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_4304773
_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         'C36 H42 Cl2 N8 O3 P0 Re2 S2'
_chemical_formula_sum            'C36 H42 Cl2 N8 O3 P0 Re2 S2'
_chemical_formula_weight         1142.20
_chemical_name_common            '[{ReOCl(Et2tcbPy)}2O]'
_chemical_name_systematic
;
 mu-Oxobis[chloro(N-(N',N'-diethylaminothiocarbonyl)
-N'-picolylbenzamidinato)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                 99.538(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   10.0027(10)
_cell_length_b                   10.6300(10)
_cell_length_c                   19.441(2)
_cell_measurement_reflns_used    7686
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.19
_cell_measurement_theta_min      2.16
_cell_volume                     2038.6(4)
_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 0.957
_diffrn_measured_fraction_theta_max 0.957
_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  0.0551
_diffrn_reflns_av_sigmaI/netI    0.0652
_diffrn_reflns_limit_h_max       12
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7811
_diffrn_reflns_theta_full        26.79
_diffrn_reflns_theta_max         26.79
_diffrn_reflns_theta_min         2.82
_diffrn_standards_decay_%        0.1
_exptl_absorpt_coefficient_mu    6.212
_exptl_absorpt_correction_T_max  0.6763
_exptl_absorpt_correction_T_min  0.4677
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED'
_exptl_crystal_colour            violet
_exptl_crystal_density_diffrn    1.861
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       polyeder
_exptl_crystal_F_000             1108
_exptl_crystal_size_max          0.400
_exptl_crystal_size_mid          0.197
_exptl_crystal_size_min          0.040
_refine_diff_density_max         1.148
_refine_diff_density_min         -1.319
_refine_diff_density_rms         0.139
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.949
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     241
_refine_ls_number_reflns         4181
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.949
_refine_ls_R_factor_all          0.0569
_refine_ls_R_factor_gt           0.0341
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0343P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0648
_refine_ls_wR_factor_ref         0.0701
_reflns_number_gt                3107
_reflns_number_total             4181
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702344s-file010_5.cif
_cod_data_source_block           hnpyet
_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 
;
_cod_original_cell_volume        2038.5(3)
_cod_database_code               4304773