Crystal structure of bis(ethylenedithio)tetrathiafulvalenium μ~2~-acetato-bis[tribromidorhenate(III)] 1,1,2-trichloroethane hemisolvate
Golichenko, Alexander A.; Kravchenko, Andrey V.; Omelchenko, Irina V.; Chudak, Denis M.; Starodub, Vladimir A.; Barszcz, Boleslaw; Shtemenko, Alexander V.; Acta Crystallographica Section E 72 (2016) 712–715; doi:10.1107/S2056989016006058

data_2241665
_publ_section_title
;
 Crystal structure of bis(ethylenedithio)tetrathiafulvalenium
 \m~2~-acetato-bis[tribromidorhenate(III)] 1,1,2-trichloroethane
 hemisolvate
;
_journal_coeditor_code           RZ5188
_journal_issue                   5
_journal_name_full               'Acta Crystallographica Section E'
_journal_page_first              712
_journal_page_last               715
_journal_paper_doi               10.1107/S2056989016006058
_journal_volume                  72
_journal_year                    2016
_chemical_formula_iupac
'(C10 H8 S8) [Re2 Br6 (C2 H3 O2)], 0.5C2 H3 Cl3'
_chemical_formula_moiety
'C10 H8 S8 +, C2 H3 Br6 O2 Re2 -, C H1.5 Cl1.5'
_chemical_formula_sum            'C13 H12.5 Br6 Cl1.5 O2 Re2 S8'
_chemical_formula_weight         1362.24
_chemical_name_systematic
;
Bis(ethylenedithio)tetrathiafulvalenium
\m~2~-acetato-bis[tribromidorhenate(III)] 1,1,2-trichloroethane hemisolvate
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2ya'
_space_group_name_H-M_alt        'I 1 2/a 1'
_symmetry_space_group_name_Hall  '-I 2ya'
_symmetry_space_group_name_H-M   'I 1 2/a 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method
;
Olex2 1.2
(compiled 2015.09.30 svn.r3233 for OlexSys, GUI svn.r5103)
;
_cell_angle_alpha                90.00
_cell_angle_beta                 100.8440(17)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   27.1825(5)
_cell_length_b                   8.53737(13)
_cell_length_c                   26.0667(5)
_cell_measurement_reflns_used    18811
_cell_measurement_temperature    298
_cell_measurement_theta_max      30.6800
_cell_measurement_theta_min      2.9210
_cell_volume                     5941.20(19)
_computing_cell_refinement
;
<i>CrysAlis PRO</i> (Agilent, 2014)
;
_computing_data_collection
;
<i>CrysAlis PRO</i> (Agilent, 2014)
;
_computing_data_reduction
;
<i>CrysAlis PRO</i> (Agilent, 2014)
;
_computing_molecular_graphics
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_publication_material
;
<i>OLEX2</i> (Dolomanov <i>et al.</i>,  2009)
;
_computing_structure_refinement
;
SHELXL2014 (Sheldrick, 2015)
;
_computing_structure_solution
;
SHELXS97 (Sheldrick, 2008)
;
_diffrn_ambient_temperature      298
_diffrn_detector_area_resol_mean 16.1827
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.989
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Agilent Xcalibur Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0394
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -35
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            36051
_diffrn_reflns_theta_full        27.50
_diffrn_reflns_theta_max         27.50
_diffrn_reflns_theta_min         2.86
_exptl_absorpt_coefficient_mu    16.925
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.06678
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
(<i>CrysAlis PRO</i>; Agilent, 2014)
;
_exptl_crystal_colour            'metallic dark violet'
_exptl_crystal_density_diffrn    3.046
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4960
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.4
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.767
_refine_diff_density_min         -1.903
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.136
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     334
_refine_ls_number_reflns         6755
_refine_ls_number_restraints     99
_refine_ls_restrained_S_all      1.999
_refine_ls_R_factor_all          0.0555
_refine_ls_R_factor_gt           0.0521
_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^)+(0.0534P)^2^+229.8497P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1357
_refine_ls_wR_factor_ref         0.1373
_reflns_number_gt                6304
_reflns_number_total             6755
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            rz5188sup1.cif
_cod_data_source_block           I
_cod_original_cell_volume        5941.21(18)
_cod_original_formula_sum        'C13 H12.50 Br6 Cl1.50 O2 Re2 S8'
_cod_database_code               2241665
_cod_database_fobs_code 2241665