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_4304754
_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         'C68 H56 N7 O4 P2 Re'
_chemical_formula_sum            'C68 H56 N7 O4 P2 Re'
_chemical_formula_weight         1283.34
_chemical_name_systematic
;
Bis(5,6-diphenyl-1,2,4-triazine-3-ketonato)bis(triphenylphosphine)-
nitridorhenium(V) ethanol/water solvate
;
_space_group_IT_number           19
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_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                   12.227(1)
_cell_length_b                   20.482(1)
_cell_length_c                   26.183(1)
_cell_measurement_reflns_used    43416
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.13
_cell_measurement_theta_min      2.09
_cell_volume                     6557.1(7)
_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 0.991
_diffrn_measured_fraction_theta_max 0.991
_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  0.0996
_diffrn_reflns_av_sigmaI/netI    0.0815
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       33
_diffrn_reflns_limit_l_min       -33
_diffrn_reflns_number            13926
_diffrn_reflns_theta_full        26.83
_diffrn_reflns_theta_max         26.83
_diffrn_reflns_theta_min         1.56
_exptl_absorpt_coefficient_mu    1.952
_exptl_absorpt_correction_T_max  .7451
_exptl_absorpt_correction_T_min  .5052
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE XABS'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.300
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             2600
_exptl_crystal_size_max          .25
_exptl_crystal_size_mid          .20
_exptl_crystal_size_min          .15
_refine_diff_density_max         1.293
_refine_diff_density_min         -1.289
_refine_diff_density_rms         0.310
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -0.002(8)
_refine_ls_extinction_coef       0.0112(4)
_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   0.905
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     755
_refine_ls_number_reflns         13926
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.905
_refine_ls_R_factor_all          0.0670
_refine_ls_R_factor_gt           0.0485
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.0949P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1168
_refine_ls_wR_factor_ref         0.1343
_reflns_number_gt                11212
_reflns_number_total             13926
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic702326v-file007_3.cif
_cod_data_source_block           ren(ON)2(PPh3)2
_cod_original_cell_volume        6557.3(7)
_cod_database_code               4304754