#------------------------------------------------------------------------------
#$Date: 2020-02-04 05:09:47 +0200 (Tue, 04 Feb 2020) $
#$Revision: 247525 $
#$URL: file:///home/coder/svn-repositories/cod/cif/4/13/39/4133955.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_4133955
loop_
_publ_author_name
'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'
_publ_section_title
;
 Organic Counteranion Co-assembly Strategy for the Formation of
 γ-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
'1.5(C96 H160 O80), 5(C8 H7 O4), 2(C H4 O), 6(K) '
_chemical_formula_sum            'C186 H283 K6 O142'
_chemical_formula_weight         5025.71
_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             2019-04-22
_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            8
_cell_length_a                   31.089(2)
_cell_length_b                   31.089(2)
_cell_length_c                   61.485(6)
_cell_measurement_reflns_used    9234
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      64.627
_cell_measurement_theta_min      2.843
_cell_volume                     59427(8)
_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      100.1
_diffrn_detector_area_resol_mean 8
_diffrn_measured_fraction_theta_full 0.962
_diffrn_measured_fraction_theta_max 0.947
_diffrn_measurement_device_type  'Bruker Kappa APEX CCD area detector'
_diffrn_measurement_method       'ω and φ scans'
_diffrn_radiation_monochromator  'MX optics'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.1173
_diffrn_reflns_av_unetI/netI     0.0703
_diffrn_reflns_Laue_measured_fraction_full 0.962
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       35
_diffrn_reflns_limit_h_min       -34
_diffrn_reflns_limit_k_max       36
_diffrn_reflns_limit_k_min       -36
_diffrn_reflns_limit_l_max       70
_diffrn_reflns_limit_l_min       -72
_diffrn_reflns_number            535998
_diffrn_reflns_point_group_measured_fraction_full 0.958
_diffrn_reflns_point_group_measured_fraction_max 0.943
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         68.515
_diffrn_reflns_theta_min         1.592
_diffrn_source                   microsource
_exptl_absorpt_coefficient_mu    1.568
_exptl_absorpt_correction_T_max  0.7503
_exptl_absorpt_correction_T_min  0.6601
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1249 before and 0.0899 after correction. The Ratio of minimum to maximum transmission is 0.8798. The λ/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.123
_exptl_crystal_description       block
_exptl_crystal_F_000             21192
_exptl_crystal_recrystallization_method
'The material was recrystallised from --- by as supplied'
_exptl_crystal_size_max          0.595
_exptl_crystal_size_mid          0.158
_exptl_crystal_size_min          0.092
_refine_diff_density_max         1.203
_refine_diff_density_min         -0.501
_refine_diff_density_rms         0.110
_refine_ls_abs_structure_details
;
 Flack x determined using 14013 quotients [(I+)-(I-)]/[(I+)+(I-)]
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259).
;
_refine_ls_abs_structure_Flack   0.067(4)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.004
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     3110
_refine_ls_number_reflns         51602
_refine_ls_number_restraints     305
_refine_ls_restrained_S_all      5.328
_refine_ls_R_factor_all          0.0936
_refine_ls_R_factor_gt           0.0732
_refine_ls_shift/su_max          0.005
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[σ²(Fo²)+(0.1404P)²] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1932
_refine_ls_wR_factor_ref         0.2073
_reflns_Friedel_coverage         0.848
_reflns_Friedel_fraction_full    0.954
_reflns_Friedel_fraction_max     0.938
_reflns_number_gt                38993
_reflns_number_total             51602
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            ja9b12527_si_003.cif
_cod_data_source_block           cx1531
_cod_depositor_comments
'Adding full bibliography for 4133954--4133957.cif.'
_cod_original_cell_volume        59425(10)
_cod_database_code               4133955
_shelx_shelxl_version_number     2017/1
_shelx_space_group_comment
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_shelx_estimated_absorpt_t_max   0.869
_shelx_estimated_absorpt_t_min   0.456
_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
2. Restrained distances
 C40S-C34S
 1.54 with sigma of 0.02
 O30-H30
 0.87 with sigma of 0.01
 O23B-H23C
 0.87 with sigma of 0.01
 O30A-H30A
 0.87 with sigma of 0.01
 O22B-H22C
 0.87 with sigma of 0.01
 C36-H30
 1.899944 with sigma of 0.02
 K3-H30
 3.718792 with sigma of 0.02
 C27B-H23C
 1.92173 with sigma of 0.02
 K2-H23C
 3.429606 with sigma of 0.02
 C36A-H30A
 1.889237 with sigma of 0.02
 K2-H30A
 3.461531 with sigma of 0.02
 C26B-H22C
 1.910524 with sigma of 0.02
 K3-H22C
 3.66534 with sigma of 0.02
 O2AA-C12A \\sim O10A-C12A
 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
O17S \\sim O18S \\sim O19S \\sim O20S \\sim C34S \\sim C35S \\sim C36S \\sim
H36S \\sim C37S \\sim C38S \\sim H38S \\sim C39S \\sim H39S \\sim C40S \\sim
C41S \\sim H41C \\sim H41D \\sim H41E: within 2A with sigma of 0.01 and sigma
for terminal atoms of 0.02
O35B \\sim C42B: within 2A with sigma of 0.01 and sigma for terminal atoms of
0.02
4. Rigid body (RIGU) restrains
 O13S, O14S, O15S, O16S, C26S, C27S, C28S, C29S, C30S, C31S, C32S, C33S
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O17S, O18S, O19S, O20S, C34S, C35S, C36S, C37S, C38S, C39S, C40S, C41S
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5. Others
 Sof(O2AA)=Sof(H2AA)=Sof(H12D)=Sof(H12E)=1-FVAR(1)
 Sof(O10A)=Sof(H10A)=Sof(H12B)=Sof(H12C)=FVAR(1)
 Fixed Sof: K3(0.5) K6(0.5)
6.a Ternary CH refined with riding coordinates:
 C1A(H1A), C2A(H2AB), 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(H35D), 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(H35E), C37(H37E),
 C38(H38E), C39(H39), C40(H40E), C41(H41), C43(H43), C44(H44), C45(H45),
 C46(H46), C47(H47)
6.b 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), C48B(H48C,H48D), C6(H6A,H6B),
 C12(H12I,H12J), C18(H18G,H18H), C24(H24E,H24F), C30(H30G,H30H), C36(H36E,H36F),
  C42(H42E,H42F), C48(H48E,H48F)
6.c Aromatic/amide H refined with riding coordinates:
 C11S(H11S), C12S(H12S), C14S(H14S), C19S(H19S), C20S(H20S), C23S(H23S),
 C27S(H27S), C28S(H28S), C30S(H30S), C36S(H36S), C38S(H38S), C39S(H39S),
 C4S(H4S), C6S(H6S), C7S(H7SA)
6.d Tetrahedral OH refined with riding coordinates:
 O30A(H30A), O37A(H37A), O2B(H2B), O3B(H3B), O22B(H22C), O19S(H19C), O21S(H21S)
6.e Idealised Me refined as rotating group:
 C17S(H17F,H17G,H17H), C25S(H25F,H25G,H25H), C33S(H33F,H33G,H33H), C41S(H41C,
 H41D,H41E), C9S(H9SA,H9SB,H9SC), C42S(H42G,H42H,H42I), C43S(H43C,H43D,H43E)
6.f Idealised tetrahedral OH refined as rotating group:
 O2A(H2A), O2AA(H2AA), O3A(H3A), O5A(H5A), O7A(H7A), O8A(H8A), O10A(H10A),
 O12A(H12A), O13A(H13A), O15A(H15A), O17A(H17A), O18A(H18A), O20A(H20A),
 O22A(H22A), O23A(H23A), O25A(H25A), O27A(H27A), O28A(H28A), O32A(H32A),
 O33A(H33A), O35A(H35A), O38A(H38A), O40A(H40A), O5B(H5B), O7B(H7B), O8B(H8B),
 O10B(H10C), O12B(H12F), O13B(H13C), O15B(H15C), O17B(H17C), O18B(H18D),
 O20B(H20C), O25B(H25C), O27B(H27C), O28B(H28C), O30B(H30D), O32B(H32C),
 O33B(H33C), O35B(H35C), O37B(H37C), O38B(H38C), O40B(H40C), O2(H2), O3(H3),
 O5(H5), O7(H7), O8(H8), O10(H10), O12(H12), O13(H13), O15(H15), O17(H17),
 O18(H18), O20(H20), O22(H22), O23(H23), O25(H25), O27(H27), O28(H28), O32(H32),
  O33(H33), O35(H35), O37(H37), O38(H38), O40(H40), O7S(H7S), O11S(H11C),
 O15S(H15S), O3S(H3S), O22S(H22S)
;
