Efficient and robust photocatalysts based on {P<sub>2</sub>W<sub>18</sub>} modified by an Ag complex.
Fan, Xiao-Ying; Guo, Heng; Lv, Jing-Hua; Yu, Kai; Su, Zhan-Hua; Wang, Lu; Wang, Chun-Mei; Zhou, Bai-Bin; Dalton transactions (Cambridge, England : 2003) 47 (2018) 4273–4281; doi:10.1039/c8dt00229k

data_7045607
_publ_section_title
;
 Efficient and robust photocatalysts based on
 {P<sub>2</sub>W<sub>18</sub>} modified by an Ag complex.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4273
_journal_page_last               4281
_journal_paper_doi               10.1039/c8dt00229k
_journal_volume                  47
_journal_year                    2018
_chemical_formula_moiety
'O62 P2 W18, 0.5(C10 H14 Ag N4), 0.5(C10 H16 Ag N4), C10 H14 N4,'
_chemical_formula_sum            'C30 H43 Ag N12 O63 P2 W18 en lv so t'
_chemical_formula_weight         5058.69
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_symmetry_space_group_name_Hall  '-P 1'
_symmetry_space_group_name_H-M   'P -1'
_atom_sites_solution_hydrogens   mixed
_audit_creation_date             2018-01-29
_audit_creation_method
;
Olex2 1.2
(compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5292)
;
_audit_update_record
;
2018-02-05 deposited with the CCDC.
2018-02-12 downloaded from the CCDC.
;
_cell_angle_alpha                71.8570(10)
_cell_angle_beta                 86.2520(10)
_cell_angle_gamma                73.1560(10)
_cell_formula_units_Z            2
_cell_length_a                   13.6198(16)
_cell_length_b                   14.9084(17)
_cell_length_c                   22.869(3)
_cell_measurement_reflns_used    8750
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.32
_cell_measurement_theta_min      2.31
_cell_volume                     4221.8(9)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_reduction        'SAINT V8.18C (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL (Sheldrick, 2008)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.947
_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  0.0438
_diffrn_reflns_av_unetI/netI     0.0812
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.947
_diffrn_reflns_limit_h_max       18
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            31658
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.947
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.453
_diffrn_reflns_theta_min         2.240
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    24.778
_exptl_absorpt_correction_T_max  0.018
_exptl_absorpt_correction_T_min  0.011
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            Yellow
_exptl_crystal_density_diffrn    3.980
_exptl_crystal_description       block
_exptl_crystal_F_000             4440.0
_exptl_crystal_size_max          0.20
_exptl_crystal_size_mid          0.18
_exptl_crystal_size_min          0.16
_platon_squeeze_details
;
TITL GH744_0m  P -1         R = 0.06
CELL   13.6198   14.9084   22.8690     71.86     86.25     73.16
SPGR P-1
C101 0.935 0.449 0.179 !       6.33 eA-3
C102 0.932 0.564 0.106 !       5.83 eA-3
Q103 0.417 0.543 0.357 !       5.81 eA-3
Q104 0.530 0.810 0.304 !       5.77 eA-3
Q105 0.157 0.706 0.149 !       5.65 eA-3
C106 0.017 0.420 0.158 !       5.56 eA-3
Q107 0.409 0.577 0.406 !       5.50 eA-3
Q108 0.516 0.873 0.216 !       5.47 eA-3
Q109 0.433 0.483 0.439 !       5.47 eA-3
Q110 0.161 0.594 0.352 !       5.43 eA-3
Q111 0.014 0.703 0.204 !       5.42 eA-3
Q112 0.144 0.782 0.448 !       5.39 eA-3
Q113 0.150 0.768 0.376 !       5.39 eA-3
Q114 0.384 0.796 0.367 !       5.36 eA-3
Q115 0.569 0.565 0.291 !       5.34 eA-3
Q116 0.553 0.607 0.213 !       5.33 eA-3
Q117 0.101 0.018 0.088 !       5.31 eA-3
C118 0.027 0.452 0.116 !       5.29 eA-3
Q119 0.038 0.642 0.283 !       5.22 eA-3
Q120 0.126 0.845 0.357 !       5.18 eA-3
Q121 0.093 0.049 0.140 !       5.18 eA-3
Q122 1.003 0.748 0.241 !       5.17 eA-3
Q123 0.400 0.732 0.455 !       5.17 eA-3
Q124 0.188 0.435 0.242 !       5.14 eA-3
Q125 0.238 0.111 0.227 !       5.09 eA-3
Q126 0.456 0.362 0.325 !       5.08 eA-3
Q127 0.137 0.769 0.070 !       4.95 eA-3
Q128 0.177 0.470 0.297 !       4.92 eA-3
Q129 0.221 0.170 0.148 !       4.90 eA-3
Q130 0.203 0.394 0.318 !       4.89 eA-3
C131 0.982 0.483 0.141 !       4.88 eA-3
Q132 0.042 0.606 0.242 !       4.87 eA-3
Q133 0.978 0.953 0.220 !       4.87 eA-3
Q134 0.379 0.969 0.316 !       4.86 eA-3
Q135 0.203 0.379 0.250 !       4.84 eA-3
Q136 0.385 0.970 0.085 !       4.82 eA-3
Q137 0.185 0.501 0.385 !       4.82 eA-3
Q138 0.112 0.971 0.160 !       4.79 eA-3
Q139 0.180 0.532 0.430 !       4.77 eA-3
Q140 0.398 0.902 0.173 !       4.73 eA-3
Q141 0.433 0.689 0.070 !       4.71 eA-3
Q142 0.540 0.781 0.251 !       4.70 eA-3
Q143 0.374 0.985 0.149 !       4.68 eA-3
Q144 0.409 0.721 0.377 !       4.65 eA-3
Q145 0.456 0.439 0.409 !       4.65 eA-3
Q146 0.123 0.936 0.116 !       4.64 eA-3
Q147 0.117 0.875 0.408 !       4.59 eA-3
Q148 0.423 0.858 0.147 !       4.55 eA-3
Q149 0.438 0.439 0.282 !       4.52 eA-3
Q150 0.368 0.018 0.356 !       4.49 eA-3
Q151 0.435 0.654 0.157 !       4.47 eA-3
Q152 0.181 0.528 0.350 !       4.45 eA-3
Q153 0.325 0.457 0.187 !       4.43 eA-3
Q154 0.547 0.642 0.273 !       4.41 eA-3
Q155 0.979 0.937 0.303 !       4.40 eA-3
C156 0.052 0.471 0.090 !       4.39 eA-3
Q157 0.450 0.395 0.242 !       4.37 eA-3
Q158 0.359 0.857 0.389 !       4.37 eA-3
Q159 0.965 0.984 0.266 !       4.36 eA-3
Q160 0.530 0.674 0.231 !       4.33 eA-3
Q161 0.907 0.433 0.219 !       4.31 eA-3
Q162 0.154 0.627 0.397 !       4.30 eA-3
Q163 0.121 0.015 0.307 !       4.30 eA-3
Q164 0.413 0.722 0.141 !       4.27 eA-3
Q165 0.346 0.077 0.353 !       4.23 eA-3
Q166 0.573 0.547 0.224 !       4.23 eA-3
Q167 0.300 0.534 0.157 !       4.23 eA-3
Q168 0.513 0.891 0.282 !       4.22 eA-3
Q169 0.133 0.779 0.141 !       4.22 eA-3
Q170 0.446 0.470 0.363 !       4.20 eA-3
Q171 0.307 0.500 0.109 !       4.20 eA-3
Q172 0.408 0.545 0.445 !       4.20 eA-3
Q173 0.993 0.892 0.226 !       4.13 eA-3
Q174 0.467 0.328 0.258 !       4.13 eA-3
Q175 0.202 0.641 0.140 !       4.12 eA-3
Q176 0.088 0.126 0.343 !       4.12 eA-3
Q177 0.010 0.703 0.280 !       4.08 eA-3
Q178 0.408 0.889 0.109 !       4.07 eA-3
Q179 0.379 0.814 0.432 !       4.05 eA-3
Q180 0.155 0.701 0.076 !       4.04 eA-3
Q181 0.168 0.733 0.420 !       4.03 eA-3
Q182 0.068 0.581 0.268 !       4.02 eA-3
Q183 0.898 0.389 0.242 !       4.01 eA-3
Q184 0.479 0.297 0.304 !       3.99 eA-3
Q185 0.205 0.221 0.171 !       3.93 eA-3
Q186 0.996 0.894 0.299 !       3.91 eA-3
Q187 0.252 0.063 0.198 !       3.89 eA-3
Q188 0.015 0.844 0.274 !       3.86 eA-3
Q189 0.328 0.437 0.123 !       3.85 eA-3
Q190 0.467 0.594 0.136 !       3.83 eA-3
C191 0.979 0.575 0.079 !       3.83 eA-3
Q192 0.349 0.061 0.281 !       3.75 eA-3
Q193 0.100 0.092 0.283 !       3.73 eA-3
Q194 0.028 0.672 0.197 !       3.65 eA-3
Q195 0.421 0.688 0.423 !       3.63 eA-3
Q196 0.111 0.046 0.367 !       3.63 eA-3
C197 0.134 0.513 0.010 !       3.63 eA-3
C198 0.315 0.341-0.003 !       3.60 eA-3
Q199 0.303 0.517 0.187 !       3.58 eA-3
;
_refine_diff_density_max         5.227
_refine_diff_density_min         -5.549
_refine_diff_density_rms         0.655
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.023
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1138
_refine_ls_number_reflns         20174
_refine_ls_number_restraints     309
_refine_ls_restrained_S_all      1.017
_refine_ls_R_factor_all          0.0829
_refine_ls_R_factor_gt           0.0616
_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^)+(0.1091P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1639
_refine_ls_wR_factor_ref         0.1822
_reflns_Friedel_coverage         0.000
_reflns_number_gt                14934
_reflns_number_total             21294
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00229k2.cif
_cod_data_source_block           2_0m
_cod_depositor_comments
'Adding full bibliography for 7045606--7045607.cif.'
_cod_original_cell_volume        4221.8(8)
_cod_original_formula_sum        'C30 H43 Ag N12 O63 P2 W18 solvent'
_cod_database_code               7045607
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.018
_shelx_estimated_absorpt_t_min   0.011
_exptl_absorpt_special_details
; 
 "SADABS v.2.10 (Bruker, 2003) was used for absorption correction. R(int) was 0.0928 before and 0.0438 after correction. The Ratio of minimum to maximum transmission is 0.6111. The \l/2 correction factor is 0.0015." 
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All O(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C4-C5
 1.5 with sigma of 0.02
 N2-C11
 1.33 with sigma of 0.02
 N2-C13
 1.33 with sigma of 0.02
 C13-C12
 1.33 with sigma of 0.02
 C11-N1
 1.33 with sigma of 0.02
 C12-N1
 1.33 with sigma of 0.02
 O50-N8
 2.93 with sigma of 0.02
3. Restrained planarity
 N1, C12, C13, N2, C11
 with sigma of 0.1
4. Rigid bond restraints
 N9, C30, C28, C29, N10
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N1, C12, C13, N2, C11
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 N4, C20
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C15, C16
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C16, C17
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
 N11, C4
 with sigma for 1-2 distances of 0.02 and sigma for 1-3 distances of 0.02
5. Uiso/Uaniso restraints and constraints
N9 \\sim C30 \\sim C28 \\sim C29 \\sim N10: within 3.8A with sigma of 0.04 and
sigma for terminal atoms of 0.08
N1 \\sim C12 \\sim C13 \\sim N2 \\sim C11: within 3.8A with sigma of 0.04 and
sigma for terminal atoms of 0.08
O20: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
N11 \\sim C4: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.04
Uanis(O32) \\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(N10) \\sim Ueq, Uanis(O24)
\\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C10) \\sim Ueq,
Uanis(C13) \\sim Ueq, Uanis(O33) \\sim Ueq, Uanis(O39) \\sim Ueq, Uanis(C11)
\\sim Ueq, Uanis(C14) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(N2) \\sim Ueq: with
sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(O1) \\sim Ueq, Uanis(O14) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O20) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O4) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O27) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N8) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O6) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O7) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O16) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C26) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O21) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
6.a Riding coordinates:
 O63(H63A,H63B)
6.b Secondary CH2 refined with riding coordinates:
 C24(H24A,H24B), C25(H25A,H25B), C27(H27A,H27B), C17(H17A,H17B), C26(H26A,
 H26B), C15(H15A,H15B), C4(H4A,H4B), C14(H14A,H14B), C16(H16A,H16B), C10(H10A,
 H10B), C9(H9A,H9B)
6.c Me refined with riding coordinates:
 C5(H5A,H5B,H5C)
6.d Aromatic/amide H refined with riding coordinates:
 C20(H20), C8(H8), C7(H7), C19(H19), C18(H18), C6(H6), C30(H30), C23(H23),
 C28(H28), C3(H3), C29(H29), C2(H2), C1(H1), C12(H12), C13(H13), C11(H11)
;
_platon_squeeze_void_probe_radius 1.20
_olex2_submission_special_instructions 'No special instructions were received'