Mixed Chloride/Phosphine Complexes of the Dirhenium Core. 10. Redox Reactions of an Edge-Sharing Dirhenium(III) Non-metal-Metal-Bonded Complex, Re2(μ-Cl)2Cl4(PMe3)4
F. Albert Cotton; Evgeny V. Dikarev; Marina A. Petrukhina; Inorganic Chemistry 40 (2001) 6825–6831; doi:10.1021/ic010653w

data_4320719
_publ_section_title
;
 Mixed Chloride/Phosphine Complexes of the Dirhenium Core. 10. Redox
 Reactions of an Edge-Sharing Dirhenium(III) Non-metal-Metal-Bonded
 Complex, Re2(\m-Cl)2Cl4(PMe3)4
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6825
_journal_page_last               6831
_journal_paper_doi               10.1021/ic010653w
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         '[N (C4 H9)4] [Re2 Cl5 (P (C H3)3)5]'
_chemical_formula_structural     '[n-Bu4N][1,2,7-Re2Cl5(PMe3)3]'
_chemical_formula_sum            'C25 H63 Cl5 N P3 Re2'
_chemical_formula_weight         1020.32
_chemical_melting_point          ?
_chemical_name_systematic
; 
Penta-chloro-tris-trimethylphosphine-di-rhenium(II,II), tetrabutyl- 
ammonium salt 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_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                 101.15(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.561(2)
_cell_length_b                   21.812(3)
_cell_length_c                   18.864(2)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.05
_cell_volume                     3859.7(11)
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0910
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            5068
_diffrn_reflns_theta_max         22.54
_diffrn_reflns_theta_min         2.17
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    6.753
_exptl_absorpt_correction_T_max  0.720
_exptl_absorpt_correction_T_min  0.389
_exptl_absorpt_correction_type   'SORTAV (Blessing, 1995)'
_exptl_crystal_colour            greenish-brown
_exptl_crystal_density_diffrn    1.756
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       plate-shaped
_exptl_crystal_F_000             2000
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.782
_refine_diff_density_min         -1.042
_refine_diff_density_rms         0.211
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.073
_refine_ls_goodness_of_fit_obs   1.138
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     324
_refine_ls_number_reflns         5068
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.073
_refine_ls_restrained_S_obs      1.138
_refine_ls_R_factor_all          0.0606
_refine_ls_R_factor_obs          0.0467
_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^)+(0.0566P)^2^+0.4869P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1297
_refine_ls_wR_factor_obs         0.1215
_reflns_number_observed          4012
_reflns_number_total             5068
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic010653w_3.cif
_cod_data_source_block           '[n-Bu4N][1,2,7-Re2Cl5(PMe3)3]_(4)'
_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^)+(0.0566P)^2^+0.4869P] 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^)+(0.0566P)^2^+0.4869P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        3860(1)
_cod_database_code               4320719