# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Nadia Marino' _publ_contact_author_email nmarino@syr.edu loop_ _publ_author_name N.Marino F.Lloret M.Julve T.M.Korter R.P.Doyle data_1 _database_code_depnum_ccdc_archive 'CCDC 825039' #TrackingRef '- 1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H44 N8 O16 V6, 2(C H4 O), 4(H2 O)' _chemical_formula_sum 'C54 H60 N8 O22 V6' _chemical_formula_weight 1478.74 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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M P2(1)/C 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 9.5771(10) _cell_length_b 22.075(2) _cell_length_c 13.9276(15) _cell_angle_alpha 90.00 _cell_angle_beta 97.924(2) _cell_angle_gamma 90.00 _cell_volume 2916.4(5) _cell_formula_units_Z 2 _cell_measurement_temperature 98(2) _cell_measurement_reflns_used 8561 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 28.28 _exptl_crystal_description PARALLELEPIPED _exptl_crystal_colour BROWN _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.684 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1508 _exptl_absorpt_coefficient_mu 1.010 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.855 _exptl_absorpt_correction_T_max 0.960 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 98(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 18499 _diffrn_reflns_av_R_equivalents 0.0228 _diffrn_reflns_av_sigmaI/netI 0.0229 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.74 _diffrn_reflns_theta_max 26.38 _reflns_number_total 5923 _reflns_number_gt 5159 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0460P)^2^+2.0729P] 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 5923 _refine_ls_number_parameters 422 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0368 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0864 _refine_ls_wR_factor_gt 0.0822 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.51951(4) 0.572441(15) 0.21746(2) 0.01580(9) Uani 1 1 d . . . V2 V 0.67869(3) 0.491163(14) 0.37889(2) 0.01426(9) Uani 1 1 d . . . V3 V 0.33465(3) 0.562986(14) 0.38422(2) 0.01444(9) Uani 1 1 d . . . O1 O 0.50689(14) 0.53796(6) 0.34655(9) 0.0154(3) Uani 1 1 d . . . O2 O 0.60823(16) 0.63486(7) 0.21022(11) 0.0242(3) Uani 1 1 d . . . O3 O 0.46226(16) 0.54774(7) 0.10742(11) 0.0251(3) Uani 1 1 d . . . O7 O 0.67550(16) 0.51365(7) 0.23976(10) 0.0221(3) Uani 1 1 d . . . C25 C 0.7746(3) 0.50444(12) 0.17547(17) 0.0328(6) Uani 1 1 d . . . H25A H 0.8365 0.5399 0.1767 0.049 Uiso 1 1 calc R . . H25B H 0.7252 0.4986 0.1097 0.049 Uiso 1 1 calc R . . H25C H 0.8311 0.4684 0.1953 0.049 Uiso 1 1 calc R . . O4 O 0.79701(15) 0.53754(6) 0.42799(11) 0.0216(3) Uani 1 1 d . . . O8 O 0.33601(14) 0.60210(6) 0.24526(10) 0.0178(3) Uani 1 1 d . . . C26 C 0.2139(2) 0.59552(11) 0.17200(17) 0.0284(5) Uani 1 1 d . . . H26A H 0.1971 0.5524 0.1578 0.043 Uiso 1 1 calc R . . H26B H 0.2308 0.6166 0.1128 0.043 Uiso 1 1 calc R . . H26C H 0.1311 0.6130 0.1959 0.043 Uiso 1 1 calc R . . O5 O 0.21750(15) 0.51328(6) 0.34335(10) 0.0196(3) Uani 1 1 d . . . O6 O 0.36920(14) 0.54661(6) 0.50554(10) 0.0165(3) Uani 1 1 d . . . C10 C 0.4156(2) 0.39964(9) 0.28813(14) 0.0193(4) Uani 1 1 d . . . H10 H 0.3580 0.4349 0.2832 0.023 Uiso 1 1 calc R . . C9 C 0.3513(2) 0.34297(10) 0.26629(15) 0.0206(4) Uani 1 1 d . . . H9 H 0.2525 0.3404 0.2466 0.025 Uiso 1 1 calc R . . C8 C 0.4320(2) 0.29163(9) 0.27355(15) 0.0210(4) Uani 1 1 d . . . H8 H 0.3897 0.2531 0.2605 0.025 Uiso 1 1 calc R . . C7 C 0.5787(2) 0.29676(9) 0.30070(14) 0.0186(4) Uani 1 1 d . . . C6 C 0.6733(2) 0.24596(9) 0.30724(15) 0.0222(4) Uani 1 1 d . . . H6 H 0.6365 0.2062 0.2958 0.027 Uiso 1 1 calc R . . C5 C 0.8144(2) 0.25398(9) 0.32951(15) 0.0214(4) Uani 1 1 d . . . H5 H 0.8752 0.2198 0.3322 0.026 Uiso 1 1 calc R . . C4 C 0.8736(2) 0.31320(9) 0.34909(14) 0.0177(4) Uani 1 1 d . . . C3 C 1.0195(2) 0.32387(10) 0.37092(15) 0.0217(4) Uani 1 1 d . . . H3 H 1.0847 0.2914 0.3710 0.026 Uiso 1 1 calc R . . C2 C 1.0662(2) 0.38173(10) 0.39209(15) 0.0219(4) Uani 1 1 d . . . H2 H 1.1642 0.3898 0.4063 0.026 Uiso 1 1 calc R . . C1 C 0.9680(2) 0.42880(9) 0.39255(15) 0.0192(4) Uani 1 1 d . . . H1 H 1.0017 0.4684 0.4094 0.023 Uiso 1 1 calc R . . C11 C 0.7826(2) 0.36321(9) 0.34736(14) 0.0163(4) Uani 1 1 d . . . C12 C 0.6337(2) 0.35513(9) 0.32046(14) 0.0161(4) Uani 1 1 d . . . N2 N 0.55320(18) 0.40590(7) 0.31536(12) 0.0162(3) Uani 1 1 d . . . N1 N 0.83035(17) 0.42049(7) 0.37044(12) 0.0156(3) Uani 1 1 d . . . C22 C 0.0319(2) 0.61772(10) 0.36645(15) 0.0206(4) Uani 1 1 d . . . H22 H 0.0046 0.5766 0.3566 0.025 Uiso 1 1 calc R . . C21 C -0.0736(2) 0.66202(10) 0.35687(16) 0.0238(5) Uani 1 1 d . . . H21 H -0.1697 0.6510 0.3400 0.029 Uiso 1 1 calc R . . C20 C -0.0366(2) 0.72153(10) 0.37218(16) 0.0237(5) Uani 1 1 d . . . H20 H -0.1069 0.7522 0.3661 0.028 Uiso 1 1 calc R . . C19 C 0.1065(2) 0.73697(9) 0.39693(15) 0.0204(4) Uani 1 1 d . . . C18 C 0.1562(2) 0.79784(10) 0.41391(17) 0.0256(5) Uani 1 1 d . . . H18 H 0.0903 0.8302 0.4081 0.031 Uiso 1 1 calc R . . C17 C 0.2949(2) 0.81013(10) 0.43794(16) 0.0253(5) Uani 1 1 d . . . H17 H 0.3247 0.8509 0.4493 0.030 Uiso 1 1 calc R . . C16 C 0.3979(2) 0.76233(9) 0.44648(15) 0.0199(4) Uani 1 1 d . . . C15 C 0.5432(2) 0.77133(10) 0.47361(16) 0.0228(4) Uani 1 1 d . . . H15 H 0.5790 0.8107 0.4895 0.027 Uiso 1 1 calc R . . C14 C 0.6327(2) 0.72262(9) 0.47689(15) 0.0213(4) Uani 1 1 d . . . H14 H 0.7311 0.7279 0.4960 0.026 Uiso 1 1 calc R . . C13 C 0.5777(2) 0.66481(9) 0.45170(14) 0.0184(4) Uani 1 1 d . . . H13 H 0.6409 0.6316 0.4527 0.022 Uiso 1 1 calc R . . C24 C 0.3525(2) 0.70258(9) 0.42676(14) 0.0161(4) Uani 1 1 d . . . C23 C 0.2053(2) 0.68951(9) 0.40367(14) 0.0164(4) Uani 1 1 d . . . N4 N 0.16857(17) 0.63028(8) 0.38864(12) 0.0167(3) Uani 1 1 d . . . N3 N 0.44167(17) 0.65492(7) 0.42675(12) 0.0159(3) Uani 1 1 d . . . O1W O 0.5684(2) 0.57600(7) -0.05982(12) 0.0324(4) Uani 1 1 d D . . H1W H 0.555(3) 0.5374(7) -0.0894(17) 0.050 Uiso 1 1 d D . . H2W H 0.528(3) 0.5705(11) -0.0018(12) 0.050 Uiso 1 1 d D . . O2W O 0.85157(18) 0.68143(8) 0.12279(13) 0.0357(4) Uani 1 1 d D . . H3W H 0.855(3) 0.6568(11) 0.0671(14) 0.050 Uiso 1 1 d D . . H4W H 0.773(2) 0.6651(12) 0.1483(18) 0.050 Uiso 1 1 d D . . O9 O 0.83444(19) 0.61968(8) -0.05563(13) 0.0368(4) Uani 1 1 d . . . H9A H 0.7488 0.6103 -0.0597 0.055 Uiso 1 1 calc R . . C27 C 0.9153(4) 0.56699(13) -0.0634(3) 0.0573(9) Uani 1 1 d . . . H27A H 1.0119 0.5738 -0.0317 0.086 Uiso 1 1 calc R . . H27B H 0.9167 0.5575 -0.1320 0.086 Uiso 1 1 calc R . . H27C H 0.8735 0.5331 -0.0320 0.086 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.01629(18) 0.01338(17) 0.01835(18) 0.00195(12) 0.00458(13) 0.00095(12) V2 0.01262(17) 0.01061(16) 0.01980(17) 0.00013(12) 0.00314(13) 0.00058(12) V3 0.01241(17) 0.01166(16) 0.01976(18) 0.00018(12) 0.00404(13) 0.00019(12) O1 0.0148(7) 0.0144(7) 0.0176(7) 0.0026(5) 0.0041(5) 0.0024(5) O2 0.0205(8) 0.0180(7) 0.0350(9) 0.0040(6) 0.0076(6) 0.0002(6) O3 0.0262(8) 0.0278(8) 0.0217(8) -0.0025(6) 0.0048(6) 0.0023(6) O7 0.0234(8) 0.0227(8) 0.0225(7) 0.0058(6) 0.0112(6) 0.0093(6) C25 0.0301(13) 0.0433(14) 0.0284(12) 0.0090(10) 0.0158(10) 0.0149(11) O4 0.0166(7) 0.0146(7) 0.0338(8) -0.0022(6) 0.0046(6) -0.0012(6) O8 0.0154(7) 0.0182(7) 0.0197(7) 0.0024(5) 0.0020(6) 0.0024(5) C26 0.0267(12) 0.0284(12) 0.0289(12) 0.0019(9) -0.0002(10) 0.0015(9) O5 0.0167(7) 0.0161(7) 0.0262(8) -0.0011(6) 0.0038(6) -0.0013(5) O6 0.0153(7) 0.0151(7) 0.0196(7) 0.0002(5) 0.0042(5) 0.0018(5) C10 0.0182(10) 0.0184(10) 0.0214(10) -0.0011(8) 0.0033(8) 0.0019(8) C9 0.0164(10) 0.0249(11) 0.0207(10) -0.0032(8) 0.0031(8) -0.0027(8) C8 0.0257(11) 0.0180(10) 0.0199(10) -0.0041(8) 0.0056(8) -0.0068(8) C7 0.0231(11) 0.0165(10) 0.0171(9) -0.0005(8) 0.0063(8) -0.0007(8) C6 0.0306(12) 0.0130(9) 0.0238(10) -0.0022(8) 0.0068(9) -0.0010(8) C5 0.0278(11) 0.0137(10) 0.0236(11) 0.0003(8) 0.0064(9) 0.0060(8) C4 0.0202(10) 0.0171(10) 0.0163(9) -0.0002(7) 0.0040(8) 0.0020(8) C3 0.0211(11) 0.0210(10) 0.0230(10) 0.0007(8) 0.0029(8) 0.0084(8) C2 0.0155(10) 0.0249(11) 0.0252(11) -0.0006(8) 0.0029(8) 0.0024(8) C1 0.0176(10) 0.0186(10) 0.0218(10) -0.0012(8) 0.0039(8) 0.0008(8) C11 0.0204(10) 0.0134(9) 0.0156(9) 0.0011(7) 0.0048(8) 0.0020(8) C12 0.0189(10) 0.0153(9) 0.0149(9) 0.0006(7) 0.0047(8) 0.0007(7) N2 0.0168(8) 0.0152(8) 0.0169(8) -0.0005(6) 0.0027(7) 0.0012(6) N1 0.0150(8) 0.0134(8) 0.0188(8) 0.0008(6) 0.0039(6) 0.0006(6) C22 0.0174(10) 0.0210(10) 0.0238(10) 0.0029(8) 0.0037(8) -0.0008(8) C21 0.0136(10) 0.0306(12) 0.0277(11) 0.0060(9) 0.0048(8) 0.0015(8) C20 0.0194(11) 0.0274(11) 0.0251(11) 0.0059(9) 0.0060(9) 0.0094(9) C19 0.0198(11) 0.0208(10) 0.0212(10) 0.0028(8) 0.0046(8) 0.0048(8) C18 0.0259(12) 0.0183(10) 0.0329(12) 0.0003(9) 0.0050(9) 0.0089(9) C17 0.0308(12) 0.0138(10) 0.0310(12) -0.0008(8) 0.0036(10) 0.0032(9) C16 0.0240(11) 0.0151(10) 0.0208(10) 0.0008(8) 0.0030(8) 0.0009(8) C15 0.0256(11) 0.0169(10) 0.0259(11) -0.0012(8) 0.0029(9) -0.0044(8) C14 0.0182(10) 0.0205(10) 0.0246(11) 0.0004(8) 0.0005(8) -0.0033(8) C13 0.0164(10) 0.0179(10) 0.0210(10) 0.0009(8) 0.0031(8) 0.0020(8) C24 0.0189(10) 0.0152(9) 0.0146(9) 0.0011(7) 0.0035(8) 0.0013(7) C23 0.0171(10) 0.0172(10) 0.0155(9) 0.0020(7) 0.0043(8) 0.0026(8) N4 0.0152(8) 0.0166(8) 0.0187(8) 0.0021(6) 0.0039(7) 0.0010(6) N3 0.0163(8) 0.0140(8) 0.0175(8) 0.0006(6) 0.0024(7) 0.0016(6) O1W 0.0469(11) 0.0244(8) 0.0289(9) -0.0020(7) 0.0156(8) -0.0065(7) O2W 0.0307(9) 0.0403(10) 0.0363(10) -0.0005(8) 0.0048(8) -0.0120(8) O9 0.0388(10) 0.0310(9) 0.0412(10) -0.0032(8) 0.0073(8) -0.0030(8) C27 0.0495(19) 0.0342(16) 0.093(3) 0.0030(16) 0.0263(18) -0.0008(13) _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 O2 1.6292(15) . ? V1 O3 1.6479(15) . ? V1 O8 1.9633(14) . ? V1 O7 1.9710(14) . ? V1 O1 1.9714(14) . ? V1 V2 3.1069(5) . ? V1 V3 3.1153(5) . ? V2 O4 1.6081(14) . ? V2 O6 1.9236(14) 3_666 ? V2 O1 1.9424(13) . ? V2 O7 1.9963(15) . ? V2 N1 2.1458(17) . ? V2 N2 2.3402(17) . ? V2 V3 3.5281(6) 3_666 ? V2 V3 3.6665(6) . ? V2 V2 5.1411(8) 3_666 ? V3 O5 1.6157(14) . ? V3 O6 1.7150(14) . ? V3 O1 1.8815(14) . ? V3 O8 2.1209(14) . ? V3 N4 2.1835(17) . ? V3 N3 2.3137(17) . ? O7 C25 1.406(3) . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? O8 C26 1.450(3) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? O6 V2 1.9236(14) 3_666 ? C10 N2 1.328(3) . ? C10 C9 1.409(3) . ? C10 H10 0.9500 . ? C9 C8 1.368(3) . ? C9 H9 0.9500 . ? C8 C7 1.408(3) . ? C8 H8 0.9500 . ? C7 C12 1.405(3) . ? C7 C6 1.437(3) . ? C6 C5 1.356(3) . ? C6 H6 0.9500 . ? C5 C4 1.436(3) . ? C5 H5 0.9500 . ? C4 C11 1.404(3) . ? C4 C3 1.408(3) . ? C3 C2 1.372(3) . ? C3 H3 0.9500 . ? C2 C1 1.402(3) . ? C2 H2 0.9500 . ? C1 N1 1.325(3) . ? C1 H1 0.9500 . ? C11 N1 1.368(2) . ? C11 C12 1.434(3) . ? C12 N2 1.357(3) . ? C22 N4 1.332(3) . ? C22 C21 1.399(3) . ? C22 H22 0.9500 . ? C21 C20 1.370(3) . ? C21 H21 0.9500 . ? C20 C19 1.408(3) . ? C20 H20 0.9500 . ? C19 C23 1.406(3) . ? C19 C18 1.434(3) . ? C18 C17 1.352(3) . ? C18 H18 0.9500 . ? C17 C16 1.438(3) . ? C17 H17 0.9500 . ? C16 C24 1.404(3) . ? C16 C15 1.404(3) . ? C15 C14 1.372(3) . ? C15 H15 0.9500 . ? C14 C13 1.406(3) . ? C14 H14 0.9500 . ? C13 N3 1.319(3) . ? C13 H13 0.9500 . ? C24 N3 1.355(3) . ? C24 C23 1.431(3) . ? C23 N4 1.363(3) . ? O1W H1W 0.947(10) . ? O1W H2W 0.952(10) . ? O2W H3W 0.953(10) . ? O2W H4W 0.945(10) . ? O9 C27 1.410(3) . ? O9 H9A 0.8400 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? 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 V1 O3 109.38(8) . . ? O2 V1 O8 102.64(7) . . ? O3 V1 O8 95.83(7) . . ? O2 V1 O7 100.15(7) . . ? O3 V1 O7 94.38(7) . . ? O8 V1 O7 150.24(6) . . ? O2 V1 O1 118.76(7) . . ? O3 V1 O1 131.77(7) . . ? O8 V1 O1 77.28(6) . . ? O7 V1 O1 75.08(6) . . ? O2 V1 V2 108.97(6) . . ? O3 V1 V2 123.30(6) . . ? O8 V1 V2 114.40(4) . . ? O7 V1 V2 38.74(4) . . ? O1 V1 V2 37.13(4) . . ? O2 V1 V3 117.24(6) . . ? O3 V1 V3 121.39(6) . . ? O8 V1 V3 42.20(4) . . ? O7 V1 V3 109.55(4) . . ? O1 V1 V3 35.08(4) . . ? V2 V1 V3 72.208(13) . . ? O4 V2 O6 98.94(7) . 3_666 ? O4 V2 O1 106.54(7) . . ? O6 V2 O1 97.61(6) 3_666 . ? O4 V2 O7 99.80(7) . . ? O6 V2 O7 161.17(6) 3_666 . ? O1 V2 O7 75.15(6) . . ? O4 V2 N1 92.49(7) . . ? O6 V2 N1 88.40(6) 3_666 . ? O1 V2 N1 158.76(6) . . ? O7 V2 N1 92.72(6) . . ? O4 V2 N2 165.42(7) . . ? O6 V2 N2 78.38(6) 3_666 . ? O1 V2 N2 88.03(6) . . ? O7 V2 N2 83.95(6) . . ? N1 V2 N2 73.19(6) . . ? O4 V2 V1 100.77(5) . . ? O6 V2 V1 134.92(4) 3_666 . ? O1 V2 V1 37.78(4) . . ? O7 V2 V1 38.16(4) . . ? N1 V2 V1 130.43(5) . . ? N2 V2 V1 90.90(4) . . ? O4 V2 V3 86.11(6) . 3_666 ? O6 V2 V3 13.35(4) 3_666 3_666 ? O1 V2 V3 104.97(4) . 3_666 ? O7 V2 V3 173.84(5) . 3_666 ? N1 V2 V3 85.24(5) . 3_666 ? N2 V2 V3 89.90(4) . 3_666 ? V1 V2 V3 142.653(14) . 3_666 ? O4 V2 V3 107.38(5) . . ? O6 V2 V3 81.49(4) 3_666 . ? O1 V2 V3 16.23(4) . . ? O7 V2 V3 91.07(4) . . ? N1 V2 V3 158.82(5) . . ? N2 V2 V3 86.52(4) . . ? V1 V2 V3 54.003(10) . . ? V3 V2 V3 88.802(11) 3_666 . ? O4 V2 V2 99.58(6) . 3_666 ? O6 V2 V2 39.35(4) 3_666 3_666 ? O1 V2 V2 59.50(4) . 3_666 ? O7 V2 V2 134.07(4) . 3_666 ? N1 V2 V2 127.45(5) . 3_666 ? N2 V2 V2 87.45(4) . 3_666 ? V1 V2 V2 97.261(14) . 3_666 ? V3 V2 V2 45.480(8) 3_666 3_666 ? V3 V2 V2 43.322(8) . 3_666 ? O5 V3 O6 103.54(7) . . ? O5 V3 O1 107.17(7) . . ? O6 V3 O1 98.94(6) . . ? O5 V3 O8 92.66(7) . . ? O6 V3 O8 163.79(6) . . ? O1 V3 O8 75.48(5) . . ? O5 V3 N4 89.94(7) . . ? O6 V3 N4 99.09(6) . . ? O1 V3 N4 151.37(6) . . ? O8 V3 N4 81.08(6) . . ? O5 V3 N3 161.35(7) . . ? O6 V3 N3 85.07(6) . . ? O1 V3 N3 87.39(6) . . ? O8 V3 N3 79.53(6) . . ? N4 V3 N3 72.22(6) . . ? O5 V3 V1 102.78(5) . . ? O6 V3 V1 134.14(5) . . ? O1 V3 V1 37.03(4) . . ? O8 V3 V1 38.45(4) . . ? N4 V3 V1 117.81(5) . . ? N3 V3 V1 81.66(4) . . ? O5 V3 V2 106.35(5) . . ? O6 V3 V2 82.93(5) . . ? O1 V3 V2 16.77(4) . . ? O8 V3 V2 92.23(4) . . ? N4 V3 V2 162.73(5) . . ? N3 V3 V2 90.97(4) . . ? V1 V3 V2 53.789(10) . . ? V3 O1 V2 147.01(8) . . ? V3 O1 V1 107.89(6) . . ? V2 O1 V1 105.09(6) . . ? C25 O7 V1 123.93(13) . . ? C25 O7 V2 131.35(13) . . ? V1 O7 V2 103.09(7) . . ? O7 C25 H25A 109.5 . . ? O7 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? O7 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C26 O8 V1 119.03(13) . . ? C26 O8 V3 119.71(13) . . ? V1 O8 V3 99.35(6) . . ? O8 C26 H26A 109.5 . . ? O8 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? O8 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? V3 O6 V2 151.64(8) . 3_666 ? N2 C10 C9 122.77(19) . . ? N2 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? C8 C9 C10 119.62(19) . . ? C8 C9 H9 120.2 . . ? C10 C9 H9 120.2 . . ? C9 C8 C7 119.07(19) . . ? C9 C8 H8 120.5 . . ? C7 C8 H8 120.5 . . ? C12 C7 C8 117.39(19) . . ? C12 C7 C6 119.14(19) . . ? C8 C7 C6 123.46(19) . . ? C5 C6 C7 120.84(19) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C6 C5 C4 121.13(19) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C11 C4 C3 117.84(18) . . ? C11 C4 C5 119.00(18) . . ? C3 C4 C5 123.16(19) . . ? C2 C3 C4 119.10(19) . . ? C2 C3 H3 120.4 . . ? C4 C3 H3 120.5 . . ? C3 C2 C1 119.50(19) . . ? C3 C2 H2 120.3 . . ? C1 C2 H2 120.3 . . ? N1 C1 C2 122.87(19) . . ? N1 C1 H1 118.6 . . ? C2 C1 H1 118.6 . . ? N1 C11 C4 122.42(18) . . ? N1 C11 C12 117.67(17) . . ? C4 C11 C12 119.92(18) . . ? N2 C12 C7 123.50(19) . . ? N2 C12 C11 116.64(17) . . ? C7 C12 C11 119.86(18) . . ? C10 N2 C12 117.63(17) . . ? C10 N2 V2 129.03(14) . . ? C12 N2 V2 112.70(13) . . ? C1 N1 C11 118.19(17) . . ? C1 N1 V2 123.10(14) . . ? C11 N1 V2 118.56(13) . . ? N4 C22 C21 123.4(2) . . ? N4 C22 H22 118.3 . . ? C21 C22 H22 118.3 . . ? C20 C21 C22 119.2(2) . . ? C20 C21 H21 120.4 . . ? C22 C21 H21 120.4 . . ? C21 C20 C19 119.5(2) . . ? C21 C20 H20 120.2 . . ? C19 C20 H20 120.2 . . ? C23 C19 C20 117.33(19) . . ? C23 C19 C18 118.81(19) . . ? C20 C19 C18 123.85(19) . . ? C17 C18 C19 121.4(2) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C18 C17 C16 120.8(2) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C24 C16 C15 117.00(19) . . ? C24 C16 C17 118.87(19) . . ? C15 C16 C17 124.13(19) . . ? C14 C15 C16 119.30(19) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C15 C14 C13 119.45(19) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? N3 C13 C14 122.56(19) . . ? N3 C13 H13 118.7 . . ? C14 C13 H13 118.7 . . ? N3 C24 C16 123.46(18) . . ? N3 C24 C23 116.39(17) . . ? C16 C24 C23 120.15(18) . . ? N4 C23 C19 123.19(19) . . ? N4 C23 C24 116.97(17) . . ? C19 C23 C24 119.83(18) . . ? C22 N4 C23 117.39(18) . . ? C22 N4 V3 123.24(14) . . ? C23 N4 V3 118.91(13) . . ? C13 N3 C24 118.09(17) . . ? C13 N3 V3 126.81(13) . . ? C24 N3 V3 115.10(13) . . ? H1W O1W H2W 101.9(13) . . ? H3W O2W H4W 102.2(13) . . ? C27 O9 H9A 109.5 . . ? O9 C27 H27A 109.5 . . ? O9 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? O9 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H2W O3 0.952(10) 1.795(11) 2.739(2) 171(2) . O1W H1W O3 0.947(10) 1.901(13) 2.816(2) 162(2) 3_665 O2W H4W O2 0.945(10) 2.016(10) 2.959(2) 176(2) . O2W H3W O9 0.953(10) 1.880(12) 2.819(3) 168(3) . O9 H9A O1W 0.84 1.89 2.717(3) 169.9 . _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.744 _refine_diff_density_min -0.322 _refine_diff_density_rms 0.073 # Attachment '- 2.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 825040' #TrackingRef '- 2.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C44 H44 N8 O16 V6, 2(C H4 O)' _chemical_formula_sum 'C46 H52 N8 O18 V6' _chemical_formula_weight 1310.60 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting MONOCLINIC _symmetry_space_group_name_H-M P2(1)/C 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 9.8178(7) _cell_length_b 17.4725(12) _cell_length_c 15.6874(11) _cell_angle_alpha 90.00 _cell_angle_beta 106.1220(10) _cell_angle_gamma 90.00 _cell_volume 2585.2(3) _cell_formula_units_Z 2 _cell_measurement_temperature 98(2) _cell_measurement_reflns_used 5868 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 28.19 _exptl_crystal_description parallelepiped _exptl_crystal_colour brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.684 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1332 _exptl_absorpt_coefficient_mu 1.122 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.856 _exptl_absorpt_correction_T_max 0.981 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 98(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 23682 _diffrn_reflns_av_R_equivalents 0.0332 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.10 _reflns_number_total 5714 _reflns_number_gt 4766 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0540P)^2^+2.5959P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment riding _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5714 _refine_ls_number_parameters 356 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0495 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.1067 _refine_ls_wR_factor_gt 0.1006 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.22171(5) 0.04421(3) 0.77208(3) 0.02215(12) Uani 1 1 d . . . V2 V 0.23903(4) 0.06262(2) 0.57840(3) 0.01950(11) Uani 1 1 d . . . V3 V -0.06320(4) -0.01366(2) 0.64437(3) 0.01955(11) Uani 1 1 d . . . O3 O 0.2241(2) 0.11030(12) 0.84571(13) 0.0335(5) Uani 1 1 d . . . O2 O 0.3392(2) -0.02131(12) 0.81620(13) 0.0322(5) Uani 1 1 d . . . O1 O 0.11314(17) 0.03070(9) 0.64534(11) 0.0185(3) Uani 1 1 d . . . O4 O 0.35148(18) -0.00532(10) 0.58380(12) 0.0218(4) Uani 1 1 d . . . O5 O -0.17024(19) 0.05676(10) 0.64363(13) 0.0237(4) Uani 1 1 d . . . O6 O -0.11642(18) -0.04706(9) 0.53296(11) 0.0195(4) Uani 1 1 d . . . O7 O 0.32755(18) 0.10427(10) 0.70394(12) 0.0234(4) Uani 1 1 d . . . O8 O 0.04392(19) -0.00349(11) 0.77774(12) 0.0244(4) Uani 1 1 d . . . C1 C 0.4982(3) 0.11963(15) 0.52306(18) 0.0239(5) Uani 1 1 d . . . H1 H 0.5258 0.0677 0.5347 0.029 Uiso 1 1 calc R . . C2 C 0.5906(3) 0.16892(16) 0.49877(19) 0.0268(6) Uani 1 1 d . . . H2 H 0.6796 0.1513 0.4938 0.032 Uiso 1 1 calc R . . C3 C 0.5509(3) 0.24446(16) 0.48180(19) 0.0293(6) Uani 1 1 d . . . H3 H 0.6127 0.2797 0.4652 0.035 Uiso 1 1 calc R . . C4 C 0.4199(3) 0.26847(16) 0.48918(19) 0.0279(6) Uani 1 1 d . . . H4 H 0.3908 0.3202 0.4775 0.034 Uiso 1 1 calc R . . C5 C 0.3320(3) 0.21575(14) 0.51392(16) 0.0201(5) Uani 1 1 d . . . C6 C 0.1926(3) 0.23667(14) 0.52608(16) 0.0198(5) Uani 1 1 d . . . C7 C 0.1308(3) 0.30839(15) 0.50523(18) 0.0263(6) Uani 1 1 d . . . H7 H 0.1761 0.3467 0.4799 0.032 Uiso 1 1 calc R . . C8 C 0.0023(3) 0.32281(15) 0.52208(18) 0.0271(6) Uani 1 1 d . . . H8 H -0.0418 0.3714 0.5087 0.032 Uiso 1 1 calc R . . C9 C -0.0614(3) 0.26584(15) 0.55859(18) 0.0255(5) Uani 1 1 d . . . H9 H -0.1485 0.2749 0.5720 0.031 Uiso 1 1 calc R . . C10 C 0.0046(3) 0.19525(15) 0.57513(18) 0.0240(5) Uani 1 1 d . . . H10 H -0.0409 0.1555 0.5981 0.029 Uiso 1 1 calc R . . C11 C 0.1754(3) -0.14674(15) 0.66441(18) 0.0238(5) Uani 1 1 d . . . H11 H 0.2254 -0.1076 0.6437 0.029 Uiso 1 1 calc R . . C12 C 0.2386(3) -0.21782(15) 0.68393(18) 0.0260(6) Uani 1 1 d . . . H12 H 0.3310 -0.2268 0.6782 0.031 Uiso 1 1 calc R . . C13 C 0.1650(3) -0.27554(15) 0.71195(19) 0.0293(6) Uani 1 1 d . . . H13 H 0.2061 -0.3248 0.7258 0.035 Uiso 1 1 calc R . . C14 C 0.0301(3) -0.26030(15) 0.71960(18) 0.0269(6) Uani 1 1 d . . . H14 H -0.0239 -0.2994 0.7369 0.032 Uiso 1 1 calc R . . C15 C -0.0244(3) -0.18697(14) 0.70146(16) 0.0198(5) Uani 1 1 d . . . C16 C -0.1633(3) -0.16300(14) 0.71236(16) 0.0198(5) Uani 1 1 d . . . C17 C -0.2479(3) -0.21063(15) 0.74779(18) 0.0262(6) Uani 1 1 d . . . H17 H -0.2215 -0.2624 0.7617 0.031 Uiso 1 1 calc R . . C18 C -0.3704(3) -0.18164(17) 0.76235(19) 0.0294(6) Uani 1 1 d . . . H18 H -0.4264 -0.2126 0.7893 0.035 Uiso 1 1 calc R . . C19 C -0.4112(3) -0.10714(16) 0.73740(19) 0.0276(6) Uani 1 1 d . . . H19 H -0.4954 -0.0862 0.7463 0.033 Uiso 1 1 calc R . . C20 C -0.3254(3) -0.06431(15) 0.69918(18) 0.0249(5) Uani 1 1 d . . . H20 H -0.3548 -0.0140 0.6795 0.030 Uiso 1 1 calc R . . N1 N 0.3707(2) 0.14161(11) 0.53105(13) 0.0195(4) Uani 1 1 d . . . N2 N 0.1298(2) 0.18060(11) 0.56019(14) 0.0203(4) Uani 1 1 d . . . N3 N 0.0469(2) -0.13097(11) 0.67354(13) 0.0187(4) Uani 1 1 d . . . N4 N -0.2026(2) -0.09033(12) 0.68843(13) 0.0192(4) Uani 1 1 d . . . O9 O 0.2962(3) -0.08709(15) 0.97331(18) 0.0574(7) Uani 1 1 d . . . H9A H 0.3223 -0.0767 0.9280 0.086 Uiso 1 1 calc R . . C21 C 0.4730(3) 0.12086(17) 0.7447(2) 0.0304(6) Uani 1 1 d . . . H21C H 0.4822 0.1482 0.8006 0.046 Uiso 1 1 calc R . . H21B H 0.5100 0.1529 0.7049 0.046 Uiso 1 1 calc R . . H21A H 0.5269 0.0730 0.7567 0.046 Uiso 1 1 calc R . . C22 C -0.0194(3) 0.00923(18) 0.84777(19) 0.0317(6) Uani 1 1 d . . . H22C H 0.0549 0.0155 0.9038 0.048 Uiso 1 1 calc R . . H22B H -0.0792 -0.0347 0.8523 0.048 Uiso 1 1 calc R . . H22A H -0.0777 0.0556 0.8354 0.048 Uiso 1 1 calc R . . C23 C 0.3377(5) -0.0264(3) 1.0368(3) 0.0614(11) Uani 1 1 d . . . H23A H 0.2799 -0.0284 1.0786 0.092 Uiso 1 1 calc R . . H23B H 0.3235 0.0230 1.0059 0.092 Uiso 1 1 calc R . . H23C H 0.4379 -0.0322 1.0692 0.092 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0182(2) 0.0264(2) 0.0214(2) -0.00632(17) 0.00464(17) 0.00117(17) V2 0.0216(2) 0.0134(2) 0.0266(2) -0.00107(16) 0.01191(18) -0.00042(16) V3 0.0149(2) 0.0153(2) 0.0282(2) 0.00291(16) 0.00537(17) -0.00060(15) O3 0.0312(11) 0.0375(11) 0.0345(11) -0.0156(9) 0.0136(9) -0.0050(9) O2 0.0234(10) 0.0408(12) 0.0316(11) 0.0002(9) 0.0063(8) 0.0077(8) O1 0.0162(8) 0.0186(8) 0.0209(8) -0.0021(7) 0.0055(7) -0.0026(6) O4 0.0201(9) 0.0175(8) 0.0285(10) -0.0003(7) 0.0080(7) -0.0007(7) O5 0.0216(9) 0.0157(8) 0.0352(10) 0.0023(7) 0.0106(8) 0.0005(7) O6 0.0174(8) 0.0178(8) 0.0233(9) 0.0004(7) 0.0057(7) -0.0040(7) O7 0.0153(8) 0.0266(9) 0.0276(9) -0.0084(7) 0.0045(7) -0.0053(7) O8 0.0220(9) 0.0327(10) 0.0208(9) -0.0023(7) 0.0094(7) -0.0004(8) C1 0.0220(13) 0.0200(12) 0.0305(14) -0.0019(10) 0.0088(11) 0.0005(10) C2 0.0205(13) 0.0267(14) 0.0353(15) -0.0009(11) 0.0113(11) -0.0016(10) C3 0.0242(14) 0.0271(14) 0.0390(16) 0.0063(12) 0.0125(12) -0.0030(11) C4 0.0271(14) 0.0214(13) 0.0368(15) 0.0061(11) 0.0113(12) 0.0009(11) C5 0.0188(12) 0.0198(12) 0.0204(12) -0.0002(9) 0.0034(10) 0.0000(9) C6 0.0192(12) 0.0200(12) 0.0194(12) -0.0009(9) 0.0042(10) -0.0020(9) C7 0.0279(14) 0.0209(13) 0.0313(14) 0.0057(11) 0.0104(12) 0.0011(10) C8 0.0269(14) 0.0221(13) 0.0311(14) 0.0032(11) 0.0063(12) 0.0056(11) C9 0.0223(13) 0.0244(13) 0.0303(14) -0.0011(11) 0.0081(11) 0.0015(10) C10 0.0206(13) 0.0214(13) 0.0308(14) -0.0015(10) 0.0084(11) -0.0020(10) C11 0.0202(13) 0.0229(13) 0.0288(13) 0.0004(10) 0.0076(11) -0.0009(10) C12 0.0199(13) 0.0249(13) 0.0331(14) -0.0018(11) 0.0071(11) 0.0037(10) C13 0.0291(15) 0.0202(13) 0.0389(16) 0.0032(11) 0.0100(12) 0.0056(11) C14 0.0284(14) 0.0200(13) 0.0335(15) 0.0046(11) 0.0107(12) -0.0001(11) C15 0.0188(12) 0.0199(12) 0.0196(12) -0.0002(9) 0.0037(10) -0.0015(9) C16 0.0172(12) 0.0211(12) 0.0193(12) 0.0009(9) 0.0018(10) -0.0018(9) C17 0.0231(13) 0.0232(13) 0.0315(14) 0.0080(11) 0.0061(11) -0.0004(10) C18 0.0229(14) 0.0347(15) 0.0311(14) 0.0075(12) 0.0085(12) -0.0055(11) C19 0.0192(13) 0.0316(14) 0.0327(14) -0.0001(11) 0.0082(11) -0.0014(11) C20 0.0208(13) 0.0213(13) 0.0323(14) 0.0020(11) 0.0067(11) 0.0003(10) N1 0.0198(10) 0.0172(10) 0.0217(10) -0.0019(8) 0.0059(9) -0.0008(8) N2 0.0196(10) 0.0157(10) 0.0255(11) -0.0025(8) 0.0062(9) -0.0026(8) N3 0.0172(10) 0.0181(10) 0.0204(10) 0.0007(8) 0.0043(8) -0.0013(8) N4 0.0166(10) 0.0191(10) 0.0212(10) 0.0007(8) 0.0038(8) -0.0008(8) O9 0.0685(18) 0.0488(15) 0.0590(17) 0.0141(13) 0.0244(14) -0.0025(13) C21 0.0175(13) 0.0333(15) 0.0384(16) -0.0111(12) 0.0045(12) -0.0064(11) C22 0.0336(16) 0.0375(16) 0.0284(15) -0.0004(12) 0.0157(13) 0.0008(12) C23 0.059(3) 0.081(3) 0.042(2) 0.001(2) 0.0099(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 V1 O3 1.6287(19) . ? V1 O2 1.636(2) . ? V1 O8 1.9585(18) . ? V1 O7 1.9850(18) . ? V1 O1 1.9919(17) . ? V1 V2 3.1065(6) . ? V1 V3 3.1222(6) . ? V2 O4 1.6072(17) . ? V2 O6 1.8458(18) 3_556 ? V2 O1 1.9136(17) . ? V2 O7 2.0526(18) . ? V2 N1 2.159(2) . ? V2 N2 2.305(2) . ? V2 V3 3.5460(7) 3_556 ? V2 V3 3.6546(6) . ? V2 V2 5.1435(9) 3_556 ? V3 O5 1.6160(17) . ? V3 O6 1.7780(18) . ? V3 O1 1.8930(17) . ? V3 O8 2.0719(18) . ? V3 N4 2.161(2) . ? V3 N3 2.303(2) . ? O6 V2 1.8458(18) 3_556 ? O7 C21 1.423(3) . ? O8 C22 1.422(3) . ? C1 N1 1.349(3) . ? C1 C2 1.379(4) . ? C1 H1 0.9500 . ? C2 C3 1.381(4) . ? C2 H2 0.9500 . ? C3 C4 1.388(4) . ? C3 H3 0.9500 . ? C4 C5 1.389(3) . ? C4 H4 0.9500 . ? C5 N1 1.356(3) . ? C5 C6 1.479(3) . ? C6 N2 1.345(3) . ? C6 C7 1.391(4) . ? C7 C8 1.382(4) . ? C7 H7 0.9500 . ? C8 C9 1.381(4) . ? C8 H8 0.9500 . ? C9 C10 1.384(4) . ? C9 H9 0.9500 . ? C10 N2 1.338(3) . ? C10 H10 0.9500 . ? C11 N3 1.338(3) . ? C11 C12 1.384(4) . ? C11 H11 0.9500 . ? C12 C13 1.381(4) . ? C12 H12 0.9500 . ? C13 C14 1.388(4) . ? C13 H13 0.9500 . ? C14 C15 1.387(4) . ? C14 H14 0.9500 . ? C15 N3 1.345(3) . ? C15 C16 1.481(3) . ? C16 N4 1.350(3) . ? C16 C17 1.396(3) . ? C17 C18 1.381(4) . ? C17 H17 0.9500 . ? C18 C19 1.386(4) . ? C18 H18 0.9500 . ? C19 C20 1.381(4) . ? C19 H19 0.9500 . ? C20 N4 1.342(3) . ? C20 H20 0.9500 . ? O9 C23 1.434(5) . ? O9 H9A 0.8400 . ? C21 H21C 0.9800 . ? C21 H21B 0.9800 . ? C21 H21A 0.9800 . ? C22 H22C 0.9800 . ? C22 H22B 0.9800 . ? C22 H22A 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? 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 O2 109.05(11) . . ? O3 V1 O8 96.16(9) . . ? O2 V1 O8 102.44(9) . . ? O3 V1 O7 95.76(9) . . ? O2 V1 O7 100.65(9) . . ? O8 V1 O7 148.85(8) . . ? O3 V1 O1 133.65(9) . . ? O2 V1 O1 117.28(9) . . ? O8 V1 O1 76.00(7) . . ? O7 V1 O1 74.95(7) . . ? O3 V1 V2 128.77(8) . . ? O2 V1 V2 105.22(7) . . ? O8 V1 V2 112.33(5) . . ? O7 V1 V2 40.50(5) . . ? O1 V1 V2 36.44(5) . . ? O3 V1 V3 121.24(7) . . ? O2 V1 V3 116.46(8) . . ? O8 V1 V3 40.56(5) . . ? O7 V1 V3 109.59(5) . . ? O1 V1 V3 35.45(5) . . ? V2 V1 V3 71.851(15) . . ? O4 V2 O6 101.48(8) . 3_556 ? O4 V2 O1 107.14(8) . . ? O6 V2 O1 97.22(7) 3_556 . ? O4 V2 O7 96.30(8) . . ? O6 V2 O7 162.07(8) 3_556 . ? O1 V2 O7 75.09(7) . . ? O4 V2 N1 91.27(8) . . ? O6 V2 N1 93.67(8) 3_556 . ? O1 V2 N1 156.17(8) . . ? O7 V2 N1 88.22(7) . . ? O4 V2 N2 163.01(8) . . ? O6 V2 N2 81.70(8) 3_556 . ? O1 V2 N2 88.82(7) . . ? O7 V2 N2 81.97(7) . . ? N1 V2 N2 71.82(7) . . ? O4 V2 V1 95.47(7) . . ? O6 V2 V1 135.40(5) 3_556 . ? O1 V2 V1 38.19(5) . . ? O7 V2 V1 38.91(5) . . ? N1 V2 V1 127.11(6) . . ? N2 V2 V1 93.66(5) . . ? O4 V2 V3 90.75(7) . 3_556 ? O6 V2 V3 11.66(5) 3_556 3_556 ? O1 V2 V3 104.99(5) . 3_556 ? O7 V2 V3 172.61(6) . 3_556 ? N1 V2 V3 89.38(6) . 3_556 ? N2 V2 V3 90.64(5) . 3_556 ? V1 V2 V3 142.660(17) . 3_556 ? O4 V2 V3 108.40(6) . . ? O6 V2 V3 81.19(5) 3_556 . ? O1 V2 V3 16.16(5) . . ? O7 V2 V3 91.05(5) . . ? N1 V2 V3 160.27(6) . . ? N2 V2 V3 88.56(5) . . ? V1 V2 V3 54.274(12) . . ? V3 V2 V3 88.840(14) 3_556 . ? O4 V2 V2 103.49(6) . 3_556 ? O6 V2 V2 38.37(5) 3_556 3_556 ? O1 V2 V2 59.73(5) . 3_556 ? O7 V2 V2 134.17(5) . 3_556 ? N1 V2 V2 131.41(6) . 3_556 ? N2 V2 V2 89.42(5) . 3_556 ? V1 V2 V2 97.657(15) . 3_556 ? V3 V2 V2 45.266(10) 3_556 3_556 ? V3 V2 V2 43.574(10) . 3_556 ? O5 V3 O6 103.29(9) . . ? O5 V3 O1 106.25(8) . . ? O6 V3 O1 99.25(7) . . ? O5 V3 O8 95.09(9) . . ? O6 V3 O8 161.62(8) . . ? O1 V3 O8 75.53(7) . . ? O5 V3 N4 90.34(8) . . ? O6 V3 N4 94.11(8) . . ? O1 V3 N4 155.53(8) . . ? O8 V3 N4 85.36(7) . . ? O5 V3 N3 161.33(8) . . ? O6 V3 N3 84.07(8) . . ? O1 V3 N3 89.15(7) . . ? O8 V3 N3 78.29(7) . . ? N4 V3 N3 71.86(7) . . ? O5 V3 V1 102.89(7) . . ? O6 V3 V1 134.70(6) . . ? O1 V3 V1 37.61(5) . . ? O8 V3 V1 37.93(5) . . ? N4 V3 V1 121.98(6) . . ? N3 V3 V1 82.73(5) . . ? O5 V3 V2 107.33(6) . . ? O6 V3 V2 83.19(5) . . ? O1 V3 V2 16.34(5) . . ? O8 V3 V2 91.74(5) . . ? N4 V3 V2 162.29(6) . . ? N3 V3 V2 90.44(5) . . ? V1 V3 V2 53.874(13) . . ? V3 O1 V2 147.51(10) . . ? V3 O1 V1 106.94(8) . . ? V2 O1 V1 105.37(8) . . ? V3 O6 V2 156.23(11) . 3_556 ? C21 O7 V1 118.40(17) . . ? C21 O7 V2 127.46(16) . . ? V1 O7 V2 100.59(8) . . ? C22 O8 V1 123.70(17) . . ? C22 O8 V3 125.82(17) . . ? V1 O8 V3 101.51(8) . . ? N1 C1 C2 123.1(2) . . ? N1 C1 H1 118.4 . . ? C2 C1 H1 118.4 . . ? C1 C2 C3 118.6(2) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C2 C3 C4 119.4(2) . . ? C2 C3 H3 120.3 . . ? C4 C3 H3 120.3 . . ? C3 C4 C5 119.0(2) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? N1 C5 C4 121.9(2) . . ? N1 C5 C6 115.4(2) . . ? C4 C5 C6 122.7(2) . . ? N2 C6 C7 122.1(2) . . ? N2 C6 C5 114.5(2) . . ? C7 C6 C5 123.4(2) . . ? C8 C7 C6 118.8(2) . . ? C8 C7 H7 120.6 . . ? C6 C7 H7 120.6 . . ? C9 C8 C7 119.3(2) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 C10 118.5(2) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? N2 C10 C9 122.9(2) . . ? N2 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? N3 C11 C12 122.6(2) . . ? N3 C11 H11 118.7 . . ? C12 C11 H11 118.7 . . ? C13 C12 C11 119.0(2) . . ? C13 C12 H12 120.5 . . ? C11 C12 H12 120.5 . . ? C12 C13 C14 118.9(2) . . ? C12 C13 H13 120.6 . . ? C14 C13 H13 120.6 . . ? C15 C14 C13 118.8(2) . . ? C15 C14 H14 120.6 . . ? C13 C14 H14 120.6 . . ? N3 C15 C14 122.2(2) . . ? N3 C15 C16 114.2(2) . . ? C14 C15 C16 123.5(2) . . ? N4 C16 C17 121.0(2) . . ? N4 C16 C15 115.8(2) . . ? C17 C16 C15 123.1(2) . . ? C18 C17 C16 119.3(2) . . ? C18 C17 H17 120.4 . . ? C16 C17 H17 120.4 . . ? C17 C18 C19 119.6(2) . . ? C17 C18 H18 120.2 . . ? C19 C18 H18 120.2 . . ? C20 C19 C18 117.9(2) . . ? C20 C19 H19 121.0 . . ? C18 C19 H19 121.0 . . ? N4 C20 C19 123.2(2) . . ? N4 C20 H20 118.4 . . ? C19 C20 H20 118.4 . . ? C1 N1 C5 118.0(2) . . ? C1 N1 V2 120.67(17) . . ? C5 N1 V2 121.18(16) . . ? C10 N2 C6 118.4(2) . . ? C10 N2 V2 124.59(17) . . ? C6 N2 V2 116.85(16) . . ? C11 N3 C15 118.5(2) . . ? C11 N3 V3 124.52(17) . . ? C15 N3 V3 117.02(16) . . ? C20 N4 C16 118.8(2) . . ? C20 N4 V3 120.07(17) . . ? C16 N4 V3 120.96(16) . . ? C23 O9 H9A 109.5 . . ? O7 C21 H21C 109.5 . . ? O7 C21 H21B 109.5 . . ? H21C C21 H21B 109.5 . . ? O7 C21 H21A 109.5 . . ? H21C C21 H21A 109.5 . . ? H21B C21 H21A 109.5 . . ? O8 C22 H22C 109.5 . . ? O8 C22 H22B 109.5 . . ? H22C C22 H22B 109.5 . . ? O8 C22 H22A 109.5 . . ? H22C C22 H22A 109.5 . . ? H22B C22 H22A 109.5 . . ? O9 C23 H23A 109.5 . . ? O9 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? O9 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O9 H9A O2 0.84 2.05 2.855(3) 160.6 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.869 _refine_diff_density_min -0.484 _refine_diff_density_rms 0.087