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_4117097
_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 reaction of 1,2,7-isomer of
 Re2Cl5(PMe3)3 with cobaltocene in dichloromethane at room
 temperature followed by addition of PMe3 to the reaction
 mixture. Single crystals were obtained by slow diffusion
 of isomeric hexanes into dichloromethane solution.
;
_chemical_formula_moiety         'Re2 Cl4 (P (C H3)3)4'
_chemical_formula_structural     1,2,7,8-Re2Cl4(PMe3)4
_chemical_formula_sum            'C12 H36 Cl4 P4 Re2'
_chemical_formula_weight         818.49
_chemical_name_common
;
 Tetrachloro-tetrakis(trimethylphosphine)-di-rhenium (II)
;
_chemical_name_systematic
; 
 Bis(dichloro-bis(trimethylphosphine))-di-rhenium (II) 
;
_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                 91.24(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.101(2)
_cell_length_b                   14.526(3)
_cell_length_c                   9.3519(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      15.86
_cell_measurement_theta_min      10.40
_cell_volume                     1236.0(4)
_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      293(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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0516
_diffrn_reflns_av_sigmaI/netI    0.0320
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            8470
_diffrn_reflns_theta_max         24.98
_diffrn_reflns_theta_min         2.59
_diffrn_standards_decay_%        4.4
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  60
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    10.471
_exptl_absorpt_correction_T_max  0.9974
_exptl_absorpt_correction_T_min  0.5411
_exptl_absorpt_correction_type   'empirical, via \y-scans'
_exptl_crystal_colour            green-brown
_exptl_crystal_density_diffrn    2.199
_exptl_crystal_density_method    none
_exptl_crystal_description       block-shaped
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.35
_exptl_crystal_size_mid          0.28
_exptl_crystal_size_min          0.23
_refine_diff_density_max         2.396
_refine_diff_density_min         -2.379
_refine_diff_density_rms         0.209
_refine_ls_extinction_coef       noref
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.081
_refine_ls_goodness_of_fit_obs   1.117
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     137
_refine_ls_number_reflns         2168
_refine_ls_number_restraints     30
_refine_ls_restrained_S_all      1.093
_refine_ls_restrained_S_obs      1.129
_refine_ls_R_factor_all          0.0466
_refine_ls_R_factor_obs          0.0377
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+10.1060P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1042
_refine_ls_wR_factor_obs         0.0967
_reflns_number_observed          1779
_reflns_number_total             2169
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ja9733245_2.cif
_cod_data_source_block           1,2,7,8-Re2Cl4(PMe3)4(2)
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0495P)^2^+10.1060P] 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^)+(0.0495P)^2^+10.1060P] 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               4117097