#------------------------------------------------------------------------------ #$Date: 2016-03-21 04:06:01 +0000 (Mon, 21 Mar 2016) $ #$Revision: 178490 $ #$URL: svn://www.crystallography.net/cod/cif/4/06/01/4060160.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_4060160 _journal_name_full Organometallics _journal_paper_doi 10.1021/om0493199 _journal_year 2005 _chemical_formula_sum 'C18 H38 Al2 O4' _chemical_formula_weight 372.44 _chemical_name_common '(2) [Al(Et)2(OTHF)]2' _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 96.019(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 15.3187(16) _cell_length_b 7.9024(8) _cell_length_c 18.3558(19) _cell_measurement_reflns_used ? _cell_measurement_temperature 203(2) _cell_measurement_theta_max ? _cell_measurement_theta_min ? _cell_volume 2209.8(4) _diffrn_ambient_temperature 203(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 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 17031 _diffrn_reflns_theta_max 26.39 _diffrn_reflns_theta_min 1.65 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 0.148 _exptl_absorpt_correction_T_max ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 1.119 _exptl_crystal_density_meas 0 _exptl_crystal_density_method 'not measured' _exptl_crystal_description irregular _exptl_crystal_F_000 816 _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 221 _refine_ls_number_reflns 4513 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.027 _refine_ls_R_factor_all 0.0945 _refine_ls_R_factor_gt 0.0763 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0957P)^2^+3.5221P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1912 _refine_ls_wR_factor_ref 0.2064 _reflns_number_gt 3509 _reflns_number_total 4513 _reflns_threshold_expression >2sigma(I) _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_original_sg_symbol_H-M 'P 21/n' _cod_database_code 4060160 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 Al1 Al -0.00448(6) -0.07431(11) 0.07346(5) 0.0309(3) Uani 1 1 d . . . Al2 Al 1.00117(6) 0.52525(12) 0.41969(5) 0.0345(3) Uani 1 1 d . . . O1 O 0.04356(13) 0.1057(3) 0.02798(11) 0.0338(5) Uani 1 1 d . . . O2 O 0.07192(19) 0.0652(3) 0.16479(14) 0.0559(7) Uani 1 1 d . . . O3 O 0.94318(14) 0.5944(3) 0.49773(12) 0.0372(5) Uani 1 1 d . . . O4 O 0.90666(17) 0.7053(4) 0.37095(13) 0.0539(7) Uani 1 1 d . . . C1 C 0.0991(3) 0.2270(5) 0.06507(19) 0.0511(9) Uani 1 1 d . . . H1A H 0.0873 0.3381 0.0425 0.061 Uiso 1 1 calc R . . H1B H 0.1603 0.1977 0.0602 0.061 Uiso 1 1 calc R . . C2 C 0.0863(4) 0.2362(6) 0.1417(2) 0.0803(16) Uani 1 1 d . . . H2 H 0.0319 0.3013 0.1461 0.096 Uiso 1 1 calc R . . C3 C 0.1574(3) 0.3082(5) 0.1953(2) 0.0544(10) Uani 1 1 d . . . H3A H 0.2095 0.3354 0.1709 0.065 Uiso 1 1 calc R . . H3B H 0.1371 0.4114 0.2179 0.065 Uiso 1 1 calc R . . C4 C 0.1770(4) 0.1769(7) 0.2501(3) 0.099(2) Uani 1 1 d . . . H4A H 0.1696 0.2211 0.2989 0.118 Uiso 1 1 calc R . . H4B H 0.2378 0.1389 0.2498 0.118 Uiso 1 1 calc R . . C5 C 0.1170(3) 0.0364(6) 0.2326(2) 0.0715(14) Uani 1 1 d . . . H5A H 0.1500 -0.0698 0.2319 0.086 Uiso 1 1 calc R . . H5B H 0.0758 0.0271 0.2697 0.086 Uiso 1 1 calc R . . C6 C -0.1152(2) -0.0394(5) 0.1175(2) 0.0473(8) Uani 1 1 d . . . H6A H -0.1010 -0.0126 0.1695 0.057 Uiso 1 1 calc R . . H6B H -0.1452 0.0592 0.0942 0.057 Uiso 1 1 calc R . . C7 C -0.1784(3) -0.1873(7) 0.1113(3) 0.0793(16) Uani 1 1 d . . . H7A H -0.1958 -0.2115 0.0601 0.119 Uiso 1 1 calc R . . H7B H -0.2299 -0.1592 0.1355 0.119 Uiso 1 1 calc R . . H7C H -0.1499 -0.2860 0.1345 0.119 Uiso 1 1 calc R . . C8 C 0.0646(2) -0.2825(4) 0.0954(2) 0.0421(8) Uani 1 1 d . . . H8A H 0.0749 -0.2959 0.1487 0.051 Uiso 1 1 calc R . . H8B H 0.0299 -0.3797 0.0760 0.051 Uiso 1 1 calc R . . C9 C 0.1524(3) -0.2853(5) 0.0641(3) 0.0618(11) Uani 1 1 d . . . H9A H 0.1429 -0.2785 0.0111 0.093 Uiso 1 1 calc R . . H9B H 0.1830 -0.3897 0.0783 0.093 Uiso 1 1 calc R . . H9C H 0.1875 -0.1897 0.0830 0.093 Uiso 1 1 calc R . . C10 C 0.8762(3) 0.7172(5) 0.4916(2) 0.0555(10) Uani 1 1 d . . . H10A H 0.8297 0.6830 0.5214 0.067 Uiso 1 1 calc R . . H10B H 0.9001 0.8254 0.5106 0.067 Uiso 1 1 calc R . . C11 C 0.8403(4) 0.7382(10) 0.4186(3) 0.115(3) Uani 1 1 d . . . H11 H 0.7990 0.6422 0.4098 0.138 Uiso 1 1 calc R . . C12 C 0.7890(3) 0.8875(6) 0.3893(2) 0.0592(11) Uani 1 1 d . . . H12A H 0.8046 0.9886 0.4187 0.071 Uiso 1 1 calc R . . H12B H 0.7258 0.8671 0.3885 0.071 Uiso 1 1 calc R . . C13 C 0.8148(3) 0.9065(7) 0.3132(3) 0.0743(14) Uani 1 1 d . . . H13A H 0.7722 0.8499 0.2778 0.089 Uiso 1 1 calc R . . H13B H 0.8176 1.0263 0.3000 0.089 Uiso 1 1 calc R . . C14 C 0.9017(3) 0.8273(7) 0.3138(3) 0.0794(15) Uani 1 1 d . . . H14A H 0.9078 0.7728 0.2667 0.095 Uiso 1 1 calc R . . H14B H 0.9482 0.9120 0.3233 0.095 Uiso 1 1 calc R . . C15 C 0.9542(3) 0.3351(5) 0.3580(2) 0.0511(9) Uani 1 1 d . . . H15A H 0.9994 0.2469 0.3600 0.061 Uiso 1 1 calc R . . H15B H 0.9040 0.2880 0.3802 0.061 Uiso 1 1 calc R . . C16 C 0.9248(3) 0.3710(7) 0.2781(2) 0.0712(13) Uani 1 1 d . . . H16A H 0.8728 0.4419 0.2744 0.107 Uiso 1 1 calc R . . H16B H 0.9114 0.2653 0.2525 0.107 Uiso 1 1 calc R . . H16C H 0.9714 0.4289 0.2561 0.107 Uiso 1 1 calc R . . C17 C 1.1013(2) 0.6539(5) 0.3878(2) 0.0474(9) Uani 1 1 d . . . H17A H 1.1527 0.5795 0.3910 0.057 Uiso 1 1 calc R . . H17B H 1.0873 0.6849 0.3362 0.057 Uiso 1 1 calc R . . C18 C 1.1256(3) 0.8147(6) 0.4315(3) 0.0661(12) Uani 1 1 d . . . H18A H 1.0771 0.8940 0.4253 0.099 Uiso 1 1 calc R . . H18B H 1.1772 0.8655 0.4141 0.099 Uiso 1 1 calc R . . H18C H 1.1381 0.7865 0.4830 0.099 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 Al1 0.0347(5) 0.0242(5) 0.0336(5) 0.0048(3) 0.0028(4) -0.0009(4) Al2 0.0361(5) 0.0352(5) 0.0332(5) -0.0012(4) 0.0086(4) 0.0029(4) O1 0.0399(12) 0.0250(10) 0.0354(11) 0.0019(9) -0.0003(9) -0.0063(9) O2 0.0771(18) 0.0370(14) 0.0482(15) 0.0116(11) -0.0185(13) -0.0181(13) O3 0.0387(12) 0.0379(12) 0.0365(11) 0.0013(9) 0.0107(9) 0.0114(10) O4 0.0583(15) 0.0625(17) 0.0426(13) 0.0108(12) 0.0133(11) 0.0264(13) C1 0.072(2) 0.0376(19) 0.0435(19) -0.0035(15) 0.0039(17) -0.0255(18) C2 0.128(4) 0.051(3) 0.055(3) 0.011(2) -0.028(3) -0.037(3) C3 0.070(3) 0.044(2) 0.046(2) -0.0025(16) -0.0116(18) -0.0163(19) C4 0.099(4) 0.078(4) 0.104(4) 0.032(3) -0.062(3) -0.032(3) C5 0.098(3) 0.058(3) 0.052(2) 0.017(2) -0.025(2) -0.020(2) C6 0.048(2) 0.048(2) 0.048(2) 0.0087(16) 0.0149(16) 0.0020(16) C7 0.062(3) 0.116(4) 0.063(3) -0.022(3) 0.020(2) -0.041(3) C8 0.0474(19) 0.0289(16) 0.0494(19) 0.0087(14) 0.0022(15) 0.0023(14) C9 0.054(2) 0.049(2) 0.083(3) 0.018(2) 0.013(2) 0.0165(19) C10 0.056(2) 0.063(3) 0.049(2) 0.0047(18) 0.0131(17) 0.031(2) C11 0.120(5) 0.158(6) 0.074(3) 0.045(4) 0.046(3) 0.104(5) C12 0.055(2) 0.057(2) 0.065(3) 0.013(2) 0.0047(19) 0.0224(19) C13 0.069(3) 0.078(3) 0.076(3) 0.024(3) 0.004(2) 0.022(2) C14 0.082(3) 0.095(4) 0.063(3) 0.034(3) 0.014(2) 0.031(3) C15 0.058(2) 0.045(2) 0.051(2) -0.0121(17) 0.0087(17) -0.0019(17) C16 0.076(3) 0.080(3) 0.056(3) -0.026(2) -0.005(2) 0.000(2) C17 0.047(2) 0.048(2) 0.049(2) 0.0064(16) 0.0156(16) 0.0031(16) C18 0.056(2) 0.064(3) 0.080(3) -0.004(2) 0.014(2) -0.016(2)