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_4323174
_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 solution of [Bu4N]2[Re2Cl8]
 in acetonitrile with an excess of PEt2H for 1 hour at room
 temperature. Single crystals were obtained by slow crystallization
 from toluene solution at -30 C.
;
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety
;
 [(C4 H9)4 N][Re2 (P (C2 H5)2)3 Cl6], 1.5(C7 H8)
;
_chemical_formula_structural     '[(n-Bu)4N][Re2(PEt2)3Cl6],1.5C7H8'
_chemical_formula_sum            'C38.5 H78 Cl6 N P3 Re2'
_chemical_formula_weight         1233.03
_chemical_melting_point          ?
_chemical_name_common
;
 Tetra-n-butylammonium-tris(\m2-diethylphosphido)-hexachloro-
 di-rhenium (IV), toluene solvate
;
_chemical_name_systematic
; 
 Tetra-n-butylammonium-tris(\m2-diethylphosphido)-bis(trichloro)-
 di-rhenium (IV), toluene solvate
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 110.35(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   38.746(9)
_cell_length_b                   10.322(2)
_cell_length_c                   27.277(3)
_cell_measurement_reflns_used    248
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      6.0
_cell_volume                     10228(3)
_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  0.0885
_diffrn_reflns_av_sigmaI/netI    0.0540
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -42
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            23297
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         2.05
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    5.163
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red-violet
_exptl_crystal_density_diffrn    1.601
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             4904
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.08
_refine_diff_density_max         2.013
_refine_diff_density_min         -3.286
_refine_diff_density_rms         0.194
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.086
_refine_ls_goodness_of_fit_obs   1.106
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     448
_refine_ls_number_reflns         6469
_refine_ls_number_restraints     15
_refine_ls_restrained_S_all      1.126
_refine_ls_restrained_S_obs      1.105
_refine_ls_R_factor_all          0.0654
_refine_ls_R_factor_obs          0.0522
_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^)+(0.0655P)^2^+167.5306P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1423
_refine_ls_wR_factor_obs         0.1265
_reflns_number_observed          5526
_reflns_number_total             6658
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980701l_3.cif
_cod_data_source_block           '[n-Bu4N][Re2(\m-PEt2)3Cl6],1.5C7H8'
_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^)+(0.0655P)^2^+167.5306P] 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^)+(0.0655P)^2^+167.5306P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_formula_sum        'C38.50 H78 Cl6 N P3 Re2'
_cod_database_code               4323174