Preparation, Structures, and Redox and Emission Characteristics of the Isothiocyanate Complexes of Hexarhenium(III) Clusters [Re6(μ3-E)8(NCS)6]4- (E = S, Se)
Takashi Yoshimura; Zhong-Ning Chen; Ai Itasaka; Masaaki Abe; Yoichi Sasaki; Shoji Ishizaka; Noboru Kitamura; Spartak S. Yarovoi; Sergey F. Solodovnikov; Vladimir E. Fedorov; Inorganic Chemistry 42 (2003) 4857–4863; doi:10.1021/ic030030d

data_4313941
_publ_section_title
;
 Preparation, Structures, and Redox and Emission Characteristics of the
 Isothiocyanate Complexes of Hexarhenium(III) Clusters
 [Re6(\m3-E)8(NCS)6]4- (E = S, Se)
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4857
_journal_page_last               4863
_journal_paper_doi               10.1021/ic030030d
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C40.5 H36 N3.5 O P2 Re1.5 S1.5 Se2'
_chemical_formula_weight         1134.98
_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                84.07(1)
_cell_angle_beta                 84.95(1)
_cell_angle_gamma                74.21(1)
_cell_formula_units_Z            4
_cell_length_a                   15.263(2)
_cell_length_b                   16.429(2)
_cell_length_c                   17.111(2)
_cell_measurement_reflns_used    24
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      14.12
_cell_measurement_theta_min      10.19
_cell_volume                     4098.6(9)
_computing_cell_refinement       'CD4CAO (Enraf-Nonius)'
_computing_data_collection       'CD4CAO (Enraf-Nonius)'
_computing_data_reduction        'CADDAT (Enraf-Nonius)'
_computing_molecular_graphics    'local programs'
_computing_publication_material  'local programs'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.590
_diffrn_measured_fraction_theta_max 0.590
_diffrn_measurement_device_type  'Enraf-Nonius CAD4'
_diffrn_measurement_method       \q/2\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0314
_diffrn_reflns_av_sigmaI/netI    0.0892
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            11610
_diffrn_reflns_theta_full        27.47
_diffrn_reflns_theta_max         27.47
_diffrn_reflns_theta_min         1.20
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.400
_exptl_absorpt_correction_T_max  1.16377
_exptl_absorpt_correction_T_min  0.83623
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'CADDAT (Enraf-Nonius)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.839
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       fragment
_exptl_crystal_F_000             2184
_exptl_crystal_size_max          0.48
_exptl_crystal_size_mid          0.40
_exptl_crystal_size_min          0.40
_refine_diff_density_max         1.331
_refine_diff_density_min         -1.421
_refine_diff_density_rms         0.252
_refine_ls_extinction_coef       0.00089(3)
_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   0.952
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     938
_refine_ls_number_reflns         11057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.952
_refine_ls_R_factor_all          0.0625
_refine_ls_R_factor_gt           0.0309
_refine_ls_shift/su_max          0.051
_refine_ls_shift/su_mean         0.004
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0335P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0838
_reflns_number_gt                6902
_reflns_number_total             11057
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic030030d_2.cif
_cod_data_source_block
(P2NC36H30)4[Re6Se8(NCS)6].4(C3H6NO):Complex_2ao4DMF
_cod_depositor_comments
;
The following automatic conversions were performed:

data name '_atom_site_symetry_multiplicity' was replaced with
'_atom_site_symmetry_multiplicity' as specified in the replacement
file 'data/replacement-values/replacement_tags.lst'.

Automatic conversion script
Id: cif_correct_tags 9268 2022-04-12 08:56:07Z antanas 
;
_cod_original_formula_sum        'C40.50 H36 N3.50 O P2 Re1.50 S1.50 Se2'
_cod_database_code               4313941