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_7720394
_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         '2(C35 H28 N10 V), C7 H8'
_chemical_formula_sum            'C77 H64 N20 V2'
_chemical_formula_weight         1371.36
_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
_audit_creation_date             2026-01-14
_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                96.111(15)
_cell_angle_beta                 103.119(15)
_cell_angle_gamma                89.988(15)
_cell_formula_units_Z            1
_cell_length_a                   11.420(2)
_cell_length_b                   11.3445(19)
_cell_length_c                   13.155(3)
_cell_measurement_reflns_used    4414
_cell_measurement_temperature    150
_cell_measurement_theta_max      23.49
_cell_measurement_theta_min      1.57
_cell_volume                     1649.9(6)
_computing_cell_refinement       'STOE X-AREA'
_computing_data_collection       'STOE X-AREA'
_computing_data_reduction        'STOE X-RED'
_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 2018/2 (Sheldrick, 2018)'
_diffrn_ambient_temperature      150
_diffrn_detector_area_resol_mean 6.67
_diffrn_detector_type            STOE
_diffrn_measured_fraction_theta_full 0.997
_diffrn_measured_fraction_theta_max 0.997
_diffrn_measurement_details
;
 220 frames, detector distance = 100 mm
;
_diffrn_measurement_device       '2-circle goniometer'
_diffrn_measurement_device_type  'STOE IPDS 2'
_diffrn_measurement_method       'rotation method'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0385
_diffrn_reflns_av_unetI/netI     0.0744
_diffrn_reflns_Laue_measured_fraction_full 0.997
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -13
_diffrn_reflns_limit_k_max       13
_diffrn_reflns_limit_k_min       -13
_diffrn_reflns_limit_l_max       15
_diffrn_reflns_limit_l_min       -15
_diffrn_reflns_number            13060
_diffrn_reflns_point_group_measured_fraction_full 0.997
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.000
_diffrn_reflns_theta_max         24.999
_diffrn_reflns_theta_min         1.599
_exptl_absorpt_coefficient_mu    0.347
_exptl_absorpt_correction_type   none
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.380
_exptl_crystal_description       block
_exptl_crystal_F_000             712
_exptl_crystal_size_max          0.1
_exptl_crystal_size_mid          0.1
_exptl_crystal_size_min          0.1
_refine_diff_density_max         0.930
_refine_diff_density_min         -0.306
_refine_diff_density_rms         0.044
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.803
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     467
_refine_ls_number_reflns         5799
_refine_ls_number_restraints     72
_refine_ls_restrained_S_all      0.816
_refine_ls_R_factor_all          0.0601
_refine_ls_R_factor_gt           0.0379
_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^)+(0.0464P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0826
_refine_ls_wR_factor_ref         0.0859
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3598
_reflns_number_total             5799
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00230g2.cif
_cod_data_source_block           '[v(ai)5]'
_cod_depositor_comments
'Adding full bibliography for 7720394--7720397.cif.'
_cod_original_cell_volume        1649.7(5)
_cod_database_code               7720394
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.966
_shelx_estimated_absorpt_t_min   0.966
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups, All N(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2. Restrained distances
 C41-C36 \\sim C37-C38 \\sim C39-C40
 with sigma of 0.05
3. Rigid body (RIGU) restrains
 N1, C1, C2, C4, N2, C3, C5, C7, C6
 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001
4. Others
 Fixed Sof: C42(0.5) H42A(0.5) H42B(0.5) H42C(0.5) C41(0.5) C40(0.5) H40(0.5)
 C39(0.5) H39(0.5) C38(0.5) H38(0.5) C37(0.5) H37(0.5) C36(0.5) H36(0.5)
5.a Aromatic/amide H refined with riding coordinates:
 N8(H8), N10(H10), N6(H6), C29(H29), C30(H30), C8(H8A), C22(H22), C35(H35),
 C1(H1), C31(H31), C9(H9), C7(H7), C2(H2), C28(H28), C24(H24), C34(H34),
 C23(H23), C6(H6A), C15(H15), C27(H27), C16(H16), C12(H12), C21(H21), C14(H14),
 C17(H17), C13(H13), C20(H20), C5(H5), C40(H40), C39(H39), C38(H38), C37(H37),
 C36(H36)
5.b Fitted hexagon refined as free rotating group:
 C41(C40,C39,C38,C37,C36)
5.c Idealised Me refined as rotating group:
 C42(H42A,H42B,H42C)
;
_shelx_res_checksum              11736
_shelx_hkl_checksum              70094
_olex2_submission_special_instructions 'No special instructions were received'