#------------------------------------------------------------------------------ #$Date: 2016-03-21 04:06:01 +0000 (Mon, 21 Mar 2016) $ #$Revision: 178490 $ #$URL: svn://www.crystallography.net/cod/cif/4/06/01/4060159.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_4060159 _journal_name_full Organometallics _journal_paper_doi 10.1021/om0493199 _journal_year 2005 _chemical_formula_moiety 'C14 H28 Al2 O4' _chemical_formula_sum 'C14 H28 Al2 O4' _chemical_formula_weight 314.32 _chemical_name_common '(1) [Al(CH3)2(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 123.231(4) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 16.242(4) _cell_length_b 9.887(2) _cell_length_c 13.764(3) _cell_measurement_temperature 273(2) _cell_volume 1848.7(7) _diffrn_ambient_temperature 273(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 0.0245 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 4036 _diffrn_reflns_theta_max 23.35 _diffrn_reflns_theta_min 2.55 _diffrn_standards_decay_% ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_number ? _exptl_absorpt_coefficient_mu 0.166 _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 1.129 _exptl_crystal_density_meas 0 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 680 _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.02 _refine_ls_extinction_coef ? _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 93 _refine_ls_number_reflns 1340 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.080 _refine_ls_R_factor_all 0.1168 _refine_ls_R_factor_gt 0.0874 _refine_ls_shift/su_max 0.010 _refine_ls_shift/su_mean 0.002 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1304P)^2^+3.5676P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2472 _refine_ls_wR_factor_ref 0.2760 _reflns_number_gt 866 _reflns_number_total 1340 _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 'C 2/c' _cod_database_code 4060159 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 0.40357(10) 0.73871(16) 0.23669(13) 0.0665(8) Uani 1 1 d . . . O1 O 0.4109(3) 0.7374(5) 0.3993(4) 0.120(2) Uani 1 1 d . . . O2 O 0.4641(2) 0.7360(4) 0.1512(3) 0.0777(13) Uani 1 1 d . . . C1 C 0.3456(5) 0.7433(6) 0.4352(6) 0.098(2) Uani 1 1 d . . . H1A H 0.3057 0.6621 0.4122 0.117 Uiso 1 1 calc R . . H1B H 0.3025 0.8211 0.4013 0.117 Uiso 1 1 calc R . . C2 C 0.4066(8) 0.7548(8) 0.5605(8) 0.155(4) Uani 1 1 d . . . H2A H 0.3927 0.8395 0.5844 0.186 Uiso 1 1 calc R . . H2B H 0.3918 0.6814 0.5954 0.186 Uiso 1 1 calc R . . C3 C 0.5095(6) 0.7499(6) 0.6001(6) 0.095(2) Uani 1 1 d . . . H3A H 0.5444 0.8284 0.6472 0.114 Uiso 1 1 calc R . . H3B H 0.5406 0.6688 0.6455 0.114 Uiso 1 1 calc R . . C5 C 0.3284(4) 0.5731(6) 0.1866(5) 0.094(2) Uani 1 1 d . . . H5A H 0.3716 0.4978 0.2252 0.140 Uiso 1 1 calc R . . H5B H 0.2966 0.5634 0.1041 0.140 Uiso 1 1 calc R . . H5C H 0.2796 0.5759 0.2054 0.140 Uiso 1 1 calc R . . C6 C 0.3380(4) 0.9147(6) 0.1927(5) 0.094(2) Uani 1 1 d . . . H6A H 0.3859 0.9849 0.2331 0.142 Uiso 1 1 calc R . . H6B H 0.2902 0.9182 0.2130 0.142 Uiso 1 1 calc R . . H6C H 0.3058 0.9273 0.1105 0.142 Uiso 1 1 calc R . . C7 C 0.4271(4) 0.7432(6) 0.0329(5) 0.093(2) Uani 1 1 d . . . H7A H 0.3857 0.6646 -0.0046 0.111 Uiso 1 1 calc R . . H7B H 0.3853 0.8225 0.0014 0.111 Uiso 1 1 calc R . . C4 C 0.5085(6) 0.7489(11) 0.4954(7) 0.205(7) 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 0.0378(10) 0.1098(15) 0.0509(11) -0.0002(8) 0.0237(8) 0.0001(7) O1 0.062(3) 0.254(7) 0.058(3) -0.005(3) 0.042(2) -0.006(3) O2 0.041(2) 0.147(4) 0.047(2) 0.0028(19) 0.0250(17) 0.0014(17) C1 0.090(5) 0.137(6) 0.099(5) -0.002(4) 0.073(5) 0.005(3) C2 0.150(9) 0.243(12) 0.115(7) -0.022(6) 0.101(7) 0.000(6) C3 0.115(6) 0.121(5) 0.062(4) -0.004(3) 0.057(4) 0.004(4) C5 0.080(4) 0.116(5) 0.079(4) 0.012(3) 0.040(4) -0.001(3) C6 0.086(4) 0.115(5) 0.082(4) -0.019(3) 0.045(4) -0.006(3) C7 0.057(3) 0.165(7) 0.042(3) 0.002(3) 0.019(3) 0.002(3) C4 0.078(5) 0.49(2) 0.058(4) -0.035(7) 0.047(4) -0.022(7)