Four Keggin-based compounds constructed by a series of pyridine derivatives: synthesis, and electrochemical, photocatalytic and fluorescence sensing properties
Mou, Hai-chen; Ying, Jun; Tian, Ai-xiang; Cui, Hong-tao; Wang, Xiu-li; New Journal of Chemistry 44 (2020) 15122–15130; doi:10.1039/D0NJ00103A

data_7059885
_publ_section_title
;
 Four Keggin-based compounds constructed by a series of pyridine
 derivatives: synthesis, and electrochemical, photocatalytic and
 fluorescence sensing properties
;
_journal_issue                   35
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              15122
_journal_page_last               15130
_journal_paper_doi               10.1039/D0NJ00103A
_journal_volume                  44
_journal_year                    2020
_chemical_formula_moiety
'2.5(C28 H16 Ag2 N8 S4), 2(Mo12 O40 P), Ag, 2(C14 H8 N4 S2), 6(H2 O)'
_chemical_formula_sum            'C98 H68 Ag6 Mo24 N28 O86 P2 S14'
_chemical_formula_weight         6474.36
_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   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2019-10-04
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-08-06 deposited with the CCDC.	2020-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 91.734(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   22.563(6)
_cell_length_b                   25.768(6)
_cell_length_c                   27.347(6)
_cell_measurement_reflns_used    3770
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      50.284
_cell_measurement_theta_min      2.4
_cell_volume                     15892(7)
_computing_cell_refinement       'SAINT V8.18C (?, 2016)'
_computing_data_collection       'SMART (Bruker, 2001)'
_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  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'XT (Sheldrick, 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.975
_diffrn_measured_fraction_theta_max 0.975
_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  0.1007
_diffrn_reflns_av_unetI/netI     0.0991
_diffrn_reflns_Laue_measured_fraction_full 0.975
_diffrn_reflns_Laue_measured_fraction_max 0.975
_diffrn_reflns_limit_h_max       26
_diffrn_reflns_limit_h_min       -23
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       32
_diffrn_reflns_limit_l_min       -27
_diffrn_reflns_number            42789
_diffrn_reflns_point_group_measured_fraction_full 0.975
_diffrn_reflns_point_group_measured_fraction_max 0.975
_diffrn_reflns_theta_full        25.142
_diffrn_reflns_theta_max         25.142
_diffrn_reflns_theta_min         1.200
_exptl_absorpt_coefficient_mu    2.853
_exptl_absorpt_correction_T_max  0.652
_exptl_absorpt_correction_T_min  0.587
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_density_diffrn    2.706
_exptl_crystal_description       block
_exptl_crystal_F_000             12336
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.291
_refine_diff_density_min         -2.180
_refine_diff_density_rms         0.330
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1138
_refine_ls_number_reflns         13864
_refine_ls_number_restraints     209
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1327
_refine_ls_R_factor_gt           0.0770
_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^)+(0.1118P)^2^+233.3726P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1908
_refine_ls_wR_factor_ref         0.2246
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8462
_reflns_number_total             13864
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj00103a2.cif
_cod_data_source_block           compound-4
_cod_depositor_comments
'Adding full bibliography for 7059883--7059886.cif.'
_cod_original_cell_volume        15893(6)
_cod_database_code               7059885
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1082 before and 0.0461 after correction.
The Ratio of minimum to maximum transmission is 0.4426.
The \l/2 correction factor is 0.0015.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All O(H,H) groups
2. Restrained distances
 C45-N14
 2.5 with sigma of 0.02
 C45-C44
 1.45 with sigma of 0.02
 C49-C48
 1.3 with sigma of 0.02
 C47-C46
 1.3 with sigma of 0.02
 N14-C49
 1.34 with sigma of 0.02
3. Rigid bond restraints
 O14, N14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
 O40, N14
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
4. Uiso/Uaniso restraints and constraints
O14 \\sim O40: within 3.8A with sigma of 0.02 and sigma for terminal atoms of
0.02
N14: within 2A with sigma of 0.02 and sigma for terminal atoms of 0.03
Uanis(O17) \\sim Ueq, Uanis(O12) \\sim Ueq, Uanis(C44) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(O17) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C33) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O40) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
Uanis(O14) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O11) \\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(N13) \\sim Ueq, Uanis(C44)
\\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.001 and sigma for terminal
atoms of 0.002
Uanis(N14) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.001
Uanis(O24) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(O40) \\sim Ueq, Uanis(N6)
\\sim Ueq, Uanis(N8) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C9) \\sim Ueq,
Uanis(C20) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C13) \\sim Ueq, Uanis(C18)
\\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(N11) \\sim Ueq, Uanis(C45) \\sim Ueq,
Uanis(C41) \\sim Ueq, Uanis(N12) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N7) \\sim Ueq, Uanis(C49) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O17) \\sim Ueq, Uanis(C48) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(O1W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
5.a Everything fixed:
 O1W, H1WA, H1WB, O3W, H3WA, H3WB, O2W, H2WA, H2WB
5.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C28(H28), C25(H25), C27(H27), C46(H46), C37(H37), C38(H38), C26(H26),
 C32(H32), C3(H3), C4(H4), C2(H2), C14(H14), C48(H48), C13(H13), C11(H11),
 C12(H12), C16(H16), C31(H31), C40(H40), C15(H15), C18(H18), C29(H29), C49(H49),
  C47(H47), C17(H17), C30(H30), C36(H36)
;
_shelx_res_checksum              8147
_olex2_submission_special_instructions 'No special instructions were received'