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_4106954
_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 ad
_chemical_formula_sum            'C124.5 H89.5 Cl13.5 F12 N12 O0.5'
_chemical_formula_weight         2468.16
_chemical_name_systematic
; 
 ? 
;
_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            6
_cell_length_a                   30.587(2)
_cell_length_b                   30.587(2)
_cell_length_c                   21.553(2)
_cell_measurement_reflns_used    7609
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.50
_cell_measurement_theta_min      2.24
_cell_volume                     17463(2)
_computing_cell_refinement       'Bruker AXS SAINT V7.68A'
_computing_data_collection
;
CrystalClear-SM Expert 2.0 r6 (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      100(2)
_diffrn_detector                 CCD
_diffrn_detector_area_resol_mean 28.5714
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device
;
AFC12 (Right): Kappa 3 circle
;
_diffrn_measurement_device_type
;
Rigaku Saturn724+ (2x2 bin mode)
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_monochromator  Confocal
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0794
_diffrn_reflns_av_sigmaI/netI    0.0819
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_k_min       -32
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            45224
_diffrn_reflns_theta_full        23.25
_diffrn_reflns_theta_max         23.25
_diffrn_reflns_theta_min         2.04
_diffrn_source                   'Rotating Anode'
_diffrn_source_current           24.0
_diffrn_source_power             1.2
_diffrn_source_voltage           50.0
_exptl_absorpt_coefficient_mu    0.395
_exptl_absorpt_correction_T_max  1.0000
_exptl_absorpt_correction_T_min  0.6543
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS 2008/1 (Sheldrick, 2008)'
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.408
_exptl_crystal_description       plate
_exptl_crystal_F_000             7572
_exptl_crystal_size_max          0.12
_exptl_crystal_size_mid          0.10
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.934
_refine_diff_density_min         -0.620
_refine_diff_density_rms         0.102
_refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881'
_refine_ls_abs_structure_Flack   0.04(10)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.249
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     980
_refine_ls_number_reflns         11108
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.249
_refine_ls_R_factor_all          0.1229
_refine_ls_R_factor_gt           0.0828
_refine_ls_shift/su_max          0.000
_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^+40.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2118
_refine_ls_wR_factor_ref         0.2298
_reflns_number_gt                7689
_reflns_number_total             11108
_reflns_threshold_expression     >2sigma(I)
_cod_data_source_file            ja2056374_si_005.cif
_cod_data_source_block           marf
_cod_original_cell_volume        17462(2)
_cod_original_sg_symbol_H-M      'R 3'
_cod_original_formula_sum        'C124.50 H89.50 Cl13.50 F12 N12 O0.50'
_cod_database_code               4106954