Preparations, Characterizations, and Structures of (Biimidazole)dihalobis(triphenylphosphine)rhenium(III) Salts: Strong Ion-Pairing and Acid-Base Properties
Sébastien Fortin; André L. Beauchamp; Inorganic Chemistry 40 (2001) 105–112; doi:10.1021/ic0006807

data_4319123
_publ_contact_author
;
    Dr. Andr\'e L. Beauchamp
    D\'epartement de Chimie
    Universit\'e de Montr\'eal
    C.P. 6128, Succ. Centre-ville
    Montr\'eal, Qu\'ebec
    Canada H3C 3J7
;
_publ_contact_author_email       beauchmp@ere.umontreal.ca
_publ_contact_author_fax         '514 343 7586'
_publ_contact_author_phone       '514 343 6446'
_publ_section_title
;
 Preparations, Characterizations, and Structures of
 (Biimidazole)dihalobis(triphenylphosphine)rhenium(III) Salts: Strong
 Ion-Pairing and Acid-Base Properties
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              105
_journal_page_last               112
_journal_paper_doi               10.1021/ic0006807
_journal_volume                  40
_journal_year                    2001
_chemical_compound_source        'synthesized by the authors, see text'
_chemical_formula_moiety         'C49.50 H42 Cl3 N4 O2 P2 Re'
_chemical_formula_sum            'C49.5 H42 Cl3 N4 O2 P2 Re'
_chemical_formula_weight         1079.353
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           29
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2c -2ac'
_symmetry_space_group_name_H-M   'P c a 21'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           'SHELXL93 (Sheldrick, 1993)'
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   32.4702(2)
_cell_length_b                   9.45300(10)
_cell_length_c                   30.3331(2)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      20.00
_cell_volume                     9310.47(13)
_computing_cell_refinement       'SAINT (Siemens, 1996)'
_computing_data_collection       'SMART (Siemens, 1996)'
_computing_data_reduction        'SAINT (Siemens, 1996)'
_computing_molecular_graphics
'ORTEPII (Johnson, 1976) in NRCVAX (Gabe et al, 1989)'
_computing_publication_material
'NRCVAX (Gabe et al, 1989) and SHELXL93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Bruker AXS SMART 2K/Platform'
_diffrn_measurement_method       '\w scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus xray tube'
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0953
_diffrn_reflns_av_sigmaI/netI    0.0926
_diffrn_reflns_limit_h_max       40
_diffrn_reflns_limit_h_min       -40
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            74231
_diffrn_reflns_theta_max         72.92
_diffrn_reflns_theta_min         2.72
_diffrn_standards_decay_%        1.0
_diffrn_standards_number         ****
_exptl_absorpt_coefficient_mu    7.551
_exptl_absorpt_correction_T_max  0.204
_exptl_absorpt_correction_T_min  0.067
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS (Sheldrick, 1996)'
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.540
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             4312.0
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.41
_exptl_crystal_size_min          0.21
_refine_diff_density_max         3.697
_refine_diff_density_min         -1.614
_refine_diff_density_rms         0.240
_refine_ls_abs_structure_details 'Flack (1983)'
_refine_ls_abs_structure_Flack   0.657(17)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.008
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     969
_refine_ls_number_reflns         18156
_refine_ls_number_restraints     257
_refine_ls_restrained_S_all      1.008
_refine_ls_restrained_S_obs      1.135
_refine_ls_R_factor_all          0.1086
_refine_ls_R_factor_gt           0.0823
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1225P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.2085
_refine_ls_wR_factor_ref         0.1954
_reflns_number_gt                12858
_reflns_number_total             18153
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic0006807_1.cif
_cod_data_source_block           COMPOUND_4
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Orthorhombic' changed to
'orthorhombic' according to the built-in table from CIF Core
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z 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 
;
_cod_original_formula_sum        'C49.50 H42 Cl3 N4 O2 P2 Re'
_cod_database_code               4319123