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

data_4311961
_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_sum            'C28 H48 F3.3 N8 O5.8 P0.55 Re1.45'
_chemical_formula_weight         939.27
_chemical_name_systematic        ?
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_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                 95.63(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.309(2)
_cell_length_b                   20.142(3)
_cell_length_c                   18.763(3)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      11.47
_cell_measurement_theta_min      7.77
_cell_volume                     3877.2(11)
_computing_cell_refinement       SET4
_computing_data_collection       CAD4
_computing_data_reduction        WINGX
_computing_molecular_graphics    ORTEP
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.894
_diffrn_measured_fraction_theta_max 0.894
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       'omega 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  0.0386
_diffrn_reflns_av_sigmaI/netI    0.0606
_diffrn_reflns_limit_h_max       7
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -1
_diffrn_reflns_number            8063
_diffrn_reflns_theta_full        26.97
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         3.11
_diffrn_standards_decay_%        5
_diffrn_standards_interval_count 400
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    4.615
_exptl_absorpt_correction_T_max  .503
_exptl_absorpt_correction_T_min  .063
_exptl_absorpt_correction_type   'empirical, DELABS'
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.609
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1860
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .2
_refine_diff_density_max         0.700
_refine_diff_density_min         -1.759
_refine_diff_density_rms         0.223
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.019
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         7542
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.019
_refine_ls_R_factor_all          0.1058
_refine_ls_R_factor_gt           0.0550
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0989P)^2^+10.7143P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1417
_refine_ls_wR_factor_ref         0.1770
_reflns_number_gt                4926
_reflns_number_total             7542
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0497578rom20040224_091421_3.cif
_cod_data_source_block           reo2mecarb
_cod_original_cell_volume        3877(1)
_cod_original_formula_sum        'C28 H48 F3.30 N8 O5.80 P0.55 Re1.45'
_cod_database_code               4311961