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_4328752
_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         '[TcO3(eg)(tacn-ba)]Br'
_chemical_formula_sum            'C17 H28 Br N4 O4 Tc'
_chemical_formula_weight         530.34
_chemical_name_common            '[TcO3(eg)(tacn-ba)]Br'
_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                106.501(3)
_cell_angle_beta                 93.887(3)
_cell_angle_gamma                96.816(3)
_cell_formula_units_Z            2
_cell_length_a                   7.8503(3)
_cell_length_b                   10.8590(3)
_cell_length_c                   12.3046(4)
_cell_measurement_reflns_used    3738
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      30.8212
_cell_measurement_theta_min      2.6226
_cell_volume                     992.92(6)
_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, 1997)'
_computing_structure_solution    'SIR-97 (Altomare, 1999)'
_diffrn_ambient_temperature      183(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0381
_diffrn_reflns_av_sigmaI/netI    0.1006
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            9033
_diffrn_reflns_theta_full        28.28
_diffrn_reflns_theta_max         28.28
_diffrn_reflns_theta_min         2.63
_exptl_absorpt_coefficient_mu    2.768
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.96197
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   none
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.774
_exptl_crystal_description       plate
_exptl_crystal_F_000             536
_exptl_crystal_size_max          0.0083
_exptl_crystal_size_mid          0.0034
_exptl_crystal_size_min          0.0018
_refine_diff_density_max         0.550
_refine_diff_density_min         -0.714
_refine_diff_density_rms         0.109
_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     244
_refine_ls_number_reflns         4919
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.847
_refine_ls_R_factor_all          0.0673
_refine_ls_R_factor_gt           0.0375
_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^)+(0.0109P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0476
_refine_ls_wR_factor_ref         0.0507
_reflns_number_gt                3346
_reflns_number_total             4919
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic202212e_si_002_4.cif
_cod_data_source_block           si080410
_cod_database_code               4328752