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_4125647
_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 H156, 4(C H Cl3)'
_chemical_formula_sum            'C148 H160 Cl12'
_chemical_formula_weight         2364.15
_space_group_crystal_system      trigonal
_space_group_IT_number           148
_space_group_name_Hall           '-R 3'
_space_group_name_H-M_alt        'R -3 :H'
_symmetry_space_group_name_Hall  '-R 3'
_symmetry_space_group_name_H-M   'R -3 :H'
_atom_sites_solution_hydrogens   geom
_audit_creation_method           SHELXL-2014/7
_audit_update_record
; 
? 
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                120
_cell_formula_units_Z            6
_cell_length_a                   25.0005(10)
_cell_length_b                   25.0005(10)
_cell_length_c                   48.793(2)
_cell_measurement_reflns_used    9760
_cell_measurement_temperature    101(2)
_cell_measurement_theta_max      76.97
_cell_measurement_theta_min      2.72
_cell_volume                     26411.0(18)
_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      101(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.984
_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           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_radiation_wavelength_id  cd93us_sq
_diffrn_reflns_av_R_equivalents  0.0639
_diffrn_reflns_av_unetI/netI     0.0315
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.984
_diffrn_reflns_limit_h_max       31
_diffrn_reflns_limit_h_min       -30
_diffrn_reflns_limit_k_max       31
_diffrn_reflns_limit_k_min       -31
_diffrn_reflns_limit_l_max       58
_diffrn_reflns_limit_l_min       -61
_diffrn_reflns_number            92907
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.984
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         77.922
_diffrn_reflns_theta_min         2.232
_exptl_absorpt_coefficient_mu    2.006
_exptl_absorpt_correction_T_max  0.7541
_exptl_absorpt_correction_T_min  0.4870
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS V2014/5 (Bruker, 2014)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.892
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             7512
_exptl_crystal_id                cd93us_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 1 2) scattering 
planes roughly normal to the spindle axis. 
;
_exptl_crystal_size_max          0.562
_exptl_crystal_size_mid          0.477
_exptl_crystal_size_min          0.32
_platon_squeeze_details
; 
Three disordered chloroforms and one disordered ethanol were squeezed from 
asymmetric unit. In addition there was extra void space that contained solvent 
that was too disordered to identify.  The ordered solvate molecules were left 
in the structure model and the disordered solvate molecules were squeezed from 
the remaining accessable void spaces. 
;
_refine_diff_density_max         0.897
_refine_diff_density_min         -0.505
_refine_diff_density_rms         0.086
_refine_ls_extinction_coef       0.000153(9)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.131
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         12361
_refine_ls_number_restraints     258
_refine_ls_restrained_S_all      1.133
_refine_ls_R_factor_all          0.0744
_refine_ls_R_factor_gt           0.0698
_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^)+(0.0764P)^2^+198.2235P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1925
_refine_ls_wR_factor_ref         0.1956
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11332
_reflns_number_total             12361
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b00189_si_009.cif
_cod_data_source_block           cd93us_sq
_cod_original_cell_volume        26411(2)
_cod_database_code               4125647
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_min   0.399
_shelx_estimated_absorpt_t_max   0.566
_shelx_res_checksum              85563
_shelx_hkl_checksum              95044
_platon_squeeze_void_probe_radius 1.20
_shelx_fab_checksum              50411