Cation-based Structural Tuning of Pyridine Dipyrrolate Cages and Morphological Control over Their Self-assembly.
Zhang, Huacheng; Lee, Juhoon; Brewster, 2nd, James T; Chi, Xiaodong; Lynch, Vincent M.; Sessler, Jonathan L.; Journal of the American Chemical Society 141 (2019) 4749–4755; doi:10.1021/jacs.9b01042

data_4128936
_publ_section_title
;
 Cation-based Structural Tuning of Pyridine Dipyrrolate Cages and
 Morphological Control over Their Self-assembly.
;
_journal_issue                   11
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4749
_journal_page_last               4755
_journal_paper_doi               10.1021/jacs.9b01042
_journal_volume                  141
_journal_year                    2019
_chemical_formula_moiety
;
 4 C23 H25 N3 O4 2-, 4 Zn 2+, 2 C5 H5 Co 1+, O H 1-, 
 2 H2 O, 7 C3 H7 N O
;
_chemical_formula_sum            'C246 H328 Co2 N38 O52 Zn8'
_chemical_formula_weight         5290.26
_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'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 92.307(4)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   16.7237(6)
_cell_length_b                   21.2669(7)
_cell_length_c                   39.8228(13)
_cell_measurement_reflns_used    10149
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      72.9
_cell_measurement_theta_min      3.03
_cell_volume                     14151.9(8)
_computing_cell_refinement
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_data_collection
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_data_reduction
'CrysAlisPro V 1.171.37.31, Agilent Technologies'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XL SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'Shelxl-2013, Sheldrick, G. M.'
_computing_structure_solution
;

SHELXT.  G. M. Sheldrick, (2015).  Acta Cryst. C71, 9-18.
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.989
_diffrn_measured_fraction_theta_max 0.950
_diffrn_measurement_device_type  'Agilent SuperNova with AtlasS2 CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0472
_diffrn_reflns_av_unetI/netI     0.0818
_diffrn_reflns_Laue_measured_fraction_full 0.989
_diffrn_reflns_Laue_measured_fraction_max 0.950
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       49
_diffrn_reflns_limit_l_min       -40
_diffrn_reflns_number            52383
_diffrn_reflns_point_group_measured_fraction_full 0.989
_diffrn_reflns_point_group_measured_fraction_max 0.950
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.541
_diffrn_reflns_theta_min         2.827
_diffrn_source                   'microfocus sealed tube'
_exptl_absorpt_coefficient_mu    2.231
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.893
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.27t (Agilent, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'pale yellow'
_exptl_crystal_density_diffrn    1.241
_exptl_crystal_description       needle
_exptl_crystal_F_000             5560
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.07
_exptl_crystal_size_min          0.04
_refine_diff_density_max         0.925
_refine_diff_density_min         -0.741
_refine_diff_density_rms         0.085
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1670
_refine_ls_number_reflns         27119
_refine_ls_number_restraints     1754
_refine_ls_restrained_S_all      1.018
_refine_ls_R_factor_all          0.0987
_refine_ls_R_factor_gt           0.0679
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0513P)^2^+39.8434P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1533
_refine_ls_wR_factor_ref         0.1685
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19198
_reflns_number_total             27119
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01042_si_005.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_database_code               4128936
_shelx_shelxl_version_number     2014/7
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              18996
_shelx_hkl_checksum              79640
_shelx_fab_checksum              58525