#------------------------------------------------------------------------------ #$Date: 2016-02-19 22:18:51 +0000 (Fri, 19 Feb 2016) $ #$Revision: 176760 $ #$URL: svn://www.crystallography.net/cod/cif/2/01/16/2011652.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_2011652 loop_ _publ_author_name 'Hensen, Karl' 'Lemke, Alexander' 'Bolte, Michael' _publ_section_title ; Tetrabromo(2-methylpyridine-N)titanate(IV) ; _journal_issue 12 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first e565 _journal_page_last e566 _journal_paper_doi 10.1107/S0108270100015407 _journal_volume 56 _journal_year 2000 _chemical_formula_sum 'C6 H7 Br4 N Ti' _chemical_formula_weight 460.67 _chemical_name_systematic ; ? ; _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' _audit_creation_method SHELXL-97 _cell_angle_alpha 90 _cell_angle_beta 91.8200(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 6.74160(10) _cell_length_b 9.8984(2) _cell_length_c 17.3338(3) _cell_measurement_reflns_used 6306 _cell_measurement_temperature 173 _cell_measurement_theta_max 25.00 _cell_measurement_theta_min 1.00 _cell_volume 1156.12(4) _computing_cell_refinement SMART _computing_data_collection 'SMART (Siemens, 1995)' _computing_data_reduction 'SAINT (Siemens, 1995)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990)' _diffrn_ambient_temperature 173 _diffrn_measured_fraction_theta_full .874 _diffrn_measured_fraction_theta_max .874 _diffrn_measurement_device 'Siemens CCD three-circle' _diffrn_measurement_method \w _diffrn_radiation_monochromator 'highly oriented graphite crystal' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength .71073 _diffrn_reflns_av_R_equivalents .086 _diffrn_reflns_av_sigmaI/netI .0706 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 15542 _diffrn_reflns_theta_full 26.21 _diffrn_reflns_theta_max 26.21 _diffrn_reflns_theta_min 2.35 _diffrn_standards_decay_% 0 _diffrn_standards_interval_time 1000 _diffrn_standards_number 131 _exptl_absorpt_coefficient_mu 14.515 _exptl_absorpt_correction_T_max .055 _exptl_absorpt_correction_T_min .026 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details ; The data collection nominally covered a sphere of reciprocal space, by a combination of seven sets of exposures; each set had a different \f angle for the crystal and each exposure covered 0.3\% in \w. The crystal-to-detector distance was 6 cm. Coverage of the unique set for all structures is 100% complete to at least 25.0\% in \q. Crystal decay was monitored by repeating the initial frames at the end of data collection and analyzing the duplicate reflections. ; _exptl_crystal_colour red _exptl_crystal_density_diffrn 2.647 _exptl_crystal_density_method 'not measured' _exptl_crystal_description block _exptl_crystal_F_000 848 _exptl_crystal_size_max .25 _exptl_crystal_size_mid .20 _exptl_crystal_size_min .20 _refine_diff_density_max .976 _refine_diff_density_min -.924 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_all 1.088 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 110 _refine_ls_number_reflns 2159 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.088 _refine_ls_R_factor_all .093 _refine_ls_R_factor_obs .055 _refine_ls_shift/su_max <0.001 _refine_ls_shift/su_mean <0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0402P)^2^+4.5123P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_all .106 _refine_ls_wR_factor_obs .095 _refine_ls_wR_factor_ref .106 _reflns_number_gt 1587 _reflns_number_total 2159 _reflns_threshold_expression I>2\s(I) _cod_data_source_file qa0449.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 The following automatic conversions were performed: '_refine_ls_weighting_scheme' value 'calc w = 1/[\s^2^(Fo^2^)+(0.0402P)^2^+4.5123P] where P = (Fo^2^+2Fc^2^)/3' was changed to 'calc'. New tag '_refine_ls_weighting_details' was created. The value of the new tag was set to 'w = 1/[\s^2^(Fo^2^)+(0.0402P)^2^+4.5123P] where P = (Fo^2^+2Fc^2^)/3'. Automatic conversion script Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas ; _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 2011652 _cod_database_fobs_code 2011652 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_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 Ti1 .7481(2) .26630(15) .42258(8) .0184(4) Uani d . 1 . . Ti Br1 1.05923(14) .17272(9) .45641(5) .0297(3) Uani d . 1 . . Br Br2 .58777(15) .31811(10) .53559(5) .0346(3) Uani d . 1 . . Br Br3 .59407(14) .04955(9) .39896(6) .0290(3) Uani d . 1 . . Br Br4 .88825(14) .48695(9) .39882(5) .0285(3) Uani d . 1 . . Br N1 .5880(10) .3157(7) .3175(4) .0216(17) Uani d . 1 . . N C2 .6561(12) .2868(8) .2483(5) .0183(19) Uani d . 1 . . C C21 .8543(14) .2160(10) .2442(5) .030(2) Uani d . 1 . . C H21A .9498 .2587 .2804 .044 Uiso calc R 1 . . H H21B .9029 .2228 .1917 .044 Uiso calc R 1 . . H H21C .8388 .1206 .2580 .044 Uiso calc R 1 . . H C3 .5478(14) .3269(9) .1821(5) .029(2) Uani d . 1 . . C H3 .5975 .3080 .1326 .035 Uiso calc R 1 . . H C4 .3717(14) .3927(10) .1881(6) .032(2) Uani d . 1 . . C H4 .2974 .4185 .1430 .039 Uiso calc R 1 . . H C5 .3017(14) .4219(9) .2606(6) .031(2) Uani d . 1 . . C H5 .1801 .4689 .2663 .037 Uiso calc R 1 . . H C6 .4123(14) .3814(9) .3232(5) .027(2) Uani d . 1 . . C H6 .3648 .3998 .3731 .033 Uiso calc R 1 . . 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 Ti1 .0187(9) .0193(8) .0170(8) .0001(7) -.0001(6) -.0001(7) Br1 .0230(5) .0308(5) .0348(6) .0041(4) -.0054(4) .0022(4) Br2 .0443(6) .0356(6) .0244(5) .0046(5) .0118(4) -.0016(4) Br3 .0269(5) .0224(5) .0379(6) -.0058(4) .0017(4) .0011(4) Br4 .0332(5) .0217(5) .0303(5) -.0065(4) -.0054(4) .0026(4) N1 .021(4) .020(4) .024(4) -.003(3) .003(3) -.004(3) C2 .012(4) .024(5) .019(5) -.010(4) .001(3) -.007(4) C21 .037(6) .037(6) .015(5) -.011(5) .002(4) -.007(4) C3 .033(6) .033(6) .021(5) -.007(5) -.004(4) .000(4) C4 .029(6) .034(6) .033(6) -.009(5) -.019(4) .009(5) C5 .023(5) .033(6) .036(6) -.001(4) -.008(4) .009(5) C6 .034(6) .021(5) .027(6) -.006(4) .003(4) .002(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C .0033 .0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H .0000 .0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N .0061 .0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ti Ti .2776 .4457 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -.2901 2.4595 '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 _geom_angle_publ_flag N1 Ti1 Br2 115.5(2) y N1 Ti1 Br1 136.3(2) y Br2 Ti1 Br1 108.17(7) y N1 Ti1 Br3 81.74(19) y Br2 Ti1 Br3 97.47(6) y Br1 Ti1 Br3 93.88(6) y N1 Ti1 Br4 80.69(19) y Br2 Ti1 Br4 97.98(6) y Br1 Ti1 Br4 92.75(6) y Br3 Ti1 Br4 160.36(7) y C2 N1 C6 119.8(7) y C2 N1 Ti1 122.6(6) y C6 N1 Ti1 117.6(6) y N1 C2 C3 119.6(8) ? N1 C2 C21 118.3(7) ? C3 C2 C21 122.1(7) ? C4 C3 C2 120.5(9) ? C3 C4 C5 119.4(8) ? C6 C5 C4 118.0(9) ? N1 C6 C5 122.8(9) ? 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 Ti1 N1 . 2.145(7) y Ti1 Br2 . 2.3245(17) y Ti1 Br1 . 2.3502(17) y Ti1 Br3 . 2.4129(17) y Ti1 Br4 . 2.4202(17) y N1 C2 . 1.328(10) ? N1 C6 . 1.357(11) ? C2 C3 . 1.398(12) ? C2 C21 . 1.513(12) ? C3 C4 . 1.362(13) ? C4 C5 . 1.386(14) ? C5 C6 . 1.358(12) ? 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 _geom_torsion_publ_flag Br2 Ti1 N1 C2 -176.9(6) y Br1 Ti1 N1 C2 4.4(8) y Br3 Ti1 N1 C2 -82.5(6) y Br4 Ti1 N1 C2 88.6(6) y Br2 Ti1 N1 C6 4.4(7) ? Br1 Ti1 N1 C6 -174.3(5) ? Br3 Ti1 N1 C6 98.7(6) ? Br4 Ti1 N1 C6 -90.1(6) ? C6 N1 C2 C3 1.3(12) ? Ti1 N1 C2 C3 -177.4(6) ? C6 N1 C2 C21 178.8(8) ? Ti1 N1 C2 C21 .1(10) ? N1 C2 C3 C4 -1.3(13) ? C21 C2 C3 C4 -178.7(8) ? C2 C3 C4 C5 1.1(14) ? C3 C4 C5 C6 -.8(14) ? C2 N1 C6 C5 -1.1(13) ? Ti1 N1 C6 C5 177.6(7) ? C4 C5 C6 N1 .9(14) ?