Rim-differentiated pillar[5]arene-modified surfaces for rapid PFOA/PFOS detection.
Gao, Tu-Nan; Yang, Zhen; Goed, Jesse M. S.; Zuilhof, Han; Miloserdov, Fedor M.; Chemical communications (Cambridge, England) 60 (2024) 9789–9792; doi:10.1039/d4cc02676d

data_7133410
_publ_section_title
;
 Rim-differentiated pillar[5]arene-modified surfaces for rapid PFOA/PFOS
 detection.
;
_journal_issue                   72
_journal_name_full               'Chemical communications (Cambridge, England)'
_journal_page_first              9789
_journal_page_last               9792
_journal_paper_doi               10.1039/d4cc02676d
_journal_volume                  60
_journal_year                    2024
_chemical_formula_moiety
'2(C75 H100 N5 O10), 0.6(C3 H6 O), 4(C2 H6 O), 2(C H4 O), 10(Br), 10.4(H2 O)'
_chemical_formula_sum            'C161.8 H256.4 Br10 N10 O37'
_chemical_formula_weight         3732.85
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2024-05-29 deposited with the CCDC.	2024-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.2663(7)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   26.50453(14)
_cell_length_b                   14.53119(6)
_cell_length_c                   25.82392(16)
_cell_measurement_reflns_used    109448
_cell_measurement_temperature    150(2)
_cell_measurement_theta_max      72.8630
_cell_measurement_theta_min      4.0080
_cell_volume                     9067.12(10)
_computing_cell_refinement       'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 42.94a (release 21-06-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.104a (Rigaku OD, 2023)'
_computing_molecular_graphics
'ORTEP3 for Windows - Farrugia, L. J. J. Appl. Crystallogr. 1997, 30, 565'
_computing_publication_material
;
 'WinGX publication routines, Farrugia, 
 L. J., J. Appl. Crystallogr., 1999, 32, 837-838
;
_computing_structure_refinement
;
 SHELXL-2018/3 (Sheldrick, 2018)
 Sheldrick GM (2008) Acta Crystallogr A64:112--122 and 
 C. B. H\"ubschle, G. M. Sheldrick and B. Dittrich
 ShelXle: a Qt graphical user interface for SHELXL
 J. Appl. Cryst., 44, (2011) 1281-1284.
;
_computing_structure_solution
; 
 SHELXT
 Sheldrick, G. M. (2008). Acta Cryst. A64, 112-122.
;
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.1150
_diffrn_detector_type            EosS2
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.995
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, EosS2'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Cu K\a'
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0449
_diffrn_reflns_av_unetI/netI     0.0163
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.995
_diffrn_reflns_limit_h_max       32
_diffrn_reflns_limit_h_min       -32
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -17
_diffrn_reflns_limit_l_max       27
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            211614
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.995
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         73.117
_diffrn_reflns_theta_min         3.574
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    3.214
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.118
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.104a (Rigaku Oxford Diffraction, 2023)
Numerical absorption correction based on gaussian integration over
a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            colourless
_exptl_crystal_density_diffrn    1.367
_exptl_crystal_description       plate
_exptl_crystal_F_000             3886
_exptl_crystal_size_max          0.768
_exptl_crystal_size_mid          0.426
_exptl_crystal_size_min          0.061
_refine_diff_density_max         1.158
_refine_diff_density_min         -0.776
_refine_diff_density_rms         0.058
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.032
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1294
_refine_ls_number_reflns         18049
_refine_ls_number_restraints     252
_refine_ls_restrained_S_all      1.053
_refine_ls_R_factor_all          0.0395
_refine_ls_R_factor_gt           0.0369
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+9.7309P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0972
_refine_ls_wR_factor_ref         0.0993
_reflns_Friedel_coverage         0.000
_reflns_number_gt                16803
_reflns_number_total             18049
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4cc02676d2.cif
_cod_data_source_block           rd-p5-2
_cod_depositor_comments          'Adding full bibliography for 7133410.cif.'
_cod_original_cell_volume        9067.12(9)
_cod_original_sg_symbol_H-M      'P 21/c'
_cod_original_formula_sum        'C161.80 H256.40 Br10 N10 O37'
_cod_database_code               7133410
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.192
_shelx_estimated_absorpt_t_max   0.828
_oxdiff_exptl_absorpt_empirical_full_min 0.675
_oxdiff_exptl_absorpt_empirical_full_max 2.308
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_shelx_res_checksum              88847
_shelx_hkl_checksum              20081