# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_publication_text _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 loop_ _publ_contact_author_name _publ_contact_author_email 'Cindric, Marina' marina@chem.pmf.hr _publ_contact_author_address ; Department of Chemistry, Faculty of Science, University of Zagreb Horvatovac 102a HR-10000 Zagreb Croatia ; loop_ _publ_author_name M.Rubcic D.Milic G.Horvat I.Dilovic N.Galic V.Tomisic ; M.Cindric ; data_1b _database_code_depnum_ccdc_archive 'CCDC 733234' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Ethoxo-oxo-[salicylaldehydehyde 4-phenylthiosemicarbazonato(2-)]vanadium(V) ; _chemical_name_common ;Ethoxo-oxo-(salicylaldehydehyde 4-phenylthiosemicarbazonato(2- ))vanadium(V) ; _chemical_melting_point ? _chemical_formula_moiety 'C16 H16 N3 O3 S V' _chemical_formula_sum 'C16 H16 N3 O3 S V' _chemical_formula_weight 381.32 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.8123(2) _cell_length_b 9.8588(2) _cell_length_c 16.0968(4) _cell_angle_alpha 90.00 _cell_angle_beta 102.663(2) _cell_angle_gamma 90.00 _cell_volume 1674.12(6) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 7236 _cell_measurement_theta_min 3.7847 _cell_measurement_theta_max 28.4222 _exptl_crystal_description prismatic _exptl_crystal_colour black _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.513 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.736 _exptl_absorpt_correction_T_min 0.828 _exptl_absorpt_correction_T_max 0.895 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10935 _diffrn_reflns_av_R_equivalents 0.0151 _diffrn_reflns_av_sigmaI/netI 0.0148 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.86 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2925 _reflns_number_gt 2505 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.0394P)^2^+0.5495P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2925 _refine_ls_number_parameters 236 _refine_ls_number_restraints 69 _refine_ls_R_factor_all 0.0335 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0741 _refine_ls_wR_factor_gt 0.0694 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.35737(17) -0.11225(18) 0.03740(11) 0.0376(4) Uani 1 1 d . . . C2 C 0.46349(17) -0.17176(18) 0.09080(11) 0.0367(4) Uani 1 1 d . . . C3 C 0.47561(19) -0.31325(19) 0.09075(12) 0.0436(4) Uani 1 1 d . . . H3 H 0.5454 -0.3540 0.1260 0.052 Uiso 1 1 calc R . . C4 C 0.38628(19) -0.3924(2) 0.03959(13) 0.0495(5) Uani 1 1 d . . . H4 H 0.3947 -0.4863 0.0407 0.059 Uiso 1 1 calc R . . C5 C 0.2833(2) -0.3319(2) -0.01382(14) 0.0524(5) Uani 1 1 d . . . H5 H 0.2232 -0.3857 -0.0492 0.063 Uiso 1 1 calc R . . C6 C 0.26851(19) -0.1931(2) -0.01533(13) 0.0477(5) Uani 1 1 d . . . H6 H 0.1990 -0.1537 -0.0517 0.057 Uiso 1 1 calc R . . C7 C 0.56185(17) -0.09071(18) 0.14241(11) 0.0375(4) Uani 1 1 d . A . H7 H 0.6372 -0.1342 0.1673 0.045 Uiso 1 1 calc R . . C8 C 0.65528(16) 0.22063(18) 0.21722(11) 0.0366(4) Uani 1 1 d . A . C9 C 0.87939(17) 0.25839(19) 0.29872(12) 0.0400(4) Uani 1 1 d . . . C10 C 0.9515(2) 0.3509(2) 0.35455(14) 0.0546(5) Uani 1 1 d . . . H10 H 0.9144 0.4304 0.3684 0.066 Uiso 1 1 calc R . . C11 C 1.0773(2) 0.3253(3) 0.38935(15) 0.0650(7) Uani 1 1 d . . . H11 H 1.1248 0.3883 0.4260 0.078 Uiso 1 1 calc R . . C12 C 1.1331(2) 0.2079(3) 0.37049(15) 0.0619(6) Uani 1 1 d . . . H12 H 1.2179 0.1905 0.3946 0.074 Uiso 1 1 calc R . . C13 C 1.0629(2) 0.1165(3) 0.31579(15) 0.0602(6) Uani 1 1 d . . . H13 H 1.1009 0.0371 0.3026 0.072 Uiso 1 1 calc R . . C14 C 0.93569(19) 0.1402(2) 0.27953(14) 0.0502(5) Uani 1 1 d . . . H14 H 0.8890 0.0770 0.2427 0.060 Uiso 1 1 calc R . . O1 O 0.32587(12) 0.08472(14) 0.20256(9) 0.0489(3) Uani 1 1 d . . . O2 O 0.34229(12) 0.02320(13) 0.03600(8) 0.0449(3) Uani 1 1 d . . . O3 O 0.27303(12) 0.27604(13) 0.08089(9) 0.0471(3) Uani 1 1 d D . . C15A C 0.1821(5) 0.3671(5) 0.1021(6) 0.0644(19) Uani 0.715(13) 1 d PDU A 1 H15A H 0.1521 0.4293 0.0553 0.077 Uiso 0.715(13) 1 calc PR A 1 H15B H 0.2205 0.4197 0.1520 0.077 Uiso 0.715(13) 1 calc PR A 1 C16A C 0.0754(6) 0.2869(5) 0.1192(5) 0.090(2) Uani 0.715(13) 1 d PDU A 1 H16A H 0.0150 0.3464 0.1360 0.135 Uiso 0.715(13) 1 calc PR A 1 H16B H 0.1064 0.2234 0.1642 0.135 Uiso 0.715(13) 1 calc PR A 1 H16C H 0.0355 0.2385 0.0687 0.135 Uiso 0.715(13) 1 calc PR A 1 C15B C 0.1883(10) 0.3381(16) 0.1257(6) 0.050(4) Uani 0.285(13) 1 d PDU A 2 H15C H 0.2233 0.4246 0.1482 0.060 Uiso 0.285(13) 1 calc PR A 2 H15D H 0.1814 0.2811 0.1737 0.060 Uiso 0.285(13) 1 calc PR A 2 C16B C 0.0594(11) 0.361(3) 0.0720(12) 0.119(9) Uani 0.285(13) 1 d PDU A 2 H16D H 0.0060 0.3999 0.1060 0.179 Uiso 0.285(13) 1 calc PR A 2 H16E H 0.0243 0.2756 0.0491 0.179 Uiso 0.285(13) 1 calc PR A 2 H16F H 0.0648 0.4212 0.0262 0.179 Uiso 0.285(13) 1 calc PR A 2 N1 N 0.55392(13) 0.03704(15) 0.15683(9) 0.0351(3) Uani 1 1 d . . . N2 N 0.66514(13) 0.09207(16) 0.20574(10) 0.0393(4) Uani 1 1 d . A . N3 N 0.75342(14) 0.29535(16) 0.26296(10) 0.0452(4) Uani 1 1 d . . . H3N H 0.7351 0.3785 0.2712 0.054 Uiso 1 1 calc R . . S1 S 0.52044(4) 0.31636(5) 0.17391(3) 0.04162(14) Uani 1 1 d . . . V1 V 0.37660(3) 0.14415(3) 0.124495(19) 0.03558(11) Uani 1 1 d . A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0372(10) 0.0342(9) 0.0407(10) -0.0017(8) 0.0067(8) 0.0008(8) C2 0.0343(9) 0.0343(10) 0.0413(10) -0.0014(7) 0.0078(8) 0.0002(7) C3 0.0430(11) 0.0352(10) 0.0508(11) -0.0009(8) 0.0062(9) 0.0040(8) C4 0.0525(12) 0.0332(10) 0.0616(13) -0.0043(9) 0.0101(10) -0.0015(9) C5 0.0511(12) 0.0441(12) 0.0572(13) -0.0123(10) 0.0017(10) -0.0083(9) C6 0.0421(11) 0.0452(11) 0.0504(11) -0.0036(9) -0.0018(9) 0.0022(9) C7 0.0324(9) 0.0337(9) 0.0441(10) 0.0014(8) 0.0036(8) 0.0043(7) C8 0.0323(9) 0.0368(10) 0.0393(9) 0.0003(8) 0.0048(7) -0.0003(8) C9 0.0340(10) 0.0411(10) 0.0428(10) 0.0029(8) 0.0035(8) -0.0058(8) C10 0.0492(12) 0.0467(12) 0.0611(13) -0.0059(10) -0.0027(10) -0.0079(10) C11 0.0516(13) 0.0655(16) 0.0668(15) -0.0001(12) -0.0114(11) -0.0183(12) C12 0.0349(11) 0.0728(16) 0.0719(15) 0.0122(13) -0.0017(10) -0.0060(11) C13 0.0396(11) 0.0622(14) 0.0769(15) -0.0005(12) 0.0090(11) 0.0040(11) C14 0.0360(10) 0.0516(12) 0.0597(13) -0.0072(10) 0.0037(9) -0.0009(9) O1 0.0408(7) 0.0464(8) 0.0607(9) 0.0085(7) 0.0141(6) 0.0025(6) O2 0.0445(7) 0.0354(7) 0.0474(8) -0.0014(6) -0.0058(6) 0.0052(6) O3 0.0364(7) 0.0396(7) 0.0599(8) -0.0010(6) -0.0017(6) 0.0071(6) C15A 0.047(3) 0.035(3) 0.107(4) 0.007(2) 0.009(3) 0.0182(17) C16A 0.068(3) 0.077(3) 0.141(5) 0.008(3) 0.056(3) 0.011(2) C15B 0.041(6) 0.018(5) 0.082(7) 0.001(5) -0.007(4) 0.015(4) C16B 0.043(6) 0.18(2) 0.128(12) -0.063(12) -0.008(6) 0.038(9) N1 0.0290(7) 0.0342(8) 0.0396(8) -0.0011(6) 0.0019(6) 0.0009(6) N2 0.0306(8) 0.0362(9) 0.0469(9) -0.0026(7) -0.0005(6) -0.0006(6) N3 0.0368(8) 0.0340(8) 0.0597(10) -0.0086(7) -0.0005(7) -0.0007(7) S1 0.0359(3) 0.0311(2) 0.0540(3) 0.0002(2) 0.0016(2) 0.00230(18) V1 0.02967(17) 0.03081(18) 0.04374(19) 0.00153(13) 0.00255(13) 0.00267(12) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.345(2) . ? C1 C6 1.386(3) . ? C1 C2 1.403(2) . ? C2 C3 1.401(3) . ? C2 C7 1.440(2) . ? C3 C4 1.368(3) . ? C3 H3 0.9300 . ? C4 C5 1.384(3) . ? C4 H4 0.9300 . ? C5 C6 1.378(3) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 N1 1.287(2) . ? C7 H7 0.9300 . ? C8 N2 1.289(2) . ? C8 N3 1.367(2) . ? C8 S1 1.7483(18) . ? C9 C14 1.380(3) . ? C9 C10 1.393(3) . ? C9 N3 1.406(2) . ? C10 C11 1.376(3) . ? C10 H10 0.9300 . ? C11 C12 1.370(4) . ? C11 H11 0.9300 . ? C12 C13 1.367(3) . ? C12 H12 0.9300 . ? C13 C14 1.391(3) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? O1 V1 1.5891(13) . ? O2 V1 1.8322(13) . ? O3 C15B 1.423(5) . ? O3 C15A 1.427(3) . ? O3 V1 1.7586(13) . ? C15A C16A 1.474(4) . ? C15A H15A 0.9700 . ? C15A H15B 0.9700 . ? C16A H16A 0.9600 . ? C16A H16B 0.9600 . ? C16A H16C 0.9600 . ? C15B C16B 1.487(5) . ? C15B H15C 0.9700 . ? C15B H15D 0.9700 . ? C16B H16D 0.9600 . ? C16B H16E 0.9600 . ? C16B H16F 0.9600 . ? N1 N2 1.395(2) . ? N1 V1 2.1504(14) . ? N3 H3N 0.8600 . ? S1 V1 2.3220(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 C6 119.70(17) . . ? O2 C1 C2 120.36(16) . . ? C6 C1 C2 119.93(17) . . ? C3 C2 C1 118.69(17) . . ? C3 C2 C7 119.71(16) . . ? C1 C2 C7 121.55(16) . . ? C4 C3 C2 120.97(18) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 119.60(19) . . ? C3 C4 H4 120.2 . . ? C5 C4 H4 120.2 . . ? C6 C5 C4 120.90(19) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C1 119.89(18) . . ? C5 C6 H6 120.1 . . ? C1 C6 H6 120.1 . . ? N1 C7 C2 125.26(16) . . ? N1 C7 H7 117.4 . . ? C2 C7 H7 117.4 . . ? N2 C8 N3 121.90(16) . . ? N2 C8 S1 124.18(14) . . ? N3 C8 S1 113.89(13) . . ? C14 C9 C10 119.02(18) . . ? C14 C9 N3 124.23(17) . . ? C10 C9 N3 116.71(18) . . ? C11 C10 C9 120.4(2) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C12 C11 C10 120.6(2) . . ? C12 C11 H11 119.7 . . ? C10 C11 H11 119.7 . . ? C13 C12 C11 119.3(2) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C12 C13 C14 121.2(2) . . ? C12 C13 H13 119.4 . . ? C14 C13 H13 119.4 . . ? C9 C14 C13 119.5(2) . . ? C9 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C1 O2 V1 129.05(12) . . ? C15B O3 V1 122.7(5) . . ? C15A O3 V1 141.4(4) . . ? O3 C15A C16A 108.4(4) . . ? O3 C15A H15A 110.0 . . ? C16A C15A H15A 110.0 . . ? O3 C15A H15B 110.0 . . ? C16A C15A H15B 110.0 . . ? H15A C15A H15B 108.4 . . ? C15A C16A H16A 109.5 . . ? C15A C16A H16B 109.5 . . ? H16A C16A H16B 109.5 . . ? C15A C16A H16C 109.5 . . ? H16A C16A H16C 109.5 . . ? H16B C16A H16C 109.5 . . ? O3 C15B C16B 113.2(8) . . ? O3 C15B H15C 108.9 . . ? C16B C15B H15C 108.9 . . ? O3 C15B H15D 108.9 . . ? C16B C15B H15D 108.9 . . ? H15C C15B H15D 107.7 . . ? C15B C16B H16D 109.5 . . ? C15B C16B H16E 109.5 . . ? H16D C16B H16E 109.5 . . ? C15B C16B H16F 109.5 . . ? H16D C16B H16F 109.5 . . ? H16E C16B H16F 109.5 . . ? C7 N1 N2 113.53(14) . . ? C7 N1 V1 121.87(12) . . ? N2 N1 V1 123.94(11) . . ? C8 N2 N1 112.04(14) . . ? C8 N3 C9 130.47(16) . . ? C8 N3 H3N 114.8 . . ? C9 N3 H3N 114.8 . . ? C8 S1 V1 100.33(6) . . ? O1 V1 O3 106.75(7) . . ? O1 V1 O2 109.19(7) . . ? O3 V1 O2 99.69(6) . . ? O1 V1 N1 94.10(6) . . ? O3 V1 N1 156.29(6) . . ? O2 V1 N1 83.48(6) . . ? O1 V1 S1 108.67(5) . . ? O3 V1 S1 85.19(5) . . ? O2 V1 S1 138.46(5) . . ? N1 V1 S1 77.38(4) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.166 _refine_diff_density_min -0.286 _refine_diff_density_rms 0.041 # Attachment 'new_733235.cif' data_1c _database_code_depnum_ccdc_archive 'CCDC 733235' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ;Oxo-propoxo-(salicylaldehyde 4-phenylthiosemicarbazonato(2- ))vanadium(V) ; _chemical_melting_point ? _chemical_formula_moiety 'C17 H18 N3 O3 S V' _chemical_formula_sum 'C17 H18 N3 O3 S V' _chemical_formula_weight 395.34 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' Ca Ca 0.2262 0.3064 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.1837(4) _cell_length_b 8.0325(2) _cell_length_c 16.0582(5) _cell_angle_alpha 90.00 _cell_angle_beta 114.404(4) _cell_angle_gamma 90.00 _cell_volume 1783.52(10) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 5529 _cell_measurement_theta_min 3.7597 _cell_measurement_theta_max 28.9725 _exptl_crystal_description prismatic _exptl_crystal_colour black _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.472 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 0.694 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.761 _exptl_absorpt_correction_T_max 0.841 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9284 _diffrn_reflns_av_R_equivalents 0.0204 _diffrn_reflns_av_sigmaI/netI 0.0307 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 3124 _reflns_number_gt 2455 _reflns_threshold_expression >2\s(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^ > 2\s(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^)+(0.0504P)^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_number_reflns 3124 _refine_ls_number_parameters 254 _refine_ls_number_restraints 113 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0299 _refine_ls_wR_factor_ref 0.0806 _refine_ls_wR_factor_gt 0.0770 _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.30989(14) 0.2087(2) 0.01051(12) 0.0188(4) Uani 1 1 d . . . C2 C 0.38969(14) 0.1990(2) -0.01160(12) 0.0185(4) Uani 1 1 d . . . C3 C 0.38746(15) 0.0841(2) -0.07861(13) 0.0224(5) Uani 1 1 d . . . H3 H 0.4409 0.0773 -0.0948 0.027 Uiso 1 1 calc R . . C4 C 0.30900(16) -0.0185(3) -0.12093(14) 0.0258(5) Uani 1 1 d . . . H4 H 0.3080 -0.0951 -0.1664 0.031 Uiso 1 1 calc R . . C5 C 0.23128(16) -0.0093(3) -0.09667(14) 0.0275(5) Uani 1 1 d . . . H5 H 0.1776 -0.0816 -0.1250 0.033 Uiso 1 1 calc R . . C6 C 0.23096(14) 0.1039(2) -0.03177(13) 0.0230(5) Uani 1 1 d . . . H6 H 0.1771 0.1099 -0.0162 0.028 Uiso 1 1 calc R . . C7 C 0.47630(14) 0.2931(2) 0.03662(12) 0.0168(4) Uani 1 1 d . A . H7 H 0.5311 0.2676 0.0247 0.020 Uiso 1 1 calc R . . C8 C 0.59027(14) 0.5717(2) 0.20482(13) 0.0169(4) Uani 1 1 d . A . C9 C 0.76590(14) 0.6333(2) 0.24702(13) 0.0199(4) Uani 1 1 d . . . C10 C 0.78007(15) 0.5408(3) 0.18004(13) 0.0220(5) Uani 1 1 d . . . H10 H 0.7288 0.4763 0.1374 0.026 Uiso 1 1 calc R . . C11 C 0.86986(15) 0.5441(3) 0.17635(14) 0.0278(5) Uani 1 1 d . . . H11 H 0.8794 0.4816 0.1305 0.033 Uiso 1 1 calc R . . C12 C 0.94545(16) 0.6361(3) 0.23770(15) 0.0356(6) Uani 1 1 d . . . H12 H 1.0064 0.6375 0.2343 0.043 Uiso 1 1 calc R . . C13 C 0.93109(16) 0.7263(3) 0.30425(15) 0.0360(6) Uani 1 1 d . . . H13 H 0.9828 0.7898 0.3470 0.043 Uiso 1 1 calc R . . C14 C 0.84270(15) 0.7253(3) 0.30944(14) 0.0281(5) Uani 1 1 d . . . H14 H 0.8341 0.7877 0.3558 0.034 Uiso 1 1 calc R . . O1 O 0.34183(10) 0.64576(16) 0.02440(9) 0.0226(3) Uani 1 1 d . . . O2 O 0.30889(9) 0.31796(16) 0.07424(8) 0.0193(3) Uani 1 1 d . . . O3 O 0.29124(9) 0.59627(16) 0.16236(9) 0.0212(3) Uani 1 1 d D . . C15A C 0.2256(3) 0.7333(7) 0.1415(11) 0.030(3) Uani 0.557(5) 1 d PDU A 1 H15A H 0.2371 0.8101 0.0988 0.036 Uiso 0.557(5) 1 calc PR A 1 H15B H 0.2365 0.7953 0.1982 0.036 Uiso 0.557(5) 1 calc PR A 1 C16A C 0.1238(3) 0.6711(6) 0.0989(4) 0.0316(13) Uani 0.557(5) 1 d PDU A 1 H16A H 0.1129 0.5949 0.1422 0.038 Uiso 0.557(5) 1 calc PR A 1 H16B H 0.1142 0.6067 0.0432 0.038 Uiso 0.557(5) 1 calc PR A 1 C17A C 0.0504(3) 0.8109(5) 0.0737(3) 0.0384(13) Uani 0.557(5) 1 d PDU A 1 H17A H -0.0150 0.7640 0.0492 0.058 Uiso 0.557(5) 1 calc PR A 1 H17B H 0.0577 0.8820 0.0273 0.058 Uiso 0.557(5) 1 calc PR A 1 H17C H 0.0610 0.8773 0.1282 0.058 Uiso 0.557(5) 1 calc PR A 1 C15B C 0.2433(5) 0.7509(7) 0.1587(14) 0.018(2) Uani 0.443(5) 1 d PDU A 2 H15C H 0.2437 0.8187 0.1074 0.022 Uiso 0.443(5) 1 calc PR A 2 H15D H 0.2783 0.8134 0.2161 0.022 Uiso 0.443(5) 1 calc PR A 2 C16B C 0.1412(4) 0.7221(8) 0.1460(4) 0.0273(15) Uani 0.443(5) 1 d PDU A 2 H16C H 0.1144 0.8273 0.1579 0.033 Uiso 0.443(5) 1 calc PR A 2 H16D H 0.1406 0.6387 0.1911 0.033 Uiso 0.443(5) 1 calc PR A 2 C17B C 0.0776(5) 0.6618(9) 0.0509(4) 0.045(2) Uani 0.443(5) 1 d PDU A 2 H17D H 0.0115 0.6461 0.0455 0.068 Uiso 0.443(5) 1 calc PR A 2 H17E H 0.1026 0.5558 0.0394 0.068 Uiso 0.443(5) 1 calc PR A 2 H17F H 0.0775 0.7445 0.0059 0.068 Uiso 0.443(5) 1 calc PR A 2 N1 N 0.48573(11) 0.41090(19) 0.09552(10) 0.0165(4) Uani 1 1 d . . . N2 N 0.58047(11) 0.46724(19) 0.14006(10) 0.0177(4) Uani 1 1 d . A . N3 N 0.67811(11) 0.6414(2) 0.25654(11) 0.0200(4) Uani 1 1 d . . . H3N H 0.6800 0.7009 0.3033 0.024 Uiso 1 1 calc R . . S1 S 0.49597(4) 0.63256(6) 0.23461(3) 0.02130(14) Uani 1 1 d . . . V1 V 0.36511(2) 0.52611(4) 0.10910(2) 0.01714(12) Uani 1 1 d . A . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0225(11) 0.0167(10) 0.0150(10) 0.0039(8) 0.0057(9) 0.0024(8) C2 0.0208(11) 0.0160(10) 0.0172(10) 0.0042(8) 0.0064(9) 0.0022(8) C3 0.0281(12) 0.0197(10) 0.0185(11) 0.0024(9) 0.0086(9) 0.0053(9) C4 0.0330(13) 0.0206(11) 0.0181(11) -0.0027(9) 0.0047(9) -0.0005(9) C5 0.0273(12) 0.0247(11) 0.0228(12) -0.0028(9) 0.0026(10) -0.0066(9) C6 0.0180(11) 0.0248(11) 0.0227(11) 0.0013(9) 0.0050(9) -0.0020(9) C7 0.0197(10) 0.0166(10) 0.0162(10) 0.0031(8) 0.0096(8) 0.0037(8) C8 0.0171(10) 0.0175(10) 0.0182(10) 0.0015(9) 0.0094(8) -0.0002(8) C9 0.0193(11) 0.0186(10) 0.0217(11) 0.0069(9) 0.0084(9) 0.0019(8) C10 0.0215(11) 0.0262(11) 0.0189(11) 0.0026(9) 0.0090(9) 0.0006(9) C11 0.0226(12) 0.0409(13) 0.0232(11) 0.0060(10) 0.0127(10) 0.0052(10) C12 0.0198(12) 0.0515(15) 0.0376(14) 0.0081(12) 0.0140(11) 0.0004(11) C13 0.0225(12) 0.0452(15) 0.0371(13) -0.0059(12) 0.0091(10) -0.0102(11) C14 0.0254(12) 0.0272(12) 0.0312(13) -0.0009(10) 0.0112(10) -0.0043(10) O1 0.0244(8) 0.0239(7) 0.0219(8) 0.0037(6) 0.0121(6) 0.0048(6) O2 0.0182(7) 0.0193(7) 0.0218(7) -0.0015(6) 0.0098(6) -0.0022(6) O3 0.0207(7) 0.0208(7) 0.0259(8) -0.0009(6) 0.0136(6) 0.0018(6) C15A 0.033(4) 0.027(4) 0.030(6) 0.004(3) 0.014(4) 0.008(3) C16A 0.025(3) 0.033(3) 0.034(4) -0.004(3) 0.009(3) 0.001(2) C17A 0.028(2) 0.040(3) 0.044(3) 0.004(2) 0.012(2) 0.011(2) C15B 0.017(3) 0.014(4) 0.029(6) -0.001(3) 0.014(4) 0.006(3) C16B 0.016(3) 0.032(4) 0.033(4) -0.003(3) 0.010(3) 0.001(2) C17B 0.038(4) 0.050(4) 0.034(4) -0.008(3) 0.002(3) 0.006(3) N1 0.0161(8) 0.0178(8) 0.0164(9) 0.0017(7) 0.0077(7) -0.0006(7) N2 0.0156(8) 0.0184(9) 0.0200(9) -0.0017(7) 0.0083(7) -0.0027(7) N3 0.0190(9) 0.0224(9) 0.0201(9) -0.0063(7) 0.0094(7) -0.0035(7) S1 0.0194(3) 0.0250(3) 0.0219(3) -0.0066(2) 0.0109(2) -0.0007(2) V1 0.0171(2) 0.0180(2) 0.0188(2) 0.00029(14) 0.00991(15) 0.00046(14) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O2 1.353(2) . ? C1 C6 1.390(3) . ? C1 C2 1.398(2) . ? C2 C3 1.407(3) . ? C2 C7 1.435(3) . ? C3 C4 1.375(3) . ? C3 H3 0.9500 . ? C4 C5 1.389(3) . ? C4 H4 0.9500 . ? C5 C6 1.384(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 N1 1.303(2) . ? C7 H7 0.9500 . ? C8 N2 1.296(2) . ? C8 N3 1.366(2) . ? C8 S1 1.7561(18) . ? C9 C14 1.395(3) . ? C9 C10 1.395(3) . ? C9 N3 1.405(2) . ? C10 C11 1.389(3) . ? C10 H10 0.9500 . ? C11 C12 1.378(3) . ? C11 H11 0.9500 . ? C12 C13 1.381(3) . ? C12 H12 0.9500 . ? C13 C14 1.379(3) . ? C13 H13 0.9500 . ? C14 H14 0.9500 . ? O1 V1 1.5816(13) . ? O2 V1 1.8555(13) . ? O3 C15A 1.428(4) . ? O3 C15B 1.429(4) . ? O3 V1 1.7606(12) . ? C15A C16A 1.494(4) . ? C15A H15A 0.9900 . ? C15A H15B 0.9900 . ? C16A C17A 1.515(4) . ? C16A H16A 0.9900 . ? C16A H16B 0.9900 . ? C17A H17A 0.9800 . ? C17A H17B 0.9800 . ? C17A H17C 0.9800 . ? C15B C16B 1.494(5) . ? C15B H15C 0.9900 . ? C15B H15D 0.9900 . ? C16B C17B 1.510(4) . ? C16B H16C 0.9900 . ? C16B H16D 0.9900 . ? C17B H17D 0.9800 . ? C17B H17E 0.9800 . ? C17B H17F 0.9800 . ? N1 N2 1.391(2) . ? N1 V1 2.1420(15) . ? N3 H3N 0.8800 . ? S1 V1 2.3306(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 C1 C6 119.03(17) . . ? O2 C1 C2 120.66(17) . . ? C6 C1 C2 120.30(18) . . ? C1 C2 C3 118.76(18) . . ? C1 C2 C7 122.04(17) . . ? C3 C2 C7 119.03(17) . . ? C4 C3 C2 120.86(19) . . ? C4 C3 H3 119.6 . . ? C2 C3 H3 119.6 . . ? C3 C4 C5 119.50(19) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C6 C5 C4 120.91(19) . . ? C6 C5 H5 119.5 . . ? C4 C5 H5 119.5 . . ? C5 C6 C1 119.65(19) . . ? C5 C6 H6 120.2 . . ? C1 C6 H6 120.2 . . ? N1 C7 C2 125.14(17) . . ? N1 C7 H7 117.4 . . ? C2 C7 H7 117.4 . . ? N2 C8 N3 120.83(17) . . ? N2 C8 S1 124.23(15) . . ? N3 C8 S1 114.93(14) . . ? C14 C9 C10 119.14(19) . . ? C14 C9 N3 116.50(17) . . ? C10 C9 N3 124.36(18) . . ? C11 C10 C9 119.3(2) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C12 C11 C10 121.4(2) . . ? C12 C11 H11 119.3 . . ? C10 C11 H11 119.3 . . ? C11 C12 C13 118.9(2) . . ? C11 C12 H12 120.6 . . ? C13 C12 H12 120.6 . . ? C14 C13 C12 120.9(2) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C9 120.34(19) . . ? C13 C14 H14 119.8 . . ? C9 C14 H14 119.8 . . ? C15A O3 V1 130.9(7) . . ? C15B O3 V1 132.4(7) . . ? O3 C15A C16A 109.8(4) . . ? O3 C15A H15A 109.7 . . ? C16A C15A H15A 109.7 . . ? O3 C15A H15B 109.7 . . ? C16A C15A H15B 109.7 . . ? H15A C15A H15B 108.2 . . ? C15A C16A C17A 112.5(4) . . ? C15A C16A H16A 109.1 . . ? C17A C16A H16A 109.1 . . ? C15A C16A H16B 109.1 . . ? C17A C16A H16B 109.1 . . ? H16A C16A H16B 107.8 . . ? C16A C17A H17A 109.5 . . ? C16A C17A H17B 109.5 . . ? H17A C17A H17B 109.5 . . ? C16A C17A H17C 109.5 . . ? H17A C17A H17C 109.5 . . ? H17B C17A H17C 109.5 . . ? O3 C15B C16B 110.7(5) . . ? O3 C15B H15C 109.5 . . ? C16B C15B H15C 109.5 . . ? O3 C15B H15D 109.5 . . ? C16B C15B H15D 109.5 . . ? H15C C15B H15D 108.1 . . ? C15B C16B C17B 112.4(8) . . ? C15B C16B H16C 109.1 . . ? C17B C16B H16C 109.1 . . ? C15B C16B H16D 109.1 . . ? C17B C16B H16D 109.1 . . ? H16C C16B H16D 107.9 . . ? C16B C17B H17D 109.5 . . ? C16B C17B H17E 109.5 . . ? H17D C17B H17E 109.5 . . ? C16B C17B H17F 109.5 . . ? H17D C17B H17F 109.5 . . ? H17E C17B H17F 109.5 . . ? C7 N1 N2 112.92(15) . . ? C7 N1 V1 123.05(13) . . ? N2 N1 V1 123.58(12) . . ? C8 N2 N1 112.00(15) . . ? C8 N3 C9 130.29(16) . . ? C8 N3 H3N 114.9 . . ? C9 N3 H3N 114.9 . . ? C8 S1 V1 99.33(7) . . ? O1 V1 O3 105.21(6) . . ? O1 V1 O2 112.12(6) . . ? O3 V1 O2 97.41(6) . . ? O1 V1 N1 94.11(6) . . ? O3 V1 N1 158.57(6) . . ? O2 V1 N1 83.46(6) . . ? O1 V1 S1 109.18(5) . . ? O3 V1 S1 87.08(5) . . ? O2 V1 S1 135.49(4) . . ? N1 V1 S1 77.72(4) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.355 _refine_diff_density_min -0.289 _refine_diff_density_rms 0.053 #===END data_3a_x_0.5_MeOH _database_code_depnum_ccdc_archive 'CCDC 733236' _audit_creation_method SHELXL-97 _chemical_name_systematic ;\ dimethoxo-\m-oxo-dioxobis[2-(5-phenylamino-[1,3,4]thiadiazol-2-yl)-phenolato]\ divanadium(V) methanol hemisolvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H26 N6 O7 S2 V2, 0.5(C H4 O)' _chemical_formula_sum 'C30.50 H28 N6 O7.50 S2 V2' _chemical_formula_weight 764.59 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8680(19) _cell_length_b 11.963(2) _cell_length_c 14.3202(9) _cell_angle_alpha 102.100(10) _cell_angle_beta 96.852(8) _cell_angle_gamma 119.640(19) _cell_volume 1667.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 13797 _cell_measurement_theta_min 3.7256 _cell_measurement_theta_max 31.8941 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.523 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 782 _exptl_absorpt_coefficient_mu 0.743 _exptl_absorpt_correction_T_min 0.818 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19578 _diffrn_reflns_av_R_equivalents 0.0183 _diffrn_reflns_av_sigmaI/netI 0.0224 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.69 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5847 _reflns_number_gt 4798 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0630P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5847 _refine_ls_number_parameters 453 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.0400 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0932 _refine_ls_wR_factor_gt 0.0897 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.087 _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 C11 C 1.1798(2) 0.5806(2) 0.35481(14) 0.0241(5) Uani 1 1 d . . . C12 C 1.0563(2) 0.5459(2) 0.37775(14) 0.0233(5) Uani 1 1 d . . . C13 C 1.0332(2) 0.6496(2) 0.41652(14) 0.0243(5) Uani 1 1 d . . . H13 H 0.9492 0.6257 0.4302 0.029 Uiso 1 1 calc R . . C14 C 1.1290(2) 0.7833(2) 0.43487(15) 0.0318(5) Uani 1 1 d . . . H14 H 1.1117 0.8516 0.4606 0.038 Uiso 1 1 calc R . . C15 C 1.2515(3) 0.8174(2) 0.41523(16) 0.0328(5) Uani 1 1 d . . . H15 H 1.3197 0.9100 0.4298 0.039 Uiso 1 1 calc R . . C16 C 1.2764(2) 0.7177(2) 0.37433(15) 0.0288(5) Uani 1 1 d . . . H16 H 1.3602 0.7434 0.3596 0.035 Uiso 1 1 calc R . . C17 C 0.9567(2) 0.4040(2) 0.36071(14) 0.0223(4) Uani 1 1 d . . . C18 C 0.7625(2) 0.1797(2) 0.33037(14) 0.0218(4) Uani 1 1 d . . . C19 C 0.5168(2) 0.0502(2) 0.30257(15) 0.0230(5) Uani 1 1 d . . . C21 C 0.6797(2) -0.1663(2) 0.11311(15) 0.0234(5) Uani 1 1 d . . . C22 C 0.7443(2) -0.1178(2) 0.04138(15) 0.0232(5) Uani 1 1 d . . . C23 C 0.6814(2) -0.1944(2) -0.06063(15) 0.0275(5) Uani 1 1 d . . . H23 H 0.7250 -0.1612 -0.1090 0.033 Uiso 1 1 calc R . . C24 C 0.5598(2) -0.3144(2) -0.09077(17) 0.0361(6) Uani 1 1 d . . . H24 H 0.5202 -0.3643 -0.1591 0.043 Uiso 1 1 calc R . . C25 C 0.4949(2) -0.3626(2) -0.02082(17) 0.0352(6) Uani 1 1 d . . . H25 H 0.4098 -0.4452 -0.0413 0.042 Uiso 1 1 calc R . . C26 C 0.5538(2) -0.2905(2) 0.07945(16) 0.0293(5) Uani 1 1 d . . . H26 H 0.5083 -0.3256 0.1265 0.035 Uiso 1 1 calc R . . C27 C 0.8683(2) 0.0154(2) 0.07414(15) 0.0221(4) Uani 1 1 d . . . C28 C 1.0549(2) 0.2432(2) 0.10200(14) 0.0210(4) Uani 1 1 d . . . C29 C 1.1475(2) 0.4303(2) 0.03101(15) 0.0232(5) Uani 1 1 d . . . C31 C 1.4537(2) 0.4675(3) 0.35395(18) 0.0400(6) Uani 1 1 d . . . H31A H 1.4673 0.5312 0.3167 0.060 Uiso 1 1 calc R . . H31B H 1.5197 0.4414 0.3494 0.060 Uiso 1 1 calc R . . H31C H 1.4649 0.5105 0.4235 0.060 Uiso 1 1 calc R . . C41 C 0.8104(2) -0.1606(2) 0.41552(18) 0.0354(6) Uani 1 1 d . . . H41A H 0.7120 -0.2134 0.3931 0.053 Uiso 1 1 calc R . . H41B H 0.8385 -0.1452 0.4866 0.053 Uiso 1 1 calc R . . H41C H 0.8452 -0.2105 0.3794 0.053 Uiso 1 1 calc R . . C110 C 0.5030(2) 0.1471(2) 0.36809(16) 0.0288(5) Uani 1 1 d . . . H110 H 0.5774 0.2202 0.4199 0.035 Uiso 1 1 calc R . . C111 C 0.3787(2) 0.1326(2) 0.35457(18) 0.0333(5) Uani 1 1 d . . . H111 H 0.3682 0.1979 0.3963 0.040 Uiso 1 1 calc R . . C112 C 0.2690(2) 0.0237(3) 0.28073(18) 0.0376(6) Uani 1 1 d . . . H112 H 0.1846 0.0160 0.2713 0.045 Uiso 1 1 calc R . . C113 C 0.2824(2) -0.0745(2) 0.22027(17) 0.0337(5) Uani 1 1 d . . . H113 H 0.2060 -0.1515 0.1723 0.040 Uiso 1 1 calc R . . C114 C 0.4061(2) -0.0603(2) 0.23000(15) 0.0280(5) Uani 1 1 d . . . H114 H 0.4157 -0.1256 0.1873 0.034 Uiso 1 1 calc R . . C210 C 1.1130(2) 0.3572(2) -0.06985(15) 0.0276(5) Uani 1 1 d . . . H210 H 1.0918 0.2667 -0.0888 0.033 Uiso 1 1 calc R . . C211 C 1.1103(2) 0.4191(2) -0.14026(16) 0.0317(5) Uani 1 1 d . . . H211 H 1.0851 0.3704 -0.2085 0.038 Uiso 1 1 calc R . . C212 C 1.1446(2) 0.5530(2) -0.11169(17) 0.0342(5) Uani 1 1 d . . . H212 H 1.1413 0.5948 -0.1606 0.041 Uiso 1 1 calc R . . C213 C 1.1838(2) 0.6264(2) -0.01142(16) 0.0307(5) Uani 1 1 d . . . H213 H 1.2109 0.7189 0.0075 0.037 Uiso 1 1 calc R . . C214 C 1.1833(2) 0.5650(2) 0.05958(15) 0.0254(5) Uani 1 1 d . . . H214 H 1.2070 0.6138 0.1276 0.030 Uiso 1 1 calc R . . N11 N 0.98265(16) 0.30776(16) 0.34780(11) 0.0207(4) Uani 1 1 d . . . N12 N 0.87344(16) 0.17965(16) 0.33063(11) 0.0203(4) Uani 1 1 d . . . N13 N 0.64339(17) 0.06344(18) 0.31106(13) 0.0247(4) Uani 1 1 d D . . N21 N 0.94662(16) 0.07800(16) 0.16524(12) 0.0201(4) Uani 1 1 d . . . N22 N 1.05387(16) 0.20737(16) 0.18203(12) 0.0203(4) Uani 1 1 d . . . N23 N 1.14621(17) 0.37104(18) 0.10578(13) 0.0236(4) Uani 1 1 d D . . O4 O 1.08520(13) 0.15587(13) 0.34931(9) 0.0214(3) Uani 1 1 d . . . O11 O 1.23875(14) 0.41396(14) 0.47027(10) 0.0279(3) Uani 1 1 d . . . O12 O 1.20389(14) 0.48549(13) 0.31139(10) 0.0232(3) Uani 1 1 d . . . O13 O 1.32160(14) 0.35007(15) 0.31357(10) 0.0274(3) Uani 1 1 d . . . O21 O 0.94688(14) -0.11096(14) 0.24974(10) 0.0259(3) Uani 1 1 d . . . O22 O 0.73018(14) -0.09679(14) 0.21057(10) 0.0236(3) Uani 1 1 d . . . O23 O 0.86153(14) -0.03454(14) 0.39737(10) 0.0258(3) Uani 1 1 d . . . S1 S 0.78748(5) 0.34128(5) 0.35384(4) 0.02418(14) Uani 1 1 d . . . S2 S 0.92548(5) 0.11435(5) -0.00267(4) 0.02352(14) Uani 1 1 d . . . V1 V 1.17748(3) 0.33102(3) 0.35338(2) 0.02104(11) Uani 1 1 d . . . V2 V 0.91646(3) 0.00418(3) 0.29247(2) 0.02015(11) Uani 1 1 d . . . H13N H 0.643(2) -0.0078(19) 0.2788(16) 0.040(7) Uiso 1 1 d D . . H23N H 1.185(2) 0.4263(19) 0.1672(12) 0.023(6) Uiso 1 1 d D . . C51 C 0.495(5) 0.000(4) -0.009(4) 0.101(6) Uani 0.50 1 d PDU A -1 H51A H 0.5809 0.0086 -0.0106 0.151 Uiso 0.50 1 calc PR A -1 H51B H 0.4778 -0.0064 0.0556 0.151 Uiso 0.50 1 calc PR A -1 H51C H 0.4979 0.0799 -0.0194 0.151 Uiso 0.50 1 calc PR A -1 O5 O 0.3901(8) -0.1181(7) -0.0848(6) 0.143(3) Uani 0.50 1 d PDU A -1 H5 H 0.3172 -0.1219 -0.0864 0.214 Uiso 0.50 1 calc PR A -1 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 C11 0.0318(12) 0.0214(11) 0.0184(10) 0.0068(9) 0.0054(9) 0.0137(10) C12 0.0305(12) 0.0231(11) 0.0150(10) 0.0072(8) 0.0056(9) 0.0131(10) C13 0.0345(12) 0.0263(12) 0.0181(10) 0.0083(9) 0.0085(9) 0.0197(10) C14 0.0508(15) 0.0267(12) 0.0222(11) 0.0071(10) 0.0102(10) 0.0236(12) C15 0.0433(14) 0.0197(12) 0.0267(12) 0.0071(10) 0.0073(10) 0.0113(11) C16 0.0294(12) 0.0247(12) 0.0276(12) 0.0097(10) 0.0092(10) 0.0103(10) C17 0.0256(11) 0.0258(12) 0.0186(10) 0.0081(9) 0.0078(9) 0.0152(10) C18 0.0265(11) 0.0248(11) 0.0185(10) 0.0079(9) 0.0078(9) 0.0159(10) C19 0.0210(11) 0.0273(12) 0.0258(11) 0.0140(9) 0.0085(9) 0.0139(10) C21 0.0234(11) 0.0208(11) 0.0277(12) 0.0041(9) 0.0048(9) 0.0147(10) C22 0.0214(11) 0.0223(11) 0.0279(11) 0.0071(9) 0.0064(9) 0.0133(9) C23 0.0290(12) 0.0300(12) 0.0221(11) 0.0047(9) 0.0056(9) 0.0163(10) C24 0.0326(13) 0.0308(13) 0.0306(13) -0.0011(10) 0.0018(10) 0.0124(11) C25 0.0242(12) 0.0251(12) 0.0392(14) 0.0003(11) 0.0035(10) 0.0059(10) C26 0.0256(12) 0.0263(12) 0.0359(13) 0.0103(10) 0.0118(10) 0.0127(10) C27 0.0244(11) 0.0246(11) 0.0224(11) 0.0068(9) 0.0071(9) 0.0167(10) C28 0.0212(11) 0.0225(11) 0.0225(11) 0.0069(9) 0.0079(9) 0.0135(9) C29 0.0221(11) 0.0250(11) 0.0239(11) 0.0095(9) 0.0081(9) 0.0124(10) C31 0.0214(12) 0.0441(15) 0.0409(14) 0.0114(12) 0.0103(11) 0.0083(11) C41 0.0406(14) 0.0272(13) 0.0390(14) 0.0184(11) 0.0148(11) 0.0145(11) C110 0.0285(12) 0.0292(12) 0.0339(12) 0.0120(10) 0.0119(10) 0.0175(11) C111 0.0376(14) 0.0378(14) 0.0459(14) 0.0231(12) 0.0235(12) 0.0287(12) C112 0.0287(13) 0.0485(16) 0.0487(15) 0.0259(13) 0.0151(11) 0.0248(13) C113 0.0264(12) 0.0394(14) 0.0328(13) 0.0160(11) 0.0036(10) 0.0149(11) C114 0.0301(12) 0.0298(13) 0.0278(12) 0.0127(10) 0.0092(10) 0.0169(11) C210 0.0310(12) 0.0253(12) 0.0242(11) 0.0091(9) 0.0076(9) 0.0129(10) C211 0.0371(13) 0.0316(13) 0.0195(11) 0.0082(10) 0.0068(10) 0.0136(11) C212 0.0363(14) 0.0382(14) 0.0323(13) 0.0206(11) 0.0100(11) 0.0190(12) C213 0.0334(13) 0.0240(12) 0.0353(13) 0.0106(10) 0.0095(10) 0.0151(11) C214 0.0244(11) 0.0253(12) 0.0213(11) 0.0049(9) 0.0044(9) 0.0109(10) N11 0.0233(9) 0.0196(9) 0.0197(9) 0.0073(7) 0.0070(7) 0.0112(8) N12 0.0197(9) 0.0197(9) 0.0221(9) 0.0071(7) 0.0071(7) 0.0104(8) N13 0.0210(10) 0.0216(10) 0.0324(10) 0.0062(8) 0.0088(8) 0.0125(8) N21 0.0198(9) 0.0195(9) 0.0217(9) 0.0064(7) 0.0072(7) 0.0105(8) N22 0.0201(9) 0.0207(9) 0.0218(9) 0.0081(7) 0.0069(7) 0.0113(8) N23 0.0269(10) 0.0227(10) 0.0180(9) 0.0061(8) 0.0042(8) 0.0115(8) O4 0.0221(7) 0.0240(8) 0.0217(7) 0.0092(6) 0.0067(6) 0.0139(7) O11 0.0250(8) 0.0280(8) 0.0254(8) 0.0086(7) 0.0042(6) 0.0108(7) O12 0.0261(8) 0.0200(8) 0.0230(7) 0.0064(6) 0.0079(6) 0.0117(7) O13 0.0214(8) 0.0299(8) 0.0324(8) 0.0122(7) 0.0100(6) 0.0132(7) O21 0.0278(8) 0.0243(8) 0.0300(8) 0.0093(6) 0.0085(6) 0.0164(7) O22 0.0235(8) 0.0228(8) 0.0250(8) 0.0059(6) 0.0077(6) 0.0131(7) O23 0.0288(8) 0.0232(8) 0.0267(8) 0.0116(6) 0.0109(6) 0.0127(7) S1 0.0258(3) 0.0228(3) 0.0286(3) 0.0084(2) 0.0092(2) 0.0157(2) S2 0.0257(3) 0.0229(3) 0.0203(3) 0.0067(2) 0.0043(2) 0.0122(2) V1 0.0198(2) 0.0218(2) 0.0219(2) 0.00811(15) 0.00605(15) 0.01078(17) V2 0.0215(2) 0.0198(2) 0.0223(2) 0.00802(15) 0.00770(15) 0.01230(17) C51 0.134(9) 0.133(6) 0.098(16) 0.066(6) 0.057(7) 0.099(5) O5 0.122(6) 0.113(6) 0.168(7) 0.060(5) 0.053(5) 0.036(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 C11 O12 1.353(2) . ? C11 C16 1.398(3) . ? C11 C12 1.414(3) . ? C12 C13 1.415(3) . ? C12 C17 1.453(3) . ? C13 C14 1.369(3) . ? C13 H13 0.9500 . ? C14 C15 1.385(3) . ? C14 H14 0.9500 . ? C15 C16 1.396(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 N11 1.315(3) . ? C17 S1 1.743(2) . ? C18 N12 1.316(2) . ? C18 N13 1.346(3) . ? C18 S1 1.754(2) . ? C19 C114 1.390(3) . ? C19 N13 1.418(3) . ? C19 C110 1.422(3) . ? C21 O22 1.349(2) . ? C21 C22 1.406(3) . ? C21 C26 1.416(3) . ? C22 C23 1.426(3) . ? C22 C27 1.458(3) . ? C23 C24 1.369(3) . ? C23 H23 0.9500 . ? C24 C25 1.384(3) . ? C24 H24 0.9500 . ? C25 C26 1.393(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 N21 1.319(3) . ? C27 S2 1.733(2) . ? C28 N22 1.304(2) . ? C28 N23 1.352(3) . ? C28 S2 1.767(2) . ? C29 C214 1.397(3) . ? C29 N23 1.400(3) . ? C29 C210 1.412(3) . ? C31 O13 1.425(3) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C41 O23 1.417(3) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C110 C111 1.381(3) . ? C110 H110 0.9500 . ? C111 C112 1.388(3) . ? C111 H111 0.9500 . ? C112 C113 1.395(3) . ? C112 H112 0.9500 . ? C113 C114 1.377(3) . ? C113 H113 0.9500 . ? C114 H114 0.9500 . ? C210 C211 1.376(3) . ? C210 H210 0.9500 . ? C211 C212 1.393(3) . ? C211 H211 0.9500 . ? C212 C213 1.399(3) . ? C212 H212 0.9500 . ? C213 C214 1.372(3) . ? C213 H213 0.9500 . ? C214 H214 0.9500 . ? N11 N12 1.375(2) . ? N11 V1 2.1772(17) . ? N12 V2 2.3689(16) . ? N13 H13N 0.880(16) . ? N21 N22 1.377(2) . ? N21 V2 2.1783(16) . ? N22 V1 2.4154(17) . ? N23 H23N 0.883(15) . ? O4 V1 1.8047(14) . ? O4 V2 1.8339(15) . ? O11 V1 1.6170(14) . ? O12 V1 1.9525(14) . ? O13 V1 1.7900(14) . ? O21 V2 1.6104(14) . ? O22 V2 1.9668(15) . ? O23 V2 1.7672(13) . ? C51 O5 1.42(2) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? O5 H5 0.8400 . ? 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 O12 C11 C16 119.92(19) . . ? O12 C11 C12 121.98(19) . . ? C16 C11 C12 118.05(19) . . ? C11 C12 C13 119.41(19) . . ? C11 C12 C17 118.53(18) . . ? C13 C12 C17 122.06(19) . . ? C14 C13 C12 121.7(2) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C13 C14 C15 118.8(2) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? C14 C15 C16 121.1(2) . . ? C14 C15 H15 119.5 . . ? C16 C15 H15 119.5 . . ? C15 C16 C11 120.9(2) . . ? C15 C16 H16 119.5 . . ? C11 C16 H16 119.5 . . ? N11 C17 C12 124.43(19) . . ? N11 C17 S1 112.02(16) . . ? C12 C17 S1 123.55(15) . . ? N12 C18 N13 120.98(18) . . ? N12 C18 S1 113.56(15) . . ? N13 C18 S1 125.44(15) . . ? C114 C19 N13 118.87(18) . . ? C114 C19 C110 120.61(19) . . ? N13 C19 C110 120.51(19) . . ? O22 C21 C22 122.67(19) . . ? O22 C21 C26 119.72(18) . . ? C22 C21 C26 117.55(19) . . ? C21 C22 C23 119.27(19) . . ? C21 C22 C27 118.16(18) . . ? C23 C22 C27 122.36(18) . . ? C24 C23 C22 121.8(2) . . ? C24 C23 H23 119.1 . . ? C22 C23 H23 119.1 . . ? C23 C24 C25 119.4(2) . . ? C23 C24 H24 120.3 . . ? C25 C24 H24 120.3 . . ? C24 C25 C26 120.3(2) . . ? C24 C25 H25 119.9 . . ? C26 C25 H25 119.9 . . ? C25 C26 C21 121.7(2) . . ? C25 C26 H26 119.1 . . ? C21 C26 H26 119.1 . . ? N21 C27 C22 125.10(18) . . ? N21 C27 S2 111.76(15) . . ? C22 C27 S2 123.06(15) . . ? N22 C28 N23 119.87(18) . . ? N22 C28 S2 113.81(15) . . ? N23 C28 S2 126.26(15) . . ? C214 C29 N23 117.54(18) . . ? C214 C29 C210 120.72(19) . . ? N23 C29 C210 121.74(19) . . ? O13 C31 H31A 109.5 . . ? O13 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O13 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? O23 C41 H41A 109.5 . . ? O23 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? O23 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C111 C110 C19 118.4(2) . . ? C111 C110 H110 120.8 . . ? C19 C110 H110 120.8 . . ? C110 C111 C112 120.8(2) . . ? C110 C111 H111 119.6 . . ? C112 C111 H111 119.6 . . ? C111 C112 C113 120.2(2) . . ? C111 C112 H112 119.9 . . ? C113 C112 H112 119.9 . . ? C114 C113 C112 120.2(2) . . ? C114 C113 H113 119.9 . . ? C112 C113 H113 119.9 . . ? C113 C114 C19 119.7(2) . . ? C113 C114 H114 120.1 . . ? C19 C114 H114 120.1 . . ? C211 C210 C29 119.0(2) . . ? C211 C210 H210 120.5 . . ? C29 C210 H210 120.5 . . ? C210 C211 C212 120.1(2) . . ? C210 C211 H211 119.9 . . ? C212 C211 H211 119.9 . . ? C211 C212 C213 120.5(2) . . ? C211 C212 H212 119.8 . . ? C213 C212 H212 119.8 . . ? C214 C213 C212 120.1(2) . . ? C214 C213 H213 119.9 . . ? C212 C213 H213 119.9 . . ? C213 C214 C29 119.46(19) . . ? C213 C214 H214 120.3 . . ? C29 C214 H214 120.3 . . ? C17 N11 N12 115.13(17) . . ? C17 N11 V1 127.15(14) . . ? N12 N11 V1 117.71(12) . . ? C18 N12 N11 111.68(16) . . ? C18 N12 V2 132.97(14) . . ? N11 N12 V2 115.02(11) . . ? C18 N13 C19 125.95(17) . . ? C18 N13 H13N 112.6(16) . . ? C19 N13 H13N 116.7(16) . . ? C27 N21 N22 115.71(16) . . ? C27 N21 V2 127.02(14) . . ? N22 N21 V2 117.12(12) . . ? C28 N22 N21 111.14(16) . . ? C28 N22 V1 133.00(13) . . ? N21 N22 V1 115.04(11) . . ? C28 N23 C29 126.45(18) . . ? C28 N23 H23N 112.0(14) . . ? C29 N23 H23N 116.7(14) . . ? V1 O4 V2 138.66(8) . . ? C11 O12 V1 126.81(12) . . ? C31 O13 V1 124.27(14) . . ? C21 O22 V2 129.55(12) . . ? C41 O23 V2 126.49(13) . . ? C17 S1 C18 87.59(10) . . ? C27 S2 C28 87.48(10) . . ? O11 V1 O13 103.16(7) . . ? O11 V1 O4 104.10(7) . . ? O13 V1 O4 103.10(7) . . ? O11 V1 O12 95.40(7) . . ? O13 V1 O12 88.44(6) . . ? O4 V1 O12 154.19(6) . . ? O11 V1 N11 94.46(7) . . ? O13 V1 N11 159.36(6) . . ? O4 V1 N11 82.56(6) . . ? O12 V1 N11 79.18(6) . . ? O11 V1 N22 170.73(7) . . ? O13 V1 N22 85.88(6) . . ? O4 V1 N22 75.37(6) . . ? O12 V1 N22 82.66(6) . . ? N11 V1 N22 76.28(6) . . ? O21 V2 O23 102.50(7) . . ? O21 V2 O4 102.83(7) . . ? O23 V2 O4 101.88(6) . . ? O21 V2 O22 95.64(7) . . ? O23 V2 O22 91.41(6) . . ? O4 V2 O22 154.16(6) . . ? O21 V2 N21 93.18(7) . . ? O23 V2 N21 162.61(6) . . ? O4 V2 N21 81.60(6) . . ? O22 V2 N21 79.46(6) . . ? O21 V2 N12 170.88(6) . . ? O23 V2 N12 86.34(6) . . ? O4 V2 N12 77.18(6) . . ? O22 V2 N12 81.74(6) . . ? N21 V2 N12 77.77(6) . . ? C51 O5 H5 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.481 _refine_diff_density_min -0.306 _refine_diff_density_rms 0.058 #===END data_3b _database_code_depnum_ccdc_archive 'CCDC 733237' _audit_creation_method SHELXL-97 _chemical_name_systematic ;\ diethoxo-\m-oxo-dioxobis[2-(5-phenylamino-[1,3,4]thiadiazol-2-yl)-phenolato]\ divanadium(V) ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H30 N6 O7 S2 V2' _chemical_formula_sum 'C32 H30 N6 O7 S2 V2' _chemical_formula_weight 776.62 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4910(9) _cell_length_b 11.8518(9) _cell_length_c 14.7813(13) _cell_angle_alpha 92.462(7) _cell_angle_beta 100.455(7) _cell_angle_gamma 118.288(8) _cell_volume 1723.8(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1717 _cell_measurement_theta_min 3.6790 _cell_measurement_theta_max 28.6066 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.496 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 796 _exptl_absorpt_coefficient_mu 0.719 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur CCD' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12872 _diffrn_reflns_av_R_equivalents 0.1016 _diffrn_reflns_av_sigmaI/netI 0.3343 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.68 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5869 _reflns_number_gt 1896 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0352P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5869 _refine_ls_number_parameters 448 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1885 _refine_ls_R_factor_gt 0.0588 _refine_ls_wR_factor_ref 0.1126 _refine_ls_wR_factor_gt 0.0959 _refine_ls_goodness_of_fit_ref 0.711 _refine_ls_restrained_S_all 0.711 _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 H13N H 0.469(5) 0.762(5) 0.3336(17) 0.03(2) Uiso 1 1 d D . . C11 C 1.0706(7) 1.2314(7) 0.3855(5) 0.041(2) Uani 1 1 d . . . C12 C 1.0038(7) 1.1587(7) 0.4539(5) 0.0339(18) Uani 1 1 d . . . C13 C 1.0714(6) 1.2070(6) 0.5493(5) 0.0307(18) Uani 1 1 d . . . H13 H 1.0310 1.1621 0.5949 0.037 Uiso 1 1 calc R . . C14 C 1.1911(7) 1.3151(7) 0.5746(5) 0.044(2) Uani 1 1 d . . . H14 H 1.2324 1.3446 0.6374 0.053 Uiso 1 1 calc R . . C15 C 1.2544(7) 1.3834(7) 0.5093(6) 0.055(2) Uani 1 1 d . . . H15 H 1.3384 1.4580 0.5291 0.066 Uiso 1 1 calc R . . C16 C 1.1972(7) 1.3449(6) 0.4147(5) 0.0398(19) Uani 1 1 d . . . H16 H 1.2416 1.3930 0.3715 0.048 Uiso 1 1 calc R . . C17 C 0.8681(6) 1.0455(6) 0.4243(5) 0.0342(19) Uani 1 1 d . . . C18 C 0.6433(7) 0.8713(7) 0.3960(5) 0.037(2) Uani 1 1 d . . . C19 C 0.4340(8) 0.7604(6) 0.4545(5) 0.0381(19) Uani 1 1 d . . . C21 C 0.3467(7) 0.7651(7) 0.1399(5) 0.0365(19) Uani 1 1 d . . . C22 C 0.3846(7) 0.8862(7) 0.1101(5) 0.0378(19) Uani 1 1 d . . . C23 C 0.2809(6) 0.9073(7) 0.0598(4) 0.0368(19) Uani 1 1 d . . . H23 H 0.3054 0.9893 0.0438 0.044 Uiso 1 1 calc R . . C24 C 0.1461(8) 0.8138(8) 0.0333(5) 0.060(2) Uani 1 1 d . . . H24 H 0.0802 0.8283 -0.0020 0.072 Uiso 1 1 calc R . . C25 C 0.1174(7) 0.6975(9) 0.0633(5) 0.057(2) Uani 1 1 d . . . H25 H 0.0277 0.6310 0.0466 0.069 Uiso 1 1 calc R . . C26 C 0.2106(7) 0.6716(8) 0.1160(5) 0.054(2) Uani 1 1 d . . . H26 H 0.1825 0.5912 0.1358 0.064 Uiso 1 1 calc R . . C27 C 0.5242(7) 0.9860(7) 0.1297(4) 0.0370(19) Uani 1 1 d . . . C28 C 0.7486(7) 1.1760(8) 0.1637(4) 0.0363(19) Uani 1 1 d . . . C29 C 0.8708(7) 1.4131(7) 0.1872(5) 0.041(2) Uani 1 1 d . . . C31 C 1.1474(7) 1.1454(7) 0.1362(5) 0.057(2) Uani 1 1 d . . . H31A H 1.1782 1.0840 0.1526 0.068 Uiso 1 1 calc R . . H31B H 1.1956 1.2202 0.1845 0.068 Uiso 1 1 calc R . . C32 C 1.1787(6) 1.1857(7) 0.0470(5) 0.064(3) Uani 1 1 d . . . H32A H 1.1335 1.1112 -0.0005 0.096 Uiso 1 1 calc R . . H32B H 1.2750 1.2259 0.0525 0.096 Uiso 1 1 calc R . . H32C H 1.1481 1.2463 0.0306 0.096 Uiso 1 1 calc R . . C41 C 0.4917(7) 0.5041(7) 0.1786(5) 0.053(2) Uani 1 1 d . . . H41A H 0.4997 0.4818 0.1169 0.064 Uiso 1 1 calc R . . H41B H 0.4023 0.4952 0.1732 0.064 Uiso 1 1 calc R . . C42 C 0.5078(6) 0.4116(7) 0.2421(5) 0.058(2) Uani 1 1 d . . . H42A H 0.6009 0.4309 0.2563 0.086 Uiso 1 1 calc R . . H42B H 0.4510 0.3239 0.2113 0.086 Uiso 1 1 calc R . . H42C H 0.4817 0.4218 0.2988 0.086 Uiso 1 1 calc R . . C110 C 0.4902(8) 0.7917(7) 0.5510(6) 0.062(2) Uani 1 1 d . . . H110 H 0.5828 0.8233 0.5729 0.074 Uiso 1 1 calc R . . C111 C 0.4102(8) 0.7764(7) 0.6133(6) 0.060(2) Uani 1 1 d . . . H111 H 0.4486 0.8007 0.6768 0.072 Uiso 1 1 calc R . . C112 C 0.2710(9) 0.7240(7) 0.5799(6) 0.055(2) Uani 1 1 d . . . H112 H 0.2158 0.7124 0.6215 0.066 Uiso 1 1 calc R . . C113 C 0.2142(8) 0.6893(7) 0.4857(6) 0.055(2) Uani 1 1 d . . . H113 H 0.1206 0.6512 0.4638 0.066 Uiso 1 1 calc R . . C114 C 0.2970(7) 0.7113(7) 0.4246(5) 0.050(2) Uani 1 1 d . . . H114 H 0.2588 0.6924 0.3610 0.060 Uiso 1 1 calc R . . C210 C 0.7827(7) 1.4324(7) 0.1156(5) 0.045(2) Uani 1 1 d . . . H210 H 0.7214 1.3662 0.0674 0.054 Uiso 1 1 calc R . . C211 C 0.7922(8) 1.5548(8) 0.1211(6) 0.056(2) Uani 1 1 d . . . H211 H 0.7359 1.5702 0.0758 0.067 Uiso 1 1 calc R . . C212 C 0.8831(8) 1.6525(8) 0.1919(6) 0.055(2) Uani 1 1 d . . . H212 H 0.8842 1.7315 0.1958 0.066 Uiso 1 1 calc R . . C213 C 0.9740(7) 1.6347(8) 0.2583(5) 0.056(2) Uani 1 1 d . . . H213 H 1.0406 1.7031 0.3032 0.067 Uiso 1 1 calc R . . C214 C 0.9626(7) 1.5130(8) 0.2556(5) 0.045(2) Uani 1 1 d . . . H214 H 1.0189 1.4989 0.3018 0.054 Uiso 1 1 calc R . . N11 N 0.8247(5) 0.9831(5) 0.3382(4) 0.0316(15) Uani 1 1 d . . . N12 N 0.6938(5) 0.8815(5) 0.3215(4) 0.0368(15) Uani 1 1 d . . . N13 N 0.5124(6) 0.7825(5) 0.3913(4) 0.0317(15) Uani 1 1 d D . . N21 N 0.6267(5) 0.9599(5) 0.1511(4) 0.0369(15) Uani 1 1 d . . . N22 N 0.7540(5) 1.0685(5) 0.1714(3) 0.0312(14) Uani 1 1 d . . . N23 N 0.8592(6) 1.2912(6) 0.1894(4) 0.0426(16) Uani 1 1 d D . . H23N H 0.9336 1.2903 0.2103 0.051 Uiso 1 1 calc RD . . O4 O 0.7882(4) 0.8641(4) 0.1718(3) 0.0346(11) Uani 1 1 d . . . O11 O 1.0389(4) 0.9830(4) 0.2801(3) 0.0383(12) Uani 1 1 d . . . O12 O 1.0145(4) 1.1965(4) 0.2943(3) 0.0378(12) Uani 1 1 d . . . O13 O 1.0041(4) 1.0866(4) 0.1311(3) 0.0344(12) Uani 1 1 d . . . O21 O 0.5490(4) 0.7179(4) 0.0556(3) 0.0403(12) Uani 1 1 d . . . O22 O 0.4388(4) 0.7436(4) 0.1927(3) 0.0376(12) Uani 1 1 d . . . O23 O 0.5915(4) 0.6332(4) 0.2143(3) 0.0393(12) Uani 1 1 d . . . S1 S 0.75540(18) 0.98391(19) 0.49149(13) 0.0436(6) Uani 1 1 d . . . S2 S 0.58374(18) 1.15025(18) 0.13057(13) 0.0416(5) Uani 1 1 d . . . V1 V 0.93268(11) 1.02076(12) 0.22686(8) 0.0361(4) Uani 1 1 d . . . V2 V 0.60885(11) 0.77205(12) 0.16384(9) 0.0392(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C11 0.057(5) 0.022(5) 0.042(6) 0.007(4) -0.006(5) 0.024(4) C12 0.042(5) 0.039(5) 0.035(5) 0.019(4) 0.011(4) 0.030(4) C13 0.034(4) 0.030(5) 0.031(5) 0.017(4) 0.010(4) 0.017(4) C14 0.047(5) 0.019(5) 0.056(6) 0.011(4) 0.006(4) 0.010(4) C15 0.056(5) 0.038(6) 0.053(6) 0.002(5) 0.002(5) 0.013(4) C16 0.050(5) 0.027(5) 0.031(5) 0.004(4) -0.001(4) 0.015(4) C17 0.026(4) 0.020(5) 0.050(6) 0.004(4) -0.003(4) 0.011(4) C18 0.039(5) 0.054(6) 0.031(5) 0.024(4) 0.009(4) 0.031(5) C19 0.044(5) 0.034(5) 0.032(5) 0.011(4) 0.015(4) 0.013(4) C21 0.033(4) 0.043(5) 0.034(5) 0.015(4) 0.012(4) 0.017(4) C22 0.033(4) 0.042(5) 0.039(5) 0.011(4) 0.013(4) 0.017(4) C23 0.028(4) 0.059(6) 0.029(5) 0.011(4) 0.006(4) 0.025(4) C24 0.051(6) 0.083(7) 0.048(6) 0.026(5) 0.011(5) 0.033(5) C25 0.039(5) 0.105(8) 0.033(5) 0.030(5) 0.024(4) 0.033(5) C26 0.036(5) 0.080(7) 0.046(6) 0.025(5) 0.015(4) 0.027(5) C27 0.034(4) 0.051(5) 0.030(5) 0.021(4) 0.011(4) 0.021(4) C28 0.056(5) 0.043(6) 0.019(4) 0.008(4) 0.017(4) 0.028(5) C29 0.058(5) 0.015(5) 0.044(6) 0.005(4) 0.029(4) 0.007(4) C31 0.050(5) 0.075(7) 0.054(6) 0.027(5) 0.024(5) 0.033(5) C32 0.029(4) 0.088(7) 0.059(6) 0.016(5) 0.016(4) 0.013(5) C41 0.044(5) 0.042(6) 0.062(6) 0.009(5) 0.004(4) 0.016(4) C42 0.061(5) 0.046(6) 0.059(6) 0.022(5) 0.005(4) 0.022(4) C110 0.066(6) 0.064(6) 0.041(6) 0.014(5) 0.023(5) 0.015(5) C111 0.066(6) 0.077(7) 0.036(6) 0.014(5) 0.018(5) 0.032(5) C112 0.066(6) 0.044(6) 0.074(7) 0.031(5) 0.039(6) 0.033(5) C113 0.049(5) 0.051(6) 0.063(7) 0.009(5) 0.018(5) 0.022(5) C114 0.046(5) 0.051(6) 0.055(6) 0.017(4) 0.017(5) 0.022(4) C210 0.056(5) 0.046(6) 0.043(5) 0.024(4) 0.013(4) 0.030(4) C211 0.078(6) 0.053(6) 0.049(6) 0.022(5) 0.025(5) 0.038(5) C212 0.061(5) 0.038(6) 0.084(7) 0.028(5) 0.029(5) 0.032(5) C213 0.051(5) 0.044(6) 0.067(6) 0.013(5) 0.015(5) 0.018(5) C214 0.038(5) 0.039(5) 0.059(6) 0.013(5) 0.019(4) 0.016(4) N11 0.034(4) 0.022(4) 0.032(4) 0.007(3) 0.006(3) 0.009(3) N12 0.034(4) 0.039(4) 0.034(4) 0.021(3) 0.001(3) 0.017(3) N13 0.027(4) 0.036(4) 0.018(4) 0.011(3) 0.001(3) 0.005(3) N21 0.043(4) 0.034(4) 0.028(4) 0.009(3) 0.007(3) 0.014(3) N22 0.040(3) 0.018(4) 0.037(4) 0.009(3) 0.005(3) 0.016(3) N23 0.047(4) 0.034(4) 0.053(4) 0.010(3) 0.006(3) 0.027(4) O4 0.054(3) 0.024(3) 0.020(3) 0.007(2) 0.011(2) 0.013(2) O11 0.038(3) 0.040(3) 0.035(3) 0.008(2) 0.007(2) 0.018(2) O12 0.039(3) 0.031(3) 0.034(3) 0.015(2) 0.009(3) 0.009(2) O13 0.032(3) 0.032(3) 0.037(3) 0.015(2) 0.011(2) 0.012(2) O21 0.029(2) 0.052(3) 0.030(3) 0.008(2) 0.000(2) 0.015(2) O22 0.037(3) 0.048(3) 0.025(3) 0.013(2) 0.001(2) 0.020(3) O23 0.037(3) 0.024(3) 0.044(3) 0.009(2) 0.004(2) 0.007(2) S1 0.0533(13) 0.0463(14) 0.0320(13) 0.0111(11) 0.0105(11) 0.0243(11) S2 0.0504(12) 0.0405(14) 0.0410(14) 0.0115(11) 0.0120(10) 0.0268(11) V1 0.0426(8) 0.0328(9) 0.0340(8) 0.0112(7) 0.0068(7) 0.0195(7) V2 0.0411(8) 0.0386(9) 0.0366(9) 0.0120(7) 0.0052(7) 0.0192(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 C11 O12 1.337(7) . ? C11 C16 1.407(8) . ? C11 C12 1.443(8) . ? C12 C13 1.425(8) . ? C12 C17 1.464(9) . ? C13 C14 1.333(8) . ? C13 H13 0.9300 . ? C14 C15 1.370(9) . ? C14 H14 0.9300 . ? C15 C16 1.388(8) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 N11 1.325(7) . ? C17 S1 1.682(7) . ? C18 N12 1.319(7) . ? C18 N13 1.353(8) . ? C18 S1 1.726(7) . ? C19 N13 1.362(8) . ? C19 C114 1.367(8) . ? C19 C110 1.408(9) . ? C21 O22 1.328(7) . ? C21 C26 1.387(8) . ? C21 C22 1.406(8) . ? C22 C23 1.418(8) . ? C22 C27 1.435(8) . ? C23 C24 1.376(8) . ? C23 H23 0.9300 . ? C24 C25 1.371(9) . ? C24 H24 0.9300 . ? C25 C26 1.370(8) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 N21 1.343(7) . ? C27 S2 1.729(7) . ? C28 N22 1.313(7) . ? C28 N23 1.326(8) . ? C28 S2 1.740(7) . ? C29 C214 1.365(9) . ? C29 N23 1.389(7) . ? C29 C210 1.431(9) . ? C31 O13 1.438(7) . ? C31 C32 1.470(8) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C41 O23 1.408(7) . ? C41 C42 1.529(8) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C110 C111 1.374(8) . ? C110 H110 0.9300 . ? C111 C112 1.390(9) . ? C111 H111 0.9300 . ? C112 C113 1.378(9) . ? C112 H112 0.9300 . ? C113 C114 1.375(8) . ? C113 H113 0.9300 . ? C114 H114 0.9300 . ? C210 C211 1.400(9) . ? C210 H210 0.9300 . ? C211 C212 1.371(9) . ? C211 H211 0.9300 . ? C212 C213 1.397(9) . ? C212 H212 0.9300 . ? C213 C214 1.383(9) . ? C213 H213 0.9300 . ? C214 H214 0.9300 . ? N11 N12 1.377(6) . ? N11 V1 2.174(5) . ? N12 V2 2.405(6) . ? N13 H13N 0.864(19) . ? N21 N22 1.382(6) . ? N21 V2 2.157(5) . ? N22 V1 2.395(5) . ? N23 H23N 0.8600 . ? O4 V2 1.794(4) . ? O4 V1 1.823(4) . ? O11 V1 1.583(4) . ? O12 V1 1.960(4) . ? O13 V1 1.787(4) . ? O21 V2 1.594(4) . ? O22 V2 1.951(4) . ? O23 V2 1.775(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O12 C11 C16 118.2(7) . . ? O12 C11 C12 122.1(6) . . ? C16 C11 C12 119.7(7) . . ? C13 C12 C11 117.3(6) . . ? C13 C12 C17 122.7(6) . . ? C11 C12 C17 119.9(6) . . ? C14 C13 C12 121.5(7) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C13 C14 C15 121.0(7) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C14 C15 C16 122.1(7) . . ? C14 C15 H15 118.9 . . ? C16 C15 H15 118.9 . . ? C15 C16 C11 118.4(7) . . ? C15 C16 H16 120.8 . . ? C11 C16 H16 120.8 . . ? N11 C17 C12 120.3(6) . . ? N11 C17 S1 114.4(5) . . ? C12 C17 S1 125.3(6) . . ? N12 C18 N13 119.9(7) . . ? N12 C18 S1 113.9(5) . . ? N13 C18 S1 126.2(6) . . ? N13 C19 C114 119.8(7) . . ? N13 C19 C110 122.0(7) . . ? C114 C19 C110 118.1(7) . . ? O22 C21 C26 121.4(7) . . ? O22 C21 C22 120.4(6) . . ? C26 C21 C22 118.1(7) . . ? C21 C22 C23 118.2(6) . . ? C21 C22 C27 121.1(6) . . ? C23 C22 C27 120.7(7) . . ? C24 C23 C22 124.0(7) . . ? C24 C23 H23 118.0 . . ? C22 C23 H23 118.0 . . ? C25 C24 C23 114.4(7) . . ? C25 C24 H24 122.8 . . ? C23 C24 H24 122.8 . . ? C26 C25 C24 125.0(8) . . ? C26 C25 H25 117.5 . . ? C24 C25 H25 117.5 . . ? C25 C26 C21 120.2(7) . . ? C25 C26 H26 119.9 . . ? C21 C26 H26 119.9 . . ? N21 C27 C22 122.1(6) . . ? N21 C27 S2 111.4(5) . . ? C22 C27 S2 126.5(5) . . ? N22 C28 N23 121.4(6) . . ? N22 C28 S2 113.2(6) . . ? N23 C28 S2 125.0(6) . . ? C214 C29 N23 119.8(7) . . ? C214 C29 C210 120.1(7) . . ? N23 C29 C210 120.0(7) . . ? O13 C31 C32 111.2(6) . . ? O13 C31 H31A 109.4 . . ? C32 C31 H31A 109.4 . . ? O13 C31 H31B 109.4 . . ? C32 C31 H31B 109.4 . . ? H31A C31 H31B 108.0 . . ? 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 . . ? O23 C41 C42 110.6(6) . . ? O23 C41 H41A 109.5 . . ? C42 C41 H41A 109.5 . . ? O23 C41 H41B 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 108.1 . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C111 C110 C19 121.0(7) . . ? C111 C110 H110 119.5 . . ? C19 C110 H110 119.5 . . ? C110 C111 C112 119.0(7) . . ? C110 C111 H111 120.5 . . ? C112 C111 H111 120.5 . . ? C113 C112 C111 120.5(7) . . ? C113 C112 H112 119.7 . . ? C111 C112 H112 119.7 . . ? C114 C113 C112 119.4(7) . . ? C114 C113 H113 120.3 . . ? C112 C113 H113 120.3 . . ? C19 C114 C113 121.9(7) . . ? C19 C114 H114 119.1 . . ? C113 C114 H114 119.1 . . ? C211 C210 C29 117.4(7) . . ? C211 C210 H210 121.3 . . ? C29 C210 H210 121.3 . . ? C212 C211 C210 121.2(8) . . ? C212 C211 H211 119.4 . . ? C210 C211 H211 119.4 . . ? C211 C212 C213 120.8(7) . . ? C211 C212 H212 119.6 . . ? C213 C212 H212 119.6 . . ? C214 C213 C212 118.4(8) . . ? C214 C213 H213 120.8 . . ? C212 C213 H213 120.8 . . ? C29 C214 C213 121.8(7) . . ? C29 C214 H214 119.1 . . ? C213 C214 H214 119.1 . . ? C17 N11 N12 112.6(6) . . ? C17 N11 V1 128.5(5) . . ? N12 N11 V1 118.9(4) . . ? C18 N12 N11 111.3(6) . . ? C18 N12 V2 135.4(5) . . ? N11 N12 V2 113.3(4) . . ? C18 N13 C19 131.2(7) . . ? C18 N13 H13N 108(4) . . ? C19 N13 H13N 116(4) . . ? C27 N21 N22 114.0(5) . . ? C27 N21 V2 126.6(4) . . ? N22 N21 V2 119.3(4) . . ? C28 N22 N21 112.4(5) . . ? C28 N22 V1 134.2(5) . . ? N21 N22 V1 113.0(4) . . ? C28 N23 C29 128.6(6) . . ? C28 N23 H23N 115.7 . . ? C29 N23 H23N 115.7 . . ? V2 O4 V1 139.4(2) . . ? C11 O12 V1 125.1(4) . . ? C31 O13 V1 122.0(4) . . ? C21 O22 V2 125.5(4) . . ? C41 O23 V2 125.8(4) . . ? C17 S1 C18 87.8(4) . . ? C27 S2 C28 88.9(3) . . ? O11 V1 O13 102.16(19) . . ? O11 V1 O4 103.0(2) . . ? O13 V1 O4 102.67(18) . . ? O11 V1 O12 97.6(2) . . ? O13 V1 O12 89.77(18) . . ? O4 V1 O12 152.92(17) . . ? O11 V1 N11 92.76(19) . . ? O13 V1 N11 162.65(19) . . ? O4 V1 N11 82.2(2) . . ? O12 V1 N11 79.40(19) . . ? O11 V1 N22 169.25(19) . . ? O13 V1 N22 88.47(18) . . ? O4 V1 N22 75.84(18) . . ? O12 V1 N22 80.63(18) . . ? N11 V1 N22 76.49(18) . . ? O21 V2 O23 103.4(2) . . ? O21 V2 O4 102.8(2) . . ? O23 V2 O4 102.86(18) . . ? O21 V2 O22 96.49(19) . . ? O23 V2 O22 89.55(18) . . ? O4 V2 O22 153.80(18) . . ? O21 V2 N21 95.0(2) . . ? O23 V2 N21 159.8(2) . . ? O4 V2 N21 80.91(19) . . ? O22 V2 N21 79.89(19) . . ? O21 V2 N12 171.1(2) . . ? O23 V2 N12 85.05(19) . . ? O4 V2 N12 77.66(19) . . ? O22 V2 N12 80.59(18) . . ? N21 V2 N12 76.31(18) . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.481 _refine_diff_density_min -0.321 _refine_diff_density_rms 0.074 #===END data_3b_x_0.5_EtOH _database_code_depnum_ccdc_archive 'CCDC 733238' _audit_creation_method SHELXL-97 _chemical_name_systematic ;\ diethoxo-\m-oxo-dioxobis[2-(5-phenylamino-[1,3,4]thiadiazol-2-yl)-phenolato]\ divanadium(V) ethanol hemisolvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H30 N6 O7 S2 V2, 0.5(C2 H6 O)' _chemical_formula_sum 'C33 H33 N6 O7.50 S2 V2' _chemical_formula_weight 799.65 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_Int_Tables_number 2 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6448(4) _cell_length_b 12.1611(4) _cell_length_c 14.4691(5) _cell_angle_alpha 73.441(3) _cell_angle_beta 84.791(3) _cell_angle_gamma 62.827(3) _cell_volume 1745.41(12) _cell_formula_units_Z 2 _cell_measurement_temperature 120(1) _cell_measurement_reflns_used 8271 _cell_measurement_theta_min 3.7802 _cell_measurement_theta_max 28.3658 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.55 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.522 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 822 _exptl_absorpt_coefficient_mu 0.713 _exptl_absorpt_correction_T_min 0.775 _exptl_absorpt_correction_T_max 0.945 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(1) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur CCD' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.3426 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15723 _diffrn_reflns_av_R_equivalents 0.0251 _diffrn_reflns_av_sigmaI/netI 0.0418 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.79 _diffrn_reflns_theta_max 28.43 _reflns_number_total 7536 _reflns_number_gt 5391 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.15 (release 10-01-2008 CrysAlis171 .NET) (compiled Jan 10 2008,16:37:18) ; _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0548P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7536 _refine_ls_number_parameters 489 _refine_ls_number_restraints 100 _refine_ls_R_factor_all 0.0525 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0913 _refine_ls_wR_factor_gt 0.0878 _refine_ls_goodness_of_fit_ref 0.960 _refine_ls_restrained_S_all 0.954 _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 C11 C 0.65492(18) 0.64353(19) 0.12851(15) 0.0316(5) Uani 1 1 d . . . C12 C 0.63664(18) 0.5930(2) 0.05739(15) 0.0322(5) Uani 1 1 d . . . C13 C 0.6124(2) 0.6675(2) -0.03965(16) 0.0396(5) Uani 1 1 d . . . H13 H 0.6020 0.6332 -0.0879 0.048 Uiso 1 1 calc R . . C14 C 0.6036(2) 0.7887(2) -0.06546(18) 0.0484(6) Uani 1 1 d . . . H14 H 0.5835 0.8394 -0.1307 0.058 Uiso 1 1 calc R . . C15 C 0.6241(2) 0.8370(2) 0.00385(18) 0.0465(6) Uani 1 1 d . . . H15 H 0.6206 0.9200 -0.0146 0.056 Uiso 1 1 calc R . . C16 C 0.6495(2) 0.7661(2) 0.09933(17) 0.0380(5) Uani 1 1 d . . . H16 H 0.6634 0.8008 0.1459 0.046 Uiso 1 1 calc R . . C17 C 0.64976(18) 0.4638(2) 0.08554(15) 0.0301(5) Uani 1 1 d . . . C18 C 0.69318(19) 0.2447(2) 0.10574(15) 0.0309(5) Uani 1 1 d . . . C21 C 0.8984(2) -0.06505(19) 0.34825(14) 0.0317(5) Uani 1 1 d . . . C22 C 0.98614(19) -0.02810(19) 0.37621(14) 0.0305(4) Uani 1 1 d . . . C23 C 1.10976(19) -0.1220(2) 0.41341(14) 0.0315(5) Uani 1 1 d . . . H23 H 1.1692 -0.0965 0.4300 0.038 Uiso 1 1 calc R . . C24 C 1.1473(2) -0.2505(2) 0.42658(16) 0.0391(5) Uani 1 1 d . . . H24 H 1.2315 -0.3133 0.4523 0.047 Uiso 1 1 calc R . . C25 C 1.0599(2) -0.2872(2) 0.40164(17) 0.0431(6) Uani 1 1 d . . . H25 H 1.0846 -0.3758 0.4114 0.052 Uiso 1 1 calc R . . C26 C 0.9373(2) -0.1963(2) 0.36278(16) 0.0387(5) Uani 1 1 d . . . H26 H 0.8793 -0.2234 0.3459 0.046 Uiso 1 1 calc R . . C27 C 0.94654(19) 0.10720(19) 0.36252(14) 0.0281(4) Uani 1 1 d . . . C28 C 0.91939(19) 0.3221(2) 0.33763(15) 0.0303(4) Uani 1 1 d . . . C29 C 1.02731(19) 0.4624(2) 0.29722(16) 0.0332(5) Uani 1 1 d . . . C31 C 0.5554(2) 0.6282(2) 0.43459(19) 0.0480(6) Uani 1 1 d D . . H31A H 0.5234 0.6095 0.5001 0.058 Uiso 1 1 calc R . . H31B H 0.4802 0.6905 0.3897 0.058 Uiso 1 1 calc R . . C32 C 0.6451(3) 0.6849(3) 0.4346(2) 0.0654(8) Uani 1 1 d D . . H32A H 0.7219 0.6213 0.4761 0.098 Uiso 1 1 calc R . . H32B H 0.6014 0.7608 0.4591 0.098 Uiso 1 1 calc R . . H32C H 0.6710 0.7100 0.3687 0.098 Uiso 1 1 calc R . . C19 C 0.7753(2) 0.0701(2) 0.02617(15) 0.0343(5) Uani 1 1 d . . . C110 C 0.7223(2) 0.1393(2) -0.06753(17) 0.0443(6) Uani 1 1 d . . . H110 H 0.6519 0.2230 -0.0793 0.053 Uiso 1 1 calc R . . C111 C 0.7729(3) 0.0851(3) -0.14295(18) 0.0543(7) Uani 1 1 d . . . H111 H 0.7386 0.1325 -0.2070 0.065 Uiso 1 1 calc R . . C112 C 0.8735(3) -0.0379(3) -0.1252(2) 0.0576(7) Uani 1 1 d . . . H112 H 0.9089 -0.0746 -0.1772 0.069 Uiso 1 1 calc R . . C113 C 0.9226(2) -0.1073(2) -0.03247(19) 0.0502(6) Uani 1 1 d . . . H113 H 0.9900 -0.1927 -0.0204 0.060 Uiso 1 1 calc R . . C114 C 0.8740(2) -0.0529(2) 0.04352(18) 0.0406(5) Uani 1 1 d . . . H114 H 0.9088 -0.1006 0.1074 0.049 Uiso 1 1 calc R . . C210 C 1.1501(2) 0.3808(2) 0.34015(18) 0.0431(6) Uani 1 1 d . . . H210 H 1.1648 0.3052 0.3905 0.052 Uiso 1 1 calc R . . C211 C 1.2507(2) 0.4110(2) 0.3088(2) 0.0483(6) Uani 1 1 d . . . H211 H 1.3353 0.3544 0.3368 0.058 Uiso 1 1 calc R . . C212 C 1.2301(2) 0.5212(2) 0.23786(19) 0.0462(6) Uani 1 1 d . . . H212 H 1.3003 0.5400 0.2161 0.055 Uiso 1 1 calc R . . C213 C 1.1075(2) 0.6046(2) 0.19821(17) 0.0431(6) Uani 1 1 d . . . H213 H 1.0925 0.6826 0.1507 0.052 Uiso 1 1 calc R . . C214 C 1.0063(2) 0.5754(2) 0.22708(16) 0.0373(5) Uani 1 1 d . . . H214 H 0.9220 0.6329 0.1989 0.045 Uiso 1 1 calc R . . N11 N 0.63628(15) 0.40468(15) 0.17291(12) 0.0279(4) Uani 1 1 d . . . N12 N 0.65929(15) 0.27954(15) 0.18590(12) 0.0283(4) Uani 1 1 d . . . N13 N 0.72933(17) 0.12285(18) 0.10493(14) 0.0345(4) Uani 1 1 d D . . N21 N 0.82637(15) 0.19519(15) 0.34849(11) 0.0264(4) Uani 1 1 d . . . N22 N 0.80952(15) 0.31781(15) 0.33392(11) 0.0278(4) Uani 1 1 d . . . N23 N 0.92081(17) 0.43596(18) 0.32330(14) 0.0376(4) Uani 1 1 d D . . O4 O 0.57324(12) 0.33473(13) 0.34948(10) 0.0293(3) Uani 1 1 d . . . O11 O 0.45420(13) 0.58818(14) 0.26238(11) 0.0388(4) Uani 1 1 d . . . O12 O 0.68355(13) 0.57529(13) 0.22092(10) 0.0313(3) Uani 1 1 d . . . O13 O 0.62105(14) 0.51210(13) 0.40544(10) 0.0352(3) Uani 1 1 d D . . O21 O 0.66990(14) 0.09474(14) 0.46144(10) 0.0377(3) Uani 1 1 d . . . O22 O 0.78187(13) 0.02074(13) 0.30635(10) 0.0330(3) Uani 1 1 d . . . O23 O 0.52560(13) 0.14675(14) 0.30896(11) 0.0365(3) Uani 1 1 d D . . C41A C 0.4762(4) 0.0578(4) 0.3686(3) 0.0455(9) Uani 0.747(6) 1 d PDU A 1 H41A H 0.4130 0.1008 0.4129 0.055 Uiso 0.747(6) 1 calc PR A 1 H41B H 0.5489 -0.0189 0.4085 0.055 Uiso 0.747(6) 1 calc PR A 1 C42A C 0.4131(5) 0.0155(5) 0.3100(3) 0.0534(11) Uani 0.747(6) 1 d PDU A 1 H42A H 0.3365 0.0902 0.2745 0.080 Uiso 0.747(6) 1 calc PR A 1 H42B H 0.3873 -0.0471 0.3528 0.080 Uiso 0.747(6) 1 calc PR A 1 H42C H 0.4740 -0.0242 0.2641 0.080 Uiso 0.747(6) 1 calc PR A 1 C41B C 0.5264(12) 0.0245(11) 0.3299(10) 0.0455(9) Uani 0.253(6) 1 d PU A 2 H41C H 0.5661 -0.0176 0.2780 0.055 Uiso 0.253(6) 1 calc PR A 2 H41D H 0.5741 -0.0328 0.3919 0.055 Uiso 0.253(6) 1 calc PR A 2 C42B C 0.3929(17) 0.0552(15) 0.3352(12) 0.0534(11) Uani 0.253(6) 1 d PU A 2 H42D H 0.3563 0.0954 0.3877 0.080 Uiso 0.253(6) 1 calc PR A 2 H42E H 0.3832 -0.0236 0.3476 0.080 Uiso 0.253(6) 1 calc PR A 2 H42F H 0.3473 0.1149 0.2740 0.080 Uiso 0.253(6) 1 calc PR A 2 S1 S 0.69285(5) 0.36703(5) 0.00716(4) 0.03494(13) Uani 1 1 d . . . S2 S 1.05281(5) 0.17173(5) 0.36077(4) 0.03311(13) Uani 1 1 d . . . V1 V 0.59549(3) 0.47847(3) 0.29995(3) 0.02871(10) Uani 1 1 d . . . V2 V 0.65316(3) 0.16815(3) 0.34888(2) 0.02886(10) Uani 1 1 d . A . H23N H 0.8479(17) 0.497(2) 0.3016(17) 0.049(7) Uiso 1 1 d D . . H13N H 0.744(2) 0.072(2) 0.1608(13) 0.041(7) Uiso 1 1 d D . . C52 C 0.9858(12) 0.5438(14) -0.0164(9) 0.072(4) Uani 0.50 1 d PU B -1 H52A H 0.9322 0.6091 0.0167 0.109 Uiso 0.50 1 calc PR B -1 H52B H 0.9322 0.5432 -0.0645 0.109 Uiso 0.50 1 calc PR B -1 H52C H 1.0545 0.5638 -0.0486 0.109 Uiso 0.50 1 calc PR B -1 C51 C 1.0441(11) 0.4159(15) 0.0549(8) 0.068(3) Uani 0.50 1 d PU B -1 H51A H 1.0994 0.3511 0.0207 0.082 Uiso 0.50 1 calc PR B -1 H51B H 1.1006 0.4168 0.1015 0.082 Uiso 0.50 1 calc PR B -1 O5 O 0.9536(4) 0.3771(4) 0.1067(3) 0.0687(11) Uani 0.50 1 d PU B -1 H5 H 0.9104 0.4279 0.1399 0.103 Uiso 0.50 1 calc PR B -1 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 C11 0.0242(10) 0.0289(11) 0.0361(12) -0.0047(9) -0.0003(8) -0.0093(9) C12 0.0254(10) 0.0327(12) 0.0338(12) -0.0054(9) -0.0003(8) -0.0112(9) C13 0.0393(12) 0.0394(13) 0.0309(12) -0.0021(10) -0.0035(9) -0.0136(11) C14 0.0492(14) 0.0451(15) 0.0364(14) 0.0060(11) -0.0030(10) -0.0183(12) C15 0.0451(13) 0.0309(12) 0.0537(16) 0.0022(11) 0.0001(11) -0.0166(11) C16 0.0345(11) 0.0299(12) 0.0459(14) -0.0052(10) -0.0018(9) -0.0139(10) C17 0.0238(9) 0.0334(11) 0.0311(12) -0.0082(9) -0.0026(8) -0.0109(9) C18 0.0274(10) 0.0340(11) 0.0303(12) -0.0105(9) -0.0027(8) -0.0113(9) C21 0.0369(11) 0.0285(11) 0.0267(11) -0.0092(9) -0.0034(8) -0.0105(10) C22 0.0365(11) 0.0283(11) 0.0250(11) -0.0082(8) -0.0017(8) -0.0123(9) C23 0.0322(11) 0.0334(12) 0.0255(11) -0.0102(9) -0.0022(8) -0.0101(10) C24 0.0415(12) 0.0309(12) 0.0345(13) -0.0105(10) -0.0064(9) -0.0053(10) C25 0.0518(14) 0.0250(11) 0.0442(14) -0.0112(10) -0.0087(11) -0.0076(11) C26 0.0449(13) 0.0301(12) 0.0418(14) -0.0140(10) -0.0063(10) -0.0137(11) C27 0.0323(10) 0.0302(11) 0.0219(10) -0.0088(8) -0.0015(8) -0.0126(9) C28 0.0312(11) 0.0304(11) 0.0301(11) -0.0105(9) 0.0000(8) -0.0130(9) C29 0.0304(11) 0.0309(11) 0.0424(13) -0.0133(10) -0.0011(9) -0.0150(10) C31 0.0589(15) 0.0410(14) 0.0574(16) -0.0314(12) 0.0154(12) -0.0256(13) C32 0.081(2) 0.0542(17) 0.084(2) -0.0372(16) 0.0067(16) -0.0394(17) C19 0.0378(11) 0.0350(12) 0.0352(13) -0.0182(10) 0.0014(9) -0.0157(10) C110 0.0539(14) 0.0387(13) 0.0369(14) -0.0160(11) -0.0041(10) -0.0136(12) C111 0.0770(18) 0.0505(16) 0.0347(14) -0.0177(12) 0.0023(12) -0.0247(15) C112 0.0774(19) 0.0591(18) 0.0462(17) -0.0326(14) 0.0200(13) -0.0315(16) C113 0.0514(15) 0.0427(14) 0.0598(18) -0.0278(13) 0.0086(12) -0.0169(13) C114 0.0451(13) 0.0349(12) 0.0434(14) -0.0157(10) -0.0021(10) -0.0159(11) C210 0.0358(12) 0.0338(12) 0.0610(16) -0.0116(11) -0.0067(10) -0.0160(11) C211 0.0295(12) 0.0450(15) 0.0737(19) -0.0240(13) -0.0023(11) -0.0142(11) C212 0.0402(13) 0.0523(15) 0.0581(16) -0.0243(13) 0.0116(11) -0.0272(12) C213 0.0457(13) 0.0440(14) 0.0467(15) -0.0139(11) 0.0054(10) -0.0260(12) C214 0.0334(11) 0.0371(12) 0.0439(14) -0.0147(10) 0.0000(9) -0.0155(10) N11 0.0278(8) 0.0256(9) 0.0301(10) -0.0065(7) -0.0025(7) -0.0120(8) N12 0.0292(9) 0.0266(9) 0.0299(10) -0.0098(7) -0.0021(7) -0.0116(8) N13 0.0409(10) 0.0321(10) 0.0295(11) -0.0122(8) -0.0025(8) -0.0126(9) N21 0.0316(9) 0.0234(8) 0.0241(9) -0.0078(7) -0.0029(7) -0.0109(8) N22 0.0297(9) 0.0260(9) 0.0298(10) -0.0089(7) -0.0006(7) -0.0134(8) N23 0.0266(9) 0.0292(10) 0.0583(13) -0.0129(9) -0.0007(8) -0.0127(9) O4 0.0311(7) 0.0288(7) 0.0326(8) -0.0124(6) 0.0045(6) -0.0156(6) O11 0.0316(8) 0.0302(8) 0.0549(10) -0.0155(7) 0.0044(6) -0.0125(7) O12 0.0334(7) 0.0272(7) 0.0332(8) -0.0053(6) -0.0025(6) -0.0145(6) O13 0.0479(9) 0.0307(8) 0.0355(9) -0.0156(7) 0.0072(6) -0.0219(7) O21 0.0490(9) 0.0352(8) 0.0335(9) -0.0071(7) -0.0004(6) -0.0237(8) O22 0.0362(8) 0.0271(7) 0.0334(8) -0.0099(6) -0.0068(6) -0.0100(7) O23 0.0383(8) 0.0307(8) 0.0447(9) -0.0114(7) -0.0041(6) -0.0174(7) C41A 0.056(2) 0.047(2) 0.049(3) -0.0112(16) 0.0005(16) -0.036(2) C42A 0.076(3) 0.055(3) 0.046(3) -0.0079(17) 0.0000(19) -0.047(3) C41B 0.056(2) 0.047(2) 0.049(3) -0.0112(16) 0.0005(16) -0.036(2) C42B 0.076(3) 0.055(3) 0.046(3) -0.0079(17) 0.0000(19) -0.047(3) S1 0.0380(3) 0.0380(3) 0.0288(3) -0.0107(2) 0.0019(2) -0.0163(3) S2 0.0286(3) 0.0297(3) 0.0404(3) -0.0118(2) -0.0021(2) -0.0108(2) V1 0.03023(18) 0.02561(19) 0.0322(2) -0.01070(15) 0.00222(14) -0.01277(16) V2 0.03312(19) 0.02686(19) 0.0296(2) -0.00931(15) -0.00049(14) -0.01480(16) C52 0.064(9) 0.082(11) 0.080(8) -0.049(8) 0.003(6) -0.025(12) C51 0.041(5) 0.077(9) 0.097(9) -0.060(8) 0.001(5) -0.014(5) O5 0.049(2) 0.073(3) 0.089(3) -0.051(2) 0.0034(19) -0.016(2) _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 C11 O12 1.336(2) . ? C11 C16 1.402(3) . ? C11 C12 1.415(3) . ? C12 C13 1.409(3) . ? C12 C17 1.445(3) . ? C13 C14 1.371(3) . ? C13 H13 0.9500 . ? C14 C15 1.384(4) . ? C14 H14 0.9500 . ? C15 C16 1.379(3) . ? C15 H15 0.9500 . ? C16 H16 0.9500 . ? C17 N11 1.299(3) . ? C17 S1 1.743(2) . ? C18 N12 1.313(3) . ? C18 N13 1.346(3) . ? C18 S1 1.742(2) . ? C21 O22 1.339(2) . ? C21 C26 1.402(3) . ? C21 C22 1.417(3) . ? C22 C23 1.398(3) . ? C22 C27 1.448(3) . ? C23 C24 1.375(3) . ? C23 H23 0.9500 . ? C24 C25 1.391(3) . ? C24 H24 0.9500 . ? C25 C26 1.388(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 N21 1.306(2) . ? C27 S2 1.737(2) . ? C28 N22 1.311(2) . ? C28 N23 1.348(3) . ? C28 S2 1.738(2) . ? C29 C214 1.386(3) . ? C29 C210 1.389(3) . ? C29 N23 1.412(3) . ? C31 O13 1.432(2) . ? C31 C32 1.492(3) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C19 C114 1.375(3) . ? C19 C110 1.398(3) . ? C19 N13 1.410(3) . ? C110 C111 1.382(3) . ? C110 H110 0.9500 . ? C111 C112 1.383(4) . ? C111 H111 0.9500 . ? C112 C113 1.376(4) . ? C112 H112 0.9500 . ? C113 C114 1.388(3) . ? C113 H113 0.9500 . ? C114 H114 0.9500 . ? C210 C211 1.383(3) . ? C210 H210 0.9500 . ? C211 C212 1.369(4) . ? C211 H211 0.9500 . ? C212 C213 1.375(3) . ? C212 H212 0.9500 . ? C213 C214 1.376(3) . ? C213 H213 0.9500 . ? C214 H214 0.9500 . ? N11 N12 1.377(2) . ? N11 V1 2.1913(16) . ? N12 V2 2.3745(17) . ? N13 H13N 0.843(16) . ? N21 N22 1.367(2) . ? N21 V2 2.1861(16) . ? N22 V1 2.3448(16) . ? N23 H23N 0.843(16) . ? O4 V2 1.8046(13) . ? O4 V1 1.8172(14) . ? O11 V1 1.5895(14) . ? O12 V1 1.9667(14) . ? O13 V1 1.7706(14) . ? O21 V2 1.5991(15) . ? O22 V2 1.9611(14) . ? O23 C41B 1.426(11) . ? O23 C41A 1.481(4) . ? O23 V2 1.7895(14) . ? C41A C42A 1.494(6) . ? C41A H41A 0.9900 . ? C41A H41B 0.9900 . ? C42A H42A 0.9800 . ? C42A H42B 0.9800 . ? C42A H42C 0.9800 . ? C41B C42B 1.42(2) . ? C41B H41C 0.9900 . ? C41B H41D 0.9900 . ? C42B H42D 0.9800 . ? C42B H42E 0.9800 . ? C42B H42F 0.9800 . ? C52 C51 1.481(11) . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C51 O5 1.417(14) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? O5 H5 0.8400 . ? 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 O12 C11 C16 119.60(19) . . ? O12 C11 C12 121.87(18) . . ? C16 C11 C12 118.4(2) . . ? C13 C12 C11 119.2(2) . . ? C13 C12 C17 121.7(2) . . ? C11 C12 C17 119.03(18) . . ? C14 C13 C12 120.9(2) . . ? C14 C13 H13 119.5 . . ? C12 C13 H13 119.5 . . ? C13 C14 C15 119.8(2) . . ? C13 C14 H14 120.1 . . ? C15 C14 H14 120.1 . . ? C16 C15 C14 120.8(2) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C11 120.8(2) . . ? C15 C16 H16 119.6 . . ? C11 C16 H16 119.6 . . ? N11 C17 C12 123.82(19) . . ? N11 C17 S1 112.46(16) . . ? C12 C17 S1 123.65(16) . . ? N12 C18 N13 120.82(19) . . ? N12 C18 S1 113.73(16) . . ? N13 C18 S1 125.39(16) . . ? O22 C21 C26 119.18(18) . . ? O22 C21 C22 122.46(18) . . ? C26 C21 C22 118.33(19) . . ? C23 C22 C21 119.56(19) . . ? C23 C22 C27 121.55(18) . . ? C21 C22 C27 118.86(18) . . ? C24 C23 C22 121.5(2) . . ? C24 C23 H23 119.2 . . ? C22 C23 H23 119.2 . . ? C23 C24 C25 118.9(2) . . ? C23 C24 H24 120.5 . . ? C25 C24 H24 120.5 . . ? C26 C25 C24 121.1(2) . . ? C26 C25 H25 119.5 . . ? C24 C25 H25 119.5 . . ? C25 C26 C21 120.5(2) . . ? C25 C26 H26 119.7 . . ? C21 C26 H26 119.7 . . ? N21 C27 C22 123.65(18) . . ? N21 C27 S2 112.18(15) . . ? C22 C27 S2 124.17(15) . . ? N22 C28 N23 120.09(18) . . ? N22 C28 S2 113.32(15) . . ? N23 C28 S2 126.58(16) . . ? C214 C29 C210 119.6(2) . . ? C214 C29 N23 117.97(18) . . ? C210 C29 N23 122.4(2) . . ? O13 C31 C32 110.0(2) . . ? O13 C31 H31A 109.7 . . ? C32 C31 H31A 109.7 . . ? O13 C31 H31B 109.7 . . ? C32 C31 H31B 109.7 . . ? H31A C31 H31B 108.2 . . ? 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 . . ? C114 C19 C110 120.0(2) . . ? C114 C19 N13 118.3(2) . . ? C110 C19 N13 121.7(2) . . ? C111 C110 C19 119.6(2) . . ? C111 C110 H110 120.2 . . ? C19 C110 H110 120.2 . . ? C110 C111 C112 120.0(2) . . ? C110 C111 H111 120.0 . . ? C112 C111 H111 120.0 . . ? C113 C112 C111 120.2(2) . . ? C113 C112 H112 119.9 . . ? C111 C112 H112 119.9 . . ? C112 C113 C114 120.2(2) . . ? C112 C113 H113 119.9 . . ? C114 C113 H113 119.9 . . ? C19 C114 C113 119.9(2) . . ? C19 C114 H114 120.1 . . ? C113 C114 H114 120.1 . . ? C211 C210 C29 119.2(2) . . ? C211 C210 H210 120.4 . . ? C29 C210 H210 120.4 . . ? C212 C211 C210 120.9(2) . . ? C212 C211 H211 119.5 . . ? C210 C211 H211 119.5 . . ? C211 C212 C213 119.8(2) . . ? C211 C212 H212 120.1 . . ? C213 C212 H212 120.1 . . ? C212 C213 C214 120.3(2) . . ? C212 C213 H213 119.9 . . ? C214 C213 H213 119.9 . . ? C213 C214 C29 120.1(2) . . ? C213 C214 H214 119.9 . . ? C29 C214 H214 119.9 . . ? C17 N11 N12 114.83(16) . . ? C17 N11 V1 126.94(14) . . ? N12 N11 V1 118.07(12) . . ? C18 N12 N11 111.59(17) . . ? C18 N12 V2 133.95(14) . . ? N11 N12 V2 114.00(11) . . ? C18 N13 C19 127.0(2) . . ? C18 N13 H13N 113.0(16) . . ? C19 N13 H13N 117.8(16) . . ? C27 N21 N22 114.65(16) . . ? C27 N21 V2 127.84(13) . . ? N22 N21 V2 117.49(11) . . ? C28 N22 N21 112.19(16) . . ? C28 N22 V1 132.54(13) . . ? N21 N22 V1 115.19(11) . . ? C28 N23 C29 126.76(18) . . ? C28 N23 H23N 110.5(17) . . ? C29 N23 H23N 115.5(17) . . ? V2 O4 V1 138.13(8) . . ? C11 O12 V1 126.56(12) . . ? C31 O13 V1 129.48(15) . . ? C21 O22 V2 127.15(12) . . ? C41B O23 V2 122.9(5) . . ? C41A O23 V2 123.62(17) . . ? O23 C41A C42A 113.0(3) . . ? O23 C41A H41A 109.0 . . ? C42A C41A H41A 109.0 . . ? O23 C41A H41B 109.0 . . ? C42A C41A H41B 109.0 . . ? H41A C41A H41B 107.8 . . ? C42B C41B O23 103.3(11) . . ? C42B C41B H41C 111.1 . . ? O23 C41B H41C 111.1 . . ? C42B C41B H41D 111.1 . . ? O23 C41B H41D 111.1 . . ? H41C C41B H41D 109.1 . . ? C41B C42B H42D 109.5 . . ? C41B C42B H42E 109.5 . . ? H42D C42B H42E 109.5 . . ? C41B C42B H42F 109.5 . . ? H42D C42B H42F 109.5 . . ? H42E C42B H42F 109.5 . . ? C18 S1 C17 87.34(10) . . ? C27 S2 C28 87.64(10) . . ? O11 V1 O13 102.84(7) . . ? O11 V1 O4 103.84(7) . . ? O13 V1 O4 102.16(6) . . ? O11 V1 O12 94.62(7) . . ? O13 V1 O12 91.92(6) . . ? O4 V1 O12 153.47(6) . . ? O11 V1 N11 95.35(7) . . ? O13 V1 N11 160.30(6) . . ? O4 V1 N11 80.43(6) . . ? O12 V1 N11 79.00(6) . . ? O11 V1 N22 172.45(7) . . ? O13 V1 N22 83.65(6) . . ? O4 V1 N22 78.22(6) . . ? O12 V1 N22 81.18(6) . . ? N11 V1 N22 77.74(6) . . ? O21 V2 O23 102.50(7) . . ? O21 V2 O4 102.31(7) . . ? O23 V2 O4 102.52(6) . . ? O21 V2 O22 96.32(7) . . ? O23 V2 O22 90.35(6) . . ? O4 V2 O22 154.33(6) . . ? O21 V2 N21 94.11(7) . . ? O23 V2 N21 161.04(6) . . ? O4 V2 N21 82.50(6) . . ? O22 V2 N21 78.67(6) . . ? O21 V2 N12 170.67(7) . . ? O23 V2 N12 86.73(6) . . ? O4 V2 N12 76.66(6) . . ? O22 V2 N12 82.09(6) . . ? N21 V2 N12 76.56(6) . . ? O5 C51 C52 114.5(9) . . ? O5 C51 H51A 108.6 . . ? C52 C51 H51A 108.6 . . ? O5 C51 H51B 108.6 . . ? C52 C51 H51B 108.6 . . ? H51A C51 H51B 107.6 . . ? _diffrn_measured_fraction_theta_max 0.857 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.427 _refine_diff_density_min -0.409 _refine_diff_density_rms 0.055 #===END data_3c_x_0.5_PrOH _database_code_depnum_ccdc_archive 'CCDC 733239' _audit_creation_method SHELXL-97 _chemical_name_systematic ;\ \m-oxo-dioxobis[2-(5-phenylamino-[1,3,4]thiadiazol-2-yl)-phenolato]-dipropoxo-\ divanadium(V) propanol hemisolvate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H34 N6 O7 S2 V2, 0.5(C3 H8 O)' _chemical_formula_sum 'C35.50 H38 N6 O7.50 S2 V2' _chemical_formula_weight 834.72 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' S S 0.1246 0.1234 '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 'P 21/c' _symmetry_Int_Tables_number 14 _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.4762(5) _cell_length_b 17.2325(7) _cell_length_c 17.0544(6) _cell_angle_alpha 90.00 _cell_angle_beta 101.835(4) _cell_angle_gamma 90.00 _cell_volume 3876.3(3) _cell_formula_units_Z 4 _cell_measurement_temperature 295(2) _cell_measurement_reflns_used 3940 _cell_measurement_theta_min 3.7252 _cell_measurement_theta_max 34.8212 _exptl_crystal_description needle _exptl_crystal_colour red _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.430 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1724 _exptl_absorpt_coefficient_mu 0.646 _exptl_absorpt_correction_T_min 0.694 _exptl_absorpt_correction_T_max 0.968 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 295(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcalibur CCD' _diffrn_measurement_method '\w scans' _diffrn_radiation_collimation '0.8 mm' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16269 _diffrn_reflns_av_R_equivalents 0.0474 _diffrn_reflns_av_sigmaI/netI 0.0981 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.85 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6706 _reflns_number_gt 3288 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.5 (release 28-08-2006 CrysAlis171 .NET) (compiled Aug 28 2006,13:05:05) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0449P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6706 _refine_ls_number_parameters 506 _refine_ls_number_restraints 235 _refine_ls_R_factor_all 0.1066 _refine_ls_R_factor_gt 0.0409 _refine_ls_wR_factor_ref 0.0999 _refine_ls_wR_factor_gt 0.0807 _refine_ls_goodness_of_fit_ref 0.866 _refine_ls_restrained_S_all 0.859 _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 C11 C 0.0219(3) 0.7377(2) 0.54280(19) 0.0585(10) Uani 1 1 d . . . C12 C 0.1091(3) 0.7043(2) 0.59085(19) 0.0545(9) Uani 1 1 d . . . C13 C 0.0982(3) 0.6634(2) 0.65988(18) 0.0615(10) Uani 1 1 d . . . H13 H 0.1550 0.6404 0.6916 0.074 Uiso 1 1 calc R . . C14 C 0.0068(4) 0.6567(3) 0.6815(2) 0.0809(12) Uani 1 1 d . . . H14 H 0.0012 0.6298 0.7277 0.097 Uiso 1 1 calc R . . C15 C -0.0776(3) 0.6904(3) 0.6339(2) 0.0845(13) Uani 1 1 d . . . H15 H -0.1402 0.6860 0.6484 0.101 Uiso 1 1 calc R . . C16 C -0.0707(3) 0.7298(2) 0.5661(2) 0.0762(12) Uani 1 1 d . . . H16 H -0.1286 0.7517 0.5350 0.091 Uiso 1 1 calc R . . C17 C 0.2048(3) 0.7096(2) 0.56573(18) 0.0520(9) Uani 1 1 d . . . C18 C 0.3713(3) 0.6958(2) 0.53735(18) 0.0548(9) Uani 1 1 d . . . C19 C 0.5284(3) 0.6171(2) 0.5603(2) 0.0733(11) Uani 1 1 d . . . C21 C 0.4217(3) 0.7046(2) 0.2987(2) 0.0638(10) Uani 1 1 d . . . C22 C 0.3286(3) 0.6804(2) 0.25105(18) 0.0562(9) Uani 1 1 d . . . C23 C 0.3290(3) 0.6412(2) 0.17826(19) 0.0666(11) Uani 1 1 d . . . H23 H 0.2680 0.6243 0.1471 0.080 Uiso 1 1 calc R . . C24 C 0.4165(4) 0.6279(3) 0.1531(2) 0.0847(13) Uani 1 1 d . . . H24 H 0.4151 0.6029 0.1045 0.102 Uiso 1 1 calc R . . C25 C 0.5066(4) 0.6512(3) 0.1992(3) 0.0987(15) Uani 1 1 d . . . H25 H 0.5665 0.6418 0.1818 0.118 Uiso 1 1 calc R . . C26 C 0.5101(3) 0.6891(3) 0.2720(2) 0.0846(13) Uani 1 1 d . . . H26 H 0.5723 0.7040 0.3029 0.102 Uiso 1 1 calc R . . C27 C 0.2348(3) 0.6955(2) 0.27751(18) 0.0546(9) Uani 1 1 d . . . C28 C 0.0707(3) 0.7010(2) 0.30999(18) 0.0560(9) Uani 1 1 d . . . C29 C -0.1005(3) 0.6415(2) 0.2984(2) 0.0668(11) Uani 1 1 d . . . C110 C 0.5283(3) 0.5888(3) 0.6365(3) 0.1001(16) Uani 1 1 d . . . H110 H 0.4857 0.6096 0.6677 0.120 Uiso 1 1 calc R . . C111 C 0.5945(4) 0.5279(4) 0.6647(3) 0.127(2) Uani 1 1 d . . . H111 H 0.5952 0.5069 0.7151 0.153 Uiso 1 1 calc R . . C112 C 0.6578(5) 0.4991(4) 0.6193(4) 0.136(2) Uani 1 1 d . . . H112 H 0.7016 0.4588 0.6393 0.163 Uiso 1 1 calc R . . C113 C 0.6583(4) 0.5275(3) 0.5461(4) 0.137(2) Uani 1 1 d . . . H113 H 0.7024 0.5074 0.5158 0.164 Uiso 1 1 calc R . . C114 C 0.5924(4) 0.5872(3) 0.5162(3) 0.1013(16) Uani 1 1 d . . . H114 H 0.5920 0.6069 0.4653 0.122 Uiso 1 1 calc R . . C214 C -0.1741(3) 0.6343(3) 0.3437(3) 0.0866(13) Uani 1 1 d . . . H214 H -0.1719 0.6661 0.3881 0.104 Uiso 1 1 calc R . . C213 C -0.2509(4) 0.5804(3) 0.3238(4) 0.1114(17) Uani 1 1 d . . . H213 H -0.2998 0.5756 0.3549 0.134 Uiso 1 1 calc R . . C212 C -0.2548(5) 0.5342(3) 0.2583(4) 0.119(2) Uani 1 1 d . . . H212 H -0.3062 0.4976 0.2449 0.143 Uiso 1 1 calc R . . C211 C -0.1844(5) 0.5415(3) 0.2129(4) 0.116(2) Uani 1 1 d . . . H211 H -0.1874 0.5095 0.1686 0.139 Uiso 1 1 calc R . . C210 C -0.1068(3) 0.5965(3) 0.2314(3) 0.1002(16) Uani 1 1 d . . . H210 H -0.0601 0.6025 0.1985 0.120 Uiso 1 1 calc R . . N11 N 0.2239(2) 0.75851(15) 0.51250(14) 0.0499(7) Uani 1 1 d . . . N12 N 0.3184(2) 0.75157(16) 0.49545(14) 0.0530(7) Uani 1 1 d . . . N13 N 0.4631(3) 0.6778(2) 0.52620(17) 0.0693(9) Uani 1 1 d D . . H13N H 0.479(3) 0.695(2) 0.4854(15) 0.083 Uiso 1 1 d D . . N21 N 0.2266(2) 0.74944(15) 0.32955(13) 0.0487(7) Uani 1 1 d . . . N22 N 0.1329(2) 0.75375(15) 0.34843(14) 0.0501(7) Uani 1 1 d . . . N23 N -0.0227(3) 0.69644(18) 0.32428(17) 0.0645(9) Uani 1 1 d D . . H23N H -0.037(3) 0.7312(17) 0.3576(17) 0.077 Uiso 1 1 d D . . O4 O 0.23785(16) 0.87598(12) 0.41648(11) 0.0553(6) Uani 1 1 d . . . O11 O 0.12936(18) 0.90094(13) 0.52607(12) 0.0688(7) Uani 1 1 d . . . O12 O 0.02428(16) 0.77382(13) 0.47380(12) 0.0587(6) Uani 1 1 d . . . O13 O 0.02748(17) 0.89326(13) 0.37652(12) 0.0634(7) Uani 1 1 d DU . . C31A C -0.0521(6) 0.9421(4) 0.3939(9) 0.077(2) Uani 0.729(6) 1 d PDU A 1 H31A H -0.0274 0.9950 0.4011 0.092 Uiso 0.729(6) 1 calc PR A 1 H31B H -0.0691 0.9253 0.4438 0.092 Uiso 0.729(6) 1 calc PR A 1 C32A C -0.1456(4) 0.9408(4) 0.3297(4) 0.0865(19) Uani 0.729(6) 1 d PDU A 1 H32A H -0.1282 0.9543 0.2789 0.104 Uiso 0.729(6) 1 calc PR A 1 H32B H -0.1928 0.9794 0.3414 0.104 Uiso 0.729(6) 1 calc PR A 1 C33A C -0.1970(19) 0.8611(12) 0.3221(9) 0.124(3) Uani 0.729(6) 1 d PDU A 1 H33A H -0.1555 0.8245 0.3011 0.186 Uiso 0.729(6) 1 calc PR A 1 H33B H -0.2620 0.8647 0.2866 0.186 Uiso 0.729(6) 1 calc PR A 1 H33C H -0.2056 0.8442 0.3739 0.186 Uiso 0.729(6) 1 calc PR A 1 C31B C -0.0397(15) 0.9554(9) 0.383(3) 0.077(2) Uani 0.271(6) 1 d PDU A 2 H31C H -0.0531 0.9856 0.3336 0.092 Uiso 0.271(6) 1 calc PR A 2 H31D H -0.0105 0.9894 0.4268 0.092 Uiso 0.271(6) 1 calc PR A 2 C32B C -0.1351(10) 0.9197(10) 0.3971(11) 0.0865(19) Uani 0.271(6) 1 d PDU A 2 H32C H -0.1782 0.9597 0.4123 0.104 Uiso 0.271(6) 1 calc PR A 2 H32D H -0.1191 0.8829 0.4409 0.104 Uiso 0.271(6) 1 calc PR A 2 C33B C -0.191(5) 0.879(4) 0.323(2) 0.124(3) Uani 0.271(6) 1 d PDU A 2 H33D H -0.1983 0.9135 0.2779 0.186 Uiso 0.271(6) 1 calc PR A 2 H33E H -0.2564 0.8630 0.3304 0.186 Uiso 0.271(6) 1 calc PR A 2 H33F H -0.1528 0.8340 0.3129 0.186 Uiso 0.271(6) 1 calc PR A 2 O21 O 0.35006(18) 0.87212(14) 0.30477(12) 0.0699(7) Uani 1 1 d . . . O22 O 0.42582(17) 0.74068(13) 0.36912(12) 0.0614(7) Uani 1 1 d . . . O23 O 0.44946(18) 0.87060(14) 0.45517(13) 0.0686(7) Uani 1 1 d DU . . C41A C 0.5343(4) 0.9091(4) 0.4331(5) 0.094(2) Uani 0.842(8) 1 d PDU C 1 H41A H 0.5142 0.9610 0.4144 0.113 Uiso 0.842(8) 1 calc PR C 1 H41B H 0.5538 0.8811 0.3892 0.113 Uiso 0.842(8) 1 calc PR C 1 C42A C 0.6224(7) 0.9141(7) 0.5004(7) 0.129(3) Uani 0.842(8) 1 d PDU C 1 H42A H 0.6029 0.9420 0.5443 0.155 Uiso 0.842(8) 1 calc PR C 1 H42B H 0.6759 0.9433 0.4836 0.155 Uiso 0.842(8) 1 calc PR C 1 C43A C 0.6633(5) 0.8337(5) 0.5302(5) 0.148(3) Uani 0.842(8) 1 d PDU C 1 H43A H 0.6168 0.8093 0.5583 0.223 Uiso 0.842(8) 1 calc PR C 1 H43B H 0.7281 0.8395 0.5656 0.223 Uiso 0.842(8) 1 calc PR C 1 H43C H 0.6704 0.8022 0.4852 0.223 Uiso 0.842(8) 1 calc PR C 1 C41B C 0.5495(15) 0.880(3) 0.438(3) 0.094(2) Uani 0.158(8) 1 d PDU C 2 H41C H 0.5490 0.9240 0.4030 0.113 Uiso 0.158(8) 1 calc PR C 2 H41D H 0.5658 0.8341 0.4105 0.113 Uiso 0.158(8) 1 calc PR C 2 C42B C 0.630(4) 0.892(5) 0.512(3) 0.129(3) Uani 0.158(8) 1 d PDU C 2 H42C H 0.6574 0.8419 0.5320 0.155 Uiso 0.158(8) 1 calc PR C 2 H42D H 0.6018 0.9169 0.5527 0.155 Uiso 0.158(8) 1 calc PR C 2 C43B C 0.716(2) 0.942(2) 0.492(2) 0.148(3) Uani 0.158(8) 1 d PDU C 2 H43D H 0.7221 0.9330 0.4378 0.223 Uiso 0.158(8) 1 calc PR C 2 H43E H 0.7787 0.9286 0.5276 0.223 Uiso 0.158(8) 1 calc PR C 2 H43F H 0.7012 0.9957 0.4990 0.223 Uiso 0.158(8) 1 calc PR C 2 S1 S 0.30660(7) 0.64986(6) 0.60266(5) 0.0653(3) Uani 1 1 d . . . S2 S 0.12370(7) 0.64409(5) 0.24629(5) 0.0641(3) Uani 1 1 d . . . V1 V 0.12373(4) 0.84815(3) 0.44922(3) 0.05387(19) Uani 1 1 d . A . V2 V 0.34488(5) 0.83009(3) 0.38672(3) 0.0568(2) Uani 1 1 d . C . O5 O 0.0772(16) 0.5300(8) 0.4275(8) 0.206(4) Uani 0.50 1 d PDU D -1 H5 H 0.0677 0.5765 0.4187 0.310 Uiso 0.50 1 calc PR D -1 C51 C 0.051(2) 0.5110(13) 0.5001(12) 0.206(4) Uani 0.50 1 d PDU D -1 H51A H 0.0862 0.5464 0.5406 0.248 Uiso 0.50 1 calc PR D -1 H51B H 0.0764 0.4593 0.5150 0.248 Uiso 0.50 1 calc PR D -1 C52 C -0.055(2) 0.5123(11) 0.5039(14) 0.206(4) Uani 0.50 1 d PDU D -1 H52A H -0.0960 0.5076 0.4502 0.248 Uiso 0.50 1 calc PR D -1 H52B H -0.0712 0.5618 0.5256 0.248 Uiso 0.50 1 calc PR D -1 C53 C -0.083(2) 0.4480(12) 0.5551(12) 0.206(4) Uani 0.50 1 d PDU D -1 H53A H -0.1546 0.4491 0.5532 0.310 Uiso 0.50 1 calc PR D -1 H53B H -0.0471 0.4548 0.6094 0.310 Uiso 0.50 1 calc PR D -1 H53C H -0.0648 0.3990 0.5353 0.310 Uiso 0.50 1 calc PR D -1 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 C11 0.071(3) 0.066(3) 0.042(2) -0.0099(18) 0.0185(18) 0.003(2) C12 0.067(3) 0.052(2) 0.043(2) -0.0102(17) 0.0078(18) 0.0060(19) C13 0.074(3) 0.069(3) 0.041(2) -0.0001(18) 0.0120(18) -0.001(2) C14 0.102(4) 0.094(3) 0.051(2) 0.000(2) 0.024(2) -0.015(3) C15 0.077(3) 0.120(4) 0.064(3) 0.000(3) 0.030(2) -0.010(3) C16 0.071(3) 0.103(3) 0.058(2) -0.004(2) 0.020(2) 0.009(2) C17 0.060(2) 0.053(2) 0.0406(19) -0.0038(17) 0.0045(17) 0.0058(19) C18 0.064(2) 0.058(2) 0.0413(19) 0.0007(17) 0.0103(17) 0.013(2) C19 0.070(3) 0.080(3) 0.066(3) 0.014(2) 0.005(2) 0.023(2) C21 0.066(3) 0.069(3) 0.056(2) 0.014(2) 0.011(2) 0.022(2) C22 0.080(3) 0.051(2) 0.0406(19) 0.0096(16) 0.0190(18) 0.023(2) C23 0.089(3) 0.065(3) 0.048(2) 0.0091(18) 0.019(2) 0.029(2) C24 0.104(4) 0.089(3) 0.066(3) 0.004(2) 0.030(3) 0.036(3) C25 0.104(4) 0.127(4) 0.077(3) 0.006(3) 0.047(3) 0.041(3) C26 0.066(3) 0.118(4) 0.072(3) 0.014(3) 0.020(2) 0.026(3) C27 0.075(3) 0.053(2) 0.0371(18) 0.0111(17) 0.0135(17) 0.022(2) C28 0.071(3) 0.048(2) 0.047(2) -0.0085(17) 0.0066(19) 0.014(2) C29 0.069(3) 0.052(3) 0.072(3) -0.012(2) -0.001(2) 0.011(2) C110 0.078(3) 0.130(4) 0.086(3) 0.042(3) 0.002(2) 0.030(3) C111 0.104(4) 0.152(6) 0.119(4) 0.069(4) 0.006(4) 0.029(4) C112 0.114(5) 0.128(5) 0.156(6) 0.056(5) 0.006(4) 0.060(4) C113 0.135(5) 0.126(5) 0.148(5) 0.023(4) 0.027(4) 0.080(4) C114 0.104(4) 0.120(4) 0.081(3) 0.017(3) 0.024(3) 0.055(3) C214 0.073(3) 0.084(3) 0.098(3) -0.008(3) 0.007(3) -0.005(3) C213 0.088(4) 0.094(4) 0.147(5) 0.009(4) 0.011(3) -0.021(3) C212 0.099(5) 0.069(4) 0.172(6) -0.022(4) -0.011(4) -0.009(3) C211 0.088(4) 0.099(4) 0.150(5) -0.063(4) -0.004(4) 0.005(3) C210 0.073(3) 0.102(4) 0.120(4) -0.053(3) 0.006(3) 0.007(3) N11 0.0593(19) 0.0465(18) 0.0425(16) -0.0035(13) 0.0071(14) 0.0070(15) N12 0.0521(18) 0.057(2) 0.0478(16) 0.0020(14) 0.0064(13) 0.0135(16) N13 0.066(2) 0.082(2) 0.065(2) 0.0247(18) 0.0254(17) 0.0316(19) N21 0.0639(19) 0.0485(18) 0.0343(14) -0.0009(13) 0.0115(13) 0.0173(15) N22 0.0607(19) 0.0519(18) 0.0384(15) -0.0033(13) 0.0115(14) 0.0116(16) N23 0.069(2) 0.057(2) 0.067(2) -0.0180(15) 0.0121(18) 0.0076(19) O4 0.0635(15) 0.0477(14) 0.0543(12) -0.0016(11) 0.0109(11) 0.0109(12) O11 0.0816(18) 0.0648(17) 0.0583(14) -0.0166(12) 0.0103(12) 0.0179(14) O12 0.0575(15) 0.0692(16) 0.0491(14) -0.0035(12) 0.0104(11) 0.0093(12) O13 0.0703(16) 0.0638(16) 0.0543(13) -0.0008(12) 0.0089(12) 0.0230(13) C31A 0.082(3) 0.074(4) 0.075(5) -0.005(3) 0.015(3) 0.034(3) C32A 0.071(3) 0.079(4) 0.106(5) 0.000(4) 0.008(3) 0.028(3) C33A 0.095(5) 0.097(11) 0.176(5) -0.015(5) 0.019(4) -0.001(6) C31B 0.082(3) 0.074(4) 0.075(5) -0.005(3) 0.015(3) 0.034(3) C32B 0.071(3) 0.079(4) 0.106(5) 0.000(4) 0.008(3) 0.028(3) C33B 0.095(5) 0.097(11) 0.176(5) -0.015(5) 0.019(4) -0.001(6) O21 0.0835(17) 0.0693(17) 0.0586(14) 0.0157(12) 0.0187(12) 0.0166(14) O22 0.0652(16) 0.0725(17) 0.0454(13) 0.0007(12) 0.0090(11) 0.0205(13) O23 0.0620(15) 0.0768(18) 0.0670(15) -0.0026(13) 0.0131(12) -0.0030(14) C41A 0.078(3) 0.103(6) 0.102(3) 0.012(4) 0.023(3) -0.011(3) C42A 0.073(4) 0.160(8) 0.154(5) -0.019(5) 0.025(3) -0.019(4) C43A 0.075(4) 0.185(7) 0.185(7) 0.001(6) 0.027(4) 0.025(4) C41B 0.078(3) 0.103(6) 0.102(3) 0.012(4) 0.023(3) -0.011(3) C42B 0.073(4) 0.160(8) 0.154(5) -0.019(5) 0.025(3) -0.019(4) C43B 0.075(4) 0.185(7) 0.185(7) 0.001(6) 0.027(4) 0.025(4) S1 0.0790(7) 0.0649(6) 0.0521(5) 0.0121(5) 0.0138(5) 0.0166(5) S2 0.0804(7) 0.0558(6) 0.0550(5) -0.0117(4) 0.0111(5) 0.0122(5) V1 0.0626(4) 0.0524(4) 0.0456(3) -0.0055(3) 0.0088(3) 0.0144(3) V2 0.0638(4) 0.0567(4) 0.0497(3) 0.0052(3) 0.0108(3) 0.0099(3) O5 0.253(6) 0.152(8) 0.188(7) 0.014(5) -0.015(6) 0.066(6) C51 0.253(6) 0.152(8) 0.188(7) 0.014(5) -0.015(6) 0.066(6) C52 0.253(6) 0.152(8) 0.188(7) 0.014(5) -0.015(6) 0.066(6) C53 0.253(6) 0.152(8) 0.188(7) 0.014(5) -0.015(6) 0.066(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C11 O12 1.337(4) . ? C11 C16 1.393(5) . ? C11 C12 1.410(5) . ? C12 C13 1.405(5) . ? C12 C17 1.443(5) . ? C13 C14 1.362(5) . ? C13 H13 0.9300 . ? C14 C15 1.383(5) . ? C14 H14 0.9300 . ? C15 C16 1.359(5) . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C17 N11 1.303(4) . ? C17 S1 1.728(3) . ? C18 N12 1.317(4) . ? C18 N13 1.326(4) . ? C18 S1 1.739(4) . ? C19 C114 1.358(5) . ? C19 C110 1.388(5) . ? C19 N13 1.412(5) . ? C21 O22 1.343(4) . ? C21 C26 1.387(5) . ? C21 C22 1.410(5) . ? C22 C23 1.414(4) . ? C22 C27 1.451(5) . ? C23 C24 1.354(5) . ? C23 H23 0.9300 . ? C24 C25 1.365(6) . ? C24 H24 0.9300 . ? C25 C26 1.395(5) . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C27 N21 1.305(4) . ? C27 S2 1.727(4) . ? C28 N22 1.316(4) . ? C28 N23 1.333(4) . ? C28 S2 1.723(4) . ? C29 C210 1.370(5) . ? C29 C214 1.383(6) . ? C29 N23 1.414(5) . ? C110 C111 1.398(6) . ? C110 H110 0.9300 . ? C111 C112 1.359(7) . ? C111 H111 0.9300 . ? C112 C113 1.342(7) . ? C112 H112 0.9300 . ? C113 C114 1.386(6) . ? C113 H113 0.9300 . ? C114 H114 0.9300 . ? C214 C213 1.380(6) . ? C214 H214 0.9300 . ? C213 C212 1.365(7) . ? C213 H213 0.9300 . ? C212 C211 1.348(7) . ? C212 H212 0.9300 . ? C211 C210 1.398(7) . ? C211 H211 0.9300 . ? C210 H210 0.9300 . ? N11 N12 1.368(3) . ? N11 V1 2.185(3) . ? N12 V2 2.381(3) . ? N13 H13N 0.828(18) . ? N21 N22 1.368(3) . ? N21 V2 2.188(3) . ? N22 V1 2.388(3) . ? N23 H23N 0.873(18) . ? O4 V1 1.805(2) . ? O4 V2 1.806(2) . ? O11 V1 1.584(2) . ? O12 V1 1.960(2) . ? O13 C31B 1.420(10) . ? O13 C31A 1.441(6) . ? O13 V1 1.779(2) . ? C31A C32A 1.490(12) . ? C31A H31A 0.9700 . ? C31A H31B 0.9700 . ? C32A C33A 1.531(14) . ? C32A H32A 0.9700 . ? C32A H32B 0.9700 . ? C33A H33A 0.9600 . ? C33A H33B 0.9600 . ? C33A H33C 0.9600 . ? C31B C32B 1.490(10) . ? C31B H31C 0.9700 . ? C31B H31D 0.9700 . ? C32B C33B 1.507(10) . ? C32B H32C 0.9700 . ? C32B H32D 0.9700 . ? C33B H33D 0.9600 . ? C33B H33E 0.9600 . ? C33B H33F 0.9600 . ? O21 V2 1.588(2) . ? O22 V2 1.946(2) . ? O23 C41A 1.437(5) . ? O23 C41B 1.442(10) . ? O23 V2 1.778(2) . ? C41A C42A 1.475(6) . ? C41A H41A 0.9700 . ? C41A H41B 0.9700 . ? C42A C43A 1.538(13) . ? C42A H42A 0.9700 . ? C42A H42B 0.9700 . ? C43A H43A 0.9600 . ? C43A H43B 0.9600 . ? C43A H43C 0.9600 . ? C41B C42B 1.493(18) . ? C41B H41C 0.9700 . ? C41B H41D 0.9700 . ? C42B C43B 1.53(2) . ? C42B H42C 0.9700 . ? C42B H42D 0.9700 . ? C43B H43D 0.9600 . ? C43B H43E 0.9600 . ? C43B H43F 0.9600 . ? O5 C51 1.396(10) . ? O5 H5 0.8200 . ? C51 C52 1.445(8) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C52 C53 1.504(10) . ? C52 H52A 0.9700 . ? C52 H52B 0.9700 . ? C53 H53A 0.9600 . ? C53 H53B 0.9600 . ? C53 H53C 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 O12 C11 C16 118.8(3) . . ? O12 C11 C12 122.3(4) . . ? C16 C11 C12 118.8(4) . . ? C13 C12 C11 118.3(4) . . ? C13 C12 C17 122.3(3) . . ? C11 C12 C17 119.3(3) . . ? C14 C13 C12 121.7(4) . . ? C14 C13 H13 119.2 . . ? C12 C13 H13 119.2 . . ? C13 C14 C15 119.1(4) . . ? C13 C14 H14 120.5 . . ? C15 C14 H14 120.5 . . ? C16 C15 C14 121.1(4) . . ? C16 C15 H15 119.4 . . ? C14 C15 H15 119.4 . . ? C15 C16 C11 120.9(4) . . ? C15 C16 H16 119.5 . . ? C11 C16 H16 119.5 . . ? N11 C17 C12 124.4(3) . . ? N11 C17 S1 112.5(3) . . ? C12 C17 S1 123.0(3) . . ? N12 C18 N13 120.7(3) . . ? N12 C18 S1 113.2(3) . . ? N13 C18 S1 126.2(3) . . ? C114 C19 C110 120.5(4) . . ? C114 C19 N13 117.8(4) . . ? C110 C19 N13 121.7(4) . . ? O22 C21 C26 120.1(4) . . ? O22 C21 C22 121.5(4) . . ? C26 C21 C22 118.4(4) . . ? C21 C22 C23 119.0(4) . . ? C21 C22 C27 119.7(3) . . ? C23 C22 C27 121.3(4) . . ? C24 C23 C22 121.3(4) . . ? C24 C23 H23 119.3 . . ? C22 C23 H23 119.3 . . ? C23 C24 C25 119.7(4) . . ? C23 C24 H24 120.1 . . ? C25 C24 H24 120.1 . . ? C24 C25 C26 121.0(4) . . ? C24 C25 H25 119.5 . . ? C26 C25 H25 119.5 . . ? C21 C26 C25 120.5(4) . . ? C21 C26 H26 119.7 . . ? C25 C26 H26 119.7 . . ? N21 C27 C22 122.7(3) . . ? N21 C27 S2 112.7(3) . . ? C22 C27 S2 124.6(3) . . ? N22 C28 N23 118.6(3) . . ? N22 C28 S2 113.8(3) . . ? N23 C28 S2 127.6(3) . . ? C210 C29 C214 119.1(4) . . ? C210 C29 N23 123.7(4) . . ? C214 C29 N23 117.2(4) . . ? C19 C110 C111 117.6(5) . . ? C19 C110 H110 121.2 . . ? C111 C110 H110 121.2 . . ? C112 C111 C110 120.6(5) . . ? C112 C111 H111 119.7 . . ? C110 C111 H111 119.7 . . ? C113 C112 C111 121.4(5) . . ? C113 C112 H112 119.3 . . ? C111 C112 H112 119.3 . . ? C112 C113 C114 119.2(5) . . ? C112 C113 H113 120.4 . . ? C114 C113 H113 120.4 . . ? C19 C114 C113 120.7(5) . . ? C19 C114 H114 119.7 . . ? C113 C114 H114 119.7 . . ? C213 C214 C29 120.7(5) . . ? C213 C214 H214 119.6 . . ? C29 C214 H214 119.6 . . ? C212 C213 C214 119.7(6) . . ? C212 C213 H213 120.2 . . ? C214 C213 H213 120.2 . . ? C211 C212 C213 120.2(5) . . ? C211 C212 H212 119.9 . . ? C213 C212 H212 119.9 . . ? C212 C211 C210 121.0(5) . . ? C212 C211 H211 119.5 . . ? C210 C211 H211 119.5 . . ? C29 C210 C211 119.2(5) . . ? C29 C210 H210 120.4 . . ? C211 C210 H210 120.4 . . ? C17 N11 N12 114.7(3) . . ? C17 N11 V1 127.6(2) . . ? N12 N11 V1 117.7(2) . . ? C18 N12 N11 111.9(3) . . ? C18 N12 V2 133.4(2) . . ? N11 N12 V2 114.23(18) . . ? C18 N13 C19 129.4(3) . . ? C18 N13 H13N 117(3) . . ? C19 N13 H13N 111(3) . . ? C27 N21 N22 114.2(3) . . ? C27 N21 V2 126.8(2) . . ? N22 N21 V2 118.96(19) . . ? C28 N22 N21 111.7(3) . . ? C28 N22 V1 135.0(3) . . ? N21 N22 V1 113.13(19) . . ? C28 N23 C29 130.5(3) . . ? C28 N23 H23N 115(2) . . ? C29 N23 H23N 115(2) . . ? V1 O4 V2 138.64(13) . . ? C11 O12 V1 129.2(2) . . ? C31B O13 V1 131.5(18) . . ? C31A O13 V1 125.4(6) . . ? O13 C31A C32A 113.1(9) . . ? O13 C31A H31A 109.0 . . ? C32A C31A H31A 109.0 . . ? O13 C31A H31B 109.0 . . ? C32A C31A H31B 109.0 . . ? H31A C31A H31B 107.8 . . ? C31A C32A C33A 112.1(10) . . ? C31A C32A H32A 109.2 . . ? C33A C32A H32A 109.2 . . ? C31A C32A H32B 109.2 . . ? C33A C32A H32B 109.2 . . ? H32A C32A H32B 107.9 . . ? O13 C31B C32B 106.6(11) . . ? O13 C31B H31C 110.4 . . ? C32B C31B H31C 110.4 . . ? O13 C31B H31D 110.4 . . ? C32B C31B H31D 110.4 . . ? H31C C31B H31D 108.6 . . ? C31B C32B C33B 110.6(15) . . ? C31B C32B H32C 109.5 . . ? C33B C32B H32C 109.5 . . ? C31B C32B H32D 109.5 . . ? C33B C32B H32D 109.5 . . ? H32C C32B H32D 108.1 . . ? C32B C33B H33D 109.5 . . ? C32B C33B H33E 109.5 . . ? H33D C33B H33E 109.5 . . ? C32B C33B H33F 109.5 . . ? H33D C33B H33F 109.5 . . ? H33E C33B H33F 109.5 . . ? C21 O22 V2 125.62(19) . . ? C41A O23 V2 125.1(4) . . ? C41B O23 V2 124(2) . . ? O23 C41A C42A 112.3(6) . . ? O23 C41A H41A 109.1 . . ? C42A C41A H41A 109.1 . . ? O23 C41A H41B 109.1 . . ? C42A C41A H41B 109.1 . . ? H41A C41A H41B 107.9 . . ? C41A C42A C43A 112.4(7) . . ? C41A C42A H42A 109.1 . . ? C43A C42A H42A 109.1 . . ? C41A C42A H42B 109.1 . . ? C43A C42A H42B 109.1 . . ? H42A C42A H42B 107.9 . . ? C42A C43A H43A 109.5 . . ? C42A C43A H43B 109.5 . . ? H43A C43A H43B 109.5 . . ? C42A C43A H43C 109.5 . . ? H43A C43A H43C 109.5 . . ? H43B C43A H43C 109.5 . . ? O23 C41B C42B 114(3) . . ? O23 C41B H41C 108.8 . . ? C42B C41B H41C 108.8 . . ? O23 C41B H41D 108.8 . . ? C42B C41B H41D 108.8 . . ? H41C C41B H41D 107.7 . . ? C41B C42B C43B 111(2) . . ? C41B C42B H42C 109.5 . . ? C43B C42B H42C 109.5 . . ? C41B C42B H42D 109.5 . . ? C43B C42B H42D 109.5 . . ? H42C C42B H42D 108.1 . . ? C42B C43B H43D 109.5 . . ? C42B C43B H43E 109.5 . . ? H43D C43B H43E 109.5 . . ? C42B C43B H43F 109.5 . . ? H43D C43B H43F 109.5 . . ? H43E C43B H43F 109.5 . . ? C17 S1 C18 87.72(18) . . ? C28 S2 C27 87.63(19) . . ? O11 V1 O13 103.29(11) . . ? O11 V1 O4 101.77(12) . . ? O13 V1 O4 102.35(10) . . ? O11 V1 O12 96.73(11) . . ? O13 V1 O12 90.10(10) . . ? O4 V1 O12 154.53(10) . . ? O11 V1 N11 94.44(10) . . ? O13 V1 N11 160.29(10) . . ? O4 V1 N11 82.03(10) . . ? O12 V1 N11 79.21(10) . . ? O11 V1 N22 170.32(10) . . ? O13 V1 N22 86.21(9) . . ? O4 V1 N22 77.61(10) . . ? O12 V1 N22 81.22(10) . . ? N11 V1 N22 75.89(9) . . ? O21 V2 O23 103.11(12) . . ? O21 V2 O4 103.26(11) . . ? O23 V2 O4 102.40(10) . . ? O21 V2 O22 95.63(11) . . ? O23 V2 O22 91.05(11) . . ? O4 V2 O22 153.49(11) . . ? O21 V2 N21 93.26(11) . . ? O23 V2 N21 161.63(10) . . ? O4 V2 N21 81.51(10) . . ? O22 V2 N21 78.96(10) . . ? O21 V2 N12 170.11(11) . . ? O23 V2 N12 86.39(10) . . ? O4 V2 N12 76.94(10) . . ? O22 V2 N12 81.29(10) . . ? N21 V2 N12 76.94(9) . . ? C51 O5 H5 109.5 . . ? O5 C51 C52 118.1(14) . . ? O5 C51 H51A 107.8 . . ? C52 C51 H51A 107.8 . . ? O5 C51 H51B 107.8 . . ? C52 C51 H51B 107.8 . . ? H51A C51 H51B 107.1 . . ? C51 C52 C53 112.3(13) . . ? C51 C52 H52A 109.1 . . ? C53 C52 H52A 109.1 . . ? C51 C52 H52B 109.1 . . ? C53 C52 H52B 109.1 . . ? H52A C52 H52B 107.9 . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.247 _refine_diff_density_min -0.236 _refine_diff_density_rms 0.048