Rhenium(V) Oxo Complexes with N-Heterocyclic Carbenes
Theresa I. Kückmann; Ulrich Abram; Inorganic Chemistry 43 (2004) 7068–7074; doi:10.1021/ic0497578

data_4311960
_publ_section_title
;
 Rhenium(V) Oxo Complexes with N-Heterocyclic Carbenes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              7068
_journal_page_last               7074
_journal_paper_doi               10.1021/ic0497578
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         '[ReOCl(Etcarbene)4][PF6]x 2KPF6'
_chemical_formula_sum            'C36 H64 Cl F24 K2 N8 O P4 Re'
_chemical_formula_weight         1504.68
_chemical_name_systematic
;
Chlorotetrakis(3,4-dimethyl-2,5-diethylimidazolylidene)oxorhenium(V)-
bis(hexafluorophosphate) x 2 KPF6
;
_space_group_IT_number           79
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'I 4'
_symmetry_space_group_name_H-M   'I 4'
_atom_sites_solution_hydrogens   geom
_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            2
_cell_length_a                   17.098(2)
_cell_length_b                   17.098(2)
_cell_length_c                   9.673(2)
_cell_measurement_temperature    193(2)
_cell_volume                     2827.8(7)
_computing_cell_refinement       SMART
_computing_data_collection       SMART
_computing_data_reduction        SAINT
_computing_molecular_graphics    ORTEP
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      193(2)
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker SMART'
_diffrn_measurement_method       'omega and phi 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  0.0804
_diffrn_reflns_av_sigmaI/netI    0.0749
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -22
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            17381
_diffrn_reflns_theta_full        30.72
_diffrn_reflns_theta_max         30.72
_diffrn_reflns_theta_min         1.68
_diffrn_standards_decay_%        0
_exptl_absorpt_coefficient_mu    2.574
_exptl_absorpt_correction_T_max  .923
_exptl_absorpt_correction_T_min  .885
_exptl_absorpt_correction_type   SADABS
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.767
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1500
_exptl_crystal_size_max          .5
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .1
_refine_diff_density_max         1.104
_refine_diff_density_min         -0.860
_refine_diff_density_rms         0.116
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.001(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     180
_refine_ls_number_reflns         4303
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.0629
_refine_ls_R_factor_gt           0.0491
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0582P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0978
_refine_ls_wR_factor_ref         0.1053
_reflns_number_gt                3643
_reflns_number_total             4303
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0497578rom20040224_091421_2.cif
_cod_data_source_block           reocletcarb
_cod_database_code               4311960