Targeted synthesis of a large triazine-based [4+6] organic molecular cage: structure, porosity and gas separation
Huimin Ding; Yihui Yang; Bijian Li; Feng Pan; Guozhu Zhu; Matthias Zeller; Daqiang Yuan; Cheng Wang; Chem.Commun. 51 (2015) 1976–; doi:10.1039/C4cc08883B

data_7116438
_publ_section_title
;
 Targeted synthesis of a large triazine-based [4+6] organic molecular
 cage: structure, porosity and gas separation
;
_journal_name_full               Chem.Commun.
_journal_page_first              1976
_journal_paper_doi               10.1039/C4cc08883B
_journal_volume                  51
_journal_year                    2015
_chemical_absolute_configuration unk
_chemical_formula_sum            'C132 H120 N24'
_chemical_formula_weight         2042.51
_space_group_crystal_system      orthorhombic
_space_group_IT_number           19
_space_group_name_Hall           'P 2ac 2ab'
_space_group_name_H-M_alt        'P 21 21 21'
_symmetry_space_group_name_Hall  'P 2ac 2ab'
_symmetry_space_group_name_H-M   'P 21 21 21'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014
_audit_update_record
;
2014-09-01 deposited with the CCDC.
2014-12-16 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   23.855(5)
_cell_length_b                   26.655(5)
_cell_length_c                   27.082(5)
_cell_measurement_reflns_used    149926
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.44
_cell_measurement_theta_min      0.45
_cell_volume                     17220(6)
_computing_cell_refinement       'HKL2000 (Z. Otwinowski and W. Minor, 1997)'
_computing_data_collection
; 
marccd, control software for MarCCD-165 detector
;
_computing_data_reduction        'HKL2000 (Z. Otwinowski and W. Minor, 1997)'
_computing_structure_refinement
;  
SHELXL-2014 (Sheldrick, 2014), 
SHELXLE Rev609 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXD / XM (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.745
_diffrn_measured_fraction_theta_max 0.767
_diffrn_measurement_device_type
; 
Beijing Synchrotron Radiation Facility, beam line station 
3W1A equipped with a MarCCD-165 detector (the monochrome 
x-ray source is produced by accelerator and selected by 
a double crystal monochromator)
;
_diffrn_measurement_method       'omega and phi scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.800
_diffrn_reflns_av_R_equivalents  0.0243
_diffrn_reflns_av_unetI/netI     0.0427
_diffrn_reflns_Laue_measured_fraction_full 0.745
_diffrn_reflns_Laue_measured_fraction_max 0.767
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       0
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            40104
_diffrn_reflns_point_group_measured_fraction_full 0.707
_diffrn_reflns_point_group_measured_fraction_max 0.728
_diffrn_reflns_theta_full        28.685
_diffrn_reflns_theta_max         28.381
_diffrn_reflns_theta_min         1.917
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    0.061
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.788
_exptl_crystal_description       rod
_exptl_crystal_F_000             4320
_exptl_crystal_size_max          0.300
_exptl_crystal_size_mid          0.200
_exptl_crystal_size_min          0.050
_refine_diff_density_max         0.185
_refine_diff_density_min         -0.187
_refine_diff_density_rms         0.042
_refine_ls_extinction_coef       0.0022(3)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     SHELXL
_refine_ls_goodness_of_fit_ref   0.958
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1406
_refine_ls_number_reflns         22034
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.958
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0603
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1217P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1583
_refine_ls_wR_factor_ref         0.1734
_reflns_Friedel_coverage         0.772
_reflns_Friedel_fraction_full    0.663
_reflns_Friedel_fraction_max     0.683
_reflns_number_gt                15201
_reflns_number_total             22034
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc08883b2.cif
_cod_data_source_block           Cage-1
_cod_database_code               7116438
_shelx_estimated_absorpt_t_min   0.982
_shelx_estimated_absorpt_t_max   0.997
_shelxl_version_number           2014-3
_shelx_res_checksum              64440
_shelx_hkl_checksum              50581