Layered K4[Re6S10(CN)2] and Chainlike K4[Re6Se10(CN)4]: New Types of Chalcocyanide Cluster Compounds with Bridging Chalcogenide Ligands
Yuri V. Mironov; Vladimir E. Fedorov; Craig C. McLauchlan; James A. Ibers; Inorganic Chemistry 39 (2000) 1809–1811; doi:10.1021/ic990936c

data_4320864
_publ_section_title
;
 Layered K4[Re6S10(CN)2] and Chainlike K4[Re6Se10(CN)4]: New Types of
 Chalcocyanide Cluster Compounds with Bridging Chalcogenide Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1809
_journal_page_last               1811
_journal_paper_doi               10.1021/ic990936c
_journal_volume                  39
_journal_year                    2000
_chemical_formula_moiety         '(K4) (C2 N2 Re6 S10)'
_chemical_formula_sum            'C2 K4 N2 Re6 S10'
_chemical_formula_weight         1646.24
_chemical_name_systematic
; 
 potassium dicyano-octa-\m3-sulfido-tetrasulfido-octahedro-
 hexarhenate(III)
;
_space_group_IT_number           53
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2'
_symmetry_space_group_name_H-M   'P m n a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   11.183(11)
_cell_length_b                   9.198(9)
_cell_length_c                   10.028(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      20
_cell_measurement_theta_min      15
_cell_volume                     1031.5(17)
_computing_cell_refinement       'CELLREF(local program)'
_computing_data_collection       'PCPS(local program)'
_computing_data_reduction        'NUPICK,(local program)'
_computing_molecular_graphics    'SHELXTL-97 (Sheldrick, 1997)'
_computing_publication_material  'SHELXTL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  Picker
_diffrn_measurement_method       \q/\2q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'standard sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.70930
_diffrn_reflns_av_R_equivalents  0.1562
_diffrn_reflns_av_sigmaI/netI    0.1044
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -10
_diffrn_reflns_number            7301
_diffrn_reflns_theta_full        31.50
_diffrn_reflns_theta_max         31.50
_diffrn_reflns_theta_min         2.72
_diffrn_standards_decay_%        '< 2'
_diffrn_standards_interval_count 100
_diffrn_standards_number         6
_exptl_absorpt_coefficient_mu    36.874
_exptl_absorpt_correction_type   'analytical (de Meulenaer & Tompa, 1965)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    5.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1424
_refine_diff_density_max         4.106
_refine_diff_density_min         -3.411
_refine_diff_density_rms         0.638
_refine_ls_extinction_coef       0.00018(9)
_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    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     69
_refine_ls_number_reflns         1811
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.088
_refine_ls_R_factor_all          0.1019
_refine_ls_R_factor_gt           0.0522
_refine_ls_shift/su_max          0.267
_refine_ls_shift/su_mean         0.017
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
; calc 
 1/[\s^2^(Fo^2^)+(0.0400Fo^2^)^2^]  
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1000
_refine_ls_wR_factor_ref         0.1138
_reflns_number_gt                1134
_reflns_number_total             1811
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic990936c_1.cif
_cod_data_source_block           rescn
_cod_original_cell_volume        1031.5(16)
_cod_database_code               4320864