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_4130122
_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
;
 3 C23 H25 N3 O4 2-, 4 Zn 2+, O H -1, C2 H3 O2 1-, 
 5 C3 H7 N O, 1/4 C6 H14
;
_chemical_formula_sum            'C87.5 H119.5 N14 O21 Zn4'
_chemical_formula_weight         1964.94
_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                 101.593(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   14.7663(12)
_cell_length_b                   26.944(2)
_cell_length_c                   24.182(2)
_cell_measurement_reflns_used    28056
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      27.5
_cell_measurement_theta_min      1.14
_cell_volume                     9424.9(13)
_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 0.998
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Rigaku AFC-12 with Saturn 724+ CCD'
_diffrn_measurement_method       \w-scans
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0766
_diffrn_reflns_av_unetI/netI     0.0564
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       31
_diffrn_reflns_limit_l_min       -31
_diffrn_reflns_number            145206
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         27.484
_diffrn_reflns_theta_min         3.019
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    1.081
_exptl_absorpt_correction_T_max  1.00
_exptl_absorpt_correction_T_min  0.755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
Abscor. T. Higashi (2001). The Rigaku Corporation, Tokyo, Japan.
;
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.385
_exptl_crystal_description       prisms
_exptl_crystal_F_000             4122
_exptl_crystal_size_max          0.32
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.578
_refine_diff_density_min         -0.536
_refine_diff_density_rms         0.090
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.084
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1184
_refine_ls_number_reflns         21571
_refine_ls_number_restraints     1008
_refine_ls_restrained_S_all      1.062
_refine_ls_R_factor_all          0.0757
_refine_ls_R_factor_gt           0.0544
_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^)+(0.0108P)^2^+21.7329P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0936
_refine_ls_wR_factor_ref         0.1000
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16848
_reflns_number_total             21571
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b00564_si_003.cif
_cod_data_source_block           shelx
_cod_original_sg_symbol_H-M      'P 21/n'
_cod_original_formula_sum        'C87.50 H119.50 N14 O21 Zn4'
_cod_database_code               4130122
_shelx_shelxl_version_number     2014/7
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              58029
_shelx_hkl_checksum              72880
_shelx_fab_checksum              49682