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_4304756
_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         'C50 H50 N7 P2 Re S2'
_chemical_formula_sum            'C50 H50 N7 P2 Re S2'
_chemical_formula_weight         1061.23
_chemical_name_common            '[ReNL1)2(PEt2PhP)2]'
_chemical_name_systematic
;
Bis(diethylphenylphosphine)bis(5,6-diphenyl-1,2,4-triazine-3-thionato)-
nitridorhenium(V)
;
_space_group_IT_number           76
_symmetry_cell_setting           tetragonal
_symmetry_space_group_name_Hall  'P 4w'
_symmetry_space_group_name_H-M   'P 41'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   12.387(2)
_cell_length_b                   12.387(2)
_cell_length_c                   30.963(2)
_cell_measurement_reflns_used    23683
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      29.35
_cell_measurement_theta_min      2.56
_cell_volume                     4750.9(11)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_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_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.990
_diffrn_measured_fraction_theta_max 0.990
_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  0.1351
_diffrn_reflns_av_sigmaI/netI    0.1299
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       42
_diffrn_reflns_limit_l_min       -42
_diffrn_reflns_number            51670
_diffrn_reflns_theta_full        29.26
_diffrn_reflns_theta_max         29.26
_diffrn_reflns_theta_min         2.57
_diffrn_standards_decay_%        .1
_exptl_absorpt_coefficient_mu    2.755
_exptl_absorpt_correction_T_max  .7745
_exptl_absorpt_correction_T_min  .6464
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED32'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    1.484
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2144
_exptl_crystal_size_max          .2
_exptl_crystal_size_mid          .167
_exptl_crystal_size_min          .150
_refine_diff_density_max         1.279
_refine_diff_density_min         -1.768
_refine_diff_density_rms         0.131
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.018(7)
_refine_ls_extinction_coef       0.00079(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.885
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     533
_refine_ls_number_reflns         12783
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.885
_refine_ls_R_factor_all          0.0853
_refine_ls_R_factor_gt           0.0468
_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^)+(0.0224P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0782
_refine_ls_wR_factor_ref         0.0890
_reflns_number_gt                8699
_reflns_number_total             12783
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702326v-file007_5.cif
_cod_data_source_block           ren(NS)2(et2php)2
_cod_database_code               4304756