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_4322751
_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 stirring a suspension of [Bu4N]2[Re2Cl8]
 in acetonitrile with an excess of PMe2Ph for 1 hour at room
 temperature. Single crystals were obtained by slow diffusion
 of isomeric hexanes into acetone/dichloromethane solution.
;
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         'Re2 Cl5 (P ((C H3)2 C 6 H5))3'
_chemical_formula_structural     1,3,6-Re2Cl5(PMe2Ph)3
_chemical_formula_sum            'C24 H33 Cl5 P3 Re2'
_chemical_formula_weight         964.06
_chemical_melting_point          ?
_chemical_name_common
;
 Pentachloro-tris(dimethylphenylphosphine)-di-rhenium,
 1,3,6-isomer
;
_chemical_name_systematic
; 
 Pentachloro-tris(dimethylphenylphosphine)-di-rhenium
;
_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                 97.84(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.202(4)
_cell_length_b                   14.357(6)
_cell_length_c                   19.509(5)
_cell_measurement_reflns_used    247
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.80
_cell_measurement_theta_min      9.05
_cell_volume                     3108.2(19)
_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  0.0474
_diffrn_reflns_av_sigmaI/netI    0.0396
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            12809
_diffrn_reflns_theta_max         22.55
_diffrn_reflns_theta_min         2.32
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    8.380
_exptl_absorpt_correction_T_max  0.512
_exptl_absorpt_correction_T_min  0.192
_exptl_absorpt_correction_type   'SORTAV (Blessing, 1995)'
_exptl_crystal_colour            dark-green
_exptl_crystal_density_diffrn    2.060
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             1828
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         8.543
_refine_diff_density_min         -2.782
_refine_diff_density_rms         0.249
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.044
_refine_ls_goodness_of_fit_obs   1.059
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     307
_refine_ls_number_reflns         4057
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_restrained_S_obs      1.059
_refine_ls_R_factor_all          0.0650
_refine_ls_R_factor_obs          0.0566
_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^)+(0.0687P)^2^+96.2552P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1525
_refine_ls_wR_factor_obs         0.1427
_reflns_number_observed          3490
_reflns_number_total             4057
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic971522r_2.cif
_cod_data_source_block           1,3,6-Re2Cl5(PMe2Ph)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^)+(0.0687P)^2^+96.2552P] 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^)+(0.0687P)^2^+96.2552P] 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        3108(2)
_cod_database_code               4322751