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_4308262
_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         'C48 H60  N8 O7  Re2 S4'
_chemical_formula_sum            'C48 H60 N8 O7 Re2 S4'
_chemical_formula_weight         1361.68
_chemical_name_common            Re2O3(PhCONCSCEt2)4
_chemical_name_systematic
;
mu-oxo{bis(N-benzoyl-N'N'-diethylthioureato)oxorhenium(V)} 
;
_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     heavy
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 108.50(5)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   20.955(9)
_cell_length_b                   15.933(9)
_cell_length_c                   16.66(1)
_cell_measurement_reflns_used    355
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      28.39
_cell_measurement_theta_min      3.20
_cell_volume                     5275(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 0.986
_diffrn_measured_fraction_theta_max 0.986
_diffrn_measurement_device_type  STOE
_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  0.1978
_diffrn_reflns_av_sigmaI/netI    0.1462
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            56774
_diffrn_reflns_theta_full        29.28
_diffrn_reflns_theta_max         29.28
_diffrn_reflns_theta_min         1.88
_diffrn_standards_decay_%        0.5
_exptl_absorpt_coefficient_mu    4.800
_exptl_absorpt_correction_T_max  0.6845
_exptl_absorpt_correction_T_min  0.4659
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED'
_exptl_crystal_colour            green
_exptl_crystal_density_diffrn    1.715
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             2696
_exptl_crystal_size_max          1.000
_exptl_crystal_size_mid          0.400
_exptl_crystal_size_min          0.100
_refine_diff_density_max         2.891
_refine_diff_density_min         -4.707
_refine_diff_density_rms         0.197
_refine_ls_extinction_coef       0.00102(8)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     618
_refine_ls_number_reflns         14195
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.032
_refine_ls_R_factor_all          0.1237
_refine_ls_R_factor_gt           0.0782
_refine_ls_shift/su_max          0.007
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0217P)^2^+10.8305P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1123
_refine_ls_wR_factor_ref         0.1225
_reflns_number_gt                9066
_reflns_number_total             14195
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic070323x-file001_6.cif
_cod_data_source_block           dimerreoet2btu
_cod_depositor_comments
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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_formula_sum        'C48 H60 N8 O7  Re2 S4'
_cod_database_code               4308262