Selective Two-Step Oxidation of μ2-S Ligands in Trigonal Prismatic Unit {Re3(μ6-C)(μ2-S)3Re3} of the Bioctahedral Cluster Anion [Re12CS17(CN)6]6-
Yuri V. Mironov; Yakov M. Gayfulin; Svetlana G. Kozlova; Anton I. Smolentsev; Maria S. Tarasenko; Anton S. Nizovtsev; Vladimir E. Fedorov; Inorganic Chemistry 51 (2012) 4359–4367; doi:10.1021/ic300051w

data_4328835
_publ_contact_author_address
;Nikolaev Institute of Inorganic Chemistry,
SB Russian Academy of Sciences,
Akad. Lavrentiev prospekt 3,
Novosibirsk,
630090, Russian Federation 
;
_publ_contact_author_email       yuri@niic.nsc.ru
_publ_contact_author_fax         '+7 (383) 3309489'
_publ_contact_author_name        'Prof. Y.V. Mironov'
_publ_contact_author_phone       '+7 (383) 3309466'
_publ_section_title
;
 Selective Two-Step Oxidation of \m2-S Ligands in Trigonal Prismatic Unit
 {Re3(\m6-C)(\m2-S)3Re3} of the Bioctahedral Cluster Anion
 [Re12CS17(CN)6]6-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4359
_journal_page_last               4367
_journal_paper_doi               10.1021/ic300051w
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         '(C7 N6 O6 Re12 S17), (H18 N6 Ni)3, 4(H2 O)'
_chemical_formula_sum            'C7 H62 N24 Ni3 O10 Re12 S17'
_chemical_formula_weight         3598.36
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                120.00
_cell_formula_units_Z            6
_cell_length_a                   12.1632(6)
_cell_length_b                   12.1632(6)
_cell_length_c                   79.544(4)
_cell_measurement_reflns_used    8472
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.52
_cell_measurement_theta_min      2.82
_cell_volume                     10191.4(9)
_computing_cell_refinement       'SAINT (Bruker, 2004)'
_computing_data_collection       'APEX2 (Bruker, 2004)'
_computing_data_reduction        'SAINT (Bruker, 2004)'
_computing_molecular_graphics    'SHELXTL (Bruker, 2004)'
_computing_publication_material  'SHELXTL (Bruker, 2004)'
_computing_structure_refinement  'SHELXTL (Bruker, 2004)'
_computing_structure_solution    'SHELXTL (Bruker, 2004)'
_diffrn_ambient_temperature      150(2)
_diffrn_detector_area_resol_mean 25
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Nonius X8Apex CCD area-detector'
_diffrn_measurement_method       '\f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0446
_diffrn_reflns_av_sigmaI/netI    0.0296
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       89
_diffrn_reflns_limit_l_min       -99
_diffrn_reflns_number            11145
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.19
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    22.658
_exptl_absorpt_correction_T_max  0.3971
_exptl_absorpt_correction_T_min  0.0928
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.518
_exptl_crystal_description       plate
_exptl_crystal_F_000             9648
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         2.549
_refine_diff_density_min         -2.927
_refine_diff_density_rms         0.316
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.389
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     126
_refine_ls_number_reflns         2329
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.384
_refine_ls_R_factor_all          0.0624
_refine_ls_R_factor_gt           0.0559
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0000P)^2^+1984.3213P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1184
_refine_ls_wR_factor_ref         0.1199
_reflns_number_gt                2075
_reflns_number_total             2329
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300051w_si_001_2.cif
_cod_data_source_block           compound4
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-10-20
;
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4328835