Impact of Shape Persistence on the Porosity of Molecular Cages.
Moneypenny, 2nd, Timothy P; Walter, Nathan P.; Cai, Zhikun; Miao, Yu-Run; Gray, Danielle L.; Hinman, Jordan J.; Lee, Semin; Zhang, Yang; Moore, Jeffrey S.; Journal of the American Chemical Society 139 (2017) 3259–3264; doi:10.1021/jacs.7b00189

data_4125648
_publ_contact_author
; 
Jeffrey S. Moore 
University of Illinois 
Beckman Institute for Advanced Science and Technology 
405 North Mathews Avenue 
Urbana, Illinois  61801 
USA 
;
_publ_section_title
;
 Impact of Shape Persistence on the Porosity of Molecular Cages.
;
_journal_issue                   8
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              3259
_journal_page_last               3264
_journal_paper_doi               10.1021/jacs.7b00189
_journal_volume                  139
_journal_year                    2017
_chemical_formula_moiety         'C144 H132 Br12'
_chemical_formula_sum            'C144 H132 Br12'
_chemical_formula_weight         2821.41
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_symmetry_space_group_name_Hall  '-C 2yc'
_symmetry_space_group_name_H-M   'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_audit_creation_method           SHELXL-2014/7
_audit_update_record
; 
? 
;
_cell_angle_alpha                90
_cell_angle_beta                 121.4860(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   43.8917(19)
_cell_length_b                   20.3623(8)
_cell_length_c                   25.1357(10)
_cell_measurement_reflns_used    9513
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.61
_cell_measurement_theta_min      2.45
_cell_volume                     19157.2(14)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'APEX2 V2014.9-0 (Bruker, 2014)'
_computing_data_reduction
; 
SAINT V8.34A, XPREP v2014/2, SADABS V2014/5, 
(Bruker, 2012 & 2014) 
;
_computing_molecular_graphics
; 
SHELXTL v2014-7 (Bruker, 2014), CrystalMaker v2.7.7 (CrystalMaker, 1994) 
;
_computing_publication_material  'XCIF V2014-2 (Bruker, 2014)'
_computing_structure_refinement  'SHELX-2014-7 (Sheldrick, 2014)'
_computing_structure_solution    'SHELX-2014-7 (Sheldrick, 2014)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'Bruker D8 Venture/Photon 100'
_diffrn_measurement_method       'profile data from \f and \w scans'
_diffrn_radiation_monochromator  'multilayer mirrors'
_diffrn_radiation_source         'microfocus sealed tube'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_wavelength_id  cd39wsa_sq
_diffrn_reflns_av_R_equivalents  0.0655
_diffrn_reflns_av_unetI/netI     0.0274
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       52
_diffrn_reflns_limit_h_min       -52
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -24
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            17594
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.408
_diffrn_reflns_theta_min         2.176
_exptl_absorpt_coefficient_mu    2.542
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.5553
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.978
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5664
_exptl_crystal_id                cd39wsa_sq
_exptl_crystal_preparation
; 
The data crystal was mounted using oil (Parantone-N, Exxon) to a 
0.3 mm cryo-loop (Hampton Research) with the (1 2 -2) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.342
_exptl_crystal_size_mid          0.247
_exptl_crystal_size_min          0.142
_platon_squeeze_details
; 
The solvent in the void space is highly disordered.  The pre-SQUEEZE 
model showed evidence of both chloroform and toluene being present 
in the structure.  The number of electrons squeezed from the model 
is consistent with between 7-9 solvent molecules per formula unit 
of the organic cage molecule. The void volume supports the 
possibility of this number of solvent molecules. 
;
_refine_diff_density_max         1.614
_refine_diff_density_min         -0.818
_refine_diff_density_rms         0.100
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.094
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     880
_refine_ls_number_reflns         17594
_refine_ls_number_restraints     1295
_refine_ls_restrained_S_all      1.077
_refine_ls_R_factor_all          0.0905
_refine_ls_R_factor_gt           0.0651
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+107.0000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1922
_refine_ls_wR_factor_ref         0.2150
_reflns_Friedel_coverage         0.000
_reflns_number_gt                12936
_reflns_number_total             17594
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b00189_si_008.cif
_cod_data_source_block           cd39wsa_sq
_cod_original_cell_volume        19157.1(14)
_cod_database_code               4125648
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.477
_shelx_estimated_absorpt_t_max   0.714
_shelx_res_checksum              60213
_shelx_hkl_checksum              42260
_platon_squeeze_void_probe_radius 1.20
_shelx_fab_checksum              34229