Hourglass-type polyoxometalate-based crystalline materials as efficient cooperating photocatalysts for the reduction of Cr(vi) and oxidation of dyes
Tian, Xuerui; Zhang, Yaqi; Ma, Yuanyuan; Zhao, Qing; Han, Zhangang; Catalysis Science & Technology 10 (2020) 2593–2601; doi:10.1039/D0CY00208A

data_1557528
_publ_section_title
;
 Hourglass-type polyoxometalate-based crystalline materials as efficient
 cooperating photocatalysts for the reduction of Cr(vi) and oxidation of
 dyes
;
_journal_issue                   8
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              2593
_journal_page_last               2601
_journal_paper_doi               10.1039/D0CY00208A
_journal_volume                  10
_journal_year                    2020
_chemical_formula_moiety
'0.5(Cd2 H12 Mo24 O124 P16 Zn4), 3(C13 H16 N2)'
_chemical_formula_sum            'C39 H72 Cd Mo12 N6 O68 P8 Zn2'
_chemical_formula_weight         3355.20
_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
_audit_creation_date             2019-07-25
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2019-07-31 deposited with the CCDC.	2020-03-06 downloaded from the CCDC.
;
_cell_angle_alpha                113.698(4)
_cell_angle_beta                 101.194(4)
_cell_angle_gamma                90.634(4)
_cell_formula_units_Z            4
_cell_length_a                   13.126(4)
_cell_length_b                   25.198(7)
_cell_length_c                   30.034(8)
_cell_measurement_reflns_used    9867
_cell_measurement_temperature    296(2)
_cell_measurement_theta_max      28.06
_cell_measurement_theta_min      2.29
_cell_volume                     8879(4)
_computing_cell_refinement       'Bruker SMART'
_computing_data_collection       'Bruker SMART'
_computing_data_reduction        'Bruker SAINT'
_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    'Bruker SHELXTL'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.937
_diffrn_measured_fraction_theta_max 0.937
_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  0.0261
_diffrn_reflns_av_unetI/netI     0.0512
_diffrn_reflns_Laue_measured_fraction_full 0.937
_diffrn_reflns_Laue_measured_fraction_max 0.937
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -29
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -35
_diffrn_reflns_number            39508
_diffrn_reflns_point_group_measured_fraction_full 0.937
_diffrn_reflns_point_group_measured_fraction_max 0.937
_diffrn_reflns_theta_full        24.999
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         2.074
_exptl_absorpt_coefficient_mu    2.658
_exptl_absorpt_correction_T_max  0.671
_exptl_absorpt_correction_T_min  0.610
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details   sadabs
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    2.510
_exptl_crystal_description       block
_exptl_crystal_F_000             6496
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         7.318
_refine_diff_density_min         -1.423
_refine_diff_density_rms         0.243
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.044
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     2335
_refine_ls_number_reflns         29286
_refine_ls_number_restraints     1417
_refine_ls_restrained_S_all      1.025
_refine_ls_R_factor_all          0.0798
_refine_ls_R_factor_gt           0.0601
_refine_ls_shift/su_max          0.020
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0720P)^2^+195.8229P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1644
_refine_ls_wR_factor_ref         0.1838
_reflns_Friedel_coverage         0.000
_reflns_number_gt                22136
_reflns_number_total             29286
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cy00208a3.cif
_cod_data_source_block           txr85_0m
_cod_depositor_comments
;Adding full bibliography for 1557528--1557530.cif.

 Adding full bibliography for 1557528--1557530.cif.
;
_cod_database_code               1557528
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.646
_shelx_estimated_absorpt_t_min   0.618
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups, All N(H) groups
 At 1.5 times of:
  All O(H) groups
2. Restrained distances
 C74-C73
 1.55 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 C73
\\sim C74 \\sim C75 \\sim C76 \\sim C77 \\sim C78: within 3.8A with sigma of
0.04 and sigma for terminal atoms of 0.02
Uanis(C1) \\sim Ueq, Uanis(C23) \\sim Ueq, Uanis(C31) \\sim Ueq, Uanis(C72)
\\sim Ueq, Uanis(N8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms
of 0.02
Uanis(N12) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
4.a Secondary CH2 refined with riding coordinates:
 C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C19(H19A,H19B), C20(H20A,H20B),
 C21(H21A,H21B), C32(H32A,H32B), C33(H33A,H33B), C34(H34A,H34B), C45(H45A,H45B),
  C46(H46A,H46B), C47(H47A,H47B), C58(H58A,H58B), C59(H59A,H59B), C60(H60A,
 H60B), C71(H71A,H71B), C72(H72A,H72B), C73(H73A,H73B)
4.b Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C4(H4), C5(H5), C9(H9), C10(H10), C12(H12), C13(H13A),
 C14(H14), C15(H15), C17(H17), C18(H18), C22(H22), C23(H23), C25(H25), C26(H26),
  C27(H27), C28(H28), C30(H30A), C31(H31), C35(H35A), C36(H36), C38(H38),
 C39(H39A), C40(H40), C41(H41), C43(H43), C44(H44), C48(H48), C49(H49),
 C51(H51), C52(H52), C53(H53), C54(H54), C56(H56), C57(H57), C61(H61), C62(H62),
  C64(H64), C65(H65), C66(H66), C67(H67A), C69(H69), C70(H70), C75(H75),
 C76(H76), N12(H12A), C77(H77), C78(H78), N1(H1A), N2(H2A), N3(H3), N4(H4A),
 N5(H5A), N6(H6), N7(H7), N8(H8), N9(H9A), N10(H10A), N11(H11)
4.c Fitted hexagon refined as free rotating group:
 C74(C75,C76,N12,C77,C78)
4.d Tetrahedral OH refined with riding coordinates:
 O13(H13), O20(H20), O30(H30), O32(H32), O35(H35), O39(H39), O67(H67),
 O82(H82), O85(H85), O98(H98), O115(H115), O121(H121)
;
_shelx_res_checksum              61522
_olex2_submission_special_instructions 'No special instructions were received'