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_4322752
_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 cobaltocene in dichloromethane at
 room temperature followed by the addition of PMe2Ph to the
 reaction mixture. Single crystals were obtained by slow
 diffusion of isomeric hexanes into dichloromethane solution.
;
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         'Re2 Cl4 (P ((C H3)2 C6 H5))4'
_chemical_formula_structural     1,2,7,8-Re2Cl4(PMe2Ph)4
_chemical_formula_sum            'C32 H44 Cl4 P4 Re2'
_chemical_formula_weight         1066.75
_chemical_melting_point          ?
_chemical_name_common
;
 Tetrachloro-tetrakis(dimethylphenylphosphine)-di-rhenium (II)
;
_chemical_name_systematic
; 
 Bis(dichloro-bis(dimethylphenylphosphine))-di-rhenium (II)
;
_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                76.111(8)
_cell_angle_beta                 88.523(9)
_cell_angle_gamma                88.95(2)
_cell_formula_units_Z            2
_cell_length_a                   11.847(4)
_cell_length_b                   12.094(3)
_cell_length_c                   13.056(5)
_cell_measurement_reflns_used    216
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      6.85
_cell_volume                     1815.2(10)
_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  0.0755
_diffrn_reflns_av_sigmaI/netI    0.0541
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8886
_diffrn_reflns_theta_max         22.57
_diffrn_reflns_theta_min         2.33
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    7.156
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.952
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             1028
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         2.827
_refine_diff_density_min         -1.119
_refine_diff_density_rms         0.239
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.121
_refine_ls_goodness_of_fit_obs   1.127
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     379
_refine_ls_number_reflns         4468
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.151
_refine_ls_restrained_S_obs      1.127
_refine_ls_R_factor_all          0.0553
_refine_ls_R_factor_obs          0.0468
_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^)+(0.0436P)^2^+42.0701P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1278
_refine_ls_wR_factor_obs         0.1168
_reflns_number_observed          3943
_reflns_number_total             4476
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971522r_3.cif
_cod_data_source_block           1,2,7,8-Re2Cl4(PMe2Ph)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 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^)+(0.0436P)^2^+42.0701P] 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^)+(0.0436P)^2^+42.0701P] 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        1815(1)
_cod_database_code               4322752