#------------------------------------------------------------------------------ #$Date: 2014-07-23 10:49:31 +0100 (Wed, 23 Jul 2014) $ #$Revision: 120677 $ #$URL: svn://www.crystallography.net/cod/cif/4/00/02/4000292.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_4000292 _journal_name_full 'Chemistry of Materials' _journal_year 2003 _chemical_formula_sum 'Sb7.73 Ti10.84' _[local]_cod_chemical_formula_sum_orig Ti10.84Sb7.73 _chemical_formula_weight 1460 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'Pnma' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 14.6228(9) _cell_length_b 5.5972(4) _cell_length_c 17.6440(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1444.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour black _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.01 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 6.717 _exptl_crystal_density_method ? _exptl_crystal_F_000 2531 _exptl_absorpt_coefficient_mu 19.759 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.33 _exptl_absorpt_correction_T_max 0.37 _diffrn_ambient_temperature 293(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 ? _diffrn_measurement_method ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2037 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1698 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 0 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 28.90 _reflns_number_total 2037 _reflns_number_observed 954 _reflns_observed_criterion >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+0.0000P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.000007(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2037 _refine_ls_number_parameters 110 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0772 _refine_ls_R_factor_obs 0.0267 _refine_ls_wR_factor_all 0.0413 _refine_ls_wR_factor_obs 0.0361 _refine_ls_goodness_of_fit_all 0.497 _refine_ls_goodness_of_fit_obs 0.655 _refine_ls_restrained_S_all 0.497 _refine_ls_restrained_S_obs 0.655 _refine_ls_shift/esd_max 0.000 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Sb1 Sb 0.29577(7) 0.2500 0.30250(5) 0.0071(2) Uani 1 d S . Sb2 Sb 0.43936(8) 0.2500 0.51761(5) 0.0065(2) Uani 1 d S . Sb3 Sb 0.08212(7) 0.2500 0.19467(5) 0.0071(2) Uani 1 d S . Sb4 Sb 0.23033(8) 0.2500 0.90905(5) 0.0113(2) Uani 1 d S . Sb5 Sb 0.01601(8) 0.2500 0.73966(6) 0.0120(2) Uani 1 d S . Sb6 Sb 0.04852(8) 0.2500 0.43805(6) 0.0218(3) Uani 1 d S . Sb7 Sb 0.28753(5) 0.0036(2) 0.10813(4) 0.0116(2) Uani 0.867(5) d P . TB7 Ti 0.28753(5) 0.0036(2) 0.10813(4) 0.0116(2) Uani 0.133(5) d P . Ti1 Ti 0.4332(2) 0.2500 0.19206(14) 0.0097(5) Uani 1 d S . Ti2 Ti 0.1257(2) 0.2500 0.04007(14) 0.0089(6) Uani 1 d S . Ti3 Ti 0.2013(2) 0.2500 0.74941(15) 0.0076(5) Uani 1 d S . Ti4 Ti 0.3663(2) 0.2500 0.66272(14) 0.0080(6) Uani 1 d S . Ti5 Ti 0.2475(2) 0.2500 0.46618(14) 0.0094(6) Uani 1 d S . Ti6 Ti 0.3822(3) 0.2500 0.9922(2) 0.0176(14) Uani 0.753(13) d SP . Ti7 Ti 0.0432(3) 0.2500 0.5911(2) 0.0195(14) Uani 0.819(13) d SP . Ti8 Ti 0.06186(13) 0.0042(3) 0.87923(8) 0.0069(3) Uani 1 d . . Ti9 Ti 0.36578(12) 0.0082(3) 0.82343(9) 0.0078(4) Uani 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 Sb1 0.0060(5) 0.0085(5) 0.0070(5) 0.000 0.0001(4) 0.000 Sb2 0.0076(5) 0.0073(4) 0.0046(4) 0.000 -0.0002(4) 0.000 Sb3 0.0078(6) 0.0091(5) 0.0043(4) 0.000 -0.0004(4) 0.000 Sb4 0.0170(6) 0.0093(5) 0.0076(4) 0.000 0.0054(4) 0.000 Sb5 0.0071(5) 0.0084(5) 0.0203(5) 0.000 -0.0009(4) 0.000 Sb6 0.0101(6) 0.0451(8) 0.0102(4) 0.000 -0.0015(4) 0.000 Sb7 0.0091(4) 0.0172(4) 0.0084(3) 0.0021(3) -0.0007(3) -0.0024(4) TB7 0.0091(4) 0.0172(4) 0.0084(3) 0.0021(3) -0.0007(3) -0.0024(4) Ti1 0.0081(14) 0.0146(13) 0.0065(11) 0.000 -0.0003(11) 0.000 Ti2 0.0098(15) 0.0117(14) 0.0051(12) 0.000 0.0012(11) 0.000 Ti3 0.0103(14) 0.0080(12) 0.0044(11) 0.000 0.0012(11) 0.000 Ti4 0.007(2) 0.0081(12) 0.0089(12) 0.000 -0.0005(11) 0.000 Ti5 0.0088(14) 0.0127(13) 0.0067(13) 0.000 0.0002(10) 0.000 Ti6 0.005(2) 0.033(3) 0.015(2) 0.000 -0.001(2) 0.000 Ti7 0.017(2) 0.037(3) 0.005(2) 0.000 0.0033(14) 0.000 Ti8 0.0075(9) 0.0061(8) 0.0071(7) -0.0010(7) 0.0000(6) 0.0017(9) Ti9 0.0042(10) 0.0099(9) 0.0092(7) -0.0023(8) 0.0011(6) -0.0013(9) _cod_database_code 4000292 _journal_paper_doi 10.1021/cm034328d