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_4110862
_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            'C120 H104 N8 O16 P4 Ti2'
_chemical_formula_weight         2133.79
_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                105.879(4)
_cell_angle_beta                 100.689(4)
_cell_angle_gamma                110.322(4)
_cell_formula_units_Z            1
_cell_length_a                   14.038(3)
_cell_length_b                   15.014(3)
_cell_length_c                   15.241(3)
_cell_measurement_reflns_used    900
_cell_measurement_temperature    153(2)
_cell_measurement_theta_max      22.5
_cell_measurement_theta_min      1
_cell_volume                     2753.7(10)
_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 0.999
_diffrn_measured_fraction_theta_max 0.999
_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  0.1019
_diffrn_reflns_av_sigmaI/netI    0.1501
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19230
_diffrn_reflns_theta_full        23.50
_diffrn_reflns_theta_max         23.50
_diffrn_reflns_theta_min         1.46
_exptl_absorpt_coefficient_mu    0.272
_exptl_absorpt_correction_T_max  0.9946
_exptl_absorpt_correction_T_min  0.9681
_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 = 0.796373  

;
_exptl_crystal_colour            red-brown
_exptl_crystal_density_diffrn    1.287
_exptl_crystal_description       'transparent plates'
_exptl_crystal_F_000             1112
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         1.432
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.091
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    noref
_refine_ls_matrix_type           full
_refine_ls_number_parameters     681
_refine_ls_number_reflns         8128
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.977
_refine_ls_R_factor_all          0.1717
_refine_ls_R_factor_gt           0.0877
_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^)+(0.1442P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2141
_refine_ls_wR_factor_ref         0.2654
_reflns_number_gt                4124
_reflns_number_total             8128
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja063655usi20060605_060949.cif
_cod_data_source_block           sad_complex_(PNP)2(17)x3MeOH
_cod_original_cell_volume        2753.8(10)
_cod_database_code               4110862