Supramolecular Engineering of Intrinsic and Extrinsic Porosity in Covalent Organic Cages
Michael J. Bojdys; Michael E. Briggs; James T. A. Jones; Dave J. Adams; Samantha Y. Chong; Marc Schmidtmann; Andrew I. Cooper; Journal of the American Chemical Society 133 (2011) 16566–16571; doi:10.1021/ja2056374

data_4106952
_publ_section_title
;
 Supramolecular Engineering of Intrinsic and Extrinsic Porosity in
 Covalent Organic Cages
;
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              16566
_journal_page_last               16571
_journal_paper_doi               10.1021/ja2056374
_journal_volume                  133
_journal_year                    2011
_chemical_absolute_configuration syn
_chemical_formula_sum            'C120 H96 N12'
_chemical_formula_weight         1706.09
_space_group_IT_number           146
_symmetry_cell_setting           trigonal
_symmetry_space_group_name_Hall  'R 3'
_symmetry_space_group_name_H-M   'R 3 :H'
_atom_sites_solution_hydrogens   difmap
_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            3
_cell_length_a                   29.494(5)
_cell_length_b                   29.494(5)
_cell_length_c                   11.036(3)
_cell_measurement_reflns_used    3303
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      17.78
_cell_measurement_theta_min      2.32
_cell_volume                     8314(3)
_computing_cell_refinement       'Bruker AXS SAINT V7.68A'
_computing_data_collection       'CrystalClear-SM Expert 2.0r6 (Rigaku, 2010)'
_computing_data_reduction        'Bruker AXS SAINT V7.68A'
_computing_structure_refinement  'SHELXL (Sheldrick, 2008)'
_computing_structure_solution    'SHELXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      298(2)
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device
;
CrystalLogic Kappa (3 circle)
;
_diffrn_measurement_device_type  'Rigaku Saturn724+ (2x2 bin mode)'
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_source         Synchrotron
_diffrn_radiation_wavelength     0.68890
_diffrn_reflns_av_R_equivalents  0.0588
_diffrn_reflns_av_sigmaI/netI    0.0522
_diffrn_reflns_limit_h_max       29
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            17139
_diffrn_reflns_theta_full        20.14
_diffrn_reflns_theta_max         20.14
_diffrn_reflns_theta_min         1.95
_exptl_absorpt_coefficient_mu    0.060
_exptl_absorpt_correction_T_max  0.7445
_exptl_absorpt_correction_T_min  0.6409
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Sheldrick, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.022
_exptl_crystal_description       needle
_exptl_crystal_F_000             2700
_exptl_crystal_size_max          0.10
_exptl_crystal_size_mid          0.01
_exptl_crystal_size_min          0.01
_refine_diff_density_max         0.081
_refine_diff_density_min         -0.082
_refine_diff_density_rms         0.018
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   -4(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.986
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     397
_refine_ls_number_reflns         3878
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      0.986
_refine_ls_R_factor_all          0.0867
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0400P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0807
_refine_ls_wR_factor_ref         0.0947
_reflns_number_gt                2448
_reflns_number_total             3878
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2056374_si_003.cif
_cod_data_source_block           mjr0853
_cod_original_sg_symbol_H-M      'R 3'
_cod_database_code               4106952