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_1557529
_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(C26 N4), 0.25(Cd4.8 Co3.2 H32 Mo48 Na16 O268 P32), C13 H16 N2, 2(O)'
_chemical_formula_sum            'C26 H24 Cd1.2 Co0.8 Mo12 N4 Na4 O69 P8'
_chemical_formula_weight         3169.51
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   mixed
_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                90
_cell_angle_beta                 100.716(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   21.0842(6)
_cell_length_b                   18.3743(5)
_cell_length_c                   21.9022(6)
_cell_measurement_reflns_used    15730
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      25.010
_cell_measurement_theta_min      3.129
_cell_volume                     8337.1(4)
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_diffrn_ambient_temperature      293(2)
_diffrn_measured_fraction_theta_full 0.996
_diffrn_measured_fraction_theta_max 0.996
_diffrn_measurement_device_type  'CCD area detector'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0255
_diffrn_reflns_av_unetI/netI     0.0392
_diffrn_reflns_Laue_measured_fraction_full 0.996
_diffrn_reflns_Laue_measured_fraction_max 0.996
_diffrn_reflns_limit_h_max       25
_diffrn_reflns_limit_h_min       -25
_diffrn_reflns_limit_k_max       21
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       25
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            15730
_diffrn_reflns_point_group_measured_fraction_full 0.996
_diffrn_reflns_point_group_measured_fraction_max 0.996
_diffrn_reflns_theta_full        25.010
_diffrn_reflns_theta_max         25.010
_diffrn_reflns_theta_min         3.129
_exptl_absorpt_coefficient_mu    2.485
_exptl_absorpt_correction_T_max  0.723
_exptl_absorpt_correction_T_min  0.661
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            'brownish red'
_exptl_crystal_density_diffrn    2.525
_exptl_crystal_description       block
_exptl_crystal_F_000             6029
_exptl_crystal_size_max          0.2
_exptl_crystal_size_mid          0.19
_exptl_crystal_size_min          0.18
_refine_diff_density_max         1.661
_refine_diff_density_min         -3.914
_refine_diff_density_rms         0.202
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     623
_refine_ls_number_reflns         7315
_refine_ls_number_restraints     655
_refine_ls_restrained_S_all      1.003
_refine_ls_R_factor_all          0.0494
_refine_ls_R_factor_gt           0.0429
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0560P)^2^+190.7261P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1165
_refine_ls_wR_factor_ref         0.1205
_reflns_Friedel_coverage         0.000
_reflns_number_gt                6480
_reflns_number_total             7315
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cy00208a3.cif
_cod_data_source_block           170717-cd-co-ml_sq
_cod_depositor_comments
;Adding full bibliography for 1557528--1557530.cif.

 Adding full bibliography for 1557528--1557530.cif.
;
_cod_original_formula_sum        'C26 H24 Cd1.20 Co0.80 Mo12 N4 Na4 O69 P8'
_cod_database_code               1557529
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.663
_shelx_estimated_absorpt_t_min   0.636
_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. Shared sites
{Cd2, Co2}
3. Restrained distances
 C14-C15
 1.55 with sigma of 0.02
4. Uiso/Uaniso restraints and constraints
C14' \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C9' \\sim C10' \\sim
C11' \\sim C12' \\sim C13' \\sim C15 \\sim N1 \\sim N2 \\sim N2': within 3.8A
with sigma of 0.04 and sigma for terminal atoms of 0.02
C14' \\sim C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C7 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C9' \\sim C10' \\sim
C11' \\sim C12' \\sim C13' \\sim C15: within 3.8A with sigma of 0.04 and sigma
for terminal atoms of 0.02
Uanis(O3W) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02
Uanis(Cd2) = Uanis(Co2)
5. Others
 Fixed Sof: C14'(0.5) Cd2(0.1) Co2(0.4) H1A(0.5) H1B(0.5) N2(0.5) C9(0.5)
 C10(0.5) C11(0.5) C12(0.5) C13(0.5) C14(0.5) N2'(0.5) C9'(0.5) C10'(0.5)
 C11'(0.5) C12'(0.5) C13'(0.5) C15(0.5) O2W(0.75) O3W(0.5) O4W(0.25)
6.a Riding coordinates:
 O5(H5), O7(H7), O12(H12)
6.b Secondary CH2 refined with riding coordinates:
 C1(H1A,H1B), C2(H2A,H2B)
6.c Aromatic/amide H refined with riding coordinates:
 N1(H1), C3(H3), C5(H5A), C7(H7A), C8(H8)
6.d Fitted hexagon refined as free rotating group:
 N2(C9,C10,C11,C12,C13), N2'(C9',C10',C11',C12',C13')
6.e Tetrahedral OH refined with riding coordinates:
 O18(H18)
;
_shelx_res_checksum              78835
_shelx_fab_checksum              13834
_olex2_submission_special_instructions 'No special instructions were received'