Mixed Chloride/Phosphine Complexes of the Dirhenium Core. 6. Rare or Unprecedented Isomers of [Re2Cl6(PR3)2] Stoichiometry
F. Albert Cotton; Evgeny V. Dikarev; Marina A. Petrukhina; Inorganic Chemistry 38 (1999) 3889–3894; doi:10.1021/ic9906095

data_4322221
_publ_section_title
;
 Mixed Chloride/Phosphine Complexes of the Dirhenium Core. 6. Rare or
 Unprecedented Isomers of [Re2Cl6(PR3)2] Stoichiometry
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              3889
_journal_page_last               3894
_journal_paper_doi               10.1021/ic9906095
_journal_volume                  38
_journal_year                    1999
_chemical_compound_source        synthesized
_chemical_formula_analytical     'not measured'
_chemical_formula_moiety
;
 [N (C4 H9)4](+) [Re2 Cl6 (P (C3 H7)3)2](-)
;
_chemical_formula_structural     '[n-Bu4N][1,7-Re2Cl6(Pn-Pr3)2]'
_chemical_formula_sum            'C34 H78 Cl6 N P2 Re2'
_chemical_formula_weight         1148.01
_chemical_melting_point          ?
_chemical_name_systematic
; 
 Hexachloro-bis(tripropylphosphine)-di-rhenium (II, III),
 1,7-isomer, tetrabutylammonium salt
;
_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                 104.22(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.758(1)
_cell_length_b                   15.755(5)
_cell_length_c                   24.160(3)
_cell_measurement_reflns_used    249
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.8
_cell_measurement_theta_min      9.05
_cell_volume                     4707.4(17)
_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  0.0617
_diffrn_reflns_av_sigmaI/netI    0.0395
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21494
_diffrn_reflns_theta_max         22.74
_diffrn_reflns_theta_min         2.42
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    5.570
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.620
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       needle-shaped
_exptl_crystal_F_000             2284
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.380
_refine_diff_density_min         -0.921
_refine_diff_density_rms         0.131
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.122
_refine_ls_goodness_of_fit_obs   1.121
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     412
_refine_ls_number_reflns         6225
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.132
_refine_ls_restrained_S_obs      1.131
_refine_ls_R_factor_all          0.0407
_refine_ls_R_factor_obs          0.0341
_refine_ls_shift/esd_max         -0.003
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0172P)^2^+30.8875P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0803
_refine_ls_wR_factor_obs         0.0753
_reflns_number_observed          5542
_reflns_number_total             6225
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic9906095_2.cif
_cod_data_source_block           '[n-Bu4N][1,7-Re2Cl6(Pn-Pr3)2]'
_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^)+(0.0172P)^2^+30.8875P] 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^)+(0.0172P)^2^+30.8875P] 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        4707(2)
_cod_database_code               4322221