# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013


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# 
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#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
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data_SB10VO1
_database_code_depnum_ccdc_archive 'CCDC 926559'
#TrackingRef 'SB10VO1.cif'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         'C30 H36 N4 O10 V2'
_chemical_formula_sum            'C30 H36 N4 O10 V2'
_chemical_formula_weight         714.51
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           triclinic
_symmetry_space_group_name_H-M   'P -1'
_symmetry_space_group_name_Hall  '-P 1'
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, -z'
_cell_length_a                   8.8519(5)
_cell_length_b                   9.8955(6)
_cell_length_c                   10.3659(6)
_cell_angle_alpha                78.910(3)
_cell_angle_beta                 68.375(3)
_cell_angle_gamma                65.880(3)
_cell_volume                     769.45(8)
_cell_formula_units_Z            1
_cell_measurement_temperature    150(2)
_cell_measurement_reflns_used    8472
_cell_measurement_theta_min      2.26
_cell_measurement_theta_max      33.31
_exptl_crystal_description       prism
_exptl_crystal_colour            red
_exptl_crystal_size_max          0.38
_exptl_crystal_size_mid          0.25
_exptl_crystal_size_min          0.21
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    1.542
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             370
_exptl_absorpt_coefficient_mu    0.672
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.7843
_exptl_absorpt_correction_T_max  0.8718
_exptl_absorpt_process_details   sadabs
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      150(2)
_diffrn_radiation_wavelength     0.71069
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Bruker APEX-II CCD'
_diffrn_measurement_method       '\f and \w scans'
_diffrn_detector_area_resol_mean ?
_diffrn_standards_number         ?
_diffrn_standards_interval_count ?
_diffrn_standards_interval_time  ?
_diffrn_standards_decay_%        ?
_diffrn_reflns_number            13491
_diffrn_reflns_av_R_equivalents  0.0361
_diffrn_reflns_av_sigmaI/netI    0.0251
_diffrn_reflns_limit_h_min       -10
_diffrn_reflns_limit_h_max       9
_diffrn_reflns_limit_k_min       -11
_diffrn_reflns_limit_k_max       11
_diffrn_reflns_limit_l_min       -12
_diffrn_reflns_limit_l_max       12
_diffrn_reflns_theta_min         2.66
_diffrn_reflns_theta_max         25.34
_reflns_number_total             2794
_reflns_number_gt                2582
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       'Bruker APEX2'
_computing_cell_refinement       'Bruker SAINT'
_computing_data_reduction        'Bruker SAINT'
_computing_structure_solution    'SHELXS-97 (Sheldrick, 2008)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 2008)'
_computing_molecular_graphics    'Bruker SHELXTL'
_computing_publication_material  'Bruker SHELXTL'
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness 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 threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) 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
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0530P)^2^+0.9981P] 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    mixed
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         2794
_refine_ls_number_parameters     213
_refine_ls_number_restraints     7
_refine_ls_R_factor_all          0.0410
_refine_ls_R_factor_gt           0.0382
_refine_ls_wR_factor_ref         0.1042
_refine_ls_wR_factor_gt          0.1024
_refine_ls_goodness_of_fit_ref   1.062
_refine_ls_restrained_S_all      1.081
_refine_ls_shift/su_max          0.000
_refine_ls_shift/su_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_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
C1 C 0.5705(3) 0.2982(3) 0.6977(3) 0.0217(5) Uani 1 1 d . . .
C2 C 0.6572(3) 0.3538(3) 0.7497(3) 0.0255(6) Uani 1 1 d . . .
H2 H 0.6339 0.3508 0.8471 0.031 Uiso 1 1 calc R . .
C3 C 0.7773(3) 0.4136(3) 0.6591(3) 0.0246(5) Uani 1 1 d . . .
H3 H 0.8363 0.4508 0.6952 0.030 Uiso 1 1 calc R . .
C4 C 0.8123(3) 0.4198(3) 0.5170(3) 0.0232(5) Uani 1 1 d . . .
H4 H 0.8947 0.4610 0.4558 0.028 Uiso 1 1 calc R . .
C5 C 0.7267(3) 0.3659(3) 0.4651(3) 0.0206(5) Uani 1 1 d . . .
H5 H 0.7515 0.3695 0.3675 0.025 Uiso 1 1 calc R . .
C6 C 0.6037(3) 0.3057(2) 0.5533(2) 0.0169(5) Uani 1 1 d . . .
C7 C 0.5204(3) 0.2476(2) 0.4938(2) 0.0166(5) Uani 1 1 d . . .
H7 H 0.5603 0.2413 0.3958 0.020 Uiso 1 1 calc R . .
C11 C 0.1909(3) 0.1210(2) 0.5854(2) 0.0159(5) Uani 1 1 d . . .
C12 C 0.0934(3) 0.0599(2) 0.5398(2) 0.0148(5) Uani 1 1 d . . .
C13 C -0.0385(3) 0.0177(3) 0.6393(2) 0.0178(5) Uani 1 1 d . . .
H13 H -0.0651 0.0299 0.7349 0.021 Uiso 1 1 calc R . .
C14 C -0.1302(3) -0.0414(3) 0.6001(2) 0.0185(5) Uani 1 1 d . . .
H14 H -0.2195 -0.0699 0.6689 0.022 Uiso 1 1 calc R . .
C21 C 0.5073(3) -0.1186(3) 0.8863(3) 0.0261(6) Uani 1 1 d . . .
H21A H 0.4105 -0.1077 0.9756 0.031 Uiso 1 1 calc R . .
H21B H 0.5838 -0.0723 0.8938 0.031 Uiso 1 1 calc R . .
C22 C 0.6111(4) -0.2809(3) 0.8623(3) 0.0305(6) Uani 1 1 d . . .
H22A H 0.5357 -0.3277 0.8560 0.046 Uiso 1 1 calc R . .
H22B H 0.6558 -0.3283 0.9399 0.046 Uiso 1 1 calc R . .
H22C H 0.7094 -0.2925 0.7756 0.046 Uiso 1 1 calc R . .
C31 C 0.0193(3) 0.2581(3) 1.0632(3) 0.0298(6) Uani 1 1 d . . .
H31A H 0.0033 0.3638 1.0391 0.036 Uiso 1 1 calc R . .
H31B H 0.0344 0.2330 1.1559 0.036 Uiso 1 1 calc R . .
C32 C -0.1400(5) 0.2347(4) 1.0679(4) 0.0511(9) Uani 1 1 d U . .
H32A H -0.1564 0.2617 0.9766 0.077 Uiso 1 1 calc R . .
H32B H -0.2430 0.2969 1.1377 0.077 Uiso 1 1 calc R . .
H32C H -0.1245 0.1303 1.0924 0.077 Uiso 1 1 calc R . .
N1 N 0.3935(2) 0.2034(2) 0.56762(19) 0.0149(4) Uani 1 1 d . . .
N2 N 0.3264(2) 0.1479(2) 0.4957(2) 0.0161(4) Uani 1 1 d . . .
O1 O 0.4679(2) 0.2279(2) 0.78646(18) 0.0270(4) Uani 1 1 d . . .
O2 O 0.1377(2) 0.14347(18) 0.71730(16) 0.0182(4) Uani 1 1 d . . .
O10 O 0.1480(3) 0.3896(2) 0.77951(19) 0.0297(4) Uani 1 1 d . . .
O20 O 0.4354(2) -0.0413(2) 0.77623(18) 0.0237(4) Uani 1 1 d D . .
O30 O 0.1713(2) 0.1683(2) 0.96310(17) 0.0235(4) Uani 1 1 d . . .
V1 V 0.26484(5) 0.21716(4) 0.78627(4) 0.01667(15) Uani 1 1 d . . .
H20 H 0.523(3) -0.066(3) 0.687(2) 0.025 Uiso 1 1 d D . .
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
C1 0.0194(12) 0.0256(13) 0.0219(12) -0.0039(10) -0.0039(10) -0.0113(10)
C2 0.0260(13) 0.0319(14) 0.0236(13) -0.0086(11) -0.0066(10) -0.0138(11)
C3 0.0226(12) 0.0228(13) 0.0343(15) -0.0055(11) -0.0105(11) -0.0111(10)
C4 0.0201(12) 0.0193(12) 0.0328(14) 0.0025(10) -0.0090(11) -0.0109(10)
C5 0.0206(12) 0.0189(12) 0.0215(12) 0.0026(9) -0.0065(10) -0.0085(9)
C6 0.0144(11) 0.0153(11) 0.0202(12) -0.0022(9) -0.0053(9) -0.0045(9)
C7 0.0172(11) 0.0170(11) 0.0143(11) -0.0004(9) -0.0047(9) -0.0057(9)
C11 0.0160(11) 0.0153(11) 0.0165(11) -0.0013(9) -0.0068(9) -0.0043(9)
C12 0.0140(11) 0.0138(11) 0.0170(11) -0.0022(9) -0.0069(9) -0.0031(9)
C13 0.0184(11) 0.0218(12) 0.0136(11) -0.0029(9) -0.0057(9) -0.0065(9)
C14 0.0175(11) 0.0234(12) 0.0158(11) -0.0016(9) -0.0037(9) -0.0099(10)
C21 0.0290(13) 0.0300(14) 0.0205(13) -0.0015(10) -0.0084(11) -0.0116(11)
C22 0.0327(15) 0.0286(14) 0.0292(14) 0.0003(11) -0.0106(12) -0.0108(12)
C31 0.0284(14) 0.0375(15) 0.0166(12) -0.0030(11) -0.0011(11) -0.0100(12)
C32 0.0462(12) 0.0595(12) 0.0482(12) -0.0034(9) -0.0169(9) -0.0184(9)
N1 0.0178(10) 0.0167(9) 0.0140(9) -0.0005(7) -0.0071(8) -0.0085(8)
N2 0.0177(10) 0.0205(10) 0.0146(9) -0.0027(8) -0.0072(8) -0.0088(8)
O1 0.0326(10) 0.0398(11) 0.0192(9) 0.0012(8) -0.0083(8) -0.0249(9)
O2 0.0188(8) 0.0264(9) 0.0133(8) -0.0031(7) -0.0046(6) -0.0117(7)
O10 0.0378(11) 0.0275(10) 0.0234(9) -0.0039(8) -0.0085(8) -0.0116(8)
O20 0.0231(9) 0.0282(9) 0.0187(9) -0.0009(7) -0.0059(7) -0.0095(7)
O30 0.0245(9) 0.0303(10) 0.0176(9) -0.0039(7) -0.0038(7) -0.0132(8)
V1 0.0202(2) 0.0225(2) 0.0115(2) -0.00175(15) -0.00409(16) -0.01238(17)
_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
C1 O1 1.345(3) . ?
C1 C2 1.395(3) . ?
C1 C6 1.408(3) . ?
C2 C3 1.388(4) . ?
C2 H2 0.9500 . ?
C3 C4 1.384(4) . ?
C3 H3 0.9500 . ?
C4 C5 1.374(3) . ?
C4 H4 0.9500 . ?
C5 C6 1.401(3) . ?
C5 H5 0.9500 . ?
C6 C7 1.440(3) . ?
C7 N1 1.295(3) . ?
C7 H7 0.9500 . ?
C11 O2 1.302(3) . ?
C11 N2 1.310(3) . ?
C11 C12 1.474(3) . ?
C12 C13 1.395(3) . ?
C12 C14 1.396(3) 2_556 ?
C13 C14 1.374(3) . ?
C13 H13 0.9500 . ?
C14 C12 1.396(3) 2_556 ?
C14 H14 0.9500 . ?
C21 O20 1.447(3) . ?
C21 C22 1.505(4) . ?
C21 H21A 0.9900 . ?
C21 H21B 0.9900 . ?
C22 H22A 0.9800 . ?
C22 H22B 0.9800 . ?
C22 H22C 0.9800 . ?
C31 O30 1.423(3) . ?
C31 C32 1.502(4) . ?
C31 H31A 0.9900 . ?
C31 H31B 0.9900 . ?
C32 H32A 0.9800 . ?
C32 H32B 0.9800 . ?
C32 H32C 0.9800 . ?
N1 N2 1.401(3) . ?
N1 V1 2.1313(19) . ?
O1 V1 1.8441(18) . ?
O2 V1 1.9426(16) . ?
O10 V1 1.5975(19) . ?
O20 V1 2.3797(18) . ?
O20 H20 0.955(18) . ?
O30 V1 1.7738(17) . ?
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 C1 C2 118.7(2) . . ?
O1 C1 C6 121.6(2) . . ?
C2 C1 C6 119.5(2) . . ?
C3 C2 C1 120.0(2) . . ?
C3 C2 H2 120.0 . . ?
C1 C2 H2 120.0 . . ?
C4 C3 C2 120.9(2) . . ?
C4 C3 H3 119.5 . . ?
C2 C3 H3 119.5 . . ?
C5 C4 C3 119.4(2) . . ?
C5 C4 H4 120.3 . . ?
C3 C4 H4 120.3 . . ?
C4 C5 C6 121.3(2) . . ?
C4 C5 H5 119.3 . . ?
C6 C5 H5 119.3 . . ?
C5 C6 C1 118.9(2) . . ?
C5 C6 C7 119.2(2) . . ?
C1 C6 C7 121.8(2) . . ?
N1 C7 C6 123.1(2) . . ?
N1 C7 H7 118.5 . . ?
C6 C7 H7 118.5 . . ?
O2 C11 N2 122.8(2) . . ?
O2 C11 C12 116.9(2) . . ?
N2 C11 C12 120.3(2) . . ?
C13 C12 C14 118.8(2) . 2_556 ?
C13 C12 C11 119.2(2) . . ?
C14 C12 C11 122.0(2) 2_556 . ?
C14 C13 C12 120.5(2) . . ?
C14 C13 H13 119.7 . . ?
C12 C13 H13 119.7 . . ?
C13 C14 C12 120.6(2) . 2_556 ?
C13 C14 H14 119.7 . . ?
C12 C14 H14 119.7 2_556 . ?
O20 C21 C22 112.6(2) . . ?
O20 C21 H21A 109.1 . . ?
C22 C21 H21A 109.1 . . ?
O20 C21 H21B 109.1 . . ?
C22 C21 H21B 109.1 . . ?
H21A C21 H21B 107.8 . . ?
C21 C22 H22A 109.5 . . ?
C21 C22 H22B 109.5 . . ?
H22A C22 H22B 109.5 . . ?
C21 C22 H22C 109.5 . . ?
H22A C22 H22C 109.5 . . ?
H22B C22 H22C 109.5 . . ?
O30 C31 C32 110.7(2) . . ?
O30 C31 H31A 109.5 . . ?
C32 C31 H31A 109.5 . . ?
O30 C31 H31B 109.5 . . ?
C32 C31 H31B 109.5 . . ?
H31A C31 H31B 108.1 . . ?
C31 C32 H32A 109.5 . . ?
C31 C32 H32B 109.5 . . ?
H32A C32 H32B 109.5 . . ?
C31 C32 H32C 109.5 . . ?
H32A C32 H32C 109.5 . . ?
H32B C32 H32C 109.5 . . ?
C7 N1 N2 116.80(19) . . ?
C7 N1 V1 127.13(15) . . ?
N2 N1 V1 115.97(13) . . ?
C11 N2 N1 107.92(18) . . ?
C1 O1 V1 131.00(16) . . ?
C11 O2 V1 119.24(14) . . ?
C21 O20 V1 120.09(14) . . ?
C21 O20 H20 110.7(17) . . ?
V1 O20 H20 111.6(17) . . ?
C31 O30 V1 127.67(17) . . ?
O10 V1 O30 100.96(9) . . ?
O10 V1 O1 100.10(9) . . ?
O30 V1 O1 101.92(8) . . ?
O10 V1 O2 97.99(9) . . ?
O30 V1 O2 94.84(7) . . ?
O1 V1 O2 152.42(8) . . ?
O10 V1 N1 95.18(8) . . ?
O30 V1 N1 161.59(8) . . ?
O1 V1 N1 83.70(7) . . ?
O2 V1 N1 74.06(7) . . ?
O10 V1 O20 174.57(8) . . ?
O30 V1 O20 82.90(7) . . ?
O1 V1 O20 82.68(8) . . ?
O2 V1 O20 77.79(7) . . ?
N1 V1 O20 80.44(7) . . ?
loop_
_geom_hbond_atom_site_label_D
_geom_hbond_atom_site_label_H
_geom_hbond_atom_site_label_A
_geom_hbond_distance_DH
_geom_hbond_distance_HA
_geom_hbond_distance_DA
_geom_hbond_angle_DHA
_geom_hbond_site_symmetry_A
O20 H20 N2 0.955(18) 1.971(19) 2.907(3) 166(3) 2_656
_diffrn_measured_fraction_theta_max 0.992
_diffrn_reflns_theta_full        25.34
_diffrn_measured_fraction_theta_full 0.992
_refine_diff_density_max         0.920
_refine_diff_density_min         -0.541
_refine_diff_density_rms         0.069