Oxotechnetium(V) Complexes with a Novel Class of Tridentate Thiosemicarbazide Ligands
Hung Huy Nguyen; Pedro I. da S. Maia; Victor M. Deflon; Ulrich Abram; Inorganic Chemistry 48 (2009) 25–27; doi:10.1021/ic802044r

data_4301171
_publ_contact_author
;
      Ulrich Abram
      Free University of Berlin     
      Institute of Chemistry             
      Fabeckstrasse 34-36                     
      D-14195 Berlin         
      Germany                          
;
_publ_contact_author_email       abram@chemie.fu-berlin.de
_publ_contact_author_fax         '0049 (0)30 838 52676'
_publ_contact_author_phone       '0049 (0)30 838 54002'
_publ_section_title
;
Oxotechnetium(V) Complexes with a Novel Class of Tridentate
Thiosemicarbazide Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              25
_journal_page_last               27
_journal_paper_doi               10.1021/ic802044r
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         '[Et2NCSNC(Ph)HNNHCSNMe2]'
_chemical_formula_sum            'C15 H23 N5 O0 S2'
_chemical_formula_weight         337.52
_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                63.66(1)
_cell_angle_beta                 65.23(1)
_cell_angle_gamma                83.92(1)
_cell_formula_units_Z            2
_cell_length_a                   9.603(1)
_cell_length_b                   10.227(1)
_cell_length_c                   10.978(1)
_cell_measurement_reflns_used    9544
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.57
_cell_measurement_theta_min      2.78
_cell_volume                     873.07(19)
_computing_cell_refinement       'STOE XAREA'
_computing_data_collection       'STOE XAREA'
_computing_data_reduction        'STOE XRED32'
_computing_molecular_graphics    WINGX
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'direct methods'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.941
_diffrn_measured_fraction_theta_max 0.941
_diffrn_measurement_device_type  'STOE IPDS 2T'
_diffrn_measurement_method       'rotation method'
_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  0.0298
_diffrn_reflns_av_sigmaI/netI    0.0459
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            8476
_diffrn_reflns_theta_full        29.29
_diffrn_reflns_theta_max         29.29
_diffrn_reflns_theta_min         2.78
_exptl_absorpt_coefficient_mu    0.309
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.284
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             360
_exptl_crystal_size_max          .3
_exptl_crystal_size_mid          .2
_exptl_crystal_size_min          .2
_refine_diff_density_max         0.237
_refine_diff_density_min         -0.219
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.855
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     207
_refine_ls_number_reflns         4488
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.855
_refine_ls_R_factor_all          0.0689
_refine_ls_R_factor_gt           0.0399
_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^)+(0.0726P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0979
_refine_ls_wR_factor_ref         0.1084
_reflns_number_gt                3020
_reflns_number_total             4488
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic802044r_si_001_2.cif
_cod_data_source_block           hnthio
_cod_original_cell_volume        873.3(2)
_cod_database_code               4301171