Organic Counteranion Co-assembly Strategy for the Formation of γ-Cyclodextrin-Containing Hybrid Frameworks.
Shen, Dengke; Cooper, James A.; Li, Peng; Guo, Qing-Hui; Cai, Kang; Wang, Xingjie; Wu, Huang; Chen, Hongliang; Zhang, Long; Jiao, Yang; Qiu, Yunyan; Stern, Charlotte L.; Liu, Zhichang; Sue, Andrew C.-H.; Yang, Ying-Wei; Alsubaie, Fehaid M.; Farha, Omar K.; Stoddart, J. Fraser; Journal of the American Chemical Society 142 (2020) 2042–2050; doi:10.1021/jacs.9b12527

data_4133957
_publ_section_title
;
 Organic Counteranion Co-assembly Strategy for the Formation of
 \g-Cyclodextrin-Containing Hybrid Frameworks.
;
_journal_issue                   4
_journal_name_full               'Journal of the American Chemical Society'
_journal_page_first              2042
_journal_page_last               2050
_journal_paper_doi               10.1021/jacs.9b12527
_journal_volume                  142
_journal_year                    2020
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C48 H80 K2 O40'
_chemical_formula_sum            'C48 H80 K2 O40'
_chemical_formula_weight         1375.32
_space_group_crystal_system      cubic
_space_group_IT_number           211
_space_group_name_Hall           'I 4 2 3'
_space_group_name_H-M_alt        'I 4 3 2'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2019-05-22
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_cell_angle_alpha                90
_cell_angle_beta                 90
_cell_angle_gamma                90
_cell_formula_units_Z            12
_cell_length_a                   31.0134(14)
_cell_length_b                   31.0134(14)
_cell_length_c                   31.0134(14)
_cell_measurement_reflns_used    9970
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      19.300
_cell_measurement_theta_min      2.275
_cell_volume                     29830(2)
_computing_cell_refinement       'SAINT V8.34A (Bruker, 2017)'
_computing_data_collection       'APEX2 V2017.3 (Bruker, 2017)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXD (Sheldrick, 2008)'
_diffrn_ambient_temperature      100.07
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  Triumph
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0482
_diffrn_reflns_av_unetI/netI     0.0208
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -37
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -36
_diffrn_reflns_number            59302
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.290
_diffrn_reflns_theta_min         0.928
_diffrn_source                   'sealed tube'
_exptl_absorpt_coefficient_mu    0.161
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.6984
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0589 before and 0.0457 after correction. The Ratio of minimum to maximum transmission is 0.9372. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.919
_exptl_crystal_description       block
_exptl_crystal_F_000             8712
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.532
_exptl_crystal_size_mid          0.294
_exptl_crystal_size_min          0.232
_refine_diff_density_max         0.361
_refine_diff_density_min         -0.408
_refine_diff_density_rms         0.112
_refine_ls_abs_structure_details
;
 Flack x determined using 1092 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.061(16)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.347
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     204
_refine_ls_number_reflns         4557
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.347
_refine_ls_R_factor_all          0.1369
_refine_ls_R_factor_gt           0.1085
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3079
_refine_ls_wR_factor_ref         0.3410
_reflns_Friedel_coverage         0.747
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                3243
_reflns_number_total             4557
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12527_si_004.cif
_cod_data_source_block           cx1545
_cod_depositor_comments
'Adding full bibliography for 4133954--4133957.cif.'
_cod_original_cell_volume        29830(4)
_cod_database_code               4133957
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.919
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2.a Ternary CH refined with riding coordinates:
 C1(H1A), C2(H2A), C3(H3), C4(H4), C5(H5), C7(H7), C8(H8), C9(H9), C10(H10A),
 C11(H11)
2.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C12(H12A,H12B)
2.c Tetrahedral OH refined with riding coordinates:
 O1(H1), O2(H2), O4(H4A), O6(H6), O7(H7A), O10(H10)
;
_shelx_res_checksum              80588
_shelx_hkl_checksum              29484
_shelx_fab_checksum              79945
_olex2_date_sample_data_collection 2019-04-24
_olex2_date_sample_submission    2019-04-18
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder with Paratone oil'
_olex2_submission_original_sample_id cx1545
_olex2_submission_special_instructions 'No special instructions were received'