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_4130124
_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
'C23 H26 N3 O4 1-, C16 H36 N 1+, H2 O, 1/2 C H2 Cl2'
_chemical_formula_sum            'C39.5 H65 Cl N4 O5'
_chemical_formula_weight         711.40
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_method           SHELXL-2014/7
_cell_angle_alpha                90
_cell_angle_beta                 106.877(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   18.156(3)
_cell_length_b                   9.0535(12)
_cell_length_c                   25.803(4)
_cell_measurement_reflns_used    11208
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.1
_cell_measurement_theta_min      1.16
_cell_volume                     4058.7(11)
_computing_cell_refinement       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_collection       'CrystalClear (Rigaku Inc., 2008)'
_computing_data_reduction        'CrystalClear (Rigaku Inc., 2008)'
_computing_molecular_graphics    'XP SHELXTL/PC, Siemens Analytical'
_computing_publication_material  'XP SHELXTL/PC, Siemens Analytical'
_computing_structure_refinement  'SHELXL-2014/7 (Sheldrick, 2015)'
_computing_structure_solution
;

Sir2004.  Burla M.C., Caliandro, R., Camalli M., Carrozzini, B., Cascarano G.L., 
De Caro, L., Giacovazzo C., Polidori G., Spagna R. 
;
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_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  0.0387
_diffrn_reflns_av_unetI/netI     0.0257
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       10
_diffrn_reflns_limit_k_min       -10
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            49564
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.025
_diffrn_reflns_theta_max         25.025
_diffrn_reflns_theta_min         3.165
_diffrn_source                   'sealed fine focus tube'
_exptl_absorpt_coefficient_mu    0.139
_exptl_crystal_colour            colorless
_exptl_crystal_density_diffrn    1.164
_exptl_crystal_description       plate
_exptl_crystal_F_000             1548
_refine_diff_density_max         0.713
_refine_diff_density_min         -0.358
_refine_diff_density_rms         0.045
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.009
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     492
_refine_ls_number_reflns         7162
_refine_ls_number_restraints     79
_refine_ls_restrained_S_all      1.036
_refine_ls_R_factor_all          0.0602
_refine_ls_R_factor_gt           0.0513
_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^)+(0.0632P)^2^+3.3513P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1266
_refine_ls_wR_factor_ref         0.1327
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6148
_reflns_number_total             7162
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja6b00564_si_002.cif
_cod_data_source_block           shelx
_cod_original_cell_volume        4058.8(10)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C39.50 H65 Cl N4 O5'
_cod_database_code               4130124
_shelx_shelxl_version_number     2014/7
_platon_squeeze_void_probe_radius 1.20
_shelx_res_checksum              45705
_shelx_hkl_checksum              67881
_shelx_fab_checksum              96602