Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2001 data_global _journal_coden_Cambridge 186 _publ_requested_journal 'Dalton Transactions' loop_ _publ_author_name 'Kabanos, Themistoklis A.' 'Keramidas, Anastasios D.' 'Manos, Manolis J' 'Raptopoulou, Catherine' 'Slawin, A.' 'Tasiopoulos, Anastasios J.' 'Terzis, Aris' 'Woollins, J.' _publ_contact_author_name 'Dr Themistoklis A. Kabanos' _publ_contact_author_address ; Dr Themistoklis A. Kabanos Department of Chemistry, Section of Inorganic & Analytical Chemistry University of Ioannina 45110 Ioannina GREECE ; data_1 _database_code_CSD 156232 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C27 H18 N3 O3 V.[C H4 O]0.5' _chemical_formula_structural 'C27.50 H20 N3 O3.50 V' _chemical_formula_analytical 'C27.50 H20 N3 O3.50 V' _chemical_formula_sum 'C27.50 H20 N3 O3.50 V' _chemical_formula_weight 499.40 _chemical_melting_point - _chemical_compound_source - loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'V' 'V' 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 10.9438(10) _cell_length_b 13.4026(13) _cell_length_c 16.912(2) _cell_angle_alpha 90.00 _cell_angle_beta 97.921(2) _cell_angle_gamma 90.00 _cell_volume 2456.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 106 _cell_measurement_theta_min 12 _cell_measurement_theta_max 168 _exptl_crystal_description prism _exptl_crystal_colour 'dark blue' _exptl_crystal_size_max .32 _exptl_crystal_size_mid .27 _exptl_crystal_size_min .19 _exptl_crystal_density_meas - _exptl_crystal_density_diffrn 1.350 _exptl_crystal_density_method - _exptl_crystal_F_000 1028 _exptl_absorpt_coefficient_mu 0.440 _exptl_absorpt_correction_type sadabs _exptl_absorpt_correction_T_min 0.819375 _exptl_absorpt_correction_T_max 1.000000 _exptl_special_details ; - ; _diffrn_ambient_temperature 298(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 SMART _diffrn_measurement_method CCD _diffrn_standards_number - _diffrn_standards_interval_count - _diffrn_standards_interval_time - _diffrn_standards_decay_% - _diffrn_reflns_number 10461 _diffrn_reflns_av_R_equivalents 0.0189 _diffrn_reflns_av_sigmaI/netI 0.0210 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.95 _diffrn_reflns_theta_max 23.25 _reflns_number_total 3515 _reflns_number_observed 2756 _reflns_observed_criterion >2sigma(I) _computing_data_collection SMART _computing_cell_refinement SMART/SAINT _computing_data_reduction SAINT _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics SHELXTL _computing_publication_material SHELXTL _refine_special_details ; Refinement on F^2^ for ALL reflections except for 26 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1206P)^2^+0.2070P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0012(7) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3489 _refine_ls_number_parameters 328 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_obs 0.0412 _refine_ls_wR_factor_all 0.1708 _refine_ls_wR_factor_obs 0.1326 _refine_ls_goodness_of_fit_all 0.916 _refine_ls_goodness_of_fit_obs 0.969 _refine_ls_restrained_S_all 1.101 _refine_ls_restrained_S_obs 0.969 _refine_ls_shift/esd_max 0.072 _refine_ls_shift/esd_mean 0.011 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group V1 V 0.42491(4) -0.02443(3) 1.24037(3) 0.0427(2) Uani 1 d . . N1 N 0.3788(2) 0.0101(2) 1.11722(14) 0.0455(6) Uani 1 d . . C1A C 0.3681(3) -0.0766(2) 1.0742(2) 0.0448(7) Uani 1 d . . C2 C 0.3635(3) 0.0957(2) 1.0774(2) 0.0557(8) Uani 1 d . . H2A H 0.3717(3) 0.1550(2) 1.1062(2) 0.067 Uiso 1 calc R . C3 C 0.3355(3) 0.1008(3) 0.9942(2) 0.0645(9) Uani 1 d . . H3A H 0.3238(3) 0.1624(3) 0.9689(2) 0.077 Uiso 1 calc R . C4 C 0.3257(3) 0.0153(3) 0.9509(2) 0.0668(10) Uani 1 d . . H4A H 0.3089(3) 0.0183(3) 0.8955(2) 0.080 Uiso 1 calc R . C4A C 0.3409(3) -0.0783(2) 0.9896(2) 0.0557(8) Uani 1 d . . C5 C 0.3347(3) -0.1720(3) 0.9514(2) 0.0679(9) Uani 1 d . . H5A H 0.3171(3) -0.1757(3) 0.8961(2) 0.082 Uiso 1 calc R . C6 C 0.3542(3) -0.2566(3) 0.9949(2) 0.0697(10) Uani 1 d . . H6A H 0.3504(3) -0.3176(3) 0.9684(2) 0.084 Uiso 1 calc R . C7 C 0.3801(3) -0.2557(2) 1.0789(2) 0.0588(8) Uani 1 d . . H7A H 0.3919(3) -0.3154(2) 1.1069(2) 0.071 Uiso 1 calc R . C8 C 0.3878(3) -0.1656(2) 1.1194(2) 0.0495(7) Uani 1 d . . O8 O 0.4123(2) -0.15777(14) 1.19880(12) 0.0511(5) Uani 1 d . . N11 N 0.4472(2) -0.0744(2) 1.36014(14) 0.0511(6) Uani 1 d . . C11A C 0.3364(3) -0.0729(2) 1.3897(2) 0.0517(8) Uani 1 d . . C12 C 0.5457(4) -0.1095(3) 1.4065(2) 0.0670(9) Uani 1 d . . H12A H 0.6206(4) -0.1114(3) 1.3863(2) 0.080 Uiso 1 calc R . C13 C 0.5421(5) -0.1435(3) 1.4834(2) 0.0872(12) Uani 1 d . . H13A H 0.6133(5) -0.1671(3) 1.5141(2) 0.105 Uiso 1 calc R . C14 C 0.4353(5) -0.1421(3) 1.5129(2) 0.0897(13) Uani 1 d . . H14A H 0.4329(5) -0.1644(3) 1.5648(2) 0.108 Uiso 1 calc R . C14A C 0.3249(4) -0.1074(3) 1.4670(2) 0.0719(11) Uani 1 d . . C15 C 0.2067(5) -0.1042(3) 1.4914(3) 0.0914(14) Uani 1 d . . H15A H 0.1949(5) -0.1274(3) 1.5417(3) 0.110 Uiso 1 calc R . C16 C 0.1116(5) -0.0671(3) 1.4416(3) 0.0932(15) Uani 1 d . . H16A H 0.0346(5) -0.0645(3) 1.4588(3) 0.112 Uiso 1 calc R . C17 C 0.1226(3) -0.0319(2) 1.3640(3) 0.0719(11) Uani 1 d . . H17A H 0.0539(3) -0.0071(2) 1.3314(3) 0.086 Uiso 1 calc R . C18 C 0.2365(3) -0.0346(2) 1.3370(2) 0.0516(8) Uani 1 d . . O18 O 0.2580(2) -0.00340(15) 1.26533(13) 0.0519(5) Uani 1 d . . N21 N 0.4569(2) 0.1306(2) 1.27262(13) 0.0440(6) Uani 1 d . . C21A C 0.5795(2) 0.1552(2) 1.2734(2) 0.0426(7) Uani 1 d . . C22 C 0.3801(3) 0.2018(2) 1.2881(2) 0.0567(8) Uani 1 d . . H22A H 0.2971(3) 0.1864(2) 1.2873(2) 0.068 Uiso 1 calc R . C23 C 0.4196(3) 0.2997(2) 1.3055(2) 0.0682(10) Uani 1 d . . H23A H 0.3634(3) 0.3478(2) 1.3169(2) 0.082 Uiso 1 calc R . C24A C 0.6256(3) 0.2519(2) 1.2891(2) 0.0521(8) Uani 1 d . . C24 C 0.5390(4) 0.3243(2) 1.3058(2) 0.0672(10) Uani 1 d . . H24A H 0.5646(4) 0.3896(2) 1.3172(2) 0.081 Uiso 1 calc R . C25 C 0.7528(3) 0.2688(3) 1.2873(2) 0.0651(9) Uani 1 d . . H25A H 0.7854(3) 0.3326(3) 1.2957(2) 0.078 Uiso 1 calc R . C26 C 0.8274(3) 0.1911(3) 1.2730(2) 0.0654(9) Uani 1 d . . H26A H 0.9110(3) 0.2027(3) 1.2722(2) 0.078 Uiso 1 calc R . C27 C 0.7811(3) 0.0943(3) 1.2597(2) 0.0574(8) Uani 1 d . . H27A H 0.8346(3) 0.0426(3) 1.2515(2) 0.069 Uiso 1 calc R . C28 C 0.6569(3) 0.0745(2) 1.2584(2) 0.0444(7) Uani 1 d . . O28 O 0.6038(2) -0.01295(14) 1.24419(13) 0.0495(5) Uani 1 d . . O30 O 0.0418(4) 0.0552(3) 1.1691(4) 0.079(2) Uani 0.50 d P . H30 H 0.0819(81) 0.0091(27) 1.1538(36) 0.118 Uiso 0.50 calc PR . C30 C 0.0440(7) 0.1287(7) 1.1224(6) 0.112(4) Uani 0.50 d P . H30A H -0.0385(10) 0.1524(39) 1.1066(39) 0.168 Uiso 0.50 calc PR . H30B H 0.0790(68) 0.1082(15) 1.0759(21) 0.168 Uiso 0.50 calc PR . H30C H 0.0932(60) 0.1811(22) 1.1491(16) 0.168 Uiso 0.50 calc PR . 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 0.0419(3) 0.0461(4) 0.0403(3) 0.0018(2) 0.0069(2) -0.0006(2) N1 0.0439(14) 0.0485(14) 0.0448(14) 0.0045(11) 0.0090(11) -0.0001(10) C1A 0.039(2) 0.051(2) 0.045(2) 0.0014(14) 0.0093(13) 0.0004(13) C2 0.062(2) 0.051(2) 0.055(2) 0.004(2) 0.012(2) 0.0019(15) C3 0.077(2) 0.065(2) 0.052(2) 0.016(2) 0.013(2) 0.007(2) C4 0.075(2) 0.087(3) 0.040(2) 0.009(2) 0.010(2) 0.010(2) C4A 0.048(2) 0.074(2) 0.046(2) -0.002(2) 0.0089(14) 0.004(2) C5 0.073(2) 0.080(2) 0.050(2) -0.013(2) 0.007(2) 0.002(2) C6 0.072(2) 0.066(2) 0.069(2) -0.023(2) 0.005(2) 0.002(2) C7 0.062(2) 0.050(2) 0.064(2) -0.007(2) 0.006(2) 0.0012(15) C8 0.042(2) 0.055(2) 0.052(2) -0.0026(15) 0.0071(14) -0.0014(13) O8 0.0617(13) 0.0448(11) 0.0461(12) 0.0022(9) 0.0052(10) -0.0005(9) N11 0.058(2) 0.0526(15) 0.0427(14) -0.0003(11) 0.0077(12) 0.0001(12) C11A 0.070(2) 0.044(2) 0.044(2) -0.0068(13) 0.020(2) -0.0082(15) C12 0.071(2) 0.077(2) 0.050(2) 0.007(2) 0.001(2) 0.012(2) C13 0.105(3) 0.100(3) 0.055(2) 0.014(2) 0.001(2) 0.021(3) C14 0.136(4) 0.090(3) 0.042(2) 0.012(2) 0.011(2) 0.005(3) C14A 0.107(3) 0.059(2) 0.055(2) -0.007(2) 0.033(2) -0.009(2) C15 0.126(4) 0.085(3) 0.075(3) -0.003(2) 0.056(3) -0.014(3) C16 0.096(3) 0.093(3) 0.106(4) -0.026(3) 0.070(3) -0.027(3) C17 0.064(2) 0.067(2) 0.091(3) -0.017(2) 0.033(2) -0.013(2) C18 0.052(2) 0.045(2) 0.060(2) -0.0092(15) 0.020(2) -0.0100(14) O18 0.0420(11) 0.0584(12) 0.0565(13) 0.0042(10) 0.0108(10) -0.0023(9) N21 0.0464(14) 0.0470(13) 0.0396(13) -0.0009(11) 0.0090(10) 0.0026(11) C21A 0.047(2) 0.048(2) 0.0337(15) 0.0028(12) 0.0080(13) -0.0025(13) C22 0.055(2) 0.059(2) 0.058(2) 0.003(2) 0.014(2) 0.010(2) C23 0.079(3) 0.048(2) 0.080(3) 0.001(2) 0.019(2) 0.015(2) C24A 0.064(2) 0.049(2) 0.043(2) 0.0003(14) 0.0085(15) -0.0091(15) C24 0.086(3) 0.045(2) 0.073(2) -0.003(2) 0.017(2) -0.003(2) C25 0.073(2) 0.064(2) 0.060(2) -0.006(2) 0.013(2) -0.023(2) C26 0.052(2) 0.088(3) 0.056(2) -0.005(2) 0.007(2) -0.020(2) C27 0.044(2) 0.073(2) 0.056(2) -0.008(2) 0.0088(14) 0.000(2) C28 0.047(2) 0.049(2) 0.0372(15) 0.0010(13) 0.0076(13) -0.0008(13) O28 0.0446(11) 0.0478(11) 0.0571(13) -0.0062(9) 0.0111(10) -0.0006(9) O30 0.036(2) 0.050(2) 0.147(5) 0.050(3) 0.000(3) 0.002(2) C30 0.057(5) 0.136(8) 0.150(9) 0.074(7) 0.043(5) 0.041(5) _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 O8 1.918(2) . ? V1 O18 1.952(2) . ? V1 O28 1.956(2) . ? V1 N11 2.115(2) . ? V1 N1 2.125(2) . ? V1 N21 2.164(2) . ? N1 C2 1.330(4) . ? N1 C1A 1.367(4) . ? C1A C8 1.417(4) . ? C1A C4A 1.421(4) . ? C2 C3 1.400(4) . ? C3 C4 1.357(5) . ? C4 C4A 1.415(5) . ? C4A C5 1.410(5) . ? C5 C6 1.353(5) . ? C6 C7 1.409(5) . ? C7 C8 1.386(4) . ? C8 O8 1.337(4) . ? N11 C12 1.329(4) . ? N11 C11A 1.373(4) . ? C11A C14A 1.409(4) . ? C11A C18 1.408(5) . ? C12 C13 1.384(5) . ? C13 C14 1.333(6) . ? C14 C14A 1.421(6) . ? C14A C15 1.413(6) . ? C15 C16 1.341(6) . ? C16 C17 1.414(6) . ? C17 C18 1.386(4) . ? C18 O18 1.334(4) . ? N21 C22 1.321(4) . ? N21 C21A 1.380(3) . ? C21A C24A 1.404(4) . ? C21A C28 1.418(4) . ? C22 C23 1.400(5) . ? C23 C24 1.347(5) . ? C24A C24 1.412(5) . ? C24A C25 1.415(5) . ? C25 C26 1.366(5) . ? C26 C27 1.400(5) . ? C27 C28 1.382(4) . ? C28 O28 1.316(3) . ? O30 C30 1.265(9) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O8 V1 O18 101.03(9) . . ? O8 V1 O28 96.13(8) . . ? O18 V1 O28 160.76(9) . . ? O8 V1 N11 92.80(9) . . ? O18 V1 N11 80.01(9) . . ? O28 V1 N11 90.60(9) . . ? O8 V1 N1 81.26(9) . . ? O18 V1 N1 94.44(9) . . ? O28 V1 N1 96.70(9) . . ? N11 V1 N1 171.02(9) . . ? O8 V1 N21 170.99(8) . . ? O18 V1 N21 86.01(8) . . ? O28 V1 N21 77.87(8) . . ? N11 V1 N21 93.98(9) . . ? N1 V1 N21 92.67(9) . . ? C2 N1 C1A 117.9(2) . . ? C2 N1 V1 132.9(2) . . ? C1A N1 V1 109.2(2) . . ? N1 C1A C8 115.6(2) . . ? N1 C1A C4A 122.7(3) . . ? C8 C1A C4A 121.7(3) . . ? N1 C2 C3 123.1(3) . . ? C4 C3 C2 119.5(3) . . ? C3 C4 C4A 120.2(3) . . ? C5 C4A C4 125.6(3) . . ? C5 C4A C1A 117.8(3) . . ? C4 C4A C1A 116.6(3) . . ? C6 C5 C4A 120.2(3) . . ? C5 C6 C7 122.4(3) . . ? C8 C7 C6 119.7(3) . . ? O8 C8 C7 123.7(3) . . ? O8 C8 C1A 118.1(2) . . ? C7 C8 C1A 118.2(3) . . ? C8 O8 V1 115.8(2) . . ? C12 N11 C11A 118.4(3) . . ? C12 N11 V1 130.9(2) . . ? C11A N11 V1 110.6(2) . . ? N11 C11A C14A 121.9(3) . . ? N11 C11A C18 115.0(2) . . ? C14A C11A C18 123.0(3) . . ? N11 C12 C13 123.0(4) . . ? C14 C13 C12 119.2(4) . . ? C13 C14 C14A 121.5(3) . . ? C15 C14A C11A 117.7(4) . . ? C15 C14A C14 126.4(4) . . ? C11A C14A C14 116.0(3) . . ? C16 C15 C14A 119.3(4) . . ? C15 C16 C17 123.3(4) . . ? C18 C17 C16 119.5(4) . . ? O18 C18 C17 124.8(3) . . ? O18 C18 C11A 118.0(3) . . ? C17 C18 C11A 117.2(3) . . ? C18 O18 V1 116.0(2) . . ? C22 N21 C21A 118.0(3) . . ? C22 N21 V1 131.2(2) . . ? C21A N21 V1 110.8(2) . . ? N21 C21A C24A 123.1(3) . . ? N21 C21A C28 114.9(2) . . ? C24A C21A C28 122.0(3) . . ? N21 C22 C23 122.2(3) . . ? C24 C23 C22 120.1(3) . . ? C21A C24A C24 116.1(3) . . ? C21A C24A C25 118.2(3) . . ? C24 C24A C25 125.7(3) . . ? C23 C24 C24A 120.6(3) . . ? C26 C25 C24A 119.7(3) . . ? C25 C26 C27 121.6(3) . . ? C28 C27 C26 120.9(3) . . ? O28 C28 C27 125.7(3) . . ? O28 C28 C21A 116.8(2) . . ? C27 C28 C21A 117.5(3) . . ? C28 O28 V1 119.4(2) . . ? 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 O8 V1 N1 C2 -179.3(3) . . . . ? O18 V1 N1 C2 80.2(3) . . . . ? O28 V1 N1 C2 -84.1(3) . . . . ? N11 V1 N1 C2 131.7(6) . . . . ? N21 V1 N1 C2 -6.0(3) . . . . ? O8 V1 N1 C1A -1.7(2) . . . . ? O18 V1 N1 C1A -102.2(2) . . . . ? O28 V1 N1 C1A 93.5(2) . . . . ? N11 V1 N1 C1A -50.7(7) . . . . ? N21 V1 N1 C1A 171.6(2) . . . . ? C2 N1 C1A C8 178.7(2) . . . . ? V1 N1 C1A C8 0.7(3) . . . . ? C2 N1 C1A C4A -0.4(4) . . . . ? V1 N1 C1A C4A -178.4(2) . . . . ? C1A N1 C2 C3 0.9(4) . . . . ? V1 N1 C2 C3 178.4(2) . . . . ? N1 C2 C3 C4 -1.4(5) . . . . ? C2 C3 C4 C4A 1.4(5) . . . . ? C3 C4 C4A C5 -179.0(3) . . . . ? C3 C4 C4A C1A -0.9(5) . . . . ? N1 C1A C4A C5 178.7(3) . . . . ? C8 C1A C4A C5 -0.4(4) . . . . ? N1 C1A C4A C4 0.3(4) . . . . ? C8 C1A C4A C4 -178.7(3) . . . . ? C4 C4A C5 C6 178.2(3) . . . . ? C1A C4A C5 C6 0.1(5) . . . . ? C4A C5 C6 C7 0.5(6) . . . . ? C5 C6 C7 C8 -0.8(5) . . . . ? C6 C7 C8 O8 -179.8(3) . . . . ? C6 C7 C8 C1A 0.5(4) . . . . ? N1 C1A C8 O8 1.3(4) . . . . ? C4A C1A C8 O8 -179.6(2) . . . . ? N1 C1A C8 C7 -179.0(3) . . . . ? C4A C1A C8 C7 0.1(4) . . . . ? C7 C8 O8 V1 177.5(2) . . . . ? C1A C8 O8 V1 -2.9(3) . . . . ? O18 V1 O8 C8 95.3(2) . . . . ? O28 V1 O8 C8 -93.4(2) . . . . ? N11 V1 O8 C8 175.7(2) . . . . ? N1 V1 O8 C8 2.4(2) . . . . ? N21 V1 O8 C8 -45.6(6) . . . . ? O8 V1 N11 C12 79.8(3) . . . . ? O18 V1 N11 C12 -179.5(3) . . . . ? O28 V1 N11 C12 -16.4(3) . . . . ? N1 V1 N11 C12 128.1(6) . . . . ? N21 V1 N11 C12 -94.3(3) . . . . ? O8 V1 N11 C11A -96.6(2) . . . . ? O18 V1 N11 C11A 4.2(2) . . . . ? O28 V1 N11 C11A 167.3(2) . . . . ? N1 V1 N11 C11A -48.2(7) . . . . ? N21 V1 N11 C11A 89.4(2) . . . . ? C12 N11 C11A C14A -0.1(4) . . . . ? V1 N11 C11A C14A 176.8(2) . . . . ? C12 N11 C11A C18 180.0(3) . . . . ? V1 N11 C11A C18 -3.2(3) . . . . ? C11A N11 C12 C13 -0.8(5) . . . . ? V1 N11 C12 C13 -176.9(3) . . . . ? N11 C12 C13 C14 0.5(6) . . . . ? C12 C13 C14 C14A 0.6(7) . . . . ? N11 C11A C14A C15 -179.1(3) . . . . ? C18 C11A C14A C15 0.9(5) . . . . ? N11 C11A C14A C14 1.1(5) . . . . ? C18 C11A C14A C14 -178.9(3) . . . . ? C13 C14 C14A C15 178.8(4) . . . . ? C13 C14 C14A C11A -1.4(6) . . . . ? C11A C14A C15 C16 -1.2(6) . . . . ? C14 C14A C15 C16 178.5(4) . . . . ? C14A C15 C16 C17 1.0(7) . . . . ? C15 C16 C17 C18 -0.2(6) . . . . ? C16 C17 C18 O18 -179.9(3) . . . . ? C16 C17 C18 C11A -0.2(4) . . . . ? N11 C11A C18 O18 -0.4(4) . . . . ? C14A C11A C18 O18 179.6(3) . . . . ? N11 C11A C18 C17 179.8(3) . . . . ? C14A C11A C18 C17 -0.2(4) . . . . ? C17 C18 O18 V1 -176.0(2) . . . . ? C11A C18 O18 V1 4.3(3) . . . . ? O8 V1 O18 C18 86.4(2) . . . . ? O28 V1 O18 C18 -66.4(3) . . . . ? N11 V1 O18 C18 -4.6(2) . . . . ? N1 V1 O18 C18 168.3(2) . . . . ? N21 V1 O18 C18 -99.3(2) . . . . ? O8 V1 N21 C22 132.3(5) . . . . ? O18 V1 N21 C22 -9.3(3) . . . . ? O28 V1 N21 C22 -178.7(3) . . . . ? N11 V1 N21 C22 -89.0(3) . . . . ? N1 V1 N21 C22 85.0(3) . . . . ? O8 V1 N21 C21A -45.1(6) . . . . ? O18 V1 N21 C21A 173.3(2) . . . . ? O28 V1 N21 C21A 3.8(2) . . . . ? N11 V1 N21 C21A 93.6(2) . . . . ? N1 V1 N21 C21A -92.4(2) . . . . ? C22 N21 C21A C24A -0.5(4) . . . . ? V1 N21 C21A C24A 177.3(2) . . . . ? C22 N21 C21A C28 178.4(3) . . . . ? V1 N21 C21A C28 -3.8(3) . . . . ? C21A N21 C22 C23 -0.6(5) . . . . ? V1 N21 C22 C23 -177.8(2) . . . . ? N21 C22 C23 C24 1.0(5) . . . . ? N21 C21A C24A C24 1.0(4) . . . . ? C28 C21A C24A C24 -177.8(3) . . . . ? N21 C21A C24A C25 -179.2(3) . . . . ? C28 C21A C24A C25 2.0(4) . . . . ? C22 C23 C24 C24A -0.4(5) . . . . ? C21A C24A C24 C23 -0.6(5) . . . . ? C25 C24A C24 C23 179.7(3) . . . . ? C21A C24A C25 C26 -2.1(5) . . . . ? C24 C24A C25 C26 177.6(3) . . . . ? C24A C25 C26 C27 0.3(5) . . . . ? C25 C26 C27 C28 1.7(5) . . . . ? C26 C27 C28 O28 178.0(3) . . . . ? C26 C27 C28 C21A -1.8(4) . . . . ? N21 C21A C28 O28 1.2(4) . . . . ? C24A C21A C28 O28 -179.9(2) . . . . ? N21 C21A C28 C27 -179.0(2) . . . . ? C24A C21A C28 C27 -0.1(4) . . . . ? C27 C28 O28 V1 -177.3(2) . . . . ? C21A C28 O28 V1 2.5(3) . . . . ? O8 V1 O28 C28 169.7(2) . . . . ? O18 V1 O28 C28 -37.2(4) . . . . ? N11 V1 O28 C28 -97.4(2) . . . . ? N1 V1 O28 C28 87.8(2) . . . . ? N21 V1 O28 C28 -3.5(2) . . . . ? _refine_diff_density_max 0.566 _refine_diff_density_min -0.232 _refine_diff_density_rms 0.058 data_shel93 _database_code_CSD 156233 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical '[V(III)Cl2(acac)(bpy)].CH3COCH3' _chemical_formula_sum 'C18 H21 Cl2 N2 O3 V' _chemical_formula_weight 435.21 _chemical_melting_point ? _chemical_compound_source ? 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' 'Cl' 'Cl' 0.1484 0.1585 '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 P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.616(2) _cell_length_b 12.451(2) _cell_length_c 14.337(3) _cell_angle_alpha 90.00 _cell_angle_beta 115.699(6) _cell_angle_gamma 90.00 _cell_volume 2029.3(7) _cell_formula_units_Z 4 _cell_measurement_temperature 298 _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.5 _cell_measurement_theta_max 11 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas 1.40 _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'floating method' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 0.771 _exptl_absorpt_correction_type 'psi-scan empirical' _exptl_absorpt_correction_T_min 0.95 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 298 _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device 'P21 Nicolet upgraded by Crystal Logic' _diffrn_measurement_method 'theta-2theta scans' _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 1.2 _diffrn_reflns_number 3921 _diffrn_reflns_av_R_equivalents 0.0253 _diffrn_reflns_av_sigmaI/netI 0.0749 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 25.50 _reflns_number_total 3766 _reflns_number_observed 2226 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 3 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.0970P)^2^+4.3016P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3763 _refine_ls_number_parameters 279 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1267 _refine_ls_R_factor_obs 0.0690 _refine_ls_wR_factor_all 0.2357 _refine_ls_wR_factor_obs 0.1840 _refine_ls_goodness_of_fit_all 1.100 _refine_ls_goodness_of_fit_obs 1.141 _refine_ls_restrained_S_all 1.104 _refine_ls_restrained_S_obs 1.141 _refine_ls_shift/esd_max 0.182 _refine_ls_shift/esd_mean 0.004 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group V V 0.73875(10) 0.20730(9) 0.97820(9) 0.0506(4) Uani 1 d . . Cl1 Cl 0.5817(2) 0.28554(14) 0.99804(15) 0.0591(5) Uani 1 d . . Cl2 Cl 0.8684(2) 0.3319(2) 1.0721(2) 0.0786(6) Uani 1 d . . O1 O 0.6916(4) 0.2788(4) 0.8439(3) 0.0586(13) Uani 1 d . . O2 O 0.8612(4) 0.1327(4) 0.9508(3) 0.0516(11) Uani 1 d . . N1 N 0.6285(4) 0.0720(4) 0.9068(4) 0.0448(12) Uani 1 d . . N2 N 0.7744(4) 0.0975(4) 1.1031(4) 0.0458(12) Uani 1 d . . C1 C 0.5549(7) 0.0646(7) 0.8066(6) 0.059(2) Uani 1 d . . C2 C 0.4867(8) -0.0240(8) 0.7643(7) 0.071(2) Uani 1 d . . C3 C 0.4955(8) -0.1088(7) 0.8273(8) 0.075(3) Uani 1 d . . C4 C 0.5690(8) -0.1033(7) 0.9285(8) 0.063(2) Uani 1 d . . C5 C 0.6353(6) -0.0111(5) 0.9693(5) 0.0475(15) Uani 1 d . . C6 C 0.7161(6) 0.0048(5) 1.0798(5) 0.0468(15) Uani 1 d . . C7 C 0.7296(9) -0.0697(8) 1.1574(8) 0.067(2) Uani 1 d . . C8 C 0.8011(9) -0.0468(9) 1.2581(7) 0.076(3) Uani 1 d . . C9 C 0.8610(9) 0.0473(8) 1.2812(7) 0.070(2) Uani 1 d . . C10 C 0.8474(7) 0.1184(7) 1.2041(6) 0.060(2) Uani 1 d . . C11 C 0.6964(8) 0.3673(7) 0.7015(6) 0.076(2) Uani 1 d . . H11A H 0.7371(48) 0.3618(51) 0.6587(35) 0.158(29) Uiso 1 calc R . H11B H 0.7009(66) 0.4398(10) 0.7257(6) 0.158(29) Uiso 1 calc R . H11C H 0.6154(22) 0.3477(43) 0.6621(37) 0.158(29) Uiso 1 calc R . C12 C 0.7519(6) 0.2932(5) 0.7923(5) 0.0483(15) Uani 1 d . . C13 C 0.8562(7) 0.2413(6) 0.8163(6) 0.056(2) Uani 1 d . . C14 C 0.9054(5) 0.1627(5) 0.8904(5) 0.0436(14) Uani 1 d . . C15 C 1.0162(6) 0.1065(6) 0.9006(6) 0.057(2) Uani 1 d . . H15A H 1.0080(29) 0.0860(60) 0.8333(8) 0.159(29) Uiso 1 calc R . H15B H 1.0289(40) 0.0436(37) 0.9429(54) 0.159(29) Uiso 1 calc R . H15C H 1.0821(13) 0.1542(24) 0.9322(59) 0.159(29) Uiso 1 calc R . O3 O 0.2138(7) 0.3137(7) -0.0558(7) 0.126(3) Uani 1 d . . C16 C 0.2348(7) 0.3775(6) 0.0159(7) 0.072(2) Uani 1 d . . C17 C 0.3520(8) 0.4286(8) 0.0685(8) 0.085(3) Uani 1 d . . H17A H 0.3710(41) 0.4389(77) 0.1403(19) 0.195(38) Uiso 1 calc R . H17B H 0.3509(28) 0.4969(39) 0.0369(54) 0.195(38) Uiso 1 calc R . H17C H 0.4101(16) 0.3832(40) 0.0622(71) 0.195(38) Uiso 1 calc R . C18 C 0.1444(8) 0.4069(9) 0.0506(9) 0.099(3) Uani 1 d . . H18A H 0.1349(38) 0.4835(9) 0.0478(45) 0.111(20) Uiso 1 calc R . H18B H 0.1685(26) 0.3827(44) 0.1205(19) 0.111(20) Uiso 1 calc R . H18C H 0.0711(16) 0.3737(40) 0.0063(30) 0.111(20) Uiso 1 calc R . H1 H 0.5507(49) 0.1165(48) 0.7700(45) 0.030(15) Uiso 1 d . . H2 H 0.4407(71) -0.0237(66) 0.7065(64) 0.068(26) Uiso 1 d . . H3 H 0.4539(65) -0.1664(64) 0.7973(58) 0.061(21) Uiso 1 d . . H4 H 0.5814(77) -0.1365(70) 0.9673(66) 0.064(32) Uiso 1 d . . H7 H 0.6935(62) -0.1166(57) 1.1404(55) 0.044(23) Uiso 1 d . . H8 H 0.8051(89) -0.0907(84) 1.2948(79) 0.100(35) Uiso 1 d . . H9 H 0.9113(79) 0.0618(74) 1.3409(71) 0.087(31) Uiso 1 d . . H10 H 0.9135(93) 0.1633(92) 1.2153(80) 0.121(38) Uiso 1 d . . H13 H 0.8842(59) 0.2542(55) 0.7748(51) 0.051(19) Uiso 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 V 0.0568(7) 0.0538(7) 0.0507(6) 0.0168(5) 0.0322(5) 0.0162(5) Cl1 0.0624(10) 0.0538(10) 0.0763(12) 0.0022(8) 0.0444(9) 0.0088(8) Cl2 0.0763(13) 0.0762(14) 0.0715(13) -0.0098(11) 0.0209(11) -0.0123(11) O1 0.059(3) 0.069(3) 0.053(3) 0.023(2) 0.029(2) 0.022(2) O2 0.059(3) 0.052(3) 0.054(3) 0.015(2) 0.034(2) 0.014(2) N1 0.051(3) 0.044(3) 0.044(3) -0.001(2) 0.025(2) 0.005(2) N2 0.048(3) 0.048(3) 0.045(3) 0.007(2) 0.024(2) 0.009(2) C1 0.069(5) 0.055(4) 0.053(4) 0.005(4) 0.026(4) 0.004(4) C2 0.060(5) 0.085(6) 0.056(5) -0.026(5) 0.013(4) 0.001(4) C3 0.070(5) 0.058(5) 0.106(8) -0.029(5) 0.048(5) -0.018(4) C4 0.067(5) 0.056(5) 0.074(6) 0.005(5) 0.039(5) 0.005(4) C5 0.052(4) 0.039(3) 0.064(4) 0.004(3) 0.037(3) 0.010(3) C6 0.054(4) 0.048(4) 0.051(4) 0.009(3) 0.034(3) 0.011(3) C7 0.076(6) 0.060(5) 0.082(6) 0.018(5) 0.049(5) 0.007(5) C8 0.091(6) 0.089(7) 0.059(5) 0.038(5) 0.041(5) 0.028(5) C9 0.075(5) 0.083(6) 0.049(5) 0.018(4) 0.023(4) 0.019(5) C10 0.056(4) 0.073(5) 0.054(4) 0.009(4) 0.025(3) 0.008(4) C11 0.092(6) 0.080(6) 0.062(5) 0.034(4) 0.041(4) 0.024(5) C12 0.059(4) 0.048(3) 0.040(3) 0.004(3) 0.023(3) 0.002(3) C13 0.069(5) 0.058(4) 0.056(4) 0.012(3) 0.040(4) 0.004(3) C14 0.048(3) 0.042(3) 0.044(3) -0.005(3) 0.023(3) -0.003(3) C15 0.052(4) 0.063(4) 0.064(4) -0.003(4) 0.031(3) 0.003(3) O3 0.105(6) 0.108(6) 0.153(7) -0.048(6) 0.044(5) -0.018(5) C16 0.071(5) 0.049(4) 0.087(6) 0.006(4) 0.027(5) 0.002(4) C17 0.078(6) 0.079(6) 0.102(7) -0.009(5) 0.043(5) -0.014(5) C18 0.069(6) 0.091(7) 0.142(9) 0.030(7) 0.051(6) 0.005(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V O1 1.964(4) . ? V O2 1.982(4) . ? V N2 2.140(5) . ? V N1 2.142(6) . ? V Cl2 2.233(3) . ? V Cl1 2.333(2) . ? O1 C12 1.284(8) . ? O2 C14 1.273(7) . ? N1 C1 1.332(9) . ? N1 C5 1.348(8) . ? N2 C6 1.331(8) . ? N2 C10 1.362(9) . ? C1 C2 1.368(12) . ? C2 C3 1.363(13) . ? C3 C4 1.342(13) . ? C4 C5 1.391(11) . ? C5 C6 1.480(10) . ? C6 C7 1.400(10) . ? C7 C8 1.360(14) . ? C8 C9 1.355(14) . ? C9 C10 1.367(11) . ? C11 C12 1.498(9) . ? C12 C13 1.369(10) . ? C13 C14 1.377(9) . ? C14 C15 1.513(9) . ? O3 C16 1.233(11) . ? C16 C18 1.476(13) . ? C16 C17 1.481(12) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 V O2 87.1(2) . . ? O1 V N2 166.9(2) . . ? O2 V N2 88.1(2) . . ? O1 V N1 91.7(2) . . ? O2 V N1 86.4(2) . . ? N2 V N1 75.8(2) . . ? O1 V Cl2 96.1(2) . . ? O2 V Cl2 90.9(2) . . ? N2 V Cl2 96.1(2) . . ? N1 V Cl2 171.5(2) . . ? O1 V Cl1 91.02(15) . . ? O2 V Cl1 174.7(2) . . ? N2 V Cl1 92.64(14) . . ? N1 V Cl1 88.67(14) . . ? Cl2 V Cl1 94.32(9) . . ? C12 O1 V 128.7(4) . . ? C14 O2 V 127.3(4) . . ? C1 N1 C5 118.5(6) . . ? C1 N1 V 125.0(5) . . ? C5 N1 V 116.4(4) . . ? C6 N2 C10 118.5(6) . . ? C6 N2 V 116.8(4) . . ? C10 N2 V 124.6(5) . . ? N1 C1 C2 122.9(8) . . ? C3 C2 C1 118.4(8) . . ? C4 C3 C2 119.8(8) . . ? C3 C4 C5 120.3(9) . . ? N1 C5 C4 120.1(7) . . ? N1 C5 C6 115.1(6) . . ? C4 C5 C6 124.8(7) . . ? N2 C6 C7 120.8(7) . . ? N2 C6 C5 115.7(5) . . ? C7 C6 C5 123.5(7) . . ? C8 C7 C6 120.0(9) . . ? C9 C8 C7 118.9(8) . . ? C8 C9 C10 120.1(9) . . ? N2 C10 C9 121.7(8) . . ? O1 C12 C13 122.3(6) . . ? O1 C12 C11 114.6(6) . . ? C13 C12 C11 123.1(6) . . ? C12 C13 C14 126.3(6) . . ? O2 C14 C13 123.3(6) . . ? O2 C14 C15 117.2(6) . . ? C13 C14 C15 119.5(6) . . ? O3 C16 C18 121.5(9) . . ? O3 C16 C17 120.5(9) . . ? C18 C16 C17 117.9(9) . . ? _refine_diff_density_max 1.108 _refine_diff_density_min -0.709 _refine_diff_density_rms 0.096 #===END data_vman _database_code_CSD 156234 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical '(Et3NH)2[VO2(m2-3,5-dtbc)]2' _chemical_formula_sum 'C40 H72 N2 O8 V2' _chemical_formula_weight 810.88 _chemical_melting_point ? _chemical_compound_source ? loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'V' 'V' 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.915(15) _cell_length_b 15.029(14) _cell_length_c 11.091(12) _cell_angle_alpha 90.15(3) _cell_angle_beta 99.02(4) _cell_angle_gamma 107.11(3) _cell_volume 2343.7(41) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 5.4 _cell_measurement_theta_max 11.5 _exptl_crystal_description 'parallelipiped' _exptl_crystal_colour 'red' _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.149 _exptl_crystal_density_method ? _exptl_crystal_F_000 872 _exptl_absorpt_coefficient_mu 0.444 _exptl_absorpt_correction_type ? _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 ? _diffrn_measurement_method ? _diffrn_standards_number 3 _diffrn_standards_interval_count 97 _diffrn_standards_interval_time ? _diffrn_standards_decay_% 2.9 _diffrn_reflns_number 6829 _diffrn_reflns_av_R_equivalents 0.0132 _diffrn_reflns_av_sigmaI/netI 0.0497 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 1.42 _diffrn_reflns_theta_max 23.25 _reflns_number_total 6451 _reflns_number_observed 5101 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme 'calc w=1/[\s^2^(Fo^2^)+(0.1472P)^2^+3.8926P] 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 ? _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6449 _refine_ls_number_parameters 517 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1078 _refine_ls_R_factor_obs 0.0910 _refine_ls_wR_factor_all 0.2555 _refine_ls_wR_factor_obs 0.2328 _refine_ls_goodness_of_fit_all 1.067 _refine_ls_goodness_of_fit_obs 1.102 _refine_ls_restrained_S_all 1.069 _refine_ls_restrained_S_obs 1.102 _refine_ls_shift/esd_max 0.002 _refine_ls_shift/esd_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group V1 V -0.00360(7) 0.73988(6) 0.06484(8) 0.0498(3) Uani 1 d . . V2 V -0.04916(7) 0.73222(6) 0.34714(7) 0.0492(3) Uani 1 d . . O1 O -0.0340(4) 0.8205(3) -0.0075(4) 0.0754(12) Uani 1 d . . O2 O -0.0274(3) 0.6477(3) -0.0250(4) 0.0638(11) Uani 1 d . . O3 O -0.0281(3) 0.8413(2) 0.3919(3) 0.0628(11) Uani 1 d . . O4 O -0.0108(3) 0.6760(3) 0.4551(4) 0.0643(11) Uani 1 d . . O5 O -0.1059(3) 0.7025(3) 0.1675(3) 0.0540(9) Uani 1 d . . O6 O -0.1835(3) 0.6802(3) 0.3512(4) 0.0721(12) Uani 1 d . . O7 O 0.0501(2) 0.7439(3) 0.2434(3) 0.0528(9) Uani 1 d . . O8 O 0.1329(3) 0.7893(3) 0.0687(4) 0.0746(12) Uani 1 d . . C1 C -0.2028(4) 0.6895(4) 0.1423(6) 0.0551(14) Uani 1 d . . C2 C -0.2528(4) 0.6893(4) 0.0288(5) 0.0601(15) Uani 1 d . . H2 H -0.2230(4) 0.6958(4) -0.0397(5) 0.041(13) Uiso 1 calc R . C3 C -0.3504(4) 0.6790(4) 0.0173(6) 0.063(2) Uani 1 d . . C4 C -0.3902(4) 0.6697(4) 0.1218(6) 0.067(2) Uani 1 d . . H4 H -0.4549(4) 0.6631(4) 0.1133(6) 0.084(21) Uiso 1 calc R . C5 C -0.3413(4) 0.6693(4) 0.2399(6) 0.064(2) Uani 1 d . . C6 C -0.2428(4) 0.6785(4) 0.2467(5) 0.0571(14) Uani 1 d . . C7 C -0.4087(6) 0.6819(6) -0.1088(6) 0.085(2) Uani 1 d . . C8 C -0.3790(10) 0.6371(13) -0.2064(9) 0.206(8) Uani 1 d . . H8A H -0.3700(65) 0.5791(32) -0.1798(34) 0.209(35) Uiso 1 calc R . H8B H -0.3204(36) 0.6772(29) -0.2255(59) 0.209(35) Uiso 1 calc R . H8C H -0.4272(32) 0.6255(63) -0.2778(30) 0.209(35) Uiso 1 calc R . C9 C -0.5150(7) 0.6302(10) -0.1137(9) 0.153(5) Uani 1 d . . H9A H -0.5422(19) 0.6648(39) -0.0649(81) 0.238(41) Uiso 1 calc R . H9B H -0.5219(8) 0.5694(29) -0.0825(93) 0.238(41) Uiso 1 calc R . H9C H -0.5470(16) 0.6240(69) -0.1968(16) 0.238(41) Uiso 1 calc R . C10 C -0.3986(14) 0.7790(10) -0.1348(13) 0.272(12) Uani 1 d . . H10A H -0.4193(53) 0.8079(18) -0.0716(43) 0.180(29) Uiso 1 calc R . H10B H -0.4367(50) 0.7819(10) -0.2121(39) 0.180(29) Uiso 1 calc R . H10C H -0.3331(18) 0.8111(17) -0.1379(73) 0.180(29) Uiso 1 calc R . C11 C -0.3861(5) 0.6626(6) 0.3544(7) 0.081(2) Uani 1 d . . C12 C -0.4934(6) 0.6508(7) 0.3260(8) 0.108(3) Uani 1 d . . H12A H -0.5191(9) 0.6446(37) 0.4008(9) 0.114(17) Uiso 1 calc R . H12B H -0.5246(8) 0.5960(20) 0.2734(39) 0.114(17) Uiso 1 calc R . H12C H -0.5036(6) 0.7045(17) 0.2861(43) 0.114(17) Uiso 1 calc R . C13 C -0.3732(6) 0.5776(7) 0.4243(8) 0.105(3) Uani 1 d . . H13A H -0.3980(34) 0.5759(21) 0.4994(23) 0.116(17) Uiso 1 calc R . H13B H -0.3068(7) 0.5824(20) 0.4421(42) 0.116(17) Uiso 1 calc R . H13C H -0.4068(31) 0.5216(7) 0.3751(20) 0.116(17) Uiso 1 calc R . C14 C -0.3393(6) 0.7515(7) 0.4361(8) 0.109(3) Uani 1 d . . H14A H -0.3672(23) 0.7465(15) 0.5091(21) 0.102(15) Uiso 1 calc R . H14B H -0.3490(28) 0.8041(8) 0.3930(17) 0.102(15) Uiso 1 calc R . H14C H -0.2724(8) 0.7597(18) 0.4575(35) 0.102(15) Uiso 1 calc R . C15 C 0.1489(4) 0.7790(3) 0.2772(5) 0.0522(13) Uani 1 d . . C16 C 0.1956(4) 0.7876(4) 0.3929(5) 0.0577(14) Uani 1 d . . H16 H 0.1624(4) 0.7709(4) 0.4578(5) 0.037(12) Uiso 1 calc R . C17 C 0.2947(4) 0.8221(4) 0.4134(6) 0.0610(15) Uani 1 d . . C18 C 0.3389(4) 0.8460(4) 0.3123(6) 0.0600(15) Uani 1 d . . H18 H 0.4049(4) 0.8695(4) 0.3260(6) 0.083(21) Uiso 1 calc R . C19 C 0.2926(4) 0.8379(4) 0.1920(5) 0.0563(14) Uani 1 d . . C20 C 0.1915(4) 0.8019(4) 0.1764(5) 0.0549(14) Uani 1 d . . C21 C 0.3479(5) 0.8349(6) 0.5461(6) 0.081(2) Uani 1 d . . C22 C 0.4563(6) 0.8629(7) 0.5523(8) 0.111(3) Uani 1 d . . H22A H 0.4769(8) 0.9196(22) 0.5110(47) 0.130(19) Uiso 1 calc R . H22B H 0.4731(7) 0.8142(19) 0.5135(47) 0.130(19) Uiso 1 calc R . H22C H 0.4868(6) 0.8723(41) 0.6362(8) 0.130(19) Uiso 1 calc R . C23 C 0.3178(8) 0.7445(8) 0.6104(9) 0.146(5) Uani 1 d . . H23A H 0.3520(47) 0.7525(20) 0.6925(27) 0.199(32) Uiso 1 calc R . H23B H 0.3316(56) 0.6960(16) 0.5671(46) 0.199(32) Uiso 1 calc R . H23C H 0.2508(15) 0.7277(33) 0.6122(71) 0.199(32) Uiso 1 calc R . C24 C 0.3260(8) 0.9133(9) 0.6101(9) 0.144(4) Uani 1 d . . H24A H 0.3447(40) 0.9692(14) 0.5667(33) 0.144(22) Uiso 1 calc R . H24B H 0.3605(36) 0.9237(30) 0.6922(20) 0.144(22) Uiso 1 calc R . H24C H 0.2590(11) 0.8968(20) 0.6121(51) 0.144(22) Uiso 1 calc R . C25 C 0.3447(5) 0.8664(5) 0.0838(6) 0.071(2) Uani 1 d . . C26 C 0.3116(6) 0.9444(6) 0.0201(9) 0.109(3) Uani 1 d . . H26A H 0.3453(25) 0.9638(23) -0.0469(27) 0.100(14) Uiso 1 calc R . H26B H 0.3244(30) 0.9964(14) 0.0773(14) 0.100(14) Uiso 1 calc R . H26C H 0.2446(9) 0.9219(11) -0.0100(38) 0.100(14) Uiso 1 calc R . C27 C 0.3225(6) 0.7834(6) -0.0068(8) 0.103(3) Uani 1 d . . H27A H 0.3538(30) 0.8026(10) -0.0759(23) 0.115(17) Uiso 1 calc R . H27B H 0.2550(7) 0.7603(23) -0.0338(36) 0.115(17) Uiso 1 calc R . H27C H 0.3446(32) 0.7350(15) 0.0321(16) 0.115(17) Uiso 1 calc R . C28 C 0.4532(5) 0.9014(6) 0.1213(8) 0.099(3) Uani 1 d . . H28A H 0.4823(5) 0.9167(31) 0.0497(9) 0.097(14) Uiso 1 calc R . H28B H 0.4750(6) 0.8535(13) 0.1622(38) 0.097(14) Uiso 1 calc R . H28C H 0.4703(6) 0.9558(19) 0.1754(33) 0.097(14) Uiso 1 calc R . N1 N 0.9798(5) 0.9973(3) 0.2598(5) 0.083(2) Uani 1 d . . HN1 H 0.9766(5) 0.9454(3) 0.3030(5) 0.079(20) Uiso 1 calc R . C29 C 1.0721(8) 1.0186(5) 0.2100(8) 0.102(3) Uani 1 d . . H29A H 1.0689(8) 0.9675(5) 0.1542(8) 0.122(21) Uiso 1 calc R . H29B H 1.0795(8) 1.0742(5) 0.1638(8) 0.122(21) Uiso 1 calc R . C30 C 1.1579(8) 1.0331(7) 0.3075(11) 0.136(4) Uani 1 d . . H30A H 1.2136(10) 1.0423(43) 0.2701(11) 0.141(21) Uiso 1 calc R . H30B H 1.1501(21) 0.9793(19) 0.3559(37) 0.141(21) Uiso 1 calc R . H30C H 1.1649(26) 1.0870(26) 0.3589(35) 0.141(21) Uiso 1 calc R . C31 C 0.9728(8) 1.0691(5) 0.3475(7) 0.105(3) Uani 1 d . . H31A H 1.0276(8) 1.0830(5) 0.4121(7) 0.094(17) Uiso 1 calc R . H31B H 0.9165(8) 1.0439(5) 0.3846(7) 0.094(17) Uiso 1 calc R . C32 C 0.9678(10) 1.1591(6) 0.2885(9) 0.149(5) Uani 1 d . . H32A H 0.9474(63) 1.1961(29) 0.3430(36) 0.204(33) Uiso 1 calc R . H32B H 0.9234(47) 1.1448(6) 0.2134(43) 0.204(33) Uiso 1 calc R . H32C H 1.0296(16) 1.1933(30) 0.2719(74) 0.204(33) Uiso 1 calc R . C33 C 0.8969(7) 0.9692(5) 0.1565(6) 0.091(3) Uani 1 d . . H33A H 0.9059(7) 0.9225(5) 0.1030(6) 0.088(15) Uiso 1 calc R . H33B H 0.8950(7) 1.0230(5) 0.1093(6) 0.088(15) Uiso 1 calc R . C34 C 0.8026(8) 0.9301(7) 0.2017(10) 0.120(3) Uani 1 d . . H34A H 0.7545(14) 0.8988(46) 0.1346(17) 0.170(27) Uiso 1 calc R . H34B H 0.7848(28) 0.9802(9) 0.2353(64) 0.170(27) Uiso 1 calc R . H34C H 0.8089(17) 0.8868(41) 0.2635(50) 0.170(27) Uiso 1 calc R . N2 N 0.0763(4) 0.4713(3) 0.2236(4) 0.0639(13) Uani 1 d . . HN2 H 0.0615(4) 0.4240(3) 0.1656(4) 0.071(18) Uiso 1 calc R . C35 C 0.1210(6) 0.4378(5) 0.3357(6) 0.082(2) Uani 1 d . . H35A H 0.1746(6) 0.4189(5) 0.3181(6) 0.084(15) Uiso 1 calc R . H35B H 0.0754(6) 0.3836(5) 0.3611(6) 0.084(15) Uiso 1 calc R . C36 C 0.1551(9) 0.5131(7) 0.4402(8) 0.138(4) Uani 1 d . . H36A H 0.1804(61) 0.4879(20) 0.5126(24) 0.204(33) Uiso 1 calc R . H36B H 0.1026(15) 0.5336(45) 0.4557(55) 0.204(33) Uiso 1 calc R . H36C H 0.2037(44) 0.5650(28) 0.4176(34) 0.204(33) Uiso 1 calc R . C37 C 0.1389(7) 0.5549(5) 0.1716(8) 0.095(2) Uani 1 d . . H37A H 0.1031(7) 0.5709(5) 0.0984(8) 0.124(22) Uiso 1 calc R . H37B H 0.1567(7) 0.6075(5) 0.2305(8) 0.124(22) Uiso 1 calc R . C38 C 0.2244(9) 0.5393(7) 0.1415(13) 0.148(4) Uani 1 d . . H38A H 0.2647(27) 0.5963(15) 0.1166(71) 0.176(28) Uiso 1 calc R . H38B H 0.2075(10) 0.4925(40) 0.0760(48) 0.176(28) Uiso 1 calc R . H38C H 0.2577(29) 0.5187(52) 0.2120(23) 0.176(28) Uiso 1 calc R . C39 C -0.0163(7) 0.4919(6) 0.2324(8) 0.099(3) Uani 1 d . . H39A H -0.0058(7) 0.5347(6) 0.3025(8) 0.162(30) Uiso 1 calc R . H39B H -0.0338(7) 0.5231(6) 0.1600(8) 0.162(30) Uiso 1 calc R . C40 C -0.0935(8) 0.4117(9) 0.2439(12) 0.142(4) Uani 1 d . . H40A H -0.1510(13) 0.4291(15) 0.2382(80) 0.199(33) Uiso 1 calc R . H40B H -0.0813(29) 0.3859(35) 0.3216(34) 0.199(33) Uiso 1 calc R . H40C H -0.1004(40) 0.3662(26) 0.1796(48) 0.199(33) 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 0.0755(7) 0.0397(5) 0.0373(5) -0.0030(4) 0.0054(4) 0.0241(4) V2 0.0736(7) 0.0392(5) 0.0364(5) -0.0012(4) 0.0039(4) 0.0218(4) O1 0.104(3) 0.070(3) 0.071(3) 0.023(2) 0.021(2) 0.050(3) O2 0.070(3) 0.058(2) 0.058(2) -0.027(2) 0.005(2) 0.014(2) O3 0.094(3) 0.039(2) 0.057(2) -0.005(2) 0.010(2) 0.025(2) O4 0.086(3) 0.056(2) 0.052(2) 0.010(2) 0.001(2) 0.030(2) O5 0.049(2) 0.059(2) 0.051(2) -0.005(2) 0.001(2) 0.016(2) O6 0.066(3) 0.095(3) 0.049(2) 0.002(2) 0.003(2) 0.017(2) O7 0.046(2) 0.054(2) 0.053(2) -0.007(2) 0.000(2) 0.011(2) O8 0.068(3) 0.094(3) 0.050(2) 0.003(2) 0.005(2) 0.009(2) C1 0.051(3) 0.045(3) 0.069(4) -0.005(3) 0.001(3) 0.019(2) C2 0.072(4) 0.063(4) 0.049(3) -0.004(3) 0.003(3) 0.030(3) C3 0.063(4) 0.063(4) 0.065(4) -0.008(3) -0.003(3) 0.030(3) C4 0.054(4) 0.070(4) 0.079(5) -0.007(3) 0.003(3) 0.026(3) C5 0.065(4) 0.061(4) 0.063(4) -0.005(3) 0.001(3) 0.019(3) C6 0.053(3) 0.051(3) 0.059(4) -0.005(3) -0.011(3) 0.014(3) C7 0.091(5) 0.107(6) 0.062(4) -0.006(4) -0.011(4) 0.052(5) C8 0.173(12) 0.404(25) 0.067(6) -0.065(10) -0.037(7) 0.154(15) C9 0.086(7) 0.257(15) 0.100(7) -0.005(8) -0.036(6) 0.052(8) C10 0.429(28) 0.124(10) 0.186(14) 0.013(10) -0.182(17) 0.085(14) C11 0.062(4) 0.097(5) 0.078(5) -0.005(4) 0.013(3) 0.014(4) C12 0.079(5) 0.156(9) 0.090(6) -0.001(6) 0.022(4) 0.034(5) C13 0.092(6) 0.133(8) 0.090(6) 0.025(5) 0.027(5) 0.025(5) C14 0.103(6) 0.131(7) 0.087(6) -0.026(5) 0.028(5) 0.019(5) C15 0.050(3) 0.038(3) 0.067(4) -0.007(2) 0.006(3) 0.014(2) C16 0.062(4) 0.053(3) 0.054(3) -0.003(3) 0.005(3) 0.014(3) C17 0.056(4) 0.061(4) 0.060(4) -0.005(3) 0.000(3) 0.014(3) C18 0.048(3) 0.051(3) 0.075(4) 0.001(3) 0.003(3) 0.010(3) C19 0.057(3) 0.050(3) 0.059(3) 0.002(3) 0.003(3) 0.016(3) C20 0.054(3) 0.043(3) 0.059(3) -0.007(2) -0.015(3) 0.014(2) C21 0.072(4) 0.094(5) 0.065(4) -0.006(4) -0.010(3) 0.015(4) C22 0.081(6) 0.157(9) 0.081(5) 0.004(5) -0.020(4) 0.032(5) C23 0.136(9) 0.152(10) 0.095(7) 0.041(7) -0.035(6) -0.012(7) C24 0.129(9) 0.190(12) 0.105(7) -0.068(8) -0.034(6) 0.066(8) C25 0.063(4) 0.069(4) 0.078(4) 0.007(3) 0.011(3) 0.015(3) C26 0.100(6) 0.103(6) 0.136(8) 0.059(6) 0.039(6) 0.035(5) C27 0.100(6) 0.112(6) 0.093(6) -0.009(5) 0.038(5) 0.013(5) C28 0.076(5) 0.118(7) 0.093(6) 0.027(5) 0.020(4) 0.011(4) N1 0.154(6) 0.037(3) 0.063(3) 0.001(2) 0.018(4) 0.037(3) C29 0.164(9) 0.056(4) 0.084(5) 0.008(4) 0.025(6) 0.024(5) C30 0.147(9) 0.087(7) 0.147(10) 0.008(6) -0.003(8) 0.007(6) C31 0.212(10) 0.056(4) 0.056(4) -0.006(3) 0.032(5) 0.047(5) C32 0.314(17) 0.062(5) 0.090(6) -0.003(4) 0.042(8) 0.080(8) C33 0.154(8) 0.076(5) 0.064(4) -0.008(3) -0.001(5) 0.073(5) C34 0.146(9) 0.090(6) 0.142(9) 0.008(6) 0.012(7) 0.068(6) N2 0.084(4) 0.043(3) 0.060(3) -0.015(2) -0.002(3) 0.020(2) C35 0.113(6) 0.060(4) 0.069(4) 0.003(3) -0.009(4) 0.031(4) C36 0.190(11) 0.118(8) 0.081(6) -0.024(5) -0.045(7) 0.043(7) C37 0.127(7) 0.047(4) 0.105(6) 0.002(4) 0.001(5) 0.025(4) C38 0.137(9) 0.085(7) 0.212(14) 0.009(7) 0.053(9) 0.003(6) C39 0.126(7) 0.087(5) 0.098(6) -0.019(4) 0.012(5) 0.058(6) C40 0.106(7) 0.150(10) 0.175(11) -0.025(8) 0.059(8) 0.027(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O1 1.591(4) . ? V1 O2 1.622(4) . ? V1 O8 1.945(5) . ? V1 O5 1.997(4) . ? V1 O7 2.010(4) . ? V2 O4 1.597(4) . ? V2 O3 1.636(4) . ? V2 O6 1.933(5) . ? V2 O7 1.981(4) . ? V2 O5 2.032(4) . ? O5 C1 1.382(7) . ? O6 C6 1.339(7) . ? O7 C15 1.400(7) . ? O8 C20 1.342(7) . ? C1 C2 1.357(8) . ? C1 C6 1.372(9) . ? C2 C3 1.403(9) . ? C3 C4 1.372(9) . ? C3 C7 1.535(9) . ? C4 C5 1.396(9) . ? C5 C6 1.425(9) . ? C5 C11 1.517(9) . ? C7 C10 1.456(14) . ? C7 C8 1.464(13) . ? C7 C9 1.538(13) . ? C11 C14 1.530(11) . ? C11 C12 1.539(10) . ? C11 C13 1.540(11) . ? C15 C16 1.347(8) . ? C15 C20 1.367(8) . ? C16 C17 1.396(8) . ? C17 C18 1.385(9) . ? C17 C21 1.541(9) . ? C18 C19 1.390(8) . ? C19 C20 1.426(8) . ? C19 C25 1.525(9) . ? C21 C24 1.514(12) . ? C21 C23 1.518(12) . ? C21 C22 1.537(11) . ? C25 C27 1.524(10) . ? C25 C26 1.534(10) . ? C25 C28 1.535(10) . ? N1 C31 1.489(8) . ? N1 C33 1.505(10) . ? N1 C29 1.511(11) . ? C29 C30 1.502(13) . ? C31 C32 1.520(11) . ? C33 C34 1.520(13) . ? N2 C35 1.478(8) . ? N2 C37 1.506(9) . ? N2 C39 1.519(10) . ? C35 C36 1.534(11) . ? C37 C38 1.451(13) . ? C39 C40 1.424(13) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 V1 O2 110.2(2) . . ? O1 V1 O8 97.9(2) . . ? O2 V1 O8 100.3(2) . . ? O1 V1 O5 100.0(2) . . ? O2 V1 O5 101.9(2) . . ? O8 V1 O5 144.5(2) . . ? O1 V1 O7 126.9(2) . . ? O2 V1 O7 122.8(2) . . ? O8 V1 O7 76.6(2) . . ? O5 V1 O7 68.1(2) . . ? O4 V2 O3 110.5(2) . . ? O4 V2 O6 97.9(2) . . ? O3 V2 O6 102.7(2) . . ? O4 V2 O7 99.5(2) . . ? O3 V2 O7 100.7(2) . . ? O6 V2 O7 143.7(2) . . ? O4 V2 O5 135.0(2) . . ? O3 V2 O5 114.2(2) . . ? O6 V2 O5 77.1(2) . . ? O7 V2 O5 68.0(2) . . ? C1 O5 V1 132.4(4) . . ? C1 O5 V2 114.0(3) . . ? V1 O5 V2 110.1(2) . . ? C6 O6 V2 116.7(4) . . ? C15 O7 V2 128.3(3) . . ? C15 O7 V1 117.4(3) . . ? V2 O7 V1 111.6(2) . . ? C20 O8 V1 119.3(4) . . ? C2 C1 C6 123.6(5) . . ? C2 C1 O5 124.7(6) . . ? C6 C1 O5 111.7(5) . . ? C1 C2 C3 118.5(6) . . ? C4 C3 C2 118.0(6) . . ? C4 C3 C7 121.9(6) . . ? C2 C3 C7 120.1(6) . . ? C3 C4 C5 125.2(6) . . ? C4 C5 C6 114.7(6) . . ? C4 C5 C11 124.2(6) . . ? C6 C5 C11 121.1(6) . . ? O6 C6 C1 116.1(5) . . ? O6 C6 C5 124.0(6) . . ? C1 C6 C5 119.9(5) . . ? C10 C7 C8 109.6(12) . . ? C10 C7 C3 108.4(7) . . ? C8 C7 C3 112.7(7) . . ? C10 C7 C9 108.6(10) . . ? C8 C7 C9 105.4(9) . . ? C3 C7 C9 112.0(7) . . ? C5 C11 C14 109.8(6) . . ? C5 C11 C12 112.5(6) . . ? C14 C11 C12 107.5(7) . . ? C5 C11 C13 109.7(6) . . ? C14 C11 C13 109.7(7) . . ? C12 C11 C13 107.5(7) . . ? C16 C15 C20 124.7(5) . . ? C16 C15 O7 124.6(5) . . ? C20 C15 O7 110.6(5) . . ? C15 C16 C17 118.7(6) . . ? C18 C17 C16 117.3(6) . . ? C18 C17 C21 124.0(6) . . ? C16 C17 C21 118.7(6) . . ? C17 C18 C19 125.3(6) . . ? C18 C19 C20 115.0(5) . . ? C18 C19 C25 123.2(5) . . ? C20 C19 C25 121.8(5) . . ? O8 C20 C15 116.0(5) . . ? O8 C20 C19 124.9(6) . . ? C15 C20 C19 119.0(5) . . ? C24 C21 C23 111.4(9) . . ? C24 C21 C22 107.1(7) . . ? C23 C21 C22 108.0(7) . . ? C24 C21 C17 108.5(7) . . ? C23 C21 C17 109.8(6) . . ? C22 C21 C17 112.1(6) . . ? C27 C25 C19 110.1(5) . . ? C27 C25 C26 109.2(7) . . ? C19 C25 C26 109.0(6) . . ? C27 C25 C28 107.0(6) . . ? C19 C25 C28 113.0(6) . . ? C26 C25 C28 108.5(6) . . ? C31 N1 C33 113.3(6) . . ? C31 N1 C29 115.8(6) . . ? C33 N1 C29 110.0(6) . . ? C30 C29 N1 113.4(8) . . ? N1 C31 C32 113.3(6) . . ? N1 C33 C34 112.3(7) . . ? C35 N2 C37 115.7(6) . . ? C35 N2 C39 115.4(6) . . ? C37 N2 C39 107.0(6) . . ? N2 C35 C36 111.8(6) . . ? C38 C37 N2 112.8(7) . . ? C40 C39 N2 114.3(7) . . ? _refine_diff_density_max 1.382 _refine_diff_density_min -0.800 _refine_diff_density_rms 0.110 #===END