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_4118023
_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         'C56 H56 N O2 P2 Tc'
_chemical_formula_sum            'C56 H56 N O2 P2 Tc'
_chemical_formula_weight         934.96
_chemical_name_common            TcNPh2(PPh3)2
_chemical_name_systematic
;
Nitridodiphenylbis(triphenylphosphine)technetium(V) tetrahydrofuran solvate
;
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                105.39(1)
_cell_angle_beta                 93.52(1)
_cell_angle_gamma                99.12(1)
_cell_formula_units_Z            2
_cell_length_a                   9.984(1)
_cell_length_b                   13.382(1)
_cell_length_c                   18.572(2)
_cell_measurement_reflns_used    13150
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.47
_cell_measurement_theta_min      2.22
_cell_volume                     2348.1(4)
_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 0.967
_diffrn_measured_fraction_theta_max 0.967
_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  0.1229
_diffrn_reflns_av_sigmaI/netI    0.1646
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            24749
_diffrn_reflns_theta_full        29.25
_diffrn_reflns_theta_max         29.25
_diffrn_reflns_theta_min         2.55
_diffrn_standards_decay_%        0.1
_exptl_absorpt_coefficient_mu    0.418
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.323
_exptl_crystal_description       plate
_exptl_crystal_F_000             976
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.595
_refine_diff_density_min         -0.767
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.788
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     559
_refine_ls_number_reflns         12395
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.788
_refine_ls_R_factor_all          0.1245
_refine_ls_R_factor_gt           0.0545
_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^)+(0.0559P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1002
_refine_ls_wR_factor_ref         0.1242
_reflns_number_gt                6675
_reflns_number_total             12395
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ja3033718_si_002_2.cif
_cod_data_source_block           eopa10
_cod_original_cell_volume        2347.8(3)
_cod_database_code               4118023