 1 calc R . . H31B H 0.5116 0.5363 0.1466 0.089 Uiso 1 1 calc R . . H31C H 0.5304 0.5853 0.0836 0.089 Uiso 1 1 calc R . . C32 C 0.6399(3) 0.3907(4) 0.05514(18) 0.0647(12) Uani 1 1 d . . . H32A H 0.6546 0.3042 0.0452 0.097 Uiso 1 1 calc R . . H32B H 0.6876 0.4451 0.0726 0.097 Uiso 1 1 calc R . . H32C H 0.6016 0.4292 0.0139 0.097 Uiso 1 1 calc R . . N41 N 0.61168(14) 0.3450(2) 0.31051(13) 0.0324(6) Uani 1 1 d . . . N42 N 0.79170(15) 0.3203(3) 0.40539(13) 0.0381(7) Uani 1 1 d . . . C43 C 0.6457(2) 0.2973(3) 0.38409(16) 0.0409(9) Uani 1 1 d . . . H43A H 0.6071 0.3187 0.4049 0.049 Uiso 1 1 calc R . . H43B H 0.6503 0.2019 0.3839 0.049 Uiso 1 1 calc R . . C44 C 0.7271(2) 0.3530(3) 0.42846(17) 0.0433(9) Uani 1 1 d . . . H44A H 0.7226 0.4483 0.4297 0.052 Uiso 1 1 calc R . . H44B H 0.7414 0.3205 0.4749 0.052 Uiso 1 1 calc R . . C45 C 0.5989(2) 0.4911(3) 0.30903(19) 0.0457(9) Uani 1 1 d . . . H45A H 0.5753 0.5206 0.2622 0.069 Uiso 1 1 calc R . . H45B H 0.6501 0.5344 0.3319 0.069 Uiso 1 1 calc R . . H45C H 0.5630 0.5120 0.3320 0.069 Uiso 1 1 calc R . . C46 C 0.53209(19) 0.2794(4) 0.27416(19) 0.0464(9) Uani 1 1 d . . . H46A H 0.4968 0.2966 0.2982 0.070 Uiso 1 1 calc R . . H46B H 0.5401 0.1860 0.2725 0.070 Uiso 1 1 calc R . . H46C H 0.5079 0.3134 0.2282 0.070 Uiso 1 1 calc R . . C47 C 0.8725(2) 0.3357(4) 0.45844(18) 0.0628(12) Uani 1 1 d . . . H47A H 0.9118 0.2950 0.4437 0.094 Uiso 1 1 calc R . . H47B H 0.8742 0.2945 0.5000 0.094 Uiso 1 1 calc R . . H47C H 0.8847 0.4280 0.4666 0.094 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 0.0263(2) 0.0235(2) 0.0331(2) -0.00045(18) 0.01465(18) -0.00096(18) Si1 0.0638(7) 0.0342(6) 0.0368(6) 0.0044(5) 0.0164(5) -0.0007(5) Si2 0.0507(6) 0.0423(6) 0.0412(6) -0.0109(5) 0.0249(5) -0.0080(5) Si3 0.0263(5) 0.0456(6) 0.0721(7) -0.0002(5) 0.0214(5) -0.0036(5) Si4 0.0390(6) 0.0421(6) 0.0362(5) 0.0017(5) 0.0068(4) 0.0018(5) C1 0.042(2) 0.0213(17) 0.0368(19) -0.0004(14) 0.0194(16) -0.0005(15) B2 0.032(2) 0.025(2) 0.041(2) -0.0014(17) 0.0152(18) 0.0007(17) C3 0.0353(18) 0.0244(17) 0.0355(19) -0.0013(15) 0.0159(15) -0.0052(14) B4 0.034(2) 0.027(2) 0.044(2) 0.0001(18) 0.0151(18) -0.0065(17) B5 0.042(2) 0.024(2) 0.046(2) 0.0013(18) 0.025(2) -0.0018(17) B6 0.042(2) 0.029(2) 0.042(2) -0.0023(18) 0.0203(19) -0.0063(18) C11 0.0257(18) 0.0226(17) 0.047(2) 0.0018(15) 0.0160(15) -0.0008(14) B12 0.037(2) 0.025(2) 0.040(2) 0.0013(17) 0.0197(19) 0.0012(17) C13 0.0304(18) 0.0243(17) 0.0370(18) -0.0006(14) 0.0135(15) -0.0020(14) B14 0.027(2) 0.0237(19) 0.036(2) -0.0018(16) 0.0155(17) -0.0013(16) B15 0.027(2) 0.022(2) 0.045(2) -0.0009(17) 0.0144(18) -0.0016(16) B16 0.029(2) 0.024(2) 0.043(2) 0.0014(18) 0.0140(18) -0.0007(16) C21 0.063(3) 0.128(5) 0.067(3) 0.031(3) 0.002(2) 0.006(3) C22 0.180(6) 0.059(3) 0.047(3) 0.002(2) 0.051(3) 0.019(3) C23 0.115(4) 0.047(3) 0.061(3) 0.017(2) 0.025(3) -0.013(3) C24 0.062(3) 0.113(4) 0.040(2) -0.018(2) 0.011(2) -0.014(3) C25 0.053(2) 0.078(3) 0.044(2) -0.001(2) 0.0281(19) -0.003(2) C26 0.169(5) 0.052(3) 0.113(4) -0.018(3) 0.108(4) -0.008(3) C27 0.055(3) 0.065(3) 0.156(5) -0.029(3) 0.043(3) -0.025(2) C28 0.055(3) 0.128(5) 0.108(4) 0.003(3) 0.054(3) -0.015(3) C29 0.041(2) 0.086(4) 0.119(4) 0.014(3) 0.024(3) 0.016(2) C30 0.051(3) 0.068(3) 0.057(3) -0.003(2) -0.004(2) -0.011(2) C31 0.060(3) 0.055(3) 0.051(2) 0.008(2) 0.007(2) 0.011(2) C32 0.073(3) 0.080(3) 0.036(2) 0.008(2) 0.015(2) 0.005(2) N41 0.0296(15) 0.0293(15) 0.0435(16) -0.0023(13) 0.0198(13) 0.0017(12) N42 0.0332(16) 0.0443(17) 0.0319(16) -0.0052(13) 0.0068(13) -0.0022(13) C43 0.047(2) 0.041(2) 0.045(2) -0.0013(17) 0.0286(18) -0.0014(17) C44 0.051(2) 0.042(2) 0.039(2) -0.0063(17) 0.0189(18) -0.0029(18) C45 0.047(2) 0.032(2) 0.067(2) -0.0010(18) 0.032(2) 0.0092(17) C46 0.0280(19) 0.050(2) 0.065(2) -0.0062(19) 0.0221(18) -0.0054(17) C47 0.050(2) 0.086(3) 0.044(2) -0.006(2) 0.0073(19) 0.000(2) _cod_database_code 1100797