Mixed Chloride/Phosphine Complexes of the Dirhenium Core. 8. Synthesis and Crystal Structure of the Quadruply Bonded Dirhenium(III) Anion [Re2Cl7(PMe3)]-
F. Albert Cotton; Evgeny V. Dikarev; Marina A. Petrukhina; Inorganic Chemistry 40 (2001) 5716–5718; doi:10.1021/ic010504d

data_4320431
_publ_section_title
;
 Mixed Chloride/Phosphine Complexes of the Dirhenium Core. 8. Synthesis
 and Crystal Structure of the Quadruply Bonded Dirhenium(III) Anion
 [Re2Cl7(PMe3)]-
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5716
_journal_page_last               5718
_journal_paper_doi               10.1021/ic010504d
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety
;
  [(C4 H9)4 N]4 [Re2 Cl7 (P (C H3)3)]2 [Re2 Cl8], 2(C H2 Cl2)
;
_chemical_formula_structural
;
  4[n-Bu4N](+),2[Re2Cl7(PMe3)](-),[Re2Cl8](2-),2CH2Cl2
;
_chemical_formula_sum            'C72 H166 Cl26 N4 P2 Re6'
_chemical_formula_weight         3188.93
_chemical_melting_point          ?
_chemical_name_systematic
;
  Heptachloro-trimethylphosphine-di-rhenate(III,III),
  octachloro-di-rhenate(III,III),
  tetra-n-butylammonium salt, dichloromethane solvate
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.813(4)
_cell_length_b                   17.804(5)
_cell_length_c                   40.935(6)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      8.0
_cell_volume                     11525(5)
_computing_cell_refinement       'MADNES (Enraf-Nonius, 1989)'
_computing_data_collection       'MADNES (Enraf-Nonius, 1989)'
_computing_data_reduction        'PROCOR (Kabsch, 1988)'
_computing_molecular_graphics    'SHELXTL V.5 (Siemens, 1994)'
_computing_publication_material  CIFTAB
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXTL V.5 (Siemens, 1994)'
_diffrn_ambient_temperature      213(2)
_diffrn_measurement_device       'Nonius FAST area detector'
_diffrn_measurement_method       'Ellipsoid-mask fitting'
_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  0.1093
_diffrn_reflns_av_sigmaI/netI    0.0618
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            34289
_diffrn_reflns_theta_max         22.23
_diffrn_reflns_theta_min         1.63
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    6.944
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            blue-green
_exptl_crystal_density_diffrn    1.838
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       plate-shaped
_exptl_crystal_F_000             6192
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.577
_refine_diff_density_min         -1.175
_refine_diff_density_rms         0.196
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.148
_refine_ls_goodness_of_fit_obs   1.197
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     513
_refine_ls_number_reflns         6717
_refine_ls_number_restraints     37
_refine_ls_restrained_S_all      1.166
_refine_ls_restrained_S_obs      1.202
_refine_ls_R_factor_all          0.0925
_refine_ls_R_factor_obs          0.0678
_refine_ls_shift/esd_max         0.001
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+226.1107P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1597
_refine_ls_wR_factor_obs         0.1459
_reflns_number_observed          5442
_reflns_number_total             6717
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010504d_1.cif
_cod_data_source_block           '[n-Bu4N]4[Re2Cl7(PMe3)]2[Re2Cl8],2CH2Cl2_(3)'
_cod_depositor_comments
;
The following automatic conversions were performed:

'_chemical_melting_point' value 'not measured' was changed to '?' -
the value is undefined or not given.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 

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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+226.1107P] where P=(Fo^2^+2Fc^2^)/3'
was changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0500P)^2^+226.1107P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4320431