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

data_4311962
_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         '[ReO2(L1)4][ReO4]'
_chemical_formula_sum            'C50 H92 N8 O7.5 Re2'
_chemical_formula_weight         1297.72
_chemical_name_common            ReO2Carben
_chemical_name_systematic
;
Tetrakis(1,3-diisopropyl-4,5-dimethylimidazole-2-yliden)dioxorheniumperrhenat 
x 1.5 THF
;
_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           SHELXL-97
_cell_angle_alpha                100.403(5)
_cell_angle_beta                 97.834(5)
_cell_angle_gamma                106.272(5)
_cell_formula_units_Z            2
_cell_length_a                   12.311(5)
_cell_length_b                   16.525(5)
_cell_length_c                   16.743(5)
_cell_measurement_reflns_used    997
_cell_measurement_temperature    173(2)
_cell_measurement_theta_max      30.311
_cell_measurement_theta_min      2.7755
_cell_volume                     3152.4(19)
_computing_cell_refinement       'BRUKER SMART'
_computing_data_collection       'BRUKER SMART'
_computing_data_reduction        'BRUKER SMART'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SIR97
_diffrn_ambient_temperature      173(2)
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_diffrn_measurement_device_type  'ccd area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0213
_diffrn_reflns_av_sigmaI/netI    0.0338
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            39568
_diffrn_reflns_theta_full        30.56
_diffrn_reflns_theta_max         30.56
_diffrn_reflns_theta_min         1.26
_diffrn_standards_interval_time  '20sec / frame'
_exptl_absorpt_coefficient_mu    3.885
_exptl_absorpt_correction_T_max  1.000000
_exptl_absorpt_correction_T_min  0.798197
_exptl_absorpt_correction_type   empirical
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1316
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.17
_refine_diff_density_max         2.888
_refine_diff_density_min         -0.738
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.095
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     686
_refine_ls_number_reflns         18931
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.095
_refine_ls_R_factor_all          0.0483
_refine_ls_R_factor_gt           0.0370
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0678P)^2^+3.1661P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1117
_refine_ls_wR_factor_ref         0.1187
_reflns_number_gt                16037
_reflns_number_total             18931
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0497578rom20040224_091421_4.cif
_cod_data_source_block           reo2iprcarbreo4
_cod_original_formula_sum        'C50 H92 N8 O7.50 Re2'
_cod_database_code               4311962