Amine functionalized quinolinium polyoxometalates as highly active heterogeneous catalysts for solvent-free CO<sub>2</sub> cycloaddition and Knoevenagel condensation reactions.
Routh, Kousik; Kumar Swain, Rajesha; Kumar, Gaurav; Pradeep, Chullikkattil P.; Dalton transactions (Cambridge, England : 2003) 54 (2025) 12324–12339; doi:10.1039/d5dt00934k

data_7719124
_publ_section_title
;
 Amine functionalized quinolinium polyoxometalates as highly active
 heterogeneous catalysts for solvent-free CO<sub>2</sub> cycloaddition and
 Knoevenagel condensation reactions.
;
_journal_issue                   32
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              12324
_journal_page_last               12339
_journal_paper_doi               10.1039/d5dt00934k
_journal_volume                  54
_journal_year                    2025
_chemical_formula_moiety         'O28 V10, 4(C10 H10 Cl N2), 2(C3 H7 N O), 2(O)'
_chemical_formula_sum            'C46 H60 Cl4 N10 O32 V10'
_chemical_formula_weight         1916.24
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-08-27
_audit_creation_method
;
Olex2 1.3
(compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6408)
;
_audit_update_record
;
2024-10-11 deposited with the CCDC.	2025-07-16 downloaded from the CCDC.
;
_cell_angle_alpha                114.428(5)
_cell_angle_beta                 99.672(4)
_cell_angle_gamma                99.647(4)
_cell_formula_units_Z            1
_cell_length_a                   10.7219(4)
_cell_length_b                   12.6345(6)
_cell_length_c                   14.2538(10)
_cell_measurement_reflns_used    3466
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      27.4030
_cell_measurement_theta_min      2.2080
_cell_volume                     1671.52(18)
_computing_cell_refinement       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_collection       'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_computing_data_reduction        'CrysAlisPro 1.171.39.46e (Rigaku OD, 2018)'
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.977
_diffrn_measured_fraction_theta_max 0.858
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w     35.00 120.00   1.00   59.55    --   26.84 178.00  90.00   85
  2  \w     28.00 102.00   1.00   59.55    --   26.84  37.00 -60.00   74
  3  \w    -51.00  65.00   1.00   59.55    --   26.84 -77.00  60.00  116
  4  \w    -47.00  64.00   1.00   59.55    --   26.84 -57.00 150.00  111
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'SuperNova, Dual, Cu at home/near, Eos'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0279178000
_diffrn_orient_matrix_UB_12      0.0111277000
_diffrn_orient_matrix_UB_13      0.0530526000
_diffrn_orient_matrix_UB_21      -0.0304922000
_diffrn_orient_matrix_UB_22      -0.0604714000
_diffrn_orient_matrix_UB_23      -0.0131288000
_diffrn_orient_matrix_UB_31      0.0559651000
_diffrn_orient_matrix_UB_32      -0.0175056000
_diffrn_orient_matrix_UB_33      -0.0149903000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0454
_diffrn_reflns_av_unetI/netI     0.0730
_diffrn_reflns_Laue_measured_fraction_full 0.977
_diffrn_reflns_Laue_measured_fraction_max 0.858
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -12
_diffrn_reflns_limit_k_max       12
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       17
_diffrn_reflns_limit_l_min       -18
_diffrn_reflns_number            9772
_diffrn_reflns_point_group_measured_fraction_full 0.977
_diffrn_reflns_point_group_measured_fraction_max 0.858
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.173
_diffrn_reflns_theta_min         1.835
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.586
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.618
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.46e (Rigaku Oxford Diffraction, 2018)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_density_diffrn    1.904
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       triclinic
_exptl_crystal_F_000             960
_exptl_crystal_size_max          0.233
_exptl_crystal_size_mid          0.126
_exptl_crystal_size_min          0.084
_refine_diff_density_max         1.130
_refine_diff_density_min         -0.979
_refine_diff_density_rms         0.129
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.039
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     465
_refine_ls_number_reflns         7052
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.039
_refine_ls_R_factor_all          0.0939
_refine_ls_R_factor_gt           0.0687
_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^)+(0.1076P)^2^+0.8086P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1770
_refine_ls_wR_factor_ref         0.2064
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4986
_reflns_number_total             7052
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00934k2.cif
_cod_data_source_block           gk_114_1_rt_mo
_cod_depositor_comments
'Adding full bibliography for 7719124--7719126.cif.'
_cod_original_cell_volume        1671.50(17)
_cod_database_code               7719124
_shelx_shelxl_version_number     2018/3
_publ_section_exptl
;
Any special experimental details
;
_chemical_oxdiff_formula         'C46  H58  Cl4  N10  O32  V10  '
_reflns_odcompleteness_completeness 98.35
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     26.32
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H,H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Rotating group:
 N4(H4A,H4B)
2.b Aromatic/amide H refined with riding coordinates:
 C18(H18), C15(H15), C12(H12), C5(H5), C2(H2), C11(H11), C16(H16), C8(H8),
 C6(H6), C23(H23), C1(H1)
2.c X=CH2 refined with riding coordinates:
 N2(H2A,H2B)
2.d Idealised Me refined as rotating group:
 C20(H20A,H20B,H20C), C10(H10A,H10B,H10C), C21(H21A,H21B,H21C), C22(H22A,H22B,
 H22C)
;
_shelx_res_checksum              36340
_shelx_hkl_checksum              20079
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 8.919
_oxdiff_exptl_absorpt_empirical_full_min 0.590