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_4002833
_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 H72 Ce2 N40 O30, C30 H30 N20 O10, 4(Cl), H2 O, 16.5(O)'
_chemical_formula_sum            'C90 H104 Ce2 Cl4 N60 O57.5'
_chemical_formula_weight         3368.37
_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                71.45(3)
_cell_angle_beta                 66.73(3)
_cell_angle_gamma                74.75(3)
_cell_formula_units_Z            2
_cell_length_a                   20.852(4)
_cell_length_b                   21.303(4)
_cell_length_c                   22.769(5)
_cell_measurement_reflns_used    10000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      24.999
_cell_measurement_theta_min      1.021
_cell_volume                     8699(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 0.916
_diffrn_measured_fraction_theta_max 0.916
_diffrn_measurement_device_type  'ADSC Quantum Detector'
_diffrn_measurement_method       '\p  scans'
_diffrn_radiation_type
'silicon double crystal monochromated synchrotron'
_diffrn_radiation_wavelength     0.7108
_diffrn_reflns_av_R_equivalents  0.0685
_diffrn_reflns_av_unetI/netI     0.0586
_diffrn_reflns_Laue_measured_fraction_full 0.916
_diffrn_reflns_Laue_measured_fraction_max 0.916
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -24
_diffrn_reflns_limit_k_max       25
_diffrn_reflns_limit_k_min       -25
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            107876
_diffrn_reflns_point_group_measured_fraction_full 0.916
_diffrn_reflns_point_group_measured_fraction_max 0.916
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.021
_diffrn_source                   'Australian Synchrotron MX1'
_exptl_absorpt_coefficient_mu    0.668
_exptl_absorpt_correction_T_max  0.8624
_exptl_absorpt_correction_T_min  0.7318
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1337 before and 0.0717 after correction.
The Ratio of minimum to maximum transmission is 0.8486.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.286
_exptl_crystal_description       prism
_exptl_crystal_F_000             3415
_exptl_crystal_size_max          0.120
_exptl_crystal_size_mid          0.060
_exptl_crystal_size_min          0.045
_refine_diff_density_max         2.110
_refine_diff_density_min         -1.718
_refine_diff_density_rms         0.147
_refine_ls_extinction_coef       0.00036(17)
_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   1.050
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1946
_refine_ls_number_reflns         28066
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.050
_refine_ls_R_factor_all          0.0975
_refine_ls_R_factor_gt           0.0790
_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^)+(0.1527P)^2^+32.2112P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2363
_refine_ls_wR_factor_ref         0.2519
_reflns_Friedel_coverage         0.000
_reflns_number_gt                21297
_reflns_number_total             28066
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm7b01751_si_003.cif
_cod_data_source_block           p-1_sq
_cod_original_formula_sum        'C90 H104 Ce2 Cl4 N60 O57.50'
_cod_database_code               4002833
_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. Others
 Fixed Sof: Cl4(0.5) Cl5(0.5) Cl6(0.5) O59(0.5) O42(0.5) O43(0.5) O44(0.5)
 O45(0.5)
3.a Riding coordinates:
 O21(H21A,H21B), O22(H22A,H22B), O23(H23A,H23B), O24(H24A,H24B), O26(H26A,
 H26B), O27(H27A,H27B), O41(H41A,H41B)
3.b Ternary CH refined with riding coordinates:
 C13(H13), C15(H15), C18(H18), C19(H19), C22(H22), C25(H25), C27(H27),
 C29(H29), C33(H33), C35(H35), C40(H40), C42(H42), C45(H45), C46(H46), C49(H49),
  C50(H50), C53(H53), C54(H54), C58(H58), C60(H60), C62(H62), C64(H64),
 C67(H67), C69(H69), C73(H73), C75(H75), C79(H79), C81(H81), C85(H85), C87(H87)
3.c Secondary CH2 refined with riding coordinates:
 C2(H2A,H2B), C4(H4A,H4B), C6(H6A,H6B), C9(H9A,H9B), C11(H11A,H11B), C16(H16A,
 H16B), C20(H20A,H20B), C23(H23C,H23D), C28(H28A,H28B), C30(H30A,H30B),
 C32(H32A,H32B), C36(H36A,H36B), C37(H37A,H37B), C39(H39A,H39B), C43(H43A,H43B),
  C47(H47A,H47B), C51(H51A,H51B), C55(H55A,H55B), C57(H57A,H57B), C59(H59A,
 H59B), C65(H65A,H65B), C70(H70A,H70B), C71(H71A,H71B), C76(H76A,H76B),
 C77(H77A,H77B), C82(H82A,H82B), C83(H83A,H83B), C88(H88A,H88B), C89(H89A,H89B),
  C90(H90A,H90B)
;
_shelx_res_checksum              58154
_shelx_hkl_checksum              77150
_shelx_fab_checksum              35451
_olex2_submission_special_instructions 'No special instructions were received'