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_4133954
_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      trigonal
_space_group_IT_number           155
_space_group_name_Hall           'R 3 2"'
_space_group_name_H-M_alt        'R 3 2 :H'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-06-10
_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                120
_cell_formula_units_Z            18
_cell_length_a                   43.512(6)
_cell_length_b                   43.512(6)
_cell_length_c                   27.788(5)
_cell_measurement_reflns_used    9718
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.573
_cell_measurement_theta_min      6.276
_cell_volume                     45562(12)
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100.15
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0611
_diffrn_reflns_av_unetI/netI     0.0344
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       48
_diffrn_reflns_limit_h_min       -50
_diffrn_reflns_limit_k_max       49
_diffrn_reflns_limit_k_min       -51
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            137780
_diffrn_reflns_point_group_measured_fraction_full 0.992
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        65.348
_diffrn_reflns_theta_max         65.347
_diffrn_reflns_theta_min         5.935
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    1.396
_exptl_absorpt_correction_T_max  0.7526
_exptl_absorpt_correction_T_min  0.6151
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0851 before and 0.0633 after correction. The Ratio of minimum to maximum transmission is 0.8173. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    0.902
_exptl_crystal_description       block
_exptl_crystal_F_000             13068
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.455
_exptl_crystal_size_mid          0.331
_exptl_crystal_size_min          0.226
_refine_diff_density_max         0.635
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.054
_refine_ls_abs_structure_details
;
 Flack x determined using 5876 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.082(8)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1218
_refine_ls_number_reflns         17283
_refine_ls_number_restraints     1184
_refine_ls_restrained_S_all      1.069
_refine_ls_R_factor_all          0.0779
_refine_ls_R_factor_gt           0.0665
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1480P)^2^+20.6134P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1939
_refine_ls_wR_factor_ref         0.2115
_reflns_Friedel_coverage         0.911
_reflns_Friedel_fraction_full    0.989
_reflns_Friedel_fraction_max     0.989
_reflns_number_gt                14141
_reflns_number_total             17283
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12527_si_005.cif
_cod_data_source_block           cx1570
_cod_depositor_comments
'Adding full bibliography for 4133954--4133957.cif.'
_cod_original_cell_volume        45563(15)
_cod_original_sg_symbol_H-M      'R 3 2'
_cod_database_code               4133954
_shelx_shelxl_version_number     2017/1
_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. Restrained distances
 O1A-H1A
 0.87 with sigma of 0.01
 O2A-H2A
 0.87 with sigma of 0.01
 O34-C42 = O4-C6 = O36A-C44A = O37A-C45A = O39A-C48A
 1.4 with sigma of 0.01
 C2A-H1A
 1.903043 with sigma of 0.02
 C3A-H2A
 1.953168 with sigma of 0.02
 K1A-H1A
 3.435224 with sigma of 0.02
 K1A-H2A
 3.581769 with sigma of 0.02
3. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Sof(O1A)=Sof(H1A)=Sof(O2A)=Sof(H2A)=Sof(O3A)=Sof(O4A)=Sof(H4A)=Sof(O21A)=
 Sof(H21A)=Sof(O22A)=Sof(H22A)=Sof(O23A)=Sof(O24A)=Sof(H24A)=Sof(O25A)=
 Sof(O26A)=Sof(H26A)=Sof(O27A)=Sof(H27A)=Sof(O28A)=Sof(O29A)=Sof(H29A)=
 Sof(O30A)=Sof(O36A)=Sof(H36A)=Sof(O37A)=Sof(H37A)=Sof(O38A)=Sof(O39A)=
 Sof(H39A)=Sof(C1A)=Sof(H1AA)=Sof(C2A)=Sof(H2AA)=Sof(C3A)=Sof(H3A)=Sof(C4A)=
 Sof(H4AA)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6AA)=Sof(H6AB)=Sof(C25A)=Sof(H25A)=
 Sof(C26A)=Sof(H26C)=Sof(C27A)=Sof(H27C)=Sof(C28A)=Sof(H28A)=Sof(C29A)=
 Sof(H29C)=Sof(C30A)=Sof(H30C)=Sof(H30D)=Sof(C31A)=Sof(H31B)=Sof(C32A)=
 Sof(H32B)=Sof(C33A)=Sof(H33A)=Sof(C34A)=Sof(H34B)=Sof(C35A)=Sof(H35A)=
 Sof(C36A)=Sof(H36D)=Sof(H36E)=Sof(H37C)=Sof(C43A)=Sof(H43A)=Sof(C44A)=
 Sof(H44A)=Sof(C45A)=Sof(H45A)=Sof(C46A)=Sof(H46A)=Sof(C47A)=Sof(H47A)=
 Sof(C48A)=Sof(H48C)=Sof(H48D)=1-FVAR(1)
 Sof(K1A)=Sof(K3A)=0.5*(1-FVAR(2))
 Sof(K1)=Sof(K3)=0.5*FVAR(2)
 Sof(O1)=Sof(H1)=Sof(O2)=Sof(H2)=Sof(O3)=Sof(O4)=Sof(H4)=Sof(O21)=Sof(H21)=
 Sof(O22)=Sof(H22)=Sof(O23)=Sof(O24)=Sof(H24)=Sof(O25)=Sof(O26)=Sof(H26)=
 Sof(O27)=Sof(H27)=Sof(O28)=Sof(O29)=Sof(H29)=Sof(O30)=Sof(O36)=Sof(H36)=
 Sof(O37)=Sof(H37)=Sof(O38)=Sof(O39)=Sof(H39)=Sof(C1)=Sof(H1B)=Sof(C2)=Sof(H2B)=
 Sof(C3)=Sof(H3)=Sof(C4)=Sof(H4B)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6A)=Sof(H6B)=
 Sof(C25)=Sof(H25)=Sof(C26)=Sof(H26B)=Sof(C27)=Sof(H27B)=Sof(C28)=Sof(H28)=
 Sof(C29)=Sof(H29B)=Sof(C30)=Sof(H30A)=Sof(H30B)=Sof(C31)=Sof(H31A)=Sof(C32)=
 Sof(H32A)=Sof(C33)=Sof(H33)=Sof(C34)=Sof(H34A)=Sof(C35)=Sof(H35)=Sof(C36)=
 Sof(H36B)=Sof(H36C)=Sof(H37B)=Sof(C43)=Sof(H43)=Sof(C44)=Sof(H44)=Sof(C45)=
 Sof(H45)=Sof(C46)=Sof(H46)=Sof(C47)=Sof(H47)=Sof(C48)=Sof(H48A)=Sof(H48B)=
 FVAR(1)
5.a Ternary CH refined with riding coordinates:
 C1(H1B), C1A(H1AA), C2(H2B), C2A(H2AA), C3(H3), C3A(H3A), C4(H4B), C4A(H4AA),
 C5(H5), C5A(H5A), C7(H7A), C8(H8), C9(H9A), C10(H10), C11(H11A), C13(H13),
 C14(H14A), C15(H15), C16(H16A), C17(H17A), C19(H19A), C20(H20), C21(H21B),
 C22(H22B), C23(H23), C25(H25), C25A(H25A), C26(H26B), C26A(H26C), C27(H27B),
 C27A(H27C), C28(H28), C28A(H28A), C29(H29B), C29A(H29C), C31(H31A), C31A(H31B),
  C32(H32A), C32A(H32B), C33(H33), C33A(H33A), C34(H34A), C34A(H34B), C35(H35),
 C35A(H35A), C37(H37C), C37(H37B), C38(H38), C39(H39B), C40(H40), C41(H41),
 C43(H43), C43A(H43A), C44(H44), C44A(H44A), C45(H45), C45A(H45A), C46(H46),
 C46A(H46A), C47(H47), C47A(H47A)
5.b Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C6A(H6AA,H6AB), C12(H12A,H12B), C18(H18A,H18B), C24(H24B,H24C),
 C30(H30A,H30B), C30A(H30C,H30D), C36(H36B,H36C), C36A(H36D,H36E), C42(H42A,
 H42B), C48(H48A,H48B), C48A(H48C,H48D)
5.c Tetrahedral OH refined with riding coordinates:
 O1(H1), O2(H2), O4(H4), O6(H6), O7(H7), O9(H9), O11(H11), O12(H12), O14(H14),
 O16(H16), O19(H19), O21(H21), O21A(H21A), O22(H22), O22A(H22A), O24(H24),
 O26(H26), O26A(H26A), O27(H27), O27A(H27A), O29(H29), O29A(H29A), O31(H31),
 O32(H32), O34(H34), O36(H36), O36A(H36A), O37(H37), O37A(H37A), O39(H39),
 O39A(H39A)
5.d Idealised tetrahedral OH refined as rotating group:
 O4A(H4A), O17(H17), O24A(H24A)
;
_shelx_res_checksum              47940
_shelx_hkl_checksum              55564
_shelx_fab_checksum              51289
_olex2_date_sample_data_collection 2019-05-21
_olex2_date_sample_submission    2019-05-15
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_exptl_crystal_mounting_method
'The crystal was mounted on a MITIGEN holder'
_olex2_submission_original_sample_id cx1570
_olex2_submission_special_instructions 'No special instructions were received'