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_4328836
_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 H12 Cu N10 O7 Re12 S17)0.4,(C7 N6 O6 Re12 S17)0.6, (Cu H15 N5)2.6, 5(H2 O)'
_chemical_formula_sum            'C7 H53.8 Cu3 N20.6 O11.4 Re12 S17'
_chemical_formula_weight         3579.35
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 126.296(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.0539(5)
_cell_length_b                   19.4392(6)
_cell_length_c                   25.4215(7)
_cell_measurement_reflns_used    9909
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      27.45
_cell_measurement_theta_min      2.53
_cell_volume                     6394.1(4)
_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 0.996
_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  0.0549
_diffrn_reflns_av_sigmaI/netI    0.0531
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            48415
_diffrn_reflns_theta_full        25.25
_diffrn_reflns_theta_max         27.54
_diffrn_reflns_theta_min         1.89
_diffrn_standards_decay_%        0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    24.183
_exptl_absorpt_correction_T_max  0.3248
_exptl_absorpt_correction_T_min  0.1594
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Bruker, 2004)'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    3.697
_exptl_crystal_description       block
_exptl_crystal_F_000             6321
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         4.492
_refine_diff_density_min         -3.150
_refine_diff_density_rms         0.322
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.090
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     706
_refine_ls_number_reflns         14705
_refine_ls_number_restraints     49
_refine_ls_restrained_S_all      1.090
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0458
_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^)+(0.0528P)^2^+48.1021P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1143
_refine_ls_wR_factor_ref         0.1249
_reflns_number_gt                10120
_reflns_number_total             14705
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic300051w_si_001_3.cif
_cod_data_source_block           compound7
_cod_depositor_comments
;
 Marking attached hydrogen atoms.

 Antanas Vaitkus,
 2017-10-20
;
_cod_original_cell_volume        6394.1(3)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4328836