Mixed Chloride/Phosphine Complexes of the Dirhenium Core. 2. New Reactions Involving Dimethylphenylphosphine
F. Albert Cotton; Evgeny V. Dikarev; Marina A. Petrukhina; Inorganic Chemistry 37 (1998) 1949–1958; doi:10.1021/ic971522r

data_4322753
_publ_section_title
;
 Mixed Chloride/Phosphine Complexes of the Dirhenium Core. 2. New
 Reactions Involving Dimethylphenylphosphine
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1949
_journal_page_last               1958
_journal_paper_doi               10.1021/ic971522r
_journal_volume                  37
_journal_year                    1998
_chemical_compound_source
;
 Compound was prepared by reaction of 1,2,7-isomer of
 Re2Cl5(PMe2Ph)3 with nitrosonium tetrafluoroborate in the
 presence of tetrabutylammonium chloride in dichloromethane
 solution at room temperature. Single crystals were obtained
 by slow diffusion of isomeric hexanes into dichloromethane
 solution.
;
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         'Re2 Cl6 (P ((C H3)2 C6 H5))2'
_chemical_formula_structural     1,7-Re2Cl6(PMe2Ph)2
_chemical_formula_sum            'C16 H22 Cl6 P2 Re2'
_chemical_formula_weight         861.38
_chemical_melting_point          ?
_chemical_name_common
;
 Hexachloro-bis(dimethylphenylphosphine)-di-rhenium (III)
;
_chemical_name_systematic
; 
 Bis(trichloro-dimethylphenylphosphine)-di-rhenium (III)
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                81.74(2)
_cell_angle_beta                 69.89(2)
_cell_angle_gamma                66.35(2)
_cell_formula_units_Z            2
_cell_length_a                   9.209(1)
_cell_length_b                   11.480(2)
_cell_length_c                   13.389(2)
_cell_measurement_reflns_used    221
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.85
_cell_measurement_theta_min      9.05
_cell_volume                     1217.5(4)
_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  0.0515
_diffrn_reflns_av_sigmaI/netI    0.0485
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            4753
_diffrn_reflns_theta_max         22.58
_diffrn_reflns_theta_min         2.52
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    10.724
_exptl_absorpt_correction_T_max  0.601
_exptl_absorpt_correction_T_min  0.290
_exptl_absorpt_correction_type   'SORTAV (Blessing, 1995)'
_exptl_crystal_colour            olive-green
_exptl_crystal_density_diffrn    2.350
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       plate-shaped
_exptl_crystal_F_000             800
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.05
_refine_diff_density_max         3.002
_refine_diff_density_min         -1.907
_refine_diff_density_rms         0.268
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.142
_refine_ls_goodness_of_fit_obs   1.155
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     235
_refine_ls_number_reflns         2759
_refine_ls_number_restraints     18
_refine_ls_restrained_S_all      1.141
_refine_ls_restrained_S_obs      1.152
_refine_ls_R_factor_all          0.0544
_refine_ls_R_factor_obs          0.0498
_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^)+(0.0375P)^2^+53.2628P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1315
_refine_ls_wR_factor_obs         0.1273
_reflns_number_observed          2550
_reflns_number_total             2760
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971522r_4.cif
_cod_data_source_block           1,7-Re2Cl6(PMe2Ph)2
_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^)+(0.0375P)^2^+53.2628P] 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^)+(0.0375P)^2^+53.2628P] 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        1217.6(3)
_cod_database_code               4322753