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_4328834
_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), (Cu H15 N5)3, 9.5(H2 O)'
_chemical_formula_sum            'C7 H64 Cu3 N21 O15.5 Re12 S17'
_chemical_formula_weight         3660.83
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                84.1720(10)
_cell_angle_beta                 74.363(2)
_cell_angle_gamma                77.3660(10)
_cell_formula_units_Z            2
_cell_length_a                   13.2443(7)
_cell_length_b                   13.4391(7)
_cell_length_c                   19.0726(9)
_cell_measurement_reflns_used    9930
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      32.63
_cell_measurement_theta_min      2.40
_cell_volume                     3186.7(3)
_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 0.948
_diffrn_measured_fraction_theta_max 0.942
_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  0.0233
_diffrn_reflns_av_sigmaI/netI    0.0419
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            23904
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         27.48
_diffrn_reflns_theta_min         1.72
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    24.277
_exptl_absorpt_correction_T_max  0.5296
_exptl_absorpt_correction_T_min  0.1587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    3.815
_exptl_crystal_description       block
_exptl_crystal_F_000             3272
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.990
_refine_diff_density_min         -2.373
_refine_diff_density_rms         0.420
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.133
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     710
_refine_ls_number_reflns         13767
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0679
_refine_ls_R_factor_gt           0.0415
_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^)+(0.0637P)^2^+10.4015P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1238
_reflns_number_gt                10230
_reflns_number_total             13767
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300051w_si_001_1.cif
_cod_data_source_block           compound3
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-10-20
;
_cod_original_formula_sum        'C7 H64 Cu3 N21 O15.50 Re12 S17'
_cod_database_code               4328834