Self-Assembled Pyridine-Dipyrrolate Cages.
Zhang, Huacheng; Lee, Juhoon; Lammer, Aaron D.; Chi, Xiaodong; Brewster, James T.; Lynch, Vincent M.; Li, Hao; Zhang, Zhan; Sessler, Jonathan L.; Journal of the American Chemical Society 138 (2016) 4573–4579; doi:10.1021/jacs.6b00564

data_4130125
_publ_section_title
;
 Self-Assembled Pyridine-Dipyrrolate Cages.
;
_journal_issue                   13
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              4573
_journal_page_last               4579
_journal_paper_doi               10.1021/jacs.6b00564
_journal_volume                  138
_journal_year                    2016
_chemical_formula_moiety
;         
  8 C23 H25 N3 O4 -2, 8 Zn 2+, 2 C2 H8 N 1+, 2 O H 1-, 
 7 C3 H7 N O
;
_chemical_formula_sum            'C209 H267 N33 O41 Zn8'
_chemical_formula_weight         4420.50
_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   mixed
_audit_creation_method           SHELXL-2013
_cell_angle_alpha                105.094(4)
_cell_angle_beta                 103.903(4)
_cell_angle_gamma                91.781(5)
_cell_formula_units_Z            1
_cell_length_a                   15.916(5)
_cell_length_b                   18.830(6)
_cell_length_c                   19.364(6)
_cell_measurement_reflns_used    20870
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.8
_cell_measurement_theta_min      3.56
_cell_volume                     5412(3)
_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
;

SUPERFLIP.  Palatinus, L. and Chapuis, G., J. Appl. Cryst. 40, 786-790.
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.991
_diffrn_measured_fraction_theta_max 0.954
_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  0.0199
_diffrn_reflns_av_unetI/netI     0.0281
_diffrn_reflns_Laue_measured_fraction_full 0.991
_diffrn_reflns_Laue_measured_fraction_max 0.954
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       23
_diffrn_reflns_limit_k_min       -21
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            41174
_diffrn_reflns_point_group_measured_fraction_full 0.991
_diffrn_reflns_point_group_measured_fraction_max 0.954
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         74.089
_diffrn_reflns_theta_min         2.875
_diffrn_source                   'sealed microfocus tube'
_exptl_absorpt_coefficient_mu    1.616
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.921
_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            colorless
_exptl_crystal_density_diffrn    1.356
_exptl_crystal_description       plate
_exptl_crystal_F_000             2320
_exptl_crystal_size_max          0.16
_exptl_crystal_size_mid          0.08
_exptl_crystal_size_min          0.05
_refine_diff_density_max         0.601
_refine_diff_density_min         -0.502
_refine_diff_density_rms         0.053
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.977
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1444
_refine_ls_number_reflns         21005
_refine_ls_number_restraints     365
_refine_ls_restrained_S_all      1.143
_refine_ls_R_factor_all          0.0428
_refine_ls_R_factor_gt           0.0338
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0398P)^2^+4.7091P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0831
_refine_ls_wR_factor_ref         0.0880
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18188
_reflns_number_total             21005
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b00564_si_005.cif
_cod_data_source_block           shelx
_cod_database_code               4130125
_shelxl_version_number           2013-4
_shelx_res_checksum              45436
_shelx_hkl_checksum              13958