Vanadium Pyridonates: Dimerization, Redox Behaviour, and Metal-Ligand Cooperativity
Griffin, Samuel E.; Adamczyk, Olivia V.; Schafer, Laurel L.; Dalton Transactions  (2022) –; doi:10.1039/D2DT02177C

data_7711143
_publ_section_title
;
 Vanadium Pyridonates: Dimerization, Redox Behaviour, and Metal-Ligand
 Cooperativity
;
_journal_name_full               'Dalton Transactions'
_journal_paper_doi               10.1039/D2DT02177C
_journal_year                    2022
_chemical_formula_moiety         'C42 H56 N4 O2 V'
_chemical_formula_sum            'C42 H56 N4 O2 V'
_chemical_formula_weight         699.84
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_Hall           '-P 2ybc'
_space_group_name_H-M_alt        'P 1 21/c 1'
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_audit_creation_date             2021-02-12
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2021-02-12 deposited with the CCDC.	2022-08-30 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 108.269(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   13.2954(10)
_cell_length_b                   30.480(2)
_cell_length_c                   10.2846(8)
_cell_measurement_reflns_used    7519
_cell_measurement_temperature    100
_cell_measurement_theta_max      23.95
_cell_measurement_theta_min      2.29
_cell_volume                     3957.7(5)
_computing_cell_refinement       'SAINT V8.38A (?, 2016)'
_computing_data_reduction        'SAINT V8.38A (?, 2016)'
_computing_molecular_graphics    'Olex2 (Dolomanov et al., 2009)'
_computing_publication_material  'Olex2 (Dolomanov et al., 2009)'
_computing_structure_refinement  'ShelXL (Sheldrick, 2015)'
_computing_structure_solution    'ShelXT (Sheldrick, 2015)'
_diffrn_ambient_temperature      100
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 0.988
_diffrn_measured_fraction_theta_max 0.988
_diffrn_measurement_device       'Bruker D8 Kappa diffractometer'
_diffrn_measurement_device_type  'Bruker APEX II area detector'
_diffrn_measurement_method       '\w and \f scans'
_diffrn_radiation_monochromator  'TRIUMPH curved-crystal'
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           MoK\a
_diffrn_radiation_wavelength     0.71073
_diffrn_reflns_av_R_equivalents  0.0569
_diffrn_reflns_av_unetI/netI     0.0634
_diffrn_reflns_Laue_measured_fraction_full 0.988
_diffrn_reflns_Laue_measured_fraction_max 0.988
_diffrn_reflns_limit_h_max       15
_diffrn_reflns_limit_h_min       -15
_diffrn_reflns_limit_k_max       35
_diffrn_reflns_limit_k_min       -35
_diffrn_reflns_limit_l_max       11
_diffrn_reflns_limit_l_min       -11
_diffrn_reflns_number            24373
_diffrn_reflns_point_group_measured_fraction_full 0.988
_diffrn_reflns_point_group_measured_fraction_max 0.988
_diffrn_reflns_theta_full        24.184
_diffrn_reflns_theta_max         24.184
_diffrn_reflns_theta_min         1.746
_diffrn_source                   'sealed X-ray tube'
_diffrn_source_type              'Incoatec I\ms'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.289
_exptl_absorpt_correction_T_max  0.7450
_exptl_absorpt_correction_T_min  0.5844
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1273 before and 0.0530 after correction. The Ratio of minimum to maximum transmission is 0.8187. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            red
_exptl_crystal_colour_primary    red
_exptl_crystal_density_diffrn    1.175
_exptl_crystal_description       irregular
_exptl_crystal_F_000             1500
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene/pentane'
_exptl_crystal_size_max          0.44
_exptl_crystal_size_mid          0.11
_exptl_crystal_size_min          0.08
_refine_diff_density_max         0.316
_refine_diff_density_min         -0.438
_refine_diff_density_rms         0.064
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.093
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     454
_refine_ls_number_reflns         6264
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.093
_refine_ls_R_factor_all          0.1156
_refine_ls_R_factor_gt           0.0786
_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^)+(0.0001P)^2^+14.8317P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1563
_refine_ls_wR_factor_ref         0.1677
_reflns_Friedel_coverage         0.000
_reflns_number_gt                4027
_reflns_number_total             6264
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02177c3.cif
_cod_data_source_block           ls751_0m_a
_cod_original_cell_volume        3957.6(5)
_cod_database_code               7711143
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.977
_shelx_estimated_absorpt_t_min   0.883
_olex2_refinement_description
;
1. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
2.a Ternary CH refined with riding coordinates:
 C36(H36), C29(H29), C10(H10), C17(H17)
2.b Aromatic/amide H refined with riding coordinates:
 C26(H26), C7(H7), C34(H34), C32(H32), C3(H3), C15(H15), C22(H22), C24(H24),
 C14(H14), C33(H33), C23(H23), C13(H13), C25(H25), C4(H4), C6(H6), C5(H5)
2.c Idealised Me refined as rotating group:
 C37(H37A,H37B,H37C), C42(H42A,H42B,H42C), C31(H31A,H31B,H31C), C39(H39A,H39B,
 H39C), C19(H19A,H19B,H19C), C38(H38A,H38B,H38C), C30(H30A,H30B,H30C), C41(H41A,
 H41B,H41C), C40(H40A,H40B,H40C), C18(H18A,H18B,H18C), C11(H11A,H11B,H11C),
 C12(H12A,H12B,H12C)
;
_shelx_res_checksum              42010
_shelx_hkl_checksum              38771
_olex2_submission_original_sample_id SEG-111
_olex2_submission_special_instructions 'No special instructions were received'