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_7045606
_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
'2(C15 H21 Ag1.50 N6 O62 P2 W18), 2(C10 H12 N4), 2(C10 H14 N4)'
_chemical_formula_sum            'C70 H94 Ag3 N28 O124 P4 W36'
_chemical_formula_weight         10377.44
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_space_group_name_Hall  '-P 2yn'
_symmetry_space_group_name_H-M   'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2018-01-30
_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                90
_cell_angle_beta                 93.1300(10)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.7549(6)
_cell_length_b                   25.9946(11)
_cell_length_c                   21.5866(9)
_cell_measurement_reflns_used    9940
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.32
_cell_volume                     8267.1(6)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_collection       'Bruker SMART'
_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)'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.991
_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  0.0638
_diffrn_reflns_av_unetI/netI     0.0674
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.991
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       34
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            67279
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.991
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.302
_diffrn_reflns_theta_min         2.324
_diffrn_source                   'fine-focus sealed tube'
_exptl_absorpt_coefficient_mu    25.425
_exptl_absorpt_correction_T_max  0.010
_exptl_absorpt_correction_T_min  0.006
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    4.169
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             9134.0
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.16
_exptl_crystal_size_min          0.12
_refine_diff_density_max         3.131
_refine_diff_density_min         -3.362
_refine_diff_density_rms         0.441
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.005
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1198
_refine_ls_number_reflns         20357
_refine_ls_number_restraints     756
_refine_ls_restrained_S_all      7.581
_refine_ls_R_factor_all          0.0639
_refine_ls_R_factor_gt           0.0423
_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^)+(0.0430P)^2^+107.2370P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0927
_refine_ls_wR_factor_ref         0.1035
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15611
_reflns_number_total             20547
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            c8dt00229k2.cif
_cod_data_source_block           1_0m
_cod_depositor_comments
'Adding full bibliography for 7045606--7045607.cif.'
_cod_database_code               7045606
_shelx_shelxl_version_number     2014/7
_exptl_absorpt_special_details
; 
 "SADABS v.2.10 (Bruker, 2003) was used for absorption correction. R(int) was 0.1009 before and 0.0638 after correction. The Ratio of minimum to maximum transmission is 0.6000. 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
2. Restrained distances
 O39-N11
 3.2 with sigma of 0.01
3. Rigid bond restraints
 C44, N14, C39
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
 N1, C30, C34
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C28, C36, N12
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N9, C30
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 N5, C34
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C25, C37
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 O61, W11
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 Ag2, N4, N5
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
 C41, C43, C44, C45, C46, C47, C49, C50, C51, C52, C53, C8, C13, C14, C16, C17,
  C18, C20, C21, C22, C23, C25, C26, C27, C28, C10, C30, C31, C32, C33, C34,
 C35, C36, C37, C39
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
C43 \\sim C44: within 3.8A with sigma of 0.001 and sigma for terminal atoms of
0.002
C28 \\sim C36 \\sim N12: within 2A with sigma of 0.001 and sigma for terminal
atoms of 0.002
N10 \\sim N14 \\sim N4 \\sim N1 \\sim N8 \\sim N5 \\sim N11 \\sim N6 \\sim N9
\\sim N7 \\sim N2 \\sim N3 \\sim N13 \\sim N12: within 3.8A with sigma of 0.001
and sigma for terminal atoms of 0.02
N9 \\sim C30: within 3.8A with sigma of 0.001 and sigma for terminal atoms of
0.002
N5 \\sim C34: within 3.8A with sigma of 0.001 and sigma for terminal atoms of
0.002
C25 \\sim C37: within 3.8A with sigma of 0.001 and sigma for terminal atoms of
0.002
O61 \\sim W11: within 3.8A with sigma of 0.001 and sigma for terminal atoms of
0.002
Ag2 \\sim N4 \\sim N5: within 3.8A with sigma of 0.001 and sigma for terminal
atoms of 0.002
C41 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C49 \\sim C50 \\sim
C51 \\sim C52 \\sim C53 \\sim C8 \\sim C13 \\sim C14 \\sim C16 \\sim C17 \\sim
C18 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C25 \\sim C26 \\sim C27 \\sim
C28 \\sim C10 \\sim C30 \\sim C31 \\sim C32 \\sim C33 \\sim C34 \\sim C35 \\sim
C36 \\sim C37 \\sim C39: within 3.8A with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(O55) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O18) \\sim Ueq, Uanis(O34) \\sim Ueq, Uanis(O55) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C44) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C43) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(C44) \\sim Ueq, Uanis(C43) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C41) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(N12) \\sim Ueq, Uanis(C28) \\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(N14) \\sim Ueq, Uanis(C44) \\sim Ueq, Uanis(C39) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O7) \\sim Ueq, Uanis(O61) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O9) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O32) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(N9) \\sim Ueq, Uanis(C30) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(N5) \\sim Ueq, Uanis(C34) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C25) \\sim Ueq, Uanis(C37) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(Ag2) \\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(N5) \\sim Ueq: with sigma of
0.001 and sigma for terminal atoms of 0.002
Uanis(O61) \\sim Ueq, Uanis(W11) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(P1) \\sim Ueq, Uanis(O4) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O22) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
5. Others
 Fixed Sof: Ag1(0.5)
6.a Ternary CH refined with riding coordinates:
 C30(H30), C34(H34)
6.b Secondary CH2 refined with riding coordinates:
 C49(H49A,H49B), C50(H50A,H50B), C51(H51A,H51B), C52(H52A,H52B), C53(H53A,
 H53B), C17(H17A,H17B), C21(H21A,H21B), C23(H23A,H23B), C25(H25A,H25B),
 C26(H26A,H26B), C32(H32A,H32B), C33(H33A,H33B), C35(H35A,H35B), C37(H37A,H37B)
6.c Aromatic/amide H refined with riding coordinates:
 C41(H41), C43(H43), C45(H45), C46(H46), C47(H47), C8(H8), C13(H13), C14(H14),
 C16(H16), C18(H18), C20(H20), C22(H22), C27(H27), C28(H28), C10(H10), C31(H31),
  C36(H36)
;
_olex2_submission_special_instructions 'No special instructions were received'