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_4121179
_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         C18H24ClF12N8OP2Tc
_chemical_formula_sum            'C18 H24 Cl F12 N8 O P2 Tc'
_chemical_formula_weight         791.84
_chemical_name_common            '[99TcOCl(L2)2](PF6)2'
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           1
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                83.541(3)
_cell_angle_beta                 87.715(4)
_cell_angle_gamma                62.811(4)
_cell_formula_units_Z            2
_cell_length_a                   10.9223(5)
_cell_length_b                   11.4201(4)
_cell_length_c                   12.9602(6)
_cell_measurement_reflns_used    6678
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      30.4080
_cell_measurement_theta_min      2.6890
_cell_volume                     1428.70(12)
_computing_cell_refinement
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_collection
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_computing_data_reduction
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
;
_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_detector_area_resol_mean 10.4498
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Xcalibur, Ruby'
_diffrn_measurement_method       '\w scans'
_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  0.0406
_diffrn_reflns_av_sigmaI/netI    0.0613
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            24706
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.43
_exptl_absorpt_coefficient_mu    0.819
_exptl_absorpt_correction_T_max  0.9190
_exptl_absorpt_correction_T_min  0.8172
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.19 (release 27-10-2011 CrysAlis171 .NET)
(compiled Oct 27 2011,15:02:11)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.841
_exptl_crystal_description       plate
_exptl_crystal_F_000             788
_exptl_crystal_size_max          0.26
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.11
_refine_diff_density_max         0.463
_refine_diff_density_min         -0.584
_refine_diff_density_rms         0.067
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.00(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     810
_refine_ls_number_reflns         13357
_refine_ls_number_restraints     35
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0447
_refine_ls_shift/su_max          0.011
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0364P)^2^+0.4725P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0945
_refine_ls_wR_factor_ref         0.1013
_reflns_number_gt                11832
_reflns_number_total             13357
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja409499u_si_002_5.cif
_cod_data_source_block           '[99TcOCl(L2)2](PF6)2'
_cod_original_cell_volume        1428.70(10)
_cod_database_code               4121179