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_4319125
_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         'C42 H38 Br3 N4 O P2 Re'
_chemical_formula_sum            'C42 H38 Br3 N4 O P2 Re'
_chemical_formula_weight         1102.644
_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           'SHELXL93 (Sheldrick, 1993)'
_cell_angle_alpha                90.00
_cell_angle_beta                 104.28(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   9.3423(18)
_cell_length_b                   35.955(16)
_cell_length_c                   12.825(5)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.00
_cell_measurement_theta_min      20.00
_cell_volume                     4175(3)
_computing_cell_refinement       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_collection       'CAD-4 software (Enraf-Nonius, 1989)'
_computing_data_reduction        'NRC-2, NRC-2A (Ahmed et al, 1973)'
_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
'NRCVAX (Gabe et al, 1989) and SHELXL93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device_type  'Nonius CAD-4'
_diffrn_measurement_method       '\w/2\q scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'normal-focus xray tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54056
_diffrn_reflns_av_R_equivalents  0.000
_diffrn_reflns_av_sigmaI/netI    0.0841
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       43
_diffrn_reflns_limit_k_min       -43
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            69460
_diffrn_reflns_theta_max         69.91
_diffrn_reflns_theta_min         2.46
_diffrn_standards_decay_%        'no decay, variation  1.0'
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    9.920
_exptl_absorpt_correction_T_max  0.475
_exptl_absorpt_correction_T_min  0.126
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'clear intense red-orange'
_exptl_crystal_density_diffrn    1.7543
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       needle
_exptl_crystal_F_000             2144.0
_exptl_crystal_size_max          0.87
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.499
_refine_diff_density_min         -1.345
_refine_diff_density_rms         0.122
_refine_ls_extinction_coef       0.000091(10)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL93 (Sheldrick, 1993)'
_refine_ls_goodness_of_fit_all   0.857
_refine_ls_goodness_of_fit_ref   0.999
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         7931
_refine_ls_number_restraints     6
_refine_ls_restrained_S_all      0.863
_refine_ls_restrained_S_obs      1.009
_refine_ls_R_factor_all          0.0595
_refine_ls_R_factor_gt           0.0398
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0393P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1009
_refine_ls_wR_factor_ref         0.0965
_reflns_number_gt                5477
_reflns_number_total             7931
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic0006807_3.cif
_cod_data_source_block           compound_2
_cod_depositor_comments
;
The following automatic conversions were performed:

'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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_sg_symbol_H-M      'P 21/c'
_cod_database_code               4319125