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_7059886
_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
'C51.33 H35.6 Ag4 Mo24 N16 O80.8 Si2, 1.2(H2 O), 0.67(C)'
_chemical_formula_sum            'C52 H38 Ag4 Mo24 N16 O82 Si2'
_chemical_formula_weight         4989.20
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2020-01-30
_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                 98.963(5)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   21.340(5)
_cell_length_b                   15.114(5)
_cell_length_c                   16.206(5)
_cell_measurement_reflns_used    5200
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.308
_cell_measurement_theta_min      2.531
_cell_volume                     5163(3)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_collection       'SMART (Bruker, 2001)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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      293(2)
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'Bruker P4'
_diffrn_measurement_method       '\w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71069
_diffrn_reflns_av_R_equivalents  0.0485
_diffrn_reflns_av_unetI/netI     0.0542
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       27
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -20
_diffrn_reflns_number            35723
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.240
_diffrn_reflns_theta_max         27.455
_diffrn_reflns_theta_min         1.658
_exptl_absorpt_coefficient_mu    3.690
_exptl_absorpt_correction_T_max  0.554
_exptl_absorpt_correction_T_min  0.501
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.209
_exptl_crystal_description       block
_exptl_crystal_F_000             4684
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.16
_refine_diff_density_max         2.299
_refine_diff_density_min         -1.914
_refine_diff_density_rms         0.183
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.021
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     972
_refine_ls_number_reflns         11770
_refine_ls_number_restraints     417
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0817
_refine_ls_R_factor_gt           0.0482
_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^)+(0.0518P)^2^+27.6812P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1113
_refine_ls_wR_factor_ref         0.1265
_reflns_Friedel_coverage         0.000
_reflns_number_gt                8072
_reflns_number_total             11770
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj00103a2.cif
_cod_data_source_block           compound-2
_cod_depositor_comments
'Adding full bibliography for 7059883--7059886.cif.'
_cod_database_code               7059886
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1081 before and 0.0467 after correction.
The Ratio of minimum to maximum transmission is 0.4654.
The \l/2 correction factor is 0.0015.
;
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Restrained distances
 C16-C17 \\sim C16A-C17A
 with sigma of 0.02
 C16-C15 \\sim C16A-C15A
 with sigma of 0.02
 C14-N5 \\sim C14A-N5A
 with sigma of 0.02
 C15-N5 \\sim C15A-N5A
 with sigma of 0.02
 C21-N7 \\sim C21A-N7A
 with sigma of 0.04
 C17-C18 \\sim C17A-C18A
 with sigma of 0.04
 C15-C17 \\sim C15A-C17A
 with sigma of 0.04
 C21-C17 \\sim C21A-C17A
 with sigma of 0.02
 C17-N7 \\sim C17A-N7A
 with sigma of 0.02
 N7-C18 \\sim N7A-C18A
 with sigma of 0.02
 C18-C19 \\sim C18A-C19A
 with sigma of 0.02
 C21-C19 \\sim C21A-C19A
 with sigma of 0.04
 N7-C19 \\sim N7A-C19A
 with sigma of 0.04
 C16-C14 \\sim C16A-C14A
 with sigma of 0.04
 C16-N5 \\sim C16A-N5A
 with sigma of 0.04
 C16-C21 \\sim C16A-C21A
 with sigma of 0.04
 C16-N7 \\sim C16A-N7A
 with sigma of 0.04
 C14-C15 \\sim C14A-C15A
 with sigma of 0.04
 C26-C23 \\sim C26A-C23A
 with sigma of 0.04
 N5-N8 \\sim N5A-N8A
 with sigma of 0.04
 C15-C26 \\sim C15A-C26A
 with sigma of 0.02
 C23-C21 \\sim C23A-C21A
 with sigma of 0.04
 C25-N8 \\sim C25A-N8A
 with sigma of 0.02
 C25-C24 \\sim C25A-C24A
 with sigma of 0.02
 N8-C26 \\sim N8A-C26A
 with sigma of 0.02
 C25-C23 \\sim C25A-C23A
 with sigma of 0.04
 N8-C22 \\sim N8A-C22A
 with sigma of 0.04
 C26-C22 \\sim C26A-C22A
 with sigma of 0.02
 C22-C23 \\sim C22A-C23A
 with sigma of 0.02
 C22-C21 \\sim C22A-C21A
 with sigma of 0.02
 C23-C24 \\sim C23A-C24A
 with sigma of 0.02
 C22-C24 \\sim C22A-C24A
 with sigma of 0.04
 C15-C22 \\sim C15A-C22A
 with sigma of 0.04
 N5-C26 \\sim N5A-C26A
 with sigma of 0.04
 C25-C26 \\sim C25A-C26A
 with sigma of 0.04
 N8-C24 \\sim N8A-C24A
 with sigma of 0.04
 C26-C21 \\sim C26A-C21A
 with sigma of 0.04
 C22-C17 \\sim C22A-C17A
 with sigma of 0.04
 C16-C26 \\sim C16A-C26A
 with sigma of 0.04
 C15-N8 \\sim C15A-N8A
 with sigma of 0.04
 N6-C16 \\sim N6A-C16A
 with sigma of 0.02
 N6-C14 \\sim N6A-C14A
 with sigma of 0.02
 N6-C15 \\sim N6A-C15A
 with sigma of 0.04
 N6-N5 \\sim N6A-N5A
 with sigma of 0.04
 N6-C17 \\sim N6A-C17A
 with sigma of 0.04
 Ag2-N5 \\sim Ag2A-N5A
 with sigma of 0.02
 Ag2-C14 \\sim Ag2A-C14A
 with sigma of 0.04
 Ag2-C15 \\sim Ag2A-C15A
 with sigma of 0.04
 Ag2-N8 \\sim Ag2A-N8A
 with sigma of 0.02
 Ag2-C25 \\sim Ag2A-C25A
 with sigma of 0.04
 Ag2-C26 \\sim Ag2A-C26A
 with sigma of 0.04
 C21-C20 \\sim C21A-C20A
 with sigma of 0.02
 C19-C20 \\sim C19A-C20A
 with sigma of 0.02
 C17-C20 \\sim C17A-C20A
 with sigma of 0.04
 C18-C20 \\sim C18A-C20A
 with sigma of 0.04
 C22-C20 \\sim C22A-C20A
 with sigma of 0.04
3. Rigid bond restraints
 O0AA, Ag2A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
4. Uiso/Uaniso restraints and constraints
N7A \\sim CAA: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
O0AA \\sim O1W: within 2A with sigma of 0.001 and sigma for terminal atoms of
0.002
Uanis(C18A) \\sim Ueq, Uanis(C24A) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(C17) \\sim Ueq, Uanis(C21) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
Uanis(N7A) \\sim Ueq, Uanis(CAA) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(C17A) \\sim Ueq, Uanis(C20A) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
Uanis(O1W) \\sim Ueq, Uanis(O0AA) \\sim Ueq: with sigma of 0.001 and sigma for
terminal atoms of 0.002
5. Rigid body (RIGU) restrains
 N7, N6, C16, C14, C15, C17, N5, C26, C21, N8, C22, C20, C18, C25, C23, C19, C24
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 C21A, C26A, N8A, C15A, C22A, C25A, N5A, C16A, C23A, C24A, C14A, N6A, C17A,
 C20A, N7A, C19A, C18A
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
 O0AA, O1W
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.002
6. Others
 Fixed Sof: Ag2(0.6) N6(0.6) H6(0.6) C16(0.6) C14(0.6) H14(0.6) C15(0.6)
 N5(0.6) C25(0.6) H25(0.6) N8(0.6) C26(0.6) C22(0.6) C23(0.6) H23(0.6) C24(0.6)
 H24(0.6) C21(0.6) C17(0.6) N7(0.6) C18(0.6) H18(0.6) C19(0.6) H19(0.6)
 C20(0.33333) H20(0.5) O1W(0.6) H1WA(0.6) H1WB(0.6) C26A(0.4) Ag2A(0.4)
 N5A(0.4) N8A(0.4) C14A(0.4) H14A(0.4) C15A(0.4) C25A(0.4) H25A(0.4) N6A(0.4)
 H6AA(0.4) C16A(0.4) C24A(0.4) H24A(0.4) C22A(0.4) C17A(0.4) C23A(0.4)
 H23A(0.4) C21A(0.4) N7A(0.4) C20A(0.3333) H20A(0.5) C18A(0.4) H18A(0.4)
 C19A(0.4) H19A(0.4) CAA(0.33333) O0AA(0.4) H0AA(0.4) H0AB(0.4)
7.a Everything fixed:
 O1W, H1WA, H1WB
7.b Rotating group:
 O0AA(H0AA,H0AB)
7.c Aromatic/amide H refined with riding coordinates:
 N2(H2), N6(H6), C14(H14), C5(H5), C10(H10), C11(H11), C12(H12), C7(H7),
 C1(H1), C6(H6A), C25(H25), C23(H23), C24(H24), C18(H18), C19(H19), C20(H20),
 C14A(H14A), C25A(H25A), N6A(H6AA), C24A(H24A), C23A(H23A), C20A(H20A),
 C18A(H18A), C19A(H19A)
7.d Fitted hexagon refined as free rotating group:
 C25(N8,C26,C22,C23,C24)
7.e Idealised tetrahedral OH refined as rotating group:
 O40(H40)
;
_shelx_res_checksum              64489
_olex2_submission_special_instructions 'No special instructions were received'