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_4315884
_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
'3(C6 N6 Se8 Tc6), 8(C4 H12 N), 4(C4 N), 8(O) '
_chemical_formula_sum            'C66 H96 N30 O8 Se24 Tc18'
_chemical_formula_weight         5114.72
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_Int_Tables_number      14
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_cell_angle_alpha                90
_cell_angle_beta                 101.40(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.41(1)
_cell_length_b                   32.55(2)
_cell_length_c                   20.29(2)
_cell_measurement_reflns_used    1994
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      26.3
_cell_measurement_theta_min      3.1
_cell_volume                     7387(11)
_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    SIR92
_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  0.091
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       42
_diffrn_reflns_limit_k_min       -42
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            42821
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.48
_exptl_absorpt_coefficient_mu    7.566
_exptl_absorpt_correction_T_max  0.469
_exptl_absorpt_correction_T_min  0.170
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(Higashi, 1995)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.283
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             4712.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.100
_refine_diff_density_max         1.81
_refine_diff_density_min         -0.83
_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   1.129
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     592
_refine_ls_number_reflns         15871
_refine_ls_R_factor_gt           0.0476
_refine_ls_shift/su_max          0.0060
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.0150P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.0920
_reflns_number_gt                5929
_reflns_number_total             15871
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ic1000717_si_002_2.cif
_cod_data_source_block           (NMe4)4[Tc6Se8(CN)6]
_cod_original_cell_volume        7387(9)
_cod_original_sg_symbol_H-M      'P 21/n '
_cod_original_formula_sum        'C66 H96 N30 O8 Se24 Tc18 '
_cod_database_code               4315884