Synthesis and Structural Characterization of Cationic Rhenium(V) and Technetium(V) Dioxo Complexes Containing Four N-Heterocyclic Carbene Ligands
Henrik Braband; Theresa I. Zahn; Ulrich Abram; Inorganic Chemistry 42 (2003) 6160–6162; doi:10.1021/ic0348345

data_4314391
_publ_contact_author
;
      Ulrich Abram
      Free University of Berlin     
      Institute of Chemistry             
      Fabeckstrasse 34-36                     
      D-14195 Berlin         
      Germany                          
;
_publ_contact_author_email       abram@chemie.fu-berlin.de
_publ_contact_author_fax         '0049 (0)30 838 52676'
_publ_contact_author_phone       '0049 (0)30 838 54002'
_publ_section_title
;
 Synthesis and Structural Characterization of Cationic Rhenium(V) and
 Technetium(V) Dioxo Complexes Containing Four N-Heterocyclic Carbene
 Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              6160
_journal_page_last               6162
_journal_paper_doi               10.1021/ic0348345
_journal_volume                  42
_journal_year                    2003
_chemical_formula_sum            'C54 H100 N8 O8.5 Tc2'
_chemical_formula_weight         1193.42
_chemical_name_systematic
;
Tetrakis(1,3-diisopropyl-4,5-dimethylimidazol-2-ylidene)dioxotechnetium(V) 
pertechnetate
;
_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                100.134(5)
_cell_angle_beta                 98.187(5)
_cell_angle_gamma                106.092(5)
_cell_formula_units_Z            2
_cell_length_a                   12.302(5)
_cell_length_b                   16.386(5)
_cell_length_c                   16.688(5)
_cell_measurement_temperature    173(2)
_cell_volume                     3116.1(18)
_computing_cell_refinement       'Bruker Smart'
_computing_data_collection       'Bruker 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      173(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker Smart'
_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  0.0367
_diffrn_reflns_av_sigmaI/netI    0.0600
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            32131
_diffrn_reflns_theta_full        28.00
_diffrn_reflns_theta_max         28.00
_diffrn_reflns_theta_min         1.85
_diffrn_standards_decay_%        0
_diffrn_standards_interval_time  10sec/frame
_exptl_absorpt_coefficient_mu    0.498
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.272
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1268
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.909
_refine_diff_density_min         -1.888
_refine_diff_density_rms         0.110
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.027
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     696
_refine_ls_number_reflns         14919
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.027
_refine_ls_R_factor_all          0.0864
_refine_ls_R_factor_gt           0.0574
_refine_ls_shift/su_max          0.396
_refine_ls_shift/su_mean         0.010
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0945P)^2^+2.8722P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1531
_refine_ls_wR_factor_ref         0.1703
_reflns_number_gt                10796
_reflns_number_total             14919
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic0348345si20030716_125321_2.cif
_cod_data_source_block           tcocarb
_cod_depositor_comments
;
The following automatic conversions were performed:

'_exptl_absorpt_correction_type' value 'None' changed to 'none'
according to the built-in table from CIF Core dictionary named
'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_values 1646 2011-03-28 12:23:43Z adriana 
;
_cod_original_formula_sum        'C54 H100 N8 O8.50 Tc2'
_cod_database_code               4314391