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_4128934
_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+, O H 1-, H2 O, 
  8 C3 H7 N O, 1/2 C6 H7 N 1+
;
_chemical_formula_sum            'C123 H170 N21 O27 Zn4'
_chemical_formula_weight         2636.27
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                89.034(3)
_cell_angle_beta                 72.865(4)
_cell_angle_gamma                80.624(4)
_cell_formula_units_Z            2
_cell_length_a                   16.1706(9)
_cell_length_b                   19.1783(7)
_cell_length_c                   22.1386(10)
_cell_measurement_reflns_used    4650
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.4
_cell_measurement_theta_min      3.00
_cell_volume                     6469.8(5)
_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-2014/7, Sheldrick, G. M.'
_computing_structure_solution
;

Sheldrick, G. M. (2015).  SHELXT.  Acta Cryst. A71, 3-8.
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.987
_diffrn_measured_fraction_theta_max 0.944
_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  0.0653
_diffrn_reflns_av_unetI/netI     0.1012
_diffrn_reflns_Laue_measured_fraction_full 0.987
_diffrn_reflns_Laue_measured_fraction_max 0.944
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            40457
_diffrn_reflns_point_group_measured_fraction_full 0.987
_diffrn_reflns_point_group_measured_fraction_max 0.944
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.757
_diffrn_reflns_theta_min         3.031
_diffrn_source                   'sealed microfocus tube'
_exptl_absorpt_coefficient_mu    1.489
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.937
_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            orange
_exptl_crystal_density_diffrn    1.353
_exptl_crystal_description       prism
_exptl_crystal_F_000             2782
_exptl_crystal_size_max          0.310
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.060
_refine_diff_density_max         0.786
_refine_diff_density_min         -0.592
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.993
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1651
_refine_ls_number_reflns         25046
_refine_ls_number_restraints     1116
_refine_ls_restrained_S_all      0.987
_refine_ls_R_factor_all          0.0994
_refine_ls_R_factor_gt           0.0604
_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^)+(0.0579P)^2^+3.0373P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1446
_refine_ls_wR_factor_ref         0.1723
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16147
_reflns_number_total             25046
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b01042_si_003.cif
_cod_data_source_block           shelx
_cod_database_code               4128934
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.655
_shelx_estimated_absorpt_t_max   0.916
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              84238
_shelx_hkl_checksum              68633
_shelx_fab_checksum              29056