Synthesis of Re^I^ tricarbonyl complexes with various sulfur- and oxygen-donating ligands: crystal structures of two Re^I^ dinuclear structures bridged by S atoms
Nkoe, Pheello I.; Visser, Hendrik G.; Swart, Chantel; Brink, Alice; Schutte-Smith, Marietjie; Acta Crystallographica Section C 74 (2018) 1116–1122; doi:10.1107/S205322961801207X

data_2021228
_publ_section_title
;
 Synthesis of Re^I^ tricarbonyl complexes with various sulfur- and
 oxygen-donating ligands: crystal structures of two Re^I^ dinuclear
 structures bridged by S atoms
;
_journal_coeditor_code           YP3163
_journal_issue                   10
_journal_name_full               'Acta Crystallographica Section C'
_journal_page_first              1116
_journal_page_last               1122
_journal_paper_doi               10.1107/S205322961801207X
_journal_volume                  74
_journal_year                    2018
_chemical_formula_iupac          '(C8 H20 N) [Re2 (C7 H7 O S)3 (C O)6]'
_chemical_formula_moiety         'C8 H20 N +, C27 H21 O9 Re2 S3 -'
_chemical_formula_sum            'C35 H41 N O9 Re2 S3'
_chemical_formula_weight         1088.27
_chemical_name_systematic
;Tetraethylammonium
<i>fac</i>-tris(\m-2-methoxybenzenethiolato-\k^2^<i>S</i>:<i>S</i>)bis[tricarbonylrhenium(I)]
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           9
_space_group_name_Hall           'C -2yc'
_space_group_name_H-M_alt        'C 1 c 1'
_symmetry_space_group_name_Hall  'C -2yc'
_symmetry_space_group_name_H-M   'C 1 c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 91.470(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   12.7120(5)
_cell_length_b                   17.1050(6)
_cell_length_c                   18.1440(10)
_cell_measurement_reflns_used    9974
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.98
_cell_measurement_theta_min      2.31
_cell_volume                     3943.9(3)
_computing_cell_refinement
;
SAINT-Plus (Bruker, 2008)
;
_computing_data_collection
;
APEX2 (Bruker, 2008)
;
_computing_data_reduction
;
SAINT-Plus and XPREP (Bruker, 2008)
;
_computing_molecular_graphics
;
DIAMOND (Brandenburg & Putz, 2005)
;
_computing_publication_material
;
SHELXL2014 (Sheldrick, 2015) and WinGX (Farrugia, 2012)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015) and WinGX (Farrugia, 2012)
;
_computing_structure_solution
;
SIR97 (Altomare <i>et al.</i>, 1999)
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEXII CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0851
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            36944
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.334
_diffrn_reflns_theta_min         2.975
_exptl_absorpt_coefficient_mu    6.343
_exptl_absorpt_correction_T_max  0.455
_exptl_absorpt_correction_T_min  0.294
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(SADABS; Bruker, 2008)
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.833
_exptl_crystal_description       cuboid
_exptl_crystal_F_000             2112
_exptl_crystal_size_max          0.303
_exptl_crystal_size_mid          0.166
_exptl_crystal_size_min          0.124
_refine_diff_density_max         0.867
_refine_diff_density_min         -0.951
_refine_ls_abs_structure_details
;
Flack x determined using 3336 quotients [(I+)-(I-)]/[(I+)+(I-)]
(Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.005(7)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.918
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     491
_refine_ls_number_reflns         9551
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.918
_refine_ls_R_factor_all          0.0435
_refine_ls_R_factor_gt           0.0328
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     'w=1/[\s^2^(Fo^2^)] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0634
_refine_ls_wR_factor_ref         0.0682
_reflns_number_gt                8238
_reflns_number_total             9829
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            yp3163sup1.cif
_cod_data_source_block           14cpn4_0ma
_cod_depositor_comments
'Adding full bibliography for 2021227--2021228.cif.'
_cod_database_code               2021228
_cod_database_fobs_code          2021228
_shelx_estimated_absorpt_t_min   0.250
_shelx_estimated_absorpt_t_max   0.507
_shelx_hkl_checksum              56937
_shelx_res_checksum              60731