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_7719125
_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         'Mo12 O40 Si, 4(C10 H10 Cl N2), C3 H7 N O'
_chemical_formula_sum            'C43 H47 Cl4 Mo12 N9 O41 Si'
_chemical_formula_weight         2667.06
_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'
_atom_sites_solution_hydrogens   mixed
_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                 100.435(5)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.9068(5)
_cell_length_b                   27.6783(16)
_cell_length_c                   27.601(2)
_cell_measurement_reflns_used    6019
_cell_measurement_temperature    150.00(10)
_cell_measurement_theta_max      27.3260
_cell_measurement_theta_min      2.0990
_cell_volume                     10448.4(11)
_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  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'olex2.solve 1.3 (Bourhis et al., 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      150.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 15.9974
_diffrn_detector_type            Eos
_diffrn_measured_fraction_theta_full 0.761
_diffrn_measured_fraction_theta_max 0.676
_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  82.00   1.00   24.00    --   26.84 178.00   0.00   47
  2  \w     -4.00  95.00   1.00   24.00    --   26.84  57.00-180.00   99
  3  \w     35.00 113.00   1.00   24.00    --   26.84 178.00  90.00   78
;
_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      0.0003781000
_diffrn_orient_matrix_UB_12      0.0040212000
_diffrn_orient_matrix_UB_13      0.0254426000
_diffrn_orient_matrix_UB_21      0.0169858000
_diffrn_orient_matrix_UB_22      -0.0238673000
_diffrn_orient_matrix_UB_23      0.0049086000
_diffrn_orient_matrix_UB_31      0.0490349000
_diffrn_orient_matrix_UB_32      0.0084405000
_diffrn_orient_matrix_UB_33      0.0028665000
_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  0.2113
_diffrn_reflns_av_unetI/netI     0.3007
_diffrn_reflns_Laue_measured_fraction_full 0.761
_diffrn_reflns_Laue_measured_fraction_max 0.676
_diffrn_reflns_limit_h_max       17
_diffrn_reflns_limit_h_min       -18
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -18
_diffrn_reflns_limit_l_max       34
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            26079
_diffrn_reflns_point_group_measured_fraction_full 0.761
_diffrn_reflns_point_group_measured_fraction_max 0.676
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.159
_diffrn_reflns_theta_min         2.414
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'SuperNova (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    1.572
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.584
_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    1.696
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       monoclinic
_exptl_crystal_F_000             5128
_exptl_crystal_size_max          0.228
_exptl_crystal_size_mid          0.136
_exptl_crystal_size_min          0.118
_refine_diff_density_max         3.115
_refine_diff_density_min         -1.341
_refine_diff_density_rms         0.189
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.956
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     994
_refine_ls_number_reflns         17321
_refine_ls_number_restraints     2
_refine_ls_restrained_S_all      0.957
_refine_ls_R_factor_all          0.1972
_refine_ls_R_factor_gt           0.0958
_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^)+(0.0448P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1904
_refine_ls_wR_factor_ref         0.2500
_reflns_Friedel_coverage         0.000
_reflns_number_gt                7307
_reflns_number_total             17321
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt00934k2.cif
_cod_data_source_block           gkhy_3_lt_mo
_cod_depositor_comments
'Adding full bibliography for 7719124--7719126.cif.'
_cod_original_cell_volume        10448.2(11)
_cod_database_code               7719125
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         'C172  H196  Cl16  Mo48  N36  O172  Si4  '
_reflns_odcompleteness_completeness 97.92
_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. Restrained distances
 C7-C8
 1.4 with sigma of 0.02
 C24-C25
 1.4 with sigma of 0.02
3.a Rotating group:
 N2(H2A,H2B), N4(H4A,H4B)
3.b Aromatic/amide H refined with riding coordinates:
 C16(H16), C38(H38), C36(H36), C31(H31), C12(H12), C32(H32), C28(H28),
 C15(H15), C18(H18), C11(H11), C35(H35), C6(H6), C26(H26), C5(H5), C2(H2),
 C8(H8), C25(H25), C21(H21), C22(H22), C1(H1), C41(H41)
3.c X=CH2 refined with riding coordinates:
 N8(H8A,H8B), N6(H6A,H6B)
3.d Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C), C20(H20A,H20B,H20C), C40(H40A,H40B,H40C), C43(H43A,H43B,
 H43C), C10(H10A,H10B,H10C), C30(H30A,H30B,H30C)
;
_shelx_res_checksum              94713
_shelx_hkl_checksum              49379
_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 2.778
_oxdiff_exptl_absorpt_empirical_full_min 0.558