Colorimetric Determination of Perfluorocarboxylic Acids using Porphyrin Hosts and Mobile Phone Photographs
Taylor, Chloe M.; Breadmore, Michael; Kilah, Nathan Laird; Sensors & Diagnostics  (2023) –; doi:10.1039/D3SD00035D

data_1568722
_publ_section_title
;
 Colorimetric Determination of Perfluorocarboxylic Acids using Porphyrin
 Hosts and Mobile Phone Photographs
;
_journal_name_full               'Sensors &amp; Diagnostics'
_journal_paper_doi               10.1039/D3SD00035D
_journal_year                    2023
_chemical_formula_moiety         'C60 H30 F28 N8 O4, 5(C2 H3 N)'
_chemical_formula_sum            'C70 H45 F28 N13 O4'
_chemical_formula_weight         1664.19
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2021-12-14
_audit_creation_method
;
Olex2 1.2
(compiled May 18 2018 14:05:52 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-12-14 deposited with the CCDC.	2023-03-24 downloaded from the CCDC.
;
_cell_angle_alpha                70.46(3)
_cell_angle_beta                 74.20(3)
_cell_angle_gamma                71.85(3)
_cell_formula_units_Z            2
_cell_length_a                   14.620(3)
_cell_length_b                   14.790(3)
_cell_length_c                   18.860(4)
_cell_measurement_reflns_used    92681
_cell_measurement_temperature    100
_cell_measurement_theta_max      29.213
_cell_measurement_theta_min      1.166
_cell_volume                     3587.1(15)
_computing_cell_refinement       'XDS (Kabsch, 1993)'
_computing_data_collection       'BluIce (McPhillips, 2002)'
_computing_data_reduction        'XDS (Kabsch, 1993)'
_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    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_type            'ADSC Quantum 210r'
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.835
_diffrn_measurement_device_type  'ADSC Quantum 210r'
_diffrn_measurement_method       'Phi Scan'
_diffrn_radiation_monochromator  'Silicon Double Crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           Synchrotron
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0415
_diffrn_reflns_av_unetI/netI     0.0252
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.851
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       20
_diffrn_reflns_limit_k_min       -20
_diffrn_reflns_limit_l_max       24
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            92681
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.851
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.213
_diffrn_reflns_theta_min         1.166
_diffrn_source                   'MX1 Beamline Australian Synchrotron'
_exptl_absorpt_coefficient_mu    0.148
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details   'XDS (Kabsch, 1993)'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.541
_exptl_crystal_density_meas      ?
_exptl_crystal_description       plate
_exptl_crystal_F_000             1680
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: Acetonitrile'
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.05
_exptl_crystal_size_min          0.02
_refine_diff_density_max         0.470
_refine_diff_density_min         -0.528
_refine_diff_density_rms         0.067
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.083
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1193
_refine_ls_number_reflns         16555
_refine_ls_number_restraints     50
_refine_ls_restrained_S_all      1.083
_refine_ls_R_factor_all          0.0587
_refine_ls_R_factor_gt           0.0467
_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^)+(0.0724P)^2^+1.3670P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1379
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14708
_reflns_number_total             16555
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d3sd00035d1.cif
_cod_data_source_block           asp0441_10_merged
_cod_depositor_comments
;
The following automatic conversions were performed:

data item '_exptl_crystal_density_meas' value 'not measured' was
changed to '?' -- the value is perceived as not measured.

Automatic conversion script
Id: cif_fix_values 7556 2019-12-06 15:28:31Z antanas 
;
_cod_original_cell_volume        3587.0(16)
_cod_database_code               1568722
_shelx_shelxl_version_number     2018/3
_shelx_estimated_absorpt_t_max   0.997
_shelx_estimated_absorpt_t_min   0.993
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 F23-C21 \\sim F23A-C21A
 with sigma of 0.02
 F24-C22 \\sim F24A-C22A
 with sigma of 0.02
 F22-C21 \\sim F22A-C21A
 with sigma of 0.02
 C20-C21 \\sim C20-C21A
 with sigma of 0.02
 F25-C22 \\sim F25A-C22A
 with sigma of 0.02
 F26-C22 \\sim F26A-C22A
 with sigma of 0.02
 C22-C21 \\sim C22A-C21A
 with sigma of 0.02
 F23-F22 \\sim F23A-F22A
 with sigma of 0.04
 F23-C20 \\sim F23A-C20
 with sigma of 0.04
 F23-C22 \\sim F23A-C22A
 with sigma of 0.04
 F24-F25 \\sim F24A-F25A
 with sigma of 0.04
 F24-F26 \\sim F24A-F26A
 with sigma of 0.04
 F24-C21 \\sim F24A-C21A
 with sigma of 0.04
 F22-C20 \\sim F22A-C20
 with sigma of 0.04
 F22-C22 \\sim F22A-C22A
 with sigma of 0.04
 C20-C22 \\sim C20-C22A
 with sigma of 0.04
 F25-F26 \\sim F25A-F26A
 with sigma of 0.04
 F25-C21 \\sim F25A-C21A
 with sigma of 0.04
 F26-C21 \\sim F26A-C21A
 with sigma of 0.04
 F42-C41 \\sim F42A-C41A
 with sigma of 0.02
 F43-C41 \\sim F43A-C41A
 with sigma of 0.02
 F46-C42 \\sim F46A-C42A
 with sigma of 0.02
 C40-C41 \\sim C40-C41A
 with sigma of 0.02
 C41-C42 \\sim C41A-C42A
 with sigma of 0.02
 F45-C42 \\sim F45A-C42A
 with sigma of 0.02
 C42-F44 \\sim C42A-F44A
 with sigma of 0.02
 F42-F43 \\sim F42A-F43A
 with sigma of 0.04
 F42-C40 \\sim F42A-C40
 with sigma of 0.04
 F42-C42 \\sim F42A-C42A
 with sigma of 0.04
 F43-C40 \\sim F43A-C40
 with sigma of 0.04
 F43-C42 \\sim F43A-C42A
 with sigma of 0.04
 F46-C41 \\sim F46A-C41A
 with sigma of 0.04
 F46-F45 \\sim F46A-F45A
 with sigma of 0.04
 F46-F44 \\sim F46A-F44A
 with sigma of 0.04
 C40-C42 \\sim C40-C42A
 with sigma of 0.04
 C41-F45 \\sim C41A-F45A
 with sigma of 0.04
 C41-F44 \\sim C41A-F44A
 with sigma of 0.04
 F45-F44 \\sim F45A-F44A
 with sigma of 0.04
3. Uiso/Uaniso restraints and constraints
C64 \\sim C63 \\sim N62: within 2A with sigma of 0.04 and sigma for terminal
atoms of 0.08
4. Others
 Sof(F22A)=Sof(C21A)=Sof(F23A)=Sof(C22A)=Sof(F26A)=Sof(F24A)=Sof(F25A)=1-FVAR(1)
 Sof(F23)=Sof(F24)=Sof(F22)=Sof(F25)=Sof(F26)=Sof(C22)=Sof(C21)=FVAR(1)
 Sof(F42A)=Sof(C41A)=Sof(F43A)=Sof(F44A)=Sof(C42A)=Sof(F46A)=Sof(F45A)=1-FVAR(2)
 Sof(F42)=Sof(F43)=Sof(F46)=Sof(C41)=Sof(F45)=Sof(C42)=Sof(F44)=FVAR(2)
5.a Aromatic/amide H refined with riding coordinates:
 C404(H404), C203(H203), C403(H403), C104(H104), C208(H208), C303(H303),
 C204(H204), C103(H103), C308(H308), C304(H304), C108(H108), C411(H411),
 C309(H309), C111(H111), C209(H209), C211(H211), C311(H311), C408(H408),
 C310(H310), C210(H210), C109(H109), C410(H410), C110(H110), C409(H409)
5.b Idealised Me refined as rotating group:
 C61(H61A,H61B,H61C), C58(H58A,H58B,H58C), C55(H55A,H55B,H55C), C52(H52A,H52B,
 H52C), C64(H64A,H64B,H64C)
;
_shelx_res_checksum              83473
_shelx_hkl_checksum              61271
_olex2_submission_special_instructions 'No special instructions were received'