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_7059883
_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(C18 H16 Ag Mo12 N5 O41 Si), 8(H2 O)'
_chemical_formula_sum            'C36 H48 Ag2 Mo24 N10 O90 Si2'
_chemical_formula_weight         4635.32
_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
_audit_block_doi                 10.5517/ccdc.csd.cc23pxxn
_audit_creation_date             2020-02-02
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-15 deposited with the CCDC.	2020-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 101.353(2)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   15.3224(12)
_cell_length_b                   18.0088(15)
_cell_length_c                   18.5733(15)
_cell_measurement_reflns_used    3119
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      50.736
_cell_measurement_theta_min      2.71
_cell_volume                     5024.8(7)
_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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      293(2)
_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_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0750
_diffrn_reflns_av_unetI/netI     0.0779
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            28516
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.590
_exptl_absorpt_coefficient_mu    3.411
_exptl_absorpt_correction_T_max  0.600
_exptl_absorpt_correction_T_min  0.528
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.064
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             4368
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         1.688
_refine_diff_density_min         -0.949
_refine_diff_density_rms         0.201
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.000
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     748
_refine_ls_number_reflns         8845
_refine_ls_number_restraints     22
_refine_ls_restrained_S_all      1.013
_refine_ls_R_factor_all          0.0786
_refine_ls_R_factor_gt           0.0421
_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^)+(0.0367P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0810
_refine_ls_wR_factor_ref         0.0948
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6047
_reflns_number_total             8845
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj00103a2.cif
_cod_data_source_block           compound-3
_cod_depositor_comments
'Adding full bibliography for 7059883--7059886.cif.'
_cod_database_code               7059883
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1090 before and 0.0367 after correction.
The Ratio of minimum to maximum transmission is 0.5626.
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
 At 1.5 times of:
  All O(H) groups, All O(H,H) groups
2. Shared sites
{C10, C10A}
{C11, C11A}
{C16, C16A}
{C15, C15A}
3. Restrained distances
 H41A-N4
 1 with sigma of 0.1
 H42A-N4
 1 with sigma of 0.1
4. Rigid bond restraints
 C12, N5
 with sigma for 1-2 distances of 0.005 and sigma for 1-3 distances of 0.005
 N4, C18
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Uiso/Uaniso restraints and constraints
Uanis(C1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N1) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N4) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.001
Uanis(C10) = Uanis(C10A)
Uanis(C11) = Uanis(C11A)
Uanis(C16) = Uanis(C16A)
Uanis(C15) = Uanis(C15A)
6. Others
 Sof(H12A)=Sof(H13A)=Sof(H18A)=Sof(H17A)=Sof(O42)=Sof(H42A)=Sof(H42B)=
 Sof(C10A)=Sof(H10A)=Sof(C11A)=Sof(H11A)=Sof(C16A)=Sof(H16A)=Sof(C15A)=
 Sof(H15A)=1-FVAR(1)
 Sof(C15)=Sof(H15)=Sof(C10)=Sof(H10)=Sof(C11)=Sof(H11)=Sof(H12)=Sof(H13)=
 Sof(C16)=Sof(H16)=Sof(H18)=Sof(H17)=Sof(O41)=Sof(H41A)=Sof(H41B)=FVAR(1)
7.a Everything fixed:
 O3W, H3WA, H3WB, H25
7.b Riding coordinates:
 O41(H41A,H41B), O42(H42A,H42B)
7.c Free rotating group:
 O2W(H2WA,H2WB), O4W(H4WA,H4WB)
7.d Rotating group:
 O1W(H1WA,H1WB)
7.e Aromatic/amide H refined with riding coordinates:
 C15(H15), C10(H10), C2(H2), C1(H1), C3(H3), C5(H5), C11(H11), C12(H12),
 C12(H12A), C13(H13), C13(H13A), C16(H16), C18(H18), C18(H18A), C17(H17),
 C17(H17A), C10A(H10A), C11A(H11A), C16A(H16A), C15A(H15A)
7.f Idealised tetrahedral OH refined as rotating group:
 O35(H35)
;
_shelx_res_checksum              27151
_olex2_submission_special_instructions 'No special instructions were received'