Sulfate-templated self-assembly of new M4L6 tetrahedral metal organic cages
Song Yi; Valentina Brega; Burjor Captain; Angel E. Kaifer; Chem.Commun. 48 (2012) 10295–; doi:10.1039/c2cc35095e

data_7108452
_publ_section_title
;
 Sulfate-templated self-assembly of new M4L6 tetrahedral metal organic
 cages
;
_journal_name_full               Chem.Commun.
_journal_page_first              10295
_journal_paper_doi               10.1039/c2cc35095e
_journal_volume                  48
_journal_year                    2012
_chemical_formula_sum            'C162 H144 Fe4 N36 O22 S4'
_chemical_formula_weight         3298.77
_chemical_name_systematic
;
?
;
_space_group_IT_number           197
_symmetry_cell_setting           cubic
_symmetry_space_group_name_Hall  'I 2 2 3'
_symmetry_space_group_name_H-M   'I 2 3'
_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                 90.00
_cell_angle_gamma                90.00
_cell_formula_units_Z            2
_cell_length_a                   22.1233(8)
_cell_length_b                   22.1233(8)
_cell_length_c                   22.1233(8)
_cell_measurement_reflns_used    9921
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.37
_cell_measurement_theta_min      2.25
_cell_volume                     10828.0(7)
_computing_cell_refinement       'SAINT+ V7.46A (Bruker, 2007)'
_computing_data_collection       'APEX2 v2.2-0 (Bruker, 2007)'
_computing_data_reduction        'SAINT+ V7.46A (Bruker, 2007)'
_computing_molecular_graphics    'XSHELL v4.02 (Bruker, 2000)'
_computing_publication_material  'XCIF v6.12 (Bruker, 2001)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker SMART APEX2 CCD diffractometer'
_diffrn_measurement_method       'omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0402
_diffrn_reflns_av_sigmaI/netI    0.0177
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            44282
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.84
_exptl_absorpt_coefficient_mu    0.359
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6689
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS 2007/4 Bruker)'
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.012
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3424
_exptl_crystal_size_max          0.42
_exptl_crystal_size_mid          0.36
_exptl_crystal_size_min          0.20
_platon_squeeze_details
;During the final stages of refinement the packing of the molecules of
cage 3, generates large cavities that are filled with disordered molecules
from the solvent of crystallization. No reasonable disorder model could be
obtained for these molecules despite many attempts. They were therefore
accounted for by the SQUEEZE/PLATON program. The program calculated a total
solvent-accessible volume per unit cell of 2619.5 3, or 24.2% of the total
unit cell volume, corresponding to 878 e-/cell. The contribution of these
diffusely scattering species was removed from the structure factor calculations.
The tabulated F(000), MW and density reflect the known unit cell contents only.
It is not possible to estimate with any confidence (water, dioxane) what was
removed by the SQUEEZE process.
;
_refine_diff_density_max         0.506
_refine_diff_density_min         -0.563
_refine_diff_density_rms         0.107
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.23(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.109
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     182
_refine_ls_number_reflns         3202
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.117
_refine_ls_R_factor_all          0.0802
_refine_ls_R_factor_gt           0.0778
_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^)+(0.1719P)^2^+4.4057P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2187
_refine_ls_wR_factor_ref         0.2216
_reflns_number_gt                2985
_reflns_number_total             3202
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc35095e.txt
_cod_data_source_block           squeeze_Fe4_Td_Cage(Rev)
_cod_original_sg_symbol_H-M      I23
_cod_database_code               7108452