Molecular engineering of polyoxometalate–porphyrin ion-pair hybrids: crystallographic insight and visible-light driven photocatalytic oxidative coupling of amines
Bandaru, Rohith Phaneendra; Gaonkar, Asmita Dileep; Vankayala, Kiran; Tripuramallu, Bharat Kumar; Catalysis Science & Technology  (2026) –; doi:10.1039/D6CY00008H

data_1576645
_publ_section_title
;
 Molecular engineering of polyoxometalate--porphyrin ion-pair hybrids:
 crystallographic insight and visible-light driven photocatalytic
 oxidative coupling of amines
;
_journal_issue                   7
_journal_name_full               'Catalysis Science &amp; Technology'
_journal_page_first              2276
_journal_page_last               2281
_journal_paper_doi               10.1039/D6CY00008H
_journal_volume                  16
_journal_year                    2026
_chemical_formula_moiety         '2(Mo6 O19), C44 H38 N8, 4(C3 H7 N O)'
_chemical_formula_sum            'C56 H66 Mo12 N12 O42'
_chemical_formula_weight         2730.48
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2025-07-23
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2025-10-30 deposited with the CCDC.	2026-02-11 downloaded from the CCDC.
;
_cell_angle_alpha                83.4680(10)
_cell_angle_beta                 72.0640(10)
_cell_angle_gamma                69.9960(10)
_cell_formula_units_Z            1
_cell_length_a                   11.4946(3)
_cell_length_b                   11.7114(3)
_cell_length_c                   17.2449(4)
_cell_measurement_reflns_used    9861
_cell_measurement_temperature    296.15
_cell_measurement_theta_max      28.36
_cell_measurement_theta_min      2.86
_cell_volume                     2075.31(9)
_computing_cell_refinement       'SAINT v8.34A (Bruker, 2013)'
_computing_data_reduction        'SAINT v8.34A (Bruker, 2013)'
_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)'
_computing_structure_solution    'olex2.solve 1.5 (Bourhis et al., 2015)'
_diffrn_ambient_temperature      296.15
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.994
_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  0.0191
_diffrn_reflns_av_unetI/netI     0.0191
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.994
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       23
_diffrn_reflns_limit_l_min       -23
_diffrn_reflns_number            38481
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.994
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         28.365
_diffrn_reflns_theta_min         1.851
_diffrn_source_current           0.6
_diffrn_source_power             0.03
_diffrn_source_voltage           50.0
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    1.845
_exptl_absorpt_correction_T_max  0.7457
_exptl_absorpt_correction_T_min  0.6923
_exptl_absorpt_correction_type   empirical
_exptl_absorpt_process_details
;
SADABS-2014/5 (Bruker,2014/5) was used for absorption correction.
wR2(int) was 0.0659 before and 0.0329 after correction.
The Ratio of minimum to maximum transmission is 0.9284.
The \l/2 correction factor is 0.00150.
;
_exptl_crystal_density_diffrn    2.185
_exptl_crystal_description       block
_exptl_crystal_F_000             1326
_exptl_crystal_size_max          0.28
_exptl_crystal_size_mid          0.24
_exptl_crystal_size_min          0.15
_refine_diff_density_max         2.641
_refine_diff_density_min         -1.002
_refine_diff_density_rms         0.107
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.030
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     554
_refine_ls_number_reflns         10351
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.030
_refine_ls_R_factor_all          0.0300
_refine_ls_R_factor_gt           0.0269
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+6.4996P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0636
_refine_ls_wR_factor_ref         0.0653
_reflns_Friedel_coverage         0.000
_reflns_number_gt                9481
_reflns_number_total             10351
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6cy00008h2.cif
_cod_data_source_block           mo_bkt13_0m_a
_cod_depositor_comments          'Adding full bibliography for 1576645.cif.'
_cod_database_code               1576645
_shelxl_version_number           2014-3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 N3(H3), C6(H6), C14(H14), C13(H13), C5(H5), C2(H2), C3(H3A), C10(H10), C9(H9),
  C18(H18), C21(H21), C20(H20), C19(H19), C01I(H01I), C01S(H01S)
2.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C01L(H01A,H01B,H01C), C22(H22A,H22B,H22C), C01N(H01D,H01E,
 H01F), C01O(H01G,H01H,H01J), C01Q(H01K,H01L,H01M)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              90153
_shelx_fab_checksum              68803
_olex2_submission_special_instructions 'No special instructions were received'