Bipodal Acylthiourea Ligands as Building Blocks for Bi-, Tetra-, and Polynuclear Oxorhenium(V) Complexes
Hung Huy Nguyen; Pham Chien Thang; Axel Rodenstein; Reinhard Kirmse; Ulrich Abram; Inorganic Chemistry 50 (2011) 590–596; doi:10.1021/ic1017642

data_4324231
_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
;
 Bipodal Acylthiourea Ligands as Building Blocks for Bi-, Tetra-, and
 Polynuclear Oxorhenium(V) Complexes
;
_journal_name_full               'Inorganic Chemistry'
_journal_page_first              590
_journal_page_last               596
_journal_paper_doi               10.1021/ic1017642
_journal_volume                  50
_journal_year                    2011
_chemical_formula_moiety         'C41 H54 Cl6 N8 O8 Re2 S4'
_chemical_formula_sum            'C41 H54 Cl6 N8 O8 Re2 S4'
_chemical_formula_weight         1500.26
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 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                 96.568(10)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   27.3356(10)
_cell_length_b                   8.2458(10)
_cell_length_c                   25.0206(10)
_cell_measurement_reflns_used    22118
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      27.30
_cell_measurement_theta_min      2.09
_cell_volume                     5602.7(8)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_computing_molecular_graphics    ORTEP3
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1997)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 6.67
_diffrn_measured_fraction_theta_full 0.976
_diffrn_measured_fraction_theta_max 0.976
_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  0.0629
_diffrn_reflns_av_sigmaI/netI    0.0466
_diffrn_reflns_limit_h_max       34
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            14446
_diffrn_reflns_theta_full        26.88
_diffrn_reflns_theta_max         26.88
_diffrn_reflns_theta_min         1.50
_diffrn_standards_decay_%        0.5
_exptl_absorpt_coefficient_mu    4.806
_exptl_absorpt_correction_T_max  0.6276
_exptl_absorpt_correction_T_min  0.2339
_exptl_absorpt_correction_type   integration
_exptl_absorpt_process_details   'STOE X-RED'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.779
_exptl_crystal_description       block
_exptl_crystal_F_000             2944
_exptl_crystal_size_max          0.200
_exptl_crystal_size_mid          0.133
_exptl_crystal_size_min          0.100
_refine_diff_density_max         5.438
_refine_diff_density_min         -2.419
_refine_diff_density_rms         0.455
_refine_ls_extinction_coef       0.00091(10)
_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   0.929
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     313
_refine_ls_number_reflns         5904
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.929
_refine_ls_R_factor_all          0.0590
_refine_ls_R_factor_gt           0.0474
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1333P)^2^+15.8939P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1401
_refine_ls_wR_factor_ref         0.1582
_reflns_number_gt                5104
_reflns_number_total             5904
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ic1017642_si_002_2.cif
_cod_data_source_block           hnlepet
_cod_original_cell_volume        5602.7(7)
_cod_database_code               4324231