#------------------------------------------------------------------------------ #$Date: 2013-12-28 15:58:47 +0200 (Sat, 28 Dec 2013) $ #$Revision: 91933 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/01/25/2012541.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_2012541 loop_ _publ_author_name 'Ma, Guibin' 'Fischer, Andreas' 'Glaser, Julius' _publ_section_title ; The trigonal--bipyramidal triiodothallium(III) complex [TlI~3~{(CH~3~)~2~SO}~2~] ; _journal_issue 3 _journal_name_full 'Acta Crystallographica Section C' _journal_page_first m177 _journal_page_last m178 _journal_volume 58 _journal_year 2002 _chemical_formula_iupac '[TlI~3~{(CH~3~)~2~SO}~2~]' _chemical_formula_moiety 'C4 H12 I3 O2 S2 Tl ' _chemical_formula_sum 'C4 H12 I3 O2 S2 Tl' _chemical_formula_weight 741.341 _chemical_name_systematic ; ? ; _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_primary direct _atom_sites_solution_secondary difmap _cell_angle_alpha 90.00 _cell_angle_beta 102.065(2) _cell_angle_gamma 90.00 _cell_formula_units_Z 4 _cell_length_a 8.8785(3) _cell_length_b 14.9833(6) _cell_length_c 12.5835(5) _cell_measurement_reflns_used 10534 _cell_measurement_temperature 298 _cell_measurement_theta_max 27.485 _cell_measurement_theta_min 2.910 _cell_volume 1637.00(11) _computing_cell_refinement 'maXus (Mackay et al., 1999)' _computing_data_collection 'maXus (Mackay et al., 1999)' _computing_data_reduction 'Denzo and Scalepak (Otwinowski & Minor, 1997)' _computing_molecular_graphics 'DIAMOND (Bergerhoff, 1996) and maXus?' _computing_publication_material 'maXus (Mackay et al., 1999)??' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_measured_fraction_theta_full .985 _diffrn_measured_fraction_theta_max .985 _diffrn_measurement_device 'Nonius KappaCCD' _diffrn_measurement_method '\f scans' _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type ' MoK\a' _diffrn_reflns_av_R_equivalents .0653 _diffrn_reflns_av_sigmaI/netI .0430 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_number 7155 _diffrn_reflns_theta_full 27.43 _diffrn_reflns_theta_max 27.43 _exptl_absorpt_coefficient_mu 15.756 _exptl_absorpt_correction_T_max .2647 _exptl_absorpt_correction_T_min .0388 _exptl_absorpt_correction_type integration _exptl_absorpt_process_details 'HABITUS (Herrendorf & Baernighausen, 1993)' _exptl_crystal_colour 'Yellow red' _exptl_crystal_density_diffrn 3.008 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Cube _exptl_crystal_size_max .30 _exptl_crystal_size_mid .27 _exptl_crystal_size_min .20 _refine_diff_density_max 1.616 _refine_diff_density_min -1.866 _refine_ls_extinction_coef .0017(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method SHELXL _refine_ls_goodness_of_fit_ref 1.085 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 59 _refine_ls_number_reflns 1842 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.085 _refine_ls_R_factor_all .0444 _refine_ls_R_factor_gt .0411 _refine_ls_shift/su_max .000 _refine_ls_shift/su_mean .000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0422P)^2^+14.8122P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt .1015 _refine_ls_wR_factor_ref .1046 _reflns_number_gt 1715 _reflns_number_total 1842 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file bj1035.cif _[local]_cod_data_source_block I _[local]_cod_cif_authors_sg_H-M 'C 2/c' _[local]_cod_chemical_formula_sum_orig 'C4 H12 I3 O2 S2 Tl ' _cod_original_cell_volume 1637.00(10) _cod_database_code 2012541 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_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 Tl1 .5000 .28189(3) .2500 .0517(2) Uani d S 1 . . Tl I1 .24771(9) .37076(7) .14114(8) .1000(3) Uani d . 1 . . I I2 .5000 .10224(6) .2500 .1013(5) Uani d S 1 . . I S1 .3785(3) .38279(16) .46274(19) .0653(5) Uani d . 1 . . S O1 .3878(9) .2908(4) .4134(5) .0684(17) Uani d . 1 . . O C1 .4407(18) .3661(11) .6046(10) .103(5) Uani d . 1 . . C C2 .1803(14) .3981(8) .4629(9) .078(3) Uani d . 1 . . C H1A .548(9) .3566(14) .6212(18) .123 Uiso calc R 1 . . H H1B .390(4) .316(4) .626(2) .123 Uiso calc R 1 . . H H1C .417(3) .417(4) .642(3) .123 Uiso calc R 1 . . H H2A .123(4) .4085(10) .388(5) .094 Uiso calc R 1 . . H H2B .1679(17) .450(4) .509(3) .094 Uiso calc R 1 . . H H2C .140(3) .344(4) .493(2) .094 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 Tl1 .0610(3) .0359(2) .0598(3) .000 .01587(18) .000 I1 .0709(5) .1111(7) .1151(6) .0225(4) .0127(4) .0445(5) I2 .1841(14) .0346(4) .0977(7) .000 .0579(8) .000 S1 .0823(14) .0478(11) .0709(12) -.0016(10) .0279(11) -.0038(9) O1 .097(5) .047(3) .068(4) .000(3) .034(3) .000(3) C1 .125(11) .099(10) .076(7) .017(9) .003(7) -.017(6) C2 .090(7) .061(6) .089(7) .009(5) .030(5) .001(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 Tl1 O1 . 2.469(6) y Tl1 I2 . 2.6916(10) y Tl1 I1 . 2.7173(7) y S1 O1 . 1.521(7) y S1 C1 . 1.772(13) y S1 C2 . 1.775(12) y C1 H1A . .9408 n C2 H2A . .9921 n loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Tl Tl -2.8358 9.6688 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S .1246 .1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O .0106 .0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' loop_ _diffrn_radiation_wavelength .71073 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 Tl1 O1 2_655 . 173.8(3) y O1 Tl1 I2 . . 93.09(15) y O1 Tl1 I1 . 2_655 89.26(18) y O1 Tl1 I1 . . 87.71(18) y I2 Tl1 I1 . . 119.34(3) y I1 Tl1 I1 2_655 . 121.31(5) y O1 S1 C1 . . 104.5(6) y O1 S1 C2 . . 104.8(5) y C1 S1 C2 . . 96.7(6) y S1 O1 Tl1 . . 117.0(4) n S1 C1 H1A . . 109.5 n S1 C1 H1B . . 109.5 n H1A C1 H1B . . 109.5 n S1 C1 H1C . . 109.5 n H1A C1 H1C . . 109.5 n H1B C1 H1C . . 109.5 n S1 C2 H2A . . 109.5 n S1 C2 H2B . . 109.5 n H2A C2 H2B . . 109.5 n S1 C2 H2C . . 109.5 n H2A C2 H2C . . 109.5 n H2B C2 H2C . . 109.5 n _journal_paper_doi 10.1107/S0108270101020649