Neutral and cationic biimidazoledihalogenobis(trimethylphosphine)rhenium(iii) complexes: ion-pairing, acid‒base and redox properties
Fortin, Sébastien; Fabre, Paul-Louis; Dartiguenave, Michèle; Beauchamp, André L.; Journal of the Chemical Society, Dalton Transactions  (2001) 3520–; doi:10.1039/b103719f

data_7010786
_publ_section_title
;
 Neutral and cationic
 biimidazoledihalogenobis(trimethylphosphine)rhenium(iii) complexes:
 ion-pairing, acid--base and redox properties
;
_journal_issue                   23
_journal_name_full
'Journal of the Chemical Society, Dalton Transactions'
_journal_page_first              3520
_journal_paper_doi               10.1039/b103719f
_journal_year                    2001
_chemical_compound_source        'synthesized by the authors, see text'
_chemical_formula_moiety         'C16.4 H35 Br3 N4 O1.1 P2 Re'
_chemical_formula_sum            'C16.4 H35 Br3 N4 O1.1 P2 Re'
_chemical_formula_weight         793.75
_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           'SHELXL93 (Sheldrick, 1993)'
_cell_angle_alpha                82.36(5)
_cell_angle_beta                 69.27(6)
_cell_angle_gamma                68.09(6)
_cell_formula_units_Z            4
_cell_length_a                   12.952(10)
_cell_length_b                   15.892(9)
_cell_length_c                   15.898(10)
_cell_measurement_reflns_used    23
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      21.00
_cell_measurement_theta_min      20.00
_cell_volume                     2839(4)
_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     1.54178
_diffrn_reflns_av_R_equivalents  0.017
_diffrn_reflns_av_sigmaI/netI    0.0318
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            5748
_diffrn_reflns_theta_max         49.91
_diffrn_reflns_theta_min         2.97
_diffrn_standards_decay_%        'no decay, variation  1.0'
_diffrn_standards_interval_time  60
_diffrn_standards_number         5
_exptl_absorpt_coefficient_mu    14.28
_exptl_absorpt_correction_T_max  0.13
_exptl_absorpt_correction_T_min  0.05
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'ABSORP in NRCVAX (Gabe et al, 1989)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.857
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    .
_exptl_crystal_description       block
_exptl_crystal_F_000             1520.8
_exptl_crystal_size_max          0.53
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.14
_refine_diff_density_max         0.899
_refine_diff_density_min         -0.655
_refine_diff_density_rms         0.093
_refine_ls_extinction_coef       0.00020(2)
_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   1.062
_refine_ls_goodness_of_fit_ref   1.139
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     400
_refine_ls_number_reflns         5444
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.062
_refine_ls_restrained_S_obs      1.139
_refine_ls_R_factor_all          0.0489
_refine_ls_R_factor_gt           0.0388
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0648P)^2^+0.5482P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.1089
_refine_ls_wR_factor_ref         0.1042
_reflns_number_gt                4406
_reflns_number_total             5444
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            b103719f.txt
_cod_data_source_block           compound_5
_cod_depositor_comments
;
 Replacing data item names '_geom_hbond_atom_site_label_1' and
 '_geom_hbond_site_symmetry_1' with '_geom_hbond_atom_site_label_A' and
 '_geom_hbond_site_symmetry_1' accordingly.

 Antanas Vaitkus,
 2017-03-03

The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2839(3)
_cod_database_code               7010786