#------------------------------------------------------------------------------ #$Date: 2014-07-23 10:49:31 +0100 (Wed, 23 Jul 2014) $ #$Revision: 120677 $ #$URL: svn://www.crystallography.net/cod/cif/4/06/01/4060165.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_4060165 _journal_name_full Organometallics _journal_year 2005 _chemical_formula_moiety 'C55 H62 Al2 O6 Si2' _chemical_formula_sum 'C55 H62 Al2 O6 Si2' _chemical_formula_weight 929.19 _chemical_name_common '(6) [Al(CH3)(TPS)(OTHF)]2' _space_group_IT_number 15 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-C 2yc' _symmetry_space_group_name_H-M 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 98.444(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 11.542(3) _cell_length_b 19.145(5) _cell_length_c 23.515(6) _cell_measurement_reflns_used ? _cell_measurement_temperature 203(2) _cell_measurement_theta_max ? _cell_measurement_theta_min ? _cell_volume 5140(2) _diffrn_ambient_temperature 203(2) _diffrn_detector_area_resol_mean ? _diffrn_measurement_device_type ? _diffrn_measurement_method ? _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 0.0483 _diffrn_reflns_av_sigmaI/netI 0.0528 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_number 19792 _diffrn_reflns_theta_max 26.36 _diffrn_reflns_theta_min 1.75 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 0.151 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_crystal_colour ? _exptl_crystal_density_diffrn 1.201 _exptl_crystal_density_meas ? _exptl_crystal_density_method 'not measured' _exptl_crystal_description ? _exptl_crystal_F_000 1976 _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 262 _refine_ls_number_reflns 5227 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.040 _refine_ls_R_factor_all 0.1339 _refine_ls_R_factor_gt 0.0977 _refine_ls_shift/su_max 0.052 _refine_ls_shift/su_mean 0.008 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1654P)^2^+10.0338P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2695 _refine_ls_wR_factor_ref 0.2968 _reflns_number_gt 3387 _reflns_number_total 5227 _reflns_threshold_expression >2sigma(I) _[local]_cod_cif_authors_sg_H-M C2/c _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 4060165 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -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 Al1 Al 0.43988(11) 1.06508(7) 0.47871(5) 0.0410(4) Uani 1 1 d . . . Si1 Si 0.20516(10) 1.04610(6) 0.38105(5) 0.0424(4) Uani 1 1 d . . . O1 O 0.3161(3) 1.05068(19) 0.42899(15) 0.0637(10) Uani 1 1 d . . . O2 O 0.3473(4) 1.1145(2) 0.53543(17) 0.0894(15) Uani 1 1 d . . . O3 O 0.5371(3) 0.99330(17) 0.45824(12) 0.0464(8) Uani 1 1 d . . . C1 C 0.1569(4) 0.9529(2) 0.37028(19) 0.0453(10) Uani 1 1 d . . . C2 C 0.0525(4) 0.9332(2) 0.3358(2) 0.0541(12) Uani 1 1 d . . . C3 C 0.0168(5) 0.8637(3) 0.3282(3) 0.0682(15) Uani 1 1 d . . . C4 C 0.0841(6) 0.8115(3) 0.3581(3) 0.0739(16) Uani 1 1 d . . . C5 C 0.1876(7) 0.8296(3) 0.3925(3) 0.087(2) Uani 1 1 d . . . C6 C 0.2271(5) 0.8995(3) 0.3995(3) 0.0685(15) Uani 1 1 d . . . C7 C 0.2385(4) 1.0847(2) 0.3120(2) 0.0474(11) Uani 1 1 d . . . C8 C 0.1798(5) 1.0659(3) 0.2584(2) 0.0662(15) Uani 1 1 d . . . C9 C 0.2048(5) 1.0950(3) 0.2072(2) 0.0687(15) Uani 1 1 d . . . C10 C 0.2870(6) 1.1460(4) 0.2091(3) 0.095(2) Uani 1 1 d . . . C11 C 0.3396(7) 1.1727(5) 0.2623(3) 0.121(3) Uani 1 1 d . . . C12 C 0.3183(6) 1.1398(4) 0.3138(3) 0.096(2) Uani 1 1 d . . . C13 C 0.0786(4) 1.0956(2) 0.40313(18) 0.0430(10) Uani 1 1 d . . . C14 C 0.0554(5) 1.1653(2) 0.3874(2) 0.0567(12) Uani 1 1 d . . . C15 C -0.0306(5) 1.2026(3) 0.4101(3) 0.0700(15) Uani 1 1 d . . . C16 C -0.0968(5) 1.1716(3) 0.4482(2) 0.0691(16) Uani 1 1 d . . . C17 C -0.0802(6) 1.1030(3) 0.4626(3) 0.0787(18) Uani 1 1 d . . . C18 C 0.0092(5) 1.0646(3) 0.4399(2) 0.0635(14) Uani 1 1 d . . . C19 C 0.2687(7) 1.1706(4) 0.5333(3) 0.092(2) Uani 1 1 d . . . C20 C 0.2107(11) 1.1604(8) 0.5841(5) 0.201(7) Uani 1 1 d . . . C21 C 0.2589(8) 1.1069(6) 0.6197(3) 0.135(4) Uani 1 1 d . . . C22 C 0.3515(15) 1.0790(7) 0.5893(5) 0.265(10) Uani 1 1 d . . . C23 C 0.5945(5) 0.9836(3) 0.4098(2) 0.0699(16) Uani 1 1 d . . . C24 C 0.5342(5) 1.1490(3) 0.4666(3) 0.0716(16) 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 Al1 0.0427(7) 0.0481(8) 0.0307(7) 0.0065(5) -0.0001(5) 0.0044(5) Si1 0.0406(7) 0.0483(7) 0.0364(6) 0.0083(5) -0.0013(5) 0.0056(5) O1 0.049(2) 0.079(3) 0.057(2) 0.0164(18) -0.0125(17) 0.0033(17) O2 0.120(4) 0.090(3) 0.067(3) 0.029(2) 0.045(2) 0.057(3) O3 0.0506(18) 0.0614(19) 0.0279(14) 0.0071(13) 0.0080(13) 0.0120(14) C1 0.048(3) 0.051(3) 0.039(2) 0.0098(19) 0.0145(19) 0.0124(19) C2 0.047(3) 0.051(3) 0.063(3) 0.010(2) 0.004(2) -0.004(2) C3 0.075(4) 0.065(3) 0.071(4) 0.000(3) 0.031(3) -0.007(3) C4 0.090(4) 0.055(3) 0.081(4) -0.002(3) 0.028(4) 0.016(3) C5 0.114(5) 0.048(3) 0.101(5) 0.007(3) 0.024(4) 0.036(3) C6 0.083(4) 0.054(3) 0.069(3) 0.011(3) 0.014(3) 0.029(3) C7 0.034(2) 0.058(3) 0.049(3) 0.012(2) 0.0032(19) -0.0009(19) C8 0.064(3) 0.090(4) 0.042(3) 0.015(3) -0.002(2) -0.021(3) C9 0.067(4) 0.088(4) 0.049(3) 0.013(3) 0.002(3) -0.012(3) C10 0.082(4) 0.143(6) 0.060(4) 0.031(4) 0.011(3) -0.033(4) C11 0.110(6) 0.170(8) 0.078(5) 0.032(5) 0.001(4) -0.075(6) C12 0.086(4) 0.127(6) 0.069(4) 0.021(4) -0.008(3) -0.049(4) C13 0.043(2) 0.045(2) 0.039(2) 0.0011(18) 0.0011(18) 0.0050(18) C14 0.065(3) 0.046(3) 0.058(3) 0.007(2) 0.003(2) 0.010(2) C15 0.087(4) 0.048(3) 0.076(4) 0.004(3) 0.013(3) 0.018(3) C16 0.089(4) 0.063(3) 0.060(3) 0.000(3) 0.024(3) 0.026(3) C17 0.111(5) 0.068(4) 0.067(4) 0.014(3) 0.046(4) 0.032(3) C18 0.085(4) 0.057(3) 0.053(3) 0.013(2) 0.026(3) 0.019(3) C19 0.121(5) 0.079(4) 0.074(4) -0.009(3) 0.010(4) 0.049(4) C20 0.202(12) 0.272(16) 0.156(10) 0.077(10) 0.121(10) 0.131(12) C21 0.132(7) 0.212(10) 0.066(4) 0.008(5) 0.036(4) 0.110(7) C22 0.43(2) 0.252(13) 0.171(10) 0.156(10) 0.236(13) 0.272(15) C23 0.090(4) 0.085(4) 0.039(3) 0.011(3) 0.026(3) 0.029(3) C24 0.077(4) 0.055(3) 0.078(4) 0.014(3) -0.002(3) -0.013(3) _journal_paper_doi 10.1021/om0493199