Tricarbonylrhenium(I) Complexes with Thiosemicarbazone Derivatives of 2-Acetylpyridine and 2-Pyridine Formamide Showing Two Unusual Coordination Modes of Tridentate Thiosemicarbazone Ligands
Isabel García Santos; Ulrich Abram; Roger Alberto; Ezequiel Vázquez López; Agustín Sánchez; Inorganic Chemistry 43 (2004) 1834–1836; doi:10.1021/ic035367u

data_4310758
_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
;
 Tricarbonylrhenium(I) Complexes with Thiosemicarbazone Derivatives of
 2-Acetylpyridine and 2-Pyridine Formamide Showing Two Unusual
 Coordination Modes of Tridentate Thiosemicarbazone Ligands
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              1834
_journal_page_last               1836
_journal_paper_doi               10.1021/ic035367u
_journal_volume                  43
_journal_year                    2004
_chemical_formula_moiety         '[Re(CO)3Br(Hpytsc)] x 4 DMSO'
_chemical_formula_sum            'C18 H33 Br N5 O7 Re S5'
_chemical_formula_weight         857.90
_chemical_name_systematic
;
Bromo(2-pyridine formamide thiosemicarbazone-N,N)tricarbonylrhenium(I)
;
_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     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 111.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   18.067
_cell_length_b                   9.479
_cell_length_c                   20.290
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.3
_cell_measurement_theta_min      7.09
_cell_volume                     3244.011
_computing_cell_refinement       SET4
_computing_data_collection       CAD4
_computing_data_reduction        CAD4X
_computing_molecular_graphics    ORTEP
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       'omega scans'
_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  0.0662
_diffrn_reflns_av_sigmaI/netI    0.1527
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       0
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            7709
_diffrn_reflns_theta_full        26.98
_diffrn_reflns_theta_max         26.98
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        6
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    5.341
_exptl_absorpt_correction_T_max  .857
_exptl_absorpt_correction_T_min  .540
_exptl_absorpt_correction_type   DIFABS
_exptl_absorpt_process_details   None
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    1.757
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       needle
_exptl_crystal_F_000             1688
_exptl_crystal_size_max          .4
_exptl_crystal_size_mid          .1
_exptl_crystal_size_min          .1
_refine_diff_density_max         2.005
_refine_diff_density_min         -2.156
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.038
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     330
_refine_ls_number_reflns         7034
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.038
_refine_ls_R_factor_all          0.1750
_refine_ls_R_factor_gt           0.0598
_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^)+(0.0533P)^2^+1.8650P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1154
_refine_ls_wR_factor_ref         0.1429
_reflns_number_gt                3757
_reflns_number_total             7034
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035367usi20040130_124545_2.cif
_cod_data_source_block           rebrtsc
_cod_original_cell_volume        3243.9
_cod_database_code               4310758