# 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 _publ_section_title ; Air oxidation of divanadium(IV) complexes ; _audit_creation_method 'SHELXL-97 plus manual editing' ## contact for matters related to this CIF _publ_contact_author_name 'Andrew D. Bond' _publ_contact_author_address ; University of Southern Denmark Department of Physics and Chemistry Campusvej 55 5230 Odense Denmark ; _publ_contact_author_email adb@chem.sdu.dk _publ_contact_author_fax '+45 6615 8780' _publ_contact_author_phone '+45 6650 2545' loop_ _publ_author_name A.Bond R.K.Egdal #===END #------------------------------------------------------------------------ data_1 _database_code_depnum_ccdc_archive 'CCDC 717959' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H43 N6 O5 V2 3+, 3(Cl O4 -), H2 O' _chemical_formula_sum 'C36 H45 Cl3 N6 O18 V2' _chemical_formula_weight 1058.01 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 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' 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 10.8133(6) _cell_length_b 22.2245(11) _cell_length_c 18.1295(9) _cell_angle_alpha 90.00 _cell_angle_beta 93.608(2) _cell_angle_gamma 90.00 _cell_volume 4348.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 3597 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 20.83 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.616 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2176 _exptl_absorpt_coefficient_mu 0.697 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.632 _exptl_absorpt_correction_T_max 0.946 _exptl_absorpt_process_details 'SADABS (Sheldrick, 2003)' _exptl_special_details ; H atoms of the water molecules were located from difference Fourier maps and refined with O---H restrained to 0.84(1) \%A, H...H restrained to 1.32(1) \%A and U~iso~(H) = 1.5U~eq~(O). ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 46075 _diffrn_reflns_av_R_equivalents 0.0831 _diffrn_reflns_av_sigmaI/netI 0.1024 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.54 _diffrn_reflns_theta_max 24.68 _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 24.68 _diffrn_measured_fraction_theta_full 0.993 _reflns_number_total 7328 _reflns_number_gt 4346 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10' _computing_molecular_graphics 'SHELXTL v.6.10' _computing_publication_material 'SHELXTL v.6.10' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0417P)^2^] 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 7328 _refine_ls_number_parameters 605 _refine_ls_number_restraints 9 _refine_ls_R_factor_all 0.0829 _refine_ls_R_factor_gt 0.0404 _refine_ls_wR_factor_ref 0.0873 _refine_ls_wR_factor_gt 0.0811 _refine_ls_goodness_of_fit_ref 0.909 _refine_ls_restrained_S_all 0.909 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.468 _refine_diff_density_min -0.413 _refine_diff_density_rms 0.070 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 0.25289(5) 0.32380(2) 0.23773(3) 0.01757(15) Uani 1 1 d . . . V2 V 0.56511(5) 0.35248(2) 0.17901(3) 0.01784(15) Uani 1 1 d . . . O1 O 0.41118(17) 0.37419(9) 0.23538(10) 0.0166(5) Uani 1 1 d . . . O2 O 0.22005(18) 0.30902(9) 0.15217(11) 0.0245(6) Uani 1 1 d . . . O3 O 0.35611(19) 0.25248(9) 0.26940(13) 0.0253(6) Uani 1 1 d D . . H31W H 0.4275(14) 0.2485(12) 0.2892(16) 0.038 Uiso 1 1 d D . . H32W H 0.330(2) 0.2172(6) 0.2638(18) 0.038 Uiso 1 1 d D . . O4 O 0.60266(18) 0.28678(9) 0.20586(11) 0.0233(5) Uani 1 1 d . . . O5 O 0.44467(18) 0.33677(10) 0.09018(11) 0.0226(6) Uani 1 1 d D . . H51W H 0.3701(12) 0.3278(13) 0.0956(15) 0.034 Uiso 1 1 d D . . H52W H 0.461(2) 0.3171(12) 0.0524(11) 0.034 Uiso 1 1 d D . . N1 N 0.2423(2) 0.35233(11) 0.35781(13) 0.0139(6) Uani 1 1 d . . . N2 N 0.1478(2) 0.40410(11) 0.23045(14) 0.0167(6) Uani 1 1 d . . . N3 N 0.1061(2) 0.27384(11) 0.27891(14) 0.0190(6) Uani 1 1 d . . . N4 N 0.5713(2) 0.45111(11) 0.14232(13) 0.0154(6) Uani 1 1 d . . . N5 N 0.6820(2) 0.39436(12) 0.26235(13) 0.0169(6) Uani 1 1 d . . . N6 N 0.7078(2) 0.35853(12) 0.10419(13) 0.0173(6) Uani 1 1 d . . . C1 C 0.4115(3) 0.42975(14) 0.27140(17) 0.0153(7) Uani 1 1 d . . . C2 C 0.3965(2) 0.43147(14) 0.34767(17) 0.0150(7) Uani 1 1 d . . . C3 C 0.3967(3) 0.48698(14) 0.38246(17) 0.0181(8) Uani 1 1 d . . . H3 H 0.3865 0.4880 0.4341 0.022 Uiso 1 1 calc R . . C4 C 0.4108(3) 0.54081(14) 0.34617(17) 0.0166(8) Uani 1 1 d . . . C5 C 0.4252(2) 0.53719(14) 0.26957(17) 0.0176(8) Uani 1 1 d . . . H5 H 0.4351 0.5733 0.2425 0.021 Uiso 1 1 calc R . . C6 C 0.4256(3) 0.48280(14) 0.23248(16) 0.0143(7) Uani 1 1 d . . . C7 C 0.4115(3) 0.60183(13) 0.38495(17) 0.0205(8) Uani 1 1 d . . . C8 C 0.3813(3) 0.59642(16) 0.46614(18) 0.0392(10) Uani 1 1 d . . . H8A H 0.3831 0.6364 0.4889 0.059 Uiso 1 1 calc R . . H8B H 0.4428 0.5705 0.4924 0.059 Uiso 1 1 calc R . . H8C H 0.2986 0.5789 0.4691 0.059 Uiso 1 1 calc R . . C9 C 0.3158(4) 0.64265(16) 0.3467(2) 0.0486(11) Uani 1 1 d . . . H9A H 0.3168 0.6818 0.3716 0.073 Uiso 1 1 calc R . . H9B H 0.2335 0.6245 0.3486 0.073 Uiso 1 1 calc R . . H9C H 0.3350 0.6482 0.2950 0.073 Uiso 1 1 calc R . . C10 C 0.5401(3) 0.63010(17) 0.3834(2) 0.0576(13) Uani 1 1 d . . . H10A H 0.5405 0.6692 0.4083 0.086 Uiso 1 1 calc R . . H10B H 0.5610 0.6356 0.3320 0.086 Uiso 1 1 calc R . . H10C H 0.6014 0.6036 0.4088 0.086 Uiso 1 1 calc R . . C11 C 0.3658(3) 0.37465(14) 0.38755(17) 0.0186(8) Uani 1 1 d . . . H11A H 0.4300 0.3438 0.3803 0.022 Uiso 1 1 calc R . . H11B H 0.3639 0.3827 0.4412 0.022 Uiso 1 1 calc R . . C12 C 0.1460(3) 0.39975(14) 0.36342(16) 0.0185(8) Uani 1 1 d . . . H12A H 0.1722 0.4279 0.4038 0.022 Uiso 1 1 calc R . . H12B H 0.0673 0.3808 0.3761 0.022 Uiso 1 1 calc R . . C13 C 0.1249(3) 0.43423(15) 0.29305(17) 0.0179(8) Uani 1 1 d . . . C14 C 0.0783(3) 0.49195(15) 0.29132(19) 0.0239(8) Uani 1 1 d . . . H14 H 0.0670 0.5131 0.3359 0.029 Uiso 1 1 calc R . . C15 C 0.0484(3) 0.51851(16) 0.2235(2) 0.0309(9) Uani 1 1 d . . . H15 H 0.0154 0.5581 0.2211 0.037 Uiso 1 1 calc R . . C16 C 0.0664(3) 0.48748(16) 0.16009(19) 0.0298(9) Uani 1 1 d . . . H16 H 0.0443 0.5049 0.1133 0.036 Uiso 1 1 calc R . . C17 C 0.1171(3) 0.43054(15) 0.16475(18) 0.0222(8) Uani 1 1 d . . . H17 H 0.1309 0.4093 0.1205 0.027 Uiso 1 1 calc R . . C18 C 0.2045(3) 0.29760(13) 0.39782(16) 0.0175(8) Uani 1 1 d . . . H18A H 0.2750 0.2692 0.4039 0.021 Uiso 1 1 calc R . . H18B H 0.1785 0.3086 0.4474 0.021 Uiso 1 1 calc R . . C19 C 0.0999(3) 0.26923(13) 0.35365(17) 0.0161(8) Uani 1 1 d . . . C20 C 0.0032(3) 0.24014(14) 0.38351(18) 0.0238(8) Uani 1 1 d . . . H20 H -0.0018 0.2388 0.4356 0.029 Uiso 1 1 calc R . . C21 C -0.0871(3) 0.21282(15) 0.3379(2) 0.0297(9) Uani 1 1 d . . . H21 H -0.1543 0.1924 0.3581 0.036 Uiso 1 1 calc R . . C22 C -0.0782(3) 0.21564(15) 0.2626(2) 0.0311(9) Uani 1 1 d . . . H22 H -0.1381 0.1964 0.2301 0.037 Uiso 1 1 calc R . . C23 C 0.0183(3) 0.24664(14) 0.23529(19) 0.0254(8) Uani 1 1 d . . . H23 H 0.0232 0.2490 0.1832 0.031 Uiso 1 1 calc R . . C24 C 0.4490(3) 0.48061(14) 0.15157(16) 0.0190(8) Uani 1 1 d . . . H24A H 0.3823 0.4576 0.1244 0.023 Uiso 1 1 calc R . . H24B H 0.4494 0.5219 0.1311 0.023 Uiso 1 1 calc R . . C25 C 0.6714(3) 0.48362(14) 0.18626(16) 0.0184(8) Uani 1 1 d . . . H25A H 0.6442 0.5254 0.1951 0.022 Uiso 1 1 calc R . . H25B H 0.7461 0.4855 0.1574 0.022 Uiso 1 1 calc R . . C26 C 0.7045(3) 0.45400(15) 0.25896(17) 0.0165(8) Uani 1 1 d . . . C27 C 0.7639(3) 0.48409(15) 0.31747(18) 0.0248(8) Uani 1 1 d . . . H27 H 0.7754 0.5264 0.3147 0.030 Uiso 1 1 calc R . . C28 C 0.8067(3) 0.45334(16) 0.37984(18) 0.0271(9) Uani 1 1 d . . . H28 H 0.8479 0.4738 0.4203 0.033 Uiso 1 1 calc R . . C29 C 0.7881(3) 0.39167(16) 0.38198(18) 0.0261(9) Uani 1 1 d . . . H29 H 0.8189 0.3687 0.4233 0.031 Uiso 1 1 calc R . . C30 C 0.7245(3) 0.36455(15) 0.32339(18) 0.0222(8) Uani 1 1 d . . . H30 H 0.7097 0.3225 0.3259 0.027 Uiso 1 1 calc R . . C31 C 0.6003(3) 0.44788(14) 0.06375(15) 0.0193(8) Uani 1 1 d . . . H31A H 0.6208 0.4884 0.0454 0.023 Uiso 1 1 calc R . . H31B H 0.5281 0.4322 0.0333 0.023 Uiso 1 1 calc R . . C32 C 0.7093(3) 0.40628(15) 0.05902(17) 0.0202(8) Uani 1 1 d . . . C33 C 0.8044(3) 0.41606(16) 0.01329(17) 0.0272(9) Uani 1 1 d . . . H33 H 0.8035 0.4503 -0.0180 0.033 Uiso 1 1 calc R . . C34 C 0.9002(3) 0.37580(16) 0.01353(18) 0.0284(9) Uani 1 1 d . . . H34 H 0.9665 0.3817 -0.0177 0.034 Uiso 1 1 calc R . . C35 C 0.8994(3) 0.32686(16) 0.05934(17) 0.0262(9) Uani 1 1 d . . . H35 H 0.9653 0.2985 0.0606 0.031 Uiso 1 1 calc R . . C36 C 0.8021(3) 0.31931(15) 0.10344(17) 0.0229(8) Uani 1 1 d . . . H36 H 0.8015 0.2850 0.1347 0.027 Uiso 1 1 calc R . . Cl1 Cl 0.04704(8) 0.38071(4) 0.57195(5) 0.0304(2) Uani 1 1 d . . . O1A O 0.1662(2) 0.39267(13) 0.54663(14) 0.0600(8) Uani 1 1 d . . . O1B O -0.0357(2) 0.42763(13) 0.54553(14) 0.0640(9) Uani 1 1 d . . . O1C O 0.0532(2) 0.38225(11) 0.65162(12) 0.0396(7) Uani 1 1 d . . . O1D O 0.0014(3) 0.32472(12) 0.54604(16) 0.0754(10) Uani 1 1 d . . . Cl2 Cl 0.22905(7) 0.10707(4) 0.44969(5) 0.0273(2) Uani 1 1 d . . . O2A O 0.2112(2) 0.16372(10) 0.48494(13) 0.0412(7) Uani 1 1 d . . . O2B O 0.1450(2) 0.10255(11) 0.38520(12) 0.0403(7) Uani 1 1 d . . . O2C O 0.3531(2) 0.10119(11) 0.42726(13) 0.0434(7) Uani 1 1 d . . . O2D O 0.2027(3) 0.05994(12) 0.49951(15) 0.0661(9) Uani 1 1 d . . . Cl3 Cl 0.59680(8) 0.22104(5) 0.42624(5) 0.0392(3) Uani 1 1 d . . . O3A O 0.6173(2) 0.15861(12) 0.41868(16) 0.0674(9) Uani 1 1 d . . . O3B O 0.4931(2) 0.23093(12) 0.47072(15) 0.0649(9) Uani 1 1 d . . . O3C O 0.5673(2) 0.24648(12) 0.35482(13) 0.0538(8) Uani 1 1 d . . . O3D O 0.7048(2) 0.25070(14) 0.45777(14) 0.0622(9) Uani 1 1 d . . . O1W O 0.2549(2) 0.14585(11) 0.25592(13) 0.0327(6) Uani 1 1 d D . . H11W H 0.220(2) 0.1358(16) 0.2939(9) 0.049 Uiso 1 1 d D . . H12W H 0.198(2) 0.1439(17) 0.2222(10) 0.049 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0182(3) 0.0198(3) 0.0148(3) -0.0009(3) 0.0019(2) -0.0005(3) V2 0.0188(3) 0.0187(3) 0.0162(3) 0.0001(3) 0.0022(2) -0.0007(3) O1 0.0191(12) 0.0166(13) 0.0142(12) -0.0015(11) 0.0014(9) -0.0005(9) O2 0.0265(13) 0.0313(15) 0.0155(12) -0.0035(12) 0.0006(10) -0.0037(11) O3 0.0200(13) 0.0175(13) 0.0378(15) -0.0015(13) -0.0025(11) -0.0013(10) O4 0.0280(13) 0.0168(13) 0.0255(13) 0.0011(12) 0.0058(10) 0.0009(10) O5 0.0200(12) 0.0330(15) 0.0150(13) -0.0031(12) 0.0024(10) -0.0020(11) N1 0.0152(14) 0.0145(15) 0.0119(14) -0.0009(13) -0.0005(11) 0.0035(12) N2 0.0145(14) 0.0220(17) 0.0136(15) 0.0013(15) 0.0023(12) -0.0018(12) N3 0.0156(15) 0.0202(16) 0.0210(17) -0.0012(15) -0.0004(12) 0.0015(12) N4 0.0142(14) 0.0194(15) 0.0127(14) 0.0006(13) 0.0016(11) 0.0003(12) N5 0.0165(15) 0.0176(17) 0.0165(16) 0.0050(15) -0.0001(12) 0.0020(12) N6 0.0181(15) 0.0180(16) 0.0152(15) -0.0012(15) -0.0025(12) 0.0010(13) C1 0.0115(17) 0.015(2) 0.0194(19) -0.0063(19) 0.0008(14) 0.0005(14) C2 0.0120(17) 0.016(2) 0.0169(19) 0.0017(18) -0.0020(13) -0.0013(14) C3 0.0171(18) 0.022(2) 0.0150(19) -0.0035(19) -0.0008(14) 0.0020(15) C4 0.0123(17) 0.016(2) 0.022(2) 0.0002(18) -0.0015(14) 0.0009(14) C5 0.0160(18) 0.0142(19) 0.023(2) 0.0039(18) 0.0010(14) 0.0018(14) C6 0.0140(17) 0.018(2) 0.0116(18) 0.0004(18) 0.0027(14) 0.0031(14) C7 0.0202(19) 0.0141(19) 0.027(2) -0.0017(18) 0.0041(15) 0.0023(15) C8 0.050(3) 0.030(2) 0.037(2) -0.008(2) 0.0013(19) 0.0023(19) C9 0.064(3) 0.032(2) 0.049(3) -0.002(2) -0.005(2) 0.020(2) C10 0.050(3) 0.048(3) 0.076(3) -0.035(3) 0.020(2) -0.018(2) C11 0.0195(18) 0.021(2) 0.0147(18) -0.0002(17) -0.0029(14) 0.0012(15) C12 0.0187(18) 0.022(2) 0.0149(18) -0.0043(18) 0.0020(14) -0.0002(15) C13 0.0115(17) 0.022(2) 0.020(2) 0.0041(19) 0.0016(14) -0.0026(15) C14 0.0231(19) 0.022(2) 0.027(2) -0.0015(19) 0.0043(16) 0.0047(16) C15 0.029(2) 0.025(2) 0.039(3) 0.009(2) 0.0023(18) 0.0098(17) C16 0.032(2) 0.036(2) 0.021(2) 0.016(2) -0.0017(17) 0.0070(18) C17 0.0193(19) 0.031(2) 0.016(2) 0.0058(19) 0.0009(15) -0.0022(16) C18 0.0257(19) 0.0144(18) 0.0124(18) 0.0012(17) 0.0011(14) -0.0014(15) C19 0.0209(19) 0.0114(18) 0.0166(19) 0.0027(17) 0.0049(15) 0.0007(15) C20 0.030(2) 0.020(2) 0.022(2) 0.0008(18) 0.0088(17) -0.0003(16) C21 0.022(2) 0.029(2) 0.038(2) 0.002(2) 0.0084(17) -0.0069(17) C22 0.025(2) 0.035(2) 0.033(2) -0.003(2) -0.0038(17) -0.0115(18) C23 0.024(2) 0.029(2) 0.023(2) -0.0035(19) -0.0027(16) 0.0000(17) C24 0.0187(18) 0.0167(19) 0.021(2) 0.0036(17) -0.0014(15) 0.0010(15) C25 0.0215(19) 0.0181(19) 0.0162(19) -0.0013(18) 0.0051(15) -0.0027(15) C26 0.0132(17) 0.021(2) 0.0157(19) 0.0033(18) 0.0024(14) 0.0023(15) C27 0.028(2) 0.024(2) 0.023(2) -0.002(2) 0.0020(17) -0.0060(17) C28 0.028(2) 0.035(3) 0.018(2) -0.010(2) -0.0022(16) -0.0061(18) C29 0.030(2) 0.035(2) 0.013(2) 0.005(2) -0.0018(16) 0.0006(18) C30 0.0223(19) 0.021(2) 0.024(2) 0.0035(19) 0.0025(16) 0.0014(16) C31 0.0218(18) 0.025(2) 0.0110(18) 0.0018(17) 0.0020(14) -0.0031(16) C32 0.022(2) 0.025(2) 0.0136(18) -0.0058(19) -0.0005(15) -0.0038(16) C33 0.026(2) 0.033(2) 0.023(2) 0.0020(19) 0.0071(16) -0.0061(18) C34 0.020(2) 0.039(2) 0.027(2) -0.002(2) 0.0107(16) -0.0083(18) C35 0.022(2) 0.034(2) 0.022(2) -0.011(2) 0.0012(16) 0.0036(17) C36 0.026(2) 0.023(2) 0.0187(19) -0.0012(18) -0.0027(16) 0.0006(17) Cl1 0.0329(5) 0.0347(6) 0.0231(5) -0.0066(5) -0.0020(4) 0.0002(5) O1A 0.0354(16) 0.100(2) 0.0462(17) -0.0188(18) 0.0141(13) -0.0111(16) O1B 0.073(2) 0.070(2) 0.0458(18) 0.0083(17) -0.0206(15) 0.0291(17) O1C 0.0558(17) 0.0450(17) 0.0181(14) 0.0012(13) 0.0020(12) 0.0122(13) O1D 0.101(2) 0.0453(19) 0.080(2) -0.0346(19) 0.0100(19) -0.0290(18) Cl2 0.0308(5) 0.0305(6) 0.0208(5) -0.0033(5) 0.0016(4) 0.0057(4) O2A 0.0436(16) 0.0358(16) 0.0436(16) -0.0226(14) -0.0026(12) 0.0108(12) O2B 0.0316(14) 0.0617(19) 0.0263(14) -0.0108(14) -0.0079(11) -0.0042(13) O2C 0.0240(14) 0.0576(18) 0.0487(17) -0.0173(15) 0.0040(12) 0.0036(12) O2D 0.108(2) 0.0415(18) 0.0539(19) 0.0250(17) 0.0420(17) 0.0250(16) Cl3 0.0281(6) 0.0516(7) 0.0382(6) 0.0244(6) 0.0055(4) 0.0078(5) O3A 0.0592(19) 0.050(2) 0.096(2) 0.0238(19) 0.0231(17) 0.0174(15) O3B 0.0546(18) 0.068(2) 0.077(2) 0.0373(18) 0.0425(16) 0.0178(16) O3C 0.0392(16) 0.085(2) 0.0347(16) 0.0359(17) -0.0142(12) -0.0136(15) O3D 0.0329(16) 0.099(2) 0.0525(18) 0.0083(18) -0.0167(13) -0.0020(15) O1W 0.0426(16) 0.0269(14) 0.0284(15) 0.0003(15) 0.0001(12) -0.0061(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O2 1.603(2) . ? V1 O3 2.002(2) . ? V1 O1 2.0482(19) . ? V1 N3 2.112(2) . ? V1 N2 2.115(3) . ? V1 N1 2.277(2) . ? V2 O4 1.584(2) . ? V2 O5 2.037(2) . ? V2 O1 2.0644(19) . ? V2 N6 2.122(2) . ? V2 N5 2.123(2) . ? V2 N4 2.293(2) . ? O1 C1 1.397(3) . ? O3 H31W 0.84(1) . ? O3 H32W 0.84(1) . ? O5 H51W 0.84(1) . ? O5 H52W 0.84(1) . ? N1 C18 1.486(3) . ? N1 C12 1.489(3) . ? N1 C11 1.494(3) . ? N2 C17 1.351(4) . ? N2 C13 1.354(4) . ? N3 C23 1.341(4) . ? N3 C19 1.365(4) . ? N4 C31 1.479(3) . ? N4 C25 1.490(4) . ? N4 C24 1.495(3) . ? N5 C30 1.346(4) . ? N5 C26 1.350(4) . ? N6 C32 1.341(4) . ? N6 C36 1.342(4) . ? C1 C6 1.387(4) . ? C1 C2 1.403(4) . ? C2 C3 1.385(4) . ? C2 C11 1.502(4) . ? C3 C4 1.378(4) . ? C3 H3 0.950 . ? C4 C5 1.410(4) . ? C4 C7 1.527(4) . ? C5 C6 1.383(4) . ? C5 H5 0.950 . ? C6 C24 1.505(4) . ? C7 C9 1.512(4) . ? C7 C10 1.528(4) . ? C7 C8 1.532(4) . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 H9A 0.980 . ? C9 H9B 0.980 . ? C9 H9C 0.980 . ? C10 H10A 0.980 . ? C10 H10B 0.980 . ? C10 H10C 0.980 . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C12 C13 1.493(4) . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C13 C14 1.378(4) . ? C14 C15 1.384(4) . ? C14 H14 0.950 . ? C15 C16 1.365(4) . ? C15 H15 0.950 . ? C16 C17 1.380(4) . ? C16 H16 0.950 . ? C17 H17 0.950 . ? C18 C19 1.485(4) . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C19 C20 1.370(4) . ? C20 C21 1.380(4) . ? C20 H20 0.950 . ? C21 C22 1.375(4) . ? C21 H21 0.950 . ? C22 C23 1.369(4) . ? C22 H22 0.950 . ? C23 H23 0.950 . ? C24 H24A 0.990 . ? C24 H24B 0.990 . ? C25 C26 1.496(4) . ? C25 H25A 0.990 . ? C25 H25B 0.990 . ? C26 C27 1.378(4) . ? C27 C28 1.376(4) . ? C27 H27 0.950 . ? C28 C29 1.386(4) . ? C28 H28 0.950 . ? C29 C30 1.368(4) . ? C29 H29 0.950 . ? C30 H30 0.950 . ? C31 C32 1.505(4) . ? C31 H31A 0.990 . ? C31 H31B 0.990 . ? C32 C33 1.378(4) . ? C33 C34 1.368(4) . ? C33 H33 0.950 . ? C34 C35 1.369(4) . ? C34 H34 0.950 . ? C35 C36 1.371(4) . ? C35 H35 0.950 . ? C36 H36 0.950 . ? Cl1 O1D 1.408(3) . ? Cl1 O1A 1.420(2) . ? Cl1 O1B 1.436(3) . ? Cl1 O1C 1.442(2) . ? Cl2 O2D 1.424(3) . ? Cl2 O2A 1.430(2) . ? Cl2 O2C 1.432(2) . ? Cl2 O2B 1.439(2) . ? Cl3 O3A 1.413(3) . ? Cl3 O3D 1.429(3) . ? Cl3 O3C 1.430(2) . ? Cl3 O3B 1.438(2) . ? O1W H11W 0.84(1) . ? O1W H12W 0.84(1) . ? 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 101.58(10) . . ? O2 V1 O1 103.08(9) . . ? O3 V1 O1 89.27(8) . . ? O2 V1 N3 96.23(10) . . ? O3 V1 N3 84.27(9) . . ? O1 V1 N3 160.51(9) . . ? O2 V1 N2 91.55(10) . . ? O3 V1 N2 166.80(10) . . ? O1 V1 N2 89.08(8) . . ? N3 V1 N2 93.03(9) . . ? O2 V1 N1 163.83(9) . . ? O3 V1 N1 90.41(9) . . ? O1 V1 N1 87.72(8) . . ? N3 V1 N1 73.99(9) . . ? N2 V1 N1 76.44(9) . . ? O4 V2 O5 102.93(10) . . ? O4 V2 O1 105.22(9) . . ? O5 V2 O1 86.33(8) . . ? O4 V2 N6 94.14(10) . . ? O5 V2 N6 87.71(9) . . ? O1 V2 N6 160.57(9) . . ? O4 V2 N5 93.20(10) . . ? O5 V2 N5 163.83(10) . . ? O1 V2 N5 90.44(8) . . ? N6 V2 N5 90.16(9) . . ? O4 V2 N4 163.50(9) . . ? O5 V2 N4 87.90(9) . . ? O1 V2 N4 87.67(8) . . ? N6 V2 N4 73.64(9) . . ? N5 V2 N4 76.13(9) . . ? C1 O1 V1 116.82(16) . . ? C1 O1 V2 117.36(16) . . ? V1 O1 V2 125.69(10) . . ? V1 O3 H31W 133.7(19) . . ? V1 O3 H32W 121.9(18) . . ? H31W O3 H32W 104.4(15) . . ? V2 O5 H51W 121.2(19) . . ? V2 O5 H52W 125.1(19) . . ? H51W O5 H52W 103.0(15) . . ? C18 N1 C12 109.4(2) . . ? C18 N1 C11 111.2(2) . . ? C12 N1 C11 110.7(2) . . ? C18 N1 V1 105.70(17) . . ? C12 N1 V1 109.87(17) . . ? C11 N1 V1 109.86(17) . . ? C17 N2 C13 118.4(3) . . ? C17 N2 V1 121.6(2) . . ? C13 N2 V1 119.4(2) . . ? C23 N3 C19 118.3(3) . . ? C23 N3 V1 123.3(2) . . ? C19 N3 V1 118.4(2) . . ? C31 N4 C25 110.3(2) . . ? C31 N4 C24 111.8(2) . . ? C25 N4 C24 110.2(2) . . ? C31 N4 V2 104.17(18) . . ? C25 N4 V2 110.00(17) . . ? C24 N4 V2 110.15(17) . . ? C30 N5 C26 117.9(3) . . ? C30 N5 V2 121.8(2) . . ? C26 N5 V2 119.9(2) . . ? C32 N6 C36 118.0(3) . . ? C32 N6 V2 118.5(2) . . ? C36 N6 V2 123.3(2) . . ? C6 C1 O1 120.7(3) . . ? C6 C1 C2 120.1(3) . . ? O1 C1 C2 119.2(3) . . ? C3 C2 C1 118.4(3) . . ? C3 C2 C11 121.6(3) . . ? C1 C2 C11 119.6(3) . . ? C4 C3 C2 123.5(3) . . ? C4 C3 H3 118.2 . . ? C2 C3 H3 118.2 . . ? C3 C4 C5 116.3(3) . . ? C3 C4 C7 123.3(3) . . ? C5 C4 C7 120.4(3) . . ? C6 C5 C4 122.2(3) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C5 C6 C1 119.4(3) . . ? C5 C6 C24 120.5(3) . . ? C1 C6 C24 119.9(3) . . ? C9 C7 C4 109.8(3) . . ? C9 C7 C10 110.0(3) . . ? C4 C7 C10 109.5(2) . . ? C9 C7 C8 107.9(3) . . ? C4 C7 C8 112.2(3) . . ? C10 C7 C8 107.4(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N1 C11 C2 109.0(2) . . ? N1 C11 H11A 109.9 . . ? C2 C11 H11A 109.9 . . ? N1 C11 H11B 109.9 . . ? C2 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? N1 C12 C13 112.0(2) . . ? N1 C12 H12A 109.2 . . ? C13 C12 H12A 109.2 . . ? N1 C12 H12B 109.2 . . ? C13 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? N2 C13 C14 121.8(3) . . ? N2 C13 C12 115.8(3) . . ? C14 C13 C12 122.2(3) . . ? C13 C14 C15 118.8(3) . . ? C13 C14 H14 120.6 . . ? C15 C14 H14 120.6 . . ? C16 C15 C14 119.7(3) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C17 119.3(3) . . ? C15 C16 H16 120.4 . . ? C17 C16 H16 120.4 . . ? N2 C17 C16 121.9(3) . . ? N2 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C19 C18 N1 107.9(2) . . ? C19 C18 H18A 110.1 . . ? N1 C18 H18A 110.1 . . ? C19 C18 H18B 110.1 . . ? N1 C18 H18B 110.1 . . ? H18A C18 H18B 108.4 . . ? N3 C19 C20 120.9(3) . . ? N3 C19 C18 114.9(3) . . ? C20 C19 C18 124.2(3) . . ? C19 C20 C21 120.0(3) . . ? C19 C20 H20 120.0 . . ? C21 C20 H20 120.0 . . ? C22 C21 C20 118.9(3) . . ? C22 C21 H21 120.5 . . ? C20 C21 H21 120.5 . . ? C23 C22 C21 119.0(3) . . ? C23 C22 H22 120.5 . . ? C21 C22 H22 120.5 . . ? N3 C23 C22 122.7(3) . . ? N3 C23 H23 118.6 . . ? C22 C23 H23 118.6 . . ? N4 C24 C6 109.1(2) . . ? N4 C24 H24A 109.9 . . ? C6 C24 H24A 109.9 . . ? N4 C24 H24B 109.9 . . ? C6 C24 H24B 109.9 . . ? H24A C24 H24B 108.3 . . ? N4 C25 C26 112.5(2) . . ? N4 C25 H25A 109.1 . . ? C26 C25 H25A 109.1 . . ? N4 C25 H25B 109.1 . . ? C26 C25 H25B 109.1 . . ? H25A C25 H25B 107.8 . . ? N5 C26 C27 121.2(3) . . ? N5 C26 C25 116.0(3) . . ? C27 C26 C25 122.6(3) . . ? C28 C27 C26 120.5(3) . . ? C28 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C27 C28 C29 118.2(3) . . ? C27 C28 H28 120.9 . . ? C29 C28 H28 120.9 . . ? C30 C29 C28 118.7(3) . . ? C30 C29 H29 120.6 . . ? C28 C29 H29 120.6 . . ? N5 C30 C29 123.4(3) . . ? N5 C30 H30 118.3 . . ? C29 C30 H30 118.3 . . ? N4 C31 C32 107.4(2) . . ? N4 C31 H31A 110.2 . . ? C32 C31 H31A 110.2 . . ? N4 C31 H31B 110.2 . . ? C32 C31 H31B 110.2 . . ? H31A C31 H31B 108.5 . . ? N6 C32 C33 122.0(3) . . ? N6 C32 C31 114.3(3) . . ? C33 C32 C31 123.7(3) . . ? C34 C33 C32 119.2(3) . . ? C34 C33 H33 120.4 . . ? C32 C33 H33 120.4 . . ? C33 C34 C35 119.2(3) . . ? C33 C34 H34 120.4 . . ? C35 C34 H34 120.4 . . ? C34 C35 C36 119.1(3) . . ? C34 C35 H35 120.5 . . ? C36 C35 H35 120.5 . . ? N6 C36 C35 122.5(3) . . ? N6 C36 H36 118.7 . . ? C35 C36 H36 118.7 . . ? O1D Cl1 O1A 111.30(17) . . ? O1D Cl1 O1B 109.43(18) . . ? O1A Cl1 O1B 108.38(18) . . ? O1D Cl1 O1C 110.37(17) . . ? O1A Cl1 O1C 109.50(15) . . ? O1B Cl1 O1C 107.77(15) . . ? O2D Cl2 O2A 109.04(15) . . ? O2D Cl2 O2C 109.96(16) . . ? O2A Cl2 O2C 111.24(14) . . ? O2D Cl2 O2B 108.84(17) . . ? O2A Cl2 O2B 109.18(14) . . ? O2C Cl2 O2B 108.54(14) . . ? O3A Cl3 O3D 111.24(18) . . ? O3A Cl3 O3C 109.13(18) . . ? O3D Cl3 O3C 108.04(16) . . ? O3A Cl3 O3B 109.72(16) . . ? O3D Cl3 O3B 110.58(18) . . ? O3C Cl3 O3B 108.05(16) . . ? H11W O1W H12W 103.7(15) . . ? 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 O1 C1 127.18(19) . . . . ? O3 V1 O1 C1 -131.1(2) . . . . ? N3 V1 O1 C1 -60.7(4) . . . . ? N2 V1 O1 C1 35.8(2) . . . . ? N1 V1 O1 C1 -40.67(19) . . . . ? O2 V1 O1 V2 -48.67(14) . . . . ? O3 V1 O1 V2 53.05(13) . . . . ? N3 V1 O1 V2 123.5(3) . . . . ? N2 V1 O1 V2 -140.04(12) . . . . ? N1 V1 O1 V2 143.49(12) . . . . ? O4 V2 O1 C1 130.59(19) . . . . ? O5 V2 O1 C1 -127.00(19) . . . . ? N6 V2 O1 C1 -54.6(4) . . . . ? N5 V2 O1 C1 37.2(2) . . . . ? N4 V2 O1 C1 -38.95(19) . . . . ? O4 V2 O1 V1 -53.59(14) . . . . ? O5 V2 O1 V1 48.82(12) . . . . ? N6 V2 O1 V1 121.3(2) . . . . ? N5 V2 O1 V1 -147.03(12) . . . . ? N4 V2 O1 V1 136.87(12) . . . . ? O2 V1 N1 C18 88.6(4) . . . . ? O3 V1 N1 C18 -49.53(17) . . . . ? O1 V1 N1 C18 -138.79(17) . . . . ? N3 V1 N1 C18 34.39(17) . . . . ? N2 V1 N1 C18 131.61(18) . . . . ? O2 V1 N1 C12 -29.2(4) . . . . ? O3 V1 N1 C12 -167.43(18) . . . . ? O1 V1 N1 C12 103.32(18) . . . . ? N3 V1 N1 C12 -83.50(19) . . . . ? N2 V1 N1 C12 13.72(18) . . . . ? O2 V1 N1 C11 -151.3(3) . . . . ? O3 V1 N1 C11 70.56(18) . . . . ? O1 V1 N1 C11 -18.69(18) . . . . ? N3 V1 N1 C11 154.49(19) . . . . ? N2 V1 N1 C11 -108.29(18) . . . . ? O2 V1 N2 C17 -19.0(2) . . . . ? O3 V1 N2 C17 166.9(3) . . . . ? O1 V1 N2 C17 84.0(2) . . . . ? N3 V1 N2 C17 -115.4(2) . . . . ? N1 V1 N2 C17 171.9(2) . . . . ? O2 V1 N2 C13 170.1(2) . . . . ? O3 V1 N2 C13 -4.0(5) . . . . ? O1 V1 N2 C13 -86.8(2) . . . . ? N3 V1 N2 C13 73.8(2) . . . . ? N1 V1 N2 C13 1.0(2) . . . . ? O2 V1 N3 C23 -4.9(3) . . . . ? O3 V1 N3 C23 -105.9(2) . . . . ? O1 V1 N3 C23 -177.2(2) . . . . ? N2 V1 N3 C23 87.0(2) . . . . ? N1 V1 N3 C23 162.0(3) . . . . ? O2 V1 N3 C19 175.5(2) . . . . ? O3 V1 N3 C19 74.4(2) . . . . ? O1 V1 N3 C19 3.1(4) . . . . ? N2 V1 N3 C19 -92.7(2) . . . . ? N1 V1 N3 C19 -17.7(2) . . . . ? O4 V2 N4 C31 79.7(4) . . . . ? O5 V2 N4 C31 -51.96(17) . . . . ? O1 V2 N4 C31 -138.37(17) . . . . ? N6 V2 N4 C31 36.27(16) . . . . ? N5 V2 N4 C31 130.60(18) . . . . ? O4 V2 N4 C25 -38.5(4) . . . . ? O5 V2 N4 C25 -170.20(18) . . . . ? O1 V2 N4 C25 103.38(18) . . . . ? N6 V2 N4 C25 -81.97(18) . . . . ? N5 V2 N4 C25 12.36(17) . . . . ? O4 V2 N4 C24 -160.2(3) . . . . ? O5 V2 N4 C24 68.11(18) . . . . ? O1 V2 N4 C24 -18.31(17) . . . . ? N6 V2 N4 C24 156.33(19) . . . . ? N5 V2 N4 C24 -109.34(18) . . . . ? O4 V2 N5 C30 -18.7(2) . . . . ? O5 V2 N5 C30 164.8(3) . . . . ? O1 V2 N5 C30 86.5(2) . . . . ? N6 V2 N5 C30 -112.9(2) . . . . ? N4 V2 N5 C30 174.0(2) . . . . ? O4 V2 N5 C26 168.5(2) . . . . ? O5 V2 N5 C26 -7.9(4) . . . . ? O1 V2 N5 C26 -86.2(2) . . . . ? N6 V2 N5 C26 74.4(2) . . . . ? N4 V2 N5 C26 1.3(2) . . . . ? O4 V2 N6 C32 173.1(2) . . . . ? O5 V2 N6 C32 70.3(2) . . . . ? O1 V2 N6 C32 -1.9(4) . . . . ? N5 V2 N6 C32 -93.7(2) . . . . ? N4 V2 N6 C32 -18.2(2) . . . . ? O4 V2 N6 C36 -12.0(2) . . . . ? O5 V2 N6 C36 -114.9(2) . . . . ? O1 V2 N6 C36 172.9(2) . . . . ? N5 V2 N6 C36 81.2(2) . . . . ? N4 V2 N6 C36 156.7(2) . . . . ? V1 O1 C1 C6 -118.3(2) . . . . ? V2 O1 C1 C6 57.9(3) . . . . ? V1 O1 C1 C2 61.3(3) . . . . ? V2 O1 C1 C2 -122.5(2) . . . . ? C6 C1 C2 C3 -0.2(4) . . . . ? O1 C1 C2 C3 -179.8(2) . . . . ? C6 C1 C2 C11 172.5(3) . . . . ? O1 C1 C2 C11 -7.0(4) . . . . ? C1 C2 C3 C4 0.0(4) . . . . ? C11 C2 C3 C4 -172.6(3) . . . . ? C2 C3 C4 C5 0.2(4) . . . . ? C2 C3 C4 C7 -179.7(3) . . . . ? C3 C4 C5 C6 -0.1(4) . . . . ? C7 C4 C5 C6 179.8(3) . . . . ? C4 C5 C6 C1 -0.1(4) . . . . ? C4 C5 C6 C24 -176.3(3) . . . . ? O1 C1 C6 C5 179.8(2) . . . . ? C2 C1 C6 C5 0.3(4) . . . . ? O1 C1 C6 C24 -4.0(4) . . . . ? C2 C1 C6 C24 176.5(3) . . . . ? C3 C4 C7 C9 -125.9(3) . . . . ? C5 C4 C7 C9 54.2(4) . . . . ? C3 C4 C7 C10 113.2(3) . . . . ? C5 C4 C7 C10 -66.7(4) . . . . ? C3 C4 C7 C8 -6.0(4) . . . . ? C5 C4 C7 C8 174.1(3) . . . . ? C18 N1 C11 C2 -177.4(2) . . . . ? C12 N1 C11 C2 -55.6(3) . . . . ? V1 N1 C11 C2 66.0(3) . . . . ? C3 C2 C11 N1 109.2(3) . . . . ? C1 C2 C11 N1 -63.3(3) . . . . ? C18 N1 C12 C13 -141.1(2) . . . . ? C11 N1 C12 C13 96.0(3) . . . . ? V1 N1 C12 C13 -25.5(3) . . . . ? C17 N2 C13 C14 -3.8(4) . . . . ? V1 N2 C13 C14 167.3(2) . . . . ? C17 N2 C13 C12 172.6(2) . . . . ? V1 N2 C13 C12 -16.2(3) . . . . ? N1 C12 C13 N2 28.1(3) . . . . ? N1 C12 C13 C14 -155.5(3) . . . . ? N2 C13 C14 C15 3.3(5) . . . . ? C12 C13 C14 C15 -172.9(3) . . . . ? C13 C14 C15 C16 -0.6(5) . . . . ? C14 C15 C16 C17 -1.5(5) . . . . ? C13 N2 C17 C16 1.6(4) . . . . ? V1 N2 C17 C16 -169.4(2) . . . . ? C15 C16 C17 N2 1.1(5) . . . . ? C12 N1 C18 C19 72.1(3) . . . . ? C11 N1 C18 C19 -165.4(2) . . . . ? V1 N1 C18 C19 -46.2(2) . . . . ? C23 N3 C19 C20 -3.2(4) . . . . ? V1 N3 C19 C20 176.5(2) . . . . ? C23 N3 C19 C18 176.6(3) . . . . ? V1 N3 C19 C18 -3.7(3) . . . . ? N1 C18 C19 N3 35.0(3) . . . . ? N1 C18 C19 C20 -145.2(3) . . . . ? N3 C19 C20 C21 2.7(5) . . . . ? C18 C19 C20 C21 -177.1(3) . . . . ? C19 C20 C21 C22 -0.3(5) . . . . ? C20 C21 C22 C23 -1.5(5) . . . . ? C19 N3 C23 C22 1.4(5) . . . . ? V1 N3 C23 C22 -178.3(2) . . . . ? C21 C22 C23 N3 1.0(5) . . . . ? C31 N4 C24 C6 -179.6(2) . . . . ? C25 N4 C24 C6 -56.5(3) . . . . ? V2 N4 C24 C6 65.0(3) . . . . ? C5 C6 C24 N4 111.7(3) . . . . ? C1 C6 C24 N4 -64.5(3) . . . . ? C31 N4 C25 C26 -137.7(2) . . . . ? C24 N4 C25 C26 98.3(3) . . . . ? V2 N4 C25 C26 -23.3(3) . . . . ? C30 N5 C26 C27 -3.0(4) . . . . ? V2 N5 C26 C27 170.0(2) . . . . ? C30 N5 C26 C25 171.7(2) . . . . ? V2 N5 C26 C25 -15.3(3) . . . . ? N4 C25 C26 N5 26.0(4) . . . . ? N4 C25 C26 C27 -159.3(3) . . . . ? N5 C26 C27 C28 2.9(4) . . . . ? C25 C26 C27 C28 -171.6(3) . . . . ? C26 C27 C28 C29 -0.1(5) . . . . ? C27 C28 C29 C30 -2.2(4) . . . . ? C26 N5 C30 C29 0.6(4) . . . . ? V2 N5 C30 C29 -172.3(2) . . . . ? C28 C29 C30 N5 2.1(5) . . . . ? C25 N4 C31 C32 69.0(3) . . . . ? C24 N4 C31 C32 -168.0(2) . . . . ? V2 N4 C31 C32 -49.0(2) . . . . ? C36 N6 C32 C33 -0.7(4) . . . . ? V2 N6 C32 C33 174.5(2) . . . . ? C36 N6 C32 C31 -179.8(3) . . . . ? V2 N6 C32 C31 -4.6(3) . . . . ? N4 C31 C32 N6 38.1(3) . . . . ? N4 C31 C32 C33 -141.0(3) . . . . ? N6 C32 C33 C34 0.3(5) . . . . ? C31 C32 C33 C34 179.4(3) . . . . ? C32 C33 C34 C35 -0.2(5) . . . . ? C33 C34 C35 C36 0.4(5) . . . . ? C32 N6 C36 C35 0.9(4) . . . . ? V2 N6 C36 C35 -174.0(2) . . . . ? C34 C35 C36 N6 -0.8(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1W H11W O2B 0.84(1) 2.03(1) 2.861(3) 174(4) . O1W H12W O1C 0.84(1) 2.05(1) 2.865(3) 165(3) 4_565 O3 H31W O3C 0.84(1) 1.87(1) 2.681(3) 165(3) . O3 H31W O4 0.84(1) 2.64(3) 3.066(3) 113(2) . O3 H32W O1W 0.84(1) 1.78(1) 2.615(3) 172(3) . O5 H51W O2 0.84(1) 2.02(1) 2.808(3) 156(3) . O5 H51W O2A 0.84(1) 2.56(3) 3.067(3) 119(2) 4_565 O5 H52W O3B 0.84(1) 1.88(1) 2.715(3) 176(3) 4_565 #===END #------------------------------------------------------------------------ data_2 _database_code_depnum_ccdc_archive 'CCDC 717960' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C36 H39 N6 O7 V2 +, Cl O4 -' _chemical_formula_sum 'C36 H39 Cl N6 O11 V2' _chemical_formula_weight 869.06 _chemical_absolute_configuration unk 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 'C 2' _symmetry_space_group_name_Hall 'C 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 14.0031(6) _cell_length_b 19.7115(9) _cell_length_c 13.8599(6) _cell_angle_alpha 90.00 _cell_angle_beta 104.205(2) _cell_angle_gamma 90.00 _cell_volume 3708.7(3) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 5996 _cell_measurement_theta_min 2.56 _cell_measurement_theta_max 20.84 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.556 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1792 _exptl_absorpt_coefficient_mu 0.646 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.687 _exptl_absorpt_correction_T_max 0.882 _exptl_absorpt_process_details 'TWINABS (Sheldrick, 2003)' _exptl_special_details ; #------------------------------------------------------------ ** The crystal is twinned by 180 deg. rotation about [100] ** #------------------------------------------------------------ Two twin components were indexed using CELL_NOW (Bruker-Nonius, 2003) and integrated using SAINT-Plus (Sheldrick, 2003). The two components fit 100% of the data: 16379 data (1798 unique) involve component 1 only 16385 data (1800 unique) involve component 2 only 16126 data (2068 unique) involve 2 components Equivalent data were merged according to point group 2 using TWINABS. The merging R-factor is ca 8 %. Refinement was performed with the HKLF-5 facility in SHELXL. Refined batch scale factor: 0.500(1). ** Refined Flack parameter: 0.499(3) suggest possible inversion twin. The tetrahedral geometry is restrained for the perchlorate anions and the tert-butyl group of the ligand through all bond distances and all 1,3-distances. Only V, Cl and O atoms are refined anisotropically, and the ADPs of the O atoms of the perchlorate anions were restrained to approximate isotropic behaviour (ISOR in SHELXL). ; _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius X8APEX-II CCD' _diffrn_measurement_method 'thin-slice \w and \f scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 48890 _diffrn_reflns_av_R_equivalents 0.081 ## Data are not merged by SHELXL for an HKLF-5 refinement. ## The merging R-factor is obtained from TWINABS ## See _exptl_special_details _diffrn_reflns_av_sigmaI/netI 0.1390 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.61 _diffrn_reflns_theta_max 25.91 _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.91 _diffrn_measured_fraction_theta_full 0.985 _reflns_number_total 10862 _reflns_number_gt 6494 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'APEX2 v.1.0-22 (Bruker-Nonius, 2004)' _computing_cell_refinement 'SAINT v.7.06a (Bruker, 2003)' _computing_data_reduction 'SAINT v.7.06a' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10' _computing_molecular_graphics 'SHELXTL v.6.10' _computing_publication_material 'SHELXTL v.6.10' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0718P)^2^] 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_abs_structure_details ? _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 10862 _refine_ls_number_parameters 320 _refine_ls_number_restraints 105 _refine_ls_R_factor_all 0.0890 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1332 _refine_ls_wR_factor_gt 0.1274 _refine_ls_goodness_of_fit_ref 0.903 _refine_ls_restrained_S_all 0.953 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 0.643 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.085 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 0.37332(6) 0.20082(5) 0.05883(6) 0.0242(2) Uani 1 1 d . . . O1 O 0.5000 0.2458(2) 0.0000 0.0205(11) Uani 1 2 d SU . . O2 O 0.2726(3) 0.18450(17) 0.0918(3) 0.0322(9) Uani 1 1 d U . . O3 O 0.4688(3) 0.17279(18) 0.1702(3) 0.0321(9) Uani 1 1 d U . . O4 O 0.4470(3) 0.12282(17) 0.0947(3) 0.0300(9) Uani 1 1 d U . . N1 N 0.2853(3) 0.2736(2) -0.0492(3) 0.0229(10) Uiso 1 1 d . . . N2 N 0.3231(3) 0.1438(2) -0.0762(3) 0.0253(11) Uiso 1 1 d . . . N3 N 0.3885(3) 0.29389(19) 0.1409(3) 0.0223(10) Uiso 1 1 d . . . C1 C 0.5000 0.3138(3) 0.0000 0.0194(16) Uiso 1 2 d S . . C2 C 0.4228(4) 0.3510(2) -0.0605(4) 0.0192(12) Uiso 1 1 d . . . C3 C 0.4245(4) 0.4206(3) -0.0597(4) 0.0257(13) Uiso 1 1 d . . . H3A H 0.3712 0.4441 -0.1022 0.031 Uiso 1 1 calc R . . C4 C 0.5000 0.4588(3) 0.0000 0.031(2) Uiso 1 2 d SD . . C5 C 0.5000 0.5366(4) 0.0000 0.033(2) Uiso 1 2 d SD . . C51 C 0.5869(7) 0.5670(5) 0.0668(8) 0.062(4) Uiso 0.50 1 d PD . . H51A H 0.6312 0.5311 0.1002 0.094 Uiso 0.50 1 calc PR . . H51B H 0.5664 0.5949 0.1166 0.094 Uiso 0.50 1 calc PR . . H51C H 0.6213 0.5955 0.0281 0.094 Uiso 0.50 1 calc PR . . C52 C 0.4922(9) 0.5595(5) -0.1096(6) 0.051(4) Uiso 0.50 1 d PD . . H52A H 0.4338 0.5390 -0.1536 0.077 Uiso 0.50 1 calc PR . . H52B H 0.5512 0.5450 -0.1300 0.077 Uiso 0.50 1 calc PR . . H52C H 0.4867 0.6091 -0.1139 0.077 Uiso 0.50 1 calc PR . . C53 C 0.4019(7) 0.5601(5) 0.0220(9) 0.064(4) Uiso 0.50 1 d PD . . H53A H 0.3466 0.5379 -0.0244 0.095 Uiso 0.50 1 calc PR . . H53B H 0.3956 0.6095 0.0138 0.095 Uiso 0.50 1 calc PR . . H53C H 0.4014 0.5479 0.0904 0.095 Uiso 0.50 1 calc PR . . C6 C 0.3368(4) 0.3089(3) -0.1187(4) 0.0260(13) Uiso 1 1 d . . . H6A H 0.2895 0.3388 -0.1645 0.031 Uiso 1 1 calc R . . H6B H 0.3612 0.2748 -0.1593 0.031 Uiso 1 1 calc R . . C7 C 0.2039(4) 0.2334(3) -0.1124(4) 0.0279(13) Uiso 1 1 d . . . H7A H 0.1554 0.2211 -0.0740 0.034 Uiso 1 1 calc R . . H7B H 0.1698 0.2605 -0.1709 0.034 Uiso 1 1 calc R . . C8 C 0.2456(4) 0.1714(3) -0.1455(4) 0.0261(13) Uiso 1 1 d . . . C9 C 0.2106(4) 0.1407(3) -0.2347(4) 0.0378(15) Uiso 1 1 d . . . H9A H 0.1576 0.1608 -0.2823 0.045 Uiso 1 1 calc R . . C10 C 0.2513(4) 0.0802(3) -0.2575(5) 0.0360(15) Uiso 1 1 d . . . H10A H 0.2282 0.0594 -0.3208 0.043 Uiso 1 1 calc R . . C11 C 0.3262(4) 0.0512(3) -0.1855(4) 0.0344(14) Uiso 1 1 d . . . H11A H 0.3540 0.0090 -0.1975 0.041 Uiso 1 1 calc R . . C12 C 0.3601(4) 0.0843(2) -0.0963(4) 0.0233(13) Uiso 1 1 d . . . H12A H 0.4118 0.0642 -0.0472 0.028 Uiso 1 1 calc R . . C13 C 0.2455(3) 0.3244(3) 0.0095(3) 0.0259(12) Uiso 1 1 d . . . H13A H 0.1866 0.3057 0.0276 0.031 Uiso 1 1 calc R . . H13B H 0.2253 0.3656 -0.0312 0.031 Uiso 1 1 calc R . . C14 C 0.3229(4) 0.3430(3) 0.1038(4) 0.0279(13) Uiso 1 1 d . . . C15 C 0.3236(4) 0.4049(3) 0.1498(4) 0.0349(14) Uiso 1 1 d . . . H15A H 0.2757 0.4384 0.1228 0.042 Uiso 1 1 calc R . . C16 C 0.3948(5) 0.4174(3) 0.2353(5) 0.0431(17) Uiso 1 1 d . . . H16A H 0.3989 0.4607 0.2662 0.052 Uiso 1 1 calc R . . C17 C 0.4603(4) 0.3673(3) 0.2759(4) 0.0320(14) Uiso 1 1 d . . . H17A H 0.5080 0.3746 0.3368 0.038 Uiso 1 1 calc R . . C18 C 0.4559(4) 0.3065(3) 0.2275(4) 0.0292(13) Uiso 1 1 d . . . H18A H 0.5016 0.2719 0.2555 0.035 Uiso 1 1 calc R . . V2 V 0.14937(7) 0.32551(5) 0.58228(6) 0.0272(2) Uani 1 1 d . . . O5 O 0.0000 0.3716(2) 0.5000 0.0209(12) Uani 1 2 d SU . . O6 O 0.2624(3) 0.3078(2) 0.6349(3) 0.0414(11) Uani 1 1 d U . . O7 O 0.0848(3) 0.29788(18) 0.6769(3) 0.0335(10) Uani 1 1 d U . . O8 O 0.0821(3) 0.24844(17) 0.6025(3) 0.0344(10) Uani 1 1 d U . . N4 N 0.2053(4) 0.3999(2) 0.4887(3) 0.0320(11) Uiso 1 1 d . . . N5 N 0.1608(4) 0.4170(2) 0.6661(3) 0.0308(11) Uiso 1 1 d . . . N6 N 0.1557(3) 0.2699(2) 0.4505(3) 0.0277(11) Uiso 1 1 d . . . C19 C 0.0000 0.4420(4) 0.5000 0.0190(17) Uiso 1 2 d S . . C20 C 0.0609(4) 0.4767(3) 0.4537(4) 0.0310(14) Uiso 1 1 d . . . C21 C 0.0606(5) 0.5463(3) 0.4526(5) 0.0490(17) Uiso 1 1 d . . . H21A H 0.1022 0.5697 0.4190 0.059 Uiso 1 1 calc R . . C22 C 0.0000 0.5836(4) 0.5000 0.042(2) Uiso 1 2 d SD . . C23 C 0.0000 0.6607(5) 0.5000 0.085(4) Uiso 1 2 d SD . . C231 C -0.0266(10) 0.6940(6) 0.4064(7) 0.066(4) Uiso 0.50 1 d PD . . H23A H -0.0434 0.6601 0.3531 0.100 Uiso 0.50 1 calc PR . . H23B H 0.0288 0.7216 0.3974 0.100 Uiso 0.50 1 calc PR . . H23C H -0.0837 0.7233 0.4039 0.100 Uiso 0.50 1 calc PR . . C232 C -0.0861(7) 0.6818(5) 0.5608(8) 0.055(4) Uiso 0.50 1 d PD . . H23D H -0.1507 0.6658 0.5230 0.083 Uiso 0.50 1 calc PR . . H23E H -0.0877 0.7313 0.5680 0.083 Uiso 0.50 1 calc PR . . H23F H -0.0700 0.6607 0.6269 0.083 Uiso 0.50 1 calc PR . . C233 C 0.0890(6) 0.6865(5) 0.5805(7) 0.032(3) Uiso 0.50 1 d PD . . H23G H 0.1501 0.6728 0.5635 0.047 Uiso 0.50 1 calc PR . . H23H H 0.0871 0.6672 0.6451 0.047 Uiso 0.50 1 calc PR . . H23I H 0.0864 0.7361 0.5840 0.047 Uiso 0.50 1 calc PR . . C24 C 0.1306(4) 0.4353(3) 0.4076(4) 0.0356(15) Uiso 1 1 d . . . H24A H 0.0926 0.4013 0.3610 0.043 Uiso 1 1 calc R . . H24B H 0.1646 0.4655 0.3698 0.043 Uiso 1 1 calc R . . C25 C 0.2670(5) 0.3597(3) 0.4363(5) 0.0437(16) Uiso 1 1 d . . . H25A H 0.3289 0.3456 0.4838 0.052 Uiso 1 1 calc R . . H25B H 0.2841 0.3874 0.3834 0.052 Uiso 1 1 calc R . . C26 C 0.2083(5) 0.2973(3) 0.3910(4) 0.0391(16) Uiso 1 1 d . . . C27 C 0.2105(5) 0.2708(4) 0.3008(5) 0.0558(19) Uiso 1 1 d . . . H27A H 0.2457 0.2931 0.2594 0.067 Uiso 1 1 calc R . . C28 C 0.1607(5) 0.2111(3) 0.2706(5) 0.0520(17) Uiso 1 1 d . . . H28A H 0.1600 0.1919 0.2076 0.062 Uiso 1 1 calc R . . C29 C 0.1139(4) 0.1812(3) 0.3312(4) 0.0383(16) Uiso 1 1 d . . . H29A H 0.0820 0.1390 0.3123 0.046 Uiso 1 1 calc R . . C30 C 0.1103(4) 0.2097(3) 0.4206(4) 0.0403(15) Uiso 1 1 d . . . H30A H 0.0758 0.1870 0.4622 0.048 Uiso 1 1 calc R . . C31 C 0.2637(5) 0.4493(3) 0.5586(4) 0.0406(16) Uiso 1 1 d . . . H31A H 0.3300 0.4303 0.5875 0.049 Uiso 1 1 calc R . . H31B H 0.2720 0.4911 0.5219 0.049 Uiso 1 1 calc R . . C32 C 0.2169(4) 0.4667(3) 0.6395(4) 0.0339(14) Uiso 1 1 d . . . C33 C 0.2270(5) 0.5284(3) 0.6865(5) 0.0484(17) Uiso 1 1 d . . . H33A H 0.2656 0.5627 0.6663 0.058 Uiso 1 1 calc R . . C34 C 0.1821(5) 0.5415(3) 0.7626(5) 0.0542(18) Uiso 1 1 d . . . H34A H 0.1875 0.5848 0.7939 0.065 Uiso 1 1 calc R . . C35 C 0.1279(5) 0.4886(3) 0.7925(5) 0.0436(16) Uiso 1 1 d . . . H35A H 0.0982 0.4945 0.8467 0.052 Uiso 1 1 calc R . . C36 C 0.1191(4) 0.4288(3) 0.7417(4) 0.0370(15) Uiso 1 1 d . . . H36A H 0.0813 0.3936 0.7609 0.044 Uiso 1 1 calc R . . Cl1 Cl 0.0000 0.39512(11) 0.0000 0.0508(6) Uani 1 2 d SD . . O1A O 0.0832(4) 0.4349(2) 0.0166(6) 0.100(2) Uani 1 1 d DU . . O1B O -0.0004(6) 0.3513(4) 0.0750(6) 0.180(4) Uani 1 1 d DU . . Cl2 Cl 0.0029(9) 0.02224(13) 0.4853(6) 0.0306(17) Uani 0.50 1 d PD . . O2A O 0.0177(7) 0.0338(4) 0.3916(6) 0.068(3) Uani 0.50 1 d PDU . . O2B O 0.0851(5) 0.0517(3) 0.5418(5) 0.137(3) Uani 1 1 d DU . . O2C O 0.0000 -0.0454(3) 0.5000 0.070(2) Uani 1 2 d SDU . . 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 0.0186(5) 0.0290(5) 0.0261(5) 0.0019(5) 0.0079(4) 0.0004(5) O1 0.015(3) 0.025(3) 0.026(3) 0.000 0.013(2) 0.000 O2 0.0196(19) 0.040(2) 0.043(2) 0.0073(17) 0.0197(18) -0.0055(18) O3 0.034(2) 0.037(2) 0.027(2) -0.0018(17) 0.0104(17) 0.0038(18) O4 0.027(2) 0.032(2) 0.032(2) 0.0015(17) 0.0103(17) 0.0052(17) V2 0.0197(5) 0.0324(5) 0.0296(5) 0.0013(5) 0.0061(4) 0.0066(5) O5 0.018(3) 0.023(3) 0.021(3) 0.000 0.005(2) 0.000 O6 0.020(2) 0.058(3) 0.040(2) 0.0058(19) -0.0023(19) 0.016(2) O7 0.033(2) 0.041(2) 0.026(2) 0.0028(17) 0.0067(18) 0.0058(18) O8 0.041(3) 0.029(2) 0.039(2) 0.0042(18) 0.020(2) 0.0014(18) Cl1 0.0237(13) 0.0393(13) 0.0957(19) 0.000 0.0266(13) 0.000 O1A 0.045(3) 0.056(3) 0.199(6) -0.034(4) 0.028(4) -0.016(3) O1B 0.123(5) 0.182(7) 0.233(7) 0.137(6) 0.043(6) 0.038(5) Cl2 0.0183(17) 0.0444(16) 0.031(5) 0.0000(17) 0.010(3) -0.001(2) O2A 0.050(6) 0.088(6) 0.064(6) 0.014(5) 0.010(5) -0.009(5) O2B 0.078(5) 0.123(5) 0.181(6) -0.044(5) -0.024(4) -0.025(4) O2C 0.092(5) 0.042(4) 0.085(5) 0.000 0.038(4) 0.000 _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 1.618(3) . ? V1 O4 1.850(3) . ? V1 O3 1.861(4) . ? V1 N3 2.141(4) . ? V1 N2 2.148(4) . ? V1 N1 2.217(4) . ? V1 O1 2.3043(19) . ? O1 C1 1.339(8) . ? O1 V1 2.3043(19) 2_655 ? O3 O4 1.415(5) . ? N1 C13 1.483(7) . ? N1 C7 1.484(6) . ? N1 C6 1.508(6) . ? N2 C12 1.339(6) . ? N2 C8 1.373(6) . ? N3 C14 1.347(6) . ? N3 C18 1.356(6) . ? C1 C2 1.401(6) 2_655 ? C1 C2 1.401(6) . ? C2 C3 1.373(7) . ? C2 C6 1.521(7) . ? C3 C4 1.392(6) . ? C3 H3A 0.950 . ? C4 C3 1.392(6) 2_655 ? C4 C5 1.533(9) . ? C5 C51 1.465(8) . ? C5 C51 1.465(8) 2_655 ? C5 C53 1.550(8) 2_655 ? C5 C53 1.550(8) . ? C5 C52 1.563(7) 2_655 ? C5 C52 1.563(7) . ? C51 H51A 0.980 . ? C51 H51B 0.980 . ? C51 H51C 0.980 . ? C52 H52A 0.980 . ? C52 H52B 0.980 . ? C52 H52C 0.980 . ? C53 H53A 0.980 . ? C53 H53B 0.980 . ? C53 H53C 0.980 . ? C6 H6A 0.990 . ? C6 H6B 0.990 . ? C7 C8 1.474(7) . ? C7 H7A 0.990 . ? C7 H7B 0.990 . ? C8 C9 1.355(7) . ? C9 C10 1.392(8) . ? C9 H9A 0.950 . ? C10 C11 1.382(8) . ? C10 H10A 0.950 . ? C11 C12 1.375(7) . ? C11 H11A 0.950 . ? C12 H12A 0.950 . ? C13 C14 1.523(6) . ? C13 H13A 0.990 . ? C13 H13B 0.990 . ? C14 C15 1.375(7) . ? C15 C16 1.371(8) . ? C15 H15A 0.950 . ? C16 C17 1.372(8) . ? C16 H16A 0.950 . ? C17 C18 1.367(7) . ? C17 H17A 0.950 . ? C18 H18A 0.950 . ? V2 O6 1.611(4) . ? V2 O8 1.845(4) . ? V2 O7 1.849(4) . ? V2 N5 2.130(4) . ? V2 N6 2.151(4) . ? V2 N4 2.223(5) . ? V2 O5 2.3086(19) . ? O5 C19 1.389(8) . ? O5 V2 2.309(2) 2_556 ? O7 O8 1.413(5) . ? N4 C31 1.473(7) . ? N4 C25 1.487(7) . ? N4 C24 1.506(7) . ? N5 C36 1.339(7) . ? N5 C32 1.363(7) . ? N6 C26 1.347(7) . ? N6 C30 1.361(7) . ? C19 C20 1.369(6) . ? C19 C20 1.369(6) 2_556 ? C20 C21 1.372(8) . ? C20 C24 1.528(8) . ? C21 C22 1.402(8) . ? C21 H21A 0.950 . ? C22 C21 1.402(8) 2_556 ? C22 C23 1.519(12) . ? C23 C231 1.420(8) 2_556 ? C23 C231 1.420(8) . ? C23 C233 1.541(7) . ? C23 C233 1.541(7) 2_556 ? C23 C232 1.684(8) 2_556 ? C23 C232 1.684(8) . ? C231 H23A 0.980 . ? C231 H23B 0.980 . ? C231 H23C 0.980 . ? C232 H23D 0.980 . ? C232 H23E 0.980 . ? C232 H23F 0.980 . ? C233 H23G 0.980 . ? C233 H23H 0.980 . ? C233 H23I 0.980 . ? C24 H24A 0.990 . ? C24 H24B 0.990 . ? C25 C26 1.527(8) . ? C25 H25A 0.990 . ? C25 H25B 0.990 . ? C26 C27 1.363(9) . ? C27 C28 1.379(9) . ? C27 H27A 0.950 . ? C28 C29 1.323(8) . ? C28 H28A 0.950 . ? C29 C30 1.372(8) . ? C29 H29A 0.950 . ? C30 H30A 0.950 . ? C31 C32 1.471(8) . ? C31 H31A 0.990 . ? C31 H31B 0.990 . ? C32 C33 1.371(8) . ? C33 C34 1.378(9) . ? C33 H33A 0.950 . ? C34 C35 1.411(9) . ? C34 H34A 0.950 . ? C35 C36 1.364(8) . ? C35 H35A 0.950 . ? C36 H36A 0.950 . ? Cl1 O1B 1.353(6) 2 ? Cl1 O1B 1.353(6) . ? Cl1 O1A 1.376(5) 2 ? Cl1 O1A 1.376(5) . ? Cl2 O2B 1.329(14) 2_556 ? Cl2 O2C 1.350(6) . ? Cl2 O2B 1.353(10) . ? Cl2 O2A 1.383(10) . ? O2B Cl2 1.329(14) 2_556 ? O2C Cl2 1.350(6) 2_556 ? 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 O4 103.07(17) . . ? O2 V1 O3 101.83(17) . . ? O4 V1 O3 44.82(15) . . ? O2 V1 N3 90.00(17) . . ? O4 V1 N3 126.38(16) . . ? O3 V1 N3 81.75(16) . . ? O2 V1 N2 91.15(18) . . ? O4 V1 N2 80.86(16) . . ? O3 V1 N2 125.62(16) . . ? N3 V1 N2 151.58(15) . . ? O2 V1 N1 86.61(17) . . ? O4 V1 N1 154.18(16) . . ? O3 V1 N1 156.90(16) . . ? N3 V1 N1 76.74(15) . . ? N2 V1 N1 74.99(15) . . ? O2 V1 O1 167.61(16) . . ? O4 V1 O1 89.32(15) . . ? O3 V1 O1 87.10(12) . . ? N3 V1 O1 82.72(15) . . ? N2 V1 O1 90.54(13) . . ? N1 V1 O1 81.97(13) . . ? C1 O1 V1 112.66(10) . . ? C1 O1 V1 112.66(10) . 2_655 ? V1 O1 V1 134.7(2) . 2_655 ? O4 O3 V1 67.2(2) . . ? O3 O4 V1 68.0(2) . . ? C13 N1 C7 110.3(4) . . ? C13 N1 C6 110.0(4) . . ? C7 N1 C6 106.7(4) . . ? C13 N1 V1 106.7(3) . . ? C7 N1 V1 105.8(3) . . ? C6 N1 V1 117.2(3) . . ? C12 N2 C8 118.8(4) . . ? C12 N2 V1 125.4(3) . . ? C8 N2 V1 115.8(3) . . ? C14 N3 C18 117.8(4) . . ? C14 N3 V1 116.4(3) . . ? C18 N3 V1 125.7(3) . . ? O1 C1 C2 121.6(3) . 2_655 ? O1 C1 C2 121.6(3) . . ? C2 C1 C2 116.9(6) 2_655 . ? C3 C2 C1 120.6(5) . . ? C3 C2 C6 124.0(5) . . ? C1 C2 C6 115.2(4) . . ? C2 C3 C4 123.6(5) . . ? C2 C3 H3A 118.2 . . ? C4 C3 H3A 118.2 . . ? C3 C4 C3 114.6(6) 2_655 . ? C3 C4 C5 122.7(3) 2_655 . ? C3 C4 C5 122.7(3) . . ? C51 C5 C51 131.6(10) . 2_655 ? C51 C5 C4 114.2(5) . . ? C51 C5 C4 114.2(5) 2_655 . ? C51 C5 C53 50.3(6) . 2_655 ? C51 C5 C53 113.1(6) 2_655 2_655 ? C4 C5 C53 107.4(5) . 2_655 ? C51 C5 C53 113.1(6) . . ? C51 C5 C53 50.3(6) 2_655 . ? C4 C5 C53 107.4(5) . . ? C53 C5 C53 145.1(9) 2_655 . ? C51 C5 C52 54.4(6) . 2_655 ? C51 C5 C52 110.1(6) 2_655 2_655 ? C4 C5 C52 106.8(5) . 2_655 ? C53 C5 C52 104.5(5) 2_655 2_655 ? C53 C5 C52 64.9(5) . 2_655 ? C51 C5 C52 110.1(6) . . ? C51 C5 C52 54.4(6) 2_655 . ? C4 C5 C52 106.8(5) . . ? C53 C5 C52 64.9(5) 2_655 . ? C53 C5 C52 104.5(5) . . ? C52 C5 C52 146.3(9) 2_655 . ? C5 C51 H51A 109.5 . . ? C5 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C5 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C5 C52 H52A 109.5 . . ? C5 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C5 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C5 C53 H53A 109.5 . . ? C5 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C5 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N1 C6 C2 110.7(4) . . ? N1 C6 H6A 109.5 . . ? C2 C6 H6A 109.5 . . ? N1 C6 H6B 109.5 . . ? C2 C6 H6B 109.5 . . ? H6A C6 H6B 108.1 . . ? C8 C7 N1 108.7(4) . . ? C8 C7 H7A 109.9 . . ? N1 C7 H7A 109.9 . . ? C8 C7 H7B 109.9 . . ? N1 C7 H7B 109.9 . . ? H7A C7 H7B 108.3 . . ? C9 C8 N2 120.5(5) . . ? C9 C8 C7 124.9(5) . . ? N2 C8 C7 114.6(5) . . ? C8 C9 C10 120.9(6) . . ? C8 C9 H9A 119.6 . . ? C10 C9 H9A 119.6 . . ? C11 C10 C9 118.1(6) . . ? C11 C10 H10A 120.9 . . ? C9 C10 H10A 120.9 . . ? C12 C11 C10 119.1(6) . . ? C12 C11 H11A 120.4 . . ? C10 C11 H11A 120.4 . . ? N2 C12 C11 122.5(5) . . ? N2 C12 H12A 118.8 . . ? C11 C12 H12A 118.8 . . ? N1 C13 C14 110.5(4) . . ? N1 C13 H13A 109.6 . . ? C14 C13 H13A 109.6 . . ? N1 C13 H13B 109.6 . . ? C14 C13 H13B 109.6 . . ? H13A C13 H13B 108.1 . . ? N3 C14 C15 122.3(5) . . ? N3 C14 C13 115.4(5) . . ? C15 C14 C13 122.3(5) . . ? C16 C15 C14 118.7(6) . . ? C16 C15 H15A 120.6 . . ? C14 C15 H15A 120.6 . . ? C15 C16 C17 119.8(6) . . ? C15 C16 H16A 120.1 . . ? C17 C16 H16A 120.1 . . ? C18 C17 C16 119.0(5) . . ? C18 C17 H17A 120.5 . . ? C16 C17 H17A 120.5 . . ? N3 C18 C17 122.2(5) . . ? N3 C18 H18A 118.9 . . ? C17 C18 H18A 118.9 . . ? O6 V2 O8 103.57(19) . . ? O6 V2 O7 102.26(18) . . ? O8 V2 O7 45.00(15) . . ? O6 V2 N5 90.1(2) . . ? O8 V2 N5 125.97(17) . . ? O7 V2 N5 81.17(17) . . ? O6 V2 N6 91.94(19) . . ? O8 V2 N6 80.65(16) . . ? O7 V2 N6 125.55(17) . . ? N5 V2 N6 151.88(17) . . ? O6 V2 N4 87.65(19) . . ? O8 V2 N4 153.86(17) . . ? O7 V2 N4 155.77(17) . . ? N5 V2 N4 76.70(17) . . ? N6 V2 N4 75.37(16) . . ? O6 V2 O5 168.45(18) . . ? O8 V2 O5 87.98(16) . . ? O7 V2 O5 85.69(12) . . ? N5 V2 O5 82.77(16) . . ? N6 V2 O5 90.12(13) . . ? N4 V2 O5 81.88(14) . . ? C19 O5 V2 113.17(11) . 2_556 ? C19 O5 V2 113.17(10) . . ? V2 O5 V2 133.7(2) 2_556 . ? O8 O7 V2 67.4(2) . . ? O7 O8 V2 67.7(2) . . ? C31 N4 C25 112.2(5) . . ? C31 N4 C24 110.9(4) . . ? C25 N4 C24 105.2(4) . . ? C31 N4 V2 105.8(3) . . ? C25 N4 V2 105.3(3) . . ? C24 N4 V2 117.5(4) . . ? C36 N5 C32 118.5(5) . . ? C36 N5 V2 125.9(4) . . ? C32 N5 V2 115.6(4) . . ? C26 N6 C30 116.6(5) . . ? C26 N6 V2 117.2(4) . . ? C30 N6 V2 126.2(4) . . ? C20 C19 C20 120.1(7) . 2_556 ? C20 C19 O5 120.0(3) . . ? C20 C19 O5 120.0(3) 2_556 . ? C19 C20 C21 120.2(6) . . ? C19 C20 C24 117.7(5) . . ? C21 C20 C24 122.1(6) . . ? C20 C21 C22 121.3(7) . . ? C20 C21 H21A 119.3 . . ? C22 C21 H21A 119.3 . . ? C21 C22 C21 116.7(8) . 2_556 ? C21 C22 C23 121.6(4) . . ? C21 C22 C23 121.6(4) 2_556 . ? C231 C23 C231 124.9(12) 2_556 . ? C231 C23 C22 117.6(6) 2_556 . ? C231 C23 C22 117.6(6) . . ? C231 C23 C233 119.5(7) . . ? C22 C23 C233 109.3(5) . . ? C231 C23 C233 119.5(7) 2_556 2_556 ? C22 C23 C233 109.3(5) . 2_556 ? C233 C23 C233 141.4(10) . 2_556 ? C231 C23 C232 106.4(6) 2_556 2_556 ? C22 C23 C232 104.3(5) . 2_556 ? C233 C23 C232 74.3(5) . 2_556 ? C233 C23 C232 96.1(5) 2_556 2_556 ? C231 C23 C232 106.4(6) . . ? C22 C23 C232 104.3(5) . . ? C233 C23 C232 96.1(5) . . ? C233 C23 C232 74.3(5) 2_556 . ? C232 C23 C232 151.3(10) 2_556 . ? C23 C231 H23A 109.5 . . ? C23 C231 H23B 109.5 . . ? H23A C231 H23B 109.5 . . ? C23 C231 H23C 109.5 . . ? H23A C231 H23C 109.5 . . ? H23B C231 H23C 109.5 . . ? C23 C232 H23D 109.5 . . ? C23 C232 H23E 109.5 . . ? H23D C232 H23E 109.5 . . ? C23 C232 H23F 109.5 . . ? H23D C232 H23F 109.5 . . ? H23E C232 H23F 109.5 . . ? C23 C233 H23G 109.5 . . ? C23 C233 H23H 109.5 . . ? H23G C233 H23H 109.5 . . ? C23 C233 H23I 109.5 . . ? H23G C233 H23I 109.5 . . ? H23H C233 H23I 109.5 . . ? N4 C24 C20 109.5(5) . . ? N4 C24 H24A 109.8 . . ? C20 C24 H24A 109.8 . . ? N4 C24 H24B 109.8 . . ? C20 C24 H24B 109.8 . . ? H24A C24 H24B 108.2 . . ? N4 C25 C26 108.1(5) . . ? N4 C25 H25A 110.1 . . ? C26 C25 H25A 110.1 . . ? N4 C25 H25B 110.1 . . ? C26 C25 H25B 110.1 . . ? H25A C25 H25B 108.4 . . ? N6 C26 C27 123.2(6) . . ? N6 C26 C25 113.1(5) . . ? C27 C26 C25 123.7(6) . . ? C26 C27 C28 118.7(6) . . ? C26 C27 H27A 120.7 . . ? C28 C27 H27A 120.7 . . ? C29 C28 C27 118.7(6) . . ? C29 C28 H28A 120.6 . . ? C27 C28 H28A 120.6 . . ? C28 C29 C30 121.6(6) . . ? C28 C29 H29A 119.2 . . ? C30 C29 H29A 119.2 . . ? N6 C30 C29 120.9(6) . . ? N6 C30 H30A 119.5 . . ? C29 C30 H30A 119.5 . . ? C32 C31 N4 112.0(5) . . ? C32 C31 H31A 109.2 . . ? N4 C31 H31A 109.2 . . ? C32 C31 H31B 109.2 . . ? N4 C31 H31B 109.2 . . ? H31A C31 H31B 107.9 . . ? N5 C32 C33 120.5(5) . . ? N5 C32 C31 115.7(5) . . ? C33 C32 C31 123.8(5) . . ? C32 C33 C34 121.2(6) . . ? C32 C33 H33A 119.4 . . ? C34 C33 H33A 119.4 . . ? C33 C34 C35 117.7(6) . . ? C33 C34 H34A 121.1 . . ? C35 C34 H34A 121.1 . . ? C36 C35 C34 118.3(6) . . ? C36 C35 H35A 120.9 . . ? C34 C35 H35A 120.9 . . ? N5 C36 C35 123.6(6) . . ? N5 C36 H36A 118.2 . . ? C35 C36 H36A 118.2 . . ? O1B Cl1 O1B 100.6(8) 2 . ? O1B Cl1 O1A 113.5(5) 2 2 ? O1B Cl1 O1A 109.2(4) . 2 ? O1B Cl1 O1A 109.2(4) 2 . ? O1B Cl1 O1A 113.5(5) . . ? O1A Cl1 O1A 110.5(4) 2 . ? O2B Cl2 O2C 114.4(8) 2_556 . ? O2B Cl2 O2B 125.0(6) 2_556 . ? O2C Cl2 O2B 112.9(7) . . ? O2B Cl2 O2A 90.2(7) 2_556 . ? O2C Cl2 O2A 108.7(5) . . ? O2B Cl2 O2A 99.8(7) . . ? O2B Cl2 O2A 82.0(6) 2_556 2_556 ? O2C Cl2 O2A 88.0(5) . 2_556 ? O2B Cl2 O2A 73.2(5) . 2_556 ? O2A Cl2 O2A 163.2(7) . 2_556 ? 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 O1 C1 26.4(7) . . . . ? O4 V1 O1 C1 -154.87(11) . . . . ? O3 V1 O1 C1 -110.08(11) . . . . ? N3 V1 O1 C1 -28.03(11) . . . . ? N2 V1 O1 C1 124.28(11) . . . . ? N1 V1 O1 C1 49.52(11) . . . . ? O2 V1 O1 V1 -153.6(7) . . . 2_655 ? O4 V1 O1 V1 25.13(11) . . . 2_655 ? O3 V1 O1 V1 69.92(11) . . . 2_655 ? N3 V1 O1 V1 151.96(11) . . . 2_655 ? N2 V1 O1 V1 -55.72(11) . . . 2_655 ? N1 V1 O1 V1 -130.48(11) . . . 2_655 ? O2 V1 O3 O4 96.7(2) . . . . ? N3 V1 O3 O4 -175.0(2) . . . . ? N2 V1 O3 O4 -3.4(3) . . . . ? N1 V1 O3 O4 -153.6(4) . . . . ? O1 V1 O3 O4 -92.0(2) . . . . ? O2 V1 O4 O3 -93.7(2) . . . . ? N3 V1 O4 O3 6.1(3) . . . . ? N2 V1 O4 O3 177.2(2) . . . . ? N1 V1 O4 O3 156.4(3) . . . . ? O1 V1 O4 O3 86.6(2) . . . . ? O2 V1 N1 C13 60.2(3) . . . . ? O4 V1 N1 C13 173.7(3) . . . . ? O3 V1 N1 C13 -52.4(6) . . . . ? N3 V1 N1 C13 -30.6(3) . . . . ? N2 V1 N1 C13 152.4(3) . . . . ? O1 V1 N1 C13 -114.9(3) . . . . ? O2 V1 N1 C7 -57.3(3) . . . . ? O4 V1 N1 C7 56.2(5) . . . . ? O3 V1 N1 C7 -169.9(4) . . . . ? N3 V1 N1 C7 -148.1(3) . . . . ? N2 V1 N1 C7 34.8(3) . . . . ? O1 V1 N1 C7 127.6(3) . . . . ? O2 V1 N1 C6 -176.1(3) . . . . ? O4 V1 N1 C6 -62.6(5) . . . . ? O3 V1 N1 C6 71.3(5) . . . . ? N3 V1 N1 C6 93.1(3) . . . . ? N2 V1 N1 C6 -84.0(3) . . . . ? O1 V1 N1 C6 8.8(3) . . . . ? O2 V1 N2 C12 -110.3(4) . . . . ? O4 V1 N2 C12 -7.2(4) . . . . ? O3 V1 N2 C12 -4.8(5) . . . . ? N3 V1 N2 C12 157.6(4) . . . . ? N1 V1 N2 C12 163.5(5) . . . . ? O1 V1 N2 C12 82.0(4) . . . . ? O2 V1 N2 C8 68.7(4) . . . . ? O4 V1 N2 C8 171.8(4) . . . . ? O3 V1 N2 C8 174.2(3) . . . . ? N3 V1 N2 C8 -23.4(6) . . . . ? N1 V1 N2 C8 -17.4(4) . . . . ? O1 V1 N2 C8 -99.0(4) . . . . ? O2 V1 N3 C14 -69.8(4) . . . . ? O4 V1 N3 C14 -176.1(3) . . . . ? O3 V1 N3 C14 -171.8(4) . . . . ? N2 V1 N3 C14 22.6(6) . . . . ? N1 V1 N3 C14 16.7(4) . . . . ? O1 V1 N3 C14 100.1(4) . . . . ? O2 V1 N3 C18 108.1(4) . . . . ? O4 V1 N3 C18 1.8(5) . . . . ? O3 V1 N3 C18 6.1(4) . . . . ? N2 V1 N3 C18 -159.5(4) . . . . ? N1 V1 N3 C18 -165.4(4) . . . . ? O1 V1 N3 C18 -82.0(4) . . . . ? V1 O1 C1 C2 115.3(2) . . . 2_655 ? V1 O1 C1 C2 -64.7(2) 2_655 . . 2_655 ? V1 O1 C1 C2 -64.7(2) . . . . ? V1 O1 C1 C2 115.3(2) 2_655 . . . ? O1 C1 C2 C3 -179.7(4) . . . . ? C2 C1 C2 C3 0.3(4) 2_655 . . . ? O1 C1 C2 C6 4.6(5) . . . . ? C2 C1 C2 C6 -175.4(5) 2_655 . . . ? C1 C2 C3 C4 -0.7(8) . . . . ? C6 C2 C3 C4 174.6(4) . . . . ? C2 C3 C4 C3 0.3(4) . . . 2_655 ? C2 C3 C4 C5 -179.7(4) . . . . ? C3 C4 C5 C51 1.0(6) 2_655 . . . ? C3 C4 C5 C51 -179.0(6) . . . . ? C3 C4 C5 C51 -179.0(6) 2_655 . . 2_655 ? C3 C4 C5 C51 1.0(6) . . . 2_655 ? C3 C4 C5 C53 54.7(6) 2_655 . . 2_655 ? C3 C4 C5 C53 -125.3(6) . . . 2_655 ? C3 C4 C5 C53 -125.3(6) 2_655 . . . ? C3 C4 C5 C53 54.7(6) . . . . ? C3 C4 C5 C52 -57.0(5) 2_655 . . 2_655 ? C3 C4 C5 C52 123.0(5) . . . 2_655 ? C3 C4 C5 C52 123.0(5) 2_655 . . . ? C3 C4 C5 C52 -57.0(5) . . . . ? C13 N1 C6 C2 61.0(5) . . . . ? C7 N1 C6 C2 -179.3(4) . . . . ? V1 N1 C6 C2 -61.0(5) . . . . ? C3 C2 C6 N1 -110.3(6) . . . . ? C1 C2 C6 N1 65.2(5) . . . . ? C13 N1 C7 C8 -163.0(4) . . . . ? C6 N1 C7 C8 77.5(5) . . . . ? V1 N1 C7 C8 -48.0(4) . . . . ? C12 N2 C8 C9 -3.3(8) . . . . ? V1 N2 C8 C9 177.6(4) . . . . ? C12 N2 C8 C7 174.3(5) . . . . ? V1 N2 C8 C7 -4.8(6) . . . . ? N1 C7 C8 C9 -146.2(5) . . . . ? N1 C7 C8 N2 36.2(6) . . . . ? N2 C8 C9 C10 1.0(9) . . . . ? C7 C8 C9 C10 -176.5(5) . . . . ? C8 C9 C10 C11 2.0(9) . . . . ? C9 C10 C11 C12 -2.5(8) . . . . ? C8 N2 C12 C11 2.8(8) . . . . ? V1 N2 C12 C11 -178.2(4) . . . . ? C10 C11 C12 N2 0.2(8) . . . . ? C7 N1 C13 C14 154.7(4) . . . . ? C6 N1 C13 C14 -87.8(5) . . . . ? V1 N1 C13 C14 40.3(5) . . . . ? C18 N3 C14 C15 1.1(8) . . . . ? V1 N3 C14 C15 179.2(4) . . . . ? C18 N3 C14 C13 -176.7(4) . . . . ? V1 N3 C14 C13 1.4(6) . . . . ? N1 C13 C14 N3 -29.1(6) . . . . ? N1 C13 C14 C15 153.0(5) . . . . ? N3 C14 C15 C16 1.3(9) . . . . ? C13 C14 C15 C16 179.0(5) . . . . ? C14 C15 C16 C17 -3.4(9) . . . . ? C15 C16 C17 C18 3.0(9) . . . . ? C14 N3 C18 C17 -1.6(8) . . . . ? V1 N3 C18 C17 -179.4(4) . . . . ? C16 C17 C18 N3 -0.5(9) . . . . ? O6 V2 O5 C19 -23.3(8) . . . . ? O8 V2 O5 C19 155.72(11) . . . . ? O7 V2 O5 C19 110.71(11) . . . . ? N5 V2 O5 C19 29.08(12) . . . . ? N6 V2 O5 C19 -123.63(12) . . . . ? N4 V2 O5 C19 -48.44(12) . . . . ? O6 V2 O5 V2 156.7(8) . . . 2_556 ? O8 V2 O5 V2 -24.27(11) . . . 2_556 ? O7 V2 O5 V2 -69.29(11) . . . 2_556 ? N5 V2 O5 V2 -150.92(12) . . . 2_556 ? N6 V2 O5 V2 56.37(12) . . . 2_556 ? N4 V2 O5 V2 131.56(12) . . . 2_556 ? O6 V2 O7 O8 -97.0(2) . . . . ? N5 V2 O7 O8 174.8(2) . . . . ? N6 V2 O7 O8 4.4(3) . . . . ? N4 V2 O7 O8 150.6(4) . . . . ? O5 V2 O7 O8 91.5(2) . . . . ? O6 V2 O8 O7 93.9(2) . . . . ? N5 V2 O8 O7 -6.4(3) . . . . ? N6 V2 O8 O7 -176.4(2) . . . . ? N4 V2 O8 O7 -152.8(4) . . . . ? O5 V2 O8 O7 -85.9(2) . . . . ? O6 V2 N4 C31 -60.8(4) . . . . ? O8 V2 N4 C31 -177.5(4) . . . . ? O7 V2 N4 C31 54.5(6) . . . . ? N5 V2 N4 C31 29.9(4) . . . . ? N6 V2 N4 C31 -153.4(4) . . . . ? O5 V2 N4 C31 114.3(4) . . . . ? O6 V2 N4 C25 58.2(4) . . . . ? O8 V2 N4 C25 -58.5(6) . . . . ? O7 V2 N4 C25 173.5(4) . . . . ? N5 V2 N4 C25 148.9(4) . . . . ? N6 V2 N4 C25 -34.4(3) . . . . ? O5 V2 N4 C25 -126.7(3) . . . . ? O6 V2 N4 C24 174.9(4) . . . . ? O8 V2 N4 C24 58.2(6) . . . . ? O7 V2 N4 C24 -69.9(6) . . . . ? N5 V2 N4 C24 -94.5(4) . . . . ? N6 V2 N4 C24 82.2(4) . . . . ? O5 V2 N4 C24 -10.0(4) . . . . ? O6 V2 N5 C36 -108.1(5) . . . . ? O8 V2 N5 C36 -1.1(5) . . . . ? O7 V2 N5 C36 -5.7(5) . . . . ? N6 V2 N5 C36 157.6(4) . . . . ? N4 V2 N5 C36 164.4(5) . . . . ? O5 V2 N5 C36 81.1(4) . . . . ? O6 V2 N5 C32 71.2(4) . . . . ? O8 V2 N5 C32 178.1(4) . . . . ? O7 V2 N5 C32 173.6(4) . . . . ? N6 V2 N5 C32 -23.1(6) . . . . ? N4 V2 N5 C32 -16.4(4) . . . . ? O5 V2 N5 C32 -99.7(4) . . . . ? O6 V2 N6 C26 -71.9(4) . . . . ? O8 V2 N6 C26 -175.4(4) . . . . ? O7 V2 N6 C26 -178.5(4) . . . . ? N5 V2 N6 C26 22.0(6) . . . . ? N4 V2 N6 C26 15.1(4) . . . . ? O5 V2 N6 C26 96.7(4) . . . . ? O6 V2 N6 C30 109.0(5) . . . . ? O8 V2 N6 C30 5.5(4) . . . . ? O7 V2 N6 C30 2.4(5) . . . . ? N5 V2 N6 C30 -157.1(4) . . . . ? N4 V2 N6 C30 -164.0(5) . . . . ? O5 V2 N6 C30 -82.4(5) . . . . ? V2 O5 C19 C20 -117.0(3) 2_556 . . . ? V2 O5 C19 C20 63.0(3) . . . . ? V2 O5 C19 C20 63.0(3) 2_556 . . 2_556 ? V2 O5 C19 C20 -117.0(3) . . . 2_556 ? C20 C19 C20 C21 -0.7(4) 2_556 . . . ? O5 C19 C20 C21 179.3(4) . . . . ? C20 C19 C20 C24 177.2(5) 2_556 . . . ? O5 C19 C20 C24 -2.8(5) . . . . ? C19 C20 C21 C22 1.3(8) . . . . ? C24 C20 C21 C22 -176.4(5) . . . . ? C20 C21 C22 C21 -0.7(4) . . . 2_556 ? C20 C21 C22 C23 179.3(4) . . . . ? C21 C22 C23 C231 -119.8(7) . . . 2_556 ? C21 C22 C23 C231 60.2(7) 2_556 . . 2_556 ? C21 C22 C23 C231 60.2(7) . . . . ? C21 C22 C23 C231 -119.8(7) 2_556 . . . ? C21 C22 C23 C233 -80.3(5) . . . . ? C21 C22 C23 C233 99.7(5) 2_556 . . . ? C21 C22 C23 C233 99.7(5) . . . 2_556 ? C21 C22 C23 C233 -80.3(5) 2_556 . . 2_556 ? C21 C22 C23 C232 -2.2(5) . . . 2_556 ? C21 C22 C23 C232 177.8(5) 2_556 . . 2_556 ? C21 C22 C23 C232 177.8(5) . . . . ? C21 C22 C23 C232 -2.2(5) 2_556 . . . ? C31 N4 C24 C20 -60.1(6) . . . . ? C25 N4 C24 C20 178.3(5) . . . . ? V2 N4 C24 C20 61.6(5) . . . . ? C19 C20 C24 N4 -66.2(6) . . . . ? C21 C20 C24 N4 111.6(6) . . . . ? C31 N4 C25 C26 163.3(5) . . . . ? C24 N4 C25 C26 -76.0(5) . . . . ? V2 N4 C25 C26 48.7(5) . . . . ? C30 N6 C26 C27 5.8(9) . . . . ? V2 N6 C26 C27 -173.4(5) . . . . ? C30 N6 C26 C25 -172.6(5) . . . . ? V2 N6 C26 C25 8.2(6) . . . . ? N4 C25 C26 N6 -39.1(7) . . . . ? N4 C25 C26 C27 142.5(6) . . . . ? N6 C26 C27 C28 -3.4(10) . . . . ? C25 C26 C27 C28 174.8(6) . . . . ? C26 C27 C28 C29 -1.1(10) . . . . ? C27 C28 C29 C30 2.9(10) . . . . ? C26 N6 C30 C29 -3.8(8) . . . . ? V2 N6 C30 C29 175.3(4) . . . . ? C28 C29 C30 N6 -0.4(9) . . . . ? C25 N4 C31 C32 -154.7(5) . . . . ? C24 N4 C31 C32 88.0(6) . . . . ? V2 N4 C31 C32 -40.4(5) . . . . ? C36 N5 C32 C33 -2.6(8) . . . . ? V2 N5 C32 C33 178.1(5) . . . . ? C36 N5 C32 C31 177.7(5) . . . . ? V2 N5 C32 C31 -1.7(6) . . . . ? N4 C31 C32 N5 29.8(7) . . . . ? N4 C31 C32 C33 -150.0(6) . . . . ? N5 C32 C33 C34 0.9(9) . . . . ? C31 C32 C33 C34 -179.4(6) . . . . ? C32 C33 C34 C35 1.9(10) . . . . ? C33 C34 C35 C36 -3.0(10) . . . . ? C32 N5 C36 C35 1.4(9) . . . . ? V2 N5 C36 C35 -179.3(4) . . . . ? C34 C35 C36 N5 1.4(9) . . . . ? #===END #------------------------------------------------------------------------ data_3 _database_code_depnum_ccdc_archive 'CCDC 717961' _chemical_name_systematic ? _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ; C36 H41 N6 O5 V2 2+, 2(Cl O4 -), 2(H2 O), C2 H6 O ; _chemical_formula_sum 'C38 H51 Cl2 N6 O16 V2' _chemical_formula_weight 1020.63 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' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.740(3) _cell_length_b 11.952(3) _cell_length_c 17.766(4) _cell_angle_alpha 91.023(5) _cell_angle_beta 99.366(5) _cell_angle_gamma 101.768(5) _cell_volume 2199.7(10) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1119 _cell_measurement_theta_min 2.48 _cell_measurement_theta_max 24.25 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.02 _exptl_crystal_size_mid 0.02 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.541 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1058 _exptl_absorpt_coefficient_mu 0.624 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.709 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_process_details ; SADABS v.2.05 (Sheldrick, 2002) Ratio of minimum to maximum apparent transmission: 0.717897 The transmission factors are not real since they include corrections for beam decay and possibly crystal decay (the two cannot be distinguished). ; _exptl_special_details ; H atoms associated with water molecule bound to V were located in a difference Fourier map and refined with the O---H distances restrained to a common refined value and the H...H distance restrained to 1.60 times that value. The H atoms of the lattice water molecules were placed so as to form a reasonable hydrogen-bond network and subsequently allowed to ride on their parent O atom with U~iso~(H) = 1.5 x U~eq~(O). The hydroxyl H atom of the ethanol molecule was placed geometrically and allowed to rotate about the C---O bond (AFIX 147). The perchlorate anions were restrained to form regular tetrahedra (although removal of these restraints leads only to a very small distortion). The highest residual peak is associated with one perchlorate anion. The ethanol molecule is clear in the difference Fourier map and was refined with bond distances and the 1,3-distance restrained. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.8974 _diffrn_radiation_type synchrotron _diffrn_radiation_source ; Beamline I711 at the MAX-II storage ring: MAX-Lab, Lund, Sweden ; _diffrn_radiation_monochromator 'Silicon 111' _diffrn_measurement_device_type 'Bruker SMART1000 CCD' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_standards_number 0 _diffrn_standards_interval_count . _diffrn_standards_interval_time . _diffrn_standards_decay_% ? _diffrn_reflns_number 14402 _diffrn_reflns_av_R_equivalents 0.0568 _diffrn_reflns_av_sigmaI/netI 0.0936 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 29.90 _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 29.90 _diffrn_measured_fraction_theta_full 0.992 _reflns_number_total 6271 _reflns_number_gt 3696 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'SMART v.5.628 (Bruker, 2002)' _computing_cell_refinement 'SAINT v.6.36 (Bruker, 2002)' _computing_data_reduction 'SAINT v.6.36' _computing_structure_solution 'SHELXTL v.6.10 (Sheldrick, 2000)' _computing_structure_refinement 'SHELXTL v.6.10' _computing_molecular_graphics 'SHELXTL v.6.10' _computing_publication_material 'SHELXTL v.6.10' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1512P)^2^] 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 6271 _refine_ls_number_parameters 565 _refine_ls_number_restraints 25 _refine_ls_R_factor_all 0.1194 _refine_ls_R_factor_gt 0.0757 _refine_ls_wR_factor_ref 0.2300 _refine_ls_wR_factor_gt 0.2081 _refine_ls_goodness_of_fit_ref 0.941 _refine_ls_restrained_S_all 0.949 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_diff_density_max 1.295 _refine_diff_density_min -1.072 _refine_diff_density_rms 0.097 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 0.57302(12) 0.70406(11) 0.84175(7) 0.0448(4) Uani 1 1 d . . . V2 V 0.23331(11) 0.79309(10) 0.81247(6) 0.0415(4) Uani 1 1 d . . . O1 O 0.3817(4) 0.7575(4) 0.7699(2) 0.0383(11) Uani 1 1 d . . . O2 O 0.7035(4) 0.6614(4) 0.8750(3) 0.0512(13) Uani 1 1 d . . . O3 O 0.5698(4) 0.8111(4) 0.9016(3) 0.0510(13) Uani 1 1 d . . . O4 O 0.1866(5) 0.6876(4) 0.8613(3) 0.0547(14) Uani 1 1 d . . . O5 O 0.3649(5) 0.9027(5) 0.8829(3) 0.0516(15) Uani 1 1 d D . . H1 H 0.434(6) 0.876(7) 0.894(4) 0.077 Uiso 1 1 d D . . H2 H 0.350(7) 0.931(7) 0.925(3) 0.077 Uiso 1 1 d D . . N1 N 0.5206(5) 0.5703(5) 0.7465(3) 0.0450(15) Uani 1 1 d . . . N2 N 0.4496(5) 0.5724(5) 0.8839(3) 0.0428(15) Uani 1 1 d . . . N3 N 0.6513(5) 0.7894(5) 0.7539(3) 0.0437(15) Uani 1 1 d . . . N4 N 0.2289(5) 0.9382(5) 0.7302(3) 0.0384(14) Uani 1 1 d . . . N5 N 0.1071(5) 0.7170(5) 0.7125(3) 0.0443(15) Uani 1 1 d . . . N6 N 0.1013(5) 0.8878(5) 0.8428(3) 0.0448(15) Uani 1 1 d . . . C1 C 0.3753(6) 0.7600(6) 0.6913(4) 0.0374(17) Uani 1 1 d . . . C2 C 0.3798(6) 0.6608(6) 0.6517(4) 0.0398(17) Uani 1 1 d . . . C3 C 0.3710(6) 0.6611(6) 0.5733(4) 0.0434(18) Uani 1 1 d . . . H3A H 0.3740 0.5928 0.5461 0.052 Uiso 1 1 calc R . . C4 C 0.3580(6) 0.7575(6) 0.5326(4) 0.0377(17) Uani 1 1 d . . . C5 C 0.3558(6) 0.8560(6) 0.5750(4) 0.0362(16) Uani 1 1 d . . . H5A H 0.3489 0.9239 0.5491 0.043 Uiso 1 1 calc R . . C6 C 0.3632(6) 0.8586(6) 0.6533(4) 0.0364(16) Uani 1 1 d . . . C7 C 0.3418(6) 0.7582(6) 0.4447(4) 0.0407(17) Uani 1 1 d . . . C8 C 0.2042(6) 0.7736(6) 0.4138(4) 0.050(2) Uani 1 1 d . . . H8A H 0.1414 0.7098 0.4286 0.074 Uiso 1 1 calc R . . H8B H 0.1920 0.7750 0.3580 0.074 Uiso 1 1 calc R . . H8C H 0.1915 0.8458 0.4352 0.074 Uiso 1 1 calc R . . C9 C 0.4401(7) 0.8583(6) 0.4216(4) 0.0477(19) Uani 1 1 d . . . H9A H 0.5277 0.8487 0.4414 0.072 Uiso 1 1 calc R . . H9B H 0.4271 0.9304 0.4429 0.072 Uiso 1 1 calc R . . H9C H 0.4281 0.8596 0.3658 0.072 Uiso 1 1 calc R . . C10 C 0.3593(7) 0.6459(6) 0.4097(4) 0.0466(19) Uani 1 1 d . . . H10A H 0.2963 0.5821 0.4244 0.070 Uiso 1 1 calc R . . H10B H 0.4468 0.6349 0.4285 0.070 Uiso 1 1 calc R . . H10C H 0.3461 0.6485 0.3540 0.070 Uiso 1 1 calc R . . C11 C 0.3928(7) 0.5554(6) 0.6941(4) 0.0429(18) Uani 1 1 d . . . H11A H 0.3835 0.4903 0.6570 0.051 Uiso 1 1 calc R . . H11B H 0.3224 0.5369 0.7245 0.051 Uiso 1 1 calc R . . C12 C 0.5196(7) 0.4618(6) 0.7877(4) 0.0508(19) Uani 1 1 d . . . H12A H 0.6087 0.4561 0.8099 0.061 Uiso 1 1 calc R . . H12B H 0.4808 0.3945 0.7520 0.061 Uiso 1 1 calc R . . C13 C 0.4396(7) 0.4659(6) 0.8508(4) 0.0477(19) Uani 1 1 d . . . C14 C 0.3679(8) 0.3712(7) 0.8760(5) 0.061(2) Uani 1 1 d . . . H14A H 0.3603 0.2981 0.8516 0.073 Uiso 1 1 calc R . . C15 C 0.3065(8) 0.3818(8) 0.9370(5) 0.067(2) Uani 1 1 d . . . H15A H 0.2562 0.3162 0.9551 0.081 Uiso 1 1 calc R . . C16 C 0.3184(7) 0.4881(7) 0.9716(4) 0.053(2) Uani 1 1 d . . . H16A H 0.2789 0.4970 1.0148 0.064 Uiso 1 1 calc R . . C17 C 0.3887(7) 0.5810(7) 0.9423(4) 0.0492(19) Uani 1 1 d . . . H17A H 0.3940 0.6549 0.9649 0.059 Uiso 1 1 calc R . . C18 C 0.6269(7) 0.5967(7) 0.7026(4) 0.050(2) Uani 1 1 d . . . H18A H 0.6001 0.5565 0.6516 0.060 Uiso 1 1 calc R . . H18B H 0.7026 0.5694 0.7293 0.060 Uiso 1 1 calc R . . C19 C 0.6626(6) 0.7213(7) 0.6940(4) 0.0461(18) Uani 1 1 d . . . C20 C 0.7137(7) 0.7721(8) 0.6325(4) 0.056(2) Uani 1 1 d . . . H20A H 0.7214 0.7253 0.5904 0.067 Uiso 1 1 calc R . . C21 C 0.7538(7) 0.8911(8) 0.6319(5) 0.059(2) Uani 1 1 d . . . H21A H 0.7884 0.9258 0.5900 0.071 Uiso 1 1 calc R . . C22 C 0.7416(7) 0.9555(7) 0.6934(5) 0.056(2) Uani 1 1 d . . . H22A H 0.7697 1.0364 0.6953 0.068 Uiso 1 1 calc R . . C23 C 0.6887(6) 0.9037(7) 0.7525(4) 0.0472(19) Uani 1 1 d . . . H23A H 0.6781 0.9502 0.7939 0.057 Uiso 1 1 calc R . . C24 C 0.3521(6) 0.9639(6) 0.6976(4) 0.0401(17) Uani 1 1 d . . . H24A H 0.4271 0.9858 0.7394 0.048 Uiso 1 1 calc R . . H24B H 0.3513 1.0284 0.6635 0.048 Uiso 1 1 calc R . . C25 C 0.1165(6) 0.9053(6) 0.6678(4) 0.0409(17) Uani 1 1 d . . . H25A H 0.1379 0.9417 0.6206 0.049 Uiso 1 1 calc R . . H25B H 0.0424 0.9338 0.6817 0.049 Uiso 1 1 calc R . . C26 C 0.0792(6) 0.7790(6) 0.6530(4) 0.0422(18) Uani 1 1 d . . . C27 C 0.0129(6) 0.7307(7) 0.5826(4) 0.049(2) Uani 1 1 d . . . H27A H -0.0058 0.7774 0.5413 0.059 Uiso 1 1 calc R . . C28 C -0.0261(7) 0.6110(8) 0.5739(5) 0.062(2) Uani 1 1 d . . . H28A H -0.0722 0.5755 0.5264 0.074 Uiso 1 1 calc R . . C29 C 0.0028(7) 0.5463(7) 0.6341(5) 0.060(2) Uani 1 1 d . . . H29A H -0.0222 0.4652 0.6289 0.072 Uiso 1 1 calc R . . C30 C 0.0694(7) 0.6005(7) 0.7031(5) 0.055(2) Uani 1 1 d . . . H30A H 0.0894 0.5553 0.7450 0.067 Uiso 1 1 calc R . . C31 C 0.2158(7) 1.0380(6) 0.7754(4) 0.0452(18) Uani 1 1 d . . . H31A H 0.1888 1.0963 0.7412 0.054 Uiso 1 1 calc R . . H31B H 0.2994 1.0727 0.8077 0.054 Uiso 1 1 calc R . . C32 C 0.1161(7) 0.9976(7) 0.8243(4) 0.0478(19) Uani 1 1 d . . . C33 C 0.0453(7) 1.0713(7) 0.8499(4) 0.056(2) Uani 1 1 d . . . H33A H 0.0584 1.1492 0.8372 0.067 Uiso 1 1 calc R . . C34 C -0.0462(8) 1.0259(9) 0.8952(4) 0.068(3) Uani 1 1 d . . . H34A H -0.0958 1.0738 0.9143 0.081 Uiso 1 1 calc R . . C35 C -0.0648(8) 0.9109(8) 0.9125(4) 0.060(2) Uani 1 1 d . . . H35A H -0.1286 0.8788 0.9417 0.072 Uiso 1 1 calc R . . C36 C 0.0109(7) 0.8460(7) 0.8861(4) 0.053(2) Uani 1 1 d . . . H36A H 0.0000 0.7681 0.8985 0.064 Uiso 1 1 calc R . . Cl2 Cl 0.22708(19) 0.25301(18) 0.59329(12) 0.0599(6) Uani 1 1 d D . . O2A O 0.3161(5) 0.2498(5) 0.6615(3) 0.0622(15) Uani 1 1 d D . . O2B O 0.2826(6) 0.3365(5) 0.5450(3) 0.0806(18) Uani 1 1 d D . . O2C O 0.1983(6) 0.1447(5) 0.5520(3) 0.088(2) Uani 1 1 d D . . O2D O 0.1159(6) 0.2809(7) 0.6108(4) 0.112(3) Uani 1 1 d D . . Cl1 Cl 0.6173(3) 0.1939(2) 0.8773(2) 0.1144(12) Uani 1 1 d D . . O1A O 0.6744(6) 0.3066(5) 0.8997(4) 0.099(2) Uani 1 1 d D . . O1B O 0.5388(9) 0.1871(8) 0.8026(4) 0.148(4) Uani 1 1 d D . . O1C O 0.6961(10) 0.1178(8) 0.8791(7) 0.186(5) Uani 1 1 d D . . O1D O 0.5214(8) 0.1608(8) 0.9291(6) 0.159(4) Uani 1 1 d D . . O1W O 0.2971(6) 1.0135(6) 0.9901(4) 0.096(2) Uani 1 1 d . . . H1W H 0.3355 1.0797 1.0073 0.144 Uiso 1 1 d R . . H2W H 0.2959 0.9702 1.0268 0.144 Uiso 1 1 d R . . O2W O 0.0805(13) 0.3240(11) 0.7664(7) 0.221(6) Uiso 1 1 d . . . H3W H 0.0820 0.2919 0.7242 0.331 Uiso 1 1 d R . . H4W H 0.0038 0.3317 0.7630 0.331 Uiso 1 1 d R . . O1S O -0.0994(18) 0.3755(16) 0.8103(11) 0.295(9) Uiso 1 1 d D . . H1S H -0.1587 0.4043 0.7869 0.442 Uiso 1 1 d R . . C1S C -0.042(3) 0.443(2) 0.8808(12) 0.278(12) Uiso 1 1 d D . . H1S1 H -0.1005 0.4889 0.8970 0.334 Uiso 1 1 calc R . . H1S2 H 0.0417 0.4932 0.8766 0.334 Uiso 1 1 calc R . . C2S C -0.025(3) 0.347(2) 0.9340(14) 0.281(13) Uiso 1 1 d D . . H2S1 H 0.0142 0.3800 0.9854 0.422 Uiso 1 1 calc R . . H2S2 H 0.0316 0.3020 0.9153 0.422 Uiso 1 1 calc R . . H2S3 H -0.1091 0.2977 0.9356 0.422 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 0.0486(8) 0.0454(8) 0.0377(7) -0.0045(6) 0.0040(6) 0.0070(6) V2 0.0410(7) 0.0473(8) 0.0352(7) -0.0017(6) 0.0062(5) 0.0080(6) O1 0.045(3) 0.038(3) 0.031(2) -0.006(2) 0.001(2) 0.010(2) O2 0.048(3) 0.059(3) 0.046(3) 0.002(3) 0.006(2) 0.010(2) O3 0.047(3) 0.055(3) 0.043(3) -0.005(2) -0.004(2) 0.002(2) O4 0.058(3) 0.063(4) 0.045(3) 0.011(3) 0.014(2) 0.013(3) O5 0.041(3) 0.066(4) 0.043(3) -0.022(3) -0.004(2) 0.012(3) N1 0.045(3) 0.048(4) 0.040(3) -0.004(3) 0.000(3) 0.013(3) N2 0.045(3) 0.046(4) 0.033(3) -0.003(3) -0.002(3) 0.008(3) N3 0.034(3) 0.057(4) 0.040(3) 0.001(3) 0.002(3) 0.014(3) N4 0.040(3) 0.038(3) 0.035(3) -0.008(3) 0.005(3) 0.005(3) N5 0.034(3) 0.047(4) 0.048(4) -0.004(3) 0.004(3) 0.001(3) N6 0.038(3) 0.056(4) 0.038(3) -0.002(3) 0.005(3) 0.005(3) C1 0.031(4) 0.044(4) 0.031(4) -0.006(3) 0.000(3) 0.000(3) C2 0.042(4) 0.045(4) 0.029(4) -0.008(3) 0.000(3) 0.005(3) C3 0.038(4) 0.046(5) 0.043(4) -0.012(4) 0.003(3) 0.007(3) C4 0.034(4) 0.045(4) 0.033(4) -0.004(3) 0.006(3) 0.006(3) C5 0.032(4) 0.039(4) 0.035(4) 0.002(3) 0.007(3) 0.002(3) C6 0.030(4) 0.041(4) 0.038(4) -0.005(3) 0.005(3) 0.007(3) C7 0.036(4) 0.049(4) 0.035(4) -0.004(3) 0.005(3) 0.005(3) C8 0.044(4) 0.057(5) 0.040(4) -0.008(4) -0.001(3) 0.002(4) C9 0.044(4) 0.054(5) 0.042(4) 0.000(4) 0.011(3) 0.000(4) C10 0.061(5) 0.045(5) 0.033(4) -0.007(3) 0.012(3) 0.009(4) C11 0.053(4) 0.040(4) 0.034(4) -0.006(3) -0.001(3) 0.012(3) C12 0.055(5) 0.043(5) 0.053(5) -0.001(4) -0.004(4) 0.018(4) C13 0.046(4) 0.048(5) 0.043(4) 0.006(4) -0.002(3) 0.003(4) C14 0.059(5) 0.056(5) 0.061(5) 0.008(4) -0.002(4) 0.003(4) C15 0.047(5) 0.067(6) 0.080(6) 0.018(5) 0.006(5) -0.001(4) C16 0.049(5) 0.057(5) 0.050(5) 0.008(4) 0.001(4) 0.011(4) C17 0.048(5) 0.058(5) 0.041(4) 0.003(4) 0.003(4) 0.014(4) C18 0.056(5) 0.059(5) 0.039(4) -0.006(4) 0.007(4) 0.018(4) C19 0.038(4) 0.057(5) 0.047(4) 0.001(4) 0.007(3) 0.016(4) C20 0.042(4) 0.091(7) 0.039(4) -0.007(4) 0.003(4) 0.025(4) C21 0.046(5) 0.073(6) 0.055(5) 0.014(5) 0.009(4) 0.005(4) C22 0.045(5) 0.054(5) 0.063(5) 0.007(5) -0.002(4) 0.003(4) C23 0.038(4) 0.046(5) 0.052(5) -0.003(4) -0.004(4) 0.006(3) C24 0.036(4) 0.040(4) 0.043(4) -0.002(3) 0.008(3) 0.005(3) C25 0.032(4) 0.052(5) 0.038(4) -0.001(3) 0.002(3) 0.012(3) C26 0.034(4) 0.045(4) 0.047(4) -0.007(4) 0.006(3) 0.006(3) C27 0.035(4) 0.066(6) 0.044(4) -0.013(4) 0.001(3) 0.011(4) C28 0.044(5) 0.073(6) 0.062(6) -0.017(5) -0.003(4) 0.012(4) C29 0.049(5) 0.050(5) 0.074(6) -0.008(5) -0.001(4) 0.003(4) C30 0.048(5) 0.045(5) 0.066(5) 0.001(4) -0.003(4) 0.002(4) C31 0.044(4) 0.042(4) 0.049(4) -0.010(4) 0.007(3) 0.008(3) C32 0.041(4) 0.065(6) 0.037(4) -0.007(4) 0.005(3) 0.011(4) C33 0.050(5) 0.066(6) 0.054(5) -0.006(4) 0.009(4) 0.016(4) C34 0.055(5) 0.105(8) 0.048(5) -0.021(5) 0.013(4) 0.028(5) C35 0.051(5) 0.086(7) 0.044(5) -0.006(5) 0.016(4) 0.011(5) C36 0.048(5) 0.066(5) 0.043(4) -0.006(4) 0.008(4) 0.009(4) Cl2 0.0496(12) 0.0599(14) 0.0623(13) -0.0001(11) -0.0081(10) 0.0078(10) O2A 0.051(3) 0.069(4) 0.055(3) 0.005(3) -0.018(3) 0.008(3) O2B 0.098(5) 0.070(4) 0.063(4) 0.011(3) 0.003(3) 0.002(4) O2C 0.108(5) 0.057(4) 0.078(4) -0.006(3) -0.022(4) 0.002(3) O2D 0.070(5) 0.180(8) 0.095(5) -0.015(5) 0.025(4) 0.041(5) Cl1 0.0820(19) 0.075(2) 0.172(3) -0.023(2) -0.013(2) 0.0111(15) O1A 0.097(5) 0.084(5) 0.105(5) -0.025(4) 0.006(4) 0.004(4) O1B 0.168(9) 0.133(8) 0.122(7) -0.053(6) -0.024(7) 0.025(6) O1C 0.192(10) 0.155(9) 0.251(13) 0.003(9) 0.050(10) 0.122(9) O1D 0.106(7) 0.172(9) 0.217(11) 0.038(8) 0.090(7) 0.013(6) O1W 0.075(4) 0.114(6) 0.092(5) -0.045(4) 0.008(4) 0.016(4) _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 1.614(5) . ? V1 O3 1.658(5) . ? V1 N2 2.075(6) . ? V1 N3 2.078(6) . ? V1 N1 2.227(6) . ? V1 O1 2.444(4) . ? V2 O4 1.587(5) . ? V2 O5 1.972(5) . ? V2 O1 1.987(4) . ? V2 N6 2.113(6) . ? V2 N5 2.116(6) . ? V2 N4 2.291(6) . ? O1 C1 1.389(7) . ? O5 H1 0.86(5) . ? O5 H2 0.86(5) . ? N1 C18 1.470(9) . ? N1 C12 1.500(9) . ? N1 C11 1.504(8) . ? N2 C17 1.327(9) . ? N2 C13 1.369(9) . ? N3 C23 1.345(9) . ? N3 C19 1.363(9) . ? N4 C31 1.469(8) . ? N4 C25 1.482(8) . ? N4 C24 1.508(8) . ? N5 C26 1.331(9) . ? N5 C30 1.367(9) . ? N6 C32 1.342(9) . ? N6 C36 1.358(9) . ? C1 C2 1.382(9) . ? C1 C6 1.387(9) . ? C2 C3 1.381(9) . ? C2 C11 1.499(10) . ? C3 C4 1.390(10) . ? C3 H3A 0.950 . ? C4 C5 1.392(9) . ? C4 C7 1.544(9) . ? C5 C6 1.379(9) . ? C5 H5A 0.950 . ? C6 C24 1.508(9) . ? C7 C10 1.528(9) . ? C7 C9 1.535(9) . ? C7 C8 1.539(10) . ? C8 H8A 0.980 . ? C8 H8B 0.980 . ? C8 H8C 0.980 . ? C9 H9A 0.980 . ? C9 H9B 0.980 . ? C9 H9C 0.980 . ? C10 H10A 0.980 . ? C10 H10B 0.980 . ? C10 H10C 0.980 . ? C11 H11A 0.990 . ? C11 H11B 0.990 . ? C12 C13 1.526(10) . ? C12 H12A 0.990 . ? C12 H12B 0.990 . ? C13 C14 1.360(10) . ? C14 C15 1.373(11) . ? C14 H14A 0.950 . ? C15 C16 1.374(11) . ? C15 H15A 0.950 . ? C16 C17 1.371(10) . ? C16 H16A 0.950 . ? C17 H17A 0.950 . ? C18 C19 1.477(10) . ? C18 H18A 0.990 . ? C18 H18B 0.990 . ? C19 C20 1.396(10) . ? C20 C21 1.400(11) . ? C20 H20A 0.950 . ? C21 C22 1.365(11) . ? C21 H21A 0.950 . ? C22 C23 1.372(10) . ? C22 H22A 0.950 . ? C23 H23A 0.950 . ? C24 H24A 0.990 . ? C24 H24B 0.990 . ? C25 C26 1.488(9) . ? C25 H25A 0.990 . ? C25 H25B 0.990 . ? C26 C27 1.386(9) . ? C27 C28 1.404(11) . ? C27 H27A 0.950 . ? C28 C29 1.364(12) . ? C28 H28A 0.950 . ? C29 C30 1.390(10) . ? C29 H29A 0.950 . ? C30 H30A 0.950 . ? C31 C32 1.497(10) . ? C31 H31A 0.990 . ? C31 H31B 0.990 . ? C32 C33 1.389(10) . ? C33 C34 1.401(11) . ? C33 H33A 0.950 . ? C34 C35 1.395(12) . ? C34 H34A 0.950 . ? C35 C36 1.360(11) . ? C35 H35A 0.950 . ? C36 H36A 0.950 . ? Cl2 O2D 1.384(5) . ? Cl2 O2A 1.423(4) . ? Cl2 O2C 1.427(5) . ? Cl2 O2B 1.429(5) . ? Cl1 O1C 1.361(7) . ? Cl1 O1A 1.383(6) . ? Cl1 O1B 1.443(7) . ? Cl1 O1D 1.490(7) . ? O1W H1W 0.840 . ? O1W H2W 0.840 . ? O2W H3W 0.840 . ? O2W H4W 0.840 . ? O1S C1S 1.451(10) . ? O1S H1S 0.840 . ? C1S C2S 1.515(10) . ? C1S H1S1 0.990 . ? C1S H1S2 0.990 . ? C2S H2S1 0.980 . ? C2S H2S2 0.980 . ? C2S H2S3 0.980 . ? 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 104.8(2) . . ? O2 V1 N2 95.5(2) . . ? O3 V1 N2 99.9(2) . . ? O2 V1 N3 93.7(2) . . ? O3 V1 N3 102.3(2) . . ? N2 V1 N3 152.9(2) . . ? O2 V1 N1 92.1(2) . . ? O3 V1 N1 163.0(2) . . ? N2 V1 N1 76.7(2) . . ? N3 V1 N1 77.5(2) . . ? O2 V1 O1 170.1(2) . . ? O3 V1 O1 83.79(19) . . ? N2 V1 O1 87.66(19) . . ? N3 V1 O1 79.49(18) . . ? N1 V1 O1 79.44(18) . . ? O4 V2 O5 106.1(2) . . ? O4 V2 O1 105.6(2) . . ? O5 V2 O1 85.29(19) . . ? O4 V2 N6 94.4(3) . . ? O5 V2 N6 85.4(2) . . ? O1 V2 N6 159.5(2) . . ? O4 V2 N5 92.3(3) . . ? O5 V2 N5 161.6(2) . . ? O1 V2 N5 89.77(19) . . ? N6 V2 N5 93.4(2) . . ? O4 V2 N4 161.1(2) . . ? O5 V2 N4 87.1(2) . . ? O1 V2 N4 88.63(19) . . ? N6 V2 N4 72.7(2) . . ? N5 V2 N4 75.1(2) . . ? C1 O1 V2 117.2(4) . . ? C1 O1 V1 116.2(4) . . ? V2 O1 V1 126.5(2) . . ? V2 O5 H1 110(5) . . ? V2 O5 H2 123(5) . . ? H1 O5 H2 107(3) . . ? C18 N1 C12 112.6(6) . . ? C18 N1 C11 110.3(5) . . ? C12 N1 C11 106.9(5) . . ? C18 N1 V1 104.3(4) . . ? C12 N1 V1 102.7(4) . . ? C11 N1 V1 119.9(4) . . ? C17 N2 C13 118.2(6) . . ? C17 N2 V1 126.3(5) . . ? C13 N2 V1 115.3(5) . . ? C23 N3 C19 119.7(6) . . ? C23 N3 V1 124.8(5) . . ? C19 N3 V1 115.5(5) . . ? C31 N4 C25 110.0(5) . . ? C31 N4 C24 110.6(5) . . ? C25 N4 C24 110.1(5) . . ? C31 N4 V2 106.3(4) . . ? C25 N4 V2 109.8(4) . . ? C24 N4 V2 110.1(4) . . ? C26 N5 C30 118.2(6) . . ? C26 N5 V2 120.9(5) . . ? C30 N5 V2 120.1(5) . . ? C32 N6 C36 118.8(7) . . ? C32 N6 V2 118.0(5) . . ? C36 N6 V2 122.9(5) . . ? C2 C1 C6 120.7(6) . . ? C2 C1 O1 118.0(6) . . ? C6 C1 O1 121.2(6) . . ? C3 C2 C1 118.8(7) . . ? C3 C2 C11 121.5(6) . . ? C1 C2 C11 119.7(6) . . ? C2 C3 C4 122.5(6) . . ? C2 C3 H3A 118.7 . . ? C4 C3 H3A 118.7 . . ? C3 C4 C5 116.7(6) . . ? C3 C4 C7 123.3(6) . . ? C5 C4 C7 119.9(6) . . ? C6 C5 C4 122.4(7) . . ? C6 C5 H5A 118.8 . . ? C4 C5 H5A 118.8 . . ? C5 C6 C1 118.9(6) . . ? C5 C6 C24 121.6(6) . . ? C1 C6 C24 119.5(6) . . ? C10 C7 C9 109.6(6) . . ? C10 C7 C8 108.3(5) . . ? C9 C7 C8 109.4(6) . . ? C10 C7 C4 111.7(6) . . ? C9 C7 C4 109.7(5) . . ? C8 C7 C4 108.1(5) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C2 C11 N1 112.0(6) . . ? C2 C11 H11A 109.2 . . ? N1 C11 H11A 109.2 . . ? C2 C11 H11B 109.2 . . ? N1 C11 H11B 109.2 . . ? H11A C11 H11B 107.9 . . ? N1 C12 C13 107.0(6) . . ? N1 C12 H12A 110.3 . . ? C13 C12 H12A 110.3 . . ? N1 C12 H12B 110.3 . . ? C13 C12 H12B 110.3 . . ? H12A C12 H12B 108.6 . . ? C14 C13 N2 121.3(7) . . ? C14 C13 C12 123.4(7) . . ? N2 C13 C12 115.1(6) . . ? C13 C14 C15 119.6(8) . . ? C13 C14 H14A 120.2 . . ? C15 C14 H14A 120.2 . . ? C14 C15 C16 119.5(8) . . ? C14 C15 H15A 120.3 . . ? C16 C15 H15A 120.3 . . ? C17 C16 C15 118.4(8) . . ? C17 C16 H16A 120.8 . . ? C15 C16 H16A 120.8 . . ? N2 C17 C16 123.0(7) . . ? N2 C17 H17A 118.5 . . ? C16 C17 H17A 118.5 . . ? N1 C18 C19 110.3(6) . . ? N1 C18 H18A 109.6 . . ? C19 C18 H18A 109.6 . . ? N1 C18 H18B 109.6 . . ? C19 C18 H18B 109.6 . . ? H18A C18 H18B 108.1 . . ? N3 C19 C20 119.1(7) . . ? N3 C19 C18 115.9(6) . . ? C20 C19 C18 124.9(7) . . ? C19 C20 C21 120.9(7) . . ? C19 C20 H20A 119.5 . . ? C21 C20 H20A 119.5 . . ? C22 C21 C20 117.9(8) . . ? C22 C21 H21A 121.1 . . ? C20 C21 H21A 121.1 . . ? C21 C22 C23 120.1(8) . . ? C21 C22 H22A 120.0 . . ? C23 C22 H22A 120.0 . . ? N3 C23 C22 122.4(7) . . ? N3 C23 H23A 118.8 . . ? C22 C23 H23A 118.8 . . ? N4 C24 C6 108.8(5) . . ? N4 C24 H24A 109.9 . . ? C6 C24 H24A 109.9 . . ? N4 C24 H24B 109.9 . . ? C6 C24 H24B 109.9 . . ? H24A C24 H24B 108.3 . . ? N4 C25 C26 111.5(6) . . ? N4 C25 H25A 109.3 . . ? C26 C25 H25A 109.3 . . ? N4 C25 H25B 109.3 . . ? C26 C25 H25B 109.3 . . ? H25A C25 H25B 108.0 . . ? N5 C26 C27 122.8(7) . . ? N5 C26 C25 115.7(6) . . ? C27 C26 C25 121.3(7) . . ? C26 C27 C28 118.4(8) . . ? C26 C27 H27A 120.8 . . ? C28 C27 H27A 120.8 . . ? C29 C28 C27 119.4(7) . . ? C29 C28 H28A 120.3 . . ? C27 C28 H28A 120.3 . . ? C28 C29 C30 119.1(8) . . ? C28 C29 H29A 120.4 . . ? C30 C29 H29A 120.4 . . ? N5 C30 C29 122.0(8) . . ? N5 C30 H30A 119.0 . . ? C29 C30 H30A 119.0 . . ? N4 C31 C32 107.7(6) . . ? N4 C31 H31A 110.2 . . ? C32 C31 H31A 110.2 . . ? N4 C31 H31B 110.2 . . ? C32 C31 H31B 110.2 . . ? H31A C31 H31B 108.5 . . ? N6 C32 C33 122.5(7) . . ? N6 C32 C31 116.2(6) . . ? C33 C32 C31 121.2(8) . . ? C32 C33 C34 117.3(8) . . ? C32 C33 H33A 121.4 . . ? C34 C33 H33A 121.4 . . ? C35 C34 C33 120.4(8) . . ? C35 C34 H34A 119.8 . . ? C33 C34 H34A 119.8 . . ? C36 C35 C34 118.1(8) . . ? C36 C35 H35A 121.0 . . ? C34 C35 H35A 121.0 . . ? N6 C36 C35 122.9(8) . . ? N6 C36 H36A 118.6 . . ? C35 C36 H36A 118.6 . . ? O2D Cl2 O2A 109.9(4) . . ? O2D Cl2 O2C 110.7(4) . . ? O2A Cl2 O2C 109.6(4) . . ? O2D Cl2 O2B 109.0(5) . . ? O2A Cl2 O2B 110.3(3) . . ? O2C Cl2 O2B 107.3(4) . . ? O1C Cl1 O1A 117.3(6) . . ? O1C Cl1 O1B 109.6(6) . . ? O1A Cl1 O1B 110.4(5) . . ? O1C Cl1 O1D 110.6(7) . . ? O1A Cl1 O1D 104.4(5) . . ? O1B Cl1 O1D 103.7(6) . . ? H1W O1W H2W 108.1 . . ? H3W O2W H4W 103.8 . . ? C1S O1S H1S 109.5 . . ? O1S C1S C2S 99.8(19) . . ? O1S C1S H1S1 111.8 . . ? C2S C1S H1S1 111.8 . . ? O1S C1S H1S2 111.8 . . ? C2S C1S H1S2 111.8 . . ? H1S1 C1S H1S2 109.5 . . ? C1S C2S H2S1 109.5 . . ? C1S C2S H2S2 109.5 . . ? H2S1 C2S H2S2 109.5 . . ? C1S C2S H2S3 109.5 . . ? H2S1 C2S H2S3 109.5 . . ? H2S2 C2S H2S3 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 V2 O1 C1 125.5(4) . . . . ? O5 V2 O1 C1 -129.1(5) . . . . ? N6 V2 O1 C1 -65.9(7) . . . . ? N5 V2 O1 C1 33.1(4) . . . . ? N4 V2 O1 C1 -41.9(4) . . . . ? O4 V2 O1 V1 -52.7(3) . . . . ? O5 V2 O1 V1 52.7(3) . . . . ? N6 V2 O1 V1 116.0(5) . . . . ? N5 V2 O1 V1 -145.0(3) . . . . ? N4 V2 O1 V1 139.9(3) . . . . ? O3 V1 O1 C1 136.9(4) . . . . ? N2 V1 O1 C1 -122.8(4) . . . . ? N3 V1 O1 C1 33.2(4) . . . . ? N1 V1 O1 C1 -45.9(4) . . . . ? O3 V1 O1 V2 -44.9(3) . . . . ? N2 V1 O1 V2 55.3(3) . . . . ? N3 V1 O1 V2 -148.7(3) . . . . ? N1 V1 O1 V2 132.3(3) . . . . ? O2 V1 N1 C18 -61.8(5) . . . . ? O3 V1 N1 C18 122.6(8) . . . . ? N2 V1 N1 C18 -156.9(5) . . . . ? N3 V1 N1 C18 31.5(4) . . . . ? O1 V1 N1 C18 113.0(4) . . . . ? O2 V1 N1 C12 55.9(4) . . . . ? O3 V1 N1 C12 -119.7(8) . . . . ? N2 V1 N1 C12 -39.2(4) . . . . ? N3 V1 N1 C12 149.2(4) . . . . ? O1 V1 N1 C12 -129.3(4) . . . . ? O2 V1 N1 C11 174.2(5) . . . . ? O3 V1 N1 C11 -1.4(11) . . . . ? N2 V1 N1 C11 79.0(5) . . . . ? N3 V1 N1 C11 -92.5(5) . . . . ? O1 V1 N1 C11 -11.0(5) . . . . ? O2 V1 N2 C17 106.8(6) . . . . ? O3 V1 N2 C17 0.7(6) . . . . ? N3 V1 N2 C17 -143.9(6) . . . . ? N1 V1 N2 C17 -162.3(6) . . . . ? O1 V1 N2 C17 -82.6(6) . . . . ? O2 V1 N2 C13 -68.0(5) . . . . ? O3 V1 N2 C13 -174.1(5) . . . . ? N3 V1 N2 C13 41.3(8) . . . . ? N1 V1 N2 C13 22.9(5) . . . . ? O1 V1 N2 C13 102.6(5) . . . . ? O2 V1 N3 C23 -105.1(5) . . . . ? O3 V1 N3 C23 0.9(6) . . . . ? N2 V1 N3 C23 145.2(6) . . . . ? N1 V1 N3 C23 163.5(6) . . . . ? O1 V1 N3 C23 82.1(5) . . . . ? O2 V1 N3 C19 75.6(5) . . . . ? O3 V1 N3 C19 -178.3(5) . . . . ? N2 V1 N3 C19 -34.1(8) . . . . ? N1 V1 N3 C19 -15.7(4) . . . . ? O1 V1 N3 C19 -97.1(5) . . . . ? O4 V2 N4 C31 86.0(8) . . . . ? O5 V2 N4 C31 -49.1(4) . . . . ? O1 V2 N4 C31 -134.4(4) . . . . ? N6 V2 N4 C31 37.0(4) . . . . ? N5 V2 N4 C31 135.5(4) . . . . ? O4 V2 N4 C25 -33.0(9) . . . . ? O5 V2 N4 C25 -168.0(4) . . . . ? O1 V2 N4 C25 106.6(4) . . . . ? N6 V2 N4 C25 -81.9(4) . . . . ? N5 V2 N4 C25 16.5(4) . . . . ? O4 V2 N4 C24 -154.3(6) . . . . ? O5 V2 N4 C24 70.7(4) . . . . ? O1 V2 N4 C24 -14.7(4) . . . . ? N6 V2 N4 C24 156.8(4) . . . . ? N5 V2 N4 C24 -104.8(4) . . . . ? O4 V2 N5 C26 163.7(5) . . . . ? O5 V2 N5 C26 -16.5(10) . . . . ? O1 V2 N5 C26 -90.7(5) . . . . ? N6 V2 N5 C26 69.1(5) . . . . ? N4 V2 N5 C26 -2.1(5) . . . . ? O4 V2 N5 C30 -26.9(6) . . . . ? O5 V2 N5 C30 153.0(7) . . . . ? O1 V2 N5 C30 78.8(5) . . . . ? N6 V2 N5 C30 -121.5(5) . . . . ? N4 V2 N5 C30 167.4(6) . . . . ? O4 V2 N6 C32 169.5(5) . . . . ? O5 V2 N6 C32 63.6(5) . . . . ? O1 V2 N6 C32 0.4(9) . . . . ? N5 V2 N6 C32 -98.0(5) . . . . ? N4 V2 N6 C32 -24.7(5) . . . . ? O4 V2 N6 C36 -4.0(5) . . . . ? O5 V2 N6 C36 -109.9(5) . . . . ? O1 V2 N6 C36 -173.1(5) . . . . ? N5 V2 N6 C36 88.5(5) . . . . ? N4 V2 N6 C36 161.8(5) . . . . ? V2 O1 C1 C2 -120.1(5) . . . . ? V1 O1 C1 C2 58.2(7) . . . . ? V2 O1 C1 C6 59.2(7) . . . . ? V1 O1 C1 C6 -122.5(5) . . . . ? C6 C1 C2 C3 -0.6(10) . . . . ? O1 C1 C2 C3 178.7(6) . . . . ? C6 C1 C2 C11 -179.9(6) . . . . ? O1 C1 C2 C11 -0.6(9) . . . . ? C1 C2 C3 C4 0.1(10) . . . . ? C11 C2 C3 C4 179.5(6) . . . . ? C2 C3 C4 C5 0.8(10) . . . . ? C2 C3 C4 C7 -177.1(6) . . . . ? C3 C4 C5 C6 -1.4(9) . . . . ? C7 C4 C5 C6 176.6(6) . . . . ? C4 C5 C6 C1 1.0(10) . . . . ? C4 C5 C6 C24 -176.0(6) . . . . ? C2 C1 C6 C5 0.0(9) . . . . ? O1 C1 C6 C5 -179.2(5) . . . . ? C2 C1 C6 C24 177.1(6) . . . . ? O1 C1 C6 C24 -2.2(9) . . . . ? C3 C4 C7 C10 -7.3(9) . . . . ? C5 C4 C7 C10 174.8(6) . . . . ? C3 C4 C7 C9 -129.0(7) . . . . ? C5 C4 C7 C9 53.1(8) . . . . ? C3 C4 C7 C8 111.8(7) . . . . ? C5 C4 C7 C8 -66.1(8) . . . . ? C3 C2 C11 N1 114.7(7) . . . . ? C1 C2 C11 N1 -65.9(8) . . . . ? C18 N1 C11 C2 -59.5(7) . . . . ? C12 N1 C11 C2 177.8(5) . . . . ? V1 N1 C11 C2 61.7(7) . . . . ? C18 N1 C12 C13 160.5(5) . . . . ? C11 N1 C12 C13 -78.2(6) . . . . ? V1 N1 C12 C13 48.9(6) . . . . ? C17 N2 C13 C14 0.9(10) . . . . ? V1 N2 C13 C14 176.1(6) . . . . ? C17 N2 C13 C12 -175.9(6) . . . . ? V1 N2 C13 C12 -0.7(7) . . . . ? N1 C12 C13 C14 148.5(7) . . . . ? N1 C12 C13 N2 -34.8(8) . . . . ? N2 C13 C14 C15 -1.5(11) . . . . ? C12 C13 C14 C15 175.1(7) . . . . ? C13 C14 C15 C16 0.0(12) . . . . ? C14 C15 C16 C17 1.9(11) . . . . ? C13 N2 C17 C16 1.2(10) . . . . ? V1 N2 C17 C16 -173.5(5) . . . . ? C15 C16 C17 N2 -2.6(11) . . . . ? C12 N1 C18 C19 -153.5(6) . . . . ? C11 N1 C18 C19 87.2(7) . . . . ? V1 N1 C18 C19 -42.8(6) . . . . ? C23 N3 C19 C20 0.4(9) . . . . ? V1 N3 C19 C20 179.7(5) . . . . ? C23 N3 C19 C18 176.3(6) . . . . ? V1 N3 C19 C18 -4.4(8) . . . . ? N1 C18 C19 N3 33.9(8) . . . . ? N1 C18 C19 C20 -150.5(7) . . . . ? N3 C19 C20 C21 0.4(10) . . . . ? C18 C19 C20 C21 -175.2(7) . . . . ? C19 C20 C21 C22 0.2(11) . . . . ? C20 C21 C22 C23 -1.4(11) . . . . ? C19 N3 C23 C22 -1.7(10) . . . . ? V1 N3 C23 C22 179.1(5) . . . . ? C21 C22 C23 N3 2.3(11) . . . . ? C31 N4 C24 C6 178.7(5) . . . . ? C25 N4 C24 C6 -59.5(7) . . . . ? V2 N4 C24 C6 61.6(6) . . . . ? C5 C6 C24 N4 112.9(7) . . . . ? C1 C6 C24 N4 -64.1(7) . . . . ? C31 N4 C25 C26 -144.4(6) . . . . ? C24 N4 C25 C26 93.5(6) . . . . ? V2 N4 C25 C26 -27.8(6) . . . . ? C30 N5 C26 C27 0.6(10) . . . . ? V2 N5 C26 C27 170.3(5) . . . . ? C30 N5 C26 C25 176.9(6) . . . . ? V2 N5 C26 C25 -13.5(8) . . . . ? N4 C25 C26 N5 28.0(8) . . . . ? N4 C25 C26 C27 -155.7(6) . . . . ? N5 C26 C27 C28 -0.2(10) . . . . ? C25 C26 C27 C28 -176.2(6) . . . . ? C26 C27 C28 C29 -0.4(11) . . . . ? C27 C28 C29 C30 0.6(12) . . . . ? C26 N5 C30 C29 -0.5(11) . . . . ? V2 N5 C30 C29 -170.2(6) . . . . ? C28 C29 C30 N5 -0.1(12) . . . . ? C25 N4 C31 C32 74.9(7) . . . . ? C24 N4 C31 C32 -163.3(6) . . . . ? V2 N4 C31 C32 -43.9(6) . . . . ? C36 N6 C32 C33 2.1(10) . . . . ? V2 N6 C32 C33 -171.6(5) . . . . ? C36 N6 C32 C31 -179.0(6) . . . . ? V2 N6 C32 C31 7.2(8) . . . . ? N4 C31 C32 N6 26.9(8) . . . . ? N4 C31 C32 C33 -154.3(6) . . . . ? N6 C32 C33 C34 -1.4(10) . . . . ? C31 C32 C33 C34 179.8(6) . . . . ? C32 C33 C34 C35 -0.7(11) . . . . ? C33 C34 C35 C36 2.0(12) . . . . ? C32 N6 C36 C35 -0.7(10) . . . . ? V2 N6 C36 C35 172.7(6) . . . . ? C34 C35 C36 N6 -1.4(11) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H1 O3 0.86(5) 1.77(5) 2.628(7) 170(6) . O5 H2 O1W 0.86(5) 1.75(5) 2.582(7) 162(7) . O1W H1W O3 0.84 2.05 2.806(7) 149.4 2_677 O1W H2W O1C 0.84 1.99 2.827(13) 173.8 2_667 O2W H3W O2D 0.84 2.11 2.902(15) 156.8 . O2W H4W O1S 0.84 1.65 2.38(2) 143.8 .