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_4310759
_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(SB)]'
_chemical_formula_sum            'C13 H14 Br N2 O3 Re'
_chemical_formula_weight         512.37
_chemical_name_common            '[Re(CO)3Br(SB)]'
_chemical_name_systematic
'[2-(1-n-butyliminomethyl)pyridine-N,N]bromotricarbonylrhenium(I)'
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     Patterson
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL
_cell_angle_alpha                77.57(5)
_cell_angle_beta                 77.81(5)
_cell_angle_gamma                82.06(5)
_cell_formula_units_Z            2
_cell_length_a                   7.218(5)
_cell_length_b                   8.088(6)
_cell_length_c                   13.936(9)
_cell_measurement_reflns_used    25
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      13.58
_cell_measurement_theta_min      7.81
_cell_volume                     772.9(10)
_computing_cell_refinement       CAD4
_computing_data_collection       CAD4
_computing_data_reduction        'HELENA, PLATON (Spek, 1994)'
_computing_molecular_graphics
'SCHAKAL (Keller, 1992), ZORTEP (Zsolnai, 1994)'
_computing_publication_material  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_refinement  'SHELXL-93 (Sheldrick, 1993)'
_computing_structure_solution    'SHELXS-86 (Sheldrick, 1990)'
_diffrn_ambient_temperature      293(2)
_diffrn_measurement_device       CAD4
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoKa
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0309
_diffrn_reflns_av_sigmaI/netI    0.0282
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -1
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            4190
_diffrn_reflns_theta_max         27.01
_diffrn_reflns_theta_min         3.01
_diffrn_standards_decay_%        0
_diffrn_standards_interval_count 200
_diffrn_standards_interval_time  3600
_diffrn_standards_number         3
_exptl_absorpt_coefficient_mu    10.453
_exptl_absorpt_correction_T_max  0.94169
_exptl_absorpt_correction_T_min  0.73337
_exptl_absorpt_correction_type   psi-scan
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    2.202
_exptl_crystal_density_meas      ?
_exptl_crystal_description       needle
_exptl_crystal_F_000             480
_exptl_crystal_size_max          0.15
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.255
_refine_diff_density_min         -1.128
_refine_diff_density_rms         .127
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_all   1.115
_refine_ls_goodness_of_fit_obs   1.132
_refine_ls_hydrogen_treatment    'riding model'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     181
_refine_ls_number_reflns         3377
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.120
_refine_ls_restrained_S_obs      1.137
_refine_ls_R_factor_all          0.0347
_refine_ls_R_factor_obs          0.0299
_refine_ls_shift/esd_max         0.000
_refine_ls_shift/esd_mean        0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[s^2^(Fo^2^)+( 0.0391P)^2^+1.6299P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_all         0.0804
_refine_ls_wR_factor_obs         0.0780
_reflns_number_observed          3102
_reflns_number_total             3377
_reflns_observed_criterion       >2sigma(I)
_cod_data_source_file            ic035367usi20040130_124545_3.cif
_cod_data_source_block           sb
_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:

'_exptl_crystal_density_meas' value 'none' was changed to '?' - the
value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 3008 2015-01-20 13:52:24Z robertas 

The following automatic conversions were performed:

'_refine_ls_weighting_scheme' value 'calc w=1/[s^2^(Fo^2^)+(
0.0391P)^2^+1.6299P] 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^)+( 0.0391P)^2^+1.6299P] where
P=(Fo^2^+2Fc^2^)/3'.

Automatic conversion script
Id: cif_fix_values 3143 2015-03-26 13:38:13Z robertas 
;
_cod_original_cell_volume        772.9(9)
_cod_database_code               4310759