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_4121178
_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         C18H26F6N8O3PTc
_chemical_formula_sum            'C18 H26 F6 N8 O3 P Tc'
_chemical_formula_weight         645.44
_chemical_name_common            '[TcO2(L2)2](PF6)xH2O'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           13
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yc'
_symmetry_space_group_name_H-M   'P 1 2/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                 90.694(8)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.7640(10)
_cell_length_b                   8.2135(6)
_cell_length_c                   15.6688(15)
_cell_measurement_reflns_used    9164
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      29.42
_cell_measurement_theta_min      2.475
_cell_volume                     1256.5(2)
_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, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.963
_diffrn_measured_fraction_theta_max 0.963
_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  0.0445
_diffrn_reflns_av_sigmaI/netI    0.0366
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7467
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.48
_diffrn_standards_interval_count 'every image'
_diffrn_standards_interval_time  18
_diffrn_standards_number         50-200
_exptl_absorpt_coefficient_mu    0.719
_exptl_absorpt_correction_T_max  0.9568
_exptl_absorpt_correction_T_min  0.8961
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   '(Coppens et al., 1965)'
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.706
_exptl_crystal_description       block
_exptl_crystal_F_000             652
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.06
_refine_diff_density_max         1.224
_refine_diff_density_min         -0.815
_refine_diff_density_rms         0.156
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.118
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     176
_refine_ls_number_reflns         2476
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0657
_refine_ls_R_factor_gt           0.0496
_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^)+(0.0682P)^2^+1.9568P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1202
_refine_ls_wR_factor_ref         0.1278
_reflns_number_gt                2009
_reflns_number_total             2476
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja409499u_si_002_4.cif
_cod_data_source_block           '[TcO2(L2)2](PF6)xH2O'
_cod_database_code               4121178