The Mixed Polychalcogenorhenate(IV) Anions [Re4Q4(S3)4(S4)2]4- (Q = Se, Te): Syntheses and Crystal Structures of [NMe4]5[Me2NH2]3[Re4Se4(S3)4(S4)2]2.2.25H2O and [NH4]4[Re4Te4(S3)4(S4)2].8H2O
Yuri V. Mironov; Michael A. Pell; Thomas E. Albrecht-Schmitt; James A. Ibers; Inorganic Chemistry 40 (2001) 5472–5474; doi:10.1021/ic010434a

data_4320352
_publ_section_title
;
 The Mixed Polychalcogenorhenate(IV) Anions [Re4Q4(S3)4(S4)2]4- (Q = Se,
 Te): Syntheses and Crystal Structures of
 [NMe4]5[Me2NH2]3[Re4Se4(S3)4(S4)2]2.2.25H2O and
 [NH4]4[Re4Te4(S3)4(S4)2].8H2O
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5472
_journal_page_last               5474
_journal_paper_doi               10.1021/ic010434a
_journal_volume                  40
_journal_year                    2001
_chemical_formula_sum            'C26 H88.5 N8 O2.25 Re8 S40 Se8'
_chemical_formula_weight         3953.2
_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                 93.135(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.5552(12)
_cell_length_b                   38.397(4)
_cell_length_c                   19.4653(19)
_cell_measurement_temperature    153(2)
_cell_volume                     9369.8(16)
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      153(2)
_diffrn_measured_fraction_theta_full 0.931
_diffrn_measured_fraction_theta_max 0.931
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'standard-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1227
_diffrn_reflns_av_sigmaI/netI    0.1180
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       51
_diffrn_reflns_limit_k_min       -52
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            111257
_diffrn_reflns_theta_full        28.88
_diffrn_reflns_theta_max         28.88
_diffrn_reflns_theta_min         1.06
_exptl_absorpt_coefficient_mu    14.324
_exptl_absorpt_correction_T_max  0.60245
_exptl_absorpt_correction_T_min  0.09659
_exptl_crystal_colour            dark_red
_exptl_crystal_density_diffrn    2.799
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             7312
_exptl_crystal_size_max          0.252
_exptl_crystal_size_mid          0.044
_exptl_crystal_size_min          0.038
_refine_diff_density_max         2.925
_refine_diff_density_min         -2.274
_refine_diff_density_rms         0.357
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.102
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     838
_refine_ls_number_reflns         22937
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.102
_refine_ls_R_factor_all          0.1414
_refine_ls_R_factor_gt           0.0560
_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
   [1.00000+0.00000exp(0.00(sin\q/\l)^2^)]/
     [\s^2^(Fo^2^)+0.0000+0.0000*P+(0.0400P)^2^+0.0000sin\q/\l]
   where P = 1.00000Fo^2^ + 0.00000Fc^2^
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0976
_refine_ls_wR_factor_ref         0.1228
_reflns_number_gt                12754
_reflns_number_total             22937
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic010434a_1.cif
_cod_data_source_block           sad
_cod_database_code               4320352