Supplementary Material (ESI) for Chemical Communications This journal is © The Royal Society of Chemistry 2001 data_global #====================================================================== _journal_coden_Cambridge 182 # 1. SUBMISSION DETAILS _publ_contact_author # Name and address of author for correspondence ; Dieter Rehder Institut f\"ur Anorganische und Angewandte Chemie Universit\"at Hamburg Martin-Luther-King-Platz 6 D-20146 Hamburg Bundesrepublik Deutschland ; _publ_contact_author_phone '0049 40 42838 6087' _publ_contact_author_fax '0049 40 42838 2893' _publ_contact_author_email 'rehder@xray.chemie.uni-hamburg.de' _publ_requested_journal 'J.Chem. Soc., Chem. Commun.' _publ_requested_coeditor_name ? _publ_contact_letter ; ? ; #====================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Towards hydroperoxovanadium complexes: A peroxovanadium(V) complex containing a V(O2)(RCO2H)(H2O)2 cluster with hydrogen-bond inter-linkages ; loop_ _publ_author_name _publ_author_address 'Casny, Marian' ; Institut f\"ur Anorganische und Angewandte Chemie der Universit\"at Hamburg Martin-Luther-King-Platz 6 D-20146 Hamburg Bundesrepublik Deutschland ; 'Rehder, Dieter' ; Institut f\"ur Anorganische und Angewandte Chemie der Universit\"at Hamburg Martin-Luther-King-Platz 6 D-20146 Hamburg Bundesrepublik Deutschland ; #====================================================================== # 4. TEXT _publ_section_abstract ; The molecular structure of the oxo-peroxovanadium complex [VO(O2)bpaH]ClO4.2H2O, containing the new ligand N,N-bis(2-pyridylmethyl)-beta-alanine (bpaH) reveals an unusually tight binding of the carboxylic acid moiety through the doubly bonded oxygen. The carboxylic acid proton promotes a tight hydrogen bonded cluster involving the peroxo group and the two waters of crystallisation, thus providing the basis for the formation of a hydroperoxo species. ; _publ_section_comment ; ; _publ_section_experimental ; ; _publ_section_references ; ; _publ_section_figure_captions ; ; _publ_section_acknowledgements ; ; #========================================================================== data_m3arian _database_code_CSD 157361 _audit_creation_method SHELXL-97 _chemical_name_systematic ; N,N-bis(2-pyridylmethyl)-beta-alanine-oxo-peroxovanadium perchlorate dihydrate ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C15 H21 Cl N3 O11 V' _chemical_formula_weight 505.74 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'V' 'V' 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting 'Monoclinic' _symmetry_space_group_name_H-M 'C2/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.612(7) _cell_length_b 7.1835(17) _cell_length_c 21.290(5) _cell_angle_alpha 90.00 _cell_angle_beta 123.274(4) _cell_angle_gamma 90.00 _cell_volume 4042.1(16) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4382 _cell_measurement_theta_min 1.54 _cell_measurement_theta_max 27.00 _exptl_crystal_description 'plate' _exptl_crystal_colour 'orange' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2080 _exptl_absorpt_coefficient_mu 0.689 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.8745 _exptl_absorpt_correction_T_max 0.9343 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11777 _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_sigmaI/netI 0.0376 _diffrn_reflns_limit_h_min -31 _diffrn_reflns_limit_h_max 40 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 27.00 _reflns_number_total 4382 _reflns_number_gt 3378 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0588P)^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 4382 _refine_ls_number_parameters 298 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0553 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.1079 _refine_ls_wR_factor_gt 0.1005 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.995 _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 V1 V 0.162162(14) 0.76322(5) 0.26305(2) 0.03055(12) Uani 1 1 d . . . O1 O 0.16908(6) 0.9060(2) 0.19556(9) 0.0424(4) Uani 1 1 d . . . O2 O 0.21673(6) 0.8641(2) 0.26196(9) 0.0422(4) Uani 1 1 d . . . O3 O 0.15116(6) 0.9177(2) 0.30563(9) 0.0402(4) Uani 1 1 d . . . O4 O 0.17042(6) 0.5240(2) 0.20536(8) 0.0355(4) Uani 1 1 d . . . O5 O 0.12835(7) 0.3431(3) 0.10547(10) 0.0493(5) Uani 1 1 d D . . H5 H 0.1402(12) 0.416(4) 0.0894(18) 0.079(5) Uiso 1 1 d D . . C1 C 0.13933(9) 0.4010(3) 0.17074(13) 0.0339(5) Uani 1 1 d . . . C2 C 0.11116(9) 0.3062(3) 0.19911(13) 0.0373(5) Uani 1 1 d . . . H2A H 0.1135 0.1727 0.1951 0.038(2) Uiso 1 1 calc R . . H2B H 0.0757 0.3404 0.1676 0.038(2) Uiso 1 1 calc R . . C3 C 0.13068(9) 0.3546(3) 0.27971(13) 0.0361(5) Uani 1 1 d . . . H3A H 0.1123 0.2803 0.2952 0.038(2) Uiso 1 1 calc R . . H3B H 0.1660 0.3181 0.3108 0.038(2) Uiso 1 1 calc R . . C4 C 0.15378(9) 0.5751(3) 0.37855(12) 0.0389(5) Uani 1 1 d . . . H4A H 0.1446 0.4738 0.3990 0.038(2) Uiso 1 1 calc R . . H4B H 0.1447 0.6916 0.3912 0.038(2) Uiso 1 1 calc R . . C5 C 0.20928(9) 0.5707(3) 0.41057(13) 0.0378(5) Uani 1 1 d . . . C6 C 0.27127(9) 0.6407(3) 0.38807(15) 0.0439(6) Uani 1 1 d . . . H6 H 0.2803 0.6871 0.3562 0.056(3) Uiso 1 1 calc R . . C7 C 0.30838(10) 0.5738(4) 0.45698(16) 0.0530(7) Uani 1 1 d . . . H7 H 0.3420 0.5751 0.4717 0.056(3) Uiso 1 1 calc R . . C8 C 0.29510(11) 0.5043(4) 0.50419(15) 0.0534(7) Uani 1 1 d . . . H8 H 0.3198 0.4595 0.5515 0.056(3) Uiso 1 1 calc R . . C9 C 0.24518(11) 0.5018(4) 0.48075(14) 0.0477(6) Uani 1 1 d . . . H9A H 0.2356 0.4543 0.5118 0.056(3) Uiso 1 1 calc R . . C10 C 0.07271(9) 0.6134(3) 0.25953(14) 0.0388(5) Uani 1 1 d . . . H10A H 0.0532 0.5105 0.2603 0.038(2) Uiso 1 1 calc R . . H10B H 0.0705 0.7164 0.2871 0.038(2) Uiso 1 1 calc R . . C11 C 0.05191(9) 0.6707(3) 0.18033(14) 0.0367(5) Uani 1 1 d . . . C12 C 0.07010(10) 0.7991(4) 0.09841(14) 0.0439(6) Uani 1 1 d . . . H12 H 0.0933 0.8512 0.0897 0.056(3) Uiso 1 1 calc R . . C13 C 0.02113(11) 0.7783(4) 0.03948(15) 0.0548(7) Uani 1 1 d . . . H13 H 0.0113 0.8147 -0.0086 0.056(3) Uiso 1 1 calc R . . C14 C -0.01328(11) 0.7034(4) 0.05208(17) 0.0606(8) Uani 1 1 d . . . H14 H -0.0469 0.6903 0.0127 0.056(3) Uiso 1 1 calc R . . C15 C 0.00215(10) 0.6476(4) 0.12312(16) 0.0504(7) Uani 1 1 d . . . H15 H -0.0208 0.5949 0.1324 0.056(3) Uiso 1 1 calc R . . N1 N 0.08593(7) 0.7467(2) 0.16873(11) 0.0344(4) Uani 1 1 d . . . N2 N 0.12671(7) 0.5561(2) 0.29564(10) 0.0313(4) Uani 1 1 d . . . N3 N 0.22231(7) 0.6419(2) 0.36487(10) 0.0349(4) Uani 1 1 d . . . Cl1 Cl -0.05371(3) 0.13424(9) 0.11631(4) 0.04852(18) Uani 1 1 d . . . O6 O -0.08243(10) 0.1364(5) 0.03699(14) 0.1201(12) Uani 1 1 d . . . O7 O -0.06884(11) -0.0188(4) 0.13948(18) 0.1137(10) Uani 1 1 d . . . O8 O -0.06439(14) 0.2978(4) 0.1398(2) 0.1418(15) Uani 1 1 d . . . O9 O -0.00234(8) 0.1288(4) 0.14103(13) 0.0833(7) Uani 1 1 d . . . O10 O 0.24662(8) 0.7040(3) 0.16183(12) 0.0579(5) Uani 1 1 d D . . H10C H 0.2365(11) 0.760(3) 0.1847(13) 0.079(5) Uiso 1 1 d D . . H10D H 0.2605(11) 0.610(3) 0.1869(14) 0.079(5) Uiso 1 1 d D . . O11 O 0.15912(9) 0.5622(3) 0.04439(12) 0.0649(6) Uani 1 1 d D . . H11A H 0.1370(7) 0.641(3) 0.0226(15) 0.079(5) Uiso 1 1 d D . . H11B H 0.1845(6) 0.620(3) 0.0756(14) 0.079(5) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0351(2) 0.0268(2) 0.0326(2) -0.00053(15) 0.02041(18) -0.00196(15) O1 0.0484(11) 0.0405(9) 0.0447(10) 0.0074(7) 0.0295(9) -0.0021(8) O2 0.0411(10) 0.0418(9) 0.0471(10) 0.0002(8) 0.0264(9) -0.0084(7) O3 0.0504(10) 0.0316(8) 0.0433(10) -0.0023(7) 0.0288(8) 0.0006(7) O4 0.0343(9) 0.0377(9) 0.0381(9) -0.0053(7) 0.0222(8) -0.0025(7) O5 0.0533(12) 0.0564(12) 0.0371(10) -0.0105(9) 0.0240(9) -0.0036(9) C1 0.0325(12) 0.0318(12) 0.0339(12) -0.0002(9) 0.0160(10) 0.0085(10) C2 0.0365(13) 0.0291(11) 0.0455(14) -0.0055(10) 0.0219(12) -0.0008(10) C3 0.0420(14) 0.0288(11) 0.0432(13) 0.0024(10) 0.0269(12) 0.0001(10) C4 0.0492(15) 0.0409(13) 0.0326(12) 0.0007(10) 0.0264(12) -0.0025(11) C5 0.0475(15) 0.0323(12) 0.0330(12) -0.0038(9) 0.0217(11) -0.0026(10) C6 0.0381(15) 0.0437(14) 0.0451(15) -0.0021(11) 0.0197(12) -0.0036(11) C7 0.0372(15) 0.0482(16) 0.0554(17) -0.0045(13) 0.0139(13) -0.0019(12) C8 0.0526(18) 0.0450(15) 0.0366(14) -0.0007(12) 0.0079(13) 0.0046(12) C9 0.0605(18) 0.0419(14) 0.0363(14) -0.0003(11) 0.0237(13) -0.0007(12) C10 0.0380(13) 0.0395(13) 0.0470(14) 0.0024(11) 0.0284(12) 0.0034(10) C11 0.0359(13) 0.0316(11) 0.0457(14) -0.0004(10) 0.0244(12) 0.0057(10) C12 0.0485(16) 0.0455(14) 0.0369(14) 0.0035(11) 0.0230(12) 0.0070(12) C13 0.0546(18) 0.0621(18) 0.0370(15) 0.0040(12) 0.0185(14) 0.0131(14) C14 0.0383(16) 0.072(2) 0.0497(17) -0.0043(14) 0.0104(14) 0.0067(14) C15 0.0351(15) 0.0542(16) 0.0596(18) -0.0026(13) 0.0243(14) 0.0007(12) N1 0.0355(11) 0.0329(10) 0.0348(10) 0.0019(8) 0.0192(9) 0.0052(8) N2 0.0350(10) 0.0301(9) 0.0333(10) 0.0010(8) 0.0216(9) 0.0013(8) N3 0.0375(11) 0.0314(10) 0.0331(10) -0.0033(8) 0.0176(9) -0.0040(8) Cl1 0.0499(4) 0.0504(4) 0.0557(4) 0.0017(3) 0.0356(3) 0.0019(3) O6 0.0742(19) 0.217(4) 0.0582(16) -0.0007(19) 0.0294(15) -0.025(2) O7 0.109(2) 0.096(2) 0.156(3) 0.0503(19) 0.085(2) -0.0012(17) O8 0.179(4) 0.087(2) 0.243(5) -0.040(2) 0.169(4) 0.002(2) O9 0.0480(14) 0.109(2) 0.0870(18) 0.0019(14) 0.0337(13) 0.0014(13) O10 0.0629(14) 0.0486(12) 0.0760(14) 0.0164(10) 0.0469(12) 0.0110(10) O11 0.0715(15) 0.0760(14) 0.0527(13) 0.0087(11) 0.0376(12) 0.0094(12) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O3 1.5877(15) . y V1 O1 1.8734(16) . y V1 O2 1.8827(16) . y V1 N1 2.132(2) . y V1 N3 2.133(2) . y V1 N2 2.1919(18) . y V1 O4 2.2095(16) . y O1 O2 1.422(2) . y O4 C1 1.222(3) . y O5 C1 1.302(3) . y O5 H5 0.820 . y C1 C2 1.487(3) . y C2 C3 1.511(3) . y C2 H2A 0.9700 . y C2 H2B 0.9700 . y C3 N2 1.508(3) . y C3 H3A 0.9700 . y C3 H3B 0.9700 . y C4 N2 1.486(3) . y C4 C5 1.494(3) . y C4 H4A 0.9700 . y C4 H4B 0.9700 . y C5 N3 1.348(3) . y C5 C9 1.380(3) . y C6 N3 1.342(3) . y C6 C7 1.368(4) . y C6 H6 0.9300 . y C7 C8 1.378(4) . y C7 H7 0.9300 . y C8 C9 1.370(4) . y C8 H8 0.9300 . y C9 H9A 0.9300 . y C10 C11 1.493(3) . y C10 N2 1.495(3) . y C10 H10A 0.9700 . y C10 H10B 0.9700 . y C11 N1 1.344(3) . y C11 C15 1.372(3) . y C12 N1 1.346(3) . y C12 C13 1.364(4) . y C12 H12 0.9300 . y C13 C14 1.366(4) . y C13 H13 0.9300 . y C14 C15 1.370(4) . y C14 H14 0.9300 . y C15 H15 0.9300 . y Cl1 O8 1.390(3) . y Cl1 O7 1.393(2) . y Cl1 O9 1.406(2) . y Cl1 O6 1.412(3) . y O10 H10C 0.8200 . y O10 H10D 0.8200 . y O11 H11A 0.8200 . y O11 H11B 0.8200 . y loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 V1 O1 102.10(8) . . y O3 V1 O2 103.14(8) . . y O1 V1 O2 44.48(7) . . y O3 V1 N1 95.06(8) . . y O1 V1 N1 81.68(8) . . y O2 V1 N1 125.43(8) . . y O3 V1 N3 93.31(8) . . y O1 V1 N3 126.09(8) . . y O2 V1 N3 81.83(8) . . y N1 V1 N3 148.34(7) . . y O3 V1 N2 89.06(8) . . y O1 V1 N2 155.44(8) . . y O2 V1 N2 153.66(7) . . y N1 V1 N2 75.53(7) . . y N3 V1 N2 74.13(7) . . y O3 V1 O4 172.25(7) . . y O1 V1 O4 84.28(7) . . y O2 V1 O4 84.49(7) . . y N1 V1 O4 81.39(6) . . y N3 V1 O4 86.32(7) . . y N2 V1 O4 83.39(6) . . y O2 O1 V1 68.11(9) . . y O1 O2 V1 67.41(9) . . y C1 O4 V1 126.58(14) . . y C1 O5 H5 109(2) . . y O4 C1 O5 122.0(2) . . y O4 C1 C2 123.3(2) . . y O5 C1 C2 114.8(2) . . y C1 C2 C3 113.18(19) . . y C1 C2 H2A 108.9 . . y C3 C2 H2A 108.9 . . y C1 C2 H2B 108.9 . . y C3 C2 H2B 108.9 . . y H2A C2 H2B 107.8 . . y N2 C3 C2 116.33(18) . . y N2 C3 H3A 108.2 . . y C2 C3 H3A 108.2 . . y N2 C3 H3B 108.2 . . y C2 C3 H3B 108.2 . . y H3A C3 H3B 107.4 . . y N2 C4 C5 107.87(17) . . y N2 C4 H4A 110.1 . . y C5 C4 H4A 110.1 . . y N2 C4 H4B 110.1 . . y C5 C4 H4B 110.1 . . y H4A C4 H4B 108.4 . . y N3 C5 C9 121.5(2) . . y N3 C5 C4 114.2(2) . . y C9 C5 C4 124.3(2) . . y N3 C6 C7 122.3(2) . . y N3 C6 H6 118.9 . . y C7 C6 H6 118.9 . . y C6 C7 C8 119.0(3) . . y C6 C7 H7 120.5 . . y C8 C7 H7 120.5 . . y C9 C8 C7 119.4(3) . . y C9 C8 H8 120.3 . . y C7 C8 H8 120.3 . . y C8 C9 C5 119.2(2) . . y C8 C9 H9A 120.4 . . y C5 C9 H9A 120.4 . . y C11 C10 N2 109.14(18) . . y C11 C10 H10A 109.9 . . y N2 C10 H10A 109.9 . . y C11 C10 H10B 109.9 . . y N2 C10 H10B 109.9 . . y H10A C10 H10B 108.3 . . y N1 C11 C15 121.9(2) . . y N1 C11 C10 114.7(2) . . y C15 C11 C10 123.3(2) . . y N1 C12 C13 122.3(3) . . y N1 C12 H12 118.9 . . y C13 C12 H12 118.9 . . y C12 C13 C14 119.1(3) . . y C12 C13 H13 120.4 . . y C14 C13 H13 120.4 . . y C13 C14 C15 119.5(3) . . y C13 C14 H14 120.2 . . y C15 C14 H14 120.2 . . y C14 C15 C11 119.0(3) . . y C14 C15 H15 120.5 . . y C11 C15 H15 120.5 . . y C11 N1 C12 118.1(2) . . y C11 N1 V1 117.03(15) . . y C12 N1 V1 124.79(17) . . y C4 N2 C10 109.66(17) . . y C4 N2 C3 106.90(17) . . y C10 N2 C3 111.19(18) . . y C4 N2 V1 104.60(13) . . y C10 N2 V1 106.74(13) . . y C3 N2 V1 117.42(13) . . y C6 N3 C5 118.7(2) . . y C6 N3 V1 125.56(16) . . y C5 N3 V1 115.68(16) . . y O8 Cl1 O7 110.0(2) . . y O8 Cl1 O9 110.35(19) . . y O7 Cl1 O9 113.32(16) . . y O8 Cl1 O6 107.3(2) . . y O7 Cl1 O6 108.2(2) . . y O9 Cl1 O6 107.50(15) . . y H10C O10 H10D 104.9 . . y H11A O11 H11B 104.9 . . y loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 V1 O1 O2 96.51(11) . . . . y N1 V1 O1 O2 -170.06(11) . . . . y N3 V1 O1 O2 -6.75(13) . . . . y N2 V1 O1 O2 -148.09(16) . . . . y O4 V1 O1 O2 -87.96(10) . . . . y O3 V1 O2 O1 -93.99(11) . . . . y N1 V1 O2 O1 12.10(13) . . . . y N3 V1 O2 O1 174.49(11) . . . . y N2 V1 O2 O1 150.33(15) . . . . y O4 V1 O2 O1 87.43(10) . . . . y O3 V1 O4 C1 26.7(3) . . . . y O1 V1 O4 C1 -118.91(19) . . . . y O2 V1 O4 C1 -163.61(19) . . . . y N1 V1 O4 C1 -36.48(18) . . . . y N3 V1 O4 C1 114.25(19) . . . . y N2 V1 O4 C1 39.82(18) . . . . y V1 O4 C1 O5 135.11(19) . . . . y V1 O4 C1 C2 -44.8(3) . . . . y O4 C1 C2 C3 -9.2(3) . . . . y O5 C1 C2 C3 170.8(2) . . . . y C1 C2 C3 N2 62.5(3) . . . . y N2 C4 C5 N3 31.1(3) . . . . y N2 C4 C5 C9 -149.2(2) . . . . y N3 C6 C7 C8 0.3(4) . . . . y C6 C7 C8 C9 0.8(4) . . . . y C7 C8 C9 C5 -0.6(4) . . . . y N3 C5 C9 C8 -0.6(4) . . . . y C4 C5 C9 C8 179.8(2) . . . . y N2 C10 C11 N1 -31.2(3) . . . . y N2 C10 C11 C15 148.4(2) . . . . y N1 C12 C13 C14 0.6(4) . . . . y C12 C13 C14 C15 -1.2(4) . . . . y C13 C14 C15 C11 0.8(4) . . . . y N1 C11 C15 C14 0.1(4) . . . . y C10 C11 C15 C14 -179.5(2) . . . . y C15 C11 N1 C12 -0.7(3) . . . . y C10 C11 N1 C12 179.0(2) . . . . y C15 C11 N1 V1 -177.85(18) . . . . y C10 C11 N1 V1 1.8(2) . . . . y C13 C12 N1 C11 0.3(3) . . . . y C13 C12 N1 V1 177.26(19) . . . . y O3 V1 N1 C11 -69.62(16) . . . . y O1 V1 N1 C11 -171.14(16) . . . . y O2 V1 N1 C11 -179.68(14) . . . . y N3 V1 N1 C11 35.1(2) . . . . y N2 V1 N1 C11 18.10(15) . . . . y O4 V1 N1 C11 103.44(16) . . . . y O3 V1 N1 C12 113.41(19) . . . . y O1 V1 N1 C12 11.89(18) . . . . y O2 V1 N1 C12 3.4(2) . . . . y N3 V1 N1 C12 -141.87(18) . . . . y N2 V1 N1 C12 -158.87(19) . . . . y O4 V1 N1 C12 -73.53(18) . . . . y C5 C4 N2 C10 -163.90(18) . . . . y C5 C4 N2 C3 75.5(2) . . . . y C5 C4 N2 V1 -49.74(19) . . . . y C11 C10 N2 C4 156.47(18) . . . . y C11 C10 N2 C3 -85.5(2) . . . . y C11 C10 N2 V1 43.7(2) . . . . y C2 C3 N2 C4 -172.89(19) . . . . y C2 C3 N2 C10 67.5(2) . . . . y C2 C3 N2 V1 -55.9(2) . . . . y O3 V1 N2 C4 -53.58(14) . . . . y O1 V1 N2 C4 -171.52(16) . . . . y O2 V1 N2 C4 65.0(2) . . . . y N1 V1 N2 C4 -149.05(14) . . . . y N3 V1 N2 C4 40.13(13) . . . . y O4 V1 N2 C4 128.17(14) . . . . y O3 V1 N2 C10 62.61(15) . . . . y O1 V1 N2 C10 -55.3(2) . . . . y O2 V1 N2 C10 -178.76(15) . . . . y N1 V1 N2 C10 -32.86(13) . . . . y N3 V1 N2 C10 156.33(15) . . . . y O4 V1 N2 C10 -115.63(14) . . . . y O3 V1 N2 C3 -171.84(16) . . . . y O1 V1 N2 C3 70.2(2) . . . . y O2 V1 N2 C3 -53.2(2) . . . . y N1 V1 N2 C3 92.69(16) . . . . y N3 V1 N2 C3 -78.13(16) . . . . y O4 V1 N2 C3 9.91(15) . . . . y C7 C6 N3 C5 -1.5(3) . . . . y C7 C6 N3 V1 174.49(19) . . . . y C9 C5 N3 C6 1.6(3) . . . . y C4 C5 N3 C6 -178.7(2) . . . . y C9 C5 N3 V1 -174.71(18) . . . . y C4 C5 N3 V1 5.0(2) . . . . y O3 V1 N3 C6 -113.99(19) . . . . y O1 V1 N3 C6 -6.4(2) . . . . y O2 V1 N3 C6 -11.19(19) . . . . y N1 V1 N3 C6 140.81(19) . . . . y N2 V1 N3 C6 157.9(2) . . . . y O4 V1 N3 C6 73.77(18) . . . . y O3 V1 N3 C5 62.06(16) . . . . y O1 V1 N3 C5 169.64(14) . . . . y O2 V1 N3 C5 164.87(16) . . . . y N1 V1 N3 C5 -43.1(2) . . . . y N2 V1 N3 C5 -26.01(15) . . . . y O4 V1 N3 C5 -110.18(16) . . . . y _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.548 _refine_diff_density_min -0.314 _refine_diff_density_rms 0.059 #============================================================================= #eof #End of Crystallographic Information File