Ligand-Promoted Solvent-Dependent Ionization and Conformational Equilibria of Re(CO)3Br[CH2(S-tim)2] (tim = 1-methylthioimidazolyl). Crystal Structures of Re(CO)3Br[CH2(S-tim)2] and {Re(CO)3(CH3CN)[CH2(S-tim)2]}(PF6)
Silva, Rosalice M.; Liddle, Brendan J.; Lindeman, Sergey J.; Smith, Mark D.; Gardinier, James R.; Inorganic Chemistry 45 (2006) 6794–6802; doi:10.1021/ic060765t

data_4332736
_publ_section_title
;
 Ligand-Promoted Solvent-Dependent Ionization and Conformational
 Equilibria of Re(CO)3Br[CH2(S-tim)2] (tim = 1-methylthioimidazolyl).
 Crystal Structures of Re(CO)3Br[CH2(S-tim)2] and
 {Re(CO)3(CH3CN)[CH2(S-tim)2]}(PF6)
;
_journal_issue                   17
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6794
_journal_page_last               6802
_journal_paper_doi               10.1021/ic060765t
_journal_volume                  45
_journal_year                    2006
_chemical_formula_sum            'C14 H15 F6 N5 O3 P Re S2'
_chemical_formula_weight         696.60
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           61
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  '-P 2ac 2ab'
_symmetry_space_group_name_H-M   'P b c a'
_atom_sites_solution_hydrogens   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   13.635(2)
_cell_length_b                   13.746(2)
_cell_length_c                   23.788(4)
_cell_measurement_reflns_used    7660
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      31
_cell_measurement_theta_min      3
_cell_volume                     4458.5(12)
_computing_cell_refinement       'SAINT v7.23A (Bruker, 2005)'
_computing_data_collection       'APEX2 v2.0-2 (Bruker, 2005)'
_computing_data_reduction        'SADABS-2004/1 (Bruker, 2005)'
_computing_molecular_graphics    'XP v5.1 (Bruker, 1998)'
_computing_publication_material  'XCIF v6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 v.97-2 (Sheldrick, 1993-1997)'
_computing_structure_solution    'XS/SHELXTL v6.12 (Bruker, 2001)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'Bruker APEX2 CCD detector'
_diffrn_measurement_method       '\w 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  0.0294
_diffrn_reflns_av_sigmaI/netI    0.0155
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            71693
_diffrn_reflns_theta_full        31.95
_diffrn_reflns_theta_max         31.95
_diffrn_reflns_theta_min         1.71
_exptl_absorpt_coefficient_mu    5.786
_exptl_absorpt_correction_T_max  0.7228
_exptl_absorpt_correction_T_min  0.2589
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    2.076
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             2672
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.27
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.187
_refine_diff_density_min         -0.678
_refine_diff_density_rms         0.101
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     349
_refine_ls_number_reflns         7448
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.033
_refine_ls_R_factor_all          0.0225
_refine_ls_R_factor_gt           0.0184
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0246P)^2^+2.9490P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0440
_refine_ls_wR_factor_ref         0.0453
_reflns_number_gt                6571
_reflns_number_total             7448
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic060765tsup1.cif
_cod_data_source_block           compound2
_cod_original_cell_volume        4458.6(12)
_cod_original_sg_symbol_H-M      'P bca'
_cod_database_code               4332736