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_4125535
_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, 4(C H Cl3)'
_chemical_formula_sum            'C148 H136 Cl12'
_chemical_formula_weight         2339.97
_chemical_name_systematic
; 
? 
;
_space_group_crystal_system      tetragonal
_space_group_IT_number           88
_space_group_name_Hall           '-I 4ad'
_space_group_name_H-M_alt        'I 41/a'
_symmetry_space_group_name_Hall  '-I 4ad'
_symmetry_space_group_name_H-M   'I 41/a :2'
_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                90
_cell_formula_units_Z            4
_cell_length_a                   18.9935(5)
_cell_length_b                   18.9935(5)
_cell_length_c                   50.612(3)
_cell_measurement_reflns_used    9886
_cell_measurement_temperature    200(2)
_cell_measurement_theta_max      38.30
_cell_measurement_theta_min      2.81
_cell_volume                     18258.4(13)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2005)'
_computing_data_collection       'Bruker APEX2 v2014.11.0 (Bruker, 2014)'
_computing_data_reduction        'Bruker SAINT v8.34A'
_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, 2015)'
_computing_structure_solution    'SHELX-2014-7 (Sheldrick, 2015)'
_diffrn_ambient_temperature      200(2)
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.998
_diffrn_measurement_device_type  'Bruker PHOTON100 CMOS'
_diffrn_measurement_method       'omega-phi scans'
_diffrn_radiation_monochromator  'Si-<111> channel cut crystal'
_diffrn_radiation_source         synchrotron
_diffrn_radiation_type           synchrotron
_diffrn_radiation_wavelength     1.2399
_diffrn_radiation_wavelength_id  ill002c
_diffrn_reflns_av_R_equivalents  0.1087
_diffrn_reflns_av_unetI/netI     0.0575
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -8
_diffrn_reflns_limit_l_max       43
_diffrn_reflns_limit_l_min       -50
_diffrn_reflns_number            27663
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        38.332
_diffrn_reflns_theta_max         38.332
_diffrn_reflns_theta_min         2.808
_exptl_absorpt_coefficient_mu    1.024
_exptl_absorpt_correction_T_max  0.9645
_exptl_absorpt_correction_T_min  0.3033
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   'SADABS v2014.5 (Sheldrick)'
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    0.851
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4912
_exptl_crystal_id                ill002c
_exptl_crystal_preparation
; 
? 
;
_exptl_crystal_size_max          0.23
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.14
_platon_squeeze_details
; 
The contribution of approximately 200 electrons per asymmetric unit 
were removed from the diffraction intensities.  This is equivalent to 
between 3 and 4 solvate molecules.  The presqueezed model showed 3 
areas of unknown solvate electron density. 
;
_refine_diff_density_max         0.529
_refine_diff_density_min         -0.427
_refine_diff_density_rms         0.048
_refine_ls_extinction_coef       0.00012(5)
_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   1.083
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     434
_refine_ls_number_reflns         4787
_refine_ls_number_restraints     695
_refine_ls_restrained_S_all      1.196
_refine_ls_R_factor_all          0.1060
_refine_ls_R_factor_gt           0.0881
_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^)+(0.1433P)^2^+32.5945P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2624
_refine_ls_wR_factor_ref         0.2817
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3599
_reflns_number_total             4787
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja7b00189_si_007.cif
_cod_data_source_block           ill002c
_cod_depositor_comments          'Adding full bibliography for 4125535.cif.'
_cod_original_cell_volume        18258.5(13)
_cod_database_code               4125535
_shelx_shelxl_version_number     2014/7
_shelx_res_checksum              39709
_shelx_hkl_checksum              28076
_platon_squeeze_void_probe_radius 1.20
_shelx_fab_checksum              18239