Combining Bifunctional Chelator with (3 + 2)-Cycloaddition Approaches: Synthesis of Dual-Function Technetium Complexes
Henrik Braband; Sebastian Imstepf; Michael Benz; Bernhard Spingler; Roger Alberto; Inorganic Chemistry 51 (2012) 4051–4057; doi:10.1021/ic202212e

data_4328749
_publ_section_title
;
 Combining Bifunctional Chelator with (3 + 2)-Cycloaddition Approaches:
 Synthesis of Dual-Function Technetium Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              4051
_journal_page_last               4057
_journal_paper_doi               10.1021/ic202212e
_journal_volume                  51
_journal_year                    2012
_chemical_formula_moiety         '[Tc(NOTA3H)(CO)3]Cl'
_chemical_formula_sum            'C15 H21 Cl N3 O9 Tc'
_chemical_formula_weight         520.80
_chemical_name_common            '[Tc(NOTA3H)(CO)3]Cl'
_chemical_name_systematic
;
 ?
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                94.55(2)
_cell_angle_beta                 98.59(2)
_cell_angle_gamma                107.66(2)
_cell_formula_units_Z            2
_cell_length_a                   8.794(2)
_cell_length_b                   8.958(2)
_cell_length_c                   13.342(3)
_cell_measurement_reflns_used    3386
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      30.6537
_cell_measurement_theta_min      2.4673
_cell_volume                     981.6(4)
_computing_cell_refinement       'CrysAlis RED (Oxford, 2007)'
_computing_data_collection       'CrysAlis RED (Oxford, 2007)'
_computing_data_reduction        'CrysAlis RED (Oxford, 2007)'
_computing_molecular_graphics    'ORTEP-3 (Farrugia, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0414
_diffrn_reflns_av_sigmaI/netI    0.0987
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            8196
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         2.47
_exptl_absorpt_coefficient_mu    0.924
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.99387
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Oxford Diffraction Ltd.,
Version 1.171.33.66 (release 28-04-2010 CrysAlis171 .NET)
(compiled Apr 28 2010,14:27:37)
empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.762
_exptl_crystal_description       plate
_exptl_crystal_F_000             528
_exptl_crystal_size_max          0.144
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.640
_refine_diff_density_min         -0.585
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.847
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     265
_refine_ls_number_reflns         3999
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.847
_refine_ls_R_factor_all          0.0582
_refine_ls_R_factor_gt           0.0369
_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^)+(0.0083P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0457
_refine_ls_wR_factor_ref         0.0480
_reflns_number_gt                2930
_reflns_number_total             3999
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic202212e_si_002_1.cif
_cod_data_source_block           mb300710
_cod_database_code               4328749