# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name 'Lilia Reytman' 'Edit Tshuva' _publ_contact_author_name 'Dr Edit Tshuva' _publ_contact_author_email tshuva@chem.ch.huji.ac.il # Attachment '- cifs.cif' data_L1VO(OiPr) _database_code_depnum_ccdc_archive 'CCDC 838966' #TrackingRef '- cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C25 H37 N2 O4 V' _chemical_formula_sum 'C25 H37 N2 O4 V' _chemical_formula_weight 480.51 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 Hexagonal _symmetry_space_group_name_H-M R-3c _symmetry_space_group_name_Hall '-R 3 2"c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'y+2/3, x+1/3, -z+5/6' 'x-y+2/3, -y+1/3, -z+5/6' '-x+2/3, -x+y+1/3, -z+5/6' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' 'y+1/3, x+2/3, -z+7/6' 'x-y+1/3, -y+2/3, -z+7/6' '-x+1/3, -x+y+2/3, -z+7/6' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-y+2/3, -x+1/3, z-1/6' '-x+y+2/3, y+1/3, z-1/6' 'x+2/3, x-y+1/3, z-1/6' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' '-y+1/3, -x+2/3, z+1/6' '-x+y+1/3, y+2/3, z+1/6' 'x+1/3, x-y+2/3, z+1/6' _cell_length_a 19.8537(8) _cell_length_b 19.8537(8) _cell_length_c 67.448(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 23024(2) _cell_formula_units_Z 36 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description shapeless _exptl_crystal_colour 'dark purple' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.248 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9216 _exptl_absorpt_coefficient_mu 0.419 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.9209 _exptl_absorpt_correction_T_max 0.9713 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 82154 _diffrn_reflns_av_R_equivalents 0.1254 _diffrn_reflns_av_sigmaI/netI 0.0530 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -86 _diffrn_reflns_limit_l_max 86 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 27.00 _reflns_number_total 5590 _reflns_number_gt 4937 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0377P)^2^+128.6715P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5590 _refine_ls_number_parameters 326 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1314 _refine_ls_R_factor_gt 0.1157 _refine_ls_wR_factor_ref 0.1915 _refine_ls_wR_factor_gt 0.1853 _refine_ls_goodness_of_fit_ref 1.392 _refine_ls_restrained_S_all 1.392 _refine_ls_shift/su_max 0.001 _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 0.4963(2) 0.6587(2) 0.49493(6) 0.0282(9) Uani 1 1 d . . . C2 C 0.4152(2) 0.6095(2) 0.49364(6) 0.0285(9) Uani 1 1 d . . . C3 C 0.3814(3) 0.5902(2) 0.47501(7) 0.0357(11) Uani 1 1 d . . . H3 H 0.3265 0.5585 0.4741 0.043 Uiso 1 1 calc R . . C4 C 0.4241(3) 0.6150(3) 0.45783(7) 0.0366(11) Uani 1 1 d . . . C5 C 0.5039(3) 0.6616(3) 0.45936(7) 0.0347(11) Uani 1 1 d . . . H5 H 0.5342 0.6785 0.4476 0.042 Uiso 1 1 calc R . . C6 C 0.5413(3) 0.6846(2) 0.47764(7) 0.0301(10) Uani 1 1 d . . . C7 C 0.6283(3) 0.7352(3) 0.47831(7) 0.0383(11) Uani 1 1 d . . . H7A H 0.6498 0.7294 0.4656 0.046 Uiso 1 1 calc R . . H7B H 0.6412 0.7901 0.4793 0.046 Uiso 1 1 calc R . . C8 C 0.6501(3) 0.6367(3) 0.49386(7) 0.0373(11) Uani 1 1 d . . . H8A H 0.6822 0.6315 0.4834 0.045 Uiso 1 1 calc R . . H8B H 0.5947 0.6026 0.4903 0.045 Uiso 1 1 calc R . . C9 C 0.6663(3) 0.6109(3) 0.51351(7) 0.0366(11) Uani 1 1 d . . . H9A H 0.6527 0.5557 0.5126 0.044 Uiso 1 1 calc R . . H9B H 0.7224 0.6425 0.5166 0.044 Uiso 1 1 calc R . . C10 C 0.6515(3) 0.6198(3) 0.54939(8) 0.0421(12) Uani 1 1 d . . . H10A H 0.6444 0.5675 0.5519 0.051 Uiso 1 1 calc R . . H10B H 0.6205 0.6290 0.5594 0.051 Uiso 1 1 calc R . . C11 C 0.7355(3) 0.6789(3) 0.55226(7) 0.0376(11) Uani 1 1 d . . . C12 C 0.7818(3) 0.6598(3) 0.56365(7) 0.0431(12) Uani 1 1 d . . . H12 H 0.7593 0.6089 0.5691 0.052 Uiso 1 1 calc R . . C13 C 0.8590(3) 0.7116(3) 0.56732(8) 0.0514(14) Uani 1 1 d . . . C14 C 0.8909(3) 0.7842(3) 0.55872(9) 0.0573(16) Uani 1 1 d . . . H14 H 0.9445 0.8201 0.5608 0.069 Uiso 1 1 calc R . . C15 C 0.8482(3) 0.8071(3) 0.54720(9) 0.0501(14) Uani 1 1 d . . . C16 C 0.7690(3) 0.7541(3) 0.54422(7) 0.0403(12) Uani 1 1 d . . . C17 C 0.3682(2) 0.5783(3) 0.51220(7) 0.0361(11) Uani 1 1 d . . . H17A H 0.3768 0.6216 0.5208 0.054 Uiso 1 1 calc R . . H17B H 0.3841 0.5451 0.5191 0.054 Uiso 1 1 calc R . . H17C H 0.3129 0.5477 0.5088 0.054 Uiso 1 1 calc R . . C18 C 0.3851(3) 0.5904(3) 0.43790(7) 0.0520(14) Uani 1 1 d . . . H18A H 0.4165 0.5778 0.4291 0.078 Uiso 1 1 calc R . . H18B H 0.3800 0.6329 0.4321 0.078 Uiso 1 1 calc R . . H18C H 0.3334 0.5445 0.4395 0.078 Uiso 1 1 calc R . . C19 C 0.7526(3) 0.7721(3) 0.49206(8) 0.0478(13) Uani 1 1 d . . . H19A H 0.7814 0.7609 0.5021 0.072 Uiso 1 1 calc R . . H19B H 0.7644 0.8261 0.4935 0.072 Uiso 1 1 calc R . . H19C H 0.7679 0.7646 0.4788 0.072 Uiso 1 1 calc R . . C20 C 0.5392(3) 0.5532(3) 0.52923(9) 0.0444(13) Uani 1 1 d . . . H20A H 0.5166 0.5484 0.5160 0.067 Uiso 1 1 calc R . . H20B H 0.5080 0.5621 0.5390 0.067 Uiso 1 1 calc R . . H20C H 0.5395 0.5053 0.5325 0.067 Uiso 1 1 calc R . . C21 C 0.9069(4) 0.6887(4) 0.58033(10) 0.079(2) Uani 1 1 d . . . H21A H 0.9199 0.7182 0.5928 0.119 Uiso 1 1 calc R . . H21B H 0.9549 0.7004 0.5734 0.119 Uiso 1 1 calc R . . H21C H 0.8768 0.6330 0.5832 0.119 Uiso 1 1 calc R . . C22 C 0.8824(3) 0.8866(3) 0.53839(11) 0.077(2) Uani 1 1 d . . . H22A H 0.8503 0.9095 0.5420 0.116 Uiso 1 1 calc R . . H22B H 0.8839 0.8831 0.5239 0.116 Uiso 1 1 calc R . . H22C H 0.9353 0.9195 0.5435 0.116 Uiso 1 1 calc R . . C23 C 0.5159(9) 0.7400(7) 0.55362(18) 0.049(3) Uani 0.50 1 d P A -1 H23 H 0.4788 0.7209 0.5422 0.059 Uiso 0.50 1 calc PR A -1 C24 C 0.5394(8) 0.8221(7) 0.55657(18) 0.060(3) Uani 0.50 1 d P A -1 H24A H 0.4938 0.8263 0.5601 0.090 Uiso 0.50 1 calc PR A -1 H24B H 0.5626 0.8511 0.5443 0.090 Uiso 0.50 1 calc PR A -1 H24C H 0.5777 0.8437 0.5673 0.090 Uiso 0.50 1 calc PR A -1 C25 C 0.4725(13) 0.6895(12) 0.5714(3) 0.082(6) Uani 0.50 1 d P A -1 H25A H 0.5080 0.7041 0.5828 0.124 Uiso 0.50 1 calc PR A -1 H25B H 0.4527 0.6347 0.5682 0.124 Uiso 0.50 1 calc PR A -1 H25C H 0.4289 0.6973 0.5748 0.124 Uiso 0.50 1 calc PR A -1 C23A C 0.5690(9) 0.7769(9) 0.5598(2) 0.067(4) Uani 0.50 1 d P A -2 H23A H 0.5764 0.8228 0.5519 0.081 Uiso 0.50 1 calc PR A -2 C24A C 0.6204(13) 0.8033(15) 0.5769(3) 0.169(11) Uani 0.50 1 d P A -2 H24D H 0.6225 0.7592 0.5828 0.253 Uiso 0.50 1 calc PR A -2 H24E H 0.6006 0.8254 0.5868 0.253 Uiso 0.50 1 calc PR A -2 H24F H 0.6727 0.8431 0.5728 0.253 Uiso 0.50 1 calc PR A -2 C25A C 0.4876(13) 0.7294(16) 0.5653(4) 0.117(9) Uani 0.50 1 d P A -2 H25D H 0.4583 0.6960 0.5541 0.175 Uiso 0.50 1 calc PR A -2 H25E H 0.4665 0.7631 0.5688 0.175 Uiso 0.50 1 calc PR A -2 H25F H 0.4833 0.6970 0.5767 0.175 Uiso 0.50 1 calc PR A -2 N1 N 0.6678(2) 0.7187(2) 0.49483(6) 0.0340(9) Uani 1 1 d . . . N2 N 0.6203(2) 0.6200(2) 0.52943(6) 0.0338(9) Uani 1 1 d . . . O1 O 0.52811(16) 0.67662(17) 0.51300(4) 0.0301(7) Uani 1 1 d . . . O2 O 0.72737(18) 0.77781(17) 0.53341(5) 0.0441(9) Uani 1 1 d . . . O3 O 0.63993(19) 0.82215(18) 0.51583(5) 0.0412(8) Uani 1 1 d . . . O4 O 0.5834(2) 0.72903(19) 0.54805(5) 0.0404(8) Uani 1 1 d . . . V1 V 0.62653(4) 0.74130(4) 0.524265(12) 0.0294(2) Uani 1 1 d . A . 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 0.032(2) 0.023(2) 0.036(2) -0.0024(18) -0.007(2) 0.0195(19) C2 0.025(2) 0.024(2) 0.042(3) -0.0006(19) -0.0049(19) 0.0160(18) C3 0.032(2) 0.024(2) 0.056(3) -0.003(2) -0.010(2) 0.019(2) C4 0.049(3) 0.031(2) 0.040(3) -0.006(2) -0.018(2) 0.027(2) C5 0.046(3) 0.035(3) 0.033(2) 0.003(2) 0.000(2) 0.028(2) C6 0.034(2) 0.027(2) 0.036(2) 0.0005(19) -0.004(2) 0.020(2) C7 0.038(3) 0.038(3) 0.041(3) 0.006(2) 0.003(2) 0.020(2) C8 0.025(2) 0.027(2) 0.062(3) -0.009(2) -0.004(2) 0.014(2) C9 0.029(2) 0.027(2) 0.061(3) -0.008(2) -0.012(2) 0.019(2) C10 0.038(3) 0.032(3) 0.057(3) 0.010(2) -0.004(2) 0.018(2) C11 0.039(3) 0.036(3) 0.042(3) -0.004(2) -0.012(2) 0.021(2) C12 0.051(3) 0.046(3) 0.040(3) -0.005(2) -0.015(2) 0.031(3) C13 0.053(3) 0.058(4) 0.057(3) -0.018(3) -0.029(3) 0.038(3) C14 0.036(3) 0.054(4) 0.080(4) -0.026(3) -0.030(3) 0.021(3) C15 0.038(3) 0.033(3) 0.073(4) -0.012(3) -0.022(3) 0.013(2) C16 0.038(3) 0.030(2) 0.052(3) -0.009(2) -0.017(2) 0.016(2) C17 0.023(2) 0.033(2) 0.051(3) -0.003(2) -0.004(2) 0.013(2) C18 0.070(4) 0.044(3) 0.048(3) -0.008(3) -0.025(3) 0.033(3) C19 0.024(2) 0.037(3) 0.073(4) 0.003(3) 0.004(2) 0.009(2) C20 0.028(2) 0.021(2) 0.079(4) 0.003(2) -0.005(2) 0.009(2) C21 0.085(5) 0.090(5) 0.090(5) -0.030(4) -0.055(4) 0.064(4) C22 0.039(3) 0.036(3) 0.130(6) -0.007(4) -0.029(4) 0.000(3) C23 0.058(8) 0.044(7) 0.040(7) 0.003(6) 0.000(6) 0.022(6) C24 0.079(9) 0.069(8) 0.054(7) -0.013(6) -0.005(6) 0.053(8) C25 0.080(13) 0.088(14) 0.059(10) 0.023(10) 0.040(9) 0.027(11) C23A 0.085(11) 0.071(9) 0.065(9) -0.024(7) -0.009(8) 0.054(9) C24A 0.17(2) 0.23(3) 0.143(17) -0.144(19) -0.118(16) 0.13(2) C25A 0.080(15) 0.14(3) 0.11(2) 0.005(17) 0.049(14) 0.046(17) N1 0.0200(18) 0.0271(19) 0.053(2) 0.0013(17) -0.0001(17) 0.0104(16) N2 0.0274(19) 0.0196(18) 0.054(2) 0.0018(17) -0.0054(18) 0.0116(16) O1 0.0236(15) 0.0333(16) 0.0342(17) -0.0036(13) -0.0060(13) 0.0149(13) O2 0.0314(18) 0.0238(16) 0.071(2) -0.0018(16) -0.0201(17) 0.0092(14) O3 0.046(2) 0.0251(16) 0.057(2) 0.0003(15) -0.0064(16) 0.0209(15) O4 0.053(2) 0.0370(19) 0.0368(19) -0.0076(15) -0.0077(16) 0.0268(17) V1 0.0292(4) 0.0198(4) 0.0415(4) -0.0028(3) -0.0085(3) 0.0141(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 C1 O1 1.336(5) . ? C1 C6 1.401(6) . ? C1 C2 1.408(6) . ? C2 C3 1.384(6) . ? C2 C17 1.498(6) . ? C3 C4 1.374(7) . ? C3 H3 0.9500 . ? C4 C5 1.382(7) . ? C4 C18 1.506(6) . ? C5 C6 1.393(6) . ? C5 H5 0.9500 . ? C6 C7 1.503(6) . ? C7 N1 1.490(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N1 1.487(5) . ? C8 C9 1.513(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 N2 1.478(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N2 1.483(6) . ? C10 C11 1.497(7) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.389(6) . ? C11 C16 1.405(7) . ? C12 C13 1.375(7) . ? C12 H12 0.9500 . ? C13 C14 1.380(8) . ? C13 C21 1.520(7) . ? C14 C15 1.384(7) . ? C14 H14 0.9500 . ? C15 C16 1.402(7) . ? C15 C22 1.495(8) . ? C16 O2 1.351(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 N1 1.486(5) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 N2 1.489(6) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.467(16) . ? C23 O4 1.509(15) . ? C23 C25 1.525(17) . ? C23 H23 1.0000 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C23A O4 1.373(12) . ? C23A C25A 1.45(2) . ? C23A C24A 1.457(19) . ? C23A H23A 1.0000 . ? C24A H24D 0.9800 . ? C24A H24E 0.9800 . ? C24A H24F 0.9800 . ? C25A H25D 0.9800 . ? C25A H25E 0.9800 . ? C25A H25F 0.9800 . ? N1 V1 2.276(4) . ? N2 V1 2.375(3) . ? O1 V1 1.880(3) . ? O2 V1 1.861(3) . ? O3 V1 1.595(3) . ? O4 V1 1.777(3) . ? 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 C6 122.1(4) . . ? O1 C1 C2 117.8(4) . . ? C6 C1 C2 120.1(4) . . ? C3 C2 C1 118.4(4) . . ? C3 C2 C17 121.9(4) . . ? C1 C2 C17 119.7(4) . . ? C4 C3 C2 122.7(4) . . ? C4 C3 H3 118.7 . . ? C2 C3 H3 118.7 . . ? C3 C4 C5 118.2(4) . . ? C3 C4 C18 120.8(5) . . ? C5 C4 C18 121.0(5) . . ? C4 C5 C6 122.0(4) . . ? C4 C5 H5 119.0 . . ? C6 C5 H5 119.0 . . ? C5 C6 C1 118.6(4) . . ? C5 C6 C7 119.4(4) . . ? C1 C6 C7 121.9(4) . . ? N1 C7 C6 115.6(4) . . ? N1 C7 H7A 108.4 . . ? C6 C7 H7A 108.4 . . ? N1 C7 H7B 108.4 . . ? C6 C7 H7B 108.4 . . ? H7A C7 H7B 107.5 . . ? N1 C8 C9 111.0(4) . . ? N1 C8 H8A 109.4 . . ? C9 C8 H8A 109.4 . . ? N1 C8 H8B 109.4 . . ? C9 C8 H8B 109.4 . . ? H8A C8 H8B 108.0 . . ? N2 C9 C8 110.3(3) . . ? N2 C9 H9A 109.6 . . ? C8 C9 H9A 109.6 . . ? N2 C9 H9B 109.6 . . ? C8 C9 H9B 109.6 . . ? H9A C9 H9B 108.1 . . ? N2 C10 C11 114.7(4) . . ? N2 C10 H10A 108.6 . . ? C11 C10 H10A 108.6 . . ? N2 C10 H10B 108.6 . . ? C11 C10 H10B 108.6 . . ? H10A C10 H10B 107.6 . . ? C12 C11 C16 118.6(5) . . ? C12 C11 C10 119.2(4) . . ? C16 C11 C10 122.2(4) . . ? C13 C12 C11 122.5(5) . . ? C13 C12 H12 118.8 . . ? C11 C12 H12 118.8 . . ? C12 C13 C14 117.6(5) . . ? C12 C13 C21 120.7(6) . . ? C14 C13 C21 121.7(5) . . ? C13 C14 C15 122.9(5) . . ? C13 C14 H14 118.5 . . ? C15 C14 H14 118.5 . . ? C14 C15 C16 118.4(5) . . ? C14 C15 C22 122.8(5) . . ? C16 C15 C22 118.8(5) . . ? O2 C16 C15 117.9(4) . . ? O2 C16 C11 122.1(4) . . ? C15 C16 C11 120.0(4) . . ? C2 C17 H17A 109.5 . . ? C2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C4 C18 H18A 109.5 . . ? C4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N1 C19 H19A 109.5 . . ? N1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N2 C20 H20A 109.5 . . ? N2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C13 C21 H21A 109.5 . . ? C13 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C13 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C15 C22 H22A 109.5 . . ? C15 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C15 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 O4 112.4(11) . . ? C24 C23 C25 112.6(13) . . ? O4 C23 C25 110.6(13) . . ? C24 C23 H23 106.9 . . ? O4 C23 H23 106.9 . . ? C25 C23 H23 106.9 . . ? O4 C23A C25A 104.3(15) . . ? O4 C23A C24A 110.9(13) . . ? C25A C23A C24A 112.4(18) . . ? O4 C23A H23A 109.7 . . ? C25A C23A H23A 109.7 . . ? C24A C23A H23A 109.7 . . ? C23A C24A H24D 109.5 . . ? C23A C24A H24E 109.5 . . ? H24D C24A H24E 109.5 . . ? C23A C24A H24F 109.5 . . ? H24D C24A H24F 109.5 . . ? H24E C24A H24F 109.5 . . ? C23A C25A H25D 109.5 . . ? C23A C25A H25E 109.5 . . ? H25D C25A H25E 109.5 . . ? C23A C25A H25F 109.5 . . ? H25D C25A H25F 109.5 . . ? H25E C25A H25F 109.5 . . ? C19 N1 C8 109.8(3) . . ? C19 N1 C7 106.4(4) . . ? C8 N1 C7 110.2(4) . . ? C19 N1 V1 111.1(3) . . ? C8 N1 V1 110.0(3) . . ? C7 N1 V1 109.2(3) . . ? C9 N2 C10 112.0(4) . . ? C9 N2 C20 110.1(4) . . ? C10 N2 C20 105.8(4) . . ? C9 N2 V1 107.2(3) . . ? C10 N2 V1 109.0(3) . . ? C20 N2 V1 112.7(3) . . ? C1 O1 V1 137.9(3) . . ? C16 O2 V1 140.3(3) . . ? C23A O4 C23 41.3(7) . . ? C23A O4 V1 132.7(7) . . ? C23 O4 V1 127.4(5) . . ? O3 V1 O4 106.65(16) . . ? O3 V1 O2 96.92(16) . . ? O4 V1 O2 96.04(16) . . ? O3 V1 O1 97.85(15) . . ? O4 V1 O1 90.36(14) . . ? O2 V1 O1 161.49(14) . . ? O3 V1 N1 89.50(16) . . ? O4 V1 N1 163.09(14) . . ? O2 V1 N1 86.71(15) . . ? O1 V1 N1 82.32(13) . . ? O3 V1 N2 166.12(16) . . ? O4 V1 N2 87.23(14) . . ? O2 V1 N2 81.17(13) . . ? O1 V1 N2 81.81(13) . . ? N1 V1 N2 76.68(13) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.462 _refine_diff_density_min -0.445 _refine_diff_density_rms 0.066 #===END data_(L1VO)2O _database_code_depnum_ccdc_archive 'CCDC 838967' #TrackingRef '- cifs.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H60 N4 O7 V2, 2(C7 H8)' _chemical_formula_sum 'C58 H68 N4 O7 V2' _chemical_formula_weight 1035.04 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 C2/c _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 11.7043(12) _cell_length_b 24.115(3) _cell_length_c 19.876(2) _cell_angle_alpha 90.00 _cell_angle_beta 101.532(2) _cell_angle_gamma 90.00 _cell_volume 5496.8(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(1) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour 'dark violet' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.251 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2184 _exptl_absorpt_coefficient_mu 0.394 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29432 _diffrn_reflns_av_R_equivalents 0.0576 _diffrn_reflns_av_sigmaI/netI 0.0575 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_k_max 31 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 28.18 _reflns_number_total 6544 _reflns_number_gt 4781 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _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^)+(0.0842P)^2^+27.1252P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6544 _refine_ls_number_parameters 345 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1534 _refine_ls_R_factor_gt 0.1199 _refine_ls_wR_factor_ref 0.2613 _refine_ls_wR_factor_gt 0.2447 _refine_ls_goodness_of_fit_ref 1.271 _refine_ls_restrained_S_all 1.271 _refine_ls_shift/su_max 0.001 _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 0.3958(4) 0.4459(2) 0.8547(2) 0.0380(12) Uani 1 1 d . . . C2 C 0.4713(5) 0.4007(2) 0.8697(3) 0.0374(11) Uani 1 1 d . . . C3 C 0.4333(5) 0.3529(2) 0.8980(3) 0.0432(13) Uani 1 1 d . . . H3 H 0.4847 0.3222 0.9081 0.052 Uiso 1 1 calc R . . C4 C 0.3219(5) 0.3492(2) 0.9117(3) 0.0436(14) Uani 1 1 d . . . C5 C 0.2486(5) 0.3940(3) 0.8960(3) 0.0462(14) Uani 1 1 d . . . H5 H 0.1723 0.3918 0.9055 0.055 Uiso 1 1 calc R . . C6 C 0.2818(5) 0.4425(3) 0.8668(3) 0.0421(13) Uani 1 1 d . . . C7 C 0.1938(5) 0.4885(3) 0.8477(3) 0.0545(17) Uani 1 1 d . . . H7A H 0.1509 0.4819 0.8002 0.065 Uiso 1 1 calc R . . H7B H 0.1366 0.4860 0.8781 0.065 Uiso 1 1 calc R . . C8 C 0.2990(5) 0.5603(3) 0.9231(3) 0.0499(16) Uani 1 1 d . . . H8A H 0.3477 0.5286 0.9434 0.060 Uiso 1 1 calc R . . H8B H 0.2392 0.5669 0.9511 0.060 Uiso 1 1 calc R . . C9 C 0.3747(5) 0.6113(3) 0.9250(3) 0.0477(15) Uani 1 1 d . . . H9A H 0.3258 0.6437 0.9071 0.057 Uiso 1 1 calc R . . H9B H 0.4137 0.6194 0.9729 0.057 Uiso 1 1 calc R . . C10 C 0.5139(4) 0.6550(3) 0.8636(3) 0.0449(14) Uani 1 1 d . . . H10A H 0.5738 0.6463 0.8364 0.054 Uiso 1 1 calc R . . H10B H 0.5541 0.6734 0.9064 0.054 Uiso 1 1 calc R . . C11 C 0.4288(4) 0.6956(2) 0.8236(3) 0.0381(12) Uani 1 1 d . . . C12 C 0.4480(5) 0.7529(3) 0.8326(3) 0.0482(15) Uani 1 1 d . . . H12 H 0.5149 0.7650 0.8646 0.058 Uiso 1 1 calc R . . C13 C 0.3746(5) 0.7924(3) 0.7971(3) 0.0486(14) Uani 1 1 d . . . C14 C 0.2754(6) 0.7742(3) 0.7520(3) 0.0494(14) Uani 1 1 d . . . H14 H 0.2222 0.8007 0.7282 0.059 Uiso 1 1 calc R . . C15 C 0.2524(5) 0.7178(2) 0.7408(3) 0.0414(12) Uani 1 1 d . . . C16 C 0.3304(4) 0.6781(2) 0.7753(2) 0.0333(11) Uani 1 1 d . . . C17 C 0.5940(5) 0.4051(3) 0.8554(4) 0.0515(15) Uani 1 1 d . . . H17A H 0.6386 0.4324 0.8865 0.077 Uiso 1 1 calc R . . H17B H 0.5898 0.4167 0.8078 0.077 Uiso 1 1 calc R . . H17C H 0.6325 0.3689 0.8629 0.077 Uiso 1 1 calc R . . C18 C 0.2827(7) 0.2972(3) 0.9438(4) 0.0648(19) Uani 1 1 d . . . H18A H 0.2350 0.3076 0.9771 0.097 Uiso 1 1 calc R . . H18B H 0.3512 0.2764 0.9672 0.097 Uiso 1 1 calc R . . H18C H 0.2366 0.2740 0.9078 0.097 Uiso 1 1 calc R . . C19 C 0.1385(5) 0.5831(3) 0.8290(3) 0.0588(18) Uani 1 1 d . . . H19A H 0.0782 0.5746 0.8554 0.088 Uiso 1 1 calc R . . H19B H 0.1071 0.5772 0.7800 0.088 Uiso 1 1 calc R . . H19C H 0.1629 0.6218 0.8368 0.088 Uiso 1 1 calc R . . C20 C 0.5626(5) 0.5689(3) 0.9214(3) 0.0560(18) Uani 1 1 d . . . H20A H 0.6024 0.5903 0.9611 0.084 Uiso 1 1 calc R . . H20B H 0.6177 0.5605 0.8916 0.084 Uiso 1 1 calc R . . H20C H 0.5330 0.5342 0.9372 0.084 Uiso 1 1 calc R . . C21 C 0.3974(7) 0.8543(3) 0.8085(4) 0.070(2) Uani 1 1 d . . . H21A H 0.3588 0.8674 0.8450 0.106 Uiso 1 1 calc R . . H21B H 0.3665 0.8744 0.7660 0.106 Uiso 1 1 calc R . . H21C H 0.4815 0.8608 0.8220 0.106 Uiso 1 1 calc R . . C22 C 0.1454(6) 0.6991(3) 0.6905(3) 0.0572(17) Uani 1 1 d . . . H22A H 0.1018 0.6725 0.7129 0.086 Uiso 1 1 calc R . . H22B H 0.1689 0.6814 0.6510 0.086 Uiso 1 1 calc R . . H22C H 0.0960 0.7312 0.6748 0.086 Uiso 1 1 calc R . . C23 C 0.2949(12) 0.7662(6) 1.0070(8) 0.061(3) Uani 0.50 1 d P . . C24 C 0.2457(8) 0.7333(3) 1.0559(5) 0.077(2) Uani 1 1 d . . . C25 C 0.1439(15) 0.7003(7) 1.0183(9) 0.071(4) Uani 0.50 1 d P . . C26 C 0.1027(8) 0.6987(4) 0.9549(6) 0.089(3) Uani 1 1 d . . . C27 C 0.1521(15) 0.7329(7) 0.9093(7) 0.071(4) Uani 0.50 1 d P . . C28 C -0.1019(14) 0.5065(11) 0.4307(9) 0.189(9) Uani 1 1 d . . . C29 C -0.0319(8) 0.5445(5) 0.4689(5) 0.093(4) Uani 1 1 d . . . C30 C 0.0568(13) 0.5477(9) 0.5278(8) 0.170(7) Uani 1 1 d . . . C31 C 0.1232(11) 0.5670(11) 0.5650(8) 0.086(7) Uani 0.50 1 d P . . N1 N 0.2404(4) 0.5461(2) 0.8516(2) 0.0432(12) Uani 1 1 d . . . N2 N 0.4637(4) 0.6018(2) 0.8824(2) 0.0393(11) Uani 1 1 d . . . O1 O 0.4372(3) 0.49246(15) 0.83111(18) 0.0399(9) Uani 1 1 d . . . O2 O 0.3069(3) 0.62469(14) 0.75977(16) 0.0331(8) Uani 1 1 d . . . O3 O 0.5000 0.56696(19) 0.7500 0.0308(10) Uani 1 2 d S . . O4 O 0.2800(3) 0.52177(15) 0.72286(18) 0.0404(9) Uani 1 1 d . . . V1 V 0.36986(7) 0.55388(4) 0.78133(4) 0.0280(2) Uani 1 1 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 0.032(3) 0.056(3) 0.027(2) 0.011(2) 0.0078(19) 0.003(2) C2 0.041(3) 0.041(3) 0.030(3) 0.002(2) 0.008(2) -0.001(2) C3 0.053(3) 0.039(3) 0.036(3) 0.000(2) 0.007(2) -0.010(3) C4 0.057(3) 0.043(3) 0.031(3) 0.001(2) 0.008(2) -0.025(3) C5 0.039(3) 0.070(4) 0.030(3) 0.006(3) 0.010(2) -0.022(3) C6 0.036(3) 0.060(4) 0.032(3) 0.010(3) 0.013(2) -0.004(3) C7 0.030(3) 0.084(5) 0.055(4) 0.024(3) 0.021(3) 0.003(3) C8 0.049(3) 0.074(4) 0.033(3) 0.008(3) 0.024(2) 0.029(3) C9 0.046(3) 0.080(4) 0.020(2) -0.002(3) 0.013(2) 0.026(3) C10 0.027(3) 0.067(4) 0.038(3) -0.021(3) 0.000(2) 0.005(3) C11 0.030(3) 0.055(3) 0.030(3) -0.013(2) 0.009(2) 0.003(2) C12 0.040(3) 0.064(4) 0.042(3) -0.024(3) 0.012(2) -0.013(3) C13 0.057(4) 0.047(3) 0.046(3) -0.005(3) 0.021(3) -0.005(3) C14 0.058(4) 0.048(3) 0.042(3) 0.000(3) 0.009(3) 0.007(3) C15 0.044(3) 0.039(3) 0.039(3) 0.000(2) 0.003(2) 0.004(2) C16 0.028(2) 0.046(3) 0.026(2) -0.009(2) 0.0043(19) -0.003(2) C17 0.039(3) 0.046(3) 0.073(4) 0.010(3) 0.020(3) 0.008(3) C18 0.080(5) 0.060(4) 0.057(4) 0.004(3) 0.020(4) -0.032(4) C19 0.033(3) 0.093(5) 0.056(4) 0.018(4) 0.023(3) 0.025(3) C20 0.041(3) 0.087(5) 0.034(3) -0.009(3) -0.008(2) 0.030(3) C21 0.091(6) 0.052(4) 0.072(5) -0.014(4) 0.027(4) -0.022(4) C22 0.053(4) 0.050(4) 0.056(4) 0.009(3) -0.018(3) 0.005(3) C23 0.053(8) 0.061(9) 0.070(9) -0.005(7) 0.016(7) 0.015(6) C24 0.085(6) 0.060(5) 0.096(7) 0.016(4) 0.042(5) 0.022(4) C25 0.078(11) 0.065(10) 0.077(11) 0.010(8) 0.030(9) -0.007(8) C26 0.066(5) 0.089(6) 0.110(8) -0.007(6) 0.012(5) 0.007(5) C27 0.080(10) 0.082(11) 0.049(8) 0.004(7) 0.011(7) 0.031(9) C28 0.114(11) 0.33(3) 0.151(14) 0.036(16) 0.090(11) 0.095(16) C29 0.058(5) 0.161(10) 0.067(5) 0.054(6) 0.030(4) 0.062(6) C30 0.100(10) 0.31(2) 0.131(12) 0.036(13) 0.094(9) 0.074(12) C31 0.015(6) 0.19(2) 0.048(8) -0.012(11) -0.002(5) -0.009(9) N1 0.026(2) 0.074(3) 0.034(2) 0.013(2) 0.0148(17) 0.015(2) N2 0.029(2) 0.067(3) 0.0205(19) -0.0078(19) 0.0029(16) 0.019(2) O1 0.0319(18) 0.047(2) 0.046(2) 0.0233(17) 0.0207(16) 0.0110(16) O2 0.0309(18) 0.040(2) 0.0263(17) -0.0047(14) -0.0003(13) 0.0041(15) O3 0.033(2) 0.034(3) 0.031(2) 0.000 0.021(2) 0.000 O4 0.046(2) 0.038(2) 0.037(2) -0.0019(16) 0.0101(16) -0.0031(17) V1 0.0278(4) 0.0379(5) 0.0213(4) 0.0041(3) 0.0120(3) 0.0043(4) _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 1.344(6) . ? C1 C2 1.397(7) . ? C1 C6 1.404(7) . ? C2 C3 1.394(7) . ? C2 C17 1.522(7) . ? C3 C4 1.387(8) . ? C3 H3 0.9500 . ? C4 C5 1.375(9) . ? C4 C18 1.520(8) . ? C5 C6 1.396(8) . ? C5 H5 0.9500 . ? C6 C7 1.510(8) . ? C7 N1 1.488(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N1 1.488(7) . ? C8 C9 1.513(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 N2 1.485(6) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 N2 1.490(8) . ? C10 C11 1.507(8) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.406(8) . ? C11 C16 1.408(7) . ? C12 C13 1.377(9) . ? C12 H12 0.9500 . ? C13 C14 1.388(8) . ? C13 C21 1.525(9) . ? C14 C15 1.396(8) . ? C14 H14 0.9500 . ? C15 C16 1.404(7) . ? C15 C22 1.508(8) . ? C16 O2 1.340(6) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 N1 1.485(7) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 N2 1.487(6) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.247(17) 7_567 ? C23 C25 1.25(2) 7_567 ? C23 C23 1.29(3) 7_567 ? C23 C24 1.459(18) . ? C23 C26 1.538(17) 7_567 ? C23 C27 1.65(2) 7_567 ? C24 C23 1.247(17) 7_567 ? C24 C27 1.498(19) 7_567 ? C24 C25 1.501(19) . ? C25 C23 1.25(2) 7_567 ? C25 C26 1.256(18) . ? C26 C27 1.430(19) . ? C26 C23 1.538(17) 7_567 ? C27 C24 1.498(19) 7_567 ? C27 C23 1.65(2) 7_567 ? C28 C29 1.36(2) . ? C28 C30 1.58(2) 5_566 ? C28 C31 1.79(3) 5_566 ? C29 C30 1.403(18) . ? C30 C31 1.07(2) . ? C30 C28 1.58(2) 5_566 ? C31 C28 1.79(3) 5_566 ? N1 V1 2.264(4) . ? N2 V1 2.387(4) . ? O1 V1 1.866(3) . ? O2 V1 1.875(3) . ? O3 V1 1.7851(11) 2_656 ? O3 V1 1.7851(11) . ? O4 V1 1.603(4) . ? 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 118.0(4) . . ? O1 C1 C6 122.0(5) . . ? C2 C1 C6 120.0(5) . . ? C3 C2 C1 119.5(5) . . ? C3 C2 C17 121.4(5) . . ? C1 C2 C17 119.1(5) . . ? C4 C3 C2 121.3(6) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C5 C4 C3 118.3(5) . . ? C5 C4 C18 121.1(6) . . ? C3 C4 C18 120.6(6) . . ? C4 C5 C6 122.6(5) . . ? C4 C5 H5 118.7 . . ? C6 C5 H5 118.7 . . ? C5 C6 C1 118.3(5) . . ? C5 C6 C7 119.2(5) . . ? C1 C6 C7 122.6(5) . . ? N1 C7 C6 116.6(5) . . ? N1 C7 H7A 108.2 . . ? C6 C7 H7A 108.2 . . ? N1 C7 H7B 108.2 . . ? C6 C7 H7B 108.2 . . ? H7A C7 H7B 107.3 . . ? N1 C8 C9 111.5(4) . . ? N1 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? N1 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? N2 C9 C8 109.5(5) . . ? N2 C9 H9A 109.8 . . ? C8 C9 H9A 109.8 . . ? N2 C9 H9B 109.8 . . ? C8 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? N2 C10 C11 116.1(4) . . ? N2 C10 H10A 108.3 . . ? C11 C10 H10A 108.3 . . ? N2 C10 H10B 108.3 . . ? C11 C10 H10B 108.3 . . ? H10A C10 H10B 107.4 . . ? C12 C11 C16 118.0(5) . . ? C12 C11 C10 120.0(5) . . ? C16 C11 C10 121.9(5) . . ? C13 C12 C11 123.1(5) . . ? C13 C12 H12 118.4 . . ? C11 C12 H12 118.4 . . ? C12 C13 C14 117.9(6) . . ? C12 C13 C21 121.8(6) . . ? C14 C13 C21 120.2(6) . . ? C13 C14 C15 121.3(6) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C14 C15 C16 120.1(5) . . ? C14 C15 C22 120.4(5) . . ? C16 C15 C22 119.5(5) . . ? O2 C16 C15 117.4(4) . . ? O2 C16 C11 123.2(5) . . ? C15 C16 C11 119.4(5) . . ? C2 C17 H17A 109.5 . . ? C2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C4 C18 H18A 109.5 . . ? C4 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C4 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N1 C19 H19A 109.5 . . ? N1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N2 C20 H20A 109.5 . . ? N2 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N2 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C13 C21 H21A 109.5 . . ? C13 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C13 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C15 C22 H22A 109.5 . . ? C15 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C15 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C25 73.9(13) 7_567 7_567 ? C24 C23 C23 70.1(14) 7_567 7_567 ? C25 C23 C23 144(2) 7_567 7_567 ? C24 C23 C24 123.5(12) 7_567 . ? C25 C23 C24 162.5(17) 7_567 . ? C23 C23 C24 53.5(12) 7_567 . ? C24 C23 C26 126.2(13) 7_567 7_567 ? C25 C23 C26 52.3(10) 7_567 7_567 ? C23 C23 C26 163(2) 7_567 7_567 ? C24 C23 C26 110.2(13) . 7_567 ? C24 C23 C27 178.6(13) 7_567 7_567 ? C25 C23 C27 105.4(15) 7_567 7_567 ? C23 C23 C27 110.6(19) 7_567 7_567 ? C24 C23 C27 57.1(10) . 7_567 ? C26 C23 C27 53.1(9) 7_567 7_567 ? C23 C24 C23 56.5(12) 7_567 . ? C23 C24 C27 124.5(11) 7_567 7_567 ? C23 C24 C27 68.0(9) . 7_567 ? C23 C24 C25 53.2(10) 7_567 . ? C23 C24 C25 109.6(12) . . ? C27 C24 C25 177.6(11) 7_567 . ? C23 C25 C26 75.7(13) 7_567 . ? C23 C25 C24 52.9(10) 7_567 . ? C26 C25 C24 128.6(13) . . ? C25 C26 C27 119.6(12) . . ? C25 C26 C23 52.0(10) . 7_567 ? C27 C26 C23 67.6(10) . 7_567 ? C26 C27 C24 114.1(11) . 7_567 ? C26 C27 C23 59.3(8) . 7_567 ? C24 C27 C23 54.9(8) 7_567 7_567 ? C29 C28 C30 99.5(16) . 5_566 ? C29 C28 C31 135.7(15) . 5_566 ? C30 C28 C31 36.2(9) 5_566 5_566 ? C28 C29 C30 140.1(14) . . ? C31 C30 C29 156(3) . . ? C31 C30 C28 83.0(19) . 5_566 ? C29 C30 C28 120.4(19) . 5_566 ? C30 C31 C28 60.8(17) . 5_566 ? C19 N1 C8 109.8(5) . . ? C19 N1 C7 106.3(5) . . ? C8 N1 C7 111.0(5) . . ? C19 N1 V1 111.1(3) . . ? C8 N1 V1 109.4(3) . . ? C7 N1 V1 109.2(3) . . ? C9 N2 C20 110.3(4) . . ? C9 N2 C10 111.5(4) . . ? C20 N2 C10 106.6(5) . . ? C9 N2 V1 107.3(3) . . ? C20 N2 V1 111.1(3) . . ? C10 N2 V1 110.2(3) . . ? C1 O1 V1 134.8(3) . . ? C16 O2 V1 140.3(3) . . ? V1 O3 V1 159.6(3) 2_656 . ? O4 V1 O3 108.34(15) . . ? O4 V1 O1 98.48(19) . . ? O3 V1 O1 91.48(15) . . ? O4 V1 O2 95.93(17) . . ? O3 V1 O2 94.77(17) . . ? O1 V1 O2 161.62(16) . . ? O4 V1 N1 89.09(18) . . ? O3 V1 N1 162.28(13) . . ? O1 V1 N1 82.58(15) . . ? O2 V1 N1 86.32(16) . . ? O4 V1 N2 165.78(17) . . ? O3 V1 N2 85.81(13) . . ? O1 V1 N2 82.15(17) . . ? O2 V1 N2 81.09(15) . . ? N1 V1 N2 76.87(17) . . ? _diffrn_measured_fraction_theta_max 0.967 _diffrn_reflns_theta_full 28.18 _diffrn_measured_fraction_theta_full 0.967 _refine_diff_density_max 1.059 _refine_diff_density_min -0.806 _refine_diff_density_rms 0.119