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_7108453
_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 N36 Ni4 O10 S'
_chemical_formula_weight         3022.03
_space_group_IT_number           147
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  '-P 3'
_symmetry_space_group_name_H-M   'P -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                120.00
_cell_formula_units_Z            2
_cell_length_a                   25.0734(12)
_cell_length_b                   25.0734(12)
_cell_length_c                   19.3734(9)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    100
_cell_measurement_theta_max      22.23
_cell_measurement_theta_min      2.30
_cell_volume                     10547.8(9)
_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 1.000
_diffrn_measured_fraction_theta_max 1.000
_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  0.0589
_diffrn_reflns_av_sigmaI/netI    0.0428
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            84637
_diffrn_reflns_theta_full        25.00
_diffrn_reflns_theta_max         25.00
_diffrn_reflns_theta_min         1.41
_exptl_absorpt_coefficient_mu    0.413
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6071
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   '(SADABS 2007/4 Bruker)'
_exptl_crystal_colour            Orange
_exptl_crystal_density_diffrn    0.952
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       Block
_exptl_crystal_F_000             3152
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.26
_exptl_crystal_size_min          0.04
_platon_squeeze_details
; The packing of the molecules of cage 4, 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
4213.6 3, or 39.9.2% of the total unit cell volume, corresponding
to 1237 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, sulfate) what was removed by the SQUEEZE process.
;
_refine_diff_density_max         0.655
_refine_diff_density_min         -0.539
_refine_diff_density_rms         0.066
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.013
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     640
_refine_ls_number_reflns         12393
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0832
_refine_ls_R_factor_gt           0.0593
_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^)+(0.1145P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1634
_refine_ls_wR_factor_ref         0.1754
_reflns_number_gt                8761
_reflns_number_total             12393
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            c2cc35095e.txt
_cod_data_source_block           squeeze_Ni4_Td_Cage(Rev)
_cod_original_sg_symbol_H-M      P-3
_cod_database_code               7108453