Vanadyl complexes supported by O,O-and N,O-chelate ligation: Structures and polymerization catalysis
Shibata, Kaname; Michiue, Kenji; Motuzis, Ignas; Elsegood, Mark Robert James; Redshaw, Carl; Dalton Transactions  (2026) –; doi:10.1039/D6DT00387G

data_7720685
_publ_section_title
;
 Vanadyl complexes supported by O,O- and N,O-chelate ligation: structures
 and polymerization catalysis.
;
_journal_issue                   14
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              5644
_journal_page_last               5666
_journal_paper_doi               10.1039/d6dt00387g
_journal_volume                  55
_journal_year                    2026
_chemical_absolute_configuration ad
_chemical_formula_moiety         'C26 H26 Br4 N O2 1-, C6 H16 N 1+'
_chemical_formula_sum            'C32 H42 Br4 N2 O2'
_chemical_formula_weight         806.31
_space_group_crystal_system      monoclinic
_space_group_IT_number           4
_space_group_name_Hall           'P 2yb'
_space_group_name_H-M_alt        'P 1 21 1'
_atom_sites_solution_hydrogens   mixed
_atom_sites_solution_primary     iterative
_audit_creation_method           SHELXL-2019/3
_audit_update_record
;
2026-01-19 deposited with the CCDC.	2026-03-10 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 114.9069(12)
_cell_angle_gamma                90
_cell_formula_units_Z            2
_cell_length_a                   11.05269(11)
_cell_length_b                   14.86773(11)
_cell_length_c                   11.54433(11)
_cell_measurement_reflns_used    24109
_cell_measurement_temperature    100(2)
_cell_measurement_theta_max      73.00
_cell_measurement_theta_min      4.21
_cell_volume                     1720.62(3)
_computing_cell_refinement       'CrysAlisPro 1.171.43.98a (Rigaku OD, 2023)'
_computing_data_collection
'CrysAlisPro system (CCD 43.101a 64-bit (release 13-12-2023))'
_computing_data_reduction        'CrysAlisPro 1.171.43.98a (Rigaku OD, 2023)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_computing_structure_refinement  'SHELXL-2019/3 (Sheldrick, 2019)'
_computing_structure_solution    'SHELXT 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      100(2)
_diffrn_detector_area_resol_mean 10
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.949
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type
; 
Rigaku 007HF diffractometer with HF Varimax confocal mirrors, 
an UG2 goniometer and HyPix Arc-100 detector 
;
_diffrn_measurement_method       'profile data from \w-scans'
_diffrn_radiation_collimation    0.3
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54178
_diffrn_reflns_av_R_equivalents  0.0321
_diffrn_reflns_av_unetI/netI     0.0273
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.949
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       18
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       14
_diffrn_reflns_limit_l_min       -14
_diffrn_reflns_number            27863
_diffrn_reflns_point_group_measured_fraction_full 0.907
_diffrn_reflns_point_group_measured_fraction_max 0.850
_diffrn_reflns_theta_full        67.679
_diffrn_reflns_theta_max         73.713
_diffrn_reflns_theta_min         4.222
_diffrn_source                   'Rotating anode'
_exptl_absorpt_coefficient_mu    5.935
_exptl_absorpt_correction_T_max  0.854
_exptl_absorpt_correction_T_min  0.612
_exptl_absorpt_correction_type   analytical
_exptl_absorpt_process_details
; 
CrysAlisPro 1.171.43.98a (Rigaku Oxford Diffraction, 2023) 
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            colourless
_exptl_crystal_density_diffrn    1.556
_exptl_crystal_description       rod
_exptl_crystal_F_000             808
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: acetonitrile'
_exptl_crystal_size_max          0.175
_exptl_crystal_size_mid          0.043
_exptl_crystal_size_min          0.034
_refine_diff_density_max         0.664
_refine_diff_density_min         -0.404
_refine_diff_density_rms         0.048
_refine_ls_abs_structure_details
; 
 Flack x determined using 2351 quotients [(I+)-(I-)]/[(I+)+(I-)] 
 (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). 
;
_refine_ls_abs_structure_Flack   -0.034(9)
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.026
_refine_ls_hydrogen_treatment    mixed
_refine_ls_matrix_type           full
_refine_ls_number_parameters     376
_refine_ls_number_reflns         5912
_refine_ls_number_restraints     1
_refine_ls_restrained_S_all      1.026
_refine_ls_R_factor_all          0.0207
_refine_ls_R_factor_gt           0.0201
_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^)+(0.0213P)^2^+0.4885P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0452
_refine_ls_wR_factor_ref         0.0455
_reflns_Friedel_coverage         0.721
_reflns_Friedel_fraction_full    0.806
_reflns_Friedel_fraction_max     0.742
_reflns_number_gt                5792
_reflns_number_total             5912
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00387g2.cif
_cod_data_source_block           LHEt3NH
_cod_depositor_comments
'Adding full bibliography for 7720679--7720691.cif.'
_cod_original_sg_symbol_H-M      'P 21'
_cod_database_code               7720685
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_min   0.423
_shelx_estimated_absorpt_t_max   0.824
_shelx_res_checksum              81025