Rhenium Complexes with Triazine Derivatives Formed from Semicarbazones and Thiosemicarbazones
Elena López-Torres; Ulrich Abram; Inorganic Chemistry 47 (2008) 2890–2896; doi:10.1021/ic702326v

data_4304752
_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 Complexes with Triazine Derivatives Formed from Semicarbazones and
Thiosemicarbazones
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              2890
_journal_page_last               2896
_journal_paper_doi               10.1021/ic702326v
_journal_volume                  47
_journal_year                    2008
_chemical_formula_moiety         'C63 H45 N9 P Re S3  C1.5 H3 O0.5'
_chemical_formula_sum            'C64.5 H48 N9 O0.5 P Re S3'
_chemical_formula_weight         1270.47
_chemical_name_systematic
;
Tris(5,6-diphenyl-1,2,4-triazine-3-thionato)(triphenylphosphine)-
rhenium(III) acetone solvate
;
_space_group_IT_number           4
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  'P 2yb'
_symmetry_space_group_name_H-M   'P 1 21 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                 103.03(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   9.564(1)
_cell_length_b                   22.511(1)
_cell_length_c                   13.818(1)
_cell_measurement_reflns_used    15473
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.56
_cell_measurement_theta_min      2.36
_cell_volume                     2898.4(4)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    ORTEP32
_computing_publication_material  WINGX
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    SHELXS-97
_diffrn_ambient_temperature      293(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_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  0.1168
_diffrn_reflns_av_sigmaI/netI    0.1442
_diffrn_reflns_limit_h_max       10
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       27
_diffrn_reflns_limit_k_min       -27
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            15844
_diffrn_reflns_theta_full        26.00
_diffrn_reflns_theta_max         26.00
_diffrn_reflns_theta_min         2.36
_diffrn_standards_decay_%        .1
_exptl_absorpt_coefficient_mu    2.282
_exptl_absorpt_correction_T_max  .7919
_exptl_absorpt_correction_T_min  .7467
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED32'
_exptl_crystal_colour            blue
_exptl_crystal_density_diffrn    1.456
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             1280
_exptl_crystal_size_max          .55
_exptl_crystal_size_mid          .38
_exptl_crystal_size_min          .1
_refine_diff_density_max         2.232
_refine_diff_density_min         -2.090
_refine_diff_density_rms         0.162
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.001(11)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     715
_refine_ls_number_reflns         10967
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0964
_refine_ls_R_factor_gt           0.0667
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0710P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1372
_refine_ls_wR_factor_ref         0.1500
_reflns_number_gt                8341
_reflns_number_total             10967
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702326v-file007_1.cif
_cod_data_source_block           re(SN)3(pph3)
_cod_depositor_comments
;
The following automatic conversions were performed:
'_exptl_absorpt_correction_type' value 'Integration' changed to
'integration' 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 
;
_cod_original_cell_volume        2898.4(3)
_cod_original_sg_symbol_H-M      'P 21'
_cod_original_formula_sum        'C64.50 H48 N9 O0.50 P Re S3'
_cod_database_code               4304752