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_4110861
_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            'C102 H98 As2 N8 O10 S8 Ti2'
_chemical_formula_weight         2098.00
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           2
_symmetry_cell_setting           triclinic
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-97
_cell_angle_alpha                80.544(2)
_cell_angle_beta                 76.820(2)
_cell_angle_gamma                85.068(3)
_cell_formula_units_Z            1
_cell_length_a                   8.4004(10)
_cell_length_b                   16.4984(19)
_cell_length_c                   17.952(2)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      1
_cell_volume                     2386.5(5)
_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      153(2)
_diffrn_detector_area_resol_mean 80
_diffrn_measured_fraction_theta_full 0.985
_diffrn_measured_fraction_theta_max 0.985
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'Omega and Phi scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0399
_diffrn_reflns_av_sigmaI/netI    0.0747
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            28266
_diffrn_reflns_theta_full        30.08
_diffrn_reflns_theta_max         30.08
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    1.095
_exptl_absorpt_correction_T_max  0.9372
_exptl_absorpt_correction_T_min  0.7868
_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 = 0.875136  

;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.460
_exptl_crystal_description       'transparent needles'
_exptl_crystal_F_000             1084
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.06
_exptl_crystal_size_min          0.06
_refine_diff_density_max         0.798
_refine_diff_density_min         -0.459
_refine_diff_density_rms         0.083
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.007
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     608
_refine_ls_number_reflns         13819
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0746
_refine_ls_R_factor_gt           0.0464
_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^)+(0.0489P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1013
_refine_ls_wR_factor_ref         0.1107
_reflns_number_gt                9875
_reflns_number_total             13819
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja063655usi20060605_060923.cif
_cod_data_source_block           sad_complex_(Ph4As)4(16)x4DMF
_cod_original_cell_volume        2386.6(5)
_cod_database_code               4110861