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_1572379
_publ_section_title
;
 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         '0.5(C2 H4 Cl4), C51 H51 N3 O12'
_chemical_formula_sum            'C52 H53 Cl2 N3 O12'
_chemical_formula_weight         982.87
_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             2019-12-03
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-01-04 deposited with the CCDC.	2024-08-15 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.3280(10)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.6288(6)
_cell_length_b                   14.0186(4)
_cell_length_c                   17.8883(5)
_cell_measurement_reflns_used    8947
_cell_measurement_temperature    99.23
_cell_measurement_theta_max      59.115
_cell_measurement_theta_min      3.743
_cell_volume                     5498.1(3)
_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  'XL (Sheldrick, 2008)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      99.23
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0373
_diffrn_reflns_av_unetI/netI     0.0335
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       24
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            15554
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        59.181
_diffrn_reflns_theta_max         59.181
_diffrn_reflns_theta_min         2.549
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.554
_exptl_absorpt_correction_T_max  0.7516
_exptl_absorpt_correction_T_min  0.5836
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0915 before and 0.0558 after correction. The Ratio of minimum to maximum transmission is 0.7765. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            colourless
_exptl_crystal_colour_primary    colourless
_exptl_crystal_density_diffrn    1.187
_exptl_crystal_description       block
_exptl_crystal_F_000             2064
_exptl_crystal_size_max          0.3
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.542
_refine_diff_density_min         -0.377
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.082
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     338
_refine_ls_number_reflns         4143
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.082
_refine_ls_R_factor_all          0.0735
_refine_ls_R_factor_gt           0.0613
_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^)+(0.0469P)^2^+30.1351P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1531
_refine_ls_wR_factor_ref         0.1615
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3383
_reflns_number_total             4143
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4sc04950k2.cif
_cod_data_source_block           c2m
_cod_depositor_comments
'Adding full bibliography for 1572379--1572380.cif.'
_cod_database_code               1572379
_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
 At 1.5 times of:
  All C(H,H,H) groups
2. Others
 Sof(O6A)=1-FVAR(1)
 Sof(O6B)=FVAR(1)
 Fixed Sof: H28A(0.5) H28B(0.5)
3.a Secondary CH2 refined with riding coordinates:
 C11(H11A,H11B), C13(H13A,H13B), C23(H23A,H23B), C28(H28A,H28B), C18(H18A,
 H18B), C7(H7A,H7B), C9(H9A,H9B)
3.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C17(H17), C21(H21), C22(H22), C26(H26), C27(H27)
3.c Idealised Me refined as rotating group:
 C12(H12A,H12B,H12C), C8(H8A,H8B,H8C), C10(H10A,H10B,H10C)
;
_shelx_res_checksum              16560
_shelx_fab_checksum              31343
_olex2_submission_special_instructions 'No special instructions were received'