Facile Synthesis and Structure of Heavy Alkali Metal Thiocarboxylates: Structural Comparison with the Selenium and Tellurium Isologues
Osamu Niyomura; Shinzi Kato; Takahiro Kanda; Inorganic Chemistry 38 (1999) 507–518; doi:10.1021/ic9808091

data_4321767
_publ_section_title
;
 Facile Synthesis and Structure of Heavy Alkali Metal Thiocarboxylates:
 Structural Comparison with the Selenium and Tellurium Isologues
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              507
_journal_page_last               518
_journal_paper_doi               10.1021/ic9808091
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C12 H16 F3 N O S'
_chemical_formula_weight         279.32
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yab'
_symmetry_space_group_name_H-M   'P 1 21/a 1'
_audit_creation_date             'Wed Jun 24 14:33:18 1998'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 95.53(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.983(2)
_cell_length_b                   9.064(2)
_cell_length_c                   12.882(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.7
_cell_volume                     1392.7(4)
_computing_cell_refinement       'Rigaku/AFC Diffractometer Control'
_computing_data_collection       'Rigaku/AFC Diffractometer Control'
_computing_data_reduction        teXsan
_computing_publication_material  teXsan
_computing_structure_refinement  teXsan
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      296.2
_diffrn_measurement_device_type  'Rigaku AFC7R'
_diffrn_measurement_method       \w-2\q
_diffrn_orient_matrix_UB_11      -0.06156
_diffrn_orient_matrix_UB_12      0.01156
_diffrn_orient_matrix_UB_13      -0.05758
_diffrn_orient_matrix_UB_21      0.05656
_diffrn_orient_matrix_UB_22      0.00019
_diffrn_orient_matrix_UB_23      -0.05223
_diffrn_orient_matrix_UB_31      -0.00639
_diffrn_orient_matrix_UB_32      -0.10972
_diffrn_orient_matrix_UB_33      -0.00616
_diffrn_radiation_detector       'scintillation counter'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'Rigaku rotating anode'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.018
_diffrn_reflns_av_sigmaI/netI    0.098
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            3201
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.49
_diffrn_reflns_theta_min         2.22
_diffrn_standards_decay_%        0.00
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.255
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.332
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             584.00
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.290
_exptl_crystal_size_min          0.170
_refine_diff_density_max         0.54
_refine_diff_density_min         -0.31
_refine_ls_extinction_coef       0.007(3)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.865
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     164
_refine_ls_number_reflns         1746
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0487
_refine_ls_R_factor_gt           0.0487
_refine_ls_shift/su_max          0.0110
_refine_ls_shift/su_mean         0.0010
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00022|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0584
_refine_ls_wR_factor_ref         0.0584
_reflns_number_gt                1746
_reflns_number_total             3201
_reflns_threshold_expression     >3.0sigma(I)
_cod_data_source_file            ic9808091_6.cif
_cod_data_source_block           2-CF3C6H4COS-+NMe4
_cod_original_cell_volume        1392.7(3)
_cod_original_sg_symbol_H-M      'P 21/a '
_cod_original_formula_sum        'C12 H16 F3 N O S '
_cod_database_code               4321767