# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Eric McInnes' _publ_contact_author_email ERIC.MCINNES@MANCHESTER.AC.UK _publ_section_title ; Tri, tetra- and octa-metallic vanadium(III) clusters from new, simple starting materials: interplay of exchange and anisotropy effects ; loop_ _publ_author_name 'Eric McInnes' 'Luke J. Batchelor' 'Andrea Caneschi' 'Rebecca Laye' 'Emma Scales' 'Jurgen Schnack' ; L.Sorace ; 'Ian S. Tidmarsh' # Attachment '1.cif' data_oejlmprofp21c _database_code_depnum_ccdc_archive 'CCDC 736080' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[VCl3(bipy)(MeCN)]' _chemical_formula_sum 'C12 H11 Cl3 N3 V' _chemical_formula_weight 354.53 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 8.1267(4) _cell_length_b 6.6923(3) _cell_length_c 25.9029(10) _cell_angle_alpha 90.00 _cell_angle_beta 92.583(4) _cell_angle_gamma 90.00 _cell_volume 1407.33(11) _cell_formula_units_Z 4 _cell_measurement_temperature 373(2) _cell_measurement_reflns_used 1563 _cell_measurement_theta_min 2.6576 _cell_measurement_theta_max 31.8766 _exptl_crystal_description needle _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.673 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 712 _exptl_absorpt_coefficient_mu 1.261 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.5712 _exptl_absorpt_correction_T_max 0.5712 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcaliber 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13877 _diffrn_reflns_av_R_equivalents 0.0341 _diffrn_reflns_av_sigmaI/netI 0.0504 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 30.51 _reflns_number_total 4295 _reflns_number_gt 3201 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) ; _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 ; The structure was solved by direct methods. Data processing was carried out to 0.70 angstroms as the data was only complete to this resolution. Hydrogen atoms were included in calculated positions. 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^)+(0.0533P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4295 _refine_ls_number_parameters 173 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0547 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.1013 _refine_ls_wR_factor_gt 0.0729 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _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 1.13859(5) 0.71205(6) 0.138969(15) 0.00803(10) Uani 1 1 d . . . Cl1 Cl 1.03377(7) 0.87414(9) 0.20914(2) 0.01433(13) Uani 1 1 d . . . Cl2 Cl 1.37033(7) 0.91549(9) 0.13647(2) 0.01381(13) Uani 1 1 d . . . Cl3 Cl 1.21809(7) 0.52094(8) 0.06870(2) 0.01056(12) Uani 1 1 d . . . N1 N 0.9168(2) 0.5424(3) 0.13469(7) 0.0087(4) Uani 1 1 d . . . N2 N 0.9824(2) 0.8884(3) 0.09017(7) 0.0084(4) Uani 1 1 d . . . N3 N 1.2586(2) 0.5041(3) 0.18998(8) 0.0118(4) Uani 1 1 d . . . C1 C 0.7928(3) 0.6225(3) 0.10453(9) 0.0096(4) Uani 1 1 d . . . C2 C 0.6400(3) 0.5292(4) 0.09966(10) 0.0138(5) Uani 1 1 d . . . H2 H 0.5556 0.5851 0.0790 0.017 Uiso 1 1 calc R . . C3 C 0.6145(3) 0.3520(4) 0.12593(10) 0.0142(5) Uani 1 1 d . . . H3 H 0.5129 0.2881 0.1231 0.017 Uiso 1 1 calc R . . C4 C 0.7413(3) 0.2716(3) 0.15629(10) 0.0133(5) Uani 1 1 d . . . H4 H 0.7265 0.1531 0.1742 0.016 Uiso 1 1 calc R . . C5 C 0.8916(3) 0.3703(3) 0.15965(9) 0.0109(4) Uani 1 1 d . . . H5 H 0.9775 0.3153 0.1799 0.013 Uiso 1 1 calc R . . C6 C 0.8305(3) 0.8131(3) 0.07894(9) 0.0099(4) Uani 1 1 d . . . C7 C 0.7187(3) 0.9120(4) 0.04606(10) 0.0143(5) Uani 1 1 d . . . H7 H 0.6155 0.8570 0.0382 0.017 Uiso 1 1 calc R . . C8 C 0.7620(3) 1.0925(4) 0.02510(10) 0.0141(5) Uani 1 1 d . . . H8 H 0.6891 1.1602 0.0026 0.017 Uiso 1 1 calc R . . C9 C 0.9146(3) 1.1713(3) 0.03794(9) 0.0113(5) Uani 1 1 d . . . H9 H 0.9453 1.2945 0.0248 0.014 Uiso 1 1 calc R . . C10 C 1.0218(3) 1.0652(3) 0.07055(9) 0.0095(4) Uani 1 1 d . . . H10 H 1.1250 1.1191 0.0791 0.011 Uiso 1 1 calc R . . C11 C 1.3053(3) 0.3817(4) 0.21726(9) 0.0123(5) Uani 1 1 d . . . C12 C 1.3651(3) 0.2255(4) 0.25225(10) 0.0180(5) Uani 1 1 d . . . H12A H 1.4687 0.2652 0.2683 0.027 Uiso 1 1 calc R . . H12B H 1.3794 0.1041 0.2332 0.027 Uiso 1 1 calc R . . H12C H 1.2867 0.2039 0.2783 0.027 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.00810(18) 0.00695(17) 0.00892(19) 0.00088(14) -0.00068(13) -0.00123(14) Cl1 0.0181(3) 0.0142(3) 0.0108(3) -0.0021(2) 0.0015(2) 0.0002(2) Cl2 0.0111(3) 0.0112(2) 0.0189(3) 0.0010(2) -0.0016(2) -0.0043(2) Cl3 0.0101(2) 0.0096(2) 0.0120(3) -0.0006(2) 0.00066(19) -0.0006(2) N1 0.0084(9) 0.0089(9) 0.0091(9) -0.0008(7) 0.0018(7) -0.0004(7) N2 0.0094(9) 0.0074(8) 0.0085(9) -0.0011(7) 0.0007(7) -0.0007(7) N3 0.0095(9) 0.0136(9) 0.0121(10) 0.0002(8) -0.0004(7) -0.0013(8) C1 0.0074(10) 0.0092(10) 0.0121(11) -0.0010(8) 0.0007(8) -0.0004(8) C2 0.0084(10) 0.0140(11) 0.0189(13) -0.0002(9) 0.0001(9) -0.0003(9) C3 0.0102(11) 0.0119(10) 0.0207(13) -0.0017(10) 0.0051(9) -0.0043(9) C4 0.0147(11) 0.0091(10) 0.0164(12) 0.0011(9) 0.0052(9) -0.0017(9) C5 0.0122(11) 0.0097(10) 0.0109(11) 0.0006(9) 0.0013(8) -0.0005(8) C6 0.0086(10) 0.0095(10) 0.0117(11) -0.0001(8) 0.0015(8) -0.0007(8) C7 0.0103(11) 0.0144(11) 0.0178(13) 0.0026(10) -0.0042(9) -0.0016(9) C8 0.0139(11) 0.0130(11) 0.0150(12) 0.0032(9) -0.0019(9) 0.0030(9) C9 0.0147(11) 0.0086(10) 0.0107(11) 0.0009(8) 0.0016(9) 0.0005(9) C10 0.0105(10) 0.0086(10) 0.0093(11) -0.0007(8) 0.0003(8) -0.0013(8) C11 0.0108(11) 0.0131(11) 0.0129(12) -0.0016(9) -0.0001(9) -0.0015(9) C12 0.0209(13) 0.0154(12) 0.0173(13) 0.0042(10) -0.0040(10) 0.0042(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 N2 2.1113(19) . ? V1 N3 2.126(2) . ? V1 N1 2.1287(19) . ? V1 Cl1 2.3120(7) . ? V1 Cl2 2.3271(7) . ? V1 Cl3 2.3394(7) . ? N1 C5 1.341(3) . ? N1 C1 1.358(3) . ? N2 C10 1.333(3) . ? N2 C6 1.353(3) . ? N3 C11 1.136(3) . ? C1 C2 1.390(3) . ? C1 C6 1.476(3) . ? C2 C3 1.387(3) . ? C3 C4 1.377(4) . ? C4 C5 1.387(3) . ? C6 C7 1.385(3) . ? C7 C8 1.377(3) . ? C8 C9 1.374(3) . ? C9 C10 1.382(3) . ? C11 C12 1.453(3) . ? 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 N2 V1 N3 170.02(8) . . ? N2 V1 N1 77.43(7) . . ? N3 V1 N1 92.68(7) . . ? N2 V1 Cl1 88.60(5) . . ? N3 V1 Cl1 89.63(6) . . ? N1 V1 Cl1 87.14(5) . . ? N2 V1 Cl2 96.99(5) . . ? N3 V1 Cl2 92.93(6) . . ? N1 V1 Cl2 174.22(6) . . ? Cl1 V1 Cl2 94.29(3) . . ? N2 V1 Cl3 91.11(5) . . ? N3 V1 Cl3 89.46(6) . . ? N1 V1 Cl3 86.03(5) . . ? Cl1 V1 Cl3 173.06(3) . . ? Cl2 V1 Cl3 92.63(2) . . ? C5 N1 C1 119.4(2) . . ? C5 N1 V1 125.50(16) . . ? C1 N1 V1 115.11(15) . . ? C10 N2 C6 118.78(19) . . ? C10 N2 V1 125.20(15) . . ? C6 N2 V1 116.02(15) . . ? C11 N3 V1 171.91(19) . . ? N1 C1 C2 120.8(2) . . ? N1 C1 C6 115.84(19) . . ? C2 C1 C6 123.4(2) . . ? C3 C2 C1 119.5(2) . . ? C4 C3 C2 119.3(2) . . ? C3 C4 C5 118.9(2) . . ? N1 C5 C4 122.1(2) . . ? N2 C6 C7 121.4(2) . . ? N2 C6 C1 115.5(2) . . ? C7 C6 C1 123.1(2) . . ? C8 C7 C6 119.3(2) . . ? C9 C8 C7 119.0(2) . . ? C8 C9 C10 119.2(2) . . ? N2 C10 C9 122.2(2) . . ? N3 C11 C12 179.9(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 V1 N1 C5 -178.0(2) . . . . ? N3 V1 N1 C5 0.7(2) . . . . ? Cl1 V1 N1 C5 -88.81(18) . . . . ? Cl2 V1 N1 C5 166.7(5) . . . . ? Cl3 V1 N1 C5 89.96(18) . . . . ? N2 V1 N1 C1 0.67(16) . . . . ? N3 V1 N1 C1 179.37(16) . . . . ? Cl1 V1 N1 C1 89.88(16) . . . . ? Cl2 V1 N1 C1 -14.6(7) . . . . ? Cl3 V1 N1 C1 -91.36(16) . . . . ? N3 V1 N2 C10 169.9(4) . . . . ? N1 V1 N2 C10 177.4(2) . . . . ? Cl1 V1 N2 C10 90.05(18) . . . . ? Cl2 V1 N2 C10 -4.09(19) . . . . ? Cl3 V1 N2 C10 -96.88(18) . . . . ? N3 V1 N2 C6 -9.5(5) . . . . ? N1 V1 N2 C6 -1.94(16) . . . . ? Cl1 V1 N2 C6 -89.33(16) . . . . ? Cl2 V1 N2 C6 176.52(15) . . . . ? Cl3 V1 N2 C6 83.73(16) . . . . ? N2 V1 N3 C11 2.2(18) . . . . ? N1 V1 N3 C11 -5.2(15) . . . . ? Cl1 V1 N3 C11 81.9(15) . . . . ? Cl2 V1 N3 C11 176.2(15) . . . . ? Cl3 V1 N3 C11 -91.2(15) . . . . ? C5 N1 C1 C2 0.6(3) . . . . ? V1 N1 C1 C2 -178.18(18) . . . . ? C5 N1 C1 C6 179.3(2) . . . . ? V1 N1 C1 C6 0.6(3) . . . . ? N1 C1 C2 C3 -0.1(4) . . . . ? C6 C1 C2 C3 -178.7(2) . . . . ? C1 C2 C3 C4 -0.1(4) . . . . ? C2 C3 C4 C5 -0.1(4) . . . . ? C1 N1 C5 C4 -0.9(3) . . . . ? V1 N1 C5 C4 177.74(17) . . . . ? C3 C4 C5 N1 0.7(4) . . . . ? C10 N2 C6 C7 2.6(3) . . . . ? V1 N2 C6 C7 -177.98(18) . . . . ? C10 N2 C6 C1 -176.6(2) . . . . ? V1 N2 C6 C1 2.8(3) . . . . ? N1 C1 C6 N2 -2.3(3) . . . . ? C2 C1 C6 N2 176.5(2) . . . . ? N1 C1 C6 C7 178.6(2) . . . . ? C2 C1 C6 C7 -2.7(4) . . . . ? N2 C6 C7 C8 -1.2(4) . . . . ? C1 C6 C7 C8 177.9(2) . . . . ? C6 C7 C8 C9 -0.9(4) . . . . ? C7 C8 C9 C10 1.5(4) . . . . ? C6 N2 C10 C9 -1.9(3) . . . . ? V1 N2 C10 C9 178.69(17) . . . . ? C8 C9 C10 N2 -0.1(4) . . . . ? V1 N3 C11 C12 -106(100) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.893 _refine_diff_density_min -0.789 _refine_diff_density_rms 0.262 # Attachment '2.cif' data_oejlm248sadp21c _database_code_depnum_ccdc_archive 'CCDC 736081' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[VCl3(phen)(MeCN)]' _chemical_formula_sum 'C14 H11 Cl3 N3 V' _chemical_formula_weight 378.55 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 7.1643(3) _cell_length_b 13.6669(6) _cell_length_c 15.3407(7) _cell_angle_alpha 90.00 _cell_angle_beta 101.388(4) _cell_angle_gamma 90.00 _cell_volume 1472.49(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 10627 _cell_measurement_theta_min 2.8945 _cell_measurement_theta_max 31.6634 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.37 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.708 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 760 _exptl_absorpt_coefficient_mu 1.212 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5825 _exptl_absorpt_correction_T_max 0.5825 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcaliber 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10981 _diffrn_reflns_av_R_equivalents 0.0171 _diffrn_reflns_av_sigmaI/netI 0.0117 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.75 _diffrn_reflns_theta_max 26.37 _reflns_number_total 2970 _reflns_number_gt 2758 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) ; _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 ; The structure was solved by direct methods. Data processing was carried out to 0.80 angstroms as the data was only complete to this resolution. Hydrogen atoms were included in calculated positions. 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^)+(0.0295P)^2^+0.7440P] 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 2970 _refine_ls_number_parameters 191 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0219 _refine_ls_R_factor_gt 0.0198 _refine_ls_wR_factor_ref 0.0519 _refine_ls_wR_factor_gt 0.0511 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.35195(3) 0.750094(14) 0.138246(13) 0.00899(7) Uani 1 1 d . . . Cl1 Cl 0.04709(4) 0.70332(2) 0.06198(2) 0.01254(8) Uani 1 1 d . . . Cl2 Cl 0.37833(4) 0.61555(2) 0.22998(2) 0.01426(8) Uani 1 1 d . . . Cl3 Cl 0.64513(4) 0.81608(2) 0.19904(2) 0.01276(8) Uani 1 1 d . . . N1 N 0.29798(15) 0.88132(8) 0.06035(7) 0.0099(2) Uani 1 1 d . . . N2 N 0.23093(15) 0.84252(8) 0.22275(7) 0.0104(2) Uani 1 1 d . . . N3 N 0.47822(16) 0.67689(8) 0.04129(7) 0.0136(2) Uani 1 1 d . . . C1 C 0.23764(17) 0.95694(9) 0.10596(8) 0.0100(2) Uani 1 1 d . . . C2 C 0.20443(18) 1.05157(9) 0.07000(8) 0.0109(2) Uani 1 1 d . . . C3 C 0.22852(18) 1.06557(10) -0.01817(9) 0.0127(3) Uani 1 1 d . . . H3 H 0.2074 1.1268 -0.0448 0.015 Uiso 1 1 calc R . . C4 C 0.28319(18) 0.98854(10) -0.06442(8) 0.0124(3) Uani 1 1 d . . . H4 H 0.2964 0.9965 -0.1231 0.015 Uiso 1 1 calc R . . C5 C 0.31905(18) 0.89760(9) -0.02233(8) 0.0115(2) Uani 1 1 d . . . H5 H 0.3595 0.8463 -0.0539 0.014 Uiso 1 1 calc R . . C6 C 0.20215(17) 0.93624(9) 0.19253(8) 0.0102(2) Uani 1 1 d . . . C7 C 0.13673(18) 1.01079(9) 0.24191(9) 0.0117(2) Uani 1 1 d . . . C8 C 0.09552(19) 0.98543(10) 0.32481(9) 0.0146(3) Uani 1 1 d . . . H8 H 0.0507 1.0324 0.3594 0.018 Uiso 1 1 calc R . . C9 C 0.12204(19) 0.89073(10) 0.35431(9) 0.0151(3) Uani 1 1 d . . . H9 H 0.0947 0.8729 0.4089 0.018 Uiso 1 1 calc R . . C10 C 0.19078(18) 0.82119(10) 0.30133(8) 0.0125(3) Uani 1 1 d . . . H10 H 0.2090 0.7573 0.3222 0.015 Uiso 1 1 calc R . . C11 C 0.14589(18) 1.12715(10) 0.12362(9) 0.0133(3) Uani 1 1 d . . . H11 H 0.1296 1.1906 0.1014 0.016 Uiso 1 1 calc R . . C12 C 0.11392(18) 1.10782(9) 0.20596(9) 0.0130(3) Uani 1 1 d . . . H12 H 0.0767 1.1581 0.2396 0.016 Uiso 1 1 calc R . . C13 C 0.54988(19) 0.63894(10) -0.00960(9) 0.0141(3) Uani 1 1 d . . . C14 C 0.6389(2) 0.58972(11) -0.07499(9) 0.0203(3) Uani 1 1 d . . . H14A H 0.7639 0.5680 -0.0471 0.031 Uiso 1 1 calc R . . H14B H 0.6486 0.6343 -0.1222 0.031 Uiso 1 1 calc R . . H14C H 0.5631 0.5344 -0.0987 0.031 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.01073(12) 0.00842(12) 0.00818(12) 0.00073(7) 0.00272(9) 0.00036(7) Cl1 0.01309(16) 0.01314(15) 0.01115(15) -0.00004(11) 0.00182(11) -0.00164(11) Cl2 0.01681(16) 0.01169(15) 0.01464(16) 0.00422(11) 0.00402(12) 0.00111(11) Cl3 0.01188(15) 0.01375(15) 0.01248(15) 0.00162(11) 0.00203(11) -0.00083(11) N1 0.0092(5) 0.0107(5) 0.0097(5) 0.0001(4) 0.0013(4) -0.0010(4) N2 0.0095(5) 0.0116(5) 0.0100(5) 0.0001(4) 0.0014(4) -0.0005(4) N3 0.0152(6) 0.0139(5) 0.0119(5) -0.0003(4) 0.0034(4) 0.0006(4) C1 0.0069(6) 0.0114(6) 0.0111(6) -0.0002(5) 0.0006(4) -0.0012(4) C2 0.0079(6) 0.0115(6) 0.0128(6) 0.0003(5) 0.0007(5) -0.0022(4) C3 0.0096(6) 0.0132(6) 0.0142(6) 0.0045(5) -0.0002(5) -0.0021(5) C4 0.0095(6) 0.0178(6) 0.0095(6) 0.0023(5) 0.0009(5) -0.0028(5) C5 0.0095(6) 0.0137(6) 0.0114(6) -0.0020(5) 0.0022(5) -0.0020(5) C6 0.0081(6) 0.0118(6) 0.0102(6) -0.0001(5) 0.0005(4) -0.0011(4) C7 0.0083(6) 0.0143(6) 0.0118(6) -0.0018(5) 0.0002(5) -0.0004(5) C8 0.0117(6) 0.0188(7) 0.0133(6) -0.0042(5) 0.0027(5) 0.0019(5) C9 0.0145(6) 0.0218(7) 0.0099(6) 0.0004(5) 0.0046(5) 0.0004(5) C10 0.0128(6) 0.0133(6) 0.0113(6) 0.0027(5) 0.0020(5) 0.0001(5) C11 0.0109(6) 0.0095(6) 0.0182(7) 0.0014(5) 0.0002(5) -0.0005(4) C12 0.0109(6) 0.0117(6) 0.0157(6) -0.0038(5) 0.0009(5) 0.0007(5) C13 0.0141(6) 0.0136(6) 0.0141(6) 0.0007(5) 0.0014(5) -0.0020(5) C14 0.0199(7) 0.0251(7) 0.0181(7) -0.0057(6) 0.0088(6) 0.0012(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 N2 2.1147(11) . ? V1 N3 2.1361(11) . ? V1 N1 2.1475(11) . ? V1 Cl2 2.3005(4) . ? V1 Cl3 2.3068(4) . ? V1 Cl1 2.3534(4) . ? N1 C5 1.3254(17) . ? N1 C1 1.3653(16) . ? N2 C10 1.3258(16) . ? N2 C6 1.3640(17) . ? N3 C13 1.1404(18) . ? C1 C2 1.4078(18) . ? C1 C6 1.4288(17) . ? C2 C3 1.4100(18) . ? C2 C11 1.4338(18) . ? C3 C4 1.3692(19) . ? C3 H3 0.9300 . ? C4 C5 1.4008(18) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.4042(18) . ? C7 C8 1.4045(19) . ? C7 C12 1.4332(18) . ? C8 C9 1.372(2) . ? C8 H8 0.9300 . ? C9 C10 1.4016(19) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.3536(19) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.4555(19) . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? 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 N2 V1 N3 171.08(4) . . ? N2 V1 N1 77.98(4) . . ? N3 V1 N1 93.33(4) . . ? N2 V1 Cl2 95.54(3) . . ? N3 V1 Cl2 93.25(3) . . ? N1 V1 Cl2 172.74(3) . . ? N2 V1 Cl3 88.25(3) . . ? N3 V1 Cl3 89.29(3) . . ? N1 V1 Cl3 87.02(3) . . ? Cl2 V1 Cl3 96.137(14) . . ? N2 V1 Cl1 90.83(3) . . ? N3 V1 Cl1 90.33(3) . . ? N1 V1 Cl1 84.42(3) . . ? Cl2 V1 Cl1 92.469(13) . . ? Cl3 V1 Cl1 171.393(14) . . ? C5 N1 C1 118.09(11) . . ? C5 N1 V1 129.10(9) . . ? C1 N1 V1 112.79(8) . . ? C10 N2 C6 118.05(11) . . ? C10 N2 V1 127.95(9) . . ? C6 N2 V1 113.91(8) . . ? C13 N3 V1 178.27(11) . . ? N1 C1 C2 122.73(12) . . ? N1 C1 C6 117.32(11) . . ? C2 C1 C6 119.92(11) . . ? C1 C2 C3 117.22(12) . . ? C1 C2 C11 118.88(12) . . ? C3 C2 C11 123.90(12) . . ? C4 C3 C2 119.63(12) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 119.25(12) . . ? C3 C4 H4 120.4 . . ? C5 C4 H4 120.4 . . ? N1 C5 C4 123.01(12) . . ? N1 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? N2 C6 C7 122.82(12) . . ? N2 C6 C1 117.34(11) . . ? C7 C6 C1 119.83(12) . . ? C6 C7 C8 117.50(12) . . ? C6 C7 C12 119.25(12) . . ? C8 C7 C12 123.25(12) . . ? C9 C8 C7 119.42(12) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 C10 119.34(12) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? N2 C10 C9 122.85(12) . . ? N2 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? C12 C11 C2 121.15(12) . . ? C12 C11 H11 119.4 . . ? C2 C11 H11 119.4 . . ? C11 C12 C7 120.82(12) . . ? C11 C12 H12 119.6 . . ? C7 C12 H12 119.6 . . ? N3 C13 C14 179.21(15) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 V1 N1 C5 -174.68(12) . . . . ? N3 V1 N1 C5 7.37(11) . . . . ? Cl2 V1 N1 C5 -147.5(2) . . . . ? Cl3 V1 N1 C5 96.48(11) . . . . ? Cl1 V1 N1 C5 -82.64(11) . . . . ? N2 V1 N1 C1 6.82(8) . . . . ? N3 V1 N1 C1 -171.14(9) . . . . ? Cl2 V1 N1 C1 33.9(3) . . . . ? Cl3 V1 N1 C1 -82.02(8) . . . . ? Cl1 V1 N1 C1 98.86(8) . . . . ? N3 V1 N2 C10 -169.9(2) . . . . ? N1 V1 N2 C10 176.79(12) . . . . ? Cl2 V1 N2 C10 0.11(11) . . . . ? Cl3 V1 N2 C10 -95.89(11) . . . . ? Cl1 V1 N2 C10 92.67(11) . . . . ? N3 V1 N2 C6 6.3(3) . . . . ? N1 V1 N2 C6 -6.95(8) . . . . ? Cl2 V1 N2 C6 176.37(8) . . . . ? Cl3 V1 N2 C6 80.37(8) . . . . ? Cl1 V1 N2 C6 -91.07(8) . . . . ? N2 V1 N3 C13 71(4) . . . . ? N1 V1 N3 C13 84(4) . . . . ? Cl2 V1 N3 C13 -99(4) . . . . ? Cl3 V1 N3 C13 -3(4) . . . . ? Cl1 V1 N3 C13 168(4) . . . . ? C5 N1 C1 C2 -2.51(18) . . . . ? V1 N1 C1 C2 176.17(10) . . . . ? C5 N1 C1 C6 175.47(11) . . . . ? V1 N1 C1 C6 -5.85(14) . . . . ? N1 C1 C2 C3 2.54(18) . . . . ? C6 C1 C2 C3 -175.39(11) . . . . ? N1 C1 C2 C11 -178.42(11) . . . . ? C6 C1 C2 C11 3.65(18) . . . . ? C1 C2 C3 C4 -0.38(18) . . . . ? C11 C2 C3 C4 -179.37(12) . . . . ? C2 C3 C4 C5 -1.65(19) . . . . ? C1 N1 C5 C4 0.32(19) . . . . ? V1 N1 C5 C4 -178.11(9) . . . . ? C3 C4 C5 N1 1.75(19) . . . . ? C10 N2 C6 C7 1.59(18) . . . . ? V1 N2 C6 C7 -175.06(10) . . . . ? C10 N2 C6 C1 -177.15(11) . . . . ? V1 N2 C6 C1 6.20(14) . . . . ? N1 C1 C6 N2 -0.14(17) . . . . ? C2 C1 C6 N2 177.90(11) . . . . ? N1 C1 C6 C7 -178.92(11) . . . . ? C2 C1 C6 C7 -0.88(18) . . . . ? N2 C6 C7 C8 -1.65(19) . . . . ? C1 C6 C7 C8 177.06(11) . . . . ? N2 C6 C7 C12 178.76(11) . . . . ? C1 C6 C7 C12 -2.53(18) . . . . ? C6 C7 C8 C9 0.63(19) . . . . ? C12 C7 C8 C9 -179.80(13) . . . . ? C7 C8 C9 C10 0.3(2) . . . . ? C6 N2 C10 C9 -0.52(19) . . . . ? V1 N2 C10 C9 175.60(10) . . . . ? C8 C9 C10 N2 -0.4(2) . . . . ? C1 C2 C11 C12 -3.08(19) . . . . ? C3 C2 C11 C12 175.90(12) . . . . ? C2 C11 C12 C7 -0.3(2) . . . . ? C6 C7 C12 C11 3.17(19) . . . . ? C8 C7 C12 C11 -176.39(12) . . . . ? V1 N3 C13 C14 174(100) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.309 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.051 # Attachment '3.cif' data_oejlm247profc2c _database_code_depnum_ccdc_archive 'CCDC 736082' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[V3(O)Cl3(O2CPh)2(bipy)2(OEt)2]' _chemical_formula_sum 'C38 H36 Cl3 N4 O7 V3' _chemical_formula_weight 919.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 10.5712(6) _cell_length_b 21.0167(15) _cell_length_c 17.3205(10) _cell_angle_alpha 90.00 _cell_angle_beta 91.323(5) _cell_angle_gamma 90.00 _cell_volume 3847.1(4) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8523 _cell_measurement_theta_min 2.7275 _cell_measurement_theta_max 31.7439 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.588 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1872 _exptl_absorpt_coefficient_mu 0.977 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.6407 _exptl_absorpt_correction_T_max 0.6407 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcaliber 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17704 _diffrn_reflns_av_R_equivalents 0.0278 _diffrn_reflns_av_sigmaI/netI 0.0246 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.23 _diffrn_reflns_theta_max 30.55 _reflns_number_total 5794 _reflns_number_gt 5069 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) ; _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 ; The structure was solved by direct methods. Data processing was carried out to 0.70 angstroms as the data was only complete to this resolution. Hydrogen atoms were included in calculated positions. The ethyl group of the methoxide O4 C18 C19 is disordered over two sites. Geometric and displacement restraints were applied to the anisotropic thermal parameters of the atoms of this group. The benzoate group (O2 O3 C11 > C17) is not flat as would be expected. The elongated shape of the anisotropic thermal elipsoids for the carbon atoms C13 > C17 suggest that this group may be slightly disordered. This may be causing the deviation from planarity. Attempts to model this disorder failed as did attempts to flattern the group using geometric and dislacement restraints (FLAT command). This small degree of unmodeled disorder may be responsible for the slightly high Goodness of fit. 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^)+(0.0000P)^2^+36.8834P] 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 5794 _refine_ls_number_parameters 272 _refine_ls_number_restraints 41 _refine_ls_R_factor_all 0.0749 _refine_ls_R_factor_gt 0.0651 _refine_ls_wR_factor_ref 0.1474 _refine_ls_wR_factor_gt 0.1442 _refine_ls_goodness_of_fit_ref 1.292 _refine_ls_restrained_S_all 1.288 _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 0.39140(5) 0.41874(3) 0.16464(3) 0.01400(12) Uani 1 1 d . A . V2 V 0.5000 0.31245(4) 0.2500 0.01351(16) Uani 1 2 d S . . Cl1 Cl 0.24691(8) 0.42787(4) 0.05860(5) 0.02367(18) Uani 1 1 d . . . Cl2 Cl 0.5000 0.19935(6) 0.2500 0.0292(3) Uani 1 2 d S . . O1 O 0.5000 0.41077(15) 0.2500 0.0150(6) Uani 1 2 d S . . O2 O 0.5346(2) 0.39742(12) 0.09256(15) 0.0179(5) Uani 1 1 d . . . O3 O 0.6140(2) 0.31373(11) 0.15744(15) 0.0178(5) Uani 1 1 d . . . O4 O 0.3535(2) 0.32643(11) 0.18199(16) 0.0208(5) Uani 1 1 d D . . N1 N 0.4244(3) 0.51790(14) 0.15501(18) 0.0189(6) Uani 1 1 d . . . N2 N 0.2537(3) 0.45905(15) 0.23734(18) 0.0196(6) Uani 1 1 d . . . C1 C 0.3459(4) 0.55600(17) 0.1948(2) 0.0248(8) Uani 1 1 d . A . C2 C 0.3545(6) 0.6215(2) 0.1888(3) 0.0440(13) Uani 1 1 d . . . H2 H 0.2994 0.6475 0.2155 0.053 Uiso 1 1 calc R A . C3 C 0.4459(7) 0.6480(2) 0.1426(3) 0.0577(18) Uani 1 1 d . A . H3 H 0.4537 0.6919 0.1389 0.069 Uiso 1 1 calc R . . C4 C 0.5252(6) 0.60867(19) 0.1020(3) 0.0397(12) Uani 1 1 d . . . H4 H 0.5866 0.6255 0.0703 0.048 Uiso 1 1 calc R A . C5 C 0.5109(4) 0.54373(18) 0.1097(2) 0.0260(8) Uani 1 1 d . A . H5 H 0.5636 0.5170 0.0823 0.031 Uiso 1 1 calc R . . C6 C 0.2543(4) 0.52294(18) 0.2429(2) 0.0233(7) Uani 1 1 d . A . C7 C 0.1742(4) 0.5540(3) 0.2924(4) 0.0455(13) Uani 1 1 d . . . H7 H 0.1737 0.5982 0.2950 0.055 Uiso 1 1 calc R A . C8 C 0.0950(5) 0.5187(3) 0.3380(4) 0.067(2) Uani 1 1 d . A . H8 H 0.0435 0.5388 0.3734 0.081 Uiso 1 1 calc R . . C9 C 0.0932(5) 0.4538(3) 0.3307(4) 0.0513(15) Uani 1 1 d . . . H9 H 0.0378 0.4295 0.3595 0.062 Uiso 1 1 calc R A . C10 C 0.1743(3) 0.4248(2) 0.2802(3) 0.0289(8) Uani 1 1 d . A . H10 H 0.1739 0.3807 0.2758 0.035 Uiso 1 1 calc R . . C11 C 0.6174(3) 0.35509(16) 0.1049(2) 0.0168(6) Uani 1 1 d . . . C12 C 0.7295(3) 0.35482(19) 0.0542(2) 0.0233(7) Uani 1 1 d . . . C13 C 0.8124(4) 0.3038(2) 0.0562(3) 0.0351(10) Uani 1 1 d . . . H13 H 0.7962 0.2691 0.0877 0.042 Uiso 1 1 calc R . . C14 C 0.9201(5) 0.3042(3) 0.0113(4) 0.0529(16) Uani 1 1 d . . . H14 H 0.9754 0.2698 0.0123 0.063 Uiso 1 1 calc R . . C15 C 0.9433(5) 0.3564(3) -0.0347(4) 0.064(2) Uani 1 1 d . . . H15 H 1.0149 0.3571 -0.0649 0.077 Uiso 1 1 calc R . . C16 C 0.8617(5) 0.4074(3) -0.0364(4) 0.064(2) Uani 1 1 d . . . H16 H 0.8788 0.4425 -0.0672 0.076 Uiso 1 1 calc R . . C17 C 0.7543(4) 0.4065(2) 0.0076(3) 0.0381(11) Uani 1 1 d . . . H17 H 0.6986 0.4407 0.0059 0.046 Uiso 1 1 calc R . . C18X C 0.2399(6) 0.2884(3) 0.1668(4) 0.0231(18) Uani 0.501(10) 1 d PDU A 1 H18A H 0.1657 0.3152 0.1603 0.028 Uiso 0.501(10) 1 calc PR A 1 H18B H 0.2260 0.2582 0.2081 0.028 Uiso 0.501(10) 1 calc PR A 1 C19X C 0.2707(9) 0.2545(4) 0.0920(5) 0.034(2) Uani 0.501(10) 1 d PDU A 1 H19A H 0.2872 0.2854 0.0527 0.052 Uiso 0.501(10) 1 calc PR A 1 H19B H 0.2002 0.2285 0.0759 0.052 Uiso 0.501(10) 1 calc PR A 1 H19C H 0.3441 0.2282 0.1000 0.052 Uiso 0.501(10) 1 calc PR A 1 C18Y C 0.3197(7) 0.2825(3) 0.1192(4) 0.0241(18) Uani 0.499(10) 1 d PDU A 2 H18C H 0.3763 0.2462 0.1202 0.029 Uiso 0.499(10) 1 calc PR A 2 H18D H 0.3267 0.3037 0.0698 0.029 Uiso 0.499(10) 1 calc PR A 2 C19Y C 0.1844(10) 0.2609(7) 0.1308(7) 0.060(4) Uani 0.499(10) 1 d PDU A 2 H19D H 0.1767 0.2437 0.1818 0.090 Uiso 0.499(10) 1 calc PR A 2 H19E H 0.1626 0.2288 0.0933 0.090 Uiso 0.499(10) 1 calc PR A 2 H19F H 0.1282 0.2965 0.1245 0.090 Uiso 0.499(10) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0116(2) 0.0104(2) 0.0201(3) 0.0001(2) 0.00259(19) 0.00101(18) V2 0.0130(3) 0.0083(3) 0.0194(4) 0.000 0.0037(3) 0.000 Cl1 0.0185(4) 0.0263(4) 0.0261(4) 0.0005(3) -0.0020(3) 0.0000(3) Cl2 0.0471(8) 0.0079(5) 0.0327(7) 0.000 -0.0003(6) 0.000 O1 0.0152(15) 0.0089(14) 0.0211(16) 0.000 0.0057(12) 0.000 O2 0.0145(11) 0.0161(11) 0.0235(12) 0.0020(9) 0.0045(9) 0.0020(8) O3 0.0166(11) 0.0122(10) 0.0249(12) -0.0006(9) 0.0061(9) 0.0019(8) O4 0.0207(12) 0.0126(11) 0.0290(14) 0.0021(10) -0.0033(10) -0.0043(9) N1 0.0231(14) 0.0127(12) 0.0207(14) -0.0008(11) -0.0025(11) 0.0014(10) N2 0.0137(13) 0.0212(14) 0.0239(15) -0.0002(12) 0.0025(11) 0.0063(10) C1 0.037(2) 0.0148(15) 0.0225(17) -0.0021(13) -0.0034(15) 0.0096(14) C2 0.085(4) 0.0138(18) 0.033(2) -0.0024(16) 0.003(2) 0.017(2) C3 0.126(6) 0.0067(16) 0.041(3) 0.0023(17) 0.012(3) 0.000(2) C4 0.076(4) 0.0144(17) 0.029(2) 0.0055(15) 0.007(2) -0.0076(19) C5 0.039(2) 0.0156(16) 0.0236(18) 0.0015(13) -0.0011(16) -0.0027(14) C6 0.0194(16) 0.0224(17) 0.0281(19) -0.0069(14) -0.0001(14) 0.0092(13) C7 0.026(2) 0.041(3) 0.070(4) -0.023(3) 0.013(2) 0.0107(19) C8 0.037(3) 0.064(4) 0.103(6) -0.037(4) 0.047(3) -0.005(3) C9 0.023(2) 0.065(4) 0.067(4) -0.008(3) 0.031(2) -0.005(2) C10 0.0126(15) 0.036(2) 0.038(2) 0.0048(18) 0.0067(15) 0.0035(14) C11 0.0127(14) 0.0148(14) 0.0230(16) -0.0012(12) 0.0045(12) -0.0002(11) C12 0.0153(16) 0.0259(18) 0.0291(19) 0.0039(15) 0.0077(14) 0.0034(13) C13 0.024(2) 0.027(2) 0.055(3) 0.0052(19) 0.0217(19) 0.0064(15) C14 0.031(2) 0.042(3) 0.087(4) 0.016(3) 0.038(3) 0.016(2) C15 0.036(3) 0.068(4) 0.090(5) 0.035(4) 0.046(3) 0.022(3) C16 0.040(3) 0.068(4) 0.085(4) 0.049(3) 0.047(3) 0.027(3) C17 0.0215(19) 0.047(3) 0.047(3) 0.025(2) 0.0179(18) 0.0144(18) C18X 0.017(3) 0.018(3) 0.034(4) -0.006(3) 0.003(3) -0.003(2) C19X 0.032(5) 0.030(4) 0.041(5) -0.014(4) -0.003(4) 0.002(4) C18Y 0.032(4) 0.015(3) 0.025(4) -0.003(3) -0.004(3) -0.007(3) C19Y 0.054(7) 0.071(8) 0.054(7) -0.002(6) -0.002(5) -0.047(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 O1 1.8583(7) . ? V1 O4 2.005(2) . ? V1 O2 2.034(2) . ? V1 N1 2.120(3) . ? V1 N2 2.123(3) . ? V1 Cl1 2.3694(11) . ? V1 V2 2.9009(8) . ? V2 O4 1.946(3) . ? V2 O4 1.946(3) 2_655 ? V2 O3 2.028(2) . ? V2 O3 2.028(2) 2_655 ? V2 O1 2.066(3) . ? V2 Cl2 2.3769(14) . ? V2 V1 2.9009(8) 2_655 ? O1 V1 1.8583(7) 2_655 ? O2 C11 1.263(4) . ? O3 C11 1.259(4) . ? O4 C18X 1.462(5) . ? O4 C18Y 1.464(6) . ? N1 C5 1.334(5) . ? N1 C1 1.353(5) . ? N2 C10 1.342(5) . ? N2 C6 1.346(5) . ? C1 C2 1.383(5) . ? C1 C6 1.466(6) . ? C2 C3 1.385(8) . ? C2 H2 0.9300 . ? C3 C4 1.381(8) . ? C3 H3 0.9300 . ? C4 C5 1.380(5) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.383(5) . ? C7 C8 1.380(8) . ? C7 H7 0.9300 . ? C8 C9 1.370(9) . ? C8 H8 0.9300 . ? C9 C10 1.381(6) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C12 1.492(5) . ? C12 C17 1.381(6) . ? C12 C13 1.384(5) . ? C13 C14 1.393(6) . ? C13 H13 0.9300 . ? C14 C15 1.382(7) . ? C14 H14 0.9300 . ? C15 C16 1.375(7) . ? C15 H15 0.9300 . ? C16 C17 1.383(6) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18X C19X 1.521(8) . ? C18X H18A 0.9700 . ? C18X H18B 0.9700 . ? C19X H19A 0.9600 . ? C19X H19B 0.9600 . ? C19X H19C 0.9600 . ? C18Y C19Y 1.519(8) . ? C18Y H18C 0.9700 . ? C18Y H18D 0.9700 . ? C19Y H19D 0.9600 . ? C19Y H19E 0.9600 . ? C19Y H19F 0.9600 . ? 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 O4 85.15(12) . . ? O1 V1 O2 90.78(8) . . ? O4 V1 O2 91.88(11) . . ? O1 V1 N1 92.94(13) . . ? O4 V1 N1 175.33(12) . . ? O2 V1 N1 92.41(11) . . ? O1 V1 N2 89.05(9) . . ? O4 V1 N2 98.94(12) . . ? O2 V1 N2 169.13(11) . . ? N1 V1 N2 76.74(12) . . ? O1 V1 Cl1 177.98(5) . . ? O4 V1 Cl1 93.85(8) . . ? O2 V1 Cl1 91.00(8) . . ? N1 V1 Cl1 87.92(9) . . ? N2 V1 Cl1 89.37(9) . . ? O1 V1 V2 45.19(10) . . ? O4 V1 V2 41.97(8) . . ? O2 V1 V2 81.48(7) . . ? N1 V1 V2 137.14(9) . . ? N2 V1 V2 105.89(9) . . ? Cl1 V1 V2 134.26(3) . . ? O4 V2 O4 162.63(15) . 2_655 ? O4 V2 O3 89.91(11) . . ? O4 V2 O3 89.86(11) 2_655 . ? O4 V2 O3 89.86(11) . 2_655 ? O4 V2 O3 89.90(11) 2_655 2_655 ? O3 V2 O3 178.48(14) . 2_655 ? O4 V2 O1 81.31(7) . . ? O4 V2 O1 81.32(7) 2_655 . ? O3 V2 O1 89.24(7) . . ? O3 V2 O1 89.24(7) 2_655 . ? O4 V2 Cl2 98.69(7) . . ? O4 V2 Cl2 98.68(7) 2_655 . ? O3 V2 Cl2 90.76(7) . . ? O3 V2 Cl2 90.76(7) 2_655 . ? O1 V2 Cl2 180.0 . . ? O4 V2 V1 119.49(8) . 2_655 ? O4 V2 V1 43.55(7) 2_655 2_655 ? O3 V2 V1 99.05(7) . 2_655 ? O3 V2 V1 79.76(7) 2_655 2_655 ? O1 V2 V1 39.643(15) . 2_655 ? Cl2 V2 V1 140.357(15) . 2_655 ? O4 V2 V1 43.55(7) . . ? O4 V2 V1 119.49(8) 2_655 . ? O3 V2 V1 79.76(7) . . ? O3 V2 V1 99.05(7) 2_655 . ? O1 V2 V1 39.642(15) . . ? Cl2 V2 V1 140.358(15) . . ? V1 V2 V1 79.29(3) 2_655 . ? V1 O1 V1 169.66(19) 2_655 . ? V1 O1 V2 95.17(10) 2_655 . ? V1 O1 V2 95.17(10) . . ? C11 O2 V1 125.0(2) . . ? C11 O3 V2 127.4(2) . . ? C18X O4 C18Y 48.4(4) . . ? C18X O4 V2 131.7(4) . . ? C18Y O4 V2 122.1(3) . . ? C18X O4 V1 131.9(3) . . ? C18Y O4 V1 123.0(3) . . ? V2 O4 V1 94.48(11) . . ? C5 N1 C1 119.7(3) . . ? C5 N1 V1 124.2(3) . . ? C1 N1 V1 115.9(3) . . ? C10 N2 C6 119.8(3) . . ? C10 N2 V1 124.1(3) . . ? C6 N2 V1 116.0(3) . . ? N1 C1 C2 120.5(4) . . ? N1 C1 C6 115.4(3) . . ? C2 C1 C6 124.0(4) . . ? C1 C2 C3 119.4(4) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C4 C3 C2 119.6(4) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C5 C4 C3 118.2(5) . . ? C5 C4 H4 120.9 . . ? C3 C4 H4 120.9 . . ? N1 C5 C4 122.5(4) . . ? N1 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? N2 C6 C7 120.9(4) . . ? N2 C6 C1 115.7(3) . . ? C7 C6 C1 123.4(4) . . ? C8 C7 C6 119.3(5) . . ? C8 C7 H7 120.3 . . ? C6 C7 H7 120.3 . . ? C9 C8 C7 119.3(5) . . ? C9 C8 H8 120.3 . . ? C7 C8 H8 120.3 . . ? C8 C9 C10 119.3(5) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? N2 C10 C9 121.3(4) . . ? N2 C10 H10 119.3 . . ? C9 C10 H10 119.3 . . ? O3 C11 O2 125.3(3) . . ? O3 C11 C12 117.4(3) . . ? O2 C11 C12 117.4(3) . . ? C17 C12 C13 119.7(4) . . ? C17 C12 C11 120.3(3) . . ? C13 C12 C11 120.0(3) . . ? C12 C13 C14 120.4(4) . . ? C12 C13 H13 119.8 . . ? C14 C13 H13 119.8 . . ? C15 C14 C13 119.0(4) . . ? C15 C14 H14 120.5 . . ? C13 C14 H14 120.5 . . ? C16 C15 C14 120.7(4) . . ? C16 C15 H15 119.6 . . ? C14 C15 H15 119.6 . . ? C15 C16 C17 120.0(5) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C12 C17 C16 120.2(4) . . ? C12 C17 H17 119.9 . . ? C16 C17 H17 119.9 . . ? O4 C18X C19X 102.6(5) . . ? O4 C18X H18A 111.2 . . ? C19X C18X H18A 111.2 . . ? O4 C18X H18B 111.2 . . ? C19X C18X H18B 111.2 . . ? H18A C18X H18B 109.2 . . ? O4 C18Y C19Y 107.8(6) . . ? O4 C18Y H18C 110.1 . . ? C19Y C18Y H18C 110.1 . . ? O4 C18Y H18D 110.1 . . ? C19Y C18Y H18D 110.1 . . ? H18C C18Y H18D 108.5 . . ? C18Y C19Y H19D 109.5 . . ? C18Y C19Y H19E 109.5 . . ? H19D C19Y H19E 109.5 . . ? C18Y C19Y H19F 109.5 . . ? H19D C19Y H19F 109.5 . . ? H19E C19Y H19F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 V1 V2 O4 157.83(12) . . . . ? O2 V1 V2 O4 -102.48(14) . . . . ? N1 V1 V2 O4 173.20(18) . . . . ? N2 V1 V2 O4 85.71(15) . . . . ? Cl1 V1 V2 O4 -19.44(12) . . . . ? O1 V1 V2 O4 -17.38(9) . . . 2_655 ? O4 V1 V2 O4 -175.21(5) . . . 2_655 ? O2 V1 V2 O4 82.31(12) . . . 2_655 ? N1 V1 V2 O4 -2.01(16) . . . 2_655 ? N2 V1 V2 O4 -89.50(13) . . . 2_655 ? Cl1 V1 V2 O4 165.35(10) . . . 2_655 ? O1 V1 V2 O3 -101.35(7) . . . . ? O4 V1 V2 O3 100.81(14) . . . . ? O2 V1 V2 O3 -1.66(10) . . . . ? N1 V1 V2 O3 -85.99(15) . . . . ? N2 V1 V2 O3 -173.48(12) . . . . ? Cl1 V1 V2 O3 81.37(8) . . . . ? O1 V1 V2 O3 77.68(7) . . . 2_655 ? O4 V1 V2 O3 -80.15(14) . . . 2_655 ? O2 V1 V2 O3 177.37(10) . . . 2_655 ? N1 V1 V2 O3 93.05(15) . . . 2_655 ? N2 V1 V2 O3 5.56(12) . . . 2_655 ? Cl1 V1 V2 O3 -99.59(8) . . . 2_655 ? O4 V1 V2 O1 -157.83(12) . . . . ? O2 V1 V2 O1 99.69(8) . . . . ? N1 V1 V2 O1 15.36(13) . . . . ? N2 V1 V2 O1 -72.12(9) . . . . ? Cl1 V1 V2 O1 -177.27(5) . . . . ? O1 V1 V2 Cl2 180.0 . . . . ? O4 V1 V2 Cl2 22.17(12) . . . . ? O2 V1 V2 Cl2 -80.31(8) . . . . ? N1 V1 V2 Cl2 -164.64(13) . . . . ? N2 V1 V2 Cl2 107.88(9) . . . . ? Cl1 V1 V2 Cl2 2.73(5) . . . . ? O1 V1 V2 V1 0.0 . . . 2_655 ? O4 V1 V2 V1 -157.83(12) . . . 2_655 ? O2 V1 V2 V1 99.69(8) . . . 2_655 ? N1 V1 V2 V1 15.36(13) . . . 2_655 ? N2 V1 V2 V1 -72.12(9) . . . 2_655 ? Cl1 V1 V2 V1 -177.27(5) . . . 2_655 ? O4 V1 O1 V1 -165.34(8) . . . 2_655 ? O2 V1 O1 V1 102.85(7) . . . 2_655 ? N1 V1 O1 V1 10.39(9) . . . 2_655 ? N2 V1 O1 V1 -66.28(9) . . . 2_655 ? Cl1 V1 O1 V1 -105(3) . . . 2_655 ? V2 V1 O1 V1 179.995(1) . . . 2_655 ? O4 V1 O1 V2 14.67(8) . . . . ? O2 V1 O1 V2 -77.15(7) . . . . ? N1 V1 O1 V2 -169.60(9) . . . . ? N2 V1 O1 V2 113.72(9) . . . . ? Cl1 V1 O1 V2 75(3) . . . . ? O4 V2 O1 V1 164.75(8) . . . 2_655 ? O4 V2 O1 V1 -15.25(8) 2_655 . . 2_655 ? O3 V2 O1 V1 -105.22(7) . . . 2_655 ? O3 V2 O1 V1 74.77(7) 2_655 . . 2_655 ? Cl2 V2 O1 V1 -53(55) . . . 2_655 ? V1 V2 O1 V1 180.0 . . . 2_655 ? O4 V2 O1 V1 -15.25(8) . . . . ? O4 V2 O1 V1 164.75(8) 2_655 . . . ? O3 V2 O1 V1 74.77(7) . . . . ? O3 V2 O1 V1 -105.23(7) 2_655 . . . ? Cl2 V2 O1 V1 127(55) . . . . ? V1 V2 O1 V1 180.0 2_655 . . . ? O1 V1 O2 C11 40.9(3) . . . . ? O4 V1 O2 C11 -44.3(3) . . . . ? N1 V1 O2 C11 133.8(3) . . . . ? N2 V1 O2 C11 129.9(6) . . . . ? Cl1 V1 O2 C11 -138.2(3) . . . . ? V2 V1 O2 C11 -3.5(3) . . . . ? O4 V2 O3 C11 50.5(3) . . . . ? O4 V2 O3 C11 -112.1(3) 2_655 . . . ? O3 V2 O3 C11 -30.8(3) 2_655 . . . ? O1 V2 O3 C11 -30.8(3) . . . . ? Cl2 V2 O3 C11 149.2(3) . . . . ? V1 V2 O3 C11 -69.3(3) 2_655 . . . ? V1 V2 O3 C11 8.0(3) . . . . ? O4 V2 O4 C18X -151.3(4) 2_655 . . . ? O3 V2 O4 C18X 119.4(4) . . . . ? O3 V2 O4 C18X -62.1(4) 2_655 . . . ? O1 V2 O4 C18X -151.3(4) . . . . ? Cl2 V2 O4 C18X 28.7(4) . . . . ? V1 V2 O4 C18X -140.2(4) 2_655 . . . ? V1 V2 O4 C18X -165.4(5) . . . . ? O4 V2 O4 C18Y 148.1(4) 2_655 . . . ? O3 V2 O4 C18Y 58.8(4) . . . . ? O3 V2 O4 C18Y -122.7(4) 2_655 . . . ? O1 V2 O4 C18Y 148.1(4) . . . . ? Cl2 V2 O4 C18Y -31.9(4) . . . . ? V1 V2 O4 C18Y 159.2(4) 2_655 . . . ? V1 V2 O4 C18Y 134.0(4) . . . . ? O4 V2 O4 V1 14.09(7) 2_655 . . . ? O3 V2 O4 V1 -75.15(11) . . . . ? O3 V2 O4 V1 103.34(11) 2_655 . . . ? O1 V2 O4 V1 14.09(7) . . . . ? Cl2 V2 O4 V1 -165.91(7) . . . . ? V1 V2 O4 V1 25.21(13) 2_655 . . . ? O1 V1 O4 C18X 149.8(4) . . . . ? O2 V1 O4 C18X -119.6(4) . . . . ? N1 V1 O4 C18X 83.7(15) . . . . ? N2 V1 O4 C18X 61.5(4) . . . . ? Cl1 V1 O4 C18X -28.4(4) . . . . ? V2 V1 O4 C18X 165.4(5) . . . . ? O1 V1 O4 C18Y -149.0(4) . . . . ? O2 V1 O4 C18Y -58.3(4) . . . . ? N1 V1 O4 C18Y 145.0(14) . . . . ? N2 V1 O4 C18Y 122.8(4) . . . . ? Cl1 V1 O4 C18Y 32.8(4) . . . . ? V2 V1 O4 C18Y -133.4(4) . . . . ? O1 V1 O4 V2 -15.58(9) . . . . ? O2 V1 O4 V2 75.05(12) . . . . ? N1 V1 O4 V2 -81.6(14) . . . . ? N2 V1 O4 V2 -103.86(12) . . . . ? Cl1 V1 O4 V2 166.18(9) . . . . ? O1 V1 N1 C5 93.9(3) . . . . ? O4 V1 N1 C5 159.7(13) . . . . ? O2 V1 N1 C5 3.0(3) . . . . ? N2 V1 N1 C5 -177.7(3) . . . . ? Cl1 V1 N1 C5 -87.9(3) . . . . ? V2 V1 N1 C5 83.1(3) . . . . ? O1 V1 N1 C1 -90.0(3) . . . . ? O4 V1 N1 C1 -24.3(16) . . . . ? O2 V1 N1 C1 179.1(3) . . . . ? N2 V1 N1 C1 -1.7(3) . . . . ? Cl1 V1 N1 C1 88.1(3) . . . . ? V2 V1 N1 C1 -100.9(3) . . . . ? O1 V1 N2 C10 -83.3(3) . . . . ? O4 V1 N2 C10 1.6(3) . . . . ? O2 V1 N2 C10 -172.6(5) . . . . ? N1 V1 N2 C10 -176.6(3) . . . . ? Cl1 V1 N2 C10 95.4(3) . . . . ? V2 V1 N2 C10 -40.9(3) . . . . ? O1 V1 N2 C6 92.4(3) . . . . ? O4 V1 N2 C6 177.4(3) . . . . ? O2 V1 N2 C6 3.2(8) . . . . ? N1 V1 N2 C6 -0.8(3) . . . . ? Cl1 V1 N2 C6 -88.8(3) . . . . ? V2 V1 N2 C6 134.9(3) . . . . ? C5 N1 C1 C2 0.1(6) . . . . ? V1 N1 C1 C2 -176.1(4) . . . . ? C5 N1 C1 C6 180.0(3) . . . . ? V1 N1 C1 C6 3.8(4) . . . . ? N1 C1 C2 C3 -1.2(8) . . . . ? C6 C1 C2 C3 179.0(5) . . . . ? C1 C2 C3 C4 1.4(9) . . . . ? C2 C3 C4 C5 -0.6(9) . . . . ? C1 N1 C5 C4 0.7(6) . . . . ? V1 N1 C5 C4 176.6(4) . . . . ? C3 C4 C5 N1 -0.5(8) . . . . ? C10 N2 C6 C7 0.1(6) . . . . ? V1 N2 C6 C7 -175.8(4) . . . . ? C10 N2 C6 C1 179.0(4) . . . . ? V1 N2 C6 C1 3.0(4) . . . . ? N1 C1 C6 N2 -4.5(5) . . . . ? C2 C1 C6 N2 175.4(4) . . . . ? N1 C1 C6 C7 174.3(4) . . . . ? C2 C1 C6 C7 -5.8(7) . . . . ? N2 C6 C7 C8 1.6(8) . . . . ? C1 C6 C7 C8 -177.1(5) . . . . ? C6 C7 C8 C9 -3.0(10) . . . . ? C7 C8 C9 C10 2.7(11) . . . . ? C6 N2 C10 C9 -0.5(6) . . . . ? V1 N2 C10 C9 175.1(4) . . . . ? C8 C9 C10 N2 -0.9(9) . . . . ? V2 O3 C11 O2 -13.8(5) . . . . ? V2 O3 C11 C12 165.0(2) . . . . ? V1 O2 C11 O3 10.9(5) . . . . ? V1 O2 C11 C12 -167.9(2) . . . . ? O3 C11 C12 C17 -165.2(4) . . . . ? O2 C11 C12 C17 13.7(6) . . . . ? O3 C11 C12 C13 11.8(6) . . . . ? O2 C11 C12 C13 -169.3(4) . . . . ? C17 C12 C13 C14 -0.4(8) . . . . ? C11 C12 C13 C14 -177.5(5) . . . . ? C12 C13 C14 C15 0.5(10) . . . . ? C13 C14 C15 C16 0.0(12) . . . . ? C14 C15 C16 C17 -0.7(12) . . . . ? C13 C12 C17 C16 -0.3(8) . . . . ? C11 C12 C17 C16 176.7(5) . . . . ? C15 C16 C17 C12 0.9(11) . . . . ? C18Y O4 C18X C19X 0.0(6) . . . . ? V2 O4 C18X C19X -99.2(6) . . . . ? V1 O4 C18X C19X 100.5(6) . . . . ? C18X O4 C18Y C19Y 4.5(7) . . . . ? V2 O4 C18Y C19Y 124.0(7) . . . . ? V1 O4 C18Y C19Y -114.8(7) . . . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 30.55 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.586 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.117 # Attachment '4.cif' data_oejlm242profp-1 _database_code_depnum_ccdc_archive 'CCDC 736083' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[V4Cl6(thme)2(bipy)3]2.5MeCN' _chemical_formula_sum 'C45 H49.50 Cl6 N8.50 O6 V4' _chemical_formula_weight 1221.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4530(6) _cell_length_b 12.7770(8) _cell_length_c 19.8817(7) _cell_angle_alpha 83.718(4) _cell_angle_beta 78.696(4) _cell_angle_gamma 66.155(5) _cell_volume 2608.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 5682 _cell_measurement_theta_min 2.6155 _cell_measurement_theta_max 31.9514 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1242 _exptl_absorpt_coefficient_mu 1.057 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.6201 _exptl_absorpt_correction_T_max 0.6201 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcaliber 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20125 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0661 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.62 _diffrn_reflns_theta_max 26.37 _reflns_number_total 10626 _reflns_number_gt 7123 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) ; _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 ; The structure was solved by direct methods. Data processing was carried out to 0.80 angstroms as the data was only complete to this resolution. Hydrogen atoms were included in calculated positions. In the acetonitrile molecule N8 C43 C44, the atoms C43 and C44 share the same atomic coordinates. The acetonitrile molecule N9 C45 C46 is disordered over two sites. Geometric and displacement restraints were applied to the anisotropic thermal parameters of the atoms of this molecule. 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^)+(0.0596P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10626 _refine_ls_number_parameters 664 _refine_ls_number_restraints 60 _refine_ls_R_factor_all 0.0600 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.1079 _refine_ls_wR_factor_gt 0.0882 _refine_ls_goodness_of_fit_ref 0.996 _refine_ls_restrained_S_all 0.993 _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 0.23950(5) 0.12767(4) 0.24912(3) 0.01133(13) Uani 1 1 d . . . V2 V 0.05906(5) 0.23206(4) 0.38301(3) 0.01236(13) Uani 1 1 d . . . V3 V 0.35713(5) -0.13423(4) 0.23221(3) 0.01293(13) Uani 1 1 d . . . V4 V 0.30735(5) 0.28223(4) 0.12950(3) 0.01399(13) Uani 1 1 d . . . Cl1 Cl -0.15286(8) 0.37570(7) 0.40305(4) 0.01884(18) Uani 1 1 d . . . Cl2 Cl -0.01774(8) 0.08660(7) 0.40525(4) 0.01799(18) Uani 1 1 d . . . Cl3 Cl 0.25961(9) -0.26828(7) 0.24687(4) 0.0235(2) Uani 1 1 d . . . Cl4 Cl 0.36488(8) -0.12908(7) 0.11497(4) 0.02125(19) Uani 1 1 d . . . Cl5 Cl 0.28792(8) 0.29218(7) 0.01319(4) 0.02087(19) Uani 1 1 d . . . Cl6 Cl 0.11609(8) 0.44417(7) 0.15403(4) 0.01924(18) Uani 1 1 d . . . O1 O 0.0602(2) 0.23447(17) 0.28151(10) 0.0127(5) Uani 1 1 d . . . O2 O 0.18604(19) 0.00141(17) 0.24725(10) 0.0116(5) Uani 1 1 d . . . O3 O 0.2187(2) 0.17266(17) 0.15381(10) 0.0136(5) Uani 1 1 d . . . O4 O 0.24183(19) 0.13782(17) 0.34823(10) 0.0128(5) Uani 1 1 d . . . O5 O 0.40815(19) -0.00912(17) 0.24201(10) 0.0131(5) Uani 1 1 d . . . O6 O 0.33716(19) 0.23126(17) 0.22357(10) 0.0132(5) Uani 1 1 d . . . N1 N 0.1180(2) 0.3692(2) 0.38119(13) 0.0135(6) Uani 1 1 d . . . N2 N 0.0904(2) 0.2337(2) 0.48558(13) 0.0137(6) Uani 1 1 d . . . N3 N 0.3752(2) -0.1826(2) 0.33686(13) 0.0145(6) Uani 1 1 d . . . N4 N 0.5500(2) -0.2601(2) 0.22830(13) 0.0142(6) Uani 1 1 d . . . N5 N 0.4232(3) 0.3828(2) 0.11036(13) 0.0153(6) Uani 1 1 d . . . N6 N 0.4960(3) 0.1634(2) 0.09379(13) 0.0164(6) Uani 1 1 d . . . C1 C -0.0376(3) 0.2372(3) 0.24672(16) 0.0154(7) Uani 1 1 d . . . H1A H -0.0755 0.3126 0.2254 0.019 Uiso 1 1 calc R . . H1B H -0.1054 0.2245 0.2799 0.019 Uiso 1 1 calc R . . C2 C 0.0705(3) 0.0245(3) 0.22132(16) 0.0145(7) Uani 1 1 d . . . H2A H 0.0072 0.0123 0.2580 0.017 Uiso 1 1 calc R . . H2B H 0.0891 -0.0290 0.1858 0.017 Uiso 1 1 calc R . . C3 C 0.1079(3) 0.1719(3) 0.13255(16) 0.0174(7) Uani 1 1 d . . . H3A H 0.1357 0.1143 0.0983 0.021 Uiso 1 1 calc R . . H3B H 0.0634 0.2457 0.1110 0.021 Uiso 1 1 calc R . . C4 C 0.0124(3) 0.1474(3) 0.19151(16) 0.0144(7) Uani 1 1 d . . . C5 C -0.1046(3) 0.1569(3) 0.16117(17) 0.0207(8) Uani 1 1 d . . . H5A H -0.1643 0.1379 0.1961 0.031 Uiso 1 1 calc R . . H5B H -0.0762 0.1049 0.1243 0.031 Uiso 1 1 calc R . . H5C H -0.1465 0.2338 0.1440 0.031 Uiso 1 1 calc R . . C6 C 0.3611(3) 0.1204(3) 0.36876(16) 0.0155(7) Uani 1 1 d . . . H6A H 0.3860 0.0524 0.3986 0.019 Uiso 1 1 calc R . . H6B H 0.3481 0.1850 0.3951 0.019 Uiso 1 1 calc R . . C7 C 0.5112(3) -0.0033(3) 0.26970(17) 0.0158(7) Uani 1 1 d . . . H7A H 0.5822 -0.0087 0.2326 0.019 Uiso 1 1 calc R . . H7B H 0.5422 -0.0686 0.3009 0.019 Uiso 1 1 calc R . . C8 C 0.4407(3) 0.2128(3) 0.25933(16) 0.0156(7) Uani 1 1 d . . . H8A H 0.4186 0.2798 0.2856 0.019 Uiso 1 1 calc R . . H8B H 0.5177 0.2049 0.2260 0.019 Uiso 1 1 calc R . . C9 C 0.4721(3) 0.1067(3) 0.30812(16) 0.0148(7) Uani 1 1 d . . . C10 C 0.5897(3) 0.0957(3) 0.33861(17) 0.0205(8) Uani 1 1 d . . . H10A H 0.6630 0.0823 0.3026 0.031 Uiso 1 1 calc R . . H10B H 0.6088 0.0328 0.3715 0.031 Uiso 1 1 calc R . . H10C H 0.5709 0.1651 0.3608 0.031 Uiso 1 1 calc R . . C11 C 0.1430(3) 0.3937(3) 0.43992(16) 0.0150(7) Uani 1 1 d . . . C12 C 0.1804(3) 0.4837(3) 0.44212(17) 0.0210(8) Uani 1 1 d . . . H12 H 0.1969 0.4999 0.4829 0.025 Uiso 1 1 calc R . . C13 C 0.1928(4) 0.5485(3) 0.38333(18) 0.0269(9) Uani 1 1 d . . . H13 H 0.2179 0.6091 0.3839 0.032 Uiso 1 1 calc R . . C14 C 0.1675(4) 0.5228(3) 0.32338(18) 0.0248(8) Uani 1 1 d . . . H14 H 0.1757 0.5656 0.2831 0.030 Uiso 1 1 calc R . . C15 C 0.1299(3) 0.4330(3) 0.32407(16) 0.0182(7) Uani 1 1 d . . . H15 H 0.1123 0.4160 0.2838 0.022 Uiso 1 1 calc R . . C16 C 0.1268(3) 0.3171(3) 0.49909(16) 0.0151(7) Uani 1 1 d . . . C17 C 0.1478(4) 0.3279(3) 0.56355(17) 0.0252(8) Uani 1 1 d . . . H17 H 0.1724 0.3857 0.5719 0.030 Uiso 1 1 calc R . . C18 C 0.1314(4) 0.2509(3) 0.61576(18) 0.0318(9) Uani 1 1 d . . . H18 H 0.1456 0.2560 0.6595 0.038 Uiso 1 1 calc R . . C19 C 0.0938(4) 0.1671(3) 0.60190(18) 0.0286(9) Uani 1 1 d . . . H19 H 0.0818 0.1151 0.6363 0.034 Uiso 1 1 calc R . . C20 C 0.0744(3) 0.1610(3) 0.53679(17) 0.0199(8) Uani 1 1 d . . . H20 H 0.0490 0.1041 0.5279 0.024 Uiso 1 1 calc R . . C21 C 0.4844(3) -0.2706(3) 0.34981(16) 0.0170(7) Uani 1 1 d . . . C22 C 0.4965(4) -0.3210(3) 0.41443(17) 0.0252(8) Uani 1 1 d . . . H22 H 0.5722 -0.3822 0.4222 0.030 Uiso 1 1 calc R . . C23 C 0.3940(4) -0.2790(3) 0.46727(18) 0.0325(9) Uani 1 1 d . . . H23 H 0.3992 -0.3121 0.5112 0.039 Uiso 1 1 calc R . . C24 C 0.2840(4) -0.1874(3) 0.45423(18) 0.0278(9) Uani 1 1 d . . . H24 H 0.2149 -0.1566 0.4895 0.033 Uiso 1 1 calc R . . C25 C 0.2775(3) -0.1422(3) 0.38887(17) 0.0218(8) Uani 1 1 d . . . H25 H 0.2024 -0.0810 0.3803 0.026 Uiso 1 1 calc R . . C26 C 0.5867(3) -0.3091(3) 0.28901(16) 0.0153(7) Uani 1 1 d . . . C27 C 0.7109(3) -0.3888(3) 0.29258(18) 0.0224(8) Uani 1 1 d . . . H27 H 0.7338 -0.4218 0.3347 0.027 Uiso 1 1 calc R . . C28 C 0.8001(4) -0.4188(3) 0.23329(19) 0.0298(9) Uani 1 1 d . . . H28 H 0.8841 -0.4716 0.2348 0.036 Uiso 1 1 calc R . . C29 C 0.7632(3) -0.3694(3) 0.17156(19) 0.0286(9) Uani 1 1 d . . . H29 H 0.8220 -0.3890 0.1309 0.034 Uiso 1 1 calc R . . C30 C 0.6387(3) -0.2908(3) 0.17068(17) 0.0214(8) Uani 1 1 d . . . H30 H 0.6147 -0.2577 0.1288 0.026 Uiso 1 1 calc R . . C31 C 0.5489(3) 0.3276(3) 0.08189(16) 0.0151(7) Uani 1 1 d . . . C32 C 0.6306(3) 0.3853(3) 0.06163(17) 0.0213(8) Uani 1 1 d . . . H32 H 0.7166 0.3458 0.0423 0.026 Uiso 1 1 calc R . . C33 C 0.5831(4) 0.5014(3) 0.07032(17) 0.0236(8) Uani 1 1 d . . . H33 H 0.6366 0.5413 0.0568 0.028 Uiso 1 1 calc R . . C34 C 0.4556(4) 0.5576(3) 0.09926(17) 0.0239(8) Uani 1 1 d . . . H34 H 0.4216 0.6361 0.1054 0.029 Uiso 1 1 calc R . . C35 C 0.3793(3) 0.4964(3) 0.11889(17) 0.0200(8) Uani 1 1 d . . . H35 H 0.2936 0.5349 0.1390 0.024 Uiso 1 1 calc R . . C36 C 0.5905(3) 0.2034(3) 0.07361(16) 0.0159(7) Uani 1 1 d . . . C37 C 0.7136(3) 0.1323(3) 0.04585(16) 0.0203(8) Uani 1 1 d . . . H37 H 0.7777 0.1610 0.0319 0.024 Uiso 1 1 calc R . . C38 C 0.7413(3) 0.0175(3) 0.03887(17) 0.0256(8) Uani 1 1 d . . . H38 H 0.8248 -0.0320 0.0213 0.031 Uiso 1 1 calc R . . C39 C 0.6449(3) -0.0223(3) 0.05806(17) 0.0233(8) Uani 1 1 d . . . H39 H 0.6614 -0.0986 0.0527 0.028 Uiso 1 1 calc R . . C40 C 0.5238(3) 0.0520(3) 0.08532(16) 0.0209(8) Uani 1 1 d . . . H40 H 0.4583 0.0248 0.0985 0.025 Uiso 1 1 calc R . . N7 N 0.5061(4) 0.4056(4) 0.3840(2) 0.0612(12) Uani 1 1 d . . . C41 C 0.5348(4) 0.4208(4) 0.3270(3) 0.0425(11) Uani 1 1 d . . . C42 C 0.5684(5) 0.4395(4) 0.2543(2) 0.0582(14) Uani 1 1 d . . . H42A H 0.5599 0.3828 0.2300 0.087 Uiso 1 1 calc R . . H42B H 0.6561 0.4339 0.2439 0.087 Uiso 1 1 calc R . . H42C H 0.5114 0.5144 0.2407 0.087 Uiso 1 1 calc R . . N8 N 0.0774(6) 0.6227(6) 0.9862(3) 0.0309(15) Uani 0.50 1 d P . . C43 C 0.0288(4) 0.5448(4) 0.9938(2) 0.0517(14) Uani 0.50 1 d P . . C44 C 0.0288(4) 0.5448(4) 0.9938(2) 0.0517(14) Uani 0.50 1 d P . . H44A H -0.0362 0.6172 1.0095 0.078 Uiso 0.50 1 calc PR . . H44B H 0.0592 0.5515 0.9457 0.078 Uiso 0.50 1 calc PR . . H44C H 0.0997 0.5226 1.0185 0.078 Uiso 0.50 1 calc PR . . N9X N 0.0522(8) 0.7785(7) 0.0389(4) 0.046(3) Uani 0.412(7) 1 d PDU A 1 C45X C 0.0235(12) 0.7722(13) 0.0976(5) 0.034(3) Uani 0.412(7) 1 d PDU A 1 C46X C -0.0123(15) 0.7646(12) 0.1703(4) 0.044(3) Uani 0.412(7) 1 d PDU A 1 H46A H -0.0948 0.8250 0.1844 0.066 Uiso 0.412(7) 1 calc PR A 1 H46B H 0.0517 0.7716 0.1921 0.066 Uiso 0.412(7) 1 calc PR A 1 H46C H -0.0180 0.6919 0.1832 0.066 Uiso 0.412(7) 1 calc PR A 1 N9Y N -0.1464(6) 0.8666(6) 0.2220(3) 0.055(2) Uani 0.588(7) 1 d PDU A 2 C45Y C -0.0608(7) 0.8245(8) 0.1790(4) 0.034(2) Uani 0.588(7) 1 d PDU A 2 C46Y C 0.0438(8) 0.7749(12) 0.1246(5) 0.055(3) Uani 0.588(7) 1 d PDU A 2 H46D H 0.1178 0.7878 0.1311 0.083 Uiso 0.588(7) 1 calc PR A 2 H46E H 0.0188 0.8094 0.0816 0.083 Uiso 0.588(7) 1 calc PR A 2 H46F H 0.0654 0.6940 0.1247 0.083 Uiso 0.588(7) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0138(3) 0.0105(3) 0.0103(3) 0.0007(2) -0.0021(2) -0.0056(2) V2 0.0150(3) 0.0116(3) 0.0103(3) -0.0004(2) -0.0003(2) -0.0059(2) V3 0.0166(3) 0.0097(3) 0.0125(3) 0.0004(2) -0.0016(2) -0.0057(2) V4 0.0191(3) 0.0114(3) 0.0109(3) 0.0006(2) 0.0001(2) -0.0069(2) Cl1 0.0196(4) 0.0149(4) 0.0188(4) -0.0024(3) -0.0030(3) -0.0031(3) Cl2 0.0213(4) 0.0154(4) 0.0163(4) 0.0003(3) 0.0020(3) -0.0088(3) Cl3 0.0323(5) 0.0184(4) 0.0254(5) 0.0040(4) -0.0047(4) -0.0170(4) Cl4 0.0304(5) 0.0183(4) 0.0156(4) 0.0007(3) -0.0039(4) -0.0104(4) Cl5 0.0329(5) 0.0193(4) 0.0119(4) -0.0003(3) -0.0004(3) -0.0133(4) Cl6 0.0192(4) 0.0182(4) 0.0161(4) -0.0011(3) -0.0005(3) -0.0040(3) O1 0.0153(11) 0.0148(11) 0.0099(11) 0.0007(9) -0.0032(9) -0.0077(9) O2 0.0132(11) 0.0117(11) 0.0118(11) 0.0016(9) -0.0037(9) -0.0065(9) O3 0.0155(11) 0.0155(11) 0.0122(11) 0.0032(9) -0.0032(9) -0.0091(10) O4 0.0138(11) 0.0143(11) 0.0123(11) -0.0007(9) -0.0025(9) -0.0073(9) O5 0.0129(11) 0.0118(11) 0.0156(12) 0.0004(9) -0.0037(9) -0.0054(9) O6 0.0145(11) 0.0136(11) 0.0124(11) 0.0023(9) -0.0031(9) -0.0068(9) N1 0.0180(14) 0.0099(13) 0.0127(14) -0.0011(11) -0.0004(11) -0.0065(11) N2 0.0170(14) 0.0146(14) 0.0104(14) -0.0006(11) -0.0019(11) -0.0070(12) N3 0.0164(14) 0.0120(14) 0.0123(14) 0.0011(11) 0.0004(11) -0.0043(12) N4 0.0166(14) 0.0123(14) 0.0137(14) -0.0001(11) -0.0003(11) -0.0066(12) N5 0.0210(15) 0.0140(14) 0.0119(14) 0.0006(11) -0.0005(11) -0.0092(12) N6 0.0226(15) 0.0132(14) 0.0127(14) -0.0021(11) 0.0010(12) -0.0075(12) C1 0.0161(17) 0.0167(17) 0.0146(17) 0.0008(14) -0.0047(13) -0.0068(14) C2 0.0168(17) 0.0152(16) 0.0160(17) 0.0015(13) -0.0052(14) -0.0103(14) C3 0.0216(18) 0.0195(18) 0.0149(17) 0.0017(14) -0.0059(14) -0.0110(15) C4 0.0167(17) 0.0153(17) 0.0136(16) 0.0016(13) -0.0058(13) -0.0078(14) C5 0.0223(18) 0.0240(19) 0.0195(18) 0.0025(15) -0.0089(15) -0.0112(16) C6 0.0175(17) 0.0165(17) 0.0153(17) -0.0004(14) -0.0062(14) -0.0078(14) C7 0.0120(16) 0.0147(17) 0.0198(18) -0.0010(14) -0.0021(13) -0.0047(14) C8 0.0153(17) 0.0178(17) 0.0168(17) -0.0012(14) -0.0039(14) -0.0090(14) C9 0.0152(16) 0.0143(17) 0.0152(17) -0.0004(13) -0.0040(13) -0.0056(14) C10 0.0192(18) 0.0218(18) 0.0233(19) -0.0010(15) -0.0067(15) -0.0096(15) C11 0.0156(17) 0.0142(17) 0.0138(17) -0.0003(13) 0.0000(13) -0.0056(14) C12 0.029(2) 0.0226(19) 0.0145(17) -0.0059(15) -0.0005(15) -0.0133(16) C13 0.037(2) 0.0211(19) 0.028(2) -0.0025(16) 0.0019(17) -0.0205(18) C14 0.038(2) 0.0214(19) 0.0178(19) 0.0022(15) 0.0018(16) -0.0184(17) C15 0.0251(19) 0.0158(17) 0.0119(17) -0.0015(14) 0.0019(14) -0.0081(15) C16 0.0154(17) 0.0140(16) 0.0150(17) 0.0007(14) -0.0011(13) -0.0058(14) C17 0.037(2) 0.027(2) 0.0201(19) -0.0015(16) -0.0087(16) -0.0197(18) C18 0.050(3) 0.038(2) 0.0142(19) 0.0050(17) -0.0114(17) -0.023(2) C19 0.048(2) 0.028(2) 0.0170(19) 0.0101(16) -0.0092(17) -0.0226(19) C20 0.029(2) 0.0189(18) 0.0163(18) 0.0038(14) -0.0068(15) -0.0135(16) C21 0.0205(18) 0.0150(17) 0.0151(17) 0.0014(14) -0.0052(14) -0.0062(15) C22 0.026(2) 0.027(2) 0.0190(19) 0.0070(16) -0.0063(15) -0.0081(17) C23 0.042(2) 0.042(2) 0.0129(18) 0.0112(17) -0.0053(17) -0.019(2) C24 0.029(2) 0.035(2) 0.0135(18) -0.0019(16) 0.0035(16) -0.0096(18) C25 0.0204(18) 0.0185(18) 0.0199(19) -0.0010(15) 0.0010(15) -0.0029(15) C26 0.0183(17) 0.0119(16) 0.0154(17) -0.0012(13) -0.0015(14) -0.0062(14) C27 0.0234(19) 0.0186(18) 0.0235(19) 0.0003(15) -0.0080(15) -0.0048(15) C28 0.0209(19) 0.026(2) 0.034(2) -0.0046(18) -0.0039(17) 0.0004(16) C29 0.0219(19) 0.030(2) 0.027(2) -0.0108(17) 0.0056(16) -0.0047(17) C30 0.0232(19) 0.0203(18) 0.0172(18) -0.0031(15) 0.0036(15) -0.0075(16) C31 0.0202(17) 0.0175(17) 0.0092(16) 0.0015(13) -0.0037(13) -0.0089(15) C32 0.0252(19) 0.028(2) 0.0149(18) 0.0023(15) -0.0034(15) -0.0159(17) C33 0.035(2) 0.026(2) 0.0191(19) 0.0040(16) -0.0048(16) -0.0221(18) C34 0.040(2) 0.0165(18) 0.0207(19) 0.0011(15) -0.0064(17) -0.0165(17) C35 0.0256(19) 0.0132(17) 0.0208(18) -0.0008(14) -0.0018(15) -0.0081(15) C36 0.0205(18) 0.0191(18) 0.0086(16) 0.0012(13) -0.0038(13) -0.0080(15) C37 0.0202(18) 0.026(2) 0.0127(17) -0.0025(15) -0.0026(14) -0.0062(16) C38 0.0222(19) 0.028(2) 0.0171(18) -0.0067(16) -0.0037(15) 0.0021(16) C39 0.036(2) 0.0108(17) 0.0165(18) -0.0040(14) -0.0012(16) -0.0038(16) C40 0.031(2) 0.0163(18) 0.0156(18) 0.0003(14) 0.0005(15) -0.0117(16) N7 0.067(3) 0.067(3) 0.049(3) 0.010(2) -0.026(2) -0.021(2) C41 0.046(3) 0.034(2) 0.053(3) 0.001(2) -0.024(2) -0.015(2) C42 0.087(4) 0.057(3) 0.049(3) -0.004(3) -0.004(3) -0.051(3) N8 0.023(3) 0.040(4) 0.036(4) 0.012(3) -0.011(3) -0.019(3) C43 0.031(3) 0.065(4) 0.029(2) 0.002(2) -0.005(2) 0.011(2) C44 0.031(3) 0.065(4) 0.029(2) 0.002(2) -0.005(2) 0.011(2) N9X 0.028(5) 0.044(6) 0.060(6) -0.003(5) 0.008(4) -0.016(4) C45X 0.020(5) 0.023(6) 0.061(7) 0.008(7) -0.010(6) -0.012(5) C46X 0.051(9) 0.028(7) 0.056(7) 0.001(7) -0.016(7) -0.017(7) N9Y 0.050(4) 0.073(5) 0.049(4) 0.008(4) -0.012(3) -0.034(4) C45Y 0.042(5) 0.033(5) 0.036(4) 0.007(4) -0.018(3) -0.022(4) C46Y 0.054(7) 0.049(6) 0.057(7) -0.020(6) -0.018(5) -0.007(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 O2 1.949(2) . ? V1 O3 1.951(2) . ? V1 O1 1.975(2) . ? V1 O4 1.995(2) . ? V1 O5 2.006(2) . ? V1 O6 2.022(2) . ? V1 V2 3.0867(7) . ? V1 V3 3.0902(7) . ? V1 V4 3.1062(7) . ? V2 O4 1.971(2) . ? V2 O1 2.012(2) . ? V2 N1 2.113(3) . ? V2 N2 2.142(3) . ? V2 Cl2 2.3265(9) . ? V2 Cl1 2.3659(9) . ? V3 O5 1.950(2) . ? V3 O2 2.018(2) . ? V3 N3 2.130(3) . ? V3 N4 2.135(3) . ? V3 Cl4 2.3099(10) . ? V3 Cl3 2.3613(9) . ? V4 O6 1.960(2) . ? V4 O3 2.008(2) . ? V4 N6 2.112(3) . ? V4 N5 2.152(3) . ? V4 Cl6 2.3355(10) . ? V4 Cl5 2.3509(10) . ? O1 C1 1.415(4) . ? O2 C2 1.422(4) . ? O3 C3 1.418(4) . ? O4 C6 1.426(4) . ? O5 C7 1.427(4) . ? O6 C8 1.427(4) . ? N1 C15 1.341(4) . ? N1 C11 1.351(4) . ? N2 C20 1.337(4) . ? N2 C16 1.359(4) . ? N3 C25 1.335(4) . ? N3 C21 1.349(4) . ? N4 C30 1.348(4) . ? N4 C26 1.359(4) . ? N5 C35 1.348(4) . ? N5 C31 1.355(4) . ? N6 C40 1.350(4) . ? N6 C36 1.350(4) . ? C1 C4 1.532(4) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C4 1.538(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.538(4) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.530(4) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C9 1.538(4) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C9 1.534(4) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.537(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.533(4) . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 C12 1.387(4) . ? C11 C16 1.478(4) . ? C12 C13 1.375(5) . ? C12 H12 0.9300 . ? C13 C14 1.382(5) . ? C13 H13 0.9300 . ? C14 C15 1.377(5) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.381(4) . ? C17 C18 1.390(5) . ? C17 H17 0.9300 . ? C18 C19 1.375(5) . ? C18 H18 0.9300 . ? C19 C20 1.371(5) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.379(4) . ? C21 C26 1.478(4) . ? C22 C23 1.378(5) . ? C22 H22 0.9300 . ? C23 C24 1.376(5) . ? C23 H23 0.9300 . ? C24 C25 1.366(5) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.385(4) . ? C27 C28 1.375(5) . ? C27 H27 0.9300 . ? C28 C29 1.379(5) . ? C28 H28 0.9300 . ? C29 C30 1.375(5) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.387(4) . ? C31 C36 1.480(4) . ? C32 C33 1.377(5) . ? C32 H32 0.9300 . ? C33 C34 1.376(5) . ? C33 H33 0.9300 . ? C34 C35 1.371(5) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C37 1.374(4) . ? C37 C38 1.387(5) . ? C37 H37 0.9300 . ? C38 C39 1.368(5) . ? C38 H38 0.9300 . ? C39 C40 1.368(5) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? N7 C41 1.134(6) . ? C41 C42 1.440(6) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? N8 C43 1.306(7) . ? C43 C44 1.512(11) 2_567 ? N9X C45X 1.1520(8) . ? C45X C46X 1.4261(8) . ? C46X H46A 0.9600 . ? C46X H46B 0.9600 . ? C46X H46C 0.9600 . ? N9Y C45Y 1.1520(9) . ? C45Y C46Y 1.4262(9) . ? C46Y H46D 0.9600 . ? C46Y H46E 0.9600 . ? C46Y H46F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 V1 O3 92.06(8) . . ? O2 V1 O1 92.21(8) . . ? O3 V1 O1 90.98(9) . . ? O2 V1 O4 103.89(8) . . ? O3 V1 O4 160.87(9) . . ? O1 V1 O4 78.11(8) . . ? O2 V1 O5 77.44(8) . . ? O3 V1 O5 103.85(9) . . ? O1 V1 O5 162.07(8) . . ? O4 V1 O5 90.07(8) . . ? O2 V1 O6 160.76(9) . . ? O3 V1 O6 76.93(8) . . ? O1 V1 O6 103.56(9) . . ? O4 V1 O6 90.27(8) . . ? O5 V1 O6 89.78(8) . . ? O2 V1 V2 97.14(6) . . ? O3 V1 V2 129.87(7) . . ? O1 V1 V2 39.72(6) . . ? O4 V1 V2 38.63(6) . . ? O5 V1 V2 126.26(6) . . ? O6 V1 V2 102.03(6) . . ? O2 V1 V3 39.63(6) . . ? O3 V1 V3 97.47(6) . . ? O1 V1 V3 131.05(6) . . ? O4 V1 V3 101.54(6) . . ? O5 V1 V3 37.99(6) . . ? O6 V1 V3 125.34(6) . . ? V2 V1 V3 120.24(2) . . ? O2 V1 V4 129.82(6) . . ? O3 V1 V4 38.97(6) . . ? O1 V1 V4 97.53(6) . . ? O4 V1 V4 126.29(6) . . ? O5 V1 V4 100.35(6) . . ? O6 V1 V4 38.03(6) . . ? V2 V1 V4 120.99(2) . . ? V3 V1 V4 118.76(2) . . ? O4 V2 O1 77.78(8) . . ? O4 V2 N1 86.59(9) . . ? O1 V2 N1 96.76(9) . . ? O4 V2 N2 94.39(9) . . ? O1 V2 N2 169.54(9) . . ? N1 V2 N2 75.64(10) . . ? O4 V2 Cl2 98.41(6) . . ? O1 V2 Cl2 92.71(6) . . ? N1 V2 Cl2 170.06(7) . . ? N2 V2 Cl2 95.33(7) . . ? O4 V2 Cl1 166.24(7) . . ? O1 V2 Cl1 92.93(6) . . ? N1 V2 Cl1 84.44(7) . . ? N2 V2 Cl1 93.46(7) . . ? Cl2 V2 Cl1 92.08(3) . . ? O4 V2 V1 39.18(6) . . ? O1 V2 V1 38.84(6) . . ? N1 V2 V1 95.44(7) . . ? N2 V2 V1 133.55(7) . . ? Cl2 V2 V1 93.83(3) . . ? Cl1 V2 V1 131.59(3) . . ? O5 V3 O2 77.14(8) . . ? O5 V3 N3 88.32(9) . . ? O2 V3 N3 98.46(9) . . ? O5 V3 N4 93.05(9) . . ? O2 V3 N4 168.76(9) . . ? N3 V3 N4 75.49(10) . . ? O5 V3 Cl4 101.45(7) . . ? O2 V3 Cl4 93.52(6) . . ? N3 V3 Cl4 166.00(7) . . ? N4 V3 Cl4 93.81(7) . . ? O5 V3 Cl3 165.35(7) . . ? O2 V3 Cl3 93.57(6) . . ? N3 V3 Cl3 81.80(7) . . ? N4 V3 Cl3 94.90(7) . . ? Cl4 V3 Cl3 90.29(3) . . ? O5 V3 V1 39.28(6) . . ? O2 V3 V1 38.04(6) . . ? N3 V3 V1 97.23(7) . . ? N4 V3 V1 132.32(7) . . ? Cl4 V3 V1 96.67(3) . . ? Cl3 V3 V1 131.28(3) . . ? O6 V4 O3 77.04(8) . . ? O6 V4 N6 88.55(9) . . ? O3 V4 N6 98.64(9) . . ? O6 V4 N5 97.03(9) . . ? O3 V4 N5 172.13(10) . . ? N6 V4 N5 75.84(10) . . ? O6 V4 Cl6 98.83(7) . . ? O3 V4 Cl6 93.87(7) . . ? N6 V4 Cl6 166.65(8) . . ? N5 V4 Cl6 92.14(8) . . ? O6 V4 Cl5 165.07(7) . . ? O3 V4 Cl5 92.39(7) . . ? N6 V4 Cl5 82.58(8) . . ? N5 V4 Cl5 92.43(7) . . ? Cl6 V4 Cl5 92.31(3) . . ? O6 V4 V1 39.45(6) . . ? O3 V4 V1 37.66(6) . . ? N6 V4 V1 96.51(7) . . ? N5 V4 V1 136.44(7) . . ? Cl6 V4 V1 96.23(3) . . ? Cl5 V4 V1 129.64(3) . . ? C1 O1 V1 117.53(18) . . ? C1 O1 V2 129.19(18) . . ? V1 O1 V2 101.44(9) . . ? C2 O2 V1 118.09(17) . . ? C2 O2 V3 129.40(18) . . ? V1 O2 V3 102.33(9) . . ? C3 O3 V1 117.33(18) . . ? C3 O3 V4 130.45(18) . . ? V1 O3 V4 103.37(9) . . ? C6 O4 V2 133.53(18) . . ? C6 O4 V1 118.75(17) . . ? V2 O4 V1 102.19(9) . . ? C7 O5 V3 133.10(18) . . ? C7 O5 V1 118.51(17) . . ? V3 O5 V1 102.73(9) . . ? C8 O6 V4 133.55(18) . . ? C8 O6 V1 117.57(17) . . ? V4 O6 V1 102.52(9) . . ? C15 N1 C11 119.4(3) . . ? C15 N1 V2 122.1(2) . . ? C11 N1 V2 118.5(2) . . ? C20 N2 C16 118.3(3) . . ? C20 N2 V2 125.1(2) . . ? C16 N2 V2 116.5(2) . . ? C25 N3 C21 118.5(3) . . ? C25 N3 V3 123.2(2) . . ? C21 N3 V3 117.6(2) . . ? C30 N4 C26 118.0(3) . . ? C30 N4 V3 124.9(2) . . ? C26 N4 V3 117.0(2) . . ? C35 N5 C31 117.9(3) . . ? C35 N5 V4 125.8(2) . . ? C31 N5 V4 116.1(2) . . ? C40 N6 C36 118.9(3) . . ? C40 N6 V4 123.0(2) . . ? C36 N6 V4 117.9(2) . . ? O1 C1 C4 113.1(2) . . ? O1 C1 H1A 109.0 . . ? C4 C1 H1A 109.0 . . ? O1 C1 H1B 109.0 . . ? C4 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? O2 C2 C4 112.7(2) . . ? O2 C2 H2A 109.1 . . ? C4 C2 H2A 109.1 . . ? O2 C2 H2B 109.1 . . ? C4 C2 H2B 109.1 . . ? H2A C2 H2B 107.8 . . ? O3 C3 C4 113.6(3) . . ? O3 C3 H3A 108.8 . . ? C4 C3 H3A 108.8 . . ? O3 C3 H3B 108.8 . . ? C4 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C5 C4 C1 107.0(3) . . ? C5 C4 C3 107.2(3) . . ? C1 C4 C3 111.4(3) . . ? C5 C4 C2 106.8(3) . . ? C1 C4 C2 112.4(3) . . ? C3 C4 C2 111.7(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O4 C6 C9 113.4(2) . . ? O4 C6 H6A 108.9 . . ? C9 C6 H6A 108.9 . . ? O4 C6 H6B 108.9 . . ? C9 C6 H6B 108.9 . . ? H6A C6 H6B 107.7 . . ? O5 C7 C9 113.5(2) . . ? O5 C7 H7A 108.9 . . ? C9 C7 H7A 108.9 . . ? O5 C7 H7B 108.9 . . ? C9 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? O6 C8 C9 114.1(2) . . ? O6 C8 H8A 108.7 . . ? C9 C8 H8A 108.7 . . ? O6 C8 H8B 108.7 . . ? C9 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C10 C9 C7 106.9(3) . . ? C10 C9 C8 107.2(3) . . ? C7 C9 C8 111.7(3) . . ? C10 C9 C6 106.7(3) . . ? C7 C9 C6 112.1(3) . . ? C8 C9 C6 111.9(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 121.1(3) . . ? N1 C11 C16 114.1(3) . . ? C12 C11 C16 124.7(3) . . ? C13 C12 C11 119.2(3) . . ? C13 C12 H12 120.4 . . ? C11 C12 H12 120.4 . . ? C12 C13 C14 119.3(3) . . ? C12 C13 H13 120.3 . . ? C14 C13 H13 120.3 . . ? C15 C14 C13 119.1(3) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? N1 C15 C14 121.8(3) . . ? N1 C15 H15 119.1 . . ? C14 C15 H15 119.1 . . ? N2 C16 C17 121.8(3) . . ? N2 C16 C11 115.2(3) . . ? C17 C16 C11 123.0(3) . . ? C16 C17 C18 118.7(3) . . ? C16 C17 H17 120.6 . . ? C18 C17 H17 120.6 . . ? C19 C18 C17 119.2(3) . . ? C19 C18 H18 120.4 . . ? C17 C18 H18 120.4 . . ? C20 C19 C18 119.2(3) . . ? C20 C19 H19 120.4 . . ? C18 C19 H19 120.4 . . ? N2 C20 C19 122.7(3) . . ? N2 C20 H20 118.6 . . ? C19 C20 H20 118.6 . . ? N3 C21 C22 122.0(3) . . ? N3 C21 C26 114.4(3) . . ? C22 C21 C26 123.6(3) . . ? C23 C22 C21 118.7(3) . . ? C23 C22 H22 120.7 . . ? C21 C22 H22 120.7 . . ? C24 C23 C22 119.2(3) . . ? C24 C23 H23 120.4 . . ? C22 C23 H23 120.4 . . ? C25 C24 C23 119.3(3) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? N3 C25 C24 122.4(3) . . ? N3 C25 H25 118.8 . . ? C24 C25 H25 118.8 . . ? N4 C26 C27 121.8(3) . . ? N4 C26 C21 114.8(3) . . ? C27 C26 C21 123.4(3) . . ? C28 C27 C26 119.3(3) . . ? C28 C27 H27 120.3 . . ? C26 C27 H27 120.3 . . ? C27 C28 C29 119.1(3) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C30 C29 C28 119.4(3) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? N4 C30 C29 122.4(3) . . ? N4 C30 H30 118.8 . . ? C29 C30 H30 118.8 . . ? N5 C31 C32 121.6(3) . . ? N5 C31 C36 115.1(3) . . ? C32 C31 C36 123.3(3) . . ? C33 C32 C31 119.4(3) . . ? C33 C32 H32 120.3 . . ? C31 C32 H32 120.3 . . ? C34 C33 C32 119.1(3) . . ? C34 C33 H33 120.5 . . ? C32 C33 H33 120.5 . . ? C35 C34 C33 119.1(3) . . ? C35 C34 H34 120.4 . . ? C33 C34 H34 120.4 . . ? N5 C35 C34 122.9(3) . . ? N5 C35 H35 118.6 . . ? C34 C35 H35 118.6 . . ? N6 C36 C37 121.1(3) . . ? N6 C36 C31 114.8(3) . . ? C37 C36 C31 124.1(3) . . ? C36 C37 C38 119.3(3) . . ? C36 C37 H37 120.4 . . ? C38 C37 H37 120.4 . . ? C39 C38 C37 119.5(3) . . ? C39 C38 H38 120.3 . . ? C37 C38 H38 120.3 . . ? C38 C39 C40 119.0(3) . . ? C38 C39 H39 120.5 . . ? C40 C39 H39 120.5 . . ? N6 C40 C39 122.2(3) . . ? N6 C40 H40 118.9 . . ? C39 C40 H40 118.9 . . ? N7 C41 C42 178.4(5) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N8 C43 C44 177.3(6) . 2_567 ? N9X C45X C46X 180(2) . . ? N9Y C45Y C46Y 178.5(11) . . ? C45Y C46Y H46D 109.5 . . ? C45Y C46Y H46E 109.5 . . ? H46D C46Y H46E 109.5 . . ? C45Y C46Y H46F 109.5 . . ? H46D C46Y H46F 109.5 . . ? H46E C46Y H46F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 V1 V2 O4 103.34(11) . . . . ? O3 V1 V2 O4 -157.92(12) . . . . ? O1 V1 V2 O4 -171.81(13) . . . . ? O5 V1 V2 O4 23.71(12) . . . . ? O6 V1 V2 O4 -75.00(11) . . . . ? V3 V1 V2 O4 68.98(9) . . . . ? V4 V1 V2 O4 -110.76(9) . . . . ? O2 V1 V2 O1 -84.84(11) . . . . ? O3 V1 V2 O1 13.89(12) . . . . ? O4 V1 V2 O1 171.81(13) . . . . ? O5 V1 V2 O1 -164.48(12) . . . . ? O6 V1 V2 O1 96.81(11) . . . . ? V3 V1 V2 O1 -119.20(9) . . . . ? V4 V1 V2 O1 61.05(9) . . . . ? O2 V1 V2 N1 -178.87(9) . . . . ? O3 V1 V2 N1 -80.14(11) . . . . ? O1 V1 V2 N1 -94.03(12) . . . . ? O4 V1 V2 N1 77.78(12) . . . . ? O5 V1 V2 N1 101.50(10) . . . . ? O6 V1 V2 N1 2.78(9) . . . . ? V3 V1 V2 N1 146.77(7) . . . . ? V4 V1 V2 N1 -32.97(8) . . . . ? O2 V1 V2 N2 105.79(11) . . . . ? O3 V1 V2 N2 -155.47(12) . . . . ? O1 V1 V2 N2 -169.37(14) . . . . ? O4 V1 V2 N2 2.45(13) . . . . ? O5 V1 V2 N2 26.16(12) . . . . ? O6 V1 V2 N2 -72.55(11) . . . . ? V3 V1 V2 N2 71.43(10) . . . . ? V4 V1 V2 N2 -108.31(10) . . . . ? O2 V1 V2 Cl2 4.72(6) . . . . ? O3 V1 V2 Cl2 103.46(8) . . . . ? O1 V1 V2 Cl2 89.56(9) . . . . ? O4 V1 V2 Cl2 -98.62(10) . . . . ? O5 V1 V2 Cl2 -74.91(8) . . . . ? O6 V1 V2 Cl2 -173.62(6) . . . . ? V3 V1 V2 Cl2 -29.64(3) . . . . ? V4 V1 V2 Cl2 150.62(3) . . . . ? O2 V1 V2 Cl1 -91.48(7) . . . . ? O3 V1 V2 Cl1 7.25(9) . . . . ? O1 V1 V2 Cl1 -6.64(10) . . . . ? O4 V1 V2 Cl1 165.17(10) . . . . ? O5 V1 V2 Cl1 -171.12(8) . . . . ? O6 V1 V2 Cl1 90.17(7) . . . . ? V3 V1 V2 Cl1 -125.84(4) . . . . ? V4 V1 V2 Cl1 54.41(5) . . . . ? O2 V1 V3 O5 -172.86(13) . . . . ? O3 V1 V3 O5 102.96(11) . . . . ? O1 V1 V3 O5 -159.16(13) . . . . ? O4 V1 V3 O5 -74.96(11) . . . . ? O6 V1 V3 O5 23.71(12) . . . . ? V2 V1 V3 O5 -111.46(10) . . . . ? V4 V1 V3 O5 68.29(10) . . . . ? O3 V1 V3 O2 -84.18(11) . . . . ? O1 V1 V3 O2 13.70(12) . . . . ? O4 V1 V3 O2 97.90(11) . . . . ? O5 V1 V3 O2 172.86(13) . . . . ? O6 V1 V3 O2 -163.43(12) . . . . ? V2 V1 V3 O2 61.41(9) . . . . ? V4 V1 V3 O2 -118.85(10) . . . . ? O2 V1 V3 N3 -94.51(12) . . . . ? O3 V1 V3 N3 -178.69(9) . . . . ? O1 V1 V3 N3 -80.81(11) . . . . ? O4 V1 V3 N3 3.39(9) . . . . ? O5 V1 V3 N3 78.35(12) . . . . ? O6 V1 V3 N3 102.06(10) . . . . ? V2 V1 V3 N3 -33.10(8) . . . . ? V4 V1 V3 N3 146.64(7) . . . . ? O2 V1 V3 N4 -171.45(14) . . . . ? O3 V1 V3 N4 104.37(11) . . . . ? O1 V1 V3 N4 -157.75(12) . . . . ? O4 V1 V3 N4 -73.55(12) . . . . ? O5 V1 V3 N4 1.41(13) . . . . ? O6 V1 V3 N4 25.12(13) . . . . ? V2 V1 V3 N4 -110.04(10) . . . . ? V4 V1 V3 N4 69.70(10) . . . . ? O2 V1 V3 Cl4 87.19(10) . . . . ? O3 V1 V3 Cl4 3.01(7) . . . . ? O1 V1 V3 Cl4 100.89(9) . . . . ? O4 V1 V3 Cl4 -174.91(6) . . . . ? O5 V1 V3 Cl4 -99.95(10) . . . . ? O6 V1 V3 Cl4 -76.24(8) . . . . ? V2 V1 V3 Cl4 148.59(3) . . . . ? V4 V1 V3 Cl4 -31.66(4) . . . . ? O2 V1 V3 Cl3 -9.09(10) . . . . ? O3 V1 V3 Cl3 -93.27(7) . . . . ? O1 V1 V3 Cl3 4.61(9) . . . . ? O4 V1 V3 Cl3 88.81(7) . . . . ? O5 V1 V3 Cl3 163.77(11) . . . . ? O6 V1 V3 Cl3 -172.52(8) . . . . ? V2 V1 V3 Cl3 52.31(5) . . . . ? V4 V1 V3 Cl3 -127.94(4) . . . . ? O2 V1 V4 O6 -158.34(13) . . . . ? O3 V1 V4 O6 -175.40(14) . . . . ? O1 V1 V4 O6 102.41(11) . . . . ? O4 V1 V4 O6 21.67(12) . . . . ? O5 V1 V4 O6 -76.13(11) . . . . ? V2 V1 V4 O6 68.08(10) . . . . ? V3 V1 V4 O6 -111.67(10) . . . . ? O2 V1 V4 O3 17.07(13) . . . . ? O1 V1 V4 O3 -82.18(12) . . . . ? O4 V1 V4 O3 -162.93(12) . . . . ? O5 V1 V4 O3 99.28(11) . . . . ? O6 V1 V4 O3 175.40(14) . . . . ? V2 V1 V4 O3 -116.52(10) . . . . ? V3 V1 V4 O3 63.73(10) . . . . ? O2 V1 V4 N6 -78.64(11) . . . . ? O3 V1 V4 N6 -95.71(12) . . . . ? O1 V1 V4 N6 -177.89(9) . . . . ? O4 V1 V4 N6 101.36(11) . . . . ? O5 V1 V4 N6 3.57(9) . . . . ? O6 V1 V4 N6 79.70(12) . . . . ? V2 V1 V4 N6 147.77(8) . . . . ? V3 V1 V4 N6 -31.97(8) . . . . ? O2 V1 V4 N5 -154.91(13) . . . . ? O3 V1 V4 N5 -171.98(14) . . . . ? O1 V1 V4 N5 105.84(12) . . . . ? O4 V1 V4 N5 25.09(13) . . . . ? O5 V1 V4 N5 -72.70(12) . . . . ? O6 V1 V4 N5 3.43(14) . . . . ? V2 V1 V4 N5 71.50(11) . . . . ? V3 V1 V4 N5 -108.24(11) . . . . ? O2 V1 V4 Cl6 105.33(8) . . . . ? O3 V1 V4 Cl6 88.27(10) . . . . ? O1 V1 V4 Cl6 6.08(7) . . . . ? O4 V1 V4 Cl6 -74.66(8) . . . . ? O5 V1 V4 Cl6 -172.46(6) . . . . ? O6 V1 V4 Cl6 -96.33(10) . . . . ? V2 V1 V4 Cl6 -28.25(3) . . . . ? V3 V1 V4 Cl6 152.00(3) . . . . ? O2 V1 V4 Cl5 7.10(9) . . . . ? O3 V1 V4 Cl5 -9.96(10) . . . . ? O1 V1 V4 Cl5 -92.15(7) . . . . ? O4 V1 V4 Cl5 -172.89(8) . . . . ? O5 V1 V4 Cl5 89.31(7) . . . . ? O6 V1 V4 Cl5 165.44(10) . . . . ? V2 V1 V4 Cl5 -126.48(4) . . . . ? V3 V1 V4 Cl5 53.77(5) . . . . ? O2 V1 O1 C1 -47.8(2) . . . . ? O3 V1 O1 C1 44.3(2) . . . . ? O4 V1 O1 C1 -151.6(2) . . . . ? O5 V1 O1 C1 -101.9(3) . . . . ? O6 V1 O1 C1 121.1(2) . . . . ? V2 V1 O1 C1 -146.4(2) . . . . ? V3 V1 O1 C1 -56.5(2) . . . . ? V4 V1 O1 C1 82.82(19) . . . . ? O2 V1 O1 V2 98.52(9) . . . . ? O3 V1 O1 V2 -169.38(9) . . . . ? O4 V1 O1 V2 -5.21(8) . . . . ? O5 V1 O1 V2 44.5(3) . . . . ? O6 V1 O1 V2 -92.59(9) . . . . ? V3 V1 O1 V2 89.82(9) . . . . ? V4 V1 O1 V2 -130.83(7) . . . . ? O4 V2 O1 C1 145.9(2) . . . . ? N1 V2 O1 C1 -129.1(2) . . . . ? N2 V2 O1 C1 -171.9(5) . . . . ? Cl2 V2 O1 C1 47.9(2) . . . . ? Cl1 V2 O1 C1 -44.3(2) . . . . ? V1 V2 O1 C1 140.7(3) . . . . ? O4 V2 O1 V1 5.28(8) . . . . ? N1 V2 O1 V1 90.29(10) . . . . ? N2 V2 O1 V1 47.4(5) . . . . ? Cl2 V2 O1 V1 -92.74(8) . . . . ? Cl1 V2 O1 V1 175.03(7) . . . . ? O3 V1 O2 C2 -49.3(2) . . . . ? O1 V1 O2 C2 41.7(2) . . . . ? O4 V1 O2 C2 120.0(2) . . . . ? O5 V1 O2 C2 -153.0(2) . . . . ? O6 V1 O2 C2 -103.6(3) . . . . ? V2 V1 O2 C2 81.3(2) . . . . ? V3 V1 O2 C2 -148.6(2) . . . . ? V4 V1 O2 C2 -60.0(2) . . . . ? O3 V1 O2 V3 99.24(10) . . . . ? O1 V1 O2 V3 -169.70(9) . . . . ? O4 V1 O2 V3 -91.41(9) . . . . ? O5 V1 O2 V3 -4.49(8) . . . . ? O6 V1 O2 V3 44.9(3) . . . . ? V2 V1 O2 V3 -130.14(7) . . . . ? V4 V1 O2 V3 88.60(9) . . . . ? O5 V3 O2 C2 148.1(2) . . . . ? N3 V3 O2 C2 -125.6(2) . . . . ? N4 V3 O2 C2 177.8(4) . . . . ? Cl4 V3 O2 C2 47.1(2) . . . . ? Cl3 V3 O2 C2 -43.4(2) . . . . ? V1 V3 O2 C2 143.4(3) . . . . ? O5 V3 O2 V1 4.63(9) . . . . ? N3 V3 O2 V1 90.93(10) . . . . ? N4 V3 O2 V1 34.3(5) . . . . ? Cl4 V3 O2 V1 -96.32(8) . . . . ? Cl3 V3 O2 V1 173.16(7) . . . . ? O2 V1 O3 C3 42.2(2) . . . . ? O1 V1 O3 C3 -50.1(2) . . . . ? O4 V1 O3 C3 -104.6(3) . . . . ? O5 V1 O3 C3 119.7(2) . . . . ? O6 V1 O3 C3 -153.8(2) . . . . ? V2 V1 O3 C3 -58.9(2) . . . . ? V3 V1 O3 C3 81.6(2) . . . . ? V4 V1 O3 C3 -150.9(2) . . . . ? O2 V1 O3 V4 -166.96(10) . . . . ? O1 V1 O3 V4 100.79(10) . . . . ? O4 V1 O3 V4 46.2(3) . . . . ? O5 V1 O3 V4 -89.39(10) . . . . ? O6 V1 O3 V4 -2.91(9) . . . . ? V2 V1 O3 V4 91.96(9) . . . . ? V3 V1 O3 V4 -127.55(7) . . . . ? O6 V4 O3 C3 148.4(3) . . . . ? N6 V4 O3 C3 -125.2(2) . . . . ? N5 V4 O3 C3 -170.0(6) . . . . ? Cl6 V4 O3 C3 50.2(2) . . . . ? Cl5 V4 O3 C3 -42.3(2) . . . . ? V1 V4 O3 C3 145.4(3) . . . . ? O6 V4 O3 V1 2.99(9) . . . . ? N6 V4 O3 V1 89.48(11) . . . . ? N5 V4 O3 V1 44.6(7) . . . . ? Cl6 V4 O3 V1 -95.18(8) . . . . ? Cl5 V4 O3 V1 172.34(8) . . . . ? O1 V2 O4 C6 146.9(3) . . . . ? N1 V2 O4 C6 49.2(3) . . . . ? N2 V2 O4 C6 -26.1(3) . . . . ? Cl2 V2 O4 C6 -122.1(2) . . . . ? Cl1 V2 O4 C6 98.6(4) . . . . ? V1 V2 O4 C6 152.1(3) . . . . ? O1 V2 O4 V1 -5.24(8) . . . . ? N1 V2 O4 V1 -102.92(10) . . . . ? N2 V2 O4 V1 -178.22(10) . . . . ? Cl2 V2 O4 V1 85.72(8) . . . . ? Cl1 V2 O4 V1 -53.6(3) . . . . ? O2 V1 O4 C6 118.7(2) . . . . ? O3 V1 O4 C6 -95.6(3) . . . . ? O1 V1 O4 C6 -151.9(2) . . . . ? O5 V1 O4 C6 41.7(2) . . . . ? O6 V1 O4 C6 -48.1(2) . . . . ? V2 V1 O4 C6 -157.3(2) . . . . ? V3 V1 O4 C6 78.1(2) . . . . ? V4 V1 O4 C6 -61.3(2) . . . . ? O2 V1 O4 V2 -84.01(10) . . . . ? O3 V1 O4 V2 61.7(3) . . . . ? O1 V1 O4 V2 5.34(9) . . . . ? O5 V1 O4 V2 -161.08(9) . . . . ? O6 V1 O4 V2 109.14(9) . . . . ? V3 V1 O4 V2 -124.61(7) . . . . ? V4 V1 O4 V2 95.99(8) . . . . ? O2 V3 O5 C7 147.3(3) . . . . ? N3 V3 O5 C7 48.2(3) . . . . ? N4 V3 O5 C7 -27.1(3) . . . . ? Cl4 V3 O5 C7 -121.6(2) . . . . ? Cl3 V3 O5 C7 95.7(3) . . . . ? V1 V3 O5 C7 151.8(3) . . . . ? O2 V3 O5 V1 -4.50(8) . . . . ? N3 V3 O5 V1 -103.58(10) . . . . ? N4 V3 O5 V1 -178.95(10) . . . . ? Cl4 V3 O5 V1 86.53(8) . . . . ? Cl3 V3 O5 V1 -56.1(3) . . . . ? O2 V1 O5 C7 -152.2(2) . . . . ? O3 V1 O5 C7 118.7(2) . . . . ? O1 V1 O5 C7 -96.3(3) . . . . ? O4 V1 O5 C7 -48.0(2) . . . . ? O6 V1 O5 C7 42.2(2) . . . . ? V2 V1 O5 C7 -62.6(2) . . . . ? V3 V1 O5 C7 -156.9(2) . . . . ? V4 V1 O5 C7 79.0(2) . . . . ? O2 V1 O5 V3 4.66(9) . . . . ? O3 V1 O5 V3 -84.37(10) . . . . ? O1 V1 O5 V3 60.6(3) . . . . ? O4 V1 O5 V3 108.87(10) . . . . ? O6 V1 O5 V3 -160.85(10) . . . . ? V2 V1 O5 V3 94.34(9) . . . . ? V4 V1 O5 V3 -124.12(7) . . . . ? O3 V4 O6 C8 147.0(3) . . . . ? N6 V4 O6 C8 47.8(3) . . . . ? N5 V4 O6 C8 -27.7(3) . . . . ? Cl6 V4 O6 C8 -121.0(2) . . . . ? Cl5 V4 O6 C8 101.2(3) . . . . ? V1 V4 O6 C8 149.9(3) . . . . ? O3 V4 O6 V1 -2.88(9) . . . . ? N6 V4 O6 V1 -102.08(10) . . . . ? N5 V4 O6 V1 -177.62(10) . . . . ? Cl6 V4 O6 V1 89.09(8) . . . . ? Cl5 V4 O6 V1 -48.7(3) . . . . ? O2 V1 O6 C8 -96.4(3) . . . . ? O3 V1 O6 C8 -152.8(2) . . . . ? O1 V1 O6 C8 119.3(2) . . . . ? O4 V1 O6 C8 41.5(2) . . . . ? O5 V1 O6 C8 -48.6(2) . . . . ? V2 V1 O6 C8 78.6(2) . . . . ? V3 V1 O6 C8 -62.9(2) . . . . ? V4 V1 O6 C8 -155.8(2) . . . . ? O2 V1 O6 V4 59.4(3) . . . . ? O3 V1 O6 V4 2.97(9) . . . . ? O1 V1 O6 V4 -84.86(10) . . . . ? O4 V1 O6 V4 -162.69(9) . . . . ? O5 V1 O6 V4 107.24(10) . . . . ? V2 V1 O6 V4 -125.60(7) . . . . ? V3 V1 O6 V4 92.91(9) . . . . ? O4 V2 N1 C15 84.0(2) . . . . ? O1 V2 N1 C15 6.8(2) . . . . ? N2 V2 N1 C15 179.5(3) . . . . ? Cl2 V2 N1 C15 -155.4(4) . . . . ? Cl1 V2 N1 C15 -85.5(2) . . . . ? V1 V2 N1 C15 45.8(2) . . . . ? O4 V2 N1 C11 -96.7(2) . . . . ? O1 V2 N1 C11 -174.0(2) . . . . ? N2 V2 N1 C11 -1.3(2) . . . . ? Cl2 V2 N1 C11 23.9(6) . . . . ? Cl1 V2 N1 C11 93.7(2) . . . . ? V1 V2 N1 C11 -134.9(2) . . . . ? O4 V2 N2 C20 -94.6(3) . . . . ? O1 V2 N2 C20 -135.7(5) . . . . ? N1 V2 N2 C20 -179.9(3) . . . . ? Cl2 V2 N2 C20 4.3(3) . . . . ? Cl1 V2 N2 C20 96.7(3) . . . . ? V1 V2 N2 C20 -96.1(3) . . . . ? O4 V2 N2 C16 86.8(2) . . . . ? O1 V2 N2 C16 45.7(6) . . . . ? N1 V2 N2 C16 1.5(2) . . . . ? Cl2 V2 N2 C16 -174.3(2) . . . . ? Cl1 V2 N2 C16 -81.9(2) . . . . ? V1 V2 N2 C16 85.3(2) . . . . ? O5 V3 N3 C25 90.0(3) . . . . ? O2 V3 N3 C25 13.3(3) . . . . ? N4 V3 N3 C25 -176.4(3) . . . . ? Cl4 V3 N3 C25 -135.3(3) . . . . ? Cl3 V3 N3 C25 -79.1(3) . . . . ? V1 V3 N3 C25 51.7(3) . . . . ? O5 V3 N3 C21 -100.1(2) . . . . ? O2 V3 N3 C21 -176.8(2) . . . . ? N4 V3 N3 C21 -6.5(2) . . . . ? Cl4 V3 N3 C21 34.6(5) . . . . ? Cl3 V3 N3 C21 90.7(2) . . . . ? V1 V3 N3 C21 -138.4(2) . . . . ? O5 V3 N4 C30 -87.7(3) . . . . ? O2 V3 N4 C30 -116.6(5) . . . . ? N3 V3 N4 C30 -175.2(3) . . . . ? Cl4 V3 N4 C30 14.0(3) . . . . ? Cl3 V3 N4 C30 104.6(3) . . . . ? V1 V3 N4 C30 -88.6(3) . . . . ? O5 V3 N4 C26 89.5(2) . . . . ? O2 V3 N4 C26 60.6(6) . . . . ? N3 V3 N4 C26 2.0(2) . . . . ? Cl4 V3 N4 C26 -168.8(2) . . . . ? Cl3 V3 N4 C26 -78.2(2) . . . . ? V1 V3 N4 C26 88.6(2) . . . . ? O6 V4 N5 C35 -94.5(3) . . . . ? O3 V4 N5 C35 -135.2(6) . . . . ? N6 V4 N5 C35 178.8(3) . . . . ? Cl6 V4 N5 C35 4.7(3) . . . . ? Cl5 V4 N5 C35 97.1(3) . . . . ? V1 V4 N5 C35 -96.7(3) . . . . ? O6 V4 N5 C31 91.3(2) . . . . ? O3 V4 N5 C31 50.6(8) . . . . ? N6 V4 N5 C31 4.6(2) . . . . ? Cl6 V4 N5 C31 -169.5(2) . . . . ? Cl5 V4 N5 C31 -77.1(2) . . . . ? V1 V4 N5 C31 89.1(2) . . . . ? O6 V4 N6 C40 84.1(3) . . . . ? O3 V4 N6 C40 7.4(3) . . . . ? N5 V4 N6 C40 -178.3(3) . . . . ? Cl6 V4 N6 C40 -152.0(3) . . . . ? Cl5 V4 N6 C40 -83.9(2) . . . . ? V1 V4 N6 C40 45.3(2) . . . . ? O6 V4 N6 C36 -101.3(2) . . . . ? O3 V4 N6 C36 -177.9(2) . . . . ? N5 V4 N6 C36 -3.6(2) . . . . ? Cl6 V4 N6 C36 22.7(5) . . . . ? Cl5 V4 N6 C36 90.8(2) . . . . ? V1 V4 N6 C36 -140.0(2) . . . . ? V1 O1 C1 C4 4.5(3) . . . . ? V2 O1 C1 C4 -131.1(2) . . . . ? V1 O2 C2 C4 5.8(3) . . . . ? V3 O2 C2 C4 -132.9(2) . . . . ? V1 O3 C3 C4 6.2(3) . . . . ? V4 O3 C3 C4 -135.3(2) . . . . ? O1 C1 C4 C5 177.3(2) . . . . ? O1 C1 C4 C3 -65.8(3) . . . . ? O1 C1 C4 C2 60.4(3) . . . . ? O3 C3 C4 C5 176.6(3) . . . . ? O3 C3 C4 C1 59.8(3) . . . . ? O3 C3 C4 C2 -66.8(3) . . . . ? O2 C2 C4 C5 176.0(3) . . . . ? O2 C2 C4 C1 -66.9(3) . . . . ? O2 C2 C4 C3 59.1(3) . . . . ? V2 O4 C6 C9 -143.1(2) . . . . ? V1 O4 C6 C9 5.5(3) . . . . ? V3 O5 C7 C9 -142.9(2) . . . . ? V1 O5 C7 C9 5.5(3) . . . . ? V4 O6 C8 C9 -140.6(2) . . . . ? V1 O6 C8 C9 5.9(3) . . . . ? O5 C7 C9 C10 176.1(3) . . . . ? O5 C7 C9 C8 -66.9(3) . . . . ? O5 C7 C9 C6 59.6(3) . . . . ? O6 C8 C9 C10 176.6(3) . . . . ? O6 C8 C9 C7 59.8(3) . . . . ? O6 C8 C9 C6 -66.7(3) . . . . ? O4 C6 C9 C10 176.9(2) . . . . ? O4 C6 C9 C7 -66.4(3) . . . . ? O4 C6 C9 C8 59.9(3) . . . . ? C15 N1 C11 C12 0.1(5) . . . . ? V2 N1 C11 C12 -179.2(2) . . . . ? C15 N1 C11 C16 -179.8(3) . . . . ? V2 N1 C11 C16 0.9(3) . . . . ? N1 C11 C12 C13 -0.3(5) . . . . ? C16 C11 C12 C13 179.6(3) . . . . ? C11 C12 C13 C14 0.1(5) . . . . ? C12 C13 C14 C15 0.3(5) . . . . ? C11 N1 C15 C14 0.3(5) . . . . ? V2 N1 C15 C14 179.5(3) . . . . ? C13 C14 C15 N1 -0.5(5) . . . . ? C20 N2 C16 C17 0.2(5) . . . . ? V2 N2 C16 C17 178.9(2) . . . . ? C20 N2 C16 C11 179.8(3) . . . . ? V2 N2 C16 C11 -1.5(3) . . . . ? N1 C11 C16 N2 0.4(4) . . . . ? C12 C11 C16 N2 -179.5(3) . . . . ? N1 C11 C16 C17 180.0(3) . . . . ? C12 C11 C16 C17 0.0(5) . . . . ? N2 C16 C17 C18 0.2(5) . . . . ? C11 C16 C17 C18 -179.3(3) . . . . ? C16 C17 C18 C19 -0.5(6) . . . . ? C17 C18 C19 C20 0.5(6) . . . . ? C16 N2 C20 C19 -0.3(5) . . . . ? V2 N2 C20 C19 -178.9(3) . . . . ? C18 C19 C20 N2 0.0(6) . . . . ? C25 N3 C21 C22 1.6(5) . . . . ? V3 N3 C21 C22 -168.8(3) . . . . ? C25 N3 C21 C26 -180.0(3) . . . . ? V3 N3 C21 C26 9.6(4) . . . . ? N3 C21 C22 C23 -0.8(5) . . . . ? C26 C21 C22 C23 -179.1(3) . . . . ? C21 C22 C23 C24 -0.9(6) . . . . ? C22 C23 C24 C25 1.7(6) . . . . ? C21 N3 C25 C24 -0.7(5) . . . . ? V3 N3 C25 C24 169.1(3) . . . . ? C23 C24 C25 N3 -0.9(6) . . . . ? C30 N4 C26 C27 -0.3(5) . . . . ? V3 N4 C26 C27 -177.7(2) . . . . ? C30 N4 C26 C21 179.6(3) . . . . ? V3 N4 C26 C21 2.2(3) . . . . ? N3 C21 C26 N4 -7.7(4) . . . . ? C22 C21 C26 N4 170.7(3) . . . . ? N3 C21 C26 C27 172.3(3) . . . . ? C22 C21 C26 C27 -9.4(5) . . . . ? N4 C26 C27 C28 0.5(5) . . . . ? C21 C26 C27 C28 -179.4(3) . . . . ? C26 C27 C28 C29 -0.6(5) . . . . ? C27 C28 C29 C30 0.5(6) . . . . ? C26 N4 C30 C29 0.2(5) . . . . ? V3 N4 C30 C29 177.4(3) . . . . ? C28 C29 C30 N4 -0.3(5) . . . . ? C35 N5 C31 C32 -0.3(5) . . . . ? V4 N5 C31 C32 174.3(2) . . . . ? C35 N5 C31 C36 -179.6(3) . . . . ? V4 N5 C31 C36 -5.0(3) . . . . ? N5 C31 C32 C33 -0.2(5) . . . . ? C36 C31 C32 C33 179.0(3) . . . . ? C31 C32 C33 C34 0.3(5) . . . . ? C32 C33 C34 C35 0.2(5) . . . . ? C31 N5 C35 C34 0.9(5) . . . . ? V4 N5 C35 C34 -173.2(2) . . . . ? C33 C34 C35 N5 -0.9(5) . . . . ? C40 N6 C36 C37 -1.0(5) . . . . ? V4 N6 C36 C37 -175.9(2) . . . . ? C40 N6 C36 C31 177.1(3) . . . . ? V4 N6 C36 C31 2.2(3) . . . . ? N5 C31 C36 N6 1.9(4) . . . . ? C32 C31 C36 N6 -177.4(3) . . . . ? N5 C31 C36 C37 179.9(3) . . . . ? C32 C31 C36 C37 0.7(5) . . . . ? N6 C36 C37 C38 -0.4(5) . . . . ? C31 C36 C37 C38 -178.4(3) . . . . ? C36 C37 C38 C39 1.7(5) . . . . ? C37 C38 C39 C40 -1.6(5) . . . . ? C36 N6 C40 C39 1.1(5) . . . . ? V4 N6 C40 C39 175.8(2) . . . . ? C38 C39 C40 N6 0.2(5) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.971 _refine_diff_density_min -0.491 _refine_diff_density_rms 0.127 # Attachment '5.cif' data_oejlm244profp-1 _database_code_depnum_ccdc_archive 'CCDC 736084' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common sy _chemical_melting_point ? _chemical_formula_moiety '[V4Cl6(tmp)2(bipy)3]2.5MeCN' _chemical_formula_sum 'C47 H53.50 Cl6 N8.50 O6 V4' _chemical_formula_weight 1249.94 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8469(4) _cell_length_b 12.7487(5) _cell_length_c 19.7931(8) _cell_angle_alpha 83.295(3) _cell_angle_beta 78.009(3) _cell_angle_gamma 65.219(4) _cell_volume 2653.43(17) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8586 _cell_measurement_theta_min 2.6935 _cell_measurement_theta_max 31.9250 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.564 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1274 _exptl_absorpt_coefficient_mu 1.040 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.6243 _exptl_absorpt_correction_T_max 0.6243 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcaliber 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27231 _diffrn_reflns_av_R_equivalents 0.0314 _diffrn_reflns_av_sigmaI/netI 0.0763 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 30.51 _reflns_number_total 15797 _reflns_number_gt 10256 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) ; _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 ; The structure was solved by direct methods. Data processing was carried out to 0.80 angstroms as the data was only complete to this resolution. Hydrogen atoms were included in calculated positions. In the acetonitrile molecule N9 C47 C48, the atoms C47 and C48 share the same atomic coordinates. The acetonitrile molecule N8 C45 C46 is disordered over two sites. Geometric and displacement restraints were applied to the anisotropic thermal parameters of the atoms of this molecule. The methyl group C12 is also disordered over two sites and was treated in a similar manner 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^)+(0.0482P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15797 _refine_ls_number_parameters 690 _refine_ls_number_restraints 75 _refine_ls_R_factor_all 0.0649 _refine_ls_R_factor_gt 0.0376 _refine_ls_wR_factor_ref 0.0943 _refine_ls_wR_factor_gt 0.0901 _refine_ls_goodness_of_fit_ref 0.946 _refine_ls_restrained_S_all 0.945 _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 0.76175(3) 0.36970(3) 0.249035(17) 0.00951(7) Uani 1 1 d . . . V2 V 0.69283(3) 0.21490(3) 0.368762(17) 0.01154(8) Uani 1 1 d . . . V3 V 0.64495(3) 0.63410(3) 0.266959(18) 0.01170(8) Uani 1 1 d . . . V4 V 0.94517(3) 0.26390(3) 0.115608(17) 0.01126(8) Uani 1 1 d . . . Cl1 Cl 0.87939(5) 0.04903(4) 0.34445(3) 0.01818(11) Uani 1 1 d . . . Cl2 Cl 0.70906(5) 0.20147(4) 0.48632(3) 0.01655(11) Uani 1 1 d . . . Cl3 Cl 0.63528(5) 0.63012(5) 0.38471(3) 0.02078(12) Uani 1 1 d . . . Cl4 Cl 0.74256(6) 0.76567(5) 0.25115(3) 0.02255(12) Uani 1 1 d . . . Cl5 Cl 1.01589(5) 0.41174(4) 0.09465(3) 0.01673(11) Uani 1 1 d . . . Cl6 Cl 1.15347(5) 0.11945(4) 0.09685(3) 0.01830(11) Uani 1 1 d . . . O1 O 0.77830(13) 0.32354(12) 0.34547(7) 0.0119(3) Uani 1 1 d . . . O2 O 0.81215(12) 0.49555(11) 0.25309(7) 0.0108(3) Uani 1 1 d . . . O3 O 0.93705(13) 0.26090(11) 0.21757(7) 0.0111(3) Uani 1 1 d . . . O4 O 0.66680(13) 0.26768(12) 0.27315(7) 0.0124(3) Uani 1 1 d . . . O5 O 0.59681(12) 0.50909(12) 0.25552(7) 0.0117(3) Uani 1 1 d . . . O6 O 0.76577(13) 0.36064(12) 0.14892(7) 0.0116(3) Uani 1 1 d . . . N1 N 0.57735(17) 0.11785(15) 0.38752(9) 0.0144(4) Uani 1 1 d . . . N2 N 0.50869(16) 0.33846(14) 0.40439(9) 0.0138(4) Uani 1 1 d . . . N3 N 0.45521(16) 0.76119(14) 0.27192(9) 0.0149(4) Uani 1 1 d . . . N4 N 0.62696(16) 0.68507(15) 0.16185(9) 0.0148(4) Uani 1 1 d . . . N5 N 0.88613(17) 0.12840(14) 0.11658(9) 0.0145(4) Uani 1 1 d . . . N6 N 0.92215(16) 0.26087(14) 0.01126(9) 0.0134(4) Uani 1 1 d . . . C1 C 0.88372(19) 0.32566(19) 0.36834(10) 0.0151(4) Uani 1 1 d . . . H1A H 0.9259 0.2524 0.3918 0.018 Uiso 1 1 calc R . . H1B H 0.8532 0.3858 0.4017 0.018 Uiso 1 1 calc R . . C2 C 0.92470(19) 0.47042(18) 0.27839(11) 0.0143(4) Uani 1 1 d . . . H2A H 0.9071 0.5253 0.3133 0.017 Uiso 1 1 calc R . . H2B H 0.9870 0.4803 0.2408 0.017 Uiso 1 1 calc R . . C3 C 1.02960(19) 0.25460(18) 0.25485(11) 0.0153(4) Uani 1 1 d . . . H3A H 1.0994 0.2628 0.2225 0.018 Uiso 1 1 calc R . . H3B H 1.0619 0.1788 0.2774 0.018 Uiso 1 1 calc R . . C4 C 0.98032(18) 0.34714(17) 0.30974(10) 0.0122(4) Uani 1 1 d . . . C5 C 1.09168(19) 0.3340(2) 0.34347(11) 0.0167(4) Uani 1 1 d . . . H5A H 1.0587 0.3835 0.3829 0.020 Uiso 1 1 calc R . . H5B H 1.1294 0.2548 0.3608 0.020 Uiso 1 1 calc R . . C6 C 1.1955(2) 0.3628(2) 0.29670(12) 0.0263(5) Uani 1 1 d . . . H6A H 1.2237 0.3199 0.2553 0.039 Uiso 1 1 calc R . . H6B H 1.2651 0.3426 0.3204 0.039 Uiso 1 1 calc R . . H6C H 1.1630 0.4441 0.2850 0.039 Uiso 1 1 calc R . . C7 C 0.57076(19) 0.28589(18) 0.23463(11) 0.0148(4) Uani 1 1 d . . . H7A H 0.4942 0.2925 0.2667 0.018 Uiso 1 1 calc R . . H7B H 0.5968 0.2186 0.2073 0.018 Uiso 1 1 calc R . . C8 C 0.49854(19) 0.50387(17) 0.22686(11) 0.0140(4) Uani 1 1 d . . . H8A H 0.4671 0.5712 0.1965 0.017 Uiso 1 1 calc R . . H8B H 0.4294 0.5071 0.2640 0.017 Uiso 1 1 calc R . . C9 C 0.65122(19) 0.38240(19) 0.12661(10) 0.0144(4) Uani 1 1 d . . . H9A H 0.6652 0.3197 0.0981 0.017 Uiso 1 1 calc R . . H9B H 0.6283 0.4529 0.0981 0.017 Uiso 1 1 calc R . . C10 C 0.54053(18) 0.39441(17) 0.18597(10) 0.0124(4) Uani 1 1 d . B . C11 C 0.4272(2) 0.4058(2) 0.15430(12) 0.0227(5) Uani 1 1 d D . . H11A H 0.4399 0.3288 0.1437 0.027 Uiso 1 1 calc R A 1 H11B H 0.3522 0.4342 0.1896 0.027 Uiso 1 1 calc R A 1 C12X C 0.4004(3) 0.4800(3) 0.09176(17) 0.0286(9) Uani 0.766(5) 1 d PD B 1 H12A H 0.4703 0.4495 0.0546 0.043 Uiso 0.766(5) 1 calc PR B 1 H12B H 0.3879 0.5568 0.1007 0.043 Uiso 0.766(5) 1 calc PR B 1 H12C H 0.3255 0.4819 0.0792 0.043 Uiso 0.766(5) 1 calc PR B 1 C12Y C 0.4186(10) 0.3174(8) 0.1186(5) 0.028(3) Uani 0.234(5) 1 d PD B 2 H12D H 0.3436 0.3502 0.0983 0.042 Uiso 0.234(5) 1 calc PR B 2 H12E H 0.4151 0.2560 0.1508 0.042 Uiso 0.234(5) 1 calc PR B 2 H12F H 0.4914 0.2876 0.0829 0.042 Uiso 0.234(5) 1 calc PR B 2 C13 C 0.4543(2) 0.17608(19) 0.41592(10) 0.0155(4) Uani 1 1 d . . . C14 C 0.3735(2) 0.1209(2) 0.43616(12) 0.0227(5) Uani 1 1 d . . . H14 H 0.2893 0.1626 0.4552 0.027 Uiso 1 1 calc R . . C15 C 0.4185(2) 0.0037(2) 0.42788(12) 0.0273(6) Uani 1 1 d . . . H15 H 0.3654 -0.0347 0.4415 0.033 Uiso 1 1 calc R . . C16 C 0.5431(3) -0.0556(2) 0.39912(13) 0.0280(6) Uani 1 1 d . . . H16 H 0.5756 -0.1349 0.3931 0.034 Uiso 1 1 calc R . . C17 C 0.6187(2) 0.00392(18) 0.37936(12) 0.0217(5) Uani 1 1 d . . . H17 H 0.7025 -0.0367 0.3594 0.026 Uiso 1 1 calc R . . C18 C 0.41579(19) 0.30057(18) 0.42451(10) 0.0146(4) Uani 1 1 d . . . C19 C 0.2944(2) 0.3752(2) 0.45199(11) 0.0216(5) Uani 1 1 d . . . H19 H 0.2305 0.3488 0.4651 0.026 Uiso 1 1 calc R . . C20 C 0.2694(2) 0.4904(2) 0.45961(12) 0.0246(5) Uani 1 1 d . . . H20 H 0.1884 0.5420 0.4777 0.029 Uiso 1 1 calc R . . C21 C 0.3647(2) 0.52682(19) 0.44037(11) 0.0242(5) Uani 1 1 d . . . H21 H 0.3496 0.6034 0.4457 0.029 Uiso 1 1 calc R . . C22 C 0.4838(2) 0.44912(18) 0.41292(11) 0.0193(5) Uani 1 1 d . . . H22 H 0.5486 0.4743 0.4000 0.023 Uiso 1 1 calc R . . C23 C 0.4178(2) 0.80889(18) 0.21122(11) 0.0169(4) Uani 1 1 d . . . C24 C 0.2953(2) 0.8854(2) 0.20807(13) 0.0246(5) Uani 1 1 d . . . H24 H 0.2720 0.9176 0.1658 0.029 Uiso 1 1 calc R . . C25 C 0.2080(2) 0.9137(2) 0.26825(14) 0.0307(6) Uani 1 1 d . . . H25 H 0.1247 0.9645 0.2670 0.037 Uiso 1 1 calc R . . C26 C 0.2450(2) 0.8662(2) 0.33011(13) 0.0271(6) Uani 1 1 d . . . H26 H 0.1873 0.8843 0.3713 0.033 Uiso 1 1 calc R . . C27 C 0.3692(2) 0.79131(19) 0.33002(11) 0.0198(5) Uani 1 1 d . . . H27 H 0.3944 0.7603 0.3720 0.024 Uiso 1 1 calc R . . C28 C 0.5178(2) 0.77199(19) 0.14962(11) 0.0190(5) Uani 1 1 d . . . C29 C 0.5053(2) 0.8220(2) 0.08441(13) 0.0311(6) Uani 1 1 d . . . H29 H 0.4299 0.8823 0.0768 0.037 Uiso 1 1 calc R . . C30 C 0.6053(3) 0.7817(3) 0.03090(13) 0.0380(7) Uani 1 1 d . . . H30 H 0.5988 0.8156 -0.0131 0.046 Uiso 1 1 calc R . . C31 C 0.7152(2) 0.6907(2) 0.04291(12) 0.0326(6) Uani 1 1 d . . . H31 H 0.7829 0.6608 0.0069 0.039 Uiso 1 1 calc R . . C32 C 0.7232(2) 0.6447(2) 0.10918(11) 0.0212(5) Uani 1 1 d . . . H32 H 0.7977 0.5838 0.1176 0.025 Uiso 1 1 calc R . . C33 C 0.8597(2) 0.10751(18) 0.05749(10) 0.0159(4) Uani 1 1 d . . . C34 C 0.8144(2) 0.0238(2) 0.05590(12) 0.0222(5) Uani 1 1 d . . . H34 H 0.7971 0.0100 0.0149 0.027 Uiso 1 1 calc R . . C35 C 0.7954(3) -0.0385(2) 0.11535(13) 0.0300(6) Uani 1 1 d . . . H35 H 0.7638 -0.0941 0.1152 0.036 Uiso 1 1 calc R . . C36 C 0.8239(2) -0.0175(2) 0.17545(12) 0.0262(6) Uani 1 1 d . . . H36 H 0.8127 -0.0593 0.2161 0.031 Uiso 1 1 calc R . . C37 C 0.8691(2) 0.06646(18) 0.17410(11) 0.0196(5) Uani 1 1 d . . . H37 H 0.8884 0.0804 0.2144 0.024 Uiso 1 1 calc R . . C38 C 0.8832(2) 0.18079(18) -0.00240(11) 0.0166(4) Uani 1 1 d . . . C39 C 0.8681(2) 0.1684(2) -0.06817(12) 0.0254(5) Uani 1 1 d . . . H39 H 0.8412 0.1129 -0.0763 0.030 Uiso 1 1 calc R . . C40 C 0.8938(3) 0.2400(2) -0.12161(12) 0.0332(6) Uani 1 1 d . . . H40 H 0.8843 0.2333 -0.1662 0.040 Uiso 1 1 calc R . . C41 C 0.9337(3) 0.3222(2) -0.10779(12) 0.0283(6) Uani 1 1 d . . . H41 H 0.9517 0.3710 -0.1429 0.034 Uiso 1 1 calc R . . C42 C 0.9462(2) 0.32989(19) -0.04116(11) 0.0191(5) Uani 1 1 d . . . H42 H 0.9723 0.3853 -0.0320 0.023 Uiso 1 1 calc R . . N7 N 0.4925(4) 0.0892(3) 0.1161(2) 0.0884(12) Uani 1 1 d . . . C43 C 0.4677(4) 0.0733(3) 0.1742(2) 0.0588(10) Uani 1 1 d . . . C44 C 0.4395(4) 0.0530(3) 0.2484(2) 0.0727(12) Uani 1 1 d . . . H44A H 0.4951 -0.0237 0.2607 0.109 Uiso 1 1 calc R . . H44B H 0.3536 0.0612 0.2613 0.109 Uiso 1 1 calc R . . H44C H 0.4511 0.1083 0.2722 0.109 Uiso 1 1 calc R . . N8X N 0.9424(5) 0.7101(7) 0.4616(3) 0.084(3) Uani 0.514(7) 1 d PDU C 1 C45X C 0.9654(8) 0.7260(6) 0.4017(4) 0.044(2) Uani 0.514(7) 1 d PDU C 1 C46X C 1.0079(10) 0.7317(8) 0.3287(4) 0.054(2) Uani 0.514(7) 1 d PDU C 1 H46A H 1.0942 0.6774 0.3174 0.081 Uiso 0.514(7) 1 calc PR C 1 H46B H 1.0019 0.8083 0.3150 0.081 Uiso 0.514(7) 1 calc PR C 1 H46C H 0.9562 0.7131 0.3049 0.081 Uiso 0.514(7) 1 calc PR C 1 N8Y N 1.1303(7) 0.6635(6) 0.2869(3) 0.069(2) Uani 0.486(7) 1 d PDU C 2 C45Y C 1.0429(9) 0.6880(9) 0.3335(4) 0.051(2) Uani 0.486(7) 1 d PDU C 2 C46Y C 0.9370(10) 0.7090(10) 0.3896(5) 0.071(3) Uani 0.486(7) 1 d PDU C 2 H46D H 0.8640 0.7180 0.3718 0.106 Uiso 0.486(7) 1 calc PR C 2 H46E H 0.9201 0.7781 0.4121 0.106 Uiso 0.486(7) 1 calc PR C 2 H46F H 0.9567 0.6447 0.4223 0.106 Uiso 0.486(7) 1 calc PR C 2 N9 N 0.9139(4) 0.8825(4) 0.5201(2) 0.0394(12) Uani 0.50 1 d P . . C47 C 0.9729(3) 0.9581(3) 0.50718(14) 0.0499(9) Uani 0.50 1 d P . . C48 C 0.9729(3) 0.9581(3) 0.50718(14) 0.0499(9) Uani 0.50 1 d P . . H48A H 0.9272 0.9655 0.5537 0.075 Uiso 0.50 1 calc PR . . H48B H 1.0389 0.8818 0.5017 0.075 Uiso 0.50 1 calc PR . . H48C H 0.9164 0.9710 0.4757 0.075 Uiso 0.50 1 calc PR . . 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 0.01093(16) 0.00891(16) 0.00965(16) -0.00050(13) -0.00043(12) -0.00556(13) V2 0.01407(17) 0.00966(17) 0.01065(16) 0.00006(13) 0.00104(13) -0.00618(14) V3 0.01455(17) 0.00805(16) 0.01186(17) -0.00046(13) -0.00019(13) -0.00494(14) V4 0.01444(17) 0.01036(17) 0.00952(16) -0.00186(13) 0.00153(13) -0.00685(14) Cl1 0.0172(3) 0.0159(3) 0.0162(2) -0.0019(2) 0.00045(19) -0.0030(2) Cl2 0.0226(3) 0.0159(2) 0.0116(2) -0.00068(19) 0.00027(19) -0.0097(2) Cl3 0.0287(3) 0.0173(3) 0.0160(3) 0.0000(2) -0.0023(2) -0.0100(2) Cl4 0.0319(3) 0.0169(3) 0.0250(3) 0.0031(2) -0.0040(2) -0.0174(2) Cl5 0.0195(3) 0.0138(2) 0.0166(2) -0.0009(2) 0.00299(19) -0.0092(2) Cl6 0.0200(3) 0.0127(2) 0.0177(3) -0.0036(2) -0.0025(2) -0.0019(2) O1 0.0132(7) 0.0146(7) 0.0107(7) 0.0013(6) -0.0013(5) -0.0090(6) O2 0.0109(7) 0.0106(7) 0.0117(7) 0.0004(6) -0.0029(5) -0.0050(6) O3 0.0122(7) 0.0110(7) 0.0111(7) 0.0000(6) -0.0013(5) -0.0061(6) O4 0.0135(7) 0.0136(7) 0.0122(7) 0.0010(6) -0.0012(5) -0.0085(6) O5 0.0109(7) 0.0122(7) 0.0137(7) 0.0002(6) -0.0027(5) -0.0064(6) O6 0.0114(7) 0.0125(7) 0.0125(7) -0.0014(6) -0.0011(5) -0.0065(6) N1 0.0179(9) 0.0136(9) 0.0139(9) -0.0007(7) -0.0001(7) -0.0097(8) N2 0.0183(9) 0.0114(8) 0.0108(8) -0.0011(7) 0.0000(7) -0.0062(7) N3 0.0165(9) 0.0091(8) 0.0164(9) -0.0004(7) 0.0017(7) -0.0047(7) N4 0.0146(9) 0.0156(9) 0.0124(8) 0.0010(7) 0.0002(7) -0.0059(7) N5 0.0222(9) 0.0098(8) 0.0113(8) -0.0032(7) 0.0030(7) -0.0084(8) N6 0.0166(9) 0.0113(8) 0.0117(8) -0.0015(7) 0.0009(7) -0.0063(7) C1 0.0156(10) 0.0209(11) 0.0126(10) 0.0017(8) -0.0038(8) -0.0113(9) C2 0.0153(10) 0.0150(10) 0.0163(10) -0.0006(8) -0.0026(8) -0.0098(9) C3 0.0125(10) 0.0151(10) 0.0168(10) -0.0015(8) -0.0037(8) -0.0034(9) C4 0.0114(10) 0.0145(10) 0.0124(10) 0.0000(8) -0.0032(7) -0.0066(8) C5 0.0149(10) 0.0248(12) 0.0132(10) 0.0008(9) -0.0037(8) -0.0106(9) C6 0.0172(12) 0.0437(15) 0.0232(12) 0.0020(11) -0.0038(9) -0.0181(11) C7 0.0160(10) 0.0169(10) 0.0151(10) -0.0011(8) -0.0015(8) -0.0107(9) C8 0.0106(10) 0.0128(10) 0.0183(10) -0.0002(8) -0.0031(8) -0.0044(8) C9 0.0151(10) 0.0182(11) 0.0124(10) -0.0015(8) -0.0030(8) -0.0087(9) C10 0.0108(10) 0.0144(10) 0.0133(10) 0.0011(8) -0.0018(7) -0.0069(8) C11 0.0196(11) 0.0331(13) 0.0224(12) -0.0001(10) -0.0042(9) -0.0175(11) C12X 0.0199(16) 0.0328(19) 0.0354(19) 0.0068(15) -0.0129(14) -0.0112(15) C12Y 0.028(6) 0.039(7) 0.032(6) -0.011(5) -0.015(5) -0.021(5) C13 0.0175(11) 0.0201(11) 0.0116(10) 0.0000(8) -0.0022(8) -0.0106(9) C14 0.0216(12) 0.0298(13) 0.0204(12) 0.0002(10) 0.0001(9) -0.0162(11) C15 0.0376(15) 0.0323(14) 0.0253(13) 0.0006(11) -0.0015(11) -0.0293(12) C16 0.0424(15) 0.0176(12) 0.0313(14) -0.0025(10) -0.0035(11) -0.0202(12) C17 0.0276(13) 0.0137(11) 0.0238(12) -0.0054(9) 0.0035(10) -0.0110(10) C18 0.0157(10) 0.0190(11) 0.0091(9) -0.0010(8) -0.0019(8) -0.0070(9) C19 0.0157(11) 0.0291(13) 0.0183(11) -0.0050(10) -0.0013(9) -0.0071(10) C20 0.0201(12) 0.0230(12) 0.0201(12) -0.0069(10) -0.0012(9) 0.0020(10) C21 0.0365(14) 0.0118(11) 0.0174(11) -0.0039(9) -0.0004(10) -0.0042(10) C22 0.0281(12) 0.0139(10) 0.0151(11) -0.0012(9) 0.0001(9) -0.0095(10) C23 0.0164(11) 0.0138(10) 0.0180(11) 0.0017(9) -0.0009(8) -0.0054(9) C24 0.0229(12) 0.0198(12) 0.0270(13) 0.0027(10) -0.0073(10) -0.0043(10) C25 0.0164(12) 0.0216(13) 0.0443(16) -0.0059(12) -0.0008(11) 0.0009(10) C26 0.0212(12) 0.0250(13) 0.0284(13) -0.0095(11) 0.0065(10) -0.0057(11) C27 0.0208(11) 0.0172(11) 0.0166(11) -0.0038(9) 0.0039(9) -0.0056(9) C28 0.0180(11) 0.0202(11) 0.0177(11) 0.0038(9) -0.0030(8) -0.0079(10) C29 0.0234(13) 0.0391(15) 0.0239(13) 0.0138(11) -0.0078(10) -0.0081(12) C30 0.0353(15) 0.062(2) 0.0144(12) 0.0136(12) -0.0049(10) -0.0208(15) C31 0.0292(14) 0.0500(17) 0.0150(12) -0.0001(11) 0.0055(10) -0.0172(13) C32 0.0180(11) 0.0233(12) 0.0183(11) -0.0028(9) 0.0024(9) -0.0066(10) C33 0.0216(11) 0.0149(10) 0.0122(10) -0.0015(8) 0.0015(8) -0.0103(9) C34 0.0331(13) 0.0221(12) 0.0171(11) -0.0060(9) 0.0003(9) -0.0176(11) C35 0.0456(16) 0.0252(13) 0.0279(14) -0.0076(11) 0.0059(11) -0.0269(13) C36 0.0474(16) 0.0210(12) 0.0162(11) -0.0014(9) 0.0052(10) -0.0243(12) C37 0.0327(13) 0.0166(11) 0.0114(10) -0.0022(9) 0.0024(9) -0.0143(10) C38 0.0205(11) 0.0159(11) 0.0142(10) -0.0025(8) 0.0013(8) -0.0095(9) C39 0.0433(15) 0.0247(12) 0.0170(11) -0.0029(10) -0.0053(10) -0.0218(12) C40 0.0573(18) 0.0366(15) 0.0131(11) 0.0010(11) -0.0074(11) -0.0263(14) C41 0.0515(17) 0.0283(13) 0.0121(11) 0.0046(10) -0.0040(10) -0.0251(13) C42 0.0291(13) 0.0168(11) 0.0150(11) -0.0005(9) -0.0010(9) -0.0140(10) N7 0.108(3) 0.092(3) 0.074(3) 0.020(2) -0.042(2) -0.043(2) C43 0.071(3) 0.052(2) 0.064(2) 0.0150(19) -0.033(2) -0.029(2) C44 0.100(3) 0.059(2) 0.072(3) -0.002(2) -0.020(2) -0.043(2) N8X 0.042(4) 0.137(7) 0.075(4) 0.031(5) -0.007(3) -0.048(4) C45X 0.036(4) 0.018(3) 0.078(5) -0.006(3) 0.011(4) -0.020(3) C46X 0.070(6) 0.037(5) 0.071(5) 0.021(4) -0.040(5) -0.029(5) N8Y 0.099(6) 0.068(5) 0.050(4) 0.011(3) -0.013(3) -0.047(4) C45Y 0.086(7) 0.047(6) 0.043(4) 0.027(4) -0.042(4) -0.043(5) C46Y 0.088(8) 0.071(7) 0.076(6) -0.045(5) 0.003(5) -0.052(6) N9 0.037(3) 0.041(3) 0.043(3) 0.019(2) -0.016(2) -0.020(2) C47 0.055(2) 0.0391(18) 0.0231(14) -0.0034(14) -0.0121(14) 0.0153(15) C48 0.055(2) 0.0391(18) 0.0231(14) -0.0034(14) -0.0121(14) 0.0153(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 O2 1.9468(14) . ? V1 O1 1.9557(14) . ? V1 O3 1.9683(14) . ? V1 O6 1.9879(14) . ? V1 O5 2.0077(14) . ? V1 O4 2.0108(14) . ? V1 V4 3.0832(5) . ? V1 V3 3.0932(5) . ? V1 V2 3.1036(5) . ? V2 O4 1.9750(14) . ? V2 O1 1.9973(14) . ? V2 N2 2.1159(17) . ? V2 N1 2.1542(17) . ? V2 Cl1 2.3379(6) . ? V2 Cl2 2.3550(6) . ? V3 O5 1.9535(14) . ? V3 O2 2.0182(14) . ? V3 N4 2.1326(17) . ? V3 N3 2.1400(17) . ? V3 Cl3 2.3051(6) . ? V3 Cl4 2.3668(6) . ? V4 O6 1.9705(14) . ? V4 O3 1.9970(14) . ? V4 N5 2.1151(17) . ? V4 N6 2.1454(17) . ? V4 Cl5 2.3288(6) . ? V4 Cl6 2.3639(6) . ? O1 C1 1.425(2) . ? O2 C2 1.419(2) . ? O3 C3 1.415(2) . ? O4 C7 1.424(2) . ? O5 C8 1.425(2) . ? O6 C9 1.421(2) . ? N1 C17 1.342(3) . ? N1 C13 1.357(3) . ? N2 C22 1.339(3) . ? N2 C18 1.350(3) . ? N3 C27 1.340(3) . ? N3 C23 1.355(3) . ? N4 C32 1.338(3) . ? N4 C28 1.351(3) . ? N5 C37 1.337(3) . ? N5 C33 1.353(3) . ? N6 C42 1.344(3) . ? N6 C38 1.356(3) . ? C1 C4 1.539(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C4 1.537(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.540(3) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.539(3) . ? C5 C6 1.527(3) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 C10 1.545(3) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C10 1.538(3) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.535(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 C11 1.543(3) . ? C11 C12Y 1.446(7) . ? C11 C12X 1.472(4) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C12X H12A 0.9600 . ? C12X H12B 0.9600 . ? C12X H12C 0.9600 . ? C12Y H12D 0.9600 . ? C12Y H12E 0.9600 . ? C12Y H12F 0.9600 . ? C13 C14 1.383(3) . ? C13 C18 1.476(3) . ? C14 C15 1.376(3) . ? C14 H14 0.9300 . ? C15 C16 1.375(3) . ? C15 H15 0.9300 . ? C16 C17 1.374(3) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.385(3) . ? C19 C20 1.391(3) . ? C19 H19 0.9300 . ? C20 C21 1.361(3) . ? C20 H20 0.9300 . ? C21 C22 1.380(3) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.377(3) . ? C23 C28 1.476(3) . ? C24 C25 1.376(3) . ? C24 H24 0.9300 . ? C25 C26 1.373(4) . ? C25 H25 0.9300 . ? C26 C27 1.378(3) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.379(3) . ? C29 C30 1.373(3) . ? C29 H29 0.9300 . ? C30 C31 1.377(4) . ? C30 H30 0.9300 . ? C31 C32 1.378(3) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.386(3) . ? C33 C38 1.476(3) . ? C34 C35 1.374(3) . ? C34 H34 0.9300 . ? C35 C36 1.385(3) . ? C35 H35 0.9300 . ? C36 C37 1.379(3) . ? C36 H36 0.9300 . ? C37 H37 0.9300 . ? C38 C39 1.386(3) . ? C39 C40 1.385(3) . ? C39 H39 0.9300 . ? C40 C41 1.390(3) . ? C40 H40 0.9300 . ? C41 C42 1.376(3) . ? C41 H41 0.9300 . ? C42 H42 0.9300 . ? N7 C43 1.143(5) . ? C43 C44 1.454(5) . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? N8X C45X 1.174(7) . ? C45X C46X 1.432(7) . ? C46X H46A 0.9600 . ? C46X H46B 0.9600 . ? C46X H46C 0.9600 . ? N8Y C45Y 1.191(7) . ? C45Y C46Y 1.446(7) . ? C46Y H46D 0.9600 . ? C46Y H46E 0.9600 . ? C46Y H46F 0.9600 . ? N9 C47 1.384(6) . ? C47 C48 1.436(7) 2_776 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 V1 O1 91.46(6) . . ? O2 V1 O3 92.37(6) . . ? O1 V1 O3 90.89(6) . . ? O2 V1 O6 103.91(6) . . ? O1 V1 O6 161.08(6) . . ? O3 V1 O6 77.71(6) . . ? O2 V1 O5 77.45(6) . . ? O1 V1 O5 103.82(6) . . ? O3 V1 O5 162.17(6) . . ? O6 V1 O5 90.43(6) . . ? O2 V1 O4 160.25(6) . . ? O1 V1 O4 77.11(6) . . ? O3 V1 O4 103.72(6) . . ? O6 V1 O4 90.83(6) . . ? O5 V1 O4 89.56(6) . . ? O2 V1 V4 97.22(4) . . ? O1 V1 V4 129.47(4) . . ? O3 V1 V4 39.30(4) . . ? O6 V1 V4 38.64(4) . . ? O5 V1 V4 126.67(4) . . ? O4 V1 V4 102.49(4) . . ? O2 V1 V3 39.56(4) . . ? O1 V1 V3 97.28(4) . . ? O3 V1 V3 131.10(4) . . ? O6 V1 V3 101.59(4) . . ? O5 V1 V3 38.04(4) . . ? O4 V1 V3 125.13(4) . . ? V4 V1 V3 120.316(14) . . ? O2 V1 V2 128.98(4) . . ? O1 V1 V2 38.74(4) . . ? O3 V1 V2 97.42(4) . . ? O6 V1 V2 127.11(4) . . ? O5 V1 V2 100.36(4) . . ? O4 V1 V2 38.45(4) . . ? V4 V1 V2 121.175(14) . . ? V3 V1 V2 118.505(14) . . ? O4 V2 O1 76.99(6) . . ? O4 V2 N2 88.64(6) . . ? O1 V2 N2 97.66(6) . . ? O4 V2 N1 97.06(6) . . ? O1 V2 N1 171.36(6) . . ? N2 V2 N1 75.74(7) . . ? O4 V2 Cl1 98.79(4) . . ? O1 V2 Cl1 94.43(4) . . ? N2 V2 Cl1 166.99(5) . . ? N1 V2 Cl1 92.67(5) . . ? O4 V2 Cl2 165.64(4) . . ? O1 V2 Cl2 92.67(4) . . ? N2 V2 Cl2 82.82(5) . . ? N1 V2 Cl2 92.02(5) . . ? Cl1 V2 Cl2 91.85(2) . . ? O4 V2 V1 39.28(4) . . ? O1 V2 V1 37.79(4) . . ? N2 V2 V1 96.02(5) . . ? N1 V2 V1 136.25(5) . . ? Cl1 V2 V1 96.485(18) . . ? Cl2 V2 V1 130.131(19) . . ? O5 V3 O2 77.05(6) . . ? O5 V3 N4 87.66(6) . . ? O2 V3 N4 99.86(6) . . ? O5 V3 N3 92.40(6) . . ? O2 V3 N3 168.71(6) . . ? N4 V3 N3 75.39(7) . . ? O5 V3 Cl3 102.77(4) . . ? O2 V3 Cl3 93.05(4) . . ? N4 V3 Cl3 164.99(5) . . ? N3 V3 Cl3 93.21(5) . . ? O5 V3 Cl4 163.75(4) . . ? O2 V3 Cl4 92.81(4) . . ? N4 V3 Cl4 81.54(5) . . ? N3 V3 Cl4 96.55(5) . . ? Cl3 V3 Cl4 90.28(2) . . ? O5 V3 V1 39.29(4) . . ? O2 V3 V1 37.91(4) . . ? N4 V3 V1 97.49(5) . . ? N3 V3 V1 131.69(5) . . ? Cl3 V3 V1 97.400(18) . . ? Cl4 V3 V1 130.20(2) . . ? O6 V4 O3 77.44(6) . . ? O6 V4 N5 85.71(6) . . ? O3 V4 N5 96.08(6) . . ? O6 V4 N6 94.92(6) . . ? O3 V4 N6 169.12(6) . . ? N5 V4 N6 75.42(7) . . ? O6 V4 Cl5 97.42(4) . . ? O3 V4 Cl5 93.38(4) . . ? N5 V4 Cl5 170.48(5) . . ? N6 V4 Cl5 95.31(5) . . ? O6 V4 Cl6 166.94(4) . . ? O3 V4 Cl6 93.30(4) . . ? N5 V4 Cl6 86.15(5) . . ? N6 V4 Cl6 92.90(5) . . ? Cl5 V4 Cl6 92.25(2) . . ? O6 V4 V1 39.04(4) . . ? O3 V4 V1 38.63(4) . . ? N5 V4 V1 94.43(5) . . ? N6 V4 V1 133.91(5) . . ? Cl5 V4 V1 93.626(18) . . ? Cl6 V4 V1 131.81(2) . . ? C1 O1 V1 117.24(11) . . ? C1 O1 V2 131.26(12) . . ? V1 O1 V2 103.46(6) . . ? C2 O2 V1 118.41(12) . . ? C2 O2 V3 130.34(12) . . ? V1 O2 V3 102.53(6) . . ? C3 O3 V1 117.46(11) . . ? C3 O3 V4 129.45(12) . . ? V1 O3 V4 102.07(6) . . ? C7 O4 V2 134.87(12) . . ? C7 O4 V1 117.43(11) . . ? V2 O4 V1 102.27(6) . . ? C8 O5 V3 133.66(12) . . ? C8 O5 V1 118.20(11) . . ? V3 O5 V1 102.67(6) . . ? C9 O6 V4 134.25(12) . . ? C9 O6 V1 118.45(11) . . ? V4 O6 V1 102.32(6) . . ? C17 N1 C13 117.69(19) . . ? C17 N1 V2 125.77(15) . . ? C13 N1 V2 116.25(14) . . ? C22 N2 C18 119.43(18) . . ? C22 N2 V2 122.63(15) . . ? C18 N2 V2 117.70(13) . . ? C27 N3 C23 117.94(18) . . ? C27 N3 V3 124.79(15) . . ? C23 N3 V3 117.13(13) . . ? C32 N4 C28 119.17(19) . . ? C32 N4 V3 122.84(15) . . ? C28 N4 V3 117.50(14) . . ? C37 N5 C33 119.27(18) . . ? C37 N5 V4 122.18(14) . . ? C33 N5 V4 118.48(13) . . ? C42 N6 C38 118.20(18) . . ? C42 N6 V4 125.05(14) . . ? C38 N6 V4 116.73(13) . . ? O1 C1 C4 113.81(16) . . ? O1 C1 H1A 108.8 . . ? C4 C1 H1A 108.8 . . ? O1 C1 H1B 108.8 . . ? C4 C1 H1B 108.8 . . ? H1A C1 H1B 107.7 . . ? O2 C2 C4 112.97(16) . . ? O2 C2 H2A 109.0 . . ? C4 C2 H2A 109.0 . . ? O2 C2 H2B 109.0 . . ? C4 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? O3 C3 C4 113.77(16) . . ? O3 C3 H3A 108.8 . . ? C4 C3 H3A 108.8 . . ? O3 C3 H3B 108.8 . . ? C4 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C2 C4 C1 111.14(17) . . ? C2 C4 C5 108.70(17) . . ? C1 C4 C5 105.81(16) . . ? C2 C4 C3 112.21(17) . . ? C1 C4 C3 110.56(17) . . ? C5 C4 C3 108.15(16) . . ? C6 C5 C4 115.82(18) . . ? C6 C5 H5A 108.3 . . ? C4 C5 H5A 108.3 . . ? C6 C5 H5B 108.3 . . ? C4 C5 H5B 108.3 . . ? H5A C5 H5B 107.4 . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O4 C7 C10 114.25(16) . . ? O4 C7 H7A 108.7 . . ? C10 C7 H7A 108.7 . . ? O4 C7 H7B 108.7 . . ? C10 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? O5 C8 C10 113.57(16) . . ? O5 C8 H8A 108.9 . . ? C10 C8 H8A 108.9 . . ? O5 C8 H8B 108.9 . . ? C10 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? O6 C9 C10 113.88(16) . . ? O6 C9 H9A 108.8 . . ? C10 C9 H9A 108.8 . . ? O6 C9 H9B 108.8 . . ? C10 C9 H9B 108.8 . . ? H9A C9 H9B 107.7 . . ? C9 C10 C8 111.93(17) . . ? C9 C10 C11 108.01(17) . . ? C8 C10 C11 107.22(17) . . ? C9 C10 C7 111.93(17) . . ? C8 C10 C7 110.82(17) . . ? C11 C10 C7 106.63(17) . . ? C12Y C11 C12X 87.0(5) . . ? C12Y C11 C10 126.4(5) . . ? C12X C11 C10 118.5(2) . . ? C12Y C11 H11A 22.1 . . ? C12X C11 H11A 107.7 . . ? C10 C11 H11A 107.7 . . ? C12Y C11 H11B 107.2 . . ? C12X C11 H11B 107.7 . . ? C10 C11 H11B 107.7 . . ? H11A C11 H11B 107.1 . . ? C11 C12X H12A 109.5 . . ? C11 C12X H12B 109.5 . . ? C11 C12X H12C 109.5 . . ? C11 C12Y H12D 109.5 . . ? C11 C12Y H12E 109.5 . . ? H12D C12Y H12E 109.5 . . ? C11 C12Y H12F 109.5 . . ? H12D C12Y H12F 109.5 . . ? H12E C12Y H12F 109.5 . . ? N1 C13 C14 121.7(2) . . ? N1 C13 C18 114.85(18) . . ? C14 C13 C18 123.5(2) . . ? C15 C14 C13 119.5(2) . . ? C15 C14 H14 120.3 . . ? C13 C14 H14 120.3 . . ? C16 C15 C14 119.0(2) . . ? C16 C15 H15 120.5 . . ? C14 C15 H15 120.5 . . ? C17 C16 C15 118.9(2) . . ? C17 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? N1 C17 C16 123.2(2) . . ? N1 C17 H17 118.4 . . ? C16 C17 H17 118.4 . . ? N2 C18 C19 121.0(2) . . ? N2 C18 C13 115.20(18) . . ? C19 C18 C13 123.8(2) . . ? C18 C19 C20 119.0(2) . . ? C18 C19 H19 120.5 . . ? C20 C19 H19 120.5 . . ? C21 C20 C19 119.4(2) . . ? C21 C20 H20 120.3 . . ? C19 C20 H20 120.3 . . ? C20 C21 C22 119.4(2) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? N2 C22 C21 121.8(2) . . ? N2 C22 H22 119.1 . . ? C21 C22 H22 119.1 . . ? N3 C23 C24 121.9(2) . . ? N3 C23 C28 114.80(18) . . ? C24 C23 C28 123.3(2) . . ? C25 C24 C23 119.1(2) . . ? C25 C24 H24 120.4 . . ? C23 C24 H24 120.4 . . ? C26 C25 C24 119.4(2) . . ? C26 C25 H25 120.3 . . ? C24 C25 H25 120.3 . . ? C25 C26 C27 118.7(2) . . ? C25 C26 H26 120.6 . . ? C27 C26 H26 120.6 . . ? N3 C27 C26 122.8(2) . . ? N3 C27 H27 118.6 . . ? C26 C27 H27 118.6 . . ? N4 C28 C29 121.2(2) . . ? N4 C28 C23 114.59(19) . . ? C29 C28 C23 124.2(2) . . ? C30 C29 C28 119.3(2) . . ? C30 C29 H29 120.3 . . ? C28 C29 H29 120.3 . . ? C29 C30 C31 119.5(2) . . ? C29 C30 H30 120.2 . . ? C31 C30 H30 120.2 . . ? C30 C31 C32 118.8(2) . . ? C30 C31 H31 120.6 . . ? C32 C31 H31 120.6 . . ? N4 C32 C31 122.0(2) . . ? N4 C32 H32 119.0 . . ? C31 C32 H32 119.0 . . ? N5 C33 C34 121.04(19) . . ? N5 C33 C38 114.10(18) . . ? C34 C33 C38 124.9(2) . . ? C35 C34 C33 119.5(2) . . ? C35 C34 H34 120.2 . . ? C33 C34 H34 120.2 . . ? C34 C35 C36 119.1(2) . . ? C34 C35 H35 120.4 . . ? C36 C35 H35 120.4 . . ? C37 C36 C35 119.0(2) . . ? C37 C36 H36 120.5 . . ? C35 C36 H36 120.5 . . ? N5 C37 C36 122.0(2) . . ? N5 C37 H37 119.0 . . ? C36 C37 H37 119.0 . . ? N6 C38 C39 122.1(2) . . ? N6 C38 C33 115.19(18) . . ? C39 C38 C33 122.7(2) . . ? C40 C39 C38 118.9(2) . . ? C40 C39 H39 120.6 . . ? C38 C39 H39 120.6 . . ? C39 C40 C41 119.2(2) . . ? C39 C40 H40 120.4 . . ? C41 C40 H40 120.4 . . ? C42 C41 C40 118.7(2) . . ? C42 C41 H41 120.6 . . ? C40 C41 H41 120.6 . . ? N6 C42 C41 122.9(2) . . ? N6 C42 H42 118.5 . . ? C41 C42 H42 118.5 . . ? N7 C43 C44 178.4(4) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N8X C45X C46X 172.6(9) . . ? C45X C46X H46A 109.5 . . ? C45X C46X H46B 109.5 . . ? H46A C46X H46B 109.5 . . ? C45X C46X H46C 109.5 . . ? H46A C46X H46C 109.5 . . ? H46B C46X H46C 109.5 . . ? N8Y C45Y C46Y 175.5(11) . . ? C45Y C46Y H46D 109.5 . . ? C45Y C46Y H46E 109.5 . . ? H46D C46Y H46E 109.5 . . ? C45Y C46Y H46F 109.5 . . ? H46D C46Y H46F 109.5 . . ? H46E C46Y H46F 109.5 . . ? N9 C47 C48 176.6(4) . 2_776 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 V1 V2 O4 158.11(8) . . . . ? O1 V1 V2 O4 175.16(9) . . . . ? O3 V1 V2 O4 -102.73(7) . . . . ? O6 V1 V2 O4 -22.56(8) . . . . ? O5 V1 V2 O4 75.94(7) . . . . ? V4 V1 V2 O4 -69.17(6) . . . . ? V3 V1 V2 O4 111.67(6) . . . . ? O2 V1 V2 O1 -17.05(8) . . . . ? O3 V1 V2 O1 82.10(8) . . . . ? O6 V1 V2 O1 162.27(8) . . . . ? O5 V1 V2 O1 -99.22(8) . . . . ? O4 V1 V2 O1 -175.16(9) . . . . ? V4 V1 V2 O1 115.67(7) . . . . ? V3 V1 V2 O1 -63.50(7) . . . . ? O2 V1 V2 N2 77.70(7) . . . . ? O1 V1 V2 N2 94.75(8) . . . . ? O3 V1 V2 N2 176.85(6) . . . . ? O6 V1 V2 N2 -102.97(7) . . . . ? O5 V1 V2 N2 -4.47(6) . . . . ? O4 V1 V2 N2 -80.41(8) . . . . ? V4 V1 V2 N2 -149.58(5) . . . . ? V3 V1 V2 N2 31.25(5) . . . . ? O2 V1 V2 N1 153.33(9) . . . . ? O1 V1 V2 N1 170.39(9) . . . . ? O3 V1 V2 N1 -107.51(8) . . . . ? O6 V1 V2 N1 -27.34(9) . . . . ? O5 V1 V2 N1 71.16(8) . . . . ? O4 V1 V2 N1 -4.78(9) . . . . ? V4 V1 V2 N1 -73.94(7) . . . . ? V3 V1 V2 N1 106.89(7) . . . . ? O2 V1 V2 Cl1 -105.92(5) . . . . ? O1 V1 V2 Cl1 -88.87(7) . . . . ? O3 V1 V2 Cl1 -6.76(4) . . . . ? O6 V1 V2 Cl1 73.41(5) . . . . ? O5 V1 V2 Cl1 171.91(4) . . . . ? O4 V1 V2 Cl1 95.97(6) . . . . ? V4 V1 V2 Cl1 26.80(2) . . . . ? V3 V1 V2 Cl1 -152.36(2) . . . . ? O2 V1 V2 Cl2 -7.97(6) . . . . ? O1 V1 V2 Cl2 9.08(7) . . . . ? O3 V1 V2 Cl2 91.18(5) . . . . ? O6 V1 V2 Cl2 171.35(5) . . . . ? O5 V1 V2 Cl2 -90.14(5) . . . . ? O4 V1 V2 Cl2 -166.08(7) . . . . ? V4 V1 V2 Cl2 124.75(2) . . . . ? V3 V1 V2 Cl2 -54.42(3) . . . . ? O2 V1 V3 O5 173.41(9) . . . . ? O1 V1 V3 O5 -103.15(7) . . . . ? O3 V1 V3 O5 159.25(8) . . . . ? O6 V1 V3 O5 75.54(7) . . . . ? O4 V1 V3 O5 -23.82(8) . . . . ? V4 V1 V3 O5 112.05(6) . . . . ? V2 V1 V3 O5 -68.78(6) . . . . ? O1 V1 V3 O2 83.44(7) . . . . ? O3 V1 V3 O2 -14.16(8) . . . . ? O6 V1 V3 O2 -97.87(7) . . . . ? O5 V1 V3 O2 -173.41(9) . . . . ? O4 V1 V3 O2 162.77(8) . . . . ? V4 V1 V3 O2 -61.36(6) . . . . ? V2 V1 V3 O2 117.81(6) . . . . ? O2 V1 V3 N4 96.46(8) . . . . ? O1 V1 V3 N4 179.89(6) . . . . ? O3 V1 V3 N4 82.29(7) . . . . ? O6 V1 V3 N4 -1.42(6) . . . . ? O5 V1 V3 N4 -76.95(8) . . . . ? O4 V1 V3 N4 -100.77(7) . . . . ? V4 V1 V3 N4 35.10(5) . . . . ? V2 V1 V3 N4 -145.73(5) . . . . ? O2 V1 V3 N3 173.53(9) . . . . ? O1 V1 V3 N3 -103.03(8) . . . . ? O3 V1 V3 N3 159.37(8) . . . . ? O6 V1 V3 N3 75.66(8) . . . . ? O5 V1 V3 N3 0.12(9) . . . . ? O4 V1 V3 N3 -23.70(8) . . . . ? V4 V1 V3 N3 112.17(7) . . . . ? V2 V1 V3 N3 -68.66(7) . . . . ? O2 V1 V3 Cl3 -85.44(6) . . . . ? O1 V1 V3 Cl3 -2.01(4) . . . . ? O3 V1 V3 Cl3 -99.60(6) . . . . ? O6 V1 V3 Cl3 176.69(4) . . . . ? O5 V1 V3 Cl3 101.15(7) . . . . ? O4 V1 V3 Cl3 77.33(5) . . . . ? V4 V1 V3 Cl3 -146.80(2) . . . . ? V2 V1 V3 Cl3 32.37(2) . . . . ? O2 V1 V3 Cl4 11.23(7) . . . . ? O1 V1 V3 Cl4 94.66(5) . . . . ? O3 V1 V3 Cl4 -2.94(6) . . . . ? O6 V1 V3 Cl4 -86.65(5) . . . . ? O5 V1 V3 Cl4 -162.18(7) . . . . ? O4 V1 V3 Cl4 174.00(5) . . . . ? V4 V1 V3 Cl4 -50.13(3) . . . . ? V2 V1 V3 Cl4 129.04(3) . . . . ? O2 V1 V4 O6 -103.28(7) . . . . ? O1 V1 V4 O6 158.82(8) . . . . ? O3 V1 V4 O6 171.82(9) . . . . ? O5 V1 V4 O6 -23.58(8) . . . . ? O4 V1 V4 O6 75.34(8) . . . . ? V3 V1 V4 O6 -68.98(6) . . . . ? V2 V1 V4 O6 111.87(6) . . . . ? O2 V1 V4 O3 84.90(7) . . . . ? O1 V1 V4 O3 -13.00(8) . . . . ? O6 V1 V4 O3 -171.82(9) . . . . ? O5 V1 V4 O3 164.60(8) . . . . ? O4 V1 V4 O3 -96.48(7) . . . . ? V3 V1 V4 O3 119.20(6) . . . . ? V2 V1 V4 O3 -59.95(6) . . . . ? O2 V1 V4 N5 179.11(6) . . . . ? O1 V1 V4 N5 81.20(7) . . . . ? O3 V1 V4 N5 94.21(8) . . . . ? O6 V1 V4 N5 -77.61(8) . . . . ? O5 V1 V4 N5 -101.19(7) . . . . ? O4 V1 V4 N5 -2.27(6) . . . . ? V3 V1 V4 N5 -146.59(5) . . . . ? V2 V1 V4 N5 34.26(5) . . . . ? O2 V1 V4 N6 -106.90(8) . . . . ? O1 V1 V4 N6 155.19(8) . . . . ? O3 V1 V4 N6 168.19(9) . . . . ? O6 V1 V4 N6 -3.62(9) . . . . ? O5 V1 V4 N6 -27.20(8) . . . . ? O4 V1 V4 N6 71.71(8) . . . . ? V3 V1 V4 N6 -72.61(7) . . . . ? V2 V1 V4 N6 108.24(7) . . . . ? O2 V1 V4 Cl5 -5.97(4) . . . . ? O1 V1 V4 Cl5 -103.88(6) . . . . ? O3 V1 V4 Cl5 -90.88(6) . . . . ? O6 V1 V4 Cl5 97.31(6) . . . . ? O5 V1 V4 Cl5 73.73(5) . . . . ? O4 V1 V4 Cl5 172.64(4) . . . . ? V3 V1 V4 Cl5 28.33(2) . . . . ? V2 V1 V4 Cl5 -150.83(2) . . . . ? O2 V1 V4 Cl6 90.32(5) . . . . ? O1 V1 V4 Cl6 -7.59(6) . . . . ? O3 V1 V4 Cl6 5.41(7) . . . . ? O6 V1 V4 Cl6 -166.41(7) . . . . ? O5 V1 V4 Cl6 170.01(5) . . . . ? O4 V1 V4 Cl6 -91.07(5) . . . . ? V3 V1 V4 Cl6 124.61(3) . . . . ? V2 V1 V4 Cl6 -54.54(3) . . . . ? O2 V1 O1 C1 -40.82(14) . . . . ? O3 V1 O1 C1 51.57(14) . . . . ? O6 V1 O1 C1 103.9(2) . . . . ? O5 V1 O1 C1 -118.25(13) . . . . ? O4 V1 O1 C1 155.44(14) . . . . ? V4 V1 O1 C1 59.77(14) . . . . ? V3 V1 O1 C1 -80.09(13) . . . . ? V2 V1 O1 C1 152.36(16) . . . . ? O2 V1 O1 V2 166.82(6) . . . . ? O3 V1 O1 V2 -100.79(6) . . . . ? O6 V1 O1 V2 -48.5(2) . . . . ? O5 V1 O1 V2 89.39(7) . . . . ? O4 V1 O1 V2 3.08(6) . . . . ? V4 V1 O1 V2 -92.59(6) . . . . ? V3 V1 O1 V2 127.55(5) . . . . ? O4 V2 O1 C1 -149.87(17) . . . . ? N2 V2 O1 C1 123.32(16) . . . . ? N1 V2 O1 C1 163.0(4) . . . . ? Cl1 V2 O1 C1 -51.85(16) . . . . ? Cl2 V2 O1 C1 40.21(16) . . . . ? V1 V2 O1 C1 -146.73(19) . . . . ? O4 V2 O1 V1 -3.14(6) . . . . ? N2 V2 O1 V1 -89.95(7) . . . . ? N1 V2 O1 V1 -50.2(4) . . . . ? Cl1 V2 O1 V1 94.88(5) . . . . ? Cl2 V2 O1 V1 -173.06(5) . . . . ? O1 V1 O2 C2 51.24(13) . . . . ? O3 V1 O2 C2 -39.71(13) . . . . ? O6 V1 O2 C2 -117.62(13) . . . . ? O5 V1 O2 C2 155.08(14) . . . . ? O4 V1 O2 C2 105.1(2) . . . . ? V4 V1 O2 C2 -78.86(13) . . . . ? V3 V1 O2 C2 150.93(16) . . . . ? V2 V1 O2 C2 61.82(14) . . . . ? O1 V1 O2 V3 -99.68(6) . . . . ? O3 V1 O2 V3 169.37(6) . . . . ? O6 V1 O2 V3 91.45(6) . . . . ? O5 V1 O2 V3 4.15(6) . . . . ? O4 V1 O2 V3 -45.79(19) . . . . ? V4 V1 O2 V3 130.21(5) . . . . ? V2 V1 O2 V3 -89.11(6) . . . . ? O5 V3 O2 C2 -150.17(16) . . . . ? N4 V3 O2 C2 124.57(16) . . . . ? N3 V3 O2 C2 -171.4(3) . . . . ? Cl3 V3 O2 C2 -47.76(15) . . . . ? Cl4 V3 O2 C2 42.67(15) . . . . ? V1 V3 O2 C2 -145.90(18) . . . . ? O5 V3 O2 V1 -4.28(6) . . . . ? N4 V3 O2 V1 -89.54(7) . . . . ? N3 V3 O2 V1 -25.5(3) . . . . ? Cl3 V3 O2 V1 98.14(5) . . . . ? Cl4 V3 O2 V1 -171.44(5) . . . . ? O2 V1 O3 C3 49.00(14) . . . . ? O1 V1 O3 C3 -42.50(14) . . . . ? O6 V1 O3 C3 152.72(14) . . . . ? O5 V1 O3 C3 103.4(2) . . . . ? O4 V1 O3 C3 -119.45(13) . . . . ? V4 V1 O3 C3 147.50(16) . . . . ? V3 V1 O3 C3 57.97(14) . . . . ? V2 V1 O3 C3 -80.82(13) . . . . ? O2 V1 O3 V4 -98.50(6) . . . . ? O1 V1 O3 V4 170.00(6) . . . . ? O6 V1 O3 V4 5.22(6) . . . . ? O5 V1 O3 V4 -44.1(2) . . . . ? O4 V1 O3 V4 93.05(6) . . . . ? V3 V1 O3 V4 -89.53(6) . . . . ? V2 V1 O3 V4 131.68(5) . . . . ? O6 V4 O3 C3 -147.14(16) . . . . ? N5 V4 O3 C3 128.64(15) . . . . ? N6 V4 O3 C3 166.8(3) . . . . ? Cl5 V4 O3 C3 -50.29(15) . . . . ? Cl6 V4 O3 C3 42.17(15) . . . . ? V1 V4 O3 C3 -141.87(18) . . . . ? O6 V4 O3 V1 -5.27(6) . . . . ? N5 V4 O3 V1 -89.49(7) . . . . ? N6 V4 O3 V1 -51.3(3) . . . . ? Cl5 V4 O3 V1 91.58(5) . . . . ? Cl6 V4 O3 V1 -175.96(5) . . . . ? O1 V2 O4 C7 -148.82(18) . . . . ? N2 V2 O4 C7 -50.63(17) . . . . ? N1 V2 O4 C7 24.82(18) . . . . ? Cl1 V2 O4 C7 118.64(17) . . . . ? Cl2 V2 O4 C7 -104.0(2) . . . . ? V1 V2 O4 C7 -151.9(2) . . . . ? O1 V2 O4 V1 3.04(6) . . . . ? N2 V2 O4 V1 101.22(7) . . . . ? N1 V2 O4 V1 176.67(6) . . . . ? Cl1 V2 O4 V1 -89.51(5) . . . . ? Cl2 V2 O4 V1 47.9(2) . . . . ? O2 V1 O4 C7 98.8(2) . . . . ? O1 V1 O4 C7 154.77(14) . . . . ? O3 V1 O4 C7 -117.49(13) . . . . ? O6 V1 O4 C7 -39.95(13) . . . . ? O5 V1 O4 C7 50.48(13) . . . . ? V4 V1 O4 C7 -77.11(13) . . . . ? V3 V1 O4 C7 64.88(14) . . . . ? V2 V1 O4 C7 157.87(16) . . . . ? O2 V1 O4 V2 -59.05(19) . . . . ? O1 V1 O4 V2 -3.10(6) . . . . ? O3 V1 O4 V2 84.63(7) . . . . ? O6 V1 O4 V2 162.18(6) . . . . ? O5 V1 O4 V2 -107.40(6) . . . . ? V4 V1 O4 V2 125.01(5) . . . . ? V3 V1 O4 V2 -92.99(6) . . . . ? O2 V3 O5 C8 -147.97(17) . . . . ? N4 V3 O5 C8 -47.29(17) . . . . ? N3 V3 O5 C8 27.97(17) . . . . ? Cl3 V3 O5 C8 121.81(16) . . . . ? Cl4 V3 O5 C8 -95.5(2) . . . . ? V1 V3 O5 C8 -152.1(2) . . . . ? O2 V3 O5 V1 4.15(6) . . . . ? N4 V3 O5 V1 104.83(7) . . . . ? N3 V3 O5 V1 -179.91(7) . . . . ? Cl3 V3 O5 V1 -86.07(5) . . . . ? Cl4 V3 O5 V1 56.60(19) . . . . ? O2 V1 O5 C8 153.13(14) . . . . ? O1 V1 O5 C8 -118.46(13) . . . . ? O3 V1 O5 C8 96.8(2) . . . . ? O6 V1 O5 C8 48.98(13) . . . . ? O4 V1 O5 C8 -41.86(13) . . . . ? V4 V1 O5 C8 63.44(14) . . . . ? V3 V1 O5 C8 157.43(16) . . . . ? V2 V1 O5 C8 -78.96(13) . . . . ? O2 V1 O5 V3 -4.29(6) . . . . ? O1 V1 O5 V3 84.11(7) . . . . ? O3 V1 O5 V3 -60.7(2) . . . . ? O6 V1 O5 V3 -108.45(6) . . . . ? O4 V1 O5 V3 160.72(6) . . . . ? V4 V1 O5 V3 -93.99(6) . . . . ? V2 V1 O5 V3 123.62(5) . . . . ? O3 V4 O6 C9 -148.09(17) . . . . ? N5 V4 O6 C9 -50.87(17) . . . . ? N6 V4 O6 C9 24.07(17) . . . . ? Cl5 V4 O6 C9 120.09(16) . . . . ? Cl6 V4 O6 C9 -102.5(2) . . . . ? V1 V4 O6 C9 -153.3(2) . . . . ? O3 V4 O6 V1 5.22(6) . . . . ? N5 V4 O6 V1 102.44(7) . . . . ? N6 V4 O6 V1 177.38(6) . . . . ? Cl5 V4 O6 V1 -86.61(5) . . . . ? Cl6 V4 O6 V1 50.8(2) . . . . ? O2 V1 O6 C9 -117.35(13) . . . . ? O1 V1 O6 C9 99.2(2) . . . . ? O3 V1 O6 C9 153.24(14) . . . . ? O5 V1 O6 C9 -40.18(14) . . . . ? O4 V1 O6 C9 49.38(14) . . . . ? V4 V1 O6 C9 158.53(16) . . . . ? V3 V1 O6 C9 -76.81(13) . . . . ? V2 V1 O6 C9 63.19(14) . . . . ? O2 V1 O6 V4 84.11(7) . . . . ? O1 V1 O6 V4 -59.35(19) . . . . ? O3 V1 O6 V4 -5.29(6) . . . . ? O5 V1 O6 V4 161.29(6) . . . . ? O4 V1 O6 V4 -109.15(6) . . . . ? V3 V1 O6 V4 124.66(5) . . . . ? V2 V1 O6 V4 -95.35(6) . . . . ? O4 V2 N1 C17 94.85(18) . . . . ? O1 V2 N1 C17 140.8(4) . . . . ? N2 V2 N1 C17 -178.37(19) . . . . ? Cl1 V2 N1 C17 -4.36(18) . . . . ? Cl2 V2 N1 C17 -96.30(18) . . . . ? V1 V2 N1 C17 97.89(18) . . . . ? O4 V2 N1 C13 -91.42(15) . . . . ? O1 V2 N1 C13 -45.4(5) . . . . ? N2 V2 N1 C13 -4.64(14) . . . . ? Cl1 V2 N1 C13 169.37(14) . . . . ? Cl2 V2 N1 C13 77.43(14) . . . . ? V1 V2 N1 C13 -88.38(15) . . . . ? O4 V2 N2 C22 -84.13(16) . . . . ? O1 V2 N2 C22 -7.45(17) . . . . ? N1 V2 N2 C22 178.24(17) . . . . ? Cl1 V2 N2 C22 150.67(18) . . . . ? Cl2 V2 N2 C22 84.30(16) . . . . ? V1 V2 N2 C22 -45.48(16) . . . . ? O4 V2 N2 C18 101.53(15) . . . . ? O1 V2 N2 C18 178.21(14) . . . . ? N1 V2 N2 C18 3.90(14) . . . . ? Cl1 V2 N2 C18 -23.7(3) . . . . ? Cl2 V2 N2 C18 -90.04(14) . . . . ? V1 V2 N2 C18 140.17(14) . . . . ? O5 V3 N3 C27 88.71(18) . . . . ? O2 V3 N3 C27 109.3(3) . . . . ? N4 V3 N3 C27 175.65(19) . . . . ? Cl3 V3 N3 C27 -14.24(18) . . . . ? Cl4 V3 N3 C27 -104.88(17) . . . . ? V1 V3 N3 C27 88.63(18) . . . . ? O5 V3 N3 C23 -86.88(15) . . . . ? O2 V3 N3 C23 -66.2(4) . . . . ? N4 V3 N3 C23 0.07(15) . . . . ? Cl3 V3 N3 C23 170.18(15) . . . . ? Cl4 V3 N3 C23 79.53(15) . . . . ? V1 V3 N3 C23 -86.95(16) . . . . ? O5 V3 N4 C32 -90.35(18) . . . . ? O2 V3 N4 C32 -13.93(18) . . . . ? N3 V3 N4 C32 176.55(19) . . . . ? Cl3 V3 N4 C32 135.06(19) . . . . ? Cl4 V3 N4 C32 77.46(17) . . . . ? V1 V3 N4 C32 -52.22(17) . . . . ? O5 V3 N4 C28 97.84(16) . . . . ? O2 V3 N4 C28 174.26(16) . . . . ? N3 V3 N4 C28 4.74(16) . . . . ? Cl3 V3 N4 C28 -36.7(3) . . . . ? Cl4 V3 N4 C28 -94.34(16) . . . . ? V1 V3 N4 C28 135.97(15) . . . . ? O6 V4 N5 C37 -82.97(17) . . . . ? O3 V4 N5 C37 -6.11(17) . . . . ? N6 V4 N5 C37 -179.19(18) . . . . ? Cl5 V4 N5 C37 167.4(2) . . . . ? Cl6 V4 N5 C37 86.81(17) . . . . ? V1 V4 N5 C37 -44.87(17) . . . . ? O6 V4 N5 C33 94.16(16) . . . . ? O3 V4 N5 C33 171.02(15) . . . . ? N6 V4 N5 C33 -2.05(15) . . . . ? Cl5 V4 N5 C33 -15.4(4) . . . . ? Cl6 V4 N5 C33 -96.06(15) . . . . ? V1 V4 N5 C33 132.26(15) . . . . ? O6 V4 N6 C42 97.84(17) . . . . ? O3 V4 N6 C42 142.7(3) . . . . ? N5 V4 N6 C42 -177.90(18) . . . . ? Cl5 V4 N6 C42 -0.10(17) . . . . ? Cl6 V4 N6 C42 -92.64(17) . . . . ? V1 V4 N6 C42 100.13(17) . . . . ? O6 V4 N6 C38 -83.83(15) . . . . ? O3 V4 N6 C38 -39.0(4) . . . . ? N5 V4 N6 C38 0.43(15) . . . . ? Cl5 V4 N6 C38 178.23(14) . . . . ? Cl6 V4 N6 C38 85.69(15) . . . . ? V1 V4 N6 C38 -81.54(16) . . . . ? V1 O1 C1 C4 -8.7(2) . . . . ? V2 O1 C1 C4 134.43(15) . . . . ? V1 O2 C2 C4 -8.9(2) . . . . ? V3 O2 C2 C4 132.63(15) . . . . ? V1 O3 C3 C4 -7.6(2) . . . . ? V4 O3 C3 C4 129.56(15) . . . . ? O2 C2 C4 C1 -57.0(2) . . . . ? O2 C2 C4 C5 -173.05(16) . . . . ? O2 C2 C4 C3 67.4(2) . . . . ? O1 C1 C4 C2 67.8(2) . . . . ? O1 C1 C4 C5 -174.39(17) . . . . ? O1 C1 C4 C3 -57.5(2) . . . . ? O3 C3 C4 C2 -57.3(2) . . . . ? O3 C3 C4 C1 67.4(2) . . . . ? O3 C3 C4 C5 -177.22(16) . . . . ? C2 C4 C5 C6 -54.9(2) . . . . ? C1 C4 C5 C6 -174.38(19) . . . . ? C3 C4 C5 C6 67.1(2) . . . . ? V2 O4 C7 C10 140.50(15) . . . . ? V1 O4 C7 C10 -8.2(2) . . . . ? V3 O5 C8 C10 141.35(14) . . . . ? V1 O5 C8 C10 -7.5(2) . . . . ? V4 O6 C9 C10 142.13(14) . . . . ? V1 O6 C9 C10 -7.9(2) . . . . ? O6 C9 C10 C8 67.6(2) . . . . ? O6 C9 C10 C11 -174.58(17) . . . . ? O6 C9 C10 C7 -57.5(2) . . . . ? O5 C8 C10 C9 -57.9(2) . . . . ? O5 C8 C10 C11 -176.12(16) . . . . ? O5 C8 C10 C7 67.9(2) . . . . ? O4 C7 C10 C9 67.2(2) . . . . ? O4 C7 C10 C8 -58.5(2) . . . . ? O4 C7 C10 C11 -174.84(17) . . . . ? C9 C10 C11 C12Y 67.0(6) . . . . ? C8 C10 C11 C12Y -172.2(6) . . . . ? C7 C10 C11 C12Y -53.5(6) . . . . ? C9 C10 C11 C12X -42.2(3) . . . . ? C8 C10 C11 C12X 78.6(3) . . . . ? C7 C10 C11 C12X -162.6(2) . . . . ? C17 N1 C13 C14 0.2(3) . . . . ? V2 N1 C13 C14 -174.07(16) . . . . ? C17 N1 C13 C18 178.98(18) . . . . ? V2 N1 C13 C18 4.7(2) . . . . ? N1 C13 C14 C15 0.5(3) . . . . ? C18 C13 C14 C15 -178.2(2) . . . . ? C13 C14 C15 C16 -0.5(4) . . . . ? C14 C15 C16 C17 -0.2(4) . . . . ? C13 N1 C17 C16 -0.9(3) . . . . ? V2 N1 C17 C16 172.78(18) . . . . ? C15 C16 C17 N1 0.9(4) . . . . ? C22 N2 C18 C19 1.9(3) . . . . ? V2 N2 C18 C19 176.41(15) . . . . ? C22 N2 C18 C13 -177.23(18) . . . . ? V2 N2 C18 C13 -2.7(2) . . . . ? N1 C13 C18 N2 -1.4(3) . . . . ? C14 C13 C18 N2 177.4(2) . . . . ? N1 C13 C18 C19 179.52(19) . . . . ? C14 C13 C18 C19 -1.7(3) . . . . ? N2 C18 C19 C20 -0.9(3) . . . . ? C13 C18 C19 C20 178.1(2) . . . . ? C18 C19 C20 C21 -0.4(3) . . . . ? C19 C20 C21 C22 0.7(3) . . . . ? C18 N2 C22 C21 -1.5(3) . . . . ? V2 N2 C22 C21 -175.78(16) . . . . ? C20 C21 C22 N2 0.2(3) . . . . ? C27 N3 C23 C24 -0.5(3) . . . . ? V3 N3 C23 C24 175.39(18) . . . . ? C27 N3 C23 C28 179.74(19) . . . . ? V3 N3 C23 C28 -4.4(2) . . . . ? N3 C23 C24 C25 -0.5(4) . . . . ? C28 C23 C24 C25 179.2(2) . . . . ? C23 C24 C25 C26 0.7(4) . . . . ? C24 C25 C26 C27 0.1(4) . . . . ? C23 N3 C27 C26 1.4(3) . . . . ? V3 N3 C27 C26 -174.19(17) . . . . ? C25 C26 C27 N3 -1.2(4) . . . . ? C32 N4 C28 C29 -2.0(3) . . . . ? V3 N4 C28 C29 170.11(19) . . . . ? C32 N4 C28 C23 179.4(2) . . . . ? V3 N4 C28 C23 -8.4(3) . . . . ? N3 C23 C28 N4 8.3(3) . . . . ? C24 C23 C28 N4 -171.4(2) . . . . ? N3 C23 C28 C29 -170.2(2) . . . . ? C24 C23 C28 C29 10.1(4) . . . . ? N4 C28 C29 C30 0.7(4) . . . . ? C23 C28 C29 C30 179.1(2) . . . . ? C28 C29 C30 C31 1.4(4) . . . . ? C29 C30 C31 C32 -2.0(4) . . . . ? C28 N4 C32 C31 1.3(4) . . . . ? V3 N4 C32 C31 -170.39(19) . . . . ? C30 C31 C32 N4 0.7(4) . . . . ? C37 N5 C33 C34 0.6(3) . . . . ? V4 N5 C33 C34 -176.66(17) . . . . ? C37 N5 C33 C38 -179.57(19) . . . . ? V4 N5 C33 C38 3.2(2) . . . . ? N5 C33 C34 C35 0.4(3) . . . . ? C38 C33 C34 C35 -179.5(2) . . . . ? C33 C34 C35 C36 -1.0(4) . . . . ? C34 C35 C36 C37 0.8(4) . . . . ? C33 N5 C37 C36 -0.8(3) . . . . ? V4 N5 C37 C36 176.30(18) . . . . ? C35 C36 C37 N5 0.1(4) . . . . ? C42 N6 C38 C39 0.2(3) . . . . ? V4 N6 C38 C39 -178.30(17) . . . . ? C42 N6 C38 C33 179.51(19) . . . . ? V4 N6 C38 C33 1.1(2) . . . . ? N5 C33 C38 N6 -2.7(3) . . . . ? C34 C33 C38 N6 177.1(2) . . . . ? N5 C33 C38 C39 176.6(2) . . . . ? C34 C33 C38 C39 -3.5(4) . . . . ? N6 C38 C39 C40 0.1(4) . . . . ? C33 C38 C39 C40 -179.2(2) . . . . ? C38 C39 C40 C41 -0.1(4) . . . . ? C39 C40 C41 C42 -0.2(4) . . . . ? C38 N6 C42 C41 -0.4(3) . . . . ? V4 N6 C42 C41 177.88(18) . . . . ? C40 C41 C42 N6 0.5(4) . . . . ? _diffrn_measured_fraction_theta_max 0.976 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.976 _refine_diff_density_max 1.077 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.094 # Attachment '6.cif' data_oejlm241sadp-1 _database_code_depnum_ccdc_archive 'CCDC 736085' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[V4Cl6(Hpeol)2(bipy)3]2.5MeCN' _chemical_formula_sum 'C45 H49.50 Cl6 N8.50 O8 V4' _chemical_formula_weight 1253.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8723(6) _cell_length_b 12.7119(6) _cell_length_c 19.8113(8) _cell_angle_alpha 83.160(4) _cell_angle_beta 77.797(4) _cell_angle_gamma 65.316(5) _cell_volume 2653.7(2) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 1030 _cell_measurement_theta_min 2.7910 _cell_measurement_theta_max 31.8477 _exptl_crystal_description needle _exptl_crystal_colour brown _exptl_crystal_size_max 0.60 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.569 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1274 _exptl_absorpt_coefficient_mu 1.043 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6235 _exptl_absorpt_correction_T_max 0.6235 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcaliber 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15443 _diffrn_reflns_av_R_equivalents 0.0273 _diffrn_reflns_av_sigmaI/netI 0.0318 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 3.09 _diffrn_reflns_theta_max 23.26 _reflns_number_total 7561 _reflns_number_gt 6112 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) ; _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 ; The structure was solved by direct methods. Data processing was carried out to 0.90 angstroms as the data was only complete to this resolution. Hydrogen atoms were included in calculated positions. In the acetonitrile molecule N8 C43 C44, the atoms C43 and C44 share the same atomic coordinates. This molecule was left isotropic. The acetonitrile molecule N9 C45 C46 is disordered over two sites. Geometric and displacement restraints were applied to the anisotropic thermal parameters of the atoms of this molecule. The hydroxyl groups O7 and O8 are disordered over two sites and were treated in a similar manner. Further splitting of hydroxyl O7 may have been beneficial but this was not done as doing so would have added no additional chemical information. The residual electron density is a result of unresolved disorder around the two split hydroxides (O7 and O8). 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^)+(0.0610P)^2^+6.5533P] 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 7561 _refine_ls_number_parameters 710 _refine_ls_number_restraints 116 _refine_ls_R_factor_all 0.0579 _refine_ls_R_factor_gt 0.0436 _refine_ls_wR_factor_ref 0.1208 _refine_ls_wR_factor_gt 0.1118 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.054 _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 0.73765(6) 0.13037(6) 0.24843(3) 0.01761(17) Uani 1 1 d . . . V2 V 0.55631(6) 0.23414(6) 0.38273(3) 0.01973(18) Uani 1 1 d . . . V3 V 0.85788(7) -0.13478(6) 0.23123(3) 0.02084(18) Uani 1 1 d . . . V4 V 0.80293(7) 0.28911(6) 0.12922(3) 0.02249(19) Uani 1 1 d . . . Cl1 Cl 0.34771(10) 0.37887(9) 0.40299(5) 0.0271(3) Uani 1 1 d . . . Cl2 Cl 0.48584(10) 0.08769(9) 0.40548(5) 0.0298(3) Uani 1 1 d . . . Cl3 Cl 0.76507(12) -0.26963(10) 0.24763(6) 0.0369(3) Uani 1 1 d . . . Cl4 Cl 0.86956(11) -0.13177(9) 0.11399(6) 0.0334(3) Uani 1 1 d . . . Cl5 Cl 0.78519(11) 0.30253(9) 0.01180(5) 0.0316(3) Uani 1 1 d . . . Cl6 Cl 0.61452(11) 0.45482(9) 0.15290(5) 0.0318(3) Uani 1 1 d . . . O1 O 0.5609(2) 0.2368(2) 0.28121(13) 0.0195(6) Uani 1 1 d . . . O2 O 0.6897(2) 0.0024(2) 0.24514(13) 0.0194(6) Uani 1 1 d . . . O3 O 0.7192(3) 0.1779(2) 0.15295(13) 0.0223(6) Uani 1 1 d . . . O4 O 0.7363(2) 0.1400(2) 0.34785(13) 0.0201(6) Uani 1 1 d . . . O5 O 0.9037(2) -0.0069(2) 0.24089(14) 0.0207(6) Uani 1 1 d . . . O6 O 0.8284(3) 0.2372(2) 0.22365(13) 0.0224(6) Uani 1 1 d . . . O7X O 0.3305(7) 0.2781(6) 0.1314(4) 0.056(2) Uani 0.427(8) 1 d PDU A 1 H7X H 0.3742 0.3022 0.1015 0.084 Uiso 0.427(8) 1 calc PR A 1 O7Y O 0.3128(11) 0.1166(8) 0.1992(7) 0.045(4) Uani 0.143(7) 1 d PDU A 2 H7Y H 0.3471 0.0480 0.2104 0.067 Uiso 0.143(7) 1 calc PR A 2 O7Z O 0.4540(7) 0.0874(7) 0.0915(4) 0.061(2) Uani 0.430(8) 1 d PDU A 3 H7Z H 0.4984 0.1116 0.0623 0.091 Uiso 0.430(8) 1 calc PR A 3 O8X O 1.1815(4) 0.0971(4) 0.2889(2) 0.0514(13) Uani 0.860(8) 1 d PDU B 1 H8X H 1.2067 0.0402 0.2653 0.077 Uiso 0.860(8) 1 calc PR B 1 O8Y O 1.1226(14) 0.0024(12) 0.3871(7) 0.045(5) Uani 0.087(7) 1 d PDU B 2 H8Y H 1.1494 -0.0578 0.3663 0.067 Uiso 0.087(7) 1 calc PR B 2 O8Z O 1.0443(19) 0.2014(13) 0.3815(7) 0.040(5) Uani 0.053(7) 1 d PDU B 3 H8Z H 0.9858 0.2079 0.4137 0.060 Uiso 0.053(7) 1 calc PR B 3 N1 N 0.6107(3) 0.3739(3) 0.38124(17) 0.0206(8) Uani 1 1 d . . . N2 N 0.5863(3) 0.2344(3) 0.48557(17) 0.0221(8) Uani 1 1 d . . . N3 N 0.8725(3) -0.1819(3) 0.33707(17) 0.0262(8) Uani 1 1 d . . . N4 N 1.0475(3) -0.2607(3) 0.22885(17) 0.0243(8) Uani 1 1 d . . . N5 N 0.9857(3) 0.1660(3) 0.09347(17) 0.0257(8) Uani 1 1 d . . . N6 N 0.9176(4) 0.3860(3) 0.11206(17) 0.0263(8) Uani 1 1 d . . . C1 C 0.4683(4) 0.2404(4) 0.2448(2) 0.0252(9) Uani 1 1 d . . . H1A H 0.4317 0.3170 0.2235 0.030 Uiso 1 1 calc R . . H1B H 0.4016 0.2272 0.2773 0.030 Uiso 1 1 calc R . . C2 C 0.5797(4) 0.0256(4) 0.2186(2) 0.0263(10) Uani 1 1 d . . . H2A H 0.5176 0.0131 0.2553 0.032 Uiso 1 1 calc R . . H2B H 0.6001 -0.0286 0.1828 0.032 Uiso 1 1 calc R . . C3 C 0.6155(4) 0.1755(4) 0.1299(2) 0.0291(10) Uani 1 1 d . . . H3A H 0.6464 0.1168 0.0956 0.035 Uiso 1 1 calc R . . H3B H 0.5718 0.2498 0.1079 0.035 Uiso 1 1 calc R . . C4 C 0.5221(4) 0.1497(4) 0.1885(2) 0.0249(9) Uani 1 1 d . A . C5 C 0.4115(4) 0.1573(4) 0.1567(2) 0.0426(11) Uani 1 1 d DU . . H5A H 0.4447 0.1061 0.1181 0.051 Uiso 1 1 calc R A 1 H5B H 0.3581 0.1291 0.1909 0.051 Uiso 1 1 calc R A 1 C6 C 0.8508(4) 0.1209(4) 0.3687(2) 0.0257(10) Uani 1 1 d . . . H6A H 0.8760 0.0504 0.3973 0.031 Uiso 1 1 calc R . . H6B H 0.8365 0.1845 0.3967 0.031 Uiso 1 1 calc R . . C7 C 1.0024(4) -0.0002(4) 0.2677(2) 0.0273(10) Uani 1 1 d . . . H7A H 1.0703 -0.0028 0.2298 0.033 Uiso 1 1 calc R . . H7B H 1.0353 -0.0670 0.2982 0.033 Uiso 1 1 calc R . . C8 C 0.9258(4) 0.2204(4) 0.2602(2) 0.0262(10) Uani 1 1 d . . . H8A H 0.8999 0.2872 0.2881 0.031 Uiso 1 1 calc R . . H8B H 1.0008 0.2155 0.2273 0.031 Uiso 1 1 calc R . . C9 C 0.9584(4) 0.1106(4) 0.3075(2) 0.0253(10) Uani 1 1 d D B . C10 C 1.0695(4) 0.1023(4) 0.3400(2) 0.0375(11) Uani 1 1 d DU . . H10A H 1.0416 0.1689 0.3683 0.045 Uiso 1 1 calc R B 1 H10B H 1.0931 0.0335 0.3702 0.045 Uiso 1 1 calc R B 1 C11 C 0.6367(4) 0.3955(3) 0.4396(2) 0.0224(9) Uani 1 1 d . . . C12 C 0.6740(4) 0.4844(4) 0.4415(2) 0.0278(10) Uani 1 1 d . . . H12 H 0.6914 0.4988 0.4822 0.033 Uiso 1 1 calc R . . C13 C 0.6851(4) 0.5514(4) 0.3826(2) 0.0319(11) Uani 1 1 d . . . H13 H 0.7110 0.6110 0.3829 0.038 Uiso 1 1 calc R . . C14 C 0.6575(4) 0.5289(4) 0.3234(2) 0.0305(11) Uani 1 1 d . . . H14 H 0.6641 0.5732 0.2831 0.037 Uiso 1 1 calc R . . C15 C 0.6200(4) 0.4400(3) 0.3244(2) 0.0244(9) Uani 1 1 d . . . H15 H 0.6005 0.4254 0.2844 0.029 Uiso 1 1 calc R . . C16 C 0.6238(4) 0.3163(3) 0.4988(2) 0.0228(9) Uani 1 1 d . . . C17 C 0.6483(4) 0.3233(4) 0.5627(2) 0.0320(11) Uani 1 1 d . . . H17 H 0.6727 0.3807 0.5707 0.038 Uiso 1 1 calc R . . C18 C 0.6361(5) 0.2440(4) 0.6147(2) 0.0396(12) Uani 1 1 d . . . H18 H 0.6530 0.2468 0.6580 0.047 Uiso 1 1 calc R . . C19 C 0.5986(5) 0.1609(4) 0.6014(2) 0.0389(12) Uani 1 1 d . . . H19 H 0.5900 0.1067 0.6357 0.047 Uiso 1 1 calc R . . C20 C 0.5739(4) 0.1588(4) 0.5371(2) 0.0294(10) Uani 1 1 d . . . H20 H 0.5476 0.1029 0.5289 0.035 Uiso 1 1 calc R . . C21 C 0.9811(4) -0.2675(4) 0.3509(2) 0.0291(10) Uani 1 1 d . . . C22 C 0.9912(5) -0.3158(5) 0.4163(3) 0.0447(13) Uani 1 1 d . . . H22 H 1.0659 -0.3757 0.4248 0.054 Uiso 1 1 calc R . . C23 C 0.8899(6) -0.2749(5) 0.4689(3) 0.0565(16) Uani 1 1 d . . . H23 H 0.8952 -0.3071 0.5134 0.068 Uiso 1 1 calc R . . C24 C 0.7799(5) -0.1853(5) 0.4552(3) 0.0486(14) Uani 1 1 d . . . H24 H 0.7108 -0.1554 0.4904 0.058 Uiso 1 1 calc R . . C25 C 0.7746(5) -0.1414(4) 0.3887(2) 0.0356(11) Uani 1 1 d . . . H25 H 0.7005 -0.0815 0.3793 0.043 Uiso 1 1 calc R . . C26 C 1.0823(4) -0.3058(3) 0.2900(2) 0.0254(10) Uani 1 1 d . . . C27 C 1.2050(4) -0.3824(4) 0.2945(3) 0.0343(11) Uani 1 1 d . . . H27 H 1.2269 -0.4130 0.3372 0.041 Uiso 1 1 calc R . . C28 C 1.2935(5) -0.4122(4) 0.2352(3) 0.0393(12) Uani 1 1 d . . . H28 H 1.3765 -0.4626 0.2372 0.047 Uiso 1 1 calc R . . C29 C 1.2582(5) -0.3665(4) 0.1725(3) 0.0376(12) Uani 1 1 d . . . H29 H 1.3167 -0.3860 0.1317 0.045 Uiso 1 1 calc R . . C30 C 1.1354(4) -0.2917(4) 0.1714(2) 0.0291(10) Uani 1 1 d . . . H30 H 1.1120 -0.2613 0.1289 0.035 Uiso 1 1 calc R . . C31 C 1.0793(4) 0.2026(4) 0.0760(2) 0.0266(10) Uani 1 1 d . . . C32 C 1.2012(5) 0.1274(5) 0.0513(2) 0.0398(12) Uani 1 1 d . . . H32 H 1.2655 0.1536 0.0400 0.048 Uiso 1 1 calc R . . C33 C 1.2264(5) 0.0129(5) 0.0437(2) 0.0434(13) Uani 1 1 d . . . H33 H 1.3083 -0.0393 0.0279 0.052 Uiso 1 1 calc R . . C34 C 1.1312(5) -0.0230(4) 0.0593(2) 0.0409(13) Uani 1 1 d . . . H34 H 1.1465 -0.0995 0.0532 0.049 Uiso 1 1 calc R . . C35 C 1.0119(5) 0.0548(4) 0.0842(2) 0.0329(11) Uani 1 1 d . . . H35 H 0.9469 0.0297 0.0951 0.039 Uiso 1 1 calc R . . C36 C 1.0399(4) 0.3276(4) 0.0841(2) 0.0294(10) Uani 1 1 d . . . C37 C 1.1198(5) 0.3841(5) 0.0638(2) 0.0409(13) Uani 1 1 d . . . H37 H 1.2036 0.3430 0.0441 0.049 Uiso 1 1 calc R . . C38 C 1.0751(6) 0.5010(5) 0.0728(3) 0.0507(15) Uani 1 1 d . . . H38 H 1.1278 0.5398 0.0586 0.061 Uiso 1 1 calc R . . C39 C 0.9526(6) 0.5594(4) 0.1027(3) 0.0477(15) Uani 1 1 d . . . H39 H 0.9208 0.6383 0.1101 0.057 Uiso 1 1 calc R . . C40 C 0.8766(5) 0.4996(4) 0.1215(2) 0.0373(12) Uani 1 1 d . . . H40 H 0.7930 0.5398 0.1418 0.045 Uiso 1 1 calc R . . N7 N -0.0089(7) 0.4115(6) 0.3881(4) 0.095(2) Uani 1 1 d . . . C41 C 0.0379(7) 0.4135(6) 0.3321(5) 0.0672(18) Uani 1 1 d . . . C42 C 0.0938(8) 0.4095(7) 0.2624(4) 0.088(2) Uani 1 1 d . . . H42A H 0.1340 0.3305 0.2486 0.132 Uiso 1 1 calc R . . H42B H 0.1553 0.4420 0.2557 0.132 Uiso 1 1 calc R . . H42C H 0.0303 0.4532 0.2350 0.132 Uiso 1 1 calc R . . N8 N 0.5652(10) 0.6298(9) 0.9868(5) 0.061(3) Uiso 0.50 1 d P . . C43 C 0.5240(8) 0.5444(7) 0.9935(4) 0.093(2) Uiso 0.50 1 d PU . 1 C44 C 0.5240(8) 0.5444(7) 0.9935(4) 0.093(2) Uiso 0.50 1 d PU . 2 H44A H 0.4565 0.6181 1.0054 0.139 Uiso 0.50 1 calc PR . 2 H44B H 0.5599 0.5465 0.9454 0.139 Uiso 0.50 1 calc PR . 2 H44C H 0.5875 0.5278 1.0209 0.139 Uiso 0.50 1 calc PR . 2 N9X N 0.3458(6) 0.8850(6) 0.2220(3) 0.0500(17) Uani 0.727(7) 1 d PDU C 1 C45X C 0.4340(7) 0.8375(7) 0.1809(4) 0.0494(17) Uani 0.727(7) 1 d PDU C 1 C46X C 0.5425(8) 0.7863(9) 0.1278(5) 0.068(2) Uani 0.727(7) 1 d PDU C 1 H46A H 0.5365 0.8381 0.0880 0.103 Uiso 0.727(7) 1 calc PR C 1 H46B H 0.5457 0.7143 0.1152 0.103 Uiso 0.727(7) 1 calc PR C 1 H46C H 0.6176 0.7723 0.1449 0.103 Uiso 0.727(7) 1 calc PR C 1 N9Y N 0.5506(14) 0.7753(16) 0.0248(9) 0.060(4) Uani 0.273(7) 1 d PDU C 2 C45Y C 0.526(2) 0.778(2) 0.0866(9) 0.063(4) Uani 0.273(7) 1 d PDU C 2 C46Y C 0.505(3) 0.768(2) 0.1608(9) 0.061(3) Uani 0.273(7) 1 d PDU C 2 H46D H 0.4971 0.6961 0.1755 0.092 Uiso 0.273(7) 1 calc PR C 2 H46E H 0.4293 0.8314 0.1793 0.092 Uiso 0.273(7) 1 calc PR C 2 H46F H 0.5750 0.7692 0.1772 0.092 Uiso 0.273(7) 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0224(4) 0.0183(4) 0.0143(3) -0.0001(3) 0.0010(3) -0.0125(3) V2 0.0255(4) 0.0208(4) 0.0142(4) -0.0017(3) 0.0030(3) -0.0134(3) V3 0.0265(4) 0.0173(4) 0.0185(4) 0.0004(3) 0.0014(3) -0.0114(3) V4 0.0308(4) 0.0173(4) 0.0162(4) -0.0005(3) 0.0070(3) -0.0119(3) Cl1 0.0305(6) 0.0240(5) 0.0238(5) -0.0040(4) 0.0005(4) -0.0099(5) Cl2 0.0361(6) 0.0280(6) 0.0244(5) 0.0000(4) 0.0049(5) -0.0172(5) Cl3 0.0516(7) 0.0293(6) 0.0375(6) 0.0042(5) -0.0002(5) -0.0289(6) Cl4 0.0474(7) 0.0259(6) 0.0265(6) 0.0000(4) -0.0012(5) -0.0171(5) Cl5 0.0490(7) 0.0268(6) 0.0172(5) -0.0023(4) 0.0073(5) -0.0193(5) Cl6 0.0339(6) 0.0287(6) 0.0200(5) -0.0035(4) 0.0047(4) -0.0041(5) O1 0.0231(15) 0.0225(14) 0.0156(14) -0.0003(11) -0.0008(11) -0.0131(12) O2 0.0208(15) 0.0213(14) 0.0196(14) 0.0004(11) -0.0011(12) -0.0133(12) O3 0.0272(16) 0.0261(15) 0.0163(14) 0.0025(12) -0.0002(12) -0.0160(13) O4 0.0236(15) 0.0224(15) 0.0164(14) -0.0026(11) 0.0014(12) -0.0133(12) O5 0.0192(15) 0.0220(14) 0.0213(15) -0.0006(11) 0.0006(12) -0.0110(12) O6 0.0279(16) 0.0253(15) 0.0171(14) 0.0002(12) 0.0014(12) -0.0166(13) O7X 0.054(5) 0.070(4) 0.056(5) -0.002(4) -0.022(4) -0.032(4) O7Y 0.032(7) 0.086(8) 0.032(7) 0.011(7) -0.020(6) -0.037(6) O7Z 0.024(4) 0.135(6) 0.036(4) -0.024(4) -0.012(3) -0.037(4) O8X 0.046(2) 0.080(3) 0.047(2) -0.005(2) -0.0007(17) -0.046(2) O8Y 0.031(8) 0.044(8) 0.065(8) -0.006(5) -0.022(7) -0.014(7) O8Z 0.033(9) 0.051(8) 0.046(9) -0.009(6) -0.004(8) -0.026(8) N1 0.0245(19) 0.0188(17) 0.0176(18) -0.0035(14) 0.0048(14) -0.0111(15) N2 0.029(2) 0.0209(18) 0.0168(18) -0.0018(14) 0.0034(15) -0.0136(16) N3 0.031(2) 0.0255(19) 0.0191(19) 0.0024(15) 0.0030(16) -0.0123(17) N4 0.029(2) 0.0178(17) 0.024(2) -0.0007(15) 0.0015(16) -0.0100(16) N5 0.034(2) 0.0213(19) 0.0182(18) -0.0017(14) 0.0056(15) -0.0128(17) N6 0.041(2) 0.0200(19) 0.0177(18) -0.0017(14) 0.0062(16) -0.0178(17) C1 0.025(2) 0.028(2) 0.023(2) 0.0002(18) -0.0040(18) -0.0121(19) C2 0.027(2) 0.026(2) 0.031(2) -0.0020(19) -0.0033(19) -0.016(2) C3 0.035(3) 0.037(3) 0.020(2) 0.0027(19) -0.0056(19) -0.021(2) C4 0.032(2) 0.030(2) 0.018(2) 0.0003(18) -0.0053(18) -0.019(2) C5 0.035(3) 0.073(3) 0.031(2) -0.001(2) -0.008(2) -0.032(2) C6 0.027(2) 0.030(2) 0.025(2) -0.0008(18) -0.0071(19) -0.014(2) C7 0.022(2) 0.032(2) 0.031(2) -0.0021(19) -0.0007(19) -0.015(2) C8 0.030(2) 0.030(2) 0.026(2) -0.0049(18) 0.0009(19) -0.021(2) C9 0.026(2) 0.031(2) 0.024(2) -0.0020(18) -0.0025(18) -0.018(2) C10 0.033(2) 0.049(3) 0.040(3) -0.006(2) -0.0050(17) -0.025(2) C11 0.022(2) 0.024(2) 0.020(2) -0.0051(17) 0.0051(17) -0.0119(19) C12 0.035(3) 0.031(2) 0.023(2) -0.0086(19) 0.0029(19) -0.020(2) C13 0.041(3) 0.029(2) 0.032(3) -0.002(2) 0.002(2) -0.024(2) C14 0.044(3) 0.026(2) 0.023(2) -0.0014(19) 0.009(2) -0.023(2) C15 0.032(2) 0.025(2) 0.016(2) -0.0027(17) 0.0044(18) -0.014(2) C16 0.023(2) 0.024(2) 0.019(2) -0.0016(17) 0.0028(17) -0.0097(19) C17 0.043(3) 0.035(3) 0.027(2) -0.003(2) -0.004(2) -0.024(2) C18 0.061(3) 0.045(3) 0.022(2) 0.003(2) -0.012(2) -0.029(3) C19 0.061(3) 0.042(3) 0.022(2) 0.008(2) -0.007(2) -0.031(3) C20 0.043(3) 0.030(2) 0.021(2) 0.0027(19) -0.002(2) -0.023(2) C21 0.030(3) 0.029(2) 0.026(2) 0.0021(19) -0.0035(19) -0.011(2) C22 0.044(3) 0.051(3) 0.030(3) 0.013(2) -0.008(2) -0.014(3) C23 0.063(4) 0.071(4) 0.026(3) 0.019(3) -0.011(3) -0.021(3) C24 0.051(3) 0.060(4) 0.023(3) 0.005(2) 0.006(2) -0.018(3) C25 0.033(3) 0.036(3) 0.029(3) 0.001(2) 0.005(2) -0.011(2) C26 0.031(3) 0.020(2) 0.025(2) -0.0015(18) -0.0008(19) -0.013(2) C27 0.037(3) 0.028(2) 0.038(3) -0.001(2) -0.011(2) -0.011(2) C28 0.026(3) 0.031(3) 0.052(3) -0.012(2) -0.001(2) -0.003(2) C29 0.032(3) 0.037(3) 0.037(3) -0.013(2) 0.008(2) -0.011(2) C30 0.032(3) 0.025(2) 0.026(2) -0.0059(19) 0.006(2) -0.011(2) C31 0.032(3) 0.032(2) 0.014(2) -0.0027(18) 0.0002(18) -0.014(2) C32 0.029(3) 0.056(3) 0.031(3) -0.014(2) 0.000(2) -0.014(2) C33 0.040(3) 0.045(3) 0.027(3) -0.009(2) -0.005(2) 0.002(3) C34 0.060(4) 0.021(2) 0.025(3) -0.004(2) 0.003(2) -0.005(2) C35 0.051(3) 0.023(2) 0.020(2) -0.0033(18) 0.008(2) -0.017(2) C36 0.041(3) 0.035(3) 0.018(2) -0.0029(19) 0.003(2) -0.023(2) C37 0.047(3) 0.062(3) 0.027(3) -0.011(2) 0.006(2) -0.039(3) C38 0.087(5) 0.062(4) 0.032(3) -0.005(3) 0.005(3) -0.064(4) C39 0.091(5) 0.036(3) 0.029(3) -0.003(2) 0.001(3) -0.043(3) C40 0.059(3) 0.025(2) 0.028(3) -0.003(2) 0.005(2) -0.023(2) N7 0.086(5) 0.104(5) 0.093(5) 0.003(4) -0.042(4) -0.026(4) C41 0.060(4) 0.068(4) 0.085(6) -0.004(4) -0.024(4) -0.031(4) C42 0.090(6) 0.098(6) 0.107(7) -0.008(5) -0.007(5) -0.072(5) N9X 0.059(4) 0.062(4) 0.044(4) 0.014(3) -0.019(2) -0.039(3) C45X 0.051(4) 0.052(4) 0.060(4) 0.001(3) -0.025(2) -0.029(3) C46X 0.063(4) 0.064(4) 0.077(5) -0.007(4) -0.013(3) -0.023(4) N9Y 0.023(7) 0.070(8) 0.072(6) 0.024(7) 0.009(6) -0.021(6) C45Y 0.049(6) 0.062(6) 0.074(6) 0.007(6) -0.007(6) -0.023(5) C46Y 0.058(6) 0.055(6) 0.073(6) 0.000(6) -0.011(5) -0.026(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O3 1.945(3) . ? V1 O2 1.947(3) . ? V1 O1 1.979(3) . ? V1 O4 1.984(3) . ? V1 O5 2.004(3) . ? V1 O6 2.021(3) . ? V1 V2 3.0817(9) . ? V1 V3 3.0926(9) . ? V1 V4 3.1059(9) . ? V2 O4 1.978(3) . ? V2 O1 1.997(3) . ? V2 N1 2.124(3) . ? V2 N2 2.142(3) . ? V2 Cl2 2.3045(12) . ? V2 Cl1 2.3726(13) . ? V3 O5 1.958(3) . ? V3 O2 2.019(3) . ? V3 N3 2.134(3) . ? V3 N4 2.144(4) . ? V3 Cl4 2.2940(13) . ? V3 Cl3 2.3562(13) . ? V4 O6 1.951(3) . ? V4 O3 2.006(3) . ? V4 N5 2.107(4) . ? V4 N6 2.143(3) . ? V4 Cl6 2.3489(13) . ? V4 Cl5 2.3595(13) . ? O1 C1 1.419(5) . ? O2 C2 1.415(5) . ? O3 C3 1.413(5) . ? O4 C6 1.419(5) . ? O5 C7 1.421(5) . ? O6 C8 1.421(5) . ? O7X C5 1.524(6) . ? O7X H7X 0.8200 . ? O7Y C5 1.527(7) . ? O7Y H7Y 0.8200 . ? O7Z C5 1.529(6) . ? O7Z H7Z 0.8200 . ? O8X C10 1.474(5) . ? O8X H8X 0.8200 . ? O8Y C10 1.475(6) . ? O8Y H8Y 0.8200 . ? O8Z C10 1.476(6) . ? O8Z H8Z 0.8200 . ? N1 C15 1.335(5) . ? N1 C11 1.344(5) . ? N2 C20 1.345(5) . ? N2 C16 1.362(5) . ? N3 C25 1.336(6) . ? N3 C21 1.352(6) . ? N4 C30 1.342(5) . ? N4 C26 1.347(6) . ? N5 C35 1.340(5) . ? N5 C31 1.342(6) . ? N6 C40 1.340(5) . ? N6 C36 1.350(6) . ? C1 C4 1.540(6) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 C4 1.537(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.534(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C4 C5 1.536(6) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C6 C9 1.538(6) . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C9 1.536(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C8 C9 1.537(6) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.548(6) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.381(6) . ? C11 C16 1.479(6) . ? C12 C13 1.377(6) . ? C12 H12 0.9300 . ? C13 C14 1.373(6) . ? C13 H13 0.9300 . ? C14 C15 1.373(6) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 C17 1.377(6) . ? C17 C18 1.382(6) . ? C17 H17 0.9300 . ? C18 C19 1.376(7) . ? C18 H18 0.9300 . ? C19 C20 1.371(6) . ? C19 H19 0.9300 . ? C20 H20 0.9300 . ? C21 C22 1.373(6) . ? C21 C26 1.474(6) . ? C22 C23 1.371(8) . ? C22 H22 0.9300 . ? C23 C24 1.382(8) . ? C23 H23 0.9300 . ? C24 C25 1.371(7) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 C27 1.389(6) . ? C27 C28 1.372(7) . ? C27 H27 0.9300 . ? C28 C29 1.377(7) . ? C28 H28 0.9300 . ? C29 C30 1.372(7) . ? C29 H29 0.9300 . ? C30 H30 0.9300 . ? C31 C32 1.380(6) . ? C31 C36 1.476(6) . ? C32 C33 1.379(7) . ? C32 H32 0.9300 . ? C33 C34 1.354(8) . ? C33 H33 0.9300 . ? C34 C35 1.370(7) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C37 1.385(6) . ? C37 C38 1.373(7) . ? C37 H37 0.9300 . ? C38 C39 1.363(8) . ? C38 H38 0.9300 . ? C39 C40 1.376(7) . ? C39 H39 0.9300 . ? C40 H40 0.9300 . ? N7 C41 1.134(9) . ? C41 C42 1.397(11) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? N8 C43 1.348(12) . ? C43 C43 1.439(16) 2_667 ? N9X C45X 1.164(7) . ? C45X C46X 1.442(8) . ? C46X H46A 0.9600 . ? C46X H46B 0.9600 . ? C46X H46C 0.9600 . ? N9Y C45Y 1.199(9) . ? C45Y C46Y 1.437(9) . ? C46Y H46D 0.9600 . ? C46Y H46E 0.9600 . ? C46Y H46F 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O3 V1 O2 92.09(11) . . ? O3 V1 O1 90.81(11) . . ? O2 V1 O1 91.92(11) . . ? O3 V1 O4 160.32(11) . . ? O2 V1 O4 104.32(11) . . ? O1 V1 O4 78.07(11) . . ? O3 V1 O5 104.03(11) . . ? O2 V1 O5 77.64(11) . . ? O1 V1 O5 162.02(11) . . ? O4 V1 O5 90.24(11) . . ? O3 V1 O6 76.58(11) . . ? O2 V1 O6 160.82(11) . . ? O1 V1 O6 103.51(11) . . ? O4 V1 O6 90.15(11) . . ? O5 V1 O6 89.98(11) . . ? O3 V1 V2 129.30(9) . . ? O2 V1 V2 97.29(8) . . ? O1 V1 V2 39.41(8) . . ? O4 V1 V2 38.88(8) . . ? O5 V1 V2 126.66(8) . . ? O6 V1 V2 101.86(8) . . ? O3 V1 V3 98.19(8) . . ? O2 V1 V3 39.60(8) . . ? O1 V1 V3 130.59(8) . . ? O4 V1 V3 101.38(8) . . ? O5 V1 V3 38.16(8) . . ? O6 V1 V3 125.86(8) . . ? V2 V1 V3 120.05(3) . . ? O3 V1 V4 38.87(8) . . ? O2 V1 V4 129.68(8) . . ? O1 V1 V4 97.78(8) . . ? O4 V1 V4 125.99(8) . . ? O5 V1 V4 100.15(8) . . ? O6 V1 V4 37.76(8) . . ? V2 V1 V4 120.78(3) . . ? V3 V1 V4 119.16(3) . . ? O4 V2 O1 77.79(11) . . ? O4 V2 N1 86.10(12) . . ? O1 V2 N1 96.74(12) . . ? O4 V2 N2 93.36(12) . . ? O1 V2 N2 168.67(12) . . ? N1 V2 N2 75.40(12) . . ? O4 V2 Cl2 98.82(8) . . ? O1 V2 Cl2 93.22(8) . . ? N1 V2 Cl2 169.64(9) . . ? N2 V2 Cl2 95.13(9) . . ? O4 V2 Cl1 166.18(8) . . ? O1 V2 Cl1 93.08(8) . . ? N1 V2 Cl1 84.69(9) . . ? N2 V2 Cl1 94.27(10) . . ? Cl2 V2 Cl1 91.96(4) . . ? O4 V2 V1 39.02(8) . . ? O1 V2 V1 38.99(8) . . ? N1 V2 V1 94.98(9) . . ? N2 V2 V1 132.34(10) . . ? Cl2 V2 V1 94.55(4) . . ? Cl1 V2 V1 131.85(4) . . ? O5 V3 O2 77.05(11) . . ? O5 V3 N3 88.02(12) . . ? O2 V3 N3 98.62(12) . . ? O5 V3 N4 92.48(12) . . ? O2 V3 N4 168.14(12) . . ? N3 V3 N4 75.17(13) . . ? O5 V3 Cl4 101.75(9) . . ? O2 V3 Cl4 93.39(8) . . ? N3 V3 Cl4 166.00(10) . . ? N4 V3 Cl4 94.20(10) . . ? O5 V3 Cl3 164.50(9) . . ? O2 V3 Cl3 93.16(8) . . ? N3 V3 Cl3 81.54(10) . . ? N4 V3 Cl3 95.85(10) . . ? Cl4 V3 Cl3 90.68(5) . . ? O5 V3 V1 39.23(8) . . ? O2 V3 V1 37.93(7) . . ? N3 V3 V1 96.55(10) . . ? N4 V3 V1 131.67(9) . . ? Cl4 V3 V1 97.35(4) . . ? Cl3 V3 V1 130.58(4) . . ? O6 V4 O3 76.82(11) . . ? O6 V4 N5 88.76(13) . . ? O3 V4 N5 96.96(12) . . ? O6 V4 N6 96.02(12) . . ? O3 V4 N6 170.20(13) . . ? N5 V4 N6 75.97(13) . . ? O6 V4 Cl6 99.17(9) . . ? O3 V4 Cl6 94.51(9) . . ? N5 V4 Cl6 167.31(10) . . ? N6 V4 Cl6 93.24(10) . . ? O6 V4 Cl5 165.67(9) . . ? O3 V4 Cl5 92.46(8) . . ? N5 V4 Cl5 83.07(10) . . ? N6 V4 Cl5 93.39(10) . . ? Cl6 V4 Cl5 91.04(5) . . ? O6 V4 V1 39.38(8) . . ? O3 V4 V1 37.48(8) . . ? N5 V4 V1 95.17(9) . . ? N6 V4 V1 135.24(10) . . ? Cl6 V4 V1 97.24(4) . . ? Cl5 V4 V1 129.58(4) . . ? C1 O1 V1 117.5(2) . . ? C1 O1 V2 130.0(2) . . ? V1 O1 V2 101.60(12) . . ? C2 O2 V1 118.1(2) . . ? C2 O2 V3 129.8(2) . . ? V1 O2 V3 102.47(12) . . ? C3 O3 V1 118.0(2) . . ? C3 O3 V4 130.5(2) . . ? V1 O3 V4 103.64(13) . . ? C6 O4 V2 134.3(2) . . ? C6 O4 V1 118.6(2) . . ? V2 O4 V1 102.10(12) . . ? C7 O5 V3 133.2(2) . . ? C7 O5 V1 118.8(2) . . ? V3 O5 V1 102.62(12) . . ? C8 O6 V4 133.3(2) . . ? C8 O6 V1 117.7(2) . . ? V4 O6 V1 102.86(13) . . ? C5 O7X H7X 109.5 . . ? C5 O7Y H7Y 109.5 . . ? C5 O7Z H7Z 109.5 . . ? C10 O8X H8X 109.5 . . ? C10 O8Y H8Y 109.5 . . ? C10 O8Z H8Z 109.5 . . ? C15 N1 C11 119.4(3) . . ? C15 N1 V2 122.2(3) . . ? C11 N1 V2 118.4(3) . . ? C20 N2 C16 117.9(4) . . ? C20 N2 V2 125.3(3) . . ? C16 N2 V2 116.8(3) . . ? C25 N3 C21 119.1(4) . . ? C25 N3 V3 122.7(3) . . ? C21 N3 V3 117.6(3) . . ? C30 N4 C26 118.1(4) . . ? C30 N4 V3 124.6(3) . . ? C26 N4 V3 117.2(3) . . ? C35 N5 C31 118.6(4) . . ? C35 N5 V4 123.4(3) . . ? C31 N5 V4 117.9(3) . . ? C40 N6 C36 118.1(4) . . ? C40 N6 V4 125.8(3) . . ? C36 N6 V4 115.8(3) . . ? O1 C1 C4 112.8(3) . . ? O1 C1 H1A 109.0 . . ? C4 C1 H1A 109.0 . . ? O1 C1 H1B 109.0 . . ? C4 C1 H1B 109.0 . . ? H1A C1 H1B 107.8 . . ? O2 C2 C4 113.0(3) . . ? O2 C2 H2A 109.0 . . ? C4 C2 H2A 109.0 . . ? O2 C2 H2B 109.0 . . ? C4 C2 H2B 109.0 . . ? H2A C2 H2B 107.8 . . ? O3 C3 C4 113.1(3) . . ? O3 C3 H3A 109.0 . . ? C4 C3 H3A 109.0 . . ? O3 C3 H3B 109.0 . . ? C4 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C3 C4 C5 107.1(3) . . ? C3 C4 C2 111.8(4) . . ? C5 C4 C2 106.3(3) . . ? C3 C4 C1 111.7(3) . . ? C5 C4 C1 107.5(4) . . ? C2 C4 C1 112.0(3) . . ? O7X C5 O7Y 102.3(4) . . ? O7X C5 O7Z 102.3(4) . . ? O7Y C5 O7Z 102.2(4) . . ? O7X C5 C4 115.1(5) . . ? O7Y C5 C4 119.8(8) . . ? O7Z C5 C4 113.0(4) . . ? O7X C5 H5A 108.5 . . ? O7Y C5 H5A 101.5 . . ? O7Z C5 H5A 6.3 . . ? C4 C5 H5A 108.5 . . ? O7X C5 H5B 108.5 . . ? O7Y C5 H5B 11.3 . . ? O7Z C5 H5B 109.2 . . ? C4 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? O4 C6 C9 113.1(3) . . ? O4 C6 H6A 109.0 . . ? C9 C6 H6A 109.0 . . ? O4 C6 H6B 109.0 . . ? C9 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? O5 C7 C9 112.4(3) . . ? O5 C7 H7A 109.1 . . ? C9 C7 H7A 109.1 . . ? O5 C7 H7B 109.1 . . ? C9 C7 H7B 109.1 . . ? H7A C7 H7B 107.9 . . ? O6 C8 C9 113.2(3) . . ? O6 C8 H8A 108.9 . . ? C9 C8 H8A 108.9 . . ? O6 C8 H8B 108.9 . . ? C9 C8 H8B 108.9 . . ? H8A C8 H8B 107.8 . . ? C7 C9 C8 112.7(3) . . ? C7 C9 C6 112.3(3) . . ? C8 C9 C6 111.9(3) . . ? C7 C9 C10 107.5(3) . . ? C8 C9 C10 106.4(3) . . ? C6 C9 C10 105.4(3) . . ? O8X C10 O8Y 102.6(6) . . ? O8X C10 O8Z 102.4(6) . . ? O8Y C10 O8Z 102.4(6) . . ? O8X C10 C9 113.8(4) . . ? O8Y C10 C9 118.1(8) . . ? O8Z C10 C9 115.5(8) . . ? O8X C10 H10A 108.8 . . ? O8Y C10 H10A 104.0 . . ? O8Z C10 H10A 7.4 . . ? C9 C10 H10A 108.8 . . ? O8X C10 H10B 108.8 . . ? O8Y C10 H10B 9.4 . . ? O8Z C10 H10B 107.2 . . ? C9 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? N1 C11 C12 121.0(4) . . ? N1 C11 C16 114.5(3) . . ? C12 C11 C16 124.5(4) . . ? C13 C12 C11 119.5(4) . . ? C13 C12 H12 120.3 . . ? C11 C12 H12 120.3 . . ? C14 C13 C12 119.0(4) . . ? C14 C13 H13 120.5 . . ? C12 C13 H13 120.5 . . ? C15 C14 C13 119.2(4) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? N1 C15 C14 121.9(4) . . ? N1 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? N2 C16 C17 122.0(4) . . ? N2 C16 C11 114.8(4) . . ? C17 C16 C11 123.2(4) . . ? C16 C17 C18 119.1(4) . . ? C16 C17 H17 120.4 . . ? C18 C17 H17 120.4 . . ? C19 C18 C17 119.1(4) . . ? C19 C18 H18 120.5 . . ? C17 C18 H18 120.5 . . ? C20 C19 C18 119.3(4) . . ? C20 C19 H19 120.3 . . ? C18 C19 H19 120.3 . . ? N2 C20 C19 122.6(4) . . ? N2 C20 H20 118.7 . . ? C19 C20 H20 118.7 . . ? N3 C21 C22 121.3(4) . . ? N3 C21 C26 114.4(4) . . ? C22 C21 C26 124.3(4) . . ? C23 C22 C21 119.4(5) . . ? C23 C22 H22 120.3 . . ? C21 C22 H22 120.3 . . ? C22 C23 C24 119.3(5) . . ? C22 C23 H23 120.3 . . ? C24 C23 H23 120.3 . . ? C25 C24 C23 118.8(5) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? N3 C25 C24 122.1(5) . . ? N3 C25 H25 118.9 . . ? C24 C25 H25 118.9 . . ? N4 C26 C27 121.8(4) . . ? N4 C26 C21 115.1(4) . . ? C27 C26 C21 123.1(4) . . ? C28 C27 C26 119.1(5) . . ? C28 C27 H27 120.5 . . ? C26 C27 H27 120.5 . . ? C27 C28 C29 119.2(5) . . ? C27 C28 H28 120.4 . . ? C29 C28 H28 120.4 . . ? C30 C29 C28 119.0(4) . . ? C30 C29 H29 120.5 . . ? C28 C29 H29 120.5 . . ? N4 C30 C29 122.8(4) . . ? N4 C30 H30 118.6 . . ? C29 C30 H30 118.6 . . ? N5 C31 C32 121.3(4) . . ? N5 C31 C36 114.6(4) . . ? C32 C31 C36 124.0(4) . . ? C33 C32 C31 119.0(5) . . ? C33 C32 H32 120.5 . . ? C31 C32 H32 120.5 . . ? C34 C33 C32 119.5(5) . . ? C34 C33 H33 120.2 . . ? C32 C33 H33 120.2 . . ? C33 C34 C35 119.2(5) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? N5 C35 C34 122.3(5) . . ? N5 C35 H35 118.8 . . ? C34 C35 H35 118.8 . . ? N6 C36 C37 121.0(4) . . ? N6 C36 C31 115.4(4) . . ? C37 C36 C31 123.6(4) . . ? C38 C37 C36 119.8(5) . . ? C38 C37 H37 120.1 . . ? C36 C37 H37 120.1 . . ? C39 C38 C37 119.2(5) . . ? C39 C38 H38 120.4 . . ? C37 C38 H38 120.4 . . ? C38 C39 C40 118.8(5) . . ? C38 C39 H39 120.6 . . ? C40 C39 H39 120.6 . . ? N6 C40 C39 123.0(5) . . ? N6 C40 H40 118.5 . . ? C39 C40 H40 118.5 . . ? N7 C41 C42 176.1(8) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N8 C43 C43 175.2(12) . 2_667 ? N9X C45X C46X 176.1(9) . . ? C45X C46X H46A 109.5 . . ? C45X C46X H46B 109.5 . . ? H46A C46X H46B 109.5 . . ? C45X C46X H46C 109.5 . . ? H46A C46X H46C 109.5 . . ? H46B C46X H46C 109.5 . . ? N9Y C45Y C46Y 174(3) . . ? C45Y C46Y H46D 109.5 . . ? C45Y C46Y H46E 109.5 . . ? H46D C46Y H46E 109.5 . . ? C45Y C46Y H46F 109.5 . . ? H46D C46Y H46F 109.5 . . ? H46E C46Y H46F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 V1 V2 O4 -157.43(16) . . . . ? O2 V1 V2 O4 103.81(14) . . . . ? O1 V1 V2 O4 -172.08(17) . . . . ? O5 V1 V2 O4 23.81(15) . . . . ? O6 V1 V2 O4 -75.16(14) . . . . ? V3 V1 V2 O4 69.23(12) . . . . ? V4 V1 V2 O4 -110.55(12) . . . . ? O3 V1 V2 O1 14.65(16) . . . . ? O2 V1 V2 O1 -84.11(14) . . . . ? O4 V1 V2 O1 172.08(17) . . . . ? O5 V1 V2 O1 -164.11(15) . . . . ? O6 V1 V2 O1 96.92(14) . . . . ? V3 V1 V2 O1 -118.68(12) . . . . ? V4 V1 V2 O1 61.53(12) . . . . ? O3 V1 V2 N1 -79.91(14) . . . . ? O2 V1 V2 N1 -178.67(12) . . . . ? O1 V1 V2 N1 -94.56(15) . . . . ? O4 V1 V2 N1 77.52(15) . . . . ? O5 V1 V2 N1 101.33(13) . . . . ? O6 V1 V2 N1 2.36(13) . . . . ? V3 V1 V2 N1 146.76(10) . . . . ? V4 V1 V2 N1 -33.03(10) . . . . ? O3 V1 V2 N2 -154.67(16) . . . . ? O2 V1 V2 N2 106.57(14) . . . . ? O1 V1 V2 N2 -169.32(17) . . . . ? O4 V1 V2 N2 2.76(16) . . . . ? O5 V1 V2 N2 26.57(16) . . . . ? O6 V1 V2 N2 -72.40(15) . . . . ? V3 V1 V2 N2 71.99(12) . . . . ? V4 V1 V2 N2 -107.79(12) . . . . ? O3 V1 V2 Cl2 104.15(11) . . . . ? O2 V1 V2 Cl2 5.39(9) . . . . ? O1 V1 V2 Cl2 89.50(12) . . . . ? O4 V1 V2 Cl2 -98.41(12) . . . . ? O5 V1 V2 Cl2 -74.61(10) . . . . ? O6 V1 V2 Cl2 -173.57(9) . . . . ? V3 V1 V2 Cl2 -29.18(5) . . . . ? V4 V1 V2 Cl2 151.04(4) . . . . ? O3 V1 V2 Cl1 7.42(12) . . . . ? O2 V1 V2 Cl1 -91.34(9) . . . . ? O1 V1 V2 Cl1 -7.23(12) . . . . ? O4 V1 V2 Cl1 164.85(13) . . . . ? O5 V1 V2 Cl1 -171.34(10) . . . . ? O6 V1 V2 Cl1 89.69(10) . . . . ? V3 V1 V2 Cl1 -125.91(5) . . . . ? V4 V1 V2 Cl1 54.30(6) . . . . ? O3 V1 V3 O5 102.31(15) . . . . ? O2 V1 V3 O5 -174.35(17) . . . . ? O1 V1 V3 O5 -159.52(16) . . . . ? O4 V1 V3 O5 -75.57(15) . . . . ? O6 V1 V3 O5 22.99(16) . . . . ? V2 V1 V3 O5 -112.34(13) . . . . ? V4 V1 V3 O5 67.44(13) . . . . ? O3 V1 V3 O2 -83.34(15) . . . . ? O1 V1 V3 O2 14.83(16) . . . . ? O4 V1 V3 O2 98.78(15) . . . . ? O5 V1 V3 O2 174.35(17) . . . . ? O6 V1 V3 O2 -162.66(16) . . . . ? V2 V1 V3 O2 62.01(12) . . . . ? V4 V1 V3 O2 -118.20(12) . . . . ? O3 V1 V3 N3 -178.97(13) . . . . ? O2 V1 V3 N3 -95.64(16) . . . . ? O1 V1 V3 N3 -80.81(14) . . . . ? O4 V1 V3 N3 3.15(13) . . . . ? O5 V1 V3 N3 78.72(16) . . . . ? O6 V1 V3 N3 101.70(14) . . . . ? V2 V1 V3 N3 -33.63(10) . . . . ? V4 V1 V3 N3 146.16(10) . . . . ? O3 V1 V3 N4 105.07(15) . . . . ? O2 V1 V3 N4 -171.59(18) . . . . ? O1 V1 V3 N4 -156.76(16) . . . . ? O4 V1 V3 N4 -72.81(15) . . . . ? O5 V1 V3 N4 2.76(17) . . . . ? O6 V1 V3 N4 25.75(16) . . . . ? V2 V1 V3 N4 -109.58(13) . . . . ? V4 V1 V3 N4 70.20(13) . . . . ? O3 V1 V3 Cl4 2.73(9) . . . . ? O2 V1 V3 Cl4 86.06(13) . . . . ? O1 V1 V3 Cl4 100.89(11) . . . . ? O4 V1 V3 Cl4 -175.15(9) . . . . ? O5 V1 V3 Cl4 -99.58(13) . . . . ? O6 V1 V3 Cl4 -76.60(11) . . . . ? V2 V1 V3 Cl4 148.07(4) . . . . ? V4 V1 V3 Cl4 -32.14(5) . . . . ? O3 V1 V3 Cl3 -94.52(10) . . . . ? O2 V1 V3 Cl3 -11.19(13) . . . . ? O1 V1 V3 Cl3 3.64(12) . . . . ? O4 V1 V3 Cl3 87.60(10) . . . . ? O5 V1 V3 Cl3 163.17(14) . . . . ? O6 V1 V3 Cl3 -173.85(11) . . . . ? V2 V1 V3 Cl3 50.82(6) . . . . ? V4 V1 V3 Cl3 -129.39(5) . . . . ? O3 V1 V4 O6 -176.40(18) . . . . ? O2 V1 V4 O6 -158.90(17) . . . . ? O1 V1 V4 O6 102.05(15) . . . . ? O4 V1 V4 O6 21.17(16) . . . . ? O5 V1 V4 O6 -76.60(15) . . . . ? V2 V1 V4 O6 67.76(13) . . . . ? V3 V1 V4 O6 -112.03(13) . . . . ? O2 V1 V4 O3 17.50(17) . . . . ? O1 V1 V4 O3 -81.55(15) . . . . ? O4 V1 V4 O3 -162.42(17) . . . . ? O5 V1 V4 O3 99.80(15) . . . . ? O6 V1 V4 O3 176.40(18) . . . . ? V2 V1 V4 O3 -115.84(13) . . . . ? V3 V1 V4 O3 64.38(13) . . . . ? O3 V1 V4 N5 -94.71(16) . . . . ? O2 V1 V4 N5 -77.21(15) . . . . ? O1 V1 V4 N5 -176.26(13) . . . . ? O4 V1 V4 N5 102.86(14) . . . . ? O5 V1 V4 N5 5.09(13) . . . . ? O6 V1 V4 N5 81.69(16) . . . . ? V2 V1 V4 N5 149.45(10) . . . . ? V3 V1 V4 N5 -30.33(11) . . . . ? O3 V1 V4 N6 -169.97(19) . . . . ? O2 V1 V4 N6 -152.47(17) . . . . ? O1 V1 V4 N6 108.48(16) . . . . ? O4 V1 V4 N6 27.61(17) . . . . ? O5 V1 V4 N6 -70.17(16) . . . . ? O6 V1 V4 N6 6.43(18) . . . . ? V2 V1 V4 N6 74.20(14) . . . . ? V3 V1 V4 N6 -105.59(14) . . . . ? O3 V1 V4 Cl6 87.96(14) . . . . ? O2 V1 V4 Cl6 105.46(11) . . . . ? O1 V1 V4 Cl6 6.41(9) . . . . ? O4 V1 V4 Cl6 -74.47(11) . . . . ? O5 V1 V4 Cl6 -172.24(9) . . . . ? O6 V1 V4 Cl6 -95.64(13) . . . . ? V2 V1 V4 Cl6 -27.88(5) . . . . ? V3 V1 V4 Cl6 152.34(4) . . . . ? O3 V1 V4 Cl5 -9.44(14) . . . . ? O2 V1 V4 Cl5 8.06(12) . . . . ? O1 V1 V4 Cl5 -90.99(9) . . . . ? O4 V1 V4 Cl5 -171.86(11) . . . . ? O5 V1 V4 Cl5 90.36(9) . . . . ? O6 V1 V4 Cl5 166.96(14) . . . . ? V2 V1 V4 Cl5 -125.28(5) . . . . ? V3 V1 V4 Cl5 54.94(6) . . . . ? O3 V1 O1 C1 43.4(3) . . . . ? O2 V1 O1 C1 -48.7(3) . . . . ? O4 V1 O1 C1 -152.9(3) . . . . ? O5 V1 O1 C1 -102.5(4) . . . . ? O6 V1 O1 C1 119.8(3) . . . . ? V2 V1 O1 C1 -147.9(3) . . . . ? V3 V1 O1 C1 -58.1(3) . . . . ? V4 V1 O1 C1 81.8(3) . . . . ? O3 V1 O1 V2 -168.71(12) . . . . ? O2 V1 O1 V2 99.17(12) . . . . ? O4 V1 O1 V2 -5.07(11) . . . . ? O5 V1 O1 V2 45.3(4) . . . . ? O6 V1 O1 V2 -92.32(12) . . . . ? V3 V1 O1 V2 89.77(12) . . . . ? V4 V1 O1 V2 -130.34(9) . . . . ? O4 V2 O1 C1 147.0(3) . . . . ? N1 V2 O1 C1 -128.4(3) . . . . ? N2 V2 O1 C1 -173.8(5) . . . . ? Cl2 V2 O1 C1 48.7(3) . . . . ? Cl1 V2 O1 C1 -43.4(3) . . . . ? V1 V2 O1 C1 142.0(4) . . . . ? O4 V2 O1 V1 5.09(11) . . . . ? N1 V2 O1 V1 89.60(13) . . . . ? N2 V2 O1 V1 44.2(6) . . . . ? Cl2 V2 O1 V1 -93.25(10) . . . . ? Cl1 V2 O1 V1 174.61(9) . . . . ? O3 V1 O2 C2 -49.0(3) . . . . ? O1 V1 O2 C2 41.9(3) . . . . ? O4 V1 O2 C2 120.0(3) . . . . ? O5 V1 O2 C2 -152.9(3) . . . . ? O6 V1 O2 C2 -102.0(4) . . . . ? V2 V1 O2 C2 81.1(3) . . . . ? V3 V1 O2 C2 -149.3(3) . . . . ? V4 V1 O2 C2 -59.9(3) . . . . ? O3 V1 O2 V3 100.33(13) . . . . ? O1 V1 O2 V3 -168.79(12) . . . . ? O4 V1 O2 V3 -90.61(13) . . . . ? O5 V1 O2 V3 -3.57(11) . . . . ? O6 V1 O2 V3 47.3(4) . . . . ? V2 V1 O2 V3 -129.60(9) . . . . ? V4 V1 O2 V3 89.45(12) . . . . ? O5 V3 O2 C2 147.8(3) . . . . ? N3 V3 O2 C2 -126.2(3) . . . . ? N4 V3 O2 C2 176.3(5) . . . . ? Cl4 V3 O2 C2 46.6(3) . . . . ? Cl3 V3 O2 C2 -44.3(3) . . . . ? V1 V3 O2 C2 144.2(4) . . . . ? O5 V3 O2 V1 3.66(11) . . . . ? N3 V3 O2 V1 89.60(14) . . . . ? N4 V3 O2 V1 32.1(6) . . . . ? Cl4 V3 O2 V1 -97.62(10) . . . . ? Cl3 V3 O2 V1 171.51(10) . . . . ? O2 V1 O3 C3 41.0(3) . . . . ? O1 V1 O3 C3 -51.0(3) . . . . ? O4 V1 O3 C3 -105.9(4) . . . . ? O5 V1 O3 C3 118.8(3) . . . . ? O6 V1 O3 C3 -154.7(3) . . . . ? V2 V1 O3 C3 -60.2(3) . . . . ? V3 V1 O3 C3 80.3(3) . . . . ? V4 V1 O3 C3 -152.4(3) . . . . ? O2 V1 O3 V4 -166.61(13) . . . . ? O1 V1 O3 V4 101.44(13) . . . . ? O4 V1 O3 V4 46.5(4) . . . . ? O5 V1 O3 V4 -88.83(13) . . . . ? O6 V1 O3 V4 -2.26(12) . . . . ? V2 V1 O3 V4 92.20(12) . . . . ? V3 V1 O3 V4 -127.30(10) . . . . ? O6 V4 O3 C3 149.8(3) . . . . ? N5 V4 O3 C3 -123.1(3) . . . . ? N6 V4 O3 C3 -166.4(6) . . . . ? Cl6 V4 O3 C3 51.5(3) . . . . ? Cl5 V4 O3 C3 -39.8(3) . . . . ? V1 V4 O3 C3 147.5(4) . . . . ? O6 V4 O3 V1 2.34(12) . . . . ? N5 V4 O3 V1 89.42(14) . . . . ? N6 V4 O3 V1 46.1(8) . . . . ? Cl6 V4 O3 V1 -96.03(11) . . . . ? Cl5 V4 O3 V1 172.73(10) . . . . ? O1 V2 O4 C6 148.2(3) . . . . ? N1 V2 O4 C6 50.5(3) . . . . ? N2 V2 O4 C6 -24.6(3) . . . . ? Cl2 V2 O4 C6 -120.4(3) . . . . ? Cl1 V2 O4 C6 98.8(5) . . . . ? V1 V2 O4 C6 153.3(4) . . . . ? O1 V2 O4 V1 -5.09(11) . . . . ? N1 V2 O4 V1 -102.85(13) . . . . ? N2 V2 O4 V1 -177.96(12) . . . . ? Cl2 V2 O4 V1 86.32(10) . . . . ? Cl1 V2 O4 V1 -54.6(4) . . . . ? O3 V1 O4 C6 -96.7(4) . . . . ? O2 V1 O4 C6 117.7(3) . . . . ? O1 V1 O4 C6 -153.4(3) . . . . ? O5 V1 O4 C6 40.4(3) . . . . ? O6 V1 O4 C6 -49.6(3) . . . . ? V2 V1 O4 C6 -158.5(3) . . . . ? V3 V1 O4 C6 77.1(3) . . . . ? V4 V1 O4 C6 -62.4(3) . . . . ? O3 V1 O4 V2 61.9(4) . . . . ? O2 V1 O4 V2 -83.80(13) . . . . ? O1 V1 O4 V2 5.13(11) . . . . ? O5 V1 O4 V2 -161.11(12) . . . . ? O6 V1 O4 V2 108.91(12) . . . . ? V3 V1 O4 V2 -124.36(9) . . . . ? V4 V1 O4 V2 96.14(11) . . . . ? O2 V3 O5 C7 149.0(3) . . . . ? N3 V3 O5 C7 49.7(3) . . . . ? N4 V3 O5 C7 -25.4(3) . . . . ? Cl4 V3 O5 C7 -120.2(3) . . . . ? Cl3 V3 O5 C7 97.2(4) . . . . ? V1 V3 O5 C7 152.6(4) . . . . ? O2 V3 O5 V1 -3.56(11) . . . . ? N3 V3 O5 V1 -102.87(14) . . . . ? N4 V3 O5 V1 -177.94(13) . . . . ? Cl4 V3 O5 V1 87.25(10) . . . . ? Cl3 V3 O5 V1 -55.4(4) . . . . ? O3 V1 O5 C7 117.1(3) . . . . ? O2 V1 O5 C7 -153.8(3) . . . . ? O1 V1 O5 C7 -98.1(4) . . . . ? O4 V1 O5 C7 -49.2(3) . . . . ? O6 V1 O5 C7 41.0(3) . . . . ? V2 V1 O5 C7 -63.9(3) . . . . ? V3 V1 O5 C7 -157.5(3) . . . . ? V4 V1 O5 C7 77.5(3) . . . . ? O3 V1 O5 V3 -85.39(13) . . . . ? O2 V1 O5 V3 3.68(11) . . . . ? O1 V1 O5 V3 59.4(4) . . . . ? O4 V1 O5 V3 108.30(12) . . . . ? O6 V1 O5 V3 -161.55(12) . . . . ? V2 V1 O5 V3 93.62(12) . . . . ? V4 V1 O5 V3 -124.99(9) . . . . ? O3 V4 O6 C8 148.2(4) . . . . ? N5 V4 O6 C8 50.8(3) . . . . ? N6 V4 O6 C8 -25.0(4) . . . . ? Cl6 V4 O6 C8 -119.2(3) . . . . ? Cl5 V4 O6 C8 105.8(4) . . . . ? V1 V4 O6 C8 150.5(4) . . . . ? O3 V4 O6 V1 -2.25(11) . . . . ? N5 V4 O6 V1 -99.70(14) . . . . ? N6 V4 O6 V1 -175.45(13) . . . . ? Cl6 V4 O6 V1 90.27(11) . . . . ? Cl5 V4 O6 V1 -44.6(4) . . . . ? O3 V1 O6 C8 -153.8(3) . . . . ? O2 V1 O6 C8 -98.6(4) . . . . ? O1 V1 O6 C8 118.6(3) . . . . ? O4 V1 O6 C8 40.9(3) . . . . ? O5 V1 O6 C8 -49.4(3) . . . . ? V2 V1 O6 C8 78.2(3) . . . . ? V3 V1 O6 C8 -63.3(3) . . . . ? V4 V1 O6 C8 -156.1(3) . . . . ? O3 V1 O6 V4 2.32(12) . . . . ? O2 V1 O6 V4 57.5(4) . . . . ? O1 V1 O6 V4 -85.25(13) . . . . ? O4 V1 O6 V4 -163.01(13) . . . . ? O5 V1 O6 V4 106.75(13) . . . . ? V2 V1 O6 V4 -125.65(9) . . . . ? V3 V1 O6 V4 92.79(12) . . . . ? O4 V2 N1 C15 85.5(3) . . . . ? O1 V2 N1 C15 8.3(3) . . . . ? N2 V2 N1 C15 -180.0(3) . . . . ? Cl2 V2 N1 C15 -155.6(4) . . . . ? Cl1 V2 N1 C15 -84.1(3) . . . . ? V1 V2 N1 C15 47.5(3) . . . . ? O4 V2 N1 C11 -94.3(3) . . . . ? O1 V2 N1 C11 -171.5(3) . . . . ? N2 V2 N1 C11 0.2(3) . . . . ? Cl2 V2 N1 C11 24.6(8) . . . . ? Cl1 V2 N1 C11 96.1(3) . . . . ? V1 V2 N1 C11 -132.3(3) . . . . ? O4 V2 N2 C20 -93.9(3) . . . . ? O1 V2 N2 C20 -132.1(6) . . . . ? N1 V2 N2 C20 -179.0(4) . . . . ? Cl2 V2 N2 C20 5.3(3) . . . . ? Cl1 V2 N2 C20 97.6(3) . . . . ? V1 V2 N2 C20 -95.6(3) . . . . ? O4 V2 N2 C16 84.5(3) . . . . ? O1 V2 N2 C16 46.3(7) . . . . ? N1 V2 N2 C16 -0.6(3) . . . . ? Cl2 V2 N2 C16 -176.3(3) . . . . ? Cl1 V2 N2 C16 -84.0(3) . . . . ? V1 V2 N2 C16 82.7(3) . . . . ? O5 V3 N3 C25 91.0(4) . . . . ? O2 V3 N3 C25 14.5(4) . . . . ? N4 V3 N3 C25 -175.9(4) . . . . ? Cl4 V3 N3 C25 -134.3(4) . . . . ? Cl3 V3 N3 C25 -77.5(3) . . . . ? V1 V3 N3 C25 52.7(4) . . . . ? O5 V3 N3 C21 -97.8(3) . . . . ? O2 V3 N3 C21 -174.4(3) . . . . ? N4 V3 N3 C21 -4.7(3) . . . . ? Cl4 V3 N3 C21 36.9(6) . . . . ? Cl3 V3 N3 C21 93.7(3) . . . . ? V1 V3 N3 C21 -136.1(3) . . . . ? O5 V3 N4 C30 -88.1(3) . . . . ? O2 V3 N4 C30 -115.8(6) . . . . ? N3 V3 N4 C30 -175.4(4) . . . . ? Cl4 V3 N4 C30 13.9(3) . . . . ? Cl3 V3 N4 C30 105.0(3) . . . . ? V1 V3 N4 C30 -89.9(3) . . . . ? O5 V3 N4 C26 87.5(3) . . . . ? O2 V3 N4 C26 59.8(7) . . . . ? N3 V3 N4 C26 0.2(3) . . . . ? Cl4 V3 N4 C26 -170.5(3) . . . . ? Cl3 V3 N4 C26 -79.4(3) . . . . ? V1 V3 N4 C26 85.7(3) . . . . ? O6 V4 N5 C35 84.8(3) . . . . ? O3 V4 N5 C35 8.2(3) . . . . ? N6 V4 N5 C35 -178.7(4) . . . . ? Cl6 V4 N5 C35 -146.3(4) . . . . ? Cl5 V4 N5 C35 -83.4(3) . . . . ? V1 V4 N5 C35 45.9(3) . . . . ? O6 V4 N5 C31 -98.6(3) . . . . ? O3 V4 N5 C31 -175.1(3) . . . . ? N6 V4 N5 C31 -2.1(3) . . . . ? Cl6 V4 N5 C31 30.4(7) . . . . ? Cl5 V4 N5 C31 93.2(3) . . . . ? V1 V4 N5 C31 -137.5(3) . . . . ? O6 V4 N6 C40 -94.0(4) . . . . ? O3 V4 N6 C40 -136.6(7) . . . . ? N5 V4 N6 C40 178.8(4) . . . . ? Cl6 V4 N6 C40 5.6(4) . . . . ? Cl5 V4 N6 C40 96.9(4) . . . . ? V1 V4 N6 C40 -98.1(4) . . . . ? O6 V4 N6 C36 91.5(3) . . . . ? O3 V4 N6 C36 48.9(9) . . . . ? N5 V4 N6 C36 4.3(3) . . . . ? Cl6 V4 N6 C36 -168.9(3) . . . . ? Cl5 V4 N6 C36 -77.7(3) . . . . ? V1 V4 N6 C36 87.4(3) . . . . ? V1 O1 C1 C4 5.4(4) . . . . ? V2 O1 C1 C4 -131.7(3) . . . . ? V1 O2 C2 C4 6.4(4) . . . . ? V3 O2 C2 C4 -133.2(3) . . . . ? V1 O3 C3 C4 7.6(5) . . . . ? V4 O3 C3 C4 -136.1(3) . . . . ? O3 C3 C4 C5 176.6(3) . . . . ? O3 C3 C4 C2 -67.3(5) . . . . ? O3 C3 C4 C1 59.1(5) . . . . ? O2 C2 C4 C3 58.7(5) . . . . ? O2 C2 C4 C5 175.3(3) . . . . ? O2 C2 C4 C1 -67.6(5) . . . . ? O1 C1 C4 C3 -66.5(4) . . . . ? O1 C1 C4 C5 176.2(3) . . . . ? O1 C1 C4 C2 59.8(5) . . . . ? C3 C4 C5 O7X -67.4(5) . . . . ? C2 C4 C5 O7X 172.9(4) . . . . ? C1 C4 C5 O7X 52.8(5) . . . . ? C3 C4 C5 O7Y 170.0(4) . . . . ? C2 C4 C5 O7Y 50.3(5) . . . . ? C1 C4 C5 O7Y -69.8(5) . . . . ? C3 C4 C5 O7Z 49.5(5) . . . . ? C2 C4 C5 O7Z -70.1(5) . . . . ? C1 C4 C5 O7Z 169.8(4) . . . . ? V2 O4 C6 C9 -142.4(3) . . . . ? V1 O4 C6 C9 7.6(4) . . . . ? V3 O5 C7 C9 -141.9(3) . . . . ? V1 O5 C7 C9 7.2(4) . . . . ? V4 O6 C8 C9 -139.5(3) . . . . ? V1 O6 C8 C9 7.7(4) . . . . ? O5 C7 C9 C8 -68.6(4) . . . . ? O5 C7 C9 C6 59.0(5) . . . . ? O5 C7 C9 C10 174.5(3) . . . . ? O6 C8 C9 C7 59.5(4) . . . . ? O6 C8 C9 C6 -68.3(4) . . . . ? O6 C8 C9 C10 177.1(3) . . . . ? O4 C6 C9 C7 -68.5(5) . . . . ? O4 C6 C9 C8 59.5(4) . . . . ? O4 C6 C9 C10 174.7(3) . . . . ? C7 C9 C10 O8X 62.7(5) . . . . ? C8 C9 C10 O8X -58.3(5) . . . . ? C6 C9 C10 O8X -177.3(4) . . . . ? C7 C9 C10 O8Y -57.7(6) . . . . ? C8 C9 C10 O8Y -178.7(6) . . . . ? C6 C9 C10 O8Y 62.3(6) . . . . ? C7 C9 C10 O8Z -179.3(6) . . . . ? C8 C9 C10 O8Z 59.7(6) . . . . ? C6 C9 C10 O8Z -59.3(6) . . . . ? C15 N1 C11 C12 -0.6(6) . . . . ? V2 N1 C11 C12 179.2(3) . . . . ? C15 N1 C11 C16 -179.7(3) . . . . ? V2 N1 C11 C16 0.1(4) . . . . ? N1 C11 C12 C13 -0.3(6) . . . . ? C16 C11 C12 C13 178.7(4) . . . . ? C11 C12 C13 C14 0.7(7) . . . . ? C12 C13 C14 C15 -0.2(7) . . . . ? C11 N1 C15 C14 1.1(6) . . . . ? V2 N1 C15 C14 -178.7(3) . . . . ? C13 C14 C15 N1 -0.7(7) . . . . ? C20 N2 C16 C17 -0.2(6) . . . . ? V2 N2 C16 C17 -178.7(3) . . . . ? C20 N2 C16 C11 179.4(4) . . . . ? V2 N2 C16 C11 0.9(4) . . . . ? N1 C11 C16 N2 -0.6(5) . . . . ? C12 C11 C16 N2 -179.7(4) . . . . ? N1 C11 C16 C17 178.9(4) . . . . ? C12 C11 C16 C17 -0.1(7) . . . . ? N2 C16 C17 C18 0.8(7) . . . . ? C11 C16 C17 C18 -178.7(4) . . . . ? C16 C17 C18 C19 -0.6(7) . . . . ? C17 C18 C19 C20 -0.1(8) . . . . ? C16 N2 C20 C19 -0.6(7) . . . . ? V2 N2 C20 C19 177.7(4) . . . . ? C18 C19 C20 N2 0.8(8) . . . . ? C25 N3 C21 C22 2.1(7) . . . . ? V3 N3 C21 C22 -169.4(4) . . . . ? C25 N3 C21 C26 179.6(4) . . . . ? V3 N3 C21 C26 8.1(5) . . . . ? N3 C21 C22 C23 -1.4(8) . . . . ? C26 C21 C22 C23 -178.6(5) . . . . ? C21 C22 C23 C24 -0.4(9) . . . . ? C22 C23 C24 C25 1.3(9) . . . . ? C21 N3 C25 C24 -1.2(7) . . . . ? V3 N3 C25 C24 169.8(4) . . . . ? C23 C24 C25 N3 -0.5(8) . . . . ? C30 N4 C26 C27 0.0(6) . . . . ? V3 N4 C26 C27 -175.8(3) . . . . ? C30 N4 C26 C21 179.8(4) . . . . ? V3 N4 C26 C21 3.9(5) . . . . ? N3 C21 C26 N4 -7.8(6) . . . . ? C22 C21 C26 N4 169.6(5) . . . . ? N3 C21 C26 C27 171.9(4) . . . . ? C22 C21 C26 C27 -10.7(7) . . . . ? N4 C26 C27 C28 0.5(7) . . . . ? C21 C26 C27 C28 -179.2(4) . . . . ? C26 C27 C28 C29 -0.7(7) . . . . ? C27 C28 C29 C30 0.4(7) . . . . ? C26 N4 C30 C29 -0.4(6) . . . . ? V3 N4 C30 C29 175.2(3) . . . . ? C28 C29 C30 N4 0.1(7) . . . . ? C35 N5 C31 C32 -2.3(6) . . . . ? V4 N5 C31 C32 -179.2(3) . . . . ? C35 N5 C31 C36 176.6(4) . . . . ? V4 N5 C31 C36 -0.3(5) . . . . ? N5 C31 C32 C33 0.9(7) . . . . ? C36 C31 C32 C33 -177.8(4) . . . . ? C31 C32 C33 C34 1.1(7) . . . . ? C32 C33 C34 C35 -1.7(7) . . . . ? C31 N5 C35 C34 1.7(6) . . . . ? V4 N5 C35 C34 178.4(3) . . . . ? C33 C34 C35 N5 0.3(7) . . . . ? C40 N6 C36 C37 -2.1(6) . . . . ? V4 N6 C36 C37 172.9(3) . . . . ? C40 N6 C36 C31 179.2(4) . . . . ? V4 N6 C36 C31 -5.8(5) . . . . ? N5 C31 C36 N6 4.0(5) . . . . ? C32 C31 C36 N6 -177.1(4) . . . . ? N5 C31 C36 C37 -174.7(4) . . . . ? C32 C31 C36 C37 4.2(7) . . . . ? N6 C36 C37 C38 0.8(7) . . . . ? C31 C36 C37 C38 179.4(4) . . . . ? C36 C37 C38 C39 1.0(8) . . . . ? C37 C38 C39 C40 -1.4(8) . . . . ? C36 N6 C40 C39 1.6(7) . . . . ? V4 N6 C40 C39 -172.8(4) . . . . ? C38 C39 C40 N6 0.1(8) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 1.499 _refine_diff_density_min -0.856 _refine_diff_density_rms 0.089 # Attachment '8.cif' data_oejlm236p21c _database_code_depnum_ccdc_archive 'CCDC 736086' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[V3Cl4(Hcht)2(bipy)2]Cl2MeCN' _chemical_formula_sum 'C36 H42 Cl5 N6 O6 V3' _chemical_formula_weight 984.83 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.4708(19) _cell_length_b 14.8055(13) _cell_length_c 12.4733(11) _cell_angle_alpha 90.00 _cell_angle_beta 100.043(7) _cell_angle_gamma 90.00 _cell_volume 4086.2(6) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 3210 _cell_measurement_theta_min 2.6327 _cell_measurement_theta_max 28.2109 _exptl_crystal_description plate _exptl_crystal_colour black/brown _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.601 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 1.052 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.6214 _exptl_absorpt_correction_T_max 0.6214 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcaliber 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23227 _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_sigmaI/netI 0.0617 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 24.73 _reflns_number_total 6965 _reflns_number_gt 4732 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) ; _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 ; The structure was solved by direct methods. Data processing was carried out to 0.85 angstroms as the data was only complete to this resolution. Hydrogen atoms were included in calculated positions except for the hydrogen atoms H2F and H5F which were found in their actual positionsusing the data. 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^)+(0.0413P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6965 _refine_ls_number_parameters 515 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0528 _refine_ls_R_factor_gt 0.0311 _refine_ls_wR_factor_ref 0.0770 _refine_ls_wR_factor_gt 0.0730 _refine_ls_goodness_of_fit_ref 0.953 _refine_ls_restrained_S_all 0.953 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.15524(2) 0.54366(3) 0.22288(4) 0.01155(13) Uani 1 1 d . . . V2 V 0.20565(2) 0.47026(3) 0.45314(4) 0.01077(13) Uani 1 1 d . . . V3 V 0.33408(2) 0.47432(3) 0.59076(4) 0.01268(13) Uani 1 1 d . . . Cl1 Cl 0.23880(3) 0.62890(5) 0.19610(6) 0.01760(18) Uani 1 1 d . . . Cl2 Cl 0.08758(3) 0.66237(5) 0.16318(6) 0.01697(18) Uani 1 1 d . . . Cl3 Cl 0.39378(4) 0.59323(5) 0.68017(6) 0.0231(2) Uani 1 1 d . . . Cl4 Cl 0.30023(4) 0.42992(5) 0.75059(6) 0.02028(19) Uani 1 1 d . . . Cl5 Cl 0.06139(4) 0.35567(5) 0.57067(6) 0.02165(19) Uani 1 1 d . . . O1 O 0.20758(9) 0.44585(12) 0.29884(14) 0.0130(5) Uani 1 1 d . . . O2 O 0.15956(10) 0.35271(13) 0.44700(17) 0.0180(5) Uani 1 1 d . . . O3 O 0.28118(9) 0.39506(12) 0.49770(14) 0.0121(5) Uani 1 1 d . . . O4 O 0.15543(9) 0.56778(12) 0.37741(14) 0.0109(4) Uani 1 1 d . . . O5 O 0.16219(10) 0.48872(14) 0.58535(15) 0.0138(5) Uani 1 1 d . . . O6 O 0.26377(8) 0.55684(12) 0.52732(14) 0.0111(4) Uani 1 1 d . . . N1 N 0.14191(11) 0.48746(15) 0.06168(18) 0.0132(6) Uani 1 1 d . . . N2 N 0.07626(11) 0.46210(15) 0.21277(17) 0.0110(5) Uani 1 1 d . . . N3 N 0.37919(11) 0.49880(16) 0.45761(18) 0.0135(6) Uani 1 1 d . . . N4 N 0.40784(11) 0.38164(16) 0.61487(18) 0.0163(6) Uani 1 1 d . . . N5 N 0.42894(17) 0.6524(2) 1.0516(2) 0.0470(9) Uani 1 1 d . . . N6 N 0.3378(2) 0.4078(3) 1.0786(3) 0.0895(16) Uani 1 1 d . . . C1 C 0.22454(14) 0.35914(19) 0.2605(2) 0.0158(7) Uani 1 1 d . . . H1 H 0.2251 0.3635 0.1822 0.019 Uiso 1 1 calc R . . C2 C 0.17840(14) 0.2874(2) 0.2787(2) 0.0197(7) Uani 1 1 d . . . H2A H 0.1383 0.3069 0.2449 0.024 Uiso 1 1 calc R . . H2B H 0.1873 0.2314 0.2444 0.024 Uiso 1 1 calc R . . C3 C 0.17945(14) 0.27103(19) 0.3987(2) 0.0176(7) Uani 1 1 d . . . H3 H 0.1513 0.2220 0.4068 0.021 Uiso 1 1 calc R . . C4 C 0.24179(14) 0.24510(19) 0.4573(2) 0.0189(7) Uani 1 1 d . . . H4A H 0.2523 0.1863 0.4318 0.023 Uiso 1 1 calc R . . H4B H 0.2412 0.2403 0.5346 0.023 Uiso 1 1 calc R . . C5 C 0.28971(14) 0.31314(19) 0.4394(2) 0.0155(7) Uani 1 1 d . . . H5 H 0.3296 0.2882 0.4691 0.019 Uiso 1 1 calc R . . C6 C 0.28720(14) 0.33320(19) 0.3184(2) 0.0154(7) Uani 1 1 d . . . H6A H 0.3150 0.3820 0.3110 0.018 Uiso 1 1 calc R . . H6B H 0.3006 0.2802 0.2835 0.018 Uiso 1 1 calc R . . C7 C 0.14606(14) 0.65096(18) 0.4335(2) 0.0137(7) Uani 1 1 d . . . H7 H 0.1220 0.6921 0.3817 0.016 Uiso 1 1 calc R . . C8 C 0.11148(13) 0.63124(19) 0.5246(2) 0.0153(7) Uani 1 1 d . . . H8A H 0.0760 0.5957 0.4962 0.018 Uiso 1 1 calc R . . H8B H 0.0979 0.6877 0.5516 0.018 Uiso 1 1 calc R . . C9 C 0.14932(14) 0.58042(19) 0.6183(2) 0.0139(7) Uani 1 1 d . . . H9 H 0.1267 0.5769 0.6785 0.017 Uiso 1 1 calc R . . C10 C 0.20901(13) 0.62642(19) 0.6584(2) 0.0127(7) Uani 1 1 d . . . H10A H 0.2327 0.5894 0.7144 0.015 Uiso 1 1 calc R . . H10B H 0.2017 0.6840 0.6909 0.015 Uiso 1 1 calc R . . C11 C 0.24478(14) 0.64215(18) 0.5672(2) 0.0132(7) Uani 1 1 d . . . H11 H 0.2808 0.6779 0.5957 0.016 Uiso 1 1 calc R . . C12 C 0.20660(13) 0.69437(18) 0.4742(2) 0.0127(7) Uani 1 1 d . . . H12A H 0.2001 0.7551 0.4989 0.015 Uiso 1 1 calc R . . H12B H 0.2288 0.6990 0.4143 0.015 Uiso 1 1 calc R . . C13 C 0.08932(13) 0.44358(18) 0.0287(2) 0.0127(7) Uani 1 1 d . . . C14 C 0.07026(14) 0.41907(19) -0.0789(2) 0.0140(7) Uani 1 1 d . . . H14 H 0.0330 0.3912 -0.1003 0.017 Uiso 1 1 calc R . . C15 C 0.10702(14) 0.43631(19) -0.1537(2) 0.0177(7) Uani 1 1 d . . . H15 H 0.0947 0.4211 -0.2266 0.021 Uiso 1 1 calc R . . C16 C 0.16236(15) 0.4764(2) -0.1193(2) 0.0183(7) Uani 1 1 d . . . H16 H 0.1888 0.4861 -0.1679 0.022 Uiso 1 1 calc R . . C17 C 0.17798(14) 0.5021(2) -0.0120(2) 0.0182(7) Uani 1 1 d . . . H17 H 0.2149 0.5306 0.0104 0.022 Uiso 1 1 calc R . . C18 C 0.05493(13) 0.42236(18) 0.1154(2) 0.0119(7) Uani 1 1 d . . . C19 C 0.00640(14) 0.3642(2) 0.1031(2) 0.0175(7) Uani 1 1 d . . . H19 H -0.0080 0.3383 0.0356 0.021 Uiso 1 1 calc R . . C20 C -0.02073(14) 0.3445(2) 0.1908(2) 0.0189(7) Uani 1 1 d . . . H20 H -0.0528 0.3041 0.1838 0.023 Uiso 1 1 calc R . . C21 C 0.00030(14) 0.3857(2) 0.2895(2) 0.0178(7) Uani 1 1 d . . . H21 H -0.0175 0.3739 0.3500 0.021 Uiso 1 1 calc R . . C22 C 0.04807(13) 0.44439(19) 0.2964(2) 0.0140(7) Uani 1 1 d . . . H22 H 0.0615 0.4733 0.3624 0.017 Uiso 1 1 calc R . . C23 C 0.42740(13) 0.44727(19) 0.4497(2) 0.0136(7) Uani 1 1 d . . . C24 C 0.45846(14) 0.4566(2) 0.3641(2) 0.0186(7) Uani 1 1 d . . . H24 H 0.4924 0.4214 0.3609 0.022 Uiso 1 1 calc R . . C25 C 0.43845(14) 0.5187(2) 0.2834(2) 0.0215(8) Uani 1 1 d . . . H25 H 0.4586 0.5256 0.2249 0.026 Uiso 1 1 calc R . . C26 C 0.38874(15) 0.5698(2) 0.2905(2) 0.0220(8) Uani 1 1 d . . . H26 H 0.3743 0.6116 0.2365 0.026 Uiso 1 1 calc R . . C27 C 0.36034(14) 0.5585(2) 0.3788(2) 0.0169(7) Uani 1 1 d . . . H27 H 0.3267 0.5938 0.3837 0.020 Uiso 1 1 calc R . . C28 C 0.44410(14) 0.3810(2) 0.5389(2) 0.0157(7) Uani 1 1 d . . . C29 C 0.49250(15) 0.3223(2) 0.5447(3) 0.0220(8) Uani 1 1 d . . . H29 H 0.5160 0.3219 0.4904 0.026 Uiso 1 1 calc R . . C30 C 0.50532(15) 0.2641(2) 0.6328(3) 0.0269(8) Uani 1 1 d . . . H30 H 0.5380 0.2247 0.6389 0.032 Uiso 1 1 calc R . . C31 C 0.46920(15) 0.2655(2) 0.7107(3) 0.0268(8) Uani 1 1 d . . . H31 H 0.4773 0.2276 0.7708 0.032 Uiso 1 1 calc R . . C32 C 0.42064(15) 0.3240(2) 0.6986(2) 0.0234(8) Uani 1 1 d . . . H32 H 0.3957 0.3234 0.7509 0.028 Uiso 1 1 calc R . . C33 C 0.38280(19) 0.6497(2) 0.9986(3) 0.0315(9) Uani 1 1 d . . . C34 C 0.32401(17) 0.6456(3) 0.9284(3) 0.0459(11) Uani 1 1 d . . . H34A H 0.3207 0.6937 0.8760 0.069 Uiso 1 1 calc R . . H34B H 0.2928 0.6517 0.9716 0.069 Uiso 1 1 calc R . . H34C H 0.3197 0.5886 0.8911 0.069 Uiso 1 1 calc R . . C35 C 0.3771(2) 0.4136(3) 1.0326(3) 0.0469(11) Uani 1 1 d . . . C36 C 0.4263(2) 0.4234(3) 0.9752(3) 0.0581(13) Uani 1 1 d . . . H36A H 0.4140 0.4604 0.9120 0.087 Uiso 1 1 calc R . . H36B H 0.4383 0.3650 0.9531 0.087 Uiso 1 1 calc R . . H36C H 0.4597 0.4514 1.0218 0.087 Uiso 1 1 calc R . . H2F H 0.1321(14) 0.343(2) 0.477(2) 0.019(10) Uiso 1 1 d . . . H5F H 0.1336(16) 0.451(2) 0.579(3) 0.035(11) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0112(3) 0.0135(3) 0.0096(3) 0.0011(2) 0.0008(2) -0.0007(2) V2 0.0126(3) 0.0101(3) 0.0092(3) -0.0002(2) 0.0008(2) -0.0006(2) V3 0.0114(3) 0.0157(3) 0.0107(3) -0.0005(2) 0.0012(2) 0.0008(2) Cl1 0.0150(4) 0.0192(4) 0.0181(4) 0.0048(3) 0.0016(3) -0.0028(3) Cl2 0.0158(4) 0.0174(4) 0.0164(4) 0.0027(3) -0.0009(3) 0.0022(3) Cl3 0.0141(4) 0.0284(5) 0.0265(4) -0.0114(4) 0.0023(4) -0.0035(4) Cl4 0.0207(5) 0.0265(5) 0.0142(4) 0.0043(3) 0.0046(3) 0.0042(4) Cl5 0.0206(5) 0.0306(5) 0.0148(4) -0.0024(3) 0.0061(3) -0.0109(4) O1 0.0182(12) 0.0111(11) 0.0099(10) -0.0007(8) 0.0030(9) 0.0013(9) O2 0.0161(13) 0.0140(12) 0.0270(13) -0.0039(10) 0.0126(11) -0.0040(10) O3 0.0131(12) 0.0104(11) 0.0125(10) -0.0014(8) 0.0009(9) 0.0015(9) O4 0.0124(12) 0.0090(11) 0.0113(10) -0.0017(8) 0.0018(9) 0.0000(9) O5 0.0132(13) 0.0130(12) 0.0156(11) 0.0011(9) 0.0035(10) -0.0013(10) O6 0.0096(11) 0.0121(11) 0.0113(10) -0.0014(8) 0.0008(9) -0.0004(9) N1 0.0141(15) 0.0136(13) 0.0123(13) 0.0029(11) 0.0036(11) 0.0019(11) N2 0.0116(14) 0.0127(13) 0.0085(12) 0.0001(10) 0.0008(11) 0.0022(11) N3 0.0104(15) 0.0172(14) 0.0120(13) -0.0007(11) -0.0003(11) -0.0019(11) N4 0.0154(15) 0.0170(14) 0.0148(13) -0.0014(11) -0.0024(12) 0.0024(12) N5 0.051(2) 0.057(2) 0.0316(19) 0.0062(17) 0.0045(18) -0.022(2) N6 0.098(4) 0.114(4) 0.056(3) -0.021(2) 0.013(3) -0.060(3) C1 0.027(2) 0.0102(16) 0.0105(15) -0.0026(13) 0.0035(14) 0.0054(14) C2 0.0207(19) 0.0145(17) 0.0219(18) -0.0073(14) -0.0020(15) 0.0011(15) C3 0.0203(19) 0.0056(16) 0.0278(18) -0.0068(13) 0.0070(15) -0.0052(14) C4 0.029(2) 0.0102(16) 0.0191(17) -0.0004(13) 0.0078(15) 0.0013(15) C5 0.0164(18) 0.0126(17) 0.0169(16) -0.0033(13) 0.0015(14) 0.0032(14) C6 0.0187(19) 0.0120(16) 0.0158(16) -0.0059(13) 0.0040(14) -0.0011(14) C7 0.0187(18) 0.0101(16) 0.0118(15) -0.0005(12) 0.0013(14) 0.0034(14) C8 0.0130(18) 0.0135(16) 0.0185(16) -0.0042(13) 0.0002(14) 0.0019(14) C9 0.0168(18) 0.0125(16) 0.0134(15) -0.0031(13) 0.0055(14) 0.0018(13) C10 0.0149(18) 0.0118(16) 0.0106(15) -0.0021(12) 0.0001(13) 0.0035(13) C11 0.0150(18) 0.0101(16) 0.0146(15) -0.0047(13) 0.0027(13) -0.0018(14) C12 0.0194(18) 0.0075(15) 0.0121(15) -0.0029(12) 0.0051(14) 0.0009(13) C13 0.0135(18) 0.0084(15) 0.0150(16) 0.0010(12) -0.0006(14) 0.0025(13) C14 0.0181(18) 0.0119(16) 0.0110(15) -0.0004(13) -0.0008(14) 0.0053(14) C15 0.027(2) 0.0165(17) 0.0090(15) 0.0014(13) 0.0023(15) 0.0062(15) C16 0.027(2) 0.0178(18) 0.0123(16) 0.0040(14) 0.0087(15) 0.0056(15) C17 0.0167(19) 0.0222(18) 0.0170(17) 0.0017(14) 0.0068(15) -0.0017(14) C18 0.0126(17) 0.0101(15) 0.0129(15) 0.0011(12) 0.0021(13) 0.0042(13) C19 0.0178(19) 0.0196(18) 0.0135(16) -0.0004(13) -0.0013(14) -0.0015(15) C20 0.0132(18) 0.0187(18) 0.0243(18) -0.0005(14) 0.0018(15) -0.0075(14) C21 0.0151(18) 0.0248(19) 0.0142(16) 0.0027(14) 0.0046(14) -0.0026(15) C22 0.0119(17) 0.0186(17) 0.0113(15) -0.0014(13) 0.0009(13) 0.0013(14) C23 0.0085(17) 0.0172(17) 0.0144(16) -0.0075(13) 0.0004(13) -0.0015(14) C24 0.0117(18) 0.0198(18) 0.0248(18) -0.0103(15) 0.0045(15) -0.0059(14) C25 0.020(2) 0.030(2) 0.0160(17) -0.0064(15) 0.0079(15) -0.0070(16) C26 0.0192(19) 0.030(2) 0.0165(17) 0.0022(15) 0.0018(15) -0.0056(16) C27 0.0111(17) 0.0184(17) 0.0204(17) -0.0009(14) 0.0005(14) -0.0023(14) C28 0.0129(18) 0.0168(17) 0.0159(16) -0.0078(13) -0.0015(14) -0.0012(14) C29 0.0188(19) 0.0202(18) 0.0263(18) -0.0107(15) 0.0019(15) 0.0033(15) C30 0.020(2) 0.024(2) 0.034(2) -0.0075(16) -0.0028(17) 0.0100(16) C31 0.028(2) 0.0208(19) 0.030(2) 0.0048(15) -0.0007(17) 0.0088(16) C32 0.023(2) 0.026(2) 0.0211(18) 0.0038(15) 0.0031(15) 0.0037(16) C33 0.039(3) 0.033(2) 0.026(2) -0.0013(17) 0.016(2) -0.009(2) C34 0.034(3) 0.049(3) 0.056(3) -0.006(2) 0.011(2) 0.005(2) C35 0.054(3) 0.045(3) 0.038(3) -0.011(2) -0.003(2) -0.012(2) C36 0.050(3) 0.067(3) 0.050(3) -0.021(2) -0.010(2) 0.016(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O4 1.9596(18) . ? V1 O1 1.9973(19) . ? V1 N2 2.132(2) . ? V1 N1 2.148(2) . ? V1 Cl1 2.3341(9) . ? V1 Cl2 2.3581(9) . ? V1 V2 3.0948(7) . ? V2 O6 1.9452(19) . ? V2 O1 1.9662(18) . ? V2 O4 1.9694(19) . ? V2 O2 2.020(2) . ? V2 O3 2.0249(19) . ? V2 O5 2.076(2) . ? V2 V3 3.0905(8) . ? V3 O3 1.9121(19) . ? V3 O6 2.0442(19) . ? V3 N3 2.122(2) . ? V3 N4 2.132(2) . ? V3 Cl4 2.3482(9) . ? V3 Cl3 2.3709(9) . ? O1 C1 1.444(3) . ? O2 C3 1.456(3) . ? O2 H2F 0.79(3) . ? O3 C5 1.444(3) . ? O4 C7 1.450(3) . ? O5 C9 1.462(3) . ? O5 H5F 0.85(3) . ? O6 C11 1.449(3) . ? N1 C17 1.345(4) . ? N1 C13 1.348(4) . ? N2 C22 1.337(3) . ? N2 C18 1.359(3) . ? N3 C27 1.335(4) . ? N3 C23 1.343(4) . ? N4 C32 1.341(4) . ? N4 C28 1.353(4) . ? N5 C33 1.129(4) . ? N6 C35 1.136(5) . ? C1 C6 1.516(4) . ? C1 C2 1.529(4) . ? C1 H1 0.9800 . ? C2 C3 1.512(4) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 C4 1.512(4) . ? C3 H3 0.9800 . ? C4 C5 1.519(4) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C5 C6 1.530(4) . ? C5 H5 0.9800 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C7 C12 1.510(4) . ? C7 C8 1.512(4) . ? C7 H7 0.9800 . ? C8 C9 1.519(4) . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C9 C10 1.510(4) . ? C9 H9 0.9800 . ? C10 C11 1.522(4) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 C12 1.526(4) . ? C11 H11 0.9800 . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.385(4) . ? C13 C18 1.469(4) . ? C14 C15 1.374(4) . ? C14 H14 0.9300 . ? C15 C16 1.377(4) . ? C15 H15 0.9300 . ? C16 C17 1.377(4) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.377(4) . ? C19 C20 1.373(4) . ? C19 H19 0.9300 . ? C20 C21 1.381(4) . ? C20 H20 0.9300 . ? C21 C22 1.372(4) . ? C21 H21 0.9300 . ? C22 H22 0.9300 . ? C23 C24 1.380(4) . ? C23 C28 1.483(4) . ? C24 C25 1.379(4) . ? C24 H24 0.9300 . ? C25 C26 1.365(4) . ? C25 H25 0.9300 . ? C26 C27 1.376(4) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.384(4) . ? C29 C30 1.386(4) . ? C29 H29 0.9300 . ? C30 C31 1.370(4) . ? C30 H30 0.9300 . ? C31 C32 1.380(4) . ? C31 H31 0.9300 . ? C32 H32 0.9300 . ? C33 C34 1.453(5) . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.426(6) . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? 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 O4 V1 O1 76.44(7) . . ? O4 V1 N2 91.17(8) . . ? O1 V1 N2 91.87(8) . . ? O4 V1 N1 165.30(8) . . ? O1 V1 N1 97.91(8) . . ? N2 V1 N1 75.32(9) . . ? O4 V1 Cl1 100.28(6) . . ? O1 V1 Cl1 92.18(6) . . ? N2 V1 Cl1 168.47(7) . . ? N1 V1 Cl1 93.43(7) . . ? O4 V1 Cl2 93.75(6) . . ? O1 V1 Cl2 169.77(6) . . ? N2 V1 Cl2 85.37(7) . . ? N1 V1 Cl2 90.92(7) . . ? Cl1 V1 Cl2 92.42(3) . . ? O4 V1 V2 38.14(5) . . ? O1 V1 V2 38.30(5) . . ? N2 V1 V2 91.27(6) . . ? N1 V1 V2 134.54(6) . . ? Cl1 V1 V2 98.59(3) . . ? Cl2 V1 V2 131.78(3) . . ? O6 V2 O1 117.33(8) . . ? O6 V2 O4 91.50(8) . . ? O1 V2 O4 76.93(7) . . ? O6 V2 O2 152.02(8) . . ? O1 V2 O2 84.44(8) . . ? O4 V2 O2 111.50(9) . . ? O6 V2 O3 76.74(8) . . ? O1 V2 O3 90.40(8) . . ? O4 V2 O3 156.57(8) . . ? O2 V2 O3 86.35(8) . . ? O6 V2 O5 84.56(8) . . ? O1 V2 O5 153.58(9) . . ? O4 V2 O5 88.56(8) . . ? O2 V2 O5 80.47(9) . . ? O3 V2 O5 110.01(8) . . ? O6 V2 V3 40.40(6) . . ? O1 V2 V3 111.67(6) . . ? O4 V2 V3 130.82(6) . . ? O2 V2 V3 117.43(7) . . ? O3 V2 V3 37.00(5) . . ? O5 V2 V3 94.55(6) . . ? O6 V2 V1 108.47(6) . . ? O1 V2 V1 39.03(6) . . ? O4 V2 V1 37.92(5) . . ? O2 V2 V1 99.50(6) . . ? O3 V2 V1 126.97(5) . . ? O5 V2 V1 122.97(6) . . ? V3 V2 V1 131.59(2) . . ? O3 V3 O6 77.00(8) . . ? O3 V3 N3 87.77(8) . . ? O6 V3 N3 92.14(8) . . ? O3 V3 N4 94.38(9) . . ? O6 V3 N4 165.58(8) . . ? N3 V3 N4 75.80(9) . . ? O3 V3 Cl4 94.85(6) . . ? O6 V3 Cl4 98.81(6) . . ? N3 V3 Cl4 169.05(7) . . ? N4 V3 Cl4 93.38(7) . . ? O3 V3 Cl3 169.15(6) . . ? O6 V3 Cl3 94.24(6) . . ? N3 V3 Cl3 86.16(7) . . ? N4 V3 Cl3 92.83(7) . . ? Cl4 V3 Cl3 92.81(3) . . ? O3 V3 V2 39.59(6) . . ? O6 V3 V2 38.08(5) . . ? N3 V3 V2 95.50(7) . . ? N4 V3 V2 133.90(7) . . ? Cl4 V3 V2 93.26(3) . . ? Cl3 V3 V2 132.28(3) . . ? C1 O1 V2 122.68(16) . . ? C1 O1 V1 130.90(16) . . ? V2 O1 V1 102.67(8) . . ? C3 O2 V2 122.62(19) . . ? C3 O2 H2F 111(2) . . ? V2 O2 H2F 126(2) . . ? C5 O3 V3 134.27(18) . . ? C5 O3 V2 120.15(16) . . ? V3 O3 V2 103.40(8) . . ? C7 O4 V1 130.85(16) . . ? C7 O4 V2 120.69(16) . . ? V1 O4 V2 103.94(8) . . ? C9 O5 V2 119.28(17) . . ? C9 O5 H5F 117(2) . . ? V2 O5 H5F 107(2) . . ? C11 O6 V2 121.61(17) . . ? C11 O6 V3 129.97(16) . . ? V2 O6 V3 101.53(8) . . ? C17 N1 C13 118.0(2) . . ? C17 N1 V1 125.1(2) . . ? C13 N1 V1 116.33(18) . . ? C22 N2 C18 118.1(2) . . ? C22 N2 V1 124.59(19) . . ? C18 N2 V1 117.28(18) . . ? C27 N3 C23 118.6(3) . . ? C27 N3 V3 123.8(2) . . ? C23 N3 V3 117.54(19) . . ? C32 N4 C28 117.9(3) . . ? C32 N4 V3 125.1(2) . . ? C28 N4 V3 117.01(19) . . ? O1 C1 C6 110.1(2) . . ? O1 C1 C2 110.1(2) . . ? C6 C1 C2 110.5(2) . . ? O1 C1 H1 108.7 . . ? C6 C1 H1 108.7 . . ? C2 C1 H1 108.7 . . ? C3 C2 C1 111.4(2) . . ? C3 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? C3 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 108.0 . . ? O2 C3 C2 108.9(2) . . ? O2 C3 C4 109.6(2) . . ? C2 C3 C4 111.9(3) . . ? O2 C3 H3 108.8 . . ? C2 C3 H3 108.8 . . ? C4 C3 H3 108.8 . . ? C3 C4 C5 112.4(2) . . ? C3 C4 H4A 109.1 . . ? C5 C4 H4A 109.1 . . ? C3 C4 H4B 109.1 . . ? C5 C4 H4B 109.1 . . ? H4A C4 H4B 107.9 . . ? O3 C5 C4 108.9(2) . . ? O3 C5 C6 110.4(2) . . ? C4 C5 C6 111.6(2) . . ? O3 C5 H5 108.6 . . ? C4 C5 H5 108.6 . . ? C6 C5 H5 108.6 . . ? C1 C6 C5 113.0(2) . . ? C1 C6 H6A 109.0 . . ? C5 C6 H6A 109.0 . . ? C1 C6 H6B 109.0 . . ? C5 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? O4 C7 C12 109.0(2) . . ? O4 C7 C8 109.6(2) . . ? C12 C7 C8 112.3(2) . . ? O4 C7 H7 108.6 . . ? C12 C7 H7 108.6 . . ? C8 C7 H7 108.6 . . ? C7 C8 C9 112.4(2) . . ? C7 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? C7 C8 H8B 109.1 . . ? C9 C8 H8B 109.1 . . ? H8A C8 H8B 107.9 . . ? O5 C9 C10 107.7(2) . . ? O5 C9 C8 110.8(2) . . ? C10 C9 C8 112.2(2) . . ? O5 C9 H9 108.7 . . ? C10 C9 H9 108.7 . . ? C8 C9 H9 108.7 . . ? C9 C10 C11 112.1(2) . . ? C9 C10 H10A 109.2 . . ? C11 C10 H10A 109.2 . . ? C9 C10 H10B 109.2 . . ? C11 C10 H10B 109.2 . . ? H10A C10 H10B 107.9 . . ? O6 C11 C10 110.4(2) . . ? O6 C11 C12 110.0(2) . . ? C10 C11 C12 110.2(2) . . ? O6 C11 H11 108.7 . . ? C10 C11 H11 108.7 . . ? C12 C11 H11 108.7 . . ? C7 C12 C11 113.2(2) . . ? C7 C12 H12A 108.9 . . ? C11 C12 H12A 108.9 . . ? C7 C12 H12B 108.9 . . ? C11 C12 H12B 108.9 . . ? H12A C12 H12B 107.8 . . ? N1 C13 C14 121.9(3) . . ? N1 C13 C18 115.1(2) . . ? C14 C13 C18 123.0(3) . . ? C15 C14 C13 119.3(3) . . ? C15 C14 H14 120.4 . . ? C13 C14 H14 120.4 . . ? C14 C15 C16 119.1(3) . . ? C14 C15 H15 120.5 . . ? C16 C15 H15 120.5 . . ? C17 C16 C15 119.0(3) . . ? C17 C16 H16 120.5 . . ? C15 C16 H16 120.5 . . ? N1 C17 C16 122.6(3) . . ? N1 C17 H17 118.7 . . ? C16 C17 H17 118.7 . . ? N2 C18 C19 121.3(3) . . ? N2 C18 C13 114.6(3) . . ? C19 C18 C13 124.0(3) . . ? C20 C19 C18 119.8(3) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C21 119.1(3) . . ? C19 C20 H20 120.4 . . ? C21 C20 H20 120.4 . . ? C22 C21 C20 118.5(3) . . ? C22 C21 H21 120.8 . . ? C20 C21 H21 120.8 . . ? N2 C22 C21 123.2(3) . . ? N2 C22 H22 118.4 . . ? C21 C22 H22 118.4 . . ? N3 C23 C24 121.6(3) . . ? N3 C23 C28 115.0(3) . . ? C24 C23 C28 123.4(3) . . ? C25 C24 C23 119.1(3) . . ? C25 C24 H24 120.5 . . ? C23 C24 H24 120.5 . . ? C26 C25 C24 119.3(3) . . ? C26 C25 H25 120.4 . . ? C24 C25 H25 120.4 . . ? C25 C26 C27 118.9(3) . . ? C25 C26 H26 120.6 . . ? C27 C26 H26 120.6 . . ? N3 C27 C26 122.6(3) . . ? N3 C27 H27 118.7 . . ? C26 C27 H27 118.7 . . ? N4 C28 C29 122.1(3) . . ? N4 C28 C23 114.6(3) . . ? C29 C28 C23 123.3(3) . . ? C28 C29 C30 119.0(3) . . ? C28 C29 H29 120.5 . . ? C30 C29 H29 120.5 . . ? C31 C30 C29 119.0(3) . . ? C31 C30 H30 120.5 . . ? C29 C30 H30 120.5 . . ? C30 C31 C32 119.2(3) . . ? C30 C31 H31 120.4 . . ? C32 C31 H31 120.4 . . ? N4 C32 C31 122.8(3) . . ? N4 C32 H32 118.6 . . ? C31 C32 H32 118.6 . . ? N5 C33 C34 178.8(4) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N6 C35 C36 178.5(5) . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 V1 V2 O6 -67.42(11) . . . . ? O1 V1 V2 O6 110.90(11) . . . . ? N2 V1 V2 O6 -157.69(9) . . . . ? N1 V1 V2 O6 131.81(11) . . . . ? Cl1 V1 V2 O6 28.31(6) . . . . ? Cl2 V1 V2 O6 -72.77(7) . . . . ? O4 V1 V2 O1 -178.32(13) . . . . ? N2 V1 V2 O1 91.41(11) . . . . ? N1 V1 V2 O1 20.91(13) . . . . ? Cl1 V1 V2 O1 -82.59(9) . . . . ? Cl2 V1 V2 O1 176.33(10) . . . . ? O1 V1 V2 O4 178.32(13) . . . . ? N2 V1 V2 O4 -90.27(11) . . . . ? N1 V1 V2 O4 -160.77(13) . . . . ? Cl1 V1 V2 O4 95.73(9) . . . . ? Cl2 V1 V2 O4 -5.35(9) . . . . ? O4 V1 V2 O2 112.93(11) . . . . ? O1 V1 V2 O2 -68.75(11) . . . . ? N2 V1 V2 O2 22.66(9) . . . . ? N1 V1 V2 O2 -47.84(12) . . . . ? Cl1 V1 V2 O2 -151.34(7) . . . . ? Cl2 V1 V2 O2 107.58(7) . . . . ? O4 V1 V2 O3 -154.48(11) . . . . ? O1 V1 V2 O3 23.84(11) . . . . ? N2 V1 V2 O3 115.25(9) . . . . ? N1 V1 V2 O3 44.75(12) . . . . ? Cl1 V1 V2 O3 -58.75(7) . . . . ? Cl2 V1 V2 O3 -159.83(7) . . . . ? O4 V1 V2 O5 28.18(11) . . . . ? O1 V1 V2 O5 -153.50(12) . . . . ? N2 V1 V2 O5 -62.09(10) . . . . ? N1 V1 V2 O5 -132.59(12) . . . . ? Cl1 V1 V2 O5 123.91(8) . . . . ? Cl2 V1 V2 O5 22.83(9) . . . . ? O4 V1 V2 V3 -106.43(9) . . . . ? O1 V1 V2 V3 71.89(9) . . . . ? N2 V1 V2 V3 163.30(6) . . . . ? N1 V1 V2 V3 92.81(10) . . . . ? Cl1 V1 V2 V3 -10.69(4) . . . . ? Cl2 V1 V2 V3 -111.77(4) . . . . ? O6 V2 V3 O3 -166.19(12) . . . . ? O1 V2 V3 O3 -59.02(10) . . . . ? O4 V2 V3 O3 -150.27(11) . . . . ? O2 V2 V3 O3 36.09(11) . . . . ? O5 V2 V3 O3 117.70(10) . . . . ? V1 V2 V3 O3 -99.11(9) . . . . ? O1 V2 V3 O6 107.18(10) . . . . ? O4 V2 V3 O6 15.93(11) . . . . ? O2 V2 V3 O6 -157.72(11) . . . . ? O3 V2 V3 O6 166.19(12) . . . . ? O5 V2 V3 O6 -76.11(10) . . . . ? V1 V2 V3 O6 67.08(8) . . . . ? O6 V2 V3 N3 -86.44(10) . . . . ? O1 V2 V3 N3 20.73(9) . . . . ? O4 V2 V3 N3 -70.52(10) . . . . ? O2 V2 V3 N3 115.84(10) . . . . ? O3 V2 V3 N3 79.75(11) . . . . ? O5 V2 V3 N3 -162.55(9) . . . . ? V1 V2 V3 N3 -19.36(7) . . . . ? O6 V2 V3 N4 -162.00(12) . . . . ? O1 V2 V3 N4 -54.83(11) . . . . ? O4 V2 V3 N4 -146.08(11) . . . . ? O2 V2 V3 N4 40.28(12) . . . . ? O3 V2 V3 N4 4.19(13) . . . . ? O5 V2 V3 N4 121.89(11) . . . . ? V1 V2 V3 N4 -94.92(10) . . . . ? O6 V2 V3 Cl4 100.14(8) . . . . ? O1 V2 V3 Cl4 -152.69(6) . . . . ? O4 V2 V3 Cl4 116.06(7) . . . . ? O2 V2 V3 Cl4 -57.58(8) . . . . ? O3 V2 V3 Cl4 -93.67(9) . . . . ? O5 V2 V3 Cl4 24.03(6) . . . . ? V1 V2 V3 Cl4 167.22(3) . . . . ? O6 V2 V3 Cl3 3.36(9) . . . . ? O1 V2 V3 Cl3 110.54(7) . . . . ? O4 V2 V3 Cl3 19.29(8) . . . . ? O2 V2 V3 Cl3 -154.36(8) . . . . ? O3 V2 V3 Cl3 169.55(9) . . . . ? O5 V2 V3 Cl3 -72.74(7) . . . . ? V1 V2 V3 Cl3 70.45(5) . . . . ? O6 V2 O1 C1 113.8(2) . . . . ? O4 V2 O1 C1 -161.4(2) . . . . ? O2 V2 O1 C1 -47.8(2) . . . . ? O3 V2 O1 C1 38.5(2) . . . . ? O5 V2 O1 C1 -103.1(3) . . . . ? V3 V2 O1 C1 69.6(2) . . . . ? V1 V2 O1 C1 -160.3(2) . . . . ? O6 V2 O1 V1 -85.91(10) . . . . ? O4 V2 O1 V1 -1.06(8) . . . . ? O2 V2 O1 V1 112.55(10) . . . . ? O3 V2 O1 V1 -161.16(9) . . . . ? O5 V2 O1 V1 57.3(2) . . . . ? V3 V2 O1 V1 -130.10(6) . . . . ? O4 V1 O1 C1 159.0(2) . . . . ? N2 V1 O1 C1 68.3(2) . . . . ? N1 V1 O1 C1 -7.1(2) . . . . ? Cl1 V1 O1 C1 -100.9(2) . . . . ? Cl2 V1 O1 C1 142.4(3) . . . . ? V2 V1 O1 C1 158.0(3) . . . . ? O4 V1 O1 V2 1.07(8) . . . . ? N2 V1 O1 V2 -89.68(9) . . . . ? N1 V1 O1 V2 -165.12(9) . . . . ? Cl1 V1 O1 V2 101.12(7) . . . . ? Cl2 V1 O1 V2 -15.6(4) . . . . ? O6 V2 O2 C3 -95.7(3) . . . . ? O1 V2 O2 C3 47.5(2) . . . . ? O4 V2 O2 C3 121.1(2) . . . . ? O3 V2 O2 C3 -43.3(2) . . . . ? O5 V2 O2 C3 -154.3(2) . . . . ? V3 V2 O2 C3 -64.1(2) . . . . ? V1 V2 O2 C3 83.6(2) . . . . ? O6 V3 O3 C5 153.7(2) . . . . ? N3 V3 O3 C5 61.0(2) . . . . ? N4 V3 O3 C5 -14.6(2) . . . . ? Cl4 V3 O3 C5 -108.3(2) . . . . ? Cl3 V3 O3 C5 116.9(3) . . . . ? V2 V3 O3 C5 162.4(3) . . . . ? O6 V3 O3 V2 -8.69(8) . . . . ? N3 V3 O3 V2 -101.41(9) . . . . ? N4 V3 O3 V2 -176.97(9) . . . . ? Cl4 V3 O3 V2 89.25(7) . . . . ? Cl3 V3 O3 V2 -45.5(4) . . . . ? O6 V2 O3 C5 -156.37(19) . . . . ? O1 V2 O3 C5 -38.33(19) . . . . ? O4 V2 O3 C5 -94.8(2) . . . . ? O2 V2 O3 C5 46.08(18) . . . . ? O5 V2 O3 C5 124.55(18) . . . . ? V3 V2 O3 C5 -165.5(2) . . . . ? V1 V2 O3 C5 -53.1(2) . . . . ? O6 V2 O3 V3 9.14(8) . . . . ? O1 V2 O3 V3 127.18(9) . . . . ? O4 V2 O3 V3 70.7(2) . . . . ? O2 V2 O3 V3 -148.41(10) . . . . ? O5 V2 O3 V3 -69.94(10) . . . . ? V1 V2 O3 V3 112.44(7) . . . . ? O1 V1 O4 C7 154.4(2) . . . . ? N2 V1 O4 C7 -113.9(2) . . . . ? N1 V1 O4 C7 -136.8(3) . . . . ? Cl1 V1 O4 C7 64.6(2) . . . . ? Cl2 V1 O4 C7 -28.5(2) . . . . ? V2 V1 O4 C7 155.5(3) . . . . ? O1 V1 O4 V2 -1.07(8) . . . . ? N2 V1 O4 V2 90.57(9) . . . . ? N1 V1 O4 V2 67.7(4) . . . . ? Cl1 V1 O4 V2 -90.85(7) . . . . ? Cl2 V1 O4 V2 176.01(7) . . . . ? O6 V2 O4 C7 -39.78(19) . . . . ? O1 V2 O4 C7 -157.5(2) . . . . ? O2 V2 O4 C7 123.92(19) . . . . ? O3 V2 O4 C7 -98.7(2) . . . . ? O5 V2 O4 C7 44.75(19) . . . . ? V3 V2 O4 C7 -50.0(2) . . . . ? V1 V2 O4 C7 -158.6(2) . . . . ? O6 V2 O4 V1 118.82(9) . . . . ? O1 V2 O4 V1 1.09(8) . . . . ? O2 V2 O4 V1 -77.48(10) . . . . ? O3 V2 O4 V1 59.9(2) . . . . ? O5 V2 O4 V1 -156.65(9) . . . . ? V3 V2 O4 V1 108.58(7) . . . . ? O6 V2 O5 C9 50.70(19) . . . . ? O1 V2 O5 C9 -97.0(2) . . . . ? O4 V2 O5 C9 -40.94(19) . . . . ? O2 V2 O5 C9 -153.0(2) . . . . ? O3 V2 O5 C9 124.44(18) . . . . ? V3 V2 O5 C9 89.90(18) . . . . ? V1 V2 O5 C9 -57.8(2) . . . . ? O1 V2 O6 C11 114.48(18) . . . . ? O4 V2 O6 C11 38.43(18) . . . . ? O2 V2 O6 C11 -107.7(2) . . . . ? O3 V2 O6 C11 -162.05(19) . . . . ? O5 V2 O6 C11 -49.98(18) . . . . ? V3 V2 O6 C11 -153.6(2) . . . . ? V1 V2 O6 C11 73.01(18) . . . . ? O1 V2 O6 V3 -91.96(9) . . . . ? O4 V2 O6 V3 -168.01(8) . . . . ? O2 V2 O6 V3 45.8(2) . . . . ? O3 V2 O6 V3 -8.49(7) . . . . ? O5 V2 O6 V3 103.58(8) . . . . ? V1 V2 O6 V3 -133.42(5) . . . . ? O3 V3 O6 C11 159.3(2) . . . . ? N3 V3 O6 C11 -113.5(2) . . . . ? N4 V3 O6 C11 -146.3(3) . . . . ? Cl4 V3 O6 C11 66.3(2) . . . . ? Cl3 V3 O6 C11 -27.2(2) . . . . ? V2 V3 O6 C11 150.3(2) . . . . ? O3 V3 O6 V2 8.98(8) . . . . ? N3 V3 O6 V2 96.19(9) . . . . ? N4 V3 O6 V2 63.3(4) . . . . ? Cl4 V3 O6 V2 -84.00(7) . . . . ? Cl3 V3 O6 V2 -177.51(6) . . . . ? O4 V1 N1 C17 -155.2(3) . . . . ? O1 V1 N1 C17 -89.0(2) . . . . ? N2 V1 N1 C17 -178.9(2) . . . . ? Cl1 V1 N1 C17 3.7(2) . . . . ? Cl2 V1 N1 C17 96.1(2) . . . . ? V2 V1 N1 C17 -101.9(2) . . . . ? O4 V1 N1 C13 33.3(5) . . . . ? O1 V1 N1 C13 99.5(2) . . . . ? N2 V1 N1 C13 9.63(19) . . . . ? Cl1 V1 N1 C13 -167.82(19) . . . . ? Cl2 V1 N1 C13 -75.34(19) . . . . ? V2 V1 N1 C13 86.6(2) . . . . ? O4 V1 N2 C22 -1.3(2) . . . . ? O1 V1 N2 C22 75.2(2) . . . . ? N1 V1 N2 C22 172.8(2) . . . . ? Cl1 V1 N2 C22 -174.3(2) . . . . ? Cl2 V1 N2 C22 -95.0(2) . . . . ? V2 V1 N2 C22 36.8(2) . . . . ? O4 V1 N2 C18 -178.26(19) . . . . ? O1 V1 N2 C18 -101.80(19) . . . . ? N1 V1 N2 C18 -4.11(19) . . . . ? Cl1 V1 N2 C18 8.7(5) . . . . ? Cl2 V1 N2 C18 88.07(19) . . . . ? V2 V1 N2 C18 -140.11(19) . . . . ? O3 V3 N3 C27 82.9(2) . . . . ? O6 V3 N3 C27 6.0(2) . . . . ? N4 V3 N3 C27 178.0(2) . . . . ? Cl4 V3 N3 C27 -173.0(3) . . . . ? Cl3 V3 N3 C27 -88.1(2) . . . . ? V2 V3 N3 C27 44.0(2) . . . . ? O3 V3 N3 C23 -93.2(2) . . . . ? O6 V3 N3 C23 -170.0(2) . . . . ? N4 V3 N3 C23 1.9(2) . . . . ? Cl4 V3 N3 C23 10.9(5) . . . . ? Cl3 V3 N3 C23 95.8(2) . . . . ? V2 V3 N3 C23 -132.0(2) . . . . ? O3 V3 N4 C32 -94.6(2) . . . . ? O6 V3 N4 C32 -147.1(3) . . . . ? N3 V3 N4 C32 178.9(3) . . . . ? Cl4 V3 N4 C32 0.6(2) . . . . ? Cl3 V3 N4 C32 93.6(2) . . . . ? V2 V3 N4 C32 -97.2(2) . . . . ? O3 V3 N4 C28 85.0(2) . . . . ? O6 V3 N4 C28 32.4(5) . . . . ? N3 V3 N4 C28 -1.58(19) . . . . ? Cl4 V3 N4 C28 -179.88(19) . . . . ? Cl3 V3 N4 C28 -86.9(2) . . . . ? V2 V3 N4 C28 82.3(2) . . . . ? V2 O1 C1 C6 -57.1(3) . . . . ? V1 O1 C1 C6 148.61(18) . . . . ? V2 O1 C1 C2 65.0(3) . . . . ? V1 O1 C1 C2 -89.3(3) . . . . ? O1 C1 C2 C3 -66.3(3) . . . . ? C6 C1 C2 C3 55.5(3) . . . . ? V2 O2 C3 C2 -63.5(3) . . . . ? V2 O2 C3 C4 59.2(3) . . . . ? C1 C2 C3 O2 65.3(3) . . . . ? C1 C2 C3 C4 -56.0(3) . . . . ? O2 C3 C4 C5 -66.9(3) . . . . ? C2 C3 C4 C5 54.0(3) . . . . ? V3 O3 C5 C4 134.4(2) . . . . ? V2 O3 C5 C4 -65.5(3) . . . . ? V3 O3 C5 C6 -102.8(3) . . . . ? V2 O3 C5 C6 57.3(3) . . . . ? C3 C4 C5 O3 70.9(3) . . . . ? C3 C4 C5 C6 -51.2(3) . . . . ? O1 C1 C6 C5 68.1(3) . . . . ? C2 C1 C6 C5 -53.7(3) . . . . ? O3 C5 C6 C1 -69.4(3) . . . . ? C4 C5 C6 C1 51.8(3) . . . . ? V1 O4 C7 C12 -93.4(2) . . . . ? V2 O4 C7 C12 58.7(3) . . . . ? V1 O4 C7 C8 143.25(19) . . . . ? V2 O4 C7 C8 -64.7(3) . . . . ? O4 C7 C8 C9 70.8(3) . . . . ? C12 C7 C8 C9 -50.5(3) . . . . ? V2 O5 C9 C10 -65.9(2) . . . . ? V2 O5 C9 C8 57.2(3) . . . . ? C7 C8 C9 O5 -68.3(3) . . . . ? C7 C8 C9 C10 52.2(3) . . . . ? O5 C9 C10 C11 67.4(3) . . . . ? C8 C9 C10 C11 -54.8(3) . . . . ? V2 O6 C11 C10 65.9(3) . . . . ? V3 O6 C11 C10 -79.4(3) . . . . ? V2 O6 C11 C12 -55.9(3) . . . . ? V3 O6 C11 C12 158.76(17) . . . . ? C9 C10 C11 O6 -66.9(3) . . . . ? C9 C10 C11 C12 54.7(3) . . . . ? O4 C7 C12 C11 -69.7(3) . . . . ? C8 C7 C12 C11 52.0(3) . . . . ? O6 C11 C12 C7 68.3(3) . . . . ? C10 C11 C12 C7 -53.6(3) . . . . ? C17 N1 C13 C14 -4.3(4) . . . . ? V1 N1 C13 C14 167.8(2) . . . . ? C17 N1 C13 C18 174.4(2) . . . . ? V1 N1 C13 C18 -13.5(3) . . . . ? N1 C13 C14 C15 2.9(4) . . . . ? C18 C13 C14 C15 -175.8(3) . . . . ? C13 C14 C15 C16 0.9(4) . . . . ? C14 C15 C16 C17 -3.1(4) . . . . ? C13 N1 C17 C16 2.0(4) . . . . ? V1 N1 C17 C16 -169.4(2) . . . . ? C15 C16 C17 N1 1.7(4) . . . . ? C22 N2 C18 C19 -1.1(4) . . . . ? V1 N2 C18 C19 176.0(2) . . . . ? C22 N2 C18 C13 -178.6(2) . . . . ? V1 N2 C18 C13 -1.4(3) . . . . ? N1 C13 C18 N2 9.8(4) . . . . ? C14 C13 C18 N2 -171.5(3) . . . . ? N1 C13 C18 C19 -167.6(3) . . . . ? C14 C13 C18 C19 11.1(4) . . . . ? N2 C18 C19 C20 -1.0(4) . . . . ? C13 C18 C19 C20 176.2(3) . . . . ? C18 C19 C20 C21 1.8(4) . . . . ? C19 C20 C21 C22 -0.5(4) . . . . ? C18 N2 C22 C21 2.5(4) . . . . ? V1 N2 C22 C21 -174.4(2) . . . . ? C20 C21 C22 N2 -1.7(5) . . . . ? C27 N3 C23 C24 1.8(4) . . . . ? V3 N3 C23 C24 178.1(2) . . . . ? C27 N3 C23 C28 -178.2(2) . . . . ? V3 N3 C23 C28 -2.0(3) . . . . ? N3 C23 C24 C25 -1.7(4) . . . . ? C28 C23 C24 C25 178.3(3) . . . . ? C23 C24 C25 C26 0.5(4) . . . . ? C24 C25 C26 C27 0.7(5) . . . . ? C23 N3 C27 C26 -0.7(4) . . . . ? V3 N3 C27 C26 -176.7(2) . . . . ? C25 C26 C27 N3 -0.6(5) . . . . ? C32 N4 C28 C29 1.1(4) . . . . ? V3 N4 C28 C29 -178.5(2) . . . . ? C32 N4 C28 C23 -179.4(3) . . . . ? V3 N4 C28 C23 1.1(3) . . . . ? N3 C23 C28 N4 0.6(4) . . . . ? C24 C23 C28 N4 -179.5(3) . . . . ? N3 C23 C28 C29 -179.9(3) . . . . ? C24 C23 C28 C29 0.1(5) . . . . ? N4 C28 C29 C30 -1.9(4) . . . . ? C23 C28 C29 C30 178.6(3) . . . . ? C28 C29 C30 C31 0.9(5) . . . . ? C29 C30 C31 C32 0.8(5) . . . . ? C28 N4 C32 C31 0.7(4) . . . . ? V3 N4 C32 C31 -179.7(2) . . . . ? C30 C31 C32 N4 -1.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 24.73 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.412 _refine_diff_density_min -0.454 _refine_diff_density_rms 0.120 # Attachment '7.cif' data_platon _database_code_depnum_ccdc_archive 'CCDC 736087' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[V4Cl6(thme)2(t-bu-bipy)3]4MeCNH2O' _chemical_formula_sum 'C72 H104 Cl6 N10 O7 V4' _chemical_formula_weight 1638.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting TRICLINIC _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.0160(5) _cell_length_b 19.1213(8) _cell_length_c 19.4392(8) _cell_angle_alpha 119.051(4) _cell_angle_beta 92.253(3) _cell_angle_gamma 104.919(3) _cell_volume 4316.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 8440 _cell_measurement_theta_min 2.5707 _cell_measurement_theta_max 28.5297 _exptl_crystal_description BLOCK _exptl_crystal_colour BROWN _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.260 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1712 _exptl_absorpt_coefficient_mu 0.657 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7347 _exptl_absorpt_correction_T_max 0.8798 _exptl_absorpt_process_details ? _exptl_special_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction XCalibur 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.336 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25458 _diffrn_reflns_av_R_equivalents 0.0534 _diffrn_reflns_av_sigmaI/netI 0.1401 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.57 _diffrn_reflns_theta_max 25.03 _reflns_number_total 14776 _reflns_number_gt 7686 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.24 (release 21-04-2008 CrysAlis171 .NET) (compiled Apr 21 2008,18:23:10) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.29 (release 10-06-2008 CrysAlis171 .NET) (compiled Jun 10 2008,16:49:55) ; _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _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. Several of the isotropic displacement parameters have maxi:min ratios of around 4:1 is reflected in the large degree of disorder in the system, splitting these sites was considered but since no new chemical information would result it was decided to leave them as they were. Some of the non-H atoms in the solvent acetonitrile were left isotropic, several attempts were made to model the solvent molecules but this resulted in persistent npds, and since no new chemical information would result these attempts were abandoned. ; _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^)+(0.0474P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14776 _refine_ls_number_parameters 886 _refine_ls_number_restraints 65 _refine_ls_R_factor_all 0.1079 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.1249 _refine_ls_wR_factor_gt 0.1150 _refine_ls_goodness_of_fit_ref 0.885 _refine_ls_restrained_S_all 0.905 _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 C1 C 0.6749(4) 0.9654(2) 0.2313(3) 0.0205(11) Uani 1 1 d . . . H1A H 0.7078 1.0045 0.2884 0.025 Uiso 1 1 calc R . . H1B H 0.6985 0.9941 0.2015 0.025 Uiso 1 1 calc R . . C2 C 0.6699(3) 0.8278(2) 0.1076(2) 0.0190(11) Uani 1 1 d . . . H2A H 0.7002 0.8582 0.0807 0.023 Uiso 1 1 calc R . . H2B H 0.6936 0.7782 0.0893 0.023 Uiso 1 1 calc R . . C3 C 0.6738(3) 0.8393(3) 0.2444(3) 0.0208(11) Uani 1 1 d . . . H3A H 0.7053 0.7942 0.2281 0.025 Uiso 1 1 calc R . . H3B H 0.6985 0.8793 0.3026 0.025 Uiso 1 1 calc R . . C4 C 0.7075(4) 0.8864(3) 0.1991(3) 0.0202(11) Uani 1 1 d . . . C5 C 0.8229(3) 0.9156(3) 0.2153(3) 0.0243(12) Uani 1 1 d . . . H5A H 0.8488 0.9506 0.2733 0.036 Uiso 1 1 calc R . . H5B H 0.8473 0.9486 0.1900 0.036 Uiso 1 1 calc R . . H5C H 0.8465 0.8663 0.1930 0.036 Uiso 1 1 calc R . . C6 C 0.2932(3) 0.8454(3) 0.2235(3) 0.0192(11) Uani 1 1 d . . . H6A H 0.2607 0.8881 0.2305 0.023 Uiso 1 1 calc R . . H6B H 0.2710 0.8253 0.2603 0.023 Uiso 1 1 calc R . . C7 C 0.2898(3) 0.7966(3) 0.0748(2) 0.0173(11) Uani 1 1 d . . . H7A H 0.2556 0.7492 0.0202 0.021 Uiso 1 1 calc R . . H7B H 0.2669 0.8449 0.0846 0.021 Uiso 1 1 calc R . . C8 C 0.2907(4) 0.6951(2) 0.1243(3) 0.0201(11) Uani 1 1 d . . . H8A H 0.2594 0.6749 0.1588 0.024 Uiso 1 1 calc R . . H8B H 0.2651 0.6485 0.0678 0.024 Uiso 1 1 calc R . . C9 C 0.2573(3) 0.7704(2) 0.1362(3) 0.0188(11) Uani 1 1 d . . . C10 C 0.1418(3) 0.7417(3) 0.1199(3) 0.0247(12) Uani 1 1 d . . . H10A H 0.1183 0.7857 0.1198 0.037 Uiso 1 1 calc R . . H10B H 0.1177 0.7315 0.1619 0.037 Uiso 1 1 calc R . . H10C H 0.1157 0.6895 0.0676 0.037 Uiso 1 1 calc R . . C11 C 0.3795(4) 1.0610(3) 0.4536(3) 0.0231(12) Uani 1 1 d . . . H11 H 0.4287 1.0497 0.4781 0.028 Uiso 1 1 calc R . . C12 C 0.3103(4) 1.0917(3) 0.4960(3) 0.0255(12) Uani 1 1 d . . . H12 H 0.3122 1.1009 0.5488 0.031 Uiso 1 1 calc R . . C13 C 0.2367(4) 1.1099(3) 0.4631(3) 0.0257(12) Uani 1 1 d . . . C14 C 0.2391(4) 1.0951(3) 0.3857(3) 0.0241(12) Uani 1 1 d . . . H14 H 0.1916 1.1078 0.3610 0.029 Uiso 1 1 calc R . . C15 C 0.3095(4) 1.0623(3) 0.3445(3) 0.0179(11) Uani 1 1 d . . . C16 C 0.3142(4) 1.0431(3) 0.2616(3) 0.0193(11) Uani 1 1 d . . . C17 C 0.2397(4) 1.0418(3) 0.2124(3) 0.0227(12) Uani 1 1 d . . . H17 H 0.1815 1.0542 0.2319 0.027 Uiso 1 1 calc R . . C18 C 0.2483(4) 1.0227(2) 0.1345(3) 0.0194(11) Uani 1 1 d . . . C19 C 0.3383(4) 1.0109(2) 0.1121(3) 0.0218(12) Uani 1 1 d . . . H19 H 0.3505 1.0027 0.0614 0.026 Uiso 1 1 calc R . . C20 C 0.4104(4) 1.0111(2) 0.1629(3) 0.0220(12) Uani 1 1 d . . . H20 H 0.4709 1.0018 0.1458 0.026 Uiso 1 1 calc R . . C21 C 0.1575(4) 1.1464(3) 0.5077(3) 0.0318(13) Uani 1 1 d . . . C22 C 0.1562(4) 1.1457(3) 0.5859(3) 0.0367(14) Uani 1 1 d . . . H22A H 0.1047 1.1693 0.6122 0.055 Uiso 1 1 calc R . . H22B H 0.2223 1.1797 0.6214 0.055 Uiso 1 1 calc R . . H22C H 0.1408 1.0876 0.5742 0.055 Uiso 1 1 calc R . . C23 C 0.0535(4) 1.0942(4) 0.4535(3) 0.0500(17) Uani 1 1 d . . . H23A H 0.0503 1.1012 0.4069 0.075 Uiso 1 1 calc R . . H23B H 0.0018 1.1134 0.4835 0.075 Uiso 1 1 calc R . . H23C H 0.0416 1.0345 0.4354 0.075 Uiso 1 1 calc R . . C24 C 0.1841(5) 1.2382(3) 0.5272(3) 0.0481(17) Uani 1 1 d . . . H24A H 0.1846 1.2393 0.4774 0.072 Uiso 1 1 calc R . . H24B H 0.2508 1.2709 0.5620 0.072 Uiso 1 1 calc R . . H24C H 0.1339 1.2629 0.5548 0.072 Uiso 1 1 calc R . . C25 C 0.1646(4) 1.0146(3) 0.0765(3) 0.0259(12) Uani 1 1 d . . . C26 C 0.0659(4) 1.0130(4) 0.1077(4) 0.066(2) Uani 1 1 d . . . H26A H 0.0492 0.9700 0.1229 0.098 Uiso 1 1 calc R . . H26B H 0.0118 0.9997 0.0656 0.098 Uiso 1 1 calc R . . H26C H 0.0735 1.0684 0.1547 0.098 Uiso 1 1 calc R . . C27 C 0.1963(5) 1.0887(3) 0.0634(4) 0.0526(17) Uani 1 1 d . . . H27A H 0.2055 1.1412 0.1142 0.079 Uiso 1 1 calc R . . H27B H 0.1440 1.0821 0.0237 0.079 Uiso 1 1 calc R . . H27C H 0.2597 1.0906 0.0438 0.079 Uiso 1 1 calc R . . C28 C 0.1454(5) 0.9325(3) -0.0032(3) 0.067(2) Uani 1 1 d . . . H28A H 0.2028 0.9368 -0.0298 0.101 Uiso 1 1 calc R . . H28B H 0.0843 0.9223 -0.0375 0.101 Uiso 1 1 calc R . . H28C H 0.1368 0.8857 0.0065 0.101 Uiso 1 1 calc R . . C29 C 0.3754(4) 0.8458(3) -0.1109(3) 0.0252(12) Uani 1 1 d . . . H29 H 0.4291 0.8975 -0.0824 0.030 Uiso 1 1 calc R . . C30 C 0.3047(4) 0.8362(3) -0.1696(3) 0.0249(12) Uani 1 1 d . . . H30 H 0.3120 0.8798 -0.1815 0.030 Uiso 1 1 calc R . . C31 C 0.2227(4) 0.7623(3) -0.2109(3) 0.0235(12) Uani 1 1 d . . . C32 C 0.2196(4) 0.7007(3) -0.1908(3) 0.0232(12) Uani 1 1 d . . . H32 H 0.1657 0.6490 -0.2175 0.028 Uiso 1 1 calc R . . C33 C 0.2928(4) 0.7138(3) -0.1333(3) 0.0202(12) Uani 1 1 d . . . C34 C 0.2977(4) 0.6501(3) -0.1112(3) 0.0212(12) Uani 1 1 d . . . C35 C 0.2197(4) 0.5737(3) -0.1398(3) 0.0276(13) Uani 1 1 d . . . H35 H 0.1599 0.5613 -0.1741 0.033 Uiso 1 1 calc R . . C36 C 0.2297(4) 0.5159(3) -0.1179(3) 0.0254(13) Uani 1 1 d . . . C37 C 0.3212(4) 0.5374(3) -0.0701(3) 0.0220(12) Uani 1 1 d . . . H37 H 0.3336 0.4989 -0.0562 0.026 Uiso 1 1 calc R . . C38 C 0.3938(4) 0.6137(2) -0.0431(3) 0.0203(11) Uani 1 1 d . . . H38 H 0.4550 0.6266 -0.0101 0.024 Uiso 1 1 calc R . . C39 C 0.1419(4) 0.7451(3) -0.2762(3) 0.0290(13) Uani 1 1 d . . . C40 C 0.1551(4) 0.8210(3) -0.2870(3) 0.0330(13) Uani 1 1 d . . . H40A H 0.1521 0.8694 -0.2367 0.050 Uiso 1 1 calc R . . H40B H 0.1012 0.8071 -0.3295 0.050 Uiso 1 1 calc R . . H40C H 0.2204 0.8349 -0.3017 0.050 Uiso 1 1 calc R . . C41 C 0.0380(4) 0.7253(3) -0.2529(3) 0.0422(15) Uani 1 1 d . . . H41A H 0.0250 0.6738 -0.2503 0.063 Uiso 1 1 calc R . . H41B H -0.0147 0.7171 -0.2932 0.063 Uiso 1 1 calc R . . H41C H 0.0380 0.7724 -0.2004 0.063 Uiso 1 1 calc R . . C42 C 0.1450(5) 0.6709(3) -0.3556(3) 0.0457(16) Uani 1 1 d . . . H42A H 0.2108 0.6843 -0.3700 0.069 Uiso 1 1 calc R . . H42B H 0.0920 0.6595 -0.3975 0.069 Uiso 1 1 calc R . . H42C H 0.1343 0.6209 -0.3507 0.069 Uiso 1 1 calc R . . C43 C 0.1450(4) 0.4330(3) -0.1471(3) 0.0338(14) Uani 1 1 d . . . C44 C 0.0423(4) 0.4452(3) -0.1509(3) 0.0348(14) Uani 1 1 d . . . H44A H 0.0373 0.4883 -0.0977 0.052 Uiso 1 1 calc R . . H44B H -0.0104 0.3919 -0.1679 0.052 Uiso 1 1 calc R . . H44C H 0.0338 0.4632 -0.1895 0.052 Uiso 1 1 calc R . . C45 C 0.1567(4) 0.3690(3) -0.2304(3) 0.0554(19) Uani 1 1 d . . . H45A H 0.1030 0.3153 -0.2513 0.083 Uiso 1 1 calc R . . H45B H 0.2222 0.3604 -0.2266 0.083 Uiso 1 1 calc R . . H45C H 0.1525 0.3905 -0.2668 0.083 Uiso 1 1 calc R . . C46 C 0.1543(5) 0.4005(3) -0.0891(4) 0.065(2) Uani 1 1 d . . . H46A H 0.1627 0.4464 -0.0338 0.097 Uiso 1 1 calc R . . H46B H 0.2128 0.3804 -0.0949 0.097 Uiso 1 1 calc R . . H46C H 0.0932 0.3541 -0.1019 0.097 Uiso 1 1 calc R . . C47 C 0.3781(4) 0.4903(3) 0.1008(3) 0.0229(12) Uani 1 1 d . . . H47 H 0.4296 0.4892 0.0704 0.027 Uiso 1 1 calc R . . C48 C 0.3049(4) 0.4146(2) 0.0789(3) 0.0230(12) Uani 1 1 d . . . H48 H 0.3077 0.3634 0.0348 0.028 Uiso 1 1 calc R . . C49 C 0.2279(4) 0.4137(3) 0.1213(3) 0.0209(11) Uani 1 1 d . . . C50 C 0.2294(4) 0.4915(3) 0.1861(3) 0.0243(12) Uani 1 1 d . . . H50 H 0.1783 0.4942 0.2171 0.029 Uiso 1 1 calc R . . C51 C 0.3051(3) 0.5645(2) 0.2050(2) 0.0180(11) Uani 1 1 d . . . C52 C 0.3120(4) 0.6492(3) 0.2738(3) 0.0213(12) Uani 1 1 d . . . C53 C 0.2437(4) 0.6640(3) 0.3232(3) 0.0214(12) Uani 1 1 d . . . H53 H 0.1875 0.6181 0.3141 0.026 Uiso 1 1 calc R . . C54 C 0.2545(4) 0.7453(3) 0.3871(3) 0.0215(12) Uani 1 1 d . . . C55 C 0.3406(4) 0.8085(3) 0.3983(3) 0.0211(12) Uani 1 1 d . . . H55 H 0.3534 0.8645 0.4418 0.025 Uiso 1 1 calc R . . C56 C 0.4074(4) 0.7908(3) 0.3472(2) 0.0192(11) Uani 1 1 d . . . H56 H 0.4653 0.8352 0.3560 0.023 Uiso 1 1 calc R . . C57 C 0.1456(4) 0.3332(3) 0.1022(3) 0.0247(12) Uani 1 1 d . . . C58 C 0.1458(4) 0.2574(3) 0.0207(3) 0.0355(15) Uani 1 1 d . . . H58A H 0.0914 0.2073 0.0100 0.053 Uiso 1 1 calc R . . H58B H 0.2105 0.2471 0.0224 0.053 Uiso 1 1 calc R . . H58C H 0.1354 0.2698 -0.0219 0.053 Uiso 1 1 calc R . . C59 C 0.1699(4) 0.3135(3) 0.1684(3) 0.0333(14) Uani 1 1 d . . . H59A H 0.1662 0.3591 0.2205 0.050 Uiso 1 1 calc R . . H59B H 0.2378 0.3088 0.1698 0.050 Uiso 1 1 calc R . . H59C H 0.1210 0.2603 0.1565 0.050 Uiso 1 1 calc R . . C60 C 0.0428(4) 0.3450(3) 0.1010(3) 0.0318(14) Uani 1 1 d . . . H60A H 0.0416 0.3920 0.1531 0.048 Uiso 1 1 calc R . . H60B H -0.0086 0.2933 0.0902 0.048 Uiso 1 1 calc R . . H60C H 0.0290 0.3572 0.0589 0.048 Uiso 1 1 calc R . . C61 C 0.1731(4) 0.7607(3) 0.4374(3) 0.0265(13) Uani 1 1 d . . . C62 C 0.1616(4) 0.7065(3) 0.4770(3) 0.0408(15) Uani 1 1 d . . . H62A H 0.1454 0.6469 0.4354 0.061 Uiso 1 1 calc R . . H62B H 0.1073 0.7140 0.5075 0.061 Uiso 1 1 calc R . . H62C H 0.2248 0.7242 0.5133 0.061 Uiso 1 1 calc R . . C63 C 0.1984(4) 0.8520(3) 0.5032(3) 0.0369(15) Uani 1 1 d . . . H63A H 0.2631 0.8695 0.5376 0.055 Uiso 1 1 calc R . . H63B H 0.1457 0.8582 0.5354 0.055 Uiso 1 1 calc R . . H63C H 0.2027 0.8873 0.4794 0.055 Uiso 1 1 calc R . . C64 C 0.0740(4) 0.7320(3) 0.3820(3) 0.0416(15) Uani 1 1 d . . . H64A H 0.0801 0.7648 0.3554 0.062 Uiso 1 1 calc R . . H64B H 0.0207 0.7407 0.4134 0.062 Uiso 1 1 calc R . . H64C H 0.0573 0.6720 0.3415 0.062 Uiso 1 1 calc R . . Cl1 Cl 0.57194(9) 0.98689(6) 0.40322(6) 0.0216(3) Uani 1 1 d . . . Cl2 Cl 0.59346(9) 1.14017(6) 0.35380(7) 0.0245(3) Uani 1 1 d . . . Cl3 Cl 0.57236(9) 0.93627(6) 0.03736(6) 0.0238(3) Uani 1 1 d . . . Cl4 Cl 0.58031(10) 0.73858(7) -0.09775(7) 0.0285(3) Uani 1 1 d . . . Cl5 Cl 0.57492(9) 0.62593(6) 0.09550(6) 0.0226(3) Uani 1 1 d . . . Cl6 Cl 0.59329(10) 0.68225(7) 0.29242(7) 0.0274(3) Uani 1 1 d . . . N1 N 0.3817(3) 1.0459(2) 0.3783(2) 0.0207(10) Uani 1 1 d . . . N2 N 0.3971(3) 1.0240(2) 0.2357(2) 0.0178(9) Uani 1 1 d . . . N3 N 0.3723(3) 0.7869(2) -0.0923(2) 0.0200(10) Uani 1 1 d . . . N4 N 0.3822(3) 0.6707(2) -0.0611(2) 0.0173(9) Uani 1 1 d . . . N5 N 0.3795(3) 0.5643(2) 0.1622(2) 0.0174(9) Uani 1 1 d . . . N6 N 0.3934(3) 0.7129(2) 0.2851(2) 0.0174(9) Uani 1 1 d . . . O1 O 0.5686(2) 0.94771(16) 0.22478(16) 0.0166(7) Uani 1 1 d . . . O2 O 0.5640(2) 0.79926(16) 0.08354(16) 0.0173(7) Uani 1 1 d . . . O3 O 0.5680(2) 0.80275(16) 0.22998(16) 0.0163(7) Uani 1 1 d . . . O4 O 0.4000(2) 0.88427(16) 0.24497(16) 0.0174(7) Uani 1 1 d . . . O5 O 0.3956(2) 0.81946(16) 0.07752(16) 0.0175(7) Uani 1 1 d . . . O6 O 0.3970(2) 0.71399(16) 0.14229(16) 0.0181(7) Uani 1 1 d . . . V1 V 0.48459(6) 0.82824(4) 0.16778(4) 0.0168(2) Uani 1 1 d . . . V2 V 0.48913(6) 1.00255(4) 0.30774(4) 0.0180(2) Uani 1 1 d . . . V3 V 0.48005(6) 0.79632(4) -0.00526(4) 0.0190(2) Uani 1 1 d . . . V4 V 0.48622(6) 0.68385(4) 0.19766(4) 0.0187(2) Uani 1 1 d . . . O100 O 1.0118(4) 0.5036(3) 0.7029(2) 0.0710(15) Uani 1 1 d D . . H100 H 1.046(3) 0.478(3) 0.6538(19) 0.035(10) Uiso 1 1 d DU . . H101 H 0.948(2) 0.511(3) 0.686(2) 0.035(10) Uiso 1 1 d DU . . N10 N 0.1540(7) 0.4850(5) 0.3792(5) 0.144(3) Uiso 1 1 d D . . C100 C 0.1998(9) 0.4718(7) 0.4173(7) 0.157(3) Uiso 1 1 d DU . . C101 C 0.2662(8) 0.4486(7) 0.4655(6) 0.159(3) Uiso 1 1 d DU . . H10D H 0.2305 0.4412 0.5050 0.239 Uiso 1 1 calc R . . H10E H 0.3304 0.4942 0.4931 0.239 Uiso 1 1 calc R . . H10F H 0.2790 0.3961 0.4282 0.239 Uiso 1 1 calc R . . N11 N 0.457(3) 0.5536(12) 0.432(3) 0.91(4) Uiso 1 1 d D . . C110 C 0.5129(8) 0.6288(7) 0.4721(6) 0.127(3) Uiso 1 1 d DU . . C111 C 0.4901(7) 0.7053(5) 0.4719(5) 0.109(2) Uiso 1 1 d DU . . H11A H 0.5476 0.7566 0.5041 0.164 Uiso 1 1 calc R . . H11B H 0.4300 0.7134 0.4947 0.164 Uiso 1 1 calc R . . H11C H 0.4785 0.6934 0.4167 0.164 Uiso 1 1 calc R . . N12 N 0.2950(13) 0.2557(10) 0.3389(10) 0.108(4) Uiso 0.529(10) 1 d PDU A 1 C120 C 0.3708(14) 0.2574(11) 0.3170(10) 0.088(3) Uiso 0.529(10) 1 d PDU A 1 C121 C 0.4764(12) 0.2559(9) 0.2846(9) 0.088(3) Uiso 0.529(10) 1 d PDU A 1 H12A H 0.4929 0.2065 0.2780 0.132 Uiso 0.529(10) 1 calc PR A 1 H12B H 0.5304 0.3073 0.3235 0.132 Uiso 0.529(10) 1 calc PR A 1 H12C H 0.4693 0.2531 0.2329 0.132 Uiso 0.529(10) 1 calc PR A 1 N12A N 0.2129(13) 0.2397(9) 0.3197(9) 0.104(4) Uiso 0.471(10) 1 d PDU A 2 C220 C 0.2969(15) 0.2526(13) 0.3047(13) 0.089(3) Uiso 0.471(10) 1 d PDU A 2 C221 C 0.4139(13) 0.2628(12) 0.2951(12) 0.089(3) Uiso 0.471(10) 1 d PDU A 2 H22D H 0.4420 0.2364 0.3197 0.133 Uiso 0.471(10) 1 calc PR A 2 H22E H 0.4527 0.3228 0.3219 0.133 Uiso 0.471(10) 1 calc PR A 2 H22F H 0.4174 0.2354 0.2381 0.133 Uiso 0.471(10) 1 calc PR A 2 N13 N 0.7907(8) 0.5164(5) 0.3429(5) 0.082(3) Uiso 0.687(10) 1 d PD B 1 C130 C 0.7073(12) 0.4993(6) 0.3180(6) 0.060(2) Uiso 0.687(10) 1 d PDU B 1 C131 C 0.5959(9) 0.4833(7) 0.2801(7) 0.062(2) Uiso 0.687(10) 1 d PDU B 1 H13A H 0.5968 0.5217 0.2602 0.092 Uiso 0.687(10) 1 calc PR B 1 H13B H 0.5542 0.4935 0.3212 0.092 Uiso 0.687(10) 1 calc PR B 1 H13C H 0.5679 0.4248 0.2356 0.092 Uiso 0.687(10) 1 calc PR B 1 N13A N 0.465(3) 0.482(2) 0.269(2) 0.24(2) Uiso 0.313(10) 1 d PD B 2 C231 C 0.544(2) 0.4766(14) 0.2527(13) 0.062(2) Uiso 0.313(10) 1 d PDU B 2 C232 C 0.647(2) 0.4882(15) 0.3070(13) 0.061(2) Uiso 0.313(10) 1 d PDU B 2 H23D H 0.6936 0.4674 0.2722 0.092 Uiso 0.313(10) 1 calc PR B 2 H23E H 0.6285 0.4560 0.3340 0.092 Uiso 0.313(10) 1 calc PR B 2 H23F H 0.6783 0.5480 0.3473 0.092 Uiso 0.313(10) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.024(3) 0.015(2) 0.022(3) 0.011(2) 0.006(2) 0.003(2) C2 0.025(3) 0.013(2) 0.017(2) 0.008(2) 0.009(2) 0.003(2) C3 0.019(3) 0.022(2) 0.022(3) 0.013(2) 0.006(2) 0.005(2) C4 0.023(3) 0.019(2) 0.018(2) 0.010(2) 0.006(2) 0.005(2) C5 0.025(3) 0.023(2) 0.026(3) 0.013(2) 0.008(2) 0.008(2) C6 0.012(3) 0.023(2) 0.027(3) 0.016(2) 0.007(2) 0.006(2) C7 0.014(3) 0.022(2) 0.017(2) 0.011(2) 0.002(2) 0.003(2) C8 0.024(3) 0.014(2) 0.020(3) 0.009(2) 0.006(2) 0.001(2) C9 0.017(3) 0.018(2) 0.022(3) 0.012(2) 0.008(2) 0.003(2) C10 0.026(3) 0.019(2) 0.022(3) 0.010(2) 0.002(2) -0.001(2) C11 0.034(3) 0.025(2) 0.015(3) 0.012(2) 0.007(2) 0.013(2) C12 0.030(3) 0.034(3) 0.013(2) 0.012(2) 0.010(2) 0.011(2) C13 0.024(3) 0.025(3) 0.026(3) 0.011(2) 0.005(2) 0.008(2) C14 0.023(3) 0.030(3) 0.020(3) 0.012(2) 0.005(2) 0.012(2) C15 0.017(3) 0.019(2) 0.018(2) 0.010(2) 0.001(2) 0.004(2) C16 0.021(3) 0.017(2) 0.017(2) 0.007(2) 0.003(2) 0.005(2) C17 0.025(3) 0.021(2) 0.027(3) 0.013(2) 0.008(2) 0.012(2) C18 0.022(3) 0.016(2) 0.019(3) 0.010(2) 0.001(2) 0.002(2) C19 0.033(3) 0.019(2) 0.014(2) 0.010(2) 0.001(2) 0.006(2) C20 0.032(3) 0.016(2) 0.019(3) 0.010(2) 0.008(2) 0.005(2) C21 0.027(3) 0.043(3) 0.025(3) 0.014(3) 0.011(3) 0.017(3) C22 0.028(4) 0.048(3) 0.037(3) 0.020(3) 0.017(3) 0.018(3) C23 0.027(4) 0.076(4) 0.034(3) 0.018(3) 0.006(3) 0.019(3) C24 0.058(5) 0.059(4) 0.048(4) 0.032(3) 0.032(3) 0.039(3) C25 0.023(3) 0.032(3) 0.027(3) 0.020(2) 0.003(2) 0.006(2) C26 0.028(4) 0.128(6) 0.057(4) 0.067(4) 0.000(3) 0.011(4) C27 0.044(4) 0.051(3) 0.074(4) 0.045(3) -0.010(3) 0.009(3) C28 0.084(6) 0.046(4) 0.042(4) 0.007(3) -0.031(4) 0.017(4) C29 0.030(3) 0.018(2) 0.022(3) 0.011(2) 0.005(2) -0.001(2) C30 0.028(3) 0.024(2) 0.025(3) 0.016(2) 0.004(2) 0.005(2) C31 0.027(3) 0.021(2) 0.023(3) 0.013(2) 0.010(2) 0.005(2) C32 0.030(3) 0.018(2) 0.019(3) 0.011(2) 0.001(2) 0.001(2) C33 0.027(3) 0.017(2) 0.013(2) 0.007(2) 0.009(2) 0.002(2) C34 0.031(3) 0.013(2) 0.018(3) 0.007(2) 0.008(2) 0.006(2) C35 0.033(3) 0.021(2) 0.025(3) 0.013(2) -0.003(2) 0.002(2) C36 0.034(4) 0.014(2) 0.020(3) 0.007(2) 0.004(2) -0.001(2) C37 0.030(3) 0.017(2) 0.024(3) 0.013(2) 0.007(2) 0.011(2) C38 0.024(3) 0.016(2) 0.020(3) 0.009(2) 0.004(2) 0.004(2) C39 0.034(4) 0.026(3) 0.030(3) 0.022(2) -0.001(3) -0.001(2) C40 0.027(3) 0.041(3) 0.038(3) 0.029(3) 0.001(3) 0.002(2) C41 0.031(4) 0.049(3) 0.058(4) 0.043(3) 0.001(3) -0.001(3) C42 0.067(5) 0.040(3) 0.028(3) 0.020(3) -0.002(3) 0.010(3) C43 0.032(4) 0.020(2) 0.042(3) 0.019(3) -0.010(3) -0.005(2) C44 0.032(4) 0.026(3) 0.050(3) 0.025(3) 0.005(3) 0.003(2) C45 0.037(4) 0.017(3) 0.071(4) -0.003(3) -0.008(3) 0.003(3) C46 0.051(5) 0.051(4) 0.101(5) 0.064(4) -0.024(4) -0.018(3) C47 0.029(3) 0.020(2) 0.023(3) 0.013(2) 0.011(2) 0.007(2) C48 0.035(3) 0.013(2) 0.021(3) 0.007(2) 0.011(2) 0.009(2) C49 0.026(3) 0.017(2) 0.018(3) 0.009(2) 0.007(2) 0.005(2) C50 0.033(3) 0.020(2) 0.020(3) 0.011(2) 0.014(2) 0.007(2) C51 0.026(3) 0.014(2) 0.016(2) 0.009(2) 0.007(2) 0.005(2) C52 0.028(3) 0.019(2) 0.018(3) 0.010(2) 0.007(2) 0.006(2) C53 0.022(3) 0.020(2) 0.024(3) 0.013(2) 0.008(2) 0.004(2) C54 0.024(3) 0.023(2) 0.015(2) 0.009(2) 0.006(2) 0.006(2) C55 0.027(3) 0.015(2) 0.015(2) 0.004(2) 0.003(2) 0.006(2) C56 0.026(3) 0.017(2) 0.016(2) 0.010(2) 0.008(2) 0.005(2) C57 0.026(3) 0.016(2) 0.028(3) 0.009(2) 0.012(2) 0.002(2) C58 0.042(4) 0.016(2) 0.038(3) 0.010(2) 0.015(3) 0.001(2) C59 0.033(4) 0.025(3) 0.046(3) 0.024(3) 0.013(3) 0.004(2) C60 0.030(4) 0.020(2) 0.036(3) 0.012(2) 0.006(3) -0.001(2) C61 0.021(3) 0.025(2) 0.022(3) 0.005(2) 0.007(2) 0.002(2) C62 0.052(4) 0.040(3) 0.035(3) 0.022(3) 0.023(3) 0.012(3) C63 0.029(4) 0.037(3) 0.027(3) 0.002(2) 0.012(3) 0.011(3) C64 0.027(4) 0.042(3) 0.037(3) 0.005(3) 0.010(3) 0.013(3) Cl1 0.0269(8) 0.0196(5) 0.0177(6) 0.0100(5) 0.0040(5) 0.0055(5) Cl2 0.0276(8) 0.0174(5) 0.0258(7) 0.0107(5) 0.0055(6) 0.0035(5) Cl3 0.0305(8) 0.0175(5) 0.0227(6) 0.0120(5) 0.0073(5) 0.0030(5) Cl4 0.0342(8) 0.0271(6) 0.0212(6) 0.0101(5) 0.0121(6) 0.0089(6) Cl5 0.0292(8) 0.0188(5) 0.0218(6) 0.0113(5) 0.0113(6) 0.0079(5) Cl6 0.0302(8) 0.0312(6) 0.0273(7) 0.0202(6) 0.0074(6) 0.0085(6) N1 0.023(3) 0.0173(19) 0.017(2) 0.0071(17) 0.0051(18) 0.0032(17) N2 0.023(3) 0.0160(19) 0.019(2) 0.0119(17) 0.0052(18) 0.0063(17) N3 0.031(3) 0.0126(18) 0.014(2) 0.0074(16) 0.0050(18) 0.0026(17) N4 0.025(3) 0.0138(18) 0.013(2) 0.0065(17) 0.0031(18) 0.0066(17) N5 0.025(3) 0.0136(18) 0.015(2) 0.0083(16) 0.0095(18) 0.0042(17) N6 0.023(3) 0.0147(18) 0.014(2) 0.0073(17) 0.0064(18) 0.0046(17) O1 0.0135(19) 0.0182(15) 0.0164(16) 0.0083(13) 0.0034(14) 0.0036(13) O2 0.017(2) 0.0151(14) 0.0169(17) 0.0081(13) 0.0037(14) 0.0005(13) O3 0.0141(19) 0.0181(15) 0.0164(16) 0.0097(14) 0.0059(14) 0.0021(13) O4 0.018(2) 0.0159(15) 0.0131(16) 0.0049(13) 0.0029(14) 0.0021(13) O5 0.018(2) 0.0152(14) 0.0158(16) 0.0077(13) 0.0032(14) -0.0002(13) O6 0.019(2) 0.0163(15) 0.0195(17) 0.0109(14) 0.0054(15) 0.0035(14) V1 0.0201(5) 0.0138(4) 0.0168(4) 0.0089(3) 0.0061(4) 0.0034(3) V2 0.0227(5) 0.0160(4) 0.0155(4) 0.0084(3) 0.0053(4) 0.0055(3) V3 0.0243(5) 0.0157(4) 0.0164(4) 0.0094(3) 0.0065(4) 0.0030(3) V4 0.0249(5) 0.0154(4) 0.0180(4) 0.0101(3) 0.0092(4) 0.0056(3) O100 0.108(5) 0.042(2) 0.051(3) 0.027(2) -0.002(3) 0.002(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.427(5) . ? C1 C4 1.529(6) . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C2 O2 1.414(5) . ? C2 C4 1.543(6) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 O3 1.417(5) . ? C3 C4 1.548(6) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.533(6) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 O4 1.430(5) . ? C6 C9 1.545(6) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 O5 1.424(5) . ? C7 C9 1.545(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 O6 1.425(5) . ? C8 C9 1.543(6) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.535(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 N1 1.350(5) . ? C11 C12 1.361(6) . ? C11 H11 0.9500 . ? C12 C13 1.394(7) . ? C12 H12 0.9500 . ? C13 C14 1.393(6) . ? C13 C21 1.535(7) . ? C14 C15 1.380(6) . ? C14 H14 0.9500 . ? C15 N1 1.367(6) . ? C15 C16 1.477(6) . ? C16 N2 1.351(6) . ? C16 C17 1.373(6) . ? C17 C18 1.393(6) . ? C17 H17 0.9500 . ? C18 C19 1.388(6) . ? C18 C25 1.517(7) . ? C19 C20 1.383(7) . ? C19 H19 0.9500 . ? C20 N2 1.342(5) . ? C20 H20 0.9500 . ? C21 C22 1.526(7) . ? C21 C23 1.531(7) . ? C21 C24 1.540(7) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.519(7) . ? C25 C28 1.524(7) . ? C25 C26 1.531(7) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 N3 1.333(6) . ? C29 C30 1.389(7) . ? C29 H29 0.9500 . ? C30 C31 1.397(6) . ? C30 H30 0.9500 . ? C31 C32 1.403(6) . ? C31 C39 1.512(7) . ? C32 C33 1.368(7) . ? C32 H32 0.9500 . ? C33 N3 1.370(5) . ? C33 C34 1.490(6) . ? C34 N4 1.342(6) . ? C34 C35 1.408(6) . ? C35 C36 1.397(7) . ? C35 H35 0.9500 . ? C36 C37 1.394(7) . ? C36 C43 1.533(6) . ? C37 C38 1.373(6) . ? C37 H37 0.9500 . ? C38 N4 1.341(6) . ? C38 H38 0.9500 . ? C39 C42 1.520(6) . ? C39 C40 1.531(6) . ? C39 C41 1.551(7) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.521(7) . ? C43 C45 1.533(7) . ? C43 C46 1.543(7) . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 N5 1.331(5) . ? C47 C48 1.389(6) . ? C47 H47 0.9500 . ? C48 C49 1.385(6) . ? C48 H48 0.9500 . ? C49 C50 1.401(6) . ? C49 C57 1.528(6) . ? C50 C51 1.384(6) . ? C50 H50 0.9500 . ? C51 N5 1.359(5) . ? C51 C52 1.492(5) . ? C52 N6 1.356(5) . ? C52 C53 1.366(6) . ? C53 C54 1.404(6) . ? C53 H53 0.9500 . ? C54 C55 1.393(6) . ? C54 C61 1.524(6) . ? C55 C56 1.374(6) . ? C55 H55 0.9500 . ? C56 N6 1.341(5) . ? C56 H56 0.9500 . ? C57 C60 1.515(7) . ? C57 C58 1.543(6) . ? C57 C59 1.554(7) . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C63 1.512(6) . ? C61 C64 1.518(7) . ? C61 C62 1.548(7) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? Cl1 V2 2.3305(15) . ? Cl2 V2 2.3435(12) . ? Cl3 V3 2.3456(12) . ? Cl4 V3 2.3443(14) . ? Cl5 V4 2.3416(13) . ? Cl6 V4 2.3469(15) . ? N1 V2 2.129(4) . ? N2 V2 2.117(4) . ? N3 V3 2.131(4) . ? N4 V3 2.117(3) . ? N5 V4 2.137(3) . ? N6 V4 2.127(3) . ? O1 V1 1.971(3) . ? O1 V2 2.010(3) . ? O2 V1 1.951(3) . ? O2 V3 2.019(3) . ? O3 V1 1.955(3) . ? O3 V4 2.023(3) . ? O4 V2 1.977(3) . ? O4 V1 2.009(3) . ? O5 V3 1.979(3) . ? O5 V1 2.024(3) . ? O6 V4 1.981(3) . ? O6 V1 2.011(3) . ? V1 V4 3.0903(11) . ? V1 V2 3.0960(10) . ? V1 V3 3.1080(11) . ? O100 H100 1.044(15) . ? O100 H101 1.006(15) . ? N10 C100 1.120(10) . ? C100 C101 1.576(11) . ? C101 H10D 0.9800 . ? C101 H10E 0.9800 . ? C101 H10F 0.9800 . ? N11 C110 1.257(17) . ? C110 C111 1.577(11) . ? C111 H11A 0.9800 . ? C111 H11B 0.9800 . ? C111 H11C 0.9800 . ? N12 C120 1.159(14) . ? C120 C121 1.633(14) . ? C121 H12A 0.9800 . ? C121 H12B 0.9800 . ? C121 H12C 0.9800 . ? N12A C220 1.217(15) . ? C220 C221 1.630(14) . ? C221 H22D 0.9800 . ? C221 H22E 0.9800 . ? C221 H22F 0.9800 . ? N13 C130 1.147(12) . ? C130 C131 1.587(11) . ? C131 H13A 0.9800 . ? C131 H13B 0.9800 . ? C131 H13C 0.9800 . ? N13A C231 1.180(17) . ? C231 C232 1.644(15) . ? C232 H23D 0.9800 . ? C232 H23E 0.9800 . ? C232 H23F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C4 113.3(3) . . ? O1 C1 H1A 108.9 . . ? C4 C1 H1A 108.9 . . ? O1 C1 H1B 108.9 . . ? C4 C1 H1B 108.9 . . ? H1A C1 H1B 107.7 . . ? O2 C2 C4 113.9(3) . . ? O2 C2 H2A 108.8 . . ? C4 C2 H2A 108.8 . . ? O2 C2 H2B 108.8 . . ? C4 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? O3 C3 C4 113.6(4) . . ? O3 C3 H3A 108.8 . . ? C4 C3 H3A 108.8 . . ? O3 C3 H3B 108.8 . . ? C4 C3 H3B 108.8 . . ? H3A C3 H3B 107.7 . . ? C1 C4 C5 107.3(4) . . ? C1 C4 C2 111.6(4) . . ? C5 C4 C2 107.9(3) . . ? C1 C4 C3 111.2(3) . . ? C5 C4 C3 107.1(4) . . ? C2 C4 C3 111.5(3) . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O4 C6 C9 113.1(3) . . ? O4 C6 H6A 109.0 . . ? C9 C6 H6A 109.0 . . ? O4 C6 H6B 109.0 . . ? C9 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? O5 C7 C9 114.0(4) . . ? O5 C7 H7A 108.7 . . ? C9 C7 H7A 108.7 . . ? O5 C7 H7B 108.7 . . ? C9 C7 H7B 108.7 . . ? H7A C7 H7B 107.6 . . ? O6 C8 C9 114.0(3) . . ? O6 C8 H8A 108.7 . . ? C9 C8 H8A 108.7 . . ? O6 C8 H8B 108.7 . . ? C9 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C10 C9 C8 107.7(4) . . ? C10 C9 C6 106.7(3) . . ? C8 C9 C6 111.9(4) . . ? C10 C9 C7 106.5(4) . . ? C8 C9 C7 111.6(4) . . ? C6 C9 C7 112.2(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C12 123.3(5) . . ? N1 C11 H11 118.4 . . ? C12 C11 H11 118.4 . . ? C11 C12 C13 120.8(5) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C14 C13 C12 116.2(4) . . ? C14 C13 C21 119.8(5) . . ? C12 C13 C21 124.0(4) . . ? C15 C14 C13 120.8(5) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? N1 C15 C14 121.9(4) . . ? N1 C15 C16 114.7(4) . . ? C14 C15 C16 123.4(5) . . ? N2 C16 C17 121.4(4) . . ? N2 C16 C15 114.8(4) . . ? C17 C16 C15 123.8(4) . . ? C16 C17 C18 121.1(5) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C19 C18 C17 116.2(5) . . ? C19 C18 C25 121.2(4) . . ? C17 C18 C25 122.6(4) . . ? C20 C19 C18 120.7(4) . . ? C20 C19 H19 119.7 . . ? C18 C19 H19 119.7 . . ? N2 C20 C19 121.7(5) . . ? N2 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C22 C21 C23 108.8(4) . . ? C22 C21 C13 112.2(5) . . ? C23 C21 C13 109.0(4) . . ? C22 C21 C24 108.9(4) . . ? C23 C21 C24 110.4(5) . . ? C13 C21 C24 107.5(4) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C21 C23 H23A 109.5 . . ? C21 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C21 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C18 C25 C27 109.2(4) . . ? C18 C25 C28 109.3(4) . . ? C27 C25 C28 109.5(4) . . ? C18 C25 C26 112.1(4) . . ? C27 C25 C26 108.8(5) . . ? C28 C25 C26 107.9(5) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N3 C29 C30 123.9(4) . . ? N3 C29 H29 118.1 . . ? C30 C29 H29 118.1 . . ? C29 C30 C31 119.8(5) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? C30 C31 C32 116.0(5) . . ? C30 C31 C39 124.1(4) . . ? C32 C31 C39 119.8(4) . . ? C33 C32 C31 121.1(4) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C32 C33 N3 122.5(4) . . ? C32 C33 C34 124.4(4) . . ? N3 C33 C34 113.1(4) . . ? N4 C34 C35 121.6(4) . . ? N4 C34 C33 115.3(4) . . ? C35 C34 C33 123.1(5) . . ? C36 C35 C34 120.3(5) . . ? C36 C35 H35 119.9 . . ? C34 C35 H35 119.9 . . ? C37 C36 C35 116.1(4) . . ? C37 C36 C43 122.6(4) . . ? C35 C36 C43 121.2(5) . . ? C38 C37 C36 120.7(4) . . ? C38 C37 H37 119.6 . . ? C36 C37 H37 119.6 . . ? N4 C38 C37 123.0(5) . . ? N4 C38 H38 118.5 . . ? C37 C38 H38 118.5 . . ? C31 C39 C42 109.8(4) . . ? C31 C39 C40 112.3(4) . . ? C42 C39 C40 108.0(4) . . ? C31 C39 C41 108.7(4) . . ? C42 C39 C41 110.2(4) . . ? C40 C39 C41 107.8(4) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C39 C42 H42A 109.5 . . ? C39 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C39 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C44 C43 C36 111.0(4) . . ? C44 C43 C45 110.5(4) . . ? C36 C43 C45 107.3(4) . . ? C44 C43 C46 108.4(5) . . ? C36 C43 C46 110.0(4) . . ? C45 C43 C46 109.7(5) . . ? C43 C44 H44A 109.5 . . ? C43 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C43 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C43 C45 H45A 109.5 . . ? C43 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C43 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C43 C46 H46A 109.5 . . ? C43 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C43 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N5 C47 C48 123.3(4) . . ? N5 C47 H47 118.3 . . ? C48 C47 H47 118.3 . . ? C49 C48 C47 120.1(4) . . ? C49 C48 H48 120.0 . . ? C47 C48 H48 120.0 . . ? C48 C49 C50 116.7(4) . . ? C48 C49 C57 123.4(4) . . ? C50 C49 C57 119.9(4) . . ? C51 C50 C49 120.2(4) . . ? C51 C50 H50 119.9 . . ? C49 C50 H50 119.9 . . ? N5 C51 C50 122.3(4) . . ? N5 C51 C52 114.7(3) . . ? C50 C51 C52 123.0(4) . . ? N6 C52 C53 120.9(4) . . ? N6 C52 C51 114.8(4) . . ? C53 C52 C51 124.3(4) . . ? C52 C53 C54 121.6(4) . . ? C52 C53 H53 119.2 . . ? C54 C53 H53 119.2 . . ? C55 C54 C53 115.7(4) . . ? C55 C54 C61 123.9(4) . . ? C53 C54 C61 120.3(4) . . ? C56 C55 C54 120.7(4) . . ? C56 C55 H55 119.7 . . ? C54 C55 H55 119.7 . . ? N6 C56 C55 122.1(4) . . ? N6 C56 H56 118.9 . . ? C55 C56 H56 118.9 . . ? C60 C57 C49 110.8(4) . . ? C60 C57 C58 109.1(4) . . ? C49 C57 C58 111.7(4) . . ? C60 C57 C59 110.8(4) . . ? C49 C57 C59 106.8(4) . . ? C58 C57 C59 107.7(4) . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C57 C60 H60A 109.5 . . ? C57 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C57 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C63 C61 C64 110.8(4) . . ? C63 C61 C54 112.5(4) . . ? C64 C61 C54 108.5(4) . . ? C63 C61 C62 108.0(4) . . ? C64 C61 C62 108.1(4) . . ? C54 C61 C62 108.8(4) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C11 N1 C15 116.9(4) . . ? C11 N1 V2 126.7(3) . . ? C15 N1 V2 116.3(3) . . ? C20 N2 C16 118.6(4) . . ? C20 N2 V2 124.0(3) . . ? C16 N2 V2 117.0(3) . . ? C29 N3 C33 116.7(4) . . ? C29 N3 V3 125.8(3) . . ? C33 N3 V3 117.5(3) . . ? C38 N4 C34 118.1(4) . . ? C38 N4 V3 124.1(3) . . ? C34 N4 V3 117.4(3) . . ? C47 N5 C51 117.4(3) . . ? C47 N5 V4 125.7(3) . . ? C51 N5 V4 116.9(3) . . ? C56 N6 C52 118.9(4) . . ? C56 N6 V4 123.8(3) . . ? C52 N6 V4 117.2(3) . . ? C1 O1 V1 117.4(2) . . ? C1 O1 V2 129.5(2) . . ? V1 O1 V2 102.09(13) . . ? C2 O2 V1 117.5(2) . . ? C2 O2 V3 129.2(2) . . ? V1 O2 V3 103.02(15) . . ? C3 O3 V1 117.5(3) . . ? C3 O3 V4 129.3(3) . . ? V1 O3 V4 101.94(13) . . ? C6 O4 V2 133.8(3) . . ? C6 O4 V1 118.4(2) . . ? V2 O4 V1 101.89(13) . . ? C7 O5 V3 133.9(2) . . ? C7 O5 V1 117.5(2) . . ? V3 O5 V1 101.88(14) . . ? C8 O6 V4 134.1(3) . . ? C8 O6 V1 117.8(2) . . ? V4 O6 V1 101.45(14) . . ? O2 V1 O3 92.13(13) . . ? O2 V1 O1 91.72(11) . . ? O3 V1 O1 91.83(12) . . ? O2 V1 O4 162.20(13) . . ? O3 V1 O4 102.52(12) . . ? O1 V1 O4 77.93(11) . . ? O2 V1 O6 102.08(11) . . ? O3 V1 O6 78.56(12) . . ? O1 V1 O6 163.36(12) . . ? O4 V1 O6 90.81(11) . . ? O2 V1 O5 77.73(12) . . ? O3 V1 O5 162.86(11) . . ? O1 V1 O5 102.15(12) . . ? O4 V1 O5 90.20(12) . . ? O6 V1 O5 89.96(12) . . ? O2 V1 V4 96.33(9) . . ? O3 V1 V4 39.82(8) . . ? O1 V1 V4 131.03(10) . . ? O4 V1 V4 101.40(9) . . ? O6 V1 V4 38.92(9) . . ? O5 V1 V4 126.78(8) . . ? O2 V1 V2 130.34(8) . . ? O3 V1 V2 96.61(8) . . ? O1 V1 V2 39.41(8) . . ? O4 V1 V2 38.68(8) . . ? O6 V1 V2 127.58(8) . . ? O5 V1 V2 100.49(8) . . ? V4 V1 V2 120.74(3) . . ? O2 V1 V3 39.28(10) . . ? O3 V1 V3 130.53(9) . . ? O1 V1 V3 97.09(8) . . ? O4 V1 V3 126.94(10) . . ? O6 V1 V3 99.48(8) . . ? O5 V1 V3 38.53(8) . . ? V4 V1 V3 118.92(3) . . ? V2 V1 V3 120.34(3) . . ? O4 V2 O1 77.78(11) . . ? O4 V2 N2 85.23(13) . . ? O1 V2 N2 96.55(13) . . ? O4 V2 N1 93.86(13) . . ? O1 V2 N1 169.53(14) . . ? N2 V2 N1 76.26(15) . . ? O4 V2 Cl1 95.61(10) . . ? O1 V2 Cl1 93.48(10) . . ? N2 V2 Cl1 169.87(11) . . ? N1 V2 Cl1 93.61(11) . . ? O4 V2 Cl2 167.07(9) . . ? O1 V2 Cl2 94.45(9) . . ? N2 V2 Cl2 85.43(10) . . ? N1 V2 Cl2 92.58(10) . . ? Cl1 V2 Cl2 95.16(5) . . ? O4 V2 V1 39.43(8) . . ? O1 V2 V1 38.51(8) . . ? N2 V2 V1 93.85(9) . . ? N1 V2 V1 133.25(10) . . ? Cl1 V2 V1 93.16(4) . . ? Cl2 V2 V1 132.67(4) . . ? O5 V3 O2 77.21(12) . . ? O5 V3 N4 84.71(12) . . ? O2 V3 N4 99.27(13) . . ? O5 V3 N3 95.13(14) . . ? O2 V3 N3 171.29(13) . . ? N4 V3 N3 75.62(14) . . ? O5 V3 Cl4 164.31(10) . . ? O2 V3 Cl4 92.87(9) . . ? N4 V3 Cl4 84.95(10) . . ? N3 V3 Cl4 93.69(10) . . ? O5 V3 Cl3 98.16(8) . . ? O2 V3 Cl3 91.43(8) . . ? N4 V3 Cl3 169.28(12) . . ? N3 V3 Cl3 93.80(10) . . ? Cl4 V3 Cl3 94.17(5) . . ? O5 V3 V1 39.59(9) . . ? O2 V3 V1 37.70(8) . . ? N4 V3 V1 94.53(10) . . ? N3 V3 V1 134.70(10) . . ? Cl4 V3 V1 129.97(5) . . ? Cl3 V3 V1 94.20(4) . . ? O6 V4 O3 77.69(12) . . ? O6 V4 N6 85.47(13) . . ? O3 V4 N6 98.75(12) . . ? O6 V4 N5 94.33(14) . . ? O3 V4 N5 170.94(15) . . ? N6 V4 N5 76.10(13) . . ? O6 V4 Cl5 98.24(9) . . ? O3 V4 Cl5 91.84(8) . . ? N6 V4 Cl5 169.32(10) . . ? N5 V4 Cl5 93.58(10) . . ? O6 V4 Cl6 164.89(9) . . ? O3 V4 Cl6 92.49(10) . . ? N6 V4 Cl6 84.72(11) . . ? N5 V4 Cl6 94.42(11) . . ? Cl5 V4 Cl6 93.47(5) . . ? O6 V4 V1 39.64(8) . . ? O3 V4 V1 38.23(9) . . ? N6 V4 V1 95.65(10) . . ? N5 V4 V1 133.97(11) . . ? Cl5 V4 V1 93.54(4) . . ? Cl6 V4 V1 130.38(4) . . ? H100 O100 H101 109(3) . . ? N10 C100 C101 176.1(14) . . ? C100 C101 H10D 109.5 . . ? C100 C101 H10E 109.5 . . ? H10D C101 H10E 109.5 . . ? C100 C101 H10F 109.5 . . ? H10D C101 H10F 109.5 . . ? H10E C101 H10F 109.5 . . ? N11 C110 C111 125(2) . . ? C110 C111 H11A 109.5 . . ? C110 C111 H11B 109.5 . . ? H11A C111 H11B 109.5 . . ? C110 C111 H11C 109.5 . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? N12 C120 C121 177.8(17) . . ? C120 C121 H12A 109.5 . . ? C120 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? C120 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? N12A C220 C221 169(2) . . ? C220 C221 H22D 109.5 . . ? C220 C221 H22E 109.5 . . ? H22D C221 H22E 109.5 . . ? C220 C221 H22F 109.5 . . ? H22D C221 H22F 109.5 . . ? H22E C221 H22F 109.5 . . ? N13 C130 C131 173.3(11) . . ? C130 C131 H13A 109.5 . . ? C130 C131 H13B 109.5 . . ? H13A C131 H13B 109.5 . . ? C130 C131 H13C 109.5 . . ? H13A C131 H13C 109.5 . . ? H13B C131 H13C 109.5 . . ? N13A C231 C232 130(2) . . ? C231 C232 H23D 109.5 . . ? C231 C232 H23E 109.5 . . ? H23D C232 H23E 109.5 . . ? C231 C232 H23F 109.5 . . ? H23D C232 H23F 109.5 . . ? H23E C232 H23F 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C4 C5 -176.2(4) . . . . ? O1 C1 C4 C2 65.9(5) . . . . ? O1 C1 C4 C3 -59.3(5) . . . . ? O2 C2 C4 C1 -59.4(5) . . . . ? O2 C2 C4 C5 -177.0(3) . . . . ? O2 C2 C4 C3 65.7(5) . . . . ? O3 C3 C4 C1 67.6(5) . . . . ? O3 C3 C4 C5 -175.5(3) . . . . ? O3 C3 C4 C2 -57.7(5) . . . . ? O6 C8 C9 C10 -176.3(3) . . . . ? O6 C8 C9 C6 -59.4(5) . . . . ? O6 C8 C9 C7 67.2(5) . . . . ? O4 C6 C9 C10 -174.4(4) . . . . ? O4 C6 C9 C8 68.1(5) . . . . ? O4 C6 C9 C7 -58.2(5) . . . . ? O5 C7 C9 C10 -175.7(3) . . . . ? O5 C7 C9 C8 -58.5(5) . . . . ? O5 C7 C9 C6 67.9(5) . . . . ? N1 C11 C12 C13 -0.3(7) . . . . ? C11 C12 C13 C14 -0.3(7) . . . . ? C11 C12 C13 C21 -178.6(4) . . . . ? C12 C13 C14 C15 1.6(7) . . . . ? C21 C13 C14 C15 180.0(4) . . . . ? C13 C14 C15 N1 -2.4(7) . . . . ? C13 C14 C15 C16 178.3(4) . . . . ? N1 C15 C16 N2 -9.2(5) . . . . ? C14 C15 C16 N2 170.1(4) . . . . ? N1 C15 C16 C17 168.9(4) . . . . ? C14 C15 C16 C17 -11.8(7) . . . . ? N2 C16 C17 C18 -1.6(7) . . . . ? C15 C16 C17 C18 -179.5(4) . . . . ? C16 C17 C18 C19 -4.2(6) . . . . ? C16 C17 C18 C25 175.6(4) . . . . ? C17 C18 C19 C20 5.6(6) . . . . ? C25 C18 C19 C20 -174.2(4) . . . . ? C18 C19 C20 N2 -1.2(6) . . . . ? C14 C13 C21 C22 171.3(4) . . . . ? C12 C13 C21 C22 -10.4(7) . . . . ? C14 C13 C21 C23 50.7(6) . . . . ? C12 C13 C21 C23 -131.0(5) . . . . ? C14 C13 C21 C24 -69.0(6) . . . . ? C12 C13 C21 C24 109.3(5) . . . . ? C19 C18 C25 C27 -70.5(5) . . . . ? C17 C18 C25 C27 109.7(5) . . . . ? C19 C18 C25 C28 49.3(6) . . . . ? C17 C18 C25 C28 -130.5(5) . . . . ? C19 C18 C25 C26 168.9(4) . . . . ? C17 C18 C25 C26 -10.9(6) . . . . ? N3 C29 C30 C31 2.2(7) . . . . ? C29 C30 C31 C32 -1.7(7) . . . . ? C29 C30 C31 C39 -179.5(4) . . . . ? C30 C31 C32 C33 0.5(7) . . . . ? C39 C31 C32 C33 178.5(4) . . . . ? C31 C32 C33 N3 0.3(7) . . . . ? C31 C32 C33 C34 -176.9(4) . . . . ? C32 C33 C34 N4 171.7(4) . . . . ? N3 C33 C34 N4 -5.8(5) . . . . ? C32 C33 C34 C35 -8.8(7) . . . . ? N3 C33 C34 C35 173.7(4) . . . . ? N4 C34 C35 C36 -1.7(7) . . . . ? C33 C34 C35 C36 178.8(4) . . . . ? C34 C35 C36 C37 -2.5(7) . . . . ? C34 C35 C36 C43 178.9(4) . . . . ? C35 C36 C37 C38 3.7(6) . . . . ? C43 C36 C37 C38 -177.7(4) . . . . ? C36 C37 C38 N4 -0.8(7) . . . . ? C30 C31 C39 C42 115.3(5) . . . . ? C32 C31 C39 C42 -62.4(6) . . . . ? C30 C31 C39 C40 -4.9(7) . . . . ? C32 C31 C39 C40 177.3(4) . . . . ? C30 C31 C39 C41 -124.1(5) . . . . ? C32 C31 C39 C41 58.2(6) . . . . ? C37 C36 C43 C44 145.3(5) . . . . ? C35 C36 C43 C44 -36.3(6) . . . . ? C37 C36 C43 C45 -93.9(5) . . . . ? C35 C36 C43 C45 84.6(6) . . . . ? C37 C36 C43 C46 25.4(7) . . . . ? C35 C36 C43 C46 -156.2(5) . . . . ? N5 C47 C48 C49 0.6(8) . . . . ? C47 C48 C49 C50 -0.6(7) . . . . ? C47 C48 C49 C57 -179.0(5) . . . . ? C48 C49 C50 C51 0.0(7) . . . . ? C57 C49 C50 C51 178.4(5) . . . . ? C49 C50 C51 N5 0.7(8) . . . . ? C49 C50 C51 C52 -179.1(5) . . . . ? N5 C51 C52 N6 -2.2(6) . . . . ? C50 C51 C52 N6 177.6(5) . . . . ? N5 C51 C52 C53 178.1(5) . . . . ? C50 C51 C52 C53 -2.1(8) . . . . ? N6 C52 C53 C54 0.2(8) . . . . ? C51 C52 C53 C54 179.9(5) . . . . ? C52 C53 C54 C55 -2.2(7) . . . . ? C52 C53 C54 C61 175.6(5) . . . . ? C53 C54 C55 C56 2.3(7) . . . . ? C61 C54 C55 C56 -175.5(5) . . . . ? C54 C55 C56 N6 -0.4(7) . . . . ? C48 C49 C57 C60 -133.8(5) . . . . ? C50 C49 C57 C60 48.0(6) . . . . ? C48 C49 C57 C58 -12.0(7) . . . . ? C50 C49 C57 C58 169.8(5) . . . . ? C48 C49 C57 C59 105.5(5) . . . . ? C50 C49 C57 C59 -72.8(6) . . . . ? C55 C54 C61 C63 -2.4(7) . . . . ? C53 C54 C61 C63 179.9(5) . . . . ? C55 C54 C61 C64 120.5(5) . . . . ? C53 C54 C61 C64 -57.2(6) . . . . ? C55 C54 C61 C62 -122.0(5) . . . . ? C53 C54 C61 C62 60.3(6) . . . . ? C12 C11 N1 C15 -0.4(6) . . . . ? C12 C11 N1 V2 177.5(3) . . . . ? C14 C15 N1 C11 1.8(6) . . . . ? C16 C15 N1 C11 -178.9(4) . . . . ? C14 C15 N1 V2 -176.3(3) . . . . ? C16 C15 N1 V2 3.0(5) . . . . ? C19 C20 N2 C16 -4.7(6) . . . . ? C19 C20 N2 V2 167.9(3) . . . . ? C17 C16 N2 C20 6.1(6) . . . . ? C15 C16 N2 C20 -175.8(3) . . . . ? C17 C16 N2 V2 -167.0(3) . . . . ? C15 C16 N2 V2 11.1(5) . . . . ? C30 C29 N3 C33 -1.3(7) . . . . ? C30 C29 N3 V3 178.4(3) . . . . ? C32 C33 N3 C29 0.1(6) . . . . ? C34 C33 N3 C29 177.6(4) . . . . ? C32 C33 N3 V3 -179.7(3) . . . . ? C34 C33 N3 V3 -2.2(5) . . . . ? C37 C38 N4 C34 -3.5(6) . . . . ? C37 C38 N4 V3 169.0(3) . . . . ? C35 C34 N4 C38 4.7(6) . . . . ? C33 C34 N4 C38 -175.8(4) . . . . ? C35 C34 N4 V3 -168.3(3) . . . . ? C33 C34 N4 V3 11.2(5) . . . . ? C48 C47 N5 C51 0.1(7) . . . . ? C48 C47 N5 V4 -177.9(4) . . . . ? C50 C51 N5 C47 -0.7(7) . . . . ? C52 C51 N5 C47 179.1(4) . . . . ? C50 C51 N5 V4 177.5(4) . . . . ? C52 C51 N5 V4 -2.7(5) . . . . ? C55 C56 N6 C52 -1.7(7) . . . . ? C55 C56 N6 V4 174.0(4) . . . . ? C53 C52 N6 C56 1.8(7) . . . . ? C51 C52 N6 C56 -177.9(4) . . . . ? C53 C52 N6 V4 -174.2(4) . . . . ? C51 C52 N6 V4 6.1(5) . . . . ? C4 C1 O1 V1 -5.7(5) . . . . ? C4 C1 O1 V2 131.4(3) . . . . ? C4 C2 O2 V1 -6.0(4) . . . . ? C4 C2 O2 V3 132.8(3) . . . . ? C4 C3 O3 V1 -6.8(4) . . . . ? C4 C3 O3 V4 130.0(3) . . . . ? C9 C6 O4 V2 139.3(3) . . . . ? C9 C6 O4 V1 -8.2(5) . . . . ? C9 C7 O5 V3 137.9(3) . . . . ? C9 C7 O5 V1 -7.5(4) . . . . ? C9 C8 O6 V4 139.0(3) . . . . ? C9 C8 O6 V1 -6.4(4) . . . . ? C2 O2 V1 O3 -42.6(3) . . . . ? V3 O2 V1 O3 168.99(12) . . . . ? C2 O2 V1 O1 49.3(3) . . . . ? V3 O2 V1 O1 -99.11(13) . . . . ? C2 O2 V1 O4 103.1(5) . . . . ? V3 O2 V1 O4 -45.3(4) . . . . ? C2 O2 V1 O6 -121.4(3) . . . . ? V3 O2 V1 O6 90.24(14) . . . . ? C2 O2 V1 O5 151.3(3) . . . . ? V3 O2 V1 O5 2.95(11) . . . . ? C2 O2 V1 V4 -82.3(3) . . . . ? V3 O2 V1 V4 129.27(9) . . . . ? C2 O2 V1 V2 57.9(3) . . . . ? V3 O2 V1 V2 -90.48(13) . . . . ? C2 O2 V1 V3 148.4(3) . . . . ? C3 O3 V1 O2 49.9(3) . . . . ? V4 O3 V1 O2 -97.33(12) . . . . ? C3 O3 V1 O1 -41.9(3) . . . . ? V4 O3 V1 O1 170.88(12) . . . . ? C3 O3 V1 O4 -119.9(3) . . . . ? V4 O3 V1 O4 92.85(12) . . . . ? C3 O3 V1 O6 151.8(3) . . . . ? V4 O3 V1 O6 4.57(12) . . . . ? C3 O3 V1 O5 103.0(5) . . . . ? V4 O3 V1 O5 -44.2(5) . . . . ? C3 O3 V1 V4 147.2(3) . . . . ? C3 O3 V1 V2 -81.1(3) . . . . ? V4 O3 V1 V2 131.65(9) . . . . ? C3 O3 V1 V3 59.1(3) . . . . ? V4 O3 V1 V3 -88.18(13) . . . . ? C1 O1 V1 O2 -42.9(3) . . . . ? V2 O1 V1 O2 169.61(14) . . . . ? C1 O1 V1 O3 49.3(3) . . . . ? V2 O1 V1 O3 -98.20(14) . . . . ? C1 O1 V1 O4 151.7(3) . . . . ? V2 O1 V1 O4 4.22(13) . . . . ? C1 O1 V1 O6 103.4(5) . . . . ? V2 O1 V1 O6 -44.1(5) . . . . ? C1 O1 V1 O5 -120.7(3) . . . . ? V2 O1 V1 O5 91.79(14) . . . . ? C1 O1 V1 V4 57.0(3) . . . . ? V2 O1 V1 V4 -90.47(15) . . . . ? C1 O1 V1 V2 147.5(3) . . . . ? C1 O1 V1 V3 -81.9(3) . . . . ? V2 O1 V1 V3 130.57(11) . . . . ? C6 O4 V1 O2 96.8(5) . . . . ? V2 O4 V1 O2 -59.8(4) . . . . ? C6 O4 V1 O3 -118.4(3) . . . . ? V2 O4 V1 O3 84.91(14) . . . . ? C6 O4 V1 O1 152.4(3) . . . . ? V2 O4 V1 O1 -4.29(13) . . . . ? C6 O4 V1 O6 -40.0(3) . . . . ? V2 O4 V1 O6 163.36(14) . . . . ? C6 O4 V1 O5 50.0(3) . . . . ? V2 O4 V1 O5 -106.67(13) . . . . ? C6 O4 V1 V4 -77.7(3) . . . . ? V2 O4 V1 V4 125.64(10) . . . . ? C6 O4 V1 V2 156.7(4) . . . . ? C6 O4 V1 V3 62.6(3) . . . . ? V2 O4 V1 V3 -94.12(13) . . . . ? C8 O6 V1 O2 -119.5(3) . . . . ? V4 O6 V1 O2 85.08(14) . . . . ? C8 O6 V1 O3 150.8(3) . . . . ? V4 O6 V1 O3 -4.66(12) . . . . ? C8 O6 V1 O1 95.1(5) . . . . ? V4 O6 V1 O1 -60.4(5) . . . . ? C8 O6 V1 O4 48.2(3) . . . . ? V4 O6 V1 O4 -107.28(13) . . . . ? C8 O6 V1 O5 -42.0(3) . . . . ? V4 O6 V1 O5 162.52(13) . . . . ? C8 O6 V1 V4 155.4(3) . . . . ? C8 O6 V1 V2 61.2(3) . . . . ? V4 O6 V1 V2 -94.23(13) . . . . ? C8 O6 V1 V3 -79.6(3) . . . . ? V4 O6 V1 V3 125.01(9) . . . . ? C7 O5 V1 O2 152.3(3) . . . . ? V3 O5 V1 O2 -2.99(11) . . . . ? C7 O5 V1 O3 97.5(5) . . . . ? V3 O5 V1 O3 -57.8(4) . . . . ? C7 O5 V1 O1 -118.6(3) . . . . ? V3 O5 V1 O1 86.12(13) . . . . ? C7 O5 V1 O4 -40.9(3) . . . . ? V3 O5 V1 O4 163.82(12) . . . . ? C7 O5 V1 O6 49.9(3) . . . . ? V3 O5 V1 O6 -105.37(12) . . . . ? C7 O5 V1 V4 63.6(3) . . . . ? V3 O5 V1 V4 -91.75(12) . . . . ? C7 O5 V1 V2 -78.4(3) . . . . ? V3 O5 V1 V2 126.31(9) . . . . ? C7 O5 V1 V3 155.3(3) . . . . ? C6 O4 V2 O1 -146.9(4) . . . . ? V1 O4 V2 O1 4.21(13) . . . . ? C6 O4 V2 N2 -49.1(4) . . . . ? V1 O4 V2 N2 101.98(15) . . . . ? C6 O4 V2 N1 26.7(4) . . . . ? V1 O4 V2 N1 177.82(15) . . . . ? C6 O4 V2 Cl1 120.7(3) . . . . ? V1 O4 V2 Cl1 -88.16(12) . . . . ? C6 O4 V2 Cl2 -93.0(5) . . . . ? V1 O4 V2 Cl2 58.1(5) . . . . ? C6 O4 V2 V1 -151.1(4) . . . . ? C1 O1 V2 O4 -146.1(3) . . . . ? V1 O1 V2 O4 -4.29(14) . . . . ? C1 O1 V2 N2 130.2(3) . . . . ? V1 O1 V2 N2 -87.95(15) . . . . ? C1 O1 V2 N1 176.3(7) . . . . ? V1 O1 V2 N1 -41.9(8) . . . . ? C1 O1 V2 Cl1 -51.1(3) . . . . ? V1 O1 V2 Cl1 90.70(12) . . . . ? C1 O1 V2 Cl2 44.3(3) . . . . ? V1 O1 V2 Cl2 -173.84(11) . . . . ? C1 O1 V2 V1 -141.8(4) . . . . ? C20 N2 V2 O4 -84.8(3) . . . . ? C16 N2 V2 O4 87.8(3) . . . . ? C20 N2 V2 O1 -7.8(3) . . . . ? C16 N2 V2 O1 164.9(3) . . . . ? C20 N2 V2 N1 180.0(3) . . . . ? C16 N2 V2 N1 -7.3(3) . . . . ? C20 N2 V2 Cl1 180.0(4) . . . . ? C16 N2 V2 Cl1 -7.3(8) . . . . ? C20 N2 V2 Cl2 86.2(3) . . . . ? C16 N2 V2 Cl2 -101.1(3) . . . . ? C20 N2 V2 V1 -46.3(3) . . . . ? C16 N2 V2 V1 126.4(3) . . . . ? C11 N1 V2 O4 100.0(4) . . . . ? C15 N1 V2 O4 -82.1(3) . . . . ? C11 N1 V2 O1 136.7(7) . . . . ? C15 N1 V2 O1 -45.4(9) . . . . ? C11 N1 V2 N2 -175.9(4) . . . . ? C15 N1 V2 N2 2.0(3) . . . . ? C11 N1 V2 Cl1 4.1(3) . . . . ? C15 N1 V2 Cl1 -178.0(3) . . . . ? C11 N1 V2 Cl2 -91.2(3) . . . . ? C15 N1 V2 Cl2 86.7(3) . . . . ? C11 N1 V2 V1 101.9(3) . . . . ? C15 N1 V2 V1 -80.2(3) . . . . ? O2 V1 V2 O4 159.7(2) . . . . ? O3 V1 V2 O4 -101.80(17) . . . . ? O1 V1 V2 O4 173.4(2) . . . . ? O6 V1 V2 O4 -21.17(18) . . . . ? O5 V1 V2 O4 76.97(16) . . . . ? V4 V1 V2 O4 -67.97(14) . . . . ? V3 V1 V2 O4 112.53(15) . . . . ? O2 V1 V2 O1 -13.68(19) . . . . ? O3 V1 V2 O1 84.81(17) . . . . ? O4 V1 V2 O1 -173.4(2) . . . . ? O6 V1 V2 O1 165.44(19) . . . . ? O5 V1 V2 O1 -96.42(17) . . . . ? V4 V1 V2 O1 118.64(15) . . . . ? V3 V1 V2 O1 -60.86(15) . . . . ? O2 V1 V2 N2 82.01(16) . . . . ? O3 V1 V2 N2 -179.50(13) . . . . ? O1 V1 V2 N2 95.69(17) . . . . ? O4 V1 V2 N2 -77.70(17) . . . . ? O6 V1 V2 N2 -98.87(16) . . . . ? O5 V1 V2 N2 -0.73(13) . . . . ? V4 V1 V2 N2 -145.67(10) . . . . ? V3 V1 V2 N2 34.84(11) . . . . ? O2 V1 V2 N1 156.7(2) . . . . ? O3 V1 V2 N1 -104.79(18) . . . . ? O1 V1 V2 N1 170.4(2) . . . . ? O4 V1 V2 N1 -3.0(2) . . . . ? O6 V1 V2 N1 -24.2(2) . . . . ? O5 V1 V2 N1 73.99(18) . . . . ? V4 V1 V2 N1 -70.95(16) . . . . ? V3 V1 V2 N1 109.55(16) . . . . ? O2 V1 V2 Cl1 -105.30(13) . . . . ? O3 V1 V2 Cl1 -6.82(9) . . . . ? O1 V1 V2 Cl1 -91.63(15) . . . . ? O4 V1 V2 Cl1 94.98(15) . . . . ? O6 V1 V2 Cl1 73.81(13) . . . . ? O5 V1 V2 Cl1 171.95(9) . . . . ? V4 V1 V2 Cl1 27.02(5) . . . . ? V3 V1 V2 Cl1 -152.48(4) . . . . ? O2 V1 V2 Cl2 -5.31(15) . . . . ? O3 V1 V2 Cl2 93.17(10) . . . . ? O1 V1 V2 Cl2 8.36(15) . . . . ? O4 V1 V2 Cl2 -165.03(16) . . . . ? O6 V1 V2 Cl2 173.80(13) . . . . ? O5 V1 V2 Cl2 -88.06(10) . . . . ? V4 V1 V2 Cl2 127.01(6) . . . . ? V3 V1 V2 Cl2 -52.49(8) . . . . ? C7 O5 V3 O2 -146.1(4) . . . . ? V1 O5 V3 O2 2.90(11) . . . . ? C7 O5 V3 N4 -45.4(4) . . . . ? V1 O5 V3 N4 103.67(15) . . . . ? C7 O5 V3 N3 29.7(4) . . . . ? V1 O5 V3 N3 178.68(12) . . . . ? C7 O5 V3 Cl4 -94.3(5) . . . . ? V1 O5 V3 Cl4 54.7(4) . . . . ? C7 O5 V3 Cl3 124.2(3) . . . . ? V1 O5 V3 Cl3 -86.72(10) . . . . ? C7 O5 V3 V1 -149.0(4) . . . . ? C2 O2 V3 O5 -146.2(3) . . . . ? V1 O2 V3 O5 -3.02(11) . . . . ? C2 O2 V3 N4 131.5(3) . . . . ? V1 O2 V3 N4 -85.38(14) . . . . ? C2 O2 V3 N3 -175.1(7) . . . . ? V1 O2 V3 N3 -31.9(9) . . . . ? C2 O2 V3 Cl4 46.1(3) . . . . ? V1 O2 V3 Cl4 -170.73(10) . . . . ? C2 O2 V3 Cl3 -48.1(3) . . . . ? V1 O2 V3 Cl3 95.02(10) . . . . ? C2 O2 V3 V1 -143.1(4) . . . . ? C38 N4 V3 O5 -85.2(3) . . . . ? C34 N4 V3 O5 87.4(3) . . . . ? C38 N4 V3 O2 -9.1(4) . . . . ? C34 N4 V3 O2 163.5(3) . . . . ? C38 N4 V3 N3 178.1(4) . . . . ? C34 N4 V3 N3 -9.3(3) . . . . ? C38 N4 V3 Cl4 83.0(3) . . . . ? C34 N4 V3 Cl4 -104.4(3) . . . . ? C38 N4 V3 Cl3 168.7(4) . . . . ? C34 N4 V3 Cl3 -18.7(8) . . . . ? C38 N4 V3 V1 -46.8(3) . . . . ? C34 N4 V3 V1 125.8(3) . . . . ? C29 N3 V3 O5 103.0(4) . . . . ? C33 N3 V3 O5 -77.3(3) . . . . ? C29 N3 V3 O2 131.3(7) . . . . ? C33 N3 V3 O2 -49.0(9) . . . . ? C29 N3 V3 N4 -173.8(4) . . . . ? C33 N3 V3 N4 5.9(3) . . . . ? C29 N3 V3 Cl4 -90.0(4) . . . . ? C33 N3 V3 Cl4 89.7(3) . . . . ? C29 N3 V3 Cl3 4.5(4) . . . . ? C33 N3 V3 Cl3 -175.8(3) . . . . ? C29 N3 V3 V1 104.2(4) . . . . ? C33 N3 V3 V1 -76.1(3) . . . . ? O2 V1 V3 O5 175.38(17) . . . . ? O3 V1 V3 O5 160.84(16) . . . . ? O1 V1 V3 O5 -100.62(15) . . . . ? O4 V1 V3 O5 -20.41(15) . . . . ? O6 V1 V3 O5 77.84(15) . . . . ? V4 V1 V3 O5 113.84(12) . . . . ? V2 V1 V3 O5 -66.65(12) . . . . ? O3 V1 V3 O2 -14.54(16) . . . . ? O1 V1 V3 O2 84.01(15) . . . . ? O4 V1 V3 O2 164.21(16) . . . . ? O6 V1 V3 O2 -97.54(15) . . . . ? O5 V1 V3 O2 -175.38(17) . . . . ? V4 V1 V3 O2 -61.53(12) . . . . ? V2 V1 V3 O2 117.97(13) . . . . ? O2 V1 V3 N4 99.32(16) . . . . ? O3 V1 V3 N4 84.78(15) . . . . ? O1 V1 V3 N4 -176.68(15) . . . . ? O4 V1 V3 N4 -96.47(15) . . . . ? O6 V1 V3 N4 1.78(15) . . . . ? O5 V1 V3 N4 -76.06(16) . . . . ? V4 V1 V3 N4 37.78(12) . . . . ? V2 V1 V3 N4 -142.71(11) . . . . ? O2 V1 V3 N3 173.53(18) . . . . ? O3 V1 V3 N3 158.99(16) . . . . ? O1 V1 V3 N3 -102.46(16) . . . . ? O4 V1 V3 N3 -22.26(17) . . . . ? O6 V1 V3 N3 75.99(16) . . . . ? O5 V1 V3 N3 -1.85(17) . . . . ? V4 V1 V3 N3 112.00(13) . . . . ? V2 V1 V3 N3 -68.50(13) . . . . ? O2 V1 V3 Cl4 12.12(13) . . . . ? O3 V1 V3 Cl4 -2.42(12) . . . . ? O1 V1 V3 Cl4 96.13(11) . . . . ? O4 V1 V3 Cl4 176.33(10) . . . . ? O6 V1 V3 Cl4 -85.42(11) . . . . ? O5 V1 V3 Cl4 -163.26(13) . . . . ? V4 V1 V3 Cl4 -49.42(6) . . . . ? V2 V1 V3 Cl4 130.09(5) . . . . ? O2 V1 V3 Cl3 -86.90(13) . . . . ? O3 V1 V3 Cl3 -101.44(11) . . . . ? O1 V1 V3 Cl3 -2.90(10) . . . . ? O4 V1 V3 Cl3 77.31(11) . . . . ? O6 V1 V3 Cl3 175.56(10) . . . . ? O5 V1 V3 Cl3 97.72(12) . . . . ? V4 V1 V3 Cl3 -148.44(5) . . . . ? V2 V1 V3 Cl3 31.07(5) . . . . ? C8 O6 V4 O3 -144.7(3) . . . . ? V1 O6 V4 O3 4.52(11) . . . . ? C8 O6 V4 N6 -44.7(3) . . . . ? V1 O6 V4 N6 104.51(13) . . . . ? C8 O6 V4 N5 31.0(3) . . . . ? V1 O6 V4 N5 -179.83(13) . . . . ? C8 O6 V4 Cl5 125.2(3) . . . . ? V1 O6 V4 Cl5 -85.57(10) . . . . ? C8 O6 V4 Cl6 -94.3(5) . . . . ? V1 O6 V4 Cl6 54.9(4) . . . . ? C8 O6 V4 V1 -149.2(4) . . . . ? C3 O3 V4 O6 -146.3(3) . . . . ? V1 O3 V4 O6 -4.66(12) . . . . ? C3 O3 V4 N6 130.3(3) . . . . ? V1 O3 V4 N6 -88.03(15) . . . . ? C3 O3 V4 N5 -175.0(7) . . . . ? V1 O3 V4 N5 -33.4(8) . . . . ? C3 O3 V4 Cl5 -48.3(3) . . . . ? V1 O3 V4 Cl5 93.38(11) . . . . ? C3 O3 V4 Cl6 45.3(3) . . . . ? V1 O3 V4 Cl6 -173.07(10) . . . . ? C3 O3 V4 V1 -141.7(4) . . . . ? C56 N6 V4 O6 -85.9(4) . . . . ? C52 N6 V4 O6 89.9(3) . . . . ? C56 N6 V4 O3 -9.1(4) . . . . ? C52 N6 V4 O3 166.7(3) . . . . ? C56 N6 V4 N5 178.5(4) . . . . ? C52 N6 V4 N5 -5.7(3) . . . . ? C56 N6 V4 Cl5 163.3(5) . . . . ? C52 N6 V4 Cl5 -20.9(9) . . . . ? C56 N6 V4 Cl6 82.6(4) . . . . ? C52 N6 V4 Cl6 -101.6(3) . . . . ? C56 N6 V4 V1 -47.5(4) . . . . ? C52 N6 V4 V1 128.3(3) . . . . ? C47 N5 V4 O6 98.2(4) . . . . ? C51 N5 V4 O6 -79.8(3) . . . . ? C47 N5 V4 O3 126.3(8) . . . . ? C51 N5 V4 O3 -51.7(10) . . . . ? C47 N5 V4 N6 -177.5(4) . . . . ? C51 N5 V4 N6 4.4(3) . . . . ? C47 N5 V4 Cl5 -0.3(4) . . . . ? C51 N5 V4 Cl5 -178.4(3) . . . . ? C47 N5 V4 Cl6 -94.1(4) . . . . ? C51 N5 V4 Cl6 87.9(3) . . . . ? C47 N5 V4 V1 98.1(4) . . . . ? C51 N5 V4 V1 -80.0(3) . . . . ? O2 V1 V4 O6 -101.42(15) . . . . ? O3 V1 V4 O6 172.86(18) . . . . ? O1 V1 V4 O6 160.74(17) . . . . ? O4 V1 V4 O6 76.90(15) . . . . ? O5 V1 V4 O6 -22.02(16) . . . . ? V2 V1 V4 O6 113.13(13) . . . . ? V3 V1 V4 O6 -67.37(13) . . . . ? O2 V1 V4 O3 85.73(15) . . . . ? O1 V1 V4 O3 -12.12(17) . . . . ? O4 V1 V4 O3 -95.95(15) . . . . ? O6 V1 V4 O3 -172.86(18) . . . . ? O5 V1 V4 O3 165.12(17) . . . . ? V2 V1 V4 O3 -59.73(13) . . . . ? V3 V1 V4 O3 119.78(13) . . . . ? O2 V1 V4 N6 -177.30(13) . . . . ? O3 V1 V4 N6 96.97(16) . . . . ? O1 V1 V4 N6 84.85(15) . . . . ? O4 V1 V4 N6 1.02(13) . . . . ? O6 V1 V4 N6 -75.88(16) . . . . ? O5 V1 V4 N6 -97.91(14) . . . . ? V2 V1 V4 N6 37.24(11) . . . . ? V3 V1 V4 N6 -143.25(10) . . . . ? O2 V1 V4 N5 -101.18(16) . . . . ? O3 V1 V4 N5 173.09(18) . . . . ? O1 V1 V4 N5 160.97(16) . . . . ? O4 V1 V4 N5 77.14(16) . . . . ? O6 V1 V4 N5 0.24(17) . . . . ? O5 V1 V4 N5 -21.79(17) . . . . ? V2 V1 V4 N5 113.36(13) . . . . ? V3 V1 V4 N5 -67.13(13) . . . . ? O2 V1 V4 Cl5 -2.76(10) . . . . ? O3 V1 V4 Cl5 -88.48(13) . . . . ? O1 V1 V4 Cl5 -100.60(12) . . . . ? O4 V1 V4 Cl5 175.57(9) . . . . ? O6 V1 V4 Cl5 98.66(13) . . . . ? O5 V1 V4 Cl5 76.64(11) . . . . ? V2 V1 V4 Cl5 -148.21(4) . . . . ? V3 V1 V4 Cl5 31.30(5) . . . . ? O2 V1 V4 Cl6 94.84(10) . . . . ? O3 V1 V4 Cl6 9.11(13) . . . . ? O1 V1 V4 Cl6 -3.01(13) . . . . ? O4 V1 V4 Cl6 -86.84(10) . . . . ? O6 V1 V4 Cl6 -163.75(14) . . . . ? O5 V1 V4 Cl6 174.23(11) . . . . ? V2 V1 V4 Cl6 -50.62(7) . . . . ? V3 V1 V4 Cl6 128.89(6) . . . . ? _diffrn_measured_fraction_theta_max 0.969 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.969 _refine_diff_density_max 0.879 _refine_diff_density_min -0.804 _refine_diff_density_rms 0.082 # Attachment '9.cif' data_254sqz _database_code_depnum_ccdc_archive 'CCDC 736088' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '[V8(OH)2Cl4(cht)4(O2CPh)6(bipy)2]2MeCN' _chemical_formula_sum 'C90 H90 Cl4 N6 O26 V8' _chemical_formula_weight 2221.00 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.3600(5) _cell_length_b 15.7265(6) _cell_length_c 22.6366(8) _cell_angle_alpha 109.056(4) _cell_angle_beta 97.906(3) _cell_angle_gamma 105.983(3) _cell_volume 4810.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 11766 _cell_measurement_theta_min 2.6689 _cell_measurement_theta_max 31.8849 _exptl_crystal_description brown _exptl_crystal_colour needle _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.533 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2264 _exptl_absorpt_coefficient_mu 0.930 _exptl_absorpt_correction_type 'numeric analytical' _exptl_absorpt_correction_T_min 0.6535 _exptl_absorpt_correction_T_max 0.6535 _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.7107 _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Oxford Diffraction Xcaliber 2' _diffrn_measurement_method 'phi and omega' _diffrn_detector_area_resol_mean 8.3367 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31809 _diffrn_reflns_av_R_equivalents 0.0328 _diffrn_reflns_av_sigmaI/netI 0.0603 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.68 _diffrn_reflns_theta_max 24.71 _reflns_number_total 16265 _reflns_number_gt 10862 _reflns_threshold_expression >2sigma(I) _computing_data_collection ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) ; _computing_cell_refinement ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) ; _computing_data_reduction ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.29.1 (release 13-01-2006 CrysAlis171 .NET) (compiled Jan 13 2006,17:25:00) ; _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 ; The structure was solved by direct methods. Data processing was carried out to 0.85 angstroms as the data was only complete to this resolution. Hydrogen atoms were included in calculated positions except for the proton of the hydroxide O7 which could not be found from the data and was therefore left absent. The phenyl group C31' > C36' is disordered over two sites. Geometric and displacement restraints were applied to the anisotropic thermal parameters of this group. The atoms of the acetonitrile molecule N3 C44 C45 required the application of geometric and displacement restraints to their anisotropic thermal parameters. The acetonitrile solvent molecule N4 C46 C47 atoms had larger than average thermal parameters. The occupancy of these atoms was set to half to bring their thermal parameters in line with other similar atoms and they were left isotropic. Displacement restraints were applied to these atoms thermal parameters. The acetonotrile molecule N5 C48 C49 is disordered over three sites and has been modelled as such employing geometric and displacement restraints. The Platon Squeeze command was used to reduce the residual electron density which could not be sucessfully modelled as solvent (see below for 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^)+(0.1027P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16265 _refine_ls_number_parameters 1301 _refine_ls_number_restraints 321 _refine_ls_R_factor_all 0.0867 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1649 _refine_ls_wR_factor_gt 0.1502 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.038 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons 1 0.500 1.000 0.500 65.2 9.7 _platon_squeeze_details ; ? ; 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 0.48003(6) 1.00542(6) 0.72864(4) 0.0291(2) Uani 1 1 d . . . V2 V 0.46900(6) 0.77679(5) 0.87765(4) 0.0281(2) Uani 1 1 d . . . V3 V 0.47879(5) 0.95633(5) 0.85048(4) 0.0263(2) Uani 1 1 d . . . V4 V 0.50189(6) 1.15096(6) 0.95391(4) 0.0310(2) Uani 1 1 d . . . Cl1 Cl 0.36267(8) 0.96710(9) 0.63871(6) 0.0341(3) Uani 1 1 d . . . Cl2 Cl 0.43424(10) 0.65610(9) 0.77489(6) 0.0438(3) Uani 1 1 d . . . O1 O 0.3941(2) 0.9369(2) 0.77012(15) 0.0294(7) Uani 1 1 d . . . O2 O 0.3872(2) 0.8438(2) 0.85422(16) 0.0307(8) Uani 1 1 d . . . O3 O 0.4051(2) 1.0339(2) 0.89826(15) 0.0329(8) Uani 1 1 d . . . O4 O 0.5650(2) 1.0161(2) 0.80209(15) 0.0294(8) Uani 1 1 d . . . O5 O 0.5529(2) 0.8728(2) 0.85324(15) 0.0315(8) Uani 1 1 d . . . O6 O 0.5710(2) 1.0576(2) 0.92962(15) 0.0294(8) Uani 1 1 d . . . O7 O 0.5059(2) 1.1284(2) 1.03235(15) 0.0294(8) Uani 1 1 d . . . O8 O 0.4725(2) 1.1371(2) 0.76945(15) 0.0352(8) Uani 1 1 d . . . O9 O 0.5094(3) 1.1883(2) 0.87618(16) 0.0390(9) Uani 1 1 d . . . O10 O 0.5710(2) 0.7375(2) 0.91464(16) 0.0356(8) Uani 1 1 d . . . O11 O 0.3662(2) 0.6859(2) 0.89726(16) 0.0329(8) Uani 1 1 d . . . O12 O 0.6214(2) 1.2646(2) 0.99628(16) 0.0370(9) Uani 1 1 d . . . O13 O 0.4172(3) 1.2301(2) 0.97972(17) 0.0388(9) Uani 1 1 d . . . N1 N 0.5086(3) 0.8814(3) 0.6773(2) 0.0370(10) Uani 1 1 d . . . N2 N 0.5825(3) 1.0552(3) 0.6828(2) 0.0392(11) Uani 1 1 d . . . C1 C 0.5791(4) 0.8948(5) 0.6487(3) 0.0483(15) Uani 1 1 d . . . C2 C 0.6087(6) 0.8227(6) 0.6178(4) 0.085(3) Uani 1 1 d . . . H2 H 0.6580 0.8339 0.5984 0.102 Uiso 1 1 calc R . . C3 C 0.5644(7) 0.7327(7) 0.6158(5) 0.104(3) Uani 1 1 d . . . H3 H 0.5833 0.6822 0.5944 0.124 Uiso 1 1 calc R . . C4 C 0.4925(6) 0.7168(5) 0.6451(4) 0.081(2) Uani 1 1 d . . . H4 H 0.4626 0.6563 0.6445 0.097 Uiso 1 1 calc R . . C5 C 0.4658(4) 0.7943(4) 0.6759(3) 0.0489(15) Uani 1 1 d . . . H5 H 0.4169 0.7851 0.6959 0.059 Uiso 1 1 calc R . . C6 C 0.6210(4) 0.9921(5) 0.6524(3) 0.0443(14) Uani 1 1 d . . . C7 C 0.6969(5) 1.0206(5) 0.6288(3) 0.0621(19) Uani 1 1 d . . . H7 H 0.7282 0.9786 0.6128 0.075 Uiso 1 1 calc R . . C8 C 0.7264(5) 1.1108(6) 0.6289(3) 0.080(3) Uani 1 1 d . . . H8 H 0.7772 1.1303 0.6124 0.096 Uiso 1 1 calc R . . C9 C 0.6805(5) 1.1722(5) 0.6534(3) 0.065(2) Uani 1 1 d . . . H9 H 0.6960 1.2320 0.6506 0.079 Uiso 1 1 calc R . . C10 C 0.6109(4) 1.1436(4) 0.6823(3) 0.0451(15) Uani 1 1 d . . . H10 H 0.5828 1.1868 0.7022 0.054 Uiso 1 1 calc R . . C11 C 0.2945(3) 0.9122(3) 0.7627(2) 0.0298(11) Uani 1 1 d . . . H11 H 0.2651 0.9046 0.7192 0.036 Uiso 1 1 calc R . . C12 C 0.2561(3) 0.8163(3) 0.7707(2) 0.0322(11) Uani 1 1 d . . . H12A H 0.1883 0.7938 0.7582 0.039 Uiso 1 1 calc R . . H12B H 0.2767 0.7691 0.7420 0.039 Uiso 1 1 calc R . . C13 C 0.2882(3) 0.8249(3) 0.8389(2) 0.0301(11) Uani 1 1 d . . . H13 H 0.2562 0.7643 0.8426 0.036 Uiso 1 1 calc R . . C14 C 0.2659(3) 0.9055(4) 0.8867(2) 0.0346(12) Uani 1 1 d . . . H14A H 0.1986 0.8883 0.8799 0.042 Uiso 1 1 calc R . . H14B H 0.2916 0.9125 0.9303 0.042 Uiso 1 1 calc R . . C15 C 0.3054(3) 1.0010(4) 0.8798(2) 0.0337(12) Uani 1 1 d . . . H15 H 0.2835 1.0481 0.9081 0.040 Uiso 1 1 calc R . . C16 C 0.2734(3) 0.9911(3) 0.8112(2) 0.0321(12) Uani 1 1 d . . . H16A H 0.3038 1.0513 0.8074 0.038 Uiso 1 1 calc R . . H16B H 0.2065 0.9784 0.8011 0.038 Uiso 1 1 calc R . . C17 C 0.6641(3) 1.0352(4) 0.8196(2) 0.0344(12) Uani 1 1 d . . . H17 H 0.6930 1.0585 0.7893 0.041 Uiso 1 1 calc R . . C18 C 0.6840(3) 0.9455(4) 0.8174(2) 0.0373(13) Uani 1 1 d . . . H18A H 0.6524 0.8955 0.7751 0.045 Uiso 1 1 calc R . . H18B H 0.7506 0.9581 0.8228 0.045 Uiso 1 1 calc R . . C19 C 0.6535(3) 0.9096(4) 0.8680(2) 0.0356(12) Uani 1 1 d . . . H19 H 0.6773 0.8578 0.8676 0.043 Uiso 1 1 calc R . . C20 C 0.6923(3) 0.9894(4) 0.9346(2) 0.0374(13) Uani 1 1 d . . . H20A H 0.6670 0.9663 0.9657 0.045 Uiso 1 1 calc R . . H20B H 0.7597 1.0062 0.9467 0.045 Uiso 1 1 calc R . . C21 C 0.6693(3) 1.0777(4) 0.9376(2) 0.0341(12) Uani 1 1 d . . . H21 H 0.7015 1.1281 0.9804 0.041 Uiso 1 1 calc R . . C22 C 0.7031(3) 1.1129(4) 0.8870(2) 0.0352(12) Uani 1 1 d . . . H22A H 0.6841 1.1672 0.8880 0.042 Uiso 1 1 calc R . . H22B H 0.7709 1.1344 0.8972 0.042 Uiso 1 1 calc R . . C23 C 0.4915(3) 1.2006(3) 0.8256(2) 0.0329(12) Uani 1 1 d . . . C24 C 0.4895(4) 1.2971(4) 0.8299(3) 0.0487(15) Uani 1 1 d . . . C25 C 0.4744(5) 1.3173(4) 0.7751(3) 0.0587(18) Uani 1 1 d . . . H25 H 0.4670 1.2712 0.7348 0.070 Uiso 1 1 calc R . . C26 C 0.4702(6) 1.4051(5) 0.7801(4) 0.088(3) Uani 1 1 d . . . H26 H 0.4616 1.4193 0.7434 0.105 Uiso 1 1 calc R . . C27 C 0.4788(7) 1.4721(5) 0.8394(5) 0.104(3) Uani 1 1 d . . . H27 H 0.4752 1.5314 0.8423 0.125 Uiso 1 1 calc R . . C28 C 0.4924(7) 1.4540(5) 0.8944(4) 0.092(3) Uani 1 1 d . . . H28 H 0.4968 1.4995 0.9342 0.111 Uiso 1 1 calc R . . C29 C 0.4994(5) 1.3668(4) 0.8892(3) 0.065(2) Uani 1 1 d . . . H29 H 0.5111 1.3543 0.9264 0.078 Uiso 1 1 calc R . . C30 C 0.3360(3) 0.6847(3) 0.9454(2) 0.0320(12) Uani 1 1 d . . . C31 C 0.2384(4) 0.6185(3) 0.9331(2) 0.0340(12) Uani 1 1 d . . . C32 C 0.1901(4) 0.5554(4) 0.8706(2) 0.0408(13) Uani 1 1 d . . . H32 H 0.2192 0.5524 0.8369 0.049 Uiso 1 1 calc R . . C33 C 0.0999(4) 0.4980(4) 0.8587(3) 0.0557(17) Uani 1 1 d . . . H33 H 0.0677 0.4557 0.8168 0.067 Uiso 1 1 calc R . . C34 C 0.0562(4) 0.5016(4) 0.9077(3) 0.0618(19) Uani 1 1 d . . . H34 H -0.0052 0.4616 0.8991 0.074 Uiso 1 1 calc R . . C35 C 0.1034(4) 0.5649(4) 0.9702(3) 0.0558(17) Uani 1 1 d . . . H35 H 0.0735 0.5687 1.0035 0.067 Uiso 1 1 calc R . . C36 C 0.1944(4) 0.6219(4) 0.9824(3) 0.0439(14) Uani 1 1 d . . . H36 H 0.2268 0.6633 1.0245 0.053 Uiso 1 1 calc R . . C37 C 0.3949(4) 1.2640(3) 1.0327(3) 0.0366(13) Uani 1 1 d . . . C38 C 0.3211(4) 1.3109(4) 1.0329(3) 0.0471(15) Uani 1 1 d . . . C39 C 0.3081(4) 1.3527(4) 0.9883(3) 0.0515(16) Uani 1 1 d . . . H39 H 0.3421 1.3491 0.9572 0.062 Uiso 1 1 calc R . . C40 C 0.2428(5) 1.4002(5) 0.9911(3) 0.066(2) Uani 1 1 d . . . H40 H 0.2351 1.4308 0.9629 0.080 Uiso 1 1 calc R . . C41 C 0.1895(5) 1.4016(6) 1.0364(4) 0.076(2) Uani 1 1 d . . . H41 H 0.1445 1.4310 1.0371 0.091 Uiso 1 1 calc R . . C42 C 0.2032(5) 1.3595(6) 1.0802(4) 0.076(2) Uani 1 1 d . . . H42 H 0.1672 1.3600 1.1101 0.092 Uiso 1 1 calc R . . C43 C 0.2713(4) 1.3161(5) 1.0793(3) 0.0567(17) Uani 1 1 d . . . H43 H 0.2831 1.2907 1.1101 0.068 Uiso 1 1 calc R . . V1' V 0.96087(5) 0.78127(5) 0.37087(4) 0.02392(19) Uani 1 1 d . . . V2' V 0.87072(6) 0.64660(6) 0.56711(4) 0.0271(2) Uani 1 1 d . . . V3' V 0.95595(5) 0.66269(5) 0.45594(4) 0.02057(18) Uani 1 1 d . . . V4' V 1.06702(5) 0.53437(5) 0.39985(4) 0.02449(19) Uani 1 1 d . . . Cl1' Cl 1.05031(9) 0.93752(8) 0.38848(6) 0.0338(3) Uani 1 1 d . . . Cl2' Cl 0.79980(11) 0.76448(10) 0.59109(8) 0.0497(4) Uani 1 1 d . . . O1' O 1.0206(2) 0.7893(2) 0.45743(15) 0.0296(8) Uani 1 1 d . . . O2' O 0.9813(2) 0.7236(2) 0.55172(16) 0.0398(9) Uani 1 1 d . . . O3' O 1.0820(2) 0.6473(2) 0.47263(16) 0.0383(9) Uani 1 1 d . . . O4' O 0.8914(2) 0.6608(2) 0.37117(14) 0.0251(7) Uani 1 1 d . . . O5' O 0.8327(2) 0.6166(2) 0.47250(15) 0.0248(7) Uani 1 1 d . . . O6' O 0.9381(2) 0.5243(2) 0.40578(15) 0.0295(8) Uani 1 1 d . . . O7' O 1.0724(2) 0.4555(2) 0.44864(14) 0.0247(7) Uani 1 1 d . . . O8' O 1.0423(2) 0.7279(2) 0.32038(17) 0.0345(8) Uani 1 1 d . . . O9' O 1.0689(2) 0.6087(3) 0.34093(18) 0.0413(9) Uani 1 1 d . . . O10' O 0.7544(2) 0.5489(2) 0.56819(17) 0.0336(8) Uani 1 1 d . A . O11' O 0.9247(2) 0.6919(2) 0.66425(16) 0.0335(8) Uani 1 1 d . . . O12' O 1.0300(2) 0.4210(2) 0.31669(15) 0.0334(8) Uani 1 1 d . . . O13' O 1.2061(2) 0.5629(2) 0.40588(17) 0.0349(8) Uani 1 1 d . . . N1' N 0.8561(3) 0.8325(3) 0.40395(18) 0.0255(9) Uani 1 1 d . . . N2' N 0.8753(3) 0.7733(3) 0.28574(19) 0.0291(9) Uani 1 1 d . . . C1' C 0.7913(3) 0.8368(3) 0.3591(2) 0.0286(11) Uani 1 1 d . . . C2' C 0.7175(3) 0.8662(4) 0.3750(3) 0.0362(12) Uani 1 1 d . . . H2' H 0.6737 0.8691 0.3435 0.043 Uiso 1 1 calc R . . C3' C 0.7095(4) 0.8911(4) 0.4375(3) 0.0392(13) Uani 1 1 d . . . H3' H 0.6611 0.9122 0.4492 0.047 Uiso 1 1 calc R . . C4' C 0.7741(4) 0.8842(3) 0.4828(3) 0.0348(12) Uani 1 1 d . . . H4' H 0.7689 0.8991 0.5251 0.042 Uiso 1 1 calc R . . C5' C 0.8466(3) 0.8551(3) 0.4647(2) 0.0277(11) Uani 1 1 d . . . H5' H 0.8903 0.8510 0.4955 0.033 Uiso 1 1 calc R . . C6' C 0.8057(3) 0.8095(3) 0.2944(2) 0.0326(11) Uani 1 1 d . . . C7' C 0.7526(4) 0.8181(4) 0.2435(3) 0.0429(14) Uani 1 1 d . . . H7' H 0.7054 0.8439 0.2499 0.051 Uiso 1 1 calc R . . C8' C 0.7697(4) 0.7890(5) 0.1843(3) 0.0527(16) Uani 1 1 d . . . H8' H 0.7339 0.7938 0.1497 0.063 Uiso 1 1 calc R . . C9' C 0.8409(4) 0.7521(4) 0.1761(3) 0.0496(15) Uani 1 1 d . . . H9' H 0.8539 0.7317 0.1359 0.060 Uiso 1 1 calc R . . C10' C 0.8919(4) 0.7461(4) 0.2278(2) 0.0407(13) Uani 1 1 d . . . H10' H 0.9403 0.7219 0.2222 0.049 Uiso 1 1 calc R . . C11' C 1.1064(3) 0.8525(3) 0.5034(2) 0.0304(11) Uani 1 1 d . . . H11' H 1.1265 0.9111 0.4947 0.037 Uiso 1 1 calc R . . C12' C 1.0912(3) 0.8789(3) 0.5711(2) 0.0335(12) Uani 1 1 d . . . H12C H 1.0395 0.9029 0.5727 0.040 Uiso 1 1 calc R . . H12D H 1.1468 0.9296 0.6014 0.040 Uiso 1 1 calc R . . C13' C 1.0701(4) 0.7922(3) 0.5913(2) 0.0360(13) Uani 1 1 d . . . H13' H 1.0672 0.8135 0.6365 0.043 Uiso 1 1 calc R . . C14' C 1.1452(4) 0.7480(3) 0.5839(2) 0.0391(13) Uani 1 1 d . . . H14C H 1.1273 0.6902 0.5929 0.047 Uiso 1 1 calc R . . H14D H 1.2029 0.7922 0.6154 0.047 Uiso 1 1 calc R . . C15' C 1.1618(3) 0.7234(3) 0.5170(3) 0.0386(13) Uani 1 1 d . . . H15' H 1.2159 0.7019 0.5166 0.046 Uiso 1 1 calc R . . C16' C 1.1810(3) 0.8080(4) 0.4976(2) 0.0341(12) Uani 1 1 d . . . H16C H 1.2405 0.8556 0.5247 0.041 Uiso 1 1 calc R . . H16D H 1.1861 0.7878 0.4533 0.041 Uiso 1 1 calc R . . C17' C 0.8061(3) 0.5849(3) 0.3311(2) 0.0278(11) Uani 1 1 d . . . H17' H 0.7837 0.5988 0.2938 0.033 Uiso 1 1 calc R . . C18' C 0.7325(3) 0.5780(3) 0.3692(2) 0.0293(11) Uani 1 1 d . . . H18C H 0.6728 0.5344 0.3400 0.035 Uiso 1 1 calc R . . H18D H 0.7267 0.6405 0.3878 0.035 Uiso 1 1 calc R . . C19' C 0.7545(3) 0.5435(3) 0.4228(2) 0.0296(11) Uani 1 1 d . . . H19' H 0.7001 0.5319 0.4411 0.035 Uiso 1 1 calc R . . C20' C 0.7752(3) 0.4502(3) 0.3971(2) 0.0326(12) Uani 1 1 d . . . H20C H 0.7945 0.4329 0.4329 0.039 Uiso 1 1 calc R . . H20D H 0.7185 0.3994 0.3684 0.039 Uiso 1 1 calc R . . C21' C 0.8506(3) 0.4591(3) 0.3613(2) 0.0323(12) Uani 1 1 d . . . H21' H 0.8568 0.3961 0.3425 0.039 Uiso 1 1 calc R . . C22' C 0.8263(3) 0.4913(3) 0.3073(2) 0.0320(12) Uani 1 1 d . . . H22C H 0.7718 0.4419 0.2751 0.038 Uiso 1 1 calc R . . H22D H 0.8779 0.4999 0.2869 0.038 Uiso 1 1 calc R . . C23' C 1.0763(3) 0.6618(3) 0.3108(2) 0.0259(10) Uani 1 1 d . . . C24' C 1.1294(3) 0.6503(4) 0.2591(2) 0.0340(12) Uani 1 1 d . . . C25' C 1.1355(4) 0.7085(4) 0.2242(2) 0.0425(14) Uani 1 1 d . . . H25' H 1.1050 0.7531 0.2317 0.051 Uiso 1 1 calc R . . C26' C 1.1872(4) 0.7006(5) 0.1779(3) 0.0606(19) Uani 1 1 d . . . H26' H 1.1898 0.7382 0.1535 0.073 Uiso 1 1 calc R . . C27' C 1.2335(5) 0.6372(6) 0.1690(3) 0.075(2) Uani 1 1 d . . . H27' H 1.2697 0.6332 0.1391 0.090 Uiso 1 1 calc R . . C28' C 1.2280(5) 0.5790(6) 0.2030(4) 0.079(2) Uani 1 1 d . . . H28' H 1.2598 0.5355 0.1959 0.095 Uiso 1 1 calc R . . C29' C 1.1745(4) 0.5852(5) 0.2486(3) 0.0543(16) Uani 1 1 d . . . H29' H 1.1697 0.5452 0.2714 0.065 Uiso 1 1 calc R . . C30' C 0.7366(3) 0.4737(3) 0.5796(2) 0.0283(11) Uani 1 1 d . . . C31V C 0.6334(2) 0.4300(3) 0.5773(3) 0.0477(14) Uani 0.490(6) 1 d PGU A 1 C32V C 0.6100(3) 0.3727(5) 0.6123(3) 0.0537(16) Uani 0.490(6) 1 d PGU A 1 H32V H 0.6568 0.3642 0.6381 0.064 Uiso 0.490(6) 1 calc PR A 1 C33V C 0.5166(3) 0.3281(5) 0.6086(3) 0.0628(17) Uani 0.490(6) 1 d PGU A 1 H33V H 0.5010 0.2897 0.6320 0.075 Uiso 0.490(6) 1 calc PR A 1 C34V C 0.4466(2) 0.3407(4) 0.5700(3) 0.0642(16) Uani 0.490(6) 1 d PGU A 1 H34V H 0.3841 0.3109 0.5676 0.077 Uiso 0.490(6) 1 calc PR A 1 C35V C 0.4700(3) 0.3981(4) 0.5351(3) 0.0587(16) Uani 0.490(6) 1 d PGU A 1 H35V H 0.4232 0.4066 0.5093 0.070 Uiso 0.490(6) 1 calc PR A 1 C36V C 0.5634(3) 0.4427(4) 0.5388(3) 0.0524(15) Uani 0.490(6) 1 d PGU A 1 H36V H 0.5790 0.4811 0.5154 0.063 Uiso 0.490(6) 1 calc PR A 1 C31W C 0.6394(2) 0.4201(3) 0.5731(3) 0.0471(14) Uani 0.510(6) 1 d PGU A 2 C32W C 0.6102(3) 0.3240(3) 0.5646(4) 0.0499(16) Uani 0.510(6) 1 d PGU A 2 H32W H 0.6531 0.2921 0.5626 0.060 Uiso 0.510(6) 1 calc PR A 2 C33W C 0.5170(3) 0.2758(3) 0.5590(4) 0.0607(17) Uani 0.510(6) 1 d PGU A 2 H33W H 0.4974 0.2116 0.5533 0.073 Uiso 0.510(6) 1 calc PR A 2 C34W C 0.4529(2) 0.3236(3) 0.5618(3) 0.0649(16) Uani 0.510(6) 1 d PGU A 2 H34W H 0.3905 0.2914 0.5581 0.078 Uiso 0.510(6) 1 calc PR A 2 C35W C 0.4820(3) 0.4197(3) 0.5703(3) 0.0614(16) Uani 0.510(6) 1 d PGU A 2 H35W H 0.4392 0.4516 0.5723 0.074 Uiso 0.510(6) 1 calc PR A 2 C36W C 0.5753(3) 0.4679(3) 0.5759(3) 0.0538(15) Uani 0.510(6) 1 d PGU A 2 H36W H 0.5948 0.5321 0.5816 0.065 Uiso 0.510(6) 1 calc PR A 2 C37' C 0.9569(3) 0.6571(3) 0.7007(2) 0.0306(11) Uani 1 1 d . . . C38' C 0.9825(4) 0.7127(4) 0.7722(3) 0.0399(13) Uani 1 1 d . . . C39' C 1.0224(4) 0.6808(4) 0.8140(3) 0.0486(15) Uani 1 1 d . . . H39' H 1.0358 0.6247 0.7978 0.058 Uiso 1 1 calc R . . C40' C 1.0435(5) 0.7291(5) 0.8796(3) 0.0592(18) Uani 1 1 d . . . H40' H 1.0716 0.7057 0.9068 0.071 Uiso 1 1 calc R . . C41' C 1.0248(5) 0.8082(5) 0.9046(3) 0.069(2) Uani 1 1 d . . . H41' H 1.0394 0.8404 0.9491 0.083 Uiso 1 1 calc R . . C42' C 0.9833(6) 0.8427(5) 0.8640(4) 0.083(3) Uani 1 1 d . . . H42' H 0.9692 0.8982 0.8810 0.099 Uiso 1 1 calc R . . C43' C 0.9623(6) 0.7937(4) 0.7968(3) 0.065(2) Uani 1 1 d . . . H43' H 0.9346 0.8170 0.7693 0.078 Uiso 1 1 calc R . . N3 N 0.2512(8) 0.4237(7) 0.2568(6) 0.063(3) Uani 0.50 1 d PDU . . C44 C 0.2780(10) 0.3660(8) 0.2628(6) 0.060(3) Uani 0.50 1 d PDU . . C45 C 0.2852(11) 0.2684(9) 0.2560(8) 0.076(3) Uani 0.50 1 d PDU . . H45A H 0.2831 0.2597 0.2959 0.114 Uiso 0.50 1 calc PR . . H45B H 0.3432 0.2653 0.2458 0.114 Uiso 0.50 1 calc PR . . H45C H 0.2340 0.2188 0.2222 0.114 Uiso 0.50 1 calc PR . . N4 N 0.0975(7) 0.9363(7) 0.2111(5) 0.056(3) Uiso 0.50 1 d PU . . C46 C 0.0602(8) 0.9791(8) 0.2404(5) 0.041(2) Uiso 0.50 1 d PU . . C47 C 0.0088(7) 1.0254(7) 0.2740(4) 0.029(2) Uiso 0.50 1 d PU . . H47A H -0.0413 1.0268 0.2443 0.043 Uiso 0.50 1 calc PR . . H47B H 0.0481 1.0897 0.3012 0.043 Uiso 0.50 1 calc PR . . H47C H -0.0165 0.9924 0.3000 0.043 Uiso 0.50 1 calc PR . . N5X N 1.0380(18) 0.7519(18) 0.0737(13) 0.106(5) Uani 0.299(10) 1 d PDU B 1 C48X C 1.000(2) 0.804(2) 0.0681(16) 0.095(4) Uani 0.299(10) 1 d PDU B 1 C49X C 0.934(2) 0.860(3) 0.0580(18) 0.091(4) Uani 0.299(10) 1 d PDU B 1 H49A H 0.8757 0.8153 0.0283 0.137 Uiso 0.299(10) 1 calc PR B 1 H49B H 0.9623 0.9057 0.0409 0.137 Uiso 0.299(10) 1 calc PR B 1 H49C H 0.9224 0.8919 0.0986 0.137 Uiso 0.299(10) 1 calc PR B 1 N5Y N 1.026(2) 0.855(3) 0.0678(19) 0.096(4) Uani 0.209(10) 1 d PDU C 2 C48Y C 0.964(3) 0.878(4) 0.083(2) 0.093(4) Uani 0.209(10) 1 d PDU C 2 C49Y C 0.876(2) 0.903(3) 0.093(2) 0.087(4) Uani 0.209(10) 1 d PDU C 2 H49D H 0.8434 0.9031 0.0531 0.131 Uiso 0.209(10) 1 calc PR C 2 H49E H 0.8930 0.9651 0.1262 0.131 Uiso 0.209(10) 1 calc PR C 2 H49F H 0.8351 0.8561 0.1044 0.131 Uiso 0.209(10) 1 calc PR C 2 N5Z N 0.9050(10) 0.9637(9) -0.0160(6) 0.081(3) Uani 0.492(7) 1 d PDU D 3 C48Z C 0.9007(11) 0.9204(10) 0.0171(7) 0.076(3) Uani 0.492(7) 1 d PDU D 3 C49Z C 0.9024(15) 0.8752(14) 0.0676(9) 0.085(3) Uani 0.492(7) 1 d PDU D 3 H49G H 0.9646 0.8759 0.0818 0.127 Uiso 0.492(7) 1 calc PR D 3 H49H H 0.8599 0.8104 0.0490 0.127 Uiso 0.492(7) 1 calc PR D 3 H49I H 0.8839 0.9111 0.1039 0.127 Uiso 0.492(7) 1 calc PR D 3 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 0.0206(4) 0.0327(5) 0.0277(4) 0.0136(4) 0.0000(3) 0.0003(4) V2 0.0254(5) 0.0214(4) 0.0294(4) 0.0091(3) -0.0022(3) 0.0009(3) V3 0.0181(4) 0.0240(4) 0.0287(4) 0.0117(3) -0.0034(3) -0.0021(3) V4 0.0287(5) 0.0226(4) 0.0288(4) 0.0091(4) -0.0050(4) -0.0040(4) Cl1 0.0277(7) 0.0360(7) 0.0304(6) 0.0123(5) -0.0029(5) 0.0041(5) Cl2 0.0487(8) 0.0306(7) 0.0353(7) 0.0053(6) -0.0047(6) 0.0044(6) O1 0.0188(17) 0.0336(18) 0.0297(18) 0.0151(15) -0.0024(14) 0.0000(14) O2 0.0193(17) 0.0283(17) 0.0416(19) 0.0185(15) 0.0008(15) 0.0011(14) O3 0.0206(18) 0.0283(18) 0.0346(19) 0.0058(15) -0.0035(14) -0.0019(15) O4 0.0179(17) 0.0367(19) 0.0307(18) 0.0172(15) 0.0020(14) 0.0020(15) O5 0.0213(18) 0.0313(18) 0.0340(18) 0.0119(15) -0.0016(14) 0.0020(15) O6 0.0184(17) 0.0301(18) 0.0312(18) 0.0148(15) -0.0028(14) -0.0036(14) O7 0.0289(19) 0.0232(16) 0.0262(17) 0.0099(14) -0.0022(14) -0.0020(14) O8 0.033(2) 0.0326(19) 0.0300(19) 0.0136(16) -0.0019(15) -0.0007(16) O9 0.047(2) 0.0326(19) 0.0284(19) 0.0147(16) -0.0021(16) 0.0026(17) O10 0.035(2) 0.0278(18) 0.038(2) 0.0133(16) -0.0035(16) 0.0070(16) O11 0.035(2) 0.0244(17) 0.0309(19) 0.0123(15) 0.0002(16) -0.0010(15) O12 0.037(2) 0.0257(17) 0.0309(19) 0.0126(15) -0.0040(16) -0.0116(15) O13 0.044(2) 0.0287(19) 0.035(2) 0.0111(16) -0.0071(17) 0.0073(17) N1 0.032(3) 0.046(3) 0.035(2) 0.018(2) 0.009(2) 0.013(2) N2 0.026(2) 0.051(3) 0.031(2) 0.019(2) -0.0028(19) -0.003(2) C1 0.035(3) 0.068(4) 0.051(4) 0.027(3) 0.016(3) 0.024(3) C2 0.090(6) 0.094(6) 0.129(7) 0.070(6) 0.081(6) 0.061(5) C3 0.121(8) 0.092(6) 0.158(9) 0.062(6) 0.105(7) 0.075(6) C4 0.092(6) 0.056(4) 0.111(6) 0.031(4) 0.055(5) 0.036(4) C5 0.043(4) 0.048(4) 0.060(4) 0.021(3) 0.017(3) 0.021(3) C6 0.028(3) 0.066(4) 0.035(3) 0.022(3) 0.007(2) 0.006(3) C7 0.047(4) 0.080(5) 0.042(4) 0.012(3) 0.022(3) 0.006(4) C8 0.058(5) 0.093(6) 0.050(4) 0.014(4) 0.025(4) -0.019(4) C9 0.053(4) 0.074(5) 0.040(4) 0.023(3) 0.003(3) -0.019(4) C10 0.032(3) 0.053(4) 0.033(3) 0.020(3) -0.005(2) -0.010(3) C11 0.016(2) 0.038(3) 0.027(3) 0.013(2) -0.0041(19) 0.000(2) C12 0.020(3) 0.031(3) 0.034(3) 0.008(2) 0.001(2) -0.001(2) C13 0.014(2) 0.028(3) 0.036(3) 0.014(2) -0.003(2) -0.008(2) C14 0.020(3) 0.043(3) 0.031(3) 0.012(2) -0.001(2) -0.001(2) C15 0.019(3) 0.032(3) 0.034(3) 0.002(2) -0.001(2) 0.002(2) C16 0.019(3) 0.032(3) 0.042(3) 0.018(2) 0.003(2) 0.003(2) C17 0.017(3) 0.044(3) 0.039(3) 0.022(2) 0.001(2) 0.001(2) C18 0.018(3) 0.049(3) 0.036(3) 0.015(3) -0.001(2) 0.005(2) C19 0.017(3) 0.044(3) 0.045(3) 0.022(3) 0.000(2) 0.007(2) C20 0.019(3) 0.046(3) 0.039(3) 0.020(3) -0.004(2) 0.000(2) C21 0.021(3) 0.036(3) 0.031(3) 0.015(2) -0.008(2) -0.005(2) C22 0.017(3) 0.041(3) 0.037(3) 0.020(2) -0.005(2) -0.007(2) C23 0.026(3) 0.029(3) 0.030(3) 0.012(2) -0.004(2) -0.007(2) C24 0.049(4) 0.032(3) 0.047(3) 0.016(3) -0.012(3) -0.004(3) C25 0.070(5) 0.036(3) 0.055(4) 0.021(3) -0.009(3) 0.004(3) C26 0.132(8) 0.047(4) 0.069(5) 0.031(4) -0.020(5) 0.022(4) C27 0.151(9) 0.037(4) 0.103(7) 0.026(5) -0.011(6) 0.021(5) C28 0.142(8) 0.034(4) 0.073(5) 0.014(4) -0.008(5) 0.014(4) C29 0.094(6) 0.027(3) 0.049(4) 0.011(3) -0.013(4) 0.001(3) C30 0.030(3) 0.019(2) 0.036(3) 0.011(2) -0.008(2) -0.002(2) C31 0.033(3) 0.024(3) 0.035(3) 0.014(2) -0.002(2) -0.003(2) C32 0.037(3) 0.035(3) 0.032(3) 0.009(2) -0.004(2) -0.005(2) C33 0.045(4) 0.048(4) 0.041(3) 0.006(3) -0.008(3) -0.012(3) C34 0.035(4) 0.054(4) 0.062(4) 0.012(3) 0.002(3) -0.019(3) C35 0.043(4) 0.054(4) 0.051(4) 0.016(3) 0.012(3) -0.007(3) C36 0.041(3) 0.033(3) 0.037(3) 0.009(2) -0.002(3) -0.008(3) C37 0.038(3) 0.024(3) 0.036(3) 0.008(2) -0.007(2) 0.003(2) C38 0.044(4) 0.037(3) 0.044(3) 0.008(3) -0.013(3) 0.009(3) C39 0.058(4) 0.048(3) 0.040(3) 0.010(3) -0.004(3) 0.021(3) C40 0.078(5) 0.062(4) 0.055(4) 0.017(3) -0.008(4) 0.037(4) C41 0.077(5) 0.088(6) 0.061(5) 0.010(4) 0.006(4) 0.053(5) C42 0.075(5) 0.092(6) 0.074(5) 0.030(4) 0.017(4) 0.049(5) C43 0.048(4) 0.061(4) 0.061(4) 0.021(3) 0.011(3) 0.024(3) V1' 0.0212(4) 0.0205(4) 0.0285(4) 0.0100(3) 0.0048(3) 0.0050(3) V2' 0.0249(4) 0.0239(4) 0.0405(5) 0.0162(4) 0.0182(4) 0.0109(3) V3' 0.0152(4) 0.0173(4) 0.0256(4) 0.0071(3) 0.0039(3) 0.0019(3) V4' 0.0203(4) 0.0220(4) 0.0267(4) 0.0058(3) 0.0018(3) 0.0067(3) Cl1' 0.0342(7) 0.0245(6) 0.0404(7) 0.0165(5) 0.0051(5) 0.0039(5) Cl2' 0.0597(10) 0.0447(8) 0.0690(10) 0.0292(7) 0.0346(8) 0.0361(7) O1' 0.0265(18) 0.0186(16) 0.0344(18) 0.0118(14) -0.0051(14) -0.0021(14) O2' 0.032(2) 0.036(2) 0.0307(19) 0.0016(16) 0.0142(16) -0.0092(16) O3' 0.0250(19) 0.0224(17) 0.044(2) -0.0071(15) -0.0129(16) 0.0077(15) O4' 0.0230(17) 0.0230(16) 0.0234(16) 0.0087(13) 0.0021(13) 0.0010(14) O5' 0.0168(16) 0.0284(17) 0.0312(17) 0.0155(14) 0.0072(14) 0.0052(14) O6' 0.0150(16) 0.0186(16) 0.0410(19) 0.0009(14) -0.0019(14) 0.0021(13) O7' 0.0222(17) 0.0234(16) 0.0262(17) 0.0072(13) 0.0044(13) 0.0078(14) O8' 0.038(2) 0.0331(19) 0.045(2) 0.0228(17) 0.0209(17) 0.0162(17) O9' 0.037(2) 0.052(2) 0.053(2) 0.034(2) 0.0162(18) 0.0237(19) O10' 0.0272(19) 0.0308(18) 0.055(2) 0.0252(17) 0.0218(17) 0.0124(15) O11' 0.043(2) 0.0246(17) 0.038(2) 0.0129(16) 0.0225(17) 0.0125(16) O12' 0.037(2) 0.0310(19) 0.0270(18) 0.0024(15) 0.0015(15) 0.0179(16) O13' 0.0214(18) 0.0363(19) 0.053(2) 0.0279(18) 0.0074(16) 0.0072(16) N1' 0.026(2) 0.0187(19) 0.033(2) 0.0107(17) 0.0069(18) 0.0075(17) N2' 0.030(2) 0.028(2) 0.028(2) 0.0127(18) 0.0050(18) 0.0073(18) C1' 0.028(3) 0.022(2) 0.037(3) 0.014(2) 0.008(2) 0.007(2) C2' 0.023(3) 0.033(3) 0.050(3) 0.017(3) 0.004(2) 0.007(2) C3' 0.029(3) 0.030(3) 0.057(4) 0.011(3) 0.015(3) 0.011(2) C4' 0.034(3) 0.029(3) 0.035(3) 0.007(2) 0.011(2) 0.006(2) C5' 0.026(3) 0.022(2) 0.030(3) 0.007(2) 0.005(2) 0.003(2) C6' 0.028(3) 0.031(3) 0.037(3) 0.016(2) 0.004(2) 0.006(2) C7' 0.040(3) 0.047(3) 0.044(3) 0.024(3) 0.001(3) 0.014(3) C8' 0.051(4) 0.066(4) 0.042(4) 0.027(3) 0.000(3) 0.019(3) C9' 0.056(4) 0.057(4) 0.031(3) 0.016(3) 0.007(3) 0.016(3) C10' 0.044(3) 0.042(3) 0.033(3) 0.014(2) 0.009(3) 0.011(3) C11' 0.027(3) 0.018(2) 0.036(3) 0.015(2) -0.006(2) -0.007(2) C12' 0.027(3) 0.023(2) 0.039(3) 0.002(2) 0.001(2) 0.006(2) C13' 0.033(3) 0.031(3) 0.023(2) 0.001(2) 0.009(2) -0.012(2) C14' 0.036(3) 0.024(3) 0.039(3) 0.014(2) -0.015(2) -0.008(2) C15' 0.020(3) 0.027(3) 0.046(3) -0.005(2) -0.015(2) 0.008(2) C16' 0.016(2) 0.044(3) 0.024(2) 0.005(2) 0.002(2) -0.005(2) C17' 0.018(2) 0.027(2) 0.028(3) 0.009(2) -0.0031(19) -0.002(2) C18' 0.015(2) 0.028(3) 0.039(3) 0.011(2) -0.001(2) 0.006(2) C19' 0.014(2) 0.037(3) 0.040(3) 0.022(2) 0.004(2) 0.004(2) C20' 0.019(3) 0.024(2) 0.043(3) 0.016(2) -0.008(2) -0.006(2) C21' 0.022(3) 0.015(2) 0.046(3) 0.003(2) -0.002(2) 0.002(2) C22' 0.019(3) 0.027(3) 0.035(3) -0.001(2) 0.005(2) 0.001(2) C23' 0.018(2) 0.029(3) 0.022(2) 0.006(2) 0.0008(19) 0.001(2) C24' 0.026(3) 0.039(3) 0.027(3) 0.004(2) 0.007(2) 0.004(2) C25' 0.024(3) 0.056(4) 0.033(3) 0.014(3) 0.005(2) -0.003(3) C26' 0.037(4) 0.082(5) 0.040(4) 0.016(3) 0.013(3) -0.005(3) C27' 0.055(5) 0.098(6) 0.050(4) 0.010(4) 0.028(4) 0.008(4) C28' 0.072(5) 0.083(6) 0.078(5) 0.007(5) 0.036(4) 0.041(5) C29' 0.044(4) 0.057(4) 0.056(4) 0.008(3) 0.016(3) 0.023(3) C30' 0.027(3) 0.029(3) 0.028(3) 0.011(2) 0.009(2) 0.006(2) C31V 0.029(2) 0.048(3) 0.084(3) 0.038(3) 0.031(2) 0.017(2) C32V 0.033(2) 0.052(3) 0.090(3) 0.038(3) 0.031(3) 0.014(2) C33V 0.036(3) 0.057(3) 0.098(4) 0.033(3) 0.033(3) 0.010(2) C34V 0.034(2) 0.058(3) 0.101(3) 0.027(3) 0.033(3) 0.013(2) C35V 0.030(2) 0.058(3) 0.094(3) 0.028(3) 0.032(3) 0.017(2) C36V 0.030(2) 0.053(3) 0.088(3) 0.033(3) 0.032(2) 0.018(2) C31W 0.029(2) 0.048(3) 0.084(3) 0.039(3) 0.031(2) 0.017(2) C32W 0.031(2) 0.048(3) 0.087(3) 0.039(3) 0.032(3) 0.015(2) C33W 0.035(3) 0.054(3) 0.098(4) 0.032(3) 0.032(3) 0.011(2) C34W 0.034(2) 0.060(3) 0.101(3) 0.027(3) 0.033(3) 0.013(2) C35W 0.032(2) 0.059(3) 0.098(3) 0.030(3) 0.032(3) 0.016(2) C36W 0.031(2) 0.053(3) 0.092(3) 0.035(3) 0.031(3) 0.018(2) C37' 0.026(3) 0.026(3) 0.035(3) 0.009(2) 0.010(2) 0.005(2) C38' 0.039(3) 0.029(3) 0.041(3) 0.003(2) 0.017(3) 0.005(2) C39' 0.041(3) 0.046(3) 0.042(3) 0.007(3) 0.006(3) 0.002(3) C40' 0.058(4) 0.056(4) 0.040(3) 0.004(3) 0.012(3) 0.001(3) C41' 0.079(5) 0.068(5) 0.039(4) 0.010(4) 0.023(4) 0.002(4) C42' 0.135(8) 0.036(4) 0.063(5) 0.000(3) 0.048(5) 0.019(4) C43' 0.106(6) 0.039(4) 0.048(4) 0.012(3) 0.032(4) 0.023(4) N3 0.065(6) 0.070(6) 0.083(6) 0.039(5) 0.041(5) 0.041(5) C44 0.071(6) 0.082(6) 0.064(6) 0.042(5) 0.046(5) 0.051(5) C45 0.091(7) 0.096(7) 0.091(7) 0.056(6) 0.051(6) 0.069(6) N5X 0.096(9) 0.090(9) 0.116(10) 0.019(9) 0.030(9) 0.028(7) C48X 0.088(7) 0.081(7) 0.105(8) 0.021(6) 0.044(7) 0.022(6) C49X 0.088(7) 0.077(7) 0.101(7) 0.023(6) 0.047(6) 0.020(6) N5Y 0.089(7) 0.083(8) 0.106(8) 0.019(7) 0.043(7) 0.025(7) C48Y 0.088(7) 0.079(7) 0.103(7) 0.022(6) 0.045(7) 0.022(6) C49Y 0.088(7) 0.072(7) 0.099(8) 0.025(7) 0.046(7) 0.021(6) N5Z 0.086(7) 0.069(7) 0.093(8) 0.024(5) 0.046(6) 0.033(6) C48Z 0.078(6) 0.064(6) 0.093(7) 0.022(4) 0.048(6) 0.035(5) C49Z 0.086(7) 0.071(6) 0.097(7) 0.028(5) 0.048(6) 0.021(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 O4 1.896(3) . ? V1 O1 2.000(3) . ? V1 O8 2.016(4) . ? V1 N2 2.115(4) . ? V1 N1 2.116(4) . ? V1 Cl1 2.3126(14) . ? V1 V3 3.0983(11) . ? V2 O2 1.970(3) . ? V2 O5 1.979(3) . ? V2 O7 2.002(3) 2_677 ? V2 O10 2.011(4) . ? V2 O11 2.023(3) . ? V2 Cl2 2.3485(15) . ? V2 V3 3.0495(11) . ? V3 O1 1.965(3) . ? V3 O2 1.969(3) . ? V3 O5 1.970(3) . ? V3 O6 1.987(3) . ? V3 O3 2.044(3) . ? V3 O4 2.054(3) . ? V3 V4 3.0775(12) . ? V4 O3 1.910(3) . ? V4 O7 1.917(3) . ? V4 O12 2.018(3) . ? V4 O6 2.019(3) . ? V4 O9 2.036(3) . ? V4 O13 2.052(4) . ? O1 C11 1.443(5) . ? O2 C13 1.435(5) . ? O3 C15 1.425(6) . ? O4 C17 1.439(6) . ? O5 C19 1.440(6) . ? O6 C21 1.427(6) . ? O7 V2 2.002(3) 2_677 ? O8 C23 1.268(6) . ? O9 C23 1.230(6) . ? O10 C37 1.245(6) 2_677 ? O11 C30 1.246(6) . ? O12 C30 1.262(6) 2_677 ? O13 C37 1.278(6) . ? N1 C5 1.333(7) . ? N1 C1 1.340(7) . ? N2 C6 1.340(7) . ? N2 C10 1.342(7) . ? C1 C2 1.354(9) . ? C1 C6 1.456(8) . ? C2 C3 1.374(11) . ? C2 H2 0.9300 . ? C3 C4 1.372(10) . ? C3 H3 0.9300 . ? C4 C5 1.393(9) . ? C4 H4 0.9300 . ? C5 H5 0.9300 . ? C6 C7 1.373(8) . ? C7 C8 1.364(10) . ? C7 H7 0.9300 . ? C8 C9 1.367(11) . ? C8 H8 0.9300 . ? C9 C10 1.377(8) . ? C9 H9 0.9300 . ? C10 H10 0.9300 . ? C11 C16 1.509(7) . ? C11 C12 1.541(7) . ? C11 H11 0.9800 . ? C12 C13 1.504(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C13 C14 1.531(7) . ? C13 H13 0.9800 . ? C14 C15 1.525(7) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C15 C16 1.506(7) . ? C15 H15 0.9800 . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C17 C18 1.510(7) . ? C17 C22 1.519(7) . ? C17 H17 0.9800 . ? C18 C19 1.508(7) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 C20 1.520(7) . ? C19 H19 0.9800 . ? C20 C21 1.508(7) . ? C20 H20A 0.9700 . ? C20 H20B 0.9700 . ? C21 C22 1.521(7) . ? C21 H21 0.9800 . ? C22 H22A 0.9700 . ? C22 H22B 0.9700 . ? C23 C24 1.497(7) . ? C24 C25 1.384(8) . ? C24 C29 1.385(8) . ? C25 C26 1.367(9) . ? C25 H25 0.9300 . ? C26 C27 1.372(11) . ? C26 H26 0.9300 . ? C27 C28 1.366(11) . ? C27 H27 0.9300 . ? C28 C29 1.373(9) . ? C28 H28 0.9300 . ? C29 H29 0.9300 . ? C30 O12 1.262(6) 2_677 ? C30 C31 1.498(7) . ? C31 C36 1.375(7) . ? C31 C32 1.389(7) . ? C32 C33 1.363(8) . ? C32 H32 0.9300 . ? C33 C34 1.368(9) . ? C33 H33 0.9300 . ? C34 C35 1.384(8) . ? C34 H34 0.9300 . ? C35 C36 1.370(8) . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ? C37 O10 1.245(6) 2_677 ? C37 C38 1.514(8) . ? C38 C43 1.377(9) . ? C38 C39 1.393(8) . ? C39 C40 1.403(9) . ? C39 H39 0.9300 . ? C40 C41 1.395(10) . ? C40 H40 0.9300 . ? C41 C42 1.385(10) . ? C41 H41 0.9300 . ? C42 C43 1.397(9) . ? C42 H42 0.9300 . ? C43 H43 0.9300 . ? V1' O4' 1.904(3) . ? V1' O8' 1.980(3) . ? V1' O1' 1.994(3) . ? V1' N1' 2.110(4) . ? V1' N2' 2.124(4) . ? V1' Cl1' 2.3313(14) . ? V1' V3' 3.0821(11) . ? V2' O2' 1.944(3) . ? V2' O7' 1.988(3) 2_766 ? V2' O5' 1.999(3) . ? V2' O10' 2.020(3) . ? V2' O11' 2.045(4) . ? V2' Cl2' 2.3528(15) . ? V2' V3' 3.0415(11) . ? V3' O1' 1.951(3) . ? V3' O5' 1.967(3) . ? V3' O2' 1.994(3) . ? V3' O3' 2.016(3) . ? V3' O6' 2.018(3) . ? V3' O4' 2.022(3) . ? V3' V4' 3.0682(11) . ? V4' O3' 1.919(3) . ? V4' O7' 1.921(3) . ? V4' O6' 1.970(3) . ? V4' O12' 2.000(3) . ? V4' O13' 2.033(3) . ? V4' O9' 2.038(4) . ? O1' C11' 1.426(5) . ? O2' C13' 1.432(6) . ? O3' C15' 1.419(5) . ? O4' C17' 1.439(5) . ? O5' C19' 1.432(5) . ? O6' C21' 1.438(5) . ? O7' V2' 1.988(3) 2_766 ? O8' C23' 1.258(6) . ? O9' C23' 1.233(6) . ? O10' C30' 1.257(6) . ? O11' C37' 1.247(6) . ? O12' C37' 1.244(6) 2_766 ? O13' C30' 1.241(6) 2_766 ? N1' C5' 1.343(6) . ? N1' C1' 1.353(6) . ? N2' C10' 1.324(6) . ? N2' C6' 1.352(6) . ? C1' C2' 1.387(7) . ? C1' C6' 1.452(7) . ? C2' C3' 1.373(7) . ? C2' H2' 0.9300 . ? C3' C4' 1.378(8) . ? C3' H3' 0.9300 . ? C4' C5' 1.379(7) . ? C4' H4' 0.9300 . ? C5' H5' 0.9300 . ? C6' C7' 1.383(7) . ? C7' C8' 1.355(8) . ? C7' H7' 0.9300 . ? C8' C9' 1.380(9) . ? C8' H8' 0.9300 . ? C9' C10' 1.361(8) . ? C9' H9' 0.9300 . ? C10' H10' 0.9300 . ? C11' C16' 1.499(7) . ? C11' C12' 1.520(7) . ? C11' H11' 0.9800 . ? C12' C13' 1.542(7) . ? C12' H12C 0.9700 . ? C12' H12D 0.9700 . ? C13' C14' 1.502(8) . ? C13' H13' 0.9800 . ? C14' C15' 1.513(8) . ? C14' H14C 0.9700 . ? C14' H14D 0.9700 . ? C15' C16' 1.499(7) . ? C15' H15' 0.9800 . ? C16' H16C 0.9700 . ? C16' H16D 0.9700 . ? C17' C18' 1.515(7) . ? C17' C22' 1.527(7) . ? C17' H17' 0.9800 . ? C18' C19' 1.517(7) . ? C18' H18C 0.9700 . ? C18' H18D 0.9700 . ? C19' C20' 1.530(7) . ? C19' H19' 0.9800 . ? C20' C21' 1.504(7) . ? C20' H20C 0.9700 . ? C20' H20D 0.9700 . ? C21' C22' 1.506(7) . ? C21' H21' 0.9800 . ? C22' H22C 0.9700 . ? C22' H22D 0.9700 . ? C23' C24' 1.507(7) . ? C24' C29' 1.365(8) . ? C24' C25' 1.384(8) . ? C25' C26' 1.393(8) . ? C25' H25' 0.9300 . ? C26' C27' 1.356(11) . ? C26' H26' 0.9300 . ? C27' C28' 1.370(11) . ? C27' H27' 0.9300 . ? C28' C29' 1.400(9) . ? C28' H28' 0.9300 . ? C29' H29' 0.9300 . ? C30' O13' 1.241(6) 2_766 ? C30' C31W 1.458(5) . ? C30' C31V 1.530(5) . ? C31V C32V 1.3900 . ? C31V C36V 1.3900 . ? C32V C33V 1.3900 . ? C32V H32V 0.9300 . ? C33V C34V 1.3900 . ? C33V H33V 0.9300 . ? C34V C35V 1.3900 . ? C34V H34V 0.9300 . ? C35V C36V 1.3900 . ? C35V H35V 0.9300 . ? C36V H36V 0.9300 . ? C31W C36W 1.3900 . ? C31W C32W 1.3901 . ? C32W C33W 1.3900 . ? C32W H32W 0.9300 . ? C33W C34W 1.3900 . ? C33W H33W 0.9300 . ? C34W C35W 1.3900 . ? C34W H34W 0.9300 . ? C35W C36W 1.3899 . ? C35W H35W 0.9300 . ? C36W H36W 0.9300 . ? C37' O12' 1.244(6) 2_766 ? C37' C38' 1.500(7) . ? C38' C43' 1.353(8) . ? C38' C39' 1.358(8) . ? C39' C40' 1.372(8) . ? C39' H39' 0.9300 . ? C40' C41' 1.316(10) . ? C40' H40' 0.9300 . ? C41' C42' 1.378(11) . ? C41' H41' 0.9300 . ? C42' C43' 1.405(9) . ? C42' H42' 0.9300 . ? C43' H43' 0.9300 . ? N3 C44 1.132(8) . ? C44 C45 1.528(8) . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? N4 C46 1.116(13) . ? C46 C47 1.360(14) . ? C47 H47A 0.9600 . ? C47 H47B 0.9600 . ? C47 H47C 0.9600 . ? N5X C48X 1.162(9) . ? C48X C49X 1.546(9) . ? C49X H49A 0.9600 . ? C49X H49B 0.9600 . ? C49X H49C 0.9600 . ? N5Y C48Y 1.162(9) . ? C48Y C49Y 1.542(9) . ? C49Y H49D 0.9600 . ? C49Y H49E 0.9600 . ? C49Y H49F 0.9600 . ? N5Z C48Z 1.163(8) . ? C48Z C49Z 1.532(8) . ? C49Z H49G 0.9600 . ? C49Z H49H 0.9600 . ? C49Z H49I 0.9600 . ? 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 O4 V1 O1 78.24(13) . . ? O4 V1 O8 94.80(14) . . ? O1 V1 O8 98.84(14) . . ? O4 V1 N2 96.26(15) . . ? O1 V1 N2 168.24(17) . . ? O8 V1 N2 91.93(17) . . ? O4 V1 N1 86.77(16) . . ? O1 V1 N1 93.05(15) . . ? O8 V1 N1 168.08(16) . . ? N2 V1 N1 76.16(18) . . ? O4 V1 Cl1 170.25(11) . . ? O1 V1 Cl1 93.78(10) . . ? O8 V1 Cl1 91.94(10) . . ? N2 V1 Cl1 90.54(12) . . ? N1 V1 Cl1 88.09(12) . . ? O4 V1 V3 40.20(9) . . ? O1 V1 V3 38.22(9) . . ? O8 V1 V3 95.95(10) . . ? N2 V1 V3 136.16(12) . . ? N1 V1 V3 92.87(12) . . ? Cl1 V1 V3 131.99(5) . . ? O2 V2 O5 77.17(13) . . ? O2 V2 O7 84.92(14) . 2_677 ? O5 V2 O7 91.93(13) . 2_677 ? O2 V2 O10 167.40(14) . . ? O5 V2 O10 95.26(14) . . ? O7 V2 O10 85.30(14) 2_677 . ? O2 V2 O11 93.35(14) . . ? O5 V2 O11 170.45(14) . . ? O7 V2 O11 88.33(13) 2_677 . ? O10 V2 O11 94.28(14) . . ? O2 V2 Cl2 97.03(11) . . ? O5 V2 Cl2 92.44(10) . . ? O7 V2 Cl2 175.52(10) 2_677 . ? O10 V2 Cl2 93.30(11) . . ? O11 V2 Cl2 87.54(10) . . ? O2 V2 V3 39.26(9) . . ? O5 V2 V3 39.33(10) . . ? O7 V2 V3 79.93(9) 2_677 . ? O10 V2 V3 130.67(10) . . ? O11 V2 V3 131.60(10) . . ? Cl2 V2 V3 104.13(5) . . ? O1 V3 O2 88.76(13) . . ? O1 V3 O5 121.90(14) . . ? O2 V3 O5 77.41(13) . . ? O1 V3 O6 142.48(14) . . ? O2 V3 O6 121.28(14) . . ? O5 V3 O6 88.73(14) . . ? O1 V3 O3 86.89(14) . . ? O2 V3 O3 86.31(14) . . ? O5 V3 O3 145.97(14) . . ? O6 V3 O3 74.42(13) . . ? O1 V3 O4 75.42(13) . . ? O2 V3 O4 149.75(14) . . ? O5 V3 O4 89.15(14) . . ? O6 V3 O4 84.81(13) . . ? O3 V3 O4 117.69(14) . . ? O1 V3 V2 116.03(10) . . ? O2 V3 V2 39.28(9) . . ? O5 V3 V2 39.55(10) . . ? O6 V3 V2 101.36(10) . . ? O3 V3 V2 114.36(10) . . ? O4 V3 V2 127.23(10) . . ? O1 V3 V4 109.00(10) . . ? O2 V3 V4 115.85(10) . . ? O5 V3 V4 127.96(10) . . ? O6 V3 V4 40.17(10) . . ? O3 V3 V4 37.36(9) . . ? O4 V3 V4 93.84(10) . . ? V2 V3 V4 124.32(3) . . ? O1 V3 V1 39.03(9) . . ? O2 V3 V1 124.63(10) . . ? O5 V3 V1 110.79(10) . . ? O6 V3 V1 113.73(9) . . ? O3 V3 V1 103.08(10) . . ? O4 V3 V1 36.57(9) . . ? V2 V3 V1 134.22(4) . . ? V4 V3 V1 101.40(3) . . ? O3 V4 O7 97.76(14) . . ? O3 V4 O12 165.92(16) . . ? O7 V4 O12 90.74(13) . . ? O3 V4 O6 76.67(13) . . ? O7 V4 O6 85.97(14) . . ? O12 V4 O6 92.85(14) . . ? O3 V4 O9 88.40(14) . . ? O7 V4 O9 173.83(14) . . ? O12 V4 O9 83.14(14) . . ? O6 V4 O9 95.15(14) . . ? O3 V4 O13 97.10(15) . . ? O7 V4 O13 89.64(15) . . ? O12 V4 O13 94.14(15) . . ? O6 V4 O13 171.79(14) . . ? O9 V4 O13 89.95(15) . . ? O3 V4 V3 40.50(10) . . ? O7 V4 V3 104.38(10) . . ? O12 V4 V3 126.36(12) . . ? O6 V4 V3 39.43(9) . . ? O9 V4 V3 80.09(10) . . ? O13 V4 V3 136.06(10) . . ? C11 O1 V3 121.6(3) . . ? C11 O1 V1 131.5(3) . . ? V3 O1 V1 102.76(14) . . ? C13 O2 V3 123.0(3) . . ? C13 O2 V2 135.5(3) . . ? V3 O2 V2 101.46(14) . . ? C15 O3 V4 135.8(3) . . ? C15 O3 V3 121.3(3) . . ? V4 O3 V3 102.14(15) . . ? C17 O4 V1 134.5(3) . . ? C17 O4 V3 120.6(3) . . ? V1 O4 V3 103.23(14) . . ? C19 O5 V3 121.0(3) . . ? C19 O5 V2 130.0(3) . . ? V3 O5 V2 101.12(15) . . ? C21 O6 V3 121.8(3) . . ? C21 O6 V4 128.4(3) . . ? V3 O6 V4 100.39(14) . . ? V4 O7 V2 128.40(16) . 2_677 ? C23 O8 V1 137.9(3) . . ? C23 O9 V4 165.0(4) . . ? C37 O10 V2 138.0(4) 2_677 . ? C30 O11 V2 136.5(3) . . ? C30 O12 V4 132.7(3) 2_677 . ? C37 O13 V4 132.4(3) . . ? C5 N1 C1 119.3(5) . . ? C5 N1 V1 124.3(4) . . ? C1 N1 V1 116.2(4) . . ? C6 N2 C10 119.0(5) . . ? C6 N2 V1 116.0(4) . . ? C10 N2 V1 125.0(4) . . ? N1 C1 C2 122.3(6) . . ? N1 C1 C6 115.4(5) . . ? C2 C1 C6 122.3(6) . . ? C1 C2 C3 118.6(7) . . ? C1 C2 H2 120.7 . . ? C3 C2 H2 120.7 . . ? C4 C3 C2 120.5(7) . . ? C4 C3 H3 119.7 . . ? C2 C3 H3 119.7 . . ? C3 C4 C5 117.7(7) . . ? C3 C4 H4 121.2 . . ? C5 C4 H4 121.2 . . ? N1 C5 C4 121.6(6) . . ? N1 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? N2 C6 C7 120.7(6) . . ? N2 C6 C1 115.6(5) . . ? C7 C6 C1 123.7(6) . . ? C8 C7 C6 119.8(7) . . ? C8 C7 H7 120.1 . . ? C6 C7 H7 120.1 . . ? C7 C8 C9 119.4(6) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? C8 C9 C10 118.6(7) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? N2 C10 C9 121.8(7) . . ? N2 C10 H10 119.1 . . ? C9 C10 H10 119.1 . . ? O1 C11 C16 110.1(4) . . ? O1 C11 C12 109.0(4) . . ? C16 C11 C12 111.5(4) . . ? O1 C11 H11 108.7 . . ? C16 C11 H11 108.7 . . ? C12 C11 H11 108.7 . . ? C13 C12 C11 112.2(4) . . ? C13 C12 H12A 109.2 . . ? C11 C12 H12A 109.2 . . ? C13 C12 H12B 109.2 . . ? C11 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? O2 C13 C12 109.4(4) . . ? O2 C13 C14 109.4(4) . . ? C12 C13 C14 111.0(4) . . ? O2 C13 H13 109.0 . . ? C12 C13 H13 109.0 . . ? C14 C13 H13 109.0 . . ? C15 C14 C13 112.5(4) . . ? C15 C14 H14A 109.1 . . ? C13 C14 H14A 109.1 . . ? C15 C14 H14B 109.1 . . ? C13 C14 H14B 109.1 . . ? H14A C14 H14B 107.8 . . ? O3 C15 C16 109.2(4) . . ? O3 C15 C14 109.9(4) . . ? C16 C15 C14 110.7(4) . . ? O3 C15 H15 109.0 . . ? C16 C15 H15 109.0 . . ? C14 C15 H15 109.0 . . ? C15 C16 C11 113.2(4) . . ? C15 C16 H16A 108.9 . . ? C11 C16 H16A 108.9 . . ? C15 C16 H16B 108.9 . . ? C11 C16 H16B 108.9 . . ? H16A C16 H16B 107.8 . . ? O4 C17 C18 110.7(4) . . ? O4 C17 C22 107.6(4) . . ? C18 C17 C22 111.1(4) . . ? O4 C17 H17 109.1 . . ? C18 C17 H17 109.1 . . ? C22 C17 H17 109.1 . . ? C19 C18 C17 114.0(4) . . ? C19 C18 H18A 108.7 . . ? C17 C18 H18A 108.7 . . ? C19 C18 H18B 108.7 . . ? C17 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? O5 C19 C18 109.6(4) . . ? O5 C19 C20 110.1(4) . . ? C18 C19 C20 110.7(4) . . ? O5 C19 H19 108.8 . . ? C18 C19 H19 108.8 . . ? C20 C19 H19 108.8 . . ? C21 C20 C19 112.7(4) . . ? C21 C20 H20A 109.1 . . ? C19 C20 H20A 109.1 . . ? C21 C20 H20B 109.1 . . ? C19 C20 H20B 109.1 . . ? H20A C20 H20B 107.8 . . ? O6 C21 C20 109.7(4) . . ? O6 C21 C22 111.2(4) . . ? C20 C21 C22 110.7(5) . . ? O6 C21 H21 108.4 . . ? C20 C21 H21 108.4 . . ? C22 C21 H21 108.4 . . ? C17 C22 C21 111.9(4) . . ? C17 C22 H22A 109.2 . . ? C21 C22 H22A 109.2 . . ? C17 C22 H22B 109.2 . . ? C21 C22 H22B 109.2 . . ? H22A C22 H22B 107.9 . . ? O9 C23 O8 125.0(5) . . ? O9 C23 C24 118.1(5) . . ? O8 C23 C24 116.9(4) . . ? C25 C24 C29 118.7(6) . . ? C25 C24 C23 121.1(5) . . ? C29 C24 C23 120.1(5) . . ? C26 C25 C24 120.1(6) . . ? C26 C25 H25 120.0 . . ? C24 C25 H25 120.0 . . ? C25 C26 C27 119.8(7) . . ? C25 C26 H26 120.1 . . ? C27 C26 H26 120.1 . . ? C28 C27 C26 121.6(7) . . ? C28 C27 H27 119.2 . . ? C26 C27 H27 119.2 . . ? C27 C28 C29 118.2(8) . . ? C27 C28 H28 120.9 . . ? C29 C28 H28 120.9 . . ? C28 C29 C24 121.5(6) . . ? C28 C29 H29 119.2 . . ? C24 C29 H29 119.2 . . ? O11 C30 O12 126.5(4) . 2_677 ? O11 C30 C31 117.0(4) . . ? O12 C30 C31 116.5(5) 2_677 . ? C36 C31 C32 119.4(5) . . ? C36 C31 C30 121.0(4) . . ? C32 C31 C30 119.5(5) . . ? C33 C32 C31 119.7(5) . . ? C33 C32 H32 120.1 . . ? C31 C32 H32 120.1 . . ? C32 C33 C34 120.8(5) . . ? C32 C33 H33 119.6 . . ? C34 C33 H33 119.6 . . ? C33 C34 C35 119.9(5) . . ? C33 C34 H34 120.0 . . ? C35 C34 H34 120.0 . . ? C36 C35 C34 119.4(6) . . ? C36 C35 H35 120.3 . . ? C34 C35 H35 120.3 . . ? C35 C36 C31 120.7(5) . . ? C35 C36 H36 119.6 . . ? C31 C36 H36 119.6 . . ? O10 C37 O13 125.8(5) 2_677 . ? O10 C37 C38 115.8(5) 2_677 . ? O13 C37 C38 118.4(5) . . ? C43 C38 C39 121.0(6) . . ? C43 C38 C37 119.5(5) . . ? C39 C38 C37 119.5(6) . . ? C38 C39 C40 118.9(6) . . ? C38 C39 H39 120.5 . . ? C40 C39 H39 120.5 . . ? C41 C40 C39 119.9(7) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C42 C41 C40 120.3(7) . . ? C42 C41 H41 119.8 . . ? C40 C41 H41 119.8 . . ? C41 C42 C43 119.7(7) . . ? C41 C42 H42 120.2 . . ? C43 C42 H42 120.2 . . ? C38 C43 C42 120.0(7) . . ? C38 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? O4' V1' O8' 93.32(14) . . ? O4' V1' O1' 77.67(12) . . ? O8' V1' O1' 99.31(14) . . ? O4' V1' N1' 87.66(14) . . ? O8' V1' N1' 167.02(15) . . ? O1' V1' N1' 93.55(15) . . ? O4' V1' N2' 98.11(14) . . ? O8' V1' N2' 90.64(15) . . ? O1' V1' N2' 169.36(15) . . ? N1' V1' N2' 76.41(15) . . ? O4' V1' Cl1' 170.80(10) . . ? O8' V1' Cl1' 91.94(10) . . ? O1' V1' Cl1' 94.03(9) . . ? N1' V1' Cl1' 88.92(11) . . ? N2' V1' Cl1' 89.37(11) . . ? O4' V1' V3' 39.65(9) . . ? O8' V1' V3' 95.79(10) . . ? O1' V1' V3' 38.14(8) . . ? N1' V1' V3' 93.22(11) . . ? N2' V1' V3' 137.45(11) . . ? Cl1' V1' V3' 132.17(5) . . ? O2' V2' O7' 86.92(15) . 2_766 ? O2' V2' O5' 77.17(13) . . ? O7' V2' O5' 91.20(13) 2_766 . ? O2' V2' O10' 169.95(14) . . ? O7' V2' O10' 86.87(13) 2_766 . ? O5' V2' O10' 95.08(14) . . ? O2' V2' O11' 95.29(14) . . ? O7' V2' O11' 89.94(13) 2_766 . ? O5' V2' O11' 172.30(13) . . ? O10' V2' O11' 92.59(14) . . ? O2' V2' Cl2' 96.05(12) . . ? O7' V2' Cl2' 176.24(10) 2_766 . ? O5' V2' Cl2' 91.71(10) . . ? O10' V2' Cl2' 90.51(10) . . ? O11' V2' Cl2' 87.49(10) . . ? O2' V2' V3' 40.04(10) . . ? O7' V2' V3' 78.27(9) 2_766 . ? O5' V2' V3' 39.54(9) . . ? O10' V2' V3' 130.62(11) . . ? O11' V2' V3' 133.58(10) . . ? Cl2' V2' V3' 105.49(5) . . ? O1' V3' O5' 127.78(14) . . ? O1' V3' O2' 87.44(14) . . ? O5' V3' O2' 76.77(13) . . ? O1' V3' O3' 87.78(14) . . ? O5' V3' O3' 138.51(15) . . ? O2' V3' O3' 85.53(15) . . ? O1' V3' O6' 139.17(14) . . ? O5' V3' O6' 87.14(13) . . ? O2' V3' O6' 125.02(15) . . ? O3' V3' O6' 72.79(12) . . ? O1' V3' O4' 75.96(12) . . ? O5' V3' O4' 89.05(13) . . ? O2' V3' O4' 144.73(15) . . ? O3' V3' O4' 123.86(14) . . ? O6' V3' O4' 85.51(13) . . ? O1' V3' V2' 119.27(10) . . ? O5' V3' V2' 40.31(9) . . ? O2' V3' V2' 38.85(9) . . ? O3' V3' V2' 107.52(11) . . ? O6' V3' V2' 100.96(10) . . ? O4' V3' V2' 127.47(9) . . ? O1' V3' V4' 106.88(11) . . ? O5' V3' V4' 124.61(9) . . ? O2' V3' V4' 117.96(12) . . ? O3' V3' V4' 37.63(9) . . ? O6' V3' V4' 39.13(9) . . ? O4' V3' V4' 96.75(9) . . ? V2' V3' V4' 120.90(3) . . ? O1' V3' V1' 39.13(9) . . ? O5' V3' V1' 113.52(9) . . ? O2' V3' V1' 121.57(11) . . ? O3' V3' V1' 107.76(11) . . ? O6' V3' V1' 113.13(10) . . ? O4' V3' V1' 36.94(8) . . ? V2' V3' V1' 136.54(3) . . ? V4' V3' V1' 102.55(3) . . ? O3' V4' O7' 95.48(14) . . ? O3' V4' O6' 75.97(13) . . ? O7' V4' O6' 91.24(13) . . ? O3' V4' O12' 169.06(14) . . ? O7' V4' O12' 91.21(13) . . ? O6' V4' O12' 95.28(13) . . ? O3' V4' O13' 95.43(15) . . ? O7' V4' O13' 89.16(13) . . ? O6' V4' O13' 171.39(14) . . ? O12' V4' O13' 93.31(14) . . ? O3' V4' O9' 90.35(16) . . ? O7' V4' O9' 173.07(14) . . ? O6' V4' O9' 93.81(14) . . ? O12' V4' O9' 83.60(15) . . ? O13' V4' O9' 86.56(14) . . ? O3' V4' V3' 39.92(10) . . ? O7' V4' V3' 108.18(9) . . ? O6' V4' V3' 40.27(9) . . ? O12' V4' V3' 129.47(10) . . ? O13' V4' V3' 131.79(10) . . ? O9' V4' V3' 78.72(10) . . ? C11' O1' V3' 122.5(3) . . ? C11' O1' V1' 132.2(3) . . ? V3' O1' V1' 102.73(14) . . ? C13' O2' V2' 135.3(3) . . ? C13' O2' V3' 122.5(3) . . ? V2' O2' V3' 101.11(15) . . ? C15' O3' V4' 132.9(3) . . ? C15' O3' V3' 121.8(3) . . ? V4' O3' V3' 102.45(14) . . ? C17' O4' V1' 134.7(3) . . ? C17' O4' V3' 121.4(3) . . ? V1' O4' V3' 103.41(13) . . ? C19' O5' V3' 122.0(3) . . ? C19' O5' V2' 131.3(3) . . ? V3' O5' V2' 100.16(13) . . ? C21' O6' V4' 129.8(3) . . ? C21' O6' V3' 121.6(3) . . ? V4' O6' V3' 100.60(13) . . ? V4' O7' V2' 127.23(16) . 2_766 ? C23' O8' V1' 140.6(3) . . ? C23' O9' V4' 173.3(4) . . ? C30' O10' V2' 135.7(3) . . ? C37' O11' V2' 135.5(3) . . ? C37' O12' V4' 135.0(3) 2_766 . ? C30' O13' V4' 134.3(3) 2_766 . ? C5' N1' C1' 118.7(4) . . ? C5' N1' V1' 124.7(3) . . ? C1' N1' V1' 116.5(3) . . ? C10' N2' C6' 118.9(4) . . ? C10' N2' V1' 124.9(4) . . ? C6' N2' V1' 115.7(3) . . ? N1' C1' C2' 121.4(5) . . ? N1' C1' C6' 115.3(4) . . ? C2' C1' C6' 123.3(5) . . ? C3' C2' C1' 119.4(5) . . ? C3' C2' H2' 120.3 . . ? C1' C2' H2' 120.3 . . ? C2' C3' C4' 119.1(5) . . ? C2' C3' H3' 120.5 . . ? C4' C3' H3' 120.5 . . ? C3' C4' C5' 119.4(5) . . ? C3' C4' H4' 120.3 . . ? C5' C4' H4' 120.3 . . ? N1' C5' C4' 122.0(5) . . ? N1' C5' H5' 119.0 . . ? C4' C5' H5' 119.0 . . ? N2' C6' C7' 120.5(5) . . ? N2' C6' C1' 115.6(4) . . ? C7' C6' C1' 123.9(5) . . ? C8' C7' C6' 119.9(6) . . ? C8' C7' H7' 120.0 . . ? C6' C7' H7' 120.0 . . ? C7' C8' C9' 119.0(5) . . ? C7' C8' H8' 120.5 . . ? C9' C8' H8' 120.5 . . ? C10' C9' C8' 118.9(6) . . ? C10' C9' H9' 120.5 . . ? C8' C9' H9' 120.5 . . ? N2' C10' C9' 122.7(6) . . ? N2' C10' H10' 118.6 . . ? C9' C10' H10' 118.6 . . ? O1' C11' C16' 110.8(4) . . ? O1' C11' C12' 109.7(4) . . ? C16' C11' C12' 110.8(4) . . ? O1' C11' H11' 108.5 . . ? C16' C11' H11' 108.5 . . ? C12' C11' H11' 108.5 . . ? C11' C12' C13' 111.6(4) . . ? C11' C12' H12C 109.3 . . ? C13' C12' H12C 109.3 . . ? C11' C12' H12D 109.3 . . ? C13' C12' H12D 109.3 . . ? H12C C12' H12D 108.0 . . ? O2' C13' C14' 110.2(4) . . ? O2' C13' C12' 108.6(4) . . ? C14' C13' C12' 110.7(4) . . ? O2' C13' H13' 109.1 . . ? C14' C13' H13' 109.1 . . ? C12' C13' H13' 109.1 . . ? C13' C14' C15' 112.4(4) . . ? C13' C14' H14C 109.1 . . ? C15' C14' H14C 109.1 . . ? C13' C14' H14D 109.1 . . ? C15' C14' H14D 109.1 . . ? H14C C14' H14D 107.8 . . ? O3' C15' C16' 110.2(4) . . ? O3' C15' C14' 108.6(4) . . ? C16' C15' C14' 111.8(4) . . ? O3' C15' H15' 108.7 . . ? C16' C15' H15' 108.7 . . ? C14' C15' H15' 108.7 . . ? C11' C16' C15' 112.8(4) . . ? C11' C16' H16C 109.0 . . ? C15' C16' H16C 109.0 . . ? C11' C16' H16D 109.0 . . ? C15' C16' H16D 109.0 . . ? H16C C16' H16D 107.8 . . ? O4' C17' C18' 109.7(4) . . ? O4' C17' C22' 108.7(4) . . ? C18' C17' C22' 111.0(4) . . ? O4' C17' H17' 109.2 . . ? C18' C17' H17' 109.2 . . ? C22' C17' H17' 109.2 . . ? C17' C18' C19' 113.4(4) . . ? C17' C18' H18C 108.9 . . ? C19' C18' H18C 108.9 . . ? C17' C18' H18D 108.9 . . ? C19' C18' H18D 108.9 . . ? H18C C18' H18D 107.7 . . ? O5' C19' C18' 109.1(4) . . ? O5' C19' C20' 110.6(4) . . ? C18' C19' C20' 110.9(4) . . ? O5' C19' H19' 108.7 . . ? C18' C19' H19' 108.7 . . ? C20' C19' H19' 108.7 . . ? C21' C20' C19' 111.9(4) . . ? C21' C20' H20C 109.2 . . ? C19' C20' H20C 109.2 . . ? C21' C20' H20D 109.2 . . ? C19' C20' H20D 109.2 . . ? H20C C20' H20D 107.9 . . ? O6' C21' C20' 109.4(4) . . ? O6' C21' C22' 111.0(4) . . ? C20' C21' C22' 111.3(4) . . ? O6' C21' H21' 108.3 . . ? C20' C21' H21' 108.3 . . ? C22' C21' H21' 108.3 . . ? C21' C22' C17' 112.3(4) . . ? C21' C22' H22C 109.1 . . ? C17' C22' H22C 109.1 . . ? C21' C22' H22D 109.1 . . ? C17' C22' H22D 109.1 . . ? H22C C22' H22D 107.9 . . ? O9' C23' O8' 124.0(4) . . ? O9' C23' C24' 120.1(5) . . ? O8' C23' C24' 115.9(4) . . ? C29' C24' C25' 120.1(5) . . ? C29' C24' C23' 119.9(5) . . ? C25' C24' C23' 119.9(5) . . ? C24' C25' C26' 120.2(6) . . ? C24' C25' H25' 119.9 . . ? C26' C25' H25' 119.9 . . ? C27' C26' C25' 119.2(7) . . ? C27' C26' H26' 120.4 . . ? C25' C26' H26' 120.4 . . ? C26' C27' C28' 121.3(7) . . ? C26' C27' H27' 119.4 . . ? C28' C27' H27' 119.4 . . ? C27' C28' C29' 119.8(7) . . ? C27' C28' H28' 120.1 . . ? C29' C28' H28' 120.1 . . ? C24' C29' C28' 119.4(7) . . ? C24' C29' H29' 120.3 . . ? C28' C29' H29' 120.3 . . ? O13' C30' O10' 126.4(4) 2_766 . ? O13' C30' C31W 114.9(4) 2_766 . ? O10' C30' C31W 118.7(4) . . ? O13' C30' C31V 120.3(4) 2_766 . ? O10' C30' C31V 113.2(4) . . ? C31W C30' C31V 7.5 . . ? C32V C31V C36V 120.0 . . ? C32V C31V C30' 118.6(3) . . ? C36V C31V C30' 121.3(3) . . ? C31V C32V C33V 120.0 . . ? C31V C32V H32V 120.0 . . ? C33V C32V H32V 120.0 . . ? C32V C33V C34V 120.0 . . ? C32V C33V H33V 120.0 . . ? C34V C33V H33V 120.0 . . ? C33V C34V C35V 120.0 . . ? C33V C34V H34V 120.0 . . ? C35V C34V H34V 120.0 . . ? C36V C35V C34V 120.0 . . ? C36V C35V H35V 120.0 . . ? C34V C35V H35V 120.0 . . ? C35V C36V C31V 120.0 . . ? C35V C36V H36V 120.0 . . ? C31V C36V H36V 120.0 . . ? C36W C31W C32W 120.0 . . ? C36W C31W C30' 118.1(3) . . ? C32W C31W C30' 121.9(3) . . ? C33W C32W C31W 120.0 . . ? C33W C32W H32W 120.0 . . ? C31W C32W H32W 120.0 . . ? C34W C33W C32W 120.0 . . ? C34W C33W H33W 120.0 . . ? C32W C33W H33W 120.0 . . ? C33W C34W C35W 120.0 . . ? C33W C34W H34W 120.0 . . ? C35W C34W H34W 120.0 . . ? C36W C35W C34W 120.0 . . ? C36W C35W H35W 120.0 . . ? C34W C35W H35W 120.0 . . ? C35W C36W C31W 120.0 . . ? C35W C36W H36W 120.0 . . ? C31W C36W H36W 120.0 . . ? O12' C37' O11' 125.9(5) 2_766 . ? O12' C37' C38' 115.7(5) 2_766 . ? O11' C37' C38' 118.4(5) . . ? C43' C38' C39' 118.2(5) . . ? C43' C38' C37' 120.7(6) . . ? C39' C38' C37' 121.0(5) . . ? C38' C39' C40' 121.7(6) . . ? C38' C39' H39' 119.1 . . ? C40' C39' H39' 119.1 . . ? C41' C40' C39' 121.1(7) . . ? C41' C40' H40' 119.4 . . ? C39' C40' H40' 119.4 . . ? C40' C41' C42' 119.2(6) . . ? C40' C41' H41' 120.4 . . ? C42' C41' H41' 120.4 . . ? C41' C42' C43' 119.8(7) . . ? C41' C42' H42' 120.1 . . ? C43' C42' H42' 120.1 . . ? C38' C43' C42' 120.0(7) . . ? C38' C43' H43' 120.0 . . ? C42' C43' H43' 120.0 . . ? N3 C44 C45 162.2(16) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N4 C46 C47 175.7(13) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N5X C48X C49X 170(3) . . ? C48X C49X H49A 109.5 . . ? C48X C49X H49B 109.5 . . ? H49A C49X H49B 109.5 . . ? C48X C49X H49C 109.5 . . ? H49A C49X H49C 109.5 . . ? H49B C49X H49C 109.5 . . ? N5Y C48Y C49Y 172(5) . . ? C48Y C49Y H49D 109.5 . . ? C48Y C49Y H49E 109.5 . . ? H49D C49Y H49E 109.5 . . ? C48Y C49Y H49F 109.5 . . ? H49D C49Y H49F 109.5 . . ? H49E C49Y H49F 109.5 . . ? N5Z C48Z C49Z 172.9(18) . . ? C48Z C49Z H49G 109.5 . . ? C48Z C49Z H49H 109.5 . . ? H49G C49Z H49H 109.5 . . ? C48Z C49Z H49I 109.5 . . ? H49G C49Z H49I 109.5 . . ? H49H C49Z H49I 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 V2 V3 O1 -50.58(19) . . . . ? O5 V2 V3 O1 109.41(18) . . . . ? O7 V2 V3 O1 -144.89(15) 2_677 . . . ? O10 V2 V3 O1 140.31(18) . . . . ? O11 V2 V3 O1 -66.27(17) . . . . ? Cl2 V2 V3 O1 33.18(12) . . . . ? O5 V2 V3 O2 160.0(2) . . . . ? O7 V2 V3 O2 -94.31(18) 2_677 . . . ? O10 V2 V3 O2 -169.1(2) . . . . ? O11 V2 V3 O2 -15.7(2) . . . . ? Cl2 V2 V3 O2 83.77(16) . . . . ? O2 V2 V3 O5 -160.0(2) . . . . ? O7 V2 V3 O5 105.70(18) 2_677 . . . ? O10 V2 V3 O5 30.9(2) . . . . ? O11 V2 V3 O5 -175.7(2) . . . . ? Cl2 V2 V3 O5 -76.23(15) . . . . ? O2 V2 V3 O6 126.21(19) . . . . ? O5 V2 V3 O6 -73.80(18) . . . . ? O7 V2 V3 O6 31.89(14) 2_677 . . . ? O10 V2 V3 O6 -42.90(18) . . . . ? O11 V2 V3 O6 110.52(16) . . . . ? Cl2 V2 V3 O6 -150.03(11) . . . . ? O2 V2 V3 O3 48.32(18) . . . . ? O5 V2 V3 O3 -151.69(18) . . . . ? O7 V2 V3 O3 -46.00(14) 2_677 . . . ? O10 V2 V3 O3 -120.79(17) . . . . ? O11 V2 V3 O3 32.63(17) . . . . ? Cl2 V2 V3 O3 132.08(11) . . . . ? O2 V2 V3 O4 -141.68(19) . . . . ? O5 V2 V3 O4 18.31(18) . . . . ? O7 V2 V3 O4 124.00(15) 2_677 . . . ? O10 V2 V3 O4 49.21(19) . . . . ? O11 V2 V3 O4 -157.37(17) . . . . ? Cl2 V2 V3 O4 -57.92(13) . . . . ? O2 V2 V3 V4 89.96(16) . . . . ? O5 V2 V3 V4 -110.05(15) . . . . ? O7 V2 V3 V4 -4.36(10) 2_677 . . . ? O10 V2 V3 V4 -79.15(15) . . . . ? O11 V2 V3 V4 74.27(13) . . . . ? Cl2 V2 V3 V4 173.72(5) . . . . ? O2 V2 V3 V1 -93.60(16) . . . . ? O5 V2 V3 V1 66.39(15) . . . . ? O7 V2 V3 V1 172.09(10) 2_677 . . . ? O10 V2 V3 V1 97.29(15) . . . . ? O11 V2 V3 V1 -109.29(13) . . . . ? Cl2 V2 V3 V1 -9.83(7) . . . . ? O4 V1 V3 O1 -172.9(2) . . . . ? O8 V1 V3 O1 96.75(19) . . . . ? N2 V1 V3 O1 -164.2(3) . . . . ? N1 V1 V3 O1 -91.3(2) . . . . ? Cl1 V1 V3 O1 -1.28(16) . . . . ? O4 V1 V3 O2 -146.2(2) . . . . ? O1 V1 V3 O2 26.6(2) . . . . ? O8 V1 V3 O2 123.39(16) . . . . ? N2 V1 V3 O2 -137.6(2) . . . . ? N1 V1 V3 O2 -64.65(17) . . . . ? Cl1 V1 V3 O2 25.35(14) . . . . ? O4 V1 V3 O5 -57.43(18) . . . . ? O1 V1 V3 O5 115.43(19) . . . . ? O8 V1 V3 O5 -147.83(14) . . . . ? N2 V1 V3 O5 -48.8(2) . . . . ? N1 V1 V3 O5 24.14(16) . . . . ? Cl1 V1 V3 O5 114.14(12) . . . . ? O4 V1 V3 O6 40.67(19) . . . . ? O1 V1 V3 O6 -146.47(19) . . . . ? O8 V1 V3 O6 -49.73(15) . . . . ? N2 V1 V3 O6 49.3(2) . . . . ? N1 V1 V3 O6 122.24(16) . . . . ? Cl1 V1 V3 O6 -147.76(12) . . . . ? O4 V1 V3 O3 119.19(18) . . . . ? O1 V1 V3 O3 -67.96(18) . . . . ? O8 V1 V3 O3 28.79(14) . . . . ? N2 V1 V3 O3 127.8(2) . . . . ? N1 V1 V3 O3 -159.25(15) . . . . ? Cl1 V1 V3 O3 -69.24(11) . . . . ? O1 V1 V3 O4 172.9(2) . . . . ? O8 V1 V3 O4 -90.40(18) . . . . ? N2 V1 V3 O4 8.7(2) . . . . ? N1 V1 V3 O4 81.6(2) . . . . ? Cl1 V1 V3 O4 171.57(17) . . . . ? O4 V1 V3 V2 -96.05(16) . . . . ? O1 V1 V3 V2 76.81(16) . . . . ? O8 V1 V3 V2 173.56(10) . . . . ? N2 V1 V3 V2 -87.4(2) . . . . ? N1 V1 V3 V2 -14.48(13) . . . . ? Cl1 V1 V3 V2 75.53(8) . . . . ? O4 V1 V3 V4 80.96(16) . . . . ? O1 V1 V3 V4 -106.19(16) . . . . ? O8 V1 V3 V4 -9.44(10) . . . . ? N2 V1 V3 V4 89.6(2) . . . . ? N1 V1 V3 V4 162.53(12) . . . . ? Cl1 V1 V3 V4 -107.47(6) . . . . ? O1 V3 V4 O3 56.93(19) . . . . ? O2 V3 V4 O3 -41.20(19) . . . . ? O5 V3 V4 O3 -135.3(2) . . . . ? O6 V3 V4 O3 -149.9(2) . . . . ? O4 V3 V4 O3 132.82(18) . . . . ? V2 V3 V4 O3 -85.91(16) . . . . ? V1 V3 V4 O3 96.68(16) . . . . ? O1 V3 V4 O7 142.02(14) . . . . ? O2 V3 V4 O7 43.90(15) . . . . ? O5 V3 V4 O7 -50.16(17) . . . . ? O6 V3 V4 O7 -64.79(17) . . . . ? O3 V3 V4 O7 85.10(19) . . . . ? O4 V3 V4 O7 -142.08(14) . . . . ? V2 V3 V4 O7 -0.82(11) . . . . ? V1 V3 V4 O7 -178.22(11) . . . . ? O1 V3 V4 O12 -116.13(16) . . . . ? O2 V3 V4 O12 145.74(16) . . . . ? O5 V3 V4 O12 51.69(18) . . . . ? O6 V3 V4 O12 37.06(18) . . . . ? O3 V3 V4 O12 -173.1(2) . . . . ? O4 V3 V4 O12 -40.23(16) . . . . ? V2 V3 V4 O12 101.03(13) . . . . ? V1 V3 V4 O12 -76.37(13) . . . . ? O1 V3 V4 O6 -153.18(17) . . . . ? O2 V3 V4 O6 108.69(18) . . . . ? O5 V3 V4 O6 14.63(19) . . . . ? O3 V3 V4 O6 149.9(2) . . . . ? O4 V3 V4 O6 -77.29(17) . . . . ? V2 V3 V4 O6 63.97(14) . . . . ? V1 V3 V4 O6 -113.43(14) . . . . ? O1 V3 V4 O9 -42.33(15) . . . . ? O2 V3 V4 O9 -140.46(15) . . . . ? O5 V3 V4 O9 125.48(17) . . . . ? O6 V3 V4 O9 110.85(18) . . . . ? O3 V3 V4 O9 -99.26(19) . . . . ? O4 V3 V4 O9 33.56(14) . . . . ? V2 V3 V4 O9 174.83(11) . . . . ? V1 V3 V4 O9 -2.57(11) . . . . ? O1 V3 V4 O13 37.15(18) . . . . ? O2 V3 V4 O13 -60.97(19) . . . . ? O5 V3 V4 O13 -155.03(19) . . . . ? O6 V3 V4 O13 -169.7(2) . . . . ? O3 V3 V4 O13 -19.8(2) . . . . ? O4 V3 V4 O13 113.05(18) . . . . ? V2 V3 V4 O13 -105.69(15) . . . . ? V1 V3 V4 O13 76.91(15) . . . . ? O2 V3 O1 C11 42.0(3) . . . . ? O5 V3 O1 C11 116.3(3) . . . . ? O6 V3 O1 C11 -103.5(4) . . . . ? O3 V3 O1 C11 -44.4(3) . . . . ? O4 V3 O1 C11 -164.0(3) . . . . ? V2 V3 O1 C11 71.3(3) . . . . ? V4 V3 O1 C11 -75.0(3) . . . . ? V1 V3 O1 C11 -159.6(4) . . . . ? O2 V3 O1 V1 -158.34(16) . . . . ? O5 V3 O1 V1 -84.02(18) . . . . ? O6 V3 O1 V1 56.1(3) . . . . ? O3 V3 O1 V1 115.28(15) . . . . ? O4 V3 O1 V1 -4.39(14) . . . . ? V2 V3 O1 V1 -129.05(10) . . . . ? V4 V3 O1 V1 84.67(13) . . . . ? O4 V1 O1 C11 161.4(4) . . . . ? O8 V1 O1 C11 68.3(4) . . . . ? N2 V1 O1 C11 -135.6(7) . . . . ? N1 V1 O1 C11 -112.6(4) . . . . ? Cl1 V1 O1 C11 -24.3(4) . . . . ? V3 V1 O1 C11 156.7(5) . . . . ? O4 V1 O1 V3 4.70(15) . . . . ? O8 V1 O1 V3 -88.40(16) . . . . ? N2 V1 O1 V3 67.7(8) . . . . ? N1 V1 O1 V3 90.76(17) . . . . ? Cl1 V1 O1 V3 179.04(12) . . . . ? O1 V3 O2 C13 -41.2(3) . . . . ? O5 V3 O2 C13 -164.4(3) . . . . ? O6 V3 O2 C13 115.0(3) . . . . ? O3 V3 O2 C13 45.7(3) . . . . ? O4 V3 O2 C13 -98.8(4) . . . . ? V2 V3 O2 C13 -177.3(4) . . . . ? V4 V3 O2 C13 69.3(3) . . . . ? V1 V3 O2 C13 -57.6(4) . . . . ? O1 V3 O2 V2 136.02(16) . . . . ? O5 V3 O2 V2 12.90(14) . . . . ? O6 V3 O2 V2 -67.8(2) . . . . ? O3 V3 O2 V2 -137.02(15) . . . . ? O4 V3 O2 V2 78.5(3) . . . . ? V4 V3 O2 V2 -113.40(12) . . . . ? V1 V3 O2 V2 119.62(11) . . . . ? O5 V2 O2 C13 163.9(4) . . . . ? O7 V2 O2 C13 -103.0(4) 2_677 . . . ? O10 V2 O2 C13 -142.2(6) . . . . ? O11 V2 O2 C13 -15.0(4) . . . . ? Cl2 V2 O2 C13 73.0(4) . . . . ? V3 V2 O2 C13 176.7(5) . . . . ? O5 V2 O2 V3 -12.85(14) . . . . ? O7 V2 O2 V3 80.29(15) 2_677 . . . ? O10 V2 O2 V3 41.1(7) . . . . ? O11 V2 O2 V3 168.31(15) . . . . ? Cl2 V2 O2 V3 -103.76(13) . . . . ? O7 V4 O3 C15 87.0(4) . . . . ? O12 V4 O3 C15 -146.4(6) . . . . ? O6 V4 O3 C15 170.9(5) . . . . ? O9 V4 O3 C15 -93.4(4) . . . . ? O13 V4 O3 C15 -3.7(5) . . . . ? V3 V4 O3 C15 -170.0(5) . . . . ? O7 V4 O3 V3 -103.08(16) . . . . ? O12 V4 O3 V3 23.6(7) . . . . ? O6 V4 O3 V3 -19.11(14) . . . . ? O9 V4 O3 V3 76.57(16) . . . . ? O13 V4 O3 V3 166.32(15) . . . . ? O1 V3 O3 C15 44.3(3) . . . . ? O2 V3 O3 C15 -44.6(3) . . . . ? O5 V3 O3 C15 -105.5(4) . . . . ? O6 V3 O3 C15 -168.5(4) . . . . ? O4 V3 O3 C15 116.1(3) . . . . ? V2 V3 O3 C15 -72.9(3) . . . . ? V4 V3 O3 C15 171.8(4) . . . . ? V1 V3 O3 C15 80.1(3) . . . . ? O1 V3 O3 V4 -127.49(16) . . . . ? O2 V3 O3 V4 143.56(16) . . . . ? O5 V3 O3 V4 82.6(3) . . . . ? O6 V3 O3 V4 19.63(14) . . . . ? O4 V3 O3 V4 -55.75(19) . . . . ? V2 V3 O3 V4 115.27(12) . . . . ? V1 V3 O3 V4 -91.72(13) . . . . ? O1 V1 O4 C17 160.2(4) . . . . ? O8 V1 O4 C17 -101.8(4) . . . . ? N2 V1 O4 C17 -9.3(4) . . . . ? N1 V1 O4 C17 66.4(4) . . . . ? Cl1 V1 O4 C17 124.7(6) . . . . ? V3 V1 O4 C17 164.7(5) . . . . ? O1 V1 O4 V3 -4.51(14) . . . . ? O8 V1 O4 V3 93.55(15) . . . . ? N2 V1 O4 V3 -173.98(17) . . . . ? N1 V1 O4 V3 -98.30(17) . . . . ? Cl1 V1 O4 V3 -40.0(7) . . . . ? O1 V3 O4 C17 -162.7(4) . . . . ? O2 V3 O4 C17 -102.1(4) . . . . ? O5 V3 O4 C17 -39.4(3) . . . . ? O6 V3 O4 C17 49.4(3) . . . . ? O3 V3 O4 C17 118.8(3) . . . . ? V2 V3 O4 C17 -50.9(4) . . . . ? V4 V3 O4 C17 88.6(3) . . . . ? V1 V3 O4 C17 -167.4(4) . . . . ? O1 V3 O4 V1 4.64(14) . . . . ? O2 V3 O4 V1 65.3(3) . . . . ? O5 V3 O4 V1 128.01(16) . . . . ? O6 V3 O4 V1 -143.20(16) . . . . ? O3 V3 O4 V1 -73.83(18) . . . . ? V2 V3 O4 V1 116.47(12) . . . . ? V4 V3 O4 V1 -104.00(13) . . . . ? O1 V3 O5 C19 114.8(3) . . . . ? O2 V3 O5 C19 -164.7(3) . . . . ? O6 V3 O5 C19 -42.3(3) . . . . ? O3 V3 O5 C19 -101.4(4) . . . . ? O4 V3 O5 C19 42.6(3) . . . . ? V2 V3 O5 C19 -151.9(4) . . . . ? V4 V3 O5 C19 -51.6(4) . . . . ? V1 V3 O5 C19 72.7(3) . . . . ? O1 V3 O5 V2 -93.32(17) . . . . ? O2 V3 O5 V2 -12.83(14) . . . . ? O6 V3 O5 V2 109.66(15) . . . . ? O3 V3 O5 V2 50.5(3) . . . . ? O4 V3 O5 V2 -165.51(14) . . . . ? V4 V3 O5 V2 100.28(13) . . . . ? V1 V3 O5 V2 -135.37(10) . . . . ? O2 V2 O5 C19 161.1(4) . . . . ? O7 V2 O5 C19 76.7(4) 2_677 . . . ? O10 V2 O5 C19 -8.7(4) . . . . ? O11 V2 O5 C19 168.1(7) . . . . ? Cl2 V2 O5 C19 -102.3(4) . . . . ? V3 V2 O5 C19 148.3(5) . . . . ? O2 V2 O5 V3 12.83(14) . . . . ? O7 V2 O5 V3 -71.52(15) 2_677 . . . ? O10 V2 O5 V3 -156.97(14) . . . . ? O11 V2 O5 V3 19.9(9) . . . . ? Cl2 V2 O5 V3 109.49(12) . . . . ? O1 V3 O6 C21 -104.5(4) . . . . ? O2 V3 O6 C21 117.0(3) . . . . ? O5 V3 O6 C21 42.6(3) . . . . ? O3 V3 O6 C21 -167.3(3) . . . . ? O4 V3 O6 C21 -46.7(3) . . . . ? V2 V3 O6 C21 80.3(3) . . . . ? V4 V3 O6 C21 -148.9(4) . . . . ? V1 V3 O6 C21 -69.6(3) . . . . ? O1 V3 O6 V4 44.5(3) . . . . ? O2 V3 O6 V4 -94.09(17) . . . . ? O5 V3 O6 V4 -168.51(15) . . . . ? O3 V3 O6 V4 -18.42(13) . . . . ? O4 V3 O6 V4 102.23(14) . . . . ? V2 V3 O6 V4 -130.80(10) . . . . ? V1 V3 O6 V4 79.28(13) . . . . ? O3 V4 O6 C21 165.5(4) . . . . ? O7 V4 O6 C21 -95.5(4) . . . . ? O12 V4 O6 C21 -5.0(4) . . . . ? O9 V4 O6 C21 78.4(4) . . . . ? O13 V4 O6 C21 -153.3(9) . . . . ? V3 V4 O6 C21 146.0(4) . . . . ? O3 V4 O6 V3 19.56(14) . . . . ? O7 V4 O6 V3 118.53(14) . . . . ? O12 V4 O6 V3 -150.93(14) . . . . ? O9 V4 O6 V3 -67.56(15) . . . . ? O13 V4 O6 V3 60.7(10) . . . . ? O3 V4 O7 V2 -145.1(2) . . . 2_677 ? O12 V4 O7 V2 46.1(2) . . . 2_677 ? O6 V4 O7 V2 138.9(2) . . . 2_677 ? O9 V4 O7 V2 38.2(16) . . . 2_677 ? O13 V4 O7 V2 -48.0(2) . . . 2_677 ? V3 V4 O7 V2 174.09(18) . . . 2_677 ? O4 V1 O8 C23 -17.4(5) . . . . ? O1 V1 O8 C23 61.4(5) . . . . ? N2 V1 O8 C23 -113.9(5) . . . . ? N1 V1 O8 C23 -114.6(8) . . . . ? Cl1 V1 O8 C23 155.5(5) . . . . ? V3 V1 O8 C23 22.9(5) . . . . ? O3 V4 O9 C23 37.9(14) . . . . ? O7 V4 O9 C23 -145.3(15) . . . . ? O12 V4 O9 C23 -153.3(14) . . . . ? O6 V4 O9 C23 114.4(14) . . . . ? O13 V4 O9 C23 -59.2(14) . . . . ? V3 V4 O9 C23 77.8(14) . . . . ? O2 V2 O10 C37 67.8(9) . . . 2_677 ? O5 V2 O10 C37 120.2(5) . . . 2_677 ? O7 V2 O10 C37 28.7(5) 2_677 . . 2_677 ? O11 V2 O10 C37 -59.3(5) . . . 2_677 ? Cl2 V2 O10 C37 -147.1(5) . . . 2_677 ? V3 V2 O10 C37 101.1(5) . . . 2_677 ? O2 V2 O11 C30 -90.3(5) . . . . ? O5 V2 O11 C30 -97.1(9) . . . . ? O7 V2 O11 C30 -5.5(5) 2_677 . . . ? O10 V2 O11 C30 79.7(5) . . . . ? Cl2 V2 O11 C30 172.8(5) . . . . ? V3 V2 O11 C30 -80.4(5) . . . . ? O3 V4 O12 C30 -145.4(6) . . . 2_677 ? O7 V4 O12 C30 -18.0(5) . . . 2_677 ? O6 V4 O12 C30 -104.0(5) . . . 2_677 ? O9 V4 O12 C30 161.1(5) . . . 2_677 ? O13 V4 O12 C30 71.7(5) . . . 2_677 ? V3 V4 O12 C30 -126.6(4) . . . 2_677 ? O3 V4 O13 C37 109.8(4) . . . . ? O7 V4 O13 C37 12.1(4) . . . . ? O12 V4 O13 C37 -78.6(4) . . . . ? O6 V4 O13 C37 69.7(11) . . . . ? O9 V4 O13 C37 -161.8(4) . . . . ? V3 V4 O13 C37 122.6(4) . . . . ? O4 V1 N1 C5 84.5(5) . . . . ? O1 V1 N1 C5 6.4(5) . . . . ? O8 V1 N1 C5 -177.6(6) . . . . ? N2 V1 N1 C5 -178.3(5) . . . . ? Cl1 V1 N1 C5 -87.2(4) . . . . ? V3 V1 N1 C5 44.7(4) . . . . ? O4 V1 N1 C1 -90.7(4) . . . . ? O1 V1 N1 C1 -168.7(4) . . . . ? O8 V1 N1 C1 7.2(10) . . . . ? N2 V1 N1 C1 6.5(4) . . . . ? Cl1 V1 N1 C1 97.6(4) . . . . ? V3 V1 N1 C1 -130.5(4) . . . . ? O4 V1 N2 C6 77.9(4) . . . . ? O1 V1 N2 C6 16.5(9) . . . . ? O8 V1 N2 C6 172.9(4) . . . . ? N1 V1 N2 C6 -7.2(4) . . . . ? Cl1 V1 N2 C6 -95.1(4) . . . . ? V3 V1 N2 C6 72.3(4) . . . . ? O4 V1 N2 C10 -101.9(4) . . . . ? O1 V1 N2 C10 -163.2(6) . . . . ? O8 V1 N2 C10 -6.8(4) . . . . ? N1 V1 N2 C10 173.0(4) . . . . ? Cl1 V1 N2 C10 85.1(4) . . . . ? V3 V1 N2 C10 -107.5(4) . . . . ? C5 N1 C1 C2 0.3(9) . . . . ? V1 N1 C1 C2 175.7(6) . . . . ? C5 N1 C1 C6 179.5(5) . . . . ? V1 N1 C1 C6 -5.1(6) . . . . ? N1 C1 C2 C3 0.2(13) . . . . ? C6 C1 C2 C3 -179.0(8) . . . . ? C1 C2 C3 C4 -0.8(15) . . . . ? C2 C3 C4 C5 0.9(15) . . . . ? C1 N1 C5 C4 -0.1(9) . . . . ? V1 N1 C5 C4 -175.2(5) . . . . ? C3 C4 C5 N1 -0.4(12) . . . . ? C10 N2 C6 C7 8.8(8) . . . . ? V1 N2 C6 C7 -170.9(4) . . . . ? C10 N2 C6 C1 -173.3(5) . . . . ? V1 N2 C6 C1 6.9(6) . . . . ? N1 C1 C6 N2 -1.2(7) . . . . ? C2 C1 C6 N2 178.0(6) . . . . ? N1 C1 C6 C7 176.6(6) . . . . ? C2 C1 C6 C7 -4.2(10) . . . . ? N2 C6 C7 C8 -8.3(9) . . . . ? C1 C6 C7 C8 174.0(6) . . . . ? C6 C7 C8 C9 0.9(11) . . . . ? C7 C8 C9 C10 5.6(10) . . . . ? C6 N2 C10 C9 -2.1(8) . . . . ? V1 N2 C10 C9 177.6(4) . . . . ? C8 C9 C10 N2 -5.1(9) . . . . ? V3 O1 C11 C16 62.1(5) . . . . ? V1 O1 C11 C16 -90.9(4) . . . . ? V3 O1 C11 C12 -60.5(4) . . . . ? V1 O1 C11 C12 146.5(3) . . . . ? O1 C11 C12 C13 68.9(5) . . . . ? C16 C11 C12 C13 -52.8(5) . . . . ? V3 O2 C13 C12 59.0(5) . . . . ? V2 O2 C13 C12 -117.2(4) . . . . ? V3 O2 C13 C14 -62.8(5) . . . . ? V2 O2 C13 C14 121.0(4) . . . . ? C11 C12 C13 O2 -67.6(5) . . . . ? C11 C12 C13 C14 53.2(5) . . . . ? O2 C13 C14 C15 66.4(5) . . . . ? C12 C13 C14 C15 -54.5(5) . . . . ? V4 O3 C15 C16 107.9(4) . . . . ? V3 O3 C15 C16 -60.6(5) . . . . ? V4 O3 C15 C14 -130.4(4) . . . . ? V3 O3 C15 C14 61.1(5) . . . . ? C13 C14 C15 O3 -66.7(5) . . . . ? C13 C14 C15 C16 54.1(5) . . . . ? O3 C15 C16 C11 67.4(5) . . . . ? C14 C15 C16 C11 -53.8(5) . . . . ? O1 C11 C16 C15 -67.9(5) . . . . ? C12 C11 C16 C15 53.2(5) . . . . ? V1 O4 C17 C18 -107.3(4) . . . . ? V3 O4 C17 C18 55.3(5) . . . . ? V1 O4 C17 C22 131.1(4) . . . . ? V3 O4 C17 C22 -66.3(4) . . . . ? O4 C17 C18 C19 -67.1(5) . . . . ? C22 C17 C18 C19 52.4(6) . . . . ? V3 O5 C19 C18 -61.9(5) . . . . ? V2 O5 C19 C18 155.1(3) . . . . ? V3 O5 C19 C20 60.1(5) . . . . ? V2 O5 C19 C20 -82.9(5) . . . . ? C17 C18 C19 O5 69.8(5) . . . . ? C17 C18 C19 C20 -51.9(5) . . . . ? O5 C19 C20 C21 -68.0(5) . . . . ? C18 C19 C20 C21 53.4(6) . . . . ? V3 O6 C21 C20 -59.8(5) . . . . ? V4 O6 C21 C20 160.5(3) . . . . ? V3 O6 C21 C22 63.0(5) . . . . ? V4 O6 C21 C22 -76.7(5) . . . . ? C19 C20 C21 O6 67.5(5) . . . . ? C19 C20 C21 C22 -55.6(5) . . . . ? O4 C17 C22 C21 67.9(5) . . . . ? C18 C17 C22 C21 -53.4(6) . . . . ? O6 C21 C22 C17 -66.9(6) . . . . ? C20 C21 C22 C17 55.3(5) . . . . ? V4 O9 C23 O8 -77.7(16) . . . . ? V4 O9 C23 C24 100.7(13) . . . . ? V1 O8 C23 O9 -12.9(8) . . . . ? V1 O8 C23 C24 168.8(4) . . . . ? O9 C23 C24 C25 176.9(6) . . . . ? O8 C23 C24 C25 -4.6(8) . . . . ? O9 C23 C24 C29 -5.5(9) . . . . ? O8 C23 C24 C29 173.0(6) . . . . ? C29 C24 C25 C26 0.6(11) . . . . ? C23 C24 C25 C26 178.2(7) . . . . ? C24 C25 C26 C27 -1.6(13) . . . . ? C25 C26 C27 C28 0.7(16) . . . . ? C26 C27 C28 C29 1.3(16) . . . . ? C27 C28 C29 C24 -2.4(14) . . . . ? C25 C24 C29 C28 1.5(11) . . . . ? C23 C24 C29 C28 -176.1(7) . . . . ? V2 O11 C30 O12 -18.6(8) . . . 2_677 ? V2 O11 C30 C31 159.5(3) . . . . ? O11 C30 C31 C36 -170.7(5) . . . . ? O12 C30 C31 C36 7.6(7) 2_677 . . . ? O11 C30 C31 C32 6.5(7) . . . . ? O12 C30 C31 C32 -175.2(5) 2_677 . . . ? C36 C31 C32 C33 0.1(8) . . . . ? C30 C31 C32 C33 -177.2(5) . . . . ? C31 C32 C33 C34 0.1(10) . . . . ? C32 C33 C34 C35 0.6(11) . . . . ? C33 C34 C35 C36 -1.4(11) . . . . ? C34 C35 C36 C31 1.6(10) . . . . ? C32 C31 C36 C35 -0.9(9) . . . . ? C30 C31 C36 C35 176.3(5) . . . . ? V4 O13 C37 O10 7.0(8) . . . 2_677 ? V4 O13 C37 C38 -173.4(3) . . . . ? O10 C37 C38 C43 -24.0(7) 2_677 . . . ? O13 C37 C38 C43 156.3(5) . . . . ? O10 C37 C38 C39 152.6(5) 2_677 . . . ? O13 C37 C38 C39 -27.1(7) . . . . ? C43 C38 C39 C40 -0.2(9) . . . . ? C37 C38 C39 C40 -176.8(5) . . . . ? C38 C39 C40 C41 -2.7(10) . . . . ? C39 C40 C41 C42 2.5(11) . . . . ? C40 C41 C42 C43 0.5(12) . . . . ? C39 C38 C43 C42 3.3(10) . . . . ? C37 C38 C43 C42 179.8(6) . . . . ? C41 C42 C43 C38 -3.4(11) . . . . ? O2' V2' V3' O1' -39.0(2) . . . . ? O7' V2' V3' O1' -138.28(14) 2_766 . . . ? O5' V2' V3' O1' 115.15(18) . . . . ? O10' V2' V3' O1' 146.29(17) . . . . ? O11' V2' V3' O1' -59.77(18) . . . . ? Cl2' V2' V3' O1' 41.83(12) . . . . ? O2' V2' V3' O5' -154.1(2) . . . . ? O7' V2' V3' O5' 106.57(16) 2_766 . . . ? O10' V2' V3' O5' 31.14(18) . . . . ? O11' V2' V3' O5' -174.92(19) . . . . ? Cl2' V2' V3' O5' -73.32(14) . . . . ? O7' V2' V3' O2' -99.3(2) 2_766 . . . ? O5' V2' V3' O2' 154.1(2) . . . . ? O10' V2' V3' O2' -174.7(2) . . . . ? O11' V2' V3' O2' -20.8(2) . . . . ? Cl2' V2' V3' O2' 80.80(19) . . . . ? O2' V2' V3' O3' 58.5(2) . . . . ? O7' V2' V3' O3' -40.79(13) 2_766 . . . ? O5' V2' V3' O3' -147.36(17) . . . . ? O10' V2' V3' O3' -116.22(16) . . . . ? O11' V2' V3' O3' 37.72(17) . . . . ? Cl2' V2' V3' O3' 139.32(11) . . . . ? O2' V2' V3' O6' 133.7(2) . . . . ? O7' V2' V3' O6' 34.44(13) 2_766 . . . ? O5' V2' V3' O6' -72.13(16) . . . . ? O10' V2' V3' O6' -40.99(16) . . . . ? O11' V2' V3' O6' 112.95(16) . . . . ? Cl2' V2' V3' O6' -145.45(10) . . . . ? O2' V2' V3' O4' -133.5(2) . . . . ? O7' V2' V3' O4' 127.19(14) 2_766 . . . ? O5' V2' V3' O4' 20.62(17) . . . . ? O10' V2' V3' O4' 51.76(17) . . . . ? O11' V2' V3' O4' -154.30(17) . . . . ? Cl2' V2' V3' O4' -52.70(12) . . . . ? O2' V2' V3' V4' 97.35(19) . . . . ? O7' V2' V3' V4' -1.95(9) 2_766 . . . ? O5' V2' V3' V4' -108.52(14) . . . . ? O10' V2' V3' V4' -77.38(13) . . . . ? O11' V2' V3' V4' 76.56(14) . . . . ? Cl2' V2' V3' V4' 178.16(5) . . . . ? O2' V2' V3' V1' -84.44(19) . . . . ? O7' V2' V3' V1' 176.26(10) 2_766 . . . ? O5' V2' V3' V1' 69.68(14) . . . . ? O10' V2' V3' V1' 100.83(13) . . . . ? O11' V2' V3' V1' -105.23(14) . . . . ? Cl2' V2' V3' V1' -3.64(7) . . . . ? O4' V1' V3' O1' -174.1(2) . . . . ? O8' V1' V3' O1' 97.71(19) . . . . ? N1' V1' V3' O1' -91.66(19) . . . . ? N2' V1' V3' O1' -165.0(2) . . . . ? Cl1' V1' V3' O1' -0.20(17) . . . . ? O4' V1' V3' O5' -52.49(18) . . . . ? O8' V1' V3' O5' -140.70(14) . . . . ? O1' V1' V3' O5' 121.59(19) . . . . ? N1' V1' V3' O5' 29.93(14) . . . . ? N2' V1' V3' O5' -43.4(2) . . . . ? Cl1' V1' V3' O5' 121.38(11) . . . . ? O4' V1' V3' O2' -141.02(19) . . . . ? O8' V1' V3' O2' 130.76(16) . . . . ? O1' V1' V3' O2' 33.1(2) . . . . ? N1' V1' V3' O2' -58.60(16) . . . . ? N2' V1' V3' O2' -131.9(2) . . . . ? Cl1' V1' V3' O2' 32.85(14) . . . . ? O4' V1' V3' O3' 123.20(18) . . . . ? O8' V1' V3' O3' 34.98(14) . . . . ? O1' V1' V3' O3' -62.73(19) . . . . ? N1' V1' V3' O3' -154.38(14) . . . . ? N2' V1' V3' O3' 132.28(19) . . . . ? Cl1' V1' V3' O3' -62.93(11) . . . . ? O4' V1' V3' O6' 44.79(18) . . . . ? O8' V1' V3' O6' -43.42(14) . . . . ? O1' V1' V3' O6' -141.13(19) . . . . ? N1' V1' V3' O6' 127.21(14) . . . . ? N2' V1' V3' O6' 53.87(19) . . . . ? Cl1' V1' V3' O6' -141.33(11) . . . . ? O8' V1' V3' O4' -88.21(18) . . . . ? O1' V1' V3' O4' 174.1(2) . . . . ? N1' V1' V3' O4' 82.42(18) . . . . ? N2' V1' V3' O4' 9.1(2) . . . . ? Cl1' V1' V3' O4' 173.87(16) . . . . ? O4' V1' V3' V2' -93.91(15) . . . . ? O8' V1' V3' V2' 177.88(11) . . . . ? O1' V1' V3' V2' 80.17(17) . . . . ? N1' V1' V3' V2' -11.49(11) . . . . ? N2' V1' V3' V2' -84.83(17) . . . . ? Cl1' V1' V3' V2' 79.97(8) . . . . ? O4' V1' V3' V4' 84.51(15) . . . . ? O8' V1' V3' V4' -3.70(11) . . . . ? O1' V1' V3' V4' -101.41(16) . . . . ? N1' V1' V3' V4' 166.93(10) . . . . ? N2' V1' V3' V4' 93.60(17) . . . . ? Cl1' V1' V3' V4' -101.61(6) . . . . ? O1' V3' V4' O3' 62.6(2) . . . . ? O5' V3' V4' O3' -126.5(2) . . . . ? O2' V3' V4' O3' -33.6(2) . . . . ? O6' V3' V4' O3' -145.7(2) . . . . ? O4' V3' V4' O3' 139.9(2) . . . . ? V2' V3' V4' O3' -78.36(18) . . . . ? V1' V3' V4' O3' 102.90(18) . . . . ? O1' V3' V4' O7' 138.99(14) . . . . ? O5' V3' V4' O7' -50.17(15) . . . . ? O2' V3' V4' O7' 42.78(15) . . . . ? O3' V3' V4' O7' 76.4(2) . . . . ? O6' V3' V4' O7' -69.37(18) . . . . ? O4' V3' V4' O7' -143.68(13) . . . . ? V2' V3' V4' O7' -1.99(11) . . . . ? V1' V3' V4' O7' 179.27(10) . . . . ? O1' V3' V4' O6' -151.64(18) . . . . ? O5' V3' V4' O6' 19.19(19) . . . . ? O2' V3' V4' O6' 112.14(19) . . . . ? O3' V3' V4' O6' 145.7(2) . . . . ? O4' V3' V4' O6' -74.32(17) . . . . ? V2' V3' V4' O6' 67.37(15) . . . . ? V1' V3' V4' O6' -111.36(15) . . . . ? O1' V3' V4' O12' -113.60(17) . . . . ? O5' V3' V4' O12' 57.23(18) . . . . ? O2' V3' V4' O12' 150.18(17) . . . . ? O3' V3' V4' O12' -176.2(2) . . . . ? O6' V3' V4' O12' 38.0(2) . . . . ? O4' V3' V4' O12' -36.28(16) . . . . ? V2' V3' V4' O12' 105.41(14) . . . . ? V1' V3' V4' O12' -73.32(14) . . . . ? O1' V3' V4' O13' 33.16(17) . . . . ? O5' V3' V4' O13' -156.01(17) . . . . ? O2' V3' V4' O13' -63.06(18) . . . . ? O3' V3' V4' O13' -29.5(2) . . . . ? O6' V3' V4' O13' -175.2(2) . . . . ? O4' V3' V4' O13' 110.48(16) . . . . ? V2' V3' V4' O13' -107.83(14) . . . . ? V1' V3' V4' O13' 73.44(14) . . . . ? O1' V3' V4' O9' -41.75(15) . . . . ? O5' V3' V4' O9' 129.09(16) . . . . ? O2' V3' V4' O9' -137.96(15) . . . . ? O3' V3' V4' O9' -104.4(2) . . . . ? O6' V3' V4' O9' 109.89(19) . . . . ? O4' V3' V4' O9' 35.57(14) . . . . ? V2' V3' V4' O9' 177.26(11) . . . . ? V1' V3' V4' O9' -1.47(11) . . . . ? O5' V3' O1' C11' 115.2(3) . . . . ? O2' V3' O1' C11' 44.1(4) . . . . ? O3' V3' O1' C11' -41.5(4) . . . . ? O6' V3' O1' C11' -101.7(4) . . . . ? O4' V3' O1' C11' -167.3(4) . . . . ? V2' V3' O1' C11' 67.4(4) . . . . ? V4' V3' O1' C11' -74.4(4) . . . . ? V1' V3' O1' C11' -163.6(4) . . . . ? O5' V3' O1' V1' -81.2(2) . . . . ? O2' V3' O1' V1' -152.28(17) . . . . ? O3' V3' O1' V1' 122.10(16) . . . . ? O6' V3' O1' V1' 62.0(2) . . . . ? O4' V3' O1' V1' -3.67(14) . . . . ? V2' V3' O1' V1' -129.02(10) . . . . ? V4' V3' O1' V1' 89.24(13) . . . . ? O4' V1' O1' C11' 165.1(4) . . . . ? O8' V1' O1' C11' 73.7(4) . . . . ? N1' V1' O1' C11' -108.1(4) . . . . ? N2' V1' O1' C11' -127.3(7) . . . . ? Cl1' V1' O1' C11' -18.9(4) . . . . ? V3' V1' O1' C11' 161.3(5) . . . . ? O4' V1' O1' V3' 3.86(14) . . . . ? O8' V1' O1' V3' -87.52(16) . . . . ? N1' V1' O1' V3' 90.69(16) . . . . ? N2' V1' O1' V3' 71.4(8) . . . . ? Cl1' V1' O1' V3' 179.85(13) . . . . ? O7' V2' O2' C13' -92.1(5) 2_766 . . . ? O5' V2' O2' C13' 176.0(5) . . . . ? O10' V2' O2' C13' -143.9(8) . . . . ? O11' V2' O2' C13' -2.4(5) . . . . ? Cl2' V2' O2' C13' 85.6(5) . . . . ? V3' V2' O2' C13' -167.4(6) . . . . ? O7' V2' O2' V3' 75.39(16) 2_766 . . . ? O5' V2' O2' V3' -16.55(15) . . . . ? O10' V2' O2' V3' 23.5(10) . . . . ? O11' V2' O2' V3' 165.04(16) . . . . ? Cl2' V2' O2' V3' -106.94(15) . . . . ? O1' V3' O2' C13' -43.8(4) . . . . ? O5' V3' O2' C13' -173.6(4) . . . . ? O3' V3' O2' C13' 44.2(4) . . . . ? O6' V3' O2' C13' 109.6(4) . . . . ? O4' V3' O2' C13' -104.8(4) . . . . ? V2' V3' O2' C13' 169.6(5) . . . . ? V4' V3' O2' C13' 64.0(4) . . . . ? V1' V3' O2' C13' -63.9(4) . . . . ? O1' V3' O2' V2' 146.69(18) . . . . ? O5' V3' O2' V2' 16.86(15) . . . . ? O3' V3' O2' V2' -125.34(18) . . . . ? O6' V3' O2' V2' -60.0(2) . . . . ? O4' V3' O2' V2' 85.6(3) . . . . ? V4' V3' O2' V2' -105.54(14) . . . . ? V1' V3' O2' V2' 126.53(12) . . . . ? O7' V4' O3' C15' 87.9(5) . . . . ? O6' V4' O3' C15' 177.8(5) . . . . ? O12' V4' O3' C15' -144.6(7) . . . . ? O13' V4' O3' C15' -1.8(5) . . . . ? O9' V4' O3' C15' -88.3(5) . . . . ? V3' V4' O3' C15' -160.1(6) . . . . ? O7' V4' O3' V3' -111.94(16) . . . . ? O6' V4' O3' V3' -22.03(15) . . . . ? O12' V4' O3' V3' 15.5(9) . . . . ? O13' V4' O3' V3' 158.39(16) . . . . ? O9' V4' O3' V3' 71.80(17) . . . . ? O1' V3' O3' C15' 41.2(4) . . . . ? O5' V3' O3' C15' -110.6(4) . . . . ? O2' V3' O3' C15' -46.4(4) . . . . ? O6' V3' O3' C15' -175.2(4) . . . . ? O4' V3' O3' C15' 112.6(4) . . . . ? V2' V3' O3' C15' -78.8(4) . . . . ? V4' V3' O3' C15' 163.0(5) . . . . ? V1' V3' O3' C15' 75.4(4) . . . . ? O1' V3' O3' V4' -121.75(18) . . . . ? O5' V3' O3' V4' 86.4(2) . . . . ? O2' V3' O3' V4' 150.65(18) . . . . ? O6' V3' O3' V4' 21.83(15) . . . . ? O4' V3' O3' V4' -50.3(2) . . . . ? V2' V3' O3' V4' 118.20(13) . . . . ? V1' V3' O3' V4' -87.60(15) . . . . ? O8' V1' O4' C17' -93.4(4) . . . . ? O1' V1' O4' C17' 167.8(4) . . . . ? N1' V1' O4' C17' 73.6(4) . . . . ? N2' V1' O4' C17' -2.3(4) . . . . ? Cl1' V1' O4' C17' 141.9(6) . . . . ? V3' V1' O4' C17' 171.5(5) . . . . ? O8' V1' O4' V3' 95.07(15) . . . . ? O1' V1' O4' V3' -3.74(14) . . . . ? N1' V1' O4' V3' -97.89(15) . . . . ? N2' V1' O4' V3' -173.81(15) . . . . ? Cl1' V1' O4' V3' -29.6(8) . . . . ? O1' V3' O4' C17' -169.1(3) . . . . ? O5' V3' O4' C17' -39.6(3) . . . . ? O2' V3' O4' C17' -104.8(3) . . . . ? O3' V3' O4' C17' 113.4(3) . . . . ? O6' V3' O4' C17' 47.6(3) . . . . ? V2' V3' O4' C17' -52.8(3) . . . . ? V4' V3' O4' C17' 85.1(3) . . . . ? V1' V3' O4' C17' -173.0(4) . . . . ? O1' V3' O4' V1' 3.85(14) . . . . ? O5' V3' O4' V1' 133.33(15) . . . . ? O2' V3' O4' V1' 68.2(3) . . . . ? O3' V3' O4' V1' -73.68(19) . . . . ? O6' V3' O4' V1' -139.47(15) . . . . ? V2' V3' O4' V1' 120.16(11) . . . . ? V4' V3' O4' V1' -101.92(12) . . . . ? O1' V3' O5' C19' 113.1(3) . . . . ? O2' V3' O5' C19' -170.8(3) . . . . ? O3' V3' O5' C19' -103.5(3) . . . . ? O6' V3' O5' C19' -43.7(3) . . . . ? O4' V3' O5' C19' 41.8(3) . . . . ? V2' V3' O5' C19' -154.4(4) . . . . ? V4' V3' O5' C19' -55.7(3) . . . . ? V1' V3' O5' C19' 70.3(3) . . . . ? O1' V3' O5' V2' -92.43(17) . . . . ? O2' V3' O5' V2' -16.33(15) . . . . ? O3' V3' O5' V2' 50.9(2) . . . . ? O6' V3' O5' V2' 110.68(14) . . . . ? O4' V3' O5' V2' -163.77(14) . . . . ? V4' V3' O5' V2' 98.69(12) . . . . ? V1' V3' O5' V2' -135.29(9) . . . . ? O2' V2' O5' C19' 167.6(4) . . . . ? O7' V2' O5' C19' 81.0(4) 2_766 . . . ? O10' V2' O5' C19' -6.0(4) . . . . ? O11' V2' O5' C19' 179(92) . . . . ? Cl2' V2' O5' C19' -96.6(3) . . . . ? V3' V2' O5' C19' 150.8(4) . . . . ? O2' V2' O5' V3' 16.73(15) . . . . ? O7' V2' O5' V3' -69.83(14) 2_766 . . . ? O10' V2' O5' V3' -156.79(13) . . . . ? O11' V2' O5' V3' 28.6(11) . . . . ? Cl2' V2' O5' V3' 112.55(11) . . . . ? O3' V4' O6' C21' 170.0(4) . . . . ? O7' V4' O6' C21' -94.7(4) . . . . ? O12' V4' O6' C21' -3.3(4) . . . . ? O13' V4' O6' C21' 172.8(8) . . . . ? O9' V4' O6' C21' 80.6(4) . . . . ? V3' V4' O6' C21' 148.1(4) . . . . ? O3' V4' O6' V3' 21.86(15) . . . . ? O7' V4' O6' V3' 117.21(15) . . . . ? O12' V4' O6' V3' -151.46(15) . . . . ? O13' V4' O6' V3' 24.6(10) . . . . ? O9' V4' O6' V3' -67.55(16) . . . . ? O1' V3' O6' C21' -107.6(4) . . . . ? O5' V3' O6' C21' 44.1(3) . . . . ? O2' V3' O6' C21' 115.8(3) . . . . ? O3' V3' O6' C21' -172.7(4) . . . . ? O4' V3' O6' C21' -45.1(3) . . . . ? V2' V3' O6' C21' 82.2(3) . . . . ? V4' V3' O6' C21' -151.6(4) . . . . ? V1' V3' O6' C21' -70.3(3) . . . . ? O1' V3' O6' V4' 44.0(3) . . . . ? O5' V3' O6' V4' -164.28(15) . . . . ? O2' V3' O6' V4' -92.63(18) . . . . ? O3' V3' O6' V4' -21.09(15) . . . . ? O4' V3' O6' V4' 106.45(15) . . . . ? V2' V3' O6' V4' -126.22(11) . . . . ? V1' V3' O6' V4' 81.32(13) . . . . ? O3' V4' O7' V2' -144.43(19) . . . 2_766 ? O6' V4' O7' V2' 139.55(19) . . . 2_766 ? O12' V4' O7' V2' 44.2(2) . . . 2_766 ? O13' V4' O7' V2' -49.1(2) . . . 2_766 ? O9' V4' O7' V2' 2.8(13) . . . 2_766 ? V3' V4' O7' V2' 176.78(15) . . . 2_766 ? O4' V1' O8' C23' -29.5(5) . . . . ? O1' V1' O8' C23' 48.5(5) . . . . ? N1' V1' O8' C23' -123.5(7) . . . . ? N2' V1' O8' C23' -127.7(5) . . . . ? Cl1' V1' O8' C23' 142.9(5) . . . . ? V3' V1' O8' C23' 10.2(5) . . . . ? O3' V4' O9' C23' 32(3) . . . . ? O7' V4' O9' C23' -115(3) . . . . ? O6' V4' O9' C23' 108(3) . . . . ? O12' V4' O9' C23' -157(3) . . . . ? O13' V4' O9' C23' -63(3) . . . . ? V3' V4' O9' C23' 71(3) . . . . ? O2' V2' O10' C30' 76.3(11) . . . . ? O7' V2' O10' C30' 24.4(5) 2_766 . . . ? O5' V2' O10' C30' 115.3(5) . . . . ? O11' V2' O10' C30' -65.4(5) . . . . ? Cl2' V2' O10' C30' -152.9(5) . . . . ? V3' V2' O10' C30' 96.0(5) . . . . ? O2' V2' O11' C37' -104.2(5) . . . . ? O7' V2' O11' C37' -17.3(5) 2_766 . . . ? O5' V2' O11' C37' -115.8(10) . . . . ? O10' V2' O11' C37' 69.5(5) . . . . ? Cl2' V2' O11' C37' 159.9(5) . . . . ? V3' V2' O11' C37' -91.0(5) . . . . ? O3' V4' O12' C37' -155.4(8) . . . 2_766 ? O7' V4' O12' C37' -27.6(5) . . . 2_766 ? O6' V4' O12' C37' -119.0(5) . . . 2_766 ? O13' V4' O12' C37' 61.6(5) . . . 2_766 ? O9' V4' O12' C37' 147.8(5) . . . 2_766 ? V3' V4' O12' C37' -142.6(4) . . . 2_766 ? O3' V4' O13' C30' 111.0(5) . . . 2_766 ? O7' V4' O13' C30' 15.5(5) . . . 2_766 ? O6' V4' O13' C30' 108.3(10) . . . 2_766 ? O12' V4' O13' C30' -75.6(5) . . . 2_766 ? O9' V4' O13' C30' -159.0(5) . . . 2_766 ? V3' V4' O13' C30' 129.4(4) . . . 2_766 ? O4' V1' N1' C5' 75.9(4) . . . . ? O8' V1' N1' C5' 170.5(5) . . . . ? O1' V1' N1' C5' -1.6(4) . . . . ? N2' V1' N1' C5' 174.8(4) . . . . ? Cl1' V1' N1' C5' -95.6(3) . . . . ? V3' V1' N1' C5' 36.6(3) . . . . ? O4' V1' N1' C1' -99.9(3) . . . . ? O8' V1' N1' C1' -5.3(8) . . . . ? O1' V1' N1' C1' -177.4(3) . . . . ? N2' V1' N1' C1' -1.0(3) . . . . ? Cl1' V1' N1' C1' 88.6(3) . . . . ? V3' V1' N1' C1' -139.2(3) . . . . ? O4' V1' N2' C10' -97.4(4) . . . . ? O8' V1' N2' C10' -3.9(4) . . . . ? O1' V1' N2' C10' -163.2(6) . . . . ? N1' V1' N2' C10' 177.1(4) . . . . ? Cl1' V1' N2' C10' 88.0(4) . . . . ? V3' V1' N2' C10' -103.2(4) . . . . ? O4' V1' N2' C6' 90.5(3) . . . . ? O8' V1' N2' C6' -176.1(3) . . . . ? O1' V1' N2' C6' 24.7(9) . . . . ? N1' V1' N2' C6' 4.9(3) . . . . ? Cl1' V1' N2' C6' -84.1(3) . . . . ? V3' V1' N2' C6' 84.7(4) . . . . ? C5' N1' C1' C2' 1.6(7) . . . . ? V1' N1' C1' C2' 177.7(4) . . . . ? C5' N1' C1' C6' -178.8(4) . . . . ? V1' N1' C1' C6' -2.7(5) . . . . ? N1' C1' C2' C3' -0.3(7) . . . . ? C6' C1' C2' C3' -179.8(5) . . . . ? C1' C2' C3' C4' -1.4(7) . . . . ? C2' C3' C4' C5' 1.7(7) . . . . ? C1' N1' C5' C4' -1.3(7) . . . . ? V1' N1' C5' C4' -177.0(3) . . . . ? C3' C4' C5' N1' -0.4(7) . . . . ? C10' N2' C6' C7' -0.1(7) . . . . ? V1' N2' C6' C7' 172.5(4) . . . . ? C10' N2' C6' C1' 179.5(4) . . . . ? V1' N2' C6' C1' -7.9(5) . . . . ? N1' C1' C6' N2' 7.0(6) . . . . ? C2' C1' C6' N2' -173.4(4) . . . . ? N1' C1' C6' C7' -173.4(5) . . . . ? C2' C1' C6' C7' 6.1(8) . . . . ? N2' C6' C7' C8' 0.9(8) . . . . ? C1' C6' C7' C8' -178.7(5) . . . . ? C6' C7' C8' C9' -0.8(9) . . . . ? C7' C8' C9' C10' 0.0(9) . . . . ? C6' N2' C10' C9' -0.7(8) . . . . ? V1' N2' C10' C9' -172.6(4) . . . . ? C8' C9' C10' N2' 0.8(9) . . . . ? V3' O1' C11' C16' 60.0(5) . . . . ? V1' O1' C11' C16' -98.2(4) . . . . ? V3' O1' C11' C12' -62.6(5) . . . . ? V1' O1' C11' C12' 139.2(3) . . . . ? O1' C11' C12' C13' 68.1(5) . . . . ? C16' C11' C12' C13' -54.6(5) . . . . ? V2' O2' C13' C14' 104.4(5) . . . . ? V3' O2' C13' C14' -61.0(5) . . . . ? V2' O2' C13' C12' -134.2(4) . . . . ? V3' O2' C13' C12' 60.4(5) . . . . ? C11' C12' C13' O2' -66.9(5) . . . . ? C11' C12' C13' C14' 54.2(5) . . . . ? O2' C13' C14' C15' 66.8(5) . . . . ? C12' C13' C14' C15' -53.4(5) . . . . ? V4' O3' C15' C16' 98.3(5) . . . . ? V3' O3' C15' C16' -58.7(5) . . . . ? V4' O3' C15' C14' -138.8(4) . . . . ? V3' O3' C15' C14' 64.2(5) . . . . ? C13' C14' C15' O3' -68.3(5) . . . . ? C13' C14' C15' C16' 53.5(5) . . . . ? O1' C11' C16' C15' -67.2(5) . . . . ? C12' C11' C16' C15' 54.8(5) . . . . ? O3' C15' C16' C11' 66.9(5) . . . . ? C14' C15' C16' C11' -54.1(5) . . . . ? V1' O4' C17' C18' -113.6(4) . . . . ? V3' O4' C17' C18' 56.7(4) . . . . ? V1' O4' C17' C22' 124.9(4) . . . . ? V3' O4' C17' C22' -64.8(4) . . . . ? O4' C17' C18' C19' -68.2(5) . . . . ? C22' C17' C18' C19' 51.9(5) . . . . ? V3' O5' C19' C18' -60.9(4) . . . . ? V2' O5' C19' C18' 153.5(3) . . . . ? V3' O5' C19' C20' 61.4(4) . . . . ? V2' O5' C19' C20' -84.2(5) . . . . ? C17' C18' C19' O5' 69.8(5) . . . . ? C17' C18' C19' C20' -52.3(5) . . . . ? O5' C19' C20' C21' -67.4(5) . . . . ? C18' C19' C20' C21' 53.7(5) . . . . ? V4' O6' C21' C20' 155.9(3) . . . . ? V3' O6' C21' C20' -61.7(5) . . . . ? V4' O6' C21' C22' -80.9(5) . . . . ? V3' O6' C21' C22' 61.6(5) . . . . ? C19' C20' C21' O6' 67.3(5) . . . . ? C19' C20' C21' C22' -55.7(5) . . . . ? O6' C21' C22' C17' -66.6(5) . . . . ? C20' C21' C22' C17' 55.6(5) . . . . ? O4' C17' C22' C21' 67.6(5) . . . . ? C18' C17' C22' C21' -53.1(5) . . . . ? V4' O9' C23' O8' -70(3) . . . . ? V4' O9' C23' C24' 109(3) . . . . ? V1' O8' C23' O9' -6.3(8) . . . . ? V1' O8' C23' C24' 174.2(4) . . . . ? O9' C23' C24' C29' -4.3(7) . . . . ? O8' C23' C24' C29' 175.2(5) . . . . ? O9' C23' C24' C25' 178.4(5) . . . . ? O8' C23' C24' C25' -2.1(6) . . . . ? C29' C24' C25' C26' 0.4(8) . . . . ? C23' C24' C25' C26' 177.8(5) . . . . ? C24' C25' C26' C27' -2.0(9) . . . . ? C25' C26' C27' C28' 2.1(11) . . . . ? C26' C27' C28' C29' -0.6(12) . . . . ? C25' C24' C29' C28' 1.0(9) . . . . ? C23' C24' C29' C28' -176.3(5) . . . . ? C27' C28' C29' C24' -0.9(11) . . . . ? V2' O10' C30' O13' -0.8(8) . . . 2_766 ? V2' O10' C30' C31W -178.1(3) . . . . ? V2' O10' C30' C31V 176.3(3) . . . . ? O13' C30' C31V C32V 22.3(6) 2_766 . . . ? O10' C30' C31V C32V -155.0(4) . . . . ? C31W C30' C31V C32V 66.4(3) . . . . ? O13' C30' C31V C36V -154.4(5) 2_766 . . . ? O10' C30' C31V C36V 28.3(6) . . . . ? C31W C30' C31V C36V -110.2(2) . . . . ? C36V C31V C32V C33V 0.0 . . . . ? C30' C31V C32V C33V -176.7(4) . . . . ? C31V C32V C33V C34V 0.0 . . . . ? C32V C33V C34V C35V 0.0 . . . . ? C33V C34V C35V C36V 0.0 . . . . ? C34V C35V C36V C31V 0.0 . . . . ? C32V C31V C36V C35V 0.0 . . . . ? C30' C31V C36V C35V 176.6(4) . . . . ? O13' C30' C31W C36W 161.3(4) 2_766 . . . ? O10' C30' C31W C36W -21.1(6) . . . . ? C31V C30' C31W C36W 22.80(12) . . . . ? O13' C30' C31W C32W -18.3(6) 2_766 . . . ? O10' C30' C31W C32W 159.3(4) . . . . ? C31V C30' C31W C32W -156.8(4) . . . . ? C36W C31W C32W C33W 0.0 . . . . ? C30' C31W C32W C33W 179.6(5) . . . . ? C31W C32W C33W C34W 0.0 . . . . ? C32W C33W C34W C35W 0.0 . . . . ? C33W C34W C35W C36W 0.0 . . . . ? C34W C35W C36W C31W 0.0 . . . . ? C32W C31W C36W C35W 0.0 . . . . ? C30' C31W C36W C35W -179.6(5) . . . . ? V2' O11' C37' O12' 5.0(8) . . . 2_766 ? V2' O11' C37' C38' -174.6(3) . . . . ? O12' C37' C38' C43' -173.2(5) 2_766 . . . ? O11' C37' C38' C43' 6.5(8) . . . . ? O12' C37' C38' C39' 3.8(7) 2_766 . . . ? O11' C37' C38' C39' -176.5(5) . . . . ? C43' C38' C39' C40' -0.9(9) . . . . ? C37' C38' C39' C40' -178.0(5) . . . . ? C38' C39' C40' C41' 0.8(10) . . . . ? C39' C40' C41' C42' 0.0(11) . . . . ? C40' C41' C42' C43' -0.5(12) . . . . ? C39' C38' C43' C42' 0.4(10) . . . . ? C37' C38' C43' C42' 177.4(6) . . . . ? C41' C42' C43' C38' 0.4(12) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 24.71 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 1.231 _refine_diff_density_min -0.571 _refine_diff_density_rms 0.139