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_7719126
_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
'O40 Si W12, 4(C10 H10 Cl N2), 2(C3 H7 N O), 4[C3H7NO]'
_chemical_formula_sum            'C58 H82 Cl4 N14 O46 Si W12'
_chemical_formula_weight         4087.361
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_symmetry_Int_Tables_number      14
_atom_sites_solution_primary     iterative
_audit_creation_date             2024-10-03
_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                90
_cell_angle_beta                 100.610(3)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.7825(3)
_cell_length_b                   27.3941(6)
_cell_length_c                   26.8909(8)
_cell_measurement_reflns_used    10836
_cell_measurement_temperature    150.03(17)
_cell_measurement_theta_max      27.9380
_cell_measurement_theta_min      2.3310
_cell_volume                     9979.3(4)
_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)'
_computing_molecular_graphics    'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.3 (Dolomanov et al., 2009)'
_computing_structure_refinement  'olex2.refine 1.3 (Bourhis et al., 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.03(17)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.9946
_diffrn_measured_fraction_theta_max 0.8613
_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    -32.00  87.00   1.00   50.00    --   26.84  19.00 -60.00  119
  2  \w    -12.00  86.00   1.00   50.00    --   26.84  57.00 120.00   98
;
_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      -0.0420964000
_diffrn_orient_matrix_UB_12      0.0153215000
_diffrn_orient_matrix_UB_13      -0.0055233000
_diffrn_orient_matrix_UB_21      0.0092016000
_diffrn_orient_matrix_UB_22      0.0085117000
_diffrn_orient_matrix_UB_23      0.0253499000
_diffrn_orient_matrix_UB_31      0.0297121000
_diffrn_orient_matrix_UB_32      0.0190593000
_diffrn_orient_matrix_UB_33      -0.0069140000
_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  0.0321
_diffrn_reflns_av_unetI/netI     0.0655
_diffrn_reflns_Laue_measured_fraction_full 0.9946
_diffrn_reflns_Laue_measured_fraction_max 0.8613
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       28
_diffrn_reflns_limit_k_min       -34
_diffrn_reflns_limit_l_max       35
_diffrn_reflns_limit_l_min       -32
_diffrn_reflns_number            33309
_diffrn_reflns_point_group_measured_fraction_full 0.9946
_diffrn_reflns_point_group_measured_fraction_max 0.8613
_diffrn_reflns_theta_full        25.2417
_diffrn_reflns_theta_max         28.45
_diffrn_reflns_theta_min         1.71
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    13.977
_exptl_absorpt_correction_T_max  0.278
_exptl_absorpt_correction_T_min  0.092
_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    2.721
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       monoclinic
_exptl_crystal_F_000             7449.960
_exptl_crystal_size_max          0.273
_exptl_crystal_size_mid          0.229
_exptl_crystal_size_min          0.158
_refine_diff_density_max         5.8412
_refine_diff_density_min         -3.8391
_refine_diff_density_rms         0.4945
_refine_ls_d_res_high            0.7459
_refine_ls_d_res_low             11.9029
_refine_ls_goodness_of_fit_ref   1.0609
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_constraints    88
_refine_ls_number_parameters     891
_refine_ls_number_reflns         21694
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.0609
_refine_ls_R_factor_all          0.0873
_refine_ls_R_factor_gt           0.0635
_refine_ls_shift/su_max          0.0007
_refine_ls_shift/su_mean         0.0000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0434P)^2^+314.9622P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1349
_refine_ls_wR_factor_ref         0.1541
_reflns_Friedel_coverage         0.0
_reflns_limit_h_max              14
_reflns_limit_h_min              -18
_reflns_limit_k_max              34
_reflns_limit_k_min              0
_reflns_limit_l_max              35
_reflns_limit_l_min              -13
_reflns_number_gt                15906
_reflns_number_total             21694
_reflns_threshold_expression     I>=2u(I)
_cod_data_source_file            d5dt00934k2.cif
_cod_data_source_block           GK_HY_4_Lt_Mo
_cod_depositor_comments
'Adding full bibliography for 7719124--7719126.cif.'
_cod_original_sg_symbol_Hall     '-P 2ybc (x-z,y,z)'
_cod_original_formula_sum        'C58 Cl4 H82 N14 O46 Si1 W12 '
_cod_database_code               7719126
_chemical_oxdiff_formula         'C184  H216  Cl16  N40  O172  Si4  W48  '
_reflns_odcompleteness_completeness 99.19
_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), N6(H6a,H6b)
2.b Aromatic/amide H refined with riding coordinates:
 C6(H6), C2(H2), C8(H8), C38(H38), C1(H1), C5(H5), C35(H35), C43(H43),
 C36(H36), C28(H28), C26(H26), C25(H25), C18(H18), C11(H11), C22(H22), C16(H16),
  C15(H15), C21(H21), C12(H12), C31(H31), C32(H32), C46(H46)
2.c X=CH2 refined with riding coordinates:
 N2(H2a,H2b), N8(H8a,H8b)
2.d Idealised Me refined as rotating group:
 C10(H10a,H10b,H10c), C40(H40a,H40b,H40c), C20(H20a,H20b,H20c), C45(H45a,H45b,
 H45c), C44(H44a,H44b,H44c), C30(H30a,H30b,H30c), C42(H42a,H42b,H42c), C41(H41a,
 H41b,H41c)
;
_smtbx_masks_special_details
;
A solvent mask was calculated and 640 electrons were 
found in a volume of 3118\%A^3^ in 2 voids per unit cell. 
This is consistent with the presence of 4[C3H7NO] per Formula Unit 
which account for 640 electrons per unit cell.
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_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 1.212
_oxdiff_exptl_absorpt_empirical_full_min 0.801