#------------------------------------------------------------------------------ #$Date: 2016-02-20 03:06:23 +0000 (Sat, 20 Feb 2016) $ #$Revision: 176774 $ #$URL: svn://www.crystallography.net/cod/cif/2/20/21/2202132.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2202132 loop_ _publ_author_name 'Scholz, Stefan' 'Lerner, Hans-Wolfram' 'Bolte, Michael' _publ_section_title ; Tribromo(tetrahydrofuran)aluminium(III) ; _journal_issue 5 _journal_name_full 'Acta Crystallographica Section E' _journal_page_first m289 _journal_page_last m290 _journal_paper_doi 10.1107/S1600536803008614 _journal_volume 59 _journal_year 2003 _chemical_formula_iupac '[Al Br3 (C4 H8 O)]' _chemical_formula_moiety 'C4 H8 Al Br3 O' _chemical_formula_sum 'C4 H8 Al Br3 O' _chemical_formula_weight 338.81 _chemical_name_systematic ? _space_group_IT_number 11 _symmetry_cell_setting monoclinic _symmetry_space_group_name_Hall '-P 2yb' _symmetry_space_group_name_H-M 'P 1 21/m 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 90.00 _cell_angle_beta 106.971(13) _cell_angle_gamma 90.00 _cell_formula_units_Z 2 _cell_length_a 6.3475(11) _cell_length_b 10.779(2) _cell_length_c 7.4326(12) _cell_measurement_reflns_used 4175 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 25.22 _cell_measurement_theta_min 2.14 _cell_volume 486.39(15) _computing_cell_refinement X-AREA _computing_data_collection 'X-AREA (Stoe & Cie, 2001)' _computing_data_reduction X-AREA _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997) ' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997) ' _diffrn_ambient_temperature 100(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Stoe IPDS-II two-circle' _diffrn_measurement_method \w _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 0.0815 _diffrn_reflns_av_sigmaI/netI 0.0568 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 4060 _diffrn_reflns_theta_full 25.07 _diffrn_reflns_theta_max 25.07 _diffrn_reflns_theta_min 2.87 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 12.464 _exptl_absorpt_correction_T_max 0.546 _exptl_absorpt_correction_T_min 0.302 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(MULABS; Spek, 1990; Blessing, 1995)' _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 2.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_description plate _exptl_crystal_F_000 316 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.05 _refine_diff_density_max 1.067 _refine_diff_density_min -1.815 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 55 _refine_ls_number_reflns 918 _refine_ls_number_restraints 2 _refine_ls_restrained_S_all 1.109 _refine_ls_R_factor_all 0.0804 _refine_ls_R_factor_gt 0.0575 _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^)+(0.0137P)^2^+5.1770P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1024 _refine_ls_wR_factor_ref 0.1100 _reflns_number_gt 714 _reflns_number_total 918 _reflns_threshold_expression I>2\s(I) _cod_data_source_file ob6237.cif _cod_data_source_block 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 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_values 1715 2011-07-08 13:25:40Z adriana ; _cod_original_sg_symbol_H-M 'P 21/m' _cod_database_code 2202132 _cod_database_fobs_code 2202132 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group _atom_site_type_symbol Al1 0.5779(6) 0.2500 0.3861(5) 0.0241(8) Uani d S 1 . . Al Br1 0.2463(2) 0.2500 0.4424(2) 0.0523(5) Uani d S 1 . . Br Br2 0.63120(18) 0.07473(13) 0.23733(18) 0.0650(5) Uani d . 1 . . Br O1 0.7882(12) 0.2500 0.6136(11) 0.0265(19) Uani d S 1 . . O C1 0.8720(17) 0.1368(9) 0.7279(14) 0.041(2) Uani d D 1 . . C H1A 0.7532 0.0949 0.7664 0.049 Uiso calc R 1 A 1 H H1B 0.9371 0.0774 0.6575 0.049 Uiso calc R 1 A 1 H C2 1.043(6) 0.188(5) 0.894(4) 0.068(17) Uani d PD 0.50 . 1 C H2A 1.1881 0.1897 0.8691 0.082 Uiso d PR 0.50 . 1 H H2B 1.0539 0.1372 1.0069 0.082 Uiso d PR 0.50 . 1 H C2' 0.980(7) 0.179(4) 0.923(4) 0.058(13) Uani d PD 0.50 . 2 C H2'A 1.1091 0.1275 0.9870 0.070 Uiso d PR 0.50 . 2 H H2'B 0.8732 0.1783 0.9972 0.070 Uiso d PR 0.50 . 2 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Al1 0.0196(16) 0.0272(19) 0.0226(18) 0.000 0.0018(14) 0.000 Br1 0.0198(6) 0.1072(15) 0.0310(8) 0.000 0.0088(5) 0.000 Br2 0.0412(6) 0.0687(8) 0.0655(8) 0.0231(6) -0.0152(5) -0.0438(7) O1 0.020(4) 0.027(5) 0.028(5) 0.000 0.000(3) 0.000 C1 0.045(6) 0.039(6) 0.037(6) 0.010(5) 0.010(5) 0.011(5) C2 0.07(2) 0.11(3) 0.004(10) 0.05(2) -0.014(15) -0.003(13) C2' 0.08(2) 0.044(18) 0.05(2) 0.029(16) 0.021(16) -0.004(15) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Al Al 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Al1 Br1 . . 107.3(3) y O1 Al1 Br2 . 4_565 106.24(17) ? Br1 Al1 Br2 . 4_565 111.72(10) ? O1 Al1 Br2 . . 106.24(17) y Br1 Al1 Br2 . . 111.72(10) y Br2 Al1 Br2 4_565 . 113.13(18) y C1 O1 C1 . 4_565 109.6(9) ? C1 O1 Al1 . . 124.8(5) ? C1 O1 Al1 4_565 . 124.8(5) ? C2' C1 O1 . . 106.8(19) ? C2 C1 O1 . . 103(2) ? C2' C1 H1A . . 91.8 ? C2 C1 H1A . . 111.2 ? O1 C1 H1A . . 111.2 ? C2' C1 H1B . . 124.8 ? C2 C1 H1B . . 111.2 ? O1 C1 H1B . . 111.2 ? H1A C1 H1B . . 109.2 ? C1 C2 C2' . 4_565 108(3) ? C1 C2 H2A . . 110.1 ? C2' C2 H2A 4_565 . 108.1 ? C1 C2 H2B . . 110.3 ? C2' C2 H2B 4_565 . 110.9 ? H2A C2 H2B . . 109.2 ? C1 C2 H2'A . . 113.7 ? C2' C2 H2'A 4_565 . 128.2 ? C1 C2' C2 . 4_565 102(3) ? C1 C2' H2'A . . 111.9 ? C2 C2' H2'A 4_565 . 112.7 ? C1 C2' H2'B . . 110.0 ? C2 C2' H2'B 4_565 . 110.1 ? H2'A C2' H2'B . . 109.5 ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Al1 O1 . 1.823(8) y Al1 Br1 . 2.262(4) y Al1 Br2 4_565 2.264(2) ? Al1 Br2 . 2.264(2) y O1 C1 . 1.494(10) ? O1 C1 4_565 1.494(10) ? C1 C2' . 1.49(2) ? C1 C2 . 1.49(2) ? C1 H1A . 0.9900 ? C1 H1B . 0.9900 ? C2 C2' 4_565 1.51(4) ? C2 H2A . 0.9900 ? C2 H2B . 0.9900 ? C2' C2 4_565 1.51(4) ? C2' H2'A . 0.9900 ? C2' H2'B . 0.9900 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion Br1 Al1 O1 C1 . . . 84.2(8) Br2 Al1 O1 C1 4_565 . . -156.1(7) Br2 Al1 O1 C1 . . . -35.4(9) Br1 Al1 O1 C1 . . 4_565 -84.2(8) Br2 Al1 O1 C1 4_565 . 4_565 35.4(9) Br2 Al1 O1 C1 . . 4_565 156.1(7) C1 O1 C1 C2' 4_565 . . 9(2) Al1 O1 C1 C2' . . . -161(2) C1 O1 C1 C2 4_565 . . -12(2) Al1 O1 C1 C2 . . . 178(2) C2' C1 C2 C2' . . 4_565 -77(10) O1 C1 C2 C2' . . 4_565 28(4) C2 C1 C2' C2 . . 4_565 56(10) O1 C1 C2' C2 . . 4_565 -25(4) C1 C2 C2' C1 . 4_565 4_565 -33(5) C1 C2' C2 C1 . 4_565 4_565 33(5)