Synthesis, Spectroscopic and Electrochemical Properties, and Electronic Structures of Octahedral Hexatechnetium(III) Clusters [Tc6Q8(CN)6]4- (Q = S, Se)
Takashi Yoshimura; Takuya Ikai; Tsutomu Takayama; Tsutomu Sekine; Yasushi Kino; Atsushi Shinohara; Inorganic Chemistry 49 (2010) 5876–5882; doi:10.1021/ic1000717

data_4315883
_publ_section_title
;
 Synthesis, Spectroscopic and Electrochemical Properties, and Electronic
 Structures of Octahedral Hexatechnetium(III) Clusters [Tc6Q8(CN)6]4- (Q =
 S, Se)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5876
_journal_page_last               5882
_journal_paper_doi               10.1021/ic1000717
_journal_volume                  49
_journal_year                    2010
_chemical_formula_moiety         'C6 N6 S8 Tc6, 4(C4 H12 N), 4(O)'
_chemical_formula_sum            'C22 H48 N10 O4 S8 Tc6'
_chemical_formula_weight         1367.22
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      15
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_cell_angle_alpha                90
_cell_angle_beta                 112.00(1)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   20.191(7)
_cell_length_b                   11.659(4)
_cell_length_c                   23.201(7)
_cell_measurement_reflns_used    17926
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      27.4
_cell_measurement_theta_min      3.1
_cell_volume                     5064(3)
_computing_cell_refinement       PROCESS-AUTO
_computing_data_collection       PROCESS-AUTO
_computing_data_reduction        'teXsan Ver. 2.0'
_computing_publication_material  'teXsan Ver. 2.0'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    SHELXS86
_diffrn_ambient_temperature      296.2
_diffrn_detector_area_resol_mean 10.00
_diffrn_measured_fraction_theta_full 1.0
_diffrn_measurement_device_type  'Rigaku RAXIS-RAPID Imaging Plate'
_diffrn_measurement_method       \w
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.051
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            24574
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.43
_exptl_absorpt_coefficient_mu    1.941
_exptl_absorpt_correction_T_max  0.615
_exptl_absorpt_correction_T_min  0.383
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.793
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             2672.00
_exptl_crystal_size_max          0.250
_exptl_crystal_size_mid          0.250
_exptl_crystal_size_min          0.250
_refine_diff_density_max         1.24
_refine_diff_density_min         -0.91
_refine_ls_extinction_coef       0.0000
_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   1.088
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     216
_refine_ls_number_reflns         5703
_refine_ls_R_factor_gt           0.0463
_refine_ls_shift/su_max          0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.0877P)^2^+24.7310P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.1613
_reflns_number_gt                4847
_reflns_number_total             5703
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ic1000717_si_002_1.cif
_cod_data_source_block           (NMe4)4[Tc6S8(CN)6]
_cod_original_cell_volume        5063(3)
_cod_original_sg_symbol_H-M      'C 2/c '
_cod_original_formula_sum        'C22 H48 N10 O4 S8 Tc6 '
_cod_database_code               4315883