Cucurbit[7]uril-based carbon dots for recognizing histamine
Hu, Jian-Hang; Wang, Cheng-Hui; Bai, Qing-hong; Chen, Lixia; Zhao, anting; Yuan, Shang-Wei; Chen, Qing; Ma, PeiHua; Tao, Zhu; Xiao, Xin; Chemical Communications  (2023) –; doi:10.1039/D3CC03750A

data_7132292
_publ_section_title
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 Cucurbit[7]uril-based carbon dots for recognizing histamine
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_journal_name_full               'Chemical Communications'
_journal_paper_doi               10.1039/D3CC03750A
_journal_year                    2023
_chemical_formula_moiety
'2(Cd Cl4), C42 H48 Ca N28 O17, C5 H9 O4, 12[H2O]'
_chemical_formula_sum            'C47 H81 Ca Cd2 Cl8 N28 O33'
_chemical_formula_weight         1898.68
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-09-12
_audit_creation_method
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Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
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_audit_update_record
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2023-09-12 deposited with the CCDC.	2023-11-01 downloaded from the CCDC.
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_cell_angle_alpha                90
_cell_angle_beta                 94.92(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   16.852(3)
_cell_length_b                   17.108(3)
_cell_length_c                   29.168(6)
_cell_measurement_reflns_used    9388
_cell_measurement_temperature    273.15
_cell_measurement_theta_max      28.09
_cell_measurement_theta_min      2.42
_cell_volume                     8378(3)
_computing_cell_refinement       'SAINT V8.38A (Bruker, 2018)'
_computing_data_reduction        'SAINT V8.38A (Bruker, 2018)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      273.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.992
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0809
_diffrn_reflns_av_unetI/netI     0.0450
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.992
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       24
_diffrn_reflns_limit_k_min       -23
_diffrn_reflns_limit_l_max       41
_diffrn_reflns_limit_l_min       -41
_diffrn_reflns_number            254259
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.992
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         30.387
_diffrn_reflns_theta_min         2.268
_diffrn_source_current           1.4
_diffrn_source_power             0.07
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.901
_exptl_absorpt_correction_T_max  0.7460
_exptl_absorpt_correction_T_min  0.6354
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
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SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1340 before and 0.0780 after correction.
The Ratio of minimum to maximum transmission is 0.8517.
The \l/2 correction factor is Not present.
;
_exptl_crystal_colour            'clear light colourless'
_exptl_crystal_colour_lustre     clear
_exptl_crystal_colour_modifier   light
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.505
_exptl_crystal_description       block
_exptl_crystal_F_000             3820
_exptl_crystal_size_max          0.22
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.12
_refine_diff_density_max         1.218
_refine_diff_density_min         -1.214
_refine_diff_density_rms         0.149
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.024
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     972
_refine_ls_number_reflns         25102
_refine_ls_number_restraints     9
_refine_ls_restrained_S_all      1.024
_refine_ls_R_factor_all          0.1111
_refine_ls_R_factor_gt           0.0949
_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^)+(0.1004P)^2^+61.8883P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2506
_refine_ls_wR_factor_ref         0.2609
_reflns_Friedel_coverage         0.000
_reflns_number_gt                19379
_reflns_number_total             25102
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3cc03750a2.cif
_cod_data_source_block           a_pl_sq
_cod_database_code               7132292
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.900
_shelx_estimated_absorpt_t_min   0.826
_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 C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 Ca03-H20B \\sim Ca03-H20A
 with sigma of 0.02
 Ca03-H21A \\sim Ca03-H21B
 with sigma of 0.02
 Ca03-H19A \\sim Ca03-H19B
 with sigma of 0.02
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
 O17
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
5.a Riding coordinates:
 O20(H20A,H20B)
5.b Free rotating group:
 O21(H21A,H21B), O19(H19A,H19B)
5.c Ternary CH refined with riding coordinates:
 C21(H21), C23(H23), C25(H25), C20(H20), C18(H18), C22(H22), C24(H24),
 C19(H19), C16(H16), C26(H26), C27(H27), C17(H17), C28(H28), C15(H15)
5.d Secondary CH2 refined with riding coordinates:
 C36(H36A,H36B), C10(H10A,H10B), C8(H8A,H8B), C38(H38A,H38B), C2(H2A,H2B),
 C6(H6A,H6B), C30(H30A,H30B), C42(H42A,H42B), C34(H34A,H34B), C32(H32A,H32B),
 C40(H40A,H40B), C12(H12A,H12B), C4(H4A,H4B), C14(H14A,H14B), C43(H43A,H43B)
5.e Aromatic/amide H refined with riding coordinates:
 C46(H46)
5.f Tetrahedral OH refined with riding coordinates:
 O16(H16A), O17(H17A)
5.g Idealised Me refined as rotating group:
 C47(H47A,H47B,H47C)
5.h Idealised tetrahedral OH refined as rotating group:
 O18(H18A)
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_smtbx_masks_special_details
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A solvent mask was calculated and 488 electrons were 
found in a volume of 1976\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
12[H2O] per Asymmetric Unit 
which account for 480 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              95238
_shelx_hkl_checksum              13828
_shelx_fab_checksum              27314
_platon_squeeze_special_details
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A solvent mask was calculated and 592 electrons were 
found in a volume of 1928\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
12[H2O] per Asymmetric Unit 
which account for 560 electrons 
per unit cell.
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'