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_4322143
_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         'Re2 Cl5 (P (C3 H7)3)3'
_chemical_formula_structural     1,3,6-Re2Cl5(Pn-Pr3)3
_chemical_formula_sum            'C27 H63 Cl5 P3 Re2'
_chemical_formula_weight         1030.33
_chemical_melting_point          ?
_chemical_name_systematic
; 
 Pentachloro-tris(tripropylphosphine)-di-rhenium (II,III),
 1,3,6-isomer
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   12.214(2)
_cell_length_b                   15.296(2)
_cell_length_c                   20.945(6)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      20.38
_cell_measurement_theta_min      13.97
_cell_volume                     3913.1(14)
_computing_cell_refinement       'CAD4 EXPRESS'
_computing_data_collection       'CAD4 V.5 (Enraf-Nonius, 1989)'
_computing_data_reduction        'XCAD4 (Harms, 1993)'
_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      153(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0540
_diffrn_reflns_av_sigmaI/netI    0.0606
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            5685
_diffrn_reflns_theta_max         22.49
_diffrn_reflns_theta_min         2.13
_diffrn_standards_decay_%        12.3
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  120
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.662
_exptl_absorpt_correction_T_max  0.9970
_exptl_absorpt_correction_T_min  0.6429
_exptl_absorpt_correction_type   'empirical, via \y-scans'
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    1.749
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             2020
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.28
_refine_diff_density_max         1.653
_refine_diff_density_min         -1.359
_refine_diff_density_rms         0.170
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.01(2)
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.091
_refine_ls_goodness_of_fit_obs   1.086
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     363
_refine_ls_number_reflns         5033
_refine_ls_number_restraints     4
_refine_ls_restrained_S_all      1.091
_refine_ls_restrained_S_obs      1.087
_refine_ls_R_factor_all          0.0661
_refine_ls_R_factor_obs          0.0526
_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^)+(0.0454P)^2^+61.0188P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1313
_refine_ls_wR_factor_obs         0.1231
_reflns_number_observed          4494
_reflns_number_total             5033
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic990114f_5.cif
_cod_data_source_block           1,3,6-Re2Cl5(Pn-Pr3)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 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^)+(0.0454P)^2^+61.0188P] 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^)+(0.0454P)^2^+61.0188P] 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        3913(1)
_cod_database_code               4322143