Rational Design and Construction of Hierarchical Superstructures Using Shape-Persistent Organic Cages: Porphyrin Box-Based Metallosupramolecular Assemblies.
Kim, Younghoon; Koo, Jaehyoung; Hwang, In-Chul; Mukhopadhyay, Rahul Dev; Hong, Soonsang; Yoo, Jejoong; Dar, Ajaz Ahmad; Kim, Ikjin; Moon, Dohyun; Shin, Tae Joo; Ko, Young Ho; Kim, Kimoon; Journal of the American Chemical Society 140 (2018) 14547–14551; doi:10.1021/jacs.8b08030

data_4133029
_publ_section_title
;
 Rational Design and Construction of Hierarchical Superstructures Using
 Shape-Persistent Organic Cages: Porphyrin Box-Based Metallosupramolecular
 Assemblies.
;
_journal_issue                   44
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              14547
_journal_page_last               14551
_journal_paper_doi               10.1021/jacs.8b08030
_journal_volume                  140
_journal_year                    2018
_chemical_formula_moiety         'C592 H656 N52 O26 Zn6'
_chemical_formula_sum            'C592 H656 N52 O26 Zn6'
_chemical_formula_weight         9307.87
_space_group_crystal_system      tetragonal
_space_group_IT_number           126
_space_group_name_Hall           '-P 4a 2bc'
_space_group_name_H-M_alt        'P 4/n n c :2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2016/6
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   40.050(6)
_cell_length_b                   40.050(6)
_cell_length_c                   37.745(8)
_cell_measurement_reflns_used    485
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      21.262
_cell_measurement_theta_min      0.944
_cell_volume                     60543(18)
_computing_cell_refinement       'HKL3000 (Z. Otwinowski and W. Minor, 1997)'
_computing_data_collection       'PAL ADSC Quantum-210 ADX Program'
_computing_data_reduction        'HKL3000 (Z. Otwinowski and W. Minor, 1997)'
_computing_molecular_graphics    'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_publication_material  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_refinement  'SHELXL-2016/6 (Sheldrick, 2016)'
_computing_structure_solution    'SHELXL-2016/6 (Sheldrick, 2016)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean '4096 x 4096'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     0.660
_diffrn_reflns_av_R_equivalents  0.0401
_diffrn_reflns_av_unetI/netI     0.0481
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       44
_diffrn_reflns_limit_h_min       -43
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            80927
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        21.262
_diffrn_reflns_theta_max         21.262
_diffrn_reflns_theta_min         0.944
_diffrn_source                   'PLSII 6D bending magnet'
_exptl_absorpt_coefficient_mu    0.121
_exptl_absorpt_correction_T_max  1.0
_exptl_absorpt_correction_T_min  0.8013
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details   'Scalepack (Otwinowski & Minor, 1997)'
_exptl_crystal_colour            purple
_exptl_crystal_density_diffrn    0.511
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       stick
_exptl_crystal_F_000             9920
_exptl_crystal_size_max          0.65
_exptl_crystal_size_mid          0.55
_exptl_crystal_size_min          0.55
_refine_diff_density_max         0.321
_refine_diff_density_min         -0.330
_refine_diff_density_rms         0.053
_refine_ls_extinction_coef       0.00005(2)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2016/6 (Sheldrick 2016)'
_refine_ls_goodness_of_fit_ref   0.994
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     629
_refine_ls_number_reflns         21040
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.994
_refine_ls_R_factor_all          0.1931
_refine_ls_R_factor_gt           0.1199
_refine_ls_shift/su_max          0.067
_refine_ls_shift/su_mean         0.003
_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          0.3525
_refine_ls_wR_factor_ref         0.3809
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6739
_reflns_number_total             21040
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja8b08030_si_005.cif
_cod_data_source_block           PSS-4
_cod_original_cell_volume        60543(21)
_cod_original_sg_symbol_H-M      'P 4/n n c'
_cod_database_code               4133029
_shelx_shelxl_version_number     2016/6
_shelx_res_checksum              95311
_shelx_hkl_checksum              80806