Surface-Enhanced Raman Scattering of Phenols and Catechols by a Molecular Analogue of Titanium Dioxide.
Liu, Caiyun; Hu, Junyi; Biswas, Subharanjan; Zhu, Feng; Zhan, Jinhua; Wang, Guo; Tung, Chen-Ho; Wang, Yifeng; Analytical chemistry 92 (2020) 5929–5936; doi:10.1021/acs.analchem.0c00047

data_1557785
_publ_section_title
;
 Surface-Enhanced Raman Scattering of Phenols and Catechols by a Molecular
 Analogue of Titanium Dioxide.
;
_journal_issue                   8
_journal_name_full               'Analytical chemistry'
_journal_page_first              5929
_journal_page_last               5936
_journal_paper_doi               10.1021/acs.analchem.0c00047
_journal_volume                  92
_journal_year                    2020
_chemical_formula_moiety         '0.5(C96 H204 O92 Ti34)'
_chemical_formula_sum            'C69 H154 O47 Ti17'
_chemical_formula_weight         2545.17
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-05-05
_audit_creation_method
;
Olex2 1.2-beta
(compiled 2018.04.26 svn.r3504 for OlexSys, GUI svn.r5492)
;
_cell_angle_alpha                90
_cell_angle_beta                 97.765(2)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.4736(19)
_cell_length_b                   24.012(2)
_cell_length_c                   20.6252(17)
_cell_measurement_reflns_used    3289
_cell_measurement_temperature    173
_cell_measurement_theta_max      21.22
_cell_measurement_theta_min      2.49
_cell_volume                     11028.0(16)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      173
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 1.000
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0815
_diffrn_reflns_av_unetI/netI     0.0809
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       21
_diffrn_reflns_limit_h_min       -20
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            22058
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        19.780
_diffrn_reflns_theta_max         19.780
_diffrn_reflns_theta_min         1.247
_exptl_absorpt_coefficient_mu    1.234
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.533
_exptl_crystal_description       block
_exptl_crystal_F_000             5252
_exptl_transmission_factor_max   0.7447
_exptl_transmission_factor_min   0.6177
_platon_squeeze_details
;
TITL c2c       C 1 2/c 1    R = 0.09
CELL   22.4736   24.0120   20.6252     90.00     97.76     90.00
SPGR C2/c
Q101 0.399 0.088 0.952 !       2.31 eA-3
Q102 0.147 0.457 0.046 !       2.20 eA-3
Q103 0.055 0.432 0.982 !       1.95 eA-3
Q104 0.898 0.084 0.448 !       1.80 eA-3
Q105 0.336 0.440 0.938 !       1.65 eA-3
Q106 0.421 0.429 0.019 !       1.63 eA-3
Q107 0.420 0.042 0.931 !       1.58 eA-3
Q108 0.500 0.056 0.260 !       1.47 eA-3
Q109 0.499 0.059 0.214 !       1.47 eA-3
Q110 0.914 0.047 0.419 !       1.46 eA-3
Q111 1.001 0.048 0.736 !       1.38 eA-3
Q112 0.468 0.414 0.256 !       1.37 eA-3
Q113 0.951 0.474 0.806 !       1.37 eA-3
Q114 0.852 0.033 0.426 !       1.27 eA-3
Q115 0.452 0.424 0.300 !       1.19 eA-3
Q116 0.447 0.087 0.277 !       1.18 eA-3
Q117 0.943 0.478 0.301 !       1.17 eA-3
Q118 0.545 0.084 0.259 !       1.14 eA-3
Q119 0.048 0.021 0.016 !       1.14 eA-3
C120 0.537 0.016 0.122 !       1.14 eA-3
Q121 0.547 0.456 0.172 !       1.13 eA-3
Q122 0.500 0.102 0.252 !       1.12 eA-3
Q123 0.109 0.002 0.124 !       1.10 eA-3
Q124 0.877 0.017 0.394 !       1.07 eA-3
Q125 0.914 0.488 0.889 !       1.00 eA-3
Q126 0.367 0.009 0.885 !       0.93 eA-3
Q127 0.032 0.490 0.257 !       0.85 eA-3
C128 0.407 0.087 0.232 !       0.83 eA-3
C129 0.512 0.058 0.373 !       0.79 eA-3
Q130 0.718 0.345 0.235 !       0.77 eA-3
C131 1.000 0.066 0.857 !       0.77 eA-3
Q132 0.991 0.019 0.858 !       0.76 eA-3
Q133 0.257 0.435 0.331 !       0.74 eA-3
Q134 0.968 0.014 0.423 !       0.74 eA-3
Q135 0.500 0.438 0.747 !       0.70 eA-3
Q136 0.475 0.369 0.248 !       0.70 eA-3
Q137 0.515 0.350 0.645 !       0.70 eA-3
C138 0.571 0.049 0.440 !       0.67 eA-3
Q139 0.978 0.501 0.951 !       0.67 eA-3
Q140 0.031 0.282 0.066 !       0.66 eA-3
C141 0.970 0.443 0.904 !       0.66 eA-3
Q142 0.493 0.271 0.345 !       0.65 eA-3
Q143 0.635 0.100 0.980 !       0.65 eA-3
C144 0.561 0.122 0.299 !       0.63 eA-3
Q145 0.563 0.382 0.692 !       0.63 eA-3
Q146 1.000 0.406 0.254 !       0.62 eA-3
Q147 0.929 0.346 0.283 !       0.62 eA-3
C148 0.110 0.501 0.685 !       0.61 eA-3
Q149 0.962 0.389 0.890 !       0.61 eA-3
Q150 0.466 0.251 0.093 !       0.60 eA-3
Q151 0.423 0.219 0.106 !       0.60 eA-3
Q152 0.033 0.343 0.159 !       0.60 eA-3
Q153 0.695 0.048 0.829 !       0.60 eA-3
Q154 0.650 0.261 0.716 !       0.60 eA-3
Q155 0.196 0.257 0.371 !       0.60 eA-3
Q156 0.782 0.302 0.518 !       0.59 eA-3
Q157 0.883 0.306 0.252 !       0.59 eA-3
Q158 0.579 0.141 0.660 !       0.59 eA-3
Q159 0.242 0.346 0.763 !       0.58 eA-3
Q160 0.538 0.172 0.603 !       0.58 eA-3
C161 0.564 0.367 0.219 !       0.57 eA-3
Q162 0.735 0.383 0.266 !       0.57 eA-3
Q163 0.438 0.058 0.174 !       0.57 eA-3
Q164 0.119 0.138 0.001 !       0.57 eA-3
C165 0.953 0.364 0.807 !       0.56 eA-3
C166 0.869 0.443 0.834 !       0.56 eA-3
Q167 0.877 0.447 0.910 !       0.55 eA-3
Q168 1.000 0.437 0.251 !       0.55 eA-3
Q169 0.446 0.237 0.307 !       0.55 eA-3
Q170 0.202 0.304 0.846 !       0.55 eA-3
Q171 0.057 0.420 0.092 !       0.55 eA-3
Q172 0.814 0.504 0.722 !       0.55 eA-3
Q173 0.470 0.183 0.296 !       0.54 eA-3
Q174 0.687 0.307 0.280 !       0.54 eA-3
Q175 0.775 0.321 0.499 !       0.54 eA-3
Q176 0.664 0.171 0.294 !       0.54 eA-3
Q177 0.917 0.249 0.440 !       0.54 eA-3
Q178 0.821 0.024 0.486 !       0.54 eA-3
Q179 0.517 0.368 0.700 !       0.54 eA-3
Q180 0.508 0.380 0.846 !       0.54 eA-3
Q181 0.312 0.134 0.159 !       0.53 eA-3
Q182 0.290 0.302 0.152 !       0.53 eA-3
Q183 0.970 0.020 0.295 !       0.53 eA-3
Q184 0.100 0.346 0.312 !       0.53 eA-3
Q185 0.586 0.096 0.075 !       0.53 eA-3
Q186 0.514 0.093 0.309 !       0.52 eA-3
Q187 0.031 0.191 0.084 !       0.52 eA-3
Q188 0.845 0.411 0.763 !       0.52 eA-3
Q189 0.767 0.027 0.121 !       0.51 eA-3
Q190 0.399 0.034 0.860 !       0.51 eA-3
Q191 0.101 0.311 0.955 !       0.51 eA-3
Q192 0.788 0.206 0.394 !       0.51 eA-3
Q193 0.959 0.134 0.843 !       0.51 eA-3
Q194 0.936 0.106 0.589 !       0.51 eA-3
Q195 0.773 0.097 0.452 !       0.51 eA-3
Q196 0.234 0.337 0.078 !       0.51 eA-3
C197 0.773 0.434 0.461 !       0.50 eA-3
Q198 0.696 0.446 0.393 !       0.50 eA-3
Q199 0.712 0.496 0.408 !       0.50 eA-3
;
_refine_diff_density_max         1.271
_refine_diff_density_min         -0.471
_refine_diff_density_rms         0.104
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.063
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     503
_refine_ls_number_reflns         4995
_refine_ls_number_restraints     55
_refine_ls_restrained_S_all      1.079
_refine_ls_R_factor_all          0.1231
_refine_ls_R_factor_gt           0.0676
_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^)+(0.1072P)^2^+61.1731P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1849
_refine_ls_wR_factor_ref         0.2127
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2890
_reflns_number_total             4995
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            ac0c00047_si_002.cif
_cod_data_source_block           c2c_sq
_cod_depositor_comments          'Adding full bibliography for 1557785.cif.'
_cod_original_cell_volume        11028.1(16)
_cod_database_code               1557785
_shelx_shelxl_version_number     2014/7
_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
 C21-C2
 1.45 with sigma of 0.02
 C8-C1
 1.5 with sigma of 0.01
 C6-C7
 1.5 with sigma of 0.01
3. Rigid bond restraints
 C20, C23, C17
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C8, C1
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Uiso/Uaniso restraints and constraints
O21 \\sim C8 \\sim C1 \\sim C10: within 1.7A with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O23) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C12) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C8) \\sim Ueq, Uanis(C10) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
5.a Ternary CH refined with riding coordinates:
 C3(H3), C6(H6), C8(H8), C13(H13), C19(H19), C20(H20), C21(H21)
5.b Me refined with riding coordinates:
 C1(H1A,H1B,H1C), C2(H2A,H2B,H2C), C4(H4A,H4B,H4C), C5(H5A,H5B,H5C), C7(H7A,
 H7B,H7C), C9(H9A,H9B,H9C), C10(H10A,H10B,H10C), C11(H11A,H11B,H11C), C14(H14A,
 H14B,H14C), C17(H17A,H17B,H17C), C18(H18A,H18B,H18C), C22(H22A,H22B,H22C),
 C23(H23A,H23B,H23C), C24(H24A,H24B,H24C)
5.c Aromatic/amide H refined with riding coordinates:
 C12(H12), C16(H16)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'