Nb(V), Ta(V), and V(IV) catalyst-driven development of temperature-responsive self-healing materials based on methyl methacrylate.
Drzeżdżon, Joanna; Białek, Marzena; Zappia, Stefania; Lopresti, Mattia; Palin, Luca; Jarzembska, Katarzyna N.; Kamiński, Radosław; Datta, Janusz; Dalton transactions (Cambridge, England : 2003) 54 (2025) 9901–9913; doi:10.1039/d5dt01073j

data_7718829
_publ_section_title
;
 Nb(V), Ta(V), and V(IV) catalyst-driven development of
 temperature-responsive self-healing materials based on methyl
 methacrylate.
;
_journal_issue                   25
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              9901
_journal_page_last               9913
_journal_paper_doi               10.1039/d5dt01073j
_journal_volume                  54
_journal_year                    2025
_chemical_compound_source        Synthesis
_chemical_formula_moiety         'C21 H23 N O5 V'
_chemical_formula_sum            'C21 H23 N O5 V'
_chemical_formula_weight         420.34
_chemical_name_common            '4-Phenylpyridine vanadyl-bis(acetylacetonate)'
_chemical_name_systematic        '4-Phenylpyridine vanadyl-bis(acetylacetonate)'
_space_group_crystal_system      monoclinic
_space_group_IT_number           15
_space_group_name_Hall           '-C 2yc'
_space_group_name_H-M_alt        'C 1 2/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2024-09-12
_audit_creation_method
;
Olex2 1.5
(compiled 2023.03.06 svn.rbb2c1857 for OlexSys, GUI svn.r6748)
;
_audit_update_record
;
2024-09-12 deposited with the CCDC.	2025-05-29 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.968(7)
_cell_angle_gamma                90
_cell_formula_units_Z            8
_cell_length_a                   24.2547(15)
_cell_length_b                   8.0765(5)
_cell_length_c                   21.6591(12)
_cell_measurement_reflns_used    2921
_cell_measurement_temperature    293(2)
_cell_measurement_theta_max      24.7580
_cell_measurement_theta_min      3.0410
_cell_volume                     4012.5(4)
_computing_cell_refinement       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.38.41 (Rigaku OD, 2015)'
_computing_molecular_graphics    'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 1.5 (Dolomanov et al., 2009)'
_computing_structure_refinement  'SHELXL 2018/3 (Sheldrick, 2015)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_pressure         101.325
_diffrn_ambient_temperature      293(2)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 8.6225
_diffrn_detector_type            Sapphire3
_diffrn_measured_fraction_theta_full 0.900
_diffrn_measured_fraction_theta_max 0.890
_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    -37.00  11.00   1.00    5.00    --   19.06 112.00 168.00   48
  2  \w     38.00 105.00   1.00    5.00    --   19.06 179.00 150.00   67
  3  \w    -52.00  61.00   1.00    5.00    --   19.06 -37.00 120.00  113
  4  \w    -60.00   1.00   1.00    5.00    --   19.06  15.00-165.00   61
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'Xcalibur, Sapphire3'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      0.0019794000
_diffrn_orient_matrix_UB_12      0.0458397000
_diffrn_orient_matrix_UB_13      0.0285716000
_diffrn_orient_matrix_UB_21      -0.0057212000
_diffrn_orient_matrix_UB_22      -0.0730183000
_diffrn_orient_matrix_UB_23      0.0150881000
_diffrn_orient_matrix_UB_31      0.0303223000
_diffrn_orient_matrix_UB_32      -0.0167453000
_diffrn_orient_matrix_UB_33      0.0124557000
_diffrn_radiation_monochromator  graphite
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           'Mo K\a'
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0305
_diffrn_reflns_av_unetI/netI     0.0409
_diffrn_reflns_Laue_measured_fraction_full 0.900
_diffrn_reflns_Laue_measured_fraction_max 0.890
_diffrn_reflns_limit_h_max       28
_diffrn_reflns_limit_h_min       -29
_diffrn_reflns_limit_k_max       7
_diffrn_reflns_limit_k_min       -9
_diffrn_reflns_limit_l_max       26
_diffrn_reflns_limit_l_min       -26
_diffrn_reflns_number            6979
_diffrn_reflns_point_group_measured_fraction_full 0.900
_diffrn_reflns_point_group_measured_fraction_max 0.890
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.332
_diffrn_reflns_theta_min         2.952
_diffrn_source                   'fine-focus sealed X-ray tube'
_diffrn_source_type              'Enhance (Mo) X-ray Source'
_exptl_absorpt_coefficient_mu    0.526
_exptl_absorpt_correction_T_max  1.00000
_exptl_absorpt_correction_T_min  0.91930
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.38.41 (Rigaku Oxford Diffraction, 2015)
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            Red
_exptl_crystal_density_diffrn    1.392
_exptl_crystal_description       Twins
_exptl_crystal_F_000             1752
_exptl_crystal_recrystallization_method Evaporation
_exptl_crystal_size_max          0.100
_exptl_crystal_size_mid          0.075
_exptl_crystal_size_min          0.050
_refine_diff_density_max         1.054
_refine_diff_density_min         -0.800
_refine_diff_density_rms         0.073
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.048
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     257
_refine_ls_number_reflns         3273
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.048
_refine_ls_R_factor_all          0.0901
_refine_ls_R_factor_gt           0.0708
_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^)+(0.0832P)^2^+16.2737P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1720
_refine_ls_wR_factor_ref         0.1873
_reflns_Friedel_coverage         0.000
_reflns_number_gt                2527
_reflns_number_total             3273
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d5dt01073j2.cif
_cod_data_source_block           exp_377
_cod_depositor_comments
'Adding full bibliography for 7718829--7718831.cif.'
_cod_original_sg_symbol_H-M      'C 2/c'
_cod_database_code               7718829
_shelx_shelxl_version_number     2019/3
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C00D(H00D), C00E(H00E), C00G(H00G), C00H(H00H), C00I(H00I), C00J(H00J),
 C00K(H00K), C00M(H00M), C00P(H00R), C00R(H00V), C00S(H00W)
2.b Idealised Me refined as rotating group:
 C00L(H00A,H00B,H00C), C00N(H00F,H00L,H00N), C00O(H00O,H00P,H00Q), C00Q(H00S,
 H00T,H00U)
;
_shelx_res_checksum              96486
_shelx_hkl_checksum              3816
_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 1.149
_oxdiff_exptl_absorpt_empirical_full_min 0.701