Cucurbit[10]uril-Based Smart Supramolecular Organic Frameworks in Selective Isolation of Metal Cations
Yao, Yu-Qing; Zhang, Ying-Jie; Huang, Chao; Zhu, Qian-Jiang; Tao, Zhu; Ni, Xin-Long; Wei, Gang; Chemistry of Materials 29 (2017) 5468–; doi:10.1021/acs.chemmater.7b01751

data_4002819
_publ_section_title
;
 Cucurbit[10]uril-Based Smart Supramolecular Organic Frameworks in
 Selective Isolation of Metal Cations
;
_journal_issue                   13
_journal_name_full               'Chemistry of Materials'
_journal_page_first              5468
_journal_paper_doi               10.1021/acs.chemmater.7b01751
_journal_volume                  29
_journal_year                    2017
_chemical_formula_moiety
'C60 H68 Ba2 N40 O24, C30 H30 N20 O10, 4(Cl), 6.5(O)'
_chemical_formula_sum            'C90 H98 Ba2 Cl4 N60 O40.5'
_chemical_formula_weight         3084.74
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2017-03-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.03.02 svn.r3394 for OlexSys, GUI svn.r5324)
;
_cell_angle_alpha                71.16(3)
_cell_angle_beta                 67.42(3)
_cell_angle_gamma                75.08(3)
_cell_formula_units_Z            2
_cell_length_a                   20.918(4)
_cell_length_b                   21.165(4)
_cell_length_c                   23.176(5)
_cell_measurement_reflns_used    10000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.999
_cell_measurement_theta_min      0.983
_cell_volume                     8861(4)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BlueIce (McPhillips, et al., 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_measured_fraction_theta_full 0.919
_diffrn_measured_fraction_theta_max 0.919
_diffrn_measurement_device_type  'ADSC Quantum Detector'
_diffrn_measurement_method       '\p  scans'
_diffrn_radiation_type
'silicon double crystal monochromated synchrotron'
_diffrn_radiation_wavelength     0.71081
_diffrn_reflns_av_R_equivalents  0.1103
_diffrn_reflns_av_unetI/netI     0.0914
_diffrn_reflns_Laue_measured_fraction_full 0.919
_diffrn_reflns_Laue_measured_fraction_max 0.919
_diffrn_reflns_limit_h_max       23
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            107713
_diffrn_reflns_point_group_measured_fraction_full 0.919
_diffrn_reflns_point_group_measured_fraction_max 0.919
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         0.983
_diffrn_source                   'Australian Synchrotron MX1'
_exptl_absorpt_coefficient_mu    0.578
_exptl_absorpt_correction_T_max  0.4359
_exptl_absorpt_correction_T_min  0.2876
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1751 before and 0.0928 after correction.
The Ratio of minimum to maximum transmission is 0.6598.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.156
_exptl_crystal_description       prism
_exptl_crystal_F_000             3123
_exptl_crystal_size_max          0.025
_exptl_crystal_size_mid          0.020
_exptl_crystal_size_min          0.015
_refine_diff_density_max         3.424
_refine_diff_density_min         -2.526
_refine_diff_density_rms         0.189
_refine_ls_extinction_coef       0.0053(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   1.158
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1844
_refine_ls_number_reflns         28664
_refine_ls_number_restraints     1773
_refine_ls_restrained_S_all      1.128
_refine_ls_R_factor_all          0.1981
_refine_ls_R_factor_gt           0.1638
_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^)+(0.2055P)^2^+75.2000P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.4240
_refine_ls_wR_factor_ref         0.4507
_reflns_Friedel_coverage         0.000
_reflns_number_gt                18543
_reflns_number_total             28664
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm7b01751_si_001.cif
_cod_data_source_block           sadabs_sq
_cod_depositor_comments
'Adding full bibliography for 4002818--4002820.cif.'
_cod_original_formula_sum        'C90 H98 Ba2 Cl4 N60 O40.50'
_cod_database_code               4002819
_shelx_shelxl_version_number     2014/7
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H) groups
2. Rigid body (RIGU) restrains
 All non-hydrogen atoms
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
3. Others
 Fixed Sof: O11(0.5) H11A(0.5) H11B(0.5) O12(0.5) H12A(0.5) H12B(0.5) O13(0.5)
 H13A(0.5) H13B(0.5) O14(0.5) H14A(0.5) H14B(0.5) O25(0.5) H25A(0.5) H25B(0.5)
 O26(0.5) H26A(0.5) H26B(0.5) O27(0.5) H27A(0.5) H27B(0.5) O28(0.5) H28A(0.5)
 H28B(0.5) Cl1(0.5) Cl2(0.5) O30(0.5) Cl6(0.5) O42(0.5) O46(0.5) O47(0.5)
 O43(0.5)
4.a Riding coordinates:
 O11(H11A,H11B), O12(H12A,H12B), O13(H13A,H13B), O14(H14A,H14B), O25(H25A,
 H25B), O26(H26A,H26B), O27(H27A,H27B), O28(H28A,H28B)
4.b Ternary CH refined with riding coordinates:
 C4(H4), C6(H6), C9(H9), C16(H16), C18(H18), C22(H22), C23(H23), C26(H26),
 C27(H27), C28(H28), C33(H33), C43(H43), C45(H45), C48(H48), C49(H49), C52(H52),
  C53(H53), C56(H56), C57(H57), C59(H59), C62(H62), C64(H64), C68(H68),
 C71(H71), C74(H74), C77(H77), C83(H83), C85(H85), C89(H89), C90(H90)
4.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C7(H7A,H7B), C10(H10A,H10B), C12(H12C,H12D), C15(H15A,H15B),
 C19(H19A,H19B), C21(H21A,H21B), C24(H24A,H24B), C29(H29A,H29B), C30(H30A,H30B),
  C32(H32A,H32B), C35(H35A,H35B), C37(H37A,H37B), C39(H39A,H39B), C41(H41A,
 H41B), C46(H46A,H46B), C50(H50A,H50B), C54(H54A,H54B), C58(H58A,H58B),
 C60(H60A,H60B), C65(H65A,H65B), C66(H66A,H66B), C70(H70A,H70B), C72(H72A,H72B),
  C76(H76A,H76B), C78(H78A,H78B), C80(H80A,H80B), C82(H82A,H82B), C86(H86A,
 H86B), C88(H88A,H88B)
;
_shelx_res_checksum              89604
_shelx_hkl_checksum              65847
_shelx_fab_checksum              43716
_olex2_submission_special_instructions 'No special instructions were received'