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_4133956
_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
'C145 H242.5 K6 O121, 5.5(C8 H7 O4), 4(C H4 O), 7(H2 O)'
_chemical_formula_sum            'C193 H311 K6 O154'
_chemical_formula_weight         5330.00
_space_group_crystal_system      tetragonal
_space_group_IT_number           96
_space_group_name_Hall           'P 4nw 2abw'
_space_group_name_H-M_alt        'P 43 21 2'
_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                90
_cell_formula_units_Z            8
_cell_length_a                   31.2120(12)
_cell_length_b                   31.2120(12)
_cell_length_c                   61.302(3)
_cell_measurement_reflns_used    9603
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      20.002
_cell_measurement_theta_min      2.711
_cell_volume                     59720(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_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      100.01
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.998
_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           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1864
_diffrn_reflns_av_unetI/netI     0.1388
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.998
_diffrn_reflns_limit_h_max       39
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       38
_diffrn_reflns_limit_k_min       -39
_diffrn_reflns_limit_l_max       76
_diffrn_reflns_limit_l_min       -76
_diffrn_reflns_number            453882
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.998
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         26.401
_diffrn_reflns_theta_min         0.732
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    0.184
_exptl_absorpt_correction_T_max  0.7454
_exptl_absorpt_correction_T_min  0.6445
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1045 before and 0.0903 after correction. The Ratio of minimum to maximum transmission is 0.8646. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.186
_exptl_crystal_description       cube
_exptl_crystal_F_000             22520
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.124
_exptl_crystal_size_min          0.11
_refine_diff_density_max         1.318
_refine_diff_density_min         -0.469
_refine_diff_density_rms         0.081
_refine_ls_abs_structure_details
;
 Flack x determined using 11331 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.019(19)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.974
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3277
_refine_ls_number_reflns         61180
_refine_ls_number_restraints     111
_refine_ls_restrained_S_all      0.976
_refine_ls_R_factor_all          0.1452
_refine_ls_R_factor_gt           0.0736
_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^)+(0.1187P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1782
_refine_ls_wR_factor_ref         0.2147
_reflns_Friedel_coverage         0.862
_reflns_Friedel_fraction_full    1.000
_reflns_Friedel_fraction_max     0.998
_reflns_number_gt                34143
_reflns_number_total             61180
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ja9b12527_si_002.cif
_cod_data_source_block           cx1537_a
_cod_depositor_comments
'Adding full bibliography for 4133954--4133957.cif.'
_cod_original_cell_volume        59720(5)
_cod_database_code               4133956
_shelx_shelxl_version_number     2017/1
_shelx_estimated_absorpt_t_max   0.980
_shelx_estimated_absorpt_t_min   0.969
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O42E-O41E
 2.2 with sigma of 0.02
 O42E-C55E = O41E-C55E
 1.3 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O15A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
O35C \\sim O35B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
Uanis(C56) \\sim Ueq, Uanis(C55A) \\sim Ueq, Uanis(O41A) \\sim Ueq: with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Rigid body (RIGU) restrains
 O41E, O42E, O43E, O44E, C49E, C50E, C51E, C52E, C53E, C54E, C55E, C56E
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O15A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O35B, O35C
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(O1BA)=Sof(H1BA)=Sof(H12D)=Sof(H12E)=1-FVAR(1)
 Sof(O10A)=Sof(H10A)=Sof(H12B)=Sof(H12C)=FVAR(1)
 Sof(O35C)=Sof(H35D)=Sof(H42E)=Sof(H42F)=1-FVAR(2)
 Sof(O35B)=Sof(H35C)=Sof(H42C)=Sof(H42D)=FVAR(2)
 Fixed Sof: H17C(0.5) H18D(0.5) H21B(0.5) O41E(0.5) O42E(0.5) O43E(0.5)
 H43H(0.5) O44E(0.5) C49E(0.5) C50E(0.5) C51E(0.5) H51E(0.5) C52E(0.5)
 C53E(0.5) H53E(0.5) C54E(0.5) H54E(0.5) C55E(0.5) C56E(0.5) H56P(0.5)
 H56Q(0.5) H56R(0.5)
6.a Everything fixed:
 O10S, H10F, H10G, O9S, H9SA, H9SB, O7BA, H7BB, H7BC, O4CA, H4CA, H4CB
6.b Free rotating group:
 O0AA(H0AA,H0AB), O7S(H7SA,H7SB), O8S(H8SA,H8SB)
6.c Ternary CH refined with riding coordinates:
 C1A(H1A), C2A(H2AA), C3A(H3AA), C4A(H4A), C5A(H5AA), C7A(H7AA), C8A(H8AA),
 C9A(H9A), C10A(H10B), C11A(H11A), C13A(H13B), C14A(H14A), C15A(H15B),
 C16A(H16A), C17A(H17B), C19A(H19A), C20A(H20B), C21A(H21A), C22A(H22B),
 C23A(H23B), C25A(H25B), C26A(H26A), C27A(H27B), C28A(H28B), C29A(H29A),
 C31A(H31A), C32A(H32B), C33A(H33B), C34A(H34A), C35A(H35B), C37A(H37B),
 C38A(H38B), C39A(H39A), C40A(H40B), C41A(H41A), C43A(H43A), C44A(H44A),
 C45A(H45A), C46A(H46A), C47A(H47A), C1B(H1B), C2B(H2BA), C3B(H3BA), C4B(H4B),
 C5B(H5BA), C7B(H7BA), C8B(H8BA), C9B(H9B), C10B(H10D), C11B(H11B), C13B(H13D),
 C14B(H14B), C15B(H15D), C16B(H16B), C17B(H17D), C19B(H19B), C20B(H20D),
 C21B(H21B), C22B(H22D), C23B(H23D), C25B(H25D), C26B(H26B), C27B(H27D),
 C28B(H28D), C29B(H29B), C31B(H31B), C32B(H32D), C33B(H33D), C34B(H34B),
 C35B(H35E), C37B(H37D), C38B(H38D), C39B(H39B), C40B(H40D), C41B(H41B),
 C43B(H43B), C44B(H44B), C45B(H45B), C46B(H46B), C47B(H47B), C1(H1), C2(H2C),
 C3(H3C), C4(H4), C5(H5C), C7(H7C), C8(H8C), C9(H9), C10(H10E), C11(H11),
 C13(H13E), C14(H14), C15(H15E), C16(H16), C17(H17E), C19(H19), C20(H20E),
 C21(H21), C22(H22E), C23(H23E), C25(H25E), C26(H26), C27(H27E), C28(H28E),
 C29(H29), C31(H31), C32(H32E), C33(H33E), C34(H34), C35(H35F), C37(H37E),
 C38(H38E), C39(H39), C40(H40E), C41(H41), C43(H43), C44(H44), C45(H45),
 C46(H46), C47(H47)
6.d Secondary CH2 refined with riding coordinates:
 C6A(H6AA,H6AB), C12A(H12D,H12E), C12A(H12B,H12C), C18A(H18B,H18C), C24A(H24A,
 H24B), C30A(H30B,H30C), C36A(H36A,H36B), C42A(H42A,H42B), C48A(H48A,H48B),
 C6B(H6BA,H6BB), C12B(H12G,H12H), C18B(H18E,H18F), C24B(H24C,H24D), C30B(H30E,
 H30F), C36B(H36C,H36D), C42B(H42C,H42D), C42B(H42E,H42F), C48B(H48C,H48D),
 C6(H6A,H6B), C12(H12I,H12J), C18(H18G,H18H), C24(H24E,H24F), C30(H30G,H30H),
 C36(H36E,H36F), C42(H42G,H42H), C48(H48E,H48F)
6.e Me refined with riding coordinates:
 C56(H56M,H56N,H56O)
6.f Aromatic/amide H refined with riding coordinates:
 C51A(H51A), C53A(H53A), C54A(H54A), C51D(H51D), C53D(H53D), C54D(H54D),
 C51B(H51B), C53B(H53B), C54B(H54B), C51C(H51C), C53C(H53C), C54C(H54C),
 C51(H51), C53(H53), C54(H54), C51E(H51E), C53E(H53E), C54E(H54E)
6.g Tetrahedral OH refined with riding coordinates:
 O2A(H2A), O3A(H3A), O5A(H5A), O7A(H7A), O20A(H20A), O22A(H22A), O23A(H23A),
 O30A(H30A), O32A(H32A), O33A(H33A), O40A(H40A), O2B(H2B), O3B(H3B), O7B(H7B),
 O8B(H8B), O10B(H10C), O18B(H18D), O22B(H22C), O23B(H23C), O30B(H30D),
 O32B(H32C), O33B(H33C), O35C(H35D), O40B(H40C), O2(H2), O3(H3), O5(H5),
 O12(H12), O13(H13), O15(H15), O20(H20), O22(H22), O23(H23), O28(H28), O30(H30),
  O32(H32), O33(H33), O38(H38), O40(H40), O43C(H43F), O43(H43G), O43E(H43H),
 O1S(H1S)
6.h Idealised Me refined as rotating group:
 C56A(H56A,H56B,H56C), C56D(H56D,H56E,H56F), C56B(H56G,H56H,H56I), C56C(H56J,
 H56K,H56L), C56E(H56P,H56Q,H56R), C3S(H3SA,H3SB,H3SC), C1S(H1SA,H1SB,H1SC),
 C5S(H5SA,H5SB,H5SC), C4S(H4SA,H4SB,H4SC), C2S(H2SA,H2SB,H2SC)
6.i Idealised tetrahedral OH refined as rotating group:
 O1BA(H1BA), O8A(H8A), O10A(H10A), O12A(H12A), O13A(H13A), O15A(H15A),
 O17A(H17A), O18A(H18A), O25A(H25A), O27A(H27A), O28A(H28A), O35A(H35A),
 O37A(H37A), O38A(H38A), O5B(H5B), O12B(H12F), O13B(H13C), O15B(H15C),
 O17B(H17C), O20B(H20C), O25B(H25C), O27B(H27C), O28B(H28C), O35B(H35C),
 O37B(H37C), O38B(H38C), O7(H7), O8(H8), O10(H10), O17(H17), O18(H18), O25(H25),
  O27(H27), O35(H35), O37(H37), O43A(H43C), O43D(H43D), O43B(H43E), O3S(H3S),
 O5S(H5S), O4S(H4S), O2S(H2S)
;
_shelx_res_checksum              62687
_shelx_hkl_checksum              10688
_shelx_fab_checksum              13698
_olex2_date_sample_data_collection 2019-04-17
_olex2_date_sample_submission    2019-04-15
_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 cx1537
_olex2_submission_special_instructions 'No special instructions were received'