An <i>endo</i>-functionalized molecular cage for selective potentiometric determination of creatinine.
Lu, Yu; Wang, Song-Meng; He, Sui-Sui; Huang, Qicheng; Zhao, Cheng-Da; Yu, Shan; Jiang, Wei; Yao, Huan; Wang, Li-Li; Yang, Liu-Pan; Chemical science 15 (2024) 14791–14797; doi:10.1039/d4sc04950k

data_1572380
_publ_section_title
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 An <i>endo</i>-functionalized molecular cage for selective potentiometric
 determination of creatinine.
;
_journal_issue                   36
_journal_name_full               'Chemical science'
_journal_page_first              14791
_journal_page_last               14797
_journal_paper_doi               10.1039/d4sc04950k
_journal_volume                  15
_journal_year                    2024
_chemical_formula_moiety         '1.5(C2 H4 Cl4), C54 H54 O12'
_chemical_formula_sum            'C57 H60 Cl6 O12'
_chemical_formula_weight         1149.75
_space_group_crystal_system      monoclinic
_space_group_IT_number           12
_space_group_name_Hall           '-C 2y'
_space_group_name_H-M_alt        'C 1 2/m 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-04-26
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-06-05 deposited with the CCDC.	2024-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 102.595(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.161(2)
_cell_length_b                   14.1881(13)
_cell_length_c                   17.9966(17)
_cell_measurement_reflns_used    9920
_cell_measurement_temperature    100.00
_cell_measurement_theta_max      56.90
_cell_measurement_theta_min      3.24
_cell_volume                     5522.4(9)
_computing_cell_refinement       'SAINT V8.40B (?, 2016)'
_computing_data_reduction        'SAINT V8.40B (?, 2016)'
_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    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100.00
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.995
_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           GaK\a
_diffrn_radiation_wavelength     1.34139
_diffrn_reflns_av_R_equivalents  0.0691
_diffrn_reflns_av_unetI/netI     0.0544
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -27
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_number            35409
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        53.594
_diffrn_reflns_theta_max         57.017
_diffrn_reflns_theta_min         3.241
_diffrn_source                   'microfocus sealed X-ray tube'
_diffrn_source_current           3.0
_diffrn_source_power             0.20955
_diffrn_source_type              'Incoatec I\ms'
_diffrn_source_voltage           69.85
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    2.215
_exptl_absorpt_correction_T_max  0.7430
_exptl_absorpt_correction_T_min  0.6192
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2016/2 (Bruker,2016/2) was used for absorption correction.
wR2(int) was 0.1477 before and 0.1039 after correction.
The Ratio of minimum to maximum transmission is 0.8334.
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    1.383
_exptl_crystal_description       block
_exptl_crystal_F_000             2400
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.15
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.497
_refine_diff_density_min         -0.795
_refine_diff_density_rms         0.074
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.061
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     364
_refine_ls_number_reflns         5888
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.061
_refine_ls_R_factor_all          0.0478
_refine_ls_R_factor_gt           0.0426
_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^)+(0.0675P)^2^+3.9399P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1160
_refine_ls_wR_factor_ref         0.1204
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5162
_reflns_number_total             5888
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04950k2.cif
_cod_data_source_block           c2m_CCDC1
_cod_depositor_comments
'Adding full bibliography for 1572379--1572380.cif.'
_cod_database_code               1572380
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.809
_shelx_estimated_absorpt_t_min   0.691
_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
2. Others
 Fixed Sof: H33A(0.5) H33B(0.5) H32A(0.5) H32B(0.5) H31A(0.5) H31B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C25(H25A,H25B), C13(H13A,H13B), C6(H6A,H6B), C23(H23A,H23B), C15(H15A,H15B),
 C17(H17A,H17B), C33(H33A,H33B), C32(H32A,H32B), C31(H31A,H31B)
3.b Aromatic/amide H refined with riding coordinates:
 C20(H20), C28(H28), C4(H4), C21(H21), C1(H1), C30(H30), C29(H29), C2(H2),
 C22(H22)
3.c Idealised Me refined as rotating group:
 C14(H14A,H14B,H14C), C24(H24A,H24B,H24C), C16(H16A,H16B,H16C)
;
_olex2_submission_special_instructions 'No special instructions were received'