# Electronic Supplementary Material (ESI) for Physical Chemistry Chemical Physics.
# This journal is © the Owner Societies 2020

####################################################################### 
# 
# This file contains crystal structure data downloaded from the 
# Cambridge Structural Database (CSD) hosted by the Cambridge 
# Crystallographic Data Centre (CCDC).
# 
# Full information about CCDC data access policies and citation 
# guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 
# 
# Audit and citation data items may have been added by the CCDC. 
# Please retain this information to preserve the provenance of 
# this file and to allow appropriate attribution of the data. 
# 
#######################################################################

data_vacac
_database_code_depnum_ccdc_archive 'CCDC 1983408'
loop_
_audit_author_name
_audit_author_address
'Vickie McKee'
;Dublin City Univ and Univ Southern Denmark
Republic of Ireland
;
_audit_update_record             
;
2020-02-11 deposited with the CCDC.	2020-03-23 downloaded from the CCDC.
;
_audit_creation_date             2020-02-11
_audit_creation_method           
;
Olex2 1.2
(compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506)
;
_shelx_SHELXL_version_number     2018/3
_chemical_name_common            ?
_chemical_name_systematic        Tris(2,4-pentanedionato-O,O')-vanadium(iii)
_chemical_formula_moiety         'C15 H21 O6 V'
_chemical_formula_sum            'C15 H21 O6 V'
_chemical_formula_weight         348.26
_chemical_melting_point          ?
_chemical_oxdiff_formula         C15H21O6V
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'

_shelx_space_group_comment       
;
The symmetry employed for this shelxl refinement is uniquely defined
by the following loop, which should always be used as a source of
symmetry information in preference to the above space-group names.
They are only intended as comments.
;
_space_group_crystal_system      monoclinic
_space_group_IT_number           14
_space_group_name_H-M_alt        'P 1 21/n 1'
_space_group_name_Hall           '-P 2yn'
loop_
_space_group_symop_operation_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'

_cell_length_a                   7.9785(3)
_cell_length_b                   12.9974(5)
_cell_length_c                   15.9540(6)
_cell_angle_alpha                90
_cell_angle_beta                 90.022(4)
_cell_angle_gamma                90
_cell_volume                     1654.42(11)
_cell_formula_units_Z            4
_cell_measurement_reflns_used    5014
_cell_measurement_temperature    100.00(10)
_cell_measurement_theta_max      76.1910
_cell_measurement_theta_min      4.3720
_shelx_estimated_absorpt_T_max   ?
_shelx_estimated_absorpt_T_min   ?
_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_absorpt_special_details   ?
_exptl_crystal_colour            'clear intense orange'
_exptl_crystal_density_diffrn    1.398
_exptl_crystal_density_meas      ?
_exptl_crystal_density_method    ?
_exptl_crystal_description       block
_exptl_crystal_F_000             728
loop_
_exptl_crystal_face_index_h
_exptl_crystal_face_index_k
_exptl_crystal_face_index_l
_exptl_crystal_face_perp_dist
4 -5 -2 0.0496
-4 5 3 0.0348
2 5 -4 0.0608
5 -1 -4 0.0475
-3 -5 5 0.0416
-1 -1 -5 0.0173
1 1 5 0.0173

_exptl_crystal_size_max          0.121
_exptl_crystal_size_mid          0.087
_exptl_crystal_size_min          0.035
loop_
_exptl_oxdiff_crystal_face_indexfrac_h
_exptl_oxdiff_crystal_face_indexfrac_k
_exptl_oxdiff_crystal_face_indexfrac_l
_exptl_oxdiff_crystal_face_x
_exptl_oxdiff_crystal_face_y
_exptl_oxdiff_crystal_face_z
3.9954 -4.9937 -1.9919 -0.2067 0.1312 -0.9609
-3.9945 4.9951 2.9931 0.1268 -0.1764 0.9913
1.9956 5.0015 -4.0185 0.6361 -0.4449 -0.2192
4.9933 -0.9924 -4.0050 0.2113 -0.2204 -1.0000
-2.9941 -5.0028 5.0203 -0.7077 0.4971 0.4159
-1.0041 -1.0100 -5.0029 0.3410 0.4095 -0.0326
1.0041 1.0100 5.0029 -0.3410 -0.4095 0.0326

_exptl_transmission_factor_max   ?
_exptl_transmission_factor_min   ?
_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_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  tₑₓₚ   ω     θ     κ     φ   Frames
#--------------------------------------------------------------------------
  1  ω    -47.00   3.00   1.00    2.56    --    0.00 -38.00   0.00   50
  2  ω    -65.00   0.00   1.00    2.56    --    0.00 -38.00 120.00   65
  3  ω     37.00  64.00   1.00   10.23    --  101.75 -38.00 -90.00   27
  4  ω     48.00  99.00   1.00   10.23    --  101.75 -57.00 -60.00   51
  5  ω     37.00  64.00   1.00   10.23    --  101.75 -38.00-120.00   27
  6  ω     38.00  66.00   1.00   10.23    --  101.75 -38.00-150.00   28
  7  ω     32.00  69.00   1.00   10.23    --  101.75 -19.00 -30.00   37
  8  ω     36.00 100.00   1.00   10.23    --  101.75 -57.00  30.00   64
  9  ω     64.00 126.00   1.00   10.23    --  101.75 -77.00  90.00   62
 10  ω     32.00  66.00   1.00   10.23    --  101.75 -19.00  60.00   34
 11  ω     40.00  67.00   1.00   10.23    --  101.75 -19.00 120.00   27
 12  ω     39.00  66.00   1.00   10.23    --  101.75 -38.00 150.00   27
 13  ω     38.00  63.00   1.00   10.23    --  101.75 -38.00 120.00   25
 14  ω     99.00 142.00   1.00   10.23    --  101.75 125.00 -90.00   43
 15  ω   -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       'ω 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_source                   'micro-focus sealed X-ray tube'
_diffrn_source_type              'PhotonJet (Cu) X-ray Source'
_reflns_Friedel_coverage         0.000
_reflns_Friedel_fraction_full    .
_reflns_Friedel_fraction_max     .
_reflns_number_gt                3259
_reflns_number_total             3338
_reflns_odcompleteness_completeness 99.81
_reflns_odcompleteness_iscentric 1
_reflns_odcompleteness_theta     66.97
_reflns_special_details          
;
 Reflections were merged by SHELXL according to the crystal
 class for the calculation of statistics and refinement.
 
 _reflns_Friedel_fraction is defined as the number of unique
 Friedel pairs measured divided by the number that would be
 possible theoretically, ignoring centric projections and
 systematic absences. Completness statistics refer to single and
 composite reflections containing twin component 1 only.
;
_reflns_threshold_expression     'I > 2σ(I)'
_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_solution    'SHELXT (Sheldrick 2015)'
_computing_structure_refinement  'SHELXL-2018/3 (Sheldrick, 2015a)'
_refine_diff_density_max         0.429
_refine_diff_density_min         -0.676
_refine_diff_density_rms         0.077
_refine_ls_extinction_coef       .
_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_R_factor_all          0.0474
_refine_ls_R_factor_gt           0.0465
_refine_ls_restrained_S_all      1.064
_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/[σ²(Fo²)+(0.0799P)²+0.9469P] where P=(Fo²+2Fc²)/3'
_refine_ls_weighting_scheme      calc
_refine_ls_wR_factor_gt          0.1274
_refine_ls_wR_factor_ref         0.1291
_refine_special_details          'Refined as a 2-component twin.,Twin'
_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)
;
_atom_sites_solution_hydrogens   geom
_atom_sites_solution_primary     dual
_atom_sites_solution_secondary   ?
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_site_symmetry_order
_atom_site_calc_flag
_atom_site_refinement_flags_posn
_atom_site_refinement_flags_adp
_atom_site_refinement_flags_occupancy
_atom_site_disorder_assembly
_atom_site_disorder_group
V1 V 0.45051(6) 0.48712(3) 0.74880(4) 0.01893(15) Uani 1 1 d . . . . .
O1 O 0.4485(3) 0.62614(16) 0.69633(13) 0.0242(5) Uani 1 1 d . . . . .
O2 O 0.3468(3) 0.43419(18) 0.64385(14) 0.0257(5) Uani 1 1 d . . . . .
O3 O 0.6828(3) 0.46215(18) 0.70839(15) 0.0235(5) Uani 1 1 d . . . . .
O4 O 0.4528(3) 0.34672(16) 0.79790(14) 0.0240(5) Uani 1 1 d . . . . .
O5 O 0.5424(3) 0.55321(17) 0.85237(13) 0.0246(5) Uani 1 1 d . . . . .
O6 O 0.2214(3) 0.50642(18) 0.79859(15) 0.0237(5) Uani 1 1 d . . . . .
C1 C 0.4325(5) 0.7647(3) 0.6022(2) 0.0307(7) Uani 1 1 d . . . . .
H1A H 0.544223 0.787255 0.619868 0.046 Uiso 1 1 calc GR . . . .
H1B H 0.347178 0.804625 0.632135 0.046 Uiso 1 1 calc GR . . . .
H1C H 0.419886 0.775553 0.541712 0.046 Uiso 1 1 calc GR . . . .
C2 C 0.4111(4) 0.6524(3) 0.6219(2) 0.0235(7) Uani 1 1 d . . . . .
C3 C 0.3509(5) 0.5840(3) 0.5607(2) 0.0261(7) Uani 1 1 d . . . . .
H3 H 0.330229 0.610475 0.506158 0.031 Uiso 1 1 calc R . . . .
C4 C 0.3196(4) 0.4805(3) 0.5745(2) 0.0239(7) Uani 1 1 d . . . . .
C5 C 0.2452(5) 0.4163(3) 0.5057(2) 0.0309(8) Uani 1 1 d . . . . .
H5A H 0.279907 0.443866 0.451268 0.046 Uiso 1 1 calc GR . . . .
H5B H 0.122655 0.418027 0.509842 0.046 Uiso 1 1 calc GR . . . .
H5C H 0.284352 0.345188 0.511223 0.046 Uiso 1 1 calc GR . . . .
C6 C 0.9352(5) 0.3822(3) 0.6708(2) 0.0281(7) Uani 1 1 d . . . . .
H6A H 0.983109 0.312819 0.669220 0.042 Uiso 1 1 calc GR . . . .
H6B H 1.007120 0.427040 0.704704 0.042 Uiso 1 1 calc GR . . . .
H6C H 0.927609 0.409556 0.613705 0.042 Uiso 1 1 calc GR . . . .
C7 C 0.7654(4) 0.3781(2) 0.70843(19) 0.0209(6) Uani 1 1 d . . . . .
C8 C 0.7088(4) 0.2855(2) 0.7429(2) 0.0248(6) Uani 1 1 d . . . . .
H8 H 0.777112 0.226222 0.736118 0.030 Uiso 1 1 calc R . . . .
C9 C 0.5592(4) 0.2746(2) 0.78631(19) 0.0205(6) Uani 1 1 d . . . . .
C10 C 0.5166(4) 0.1720(3) 0.8243(2) 0.0255(7) Uani 1 1 d . . . . .
H10A H 0.416286 0.144186 0.797083 0.038 Uiso 1 1 calc GR . . . .
H10B H 0.495290 0.180578 0.884402 0.038 Uiso 1 1 calc GR . . . .
H10C H 0.610563 0.124490 0.816227 0.038 Uiso 1 1 calc GR . . . .
C11 C 0.5749(6) 0.6459(3) 0.9776(2) 0.0371(9) Uani 1 1 d . . . . .
H11A H 0.622117 0.709900 0.955265 0.056 Uiso 1 1 calc GR . . . .
H11B H 0.666049 0.598702 0.992321 0.056 Uiso 1 1 calc GR . . . .
H11C H 0.508236 0.661112 1.027622 0.056 Uiso 1 1 calc GR . . . .
C12 C 0.4642(5) 0.5965(2) 0.9119(2) 0.0247(7) Uani 1 1 d . . . . .
C13 C 0.2920(5) 0.5987(3) 0.9211(2) 0.0314(8) Uani 1 1 d . . . . .
H13 H 0.247394 0.633309 0.968550 0.038 Uiso 1 1 calc R . . . .
C14 C 0.1791(4) 0.5533(2) 0.86519(19) 0.0221(6) Uani 1 1 d . . . . .
C15 C -0.0054(5) 0.5573(3) 0.8820(2) 0.0310(8) Uani 1 1 d . . . . .
H15A H -0.053042 0.619001 0.856016 0.047 Uiso 1 1 calc GR . . . .
H15B H -0.024737 0.559466 0.942677 0.047 Uiso 1 1 calc GR . . . .
H15C H -0.059177 0.495968 0.858473 0.047 Uiso 1 1 calc GR . . . .


_geom_special_details            
;
 All esds (except the esd in the dihedral angle between two l.s. planes)
 are estimated using the full covariance matrix.  The cell esds are taken
 into account individually in the estimation of esds in distances, angles
 and torsion angles; correlations between esds in cell parameters are only
 used when they are defined by crystal symmetry.  An approximate (isotropic)
 treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
V1 O1 1.991(2) . ?
V1 O2 1.990(2) . ?
V1 O3 1.989(2) . ?
V1 O4 1.986(2) . ?
V1 O5 2.001(2) . ?
V1 O6 2.009(3) . ?
O1 C2 1.272(4) . ?
O2 C4 1.278(4) . ?
O3 C7 1.276(4) . ?
O4 C9 1.278(4) . ?
O5 C12 1.267(4) . ?
O6 C14 1.271(4) . ?
C1 C2 1.504(4) . ?
C2 C3 1.404(5) . ?
C3 C4 1.386(5) . ?
C4 C5 1.500(4) . ?
C6 C7 1.483(5) . ?
C7 C8 1.398(4) . ?
C8 C9 1.388(5) . ?
C9 C10 1.504(4) . ?
C11 C12 1.513(5) . ?
C12 C13 1.383(5) . ?
C13 C14 1.398(5) . ?
C14 C15 1.498(5) . ?

loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O1 V1 O5 87.73(9) . . ?
O1 V1 O6 92.62(10) . . ?
O2 V1 O1 87.52(9) . . ?
O2 V1 O5 174.36(10) . . ?
O2 V1 O6 89.87(10) . . ?
O3 V1 O1 91.09(10) . . ?
O3 V1 O2 93.33(10) . . ?
O3 V1 O5 89.81(10) . . ?
O3 V1 O6 175.19(9) . . ?
O4 V1 O1 178.37(9) . . ?
O4 V1 O2 91.03(10) . . ?
O4 V1 O3 88.26(10) . . ?
O4 V1 O5 93.75(9) . . ?
O4 V1 O6 88.11(10) . . ?
O5 V1 O6 87.30(10) . . ?
C2 O1 V1 129.6(2) . . ?
C4 O2 V1 129.5(2) . . ?
C7 O3 V1 128.4(2) . . ?
C9 O4 V1 128.5(2) . . ?
C12 O5 V1 129.0(2) . . ?
C14 O6 V1 129.2(2) . . ?
O1 C2 C1 115.4(3) . . ?
O1 C2 C3 124.0(3) . . ?
C3 C2 C1 120.6(3) . . ?
C4 C3 C2 124.4(3) . . ?
O2 C4 C3 124.3(3) . . ?
O2 C4 C5 116.0(3) . . ?
C3 C4 C5 119.7(3) . . ?
O3 C7 C6 116.1(3) . . ?
O3 C7 C8 124.8(3) . . ?
C8 C7 C6 119.1(3) . . ?
C9 C8 C7 124.2(3) . . ?
O4 C9 C8 124.7(3) . . ?
O4 C9 C10 116.2(3) . . ?
C8 C9 C10 119.1(3) . . ?
O5 C12 C11 114.8(3) . . ?
O5 C12 C13 125.3(3) . . ?
C13 C12 C11 119.8(3) . . ?
C12 C13 C14 124.3(3) . . ?
O6 C14 C13 124.4(3) . . ?
O6 C14 C15 115.4(3) . . ?
C13 C14 C15 120.3(3) . . ?

_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
loop_
_twin_individual_id
_twin_individual_mass_fraction_refined
1 0.565(2)
2 0.435(2)

_exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: THF'
