Two polyoxovanadates for visible light driven photocatalytic performance
Huang, Li; Yang, Yufan; Yu, Xiaoyang; Li, Xiaonan; Shen, Yuan; Song, Runhong; Zhang, Hong; CrystEngComm 26 (2024) 6226–6234; doi:10.1039/D4CE00494A

data_7249533
_publ_section_title
;
 Two polyoxovanadates for visible light driven photocatalytic performance
;
_journal_issue                   43
_journal_name_full               CrystEngComm
_journal_page_first              6226
_journal_page_last               6234
_journal_paper_doi               10.1039/D4CE00494A
_journal_volume                  26
_journal_year                    2024
_chemical_formula_moiety         'C48 H40 O56 P8 V16, 8(C2 H8 N)'
_chemical_formula_sum            'C64 H104 N8 O56 P8 V16'
_chemical_formula_weight         2944.35
_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'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2023-04-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2024-01-29 deposited with the CCDC.	2024-10-01 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.082(6)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.110(4)
_cell_length_b                   25.413(4)
_cell_length_c                   26.005(5)
_cell_measurement_reflns_used    9706
_cell_measurement_temperature    295(2)
_cell_measurement_theta_max      24.962
_cell_measurement_theta_min      2.483
_cell_volume                     13951(4)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 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    'SHELXT 2014/5 (Sheldrick, 2014)'
_diffrn_ambient_temperature      294.85
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_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  0.1223
_diffrn_reflns_av_unetI/netI     0.0658
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       30
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       30
_diffrn_reflns_limit_l_min       -30
_diffrn_reflns_number            205792
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.118
_diffrn_reflns_theta_max         25.118
_diffrn_reflns_theta_min         2.230
_exptl_absorpt_coefficient_mu    1.183
_exptl_absorpt_correction_type   none
_exptl_crystal_density_diffrn    1.402
_exptl_crystal_description       block
_exptl_crystal_F_000             5920
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.12
_exptl_crystal_size_min          0.1
_refine_diff_density_max         1.592
_refine_diff_density_min         -1.144
_refine_diff_density_rms         0.150
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1477
_refine_ls_number_reflns         24751
_refine_ls_number_restraints     2976
_refine_ls_restrained_S_all      1.059
_refine_ls_R_factor_all          0.1338
_refine_ls_R_factor_gt           0.0804
_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^)+(0.1052P)^2^+127.1692P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.2105
_refine_ls_wR_factor_ref         0.2472
_reflns_Friedel_coverage         0.000
_reflns_number_gt                15458
_reflns_number_total             24751
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00494a2.cif
_cod_data_source_block           1_sq
_cod_database_code               7249533
_shelx_shelxl_version_number     2016/6
_shelx_estimated_absorpt_t_max   0.891
_shelx_estimated_absorpt_t_min   0.815
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C62-N7
 1.5 with sigma of 0.02
 C61-N7
 1.5 with sigma of 0.02
 C62-C61
 2.5 with sigma of 0.02
 C63-N9
 1.5 with sigma of 0.02
 N9-C65
 1.5 with sigma of 0.02
 C65-C63
 2.5 with sigma of 0.02
 C66-N11
 1.5 with sigma of 0.02
 N11-C68
 1.5 with sigma of 0.02
 C68-C66
 2.5 with sigma of 0.02
 C67-N10
 1.5 with sigma of 0.02
 N10-C69
 1.5 with sigma of 0.02
 C69-C67
 2.5 with sigma of 0.02
 N8-C70
 1.5 with sigma of 0.02
 N8-C64
 1.5 with sigma of 0.02
 C70-C64
 2.5 with sigma of 0.02
 C71-N12
 1.5 with sigma of 0.02
 N12-C72
 1.5 with sigma of 0.02
 C72-C71
 2.5 with sigma of 0.02
 H69A-H10B
 2.3 with sigma of 0.02
 H68A-H11A
 2.3 with sigma of 0.02
 H67A-H10B
 2.3 with sigma of 0.02
 H3A-H35A
 2.3 with sigma of 0.02
 H4A-H56C
 2.3 with sigma of 0.02
 H4A-H39C
 2.3 with sigma of 0.02
 H3B-H35B
 2.3 with sigma of 0.02
 H8A-H70C
 2.3 with sigma of 0.02
 H8A-H64C
 2.3 with sigma of 0.02
 H3B-H35A
 2.3 with sigma of 0.02
 H3B-H49C
 2.3 with sigma of 0.02
 H8B-H70A
 2.3 with sigma of 0.02
 H4B-H39C
 2.3 with sigma of 0.02
 H4A-H39B
 2.3 with sigma of 0.02
 H72C-H12B
 2.3 with sigma of 0.02
 H12B-H71C
 2.3 with sigma of 0.02
 H12A-H71B
 2.3 with sigma of 0.02
 H12A-H72A
 2.3 with sigma of 0.02
 H11B-H66B
 2.3 with sigma of 0.02
 H11A-H66C
 2.3 with sigma of 0.02
 H4B-H56C
 2.3 with sigma of 0.02
 H4A-H56A
 2.3 with sigma of 0.02
 H3A-H49C
 2.3 with sigma of 0.02
 H3B-H49B
 2.3 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\sim C19 \\sim C20 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim C30 \\sim C31 \\sim C32 \\sim C33
\\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim C39 \\sim C40 \\sim C41
\\sim C42 \\sim C43 \\sim C44 \\sim C45 \\sim C46 \\sim C47 \\sim C48 \\sim C49
\\sim C50 \\sim C51 \\sim C52 \\sim C53 \\sim C54 \\sim C55 \\sim C56 \\sim C57
\\sim C58 \\sim C59 \\sim C60 \\sim C61 \\sim C62 \\sim C63 \\sim C64 \\sim C65
\\sim C66 \\sim C67 \\sim C68 \\sim C69 \\sim C70 \\sim C71 \\sim C72 \\sim N1
\\sim N2 \\sim N3 \\sim N4 \\sim N5 \\sim N6 \\sim N7 \\sim N8 \\sim N9 \\sim
N10 \\sim N11 \\sim N12 \\sim O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6
\\sim O7 \\sim O8 \\sim O9 \\sim O10 \\sim O11 \\sim O12 \\sim O13 \\sim O14
\\sim O15 \\sim O16 \\sim O17 \\sim O18 \\sim O19 \\sim O20 \\sim O21 \\sim O22
\\sim O23 \\sim O24 \\sim O25 \\sim O26 \\sim O27 \\sim O28 \\sim O29 \\sim O30
\\sim O31 \\sim O32 \\sim O33 \\sim O34 \\sim O35 \\sim O36 \\sim O37 \\sim O38
\\sim O39 \\sim O40 \\sim O41 \\sim O42 \\sim O43 \\sim O44 \\sim O45 \\sim O46
\\sim O47 \\sim O48 \\sim O49 \\sim O50 \\sim O51 \\sim O52 \\sim O53 \\sim O54
\\sim O55 \\sim O56: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.03
Uanis(C70) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N7) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(N11) \\sim Ueq, Uanis(C66) \\sim Ueq, Uanis(C68) \\sim Ueq, : with sigma
of 0.01 and sigma for terminal atoms of 0.02
Uanis(C69) \\sim Ueq, Uanis(C67) \\sim Ueq, Uanis(N10) \\sim Ueq, : with sigma
of 0.01 and sigma for terminal atoms of 0.02
4. Others
 Fixed Sof: C57(0.5) H57A(0.5) H57B(0.5) H57C(0.5) N5(0.5) H5A(0.5) H5B(0.5)
 C58(0.5) H58A(0.5) H58B(0.5) H58C(0.5) C59(0.5) H59A(0.5) H59B(0.5) H59C(0.5)
 N6(0.5) H6A(0.5) H6B(0.5) C60(0.5) H60A(0.5) H60B(0.5) H60C(0.5) N8(0.5)
 H8A(0.5) H8B(0.5) C63(0.33333) H63A(0.33333) H63B(0.33333) H63C(0.33333)
 C64(0.5) H64A(0.5) H64B(0.5) H64C(0.5) N9(0.33333) H9A(0.33333) H9B(0.33333)
 C65(0.33333) H65A(0.33333) H65B(0.33333) H65C(0.33333) C66(0.33333)
 H66A(0.33333) H66B(0.33333) H66C(0.33333) C67(0.33333) H67A(0.33333)
 H67B(0.33333) H67C(0.33333) N10(0.33333) H10A(0.33333) H10B(0.33333)
 C68(0.33333) H68A(0.33333) H68B(0.33333) H68C(0.33333) N11(0.33333)
 H11A(0.33333) H11B(0.33333) C69(0.33333) H69A(0.33333) H69B(0.33333)
 H69C(0.33333) C70(0.5) H70A(0.5) H70B(0.5) H70C(0.5) N12(0.5) H12A(0.5)
 H12B(0.5) C71(0.5) H71A(0.5) H71B(0.5) H71C(0.5) C72(0.5) H72A(0.5) H72B(0.5)
 H72C(0.5)
5.a Secondary CH2 refined with riding coordinates:
 N1(H1A,H1B), N2(H2A,H2B), N3(H3A,H3B), N4(H4A,H4B), N5(H5A,H5B), N6(H6A,H6B),
 N7(H7A,H7B), N8(H8A,H8B), N9(H9A,H9B), N10(H10A,H10B), N11(H11A,H11B),
 N12(H12A,H12B)
5.b Aromatic/amide H refined with riding coordinates:
 C7(H7), C8(H8), C9(H9), C10(H10), C11(H11), C12(H12), C13(H13), C14(H14),
 C15(H15), C16(H16), C17(H17), C18(H18), C19(H19), C21(H21), C22(H22), C23(H23),
  C24(H24), C26(H26), C27(H27), C28(H28), C29(H29), C30(H30), C31(H31),
 C32(H32), C33(H33), C34(H34), C38(H38), C40(H40), C41(H41), C42(H42), C43(H43),
  C44(H44), C45(H45), C46(H46), C47(H47), C50(H50), C51(H51), C52(H52),
 C53(H53), C54(H54)
5.c Fitted hexagon refined as free rotating group:
 C43(C44,C45,C46,C47,C48), C50(C51,C52,C53,C54,C55)
5.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C25(H25A,H25B,H25C), C35(H35A,H35B,H35C), C36(H36A,H36B,
 H36C), C37(H37A,H37B,H37C), C39(H39A,H39B,H39C), C49(H49A,H49B,H49C), C56(H56A,
 H56B,H56C), C57(H57A,H57B,H57C), C58(H58A,H58B,H58C), C59(H59A,H59B,H59C),
 C60(H60A,H60B,H60C), C61(H61A,H61B,H61C), C62(H62A,H62B,H62C), C63(H63A,H63B,
 H63C), C64(H64A,H64B,H64C), C65(H65A,H65B,H65C), C66(H66A,H66B,H66C), C67(H67A,
 H67B,H67C), C68(H68A,H68B,H68C), C69(H69A,H69B,H69C), C70(H70A,H70B,H70C),
 C71(H71A,H71B,H71C), C72(H72A,H72B,H72C)
;
_shelx_res_checksum              71291
_shelx_hkl_checksum              95024
_shelx_fab_checksum              1876
_olex2_submission_special_instructions 'No special instructions were received'