Jahn-Teller distortion of the open-shell 23-electron chalcogenide rhenium cluster cores in crystals of the series, {[Re~6~Q~8~]^3+^(X^-^)~6~}^3-^ (Q = S, Se; X = Cl, CN)
Baudron, Stéphane A.; Deluzet, André; Boubekeur, Kamal; Batail, Patrick; Chemical Communications  (2002) 2124–2125; doi:10.1039/b205241e

data_7114031
_publ_section_title
;
 Jahn-Teller distortion of the open-shell 23-electron chalcogenide
 rhenium cluster cores in crystals of the series, 
{[Re~6~Q~8~]^3+^(X^-^)~6~}^3-^ (Q = S, Se; X = Cl, CN)
;
_journal_issue                   18
_journal_name_full               'Chemical Communications'
_journal_page_first              2124
_journal_page_last               2125
_journal_paper_doi               10.1039/b205241e
_journal_year                    2002
_chemical_formula_moiety         '(N(C4H9)4)3 [Re6S8Cl6]'
_chemical_formula_sum            'C48 H108 Cl6 N3 Re6 S8'
_chemical_formula_weight         2313.75
_chemical_name_common            (TBA)3[Re6S8Cl6]
_chemical_name_systematic
; 
tris (tetrabutylammonium)(octa-\m~eq~3-sulfido-hexachloro-octahedro-
rhenate(IV)pentarhenate(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                96.07(3)
_cell_angle_beta                 106.44(3)
_cell_angle_gamma                103.89(3)
_cell_formula_units_Z            2
_cell_length_a                   12.422(3)
_cell_length_b                   17.341(4)
_cell_length_c                   18.197(4)
_cell_measurement_reflns_used    8000
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      26.05
_cell_measurement_theta_min      1.65
_cell_volume                     3585.6(17)
_computing_cell_refinement       'SELECT (Stoe IPDS)'
_computing_data_collection       'EXPOSE (Stoe IPDS)'
_computing_data_reduction        'INTEGRATE (Stoe IPDS)'
_computing_molecular_graphics    'DIAMOND (Brandenburg, 1999)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.66
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       'Oscillation, \D\f==1.2%'
_diffrn_radiation_detector       'area detector'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0686
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            13792
_diffrn_reflns_theta_full        25.82
_diffrn_reflns_theta_max         25.82
_diffrn_reflns_theta_min         1.80
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    10.576
_exptl_absorpt_correction_T_max  0.7324
_exptl_absorpt_correction_T_min  0.0629
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   'FACEIT (Stoe IPDS)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    2.143
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2194
_exptl_crystal_size_max          0.52
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.03
_refine_diff_density_max         3.312
_refine_diff_density_min         -3.743
_refine_diff_density_rms         0.342
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.889
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         13792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.889
_refine_ls_R_factor_all          0.0492
_refine_ls_R_factor_gt           0.0381
_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^)+(0.0873P)^2^+0.0000P] where P==(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0942
_refine_ls_wR_factor_ref         0.1076
_reflns_number_gt                10165
_reflns_number_total             13792
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b205241e.txt
_cod_data_source_block           test3
_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:

'_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_cell_volume        3585.4(12)
_cod_original_sg_symbol_H-M      P-1
_cod_database_code               7114031