data_(H3dien)[(VOPO4)2(OH)] .H2O (1) _audit_creation_method SHELXL-97 _chemical_formula_sum 'C4 H19 N3 O12 P2 V2' _chemical_formula_weight 465.04 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' 'P' 'P' 0.1023 0.0942 '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 17.8461(6) _cell_length_b 9.9884(4) _cell_length_c 18.4530(7) _cell_angle_alpha 90.00 _cell_angle_beta 117.3950(10) _cell_angle_gamma 90.00 _cell_volume 2920.44(19) _cell_formula_units_Z 8 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 8052 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 25 _exptl_crystal_description tabular _exptl_crystal_colour blue _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 2.115 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 1.569 _exptl_absorpt_correction_type Empirical _exptl_absorpt_correction_T_min 0.889 _exptl_absorpt_correction_T_max 0.979 _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_reflns_number 18485 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0411 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.29 _diffrn_reflns_theta_max 28.30 _reflns_number_total 7012 _reflns_number_gt 5770 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Brucker SMART' _computing_cell_refinement 'Brucker SMART' _computing_data_reduction 'Brucker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Brucker SHELXTL' _computing_publication_material 'Brucker 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^)+(0.0453P)^2^+3.1958P] 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_number_reflns 7012 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0561 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.0963 _refine_ls_wR_factor_gt 0.0908 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.006 _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 V1 V 0.06068(3) 0.44569(5) 0.27199(3) 0.01175(11) Uani 1 1 d . . . V2 V -0.12880(3) 0.40678(5) 0.08613(3) 0.01217(11) Uani 1 1 d . . . V3 V -0.47724(3) -0.47824(5) -0.19774(3) 0.01249(11) Uani 1 1 d . . . V4 V -0.37368(3) 0.11757(5) -0.08857(3) 0.01327(11) Uani 1 1 d . . . P1 P 0.11030(4) 0.13665(7) 0.28635(4) 0.01145(15) Uani 1 1 d . . . P2 P -0.48136(5) -0.15588(7) -0.13793(4) 0.01187(15) Uani 1 1 d . . . P3 P -0.28377(4) 0.40752(7) -0.09479(4) 0.01121(15) Uani 1 1 d . . . P4 P -0.18515(5) 0.12783(8) 0.07043(5) 0.01439(16) Uani 1 1 d . . . O1 O 0.10823(13) 0.2729(2) 0.32539(12) 0.0166(4) Uani 1 1 d . . . O2 O 0.14996(14) 0.1506(2) 0.23000(13) 0.0208(5) Uani 1 1 d . . . O3 O 0.01778(12) 0.0894(2) 0.23720(13) 0.0183(5) Uani 1 1 d . . . O4 O 0.16101(12) 0.0396(2) 0.35626(13) 0.0164(4) Uani 1 1 d . . . O5 O -0.39776(13) -0.0767(2) -0.09371(13) 0.0178(4) Uani 1 1 d . . . O6 O -0.45832(14) -0.3038(2) -0.13746(13) 0.0207(5) Uani 1 1 d . . . O7 O -0.53340(15) -0.1389(2) -0.09265(14) 0.0246(5) Uani 1 1 d . . . O8 O -0.53213(13) -0.1090(2) -0.22681(13) 0.0209(5) Uani 1 1 d . . . O9 O -0.22104(13) 0.4326(2) -0.12885(13) 0.0169(4) Uani 1 1 d . . . O10 O -0.24375(12) 0.4395(2) -0.00260(12) 0.0164(4) Uani 1 1 d . . . O11 O -0.35668(13) 0.5070(2) -0.13501(13) 0.0177(4) Uani 1 1 d . . . O12 O -0.31562(13) 0.2636(2) -0.11172(13) 0.0178(4) Uani 1 1 d . . . O13 O -0.13634(13) 0.2220(2) 0.04066(13) 0.0182(4) Uani 1 1 d . . . O14 O -0.26219(13) 0.0629(2) -0.00165(13) 0.0214(5) Uani 1 1 d . . . O15 O -0.12864(13) 0.0103(2) 0.11607(13) 0.0200(5) Uani 1 1 d . . . O16 O -0.21187(15) 0.2137(3) 0.12256(15) 0.0313(6) Uani 1 1 d . . . O17 O -0.04024(12) 0.3467(2) 0.19478(12) 0.0163(4) Uani 1 1 d . . . O18 O 0.11065(14) 0.4890(2) 0.22270(14) 0.0244(5) Uani 1 1 d . . . O19 O -0.07218(13) 0.4846(2) 0.05277(14) 0.0222(5) Uani 1 1 d . . . O21 O -0.52602(16) -0.5637(2) -0.16010(17) 0.0325(6) Uani 1 1 d . . . O20 O -0.55220(14) -0.3748(2) -0.29343(13) 0.0241(5) Uani 1 1 d . . . O22 O -0.42655(15) 0.1773(3) -0.04664(15) 0.0297(6) Uani 1 1 d . . . OW1 O -0.02434(18) 0.6367(4) 0.43406(18) 0.0498(8) Uani 1 1 d . . . OW2 O -0.34799(19) -0.3761(3) 0.02244(17) 0.0465(8) Uani 1 1 d . . . N1 N 0.39366(19) 0.4143(3) 0.42359(17) 0.0294(7) Uani 1 1 d . . . N2 N 0.25252(16) 0.3144(3) 0.20450(15) 0.0172(5) Uani 1 1 d . . . N3 N 0.22169(18) 0.2081(3) -0.00213(17) 0.0263(6) Uani 1 1 d . . . N4 N -0.05387(17) 0.3279(3) -0.06902(17) 0.0245(6) Uani 1 1 d . . . N5 N -0.21168(19) 0.2439(3) -0.22912(17) 0.0268(6) Uani 1 1 d . . . N6 N -0.35672(18) 0.1545(3) -0.41113(18) 0.0296(7) Uani 1 1 d . . . C1 C 0.3130(2) 0.3857(4) 0.3492(2) 0.0292(8) Uani 1 1 d . . . C2 C 0.3309(2) 0.3305(4) 0.2832(2) 0.0248(7) Uani 1 1 d . . . C3 C 0.2668(2) 0.2319(3) 0.14491(19) 0.0198(6) Uani 1 1 d . . . C4 C 0.1940(2) 0.2451(4) 0.0595(2) 0.0243(7) Uani 1 1 d . . . C5 C -0.2970(2) 0.1801(5) -0.2629(2) 0.0362(9) Uani 1 1 d . . . C6 C -0.3175(2) 0.0853(4) -0.3323(2) 0.0279(8) Uani 1 1 d . . . C7 C -0.1437(2) 0.1574(4) -0.1691(2) 0.0307(8) Uani 1 1 d . . . C8 C -0.0594(2) 0.2266(4) -0.1305(2) 0.0303(8) Uani 1 1 d . . . H1 H -0.0280 0.2559 0.1975 0.050 Uiso 1 1 d . . . H2 H -0.5539 -0.2889 -0.2788 0.050 Uiso 1 1 d . . . H3 H 0.2860 0.3133 0.3656 0.050 Uiso 1 1 d . . . H4 H 0.2812 0.4717 0.3323 0.050 Uiso 1 1 d . . . H5 H 0.3648 0.3859 0.2764 0.050 Uiso 1 1 d . . . H6 H 0.3563 0.2508 0.2969 0.050 Uiso 1 1 d . . . H7 H 0.2707 0.1366 0.1636 0.050 Uiso 1 1 d . . . H8 H 0.3149 0.2596 0.1453 0.050 Uiso 1 1 d . . . H9 H 0.2553 0.2595 0.0023 0.050 Uiso 1 1 d . . . H10 H 0.1731 0.3256 0.0526 0.050 Uiso 1 1 d . . . H11 H -0.2994 0.1389 -0.2159 0.050 Uiso 1 1 d . . . H12 H -0.3349 0.2525 -0.2792 0.050 Uiso 1 1 d . . . H13 H -0.2658 0.0408 -0.3282 0.050 Uiso 1 1 d . . . H14 H -0.3555 0.0163 -0.3325 0.050 Uiso 1 1 d . . . H17 H -0.1602 0.1342 -0.1263 0.050 Uiso 1 1 d . . . H18 H -0.1387 0.0824 -0.1995 0.050 Uiso 1 1 d . . . H19 H -0.0166 0.1558 -0.0970 0.050 Uiso 1 1 d . . . H20 H -0.0509 0.2708 -0.1707 0.050 Uiso 1 1 d . . . H21 H 0.4264 0.5082 0.4225 0.050 Uiso 1 1 d . . . H22 H 0.4248 0.3589 0.4325 0.050 Uiso 1 1 d . . . H23 H 0.3868 0.4306 0.4635 0.050 Uiso 1 1 d . . . H24 H 0.2372 0.4002 0.1846 0.050 Uiso 1 1 d . . . H25 H 0.2158 0.2801 0.2143 0.050 Uiso 1 1 d . . . H26 H 0.1859 0.2101 -0.0496 0.050 Uiso 1 1 d . . . H27 H -0.1011 0.3648 -0.0833 0.050 Uiso 1 1 d . . . H28 H -0.0195 0.3911 -0.0648 0.050 Uiso 1 1 d . . . H29 H -0.0349 0.2940 -0.0249 0.050 Uiso 1 1 d . . . H30 H -0.2124 0.3203 -0.2032 0.050 Uiso 1 1 d . . . H31 H -0.2000 0.2602 -0.2647 0.050 Uiso 1 1 d . . . H32 H -0.3214 0.2042 -0.4174 0.050 Uiso 1 1 d . . . H33 H -0.4004 0.2107 -0.4165 0.050 Uiso 1 1 d . . . H34 H -0.3836 0.0993 -0.4534 0.050 Uiso 1 1 d . . . H35 H 0.1481 0.1879 0.0537 0.050 Uiso 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 V1 0.0105(2) 0.0105(2) 0.0114(2) -0.00006(18) 0.00256(19) 0.00001(18) V2 0.0107(2) 0.0115(2) 0.0110(2) -0.00091(18) 0.00223(19) 0.00016(18) V3 0.0110(2) 0.0110(2) 0.0127(2) -0.00047(18) 0.00309(19) 0.00085(18) V4 0.0123(2) 0.0136(2) 0.0109(2) 0.00013(18) 0.0029(2) -0.00199(18) P1 0.0110(3) 0.0096(3) 0.0116(3) 0.0012(3) 0.0034(3) -0.0007(3) P2 0.0122(3) 0.0102(3) 0.0111(3) 0.0002(3) 0.0035(3) -0.0006(3) P3 0.0099(3) 0.0108(3) 0.0107(3) 0.0002(3) 0.0028(3) -0.0005(3) P4 0.0124(3) 0.0118(4) 0.0125(4) 0.0000(3) 0.0002(3) 0.0003(3) O1 0.0160(10) 0.0120(10) 0.0157(10) -0.0009(8) 0.0020(9) 0.0012(8) O2 0.0254(12) 0.0206(12) 0.0211(11) 0.0011(9) 0.0147(10) -0.0030(9) O3 0.0121(10) 0.0137(11) 0.0192(11) 0.0041(9) -0.0013(9) -0.0028(8) O4 0.0135(10) 0.0134(10) 0.0180(11) 0.0047(8) 0.0034(9) -0.0007(8) O5 0.0138(10) 0.0139(11) 0.0177(11) 0.0012(8) 0.0002(9) -0.0035(8) O6 0.0244(11) 0.0133(11) 0.0161(11) -0.0021(8) 0.0023(9) 0.0046(9) O7 0.0276(12) 0.0244(12) 0.0285(13) -0.0040(10) 0.0187(11) -0.0016(10) O8 0.0204(11) 0.0183(11) 0.0135(11) 0.0038(9) -0.0011(9) -0.0065(9) O9 0.0165(10) 0.0164(11) 0.0207(11) 0.0003(9) 0.0110(9) -0.0015(8) O10 0.0138(10) 0.0188(11) 0.0121(10) -0.0005(8) 0.0022(8) 0.0018(8) O11 0.0116(10) 0.0180(11) 0.0168(10) -0.0001(8) 0.0008(9) 0.0038(8) O12 0.0205(11) 0.0132(11) 0.0162(11) 0.0003(8) 0.0053(9) -0.0051(8) O13 0.0179(11) 0.0127(10) 0.0209(11) -0.0003(9) 0.0062(9) -0.0016(8) O14 0.0168(11) 0.0154(11) 0.0188(11) 0.0038(9) -0.0032(9) -0.0014(9) O15 0.0188(11) 0.0134(11) 0.0173(11) 0.0023(9) -0.0009(9) 0.0015(9) O16 0.0300(13) 0.0389(15) 0.0219(13) -0.0028(11) 0.0093(11) 0.0116(11) O17 0.0147(10) 0.0105(10) 0.0145(10) -0.0012(8) -0.0012(9) 0.0011(8) O18 0.0237(12) 0.0275(13) 0.0255(12) 0.0037(10) 0.0142(10) 0.0002(10) O19 0.0197(11) 0.0232(12) 0.0221(12) 0.0012(9) 0.0082(10) -0.0042(9) O21 0.0353(14) 0.0222(13) 0.0512(17) 0.0042(12) 0.0295(13) -0.0022(11) O20 0.0293(12) 0.0171(11) 0.0123(11) -0.0033(9) -0.0021(10) 0.0093(10) O22 0.0300(13) 0.0333(14) 0.0296(14) -0.0066(11) 0.0169(12) -0.0001(11) OW1 0.0337(16) 0.083(2) 0.0338(16) -0.0113(16) 0.0163(14) -0.0020(16) OW2 0.0547(19) 0.0439(18) 0.0344(16) 0.0011(13) 0.0148(15) 0.0114(15) N1 0.0307(16) 0.0346(17) 0.0188(14) -0.0042(12) 0.0081(13) -0.0055(13) N2 0.0179(12) 0.0183(13) 0.0158(13) -0.0002(10) 0.0081(11) -0.0018(10) N3 0.0288(15) 0.0316(16) 0.0148(13) -0.0022(12) 0.0068(12) 0.0022(13) N4 0.0215(14) 0.0253(15) 0.0251(15) -0.0050(12) 0.0093(12) -0.0032(11) N5 0.0320(16) 0.0257(16) 0.0197(14) -0.0059(12) 0.0093(13) 0.0024(12) N6 0.0263(15) 0.0344(18) 0.0266(16) -0.0030(13) 0.0107(13) -0.0007(13) C1 0.0245(17) 0.041(2) 0.0222(17) -0.0070(15) 0.0104(15) -0.0061(15) C2 0.0197(16) 0.0326(19) 0.0187(16) -0.0038(14) 0.0058(14) -0.0014(14) C3 0.0225(16) 0.0207(16) 0.0181(15) -0.0012(12) 0.0109(13) 0.0000(13) C4 0.0220(16) 0.0281(18) 0.0216(17) -0.0041(14) 0.0091(14) -0.0024(13) C5 0.0259(19) 0.057(3) 0.028(2) -0.0047(18) 0.0144(17) 0.0041(18) C6 0.0240(17) 0.0276(19) 0.034(2) 0.0007(15) 0.0147(16) -0.0011(14) C7 0.036(2) 0.0203(18) 0.0272(19) -0.0055(14) 0.0069(16) 0.0031(15) C8 0.0309(19) 0.032(2) 0.032(2) -0.0017(16) 0.0181(17) 0.0063(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 V1 O18 1.599(2) . ? V1 O3 1.958(2) 2 ? V1 O15 1.962(2) 2 ? V1 O17 1.972(2) . ? V1 O1 1.975(2) . ? V2 O19 1.605(2) . ? V2 O4 1.945(2) 2 ? V2 O10 1.976(2) . ? V2 O17 1.991(2) . ? V2 O13 2.006(2) . ? V3 O21 1.589(2) . ? V3 O11 1.923(2) 1_545 ? V3 O20 1.950(2) . ? V3 O8 1.971(2) 2_444 ? V3 O6 2.010(2) . ? V4 O22 1.586(2) . ? V4 O12 1.947(2) . ? V4 O20 1.961(2) 2_454 ? V4 O14 1.973(2) . ? V4 O5 1.980(2) . ? P1 O2 1.509(2) . ? P1 O4 1.533(2) . ? P1 O3 1.547(2) . ? P1 O1 1.548(2) . ? P2 O7 1.518(2) . ? P2 O6 1.533(2) . ? P2 O8 1.537(2) . ? P2 O5 1.548(2) . ? P3 O12 1.524(2) . ? P3 O11 1.531(2) . ? P3 O9 1.536(2) . ? P3 O10 1.545(2) . ? P4 O16 1.520(2) . ? P4 O15 1.524(2) . ? P4 O13 1.544(2) . ? P4 O14 1.548(2) . ? O3 V1 1.958(2) 2_545 ? O4 V2 1.945(2) 2_545 ? O8 V3 1.971(2) 2_454 ? O11 V3 1.923(2) 1_565 ? O15 V1 1.962(2) 2_545 ? O17 H1 0.9286 . ? O20 V4 1.961(2) 2_444 ? O20 H2 0.9041 . ? N1 C1 1.489(4) . ? N1 H21 1.1105 . ? N1 H22 0.7473 . ? N1 H23 0.8166 . ? N2 C3 1.487(4) . ? N2 C2 1.491(4) . ? N2 H24 0.9230 . ? N2 H25 0.8291 . ? N3 C4 1.481(4) . ? N3 H9 0.7647 . ? N3 H26 0.8130 . ? N4 C8 1.489(4) . ? N4 H27 0.8435 . ? N4 H28 0.8588 . ? N4 H29 0.7988 . ? N5 C7 1.486(5) . ? N5 C5 1.496(5) . ? N5 H30 0.9045 . ? N5 H31 0.7922 . ? N6 C6 1.465(5) . ? N6 H32 0.8509 . ? N6 H33 0.9280 . ? N6 H34 0.8943 . ? C1 C2 1.499(5) . ? C1 H3 0.9898 . ? C1 H4 0.9971 . ? C2 H5 0.8699 . ? C2 H6 0.8933 . ? C3 C4 1.519(4) . ? C3 H7 1.0044 . ? C3 H8 0.8979 . ? C4 H10 0.8705 . ? C4 H35 0.9627 . ? C5 C6 1.497(5) . ? C5 H11 0.9780 . ? C5 H12 0.9398 . ? C6 H13 0.9949 . ? C6 H14 0.9657 . ? C7 C8 1.504(5) . ? C7 H17 0.9886 . ? C7 H18 0.9637 . ? C8 H19 1.0156 . ? C8 H20 0.9338 . ? 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 O18 V1 O3 108.43(11) . 2 ? O18 V1 O15 105.87(11) . 2 ? O3 V1 O15 85.46(9) 2 2 ? O18 V1 O17 106.72(11) . . ? O3 V1 O17 85.77(9) 2 . ? O15 V1 O17 147.37(10) 2 . ? O18 V1 O1 107.23(11) . . ? O3 V1 O1 144.11(9) 2 . ? O15 V1 O1 81.18(9) 2 . ? O17 V1 O1 87.83(8) . . ? O19 V2 O4 106.02(11) . 2 ? O19 V2 O10 101.47(10) . . ? O4 V2 O10 83.39(9) 2 . ? O19 V2 O17 100.61(10) . . ? O4 V2 O17 87.28(9) 2 . ? O10 V2 O17 157.66(9) . . ? O19 V2 O13 102.59(11) . . ? O4 V2 O13 151.19(9) 2 . ? O10 V2 O13 87.79(9) . . ? O17 V2 O13 90.75(9) . . ? O21 V3 O11 112.45(12) . 1_545 ? O21 V3 O20 113.28(12) . . ? O11 V3 O20 134.18(10) 1_545 . ? O21 V3 O8 101.20(12) . 2_444 ? O11 V3 O8 86.52(9) 1_545 2_444 ? O20 V3 O8 87.55(9) . 2_444 ? O21 V3 O6 102.14(12) . . ? O11 V3 O6 82.92(9) 1_545 . ? O20 V3 O6 84.97(9) . . ? O8 V3 O6 156.59(10) 2_444 . ? O22 V4 O12 108.76(12) . . ? O22 V4 O20 106.15(12) . 2_454 ? O12 V4 O20 83.25(9) . 2_454 ? O22 V4 O14 108.13(12) . . ? O12 V4 O14 86.92(9) . . ? O20 V4 O14 145.70(11) 2_454 . ? O22 V4 O5 103.12(12) . . ? O12 V4 O5 148.13(9) . . ? O20 V4 O5 87.95(9) 2_454 . ? O14 V4 O5 83.30(9) . . ? O2 P1 O4 110.85(12) . . ? O2 P1 O3 109.66(13) . . ? O4 P1 O3 110.99(12) . . ? O2 P1 O1 111.01(12) . . ? O4 P1 O1 107.21(12) . . ? O3 P1 O1 107.04(12) . . ? O7 P2 O6 109.57(13) . . ? O7 P2 O8 110.11(13) . . ? O6 P2 O8 108.95(13) . . ? O7 P2 O5 109.77(13) . . ? O6 P2 O5 107.37(12) . . ? O8 P2 O5 111.01(12) . . ? O12 P3 O11 111.05(12) . . ? O12 P3 O9 110.08(12) . . ? O11 P3 O9 108.22(12) . . ? O12 P3 O10 111.14(12) . . ? O11 P3 O10 104.99(12) . . ? O9 P3 O10 111.23(12) . . ? O16 P4 O15 113.91(13) . . ? O16 P4 O13 105.90(14) . . ? O15 P4 O13 109.11(12) . . ? O16 P4 O14 111.52(14) . . ? O15 P4 O14 104.62(12) . . ? O13 P4 O14 111.88(12) . . ? P1 O1 V1 129.26(13) . . ? P1 O3 V1 143.34(13) . 2_545 ? P1 O4 V2 133.09(13) . 2_545 ? P2 O5 V4 131.39(13) . . ? P2 O6 V3 148.88(14) . . ? P2 O8 V3 139.08(13) . 2_454 ? P3 O10 V2 130.97(13) . . ? P3 O11 V3 143.85(14) . 1_565 ? P3 O12 V4 147.93(14) . . ? P4 O13 V2 110.59(12) . . ? P4 O14 V4 138.35(14) . . ? P4 O15 V1 140.05(14) . 2_545 ? V1 O17 V2 127.90(11) . . ? V1 O17 H1 109.7 . . ? V2 O17 H1 114.0 . . ? V3 O20 V4 144.70(12) . 2_444 ? V3 O20 H2 109.6 . . ? V4 O20 H2 105.7 2_444 . ? C1 N1 H21 116.0 . . ? C1 N1 H22 111.5 . . ? H21 N1 H22 106.6 . . ? C1 N1 H23 112.8 . . ? H21 N1 H23 98.4 . . ? H22 N1 H23 110.8 . . ? C3 N2 C2 112.1(2) . . ? C3 N2 H24 109.9 . . ? C2 N2 H24 105.1 . . ? C3 N2 H25 110.6 . . ? C2 N2 H25 108.2 . . ? H24 N2 H25 110.6 . . ? C4 N3 H9 105.8 . . ? C4 N3 H26 116.5 . . ? H9 N3 H26 106.8 . . ? C8 N4 H27 110.6 . . ? C8 N4 H28 111.3 . . ? H27 N4 H28 106.1 . . ? C8 N4 H29 109.7 . . ? H27 N4 H29 113.5 . . ? H28 N4 H29 105.6 . . ? C7 N5 C5 112.8(3) . . ? C7 N5 H30 107.6 . . ? C5 N5 H30 108.6 . . ? C7 N5 H31 107.6 . . ? C5 N5 H31 110.3 . . ? H30 N5 H31 109.8 . . ? C6 N6 H32 111.4 . . ? C6 N6 H33 112.7 . . ? H32 N6 H33 105.7 . . ? C6 N6 H34 113.2 . . ? H32 N6 H34 112.0 . . ? H33 N6 H34 101.1 . . ? N1 C1 C2 110.0(3) . . ? N1 C1 H3 105.0 . . ? C2 C1 H3 107.1 . . ? N1 C1 H4 107.1 . . ? C2 C1 H4 111.4 . . ? H3 C1 H4 116.0 . . ? N2 C2 C1 112.1(3) . . ? N2 C2 H5 109.3 . . ? C1 C2 H5 107.8 . . ? N2 C2 H6 107.8 . . ? C1 C2 H6 111.6 . . ? H5 C2 H6 108.1 . . ? N2 C3 C4 111.3(3) . . ? N2 C3 H7 106.2 . . ? C4 C3 H7 109.3 . . ? N2 C3 H8 108.1 . . ? C4 C3 H8 109.9 . . ? H7 C3 H8 112.0 . . ? N3 C4 C3 110.2(3) . . ? N3 C4 H10 113.0 . . ? C3 C4 H10 109.6 . . ? N3 C4 H35 109.5 . . ? C3 C4 H35 110.0 . . ? H10 C4 H35 104.3 . . ? N5 C5 C6 115.3(3) . . ? N5 C5 H11 105.2 . . ? C6 C5 H11 113.5 . . ? N5 C5 H12 104.5 . . ? C6 C5 H12 110.9 . . ? H11 C5 H12 106.8 . . ? N6 C6 C5 111.6(3) . . ? N6 C6 H13 106.8 . . ? C5 C6 H13 111.4 . . ? N6 C6 H14 108.6 . . ? C5 C6 H14 110.4 . . ? H13 C6 H14 107.9 . . ? N5 C7 C8 112.4(3) . . ? N5 C7 H17 106.9 . . ? C8 C7 H17 109.3 . . ? N5 C7 H18 106.3 . . ? C8 C7 H18 107.0 . . ? H17 C7 H18 115.1 . . ? N4 C8 C7 112.0(3) . . ? N4 C8 H19 104.0 . . ? C7 C8 H19 106.1 . . ? N4 C8 H20 107.8 . . ? C7 C8 H20 109.5 . . ? H19 C8 H20 117.4 . . ? _diffrn_measured_fraction_theta_max 0.964 _diffrn_reflns_theta_full 28.30 _diffrn_measured_fraction_theta_full 0.964 _refine_diff_density_max 1.030 _refine_diff_density_min -0.379 _refine_diff_density_rms 0.097