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

data_4311959
_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         '[ReO(OMe)(tetramethylimidazolydene)4][PF6]2'
_chemical_formula_sum            'C29 H51 F12 N8 O2 P2 Re'
_chemical_formula_weight         1019.92
_chemical_name_common            '[ReO(OMe)(tetramethylimidazolydene)4][PF6]2'
_chemical_name_systematic
;
Methoxytetrakis(1,3,4,5-tetramethylimidazol-2-ylidene)oxorhenium 
bis(hexafluorophosphate)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 99.03(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   8.459(4)
_cell_length_b                   21.184(4)
_cell_length_c                   23.314(14)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    571(2)
_cell_measurement_theta_max      14.650
_cell_measurement_theta_min      6.256
_cell_volume                     4126(3)
_computing_cell_refinement       CAD4
_computing_data_collection       CAD4
_computing_data_reduction        HELENA
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      571(2)
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_diffrn_measurement_device_type  'CAD4 ENRAF NONIS'
_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  0.0772
_diffrn_reflns_av_sigmaI/netI    0.2158
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            10546
_diffrn_reflns_theta_full        26.97
_diffrn_reflns_theta_max         26.97
_diffrn_reflns_theta_min         3.02
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 400
_diffrn_standards_interval_time  400
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    3.115
_exptl_absorpt_correction_T_max  0.9762
_exptl_absorpt_correction_T_min  0.8097
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.642
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             2040
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.226
_refine_diff_density_min         -0.709
_refine_diff_density_rms         0.136
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.902
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     596
_refine_ls_number_reflns         8759
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.902
_refine_ls_R_factor_all          0.1988
_refine_ls_R_factor_gt           0.0649
_refine_ls_shift/su_max          0.316
_refine_ls_shift/su_mean         0.018
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0562P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1074
_refine_ls_wR_factor_ref         0.1450
_reflns_number_gt                4018
_reflns_number_total             8759
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0497578rom20040224_091421_1.cif
_cod_data_source_block           reomeomecarb
_cod_depositor_comments
;
The following automatic conversions were performed:
'_symmetry_cell_setting' value 'Monoclinic' changed to 'monoclinic'
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 

The following automatic conversions were performed:

'_exptl_absorpt_correction_type' tag value 'Psi-scans' was replaced
with 'psi-scan' value.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_database_code               4311959