Mixed Chloride/Phosphine Complexes of the Dirhenium Core. 5. Reduction or Disproportionation at the Re26+ Unit in Reactions with Tertiary Phosphines in Different Solvents
F. Albert Cotton; Evgeny V. Dikarev; Marina A. Petrukhina; Inorganic Chemistry 38 (1999) 3384–3389; doi:10.1021/ic990114f

data_4322140
_publ_section_title
;
 Mixed Chloride/Phosphine Complexes of the Dirhenium Core. 5. Reduction or
 Disproportionation at the Re26+ Unit in Reactions with Tertiary
 Phosphines in Different Solvents
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3384
_journal_page_last               3389
_journal_paper_doi               10.1021/ic990114f
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         'Re Cl4 (P (C2 H5)3)2'
_chemical_formula_structural     trans-ReCl4(PEt3)2
_chemical_formula_sum            'C12 H30 Cl4 P2 Re'
_chemical_formula_weight         564.30
_chemical_melting_point          ?
_chemical_name_systematic
; 
 trans-Tetrachloro-bis(triethylphosphine)-rhenium (IV)
;
_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
_cell_angle_alpha                90.00
_cell_angle_beta                 99.167(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   8.0555(4)
_cell_length_b                   12.536(2)
_cell_length_c                   10.2041(6)
_cell_measurement_reflns_used    238
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      4.0
_cell_volume                     1017.29(18)
_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  0.0670
_diffrn_reflns_av_sigmaI/netI    0.0418
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_number            5847
_diffrn_reflns_theta_max         25.04
_diffrn_reflns_theta_min         2.59
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    6.643
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.842
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             550
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.090
_refine_diff_density_min         -1.517
_refine_diff_density_rms         0.159
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.119
_refine_ls_goodness_of_fit_obs   1.114
_refine_ls_hydrogen_treatment    allref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     133
_refine_ls_number_reflns         1708
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.119
_refine_ls_restrained_S_obs      1.114
_refine_ls_R_factor_all          0.0330
_refine_ls_R_factor_obs          0.0294
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0450P)^2^+1.8883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0840
_refine_ls_wR_factor_obs         0.0790
_reflns_number_observed          1538
_reflns_number_total             1708
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990114f_2.cif
_cod_data_source_block           1b
_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 1673 2011-04-08 12:14:43Z 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^)+(0.0450P)^2^+1.8883P] 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^)+(0.0450P)^2^+1.8883P] 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        1017.3(2)
_cod_database_code               4322140