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_7718326
_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         'O38 P W12, 4(C9 H8 N4 O), 2(O)'
_chemical_formula_sum            'C36 H32 N16 O44 P W12'
_chemical_formula_weight         3629.94
_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   mixed
_audit_creation_date             2025-02-15
_audit_creation_method
;
Olex2 1.5
(compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928)
;
_audit_update_record
;
2025-02-25 deposited with the CCDC.	2025-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                107.005(3)
_cell_angle_beta                 105.237(3)
_cell_angle_gamma                101.335(3)
_cell_formula_units_Z            1
_cell_length_a                   11.6205(13)
_cell_length_b                   13.7809(16)
_cell_length_c                   14.1474(16)
_cell_measurement_reflns_used    9778
_cell_measurement_temperature    100.28
_cell_measurement_theta_max      28.27
_cell_measurement_theta_min      2.28
_cell_volume                     1996.5(4)
_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      100.28
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.985
_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  0.0944
_diffrn_reflns_av_unetI/netI     0.0980
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.985
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            40910
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.985
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.566
_diffrn_reflns_theta_min         2.581
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    17.320
_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    orange
_exptl_crystal_density_diffrn    3.019
_exptl_crystal_description       block
_exptl_crystal_F_000             1615
_exptl_crystal_size_max          0.223
_exptl_crystal_size_mid          0.183
_exptl_crystal_size_min          0.151
_refine_diff_density_max         6.312
_refine_diff_density_min         -3.135
_refine_diff_density_rms         0.373
_refine_ls_extinction_coef       0.00025(7)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2014/7 (Sheldrick 2014'
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     536
_refine_ls_number_reflns         10047
_refine_ls_number_restraints     125
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.1123
_refine_ls_R_factor_gt           0.0524
_refine_ls_shift/su_max          4.848
_refine_ls_shift/su_mean         0.023
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0708P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1218
_refine_ls_wR_factor_ref         0.1454
_reflns_Friedel_coverage         0.000
_reflns_number_gt                5987
_reflns_number_total             10047
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d4dt03480e2.cif
_cod_data_source_block           2
_cod_depositor_comments
'Adding full bibliography for 7718325--7718327.cif.'
_cod_database_code               7718326
_shelx_shelxl_version_number     2014/7
_shelx_estimated_absorpt_t_max   0.180
_shelx_estimated_absorpt_t_min   0.113
_olex2_refinement_description
;
1. Restrained distances
 H3-C3
 0.93 with sigma of 0.02
 O2-C14 \\sim O2A-C14
 with sigma of 0.02
 C3-C4 \\sim C3-C4A
 with sigma of 0.02
 O1-C5 \\sim O1A-C9A
 with sigma of 0.02
 C4-C9 \\sim C4A-C5A
 with sigma of 0.02
 C4-C5 \\sim C4A-C9A
 with sigma of 0.02
 C9-C8 \\sim C5A-C6A
 with sigma of 0.02
 C8-C7 \\sim C6A-C7A
 with sigma of 0.02
 C7-C6 \\sim C7A-C8A
 with sigma of 0.02
 C6-C5 \\sim C8A-C9A
 with sigma of 0.02
 C3-C9 \\sim C3-C5A
 with sigma of 0.04
 C3-C5 \\sim C3-C9A
 with sigma of 0.04
 O1-C4 \\sim O1A-C4A
 with sigma of 0.04
 O1-C6 \\sim O1A-C8A
 with sigma of 0.04
 C4-C8 \\sim C4A-C6A
 with sigma of 0.04
 C4-C6 \\sim C4A-C8A
 with sigma of 0.04
 C9-C7 \\sim C5A-C7A
 with sigma of 0.04
 C9-C5 \\sim C5A-C9A
 with sigma of 0.04
 C8-C6 \\sim C6A-C8A
 with sigma of 0.04
 C7-C5 \\sim C7A-C9A
 with sigma of 0.04
2. Uiso/Uaniso restraints and constraints
Uanis(O1) \\sim Ueq, Uanis(C4) \\sim Ueq, Uanis(C9) \\sim Ueq, Uanis(C8) \\sim
Ueq, Uanis(C7) \\sim Ueq, Uanis(C6) \\sim Ueq, Uanis(C5) \\sim Ueq, Uanis(O1A)
\\sim Ueq, Uanis(C9A) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(C8A) \\sim Ueq,
Uanis(C7A) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(O11)
\\sim Ueq, Uanis(O4) \\sim Ueq, Uanis(P1) \\sim Ueq: with sigma of 0.005 and
sigma for terminal atoms of 0.01
Uanis(O2A) = Uanis(O2)
Uanis(C4) = Uanis(C4A)
Uanis(C9A) = Uanis(C5A)
Uanis(C9) = Uanis(C5)
Uanis(C9) = Uanis(C5A)
Uanis(C8) = Uanis(C6A)
Uanis(C7) = Uanis(C7A)
Uanis(C9A) = Uanis(C5)
Uanis(C8A) = Uanis(C6)
Uanis(O1A) = Uanis(O1)
3. Rigid body (RIGU) restrains
 P1, O4
 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004
4. Others
 Sof(O2A)=1-FVAR(1)
 Sof(O2)=FVAR(1)
 Sof(O1A)=Sof(C9A)=Sof(C4A)=Sof(C8A)=Sof(H8A)=Sof(C7A)=Sof(H7A)=Sof(C6A)=
 Sof(H6A)=Sof(C5A)=Sof(H5A)=1-FVAR(2)
 Sof(O1)=Sof(C4)=Sof(C9)=Sof(H9)=Sof(C8)=Sof(H8)=Sof(C7)=Sof(H7)=Sof(C6)=
 Sof(H6)=Sof(C5)=FVAR(2)
 Fixed Sof: O5(0.5) O6(0.5) O3(0.5) O4(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 N4(H4), N8(H8B), C2(H2), C1(H1), C15(H15), C16(H16), C18(H18), C12(H12),
 C11(H11), C10(H10), C9(H9), C17(H17), C8(H8), C7(H7), C6(H6), C8A(H8A),
 C7A(H7A), C6A(H6A), C5A(H5A)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              99016
_shelx_hkl_checksum              44681
_shelx_fab_checksum              11662
_olex2_submission_special_instructions 'No special instructions were received'