Aryl and NHC Compounds of Technetium and Rhenium
Elisabeth Oehlke; Shushu Kong; Pawel Arciszewski; Swantje Wiebalck; Ulrich Abram; Journal of the American Chemical Society 134 (2012) 9118–9121; doi:10.1021/ja3033718

data_4118022
_publ_contact_author_address
;Freie Universit\"at Berlin, Institute of 
Chemistry and Biochemistry, Fabeckstr. 34-36,
 D-14195 Berlin, Germany
;
_publ_contact_author_email       ulrich.abram@fu-berlin.de
_publ_contact_author_fax         '(#49) 30 83852676'
_publ_contact_author_name        'Ulrich Abram'
_publ_contact_author_phone       '(#49) 30 83854002'
_publ_section_title
;
 Aryl and NHC Compounds of Technetium and Rhenium
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              9118
_journal_page_last               9121
_journal_paper_doi               10.1021/ja3033718
_journal_volume                  134
_journal_year                    2012
_chemical_formula_moiety         'C28 H48 Cl N9 Tc, Cl'
_chemical_formula_sum            'C28 H48 Cl2 N9 Tc'
_chemical_formula_weight         679.65
_chemical_name_common            '[TcNCl(LMe)4]Cl'
_chemical_name_systematic
;
Tetrakis(1,3,4,5-tetramethylimidazol-2-ylidene)nitridotechnetium(V)
chloride
;
_space_group_IT_number           104
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4 -2n'
_symmetry_space_group_name_H-M   'P 4 n c'
_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                   13.484(1)
_cell_length_b                   13.484(1)
_cell_length_c                   9.799(1)
_cell_measurement_reflns_used    10.956
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.06
_cell_measurement_theta_min      2.56
_cell_volume                     1781.6(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    'ORTEP 3'
_computing_publication_material  WinGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.965
_diffrn_measured_fraction_theta_max 0.965
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_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  0.1001
_diffrn_reflns_av_sigmaI/netI    0.0602
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            30686
_diffrn_reflns_theta_full        29.18
_diffrn_reflns_theta_max         29.18
_diffrn_reflns_theta_min         3.38
_diffrn_standards_decay_%        0.1
_exptl_absorpt_coefficient_mu    0.584
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.267
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.154
_refine_diff_density_min         -0.768
_refine_diff_density_rms         0.094
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.27(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.690
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     115
_refine_ls_number_reflns         2326
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.690
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0671
_refine_ls_shift/su_max          0.004
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.2000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1745
_refine_ls_wR_factor_ref         0.2092
_reflns_number_gt                1296
_reflns_number_total             2326
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3033718_si_002_1.cif
_cod_data_source_block           eotctrime
_cod_database_code               4118022