# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2007 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Yi-Chou Tsai' _publ_contact_author_address ; Department of Chemistry National Tsing Hua University 101 Sec 2. Guang Fu Road Hsinchu 30013 TAIWAN ; _publ_contact_author_email yictsai@mx.nthu.edu.tw _publ_section_title ;Synthesis and Reactions of beta-Diketiminato Divanadium(I) Inverted-Sandwich Complexes ; loop_ _publ_author_name 'Yi-Chou Tsai.' 'Po-Yang Wang.' 'Shin-An Chen.' 'Jin-Ming Chen.' # Attachment 'Complex 1.cif' data_complex_1 _database_code_depnum_ccdc_archive 'CCDC 645658' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C65 H90 N4 V2' _chemical_formula_sum 'C65 H90 N4 V2' _chemical_formula_weight 1029.29 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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.6990(5) _cell_length_b 15.3858(5) _cell_length_c 24.9682(7) _cell_angle_alpha 90.00 _cell_angle_beta 107.898(2) _cell_angle_gamma 90.00 _cell_volume 6470.1(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 22227 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.35 _exptl_crystal_description prism _exptl_crystal_colour red(dark) _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.057 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2216 _exptl_absorpt_coefficient_mu 0.327 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8913 _exptl_absorpt_correction_T_max 1.0304 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 33240 _diffrn_reflns_av_R_equivalents 0.1142 _diffrn_reflns_av_sigmaI/netI 0.1555 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 2.14 _diffrn_reflns_theta_max 25.36 _reflns_number_total 11655 _reflns_number_gt 5859 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 19' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1276P)^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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0149(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11655 _refine_ls_number_parameters 643 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1746 _refine_ls_R_factor_gt 0.0974 _refine_ls_wR_factor_ref 0.2533 _refine_ls_wR_factor_gt 0.2198 _refine_ls_goodness_of_fit_ref 0.986 _refine_ls_restrained_S_all 0.986 _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 0.12956(5) 0.24388(6) 0.37152(3) 0.0354(3) Uani 1 1 d . . . V2 V 0.04933(5) 0.13388(6) 0.24343(3) 0.0356(3) Uani 1 1 d . . . N1 N 0.2358(2) 0.2548(3) 0.43523(16) 0.0355(10) Uani 1 1 d . . . N2 N 0.0832(3) 0.3358(3) 0.41393(17) 0.0423(11) Uani 1 1 d . . . N3 N -0.0496(2) 0.0582(3) 0.20932(16) 0.0405(11) Uani 1 1 d . . . N4 N 0.0759(2) 0.1233(3) 0.16862(16) 0.0346(10) Uani 1 1 d . . . C1 C 0.2927(3) 0.1867(3) 0.4385(2) 0.0376(13) Uani 1 1 d . . . C2 C 0.3472(3) 0.1926(4) 0.4081(2) 0.0415(14) Uani 1 1 d . . . C3 C 0.3531(4) 0.2737(4) 0.3755(2) 0.0561(16) Uani 1 1 d . . . H3 H 0.3015 0.3028 0.3658 0.067 Uiso 1 1 calc R . . C4 C 0.4144(7) 0.3370(5) 0.4098(3) 0.119(4) Uani 1 1 d . . . H4A H 0.4151 0.3879 0.3877 0.178 Uiso 1 1 calc R . . H4B H 0.4658 0.3102 0.4205 0.178 Uiso 1 1 calc R . . H4C H 0.4011 0.3533 0.4430 0.178 Uiso 1 1 calc R . . C5 C 0.3722(5) 0.2589(6) 0.3212(3) 0.091(3) Uani 1 1 d . . . H5A H 0.3736 0.3138 0.3032 0.136 Uiso 1 1 calc R . . H5B H 0.3322 0.2226 0.2967 0.136 Uiso 1 1 calc R . . H5C H 0.4230 0.2310 0.3292 0.136 Uiso 1 1 calc R . . C6 C 0.3997(3) 0.1243(4) 0.4112(2) 0.0512(16) Uani 1 1 d . . . H6 H 0.4358 0.1265 0.3909 0.061 Uiso 1 1 calc R . . C7 C 0.3983(4) 0.0532(4) 0.4445(3) 0.0604(19) Uani 1 1 d . . . H7 H 0.4334 0.0075 0.4460 0.072 Uiso 1 1 calc R . . C8 C 0.3470(4) 0.0484(4) 0.4750(2) 0.0544(16) Uani 1 1 d . . . H8 H 0.3479 -0.0002 0.4973 0.065 Uiso 1 1 calc R . . C9 C 0.2930(3) 0.1149(4) 0.4736(2) 0.0465(15) Uani 1 1 d . . . C10 C 0.2377(4) 0.1099(4) 0.5104(2) 0.0624(18) Uani 1 1 d . . . H10 H 0.2093 0.1654 0.5069 0.075 Uiso 1 1 calc R . . C11 C 0.2847(5) 0.0969(6) 0.5724(3) 0.099(3) Uani 1 1 d . . . H11A H 0.2487 0.0940 0.5943 0.149 Uiso 1 1 calc R . . H11B H 0.3205 0.1449 0.5851 0.149 Uiso 1 1 calc R . . H11C H 0.3145 0.0438 0.5767 0.149 Uiso 1 1 calc R . . C12 C 0.1761(5) 0.0379(5) 0.4909(3) 0.082(2) Uani 1 1 d . . . H12A H 0.1426 0.0368 0.5147 0.122 Uiso 1 1 calc R . . H12B H 0.2026 -0.0170 0.4930 0.122 Uiso 1 1 calc R . . H12C H 0.1444 0.0487 0.4527 0.122 Uiso 1 1 calc R . . C13 C 0.3363(4) 0.3147(5) 0.5203(3) 0.068(2) Uani 1 1 d . . . H13A H 0.3683 0.2696 0.5117 0.102 Uiso 1 1 calc R . . H13B H 0.3309 0.3045 0.5569 0.102 Uiso 1 1 calc R . . H13C H 0.3613 0.3700 0.5200 0.102 Uiso 1 1 calc R . . C14 C 0.2549(3) 0.3146(4) 0.4766(2) 0.0470(15) Uani 1 1 d . . . C15 C 0.2025(4) 0.3768(4) 0.4846(2) 0.0547(16) Uani 1 1 d . . . H15 H 0.2247 0.4197 0.5110 0.066 Uiso 1 1 calc R . . C16 C 0.1219(4) 0.3830(4) 0.4585(2) 0.0496(15) Uani 1 1 d . . . C17 C 0.0794(4) 0.4455(5) 0.4864(3) 0.076(2) Uani 1 1 d . . . H17A H 0.0237 0.4454 0.4663 0.114 Uiso 1 1 calc R . . H17B H 0.1004 0.5030 0.4861 0.114 Uiso 1 1 calc R . . H17C H 0.0873 0.4276 0.5246 0.114 Uiso 1 1 calc R . . C18 C -0.0032(3) 0.3432(4) 0.3954(2) 0.0485(15) Uani 1 1 d . . . C19 C -0.0465(4) 0.2801(4) 0.4144(2) 0.0574(17) Uani 1 1 d . . . C20 C -0.0052(4) 0.2034(5) 0.4528(3) 0.0688(19) Uani 1 1 d . . . H20 H 0.0439 0.1911 0.4437 0.083 Uiso 1 1 calc R . . C21 C 0.0194(6) 0.2293(6) 0.5147(3) 0.114(3) Uani 1 1 d . . . H21A H 0.0516 0.2807 0.5203 0.171 Uiso 1 1 calc R . . H21B H 0.0491 0.1828 0.5372 0.171 Uiso 1 1 calc R . . H21C H -0.0272 0.2406 0.5256 0.171 Uiso 1 1 calc R . . C22 C -0.0532(5) 0.1207(5) 0.4421(4) 0.093(3) Uani 1 1 d . . . H22A H -0.0241 0.0758 0.4665 0.139 Uiso 1 1 calc R . . H22B H -0.0633 0.1033 0.4036 0.139 Uiso 1 1 calc R . . H22C H -0.1027 0.1304 0.4494 0.139 Uiso 1 1 calc R . . C23 C -0.1279(4) 0.2859(5) 0.3977(3) 0.075(2) Uani 1 1 d . . . H23 H -0.1569 0.2442 0.4099 0.091 Uiso 1 1 calc R . . C24 C -0.1674(4) 0.3520(5) 0.3633(3) 0.082(2) Uani 1 1 d . . . H24 H -0.2224 0.3555 0.3528 0.098 Uiso 1 1 calc R . . C25 C -0.1241(4) 0.4131(5) 0.3445(3) 0.0682(19) Uani 1 1 d . . . H25 H -0.1511 0.4571 0.3207 0.082 Uiso 1 1 calc R . . C26 C -0.0409(3) 0.4109(4) 0.3603(2) 0.0533(16) Uani 1 1 d . B . C27 C 0.0018(4) 0.4795(5) 0.3380(3) 0.075(2) Uani 1 1 d . . . H27 H 0.0577 0.4641 0.3558 0.090 Uiso 1 1 calc R A 1 C28 C -0.0036(8) 0.5702(6) 0.3624(4) 0.143(4) Uani 1 1 d . B . H28A H 0.0253 0.6111 0.3473 0.215 Uiso 1 1 calc R . . H28B H 0.0188 0.5684 0.4027 0.215 Uiso 1 1 calc R . . H28C H -0.0582 0.5876 0.3527 0.215 Uiso 1 1 calc R . . C29A C 0.000(2) 0.4967(14) 0.2874(10) 0.057(8) Uiso 0.34(3) 1 d P B 1 H29A H 0.0349 0.5444 0.2876 0.085 Uiso 0.34(3) 1 calc PR B 1 H29B H -0.0533 0.5121 0.2657 0.085 Uiso 0.34(3) 1 calc PR B 1 H29C H 0.0165 0.4466 0.2711 0.085 Uiso 0.34(3) 1 calc PR B 1 C29 C -0.0406(11) 0.4856(8) 0.2701(5) 0.066(4) Uiso 0.66(3) 1 d P B 2 H29D H -0.0144 0.5292 0.2546 0.100 Uiso 0.66(3) 1 calc PR B 2 H29E H -0.0955 0.5009 0.2625 0.100 Uiso 0.66(3) 1 calc PR B 2 H29F H -0.0368 0.4304 0.2532 0.100 Uiso 0.66(3) 1 calc PR B 2 C30 C -0.1043(3) 0.0468(4) 0.2414(2) 0.0437(14) Uani 1 1 d . . . C31 C -0.1694(4) 0.1039(4) 0.2331(3) 0.0580(17) Uani 1 1 d . . . C32 C -0.1859(4) 0.1784(5) 0.1903(3) 0.0632(18) Uani 1 1 d . . . H32 H -0.1453 0.1766 0.1711 0.076 Uiso 1 1 calc R . . C33 C -0.2664(5) 0.1701(6) 0.1460(3) 0.094(3) Uani 1 1 d . . . H33A H -0.2736 0.2174 0.1198 0.141 Uiso 1 1 calc R . . H33B H -0.3073 0.1719 0.1638 0.141 Uiso 1 1 calc R . . H33C H -0.2691 0.1160 0.1264 0.141 Uiso 1 1 calc R . . C34 C -0.1817(4) 0.2672(5) 0.2182(3) 0.084(2) Uani 1 1 d . . . H34A H -0.1912 0.3118 0.1900 0.127 Uiso 1 1 calc R . . H34B H -0.1300 0.2751 0.2449 0.127 Uiso 1 1 calc R . . H34C H -0.2212 0.2706 0.2372 0.127 Uiso 1 1 calc R . . C35 C -0.2207(4) 0.0903(5) 0.2644(3) 0.0693(19) Uani 1 1 d . . . H35 H -0.2635 0.1277 0.2599 0.083 Uiso 1 1 calc R . . C36 C -0.2096(5) 0.0230(6) 0.3018(3) 0.084(2) Uani 1 1 d . . . H36 H -0.2452 0.0148 0.3221 0.101 Uiso 1 1 calc R . . C37 C -0.1472(4) -0.0319(5) 0.3096(3) 0.074(2) Uani 1 1 d . . . H37 H -0.1412 -0.0776 0.3350 0.089 Uiso 1 1 calc R . . C38 C -0.0925(4) -0.0221(4) 0.2810(2) 0.0566(17) Uani 1 1 d . . . C39 C -0.0229(4) -0.0847(4) 0.2903(3) 0.0616(18) Uani 1 1 d . . . H39 H 0.0203 -0.0536 0.2818 0.074 Uiso 1 1 calc R . . C40 C 0.0084(5) -0.1173(5) 0.3514(3) 0.084(2) Uani 1 1 d . . . H40A H 0.0226 -0.0685 0.3765 0.125 Uiso 1 1 calc R . . H40B H 0.0543 -0.1531 0.3557 0.125 Uiso 1 1 calc R . . H40C H -0.0321 -0.1506 0.3602 0.125 Uiso 1 1 calc R . . C41 C -0.0430(6) -0.1643(5) 0.2524(3) 0.105(3) Uani 1 1 d . . . H41A H 0.0030 -0.2008 0.2595 0.158 Uiso 1 1 calc R . . H41B H -0.0597 -0.1463 0.2138 0.158 Uiso 1 1 calc R . . H41C H -0.0851 -0.1962 0.2602 0.158 Uiso 1 1 calc R . . C42 C -0.1509(4) -0.0285(5) 0.1370(3) 0.071(2) Uani 1 1 d . . . H42A H -0.1755 -0.0304 0.1663 0.107 Uiso 1 1 calc R . . H42B H -0.1402 -0.0866 0.1274 0.107 Uiso 1 1 calc R . . H42C H -0.1859 -0.0004 0.1045 0.107 Uiso 1 1 calc R . . C43 C -0.0730(3) 0.0223(4) 0.1576(2) 0.0452(14) Uani 1 1 d . . . C44 C -0.0310(3) 0.0302(4) 0.1191(2) 0.0437(14) Uani 1 1 d . . . H44 H -0.0508 -0.0015 0.0860 0.052 Uiso 1 1 calc R . . C45 C 0.0371(3) 0.0793(3) 0.12324(19) 0.0352(12) Uani 1 1 d . . . C46 C 0.0625(3) 0.0792(4) 0.0697(2) 0.0466(14) Uani 1 1 d . . . H46A H 0.1088 0.1149 0.0755 0.070 Uiso 1 1 calc R . . H46B H 0.0202 0.1018 0.0388 0.070 Uiso 1 1 calc R . . H46C H 0.0745 0.0209 0.0613 0.070 Uiso 1 1 calc R . . C47 C 0.1429(3) 0.1762(3) 0.16474(18) 0.0354(13) Uani 1 1 d . . . C48 C 0.2198(3) 0.1403(3) 0.1802(2) 0.0407(13) Uani 1 1 d . . . C49 C 0.2366(4) 0.0442(4) 0.1936(3) 0.0603(17) Uani 1 1 d . . . H49 H 0.1878 0.0173 0.1963 0.072 Uiso 1 1 calc R . . C50 C 0.3024(4) 0.0265(5) 0.2487(3) 0.079(2) Uani 1 1 d . . . H50A H 0.3085 -0.0350 0.2547 0.118 Uiso 1 1 calc R . . H50B H 0.2887 0.0527 0.2793 0.118 Uiso 1 1 calc R . . H50C H 0.3514 0.0509 0.2466 0.118 Uiso 1 1 calc R . . C51 C 0.2600(4) -0.0023(5) 0.1464(3) 0.082(2) Uani 1 1 d . . . H51A H 0.2195 0.0069 0.1111 0.122 Uiso 1 1 calc R . . H51B H 0.2656 -0.0635 0.1543 0.122 Uiso 1 1 calc R . . H51C H 0.3095 0.0206 0.1444 0.122 Uiso 1 1 calc R . . C52 C 0.2825(3) 0.1939(4) 0.1804(2) 0.0461(15) Uani 1 1 d . . . H52 H 0.3337 0.1713 0.1906 0.055 Uiso 1 1 calc R . . C53 C 0.2707(4) 0.2803(4) 0.1659(2) 0.0516(15) Uani 1 1 d . . . H53 H 0.3138 0.3158 0.1676 0.062 Uiso 1 1 calc R . . C54 C 0.1958(4) 0.3139(4) 0.1492(2) 0.0467(15) Uani 1 1 d . . . H54 H 0.1885 0.3717 0.1381 0.056 Uiso 1 1 calc R . . C55 C 0.1306(3) 0.2640(3) 0.1482(2) 0.0384(13) Uani 1 1 d . . . C56 C 0.0462(3) 0.3017(4) 0.1252(2) 0.0516(16) Uani 1 1 d . . . H56 H 0.0089 0.2592 0.1319 0.062 Uiso 1 1 calc R . . C57 C 0.0257(4) 0.3152(4) 0.0616(3) 0.073(2) Uani 1 1 d . . . H57A H 0.0318 0.2612 0.0440 0.109 Uiso 1 1 calc R . . H57B H 0.0607 0.3579 0.0541 0.109 Uiso 1 1 calc R . . H57C H -0.0282 0.3348 0.0467 0.109 Uiso 1 1 calc R . . C58 C 0.0357(4) 0.3859(4) 0.1527(2) 0.0579(17) Uani 1 1 d . . . H58A H -0.0180 0.4058 0.1369 0.087 Uiso 1 1 calc R . . H58B H 0.0715 0.4286 0.1464 0.087 Uiso 1 1 calc R . . H58C H 0.0468 0.3769 0.1925 0.087 Uiso 1 1 calc R . . C59 C 0.1836(3) 0.0244(4) 0.3456(2) 0.0486(15) Uani 1 1 d . . . H59A H 0.1538 -0.0142 0.3616 0.073 Uiso 1 1 calc R . . H59B H 0.2330 0.0385 0.3735 0.073 Uiso 1 1 calc R . . H59C H 0.1939 -0.0032 0.3141 0.073 Uiso 1 1 calc R . . C60 C 0.1367(3) 0.1064(3) 0.32634(18) 0.0347(12) Uani 1 1 d . . . C61 C 0.0626(3) 0.1223(4) 0.3374(2) 0.0417(14) Uani 1 1 d . . . H61 H 0.0464 0.0849 0.3609 0.050 Uiso 1 1 calc R . . C62 C 0.0138(3) 0.1943(4) 0.3128(2) 0.0423(14) Uani 1 1 d . . . H62 H -0.0368 0.1995 0.3163 0.051 Uiso 1 1 calc R . . C63 C 0.0424(3) 0.2579(4) 0.2831(2) 0.0420(14) Uani 1 1 d . . . H63 H 0.0089 0.3017 0.2637 0.050 Uiso 1 1 calc R . . C64 C 0.1237(3) 0.2544(3) 0.28314(19) 0.0370(12) Uani 1 1 d . . . H64 H 0.1473 0.3018 0.2715 0.044 Uiso 1 1 calc R . . C65 C 0.1674(3) 0.1756(3) 0.30165(19) 0.0364(12) Uani 1 1 d . . . H65 H 0.2175 0.1697 0.2973 0.044 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0328(5) 0.0406(6) 0.0330(5) 0.0012(4) 0.0105(4) 0.0038(4) V2 0.0323(5) 0.0410(6) 0.0329(5) 0.0009(4) 0.0091(4) -0.0041(4) N1 0.033(2) 0.040(3) 0.034(2) -0.008(2) 0.0112(18) 0.004(2) N2 0.041(3) 0.048(3) 0.043(2) -0.001(2) 0.020(2) 0.005(2) N3 0.031(2) 0.051(3) 0.038(2) 0.004(2) 0.010(2) -0.010(2) N4 0.034(2) 0.035(3) 0.035(2) 0.0023(19) 0.0125(19) 0.000(2) C1 0.033(3) 0.038(3) 0.035(3) -0.008(2) 0.002(2) 0.007(3) C2 0.032(3) 0.048(4) 0.042(3) -0.011(3) 0.007(2) 0.001(3) C3 0.041(3) 0.068(5) 0.065(4) 0.006(3) 0.024(3) 0.004(3) C4 0.188(10) 0.069(6) 0.089(6) -0.005(4) 0.026(6) -0.050(6) C5 0.079(5) 0.127(7) 0.076(5) -0.015(5) 0.038(4) -0.043(5) C6 0.037(3) 0.058(4) 0.053(3) -0.011(3) 0.005(3) 0.015(3) C7 0.046(4) 0.054(4) 0.066(4) -0.021(4) -0.006(3) 0.019(3) C8 0.053(4) 0.049(4) 0.053(3) 0.002(3) 0.004(3) 0.007(3) C9 0.043(3) 0.049(4) 0.040(3) -0.007(3) 0.001(3) 0.000(3) C10 0.070(5) 0.060(4) 0.057(4) 0.014(3) 0.020(3) 0.003(4) C11 0.114(7) 0.128(7) 0.053(4) 0.005(4) 0.021(4) -0.013(6) C12 0.089(6) 0.084(6) 0.072(5) 0.020(4) 0.024(4) -0.003(5) C13 0.054(4) 0.078(5) 0.059(4) -0.024(4) -0.002(3) 0.005(4) C14 0.047(4) 0.051(4) 0.040(3) 0.001(3) 0.008(3) 0.008(3) C15 0.060(4) 0.051(4) 0.047(3) -0.011(3) 0.007(3) 0.013(3) C16 0.060(4) 0.050(4) 0.041(3) -0.005(3) 0.019(3) 0.013(3) C17 0.079(5) 0.087(5) 0.060(4) -0.014(4) 0.019(4) 0.030(4) C18 0.044(3) 0.063(4) 0.048(3) -0.001(3) 0.027(3) 0.010(3) C19 0.048(4) 0.076(5) 0.059(4) 0.002(3) 0.033(3) 0.006(3) C20 0.064(5) 0.082(5) 0.071(4) 0.023(4) 0.036(4) 0.014(4) C21 0.164(9) 0.131(8) 0.061(5) 0.032(5) 0.055(5) 0.028(7) C22 0.079(6) 0.092(6) 0.126(7) 0.038(5) 0.058(5) 0.001(5) C23 0.058(5) 0.084(5) 0.096(5) 0.022(4) 0.041(4) 0.008(4) C24 0.046(4) 0.099(6) 0.117(6) 0.005(5) 0.048(4) 0.015(4) C25 0.048(4) 0.084(5) 0.080(4) 0.018(4) 0.031(4) 0.027(4) C26 0.042(4) 0.062(4) 0.060(4) 0.005(3) 0.021(3) 0.023(3) C27 0.056(4) 0.074(5) 0.095(5) 0.044(4) 0.022(4) 0.023(4) C28 0.220(13) 0.091(8) 0.102(7) 0.017(6) 0.024(7) -0.040(8) C30 0.036(3) 0.051(4) 0.044(3) -0.004(3) 0.012(3) -0.019(3) C31 0.037(4) 0.074(5) 0.064(4) 0.002(3) 0.017(3) -0.003(3) C32 0.041(4) 0.085(5) 0.065(4) 0.006(4) 0.019(3) 0.006(3) C33 0.084(6) 0.117(7) 0.067(5) 0.014(4) 0.003(4) -0.009(5) C34 0.062(5) 0.087(6) 0.087(5) 0.013(4) -0.003(4) 0.009(4) C35 0.041(4) 0.093(6) 0.082(5) 0.007(4) 0.031(3) -0.009(4) C36 0.062(5) 0.130(7) 0.073(5) 0.019(5) 0.040(4) -0.016(5) C37 0.058(5) 0.091(6) 0.084(5) 0.026(4) 0.036(4) -0.013(4) C38 0.048(4) 0.069(5) 0.054(3) 0.001(3) 0.018(3) -0.019(3) C39 0.065(4) 0.062(4) 0.066(4) 0.014(3) 0.032(3) -0.007(4) C40 0.095(6) 0.073(5) 0.086(5) 0.020(4) 0.033(4) 0.004(4) C41 0.135(8) 0.079(6) 0.092(6) -0.013(5) 0.018(5) 0.005(5) C42 0.063(4) 0.080(5) 0.068(4) -0.016(4) 0.017(3) -0.038(4) C43 0.043(3) 0.041(3) 0.048(3) -0.003(3) 0.009(3) -0.008(3) C44 0.050(4) 0.045(3) 0.036(3) -0.006(2) 0.013(3) -0.007(3) C45 0.042(3) 0.032(3) 0.029(3) 0.001(2) 0.007(2) 0.003(3) C46 0.044(3) 0.046(4) 0.046(3) 0.003(3) 0.009(3) -0.001(3) C47 0.039(3) 0.042(3) 0.025(2) -0.005(2) 0.011(2) -0.003(3) C48 0.043(3) 0.041(3) 0.040(3) 0.005(2) 0.016(2) 0.002(3) C49 0.045(4) 0.048(4) 0.094(5) 0.007(3) 0.031(4) 0.001(3) C50 0.089(6) 0.072(5) 0.083(5) 0.026(4) 0.037(4) 0.038(4) C51 0.071(5) 0.061(5) 0.103(5) -0.022(4) 0.013(4) 0.016(4) C52 0.035(3) 0.061(4) 0.045(3) -0.002(3) 0.016(3) -0.002(3) C53 0.040(4) 0.053(4) 0.063(4) 0.002(3) 0.019(3) -0.010(3) C54 0.057(4) 0.036(3) 0.050(3) 0.003(3) 0.020(3) -0.011(3) C55 0.046(3) 0.036(3) 0.033(3) 0.002(2) 0.012(2) 0.004(3) C56 0.047(4) 0.041(4) 0.066(4) 0.015(3) 0.016(3) -0.005(3) C57 0.075(5) 0.050(4) 0.068(4) 0.002(3) -0.015(4) -0.002(4) C58 0.056(4) 0.071(5) 0.049(3) 0.016(3) 0.020(3) 0.016(3) C59 0.046(3) 0.048(4) 0.048(3) 0.003(3) 0.009(3) 0.005(3) C60 0.032(3) 0.045(3) 0.029(3) -0.001(2) 0.011(2) 0.006(2) C61 0.041(3) 0.051(4) 0.033(3) 0.009(2) 0.011(2) -0.004(3) C62 0.032(3) 0.054(4) 0.039(3) 0.000(3) 0.009(2) -0.004(3) C63 0.040(3) 0.048(4) 0.035(3) 0.003(3) 0.007(2) 0.005(3) C64 0.041(3) 0.036(3) 0.037(3) 0.003(2) 0.016(2) -0.006(3) C65 0.027(3) 0.047(3) 0.037(3) -0.005(2) 0.012(2) 0.000(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 N1 2.064(4) . ? V1 N2 2.081(4) . ? V1 C64 2.183(5) . ? V1 C61 2.238(5) . ? V1 C62 2.254(5) . ? V1 C63 2.281(5) . ? V1 C65 2.305(5) . ? V1 C60 2.419(5) . ? V2 N3 2.057(4) . ? V2 N4 2.068(4) . ? V2 C63 2.170(5) . ? V2 C60 2.211(4) . ? V2 C62 2.220(5) . ? V2 C65 2.242(5) . ? V2 C61 2.291(5) . ? V2 C64 2.313(5) . ? N1 C14 1.348(7) . ? N1 C1 1.437(6) . ? N2 C16 1.330(7) . ? N2 C18 1.459(7) . ? N3 C43 1.348(6) . ? N3 C30 1.445(7) . ? N4 C45 1.318(6) . ? N4 C47 1.466(6) . ? C1 C2 1.401(7) . ? C1 C9 1.410(8) . ? C2 C6 1.390(8) . ? C2 C3 1.510(8) . ? C3 C5 1.513(9) . ? C3 C4 1.513(10) . ? C3 H3 0.9800 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.377(9) . ? C6 H6 0.9300 . ? C7 C8 1.356(9) . ? C7 H7 0.9300 . ? C8 C9 1.394(8) . ? C8 H8 0.9300 . ? C9 C10 1.534(9) . ? C10 C12 1.525(9) . ? C10 C11 1.529(9) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.517(8) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 C15 1.388(8) . ? C15 C16 1.378(8) . ? C15 H15 0.9300 . ? C16 C17 1.516(8) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C26 1.392(8) . ? C18 C19 1.407(8) . ? C19 C23 1.375(9) . ? C19 C20 1.553(9) . ? C20 C22 1.508(10) . ? C20 C21 1.525(10) . ? C20 H20 0.9800 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.374(10) . ? C23 H23 0.9300 . ? C24 C25 1.382(10) . ? C24 H24 0.9300 . ? C25 C26 1.403(8) . ? C25 H25 0.9300 . ? C26 C27 1.503(9) . ? C27 C29A 1.28(2) . ? C27 C28 1.538(12) . ? C27 C29 1.632(16) . ? C27 H27 0.9800 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29A H29A 0.9600 . ? C29A H29B 0.9600 . ? C29A H29C 0.9600 . ? C29 H29D 0.9600 . ? C29 H29E 0.9600 . ? C29 H29F 0.9600 . ? C30 C31 1.411(8) . ? C30 C38 1.419(8) . ? C31 C35 1.385(8) . ? C31 C32 1.533(9) . ? C32 C33 1.515(9) . ? C32 C34 1.526(10) . ? C32 H32 0.9800 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.367(10) . ? C35 H35 0.9300 . ? C36 C37 1.357(10) . ? C36 H36 0.9300 . ? C37 C38 1.378(9) . ? C37 H37 0.9300 . ? C38 C39 1.524(9) . ? C39 C41 1.521(10) . ? C39 C40 1.539(9) . ? C39 H39 0.9800 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 C43 1.530(8) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 C44 1.390(7) . ? C44 C45 1.397(7) . ? C44 H44 0.9300 . ? C45 C46 1.537(7) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 C48 1.409(7) . ? C47 C55 1.409(7) . ? C48 C52 1.381(7) . ? C48 C49 1.526(8) . ? C49 C50 1.528(9) . ? C49 C51 1.540(9) . ? C49 H49 0.9800 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 C53 1.376(8) . ? C52 H52 0.9300 . ? C53 C54 1.362(8) . ? C53 H53 0.9300 . ? C54 C55 1.381(7) . ? C54 H54 0.9300 . ? C55 C56 1.540(8) . ? C56 C58 1.504(8) . ? C56 C57 1.531(8) . ? C56 H56 0.9800 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 C60 1.505(7) . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 C65 1.419(7) . ? C60 C61 1.442(7) . ? C61 C62 1.423(7) . ? C61 H61 0.9300 . ? C62 C63 1.410(7) . ? C62 H62 0.9300 . ? C63 C64 1.440(7) . ? C63 H63 0.9300 . ? C64 C65 1.435(7) . ? C64 H64 0.9300 . ? C65 H65 0.9300 . ? 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 N1 V1 N2 87.78(17) . . ? N1 V1 C64 121.46(18) . . ? N2 V1 C64 124.11(18) . . ? N1 V1 C61 127.76(18) . . ? N2 V1 C61 121.1(2) . . ? C64 V1 C61 79.72(19) . . ? N1 V1 C62 163.72(19) . . ? N2 V1 C62 97.98(19) . . ? C64 V1 C62 67.43(19) . . ? C61 V1 C62 36.93(19) . . ? N1 V1 C63 157.42(19) . . ? N2 V1 C63 99.96(18) . . ? C64 V1 C63 37.56(19) . . ? C61 V1 C63 65.71(19) . . ? C62 V1 C63 36.23(19) . . ? N1 V1 C65 102.27(17) . . ? N2 V1 C65 161.22(18) . . ? C64 V1 C65 37.18(18) . . ? C61 V1 C65 64.77(19) . . ? C62 V1 C65 76.76(19) . . ? C63 V1 C65 65.06(19) . . ? N1 V1 C60 105.35(16) . . ? N2 V1 C60 156.49(18) . . ? C64 V1 C60 65.56(18) . . ? C61 V1 C60 35.81(18) . . ? C62 V1 C60 64.43(19) . . ? C63 V1 C60 75.41(18) . . ? C65 V1 C60 34.86(17) . . ? N3 V2 N4 88.98(16) . . ? N3 V2 C63 121.8(2) . . ? N4 V2 C63 122.81(19) . . ? N3 V2 C60 122.76(18) . . ? N4 V2 C60 122.89(17) . . ? C63 V2 C60 82.07(18) . . ? N3 V2 C62 98.70(19) . . ? N4 V2 C62 159.21(18) . . ? C63 V2 C62 37.45(19) . . ? C60 V2 C62 68.54(19) . . ? N3 V2 C65 159.39(18) . . ? N4 V2 C65 100.54(17) . . ? C63 V2 C65 67.94(19) . . ? C60 V2 C65 37.16(18) . . ? C62 V2 C65 78.76(19) . . ? N3 V2 C61 100.74(18) . . ? N4 V2 C61 159.80(18) . . ? C63 V2 C61 66.6(2) . . ? C60 V2 C61 37.31(18) . . ? C62 V2 C61 36.73(19) . . ? C65 V2 C61 64.95(19) . . ? N3 V2 C64 158.62(19) . . ? N4 V2 C64 101.11(17) . . ? C63 V2 C64 37.30(19) . . ? C60 V2 C64 67.02(18) . . ? C62 V2 C64 65.80(19) . . ? C65 V2 C64 36.69(18) . . ? C61 V2 C64 75.98(18) . . ? C14 N1 C1 116.6(4) . . ? C14 N1 V1 126.9(4) . . ? C1 N1 V1 116.2(3) . . ? C16 N2 C18 116.3(5) . . ? C16 N2 V1 127.9(4) . . ? C18 N2 V1 115.5(3) . . ? C43 N3 C30 114.9(4) . . ? C43 N3 V2 126.9(4) . . ? C30 N3 V2 118.0(3) . . ? C45 N4 C47 116.5(4) . . ? C45 N4 V2 127.9(4) . . ? C47 N4 V2 115.4(3) . . ? C2 C1 C9 121.1(5) . . ? C2 C1 N1 120.6(5) . . ? C9 C1 N1 118.3(5) . . ? C6 C2 C1 118.7(5) . . ? C6 C2 C3 119.9(5) . . ? C1 C2 C3 121.3(5) . . ? C2 C3 C5 115.6(6) . . ? C2 C3 C4 112.5(5) . . ? C5 C3 C4 106.6(6) . . ? C2 C3 H3 107.2 . . ? C5 C3 H3 107.2 . . ? C4 C3 H3 107.2 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C2 119.9(6) . . ? C7 C6 H6 120.0 . . ? C2 C6 H6 120.0 . . ? C8 C7 C6 121.4(6) . . ? C8 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C7 C8 C9 121.3(6) . . ? C7 C8 H8 119.3 . . ? C9 C8 H8 119.3 . . ? C8 C9 C1 117.5(6) . . ? C8 C9 C10 120.5(6) . . ? C1 C9 C10 122.0(5) . . ? C12 C10 C11 109.9(6) . . ? C12 C10 C9 111.8(5) . . ? C11 C10 C9 111.3(6) . . ? C12 C10 H10 107.9 . . ? C11 C10 H10 107.9 . . ? C9 C10 H10 107.9 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 C15 124.1(5) . . ? N1 C14 C13 120.7(5) . . ? C15 C14 C13 115.2(5) . . ? C16 C15 C14 128.3(5) . . ? C16 C15 H15 115.9 . . ? C14 C15 H15 115.9 . . ? N2 C16 C15 123.5(5) . . ? N2 C16 C17 122.0(5) . . ? C15 C16 C17 114.4(5) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C26 C18 C19 121.5(6) . . ? C26 C18 N2 120.8(5) . . ? C19 C18 N2 117.7(5) . . ? C23 C19 C18 118.8(6) . . ? C23 C19 C20 119.2(6) . . ? C18 C19 C20 122.0(6) . . ? C22 C20 C21 111.6(6) . . ? C22 C20 C19 113.5(6) . . ? C21 C20 C19 111.2(6) . . ? C22 C20 H20 106.7 . . ? C21 C20 H20 106.7 . . ? C19 C20 H20 106.7 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C19 121.5(7) . . ? C24 C23 H23 119.3 . . ? C19 C23 H23 119.3 . . ? C23 C24 C25 119.2(7) . . ? C23 C24 H24 120.4 . . ? C25 C24 H24 120.4 . . ? C24 C25 C26 122.0(6) . . ? C24 C25 H25 119.0 . . ? C26 C25 H25 119.0 . . ? C18 C26 C25 117.0(6) . . ? C18 C26 C27 124.1(5) . . ? C25 C26 C27 118.9(6) . . ? C29A C27 C26 130.4(16) . . ? C29A C27 C28 102.6(11) . . ? C26 C27 C28 112.9(7) . . ? C29A C27 C29 25.7(12) . . ? C26 C27 C29 107.7(8) . . ? C28 C27 C29 107.2(6) . . ? C29A C27 H27 102.4 . . ? C26 C27 H27 102.4 . . ? C28 C27 H27 102.4 . . ? C29 C27 H27 124.3 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29A H29A 109.5 . . ? C27 C29A H29B 109.5 . . ? H29A C29A H29B 109.5 . . ? C27 C29A H29C 109.5 . . ? H29A C29A H29C 109.5 . . ? H29B C29A H29C 109.5 . . ? C27 C29 H29D 109.5 . . ? C27 C29 H29E 109.5 . . ? H29D C29 H29E 109.5 . . ? C27 C29 H29F 109.5 . . ? H29D C29 H29F 109.5 . . ? H29E C29 H29F 109.5 . . ? C31 C30 C38 120.4(6) . . ? C31 C30 N3 119.8(5) . . ? C38 C30 N3 119.7(5) . . ? C35 C31 C30 118.1(6) . . ? C35 C31 C32 119.2(6) . . ? C30 C31 C32 122.7(6) . . ? C33 C32 C34 108.1(6) . . ? C33 C32 C31 112.4(6) . . ? C34 C32 C31 112.3(5) . . ? C33 C32 H32 107.9 . . ? C34 C32 H32 107.9 . . ? C31 C32 H32 107.9 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C31 121.2(7) . . ? C36 C35 H35 119.4 . . ? C31 C35 H35 119.4 . . ? C37 C36 C35 120.6(7) . . ? C37 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C36 C37 C38 121.9(7) . . ? C36 C37 H37 119.1 . . ? C38 C37 H37 119.1 . . ? C37 C38 C30 117.8(6) . . ? C37 C38 C39 121.0(6) . . ? C30 C38 C39 121.2(5) . . ? C41 C39 C38 113.0(6) . . ? C41 C39 C40 107.3(6) . . ? C38 C39 C40 112.7(6) . . ? C41 C39 H39 107.9 . . ? C38 C39 H39 107.9 . . ? C40 C39 H39 107.9 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 H42A 109.5 . . ? C43 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C43 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N3 C43 C44 123.6(5) . . ? N3 C43 C42 120.7(5) . . ? C44 C43 C42 115.6(5) . . ? C43 C44 C45 128.9(5) . . ? C43 C44 H44 115.5 . . ? C45 C44 H44 115.5 . . ? N4 C45 C44 123.4(5) . . ? N4 C45 C46 122.3(5) . . ? C44 C45 C46 114.3(4) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 C55 120.3(5) . . ? C48 C47 N4 119.9(5) . . ? C55 C47 N4 119.7(5) . . ? C52 C48 C47 118.4(5) . . ? C52 C48 C49 118.4(5) . . ? C47 C48 C49 123.1(5) . . ? C48 C49 C50 114.4(5) . . ? C48 C49 C51 111.2(5) . . ? C50 C49 C51 107.3(5) . . ? C48 C49 H49 107.9 . . ? C50 C49 H49 107.9 . . ? C51 C49 H49 107.9 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C53 C52 C48 121.2(5) . . ? C53 C52 H52 119.4 . . ? C48 C52 H52 119.4 . . ? C54 C53 C52 120.2(5) . . ? C54 C53 H53 119.9 . . ? C52 C53 H53 119.9 . . ? C53 C54 C55 121.5(5) . . ? C53 C54 H54 119.2 . . ? C55 C54 H54 119.2 . . ? C54 C55 C47 118.4(5) . . ? C54 C55 C56 120.5(5) . . ? C47 C55 C56 121.0(5) . . ? C58 C56 C57 109.6(5) . . ? C58 C56 C55 113.3(5) . . ? C57 C56 C55 109.3(5) . . ? C58 C56 H56 108.2 . . ? C57 C56 H56 108.2 . . ? C55 C56 H56 108.2 . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C56 C58 H58A 109.5 . . ? C56 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C56 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C60 C59 H59A 109.5 . . ? C60 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C60 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C65 C60 C61 116.6(5) . . ? C65 C60 C59 121.4(5) . . ? C61 C60 C59 121.7(5) . . ? C65 C60 V2 72.6(3) . . ? C61 C60 V2 74.3(3) . . ? C59 C60 V2 128.2(3) . . ? C65 C60 V1 68.2(3) . . ? C61 C60 V1 65.2(3) . . ? C59 C60 V1 133.3(3) . . ? V2 C60 V1 98.48(19) . . ? C62 C61 C60 121.1(5) . . ? C62 C61 V1 72.2(3) . . ? C60 C61 V1 79.0(3) . . ? C62 C61 V2 68.9(3) . . ? C60 C61 V2 68.3(3) . . ? V1 C61 V2 101.6(2) . . ? C62 C61 H61 119.4 . . ? C60 C61 H61 119.4 . . ? V1 C61 H61 120.5 . . ? V2 C61 H61 137.9 . . ? C63 C62 C61 119.9(5) . . ? C63 C62 V2 69.4(3) . . ? C61 C62 V2 74.3(3) . . ? C63 C62 V1 72.9(3) . . ? C61 C62 V1 70.9(3) . . ? V2 C62 V1 103.3(2) . . ? C63 C62 H62 120.1 . . ? C61 C62 H62 120.1 . . ? V2 C62 H62 128.4 . . ? V1 C62 H62 128.3 . . ? C62 C63 C64 119.6(5) . . ? C62 C63 V2 73.2(3) . . ? C64 C63 V2 76.7(3) . . ? C62 C63 V1 70.8(3) . . ? C64 C63 V1 67.5(3) . . ? V2 C63 V1 104.0(2) . . ? C62 C63 H63 120.2 . . ? C64 C63 H63 120.2 . . ? V2 C63 H63 121.0 . . ? V1 C63 H63 134.9 . . ? C65 C64 C63 118.1(5) . . ? C65 C64 V1 76.0(3) . . ? C63 C64 V1 74.9(3) . . ? C65 C64 V2 68.9(3) . . ? C63 C64 V2 66.0(3) . . ? V1 C64 V2 102.6(2) . . ? C65 C64 H64 121.0 . . ? C63 C64 H64 121.0 . . ? V1 C64 H64 119.2 . . ? V2 C64 H64 138.2 . . ? C60 C65 C64 122.2(5) . . ? C60 C65 V2 70.2(3) . . ? C64 C65 V2 74.4(3) . . ? C60 C65 V1 77.0(3) . . ? C64 C65 V1 66.8(3) . . ? V2 C65 V1 101.0(2) . . ? C60 C65 H65 118.9 . . ? C64 C65 H65 118.9 . . ? V2 C65 H65 129.0 . . ? V1 C65 H65 129.9 . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 25.36 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 0.516 _refine_diff_density_min -0.556 _refine_diff_density_rms 0.147 # Attachment 'Complex 2.cif' data_complex_2 _database_code_depnum_ccdc_archive 'CCDC 645659' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C64 H96 N4 O3 V2' _chemical_formula_sum 'C64 H96 N4 O3 V2' _chemical_formula_weight 1071.33 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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 13.7676(2) _cell_length_b 21.2023(4) _cell_length_c 23.5956(5) _cell_angle_alpha 90.00 _cell_angle_beta 106.4620(10) _cell_angle_gamma 90.00 _cell_volume 6605.3(2) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 29732 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.35 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.8 _exptl_crystal_size_mid 0.8 _exptl_crystal_size_min 0.5 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.077 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2312 _exptl_absorpt_coefficient_mu 0.325 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7099 _exptl_absorpt_correction_T_max 0.9752 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32107 _diffrn_reflns_av_R_equivalents 0.1059 _diffrn_reflns_av_sigmaI/netI 0.0741 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 25.35 _reflns_number_total 11904 _reflns_number_gt 9165 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 19' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1087P)^2^+4.1296P] 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 noref _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0135(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11904 _refine_ls_number_parameters 659 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0940 _refine_ls_R_factor_gt 0.0721 _refine_ls_wR_factor_ref 0.2076 _refine_ls_wR_factor_gt 0.1911 _refine_ls_goodness_of_fit_ref 1.099 _refine_ls_restrained_S_all 1.099 _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 C1 C 0.1144(2) 0.09209(15) 0.10817(13) 0.0286(7) Uani 1 1 d . . . C2 C 0.2124(3) 0.06638(16) 0.12137(14) 0.0321(7) Uani 1 1 d . . . C3 C 0.2628(3) 0.03426(17) 0.17960(15) 0.0363(8) Uani 1 1 d . . . H3 H 0.2396 0.0556 0.2103 0.044 Uiso 1 1 calc R . . C4 C 0.2308(3) -0.03471(18) 0.17849(19) 0.0512(10) Uani 1 1 d . . . H4A H 0.2628 -0.0538 0.2160 0.077 Uiso 1 1 calc R . . H4B H 0.2508 -0.0566 0.1480 0.077 Uiso 1 1 calc R . . H4C H 0.1585 -0.0371 0.1707 0.077 Uiso 1 1 calc R . . C5 C 0.3784(3) 0.0382(2) 0.19757(17) 0.0476(10) Uani 1 1 d . . . H5A H 0.4055 0.0178 0.2350 0.071 Uiso 1 1 calc R . . H5B H 0.3988 0.0816 0.2007 0.071 Uiso 1 1 calc R . . H5C H 0.4034 0.0176 0.1683 0.071 Uiso 1 1 calc R . . C6 C 0.2614(3) 0.06825(19) 0.07688(16) 0.0424(9) Uani 1 1 d . . . H6 H 0.3254 0.0503 0.0839 0.051 Uiso 1 1 calc R . . C7 C 0.2173(3) 0.0960(2) 0.02330(17) 0.0495(10) Uani 1 1 d . . . H7 H 0.2516 0.0967 -0.0055 0.059 Uiso 1 1 calc R . . C8 C 0.1225(3) 0.1228(2) 0.01169(15) 0.0485(10) Uani 1 1 d . . . H8 H 0.0938 0.1419 -0.0247 0.058 Uiso 1 1 calc R . . C9 C 0.0696(3) 0.12140(17) 0.05348(14) 0.0378(8) Uani 1 1 d . . . C10 C -0.0353(3) 0.1511(2) 0.03815(17) 0.0528(11) Uani 1 1 d . . . H10 H -0.0619 0.1463 0.0723 0.063 Uiso 1 1 calc R . . C11 C -0.0289(5) 0.2217(3) 0.0259(2) 0.0826(18) Uani 1 1 d . . . H11A H -0.0954 0.2398 0.0163 0.124 Uiso 1 1 calc R . . H11B H -0.0009 0.2274 -0.0067 0.124 Uiso 1 1 calc R . . H11C H 0.0138 0.2420 0.0604 0.124 Uiso 1 1 calc R . . C12 C -0.1088(4) 0.1178(3) -0.0152(2) 0.0785(16) Uani 1 1 d . . . H12A H -0.1743 0.1372 -0.0236 0.118 Uiso 1 1 calc R . . H12B H -0.1140 0.0740 -0.0061 0.118 Uiso 1 1 calc R . . H12C H -0.0836 0.1215 -0.0490 0.118 Uiso 1 1 calc R . . C13 C -0.0261(3) -0.00561(19) 0.10203(18) 0.0483(10) Uani 1 1 d . . . H13A H 0.0245 -0.0017 0.0814 0.072 Uiso 1 1 calc R . . H13B H -0.0922 -0.0031 0.0743 0.072 Uiso 1 1 calc R . . H13C H -0.0186 -0.0455 0.1220 0.072 Uiso 1 1 calc R . . C14 C -0.0136(2) 0.04673(16) 0.14645(14) 0.0320(7) Uani 1 1 d . . . C15 C -0.0824(3) 0.04713(17) 0.17995(16) 0.0366(8) Uani 1 1 d . . . H15 H -0.1214 0.0109 0.1777 0.044 Uiso 1 1 calc R . . C16 C -0.1001(2) 0.09497(17) 0.21642(14) 0.0333(7) Uani 1 1 d . . . C17 C -0.1891(3) 0.0866(2) 0.2407(2) 0.0549(11) Uani 1 1 d . . . H17A H -0.1941 0.1223 0.2647 0.082 Uiso 1 1 calc R . . H17B H -0.1800 0.0490 0.2643 0.082 Uiso 1 1 calc R . . H17C H -0.2500 0.0830 0.2087 0.082 Uiso 1 1 calc R . . C18 C -0.0764(2) 0.19859(16) 0.25920(15) 0.0324(7) Uani 1 1 d . . . C19 C -0.1386(3) 0.24558(18) 0.22479(16) 0.0398(8) Uani 1 1 d . . . C20 C -0.1774(3) 0.2414(2) 0.15781(18) 0.0541(11) Uani 1 1 d . . . H20 H -0.1461 0.2045 0.1450 0.065 Uiso 1 1 calc R . . C21 C -0.1489(4) 0.3000(3) 0.1281(2) 0.0734(15) Uani 1 1 d . . . H21A H -0.1742 0.2957 0.0860 0.110 Uiso 1 1 calc R . . H21B H -0.0765 0.3042 0.1391 0.110 Uiso 1 1 calc R . . H21C H -0.1781 0.3367 0.1406 0.110 Uiso 1 1 calc R . . C22 C -0.2939(4) 0.2319(4) 0.1383(3) 0.094(2) Uani 1 1 d . . . H22A H -0.3175 0.2292 0.0960 0.142 Uiso 1 1 calc R . . H22B H -0.3259 0.2669 0.1516 0.142 Uiso 1 1 calc R . . H22C H -0.3105 0.1936 0.1552 0.142 Uiso 1 1 calc R . . C23 C -0.1665(3) 0.29665(19) 0.25339(18) 0.0449(9) Uani 1 1 d . . . H23 H -0.2074 0.3279 0.2312 0.054 Uiso 1 1 calc R . . C24 C -0.1349(3) 0.30192(19) 0.31378(18) 0.0457(9) Uani 1 1 d . . . H24 H -0.1536 0.3368 0.3321 0.055 Uiso 1 1 calc R . . C25 C -0.0758(3) 0.25567(19) 0.34704(17) 0.0441(9) Uani 1 1 d . . . H25 H -0.0560 0.2593 0.3880 0.053 Uiso 1 1 calc R . . C26 C -0.0444(3) 0.20329(17) 0.32104(15) 0.0363(8) Uani 1 1 d . . . C27 C 0.0191(3) 0.15267(18) 0.36082(16) 0.0398(8) Uani 1 1 d . . . H27 H 0.0357 0.1201 0.3356 0.048 Uiso 1 1 calc R . . C28 C -0.0404(4) 0.1215(2) 0.3995(2) 0.0599(12) Uani 1 1 d . . . H28A H 0.0009 0.0898 0.4239 0.090 Uiso 1 1 calc R . . H28B H -0.1007 0.1024 0.3747 0.090 Uiso 1 1 calc R . . H28C H -0.0585 0.1528 0.4241 0.090 Uiso 1 1 calc R . . C29 C 0.1180(3) 0.1792(2) 0.40047(17) 0.0460(9) Uani 1 1 d . . . H29A H 0.1558 0.1461 0.4246 0.069 Uiso 1 1 calc R . . H29B H 0.1033 0.2116 0.4253 0.069 Uiso 1 1 calc R . . H29C H 0.1571 0.1968 0.3765 0.069 Uiso 1 1 calc R . . C30 C 0.3991(3) 0.05117(16) 0.37085(14) 0.0317(7) Uani 1 1 d . . . C31 C 0.3211(3) 0.00619(16) 0.36009(15) 0.0347(7) Uani 1 1 d . . . C32 C 0.2144(3) 0.02152(18) 0.36239(16) 0.0383(8) Uani 1 1 d . . . H32 H 0.2091 0.0675 0.3651 0.046 Uiso 1 1 calc R . . C33 C 0.1933(3) -0.0072(3) 0.41738(19) 0.0603(12) Uani 1 1 d . . . H33A H 0.1257 0.0032 0.4178 0.090 Uiso 1 1 calc R . . H33B H 0.2407 0.0094 0.4522 0.090 Uiso 1 1 calc R . . H33C H 0.2005 -0.0522 0.4166 0.090 Uiso 1 1 calc R . . C34 C 0.1333(3) -0.0003(2) 0.30674(17) 0.0453(9) Uani 1 1 d . . . H34A H 0.0674 0.0104 0.3101 0.068 Uiso 1 1 calc R . . H34B H 0.1379 -0.0451 0.3026 0.068 Uiso 1 1 calc R . . H34C H 0.1438 0.0203 0.2727 0.068 Uiso 1 1 calc R . . C35 C 0.3453(3) -0.05563(18) 0.34902(17) 0.0446(9) Uani 1 1 d . . . H35 H 0.2951 -0.0864 0.3419 0.054 Uiso 1 1 calc R . . C36 C 0.4413(3) -0.07223(18) 0.34839(18) 0.0485(10) Uani 1 1 d . . . H36 H 0.4557 -0.1140 0.3417 0.058 Uiso 1 1 calc R . . C37 C 0.5167(3) -0.02737(19) 0.35764(16) 0.0451(9) Uani 1 1 d . . . H37 H 0.5811 -0.0391 0.3564 0.054 Uiso 1 1 calc R . . C38 C 0.4975(3) 0.03530(17) 0.36886(15) 0.0358(8) Uani 1 1 d . . . C39 C 0.5823(3) 0.0838(2) 0.37864(17) 0.0433(9) Uani 1 1 d . . . H39 H 0.5519 0.1256 0.3790 0.052 Uiso 1 1 calc R . . C40 C 0.6322(3) 0.0833(3) 0.3293(2) 0.0614(12) Uani 1 1 d . . . H40A H 0.6848 0.1145 0.3369 0.092 Uiso 1 1 calc R . . H40B H 0.5827 0.0926 0.2925 0.092 Uiso 1 1 calc R . . H40C H 0.6609 0.0424 0.3270 0.092 Uiso 1 1 calc R . . C41 C 0.6605(4) 0.0743(3) 0.4387(2) 0.0687(14) Uani 1 1 d . . . H41A H 0.7126 0.1057 0.4439 0.103 Uiso 1 1 calc R . . H41B H 0.6899 0.0331 0.4402 0.103 Uiso 1 1 calc R . . H41C H 0.6280 0.0783 0.4695 0.103 Uiso 1 1 calc R . . C42 C 0.4249(3) 0.0877(2) 0.48981(16) 0.0515(10) Uani 1 1 d . . . H42A H 0.4226 0.0458 0.4740 0.077 Uiso 1 1 calc R . . H42B H 0.3766 0.0911 0.5121 0.077 Uiso 1 1 calc R . . H42C H 0.4916 0.0961 0.5151 0.077 Uiso 1 1 calc R . . C43 C 0.3990(3) 0.13527(18) 0.43924(14) 0.0357(8) Uani 1 1 d . . . C44 C 0.3996(3) 0.19886(18) 0.45551(15) 0.0392(8) Uani 1 1 d . . . H44 H 0.4064 0.2067 0.4952 0.047 Uiso 1 1 calc R . . C45 C 0.3913(3) 0.25146(17) 0.41954(15) 0.0357(8) Uani 1 1 d . . . C46 C 0.4179(4) 0.3131(2) 0.45186(18) 0.0537(11) Uani 1 1 d . . . H46A H 0.4104 0.3468 0.4238 0.081 Uiso 1 1 calc R . . H46B H 0.4868 0.3117 0.4763 0.081 Uiso 1 1 calc R . . H46C H 0.3736 0.3202 0.4761 0.081 Uiso 1 1 calc R . . C47 C 0.3752(3) 0.30586(16) 0.32901(15) 0.0341(7) Uani 1 1 d . . . C48 C 0.2909(3) 0.34427(16) 0.30459(15) 0.0341(8) Uani 1 1 d . . . C49 C 0.1850(3) 0.32685(17) 0.30778(16) 0.0376(8) Uani 1 1 d . . . H49 H 0.1800 0.2808 0.3057 0.045 Uiso 1 1 calc R . . C50 C 0.1688(3) 0.3468(2) 0.36696(19) 0.0530(10) Uani 1 1 d . . . H50A H 0.1020 0.3347 0.3678 0.079 Uiso 1 1 calc R . . H50B H 0.1761 0.3917 0.3713 0.079 Uiso 1 1 calc R . . H50C H 0.2182 0.3264 0.3987 0.079 Uiso 1 1 calc R . . C51 C 0.1006(3) 0.3527(2) 0.25717(19) 0.0509(10) Uani 1 1 d . . . H51A H 0.0364 0.3397 0.2618 0.076 Uiso 1 1 calc R . . H51B H 0.1076 0.3368 0.2205 0.076 Uiso 1 1 calc R . . H51C H 0.1041 0.3979 0.2572 0.076 Uiso 1 1 calc R . . C52 C 0.3064(3) 0.40066(18) 0.27846(17) 0.0460(9) Uani 1 1 d . . . H52 H 0.2517 0.4272 0.2627 0.055 Uiso 1 1 calc R . . C53 C 0.4010(4) 0.4181(2) 0.2753(2) 0.0566(11) Uani 1 1 d . . . H53 H 0.4100 0.4566 0.2587 0.068 Uiso 1 1 calc R . . C54 C 0.4818(3) 0.3785(2) 0.2967(2) 0.0523(10) Uani 1 1 d . . . H54 H 0.5451 0.3903 0.2934 0.063 Uiso 1 1 calc R . . C55 C 0.4718(3) 0.32152(18) 0.32302(18) 0.0436(9) Uani 1 1 d . . . C56 C 0.5639(3) 0.2782(2) 0.3434(2) 0.0541(11) Uani 1 1 d . . . H56 H 0.5418 0.2395 0.3588 0.065 Uiso 1 1 calc R . . C57 C 0.6026(4) 0.2601(3) 0.2915(3) 0.0774(15) Uani 1 1 d . . . H57A H 0.6599 0.2326 0.3049 0.116 Uiso 1 1 calc R . . H57B H 0.6223 0.2974 0.2746 0.116 Uiso 1 1 calc R . . H57C H 0.5499 0.2388 0.2623 0.116 Uiso 1 1 calc R . . C58 C 0.6485(4) 0.3073(3) 0.3930(2) 0.0762(15) Uani 1 1 d . . . H58A H 0.7042 0.2783 0.4045 0.114 Uiso 1 1 calc R . . H58B H 0.6237 0.3160 0.4263 0.114 Uiso 1 1 calc R . . H58C H 0.6707 0.3458 0.3793 0.114 Uiso 1 1 calc R . . C59 C 0.4141(9) 0.2228(6) 0.1280(4) 0.163(4) Uani 1 1 d . . . H59A H 0.4317 0.1906 0.1579 0.245 Uiso 1 1 calc R . . H59B H 0.4723 0.2486 0.1303 0.245 Uiso 1 1 calc R . . H59C H 0.3919 0.2034 0.0897 0.245 Uiso 1 1 calc R . . C60 C 0.3348(10) 0.2607(8) 0.1373(7) 0.218(7) Uani 1 1 d . . . H60A H 0.2800 0.2322 0.1379 0.262 Uiso 1 1 calc R . . H60B H 0.3597 0.2778 0.1770 0.262 Uiso 1 1 calc R . . C61 C 0.2924(8) 0.3095(6) 0.1018(4) 0.128(3) Uani 1 1 d . . . H61A H 0.3487 0.3360 0.0998 0.154 Uiso 1 1 calc R . . H61B H 0.2661 0.2912 0.0628 0.154 Uiso 1 1 calc R . . C62 C 0.2195(10) 0.3502(6) 0.1075(5) 0.149(4) Uani 1 1 d . . . H62A H 0.1684 0.3229 0.1156 0.179 Uiso 1 1 calc R . . H62B H 0.2506 0.3718 0.1444 0.179 Uiso 1 1 calc R . . C63 C 0.1667(10) 0.3943(7) 0.0739(6) 0.170(4) Uani 1 1 d . . . H63A H 0.1319 0.3728 0.0375 0.204 Uiso 1 1 calc R . . H63B H 0.2168 0.4210 0.0641 0.204 Uiso 1 1 calc R . . C64 C 0.0956(13) 0.4357(6) 0.0837(6) 0.209(6) Uani 1 1 d . . . H64A H 0.0706 0.4621 0.0496 0.313 Uiso 1 1 calc R . . H64B H 0.1265 0.4615 0.1175 0.313 Uiso 1 1 calc R . . H64C H 0.0406 0.4124 0.0909 0.313 Uiso 1 1 calc R . . V1 V 0.08694(4) 0.16277(2) 0.20994(2) 0.02444(17) Uani 1 1 d . . . V2 V 0.32841(4) 0.17040(3) 0.31136(2) 0.02557(18) Uani 1 1 d . . . N1 N 0.05966(19) 0.09037(12) 0.15222(11) 0.0269(6) Uani 1 1 d . . . N2 N -0.0434(2) 0.14664(13) 0.22940(12) 0.0295(6) Uani 1 1 d . . . N3 N 0.37893(19) 0.11646(13) 0.38307(11) 0.0290(6) Uani 1 1 d . . . N4 N 0.3651(2) 0.24895(13) 0.36079(11) 0.0308(6) Uani 1 1 d . . . O1 O 0.07224(19) 0.22477(11) 0.17031(10) 0.0377(6) Uani 1 1 d . . . O2 O 0.40931(18) 0.16574(12) 0.27500(10) 0.0389(6) Uani 1 1 d . . . O3 O 0.19627(17) 0.15662(11) 0.27324(10) 0.0335(5) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0348(17) 0.0275(16) 0.0256(15) -0.0031(13) 0.0123(13) -0.0026(13) C2 0.0358(17) 0.0327(18) 0.0303(16) -0.0042(14) 0.0135(13) -0.0017(14) C3 0.0385(19) 0.0367(19) 0.0338(17) -0.0020(15) 0.0106(14) 0.0102(15) C4 0.063(3) 0.038(2) 0.051(2) 0.0058(18) 0.0141(19) 0.0081(19) C5 0.040(2) 0.055(2) 0.045(2) -0.0017(18) 0.0092(16) 0.0148(18) C6 0.0362(19) 0.055(2) 0.0405(19) -0.0022(17) 0.0183(15) 0.0034(17) C7 0.052(2) 0.066(3) 0.0368(19) -0.0010(19) 0.0238(17) -0.004(2) C8 0.066(3) 0.057(3) 0.0240(17) 0.0036(16) 0.0150(17) 0.002(2) C9 0.048(2) 0.039(2) 0.0261(16) -0.0007(14) 0.0102(14) 0.0042(16) C10 0.059(3) 0.069(3) 0.0293(18) 0.0059(18) 0.0109(17) 0.027(2) C11 0.126(5) 0.079(4) 0.042(2) 0.015(2) 0.024(3) 0.053(4) C12 0.053(3) 0.113(5) 0.055(3) -0.011(3) -0.008(2) 0.021(3) C13 0.050(2) 0.042(2) 0.055(2) -0.0195(19) 0.0194(18) -0.0126(18) C14 0.0317(17) 0.0297(17) 0.0342(17) -0.0029(14) 0.0088(13) -0.0016(14) C15 0.0358(18) 0.0309(18) 0.0460(19) -0.0048(15) 0.0163(15) -0.0114(15) C16 0.0300(17) 0.0380(19) 0.0348(17) -0.0028(15) 0.0137(13) -0.0060(14) C17 0.045(2) 0.067(3) 0.064(3) -0.017(2) 0.035(2) -0.020(2) C18 0.0289(16) 0.0336(18) 0.0387(18) -0.0031(15) 0.0159(14) 0.0030(14) C19 0.0357(18) 0.044(2) 0.0424(19) -0.0019(16) 0.0165(15) 0.0047(16) C20 0.052(2) 0.063(3) 0.042(2) 0.002(2) 0.0051(18) 0.024(2) C21 0.098(4) 0.074(3) 0.054(3) 0.018(2) 0.031(3) 0.039(3) C22 0.060(3) 0.135(6) 0.072(4) 0.000(4) -0.008(3) -0.001(3) C23 0.0381(19) 0.045(2) 0.056(2) 0.0025(19) 0.0214(17) 0.0125(17) C24 0.047(2) 0.043(2) 0.054(2) -0.0098(18) 0.0257(18) 0.0096(18) C25 0.047(2) 0.047(2) 0.043(2) -0.0118(17) 0.0214(17) 0.0053(18) C26 0.0355(18) 0.041(2) 0.0362(18) -0.0039(15) 0.0163(14) -0.0037(15) C27 0.046(2) 0.041(2) 0.0367(18) -0.0026(16) 0.0181(16) 0.0040(16) C28 0.062(3) 0.066(3) 0.056(3) 0.016(2) 0.024(2) -0.003(2) C29 0.048(2) 0.055(2) 0.0368(19) 0.0003(17) 0.0166(16) 0.0097(19) C30 0.0365(17) 0.0295(17) 0.0291(16) 0.0024(13) 0.0094(13) 0.0043(14) C31 0.0392(18) 0.0339(18) 0.0330(17) 0.0053(14) 0.0135(14) 0.0034(15) C32 0.0400(19) 0.0344(19) 0.0430(19) 0.0030(16) 0.0157(15) -0.0009(15) C33 0.055(3) 0.083(3) 0.048(2) 0.010(2) 0.0225(19) 0.003(2) C34 0.041(2) 0.047(2) 0.049(2) 0.0031(18) 0.0142(17) -0.0033(17) C35 0.052(2) 0.0312(19) 0.051(2) 0.0027(17) 0.0146(18) 0.0009(17) C36 0.061(3) 0.032(2) 0.053(2) 0.0005(17) 0.0167(19) 0.0127(18) C37 0.045(2) 0.049(2) 0.043(2) 0.0074(17) 0.0147(16) 0.0181(18) C38 0.0351(18) 0.039(2) 0.0329(17) 0.0095(15) 0.0089(14) 0.0084(15) C39 0.0331(19) 0.049(2) 0.047(2) 0.0041(18) 0.0099(16) 0.0060(16) C40 0.043(2) 0.077(3) 0.070(3) 0.010(2) 0.025(2) -0.002(2) C41 0.052(3) 0.085(4) 0.060(3) 0.002(3) 0.001(2) -0.007(2) C42 0.071(3) 0.051(2) 0.0302(18) 0.0096(17) 0.0107(18) 0.010(2) C43 0.0370(18) 0.043(2) 0.0281(16) 0.0040(15) 0.0103(14) 0.0018(15) C44 0.048(2) 0.044(2) 0.0260(16) -0.0061(15) 0.0100(14) -0.0021(17) C45 0.0363(18) 0.0356(19) 0.0368(18) -0.0084(15) 0.0128(14) -0.0041(15) C46 0.070(3) 0.047(2) 0.041(2) -0.0116(18) 0.0096(19) -0.006(2) C47 0.0394(19) 0.0291(17) 0.0348(17) -0.0046(14) 0.0120(14) -0.0099(15) C48 0.0431(19) 0.0264(17) 0.0350(17) -0.0052(14) 0.0147(15) -0.0060(14) C49 0.042(2) 0.0315(18) 0.0428(19) -0.0052(15) 0.0183(16) -0.0029(15) C50 0.056(3) 0.057(3) 0.052(2) -0.008(2) 0.026(2) 0.003(2) C51 0.046(2) 0.046(2) 0.059(3) 0.000(2) 0.0107(19) 0.0024(18) C52 0.055(2) 0.035(2) 0.048(2) 0.0034(17) 0.0144(18) -0.0024(18) C53 0.067(3) 0.040(2) 0.066(3) 0.009(2) 0.024(2) -0.019(2) C54 0.053(2) 0.047(2) 0.063(3) -0.001(2) 0.027(2) -0.021(2) C55 0.040(2) 0.040(2) 0.052(2) -0.0022(17) 0.0144(17) -0.0143(16) C56 0.034(2) 0.051(2) 0.076(3) 0.003(2) 0.0135(19) -0.0149(18) C57 0.049(3) 0.078(4) 0.114(4) -0.011(3) 0.037(3) -0.013(2) C58 0.049(3) 0.084(4) 0.086(4) 0.009(3) 0.002(2) -0.014(3) C59 0.172(11) 0.200(11) 0.111(7) 0.001(7) 0.028(7) -0.063(9) C60 0.147(10) 0.285(18) 0.253(16) 0.114(15) 0.105(11) 0.057(11) C61 0.125(7) 0.181(10) 0.091(5) 0.019(6) 0.052(5) 0.005(7) C62 0.171(11) 0.143(9) 0.130(8) 0.016(7) 0.036(7) 0.018(8) C63 0.170(11) 0.167(11) 0.179(11) 0.016(9) 0.061(9) 0.028(9) C64 0.276(18) 0.159(11) 0.208(13) 0.017(10) 0.095(12) 0.032(12) V1 0.0252(3) 0.0252(3) 0.0243(3) -0.0009(2) 0.0092(2) -0.0005(2) V2 0.0257(3) 0.0274(3) 0.0244(3) -0.0003(2) 0.0084(2) -0.0023(2) N1 0.0294(13) 0.0258(13) 0.0259(12) 0.0001(11) 0.0084(10) 0.0006(11) N2 0.0290(14) 0.0297(14) 0.0327(14) -0.0012(12) 0.0136(11) 0.0021(11) N3 0.0276(13) 0.0322(15) 0.0281(13) 0.0015(11) 0.0091(11) 0.0004(11) N4 0.0351(14) 0.0307(15) 0.0271(13) 0.0001(11) 0.0098(11) -0.0039(12) O1 0.0455(14) 0.0308(13) 0.0382(13) 0.0031(10) 0.0144(10) 0.0019(11) O2 0.0385(13) 0.0480(15) 0.0353(12) -0.0039(11) 0.0188(10) -0.0038(11) O3 0.0299(12) 0.0376(13) 0.0315(12) -0.0032(10) 0.0061(9) -0.0012(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.405(5) . ? C1 C9 1.407(5) . ? C1 N1 1.447(4) . ? C2 C6 1.401(5) . ? C2 C3 1.514(5) . ? C3 C4 1.526(5) . ? C3 C5 1.528(5) . ? C3 H3 0.9800 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.370(5) . ? C6 H6 0.9300 . ? C7 C8 1.378(6) . ? C7 H7 0.9300 . ? C8 C9 1.382(5) . ? C8 H8 0.9300 . ? C9 C10 1.523(5) . ? C10 C11 1.532(7) . ? C10 C12 1.543(6) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.503(5) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 N1 1.347(4) . ? C14 C15 1.395(5) . ? C15 C16 1.396(5) . ? C15 H15 0.9300 . ? C16 N2 1.329(4) . ? C16 C17 1.503(5) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C26 1.403(5) . ? C18 C19 1.412(5) . ? C18 N2 1.447(4) . ? C19 C23 1.386(5) . ? C19 C20 1.521(5) . ? C20 C21 1.531(7) . ? C20 C22 1.552(7) . ? C20 H20 0.9800 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.371(6) . ? C23 H23 0.9300 . ? C24 C25 1.371(6) . ? C24 H24 0.9300 . ? C25 C26 1.395(5) . ? C25 H25 0.9300 . ? C26 C27 1.527(5) . ? C27 C29 1.524(5) . ? C27 C28 1.539(6) . ? C27 H27 0.9800 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 C31 1.405(5) . ? C30 C38 1.410(5) . ? C30 N3 1.457(4) . ? C31 C35 1.395(5) . ? C31 C32 1.520(5) . ? C32 C33 1.534(5) . ? C32 C34 1.534(5) . ? C32 H32 0.9800 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 C36 1.373(6) . ? C35 H35 0.9300 . ? C36 C37 1.378(6) . ? C36 H36 0.9300 . ? C37 C38 1.395(5) . ? C37 H37 0.9300 . ? C38 C39 1.523(5) . ? C39 C40 1.511(6) . ? C39 C41 1.530(5) . ? C39 H39 0.9800 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 C43 1.526(5) . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 N3 1.336(4) . ? C43 C44 1.401(5) . ? C44 C45 1.386(5) . ? C44 H44 0.9300 . ? C45 N4 1.331(4) . ? C45 C46 1.506(5) . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C47 C48 1.400(5) . ? C47 C55 1.417(5) . ? C47 N4 1.448(4) . ? C48 C52 1.389(5) . ? C48 C49 1.526(5) . ? C49 C51 1.514(5) . ? C49 C50 1.535(5) . ? C49 H49 0.9800 . ? C50 H50A 0.9600 . ? C50 H50B 0.9600 . ? C50 H50C 0.9600 . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C51 H51C 0.9600 . ? C52 C53 1.375(6) . ? C52 H52 0.9300 . ? C53 C54 1.371(6) . ? C53 H53 0.9300 . ? C54 C55 1.384(6) . ? C54 H54 0.9300 . ? C55 C56 1.528(6) . ? C56 C57 1.518(7) . ? C56 C58 1.527(6) . ? C56 H56 0.9800 . ? C57 H57A 0.9600 . ? C57 H57B 0.9600 . ? C57 H57C 0.9600 . ? C58 H58A 0.9600 . ? C58 H58B 0.9600 . ? C58 H58C 0.9600 . ? C59 C60 1.423(15) . ? C59 H59A 0.9600 . ? C59 H59B 0.9600 . ? C59 H59C 0.9600 . ? C60 C61 1.355(14) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C61 C62 1.358(13) . ? C61 H61A 0.9700 . ? C61 H61B 0.9700 . ? C62 C63 1.305(13) . ? C62 H62A 0.9700 . ? C62 H62B 0.9700 . ? C63 C64 1.383(15) . ? C63 H63A 0.9700 . ? C63 H63B 0.9700 . ? C64 H64A 0.9600 . ? C64 H64B 0.9600 . ? C64 H64C 0.9600 . ? V1 O1 1.592(2) . ? V1 O3 1.800(2) . ? V1 N2 2.004(3) . ? V1 N1 2.015(3) . ? V2 O2 1.590(2) . ? V2 O3 1.810(2) . ? V2 N3 1.997(3) . ? V2 N4 2.014(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 C2 C1 C9 121.2(3) . . ? C2 C1 N1 119.6(3) . . ? C9 C1 N1 119.2(3) . . ? C6 C2 C1 117.3(3) . . ? C6 C2 C3 119.9(3) . . ? C1 C2 C3 122.7(3) . . ? C2 C3 C4 111.1(3) . . ? C2 C3 C5 113.6(3) . . ? C4 C3 C5 109.3(3) . . ? C2 C3 H3 107.5 . . ? C4 C3 H3 107.5 . . ? C5 C3 H3 107.5 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C2 121.4(3) . . ? C7 C6 H6 119.3 . . ? C2 C6 H6 119.3 . . ? C6 C7 C8 120.5(3) . . ? C6 C7 H7 119.8 . . ? C8 C7 H7 119.8 . . ? C7 C8 C9 120.7(3) . . ? C7 C8 H8 119.7 . . ? C9 C8 H8 119.7 . . ? C8 C9 C1 118.7(3) . . ? C8 C9 C10 118.6(3) . . ? C1 C9 C10 122.7(3) . . ? C9 C10 C11 110.3(4) . . ? C9 C10 C12 111.3(4) . . ? C11 C10 C12 110.6(4) . . ? C9 C10 H10 108.2 . . ? C11 C10 H10 108.2 . . ? C12 C10 H10 108.2 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 C15 123.2(3) . . ? N1 C14 C13 120.8(3) . . ? C15 C14 C13 115.9(3) . . ? C14 C15 C16 128.3(3) . . ? C14 C15 H15 115.9 . . ? C16 C15 H15 115.9 . . ? N2 C16 C15 123.1(3) . . ? N2 C16 C17 119.9(3) . . ? C15 C16 C17 116.9(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C26 C18 C19 120.6(3) . . ? C26 C18 N2 120.7(3) . . ? C19 C18 N2 118.7(3) . . ? C23 C19 C18 118.6(3) . . ? C23 C19 C20 119.2(3) . . ? C18 C19 C20 122.2(3) . . ? C19 C20 C21 111.6(4) . . ? C19 C20 C22 110.2(4) . . ? C21 C20 C22 110.3(4) . . ? C19 C20 H20 108.2 . . ? C21 C20 H20 108.2 . . ? C22 C20 H20 108.2 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C19 121.3(4) . . ? C24 C23 H23 119.4 . . ? C19 C23 H23 119.4 . . ? C25 C24 C23 119.9(4) . . ? C25 C24 H24 120.0 . . ? C23 C24 H24 120.0 . . ? C24 C25 C26 121.7(4) . . ? C24 C25 H25 119.1 . . ? C26 C25 H25 119.1 . . ? C25 C26 C18 118.0(3) . . ? C25 C26 C27 118.9(3) . . ? C18 C26 C27 123.1(3) . . ? C29 C27 C26 111.9(3) . . ? C29 C27 C28 109.1(3) . . ? C26 C27 C28 111.0(3) . . ? C29 C27 H27 108.2 . . ? C26 C27 H27 108.2 . . ? C28 C27 H27 108.2 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C31 C30 C38 121.7(3) . . ? C31 C30 N3 120.1(3) . . ? C38 C30 N3 118.2(3) . . ? C35 C31 C30 117.4(3) . . ? C35 C31 C32 119.5(3) . . ? C30 C31 C32 123.1(3) . . ? C31 C32 C33 111.2(3) . . ? C31 C32 C34 112.4(3) . . ? C33 C32 C34 109.7(3) . . ? C31 C32 H32 107.8 . . ? C33 C32 H32 107.8 . . ? C34 C32 H32 107.8 . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C31 121.6(4) . . ? C36 C35 H35 119.2 . . ? C31 C35 H35 119.2 . . ? C35 C36 C37 120.4(4) . . ? C35 C36 H36 119.8 . . ? C37 C36 H36 119.8 . . ? C36 C37 C38 120.9(4) . . ? C36 C37 H37 119.6 . . ? C38 C37 H37 119.6 . . ? C37 C38 C30 118.0(3) . . ? C37 C38 C39 119.6(3) . . ? C30 C38 C39 122.4(3) . . ? C40 C39 C38 112.0(3) . . ? C40 C39 C41 111.0(4) . . ? C38 C39 C41 111.1(3) . . ? C40 C39 H39 107.5 . . ? C38 C39 H39 107.5 . . ? C41 C39 H39 107.5 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C39 C41 H41A 109.5 . . ? C39 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C39 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C43 C42 H42A 109.5 . . ? C43 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C43 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N3 C43 C44 122.9(3) . . ? N3 C43 C42 121.0(3) . . ? C44 C43 C42 116.1(3) . . ? C45 C44 C43 127.8(3) . . ? C45 C44 H44 116.1 . . ? C43 C44 H44 116.1 . . ? N4 C45 C44 123.8(3) . . ? N4 C45 C46 121.2(3) . . ? C44 C45 C46 115.0(3) . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 C55 120.9(3) . . ? C48 C47 N4 120.6(3) . . ? C55 C47 N4 118.5(3) . . ? C52 C48 C47 118.0(3) . . ? C52 C48 C49 119.9(3) . . ? C47 C48 C49 122.0(3) . . ? C51 C49 C48 113.9(3) . . ? C51 C49 C50 109.9(3) . . ? C48 C49 C50 111.4(3) . . ? C51 C49 H49 107.1 . . ? C48 C49 H49 107.1 . . ? C50 C49 H49 107.1 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C53 C52 C48 121.4(4) . . ? C53 C52 H52 119.3 . . ? C48 C52 H52 119.3 . . ? C54 C53 C52 119.9(4) . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C53 C54 C55 121.7(4) . . ? C53 C54 H54 119.2 . . ? C55 C54 H54 119.2 . . ? C54 C55 C47 117.8(4) . . ? C54 C55 C56 119.1(4) . . ? C47 C55 C56 123.1(3) . . ? C57 C56 C58 110.7(4) . . ? C57 C56 C55 110.3(4) . . ? C58 C56 C55 112.6(4) . . ? C57 C56 H56 107.7 . . ? C58 C56 H56 107.7 . . ? C55 C56 H56 107.7 . . ? C56 C57 H57A 109.5 . . ? C56 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C56 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C56 C58 H58A 109.5 . . ? C56 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C56 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C60 C59 H59A 109.5 . . ? C60 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C60 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C61 C60 C59 123.5(12) . . ? C61 C60 H60A 106.5 . . ? C59 C60 H60A 106.5 . . ? C61 C60 H60B 106.5 . . ? C59 C60 H60B 106.5 . . ? H60A C60 H60B 106.5 . . ? C62 C61 C60 128.7(10) . . ? C62 C61 H61A 105.1 . . ? C60 C61 H61A 105.1 . . ? C62 C61 H61B 105.1 . . ? C60 C61 H61B 105.1 . . ? H61A C61 H61B 105.9 . . ? C63 C62 C61 134.0(12) . . ? C63 C62 H62A 103.7 . . ? C61 C62 H62A 103.7 . . ? C63 C62 H62B 103.7 . . ? C61 C62 H62B 103.7 . . ? H62A C62 H62B 105.3 . . ? C62 C63 C64 130.6(13) . . ? C62 C63 H63A 104.6 . . ? C64 C63 H63A 104.6 . . ? C62 C63 H63B 104.6 . . ? C64 C63 H63B 104.6 . . ? H63A C63 H63B 105.7 . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? O1 V1 O3 118.96(12) . . ? O1 V1 N2 107.60(12) . . ? O3 V1 N2 112.96(11) . . ? O1 V1 N1 105.29(11) . . ? O3 V1 N1 117.22(11) . . ? N2 V1 N1 90.99(11) . . ? O2 V2 O3 118.75(12) . . ? O2 V2 N3 107.01(12) . . ? O3 V2 N3 112.85(11) . . ? O2 V2 N4 105.34(12) . . ? O3 V2 N4 118.24(11) . . ? N3 V2 N4 90.74(11) . . ? C14 N1 C1 118.2(3) . . ? C14 N1 V1 125.6(2) . . ? C1 N1 V1 115.53(19) . . ? C16 N2 C18 119.7(3) . . ? C16 N2 V1 126.4(2) . . ? C18 N2 V1 113.9(2) . . ? C43 N3 C30 118.9(3) . . ? C43 N3 V2 126.5(2) . . ? C30 N3 V2 114.63(19) . . ? C45 N4 C47 118.0(3) . . ? C45 N4 V2 125.9(2) . . ? C47 N4 V2 115.8(2) . . ? V1 O3 V2 152.51(15) . . ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.35 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.662 _refine_diff_density_min -0.657 _refine_diff_density_rms 0.153 # Attachment 'Compplex 3.cif' data_complex_3 _database_code_depnum_ccdc_archive 'CCDC 645660' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C41 H51 N4 V' _chemical_formula_sum 'C41 H51 N4 V' _chemical_formula_weight 650.80 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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 12.7056(4) _cell_length_b 17.7171(6) _cell_length_c 18.9744(9) _cell_angle_alpha 90.00 _cell_angle_beta 98.778(2) _cell_angle_gamma 90.00 _cell_volume 4221.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 18260 _cell_measurement_theta_min 2.037 _cell_measurement_theta_max 25.682 _exptl_crystal_description prism _exptl_crystal_colour black _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.1 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.024 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.264 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8903 _exptl_absorpt_correction_T_max 0.9895 _exptl_absorpt_process_details ; ? ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(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 KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_detector_area_resol_mean 9 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22694 _diffrn_reflns_av_R_equivalents 0.1067 _diffrn_reflns_av_sigmaI/netI 0.1487 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 25.75 _reflns_number_total 7898 _reflns_number_gt 3802 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 19' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' _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^)+(0.1140P)^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 noref _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7898 _refine_ls_number_parameters 415 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1687 _refine_ls_R_factor_gt 0.0848 _refine_ls_wR_factor_ref 0.2292 _refine_ls_wR_factor_gt 0.1952 _refine_ls_goodness_of_fit_ref 0.945 _refine_ls_restrained_S_all 0.945 _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 C1 C 0.3184(4) 0.1353(2) 0.3809(3) 0.0392(12) Uani 1 1 d . . . C2 C 0.2288(4) 0.0908(2) 0.3551(3) 0.0430(13) Uani 1 1 d . . . C3 C 0.1759(4) 0.0944(3) 0.2791(3) 0.0502(14) Uani 1 1 d . . . H3 H 0.2256 0.1197 0.2521 0.060 Uiso 1 1 calc R . . C4 C 0.1511(5) 0.0170(3) 0.2445(4) 0.080(2) Uani 1 1 d . . . H4A H 0.1173 0.0236 0.1961 0.120 Uiso 1 1 calc R . . H4B H 0.1044 -0.0103 0.2706 0.120 Uiso 1 1 calc R . . H4C H 0.2161 -0.0107 0.2451 0.120 Uiso 1 1 calc R . . C5 C 0.0738(5) 0.1414(3) 0.2696(4) 0.0798(19) Uani 1 1 d . . . H5A H 0.0426 0.1417 0.2203 0.120 Uiso 1 1 calc R . . H5B H 0.0904 0.1922 0.2851 0.120 Uiso 1 1 calc R . . H5C H 0.0244 0.1200 0.2976 0.120 Uiso 1 1 calc R . . C6 C 0.1907(5) 0.0420(3) 0.4040(4) 0.0636(17) Uani 1 1 d . . . H6 H 0.1296 0.0137 0.3895 0.076 Uiso 1 1 calc R . . C7 C 0.2424(6) 0.0356(3) 0.4730(4) 0.0692(18) Uani 1 1 d . . . H7 H 0.2183 0.0011 0.5038 0.083 Uiso 1 1 calc R . . C8 C 0.3297(5) 0.0801(3) 0.4964(3) 0.0592(15) Uani 1 1 d . . . H8 H 0.3624 0.0762 0.5436 0.071 Uiso 1 1 calc R . . C9 C 0.3700(4) 0.1305(3) 0.4516(3) 0.0446(12) Uani 1 1 d . . . C10 C 0.4676(4) 0.1767(3) 0.4787(3) 0.0582(15) Uani 1 1 d . . . H10 H 0.4836 0.2090 0.4398 0.070 Uiso 1 1 calc R . . C11 C 0.5629(4) 0.1249(4) 0.5012(3) 0.079(2) Uani 1 1 d . . . H11A H 0.6243 0.1548 0.5189 0.119 Uiso 1 1 calc R . . H11B H 0.5769 0.0960 0.4609 0.119 Uiso 1 1 calc R . . H11C H 0.5474 0.0913 0.5380 0.119 Uiso 1 1 calc R . . C12 C 0.4469(5) 0.2280(4) 0.5413(3) 0.0794(19) Uani 1 1 d . . . H12A H 0.5097 0.2570 0.5577 0.119 Uiso 1 1 calc R . . H12B H 0.4295 0.1973 0.5796 0.119 Uiso 1 1 calc R . . H12C H 0.3887 0.2615 0.5253 0.119 Uiso 1 1 calc R . . C13 C 0.2616(4) 0.2920(3) 0.3695(3) 0.0472(13) Uani 1 1 d . . . H13A H 0.2539 0.2582 0.4079 0.071 Uiso 1 1 calc R . . H13B H 0.1925 0.3049 0.3444 0.071 Uiso 1 1 calc R . . H13C H 0.2974 0.3371 0.3883 0.071 Uiso 1 1 calc R . . C14 C 0.3255(3) 0.2545(2) 0.3193(3) 0.0382(11) Uani 1 1 d . . . C15 C 0.3443(4) 0.2962(2) 0.2592(3) 0.0392(11) Uani 1 1 d . . . H15 H 0.3269 0.3471 0.2608 0.047 Uiso 1 1 calc R . . C16 C 0.3845(3) 0.2746(2) 0.1974(2) 0.0374(11) Uani 1 1 d . . . C17 C 0.3688(5) 0.3300(3) 0.1357(3) 0.0603(15) Uani 1 1 d . . . H17A H 0.3982 0.3093 0.0962 0.090 Uiso 1 1 calc R . . H17B H 0.4040 0.3766 0.1503 0.090 Uiso 1 1 calc R . . H17C H 0.2941 0.3392 0.1216 0.090 Uiso 1 1 calc R . . C18 C 0.4686(4) 0.1854(2) 0.1257(2) 0.0356(11) Uani 1 1 d . . . C19 C 0.5639(4) 0.2142(3) 0.1082(3) 0.0465(12) Uani 1 1 d . . . C20 C 0.6328(4) 0.2705(3) 0.1537(3) 0.0515(14) Uani 1 1 d . . . H20 H 0.5952 0.2858 0.1928 0.062 Uiso 1 1 calc R . . C21 C 0.7381(5) 0.2327(4) 0.1865(3) 0.081(2) Uani 1 1 d . . . H21A H 0.7813 0.2685 0.2161 0.121 Uiso 1 1 calc R . . H21B H 0.7755 0.2159 0.1491 0.121 Uiso 1 1 calc R . . H21C H 0.7232 0.1903 0.2149 0.121 Uiso 1 1 calc R . . C22 C 0.6559(6) 0.3410(3) 0.1134(4) 0.087(2) Uani 1 1 d . . . H22A H 0.6995 0.3746 0.1451 0.130 Uiso 1 1 calc R . . H22B H 0.5901 0.3656 0.0950 0.130 Uiso 1 1 calc R . . H22C H 0.6927 0.3274 0.0747 0.130 Uiso 1 1 calc R . . C23 C 0.5990(4) 0.1863(3) 0.0462(3) 0.0543(14) Uani 1 1 d . . . H23 H 0.6618 0.2047 0.0332 0.065 Uiso 1 1 calc R . . C24 C 0.5425(5) 0.1329(3) 0.0050(3) 0.0599(15) Uani 1 1 d . . . H24 H 0.5665 0.1158 -0.0362 0.072 Uiso 1 1 calc R . . C25 C 0.4499(5) 0.1037(3) 0.0237(3) 0.0547(14) Uani 1 1 d . . . H25 H 0.4132 0.0664 -0.0044 0.066 Uiso 1 1 calc R . . C26 C 0.4105(4) 0.1294(3) 0.0841(3) 0.0431(12) Uani 1 1 d . . . C27 C 0.3074(4) 0.0979(3) 0.1031(3) 0.0489(13) Uani 1 1 d . . . H27 H 0.3130 0.0994 0.1552 0.059 Uiso 1 1 calc R . . C28 C 0.2112(5) 0.1472(3) 0.0725(4) 0.0766(18) Uani 1 1 d . . . H28A H 0.1475 0.1263 0.0859 0.115 Uiso 1 1 calc R . . H28B H 0.2049 0.1484 0.0214 0.115 Uiso 1 1 calc R . . H28C H 0.2214 0.1975 0.0909 0.115 Uiso 1 1 calc R . . C29 C 0.2853(5) 0.0159(3) 0.0798(4) 0.0727(18) Uani 1 1 d . . . H29A H 0.2199 -0.0006 0.0944 0.109 Uiso 1 1 calc R . . H29B H 0.3427 -0.0156 0.1016 0.109 Uiso 1 1 calc R . . H29C H 0.2794 0.0124 0.0289 0.109 Uiso 1 1 calc R . . C30 C 0.7017(4) 0.1660(3) 0.3571(2) 0.0378(11) Uani 1 1 d . . . C31 C 0.7592(4) 0.2211(3) 0.3986(3) 0.0498(13) Uani 1 1 d . . . H31 H 0.7289 0.2681 0.4042 0.060 Uiso 1 1 calc R . . C32 C 0.8627(5) 0.2056(3) 0.4318(3) 0.0597(15) Uani 1 1 d . . . H32 H 0.9008 0.2424 0.4599 0.072 Uiso 1 1 calc R . . C33 C 0.9089(4) 0.1368(3) 0.4236(3) 0.0577(15) Uani 1 1 d . . . H33 H 0.9779 0.1272 0.4462 0.069 Uiso 1 1 calc R . . C34 C 0.8539(4) 0.0827(3) 0.3825(3) 0.0596(15) Uani 1 1 d . . . H34 H 0.8858 0.0364 0.3764 0.072 Uiso 1 1 calc R . . C35 C 0.7498(4) 0.0964(3) 0.3496(3) 0.0476(13) Uani 1 1 d . . . H35 H 0.7123 0.0588 0.3223 0.057 Uiso 1 1 calc R . . C36 C 0.4971(3) -0.0154(2) 0.2494(2) 0.0359(11) Uani 1 1 d . . . C37 C 0.5610(4) -0.0330(3) 0.1972(3) 0.0481(13) Uani 1 1 d . . . H37 H 0.5922 0.0052 0.1739 0.058 Uiso 1 1 calc R . . C38 C 0.5769(4) -0.1079(3) 0.1810(3) 0.0592(15) Uani 1 1 d . . . H38 H 0.6177 -0.1197 0.1458 0.071 Uiso 1 1 calc R . . C39 C 0.5346(4) -0.1637(3) 0.2150(4) 0.0632(17) Uani 1 1 d . . . H39 H 0.5471 -0.2137 0.2037 0.076 Uiso 1 1 calc R . . C40 C 0.4722(5) -0.1474(3) 0.2672(3) 0.0617(16) Uani 1 1 d . . . H40 H 0.4431 -0.1864 0.2909 0.074 Uiso 1 1 calc R . . C41 C 0.4539(4) -0.0737(3) 0.2837(3) 0.0487(13) Uani 1 1 d . . . H41 H 0.4118 -0.0629 0.3185 0.058 Uiso 1 1 calc R . . N1 N 0.3597(3) 0.18343(19) 0.33008(19) 0.0332(9) Uani 1 1 d . . . N2 N 0.4329(3) 0.20855(18) 0.19107(19) 0.0322(9) Uani 1 1 d . . . N3 N 0.5989(3) 0.1801(2) 0.3239(2) 0.0407(10) Uani 1 1 d . . . N4 N 0.4724(3) 0.05930(19) 0.2614(2) 0.0395(10) Uani 1 1 d . . . V1 V 0.47826(6) 0.15172(4) 0.28062(4) 0.0347(3) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.041(3) 0.027(2) 0.053(3) -0.001(2) 0.019(3) 0.005(2) C2 0.043(3) 0.030(2) 0.059(4) -0.004(2) 0.020(3) 0.007(2) C3 0.048(3) 0.038(3) 0.067(4) -0.005(2) 0.015(3) -0.009(2) C4 0.074(4) 0.050(3) 0.109(6) -0.021(3) -0.007(4) -0.001(3) C5 0.096(5) 0.060(4) 0.083(5) 0.005(3) 0.011(4) 0.018(3) C6 0.073(4) 0.039(3) 0.090(5) 0.005(3) 0.046(4) -0.008(3) C7 0.094(5) 0.050(3) 0.074(5) 0.015(3) 0.047(4) 0.008(3) C8 0.069(4) 0.056(3) 0.057(4) 0.017(3) 0.026(3) 0.012(3) C9 0.049(3) 0.045(3) 0.041(3) 0.008(2) 0.012(3) 0.010(2) C10 0.056(4) 0.076(4) 0.045(4) -0.003(3) 0.018(3) 0.000(3) C11 0.051(4) 0.125(5) 0.063(4) 0.030(4) 0.012(3) 0.019(4) C12 0.071(4) 0.113(5) 0.052(4) -0.012(4) 0.002(3) -0.017(4) C13 0.047(3) 0.044(3) 0.052(3) 0.005(2) 0.013(3) 0.006(2) C14 0.036(3) 0.032(2) 0.049(3) -0.005(2) 0.013(2) 0.001(2) C15 0.045(3) 0.024(2) 0.046(3) -0.002(2) 0.001(2) 0.001(2) C16 0.041(3) 0.033(2) 0.037(3) 0.001(2) 0.002(2) -0.005(2) C17 0.079(4) 0.047(3) 0.058(4) 0.012(3) 0.021(3) 0.013(3) C18 0.039(3) 0.035(2) 0.033(3) -0.001(2) 0.004(2) 0.007(2) C19 0.056(3) 0.045(3) 0.039(3) -0.001(2) 0.010(3) 0.004(2) C20 0.055(3) 0.063(3) 0.038(3) -0.002(3) 0.014(3) -0.017(3) C21 0.059(4) 0.133(6) 0.050(4) -0.007(4) 0.008(3) -0.033(4) C22 0.107(5) 0.082(4) 0.079(5) -0.009(4) 0.038(4) -0.041(4) C23 0.058(3) 0.064(3) 0.046(4) 0.001(3) 0.022(3) 0.009(3) C24 0.062(4) 0.078(4) 0.039(3) -0.013(3) 0.007(3) 0.010(3) C25 0.071(4) 0.053(3) 0.038(3) -0.017(2) 0.003(3) 0.003(3) C26 0.051(3) 0.040(3) 0.035(3) -0.002(2) -0.002(2) 0.010(2) C27 0.049(3) 0.045(3) 0.050(4) -0.006(2) -0.001(3) -0.005(2) C28 0.059(4) 0.060(4) 0.107(6) -0.002(3) 0.000(4) 0.004(3) C29 0.075(4) 0.043(3) 0.095(5) -0.014(3) -0.001(4) -0.005(3) C30 0.037(3) 0.044(3) 0.033(3) 0.005(2) 0.007(2) -0.003(2) C31 0.051(3) 0.047(3) 0.051(3) 0.000(3) 0.003(3) -0.001(2) C32 0.057(4) 0.068(4) 0.050(4) -0.006(3) -0.003(3) -0.017(3) C33 0.038(3) 0.086(4) 0.045(4) 0.002(3) -0.007(3) 0.008(3) C34 0.056(4) 0.064(4) 0.060(4) 0.007(3) 0.012(3) 0.014(3) C35 0.044(3) 0.048(3) 0.050(4) 0.003(2) 0.006(3) 0.003(2) C36 0.031(2) 0.036(3) 0.037(3) -0.001(2) -0.007(2) 0.003(2) C37 0.051(3) 0.050(3) 0.044(3) -0.005(2) 0.010(3) 0.005(2) C38 0.048(3) 0.063(4) 0.065(4) -0.026(3) 0.004(3) 0.007(3) C39 0.056(4) 0.035(3) 0.091(5) -0.008(3) -0.012(3) 0.004(3) C40 0.069(4) 0.038(3) 0.071(4) 0.010(3) -0.014(3) -0.012(3) C41 0.053(3) 0.043(3) 0.050(3) 0.005(2) 0.005(3) -0.002(2) N1 0.035(2) 0.0318(19) 0.033(2) 0.0004(16) 0.0077(17) 0.0019(17) N2 0.035(2) 0.0274(19) 0.033(2) 0.0018(16) 0.0021(17) 0.0010(16) N3 0.042(2) 0.043(2) 0.037(2) -0.0032(18) 0.0087(19) -0.0024(18) N4 0.045(2) 0.031(2) 0.044(3) 0.0025(16) 0.010(2) 0.0041(17) V1 0.0364(5) 0.0310(4) 0.0376(5) 0.0000(3) 0.0089(3) 0.0023(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.410(7) . ? C1 C9 1.402(7) . ? C1 N1 1.445(6) . ? C2 C6 1.407(7) . ? C2 C3 1.496(7) . ? C3 C5 1.529(7) . ? C3 C4 1.532(7) . ? C3 H3 0.9800 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 C7 1.376(9) . ? C6 H6 0.9300 . ? C7 C8 1.379(8) . ? C7 H7 0.9300 . ? C8 C9 1.384(7) . ? C8 H8 0.9300 . ? C9 C10 1.509(7) . ? C10 C11 1.528(8) . ? C10 C12 1.549(7) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 C14 1.497(6) . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 N1 1.338(5) . ? C14 C15 1.409(6) . ? C15 C16 1.402(6) . ? C15 H15 0.9300 . ? C16 N2 1.336(5) . ? C16 C17 1.518(6) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 C19 1.399(6) . ? C18 C26 1.406(6) . ? C18 N2 1.444(5) . ? C19 C23 1.411(7) . ? C19 C20 1.509(7) . ? C20 C22 1.516(7) . ? C20 C21 1.540(8) . ? C20 H20 0.9800 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C22 H22C 0.9600 . ? C23 C24 1.361(7) . ? C23 H23 0.9300 . ? C24 C25 1.379(7) . ? C24 H24 0.9300 . ? C25 C26 1.396(7) . ? C25 H25 0.9300 . ? C26 C27 1.516(7) . ? C27 C29 1.533(6) . ? C27 C28 1.542(7) . ? C27 H27 0.9800 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 N3 1.384(6) . ? C30 C31 1.390(6) . ? C30 C35 1.393(6) . ? C31 C32 1.396(7) . ? C31 H31 0.9300 . ? C32 C33 1.371(7) . ? C32 H32 0.9300 . ? C33 C34 1.360(7) . ? C33 H33 0.9300 . ? C34 C35 1.395(7) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 C41 1.380(6) . ? C36 N4 1.387(5) . ? C36 C37 1.409(6) . ? C37 C38 1.383(7) . ? C37 H37 0.9300 . ? C38 C39 1.338(8) . ? C38 H38 0.9300 . ? C39 C40 1.390(8) . ? C39 H39 0.9300 . ? C40 C41 1.371(7) . ? C40 H40 0.9300 . ? C41 H41 0.9300 . ? N1 V1 1.974(3) . ? N2 V1 1.984(3) . ? N3 V1 1.701(4) . ? N4 V1 1.677(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 C2 C1 C9 122.2(4) . . ? C2 C1 N1 117.0(4) . . ? C9 C1 N1 120.6(4) . . ? C1 C2 C6 117.0(5) . . ? C1 C2 C3 122.1(4) . . ? C6 C2 C3 120.9(5) . . ? C2 C3 C5 112.6(4) . . ? C2 C3 C4 114.0(4) . . ? C5 C3 C4 108.8(5) . . ? C2 C3 H3 107.0 . . ? C5 C3 H3 107.0 . . ? C4 C3 H3 107.0 . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C2 121.1(6) . . ? C7 C6 H6 119.5 . . ? C2 C6 H6 119.5 . . ? C8 C7 C6 120.2(5) . . ? C8 C7 H7 119.9 . . ? C6 C7 H7 119.9 . . ? C7 C8 C9 121.7(6) . . ? C7 C8 H8 119.2 . . ? C9 C8 H8 119.2 . . ? C8 C9 C1 117.7(5) . . ? C8 C9 C10 120.1(5) . . ? C1 C9 C10 122.2(4) . . ? C9 C10 C11 110.1(5) . . ? C9 C10 C12 110.7(4) . . ? C11 C10 C12 111.0(5) . . ? C9 C10 H10 108.3 . . ? C11 C10 H10 108.3 . . ? C12 C10 H10 108.3 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 H13A 109.5 . . ? C14 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C14 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N1 C14 C15 121.7(4) . . ? N1 C14 C13 121.1(4) . . ? C15 C14 C13 117.2(4) . . ? C16 C15 C14 131.5(4) . . ? C16 C15 H15 114.3 . . ? C14 C15 H15 114.3 . . ? N2 C16 C15 123.1(4) . . ? N2 C16 C17 120.4(4) . . ? C15 C16 C17 116.5(4) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C26 121.6(4) . . ? C19 C18 N2 119.8(4) . . ? C26 C18 N2 118.4(4) . . ? C18 C19 C23 117.7(5) . . ? C18 C19 C20 123.6(4) . . ? C23 C19 C20 118.6(5) . . ? C19 C20 C22 113.4(5) . . ? C19 C20 C21 109.6(4) . . ? C22 C20 C21 109.8(5) . . ? C19 C20 H20 107.9 . . ? C22 C20 H20 107.9 . . ? C21 C20 H20 107.9 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C19 121.2(5) . . ? C24 C23 H23 119.4 . . ? C19 C23 H23 119.4 . . ? C23 C24 C25 120.5(5) . . ? C23 C24 H24 119.7 . . ? C25 C24 H24 119.7 . . ? C24 C25 C26 121.1(5) . . ? C24 C25 H25 119.4 . . ? C26 C25 H25 119.4 . . ? C25 C26 C18 117.8(5) . . ? C25 C26 C27 120.5(4) . . ? C18 C26 C27 121.7(4) . . ? C26 C27 C29 114.0(4) . . ? C26 C27 C28 111.4(4) . . ? C29 C27 C28 109.1(4) . . ? C26 C27 H27 107.3 . . ? C29 C27 H27 107.3 . . ? C28 C27 H27 107.3 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N3 C30 C31 120.7(4) . . ? N3 C30 C35 120.8(4) . . ? C31 C30 C35 118.6(4) . . ? C30 C31 C32 119.7(5) . . ? C30 C31 H31 120.2 . . ? C32 C31 H31 120.2 . . ? C33 C32 C31 120.9(5) . . ? C33 C32 H32 119.5 . . ? C31 C32 H32 119.5 . . ? C34 C33 C32 120.0(5) . . ? C34 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C33 C34 C35 120.2(5) . . ? C33 C34 H34 119.9 . . ? C35 C34 H34 119.9 . . ? C30 C35 C34 120.6(5) . . ? C30 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C41 C36 N4 121.4(4) . . ? C41 C36 C37 118.7(4) . . ? N4 C36 C37 119.7(4) . . ? C38 C37 C36 119.2(5) . . ? C38 C37 H37 120.4 . . ? C36 C37 H37 120.4 . . ? C39 C38 C37 121.3(5) . . ? C39 C38 H38 119.4 . . ? C37 C38 H38 119.4 . . ? C38 C39 C40 120.4(5) . . ? C38 C39 H39 119.8 . . ? C40 C39 H39 119.8 . . ? C41 C40 C39 119.7(5) . . ? C41 C40 H40 120.1 . . ? C39 C40 H40 120.1 . . ? C40 C41 C36 120.8(5) . . ? C40 C41 H41 119.6 . . ? C36 C41 H41 119.6 . . ? C14 N1 C1 121.0(3) . . ? C14 N1 V1 116.7(3) . . ? C1 N1 V1 122.0(3) . . ? C16 N2 C18 122.4(4) . . ? C16 N2 V1 116.4(3) . . ? C18 N2 V1 120.2(3) . . ? C30 N3 V1 152.3(3) . . ? C36 N4 V1 164.6(3) . . ? N4 V1 N3 113.62(18) . . ? N4 V1 N1 111.70(16) . . ? N3 V1 N1 112.54(16) . . ? N4 V1 N2 108.17(17) . . ? N3 V1 N2 112.70(16) . . ? N1 V1 N2 96.86(14) . . ? _diffrn_measured_fraction_theta_max 0.977 _diffrn_reflns_theta_full 25.75 _diffrn_measured_fraction_theta_full 0.977 _refine_diff_density_max 0.351 _refine_diff_density_min -0.393 _refine_diff_density_rms 0.096