Inorganic-organic hybrids of the phosphotungstate Keggin anion and a Schiff base cation.
Mishra, Neeraj Kumar; Panday, Rishukumar; Supriya, Sabbani; Dalton transactions (Cambridge, England : 2003) 54 (2025) 7062–7070; doi:10.1039/d4dt03480e

data_7718325
_publ_section_title
;
 Inorganic-organic hybrids of the phosphotungstate Keggin anion and a
 Schiff base cation.
;
_journal_issue                   17
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              7062
_journal_page_last               7070
_journal_paper_doi               10.1039/d4dt03480e
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'O40 P W12, 4(C9 H9 N4 O), 4(C H4 O)'
_chemical_formula_sum            'C40 H52 N16 O48 P W12'
_chemical_formula_weight         3762.14
_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             2024-12-02
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2024-12-15 deposited with the CCDC.	2025-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                73.774(3)
_cell_angle_beta                 86.419(3)
_cell_angle_gamma                64.554(2)
_cell_formula_units_Z            1
_cell_length_a                   11.5239(11)
_cell_length_b                   12.7389(11)
_cell_length_c                   14.3481(13)
_cell_measurement_reflns_used    9778
_cell_measurement_temperature    100
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.28
_cell_volume                     1822.2(3)
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'XL  (Sheldrick, 2008)'
_diffrn_ambient_temperature      100
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0514
_diffrn_reflns_av_unetI/netI     0.0361
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       17
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       19
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            59080
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.360
_diffrn_reflns_theta_min         2.277
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    18.987
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.4810
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.1157 before and 0.0611 after correction.
The Ratio of minimum to maximum transmission is 0.6450.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_colour            'metallic dark orange'
_exptl_crystal_colour_lustre     metallic
_exptl_crystal_colour_modifier   dark
_exptl_crystal_colour_primary    green
_exptl_crystal_density_diffrn    3.428
_exptl_crystal_description       block
_exptl_crystal_F_000             1691
_exptl_crystal_size_max          0.255
_exptl_crystal_size_mid          0.226
_exptl_crystal_size_min          0.215
_refine_diff_density_max         2.686
_refine_diff_density_min         -4.172
_refine_diff_density_rms         0.407
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.488
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     560
_refine_ls_number_reflns         9083
_refine_ls_number_restraints     171
_refine_ls_restrained_S_all      1.477
_refine_ls_R_factor_all          0.0844
_refine_ls_R_factor_gt           0.0733
_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^)+134.3435P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1674
_refine_ls_wR_factor_ref         0.1705
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7974
_reflns_number_total             9083
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03480e2.cif
_cod_data_source_block           1
_cod_depositor_comments
'Adding full bibliography for 7718325--7718327.cif.'
_cod_database_code               7718325
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.106
_shelx_estimated_absorpt_t_min   0.085
_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 C(H,H,H) groups, All C(H,H,H,H,H,H) groups, All O(H) groups
2. Restrained distances
 C13-C14 \\sim C13-C14A
 with sigma of 0.02
 C13-C18 \\sim C13-C18A
 with sigma of 0.02
 C14-C15 \\sim C14A-C15A
 with sigma of 0.02
 C15-C16 \\sim C15A-C16A
 with sigma of 0.02
 C16-C17 \\sim C16A-C17A
 with sigma of 0.02
 C17-C18 \\sim C17A-C18A
 with sigma of 0.02
 C18-O25 \\sim C18A-O25A
 with sigma of 0.02
 C13-C15 \\sim C13-C15A
 with sigma of 0.04
 C13-C17 \\sim C13-C17A
 with sigma of 0.04
 C13-O25 \\sim C13-O25A
 with sigma of 0.04
 C14-C16 \\sim C14A-C16A
 with sigma of 0.04
 C15-C17 \\sim C15A-C17A
 with sigma of 0.04
 C16-C18 \\sim C16A-C18A
 with sigma of 0.04
 C17-O25 \\sim C17A-O25A
 with sigma of 0.04
 O24-C9 \\sim O24A-C9A
 with sigma of 0.02
 C3-C4 \\sim C3-C4A
 with sigma of 0.02
 C4-C5 \\sim C4A-C5A
 with sigma of 0.02
 C4-C9 \\sim C4A-C9A
 with sigma of 0.02
 C5-C6 \\sim C5A-C6A
 with sigma of 0.02
 C6-C7 \\sim C6A-C7A
 with sigma of 0.02
 C7-C8 \\sim C7A-C8A
 with sigma of 0.02
 C8-C9 \\sim C8A-C9A
 with sigma of 0.02
 O24-C4 \\sim O24A-C4A
 with sigma of 0.04
 O24-C8 \\sim O24A-C8A
 with sigma of 0.04
 C3-C5 \\sim C3-C5A
 with sigma of 0.04
 C3-C9 \\sim C3-C9A
 with sigma of 0.04
 C4-C6 \\sim C4A-C6A
 with sigma of 0.04
 C4-C8 \\sim C4A-C8A
 with sigma of 0.04
 C5-C7 \\sim C5A-C7A
 with sigma of 0.04
 C5-C9 \\sim C5A-C9A
 with sigma of 0.04
 C6-C8 \\sim C6A-C8A
 with sigma of 0.04
 C7-C9 \\sim C7A-C9A
 with sigma of 0.04
 O23-C19 \\sim O23A-C19
 with sigma of 0.02
3. Uiso/Uaniso restraints and constraints
Uanis(C4) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C7) \\sim
Ueq, Uanis(C8) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C5A)
\\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C7A) \\sim Ueq, Uanis(C8A) \\sim Ueq,
Uanis(C9A) \\sim Ueq, Uanis(O25) \\sim Ueq, Uanis(O7) \\sim Ueq, Uanis(O24)
\\sim Ueq, Uanis(O24A) \\sim Ueq, Uanis(O5) \\sim Ueq, Uanis(O8) \\sim Ueq,
Uanis(O23A) \\sim Ueq, Uanis(O23) \\sim Ueq, Uanis(O2) \\sim Ueq, Uanis(O3)
\\sim Ueq, Uanis(O20) \\sim Ueq: with sigma of 0.005 and sigma for terminal
atoms of 0.01
Uanis(C1) = Uanis(C2)
Uanis(C15) = Uanis(C17A)
Uanis(C16) = Uanis(C16A)
Uanis(C17) = Uanis(C15A)
Uanis(C18) = Uanis(C14A)
Uanis(O25A) = Uanis(O25)
Uanis(C14) = Uanis(C18A)
Uanis(C4A) = Uanis(C4)
Uanis(C9) = Uanis(C9A)
Uanis(O24A) = Uanis(O24)
Uanis(C8A) = Uanis(C8)
Uanis(C7A) = Uanis(C7)
Uanis(C6) = Uanis(C6A)
Uanis(C5A) = Uanis(C5)
Uanis(O23) = Uanis(O23A)
4. Rigid body (RIGU) restrains
 O2, O3, O20
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
5. Others
 Sof(O3)=Sof(O1)=1-FVAR(1)
 Sof(O4)=Sof(O2)=FVAR(1)
 Sof(O25A)=Sof(H25A)=Sof(C18A)=Sof(C17A)=Sof(H17A)=Sof(C16A)=Sof(H16A)=
 Sof(C15A)=Sof(H15A)=Sof(C14A)=Sof(H14A)=1-FVAR(2)
 Sof(C14)=Sof(H14)=Sof(C15)=Sof(H15)=Sof(C16)=Sof(H16)=Sof(C17)=Sof(H17)=
 Sof(C18)=Sof(O25)=Sof(H25)=FVAR(2)
 Sof(H3B)=Sof(C4A)=Sof(C5A)=Sof(H5A)=Sof(C6A)=Sof(H6A)=Sof(C7A)=Sof(H7A)=
 Sof(C8A)=Sof(H8A)=Sof(C9A)=Sof(O24A)=Sof(H24A)=1-FVAR(3)
 Sof(O24)=Sof(H24)=Sof(H3A)=Sof(C4)=Sof(C5)=Sof(H5)=Sof(C6)=Sof(H6)=Sof(C7)=
 Sof(H7)=Sof(C8)=Sof(H8)=Sof(C9)=FVAR(3)
 Sof(H19D)=Sof(H19E)=Sof(H19F)=Sof(O23A)=Sof(H23A)=1-FVAR(4)
 Sof(O23)=Sof(H23)=Sof(H19A)=Sof(H19B)=Sof(H19C)=FVAR(4)
6.a Aromatic/amide H refined with riding coordinates:
 N7(H7B), C14(H14), C15(H15), C16(H16), C17(H17), C10(H10), C3(H3A), C3(H3B),
 C11(H11), N4(H4), C12(H12), C2(H2), C1(H1), C5(H5), C6(H6), C7(H7), C8(H8),
 C17A(H17A), C16A(H16A), C15A(H15A), C14A(H14A), C5A(H5A), C6A(H6A), C7A(H7A),
 C8A(H8A)
6.b Fitted hexagon refined as free rotating group:
 C13(C14,C15,C16,C17,C18), C4(C5,C6,C7,C8,C9), C4A(C5A,C6A,C7A,C8A,C9A)
6.c Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C19(H19A,H19B,H19C), C19(H19D,H19E,H19F)
6.d Idealised tetrahedral OH refined as rotating group:
 O24(H24), O23(H23), O25(H25), O22(H22), O25A(H25A), O24A(H24A), O23A(H23A)
;
_shelx_res_checksum              77905
_shelx_hkl_checksum              57965
_olex2_submission_special_instructions 'No special instructions were received'