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_7059884
_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         'O40 P W12, C26 H20 Ag N8, 2(H2 O)'
_chemical_formula_sum            'C26 H24 Ag N8 O42 P W12'
_chemical_formula_weight         3465.57
_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_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
;
2020-08-06 deposited with the CCDC.	2020-08-07 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 112.338(16)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.367(4)
_cell_length_b                   13.097(5)
_cell_length_c                   20.578(6)
_cell_measurement_reflns_used    2607
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.513
_cell_measurement_theta_min      2.276
_cell_volume                     2833.6(17)
_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    'ShelXT (Sheldrick, 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  0.0615
_diffrn_reflns_av_unetI/netI     0.0609
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 1.000
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       20
_diffrn_reflns_limit_l_min       -24
_diffrn_reflns_number            16733
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 1.000
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.499
_diffrn_reflns_theta_min         1.887
_exptl_absorpt_coefficient_mu    24.718
_exptl_absorpt_correction_T_max  0.025
_exptl_absorpt_correction_T_min  0.013
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   SADABS
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    4.062
_exptl_crystal_description       block
_exptl_crystal_F_000             3044
_exptl_crystal_size_max          0.19
_exptl_crystal_size_mid          0.17
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.251
_refine_diff_density_min         -1.975
_refine_diff_density_rms         0.259
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.020
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     416
_refine_ls_number_reflns         5278
_refine_ls_number_restraints     156
_refine_ls_restrained_S_all      1.007
_refine_ls_R_factor_all          0.0723
_refine_ls_R_factor_gt           0.0430
_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^)+(0.0203P)^2^+33.4632P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0752
_refine_ls_wR_factor_ref         0.0844
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3752
_reflns_number_total             5278
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0nj00103a2.cif
_cod_data_source_block           compound-1
_cod_depositor_comments
'Adding full bibliography for 7059883--7059886.cif.'
_cod_database_code               7059884
_shelx_shelxl_version_number     2018/3
_exptl_absorpt_special_details
;
SADABS-2008/1 (Bruker,2008) was used for absorption correction.
wR2(int) was 0.1098 before and 0.0487 after correction.
The Ratio of minimum to maximum transmission is 0.4826.
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,H) groups
2. Uiso/Uaniso restraints and constraints
O1W \\sim O2W: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(O1W) \\sim Ueq, Uanis(O2W) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
3. Rigid body (RIGU) restrains
 N1, Ag1, C3, C1, C2, C4, N2, C9, C5, N3, N4, C10, C6, C8, C13, C11, C7, C12
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.001
4. Others
 Sof(O2W)=Sof(H2WA)=Sof(H2WB)=1-FVAR(1)
 Sof(O1W)=Sof(H1WA)=Sof(H1WB)=FVAR(1)
 Fixed Sof: O13(0.5) O18(0.5) O12(0.5) O19(0.5)
5.a Everything fixed:
 O1W, H1WA, H1WB, H2WA, H2WB
5.b Aromatic/amide H refined with riding coordinates:
 C10(H10), C11(H11), C12(H12), C13(H13), N2(H2), C1(H1), C5(H5), C6(H6),
 C8(H8), C7(H7)
5.c Fitted hexagon refined as free rotating group:
 N4(C9,C10,C11,C12,C13)
;
_shelx_res_checksum              13654
_olex2_submission_special_instructions 'No special instructions were received'