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_4321766
_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 H19 N O2 S'
_chemical_formula_weight         241.35
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_Int_Tables_number      19
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_audit_creation_date             'Wed Jun 24 14:43:00 1998'
_audit_creation_method           'from TEXRAY.INF file'
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   11.3264(9)
_cell_length_b                   13.671(1)
_cell_length_c                   8.371(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      14.6
_cell_measurement_theta_min      12.8
_cell_volume                     1296.2(2)
_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      -0.01910
_diffrn_orient_matrix_UB_12      -0.00364
_diffrn_orient_matrix_UB_13      0.11650
_diffrn_orient_matrix_UB_21      -0.08599
_diffrn_orient_matrix_UB_22      0.00601
_diffrn_orient_matrix_UB_23      -0.02526
_diffrn_orient_matrix_UB_31      -0.00614
_diffrn_orient_matrix_UB_32      -0.07281
_diffrn_orient_matrix_UB_33      -0.00791
_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  0.000
_diffrn_reflns_av_sigmaI/netI    0.069
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       10
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            1720
_diffrn_reflns_reduction_process 'Lp corrections applied'
_diffrn_reflns_theta_max         27.4943
_diffrn_standards_decay_%        -0.38
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    0.236
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            slight
_exptl_crystal_density_diffrn    1.237
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prismatic
_exptl_crystal_F_000             520.00
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.290
_refine_diff_density_max         0.15
_refine_diff_density_min         -0.17
_refine_ls_abs_structure_Flack   -0.5(1)
_refine_ls_extinction_coef       0.021(3)
_refine_ls_extinction_method     'Zachariasen(1967) type 2 Gaussian isotropic'
_refine_ls_goodness_of_fit_ref   1.643
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_constraints    0
_refine_ls_number_parameters     147
_refine_ls_number_reflns         1232
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0352
_refine_ls_R_factor_gt           0.0352
_refine_ls_shift/su_max          0.0340
_refine_ls_shift/su_mean         0.0060
_refine_ls_structure_factor_coef F
_refine_ls_weighting_details     'w = 1/[\s^2^(Fo) + 0.00006|Fo|^2^]'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0358
_refine_ls_wR_factor_ref         0.0358
_reflns_number_gt                1232
_reflns_number_total             1720
_reflns_threshold_expression     >3.0sigma(I)
_cod_data_source_file            ic9808091_5.cif
_cod_data_source_block           2-MeOC6H4COS-+NMe4
_cod_original_cell_volume        1296.1(2)
_cod_original_sg_symbol_H-M      'P 21 21 21 '
_cod_original_formula_sum        'C12 H19 N O2 S '
_cod_database_code               4321766