#------------------------------------------------------------------------------ #$Date: 2008-01-14 00:15:36 +0200 (Mon, 14 Jan 2008) $ #$Revision: 14 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/1100793.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_1100793 _journal_name Organometallics _chemical_formula_sum 'C22 H60 B8 Fe2 N2 Si4' _chemical_formula_weight 663.26 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' 'Si' 'Si' 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Fe' 'Fe' 0.3463 0.8444 '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' _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 12.574(1) _cell_length_b 16.472(1) _cell_length_c 18.363(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.06(1) _cell_angle_gamma 90.00 _cell_volume 3800.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 228(2) _cell_measurement_reflns_used 39 _cell_measurement_theta_min 5.0 _cell_measurement_theta_max 10.0 _exptl_crystal_description plates _exptl_crystal_colour 'dark-green' _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.159 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1416 _exptl_absorpt_coefficient_mu 0.905 _exptl_absorpt_correction_type 'psi scan' _exptl_absorpt_correction_T_min 0.742 _exptl_absorpt_correction_T_max 0.876 _exptl_absorpt_process_details 'Siemens XEMP' _diffrn_ambient_temperature 228(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 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count 147 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3.26 _diffrn_reflns_number 4887 _diffrn_reflns_av_R_equivalents 0.026 _diffrn_reflns_av_sigmaI/netI 0.041 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 22.00 _reflns_number_total 4635 _reflns_number_gt 3807 _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^)+(0.0211P)^2^+5.7999P] 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 SHELXL _refine_ls_extinction_coef 0.00142(17) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 4635 _refine_ls_number_parameters 360 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.051 _refine_ls_R_factor_gt 0.037 _refine_ls_wR_factor_ref 0.090 _refine_ls_wR_factor_gt 0.084 _refine_ls_goodness_of_fit_ref 1.075 _refine_ls_restrained_S_all 1.075 _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 Fe1 Fe 0.73819(4) 0.94669(3) 0.19113(3) 0.02561(16) Uani 1 1 d . . . Fe2 Fe 0.73834(4) 1.01867(3) 0.06237(3) 0.02873(17) Uani 1 1 d . . . Si1 Si 0.82445(10) 0.73621(8) 0.15495(6) 0.0458(3) Uani 1 1 d . . . Si2 Si 0.93747(10) 0.84823(9) 0.33074(7) 0.0534(4) Uani 1 1 d . . . Si3 Si 0.67281(10) 1.09418(8) 0.32953(6) 0.0429(3) Uani 1 1 d . . . Si4 Si 0.53339(10) 0.87922(8) 0.33203(7) 0.0465(3) Uani 1 1 d . . . C1 C 0.8377(3) 0.8472(2) 0.1787(2) 0.0333(9) Uani 1 1 d . . . C2 C 0.8742(3) 0.8929(2) 0.2452(2) 0.0343(10) Uani 1 1 d . . . B3 B 0.8930(3) 0.9853(3) 0.2282(3) 0.0385(12) Uani 1 1 d . . . H3 H 0.9193 1.0326 0.2672 0.046 Uiso 1 1 calc R . . B4 B 0.8773(3) 0.9943(3) 0.1384(2) 0.0320(11) Uani 1 1 d . . . H4 H 0.8964 1.0524 0.1059 0.038 Uiso 1 1 d . . . B5 B 0.8373(3) 0.9021(3) 0.1086(2) 0.0323(11) Uani 1 1 d . . . H5 H 0.8288 0.8761 0.0513 0.039 Uiso 1 1 d . . . B6 B 0.9490(4) 0.9101(3) 0.1697(2) 0.0399(12) Uani 1 1 d . . . H6 H 1.0328 0.8963 0.1597 0.048 Uiso 1 1 calc R . . C11 C 0.6462(3) 1.0196(2) 0.25416(19) 0.0283(9) Uani 1 1 d . . . C12 C 0.6020(3) 0.9356(2) 0.25715(19) 0.0291(9) Uani 1 1 d . . . B13 B 0.5763(3) 0.9000(3) 0.1794(2) 0.0312(10) Uani 1 1 d . . . H13 H 0.5436 0.8396 0.1662 0.037 Uiso 1 1 calc R . . B14 B 0.5979(3) 0.9752(3) 0.1215(2) 0.0298(10) Uani 1 1 d . . . H14 H 0.5756 0.9740 0.0590 0.036 Uiso 1 1 d . . . B15 B 0.6466(3) 1.0525(3) 0.1732(2) 0.0320(10) Uani 1 1 d . . . H15 H 0.6609 1.1222 0.1599 0.038 Uiso 1 1 d . . . B16 B 0.5314(3) 1.0012(3) 0.2005(2) 0.0338(11) Uani 1 1 d . . . H16 H 0.4500 1.0253 0.2034 0.041 Uiso 1 1 calc R . . C21 C 0.7110(4) 0.7248(3) 0.0879(2) 0.0565(13) Uani 1 1 d . . . H21A H 0.6956 0.6682 0.0809 0.085 Uiso 1 1 calc R . . H21B H 0.7293 0.7486 0.0423 0.085 Uiso 1 1 calc R . . H21C H 0.6495 0.7517 0.1059 0.085 Uiso 1 1 calc R . . C22 C 0.9490(4) 0.7033(3) 0.1102(3) 0.0717(16) Uani 1 1 d . . . H22A H 0.9424 0.6474 0.0957 0.108 Uiso 1 1 calc R . . H22B H 1.0087 0.7092 0.1438 0.108 Uiso 1 1 calc R . . H22C H 0.9597 0.7363 0.0680 0.108 Uiso 1 1 calc R . . C23 C 0.7989(5) 0.6648(3) 0.2314(3) 0.0840(19) Uani 1 1 d . . . H23A H 0.7294 0.6748 0.2494 0.126 Uiso 1 1 calc R . . H23B H 0.8514 0.6730 0.2700 0.126 Uiso 1 1 calc R . . H23C H 0.8028 0.6099 0.2142 0.126 Uiso 1 1 calc R . . C24 C 1.0350(5) 0.7689(4) 0.3037(3) 0.103(2) Uani 1 1 d . . . H24A H 1.0656 0.7435 0.3466 0.154 Uiso 1 1 calc R . . H24B H 1.0903 0.7937 0.2767 0.154 Uiso 1 1 calc R . . H24C H 0.9991 0.7287 0.2739 0.154 Uiso 1 1 calc R . . C25 C 1.0167(4) 0.9260(4) 0.3826(3) 0.093(2) Uani 1 1 d . . . H25A H 0.9708 0.9695 0.3964 0.140 Uiso 1 1 calc R . . H25B H 1.0712 0.9469 0.3525 0.140 Uiso 1 1 calc R . . H25C H 1.0488 0.9017 0.4255 0.140 Uiso 1 1 calc R . . C26 C 0.8404(4) 0.8038(3) 0.3935(3) 0.0764(17) Uani 1 1 d . . . H26A H 0.8781 0.7778 0.4335 0.115 Uiso 1 1 calc R . . H26B H 0.7970 0.7645 0.3677 0.115 Uiso 1 1 calc R . . H26C H 0.7960 0.8460 0.4117 0.115 Uiso 1 1 calc R . . C27 C 0.7616(4) 1.0531(4) 0.4045(3) 0.0732(16) Uani 1 1 d . . . H27A H 0.8346 1.0617 0.3929 0.110 Uiso 1 1 calc R . . H27B H 0.7488 0.9961 0.4100 0.110 Uiso 1 1 calc R . . H27C H 0.7471 1.0806 0.4492 0.110 Uiso 1 1 calc R . . C28 C 0.7431(4) 1.1834(3) 0.2917(3) 0.0687(15) Uani 1 1 d . . . H28A H 0.7731 1.2155 0.3309 0.103 Uiso 1 1 calc R . . H28B H 0.6936 1.2157 0.2632 0.103 Uiso 1 1 calc R . . H28C H 0.7989 1.1649 0.2614 0.103 Uiso 1 1 calc R . . C29 C 0.5419(4) 1.1282(3) 0.3645(3) 0.0623(14) Uani 1 1 d . . . H29A H 0.5540 1.1664 0.4034 0.093 Uiso 1 1 calc R . . H29B H 0.5040 1.0821 0.3823 0.093 Uiso 1 1 calc R . . H29C H 0.5007 1.1534 0.3258 0.093 Uiso 1 1 calc R . . C30 C 0.5579(4) 0.7682(3) 0.3211(3) 0.0731(16) Uani 1 1 d . . . H30A H 0.6259 0.7601 0.3001 0.110 Uiso 1 1 calc R . . H30B H 0.5032 0.7453 0.2896 0.110 Uiso 1 1 calc R . . H30C H 0.5571 0.7422 0.3678 0.110 Uiso 1 1 calc R . . C31 C 0.5664(5) 0.9068(4) 0.4288(2) 0.0773(17) Uani 1 1 d . . . H31A H 0.5263 0.8732 0.4605 0.116 Uiso 1 1 calc R . . H31B H 0.5489 0.9628 0.4367 0.116 Uiso 1 1 calc R . . H31C H 0.6411 0.8987 0.4390 0.116 Uiso 1 1 calc R . . C32 C 0.3870(4) 0.8982(4) 0.3185(3) 0.0774(17) Uani 1 1 d . . . H32A H 0.3486 0.8645 0.3512 0.116 Uiso 1 1 calc R . . H32B H 0.3653 0.8857 0.2691 0.116 Uiso 1 1 calc R . . H32C H 0.3721 0.9542 0.3283 0.116 Uiso 1 1 calc R . . N41 N 0.7552(2) 0.98390(19) -0.05319(15) 0.0319(7) Uani 1 1 d . . . N42 N 0.7149(3) 1.14032(19) 0.01132(16) 0.0359(8) Uani 1 1 d . . . C43 C 0.7157(3) 1.0542(3) -0.0969(2) 0.0422(11) Uani 1 1 d . . . H43A H 0.6385 1.0533 -0.0998 0.051 Uiso 1 1 calc R . . H43B H 0.7411 1.0501 -0.1460 0.051 Uiso 1 1 calc R . . C44 C 0.7526(4) 1.1323(3) -0.0636(2) 0.0484(11) Uani 1 1 d . . . H44A H 0.8297 1.1343 -0.0626 0.058 Uiso 1 1 calc R . . H44B H 0.7259 1.1772 -0.0931 0.058 Uiso 1 1 calc R . . C45 C 0.8678(3) 0.9676(3) -0.0701(2) 0.0475(12) Uani 1 1 d . . . H45A H 0.8922 0.9202 -0.0442 0.071 Uiso 1 1 calc R . . H45B H 0.9109 1.0133 -0.0556 0.071 Uiso 1 1 calc R . . H45C H 0.8730 0.9588 -0.1216 0.071 Uiso 1 1 calc R . . C46 C 0.6909(3) 0.9123(3) -0.0739(2) 0.0431(11) Uani 1 1 d . . . H46A H 0.6172 0.9233 -0.0660 0.065 Uiso 1 1 calc R . . H46B H 0.7137 0.8666 -0.0448 0.065 Uiso 1 1 calc R . . H46C H 0.6999 0.9002 -0.1245 0.065 Uiso 1 1 calc R . . C47 C 0.7772(4) 1.2051(3) 0.0490(3) 0.0586(13) Uani 1 1 d . . . H47A H 0.8514 1.1915 0.0494 0.088 Uiso 1 1 calc R . . H47B H 0.7546 1.2102 0.0982 0.088 Uiso 1 1 calc R . . H47C H 0.7659 1.2556 0.0239 0.088 Uiso 1 1 calc R . . C48 C 0.6012(3) 1.1646(3) 0.0090(2) 0.0492(12) Uani 1 1 d . . . H48A H 0.5937 1.2167 -0.0141 0.074 Uiso 1 1 calc R . . H48B H 0.5763 1.1677 0.0577 0.074 Uiso 1 1 calc R . . H48C H 0.5601 1.1251 -0.0183 0.074 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 Fe1 0.0226(3) 0.0321(3) 0.0222(3) 0.0028(2) 0.0015(2) 0.0005(2) Fe2 0.0287(3) 0.0350(3) 0.0226(3) 0.0051(2) 0.0022(2) -0.0001(2) Si1 0.0610(8) 0.0385(7) 0.0388(7) 0.0045(6) 0.0128(6) 0.0109(6) Si2 0.0478(7) 0.0786(10) 0.0332(7) 0.0123(7) -0.0065(6) 0.0197(7) Si3 0.0456(7) 0.0488(8) 0.0346(6) -0.0133(6) 0.0035(5) -0.0010(6) Si4 0.0465(7) 0.0547(8) 0.0394(7) 0.0154(6) 0.0154(6) -0.0008(6) C1 0.028(2) 0.043(3) 0.030(2) 0.0082(19) 0.0049(17) 0.0081(18) C2 0.028(2) 0.048(3) 0.027(2) 0.0047(19) 0.0016(17) 0.0069(19) B3 0.024(2) 0.056(3) 0.036(3) 0.002(2) -0.002(2) -0.004(2) B4 0.021(2) 0.041(3) 0.035(3) 0.011(2) 0.0057(19) -0.001(2) B5 0.028(2) 0.044(3) 0.025(2) 0.006(2) 0.0057(19) 0.008(2) B6 0.029(3) 0.060(3) 0.031(3) 0.011(2) 0.003(2) -0.001(2) C11 0.0225(19) 0.033(2) 0.029(2) 0.0016(18) 0.0007(16) 0.0027(17) C12 0.024(2) 0.036(2) 0.027(2) 0.0052(18) 0.0038(16) 0.0004(17) B13 0.026(2) 0.034(3) 0.033(3) -0.002(2) 0.0027(19) 0.000(2) B14 0.024(2) 0.043(3) 0.023(2) -0.001(2) -0.0012(18) 0.003(2) B15 0.026(2) 0.039(3) 0.031(2) 0.001(2) 0.0049(19) 0.003(2) B16 0.026(2) 0.046(3) 0.030(2) 0.002(2) -0.001(2) 0.003(2) C21 0.062(3) 0.050(3) 0.058(3) -0.014(2) 0.015(2) -0.006(2) C22 0.082(4) 0.073(4) 0.060(3) -0.008(3) 0.008(3) 0.033(3) C23 0.149(6) 0.044(3) 0.061(3) 0.012(3) 0.026(4) 0.010(3) C24 0.092(4) 0.153(6) 0.062(4) 0.015(4) -0.014(3) 0.078(4) C25 0.074(4) 0.133(6) 0.069(4) 0.013(4) -0.038(3) 0.003(4) C26 0.094(4) 0.091(4) 0.044(3) 0.027(3) 0.004(3) 0.007(3) C27 0.073(4) 0.100(4) 0.046(3) -0.016(3) -0.009(3) 0.001(3) C28 0.077(4) 0.054(3) 0.076(4) -0.025(3) 0.010(3) -0.019(3) C29 0.071(3) 0.068(4) 0.049(3) -0.015(3) 0.016(3) 0.009(3) C30 0.095(4) 0.056(3) 0.070(4) 0.026(3) 0.012(3) -0.014(3) C31 0.098(4) 0.092(4) 0.043(3) 0.019(3) 0.023(3) 0.012(4) C32 0.050(3) 0.103(5) 0.082(4) 0.035(3) 0.032(3) -0.005(3) N41 0.0323(18) 0.0380(19) 0.0255(17) 0.0033(15) 0.0028(14) -0.0020(15) N42 0.044(2) 0.0311(19) 0.0325(19) 0.0019(15) -0.0021(15) -0.0062(16) C43 0.048(3) 0.051(3) 0.028(2) 0.005(2) -0.0020(19) -0.001(2) C44 0.060(3) 0.049(3) 0.037(2) 0.014(2) 0.005(2) -0.007(2) C45 0.036(2) 0.075(3) 0.033(2) 0.004(2) 0.0116(19) 0.000(2) C46 0.050(3) 0.048(3) 0.031(2) -0.009(2) 0.001(2) -0.004(2) C47 0.080(4) 0.040(3) 0.055(3) 0.000(2) -0.006(3) -0.020(3) C48 0.059(3) 0.039(3) 0.049(3) 0.012(2) 0.002(2) 0.012(2)