Breaking boundaries: novel tridecavanadate polyoxometalates with a unique six-fold tetradentate coordination capacity for lanthanum(iii) and a two-fold bidentate decavanadate ligand in a single compound
Somasundaram, Janaki Devi; Kabzan, Henrich; Gyepes, Róbert; Krivosudský, Lukáš; New Journal of Chemistry 49 (2025) 2096–2105; doi:10.1039/D4NJ03690E

data_7063584
_publ_section_title
;
 Breaking boundaries: novel tridecavanadate polyoxometalates with a unique
 six-fold tetradentate coordination capacity for lanthanum(iii) and a
 two-fold bidentate decavanadate ligand in a single compound
;
_journal_issue                   6
_journal_name_full               'New Journal of Chemistry'
_journal_page_first              2096
_journal_page_last               2105
_journal_paper_doi               10.1039/D4NJ03690E
_journal_volume                  49
_journal_year                    2025
_chemical_formula_moiety         'H28 La2 O42 V10, 8(O)'
_chemical_formula_sum            'H28 La2 O50 V10'
_chemical_formula_weight         1615.44
_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   difmap
_audit_creation_date             2024-02-02
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2024-03-20 deposited with the CCDC.	2024-12-12 downloaded from the CCDC.
;
_cell_angle_alpha                114.085(2)
_cell_angle_beta                 99.949(2)
_cell_angle_gamma                99.5610(19)
_cell_formula_units_Z            1
_cell_length_a                   10.4779(2)
_cell_length_b                   11.2361(2)
_cell_length_c                   11.6788(3)
_cell_measurement_reflns_used    20155
_cell_measurement_temperature    160.00(10)
_cell_measurement_theta_max      32.6140
_cell_measurement_theta_min      5.6590
_cell_volume                     1192.81(5)
_computing_cell_refinement       'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_data_collection
'CrysAlisPro system (CCD 41.123a 64-bit (release 20-01-2022))'
_computing_data_reduction        'CrysAlisPro 1.171.43.105a (Rigaku OD, 2024)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2019/3 (Sheldrick, 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      160.00(10)
_diffrn_detector                 'Hybrid Pixel Array Detector'
_diffrn_detector_area_resol_mean 5.8140
_diffrn_detector_type            'Pilatus 200K'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_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    -11.00  90.00   0.50    4.00    --   14.46  57.00 -60.00  202
  2  \w    -61.00  40.00   0.50    4.00    --   14.46 -57.00   0.00  202
  3  \w    -91.00  10.00   0.50    4.00    --  -15.40 -57.00 120.00  202
  4  \w    -40.00  66.00   0.50    4.00    --  -15.40  38.00 -90.00  212
  5  \w    -90.00  10.00   0.50    4.00    --  -15.40 -60.00 -23.15  200
  6  \w    -91.00  10.00   0.50    4.00    --  -15.40 -57.00-120.00  202
  7  \w    -90.00  10.00   0.50    4.00    --  -15.40 -59.00 176.48  200
  8  \w    -90.00  10.00   0.50    4.00    --  -15.40 -60.00  75.91  200
  9  \w    -61.00  -7.00   0.50    4.00    --   14.46 -57.00 -90.00  108
 10  \w    -40.00  60.00   0.50    4.00    --  -15.40  57.00  90.00  200
 11  \w    -40.00  60.00   0.50    4.00    --  -15.40  57.00 150.00  200
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, Pilatus 200K'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0645719000
_diffrn_orient_matrix_UB_12      -0.0039439000
_diffrn_orient_matrix_UB_13      -0.0344623000
_diffrn_orient_matrix_UB_21      0.0281988000
_diffrn_orient_matrix_UB_22      0.0123728000
_diffrn_orient_matrix_UB_23      -0.0463777000
_diffrn_orient_matrix_UB_31      -0.0104968000
_diffrn_orient_matrix_UB_32      -0.0704858000
_diffrn_orient_matrix_UB_33      -0.0377806000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_unetI/netI     0.0219
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -15
_diffrn_reflns_limit_l_max       16
_diffrn_reflns_limit_l_min       -16
_diffrn_reflns_number            15508
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         29.846
_diffrn_reflns_theta_min         2.439
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    3.726
_exptl_absorpt_correction_T_max  0.871
_exptl_absorpt_correction_T_min  0.662
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.43.105a (Rigaku Oxford Diffraction, 2024)
Analytical numeric absorption correction using a multifaceted crystal
model based on expressions derived by R.C. Clark & J.S. Reid.
(Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897)
Empirical absorption correction using spherical harmonics,
implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            orange
_exptl_crystal_colour_primary    orange
_exptl_crystal_density_diffrn    2.249
_exptl_crystal_description       prism
_exptl_crystal_F_000             772
_exptl_crystal_size_max          0.174
_exptl_crystal_size_mid          0.093
_exptl_crystal_size_min          0.044
_refine_diff_density_max         3.222
_refine_diff_density_min         -1.559
_refine_diff_density_rms         0.209
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.029
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     290
_refine_ls_number_reflns         15508
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.029
_refine_ls_R_factor_all          0.0530
_refine_ls_R_factor_gt           0.0462
_refine_ls_shift/su_max          0.001
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.0686P)^2^+6.8098P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1232
_refine_ls_wR_factor_ref         0.1302
_reflns_Friedel_coverage         0.000
_reflns_number_gt                13789
_reflns_number_total             15508
_reflns_threshold_expression     'I > 2\s(I)'
_twin_special_details
;
Component 2 rotated by 1.7539\% 
around [-0.11 0.88 -0.47] (reciprocal) or [0.00 0.99 -0.13] (direct)
;
_cod_data_source_file            d4nj03690e3.cif
_cod_data_source_block           twin
_cod_depositor_comments
'Adding full bibliography for 7063583--7063585.cif.'
_cod_original_cell_volume        1192.82(5)
_cod_database_code               7063584
_shelx_shelxl_version_number     2019/3
_chemical_oxdiff_formula         'La2 H62 O54 V10'
_shelx_estimated_absorpt_t_max   0.853
_shelx_estimated_absorpt_t_min   0.563
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.6294(11)
 0.3706(11)
2. Fixed Uiso
 At 1.5 times of:
  All O(H,H) groups
3.a Free rotating group:
 O4W(H4WA,H4WB)
3.b Rotating group:
 O7W(H7WA,H7WB), O6W(H6WA,H6WB), O1W(H1WA,H1WB), O5W(H5WA,H5WB), O3W(H3WA,
 H3WB), O2W(H2WA,H2WB)
;
_smtbx_masks_void_probe_radius   1.2
_smtbx_masks_void_truncation_radius 1.2
_shelx_res_checksum              27840
_shelx_fab_checksum              80555
_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 1.535
_oxdiff_exptl_absorpt_empirical_full_min 0.540
_oxdiff_twin_integration_method  simultaneous
_oxdiff_twin_items               2