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_7711144
_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         '0.21(C168 H168 N12 O12 V4), 0.57(C7 H8)'
_chemical_formula_sum            'C40 H40.57 N2.57 O2.57 V0.86'
_chemical_formula_weight         642.12
_chemical_properties_physical
Air-sensitive,Moisture-sensitive,Oxygen-sensitive
_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
_atom_sites_solution_primary     iterative
_audit_creation_date             2020-07-21
_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                 94.0449(10)
_cell_angle_gamma                90
_cell_formula_units_Z            28
_cell_length_a                   27.9809(19)
_cell_length_b                   18.6624(13)
_cell_length_c                   47.284(3)
_cell_measurement_reflns_used    9520
_cell_measurement_temperature    90(2)
_cell_measurement_theta_max      25.30
_cell_measurement_theta_min      2.35
_cell_volume                     24630(3)
_computing_cell_refinement       'SAINT V8.40A (?, 2016)'
_computing_data_reduction        'SAINT V8.40A (?, 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    'olex2.solve (Bourhis et al., 2015)'
_diffrn_ambient_temperature      90
_diffrn_detector                 'Bruker APEX2 area detector'
_diffrn_detector_area_resol_mean 7.9
_diffrn_detector_type            'CCD area detector'
_diffrn_measured_fraction_theta_full 1.000
_diffrn_measured_fraction_theta_max 0.997
_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  0.0658
_diffrn_reflns_av_unetI/netI     0.0489
_diffrn_reflns_Laue_measured_fraction_full 1.000
_diffrn_reflns_Laue_measured_fraction_max 0.997
_diffrn_reflns_limit_h_max       33
_diffrn_reflns_limit_h_min       -33
_diffrn_reflns_limit_k_max       22
_diffrn_reflns_limit_k_min       -22
_diffrn_reflns_limit_l_max       57
_diffrn_reflns_limit_l_min       -57
_diffrn_reflns_number            129460
_diffrn_reflns_point_group_measured_fraction_full 1.000
_diffrn_reflns_point_group_measured_fraction_max 0.997
_diffrn_reflns_theta_full        25.242
_diffrn_reflns_theta_max         25.404
_diffrn_reflns_theta_min         1.313
_diffrn_source                   'sealed X-ray tube'
_diffrn_standards_number         0
_exptl_absorpt_coefficient_mu    0.285
_exptl_absorpt_correction_T_max  0.7452
_exptl_absorpt_correction_T_min  0.7162
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_process_details
'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.0556 before and 0.0530 after correction. The Ratio of minimum to maximum transmission is 0.9611. The \l/2 correction factor is Not present.'
_exptl_crystal_colour            gold
_exptl_crystal_density_diffrn    1.212
_exptl_crystal_description       prism
_exptl_crystal_F_000             9488
_exptl_crystal_recrystallization_method
'Re-crystallisation from solvent: toluene'
_exptl_crystal_size_max          0.18
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.13
_refine_diff_density_max         1.488
_refine_diff_density_min         -0.626
_refine_diff_density_rms         0.060
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.071
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     1479
_refine_ls_number_reflns         22644
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.071
_refine_ls_R_factor_all          0.0781
_refine_ls_R_factor_gt           0.0530
_refine_ls_shift/su_max          0.003
_refine_ls_shift/su_mean         0.000
_refine_ls_structure_factor_coef Fsqd
_refine_ls_weighting_details
'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1451
_refine_ls_wR_factor_ref         0.1593
_reflns_Friedel_coverage         0.000
_reflns_number_gt                17129
_reflns_number_total             22644
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d2dt02177c3.cif
_cod_data_source_block           ls879
_cod_database_code               7711144
_shelx_shelxl_version_number     2018/1
_shelx_estimated_absorpt_t_max   0.964
_shelx_estimated_absorpt_t_min   0.951
_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 Aromatic/amide H refined with riding coordinates:
 C19(H19), C109(H109), C42(H42), C105(H105), C31(H31), C52(H52), C50(H50),
 C17(H17), C3(H3), C91(H91), C32(H32), C140(H140), C4(H4), C18(H18), C94(H94),
 C119(H119), C122(H122), C110(H110), C46(H46), C141(H141), C5(H5), C51(H51),
 C68(H68), C58(H58), C47(H47), C139(H139), C102(H102), C71(H71), C125(H125),
 C33(H33), C53(H53), C127(H127), C45(H45), C61(H61), C133(H133), C76(H76),
 C108(H108), C124(H124), C116(H116), C28(H28), C77(H77), C39(H39), C25(H25),
 C80(H80), C79(H79), C14(H14), C49(H49), C11(H11), C78(H78), C84(H84), C83(H83),
  C87(H87), C85(H85), C86(H86), C136(H136)
2.b Idealised Me refined as rotating group:
 C70(H70A,H70B,H70C), C101(H10D,H10E,H10F), C63(H63A,H63B,H63C), C38(H38A,H38B,
 H38C), C60(H60A,H60B,H60C), C118(H11A,H11B,H11C), C41(H41A,H41B,H41C),
 C104(H10G,H10H,H10I), C96(H96A,H96B,H96C), C107(H10J,H10K,H10L), C93(H93A,H93B,
 H93C), C90(H90A,H90B,H90C), C121(H12A,H12B,H12C), C132(H13D,H13E,H13F),
 C44(H44A,H44B,H44C), C74(H74A,H74B,H74C), C30(H30A,H30B,H30C), C27(H27A,H27B,
 H27C), C115(H11D,H11E,H11F), C24(H24A,H24B,H24C), C16(H16A,H16B,H16C),
 C10(H10A,H10B,H10C), C73(H73A,H73B,H73C), C57(H57A,H57B,H57C), C67(H67A,H67B,
 H67C), C13(H13A,H13B,H13C), C81(H81A,H81B,H81C), C138(H13G,H13H,H13I),
 C135(H13J,H13K,H13L)
;
_shelx_res_checksum              93956
_shelx_hkl_checksum              69905
_shelx_fab_checksum              99516
_olex2_diffrn_ambient_temperature_device 'Oxford Cryosystems'
_olex2_submission_special_instructions 'No special instructions were received'