# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Liwei Han' _publ_contact_author_email hanliwei@fjirsm.ac.cn loop_ _publ_author_name 'Li-Wei Han' 'Rong Cao' # Attachment '- complex 1.CIF' data_complex1 _database_code_depnum_ccdc_archive 'CCDC 876879' #TrackingRef '- complex 1.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H144 N44 O46 V4' _chemical_formula_weight 2662.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 37.778(14) _cell_length_b 14.420(5) _cell_length_c 21.471(7) _cell_angle_alpha 90.00 _cell_angle_beta 100.945(19) _cell_angle_gamma 90.00 _cell_volume 11484(7) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.540 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5568 _exptl_absorpt_coefficient_mu 0.424 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9200 _exptl_absorpt_correction_T_max 0.9276 _exptl_absorpt_process_details ? _exptl_special_details ; empirical from equivalent reflections (XEMP in SHELXTL; Siemens,1994) ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Mercury ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 36207 _diffrn_reflns_av_R_equivalents 0.0553 _diffrn_reflns_av_sigmaI/netI 0.0525 _diffrn_reflns_limit_h_min -35 _diffrn_reflns_limit_h_max 44 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.50 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10080 _reflns_number_gt 7945 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1197P)^2^+19.5580P] 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 10080 _refine_ls_number_parameters 887 _refine_ls_number_restraints 54 _refine_ls_R_factor_all 0.0930 _refine_ls_R_factor_gt 0.0742 _refine_ls_wR_factor_ref 0.2270 _refine_ls_wR_factor_gt 0.2118 _refine_ls_goodness_of_fit_ref 1.117 _refine_ls_restrained_S_all 1.120 _refine_ls_shift/su_max 0.086 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.438180(11) 0.10018(3) 0.204963(19) 0.03707(12) Uani 1 1 d . . . V2 V 0.515435(11) 0.09899(3) 0.14872(2) 0.04021(12) Uani 1 1 d . . . O11 O 0.52155(6) 0.0472(2) 0.08463(11) 0.0830(9) Uani 1 1 d . . . O12 O 0.51024(6) 0.21052(17) 0.13490(12) 0.0759(8) Uani 1 1 d . . . O13 O 0.47538(5) 0.05446(15) 0.17282(9) 0.0512(6) Uani 1 1 d . . . O14 O 0.43518(6) 0.21176(16) 0.19019(11) 0.0655(7) Uani 1 1 d . . . O15 O 0.40014(6) 0.05028(19) 0.17247(10) 0.0707(8) Uani 1 1 d . . . O16 O 0.44629(5) 0.08132(16) 0.28918(8) 0.0520(6) Uani 1 1 d . . . C1 C 0.46374(6) 0.70026(15) 0.48219(11) 0.0298(6) Uani 1 1 d . . . H1A H 0.4713 0.7255 0.5245 0.036 Uiso 1 1 calc R . . H1B H 0.4846 0.6997 0.4619 0.036 Uiso 1 1 calc R . . C2 C 0.38574(6) 0.69775(16) 0.54472(10) 0.0290(6) Uani 1 1 d . . . H2A H 0.4037 0.7218 0.5793 0.035 Uiso 1 1 calc R . . H2B H 0.3630 0.6948 0.5593 0.035 Uiso 1 1 calc R . . C3 C 0.45641(6) 0.53984(16) 0.44385(10) 0.0304(6) Uani 1 1 d . . . C4 C 0.43300(6) 0.56926(16) 0.53617(10) 0.0278(5) Uani 1 1 d . . . C5 C 0.42674(6) 0.46287(16) 0.51653(10) 0.0285(6) Uani 1 1 d . . . C6 C 0.45454(7) 0.58684(17) 0.60274(11) 0.0354(6) Uani 1 1 d . . . H6A H 0.4416 0.5623 0.6335 0.053 Uiso 1 1 calc R . . H6B H 0.4579 0.6523 0.6093 0.053 Uiso 1 1 calc R . . H6C H 0.4776 0.5569 0.6073 0.053 Uiso 1 1 calc R . . C7 C 0.44289(7) 0.39218(17) 0.56641(12) 0.0377(7) Uani 1 1 d . . . H7A H 0.4317 0.3981 0.6028 0.057 Uiso 1 1 calc R . . H7B H 0.4683 0.4030 0.5788 0.057 Uiso 1 1 calc R . . H7C H 0.4389 0.3308 0.5492 0.057 Uiso 1 1 calc R . . C8 C 0.37056(6) 0.53860(16) 0.51166(10) 0.0290(6) Uani 1 1 d . . . C9 C 0.44552(6) 0.37516(16) 0.42189(11) 0.0327(6) Uani 1 1 d . . . H9A H 0.4662 0.3822 0.4015 0.039 Uiso 1 1 calc R . . H9B H 0.4500 0.3219 0.4499 0.039 Uiso 1 1 calc R . . C10 C 0.36645(6) 0.37373(16) 0.48410(10) 0.0298(6) Uani 1 1 d . . . H10A H 0.3437 0.3796 0.4984 0.036 Uiso 1 1 calc R . . H10B H 0.3792 0.3215 0.5063 0.036 Uiso 1 1 calc R . . C11 C 0.41347(6) 0.37498(15) 0.31082(10) 0.0290(6) Uani 1 1 d . . . C12 C 0.38284(6) 0.30254(15) 0.38289(10) 0.0278(5) Uani 1 1 d . . . C13 C 0.35959(6) 0.29578(15) 0.31348(10) 0.0281(5) Uani 1 1 d . . . C14 C 0.32605(6) 0.37154(15) 0.37971(10) 0.0286(6) Uani 1 1 d . . . C15 C 0.39417(7) 0.20938(16) 0.41502(12) 0.0391(7) Uani 1 1 d . . . H15A H 0.4097 0.1773 0.3916 0.059 Uiso 1 1 calc R . . H15B H 0.3731 0.1725 0.4159 0.059 Uiso 1 1 calc R . . H15C H 0.4068 0.2201 0.4576 0.059 Uiso 1 1 calc R . . C16 C 0.35201(7) 0.19619(16) 0.28821(12) 0.0405(7) Uani 1 1 d . . . H16A H 0.3377 0.1642 0.3138 0.061 Uiso 1 1 calc R . . H16B H 0.3744 0.1639 0.2900 0.061 Uiso 1 1 calc R . . H16C H 0.3393 0.1985 0.2451 0.061 Uiso 1 1 calc R . . C17 C 0.37273(6) 0.35695(16) 0.20745(10) 0.0302(6) Uani 1 1 d . . . H17A H 0.3605 0.3014 0.1893 0.036 Uiso 1 1 calc R . . H17B H 0.3950 0.3623 0.1914 0.036 Uiso 1 1 calc R . . C18 C 0.29447(6) 0.35261(16) 0.26946(11) 0.0310(6) Uani 1 1 d . . . H18A H 0.2923 0.2976 0.2430 0.037 Uiso 1 1 calc R . . H18B H 0.2733 0.3555 0.2888 0.037 Uiso 1 1 calc R . . C19 C 0.36449(6) 0.51879(16) 0.17155(10) 0.0303(6) Uani 1 1 d . . . C20 C 0.31067(6) 0.43770(15) 0.17232(10) 0.0272(5) Uani 1 1 d . . . C21 C 0.30172(6) 0.54123(16) 0.14826(10) 0.0294(6) Uani 1 1 d . . . C22 C 0.27832(6) 0.51487(16) 0.24175(10) 0.0290(6) Uani 1 1 d . . . C23 C 0.29528(7) 0.36295(17) 0.12528(11) 0.0357(6) Uani 1 1 d . . . H23A H 0.2694 0.3661 0.1174 0.054 Uiso 1 1 calc R . . H23B H 0.3030 0.3032 0.1424 0.054 Uiso 1 1 calc R . . H23C H 0.3037 0.3722 0.0863 0.054 Uiso 1 1 calc R . . C24 C 0.27801(7) 0.55024(18) 0.08291(11) 0.0376(7) Uani 1 1 d . . . H24A H 0.2547 0.5239 0.0836 0.056 Uiso 1 1 calc R . . H24B H 0.2890 0.5179 0.0524 0.056 Uiso 1 1 calc R . . H24C H 0.2753 0.6146 0.0715 0.056 Uiso 1 1 calc R . . C25 C 0.34499(6) 0.67437(16) 0.13207(10) 0.0303(6) Uani 1 1 d . . . H25A H 0.3679 0.6744 0.1179 0.036 Uiso 1 1 calc R . . H25B H 0.3266 0.6928 0.0963 0.036 Uiso 1 1 calc R . . C26 C 0.26725(6) 0.67052(16) 0.19674(11) 0.0301(6) Uani 1 1 d . . . H26A H 0.2580 0.6876 0.1530 0.036 Uiso 1 1 calc R . . H26B H 0.2469 0.6671 0.2183 0.036 Uiso 1 1 calc R . . C27 C 0.37881(6) 0.77138(16) 0.21553(11) 0.0317(6) Uani 1 1 d . . . C28 C 0.33487(6) 0.86498(15) 0.24951(10) 0.0278(5) Uani 1 1 d . . . C29 C 0.31617(6) 0.79724(16) 0.19469(10) 0.0296(6) Uani 1 1 d . . . C30 C 0.29239(6) 0.76910(15) 0.28733(11) 0.0285(6) Uani 1 1 d . . . C31 C 0.29534(7) 0.84467(19) 0.13553(12) 0.0413(7) Uani 1 1 d . . . H31A H 0.2757 0.8794 0.1464 0.062 Uiso 1 1 calc R . . H31B H 0.2861 0.7987 0.1044 0.062 Uiso 1 1 calc R . . H31C H 0.3111 0.8858 0.1186 0.062 Uiso 1 1 calc R . . C32 C 0.32944(7) 0.96797(17) 0.23604(13) 0.0425(7) Uani 1 1 d . . . H32A H 0.3043 0.9827 0.2310 0.064 Uiso 1 1 calc R . . H32B H 0.3378 0.9833 0.1978 0.064 Uiso 1 1 calc R . . H32C H 0.3428 1.0029 0.2708 0.064 Uiso 1 1 calc R . . C33 C 0.40251(6) 0.88210(17) 0.30073(11) 0.0319(6) Uani 1 1 d . . . H33A H 0.4243 0.8753 0.2835 0.038 Uiso 1 1 calc R . . H33B H 0.3976 0.9479 0.3031 0.038 Uiso 1 1 calc R . . C34 C 0.32342(6) 0.88101(16) 0.36521(11) 0.0304(6) Uani 1 1 d . . . H34A H 0.3269 0.9471 0.3602 0.036 Uiso 1 1 calc R . . H34B H 0.3018 0.8728 0.3828 0.036 Uiso 1 1 calc R . . C35 C 0.43070(7) 0.87369(18) 0.53114(12) 0.0412(7) Uani 1 1 d . . . H35A H 0.4133 0.9096 0.5481 0.062 Uiso 1 1 calc R . . H35B H 0.4479 0.9145 0.5177 0.062 Uiso 1 1 calc R . . H35C H 0.4430 0.8325 0.5632 0.062 Uiso 1 1 calc R . . C36 C 0.43663(6) 0.78285(16) 0.38494(11) 0.0297(6) Uani 1 1 d . . . C37 C 0.39120(6) 0.87568(16) 0.41520(11) 0.0298(6) Uani 1 1 d . . . C38 C 0.41142(6) 0.81697(16) 0.47435(10) 0.0286(6) Uani 1 1 d . . . C39 C 0.34924(6) 0.78330(15) 0.45559(11) 0.0283(5) Uani 1 1 d . . . C40 C 0.39433(7) 0.98025(17) 0.42241(13) 0.0404(7) Uani 1 1 d . . . H40A H 0.3827 1.0000 0.4562 0.061 Uiso 1 1 calc R . . H40B H 0.3830 1.0094 0.3836 0.061 Uiso 1 1 calc R . . H40C H 0.4193 0.9975 0.4321 0.061 Uiso 1 1 calc R . . N1 N 0.37269(5) 0.83811(13) 0.25793(9) 0.0305(5) Uani 1 1 d . . . N2 N 0.31792(5) 0.83749(13) 0.30302(9) 0.0301(5) Uani 1 1 d . . . N3 N 0.29157(5) 0.74342(13) 0.22619(9) 0.0291(5) Uani 1 1 d . . . N4 N 0.34648(5) 0.74263(13) 0.18176(9) 0.0299(5) Uani 1 1 d . . . N5 N 0.33732(5) 0.58000(13) 0.15046(9) 0.0301(5) Uani 1 1 d . . . N6 N 0.28366(5) 0.57889(13) 0.19783(9) 0.0317(5) Uani 1 1 d . . . N7 N 0.29489(5) 0.43318(13) 0.22970(9) 0.0298(5) Uani 1 1 d . . . N8 N 0.35008(5) 0.43715(13) 0.18603(9) 0.0304(5) Uani 1 1 d . . . N9 N 0.32629(5) 0.34322(13) 0.31955(9) 0.0298(5) Uani 1 1 d . . . N10 N 0.38150(5) 0.34652(13) 0.27610(9) 0.0292(5) Uani 1 1 d . . . N11 N 0.41407(5) 0.35608(13) 0.37354(9) 0.0298(5) Uani 1 1 d . . . N12 N 0.35898(5) 0.35338(13) 0.41691(9) 0.0291(5) Uani 1 1 d . . . N13 N 0.44276(5) 0.45685(13) 0.45981(9) 0.0318(5) Uani 1 1 d . . . N14 N 0.38727(5) 0.45627(13) 0.50180(9) 0.0299(5) Uani 1 1 d . . . N15 N 0.45171(5) 0.60508(13) 0.48762(9) 0.0301(5) Uani 1 1 d . . . N16 N 0.39603(5) 0.60476(13) 0.52977(9) 0.0303(5) Uani 1 1 d . . . N17 N 0.43662(5) 0.76107(13) 0.44658(9) 0.0293(5) Uani 1 1 d . . . N18 N 0.38202(5) 0.76199(13) 0.49159(9) 0.0303(5) Uani 1 1 d . . . N19 N 0.35403(5) 0.84453(13) 0.40984(9) 0.0309(5) Uani 1 1 d . . . N20 N 0.40862(5) 0.84336(13) 0.36427(9) 0.0312(5) Uani 1 1 d . . . O1 O 0.40843(4) 0.74366(12) 0.20869(9) 0.0418(5) Uani 1 1 d . . . O2 O 0.45784(4) 0.75423(12) 0.35289(8) 0.0405(5) Uani 1 1 d . . . O3 O 0.47152(4) 0.55225(12) 0.39866(8) 0.0381(4) Uani 1 1 d . . . O4 O 0.39684(4) 0.53402(12) 0.17528(8) 0.0401(5) Uani 1 1 d . . . O5 O 0.43828(4) 0.41063(12) 0.28960(8) 0.0381(5) Uani 1 1 d . . . O6 O 0.27266(4) 0.73967(12) 0.32188(7) 0.0341(4) Uani 1 1 d . . . O7 O 0.31995(4) 0.75428(12) 0.46433(8) 0.0369(4) Uani 1 1 d . . . O8 O 0.33785(4) 0.54850(12) 0.50579(8) 0.0368(4) Uani 1 1 d . . . O9 O 0.26128(4) 0.52588(12) 0.28418(8) 0.0397(5) Uani 1 1 d . . . O10 O 0.29988(4) 0.40399(12) 0.39899(8) 0.0387(5) Uani 1 1 d . . . N21 N 0.27519(6) 0.59548(15) 0.41395(10) 0.0392(6) Uani 1 1 d D . . H19 H 0.2585(7) 0.5929(19) 0.4317(13) 0.047 Uiso 1 1 d D . . H36 H 0.3021(7) 0.5906(18) 0.4475(13) 0.047 Uiso 1 1 d D . . H38 H 0.2788(7) 0.645(2) 0.4012(13) 0.047 Uiso 1 1 d D . . H44 H 0.2795(7) 0.538(2) 0.3968(12) 0.047 Uiso 1 1 d D . . N22 N 0.5000 0.3216(2) 0.2500 0.0490(10) Uani 1 2 d SD . . H2 H 0.5210(7) 0.366(2) 0.2436(14) 0.059 Uiso 1 1 d D . . H26 H 0.5089(8) 0.286(2) 0.2753(13) 0.059 Uiso 1 1 d D . . O1W O 0.68284(5) -0.07607(15) 0.53130(12) 0.0683(7) Uani 1 1 d D . . H1WA H 0.6895(9) -0.0955(11) 0.5740(5) 0.082 Uiso 1 1 d D . . H1WB H 0.6903(7) -0.0197(8) 0.5235(9) 0.082 Uiso 1 1 d D . . O2W O 0.28520(6) 0.09703(17) 0.02082(11) 0.0705(7) Uani 1 1 d D . . H2WA H 0.2969(5) 0.1361(8) -0.0065(9) 0.085 Uiso 1 1 d D . . H2WB H 0.2966(6) 0.0377(7) 0.0140(12) 0.085 Uiso 1 1 d D . . O3W O 0.46395(11) 0.6002(2) 0.26352(16) 0.0495(11) Uani 0.50 1 d PD . . H3WA H 0.4763(6) 0.5432(7) 0.260(2) 0.059 Uiso 0.50 1 d PD . . H3WB H 0.4801(5) 0.6454(8) 0.2558(19) 0.059 Uiso 0.50 1 d PD . . O4W O 0.33973(7) 0.15994(18) 0.12967(12) 0.0819(9) Uani 1 1 d D . . H4WA H 0.3232(3) 0.1238(15) 0.1505(10) 0.098 Uiso 1 1 d D . . H4WB H 0.3613(3) 0.1203(14) 0.1409(14) 0.098 Uiso 1 1 d D . . O5W O 0.28247(6) 0.24946(16) 0.47605(11) 0.0761(7) Uani 1 1 d D . . H5WA H 0.2911(6) 0.3068(7) 0.4644(13) 0.091 Uiso 1 1 d D . . H5WB H 0.2934(5) 0.2035(8) 0.4560(11) 0.091 Uiso 1 1 d D . . O6W O 0.51891(10) -0.1187(2) 0.46530(14) 0.0797(11) Uani 0.75 1 d PD . . H6WA H 0.5427(3) -0.1279(15) 0.4624(16) 0.096 Uiso 0.75 1 d PD . . H6WB H 0.5104(5) -0.0658(10) 0.4420(13) 0.096 Uiso 0.75 1 d PD . . O7W O 0.51728(13) -0.1520(4) 0.3098(2) 0.1042(16) Uani 0.50 1 d PD . . H7WA H 0.5170(10) -0.2149(8) 0.2967(11) 0.125 Uiso 0.50 1 d PD . . H7WB H 0.5350(6) -0.1498(19) 0.3476(8) 0.125 Uiso 0.50 1 d PD . . O8W O 0.62765(12) -0.0727(3) 0.4216(2) 0.1154(18) Uani 0.50 1 d PDU . . H8WA H 0.60609(19) -0.1082(6) 0.4199(6) 0.138 Uiso 0.50 1 d PD . . H8WB H 0.6229(4) -0.0369(7) 0.3835(4) 0.138 Uiso 0.50 1 d PD . . O9W O 0.57582(13) -0.1800(3) 0.4185(2) 0.0917(19) Uani 0.50 1 d PDU . . H9WA H 0.59580(16) -0.1366(8) 0.4253(9) 0.110 Uiso 0.50 1 d PD . . H9WB H 0.5584(2) -0.1476(10) 0.3874(6) 0.110 Uiso 0.50 1 d PD . . O10W O 0.3621(3) 0.5977(7) 0.3468(5) 0.105(4) Uani 0.25 1 d PDU . . H10D H 0.3491(4) 0.5419(11) 0.335(2) 0.126 Uiso 0.25 1 d PD . . H10C H 0.3829(3) 0.5938(19) 0.3302(11) 0.126 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 0.0281(2) 0.0508(2) 0.0320(2) 0.00370(19) 0.00500(16) 0.00063(18) V2 0.0305(2) 0.0604(3) 0.0305(2) 0.0022(2) 0.00758(16) 0.00297(19) O11 0.0551(12) 0.141(2) 0.0527(12) -0.0264(14) 0.0111(10) 0.0081(14) O12 0.0637(13) 0.0730(14) 0.0883(16) 0.0303(13) 0.0074(12) -0.0044(12) O13 0.0443(10) 0.0633(12) 0.0482(10) 0.0063(9) 0.0145(8) 0.0053(9) O14 0.0712(13) 0.0596(12) 0.0679(13) 0.0098(11) 0.0187(11) 0.0182(11) O15 0.0445(11) 0.1118(19) 0.0533(12) -0.0027(13) 0.0031(9) -0.0169(12) O16 0.0367(9) 0.0851(14) 0.0331(9) 0.0043(10) 0.0039(7) -0.0038(10) C1 0.0258(10) 0.0292(11) 0.0343(11) -0.0036(10) 0.0055(9) -0.0007(9) C2 0.0308(10) 0.0312(11) 0.0271(10) 0.0005(9) 0.0109(8) 0.0044(9) C3 0.0254(10) 0.0353(12) 0.0309(11) -0.0030(10) 0.0061(9) 0.0010(9) C4 0.0249(10) 0.0295(11) 0.0288(11) -0.0014(9) 0.0049(8) 0.0018(9) C5 0.0292(10) 0.0312(11) 0.0263(10) -0.0017(9) 0.0078(8) 0.0002(9) C6 0.0348(12) 0.0403(13) 0.0291(11) -0.0069(10) 0.0008(10) 0.0007(10) C7 0.0379(13) 0.0395(13) 0.0342(12) 0.0016(11) 0.0032(10) 0.0038(11) C8 0.0294(11) 0.0339(11) 0.0242(10) -0.0036(9) 0.0060(8) 0.0004(9) C9 0.0284(11) 0.0349(12) 0.0350(12) -0.0064(10) 0.0063(9) 0.0059(10) C10 0.0320(11) 0.0314(11) 0.0271(10) -0.0012(10) 0.0087(9) -0.0056(9) C11 0.0347(11) 0.0241(10) 0.0298(10) -0.0053(9) 0.0106(9) 0.0032(9) C12 0.0302(10) 0.0242(10) 0.0301(10) -0.0017(9) 0.0081(9) 0.0000(9) C13 0.0314(10) 0.0250(10) 0.0300(10) -0.0005(9) 0.0111(9) -0.0022(9) C14 0.0307(11) 0.0268(10) 0.0300(11) -0.0002(9) 0.0099(9) -0.0043(9) C15 0.0476(14) 0.0264(11) 0.0416(13) 0.0060(11) 0.0046(11) 0.0047(11) C16 0.0544(15) 0.0252(11) 0.0412(13) -0.0072(11) 0.0069(11) -0.0065(11) C17 0.0362(11) 0.0287(11) 0.0284(10) -0.0020(9) 0.0127(9) 0.0038(9) C18 0.0296(11) 0.0322(11) 0.0314(11) 0.0015(10) 0.0065(9) -0.0066(9) C19 0.0340(11) 0.0334(11) 0.0254(10) -0.0017(9) 0.0108(8) 0.0014(10) C20 0.0266(10) 0.0295(11) 0.0268(10) -0.0026(9) 0.0086(8) -0.0006(9) C21 0.0309(11) 0.0296(11) 0.0292(11) -0.0058(9) 0.0095(9) 0.0000(9) C22 0.0256(10) 0.0341(11) 0.0279(10) -0.0039(10) 0.0064(8) -0.0043(9) C23 0.0402(12) 0.0352(12) 0.0317(12) -0.0033(10) 0.0065(10) -0.0044(11) C24 0.0402(13) 0.0397(13) 0.0313(12) -0.0017(11) 0.0033(10) 0.0039(11) C25 0.0368(11) 0.0290(11) 0.0275(10) 0.0034(9) 0.0126(9) 0.0014(10) C26 0.0250(10) 0.0315(11) 0.0348(11) -0.0058(10) 0.0079(9) 0.0010(9) C27 0.0365(11) 0.0270(11) 0.0334(11) 0.0050(10) 0.0111(9) 0.0005(10) C28 0.0254(10) 0.0282(11) 0.0307(11) 0.0027(9) 0.0076(8) 0.0007(9) C29 0.0303(11) 0.0305(11) 0.0288(10) 0.0040(10) 0.0080(9) 0.0020(9) C30 0.0258(10) 0.0289(11) 0.0311(11) 0.0035(9) 0.0060(9) 0.0088(9) C31 0.0442(14) 0.0430(14) 0.0357(12) 0.0077(11) 0.0049(11) 0.0048(12) C32 0.0441(14) 0.0299(12) 0.0531(15) 0.0069(12) 0.0080(12) 0.0015(11) C33 0.0296(11) 0.0352(12) 0.0322(11) 0.0027(10) 0.0093(9) -0.0056(10) C34 0.0276(11) 0.0331(11) 0.0313(11) -0.0052(10) 0.0076(9) 0.0069(9) C35 0.0393(13) 0.0411(13) 0.0409(13) -0.0120(12) 0.0016(11) -0.0022(11) C36 0.0269(10) 0.0285(11) 0.0344(11) -0.0045(10) 0.0072(9) -0.0026(9) C37 0.0262(10) 0.0290(11) 0.0355(11) -0.0062(10) 0.0092(9) -0.0039(9) C38 0.0259(10) 0.0289(11) 0.0320(11) -0.0073(9) 0.0080(9) -0.0022(9) C39 0.0276(10) 0.0259(10) 0.0329(11) -0.0067(9) 0.0092(9) 0.0002(9) C40 0.0449(13) 0.0286(11) 0.0473(14) -0.0052(11) 0.0077(11) -0.0024(11) N1 0.0279(9) 0.0318(9) 0.0336(9) -0.0047(8) 0.0099(7) -0.0002(8) N2 0.0297(9) 0.0336(10) 0.0288(9) -0.0043(8) 0.0105(7) -0.0048(8) N3 0.0275(9) 0.0315(9) 0.0294(9) -0.0020(8) 0.0084(7) -0.0042(8) N4 0.0258(9) 0.0331(10) 0.0317(9) -0.0039(8) 0.0076(7) 0.0014(8) N5 0.0278(9) 0.0295(9) 0.0341(10) 0.0015(8) 0.0087(8) -0.0008(8) N6 0.0342(9) 0.0314(10) 0.0316(9) -0.0012(8) 0.0116(8) 0.0022(8) N7 0.0357(9) 0.0298(9) 0.0262(9) 0.0010(8) 0.0123(7) 0.0011(8) N8 0.0253(9) 0.0302(9) 0.0362(10) 0.0016(8) 0.0070(8) -0.0017(8) N9 0.0249(9) 0.0362(10) 0.0285(9) -0.0032(8) 0.0049(7) 0.0014(8) N10 0.0285(9) 0.0318(9) 0.0281(9) -0.0003(8) 0.0077(7) -0.0025(8) N11 0.0302(9) 0.0306(9) 0.0302(9) -0.0025(8) 0.0098(7) -0.0025(8) N12 0.0274(9) 0.0331(10) 0.0273(9) -0.0019(8) 0.0065(7) 0.0011(8) N13 0.0357(10) 0.0315(10) 0.0304(9) -0.0060(8) 0.0117(8) -0.0019(8) N14 0.0282(9) 0.0270(9) 0.0336(9) -0.0032(8) 0.0037(8) 0.0015(8) N15 0.0291(9) 0.0310(9) 0.0322(9) -0.0057(8) 0.0110(7) -0.0016(8) N16 0.0255(9) 0.0294(9) 0.0364(10) -0.0081(8) 0.0073(8) 0.0000(8) N17 0.0269(9) 0.0327(10) 0.0296(9) -0.0027(8) 0.0088(7) 0.0034(8) N18 0.0281(9) 0.0326(10) 0.0314(9) -0.0007(8) 0.0086(7) 0.0011(8) N19 0.0255(9) 0.0323(10) 0.0349(10) 0.0002(8) 0.0056(8) 0.0002(8) N20 0.0289(9) 0.0326(10) 0.0344(9) -0.0016(8) 0.0114(7) 0.0033(8) O1 0.0296(8) 0.0482(10) 0.0502(10) -0.0065(8) 0.0143(7) 0.0062(7) O2 0.0379(8) 0.0457(10) 0.0425(9) -0.0030(8) 0.0192(7) 0.0067(8) O3 0.0400(8) 0.0399(9) 0.0381(8) -0.0054(8) 0.0165(7) -0.0024(7) O4 0.0294(8) 0.0388(9) 0.0546(10) 0.0047(8) 0.0142(7) -0.0015(7) O5 0.0332(8) 0.0441(9) 0.0401(9) -0.0013(8) 0.0148(7) -0.0074(7) O6 0.0327(8) 0.0399(9) 0.0317(8) 0.0009(7) 0.0112(6) -0.0048(7) O7 0.0286(8) 0.0427(9) 0.0410(9) 0.0024(8) 0.0104(7) -0.0020(7) O8 0.0256(8) 0.0389(9) 0.0476(9) -0.0011(8) 0.0109(7) 0.0007(7) O9 0.0439(9) 0.0419(9) 0.0377(8) -0.0037(8) 0.0188(7) -0.0002(8) O10 0.0322(8) 0.0493(10) 0.0365(8) -0.0066(8) 0.0111(7) 0.0036(7) N21 0.0378(10) 0.0408(11) 0.0420(11) 0.0029(9) 0.0155(9) 0.0000(9) N22 0.0452(18) 0.0487(18) 0.0500(18) 0.000 0.0011(15) 0.000 O1W 0.0348(9) 0.0655(12) 0.1121(16) -0.0358(12) 0.0330(10) -0.0015(9) O2W 0.0647(12) 0.0825(16) 0.0718(13) 0.0000(12) 0.0325(10) -0.0211(11) O3W 0.086(3) 0.0334(17) 0.0245(16) -0.0041(14) -0.0004(17) -0.0195(18) O4W 0.0938(18) 0.0688(15) 0.0724(16) -0.0070(13) -0.0117(14) 0.0148(14) O5W 0.0752(14) 0.0750(14) 0.0752(14) 0.0324(12) 0.0072(12) -0.0262(12) O6W 0.114(3) 0.079(2) 0.0471(16) -0.0115(16) 0.0190(17) -0.0154(19) O7W 0.130(3) 0.087(4) 0.127(3) -0.009(3) 0.105(2) -0.038(3) O8W 0.140(3) 0.154(4) 0.049(3) 0.020(3) 0.009(3) 0.112(3) O9W 0.120(4) 0.073(3) 0.079(3) 0.006(3) 0.011(3) 0.002(3) O10W 0.135(9) 0.085(7) 0.081(7) -0.005(6) -0.016(6) 0.000(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O15 1.640(2) . ? V1 O14 1.640(2) . ? V1 O16 1.7964(19) . ? V1 O13 1.804(2) . ? V2 O11 1.621(3) . ? V2 O12 1.640(3) . ? V2 O16 1.7892(18) 2_655 ? V2 O13 1.808(2) . ? O16 V2 1.7892(18) 2_655 ? C1 N17 1.451(3) . ? C1 N15 1.457(3) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C2 N16 1.449(3) . ? C2 N18 1.456(3) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C3 O3 1.229(3) . ? C3 N15 1.365(3) . ? C3 N13 1.372(3) . ? C4 N15 1.460(3) . ? C4 N16 1.469(3) . ? C4 C6 1.526(3) . ? C4 C5 1.597(3) . ? C5 N13 1.462(3) . ? C5 N14 1.467(3) . ? C5 C7 1.520(3) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 O8 1.227(3) . ? C8 N16 1.358(3) . ? C8 N14 1.380(3) . ? C9 N11 1.448(3) . ? C9 N13 1.447(3) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C10 N14 1.438(3) . ? C10 N12 1.446(3) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C11 O5 1.230(3) . ? C11 N10 1.357(3) . ? C11 N11 1.370(3) . ? C12 N11 1.455(3) . ? C12 N12 1.461(3) . ? C12 C15 1.533(3) . ? C12 C13 1.583(3) . ? C13 N10 1.455(3) . ? C13 N9 1.459(3) . ? C13 C16 1.543(3) . ? C14 O10 1.234(3) . ? C14 N9 1.356(3) . ? C14 N12 1.370(3) . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C17 N10 1.456(3) . ? C17 N8 1.460(3) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 N7 1.444(3) . ? C18 N9 1.459(3) . ? C18 H18A 0.9700 . ? C18 H18B 0.9700 . ? C19 O4 1.229(3) . ? C19 N8 1.358(3) . ? C19 N5 1.364(3) . ? C20 N8 1.462(3) . ? C20 N7 1.469(3) . ? C20 C23 1.516(3) . ? C20 C21 1.595(3) . ? C21 N5 1.449(3) . ? C21 N6 1.473(3) . ? C21 C24 1.520(3) . ? C22 O9 1.222(3) . ? C22 N6 1.362(3) . ? C22 N7 1.381(3) . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 N4 1.445(3) . ? C25 N5 1.461(3) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C26 N3 1.459(3) . ? C26 N6 1.458(3) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C27 O1 1.223(3) . ? C27 N4 1.361(3) . ? C27 N1 1.374(3) . ? C28 N1 1.458(3) . ? C28 N2 1.472(3) . ? C28 C32 1.519(3) . ? C28 C29 1.589(3) . ? C29 N4 1.459(3) . ? C29 N3 1.470(3) . ? C29 C31 1.523(3) . ? C30 O6 1.223(3) . ? C30 N3 1.358(3) . ? C30 N2 1.376(3) . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 N20 1.451(3) . ? C33 N1 1.457(3) . ? C33 H33A 0.9700 . ? C33 H33B 0.9700 . ? C34 N19 1.453(3) . ? C34 N2 1.454(3) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C35 C38 1.533(3) . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 O2 1.223(3) . ? C36 N17 1.360(3) . ? C36 N20 1.378(3) . ? C37 N20 1.456(3) . ? C37 N19 1.458(3) . ? C37 C40 1.518(3) . ? C37 C38 1.595(3) . ? C38 N17 1.458(3) . ? C38 N18 1.468(3) . ? C39 O7 1.230(3) . ? C39 N19 1.358(3) . ? C39 N18 1.364(3) . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? N21 H19 0.80(3) . ? N21 H36 1.13(3) . ? N21 H38 0.79(3) . ? N21 H44 0.93(3) . ? N22 H2 1.04(3) . ? N22 H26 0.78(3) . ? O1W H1WA 0.946(11) . ? O1W H1WB 0.887(12) . ? O2W H2WA 0.978(14) . ? O2W H2WB 0.982(13) . ? O3W H3WA 0.955(14) . ? O3W H3WB 0.929(15) . ? O4W H4WA 0.983(14) . ? O4W H4WB 0.987(13) . ? O5W H5WA 0.940(13) . ? O5W H5WB 0.929(14) . ? O6W H6WA 0.923(13) . ? O6W H6WB 0.935(14) . ? O7W H7WA 0.949(12) . ? O7W H7WB 0.950(14) . ? O8W H8WA 0.957(7) . ? O8W H8WB 0.954(7) . ? O9W H9WA 0.970(8) . ? O9W H9WB 0.965(8) . ? O10W H10D 0.950(15) . ? O10W H10C 0.926(15) . ? 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 O15 V1 O14 108.99(12) . . ? O15 V1 O16 109.27(11) . . ? O14 V1 O16 109.61(11) . . ? O15 V1 O13 111.13(11) . . ? O14 V1 O13 108.35(11) . . ? O16 V1 O13 109.47(9) . . ? O11 V2 O12 109.27(15) . . ? O11 V2 O16 109.99(11) . 2_655 ? O12 V2 O16 109.05(11) . 2_655 ? O11 V2 O13 109.95(12) . . ? O12 V2 O13 108.80(11) . . ? O16 V2 O13 109.75(9) 2_655 . ? V1 O13 V2 137.31(13) . . ? V2 O16 V1 133.47(12) 2_655 . ? N17 C1 N15 114.31(18) . . ? N17 C1 H1A 108.7 . . ? N15 C1 H1A 108.7 . . ? N17 C1 H1B 108.7 . . ? N15 C1 H1B 108.7 . . ? H1A C1 H1B 107.6 . . ? N16 C2 N18 113.91(18) . . ? N16 C2 H2A 108.8 . . ? N18 C2 H2A 108.8 . . ? N16 C2 H2B 108.8 . . ? N18 C2 H2B 108.8 . . ? H2A C2 H2B 107.7 . . ? O3 C3 N15 125.7(2) . . ? O3 C3 N13 125.3(2) . . ? N15 C3 N13 109.0(2) . . ? N15 C4 N16 112.97(18) . . ? N15 C4 C6 111.46(18) . . ? N16 C4 C6 110.98(19) . . ? N15 C4 C5 102.64(17) . . ? N16 C4 C5 102.67(16) . . ? C6 C4 C5 115.66(18) . . ? N13 C5 N14 112.40(17) . . ? N13 C5 C7 111.88(19) . . ? N14 C5 C7 111.36(19) . . ? N13 C5 C4 102.29(17) . . ? N14 C5 C4 102.29(17) . . ? C7 C5 C4 116.02(18) . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C5 C7 H7A 109.5 . . ? C5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O8 C8 N16 126.4(2) . . ? O8 C8 N14 124.5(2) . . ? N16 C8 N14 109.16(19) . . ? N11 C9 N13 114.91(18) . . ? N11 C9 H9A 108.5 . . ? N13 C9 H9A 108.5 . . ? N11 C9 H9B 108.5 . . ? N13 C9 H9B 108.5 . . ? H9A C9 H9B 107.5 . . ? N14 C10 N12 115.15(19) . . ? N14 C10 H10A 108.5 . . ? N12 C10 H10A 108.5 . . ? N14 C10 H10B 108.5 . . ? N12 C10 H10B 108.5 . . ? H10A C10 H10B 107.5 . . ? O5 C11 N10 125.8(2) . . ? O5 C11 N11 125.1(2) . . ? N10 C11 N11 109.1(2) . . ? N11 C12 N12 113.34(18) . . ? N11 C12 C15 111.25(18) . . ? N12 C12 C15 111.14(19) . . ? N11 C12 C13 102.85(17) . . ? N12 C12 C13 102.53(17) . . ? C15 C12 C13 115.29(18) . . ? N10 C13 N9 113.82(18) . . ? N10 C13 C16 111.17(19) . . ? N9 C13 C16 111.24(19) . . ? N10 C13 C12 102.49(17) . . ? N9 C13 C12 102.75(17) . . ? C16 C13 C12 114.92(18) . . ? O10 C14 N9 125.8(2) . . ? O10 C14 N12 125.0(2) . . ? N9 C14 N12 109.15(19) . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N10 C17 N8 114.08(18) . . ? N10 C17 H17A 108.7 . . ? N8 C17 H17A 108.7 . . ? N10 C17 H17B 108.7 . . ? N8 C17 H17B 108.7 . . ? H17A C17 H17B 107.6 . . ? N7 C18 N9 114.23(18) . . ? N7 C18 H18A 108.7 . . ? N9 C18 H18A 108.7 . . ? N7 C18 H18B 108.7 . . ? N9 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? O4 C19 N8 125.2(2) . . ? O4 C19 N5 125.6(2) . . ? N8 C19 N5 109.14(19) . . ? N8 C20 N7 113.02(17) . . ? N8 C20 C23 112.17(19) . . ? N7 C20 C23 111.22(19) . . ? N8 C20 C21 102.45(17) . . ? N7 C20 C21 102.61(17) . . ? C23 C20 C21 114.77(18) . . ? N5 C21 N6 112.87(18) . . ? N5 C21 C24 112.19(19) . . ? N6 C21 C24 111.28(19) . . ? N5 C21 C20 102.25(17) . . ? N6 C21 C20 102.12(17) . . ? C24 C21 C20 115.51(18) . . ? O9 C22 N6 126.6(2) . . ? O9 C22 N7 124.9(2) . . ? N6 C22 N7 108.44(19) . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N4 C25 N5 114.63(19) . . ? N4 C25 H25A 108.6 . . ? N5 C25 H25A 108.6 . . ? N4 C25 H25B 108.6 . . ? N5 C25 H25B 108.6 . . ? H25A C25 H25B 107.6 . . ? N3 C26 N6 114.54(18) . . ? N3 C26 H26A 108.6 . . ? N6 C26 H26A 108.6 . . ? N3 C26 H26B 108.6 . . ? N6 C26 H26B 108.6 . . ? H26A C26 H26B 107.6 . . ? O1 C27 N4 125.8(2) . . ? O1 C27 N1 125.5(2) . . ? N4 C27 N1 108.6(2) . . ? N1 C28 N2 113.14(17) . . ? N1 C28 C32 112.16(19) . . ? N2 C28 C32 110.4(2) . . ? N1 C28 C29 102.48(17) . . ? N2 C28 C29 102.38(17) . . ? C32 C28 C29 115.79(18) . . ? N4 C29 N3 112.96(18) . . ? N4 C29 C31 112.6(2) . . ? N3 C29 C31 110.42(18) . . ? N4 C29 C28 102.59(17) . . ? N3 C29 C28 102.40(17) . . ? C31 C29 C28 115.37(19) . . ? O6 C30 N3 125.9(2) . . ? O6 C30 N2 125.4(2) . . ? N3 C30 N2 108.6(2) . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C28 C32 H32A 109.5 . . ? C28 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C28 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N20 C33 N1 113.04(19) . . ? N20 C33 H33A 109.0 . . ? N1 C33 H33A 109.0 . . ? N20 C33 H33B 109.0 . . ? N1 C33 H33B 109.0 . . ? H33A C33 H33B 107.8 . . ? N19 C34 N2 113.98(19) . . ? N19 C34 H34A 108.8 . . ? N2 C34 H34A 108.8 . . ? N19 C34 H34B 108.8 . . ? N2 C34 H34B 108.8 . . ? H34A C34 H34B 107.7 . . ? C38 C35 H35A 109.5 . . ? C38 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C38 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? O2 C36 N17 126.2(2) . . ? O2 C36 N20 125.3(2) . . ? N17 C36 N20 108.5(2) . . ? N20 C37 N19 114.09(18) . . ? N20 C37 C40 110.9(2) . . ? N19 C37 C40 111.67(19) . . ? N20 C37 C38 102.22(17) . . ? N19 C37 C38 101.99(18) . . ? C40 C37 C38 115.44(19) . . ? N17 C38 N18 112.87(18) . . ? N17 C38 C35 111.83(18) . . ? N18 C38 C35 110.8(2) . . ? N17 C38 C37 102.64(18) . . ? N18 C38 C37 102.49(16) . . ? C35 C38 C37 115.69(19) . . ? O7 C39 N19 125.3(2) . . ? O7 C39 N18 125.6(2) . . ? N19 C39 N18 108.96(19) . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C27 N1 C33 121.04(19) . . ? C27 N1 C28 112.83(18) . . ? C33 N1 C28 125.77(19) . . ? C30 N2 C34 120.38(19) . . ? C30 N2 C28 112.98(18) . . ? C34 N2 C28 126.37(18) . . ? C30 N3 C26 120.82(19) . . ? C30 N3 C29 113.58(18) . . ? C26 N3 C29 125.58(18) . . ? C27 N4 C25 120.39(19) . . ? C27 N4 C29 113.05(18) . . ? C25 N4 C29 125.89(17) . . ? C19 N5 C21 113.35(19) . . ? C19 N5 C25 121.12(19) . . ? C21 N5 C25 125.53(18) . . ? C22 N6 C26 120.5(2) . . ? C22 N6 C21 113.60(19) . . ? C26 N6 C21 125.21(19) . . ? C22 N7 C18 121.28(19) . . ? C22 N7 C20 112.95(18) . . ? C18 N7 C20 125.71(19) . . ? C19 N8 C17 121.49(19) . . ? C19 N8 C20 112.74(18) . . ? C17 N8 C20 125.55(19) . . ? C14 N9 C13 112.83(17) . . ? C14 N9 C18 121.35(19) . . ? C13 N9 C18 125.53(18) . . ? C11 N10 C13 112.91(18) . . ? C11 N10 C17 122.19(19) . . ? C13 N10 C17 124.51(17) . . ? C11 N11 C9 121.69(19) . . ? C11 N11 C12 112.24(17) . . ? C9 N11 C12 125.32(19) . . ? C14 N12 C10 121.76(19) . . ? C14 N12 C12 112.49(18) . . ? C10 N12 C12 125.35(17) . . ? C3 N13 C9 119.9(2) . . ? C3 N13 C5 113.01(18) . . ? C9 N13 C5 127.05(19) . . ? C8 N14 C10 120.63(19) . . ? C8 N14 C5 112.77(18) . . ? C10 N14 C5 126.40(18) . . ? C3 N15 C1 120.7(2) . . ? C3 N15 C4 113.06(18) . . ? C1 N15 C4 126.20(19) . . ? C8 N16 C2 120.53(19) . . ? C8 N16 C4 113.04(18) . . ? C2 N16 C4 126.30(18) . . ? C36 N17 C1 121.44(19) . . ? C36 N17 C38 113.02(18) . . ? C1 N17 C38 124.67(18) . . ? C39 N18 C2 121.98(19) . . ? C39 N18 C38 112.60(18) . . ? C2 N18 C38 125.17(17) . . ? C39 N19 C34 120.91(19) . . ? C39 N19 C37 113.69(18) . . ? C34 N19 C37 125.06(19) . . ? C36 N20 C33 121.4(2) . . ? C36 N20 C37 112.94(18) . . ? C33 N20 C37 124.67(19) . . ? H19 N21 H36 113(2) . . ? H19 N21 H38 114(3) . . ? H36 N21 H38 95(2) . . ? H19 N21 H44 111(3) . . ? H36 N21 H44 90(2) . . ? H38 N21 H44 128(3) . . ? H2 N22 H26 105(3) . . ? H1WA O1W H1WB 114.8(16) . . ? H2WA O2W H2WB 98.6(15) . . ? H3WA O3W H3WB 103.9(18) . . ? H4WA O4W H4WB 98.5(15) . . ? H5WA O5W H5WB 107.4(17) . . ? H6WA O6W H6WB 108.9(19) . . ? H7WA O7W H7WB 104.5(19) . . ? H8WA O8W H8WB 103.8(9) . . ? H9WA O9W H9WB 101.6(10) . . ? H10D O10W H10C 106(2) . . ? 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 O15 V1 O13 V2 139.77(16) . . . . ? O14 V1 O13 V2 20.05(19) . . . . ? O16 V1 O13 V2 -99.44(17) . . . . ? O11 V2 O13 V1 -140.18(17) . . . . ? O12 V2 O13 V1 -20.55(19) . . . . ? O16 V2 O13 V1 98.70(17) 2_655 . . . ? O15 V1 O16 V2 168.52(17) . . . 2_655 ? O14 V1 O16 V2 -72.1(2) . . . 2_655 ? O13 V1 O16 V2 46.6(2) . . . 2_655 ? N15 C4 C5 N13 -0.41(19) . . . . ? N16 C4 C5 N13 117.00(18) . . . . ? C6 C4 C5 N13 -122.0(2) . . . . ? N15 C4 C5 N14 -116.94(17) . . . . ? N16 C4 C5 N14 0.5(2) . . . . ? C6 C4 C5 N14 121.5(2) . . . . ? N15 C4 C5 C7 121.6(2) . . . . ? N16 C4 C5 C7 -120.9(2) . . . . ? C6 C4 C5 C7 0.1(3) . . . . ? N11 C12 C13 N10 0.1(2) . . . . ? N12 C12 C13 N10 117.92(18) . . . . ? C15 C12 C13 N10 -121.2(2) . . . . ? N11 C12 C13 N9 -118.21(18) . . . . ? N12 C12 C13 N9 -0.4(2) . . . . ? C15 C12 C13 N9 120.5(2) . . . . ? N11 C12 C13 C16 120.8(2) . . . . ? N12 C12 C13 C16 -121.4(2) . . . . ? C15 C12 C13 C16 -0.5(3) . . . . ? N8 C20 C21 N5 1.9(2) . . . . ? N7 C20 C21 N5 119.23(17) . . . . ? C23 C20 C21 N5 -120.0(2) . . . . ? N8 C20 C21 N6 -115.11(18) . . . . ? N7 C20 C21 N6 2.27(19) . . . . ? C23 C20 C21 N6 123.1(2) . . . . ? N8 C20 C21 C24 124.0(2) . . . . ? N7 C20 C21 C24 -118.6(2) . . . . ? C23 C20 C21 C24 2.1(3) . . . . ? N1 C28 C29 N4 0.6(2) . . . . ? N2 C28 C29 N4 -116.81(18) . . . . ? C32 C28 C29 N4 123.0(2) . . . . ? N1 C28 C29 N3 117.91(18) . . . . ? N2 C28 C29 N3 0.5(2) . . . . ? C32 C28 C29 N3 -119.7(2) . . . . ? N1 C28 C29 C31 -122.1(2) . . . . ? N2 C28 C29 C31 120.5(2) . . . . ? C32 C28 C29 C31 0.3(3) . . . . ? N20 C37 C38 N17 -0.4(2) . . . . ? N19 C37 C38 N17 117.83(18) . . . . ? C40 C37 C38 N17 -120.9(2) . . . . ? N20 C37 C38 N18 -117.62(18) . . . . ? N19 C37 C38 N18 0.6(2) . . . . ? C40 C37 C38 N18 121.9(2) . . . . ? N20 C37 C38 C35 121.7(2) . . . . ? N19 C37 C38 C35 -120.1(2) . . . . ? C40 C37 C38 C35 1.2(3) . . . . ? O1 C27 N1 C33 -1.0(4) . . . . ? N4 C27 N1 C33 -179.90(19) . . . . ? O1 C27 N1 C28 172.6(2) . . . . ? N4 C27 N1 C28 -6.3(3) . . . . ? N20 C33 N1 C27 -99.8(2) . . . . ? N20 C33 N1 C28 87.5(3) . . . . ? N2 C28 N1 C27 112.8(2) . . . . ? C32 C28 N1 C27 -121.5(2) . . . . ? C29 C28 N1 C27 3.4(2) . . . . ? N2 C28 N1 C33 -74.0(3) . . . . ? C32 C28 N1 C33 51.7(3) . . . . ? C29 C28 N1 C33 176.5(2) . . . . ? O6 C30 N2 C34 0.3(3) . . . . ? N3 C30 N2 C34 177.24(18) . . . . ? O6 C30 N2 C28 -174.0(2) . . . . ? N3 C30 N2 C28 2.9(2) . . . . ? N19 C34 N2 C30 99.5(2) . . . . ? N19 C34 N2 C28 -87.0(3) . . . . ? N1 C28 N2 C30 -111.6(2) . . . . ? C32 C28 N2 C30 121.8(2) . . . . ? C29 C28 N2 C30 -2.0(2) . . . . ? N1 C28 N2 C34 74.5(3) . . . . ? C32 C28 N2 C34 -52.1(3) . . . . ? C29 C28 N2 C34 -175.98(19) . . . . ? O6 C30 N3 C26 -4.1(3) . . . . ? N2 C30 N3 C26 179.02(18) . . . . ? O6 C30 N3 C29 174.3(2) . . . . ? N2 C30 N3 C29 -2.5(2) . . . . ? N6 C26 N3 C30 -96.4(2) . . . . ? N6 C26 N3 C29 85.4(3) . . . . ? N4 C29 N3 C30 110.8(2) . . . . ? C31 C29 N3 C30 -122.2(2) . . . . ? C28 C29 N3 C30 1.2(2) . . . . ? N4 C29 N3 C26 -70.8(3) . . . . ? C31 C29 N3 C26 56.2(3) . . . . ? C28 C29 N3 C26 179.57(19) . . . . ? O1 C27 N4 C25 -0.9(4) . . . . ? N1 C27 N4 C25 177.99(19) . . . . ? O1 C27 N4 C29 -172.1(2) . . . . ? N1 C27 N4 C29 6.8(3) . . . . ? N5 C25 N4 C27 99.8(2) . . . . ? N5 C25 N4 C29 -90.3(3) . . . . ? N3 C29 N4 C27 -114.0(2) . . . . ? C31 C29 N4 C27 120.1(2) . . . . ? C28 C29 N4 C27 -4.5(2) . . . . ? N3 C29 N4 C25 75.4(3) . . . . ? C31 C29 N4 C25 -50.5(3) . . . . ? C28 C29 N4 C25 -175.1(2) . . . . ? O4 C19 N5 C21 177.0(2) . . . . ? N8 C19 N5 C21 -1.2(3) . . . . ? O4 C19 N5 C25 -2.5(3) . . . . ? N8 C19 N5 C25 179.29(19) . . . . ? N6 C21 N5 C19 108.4(2) . . . . ? C24 C21 N5 C19 -124.9(2) . . . . ? C20 C21 N5 C19 -0.5(2) . . . . ? N6 C21 N5 C25 -72.1(3) . . . . ? C24 C21 N5 C25 54.6(3) . . . . ? C20 C21 N5 C25 179.00(19) . . . . ? N4 C25 N5 C19 -94.3(2) . . . . ? N4 C25 N5 C21 86.2(3) . . . . ? O9 C22 N6 C26 -2.3(3) . . . . ? N7 C22 N6 C26 176.36(18) . . . . ? O9 C22 N6 C21 -173.1(2) . . . . ? N7 C22 N6 C21 5.6(2) . . . . ? N3 C26 N6 C22 100.4(2) . . . . ? N3 C26 N6 C21 -90.0(3) . . . . ? N5 C21 N6 C22 -113.9(2) . . . . ? C24 C21 N6 C22 118.9(2) . . . . ? C20 C21 N6 C22 -4.9(2) . . . . ? N5 C21 N6 C26 75.8(3) . . . . ? C24 C21 N6 C26 -51.3(3) . . . . ? C20 C21 N6 C26 -175.12(18) . . . . ? O9 C22 N7 C18 -2.5(3) . . . . ? N6 C22 N7 C18 178.74(18) . . . . ? O9 C22 N7 C20 174.9(2) . . . . ? N6 C22 N7 C20 -3.8(2) . . . . ? N9 C18 N7 C22 -94.9(2) . . . . ? N9 C18 N7 C20 88.0(3) . . . . ? N8 C20 N7 C22 110.4(2) . . . . ? C23 C20 N7 C22 -122.4(2) . . . . ? C21 C20 N7 C22 0.8(2) . . . . ? N8 C20 N7 C18 -72.4(3) . . . . ? C23 C20 N7 C18 54.9(3) . . . . ? C21 C20 N7 C18 178.06(18) . . . . ? O4 C19 N8 C17 -0.7(3) . . . . ? N5 C19 N8 C17 177.45(19) . . . . ? O4 C19 N8 C20 -175.6(2) . . . . ? N5 C19 N8 C20 2.6(3) . . . . ? N10 C17 N8 C19 96.2(2) . . . . ? N10 C17 N8 C20 -89.6(3) . . . . ? N7 C20 N8 C19 -112.4(2) . . . . ? C23 C20 N8 C19 120.9(2) . . . . ? C21 C20 N8 C19 -2.7(2) . . . . ? N7 C20 N8 C17 72.9(3) . . . . ? C23 C20 N8 C17 -53.8(3) . . . . ? C21 C20 N8 C17 -177.39(19) . . . . ? O10 C14 N9 C13 -171.6(2) . . . . ? N12 C14 N9 C13 4.8(3) . . . . ? O10 C14 N9 C18 2.6(4) . . . . ? N12 C14 N9 C18 179.06(19) . . . . ? N10 C13 N9 C14 -112.6(2) . . . . ? C16 C13 N9 C14 120.8(2) . . . . ? C12 C13 N9 C14 -2.6(2) . . . . ? N10 C13 N9 C18 73.4(3) . . . . ? C16 C13 N9 C18 -53.1(3) . . . . ? C12 C13 N9 C18 -176.6(2) . . . . ? N7 C18 N9 C14 98.1(3) . . . . ? N7 C18 N9 C13 -88.4(3) . . . . ? O5 C11 N10 C13 172.2(2) . . . . ? N11 C11 N10 C13 -6.7(3) . . . . ? O5 C11 N10 C17 -1.0(3) . . . . ? N11 C11 N10 C17 -179.84(19) . . . . ? N9 C13 N10 C11 114.1(2) . . . . ? C16 C13 N10 C11 -119.3(2) . . . . ? C12 C13 N10 C11 3.9(2) . . . . ? N9 C13 N10 C17 -72.9(3) . . . . ? C16 C13 N10 C17 53.6(3) . . . . ? C12 C13 N10 C17 176.88(19) . . . . ? N8 C17 N10 C11 -99.2(2) . . . . ? N8 C17 N10 C13 88.5(3) . . . . ? O5 C11 N11 C9 -1.6(3) . . . . ? N10 C11 N11 C9 177.30(19) . . . . ? O5 C11 N11 C12 -172.1(2) . . . . ? N10 C11 N11 C12 6.7(3) . . . . ? N13 C9 N11 C11 103.5(2) . . . . ? N13 C9 N11 C12 -87.2(3) . . . . ? N12 C12 N11 C11 -114.0(2) . . . . ? C15 C12 N11 C11 119.9(2) . . . . ? C13 C12 N11 C11 -4.0(2) . . . . ? N12 C12 N11 C9 75.9(3) . . . . ? C15 C12 N11 C9 -50.2(3) . . . . ? C13 C12 N11 C9 -174.2(2) . . . . ? O10 C14 N12 C10 -1.7(3) . . . . ? N9 C14 N12 C10 -178.22(19) . . . . ? O10 C14 N12 C12 171.4(2) . . . . ? N9 C14 N12 C12 -5.1(3) . . . . ? N14 C10 N12 C14 -102.2(2) . . . . ? N14 C10 N12 C12 85.6(3) . . . . ? N11 C12 N12 C14 113.4(2) . . . . ? C15 C12 N12 C14 -120.5(2) . . . . ? C13 C12 N12 C14 3.3(2) . . . . ? N11 C12 N12 C10 -73.8(3) . . . . ? C15 C12 N12 C10 52.4(3) . . . . ? C13 C12 N12 C10 176.09(19) . . . . ? O3 C3 N13 C9 -0.3(3) . . . . ? N15 C3 N13 C9 -177.93(18) . . . . ? O3 C3 N13 C5 179.2(2) . . . . ? N15 C3 N13 C5 1.5(2) . . . . ? N11 C9 N13 C3 -95.3(2) . . . . ? N11 C9 N13 C5 85.4(3) . . . . ? N14 C5 N13 C3 108.4(2) . . . . ? C7 C5 N13 C3 -125.5(2) . . . . ? C4 C5 N13 C3 -0.6(2) . . . . ? N14 C5 N13 C9 -72.2(3) . . . . ? C7 C5 N13 C9 53.9(3) . . . . ? C4 C5 N13 C9 178.76(19) . . . . ? O8 C8 N14 C10 -0.8(3) . . . . ? N16 C8 N14 C10 178.05(19) . . . . ? O8 C8 N14 C5 -176.0(2) . . . . ? N16 C8 N14 C5 2.9(3) . . . . ? N12 C10 N14 C8 97.6(2) . . . . ? N12 C10 N14 C5 -87.9(3) . . . . ? N13 C5 N14 C8 -111.0(2) . . . . ? C7 C5 N14 C8 122.6(2) . . . . ? C4 C5 N14 C8 -2.0(2) . . . . ? N13 C5 N14 C10 74.2(3) . . . . ? C7 C5 N14 C10 -52.3(3) . . . . ? C4 C5 N14 C10 -176.8(2) . . . . ? O3 C3 N15 C1 2.5(3) . . . . ? N13 C3 N15 C1 -179.86(18) . . . . ? O3 C3 N15 C4 -179.5(2) . . . . ? N13 C3 N15 C4 -1.8(2) . . . . ? N17 C1 N15 C3 91.1(2) . . . . ? N17 C1 N15 C4 -86.7(3) . . . . ? N16 C4 N15 C3 -108.5(2) . . . . ? C6 C4 N15 C3 125.8(2) . . . . ? C5 C4 N15 C3 1.4(2) . . . . ? N16 C4 N15 C1 69.5(3) . . . . ? C6 C4 N15 C1 -56.3(3) . . . . ? C5 C4 N15 C1 179.28(18) . . . . ? O8 C8 N16 C2 0.3(3) . . . . ? N14 C8 N16 C2 -178.50(19) . . . . ? O8 C8 N16 C4 176.3(2) . . . . ? N14 C8 N16 C4 -2.5(3) . . . . ? N18 C2 N16 C8 -94.3(2) . . . . ? N18 C2 N16 C4 90.3(2) . . . . ? N15 C4 N16 C8 111.0(2) . . . . ? C6 C4 N16 C8 -123.0(2) . . . . ? C5 C4 N16 C8 1.2(2) . . . . ? N15 C4 N16 C2 -73.3(3) . . . . ? C6 C4 N16 C2 52.7(3) . . . . ? C5 C4 N16 C2 176.9(2) . . . . ? O2 C36 N17 C1 1.5(3) . . . . ? N20 C36 N17 C1 -178.30(18) . . . . ? O2 C36 N17 C38 171.3(2) . . . . ? N20 C36 N17 C38 -8.5(2) . . . . ? N15 C1 N17 C36 -100.2(2) . . . . ? N15 C1 N17 C38 91.2(3) . . . . ? N18 C38 N17 C36 115.0(2) . . . . ? C35 C38 N17 C36 -119.3(2) . . . . ? C37 C38 N17 C36 5.4(2) . . . . ? N18 C38 N17 C1 -75.6(2) . . . . ? C35 C38 N17 C1 50.1(3) . . . . ? C37 C38 N17 C1 174.77(19) . . . . ? O7 C39 N18 C2 2.2(4) . . . . ? N19 C39 N18 C2 179.98(19) . . . . ? O7 C39 N18 C38 -172.4(2) . . . . ? N19 C39 N18 C38 5.4(3) . . . . ? N16 C2 N18 C39 99.0(2) . . . . ? N16 C2 N18 C38 -87.1(2) . . . . ? N17 C38 N18 C39 -113.3(2) . . . . ? C35 C38 N18 C39 120.4(2) . . . . ? C37 C38 N18 C39 -3.6(2) . . . . ? N17 C38 N18 C2 72.3(3) . . . . ? C35 C38 N18 C2 -54.0(3) . . . . ? C37 C38 N18 C2 -177.98(19) . . . . ? O7 C39 N19 C34 -0.9(3) . . . . ? N18 C39 N19 C34 -178.64(19) . . . . ? O7 C39 N19 C37 172.8(2) . . . . ? N18 C39 N19 C37 -5.0(3) . . . . ? N2 C34 N19 C39 -101.7(2) . . . . ? N2 C34 N19 C37 85.4(3) . . . . ? N20 C37 N19 C39 111.9(2) . . . . ? C40 C37 N19 C39 -121.3(2) . . . . ? C38 C37 N19 C39 2.6(2) . . . . ? N20 C37 N19 C34 -74.7(3) . . . . ? C40 C37 N19 C34 52.1(3) . . . . ? C38 C37 N19 C34 175.9(2) . . . . ? O2 C36 N20 C33 -2.2(3) . . . . ? N17 C36 N20 C33 177.59(19) . . . . ? O2 C36 N20 C37 -171.5(2) . . . . ? N17 C36 N20 C37 8.2(3) . . . . ? N1 C33 N20 C36 103.1(2) . . . . ? N1 C33 N20 C37 -88.9(3) . . . . ? N19 C37 N20 C36 -113.9(2) . . . . ? C40 C37 N20 C36 119.0(2) . . . . ? C38 C37 N20 C36 -4.6(2) . . . . ? N19 C37 N20 C33 77.2(3) . . . . ? C40 C37 N20 C33 -50.0(3) . . . . ? C38 C37 N20 C33 -173.58(19) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.188 _refine_diff_density_min -0.578 _refine_diff_density_rms 0.096 # Attachment '- complex 2.CIF' data_complex2 _database_code_depnum_ccdc_archive 'CCDC 876880' #TrackingRef '- complex 2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C80 H154 Li4 N40 O59 V4' _chemical_formula_weight 2851.95 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 24.277(2) _cell_length_b 29.3537(15) _cell_length_c 20.5347(18) _cell_angle_alpha 90.00 _cell_angle_beta 121.609(4) _cell_angle_gamma 90.00 _cell_volume 12462.5(18) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.520 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 5960 _exptl_absorpt_coefficient_mu 0.402 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.941 _exptl_absorpt_correction_T_max 0.961 _exptl_absorpt_process_details ? _exptl_special_details ; empirical from equivalent reflections (XEMP in SHELXTL; Siemens,1994) ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Mercury ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 43170 _diffrn_reflns_av_R_equivalents 0.0434 _diffrn_reflns_av_sigmaI/netI 0.0326 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -34 _diffrn_reflns_limit_k_max 34 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10987 _reflns_number_gt 10309 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1734P)^2^+36.7846P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr. _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10987 _refine_ls_number_parameters 885 _refine_ls_number_restraints 96 _refine_ls_R_factor_all 0.1024 _refine_ls_R_factor_gt 0.0986 _refine_ls_wR_factor_ref 0.2916 _refine_ls_wR_factor_gt 0.2862 _refine_ls_goodness_of_fit_ref 1.156 _refine_ls_restrained_S_all 1.163 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.38594(4) 0.19689(3) 0.16313(5) 0.0459(3) Uani 1 1 d . . . V2 V 0.48015(4) 0.19666(4) 0.35212(5) 0.0540(3) Uani 1 1 d . . . O52 O 0.41049(19) 0.2027(2) 0.2608(2) 0.0812(15) Uani 1 1 d . . . O8 O 0.4848(5) 0.2482(5) 0.3925(7) 0.093(3) Uani 0.50 1 d P . . O8' O 0.4762(5) 0.2181(5) 0.4176(7) 0.093(3) Uani 0.50 1 d P . . O17 O 0.4742(4) 0.1605(4) 0.4102(6) 0.081(2) Uani 0.50 1 d P . . O17' O 0.4888(4) 0.1419(4) 0.3669(6) 0.081(2) Uani 0.50 1 d P . . O65 O 0.5500(2) 0.2045(4) 0.3506(3) 0.158(4) Uani 1 1 d . . . O78 O 0.3567(4) 0.2489(4) 0.1303(5) 0.0724(18) Uani 0.50 1 d P . . O78' O 0.3198(5) 0.2249(4) 0.1078(5) 0.0724(18) Uani 0.50 1 d P . . O79 O 0.3254(4) 0.1635(3) 0.1058(5) 0.0734(17) Uani 0.50 1 d P . . O79' O 0.3718(5) 0.1432(3) 0.1444(5) 0.0734(17) Uani 0.50 1 d P . . O1 O 0.20733(14) 0.36317(11) 0.39803(18) 0.0422(7) Uani 1 1 d . . . O2 O 0.36353(14) 0.54982(10) 0.25138(18) 0.0394(7) Uani 1 1 d . . . O3 O 0.43571(15) 0.38175(11) 0.35695(18) 0.0422(7) Uani 1 1 d . . . O4 O 0.29834(13) 0.47842(10) 0.11930(17) 0.0367(6) Uani 1 1 d . . . O5 O 0.34532(14) 0.37648(10) 0.18293(18) 0.0401(7) Uani 1 1 d . . . O6 O 0.44692(15) 0.48662(11) 0.40279(18) 0.0423(7) Uani 1 1 d . . . O7 O 0.11479(16) 0.35861(12) 0.21738(19) 0.0465(8) Uani 1 1 d . . . O9 O 0.06813(16) 0.45784(13) 0.1514(2) 0.0524(9) Uani 1 1 d . . . O10 O 0.13500(15) 0.52309(13) 0.29085(19) 0.0481(8) Uani 1 1 d . . . O13 O 0.21942(14) 0.46807(12) 0.44536(18) 0.0448(8) Uani 1 1 d . . . O21 O 0.11058(17) 0.42818(13) 0.3159(2) 0.0537(9) Uani 1 1 d . . . O23 O 0.42062(17) 0.46285(12) 0.2556(2) 0.0510(8) Uani 1 1 d . . . O51 O 0.5000 0.36942(19) 0.2500 0.0747(18) Uani 1 2 d S . . O60 O 0.0000 0.5033(2) 0.2500 0.0793(19) Uani 1 2 d S . . C24 C 0.2195(2) 0.29841(14) 0.3043(3) 0.0387(10) Uani 1 1 d . . . H24A H 0.1823 0.2988 0.3101 0.046 Uiso 1 1 calc R . . H24B H 0.2316 0.2668 0.3049 0.046 Uiso 1 1 calc R . . C26 C 0.24052(19) 0.47906(14) 0.0948(2) 0.0307(8) Uani 1 1 d . . . C30 C 0.2963(2) 0.35764(13) 0.1720(2) 0.0354(9) Uani 1 1 d . . . C31 C 0.41974(18) 0.48975(15) 0.4388(2) 0.0338(9) Uani 1 1 d . . . C34 C 0.31873(19) 0.56244(12) 0.2580(2) 0.0310(8) Uani 1 1 d . . . C35 C 0.2375(2) 0.55996(14) 0.1204(2) 0.0352(9) Uani 1 1 d . . . H35A H 0.2081 0.5833 0.0868 0.042 Uiso 1 1 calc R . . H35B H 0.2753 0.5604 0.1159 0.042 Uiso 1 1 calc R . . C36 C 0.4062(2) 0.36412(14) 0.3836(2) 0.0358(9) Uani 1 1 d . . . C37 C 0.2499(2) 0.55688(16) 0.4192(3) 0.0406(10) Uani 1 1 d . . . H37A H 0.2118 0.5511 0.4220 0.049 Uiso 1 1 calc R . . H37B H 0.2696 0.5848 0.4472 0.049 Uiso 1 1 calc R . . C40 C 0.3655(2) 0.52275(15) 0.4942(2) 0.0354(9) Uani 1 1 d . . . C42 C 0.2282(2) 0.30563(13) 0.1845(3) 0.0365(9) Uani 1 1 d . . . C43 C 0.1493(2) 0.34658(14) 0.1935(2) 0.0353(9) Uani 1 1 d . . . C44 C 0.2609(2) 0.35271(14) 0.4095(2) 0.0349(9) Uani 1 1 d . . . C45 C 0.13689(19) 0.50786(16) 0.0539(2) 0.0368(9) Uani 1 1 d . . . C46 C 0.45127(19) 0.41407(16) 0.4953(2) 0.0394(10) Uani 1 1 d . . . H46A H 0.4845 0.4183 0.4831 0.047 Uiso 1 1 calc R . . H46B H 0.4726 0.4056 0.5488 0.047 Uiso 1 1 calc R . . C47 C 0.3202(2) 0.40312(16) 0.5196(3) 0.0402(10) Uani 1 1 d . . . H47A H 0.2806 0.4007 0.5202 0.048 Uiso 1 1 calc R . . H47B H 0.3559 0.3960 0.5706 0.048 Uiso 1 1 calc R . . C48 C 0.2231(2) 0.39905(15) 0.0542(2) 0.0363(9) Uani 1 1 d . . . H48A H 0.1919 0.3860 0.0050 0.044 Uiso 1 1 calc R . . H48B H 0.2631 0.4036 0.0553 0.044 Uiso 1 1 calc R . . C49 C 0.2751(2) 0.47803(16) 0.4654(2) 0.0362(9) Uani 1 1 d . . . C50 C 0.3516(2) 0.30653(14) 0.2826(3) 0.0402(10) Uani 1 1 d . . . H50A H 0.3882 0.3116 0.2766 0.048 Uiso 1 1 calc R . . H50B H 0.3474 0.2739 0.2864 0.048 Uiso 1 1 calc R . . C53 C 0.3409(2) 0.31217(14) 0.4015(3) 0.0363(9) Uani 1 1 d . . . C54 C 0.1734(2) 0.54603(15) 0.2825(3) 0.0382(9) Uani 1 1 d . . . C55 C 0.3821(2) 0.56746(15) 0.3973(2) 0.0366(9) Uani 1 1 d . . . H55A H 0.4175 0.5675 0.3882 0.044 Uiso 1 1 calc R . . H55B H 0.3872 0.5941 0.4279 0.044 Uiso 1 1 calc R . . C56 C 0.13163(19) 0.45549(16) 0.0309(2) 0.0368(9) Uani 1 1 d . . . C57 C 0.09340(19) 0.46585(17) 0.1141(2) 0.0398(10) Uani 1 1 d . . . C58 C 0.1064(2) 0.54799(18) 0.1430(3) 0.0440(11) Uani 1 1 d . . . H58A H 0.0943 0.5742 0.1094 0.053 Uiso 1 1 calc R . . H58B H 0.0722 0.5430 0.1534 0.053 Uiso 1 1 calc R . . C59 C 0.1003(2) 0.5413(2) -0.0129(3) 0.0527(12) Uani 1 1 d . . . H59A H 0.1158 0.5384 -0.0472 0.079 Uiso 1 1 calc R . . H59B H 0.1074 0.5719 0.0065 0.079 Uiso 1 1 calc R . . H59C H 0.0549 0.5346 -0.0398 0.079 Uiso 1 1 calc R . . C61 C 0.2161(2) 0.59025(14) 0.2241(3) 0.0369(9) Uani 1 1 d . . . C62 C 0.0887(2) 0.38728(17) 0.0715(3) 0.0460(11) Uani 1 1 d . . . H62A H 0.0537 0.3850 0.0812 0.055 Uiso 1 1 calc R . . H62B H 0.0725 0.3760 0.0202 0.055 Uiso 1 1 calc R . . C63 C 0.2629(2) 0.59226(13) 0.3133(3) 0.0365(9) Uani 1 1 d . . . C64 C 0.3931(2) 0.56056(17) 0.5540(3) 0.0470(11) Uani 1 1 d . . . H64A H 0.3798 0.5558 0.5901 0.070 Uiso 1 1 calc R . . H64B H 0.3773 0.5895 0.5293 0.070 Uiso 1 1 calc R . . H64C H 0.4394 0.5601 0.5803 0.070 Uiso 1 1 calc R . . C66 C 0.4346(2) 0.4684(2) 0.6131(2) 0.0493(12) Uani 1 1 d . . . H66A H 0.4729 0.4860 0.6284 0.074 Uiso 1 1 calc R . . H66B H 0.4462 0.4370 0.6264 0.074 Uiso 1 1 calc R . . H66C H 0.4139 0.4797 0.6389 0.074 Uiso 1 1 calc R . . C67 C 0.38829(19) 0.47256(16) 0.5266(2) 0.0354(9) Uani 1 1 d . . . C68 C 0.3739(2) 0.34686(15) 0.4713(2) 0.0383(9) Uani 1 1 d . . . C69 C 0.0901(2) 0.4450(2) -0.0541(3) 0.0555(13) Uani 1 1 d . . . H69A H 0.0876 0.4126 -0.0617 0.083 Uiso 1 1 calc R . . H69B H 0.1090 0.4588 -0.0803 0.083 Uiso 1 1 calc R . . H69C H 0.0474 0.4570 -0.0741 0.083 Uiso 1 1 calc R . . C70 C 0.4180(3) 0.3253(2) 0.5493(3) 0.0587(14) Uani 1 1 d . . . H70A H 0.3935 0.3045 0.5604 0.088 Uiso 1 1 calc R . . H70B H 0.4360 0.3487 0.5877 0.088 Uiso 1 1 calc R . . H70C H 0.4523 0.3092 0.5491 0.088 Uiso 1 1 calc R . . C71 C 0.1868(2) 0.33504(15) 0.1103(2) 0.0392(10) Uani 1 1 d . . . C73 C 0.3565(3) 0.26221(17) 0.4224(4) 0.0564(13) Uani 1 1 d . . . H73A H 0.4019 0.2572 0.4444 0.085 Uiso 1 1 calc R . . H73B H 0.3325 0.2439 0.3773 0.085 Uiso 1 1 calc R . . H73C H 0.3447 0.2540 0.4588 0.085 Uiso 1 1 calc R . . C74 C 0.2257(3) 0.25427(16) 0.1719(4) 0.0573(14) Uani 1 1 d . . . H74A H 0.1816 0.2441 0.1473 0.086 Uiso 1 1 calc R . . H74B H 0.2510 0.2392 0.2203 0.086 Uiso 1 1 calc R . . H74C H 0.2427 0.2472 0.1402 0.086 Uiso 1 1 calc R . . C75 C 0.1524(3) 0.3089(2) 0.0352(3) 0.0630(16) Uani 1 1 d . . . H75A H 0.1284 0.3297 -0.0063 0.095 Uiso 1 1 calc R . . H75B H 0.1234 0.2871 0.0363 0.095 Uiso 1 1 calc R . . H75C H 0.1838 0.2932 0.0284 0.095 Uiso 1 1 calc R . . C76 C 0.1876(3) 0.63595(18) 0.1844(4) 0.0611(15) Uani 1 1 d . . . H76A H 0.1616 0.6314 0.1301 0.092 Uiso 1 1 calc R . . H76B H 0.2221 0.6568 0.1960 0.092 Uiso 1 1 calc R . . H76C H 0.1613 0.6483 0.2023 0.092 Uiso 1 1 calc R . . C77 C 0.2764(3) 0.63975(16) 0.3482(4) 0.0570(13) Uani 1 1 d . . . H77A H 0.3011 0.6374 0.4030 0.085 Uiso 1 1 calc R . . H77B H 0.2362 0.6549 0.3322 0.085 Uiso 1 1 calc R . . H77C H 0.3004 0.6569 0.3315 0.085 Uiso 1 1 calc R . . N8 N 0.20097(17) 0.31821(12) 0.2308(2) 0.0354(8) Uani 1 1 d . . . N11 N 0.41789(16) 0.45691(13) 0.4844(2) 0.0362(8) Uani 1 1 d . . . N12 N 0.31855(16) 0.36942(13) 0.4671(2) 0.0365(8) Uani 1 1 d . . . N14 N 0.22991(17) 0.56349(12) 0.3398(2) 0.0368(8) Uani 1 1 d . . . N15 N 0.32185(16) 0.57165(12) 0.3244(2) 0.0350(8) Uani 1 1 d . . . N16 N 0.25725(17) 0.57102(12) 0.1986(2) 0.0355(8) Uani 1 1 d . . . N17 N 0.20633(16) 0.51611(12) 0.09535(19) 0.0343(7) Uani 1 1 d . . . N18 N 0.38753(17) 0.52763(13) 0.4406(2) 0.0369(8) Uani 1 1 d . . . N19 N 0.19922(17) 0.44308(12) 0.0611(2) 0.0361(8) Uani 1 1 d . . . N20 N 0.27220(17) 0.32158(12) 0.3684(2) 0.0366(8) Uani 1 1 d . . . N22 N 0.36494(18) 0.32775(12) 0.3532(2) 0.0369(8) Uani 1 1 d . . . N25 N 0.11045(17) 0.50825(14) 0.1031(2) 0.0414(9) Uani 1 1 d . . . N27 N 0.32701(17) 0.44945(13) 0.5020(2) 0.0378(8) Uani 1 1 d . . . N28 N 0.23472(17) 0.36693(12) 0.1134(2) 0.0358(8) Uani 1 1 d . . . N29 N 0.29537(16) 0.51953(13) 0.4562(2) 0.0364(8) Uani 1 1 d . . . N32 N 0.29398(18) 0.32321(11) 0.2156(2) 0.0375(8) Uani 1 1 d . . . N33 N 0.40968(17) 0.37705(13) 0.4495(2) 0.0377(8) Uani 1 1 d . . . N38 N 0.14114(17) 0.35805(13) 0.1252(2) 0.0398(8) Uani 1 1 d . . . N39 N 0.16569(17) 0.55850(14) 0.2144(2) 0.0418(9) Uani 1 1 d . . . N41 N 0.10557(17) 0.43507(14) 0.0743(2) 0.0431(9) Uani 1 1 d . . . Li1 Li 0.0724(8) 0.4781(7) 0.2489(11) 0.117(6) Uani 1 1 d . . . Li4 Li 0.4290(4) 0.3987(3) 0.2613(5) 0.0472(18) Uani 1 1 d . . . O81 O 0.7962(3) 0.1912(2) 0.5157(4) 0.110(2) Uani 1 1 d U . . O84 O 0.5219(3) 0.1216(3) 0.8383(5) 0.132(2) Uani 1 1 d U . . O11 O 0.3209(4) 0.1582(3) 0.4883(4) 0.120(2) Uani 1 1 d U . . O16 O 0.2359(9) 0.0560(6) -0.2821(10) 0.143(5) Uani 0.50 1 d PU . . O80 O 0.4576(7) 0.1752(5) 0.5321(8) 0.097(3) Uani 0.50 1 d PU . . O80' O 0.4350(7) 0.1586(5) 0.5032(8) 0.097(3) Uani 0.50 1 d PU . . O12 O 0.5107(14) -0.0940(8) -0.242(2) 0.073(5) Uani 0.25 1 d PU . . O12' O 0.5181(13) -0.0935(8) -0.2675(14) 0.073(5) Uani 0.25 1 d PU . . O14 O 0.0620(6) -0.1185(4) -0.2330(8) 0.090(2) Uani 0.50 1 d PU . . O14' O 0.0433(6) -0.1159(4) -0.2796(7) 0.090(2) Uani 0.50 1 d PU . . O15 O 0.4500(7) 0.3087(5) 0.1492(9) 0.101(3) Uani 0.50 1 d PU . . O15' O 0.4262(7) 0.3151(5) 0.1053(9) 0.101(3) Uani 0.50 1 d PU . . O18 O 0.5759(12) 0.3173(8) 0.5142(13) 0.091(4) Uani 0.25 1 d PU . . O18' O 0.5345(12) 0.2976(8) 0.5018(13) 0.091(4) Uani 0.25 1 d PU . . O19 O 0.2873(9) 0.2828(7) 0.5793(12) 0.172(7) Uani 0.50 1 d PU . . O20 O 0.0621(9) 0.2477(7) 0.1300(12) 0.171(7) Uani 0.50 1 d PU . . 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 0.0316(4) 0.0700(6) 0.0367(5) 0.0001(4) 0.0184(4) 0.0007(3) V2 0.0338(5) 0.0901(7) 0.0387(5) 0.0156(4) 0.0195(4) 0.0119(4) O52 0.043(2) 0.158(5) 0.042(2) 0.014(2) 0.0223(18) 0.016(2) O8 0.073(4) 0.136(9) 0.085(6) -0.006(5) 0.052(4) 0.009(5) O8' 0.073(4) 0.136(9) 0.085(6) -0.006(5) 0.052(4) 0.009(5) O17 0.063(4) 0.106(5) 0.068(4) 0.035(4) 0.029(3) 0.011(3) O17' 0.063(4) 0.106(5) 0.068(4) 0.035(4) 0.029(3) 0.011(3) O65 0.035(2) 0.396(14) 0.046(3) -0.001(4) 0.023(2) 0.008(4) O78 0.063(4) 0.095(5) 0.061(4) 0.012(4) 0.033(4) 0.014(3) O78' 0.063(4) 0.095(5) 0.061(4) 0.012(4) 0.033(4) 0.014(3) O79 0.064(4) 0.089(5) 0.071(4) -0.006(3) 0.039(3) -0.011(3) O79' 0.064(4) 0.089(5) 0.071(4) -0.006(3) 0.039(3) -0.011(3) O1 0.0326(16) 0.0564(18) 0.0415(17) -0.0026(14) 0.0222(14) -0.0007(13) O2 0.0310(15) 0.0482(17) 0.0438(17) -0.0050(13) 0.0231(13) 0.0018(12) O3 0.0432(17) 0.0491(17) 0.0461(17) 0.0022(14) 0.0317(15) -0.0033(14) O4 0.0285(15) 0.0417(15) 0.0411(16) -0.0030(12) 0.0192(13) -0.0011(11) O5 0.0373(16) 0.0443(16) 0.0456(17) -0.0005(13) 0.0264(14) -0.0069(13) O6 0.0410(17) 0.0563(18) 0.0424(17) -0.0034(14) 0.0306(15) -0.0024(14) O7 0.0399(17) 0.060(2) 0.0462(18) 0.0020(15) 0.0274(15) 0.0014(14) O9 0.0382(17) 0.077(2) 0.0492(19) 0.0049(17) 0.0281(16) -0.0060(16) O10 0.0335(16) 0.069(2) 0.0455(18) -0.0016(16) 0.0236(15) -0.0074(15) O13 0.0304(16) 0.0610(19) 0.0462(18) -0.0085(15) 0.0224(14) -0.0122(14) O21 0.0440(18) 0.066(2) 0.0474(19) -0.0060(16) 0.0217(16) 0.0042(16) O23 0.054(2) 0.0482(18) 0.051(2) -0.0017(15) 0.0271(17) 0.0013(15) O51 0.073(4) 0.056(3) 0.134(6) 0.000 0.081(4) 0.000 O60 0.039(3) 0.080(4) 0.121(6) 0.000 0.044(3) 0.000 C24 0.043(2) 0.036(2) 0.046(2) 0.0006(18) 0.029(2) -0.0097(17) C26 0.029(2) 0.040(2) 0.0237(18) 0.0040(15) 0.0143(16) 0.0000(16) C30 0.046(2) 0.0305(19) 0.040(2) -0.0092(16) 0.030(2) -0.0040(17) C31 0.0262(19) 0.048(2) 0.0270(19) -0.0094(17) 0.0135(16) -0.0095(16) C34 0.030(2) 0.0256(17) 0.041(2) -0.0002(15) 0.0211(18) -0.0025(15) C35 0.036(2) 0.038(2) 0.037(2) 0.0075(17) 0.0226(18) 0.0035(16) C36 0.032(2) 0.039(2) 0.040(2) 0.0079(17) 0.0208(19) 0.0081(17) C37 0.040(2) 0.051(2) 0.040(2) -0.0139(19) 0.027(2) -0.0044(19) C40 0.031(2) 0.052(2) 0.0266(19) -0.0111(17) 0.0176(17) -0.0116(17) C42 0.047(2) 0.031(2) 0.044(2) -0.0092(17) 0.032(2) -0.0094(17) C43 0.035(2) 0.039(2) 0.038(2) -0.0075(17) 0.0230(19) -0.0107(17) C44 0.033(2) 0.042(2) 0.031(2) 0.0062(17) 0.0179(17) 0.0023(17) C45 0.026(2) 0.053(2) 0.028(2) 0.0062(18) 0.0126(17) 0.0009(17) C46 0.0219(18) 0.058(3) 0.033(2) 0.0028(19) 0.0107(16) -0.0007(17) C47 0.040(2) 0.054(3) 0.035(2) -0.0013(19) 0.0258(19) -0.0071(19) C48 0.042(2) 0.044(2) 0.032(2) -0.0058(17) 0.0250(19) -0.0071(18) C49 0.031(2) 0.056(2) 0.0251(19) -0.0118(18) 0.0170(17) -0.0095(18) C50 0.045(2) 0.036(2) 0.050(3) 0.0018(18) 0.032(2) 0.0050(18) C53 0.037(2) 0.035(2) 0.042(2) 0.0133(17) 0.0248(19) 0.0064(17) C54 0.031(2) 0.046(2) 0.043(2) -0.0033(18) 0.0236(19) 0.0049(18) C55 0.033(2) 0.044(2) 0.037(2) -0.0087(18) 0.0204(18) -0.0119(17) C56 0.028(2) 0.056(3) 0.0230(19) 0.0030(17) 0.0112(16) -0.0034(18) C57 0.0230(19) 0.064(3) 0.029(2) 0.0065(19) 0.0119(17) 0.0002(18) C58 0.025(2) 0.065(3) 0.041(2) 0.008(2) 0.0172(19) 0.0105(19) C59 0.036(2) 0.076(3) 0.040(3) 0.022(2) 0.015(2) 0.012(2) C61 0.036(2) 0.035(2) 0.050(2) 0.0040(18) 0.030(2) 0.0075(17) C62 0.030(2) 0.061(3) 0.041(2) 0.003(2) 0.0140(19) -0.010(2) C63 0.043(2) 0.0273(19) 0.048(2) -0.0025(17) 0.030(2) 0.0040(16) C64 0.047(3) 0.057(3) 0.040(2) -0.018(2) 0.026(2) -0.018(2) C66 0.045(3) 0.075(3) 0.027(2) -0.007(2) 0.018(2) -0.014(2) C67 0.0262(19) 0.055(2) 0.028(2) -0.0101(18) 0.0165(17) -0.0122(17) C68 0.032(2) 0.046(2) 0.038(2) 0.0122(18) 0.0189(19) 0.0024(17) C69 0.041(3) 0.082(4) 0.026(2) -0.001(2) 0.006(2) -0.009(2) C70 0.050(3) 0.074(4) 0.043(3) 0.025(3) 0.018(2) 0.010(3) C71 0.041(2) 0.046(2) 0.035(2) -0.0151(18) 0.0233(19) -0.0164(19) C73 0.061(3) 0.044(3) 0.074(4) 0.023(2) 0.042(3) 0.012(2) C74 0.076(4) 0.032(2) 0.083(4) -0.015(2) 0.054(3) -0.012(2) C75 0.083(4) 0.066(3) 0.046(3) -0.033(3) 0.039(3) -0.044(3) C76 0.072(4) 0.046(3) 0.079(4) 0.021(3) 0.048(3) 0.027(3) C77 0.069(3) 0.034(2) 0.079(4) -0.015(2) 0.045(3) -0.002(2) N8 0.0372(19) 0.0350(17) 0.0409(19) -0.0024(15) 0.0254(16) -0.0025(14) N11 0.0303(17) 0.050(2) 0.0321(18) -0.0041(15) 0.0188(15) -0.0064(15) N12 0.0288(17) 0.049(2) 0.0344(18) -0.0001(15) 0.0184(15) -0.0021(15) N14 0.0361(19) 0.0406(18) 0.043(2) -0.0048(15) 0.0274(17) -0.0019(15) N15 0.0292(17) 0.0410(18) 0.0405(19) -0.0058(15) 0.0222(15) -0.0014(14) N16 0.0340(18) 0.0378(18) 0.0409(19) 0.0058(15) 0.0240(16) 0.0069(14) N17 0.0263(16) 0.0421(18) 0.0326(17) 0.0061(14) 0.0143(14) 0.0023(14) N18 0.0357(19) 0.047(2) 0.0339(18) -0.0065(15) 0.0223(16) -0.0067(15) N19 0.0291(17) 0.0465(19) 0.0329(18) -0.0018(15) 0.0165(15) -0.0034(15) N20 0.0357(18) 0.0380(18) 0.041(2) 0.0015(15) 0.0238(16) -0.0012(14) N22 0.0400(19) 0.0330(17) 0.047(2) 0.0028(15) 0.0290(17) -0.0003(14) N25 0.0311(18) 0.060(2) 0.0371(19) 0.0045(17) 0.0203(16) -0.0004(16) N27 0.0322(18) 0.050(2) 0.0356(19) -0.0059(15) 0.0208(16) -0.0121(15) N28 0.0338(18) 0.0415(18) 0.0351(18) -0.0064(15) 0.0203(16) -0.0125(15) N29 0.0276(17) 0.049(2) 0.0352(18) -0.0059(15) 0.0179(15) -0.0063(15) N32 0.043(2) 0.0311(17) 0.049(2) -0.0028(15) 0.0314(18) -0.0044(15) N33 0.0325(18) 0.048(2) 0.0371(19) 0.0058(15) 0.0213(16) -0.0023(15) N38 0.0339(19) 0.051(2) 0.0342(19) -0.0032(16) 0.0177(16) -0.0073(16) N39 0.0300(18) 0.057(2) 0.042(2) 0.0047(17) 0.0206(16) 0.0049(16) N41 0.0291(18) 0.061(2) 0.038(2) 0.0062(17) 0.0168(16) -0.0100(16) Li1 0.086(10) 0.154(15) 0.126(13) -0.039(11) 0.066(10) -0.022(9) Li4 0.042(4) 0.052(4) 0.062(5) 0.000(4) 0.037(4) 0.002(3) O81 0.078(3) 0.110(4) 0.099(4) 0.012(3) 0.017(3) -0.003(3) O84 0.088(4) 0.156(6) 0.150(6) 0.018(4) 0.060(4) 0.000(4) O11 0.144(5) 0.134(5) 0.114(4) -0.003(4) 0.090(4) -0.029(4) O16 0.157(9) 0.126(8) 0.129(9) -0.012(7) 0.061(7) 0.006(7) O80 0.096(6) 0.095(6) 0.097(6) 0.013(4) 0.048(5) 0.015(4) O80' 0.096(6) 0.095(6) 0.097(6) 0.013(4) 0.048(5) 0.015(4) O12 0.077(8) 0.068(4) 0.071(8) -0.001(6) 0.037(6) 0.001(5) O12' 0.077(8) 0.068(4) 0.071(8) -0.001(6) 0.037(6) 0.001(5) O14 0.085(5) 0.089(4) 0.100(6) 0.006(5) 0.051(5) -0.007(3) O14' 0.085(5) 0.089(4) 0.100(6) 0.006(5) 0.051(5) -0.007(3) O15 0.098(6) 0.091(4) 0.115(7) -0.014(5) 0.057(5) -0.007(4) O15' 0.098(6) 0.091(4) 0.115(7) -0.014(5) 0.057(5) -0.007(4) O18 0.096(7) 0.100(7) 0.081(6) -0.018(5) 0.048(6) 0.005(5) O18' 0.096(7) 0.100(7) 0.081(6) -0.018(5) 0.048(6) 0.005(5) O19 0.151(10) 0.187(10) 0.190(10) 0.071(8) 0.097(8) -0.033(7) O20 0.140(9) 0.167(10) 0.197(11) -0.011(8) 0.082(8) -0.042(8) _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 O79' 1.616(10) . ? V1 O78' 1.623(9) . ? V1 O79 1.641(9) . ? V1 O78 1.669(10) . ? V1 O65 1.735(5) 2_655 ? V1 O52 1.776(4) . ? V2 O8' 1.534(11) . ? V2 O17' 1.630(11) . ? V2 O17 1.658(9) . ? V2 O8 1.701(13) . ? V2 O65 1.727(5) . ? V2 O52 1.756(4) . ? O8 O8' 1.099(16) . ? O8' O17 1.696(18) . ? O17 O17' 1.242(14) . ? O65 V1 1.735(5) 2_655 ? O78 O78' 1.037(12) . ? O78' O79 1.811(15) . ? O79 O79' 1.147(13) . ? O1 C44 1.234(5) . ? O2 C34 1.222(5) . ? O3 C36 1.220(5) . ? O3 Li4 1.949(9) . ? O4 C26 1.218(5) . ? O5 C30 1.222(5) . ? O5 Li4 1.928(9) . ? O6 C31 1.226(5) . ? O7 C43 1.224(5) . ? O9 C57 1.228(5) . ? O9 Li1 2.039(17) . ? O10 C54 1.232(5) . ? O10 Li1 1.850(17) . ? O13 C49 1.225(5) . ? O21 Li1 1.89(2) . ? O23 Li4 1.892(9) . ? O51 Li4 2.044(8) 2_655 ? O51 Li4 2.044(8) . ? O60 Li1 1.919(16) 2 ? O60 Li1 1.919(16) . ? C24 N20 1.437(6) . ? C24 N8 1.453(6) . ? C26 N19 1.368(5) . ? C26 N17 1.371(5) . ? C30 N28 1.368(6) . ? C30 N32 1.370(6) . ? C31 N11 1.360(6) . ? C31 N18 1.371(6) . ? C34 N15 1.353(5) . ? C34 N16 1.367(5) . ? C35 N17 1.445(5) . ? C35 N16 1.452(6) . ? C36 N33 1.366(6) . ? C36 N22 1.371(6) . ? C37 N14 1.450(6) . ? C37 N29 1.456(6) . ? C40 N29 1.457(5) . ? C40 N18 1.461(5) . ? C40 C64 1.526(6) . ? C40 C67 1.592(6) . ? C42 N8 1.463(5) . ? C42 N32 1.467(6) . ? C42 C74 1.525(6) . ? C42 C71 1.572(7) . ? C43 N38 1.353(6) . ? C43 N8 1.359(6) . ? C44 N20 1.365(6) . ? C44 N12 1.365(6) . ? C45 N25 1.454(5) . ? C45 N17 1.456(5) . ? C45 C59 1.535(6) . ? C45 C56 1.593(7) . ? C46 N33 1.445(6) . ? C46 N11 1.448(6) . ? C47 N27 1.439(6) . ? C47 N12 1.447(6) . ? C48 N28 1.444(6) . ? C48 N19 1.453(6) . ? C49 N29 1.364(6) . ? C49 N27 1.365(6) . ? C50 N32 1.440(6) . ? C50 N22 1.449(6) . ? C53 N20 1.461(6) . ? C53 N22 1.462(5) . ? C53 C73 1.519(6) . ? C53 C68 1.591(7) . ? C54 N14 1.356(6) . ? C54 N39 1.360(6) . ? C55 N18 1.432(6) . ? C55 N15 1.449(6) . ? C56 N41 1.463(5) . ? C56 N19 1.464(5) . ? C56 C69 1.522(6) . ? C57 N41 1.352(6) . ? C57 N25 1.368(6) . ? C58 N39 1.452(6) . ? C58 N25 1.458(6) . ? C61 N16 1.461(5) . ? C61 N39 1.467(6) . ? C61 C76 1.533(6) . ? C61 C63 1.571(6) . ? C62 N38 1.450(6) . ? C62 N41 1.454(6) . ? C63 N14 1.452(6) . ? C63 N15 1.457(5) . ? C63 C77 1.523(6) . ? C66 C67 1.531(6) . ? C67 N11 1.460(5) . ? C67 N27 1.463(5) . ? C68 N33 1.465(5) . ? C68 N12 1.460(6) . ? C68 C70 1.522(6) . ? C71 N38 1.461(6) . ? C71 N28 1.468(5) . ? C71 C75 1.521(6) . ? Li1 Li1 3.54(3) 2 ? O80 O80' 0.740(17) . ? O12 O12 0.45(6) 2_654 ? O12 O12' 0.64(4) . ? O12 O12' 0.82(3) 2_654 ? O12' O12 0.82(3) 2_654 ? O12' O12' 1.40(4) 2_654 ? O14 O14' 0.821(14) . ? O15 O15' 0.797(17) . ? O18 O18' 1.07(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O79' V1 O78' 108.6(5) . . ? O79' V1 O79 41.2(4) . . ? O78' V1 O79 67.4(5) . . ? O79' V1 O78 143.4(5) . . ? O78' V1 O78 36.7(4) . . ? O79 V1 O78 103.0(5) . . ? O79' V1 O65 100.6(5) . 2_655 ? O78' V1 O65 117.6(4) . 2_655 ? O79 V1 O65 120.2(4) . 2_655 ? O78 V1 O65 92.6(5) . 2_655 ? O79' V1 O52 105.4(4) . . ? O78' V1 O52 111.4(4) . . ? O79 V1 O52 120.7(4) . . ? O78 V1 O52 100.9(4) . . ? O65 V1 O52 111.8(2) 2_655 . ? O8' V2 O17' 107.6(6) . . ? O8' V2 O17 64.0(7) . . ? O17' V2 O17 44.4(5) . . ? O8' V2 O8 39.3(5) . . ? O17' V2 O8 144.9(6) . . ? O17 V2 O8 103.2(6) . . ? O8' V2 O65 118.4(5) . . ? O17' V2 O65 95.9(5) . . ? O17 V2 O65 123.7(4) . . ? O8 V2 O65 94.3(5) . . ? O8' V2 O52 115.3(4) . . ? O17' V2 O52 104.8(4) . . ? O17 V2 O52 115.7(4) . . ? O8 V2 O52 102.2(4) . . ? O65 V2 O52 111.8(2) . . ? V2 O52 V1 139.6(3) . . ? O8' O8 V2 62.1(9) . . ? O8 O8' V2 78.6(9) . . ? O8 O8' O17 139.8(11) . . ? V2 O8' O17 61.5(6) . . ? O17' O17 V2 66.6(6) . . ? O17' O17 O8' 119.9(9) . . ? V2 O17 O8' 54.4(5) . . ? O17 O17' V2 69.0(7) . . ? V1 O65 V2 163.4(7) 2_655 . ? O78' O78 V1 69.3(8) . . ? O78 O78' V1 74.0(8) . . ? O78 O78' O79 128.8(9) . . ? V1 O78' O79 56.8(4) . . ? O79' O79 V1 68.2(7) . . ? O79' O79 O78' 124.1(9) . . ? V1 O79 O78' 55.9(4) . . ? O79 O79' V1 70.5(7) . . ? C36 O3 Li4 143.2(4) . . ? C30 O5 Li4 143.7(4) . . ? C57 O9 Li1 140.4(6) . . ? C54 O10 Li1 145.3(6) . . ? Li4 O51 Li4 130.3(6) 2_655 . ? Li1 O60 Li1 134.6(13) 2 . ? N20 C24 N8 113.9(3) . . ? O4 C26 N19 125.2(4) . . ? O4 C26 N17 125.5(4) . . ? N19 C26 N17 109.3(3) . . ? O5 C30 N28 125.5(4) . . ? O5 C30 N32 125.7(4) . . ? N28 C30 N32 108.8(4) . . ? O6 C31 N11 125.7(4) . . ? O6 C31 N18 124.9(4) . . ? N11 C31 N18 109.4(3) . . ? O2 C34 N15 126.1(4) . . ? O2 C34 N16 125.2(4) . . ? N15 C34 N16 108.7(3) . . ? N17 C35 N16 113.7(3) . . ? O3 C36 N33 125.5(4) . . ? O3 C36 N22 125.9(4) . . ? N33 C36 N22 108.5(4) . . ? N14 C37 N29 113.8(3) . . ? N29 C40 N18 113.0(3) . . ? N29 C40 C64 112.0(4) . . ? N18 C40 C64 110.8(3) . . ? N29 C40 C67 102.5(3) . . ? N18 C40 C67 102.8(3) . . ? C64 C40 C67 115.3(4) . . ? N8 C42 N32 112.8(3) . . ? N8 C42 C74 111.5(4) . . ? N32 C42 C74 111.1(4) . . ? N8 C42 C71 102.3(3) . . ? N32 C42 C71 103.1(3) . . ? C74 C42 C71 115.5(4) . . ? O7 C43 N38 125.8(4) . . ? O7 C43 N8 125.1(4) . . ? N38 C43 N8 109.1(4) . . ? O1 C44 N20 125.6(4) . . ? O1 C44 N12 125.1(4) . . ? N20 C44 N12 109.3(4) . . ? N25 C45 N17 112.9(3) . . ? N25 C45 C59 110.9(4) . . ? N17 C45 C59 111.5(4) . . ? N25 C45 C56 102.5(3) . . ? N17 C45 C56 102.8(3) . . ? C59 C45 C56 115.7(4) . . ? N33 C46 N11 114.1(3) . . ? N27 C47 N12 114.9(3) . . ? N28 C48 N19 114.3(3) . . ? O13 C49 N29 125.5(4) . . ? O13 C49 N27 125.2(4) . . ? N29 C49 N27 109.2(3) . . ? N32 C50 N22 113.9(3) . . ? N20 C53 N22 113.0(3) . . ? N20 C53 C73 111.6(4) . . ? N22 C53 C73 111.5(4) . . ? N20 C53 C68 102.2(3) . . ? N22 C53 C68 102.7(3) . . ? C73 C53 C68 115.5(4) . . ? O10 C54 N14 125.5(4) . . ? O10 C54 N39 125.7(4) . . ? N14 C54 N39 108.8(4) . . ? N18 C55 N15 115.2(3) . . ? N41 C56 N19 112.8(3) . . ? N41 C56 C69 112.2(4) . . ? N19 C56 C69 110.9(4) . . ? N41 C56 C45 102.0(3) . . ? N19 C56 C45 102.5(3) . . ? C69 C56 C45 115.9(4) . . ? O9 C57 N41 126.0(5) . . ? O9 C57 N25 124.8(5) . . ? N41 C57 N25 109.1(4) . . ? N39 C58 N25 114.4(3) . . ? N16 C61 N39 112.6(3) . . ? N16 C61 C76 110.5(4) . . ? N39 C61 C76 111.8(4) . . ? N16 C61 C63 102.6(3) . . ? N39 C61 C63 102.9(3) . . ? C76 C61 C63 115.8(4) . . ? N38 C62 N41 115.1(4) . . ? N14 C63 N15 112.9(3) . . ? N14 C63 C77 112.3(4) . . ? N15 C63 C77 110.8(4) . . ? N14 C63 C61 102.2(3) . . ? N15 C63 C61 102.6(3) . . ? C77 C63 C61 115.4(4) . . ? N11 C67 N27 112.2(3) . . ? N11 C67 C66 111.9(4) . . ? N27 C67 C66 111.0(4) . . ? N11 C67 C40 102.4(3) . . ? N27 C67 C40 102.5(3) . . ? C66 C67 C40 116.2(4) . . ? N33 C68 N12 112.5(3) . . ? N33 C68 C70 111.7(4) . . ? N12 C68 C70 111.5(4) . . ? N33 C68 C53 102.2(3) . . ? N12 C68 C53 103.0(3) . . ? C70 C68 C53 115.3(4) . . ? N38 C71 N28 111.5(3) . . ? N38 C71 C75 111.8(4) . . ? N28 C71 C75 111.6(4) . . ? N38 C71 C42 102.8(3) . . ? N28 C71 C42 102.6(3) . . ? C75 C71 C42 115.9(4) . . ? C43 N8 C24 121.4(4) . . ? C43 N8 C42 112.8(4) . . ? C24 N8 C42 125.2(4) . . ? C31 N11 C46 120.3(3) . . ? C31 N11 C67 112.9(4) . . ? C46 N11 C67 126.2(4) . . ? C44 N12 C47 120.5(4) . . ? C44 N12 C68 112.4(4) . . ? C47 N12 C68 127.0(4) . . ? C54 N14 C37 121.0(4) . . ? C54 N14 C63 113.6(4) . . ? C37 N14 C63 125.1(4) . . ? C34 N15 C55 121.2(3) . . ? C34 N15 C63 113.2(3) . . ? C55 N15 C63 125.0(3) . . ? C34 N16 C35 121.2(3) . . ? C34 N16 C61 112.6(3) . . ? C35 N16 C61 126.2(3) . . ? C26 N17 C35 120.2(3) . . ? C26 N17 C45 112.5(3) . . ? C35 N17 C45 125.9(3) . . ? C31 N18 C55 120.9(3) . . ? C31 N18 C40 112.3(4) . . ? C55 N18 C40 126.6(4) . . ? C26 N19 C48 120.8(3) . . ? C26 N19 C56 112.5(3) . . ? C48 N19 C56 126.6(3) . . ? C44 N20 C24 120.8(4) . . ? C44 N20 C53 112.9(4) . . ? C24 N20 C53 126.0(4) . . ? C36 N22 C50 121.1(4) . . ? C36 N22 C53 113.0(4) . . ? C50 N22 C53 125.7(4) . . ? C57 N25 C45 113.0(4) . . ? C57 N25 C58 121.3(4) . . ? C45 N25 C58 125.5(4) . . ? C49 N27 C47 121.6(4) . . ? C49 N27 C67 112.5(4) . . ? C47 N27 C67 125.6(4) . . ? C30 N28 C48 120.8(3) . . ? C30 N28 C71 112.7(3) . . ? C48 N28 C71 125.4(4) . . ? C49 N29 C40 112.9(4) . . ? C49 N29 C37 121.0(3) . . ? C40 N29 C37 125.8(4) . . ? C30 N32 C50 121.6(4) . . ? C30 N32 C42 112.5(4) . . ? C50 N32 C42 125.9(4) . . ? C36 N33 C46 120.8(4) . . ? C36 N33 C68 113.3(4) . . ? C46 N33 C68 125.5(4) . . ? C43 N38 C62 121.9(4) . . ? C43 N38 C71 112.8(4) . . ? C62 N38 C71 125.1(4) . . ? C54 N39 C58 120.7(4) . . ? C54 N39 C61 112.1(4) . . ? C58 N39 C61 126.0(4) . . ? C57 N41 C62 121.4(4) . . ? C57 N41 C56 113.3(4) . . ? C62 N41 C56 125.0(4) . . ? O10 Li1 O21 104.2(9) . . ? O10 Li1 O60 104.6(9) . . ? O21 Li1 O60 113.2(9) . . ? O10 Li1 O9 105.8(8) . . ? O21 Li1 O9 104.0(9) . . ? O60 Li1 O9 123.2(9) . . ? O10 Li1 Li1 125.0(6) . 2 ? O21 Li1 Li1 95.9(6) . 2 ? O60 Li1 Li1 22.7(6) . 2 ? O9 Li1 Li1 118.2(9) . 2 ? O23 Li4 O5 104.6(4) . . ? O23 Li4 O3 105.4(4) . . ? O5 Li4 O3 104.5(4) . . ? O23 Li4 O51 118.8(4) . . ? O5 Li4 O51 110.2(4) . . ? O3 Li4 O51 112.2(4) . . ? O12 O12 O12' 97(10) 2_654 . ? O12 O12 O12' 50(8) 2_654 2_654 ? O12' O12 O12' 147(5) . 2_654 ? O12 O12' O12 33(5) . 2_654 ? O12 O12' O12' 19(3) . 2_654 ? O12 O12' O12' 14(3) 2_654 2_654 ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.398 _refine_diff_density_min -1.070 _refine_diff_density_rms 0.136 # Attachment '- complex 3.CIF' data_complex3 _database_code_depnum_ccdc_archive 'CCDC 876881' #TrackingRef '- complex 3.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C60 H94 N40 Na4 O49 V4' _chemical_formula_weight 2455.47 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.945(3) _cell_length_b 18.956(3) _cell_length_c 19.344(4) _cell_angle_alpha 90.00 _cell_angle_beta 108.933(11) _cell_angle_gamma 90.00 _cell_volume 5183.7(18) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.573 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2524 _exptl_absorpt_coefficient_mu 0.478 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9105 _exptl_absorpt_correction_T_max 0.9189 _exptl_absorpt_process_details ? _exptl_special_details ; empirical from equivalent reflections (XEMP in SHELXTL; Siemens,1994) ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Mercury ; _diffrn_measurement_method dtprofit.ref _diffrn_detector_area_resol_mean ? _diffrn_standards_number none _diffrn_standards_interval_count none _diffrn_standards_interval_time none _diffrn_standards_decay_% none _diffrn_reflns_number 33421 _diffrn_reflns_av_R_equivalents 0.0856 _diffrn_reflns_av_sigmaI/netI 0.0795 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 25.50 _reflns_number_total 9595 _reflns_number_gt 6107 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Corp., 2000)' _computing_cell_refinement 'CrystalClear (Rigaku Corp., 2000)' _computing_data_reduction 'CrystalClear (Rigaku Corp., 2000)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr. _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9595 _refine_ls_number_parameters 680 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.2039 _refine_ls_R_factor_gt 0.1563 _refine_ls_wR_factor_ref 0.3888 _refine_ls_wR_factor_gt 0.3542 _refine_ls_goodness_of_fit_ref 1.921 _refine_ls_restrained_S_all 1.921 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.49923(13) 0.00198(16) 0.37150(10) 0.0892(10) Uani 1 1 d . . . V2 V 0.35091(10) 0.00275(9) 0.46225(9) 0.0423(5) Uani 1 1 d . . . Na1 Na 0.1565(3) -0.3458(2) 0.4138(2) 0.0597(11) Uani 1 1 d . . . Na2 Na 0.1618(2) -0.13886(19) 0.41615(18) 0.0427(9) Uani 1 1 d . . . O1 O 0.2695(4) -0.3382(3) 0.3544(3) 0.0432(16) Uani 1 1 d . . . O2 O 0.2569(4) -0.1630(3) 0.3451(3) 0.0415(15) Uani 1 1 d . . . O3 O 0.0498(4) -0.1049(3) 0.2963(3) 0.0400(15) Uani 1 1 d . . . O4 O 0.0597(4) -0.3934(3) 0.3010(3) 0.0374(14) Uani 1 1 d . . . O5 O -0.0786(5) -0.2499(3) 0.2649(3) 0.0456(17) Uani 1 1 d . . . O6 O 0.2663(5) -0.1593(3) 0.0300(3) 0.0461(16) Uani 1 1 d . . . O7 O 0.2598(5) -0.3343(3) 0.0341(3) 0.0448(16) Uani 1 1 d . . . O8 O 0.0566(4) -0.3973(3) -0.0204(3) 0.0347(14) Uani 1 1 d . . . O9 O -0.0787(5) -0.2543(3) -0.0543(3) 0.0407(15) Uani 1 1 d . . . O10 O 0.0528(4) -0.1087(3) -0.0222(3) 0.0419(15) Uani 1 1 d . . . O11 O 0.0729(6) -0.2430(3) 0.3937(4) 0.060(2) Uani 1 1 d . . . O12 O 0.2389(4) -0.0182(4) 0.4345(3) 0.0499(17) Uani 1 1 d . . . O13 O 0.4047(5) -0.0292(5) 0.3994(4) 0.077(2) Uani 1 1 d . . . O14 O 0.3610(6) 0.0882(5) 0.4670(6) 0.109(3) Uani 1 1 d . . . O15 O 0.5921(5) 0.0339(5) 0.4496(4) 0.083(3) Uani 1 1 d . . . O16 O 0.4612(8) 0.0637(11) 0.3127(6) 0.215(9) Uani 1 1 d . . . O17 O 0.5338(7) -0.0549(10) 0.3279(6) 0.195(8) Uani 1 1 d . . . N1 N 0.3555(4) -0.1834(4) 0.1485(3) 0.0299(15) Uani 1 1 d . . . N2 N 0.3528(5) -0.1843(4) 0.2752(3) 0.0302(15) Uani 1 1 d . . . N3 N 0.2631(5) -0.0894(4) 0.2515(4) 0.0352(17) Uani 1 1 d . . . N4 N 0.2692(5) -0.0873(4) 0.1263(3) 0.0382(18) Uani 1 1 d . . . N5 N 0.1058(5) -0.0476(3) 0.0870(3) 0.0315(16) Uani 1 1 d . . . N6 N -0.0406(5) -0.0864(3) 0.0491(3) 0.0310(16) Uani 1 1 d . . . N7 N 0.1029(5) -0.0435(3) 0.2137(3) 0.0291(15) Uani 1 1 d . . . N8 N -0.0427(5) -0.0858(4) 0.1759(3) 0.0319(16) Uani 1 1 d . . . N9 N -0.1336(5) -0.1949(3) 0.0278(3) 0.0296(15) Uani 1 1 d . . . N10 N -0.1373(5) -0.1936(3) 0.1534(3) 0.0305(16) Uani 1 1 d . . . N11 N -0.1319(5) -0.3095(4) 0.1546(3) 0.0309(16) Uani 1 1 d . . . N12 N -0.1344(5) -0.3112(3) 0.0282(3) 0.0295(15) Uani 1 1 d . . . N13 N -0.0361(5) -0.4161(3) 0.0541(3) 0.0327(16) Uani 1 1 d . . . N14 N 0.1118(5) -0.4562(3) 0.0908(3) 0.0287(15) Uani 1 1 d . . . N15 N -0.0338(5) -0.4152(3) 0.1824(3) 0.0298(15) Uani 1 1 d . . . N16 N 0.1139(4) -0.4512(3) 0.2181(3) 0.0281(15) Uani 1 1 d . . . N17 N 0.2690(5) -0.4079(3) 0.1320(3) 0.0294(15) Uani 1 1 d . . . N18 N 0.2750(5) -0.4099(4) 0.2596(3) 0.0319(16) Uani 1 1 d . . . N19 N 0.3577(4) -0.3115(4) 0.2800(4) 0.0326(16) Uani 1 1 d . . . N20 N 0.3547(5) -0.3109(3) 0.1514(4) 0.0318(16) Uani 1 1 d . . . C1 C 0.0458(6) -0.4198(4) 0.0364(4) 0.033(2) Uani 1 1 d . . . C2 C -0.0280(6) -0.4545(4) 0.1204(4) 0.034(2) Uani 1 1 d . . . H2 H -0.0732 -0.4938 0.1098 0.041 Uiso 1 1 calc R . . C3 C 0.0753(5) -0.4834(4) 0.1460(4) 0.0255(17) Uani 1 1 d . . . H3 H 0.0773 -0.5351 0.1483 0.031 Uiso 1 1 calc R . . C4 C 0.0482(5) -0.4172(4) 0.2395(4) 0.0259(17) Uani 1 1 d . . . C5 C 0.2089(6) -0.4626(5) 0.0930(4) 0.036(2) Uani 1 1 d . . . H5A H 0.2336 -0.5074 0.1153 0.043 Uiso 1 1 calc R . . H5B H 0.2106 -0.4632 0.0433 0.043 Uiso 1 1 calc R . . C6 C 0.2112(6) -0.4614(4) 0.2673(4) 0.0317(19) Uani 1 1 d . . . H6A H 0.2110 -0.4609 0.3174 0.038 Uiso 1 1 calc R . . H6B H 0.2333 -0.5074 0.2581 0.038 Uiso 1 1 calc R . . C7 C 0.2917(6) -0.3501(5) 0.0992(5) 0.036(2) Uani 1 1 d . . . C8 C 0.3254(5) -0.4157(4) 0.2081(4) 0.0246(17) Uani 1 1 d . . . H8 H 0.3657 -0.4578 0.2166 0.030 Uiso 1 1 calc R . . C9 C 0.3856(5) -0.3448(4) 0.2227(4) 0.0321(19) Uani 1 1 d . . . H9 H 0.4537 -0.3547 0.2389 0.038 Uiso 1 1 calc R . . C10 C -0.1117(6) -0.2526(5) -0.0039(4) 0.035(2) Uani 1 1 d . . . C11 C 0.3968(6) -0.2465(4) 0.3139(4) 0.035(2) Uani 1 1 d . . . H11A H 0.4635 -0.2455 0.3191 0.042 Uiso 1 1 calc R . . H11B H 0.3916 -0.2453 0.3626 0.042 Uiso 1 1 calc R . . C12 C 0.3973(6) -0.2475(4) 0.1335(5) 0.039(2) Uani 1 1 d . . . H12A H 0.4643 -0.2473 0.1613 0.046 Uiso 1 1 calc R . . H12B H 0.3913 -0.2486 0.0821 0.046 Uiso 1 1 calc R . . C13 C 0.2937(6) -0.1457(4) 0.0955(4) 0.0305(19) Uani 1 1 d . . . C14 C 0.2868(5) -0.1478(4) 0.2952(4) 0.0292(18) Uani 1 1 d . . . C15 C 0.3830(5) -0.1507(4) 0.2196(4) 0.0254(17) Uani 1 1 d . . . H15 H 0.4507 -0.1395 0.2374 0.031 Uiso 1 1 calc R . . C16 C 0.3197(5) -0.0817(4) 0.2041(4) 0.0287(18) Uani 1 1 d . . . H16 H 0.3585 -0.0390 0.2156 0.034 Uiso 1 1 calc R . . C17 C 0.2016(6) -0.0370(4) 0.0854(4) 0.0290(18) Uani 1 1 d . . . H17A H 0.2002 -0.0384 0.0350 0.035 Uiso 1 1 calc R . . H17B H 0.2225 0.0097 0.1042 0.035 Uiso 1 1 calc R . . C18 C 0.2009(5) -0.0349(4) 0.2603(4) 0.0298(18) Uani 1 1 d . . . H18A H 0.2240 0.0103 0.2497 0.036 Uiso 1 1 calc R . . H18B H 0.2030 -0.0341 0.3110 0.036 Uiso 1 1 calc R . . C19 C 0.0405(6) -0.0848(4) 0.0338(4) 0.0284(18) Uani 1 1 d . . . C20 C 0.0668(6) -0.0180(4) 0.1400(4) 0.0305(19) Uani 1 1 d . . . H20 H 0.0677 0.0337 0.1388 0.037 Uiso 1 1 calc R . . C21 C 0.0387(6) -0.0807(4) 0.2344(4) 0.0314(19) Uani 1 1 d . . . C22 C -0.0371(6) -0.0465(4) 0.1135(4) 0.0273(18) Uani 1 1 d . . . H22 H -0.0829 -0.0077 0.1015 0.033 Uiso 1 1 calc R . . C23 C -0.1245(6) -0.1240(5) 0.0034(5) 0.040(2) Uani 1 1 d . . . H23A H -0.1803 -0.0973 0.0024 0.048 Uiso 1 1 calc R . . H23B H -0.1225 -0.1261 -0.0461 0.048 Uiso 1 1 calc R . . C24 C -0.1267(6) -0.1219(5) 0.1808(5) 0.037(2) Uani 1 1 d . . . H24A H -0.1242 -0.1226 0.2316 0.044 Uiso 1 1 calc R . . H24B H -0.1822 -0.0951 0.1536 0.044 Uiso 1 1 calc R . . C25 C 0.2978(5) -0.3520(4) 0.3037(4) 0.0307(19) Uani 1 1 d . . . C26 C -0.1112(6) -0.2509(4) 0.1977(5) 0.034(2) Uani 1 1 d . . . C27 C -0.1839(5) -0.2099(4) 0.0786(4) 0.0301(18) Uani 1 1 d . . . H27 H -0.2486 -0.1914 0.0614 0.036 Uiso 1 1 calc R . . C28 C -0.1822(5) -0.2943(4) 0.0797(4) 0.0310(19) Uani 1 1 d . . . H28 H -0.2463 -0.3140 0.0647 0.037 Uiso 1 1 calc R . . C29 C -0.1180(6) -0.3812(4) 0.1849(4) 0.0302(19) Uani 1 1 d . . . H29A H -0.1166 -0.3792 0.2353 0.036 Uiso 1 1 calc R . . H29B H -0.1719 -0.4098 0.1581 0.036 Uiso 1 1 calc R . . C30 C -0.1210(5) -0.3826(4) 0.0078(4) 0.0255(17) Uani 1 1 d . . . H30A H -0.1751 -0.4106 0.0085 0.031 Uiso 1 1 calc R . . H30B H -0.1196 -0.3824 -0.0420 0.031 Uiso 1 1 calc R . . O1W O 0.3447(5) -0.5046(4) 0.4631(4) 0.0324(17) Uiso 0.75 1 d P . . O2W O 0.5033(8) -0.4919(6) 0.3677(7) 0.132(4) Uiso 1 1 d . . . O3W O -0.2074(8) -0.1455(6) 0.3240(6) 0.117(3) Uiso 1 1 d . . . O4W O -0.2065(8) -0.1483(6) -0.1777(6) 0.127(4) Uiso 1 1 d . . . O5W O 0.4683(8) -0.3195(6) -0.0043(6) 0.116(3) Uiso 1 1 d . . . O6W O 0.4599(11) -0.1736(9) -0.0123(9) 0.077(5) Uiso 0.50 1 d P . . O7W O 0.2807(13) -0.5061(9) 0.4473(10) 0.016(4) Uiso 0.25 1 d P . . O8W O 0.6545(12) -0.1597(9) 0.3960(10) 0.089(5) Uiso 0.50 1 d P . . O9W O 0.3413(16) 0.1686(12) 0.3207(13) 0.131(8) Uiso 0.50 1 d P . . O10W O 0.661(2) -0.3030(18) 0.3961(18) 0.196(13) Uiso 0.50 1 d P . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0447(11) 0.193(3) 0.0343(10) -0.0115(14) 0.0193(9) -0.0391(14) V2 0.0361(9) 0.0527(11) 0.0410(10) -0.0014(8) 0.0166(7) -0.0066(8) Na1 0.054(2) 0.093(3) 0.036(2) 0.000(2) 0.0198(19) -0.008(2) Na2 0.0443(19) 0.059(2) 0.0310(18) 0.0022(17) 0.0211(16) 0.0047(18) O1 0.048(4) 0.054(4) 0.041(4) -0.017(3) 0.033(3) -0.006(3) O2 0.053(4) 0.045(4) 0.035(3) 0.007(3) 0.027(3) 0.007(3) O3 0.052(4) 0.038(4) 0.031(3) 0.002(3) 0.015(3) 0.000(3) O4 0.047(3) 0.046(4) 0.024(3) -0.008(3) 0.019(3) 0.007(3) O5 0.051(4) 0.062(5) 0.019(3) -0.001(3) 0.005(3) 0.005(3) O6 0.062(4) 0.050(4) 0.023(3) -0.009(3) 0.009(3) -0.008(3) O7 0.066(4) 0.033(4) 0.029(3) 0.004(3) 0.007(3) -0.012(3) O8 0.053(4) 0.034(3) 0.023(3) 0.005(2) 0.021(3) 0.006(3) O9 0.064(4) 0.039(4) 0.031(3) 0.006(3) 0.031(3) 0.008(3) O10 0.053(4) 0.050(4) 0.026(3) -0.013(3) 0.018(3) -0.010(3) O11 0.072(5) 0.065(5) 0.051(4) 0.002(3) 0.029(4) -0.013(4) O12 0.033(3) 0.076(5) 0.040(4) -0.001(3) 0.013(3) -0.016(3) O13 0.055(4) 0.116(7) 0.072(5) -0.019(5) 0.036(4) -0.029(4) O14 0.075(6) 0.072(6) 0.171(10) -0.011(6) 0.026(6) -0.023(5) O15 0.057(5) 0.137(8) 0.052(5) 0.016(5) 0.013(4) -0.020(5) O16 0.098(8) 0.46(3) 0.062(7) 0.129(11) -0.008(6) -0.061(12) O17 0.098(8) 0.41(2) 0.113(9) -0.160(12) 0.077(7) -0.098(11) N1 0.032(4) 0.037(4) 0.020(3) 0.000(3) 0.008(3) -0.001(3) N2 0.040(4) 0.032(4) 0.024(3) 0.003(3) 0.017(3) -0.001(3) N3 0.044(4) 0.041(4) 0.028(4) 0.006(3) 0.022(3) 0.004(3) N4 0.053(4) 0.045(5) 0.013(3) 0.002(3) 0.006(3) 0.005(4) N5 0.048(4) 0.031(4) 0.018(3) -0.006(3) 0.014(3) -0.007(3) N6 0.041(4) 0.029(4) 0.022(3) -0.008(3) 0.010(3) 0.000(3) N7 0.041(4) 0.033(4) 0.018(3) 0.002(3) 0.015(3) 0.001(3) N8 0.043(4) 0.035(4) 0.017(3) 0.003(3) 0.009(3) 0.000(3) N9 0.045(4) 0.029(4) 0.022(3) 0.000(3) 0.021(3) -0.004(3) N10 0.051(4) 0.023(4) 0.021(3) -0.009(3) 0.017(3) -0.003(3) N11 0.038(4) 0.035(4) 0.020(3) 0.001(3) 0.010(3) 0.005(3) N12 0.039(4) 0.032(4) 0.022(3) -0.004(3) 0.016(3) -0.001(3) N13 0.052(4) 0.030(4) 0.022(3) 0.005(3) 0.021(3) -0.003(3) N14 0.038(4) 0.032(4) 0.022(3) 0.009(3) 0.017(3) 0.003(3) N15 0.042(4) 0.025(4) 0.027(4) 0.001(3) 0.017(3) 0.002(3) N16 0.036(4) 0.028(4) 0.024(3) -0.005(3) 0.015(3) -0.001(3) N17 0.044(4) 0.025(4) 0.024(3) 0.000(3) 0.018(3) -0.007(3) N18 0.036(4) 0.042(4) 0.023(3) 0.000(3) 0.016(3) -0.008(3) N19 0.031(4) 0.041(4) 0.030(4) -0.015(3) 0.016(3) -0.008(3) N20 0.037(4) 0.028(4) 0.030(4) 0.001(3) 0.011(3) -0.009(3) C1 0.046(5) 0.029(5) 0.029(4) -0.008(4) 0.018(4) -0.002(4) C2 0.055(5) 0.023(4) 0.027(4) 0.001(4) 0.016(4) -0.012(4) C3 0.032(4) 0.022(4) 0.024(4) 0.002(3) 0.012(3) 0.004(3) C4 0.029(4) 0.018(4) 0.029(4) 0.002(3) 0.006(4) 0.000(3) C5 0.043(5) 0.041(5) 0.027(4) 0.004(4) 0.018(4) 0.010(4) C6 0.045(5) 0.033(5) 0.023(4) 0.010(4) 0.020(4) 0.002(4) C7 0.040(5) 0.039(5) 0.032(5) -0.001(4) 0.013(4) 0.004(4) C8 0.029(4) 0.029(4) 0.022(4) -0.002(3) 0.018(3) -0.003(3) C9 0.024(4) 0.034(5) 0.037(5) 0.005(4) 0.007(4) 0.006(4) C10 0.037(5) 0.051(6) 0.017(4) 0.003(4) 0.008(4) -0.006(4) C11 0.036(5) 0.048(6) 0.018(4) -0.002(4) 0.003(4) 0.001(4) C12 0.037(5) 0.046(6) 0.042(5) -0.009(4) 0.026(4) 0.000(4) C13 0.040(5) 0.034(5) 0.021(4) -0.002(4) 0.015(4) -0.013(4) C14 0.035(4) 0.033(5) 0.022(4) 0.002(4) 0.013(4) 0.000(4) C15 0.025(4) 0.024(4) 0.026(4) -0.002(3) 0.007(3) -0.006(3) C16 0.036(4) 0.019(4) 0.027(4) -0.005(3) 0.004(4) -0.005(4) C17 0.049(5) 0.026(4) 0.015(4) 0.011(3) 0.015(4) -0.006(4) C18 0.034(4) 0.025(4) 0.027(4) 0.005(3) 0.004(4) 0.004(4) C19 0.042(5) 0.021(4) 0.022(4) 0.000(3) 0.011(4) 0.001(4) C20 0.047(5) 0.022(4) 0.020(4) 0.003(3) 0.009(4) 0.010(4) C21 0.045(5) 0.035(5) 0.017(4) -0.003(4) 0.014(4) 0.013(4) C22 0.044(5) 0.017(4) 0.020(4) 0.004(3) 0.009(4) 0.006(4) C23 0.049(5) 0.045(6) 0.026(4) 0.007(4) 0.011(4) 0.012(4) C24 0.034(4) 0.052(6) 0.032(5) -0.001(4) 0.022(4) 0.006(4) C25 0.026(4) 0.035(5) 0.033(5) 0.009(4) 0.013(4) 0.008(4) C26 0.038(5) 0.045(5) 0.027(4) -0.011(4) 0.020(4) -0.008(4) C27 0.027(4) 0.033(5) 0.030(4) 0.006(4) 0.010(4) 0.007(4) C28 0.023(4) 0.040(5) 0.034(5) -0.001(4) 0.014(4) -0.002(4) C29 0.038(4) 0.037(5) 0.023(4) 0.008(4) 0.020(4) -0.002(4) C30 0.030(4) 0.030(5) 0.017(4) -0.005(3) 0.007(3) 0.001(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O17 1.557(12) . ? V1 O16 1.602(13) . ? V1 O13 1.770(7) . ? V1 O15 1.793(8) . ? V2 O14 1.626(9) . ? V2 O12 1.632(6) . ? V2 O13 1.768(7) . ? V2 O15 1.782(8) 3_656 ? Na1 O11 2.281(8) . ? Na1 O6 2.316(7) 4_556 ? Na1 O1 2.334(6) . ? Na1 O4 2.369(7) . ? Na1 O10 2.435(7) 4_556 ? Na1 Na2 3.924(6) . ? Na2 O2 2.320(6) . ? Na2 O7 2.332(7) 4_556 ? Na2 O11 2.340(7) . ? Na2 O8 2.388(6) 4_556 ? Na2 O3 2.465(7) . ? Na2 O12 2.534(7) . ? O1 C25 1.217(9) . ? O2 C14 1.223(9) . ? O3 C21 1.241(9) . ? O4 C4 1.232(9) . ? O5 C26 1.232(10) . ? O6 C13 1.226(9) . ? O6 Na1 2.316(7) 4 ? O7 C7 1.230(10) . ? O7 Na2 2.332(7) 4 ? O8 C1 1.236(9) . ? O8 Na2 2.388(6) 4 ? O9 C10 1.228(10) . ? O10 C19 1.242(9) . ? O10 Na1 2.435(7) 4 ? O15 V2 1.782(8) 3_656 ? N1 C13 1.342(10) . ? N1 C12 1.437(10) . ? N1 C15 1.442(9) . ? N2 C14 1.360(10) . ? N2 C11 1.437(10) . ? N2 C15 1.443(9) . ? N3 C14 1.369(10) . ? N3 C18 1.435(10) . ? N3 C16 1.442(10) . ? N4 C13 1.362(10) . ? N4 C17 1.428(10) . ? N4 C16 1.453(10) . ? N5 C19 1.362(10) . ? N5 C20 1.446(10) . ? N5 C17 1.456(10) . ? N6 C19 1.337(10) . ? N6 C22 1.445(9) . ? N6 C23 1.464(10) . ? N7 C21 1.352(10) . ? N7 C20 1.434(9) . ? N7 C18 1.460(10) . ? N8 C21 1.370(10) . ? N8 C22 1.444(9) . ? N8 C24 1.459(10) . ? N9 C10 1.346(10) . ? N9 C27 1.446(9) . ? N9 C23 1.444(10) . ? N10 C26 1.359(10) . ? N10 C27 1.421(10) . ? N10 C24 1.449(10) . ? N11 C26 1.362(10) . ? N11 C28 1.428(10) . ? N11 C29 1.468(10) . ? N12 C10 1.368(10) . ? N12 C30 1.441(9) . ? N12 C28 1.439(9) . ? N13 C1 1.375(10) . ? N13 C30 1.442(10) . ? N13 C2 1.446(9) . ? N14 C1 1.372(10) . ? N14 C3 1.442(9) . ? N14 C5 1.444(10) . ? N15 C4 1.357(9) . ? N15 C29 1.428(10) . ? N15 C2 1.440(10) . ? N16 C4 1.348(9) . ? N16 C3 1.459(9) . ? N16 C6 1.470(10) . ? N17 C7 1.364(10) . ? N17 C5 1.417(10) . ? N17 C8 1.447(10) . ? N18 C25 1.363(10) . ? N18 C6 1.405(9) . ? N18 C8 1.434(9) . ? N19 C25 1.368(10) . ? N19 C11 1.428(10) . ? N19 C9 1.449(10) . ? N20 C7 1.357(10) . ? N20 C12 1.454(10) . ? N20 C9 1.455(10) . ? C2 C3 1.560(11) . ? C8 C9 1.590(11) . ? C15 C16 1.586(10) . ? C20 C22 1.565(11) . ? C27 C28 1.599(12) . ? O1W O7W 0.905(17) . ? 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 O17 V1 O16 103.0(8) . . ? O17 V1 O13 111.8(6) . . ? O16 V1 O13 109.1(5) . . ? O17 V1 O15 112.8(5) . . ? O16 V1 O15 110.5(6) . . ? O13 V1 O15 109.4(4) . . ? O14 V2 O12 109.1(4) . . ? O14 V2 O13 109.0(5) . . ? O12 V2 O13 109.7(3) . . ? O14 V2 O15 109.2(5) . 3_656 ? O12 V2 O15 109.9(3) . 3_656 ? O13 V2 O15 110.0(4) . 3_656 ? O11 Na1 O6 107.8(3) . 4_556 ? O11 Na1 O1 107.9(3) . . ? O6 Na1 O1 94.4(3) 4_556 . ? O11 Na1 O4 91.8(3) . . ? O6 Na1 O4 159.8(3) 4_556 . ? O1 Na1 O4 83.9(2) . . ? O11 Na1 O10 89.1(3) . 4_556 ? O6 Na1 O10 83.6(2) 4_556 4_556 ? O1 Na1 O10 162.5(3) . 4_556 ? O4 Na1 O10 92.0(2) . 4_556 ? O11 Na1 Na2 32.3(2) . . ? O6 Na1 Na2 86.7(2) 4_556 . ? O1 Na1 Na2 85.92(19) . . ? O4 Na1 Na2 113.3(2) . . ? O10 Na1 Na2 111.2(2) 4_556 . ? O2 Na2 O7 103.0(2) . 4_556 ? O2 Na2 O11 98.3(3) . . ? O7 Na2 O11 97.8(3) 4_556 . ? O2 Na2 O8 173.2(3) . 4_556 ? O7 Na2 O8 82.5(2) 4_556 4_556 ? O11 Na2 O8 84.7(2) . 4_556 ? O2 Na2 O3 81.6(2) . . ? O7 Na2 O3 175.2(3) 4_556 . ? O11 Na2 O3 82.8(3) . . ? O8 Na2 O3 92.8(2) 4_556 . ? O2 Na2 O12 85.6(2) . . ? O7 Na2 O12 87.0(2) 4_556 . ? O11 Na2 O12 173.0(3) . . ? O8 Na2 O12 90.8(2) 4_556 . ? O3 Na2 O12 92.0(2) . . ? O2 Na2 Na1 79.04(18) . . ? O7 Na2 Na1 78.31(18) 4_556 . ? O11 Na2 Na1 31.4(2) . . ? O8 Na2 Na1 106.20(17) 4_556 . ? O3 Na2 Na1 104.20(18) . . ? O12 Na2 Na1 155.59(19) . . ? C25 O1 Na1 151.6(6) . . ? C14 O2 Na2 150.8(6) . . ? C21 O3 Na2 147.2(6) . . ? C4 O4 Na1 151.7(5) . . ? C13 O6 Na1 152.7(6) . 4 ? C7 O7 Na2 149.4(6) . 4 ? C1 O8 Na2 148.6(6) . 4 ? C19 O10 Na1 150.7(5) . 4 ? Na1 O11 Na2 116.3(4) . . ? V2 O12 Na2 129.6(4) . . ? V2 O13 V1 133.0(5) . . ? V2 O15 V1 132.3(5) 3_656 . ? C13 N1 C12 122.1(7) . . ? C13 N1 C15 114.4(7) . . ? C12 N1 C15 123.2(7) . . ? C14 N2 C11 121.4(7) . . ? C14 N2 C15 114.8(7) . . ? C11 N2 C15 123.3(6) . . ? C14 N3 C18 123.8(6) . . ? C14 N3 C16 112.7(6) . . ? C18 N3 C16 122.6(6) . . ? C13 N4 C17 122.9(7) . . ? C13 N4 C16 112.9(7) . . ? C17 N4 C16 124.1(7) . . ? C19 N5 C20 112.4(7) . . ? C19 N5 C17 121.5(6) . . ? C20 N5 C17 125.9(6) . . ? C19 N6 C22 113.4(7) . . ? C19 N6 C23 122.6(7) . . ? C22 N6 C23 124.0(7) . . ? C21 N7 C20 113.4(7) . . ? C21 N7 C18 122.7(6) . . ? C20 N7 C18 123.7(6) . . ? C21 N8 C22 112.2(7) . . ? C21 N8 C24 122.1(7) . . ? C22 N8 C24 125.5(7) . . ? C10 N9 C27 113.9(6) . . ? C10 N9 C23 123.1(6) . . ? C27 N9 C23 122.0(7) . . ? C26 N10 C27 114.4(6) . . ? C26 N10 C24 122.9(7) . . ? C27 N10 C24 122.4(7) . . ? C26 N11 C28 113.3(7) . . ? C26 N11 C29 122.5(7) . . ? C28 N11 C29 123.4(7) . . ? C10 N12 C30 124.1(6) . . ? C10 N12 C28 112.6(6) . . ? C30 N12 C28 122.9(6) . . ? C1 N13 C30 122.9(6) . . ? C1 N13 C2 111.7(7) . . ? C30 N13 C2 125.2(7) . . ? C1 N14 C3 113.4(6) . . ? C1 N14 C5 122.1(6) . . ? C3 N14 C5 124.4(6) . . ? C4 N15 C29 123.9(7) . . ? C4 N15 C2 112.4(7) . . ? C29 N15 C2 123.6(7) . . ? C4 N16 C3 113.1(6) . . ? C4 N16 C6 122.0(6) . . ? C3 N16 C6 124.5(6) . . ? C7 N17 C5 123.4(7) . . ? C7 N17 C8 113.9(6) . . ? C5 N17 C8 121.8(6) . . ? C25 N18 C6 122.2(6) . . ? C25 N18 C8 114.5(6) . . ? C6 N18 C8 123.2(7) . . ? C25 N19 C11 123.0(7) . . ? C25 N19 C9 113.1(7) . . ? C11 N19 C9 123.5(7) . . ? C7 N20 C12 121.8(7) . . ? C7 N20 C9 113.2(7) . . ? C12 N20 C9 124.2(7) . . ? O8 C1 N14 125.9(7) . . ? O8 C1 N13 125.9(8) . . ? N14 C1 N13 108.1(7) . . ? N15 C2 N13 117.9(7) . . ? N15 C2 C3 103.8(6) . . ? N13 C2 C3 104.4(6) . . ? N14 C3 N16 115.5(6) . . ? N14 C3 C2 102.2(6) . . ? N16 C3 C2 101.6(6) . . ? O4 C4 N16 125.8(7) . . ? O4 C4 N15 125.5(7) . . ? N16 C4 N15 108.6(7) . . ? N17 C5 N14 114.3(7) . . ? N18 C6 N16 113.8(6) . . ? O7 C7 N20 125.0(8) . . ? O7 C7 N17 126.8(8) . . ? N20 C7 N17 108.1(7) . . ? N18 C8 N17 115.8(6) . . ? N18 C8 C9 101.9(6) . . ? N17 C8 C9 101.8(6) . . ? N19 C9 N20 116.7(7) . . ? N19 C9 C8 102.6(6) . . ? N20 C9 C8 102.6(6) . . ? O9 C10 N9 127.0(8) . . ? O9 C10 N12 124.2(8) . . ? N9 C10 N12 108.8(7) . . ? N19 C11 N2 114.8(7) . . ? N1 C12 N20 113.4(7) . . ? O6 C13 N1 126.5(8) . . ? O6 C13 N4 125.1(8) . . ? N1 C13 N4 108.3(7) . . ? O2 C14 N2 126.2(8) . . ? O2 C14 N3 126.2(7) . . ? N2 C14 N3 107.6(6) . . ? N1 C15 N2 117.4(6) . . ? N1 C15 C16 101.9(6) . . ? N2 C15 C16 101.1(6) . . ? N3 C16 N4 116.0(7) . . ? N3 C16 C15 103.6(6) . . ? N4 C16 C15 102.3(6) . . ? N4 C17 N5 114.9(6) . . ? N3 C18 N7 113.9(6) . . ? O10 C19 N6 125.8(7) . . ? O10 C19 N5 125.1(7) . . ? N6 C19 N5 108.9(7) . . ? N7 C20 N5 117.8(6) . . ? N7 C20 C22 102.8(6) . . ? N5 C20 C22 102.6(6) . . ? O3 C21 N7 126.4(8) . . ? O3 C21 N8 125.1(8) . . ? N7 C21 N8 108.5(6) . . ? N6 C22 N8 117.2(6) . . ? N6 C22 C20 102.6(6) . . ? N8 C22 C20 103.0(6) . . ? N9 C23 N6 114.2(7) . . ? N10 C24 N8 114.2(6) . . ? O1 C25 N18 126.6(7) . . ? O1 C25 N19 125.9(8) . . ? N18 C25 N19 107.5(7) . . ? O5 C26 N10 126.0(7) . . ? O5 C26 N11 126.2(8) . . ? N10 C26 N11 107.7(7) . . ? N10 C27 N9 117.2(7) . . ? N10 C27 C28 101.7(6) . . ? N9 C27 C28 101.4(6) . . ? N11 C28 N12 116.2(6) . . ? N11 C28 C27 102.5(6) . . ? N12 C28 C27 102.9(6) . . ? N15 C29 N11 114.6(6) . . ? N13 C30 N12 114.5(6) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.722 _refine_diff_density_min -1.007 _refine_diff_density_rms 0.184