Rhenium and Technetium Complexes with N,N-Dialkyl-N'-benzoylthioureas
Nguyen Hung Huy; Ulrich Abram; Inorganic Chemistry 46 (2007) 5310–5319; doi:10.1021/ic070323x

data_4308264
_publ_contact_author
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      Ulrich Abram
      Free University of Berlin     
      Institute of Chemistry             
      Fabeckstrasse 34-36                     
      D-14195 Berlin         
      Germany                          
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_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
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Rhenium and Technetium Complexes with N,N-Dialkyl-N'-benzoylthioureas
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_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5310
_journal_page_last               5319
_journal_paper_doi               10.1021/ic070323x
_journal_volume                  46
_journal_year                    2007
_chemical_formula_moiety         'C61 H49 Cl0 N6 O4 S3 Tc'
_chemical_formula_sum            'C61 H49 Cl0 N6 O4 S3 Tc'
_chemical_formula_weight         1124.24
_chemical_name_common            Tc(PhCONCSNPh2)3
_chemical_name_systematic
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Tris(N-benzoyl-N',N'-diphenylthioureato_O,S)technetium(III) x MeOH
;
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                93.08(1)
_cell_angle_beta                 106.80(1)
_cell_angle_gamma                95.57(1)
_cell_formula_units_Z            2
_cell_length_a                   12.999(1)
_cell_length_b                   13.635(1)
_cell_length_c                   16.615(2)
_cell_measurement_reflns_used    16944
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      26.92
_cell_measurement_theta_min      2.06
_cell_volume                     2795.5(5)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    Ortep
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.977
_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  0.0915
_diffrn_reflns_av_sigmaI/netI    0.1469
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            24178
_diffrn_reflns_theta_full        26.86
_diffrn_reflns_theta_max         26.86
_diffrn_reflns_theta_min         1.51
_diffrn_standards_decay_%        0.5
_exptl_absorpt_coefficient_mu    0.422
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.336
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1160
_exptl_crystal_size_max          0.450
_exptl_crystal_size_mid          0.317
_exptl_crystal_size_min          0.250
_refine_diff_density_max         0.935
_refine_diff_density_min         -0.911
_refine_diff_density_rms         0.171
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.888
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     698
_refine_ls_number_reflns         11749
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.888
_refine_ls_R_factor_all          0.1291
_refine_ls_R_factor_gt           0.0588
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0823P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1335
_refine_ls_wR_factor_ref         0.1697
_reflns_number_gt                5999
_reflns_number_total             11749
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic070323x-file001_8.cif
_cod_data_source_block           tcph2btu3
_cod_depositor_comments
;
The following automatic conversions were performed:

'_atom_sites_solution_primary' value 'heavy atom' was changed to
'heavy'.

Automatic conversion script
Id: cif_fix_values 6452 2018-10-05 10:23:21Z andrius 
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_cod_original_cell_volume        2795.6(4)
_cod_database_code               4308264