#------------------------------------------------------------------------------ #$Date: 2011-09-28 17:24:46 +0300 (Wed, 28 Sep 2011) $ #$Revision: 26848 $ #$URL: file:///home/coder/svn-repositories/cod/cif/2/20/48/2204821.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2204821 loop_ _publ_author_name 'Gao, Shan' 'Huo, Li-Hua' 'Zhao, Hui' 'Ng, Seik Weng' _publ_section_title ; (N-Benzoyl-N-phenylhydroxlaminato-\k^2^O,O')oxo(salicylaldehyde isonicotinoylhydrazonato-\k^3^O,N,N')vanadium(IV) hexane hemisolvate ; _journal_issue 12 _journal_name_full 'Acta Crystallographica, Section E' _journal_page_first m1757 _journal_page_last m1758 _journal_volume 60 _journal_year 2004 _chemical_formula_iupac '[V (C13 H10 N O2) (C13 H10 N3 O2) O], 0.5C6 H14' _chemical_formula_moiety 'C26 H20 N4 O5 V, 0.5C6 H14' _chemical_formula_sum 'C29 H27 N4 O5 V' _chemical_formula_weight 562.49 _chemical_name_systematic ; (N-Benzoyl-N-phenylhydroxlaminato-\k^2^O,O')oxo(salicylaldehyde isonicotinoylhydrazonato-\k^3^O,N,N')vanadium(IV) hexane hemisolvate ; _symmetry_cell_setting triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-97 _cell_angle_alpha 102.92(3) _cell_angle_beta 98.52(3) _cell_angle_gamma 113.49(3) _cell_formula_units_Z 2 _cell_length_a 10.071(2) _cell_length_b 12.016(2) _cell_length_c 12.966(3) _cell_measurement_reflns_used 10306 _cell_measurement_temperature 295(2) _cell_measurement_theta_max 27.4 _cell_measurement_theta_min 3.3 _cell_volume 1352.3(5) _computing_cell_refinement RAPID-AUTO _computing_data_collection ; RAPID-AUTO (Rigaku, 1998) ; _computing_data_reduction ; CrystalStructure (Rigaku/MSC, 2002) ; _computing_molecular_graphics 'ORTEPII (Johnson, 1976)' _computing_publication_material SHELXL97 _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1997)' _diffrn_ambient_temperature 295(2) _diffrn_measured_fraction_theta_full 0.984 _diffrn_measured_fraction_theta_max 0.984 _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_radiation_monochromator graphite _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.036 _diffrn_reflns_av_sigmaI/netI 0.053 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 12805 _diffrn_reflns_theta_full 27.48 _diffrn_reflns_theta_max 27.5 _diffrn_reflns_theta_min 3.2 _diffrn_standards_decay_% 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.413 _exptl_absorpt_correction_T_max 0.926 _exptl_absorpt_correction_T_min 0.725 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details '(ABSCOR; Higashi, 1995)' _exptl_crystal_colour Red _exptl_crystal_density_diffrn 1.379 _exptl_crystal_density_method 'not measured' _exptl_crystal_description Prism _exptl_crystal_F_000 582 _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.19 _refine_diff_density_max 0.335 _refine_diff_density_min -0.435 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.011 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 352 _refine_ls_number_reflns 6103 _refine_ls_number_restraints 3 _refine_ls_restrained_S_all 1.015 _refine_ls_R_factor_all 0.1083 _refine_ls_R_factor_gt 0.0578 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'calc w = 1/[\s^2^(Fo^2^)+(0.0737P)^2^+0.0547P] where P = (Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1241 _refine_ls_wR_factor_ref 0.1410 _reflns_number_gt 3780 _reflns_number_total 6103 _reflns_threshold_expression I>2\s(I) _[local]_cod_data_source_file wn6302.cif _cod_depositor_comments ; The following automatic conversions were performed: '_symmetry_cell_setting' value 'Triclinic' changed to 'triclinic' according to '/home/saulius/struct/CIF-dictionaries/cif_core.dic' dictionary named 'cif_core.dic' version 2.4.1 from 2010-06-29. Automatic conversion script Id: cif_fix_enum 1527 2010-12-29 10:47:43Z saulius ; _cod_database_code 2204821 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_refinement_flags _atom_site_occupancy _atom_site_type_symbol V1 0.64737(6) 0.79909(4) 0.78465(3) 0.05068(17) Uani d . 1 V O1 0.8236(2) 0.80155(19) 0.85510(15) 0.0593(5) Uani d . 1 O O2 0.4668(2) 0.72947(19) 0.66481(15) 0.0594(5) Uani d . 1 O O3 0.5431(2) 0.60044(16) 0.78477(14) 0.0538(5) Uani d . 1 O O4 0.5403(2) 0.79930(16) 0.89018(14) 0.0513(5) Uani d . 1 O O5 0.7097(3) 0.94608(18) 0.79665(16) 0.0688(6) Uani d . 1 O N1 0.7081(3) 0.7398(2) 0.64337(17) 0.0490(5) Uani d . 1 N N2 0.5942(3) 0.6804(2) 0.54636(18) 0.0559(6) Uani d . 1 N H2n 0.6032 0.6486 0.4830 0.067 Uiso calc R 1 H N3 0.0740(4) 0.5284(3) 0.3072(3) 0.0892(9) Uani d . 1 N N4 0.4416(2) 0.68506(19) 0.89802(16) 0.0456(5) Uani d . 1 N C1 0.9588(3) 0.8388(2) 0.8354(2) 0.0519(7) Uani d . 1 C C2 1.0880(3) 0.8960(3) 0.9219(2) 0.0581(7) Uani d . 1 C H2 1.0808 0.9139 0.9939 0.070 Uiso calc R 1 H C3 1.2260(4) 0.9263(3) 0.9016(3) 0.0664(8) Uani d . 1 C H3 1.3114 0.9648 0.9603 0.080 Uiso calc R 1 H C4 1.2408(4) 0.9009(3) 0.7960(3) 0.0707(9) Uani d . 1 C H4 1.3349 0.9207 0.7833 0.085 Uiso calc R 1 H C5 1.1145(4) 0.8459(3) 0.7101(3) 0.0660(8) Uani d . 1 C H5 1.1238 0.8285 0.6387 0.079 Uiso calc R 1 H C6 0.9708(3) 0.8150(3) 0.7271(2) 0.0517(7) Uani d . 1 C C7 0.8408(3) 0.7565(3) 0.6364(2) 0.0560(7) Uani d . 1 C H7 0.8525 0.7283 0.5670 0.067 Uiso calc R 1 H C8 0.4725(3) 0.6807(3) 0.5662(2) 0.0518(7) Uani d . 1 C C9 0.3355(3) 0.6262(3) 0.4763(2) 0.0532(7) Uani d . 1 C C10 0.3287(4) 0.5681(3) 0.3705(2) 0.0667(8) Uani d . 1 C H10 0.4119 0.5608 0.3532 0.080 Uiso calc R 1 H C11 0.1966(5) 0.5209(3) 0.2903(3) 0.0820(11) Uani d . 1 C H11 0.1937 0.4809 0.2192 0.098 Uiso calc R 1 H C12 0.0813(5) 0.5830(4) 0.4093(4) 0.0973(13) Uani d . 1 C H12 -0.0037 0.5889 0.4240 0.117 Uiso calc R 1 H C13 0.2075(4) 0.6320(4) 0.4957(3) 0.0824(11) Uani d . 1 C H13 0.2059 0.6687 0.5664 0.099 Uiso calc R 1 H C14 0.4499(3) 0.5813(2) 0.84043(19) 0.0431(6) Uani d . 1 C C15 0.3506(3) 0.4513(2) 0.8396(2) 0.0440(6) Uani d . 1 C C16 0.3027(3) 0.3542(3) 0.7413(2) 0.0578(7) Uani d . 1 C H16 0.3308 0.3729 0.6797 0.069 Uiso calc R 1 H C17 0.2138(4) 0.2305(3) 0.7349(3) 0.0754(10) Uani d . 1 C H17 0.1809 0.1659 0.6686 0.090 Uiso calc R 1 H C18 0.1728(4) 0.2009(3) 0.8250(3) 0.0772(10) Uani d . 1 C H18 0.1118 0.1168 0.8196 0.093 Uiso calc R 1 H C19 0.2221(3) 0.2961(3) 0.9236(3) 0.0612(8) Uani d . 1 C H19 0.1957 0.2760 0.9852 0.073 Uiso calc R 1 H C20 0.3100(3) 0.4205(3) 0.9312(2) 0.0495(6) Uani d . 1 C H20 0.3427 0.4845 0.9979 0.059 Uiso calc R 1 H C21 0.3507(3) 0.6970(2) 0.97120(19) 0.0430(6) Uani d . 1 C C22 0.1973(3) 0.6420(3) 0.9324(2) 0.0548(7) Uani d . 1 C H22 0.1505 0.5976 0.8584 0.066 Uiso calc R 1 H C23 0.1143(4) 0.6543(3) 1.0060(3) 0.0711(9) Uani d . 1 C H23 0.0101 0.6165 0.9815 0.085 Uiso calc R 1 H C24 0.1834(5) 0.7212(4) 1.1141(3) 0.0820(11) Uani d . 1 C H24 0.1263 0.7282 1.1631 0.098 Uiso calc R 1 H C25 0.3362(5) 0.7778(4) 1.1504(3) 0.0863(11) Uani d . 1 C H25 0.3827 0.8254 1.2239 0.104 Uiso calc R 1 H C26 0.4231(4) 0.7654(3) 1.0796(2) 0.0625(8) Uani d . 1 C H26 0.5272 0.8022 1.1045 0.075 Uiso calc R 1 H C27 0.5778(4) 1.0216(5) 0.5374(3) 0.1172(16) Uani d D 1 C H27A 0.6245 1.1137 0.5699 0.141 Uiso calc R 1 H H27B 0.5660 0.9844 0.5966 0.141 Uiso calc R 1 H C28 0.6781(6) 0.9863(5) 0.4809(5) 0.135(2) Uani d D 1 C H28A 0.6848 1.0175 0.4181 0.162 Uiso calc R 1 H H28B 0.6375 0.8940 0.4545 0.162 Uiso calc R 1 H C29 0.8377(6) 1.0443(5) 0.5606(4) 0.1297(17) Uani d D 1 C H29A 0.9022 1.0208 0.5226 0.195 Uiso calc R 1 H H29B 0.8312 1.0122 0.6221 0.195 Uiso calc R 1 H H29C 0.8782 1.1357 0.5860 0.195 Uiso calc R 1 H loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 V1 0.0599(3) 0.0470(3) 0.0413(2) 0.0169(2) 0.0237(2) 0.01337(19) O1 0.0553(12) 0.0685(13) 0.0468(10) 0.0156(10) 0.0210(9) 0.0229(9) O2 0.0629(13) 0.0682(13) 0.0475(10) 0.0293(11) 0.0238(10) 0.0126(9) O3 0.0621(12) 0.0456(11) 0.0525(10) 0.0185(9) 0.0329(10) 0.0120(8) O4 0.0604(12) 0.0415(10) 0.0448(9) 0.0147(9) 0.0238(9) 0.0091(8) O5 0.0935(16) 0.0506(12) 0.0569(11) 0.0228(11) 0.0320(12) 0.0167(9) N1 0.0531(14) 0.0482(13) 0.0442(12) 0.0188(11) 0.0178(11) 0.0156(10) N2 0.0641(16) 0.0598(15) 0.0404(12) 0.0260(13) 0.0202(12) 0.0082(10) N3 0.081(2) 0.089(2) 0.075(2) 0.0300(19) -0.0015(18) 0.0150(17) N4 0.0488(13) 0.0411(12) 0.0417(11) 0.0136(10) 0.0203(10) 0.0106(9) C1 0.0620(19) 0.0396(15) 0.0576(16) 0.0194(14) 0.0248(15) 0.0220(12) C2 0.060(2) 0.0507(17) 0.0582(17) 0.0201(15) 0.0127(16) 0.0188(14) C3 0.058(2) 0.0547(19) 0.077(2) 0.0209(16) 0.0086(17) 0.0190(16) C4 0.052(2) 0.069(2) 0.089(2) 0.0258(17) 0.0243(19) 0.0209(18) C5 0.066(2) 0.066(2) 0.071(2) 0.0308(17) 0.0334(18) 0.0182(16) C6 0.0548(18) 0.0472(16) 0.0545(15) 0.0216(14) 0.0226(14) 0.0157(12) C7 0.067(2) 0.0539(17) 0.0510(15) 0.0256(15) 0.0304(16) 0.0174(13) C8 0.0622(19) 0.0483(16) 0.0467(14) 0.0234(14) 0.0228(14) 0.0149(12) C9 0.0604(19) 0.0461(16) 0.0511(15) 0.0226(14) 0.0164(14) 0.0128(12) C10 0.076(2) 0.065(2) 0.0544(17) 0.0300(18) 0.0179(17) 0.0112(15) C11 0.097(3) 0.079(3) 0.0551(19) 0.036(2) 0.009(2) 0.0084(17) C12 0.071(3) 0.124(4) 0.092(3) 0.049(3) 0.013(2) 0.021(3) C13 0.072(2) 0.100(3) 0.065(2) 0.042(2) 0.0142(19) 0.0047(19) C14 0.0458(15) 0.0424(14) 0.0375(12) 0.0165(12) 0.0144(12) 0.0097(11) C15 0.0410(15) 0.0448(15) 0.0474(14) 0.0182(12) 0.0167(12) 0.0152(11) C16 0.0580(18) 0.0511(17) 0.0538(16) 0.0172(15) 0.0180(14) 0.0090(13) C17 0.071(2) 0.0484(19) 0.082(2) 0.0120(17) 0.0178(19) 0.0052(16) C18 0.062(2) 0.0443(18) 0.119(3) 0.0150(16) 0.027(2) 0.0285(19) C19 0.0542(19) 0.063(2) 0.084(2) 0.0296(16) 0.0300(17) 0.0413(17) C20 0.0477(16) 0.0569(17) 0.0522(15) 0.0270(14) 0.0164(13) 0.0235(13) C21 0.0491(16) 0.0427(14) 0.0422(13) 0.0216(13) 0.0208(12) 0.0144(11) C22 0.0517(18) 0.0520(17) 0.0611(17) 0.0224(14) 0.0150(14) 0.0202(13) C23 0.057(2) 0.069(2) 0.109(3) 0.0338(18) 0.044(2) 0.042(2) C24 0.098(3) 0.090(3) 0.096(3) 0.057(2) 0.071(3) 0.041(2) C25 0.106(3) 0.099(3) 0.0536(18) 0.047(2) 0.039(2) 0.0084(17) C26 0.0597(19) 0.074(2) 0.0439(14) 0.0258(16) 0.0174(14) 0.0069(14) C27 0.153(5) 0.120(4) 0.097(3) 0.064(4) 0.054(3) 0.047(3) C28 0.163(5) 0.132(4) 0.150(5) 0.076(4) 0.095(5) 0.065(4) C29 0.112(4) 0.147(5) 0.133(4) 0.053(4) 0.030(4) 0.061(4) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 V1 O2 . . 153.00(10) yes O1 V1 O3 . . 84.40(10) yes O1 V1 O4 . . 104.60(10) yes O1 V1 O5 . . 98.50(10) yes O1 V1 N1 . . 83.40(10) yes O2 V1 O3 . . 79.80(10) yes O2 V1 O4 . . 92.40(10) yes O2 V1 O5 . . 100.20(10) yes O2 V1 N1 . . 74.60(10) yes O3 V1 O4 . . 75.20(10) yes O3 V1 O5 . . 171.80(10) yes O3 V1 N1 . . 89.00(10) yes O4 V1 O5 . . 96.70(10) yes O4 V1 N1 . . 161.20(10) yes O5 V1 N1 . . 98.90(10) yes C1 O1 V1 . . 131.81(18) no C8 O2 V1 . . 118.08(18) no C14 O3 V1 . . 112.42(15) no N4 O4 V1 . . 119.39(13) no C7 N1 N2 . . 117.1(2) no C7 N1 V1 . . 126.8(2) no N2 N1 V1 . . 116.05(16) no C8 N2 N1 . . 109.2(2) no C8 N2 H2n . . 125.4 no N1 N2 H2n . . 125.4 no C12 N3 C11 . . 116.0(3) no C14 N4 O4 . . 115.43(19) no C14 N4 C21 . . 130.3(2) no O4 N4 C21 . . 114.16(18) no O1 C1 C2 . . 120.3(2) no O1 C1 C6 . . 120.2(3) no C2 C1 C6 . . 119.5(3) no C3 C2 C1 . . 120.3(3) no C3 C2 H2 . . 119.8 no C1 C2 H2 . . 119.8 no C2 C3 C4 . . 121.4(3) no C2 C3 H3 . . 119.3 no C4 C3 H3 . . 119.3 no C5 C4 C3 . . 118.8(3) no C5 C4 H4 . . 120.6 no C3 C4 H4 . . 120.6 no C4 C5 C6 . . 121.7(3) no C4 C5 H5 . . 119.2 no C6 C5 H5 . . 119.2 no C1 C6 C5 . . 118.3(3) no C1 C6 C7 . . 121.1(3) no C5 C6 C7 . . 120.6(3) no N1 C7 C6 . . 124.8(2) no N1 C7 H7 . . 117.6 no C6 C7 H7 . . 117.6 no N2 C8 O2 . . 121.9(3) no N2 C8 C9 . . 120.1(2) no O2 C8 C9 . . 118.0(2) no C10 C9 C13 . . 117.2(3) no C10 C9 C8 . . 122.2(3) no C13 C9 C8 . . 120.6(3) no C9 C10 C11 . . 118.8(3) no C9 C10 H10 . . 120.6 no C11 C10 H10 . . 120.6 no N3 C11 C10 . . 124.7(3) no N3 C11 H11 . . 117.7 no C10 C11 H11 . . 117.7 no N3 C12 C13 . . 123.9(4) no N3 C12 H12 . . 118.1 no C13 C12 H12 . . 118.1 no C9 C13 C12 . . 119.4(3) no C9 C13 H13 . . 120.3 no C12 C13 H13 . . 120.3 no O3 C14 N4 . . 116.2(2) no O3 C14 C15 . . 121.7(2) no N4 C14 C15 . . 122.1(2) no C16 C15 C20 . . 118.9(3) no C16 C15 C14 . . 116.6(2) no C20 C15 C14 . . 124.4(2) no C17 C16 C15 . . 120.0(3) no C17 C16 H16 . . 120.0 no C15 C16 H16 . . 120.0 no C18 C17 C16 . . 120.8(3) no C18 C17 H17 . . 119.6 no C16 C17 H17 . . 119.6 no C17 C18 C19 . . 119.8(3) no C17 C18 H18 . . 120.1 no C19 C18 H18 . . 120.1 no C20 C19 C18 . . 120.1(3) no C20 C19 H19 . . 119.9 no C18 C19 H19 . . 119.9 no C19 C20 C15 . . 120.3(3) no C19 C20 H20 . . 119.8 no C15 C20 H20 . . 119.8 no C26 C21 C22 . . 122.1(2) no C26 C21 N4 . . 117.5(2) no C22 C21 N4 . . 120.3(2) no C21 C22 C23 . . 118.3(3) no C21 C22 H22 . . 120.8 no C23 C22 H22 . . 120.8 no C24 C23 C22 . . 120.7(3) no C24 C23 H23 . . 119.7 no C22 C23 H23 . . 119.7 no C23 C24 C25 . . 120.1(3) no C23 C24 H24 . . 120.0 no C25 C24 H24 . . 120.0 no C24 C25 C26 . . 120.9(3) no C24 C25 H25 . . 119.5 no C26 C25 H25 . . 119.5 no C21 C26 C25 . . 117.8(3) no C21 C26 H26 . . 121.1 no C25 C26 H26 . . 121.1 no C28 C27 C27 . 2_676 113.8(5) no C28 C27 H27A . . 108.8 no C27 C27 H27A 2_676 . 108.8 no C28 C27 H27B . . 108.8 no C27 C27 H27B 2_676 . 108.8 no H27A C27 H27B . . 107.7 no C27 C28 C29 . . 110.3(4) no C27 C28 H28A . . 109.6 no C29 C28 H28A . . 109.6 no C27 C28 H28B . . 109.6 no C29 C28 H28B . . 109.6 no H28A C28 H28B . . 108.1 no C28 C29 H29A . . 109.5 no C28 C29 H29B . . 109.5 no H29A C29 H29B . . 109.5 no C28 C29 H29C . . 109.5 no H29A C29 H29C . . 109.5 no H29B C29 H29C . . 109.5 no loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag V1 O1 . 1.858(2) yes V1 O2 . 1.947(2) yes V1 O3 . 2.192(2) yes V1 O4 . 1.863(2) yes V1 O5 . 1.582(2) yes V1 N1 . 2.081(2) no O1 C1 . 1.337(3) no O2 C8 . 1.301(3) no O3 C14 . 1.248(3) no O4 N4 . 1.374(3) no N1 C7 . 1.290(3) no N1 N2 . 1.388(3) no N2 C8 . 1.290(3) no N2 H2n . 0.8600 no N3 C12 . 1.316(5) no N3 C11 . 1.319(4) no N4 C14 . 1.343(3) no N4 C21 . 1.436(3) no C1 C2 . 1.391(4) no C1 C6 . 1.402(4) no C2 C3 . 1.372(4) no C2 H2 . 0.9300 no C3 C4 . 1.378(5) no C3 H3 . 0.9300 no C4 C5 . 1.370(5) no C4 H4 . 0.9300 no C5 C6 . 1.408(4) no C5 H5 . 0.9300 no C6 C7 . 1.426(4) no C7 H7 . 0.9300 no C8 C9 . 1.467(4) no C9 C10 . 1.372(4) no C9 C13 . 1.375(4) no C10 C11 . 1.378(5) no C10 H10 . 0.9300 no C11 H11 . 0.9300 no C12 C13 . 1.380(5) no C12 H12 . 0.9300 no C13 H13 . 0.9300 no C14 C15 . 1.478(4) no C15 C16 . 1.387(4) no C15 C20 . 1.391(3) no C16 C17 . 1.371(4) no C16 H16 . 0.9300 no C17 C18 . 1.367(5) no C17 H17 . 0.9300 no C18 C19 . 1.376(5) no C18 H18 . 0.9300 no C19 C20 . 1.372(4) no C19 H19 . 0.9300 no C20 H20 . 0.9300 no C21 C26 . 1.373(4) no C21 C22 . 1.372(4) no C22 C23 . 1.379(4) no C22 H22 . 0.9300 no C23 C24 . 1.363(5) no C23 H23 . 0.9300 no C24 C25 . 1.364(5) no C24 H24 . 0.9300 no C25 C26 . 1.383(4) no C25 H25 . 0.9300 no C26 H26 . 0.9300 no C27 C28 . 1.470(5) no C27 C27 2_676 1.530(7) no C27 H27A . 0.9700 no C27 H27B . 0.9700 no C28 C29 . 1.558(6) no C28 H28A . 0.9700 no C28 H28B . 0.9700 no C29 H29A . 0.9600 no C29 H29B . 0.9600 no C29 H29C . 0.9600 no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion_site_symmetry_1 _geom_torsion _geom_torsion_publ_flag O5 V1 O1 C1 . -58.1(2) no O4 V1 O1 C1 . -157.4(2) no O2 V1 O1 C1 . 75.3(3) no N1 V1 O1 C1 . 39.9(2) no O3 V1 O1 C1 . 129.5(2) no O5 V1 O2 C8 . 99.0(2) no O1 V1 O2 C8 . -34.1(3) no O4 V1 O2 C8 . -163.78(19) no N1 V1 O2 C8 . 2.48(19) no O3 V1 O2 C8 . -89.3(2) no O5 V1 O3 C14 . 5.0(8) no O1 V1 O3 C14 . 116.36(19) no O4 V1 O3 C14 . 9.58(18) no O2 V1 O3 C14 . -85.63(18) no N1 V1 O3 C14 . -160.17(19) no O5 V1 O4 N4 . 168.68(18) no O1 V1 O4 N4 . -90.66(18) no O2 V1 O4 N4 . 68.16(18) no N1 V1 O4 N4 . 22.9(4) no O3 V1 O4 N4 . -10.67(16) no O5 V1 N1 C7 . 76.3(2) no O1 V1 N1 C7 . -21.4(2) no O4 V1 N1 C7 . -138.1(3) no O2 V1 N1 C7 . 174.4(2) no O3 V1 N1 C7 . -105.8(2) no O5 V1 N1 N2 . -101.13(19) no O1 V1 N1 N2 . 161.23(18) no O4 V1 N1 N2 . 44.5(4) no O2 V1 N1 N2 . -2.96(17) no O3 V1 N1 N2 . 76.76(18) no C7 N1 N2 C8 . -174.7(2) no V1 N1 N2 C8 . 2.9(3) no V1 O4 N4 C14 . 11.2(3) no V1 O4 N4 C21 . -171.62(16) no V1 O1 C1 C2 . 145.2(2) no V1 O1 C1 C6 . -37.8(4) no O1 C1 C2 C3 . 175.5(3) no C6 C1 C2 C3 . -1.5(4) no C1 C2 C3 C4 . -0.2(4) no C2 C3 C4 C5 . 1.0(5) no C3 C4 C5 C6 . 0.0(5) no O1 C1 C6 C5 . -174.6(3) no C2 C1 C6 C5 . 2.3(4) no O1 C1 C6 C7 . 3.0(4) no C2 C1 C6 C7 . 180.0(3) no C4 C5 C6 C1 . -1.6(4) no C4 C5 C6 C7 . -179.3(3) no N2 N1 C7 C6 . -179.7(3) no V1 N1 C7 C6 . 2.9(4) no C1 C6 C7 N1 . 11.7(4) no C5 C6 C7 N1 . -170.7(3) no N1 N2 C8 O2 . -0.9(4) no N1 N2 C8 C9 . 178.4(2) no V1 O2 C8 N2 . -1.8(4) no V1 O2 C8 C9 . 178.95(18) no N2 C8 C9 C10 . 3.4(4) no O2 C8 C9 C10 . -177.4(3) no N2 C8 C9 C13 . -176.5(3) no O2 C8 C9 C13 . 2.8(4) no C13 C9 C10 C11 . 0.8(5) no C8 C9 C10 C11 . -179.1(3) no C12 N3 C11 C10 . -1.5(6) no C9 C10 C11 N3 . 0.8(6) no C11 N3 C12 C13 . 0.7(6) no C10 C9 C13 C12 . -1.5(5) no C8 C9 C13 C12 . 178.4(3) no N3 C12 C13 C9 . 0.8(7) no V1 O3 C14 N4 . -6.6(3) no V1 O3 C14 C15 . 171.22(19) no O4 N4 C14 O3 . -1.7(3) no C21 N4 C14 O3 . -178.3(2) no O4 N4 C14 C15 . -179.5(2) no C21 N4 C14 C15 . 3.8(4) no O3 C14 C15 C16 . -34.2(4) no N4 C14 C15 C16 . 143.6(3) no O3 C14 C15 C20 . 142.3(3) no N4 C14 C15 C20 . -40.0(4) no C20 C15 C16 C17 . 1.5(4) no C14 C15 C16 C17 . 178.2(3) no C15 C16 C17 C18 . -0.8(5) no C16 C17 C18 C19 . -0.5(5) no C17 C18 C19 C20 . 1.0(5) no C18 C19 C20 C15 . -0.3(4) no C16 C15 C20 C19 . -1.0(4) no C14 C15 C20 C19 . -177.3(2) no C14 N4 C21 C26 . 115.4(3) no O4 N4 C21 C26 . -61.3(3) no C14 N4 C21 C22 . -65.0(4) no O4 N4 C21 C22 . 118.3(3) no C26 C21 C22 C23 . -1.4(4) no N4 C21 C22 C23 . 179.0(2) no C21 C22 C23 C24 . 1.0(5) no C22 C23 C24 C25 . 0.6(5) no C23 C24 C25 C26 . -1.9(6) no C22 C21 C26 C25 . 0.1(5) no N4 C21 C26 C25 . 179.7(3) no C24 C25 C26 C21 . 1.6(5) no C27 C27 C28 C29 2_676 175.0(5) no