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_4328750
_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         'C9 H15 Cl N3 O3 Tc'
_chemical_formula_sum            'C9 H15 Cl N3 O3 Tc'
_chemical_formula_weight         346.69
_chemical_name_common            '[Tc(tacn)(CO)3]Cl'
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 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                 92.167(9)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   13.1764(10)
_cell_length_b                   13.4243(6)
_cell_length_c                   7.4419(5)
_cell_measurement_reflns_used    6303
_cell_measurement_temperature    183(2)
_cell_measurement_theta_max      30.25
_cell_measurement_theta_min      3.05
_cell_volume                     1315.41(15)
_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, 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 0.992
_diffrn_measured_fraction_theta_max 0.992
_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     0.71073
_diffrn_reflns_av_R_equivalents  0.0800
_diffrn_reflns_av_sigmaI/netI    0.0630
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       9
_diffrn_reflns_limit_l_min       -8
_diffrn_reflns_number            9959
_diffrn_reflns_theta_full        26.37
_diffrn_reflns_theta_max         26.37
_diffrn_reflns_theta_min         3.09
_diffrn_standards_interval_count 'every image'
_diffrn_standards_interval_time  15
_diffrn_standards_number         50-200
_exptl_absorpt_coefficient_mu    1.298
_exptl_absorpt_correction_T_max  0.9721
_exptl_absorpt_correction_T_min  0.8979
_exptl_absorpt_correction_type   numerical
_exptl_absorpt_process_details   none
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.751
_exptl_crystal_description       needle
_exptl_crystal_F_000             696
_exptl_crystal_size_max          0.13
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.816
_refine_diff_density_min         -0.686
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     154
_refine_ls_number_reflns         2671
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0759
_refine_ls_R_factor_gt           0.0568
_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^)+(0.0883P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1361
_refine_ls_wR_factor_ref         0.1465
_reflns_number_gt                1920
_reflns_number_total             2671
_reflns_threshold_expression     >2\s(I)
_cod_data_source_file            ic202212e_si_002_2.cif
_cod_data_source_block           yt141205
_cod_database_code               4328750