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_7063923
_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 H52 N18 Ni2 O66 P2 W18, 17.5[H2O]'
_chemical_formula_sum            'C36 H87 N18 Ni2 O83.5 P2 W18'
_chemical_formula_weight         5596.89
_space_group_crystal_system      monoclinic
_space_group_IT_number           11
_space_group_name_Hall           '-P 2yb'
_space_group_name_H-M_alt        'P 1 21/m 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     dual
_audit_creation_date             2025-07-21
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-07-22 deposited with the CCDC.	2025-07-25 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 98.249(6)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   14.3045(9)
_cell_length_b                   25.6821(16)
_cell_length_c                   14.4714(9)
_cell_measurement_reflns_used    5757
_cell_measurement_temperature    298(2)
_cell_measurement_theta_max      29.1805
_cell_measurement_theta_min      2.9472
_cell_volume                     5261.3(6)
_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      298.15
_diffrn_detector_area_resol_mean 10.2375
_diffrn_measured_fraction_theta_full 0.993
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_details
;
  1 omega   -3.00   79.00   1.0000   16.1800
omega____ theta____ kappa____ phi______ frames
    -       11.9025   57.0000   90.0000 82

  2 omega   -9.00   78.00   1.0000   16.1800
omega____ theta____ kappa____ phi______ frames
    -       11.9025   57.0000 -180.0000 87
;
_diffrn_measurement_device_type  'Xcalibur, Ruby, Gemini ultra'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_UB_11      0.0317614000
_diffrn_orient_matrix_UB_12      0.0021570000
_diffrn_orient_matrix_UB_13      -0.0332285000
_diffrn_orient_matrix_UB_21      -0.0387214000
_diffrn_orient_matrix_UB_22      -0.0002273000
_diffrn_orient_matrix_UB_23      -0.0365227000
_diffrn_orient_matrix_UB_31      -0.0027970000
_diffrn_orient_matrix_UB_32      0.0275542000
_diffrn_orient_matrix_UB_33      0.0022011000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0480
_diffrn_reflns_av_unetI/netI     0.0685
_diffrn_reflns_Laue_measured_fraction_full 0.993
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -17
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -30
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -17
_diffrn_reflns_number            19859
_diffrn_reflns_point_group_measured_fraction_full 0.993
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         25.000
_diffrn_reflns_theta_min         2.953
_diffrn_source                   'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    20.082
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.11734
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro, Agilent Technologies,
Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET)
(compiled Jan 23 2012,18:06:46)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            green
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    3.533
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             5030
_exptl_crystal_size_max          0.05
_exptl_crystal_size_mid          0.04
_exptl_crystal_size_min          0.02
_refine_diff_density_max         2.035
_refine_diff_density_min         -2.030
_refine_diff_density_rms         0.324
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.010
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     671
_refine_ls_number_reflns         9411
_refine_ls_number_restraints     1155
_refine_ls_restrained_S_all      0.964
_refine_ls_R_factor_all          0.0593
_refine_ls_R_factor_gt           0.0436
_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^)+(0.0409P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0946
_refine_ls_wR_factor_ref         0.1033
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7308
_reflns_number_total             9411
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5nj02349a2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7063922--7063923.cif.'
_cod_original_formula_sum        'C36 H87 N18 Ni2 O83.50 P2 W18'
_cod_database_code               7063923
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.690
_shelx_estimated_absorpt_t_min   0.433
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All C(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups, All O(H) groups, All O(H,H) groups
2. Restrained distances
 O14-H14A
 0.85 with sigma of 0.01
 W5-H14A
 2.158321 with sigma of 0.02
 Ni1-H14A
 2.23579 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
O1 \\sim O1W \\sim O2 \\sim O2W \\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: within 3.8A with
sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
N1 \\sim N2 \\sim N3 \\sim N4 \\sim N5 \\sim N7 \\sim N8 \\sim N9 \\sim N15:
within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 3.8A
C1 \\sim C2 \\sim C3 \\sim C4 \\sim C5 \\sim C6 \\sim C7 \\sim C8 \\sim C10
\\sim C11 \\sim C12 \\sim C13 \\sim C14 \\sim C16 \\sim C17 \\sim C18 \\sim C19
\\sim C20: within 3.8A with sigma of 0.01 and sigma for terminal atoms of 0.02
within 3.8A
N4 \\sim N5 \\sim N15 \\sim C6 \\sim C14: within 2A with sigma of 0.001 and
sigma for terminal atoms of 0.002 within 2A
Uanis(C10) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(N9) \\sim Ueq, Uanis(N3)
\\sim Ueq, Uanis(C1) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.01 and
sigma for terminal atoms of 0.02
4.a Riding coordinates:
 O1W(H1WA,H1WB)
4.b Rotating group:
 O2W(H2WA,H2WB)
4.c Secondary CH2 refined with riding coordinates:
 C10(H10A,H10B), C13(H13A,H13B), C20(H20A,H20B)
4.d Aromatic/amide H refined with riding coordinates:
 C1(H1), C3(H3), C6(H6), C14(H14), C17(H17), C18(H18)
4.e Idealised Me refined as rotating group:
 C2(H2A,H2B,H2C), C8(H8A,H8B,H8C), C16(H16A,H16B,H16C)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 350 electrons were 
found in a volume of 1256\%A^3^ in 1 void per unit cell. 
This is consistent with the presence of 
17.5[H2O] per Formula Unit 
which account for 350 electrons 
per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              38837
_shelx_fab_checksum              20711
_olex2_submission_special_instructions 'No special instructions were received'