Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2006 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_title ;Synthesis, Characterizations, and Structures of Oxovanadium(V) Complexes of Schiff Bases of b-Amino Alcohols as Tunable Catalysts for Asymmetric Oxidation of Organic Sulfides and Asymmetric Alkynylation of Aldehydes ; _publ_contact_author_name 'Prof. Han-Mou Gau' _publ_contact_author_email HMGAU@DRAGON.NCHU.EDU.TW loop_ _publ_author_name 'Han-Mou Gau.' 'Sheng-Hsiang Hsieh.' 'Ya-Pei Kuo.' # Attachment '3b.CIF' data_3b _database_code_depnum_ccdc_archive 'CCDC 620539' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; Ethoxo(2-oxo-3,5-di-tert-butylbenzaldehyde 2S-(1,1,3- triphenylpropoxo) imine)oxovanadium(V) ; _chemical_melting_point ? _chemical_formula_moiety (EtO)V(O)[OC(Ph)2CH(Bn)N=CH(2-O-3,5-(t-Bu)2-C6H2)] _chemical_formula_sum 'C38 H44 N O4 V' _chemical_formula_weight 629.68 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 9.8460(8) _cell_length_b 11.2520(9) _cell_length_c 31.761(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3518.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 7293 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 25.7 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.68 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.189 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1336 _exptl_absorpt_coefficient_mu 0.320 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.624 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _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 'CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 19900 _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_sigmaI/netI 0.0349 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.98 _reflns_number_total 6877 _reflns_number_gt 5504 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1085P)^2^+0.0210P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 6877 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0556 _refine_ls_wR_factor_ref 0.1661 _refine_ls_wR_factor_gt 0.1556 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.059 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V V 0.73376(6) 0.36033(5) 0.115966(17) 0.04979(17) Uani 1 1 d . . . O1 O 0.6740(3) 0.3837(2) 0.17043(7) 0.0597(6) Uani 1 1 d . . . O2 O 0.6504(3) 0.32443(19) 0.06558(7) 0.0533(6) Uani 1 1 d . . . O3 O 0.8870(2) 0.3170(3) 0.11477(9) 0.0690(7) Uani 1 1 d . . . O4 O 0.7459(3) 0.5165(2) 0.10629(8) 0.0704(7) Uani 1 1 d . . . N1 N 0.6539(3) 0.1908(3) 0.13316(8) 0.0483(6) Uani 1 1 d . . . C1 C 0.5982(4) 0.3012(4) 0.19500(11) 0.0580(9) Uani 1 1 d . . . C2 C 0.6458(4) 0.1771(3) 0.17936(10) 0.0555(8) Uani 1 1 d . . . H2A H 0.5779 0.1168 0.1866 0.067 Uiso 1 1 calc R . . C3 C 0.7862(4) 0.1400(4) 0.19647(11) 0.0637(9) Uani 1 1 d . . . H3A H 0.8529 0.1988 0.1880 0.076 Uiso 1 1 calc R . . H3B H 0.7829 0.1393 0.2270 0.076 Uiso 1 1 calc R . . C4 C 0.4461(4) 0.3240(4) 0.18723(11) 0.0619(10) Uani 1 1 d . . . C5 C 0.4024(5) 0.4420(5) 0.18594(13) 0.0763(12) Uani 1 1 d . . . H5A H 0.4652 0.5031 0.1888 0.092 Uiso 1 1 calc R . . C6 C 0.2653(6) 0.4690(7) 0.18039(15) 0.1032(19) Uani 1 1 d . . . H6A H 0.2374 0.5479 0.1791 0.124 Uiso 1 1 calc R . . C7 C 0.1722(6) 0.3799(8) 0.17683(16) 0.110(2) Uani 1 1 d . . . H7A H 0.0807 0.3980 0.1735 0.132 Uiso 1 1 calc R . . C8 C 0.2126(6) 0.2663(8) 0.17817(19) 0.111(2) Uani 1 1 d . . . H8A H 0.1489 0.2059 0.1751 0.133 Uiso 1 1 calc R . . C9 C 0.3493(5) 0.2375(5) 0.18409(17) 0.0918(15) Uani 1 1 d . . . H9A H 0.3748 0.1580 0.1859 0.110 Uiso 1 1 calc R . . C10 C 0.6314(4) 0.3236(3) 0.24150(11) 0.0592(9) Uani 1 1 d . . . C11 C 0.5507(5) 0.2779(5) 0.27316(12) 0.0820(13) Uani 1 1 d . . . H11A H 0.4750 0.2322 0.2664 0.098 Uiso 1 1 calc R . . C12 C 0.5820(8) 0.2997(6) 0.31495(16) 0.112(2) Uani 1 1 d . . . H12A H 0.5269 0.2683 0.3360 0.135 Uiso 1 1 calc R . . C13 C 0.6919(7) 0.3664(6) 0.32586(15) 0.1047(19) Uani 1 1 d . . . H13A H 0.7127 0.3800 0.3540 0.126 Uiso 1 1 calc R . . C14 C 0.7682(7) 0.4113(5) 0.29564(17) 0.1062(18) Uani 1 1 d . . . H14A H 0.8421 0.4583 0.3030 0.127 Uiso 1 1 calc R . . C15 C 0.7421(5) 0.3910(5) 0.25250(14) 0.0880(13) Uani 1 1 d . . . H15A H 0.7988 0.4227 0.2320 0.106 Uiso 1 1 calc R . . C16 C 0.8313(4) 0.0197(4) 0.18119(11) 0.0602(9) Uani 1 1 d . . . C17 C 0.7994(6) -0.0811(5) 0.20395(14) 0.0847(14) Uani 1 1 d . . . H17A H 0.7490 -0.0739 0.2286 0.102 Uiso 1 1 calc R . . C18 C 0.8409(7) -0.1920(5) 0.19081(17) 0.0985(17) Uani 1 1 d . . . H18A H 0.8217 -0.2582 0.2073 0.118 Uiso 1 1 calc R . . C19 C 0.9093(6) -0.2059(5) 0.15403(17) 0.0941(15) Uani 1 1 d . . . H19A H 0.9330 -0.2812 0.1444 0.113 Uiso 1 1 calc R . . C20 C 0.9434(5) -0.1043(5) 0.13084(14) 0.0824(13) Uani 1 1 d . . . H20A H 0.9923 -0.1118 0.1059 0.099 Uiso 1 1 calc R . . C21 C 0.9060(4) 0.0042(4) 0.14435(12) 0.0654(10) Uani 1 1 d . . . H21A H 0.9307 0.0706 0.1287 0.079 Uiso 1 1 calc R . . C22 C 0.6281(3) 0.1062(3) 0.10788(10) 0.0488(7) Uani 1 1 d . . . H22A H 0.6008 0.0342 0.1195 0.059 Uiso 1 1 calc R . . C23 C 0.6378(3) 0.1132(3) 0.06234(10) 0.0456(7) Uani 1 1 d . . . C24 C 0.6352(4) 0.0097(3) 0.03833(11) 0.0510(8) Uani 1 1 d . . . H24A H 0.6279 -0.0634 0.0518 0.061 Uiso 1 1 calc R . . C25 C 0.6433(3) 0.0132(3) -0.00554(10) 0.0494(8) Uani 1 1 d . . . C26 C 0.6536(3) 0.1251(3) -0.02420(10) 0.0484(7) Uani 1 1 d . . . H26A H 0.6596 0.1284 -0.0534 0.058 Uiso 1 1 calc R . . C27 C 0.6556(3) 0.2330(3) -0.00211(10) 0.0437(7) Uani 1 1 d . . . C28 C 0.6497(3) 0.2256(3) 0.04188(10) 0.0448(7) Uani 1 1 d . . . C29 C 0.6458(4) -0.0994(3) -0.03272(12) 0.0593(9) Uani 1 1 d . . . C33 C 0.6617(3) 0.3526(3) -0.02501(10) 0.0519(8) Uani 1 1 d . . . C34 C 0.6824(5) 0.3370(4) -0.07292(12) 0.0734(12) Uani 1 1 d . . . H34A H 0.6090 0.2910 -0.0843 0.110 Uiso 1 1 calc R . . H34B H 0.7668 0.2968 -0.0780 0.110 Uiso 1 1 calc R . . H34C H 0.6842 0.4137 -0.0862 0.110 Uiso 1 1 calc R . . C35 C 0.5264(5) 0.4173(4) -0.01866(15) 0.0740(11) Uani 1 1 d . . . H35A H 0.5103 0.4281 0.0109 0.111 Uiso 1 1 calc R . . H35B H 0.4543 0.3709 -0.0306 0.111 Uiso 1 1 calc R . . H35C H 0.5299 0.4934 -0.0323 0.111 Uiso 1 1 calc R . . C36 C 0.7801(4) 0.4277(4) -0.00883(13) 0.0667(10) Uani 1 1 d . . . H36A H 0.7707 0.4392 0.0210 0.100 Uiso 1 1 calc R . . H36B H 0.7798 0.5034 -0.0227 0.100 Uiso 1 1 calc R . . H36C H 0.8641 0.3875 -0.0146 0.100 Uiso 1 1 calc R . . C37 C 0.6296(9) 0.5931(5) 0.1101(2) 0.138(3) Uani 1 1 d . . . H37A H 0.5491 0.5459 0.1045 0.166 Uiso 1 1 calc R . . H37B H 0.6239 0.6192 0.1392 0.166 Uiso 1 1 calc R . . C38 C 0.6248(10) 0.6895(8) 0.0856(2) 0.149(3) Uani 1 1 d . . . H38A H 0.5414 0.7314 0.0906 0.224 Uiso 1 1 calc R . . H38B H 0.6293 0.6659 0.0566 0.224 Uiso 1 1 calc R . . H38C H 0.7002 0.7404 0.0920 0.224 Uiso 1 1 calc R . . C30 C 0.6480(16) -0.0750(6) -0.0779(2) 0.235(8) Uani 1 1 d . . . H30A H 0.5576 -0.0580 -0.0875 0.353 Uiso 1 1 calc R . . H30B H 0.6825 -0.1431 -0.0927 0.353 Uiso 1 1 calc R . . H30C H 0.7055 -0.0078 -0.0834 0.353 Uiso 1 1 calc R . . C31 C 0.7521(14) -0.1768(7) -0.0185(3) 0.226(6) Uani 1 1 d . . . H31A H 0.7247 -0.2149 0.0071 0.338 Uiso 1 1 calc R . . H31B H 0.8331 -0.1314 -0.0137 0.338 Uiso 1 1 calc R . . H31C H 0.7696 -0.2360 -0.0396 0.338 Uiso 1 1 calc R . . C32 C 0.5087(8) -0.1625(7) -0.0261(3) 0.177(4) Uani 1 1 d . . . H32A H 0.4597 -0.1239 -0.0038 0.265 Uiso 1 1 calc R . . H32B H 0.5244 -0.2441 -0.0187 0.265 Uiso 1 1 calc R . . H32C H 0.4565 -0.1589 -0.0516 0.265 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V 0.0505(3) 0.0489(3) 0.0499(3) -0.0052(3) -0.0024(2) -0.0079(2) O1 0.0653(15) 0.0601(15) 0.0536(13) -0.0079(12) 0.0017(11) -0.0035(12) O2 0.0675(15) 0.0425(11) 0.0498(12) -0.0026(10) -0.0077(11) -0.0006(11) O3 0.0477(13) 0.0804(17) 0.0790(16) 0.0019(16) -0.0031(14) -0.0052(11) O4 0.092(2) 0.0502(13) 0.0684(16) -0.0035(11) 0.0045(15) -0.0137(14) N1 0.0518(16) 0.0493(14) 0.0439(14) -0.0016(12) -0.0010(11) -0.0011(12) C1 0.061(2) 0.065(2) 0.0477(18) -0.0070(17) 0.0009(16) -0.0051(17) C2 0.060(2) 0.063(2) 0.0443(17) -0.0013(15) 0.0030(15) -0.0037(17) C3 0.072(2) 0.070(2) 0.0495(18) -0.0049(18) -0.0058(16) -0.001(2) C4 0.061(2) 0.084(3) 0.0413(17) -0.0092(18) -0.0029(16) 0.0021(19) C5 0.074(3) 0.097(3) 0.057(2) 0.010(2) 0.008(2) 0.019(2) C6 0.085(4) 0.152(5) 0.072(3) 0.024(3) 0.002(3) 0.044(4) C7 0.066(3) 0.190(8) 0.074(3) -0.015(4) -0.014(2) 0.023(4) C8 0.063(3) 0.162(6) 0.107(4) -0.048(4) -0.011(3) -0.011(4) C9 0.067(3) 0.108(4) 0.101(4) -0.033(3) -0.006(3) -0.009(3) C10 0.067(2) 0.063(2) 0.0477(18) -0.0091(16) -0.0066(17) 0.0057(17) C11 0.088(3) 0.104(4) 0.054(2) -0.005(2) 0.000(2) -0.023(3) C12 0.140(6) 0.140(5) 0.057(3) 0.008(3) -0.004(3) -0.024(4) C13 0.144(5) 0.119(4) 0.051(2) -0.015(3) -0.027(3) -0.004(4) C14 0.128(5) 0.111(4) 0.079(3) -0.016(3) -0.042(3) -0.020(4) C15 0.089(3) 0.111(3) 0.064(2) -0.014(3) -0.004(2) -0.015(3) C16 0.063(2) 0.070(2) 0.0474(19) 0.0020(17) -0.0018(16) 0.0091(18) C17 0.104(4) 0.085(3) 0.064(2) 0.008(2) 0.019(2) 0.010(3) C18 0.133(5) 0.071(3) 0.091(4) 0.012(3) 0.023(3) 0.011(3) C19 0.102(4) 0.078(3) 0.103(4) -0.006(3) 0.012(3) 0.013(3) C20 0.080(3) 0.101(4) 0.066(2) -0.012(3) 0.010(2) 0.015(3) C21 0.068(2) 0.079(3) 0.0488(19) 0.007(2) 0.0012(17) 0.002(2) C22 0.0498(16) 0.0450(16) 0.0516(19) 0.0040(14) -0.0039(14) -0.0023(13) C23 0.0450(16) 0.0449(17) 0.0468(16) -0.0020(14) -0.0054(13) -0.0040(13) C24 0.0496(18) 0.0438(16) 0.060(2) 0.0011(15) -0.0072(15) -0.0040(15) C25 0.0436(17) 0.0545(18) 0.0500(18) -0.0097(15) -0.0047(14) -0.0036(15) C26 0.0441(16) 0.0543(19) 0.0468(16) -0.0067(15) -0.0059(12) -0.0025(15) C27 0.0318(15) 0.0500(17) 0.0492(17) 0.0006(14) -0.0045(12) -0.0005(13) C28 0.0382(16) 0.0480(16) 0.0482(17) -0.0048(14) -0.0044(13) -0.0025(14) C29 0.057(2) 0.0499(19) 0.070(2) -0.0204(17) -0.0051(17) 0.0016(16) C33 0.0497(18) 0.0542(19) 0.0517(18) 0.0026(16) -0.0057(14) -0.0006(16) C34 0.085(3) 0.079(3) 0.056(2) 0.004(2) -0.0026(19) -0.016(2) C35 0.065(2) 0.076(3) 0.081(3) 0.017(2) 0.000(2) 0.016(2) C36 0.060(2) 0.066(2) 0.075(2) 0.0027(19) 0.0006(19) -0.0202(19) C37 0.205(8) 0.067(3) 0.143(6) 0.030(4) 0.080(6) 0.040(4) C38 0.153(7) 0.173(8) 0.122(5) 0.042(5) 0.000(5) 0.015(6) C30 0.54(2) 0.073(4) 0.093(4) -0.043(4) 0.013(8) 0.002(8) C31 0.338(15) 0.147(6) 0.192(8) -0.107(6) -0.148(9) 0.155(9) C32 0.109(5) 0.129(6) 0.292(11) -0.135(7) 0.016(6) -0.023(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V O3 1.586(3) . ? V O4 1.788(3) . ? V O2 1.843(2) . ? V O1 1.846(2) . ? V N1 2.134(3) . ? O1 C1 1.424(4) . ? O2 C28 1.343(4) . ? O4 C37 1.439(7) . ? N1 C22 1.271(4) . ? N1 C2 1.478(4) . ? C1 C10 1.534(5) . ? C1 C4 1.540(5) . ? C1 C2 1.554(5) . ? C2 C3 1.543(5) . ? C2 H2A 0.9800 . ? C3 C16 1.505(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C9 1.367(7) . ? C4 C5 1.396(6) . ? C5 C6 1.395(7) . ? C5 H5A 0.9300 . ? C6 C7 1.363(10) . ? C6 H6A 0.9300 . ? C7 C8 1.340(10) . ? C7 H7A 0.9300 . ? C8 C9 1.397(8) . ? C8 H8A 0.9300 . ? C9 H9A 0.9300 . ? C10 C15 1.373(6) . ? C10 C11 1.381(6) . ? C11 C12 1.385(6) . ? C11 H11A 0.9300 . ? C12 C13 1.362(9) . ? C12 H12A 0.9300 . ? C13 C14 1.319(8) . ? C13 H13A 0.9300 . ? C14 C15 1.413(6) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 C17 1.381(6) . ? C16 C21 1.393(5) . ? C17 C18 1.379(7) . ? C17 H17A 0.9300 . ? C18 C19 1.357(7) . ? C18 H18A 0.9300 . ? C19 C20 1.401(7) . ? C19 H19A 0.9300 . ? C20 C21 1.345(6) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C23 1.452(4) . ? C22 H22A 0.9300 . ? C23 C24 1.393(5) . ? C23 C28 1.426(4) . ? C24 C25 1.396(5) . ? C24 H24A 0.9300 . ? C25 C26 1.395(5) . ? C25 C29 1.534(5) . ? C26 C27 1.402(4) . ? C26 H26A 0.9300 . ? C27 C28 1.401(5) . ? C27 C33 1.532(5) . ? C29 C31 1.434(9) . ? C29 C30 1.462(8) . ? C29 C32 1.540(8) . ? C33 C36 1.528(5) . ? C33 C35 1.530(5) . ? C33 C34 1.545(5) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.336(8) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? 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 O3 V O4 103.55(15) . . ? O3 V O2 109.60(14) . . ? O4 V O2 95.51(11) . . ? O3 V O1 111.67(14) . . ? O4 V O1 92.45(12) . . ? O2 V O1 134.66(12) . . ? O3 V N1 94.68(13) . . ? O4 V N1 161.29(13) . . ? O2 V N1 82.08(10) . . ? O1 V N1 76.70(11) . . ? C1 O1 V 126.0(2) . . ? C28 O2 V 132.1(2) . . ? C37 O4 V 121.4(3) . . ? C22 N1 C2 122.6(3) . . ? C22 N1 V 125.6(2) . . ? C2 N1 V 111.5(2) . . ? O1 C1 C10 108.0(3) . . ? O1 C1 C4 108.3(3) . . ? C10 C1 C4 109.5(3) . . ? O1 C1 C2 104.6(3) . . ? C10 C1 C2 113.0(3) . . ? C4 C1 C2 113.1(3) . . ? N1 C2 C3 109.2(3) . . ? N1 C2 C1 103.9(3) . . ? C3 C2 C1 113.6(3) . . ? N1 C2 H2A 110.0 . . ? C3 C2 H2A 110.0 . . ? C1 C2 H2A 110.0 . . ? C16 C3 C2 113.2(3) . . ? C16 C3 H3A 108.9 . . ? C2 C3 H3A 108.9 . . ? C16 C3 H3B 108.9 . . ? C2 C3 H3B 108.9 . . ? H3A C3 H3B 107.7 . . ? C9 C4 C5 117.4(4) . . ? C9 C4 C1 124.9(4) . . ? C5 C4 C1 117.6(4) . . ? C6 C5 C4 120.6(6) . . ? C6 C5 H5A 119.7 . . ? C4 C5 H5A 119.7 . . ? C7 C6 C5 120.1(6) . . ? C7 C6 H6A 120.0 . . ? C5 C6 H6A 120.0 . . ? C8 C7 C6 120.0(5) . . ? C8 C7 H7A 120.0 . . ? C6 C7 H7A 120.0 . . ? C7 C8 C9 120.8(6) . . ? C7 C8 H8A 119.6 . . ? C9 C8 H8A 119.6 . . ? C4 C9 C8 121.1(6) . . ? C4 C9 H9A 119.4 . . ? C8 C9 H9A 119.4 . . ? C15 C10 C11 118.5(4) . . ? C15 C10 C1 120.3(4) . . ? C11 C10 C1 121.1(4) . . ? C10 C11 C12 120.2(5) . . ? C10 C11 H11A 119.9 . . ? C12 C11 H11A 119.9 . . ? C13 C12 C11 121.2(6) . . ? C13 C12 H12A 119.4 . . ? C11 C12 H12A 119.4 . . ? C14 C13 C12 118.6(5) . . ? C14 C13 H13A 120.7 . . ? C12 C13 H13A 120.7 . . ? C13 C14 C15 122.7(5) . . ? C13 C14 H14A 118.7 . . ? C15 C14 H14A 118.7 . . ? C10 C15 C14 118.7(5) . . ? C10 C15 H15A 120.6 . . ? C14 C15 H15A 120.6 . . ? C17 C16 C21 117.2(4) . . ? C17 C16 C3 120.2(4) . . ? C21 C16 C3 122.7(4) . . ? C18 C17 C16 121.2(4) . . ? C18 C17 H17A 119.4 . . ? C16 C17 H17A 119.4 . . ? C19 C18 C17 120.8(5) . . ? C19 C18 H18A 119.6 . . ? C17 C18 H18A 119.6 . . ? C18 C19 C20 118.5(5) . . ? C18 C19 H19A 120.7 . . ? C20 C19 H19A 120.7 . . ? C21 C20 C19 120.5(4) . . ? C21 C20 H20A 119.8 . . ? C19 C20 H20A 119.8 . . ? C20 C21 C16 121.8(4) . . ? C20 C21 H21A 119.1 . . ? C16 C21 H21A 119.1 . . ? N1 C22 C23 125.1(3) . . ? N1 C22 H22A 117.4 . . ? C23 C22 H22A 117.4 . . ? C24 C23 C28 119.6(3) . . ? C24 C23 C22 119.9(3) . . ? C28 C23 C22 120.5(3) . . ? C23 C24 C25 121.5(3) . . ? C23 C24 H24A 119.3 . . ? C25 C24 H24A 119.3 . . ? C26 C25 C24 117.0(3) . . ? C26 C25 C29 120.4(3) . . ? C24 C25 C29 122.6(3) . . ? C25 C26 C27 124.7(3) . . ? C25 C26 H26A 117.6 . . ? C27 C26 H26A 117.6 . . ? C26 C27 C28 116.6(3) . . ? C26 C27 C33 121.6(3) . . ? C28 C27 C33 121.8(3) . . ? O2 C28 C27 120.6(3) . . ? O2 C28 C23 118.6(3) . . ? C27 C28 C23 120.7(3) . . ? C31 C29 C30 114.3(7) . . ? C31 C29 C25 109.7(4) . . ? C30 C29 C25 113.4(4) . . ? C31 C29 C32 108.5(7) . . ? C30 C29 C32 103.6(7) . . ? C25 C29 C32 106.8(3) . . ? C36 C33 C35 110.9(3) . . ? C36 C33 C27 110.8(3) . . ? C35 C33 C27 108.7(3) . . ? C36 C33 C34 107.1(3) . . ? C35 C33 C34 107.4(3) . . ? C27 C33 C34 111.9(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 O4 117.7(6) . . ? C38 C37 H37A 107.9 . . ? O4 C37 H37A 107.9 . . ? C38 C37 H37B 107.9 . . ? O4 C37 H37B 107.9 . . ? H37A C37 H37B 107.2 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.98 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.789 _refine_diff_density_min -0.411 _refine_diff_density_rms 0.050 # Attachment '3f.CIF' data_3f _database_code_depnum_ccdc_archive 'CCDC 620540' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ;Ethoxo(2-oxo-benzaldehyde 2S-(2-tert-butylethoxo) imine)oxovanadium(V) ; _chemical_melting_point ? _chemical_formula_moiety (EtO)V(O)[OCH2CH(t-Bu)N=CH(2-O-C6H4)] _chemical_formula_sum 'C15 H22 N O4 V' _chemical_formula_weight 331.28 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) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 8.2505(7) _cell_length_b 11.0013(10) _cell_length_c 9.4013(8) _cell_angle_alpha 90.00 _cell_angle_beta 109.720(2) _cell_angle_gamma 90.00 _cell_volume 803.28(12) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3955 _cell_measurement_theta_min 2.85 _cell_measurement_theta_max 26.0 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.370 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 348 _exptl_absorpt_coefficient_mu 0.631 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.603 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _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 'CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4478 _diffrn_reflns_av_R_equivalents 0.0143 _diffrn_reflns_av_sigmaI/netI 0.0156 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 25.99 _reflns_number_total 3054 _reflns_number_gt 2973 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0561P)^2^+0.0433P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.053(17) _refine_ls_number_reflns 3054 _refine_ls_number_parameters 190 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0273 _refine_ls_R_factor_gt 0.0265 _refine_ls_wR_factor_ref 0.0739 _refine_ls_wR_factor_gt 0.0733 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V V 0.94949(3) 0.71526(2) 0.82608(3) 0.03925(10) Uani 1 1 d . . . N N 1.03976(18) 0.53375(14) 0.84724(15) 0.0347(3) Uani 1 1 d . . . O1 O 1.16748(17) 0.72908(15) 0.96149(16) 0.0532(3) Uani 1 1 d . . . O2 O 0.82468(18) 0.66225(13) 0.62817(15) 0.0458(3) Uani 1 1 d . . . O3 O 0.93883(18) 0.87050(12) 0.77149(19) 0.0513(3) Uani 1 1 d . . . O4 O 0.8234(2) 0.70223(18) 0.92032(19) 0.0629(4) Uani 1 1 d . . . C1 C 1.2499(3) 0.6294(2) 1.0507(2) 0.0484(4) Uani 1 1 d . . . H1A H 1.2059 0.6183 1.1333 0.058 Uiso 1 1 calc R . . H1B H 1.3727 0.6446 1.0932 0.058 Uiso 1 1 calc R . . C2 C 1.2169(2) 0.51521(17) 0.95301(19) 0.0387(4) Uani 1 1 d . . . H2A H 1.2175 0.4446 1.0168 0.046 Uiso 1 1 calc R . . C3 C 1.3474(3) 0.4920(2) 0.8680(2) 0.0465(4) Uani 1 1 d . . . C4 C 1.3560(4) 0.5983(3) 0.7675(3) 0.0692(7) Uani 1 1 d . . . H4B H 1.4374 0.5805 0.7177 0.104 Uiso 1 1 calc R . . H4C H 1.3916 0.6701 0.8281 0.104 Uiso 1 1 calc R . . H4A H 1.2444 0.6115 0.6933 0.104 Uiso 1 1 calc R . . C5 C 1.5251(3) 0.4715(3) 0.9865(4) 0.0738(8) Uani 1 1 d . . . H5A H 1.6078 0.4574 0.9369 0.111 Uiso 1 1 calc R . . H5B H 1.5211 0.4021 1.0472 0.111 Uiso 1 1 calc R . . H5C H 1.5579 0.5421 1.0498 0.111 Uiso 1 1 calc R . . C6 C 1.2986(4) 0.3762(3) 0.7736(4) 0.0723(7) Uani 1 1 d . . . H6A H 1.3791 0.3627 0.7215 0.108 Uiso 1 1 calc R . . H6B H 1.1848 0.3847 0.7013 0.108 Uiso 1 1 calc R . . H6C H 1.3013 0.3084 0.8386 0.108 Uiso 1 1 calc R . . C7 C 0.9437(2) 0.44189(17) 0.7891(2) 0.0381(4) Uani 1 1 d . . . H7A H 0.9790 0.3656 0.8307 0.046 Uiso 1 1 calc R . . C8 C 0.7852(2) 0.44986(17) 0.6636(2) 0.0386(4) Uani 1 1 d . . . C9 C 0.6888(3) 0.34431(19) 0.6071(3) 0.0502(5) Uani 1 1 d . . . H9A H 0.7191 0.2718 0.6605 0.060 Uiso 1 1 calc R . . C10 C 0.5508(3) 0.3460(2) 0.4749(3) 0.0567(5) Uani 1 1 d . . . H10A H 0.4876 0.2757 0.4396 0.068 Uiso 1 1 calc R . . C11 C 0.5069(3) 0.4535(2) 0.3948(2) 0.0529(5) Uani 1 1 d . . . H11A H 0.4129 0.4550 0.3058 0.063 Uiso 1 1 calc R . . C12 C 0.6000(3) 0.55828(18) 0.4447(2) 0.0467(4) Uani 1 1 d . . . H12A H 0.5711 0.6288 0.3871 0.056 Uiso 1 1 calc R . . C13 C 0.7382(2) 0.55933(16) 0.5819(2) 0.0379(4) Uani 1 1 d . . . C14 C 1.0382(4) 0.9236(3) 0.6874(3) 0.0666(6) Uani 1 1 d . . . H14A H 1.0049 0.8872 0.5876 0.080 Uiso 1 1 calc R . . H14B H 1.1595 0.9072 0.7386 0.080 Uiso 1 1 calc R . . C15 C 1.0096(5) 1.0556(3) 0.6733(5) 0.0925(11) Uani 1 1 d . . . H15A H 1.0763 1.0899 0.6170 0.139 Uiso 1 1 calc R . . H15B H 1.0441 1.0915 0.7721 0.139 Uiso 1 1 calc R . . H15C H 0.8897 1.0715 0.6216 0.139 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V 0.03714(15) 0.03339(14) 0.04526(16) -0.00544(13) 0.01134(11) 0.00178(13) N 0.0335(7) 0.0355(7) 0.0337(6) 0.0022(6) 0.0094(5) 0.0010(6) O1 0.0465(7) 0.0435(8) 0.0575(7) -0.0118(7) 0.0017(5) -0.0022(6) O2 0.0482(7) 0.0335(6) 0.0445(6) 0.0012(5) 0.0009(6) 0.0007(5) O3 0.0494(8) 0.0350(7) 0.0645(9) -0.0033(6) 0.0128(7) -0.0013(6) O4 0.0657(9) 0.0560(9) 0.0798(9) -0.0068(9) 0.0414(8) 0.0011(8) C1 0.0433(10) 0.0561(11) 0.0387(9) -0.0049(8) 0.0043(7) 0.0001(8) C2 0.0348(8) 0.0430(10) 0.0348(8) 0.0048(7) 0.0073(7) 0.0009(7) C3 0.0405(9) 0.0533(11) 0.0460(10) 0.0007(8) 0.0149(8) 0.0052(8) C4 0.0690(15) 0.0797(17) 0.0715(14) 0.0186(13) 0.0401(13) 0.0057(14) C5 0.0442(14) 0.095(2) 0.0767(16) 0.0019(14) 0.0132(11) 0.0165(13) C6 0.0674(16) 0.0765(17) 0.0795(17) -0.0205(13) 0.0334(14) 0.0067(13) C7 0.0408(9) 0.0307(8) 0.0417(8) 0.0056(7) 0.0122(7) 0.0020(6) C8 0.0363(8) 0.0378(9) 0.0403(8) -0.0005(7) 0.0111(7) -0.0012(7) C9 0.0509(11) 0.0390(10) 0.0553(11) 0.0046(8) 0.0108(9) -0.0095(8) C10 0.0527(12) 0.0582(13) 0.0534(11) -0.0068(10) 0.0104(9) -0.0190(10) C11 0.0458(10) 0.0635(12) 0.0410(10) -0.0046(9) 0.0037(8) -0.0054(9) C12 0.0465(10) 0.0462(11) 0.0417(9) 0.0015(8) 0.0071(8) 0.0049(8) C13 0.0366(8) 0.0361(9) 0.0407(9) -0.0014(7) 0.0126(7) 0.0036(7) C14 0.0741(17) 0.0557(15) 0.0772(16) 0.0013(11) 0.0350(14) 0.0067(11) C15 0.123(3) 0.0593(18) 0.129(3) 0.0202(16) 0.086(3) 0.0087(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V O4 1.5844(14) . ? V O3 1.7769(15) . ? V O1 1.8257(13) . ? V O2 1.8893(13) . ? V N 2.1170(16) . ? N C7 1.287(2) . ? N C2 1.478(2) . ? O1 C1 1.408(3) . ? O2 C13 1.331(2) . ? O3 C14 1.441(3) . ? C1 C2 1.526(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C3 1.564(2) . ? C2 H2A 0.9800 . ? C3 C4 1.520(3) . ? C3 C6 1.527(3) . ? C3 C5 1.529(3) . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C4 H4A 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C8 1.439(3) . ? C7 H7A 0.9300 . ? C8 C9 1.406(3) . ? C8 C13 1.410(2) . ? C9 C10 1.373(3) . ? C9 H9A 0.9300 . ? C10 C11 1.383(4) . ? C10 H10A 0.9300 . ? C11 C12 1.377(3) . ? C11 H11A 0.9300 . ? C12 C13 1.404(3) . ? C12 H12A 0.9300 . ? C14 C15 1.470(4) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? 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 O4 V O3 105.70(9) . . ? O4 V O1 107.21(8) . . ? O3 V O1 93.58(7) . . ? O4 V O2 106.27(8) . . ? O3 V O2 93.14(7) . . ? O1 V O2 142.54(7) . . ? O4 V N 97.97(8) . . ? O3 V N 156.25(6) . . ? O1 V N 77.32(6) . . ? O2 V N 81.89(6) . . ? C7 N C2 120.31(15) . . ? C7 N V 123.66(12) . . ? C2 N V 115.47(11) . . ? C1 O1 V 120.97(13) . . ? C13 O2 V 129.68(12) . . ? C14 O3 V 124.48(14) . . ? O1 C1 C2 109.30(14) . . ? O1 C1 H1A 109.8 . . ? C2 C1 H1A 109.8 . . ? O1 C1 H1B 109.8 . . ? C2 C1 H1B 109.8 . . ? H1A C1 H1B 108.3 . . ? N C2 C1 103.09(14) . . ? N C2 C3 111.94(14) . . ? C1 C2 C3 115.37(16) . . ? N C2 H2A 108.7 . . ? C1 C2 H2A 108.7 . . ? C3 C2 H2A 108.7 . . ? C4 C3 C6 109.8(2) . . ? C4 C3 C5 109.4(2) . . ? C6 C3 C5 107.5(2) . . ? C4 C3 C2 112.11(17) . . ? C6 C3 C2 109.99(17) . . ? C5 C3 C2 107.93(17) . . ? C3 C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C4 H4A 109.5 . . ? H4B C4 H4A 109.5 . . ? H4C C4 H4A 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C3 C6 H6A 109.5 . . ? C3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N C7 C8 124.05(17) . . ? N C7 H7A 118.0 . . ? C8 C7 H7A 118.0 . . ? C9 C8 C13 118.89(17) . . ? C9 C8 C7 120.07(17) . . ? C13 C8 C7 120.35(16) . . ? C10 C9 C8 121.4(2) . . ? C10 C9 H9A 119.3 . . ? C8 C9 H9A 119.3 . . ? C9 C10 C11 119.3(2) . . ? C9 C10 H10A 120.3 . . ? C11 C10 H10A 120.3 . . ? C12 C11 C10 121.13(18) . . ? C12 C11 H11A 119.4 . . ? C10 C11 H11A 119.4 . . ? C11 C12 C13 120.42(18) . . ? C11 C12 H12A 119.8 . . ? C13 C12 H12A 119.8 . . ? O2 C13 C12 119.14(16) . . ? O2 C13 C8 122.01(16) . . ? C12 C13 C8 118.81(16) . . ? O3 C14 C15 110.2(2) . . ? O3 C14 H14A 109.6 . . ? C15 C14 H14A 109.6 . . ? O3 C14 H14B 109.6 . . ? C15 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.266 _refine_diff_density_min -0.175 _refine_diff_density_rms 0.039 # Attachment '3i.CIF' data_3i _database_code_depnum_ccdc_archive 'CCDC 620541' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ; Ethoxo(2-oxo-3,5-di-tert-butylbenzaldehyde 2S-(1R,3- diphenylpropoxo) imine)oxovanadium(V) ; _chemical_melting_point ? _chemical_formula_moiety (EtO)V(O)[OCH(Ph)CH(Bn)N=CH(2-O-3,5-(t-Bu)2-C6H2)] _chemical_formula_sum 'C32 H40 N O4 V' _chemical_formula_weight 553.59 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 6.3509(4) _cell_length_b 19.3947(12) _cell_length_c 25.8562(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3184.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5507 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 24.4 _exptl_crystal_description tube _exptl_crystal_colour red _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.155 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1176 _exptl_absorpt_coefficient_mu 0.344 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.779 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _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 'CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 18010 _diffrn_reflns_av_R_equivalents 0.0353 _diffrn_reflns_av_sigmaI/netI 0.0412 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.89 _diffrn_reflns_theta_max 26.02 _reflns_number_total 6243 _reflns_number_gt 4547 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0907P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(3) _refine_ls_number_reflns 6243 _refine_ls_number_parameters 343 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0757 _refine_ls_R_factor_gt 0.0530 _refine_ls_wR_factor_ref 0.1501 _refine_ls_wR_factor_gt 0.1367 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V V 0.48945(9) 0.05121(3) 0.85135(2) 0.0579(2) Uani 1 1 d . . . N N 0.2105(4) 0.09760(12) 0.87963(9) 0.0423(6) Uani 1 1 d . . . O1 O 0.3595(4) 0.08056(12) 0.79173(9) 0.0638(7) Uani 1 1 d . . . O2 O 0.4211(4) -0.01470(11) 0.89990(8) 0.0550(6) Uani 1 1 d . . . O3 O 0.6733(5) 0.00107(17) 0.81677(12) 0.0902(10) Uani 1 1 d . . . O4 O 0.6357(4) 0.10894(15) 0.87667(12) 0.0776(8) Uani 1 1 d . . . C1 C 0.1497(6) 0.10618(18) 0.79077(12) 0.0539(8) Uani 1 1 d . . . H1A H 0.0533 0.0667 0.7907 0.065 Uiso 1 1 calc R . . C2 C 0.1196(5) 0.14568(15) 0.84176(11) 0.0444(7) Uani 1 1 d . . . H2A H -0.0308 0.1524 0.8487 0.053 Uiso 1 1 calc R . . C3 C 0.2342(5) 0.21501(16) 0.84272(12) 0.0504(8) Uani 1 1 d . . . H3A H 0.3840 0.2067 0.8388 0.060 Uiso 1 1 calc R . . H3B H 0.1884 0.2421 0.8132 0.060 Uiso 1 1 calc R . . C4 C 0.1050(6) 0.14926(19) 0.74357(13) 0.0590(9) Uani 1 1 d . . . C5 C 0.2642(8) 0.1808(2) 0.71670(15) 0.0817(13) Uani 1 1 d . . . H5A H 0.4035 0.1737 0.7264 0.098 Uiso 1 1 calc R . . C6 C 0.2182(9) 0.2234(3) 0.67494(18) 0.0974(16) Uani 1 1 d . . . H6A H 0.3269 0.2454 0.6574 0.117 Uiso 1 1 calc R . . C7 C 0.0193(11) 0.2329(3) 0.65982(17) 0.0999(16) Uani 1 1 d . . . H7A H -0.0101 0.2614 0.6318 0.120 Uiso 1 1 calc R . . C8 C -0.1387(10) 0.2012(3) 0.6852(2) 0.118(2) Uani 1 1 d . . . H8A H -0.2770 0.2078 0.6744 0.141 Uiso 1 1 calc R . . C9 C -0.0972(8) 0.1589(3) 0.72700(19) 0.0911(15) Uani 1 1 d . . . H9A H -0.2075 0.1370 0.7440 0.109 Uiso 1 1 calc R . . C10 C 0.1993(6) 0.25632(16) 0.89086(13) 0.0551(9) Uani 1 1 d . . . C11 C 0.0227(8) 0.2967(2) 0.89651(15) 0.0783(11) Uani 1 1 d . . . H11A H -0.0787 0.2974 0.8705 0.094 Uiso 1 1 calc R . . C12 C -0.0057(10) 0.3367(2) 0.94113(19) 0.0907(13) Uani 1 1 d . . . H12A H -0.1249 0.3641 0.9448 0.109 Uiso 1 1 calc R . . C13 C 0.1435(9) 0.3349(2) 0.97904(17) 0.0824(14) Uani 1 1 d . . . H13A H 0.1274 0.3622 1.0083 0.099 Uiso 1 1 calc R . . C14 C 0.3119(9) 0.2945(2) 0.97458(16) 0.0772(12) Uani 1 1 d . . . H14A H 0.4096 0.2925 1.0013 0.093 Uiso 1 1 calc R . . C15 C 0.3424(7) 0.25565(18) 0.93070(14) 0.0644(10) Uani 1 1 d . . . H15A H 0.4623 0.2284 0.9279 0.077 Uiso 1 1 calc R . . C16 C 0.1238(5) 0.08748(15) 0.92333(11) 0.0428(7) Uani 1 1 d . . . H16A H 0.0054 0.1136 0.9314 0.051 Uiso 1 1 calc R . . C17 C 0.1965(5) 0.03824(15) 0.96133(11) 0.0430(7) Uani 1 1 d . . . C18 C 0.1130(6) 0.04016(16) 1.01171(11) 0.0507(8) Uani 1 1 d . . . H18A H 0.0136 0.0736 1.0200 0.061 Uiso 1 1 calc R . . C19 C 0.1754(5) -0.00632(17) 1.04898(13) 0.0526(8) Uani 1 1 d . . . C20 C 0.3143(5) -0.05853(17) 1.03301(12) 0.0527(8) Uani 1 1 d . . . H20A H 0.3537 -0.0914 1.0574 0.063 Uiso 1 1 calc R . . C21 C 0.3967(5) -0.06462(15) 0.98373(12) 0.0480(7) Uani 1 1 d . . . C22 C 0.3414(5) -0.01348(15) 0.94785(12) 0.0447(7) Uani 1 1 d . . . C23 C 0.0936(7) -0.0046(2) 1.10468(13) 0.0685(10) Uani 1 1 d . . . C24 C -0.0365(12) -0.0688(3) 1.11461(19) 0.127(2) Uani 1 1 d . . . H24A H -0.1557 -0.0693 1.0918 0.191 Uiso 1 1 calc R . . H24B H -0.0845 -0.0688 1.1498 0.191 Uiso 1 1 calc R . . H24C H 0.0482 -0.1090 1.1085 0.191 Uiso 1 1 calc R . . C25 C -0.0389(12) 0.0591(3) 1.11522(17) 0.133(3) Uani 1 1 d . . . H25A H -0.1580 0.0595 1.0924 0.200 Uiso 1 1 calc R . . H25B H 0.0446 0.0996 1.1096 0.200 Uiso 1 1 calc R . . H25C H -0.0870 0.0583 1.1504 0.200 Uiso 1 1 calc R . . C26 C 0.2827(9) -0.0048(3) 1.14209(17) 0.1007(16) Uani 1 1 d . . . H26A H 0.3670 -0.0451 1.1360 0.151 Uiso 1 1 calc R . . H26B H 0.2325 -0.0053 1.1771 0.151 Uiso 1 1 calc R . . H26C H 0.3662 0.0357 1.1365 0.151 Uiso 1 1 calc R . . C27 C 0.5382(7) -0.12597(17) 0.96857(14) 0.0636(10) Uani 1 1 d . . . C28 C 0.5692(9) -0.1758(2) 1.01400(16) 0.0873(15) Uani 1 1 d . . . H28A H 0.6372 -0.1521 1.0420 0.131 Uiso 1 1 calc R . . H28B H 0.6550 -0.2139 1.0031 0.131 Uiso 1 1 calc R . . H28C H 0.4346 -0.1926 1.0253 0.131 Uiso 1 1 calc R . . C29 C 0.7547(8) -0.1006(3) 0.9509(2) 0.0941(15) Uani 1 1 d . . . H29A H 0.7382 -0.0694 0.9224 0.141 Uiso 1 1 calc R . . H29B H 0.8387 -0.1393 0.9403 0.141 Uiso 1 1 calc R . . H29C H 0.8232 -0.0772 0.9790 0.141 Uiso 1 1 calc R . . C30 C 0.4278(8) -0.16653(19) 0.92539(15) 0.0794(13) Uani 1 1 d . . . H30A H 0.4077 -0.1371 0.8959 0.119 Uiso 1 1 calc R . . H30B H 0.2936 -0.1825 0.9375 0.119 Uiso 1 1 calc R . . H30C H 0.5132 -0.2053 0.9157 0.119 Uiso 1 1 calc R . . C31 C 0.6257(15) -0.0510(4) 0.7807(3) 0.156(3) Uani 1 1 d . . . H31A H 0.5485 -0.0313 0.7519 0.187 Uiso 1 1 calc R . . H31B H 0.5374 -0.0856 0.7969 0.187 Uiso 1 1 calc R . . C32 C 0.8239(19) -0.0839(5) 0.7613(4) 0.232(5) Uani 1 1 d . . . H32A H 0.7893 -0.1194 0.7369 0.348 Uiso 1 1 calc R . . H32B H 0.8994 -0.1038 0.7898 0.348 Uiso 1 1 calc R . . H32C H 0.9101 -0.0497 0.7448 0.348 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V 0.0550(3) 0.0728(4) 0.0458(3) 0.0114(3) 0.0149(3) 0.0133(3) N 0.0432(13) 0.0478(14) 0.0358(14) 0.0026(11) 0.0029(11) -0.0025(12) O1 0.0770(17) 0.0735(15) 0.0410(13) 0.0069(11) 0.0146(12) 0.0168(13) O2 0.0654(14) 0.0581(13) 0.0416(12) 0.0041(10) 0.0101(11) 0.0104(11) O3 0.091(2) 0.112(2) 0.0678(18) 0.0135(18) 0.0190(16) 0.0326(19) O4 0.0475(14) 0.0977(19) 0.088(2) 0.0051(16) -0.0005(13) -0.0160(14) C1 0.064(2) 0.0580(19) 0.0400(17) 0.0027(15) -0.0052(16) -0.0049(17) C2 0.0434(16) 0.0558(17) 0.0340(16) 0.0073(13) 0.0032(13) 0.0006(14) C3 0.0583(19) 0.0511(17) 0.0417(18) 0.0050(14) 0.0021(15) -0.0031(15) C4 0.075(2) 0.063(2) 0.0393(18) 0.0015(16) -0.0061(18) -0.0047(19) C5 0.082(3) 0.109(3) 0.054(2) 0.029(2) 0.014(2) 0.016(3) C6 0.099(4) 0.134(4) 0.059(3) 0.039(3) 0.014(3) 0.010(3) C7 0.129(4) 0.109(3) 0.061(3) 0.035(2) -0.017(3) 0.003(4) C8 0.096(4) 0.157(5) 0.099(4) 0.058(4) -0.042(3) -0.017(4) C9 0.071(3) 0.126(4) 0.077(3) 0.031(3) -0.025(2) -0.029(3) C10 0.070(2) 0.0460(17) 0.0489(19) 0.0048(15) 0.0073(18) 0.0009(17) C11 0.083(3) 0.089(3) 0.062(2) 0.002(2) -0.003(2) 0.020(3) C12 0.100(3) 0.079(3) 0.093(3) -0.009(2) 0.021(3) 0.026(3) C13 0.127(4) 0.065(2) 0.055(2) -0.008(2) 0.014(3) -0.010(3) C14 0.108(4) 0.062(2) 0.062(3) -0.011(2) -0.012(2) 0.000(3) C15 0.076(3) 0.055(2) 0.062(2) -0.0002(17) -0.011(2) -0.0020(19) C16 0.0423(16) 0.0475(16) 0.0385(16) 0.0009(13) 0.0010(13) -0.0017(13) C17 0.0475(16) 0.0472(17) 0.0343(15) 0.0053(13) 0.0029(13) -0.0022(14) C18 0.0591(19) 0.0540(18) 0.0389(16) 0.0024(14) 0.0079(15) 0.0046(16) C19 0.059(2) 0.0579(19) 0.0408(17) 0.0084(15) 0.0054(15) 0.0018(17) C20 0.065(2) 0.0493(17) 0.0436(17) 0.0090(15) -0.0036(15) 0.0011(17) C21 0.0534(17) 0.0424(17) 0.0482(18) 0.0029(14) -0.0050(15) -0.0023(14) C22 0.0483(17) 0.0495(17) 0.0364(16) 0.0000(13) 0.0013(13) -0.0012(15) C23 0.086(3) 0.079(2) 0.0397(19) 0.0188(18) 0.0121(19) 0.012(2) C24 0.151(6) 0.159(5) 0.072(3) 0.028(3) 0.034(3) -0.041(5) C25 0.190(7) 0.154(5) 0.054(3) 0.024(3) 0.056(3) 0.081(5) C26 0.131(4) 0.124(4) 0.047(2) 0.003(3) -0.004(3) 0.001(3) C27 0.078(3) 0.0553(19) 0.058(2) 0.0060(16) -0.0029(19) 0.0144(19) C28 0.122(4) 0.068(2) 0.072(3) 0.014(2) 0.001(3) 0.035(3) C29 0.074(3) 0.097(3) 0.112(4) 0.013(3) 0.014(3) 0.025(3) C30 0.117(4) 0.059(2) 0.062(2) -0.0121(18) 0.000(2) 0.002(2) C31 0.196(8) 0.140(5) 0.133(5) -0.053(5) -0.003(5) 0.049(6) C32 0.269(13) 0.253(10) 0.175(9) -0.057(8) 0.050(8) 0.129(10) _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 O4 1.595(3) . ? V O3 1.763(3) . ? V O1 1.839(3) . ? V O2 1.844(2) . ? V N 2.117(3) . ? N C16 1.272(4) . ? N C2 1.471(4) . ? O1 C1 1.422(4) . ? O2 C22 1.339(4) . ? O3 C31 1.407(7) . ? C1 C4 1.506(5) . ? C1 C2 1.537(4) . ? C1 H1A 0.9800 . ? C2 C3 1.529(4) . ? C2 H2A 0.9800 . ? C3 C10 1.497(5) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C9 1.367(6) . ? C4 C5 1.371(6) . ? C5 C6 1.390(6) . ? C5 H5A 0.9300 . ? C6 C7 1.335(8) . ? C6 H6A 0.9300 . ? C7 C8 1.347(8) . ? C7 H7A 0.9300 . ? C8 C9 1.382(6) . ? C8 H8A 0.9300 . ? C9 H9A 0.9300 . ? C10 C15 1.374(5) . ? C10 C11 1.376(6) . ? C11 C12 1.402(6) . ? C11 H11A 0.9300 . ? C12 C13 1.364(7) . ? C12 H12A 0.9300 . ? C13 C14 1.330(7) . ? C13 H13A 0.9300 . ? C14 C15 1.376(5) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 C17 1.446(4) . ? C16 H16A 0.9300 . ? C17 C22 1.405(4) . ? C17 C18 1.407(4) . ? C18 C19 1.378(4) . ? C18 H18A 0.9300 . ? C19 C20 1.405(5) . ? C19 C23 1.531(5) . ? C20 C21 1.383(5) . ? C20 H20A 0.9300 . ? C21 C22 1.403(4) . ? C21 C27 1.542(5) . ? C23 C24 1.516(7) . ? C23 C25 1.519(6) . ? C23 C26 1.542(7) . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C29 1.530(6) . ? C27 C28 1.534(5) . ? C27 C30 1.535(5) . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 C32 1.498(11) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? 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 O4 V O3 102.09(16) . . ? O4 V O1 112.84(13) . . ? O3 V O1 92.45(12) . . ? O4 V O2 110.13(13) . . ? O3 V O2 96.82(12) . . ? O1 V O2 132.83(12) . . ? O4 V N 92.71(12) . . ? O3 V N 164.51(14) . . ? O1 V N 77.44(10) . . ? O2 V N 82.09(10) . . ? C16 N C2 121.3(3) . . ? C16 N V 127.1(2) . . ? C2 N V 111.61(18) . . ? C1 O1 V 122.9(2) . . ? C22 O2 V 135.0(2) . . ? C31 O3 V 126.1(4) . . ? O1 C1 C4 112.6(3) . . ? O1 C1 C2 106.0(3) . . ? C4 C1 C2 113.3(3) . . ? O1 C1 H1A 108.2 . . ? C4 C1 H1A 108.2 . . ? C2 C1 H1A 108.2 . . ? N C2 C3 111.1(3) . . ? N C2 C1 101.9(2) . . ? C3 C2 C1 113.1(3) . . ? N C2 H2A 110.2 . . ? C3 C2 H2A 110.2 . . ? C1 C2 H2A 110.2 . . ? C10 C3 C2 114.4(3) . . ? C10 C3 H3A 108.7 . . ? C2 C3 H3A 108.7 . . ? C10 C3 H3B 108.7 . . ? C2 C3 H3B 108.7 . . ? H3A C3 H3B 107.6 . . ? C9 C4 C5 118.2(4) . . ? C9 C4 C1 120.5(4) . . ? C5 C4 C1 121.3(4) . . ? C4 C5 C6 120.3(5) . . ? C4 C5 H5A 119.9 . . ? C6 C5 H5A 119.9 . . ? C7 C6 C5 120.5(5) . . ? C7 C6 H6A 119.7 . . ? C5 C6 H6A 119.7 . . ? C6 C7 C8 119.9(4) . . ? C6 C7 H7A 120.0 . . ? C8 C7 H7A 120.0 . . ? C7 C8 C9 120.6(5) . . ? C7 C8 H8A 119.7 . . ? C9 C8 H8A 119.7 . . ? C4 C9 C8 120.4(5) . . ? C4 C9 H9A 119.8 . . ? C8 C9 H9A 119.8 . . ? C15 C10 C11 117.7(3) . . ? C15 C10 C3 121.4(3) . . ? C11 C10 C3 120.9(3) . . ? C10 C11 C12 120.5(4) . . ? C10 C11 H11A 119.8 . . ? C12 C11 H11A 119.8 . . ? C13 C12 C11 119.2(5) . . ? C13 C12 H12A 120.4 . . ? C11 C12 H12A 120.4 . . ? C14 C13 C12 120.8(4) . . ? C14 C13 H13A 119.6 . . ? C12 C13 H13A 119.6 . . ? C13 C14 C15 120.5(4) . . ? C13 C14 H14A 119.8 . . ? C15 C14 H14A 119.8 . . ? C10 C15 C14 121.3(4) . . ? C10 C15 H15A 119.3 . . ? C14 C15 H15A 119.3 . . ? N C16 C17 124.5(3) . . ? N C16 H16A 117.7 . . ? C17 C16 H16A 117.7 . . ? C22 C17 C18 119.7(3) . . ? C22 C17 C16 120.8(3) . . ? C18 C17 C16 119.4(3) . . ? C19 C18 C17 121.5(3) . . ? C19 C18 H18A 119.3 . . ? C17 C18 H18A 119.3 . . ? C18 C19 C20 116.5(3) . . ? C18 C19 C23 123.1(3) . . ? C20 C19 C23 120.3(3) . . ? C21 C20 C19 124.8(3) . . ? C21 C20 H20A 117.6 . . ? C19 C20 H20A 117.6 . . ? C20 C21 C22 117.0(3) . . ? C20 C21 C27 121.4(3) . . ? C22 C21 C27 121.6(3) . . ? O2 C22 C21 120.3(3) . . ? O2 C22 C17 119.3(3) . . ? C21 C22 C17 120.3(3) . . ? C24 C23 C25 109.6(4) . . ? C24 C23 C19 109.1(3) . . ? C25 C23 C19 112.0(3) . . ? C24 C23 C26 108.4(4) . . ? C25 C23 C26 108.7(4) . . ? C19 C23 C26 109.0(4) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C28 108.4(4) . . ? C29 C27 C30 111.0(4) . . ? C28 C27 C30 107.0(3) . . ? C29 C27 C21 110.6(3) . . ? C28 C27 C21 111.5(3) . . ? C30 C27 C21 108.3(3) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O3 C31 C32 110.3(7) . . ? O3 C31 H31A 109.6 . . ? C32 C31 H31A 109.6 . . ? O3 C31 H31B 109.6 . . ? C32 C31 H31B 109.6 . . ? H31A C31 H31B 108.1 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.819 _refine_diff_density_min -0.475 _refine_diff_density_rms 0.049 # Attachment '4a.CIF' data_4a _database_code_depnum_ccdc_archive 'CCDC 620542' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ;(2-propoxo)(2-oxobenzaldehyde 2S-(1,1,3-triphenylpropoxo) imine)oxovanadium(V) ; _chemical_melting_point ? _chemical_formula_moiety (2-PrO)V(O)[OC(Ph)2CH(Bn)N=CH(2-O-C6H4)] _chemical_formula_sum 'C31 H30 N O4 V' _chemical_formula_weight 531.50 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 Orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.9280(8) _cell_length_b 12.6932(10) _cell_length_c 19.5875(15) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2717.0(4) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4067 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 21.3 _exptl_crystal_description block _exptl_crystal_colour 'dark red' _exptl_crystal_size_max 0.63 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.39 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.299 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1112 _exptl_absorpt_coefficient_mu 0.401 _exptl_absorpt_correction_type SADABS _exptl_absorpt_correction_T_min 0.713 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_process_details ? _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 'CCD area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15500 _diffrn_reflns_av_R_equivalents 0.0373 _diffrn_reflns_av_sigmaI/netI 0.0436 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 26.01 _reflns_number_total 5334 _reflns_number_gt 3483 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0463P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.07(3) _refine_ls_number_reflns 5334 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0699 _refine_ls_R_factor_gt 0.0369 _refine_ls_wR_factor_ref 0.0923 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 0.920 _refine_ls_restrained_S_all 0.920 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V V 0.24873(5) 0.65393(3) 0.25386(2) 0.05994(14) Uani 1 1 d . . . O1 O 0.20367(16) 0.68108(13) 0.16547(8) 0.0603(5) Uani 1 1 d . . . O2 O 0.3147(2) 0.71670(17) 0.33167(9) 0.0804(6) Uani 1 1 d . . . O3 O 0.09830(19) 0.66600(16) 0.28712(9) 0.0747(6) Uani 1 1 d . . . O4 O 0.2795(2) 0.53283(14) 0.25855(10) 0.0810(6) Uani 1 1 d . . . N1 N 0.4112(2) 0.71094(16) 0.20797(10) 0.0509(5) Uani 1 1 d . . . C1 C 0.2795(2) 0.71489(19) 0.11112(12) 0.0521(7) Uani 1 1 d . . . C2 C 0.4128(3) 0.69098(19) 0.13423(12) 0.0526(6) Uani 1 1 d . . . H2A H 0.4696 0.7398 0.1118 0.063 Uiso 1 1 calc R . . C3 C 0.4540(3) 0.5763(2) 0.12151(14) 0.0605(7) Uani 1 1 d . . . H3A H 0.3996 0.5288 0.1456 0.073 Uiso 1 1 calc R . . H3B H 0.4480 0.5608 0.0731 0.073 Uiso 1 1 calc R . . C4 C 0.2448(3) 0.65392(19) 0.04636(12) 0.0552(6) Uani 1 1 d . . . C5 C 0.2937(3) 0.6799(2) -0.01604(14) 0.0769(9) Uani 1 1 d . . . H5A H 0.3455 0.7378 -0.0198 0.092 Uiso 1 1 calc R . . C6 C 0.2663(4) 0.6202(3) -0.07382(15) 0.0914(11) Uani 1 1 d . . . H6A H 0.3014 0.6369 -0.1157 0.110 Uiso 1 1 calc R . . C7 C 0.1867(4) 0.5361(3) -0.0684(2) 0.0934(12) Uani 1 1 d . . . H7A H 0.1667 0.4968 -0.1069 0.112 Uiso 1 1 calc R . . C8 C 0.1381(4) 0.5110(3) -0.00735(19) 0.0884(11) Uani 1 1 d . . . H8A H 0.0857 0.4535 -0.0038 0.106 Uiso 1 1 calc R . . C9 C 0.1651(3) 0.5697(2) 0.04998(15) 0.0687(8) Uani 1 1 d . . . H9A H 0.1293 0.5524 0.0915 0.082 Uiso 1 1 calc R . . C10 C 0.2558(3) 0.83327(19) 0.09929(11) 0.0530(6) Uani 1 1 d . . . C11 C 0.1358(3) 0.8678(2) 0.09956(16) 0.0720(9) Uani 1 1 d . . . H11A H 0.0730 0.8196 0.1066 0.086 Uiso 1 1 calc R . . C12 C 0.1076(4) 0.9730(3) 0.08959(18) 0.0882(10) Uani 1 1 d . . . H12A H 0.0263 0.9947 0.0909 0.106 Uiso 1 1 calc R . . C13 C 0.1979(4) 1.0453(3) 0.07783(18) 0.0838(10) Uani 1 1 d . . . H13A H 0.1787 1.1158 0.0705 0.101 Uiso 1 1 calc R . . C14 C 0.3158(4) 1.0123(2) 0.07713(19) 0.0856(11) Uani 1 1 d . . . H14A H 0.3781 1.0608 0.0694 0.103 Uiso 1 1 calc R . . C15 C 0.3448(3) 0.9075(2) 0.08779(17) 0.0746(9) Uani 1 1 d . . . H15A H 0.4265 0.8869 0.0871 0.089 Uiso 1 1 calc R . . C16 C 0.5837(3) 0.5577(2) 0.14504(14) 0.0582(7) Uani 1 1 d . . . C17 C 0.6097(3) 0.5221(2) 0.21015(15) 0.0683(8) Uani 1 1 d . . . H17A H 0.5456 0.5056 0.2395 0.082 Uiso 1 1 calc R . . C18 C 0.7279(4) 0.5106(2) 0.23242(18) 0.0871(11) Uani 1 1 d . . . H18A H 0.7432 0.4862 0.2763 0.104 Uiso 1 1 calc R . . C19 C 0.8227(4) 0.5350(3) 0.1903(2) 0.0953(12) Uani 1 1 d . . . H19A H 0.9027 0.5282 0.2058 0.114 Uiso 1 1 calc R . . C20 C 0.8007(4) 0.5699(3) 0.1247(2) 0.0942(11) Uani 1 1 d . . . H20A H 0.8656 0.5857 0.0957 0.113 Uiso 1 1 calc R . . C21 C 0.6813(3) 0.5810(2) 0.10248(16) 0.0760(9) Uani 1 1 d . . . H21A H 0.6663 0.6046 0.0583 0.091 Uiso 1 1 calc R . . C22 C 0.5064(3) 0.75101(19) 0.23674(14) 0.0547(7) Uani 1 1 d . . . H22A H 0.5707 0.7716 0.2086 0.066 Uiso 1 1 calc R . . C23 C 0.5207(3) 0.7663(2) 0.30880(14) 0.0580(7) Uani 1 1 d . . . C24 C 0.6332(3) 0.8025(2) 0.33502(17) 0.0724(8) Uani 1 1 d . . . H24A H 0.6988 0.8142 0.3057 0.087 Uiso 1 1 calc R . . C25 C 0.6462(4) 0.8204(2) 0.40354(19) 0.0840(10) Uani 1 1 d . . . H25A H 0.7211 0.8433 0.4206 0.101 Uiso 1 1 calc R . . C26 C 0.5510(4) 0.8051(3) 0.44685(18) 0.0885(11) Uani 1 1 d . . . H26A H 0.5614 0.8177 0.4933 0.106 Uiso 1 1 calc R . . C27 C 0.4391(4) 0.7711(3) 0.42295(15) 0.0840(10) Uani 1 1 d . . . H27A H 0.3739 0.7623 0.4530 0.101 Uiso 1 1 calc R . . C28 C 0.4239(3) 0.7498(2) 0.35358(15) 0.0672(8) Uani 1 1 d . . . C29 C 0.0478(4) 0.7708(3) 0.29346(19) 0.0938(11) Uani 1 1 d . . . H29A H 0.1103 0.8201 0.2772 0.113 Uiso 1 1 calc R . . C30 C -0.0588(4) 0.7831(4) 0.2489(3) 0.1310(15) Uani 1 1 d . . . H30A H -0.0363 0.7663 0.2028 0.196 Uiso 1 1 calc R . . H30B H -0.0872 0.8546 0.2510 0.196 Uiso 1 1 calc R . . H30C H -0.1227 0.7366 0.2637 0.196 Uiso 1 1 calc R . . C31 C 0.0285(4) 0.7931(3) 0.3679(2) 0.1250(16) Uani 1 1 d . . . H31A H 0.1047 0.7854 0.3918 0.188 Uiso 1 1 calc R . . H31B H -0.0302 0.7443 0.3861 0.188 Uiso 1 1 calc R . . H31C H -0.0012 0.8637 0.3734 0.188 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V 0.0753(3) 0.0534(2) 0.0511(2) 0.0060(2) 0.0070(3) -0.0095(3) O1 0.0638(12) 0.0639(11) 0.0530(10) 0.0049(9) 0.0075(9) -0.0091(9) O2 0.0892(15) 0.0993(15) 0.0528(11) -0.0043(11) 0.0082(11) -0.0205(13) O3 0.0849(15) 0.0724(13) 0.0669(12) 0.0052(11) 0.0166(11) -0.0159(12) O4 0.1074(18) 0.0592(10) 0.0762(13) 0.0160(9) 0.0066(13) -0.0055(11) N1 0.0636(15) 0.0416(11) 0.0475(12) 0.0001(9) 0.0030(11) 0.0008(11) C1 0.0599(18) 0.0504(14) 0.0460(13) 0.0027(11) 0.0071(12) -0.0046(13) C2 0.0649(18) 0.0467(14) 0.0461(14) 0.0035(11) 0.0029(13) 0.0016(13) C3 0.080(2) 0.0480(15) 0.0534(16) -0.0063(13) 0.0032(15) 0.0014(14) C4 0.0624(16) 0.0520(13) 0.0513(13) -0.0004(12) -0.0015(15) 0.0061(17) C5 0.095(2) 0.079(2) 0.0564(17) -0.0041(15) 0.0076(16) -0.0011(17) C6 0.102(3) 0.117(3) 0.0556(18) -0.0137(17) 0.002(2) 0.016(3) C7 0.097(3) 0.097(3) 0.086(3) -0.035(2) -0.029(2) 0.018(2) C8 0.096(3) 0.082(2) 0.087(3) -0.017(2) -0.022(2) -0.0084(19) C9 0.078(2) 0.0644(18) 0.0639(18) -0.0002(15) -0.0121(16) -0.0035(17) C10 0.0620(17) 0.0527(14) 0.0443(12) -0.0019(10) -0.0007(14) 0.0018(17) C11 0.065(2) 0.064(2) 0.088(2) 0.0056(16) -0.0076(17) -0.0007(16) C12 0.080(3) 0.076(2) 0.109(3) 0.004(2) -0.014(2) 0.023(2) C13 0.102(3) 0.0524(19) 0.097(3) 0.0049(17) -0.003(2) 0.009(2) C14 0.088(3) 0.054(2) 0.115(3) 0.0188(18) 0.009(2) -0.0043(19) C15 0.071(2) 0.0554(18) 0.098(2) 0.0102(17) 0.0163(18) 0.0064(17) C16 0.079(2) 0.0436(15) 0.0516(16) -0.0025(12) -0.0002(16) 0.0114(14) C17 0.095(3) 0.0506(17) 0.0593(18) 0.0037(14) 0.0002(18) 0.0124(16) C18 0.120(3) 0.0672(19) 0.074(2) 0.0086(15) -0.019(2) 0.028(2) C19 0.087(3) 0.079(2) 0.120(3) 0.004(2) -0.023(3) 0.022(2) C20 0.079(2) 0.106(3) 0.098(3) 0.023(2) 0.009(2) 0.025(2) C21 0.087(2) 0.078(2) 0.0634(19) 0.0118(16) 0.0016(19) 0.020(2) C22 0.0651(18) 0.0397(14) 0.0593(18) -0.0016(13) 0.0055(14) 0.0034(13) C23 0.070(2) 0.0434(15) 0.0602(18) -0.0043(13) -0.0102(15) 0.0062(14) C24 0.077(2) 0.0563(17) 0.084(2) -0.0082(16) -0.0120(18) 0.0055(15) C25 0.103(3) 0.066(2) 0.082(2) -0.0144(18) -0.033(2) 0.003(2) C26 0.142(4) 0.063(2) 0.061(2) -0.0067(17) -0.021(2) 0.002(2) C27 0.120(3) 0.081(2) 0.0509(18) -0.0058(16) -0.0067(19) -0.007(2) C28 0.092(2) 0.0529(17) 0.0573(18) -0.0003(14) -0.0016(18) 0.0009(17) C29 0.110(3) 0.086(3) 0.086(2) -0.009(2) 0.028(2) -0.001(2) C30 0.106(3) 0.150(4) 0.137(4) -0.004(3) 0.023(3) 0.027(3) C31 0.160(4) 0.124(3) 0.091(3) -0.024(3) 0.060(3) -0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V O4 1.5761(18) . ? V O3 1.775(2) . ? V O1 1.8328(17) . ? V O2 1.865(2) . ? V N1 2.118(2) . ? O1 C1 1.416(3) . ? O2 C28 1.336(4) . ? O3 C29 1.446(4) . ? N1 C22 1.287(3) . ? N1 C2 1.467(3) . ? C1 C4 1.534(3) . ? C1 C10 1.542(3) . ? C1 C2 1.555(4) . ? C2 C3 1.543(3) . ? C2 H2A 0.9800 . ? C3 C16 1.510(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.374(4) . ? C4 C9 1.380(4) . ? C5 C6 1.395(4) . ? C5 H5A 0.9300 . ? C6 C7 1.381(5) . ? C6 H6A 0.9300 . ? C7 C8 1.347(5) . ? C7 H7A 0.9300 . ? C8 C9 1.380(4) . ? C8 H8A 0.9300 . ? C9 H9A 0.9300 . ? C10 C15 1.374(4) . ? C10 C11 1.382(4) . ? C11 C12 1.384(4) . ? C11 H11A 0.9300 . ? C12 C13 1.367(5) . ? C12 H12A 0.9300 . ? C13 C14 1.355(5) . ? C13 H13A 0.9300 . ? C14 C15 1.383(4) . ? C14 H14A 0.9300 . ? C15 H15A 0.9300 . ? C16 C17 1.382(4) . ? C16 C21 1.385(4) . ? C17 C18 1.371(5) . ? C17 H17A 0.9300 . ? C18 C19 1.360(5) . ? C18 H18A 0.9300 . ? C19 C20 1.380(5) . ? C19 H19A 0.9300 . ? C20 C21 1.383(5) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C23 1.433(4) . ? C22 H22A 0.9300 . ? C23 C28 1.390(4) . ? C23 C24 1.410(4) . ? C24 C25 1.369(4) . ? C24 H24A 0.9300 . ? C25 C26 1.356(5) . ? C25 H25A 0.9300 . ? C26 C27 1.380(5) . ? C26 H26A 0.9300 . ? C27 C28 1.395(4) . ? C27 H27A 0.9300 . ? C29 C30 1.464(5) . ? C29 C31 1.500(5) . ? C29 H29A 0.9800 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? 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 O4 V O3 105.08(10) . . ? O4 V O1 107.20(9) . . ? O3 V O1 94.68(9) . . ? O4 V O2 106.66(11) . . ? O3 V O2 91.21(10) . . ? O1 V O2 142.72(9) . . ? O4 V N1 100.33(10) . . ? O3 V N1 154.54(9) . . ? O1 V N1 76.12(8) . . ? O2 V N1 82.92(9) . . ? C1 O1 V 127.58(15) . . ? C28 O2 V 137.92(19) . . ? C29 O3 V 117.7(2) . . ? C22 N1 C2 119.3(2) . . ? C22 N1 V 128.78(18) . . ? C2 N1 V 111.65(17) . . ? O1 C1 C4 108.9(2) . . ? O1 C1 C10 108.0(2) . . ? C4 C1 C10 109.01(19) . . ? O1 C1 C2 105.69(19) . . ? C4 C1 C2 112.0(2) . . ? C10 C1 C2 113.1(2) . . ? N1 C2 C3 109.0(2) . . ? N1 C2 C1 104.0(2) . . ? C3 C2 C1 114.2(2) . . ? N1 C2 H2A 109.8 . . ? C3 C2 H2A 109.8 . . ? C1 C2 H2A 109.8 . . ? C16 C3 C2 111.9(2) . . ? C16 C3 H3A 109.2 . . ? C2 C3 H3A 109.2 . . ? C16 C3 H3B 109.2 . . ? C2 C3 H3B 109.2 . . ? H3A C3 H3B 107.9 . . ? C5 C4 C9 118.5(3) . . ? C5 C4 C1 121.2(2) . . ? C9 C4 C1 120.3(2) . . ? C4 C5 C6 120.5(3) . . ? C4 C5 H5A 119.7 . . ? C6 C5 H5A 119.7 . . ? C7 C6 C5 119.6(3) . . ? C7 C6 H6A 120.2 . . ? C5 C6 H6A 120.2 . . ? C8 C7 C6 119.9(3) . . ? C8 C7 H7A 120.0 . . ? C6 C7 H7A 120.0 . . ? C7 C8 C9 120.7(4) . . ? C7 C8 H8A 119.6 . . ? C9 C8 H8A 119.6 . . ? C8 C9 C4 120.8(3) . . ? C8 C9 H9A 119.6 . . ? C4 C9 H9A 119.6 . . ? C15 C10 C11 117.0(2) . . ? C15 C10 C1 125.0(3) . . ? C11 C10 C1 117.9(2) . . ? C10 C11 C12 121.2(3) . . ? C10 C11 H11A 119.4 . . ? C12 C11 H11A 119.4 . . ? C13 C12 C11 120.7(3) . . ? C13 C12 H12A 119.7 . . ? C11 C12 H12A 119.7 . . ? C14 C13 C12 118.7(3) . . ? C14 C13 H13A 120.6 . . ? C12 C13 H13A 120.6 . . ? C13 C14 C15 120.9(4) . . ? C13 C14 H14A 119.6 . . ? C15 C14 H14A 119.6 . . ? C10 C15 C14 121.5(3) . . ? C10 C15 H15A 119.3 . . ? C14 C15 H15A 119.3 . . ? C17 C16 C21 117.9(3) . . ? C17 C16 C3 121.7(3) . . ? C21 C16 C3 120.4(3) . . ? C18 C17 C16 121.4(3) . . ? C18 C17 H17A 119.3 . . ? C16 C17 H17A 119.3 . . ? C19 C18 C17 120.0(3) . . ? C19 C18 H18A 120.0 . . ? C17 C18 H18A 120.0 . . ? C18 C19 C20 120.3(4) . . ? C18 C19 H19A 119.8 . . ? C20 C19 H19A 119.8 . . ? C19 C20 C21 119.3(4) . . ? C19 C20 H20A 120.3 . . ? C21 C20 H20A 120.3 . . ? C20 C21 C16 121.0(3) . . ? C20 C21 H21A 119.5 . . ? C16 C21 H21A 119.5 . . ? N1 C22 C23 124.9(3) . . ? N1 C22 H22A 117.5 . . ? C23 C22 H22A 117.5 . . ? C28 C23 C24 118.9(3) . . ? C28 C23 C22 121.2(3) . . ? C24 C23 C22 119.9(3) . . ? C25 C24 C23 120.1(3) . . ? C25 C24 H24A 119.9 . . ? C23 C24 H24A 119.9 . . ? C26 C25 C24 120.7(3) . . ? C26 C25 H25A 119.7 . . ? C24 C25 H25A 119.7 . . ? C25 C26 C27 120.9(3) . . ? C25 C26 H26A 119.6 . . ? C27 C26 H26A 119.6 . . ? C26 C27 C28 119.8(4) . . ? C26 C27 H27A 120.1 . . ? C28 C27 H27A 120.1 . . ? O2 C28 C23 121.6(3) . . ? O2 C28 C27 118.7(3) . . ? C23 C28 C27 119.6(3) . . ? O3 C29 C30 110.5(3) . . ? O3 C29 C31 108.1(3) . . ? C30 C29 C31 116.6(4) . . ? O3 C29 H29A 107.0 . . ? C30 C29 H29A 107.0 . . ? C31 C29 H29A 107.0 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.163 _refine_diff_density_min -0.263 _refine_diff_density_rms 0.032