Preparation and Characterization of Oxorhenium(V) Complexes with 2,2'-Biimidazole: The Strong Affinity of Coordinated Biimidazole for Chloride Ions via N-H...Cl-Hydrogen Bonding
Sébastien Fortin; André L. Beauchamp; Inorganic Chemistry 39 (2000) 4886–4893; doi:10.1021/ic000328t

data_4321459
_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@chimie.umontreal.ca
_publ_contact_author_fax         '514 343 7586'
_publ_contact_author_phone       '514 343 6446'
_publ_section_title
;
 Preparation and Characterization of Oxorhenium(V) Complexes with
 2,2'-Biimidazole: The Strong Affinity of Coordinated Biimidazole for
 Chloride Ions via N-H...Cl-Hydrogen Bonding
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4886
_journal_page_last               4893
_journal_paper_doi               10.1021/ic000328t
_journal_volume                  39
_journal_year                    2000
_chemical_compound_source        'synthesized by the authors, see text'
_chemical_formula_moiety         'C30 H28 Cl3 N4 O2.50 P Re'
_chemical_formula_sum            'C30 H28 Cl3 N4 O2.5 P Re'
_chemical_formula_weight         808.094
_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           'SHELXL96 (Sheldrick, 1996)'
_cell_angle_alpha                86.22(2)
_cell_angle_beta                 83.63(2)
_cell_angle_gamma                71.64(2)
_cell_formula_units_Z            2
_cell_length_a                   10.323(3)
_cell_length_b                   11.794(3)
_cell_length_c                   13.548(4)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      23
_cell_measurement_theta_min      20
_cell_volume                     1555.0(8)
_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 SHELXL96 (Sheldrick (1996))'
_computing_structure_refinement
'NRCVAX (Gabe et al, 1989) and SHELXL96 (Sheldrick, 1996)'
_computing_structure_solution    'SHELXS96 (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  0.328
_diffrn_reflns_av_sigmaI/netI    0.0687
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            18818
_diffrn_reflns_theta_max         69.86
_diffrn_reflns_theta_min         3.28
_diffrn_standards_decay_%        19.8
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    10.57
_exptl_absorpt_correction_T_max  0.2922
_exptl_absorpt_correction_T_min  0.1021
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'ABSORP in NRCVAX (Gabe et al, 1989)'
_exptl_crystal_colour            'intense blue'
_exptl_crystal_density_diffrn    1.726
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    none
_exptl_crystal_description       block
_exptl_crystal_F_000             794.0
_exptl_crystal_size_max          0.41
_exptl_crystal_size_mid          0.22
_exptl_crystal_size_min          0.20
_refine_diff_density_max         3.279
_refine_diff_density_min         -2.860
_refine_diff_density_rms         0.218
_refine_ls_extinction_coef       0.0021(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL96 (Sheldrick, 1996)'
_refine_ls_goodness_of_fit_all   1.044
_refine_ls_goodness_of_fit_ref   1.080
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     377
_refine_ls_number_reflns         5904
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.044
_refine_ls_restrained_S_obs      1.080
_refine_ls_R_factor_all          0.0585
_refine_ls_R_factor_gt           0.0554
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details     w=1/[\s^2^(Fo^2^)+(0.1131P)^2^]
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1573
_refine_ls_wR_factor_ref         0.1547
_reflns_number_gt                5363
_reflns_number_total             5904
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic000328t_3.cif
_cod_data_source_block           compound_4
_cod_depositor_comments
;
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        'C30 H28 Cl3 N4 O2.50 P Re'
_cod_database_code               4321459