Synthesis, Structural Characterization, and Biological Evaluation of Oxorhenium(V) Complexes with a Novel Type of Thiosemicarbazones Derived from N-[N',N'-Dialkylamino(thiocarbonyl)]benzimidoyl Chlorides
Hung Huy Nguyen; Jesudas J. Jegathesh; Pedro I. da S. Maia; Victor M. Deflon; Ronald Gust; Silke Bergemann; Ulrich Abram; Inorganic Chemistry 48 (2009) 9356–9364; doi:10.1021/ic901160v

data_4303276
_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
;
Synthesis, Structural Characterization, and Biological Evaluation of
Oxorhenium(V) Complexes with a Novel Type of Thiosemicarbazones Derived
from N-[N',N'-Dialkylamino(thiocarbonyl)]benzimidoyl Chlorides
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              9356
_journal_page_last               9364
_journal_paper_doi               10.1021/ic901160v
_journal_volume                  48
_journal_year                    2009
_chemical_formula_moiety         'C37 H42 N6 P Re S2'
_chemical_formula_sum            'C37 H42 N6 P Re S2'
_chemical_formula_weight         852.06
_chemical_name_common            '[ReNPPh3(PhC(NNCSNC6H12)NCSNEt2)]'
_chemical_name_systematic
;
N-(N',N'-Diethylaminothiocarbonyl)-N''-(N-1-Hexamethyleneimine
carbothioamide)benzamidinato(triphenylphosphine)nitridorhenium(V)
;
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 107.04(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   14.763(1)
_cell_length_b                   25.552(1)
_cell_length_c                   20.082(1)
_cell_measurement_reflns_used    29657
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.64
_cell_measurement_theta_min      2.18
_cell_volume                     7242.9(8)
_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  WinGX
_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 0.987
_diffrn_measured_fraction_theta_max 0.987
_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  0.0894
_diffrn_reflns_av_sigmaI/netI    0.0614
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            40089
_diffrn_reflns_theta_full        29.29
_diffrn_reflns_theta_max         29.29
_diffrn_reflns_theta_min         1.65
_diffrn_standards_decay_%        0.5
_exptl_absorpt_coefficient_mu    3.550
_exptl_absorpt_correction_T_max  0.8647
_exptl_absorpt_correction_T_min  0.4833
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.563
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             3424
_exptl_crystal_size_max          0.320
_exptl_crystal_size_mid          0.163
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.849
_refine_diff_density_min         -3.059
_refine_diff_density_rms         0.272
_refine_ls_extinction_coef       0.00163(7)
_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   1.008
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     425
_refine_ls_number_reflns         9792
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.008
_refine_ls_R_factor_all          0.0687
_refine_ls_R_factor_gt           0.0456
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0687P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1004
_refine_ls_wR_factor_ref         0.1179
_reflns_number_gt                7252
_reflns_number_total             9792
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901160v_si_001_1.cif
_cod_data_source_block           pirenl4
_cod_original_cell_volume        7243.1(7)
_cod_database_code               4303276