The First Octahedral Cluster Complexes With Terminal Formate Ligands: Synthesis, Structure, and Properties of K4[Re6S8(HCOO)6] and Cs4[Re6S8(HCOO)6]
Konstantin A. Brylev; Yuri V. Mironov; Svetlana G. Kozlova; Vladimir E. Fedorov; Sung-Jin Kim; Hans-Jürgen Pietzsch; Holger Stephan; Akitaka Ito; Shoji Ishizaka; Noboru Kitamura; Inorganic Chemistry 48 (2009) 2309–2315; doi:10.1021/ic802178q

data_4301617
_publ_contact_author_address
;Nikolaev Institute of Inorganic Chemistry SB RAS,
3 Acad. Lavrentiev Prosp.,
630090 Novosibirsk, Russia
;
_publ_contact_author_email       kbrylev@gmail.com
_publ_contact_author_fax         '007 383 3309489'
_publ_contact_author_name        'Konstantin A. Brylev'
_publ_contact_author_phone       '007 383 3309253'
_publ_section_title
;
The First Octahedral Cluster Complexes With Terminal Formate Ligands:
Synthesis, Structure, and Properties of K4[Re6S8(HCOO)6] and
Cs4[Re6S8(HCOO)6]
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2309
_journal_page_last               2315
_journal_paper_doi               10.1021/ic802178q
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         K4[Re6S8(HCOO)6]
_chemical_formula_sum            'C6 H6 K4 O12 Re6 S8'
_chemical_formula_weight         1800.19
_chemical_name_systematic
'Potassium octakis(mu3-sulfido)-hexaformato-hexa-rhenium(III)'
_space_group_IT_number           205
_symmetry_cell_setting           cubic
_symmetry_Int_Tables_number      205
_symmetry_space_group_name_Hall  '-P 2ac 2ab 3'
_symmetry_space_group_name_H-M   'P a -3'
_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            8
_cell_length_a                   17.6324(3)
_cell_length_b                   17.6324(3)
_cell_length_c                   17.6324(3)
_cell_measurement_temperature    298(2)
_cell_volume                     5481.94(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      298(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'Bruker SMART APEX CCD'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0487
_diffrn_reflns_av_sigmaI/netI    0.0208
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28633
_diffrn_reflns_theta_full        25.67
_diffrn_reflns_theta_max         25.67
_diffrn_reflns_theta_min         2.00
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    27.657
_exptl_absorpt_correction_T_max  0.1685
_exptl_absorpt_correction_T_min  0.1685
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    4.362
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       cubic
_exptl_crystal_F_000             6336
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.214
_refine_diff_density_min         -1.190
_refine_diff_density_rms         0.194
_refine_ls_extinction_coef       0.000047(6)
_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   1.732
_refine_ls_matrix_type           full
_refine_ls_number_parameters     111
_refine_ls_number_reflns         1750
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.732
_refine_ls_R_factor_all          0.0257
_refine_ls_R_factor_gt           0.0208
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0079P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0444
_refine_ls_wR_factor_ref         0.0448
_reflns_number_gt                1550
_reflns_number_total             1750
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802178q_si_001_2.cif
_cod_data_source_block           compound1
_cod_database_code               4301617