Mixed Chloride Phosphine Complexes of Dirhenium Cores. 1. New Reactions and Unprecedented Structures Involving Trimethylphosphine
F. Albert Cotton; Evgeny V. Dikarev; Marina A. Petrukhina; Journal of the American Chemical Society 119 (1997) 12541–12549; doi:10.1021/ja9733245

data_4117096
_publ_section_title
;
 Mixed Chloride Phosphine Complexes of Dirhenium Cores. 1. New Reactions
 and Unprecedented Structures Involving Trimethylphosphine
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              12541
_journal_page_last               12549
_journal_paper_doi               10.1021/ja9733245
_journal_volume                  119
_journal_year                    1997
_chemical_compound_source
;
 Compound was prepared by stirring a suspension of [Bu4N]2[Re2Cl8]
 in benzene with an excess of PMe3 for 6 hours at room temperature.
 Single crystals were obtained by slow diffusion of isomeric
 hexanes into dichloromethane solution.
;
_chemical_formula_moiety         'Re2 Cl6 (P (C H3)3)4'
_chemical_formula_structural     1,3,5,7-Re2(\m-Cl)2Cl4(PMe3)4
_chemical_formula_sum            'C12 H36 Cl6 P4 Re2'
_chemical_formula_weight         889.39
_chemical_name_common
;
 Bis(\m2-chloro)-tetrachloro-tetrakis(trimethylphosphine)-
 -di-rhenium (III)
;
_chemical_name_systematic
; 
 Bis((\m2-chloro)-bis(dichloro-bis(trimethylphosphine))-di-
 rhenium (III)
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   15.627(2)
_cell_length_b                   10.872(1)
_cell_length_c                   16.462(2)
_cell_measurement_reflns_used    249
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      20.80
_cell_measurement_theta_min      9.05
_cell_volume                     2796.8(6)
_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  'SHELXL-93 (Sheldrick, 1993)'
_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  0.0675
_diffrn_reflns_av_sigmaI/netI    0.0297
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15635
_diffrn_reflns_theta_max         25.15
_diffrn_reflns_theta_min         2.47
_diffrn_standards_number         'none (area detector data)'
_exptl_absorpt_coefficient_mu    9.449
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    2.112
_exptl_crystal_density_method    none
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             1680
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.085
_refine_diff_density_min         -0.928
_refine_diff_density_rms         0.162
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.160
_refine_ls_goodness_of_fit_obs   1.159
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         2489
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.363
_refine_ls_restrained_S_obs      1.159
_refine_ls_R_factor_all          0.0311
_refine_ls_R_factor_obs          0.0256
_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^)+(0.0215P)^2^+12.4181P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0728
_refine_ls_wR_factor_obs         0.0591
_reflns_number_observed          2282
_reflns_number_total             2492
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9733245_1.cif
_cod_data_source_block           1,3,5,7-Re2Cl6(PMe3)4(4)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0215P)^2^+12.4181P] 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^)+(0.0215P)^2^+12.4181P] 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               4117096