#------------------------------------------------------------------------------ #$Date: 2010-01-30 13:59:17 +0000 (Sat, 30 Jan 2010) $ #$Revision: 966 $ #$URL: svn://www.crystallography.net/cod/cif/4/4060163.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_4060163 _journal_name_full 'Organometallics' _journal_year 2005 _chemical_name_common '(5a) [Al2(CH3)3(OTHF)2(DBP)]' _chemical_formula_moiety 'C27 H48 Al2 O5' _chemical_formula_sum 'C27 H48 Al2 O5' _chemical_formula_weight 506.61 _symmetry_cell_setting Monoclinic _space_group_IT_number 14 _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _[local]_cod_cif_authors_sg_H-M 'P 21/n' 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' _cell_length_a 12.793(2) _cell_length_b 14.875(3) _cell_length_c 16.615(3) _cell_angle_alpha 90.00 _cell_angle_beta 110.777(3) _cell_angle_gamma 90.00 _cell_volume 2956.2(9) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 0.2 _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas 0 _exptl_crystal_density_diffrn 1.138 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1104 _exptl_absorpt_coefficient_mu 0.130 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _diffrn_ambient_temperature 203(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 20360 _diffrn_reflns_av_R_equivalents 0.0706 _diffrn_reflns_av_sigmaI/netI 0.0666 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 24.74 _reflns_number_total 5040 _reflns_number_gt 3575 _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^)+(0.0564P)^2^+4.5630P] 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 none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5040 _refine_ls_number_parameters 316 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1079 _refine_ls_R_factor_gt 0.0746 _refine_ls_wR_factor_ref 0.1722 _refine_ls_wR_factor_gt 0.1560 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _refine_ls_shift/su_max 0.001 _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 Al1 Al 0.69870(9) 0.65452(7) 0.10205(7) 0.0277(3) Uani 1 1 d . . . Al2 Al 0.49911(9) 0.73765(8) 0.12066(8) 0.0380(3) Uani 1 1 d . . . O1 O 0.82381(19) 0.71204(16) 0.12606(15) 0.0306(6) Uani 1 1 d . . . O2 O 0.5161(2) 0.7711(2) 0.25210(18) 0.0534(8) Uani 1 1 d . . . O3 O 0.6482(2) 0.71313(17) 0.18269(15) 0.0336(6) Uani 1 1 d . . . O4 O 0.6912(2) 0.62559(18) -0.02116(15) 0.0370(6) Uani 1 1 d . . . O5 O 0.5598(2) 0.69716(17) 0.03714(16) 0.0363(6) Uani 1 1 d . . . C1 C 0.9197(3) 0.7474(2) 0.1239(2) 0.0283(8) Uani 1 1 d . . . C2 C 0.9207(3) 0.8380(3) 0.0961(2) 0.0318(9) Uani 1 1 d . . . C3 C 1.0205(3) 0.8706(3) 0.0913(3) 0.0412(10) Uani 1 1 d . . . H3 H 1.0227 0.9300 0.0729 0.049 Uiso 1 1 calc R . . C4 C 1.1152(4) 0.8196(3) 0.1124(3) 0.0479(11) Uani 1 1 d . . . H4 H 1.1803 0.8430 0.1063 0.058 Uiso 1 1 calc R . . C5 C 1.1142(3) 0.7341(3) 0.1425(3) 0.0430(10) Uani 1 1 d . . . H5 H 1.1799 0.6996 0.1576 0.052 Uiso 1 1 calc R . . C6 C 1.0193(3) 0.6961(2) 0.1516(2) 0.0301(9) Uani 1 1 d . . . C7 C 0.8185(3) 0.9013(2) 0.0739(3) 0.0364(9) Uani 1 1 d . . . C8 C 0.8459(4) 0.9970(3) 0.0542(3) 0.0624(14) Uani 1 1 d . . . H8A H 0.7809 1.0351 0.0439 0.094 Uiso 1 1 calc R . . H8B H 0.8666 0.9965 0.0033 0.094 Uiso 1 1 calc R . . H8C H 0.9077 1.0201 0.1027 0.094 Uiso 1 1 calc R . . C9 C 0.7792(4) 0.9081(3) 0.1503(3) 0.0452(11) Uani 1 1 d . . . H9A H 0.8380 0.9344 0.1990 0.068 Uiso 1 1 calc R . . H9B H 0.7617 0.8485 0.1656 0.068 Uiso 1 1 calc R . . H9C H 0.7130 0.9456 0.1350 0.068 Uiso 1 1 calc R . . C10 C 0.7242(4) 0.8670(3) -0.0066(3) 0.0492(11) Uani 1 1 d . . . H10A H 0.7035 0.8065 0.0038 0.074 Uiso 1 1 calc R . . H10B H 0.7498 0.8663 -0.0550 0.074 Uiso 1 1 calc R . . H10C H 0.6599 0.9063 -0.0194 0.074 Uiso 1 1 calc R . . C11 C 1.0266(3) 0.6013(3) 0.1903(3) 0.0369(10) Uani 1 1 d . . . C12 C 1.1478(4) 0.5664(3) 0.2266(3) 0.0587(13) Uani 1 1 d . . . H12A H 1.1492 0.5081 0.2531 0.088 Uiso 1 1 calc R . . H12B H 1.1936 0.6083 0.2694 0.088 Uiso 1 1 calc R . . H12C H 1.1768 0.5609 0.1803 0.088 Uiso 1 1 calc R . . C13 C 0.9855(3) 0.6022(3) 0.2666(3) 0.0425(10) Uani 1 1 d . . . H13A H 0.9908 0.5421 0.2904 0.064 Uiso 1 1 calc R . . H13B H 0.9083 0.6222 0.2471 0.064 Uiso 1 1 calc R . . H13C H 1.0315 0.6430 0.3105 0.064 Uiso 1 1 calc R . . C14 C 0.9600(4) 0.5337(3) 0.1214(3) 0.0486(11) Uani 1 1 d . . . H14A H 0.9914 0.5308 0.0762 0.073 Uiso 1 1 calc R . . H14B H 0.8826 0.5527 0.0972 0.073 Uiso 1 1 calc R . . H14C H 0.9640 0.4748 0.1473 0.073 Uiso 1 1 calc R . . C15 C 0.4484(5) 0.7636(6) 0.3005(4) 0.115(3) Uani 1 1 d . . . H15A H 0.4043 0.7082 0.2849 0.138 Uiso 1 1 calc R . . H15B H 0.3965 0.8145 0.2884 0.138 Uiso 1 1 calc R . . C16 C 0.5144(5) 0.7620(5) 0.3897(4) 0.0852(18) Uani 1 1 d . . . H16A H 0.4998 0.7069 0.4163 0.102 Uiso 1 1 calc R . . H16B H 0.4963 0.8137 0.4189 0.102 Uiso 1 1 calc R . . C17 C 0.6331(4) 0.7655(4) 0.3974(3) 0.0621(14) Uani 1 1 d . . . H17A H 0.6735 0.7120 0.4267 0.074 Uiso 1 1 calc R . . H17B H 0.6700 0.8191 0.4291 0.074 Uiso 1 1 calc R . . C18 C 0.6278(5) 0.7688(6) 0.3067(3) 0.124(3) Uani 1 1 d . . . H18 H 0.6543 0.8303 0.3016 0.149 Uiso 1 1 calc R . . C19 C 0.6939(4) 0.7143(3) 0.2731(2) 0.0450(11) Uani 1 1 d . . . H19A H 0.7703 0.7380 0.2919 0.054 Uiso 1 1 calc R . . H19B H 0.6970 0.6529 0.2952 0.054 Uiso 1 1 calc R . . C20 C 0.7641(4) 0.6263(3) -0.0691(3) 0.0503(12) Uani 1 1 d . . . H20A H 0.7928 0.5658 -0.0724 0.060 Uiso 1 1 calc R . . H20B H 0.8274 0.6669 -0.0428 0.060 Uiso 1 1 calc R . . C21 C 0.6926(4) 0.6591(4) -0.1568(3) 0.0633(14) Uani 1 1 d . . . H21A H 0.7208 0.6372 -0.2009 0.076 Uiso 1 1 calc R . . H21B H 0.6900 0.7249 -0.1587 0.076 Uiso 1 1 calc R . . C22 C 0.5785(4) 0.6200(3) -0.1696(2) 0.0526(12) Uani 1 1 d . . . H22A H 0.5701 0.5603 -0.1961 0.063 Uiso 1 1 calc R . . H22B H 0.5189 0.6592 -0.2060 0.063 Uiso 1 1 calc R . . C23 C 0.5763(3) 0.6144(3) -0.0790(2) 0.0422(10) Uani 1 1 d . . . H23 H 0.5480 0.5548 -0.0697 0.051 Uiso 1 1 calc R . . C24 C 0.5125(3) 0.6876(3) -0.0535(2) 0.0427(10) Uani 1 1 d . . . H24A H 0.5184 0.7442 -0.0817 0.051 Uiso 1 1 calc R . . H24B H 0.4333 0.6714 -0.0709 0.051 Uiso 1 1 calc R . . C25 C 0.6957(3) 0.5289(3) 0.1376(3) 0.0423(10) Uani 1 1 d . . . H25A H 0.7072 0.4894 0.0951 0.063 Uiso 1 1 calc R . . H25B H 0.6239 0.5160 0.1425 0.063 Uiso 1 1 calc R . . H25C H 0.7547 0.5193 0.1929 0.063 Uiso 1 1 calc R . . C26 C 0.4457(4) 0.8583(3) 0.0790(3) 0.0591(13) Uani 1 1 d . . . H26A H 0.5087 0.8991 0.0931 0.089 Uiso 1 1 calc R . . H26B H 0.3943 0.8788 0.1062 0.089 Uiso 1 1 calc R . . H26C H 0.4076 0.8566 0.0171 0.089 Uiso 1 1 calc R . . C27 C 0.3900(4) 0.6412(3) 0.1121(3) 0.0555(12) Uani 1 1 d . . . H27A H 0.3792 0.6059 0.0608 0.083 Uiso 1 1 calc R . . H27B H 0.3193 0.6676 0.1090 0.083 Uiso 1 1 calc R . . H27C H 0.4177 0.6028 0.1624 0.083 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 0.0236(6) 0.0307(6) 0.0273(6) 0.0011(5) 0.0074(5) -0.0034(5) Al2 0.0267(6) 0.0407(7) 0.0472(7) 0.0023(6) 0.0138(6) 0.0014(5) O1 0.0243(14) 0.0299(14) 0.0342(14) 0.0015(11) 0.0062(11) -0.0024(11) O2 0.0421(17) 0.077(2) 0.0462(18) -0.0024(16) 0.0224(15) 0.0053(16) O3 0.0291(14) 0.0419(16) 0.0308(14) -0.0007(12) 0.0120(12) 0.0005(12) O4 0.0340(15) 0.0481(17) 0.0277(14) -0.0027(12) 0.0096(12) -0.0069(13) O5 0.0288(14) 0.0446(16) 0.0324(15) 0.0026(12) 0.0070(12) 0.0007(12) C1 0.027(2) 0.039(2) 0.0178(17) -0.0069(16) 0.0062(15) -0.0068(17) C2 0.036(2) 0.037(2) 0.0231(19) -0.0047(16) 0.0101(16) -0.0074(18) C3 0.043(3) 0.044(3) 0.040(2) -0.0035(19) 0.018(2) -0.012(2) C4 0.037(3) 0.067(3) 0.046(3) -0.004(2) 0.023(2) -0.016(2) C5 0.028(2) 0.061(3) 0.042(2) -0.006(2) 0.0149(19) 0.003(2) C6 0.025(2) 0.038(2) 0.026(2) -0.0096(16) 0.0078(16) -0.0001(17) C7 0.038(2) 0.028(2) 0.039(2) 0.0044(17) 0.0085(19) -0.0018(17) C8 0.062(3) 0.034(3) 0.091(4) 0.012(2) 0.026(3) -0.004(2) C9 0.046(3) 0.038(2) 0.051(3) -0.004(2) 0.018(2) 0.010(2) C10 0.049(3) 0.042(3) 0.045(3) 0.007(2) 0.001(2) -0.002(2) C11 0.034(2) 0.032(2) 0.042(2) -0.0045(18) 0.0086(19) 0.0080(17) C12 0.043(3) 0.061(3) 0.064(3) -0.002(2) 0.009(2) 0.015(2) C13 0.043(2) 0.039(2) 0.040(2) 0.0044(19) 0.007(2) 0.0066(19) C14 0.048(3) 0.040(3) 0.052(3) -0.011(2) 0.011(2) 0.007(2) C15 0.062(4) 0.232(9) 0.068(4) -0.027(5) 0.043(3) -0.023(5) C16 0.084(4) 0.117(5) 0.070(4) 0.028(4) 0.047(4) 0.009(4) C17 0.066(3) 0.084(4) 0.038(3) -0.008(2) 0.021(2) 0.012(3) C18 0.047(3) 0.278(10) 0.042(3) -0.036(5) 0.009(3) 0.040(5) C19 0.046(3) 0.053(3) 0.037(2) -0.002(2) 0.016(2) 0.007(2) C20 0.050(3) 0.069(3) 0.035(2) -0.001(2) 0.020(2) 0.006(2) C21 0.061(3) 0.094(4) 0.035(3) 0.004(3) 0.018(2) -0.008(3) C22 0.066(3) 0.055(3) 0.025(2) -0.003(2) 0.002(2) -0.009(2) C23 0.036(2) 0.048(3) 0.032(2) 0.0016(19) 0.0007(19) -0.010(2) C24 0.032(2) 0.050(3) 0.032(2) 0.0056(19) -0.0059(18) -0.004(2) C25 0.041(2) 0.041(2) 0.043(2) 0.0039(19) 0.012(2) -0.006(2) C26 0.049(3) 0.054(3) 0.072(3) 0.006(3) 0.018(3) 0.016(2) C27 0.046(3) 0.054(3) 0.076(3) -0.005(2) 0.033(3) -0.003(2) _cod_database_code 4060163