Two Dawson-type polyoxometalate-based metal coordination polymers as heterogeneous catalysts for desulfurization
Hao, Xiu-Li; Zhang, Chen-Hao; Feng, Chen-Kun; Su, Tian-Ru; Zhao, Mei-mei; Wen, Yan-Zhen; New Journal of Chemistry 49 (2025) 14874–14881; doi:10.1039/D5NJ02349A

data_7063922
_publ_section_title
;
 Two Dawson-type polyoxometalate-based metal coordination polymers as
 heterogeneous catalysts for desulfurization
;
_journal_issue                   34
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              14874
_journal_page_last               14881
_journal_paper_doi               10.1039/D5NJ02349A
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety
'C36 H32 Co N12 O62 P2 W18, 2(C18 H18 N6), 2(H2 O)'
_chemical_formula_sum            'C72 H72 Co N24 O64 P2 W18'
_chemical_formula_weight         5727.70
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-07-21
_audit_creation_method
;
Olex2 1.5
(compiled 2022.04.07 svn.rca3783a0 for OlexSys, GUI svn.r6498)
;
_audit_update_record
;
2025-07-22 deposited with the CCDC.	2025-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 104.396(8)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   26.675(2)
_cell_length_b                   16.1311(12)
_cell_length_c                   30.321(2)
_cell_measurement_reflns_used    5846
_cell_measurement_temperature    150.15
_cell_measurement_theta_max      29.2079
_cell_measurement_theta_min      3.0058
_cell_volume                     12637.4(16)
_computing_cell_refinement       'CrysAlisPro, Agilent Technologies,'
_computing_data_collection       'CrysAlisPro, Agilent Technologies,'
_computing_data_reduction        'CrysAlisPro, Agilent Technologies,'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      150.15
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.994
_diffrn_measurement_device_type  'multiwire proportional'
_diffrn_measurement_method       'phi and omega scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0638
_diffrn_reflns_av_unetI/netI     0.0953
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       30
_diffrn_reflns_limit_h_min       -31
_diffrn_reflns_limit_k_max       14
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_limit_l_min       -25
_diffrn_reflns_number            22761
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         3.012
_exptl_absorpt_coefficient_mu    16.556
_exptl_absorpt_correction_T_max  0.1216
_exptl_absorpt_correction_T_min  0.0989
_exptl_absorpt_correction_type   multi-scan
_exptl_crystal_colour            yellow
_exptl_crystal_colour_primary    yellow
_exptl_crystal_density_diffrn    3.010
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             10292
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.03
_exptl_crystal_size_min          0.02
_refine_diff_density_max         3.414
_refine_diff_density_min         -3.503
_refine_diff_density_rms         0.436
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.041
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     796
_refine_ls_number_reflns         11067
_refine_ls_number_restraints     1598
_refine_ls_restrained_S_all      0.980
_refine_ls_R_factor_all          0.1001
_refine_ls_R_factor_gt           0.0685
_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^)+(0.0874P)^2^+250.7069P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1632
_refine_ls_wR_factor_ref         0.1892
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7634
_reflns_number_total             11067
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj02349a2.cif
_cod_data_source_block           4
_cod_depositor_comments
'Adding full bibliography for 7063922--7063923.cif.'
_cod_database_code               7063922
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.733
_shelx_estimated_absorpt_t_min   0.492
_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,H) groups
2. Restrained distances
 C1-N1
 1.4 with sigma of 0.01
 C2-N1
 1.4 with sigma of 0.01
3. Uiso/Uaniso restraints and constraints
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C20 \\sim C8 \\sim C9
\\sim C10 \\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C15 \\sim C16 \\sim C17
\\sim C18 \\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 C37 \\sim C36 \\sim C38: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 3.8A
O1 \\sim O2 \\sim O3 \\sim O4 \\sim O5 \\sim O6 \\sim O7 \\sim O32 \\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: within 3.8A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
P1 \\sim O18 \\sim O7 \\sim O17 \\sim O5: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
N9 \\sim N19 \\sim C37 \\sim N7 \\sim C36: within 2A with sigma of 0.01 and
sigma for terminal atoms of 0.02 within 2A
C34 \\sim N10 \\sim N36 \\sim C38 \\sim N11 \\sim C35: within 2A with sigma of
0.001 and sigma for terminal atoms of 0.002 within 2A
N36 \\sim N1 \\sim N2 \\sim N3 \\sim N4 \\sim N5 \\sim N6 \\sim N9 \\sim N19
\\sim N7 \\sim N10 \\sim N11: within 3.8A with sigma of 0.01 and sigma for
terminal atoms of 0.02 within 3.8A
Uanis(P1) \\sim Ueq: with sigma of 0.001 and sigma for terminal atoms of 0.002
4. Rigid body (RIGU) restrains
 P1
 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01
5.a Riding coordinates:
 O8(H8A,H8B)
5.b Secondary CH2 refined with riding coordinates:
 C3(H3A,H3B), C16(H16A,H16B), C21(H21A,H21B), C34(H34A,H34B)
5.c Aromatic/amide H refined with riding coordinates:
 C1(H1), C2(H2), C5(H5), C6(H6), C8(H8), C9(H9), C11(H11), C12(H12), C14(H14),
 C15(H15), C17(H17), C18(H18), C27(H27), C26(H26), C24(H24), C23(H23), C29(H29),
  C30(H30), C32(H32), C33(H33), C35(H35), N36(H36), N19(H19), C37(H37),
 C36(H36A), C38(H38)
5.d Fitted pentagon refined as free rotating group:
 N9(N19,C37,N7,C36)
5.e Fitted hexagon refined as free rotating group:
 C22(C27,C26,C25,C24,C23)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 388 electrons were 
found in a volume of 2072\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
2.425[C3H7NO] per Formula Unit 
which account for 388 electrons 
per unit cell.
;
_shelx_res_checksum              13219
_shelx_fab_checksum              38419
_olex2_submission_special_instructions 'No special instructions were received'