Highly-efficient synthesis of covalent porphyrinic cages via DABCO-templated imine condensation reactions
Huimin Ding; Xiangshi Meng; Xu Cui; Yihui Yang; Tailin Zhou; Caixing Wang; Matthias Zeller; Cheng Wang; Chem.Commun. 50 (2014) 11162–; doi:10.1039/C4cc05449K

data_7115647
_publ_section_title
;
 Highly-efficient synthesis of covalent porphyrinic cages via
 DABCO-templated imine condensation reactions
;
_journal_name_full               Chem.Commun.
_journal_page_first              11162
_journal_paper_doi               10.1039/C4cc05449K
_journal_volume                  50
_journal_year                    2014
_chemical_formula_moiety         'C110 H84 N18 Zn2, 8.79(C H Cl3)'
_chemical_formula_sum            'C118.79 H92.79 Cl26.38 N18 Zn2'
_chemical_formula_weight         2838.46
_chemical_name_systematic        'porphyrin cage-1'
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2012
_cell_angle_alpha                90
_cell_angle_beta                 100.90(3)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   18.058(4)
_cell_length_b                   17.549(4)
_cell_length_c                   21.217(4)
_cell_measurement_reflns_used    84794
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      28.44
_cell_measurement_theta_min      0.45
_cell_volume                     6602(3)
_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-2013 (Sheldrick, 2013), 
SHELXLE Rev609 (H\"ubschle et al., 2011)
;
_computing_structure_solution    'SHELXD / XM (Sheldrick, 2008)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.974
_diffrn_measured_fraction_theta_max 0.997
_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     0.8001
_diffrn_reflns_av_R_equivalents  0.0197
_diffrn_reflns_av_unetI/netI     0.0289
_diffrn_reflns_Laue_measured_fraction_full 0.974
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -21
_diffrn_reflns_limit_k_max       0
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            21117
_diffrn_reflns_point_group_measured_fraction_full 0.974
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        28.689
_diffrn_reflns_theta_max         28.447
_diffrn_reflns_theta_min         2.560
_diffrn_source                   synchrotron
_exptl_absorpt_coefficient_mu    1.312
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_density_diffrn    1.428
_exptl_crystal_description       block
_exptl_crystal_F_000             2880.1
_exptl_crystal_size_max          0.45
_exptl_crystal_size_mid          0.30
_exptl_crystal_size_min          0.20
_refine_diff_density_max         0.616
_refine_diff_density_min         -0.399
_refine_diff_density_rms         0.067
_refine_ls_extinction_coef       0.0057(5)
_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   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1171
_refine_ls_number_reflns         11629
_refine_ls_number_restraints     496
_refine_ls_restrained_S_all      1.098
_refine_ls_R_factor_all          0.0607
_refine_ls_R_factor_gt           0.0524
_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^)+(0.0964P)^2^+3.7800P]
 where P=(Fo^2^+2Fc^2^)/3
;
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1508
_refine_ls_wR_factor_ref         0.1575
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9725
_reflns_number_total             11629
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c4cc05449k2.cif
_cod_data_source_block           cage_MZ
_cod_original_cell_volume        6602(2)
_cod_database_code               7115647
_shelxl_version_number           2012-9
_shelx_res_checksum              53338
_shelx_hkl_checksum              77784