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_7249532
_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 O48 P8 V12, 2(C3 H7 N O), 4(C4 H12 N)'
_chemical_formula_sum            'C70 H102 N6 O50 P8 V12'
_chemical_formula_weight         2686.61
_space_group_crystal_system      triclinic
_space_group_IT_number           2
_space_group_name_Hall           '-P 1'
_space_group_name_H-M_alt        'P -1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     iterative
_audit_creation_date             2023-04-12
_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                60.328(11)
_cell_angle_beta                 65.25(4)
_cell_angle_gamma                82.83(3)
_cell_formula_units_Z            1
_cell_length_a                   15.637(8)
_cell_length_b                   15.719(5)
_cell_length_c                   15.754(6)
_cell_measurement_reflns_used    7356
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      50.36
_cell_measurement_theta_min      3.13
_cell_volume                     3039(2)
_computing_cell_refinement       'SAINT v8.37A (Bruker, 2015)'
_computing_data_reduction        'SAINT v8.37A (Bruker, 2015)'
_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      293.15
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0782
_diffrn_reflns_av_unetI/netI     0.0925
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            21198
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        50.625
_diffrn_reflns_theta_max         50.625
_diffrn_reflns_theta_min         3.129
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    9.070
_exptl_absorpt_correction_T_max  0.7500
_exptl_absorpt_correction_T_min  0.5556
_exptl_absorpt_correction_type   none
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0873 before and 0.0563 after correction.
The Ratio of minimum to maximum transmission is 0.7408.
The \l/2 correction factor is Not present.
;
_exptl_crystal_density_diffrn    1.468
_exptl_crystal_description       block
_exptl_crystal_F_000             1360
_refine_diff_density_max         0.782
_refine_diff_density_min         -1.156
_refine_diff_density_rms         0.135
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.034
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     703
_refine_ls_number_reflns         6346
_refine_ls_number_restraints     1359
_refine_ls_restrained_S_all      1.045
_refine_ls_R_factor_all          0.1224
_refine_ls_R_factor_gt           0.0763
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1232P)^2^+17.4769P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1951
_refine_ls_wR_factor_ref         0.2208
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4262
_reflns_number_total             6346
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4ce00494a2.cif
_cod_data_source_block           cu_zhangh20230306_2_0m_sq
_cod_database_code               7249532
_shelx_shelxl_version_number     2016/6
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C35-O26
 1.2 with sigma of 0.02
 C35-N4
 1.3 with sigma of 0.02
 N4-C37
 1.4 with sigma of 0.02
 N4-C38
 1.4 with sigma of 0.02
 C38-C35
 2.4 with sigma of 0.02
 C37-C35
 2.4 with sigma of 0.02
 C37-C38
 2.4 with sigma of 0.02
 C38-O26
 2.7 with sigma of 0.02
 O26-C37
 2.7 with sigma of 0.02
 N4-O26
 2.4 with sigma of 0.02
3. Restrained planarity
 C38, O26, C35, N4, C37
 with sigma of 0.1
 N4, O26, C35, C37, C38
 with sigma of 0.1
4. Rigid bond restraints
 C3, C4
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.02
5. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C9 \\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C5
\\sim C4 \\sim C14 \\sim C7 \\sim C15 \\sim C16 \\sim C17 \\sim C6 \\sim C18
\\sim C19 \\sim C20 \\sim C8 \\sim C21 \\sim C22 \\sim C23 \\sim C24 \\sim C25
\\sim C26 \\sim C27 \\sim C28 \\sim C29 \\sim N3 \\sim C30 \\sim C31 \\sim C32
\\sim C33 \\sim C34 \\sim C35 \\sim C36 \\sim C37 \\sim C38 \\sim N1 \\sim N2
\\sim N4 \\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: within 3.8A with sigma of 0.01 and sigma for terminal
atoms of 0.03
Uanis(C11) \\sim Ueq, Uanis(N2) \\sim Ueq, Uanis(O26) \\sim Ueq, Uanis(C35)
\\sim Ueq, Uanis(N4) \\sim Ueq, Uanis(C37) \\sim Ueq, Uanis(C38) \\sim Ueq,
Uanis(C34) \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(C36) \\sim Ueq: with sigma of
0.01 and sigma for terminal atoms of 0.02
Uanis(C4) \\sim Ueq, Uanis(C3) \\sim Ueq: with sigma of 0.01 and sigma for
terminal atoms of 0.02
6. Others
 Fixed Sof: O25(0.5) O26(0.5) C11(0.5) H11A(0.5) H11B(0.5) H11C(0.5) N2(0.5)
 C34(0.5) H34(0.5) N4(0.5) C35(0.5) H35(0.5) C36(0.5) H36B(0.5) H36C(0.5)
 H36A(0.5) C37(0.5) H37C(0.5) H37B(0.5) H37A(0.5) C38(0.5) H38A(0.5) H38B(0.5)
 H38C(0.5)
7.a Aromatic/amide H refined with riding coordinates:
 C4(H4), C5(H5), C6(H6), C7(H7), C8(H8), C10(H10), C18(H18), C19(H19),
 C20(H20), C21(H21), C22(H22), C23(H23), C25(H25), C26(H26), C27(H27), C28(H28),
  C29(H29), C30(H30), C31(H31), C32(H32), C34(H34), C35(H35)
7.b Fitted hexagon refined as free rotating group:
 C3(C4,C5,C6,C7,C8)
7.c Idealised Me refined as rotating group:
 C11(H11A,H11B,H11C), C12(H12A,H12B,H12C), C13(H13A,H13B,H13C), C14(H14A,H14B,
 H14C), C15(H15A,H15B,H15C), C16(H16A,H16B,H16C), C17(H17A,H17B,H17C), C24(H24A,
 H24B,H24C), C33(H33A,H33B,H33C), C36(H36B,H36C,H36A), C37(H37C,H37B,H37A),
 C38(H38A,H38B,H38C)
;
_shelx_res_checksum              68890
_shelx_hkl_checksum              15395
_shelx_fab_checksum              42049
_olex2_submission_special_instructions 'No special instructions were received'