Rhenium and Technetium Complexes with Tridentate N-[(N",N"-Dialkylamino)(thiocarbonyl)]-N'-substituted Benzamidine Ligands
Nguyen Hung Huy; Jacqueline Grewe; Jennifer Schroer; Bernd Kuhn; Ulrich Abram; Inorganic Chemistry 47 (2008) 5136–5144; doi:10.1021/ic702344s

data_4304774
_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
;
Rhenium and Technetium Complexes with Tridentate
N-[(N",N"-Dialkylamino)(thiocarbonyl)]-N'-substituted Benzamidine 
Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              5136
_journal_page_last               5144
_journal_paper_doi               10.1021/ic702344s
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C20 H25 N3 O3 S'
_chemical_formula_sum            'C20 H25 N3 O3 S'
_chemical_formula_weight         387.49
_chemical_name_common            Et2tcbPhCOOH
_chemical_name_systematic
;
 N-(N',N'-diethylaminothiocarbonyl)-N'-(2-carboxyphenyl)benzamidine
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 102.368(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            8
_cell_length_a                   21.356(2)
_cell_length_b                   10.8093(10)
_cell_length_c                   18.663(2)
_cell_measurement_reflns_used    6146
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.67
_cell_measurement_theta_min      1.96
_cell_volume                     4208.2(7)
_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  '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 0.979
_diffrn_measured_fraction_theta_max 0.979
_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  0.1247
_diffrn_reflns_av_sigmaI/netI    0.1441
_diffrn_reflns_limit_h_max       22
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            14200
_diffrn_reflns_theta_full        29.30
_diffrn_reflns_theta_max         29.30
_diffrn_reflns_theta_min         1.95
_diffrn_standards_decay_%        0.1
_exptl_absorpt_coefficient_mu    0.178
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.223
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1648
_exptl_crystal_size_max          0.4
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.2
_refine_diff_density_max         0.318
_refine_diff_density_min         -0.335
_refine_diff_density_rms         0.102
_refine_ls_extinction_coef       0.0055(4)
_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   1.077
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     247
_refine_ls_number_reflns         5641
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.1837
_refine_ls_R_factor_gt           0.0633
_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^)+(0.0461P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1079
_refine_ls_wR_factor_ref         0.1674
_reflns_number_gt                2182
_reflns_number_total             5641
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702344s-file010_6.cif
_cod_data_source_block           jganthr
_cod_original_cell_volume        4208.1(7)
_cod_database_code               4304774