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#$Date: 2026-03-13 00:57:40 +0100 (Fri 13 de Mar de 2026) $
#$Revision: 305066 $
#$URL: svn://www.crystallography.net/cod/cif/7/72/06/7720682.cif $
#------------------------------------------------------------------------------
#
# This file is available in the Crystallography Open Database (COD),
# http://www.crystallography.net/
#
# All data on this site have been placed in the public domain by the
# contributors.
#
data_7720682
loop_
_publ_author_name
'Shibata, Kaname'
'Michiue, Kenji'
'Motuzis, Ignas'
'Elsegood, Mark Robert James'
'Redshaw, Carl'
_publ_section_title
;
 Vanadyl complexes supported by O,O-and N,O-chelate ligation: Structures
 and polymerization catalysis
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D6DT00387G
_journal_year                    2026
_chemical_formula_moiety         'C38 H40 Br4 N2 O3 V'
_chemical_formula_sum            'C38 H40 Br4 N2 O3 V'
_chemical_formula_weight         943.30
_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_method           SHELXL-2018/3
_audit_update_record
;
2026-01-19 deposited with the CCDC.	2026-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                68.3876(12)
_cell_angle_beta                 79.1420(9)
_cell_angle_gamma                81.4636(10)
_cell_formula_units_Z            1
_cell_length_a                   9.34746(10)
_cell_length_b                   9.37245(14)
_cell_length_c                   12.34112(13)
_cell_measurement_reflns_used    30524
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      76.33
_cell_measurement_theta_min      3.89
_cell_volume                     983.47(2)
_computing_cell_refinement       'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_computing_data_collection       'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_computing_data_reduction        'CrysAlisPro 1.171.42.74a (Rigaku OD, 2022)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2018)'
_computing_structure_solution    'SHELXT-2018/2 (Sheldrick, 2015)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 0.995
_diffrn_measured_fraction_theta_max 0.993
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
; 
Rigaku 007HF diffractometer with HF Varimax confocal mirrors, 
an UG2 goniometer and HyPix 6000HE detector 
;
_diffrn_measurement_method       'profile data from ω-scans'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0411
_diffrn_reflns_av_unetI/netI     0.0153
_diffrn_reflns_Laue_measured_fraction_full 0.995
_diffrn_reflns_Laue_measured_fraction_max 0.993
_diffrn_reflns_limit_h_max       11
_diffrn_reflns_limit_h_min       -11
_diffrn_reflns_limit_k_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            34358
_diffrn_reflns_point_group_measured_fraction_full 0.995
_diffrn_reflns_point_group_measured_fraction_max 0.993
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         70.060
_diffrn_reflns_theta_min         3.894
_diffrn_source                   'Rotating anode'
_exptl_absorpt_coefficient_mu    7.158
_exptl_absorpt_correction_T_max  1.000
_exptl_absorpt_correction_T_min  0.367
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.42.74a (Rigaku Oxford Diffraction, 2022) 
Empirical absorption correction using spherical harmonics, 
implemented in SCALE3 ABSPACK scaling algorithm. 
;
_exptl_crystal_colour            'dark green'
_exptl_crystal_density_diffrn    1.593
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       plate
_exptl_crystal_F_000             469
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.240
_exptl_crystal_size_mid          0.160
_exptl_crystal_size_min          0.025
_refine_diff_density_max         0.914
_refine_diff_density_min         -1.046
_refine_diff_density_rms         0.074
_refine_ls_extinction_coef       0.00268(19)
_refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc²λ³/sin(2θ)]^-1/4^
_refine_ls_extinction_method     'SHELXL-2018/3 (Sheldrick 2018)'
_refine_ls_goodness_of_fit_ref   1.125
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     231
_refine_ls_number_reflns         3714
_refine_ls_number_restraints     84
_refine_ls_restrained_S_all      1.120
_refine_ls_R_factor_all          0.0322
_refine_ls_R_factor_gt           0.0321
_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/[σ²(Fo²)+(0.0109P)²+2.6018P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0697
_refine_ls_wR_factor_ref         0.0698
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3699
_reflns_number_total             3714
_reflns_threshold_expression     'I > 2σ(I)'
_cod_data_source_file            d6dt00387g2.cif
_cod_data_source_block           5
_cod_database_code               7720682
_shelx_shelxl_version_number     2018/3
_shelx_space_group_comment
; 
The symmetry employed for this shelxl refinement is uniquely defined 
by the following loop, which should always be used as a source of 
symmetry information in preference to the above space-group names. 
They are only intended as comments. 
;
_shelx_estimated_absorpt_t_min   0.278
_shelx_estimated_absorpt_t_max   0.841
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x, -y, -z'
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.46115(10) 0.45940(10) 0.49838(8) 0.01475(19) Uani 0.5 1 d . . P . .
O1 O 0.5417(2) 0.3660(2) 0.64261(16) 0.0219(4) Uani 1 1 d . . . . .
O2 O 0.3480(4) 0.3499(5) 0.4974(4) 0.0243(9) Uani 0.5 1 d . . P . .
C1 C 0.6403(3) 0.2496(3) 0.6762(2) 0.0173(5) Uani 1 1 d . . . . .
C2 C 0.6470(3) 0.1675(3) 0.7974(2) 0.0203(6) Uani 1 1 d . . . . .
Br1 Br 0.50999(4) 0.22995(4) 0.90810(3) 0.03078(12) Uani 1 1 d . . . . .
C3 C 0.7490(3) 0.0445(3) 0.8369(2) 0.0211(6) Uani 1 1 d . . . . .
H3 H 0.750039 -0.008250 0.918881 0.025 Uiso 1 1 calc R U . . .
C4 C 0.8501(3) -0.0008(3) 0.7550(2) 0.0213(6) Uani 1 1 d . . . . .
Br2 Br 0.99268(3) -0.16803(4) 0.80692(3) 0.02846(12) Uani 1 1 d . . . . .
C5 C 0.8485(3) 0.0744(3) 0.6365(2) 0.0218(6) Uani 1 1 d . . . . .
H5 H 0.918129 0.042284 0.581360 0.026 Uiso 1 1 calc R U . . .
C6 C 0.7440(3) 0.1991(3) 0.5963(2) 0.0185(5) Uani 1 1 d . . . . .
C7 C 0.7489(3) 0.2719(3) 0.4705(2) 0.0195(6) Uani 1 1 d . . . . .
H7 H 0.821996 0.229756 0.423245 0.023 Uiso 1 1 calc R U . . .
N1 N 0.6660(3) 0.3864(3) 0.4156(2) 0.0251(5) Uani 1 1 d . . . . .
C8 C 0.6981(3) 0.4306(3) 0.2882(2) 0.0188(6) Uani 1 1 d . . . . .
C9 C 0.6311(3) 0.3606(3) 0.2317(3) 0.0268(6) Uani 1 1 d . U . . .
C10 C 0.6755(4) 0.3978(4) 0.1099(3) 0.0408(9) Uani 1 1 d . . . . .
H10 H 0.632128 0.352532 0.068055 0.049 Uiso 1 1 calc R U . . .
C11 C 0.7809(4) 0.4989(4) 0.0500(3) 0.0397(9) Uani 1 1 d . . . . .
H11 H 0.810655 0.521217 -0.032042 0.048 Uiso 1 1 calc R U . . .
C12 C 0.8420(4) 0.5666(4) 0.1081(3) 0.0352(8) Uani 1 1 d . . . . .
H12 H 0.913751 0.636846 0.065512 0.042 Uiso 1 1 calc R U . . .
C13 C 0.8024(3) 0.5356(3) 0.2281(3) 0.0239(6) Uani 1 1 d . U . . .
C14 C 0.5158(4) 0.2495(4) 0.2968(5) 0.0555(12) Uani 1 1 d . U . . .
H14 H 0.493591 0.246050 0.380200 0.067 Uiso 1 1 calc R U . . .
C15 C 0.5707(6) 0.0857(5) 0.2976(8) 0.110(3) Uani 1 1 d . U . . .
H15A H 0.590550 0.086363 0.216509 0.166 Uiso 1 1 calc R U . . .
H15B H 0.495736 0.015039 0.343209 0.166 Uiso 1 1 calc R U . . .
H15C H 0.660579 0.051481 0.333396 0.166 Uiso 1 1 calc R U . . .
C16 C 0.3751(4) 0.3046(5) 0.2413(5) 0.0647(14) Uani 1 1 d . U . . .
H16A H 0.343459 0.410256 0.238348 0.097 Uiso 1 1 calc R U . . .
H16B H 0.298569 0.236953 0.288681 0.097 Uiso 1 1 calc R U . . .
H16C H 0.393355 0.301886 0.161168 0.097 Uiso 1 1 calc R U . . .
C17 C 0.8719(4) 0.6159(4) 0.2888(4) 0.0453(9) Uani 1 1 d . U . . .
H17 H 0.821194 0.586879 0.371895 0.054 Uiso 1 1 calc R U . . .
C18 C 1.0336(6) 0.5595(6) 0.2942(7) 0.092(2) Uani 1 1 d . U . . .
H18A H 1.042955 0.447918 0.336030 0.137 Uiso 1 1 calc R U . . .
H18B H 1.074575 0.611110 0.336038 0.137 Uiso 1 1 calc R U . . .
H18C H 1.086697 0.583470 0.214040 0.137 Uiso 1 1 calc R U . . .
C19 C 0.8508(6) 0.7895(5) 0.2340(6) 0.0742(16) Uani 1 1 d . U . . .
H19A H 0.903444 0.822896 0.153479 0.111 Uiso 1 1 calc R U . . .
H19B H 0.888820 0.836165 0.280801 0.111 Uiso 1 1 calc R U . . .
H19C H 0.746372 0.821957 0.232278 0.111 Uiso 1 1 calc R U . . .
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Br Br -0.6763 1.2805 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
V1 V1 O2 177.45(18) 2_666 . ?
V1 V1 O1 73.20(11) 2_666 2_666 ?
O2 V1 O1 107.11(17) . 2_666 ?
V1 V1 O1 71.94(10) 2_666 . ?
O2 V1 O1 107.72(17) . . ?
O1 V1 O1 145.14(6) 2_666 . ?
V1 V1 N1 76.98(11) 2_666 . ?
O2 V1 N1 105.55(16) . . ?
O1 V1 N1 86.11(9) 2_666 . ?
O1 V1 N1 86.15(9) . . ?
V1 V1 N1 72.38(11) 2_666 2_666 ?
O2 V1 N1 105.10(16) . 2_666 ?
O1 V1 N1 85.13(9) 2_666 2_666 ?
O1 V1 N1 84.46(9) . 2_666 ?
N1 V1 N1 149.35(6) . 2_666 ?
C1 O1 V1 131.65(18) . 2_666 ?
C1 O1 V1 131.47(17) . . ?
O1 C1 C6 123.0(2) . . ?
O1 C1 C2 120.6(2) . . ?
C6 C1 C2 116.4(2) . . ?
C3 C2 C1 122.7(2) . . ?
C3 C2 Br1 119.3(2) . . ?
C1 C2 Br1 118.0(2) . . ?
C2 C3 C4 119.1(2) . . ?
C2 C3 H3 120.4 . . ?
C4 C3 H3 120.4 . . ?
C5 C4 C3 120.7(2) . . ?
C5 C4 Br2 119.4(2) . . ?
C3 C4 Br2 120.0(2) . . ?
C4 C5 C6 120.2(3) . . ?
C4 C5 H5 119.9 . . ?
C6 C5 H5 119.9 . . ?
C5 C6 C1 121.0(2) . . ?
C5 C6 C7 116.9(2) . . ?
C1 C6 C7 122.1(2) . . ?
N1 C7 C6 127.3(2) . . ?
N1 C7 H7 116.4 . . ?
C6 C7 H7 116.4 . . ?
C7 N1 C8 113.6(2) . . ?
C7 N1 V1 122.65(19) . . ?
C8 N1 V1 121.02(17) . . ?
C7 N1 V1 121.44(19) . 2_666 ?
C8 N1 V1 122.37(17) . 2_666 ?
C9 C8 C13 122.4(3) . . ?
C9 C8 N1 119.3(3) . . ?
C13 C8 N1 118.1(3) . . ?
C8 C9 C10 116.9(3) . . ?
C8 C9 C14 122.2(3) . . ?
C10 C9 C14 120.9(3) . . ?
C11 C10 C9 121.2(3) . . ?
C11 C10 H10 119.4 . . ?
C9 C10 H10 119.4 . . ?
C12 C11 C10 120.2(3) . . ?
C12 C11 H11 119.9 . . ?
C10 C11 H11 119.9 . . ?
C11 C12 C13 121.5(3) . . ?
C11 C12 H12 119.2 . . ?
C13 C12 H12 119.2 . . ?
C12 C13 C8 117.8(3) . . ?
C12 C13 C17 119.7(3) . . ?
C8 C13 C17 122.5(3) . . ?
C9 C14 C16 110.4(3) . . ?
C9 C14 C15 111.1(4) . . ?
C16 C14 C15 110.2(4) . . ?
C9 C14 H14 108.4 . . ?
C16 C14 H14 108.4 . . ?
C15 C14 H14 108.4 . . ?
C14 C15 H15A 109.5 . . ?
C14 C15 H15B 109.5 . . ?
H15A C15 H15B 109.5 . . ?
C14 C15 H15C 109.5 . . ?
H15A C15 H15C 109.5 . . ?
H15B C15 H15C 109.5 . . ?
C14 C16 H16A 109.5 . . ?
C14 C16 H16B 109.5 . . ?
H16A C16 H16B 109.5 . . ?
C14 C16 H16C 109.5 . . ?
H16A C16 H16C 109.5 . . ?
H16B C16 H16C 109.5 . . ?
C19 C17 C13 112.5(3) . . ?
C19 C17 C18 111.4(4) . . ?
C13 C17 C18 111.4(3) . . ?
C19 C17 H17 107.1 . . ?
C13 C17 H17 107.1 . . ?
C18 C17 H17 107.1 . . ?
C17 C18 H18A 109.5 . . ?
C17 C18 H18B 109.5 . . ?
H18A C18 H18B 109.5 . . ?
C17 C18 H18C 109.5 . . ?
H18A C18 H18C 109.5 . . ?
H18B C18 H18C 109.5 . . ?
C17 C19 H19A 109.5 . . ?
C17 C19 H19B 109.5 . . ?
H19A C19 H19B 109.5 . . ?
C17 C19 H19C 109.5 . . ?
H19A C19 H19C 109.5 . . ?
H19B C19 H19C 109.5 . . ?
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 V1 1.1427(19) 2_666 ?
V1 O2 1.583(4) . ?
V1 O1 1.901(2) 2_666 ?
V1 O1 1.914(2) . ?
V1 N1 2.137(2) . ?
V1 N1 2.184(2) 2_666 ?
O1 C1 1.313(3) . ?
C1 C6 1.408(4) . ?
C1 C2 1.416(4) . ?
C2 C3 1.382(4) . ?
C2 Br1 1.886(3) . ?
C3 C4 1.390(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.372(4) . ?
C4 Br2 1.898(3) . ?
C5 C6 1.408(4) . ?
C5 H5 0.9500 . ?
C6 C7 1.442(4) . ?
C7 N1 1.276(4) . ?
C7 H7 0.9500 . ?
N1 C8 1.454(3) . ?
C8 C9 1.389(4) . ?
C8 C13 1.394(4) . ?
C9 C10 1.406(5) . ?
C9 C14 1.511(5) . ?
C10 C11 1.379(6) . ?
C10 H10 0.9500 . ?
C11 C12 1.356(6) . ?
C11 H11 0.9500 . ?
C12 C13 1.387(4) . ?
C12 H12 0.9500 . ?
C13 C17 1.515(5) . ?
C14 C16 1.531(5) . ?
C14 C15 1.542(7) . ?
C14 H14 1.0000 . ?
C15 H15A 0.9800 . ?
C15 H15B 0.9800 . ?
C15 H15C 0.9800 . ?
C16 H16A 0.9800 . ?
C16 H16B 0.9800 . ?
C16 H16C 0.9800 . ?
C17 C19 1.513(6) . ?
C17 C18 1.530(6) . ?
C17 H17 1.0000 . ?
C18 H18A 0.9800 . ?
C18 H18B 0.9800 . ?
C18 H18C 0.9800 . ?
C19 H19A 0.9800 . ?
C19 H19B 0.9800 . ?
C19 H19C 0.9800 . ?
loop_
_geom_torsion_atom_site_label_1
_geom_torsion_atom_site_label_2
_geom_torsion_atom_site_label_3
_geom_torsion_atom_site_label_4
_geom_torsion
_geom_torsion_site_symmetry_1
_geom_torsion_site_symmetry_2
_geom_torsion_site_symmetry_3
_geom_torsion_site_symmetry_4
_geom_torsion_publ_flag
V1 O1 C1 C6 -25.1(4) 2_666 . . . ?
V1 O1 C1 C6 22.1(4) . . . . ?
V1 O1 C1 C2 154.9(2) 2_666 . . . ?
V1 O1 C1 C2 -158.0(2) . . . . ?
O1 C1 C2 C3 -179.8(3) . . . . ?
C6 C1 C2 C3 0.2(4) . . . . ?
O1 C1 C2 Br1 0.3(4) . . . . ?
C6 C1 C2 Br1 -179.8(2) . . . . ?
C1 C2 C3 C4 0.3(4) . . . . ?
Br1 C2 C3 C4 -179.8(2) . . . . ?
C2 C3 C4 C5 -0.4(4) . . . . ?
C2 C3 C4 Br2 179.4(2) . . . . ?
C3 C4 C5 C6 0.1(4) . . . . ?
Br2 C4 C5 C6 -179.7(2) . . . . ?
C4 C5 C6 C1 0.4(4) . . . . ?
C4 C5 C6 C7 -179.7(3) . . . . ?
O1 C1 C6 C5 179.5(3) . . . . ?
C2 C1 C6 C5 -0.5(4) . . . . ?
O1 C1 C6 C7 -0.4(4) . . . . ?
C2 C1 C6 C7 179.6(3) . . . . ?
C5 C6 C7 N1 -179.4(3) . . . . ?
C1 C6 C7 N1 0.5(5) . . . . ?
C6 C7 N1 C8 -179.1(3) . . . . ?
C6 C7 N1 V1 -17.6(4) . . . . ?
C6 C7 N1 V1 18.7(4) . . . 2_666 ?
C7 N1 C8 C9 88.0(3) . . . . ?
V1 N1 C8 C9 -73.8(3) . . . . ?
V1 N1 C8 C9 -110.0(3) 2_666 . . . ?
C7 N1 C8 C13 -88.2(3) . . . . ?
V1 N1 C8 C13 110.0(3) . . . . ?
V1 N1 C8 C13 73.8(3) 2_666 . . . ?
C13 C8 C9 C10 1.3(4) . . . . ?
N1 C8 C9 C10 -174.7(2) . . . . ?
C13 C8 C9 C14 -178.7(3) . . . . ?
N1 C8 C9 C14 5.3(4) . . . . ?
C8 C9 C10 C11 0.2(4) . . . . ?
C14 C9 C10 C11 -179.9(3) . . . . ?
C9 C10 C11 C12 -1.1(5) . . . . ?
C10 C11 C12 C13 0.7(5) . . . . ?
C11 C12 C13 C8 0.7(4) . . . . ?
C11 C12 C13 C17 -179.0(3) . . . . ?
C9 C8 C13 C12 -1.7(4) . . . . ?
N1 C8 C13 C12 174.3(2) . . . . ?
C9 C8 C13 C17 178.0(3) . . . . ?
N1 C8 C13 C17 -6.0(4) . . . . ?
C8 C9 C14 C16 123.6(4) . . . . ?
C10 C9 C14 C16 -56.4(5) . . . . ?
C8 C9 C14 C15 -113.9(5) . . . . ?
C10 C9 C14 C15 66.1(5) . . . . ?
C12 C13 C17 C19 56.6(5) . . . . ?
C8 C13 C17 C19 -123.1(4) . . . . ?
C12 C13 C17 C18 -69.3(5) . . . . ?
C8 C13 C17 C18 111.0(5) . . . . ?
