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_4303278
_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         'C17 H23 Cl N5 O Re S2'
_chemical_formula_sum            'C17 H23 Cl N5 O Re S2'
_chemical_formula_weight         599.02
_chemical_name_common            '[ReOCl(Pyrotsc-Et2bzm)]'
_chemical_name_systematic
;
N-(N',N'- Diethylaminothiocarbonyl)-N''-(N-1-Pyrrolidine
carbothioamide)benzamidinato(chloro)oxorhenium(V)
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 113.76(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   10.982(1)
_cell_length_b                   21.900(1)
_cell_length_c                   9.524(1)
_cell_measurement_reflns_used    11580
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      29.13
_cell_measurement_theta_min      2.22
_cell_volume                     2096.4(3)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    ORTEP3
_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 0.981
_diffrn_measured_fraction_theta_max 0.981
_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  0.0987
_diffrn_reflns_av_sigmaI/netI    0.0894
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            15000
_diffrn_reflns_theta_full        29.30
_diffrn_reflns_theta_max         29.30
_diffrn_reflns_theta_min         1.86
_diffrn_standards_decay_%        0.5
_exptl_absorpt_coefficient_mu    6.140
_exptl_absorpt_correction_T_max  0.8484
_exptl_absorpt_correction_T_min  0.2861
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.898
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1168
_exptl_crystal_size_max          0.760
_exptl_crystal_size_mid          0.310
_exptl_crystal_size_min          0.010
_refine_diff_density_max         2.220
_refine_diff_density_min         -1.468
_refine_diff_density_rms         0.415
_refine_ls_extinction_coef       0.0146(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   0.970
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     246
_refine_ls_number_reflns         5624
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.970
_refine_ls_R_factor_all          0.0904
_refine_ls_R_factor_gt           0.0520
_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^)+(0.0777P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1437
_reflns_number_gt                3672
_reflns_number_total             5624
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic901160v_si_001_3.cif
_cod_data_source_block           hnregcob2
_cod_depositor_comments
;
The following automatic conversions were performed:
'_refine_ls_hydrogen_treatment' value 'Constr' changed to 'constr'
according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic'
dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29.

Automatic conversion script
Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius 
;
_cod_original_cell_volume        2096.5(3)
_cod_database_code               4303278