#------------------------------------------------------------------------------ #$Date: 2008-01-13 22:15:36 +0000 (Sun, 13 Jan 2008) $ #$Revision: 14 $ #$URL: svn://www.crystallography.net/cod/cif/4/4060235.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_4060235 _journal_name_full 'Organometallics' _journal_year 2004 _chemical_formula_sum 'C5 H7 O2 Tl' _chemical_formula_weight 303.48 _symmetry_cell_setting 'Orthorhombic' _symmetry_space_group_name_H-M 'Iba2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z' '-x, y, z+1/2' 'x, -y, z+1/2' 'x+1/2, y+1/2, z+1/2' '-x+1/2, -y+1/2, z+1/2' '-x+1/2, y+1/2, z+1' 'x+1/2, -y+1/2, z+1' _cell_length_a 11.3256(4) _cell_length_b 20.6199(5) _cell_length_c 5.3836(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1257.25(7) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 889 _cell_measurement_theta_min 2.05 _cell_measurement_theta_max 27.86 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.207 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1072 _exptl_absorpt_coefficient_mu 25.597 _exptl_absorpt_correction_type 'multiscan' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details 'Scalepack' _diffrn_ambient_temperature 223(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_type 'Nonius KappaCCD' _diffrn_measurement_method '\w- & \f- scan' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9736 _diffrn_reflns_av_R_equivalents 0.084 _diffrn_reflns_av_sigmaI/netI 0.0204 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -7 _diffrn_reflns_limit_l_max 7 _diffrn_reflns_theta_min 0.21 _diffrn_reflns_theta_max 27.88 _reflns_number_total 833 _reflns_number_gt 757 _reflns_threshold_expression >2sigma(I) _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0673P)^2^+7.3952P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0026(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.00 _refine_ls_number_reflns 833 _refine_ls_number_parameters 76 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0429 _refine_ls_R_factor_gt 0.0388 _refine_ls_wR_factor_ref 0.1037 _refine_ls_wR_factor_gt 0.1013 _refine_ls_goodness_of_fit_ref 1.179 _refine_ls_restrained_S_all 1.178 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_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_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 Tl Tl 0.12185(3) 0.25951(2) 0.7363(5) 0.0254(3) Uani 1 1 d . . . O1 O 0.1257(8) 0.1815(7) 0.378(3) 0.035(3) Uani 1 1 d . . . O2 O 0.2915(9) 0.1816(4) 0.7989(18) 0.029(3) Uani 1 1 d . . . C1 C 0.3990(11) 0.0845(8) 0.862(3) 0.024(3) Uani 1 1 d . . . H1A H 0.4688 0.1101 0.8869 0.036 Uiso 1 1 calc R . . H1B H 0.4183 0.0467 0.7665 0.036 Uiso 1 1 calc R . . H1C H 0.3680 0.0714 1.0206 0.036 Uiso 1 1 calc R . . C2 C 0.3089(9) 0.1236(6) 0.727(4) 0.023(3) Uani 1 1 d . . . C3 C 0.2499(11) 0.0945(5) 0.517(3) 0.022(3) Uani 1 1 d . . . H3 H 0.2717 0.0522 0.4774 0.026 Uiso 1 1 calc R . . C4 C 0.1629(12) 0.1230(7) 0.365(3) 0.020(3) Uani 1 1 d . . . C5 C 0.1014(12) 0.0797(7) 0.171(3) 0.028(4) Uani 1 1 d . . . H5A H 0.0175 0.0815 0.1951 0.041 Uiso 1 1 calc R . . H5B H 0.1281 0.0358 0.1896 0.041 Uiso 1 1 calc R . . H5C H 0.1203 0.0949 0.0071 0.041 Uiso 1 1 calc R . . 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 Tl 0.0286(3) 0.0157(3) 0.0319(4) -0.0019(12) 0.0000(6) 0.00383(14) O1 0.045(7) 0.015(6) 0.045(8) -0.005(6) -0.011(5) 0.010(4) O2 0.043(5) 0.013(4) 0.029(6) -0.004(4) -0.011(4) 0.004(4) C1 0.028(7) 0.021(8) 0.023(8) -0.001(6) -0.003(6) 0.004(6) C2 0.017(5) 0.021(6) 0.031(7) -0.008(11) 0.017(10) -0.006(4) C3 0.035(7) 0.007(5) 0.024(7) -0.001(5) 0.006(6) -0.004(5) C4 0.018(6) 0.020(7) 0.022(7) -0.004(6) 0.002(6) 0.002(5) C5 0.038(7) 0.012(7) 0.033(12) -0.005(5) 0.000(6) -0.001(5)