# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1595 data_compound1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H42 N5 O6 V' _chemical_formula_weight 571.59 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'V' 'V' 0.3005 0.5294 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, z' 'x, -y+1/2, z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, -z' '-x, y-1/2, -z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 13.6607(8) _cell_length_b 17.9727(16) _cell_length_c 23.6191(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5799.0(7) _cell_formula_units_Z 8 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 25.08 _exptl_crystal_description plate _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.50 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.309 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2432 _exptl_absorpt_coefficient_mu 0.389 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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_type 'IPDS, Stoe & Cie Company, Germany' _diffrn_measurement_method 'Phi oscillation scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32314 _diffrn_reflns_av_R_equivalents 0.0590 _diffrn_reflns_av_sigmaI/netI 0.0551 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.06 _diffrn_reflns_theta_max 25.89 _reflns_number_total 5613 _reflns_number_gt 3493 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, Stoe & Cie Company, Germany' _computing_cell_refinement 'CELL, Stoe & Cie Company, Germany' _computing_data_reduction 'XRED, Stoe & Cie Company, Germany' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0386P)^2^+0.0000P] 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 5613 _refine_ls_number_parameters 347 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0641 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0736 _refine_ls_wR_factor_gt 0.0682 _refine_ls_goodness_of_fit_ref 0.839 _refine_ls_restrained_S_all 0.839 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.88315(2) 0.839744(17) 0.618459(12) 0.02644(9) Uani 1 d . . . O1 O 0.87019(9) 0.77121(7) 0.57363(5) 0.0324(3) Uani 1 d . . . O2 O 0.90319(10) 0.91377(7) 0.58106(5) 0.0364(3) Uani 1 d . . . O3 O 1.02068(9) 0.82212(7) 0.64270(5) 0.0324(3) Uani 1 d . . . O4 O 1.13140(11) 0.76103(9) 0.69488(7) 0.0521(4) Uani 1 d . . . O5 O 0.74148(9) 0.85305(7) 0.63654(5) 0.0310(3) Uani 1 d . . . O6 O 0.62281(10) 0.91406(8) 0.68221(6) 0.0451(4) Uani 1 d . . . N1 N 0.87472(11) 0.75589(8) 0.69428(6) 0.0266(3) Uani 1 d . . . N2 N 0.90270(16) 0.64559(10) 0.77521(8) 0.0497(5) Uani 1 d . . . N3 N 0.87848(11) 0.91435(8) 0.69835(6) 0.0259(3) Uani 1 d . . . N4 N 0.83929(14) 1.02297(10) 0.77913(7) 0.0422(4) Uani 1 d . . . N5 N 0.57041(11) 0.70399(8) 0.54642(6) 0.0267(3) Uani 1 d . . . C1 C 0.96450(14) 0.73398(10) 0.70921(8) 0.0292(4) Uani 1 d . . . C2 C 0.97737(18) 0.67849(12) 0.74881(9) 0.0437(6) Uani 1 d . . . H2 H 1.0414 0.6632 0.7576 0.052 Uiso 1 calc R . . C3 C 0.81422(17) 0.67063(11) 0.76185(9) 0.0407(5) Uani 1 d . . . H3 H 0.7596 0.6507 0.7807 0.049 Uiso 1 calc R . . C4 C 0.79952(15) 0.72504(11) 0.72118(8) 0.0327(5) Uani 1 d . . . H4 H 0.7355 0.7403 0.7125 0.039 Uiso 1 calc R . . C5 C 1.04733(15) 0.77436(11) 0.68057(8) 0.0331(5) Uani 1 d . . . C6 C 0.78696(14) 0.93741(10) 0.70852(7) 0.0268(4) Uani 1 d . . . C7 C 0.76828(16) 0.99167(11) 0.74825(8) 0.0365(5) Uani 1 d . . . H7 H 0.7033 1.0073 0.7539 0.044 Uiso 1 calc R . . C8 C 0.92912(16) 0.99731(11) 0.77014(8) 0.0365(5) Uani 1 d . . . H8 H 0.9808 1.0164 0.7921 0.044 Uiso 1 calc R . . C9 C 0.94980(15) 0.94371(11) 0.72987(7) 0.0303(4) Uani 1 d . . . H9 H 1.0147 0.9278 0.7246 0.036 Uiso 1 calc R . . C10 C 0.70889(14) 0.90005(11) 0.67367(8) 0.0290(4) Uani 1 d . . . C11 C 0.65975(14) 0.67361(10) 0.57707(8) 0.0302(4) Uani 1 d . . . H11A H 0.7066 0.7143 0.5821 0.036 Uiso 1 calc R . . H11B H 0.6394 0.6571 0.6148 0.036 Uiso 1 calc R . . C12 C 0.71182(16) 0.60974(12) 0.54817(9) 0.0404(5) Uani 1 d . . . H12A H 0.6650 0.5695 0.5410 0.048 Uiso 1 calc R . . H12B H 0.7376 0.6266 0.5116 0.048 Uiso 1 calc R . . C13 C 0.79494(16) 0.58052(12) 0.58402(10) 0.0459(6) Uani 1 d . . . H13A H 0.7690 0.5637 0.6205 0.055 Uiso 1 calc R . . H13B H 0.8414 0.6209 0.5914 0.055 Uiso 1 calc R . . C14 C 0.84827(19) 0.51660(13) 0.55572(11) 0.0586(7) Uani 1 d . . . H14A H 0.9006 0.4994 0.5802 0.088 Uiso 1 calc R . . H14B H 0.8756 0.5333 0.5200 0.088 Uiso 1 calc R . . H14C H 0.8027 0.4762 0.5488 0.088 Uiso 1 calc R . . C15 C 0.49686(14) 0.64286(10) 0.53371(7) 0.0291(4) Uani 1 d . . . H15A H 0.4405 0.6655 0.5146 0.035 Uiso 1 calc R . . H15B H 0.5270 0.6081 0.5069 0.035 Uiso 1 calc R . . C16 C 0.45917(15) 0.59848(11) 0.58374(8) 0.0364(5) Uani 1 d . . . H16A H 0.5144 0.5806 0.6065 0.044 Uiso 1 calc R . . H16B H 0.4183 0.6303 0.6078 0.044 Uiso 1 calc R . . C17 C 0.39967(15) 0.53295(11) 0.56258(8) 0.0374(5) Uani 1 d . . . H17A H 0.3502 0.5511 0.5359 0.045 Uiso 1 calc R . . H17B H 0.4430 0.4989 0.5420 0.045 Uiso 1 calc R . . C18 C 0.34903(17) 0.49041(12) 0.60940(10) 0.0502(6) Uani 1 d . . . H18A H 0.3129 0.4491 0.5933 0.075 Uiso 1 calc R . . H18B H 0.3042 0.5232 0.6292 0.075 Uiso 1 calc R . . H18C H 0.3975 0.4717 0.6358 0.075 Uiso 1 calc R . . C19 C 0.59833(14) 0.73643(10) 0.48909(7) 0.0283(4) Uani 1 d . . . H19A H 0.6266 0.6965 0.4660 0.034 Uiso 1 calc R . . H19B H 0.5384 0.7531 0.4702 0.034 Uiso 1 calc R . . C20 C 0.66971(16) 0.80066(12) 0.49012(8) 0.0391(5) Uani 1 d . . . H20A H 0.7338 0.7832 0.5031 0.047 Uiso 1 calc R . . H20B H 0.6466 0.8388 0.5166 0.047 Uiso 1 calc R . . C21 C 0.67912(16) 0.83390(13) 0.43083(9) 0.0460(6) Uani 1 d . . . H21A H 0.7369 0.8661 0.4298 0.055 Uiso 1 calc R . . H21B H 0.6897 0.7935 0.4037 0.055 Uiso 1 calc R . . C22 C 0.59054(19) 0.87866(13) 0.41234(10) 0.0576(7) Uani 1 d . . . H22A H 0.6016 0.8984 0.3747 0.086 Uiso 1 calc R . . H22B H 0.5801 0.9194 0.4386 0.086 Uiso 1 calc R . . H22C H 0.5332 0.8468 0.4120 0.086 Uiso 1 calc R . . C23 C 0.52626(14) 0.76305(11) 0.58477(7) 0.0320(5) Uani 1 d . . . H23A H 0.5782 0.7976 0.5960 0.038 Uiso 1 calc R . . H23B H 0.5023 0.7387 0.6192 0.038 Uiso 1 calc R . . C24 C 0.44282(17) 0.80771(13) 0.55906(9) 0.0448(6) Uani 1 d . . . H24A H 0.3895 0.7740 0.5484 0.054 Uiso 1 calc R . . H24B H 0.4658 0.8328 0.5247 0.054 Uiso 1 calc R . . C25 C 0.40468(17) 0.86564(12) 0.60100(9) 0.0443(6) Uani 1 d . . . H25A H 0.4597 0.8964 0.6137 0.053 Uiso 1 calc R . . H25B H 0.3583 0.8983 0.5814 0.053 Uiso 1 calc R . . C26 C 0.3553(2) 0.83327(14) 0.65174(10) 0.0612(7) Uani 1 d . . . H26A H 0.3244 0.8727 0.6733 0.092 Uiso 1 calc R . . H26B H 0.4034 0.8083 0.6752 0.092 Uiso 1 calc R . . H26C H 0.3060 0.7978 0.6397 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 V1 0.02243(17) 0.03555(17) 0.02135(14) -0.00230(14) 0.00094(14) -0.00009(15) O1 0.0283(8) 0.0415(8) 0.0272(6) -0.0068(6) 0.0017(6) -0.0007(6) O2 0.0400(9) 0.0410(8) 0.0282(7) 0.0022(6) 0.0036(6) -0.0005(6) O3 0.0211(7) 0.0445(8) 0.0315(7) -0.0015(6) 0.0032(6) -0.0014(6) O4 0.0232(9) 0.0718(11) 0.0614(10) 0.0042(9) -0.0074(7) 0.0073(8) O5 0.0229(7) 0.0423(8) 0.0277(6) -0.0070(6) -0.0029(5) 0.0009(6) O6 0.0212(8) 0.0662(10) 0.0478(8) -0.0128(8) -0.0009(7) 0.0082(7) N1 0.0243(9) 0.0304(8) 0.0251(7) -0.0038(7) 0.0030(7) 0.0000(7) N2 0.0625(15) 0.0410(11) 0.0455(11) 0.0109(9) 0.0073(10) 0.0061(10) N3 0.0230(9) 0.0302(8) 0.0244(7) -0.0006(6) 0.0003(7) -0.0004(7) N4 0.0420(12) 0.0398(10) 0.0447(10) -0.0137(8) -0.0047(9) 0.0048(9) N5 0.0250(9) 0.0305(9) 0.0246(8) -0.0046(7) -0.0029(7) -0.0022(7) C1 0.0296(12) 0.0317(11) 0.0263(9) -0.0067(8) -0.0001(9) 0.0042(9) C2 0.0433(14) 0.0438(13) 0.0442(12) 0.0035(10) -0.0019(11) 0.0138(11) C3 0.0478(15) 0.0334(12) 0.0408(12) -0.0009(10) 0.0139(11) -0.0047(10) C4 0.0294(12) 0.0366(12) 0.0320(10) -0.0041(9) 0.0056(9) -0.0032(9) C5 0.0292(12) 0.0397(12) 0.0305(10) -0.0081(9) -0.0008(9) 0.0034(9) C6 0.0248(11) 0.0302(11) 0.0255(9) 0.0025(8) -0.0007(8) 0.0022(8) C7 0.0320(12) 0.0375(12) 0.0401(11) -0.0059(10) -0.0015(10) 0.0081(10) C8 0.0353(13) 0.0364(12) 0.0378(11) -0.0058(10) -0.0069(10) -0.0035(10) C9 0.0234(11) 0.0359(11) 0.0316(10) -0.0022(9) -0.0028(8) -0.0026(8) C10 0.0256(12) 0.0350(11) 0.0265(10) 0.0015(9) -0.0002(9) 0.0010(9) C11 0.0249(11) 0.0372(11) 0.0285(9) 0.0000(8) -0.0054(8) -0.0001(9) C12 0.0387(13) 0.0430(13) 0.0394(11) -0.0035(10) -0.0043(10) 0.0081(10) C13 0.0406(14) 0.0414(13) 0.0557(14) 0.0060(11) -0.0054(11) 0.0064(10) C14 0.0510(16) 0.0524(15) 0.0724(17) 0.0111(13) 0.0031(13) 0.0164(12) C15 0.0246(11) 0.0348(11) 0.0278(9) -0.0048(8) -0.0022(8) -0.0058(8) C16 0.0357(13) 0.0414(12) 0.0321(11) 0.0020(9) -0.0037(9) -0.0050(9) C17 0.0357(13) 0.0338(11) 0.0426(12) -0.0037(9) 0.0086(10) -0.0033(9) C18 0.0460(14) 0.0474(13) 0.0571(14) 0.0114(12) 0.0021(12) -0.0086(11) C19 0.0282(12) 0.0339(10) 0.0227(9) 0.0001(8) -0.0016(8) -0.0011(8) C20 0.0329(13) 0.0447(12) 0.0397(11) 0.0051(10) -0.0072(10) -0.0095(10) C21 0.0358(13) 0.0562(14) 0.0460(12) 0.0110(11) 0.0006(10) -0.0137(11) C22 0.0646(19) 0.0556(15) 0.0524(15) 0.0158(12) -0.0031(13) 0.0003(13) C23 0.0331(12) 0.0359(11) 0.0270(10) -0.0065(9) -0.0014(9) 0.0012(9) C24 0.0430(14) 0.0551(14) 0.0362(11) -0.0061(11) -0.0023(10) 0.0152(11) C25 0.0438(15) 0.0422(12) 0.0468(12) -0.0025(10) 0.0004(11) 0.0069(10) C26 0.0665(19) 0.0561(16) 0.0610(15) -0.0092(13) 0.0172(13) 0.0009(14) _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 O2 1.6203(13) . ? V1 O1 1.6340(12) . ? V1 O3 1.9895(13) . ? V1 O5 1.9961(13) . ? V1 N3 2.3158(14) . ? V1 N1 2.3434(15) . ? O3 C5 1.292(2) . ? O4 C5 1.221(2) . ? O5 C10 1.296(2) . ? O6 C10 1.219(2) . ? N1 C4 1.329(2) . ? N1 C1 1.335(2) . ? N2 C3 1.328(3) . ? N2 C2 1.334(3) . ? N3 C9 1.335(2) . ? N3 C6 1.339(2) . ? N4 C8 1.328(3) . ? N4 C7 1.338(3) . ? N5 C15 1.519(2) . ? N5 C23 1.520(2) . ? N5 C11 1.520(2) . ? N5 C19 1.523(2) . ? C1 C2 1.379(3) . ? C1 C5 1.505(3) . ? C3 C4 1.385(3) . ? C6 C7 1.377(3) . ? C6 C10 1.505(3) . ? C8 C9 1.383(3) . ? C11 C12 1.513(3) . ? C12 C13 1.511(3) . ? C13 C14 1.516(3) . ? C15 C16 1.516(3) . ? C16 C17 1.516(3) . ? C17 C18 1.512(3) . ? C19 C20 1.511(3) . ? C20 C21 1.528(3) . ? C21 C22 1.517(3) . ? C23 C24 1.521(3) . ? C24 C25 1.529(3) . ? C25 C26 1.493(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 O2 V1 O1 106.50(6) . . ? O2 V1 O3 97.36(6) . . ? O1 V1 O3 99.71(6) . . ? O2 V1 O5 100.49(6) . . ? O1 V1 O5 97.12(6) . . ? O3 V1 O5 150.81(5) . . ? O2 V1 N3 88.48(6) . . ? O1 V1 N3 164.07(6) . . ? O3 V1 N3 83.32(5) . . ? O5 V1 N3 74.31(5) . . ? O2 V1 N1 162.36(6) . . ? O1 V1 N1 90.29(6) . . ? O3 V1 N1 73.98(5) . . ? O5 V1 N1 82.29(5) . . ? N3 V1 N1 75.42(5) . . ? C5 O3 V1 124.83(12) . . ? C10 O5 V1 123.76(12) . . ? C4 N1 C1 117.42(16) . . ? C4 N1 V1 132.19(13) . . ? C1 N1 V1 110.26(12) . . ? C3 N2 C2 115.76(18) . . ? C9 N3 C6 117.34(16) . . ? C9 N3 V1 131.55(13) . . ? C6 N3 V1 110.55(11) . . ? C8 N4 C7 115.91(17) . . ? C15 N5 C23 111.12(14) . . ? C15 N5 C11 111.43(14) . . ? C23 N5 C11 106.59(13) . . ? C15 N5 C19 105.48(13) . . ? C23 N5 C19 111.22(14) . . ? C11 N5 C19 111.09(14) . . ? N1 C1 C2 120.64(19) . . ? N1 C1 C5 115.44(17) . . ? C2 C1 C5 123.92(18) . . ? N2 C2 C1 122.7(2) . . ? N2 C3 C4 122.4(2) . . ? N1 C4 C3 120.93(19) . . ? O4 C5 O3 125.96(19) . . ? O4 C5 C1 119.22(18) . . ? O3 C5 C1 114.81(17) . . ? N3 C6 C7 120.96(18) . . ? N3 C6 C10 115.18(16) . . ? C7 C6 C10 123.86(17) . . ? N4 C7 C6 122.34(19) . . ? N4 C8 C9 122.73(19) . . ? N3 C9 C8 120.65(18) . . ? O6 C10 O5 125.28(18) . . ? O6 C10 C6 120.05(17) . . ? O5 C10 C6 114.66(16) . . ? C12 C11 N5 115.78(14) . . ? C13 C12 C11 111.36(16) . . ? C12 C13 C14 112.19(19) . . ? C16 C15 N5 116.83(14) . . ? C17 C16 C15 109.51(15) . . ? C18 C17 C16 113.39(17) . . ? C20 C19 N5 116.09(14) . . ? C19 C20 C21 109.77(16) . . ? C22 C21 C20 113.83(19) . . ? N5 C23 C24 115.35(14) . . ? C23 C24 C25 110.87(16) . . ? C26 C25 C24 114.13(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 V1 O3 C5 170.17(14) . . . . ? O1 V1 O3 C5 -81.61(14) . . . . ? O5 V1 O3 C5 42.8(2) . . . . ? N3 V1 O3 C5 82.59(14) . . . . ? N1 V1 O3 C5 5.89(13) . . . . ? O2 V1 O5 C10 -75.16(14) . . . . ? O1 V1 O5 C10 176.52(13) . . . . ? O3 V1 O5 C10 51.61(19) . . . . ? N3 V1 O5 C10 10.25(13) . . . . ? N1 V1 O5 C10 87.19(13) . . . . ? O2 V1 N1 C4 114.7(2) . . . . ? O1 V1 N1 C4 -82.87(16) . . . . ? O3 V1 N1 C4 177.10(17) . . . . ? O5 V1 N1 C4 14.28(16) . . . . ? N3 V1 N1 C4 89.99(16) . . . . ? O2 V1 N1 C1 -69.6(2) . . . . ? O1 V1 N1 C1 92.84(12) . . . . ? O3 V1 N1 C1 -7.19(11) . . . . ? O5 V1 N1 C1 -170.02(12) . . . . ? N3 V1 N1 C1 -94.30(12) . . . . ? O2 V1 N3 C9 -80.28(16) . . . . ? O1 V1 N3 C9 119.3(2) . . . . ? O3 V1 N3 C9 17.31(16) . . . . ? O5 V1 N3 C9 178.37(17) . . . . ? N1 V1 N3 C9 92.44(16) . . . . ? O2 V1 N3 C6 90.66(12) . . . . ? O1 V1 N3 C6 -69.7(3) . . . . ? O3 V1 N3 C6 -171.75(12) . . . . ? O5 V1 N3 C6 -10.69(11) . . . . ? N1 V1 N3 C6 -96.62(12) . . . . ? C4 N1 C1 C2 3.5(3) . . . . ? V1 N1 C1 C2 -172.92(15) . . . . ? C4 N1 C1 C5 -175.81(16) . . . . ? V1 N1 C1 C5 7.77(18) . . . . ? C3 N2 C2 C1 -1.3(3) . . . . ? N1 C1 C2 N2 -2.0(3) . . . . ? C5 C1 C2 N2 177.28(19) . . . . ? C2 N2 C3 C4 2.9(3) . . . . ? C1 N1 C4 C3 -1.9(3) . . . . ? V1 N1 C4 C3 173.53(13) . . . . ? N2 C3 C4 N1 -1.4(3) . . . . ? V1 O3 C5 O4 177.64(15) . . . . ? V1 O3 C5 C1 -3.6(2) . . . . ? N1 C1 C5 O4 174.98(17) . . . . ? C2 C1 C5 O4 -4.3(3) . . . . ? N1 C1 C5 O3 -3.9(2) . . . . ? C2 C1 C5 O3 176.84(18) . . . . ? C9 N3 C6 C7 2.8(3) . . . . ? V1 N3 C6 C7 -169.59(14) . . . . ? C9 N3 C6 C10 -177.33(15) . . . . ? V1 N3 C6 C10 10.30(18) . . . . ? C8 N4 C7 C6 -1.5(3) . . . . ? N3 C6 C7 N4 -1.2(3) . . . . ? C10 C6 C7 N4 178.96(18) . . . . ? C7 N4 C8 C9 2.6(3) . . . . ? C6 N3 C9 C8 -1.8(3) . . . . ? V1 N3 C9 C8 168.65(13) . . . . ? N4 C8 C9 N3 -0.9(3) . . . . ? V1 O5 C10 O6 173.33(15) . . . . ? V1 O5 C10 C6 -7.9(2) . . . . ? N3 C6 C10 O6 175.64(17) . . . . ? C7 C6 C10 O6 -4.5(3) . . . . ? N3 C6 C10 O5 -3.2(2) . . . . ? C7 C6 C10 O5 176.71(17) . . . . ? C15 N5 C11 C12 54.6(2) . . . . ? C23 N5 C11 C12 175.96(17) . . . . ? C19 N5 C11 C12 -62.7(2) . . . . ? N5 C11 C12 C13 -176.10(17) . . . . ? C11 C12 C13 C14 -179.84(19) . . . . ? C23 N5 C15 C16 -61.7(2) . . . . ? C11 N5 C15 C16 57.0(2) . . . . ? C19 N5 C15 C16 177.65(16) . . . . ? N5 C15 C16 C17 -171.22(16) . . . . ? C15 C16 C17 C18 -173.24(18) . . . . ? C15 N5 C19 C20 178.38(17) . . . . ? C23 N5 C19 C20 57.8(2) . . . . ? C11 N5 C19 C20 -60.7(2) . . . . ? N5 C19 C20 C21 -172.03(17) . . . . ? C19 C20 C21 C22 73.1(2) . . . . ? C15 N5 C23 C24 -65.7(2) . . . . ? C11 N5 C23 C24 172.73(17) . . . . ? C19 N5 C23 C24 51.5(2) . . . . ? N5 C23 C24 C25 -179.57(17) . . . . ? C23 C24 C25 C26 -67.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 25.89 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.269 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.046 #---------------------------------------------------------------- data_compound2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C30 H48 N3 O6 V' _chemical_formula_weight 597.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'V' 'V' 0.3005 0.5294 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.1906(8) _cell_length_b 18.1294(16) _cell_length_c 16.5682(10) _cell_angle_alpha 90.00 _cell_angle_beta 105.831(7) _cell_angle_gamma 90.00 _cell_volume 3233.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 26.05 _exptl_crystal_description bloc _exptl_crystal_colour 'light violet' _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.228 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1280 _exptl_absorpt_coefficient_mu 0.350 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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_type 'IPDS, Stoe & Cie Company, Germany' _diffrn_measurement_method 'Phi oscillation scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24916 _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 25.85 _reflns_number_total 6031 _reflns_number_gt 4359 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, Stoe & Cie Company, Germany' _computing_cell_refinement 'CELL, Stoe & Cie Company, Germany' _computing_data_reduction 'XRED, Stoe & Cie Company, Germany' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON97 (Spek, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0665P)^2^+0.0000P] 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 6031 _refine_ls_number_parameters 391 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0577 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.1028 _refine_ls_wR_factor_gt 0.0972 _refine_ls_goodness_of_fit_ref 0.952 _refine_ls_restrained_S_all 0.966 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.53519(3) 0.528386(16) 0.75758(2) 0.03138(11) Uani 1 d . . . O1 O 0.35730(12) 0.52978(7) 0.75667(9) 0.0380(3) Uani 1 d . . . O2 O 0.47729(13) 0.56641(8) 0.87703(9) 0.0420(3) Uani 1 d . . . O3 O 0.68874(12) 0.59016(7) 0.79122(9) 0.0376(3) Uani 1 d . . . O4 O 0.52103(12) 0.65490(7) 0.74251(8) 0.0355(3) Uani 1 d . . . O5 O 0.51593(14) 0.51361(7) 0.65883(9) 0.0420(4) Uani 1 d . . . O6 O 0.58694(13) 0.45115(7) 0.80479(9) 0.0405(3) Uani 1 d . . . N1 N 0.3772(2) 0.58027(12) 1.00832(16) 0.0534(5) Uani 1 d . . . H4N H 0.377(2) 0.5717(14) 1.054(2) 0.059(9) Uiso 1 d . A 2 H3N H 0.441(2) 0.5712(14) 0.9928(18) 0.054(8) Uiso 1 d . B 2 N2 N 0.53783(18) 0.80328(11) 0.73728(12) 0.0439(5) Uani 1 d . . . H1N H 0.486(2) 0.7651(13) 0.7247(14) 0.043(6) Uiso 1 d . . . H2N H 0.510(2) 0.8448(14) 0.7224(15) 0.050(7) Uiso 1 d . . . N3 N 0.47109(15) 0.80912(8) 0.98093(10) 0.0349(4) Uani 1 d . . . C1 C 0.36925(19) 0.55179(10) 0.83293(13) 0.0352(4) Uani 1 d . . . C2 C 0.25801(19) 0.55732(10) 0.86362(13) 0.0382(5) Uani 1 d . . . C3 C 0.2666(2) 0.56921(11) 0.94875(15) 0.0443(5) Uani 1 d . . . C4 C 0.1553(3) 0.57119(14) 0.97289(18) 0.0614(7) Uani 1 d . . . H4 H 0.1582 0.5797 1.0287 0.074 Uiso 1 calc R . . C5 C 0.0427(3) 0.56068(16) 0.9151(2) 0.0718(8) Uani 1 d . . . H5 H -0.0295 0.5617 0.9326 0.086 Uiso 1 calc R . . C6 C 0.0342(2) 0.54858(15) 0.83150(19) 0.0629(7) Uani 1 d . . . H6 H -0.0426 0.5417 0.7928 0.076 Uiso 1 calc R . . C7 C 0.1419(2) 0.54691(12) 0.80648(16) 0.0474(5) Uani 1 d . . . H7 H 0.1371 0.5387 0.7503 0.057 Uiso 1 calc R . . C8 C 0.63771(18) 0.65383(10) 0.77276(12) 0.0309(4) Uani 1 d . . . C9 C 0.71361(17) 0.72116(10) 0.78774(12) 0.0329(4) Uani 1 d . . . C10 C 0.8419(2) 0.71414(12) 0.82177(16) 0.0491(6) Uani 1 d . . . H10 H 0.8765 0.6673 0.8325 0.059 Uiso 1 calc R . . C11 C 0.9181(2) 0.77489(14) 0.83969(19) 0.0636(7) Uani 1 d . . . H11 H 1.0034 0.7692 0.8616 0.076 Uiso 1 calc R . . C12 C 0.8666(2) 0.84431(13) 0.82480(18) 0.0604(7) Uani 1 d . . . H12 H 0.9177 0.8856 0.8379 0.073 Uiso 1 calc R . . C13 C 0.7417(2) 0.85336(11) 0.79108(15) 0.0466(5) Uani 1 d . . . H13 H 0.7090 0.9007 0.7811 0.056 Uiso 1 calc R . . C14 C 0.66180(18) 0.79221(10) 0.77121(12) 0.0337(4) Uani 1 d . . . C15 C 0.3923(2) 0.84565(12) 1.03109(13) 0.0424(5) Uani 1 d . . . H15A H 0.4456 0.8570 1.0864 0.051 Uiso 1 calc R . . H15B H 0.3619 0.8921 1.0042 0.051 Uiso 1 calc R . . C16 C 0.2827(2) 0.80229(14) 1.04161(15) 0.0513(6) Uani 1 d . . . H16A H 0.3116 0.7564 1.0704 0.062 Uiso 1 calc R . . H16B H 0.2281 0.7904 0.9868 0.062 Uiso 1 calc R . . C17 C 0.2114(3) 0.84583(18) 1.0913(2) 0.0746(8) Uani 1 d . . . H17A H 0.2598 0.8472 1.1496 0.090 Uiso 1 calc R . . H17B H 0.2022 0.8962 1.0708 0.090 Uiso 1 calc R . . C18 C 0.0870(3) 0.8159(2) 1.0871(2) 0.0989(11) Uani 1 d . . . H18A H 0.0549 0.8396 1.1286 0.148 Uiso 1 calc R . . H18B H 0.0930 0.7638 1.0975 0.148 Uiso 1 calc R . . H18C H 0.0322 0.8249 1.0324 0.148 Uiso 1 calc R . . C19 C 0.39038(19) 0.78122(11) 0.89729(12) 0.0383(5) Uani 1 d . . . H19A H 0.4439 0.7615 0.8652 0.046 Uiso 1 calc R . . H19B H 0.3394 0.7410 0.9077 0.046 Uiso 1 calc R . . C20 C 0.3066(2) 0.83888(12) 0.84493(14) 0.0453(5) Uani 1 d . . . H20A H 0.3570 0.8781 0.8316 0.054 Uiso 1 calc R . . H20B H 0.2546 0.8601 0.8772 0.054 Uiso 1 calc R . . C21 C 0.2247(2) 0.80675(16) 0.76414(15) 0.0588(7) Uani 1 d . . . H21A H 0.1754 0.7668 0.7772 0.071 Uiso 1 calc R . . H21B H 0.2764 0.7867 0.7310 0.071 Uiso 1 calc R . . C22 C 0.1387(3) 0.86529(19) 0.71326(18) 0.0775(9) Uani 1 d . . . H22A H 0.0908 0.8443 0.6613 0.116 Uiso 1 calc R . . H22B H 0.1872 0.9056 0.7019 0.116 Uiso 1 calc R . . H22C H 0.0837 0.8829 0.7445 0.116 Uiso 1 calc R . . C23 C 0.56223(19) 0.86587(11) 0.96429(13) 0.0391(5) Uani 1 d . . . H23A H 0.6016 0.8452 0.9240 0.047 Uiso 1 calc R . . H23B H 0.5156 0.9089 0.9386 0.047 Uiso 1 calc R . . C24 C 0.6631(2) 0.89070(13) 1.04085(15) 0.0512(6) Uani 1 d . . . H24A H 0.6255 0.9141 1.0805 0.061 Uiso 1 calc R . . H24B H 0.7097 0.8482 1.0680 0.061 Uiso 1 calc R . . C25 C 0.7495(3) 0.94422(15) 1.0156(2) 0.0744(9) Uani 1 d . . . H25A H 0.7013 0.9843 0.9839 0.089 Uiso 1 calc R . . H25B H 0.7917 0.9193 0.9794 0.089 Uiso 1 calc R . . C26 C 0.8456(3) 0.97566(19) 1.0913(3) 0.1064(14) Uani 1 d . . . H26A H 0.9027 1.0064 1.0726 0.160 Uiso 1 calc R . . H26B H 0.8903 0.9360 1.1247 0.160 Uiso 1 calc R . . H26C H 0.8046 1.0045 1.1244 0.160 Uiso 1 calc R . . C27 C 0.5399(2) 0.74439(11) 1.03113(13) 0.0426(5) Uani 1 d . . . H27A H 0.5826 0.7616 1.0870 0.051 Uiso 1 calc R . . H27B H 0.4794 0.7079 1.0369 0.051 Uiso 1 calc R . . C28 C 0.6334(2) 0.70740(12) 0.99379(16) 0.0500(6) Uani 1 d . . . H28A H 0.6862 0.7443 0.9787 0.060 Uiso 1 calc R . . H28B H 0.5906 0.6808 0.9434 0.060 Uiso 1 calc R . . C29 C 0.7124(3) 0.65393(16) 1.0577(2) 0.0725(8) Uani 1 d D . . H29A H 0.7474 0.6800 1.1100 0.087 Uiso 0.75 calc PR C 1 H29B H 0.6597 0.6149 1.0687 0.087 Uiso 0.75 calc PR C 1 H29C H 0.7009 0.6064 1.0293 0.087 Uiso 0.25 d PR C 2 H29D H 0.6796 0.6488 1.1053 0.087 Uiso 0.25 d PR C 2 C30 C 0.8150(3) 0.62066(19) 1.0287(2) 0.0560(8) Uani 0.75 d PD D 1 H30A H 0.8639 0.5892 1.0719 0.084 Uiso 0.75 calc PR D 1 H30B H 0.8666 0.6591 1.0167 0.084 Uiso 0.75 calc PR D 1 H30C H 0.7808 0.5922 0.9789 0.084 Uiso 0.75 calc PR D 1 C30A C 0.8239(9) 0.6639(8) 1.0918(10) 0.091(5) Uani 0.25 d PD D 2 H30D H 0.8615 0.6182 1.1146 0.137 Uiso 0.25 calc PR D 2 H30E H 0.8332 0.6994 1.1361 0.137 Uiso 0.25 calc PR D 2 H30F H 0.8636 0.6820 1.0511 0.137 Uiso 0.25 calc PR D 2 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 V1 0.0468(2) 0.02259(16) 0.02687(19) -0.00073(13) 0.01365(14) -0.00114(14) O1 0.0475(8) 0.0361(7) 0.0324(8) -0.0006(6) 0.0141(6) -0.0029(6) O2 0.0495(9) 0.0428(8) 0.0353(9) -0.0011(6) 0.0142(7) 0.0003(6) O3 0.0443(7) 0.0276(7) 0.0400(9) 0.0032(6) 0.0098(6) 0.0016(6) O4 0.0393(8) 0.0310(7) 0.0350(8) -0.0015(5) 0.0080(6) -0.0025(6) O5 0.0640(9) 0.0356(8) 0.0301(8) -0.0029(6) 0.0188(7) -0.0046(6) O6 0.0558(8) 0.0279(7) 0.0414(9) 0.0041(6) 0.0192(7) 0.0007(6) N1 0.0767(16) 0.0568(13) 0.0323(13) 0.0054(9) 0.0241(12) 0.0034(11) N2 0.0493(11) 0.0273(9) 0.0554(13) 0.0010(8) 0.0150(9) 0.0060(9) N3 0.0500(9) 0.0308(8) 0.0229(9) -0.0024(6) 0.0082(7) 0.0018(7) C1 0.0506(12) 0.0256(9) 0.0313(12) 0.0052(8) 0.0143(9) 0.0019(8) C2 0.0528(12) 0.0280(9) 0.0382(13) 0.0083(8) 0.0200(10) 0.0088(9) C3 0.0629(14) 0.0321(11) 0.0439(14) 0.0093(9) 0.0248(11) 0.0100(9) C4 0.0799(19) 0.0616(16) 0.0558(17) 0.0125(12) 0.0407(15) 0.0207(13) C5 0.0636(17) 0.0813(19) 0.085(2) 0.0247(17) 0.0450(17) 0.0262(14) C6 0.0495(14) 0.0697(17) 0.072(2) 0.0137(14) 0.0204(13) 0.0138(12) C7 0.0507(13) 0.0463(12) 0.0469(14) 0.0080(10) 0.0160(11) 0.0092(10) C8 0.0443(11) 0.0300(10) 0.0208(10) 0.0005(7) 0.0132(8) 0.0007(8) C9 0.0411(10) 0.0328(10) 0.0269(11) -0.0010(8) 0.0127(8) -0.0031(8) C10 0.0448(12) 0.0425(12) 0.0576(16) 0.0012(10) 0.0097(11) 0.0009(10) C11 0.0437(13) 0.0632(17) 0.079(2) -0.0057(13) 0.0081(13) -0.0128(11) C12 0.0641(16) 0.0478(14) 0.0715(19) -0.0136(12) 0.0221(13) -0.0254(12) C13 0.0648(15) 0.0317(11) 0.0476(14) -0.0047(9) 0.0227(11) -0.0090(10) C14 0.0489(11) 0.0310(10) 0.0256(11) -0.0027(8) 0.0178(9) -0.0023(8) C15 0.0551(13) 0.0452(12) 0.0268(12) -0.0058(9) 0.0110(9) 0.0076(10) C16 0.0588(14) 0.0561(14) 0.0411(14) -0.0018(10) 0.0174(11) 0.0075(11) C17 0.0732(18) 0.086(2) 0.075(2) -0.0146(16) 0.0384(16) 0.0019(15) C18 0.083(2) 0.128(3) 0.091(3) 0.005(2) 0.0328(19) 0.021(2) C19 0.0528(12) 0.0362(11) 0.0255(11) -0.0069(8) 0.0099(9) -0.0039(9) C20 0.0522(13) 0.0511(13) 0.0301(12) -0.0001(9) 0.0072(10) 0.0006(10) C21 0.0437(12) 0.0867(18) 0.0414(15) -0.0111(12) 0.0038(11) -0.0006(12) C22 0.0531(15) 0.118(3) 0.0518(18) 0.0089(16) -0.0018(13) 0.0031(16) C23 0.0515(12) 0.0302(10) 0.0348(12) -0.0007(8) 0.0103(9) -0.0006(9) C24 0.0520(13) 0.0537(13) 0.0449(14) -0.0172(11) 0.0081(11) 0.0045(10) C25 0.0645(16) 0.0501(15) 0.094(2) -0.0069(14) -0.0037(15) -0.0093(13) C26 0.0649(18) 0.084(2) 0.143(4) -0.052(2) -0.018(2) -0.0023(17) C27 0.0609(13) 0.0355(11) 0.0317(12) 0.0070(8) 0.0132(10) 0.0067(9) C28 0.0611(14) 0.0416(12) 0.0513(15) 0.0103(10) 0.0220(11) 0.0110(10) C29 0.0761(19) 0.0684(18) 0.080(2) 0.0333(15) 0.0329(16) 0.0285(15) C30 0.0589(19) 0.0530(19) 0.054(2) 0.0003(16) 0.0125(16) 0.0140(16) C30A 0.045(7) 0.108(11) 0.104(12) 0.024(9) -0.009(7) -0.005(6) _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 O5 1.6132(14) . ? V1 O6 1.6312(13) . ? V1 O1 1.9868(14) . ? V1 O3 1.9987(14) . ? V1 O4 2.3079(13) . ? V1 O2 2.3476(15) . ? V1 C8 2.5286(18) . ? V1 C1 2.540(2) . ? O1 C1 1.297(2) . ? O2 C1 1.258(2) . ? O3 C8 1.287(2) . ? O4 C8 1.265(2) . ? N1 C3 1.371(3) . ? N2 C14 1.362(3) . ? N3 C15 1.518(3) . ? N3 C19 1.520(2) . ? N3 C27 1.521(2) . ? N3 C23 1.526(3) . ? C1 C2 1.471(3) . ? C2 C7 1.396(3) . ? C2 C3 1.404(3) . ? C3 C4 1.408(3) . ? C4 C5 1.373(4) . ? C5 C6 1.379(4) . ? C6 C7 1.377(3) . ? C8 C9 1.469(3) . ? C9 C10 1.397(3) . ? C9 C14 1.408(3) . ? C10 C11 1.375(3) . ? C11 C12 1.378(4) . ? C12 C13 1.367(3) . ? C13 C14 1.406(3) . ? C15 C16 1.506(3) . ? C16 C17 1.516(3) . ? C17 C18 1.478(4) . ? C19 C20 1.510(3) . ? C20 C21 1.517(3) . ? C21 C22 1.523(4) . ? C23 C24 1.518(3) . ? C24 C25 1.507(4) . ? C25 C26 1.523(4) . ? C27 C28 1.510(3) . ? C28 C29 1.527(3) . ? C29 C30A 1.234(10) . ? C29 C30 1.488(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 O5 V1 O6 105.99(7) . . ? O5 V1 O1 97.93(7) . . ? O6 V1 O1 103.80(6) . . ? O5 V1 O3 104.04(7) . . ? O6 V1 O3 100.46(6) . . ? O1 V1 O3 141.11(6) . . ? O5 V1 O4 93.96(6) . . ? O6 V1 O4 155.49(6) . . ? O1 V1 O4 86.99(5) . . ? O3 V1 O4 60.12(5) . . ? O5 V1 O2 155.85(7) . . ? O6 V1 O2 89.51(6) . . ? O1 V1 O2 59.75(5) . . ? O3 V1 O2 90.82(5) . . ? O4 V1 O2 76.87(5) . . ? O5 V1 C8 100.47(7) . . ? O6 V1 C8 129.22(7) . . ? O1 V1 C8 114.57(6) . . ? O3 V1 C8 30.25(6) . . ? O4 V1 C8 29.87(5) . . ? O2 V1 C8 82.77(6) . . ? O5 V1 C1 127.80(7) . . ? O6 V1 C1 96.85(7) . . ? O1 V1 C1 30.26(6) . . ? O3 V1 C1 117.23(6) . . ? O4 V1 C1 81.34(5) . . ? O2 V1 C1 29.51(6) . . ? C8 V1 C1 99.99(6) . . ? C1 O1 V1 99.19(12) . . ? C1 O2 V1 83.75(12) . . ? C8 O3 V1 98.30(11) . . ? C8 O4 V1 84.77(10) . . ? C15 N3 C19 110.79(15) . . ? C15 N3 C27 108.67(15) . . ? C19 N3 C27 109.16(15) . . ? C15 N3 C23 108.74(15) . . ? C19 N3 C23 108.65(15) . . ? C27 N3 C23 110.82(15) . . ? O2 C1 O1 117.25(18) . . ? O2 C1 C2 123.68(19) . . ? O1 C1 C2 119.06(18) . . ? O2 C1 V1 66.75(11) . . ? O1 C1 V1 50.55(9) . . ? C2 C1 V1 169.24(15) . . ? C7 C2 C3 119.9(2) . . ? C7 C2 C1 118.4(2) . . ? C3 C2 C1 121.69(19) . . ? N1 C3 C2 123.1(2) . . ? N1 C3 C4 119.1(2) . . ? C2 C3 C4 117.8(2) . . ? C5 C4 C3 120.9(3) . . ? C4 C5 C6 121.4(2) . . ? C7 C6 C5 118.7(3) . . ? C6 C7 C2 121.4(2) . . ? O4 C8 O3 116.81(16) . . ? O4 C8 C9 122.76(16) . . ? O3 C8 C9 120.43(17) . . ? O4 C8 V1 65.36(9) . . ? O3 C8 V1 51.46(9) . . ? C9 C8 V1 171.83(14) . . ? C10 C9 C14 119.00(18) . . ? C10 C9 C8 118.38(17) . . ? C14 C9 C8 122.60(17) . . ? C11 C10 C9 121.5(2) . . ? C10 C11 C12 119.3(2) . . ? C13 C12 C11 120.9(2) . . ? C12 C13 C14 121.0(2) . . ? N2 C14 C13 119.44(18) . . ? N2 C14 C9 122.27(18) . . ? C13 C14 C9 118.29(19) . . ? C16 C15 N3 116.63(17) . . ? C15 C16 C17 110.9(2) . . ? C18 C17 C16 114.4(3) . . ? C20 C19 N3 114.52(16) . . ? C19 C20 C21 111.84(19) . . ? C20 C21 C22 111.1(2) . . ? C24 C23 N3 115.47(18) . . ? C25 C24 C23 110.2(2) . . ? C24 C25 C26 112.0(3) . . ? C28 C27 N3 115.00(17) . . ? C27 C28 C29 109.4(2) . . ? C30A C29 C30 55.6(8) . . ? C30A C29 C28 123.1(7) . . ? C30 C29 C28 112.7(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 V1 O1 C1 -171.51(11) . . . . ? O6 V1 O1 C1 79.79(12) . . . . ? O3 V1 O1 C1 -47.24(15) . . . . ? O4 V1 O1 C1 -77.93(11) . . . . ? O2 V1 O1 C1 -1.38(10) . . . . ? C8 V1 O1 C1 -66.12(12) . . . . ? O5 V1 O2 C1 25.9(2) . . . . ? O6 V1 O2 C1 -104.91(11) . . . . ? O1 V1 O2 C1 1.42(10) . . . . ? O3 V1 O2 C1 154.63(11) . . . . ? O4 V1 O2 C1 95.63(11) . . . . ? C8 V1 O2 C1 125.41(11) . . . . ? O5 V1 O3 C8 86.73(12) . . . . ? O6 V1 O3 C8 -163.71(12) . . . . ? O1 V1 O3 C8 -35.74(16) . . . . ? O4 V1 O3 C8 0.26(10) . . . . ? O2 V1 O3 C8 -74.05(11) . . . . ? C1 V1 O3 C8 -60.33(13) . . . . ? O5 V1 O4 C8 -104.19(12) . . . . ? O6 V1 O4 C8 40.6(2) . . . . ? O1 V1 O4 C8 158.05(11) . . . . ? O3 V1 O4 C8 -0.26(10) . . . . ? O2 V1 O4 C8 98.43(11) . . . . ? C1 V1 O4 C8 128.15(11) . . . . ? V1 O2 C1 O1 -2.11(15) . . . . ? V1 O2 C1 C2 176.96(17) . . . . ? V1 O1 C1 O2 2.51(18) . . . . ? V1 O1 C1 C2 -176.61(14) . . . . ? O5 V1 C1 O2 -166.91(10) . . . . ? O6 V1 C1 O2 76.71(11) . . . . ? O1 V1 C1 O2 -177.57(18) . . . . ? O3 V1 C1 O2 -28.80(12) . . . . ? O4 V1 C1 O2 -78.62(11) . . . . ? C8 V1 C1 O2 -55.18(11) . . . . ? O5 V1 C1 O1 10.66(14) . . . . ? O6 V1 C1 O1 -105.71(11) . . . . ? O3 V1 C1 O1 148.78(10) . . . . ? O4 V1 C1 O1 98.96(11) . . . . ? O2 V1 C1 O1 177.57(18) . . . . ? C8 V1 C1 O1 122.39(11) . . . . ? O5 V1 C1 C2 26.8(7) . . . . ? O6 V1 C1 C2 -89.6(7) . . . . ? O1 V1 C1 C2 16.1(7) . . . . ? O3 V1 C1 C2 164.9(7) . . . . ? O4 V1 C1 C2 115.0(7) . . . . ? O2 V1 C1 C2 -166.3(8) . . . . ? C8 V1 C1 C2 138.5(7) . . . . ? O2 C1 C2 C7 173.59(18) . . . . ? O1 C1 C2 C7 -7.4(3) . . . . ? V1 C1 C2 C7 -21.5(8) . . . . ? O2 C1 C2 C3 -9.4(3) . . . . ? O1 C1 C2 C3 169.62(17) . . . . ? V1 C1 C2 C3 155.5(6) . . . . ? C7 C2 C3 N1 -179.6(2) . . . . ? C1 C2 C3 N1 3.5(3) . . . . ? C7 C2 C3 C4 -0.9(3) . . . . ? C1 C2 C3 C4 -177.83(18) . . . . ? N1 C3 C4 C5 179.7(2) . . . . ? C2 C3 C4 C5 1.0(3) . . . . ? C3 C4 C5 C6 -0.6(4) . . . . ? C4 C5 C6 C7 0.2(4) . . . . ? C5 C6 C7 C2 -0.2(4) . . . . ? C3 C2 C7 C6 0.5(3) . . . . ? C1 C2 C7 C6 177.6(2) . . . . ? V1 O4 C8 O3 0.40(16) . . . . ? V1 O4 C8 C9 -178.92(17) . . . . ? V1 O3 C8 O4 -0.46(18) . . . . ? V1 O3 C8 C9 178.87(15) . . . . ? O5 V1 C8 O4 79.59(12) . . . . ? O6 V1 C8 O4 -159.59(11) . . . . ? O1 V1 C8 O4 -24.23(12) . . . . ? O3 V1 C8 O4 179.55(18) . . . . ? O2 V1 C8 O4 -76.18(10) . . . . ? C1 V1 C8 O4 -52.13(11) . . . . ? O5 V1 C8 O3 -99.96(12) . . . . ? O6 V1 C8 O3 20.86(15) . . . . ? O1 V1 C8 O3 156.22(11) . . . . ? O4 V1 C8 O3 -179.55(18) . . . . ? O2 V1 C8 O3 104.27(12) . . . . ? C1 V1 C8 O3 128.32(12) . . . . ? O5 V1 C8 C9 -106.8(10) . . . . ? O6 V1 C8 C9 14.0(10) . . . . ? O1 V1 C8 C9 149.3(10) . . . . ? O3 V1 C8 C9 -6.9(9) . . . . ? O4 V1 C8 C9 173.6(10) . . . . ? O2 V1 C8 C9 97.4(10) . . . . ? C1 V1 C8 C9 121.4(10) . . . . ? O4 C8 C9 C10 179.72(19) . . . . ? O3 C8 C9 C10 0.4(3) . . . . ? V1 C8 C9 C10 6.7(11) . . . . ? O4 C8 C9 C14 1.4(3) . . . . ? O3 C8 C9 C14 -177.86(18) . . . . ? V1 C8 C9 C14 -171.6(9) . . . . ? C14 C9 C10 C11 0.3(4) . . . . ? C8 C9 C10 C11 -178.1(2) . . . . ? C9 C10 C11 C12 0.9(4) . . . . ? C10 C11 C12 C13 -1.3(4) . . . . ? C11 C12 C13 C14 0.5(4) . . . . ? C12 C13 C14 N2 -179.7(2) . . . . ? C12 C13 C14 C9 0.6(3) . . . . ? C10 C9 C14 N2 179.3(2) . . . . ? C8 C9 C14 N2 -2.4(3) . . . . ? C10 C9 C14 C13 -1.0(3) . . . . ? C8 C9 C14 C13 177.27(19) . . . . ? C19 N3 C15 C16 50.9(2) . . . . ? C27 N3 C15 C16 -69.1(2) . . . . ? C23 N3 C15 C16 170.22(18) . . . . ? N3 C15 C16 C17 -178.9(2) . . . . ? C15 C16 C17 C18 165.8(3) . . . . ? C15 N3 C19 C20 54.2(2) . . . . ? C27 N3 C19 C20 173.88(18) . . . . ? C23 N3 C19 C20 -65.2(2) . . . . ? N3 C19 C20 C21 -177.53(19) . . . . ? C19 C20 C21 C22 178.6(2) . . . . ? C15 N3 C23 C24 68.4(2) . . . . ? C19 N3 C23 C24 -170.92(17) . . . . ? C27 N3 C23 C24 -51.0(2) . . . . ? N3 C23 C24 C25 177.80(19) . . . . ? C23 C24 C25 C26 175.1(2) . . . . ? C15 N3 C27 C28 -173.52(18) . . . . ? C19 N3 C27 C28 65.5(2) . . . . ? C23 N3 C27 C28 -54.1(2) . . . . ? N3 C27 C28 C29 169.2(2) . . . . ? C27 C28 C29 C30A -111.7(10) . . . . ? C27 C28 C29 C30 -174.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.932 _diffrn_reflns_theta_full 25.85 _diffrn_measured_fraction_theta_full 0.932 _refine_diff_density_max 0.482 _refine_diff_density_min -0.215 _refine_diff_density_rms 0.041 #----------------------------------------------------------- data_compound3b _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_sum 'C10 H14 N5 O9 V' _chemical_formula_weight 399.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'V' 'V' 0.3005 0.5294 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.1752(7) _cell_length_b 9.2884(5) _cell_length_c 14.3963(9) _cell_angle_alpha 90.00 _cell_angle_beta 111.386(6) _cell_angle_gamma 90.00 _cell_volume 1515.95(15) _cell_formula_units_Z 4 _cell_measurement_temperature 223(2) _cell_measurement_reflns_used 5000 _cell_measurement_theta_min 1.65 _cell_measurement_theta_max 26.05 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.749 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 0.716 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 223(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_type 'IPDS, Stoe & Cie Company, Germany' _diffrn_measurement_method 'Phi oscillation scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11496 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0261 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.67 _diffrn_reflns_theta_max 25.87 _reflns_number_total 2918 _reflns_number_gt 2410 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'EXPOSE, Stoe & Cie Company, Germany' _computing_cell_refinement 'CELL, Stoe & Cie Company, Germany' _computing_data_reduction 'INTEGRATE, Stoe & Cie Company,Germany' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'PLATON97 (Spek, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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 w=1/[\s^2^(Fo^2^)+(0.0497P)^2^+0.0036P] 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 2918 _refine_ls_number_parameters 258 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0339 _refine_ls_R_factor_gt 0.0260 _refine_ls_wR_factor_ref 0.0731 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.65015(2) 0.42794(3) 0.80794(2) 0.02045(10) Uani 1 d . . . O1 O 0.67658(10) 0.21373(12) 0.77771(8) 0.0243(3) Uani 1 d . . . O2 O 0.65358(11) 0.05287(13) 0.65679(9) 0.0304(3) Uani 1 d . . . O3 O 0.79197(10) 0.43915(13) 0.74871(9) 0.0249(3) Uani 1 d . . . O4 O 0.98289(11) 0.39056(14) 0.78406(10) 0.0306(3) Uani 1 d . . . O5 O 0.56783(11) 0.38104(15) 0.86740(10) 0.0340(3) Uani 1 d . . . O6 O 0.70049(11) 0.61328(14) 0.86059(10) 0.0332(3) Uani 1 d . . . O7 O 0.60466(11) 0.61662(13) 0.76843(10) 0.0322(3) Uani 1 d . . . O8 O 0.9249(2) 0.5506(2) 0.60150(16) 0.0559(5) Uani 1 d . . . H1O H 0.928(3) 0.494(3) 0.647(2) 0.069(9) Uiso 1 d . . . H2O H 0.9728(19) 0.549(3) 0.6124(19) 0.014(8) Uiso 1 d . . . O9 O 0.84548(16) 0.0119(2) 0.89679(17) 0.0509(4) Uani 1 d . . . H3O H 0.798(3) 0.069(3) 0.870(2) 0.050(8) Uiso 1 d . . . H4O H 0.855(3) 0.019(4) 0.950(3) 0.088(14) Uiso 1 d . . . N1 N 0.52642(12) 0.39122(15) 0.66000(10) 0.0216(3) Uani 1 d . . . N2 N 0.37287(13) 0.31322(18) 0.47128(11) 0.0317(4) Uani 1 d . . . N3 N 0.80552(12) 0.37769(15) 0.93041(10) 0.0217(3) Uani 1 d . . . N4 N 1.01568(13) 0.30462(16) 1.08088(11) 0.0298(3) Uani 1 d . . . N5 N 0.79142(16) -0.2091(2) 0.72622(13) 0.0293(3) Uani 1 d . . . H1N H 0.753(3) -0.125(4) 0.723(2) 0.070(9) Uiso 1 d . . . H2N H 0.746(3) -0.258(4) 0.681(3) 0.088(11) Uiso 1 d . . . H3N H 0.855(3) -0.186(4) 0.713(3) 0.106(13) Uiso 1 d . . . H4N H 0.801(3) -0.253(4) 0.782(3) 0.082(10) Uiso 1 d . . . C1 C 0.53306(14) 0.26167(18) 0.62142(12) 0.0213(3) Uani 1 d . . . C2 C 0.45624(15) 0.2232(2) 0.52731(13) 0.0278(4) Uani 1 d . . . H2 H 0.4629 0.1315 0.5022 0.033 Uiso 1 calc R . . C3 C 0.36767(15) 0.4421(2) 0.51085(14) 0.0315(4) Uani 1 d . . . H3 H 0.3098 0.5078 0.4733 0.038 Uiso 1 calc R . . C4 C 0.44358(15) 0.4829(2) 0.60451(13) 0.0276(4) Uani 1 d . . . H4 H 0.4371 0.5748 0.6293 0.033 Uiso 1 calc R . . C5 C 0.62806(14) 0.16484(17) 0.68871(12) 0.0211(3) Uani 1 d . . . C6 C 0.90506(14) 0.36364(17) 0.91156(12) 0.0208(3) Uani 1 d . . . C7 C 1.00923(15) 0.32491(18) 0.98722(13) 0.0251(4) Uani 1 d . . . H7 H 1.0776 0.3125 0.9722 0.030 Uiso 1 calc R . . C8 C 0.91580(17) 0.3228(2) 1.09788(14) 0.0322(4) Uani 1 d . . . H8 H 0.9176 0.3112 1.1633 0.039 Uiso 1 calc R . . C9 C 0.81006(16) 0.35790(19) 1.02344(13) 0.0281(4) Uani 1 d . . . H9 H 0.7414 0.3678 1.0383 0.034 Uiso 1 calc R . . C10 C 0.89378(14) 0.39914(17) 0.80608(12) 0.0216(3) Uani 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 V1 0.01719(16) 0.02553(16) 0.01781(16) -0.00141(11) 0.00542(11) 0.00038(11) O1 0.0228(6) 0.0247(6) 0.0210(6) 0.0000(5) 0.0027(5) 0.0004(5) O2 0.0339(7) 0.0270(7) 0.0285(7) -0.0014(5) 0.0092(6) 0.0052(5) O3 0.0230(6) 0.0315(6) 0.0191(6) 0.0017(5) 0.0065(5) 0.0005(5) O4 0.0259(6) 0.0393(7) 0.0300(7) -0.0034(5) 0.0144(6) 0.0012(5) O5 0.0276(7) 0.0434(8) 0.0352(7) -0.0001(6) 0.0163(6) -0.0004(6) O6 0.0304(7) 0.0332(7) 0.0315(7) -0.0056(6) 0.0056(6) 0.0005(5) O7 0.0283(7) 0.0298(6) 0.0339(7) -0.0030(6) 0.0056(6) 0.0033(5) O8 0.0585(15) 0.0595(13) 0.0505(12) 0.0226(9) 0.0208(11) 0.0036(11) O9 0.0424(9) 0.0444(10) 0.0510(12) 0.0023(9) -0.0006(8) 0.0108(8) N1 0.0179(7) 0.0270(7) 0.0192(7) 0.0000(6) 0.0061(6) 0.0007(5) N2 0.0250(8) 0.0440(9) 0.0220(8) -0.0004(7) 0.0039(6) 0.0015(7) N3 0.0214(7) 0.0232(7) 0.0188(7) -0.0016(6) 0.0053(6) -0.0017(5) N4 0.0306(8) 0.0253(8) 0.0250(8) 0.0001(6) 0.0002(7) -0.0009(6) N5 0.0275(8) 0.0301(9) 0.0246(9) -0.0007(7) 0.0028(7) -0.0017(7) C1 0.0191(8) 0.0260(8) 0.0201(8) 0.0001(7) 0.0086(7) -0.0016(6) C2 0.0255(9) 0.0343(10) 0.0226(9) -0.0025(7) 0.0076(7) -0.0009(7) C3 0.0213(9) 0.0441(11) 0.0260(9) 0.0028(8) 0.0050(7) 0.0074(8) C4 0.0235(8) 0.0326(9) 0.0262(9) 0.0004(8) 0.0083(7) 0.0069(7) C5 0.0183(8) 0.0231(8) 0.0226(9) 0.0024(7) 0.0083(7) -0.0026(6) C6 0.0212(8) 0.0177(8) 0.0220(8) -0.0041(6) 0.0061(7) -0.0029(6) C7 0.0235(8) 0.0206(8) 0.0266(9) -0.0041(7) 0.0037(7) -0.0009(7) C8 0.0408(11) 0.0325(10) 0.0197(9) 0.0021(7) 0.0067(8) -0.0042(8) C9 0.0302(9) 0.0336(10) 0.0214(9) 0.0000(7) 0.0104(8) -0.0027(8) C10 0.0225(8) 0.0206(8) 0.0211(8) -0.0048(6) 0.0070(7) -0.0029(6) _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 O5 1.5977(12) . ? V1 O7 1.8634(13) . ? V1 O6 1.8908(13) . ? V1 O1 2.0865(12) . ? V1 N3 2.1148(14) . ? V1 N1 2.1405(14) . ? V1 O3 2.1892(12) . ? O1 C5 1.283(2) . ? O2 C5 1.222(2) . ? O3 C10 1.269(2) . ? O4 C10 1.239(2) . ? O6 O7 1.4119(19) . ? N1 C4 1.339(2) . ? N1 C1 1.340(2) . ? N2 C2 1.335(2) . ? N2 C3 1.337(2) . ? N3 C9 1.333(2) . ? N3 C6 1.341(2) . ? N4 C7 1.335(2) . ? N4 C8 1.336(2) . ? C1 C2 1.383(2) . ? C1 C5 1.506(2) . ? C3 C4 1.381(3) . ? C6 C7 1.384(2) . ? C6 C10 1.510(2) . ? C8 C9 1.381(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 O5 V1 O7 104.20(6) . . ? O5 V1 O6 102.03(6) . . ? O7 V1 O6 44.18(6) . . ? O5 V1 O1 91.51(6) . . ? O7 V1 O1 152.19(5) . . ? O6 V1 O1 154.12(5) . . ? O5 V1 N3 92.20(6) . . ? O7 V1 N3 122.55(6) . . ? O6 V1 N3 78.82(5) . . ? O1 V1 N3 78.72(5) . . ? O5 V1 N1 97.95(6) . . ? O7 V1 N1 79.81(5) . . ? O6 V1 N1 123.47(6) . . ? O1 V1 N1 75.32(5) . . ? N3 V1 N1 152.30(5) . . ? O5 V1 O3 163.65(6) . . ? O7 V1 O3 91.45(5) . . ? O6 V1 O3 85.78(5) . . ? O1 V1 O3 76.15(5) . . ? N3 V1 O3 75.08(5) . . ? N1 V1 O3 89.36(5) . . ? C5 O1 V1 119.74(10) . . ? C10 O3 V1 117.04(10) . . ? O7 O6 V1 66.88(7) . . ? O6 O7 V1 68.94(7) . . ? C4 N1 C1 118.02(15) . . ? C4 N1 V1 126.60(12) . . ? C1 N1 V1 115.38(11) . . ? C2 N2 C3 116.55(16) . . ? C9 N3 C6 118.71(15) . . ? C9 N3 V1 124.39(12) . . ? C6 N3 V1 116.89(11) . . ? C7 N4 C8 116.43(15) . . ? N1 C1 C2 121.09(16) . . ? N1 C1 C5 114.70(14) . . ? C2 C1 C5 124.20(15) . . ? N2 C2 C1 121.56(17) . . ? N2 C3 C4 122.87(17) . . ? N1 C4 C3 119.91(17) . . ? O2 C5 O1 126.11(15) . . ? O2 C5 C1 120.48(15) . . ? O1 C5 C1 113.39(14) . . ? N3 C6 C7 120.15(15) . . ? N3 C6 C10 115.12(14) . . ? C7 C6 C10 124.68(15) . . ? N4 C7 C6 122.06(16) . . ? N4 C8 C9 122.76(16) . . ? N3 C9 C8 119.85(17) . . ? O4 C10 O3 126.23(16) . . ? O4 C10 C6 118.44(15) . . ? O3 C10 C6 115.30(14) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O5 V1 O1 C5 108.49(12) . . . . ? O7 V1 O1 C5 -16.66(18) . . . . ? O6 V1 O1 C5 -129.37(14) . . . . ? N3 V1 O1 C5 -159.57(12) . . . . ? N1 V1 O1 C5 10.67(11) . . . . ? O3 V1 O1 C5 -82.35(11) . . . . ? O5 V1 O3 C10 -33.1(3) . . . . ? O7 V1 O3 C10 130.12(12) . . . . ? O6 V1 O3 C10 86.27(12) . . . . ? O1 V1 O3 C10 -75.05(11) . . . . ? N3 V1 O3 C10 6.73(11) . . . . ? N1 V1 O3 C10 -150.09(12) . . . . ? O5 V1 O6 O7 -98.08(9) . . . . ? O1 V1 O6 O7 141.86(11) . . . . ? N3 V1 O6 O7 172.05(8) . . . . ? N1 V1 O6 O7 10.00(10) . . . . ? O3 V1 O6 O7 96.44(8) . . . . ? O5 V1 O7 O6 92.76(9) . . . . ? O1 V1 O7 O6 -144.71(10) . . . . ? N3 V1 O7 O6 -9.26(10) . . . . ? N1 V1 O7 O6 -171.53(9) . . . . ? O3 V1 O7 O6 -82.44(8) . . . . ? O5 V1 N1 C4 84.75(15) . . . . ? O7 V1 N1 C4 -18.34(14) . . . . ? O6 V1 N1 C4 -25.40(16) . . . . ? O1 V1 N1 C4 174.24(15) . . . . ? N3 V1 N1 C4 -164.81(13) . . . . ? O3 V1 N1 C4 -109.92(14) . . . . ? O5 V1 N1 C1 -94.00(12) . . . . ? O7 V1 N1 C1 162.90(12) . . . . ? O6 V1 N1 C1 155.84(10) . . . . ? O1 V1 N1 C1 -4.52(11) . . . . ? N3 V1 N1 C1 16.43(18) . . . . ? O3 V1 N1 C1 71.32(11) . . . . ? O5 V1 N3 C9 -15.82(15) . . . . ? O7 V1 N3 C9 92.58(14) . . . . ? O6 V1 N3 C9 86.01(14) . . . . ? O1 V1 N3 C9 -106.92(14) . . . . ? N1 V1 N3 C9 -127.58(15) . . . . ? O3 V1 N3 C9 174.58(15) . . . . ? O5 V1 N3 C6 163.40(12) . . . . ? O7 V1 N3 C6 -88.20(12) . . . . ? O6 V1 N3 C6 -94.76(12) . . . . ? O1 V1 N3 C6 72.30(12) . . . . ? N1 V1 N3 C6 51.65(18) . . . . ? O3 V1 N3 C6 -6.19(11) . . . . ? C4 N1 C1 C2 -0.4(2) . . . . ? V1 N1 C1 C2 178.49(12) . . . . ? C4 N1 C1 C5 -179.69(14) . . . . ? V1 N1 C1 C5 -0.82(17) . . . . ? C3 N2 C2 C1 0.0(3) . . . . ? N1 C1 C2 N2 0.1(3) . . . . ? C5 C1 C2 N2 179.36(15) . . . . ? C2 N2 C3 C4 0.1(3) . . . . ? C1 N1 C4 C3 0.5(2) . . . . ? V1 N1 C4 C3 -178.21(12) . . . . ? N2 C3 C4 N1 -0.4(3) . . . . ? V1 O1 C5 O2 164.90(13) . . . . ? V1 O1 C5 C1 -14.06(17) . . . . ? N1 C1 C5 O2 -169.61(14) . . . . ? C2 C1 C5 O2 11.1(2) . . . . ? N1 C1 C5 O1 9.41(19) . . . . ? C2 C1 C5 O1 -169.87(15) . . . . ? C9 N3 C6 C7 2.0(2) . . . . ? V1 N3 C6 C7 -177.29(12) . . . . ? C9 N3 C6 C10 -175.47(14) . . . . ? V1 N3 C6 C10 5.26(17) . . . . ? C8 N4 C7 C6 0.4(2) . . . . ? N3 C6 C7 N4 -2.1(2) . . . . ? C10 C6 C7 N4 175.14(15) . . . . ? C7 N4 C8 C9 1.2(3) . . . . ? C6 N3 C9 C8 -0.4(2) . . . . ? V1 N3 C9 C8 178.81(13) . . . . ? N4 C8 C9 N3 -1.3(3) . . . . ? V1 O3 C10 O4 175.86(13) . . . . ? V1 O3 C10 C6 -6.07(17) . . . . ? N3 C6 C10 O4 178.90(14) . . . . ? C7 C6 C10 O4 1.6(2) . . . . ? N3 C6 C10 O3 0.7(2) . . . . ? C7 C6 C10 O3 -176.66(15) . . . . ? _diffrn_measured_fraction_theta_max 0.934 _diffrn_reflns_theta_full 25.87 _diffrn_measured_fraction_theta_full 0.934 _refine_diff_density_max 0.409 _refine_diff_density_min -0.245 _refine_diff_density_rms 0.050 #============================================================END