Hierarchical Assembly of Helicate-Type Dinuclear Titanium(IV) Complexes
Markus Albrecht; Sebastian Mirtschin; Marita de Groot; Ingo Janser; Jan Runsink; Gerhard Raabe; Michael Kogej; Christoph A. Schalley; Roland Fröhlich; Journal of the American Chemical Society 127 (2005) 10371–10387; doi:10.1021/ja052326j

data_4111817
_publ_contact_author
;
        Prof. Dr. Markus Albrecht
        Institut f\"ur Organische Chemie
        RWTH Aachen
        Landoltweg 1
        D-52074 Aachen
        Germany
;
_publ_contact_author_email       markus.albrecht@oc.rwth-aachen.de
_publ_contact_author_fax         '49 241 809 2385'
_publ_contact_author_phone       '49 241 809 4678'
_publ_section_title
;
 Hierarchical Assembly of Helicate-Type Dinuclear Titanium(IV) Complexes
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              10371
_journal_page_last               10387
_journal_paper_doi               10.1021/ja052326j
_journal_volume                  127
_journal_year                    2005
_chemical_formula_sum            'C60 H66 Li4 N4 O29 Ti2'
_chemical_formula_weight         1430.72
_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                 108.38(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   14.530(1)
_cell_length_b                   21.692(1)
_cell_length_c                   22.298(1)
_cell_measurement_temperature    198(2)
_cell_volume                     6669.5(7)
_computing_cell_refinement       'Collect (Nonius B.V., 1998)'
_computing_data_collection       'Collect (Nonius B.V., 1998)'
_computing_data_reduction        'Denzo-SMN (Otwinowski & Minor, 1997)'
_computing_molecular_graphics    'SCHAKAL (Keller, 1997)'
_computing_publication_material  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      198(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Nonius KappaCCD'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'rotating anode Nonius FR591'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0807
_diffrn_reflns_av_sigmaI/netI    0.0814
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            38983
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         2.14
_exptl_absorpt_coefficient_mu    0.329
_exptl_absorpt_correction_T_max  0.9838
_exptl_absorpt_correction_T_min  0.8797
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995 & 1997)'
_exptl_crystal_colour            orange
_exptl_crystal_density_diffrn    1.425
_exptl_crystal_description       plate
_exptl_crystal_F_000             2968
_exptl_crystal_size_max          0.40
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.05
_refine_diff_density_max         1.656
_refine_diff_density_min         -0.749
_refine_diff_density_rms         0.094
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    riding
_refine_ls_matrix_type           full
_refine_ls_number_parameters     854
_refine_ls_number_reflns         11730
_refine_ls_number_restraints     8
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1379
_refine_ls_R_factor_gt           0.0872
_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^)+(0.1304P)^2^+17.2861P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2291
_refine_ls_wR_factor_ref         0.2629
_reflns_number_gt                7368
_reflns_number_total             11730
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja052326jsi20050419_054020_3.cif
_cod_data_source_block           fro3123
_cod_original_cell_volume        6669.5(6)
_cod_original_sg_symbol_H-M      P21/c
_cod_database_code               4111817