Mixed Chloride/Phosphine Complexes of the Dirhenium Core. 3. Novel Structures with Diethylphosphido-bridges and Terminal Diethylphosphines
F. Albert Cotton; Evgeny V. Dikarev; Marina A. Petrukhina; Inorganic Chemistry 37 (1998) 6035–6043; doi:10.1021/ic980701l

data_4323176
_publ_section_title
;
 Mixed Chloride/Phosphine Complexes of the Dirhenium Core. 3. Novel
 Structures with Diethylphosphido-bridges and Terminal Diethylphosphines
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6035
_journal_page_last               6043
_journal_paper_doi               10.1021/ic980701l
_journal_volume                  37
_journal_year                    1998
_chemical_compound_source
;
 Compound was prepared by stirring a suspension of [Bu4N]2[Re2Cl8]
 in 1-propanol with an excess of PEt2H in the presence of HCl for
 1 hour at room temperature. Single crystals were obtained by slow
 diffusion of isomeric hexanes into toluene solution.
;
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety
;
 Re2 (P (C2 H5)2)2 Cl4 (P (C2 H5)2 H)4
;
_chemical_formula_structural     1,2,5,6-Re2(\m-PEt2)2Cl4(PEt2H)4
_chemical_formula_sum            'C24 H64 Cl4 P6 Re2'
_chemical_formula_weight         1052.77
_chemical_melting_point          ?
_chemical_name_common
;
 Bis(\m2-diethylphosphido)-tetrachloro-tetrakis(diethylphosphine)-
 di-rhenium (III)
;
_chemical_name_systematic
; 
 Bis((\m2-diethylphosphido)-dichloro-bis(diethylphosphine))-
 di-rhenium (III)
;
_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                 100.98(3)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   16.094(3)
_cell_length_b                   15.193(3)
_cell_length_c                   15.548(3)
_cell_measurement_reflns_used    250
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      8.5
_cell_volume                     3732.1(13)
_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  0.0631
_diffrn_reflns_av_sigmaI/netI    0.0397
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            17000
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.14
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    7.040
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.874
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       needle-shaped
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.915
_refine_diff_density_min         -1.749
_refine_diff_density_rms         0.171
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.085
_refine_ls_goodness_of_fit_obs   1.118
_refine_ls_hydrogen_treatment    'refined on P atoms'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     337
_refine_ls_number_reflns         4788
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.106
_refine_ls_restrained_S_obs      1.118
_refine_ls_R_factor_all          0.0467
_refine_ls_R_factor_obs          0.0369
_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^)+(0.0265P)^2^+33.6843P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0899
_refine_ls_wR_factor_obs         0.0827
_reflns_number_observed          4100
_reflns_number_total             4879
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980701l_5.cif
_cod_data_source_block           Re2(\m-PEt2)2Cl4(PEt2H)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^)+(0.0265P)^2^+33.6843P] 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^)+(0.0265P)^2^+33.6843P] 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        3732(1)
_cod_database_code               4323176