Supplementary Material (ESI) for Dalton Transactions
This journal is (c) The Royal Society of Chemistry 2001


data_dc36sad 

_database_code_CSD         157280

_journal_coden_Cambridge      186

_audit_creation_method      SHELXL 
_chemical_name_systematic   'Bis(N,N'-dimethylacetylacetamido)oxovanadium(IV)'
_chemical_name_common       VO(acac-NMe2)2 
_chemical_formula_sum       'C18 H26 N2 O5 V' 
_chemical_formula_weight    401.35 

_publ_requested_journal     'J.Chem.Soc., Dalton Trans'


_publ_contact_author_name     	'Prof Debbie C Crans' 
_publ_contact_author_address 
;
Prof Debbie C Crans
Department of Chemistry
Colorado State University
Fort Collins
Colorado 80523-1872
UNITED STATES OF AMERICA
;
_publ_contact_author_email       'crans@lamar.colostate.edu'

_publ_section_title
;
Bis(actylamido)oxovanadium(IV) complexes: Solid state and Solution Studies.
;

loop_
_publ_author_name
'Anderson, Oren P.'
'Crans, Debbie C.'
'Jakusch, Tamas'
'Khan, A. Raza'
'Kiss, Tamas'
'la Cour, Agnete'
'Mahroof-Tahir, Mohammed'
'Miller, Susie M.'
'Mondal, Sujit'

_abstract
;
VO(acac-NME2)2 exists as a discrete mononulear complex with the vanadium'
atom in a distorted square pyramidal coordination environment. Two oxygen 
atoms of each of the NMe2-acac- ligands (V-O = 1.976(2), 1.958(2), 1.958(2) 
1.966(2) A) coordinate to the vanadium atom in the equatorial plane.  The oxo 
group (V-O = 1.597(2) A) occupies the apical position and the vanadium atom 
lies 0.59 A above the least-aquares equatorial plane.'
;

loop_ 
_atom_type_symbol 
_atom_type_description 
_atom_type_scat_dispersion_real 
_atom_type_scat_dispersion_imag 
_atom_type_scat_source 
'C'  'C'   0.0033   0.0016 
'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' 
'N'  'N'   0.0061   0.0033 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'O'  'O'   0.0106   0.0060 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 
'V'  'V'   0.3005   0.5294 
'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 

_symmetry_cell_setting            Monoclinic 
_symmetry_space_group_name_H-M    P2(1)/n 

loop_ 
_symmetry_equiv_pos_as_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                    7.005(2) 
_cell_length_b                    19.610(6) 
_cell_length_c                    14.601(4) 
_cell_angle_alpha                 90.00 
_cell_angle_beta                  90.19(2) 
_cell_angle_gamma                 90.00 
_cell_volume                      2005.5(10) 
_cell_formula_units_Z             4 
_cell_measurement_temperature     166(2) 
_cell_measurement_reflns_used     ? 
_cell_measurement_theta_min       ? 
_cell_measurement_theta_max       ? 

_exptl_crystal_description        'prismatic shape' 
_exptl_crystal_colour             blue 
_exptl_crystal_size_max           0.75 
_exptl_crystal_size_mid           0.42 
_exptl_crystal_size_min           0.30 
_exptl_crystal_density_meas       none 
_exptl_crystal_density_diffrn     1.329 
_exptl_crystal_density_method     none 
_exptl_crystal_F_000              844 
_exptl_absorpt_coefficient_mu     0.524 
_exptl_absorpt_correction_type    SADABS 
_exptl_absorpt_correction_T_min   0.68 
_exptl_absorpt_correction_T_max   0.98
_exptl_special_details            ? 

_diffrn_ambient_temperature       166(2) 
_diffrn_radiation_wavelength      0.71073 
_diffrn_radiation_type            MoK\a 
_diffrn_radiation_source          'fine-focus sealed tube' 
_diffrn_radiation_monochromator   'graphite' 
_diffrn_measurement_device        'Bruker AXS SMART CCD area detector' 
_diffrn_reflns_number             10311 
_diffrn_reflns_av_R_equivalents   0.0353 
_diffrn_reflns_av_sigmaI/netI     0.0547 
_diffrn_reflns_limit_h_min        -9 
_diffrn_reflns_limit_h_max        7 
_diffrn_reflns_limit_k_min        -25 
_diffrn_reflns_limit_k_max        19 
_diffrn_reflns_limit_l_min        -11 
_diffrn_reflns_limit_l_max        19 
_diffrn_reflns_theta_min          1.74 
_diffrn_reflns_theta_max          28.65 
_reflns_number_total              4767 
_reflns_number_observed           3445 
_reflns_observed_criterion        >2sigma(I) 

_computing_data_collection        'SMART, Bruker' 
_computing_cell_refinement        'SMART, Bruker' 
_computing_data_reduction         'SAINT, Bruker' 
_computing_structure_solution     'SHELXS-86 (Sheldrick, 1990)' 
_computing_structure_refinement   'SHELXL-93 (Sheldrick, 1993)' 
_computing_molecular_graphics     SHELXTL 
_computing_publication_material   SHELXTL 

_refine_special_details 
; 
Refinement on F^2^ for ALL reflections except for 1 with very negative F^2^ 
or flagged by the user for potential systematic errors.  Weighted R-factors 
wR and all goodnesses of fit S are based on F^2^, conventional R-factors R 
are based on F, with F set to zero for negative F^2^. The observed criterion 
of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is 
not relevant to the choice of reflections for refinement.  R-factors based 
on F^2^ are statistically about twice as large as those based on F, and R- 
factors based on ALL data will be even larger. 
; 

_refine_ls_structure_factor_coef  Fsqd  
_refine_ls_matrix_type            full 
_refine_ls_weighting_scheme 
'calc w=1/[\s^2^(Fo^2^)+(0.0924P)^2^+1.7875P] where P=(Fo^2^+2Fc^2^)/3' 
_atom_sites_solution_primary      direct 
_atom_sites_solution_secondary    difmap 
_atom_sites_solution_hydrogens    geom 
_refine_ls_hydrogen_treatment     'riding model used in refinement' 
_refine_ls_extinction_method      none 
_refine_ls_extinction_coef        none 
_refine_ls_number_reflns          4766 
_refine_ls_number_parameters      235 
_refine_ls_number_restraints      0 
_refine_ls_R_factor_all           0.0887 
_refine_ls_R_factor_obs           0.0613 
_refine_ls_wR_factor_all          0.1823 
_refine_ls_wR_factor_obs          0.1604 
_refine_ls_goodness_of_fit_all    1.040 
_refine_ls_goodness_of_fit_obs    1.093 
_refine_ls_restrained_S_all       1.050 
_refine_ls_restrained_S_obs       1.093 
_refine_ls_shift/esd_max          -0.001 
_refine_ls_shift/esd_mean         0.000 

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_thermal_displace_type 
_atom_site_occupancy 
_atom_site_calc_flag 
_atom_site_refinement_flags 
_atom_site_disorder_group 
V V 0.28806(7) 0.59281(3) 0.25003(3) 0.0261(2) Uani 1 d . . 
C1 C 0.5059(4) 0.59174(15) 0.0757(2) 0.0276(6) Uani 1 d . . 
O1 O 0.1638(3) 0.52455(12) 0.2499(2) 0.0368(5) Uani 1 d . . 
N1 N 0.6637(4) 0.56933(15) 0.0315(2) 0.0344(6) Uani 1 d . . 
N2 N 0.6635(4) 0.56922(15) 0.4689(2) 0.0337(6) Uani 1 d . . 
C2 C 0.3599(4) 0.6281(2) 0.0278(2) 0.0309(7) Uani 1 d . . 
H2A H 0.3657(4) 0.6311(2) -0.0371(2) 0.037 Uiso 1 calc R . 
O2 O 0.4981(3) 0.58002(11) 0.16165(15) 0.0310(5) Uani 1 d . . 
O3 O 0.1750(3) 0.65485(12) 0.1599(2) 0.0349(5) Uani 1 d . . 
C3 C 0.2105(4) 0.6590(2) 0.0730(2) 0.0309(7) Uani 1 d . . 
O4 O 0.1756(3) 0.65492(12) 0.3400(2) 0.0348(5) Uani 1 d . . 
C4 C 0.0730(6) 0.7038(2) 0.0210(3) 0.0452(9) Uani 1 d . . 
H4A H -0.0237(6) 0.7216(2) 0.0631(3) 0.068 Uiso 1 calc R . 
H4B H 0.0106(6) 0.6771(2) -0.0273(3) 0.068 Uiso 1 calc R . 
H4C H 0.1427(6) 0.7419(2) -0.0066(3) 0.068 Uiso 1 calc R . 
O5 O 0.4978(3) 0.57984(11) 0.33812(14) 0.0301(5) Uani 1 d . . 
C5 C 0.8167(5) 0.5368(2) 0.0837(2) 0.0390(8) Uani 1 d . . 
H5A H 0.9198(5) 0.5236(2) 0.0421(2) 0.059 Uiso 1 calc R . 
H5B H 0.7669(5) 0.4961(2) 0.1145(2) 0.059 Uiso 1 calc R . 
H5C H 0.8660(5) 0.5688(2) 0.1295(2) 0.059 Uiso 1 calc R . 
C6 C 0.6890(5) 0.5762(2) -0.0675(2) 0.0427(8) Uani 1 d . . 
H6A H 0.8124(5) 0.5567(2) -0.0851(2) 0.064 Uiso 1 calc R . 
H6B H 0.6853(5) 0.6245(2) -0.0843(2) 0.064 Uiso 1 calc R . 
H6C H 0.5862(5) 0.5519(2) -0.0993(2) 0.064 Uiso 1 calc R . 
C7 C 0.5060(4) 0.59170(15) 0.4245(2) 0.0274(6) Uani 1 d . . 
C8 C 0.3595(4) 0.6285(2) 0.4728(2) 0.0313(7) Uani 1 d . . 
H8A H 0.3661(4) 0.6317(2) 0.5376(2) 0.038 Uiso 1 calc R . 
C9 C 0.2106(4) 0.6590(2) 0.4271(2) 0.0306(7) Uani 1 d . . 
C10 C 0.0721(6) 0.7034(2) 0.4792(3) 0.0454(9) Uani 1 d . . 
H10A H -0.0249(6) 0.7211(2) 0.4369(3) 0.068 Uiso 1 calc R . 
H10B H 0.1412(6) 0.7415(2) 0.5073(3) 0.068 Uiso 1 calc R . 
H10C H 0.0101(6) 0.6763(2) 0.5270(3) 0.068 Uiso 1 calc R . 
C11 C 0.8173(5) 0.5367(2) 0.4165(2) 0.0400(8) Uani 1 d . . 
H11A H 0.9206(5) 0.5234(2) 0.4582(2) 0.060 Uiso 1 calc R . 
H11B H 0.8665(5) 0.5689(2) 0.3710(2) 0.060 Uiso 1 calc R . 
H11C H 0.7675(5) 0.4962(2) 0.3853(2) 0.060 Uiso 1 calc R . 
C12 C 0.6881(6) 0.5763(2) 0.5676(2) 0.0433(8) Uani 1 d . . 
H12A H 0.8113(6) 0.5568(2) 0.5858(2) 0.065 Uiso 1 calc R . 
H12B H 0.5850(6) 0.5521(2) 0.5991(2) 0.065 Uiso 1 calc R . 
H12C H 0.6845(6) 0.6247(2) 0.5842(2) 0.065 Uiso 1 calc R . 
C20 C 0.8407(11) 0.2485(3) 0.2501(4) 0.085(2) Uani 1 d . . 
H20A H 0.8684(11) 0.2011(3) 0.2499(4) 0.102 Uiso 1 calc R . 
C21 C 0.9878(8) 0.2963(5) 0.2501(4) 0.102(2) Uani 1 d . . 
H21A H 1.1175(8) 0.2821(5) 0.2504(4) 0.122 Uiso 1 calc R . 
C22 C 0.9417(15) 0.3639(5) 0.2497(4) 0.119(4) Uani 1 d . . 
H22A H 1.0397(15) 0.3974(5) 0.2495(4) 0.143 Uiso 1 calc R . 
C23 C 0.7630(18) 0.3825(3) 0.2497(4) 0.108(3) Uani 1 d . . 
H23A H 0.7325(18) 0.4297(3) 0.2492(4) 0.130 Uiso 1 calc R . 
C24 C 0.6244(10) 0.3377(4) 0.2503(4) 0.090(2) Uani 1 d . . 
H24A H 0.4960(10) 0.3532(4) 0.2508(4) 0.107 Uiso 1 calc R . 
C25 C 0.6589(9) 0.2704(3) 0.2503(3) 0.076(2) Uani 1 d . . 
H25A H 0.5563(9) 0.2388(3) 0.2505(3) 0.092 Uiso 1 calc R . 

loop_ 
_atom_site_aniso_label 
_atom_site_aniso_U_11 
_atom_site_aniso_U_22 
_atom_site_aniso_U_33 
_atom_site_aniso_U_23 
_atom_site_aniso_U_13 
_atom_site_aniso_U_12 
V 0.0233(3) 0.0324(3) 0.0225(3) -0.0004(2) 0.0001(2) 0.0014(2) 
C1 0.0262(14) 0.0284(14) 0.028(2) -0.0021(12) 0.0018(11) -0.0040(11) 
O1 0.0334(12) 0.0420(13) 0.0351(13) -0.0012(10) -0.0005(10) -0.0052(9) 
N1 0.0329(14) 0.044(2) 0.0266(14) -0.0033(12) 0.0045(10) 0.0014(11) 
N2 0.0331(14) 0.042(2) 0.0258(14) 0.0022(11) -0.0045(10) 0.0002(11) 
C2 0.034(2) 0.036(2) 0.0222(15) 0.0010(12) -0.0016(12) -0.0042(12) 
O2 0.0263(10) 0.0427(13) 0.0241(11) 0.0021(9) 0.0014(8) 0.0040(8) 
O3 0.0342(12) 0.0423(13) 0.0280(12) 0.0026(9) -0.0004(9) 0.0094(9) 
C3 0.032(2) 0.032(2) 0.028(2) 0.0024(12) -0.0050(12) -0.0027(12) 
O4 0.0334(12) 0.0439(14) 0.0271(12) -0.0032(10) -0.0001(9) 0.0100(9) 
C4 0.046(2) 0.052(2) 0.037(2) 0.005(2) -0.008(2) 0.012(2) 
O5 0.0268(10) 0.0420(12) 0.0216(10) -0.0015(9) -0.0012(8) 0.0046(8) 
C5 0.030(2) 0.051(2) 0.036(2) -0.003(2) 0.0054(13) 0.0071(14) 
C6 0.043(2) 0.057(2) 0.028(2) 0.000(2) 0.0105(14) 0.002(2) 
C7 0.0286(14) 0.0280(14) 0.0255(15) 0.0024(12) -0.0010(11) -0.0048(11) 
C8 0.034(2) 0.036(2) 0.024(2) -0.0011(13) 0.0007(12) -0.0022(12) 
C9 0.033(2) 0.030(2) 0.028(2) -0.0054(12) 0.0050(12) -0.0028(12) 
C10 0.049(2) 0.050(2) 0.037(2) -0.007(2) 0.007(2) 0.009(2) 
C11 0.032(2) 0.051(2) 0.037(2) 0.001(2) -0.0034(13) 0.0080(14) 
C12 0.047(2) 0.055(2) 0.028(2) 0.001(2) -0.0080(14) 0.001(2) 
C20 0.148(6) 0.052(3) 0.056(3) 0.000(3) 0.004(3) 0.025(3) 
C21 0.044(3) 0.212(9) 0.050(3) 0.002(5) 0.003(2) -0.002(4) 
C22 0.176(8) 0.146(7) 0.035(3) -0.006(4) 0.008(4) -0.125(7) 
C23 0.237(10) 0.048(3) 0.040(3) 0.005(3) 0.007(5) 0.004(5) 
C24 0.086(4) 0.144(6) 0.039(3) 0.005(4) 0.006(2) 0.054(4) 
C25 0.077(4) 0.106(5) 0.047(3) 0.000(3) 0.002(2) -0.051(3) 

_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 
V O1 1.597(2) . ? 
V O3 1.958(2) . ? 
V O4 1.958(2) . ? 
V O5 1.966(2) . ? 
V O2 1.976(2) . ? 
C1 O2 1.278(4) . ? 
C1 N1 1.355(4) . ? 
C1 C2 1.427(4) . ? 
N1 C5 1.460(4) . ? 
N1 C6 1.462(4) . ? 
N2 C7 1.351(4) . ? 
N2 C12 1.457(4) . ? 
N2 C11 1.469(4) . ? 
C2 C3 1.379(4) . ? 
O3 C3 1.296(4) . ? 
C3 C4 1.507(5) . ? 
O4 C9 1.297(4) . ? 
O5 C7 1.284(4) . ? 
C7 C8 1.440(4) . ? 
C8 C9 1.373(5) . ? 
C9 C10 1.511(4) . ? 
C20 C25 1.344(9) . ? 
C20 C21 1.393(10) . ? 
C21 C22 1.365(12) . ? 
C22 C23 1.304(12) . ? 
C23 C24 1.310(11) . ? 
C24 C25 1.340(9) . ? 

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 V O3 107.52(11) . . ? 
O1 V O4 107.54(11) . . ? 
O3 V O4 84.35(10) . . ? 
O1 V O5 107.36(11) . . ? 
O3 V O5 145.08(10) . . ? 
O4 V O5 86.75(9) . . ? 
O1 V O2 107.48(11) . . ? 
O3 V O2 86.57(9) . . ? 
O4 V O2 144.96(10) . . ? 
O5 V O2 81.63(9) . . ? 
O2 C1 N1 116.6(3) . . ? 
O2 C1 C2 122.5(3) . . ? 
N1 C1 C2 120.9(3) . . ? 
C1 N1 C5 119.5(3) . . ? 
C1 N1 C6 122.9(3) . . ? 
C5 N1 C6 117.7(3) . . ? 
C7 N2 C12 122.5(3) . . ? 
C7 N2 C11 119.4(3) . . ? 
C12 N2 C11 118.1(3) . . ? 
C3 C2 C1 121.9(3) . . ? 
C1 O2 V 130.8(2) . . ? 
C3 O3 V 128.2(2) . . ? 
O3 C3 C2 126.1(3) . . ? 
O3 C3 C4 113.9(3) . . ? 
C2 C3 C4 120.0(3) . . ? 
C9 O4 V 128.3(2) . . ? 
C7 O5 V 130.6(2) . . ? 
O5 C7 N2 116.5(3) . . ? 
O5 C7 C8 122.8(3) . . ? 
N2 C7 C8 120.7(3) . . ? 
C9 C8 C7 121.4(3) . . ? 
O4 C9 C8 126.2(3) . . ? 
O4 C9 C10 114.1(3) . . ? 
C8 C9 C10 119.6(3) . . ? 
C25 C20 C21 119.0(6) . . ? 
C22 C21 C20 118.6(6) . . ? 
C23 C22 C21 120.0(6) . . ? 
C22 C23 C24 121.5(6) . . ? 
C23 C24 C25 121.8(6) . . ? 
C24 C25 C20 119.1(5) . . ? 

_refine_diff_density_max    0.501 
_refine_diff_density_min   -0.545 
_refine_diff_density_rms    0.080