Remarkable reversal of <sup>13</sup>C-NMR assignment in d<sup>1</sup>, d<sup>2</sup> compared to d<sup>8</sup>, d<sup>9</sup> acetylacetonate complexes: analysis and explanation based on solid-state MAS NMR and computations.
Andersen, Anders B. A.; Pyykkönen, Ari; Jensen, Hans Jørgen Aa; McKee, Vickie; Vaara, Juha; Nielsen, Ulla Gro; Physical chemistry chemical physics : PCCP 22 (2020) 8048–8059; doi:10.1039/d0cp00980f

data_7240163
_publ_section_title
;
 Remarkable reversal of <sup>13</sup>C-NMR assignment in d<sup>1</sup>,
 d<sup>2</sup> compared to d<sup>8</sup>, d<sup>9</sup> acetylacetonate
 complexes: analysis and explanation based on solid-state MAS NMR and
 computations.
;
_journal_issue                   15
_journal_name_full               'Physical chemistry chemical physics : PCCP'
_journal_page_first              8048
_journal_page_last               8059
_journal_paper_doi               10.1039/d0cp00980f
_journal_volume                  22
_journal_year                    2020
_chemical_formula_moiety         'C15 H21 O6 V'
_chemical_formula_sum            'C15 H21 O6 V'
_chemical_formula_weight         348.26
_chemical_name_systematic        Tris(2,4-pentanedionato-O,O')-vanadium(iii)
_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
_atom_sites_solution_primary     dual
_audit_creation_date             2020-02-11
_audit_creation_method
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_audit_update_record
;
2020-02-11 deposited with the CCDC.	2020-03-23 downloaded from the CCDC.
;
_cell_angle_alpha                90
_cell_angle_beta                 90.022(4)
_cell_angle_gamma                90
_cell_formula_units_Z            4
_cell_length_a                   7.9785(3)
_cell_length_b                   12.9974(5)
_cell_length_c                   15.9540(6)
_cell_measurement_reflns_used    5014
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.1910
_cell_measurement_theta_min      4.3720
_cell_volume                     1654.43(11)
_computing_cell_refinement       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_collection       'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_data_reduction        'CrysAlisPro 1.171.39.27b (Rigaku OD, 2015)'
_computing_molecular_graphics    'Mercury (Macrae at al., 2008)'
_computing_publication_material
'Olex2 (Dolomanov et al. 2009), PublCIF (Westrip, 2010)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015a)'
_computing_structure_solution    'SHELXT (Sheldrick 2015)'
_diffrn_ambient_environment      N~2~
_diffrn_ambient_temperature      100.00(10)
_diffrn_detector                 'CCD plate'
_diffrn_detector_area_resol_mean 5.2923
_diffrn_detector_type            AtlasS2
_diffrn_measured_fraction_theta_full 0.998
_diffrn_measured_fraction_theta_max 0.962
_diffrn_measurement_details
;
List of Runs (angles in degrees, time in seconds):

  # Type    Start    End  Width  t~exp~   \w     \q     \k     \f   Frames
  1  \w    -47.00   3.00   1.00    2.56    --    0.00 -38.00   0.00   50
  2  \w    -65.00   0.00   1.00    2.56    --    0.00 -38.00 120.00   65
  3  \w     37.00  64.00   1.00   10.23    --  101.75 -38.00 -90.00   27
  4  \w     48.00  99.00   1.00   10.23    --  101.75 -57.00 -60.00   51
  5  \w     37.00  64.00   1.00   10.23    --  101.75 -38.00-120.00   27
  6  \w     38.00  66.00   1.00   10.23    --  101.75 -38.00-150.00   28
  7  \w     32.00  69.00   1.00   10.23    --  101.75 -19.00 -30.00   37
  8  \w     36.00 100.00   1.00   10.23    --  101.75 -57.00  30.00   64
  9  \w     64.00 126.00   1.00   10.23    --  101.75 -77.00  90.00   62
 10  \w     32.00  66.00   1.00   10.23    --  101.75 -19.00  60.00   34
 11  \w     40.00  67.00   1.00   10.23    --  101.75 -19.00 120.00   27
 12  \w     39.00  66.00   1.00   10.23    --  101.75 -38.00 150.00   27
 13  \w     38.00  63.00   1.00   10.23    --  101.75 -38.00 120.00   25
 14  \w     99.00 142.00   1.00   10.23    --  101.75 125.00 -90.00   43
 15  \w   -114.00 -87.00   1.00   10.23    --  -80.25 -99.00  30.00   27
;
_diffrn_measurement_device       'four-circle diffractometer'
_diffrn_measurement_device_type  'XtaLAB Synergy, Dualflex, AtlasS2'
_diffrn_measurement_method       '\w scans'
_diffrn_orient_matrix_type
'CrysAlisPro convention (1999,Acta A55,543-557)'
_diffrn_orient_matrix_UB_11      -0.0085237000
_diffrn_orient_matrix_UB_12      0.0664222000
_diffrn_orient_matrix_UB_13      -0.0798553000
_diffrn_orient_matrix_UB_21      -0.0973034000
_diffrn_orient_matrix_UB_22      -0.0862148000
_diffrn_orient_matrix_UB_23      -0.0449229000
_diffrn_orient_matrix_UB_31      -0.1665136000
_diffrn_orient_matrix_UB_32      0.0470566000
_diffrn_orient_matrix_UB_33      0.0304282000
_diffrn_radiation_monochromator  mirror
_diffrn_radiation_probe          x-ray
_diffrn_radiation_type           CuK\a
_diffrn_radiation_wavelength     1.54184
_diffrn_reflns_av_R_equivalents  0.0353
_diffrn_reflns_av_unetI/netI     0.0410
_diffrn_reflns_Laue_measured_fraction_full 0.998
_diffrn_reflns_Laue_measured_fraction_max 0.962
_diffrn_reflns_limit_h_max       5
_diffrn_reflns_limit_h_min       -9
_diffrn_reflns_limit_k_max       15
_diffrn_reflns_limit_k_min       -16
_diffrn_reflns_limit_l_max       18
_diffrn_reflns_limit_l_min       -19
_diffrn_reflns_number            7657
_diffrn_reflns_point_group_measured_fraction_full 0.998
_diffrn_reflns_point_group_measured_fraction_max 0.962
_diffrn_reflns_theta_full        67.684
_diffrn_reflns_theta_max         76.234
_diffrn_reflns_theta_min         4.388
_diffrn_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_exptl_absorpt_coefficient_mu    5.243
_exptl_absorpt_correction_T_max  0.933
_exptl_absorpt_correction_T_min  0.650
_exptl_absorpt_correction_type   gaussian
_exptl_absorpt_process_details
;
CrysAlisPro 1.171.39.27b (Rigaku Oxford Diffraction, 2015)
Numerical absorption correction based on gaussian integration over
			a multifaceted crystal model
Empirical absorption correction using spherical harmonics,
 implemented in SCALE3 ABSPACK scaling algorithm.
;
_exptl_crystal_colour            'clear intense orange'
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_description       block
_exptl_crystal_F_000             728
_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
_exptl_crystal_size_max          0.121
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.035
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.077
_refine_ls_extinction_method     none
_refine_ls_goodness_of_fit_ref   1.064
_refine_ls_hydrogen_treatment    constr
_refine_ls_matrix_type           full
_refine_ls_number_parameters     206
_refine_ls_number_reflns         3338
_refine_ls_number_restraints     0
_refine_ls_restrained_S_all      1.064
_refine_ls_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0465
_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^)+(0.0799P)^2^+0.9469P] where P=(Fo^2^+2Fc^2^)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1291
_reflns_Friedel_coverage         0.000
_reflns_number_gt                3259
_reflns_number_total             3338
_reflns_threshold_expression     'I > 2\s(I)'
_cod_data_source_file            d0cp00980f2.cif
_cod_data_source_block           vacac
_cod_depositor_comments          'Adding full bibliography for 7240163.cif.'
_cod_original_cell_volume        1654.42(11)
_cod_database_code               7240163
_shelx_shelxl_version_number     2018/3
_chemical_oxdiff_formula         C15H21O6V
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_olex2_refinement_description
;
1. Twinned data refinement
 Scales: 0.565(2)
 0.435(2)
2. Fixed Uiso
 At 1.2 times of:
  All C(H) groups
 At 1.5 times of:
  All C(H,H,H) groups
3.a Aromatic/amide H refined with riding coordinates:
 C3(H3), C8(H8), C13(H13)
3.b Idealised Me refined as rotating group:
 C1(H1A,H1B,H1C), C5(H5A,H5B,H5C), C6(H6A,H6B,H6C), C10(H10A,H10B,H10C),
 C11(H11A,H11B,H11C), C15(H15A,H15B,H15C)
;
_shelx_res_checksum              76465
_olex2_submission_special_instructions 'No special instructions were received'
_oxdiff_exptl_absorpt_empirical_details
;
Empirical correction (ABSPACK) includes:
- Absorption correction using spherical harmonics
- Frame scaling
- Detector area scaling
;
_oxdiff_exptl_absorpt_empirical_full_max 1.418
_oxdiff_exptl_absorpt_empirical_full_min 0.673