A metallosupramolecular tetrahedron with a huge internal cavity
Albrecht, Markus; Janser, Ingo; Meyer, Sebastian; Weis, Patrick; Fröhlich, Roland; Chemical Communications  (2003) 2854–2855; doi:10.1039/b309495b

data_7113802
_publ_section_title
;
 A metallosupramolecular tetrahedron with a huge internal cavity
;
_journal_issue                   23
_journal_name_full               'Chemical Communications'
_journal_page_first              2854
_journal_page_last               2855
_journal_paper_doi               10.1039/b309495b
_journal_year                    2003
_chemical_formula_sum            'C225 H257 K8 N39 O47 Ti4'
_chemical_formula_weight         4764.10
_space_group_IT_number           15
_symmetry_cell_setting           monoclinic
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/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                 123.79(1)
_cell_angle_gamma                90.00
_cell_formula_units_Z            4
_cell_length_a                   35.628(1)
_cell_length_b                   32.922(1)
_cell_length_c                   26.300(1)
_cell_measurement_temperature    198(2)
_cell_volume                     25638(3)
_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 0.973
_diffrn_measured_fraction_theta_max 0.973
_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  0.0844
_diffrn_reflns_av_sigmaI/netI    0.0907
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -38
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            44276
_diffrn_reflns_theta_full        22.50
_diffrn_reflns_theta_max         22.50
_diffrn_reflns_theta_min         1.69
_exptl_absorpt_coefficient_mu    0.326
_exptl_absorpt_correction_T_max  0.9682
_exptl_absorpt_correction_T_min  0.9086
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'SORTAV (Blessing, 1995 & 1997)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.234
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9984
_exptl_crystal_size_max          0.30
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_refine_diff_density_max         1.587
_refine_diff_density_min         -1.104
_refine_diff_density_rms         0.136
_refine_ls_extinction_coef       0.00054(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   1.992
_refine_ls_hydrogen_treatment    'refined as riding atoms'
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1291
_refine_ls_number_reflns         16324
_refine_ls_number_restraints     168
_refine_ls_restrained_S_all      2.047
_refine_ls_R_factor_all          0.1908
_refine_ls_R_factor_gt           0.1288
_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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3235
_refine_ls_wR_factor_ref         0.3515
_reflns_number_gt                9559
_reflns_number_total             16324
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            b309495b.txt
_cod_data_source_block           fro2276
_cod_original_cell_volume        25637.6(14)
_cod_original_sg_symbol_H-M      C2/c
_cod_database_code               7113802