Metallosupramolecular Chemistry with Bis(benzene-o-dithiolato) Ligands
Thorsten Kreickmann; Christian Diedrich; Tania Pape; Han Vinh Huynh; Stefan Grimme; F. Ekkehardt Hahn; Journal of the American Chemical Society 128 (2006) 11808–11819; doi:10.1021/ja063655u

data_4110860
_publ_section_title
;
 Metallosupramolecular Chemistry with Bis(benzene-o-dithiolato) Ligands
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              11808
_journal_page_last               11819
_journal_paper_doi               10.1021/ja063655u
_journal_volume                  128
_journal_year                    2006
_chemical_formula_sum            'C213 H177 N13 O9 P8 S12 Ti2'
_chemical_formula_weight         3790.96
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           167
_symmetry_cell_setting           hexagonal
_symmetry_space_group_name_Hall  '-R 3 2"c'
_symmetry_space_group_name_H-M   'R -3 c :H'
_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                120.00
_cell_formula_units_Z            12
_cell_length_a                   24.5457(16)
_cell_length_b                   24.5457(16)
_cell_length_c                   112.885(10)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      75
_cell_measurement_theta_min      1
_cell_volume                     58900(8)
_computing_cell_refinement       'SAINT (Bruker AXS, 2000)'
_computing_data_collection       'SMART (Bruker AXS, 2000)'
_computing_data_reduction        'SAINT,SADABS (Bruker AXS, 2000)'
_computing_molecular_graphics
;
ORTEP3,L.J. Farrugia, J. Appl. Cryst. (1997) 30, 565
;
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 80
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  goebel-mirror
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1254
_diffrn_reflns_av_sigmaI/netI    0.0904
_diffrn_reflns_limit_h_max       20
_diffrn_reflns_limit_h_min       -28
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       135
_diffrn_reflns_limit_l_min       -132
_diffrn_reflns_number            88221
_diffrn_reflns_theta_full        70.05
_diffrn_reflns_theta_max         70.05
_diffrn_reflns_theta_min         2.22
_exptl_absorpt_coefficient_mu    2.989
_exptl_absorpt_correction_T_max  0.6796
_exptl_absorpt_correction_T_min  0.3963
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
 Corrections were done with the SADABS program, utilizing the none merged
 raw data obtained from the integration process. Integration and final cell
 refinement were done with SAINT.

 SADABS reports ratio of Tmin/Tmax = 0.586172  

;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.283
_exptl_crystal_description       prism
_exptl_crystal_F_000             23688
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.14
_refine_diff_density_max         1.723
_refine_diff_density_min         -0.723
_refine_diff_density_rms         0.130
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.040
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     786
_refine_ls_number_reflns         12393
_refine_ls_number_restraints     21
_refine_ls_restrained_S_all      1.041
_refine_ls_R_factor_all          0.1258
_refine_ls_R_factor_gt           0.0886
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1677P)^2^+219.9603P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2439
_refine_ls_wR_factor_ref         0.2790
_reflns_number_gt                8245
_reflns_number_total             12393
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja063655usi20060605_060856.cif
_cod_data_source_block           sad_complex_(PNP)4(14)x3DMF
_cod_original_cell_volume        58900(7)
_cod_original_sg_symbol_H-M      'R -3 c'
_cod_database_code               4110860