Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _publ_contact_author_name 'Dr Philip Lightfoot' _publ_contact_author_address ; School of Chemistry University of St Andrews St Andrews Fife KY16 9ST UNITED KINGDOM ; _publ_contact_author_email PL@ST-ANDREWS.AC.UK _publ_section_title ; The role of temperature in the solvothermal synthesis of hybrid vanadium oxyfluorides ; loop_ _publ_author_name 'Philip Lightfoot' 'David W. Aldous' 'Nicholas F. Stephens' data_I _database_code_depnum_ccdc_archive 'CCDC 650392' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3(C4 H12 N2), F8 O2 V2, 2(F4 H2 O2 V)' _chemical_formula_sum 'C12 H40 F16 N6 O6 V4' _chemical_formula_weight 872.26 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source V V 0.3005 0.5294 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.891(2) _cell_length_b 8.406(2) _cell_length_c 12.706(4) _cell_angle_alpha 77.569(10) _cell_angle_beta 84.464(13) _cell_angle_gamma 75.446(11) _cell_volume 695.0(3) _cell_formula_units_Z 1 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour blue _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.030 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.084 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 438 _exptl_absorpt_coefficient_mu 1.453 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8605 _exptl_absorpt_correction_T_max 0.9600 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Confocal Optics' _diffrn_measurement_device_type 'CCD Area Detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 3892 _diffrn_reflns_av_R_equivalents 0.0255 _diffrn_reflns_av_sigmaI/netI 0.0249 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 4 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 26.83 _reflns_number_total 2394 _reflns_number_gt 2049 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXL-90 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.In this structure solution, two distance restraints have been used. These both were 0.85 Angstroms and were used to restrain two hydrogen atoms attached to one oxygen atom, as a water molecule. ; _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^)+(0.0568P)^2^+1.7167P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2394 _refine_ls_number_parameters 207 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0500 _refine_ls_R_factor_gt 0.0405 _refine_ls_wR_factor_ref 0.1061 _refine_ls_wR_factor_gt 0.0998 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.034 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.28604(9) 0.38973(7) 0.88277(5) 0.01283(18) Uani 1 1 d . . . V2 V -0.04172(9) 1.12951(7) 0.59015(5) 0.01494(18) Uani 1 1 d . . . F1 F 0.3724(3) 0.1611(3) 0.89831(18) 0.0206(5) Uani 1 1 d . . . F2 F 0.2065(3) 0.6143(3) 0.82400(16) 0.0184(5) Uani 1 1 d . . . F3 F 0.5400(3) 0.4102(3) 0.87804(18) 0.0198(5) Uani 1 1 d . . . F4 F 0.0466(3) 0.3696(3) 0.84011(16) 0.0188(5) Uani 1 1 d . . . F5 F 0.0316(3) 0.9240(2) 0.69592(15) 0.0127(4) Uani 1 1 d . . . F6 F -0.1238(3) 1.2973(2) 0.46754(16) 0.0154(4) Uani 1 1 d . . . F7 F 0.1752(3) 1.0169(2) 0.48935(15) 0.0124(4) Uani 1 1 d . . . F8 F -0.2789(3) 1.1849(3) 0.66317(18) 0.0211(5) Uani 1 1 d . . . O1 O 0.2222(4) 0.3970(3) 1.0046(2) 0.0220(6) Uani 1 1 d . . . O2 O 0.3668(4) 0.3792(3) 0.7062(2) 0.0157(5) Uani 1 1 d D . . O3 O 0.1113(3) 1.2224(3) 0.63622(18) 0.0112(5) Uani 1 1 d . . . N1 N 0.0571(4) 1.0009(4) 0.8882(2) 0.0131(6) Uani 1 1 d . . . H1A H 0.0600 0.9581 0.8288 0.016 Uiso 1 1 calc R . . H1B H 0.1191 1.0859 0.8711 0.016 Uiso 1 1 calc R . . C1 C -0.1561(5) 1.0663(5) 0.9233(3) 0.0160(8) Uani 1 1 d . . . H1C H -0.2267 0.9772 0.9351 0.019 Uiso 1 1 calc R . . H1D H -0.2213 1.1556 0.8669 0.019 Uiso 1 1 calc R . . C2 C 0.1672(6) 0.8684(5) 0.9745(3) 0.0178(8) Uani 1 1 d . . . H2A H 0.3066 0.8330 0.9507 0.021 Uiso 1 1 calc R . . H2B H 0.1090 0.7717 0.9882 0.021 Uiso 1 1 calc R . . N2 N 0.1661(4) 1.3244(4) 0.2995(3) 0.0171(7) Uani 1 1 d . . . H2C H 0.1100 1.2527 0.3486 0.021 Uiso 1 1 calc R . . H2D H 0.0718 1.3854 0.2530 0.021 Uiso 1 1 calc R . . N3 N 0.5730(4) 1.2500(4) 0.3630(2) 0.0177(7) Uani 1 1 d . . . H3A H 0.6203 1.3239 0.3111 0.021 Uiso 1 1 calc R . . H3B H 0.6737 1.1925 0.4064 0.021 Uiso 1 1 calc R . . C3 C 0.3346(5) 1.2274(5) 0.2398(3) 0.0175(8) Uani 1 1 d . . . H3C H 0.3848 1.3033 0.1810 0.021 Uiso 1 1 calc R . . H3D H 0.2866 1.1489 0.2091 0.021 Uiso 1 1 calc R . . C4 C 0.5015(5) 1.1331(5) 0.3134(3) 0.0179(8) Uani 1 1 d . . . H4A H 0.4539 1.0517 0.3694 0.022 Uiso 1 1 calc R . . H4B H 0.6114 1.0731 0.2727 0.022 Uiso 1 1 calc R . . C5 C 0.4061(6) 1.3410(5) 0.4264(3) 0.0220(9) Uani 1 1 d . . . H5A H 0.4542 1.4175 0.4588 0.026 Uiso 1 1 calc R . . H5B H 0.3592 1.2613 0.4841 0.026 Uiso 1 1 calc R . . C6 C 0.2337(6) 1.4386(5) 0.3554(3) 0.0225(9) Uani 1 1 d . . . H6A H 0.1229 1.4912 0.3992 0.027 Uiso 1 1 calc R . . H6B H 0.2763 1.5263 0.3024 0.027 Uiso 1 1 calc R . . H1 H 0.476(4) 0.315(5) 0.692(4) 0.028(12) Uiso 1 1 d D . . H2 H 0.283(9) 0.341(9) 0.680(6) 0.09(3) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0124(3) 0.0121(3) 0.0115(3) 0.0014(2) -0.0044(2) 0.0001(2) V2 0.0233(3) 0.0096(3) 0.0090(3) -0.0005(2) -0.0046(2) 0.0018(2) F1 0.0209(11) 0.0109(10) 0.0261(12) 0.0029(9) -0.0040(9) -0.0009(8) F2 0.0225(11) 0.0123(10) 0.0158(11) 0.0007(9) -0.0040(9) 0.0026(8) F3 0.0155(11) 0.0216(12) 0.0223(11) -0.0016(9) -0.0071(9) -0.0041(9) F4 0.0126(10) 0.0258(12) 0.0168(11) -0.0028(9) -0.0039(8) -0.0026(8) F5 0.0147(10) 0.0114(10) 0.0096(10) 0.0013(8) -0.0036(8) -0.0002(8) F6 0.0177(10) 0.0118(10) 0.0143(10) 0.0015(8) -0.0049(8) -0.0009(8) F7 0.0109(10) 0.0147(10) 0.0103(9) -0.0019(8) -0.0001(7) -0.0013(8) F8 0.0171(11) 0.0231(12) 0.0223(12) -0.0078(10) -0.0008(9) -0.0008(9) O1 0.0228(14) 0.0271(15) 0.0135(13) 0.0000(11) -0.0056(11) -0.0027(11) O2 0.0144(13) 0.0151(13) 0.0165(13) -0.0055(11) -0.0017(10) 0.0008(10) O3 0.0134(12) 0.0090(12) 0.0117(12) -0.0029(10) -0.0029(9) -0.0018(9) N1 0.0147(15) 0.0153(15) 0.0092(14) -0.0010(12) -0.0009(11) -0.0046(12) C1 0.0119(17) 0.023(2) 0.0122(17) -0.0035(15) -0.0026(13) -0.0008(14) C2 0.0183(19) 0.020(2) 0.0121(18) -0.0045(15) -0.0033(14) 0.0035(15) N2 0.0095(15) 0.0194(16) 0.0187(16) 0.0035(13) -0.0056(12) -0.0009(12) N3 0.0108(15) 0.0293(18) 0.0128(15) -0.0003(13) -0.0043(12) -0.0064(13) C3 0.0190(19) 0.022(2) 0.0146(18) -0.0088(16) -0.0003(14) -0.0066(15) C4 0.0140(18) 0.0165(19) 0.0208(19) -0.0022(16) 0.0017(15) -0.0014(14) C5 0.020(2) 0.033(2) 0.019(2) -0.0147(18) 0.0024(15) -0.0101(17) C6 0.022(2) 0.0134(19) 0.032(2) -0.0072(17) 0.0040(17) -0.0036(15) _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 O1 1.578(3) . ? V1 F3 1.795(2) . ? V1 F1 1.836(2) . ? V1 F2 1.837(2) . ? V1 F4 1.843(2) . ? V1 O2 2.274(3) . ? V2 O3 1.672(2) . ? V2 F8 1.806(2) . ? V2 F6 1.886(2) . ? V2 F5 1.933(2) . ? V2 F7 2.052(2) . ? V2 F7 2.160(2) 2_576 ? F7 V2 2.160(2) 2_576 ? O2 H1 0.84(4) . ? O2 H2 0.85(7) . ? N1 C2 1.493(4) . ? N1 C1 1.495(4) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? C1 C2 1.503(5) 2_577 ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 C1 1.503(5) 2_577 ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? N2 C3 1.487(5) . ? N2 C6 1.492(5) . ? N2 H2C 0.9000 . ? N2 H2D 0.9000 . ? N3 C4 1.475(5) . ? N3 C5 1.484(5) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? C3 C4 1.502(5) . ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.516(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? 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 O1 V1 F3 100.67(13) . . ? O1 V1 F1 98.12(13) . . ? F3 V1 F1 91.01(10) . . ? O1 V1 F2 98.89(12) . . ? F3 V1 F2 89.28(10) . . ? F1 V1 F2 162.63(10) . . ? O1 V1 F4 98.24(12) . . ? F3 V1 F4 161.07(10) . . ? F1 V1 F4 87.26(10) . . ? F2 V1 F4 86.86(10) . . ? O1 V1 O2 177.99(12) . . ? F3 V1 O2 81.34(10) . . ? F1 V1 O2 81.99(10) . . ? F2 V1 O2 80.89(9) . . ? F4 V1 O2 79.75(10) . . ? O3 V2 F8 105.34(11) . . ? O3 V2 F6 97.63(10) . . ? F8 V2 F6 93.19(10) . . ? O3 V2 F5 93.80(10) . . ? F8 V2 F5 89.86(10) . . ? F6 V2 F5 166.93(9) . . ? O3 V2 F7 94.18(10) . . ? F8 V2 F7 160.36(9) . . ? F6 V2 F7 86.25(9) . . ? F5 V2 F7 86.62(8) . . ? O3 V2 F7 166.36(10) . 2_576 ? F8 V2 F7 88.21(9) . 2_576 ? F6 V2 F7 82.86(9) . 2_576 ? F5 V2 F7 84.54(8) . 2_576 ? F7 V2 F7 72.23(9) . 2_576 ? V2 F7 V2 107.77(9) . 2_576 ? V1 O2 H1 117(3) . . ? V1 O2 H2 111(5) . . ? H1 O2 H2 102(6) . . ? C2 N1 C1 111.6(3) . . ? C2 N1 H1A 109.3 . . ? C1 N1 H1A 109.3 . . ? C2 N1 H1B 109.3 . . ? C1 N1 H1B 109.3 . . ? H1A N1 H1B 108.0 . . ? N1 C1 C2 110.9(3) . 2_577 ? N1 C1 H1C 109.5 . . ? C2 C1 H1C 109.5 2_577 . ? N1 C1 H1D 109.5 . . ? C2 C1 H1D 109.5 2_577 . ? H1C C1 H1D 108.1 . . ? N1 C2 C1 110.5(3) . 2_577 ? N1 C2 H2A 109.6 . . ? C1 C2 H2A 109.6 2_577 . ? N1 C2 H2B 109.6 . . ? C1 C2 H2B 109.6 2_577 . ? H2A C2 H2B 108.1 . . ? C3 N2 C6 112.1(3) . . ? C3 N2 H2C 109.2 . . ? C6 N2 H2C 109.2 . . ? C3 N2 H2D 109.2 . . ? C6 N2 H2D 109.2 . . ? H2C N2 H2D 107.9 . . ? C4 N3 C5 109.9(3) . . ? C4 N3 H3A 109.7 . . ? C5 N3 H3A 109.7 . . ? C4 N3 H3B 109.7 . . ? C5 N3 H3B 109.7 . . ? H3A N3 H3B 108.2 . . ? N2 C3 C4 110.8(3) . . ? N2 C3 H3C 109.5 . . ? C4 C3 H3C 109.5 . . ? N2 C3 H3D 109.5 . . ? C4 C3 H3D 109.5 . . ? H3C C3 H3D 108.1 . . ? N3 C4 C3 110.3(3) . . ? N3 C4 H4A 109.6 . . ? C3 C4 H4A 109.6 . . ? N3 C4 H4B 109.6 . . ? C3 C4 H4B 109.6 . . ? H4A C4 H4B 108.1 . . ? N3 C5 C6 110.9(3) . . ? N3 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 . . ? N3 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 . . ? H5A C5 H5B 108.0 . . ? N2 C6 C5 110.2(3) . . ? N2 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? N2 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? 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 N1 H1A F5 0.90 1.81 2.690(4) 165.9 . N2 H2C F6 0.90 2.12 2.792(4) 130.9 . N1 H1B F1 0.90 2.08 2.855(4) 143.5 1_565 N2 H2C F5 0.90 2.16 2.754(4) 122.6 2_576 N2 H2D F4 0.90 2.14 2.925(4) 144.5 2_576 N3 H3A F2 0.90 2.04 2.874(4) 153.0 2_676 N3 H3B F7 0.90 2.07 2.902(4) 153.6 2_676 N3 H3B F5 0.90 2.41 2.863(4) 111.3 2_676 O2 H1 F8 0.84(4) 1.82(2) 2.656(3) 177(5) 1_645 O2 H2 O3 0.85(7) 1.91(7) 2.757(4) 171(7) 1_545 _diffrn_measured_fraction_theta_max 0.903 _diffrn_reflns_theta_full 26.83 _diffrn_measured_fraction_theta_full 0.903 _refine_diff_density_max 0.508 _refine_diff_density_min -0.515 _refine_diff_density_rms 0.100 #===end data_II _database_code_depnum_ccdc_archive 'CCDC 650393' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'F17 O3 V4, 4(C4 H12 N2), 4(H2 O)' _chemical_formula_sum 'C16 H56 F17 N8 O7 V4' _chemical_formula_weight 999.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source V V 0.3005 0.5294 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 '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 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.8730(14) _cell_length_b 12.7838(15) _cell_length_c 21.771(2) _cell_angle_alpha 91.217(4) _cell_angle_beta 90.464(4) _cell_angle_gamma 92.179(4) _cell_volume 3579.2(7) _cell_formula_units_Z 4 _cell_measurement_temperature 93(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Prism _exptl_crystal_colour Blue _exptl_crystal_size_max 0.2000 _exptl_crystal_size_mid 0.1000 _exptl_crystal_size_min 0.0500 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.855 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2036 _exptl_absorpt_coefficient_mu 1.151 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8035 _exptl_absorpt_correction_T_max 0.9400 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 93(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Confocal Optics' _diffrn_measurement_device_type 'CCD Area Detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22485 _diffrn_reflns_av_R_equivalents 0.0166 _diffrn_reflns_av_sigmaI/netI 0.0293 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.29 _diffrn_reflns_theta_max 25.35 _reflns_number_total 12308 _reflns_number_gt 11562 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2004)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2004)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXL-90 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.In this structure solution, sixteen distance restraints have been used. These were all of 0.85 Angstroms and were used to restrain sixteen hydrogen atoms attached to eight differnt oxygen atoms, all in water molecules. ; _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^)+(0.0338P)^2^+5.3644P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 12308 _refine_ls_number_parameters 1001 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0322 _refine_ls_R_factor_gt 0.0298 _refine_ls_wR_factor_ref 0.0787 _refine_ls_wR_factor_gt 0.0764 _refine_ls_goodness_of_fit_ref 0.984 _refine_ls_restrained_S_all 0.985 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.26893(3) 0.28589(3) 0.415275(17) 0.01250(9) Uani 1 1 d . . . V2 V 0.47627(3) 0.23798(3) 0.327518(17) 0.01257(9) Uani 1 1 d . . . V3 V 0.77012(3) 0.26430(3) 0.390389(16) 0.00901(8) Uani 1 1 d . . . V4 V 0.48813(3) 0.23674(3) 0.142602(16) 0.00987(8) Uani 1 1 d . . . V5 V 0.01467(3) 0.75744(3) 0.360478(16) 0.00960(8) Uani 1 1 d . . . V6 V -0.21783(3) 0.74165(3) 0.094266(16) 0.01008(8) Uani 1 1 d . . . V7 V 0.06249(3) 0.76444(3) 0.180140(17) 0.01219(9) Uani 1 1 d . . . V8 V 0.27157(3) 0.71606(3) 0.097930(19) 0.01798(10) Uani 1 1 d . . . F1 F 0.13910(11) 0.29596(13) 0.39498(7) 0.0312(4) Uani 1 1 d . . . F2 F 0.25773(11) 0.13680(10) 0.42839(6) 0.0195(3) Uani 1 1 d . . . F3 F 0.30544(11) 0.42557(10) 0.39480(7) 0.0245(3) Uani 1 1 d . . . F4 F 0.43378(9) 0.26400(9) 0.41744(5) 0.0115(2) Uani 1 1 d . . . F5 F 0.31646(9) 0.24786(10) 0.32728(5) 0.0120(3) Uani 1 1 d . . . F6 F 0.45048(10) 0.09130(9) 0.34743(6) 0.0147(3) Uani 1 1 d . . . F7 F 0.48475(10) 0.38434(10) 0.32125(6) 0.0178(3) Uani 1 1 d . . . F8 F 0.61046(11) 0.23091(12) 0.34597(7) 0.0276(3) Uani 1 1 d . . . F9 F 0.47150(11) 0.21650(11) 0.24681(6) 0.0259(3) Uani 1 1 d . . . F10 F 0.71951(10) 0.40430(10) 0.39309(6) 0.0183(3) Uani 1 1 d . . . F11 F 0.80443(9) 0.28705(9) 0.30478(5) 0.0127(3) Uani 1 1 d . . . F12 F 0.68870(10) 0.23333(10) 0.46239(6) 0.0169(3) Uani 1 1 d . . . F13 F 0.77372(11) 0.11758(10) 0.37074(6) 0.0180(3) Uani 1 1 d . . . F14 F 0.45621(10) 0.09085(10) 0.14276(6) 0.0178(3) Uani 1 1 d . . . F15 F 0.34389(10) 0.26425(10) 0.14882(6) 0.0182(3) Uani 1 1 d . . . F16 F 0.51144(9) 0.38464(9) 0.16764(6) 0.0130(3) Uani 1 1 d . . . F17 F 0.63015(9) 0.21983(10) 0.16969(6) 0.0136(3) Uani 1 1 d . . . F18 F -0.00740(9) 0.61126(9) 0.33179(5) 0.0122(3) Uani 1 1 d . . . F19 F -0.12077(9) 0.78365(10) 0.32717(6) 0.0154(3) Uani 1 1 d . . . F20 F 0.05429(10) 0.90335(10) 0.36422(6) 0.0157(3) Uani 1 1 d . . . F21 F 0.15963(10) 0.72398(10) 0.36188(6) 0.0180(3) Uani 1 1 d . . . F22 F -0.16461(10) 0.60201(9) 0.09077(6) 0.0154(3) Uani 1 1 d . . . F23 F -0.26400(10) 0.71129(10) 0.17740(6) 0.0149(3) Uani 1 1 d . . . F24 F -0.12414(10) 0.78027(10) 0.02832(5) 0.0165(3) Uani 1 1 d . . . F25 F -0.22599(10) 0.88747(9) 0.11760(6) 0.0144(3) Uani 1 1 d . . . F26 F 0.05070(11) 0.78040(11) 0.25966(6) 0.0249(3) Uani 1 1 d . . . F27 F -0.06662(10) 0.77432(11) 0.15154(6) 0.0220(3) Uani 1 1 d . . . F28 F 0.05172(10) 0.61630(9) 0.18334(6) 0.0153(3) Uani 1 1 d . . . F29 F 0.09296(9) 0.91266(9) 0.16753(5) 0.0115(2) Uani 1 1 d . . . F30 F 0.22047(9) 0.74631(9) 0.18761(5) 0.0114(2) Uani 1 1 d . . . F31 F 0.11577(9) 0.74667(9) 0.09262(5) 0.0107(2) Uani 1 1 d . . . F32 F 0.22843(11) 0.57368(10) 0.10956(6) 0.0216(3) Uani 1 1 d . . . F33 F 0.29409(11) 0.86549(10) 0.09752(6) 0.0213(3) Uani 1 1 d . . . F34 F 0.40255(11) 0.69047(14) 0.11996(7) 0.0338(4) Uani 1 1 d . . . O1 O 0.27383(11) 0.31776(12) 0.49479(6) 0.0125(3) Uani 1 1 d . . . O2 O 0.88288(12) 0.28790(13) 0.42053(7) 0.0194(4) Uani 1 1 d . . . O3 O 0.50932(13) 0.24855(13) 0.07019(7) 0.0176(3) Uani 1 1 d . . . O4 O -0.01564(14) 0.74316(13) 0.43085(7) 0.0212(4) Uani 1 1 d . . . O5 O -0.32516(13) 0.72231(13) 0.05765(8) 0.0218(4) Uani 1 1 d . . . O6 O 0.27915(12) 0.70172(12) 0.01925(7) 0.0154(3) Uani 1 1 d . . . N1 N 0.42032(14) 0.92258(14) 0.01186(9) 0.0153(4) Uani 1 1 d . . . H1A H 0.3704 0.8962 0.0364 0.018 Uiso 1 1 calc R . . H1B H 0.4223 0.8810 -0.0220 0.018 Uiso 1 1 calc R . . N2 N 0.01053(14) 0.94244(14) 0.05550(8) 0.0119(4) Uani 1 1 d . . . H2A H 0.0374 0.9365 0.0935 0.014 Uiso 1 1 calc R . . H2B H -0.0295 0.8846 0.0470 0.014 Uiso 1 1 calc R . . N3 N 0.49672(17) 0.50771(17) 0.06588(9) 0.0245(5) Uani 1 1 d . . . H3A H 0.4986 0.4768 0.1026 0.029 Uiso 1 1 calc R . . H3B H 0.4903 0.5769 0.0726 0.029 Uiso 1 1 calc R . . N4 N 0.02885(15) 0.55837(15) 0.05461(8) 0.0161(4) Uani 1 1 d . . . H4A H 0.0776 0.5854 0.0809 0.019 Uiso 1 1 calc R . . H4B H -0.0338 0.5761 0.0686 0.019 Uiso 1 1 calc R . . N5 N 0.54577(17) 0.43879(17) 0.45239(10) 0.0270(5) Uani 1 1 d . . . H5A H 0.6016 0.4217 0.4302 0.032 Uiso 1 1 calc R . . H5B H 0.4915 0.3973 0.4395 0.032 Uiso 1 1 calc R . . N6 N -0.00236(15) 0.49153(15) 0.43436(9) 0.0179(4) Uani 1 1 d . . . H6A H -0.0030 0.5215 0.3973 0.021 Uiso 1 1 calc R . . H6B H -0.0041 0.4216 0.4282 0.021 Uiso 1 1 calc R . . N7 N 0.53812(15) 0.08445(14) 0.46272(8) 0.0133(4) Uani 1 1 d . . . H7A H 0.4937 0.0800 0.4306 0.016 Uiso 1 1 calc R . . H7B H 0.5839 0.1380 0.4564 0.016 Uiso 1 1 calc R . . N8 N 0.09126(14) 0.02589(14) 0.46537(8) 0.0117(4) Uani 1 1 d . . . H8A H 0.0943 -0.0307 0.4402 0.014 Uiso 1 1 calc R . . H8B H 0.1453 0.0697 0.4568 0.014 Uiso 1 1 calc R . . N9 N -0.17907(14) 0.90747(14) 0.23906(8) 0.0130(4) Uani 1 1 d . . . H9A H -0.1400 0.8578 0.2551 0.016 Uiso 1 1 calc R . . H9B H -0.1940 0.8889 0.1998 0.016 Uiso 1 1 calc R . . N10 N -0.28408(14) 1.09867(14) 0.25049(8) 0.0127(4) Uani 1 1 d . . . H10A H -0.2683 1.1172 0.2897 0.015 Uiso 1 1 calc R . . H10B H -0.3233 1.1486 0.2348 0.015 Uiso 1 1 calc R . . N11 N -0.15511(14) 0.57870(14) 0.24389(8) 0.0121(4) Uani 1 1 d . . . H11A H -0.1776 0.6222 0.2151 0.014 Uiso 1 1 calc R . . H11B H -0.0961 0.6072 0.2605 0.014 Uiso 1 1 calc R . . N12 N -0.31223(14) 0.41308(14) 0.23726(8) 0.0130(4) Uani 1 1 d . . . H12A H -0.3713 0.3845 0.2207 0.016 Uiso 1 1 calc R . . H12B H -0.2895 0.3695 0.2659 0.016 Uiso 1 1 calc R . . N13 N 0.19720(15) 0.58231(15) 0.27373(9) 0.0175(4) Uani 1 1 d . . . H13A H 0.1672 0.6226 0.3024 0.021 Uiso 1 1 calc R . . H13B H 0.1781 0.6048 0.2366 0.021 Uiso 1 1 calc R . . N14 N 0.32654(15) 0.41538(15) 0.24140(10) 0.0207(4) Uani 1 1 d . . . H14A H 0.3570 0.3745 0.2132 0.025 Uiso 1 1 calc R . . H14B H 0.3453 0.3938 0.2788 0.025 Uiso 1 1 calc R . . N15 N 0.28704(14) 0.00171(14) 0.19564(8) 0.0129(4) Uani 1 1 d . . . H15A H 0.2389 -0.0447 0.1801 0.015 Uiso 1 1 calc R . . H15B H 0.3218 0.0300 0.1640 0.015 Uiso 1 1 calc R . . N16 N 0.26087(15) -0.00741(14) 0.32629(8) 0.0130(4) Uani 1 1 d . . . H16A H 0.2299 -0.0321 0.3602 0.016 Uiso 1 1 calc R . . H16B H 0.3109 0.0400 0.3382 0.016 Uiso 1 1 calc R . . C1 C 0.39265(17) 1.03008(17) -0.00651(10) 0.0148(5) Uani 1 1 d . . . H1C H 0.3820 1.0731 0.0300 0.018 Uiso 1 1 calc R . . H1D H 0.3283 1.0262 -0.0300 0.018 Uiso 1 1 calc R . . C2 C 0.52225(17) 0.92070(18) 0.04449(10) 0.0148(5) Uani 1 1 d . . . H2C H 0.5384 0.8489 0.0529 0.018 Uiso 1 1 calc R . . H2D H 0.5181 0.9584 0.0835 0.018 Uiso 1 1 calc R . . C3 C 0.09669(17) 0.94982(18) 0.01035(10) 0.0136(4) Uani 1 1 d . . . H3C H 0.1360 0.8866 0.0115 0.016 Uiso 1 1 calc R . . H3D H 0.1433 1.0087 0.0215 0.016 Uiso 1 1 calc R . . C4 C -0.05492(17) 1.03621(17) 0.05397(10) 0.0134(4) Uani 1 1 d . . . H4C H -0.0137 1.0980 0.0668 0.016 Uiso 1 1 calc R . . H4D H -0.1123 1.0275 0.0823 0.016 Uiso 1 1 calc R . . C5 C 0.59675(18) 0.48977(18) 0.03274(11) 0.0184(5) Uani 1 1 d . . . H5C H 0.6543 0.5223 0.0561 0.022 Uiso 1 1 calc R . . H5D H 0.6078 0.4152 0.0296 0.022 Uiso 1 1 calc R . . C6 C 0.40556(19) 0.4655(2) 0.03040(11) 0.0230(5) Uani 1 1 d . . . H6C H 0.3424 0.4824 0.0519 0.028 Uiso 1 1 calc R . . H6D H 0.4082 0.3899 0.0271 0.028 Uiso 1 1 calc R . . C7 C 0.04574(19) 0.60346(18) -0.00771(10) 0.0175(5) Uani 1 1 d . . . H7C H 0.1149 0.5883 -0.0219 0.021 Uiso 1 1 calc R . . H7D H 0.0402 0.6789 -0.0053 0.021 Uiso 1 1 calc R . . C8 C 0.03425(18) 0.44299(18) 0.05234(10) 0.0160(5) Uani 1 1 d . . . H8C H 0.0218 0.4155 0.0929 0.019 Uiso 1 1 calc R . . H8D H 0.1031 0.4236 0.0397 0.019 Uiso 1 1 calc R . . C9 C 0.5229(2) 0.5473(2) 0.44176(11) 0.0235(5) Uani 1 1 d . . . H9C H 0.5055 0.5558 0.3988 0.028 Uiso 1 1 calc R . . H9D H 0.5838 0.5917 0.4514 0.028 Uiso 1 1 calc R . . C10 C 0.5669(2) 0.4198(2) 0.51881(12) 0.0307(6) Uani 1 1 d . . . H10C H 0.6297 0.4589 0.5317 0.037 Uiso 1 1 calc R . . H10D H 0.5782 0.3460 0.5244 0.037 Uiso 1 1 calc R . . C11 C -0.09609(18) 0.52142(18) 0.46904(10) 0.0158(5) Uani 1 1 d . . . H11C H -0.1581 0.4967 0.4467 0.019 Uiso 1 1 calc R . . H11D H -0.0974 0.5971 0.4728 0.019 Uiso 1 1 calc R . . C12 C 0.09616(17) 0.52473(17) 0.46791(10) 0.0149(5) Uani 1 1 d . . . H12C H 0.1016 0.6005 0.4714 0.018 Uiso 1 1 calc R . . H12D H 0.1556 0.5011 0.4451 0.018 Uiso 1 1 calc R . . C13 C 0.47898(18) 0.10567(17) 0.52025(10) 0.0149(5) Uani 1 1 d . . . H13C H 0.4403 0.1688 0.5157 0.018 Uiso 1 1 calc R . . H13D H 0.5272 0.1168 0.5544 0.018 Uiso 1 1 calc R . . C14 C 0.59506(17) -0.01490(17) 0.46657(10) 0.0149(5) Uani 1 1 d . . . H14C H 0.6473 -0.0080 0.4989 0.018 Uiso 1 1 calc R . . H14D H 0.6302 -0.0281 0.4281 0.018 Uiso 1 1 calc R . . C15 C -0.00815(17) 0.07946(17) 0.45383(10) 0.0135(4) Uani 1 1 d . . . H15C H -0.0125 0.0984 0.4110 0.016 Uiso 1 1 calc R . . H15D H -0.0098 0.1431 0.4788 0.016 Uiso 1 1 calc R . . C16 C 0.09945(18) -0.00718(18) 0.53052(10) 0.0148(4) Uani 1 1 d . . . H16C H 0.1006 0.0540 0.5576 0.018 Uiso 1 1 calc R . . H16D H 0.1638 -0.0429 0.5365 0.018 Uiso 1 1 calc R . . C17 C -0.11898(17) 1.00943(17) 0.24073(10) 0.0139(4) Uani 1 1 d . . . H17A H -0.0562 1.0039 0.2167 0.017 Uiso 1 1 calc R . . H17B H -0.0992 1.0282 0.2827 0.017 Uiso 1 1 calc R . . C18 C -0.18603(18) 1.09225(17) 0.21457(10) 0.0145(5) Uani 1 1 d . . . H18A H -0.1485 1.1595 0.2162 0.017 Uiso 1 1 calc R . . H18B H -0.2026 1.0751 0.1719 0.017 Uiso 1 1 calc R . . C19 C -0.34457(17) 0.99749(17) 0.24924(10) 0.0147(5) Uani 1 1 d . . . H19A H -0.3660 0.9792 0.2074 0.018 Uiso 1 1 calc R . . H19B H -0.4065 1.0033 0.2740 0.018 Uiso 1 1 calc R . . C20 C -0.27750(17) 0.91397(17) 0.27425(10) 0.0137(4) Uani 1 1 d . . . H20A H -0.2614 0.9297 0.3171 0.016 Uiso 1 1 calc R . . H20B H -0.3153 0.8469 0.2718 0.016 Uiso 1 1 calc R . . C21 C -0.23523(18) 0.56716(18) 0.29269(10) 0.0158(5) Uani 1 1 d . . . H21A H -0.2498 0.6356 0.3099 0.019 Uiso 1 1 calc R . . H21B H -0.2087 0.5250 0.3254 0.019 Uiso 1 1 calc R . . C22 C -0.33419(17) 0.51592(17) 0.26678(11) 0.0151(5) Uani 1 1 d . . . H22A H -0.3840 0.5057 0.2995 0.018 Uiso 1 1 calc R . . H22B H -0.3643 0.5611 0.2367 0.018 Uiso 1 1 calc R . . C23 C -0.23222(18) 0.42497(18) 0.18829(10) 0.0161(5) Uani 1 1 d . . . H23A H -0.2587 0.4676 0.1558 0.019 Uiso 1 1 calc R . . H23B H -0.2178 0.3567 0.1707 0.019 Uiso 1 1 calc R . . C24 C -0.13318(17) 0.47567(17) 0.21448(10) 0.0143(5) Uani 1 1 d . . . H24A H -0.1036 0.4304 0.2447 0.017 Uiso 1 1 calc R . . H24B H -0.0830 0.4856 0.1819 0.017 Uiso 1 1 calc R . . C25 C 0.15943(18) 0.47205(17) 0.28037(11) 0.0167(5) Uani 1 1 d . . . H25A H 0.0848 0.4667 0.2737 0.020 Uiso 1 1 calc R . . H25B H 0.1740 0.4492 0.3217 0.020 Uiso 1 1 calc R . . C26 C 0.21248(17) 0.40301(18) 0.23439(11) 0.0164(5) Uani 1 1 d . . . H26A H 0.1909 0.3305 0.2405 0.020 Uiso 1 1 calc R . . H26B H 0.1923 0.4215 0.1931 0.020 Uiso 1 1 calc R . . C27 C 0.36415(18) 0.52591(18) 0.23398(12) 0.0208(5) Uani 1 1 d . . . H27A H 0.3480 0.5485 0.1929 0.025 Uiso 1 1 calc R . . H27B H 0.4390 0.5314 0.2398 0.025 Uiso 1 1 calc R . . C28 C 0.31246(18) 0.59434(18) 0.28043(11) 0.0176(5) Uani 1 1 d . . . H28A H 0.3331 0.5751 0.3215 0.021 Uiso 1 1 calc R . . H28B H 0.3343 0.6669 0.2746 0.021 Uiso 1 1 calc R . . C29 C 0.23384(17) 0.08617(17) 0.23040(10) 0.0132(4) Uani 1 1 d . . . H29A H 0.1816 0.1157 0.2043 0.016 Uiso 1 1 calc R . . H29B H 0.2842 0.1417 0.2419 0.016 Uiso 1 1 calc R . . C30 C 0.18294(17) 0.04398(18) 0.28754(10) 0.0154(5) Uani 1 1 d . . . H30A H 0.1529 0.1008 0.3107 0.019 Uiso 1 1 calc R . . H30B H 0.1274 -0.0062 0.2761 0.019 Uiso 1 1 calc R . . C31 C 0.30881(17) -0.09554(17) 0.29191(10) 0.0140(4) Uani 1 1 d . . . H31A H 0.2556 -0.1481 0.2803 0.017 Uiso 1 1 calc R . . H31B H 0.3594 -0.1280 0.3179 0.017 Uiso 1 1 calc R . . C32 C 0.36118(17) -0.05410(18) 0.23525(10) 0.0144(4) Uani 1 1 d . . . H32A H 0.4185 -0.0064 0.2473 0.017 Uiso 1 1 calc R . . H32B H 0.3894 -0.1118 0.2120 0.017 Uiso 1 1 calc R . . O7 O 0.25315(14) 0.86423(13) 0.43542(8) 0.0187(4) Uani 1 1 d D . . H17 H 0.228(2) 0.815(2) 0.4130(13) 0.043(9) Uiso 1 1 d D . . H27 H 0.267(2) 0.833(2) 0.4676(10) 0.027(8) Uiso 1 1 d D . . O8 O -0.46021(14) 0.74321(17) 0.21209(9) 0.0312(5) Uani 1 1 d D . . H18 H -0.4026(17) 0.731(3) 0.1963(14) 0.039(9) Uiso 1 1 d D . . H28 H -0.503(2) 0.730(3) 0.1832(13) 0.051(11) Uiso 1 1 d D . . O9 O 0.01332(13) 0.24630(15) 0.29431(8) 0.0240(4) Uani 1 1 d D . . H19 H 0.046(2) 0.262(3) 0.3263(11) 0.042(10) Uiso 1 1 d D . . H29 H -0.0480(15) 0.257(2) 0.3041(13) 0.030(8) Uiso 1 1 d D . . O10 O 0.16647(14) 0.19520(15) 0.09291(8) 0.0249(4) Uani 1 1 d D . . H110 H 0.165(2) 0.207(2) 0.0552(9) 0.033(8) Uiso 1 1 d D . . H210 H 0.2266(16) 0.214(3) 0.1041(15) 0.042(10) Uiso 1 1 d D . . O11 O 0.00159(15) 0.27451(16) 0.16626(9) 0.0298(4) Uani 1 1 d D . . H111 H 0.015(3) 0.269(3) 0.2034(9) 0.044(10) Uiso 1 1 d D . . H211 H 0.0476(19) 0.244(2) 0.1464(12) 0.028(8) Uiso 1 1 d D . . O12 O 0.29029(13) 0.21366(15) 0.59975(8) 0.0228(4) Uani 1 1 d D . . H112 H 0.2343(16) 0.211(2) 0.6180(12) 0.020(7) Uiso 1 1 d D . . H212 H 0.280(3) 0.244(2) 0.5666(11) 0.040(9) Uiso 1 1 d D . . O13 O 0.25308(16) 0.83399(16) -0.07342(9) 0.0317(4) Uani 1 1 d D . . H113 H 0.253(4) 0.781(3) -0.0463(18) 0.095(16) Uiso 1 1 d D . . H213 H 0.293(3) 0.813(3) -0.1043(14) 0.075(13) Uiso 1 1 d D . . O14 O 0.51327(16) 0.7493(2) 0.34144(10) 0.0417(6) Uani 1 1 d D . . H114 H 0.5732(16) 0.757(2) 0.3557(14) 0.034(9) Uiso 1 1 d D . . H214 H 0.524(3) 0.732(3) 0.3057(9) 0.038(9) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.01307(18) 0.01035(18) 0.01436(19) 0.00276(14) 0.00634(15) 0.00131(15) V2 0.01241(18) 0.01296(19) 0.01261(18) 0.00342(14) 0.00568(14) 0.00093(15) V3 0.00967(17) 0.00793(17) 0.00948(17) -0.00025(13) -0.00102(14) 0.00132(14) V4 0.00982(17) 0.01037(18) 0.00927(17) -0.00277(14) 0.00118(14) -0.00016(14) V5 0.01311(18) 0.00899(18) 0.00690(17) -0.00088(13) 0.00051(14) 0.00341(14) V6 0.01106(18) 0.00861(18) 0.01063(17) 0.00068(14) -0.00162(14) 0.00110(14) V7 0.01193(18) 0.00955(18) 0.01535(19) 0.00306(14) 0.00647(15) 0.00106(15) V8 0.0153(2) 0.0142(2) 0.0249(2) 0.00313(16) 0.01121(16) 0.00392(16) F1 0.0221(8) 0.0426(9) 0.0286(8) 0.0006(7) 0.0021(6) -0.0041(7) F2 0.0242(7) 0.0112(6) 0.0229(7) -0.0001(5) 0.0111(6) -0.0041(6) F3 0.0211(7) 0.0103(7) 0.0423(9) 0.0051(6) 0.0071(6) -0.0013(6) F4 0.0124(6) 0.0125(6) 0.0094(6) 0.0010(5) -0.0015(5) -0.0006(5) F5 0.0115(6) 0.0161(6) 0.0081(6) -0.0004(5) -0.0006(5) -0.0028(5) F6 0.0160(6) 0.0104(6) 0.0174(6) -0.0013(5) 0.0023(5) -0.0004(5) F7 0.0220(7) 0.0127(6) 0.0183(7) -0.0006(5) 0.0052(5) -0.0069(5) F8 0.0192(7) 0.0329(8) 0.0302(8) -0.0026(7) 0.0050(6) -0.0025(6) F9 0.0280(8) 0.0273(8) 0.0217(7) -0.0047(6) 0.0086(6) -0.0058(6) F10 0.0223(7) 0.0106(6) 0.0228(7) 0.0031(5) 0.0096(6) 0.0057(5) F11 0.0133(6) 0.0131(6) 0.0119(6) 0.0013(5) 0.0024(5) 0.0020(5) F12 0.0217(7) 0.0172(7) 0.0118(6) 0.0024(5) 0.0024(5) -0.0025(6) F13 0.0312(8) 0.0088(6) 0.0142(6) -0.0009(5) -0.0054(6) 0.0032(6) F14 0.0225(7) 0.0109(6) 0.0195(7) -0.0040(5) 0.0062(6) -0.0035(5) F15 0.0103(6) 0.0206(7) 0.0235(7) -0.0072(6) -0.0009(5) 0.0013(5) F16 0.0138(6) 0.0086(6) 0.0164(6) -0.0017(5) -0.0031(5) 0.0013(5) F17 0.0113(6) 0.0136(6) 0.0162(6) 0.0012(5) 0.0023(5) 0.0026(5) F18 0.0137(6) 0.0079(6) 0.0148(6) -0.0006(5) 0.0011(5) 0.0005(5) F19 0.0117(6) 0.0161(7) 0.0187(6) 0.0044(5) 0.0005(5) 0.0031(5) F20 0.0224(7) 0.0108(6) 0.0140(6) -0.0035(5) -0.0003(5) 0.0016(5) F21 0.0145(6) 0.0162(7) 0.0231(7) -0.0085(5) -0.0045(5) 0.0050(5) F22 0.0167(6) 0.0097(6) 0.0200(7) 0.0003(5) 0.0009(5) 0.0032(5) F23 0.0133(6) 0.0148(6) 0.0171(6) 0.0052(5) 0.0036(5) 0.0022(5) F24 0.0243(7) 0.0153(6) 0.0097(6) 0.0003(5) 0.0012(5) -0.0011(6) F25 0.0212(7) 0.0090(6) 0.0132(6) 0.0004(5) -0.0024(5) 0.0020(5) F26 0.0295(8) 0.0243(8) 0.0206(7) -0.0020(6) 0.0069(6) -0.0031(6) F27 0.0160(7) 0.0250(8) 0.0246(7) -0.0051(6) 0.0023(6) -0.0010(6) F28 0.0190(7) 0.0101(6) 0.0165(6) -0.0001(5) 0.0024(5) -0.0032(5) F29 0.0121(6) 0.0098(6) 0.0126(6) 0.0001(5) -0.0004(5) -0.0006(5) F30 0.0103(6) 0.0138(6) 0.0099(6) 0.0012(5) -0.0020(5) -0.0013(5) F31 0.0104(6) 0.0136(6) 0.0082(6) 0.0000(5) 0.0001(5) 0.0009(5) F32 0.0247(7) 0.0119(6) 0.0280(8) -0.0017(6) -0.0060(6) 0.0005(6) F33 0.0269(7) 0.0160(7) 0.0203(7) -0.0042(5) 0.0128(6) -0.0080(6) F34 0.0176(7) 0.0495(10) 0.0341(9) 0.0031(8) -0.0015(6) -0.0033(7) O1 0.0142(7) 0.0166(8) 0.0064(7) -0.0041(6) 0.0035(6) -0.0005(6) O2 0.0156(8) 0.0230(9) 0.0195(8) -0.0064(7) -0.0043(7) 0.0037(7) O3 0.0214(8) 0.0199(8) 0.0113(8) 0.0000(6) 0.0023(6) -0.0044(7) O4 0.0330(10) 0.0205(9) 0.0110(8) 0.0014(6) 0.0049(7) 0.0087(8) O5 0.0189(8) 0.0174(8) 0.0289(9) -0.0034(7) -0.0115(7) 0.0035(7) O6 0.0172(8) 0.0199(8) 0.0093(7) -0.0029(6) 0.0040(6) 0.0046(7) N1 0.0155(9) 0.0130(9) 0.0173(9) 0.0004(8) 0.0042(8) -0.0036(8) N2 0.0155(9) 0.0112(9) 0.0092(8) 0.0023(7) 0.0002(7) 0.0004(8) N3 0.0332(12) 0.0266(12) 0.0144(10) -0.0031(8) -0.0012(9) 0.0129(10) N4 0.0192(10) 0.0158(10) 0.0127(9) -0.0034(7) -0.0017(8) -0.0024(8) N5 0.0254(11) 0.0251(12) 0.0300(12) -0.0096(9) 0.0095(9) -0.0026(9) N6 0.0256(11) 0.0168(10) 0.0106(9) -0.0007(7) 0.0003(8) -0.0066(9) N7 0.0165(9) 0.0114(9) 0.0120(9) 0.0038(7) 0.0017(7) -0.0015(8) N8 0.0124(9) 0.0102(9) 0.0125(9) -0.0007(7) 0.0046(7) -0.0015(7) N9 0.0180(10) 0.0107(9) 0.0106(9) 0.0000(7) -0.0002(7) 0.0041(8) N10 0.0164(9) 0.0096(9) 0.0123(9) -0.0014(7) 0.0005(7) 0.0032(8) N11 0.0114(9) 0.0104(9) 0.0142(9) 0.0032(7) -0.0016(7) -0.0026(7) N12 0.0114(9) 0.0117(9) 0.0156(9) 0.0037(7) -0.0033(7) -0.0030(7) N13 0.0197(10) 0.0133(10) 0.0200(10) 0.0000(8) 0.0042(8) 0.0051(8) N14 0.0172(10) 0.0143(10) 0.0309(11) 0.0011(8) 0.0056(9) 0.0047(8) N15 0.0146(9) 0.0137(9) 0.0101(9) -0.0017(7) 0.0006(7) -0.0026(8) N16 0.0179(9) 0.0105(9) 0.0104(9) -0.0004(7) 0.0039(7) -0.0016(8) C1 0.0127(10) 0.0149(11) 0.0170(11) 0.0023(9) 0.0007(9) 0.0021(9) C2 0.0171(11) 0.0140(11) 0.0137(10) 0.0028(8) 0.0026(9) 0.0039(9) C3 0.0116(10) 0.0144(11) 0.0152(11) 0.0035(9) 0.0016(9) 0.0021(9) C4 0.0159(11) 0.0126(11) 0.0119(10) 0.0014(8) 0.0045(8) 0.0029(9) C5 0.0181(11) 0.0154(11) 0.0220(12) -0.0003(9) -0.0031(9) 0.0026(10) C6 0.0185(12) 0.0251(13) 0.0260(13) 0.0106(10) 0.0040(10) 0.0045(10) C7 0.0215(12) 0.0120(11) 0.0188(12) 0.0013(9) 0.0035(9) -0.0025(10) C8 0.0185(11) 0.0160(11) 0.0139(11) 0.0010(9) 0.0007(9) 0.0063(9) C9 0.0287(14) 0.0238(13) 0.0177(12) -0.0002(10) 0.0042(10) -0.0027(11) C10 0.0404(16) 0.0287(14) 0.0242(13) -0.0018(11) -0.0024(12) 0.0198(13) C11 0.0148(11) 0.0143(11) 0.0186(11) 0.0069(9) -0.0042(9) -0.0006(9) C12 0.0157(11) 0.0127(11) 0.0160(11) -0.0014(9) 0.0031(9) -0.0007(9) C13 0.0199(12) 0.0117(10) 0.0134(11) 0.0009(8) 0.0033(9) 0.0022(9) C14 0.0147(11) 0.0143(11) 0.0159(11) 0.0022(9) 0.0037(9) 0.0029(9) C15 0.0174(11) 0.0110(10) 0.0126(10) 0.0026(8) 0.0035(9) 0.0038(9) C16 0.0148(11) 0.0162(11) 0.0134(11) -0.0006(9) -0.0007(9) 0.0006(9) C17 0.0111(10) 0.0155(11) 0.0149(11) -0.0007(9) 0.0018(8) -0.0011(9) C18 0.0185(11) 0.0107(11) 0.0142(11) -0.0002(8) 0.0043(9) -0.0026(9) C19 0.0138(11) 0.0158(11) 0.0145(11) -0.0005(9) -0.0008(9) -0.0007(9) C20 0.0148(11) 0.0114(11) 0.0147(11) 0.0005(8) 0.0029(9) -0.0029(9) C21 0.0182(11) 0.0137(11) 0.0154(11) -0.0001(9) 0.0026(9) -0.0025(9) C22 0.0127(11) 0.0114(11) 0.0212(11) 0.0020(9) 0.0022(9) 0.0007(9) C23 0.0192(12) 0.0151(11) 0.0138(11) -0.0009(9) -0.0002(9) -0.0036(9) C24 0.0132(11) 0.0116(11) 0.0180(11) 0.0019(9) 0.0023(9) -0.0003(9) C25 0.0135(11) 0.0127(11) 0.0242(12) 0.0017(9) 0.0047(9) 0.0019(9) C26 0.0158(11) 0.0131(11) 0.0202(11) -0.0016(9) 0.0000(9) 0.0006(9) C27 0.0142(11) 0.0131(11) 0.0357(14) 0.0058(10) 0.0082(10) 0.0013(9) C28 0.0175(11) 0.0128(11) 0.0222(12) 0.0008(9) -0.0037(9) -0.0014(9) C29 0.0148(11) 0.0107(10) 0.0141(11) -0.0014(8) -0.0003(9) 0.0011(9) C30 0.0124(10) 0.0152(11) 0.0186(11) -0.0029(9) 0.0037(9) 0.0012(9) C31 0.0158(11) 0.0108(10) 0.0154(11) -0.0018(9) 0.0012(9) 0.0017(9) C32 0.0111(10) 0.0172(11) 0.0149(11) -0.0015(9) 0.0000(9) 0.0034(9) O7 0.0276(9) 0.0131(8) 0.0150(8) 0.0009(7) -0.0063(7) -0.0030(7) O8 0.0153(9) 0.0543(13) 0.0237(10) -0.0111(9) 0.0009(8) 0.0046(9) O9 0.0134(9) 0.0410(11) 0.0177(9) -0.0051(8) 0.0018(7) 0.0041(8) O10 0.0209(9) 0.0389(11) 0.0141(9) 0.0026(8) -0.0037(7) -0.0112(8) O11 0.0264(10) 0.0406(12) 0.0230(10) 0.0077(9) 0.0014(8) 0.0039(9) O12 0.0164(9) 0.0353(11) 0.0175(9) 0.0080(8) 0.0045(7) 0.0063(8) O13 0.0363(11) 0.0366(11) 0.0234(10) 0.0025(9) 0.0068(8) 0.0174(9) O14 0.0201(10) 0.0767(17) 0.0284(12) 0.0092(11) 0.0017(9) -0.0024(11) _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 F1 1.7354(15) . ? V1 O1 1.7701(14) . ? V1 F3 1.8924(14) . ? V1 F2 1.9334(13) . ? V1 F5 2.0695(12) . ? V1 F4 2.1514(13) . ? V2 F9 1.7728(14) . ? V2 F8 1.7765(15) . ? V2 F7 1.8780(13) . ? V2 F6 1.9503(13) . ? V2 F4 2.0605(12) . ? V2 F5 2.0659(13) . ? V3 O2 1.6036(16) . ? V3 F13 1.9173(13) . ? V3 F10 1.9277(13) . ? V3 F12 1.9322(13) . ? V3 F11 1.9443(12) . ? V3 F8 2.2858(15) . ? V4 O3 1.6113(15) . ? V4 F14 1.8945(13) . ? V4 F15 1.9082(13) . ? V4 F17 1.9377(13) . ? V4 F16 1.9679(13) . ? V4 F9 2.2998(15) . ? V5 O4 1.5966(15) . ? V5 F20 1.9148(13) . ? V5 F19 1.9267(13) . ? V5 F21 1.9304(13) . ? V5 F18 1.9673(12) . ? V5 F26 2.2700(14) . ? V6 O5 1.5980(16) . ? V6 F25 1.9286(13) . ? V6 F22 1.9364(13) . ? V6 F24 1.9424(13) . ? V6 F23 1.9517(13) . ? V6 F27 2.3227(14) . ? V7 F26 1.7473(14) . ? V7 F27 1.7800(14) . ? V7 F28 1.8964(13) . ? V7 F29 1.9460(12) . ? V7 F31 2.0415(12) . ? V7 F30 2.0611(12) . ? V8 O6 1.7228(15) . ? V8 F34 1.7932(15) . ? V8 F32 1.9055(14) . ? V8 F33 1.9214(14) . ? V8 F31 2.0609(12) . ? V8 F30 2.0983(12) . ? N1 C2 1.488(3) . ? N1 C1 1.495(3) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C3 1.490(3) . ? N2 C4 1.492(3) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N3 C6 1.478(3) . ? N3 C5 1.504(3) . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N4 C8 1.479(3) . ? N4 C7 1.499(3) . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? N5 C9 1.452(3) . ? N5 C10 1.496(3) . ? N5 H5A 0.9000 . ? N5 H5B 0.9000 . ? N6 C11 1.486(3) . ? N6 C12 1.501(3) . ? N6 H6A 0.9000 . ? N6 H6B 0.9000 . ? N7 C14 1.494(3) . ? N7 C13 1.496(3) . ? N7 H7A 0.9000 . ? N7 H7B 0.9000 . ? N8 C16 1.493(3) . ? N8 C15 1.496(3) . ? N8 H8A 0.9000 . ? N8 H8B 0.9000 . ? N9 C17 1.490(3) . ? N9 C20 1.490(3) . ? N9 H9A 0.9000 . ? N9 H9B 0.9000 . ? N10 C19 1.484(3) . ? N10 C18 1.494(3) . ? N10 H10A 0.9000 . ? N10 H10B 0.9000 . ? N11 C24 1.490(3) . ? N11 C21 1.492(3) . ? N11 H11A 0.9000 . ? N11 H11B 0.9000 . ? N12 C22 1.489(3) . ? N12 C23 1.495(3) . ? N12 H12A 0.9000 . ? N12 H12B 0.9000 . ? N13 C25 1.484(3) . ? N13 C28 1.491(3) . ? N13 H13A 0.9000 . ? N13 H13B 0.9000 . ? N14 C26 1.477(3) . ? N14 C27 1.489(3) . ? N14 H14A 0.9000 . ? N14 H14B 0.9000 . ? N15 C32 1.493(3) . ? N15 C29 1.496(3) . ? N15 H15A 0.9000 . ? N15 H15B 0.9000 . ? N16 C30 1.486(3) . ? N16 C31 1.495(3) . ? N16 H16A 0.9000 . ? N16 H16B 0.9000 . ? C1 C2 1.505(3) 2_675 ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 C1 1.505(3) 2_675 ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? C3 C4 1.512(3) 2_575 ? C3 H3C 0.9700 . ? C3 H3D 0.9700 . ? C4 C3 1.512(3) 2_575 ? C4 H4C 0.9700 . ? C4 H4D 0.9700 . ? C5 C6 1.501(3) 2_665 ? C5 H5C 0.9700 . ? C5 H5D 0.9700 . ? C6 C5 1.501(3) 2_665 ? C6 H6C 0.9700 . ? C6 H6D 0.9700 . ? C7 C8 1.507(3) 2_565 ? C7 H7C 0.9700 . ? C7 H7D 0.9700 . ? C8 C7 1.507(3) 2_565 ? C8 H8C 0.9700 . ? C8 H8D 0.9700 . ? C9 C10 1.513(3) 2_666 ? C9 H9C 0.9700 . ? C9 H9D 0.9700 . ? C10 C9 1.513(3) 2_666 ? C10 H10C 0.9700 . ? C10 H10D 0.9700 . ? C11 C12 1.505(3) 2_566 ? C11 H11C 0.9700 . ? C11 H11D 0.9700 . ? C12 C11 1.505(3) 2_566 ? C12 H12C 0.9700 . ? C12 H12D 0.9700 . ? C13 C14 1.507(3) 2_656 ? C13 H13C 0.9700 . ? C13 H13D 0.9700 . ? C14 C13 1.507(3) 2_656 ? C14 H14C 0.9700 . ? C14 H14D 0.9700 . ? C15 C16 1.513(3) 2_556 ? C15 H15C 0.9700 . ? C15 H15D 0.9700 . ? C16 C15 1.513(3) 2_556 ? C16 H16C 0.9700 . ? C16 H16D 0.9700 . ? C17 C18 1.509(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.506(3) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.510(3) . ? C21 H21A 0.9700 . ? C21 H21B 0.9700 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.510(3) . ? C23 H23A 0.9700 . ? C23 H23B 0.9700 . ? C24 H24A 0.9700 . ? C24 H24B 0.9700 . ? C25 C26 1.506(3) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 C28 1.499(3) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C30 1.511(3) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C30 H30A 0.9700 . ? C30 H30B 0.9700 . ? C31 C32 1.507(3) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? O7 H17 0.847(18) . ? O7 H27 0.834(17) . ? O8 H18 0.839(18) . ? O8 H28 0.840(18) . ? O9 H19 0.829(18) . ? O9 H29 0.835(18) . ? O10 H110 0.837(18) . ? O10 H210 0.834(18) . ? O11 H111 0.830(18) . ? O11 H211 0.838(17) . ? O12 H112 0.825(17) . ? O12 H212 0.838(18) . ? O13 H113 0.91(4) . ? O13 H213 0.896(19) . ? O14 H114 0.832(18) . ? O14 H214 0.818(18) . ? 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 F1 V1 O1 104.51(7) . . ? F1 V1 F3 94.09(7) . . ? O1 V1 F3 91.61(7) . . ? F1 V1 F2 94.55(7) . . ? O1 V1 F2 93.60(6) . . ? F3 V1 F2 168.47(6) . . ? F1 V1 F5 94.72(6) . . ? O1 V1 F5 160.70(6) . . ? F3 V1 F5 85.34(6) . . ? F2 V1 F5 86.35(5) . . ? F1 V1 F4 166.23(6) . . ? O1 V1 F4 89.26(6) . . ? F3 V1 F4 85.20(5) . . ? F2 V1 F4 84.59(5) . . ? F5 V1 F4 71.51(5) . . ? F9 V2 F8 103.70(7) . . ? F9 V2 F7 93.53(6) . . ? F8 V2 F7 92.96(7) . . ? F9 V2 F6 95.08(6) . . ? F8 V2 F6 91.59(6) . . ? F7 V2 F6 169.03(6) . . ? F9 V2 F4 162.58(6) . . ? F8 V2 F4 93.71(6) . . ? F7 V2 F4 86.23(5) . . ? F6 V2 F4 83.52(5) . . ? F9 V2 F5 89.14(6) . . ? F8 V2 F5 167.07(6) . . ? F7 V2 F5 87.69(5) . . ? F6 V2 F5 85.66(5) . . ? F4 V2 F5 73.44(5) . . ? O2 V3 F13 102.06(7) . . ? O2 V3 F10 98.95(7) . . ? F13 V3 F10 158.79(6) . . ? O2 V3 F12 101.09(7) . . ? F13 V3 F12 89.94(6) . . ? F10 V3 F12 88.81(6) . . ? O2 V3 F11 99.00(7) . . ? F13 V3 F11 86.40(5) . . ? F10 V3 F11 87.54(5) . . ? F12 V3 F11 159.90(6) . . ? O2 V3 F8 179.12(7) . . ? F13 V3 F8 77.83(6) . . ? F10 V3 F8 81.11(6) . . ? F12 V3 F8 79.79(6) . . ? F11 V3 F8 80.13(5) . . ? O3 V4 F14 98.38(7) . . ? O3 V4 F15 102.63(7) . . ? F14 V4 F15 90.20(6) . . ? O3 V4 F17 98.45(7) . . ? F14 V4 F17 93.04(6) . . ? F15 V4 F17 157.96(6) . . ? O3 V4 F16 98.14(7) . . ? F14 V4 F16 163.45(6) . . ? F15 V4 F16 85.27(5) . . ? F17 V4 F16 85.46(5) . . ? O3 V4 F9 175.44(7) . . ? F14 V4 F9 81.33(5) . . ? F15 V4 F9 81.93(6) . . ? F17 V4 F9 77.04(5) . . ? F16 V4 F9 82.27(5) . . ? O4 V5 F20 98.47(7) . . ? O4 V5 F19 99.23(8) . . ? F20 V5 F19 92.70(6) . . ? O4 V5 F21 101.33(8) . . ? F20 V5 F21 89.52(6) . . ? F19 V5 F21 158.75(6) . . ? O4 V5 F18 98.69(7) . . ? F20 V5 F18 162.58(5) . . ? F19 V5 F18 87.48(5) . . ? F21 V5 F18 84.21(5) . . ? O4 V5 F26 177.49(8) . . ? F20 V5 F26 81.24(5) . . ? F19 V5 F26 78.30(5) . . ? F21 V5 F26 81.17(6) . . ? F18 V5 F26 81.75(5) . . ? O5 V6 F25 100.93(7) . . ? O5 V6 F22 100.41(7) . . ? F25 V6 F22 158.49(6) . . ? O5 V6 F24 101.41(8) . . ? F25 V6 F24 89.60(5) . . ? F22 V6 F24 88.81(5) . . ? O5 V6 F23 99.83(8) . . ? F25 V6 F23 86.41(5) . . ? F22 V6 F23 87.34(5) . . ? F24 V6 F23 158.76(6) . . ? O5 V6 F27 176.97(7) . . ? F25 V6 F27 76.96(5) . . ? F22 V6 F27 81.60(5) . . ? F24 V6 F27 80.84(5) . . ? F23 V6 F27 77.93(5) . . ? F26 V7 F27 104.25(7) . . ? F26 V7 F28 93.17(6) . . ? F27 V7 F28 93.33(6) . . ? F26 V7 F29 93.62(6) . . ? F27 V7 F29 91.65(6) . . ? F28 V7 F29 170.34(5) . . ? F26 V7 F31 165.35(6) . . ? F27 V7 F31 90.31(6) . . ? F28 V7 F31 87.46(5) . . ? F29 V7 F31 84.24(5) . . ? F26 V7 F30 91.78(6) . . ? F27 V7 F30 163.96(6) . . ? F28 V7 F30 85.31(5) . . ? F29 V7 F30 87.61(5) . . ? F31 V7 F30 73.67(5) . . ? O6 V8 F34 100.66(7) . . ? O6 V8 F32 93.92(7) . . ? F34 V8 F32 91.52(7) . . ? O6 V8 F33 94.13(7) . . ? F34 V8 F33 94.66(7) . . ? F32 V8 F33 168.78(6) . . ? O6 V8 F31 91.59(6) . . ? F34 V8 F31 167.70(6) . . ? F32 V8 F31 86.51(6) . . ? F33 V8 F31 85.46(6) . . ? O6 V8 F30 163.99(7) . . ? F34 V8 F30 95.29(6) . . ? F32 V8 F30 87.10(6) . . ? F33 V8 F30 83.01(5) . . ? F31 V8 F30 72.50(5) . . ? V2 F4 V1 105.93(5) . . ? V2 F5 V1 108.80(5) . . ? V2 F8 V3 161.79(9) . . ? V2 F9 V4 163.22(8) . . ? V7 F26 V5 164.54(8) . . ? V7 F27 V6 161.16(8) . . ? V7 F30 V8 105.68(5) . . ? V7 F31 V8 107.81(5) . . ? C2 N1 C1 112.98(17) . . ? C2 N1 H1A 109.0 . . ? C1 N1 H1A 109.0 . . ? C2 N1 H1B 109.0 . . ? C1 N1 H1B 109.0 . . ? H1A N1 H1B 107.8 . . ? C3 N2 C4 111.58(16) . . ? C3 N2 H2A 109.3 . . ? C4 N2 H2A 109.3 . . ? C3 N2 H2B 109.3 . . ? C4 N2 H2B 109.3 . . ? H2A N2 H2B 108.0 . . ? C6 N3 C5 111.77(19) . . ? C6 N3 H3A 109.3 . . ? C5 N3 H3A 109.3 . . ? C6 N3 H3B 109.3 . . ? C5 N3 H3B 109.3 . . ? H3A N3 H3B 107.9 . . ? C8 N4 C7 111.10(17) . . ? C8 N4 H4A 109.4 . . ? C7 N4 H4A 109.4 . . ? C8 N4 H4B 109.4 . . ? C7 N4 H4B 109.4 . . ? H4A N4 H4B 108.0 . . ? C9 N5 C10 111.8(2) . . ? C9 N5 H5A 109.2 . . ? C10 N5 H5A 109.2 . . ? C9 N5 H5B 109.2 . . ? C10 N5 H5B 109.2 . . ? H5A N5 H5B 107.9 . . ? C11 N6 C12 111.81(17) . . ? C11 N6 H6A 109.3 . . ? C12 N6 H6A 109.3 . . ? C11 N6 H6B 109.3 . . ? C12 N6 H6B 109.3 . . ? H6A N6 H6B 107.9 . . ? C14 N7 C13 111.40(16) . . ? C14 N7 H7A 109.3 . . ? C13 N7 H7A 109.3 . . ? C14 N7 H7B 109.3 . . ? C13 N7 H7B 109.3 . . ? H7A N7 H7B 108.0 . . ? C16 N8 C15 111.33(16) . . ? C16 N8 H8A 109.4 . . ? C15 N8 H8A 109.4 . . ? C16 N8 H8B 109.4 . . ? C15 N8 H8B 109.4 . . ? H8A N8 H8B 108.0 . . ? C17 N9 C20 111.38(16) . . ? C17 N9 H9A 109.4 . . ? C20 N9 H9A 109.4 . . ? C17 N9 H9B 109.4 . . ? C20 N9 H9B 109.4 . . ? H9A N9 H9B 108.0 . . ? C19 N10 C18 111.76(16) . . ? C19 N10 H10A 109.3 . . ? C18 N10 H10A 109.3 . . ? C19 N10 H10B 109.3 . . ? C18 N10 H10B 109.3 . . ? H10A N10 H10B 107.9 . . ? C24 N11 C21 111.29(16) . . ? C24 N11 H11A 109.4 . . ? C21 N11 H11A 109.4 . . ? C24 N11 H11B 109.4 . . ? C21 N11 H11B 109.4 . . ? H11A N11 H11B 108.0 . . ? C22 N12 C23 111.25(17) . . ? C22 N12 H12A 109.4 . . ? C23 N12 H12A 109.4 . . ? C22 N12 H12B 109.4 . . ? C23 N12 H12B 109.4 . . ? H12A N12 H12B 108.0 . . ? C25 N13 C28 112.09(17) . . ? C25 N13 H13A 109.2 . . ? C28 N13 H13A 109.2 . . ? C25 N13 H13B 109.2 . . ? C28 N13 H13B 109.2 . . ? H13A N13 H13B 107.9 . . ? C26 N14 C27 112.04(18) . . ? C26 N14 H14A 109.2 . . ? C27 N14 H14A 109.2 . . ? C26 N14 H14B 109.2 . . ? C27 N14 H14B 109.2 . . ? H14A N14 H14B 107.9 . . ? C32 N15 C29 112.05(16) . . ? C32 N15 H15A 109.2 . . ? C29 N15 H15A 109.2 . . ? C32 N15 H15B 109.2 . . ? C29 N15 H15B 109.2 . . ? H15A N15 H15B 107.9 . . ? C30 N16 C31 111.03(17) . . ? C30 N16 H16A 109.4 . . ? C31 N16 H16A 109.4 . . ? C30 N16 H16B 109.4 . . ? C31 N16 H16B 109.4 . . ? H16A N16 H16B 108.0 . . ? N1 C1 C2 110.49(18) . 2_675 ? N1 C1 H1C 109.6 . . ? C2 C1 H1C 109.6 2_675 . ? N1 C1 H1D 109.6 . . ? C2 C1 H1D 109.6 2_675 . ? H1C C1 H1D 108.1 . . ? N1 C2 C1 110.85(18) . 2_675 ? N1 C2 H2C 109.5 . . ? C1 C2 H2C 109.5 2_675 . ? N1 C2 H2D 109.5 . . ? C1 C2 H2D 109.5 2_675 . ? H2C C2 H2D 108.1 . . ? N2 C3 C4 110.97(18) . 2_575 ? N2 C3 H3C 109.4 . . ? C4 C3 H3C 109.4 2_575 . ? N2 C3 H3D 109.4 . . ? C4 C3 H3D 109.4 2_575 . ? H3C C3 H3D 108.0 . . ? N2 C4 C3 109.96(17) . 2_575 ? N2 C4 H4C 109.7 . . ? C3 C4 H4C 109.7 2_575 . ? N2 C4 H4D 109.7 . . ? C3 C4 H4D 109.7 2_575 . ? H4C C4 H4D 108.2 . . ? C6 C5 N3 111.05(19) 2_665 . ? C6 C5 H5C 109.4 2_665 . ? N3 C5 H5C 109.4 . . ? C6 C5 H5D 109.4 2_665 . ? N3 C5 H5D 109.4 . . ? H5C C5 H5D 108.0 . . ? N3 C6 C5 111.0(2) . 2_665 ? N3 C6 H6C 109.4 . . ? C5 C6 H6C 109.4 2_665 . ? N3 C6 H6D 109.4 . . ? C5 C6 H6D 109.4 2_665 . ? H6C C6 H6D 108.0 . . ? N4 C7 C8 109.79(18) . 2_565 ? N4 C7 H7C 109.7 . . ? C8 C7 H7C 109.7 2_565 . ? N4 C7 H7D 109.7 . . ? C8 C7 H7D 109.7 2_565 . ? H7C C7 H7D 108.2 . . ? N4 C8 C7 110.08(18) . 2_565 ? N4 C8 H8C 109.6 . . ? C7 C8 H8C 109.6 2_565 . ? N4 C8 H8D 109.6 . . ? C7 C8 H8D 109.6 2_565 . ? H8C C8 H8D 108.2 . . ? N5 C9 C10 110.5(2) . 2_666 ? N5 C9 H9C 109.6 . . ? C10 C9 H9C 109.6 2_666 . ? N5 C9 H9D 109.6 . . ? C10 C9 H9D 109.6 2_666 . ? H9C C9 H9D 108.1 . . ? N5 C10 C9 111.0(2) . 2_666 ? N5 C10 H10C 109.4 . . ? C9 C10 H10C 109.4 2_666 . ? N5 C10 H10D 109.4 . . ? C9 C10 H10D 109.4 2_666 . ? H10C C10 H10D 108.0 . . ? N6 C11 C12 110.86(18) . 2_566 ? N6 C11 H11C 109.5 . . ? C12 C11 H11C 109.5 2_566 . ? N6 C11 H11D 109.5 . . ? C12 C11 H11D 109.5 2_566 . ? H11C C11 H11D 108.1 . . ? N6 C12 C11 109.72(18) . 2_566 ? N6 C12 H12C 109.7 . . ? C11 C12 H12C 109.7 2_566 . ? N6 C12 H12D 109.7 . . ? C11 C12 H12D 109.7 2_566 . ? H12C C12 H12D 108.2 . . ? N7 C13 C14 110.43(18) . 2_656 ? N7 C13 H13C 109.6 . . ? C14 C13 H13C 109.6 2_656 . ? N7 C13 H13D 109.6 . . ? C14 C13 H13D 109.6 2_656 . ? H13C C13 H13D 108.1 . . ? N7 C14 C13 110.65(18) . 2_656 ? N7 C14 H14C 109.5 . . ? C13 C14 H14C 109.5 2_656 . ? N7 C14 H14D 109.5 . . ? C13 C14 H14D 109.5 2_656 . ? H14C C14 H14D 108.1 . . ? N8 C15 C16 109.69(18) . 2_556 ? N8 C15 H15C 109.7 . . ? C16 C15 H15C 109.7 2_556 . ? N8 C15 H15D 109.7 . . ? C16 C15 H15D 109.7 2_556 . ? H15C C15 H15D 108.2 . . ? N8 C16 C15 110.18(18) . 2_556 ? N8 C16 H16C 109.6 . . ? C15 C16 H16C 109.6 2_556 . ? N8 C16 H16D 109.6 . . ? C15 C16 H16D 109.6 2_556 . ? H16C C16 H16D 108.1 . . ? N9 C17 C18 108.73(18) . . ? N9 C17 H17A 109.9 . . ? C18 C17 H17A 109.9 . . ? N9 C17 H17B 109.9 . . ? C18 C17 H17B 109.9 . . ? H17A C17 H17B 108.3 . . ? N10 C18 C17 109.89(17) . . ? N10 C18 H18A 109.7 . . ? C17 C18 H18A 109.7 . . ? N10 C18 H18B 109.7 . . ? C17 C18 H18B 109.7 . . ? H18A C18 H18B 108.2 . . ? N10 C19 C20 108.87(18) . . ? N10 C19 H19A 109.9 . . ? C20 C19 H19A 109.9 . . ? N10 C19 H19B 109.9 . . ? C20 C19 H19B 109.9 . . ? H19A C19 H19B 108.3 . . ? N9 C20 C19 110.96(17) . . ? N9 C20 H20A 109.4 . . ? C19 C20 H20A 109.4 . . ? N9 C20 H20B 109.4 . . ? C19 C20 H20B 109.4 . . ? H20A C20 H20B 108.0 . . ? N11 C21 C22 110.72(18) . . ? N11 C21 H21A 109.5 . . ? C22 C21 H21A 109.5 . . ? N11 C21 H21B 109.5 . . ? C22 C21 H21B 109.5 . . ? H21A C21 H21B 108.1 . . ? N12 C22 C21 110.22(18) . . ? N12 C22 H22A 109.6 . . ? C21 C22 H22A 109.6 . . ? N12 C22 H22B 109.6 . . ? C21 C22 H22B 109.6 . . ? H22A C22 H22B 108.1 . . ? N12 C23 C24 110.49(18) . . ? N12 C23 H23A 109.6 . . ? C24 C23 H23A 109.6 . . ? N12 C23 H23B 109.6 . . ? C24 C23 H23B 109.6 . . ? H23A C23 H23B 108.1 . . ? N11 C24 C23 110.06(18) . . ? N11 C24 H24A 109.6 . . ? C23 C24 H24A 109.6 . . ? N11 C24 H24B 109.6 . . ? C23 C24 H24B 109.6 . . ? H24A C24 H24B 108.2 . . ? N13 C25 C26 109.76(18) . . ? N13 C25 H25A 109.7 . . ? C26 C25 H25A 109.7 . . ? N13 C25 H25B 109.7 . . ? C26 C25 H25B 109.7 . . ? H25A C25 H25B 108.2 . . ? N14 C26 C25 110.33(19) . . ? N14 C26 H26A 109.6 . . ? C25 C26 H26A 109.6 . . ? N14 C26 H26B 109.6 . . ? C25 C26 H26B 109.6 . . ? H26A C26 H26B 108.1 . . ? N14 C27 C28 109.30(19) . . ? N14 C27 H27A 109.8 . . ? C28 C27 H27A 109.8 . . ? N14 C27 H27B 109.8 . . ? C28 C27 H27B 109.8 . . ? H27A C27 H27B 108.3 . . ? N13 C28 C27 110.09(19) . . ? N13 C28 H28A 109.6 . . ? C27 C28 H28A 109.6 . . ? N13 C28 H28B 109.6 . . ? C27 C28 H28B 109.6 . . ? H28A C28 H28B 108.2 . . ? N15 C29 C30 111.05(18) . . ? N15 C29 H29A 109.4 . . ? C30 C29 H29A 109.4 . . ? N15 C29 H29B 109.4 . . ? C30 C29 H29B 109.4 . . ? H29A C29 H29B 108.0 . . ? N16 C30 C29 110.11(17) . . ? N16 C30 H30A 109.6 . . ? C29 C30 H30A 109.6 . . ? N16 C30 H30B 109.6 . . ? C29 C30 H30B 109.6 . . ? H30A C30 H30B 108.2 . . ? N16 C31 C32 109.40(17) . . ? N16 C31 H31A 109.8 . . ? C32 C31 H31A 109.8 . . ? N16 C31 H31B 109.8 . . ? C32 C31 H31B 109.8 . . ? H31A C31 H31B 108.2 . . ? N15 C32 C31 111.46(17) . . ? N15 C32 H32A 109.3 . . ? C31 C32 H32A 109.3 . . ? N15 C32 H32B 109.3 . . ? C31 C32 H32B 109.3 . . ? H32A C32 H32B 108.0 . . ? H17 O7 H27 101(3) . . ? H18 O8 H28 103(3) . . ? H19 O9 H29 103(3) . . ? H110 O10 H210 104(3) . . ? H111 O11 H211 108(3) . . ? H112 O12 H212 107(3) . . ? H113 O13 H213 105(4) . . ? H114 O14 H214 102(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 N1 H1A F33 0.90 1.70 2.582(2) 164.7 . N2 H2A F29 0.90 1.79 2.692(2) 174.9 . N2 H2B F24 0.90 1.81 2.704(2) 172.2 . N3 H3A F16 0.90 1.87 2.754(2) 166.2 . N3 H3B F34 0.90 2.13 2.904(3) 144.0 . N4 H4A F32 0.90 2.05 2.824(2) 143.8 . N4 H4A F31 0.90 2.11 2.725(2) 124.7 . N4 H4A F28 0.90 2.29 2.894(2) 124.6 . N4 H4B F22 0.90 1.80 2.693(2) 174.1 . N5 H5A F10 0.90 1.75 2.638(2) 171.3 . N5 H5B F4 0.90 1.88 2.705(2) 150.6 . N6 H6A F18 0.90 1.85 2.736(2) 166.8 . N7 H7A F6 0.90 1.90 2.748(2) 156.5 . N7 H7B F12 0.90 1.79 2.665(2) 164.9 . N8 H8B F2 0.90 1.78 2.664(2) 168.4 . N9 H9A F19 0.90 1.87 2.635(2) 141.7 . N9 H9B F25 0.90 1.83 2.712(2) 165.2 . N9 H9B F23 0.90 2.45 2.985(2) 118.6 . N9 H9B F27 0.90 2.47 2.953(2) 114.3 . N11 H11A F23 0.90 1.82 2.681(2) 158.1 . N11 H11B F18 0.90 1.92 2.702(2) 144.5 . N13 H13A F21 0.90 1.82 2.670(2) 157.1 . N13 H13A F18 0.90 2.34 2.963(2) 126.2 . N13 H13B F28 0.90 2.00 2.758(2) 140.8 . N13 H13B F30 0.90 2.17 2.851(2) 131.6 . N14 H14A F15 0.90 1.97 2.779(2) 149.0 . N14 H14A F16 0.90 2.23 2.916(2) 132.8 . N14 H14B F7 0.90 2.02 2.713(3) 132.7 . N14 H14B F5 0.90 2.18 2.873(2) 132.9 . N15 H15B F14 0.90 1.93 2.697(2) 141.6 . N16 H16B F6 0.90 1.90 2.736(2) 154.3 . N16 H16B F2 0.90 2.42 2.859(2) 110.5 . O7 H17 F21 0.847(18) 1.789(19) 2.629(2) 171(3) . O8 H18 F23 0.839(18) 1.859(19) 2.686(2) 168(3) . O9 H19 F1 0.829(18) 1.938(19) 2.763(2) 173(3) . O10 H210 F15 0.834(18) 1.88(2) 2.689(2) 165(3) . O11 H111 O9 0.830(18) 2.01(2) 2.822(3) 167(3) . O11 H211 O10 0.838(17) 2.039(19) 2.869(3) 170(3) . O12 H212 O1 0.838(18) 1.846(19) 2.679(2) 173(3) . O13 H113 O6 0.91(4) 1.81(2) 2.687(2) 164(5) . N1 H1B O3 0.90 2.16 2.968(2) 148.7 2_665 N6 H6B O2 0.90 2.20 2.952(3) 140.1 1_455 N12 H12A F16 0.90 1.89 2.728(2) 153.2 1_455 N12 H12A F17 0.90 2.36 2.916(2) 120.0 1_455 N12 H12B F11 0.90 1.85 2.695(2) 156.4 1_455 O8 H28 F34 0.840(18) 1.881(19) 2.719(2) 175(4) 1_455 O9 H29 F11 0.835(18) 1.953(19) 2.769(2) 166(3) 1_455 N8 H8A F20 0.90 1.90 2.704(2) 147.7 1_545 N15 H15A F29 0.90 1.95 2.764(2) 149.3 1_545 N15 H15A F33 0.90 2.25 2.731(2) 113.3 1_545 N16 H16A O7 0.90 2.15 2.916(2) 141.9 1_545 N16 H16A F20 0.90 2.38 2.983(2) 124.5 1_545 N10 H10A F13 0.90 1.84 2.719(2) 164.4 1_465 N10 H10A F11 0.90 2.35 2.854(2) 115.5 1_465 N10 H10B F17 0.90 1.81 2.632(2) 150.5 1_465 O7 H27 F12 0.834(17) 1.858(18) 2.688(2) 174(3) 2_666 O14 H114 O12 0.832(18) 2.018(19) 2.844(3) 172(3) 2_666 O10 H110 F24 0.837(18) 1.902(19) 2.718(2) 164(3) 2_565 O12 H112 F19 0.825(17) 1.897(18) 2.712(2) 169(3) 2_566 O13 H213 F17 0.896(19) 1.788(19) 2.682(2) 175(4) 2_665 O14 H214 O8 0.818(18) 2.06(2) 2.839(3) 160(3) 1_655 _diffrn_measured_fraction_theta_max 0.942 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.942 _refine_diff_density_max 1.444 _refine_diff_density_min -0.548 _refine_diff_density_rms 0.066 #===end data_III _database_code_depnum_ccdc_archive 'CCDC 650394' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'F20 O3 V5, 4(C4 H12 N2), 2(H2O)' _chemical_formula_sum 'C16 H52 F20 N8 O5 V5' _chemical_formula_weight 1071.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source V V 0.3005 0.5294 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7781(17) _cell_length_b 12.5240(18) _cell_length_c 13.3317(19) _cell_angle_alpha 86.675(2) _cell_angle_beta 84.838(2) _cell_angle_gamma 67.417(2) _cell_volume 1807.8(5) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.100 _exptl_crystal_size_mid 0.030 _exptl_crystal_size_min 0.010 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.961 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1070.0 _exptl_absorpt_coefficient_mu 2.463 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0 _exptl_absorpt_correction_T_max 0 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.84600 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'SRS Daresbury Laboratories' _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13387 _diffrn_reflns_av_R_equivalents 0.0346 _diffrn_reflns_av_sigmaI/netI 0.0620 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.99 _diffrn_reflns_theta_max 33.11 _reflns_number_total 7374 _reflns_number_gt 5955 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SMART' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0856P)^2^+7.2189P] 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 7374 _refine_ls_number_parameters 481 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0776 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1755 _refine_ls_wR_factor_gt 0.1668 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 V1 V 0.33346(8) 0.85663(7) 0.27611(6) 0.0121(2) Uani 1 1 d . . . V2 V 0.13619(7) 0.67317(7) 0.25789(6) 0.00873(19) Uani 1 1 d . . . V3 V -0.15626(7) 0.83045(7) 0.22600(6) 0.0112(2) Uani 1 1 d . . . V4 V -0.33238(7) 0.63033(7) 0.22959(6) 0.00765(19) Uani 1 1 d . . . V5 V -0.19895(8) 0.35192(7) 0.25412(6) 0.0128(2) Uani 1 1 d . . . F1 F 0.4915(2) 0.7289(3) 0.2371(2) 0.0176(6) Uani 1 1 d . . . F2 F 0.4191(3) 0.9597(3) 0.2748(3) 0.0284(8) Uani 1 1 d . . . F3 F 0.3617(3) 0.8216(3) 0.4150(2) 0.0231(7) Uani 1 1 d . . . F4 F 0.2501(3) 0.7439(2) 0.2830(2) 0.0166(6) Uani 1 1 d . . . F5 F 0.3145(3) 0.8857(3) 0.1343(2) 0.0198(7) Uani 1 1 d . . . F6 F 0.1807(3) 0.9735(3) 0.3079(2) 0.0211(7) Uani 1 1 d . . . F7 F 0.1646(2) 0.6979(2) 0.1151(2) 0.0118(6) Uani 1 1 d . . . F8 F 0.0771(3) 0.6887(2) 0.3963(2) 0.0121(6) Uani 1 1 d . . . F9 F -0.0018(2) 0.8518(2) 0.2458(2) 0.0098(6) Uani 1 1 d . . . F10 F -0.0214(2) 0.6620(2) 0.2333(2) 0.0090(5) Uani 1 1 d . . . F11 F -0.1069(3) 0.8211(2) 0.0861(2) 0.0155(6) Uani 1 1 d . . . F12 F -0.1821(2) 0.8115(2) 0.3694(2) 0.0129(6) Uani 1 1 d . . . F13 F -0.2797(3) 0.7650(2) 0.2025(2) 0.0144(6) Uani 1 1 d . . . F14 F -0.3320(3) 0.6503(3) 0.3675(2) 0.0156(6) Uani 1 1 d . . . F15 F -0.3425(3) 0.6222(2) 0.0885(2) 0.0145(6) Uani 1 1 d . . . F16 F -0.1665(2) 0.5183(2) 0.2275(2) 0.0120(6) Uani 1 1 d . . . F17 F -0.3646(2) 0.4847(2) 0.2466(2) 0.0117(6) Uani 1 1 d . . . F18 F -0.2057(3) 0.3928(2) 0.3916(2) 0.0146(6) Uani 1 1 d . . . F19 F -0.0275(3) 0.2773(3) 0.2509(3) 0.0274(8) Uani 1 1 d . . . F20 F -0.1861(3) 0.3575(2) 0.1092(2) 0.0158(6) Uani 1 1 d . . . O1 O 0.2234(3) 0.5358(3) 0.2611(3) 0.0129(7) Uani 1 1 d . . . O2 O -0.2575(3) 0.9702(3) 0.2206(3) 0.0150(7) Uani 1 1 d . . . O3 O -0.2503(4) 0.2490(3) 0.2744(3) 0.0209(8) Uani 1 1 d . . . N1 N 0.9107(4) 0.0704(4) 0.9329(3) 0.0139(9) Uani 1 1 d . . . H11 H 0.8378 0.0898 0.9059 0.017 Uiso 1 1 calc R . . H12 H 0.9472 0.1174 0.9050 0.017 Uiso 1 1 calc R . . C1 C 0.8882(5) 0.0885(4) 1.0446(4) 0.0149(10) Uani 1 1 d . . . H1C H 0.8423 0.0433 1.0744 0.018 Uiso 1 1 calc R . . H1D H 0.8397 0.1695 1.0574 0.018 Uiso 1 1 calc R . . C2 C 0.9902(5) -0.0522(4) 0.9084(4) 0.0152(10) Uani 1 1 d . . . H2A H 1.0049 -0.0595 0.8359 0.018 Uiso 1 1 calc R . . H2B H 0.9481 -0.1025 0.9334 0.018 Uiso 1 1 calc R . . N2 N 0.9200(4) 0.5582(4) 0.4212(3) 0.0143(9) Uani 1 1 d . . . H21 H 0.8591 0.5637 0.3825 0.017 Uiso 1 1 calc R . . H22 H 0.9451 0.6164 0.4029 0.017 Uiso 1 1 calc R . . C3 C 1.0246(5) 0.4457(4) 0.4042(4) 0.0151(10) Uani 1 1 d . . . H3A H 1.0558 0.4417 0.3341 0.018 Uiso 1 1 calc R . . H3B H 0.9957 0.3832 0.4185 0.018 Uiso 1 1 calc R . . C4 C 0.8721(5) 0.5694(5) 0.5294(4) 0.0150(10) Uani 1 1 d . . . H4A H 0.8379 0.5112 0.5476 0.018 Uiso 1 1 calc R . . H4B H 0.8069 0.6449 0.5395 0.018 Uiso 1 1 calc R . . N3 N 0.5987(4) 0.3870(4) 0.4991(3) 0.0190(10) Uani 1 1 d . . . H31 H 0.6570 0.3986 0.4567 0.023 Uiso 1 1 calc R . . H32 H 0.6283 0.3125 0.5205 0.023 Uiso 1 1 calc R . . C5 C 0.5705(5) 0.4640(5) 0.5876(4) 0.0187(11) Uani 1 1 d . . . H5A H 0.6458 0.4501 0.6196 0.022 Uiso 1 1 calc R . . H5B H 0.5139 0.4459 0.6365 0.022 Uiso 1 1 calc R . . C6 C 0.4858(5) 0.4111(5) 0.4450(4) 0.0210(12) Uani 1 1 d . . . H6A H 0.4261 0.3913 0.4889 0.025 Uiso 1 1 calc R . . H6B H 0.5068 0.3631 0.3863 0.025 Uiso 1 1 calc R . . N4 N 0.0293(4) 0.5970(4) 0.0217(3) 0.0147(9) Uani 1 1 d . . . H41 H 0.0846 0.5958 -0.0298 0.018 Uiso 1 1 calc R . . H42 H 0.0196 0.6564 0.0610 0.018 Uiso 1 1 calc R . . C7 C 0.0763(5) 0.4861(5) 0.0815(4) 0.0168(11) Uani 1 1 d . . . H7A H 0.0190 0.4893 0.1393 0.020 Uiso 1 1 calc R . . H7B H 0.1551 0.4757 0.1061 0.020 Uiso 1 1 calc R . . C8 C -0.0914(5) 0.6141(4) -0.0183(4) 0.0158(10) Uani 1 1 d . . . H8A H -0.1526 0.6204 0.0372 0.019 Uiso 1 1 calc R . . H8B H -0.1198 0.6852 -0.0586 0.019 Uiso 1 1 calc R . . N5 N 0.4212(4) 0.0751(4) 0.5768(3) 0.0200(10) Uani 1 1 d . . . H51 H 0.3454 0.1164 0.6045 0.024 Uiso 1 1 calc R . . H52 H 0.4767 0.0837 0.6144 0.024 Uiso 1 1 calc R . . C9 C 0.4354(5) 0.1195(5) 0.4736(4) 0.0235(12) Uani 1 1 d . . . H9A H 0.4263 0.1997 0.4758 0.028 Uiso 1 1 calc R . . H9B H 0.3712 0.1164 0.4345 0.028 Uiso 1 1 calc R . . C10 C 0.4393(5) -0.0488(5) 0.5769(5) 0.0283(13) Uani 1 1 d . . . H10A H 0.3751 -0.0575 0.5414 0.034 Uiso 1 1 calc R . . H10B H 0.4333 -0.0770 0.6458 0.034 Uiso 1 1 calc R . . N6 N 0.3689(4) 0.5461(4) 0.0179(3) 0.0183(10) Uani 1 1 d . . . H61 H 0.3476 0.5072 -0.0268 0.022 Uiso 1 1 calc R . . H62 H 0.2993 0.5935 0.0510 0.022 Uiso 1 1 calc R . . C11 C 0.4482(5) 0.4625(5) 0.0911(4) 0.0205(11) Uani 1 1 d . . . H11A H 0.4049 0.4166 0.1242 0.025 Uiso 1 1 calc R . . H11B H 0.4668 0.5042 0.1422 0.025 Uiso 1 1 calc R . . C12 C 0.4332(5) 0.6160(5) -0.0366(5) 0.0229(12) Uani 1 1 d . . . H12A H 0.4514 0.6621 0.0108 0.027 Uiso 1 1 calc R . . H12B H 0.3801 0.6683 -0.0848 0.027 Uiso 1 1 calc R . . N7 N 0.0134(5) 0.9106(4) 0.4348(3) 0.0203(10) Uani 1 1 d . . . H71 H -0.0057 0.8516 0.4170 0.024 Uiso 1 1 calc R . . H72 H 0.0702 0.9183 0.3882 0.024 Uiso 1 1 calc R . . C13 C -0.0989(5) 1.0186(5) 0.4358(4) 0.0223(12) Uani 1 1 d . . . H13A H -0.1624 1.0098 0.4832 0.027 Uiso 1 1 calc R . . H13B H -0.1302 1.0346 0.3694 0.027 Uiso 1 1 calc R . . C14 C -0.0669(5) 1.1175(4) 0.4661(4) 0.0218(12) Uani 1 1 d . . . H14A H -0.0081 1.1301 0.4160 0.026 Uiso 1 1 calc R . . H14B H -0.1405 1.1878 0.4703 0.026 Uiso 1 1 calc R . . N8 N 0.4555(7) 0.0535(9) -0.0891(5) 0.105(4) Uani 1 1 d . . . H81 H 0.3946 0.0806 -0.1313 0.126 Uiso 1 1 calc R . . H82 H 0.5196 0.0697 -0.1173 0.126 Uiso 1 1 calc R . . C15 C 0.4116(7) 0.1146(6) 0.0090(6) 0.058(3) Uani 1 1 d . . . H15A H 0.3941 0.1965 -0.0014 0.069 Uiso 1 1 calc R . . H15B H 0.3366 0.1056 0.0365 0.069 Uiso 1 1 calc R . . C16 C 0.5089(8) 0.0636(10) 0.0785(8) 0.080(4) Uani 1 1 d . . . H16A H 0.5798 0.0816 0.0539 0.096 Uiso 1 1 calc R . . H16B H 0.4797 0.0981 0.1439 0.096 Uiso 1 1 calc R . . O4 O 0.3571(8) 0.2757(7) 0.2619(6) 0.099(3) Uiso 1 1 d . . . O5A O 0.1958(8) 0.1901(8) 0.3031(7) 0.0308(19) Uiso 0.50 1 d P . . O5B O 0.2102(9) 0.1826(8) 0.2269(7) 0.036(2) Uiso 0.50 1 d P . . 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 0.0125(4) 0.0082(4) 0.0150(4) 0.0027(3) -0.0061(3) -0.0025(3) V2 0.0073(4) 0.0075(4) 0.0099(4) -0.0002(3) -0.0012(3) -0.0011(3) V3 0.0088(4) 0.0153(4) 0.0096(4) 0.0012(3) -0.0006(3) -0.0050(3) V4 0.0059(4) 0.0057(4) 0.0100(4) 0.0010(3) -0.0029(3) -0.0003(3) V5 0.0153(4) 0.0066(4) 0.0125(4) -0.0003(3) -0.0027(3) 0.0007(3) F1 0.0073(14) 0.0149(15) 0.0249(17) -0.0014(12) -0.0021(12) 0.0024(12) F2 0.0227(17) 0.0177(17) 0.051(2) 0.0060(15) -0.0144(16) -0.0131(15) F3 0.0331(18) 0.0141(16) 0.0162(16) -0.0014(12) -0.0123(14) 0.0000(14) F4 0.0122(14) 0.0150(15) 0.0253(16) 0.0014(12) -0.0042(12) -0.0078(12) F5 0.0144(15) 0.0251(17) 0.0119(15) 0.0039(12) -0.0013(12) 0.0009(13) F6 0.0160(15) 0.0104(15) 0.0273(17) 0.0000(12) 0.0008(13) 0.0049(12) F7 0.0115(14) 0.0088(13) 0.0110(14) -0.0006(11) 0.0010(11) 0.0001(11) F8 0.0154(14) 0.0079(13) 0.0118(14) -0.0007(10) -0.0016(11) -0.0027(12) F9 0.0082(13) 0.0074(13) 0.0134(14) -0.0017(10) 0.0000(11) -0.0022(11) F10 0.0066(13) 0.0052(13) 0.0148(14) -0.0010(10) -0.0006(10) -0.0017(11) F11 0.0226(16) 0.0099(14) 0.0115(14) -0.0009(11) 0.0017(12) -0.0040(12) F12 0.0090(13) 0.0143(14) 0.0111(14) -0.0014(11) 0.0011(11) 0.0001(12) F13 0.0152(14) 0.0134(15) 0.0172(15) 0.0039(11) -0.0040(12) -0.0084(12) F14 0.0151(15) 0.0160(15) 0.0147(15) -0.0002(12) -0.0016(12) -0.0050(12) F15 0.0195(15) 0.0141(15) 0.0114(14) 0.0026(11) -0.0054(12) -0.0074(12) F16 0.0087(13) 0.0120(14) 0.0153(14) 0.0021(11) -0.0009(11) -0.0042(11) F17 0.0092(13) 0.0084(13) 0.0173(15) 0.0001(11) -0.0012(11) -0.0033(11) F18 0.0143(14) 0.0164(15) 0.0108(14) 0.0022(11) -0.0041(11) -0.0030(12) F19 0.0136(15) 0.0211(17) 0.038(2) -0.0087(15) -0.0065(14) 0.0066(13) F20 0.0179(15) 0.0155(15) 0.0135(14) -0.0027(11) -0.0003(12) -0.0057(13) O1 0.0097(16) 0.0050(16) 0.0212(19) -0.0009(13) -0.0009(14) 0.0003(13) O2 0.0185(18) 0.0041(16) 0.0182(18) -0.0012(13) 0.0026(15) -0.0003(14) O3 0.028(2) 0.0129(19) 0.025(2) 0.0048(15) -0.0060(17) -0.0110(17) N1 0.010(2) 0.010(2) 0.018(2) 0.0078(16) -0.0027(17) 0.0003(17) C1 0.012(2) 0.009(2) 0.017(3) 0.0017(19) 0.001(2) 0.003(2) C2 0.019(3) 0.007(2) 0.018(3) -0.0050(19) -0.003(2) -0.003(2) N2 0.011(2) 0.017(2) 0.015(2) 0.0053(17) -0.0075(17) -0.0056(18) C3 0.014(2) 0.012(2) 0.016(3) -0.0013(19) -0.002(2) -0.001(2) C4 0.010(2) 0.016(3) 0.016(3) 0.005(2) -0.0013(19) -0.003(2) N3 0.013(2) 0.015(2) 0.021(2) 0.0084(18) 0.0015(18) 0.0012(18) C5 0.015(3) 0.026(3) 0.013(3) 0.002(2) -0.002(2) -0.006(2) C6 0.023(3) 0.023(3) 0.019(3) 0.002(2) -0.001(2) -0.012(2) N4 0.018(2) 0.013(2) 0.017(2) -0.0064(17) -0.0012(17) -0.0090(18) C7 0.014(2) 0.021(3) 0.016(3) -0.002(2) -0.002(2) -0.008(2) C8 0.014(2) 0.014(2) 0.018(3) 0.001(2) 0.000(2) -0.003(2) N5 0.009(2) 0.026(3) 0.020(2) -0.0148(19) 0.0020(17) 0.0013(19) C9 0.016(3) 0.021(3) 0.026(3) -0.004(2) 0.003(2) 0.001(2) C10 0.020(3) 0.029(3) 0.031(3) -0.006(3) 0.009(2) -0.005(3) N6 0.008(2) 0.019(2) 0.025(2) -0.0111(19) -0.0031(18) 0.0004(18) C11 0.010(2) 0.023(3) 0.026(3) -0.002(2) -0.001(2) -0.004(2) C12 0.011(3) 0.016(3) 0.037(3) -0.003(2) -0.005(2) 0.000(2) N7 0.036(3) 0.009(2) 0.016(2) -0.0057(17) -0.001(2) -0.008(2) C13 0.012(2) 0.033(3) 0.016(3) -0.004(2) -0.004(2) -0.001(2) C14 0.031(3) 0.008(2) 0.015(3) 0.0021(19) -0.005(2) 0.007(2) N8 0.044(4) 0.155(9) 0.028(4) 0.015(5) -0.008(3) 0.058(5) C15 0.044(5) 0.026(4) 0.066(5) 0.025(4) 0.036(4) 0.015(3) C16 0.031(4) 0.115(9) 0.098(8) -0.076(7) 0.012(5) -0.026(6) _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 F6 1.864(3) . ? V1 F3 1.907(3) . ? V1 F2 1.918(3) . ? V1 F5 1.921(3) . ? V1 F1 1.982(3) . ? V1 F4 2.000(3) . ? V2 O1 1.631(3) . ? V2 F8 1.906(3) . ? V2 F4 1.930(3) . ? V2 F7 1.930(3) . ? V2 F10 1.972(3) . ? V2 F9 2.210(3) . ? V3 O2 1.699(3) . ? V3 F11 1.899(3) . ? V3 F12 1.924(3) . ? V3 F13 1.978(3) . ? V3 F9 1.979(3) . ? V3 F10 2.101(3) . ? V4 F14 1.870(3) . ? V4 F15 1.907(3) . ? V4 F16 1.917(3) . ? V4 F1 1.961(3) 1_455 ? V4 F17 1.997(3) . ? V4 F13 2.013(3) . ? V5 O3 1.621(4) . ? V5 F19 1.869(3) . ? V5 F18 1.918(3) . ? V5 F20 1.924(3) . ? V5 F17 2.027(3) . ? V5 F16 2.262(3) . ? F1 V4 1.961(3) 1_655 ? N1 C2 1.497(6) . ? N1 C1 1.503(6) . ? N1 H11 0.9000 . ? N1 H12 0.9000 . ? C1 C2 1.510(7) 2_757 ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 C1 1.510(7) 2_757 ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? N2 C3 1.486(6) . ? N2 C4 1.495(6) . ? N2 H21 0.9000 . ? N2 H22 0.9000 . ? C3 C4 1.516(7) 2_766 ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C3 1.516(7) 2_766 ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? N3 C6 1.489(7) . ? N3 C5 1.498(7) . ? N3 H31 0.9000 . ? N3 H32 0.9000 . ? C5 C6 1.501(8) 2_666 ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C5 1.501(8) 2_666 ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? N4 C7 1.493(7) . ? N4 C8 1.498(6) . ? N4 H41 0.9000 . ? N4 H42 0.9000 . ? C7 C8 1.497(7) 2_565 ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C7 1.497(7) 2_565 ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? N5 C9 1.474(7) . ? N5 C10 1.483(8) . ? N5 H51 0.9000 . ? N5 H52 0.9000 . ? C9 C10 1.518(7) 2_656 ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C9 1.518(7) 2_656 ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? N6 C12 1.486(7) . ? N6 C11 1.488(7) . ? N6 H61 0.9000 . ? N6 H62 0.9000 . ? C11 C12 1.513(7) 2_665 ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12 C11 1.513(7) 2_665 ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? N7 C14 1.480(7) 2_576 ? N7 C13 1.484(7) . ? N7 H71 0.9000 . ? N7 H72 0.9000 . ? C13 C14 1.510(8) . ? C13 H13A 0.9700 . ? C13 H13B 0.9700 . ? C14 N7 1.480(7) 2_576 ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? N8 C16 1.364(15) 2_655 ? N8 C15 1.502(11) . ? N8 H81 0.9000 . ? N8 H82 0.9000 . ? C15 C16 1.463(13) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C16 N8 1.364(15) 2_655 ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? O5A O5B 1.019(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 F6 V1 F3 91.72(14) . . ? F6 V1 F2 93.00(15) . . ? F3 V1 F2 89.41(15) . . ? F6 V1 F5 91.59(13) . . ? F3 V1 F5 176.68(14) . . ? F2 V1 F5 90.07(15) . . ? F6 V1 F1 176.83(14) . . ? F3 V1 F1 90.34(13) . . ? F2 V1 F1 89.43(14) . . ? F5 V1 F1 86.38(13) . . ? F6 V1 F4 88.71(13) . . ? F3 V1 F4 87.98(13) . . ? F2 V1 F4 176.92(14) . . ? F5 V1 F4 92.44(13) . . ? F1 V1 F4 88.95(13) . . ? O1 V2 F8 98.34(15) . . ? O1 V2 F4 102.17(15) . . ? F8 V2 F4 89.65(13) . . ? O1 V2 F7 96.44(15) . . ? F8 V2 F7 165.08(12) . . ? F4 V2 F7 89.26(13) . . ? O1 V2 F10 99.19(14) . . ? F8 V2 F10 86.15(12) . . ? F4 V2 F10 158.60(12) . . ? F7 V2 F10 89.46(12) . . ? O1 V2 F9 171.92(14) . . ? F8 V2 F9 82.81(11) . . ? F4 V2 F9 85.81(11) . . ? F7 V2 F9 82.27(11) . . ? F10 V2 F9 72.86(10) . . ? O2 V3 F11 95.57(15) . . ? O2 V3 F12 95.14(15) . . ? F11 V3 F12 169.22(13) . . ? O2 V3 F13 94.53(15) . . ? F11 V3 F13 89.46(13) . . ? F12 V3 F13 90.95(12) . . ? O2 V3 F9 100.88(15) . . ? F11 V3 F9 87.10(12) . . ? F12 V3 F9 89.65(12) . . ? F13 V3 F9 164.46(12) . . ? O2 V3 F10 176.05(15) . . ? F11 V3 F10 84.08(12) . . ? F12 V3 F10 85.15(11) . . ? F13 V3 F10 89.40(11) . . ? F9 V3 F10 75.18(11) . . ? F14 V4 F15 175.42(13) . . ? F14 V4 F16 90.56(12) . . ? F15 V4 F16 93.56(12) . . ? F14 V4 F1 88.78(13) . 1_455 ? F15 V4 F1 87.38(13) . 1_455 ? F16 V4 F1 172.83(12) . 1_455 ? F14 V4 F17 95.14(12) . . ? F15 V4 F17 87.56(12) . . ? F16 V4 F17 79.91(11) . . ? F1 V4 F17 93.04(12) 1_455 . ? F14 V4 F13 88.48(12) . . ? F15 V4 F13 89.25(12) . . ? F16 V4 F13 93.73(12) . . ? F1 V4 F13 93.38(12) 1_455 . ? F17 V4 F13 172.69(12) . . ? O3 V5 F19 104.73(18) . . ? O3 V5 F18 97.91(16) . . ? F19 V5 F18 90.93(14) . . ? O3 V5 F20 99.95(16) . . ? F19 V5 F20 88.81(14) . . ? F18 V5 F20 161.60(13) . . ? O3 V5 F17 97.34(16) . . ? F19 V5 F17 157.93(14) . . ? F18 V5 F17 86.46(12) . . ? F20 V5 F17 86.90(12) . . ? O3 V5 F16 168.87(16) . . ? F19 V5 F16 86.39(13) . . ? F18 V5 F16 81.04(11) . . ? F20 V5 F16 80.58(11) . . ? F17 V5 F16 71.56(10) . . ? V4 F1 V1 160.47(18) 1_655 . ? V2 F4 V1 160.54(17) . . ? V3 F9 V2 103.76(12) . . ? V2 F10 V3 108.15(12) . . ? V3 F13 V4 145.77(16) . . ? V4 F16 V5 101.25(12) . . ? V4 F17 V5 107.15(12) . . ? C2 N1 C1 112.2(4) . . ? C2 N1 H11 109.2 . . ? C1 N1 H11 109.2 . . ? C2 N1 H12 109.2 . . ? C1 N1 H12 109.2 . . ? H11 N1 H12 107.9 . . ? N1 C1 C2 109.8(4) . 2_757 ? N1 C1 H1C 109.7 . . ? C2 C1 H1C 109.7 2_757 . ? N1 C1 H1D 109.7 . . ? C2 C1 H1D 109.7 2_757 . ? H1C C1 H1D 108.2 . . ? N1 C2 C1 110.5(4) . 2_757 ? N1 C2 H2A 109.6 . . ? C1 C2 H2A 109.6 2_757 . ? N1 C2 H2B 109.6 . . ? C1 C2 H2B 109.6 2_757 . ? H2A C2 H2B 108.1 . . ? C3 N2 C4 111.0(4) . . ? C3 N2 H21 109.4 . . ? C4 N2 H21 109.4 . . ? C3 N2 H22 109.4 . . ? C4 N2 H22 109.4 . . ? H21 N2 H22 108.0 . . ? N2 C3 C4 111.4(4) . 2_766 ? N2 C3 H3A 109.4 . . ? C4 C3 H3A 109.4 2_766 . ? N2 C3 H3B 109.4 . . ? C4 C3 H3B 109.4 2_766 . ? H3A C3 H3B 108.0 . . ? N2 C4 C3 110.0(4) . 2_766 ? N2 C4 H4A 109.7 . . ? C3 C4 H4A 109.7 2_766 . ? N2 C4 H4B 109.7 . . ? C3 C4 H4B 109.7 2_766 . ? H4A C4 H4B 108.2 . . ? C6 N3 C5 110.7(4) . . ? C6 N3 H31 109.5 . . ? C5 N3 H31 109.5 . . ? C6 N3 H32 109.5 . . ? C5 N3 H32 109.5 . . ? H31 N3 H32 108.1 . . ? N3 C5 C6 110.8(4) . 2_666 ? N3 C5 H5A 109.5 . . ? C6 C5 H5A 109.5 2_666 . ? N3 C5 H5B 109.5 . . ? C6 C5 H5B 109.5 2_666 . ? H5A C5 H5B 108.1 . . ? N3 C6 C5 111.3(4) . 2_666 ? N3 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 2_666 . ? N3 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 2_666 . ? H6A C6 H6B 108.0 . . ? C7 N4 C8 110.5(4) . . ? C7 N4 H41 109.6 . . ? C8 N4 H41 109.6 . . ? C7 N4 H42 109.6 . . ? C8 N4 H42 109.6 . . ? H41 N4 H42 108.1 . . ? N4 C7 C8 110.7(4) . 2_565 ? N4 C7 H7A 109.5 . . ? C8 C7 H7A 109.5 2_565 . ? N4 C7 H7B 109.5 . . ? C8 C7 H7B 109.5 2_565 . ? H7A C7 H7B 108.1 . . ? C7 C8 N4 109.7(4) 2_565 . ? C7 C8 H8A 109.7 2_565 . ? N4 C8 H8A 109.7 . . ? C7 C8 H8B 109.7 2_565 . ? N4 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C9 N5 C10 111.1(4) . . ? C9 N5 H51 109.4 . . ? C10 N5 H51 109.4 . . ? C9 N5 H52 109.4 . . ? C10 N5 H52 109.4 . . ? H51 N5 H52 108.0 . . ? N5 C9 C10 110.8(5) . 2_656 ? N5 C9 H9A 109.5 . . ? C10 C9 H9A 109.5 2_656 . ? N5 C9 H9B 109.5 . . ? C10 C9 H9B 109.5 2_656 . ? H9A C9 H9B 108.1 . . ? N5 C10 C9 110.3(5) . 2_656 ? N5 C10 H10A 109.6 . . ? C9 C10 H10A 109.6 2_656 . ? N5 C10 H10B 109.6 . . ? C9 C10 H10B 109.6 2_656 . ? H10A C10 H10B 108.1 . . ? C12 N6 C11 111.5(4) . . ? C12 N6 H61 109.3 . . ? C11 N6 H61 109.3 . . ? C12 N6 H62 109.3 . . ? C11 N6 H62 109.3 . . ? H61 N6 H62 108.0 . . ? N6 C11 C12 109.8(5) . 2_665 ? N6 C11 H11A 109.7 . . ? C12 C11 H11A 109.7 2_665 . ? N6 C11 H11B 109.7 . . ? C12 C11 H11B 109.7 2_665 . ? H11A C11 H11B 108.2 . . ? N6 C12 C11 110.1(4) . 2_665 ? N6 C12 H12A 109.6 . . ? C11 C12 H12A 109.6 2_665 . ? N6 C12 H12B 109.6 . . ? C11 C12 H12B 109.6 2_665 . ? H12A C12 H12B 108.2 . . ? C14 N7 C13 112.5(4) 2_576 . ? C14 N7 H71 109.1 2_576 . ? C13 N7 H71 109.1 . . ? C14 N7 H72 109.1 2_576 . ? C13 N7 H72 109.1 . . ? H71 N7 H72 107.8 . . ? N7 C13 C14 109.1(4) . . ? N7 C13 H13A 109.9 . . ? C14 C13 H13A 109.9 . . ? N7 C13 H13B 109.9 . . ? C14 C13 H13B 109.9 . . ? H13A C13 H13B 108.3 . . ? N7 C14 C13 109.3(4) 2_576 . ? N7 C14 H14A 109.8 2_576 . ? C13 C14 H14A 109.8 . . ? N7 C14 H14B 109.8 2_576 . ? C13 C14 H14B 109.8 . . ? H14A C14 H14B 108.3 . . ? C16 N8 C15 113.0(7) 2_655 . ? C16 N8 H81 109.0 2_655 . ? C15 N8 H81 109.0 . . ? C16 N8 H82 109.0 2_655 . ? C15 N8 H82 109.0 . . ? H81 N8 H82 107.8 . . ? C16 C15 N8 108.0(6) . . ? C16 C15 H15A 110.1 . . ? N8 C15 H15A 110.1 . . ? C16 C15 H15B 110.1 . . ? N8 C15 H15B 110.1 . . ? H15A C15 H15B 108.4 . . ? N8 C16 C15 112.6(8) 2_655 . ? N8 C16 H16A 109.1 2_655 . ? C15 C16 H16A 109.1 . . ? N8 C16 H16B 109.1 2_655 . ? C15 C16 H16B 109.1 . . ? H16A C16 H16B 107.8 . . ? 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 N4 H42 F11 0.90 2.05 2.786(5) 137.7 . N4 H42 F7 0.90 2.16 2.788(5) 126.5 . N4 H42 F10 0.90 2.30 2.927(5) 126.2 . N6 H62 F7 0.90 1.80 2.701(5) 175.3 . N7 H71 F8 0.90 1.92 2.654(5) 137.7 . N7 H72 F6 0.90 1.92 2.793(6) 164.2 . N1 H11 F5 0.90 1.83 2.718(5) 171.3 2_666 N1 H12 F9 0.90 2.11 2.802(5) 132.5 2_666 N1 H12 F7 0.90 2.19 2.743(5) 118.9 2_666 N3 H32 F3 0.90 1.81 2.677(5) 161.2 2_666 N5 H52 F2 0.90 1.92 2.754(6) 152.4 2_666 N2 H21 F14 0.90 2.11 2.883(5) 143.0 1_655 N2 H21 F16 0.90 2.25 2.994(5) 139.8 1_655 N2 H22 F8 0.90 2.07 2.891(5) 150.7 1_655 N2 H22 F10 0.90 2.34 2.904(5) 121.1 1_655 N2 H22 F12 0.90 2.37 2.992(5) 126.7 1_655 N3 H31 F18 0.90 1.74 2.626(5) 165.8 1_655 N4 H41 F20 0.90 1.77 2.626(5) 158.2 2_565 N6 H61 F15 0.90 1.88 2.735(5) 157.3 2_565 N8 H81 F13 0.90 2.12 2.879(7) 141.9 2_565 N5 H51 F12 0.90 1.79 2.674(5) 165.0 2_566 N8 H82 F2 0.90 2.16 2.745(8) 121.8 2_665 _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 33.11 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 2.063 _refine_diff_density_min -1.231 _refine_diff_density_rms 0.156 #===end data_IV _database_code_depnum_ccdc_archive 'CCDC 650395' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C4 H12 N2, F4 H2 O2 V' _chemical_formula_sum 'C4 H14 F4 N2 O2 V' _chemical_formula_weight 249.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source V V 0.3005 0.5294 '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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' H H 0.0000 0.0000 '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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 5.7184(8) _cell_length_b 8.2456(12) _cell_length_c 9.8105(14) _cell_angle_alpha 97.444(3) _cell_angle_beta 101.073(3) _cell_angle_gamma 104.340(3) _cell_volume 432.13(11) _cell_formula_units_Z 2 _cell_measurement_temperature 125(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description platelet _exptl_crystal_colour blue _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.250 _exptl_crystal_size_min 0.050 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.914 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 254 _exptl_absorpt_coefficient_mu 1.187 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.689 _exptl_absorpt_correction_T_max 0.940 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 125(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Rotating Anode' _diffrn_radiation_monochromator 'Confocal Optics' _diffrn_measurement_device_type 'CCD Area Detector' _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4505 _diffrn_reflns_av_R_equivalents 0.0595 _diffrn_reflns_av_sigmaI/netI 0.0706 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 7 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 27.04 _reflns_number_total 1970 _reflns_number_gt 1790 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Crystalclear (Rigaku Corp., 2004)' _computing_cell_refinement 'Crystalclear (Rigaku Corp., 2004)' _computing_data_reduction 'Crystalclear (Rigaku Corp., 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger.In this structure solution, two distance restraints have been used. These were both 0.85 Angstroms and were used to restrain two hydrogen atoms attached to an oxygen atom, as a water molecules. ; _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^)+(0.0476P)^2^+0.0921P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1970 _refine_ls_number_parameters 126 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0493 _refine_ls_R_factor_gt 0.0446 _refine_ls_wR_factor_ref 0.1128 _refine_ls_wR_factor_gt 0.1107 _refine_ls_goodness_of_fit_ref 1.111 _refine_ls_restrained_S_all 1.110 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.45170(7) 0.23035(5) 0.75325(4) 0.00782(16) Uani 1 1 d . . . F1 F 0.2806(3) 0.03663(18) 0.59744(15) 0.0145(3) Uani 1 1 d . . . F2 F 0.3942(3) 0.38120(18) 0.62337(15) 0.0134(3) Uani 1 1 d . . . F3 F 0.7134(3) 0.41656(17) 0.87188(15) 0.0130(3) Uani 1 1 d . . . F4 F 0.6029(3) 0.08641(17) 0.85774(15) 0.0132(3) Uani 1 1 d . . . O2 O 0.7675(4) 0.2145(2) 0.6333(2) 0.0147(4) Uani 1 1 d D . . O1 O 0.2200(3) 0.2308(2) 0.8256(2) 0.0156(4) Uani 1 1 d . . . N1 N 1.0405(4) 0.7215(2) 0.9114(2) 0.0090(4) Uani 1 1 d . . . H1A H 0.9360 0.6200 0.9112 0.011 Uiso 1 1 calc R . . H1B H 1.1294 0.7649 1.0006 0.011 Uiso 1 1 calc R . . N2 N 0.9263(4) 0.7528(2) 0.6171(2) 0.0100(4) Uani 1 1 d . . . H2A H 0.8390 0.7116 0.5273 0.012 Uiso 1 1 calc R . . H2B H 1.0315 0.8550 0.6196 0.012 Uiso 1 1 calc R . . C1 C 0.8946(5) 0.8384(3) 0.8626(3) 0.0111(5) Uani 1 1 d . . . H1C H 1.0059 0.9511 0.8715 0.013 Uiso 1 1 calc R . . H1D H 0.7791 0.8473 0.9219 0.013 Uiso 1 1 calc R . . C2 C 0.7527(5) 0.7736(3) 0.7103(3) 0.0107(5) Uani 1 1 d . . . H2C H 0.6320 0.6650 0.7026 0.013 Uiso 1 1 calc R . . H2D H 0.6638 0.8534 0.6795 0.013 Uiso 1 1 calc R . . C3 C 1.0702(5) 0.6342(3) 0.6648(3) 0.0119(5) Uani 1 1 d . . . H3A H 1.1856 0.6251 0.6054 0.014 Uiso 1 1 calc R . . H3B H 0.9576 0.5218 0.6551 0.014 Uiso 1 1 calc R . . C4 C 1.2127(5) 0.6969(3) 0.8178(3) 0.0111(5) Uani 1 1 d . . . H4A H 1.2974 0.6148 0.8481 0.013 Uiso 1 1 calc R . . H4B H 1.3370 0.8040 0.8258 0.013 Uiso 1 1 calc R . . H1 H 0.891(5) 0.209(6) 0.695(4) 0.070(15) Uiso 1 1 d D . . H2 H 0.737(7) 0.129(3) 0.568(3) 0.034(10) Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0068(2) 0.0072(2) 0.0079(2) 0.00088(16) 0.00083(17) 0.00000(17) F1 0.0137(8) 0.0124(7) 0.0128(7) -0.0006(6) 0.0013(6) -0.0019(6) F2 0.0153(8) 0.0106(7) 0.0113(7) 0.0028(5) -0.0009(6) 0.0013(6) F3 0.0131(8) 0.0085(7) 0.0121(7) -0.0007(5) -0.0006(6) -0.0023(6) F4 0.0150(8) 0.0103(7) 0.0124(7) 0.0031(6) -0.0007(6) 0.0025(6) O2 0.0122(9) 0.0140(9) 0.0150(10) -0.0008(8) 0.0032(8) 0.0004(8) O1 0.0136(9) 0.0167(9) 0.0164(10) 0.0028(7) 0.0057(8) 0.0027(8) N1 0.0092(10) 0.0081(9) 0.0078(10) 0.0010(8) 0.0005(8) 0.0003(8) N2 0.0099(10) 0.0085(9) 0.0088(10) 0.0002(8) 0.0015(8) -0.0015(8) C1 0.0124(12) 0.0095(11) 0.0110(12) 0.0013(9) 0.0036(10) 0.0022(10) C2 0.0099(12) 0.0112(11) 0.0114(12) 0.0015(9) 0.0037(10) 0.0028(10) C3 0.0119(12) 0.0106(11) 0.0118(12) -0.0005(9) 0.0027(10) 0.0020(10) C4 0.0097(12) 0.0130(12) 0.0110(12) 0.0030(9) 0.0022(10) 0.0033(10) _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 O1 1.6197(19) . ? V1 F3 1.9186(14) . ? V1 F4 1.9209(14) . ? V1 F2 1.9316(14) . ? V1 F1 1.9657(15) . ? V1 O2 2.357(2) . ? O2 H1 0.85(4) . ? O2 H2 0.85(3) . ? N1 C1 1.489(3) . ? N1 C4 1.500(3) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N2 C3 1.491(3) . ? N2 C2 1.497(3) . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? C1 C2 1.514(3) . ? C1 H1C 0.9700 . ? C1 H1D 0.9700 . ? C2 H2C 0.9700 . ? C2 H2D 0.9700 . ? C3 C4 1.518(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? 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 O1 V1 F3 102.99(8) . . ? O1 V1 F4 100.38(8) . . ? F3 V1 F4 85.91(6) . . ? O1 V1 F2 98.26(8) . . ? F3 V1 F2 88.38(6) . . ? F4 V1 F2 161.29(7) . . ? O1 V1 F1 97.68(8) . . ? F3 V1 F1 159.33(7) . . ? F4 V1 F1 90.59(6) . . ? F2 V1 F1 88.48(6) . . ? O1 V1 O2 175.62(8) . . ? F3 V1 O2 81.33(7) . . ? F4 V1 O2 80.52(7) . . ? F2 V1 O2 81.01(7) . . ? F1 V1 O2 78.00(7) . . ? V1 O2 H1 106(3) . . ? V1 O2 H2 117(3) . . ? H1 O2 H2 106(4) . . ? C1 N1 C4 111.24(18) . . ? C1 N1 H1A 109.4 . . ? C4 N1 H1A 109.4 . . ? C1 N1 H1B 109.4 . . ? C4 N1 H1B 109.4 . . ? H1A N1 H1B 108.0 . . ? C3 N2 C2 110.52(19) . . ? C3 N2 H2A 109.5 . . ? C2 N2 H2A 109.5 . . ? C3 N2 H2B 109.5 . . ? C2 N2 H2B 109.5 . . ? H2A N2 H2B 108.1 . . ? N1 C1 C2 110.8(2) . . ? N1 C1 H1C 109.5 . . ? C2 C1 H1C 109.5 . . ? N1 C1 H1D 109.5 . . ? C2 C1 H1D 109.5 . . ? H1C C1 H1D 108.1 . . ? N2 C2 C1 110.5(2) . . ? N2 C2 H2C 109.5 . . ? C1 C2 H2C 109.5 . . ? N2 C2 H2D 109.5 . . ? C1 C2 H2D 109.5 . . ? H2C C2 H2D 108.1 . . ? N2 C3 C4 110.9(2) . . ? N2 C3 H3A 109.5 . . ? C4 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? N1 C4 C3 110.7(2) . . ? N1 C4 H4A 109.5 . . ? C3 C4 H4A 109.5 . . ? N1 C4 H4B 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 108.1 . . ? 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 N1 H1A F3 0.90 1.78 2.667(2) 167.9 . N1 H1B F4 0.90 1.89 2.738(3) 155.1 2_767 N1 H1B F3 0.90 2.31 2.841(2) 117.6 2_767 N2 H2A F2 0.90 1.73 2.609(3) 164.6 2_666 N2 H2B F1 0.90 1.86 2.746(2) 166.7 1_665 O2 H1 O1 0.85(4) 2.02(3) 2.856(3) 169(4) 1_655 O2 H2 F1 0.85(3) 1.95(3) 2.784(2) 168(4) 2_656 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.04 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.596 _refine_diff_density_min -0.646 _refine_diff_density_rms 0.128 #===end