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_4110859
_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            'C165 H149 Li N12 O10 P6 S12 Ti2'
_chemical_formula_weight         3133.24
_chemical_name_systematic
; 
 ? 
;
_space_group_IT_number           14
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-P 2ybc'
_symmetry_space_group_name_H-M   'P 1 21/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                 99.417(2)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   17.8522(4)
_cell_length_b                   23.0986(5)
_cell_length_c                   37.9215(9)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      75
_cell_measurement_theta_min      1
_cell_volume                     15426.6(6)
_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      150(2)
_diffrn_detector_area_resol_mean 80
_diffrn_measured_fraction_theta_full 0.947
_diffrn_measured_fraction_theta_max 0.947
_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     1.54184
_diffrn_reflns_av_R_equivalents  0.0776
_diffrn_reflns_av_sigmaI/netI    0.0829
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -28
_diffrn_reflns_limit_l_max       46
_diffrn_reflns_limit_l_min       -46
_diffrn_reflns_number            89879
_diffrn_reflns_theta_full        70.16
_diffrn_reflns_theta_max         70.16
_diffrn_reflns_theta_min         2.36
_exptl_absorpt_coefficient_mu    3.495
_exptl_absorpt_correction_T_max  0.7920
_exptl_absorpt_correction_T_min  0.2740
_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 
  Maximum and minimum effective transmission:  1.000000  0.562509

;
_exptl_crystal_colour            'dark red'
_exptl_crystal_density_diffrn    1.349
_exptl_crystal_description       'transparent needles'
_exptl_crystal_F_000             6528
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.07
_refine_diff_density_max         1.737
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.092
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.938
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           fullcycle
_refine_ls_number_parameters     1922
_refine_ls_number_reflns         27800
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.938
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0522
_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^)+(0.0794P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1330
_refine_ls_wR_factor_ref         0.1427
_reflns_number_gt                18674
_reflns_number_total             27800
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja063655usi20060605_060834.cif
_cod_data_source_block           sad_complex_Li(PNP)3(13)x3DMFxH2O
_cod_database_code               4110859