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_7720395
_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         'C48 H32 N4 Na V'
_chemical_formula_sum            'C48 H32 N4 Na V'
_chemical_formula_weight         738.70
_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
_audit_creation_date             2025-01-17
_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                 98.252(18)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.852(3)
_cell_length_b                   13.732(2)
_cell_length_c                   18.117(4)
_cell_measurement_reflns_used    1768
_cell_measurement_temperature    150
_cell_measurement_theta_max      24.95
_cell_measurement_theta_min      2.08
_cell_volume                     3410.5(12)
_computing_cell_refinement       'STOE X-Area'
_computing_data_collection       'STOE X-Area'
_computing_data_reduction        'STOE X-Area'
_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 Imaging Plate'
_diffrn_measured_fraction_theta_full 0.999
_diffrn_measured_fraction_theta_max 0.999
_diffrn_measurement_details
;
 128 frames, detector distance = 100 mm
;
_diffrn_measurement_device       '2-circle diffractometer'
_diffrn_measurement_device_type  'STOE IPDS II'
_diffrn_measurement_method       'rotation method, \w scans'
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0251
_diffrn_reflns_av_unetI/netI     0.0761
_diffrn_reflns_Laue_measured_fraction_full 0.999
_diffrn_reflns_Laue_measured_fraction_max 0.999
_diffrn_reflns_limit_h_max       13
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_k_max       16
_diffrn_reflns_limit_k_min       -14
_diffrn_reflns_limit_l_max       21
_diffrn_reflns_limit_l_min       -21
_diffrn_reflns_number            7516
_diffrn_reflns_point_group_measured_fraction_full 0.999
_diffrn_reflns_point_group_measured_fraction_max 0.999
_diffrn_reflns_theta_full        24.996
_diffrn_reflns_theta_max         24.996
_diffrn_reflns_theta_min         2.099
_exptl_absorpt_coefficient_mu    0.348
_exptl_absorpt_correction_T_max  0.9811
_exptl_absorpt_correction_T_min  0.9759
_exptl_absorpt_correction_type   integration
_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 a spherical absorption correction was performed within STOE LANA.
;
_exptl_crystal_colour            black
_exptl_crystal_colour_primary    black
_exptl_crystal_density_diffrn    1.439
_exptl_crystal_density_method    'not measured'
_exptl_crystal_description       block
_exptl_crystal_F_000             1528
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.2
_exptl_crystal_size_min          0.17
_refine_diff_density_max         0.189
_refine_diff_density_min         -0.277
_refine_diff_density_rms         0.035
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   0.731
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     245
_refine_ls_number_reflns         3008
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      0.731
_refine_ls_R_factor_all          0.0482
_refine_ls_R_factor_gt           0.0267
_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^)+(0.0168P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.0467
_refine_ls_wR_factor_ref         0.0485
_reflns_Friedel_coverage         0.000
_reflns_number_gt                1894
_reflns_number_total             3008
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d6dt00230g2.cif
_cod_data_source_block           '[nav(cbz)4]'
_cod_depositor_comments
'Adding full bibliography for 7720394--7720397.cif.'
_cod_original_cell_volume        3410.2(12)
_cod_database_code               7720395
_shelx_shelxl_version_number     2019/3
_shelx_estimated_absorpt_t_max   0.943
_shelx_estimated_absorpt_t_min   0.918
_olex2_refinement_description
;
1.a Aromatic/amide H refined with riding coordinates:
 C2(H2), C9(H9), C14(H14), C15(H15), C23(H23), C20(H20), C16(H16), C3(H3),
 C17(H17), C22(H22), C10(H10), C5(H5), C12(H12), C11(H11), C4(H4), C21(H21)
;
_shelx_res_checksum              45085
_shelx_hkl_checksum              94629
_olex2_submission_special_instructions 'No special instructions were received'