#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/4/4060155.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_4060155 _journal_name_full 'Organometallics' _journal_year 2005 _chemical_formula_sum 'C32 H52 O2 Si2 Zr' _chemical_formula_weight 616.14 _symmetry_cell_setting Monoclinic _space_group_IT_number 7 _symmetry_space_group_name_Hall 'P -2yac' _symmetry_space_group_name_H-M 'P 1 n 1' _[local]_cod_cif_authors_sg_H-M 'P n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 12.2632(7) _cell_length_b 10.4353(6) _cell_length_c 13.2677(7) _cell_angle_alpha 90.00 _cell_angle_beta 94.0280(10) _cell_angle_gamma 90.00 _cell_volume 1693.68(16) _cell_formula_units_Z 2 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 7525 _cell_measurement_theta_min 2.345 _cell_measurement_theta_max 27.661 _exptl_crystal_description PLATE _exptl_crystal_colour GREEN _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.208 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 0.420 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.8844 _exptl_absorpt_correction_T_max 0.9207 _exptl_absorpt_process_details SADABS _diffrn_ambient_temperature 243(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10875 _diffrn_reflns_av_R_equivalents 0.0200 _diffrn_reflns_av_sigmaI/netI 0.0212 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 27.95 _reflns_number_total 4390 _reflns_number_gt 4217 _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^)+(0.0445P)^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 SHELXL _refine_ls_extinction_coef 0.0002(4) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.35(4) _refine_ls_number_reflns 4390 _refine_ls_number_parameters 336 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0261 _refine_ls_R_factor_gt 0.0246 _refine_ls_wR_factor_ref 0.0674 _refine_ls_wR_factor_gt 0.0665 _refine_ls_goodness_of_fit_ref 1.118 _refine_ls_restrained_S_all 1.117 _refine_ls_shift/su_max 0.163 _refine_ls_shift/su_mean 0.031 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 Zr Zr 0.82942(2) 0.73922(2) 0.63829(3) 0.03456(8) Uani 1 1 d . . . C1 C 0.9078(4) 0.9206(3) 0.6791(3) 0.0707(12) Uani 1 1 d . . . O1 O 0.9487(4) 1.0185(3) 0.6934(3) 0.1120(13) Uani 1 1 d . . . C2 C 0.6979(4) 0.8602(6) 0.5818(4) 0.103(2) Uani 1 1 d . . . O2 O 0.6288(4) 0.9272(6) 0.5557(5) 0.205(3) Uani 1 1 d . . . Si1 Si 0.88696(7) 0.40733(8) 0.55312(6) 0.03700(18) Uani 1 1 d . . . Si2 Si 0.81327(7) 0.38984(8) 0.71097(6) 0.03931(19) Uani 1 1 d . . . C11 C 0.9150(2) 0.5830(3) 0.5291(2) 0.0341(6) Uani 1 1 d . . . C12 C 1.0002(2) 0.6733(3) 0.5579(2) 0.0374(6) Uani 1 1 d . . . C13 C 0.9708(3) 0.7922(3) 0.5090(2) 0.0391(7) Uani 1 1 d . . . H13A H 1.0174 0.8697 0.5112 0.047 Uiso 1 1 calc R . . C14 C 0.8723(3) 0.7791(4) 0.4494(3) 0.0433(8) Uani 1 1 d . . . C15 C 0.8357(2) 0.6526(3) 0.4642(2) 0.0403(7) Uani 1 1 d . . . H15A H 0.7728 0.6126 0.4252 0.048 Uiso 1 1 calc R . . C21 C 0.7715(2) 0.5589(3) 0.7460(2) 0.0356(6) Uani 1 1 d . . . C22 C 0.8507(2) 0.6313(3) 0.8084(2) 0.0371(6) Uani 1 1 d . . . H22A H 0.9203 0.5961 0.8392 0.045 Uiso 1 1 calc R . . C23 C 0.8082(4) 0.7519(3) 0.8312(3) 0.0432(9) Uani 1 1 d . . . C24 C 0.7029(3) 0.7581(3) 0.7822(3) 0.0427(9) Uani 1 1 d . . . H24A H 0.6507 0.8292 0.7898 0.051 Uiso 1 1 calc R . . C25 C 0.6767(2) 0.6412(3) 0.7309(2) 0.0391(7) Uani 1 1 d . . . C31 C 0.8330(3) 0.8739(3) 0.3666(2) 0.0565(9) Uani 1 1 d . . . C32 C 0.7185(5) 0.8382(5) 0.3216(4) 0.108(2) Uani 1 1 d . . . H32A H 0.6671 0.8425 0.3739 0.162 Uiso 1 1 calc R . . H32B H 0.7196 0.7518 0.2946 0.162 Uiso 1 1 calc R . . H32C H 0.6962 0.8977 0.2679 0.162 Uiso 1 1 calc R . . C33 C 0.9170(4) 0.8669(5) 0.2859(3) 0.0944(16) Uani 1 1 d . . . H33A H 0.9199 0.7800 0.2602 0.142 Uiso 1 1 calc R . . H33B H 0.9885 0.8912 0.3158 0.142 Uiso 1 1 calc R . . H33C H 0.8955 0.9249 0.2310 0.142 Uiso 1 1 calc R . . C34 C 0.8314(4) 1.0115(4) 0.4045(3) 0.0771(13) Uani 1 1 d . . . H34A H 0.7788 1.0193 0.4554 0.116 Uiso 1 1 calc R . . H34B H 0.8110 1.0684 0.3485 0.116 Uiso 1 1 calc R . . H34C H 0.9035 1.0346 0.4337 0.116 Uiso 1 1 calc R . . C35 C 0.8570(3) 0.8389(4) 0.9166(3) 0.0573(9) Uani 1 1 d . . . C36 C 0.8220(6) 0.7786(5) 1.0155(3) 0.0992(18) Uani 1 1 d . . . H36A H 0.8515 0.6926 1.0224 0.149 Uiso 1 1 calc R . . H36B H 0.7428 0.7751 1.0137 0.149 Uiso 1 1 calc R . . H36C H 0.8495 0.8303 1.0725 0.149 Uiso 1 1 calc R . . C37 C 0.8085(4) 0.9758(4) 0.9083(3) 0.0766(12) Uani 1 1 d . . . H37A H 0.8296 1.0159 0.8467 0.115 Uiso 1 1 calc R . . H37B H 0.8360 1.0262 0.9661 0.115 Uiso 1 1 calc R . . H37C H 0.7294 0.9710 0.9070 0.115 Uiso 1 1 calc R . . C38 C 0.9813(4) 0.8432(5) 0.9210(4) 0.0883(15) Uani 1 1 d . . . H38A H 1.0047 0.8805 0.8591 0.132 Uiso 1 1 calc R . . H38B H 1.0101 0.7569 0.9285 0.132 Uiso 1 1 calc R . . H38C H 1.0085 0.8949 0.9781 0.132 Uiso 1 1 calc R . . C41 C 1.1141(2) 0.6505(3) 0.6082(2) 0.0452(7) Uani 1 1 d . . . C42 C 1.1686(3) 0.7759(4) 0.6474(4) 0.0698(11) Uani 1 1 d . . . H42A H 1.1253 0.8137 0.6981 0.105 Uiso 1 1 calc R . . H42B H 1.1734 0.8353 0.5917 0.105 Uiso 1 1 calc R . . H42C H 1.2415 0.7574 0.6771 0.105 Uiso 1 1 calc R . . C43 C 1.1844(3) 0.5914(4) 0.5283(3) 0.0661(10) Uani 1 1 d . . . H43A H 1.1518 0.5112 0.5044 0.099 Uiso 1 1 calc R . . H43B H 1.2576 0.5755 0.5582 0.099 Uiso 1 1 calc R . . H43C H 1.1879 0.6502 0.4720 0.099 Uiso 1 1 calc R . . C44 C 1.1132(3) 0.5585(4) 0.6987(3) 0.0615(10) Uani 1 1 d . . . H44A H 1.0799 0.4779 0.6768 0.092 Uiso 1 1 calc R . . H44B H 1.0715 0.5963 0.7506 0.092 Uiso 1 1 calc R . . H44C H 1.1876 0.5432 0.7257 0.092 Uiso 1 1 calc R . . C45 C 0.5612(2) 0.6025(4) 0.6900(3) 0.0519(8) Uani 1 1 d . . . C46 C 0.4841(3) 0.7183(5) 0.6858(5) 0.0843(15) Uani 1 1 d . . . H46A H 0.5098 0.7817 0.6395 0.126 Uiso 1 1 calc R . . H46B H 0.4826 0.7555 0.7527 0.126 Uiso 1 1 calc R . . H46C H 0.4110 0.6909 0.6625 0.126 Uiso 1 1 calc R . . C47 C 0.5603(3) 0.5426(4) 0.5844(3) 0.0637(10) Uani 1 1 d . . . H47A H 0.6074 0.4679 0.5866 0.096 Uiso 1 1 calc R . . H47B H 0.5865 0.6048 0.5374 0.096 Uiso 1 1 calc R . . H47C H 0.4863 0.5174 0.5623 0.096 Uiso 1 1 calc R . . C48 C 0.5172(3) 0.5053(4) 0.7648(3) 0.0700(11) Uani 1 1 d . . . H48A H 0.5644 0.4307 0.7694 0.105 Uiso 1 1 calc R . . H48B H 0.4438 0.4795 0.7413 0.105 Uiso 1 1 calc R . . H48C H 0.5157 0.5447 0.8310 0.105 Uiso 1 1 calc R . . C51 C 1.0064(3) 0.2965(3) 0.5405(3) 0.0532(8) Uani 1 1 d . . . H51A H 1.0339 0.3071 0.4742 0.080 Uiso 1 1 calc R . . H51B H 0.9830 0.2086 0.5486 0.080 Uiso 1 1 calc R . . H51C H 1.0638 0.3169 0.5921 0.080 Uiso 1 1 calc R . . C52 C 0.7820(3) 0.3546(3) 0.4517(3) 0.0498(8) Uani 1 1 d . . . H52A H 0.8122 0.3618 0.3863 0.075 Uiso 1 1 calc R . . H52B H 0.7177 0.4086 0.4531 0.075 Uiso 1 1 calc R . . H52C H 0.7619 0.2662 0.4634 0.075 Uiso 1 1 calc R . . C53 C 0.9165(3) 0.3329(4) 0.8129(3) 0.0536(8) Uani 1 1 d . . . H53A H 0.8822 0.3273 0.8765 0.080 Uiso 1 1 calc R . . H53B H 0.9769 0.3930 0.8197 0.080 Uiso 1 1 calc R . . H53C H 0.9435 0.2492 0.7951 0.080 Uiso 1 1 calc R . . C54 C 0.7046(4) 0.2619(3) 0.7059(4) 0.0617(10) Uani 1 1 d . . . H54A H 0.6745 0.2551 0.7714 0.093 Uiso 1 1 calc R . . H54B H 0.7364 0.1805 0.6885 0.093 Uiso 1 1 calc R . . H54C H 0.6469 0.2844 0.6553 0.093 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 Zr 0.03554(12) 0.03098(12) 0.03684(11) -0.00093(14) 0.00035(8) 0.00420(13) C1 0.110(3) 0.0412(19) 0.066(2) -0.0113(17) 0.041(2) -0.016(2) O1 0.178(4) 0.0572(18) 0.109(2) -0.0347(17) 0.067(2) -0.054(2) C2 0.088(3) 0.121(4) 0.107(4) 0.067(3) 0.042(3) 0.059(3) O2 0.140(4) 0.263(6) 0.223(5) 0.172(5) 0.084(4) 0.153(4) Si1 0.0407(4) 0.0314(4) 0.0384(4) -0.0034(3) -0.0013(3) 0.0047(3) Si2 0.0431(4) 0.0331(4) 0.0415(4) 0.0005(3) 0.0008(3) -0.0011(4) C11 0.0379(14) 0.0301(14) 0.0341(14) -0.0011(11) 0.0018(11) 0.0046(12) C12 0.0355(14) 0.0414(16) 0.0354(14) -0.0063(12) 0.0033(11) 0.0021(12) C13 0.0494(18) 0.0340(15) 0.0343(14) -0.0016(13) 0.0054(13) -0.0052(14) C14 0.060(2) 0.0319(15) 0.0376(17) -0.0019(14) 0.0008(16) 0.0044(16) C15 0.0465(16) 0.0347(16) 0.0382(15) -0.0037(12) -0.0067(12) -0.0009(13) C21 0.0329(13) 0.0394(16) 0.0344(14) -0.0024(12) 0.0011(11) -0.0029(12) C22 0.0357(14) 0.0380(16) 0.0365(14) -0.0004(12) -0.0055(11) -0.0034(12) C23 0.0424(19) 0.050(2) 0.0368(17) -0.0073(12) -0.0012(14) -0.0046(13) C24 0.0440(18) 0.0392(19) 0.0452(18) -0.0058(13) 0.0063(15) 0.0069(12) C25 0.0356(14) 0.0441(17) 0.0374(14) -0.0064(13) -0.0002(11) -0.0023(13) C31 0.092(3) 0.0375(18) 0.0385(16) 0.0033(14) -0.0087(17) 0.0080(18) C32 0.140(4) 0.067(3) 0.105(4) 0.019(3) -0.074(3) 0.003(3) C33 0.164(5) 0.077(3) 0.0428(19) 0.013(2) 0.015(3) 0.026(3) C34 0.137(4) 0.037(2) 0.057(2) 0.0049(17) 0.002(2) 0.011(2) C35 0.066(2) 0.054(2) 0.0510(18) -0.0152(17) -0.0041(16) -0.0086(18) C36 0.150(5) 0.107(4) 0.0395(19) -0.017(2) -0.003(3) -0.045(3) C37 0.096(3) 0.064(3) 0.070(2) -0.032(2) 0.009(2) -0.003(2) C38 0.071(3) 0.085(3) 0.104(3) -0.037(3) -0.028(2) -0.014(2) C41 0.0295(14) 0.055(2) 0.0514(17) -0.0071(15) 0.0020(12) -0.0012(13) C42 0.0440(19) 0.076(3) 0.088(3) -0.024(2) -0.010(2) -0.0090(18) C43 0.0423(17) 0.085(3) 0.072(2) -0.014(2) 0.0081(16) 0.0100(18) C44 0.0433(18) 0.078(3) 0.060(2) 0.001(2) -0.0127(16) 0.0052(18) C45 0.0345(15) 0.062(2) 0.0592(19) -0.0147(17) 0.0005(13) 0.0033(15) C46 0.038(2) 0.093(3) 0.118(4) -0.026(3) -0.017(2) 0.018(2) C47 0.0465(18) 0.080(3) 0.062(2) -0.022(2) -0.0140(16) -0.0057(18) C48 0.0475(19) 0.083(3) 0.081(2) -0.014(2) 0.0161(18) -0.0191(19) C51 0.056(2) 0.0418(17) 0.062(2) -0.0012(16) 0.0045(16) 0.0148(16) C52 0.0562(18) 0.0389(17) 0.0532(18) -0.0120(14) -0.0029(15) -0.0018(14) C53 0.062(2) 0.050(2) 0.0480(17) 0.0080(15) -0.0028(16) 0.0091(17) C54 0.065(2) 0.044(2) 0.076(3) -0.0014(17) 0.007(2) -0.0118(15) _cod_database_code 4060155