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_4321724
_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            'C50 H33 B F29 N O4 P Re'
_chemical_formula_weight         1490.75
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                94.5550(10)
_cell_angle_beta                 109.2490(10)
_cell_angle_gamma                100.4580(10)
_cell_formula_units_Z            2
_cell_length_a                   14.1056(8)
_cell_length_b                   14.2860(8)
_cell_length_c                   14.7448(7)
_cell_measurement_reflns_used    75
_cell_measurement_temperature    193
_cell_volume                     2727.3(3)
_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 (Bruker)'
_computing_publication_material  'SHELXTL PC 5.03 (Bruker)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      193
_diffrn_measurement_device       'Bruker 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    0.0537
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            10302
_diffrn_reflns_theta_max         26.48
_diffrn_reflns_theta_min         1.47
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.402
_exptl_absorpt_correction_T_max  0.92
_exptl_absorpt_correction_T_min  0.80
_exptl_absorpt_correction_type   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'irregular slab'
_exptl_crystal_density_diffrn    1.815
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       colorless
_exptl_crystal_F_000             1456
_exptl_crystal_size_max          0.21
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.808
_refine_diff_density_min         -1.040
_refine_diff_density_rms         0.118
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.114
_refine_ls_goodness_of_fit_obs   1.132
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     784
_refine_ls_number_reflns         10302
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.114
_refine_ls_restrained_S_obs      1.132
_refine_ls_R_factor_all          0.0596
_refine_ls_R_factor_obs          0.0476
_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^)+(0.0759P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1276
_refine_ls_wR_factor_obs         0.1199
_reflns_number_observed          8899
_reflns_number_total             10302
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic980912q_2.cif
_cod_data_source_block           ccd31
_cod_depositor_comments
;
The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0759P)^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^)+(0.0759P)^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 
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_cod_database_code               4321724