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_4118026
_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         'C46 H34 N7 Re'
_chemical_formula_sum            'C46 H34 N7 Re'
_chemical_formula_weight         871.00
_chemical_name_common            '[ReNPh(LPh)(LPh-H)]'
_chemical_name_systematic
;
Diphenyl(1,3,4-Triphenyl-1,2,4-triazol-5-yliden-C)(1,3,4-Triphenyl-1,2,4-
triazol-5-ylidenato-C,C)nitridotechnetium(V)
;
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 121.27(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.383(1)
_cell_length_b                   16.239(1)
_cell_length_c                   21.731(2)
_cell_measurement_reflns_used    10977
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.28
_cell_measurement_theta_min      2.19
_cell_volume                     3735.0(6)
_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-86 (Sheldrick, 1986)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.1376
_diffrn_reflns_av_sigmaI/netI    0.2003
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -29
_diffrn_reflns_number            25749
_diffrn_reflns_theta_full        29.31
_diffrn_reflns_theta_max         29.31
_diffrn_reflns_theta_min         2.39
_diffrn_standards_decay_%        0.1
_exptl_absorpt_coefficient_mu    3.297
_exptl_absorpt_correction_T_max  0.6680
_exptl_absorpt_correction_T_min  0.4566
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'X-Red 32'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.549
_exptl_crystal_description       plate
_exptl_crystal_F_000             1736
_exptl_crystal_size_max          0.29
_exptl_crystal_size_mid          0.21
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.962
_refine_diff_density_min         -1.430
_refine_diff_density_rms         0.114
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.776
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     487
_refine_ls_number_reflns         9991
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.776
_refine_ls_R_factor_all          0.1632
_refine_ls_R_factor_gt           0.0523
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0199P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0679
_refine_ls_wR_factor_ref         0.0895
_reflns_number_gt                4261
_reflns_number_total             9991
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja3033718_si_002_5.cif
_cod_data_source_block           eotriazp
_cod_original_cell_volume        3735.0(5)
_cod_database_code               4118026