Diammonium hexakis(thiocyanato-κ<i>N</i>)rhenate(IV) dimethyl sulfone tetrasolvate
Kochel, Andrzej; Hołyńska, Małgorzata; Acta Crystallographica Section C 67 (2011) m134–m136; doi:10.1107/S0108270111010535

data_2018058
_publ_section_title
;
 Diammonium hexakis(thiocyanato-\k<i>N</i>)rhenate(IV) dimethyl sulfone
 tetrasolvate
;
_journal_coeditor_code           FA3250
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              m134
_journal_page_last               m136
_journal_paper_doi               10.1107/S0108270111010535
_journal_volume                  67
_journal_year                    2011
_chemical_formula_iupac          '(N1 H4)2 [Re (N C S)6] , 4C2 H6 O2 S'
_chemical_formula_moiety         '2(H4 N +), C6 N6 Re S6 2-, 4(C2 H6 O2 S)'
_chemical_formula_sum            'C14 H32 N8 O8 Re S10'
_chemical_formula_weight         947.28
_chemical_name_systematic
;
Diammonium hexakis(thiocyanato-\k<i>N</i>)rhenate(IV) dimethyl sulfone
tetrasolvate
;
_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           SHELXL97
_cell_angle_alpha                90.00
_cell_angle_beta                 113.57(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   13.128(3)
_cell_length_b                   9.493(3)
_cell_length_c                   15.412(4)
_cell_measurement_reflns_used    3295
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      28.73
_cell_measurement_theta_min      2.88
_cell_volume                     1760.5(9)
_computing_cell_refinement       'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_data_collection       'CrysAlis CCD (Oxford Diffraction, 2009)'
_computing_data_reduction        'CrysAlis RED (Oxford Diffraction, 2009)'
_computing_molecular_graphics
;
DIAMOND (Brandenburg, 2010) and SHELXTL (Sheldrick, 2008)
;
_computing_publication_material  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.928
_diffrn_measurement_device_type  'Oxford KM-4 CCD area-detector'
_diffrn_measurement_method       \w
_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  0.0250
_diffrn_reflns_av_sigmaI/netI    0.0270
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            11719
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         28.73
_diffrn_reflns_theta_min         2.88
_exptl_absorpt_coefficient_mu    4.092
_exptl_absorpt_correction_T_max  0.956
_exptl_absorpt_correction_T_min  0.789
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details   '(CrysAlis RED; Oxford Diffraction, 2009)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.787
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             942
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.88
_refine_diff_density_min         -0.74
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     191
_refine_ls_number_reflns         4234
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.004
_refine_ls_R_factor_all          0.0318
_refine_ls_R_factor_gt           0.0233
_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^)+(0.0355P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0555
_refine_ls_wR_factor_ref         0.0571
_reflns_number_gt                3483
_reflns_number_total             4234
_reflns_threshold_expression     I>2\s(I)
_cod_data_source_file            fa3250.cif
_cod_data_source_block           I
_cod_original_cell_volume        1760.5(8)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               2018058