# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_section_exptl_refinement 'In the complex 1, the atoms C13 and C14 are refined isotropically to avoid the non-postive definite. In complex 2 and 3, the hydrogen atoms of free and some coordinated water molecules can not be located due to the high degree of hydration and thermal motion, howerver they were included into the reported formulas.' _publ_contact_author_email hmc@fjirsm.ac.cn _publ_contact_author_name 'Maochun Hong' loop_ _publ_author_name 'Wentao Xu' 'Feilong Jiang' 'Youfu Zhou' 'Kecai Xiong' 'Lian Chen' 'Ming Yang' 'Rui Feng' 'Maochun Hong' ##### data_1 _database_code_depnum_ccdc_archive 'CCDC 825611' #TrackingRef '- crystal data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H57 N15 O33 V10 Zn2' _chemical_formula_sum 'C30 H57 N15 O33 V10 Zn2' _chemical_formula_weight 1796.05 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.492(5) _cell_length_b 11.830(4) _cell_length_c 13.682(5) _cell_angle_alpha 90.599(2) _cell_angle_beta 112.609(3) _cell_angle_gamma 115.2760(10) _cell_volume 1518.3(10) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3761 _cell_measurement_theta_min 3.0025 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.3000 _exptl_crystal_size_mid 0.2500 _exptl_crystal_size_min 0.2000 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.964 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 2.336 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7236 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _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 'Rigaku Mercury CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9693 _diffrn_reflns_av_R_equivalents 0.0192 _diffrn_reflns_av_sigmaI/netI 0.0304 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.80 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5112 _reflns_number_gt 4442 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2007)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2007)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2007)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0334P)^2^+1.3154P] 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 5112 _refine_ls_number_parameters 449 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0327 _refine_ls_wR_factor_ref 0.0776 _refine_ls_wR_factor_gt 0.0731 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.057 _refine_ls_shift/su_max 0.088 _refine_ls_shift/su_mean 0.001 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 Zn1 Zn 0.54950(4) 0.83235(4) 0.29550(3) 0.02936(11) Uani 1 1 d . . . V1 V 0.20925(6) 0.76852(5) 0.20352(4) 0.02776(14) Uani 1 1 d . . . V2 V -0.12083(6) 0.61358(5) 0.07648(4) 0.02902(14) Uani 1 1 d . . . V3 V 0.09418(5) 0.63118(4) -0.02945(4) 0.02113(13) Uani 1 1 d . . . V4 V 0.25026(5) 0.52837(5) 0.16199(4) 0.02297(13) Uani 1 1 d . . . V5 V 0.04788(6) 0.51596(5) 0.26431(4) 0.02943(14) Uani 1 1 d . . . O1 O 0.3178(2) 0.9137(2) 0.26551(19) 0.0415(6) Uani 1 1 d . . . O2 O 0.1722(2) 0.6877(2) 0.31008(16) 0.0305(5) Uani 1 1 d . . . O3 O 0.0382(2) 0.77072(19) 0.14557(17) 0.0301(5) Uani 1 1 d . . . O4 O -0.1065(2) 0.5541(2) 0.19879(17) 0.0310(5) Uani 1 1 d . . . O5 O -0.2473(2) 0.6496(2) 0.04920(19) 0.0407(6) Uani 1 1 d . . . O6 O 0.2029(2) 0.77643(19) 0.05259(16) 0.0266(5) Uani 1 1 d . . . O7 O 0.2207(2) 0.55925(18) 0.01246(15) 0.0224(4) Uani 1 1 d . . . O8 O -0.0866(2) 0.63997(18) -0.06004(16) 0.0236(5) Uani 1 1 d . . . O9 O 0.3787(2) 0.4945(2) 0.19100(17) 0.0330(5) Uani 1 1 d . . . O10 O 0.3426(2) 0.70210(19) 0.21757(16) 0.0258(5) Uani 1 1 d . . . O11 O 0.0583(2) 0.56266(17) 0.10121(15) 0.0206(4) Uani 1 1 d . . . O12 O 0.0880(2) 0.64966(19) -0.15324(16) 0.0272(5) Uani 1 1 d . . . O13 O 0.1905(2) 0.47894(19) 0.26597(16) 0.0273(5) Uani 1 1 d . . . O14 O 0.0337(3) 0.4772(2) 0.37243(19) 0.0441(6) Uani 1 1 d . . . O15 O 0.5690(3) 0.8811(2) 0.15157(18) 0.0436(6) Uani 1 1 d . . . O16 O 0.5446(3) 0.7992(2) 0.45137(18) 0.0393(6) Uani 1 1 d . . . O17 O -0.0773(8) 0.8682(6) -0.0951(5) 0.0673(19) Uani 0.50 1 d P A 2 N1 N 0.5414(3) 0.8161(3) -0.0154(2) 0.0428(8) Uani 1 1 d . . . N2 N 0.4833(3) 0.6683(3) 0.5608(2) 0.0419(7) Uani 1 1 d . . . N3 N 0.6903(3) 0.7622(3) 0.3281(2) 0.0371(7) Uani 1 1 d . . . N4 N 0.8161(4) 0.6721(3) 0.3157(3) 0.0544(9) Uani 1 1 d . . . H4N H 0.8444 0.6294 0.2877 0.065 Uiso 1 1 calc R . . N5 N 0.6483(3) 1.0201(3) 0.3631(2) 0.0331(7) Uani 1 1 d . . . N6 N 0.7444(3) 1.1957(3) 0.4820(2) 0.0421(8) Uani 1 1 d . . . H6N H 0.7703 1.2459 0.5406 0.050 Uiso 1 1 calc R . . N7 N -0.0477(6) 0.8367(5) -0.1649(5) 0.0387(15) Uani 0.50 1 d P B 1 H7N H -0.0677 0.7684 -0.1392 0.046 Uiso 0.50 1 calc PR B 1 N8 N 0.0057(16) 0.9834(13) -0.2633(12) 0.095(5) Uani 0.50 1 d P B 1 N9 N -0.0406(10) 0.9339(9) -0.2420(8) 0.051(2) Uani 0.50 1 d P A 2 C1 C 0.4704(5) 0.7099(5) -0.1081(3) 0.0674(14) Uani 1 1 d . . . H1A H 0.3978 0.6376 -0.0986 0.101 Uiso 1 1 calc R . . H1B H 0.5391 0.6873 -0.1132 0.101 Uiso 1 1 calc R . . H1C H 0.4278 0.7354 -0.1733 0.101 Uiso 1 1 calc R . . H5 H 0.4161 0.7133 0.0626 0.051(11) Uiso 1 1 d R . . H6 H 0.4146 0.6231 0.4061 0.050(11) Uiso 1 1 d R . . H7O8 H -0.0671 0.7193 -0.0519 0.060 Uiso 1 1 d R . . C2 C 0.6488(6) 0.9362(5) -0.0182(4) 0.096(2) Uani 1 1 d . . . H2A H 0.6814 0.9994 0.0438 0.144 Uiso 1 1 calc R . . H2B H 0.6090 0.9634 -0.0831 0.144 Uiso 1 1 calc R . . H2C H 0.7277 0.9256 -0.0170 0.144 Uiso 1 1 calc R . . C3 C 0.5100(4) 0.7998(4) 0.0675(3) 0.0407(9) Uani 1 1 d . . . C4 C 0.3874(5) 0.5445(4) 0.5709(4) 0.0724(14) Uani 1 1 d . . . H4A H 0.3245 0.4901 0.5003 0.109 Uiso 1 1 calc R . . H4B H 0.3325 0.5557 0.6045 0.109 Uiso 1 1 calc R . . H4C H 0.4422 0.5059 0.6145 0.109 Uiso 1 1 calc R . . C5 C 0.5874(5) 0.7643(5) 0.6589(3) 0.0802(17) Uani 1 1 d . . . H5A H 0.6513 0.8365 0.6419 0.120 Uiso 1 1 calc R . . H5B H 0.6405 0.7289 0.7091 0.120 Uiso 1 1 calc R . . H5C H 0.5396 0.7911 0.6906 0.120 Uiso 1 1 calc R . . C6 C 0.4718(4) 0.6957(4) 0.4658(3) 0.0373(8) Uani 1 1 d . . . C7 C 0.7067(4) 0.6933(4) 0.2634(3) 0.0440(9) Uani 1 1 d . . . H7 H 0.6482 0.6631 0.1896 0.053 Uiso 1 1 calc R . . C8 C 0.8754(5) 0.7288(5) 0.4202(4) 0.0716(15) Uani 1 1 d . . . H8 H 0.9546 0.7300 0.4759 0.086 Uiso 1 1 calc R . . C9 C 0.7968(4) 0.7842(5) 0.4284(3) 0.0606(12) Uani 1 1 d . . . H9 H 0.8126 0.8298 0.4919 0.073 Uiso 1 1 calc R . . C10 C 0.7716(4) 1.2328(4) 0.3960(3) 0.0454(9) Uani 1 1 d . . . H10 H 0.8209 1.3159 0.3889 0.054 Uiso 1 1 calc R . . C11 C 0.6714(4) 1.0695(3) 0.4605(3) 0.0379(8) Uani 1 1 d . . . H11 H 0.6405 1.0218 0.5072 0.046 Uiso 1 1 calc R . . C12 C 0.7117(4) 1.1234(3) 0.3232(3) 0.0407(9) Uani 1 1 d . . . H12 H 0.7132 1.1188 0.2558 0.049 Uiso 1 1 calc R . . C13 C -0.0516(13) 0.9379(13) -0.1337(12) 0.027(3) Uiso 0.50 1 d P B 1 H13 H -0.0755 0.9467 -0.0774 0.032 Uiso 0.50 1 calc PR B 1 C14 C -0.0190(7) 1.0259(7) -0.1881(6) 0.0286(16) Uiso 0.50 1 d P B 1 H14 H -0.0139 1.1057 -0.1760 0.034 Uiso 0.50 1 calc PR B 1 C15 C -0.008(3) 0.858(3) -0.242(2) 0.066(6) Uani 0.50 1 d P B 1 H15 H 0.0086 0.8029 -0.2773 0.080 Uiso 0.50 1 calc PR B 1 C16 C -0.0246(17) 1.0343(10) -0.3070(10) 0.098(5) Uani 0.50 1 d P A 2 H16A H -0.1134 1.0090 -0.3692 0.146 Uiso 0.50 1 calc PR A 2 H16B H 0.0480 1.0457 -0.3301 0.146 Uiso 0.50 1 calc PR A 2 H16C H 0.0020 1.1132 -0.2637 0.146 Uiso 0.50 1 calc PR A 2 C17 C -0.033(4) 0.829(3) -0.2752(19) 0.073(8) Uani 0.50 1 d P A 2 H17A H -0.1016 0.7545 -0.2642 0.110 Uiso 0.50 1 calc PR A 2 H17B H 0.0607 0.8392 -0.2342 0.110 Uiso 0.50 1 calc PR A 2 H17C H -0.0542 0.8203 -0.3507 0.110 Uiso 0.50 1 calc PR A 2 C18 C -0.062(2) 0.9540(19) -0.1554(14) 0.086(7) Uani 0.50 1 d P A 2 H18 H -0.0651 1.0283 -0.1380 0.103 Uiso 0.50 1 calc PR A 2 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 Zn1 0.0262(2) 0.0311(2) 0.0249(2) -0.00188(15) 0.00903(16) 0.01021(17) V1 0.0282(3) 0.0208(3) 0.0276(3) -0.0032(2) 0.0066(2) 0.0107(2) V2 0.0267(3) 0.0283(3) 0.0306(3) -0.0040(2) 0.0075(2) 0.0161(2) V3 0.0223(3) 0.0167(3) 0.0231(3) 0.0039(2) 0.0094(2) 0.0084(2) V4 0.0229(3) 0.0222(3) 0.0209(3) 0.0013(2) 0.0050(2) 0.0120(2) V5 0.0311(3) 0.0314(3) 0.0239(3) 0.0026(2) 0.0116(2) 0.0132(3) O1 0.0366(14) 0.0268(13) 0.0448(14) -0.0076(10) 0.0065(12) 0.0110(11) O2 0.0327(12) 0.0308(12) 0.0247(11) -0.0024(9) 0.0092(10) 0.0150(10) O3 0.0330(12) 0.0220(11) 0.0320(12) -0.0027(9) 0.0083(10) 0.0153(10) O4 0.0281(12) 0.0341(13) 0.0295(12) -0.0010(9) 0.0114(10) 0.0143(10) O5 0.0367(14) 0.0471(15) 0.0423(14) -0.0010(11) 0.0114(11) 0.0282(12) O6 0.0268(12) 0.0188(11) 0.0300(12) 0.0034(9) 0.0103(10) 0.0089(9) O7 0.0210(11) 0.0206(10) 0.0235(11) 0.0032(8) 0.0083(9) 0.0090(9) O8 0.0258(11) 0.0158(10) 0.0266(11) 0.0041(8) 0.0081(9) 0.0104(9) O9 0.0304(12) 0.0361(13) 0.0312(12) 0.0038(10) 0.0068(10) 0.0201(11) O10 0.0237(11) 0.0236(11) 0.0231(11) -0.0008(8) 0.0055(9) 0.0091(9) O11 0.0220(11) 0.0175(10) 0.0212(10) 0.0020(8) 0.0080(9) 0.0095(9) O12 0.0276(12) 0.0241(11) 0.0284(11) 0.0064(9) 0.0117(10) 0.0111(10) O13 0.0285(12) 0.0260(11) 0.0229(11) 0.0038(9) 0.0069(9) 0.0126(10) O14 0.0440(15) 0.0528(16) 0.0330(13) 0.0093(11) 0.0196(12) 0.0179(13) O15 0.0432(15) 0.0419(15) 0.0276(13) 0.0008(11) 0.0153(12) 0.0048(12) O16 0.0399(14) 0.0448(15) 0.0277(12) 0.0029(11) 0.0164(11) 0.0135(12) O17 0.126(6) 0.058(4) 0.051(4) 0.025(3) 0.047(4) 0.062(4) N1 0.0422(18) 0.0503(19) 0.0284(16) 0.0060(14) 0.0179(14) 0.0130(16) N2 0.0400(18) 0.0489(19) 0.0309(16) 0.0121(14) 0.0126(14) 0.0179(15) N3 0.0383(17) 0.0477(18) 0.0306(15) 0.0019(13) 0.0165(13) 0.0232(15) N4 0.067(2) 0.069(2) 0.067(2) 0.0222(19) 0.047(2) 0.049(2) N5 0.0307(15) 0.0355(16) 0.0280(15) -0.0037(12) 0.0106(12) 0.0130(13) N6 0.0409(18) 0.0424(18) 0.0353(17) -0.0101(14) 0.0098(14) 0.0191(15) N7 0.041(4) 0.028(3) 0.044(4) 0.014(3) 0.014(3) 0.018(3) N8 0.110(11) 0.056(10) 0.105(10) 0.030(7) 0.044(8) 0.030(8) N9 0.055(6) 0.029(5) 0.060(6) 0.009(4) 0.008(4) 0.027(5) C1 0.074(3) 0.077(3) 0.033(2) -0.001(2) 0.023(2) 0.021(3) C2 0.103(4) 0.077(4) 0.075(4) 0.014(3) 0.064(3) -0.009(3) C3 0.034(2) 0.042(2) 0.035(2) 0.0068(16) 0.0167(17) 0.0072(17) C4 0.074(3) 0.061(3) 0.063(3) 0.033(2) 0.022(3) 0.021(3) C5 0.078(4) 0.093(4) 0.027(2) 0.000(2) 0.015(2) 0.011(3) C6 0.037(2) 0.040(2) 0.0280(18) -0.0002(15) 0.0070(16) 0.0190(18) C7 0.052(2) 0.052(2) 0.039(2) 0.0063(17) 0.0248(19) 0.030(2) C8 0.063(3) 0.121(4) 0.058(3) 0.022(3) 0.025(2) 0.066(3) C9 0.051(3) 0.099(4) 0.038(2) 0.001(2) 0.012(2) 0.048(3) C10 0.041(2) 0.036(2) 0.048(2) 0.0018(17) 0.0165(19) 0.0117(18) C11 0.040(2) 0.040(2) 0.0291(18) -0.0035(15) 0.0131(16) 0.0159(17) C12 0.042(2) 0.041(2) 0.037(2) 0.0060(16) 0.0190(17) 0.0159(18) C15 0.081(9) 0.063(9) 0.075(17) 0.012(11) 0.036(12) 0.048(8) C16 0.180(15) 0.037(6) 0.091(9) 0.039(6) 0.071(9) 0.051(8) C17 0.14(2) 0.093(19) 0.052(12) 0.042(12) 0.062(15) 0.089(19) C18 0.131(13) 0.108(15) 0.054(11) 0.005(9) 0.034(9) 0.092(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 Zn1 O10 2.013(2) . ? Zn1 N5 2.018(3) . ? Zn1 N3 2.026(3) . ? Zn1 O15 2.125(2) . ? Zn1 O16 2.190(2) . ? V1 O1 1.597(2) . ? V1 O3 1.828(2) . ? V1 O2 1.839(2) . ? V1 O10 1.951(2) . ? V1 O6 2.042(2) . ? V1 O11 2.314(2) . ? V1 V3 3.0600(12) . ? V1 V5 3.0925(11) . ? V1 V2 3.1137(14) . ? V2 O5 1.597(2) . ? V2 O4 1.798(2) . ? V2 O3 1.850(2) . ? V2 O7 1.962(2) 2_565 ? V2 O8 2.053(2) . ? V2 O11 2.290(2) . ? V2 V4 3.1142(13) 2_565 ? V3 O6 1.680(2) . ? V3 O12 1.688(2) . ? V3 O7 1.896(2) . ? V3 O8 2.004(2) . ? V3 O11 2.082(2) . ? V3 O11 2.119(2) 2_565 ? V3 V5 3.0730(12) 2_565 ? V4 O9 1.598(2) . ? V4 O13 1.806(2) . ? V4 O10 1.847(2) . ? V4 O7 2.005(2) . ? V4 O8 2.043(2) 2_565 ? V4 O11 2.254(2) . ? V4 V5 3.0994(12) . ? V4 V2 3.1142(13) 2_565 ? V5 O14 1.601(2) . ? V5 O2 1.835(2) . ? V5 O13 1.861(2) . ? V5 O4 1.904(2) . ? V5 O12 2.022(2) 2_565 ? V5 O11 2.340(2) . ? V5 V3 3.0730(12) 2_565 ? O7 V2 1.962(2) 2_565 ? O8 V4 2.043(2) 2_565 ? O8 H7O8 0.8620 . ? O11 V3 2.119(2) 2_565 ? O12 V5 2.022(2) 2_565 ? O15 C3 1.236(4) . ? O16 C6 1.223(4) . ? O17 C18 1.311(19) . ? N1 C3 1.309(5) . ? N1 C2 1.443(5) . ? N1 C1 1.466(5) . ? N2 C6 1.313(5) . ? N2 C5 1.447(5) . ? N2 C4 1.457(5) . ? N3 C7 1.315(4) . ? N3 C9 1.370(5) . ? N4 C7 1.317(5) . ? N4 C8 1.341(6) . ? N4 H4N 0.8600 . ? N5 C11 1.329(4) . ? N5 C12 1.372(5) . ? N6 C11 1.322(5) . ? N6 C10 1.360(5) . ? N6 H6N 0.8600 . ? N7 C13 1.292(17) . ? N7 C15 1.28(3) . ? N7 H7N 0.8600 . ? N8 C14 1.315(16) . ? N8 C15 1.47(4) . ? N9 C17 1.36(3) . ? N9 C18 1.33(2) . ? N9 C16 1.481(12) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H5 1.1020 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6 0.9625 . ? C7 H7 0.9300 . ? C8 C9 1.357(6) . ? C8 H8 0.9300 . ? C9 H9 0.9300 . ? C10 C12 1.352(5) . ? C10 H10 0.9300 . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.295(17) . ? C13 H13 0.9300 . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18 0.9300 . ? 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 O10 Zn1 N5 132.71(10) . . ? O10 Zn1 N3 115.46(11) . . ? N5 Zn1 N3 111.48(12) . . ? O10 Zn1 O15 94.33(9) . . ? N5 Zn1 O15 89.45(11) . . ? N3 Zn1 O15 91.95(11) . . ? O10 Zn1 O16 90.18(9) . . ? N5 Zn1 O16 85.79(11) . . ? N3 Zn1 O16 88.18(11) . . ? O15 Zn1 O16 174.93(9) . . ? O1 V1 O3 102.19(11) . . ? O1 V1 O2 103.65(12) . . ? O3 V1 O2 93.02(10) . . ? O1 V1 O10 100.52(11) . . ? O3 V1 O10 155.94(9) . . ? O2 V1 O10 89.23(10) . . ? O1 V1 O6 101.10(11) . . ? O3 V1 O6 85.68(9) . . ? O2 V1 O6 154.91(9) . . ? O10 V1 O6 82.27(9) . . ? O1 V1 O11 174.82(11) . . ? O3 V1 O11 78.75(8) . . ? O2 V1 O11 81.32(8) . . ? O10 V1 O11 77.92(8) . . ? O6 V1 O11 73.84(8) . . ? O1 V1 V3 132.10(10) . . ? O3 V1 V3 80.63(7) . . ? O2 V1 V3 124.09(7) . . ? O10 V1 V3 78.31(6) . . ? O6 V1 V3 31.00(6) . . ? O11 V1 V3 42.84(5) . . ? O1 V1 V5 136.28(10) . . ? O3 V1 V5 85.34(8) . . ? O2 V1 V5 32.63(6) . . ? O10 V1 V5 83.73(7) . . ? O6 V1 V5 122.51(6) . . ? O11 V1 V5 48.71(5) . . ? V3 V1 V5 91.53(3) . . ? O1 V1 V2 134.36(9) . . ? O3 V1 V2 32.37(7) . . ? O2 V1 V2 81.92(7) . . ? O10 V1 V2 125.01(7) . . ? O6 V1 V2 83.76(6) . . ? O11 V1 V2 47.12(5) . . ? V3 V1 V2 63.542(19) . . ? V5 V1 V2 60.72(2) . . ? O5 V2 O4 103.72(12) . . ? O5 V2 O3 101.74(11) . . ? O4 V2 O3 94.62(10) . . ? O5 V2 O7 102.10(11) . 2_565 ? O4 V2 O7 92.38(9) . 2_565 ? O3 V2 O7 152.75(9) . 2_565 ? O5 V2 O8 100.51(11) . . ? O4 V2 O8 154.75(9) . . ? O3 V2 O8 87.28(9) . . ? O7 V2 O8 75.57(8) 2_565 . ? O5 V2 O11 175.26(11) . . ? O4 V2 O11 80.84(9) . . ? O3 V2 O11 78.97(9) . . ? O7 V2 O11 76.21(8) 2_565 . ? O8 V2 O11 74.81(7) . . ? O5 V2 V1 133.44(9) . . ? O4 V2 V1 82.99(7) . . ? O3 V2 V1 31.93(6) . . ? O7 V2 V1 123.88(6) 2_565 . ? O8 V2 V1 85.54(6) . . ? O11 V2 V1 47.76(5) . . ? O5 V2 V4 91.57(9) . 2_565 ? O4 V2 V4 131.13(8) . 2_565 ? O3 V2 V4 127.67(7) . 2_565 ? O7 V2 V4 38.78(6) 2_565 2_565 ? O8 V2 V4 40.40(6) . 2_565 ? O11 V2 V4 84.36(5) . 2_565 ? V1 V2 V4 118.74(2) . 2_565 ? O6 V3 O12 106.53(10) . . ? O6 V3 O7 99.37(10) . . ? O12 V3 O7 98.55(9) . . ? O6 V3 O8 95.34(9) . . ? O12 V3 O8 94.84(9) . . ? O7 V3 O8 156.36(9) . . ? O6 V3 O11 87.86(9) . . ? O12 V3 O11 165.32(9) . . ? O7 V3 O11 81.53(8) . . ? O8 V3 O11 80.64(8) . . ? O6 V3 O11 165.74(9) . 2_565 ? O12 V3 O11 87.21(9) . 2_565 ? O7 V3 O11 81.88(8) . 2_565 ? O8 V3 O11 79.40(8) . 2_565 ? O11 V3 O11 78.24(8) . 2_565 ? O6 V3 V1 38.78(7) . . ? O12 V3 V1 145.20(7) . . ? O7 V3 V1 92.12(6) . . ? O8 V3 V1 87.83(6) . . ? O11 V3 V1 49.09(6) . . ? O11 V3 V1 127.22(6) 2_565 . ? O6 V3 V5 144.18(8) . 2_565 ? O12 V3 V5 37.73(7) . 2_565 ? O7 V3 V5 91.08(6) . 2_565 ? O8 V3 V5 87.67(6) . 2_565 ? O11 V3 V5 127.71(6) . 2_565 ? O11 V3 V5 49.49(5) 2_565 2_565 ? V1 V3 V5 174.94(2) . 2_565 ? O9 V4 O13 103.17(11) . . ? O9 V4 O10 103.07(11) . . ? O13 V4 O10 96.65(10) . . ? O9 V4 O7 99.79(10) . . ? O13 V4 O7 153.47(9) . . ? O10 V4 O7 90.89(9) . . ? O9 V4 O8 99.14(10) . 2_565 ? O13 V4 O8 88.45(9) . 2_565 ? O10 V4 O8 155.37(9) . 2_565 ? O7 V4 O8 74.85(8) . 2_565 ? O9 V4 O11 173.23(9) . . ? O13 V4 O11 80.98(9) . . ? O10 V4 O11 81.55(8) . . ? O7 V4 O11 75.00(8) . . ? O8 V4 O11 75.46(8) 2_565 . ? O9 V4 V5 135.90(9) . . ? O13 V4 V5 32.86(7) . . ? O10 V4 V5 85.16(7) . . ? O7 V4 V5 123.62(6) . . ? O8 V4 V5 86.27(7) 2_565 . ? O11 V4 V5 48.75(6) . . ? O9 V4 V2 89.34(8) . 2_565 ? O13 V4 V2 129.06(7) . 2_565 ? O10 V4 V2 128.68(7) . 2_565 ? O7 V4 V2 37.79(6) . 2_565 ? O8 V4 V2 40.62(6) 2_565 2_565 ? O11 V4 V2 83.90(5) . 2_565 ? V5 V4 V2 119.27(3) . 2_565 ? O14 V5 O2 102.18(12) . . ? O14 V5 O13 102.93(12) . . ? O2 V5 O13 91.57(10) . . ? O14 V5 O4 101.70(12) . . ? O2 V5 O4 89.65(10) . . ? O13 V5 O4 154.49(10) . . ? O14 V5 O12 102.87(12) . 2_565 ? O2 V5 O12 154.83(10) . 2_565 ? O13 V5 O12 85.31(9) . 2_565 ? O4 V5 O12 82.85(9) . 2_565 ? O14 V5 O11 177.05(11) . . ? O2 V5 O11 80.68(8) . . ? O13 V5 O11 77.60(8) . . ? O4 V5 O11 77.46(8) . . ? O12 V5 O11 74.25(8) 2_565 . ? O14 V5 V3 133.58(10) . 2_565 ? O2 V5 V3 124.15(7) . 2_565 ? O13 V5 V3 80.42(7) . 2_565 ? O4 V5 V3 77.85(7) . 2_565 ? O12 V5 V3 30.73(6) 2_565 2_565 ? O11 V5 V3 43.53(5) . 2_565 ? O14 V5 V1 134.84(9) . . ? O2 V5 V1 32.70(7) . . ? O13 V5 V1 85.30(7) . . ? O4 V5 V1 82.05(8) . . ? O12 V5 V1 122.16(7) 2_565 . ? O11 V5 V1 47.99(5) . . ? V3 V5 V1 91.45(3) 2_565 . ? O14 V5 V4 134.42(10) . . ? O2 V5 V4 81.16(7) . . ? O13 V5 V4 31.77(7) . . ? O4 V5 V4 123.86(7) . . ? O12 V5 V4 83.19(7) 2_565 . ? O11 V5 V4 46.42(5) . . ? V3 V5 V4 63.49(3) 2_565 . ? V1 V5 V4 61.19(2) . . ? V5 O2 V1 114.67(11) . . ? V1 O3 V2 115.70(11) . . ? V2 O4 V5 115.80(12) . . ? V3 O6 V1 110.22(11) . . ? V3 O7 V2 108.18(10) . 2_565 ? V3 O7 V4 107.29(10) . . ? V2 O7 V4 103.44(9) 2_565 . ? V3 O8 V4 106.71(9) . 2_565 ? V3 O8 V2 106.51(9) . . ? V4 O8 V2 98.98(9) 2_565 . ? V3 O8 H7O8 108.2 . . ? V4 O8 H7O8 136.8 2_565 . ? V2 O8 H7O8 94.8 . . ? V4 O10 V1 112.11(10) . . ? V4 O10 Zn1 133.29(11) . . ? V1 O10 Zn1 114.51(10) . . ? V3 O11 V3 101.76(8) . 2_565 ? V3 O11 V4 92.80(8) . . ? V3 O11 V4 95.85(8) 2_565 . ? V3 O11 V2 95.97(8) . . ? V3 O11 V2 90.16(8) 2_565 . ? V4 O11 V2 168.15(9) . . ? V3 O11 V1 88.07(7) . . ? V3 O11 V1 169.50(10) 2_565 . ? V4 O11 V1 87.23(7) . . ? V2 O11 V1 85.12(7) . . ? V3 O11 V5 171.15(10) . . ? V3 O11 V5 86.98(7) 2_565 . ? V4 O11 V5 84.83(7) . . ? V2 O11 V5 85.30(7) . . ? V1 O11 V5 83.30(7) . . ? V3 O12 V5 111.54(11) . 2_565 ? V4 O13 V5 115.36(11) . . ? C3 O15 Zn1 121.9(2) . . ? C6 O16 Zn1 124.0(2) . . ? C3 N1 C2 122.1(3) . . ? C3 N1 C1 120.4(3) . . ? C2 N1 C1 117.5(3) . . ? C6 N2 C5 120.3(4) . . ? C6 N2 C4 121.6(3) . . ? C5 N2 C4 118.0(3) . . ? C7 N3 C9 104.8(3) . . ? C7 N3 Zn1 130.6(2) . . ? C9 N3 Zn1 124.6(2) . . ? C7 N4 C8 108.0(3) . . ? C7 N4 H4N 126.0 . . ? C8 N4 H4N 126.0 . . ? C11 N5 C12 104.9(3) . . ? C11 N5 Zn1 126.2(3) . . ? C12 N5 Zn1 128.7(2) . . ? C11 N6 C10 108.7(3) . . ? C11 N6 H6N 125.7 . . ? C10 N6 H6N 125.7 . . ? C13 N7 C15 106.9(17) . . ? C13 N7 H7N 126.5 . . ? C15 N7 H7N 126.5 . . ? C14 N8 C15 102.9(15) . . ? C17 N9 C18 125.3(16) . . ? C17 N9 C16 117.9(16) . . ? C18 N9 C16 116.8(12) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? O15 C3 N1 125.2(3) . . ? O15 C3 H5 113.7 . . ? N1 C3 H5 120.7 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O16 C6 N2 125.0(3) . . ? O16 C6 H6 118.9 . . ? N2 C6 H6 115.0 . . ? N3 C7 N4 111.9(3) . . ? N3 C7 H7 124.1 . . ? N4 C7 H7 124.1 . . ? N4 C8 C9 106.2(4) . . ? N4 C8 H8 126.9 . . ? C9 C8 H8 126.9 . . ? C8 C9 N3 109.1(4) . . ? C8 C9 H9 125.4 . . ? N3 C9 H9 125.4 . . ? C12 C10 N6 105.3(3) . . ? C12 C10 H10 127.3 . . ? N6 C10 H10 127.3 . . ? N6 C11 N5 110.9(3) . . ? N6 C11 H11 124.5 . . ? N5 C11 H11 124.5 . . ? C10 C12 N5 110.1(3) . . ? C10 C12 H12 124.9 . . ? N5 C12 H12 124.9 . . ? C14 C13 N7 113.6(14) . . ? C14 C13 H13 123.2 . . ? N7 C13 H13 123.2 . . ? C13 C14 N8 108.5(11) . . ? C13 C14 H14 125.7 . . ? N8 C14 H14 125.7 . . ? N7 C15 N8 108(2) . . ? N7 C15 H15 126.1 . . ? N8 C15 H15 126.1 . . ? N9 C16 H16A 109.5 . . ? N9 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N9 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N9 C17 H17A 109.4 . . ? N9 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N9 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? O17 C18 N9 119.6(15) . . ? O17 C18 H18 120.2 . . ? N9 C18 H18 120.2 . . ? 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 N6 H6N O2 0.86 1.93 2.758(4) 162.1 2_676 N4 H4N O4 0.86 1.88 2.721(4) 166.4 1_655 _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.377 _refine_diff_density_min -0.485 _refine_diff_density_rms 0.068 data_2 _database_code_depnum_ccdc_archive 'CCDC 825612' #TrackingRef '- crystal data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C14 H33 N21 O44 V10 Zn3' _chemical_formula_sum 'C14 H33 N21 O44 V10 Zn3' _chemical_formula_weight 1905.17 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' Zn Zn 0.2839 1.4301 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.873(5) _cell_length_b 14.831(6) _cell_length_c 16.274(7) _cell_angle_alpha 86.834(13) _cell_angle_beta 72.509(8) _cell_angle_gamma 78.682(12) _cell_volume 2906(2) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 2633 _cell_measurement_theta_min 2.0847 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.2500 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.1800 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.200 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1912 _exptl_absorpt_coefficient_mu 2.864 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5220 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _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 'Rigaku Mercury CCD area-detector' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22948 _diffrn_reflns_av_R_equivalents 0.0463 _diffrn_reflns_av_sigmaI/netI 0.0936 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 27.48 _reflns_number_total 13239 _reflns_number_gt 9207 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku, 2000)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.0608P)^2^+6.8708P] 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 SHELXL _refine_ls_extinction_coef ? _refine_ls_number_reflns 13239 _refine_ls_number_parameters 829 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0957 _refine_ls_R_factor_gt 0.0630 _refine_ls_wR_factor_ref 0.1711 _refine_ls_wR_factor_gt 0.1442 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 Zn1 Zn 0.46083(6) 0.21907(5) 0.28136(5) 0.02340(17) Uani 1 1 d . . . Zn2 Zn 0.76402(6) 0.23699(5) 0.23505(5) 0.02353(17) Uani 1 1 d . . . Zn3 Zn 1.06657(6) 0.25014(5) 0.19971(5) 0.02452(17) Uani 1 1 d . . . V6 V 1.29353(8) -0.22659(7) 0.15782(6) 0.0182(2) Uani 1 1 d . . . V1 V 1.23384(9) -0.09065(7) 0.31826(6) 0.0196(2) Uani 1 1 d . . . V5 V 1.21398(9) -0.29717(7) 0.35785(6) 0.0197(2) Uani 1 1 d . . . V4 V 1.05999(9) -0.28529(7) 0.23195(7) 0.0211(2) Uani 1 1 d . . . V8 V 1.27594(9) -0.43440(7) 0.19245(7) 0.0207(2) Uani 1 1 d . . . V3 V 1.08079(9) -0.07843(7) 0.20041(7) 0.0217(2) Uani 1 1 d . . . V7 V 1.44607(9) -0.23839(7) 0.28169(6) 0.0201(2) Uani 1 1 d . . . V10 V 1.50620(9) -0.37584(7) 0.12865(7) 0.0233(2) Uani 1 1 d . . . V2 V 1.00209(9) -0.14777(7) 0.38462(7) 0.0223(2) Uani 1 1 d . . . V9 V 1.42647(9) -0.44608(7) 0.31257(7) 0.0228(2) Uani 1 1 d . . . O15 O 1.3578(3) -0.1525(3) 0.2185(3) 0.0201(8) Uani 1 1 d . . . O13 O 1.2104(3) -0.3175(3) 0.1472(2) 0.0200(9) Uani 1 1 d . . . O11 O 1.2254(4) -0.1381(3) 0.1126(3) 0.0215(9) Uani 1 1 d . . . O16 O 1.2963(3) -0.2074(3) 0.3683(2) 0.0183(8) Uani 1 1 d . . . O22 O 1.4766(3) -0.3440(3) 0.3422(3) 0.0207(9) Uani 1 1 d . . . O8 O 1.0272(3) -0.1810(3) 0.1743(3) 0.0219(9) Uani 1 1 d . . . O27 O 1.5354(3) -0.4591(3) 0.2091(3) 0.0240(9) Uani 1 1 d . . . O24 O 1.3368(4) -0.5037(3) 0.2695(3) 0.0245(9) Uani 1 1 d . . . O5 O 0.9718(4) -0.0656(3) 0.3043(3) 0.0235(9) Uani 1 1 d . . . O2 O 1.1046(4) -0.0813(3) 0.4044(3) 0.0221(9) Uani 1 1 d . . . O3 O 1.1721(4) -0.0220(3) 0.2431(3) 0.0239(9) Uani 1 1 d . . . O25 O 1.4038(4) -0.4411(3) 0.1066(3) 0.0232(9) Uani 1 1 d . . . O10 O 1.1609(3) -0.1984(3) 0.2736(2) 0.0183(8) Uani 1 1 d . . . O14 O 1.1486(3) -0.3745(3) 0.2964(3) 0.0217(9) Uani 1 1 d . . . O18 O 1.2813(4) -0.3875(3) 0.4019(3) 0.0243(9) Uani 1 1 d . . . O20 O 1.4140(4) -0.2674(3) 0.0820(3) 0.0236(9) Uani 1 1 d . . . O19 O 1.3447(3) -0.3270(3) 0.2421(2) 0.0185(8) Uani 1 1 d . . . O23 O 1.5449(3) -0.2815(3) 0.1802(3) 0.0243(9) Uani 1 1 d . . . O29 O 0.3187(4) 0.3254(3) 0.3148(3) 0.0281(10) Uani 1 1 d . . . O1 O 1.2980(4) -0.0206(3) 0.3473(3) 0.0285(10) Uani 1 1 d . . . N17 N 0.9754(4) 0.1784(4) 0.3026(3) 0.0231(11) Uani 1 1 d . . . O7 O 0.9631(4) -0.2422(3) 0.3350(3) 0.0240(9) Uani 1 1 d . . . O34 O 1.2026(4) 0.1403(3) 0.1769(3) 0.0267(10) Uani 1 1 d . . . O9 O 1.0940(3) -0.2568(3) 0.4335(3) 0.0226(9) Uani 1 1 d . . . N7 N 0.5262(4) 0.2665(3) 0.3733(3) 0.0227(11) Uani 1 1 d . . . N11 N 1.0046(4) 0.2055(3) 0.1044(3) 0.0213(10) Uani 1 1 d . . . O28 O 1.6100(4) -0.3998(3) 0.0442(3) 0.0343(11) Uani 1 1 d . . . O12 O 0.9955(4) -0.3534(3) 0.2011(3) 0.0317(11) Uani 1 1 d . . . O6 O 1.0351(4) -0.0016(3) 0.1409(3) 0.0322(11) Uani 1 1 d . . . O17 O 1.5090(4) -0.1696(3) 0.3130(3) 0.0299(10) Uani 1 1 d . . . O21 O 1.2115(4) -0.5046(3) 0.1636(3) 0.0294(10) Uani 1 1 d . . . O4 O 0.8976(4) -0.1230(3) 0.4688(3) 0.0321(11) Uani 1 1 d . . . O33 O 1.1767(4) 0.3215(3) 0.1068(3) 0.0381(12) Uani 1 1 d . . . O31 O 0.4048(4) 0.1599(3) 0.1914(3) 0.0364(12) Uani 1 1 d . . . N1 N 0.5942(4) 0.1032(3) 0.2594(3) 0.0246(11) Uani 1 1 d . . . O30 O 0.3554(4) 0.1458(3) 0.3752(3) 0.0372(12) Uani 1 1 d . . . N9 N 0.5532(5) 0.3152(4) 0.4875(3) 0.0266(12) Uani 1 1 d . . . H9N H 0.5420 0.3321 0.5409 0.032 Uiso 1 1 calc R . . N14 N 0.9352(4) 0.3677(4) 0.2193(3) 0.0262(11) Uani 1 1 d . . . N12N N 0.9849(5) 0.1714(4) -0.0171(3) 0.0326(13) Uani 1 1 d . . . H12N H 0.9992 0.1593 -0.0721 0.039 Uiso 1 1 calc R . . N4 N 0.5446(4) 0.2958(4) 0.1788(3) 0.0256(11) Uani 1 1 d . . . N10 N 0.8959(4) 0.1986(4) 0.1182(3) 0.0246(11) Uani 1 1 d . . . N16 N 0.8670(4) 0.1689(4) 0.3140(3) 0.0246(11) Uani 1 1 d . . . N20 N 1.5467(5) 0.0037(4) 0.0905(4) 0.0376(14) Uani 1 1 d . . . C5 C 0.4786(5) 0.2916(4) 0.4538(4) 0.0261(13) Uani 1 1 d . . . H5 H 0.4026 0.2930 0.4840 0.031 Uiso 1 1 calc R . . N8 N 0.6353(4) 0.2767(4) 0.3537(3) 0.0253(11) Uani 1 1 d . . . O32 O 1.1219(4) 0.3076(4) 0.2919(3) 0.0447(13) Uani 1 1 d . . . N5 N 0.6536(4) 0.3050(4) 0.1617(3) 0.0268(12) Uani 1 1 d . . . N13 N 0.8254(5) 0.3641(4) 0.2326(4) 0.0272(12) Uani 1 1 d . . . N6 N 0.5881(5) 0.3801(4) 0.0637(3) 0.0305(13) Uani 1 1 d . . . H6N H 0.5841 0.4137 0.0181 0.037 Uiso 1 1 calc R . . N2 N 0.7040(4) 0.1092(4) 0.2360(4) 0.0271(12) Uani 1 1 d . . . N15 N 0.8404(6) 0.5069(4) 0.2266(4) 0.0439(16) Uani 1 1 d . . . H15N H 0.8236 0.5674 0.2263 0.053 Uiso 1 1 calc R . . C1 C 0.5886(6) 0.0163(4) 0.2728(5) 0.0335(16) Uani 1 1 d . . . H1 H 0.5219 -0.0075 0.2903 0.040 Uiso 1 1 calc R . . N19 N 1.5266(5) -0.0844(4) 0.0978(4) 0.0341(13) Uani 1 1 d . . . H19N H 1.4715 -0.1031 0.1371 0.041 Uiso 1 1 calc R . . N3 N 0.6915(5) -0.0343(4) 0.2580(4) 0.0389(15) Uani 1 1 d . . . H3N H 0.7097 -0.0944 0.2621 0.047 Uiso 1 1 calc R . . N18 N 0.9178(5) 0.1096(4) 0.4238(3) 0.0310(13) Uani 1 1 d . . . H18N H 0.9164 0.0822 0.4733 0.037 Uiso 1 1 calc R . . C12 C 1.0023(6) 0.1416(5) 0.3704(4) 0.0313(15) Uani 1 1 d . . . H12 H 1.0723 0.1384 0.3797 0.038 Uiso 1 1 calc R . . C2 C 0.7615(6) 0.0267(5) 0.2354(5) 0.0389(17) Uani 1 1 d . . . H2 H 0.8400 0.0113 0.2214 0.047 Uiso 1 1 calc R . . C7 C 0.8882(6) 0.1768(5) 0.0435(4) 0.0360(17) Uani 1 1 d . . . H7 H 0.8222 0.1664 0.0341 0.043 Uiso 1 1 calc R . . C3 C 0.5076(6) 0.3432(4) 0.1188(4) 0.0296(15) Uani 1 1 d . . . H3 H 0.4341 0.3502 0.1153 0.036 Uiso 1 1 calc R . . C6 C 0.6472(6) 0.3076(5) 0.4236(4) 0.0326(15) Uani 1 1 d . . . H6 H 0.7138 0.3225 0.4279 0.039 Uiso 1 1 calc R . . C4 C 0.6773(6) 0.3545(5) 0.0935(4) 0.0323(15) Uani 1 1 d . . . H4 H 0.7477 0.3709 0.0676 0.039 Uiso 1 1 calc R . . C11 C 0.8357(6) 0.1270(5) 0.3883(4) 0.0302(14) Uani 1 1 d . . . H11 H 0.7646 0.1114 0.4129 0.036 Uiso 1 1 calc R . . C14 C 1.6031(7) -0.1376(5) 0.0365(5) 0.0395(18) Uani 1 1 d . . . H14 H 1.6053 -0.2009 0.0282 0.047 Uiso 1 1 calc R . . C8 C 1.0560(6) 0.1881(5) 0.0228(4) 0.0308(15) Uani 1 1 d . . . H8 H 1.1327 0.1875 -0.0042 0.037 Uiso 1 1 calc R . . C10 C 0.9412(6) 0.4550(5) 0.2162(5) 0.0350(16) Uani 1 1 d . . . H10 H 1.0074 0.4782 0.2078 0.042 Uiso 1 1 calc R . . C9 C 0.7696(6) 0.4473(5) 0.2377(5) 0.0373(17) Uani 1 1 d . . . H9 H 0.6917 0.4641 0.2477 0.045 Uiso 1 1 calc R . . N21 N 1.6761(5) -0.0885(4) -0.0116(4) 0.0378(14) Uani 1 1 d . . . C13 C 1.6369(6) -0.0031(5) 0.0240(5) 0.0380(17) Uani 1 1 d . . . H13 H 1.6718 0.0478 0.0027 0.046 Uiso 1 1 calc R . . O26 O 1.4727(4) -0.5239(3) 0.3719(3) 0.0364(12) Uani 1 1 d . . . O1W O 1.7579(4) -0.2055(3) 0.3215(3) 0.0416(13) Uani 1 1 d . . . O2W O 1.8907(5) -0.5731(5) -0.0155(4) 0.0574(16) Uani 1 1 d . . . O3W O 1.8874(5) -0.3933(4) 0.0288(4) 0.0569(16) Uani 1 1 d . . . O4W O 1.6202(5) -0.1034(4) 0.4668(3) 0.0462(13) Uani 1 1 d . . . O5W O 0.9854(5) 0.5053(4) 0.5954(4) 0.0603(17) Uani 1 1 d . . . O7W O 1.3145(4) 0.3647(4) 0.6435(4) 0.0527(15) Uani 1 1 d . . . O6W O 0.1953(6) 0.3134(5) 0.4873(4) 0.0674(18) Uani 1 1 d . . . O9W O 1.7622(5) -0.2782(6) 0.1556(5) 0.091(3) Uani 1 1 d . . . O8W O 1.2299(11) 0.5108(7) 0.5580(5) 0.140(5) Uani 1 1 d . . . O10W O 1.3931(5) -0.0801(4) 0.4938(3) 0.0488(14) Uani 1 1 d . . . HA29 H 0.3067 0.3791 0.2930 0.059 Uiso 1 1 d R . . HB29 H 0.3068 0.3340 0.3689 0.059 Uiso 1 1 d R . . HA34 H 1.2110 0.0832 0.1893 0.059 Uiso 1 1 d R . . HB34 H 1.2506 0.1458 0.1284 0.059 Uiso 1 1 d R . . HA33 H 1.2164 0.3593 0.1128 0.059 Uiso 1 1 d R . . HB33 H 1.1983 0.3069 0.0533 0.059 Uiso 1 1 d R . . HA31 H 0.3813 0.1927 0.1570 0.059 Uiso 1 1 d R . . HB31 H 0.4471 0.1129 0.1636 0.059 Uiso 1 1 d R . . HA30 H 0.2983 0.1761 0.4129 0.059 Uiso 1 1 d R . . HB30 H 0.3315 0.1046 0.3550 0.059 Uiso 1 1 d R . . HA32 H 1.1610 0.2757 0.3221 0.059 Uiso 1 1 d R . . HB32 H 1.0735 0.3556 0.3144 0.059 Uiso 1 1 d 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 Zn1 0.0214(4) 0.0231(4) 0.0264(4) -0.0005(3) -0.0080(3) -0.0042(3) Zn2 0.0204(4) 0.0268(4) 0.0237(4) 0.0007(3) -0.0071(3) -0.0045(3) Zn3 0.0225(4) 0.0279(4) 0.0244(4) 0.0005(3) -0.0084(3) -0.0053(3) V6 0.0195(5) 0.0176(5) 0.0168(5) 0.0001(4) -0.0052(4) -0.0022(4) V1 0.0222(5) 0.0153(5) 0.0220(5) -0.0018(4) -0.0081(4) -0.0021(4) V5 0.0211(5) 0.0175(5) 0.0191(5) 0.0024(4) -0.0056(4) -0.0019(4) V4 0.0217(5) 0.0188(5) 0.0242(5) -0.0018(4) -0.0090(4) -0.0036(4) V8 0.0241(6) 0.0158(5) 0.0237(5) -0.0013(4) -0.0095(4) -0.0030(4) V3 0.0253(6) 0.0173(5) 0.0226(5) -0.0003(4) -0.0103(4) 0.0010(4) V7 0.0206(5) 0.0181(5) 0.0231(5) -0.0014(4) -0.0088(4) -0.0031(4) V10 0.0222(6) 0.0221(5) 0.0226(5) -0.0033(4) -0.0044(4) 0.0002(4) V2 0.0211(5) 0.0233(5) 0.0204(5) -0.0025(4) -0.0051(4) -0.0004(4) V9 0.0266(6) 0.0163(5) 0.0266(5) 0.0016(4) -0.0120(5) -0.0004(4) O15 0.023(2) 0.0153(19) 0.023(2) 0.0005(16) -0.0072(17) -0.0033(17) O13 0.019(2) 0.021(2) 0.019(2) -0.0069(16) -0.0069(17) 0.0019(17) O11 0.025(2) 0.017(2) 0.021(2) 0.0040(16) -0.0058(17) -0.0031(17) O16 0.016(2) 0.018(2) 0.019(2) -0.0029(16) -0.0054(16) -0.0001(16) O22 0.020(2) 0.019(2) 0.023(2) -0.0023(16) -0.0104(17) 0.0024(17) O8 0.025(2) 0.020(2) 0.022(2) -0.0013(17) -0.0102(18) -0.0026(18) O27 0.020(2) 0.025(2) 0.027(2) -0.0015(18) -0.0105(18) 0.0013(18) O24 0.028(2) 0.016(2) 0.030(2) 0.0005(17) -0.0121(19) -0.0013(18) O5 0.024(2) 0.024(2) 0.020(2) -0.0037(17) -0.0047(18) -0.0014(18) O2 0.027(2) 0.019(2) 0.020(2) -0.0041(16) -0.0090(18) 0.0011(18) O3 0.031(3) 0.015(2) 0.027(2) -0.0004(17) -0.0117(19) 0.0011(18) O25 0.029(2) 0.018(2) 0.019(2) -0.0046(16) -0.0044(18) 0.0010(18) O10 0.019(2) 0.0153(19) 0.019(2) -0.0009(16) -0.0054(16) 0.0001(16) O14 0.022(2) 0.019(2) 0.025(2) -0.0001(17) -0.0095(18) -0.0010(17) O18 0.033(3) 0.019(2) 0.021(2) 0.0037(17) -0.0090(19) -0.0056(19) O20 0.024(2) 0.022(2) 0.021(2) -0.0027(17) -0.0039(18) -0.0009(18) O19 0.020(2) 0.0144(19) 0.021(2) -0.0047(16) -0.0086(17) 0.0021(16) O23 0.020(2) 0.026(2) 0.025(2) -0.0003(18) -0.0042(18) -0.0046(18) O29 0.029(3) 0.020(2) 0.035(3) 0.0005(19) -0.012(2) -0.0024(19) O1 0.033(3) 0.019(2) 0.036(3) -0.0030(19) -0.011(2) -0.0099(19) N17 0.020(3) 0.031(3) 0.020(3) 0.006(2) -0.008(2) -0.008(2) O7 0.025(2) 0.020(2) 0.027(2) 0.0007(17) -0.0106(19) -0.0012(18) O34 0.024(2) 0.023(2) 0.030(2) 0.0039(18) -0.0035(19) -0.0036(18) O9 0.022(2) 0.022(2) 0.021(2) 0.0001(17) -0.0031(17) -0.0010(18) N7 0.020(3) 0.024(3) 0.022(3) -0.006(2) -0.002(2) -0.002(2) N11 0.020(3) 0.026(3) 0.020(2) -0.001(2) -0.008(2) -0.006(2) O28 0.029(3) 0.033(3) 0.035(3) -0.007(2) -0.002(2) -0.002(2) O12 0.029(3) 0.029(2) 0.043(3) -0.006(2) -0.018(2) -0.005(2) O6 0.040(3) 0.028(2) 0.030(2) 0.006(2) -0.015(2) -0.002(2) O17 0.031(3) 0.028(2) 0.035(3) -0.001(2) -0.014(2) -0.008(2) O21 0.035(3) 0.022(2) 0.034(3) -0.0039(19) -0.013(2) -0.006(2) O4 0.026(3) 0.041(3) 0.023(2) -0.003(2) -0.0021(19) 0.002(2) O33 0.041(3) 0.036(3) 0.034(3) 0.004(2) -0.002(2) -0.017(2) O31 0.034(3) 0.040(3) 0.039(3) -0.015(2) -0.016(2) -0.002(2) N1 0.020(3) 0.020(3) 0.034(3) 0.001(2) -0.009(2) -0.005(2) O30 0.040(3) 0.029(3) 0.039(3) -0.002(2) -0.003(2) -0.014(2) N9 0.027(3) 0.032(3) 0.020(3) -0.004(2) -0.007(2) -0.002(2) N14 0.023(3) 0.023(3) 0.032(3) 0.003(2) -0.006(2) -0.006(2) N12N 0.036(3) 0.042(3) 0.020(3) -0.007(2) -0.010(2) -0.004(3) N4 0.027(3) 0.030(3) 0.020(3) 0.003(2) -0.010(2) -0.003(2) N10 0.020(3) 0.031(3) 0.023(3) 0.000(2) -0.009(2) -0.002(2) N16 0.019(3) 0.030(3) 0.024(3) 0.003(2) -0.005(2) -0.004(2) N20 0.039(4) 0.035(3) 0.038(3) -0.002(3) -0.006(3) -0.014(3) C5 0.021(3) 0.028(3) 0.026(3) -0.005(3) -0.002(3) -0.006(3) N8 0.025(3) 0.032(3) 0.020(3) -0.002(2) -0.006(2) -0.008(2) O32 0.033(3) 0.060(4) 0.046(3) -0.010(3) -0.020(2) -0.007(3) N5 0.023(3) 0.032(3) 0.026(3) 0.004(2) -0.011(2) -0.005(2) N13 0.024(3) 0.022(3) 0.035(3) 0.001(2) -0.010(2) -0.005(2) N6 0.042(4) 0.025(3) 0.025(3) 0.004(2) -0.013(3) -0.004(3) N2 0.020(3) 0.025(3) 0.035(3) 0.002(2) -0.009(2) 0.000(2) N15 0.045(4) 0.019(3) 0.065(5) -0.009(3) -0.015(3) 0.001(3) C1 0.035(4) 0.022(3) 0.042(4) -0.003(3) -0.012(3) -0.001(3) N19 0.032(3) 0.037(3) 0.031(3) 0.010(3) -0.003(3) -0.014(3) N3 0.046(4) 0.017(3) 0.052(4) 0.001(3) -0.017(3) 0.001(3) N18 0.038(3) 0.031(3) 0.025(3) 0.003(2) -0.013(3) -0.002(3) C12 0.030(4) 0.038(4) 0.028(3) 0.002(3) -0.014(3) -0.003(3) C2 0.030(4) 0.031(4) 0.058(5) -0.003(3) -0.018(4) -0.001(3) C7 0.031(4) 0.046(4) 0.032(4) -0.012(3) -0.013(3) 0.000(3) C3 0.038(4) 0.027(3) 0.028(3) 0.003(3) -0.019(3) -0.003(3) C6 0.031(4) 0.040(4) 0.030(4) -0.003(3) -0.014(3) -0.007(3) C4 0.029(4) 0.039(4) 0.031(4) 0.007(3) -0.012(3) -0.008(3) C11 0.027(4) 0.031(3) 0.029(3) 0.005(3) -0.003(3) -0.006(3) C14 0.049(5) 0.026(4) 0.038(4) -0.005(3) -0.007(4) 0.000(3) C8 0.025(4) 0.039(4) 0.026(3) -0.011(3) -0.004(3) -0.004(3) C10 0.034(4) 0.026(3) 0.045(4) -0.003(3) -0.007(3) -0.011(3) C9 0.027(4) 0.028(4) 0.055(5) -0.003(3) -0.013(3) 0.003(3) N21 0.030(3) 0.036(3) 0.042(4) 0.008(3) -0.003(3) -0.008(3) C13 0.038(4) 0.038(4) 0.035(4) -0.001(3) 0.001(3) -0.017(3) O26 0.048(3) 0.027(2) 0.038(3) 0.007(2) -0.023(2) 0.000(2) O1W 0.029(3) 0.037(3) 0.059(3) 0.003(2) -0.020(3) 0.001(2) O2W 0.053(4) 0.080(4) 0.042(3) 0.008(3) -0.010(3) -0.026(3) O3W 0.068(4) 0.050(4) 0.054(4) 0.007(3) -0.021(3) -0.011(3) O4W 0.050(4) 0.047(3) 0.040(3) 0.003(2) -0.014(3) -0.008(3) O5W 0.059(4) 0.057(4) 0.075(4) 0.031(3) -0.021(3) -0.043(3) O7W 0.029(3) 0.046(3) 0.085(4) -0.012(3) -0.019(3) -0.005(3) O6W 0.070(5) 0.074(5) 0.049(4) 0.001(3) 0.001(3) -0.022(4) O9W 0.034(4) 0.165(8) 0.077(5) -0.050(5) -0.020(4) -0.004(4) O8W 0.248(14) 0.126(8) 0.081(6) 0.063(6) -0.071(8) -0.101(9) O10W 0.049(4) 0.059(4) 0.038(3) 0.003(3) -0.008(3) -0.018(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 N4 2.106(5) . ? Zn1 O31 2.112(4) . ? Zn1 O29 2.121(4) . ? Zn1 O30 2.122(5) . ? Zn1 N7 2.132(5) . ? Zn1 N1 2.138(5) . ? Zn2 N10 2.150(5) . ? Zn2 N8 2.154(5) . ? Zn2 N13 2.177(5) . ? Zn2 N2 2.181(5) . ? Zn2 N16 2.187(5) . ? Zn2 N5 2.188(5) . ? Zn3 O34 2.101(4) . ? Zn3 N17 2.103(5) . ? Zn3 O32 2.123(5) . ? Zn3 O33 2.131(5) . ? Zn3 N11 2.132(5) . ? Zn3 N14 2.140(5) . ? V6 O20 1.690(4) . ? V6 O11 1.691(4) . ? V6 O13 1.923(4) . ? V6 O15 1.958(4) . ? V6 O19 2.113(4) . ? V6 O10 2.124(4) . ? V6 V3 3.0780(17) . ? V6 V10 3.0946(17) . ? V1 O1 1.615(4) . ? V1 O2 1.812(4) . ? V1 O3 1.816(4) . ? V1 O16 2.000(4) . ? V1 O15 2.014(4) . ? V1 O10 2.257(4) . ? V1 V7 3.0719(17) . ? V1 V3 3.1122(16) . ? V5 O9 1.684(4) . ? V5 O18 1.694(4) . ? V5 O16 1.901(4) . ? V5 O14 2.009(4) . ? V5 O10 2.108(4) . ? V5 O19 2.114(4) . ? V5 V9 3.0821(17) . ? V5 V2 3.0920(17) . ? V4 O12 1.611(4) . ? V4 O8 1.809(4) . ? V4 O7 1.823(4) . ? V4 O13 1.996(4) . ? V4 O14 2.031(4) . ? V4 O10 2.256(4) . ? V4 V8 3.1148(17) . ? V8 O21 1.618(4) . ? V8 O25 1.800(4) . ? V8 O24 1.837(4) . ? V8 O13 1.979(4) . ? V8 O14 2.065(4) . ? V8 O19 2.258(4) . ? V8 V10 3.1111(18) . ? V8 V9 3.1167(16) . ? V3 O6 1.594(4) . ? V3 O5 1.835(4) . ? V3 O3 1.872(4) . ? V3 O8 1.905(4) . ? V3 O11 2.046(4) . ? V3 O10 2.331(4) . ? V3 V2 3.0519(18) . ? V7 O17 1.608(4) . ? V7 O23 1.813(4) . ? V7 O22 1.844(4) . ? V7 O15 1.990(4) . ? V7 O16 2.001(4) . ? V7 O19 2.262(4) . ? V10 O28 1.602(5) . ? V10 O27 1.821(4) . ? V10 O23 1.889(4) . ? V10 O25 1.905(4) . ? V10 O20 2.057(4) . ? V10 O19 2.347(4) . ? V10 V9 3.0539(18) . ? V2 O4 1.604(5) . ? V2 O5 1.814(4) . ? V2 O7 1.874(4) . ? V2 O2 1.902(4) . ? V2 O9 2.079(4) . ? V2 O10 2.310(4) . ? V9 O26 1.604(4) . ? V9 O27 1.830(4) . ? V9 O24 1.869(4) . ? V9 O22 1.895(4) . ? V9 O18 2.056(5) . ? V9 O19 2.306(4) . ? O29 HA29 0.8592 . ? O29 HB29 0.8589 . ? N17 C12 1.313(7) . ? N17 N16 1.387(7) . ? O34 HA34 0.8525 . ? O34 HB34 0.8546 . ? N7 C5 1.309(8) . ? N7 N8 1.380(7) . ? N11 C8 1.308(8) . ? N11 N10 1.373(7) . ? O33 HA33 0.8557 . ? O33 HB33 0.8561 . ? O31 HA31 0.8080 . ? O31 HB31 0.8519 . ? N1 C1 1.307(8) . ? N1 N2 1.368(7) . ? O30 HA30 0.8644 . ? O30 HB30 0.8560 . ? N9 C6 1.327(9) . ? N9 C5 1.348(8) . ? N9 H9N 0.8800 . ? N14 C10 1.310(8) . ? N14 N13 1.375(7) . ? N12N C7 1.327(9) . ? N12N C8 1.336(8) . ? N12N H12N 0.8800 . ? N4 C3 1.321(7) . ? N4 N5 1.379(7) . ? N10 C7 1.310(8) . ? N16 C11 1.316(8) . ? N20 C13 1.319(9) . ? N20 N19 1.373(8) . ? C5 H5 0.9500 . ? N8 C6 1.311(8) . ? O32 HA32 0.8648 . ? O32 HB32 0.8635 . ? N5 C4 1.288(8) . ? N13 C9 1.294(8) . ? N6 C3 1.336(9) . ? N6 C4 1.358(8) . ? N6 H6N 0.8800 . ? N2 C2 1.299(8) . ? N15 C10 1.339(9) . ? N15 C9 1.358(9) . ? N15 H15N 0.8800 . ? C1 N3 1.348(9) . ? C1 H1 0.9500 . ? N19 C14 1.333(9) . ? N19 H19N 0.8800 . ? N3 C2 1.359(9) . ? N3 H3N 0.8800 . ? N18 C12 1.324(9) . ? N18 C11 1.328(8) . ? N18 H18N 0.8800 . ? C12 H12 0.9500 . ? C2 H2 0.9500 . ? C7 H7 0.9500 . ? C3 H3 0.9500 . ? C6 H6 0.9500 . ? C4 H4 0.9500 . ? C11 H11 0.9500 . ? C14 N21 1.337(9) . ? C14 H14 0.9500 . ? C8 H8 0.9500 . ? C10 H10 0.9500 . ? C9 H9 0.9500 . ? N21 C13 1.360(9) . ? C13 H13 0.9500 . ? O2W O3W 2.789(9) . ? O3W O9W 2.661(9) . ? O4W O10W 2.777(8) . ? O7W O8W 2.733(11) . ? 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 N4 Zn1 O31 87.4(2) . . ? N4 Zn1 O29 92.29(19) . . ? O31 Zn1 O29 93.01(17) . . ? N4 Zn1 O30 170.7(2) . . ? O31 Zn1 O30 85.3(2) . . ? O29 Zn1 O30 82.20(19) . . ? N4 Zn1 N7 94.6(2) . . ? O31 Zn1 N7 174.70(19) . . ? O29 Zn1 N7 91.79(18) . . ? O30 Zn1 N7 93.09(19) . . ? N4 Zn1 N1 94.2(2) . . ? O31 Zn1 N1 87.25(19) . . ? O29 Zn1 N1 173.49(19) . . ? O30 Zn1 N1 91.3(2) . . ? N7 Zn1 N1 87.73(19) . . ? N10 Zn2 N8 178.35(19) . . ? N10 Zn2 N13 87.4(2) . . ? N8 Zn2 N13 91.4(2) . . ? N10 Zn2 N2 91.9(2) . . ? N8 Zn2 N2 89.2(2) . . ? N13 Zn2 N2 179.3(2) . . ? N10 Zn2 N16 91.71(19) . . ? N8 Zn2 N16 87.1(2) . . ? N13 Zn2 N16 91.8(2) . . ? N2 Zn2 N16 88.27(19) . . ? N10 Zn2 N5 91.08(19) . . ? N8 Zn2 N5 90.1(2) . . ? N13 Zn2 N5 89.3(2) . . ? N2 Zn2 N5 90.7(2) . . ? N16 Zn2 N5 177.1(2) . . ? O34 Zn3 N17 90.65(19) . . ? O34 Zn3 O32 91.01(19) . . ? N17 Zn3 O32 86.9(2) . . ? O34 Zn3 O33 85.00(19) . . ? N17 Zn3 O33 171.09(19) . . ? O32 Zn3 O33 85.4(2) . . ? O34 Zn3 N11 93.65(18) . . ? N17 Zn3 N11 95.92(19) . . ? O32 Zn3 N11 174.5(2) . . ? O33 Zn3 N11 92.13(19) . . ? O34 Zn3 N14 176.39(19) . . ? N17 Zn3 N14 92.6(2) . . ? O32 Zn3 N14 87.7(2) . . ? O33 Zn3 N14 91.5(2) . . ? N11 Zn3 N14 87.5(2) . . ? O20 V6 O11 106.8(2) . . ? O20 V6 O13 98.81(19) . . ? O11 V6 O13 97.50(19) . . ? O20 V6 O15 95.55(19) . . ? O11 V6 O15 96.98(18) . . ? O13 V6 O15 155.71(17) . . ? O20 V6 O19 87.62(18) . . ? O11 V6 O19 165.58(19) . . ? O13 V6 O19 80.89(16) . . ? O15 V6 O19 80.23(16) . . ? O20 V6 O10 165.45(18) . . ? O11 V6 O10 87.63(18) . . ? O13 V6 O10 80.99(16) . . ? O15 V6 O10 80.23(16) . . ? O19 V6 O10 77.96(15) . . ? O20 V6 V3 145.18(15) . . ? O11 V6 V3 38.49(14) . . ? O13 V6 V3 90.43(13) . . ? O15 V6 V3 88.85(13) . . ? O19 V6 V3 127.09(12) . . ? O10 V6 V3 49.14(10) . . ? O20 V6 V10 38.36(14) . . ? O11 V6 V10 145.13(15) . . ? O13 V6 V10 90.51(12) . . ? O15 V6 V10 88.68(12) . . ? O19 V6 V10 49.26(11) . . ? O10 V6 V10 127.21(11) . . ? V3 V6 V10 175.97(4) . . ? O1 V1 O2 103.6(2) . . ? O1 V1 O3 102.5(2) . . ? O2 V1 O3 94.53(19) . . ? O1 V1 O16 99.8(2) . . ? O2 V1 O16 90.72(18) . . ? O3 V1 O16 155.20(17) . . ? O1 V1 O15 99.2(2) . . ? O2 V1 O15 155.28(18) . . ? O3 V1 O15 89.72(18) . . ? O16 V1 O15 75.98(16) . . ? O1 V1 O10 174.2(2) . . ? O2 V1 O10 80.77(17) . . ? O3 V1 O10 80.78(16) . . ? O16 V1 O10 76.16(15) . . ? O15 V1 O10 75.89(15) . . ? O1 V1 V7 89.42(17) . . ? O2 V1 V7 130.57(13) . . ? O3 V1 V7 129.33(14) . . ? O16 V1 V7 39.85(12) . . ? O15 V1 V7 39.61(11) . . ? O10 V1 V7 84.80(11) . . ? O1 V1 V3 135.39(16) . . ? O2 V1 V3 83.59(13) . . ? O3 V1 V3 33.00(13) . . ? O16 V1 V3 124.40(12) . . ? O15 V1 V3 86.91(12) . . ? O10 V1 V3 48.29(10) . . ? V7 V1 V3 119.38(4) . . ? O9 V5 O18 106.9(2) . . ? O9 V5 O16 99.02(19) . . ? O18 V5 O16 98.65(19) . . ? O9 V5 O14 95.54(19) . . ? O18 V5 O14 94.98(19) . . ? O16 V5 O14 156.19(17) . . ? O9 V5 O10 87.48(18) . . ? O18 V5 O10 165.24(19) . . ? O16 V5 O10 81.95(16) . . ? O14 V5 O10 79.98(16) . . ? O9 V5 O19 165.49(18) . . ? O18 V5 O19 87.18(19) . . ? O16 V5 O19 81.92(16) . . ? O14 V5 O19 79.35(16) . . ? O10 V5 O19 78.29(15) . . ? O9 V5 V9 145.61(14) . . ? O18 V5 V9 38.78(15) . . ? O16 V5 V9 90.80(13) . . ? O14 V5 V9 87.69(12) . . ? O10 V5 V9 126.66(12) . . ? O19 V5 V9 48.40(10) . . ? O9 V5 V2 39.17(14) . . ? O18 V5 V2 146.03(16) . . ? O16 V5 V2 90.64(12) . . ? O14 V5 V2 88.83(12) . . ? O10 V5 V2 48.33(11) . . ? O19 V5 V2 126.60(11) . . ? V9 V5 V2 174.46(4) . . ? O12 V4 O8 101.9(2) . . ? O12 V4 O7 102.8(2) . . ? O8 V4 O7 94.16(19) . . ? O12 V4 O13 100.7(2) . . ? O8 V4 O13 91.61(18) . . ? O7 V4 O13 154.10(17) . . ? O12 V4 O14 100.6(2) . . ? O8 V4 O14 155.87(18) . . ? O7 V4 O14 89.19(18) . . ? O13 V4 O14 75.77(17) . . ? O12 V4 O10 175.8(2) . . ? O8 V4 O10 81.04(16) . . ? O7 V4 O10 79.79(17) . . ? O13 V4 O10 76.21(15) . . ? O14 V4 O10 76.05(15) . . ? O12 V4 V8 91.18(17) . . ? O8 V4 V8 129.82(15) . . ? O7 V4 V8 130.06(13) . . ? O13 V4 V8 38.21(12) . . ? O14 V4 V8 40.91(12) . . ? O10 V4 V8 84.67(11) . . ? O21 V8 O25 104.4(2) . . ? O21 V8 O24 102.2(2) . . ? O25 V8 O24 96.0(2) . . ? O21 V8 O13 100.3(2) . . ? O25 V8 O13 91.53(18) . . ? O24 V8 O13 153.68(17) . . ? O21 V8 O14 98.2(2) . . ? O25 V8 O14 155.56(18) . . ? O24 V8 O14 87.92(18) . . ? O13 V8 O14 75.38(16) . . ? O21 V8 O19 172.8(2) . . ? O25 V8 O19 81.99(17) . . ? O24 V8 O19 79.97(16) . . ? O13 V8 O19 76.15(15) . . ? O14 V8 O19 74.93(16) . . ? O21 V8 V10 138.05(18) . . ? O25 V8 V10 33.95(13) . . ? O24 V8 V10 83.44(14) . . ? O13 V8 V10 89.00(13) . . ? O14 V8 V10 123.64(12) . . ? O19 V8 V10 48.71(11) . . ? O21 V8 V4 89.47(17) . . ? O25 V8 V4 130.14(14) . . ? O24 V8 V4 128.00(15) . . ? O13 V8 V4 38.62(12) . . ? O14 V8 V4 40.09(11) . . ? O19 V8 V4 83.89(11) . . ? V10 V8 V4 119.90(5) . . ? O21 V8 V9 135.21(16) . . ? O25 V8 V9 84.51(14) . . ? O24 V8 V9 33.09(13) . . ? O13 V8 V9 123.63(12) . . ? O14 V8 V9 85.81(12) . . ? O19 V8 V9 47.57(10) . . ? V10 V8 V9 58.73(4) . . ? V4 V8 V9 118.31(5) . . ? O6 V3 O5 104.4(2) . . ? O6 V3 O3 103.8(2) . . ? O5 V3 O3 91.88(19) . . ? O6 V3 O8 100.7(2) . . ? O5 V3 O8 89.40(19) . . ? O3 V3 O8 154.35(18) . . ? O6 V3 O11 99.4(2) . . ? O5 V3 O11 156.07(17) . . ? O3 V3 O11 84.89(18) . . ? O8 V3 O11 83.64(18) . . ? O6 V3 O10 173.7(2) . . ? O5 V3 O10 81.61(16) . . ? O3 V3 O10 77.69(16) . . ? O8 V3 O10 77.17(15) . . ? O11 V3 O10 74.53(15) . . ? O6 V3 V2 137.38(19) . . ? O5 V3 V2 33.02(13) . . ? O3 V3 V2 84.26(14) . . ? O8 V3 V2 82.95(13) . . ? O11 V3 V2 123.11(12) . . ? O10 V3 V2 48.59(10) . . ? O6 V3 V6 130.37(18) . . ? O5 V3 V6 125.17(13) . . ? O3 V3 V6 79.49(13) . . ? O8 V3 V6 78.88(13) . . ? O11 V3 V6 30.96(11) . . ? O10 V3 V6 43.57(10) . . ? V2 V3 V6 92.16(4) . . ? O6 V3 V1 135.63(18) . . ? O5 V3 V1 82.32(14) . . ? O3 V3 V1 31.89(12) . . ? O8 V3 V1 123.44(12) . . ? O11 V3 V1 82.53(12) . . ? O10 V3 V1 46.28(10) . . ? V2 V3 V1 60.82(4) . . ? V6 V3 V1 62.26(4) . . ? O17 V7 O23 102.4(2) . . ? O17 V7 O22 102.4(2) . . ? O23 V7 O22 94.75(19) . . ? O17 V7 O15 101.1(2) . . ? O23 V7 O15 90.17(18) . . ? O22 V7 O15 154.31(18) . . ? O17 V7 O16 99.8(2) . . ? O23 V7 O16 155.94(18) . . ? O22 V7 O16 89.42(18) . . ? O15 V7 O16 76.49(17) . . ? O17 V7 O19 175.4(2) . . ? O23 V7 O19 81.29(17) . . ? O22 V7 O19 79.89(16) . . ? O15 V7 O19 75.96(15) . . ? O16 V7 O19 76.13(15) . . ? O17 V7 V1 90.60(17) . . ? O23 V7 V1 130.36(14) . . ? O22 V7 V1 129.22(14) . . ? O15 V7 V1 40.19(12) . . ? O16 V7 V1 39.82(11) . . ? O19 V7 V1 84.87(11) . . ? O28 V10 O27 105.3(2) . . ? O28 V10 O23 102.3(2) . . ? O27 V10 O23 92.08(19) . . ? O28 V10 O25 101.5(2) . . ? O27 V10 O25 92.08(19) . . ? O23 V10 O25 153.85(19) . . ? O28 V10 O20 99.3(2) . . ? O27 V10 O20 155.39(19) . . ? O23 V10 O20 83.28(18) . . ? O25 V10 O20 82.26(18) . . ? O28 V10 O19 172.9(2) . . ? O27 V10 O19 81.72(17) . . ? O23 V10 O19 77.56(16) . . ? O25 V10 O19 77.53(16) . . ? O20 V10 O19 73.68(15) . . ? O28 V10 V9 138.65(18) . . ? O27 V10 V9 33.32(14) . . ? O23 V10 V9 84.71(13) . . ? O25 V10 V9 84.69(13) . . ? O20 V10 V9 122.08(13) . . ? O19 V10 V9 48.40(10) . . ? O28 V10 V6 129.93(18) . . ? O27 V10 V6 124.72(14) . . ? O23 V10 V6 78.99(13) . . ? O25 V10 V6 77.45(13) . . ? O20 V10 V6 30.67(12) . . ? O19 V10 V6 43.01(9) . . ? V9 V10 V6 91.41(4) . . ? O28 V10 V8 133.27(18) . . ? O27 V10 V8 81.98(14) . . ? O23 V10 V8 123.85(14) . . ? O25 V10 V8 31.84(12) . . ? O20 V10 V8 80.69(13) . . ? O19 V10 V8 46.30(10) . . ? V9 V10 V8 60.73(3) . . ? V6 V10 V8 60.84(4) . . ? O4 V2 O5 104.6(2) . . ? O4 V2 O7 101.8(2) . . ? O5 V2 O7 92.18(18) . . ? O4 V2 O2 102.2(2) . . ? O5 V2 O2 91.65(18) . . ? O7 V2 O2 153.92(19) . . ? O4 V2 O9 99.0(2) . . ? O5 V2 O9 156.33(18) . . ? O7 V2 O9 83.13(17) . . ? O2 V2 O9 83.07(17) . . ? O4 V2 O10 172.74(19) . . ? O5 V2 O10 82.61(17) . . ? O7 V2 O10 77.37(17) . . ? O2 V2 O10 77.57(16) . . ? O9 V2 O10 73.72(15) . . ? O4 V2 V3 138.08(17) . . ? O5 V2 V3 33.45(13) . . ? O7 V2 V3 85.13(14) . . ? O2 V2 V3 83.95(13) . . ? O9 V2 V3 122.89(12) . . ? O10 V2 V3 49.17(10) . . ? O4 V2 V5 129.80(17) . . ? O5 V2 V5 125.56(14) . . ? O7 V2 V5 79.16(13) . . ? O2 V2 V5 77.66(13) . . ? O9 V2 V5 30.78(12) . . ? O10 V2 V5 42.96(10) . . ? V3 V2 V5 92.11(4) . . ? O26 V9 O27 103.9(2) . . ? O26 V9 O24 103.0(2) . . ? O27 V9 O24 91.51(19) . . ? O26 V9 O22 100.3(2) . . ? O27 V9 O22 91.29(19) . . ? O24 V9 O22 155.09(18) . . ? O26 V9 O18 99.0(2) . . ? O27 V9 O18 156.98(17) . . ? O24 V9 O18 85.51(19) . . ? O22 V9 O18 82.32(18) . . ? O26 V9 O19 173.2(2) . . ? O27 V9 O19 82.69(16) . . ? O24 V9 O19 78.07(16) . . ? O22 V9 O19 77.75(15) . . ? O18 V9 O19 74.35(15) . . ? O26 V9 V10 137.0(2) . . ? O27 V9 V10 33.14(13) . . ? O24 V9 V10 84.61(14) . . ? O22 V9 V10 84.28(13) . . ? O18 V9 V10 123.88(12) . . ? O19 V9 V10 49.55(10) . . ? O26 V9 V5 130.0(2) . . ? O27 V9 V5 125.93(13) . . ? O24 V9 V5 80.89(14) . . ? O22 V9 V5 77.46(13) . . ? O18 V9 V5 31.07(11) . . ? O19 V9 V5 43.29(10) . . ? V10 V9 V5 92.81(4) . . ? O26 V9 V8 135.43(18) . . ? O27 V9 V8 81.70(13) . . ? O24 V9 V8 32.46(12) . . ? O22 V9 V8 124.02(12) . . ? O18 V9 V8 83.65(12) . . ? O19 V9 V8 46.28(10) . . ? V10 V9 V8 60.54(4) . . ? V5 V9 V8 63.70(4) . . ? V6 O15 V7 107.64(18) . . ? V6 O15 V1 107.3(2) . . ? V7 O15 V1 100.20(18) . . ? V6 O13 V8 107.29(18) . . ? V6 O13 V4 107.44(18) . . ? V8 O13 V4 103.17(19) . . ? V6 O11 V3 110.5(2) . . ? V5 O16 V1 107.15(18) . . ? V5 O16 V7 107.46(18) . . ? V1 O16 V7 100.33(18) . . ? V7 O22 V9 114.2(2) . . ? V4 O8 V3 115.0(2) . . ? V10 O27 V9 113.5(2) . . ? V8 O24 V9 114.4(2) . . ? V2 O5 V3 113.5(2) . . ? V1 O2 V2 114.3(2) . . ? V1 O3 V3 115.1(2) . . ? V8 O25 V10 114.2(2) . . ? V5 O10 V6 101.79(17) . . ? V5 O10 V4 95.38(15) . . ? V6 O10 V4 92.28(15) . . ? V5 O10 V1 91.92(15) . . ? V6 O10 V1 93.82(16) . . ? V4 O10 V1 169.3(2) . . ? V5 O10 V2 88.71(15) . . ? V6 O10 V2 169.49(19) . . ? V4 O10 V2 86.22(14) . . ? V1 O10 V2 86.20(13) . . ? V5 O10 V3 170.7(2) . . ? V6 O10 V3 87.29(14) . . ? V4 O10 V3 86.14(13) . . ? V1 O10 V3 85.43(13) . . ? V2 O10 V3 82.23(13) . . ? V5 O14 V4 106.08(18) . . ? V5 O14 V8 106.80(19) . . ? V4 O14 V8 99.00(18) . . ? V5 O18 V9 110.1(2) . . ? V6 O20 V10 111.0(2) . . ? V6 O19 V5 101.95(17) . . ? V6 O19 V8 91.87(14) . . ? V5 O19 V8 96.82(16) . . ? V6 O19 V7 93.44(15) . . ? V5 O19 V7 91.86(14) . . ? V8 O19 V7 168.7(2) . . ? V6 O19 V9 169.7(2) . . ? V5 O19 V9 88.31(15) . . ? V8 O19 V9 86.14(14) . . ? V7 O19 V9 86.85(13) . . ? V6 O19 V10 87.73(15) . . ? V5 O19 V10 170.06(19) . . ? V8 O19 V10 84.99(13) . . ? V7 O19 V10 85.23(14) . . ? V9 O19 V10 82.05(13) . . ? V7 O23 V10 114.9(2) . . ? Zn1 O29 HA29 130.2 . . ? Zn1 O29 HB29 103.9 . . ? HA29 O29 HB29 106.1 . . ? C12 N17 N16 106.5(5) . . ? C12 N17 Zn3 129.2(4) . . ? N16 N17 Zn3 124.1(4) . . ? V4 O7 V2 115.1(2) . . ? Zn3 O34 HA34 134.8 . . ? Zn3 O34 HB34 111.5 . . ? HA34 O34 HB34 107.1 . . ? V5 O9 V2 110.1(2) . . ? C5 N7 N8 106.8(5) . . ? C5 N7 Zn1 130.7(4) . . ? N8 N7 Zn1 122.5(4) . . ? C8 N11 N10 107.2(5) . . ? C8 N11 Zn3 128.6(4) . . ? N10 N11 Zn3 123.9(4) . . ? Zn3 O33 HA33 131.0 . . ? Zn3 O33 HB33 121.3 . . ? HA33 O33 HB33 106.7 . . ? Zn1 O31 HA31 119.3 . . ? Zn1 O31 HB31 117.2 . . ? HA31 O31 HB31 106.8 . . ? C1 N1 N2 107.2(5) . . ? C1 N1 Zn1 128.2(5) . . ? N2 N1 Zn1 124.3(4) . . ? Zn1 O30 HA30 119.3 . . ? Zn1 O30 HB30 115.0 . . ? HA30 O30 HB30 105.8 . . ? C6 N9 C5 105.9(5) . . ? C6 N9 H9N 127.0 . . ? C5 N9 H9N 127.0 . . ? C10 N14 N13 106.3(5) . . ? C10 N14 Zn3 128.9(5) . . ? N13 N14 Zn3 124.7(4) . . ? C7 N12N C8 105.7(6) . . ? C7 N12N H12N 127.1 . . ? C8 N12N H12N 127.1 . . ? C3 N4 N5 106.3(5) . . ? C3 N4 Zn1 129.1(5) . . ? N5 N4 Zn1 124.6(4) . . ? C7 N10 N11 106.1(5) . . ? C7 N10 Zn2 128.1(5) . . ? N11 N10 Zn2 125.2(4) . . ? C11 N16 N17 106.3(5) . . ? C11 N16 Zn2 128.2(5) . . ? N17 N16 Zn2 124.4(4) . . ? C13 N20 N19 102.3(6) . . ? N7 C5 N9 109.9(6) . . ? N7 C5 H5 125.0 . . ? N9 C5 H5 125.0 . . ? C6 N8 N7 106.7(5) . . ? C6 N8 Zn2 126.8(5) . . ? N7 N8 Zn2 126.3(4) . . ? Zn3 O32 HA32 124.0 . . ? Zn3 O32 HB32 108.5 . . ? HA32 O32 HB32 119.5 . . ? C4 N5 N4 107.5(5) . . ? C4 N5 Zn2 128.1(5) . . ? N4 N5 Zn2 124.2(4) . . ? C9 N13 N14 108.5(5) . . ? C9 N13 Zn2 127.5(5) . . ? N14 N13 Zn2 123.8(4) . . ? C3 N6 C4 105.0(5) . . ? C3 N6 H6N 127.5 . . ? C4 N6 H6N 127.5 . . ? C2 N2 N1 108.1(6) . . ? C2 N2 Zn2 126.0(5) . . ? N1 N2 Zn2 124.1(4) . . ? C10 N15 C9 106.0(6) . . ? C10 N15 H15N 127.0 . . ? C9 N15 H15N 127.0 . . ? N1 C1 N3 109.7(6) . . ? N1 C1 H1 125.2 . . ? N3 C1 H1 125.2 . . ? C14 N19 N20 109.9(6) . . ? C14 N19 H19N 125.0 . . ? N20 N19 H19N 125.0 . . ? C1 N3 C2 105.8(6) . . ? C1 N3 H3N 127.1 . . ? C2 N3 H3N 127.1 . . ? C12 N18 C11 106.8(5) . . ? C12 N18 H18N 126.6 . . ? C11 N18 H18N 126.6 . . ? N17 C12 N18 110.2(6) . . ? N17 C12 H12 124.9 . . ? N18 C12 H12 124.9 . . ? N2 C2 N3 109.2(6) . . ? N2 C2 H2 125.4 . . ? N3 C2 H2 125.4 . . ? N10 C7 N12N 110.9(6) . . ? N10 C7 H7 124.5 . . ? N12N C7 H7 124.5 . . ? N4 C3 N6 110.5(6) . . ? N4 C3 H3 124.8 . . ? N6 C3 H3 124.8 . . ? N8 C6 N9 110.6(6) . . ? N8 C6 H6 124.7 . . ? N9 C6 H6 124.7 . . ? N5 C4 N6 110.7(6) . . ? N5 C4 H4 124.7 . . ? N6 C4 H4 124.7 . . ? N16 C11 N18 110.1(6) . . ? N16 C11 H11 125.0 . . ? N18 C11 H11 125.0 . . ? N19 C14 N21 109.9(6) . . ? N19 C14 H14 125.0 . . ? N21 C14 H14 125.0 . . ? N11 C8 N12N 110.0(6) . . ? N11 C8 H8 125.0 . . ? N12N C8 H8 125.0 . . ? N14 C10 N15 110.1(6) . . ? N14 C10 H10 124.9 . . ? N15 C10 H10 124.9 . . ? N13 C9 N15 109.0(6) . . ? N13 C9 H9 125.5 . . ? N15 C9 H9 125.5 . . ? C14 N21 C13 102.9(6) . . ? N20 C13 N21 114.8(6) . . ? N20 C13 H13 122.6 . . ? N21 C13 H13 122.6 . . ? O9W O3W O2W 135.0(3) . . ? 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 O34 HA34 O3 0.85 1.83 2.633(6) 156.8 . N9 H9N O22 0.88 1.86 2.727(6) 169.1 2_756 N18 H18N O2 0.88 1.93 2.741(7) 153.3 2_756 N12N H12N O8 0.88 1.80 2.605(7) 151.9 2_755 N6 H6N O25 0.88 2.01 2.846(7) 157.6 2_755 O29 HA29 O24 0.86 1.85 2.634(6) 151.3 1_465 O33 HA33 O21 0.86 2.21 2.945(6) 144.5 1_565 O30 HB30 O1 0.86 2.01 2.809(6) 155.7 1_455 O32 HA32 O29 0.86 2.26 2.732(7) 114.3 1_655 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.783 _refine_diff_density_min -0.937 _refine_diff_density_rms 0.162 data_3 _database_code_depnum_ccdc_archive 'CCDC 825613' #TrackingRef '- crystal data.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C9 H13 N10 O21 V5 Zn3' _chemical_formula_sum 'C9 H13 N10 O21 V5 Zn3' _chemical_formula_weight 1048.10 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 24.677(3) _cell_length_b 18.0396(19) _cell_length_c 17.2999(18) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7701.3(14) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 17048 _cell_measurement_theta_min 3.0895 _cell_measurement_theta_max 27.4835 _exptl_crystal_description Prism _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.3000 _exptl_crystal_size_mid 0.2000 _exptl_crystal_size_min 0.1500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.808 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4080 _exptl_absorpt_coefficient_mu 3.072 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5833 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_process_details '(CrystalClear; Rigaku, 2000)' _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 \w _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 56853 _diffrn_reflns_av_R_equivalents 0.0318 _diffrn_reflns_av_sigmaI/netI 0.0183 _diffrn_reflns_limit_h_min -32 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.72 _diffrn_reflns_theta_max 27.48 _reflns_number_total 8708 _reflns_number_gt 7674 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku, 2000)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _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^)+(0.1002P)^2^+9.6801P] 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 8708 _refine_ls_number_parameters 437 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0580 _refine_ls_R_factor_gt 0.0527 _refine_ls_wR_factor_ref 0.1578 _refine_ls_wR_factor_gt 0.1501 _refine_ls_goodness_of_fit_ref 1.086 _refine_ls_restrained_S_all 1.086 _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 Zn3 Zn 0.167286(19) 0.15078(2) 0.30139(3) 0.03976(14) Uani 1 1 d . . . Zn1 Zn 0.167750(17) -0.15052(2) 0.14919(2) 0.03567(13) Uani 1 1 d . . . Zn2 Zn 0.296286(18) -0.07078(2) 0.09564(2) 0.03739(13) Uani 1 1 d . . . V3 V 0.09232(2) -0.30552(3) 0.16317(3) 0.02875(14) Uani 1 1 d . . . V5 V 0.02313(2) -0.30175(4) 0.40420(3) 0.03309(15) Uani 1 1 d . . . V6 V 0.0000 -0.39299(4) 0.2500 0.02728(17) Uani 1 2 d S . . V4 V 0.11506(2) -0.38637(3) 0.31821(4) 0.03387(15) Uani 1 1 d . . . V2 V 0.0000 -0.21193(4) 0.2500 0.02863(17) Uani 1 2 d S . . V1 V 0.11444(2) -0.21670(4) 0.31794(3) 0.03432(15) Uani 1 1 d . . . O2 O 0.05039(11) -0.15513(14) 0.27948(15) 0.0366(5) Uani 1 1 d . . . O7 O 0.02880(9) -0.23420(13) 0.14883(13) 0.0305(5) Uani 1 1 d . . . O14 O 0.05087(10) -0.44884(14) 0.27966(15) 0.0342(5) Uani 1 1 d . . . O4 O 0.15240(10) -0.30154(15) 0.33874(15) 0.0374(6) Uani 1 1 d . . . O13 O 0.02876(9) -0.37103(13) 0.14835(13) 0.0304(5) Uani 1 1 d . . . O11 O 0.07348(10) -0.37597(15) 0.40779(14) 0.0377(5) Uani 1 1 d . . . O6 O 0.05043(9) -0.30227(12) 0.27869(13) 0.0284(5) Uani 1 1 d . . . O5 O 0.07320(11) -0.22719(16) 0.40751(14) 0.0385(6) Uani 1 1 d . . . O9 O 0.13006(9) -0.37736(14) 0.21017(15) 0.0342(5) Uani 1 1 d . . . O8 O 0.11641(11) -0.30260(16) 0.07687(16) 0.0418(6) Uani 1 1 d . . . O3 O 0.12860(9) -0.22664(14) 0.20939(14) 0.0330(5) Uani 1 1 d . . . N3 N 0.30449(13) -0.26265(18) 0.24380(19) 0.0396(7) Uani 1 1 d . . . N9 N 0.19228(15) 0.06100(19) 0.2443(2) 0.0434(7) Uani 1 1 d . . . N8 N 0.18762(15) -0.04732(18) 0.1860(2) 0.0432(7) Uani 1 1 d . . . O10 O 0.15697(12) -0.45030(17) 0.34097(19) 0.0479(7) Uani 1 1 d . . . O16 O 0.36155(15) -0.1284(2) 0.0371(2) 0.0617(9) Uani 1 1 d . . . N4 N 0.19096(15) -0.1490(2) 0.03709(19) 0.0455(8) Uani 1 1 d . . . O12 O -0.00108(13) -0.30125(18) 0.49066(16) 0.0478(7) Uani 1 1 d . . . N7 N 0.23664(14) -0.01520(18) 0.1665(2) 0.0414(7) Uani 1 1 d . . . C5 C 0.16314(18) -0.0005(2) 0.2311(3) 0.0463(9) Uani 1 1 d . . . H5 H 0.1282 -0.0089 0.2525 0.056 Uiso 1 1 calc R . . N2 N 0.29203(13) -0.16556(18) 0.16775(19) 0.0380(7) Uani 1 1 d . . . N1 N 0.24209(13) -0.19480(17) 0.1869(2) 0.0401(7) Uani 1 1 d . . . C1 C 0.25166(16) -0.2519(2) 0.2313(2) 0.0417(8) Uani 1 1 d . . . H1 H 0.2240 -0.2825 0.2525 0.050 Uiso 1 1 calc R . . O19 O 0.29987(17) 0.0211(2) 0.0189(2) 0.0652(9) Uani 1 1 d . . . N5 N 0.23863(14) -0.11584(19) 0.01585(18) 0.0415(7) Uani 1 1 d . . . N6 N 0.19347(16) -0.1465(2) -0.0901(2) 0.0464(8) Uani 1 1 d . . . O17 O 0.35999(15) -0.0243(2) 0.1618(2) 0.0634(9) Uani 1 1 d . . . C6 C 0.23761(18) 0.0483(2) 0.2027(3) 0.0454(9) Uani 1 1 d . . . H6 H 0.2671 0.0820 0.2001 0.055 Uiso 1 1 calc R . . C4 C 0.23871(17) -0.1153(2) -0.0601(2) 0.0442(9) Uani 1 1 d . . . H4 H 0.2673 -0.0954 -0.0905 0.053 Uiso 1 1 calc R . . O15 O 0.08647(14) -0.1126(2) 0.1105(2) 0.0660(9) Uani 1 1 d . . . O1 O 0.15553(13) -0.15108(17) 0.33963(19) 0.0496(7) Uani 1 1 d . . . C2 C 0.32800(16) -0.2077(2) 0.2029(2) 0.0404(8) Uani 1 1 d . . . H2 H 0.3661 -0.2003 0.1998 0.048 Uiso 1 1 calc R . . C3 C 0.16555(19) -0.1661(3) -0.0269(2) 0.0517(11) Uani 1 1 d . . . H3 H 0.1312 -0.1898 -0.0284 0.062 Uiso 1 1 calc R . . N10 N 0.3390(3) 0.0939(3) -0.0719(3) 0.0805(15) Uani 1 1 d . . . O18 O 0.0866(2) 0.1533(4) 0.3057(4) 0.116(2) Uani 1 1 d . . . C7 C 0.3396(3) 0.0499(4) -0.0112(4) 0.0723(15) Uani 1 1 d . . . H7 H 0.3739 0.0395 0.0114 0.087 Uiso 1 1 calc R . . C8 C 0.2875(4) 0.1062(5) -0.1185(6) 0.122(3) Uani 1 1 d . . . H8A H 0.2571 0.0812 -0.0930 0.183 Uiso 1 1 calc R . . H8B H 0.2922 0.0860 -0.1706 0.183 Uiso 1 1 calc R . . H8C H 0.2800 0.1595 -0.1218 0.183 Uiso 1 1 calc R . . C9 C 0.3872(5) 0.1237(6) -0.1036(6) 0.134(4) Uani 1 1 d . . . H9A H 0.4186 0.1040 -0.0755 0.200 Uiso 1 1 calc R . . H9B H 0.3866 0.1778 -0.0991 0.200 Uiso 1 1 calc R . . H9C H 0.3899 0.1097 -0.1583 0.200 Uiso 1 1 calc R . . O1W O -0.0325(4) -0.5072(5) 0.4288(6) 0.167(4) Uani 1 1 d . . . O2W O 0.1370(10) -0.2188(8) 0.5389(8) 0.233(12) 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 Zn3 0.0470(3) 0.0388(3) 0.0335(2) -0.00171(16) 0.00208(17) 0.00365(17) Zn1 0.0404(2) 0.0344(2) 0.0323(2) 0.00075(15) 0.00825(16) -0.00975(15) Zn2 0.0405(2) 0.0370(2) 0.0347(2) -0.00059(16) 0.00746(16) -0.01017(16) V3 0.0258(3) 0.0342(3) 0.0263(3) -0.0014(2) 0.0038(2) -0.00129(19) V5 0.0310(3) 0.0458(3) 0.0225(3) 0.0014(2) 0.0001(2) -0.0015(2) V6 0.0247(3) 0.0284(4) 0.0287(4) 0.000 -0.0017(3) 0.000 V4 0.0276(3) 0.0390(3) 0.0350(3) 0.0026(2) -0.0046(2) 0.0018(2) V2 0.0298(4) 0.0291(4) 0.0270(4) 0.000 0.0034(3) 0.000 V1 0.0327(3) 0.0399(3) 0.0303(3) -0.0028(2) -0.0001(2) -0.0086(2) O2 0.0391(13) 0.0334(12) 0.0371(13) -0.0032(10) 0.0027(10) -0.0043(9) O7 0.0312(11) 0.0355(12) 0.0248(11) 0.0032(9) 0.0042(8) -0.0010(9) O14 0.0292(11) 0.0339(12) 0.0394(13) 0.0022(10) -0.0032(10) 0.0031(9) O4 0.0268(11) 0.0498(15) 0.0357(13) 0.0015(10) -0.0040(10) -0.0030(10) O13 0.0279(11) 0.0353(12) 0.0280(11) -0.0046(9) 0.0016(8) 0.0007(9) O11 0.0319(12) 0.0490(14) 0.0321(12) 0.0074(10) -0.0046(9) 0.0001(11) O6 0.0267(10) 0.0330(11) 0.0255(11) 0.0013(8) 0.0010(8) -0.0011(8) O5 0.0359(13) 0.0516(15) 0.0279(12) -0.0071(10) -0.0029(9) -0.0040(11) O9 0.0270(11) 0.0383(12) 0.0373(13) -0.0029(10) 0.0027(9) 0.0019(9) O8 0.0390(14) 0.0540(16) 0.0325(13) -0.0005(11) 0.0114(11) -0.0007(11) O3 0.0288(11) 0.0377(12) 0.0327(12) 0.0017(10) 0.0037(9) -0.0068(9) N3 0.0415(16) 0.0381(15) 0.0393(16) 0.0026(13) 0.0068(13) -0.0029(13) N9 0.0519(19) 0.0372(16) 0.0412(17) -0.0065(13) 0.0070(14) -0.0012(14) N8 0.0453(17) 0.0365(16) 0.0477(18) -0.0019(14) 0.0093(15) -0.0072(13) O10 0.0355(13) 0.0503(16) 0.0579(18) 0.0065(13) -0.0112(12) 0.0049(12) O16 0.062(2) 0.070(2) 0.0532(19) -0.0029(16) 0.0252(16) 0.0030(17) N4 0.0470(19) 0.059(2) 0.0304(15) -0.0014(14) 0.0078(14) -0.0196(15) O12 0.0498(16) 0.0672(19) 0.0263(13) 0.0015(12) 0.0028(11) -0.0020(13) N7 0.0450(17) 0.0361(16) 0.0430(17) -0.0064(13) 0.0082(14) -0.0075(13) C5 0.048(2) 0.0374(19) 0.054(2) -0.0036(17) 0.0123(18) -0.0018(15) N2 0.0386(16) 0.0380(15) 0.0374(15) 0.0017(13) 0.0113(12) -0.0072(12) N1 0.0351(16) 0.0377(16) 0.0474(18) 0.0036(13) 0.0116(13) -0.0077(12) C1 0.0385(18) 0.0373(18) 0.049(2) 0.0075(16) 0.0124(16) -0.0048(14) O19 0.075(2) 0.056(2) 0.064(2) 0.0158(16) 0.0069(17) -0.0169(17) N5 0.0429(17) 0.0468(17) 0.0348(16) 0.0004(13) 0.0069(13) -0.0107(14) N6 0.053(2) 0.053(2) 0.0333(16) -0.0022(14) 0.0060(14) -0.0122(16) O17 0.0556(19) 0.0577(19) 0.077(2) -0.0173(17) -0.0061(17) -0.0155(15) C6 0.052(2) 0.0357(18) 0.049(2) -0.0035(16) 0.0080(18) -0.0069(16) C4 0.049(2) 0.051(2) 0.0332(18) -0.0008(16) 0.0086(15) -0.0104(17) O15 0.0522(19) 0.063(2) 0.083(3) 0.0232(18) 0.0065(17) -0.0072(15) O1 0.0464(16) 0.0507(17) 0.0516(17) -0.0066(13) -0.0035(13) -0.0164(13) C2 0.0401(19) 0.0417(19) 0.0395(19) 0.0019(15) 0.0060(15) -0.0052(15) C3 0.056(3) 0.066(3) 0.033(2) -0.0035(18) 0.0069(17) -0.023(2) N10 0.098(4) 0.070(3) 0.074(3) 0.011(3) 0.010(3) -0.017(3) O18 0.075(3) 0.155(6) 0.118(5) 0.006(4) 0.000(3) -0.003(3) C7 0.077(4) 0.075(4) 0.064(3) 0.010(3) -0.002(3) -0.017(3) C8 0.150(8) 0.115(7) 0.102(6) 0.042(5) 0.020(6) 0.042(6) C9 0.164(10) 0.146(8) 0.090(6) 0.022(6) 0.018(6) -0.079(8) O1W 0.162(7) 0.139(6) 0.201(8) 0.108(6) 0.030(6) -0.008(5) O2W 0.59(3) 0.209(13) 0.202(12) 0.047(10) -0.236(17) -0.035(16) _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 Zn3 N3 1.979(3) 7_665 ? Zn3 N6 1.987(4) 8_556 ? Zn3 O18 1.992(6) . ? Zn3 N9 1.995(3) . ? Zn1 O3 1.976(2) . ? Zn1 N4 2.022(3) . ? Zn1 N8 2.028(3) . ? Zn1 N1 2.104(4) . ? Zn1 O15 2.223(4) . ? Zn2 O17 2.117(3) . ? Zn2 N2 2.119(3) . ? Zn2 O19 2.126(3) . ? Zn2 N5 2.143(3) . ? Zn2 N7 2.162(3) . ? Zn2 O16 2.168(3) . ? V3 O8 1.608(3) . ? V3 O9 1.791(3) . ? V3 O3 1.862(2) . ? V3 O13 1.981(2) . ? V3 O7 2.043(2) . ? V3 O6 2.251(2) . ? V3 V5 3.0790(9) 4 ? V3 V4 3.1043(8) . ? V5 O12 1.611(3) . ? V5 O5 1.827(3) . ? V5 O11 1.827(3) . ? V5 O7 1.992(2) 4 ? V5 O13 2.007(2) 4 ? V5 O6 2.273(2) . ? V5 V3 3.0790(9) 4 ? V5 V1 3.1076(8) . ? V5 V4 3.1127(9) . ? V6 O14 1.689(2) 4 ? V6 O14 1.689(2) . ? V6 O13 1.937(2) 4 ? V6 O13 1.937(2) . ? V6 O6 2.115(2) . ? V6 O6 2.115(2) 4 ? V6 V4 3.0771(6) . ? V6 V4 3.0771(6) 4 ? V4 O10 1.598(3) . ? V4 O4 1.821(3) . ? V4 O11 1.868(3) . ? V4 O9 1.912(3) . ? V4 O14 2.055(3) . ? V4 O6 2.305(2) . ? V4 V1 3.0608(10) . ? V2 O2 1.690(3) . ? V2 O2 1.690(3) 4 ? V2 O7 1.931(2) . ? V2 O7 1.931(2) 4 ? V2 O6 2.110(2) 4 ? V2 O6 2.110(2) . ? V2 V1 3.0601(7) 4 ? V2 V1 3.0601(7) . ? V1 O1 1.603(3) . ? V1 O4 1.830(3) . ? V1 O5 1.863(3) . ? V1 O3 1.918(3) . ? V1 O2 2.043(3) . ? V1 O6 2.311(2) . ? O7 V5 1.992(2) 4 ? O13 V5 2.007(2) 4 ? N3 C1 1.335(5) . ? N3 C2 1.348(5) . ? N3 Zn3 1.979(3) 7_655 ? N9 C5 1.342(5) . ? N9 C6 1.349(5) . ? N8 C5 1.298(5) . ? N8 N7 1.383(5) . ? N4 C3 1.309(5) . ? N4 N5 1.370(4) . ? N7 C6 1.307(5) . ? N2 C2 1.318(5) . ? N2 N1 1.381(4) . ? N1 C1 1.307(5) . ? O19 C7 1.226(7) . ? N5 C4 1.315(5) . ? N6 C3 1.339(5) . ? N6 C4 1.353(5) . ? N6 Zn3 1.987(4) 8 ? N10 C7 1.317(8) . ? N10 C9 1.416(10) . ? N10 C8 1.522(12) . ? 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 N3 Zn3 N6 113.06(15) 7_665 8_556 ? N3 Zn3 O18 110.6(2) 7_665 . ? N6 Zn3 O18 106.9(2) 8_556 . ? N3 Zn3 N9 106.40(14) 7_665 . ? N6 Zn3 N9 109.65(15) 8_556 . ? O18 Zn3 N9 110.2(2) . . ? O3 Zn1 N4 130.78(12) . . ? O3 Zn1 N8 126.19(12) . . ? N4 Zn1 N8 102.76(14) . . ? O3 Zn1 N1 89.95(11) . . ? N4 Zn1 N1 93.17(15) . . ? N8 Zn1 N1 92.31(14) . . ? O3 Zn1 O15 86.08(11) . . ? N4 Zn1 O15 87.85(16) . . ? N8 Zn1 O15 91.74(15) . . ? N1 Zn1 O15 175.50(12) . . ? O17 Zn2 N2 92.19(14) . . ? O17 Zn2 O19 89.88(15) . . ? N2 Zn2 O19 177.37(14) . . ? O17 Zn2 N5 172.48(14) . . ? N2 Zn2 N5 92.31(13) . . ? O19 Zn2 N5 85.46(14) . . ? O17 Zn2 N7 90.89(14) . . ? N2 Zn2 N7 90.38(12) . . ? O19 Zn2 N7 91.20(14) . . ? N5 Zn2 N7 95.10(13) . . ? O17 Zn2 O16 83.74(15) . . ? N2 Zn2 O16 85.70(13) . . ? O19 Zn2 O16 92.92(15) . . ? N5 Zn2 O16 90.59(14) . . ? N7 Zn2 O16 173.22(14) . . ? O8 V3 O9 104.65(13) . . ? O8 V3 O3 101.30(13) . . ? O9 V3 O3 96.20(12) . . ? O8 V3 O13 101.08(13) . . ? O9 V3 O13 92.23(11) . . ? O3 V3 O13 153.20(10) . . ? O8 V3 O7 98.65(12) . . ? O9 V3 O7 155.47(10) . . ? O3 V3 O7 86.55(10) . . ? O13 V3 O7 75.67(10) . . ? O8 V3 O6 173.44(12) . . ? O9 V3 O6 81.64(10) . . ? O3 V3 O6 79.60(9) . . ? O13 V3 O6 76.52(9) . . ? O7 V3 O6 74.88(9) . . ? O8 V3 V5 89.43(11) . 4 ? O9 V3 V5 131.99(8) . 4 ? O3 V3 V5 126.21(8) . 4 ? O13 V3 V5 39.77(7) . 4 ? O7 V3 V5 39.66(7) . 4 ? O6 V3 V5 84.87(6) . 4 ? O8 V3 V4 138.66(11) . . ? O9 V3 V4 34.29(8) . . ? O3 V3 V4 84.32(8) . . ? O13 V3 V4 88.55(7) . . ? O7 V3 V4 122.65(7) . . ? O6 V3 V4 47.78(6) . . ? V5 V3 V4 120.31(2) 4 . ? O12 V5 O5 102.57(14) . . ? O12 V5 O11 102.99(14) . . ? O5 V5 O11 94.51(13) . . ? O12 V5 O7 100.69(13) . 4 ? O5 V5 O7 89.94(11) . 4 ? O11 V5 O7 154.30(11) . 4 ? O12 V5 O13 100.80(13) . 4 ? O5 V5 O13 154.68(11) . 4 ? O11 V5 O13 89.60(11) . 4 ? O7 V5 O13 76.23(10) 4 4 ? O12 V5 O6 175.46(13) . . ? O5 V5 O6 80.36(10) . . ? O11 V5 O6 80.10(10) . . ? O7 V5 O6 75.72(9) 4 . ? O13 V5 O6 75.75(9) 4 . ? O12 V5 V3 90.48(11) . 4 ? O5 V5 V3 130.82(9) . 4 ? O11 V5 V3 128.74(9) . 4 ? O7 V5 V3 40.89(7) 4 4 ? O13 V5 V3 39.14(7) 4 4 ? O6 V5 V3 84.98(6) . 4 ? O12 V5 V1 135.41(12) . . ? O5 V5 V1 33.01(8) . . ? O11 V5 V1 83.41(8) . . ? O7 V5 V1 86.75(7) 4 . ? O13 V5 V1 123.54(7) 4 . ? O6 V5 V1 47.82(6) . . ? V3 V5 V1 120.00(2) 4 . ? O12 V5 V4 135.80(12) . . ? O5 V5 V4 83.29(9) . . ? O11 V5 V4 33.03(8) . . ? O7 V5 V4 123.28(7) 4 . ? O13 V5 V4 86.74(7) 4 . ? O6 V5 V4 47.59(6) . . ? V3 V5 V4 118.86(2) 4 . ? V1 V5 V4 58.95(2) . . ? O14 V6 O14 106.78(17) 4 . ? O14 V6 O13 97.21(11) 4 4 ? O14 V6 O13 96.80(11) . 4 ? O14 V6 O13 96.80(11) 4 . ? O14 V6 O13 97.21(11) . . ? O13 V6 O13 156.40(15) 4 . ? O14 V6 O6 165.91(11) 4 . ? O14 V6 O6 87.30(10) . . ? O13 V6 O6 81.04(9) 4 . ? O13 V6 O6 80.75(9) . . ? O14 V6 O6 87.30(10) 4 4 ? O14 V6 O6 165.91(11) . 4 ? O13 V6 O6 80.75(9) 4 4 ? O13 V6 O6 81.04(9) . 4 ? O6 V6 O6 78.61(13) . 4 ? O14 V6 V4 145.61(9) 4 . ? O14 V6 V4 38.84(8) . . ? O13 V6 V4 88.97(7) 4 . ? O13 V6 V4 90.12(7) . . ? O6 V6 V4 48.47(6) . . ? O6 V6 V4 127.08(7) 4 . ? O14 V6 V4 38.84(8) 4 4 ? O14 V6 V4 145.61(9) . 4 ? O13 V6 V4 90.12(7) 4 4 ? O13 V6 V4 88.97(7) . 4 ? O6 V6 V4 127.08(7) . 4 ? O6 V6 V4 48.47(6) 4 4 ? V4 V6 V4 175.55(4) . 4 ? O10 V4 O4 103.36(14) . . ? O10 V4 O11 102.92(15) . . ? O4 V4 O11 91.82(12) . . ? O10 V4 O9 100.18(14) . . ? O4 V4 O9 91.22(12) . . ? O11 V4 O9 155.32(11) . . ? O10 V4 O14 100.54(13) . . ? O4 V4 O14 156.05(11) . . ? O11 V4 O14 84.31(11) . . ? O9 V4 O14 83.03(10) . . ? O10 V4 O6 174.69(13) . . ? O4 V4 O6 81.65(10) . . ? O11 V4 O6 78.46(10) . . ? O9 V4 O6 77.77(9) . . ? O14 V4 O6 74.42(9) . . ? O10 V4 V1 136.49(11) . . ? O4 V4 V1 33.13(8) . . ? O11 V4 V1 84.15(9) . . ? O9 V4 V1 85.10(8) . . ? O14 V4 V1 122.95(7) . . ? O6 V4 V1 48.54(6) . . ? O10 V4 V6 131.56(12) . . ? O4 V4 V6 125.04(9) . . ? O11 V4 V6 79.35(8) . . ? O9 V4 V6 78.88(7) . . ? O14 V4 V6 31.03(7) . . ? O6 V4 V6 43.39(6) . . ? V1 V4 V6 91.93(2) . . ? O10 V4 V3 131.97(12) . . ? O4 V4 V3 82.25(9) . . ? O11 V4 V3 124.77(8) . . ? O9 V4 V3 31.85(7) . . ? O14 V4 V3 80.67(7) . . ? O6 V4 V3 46.32(6) . . ? V1 V4 V3 61.832(19) . . ? V6 V4 V3 61.319(17) . . ? O10 V4 V5 135.05(12) . . ? O4 V4 V5 82.15(9) . . ? O11 V4 V5 32.22(8) . . ? O9 V4 V5 124.51(8) . . ? O14 V4 V5 82.09(7) . . ? O6 V4 V5 46.74(6) . . ? V1 V4 V5 60.442(19) . . ? V6 V4 V5 61.956(18) . . ? V3 V4 V5 92.91(2) . . ? O2 V2 O2 105.36(18) . 4 ? O2 V2 O7 97.40(11) . . ? O2 V2 O7 97.09(11) 4 . ? O2 V2 O7 97.09(11) . 4 ? O2 V2 O7 97.40(11) 4 4 ? O7 V2 O7 155.99(15) . 4 ? O2 V2 O6 166.74(11) . 4 ? O2 V2 O6 87.90(11) 4 4 ? O7 V2 O6 80.98(9) . 4 ? O7 V2 O6 80.53(10) 4 4 ? O2 V2 O6 87.90(11) . . ? O2 V2 O6 166.74(11) 4 . ? O7 V2 O6 80.53(10) . . ? O7 V2 O6 80.98(9) 4 . ? O6 V2 O6 78.85(12) 4 . ? O2 V2 V1 144.29(10) . 4 ? O2 V2 V1 38.94(9) 4 4 ? O7 V2 V1 89.18(7) . 4 ? O7 V2 V1 90.15(7) 4 4 ? O6 V2 V1 48.97(6) 4 4 ? O6 V2 V1 127.81(7) . 4 ? O2 V2 V1 38.94(9) . . ? O2 V2 V1 144.29(10) 4 . ? O7 V2 V1 90.15(7) . . ? O7 V2 V1 89.18(7) 4 . ? O6 V2 V1 127.81(7) 4 . ? O6 V2 V1 48.97(6) . . ? V1 V2 V1 176.77(4) 4 . ? O1 V1 O4 104.34(15) . . ? O1 V1 O5 103.05(15) . . ? O4 V1 O5 91.78(13) . . ? O1 V1 O3 100.54(14) . . ? O4 V1 O3 91.21(12) . . ? O5 V1 O3 154.67(11) . . ? O1 V1 O2 99.44(14) . . ? O4 V1 O2 156.16(11) . . ? O5 V1 O2 84.47(11) . . ? O3 V1 O2 82.70(11) . . ? O1 V1 O6 173.95(14) . . ? O4 V1 O6 81.32(10) . . ? O5 V1 O6 78.65(10) . . ? O3 V1 O6 76.96(9) . . ? O2 V1 O6 74.85(9) . . ? O1 V1 V2 130.75(13) . . ? O4 V1 V2 124.85(8) . . ? O5 V1 V2 79.53(8) . . ? O3 V1 V2 78.15(7) . . ? O2 V1 V2 31.32(7) . . ? O6 V1 V2 43.54(6) . . ? O1 V1 V4 137.29(13) . . ? O4 V1 V4 32.95(8) . . ? O5 V1 V4 84.25(9) . . ? O3 V1 V4 84.67(8) . . ? O2 V1 V4 123.23(7) . . ? O6 V1 V4 48.38(6) . . ? V2 V1 V4 91.91(2) . . ? O1 V1 V5 135.29(12) . . ? O4 V1 V5 82.17(8) . . ? O5 V1 V5 32.29(8) . . ? O3 V1 V5 123.78(7) . . ? O2 V1 V5 82.18(7) . . ? O6 V1 V5 46.82(6) . . ? V2 V1 V5 61.917(18) . . ? V4 V1 V5 60.606(19) . . ? V2 O2 V1 109.74(13) . . ? V2 O7 V5 107.93(11) . 4 ? V2 O7 V3 107.65(11) . . ? V5 O7 V3 99.45(11) 4 . ? V6 O14 V4 110.13(13) . . ? V4 O4 V1 113.92(13) . . ? V6 O13 V3 107.13(11) . . ? V6 O13 V5 107.74(11) . 4 ? V3 O13 V5 101.09(11) . 4 ? V5 O11 V4 114.76(13) . . ? V2 O6 V6 101.27(10) . . ? V2 O6 V3 94.71(9) . . ? V6 O6 V3 92.39(9) . . ? V2 O6 V5 92.68(9) . . ? V6 O6 V5 93.03(8) . . ? V3 O6 V5 169.81(12) . . ? V2 O6 V4 170.53(12) . . ? V6 O6 V4 88.13(8) . . ? V3 O6 V4 85.90(8) . . ? V5 O6 V4 85.66(8) . . ? V2 O6 V1 87.50(8) . . ? V6 O6 V1 171.16(12) . . ? V3 O6 V1 87.96(8) . . ? V5 O6 V1 85.36(8) . . ? V4 O6 V1 83.08(8) . . ? V5 O5 V1 114.71(13) . . ? V3 O9 V4 113.86(13) . . ? V3 O3 V1 113.85(12) . . ? V3 O3 Zn1 122.68(13) . . ? V1 O3 Zn1 122.69(13) . . ? C1 N3 C2 103.2(3) . . ? C1 N3 Zn3 122.6(3) . 7_655 ? C2 N3 Zn3 133.8(3) . 7_655 ? C5 N9 C6 102.3(3) . . ? C5 N9 Zn3 126.1(3) . . ? C6 N9 Zn3 131.1(3) . . ? C5 N8 N7 106.3(3) . . ? C5 N8 Zn1 132.3(3) . . ? N7 N8 Zn1 121.3(3) . . ? C3 N4 N5 106.7(3) . . ? C3 N4 Zn1 132.2(3) . . ? N5 N4 Zn1 120.4(3) . . ? C6 N7 N8 105.4(3) . . ? C6 N7 Zn2 131.8(3) . . ? N8 N7 Zn2 122.7(2) . . ? N8 C5 N9 113.0(4) . . ? C2 N2 N1 105.7(3) . . ? C2 N2 Zn2 134.8(3) . . ? N1 N2 Zn2 119.6(3) . . ? C1 N1 N2 106.3(3) . . ? C1 N1 Zn1 129.7(3) . . ? N2 N1 Zn1 124.0(2) . . ? N1 C1 N3 112.7(3) . . ? C7 O19 Zn2 128.9(4) . . ? C4 N5 N4 105.8(3) . . ? C4 N5 Zn2 129.8(3) . . ? N4 N5 Zn2 124.3(2) . . ? C3 N6 C4 102.8(3) . . ? C3 N6 Zn3 126.4(3) . 8 ? C4 N6 Zn3 130.2(3) . 8 ? N7 C6 N9 112.9(4) . . ? N5 C4 N6 112.2(3) . . ? N2 C2 N3 112.1(3) . . ? N4 C3 N6 112.4(4) . . ? C7 N10 C9 121.9(7) . . ? C7 N10 C8 121.4(6) . . ? C9 N10 C8 116.1(7) . . ? O19 C7 N10 125.7(7) . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 1.257 _refine_diff_density_min -0.611 _refine_diff_density_rms 0.134