Rhenium Complexes with Weakly Coordinating Solvent Ligands, cis-[Re(PR3)(CO)4(L)][BArF], L = CH2Cl2, Et2O, NC5F5: Decomposition to Chloride-Bridged Dimers in CH2Cl2 Solution
Jean Huhmann-Vincent; Brian L. Scott; Gregory J. Kubas; Inorganic Chemistry 38 (1999) 115–124; doi:10.1021/ic980912q

data_4321723
_publ_section_title
;
 Rhenium Complexes with Weakly Coordinating Solvent Ligands,
 cis-[Re(PR3)(CO)4(L)][BArF], L = CH2Cl2, Et2O, NC5F5: Decomposition to
 Chloride-Bridged Dimers in CH2Cl2 Solution
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              115
_journal_page_last               124
_journal_paper_doi               10.1021/ic980912q
_journal_volume                  38
_journal_year                    1999
_chemical_formula_sum            'C46 H35 B Cl2 F24 O4 P Re'
_chemical_formula_weight         1406.62
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 97.325(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.4222(5)
_cell_length_b                   16.7303(8)
_cell_length_c                   27.772(1)
_cell_measurement_reflns_used    185
_cell_measurement_temperature    203
_cell_volume                     5263.8(4)
_computing_cell_refinement       'SMART 4.210 (Bruker)'
_computing_data_collection       'SMART 4.210 (Bruker)'
_computing_data_reduction        'SMART 4.210 (Bruker)'
_computing_molecular_graphics    'SHELXTL PC 5.03 (Siemens)'
_computing_publication_material  'SHELXTL PC 5.03 (Siemens)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193
_diffrn_measurement_device       'Siemens P4/CCD/PC'
_diffrn_measurement_method       '\w and \f scans'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0417
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10403
_diffrn_reflns_theta_max         26.43
_diffrn_reflns_theta_min         1.42
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.568
_exptl_absorpt_correction_T_max  0.90
_exptl_absorpt_correction_T_min  0.72
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.775
_exptl_crystal_density_method    'not measured '
_exptl_crystal_description       'hexagonal needle'
_exptl_crystal_F_000             2752
_exptl_crystal_size_max          0.37
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.08
_refine_diff_density_max         1.967
_refine_diff_density_min         -1.095
_refine_diff_density_rms         0.103
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.268
_refine_ls_goodness_of_fit_obs   1.350
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     731
_refine_ls_number_reflns         10403
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.268
_refine_ls_restrained_S_obs      1.350
_refine_ls_R_factor_all          0.0619
_refine_ls_R_factor_obs          0.0441
_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^)+(0.0575P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1174
_refine_ls_wR_factor_obs         0.1105
_reflns_number_observed          8273
_reflns_number_total             10403
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980912q_1.cif
_cod_data_source_block           ccd27
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0575P)^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^)+(0.0575P)^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_original_cell_volume        5263.7(4)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_database_code               4321723