Examination of the Dynamic Covalent Chemistry of [2 + 3]-Imine Cages.
Schick, Tobias H. G.; Rominger, Frank; Mastalerz, Michael; The Journal of organic chemistry  (2020) –; doi:10.1021/acs.joc.0c01887

data_4038881
_publ_section_title
;
 Examination of the Dynamic Covalent Chemistry of [2 + 3]-Imine Cages.
;
_journal_name_full               'The Journal of organic chemistry'
_journal_paper_doi               10.1021/acs.joc.0c01887
_journal_year                    2020
_chemical_formula_sum            'C48 H66 N8'
_chemical_formula_weight         755.08
_space_group_crystal_system      trigonal
_space_group_IT_number           159
_space_group_name_Hall           'P 3 -2c'
_space_group_name_H-M_alt        'P 3 1 c'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2018/3
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            4
_cell_length_a                   11.9345(3)
_cell_length_b                   11.9345(3)
_cell_length_c                   40.593(2)
_cell_measurement_reflns_used    12984
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      65.72
_cell_measurement_theta_min      2.18
_cell_volume                     5007.1(3)
_computing_cell_refinement       'X-Area Recipe 1.33.0.0 (STOE, 2015)'
_computing_data_collection       'X-Area Pilatus3_SV 1.31.144.0 (STOE, 2018)'
_computing_data_reduction        'X-Area Integrate 1.73.0.0 (STOE, 2018)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2014 (Sheldrick 2014)'
_diffrn_ambient_temperature      200(2)
_diffrn_detector_area_resol_mean 5.81
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'STOE Stadivari'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0803
_diffrn_reflns_av_unetI/netI     0.0317
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -47
_diffrn_reflns_number            30462
_diffrn_reflns_point_group_measured_fraction_full 0.778
_diffrn_reflns_point_group_measured_fraction_max 0.778
_diffrn_reflns_theta_full        63.674
_diffrn_reflns_theta_max         63.674
_diffrn_reflns_theta_min         2.177
_diffrn_source                   'Genix3D Cu HF'
_exptl_absorpt_coefficient_mu    0.459
_exptl_absorpt_correction_T_max  1.481
_exptl_absorpt_correction_T_min  0.734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'STOE X-AREA LANA'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.002
_exptl_crystal_description       plank
_exptl_crystal_F_000             1640
_exptl_crystal_size_max          0.142
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.055
_refine_diff_density_max         1.137
_refine_diff_density_min         -0.695
_refine_diff_density_rms         0.167
_refine_ls_abs_structure_details
; 
 Flack x determined using 622 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   0.7(3)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.724
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         4294
_refine_ls_number_restraints     667
_refine_ls_restrained_S_all      1.680
_refine_ls_R_factor_all          0.2291
_refine_ls_R_factor_gt           0.1747
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3910
_refine_ls_wR_factor_ref         0.4431
_reflns_Friedel_coverage         0.554
_reflns_Friedel_fraction_full    0.556
_reflns_Friedel_fraction_max     0.556
_reflns_number_gt                2623
_reflns_number_total             4294
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            jo0c01887_si_001.cif
_cod_data_source_block           sct18_sq
_cod_original_cell_volume        5007.2(4)
_cod_database_code               4038881
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_min   0.938
_shelx_estimated_absorpt_t_max   0.975
_exptl_absorpt_special_details   'X-Area LANA 1.70.0.0 (STOE, 2017)'
_shelx_res_checksum              78578
_shelx_hkl_checksum              18223
_shelx_fab_checksum              35315