Homoleptic complexes of vanadium and N-heterocycles made <i>via</i> oxidation of vanadium nanoparticles.
Baumgärtner, Lena; Feldmann, Claus; Dalton transactions (Cambridge, England : 2003) 55 (2026) 4856–4866; doi:10.1039/d6dt00230g

data_7720397
_publ_section_title
;
 Homoleptic complexes of vanadium and N-heterocycles made <i>via</i>
 oxidation of vanadium nanoparticles.
;
_journal_issue                   12
_journal_name_full
'Dalton transactions (Cambridge, England : 2003)'
_journal_page_first              4856
_journal_page_last               4866
_journal_paper_doi               10.1039/d6dt00230g
_journal_volume                  55
_journal_year                    2026
_chemical_formula_moiety         'C36 H24 N6 V'
_chemical_formula_sum            'C36 H24 N6 V'
_chemical_formula_weight         591.55
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2yn'
_space_group_name_H-M_alt        'P 1 21/n 1'
_atom_sites_solution_hydrogens   geom
_audit_creation_date             2025-01-20
_audit_creation_method
;
Olex2 1.5
(compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817)
;
_audit_update_record
;
2026-01-14 deposited with the CCDC.	2026-02-27 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 103.303(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   10.2347(5)
_cell_length_b                   13.5883(8)
_cell_length_c                   20.2593(8)
_cell_measurement_reflns_used    15302
_cell_measurement_temperature    100
_cell_measurement_theta_max      31.12
_cell_measurement_theta_min      2.50
_cell_volume                     2741.9(2)
_computing_cell_refinement
;
X-Area Recipe 2.0.2 (STOE, 2024)
;
_computing_data_collection
;
X-Area Pilatus3_SV 1.31.194.0 (STOE, 2023)
;
_computing_data_reduction
;
X-Area Integrate 2.5.18.0 (STOE, 2024)
X-Area LANA 2.8.4 (STOE, 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)'
_computing_structure_solution    'SHELXT  (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector_area_resol_mean 5.81
_diffrn_detector_type            'DECTRIS PILATUS 200K'
_diffrn_measured_fraction_theta_full 0.994
_diffrn_measured_fraction_theta_max 0.813
_diffrn_measurement_details
;
 283 frames, detector distance = 40 mm
;
_diffrn_measurement_device       'Eulerian 4-circle diffractometer'
_diffrn_measurement_device_type  'STOE STADIVARI'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0574
_diffrn_reflns_av_unetI/netI     0.0697
_diffrn_reflns_Laue_measured_fraction_full 0.994
_diffrn_reflns_Laue_measured_fraction_max 0.813
_diffrn_reflns_limit_h_max       14
_diffrn_reflns_limit_h_min       -14
_diffrn_reflns_limit_k_max       19
_diffrn_reflns_limit_k_min       -19
_diffrn_reflns_limit_l_max       28
_diffrn_reflns_limit_l_min       -28
_diffrn_reflns_number            16303
_diffrn_reflns_point_group_measured_fraction_full 0.994
_diffrn_reflns_point_group_measured_fraction_max 0.813
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         31.308
_diffrn_reflns_theta_min         2.494
_exptl_absorpt_coefficient_mu    0.401
_exptl_absorpt_correction_T_max  0.9881
_exptl_absorpt_correction_T_min  0.9554
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
;
STOE X-Red32, absorption correction by Gaussian integration, analogous to
P. Coppens, "The Evaluation of Absorption and Extinction in Single-Crystal
Structure Analysis", published in: F. R. Ahmed (Editor), "Crystallographic
Computing", Munksgaard, Copenhagen (1970), 255 - 270. Afterwards scaling of
reflection intensities was performed within STOE LANA. J. Koziskova, F. Hahn,
J. Richter, J. Kozisek, Acta Chimica Slovaca, vol. 9, no. 2, 2016, pp. 136-140.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.433
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       prism
_exptl_crystal_F_000             1220
_exptl_crystal_size_max          0.114
_exptl_crystal_size_mid          0.082
_exptl_crystal_size_min          0.03
_refine_diff_density_max         0.603
_refine_diff_density_min         -1.058
_refine_diff_density_rms         0.098
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.043
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     388
_refine_ls_number_reflns         7284
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.043
_refine_ls_R_factor_all          0.1111
_refine_ls_R_factor_gt           0.0682
_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^)+(0.0904P)^2^+4.0610P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1658
_refine_ls_wR_factor_ref         0.1950
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4933
_reflns_number_total             7284
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00230g2.cif
_cod_data_source_block           '[v(phen)3]'
_cod_depositor_comments
'Adding full bibliography for 7720394--7720397.cif.'
_cod_database_code               7720397
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.988
_shelx_estimated_absorpt_t_min   0.956
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
2.a Aromatic/amide H refined with riding coordinates:
 C34(H34), C30(H30), C12(H12), C25(H25), C6(H6), C27(H27), C1(H1), C14(H14),
 C36(H36), C15(H15), C11(H11), C19(H19), C24(H24), C31(H31), C35(H35), C2(H2),
 C10(H10), C26(H26), C22(H22), C13(H13), C18(H18), C3(H3), C7(H7), C23(H23)
;
_shelx_res_checksum              3927
_shelx_hkl_checksum              76706
_olex2_submission_special_instructions 'No special instructions were received'