Triply interlocked covalent organic cages.
Hasell, Tom; Wu, Xiaofeng; Jones, James T. A.; Bacsa, John; Steiner, Alexander; Mitra, Tamoghna; Trewin, Abbie; Adams, Dave J.; Cooper, Andrew I.; Nature chemistry 2 (2010) 750–755; doi:10.1038/nchem.739

data_1508093
_publ_section_title
;
 Triply interlocked covalent organic cages.
;
_journal_issue                   9
_journal_name_full               'Nature chemistry'
_journal_page_first              750
_journal_page_last               755
_journal_paper_doi               10.1038/nchem.739
_journal_volume                  2
_journal_year                    2010
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C66 H72 N12, 7.5(C H2 CL2)'
_chemical_formula_sum            'C73.5 H87 Cl15 N12'
_chemical_formula_weight         1670.30
_chemical_name_common            cage3b-catenane
_chemical_name_systematic
;
 ?
;
_space_group_IT_number           20
_symmetry_cell_setting           orthorhombic
_symmetry_space_group_name_Hall  'C 2c 2'
_symmetry_space_group_name_H-M   'C 2 2 21'
_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            8
_cell_length_a                   16.861(3)
_cell_length_b                   32.059(6)
_cell_length_c                   29.480(6)
_cell_measurement_reflns_used    6231
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      22.1407
_cell_measurement_theta_min      2.36
_cell_volume                     15935(5)
_computing_cell_refinement       'SAINT v6.45a (Bruker, 2005)'
_computing_data_collection       'SMART v.5.632 (Bruker, 2005)'
_computing_data_reduction        'SAINT v6.45a (Bruker, 2005)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.991
_diffrn_measurement_device_type  'Bruker D8 diffractometer with APEX detector'
_diffrn_measurement_method       '\w scans with a narrow frame width'
_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  0.0982
_diffrn_reflns_av_sigmaI/netI    0.1348
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       29
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            31493
_diffrn_reflns_theta_full        23.38
_diffrn_reflns_theta_max         23.38
_diffrn_reflns_theta_min         1.38
_exptl_absorpt_coefficient_mu    0.568
_exptl_absorpt_correction_T_max  0.9454
_exptl_absorpt_correction_T_min  0.7645
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2008-1 (Sheldrick, 2008)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             6936
_exptl_crystal_size_max          0.50
_exptl_crystal_size_mid          0.20
_exptl_crystal_size_min          0.10
_platon_squeeze_details
;
 The catenane was crystallised in CH2Cl2.  The initial structure 
 solution contained an ordered cage molecule and partially ordered
 CH2Cl2 molecules.  Five CH2Cl2 molecules could be placed and their
 coordinates refined.  It was clear from the difference maps that
 significant electron density was still present, but that it was too
 diffuse to be modelled as CH2Cl2 molecules. PLATON/SQUEEZE 
 calculates 4 large solvent voids in the unit cell, volume = 
 997 A^3^ with 442 electrons for each void, corresponding to exactly
 10 CH2Cl2 molecules each.

;
_refine_diff_density_max         0.586
_refine_diff_density_min         -0.582
_refine_diff_density_rms         0.092
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.28(14)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.001
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     778
_refine_ls_number_reflns         11417
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.001
_refine_ls_R_factor_all          0.1267
_refine_ls_R_factor_gt           0.1006
_refine_ls_shift/su_max          0.008
_refine_ls_shift/su_mean         0.001
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'calc w=1/[\s^2^(Fo^2^)+(0.1748P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2551
_refine_ls_wR_factor_ref         0.2815
_reflns_number_gt                7620
_reflns_number_total             11417
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            nchem.739-s3.cif
_cod_data_source_block           cage3b-catenane
_cod_depositor_comments
;

2019-05-07
Z value and formula fixed to values more according to usual
chemical conventions.                 miguel
;
_cod_original_formula_sum            'C147 H174 Cl30 N24'
_cod_original_formula_weight         3340.60
_cod_original_formula_moiety         '2(C66 H72 N12), 15(C H2 CL2)'
_cod_original_formula_units_Z            4
_cod_original_sg_symbol_H-M      C2221
_cod_database_code               1508093