Selective recognition of aluminum ions using an esculetin@Q[8] host–guest supramolecular fluorescent probe
Luo, Guangyan; Meng, Ye; Zhang, Lin; Li, Xiaoyue; Tao, Zhu; Zhang, Qianjun; New Journal of Chemistry 46 (2022) 97–102; doi:10.1039/D1NJ04782E

data_7061068
_publ_section_title
;
 Selective recognition of aluminum ions using an esculetin@Q[8]
 host--guest supramolecular fluorescent probe
;
_journal_issue                   1
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              97
_journal_page_last               102
_journal_paper_doi               10.1039/D1NJ04782E
_journal_volume                  46
_journal_year                    2022
_chemical_formula_moiety
'2(C48 H48 N32 O16), C18 H12 Al O10, 11(O), 4(Cl)'
_chemical_formula_sum            'C114 H108 Al Cl4 N64 O53'
_chemical_formula_weight         3391.42
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-I 2yc'
_space_group_name_H-M_alt        'I 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2021-05-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-07-17 deposited with the CCDC.	2021-11-17 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.21(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   28.162(9)
_cell_length_b                   22.226(7)
_cell_length_c                   28.390(8)
_cell_measurement_reflns_used    9745
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      28.066
_cell_measurement_theta_min      2.328
_cell_volume                     17770(9)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device       'three-circle diffractometer'
_diffrn_measurement_device_type  'Bruker SMART APEX2 area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'mirror optics'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.1563
_diffrn_reflns_av_unetI/netI     0.0620
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       37
_diffrn_reflns_limit_h_min       -37
_diffrn_reflns_limit_k_max       29
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       37
_diffrn_reflns_limit_l_min       -37
_diffrn_reflns_number            359667
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.335
_diffrn_reflns_theta_min         2.328
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.164
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6414
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1240 before and 0.0789 after correction.
The Ratio of minimum to maximum transmission is 0.8601.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.268
_exptl_crystal_description       block
_exptl_crystal_F_000             6980
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.2
_refine_diff_density_max         1.749
_refine_diff_density_min         -1.645
_refine_diff_density_rms         0.116
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.421
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1066
_refine_ls_number_reflns         22095
_refine_ls_number_restraints     1050
_refine_ls_restrained_S_all      1.414
_refine_ls_R_factor_all          0.1835
_refine_ls_R_factor_gt           0.1225
_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^)+(0.2000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.3810
_refine_ls_wR_factor_ref         0.4208
_reflns_Friedel_coverage         0.000
_reflns_number_gt                11778
_reflns_number_total             22095
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d1nj04782e2.cif
_cod_data_source_block           a_a_pl_sq
_cod_depositor_comments          'Adding full bibliography for 7061068.cif.'
_cod_database_code               7061068
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.968
_shelx_estimated_absorpt_t_min   0.952
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 H20-C53
 2.46 with sigma of 0.001
 O2W-O14
 2.65 with sigma of 0.001
 O2W-O1W
 2.56 with sigma of 0.001
3. Uiso/Uaniso restraints and constraints
Uanis(O17) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 O18, C49, C50, C51, C52, C57
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 Al01, O1W
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O9, O10, O11, O12, O13, O14, O15, O16, N1, N2, N3, N4, N5, N6, N7, N8, N9,
 N10, N11, N12, N13, N14, N15, N16, C1, C2, C3, C4, C5, C6, C7, C8, C9, C10,
 C11, C12, C13, C14, C15, C16, C17, C18, C19, C20, C21, C22, C23, C24, H5A, H5B,
  H13, H19A, H19B, H11, H15, H14, H3A, H3B, H12, H16, H7A, H7B, H10, H21A, H21B,
  H17A, H17B, H1A, H1B, H23A, H23B, H9, O1, O2, O3, O4, O5, O6, O7, O8, N17,
 N18, N19, N20, N21, N22, N23, N24, N25, N26, N27, N28, N29, N30, N31, N32, C25,
  C26, C27, C28, C29, C30, C31, C32, C33, C34, C35, C36, C37, C38, C39, C40,
 C41, C42, C43, C44, C45, C46, C47, C48, H29A, H29B, H38, H35, H37, H36, H34,
 H27A, H27B, H47A, H47B, H43A, H43B, H33, H39, H40, H31A, H31B, H45A, H45B,
 H41A, H41B, H25A, H25B, Al01, O1W, O18, O19, O20, C49, C50, C51, C52, C53, C54,
  C55, C56, C57, H19, H20, H53, H56, O2W, Cl2, Cl1, O04W, O3W
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O17
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
5.a Ternary CH refined with riding coordinates:
 C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C16(H16),
 C33(H33), C34(H34), C35(H35), C36(H36), C37(H37), C38(H38), C39(H39), C40(H40)
5.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C3(H3A,H3B), C5(H5A,H5B), C7(H7A,H7B), C17(H17A,H17B), C19(H19A,
 H19B), C21(H21A,H21B), C23(H23A,H23B), C25(H25A,H25B), C27(H27A,H27B),
 C29(H29A,H29B), C31(H31A,H31B), C41(H41A,H41B), C43(H43A,H43B), C45(H45A,H45B),
  C47(H47A,H47B)
5.c Aromatic/amide H refined with riding coordinates:
 C50(H50), C51(H51), C53(H53), C56(H56)
5.d Idealised tetrahedral OH refined as rotating group:
 O19(H19), O20(H20)
;
_shelx_res_checksum              29343
_shelx_fab_checksum              54597
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'