Toward Organometallic 99mTc Imaging Agents: Synthesis of Water-Stable 99Tc-NHC Complexes
Michael Benz; Bernhard Spingler; Roger Alberto; Henrik Braband; Journal of the American Chemical Society 135 (2013) 17566–17572; doi:10.1021/ja409499u

data_4121175
_publ_section_title
;
 Toward Organometallic 99mTc Imaging Agents: Synthesis of Water-Stable
 99Tc-NHC Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              17566
_journal_page_last               17572
_journal_paper_doi               10.1021/ja409499u
_journal_volume                  135
_journal_year                    2013
_chemical_formula_moiety         C7H15LiNO6Tc
_chemical_formula_sum            'C7 H15 Li N O6 Tc'
_chemical_formula_weight         314.14
_chemical_name_common            Li[TcO(glyc)2]DMF
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 101.810(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   7.2092(7)
_cell_length_b                   9.1767(6)
_cell_length_c                   17.0327(16)
_cell_measurement_reflns_used    13656
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      29.645
_cell_measurement_theta_min      2.445
_cell_volume                     1102.97(17)
_computing_cell_refinement       'IPDS (Stoe, 1999)'
_computing_data_collection       'IPDS (Stoe, 1999)'
_computing_data_reduction        'X-Red (Stoe, 1999)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Stoe IPDS'
_diffrn_measurement_method       '/f oscillation scan'
_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  0.0000
_diffrn_reflns_av_sigmaI/netI    0.0148
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       0
_diffrn_reflns_number            2729
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.44
_diffrn_standards_interval_count 'every image'
_diffrn_standards_interval_time  13
_diffrn_standards_number         50-200
_exptl_absorpt_coefficient_mu    1.315
_exptl_absorpt_correction_T_max  0.8200
_exptl_absorpt_correction_T_min  0.6869
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(Coppens et al., 1965)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.892
_exptl_crystal_description       block
_exptl_crystal_F_000             632
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         0.523
_refine_diff_density_min         -1.369
_refine_diff_density_rms         0.180
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     147
_refine_ls_number_reflns         2729
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.0380
_refine_ls_R_factor_gt           0.0316
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0662P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0861
_refine_ls_wR_factor_ref         0.0884
_reflns_number_gt                2301
_reflns_number_total             2729
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja409499u_si_002_1.cif
_cod_data_source_block           Li[TcO(glyc)2]DMF
_cod_database_code               4121175