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_4315885
_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         '2(C24 H20 P), 0.5(C6 N6 Se8 Tc6), C2 H3 N '
_chemical_formula_sum            'C106 H86 N8 P4 Se8 Tc6'
_chemical_formula_weight         2809.47
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_Int_Tables_number      2
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_cell_angle_alpha                84.00(2)
_cell_angle_beta                 101.42(1)
_cell_angle_gamma                70.48(1)
_cell_formula_units_Z            1
_cell_length_a                   13.159(2)
_cell_length_b                   16.940(3)
_cell_length_c                   12.616(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    296.2
_cell_measurement_theta_max      15.0
_cell_measurement_theta_min      14.3
_cell_volume                     2553.4(8)
_computing_cell_refinement       'MSC/AFC Diffractometer Control'
_computing_data_collection       'MSC/AFC Diffractometer Control'
_computing_data_reduction        'teXsan Ver. 2.0'
_computing_publication_material  'teXsan Ver. 2.0'
_computing_structure_refinement  SHELXL97
_computing_structure_solution    'DIRDIF94 (PATTY)'
_diffrn_ambient_temperature      296.2
_diffrn_measured_fraction_theta_full 1.0
_diffrn_measurement_device_type  'Rigaku AFC5R'
_diffrn_measurement_method       \w-2\q
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.7107
_diffrn_reflns_av_R_equivalents  0.096
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            12170
_diffrn_reflns_theta_full        27.62
_diffrn_reflns_theta_max         27.62
_diffrn_standards_decay_%        7.48
_diffrn_standards_interval_count 150
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.747
_exptl_absorpt_correction_T_max  0.998
_exptl_absorpt_correction_T_min  0.844
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   '(North, Phillips & Mathews, 1968)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.827
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       platelet
_exptl_crystal_F_000             1368.00
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.300
_exptl_crystal_size_min          0.200
_refine_diff_density_max         1.85
_refine_diff_density_min         -1.44
_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   0.879
_refine_ls_hydrogen_treatment    noref
_refine_ls_number_parameters     595
_refine_ls_number_reflns         11770
_refine_ls_R_factor_gt           0.0595
_refine_ls_shift/su_max          -0.0010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w = 1/[\s^2^(Fo^2^) + (0.1036P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_ref         0.2132
_reflns_number_gt                4274
_reflns_number_total             11770
_reflns_threshold_expression     >2.0sigma(I)
_cod_data_source_file            ic1000717_si_002_3.cif
_cod_data_source_block           PPh4Tc6Se8CN6
_cod_original_sg_symbol_H-M      'P -1 '
_cod_original_formula_sum        'C106 H86 N8 P4 Se8 Tc6 '
_cod_database_code               4315885