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_4323173
_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
;
 [Bu4N]2[Re2Cl8] was suspended in a mixture of 1-propanol with an
 excess of PEt2H. The reaction mixture was stirred at room temperature
 for 12 hours, resulting in a red-brown solution. The solvent and the
 excess of phosphine were then removed by vacuum distillation to leave
 an oily brown residue. This was dissolved in dichloromethane and
 heated up for 24 hours. Single crystals were obtained by slow
 diffusion of isomeric hexanes into dichloromethane solution.
;
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety         '[(C4 H9)4 N][Re2 (P (C2 H5)2)3 Cl6]'
_chemical_formula_structural     '[(n-Bu)4N][Re2(\m-PEt2)3Cl6]'
_chemical_formula_sum            'C28 H66 Cl6 N P3 Re2'
_chemical_formula_weight         1094.83
_chemical_melting_point          ?
_chemical_name_common
;
 Tetra-n-butylammonium-tris(\m2-diethylphosphido)-hexachloro-
 di-rhenium (IV)
;
_chemical_name_systematic
; 
 Tetra-n-butylammonium-tris(\m2-diethylphosphido)-bis(trichloro)-
 di-rhenium (IV)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 93.637(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.482(1)
_cell_length_b                   16.512(2)
_cell_length_c                   23.986(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      15.02
_cell_measurement_theta_min      11.98
_cell_volume                     4143.1(7)
_computing_cell_refinement       'CAD4 EXPRESS'
_computing_data_collection       'CAD4 V.5 (enraf-Nonius, 1989)'
_computing_data_reduction        'XCAD4 (Harms, 1993)'
_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      173(2)
_diffrn_measurement_device       'Enraf-Nonius CAD4'
_diffrn_measurement_method       \w--\q
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus sealed tube'
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0416
_diffrn_reflns_av_sigmaI/netI    0.0796
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            6114
_diffrn_reflns_theta_max         22.94
_diffrn_reflns_theta_min         2.07
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    6.361
_exptl_absorpt_correction_T_max  0.9992
_exptl_absorpt_correction_T_min  0.7250
_exptl_absorpt_correction_type   'empirical via \y scans'
_exptl_crystal_colour            brown-purple
_exptl_crystal_density_diffrn    1.755
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             2152
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.910
_refine_diff_density_min         -0.959
_refine_diff_density_rms         0.192
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.042
_refine_ls_goodness_of_fit_obs   1.057
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     371
_refine_ls_number_reflns         5751
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.042
_refine_ls_restrained_S_obs      1.057
_refine_ls_R_factor_all          0.0909
_refine_ls_R_factor_obs          0.0366
_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^)+(0.0415P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0904
_refine_ls_wR_factor_obs         0.0765
_reflns_number_observed          4103
_reflns_number_total             5751
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980701l_2.cif
_cod_data_source_block           '[n-Bu4N][Re2(\m-PEt2)3Cl6]'
_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^)+(0.0415P)^2^+0.0000P] 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^)+(0.0415P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4323173