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_4002820
_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 H79 Gd2 N40 O32, C30 H30 N20 O10, 4.05(Cl), H1.5 O, 2.25(O)'
_chemical_formula_sum            'C90 H110.5 Cl4.05 Gd2 N60 O45.25'
_chemical_formula_weight         3214.96
_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                63.31(3)
_cell_angle_beta                 85.66(3)
_cell_angle_gamma                63.71(3)
_cell_formula_units_Z            2
_cell_length_a                   21.596(4)
_cell_length_b                   22.162(4)
_cell_length_c                   22.803(5)
_cell_measurement_reflns_used    10000
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      25.000
_cell_measurement_theta_min      1.064
_cell_volume                     8638(5)
_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 0.921
_diffrn_measured_fraction_theta_max 0.921
_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  0.0769
_diffrn_reflns_av_unetI/netI     0.0715
_diffrn_reflns_Laue_measured_fraction_full 0.921
_diffrn_reflns_Laue_measured_fraction_max 0.921
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            102990
_diffrn_reflns_point_group_measured_fraction_full 0.921
_diffrn_reflns_point_group_measured_fraction_max 0.921
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         1.064
_diffrn_source                   'Australian Synchrotron MX1'
_exptl_absorpt_coefficient_mu    0.905
_exptl_absorpt_correction_T_max  0.4359
_exptl_absorpt_correction_T_min  0.3028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2012/1 (Bruker,2012) was used for absorption correction.
wR2(int) was 0.1512 before and 0.0930 after correction.
The Ratio of minimum to maximum transmission is 0.6947.
The \l/2 correction factor is 0.0015.
;
_exptl_crystal_density_diffrn    1.236
_exptl_crystal_description       prism
_exptl_crystal_F_000             3258
_exptl_crystal_size_max          0.050
_exptl_crystal_size_mid          0.035
_exptl_crystal_size_min          0.020
_refine_diff_density_max         1.999
_refine_diff_density_min         -2.446
_refine_diff_density_rms         0.147
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.033
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1834
_refine_ls_number_reflns         28016
_refine_ls_number_restraints     1935
_refine_ls_restrained_S_all      1.006
_refine_ls_R_factor_all          0.0935
_refine_ls_R_factor_gt           0.0829
_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^)+(0.1512P)^2^+38.2872P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2450
_refine_ls_wR_factor_ref         0.2552
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22867
_reflns_number_total             28016
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            cm7b01751_si_004.cif
_cod_data_source_block           p-1_a_sq
_cod_depositor_comments
'Adding full bibliography for 4002818--4002820.cif.'
_cod_original_cell_volume        8638(4)
_cod_original_formula_sum        'C90 H110.50 Cl4.05 Gd2 N60 O45.25'
_cod_database_code               4002820
_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. Uiso/Uaniso restraints and constraints
Uanis(O44) = Uanis(O45) = Uanis(O47)
3. 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
4. Others
 Fixed Sof: Cl4(0.75) Cl1(0.75) Cl5(0.5) Cl3(0.75) Cl6(0.3) H43D(0.5) O47(0.5)
 O46(0.5) O44(0.75) O45(0.5)
5.a Riding coordinates:
 O5(H5A,H5B), O6(H6A,H6B), O7(H7A,H7B), O8(H8A,H8B), O27(H27A,H27B), O28(H28A,
 H28B), O29(H29A,H29B), O30(H30A,H30B), O31(H31A,H31B), O32(H32A,H32B),
 O43(H43C,H43D)
5.b Ternary CH refined with riding coordinates:
 C2(H2), C4(H4), C7(H7), C10(H10), C13(H13), C16(H16), C21(H21), C23(H23),
 C27(H27), C28(H28), C36(H36), C38(H38), C41(H41), C42(H42), C45(H45), C48(H48),
  C50(H50), C53(H53), C56(H56), C59(H59), C62(H62), C65(H65), C68(H68),
 C76(H76), C78(H78), C81(H81), C82(H82), C86(H86), C87(H87), C90(H90)
5.c Secondary CH2 refined with riding coordinates:
 C5(H5C,H5D), C9(H9A,H9B), C11(H11A,H11B), C15(H15A,H15B), C17(H17A,H17B),
 C19(H19A,H19B), C24(H24A,H24B), C26(H26A,H26B), C29(H29C,H29D), C30(H30C,H30D),
  C32(H32C,H32D), C34(H34A,H34B), C39(H39A,H39B), C43(H43A,H43B), C46(H46A,
 H46B), C52(H52A,H52B), C54(H54A,H54B), C58(H58A,H58B), C60(H60A,H60B),
 C63(H63A,H63B), C67(H67A,H67B), C69(H69A,H69B), C71(H71A,H71B), C73(H73A,H73B),
  C75(H75A,H75B), C79(H79A,H79B), C83(H83A,H83B), C85(H85A,H85B), C88(H88A,H88B)
5.d Aromatic/amide H refined with riding coordinates:
 C51(H51)
;
_shelx_res_checksum              13875
_shelx_hkl_checksum              2569
_shelx_fab_checksum              66748
_olex2_submission_special_instructions 'No special instructions were received'