(NBun4+)3[Re6S8Cl6]3−·: synthesis and luminescence of the paramagnetic, open shell member of a hexanuclear chalcohalide cluster redox system
Guilbaud, Christophe; Deluzet, André; Domercq, Benoît; Molinié, Philippe; Boubekeur, Kamal; Batail, Patrick; Coulon, Claude; Chemical Communications  (1999) 1867–; doi:10.1039/a904669k

data_7110618
_publ_section_title
;
 (NBun4+)3[Re6S8Cl6]3&#x2212;&#x00B7;: synthesis and luminescence of the
 paramagnetic, open shell member of a hexanuclear chalcohalide cluster
 redox system
;
_journal_issue                   18
_journal_name_full               'Chemical Communications'
_journal_page_first              1867
_journal_paper_doi               10.1039/a904669k
_journal_year                    1999
_chemical_formula_moiety         '(C16 H36 N 1+)3, Re6 S8 Cl6 3-'
_chemical_formula_structural     '((C4H9)4N)3 (Re6S8Cl6)'
_chemical_formula_sum            'C48 H108 Cl6 N3 Re6 S8'
_chemical_formula_weight         2313.80
_chemical_name_common            '(nBu4N)3 [Re6S8Cl6]'
_chemical_name_systematic
;  
tris-tetra-n-butylammonium octa-\m~eq~3-sulfido- 
hexachloro-octahedro-hexarhenate(III)  
;
_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                95.794(15)
_cell_angle_beta                 106.581(13)
_cell_angle_gamma                103.570(10)
_cell_formula_units_Z            2
_cell_length_a                   12.5106(15)
_cell_length_b                   17.789(2)
_cell_length_c                   18.139(2)
_cell_measurement_reflns_used    5000
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.80
_cell_measurement_theta_min      1.65
_cell_volume                     3699.4(8)
_computing_cell_refinement       'SELECT (Stoe IPDS)'
_computing_data_collection       'EXPOSE (Stoe IPDS)'
_computing_data_reduction        'INTEGRATE (Stoe IPDS)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_max 1.0
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'Rotation, \D\f=3\%'
_diffrn_radiation_detector       'area detector'
_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  0.0915
_diffrn_reflns_av_sigmaI/netI    0.0808
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            35884
_diffrn_reflns_reduction_process 'INTEGRATE (Stoe IPDS)'
_diffrn_reflns_theta_full        25.80
_diffrn_reflns_theta_max         25.80
_diffrn_reflns_theta_min         1.65
_exptl_absorpt_coefficient_mu    10.250
_exptl_absorpt_correction_T_max  0.8095
_exptl_absorpt_correction_T_min  0.0650
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'FACEIT (Stoe IPDS)'
_exptl_crystal_colour            'orange red'
_exptl_crystal_density_diffrn    2.077
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2194
_exptl_crystal_size_max          0.56
_exptl_crystal_size_mid          0.23
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.781
_refine_diff_density_min         -1.762
_refine_diff_density_rms         0.170
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.816
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     669
_refine_ls_number_reflns         13220
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.819
_refine_ls_R_factor_all          0.0546
_refine_ls_R_factor_gt           0.0329
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0234P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0674
_refine_ls_wR_factor_ref         0.0712
_reflns_number_gt                9098
_reflns_number_total             13220
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            904669ksup1.cif
_cod_data_source_block           tba4rt
_cod_depositor_comments
;
The following automatic conversions were performed:
'_atom_site_symetry_multiplicity' tag replaced with
'_atom_site_symmetry_multiplicity'.

Automatic conversion script
Id: cif_correct_tags 1440 2010-10-19 06:21:57Z saulius 

The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to /home/saulius/struct/CIF-dictionaries/cif_core.dic
dictionary named 'cif_core.dic' version 2.4.2 from 2011-04-26.

Automatic conversion script
Id: cif_fix_values 1891 2012-01-12 08:04:46Z andrius 

The following automatic conversions were performed:

'_exptl_crystal_density_meas' value 'not measured' was changed to '?'
- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 
;
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7110618