#------------------------------------------------------------------------------ #$Date: 2014-07-23 10:49:31 +0100 (Wed, 23 Jul 2014) $ #$Revision: 120677 $ #$URL: svn://www.crystallography.net/cod/cif/4/06/01/4060152.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_4060152 _journal_name_full Organometallics _journal_year 2005 _chemical_formula_sum 'C30 H46 O2 Si Zr' _chemical_formula_weight 557.98 _space_group_IT_number 14 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 108.5860(10) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 15.0270(11) _cell_length_b 12.9006(10) _cell_length_c 16.5083(12) _cell_measurement_reflns_used ? _cell_measurement_temperature 233(2) _cell_measurement_theta_max ? _cell_measurement_theta_min ? _cell_volume 3033.3(4) _diffrn_ambient_temperature 233(2) _diffrn_detector_area_resol_mean ? _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0184 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_number 20766 _diffrn_reflns_theta_max 28.25 _diffrn_reflns_theta_min 1.60 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 0.424 _exptl_absorpt_correction_T_max 0.9199 _exptl_absorpt_correction_T_min 0.8832 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details SADABS _exptl_crystal_colour ? _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description ? _exptl_crystal_F_000 1184 _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _refine_ls_extinction_coef 0.00116(17) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 322 _refine_ls_number_reflns 6877 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.029 _refine_ls_R_factor_all 0.0330 _refine_ls_R_factor_gt 0.0256 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0378P)^2^+0.9099P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0689 _refine_ls_wR_factor_ref 0.0731 _reflns_number_gt 5750 _reflns_number_total 6877 _reflns_threshold_expression >2sigma(I) _[local]_cod_cif_authors_sg_H-M P2(1)/n _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 4060152 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 0.765954(9) 0.248393(10) 0.025076(8) 0.02736(6) Uani 1 1 d . . . Si Si 0.57598(3) 0.28963(4) -0.12692(3) 0.03543(10) Uani 1 1 d . . . O1 O 0.99808(11) 0.27697(15) 0.07396(13) 0.0807(5) Uani 1 1 d . . . O2 O 0.79727(10) 0.13057(11) 0.21116(8) 0.0571(3) Uani 1 1 d . . . C1 C 0.92033(13) 0.27256(14) 0.05865(12) 0.0446(4) Uani 1 1 d . . . C2 C 0.78941(10) 0.16925(12) 0.14874(10) 0.0352(3) Uani 1 1 d . . . C11 C 0.67094(10) 0.18896(12) -0.11357(9) 0.0328(3) Uani 1 1 d . . . C12 C 0.76590(11) 0.18933(12) -0.11860(9) 0.0341(3) Uani 1 1 d . . . C13 C 0.81601(11) 0.10968(12) -0.06309(10) 0.0350(3) Uani 1 1 d . . . H13A H 0.8820 0.0905 -0.0555 0.042 Uiso 1 1 calc R . . C14 C 0.75766(11) 0.05699(12) -0.02525(9) 0.0332(3) Uani 1 1 d . . . C15 C 0.66913(10) 0.10601(12) -0.05525(9) 0.0330(3) Uani 1 1 d . . . H15A H 0.6115 0.0799 -0.0454 0.040 Uiso 1 1 calc R . . C21 C 0.63081(10) 0.35990(12) -0.02268(10) 0.0331(3) Uani 1 1 d . . . C22 C 0.64134(10) 0.33888(12) 0.06649(10) 0.0335(3) Uani 1 1 d . . . C23 C 0.72525(11) 0.38903(12) 0.11613(10) 0.0351(3) Uani 1 1 d . . . H23A H 0.7484 0.3906 0.1794 0.042 Uiso 1 1 calc R . . C24 C 0.76617(11) 0.44404(12) 0.06330(10) 0.0354(3) Uani 1 1 d . . . C25 C 0.70939(11) 0.42491(12) -0.02119(10) 0.0343(3) Uani 1 1 d . . . H25A H 0.7168 0.4600 -0.0720 0.041 Uiso 1 1 calc R . . C31 C 0.80150(14) 0.23793(14) -0.18744(12) 0.0438(4) Uani 1 1 d . . . C32 C 0.7423(2) 0.1912(2) -0.27277(13) 0.0749(7) Uani 1 1 d . . . H32A H 0.6776 0.2135 -0.2857 0.112 Uiso 1 1 calc R . . H32B H 0.7452 0.1161 -0.2690 0.112 Uiso 1 1 calc R . . H32C H 0.7664 0.2142 -0.3177 0.112 Uiso 1 1 calc R . . C33 C 0.90440(17) 0.2085(3) -0.17227(17) 0.0828(8) Uani 1 1 d . . . H33A H 0.9261 0.2403 -0.2158 0.124 Uiso 1 1 calc R . . H33B H 0.9098 0.1337 -0.1750 0.124 Uiso 1 1 calc R . . H33C H 0.9425 0.2328 -0.1164 0.124 Uiso 1 1 calc R . . C34 C 0.79622(18) 0.35524(16) -0.19214(14) 0.0631(6) Uani 1 1 d . . . H34A H 0.7316 0.3771 -0.2037 0.095 Uiso 1 1 calc R . . H34B H 0.8190 0.3793 -0.2376 0.095 Uiso 1 1 calc R . . H34C H 0.8347 0.3844 -0.1382 0.095 Uiso 1 1 calc R . . C41 C 0.78058(12) -0.04671(13) 0.02061(10) 0.0409(4) Uani 1 1 d . . . C42 C 0.88172(13) -0.05045(16) 0.08083(13) 0.0540(5) Uani 1 1 d . . . H42A H 0.9244 -0.0356 0.0489 0.081 Uiso 1 1 calc R . . H42B H 0.8949 -0.1189 0.1061 0.081 Uiso 1 1 calc R . . H42C H 0.8900 0.0008 0.1256 0.081 Uiso 1 1 calc R . . C43 C 0.76929(19) -0.12809(15) -0.05044(13) 0.0672(6) Uani 1 1 d . . . H43A H 0.7054 -0.1264 -0.0893 0.101 Uiso 1 1 calc R . . H43B H 0.7828 -0.1965 -0.0251 0.101 Uiso 1 1 calc R . . H43C H 0.8126 -0.1126 -0.0816 0.101 Uiso 1 1 calc R . . C44 C 0.71279(14) -0.07362(15) 0.06932(12) 0.0516(4) Uani 1 1 d . . . H44A H 0.7191 -0.0232 0.1144 0.077 Uiso 1 1 calc R . . H44B H 0.7272 -0.1422 0.0941 0.077 Uiso 1 1 calc R . . H44C H 0.6489 -0.0725 0.0304 0.077 Uiso 1 1 calc R . . C51 C 0.56628(12) 0.29993(15) 0.10470(11) 0.0424(4) Uani 1 1 d . . . C52 C 0.54123(14) 0.18538(17) 0.08839(14) 0.0579(5) Uani 1 1 d . . . H52A H 0.5967 0.1435 0.1139 0.087 Uiso 1 1 calc R . . H52B H 0.5178 0.1727 0.0273 0.087 Uiso 1 1 calc R . . H52C H 0.4932 0.1672 0.1136 0.087 Uiso 1 1 calc R . . C53 C 0.59980(15) 0.3171(2) 0.20160(12) 0.0620(6) Uani 1 1 d . . . H53A H 0.6125 0.3901 0.2137 0.093 Uiso 1 1 calc R . . H53B H 0.6567 0.2775 0.2274 0.093 Uiso 1 1 calc R . . H53C H 0.5514 0.2944 0.2250 0.093 Uiso 1 1 calc R . . C54 C 0.47795(14) 0.3656(2) 0.06560(15) 0.0675(6) Uani 1 1 d . . . H54A H 0.4308 0.3470 0.0917 0.101 Uiso 1 1 calc R . . H54B H 0.4536 0.3530 0.0046 0.101 Uiso 1 1 calc R . . H54C H 0.4936 0.4385 0.0758 0.101 Uiso 1 1 calc R . . C61 C 0.84237(13) 0.52621(13) 0.09264(11) 0.0445(4) Uani 1 1 d . . . C62 C 0.91545(16) 0.49849(18) 0.17839(14) 0.0692(6) Uani 1 1 d . . . H62A H 0.8843 0.4876 0.2209 0.104 Uiso 1 1 calc R . . H62B H 0.9603 0.5547 0.1965 0.104 Uiso 1 1 calc R . . H62C H 0.9480 0.4356 0.1720 0.104 Uiso 1 1 calc R . . C63 C 0.79207(17) 0.62589(15) 0.10425(15) 0.0623(5) Uani 1 1 d . . . H63A H 0.7452 0.6443 0.0505 0.094 Uiso 1 1 calc R . . H63B H 0.8374 0.6816 0.1223 0.094 Uiso 1 1 calc R . . H63C H 0.7617 0.6148 0.1473 0.094 Uiso 1 1 calc R . . C64 C 0.89047(16) 0.54583(18) 0.02548(15) 0.0640(6) Uani 1 1 d . . . H64A H 0.9209 0.4827 0.0161 0.096 Uiso 1 1 calc R . . H64B H 0.9371 0.6001 0.0453 0.096 Uiso 1 1 calc R . . H64C H 0.8441 0.5672 -0.0276 0.096 Uiso 1 1 calc R . . C71 C 0.55212(14) 0.38565(16) -0.21612(11) 0.0515(4) Uani 1 1 d . . . H71A H 0.5484 0.3499 -0.2688 0.077 Uiso 1 1 calc R . . H71B H 0.6025 0.4362 -0.2033 0.077 Uiso 1 1 calc R . . H71C H 0.4931 0.4206 -0.2226 0.077 Uiso 1 1 calc R . . C72 C 0.46223(12) 0.22077(17) -0.14470(13) 0.0522(5) Uani 1 1 d . . . H72A H 0.4183 0.2665 -0.1302 0.078 Uiso 1 1 calc R . . H72B H 0.4725 0.1594 -0.1089 0.078 Uiso 1 1 calc R . . H72C H 0.4367 0.2006 -0.2042 0.078 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 0.02641(8) 0.02800(9) 0.02797(9) 0.00118(5) 0.00909(6) 0.00018(5) Si 0.0306(2) 0.0403(2) 0.0321(2) 0.00405(18) 0.00531(16) 0.00467(18) O1 0.0382(8) 0.0959(12) 0.1051(14) 0.0080(11) 0.0187(8) -0.0102(8) O2 0.0672(9) 0.0623(9) 0.0392(7) 0.0072(6) 0.0132(6) -0.0016(7) C1 0.0387(9) 0.0447(10) 0.0487(10) 0.0034(8) 0.0114(8) 0.0005(7) C2 0.0328(7) 0.0339(8) 0.0368(8) -0.0034(7) 0.0081(6) -0.0015(6) C11 0.0351(8) 0.0345(8) 0.0268(7) -0.0014(6) 0.0072(6) 0.0008(6) C12 0.0382(8) 0.0357(8) 0.0302(7) 0.0003(6) 0.0134(6) 0.0030(6) C13 0.0364(8) 0.0356(8) 0.0348(8) -0.0011(6) 0.0137(6) 0.0063(6) C14 0.0388(8) 0.0284(7) 0.0310(7) -0.0020(6) 0.0090(6) 0.0010(6) C15 0.0330(7) 0.0326(8) 0.0321(7) -0.0030(6) 0.0084(6) -0.0034(6) C21 0.0318(7) 0.0329(8) 0.0356(8) 0.0045(6) 0.0123(6) 0.0078(6) C22 0.0338(7) 0.0346(8) 0.0350(8) 0.0010(6) 0.0152(6) 0.0048(6) C23 0.0426(8) 0.0327(8) 0.0325(8) -0.0024(6) 0.0153(7) 0.0015(6) C24 0.0413(8) 0.0285(7) 0.0382(8) -0.0012(6) 0.0149(7) 0.0003(6) C25 0.0391(8) 0.0300(8) 0.0360(8) 0.0043(6) 0.0152(6) 0.0046(6) C31 0.0527(10) 0.0477(10) 0.0384(9) 0.0075(7) 0.0251(8) 0.0074(8) C32 0.119(2) 0.0744(16) 0.0385(11) 0.0000(10) 0.0351(12) -0.0132(14) C33 0.0728(15) 0.112(2) 0.0854(18) 0.0388(16) 0.0560(14) 0.0281(15) C34 0.0896(16) 0.0514(12) 0.0662(13) 0.0120(10) 0.0501(12) 0.0007(11) C41 0.0533(10) 0.0306(8) 0.0375(9) 0.0020(6) 0.0126(7) 0.0029(7) C42 0.0530(11) 0.0507(11) 0.0554(11) 0.0166(9) 0.0134(9) 0.0153(9) C43 0.1140(19) 0.0326(10) 0.0542(12) -0.0041(9) 0.0257(12) 0.0055(11) C44 0.0605(11) 0.0386(10) 0.0544(11) 0.0093(8) 0.0163(9) -0.0074(8) C51 0.0370(8) 0.0526(11) 0.0429(9) 0.0035(8) 0.0204(7) 0.0037(7) C52 0.0482(10) 0.0650(13) 0.0697(13) 0.0036(10) 0.0318(10) -0.0129(9) C53 0.0611(12) 0.0880(16) 0.0483(11) 0.0020(10) 0.0333(10) -0.0043(11) C54 0.0474(11) 0.0897(17) 0.0752(14) 0.0176(12) 0.0334(10) 0.0225(11) C61 0.0528(10) 0.0354(9) 0.0452(9) -0.0025(7) 0.0155(8) -0.0099(7) C62 0.0688(14) 0.0573(13) 0.0658(13) -0.0012(10) -0.0007(11) -0.0238(11) C63 0.0865(16) 0.0346(10) 0.0693(13) -0.0102(9) 0.0295(12) -0.0077(10) C64 0.0687(13) 0.0587(13) 0.0739(14) -0.0087(11) 0.0358(11) -0.0274(11) C71 0.0517(10) 0.0553(11) 0.0405(9) 0.0122(8) 0.0048(8) 0.0107(9) C72 0.0336(9) 0.0627(12) 0.0525(11) 0.0014(9) 0.0026(8) -0.0028(8) _journal_paper_doi 10.1021/om049273j