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_4310757
_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)3(APTPhtsc)]'
_chemical_formula_sum            'C17 H13 N4 O3 Re S'
_chemical_formula_weight         539.57
_chemical_name_systematic
'(Acetylpyridine phenylthiosemicarbazonato)tricarbonylrhenium(I)'
_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   difmap
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                90.00
_cell_angle_beta                 90.31(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   11.705(1)
_cell_length_b                   13.552(1)
_cell_length_c                   11.389(1)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    213(2)
_cell_measurement_theta_max      26.77
_cell_measurement_theta_min      15.28
_cell_volume                     1806.6(3)
_computing_cell_refinement       SET4
_computing_data_collection       CAD4
_computing_data_reduction        'HELENA (Spek, 1997)'
_computing_molecular_graphics    'SCHAKAL, ZORTEP'
_computing_publication_material  SHELXL97
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      213(2)
_diffrn_measured_fraction_theta_full 0.954
_diffrn_measured_fraction_theta_max 0.954
_diffrn_measurement_device_type  CAD4
_diffrn_measurement_method       'omega scan'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0195
_diffrn_reflns_av_sigmaI/netI    0.0229
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       1
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       13
_diffrn_reflns_limit_l_min       -13
_diffrn_reflns_number            3878
_diffrn_reflns_theta_full        64.92
_diffrn_reflns_theta_max         64.92
_diffrn_reflns_theta_min         5.07
_diffrn_standards_decay_%        7.5
_diffrn_standards_interval_count 300
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    14.461
_exptl_absorpt_correction_T_max  0.6229
_exptl_absorpt_correction_T_min  0.3842
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            orange-red
_exptl_crystal_density_diffrn    1.984
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1032
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.10
_refine_diff_density_max         0.637
_refine_diff_density_min         -0.529
_refine_diff_density_rms         0.082
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.045
_refine_ls_hydrogen_treatment    refall
_refine_ls_matrix_type           full
_refine_ls_number_parameters     287
_refine_ls_number_reflns         3063
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.0285
_refine_ls_R_factor_gt           0.0227
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+2.4408P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0543
_refine_ls_wR_factor_ref         0.0563
_reflns_number_gt                2751
_reflns_number_total             3063
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic035367usi20040130_124545_1.cif
_cod_data_source_block           tsc
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'PSI scan' changed to 'psi-scan'
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 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc
w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+2.4408P] where P=(Fo^2^+2Fc^2^)/3' was
changed to 'calc'. New tag '_refine_ls_weighting_details' was
created. The value of the new tag was set to
'w=1/[\s^2^(Fo^2^)+(0.0272P)^2^+2.4408P] where P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_database_code               4310757