Inertness of the [Re6Se5Cl3]5+ cluster core to substitution by OH− in organic solutions: synthesis, structural and liquid secondary ion mass spectroscopy characterization of K(H2O)2[Re6Se5Cl9] and (n-Bu4N)[Re6Se5Cl9] and the crystal structure of (n-Bu4N)2[Re6Se6Cl8]
Santiago Uriel; Kamal Boubekeur; Patrick Batail; Jesus Orduna; André Perrin; New J. Chem. 25 (2001) 737–740; doi:10.1039/b005231k

data_7051021
_publ_section_title
;
 Inertness of the [Re6Se5Cl3]5+ cluster core to substitution by
 OH&#x2212; in organic solutions: synthesis, structural and liquid
 secondary ion mass spectroscopy characterization of K(H2O)2[Re6Se5Cl9]
 and (n-Bu4N)[Re6Se5Cl9] and the crystal structure of
 (n-Bu4N)2[Re6Se6Cl8]
;
_journal_issue                   5
_journal_name_full               'New J. Chem.'
_journal_page_first              737
_journal_page_last               740
_journal_paper_doi               10.1039/b005231k
_journal_volume                  25
_journal_year                    2001
_chemical_formula_moiety         '(C16 H36 N 1+)2, Re6 Se6 Cl8 2-'
_chemical_formula_structural     '((C4H9)4N)2 (Re6Se6Cl8)'
_chemical_formula_sum            'C32 H72 Cl8 N2 Re6 Se6'
_chemical_formula_weight         2359.48
_chemical_name_common            (nBu4N)2[Re6Se6Cl8]
_chemical_name_systematic
; 
bis-tetra-n-butylammonium hexa-\m~eq~3-seleno-di-\m~eq~3-chloro-
hexachloro-octahedro-hexarhenate(III) 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.04(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   12.833(3)
_cell_length_b                   11.588(2)
_cell_length_c                   18.563(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.1
_cell_measurement_theta_min      6.2
_cell_volume                     2760.5(10)
_computing_cell_refinement       'CAD4 EXPRESS'
_computing_data_collection       'CAD4 EXPRESS'
_computing_data_reduction        'XCAD4 (Harms, 1993)'
_computing_molecular_graphics    'ORTEP (Johnson, 1976)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.949
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w--2\q
_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  0.0240
_diffrn_reflns_av_sigmaI/netI    0.0528
_diffrn_refln_scan_width         1.00
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            4605
_diffrn_reflns_theta_full        24.97
_diffrn_reflns_theta_max         24.97
_diffrn_reflns_theta_min         1.93
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    17.472
_exptl_absorpt_correction_T_max  0.2740
_exptl_absorpt_correction_T_min  0.2740
_exptl_absorpt_correction_type   psi-scan
_exptl_absorpt_process_details   'SHELXTL (Sheldrick, 1995)'
_exptl_crystal_colour            'intense red'
_exptl_crystal_density_diffrn    2.839
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       octahedron
_exptl_crystal_F_000             2136
_exptl_crystal_size_max          0.11
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.069
_refine_diff_density_min         -3.293
_refine_diff_density_rms         0.674
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.201
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     252
_refine_ls_number_reflns         4605
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.201
_refine_ls_R_factor_all          0.1272
_refine_ls_R_factor_gt           0.0539
_refine_ls_shift/su_max          0.051
_refine_ls_shift/su_mean         0.003
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1588
_refine_ls_wR_factor_ref         0.1885
_reflns_number_gt                2657
_reflns_number_total             4605
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b005231k.txt
_cod_data_source_block           tba2rese
_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 
;
_cod_original_cell_volume        2760.3(10)
_cod_original_sg_symbol_H-M      P2(1)/n
_cod_database_code               7051021