# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_4b(CCDC-925607) _database_code_depnum_ccdc_archive 'CCDC 925607' #TrackingRef 'MoriuchiCIFCCDC925607_925609.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C20 H18 N3 O3 V' _chemical_formula_sum 'C20 H18 N3 O3 V' _chemical_formula_weight 399.31 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 16.2235(5) _cell_length_b 11.8240(3) _cell_length_c 18.6632(5) _cell_angle_alpha 90.00 _cell_angle_beta 96.4640(10) _cell_angle_gamma 90.00 _cell_volume 3557.32(18) _cell_formula_units_Z 8 _cell_measurement_temperature 103(2) _cell_measurement_reflns_used 24935 _cell_measurement_theta_min 3.06 _cell_measurement_theta_max 27.47 _exptl_crystal_description platelet _exptl_crystal_colour brown _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.491 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 0.584 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8677 _exptl_absorpt_correction_T_max 0.9827 _exptl_absorpt_process_details ; Higashi, T. (1999). Abscor - Empirical Absorption Correction based on Fourier Series Approximation. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 103(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'imaging plate' _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 34302 _diffrn_reflns_av_R_equivalents 0.0522 _diffrn_reflns_av_sigmaI/netI 0.0456 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.06 _diffrn_reflns_theta_max 27.46 _reflns_number_total 8108 _reflns_number_gt 6147 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rigaku/RAPID Diffractometer Control' _computing_cell_refinement 'Rigaku/RAPID Diffractometer Control' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 and modified' _computing_molecular_graphics ? _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^)+(0.0584P)^2^+1.6937P] 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 8108 _refine_ls_number_parameters 487 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0673 _refine_ls_R_factor_gt 0.0464 _refine_ls_wR_factor_ref 0.1167 _refine_ls_wR_factor_gt 0.1072 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.82204(2) 0.43281(3) 0.383424(19) 0.01544(10) Uani 1 1 d . . . V2 V 0.33808(2) 0.00620(3) 0.386760(19) 0.01571(10) Uani 1 1 d . . . O1 O 0.86573(10) 0.31657(13) 0.44405(8) 0.0219(4) Uani 1 1 d . . . O2 O 0.70836(10) 0.45569(13) 0.37592(9) 0.0212(3) Uani 1 1 d . . . O3 O 0.87866(10) 0.46521(12) 0.30498(8) 0.0187(3) Uani 1 1 d . . . O4 O 0.22544(10) -0.02289(13) 0.38557(9) 0.0226(4) Uani 1 1 d . . . O5 O 0.38784(10) 0.12657(13) 0.43868(8) 0.0202(3) Uani 1 1 d . . . O6 O 0.37716(10) -0.03948(13) 0.30155(9) 0.0228(4) Uani 1 1 d . . . N1 N 0.78035(11) 0.28222(14) 0.31256(9) 0.0146(4) Uani 1 1 d . . . N2 N 0.85121(12) 0.54453(15) 0.43674(10) 0.0192(4) Uani 1 1 d . . . N3 N 0.87051(12) 0.62888(16) 0.48040(11) 0.0226(4) Uani 1 1 d . . . N4 N 0.28781(11) 0.15195(14) 0.31483(9) 0.0145(4) Uani 1 1 d . . . N5 N 0.37145(12) -0.09997(16) 0.44278(10) 0.0192(4) Uani 1 1 d . . . N6 N 0.39501(12) -0.17494(15) 0.49272(10) 0.0188(4) Uani 1 1 d . . . C1 C 0.80629(13) 0.18269(18) 0.35664(12) 0.0155(4) Uani 1 1 d . . . C2 C 0.85068(14) 0.20762(18) 0.42335(12) 0.0178(4) Uani 1 1 d . . . C3 C 0.87882(16) 0.11917(19) 0.46886(12) 0.0240(5) Uani 1 1 d . . . H3 H 0.9100 0.1350 0.5139 0.029 Uiso 1 1 calc R . . C4 C 0.86164(16) 0.00800(19) 0.44875(13) 0.0260(5) Uani 1 1 d . . . H4 H 0.8807 -0.0519 0.4803 0.031 Uiso 1 1 calc R . . C5 C 0.81679(16) -0.01606(19) 0.38292(13) 0.0250(5) Uani 1 1 d . . . H5 H 0.8051 -0.0923 0.3693 0.030 Uiso 1 1 calc R . . C6 C 0.78900(14) 0.07109(19) 0.33695(13) 0.0212(5) Uani 1 1 d . . . H6 H 0.7581 0.0546 0.2919 0.025 Uiso 1 1 calc R . . C7 C 0.68995(13) 0.29627(18) 0.29687(12) 0.0172(4) Uani 1 1 d . . . C8 C 0.65741(14) 0.38862(18) 0.33133(12) 0.0185(5) Uani 1 1 d . . . C9 C 0.57245(15) 0.4107(2) 0.32053(13) 0.0237(5) Uani 1 1 d . . . H9 H 0.5500 0.4736 0.3434 0.028 Uiso 1 1 calc R . . C10 C 0.52094(15) 0.3399(2) 0.27610(14) 0.0262(5) Uani 1 1 d . . . H10 H 0.4630 0.3546 0.2688 0.031 Uiso 1 1 calc R . . C11 C 0.55290(15) 0.2482(2) 0.24228(13) 0.0256(5) Uani 1 1 d . . . H11 H 0.5170 0.2001 0.2122 0.031 Uiso 1 1 calc R . . C12 C 0.63786(15) 0.22669(19) 0.25246(13) 0.0214(5) Uani 1 1 d . . . H12 H 0.6601 0.1643 0.2290 0.026 Uiso 1 1 calc R . . C13 C 0.82512(13) 0.29474(18) 0.24876(11) 0.0156(4) Uani 1 1 d . . . C14 C 0.87341(13) 0.39286(18) 0.24798(11) 0.0157(4) Uani 1 1 d . . . C15 C 0.91691(14) 0.41534(19) 0.18929(12) 0.0202(5) Uani 1 1 d . . . H15 H 0.9494 0.4821 0.1884 0.024 Uiso 1 1 calc R . . C16 C 0.91248(15) 0.3397(2) 0.13230(12) 0.0238(5) Uani 1 1 d . . . H16 H 0.9416 0.3551 0.0920 0.029 Uiso 1 1 calc R . . C17 C 0.86553(16) 0.2409(2) 0.13375(13) 0.0249(5) Uani 1 1 d . . . H17 H 0.8633 0.1889 0.0948 0.030 Uiso 1 1 calc R . . C18 C 0.82218(15) 0.21877(19) 0.19210(12) 0.0211(5) Uani 1 1 d . . . H18 H 0.7904 0.1514 0.1932 0.025 Uiso 1 1 calc R . . C19 C 0.80598(17) 0.6798(2) 0.51782(15) 0.0346(6) Uani 1 1 d . . . H19A H 0.7826 0.6225 0.5477 0.042 Uiso 1 1 calc R . . H19B H 0.7621 0.7096 0.4825 0.042 Uiso 1 1 calc R . . H19C H 0.8297 0.7415 0.5485 0.042 Uiso 1 1 calc R . . C20 C 0.9416(2) 0.6978(3) 0.4702(2) 0.0622(11) Uani 1 1 d . . . H20A H 0.9337 0.7327 0.4223 0.075 Uiso 1 1 calc R . . H20B H 0.9915 0.6504 0.4742 0.075 Uiso 1 1 calc R . . H20C H 0.9480 0.7570 0.5071 0.075 Uiso 1 1 calc R . . C21 C 0.19714(13) 0.14016(18) 0.31079(11) 0.0166(4) Uani 1 1 d . . . C22 C 0.16988(14) 0.04834(18) 0.34928(12) 0.0188(5) Uani 1 1 d . . . C23 C 0.08492(14) 0.0301(2) 0.34992(13) 0.0235(5) Uani 1 1 d . . . H23 H 0.0660 -0.0317 0.3761 0.028 Uiso 1 1 calc R . . C24 C 0.02843(14) 0.1019(2) 0.31247(13) 0.0243(5) Uani 1 1 d . . . H24 H -0.0293 0.0899 0.3136 0.029 Uiso 1 1 calc R . . C25 C 0.05560(15) 0.1915(2) 0.27319(14) 0.0251(5) Uani 1 1 d . . . H25 H 0.0165 0.2401 0.2469 0.030 Uiso 1 1 calc R . . C26 C 0.14011(14) 0.21025(19) 0.27234(13) 0.0205(5) Uani 1 1 d . . . H26 H 0.1587 0.2714 0.2453 0.025 Uiso 1 1 calc R . . C27 C 0.32233(13) 0.25447(18) 0.35134(12) 0.0158(4) Uani 1 1 d . . . C28 C 0.37573(13) 0.23402(18) 0.41418(12) 0.0164(4) Uani 1 1 d . . . C29 C 0.41612(14) 0.32392(19) 0.45134(12) 0.0199(5) Uani 1 1 d . . . H29 H 0.4536 0.3103 0.4933 0.024 Uiso 1 1 calc R . . C30 C 0.40128(14) 0.43376(19) 0.42656(13) 0.0221(5) Uani 1 1 d . . . H30 H 0.4288 0.4953 0.4517 0.027 Uiso 1 1 calc R . . C31 C 0.34646(15) 0.45413(19) 0.36519(13) 0.0235(5) Uani 1 1 d . . . H31 H 0.3360 0.5295 0.3490 0.028 Uiso 1 1 calc R . . C32 C 0.30704(14) 0.36460(19) 0.32760(12) 0.0203(5) Uani 1 1 d . . . H32 H 0.2696 0.3786 0.2856 0.024 Uiso 1 1 calc R . . C33 C 0.32131(13) 0.13086(18) 0.24564(11) 0.0157(4) Uani 1 1 d . . . C34 C 0.36634(13) 0.03002(18) 0.24304(12) 0.0180(4) Uani 1 1 d . . . C35 C 0.39945(14) 0.00064(19) 0.17972(13) 0.0225(5) Uani 1 1 d . . . H35 H 0.4303 -0.0673 0.1775 0.027 Uiso 1 1 calc R . . C36 C 0.38710(15) 0.0709(2) 0.12037(12) 0.0240(5) Uani 1 1 d . . . H36 H 0.4085 0.0500 0.0769 0.029 Uiso 1 1 calc R . . C37 C 0.34369(15) 0.1720(2) 0.12349(12) 0.0247(5) Uani 1 1 d . . . H37 H 0.3366 0.2205 0.0827 0.030 Uiso 1 1 calc R . . C38 C 0.31077(14) 0.2018(2) 0.18651(12) 0.0215(5) Uani 1 1 d . . . H38 H 0.2811 0.2707 0.1889 0.026 Uiso 1 1 calc R . . C39 C 0.41257(15) -0.1280(2) 0.56550(12) 0.0237(5) Uani 1 1 d . . . H39A H 0.3625 -0.0916 0.5795 0.028 Uiso 1 1 calc R . . H39B H 0.4572 -0.0720 0.5661 0.028 Uiso 1 1 calc R . . H39C H 0.4297 -0.1890 0.5995 0.028 Uiso 1 1 calc R . . C40 C 0.34953(17) -0.28263(19) 0.48739(14) 0.0281(6) Uani 1 1 d . . . H40A H 0.3562 -0.3188 0.4411 0.034 Uiso 1 1 calc R . . H40B H 0.2905 -0.2684 0.4905 0.034 Uiso 1 1 calc R . . H40C H 0.3715 -0.3325 0.5269 0.034 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 0.0183(2) 0.01315(18) 0.01473(19) -0.00062(15) 0.00148(14) -0.00060(13) V2 0.01576(19) 0.01571(19) 0.01536(19) 0.00096(15) 0.00041(14) 0.00141(14) O1 0.0321(10) 0.0149(7) 0.0170(8) -0.0014(7) -0.0040(7) -0.0016(6) O2 0.0207(9) 0.0168(8) 0.0263(9) -0.0038(7) 0.0032(7) 0.0018(6) O3 0.0232(8) 0.0165(7) 0.0166(8) -0.0012(6) 0.0031(6) -0.0050(6) O4 0.0173(8) 0.0242(8) 0.0258(9) 0.0076(7) 0.0002(7) -0.0017(6) O5 0.0215(8) 0.0185(8) 0.0192(8) 0.0020(7) -0.0035(6) 0.0009(6) O6 0.0294(9) 0.0183(8) 0.0216(8) 0.0009(7) 0.0065(7) 0.0075(7) N1 0.0152(9) 0.0141(9) 0.0142(8) 0.0013(7) 0.0009(7) 0.0004(7) N2 0.0235(10) 0.0179(9) 0.0163(9) -0.0002(8) 0.0029(8) -0.0013(7) N3 0.0230(11) 0.0203(10) 0.0251(10) -0.0108(9) 0.0046(8) -0.0043(8) N4 0.0141(9) 0.0146(9) 0.0149(9) -0.0020(7) 0.0014(7) 0.0007(7) N5 0.0185(10) 0.0187(9) 0.0201(9) 0.0015(8) 0.0002(8) 0.0017(7) N6 0.0217(10) 0.0163(9) 0.0176(9) 0.0013(8) -0.0008(8) 0.0036(7) C1 0.0130(10) 0.0153(10) 0.0182(10) 0.0012(9) 0.0024(8) 0.0015(8) C2 0.0219(12) 0.0142(10) 0.0177(11) -0.0004(9) 0.0037(9) 0.0006(8) C3 0.0317(14) 0.0216(12) 0.0175(11) 0.0006(10) -0.0023(10) 0.0013(10) C4 0.0360(14) 0.0167(11) 0.0248(12) 0.0052(10) 0.0007(10) 0.0032(10) C5 0.0335(14) 0.0133(11) 0.0275(13) 0.0006(10) 0.0002(10) -0.0034(9) C6 0.0214(12) 0.0200(11) 0.0212(11) -0.0007(10) -0.0019(9) -0.0022(9) C7 0.0143(11) 0.0178(10) 0.0188(11) 0.0038(9) -0.0008(8) -0.0006(8) C8 0.0188(11) 0.0155(10) 0.0215(11) 0.0052(9) 0.0031(9) -0.0008(8) C9 0.0210(12) 0.0215(11) 0.0293(13) 0.0064(10) 0.0057(10) 0.0046(9) C10 0.0150(12) 0.0287(12) 0.0345(13) 0.0113(11) 0.0005(10) 0.0017(9) C11 0.0197(12) 0.0278(12) 0.0275(13) 0.0042(11) -0.0053(10) -0.0047(9) C12 0.0226(12) 0.0182(11) 0.0228(12) 0.0009(10) -0.0007(9) -0.0007(9) C13 0.0154(11) 0.0173(10) 0.0136(10) 0.0017(9) 0.0001(8) 0.0009(8) C14 0.0168(11) 0.0156(10) 0.0139(10) 0.0011(9) -0.0024(8) 0.0022(8) C15 0.0215(12) 0.0183(11) 0.0209(11) 0.0065(10) 0.0031(9) 0.0009(9) C16 0.0285(13) 0.0260(12) 0.0178(11) 0.0050(10) 0.0069(10) 0.0048(10) C17 0.0332(14) 0.0229(12) 0.0190(11) -0.0024(10) 0.0048(10) 0.0027(10) C18 0.0242(12) 0.0164(11) 0.0221(12) -0.0011(10) 0.0005(9) -0.0008(9) C19 0.0339(15) 0.0344(14) 0.0382(15) -0.0141(13) 0.0158(12) -0.0004(11) C20 0.0300(17) 0.0421(17) 0.119(3) -0.039(2) 0.0285(19) -0.0138(14) C21 0.0149(11) 0.0187(11) 0.0161(10) -0.0039(9) 0.0011(8) -0.0001(8) C22 0.0185(11) 0.0195(11) 0.0176(11) -0.0005(9) -0.0006(9) 0.0027(8) C23 0.0198(12) 0.0276(12) 0.0231(12) 0.0019(10) 0.0024(9) -0.0047(9) C24 0.0144(11) 0.0295(12) 0.0286(12) -0.0067(11) 0.0008(9) -0.0009(9) C25 0.0179(12) 0.0247(12) 0.0314(13) -0.0037(11) -0.0037(10) 0.0048(9) C26 0.0193(12) 0.0173(11) 0.0241(12) 0.0016(10) -0.0018(9) 0.0008(8) C27 0.0128(10) 0.0172(10) 0.0177(11) -0.0018(9) 0.0026(8) 0.0015(8) C28 0.0165(11) 0.0176(10) 0.0154(10) -0.0005(9) 0.0033(8) 0.0027(8) C29 0.0167(11) 0.0243(12) 0.0181(11) -0.0012(10) -0.0006(9) 0.0005(9) C30 0.0207(12) 0.0184(11) 0.0271(12) -0.0079(10) 0.0025(9) -0.0009(9) C31 0.0240(12) 0.0160(11) 0.0300(13) -0.0004(10) 0.0011(10) 0.0019(9) C32 0.0191(12) 0.0209(11) 0.0210(11) 0.0018(10) 0.0018(9) 0.0016(9) C33 0.0155(11) 0.0189(11) 0.0128(10) -0.0018(9) 0.0017(8) -0.0023(8) C34 0.0172(11) 0.0182(11) 0.0184(11) -0.0017(9) 0.0016(8) -0.0028(8) C35 0.0223(12) 0.0215(11) 0.0249(12) -0.0071(10) 0.0081(9) -0.0033(9) C36 0.0248(12) 0.0318(13) 0.0168(11) -0.0081(10) 0.0078(9) -0.0118(10) C37 0.0263(13) 0.0317(13) 0.0159(11) 0.0034(10) 0.0008(9) -0.0070(10) C38 0.0223(12) 0.0207(11) 0.0208(11) 0.0008(10) -0.0004(9) -0.0002(9) C39 0.0268(13) 0.0257(12) 0.0184(11) -0.0018(10) 0.0021(9) 0.0023(10) C40 0.0365(15) 0.0188(12) 0.0279(13) 0.0004(11) -0.0011(11) -0.0035(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 N2 1.6891(19) . ? V1 O2 1.8536(16) . ? V1 O3 1.8538(15) . ? V1 O1 1.8685(16) . ? V1 N1 2.2751(18) . ? V2 N5 1.6837(19) . ? V2 O5 1.8548(16) . ? V2 O4 1.8572(16) . ? V2 O6 1.8574(16) . ? V2 N4 2.2782(18) . ? O1 C2 1.359(3) . ? O2 C8 1.360(3) . ? O3 C14 1.360(3) . ? O4 C22 1.358(3) . ? O5 C28 1.357(3) . ? O6 C34 1.362(3) . ? N1 C1 1.470(3) . ? N1 C13 1.470(3) . ? N1 C7 1.472(3) . ? N2 N3 1.304(3) . ? N3 C20 1.443(3) . ? N3 C19 1.453(3) . ? N4 C27 1.470(3) . ? N4 C21 1.471(3) . ? N4 C33 1.477(3) . ? N5 N6 1.312(3) . ? N6 C39 1.465(3) . ? N6 C40 1.469(3) . ? C1 C6 1.390(3) . ? C1 C2 1.398(3) . ? C2 C3 1.391(3) . ? C3 C4 1.387(3) . ? C3 H3 0.9500 . ? C4 C5 1.385(3) . ? C4 H4 0.9500 . ? C5 C6 1.383(3) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.386(3) . ? C7 C8 1.400(3) . ? C8 C9 1.395(3) . ? C9 C10 1.389(3) . ? C9 H9 0.9500 . ? C10 C11 1.384(4) . ? C10 H10 0.9500 . ? C11 C12 1.393(3) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.384(3) . ? C13 C14 1.401(3) . ? C14 C15 1.394(3) . ? C15 C16 1.385(3) . ? C15 H15 0.9500 . ? C16 C17 1.396(3) . ? C16 H16 0.9500 . ? C17 C18 1.386(3) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C26 1.381(3) . ? C21 C22 1.401(3) . ? C22 C23 1.396(3) . ? C23 C24 1.380(3) . ? C23 H23 0.9500 . ? C24 C25 1.389(3) . ? C24 H24 0.9500 . ? C25 C26 1.391(3) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.389(3) . ? C27 C28 1.398(3) . ? C28 C29 1.392(3) . ? C29 C30 1.391(3) . ? C29 H29 0.9500 . ? C30 C31 1.390(3) . ? C30 H30 0.9500 . ? C31 C32 1.386(3) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C38 1.381(3) . ? C33 C34 1.402(3) . ? C34 C35 1.396(3) . ? C35 C36 1.381(3) . ? C35 H35 0.9500 . ? C36 C37 1.392(4) . ? C36 H36 0.9500 . ? C37 C38 1.391(3) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 V1 O2 98.09(8) . . ? N2 V1 O3 99.95(8) . . ? O2 V1 O3 119.17(7) . . ? N2 V1 O1 99.00(8) . . ? O2 V1 O1 117.35(7) . . ? O3 V1 O1 116.25(7) . . ? N2 V1 N1 178.88(8) . . ? O2 V1 N1 80.92(7) . . ? O3 V1 N1 81.02(6) . . ? O1 V1 N1 81.03(7) . . ? N5 V2 O5 99.04(8) . . ? N5 V2 O4 96.69(8) . . ? O5 V2 O4 121.21(7) . . ? N5 V2 O6 101.42(8) . . ? O5 V2 O6 120.00(7) . . ? O4 V2 O6 111.48(8) . . ? N5 V2 N4 177.02(8) . . ? O5 V2 N4 80.40(7) . . ? O4 V2 N4 81.18(7) . . ? O6 V2 N4 81.35(6) . . ? C2 O1 V1 118.77(14) . . ? C8 O2 V1 119.48(13) . . ? C14 O3 V1 119.65(13) . . ? C22 O4 V2 119.22(14) . . ? C28 O5 V2 120.29(14) . . ? C34 O6 V2 119.04(13) . . ? C1 N1 C13 113.42(16) . . ? C1 N1 C7 114.69(16) . . ? C13 N1 C7 113.55(16) . . ? C1 N1 V1 104.69(12) . . ? C13 N1 V1 104.49(12) . . ? C7 N1 V1 104.57(12) . . ? N3 N2 V1 176.60(17) . . ? N2 N3 C20 119.3(2) . . ? N2 N3 C19 118.8(2) . . ? C20 N3 C19 117.4(2) . . ? C27 N4 C21 115.37(16) . . ? C27 N4 C33 112.70(16) . . ? C21 N4 C33 113.78(16) . . ? C27 N4 V2 104.97(12) . . ? C21 N4 V2 104.36(12) . . ? C33 N4 V2 104.17(12) . . ? N6 N5 V2 173.11(16) . . ? N5 N6 C39 114.43(18) . . ? N5 N6 C40 115.70(19) . . ? C39 N6 C40 115.76(19) . . ? C6 C1 C2 120.3(2) . . ? C6 C1 N1 125.1(2) . . ? C2 C1 N1 114.58(18) . . ? O1 C2 C3 120.2(2) . . ? O1 C2 C1 120.74(19) . . ? C3 C2 C1 119.1(2) . . ? C4 C3 C2 120.3(2) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C5 C4 C3 120.3(2) . . ? C5 C4 H4 119.9 . . ? C3 C4 H4 119.9 . . ? C6 C5 C4 119.9(2) . . ? C6 C5 H5 120.0 . . ? C4 C5 H5 120.0 . . ? C5 C6 C1 120.1(2) . . ? C5 C6 H6 120.0 . . ? C1 C6 H6 120.0 . . ? C12 C7 C8 120.1(2) . . ? C12 C7 N1 125.36(19) . . ? C8 C7 N1 114.54(19) . . ? O2 C8 C9 120.1(2) . . ? O2 C8 C7 120.07(19) . . ? C9 C8 C7 119.8(2) . . ? C10 C9 C8 119.5(2) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C11 C10 C9 120.9(2) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 119.8(2) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C7 C12 C11 120.0(2) . . ? C7 C12 H12 120.0 . . ? C11 C12 H12 120.0 . . ? C18 C13 C14 120.0(2) . . ? C18 C13 N1 125.14(19) . . ? C14 C13 N1 114.82(18) . . ? O3 C14 C15 120.13(19) . . ? O3 C14 C13 119.90(19) . . ? C15 C14 C13 120.0(2) . . ? C16 C15 C14 119.5(2) . . ? C16 C15 H15 120.2 . . ? C14 C15 H15 120.2 . . ? C15 C16 C17 120.4(2) . . ? C15 C16 H16 119.8 . . ? C17 C16 H16 119.8 . . ? C18 C17 C16 120.0(2) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C13 C18 C17 120.0(2) . . ? C13 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? N3 C19 H19A 109.5 . . ? N3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 H20A 109.5 . . ? N3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C26 C21 C22 120.0(2) . . ? C26 C21 N4 125.25(19) . . ? C22 C21 N4 114.77(19) . . ? O4 C22 C23 120.0(2) . . ? O4 C22 C21 120.4(2) . . ? C23 C22 C21 119.5(2) . . ? C24 C23 C22 120.0(2) . . ? C24 C23 H23 120.0 . . ? C22 C23 H23 120.0 . . ? C23 C24 C25 120.3(2) . . ? C23 C24 H24 119.8 . . ? C25 C24 H24 119.8 . . ? C24 C25 C26 120.0(2) . . ? C24 C25 H25 120.0 . . ? C26 C25 H25 120.0 . . ? C21 C26 C25 120.1(2) . . ? C21 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C32 C27 C28 120.1(2) . . ? C32 C27 N4 125.5(2) . . ? C28 C27 N4 114.44(18) . . ? O5 C28 C29 120.3(2) . . ? O5 C28 C27 119.80(19) . . ? C29 C28 C27 119.9(2) . . ? C30 C29 C28 119.6(2) . . ? C30 C29 H29 120.2 . . ? C28 C29 H29 120.2 . . ? C31 C30 C29 120.4(2) . . ? C31 C30 H30 119.8 . . ? C29 C30 H30 119.8 . . ? C32 C31 C30 120.1(2) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C27 119.9(2) . . ? C31 C32 H32 120.0 . . ? C27 C32 H32 120.0 . . ? C38 C33 C34 120.4(2) . . ? C38 C33 N4 124.84(19) . . ? C34 C33 N4 114.72(18) . . ? O6 C34 C35 120.1(2) . . ? O6 C34 C33 120.39(19) . . ? C35 C34 C33 119.5(2) . . ? C36 C35 C34 119.6(2) . . ? C36 C35 H35 120.2 . . ? C34 C35 H35 120.2 . . ? C35 C36 C37 120.8(2) . . ? C35 C36 H36 119.6 . . ? C37 C36 H36 119.6 . . ? C38 C37 C36 119.8(2) . . ? C38 C37 H37 120.1 . . ? C36 C37 H37 120.1 . . ? C33 C38 C37 119.8(2) . . ? C33 C38 H38 120.1 . . ? C37 C38 H38 120.1 . . ? N6 C39 H39A 109.5 . . ? N6 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N6 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N6 C40 H40A 109.5 . . ? N6 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N6 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 V1 O1 C2 175.33(16) . . . . ? O2 V1 O1 C2 71.30(17) . . . . ? O3 V1 O1 C2 -78.82(17) . . . . ? N1 V1 O1 C2 -3.54(15) . . . . ? N2 V1 O2 C8 174.47(15) . . . . ? O3 V1 O2 C8 68.26(16) . . . . ? O1 V1 O2 C8 -80.96(16) . . . . ? N1 V1 O2 C8 -6.06(15) . . . . ? N2 V1 O3 C14 178.76(16) . . . . ? O2 V1 O3 C14 -76.07(16) . . . . ? O1 V1 O3 C14 73.48(16) . . . . ? N1 V1 O3 C14 -1.81(15) . . . . ? N5 V2 O4 C22 175.84(16) . . . . ? O5 V2 O4 C22 71.00(17) . . . . ? O6 V2 O4 C22 -79.07(17) . . . . ? N4 V2 O4 C22 -2.06(15) . . . . ? N5 V2 O5 C28 -178.10(15) . . . . ? O4 V2 O5 C28 -74.54(17) . . . . ? O6 V2 O5 C28 73.04(17) . . . . ? N4 V2 O5 C28 -1.06(15) . . . . ? N5 V2 O6 C34 -176.06(16) . . . . ? O5 V2 O6 C34 -68.50(18) . . . . ? O4 V2 O6 C34 81.98(17) . . . . ? N4 V2 O6 C34 5.08(16) . . . . ? O2 V1 N1 C1 -116.01(13) . . . . ? O3 V1 N1 C1 122.32(13) . . . . ? O1 V1 N1 C1 3.75(12) . . . . ? O2 V1 N1 C13 124.51(13) . . . . ? O3 V1 N1 C13 2.84(12) . . . . ? O1 V1 N1 C13 -115.73(13) . . . . ? O2 V1 N1 C7 4.94(12) . . . . ? O3 V1 N1 C7 -116.73(13) . . . . ? O1 V1 N1 C7 124.70(13) . . . . ? O5 V2 N4 C27 -0.86(12) . . . . ? O4 V2 N4 C27 123.06(13) . . . . ? O6 V2 N4 C27 -123.45(13) . . . . ? O5 V2 N4 C21 -122.61(13) . . . . ? O4 V2 N4 C21 1.32(12) . . . . ? O6 V2 N4 C21 114.80(13) . . . . ? O5 V2 N4 C33 117.79(13) . . . . ? O4 V2 N4 C33 -118.29(13) . . . . ? O6 V2 N4 C33 -4.81(12) . . . . ? C13 N1 C1 C6 -71.0(3) . . . . ? C7 N1 C1 C6 61.7(3) . . . . ? V1 N1 C1 C6 175.67(18) . . . . ? C13 N1 C1 C2 109.8(2) . . . . ? C7 N1 C1 C2 -117.5(2) . . . . ? V1 N1 C1 C2 -3.5(2) . . . . ? V1 O1 C2 C3 -176.81(17) . . . . ? V1 O1 C2 C1 2.6(3) . . . . ? C6 C1 C2 O1 -177.98(19) . . . . ? N1 C1 C2 O1 1.2(3) . . . . ? C6 C1 C2 C3 1.4(3) . . . . ? N1 C1 C2 C3 -179.34(19) . . . . ? O1 C2 C3 C4 178.2(2) . . . . ? C1 C2 C3 C4 -1.2(3) . . . . ? C2 C3 C4 C5 0.5(4) . . . . ? C3 C4 C5 C6 0.0(4) . . . . ? C4 C5 C6 C1 0.2(4) . . . . ? C2 C1 C6 C5 -1.0(3) . . . . ? N1 C1 C6 C5 179.9(2) . . . . ? C1 N1 C7 C12 -69.0(3) . . . . ? C13 N1 C7 C12 63.6(3) . . . . ? V1 N1 C7 C12 176.92(18) . . . . ? C1 N1 C7 C8 110.7(2) . . . . ? C13 N1 C7 C8 -116.6(2) . . . . ? V1 N1 C7 C8 -3.3(2) . . . . ? V1 O2 C8 C9 -174.70(16) . . . . ? V1 O2 C8 C7 6.2(3) . . . . ? C12 C7 C8 O2 178.82(19) . . . . ? N1 C7 C8 O2 -0.9(3) . . . . ? C12 C7 C8 C9 -0.3(3) . . . . ? N1 C7 C8 C9 179.92(19) . . . . ? O2 C8 C9 C10 -178.6(2) . . . . ? C7 C8 C9 C10 0.6(3) . . . . ? C8 C9 C10 C11 -0.2(3) . . . . ? C9 C10 C11 C12 -0.4(4) . . . . ? C8 C7 C12 C11 -0.3(3) . . . . ? N1 C7 C12 C11 179.4(2) . . . . ? C10 C11 C12 C7 0.6(3) . . . . ? C1 N1 C13 C18 63.3(3) . . . . ? C7 N1 C13 C18 -70.0(3) . . . . ? V1 N1 C13 C18 176.68(18) . . . . ? C1 N1 C13 C14 -116.9(2) . . . . ? C7 N1 C13 C14 109.8(2) . . . . ? V1 N1 C13 C14 -3.5(2) . . . . ? V1 O3 C14 C15 -178.84(16) . . . . ? V1 O3 C14 C13 0.2(3) . . . . ? C18 C13 C14 O3 -177.5(2) . . . . ? N1 C13 C14 O3 2.6(3) . . . . ? C18 C13 C14 C15 1.6(3) . . . . ? N1 C13 C14 C15 -178.29(19) . . . . ? O3 C14 C15 C16 178.6(2) . . . . ? C13 C14 C15 C16 -0.5(3) . . . . ? C14 C15 C16 C17 -0.7(3) . . . . ? C15 C16 C17 C18 0.8(4) . . . . ? C14 C13 C18 C17 -1.4(3) . . . . ? N1 C13 C18 C17 178.4(2) . . . . ? C16 C17 C18 C13 0.3(4) . . . . ? C27 N4 C21 C26 65.7(3) . . . . ? C33 N4 C21 C26 -66.8(3) . . . . ? V2 N4 C21 C26 -179.66(18) . . . . ? C27 N4 C21 C22 -115.1(2) . . . . ? C33 N4 C21 C22 112.4(2) . . . . ? V2 N4 C21 C22 -0.5(2) . . . . ? V2 O4 C22 C23 -177.72(16) . . . . ? V2 O4 C22 C21 2.5(3) . . . . ? C26 C21 C22 O4 178.1(2) . . . . ? N4 C21 C22 O4 -1.1(3) . . . . ? C26 C21 C22 C23 -1.6(3) . . . . ? N4 C21 C22 C23 179.15(19) . . . . ? O4 C22 C23 C24 -179.4(2) . . . . ? C21 C22 C23 C24 0.4(3) . . . . ? C22 C23 C24 C25 0.9(4) . . . . ? C23 C24 C25 C26 -0.9(4) . . . . ? C22 C21 C26 C25 1.6(3) . . . . ? N4 C21 C26 C25 -179.3(2) . . . . ? C24 C25 C26 C21 -0.3(3) . . . . ? C21 N4 C27 C32 -64.4(3) . . . . ? C33 N4 C27 C32 68.6(3) . . . . ? V2 N4 C27 C32 -178.68(18) . . . . ? C21 N4 C27 C28 116.8(2) . . . . ? C33 N4 C27 C28 -110.2(2) . . . . ? V2 N4 C27 C28 2.5(2) . . . . ? V2 O5 C28 C29 -176.99(15) . . . . ? V2 O5 C28 C27 3.1(3) . . . . ? C32 C27 C28 O5 177.36(19) . . . . ? N4 C27 C28 O5 -3.8(3) . . . . ? C32 C27 C28 C29 -2.5(3) . . . . ? N4 C27 C28 C29 176.30(18) . . . . ? O5 C28 C29 C30 -178.3(2) . . . . ? C27 C28 C29 C30 1.6(3) . . . . ? C28 C29 C30 C31 0.1(3) . . . . ? C29 C30 C31 C32 -0.9(4) . . . . ? C30 C31 C32 C27 0.0(3) . . . . ? C28 C27 C32 C31 1.7(3) . . . . ? N4 C27 C32 C31 -177.0(2) . . . . ? C27 N4 C33 C38 -63.0(3) . . . . ? C21 N4 C33 C38 70.8(3) . . . . ? V2 N4 C33 C38 -176.18(18) . . . . ? C27 N4 C33 C34 117.2(2) . . . . ? C21 N4 C33 C34 -109.0(2) . . . . ? V2 N4 C33 C34 4.0(2) . . . . ? V2 O6 C34 C35 176.21(16) . . . . ? V2 O6 C34 C33 -4.4(3) . . . . ? C38 C33 C34 O6 179.6(2) . . . . ? N4 C33 C34 O6 -0.6(3) . . . . ? C38 C33 C34 C35 -1.0(3) . . . . ? N4 C33 C34 C35 178.80(19) . . . . ? O6 C34 C35 C36 179.1(2) . . . . ? C33 C34 C35 C36 -0.3(3) . . . . ? C34 C35 C36 C37 1.5(3) . . . . ? C35 C36 C37 C38 -1.4(4) . . . . ? C34 C33 C38 C37 1.2(3) . . . . ? N4 C33 C38 C37 -178.6(2) . . . . ? C36 C37 C38 C33 0.0(3) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.551 _refine_diff_density_min -0.528 _refine_diff_density_rms 0.085 data_4dDMH4d(CCDC-925608) _database_code_depnum_ccdc_archive 'CCDC 925608' #TrackingRef 'MoriuchiCIFCCDC925607_925609.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H42 F2 N8 O6 V2' _chemical_formula_sum 'C42 H42 F2 N8 O6 V2' _chemical_formula_weight 894.72 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_space_group_name_Hall 'P 2yb' _symmetry_Int_Tables_number 4 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.3304(11) _cell_length_b 18.403(2) _cell_length_c 12.1985(14) _cell_angle_alpha 90.00 _cell_angle_beta 102.631(3) _cell_angle_gamma 90.00 _cell_volume 2043.9(4) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 8300 _cell_measurement_theta_min 3.10 _cell_measurement_theta_max 27.46 _exptl_crystal_description block _exptl_crystal_colour brown _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.454 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 924 _exptl_absorpt_coefficient_mu 0.525 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9254 _exptl_absorpt_correction_T_max 0.9592 _exptl_absorpt_process_details ; Higashi, T. (1999). Abscor - Empirical Absorption Correction based on Fourier Series Approximation. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'imaging plate' _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16022 _diffrn_reflns_av_R_equivalents 0.1343 _diffrn_reflns_av_sigmaI/netI 0.1701 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6731 _reflns_number_gt 4016 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rigaku/RAPID Diffractometer Control' _computing_cell_refinement 'Rigaku/RAPID Diffractometer Control' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 and modified' _computing_molecular_graphics ? _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^)+(0.0826P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(4) _chemical_absolute_configuration . _refine_ls_number_reflns 6731 _refine_ls_number_parameters 561 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.1353 _refine_ls_R_factor_gt 0.0742 _refine_ls_wR_factor_ref 0.1803 _refine_ls_wR_factor_gt 0.1511 _refine_ls_goodness_of_fit_ref 0.970 _refine_ls_restrained_S_all 0.970 _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 1.06514(16) 0.86645(8) 0.69344(11) 0.0278(4) Uani 1 1 d . . . V2 V 0.72608(15) 1.08792(7) 0.77000(11) 0.0261(4) Uani 1 1 d . . . F1A F 1.5251(10) 0.7796(5) 0.6824(7) 0.051(3) Uani 0.667(15) 1 d P A 1 F1B F 0.726(2) 0.6900(10) 0.5426(15) 0.065(8) Uani 0.333(15) 1 d P A 2 F2A F 1.2139(14) 1.1178(6) 0.9357(10) 0.063(5) Uani 0.525(16) 1 d P B 3 F2B F 0.5026(19) 1.3068(10) 0.8392(13) 0.092(7) Uani 0.475(16) 1 d P B 4 O1 O 1.2508(7) 0.8281(3) 0.6822(5) 0.0344(15) Uani 1 1 d . . . O2 O 1.1276(6) 0.9260(3) 0.8224(4) 0.0284(14) Uani 1 1 d . . . O3 O 0.9466(7) 0.7907(3) 0.6245(4) 0.0315(15) Uani 1 1 d . . . O4 O 0.9212(6) 1.1102(3) 0.8501(5) 0.0271(14) Uani 1 1 d . . . O5 O 0.5892(6) 1.0672(3) 0.6343(4) 0.0277(14) Uani 1 1 d . . . O6 O 0.6414(7) 1.1767(3) 0.8067(4) 0.0261(14) Uani 1 1 d . . . N1 N 1.1012(8) 0.7831(4) 0.8368(5) 0.0267(17) Uani 1 1 d . . . N2 N 1.0643(8) 0.9262(4) 0.5911(6) 0.0290(17) Uani 1 1 d . . . N3 N 1.0743(9) 0.9796(4) 0.5215(6) 0.042(2) Uani 1 1 d . . . N4 N 0.7990(7) 1.1640(4) 0.6462(5) 0.0238(16) Uani 1 1 d . . . N5 N 0.6598(8) 1.0390(4) 0.8653(6) 0.0290(18) Uani 1 1 d . . . N6 N 0.5970(10) 1.0060(5) 0.9365(7) 0.049(2) Uani 1 1 d . . . N7 N 0.8374(8) 0.9170(4) 0.7041(5) 0.0282(17) Uani 1 1 d . . . N8 N 0.8602(8) 0.9981(4) 0.7185(6) 0.0285(17) Uani 1 1 d . . . H8A H 0.8761 1.0132 0.6503 0.034 Uiso 1 1 calc R . . H8B H 0.9497 1.0020 0.7680 0.034 Uiso 1 1 calc R . . C1 C 1.2539(10) 0.7579(5) 0.8451(7) 0.031(2) Uani 1 1 d . . . C2 C 1.3220(10) 0.7827(5) 0.7631(7) 0.028(2) Uani 1 1 d . A . C3 C 1.4629(11) 0.7589(5) 0.7655(8) 0.036(2) Uani 1 1 d . . . H3B H 1.5095 0.7741 0.7076 0.043 Uiso 0.333(15) 1 calc PR A 2 C4 C 1.5384(11) 0.7140(5) 0.8483(9) 0.045(3) Uani 1 1 d . A . H4 H 1.6353 0.6986 0.8474 0.054 Uiso 1 1 calc R . . C5 C 1.4699(11) 0.6912(6) 0.9347(8) 0.044(3) Uani 1 1 d . . . H5 H 1.5201 0.6609 0.9940 0.052 Uiso 1 1 calc R A . C6 C 1.3272(11) 0.7141(5) 0.9307(8) 0.040(2) Uani 1 1 d . A . H6 H 1.2791 0.6992 0.9881 0.048 Uiso 1 1 calc R . . C7 C 1.0856(10) 0.8257(5) 0.9364(7) 0.029(2) Uani 1 1 d . . . C8 C 1.1085(10) 0.8998(5) 0.9231(7) 0.032(2) Uani 1 1 d . . . C9 C 1.0989(11) 0.9477(6) 1.0090(7) 0.038(2) Uani 1 1 d . . . H9 H 1.1123 0.9985 1.0011 0.046 Uiso 1 1 calc R . . C10 C 1.0688(11) 0.9186(6) 1.1077(7) 0.042(3) Uani 1 1 d . . . H10 H 1.0621 0.9508 1.1673 0.051 Uiso 1 1 calc R . . C11 C 1.0484(11) 0.8452(5) 1.1219(8) 0.038(3) Uani 1 1 d . . . H11 H 1.0290 0.8271 1.1902 0.046 Uiso 1 1 calc R . . C12 C 1.0568(11) 0.7983(5) 1.0345(7) 0.033(2) Uani 1 1 d . . . H12 H 1.0428 0.7475 1.0422 0.040 Uiso 1 1 calc R . . C13 C 0.9937(9) 0.7252(5) 0.7982(7) 0.027(2) Uani 1 1 d . . . C14 C 0.9160(10) 0.7326(5) 0.6858(7) 0.029(2) Uani 1 1 d . A . C15 C 0.8060(10) 0.6833(5) 0.6411(8) 0.034(2) Uani 1 1 d . . . H15 H 0.7475 0.6907 0.5678 0.041 Uiso 0.667(15) 1 calc PR A 1 C16 C 0.7812(10) 0.6234(5) 0.7033(7) 0.031(2) Uani 1 1 d . A . H16 H 0.7080 0.5890 0.6717 0.037 Uiso 1 1 calc R . . C17 C 0.8629(11) 0.6137(5) 0.8113(8) 0.038(3) Uani 1 1 d . . . H17 H 0.8452 0.5724 0.8531 0.046 Uiso 1 1 calc R A . C18 C 0.9740(11) 0.6649(5) 0.8614(8) 0.034(2) Uani 1 1 d . A . H18 H 1.0318 0.6578 0.9350 0.040 Uiso 1 1 calc R . . C19 C 1.1789(12) 1.0359(5) 0.5642(8) 0.045(3) Uani 1 1 d . . . H19A H 1.2776 1.0148 0.5853 0.054 Uiso 1 1 calc R . . H19B H 1.1535 1.0582 0.6304 0.054 Uiso 1 1 calc R . . H19C H 1.1769 1.0729 0.5062 0.054 Uiso 1 1 calc R . . C20 C 1.0396(12) 0.9656(6) 0.4005(7) 0.050(3) Uani 1 1 d . . . H20A H 0.9377 0.9490 0.3773 0.060 Uiso 1 1 calc R . . H20B H 1.1056 0.9281 0.3830 0.060 Uiso 1 1 calc R . . H20C H 1.0521 1.0104 0.3603 0.060 Uiso 1 1 calc R . . C21 C 0.9578(9) 1.1762(5) 0.6881(7) 0.029(2) Uani 1 1 d . . . C22 C 1.0135(10) 1.1447(5) 0.7961(7) 0.030(2) Uani 1 1 d . B . C23 C 1.1615(9) 1.1501(5) 0.8406(8) 0.031(2) Uani 1 1 d . . . H23 H 1.2017 1.1271 0.9102 0.037 Uiso 0.475(16) 1 calc PR B 4 C24 C 1.2546(11) 1.1888(5) 0.7860(8) 0.039(2) Uani 1 1 d . B . H24 H 1.3566 1.1927 0.8184 0.047 Uiso 1 1 calc R . . C25 C 1.1955(11) 1.2213(5) 0.6840(8) 0.036(2) Uani 1 1 d . . . H25 H 1.2586 1.2471 0.6463 0.044 Uiso 1 1 calc R B . C26 C 1.0488(10) 1.2174(5) 0.6357(7) 0.032(2) Uani 1 1 d . B . H26 H 1.0097 1.2424 0.5676 0.038 Uiso 1 1 calc R . . C27 C 0.7523(10) 1.1286(5) 0.5394(6) 0.025(2) Uani 1 1 d . . . C28 C 0.6328(9) 1.0808(5) 0.5350(6) 0.030(2) Uani 1 1 d . . . C29 C 0.5656(10) 1.0434(5) 0.4388(6) 0.033(2) Uani 1 1 d . . . H29 H 0.4864 1.0109 0.4384 0.039 Uiso 1 1 calc R . . C30 C 0.6213(10) 1.0564(5) 0.3404(7) 0.034(2) Uani 1 1 d . . . H30 H 0.5770 1.0326 0.2723 0.041 Uiso 1 1 calc R . . C31 C 0.7377(11) 1.1024(5) 0.3422(7) 0.037(2) Uani 1 1 d . . . H31 H 0.7725 1.1097 0.2754 0.044 Uiso 1 1 calc R . . C32 C 0.8068(10) 1.1393(5) 0.4416(7) 0.032(2) Uani 1 1 d . . . H32 H 0.8879 1.1707 0.4423 0.038 Uiso 1 1 calc R . . C33 C 0.7147(9) 1.2322(5) 0.6511(7) 0.025(2) Uani 1 1 d . . . C34 C 0.6399(9) 1.2345(5) 0.7396(7) 0.029(2) Uani 1 1 d . B . C35 C 0.5677(10) 1.2967(5) 0.7502(8) 0.033(2) Uani 1 1 d . . . H35 H 0.5226 1.3013 0.8126 0.040 Uiso 0.525(16) 1 calc PR B 3 C36 C 0.5555(10) 1.3537(5) 0.6765(8) 0.035(2) Uani 1 1 d . B . H36 H 0.5011 1.3957 0.6870 0.042 Uiso 1 1 calc R . . C37 C 0.6240(11) 1.3492(5) 0.5857(8) 0.041(3) Uani 1 1 d . . . H37 H 0.6164 1.3878 0.5329 0.049 Uiso 1 1 calc R B . C38 C 0.7037(10) 1.2867(5) 0.5746(7) 0.033(2) Uani 1 1 d . B . H38 H 0.7506 1.2822 0.5133 0.040 Uiso 1 1 calc R . . C39 C 0.6744(15) 0.9960(7) 1.0503(8) 0.065(4) Uani 1 1 d . . . H39A H 0.7026 1.0434 1.0848 0.078 Uiso 1 1 calc R . . H39B H 0.7627 0.9668 1.0518 0.078 Uiso 1 1 calc R . . H39C H 0.6109 0.9708 1.0922 0.078 Uiso 1 1 calc R . . C40 C 0.4515(12) 0.9755(7) 0.9021(11) 0.068(4) Uani 1 1 d . . . H40A H 0.4513 0.9384 0.8445 0.082 Uiso 1 1 calc R . . H40B H 0.3817 1.0141 0.8715 0.082 Uiso 1 1 calc R . . H40C H 0.4227 0.9534 0.9671 0.082 Uiso 1 1 calc R . . C41 C 0.7276(11) 0.9046(5) 0.5954(7) 0.040(2) Uani 1 1 d . . . H41A H 0.6369 0.9311 0.5968 0.049 Uiso 1 1 calc R . . H41B H 0.7061 0.8526 0.5861 0.049 Uiso 1 1 calc R . . H41C H 0.7682 0.9220 0.5326 0.049 Uiso 1 1 calc R . . C42 C 0.7703(11) 0.8897(5) 0.7959(7) 0.038(2) Uani 1 1 d . . . H42A H 0.7477 0.8379 0.7844 0.045 Uiso 1 1 calc R . . H42B H 0.6797 0.9167 0.7958 0.045 Uiso 1 1 calc R . . H42C H 0.8394 0.8966 0.8682 0.045 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 0.0286(9) 0.0298(8) 0.0227(7) 0.0003(7) 0.0008(6) -0.0005(8) V2 0.0189(8) 0.0327(9) 0.0236(7) 0.0011(7) -0.0019(6) 0.0007(7) F1A 0.043(6) 0.049(6) 0.060(6) -0.002(5) 0.008(5) 0.003(5) F1B 0.078(16) 0.072(15) 0.042(12) -0.003(9) 0.006(11) 0.010(12) F2A 0.062(9) 0.061(9) 0.062(9) 0.002(6) 0.003(7) -0.007(6) F2B 0.076(12) 0.121(15) 0.084(12) 0.000(10) 0.026(10) 0.032(10) O1 0.035(4) 0.032(4) 0.037(4) -0.004(3) 0.012(3) -0.002(3) O2 0.026(4) 0.035(4) 0.024(3) -0.005(3) 0.005(3) -0.008(3) O3 0.042(4) 0.025(3) 0.024(3) 0.001(3) 0.002(3) 0.003(3) O4 0.022(3) 0.029(3) 0.028(3) 0.002(3) 0.001(3) -0.004(3) O5 0.030(4) 0.025(3) 0.028(3) -0.001(2) 0.006(3) 0.000(3) O6 0.027(4) 0.022(3) 0.028(3) 0.000(3) 0.002(3) 0.001(3) N1 0.022(4) 0.031(4) 0.022(4) -0.007(3) -0.006(3) 0.002(3) N2 0.035(5) 0.020(4) 0.033(4) 0.006(3) 0.009(4) 0.000(3) N3 0.051(6) 0.044(5) 0.026(4) -0.002(4) 0.001(4) -0.002(4) N4 0.016(4) 0.040(5) 0.014(3) -0.003(3) 0.002(3) -0.001(3) N5 0.023(4) 0.041(4) 0.025(4) 0.001(3) 0.010(4) -0.007(4) N6 0.048(6) 0.060(6) 0.041(5) 0.010(4) 0.017(5) -0.003(5) N7 0.021(4) 0.033(4) 0.028(4) -0.001(3) -0.002(3) -0.008(4) N8 0.025(5) 0.028(4) 0.032(4) -0.001(3) 0.005(4) -0.003(3) C1 0.016(5) 0.042(6) 0.028(5) -0.009(4) -0.009(4) 0.000(4) C2 0.025(5) 0.040(6) 0.015(4) 0.005(4) -0.006(4) -0.004(4) C3 0.025(6) 0.048(6) 0.033(5) -0.003(5) 0.002(5) -0.012(5) C4 0.033(6) 0.043(6) 0.058(7) -0.009(5) 0.007(5) 0.007(5) C5 0.036(6) 0.053(7) 0.037(6) -0.008(5) -0.003(5) 0.020(5) C6 0.041(6) 0.040(6) 0.039(6) -0.002(5) 0.010(5) 0.012(5) C7 0.024(5) 0.027(5) 0.036(5) -0.011(4) 0.004(4) 0.003(4) C8 0.015(5) 0.053(7) 0.023(5) -0.010(4) -0.008(4) -0.005(4) C9 0.038(6) 0.041(6) 0.030(5) -0.001(4) -0.004(5) -0.003(5) C10 0.053(7) 0.052(7) 0.024(5) -0.002(5) 0.011(5) -0.003(5) C11 0.042(6) 0.047(7) 0.029(5) 0.008(4) 0.014(5) 0.003(5) C12 0.050(7) 0.025(5) 0.024(5) 0.006(4) 0.007(5) 0.004(5) C13 0.015(5) 0.028(5) 0.035(5) -0.009(4) 0.001(4) 0.006(4) C14 0.041(6) 0.026(5) 0.022(4) 0.004(4) 0.006(4) -0.002(4) C15 0.031(6) 0.034(6) 0.030(5) -0.006(4) -0.007(4) 0.000(5) C16 0.023(5) 0.032(5) 0.039(5) -0.018(4) 0.009(4) -0.007(4) C17 0.049(7) 0.019(5) 0.052(6) 0.001(4) 0.023(6) 0.002(5) C18 0.045(6) 0.019(5) 0.038(5) 0.002(4) 0.013(5) 0.008(4) C19 0.049(7) 0.037(6) 0.054(7) 0.005(5) 0.018(6) 0.001(5) C20 0.049(7) 0.073(8) 0.027(5) 0.008(5) 0.005(5) 0.011(6) C21 0.009(5) 0.040(6) 0.037(5) -0.004(4) 0.000(4) -0.009(4) C22 0.019(5) 0.044(6) 0.026(5) -0.005(4) 0.000(4) -0.008(4) C23 0.015(5) 0.038(6) 0.034(5) 0.007(4) -0.006(4) 0.000(4) C24 0.024(6) 0.046(6) 0.047(6) 0.000(5) 0.005(5) -0.006(5) C25 0.034(7) 0.044(6) 0.034(5) -0.001(4) 0.013(5) -0.001(5) C26 0.031(6) 0.039(6) 0.026(5) 0.004(4) 0.008(4) -0.005(5) C27 0.025(5) 0.032(5) 0.014(4) 0.004(4) -0.005(4) -0.002(4) C28 0.024(5) 0.042(6) 0.023(4) 0.004(4) 0.002(4) 0.002(5) C29 0.037(6) 0.040(5) 0.014(4) 0.002(4) -0.009(4) 0.033(5) C30 0.029(6) 0.038(6) 0.030(5) -0.001(4) -0.005(4) -0.002(4) C31 0.039(6) 0.050(7) 0.021(4) -0.004(4) 0.007(4) 0.012(5) C32 0.025(6) 0.033(5) 0.038(5) -0.002(4) 0.008(4) 0.000(4) C33 0.020(5) 0.026(5) 0.028(5) 0.005(4) -0.001(4) 0.005(4) C34 0.015(5) 0.034(5) 0.029(5) 0.002(4) -0.015(4) -0.006(4) C35 0.032(6) 0.023(5) 0.044(6) -0.008(4) 0.005(5) 0.005(4) C36 0.026(5) 0.017(5) 0.058(6) -0.002(4) 0.001(5) 0.002(4) C37 0.040(6) 0.039(6) 0.039(5) 0.016(5) -0.003(5) -0.002(5) C38 0.031(6) 0.031(6) 0.034(5) -0.002(4) 0.000(4) -0.002(5) C39 0.099(11) 0.071(8) 0.025(6) 0.006(5) 0.012(6) -0.008(8) C40 0.043(8) 0.074(9) 0.095(10) -0.003(7) 0.032(7) -0.028(7) C41 0.032(6) 0.047(6) 0.032(5) -0.002(4) -0.016(5) 0.009(5) C42 0.043(6) 0.028(5) 0.041(6) 0.000(4) 0.006(5) -0.002(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 N2 1.663(7) . ? V1 O3 1.862(6) . ? V1 O2 1.902(6) . ? V1 O1 1.903(6) . ? V1 N1 2.295(7) . ? V1 N7 2.349(7) . ? V2 N5 1.690(7) . ? V2 O5 1.895(6) . ? V2 O6 1.910(6) . ? V2 O4 1.913(6) . ? V2 N8 2.245(7) . ? V2 N4 2.270(7) . ? F1A C3 1.330(11) . ? F1B C15 1.276(19) . ? F2A C23 1.300(14) . ? F2B C35 1.368(16) . ? O1 C2 1.352(10) . ? O2 C8 1.367(10) . ? O3 C14 1.370(10) . ? O4 C22 1.352(10) . ? O5 C28 1.383(9) . ? O6 C34 1.340(10) . ? N1 C13 1.468(11) . ? N1 C7 1.481(10) . ? N1 C1 1.481(11) . ? N2 N3 1.315(10) . ? N3 C19 1.440(12) . ? N3 C20 1.462(11) . ? N4 C27 1.437(10) . ? N4 C21 1.475(10) . ? N4 C33 1.489(10) . ? N5 N6 1.300(10) . ? N6 C39 1.429(13) . ? N6 C40 1.444(13) . ? N7 C42 1.485(10) . ? N7 C41 1.505(10) . ? N7 N8 1.512(9) . ? N8 H8A 0.9200 . ? N8 H8B 0.9200 . ? C1 C2 1.376(11) . ? C1 C6 1.377(13) . ? C2 C3 1.379(12) . ? C3 C4 1.373(14) . ? C3 H3B 0.9500 . ? C4 C5 1.412(13) . ? C4 H4 0.9500 . ? C5 C6 1.387(13) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C12 1.379(12) . ? C7 C8 1.395(12) . ? C8 C9 1.387(13) . ? C9 C10 1.401(12) . ? C9 H9 0.9500 . ? C10 C11 1.382(13) . ? C10 H10 0.9500 . ? C11 C12 1.387(12) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.385(12) . ? C13 C14 1.411(12) . ? C14 C15 1.389(12) . ? C15 C16 1.385(12) . ? C15 H15 0.9500 . ? C16 C17 1.381(13) . ? C16 H16 0.9500 . ? C17 C18 1.435(13) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C26 1.394(11) . ? C21 C22 1.429(12) . ? C22 C23 1.373(12) . ? C23 C24 1.400(12) . ? C23 H23 0.9500 . ? C24 C25 1.381(13) . ? C24 H24 0.9500 . ? C25 C26 1.369(13) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C27 C32 1.409(11) . ? C27 C28 1.412(12) . ? C28 C29 1.386(12) . ? C29 C30 1.429(12) . ? C29 H29 0.9500 . ? C30 C31 1.374(13) . ? C30 H30 0.9500 . ? C31 C32 1.416(12) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C38 1.359(11) . ? C33 C34 1.408(11) . ? C34 C35 1.349(12) . ? C35 C36 1.369(12) . ? C35 H35 0.9500 . ? C36 C37 1.397(12) . ? C36 H36 0.9500 . ? C37 C38 1.392(13) . ? C37 H37 0.9500 . ? C38 H38 0.9500 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 V1 O3 104.6(3) . . ? N2 V1 O2 101.0(3) . . ? O3 V1 O2 148.2(2) . . ? N2 V1 O1 92.6(3) . . ? O3 V1 O1 98.6(3) . . ? O2 V1 O1 98.9(3) . . ? N2 V1 N1 172.0(3) . . ? O3 V1 N1 79.5(2) . . ? O2 V1 N1 77.7(2) . . ? O1 V1 N1 79.8(3) . . ? N2 V1 N7 85.6(3) . . ? O3 V1 N7 82.3(3) . . ? O2 V1 N7 81.0(2) . . ? O1 V1 N7 178.2(3) . . ? N1 V1 N7 101.9(2) . . ? N5 V2 O5 102.4(3) . . ? N5 V2 O6 93.6(3) . . ? O5 V2 O6 98.2(2) . . ? N5 V2 O4 102.3(3) . . ? O5 V2 O4 150.9(2) . . ? O6 V2 O4 95.4(3) . . ? N5 V2 N8 96.3(3) . . ? O5 V2 N8 85.3(3) . . ? O6 V2 N8 168.6(3) . . ? O4 V2 N8 76.9(3) . . ? N5 V2 N4 173.6(3) . . ? O5 V2 N4 77.6(2) . . ? O6 V2 N4 80.1(2) . . ? O4 V2 N4 79.5(2) . . ? N8 V2 N4 90.1(2) . . ? C2 O1 V1 119.1(5) . . ? C8 O2 V1 117.6(5) . . ? C14 O3 V1 120.8(5) . . ? C22 O4 V2 119.2(5) . . ? C28 O5 V2 117.2(5) . . ? C34 O6 V2 119.0(5) . . ? C13 N1 C7 117.7(7) . . ? C13 N1 C1 112.0(6) . . ? C7 N1 C1 112.0(7) . . ? C13 N1 V1 105.4(5) . . ? C7 N1 V1 104.3(5) . . ? C1 N1 V1 103.9(5) . . ? N3 N2 V1 171.8(7) . . ? N2 N3 C19 116.2(8) . . ? N2 N3 C20 119.2(8) . . ? C19 N3 C20 118.4(8) . . ? C27 N4 C21 117.8(7) . . ? C27 N4 C33 111.2(6) . . ? C21 N4 C33 110.9(7) . . ? C27 N4 V2 104.3(5) . . ? C21 N4 V2 106.7(5) . . ? C33 N4 V2 104.8(4) . . ? N6 N5 V2 174.0(7) . . ? N5 N6 C39 120.2(9) . . ? N5 N6 C40 121.3(9) . . ? C39 N6 C40 118.4(9) . . ? C42 N7 C41 107.2(7) . . ? C42 N7 N8 108.5(6) . . ? C41 N7 N8 107.7(6) . . ? C42 N7 V1 116.3(5) . . ? C41 N7 V1 110.0(5) . . ? N8 N7 V1 106.9(4) . . ? N7 N8 V2 133.4(5) . . ? N7 N8 H8A 103.9 . . ? V2 N8 H8A 103.9 . . ? N7 N8 H8B 103.9 . . ? V2 N8 H8B 103.9 . . ? H8A N8 H8B 105.4 . . ? C2 C1 C6 121.0(9) . . ? C2 C1 N1 115.9(8) . . ? C6 C1 N1 123.1(8) . . ? O1 C2 C1 120.3(8) . . ? O1 C2 C3 121.8(8) . . ? C1 C2 C3 117.9(8) . . ? F1A C3 C4 119.5(9) . . ? F1A C3 C2 117.7(9) . . ? C4 C3 C2 122.7(9) . . ? C4 C3 H3B 118.6 . . ? C2 C3 H3B 118.6 . . ? C3 C4 C5 119.0(9) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C6 C5 C4 118.1(9) . . ? C6 C5 H5 121.0 . . ? C4 C5 H5 121.0 . . ? C1 C6 C5 121.2(9) . . ? C1 C6 H6 119.4 . . ? C5 C6 H6 119.4 . . ? C12 C7 C8 121.5(8) . . ? C12 C7 N1 126.2(8) . . ? C8 C7 N1 112.2(8) . . ? O2 C8 C9 119.8(9) . . ? O2 C8 C7 120.2(8) . . ? C9 C8 C7 119.8(9) . . ? C8 C9 C10 117.7(9) . . ? C8 C9 H9 121.1 . . ? C10 C9 H9 121.1 . . ? C11 C10 C9 122.7(9) . . ? C11 C10 H10 118.6 . . ? C9 C10 H10 118.6 . . ? C10 C11 C12 118.7(8) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? C7 C12 C11 119.6(8) . . ? C7 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C18 C13 C14 121.0(8) . . ? C18 C13 N1 124.6(8) . . ? C14 C13 N1 114.3(8) . . ? O3 C14 C15 121.4(8) . . ? O3 C14 C13 118.8(8) . . ? C15 C14 C13 119.8(8) . . ? F1B C15 C16 117.3(12) . . ? F1B C15 C14 122.5(12) . . ? C16 C15 C14 120.1(8) . . ? C16 C15 H15 119.9 . . ? C14 C15 H15 119.9 . . ? C17 C16 C15 120.1(8) . . ? C17 C16 H16 119.9 . . ? C15 C16 H16 119.9 . . ? C16 C17 C18 121.2(8) . . ? C16 C17 H17 119.4 . . ? C18 C17 H17 119.4 . . ? C13 C18 C17 117.4(9) . . ? C13 C18 H18 121.3 . . ? C17 C18 H18 121.3 . . ? N3 C19 H19A 109.5 . . ? N3 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N3 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N3 C20 H20A 109.5 . . ? N3 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N3 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C26 C21 C22 120.6(8) . . ? C26 C21 N4 126.2(8) . . ? C22 C21 N4 113.2(7) . . ? O4 C22 C23 122.3(8) . . ? O4 C22 C21 119.9(8) . . ? C23 C22 C21 117.8(8) . . ? F2A C23 C22 118.0(10) . . ? F2A C23 C24 120.4(10) . . ? C22 C23 C24 121.6(9) . . ? C22 C23 H23 119.2 . . ? C24 C23 H23 119.2 . . ? C25 C24 C23 118.8(9) . . ? C25 C24 H24 120.6 . . ? C23 C24 H24 120.6 . . ? C26 C25 C24 122.0(9) . . ? C26 C25 H25 119.0 . . ? C24 C25 H25 119.0 . . ? C25 C26 C21 118.9(8) . . ? C25 C26 H26 120.6 . . ? C21 C26 H26 120.6 . . ? C32 C27 C28 118.9(8) . . ? C32 C27 N4 127.6(8) . . ? C28 C27 N4 113.4(7) . . ? O5 C28 C29 119.1(8) . . ? O5 C28 C27 117.4(7) . . ? C29 C28 C27 123.3(8) . . ? C28 C29 C30 116.6(9) . . ? C28 C29 H29 121.7 . . ? C30 C29 H29 121.7 . . ? C31 C30 C29 121.4(8) . . ? C31 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C30 C31 C32 121.3(8) . . ? C30 C31 H31 119.3 . . ? C32 C31 H31 119.3 . . ? C27 C32 C31 118.5(8) . . ? C27 C32 H32 120.8 . . ? C31 C32 H32 120.8 . . ? C38 C33 C34 121.8(8) . . ? C38 C33 N4 123.8(7) . . ? C34 C33 N4 114.3(7) . . ? O6 C34 C35 123.6(8) . . ? O6 C34 C33 120.2(8) . . ? C35 C34 C33 116.2(8) . . ? C34 C35 F2B 120.6(11) . . ? C34 C35 C36 123.9(8) . . ? F2B C35 C36 115.5(10) . . ? C34 C35 H35 118.1 . . ? C36 C35 H35 118.1 . . ? C35 C36 C37 119.3(8) . . ? C35 C36 H36 120.3 . . ? C37 C36 H36 120.3 . . ? C38 C37 C36 118.1(8) . . ? C38 C37 H37 120.9 . . ? C36 C37 H37 120.9 . . ? C33 C38 C37 120.4(8) . . ? C33 C38 H38 119.8 . . ? C37 C38 H38 119.8 . . ? N6 C39 H39A 109.5 . . ? N6 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N6 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N6 C40 H40A 109.5 . . ? N6 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N6 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N7 C41 H41A 109.5 . . ? N7 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N7 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N7 C42 H42A 109.5 . . ? N7 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N7 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 V1 O1 C2 168.7(6) . . . . ? O3 V1 O1 C2 -86.2(6) . . . . ? O2 V1 O1 C2 67.1(6) . . . . ? N1 V1 O1 C2 -8.6(6) . . . . ? N2 V1 O2 C8 164.9(6) . . . . ? O3 V1 O2 C8 22.0(9) . . . . ? O1 V1 O2 C8 -100.7(6) . . . . ? N1 V1 O2 C8 -23.2(6) . . . . ? N7 V1 O2 C8 81.2(6) . . . . ? N2 V1 O3 C14 -176.7(6) . . . . ? O2 V1 O3 C14 -34.4(9) . . . . ? O1 V1 O3 C14 88.3(6) . . . . ? N1 V1 O3 C14 10.4(6) . . . . ? N7 V1 O3 C14 -93.3(6) . . . . ? N5 V2 O4 C22 174.7(6) . . . . ? O5 V2 O4 C22 27.1(9) . . . . ? O6 V2 O4 C22 -90.5(6) . . . . ? N8 V2 O4 C22 81.0(6) . . . . ? N4 V2 O4 C22 -11.6(6) . . . . ? N5 V2 O5 C28 -161.3(6) . . . . ? O6 V2 O5 C28 103.2(6) . . . . ? O4 V2 O5 C28 -13.7(8) . . . . ? N8 V2 O5 C28 -65.9(6) . . . . ? N4 V2 O5 C28 25.3(6) . . . . ? N5 V2 O6 C34 -168.7(6) . . . . ? O5 V2 O6 C34 -65.6(6) . . . . ? O4 V2 O6 C34 88.6(6) . . . . ? N8 V2 O6 C34 41.4(16) . . . . ? N4 V2 O6 C34 10.3(6) . . . . ? O3 V1 N1 C13 -9.1(5) . . . . ? O2 V1 N1 C13 148.6(5) . . . . ? O1 V1 N1 C13 -109.9(5) . . . . ? N7 V1 N1 C13 70.7(5) . . . . ? O3 V1 N1 C7 -133.7(5) . . . . ? O2 V1 N1 C7 24.0(5) . . . . ? O1 V1 N1 C7 125.4(5) . . . . ? N7 V1 N1 C7 -53.9(5) . . . . ? O3 V1 N1 C1 108.9(5) . . . . ? O2 V1 N1 C1 -93.5(5) . . . . ? O1 V1 N1 C1 8.0(5) . . . . ? N7 V1 N1 C1 -171.4(5) . . . . ? O5 V2 N4 C27 -27.0(5) . . . . ? O6 V2 N4 C27 -127.8(5) . . . . ? O4 V2 N4 C27 134.8(5) . . . . ? N8 V2 N4 C27 58.1(5) . . . . ? O5 V2 N4 C21 -152.4(5) . . . . ? O6 V2 N4 C21 106.8(5) . . . . ? O4 V2 N4 C21 9.4(5) . . . . ? N8 V2 N4 C21 -67.3(5) . . . . ? O5 V2 N4 C33 89.9(5) . . . . ? O6 V2 N4 C33 -10.8(5) . . . . ? O4 V2 N4 C33 -108.2(5) . . . . ? N8 V2 N4 C33 175.1(5) . . . . ? N2 V1 N7 C42 -175.0(6) . . . . ? O3 V1 N7 C42 79.7(6) . . . . ? O2 V1 N7 C42 -73.1(6) . . . . ? N1 V1 N7 C42 2.2(6) . . . . ? N2 V1 N7 C41 63.0(6) . . . . ? O3 V1 N7 C41 -42.3(5) . . . . ? O2 V1 N7 C41 164.8(6) . . . . ? N1 V1 N7 C41 -119.8(5) . . . . ? N2 V1 N7 N8 -53.7(5) . . . . ? O3 V1 N7 N8 -159.0(5) . . . . ? O2 V1 N7 N8 48.2(4) . . . . ? N1 V1 N7 N8 123.5(4) . . . . ? C42 N7 N8 V2 -39.4(9) . . . . ? C41 N7 N8 V2 76.3(8) . . . . ? V1 N7 N8 V2 -165.6(4) . . . . ? N5 V2 N8 N7 36.1(7) . . . . ? O5 V2 N8 N7 -66.0(7) . . . . ? O6 V2 N8 N7 -174.2(11) . . . . ? O4 V2 N8 N7 137.3(7) . . . . ? N4 V2 N8 N7 -143.5(7) . . . . ? C13 N1 C1 C2 106.4(9) . . . . ? C7 N1 C1 C2 -118.7(8) . . . . ? V1 N1 C1 C2 -6.8(8) . . . . ? C13 N1 C1 C6 -75.4(11) . . . . ? C7 N1 C1 C6 59.4(11) . . . . ? V1 N1 C1 C6 171.4(8) . . . . ? V1 O1 C2 C1 7.5(11) . . . . ? V1 O1 C2 C3 -173.6(7) . . . . ? C6 C1 C2 O1 -177.3(8) . . . . ? N1 C1 C2 O1 0.9(12) . . . . ? C6 C1 C2 C3 3.7(13) . . . . ? N1 C1 C2 C3 -178.0(8) . . . . ? O1 C2 C3 F1A -2.8(13) . . . . ? C1 C2 C3 F1A 176.1(9) . . . . ? O1 C2 C3 C4 178.5(9) . . . . ? C1 C2 C3 C4 -2.5(14) . . . . ? F1A C3 C4 C5 -178.6(9) . . . . ? C2 C3 C4 C5 0.0(15) . . . . ? C3 C4 C5 C6 1.3(14) . . . . ? C2 C1 C6 C5 -2.5(15) . . . . ? N1 C1 C6 C5 179.4(8) . . . . ? C4 C5 C6 C1 -0.1(15) . . . . ? C13 N1 C7 C12 44.2(13) . . . . ? C1 N1 C7 C12 -87.8(11) . . . . ? V1 N1 C7 C12 160.5(8) . . . . ? C13 N1 C7 C8 -137.8(8) . . . . ? C1 N1 C7 C8 90.2(9) . . . . ? V1 N1 C7 C8 -21.5(9) . . . . ? V1 O2 C8 C9 -156.0(7) . . . . ? V1 O2 C8 C7 18.3(11) . . . . ? C12 C7 C8 O2 -175.8(8) . . . . ? N1 C7 C8 O2 6.1(13) . . . . ? C12 C7 C8 C9 -1.6(15) . . . . ? N1 C7 C8 C9 -179.7(8) . . . . ? O2 C8 C9 C10 175.5(8) . . . . ? C7 C8 C9 C10 1.2(14) . . . . ? C8 C9 C10 C11 -0.2(16) . . . . ? C9 C10 C11 C12 -0.6(17) . . . . ? C8 C7 C12 C11 0.8(15) . . . . ? N1 C7 C12 C11 178.6(9) . . . . ? C10 C11 C12 C7 0.2(15) . . . . ? C7 N1 C13 C18 -61.8(11) . . . . ? C1 N1 C13 C18 70.2(10) . . . . ? V1 N1 C13 C18 -177.5(7) . . . . ? C7 N1 C13 C14 122.6(8) . . . . ? C1 N1 C13 C14 -105.4(8) . . . . ? V1 N1 C13 C14 6.9(8) . . . . ? V1 O3 C14 C15 167.0(6) . . . . ? V1 O3 C14 C13 -9.9(10) . . . . ? C18 C13 C14 O3 -175.7(7) . . . . ? N1 C13 C14 O3 0.2(11) . . . . ? C18 C13 C14 C15 7.4(13) . . . . ? N1 C13 C14 C15 -176.7(8) . . . . ? O3 C14 C15 F1B -1.6(17) . . . . ? C13 C14 C15 F1B 175.3(13) . . . . ? O3 C14 C15 C16 177.4(8) . . . . ? C13 C14 C15 C16 -5.7(13) . . . . ? F1B C15 C16 C17 -178.9(12) . . . . ? C14 C15 C16 C17 2.0(13) . . . . ? C15 C16 C17 C18 0.2(13) . . . . ? C14 C13 C18 C17 -5.2(12) . . . . ? N1 C13 C18 C17 179.4(8) . . . . ? C16 C17 C18 C13 1.4(13) . . . . ? C27 N4 C21 C26 60.6(12) . . . . ? C33 N4 C21 C26 -69.0(10) . . . . ? V2 N4 C21 C26 177.4(8) . . . . ? C27 N4 C21 C22 -123.2(8) . . . . ? C33 N4 C21 C22 107.2(8) . . . . ? V2 N4 C21 C22 -6.4(8) . . . . ? V2 O4 C22 C23 -167.4(7) . . . . ? V2 O4 C22 C21 11.9(11) . . . . ? C26 C21 C22 O4 174.3(8) . . . . ? N4 C21 C22 O4 -2.1(12) . . . . ? C26 C21 C22 C23 -6.4(13) . . . . ? N4 C21 C22 C23 177.2(8) . . . . ? O4 C22 C23 F2A 3.3(15) . . . . ? C21 C22 C23 F2A -176.0(10) . . . . ? O4 C22 C23 C24 -177.1(8) . . . . ? C21 C22 C23 C24 3.7(14) . . . . ? F2A C23 C24 C25 178.7(10) . . . . ? C22 C23 C24 C25 -0.9(14) . . . . ? C23 C24 C25 C26 0.8(14) . . . . ? C24 C25 C26 C21 -3.5(14) . . . . ? C22 C21 C26 C25 6.3(13) . . . . ? N4 C21 C26 C25 -177.8(8) . . . . ? C21 N4 C27 C32 -40.6(12) . . . . ? C33 N4 C27 C32 89.0(10) . . . . ? V2 N4 C27 C32 -158.6(8) . . . . ? C21 N4 C27 C28 143.0(8) . . . . ? C33 N4 C27 C28 -87.5(8) . . . . ? V2 N4 C27 C28 24.9(8) . . . . ? V2 O5 C28 C29 156.1(6) . . . . ? V2 O5 C28 C27 -19.1(10) . . . . ? C32 C27 C28 O5 175.2(7) . . . . ? N4 C27 C28 O5 -8.0(11) . . . . ? C32 C27 C28 C29 0.2(13) . . . . ? N4 C27 C28 C29 177.0(8) . . . . ? O5 C28 C29 C30 -176.2(7) . . . . ? C27 C28 C29 C30 -1.2(13) . . . . ? C28 C29 C30 C31 1.3(12) . . . . ? C29 C30 C31 C32 -0.3(14) . . . . ? C28 C27 C32 C31 0.8(13) . . . . ? N4 C27 C32 C31 -175.4(8) . . . . ? C30 C31 C32 C27 -0.8(13) . . . . ? C27 N4 C33 C38 -54.5(11) . . . . ? C21 N4 C33 C38 78.6(10) . . . . ? V2 N4 C33 C38 -166.6(8) . . . . ? C27 N4 C33 C34 122.5(8) . . . . ? C21 N4 C33 C34 -104.4(8) . . . . ? V2 N4 C33 C34 10.4(8) . . . . ? V2 O6 C34 C35 171.8(7) . . . . ? V2 O6 C34 C33 -7.3(10) . . . . ? C38 C33 C34 O6 173.3(8) . . . . ? N4 C33 C34 O6 -3.8(11) . . . . ? C38 C33 C34 C35 -5.9(13) . . . . ? N4 C33 C34 C35 177.0(7) . . . . ? O6 C34 C35 F2B 6.6(16) . . . . ? C33 C34 C35 F2B -174.2(12) . . . . ? O6 C34 C35 C36 -174.4(9) . . . . ? C33 C34 C35 C36 4.8(13) . . . . ? C34 C35 C36 C37 -1.7(14) . . . . ? F2B C35 C36 C37 177.4(12) . . . . ? C35 C36 C37 C38 -0.6(13) . . . . ? C34 C33 C38 C37 3.9(14) . . . . ? N4 C33 C38 C37 -179.3(8) . . . . ? C36 C37 C38 C33 -0.5(14) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.468 _refine_diff_density_min -0.459 _refine_diff_density_rms 0.089 # start Validation Reply Form _vrf_PLAT213_4d ; PROBLEM: Atom C29 has ADP max/min Ratio ..... 11.3 prola RESPONSE: Such a max/min main axis ADP ratio was caused by the poor quality of the crystal analyzed. ; data_5b(CCDC-925609) _database_code_depnum_ccdc_archive 'CCDC 925609' #TrackingRef 'MoriuchiCIFCCDC925607_925609.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H22 N3 O3 V' _chemical_formula_sum 'C30 H22 N3 O3 V' _chemical_formula_weight 523.45 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 20.7200(15) _cell_length_b 9.1557(6) _cell_length_c 25.6467(18) _cell_angle_alpha 90.00 _cell_angle_beta 99.487(2) _cell_angle_gamma 90.00 _cell_volume 4798.8(6) _cell_formula_units_Z 8 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used 26273 _cell_measurement_theta_min 2.99 _cell_measurement_theta_max 27.47 _exptl_crystal_description platelet _exptl_crystal_colour brown _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2160 _exptl_absorpt_coefficient_mu 0.453 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8762 _exptl_absorpt_correction_T_max 0.9910 _exptl_absorpt_process_details ; Higashi, T. (1999). Abscor - Empirical Absorption Correction based on Fourier Series Approximation. Rigaku Corporation, Tokyo, Japan. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_radiation_detector 'imaging plate' _diffrn_measurement_device_type 'Rigaku R-AXIS RAPID' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 10.00 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 54207 _diffrn_reflns_av_R_equivalents 0.2158 _diffrn_reflns_av_sigmaI/netI 0.1333 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -10 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8399 _reflns_number_gt 4451 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Rigaku/RAPID Diffractometer Control' _computing_cell_refinement 'Rigaku/RAPID Diffractometer Control' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_publication_material 'SHELXL-97 and modified' _computing_molecular_graphics ? _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^)+(0.0740P)^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 8399 _refine_ls_number_parameters 667 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1421 _refine_ls_R_factor_gt 0.0662 _refine_ls_wR_factor_ref 0.1766 _refine_ls_wR_factor_gt 0.1352 _refine_ls_goodness_of_fit_ref 0.982 _refine_ls_restrained_S_all 0.982 _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 0.33687(4) 0.32309(10) 0.60527(4) 0.0298(3) Uani 1 1 d . . . V2 V 0.11334(4) 1.12143(10) 0.34987(3) 0.0289(3) Uani 1 1 d . . . O1 O 0.29435(16) 0.4487(4) 0.55495(13) 0.0308(8) Uani 1 1 d . . . O2 O 0.34402(16) 0.3535(4) 0.67710(13) 0.0346(9) Uani 1 1 d . . . O3 O 0.40666(15) 0.2265(4) 0.58439(13) 0.0309(8) Uani 1 1 d . . . O4 O 0.11647(16) 1.1270(4) 0.27902(13) 0.0331(9) Uani 1 1 d . . . O5 O 0.18022(15) 1.2143(3) 0.39447(13) 0.0299(8) Uani 1 1 d . . . O6 O 0.07920(16) 0.9675(4) 0.38232(14) 0.0352(9) Uani 1 1 d . . . N1 N 0.40965(19) 0.5082(4) 0.61541(15) 0.0250(10) Uani 1 1 d . . . N2 N 0.28370(18) 0.1833(4) 0.60275(16) 0.0277(10) Uani 1 1 d . . . N3 N 0.2413(2) 0.0783(5) 0.60604(16) 0.0309(10) Uani 1 1 d . . . N4 N 0.19474(19) 0.9580(4) 0.34618(16) 0.0259(10) Uani 1 1 d . . . N5 N 0.05527(18) 1.2522(4) 0.34802(16) 0.0277(10) Uani 1 1 d . . . N6 N 0.01588(19) 1.3619(5) 0.33207(16) 0.0310(10) Uani 1 1 d . . . C1 C 0.3745(2) 0.6288(5) 0.5859(2) 0.0273(12) Uani 1 1 d . . . C2 C 0.3163(3) 0.5909(6) 0.5540(2) 0.0307(13) Uani 1 1 d . . . C3 C 0.2807(2) 0.6924(6) 0.5215(2) 0.0321(13) Uani 1 1 d . . . H3 H 0.2420 0.6644 0.4984 0.039 Uiso 1 1 calc R . . C4 C 0.3022(3) 0.8360(6) 0.5229(2) 0.0333(13) Uani 1 1 d . . . H4 H 0.2781 0.9068 0.5006 0.040 Uiso 1 1 calc R . . C5 C 0.3586(2) 0.8767(6) 0.5565(2) 0.0325(13) Uani 1 1 d . . . H5 H 0.3726 0.9757 0.5579 0.039 Uiso 1 1 calc R . . C6 C 0.3944(3) 0.7736(6) 0.5881(2) 0.0344(13) Uani 1 1 d . . . H6 H 0.4328 0.8019 0.6114 0.041 Uiso 1 1 calc R . . C7 C 0.4267(2) 0.5291(5) 0.6723(2) 0.0291(12) Uani 1 1 d . . . C8 C 0.3899(2) 0.4476(6) 0.7024(2) 0.0300(12) Uani 1 1 d . . . C9 C 0.4000(3) 0.4606(6) 0.7569(2) 0.0354(13) Uani 1 1 d . . . H9 H 0.3737 0.4073 0.7772 0.042 Uiso 1 1 calc R . . C10 C 0.4489(3) 0.5521(6) 0.7815(2) 0.0392(14) Uani 1 1 d . . . H10 H 0.4562 0.5612 0.8189 0.047 Uiso 1 1 calc R . . C11 C 0.4872(2) 0.6302(6) 0.7520(2) 0.0366(14) Uani 1 1 d . . . H11 H 0.5210 0.6917 0.7693 0.044 Uiso 1 1 calc R . . C12 C 0.4766(2) 0.6194(5) 0.6975(2) 0.0309(12) Uani 1 1 d . . . H12 H 0.5030 0.6730 0.6773 0.037 Uiso 1 1 calc R . . C13 C 0.4643(2) 0.4539(5) 0.59034(19) 0.0265(12) Uani 1 1 d . . . C14 C 0.4593(2) 0.3069(6) 0.57556(19) 0.0275(12) Uani 1 1 d . . . C15 C 0.5074(2) 0.2433(6) 0.55154(19) 0.0303(12) Uani 1 1 d . . . H15 H 0.5041 0.1435 0.5413 0.036 Uiso 1 1 calc R . . C16 C 0.5607(2) 0.3268(6) 0.5426(2) 0.0350(13) Uani 1 1 d . . . H16 H 0.5941 0.2835 0.5264 0.042 Uiso 1 1 calc R . . C17 C 0.5652(2) 0.4730(6) 0.5572(2) 0.0326(13) Uani 1 1 d . . . H17 H 0.6017 0.5295 0.5511 0.039 Uiso 1 1 calc R . . C18 C 0.5166(2) 0.5362(6) 0.5806(2) 0.0293(12) Uani 1 1 d . . . H18 H 0.5192 0.6366 0.5900 0.035 Uiso 1 1 calc R . . C19 C 0.1770(2) 0.0920(5) 0.5754(2) 0.0275(12) Uani 1 1 d . . . C20 C 0.1703(3) 0.1665(6) 0.5275(2) 0.0334(13) Uani 1 1 d . . . H20 H 0.2078 0.1996 0.5141 0.040 Uiso 1 1 calc R . . C21 C 0.1084(3) 0.1916(6) 0.4999(2) 0.0344(13) Uani 1 1 d . . . H21 H 0.1032 0.2431 0.4673 0.041 Uiso 1 1 calc R . . C22 C 0.0535(3) 0.1425(6) 0.5193(2) 0.0351(13) Uani 1 1 d . . . H22 H 0.0109 0.1605 0.5001 0.042 Uiso 1 1 calc R . . C23 C 0.0610(3) 0.0680(6) 0.5662(2) 0.0346(13) Uani 1 1 d . . . H23 H 0.0234 0.0345 0.5794 0.041 Uiso 1 1 calc R . . C24 C 0.1227(2) 0.0405(5) 0.5948(2) 0.0294(12) Uani 1 1 d . . . H24 H 0.1276 -0.0126 0.6270 0.035 Uiso 1 1 calc R . . C25 C 0.2565(2) -0.0276(6) 0.6479(2) 0.0283(12) Uani 1 1 d . . . C26 C 0.2905(2) 0.0177(6) 0.6960(2) 0.0364(14) Uani 1 1 d . . . H26 H 0.3027 0.1172 0.7018 0.044 Uiso 1 1 calc R . . C27 C 0.3065(3) -0.0849(7) 0.7358(2) 0.0476(16) Uani 1 1 d . . . H27 H 0.3298 -0.0551 0.7691 0.057 Uiso 1 1 calc R . . C28 C 0.2893(3) -0.2291(7) 0.7277(3) 0.0522(17) Uani 1 1 d . . . H28 H 0.3012 -0.2987 0.7550 0.063 Uiso 1 1 calc R . . C29 C 0.2544(3) -0.2722(6) 0.6793(2) 0.0416(15) Uani 1 1 d . . . H29 H 0.2415 -0.3713 0.6738 0.050 Uiso 1 1 calc R . . C30 C 0.2381(2) -0.1721(6) 0.6389(2) 0.0359(13) Uani 1 1 d . . . H30 H 0.2148 -0.2019 0.6056 0.043 Uiso 1 1 calc R . . C31 C 0.1977(2) 0.9431(5) 0.2895(2) 0.0273(12) Uani 1 1 d . . . C32 C 0.1544(2) 1.0322(5) 0.2565(2) 0.0287(12) Uani 1 1 d . . . C33 C 0.1490(3) 1.0211(6) 0.2021(2) 0.0351(13) Uani 1 1 d . . . H33 H 0.1178 1.0783 0.1796 0.042 Uiso 1 1 calc R . . C34 C 0.1891(3) 0.9270(6) 0.1810(2) 0.0394(14) Uani 1 1 d . . . H34 H 0.1855 0.9198 0.1437 0.047 Uiso 1 1 calc R . . C35 C 0.2345(3) 0.8423(6) 0.2130(2) 0.0415(15) Uani 1 1 d . . . H35 H 0.2628 0.7794 0.1978 0.050 Uiso 1 1 calc R . . C36 C 0.2387(3) 0.8496(6) 0.2674(2) 0.0395(14) Uani 1 1 d . . . H36 H 0.2696 0.7908 0.2896 0.047 Uiso 1 1 calc R . . C37 C 0.2523(2) 1.0226(5) 0.3787(2) 0.0277(12) Uani 1 1 d . . . C38 C 0.2408(2) 1.1524(5) 0.40423(19) 0.0266(12) Uani 1 1 d . . . C39 C 0.2906(2) 1.2186(6) 0.43922(19) 0.0302(12) Uani 1 1 d . . . H39 H 0.2823 1.3051 0.4575 0.036 Uiso 1 1 calc R . . C40 C 0.3529(2) 1.1570(6) 0.4472(2) 0.0328(13) Uani 1 1 d . . . H40 H 0.3872 1.2018 0.4710 0.039 Uiso 1 1 calc R . . C41 C 0.3649(2) 1.0314(6) 0.4209(2) 0.0357(14) Uani 1 1 d . . . H41 H 0.4077 0.9911 0.4259 0.043 Uiso 1 1 calc R . . C42 C 0.3147(2) 0.9637(6) 0.3871(2) 0.0344(13) Uani 1 1 d . . . H42 H 0.3231 0.8760 0.3696 0.041 Uiso 1 1 calc R . . C43 C 0.1720(2) 0.8251(5) 0.3698(2) 0.0294(12) Uani 1 1 d . . . C44 C 0.1123(3) 0.8375(6) 0.3879(2) 0.0319(13) Uani 1 1 d . . . C45 C 0.0860(3) 0.7176(6) 0.4102(2) 0.0401(14) Uani 1 1 d . . . H45 H 0.0448 0.7249 0.4216 0.048 Uiso 1 1 calc R . . C46 C 0.1203(3) 0.5881(6) 0.4157(2) 0.0416(15) Uani 1 1 d . . . H46 H 0.1028 0.5069 0.4317 0.050 Uiso 1 1 calc R . . C47 C 0.1798(3) 0.5742(6) 0.3983(2) 0.0413(15) Uani 1 1 d . . . H47 H 0.2026 0.4839 0.4021 0.050 Uiso 1 1 calc R . . C48 C 0.2057(3) 0.6928(6) 0.3754(2) 0.0367(14) Uani 1 1 d . . . H48 H 0.2466 0.6840 0.3634 0.044 Uiso 1 1 calc R . . C49 C 0.0204(2) 1.4209(6) 0.2808(2) 0.0318(13) Uani 1 1 d . . . C50 C 0.0793(3) 1.4800(6) 0.2726(2) 0.0398(14) Uani 1 1 d . . . H50 H 0.1151 1.4867 0.3008 0.048 Uiso 1 1 calc R . . C51 C 0.0855(3) 1.5296(6) 0.2223(2) 0.0467(16) Uani 1 1 d . . . H51 H 0.1256 1.5706 0.2160 0.056 Uiso 1 1 calc R . . C52 C 0.0332(3) 1.5187(6) 0.1820(2) 0.0446(15) Uani 1 1 d . . . H52 H 0.0373 1.5518 0.1476 0.054 Uiso 1 1 calc R . . C53 C -0.0253(3) 1.4602(6) 0.1910(2) 0.0387(14) Uani 1 1 d . . . H53 H -0.0614 1.4546 0.1629 0.046 Uiso 1 1 calc R . . C54 C -0.0317(3) 1.4096(6) 0.2407(2) 0.0370(14) Uani 1 1 d . . . H54 H -0.0717 1.3676 0.2469 0.044 Uiso 1 1 calc R . . C55 C -0.0336(2) 1.4021(6) 0.36202(19) 0.0279(12) Uani 1 1 d . . . C56 C -0.0470(2) 1.3114(6) 0.4015(2) 0.0318(13) Uani 1 1 d . . . H56 H -0.0240 1.2219 0.4085 0.038 Uiso 1 1 calc R . . C57 C -0.0942(2) 1.3514(6) 0.4310(2) 0.0398(14) Uani 1 1 d . . . H57 H -0.1033 1.2894 0.4586 0.048 Uiso 1 1 calc R . . C58 C -0.1285(3) 1.4809(6) 0.4207(2) 0.0399(14) Uani 1 1 d . . . H58 H -0.1614 1.5073 0.4407 0.048 Uiso 1 1 calc R . . C59 C -0.1143(3) 1.5717(6) 0.3808(2) 0.0390(14) Uani 1 1 d . . . H59 H -0.1379 1.6602 0.3732 0.047 Uiso 1 1 calc R . . C60 C -0.0658(2) 1.5341(6) 0.3519(2) 0.0330(13) Uani 1 1 d . . . H60 H -0.0548 1.5981 0.3255 0.040 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 0.0241(5) 0.0330(5) 0.0311(5) -0.0011(4) 0.0011(4) -0.0025(4) V2 0.0228(5) 0.0337(5) 0.0290(5) 0.0019(4) 0.0006(4) 0.0024(4) O1 0.028(2) 0.030(2) 0.032(2) 0.0022(17) -0.0017(16) -0.0016(16) O2 0.033(2) 0.041(2) 0.030(2) -0.0017(18) 0.0061(17) -0.0108(17) O3 0.0228(19) 0.034(2) 0.036(2) -0.0047(17) 0.0032(16) -0.0039(16) O4 0.032(2) 0.039(2) 0.025(2) 0.0002(17) -0.0034(16) 0.0087(17) O5 0.0216(19) 0.0295(19) 0.037(2) -0.0006(17) 0.0003(16) 0.0009(15) O6 0.026(2) 0.036(2) 0.044(2) 0.0067(18) 0.0054(17) 0.0046(17) N1 0.026(2) 0.030(2) 0.019(2) -0.0009(19) 0.0020(18) 0.0029(19) N2 0.020(2) 0.030(2) 0.034(3) -0.004(2) 0.0058(19) -0.0094(19) N3 0.029(2) 0.035(3) 0.029(3) -0.003(2) 0.005(2) -0.002(2) N4 0.026(2) 0.027(2) 0.023(2) -0.0019(19) 0.0005(19) -0.0022(19) N5 0.022(2) 0.031(2) 0.029(2) 0.000(2) 0.0017(19) 0.0089(19) N6 0.026(2) 0.037(3) 0.029(3) 0.006(2) 0.000(2) 0.006(2) C1 0.026(3) 0.026(3) 0.029(3) 0.002(2) 0.004(2) 0.001(2) C2 0.037(3) 0.031(3) 0.026(3) 0.000(3) 0.012(3) -0.003(3) C3 0.028(3) 0.037(3) 0.029(3) 0.001(3) 0.001(2) 0.005(3) C4 0.037(3) 0.036(3) 0.028(3) 0.003(3) 0.008(3) 0.007(3) C5 0.033(3) 0.030(3) 0.034(3) -0.003(3) 0.006(3) 0.000(2) C6 0.027(3) 0.044(3) 0.032(3) 0.000(3) 0.003(2) 0.001(3) C7 0.021(3) 0.035(3) 0.029(3) -0.005(3) -0.001(2) 0.003(2) C8 0.022(3) 0.037(3) 0.030(3) -0.006(3) 0.003(2) 0.001(2) C9 0.038(3) 0.042(3) 0.026(3) -0.001(3) 0.006(3) -0.001(3) C10 0.032(3) 0.054(4) 0.030(3) -0.004(3) -0.001(3) 0.001(3) C11 0.027(3) 0.044(3) 0.036(3) -0.010(3) -0.003(3) -0.004(3) C12 0.029(3) 0.034(3) 0.028(3) -0.004(3) 0.001(2) 0.000(2) C13 0.026(3) 0.033(3) 0.020(3) -0.002(2) 0.003(2) 0.000(2) C14 0.022(3) 0.032(3) 0.026(3) 0.002(2) -0.003(2) -0.004(2) C15 0.030(3) 0.031(3) 0.029(3) -0.003(2) 0.002(2) -0.002(2) C16 0.024(3) 0.045(4) 0.036(3) 0.000(3) 0.003(2) 0.005(3) C17 0.028(3) 0.038(3) 0.031(3) 0.002(3) 0.003(2) -0.004(3) C18 0.020(3) 0.033(3) 0.034(3) 0.000(3) 0.001(2) -0.004(2) C19 0.024(3) 0.029(3) 0.028(3) -0.003(2) 0.002(2) 0.000(2) C20 0.032(3) 0.040(3) 0.030(3) 0.000(3) 0.010(3) -0.003(3) C21 0.036(3) 0.038(3) 0.028(3) -0.001(3) 0.000(3) 0.000(3) C22 0.027(3) 0.041(3) 0.035(3) -0.003(3) -0.002(3) -0.002(3) C23 0.029(3) 0.036(3) 0.036(3) 0.001(3) -0.002(3) -0.006(2) C24 0.028(3) 0.035(3) 0.025(3) 0.003(2) 0.007(2) -0.004(2) C25 0.022(3) 0.036(3) 0.028(3) 0.001(3) 0.006(2) 0.002(2) C26 0.031(3) 0.037(3) 0.039(4) 0.003(3) 0.001(3) -0.005(3) C27 0.045(4) 0.050(4) 0.042(4) 0.011(3) -0.012(3) -0.008(3) C28 0.040(4) 0.055(4) 0.061(5) 0.021(4) 0.005(3) 0.007(3) C29 0.045(4) 0.026(3) 0.053(4) 0.002(3) 0.005(3) 0.000(3) C30 0.033(3) 0.033(3) 0.042(4) -0.001(3) 0.007(3) 0.002(3) C31 0.030(3) 0.021(3) 0.031(3) -0.003(2) 0.005(2) 0.000(2) C32 0.020(3) 0.032(3) 0.034(3) -0.004(3) 0.004(2) 0.003(2) C33 0.035(3) 0.041(3) 0.028(3) -0.002(3) 0.001(3) -0.002(3) C34 0.043(4) 0.049(4) 0.027(3) -0.009(3) 0.008(3) -0.004(3) C35 0.044(4) 0.047(4) 0.034(3) -0.011(3) 0.007(3) 0.011(3) C36 0.043(3) 0.041(3) 0.033(3) -0.004(3) 0.002(3) 0.014(3) C37 0.023(3) 0.029(3) 0.031(3) 0.006(2) 0.004(2) 0.001(2) C38 0.019(3) 0.032(3) 0.028(3) 0.004(2) 0.001(2) -0.003(2) C39 0.029(3) 0.039(3) 0.021(3) -0.001(2) 0.000(2) -0.004(2) C40 0.025(3) 0.040(3) 0.030(3) 0.010(3) -0.004(2) -0.003(2) C41 0.021(3) 0.044(3) 0.040(4) 0.010(3) -0.003(3) 0.001(3) C42 0.029(3) 0.035(3) 0.039(3) 0.004(3) 0.003(3) 0.004(3) C43 0.032(3) 0.026(3) 0.029(3) 0.001(2) 0.003(2) -0.003(2) C44 0.034(3) 0.035(3) 0.024(3) 0.001(3) -0.003(2) -0.005(3) C45 0.038(3) 0.040(3) 0.041(4) 0.006(3) 0.006(3) -0.004(3) C46 0.048(4) 0.032(3) 0.041(4) 0.002(3) -0.003(3) -0.014(3) C47 0.045(4) 0.033(3) 0.042(4) 0.004(3) -0.005(3) 0.000(3) C48 0.037(3) 0.036(3) 0.035(3) 0.001(3) -0.003(3) 0.004(3) C49 0.027(3) 0.037(3) 0.031(3) 0.003(3) 0.003(2) 0.008(2) C50 0.026(3) 0.051(4) 0.041(4) 0.005(3) 0.000(3) 0.007(3) C51 0.039(4) 0.056(4) 0.048(4) 0.017(3) 0.015(3) 0.005(3) C52 0.050(4) 0.049(4) 0.038(4) 0.004(3) 0.013(3) 0.016(3) C53 0.047(4) 0.034(3) 0.032(3) -0.005(3) -0.003(3) 0.006(3) C54 0.037(3) 0.042(3) 0.029(3) 0.004(3) -0.004(3) 0.001(3) C55 0.019(3) 0.037(3) 0.026(3) -0.003(3) -0.004(2) 0.002(2) C56 0.027(3) 0.037(3) 0.030(3) 0.002(3) -0.001(2) -0.001(2) C57 0.027(3) 0.056(4) 0.036(3) 0.001(3) 0.005(3) -0.005(3) C58 0.032(3) 0.050(4) 0.038(4) -0.013(3) 0.007(3) 0.001(3) C59 0.033(3) 0.038(3) 0.045(4) -0.007(3) 0.002(3) 0.005(3) C60 0.033(3) 0.030(3) 0.035(3) 0.001(3) 0.003(3) 0.000(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 N2 1.683(4) . ? V1 O1 1.841(3) . ? V1 O2 1.845(3) . ? V1 O3 1.848(3) . ? V1 N1 2.255(4) . ? V2 N5 1.692(4) . ? V2 O4 1.830(3) . ? V2 O6 1.836(3) . ? V2 O5 1.852(3) . ? V2 N4 2.268(4) . ? O1 C2 1.380(6) . ? O2 C8 1.365(6) . ? O3 C14 1.365(5) . ? O4 C32 1.361(5) . ? O5 C38 1.361(5) . ? O6 C44 1.369(6) . ? N1 C7 1.456(6) . ? N1 C1 1.463(6) . ? N1 C13 1.478(6) . ? N2 N3 1.315(5) . ? N3 C19 1.435(6) . ? N3 C25 1.442(6) . ? N4 C37 1.462(6) . ? N4 C31 1.471(6) . ? N4 C43 1.472(6) . ? N5 N6 1.316(5) . ? N6 C55 1.427(6) . ? N6 C49 1.439(6) . ? C1 C2 1.386(7) . ? C1 C6 1.386(7) . ? C2 C3 1.378(7) . ? C3 C4 1.386(7) . ? C3 H3 0.9500 . ? C4 C5 1.384(7) . ? C4 H4 0.9500 . ? C5 C6 1.378(7) . ? C5 H5 0.9500 . ? C6 H6 0.9500 . ? C7 C8 1.389(7) . ? C7 C12 1.395(7) . ? C8 C9 1.384(7) . ? C9 C10 1.384(7) . ? C9 H9 0.9500 . ? C10 C11 1.382(7) . ? C10 H10 0.9500 . ? C11 C12 1.383(7) . ? C11 H11 0.9500 . ? C12 H12 0.9500 . ? C13 C18 1.375(6) . ? C13 C14 1.397(7) . ? C14 C15 1.385(7) . ? C15 C16 1.393(7) . ? C15 H15 0.9500 . ? C16 C17 1.389(7) . ? C16 H16 0.9500 . ? C17 C18 1.382(7) . ? C17 H17 0.9500 . ? C18 H18 0.9500 . ? C19 C24 1.386(6) . ? C19 C20 1.391(7) . ? C20 C21 1.379(7) . ? C20 H20 0.9500 . ? C21 C22 1.389(7) . ? C21 H21 0.9500 . ? C22 C23 1.369(7) . ? C22 H22 0.9500 . ? C23 C24 1.388(7) . ? C23 H23 0.9500 . ? C24 H24 0.9500 . ? C25 C26 1.380(7) . ? C25 C30 1.386(7) . ? C26 C27 1.386(7) . ? C26 H26 0.9500 . ? C27 C28 1.375(8) . ? C27 H27 0.9500 . ? C28 C29 1.387(8) . ? C28 H28 0.9500 . ? C29 C30 1.382(7) . ? C29 H29 0.9500 . ? C30 H30 0.9500 . ? C31 C32 1.391(7) . ? C31 C36 1.392(7) . ? C32 C33 1.386(7) . ? C33 C34 1.368(7) . ? C33 H33 0.9500 . ? C34 C35 1.381(7) . ? C34 H34 0.9500 . ? C35 C36 1.385(7) . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? C37 C42 1.385(7) . ? C37 C38 1.397(7) . ? C38 C39 1.391(7) . ? C39 C40 1.391(7) . ? C39 H39 0.9500 . ? C40 C41 1.377(7) . ? C40 H40 0.9500 . ? C41 C42 1.386(7) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.395(7) . ? C43 C48 1.395(7) . ? C44 C45 1.390(7) . ? C45 C46 1.377(7) . ? C45 H45 0.9500 . ? C46 C47 1.385(7) . ? C46 H46 0.9500 . ? C47 C48 1.385(7) . ? C47 H47 0.9500 . ? C48 H48 0.9500 . ? C49 C54 1.367(7) . ? C49 C50 1.382(7) . ? C50 C51 1.392(7) . ? C50 H50 0.9500 . ? C51 C52 1.373(8) . ? C51 H51 0.9500 . ? C52 C53 1.379(7) . ? C52 H52 0.9500 . ? C53 C54 1.383(7) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C55 C56 1.374(7) . ? C55 C60 1.385(7) . ? C56 C57 1.379(7) . ? C56 H56 0.9500 . ? C57 C58 1.386(7) . ? C57 H57 0.9500 . ? C58 C59 1.387(7) . ? C58 H58 0.9500 . ? C59 C60 1.387(7) . ? C59 H59 0.9500 . ? C60 H60 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 V1 O1 102.33(18) . . ? N2 V1 O2 95.59(17) . . ? O1 V1 O2 123.79(16) . . ? N2 V1 O3 99.42(17) . . ? O1 V1 O3 113.74(15) . . ? O2 V1 O3 115.06(16) . . ? N2 V1 N1 175.63(18) . . ? O1 V1 N1 81.08(14) . . ? O2 V1 N1 80.18(14) . . ? O3 V1 N1 81.52(14) . . ? N5 V2 O4 95.39(17) . . ? N5 V2 O6 103.30(17) . . ? O4 V2 O6 123.42(16) . . ? N5 V2 O5 98.56(17) . . ? O4 V2 O5 117.08(15) . . ? O6 V2 O5 112.16(16) . . ? N5 V2 N4 174.57(17) . . ? O4 V2 N4 80.12(14) . . ? O6 V2 N4 81.81(14) . . ? O5 V2 N4 80.95(14) . . ? C2 O1 V1 118.7(3) . . ? C8 O2 V1 120.3(3) . . ? C14 O3 V1 118.3(3) . . ? C32 O4 V2 121.4(3) . . ? C38 O5 V2 119.7(3) . . ? C44 O6 V2 119.4(3) . . ? C7 N1 C1 115.9(4) . . ? C7 N1 C13 113.8(4) . . ? C1 N1 C13 112.4(4) . . ? C7 N1 V1 105.2(3) . . ? C1 N1 V1 104.0(3) . . ? C13 N1 V1 104.1(3) . . ? N3 N2 V1 173.7(4) . . ? N2 N3 C19 118.1(4) . . ? N2 N3 C25 118.2(4) . . ? C19 N3 C25 122.4(4) . . ? C37 N4 C31 115.9(4) . . ? C37 N4 C43 112.8(4) . . ? C31 N4 C43 113.5(4) . . ? C37 N4 V2 104.6(3) . . ? C31 N4 V2 104.8(3) . . ? C43 N4 V2 103.7(3) . . ? N6 N5 V2 161.8(3) . . ? N5 N6 C55 119.6(4) . . ? N5 N6 C49 116.1(4) . . ? C55 N6 C49 123.8(4) . . ? C2 C1 C6 119.1(5) . . ? C2 C1 N1 115.3(4) . . ? C6 C1 N1 125.6(5) . . ? C3 C2 O1 120.1(5) . . ? C3 C2 C1 121.0(5) . . ? O1 C2 C1 118.9(5) . . ? C2 C3 C4 119.1(5) . . ? C2 C3 H3 120.5 . . ? C4 C3 H3 120.5 . . ? C5 C4 C3 120.4(5) . . ? C5 C4 H4 119.8 . . ? C3 C4 H4 119.8 . . ? C6 C5 C4 119.9(5) . . ? C6 C5 H5 120.1 . . ? C4 C5 H5 120.1 . . ? C5 C6 C1 120.3(5) . . ? C5 C6 H6 119.9 . . ? C1 C6 H6 119.9 . . ? C8 C7 C12 119.6(5) . . ? C8 C7 N1 114.9(4) . . ? C12 C7 N1 125.5(5) . . ? O2 C8 C9 120.8(5) . . ? O2 C8 C7 118.6(4) . . ? C9 C8 C7 120.6(5) . . ? C8 C9 C10 119.4(5) . . ? C8 C9 H9 120.3 . . ? C10 C9 H9 120.3 . . ? C11 C10 C9 120.4(5) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 120.4(5) . . ? C10 C11 H11 119.8 . . ? C12 C11 H11 119.8 . . ? C11 C12 C7 119.5(5) . . ? C11 C12 H12 120.2 . . ? C7 C12 H12 120.2 . . ? C18 C13 C14 120.3(5) . . ? C18 C13 N1 125.3(4) . . ? C14 C13 N1 114.4(4) . . ? O3 C14 C15 120.0(4) . . ? O3 C14 C13 120.1(4) . . ? C15 C14 C13 119.9(5) . . ? C14 C15 C16 119.4(5) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C17 C16 C15 120.3(5) . . ? C17 C16 H16 119.8 . . ? C15 C16 H16 119.8 . . ? C18 C17 C16 119.9(5) . . ? C18 C17 H17 120.0 . . ? C16 C17 H17 120.0 . . ? C13 C18 C17 120.1(5) . . ? C13 C18 H18 120.0 . . ? C17 C18 H18 120.0 . . ? C24 C19 C20 120.9(5) . . ? C24 C19 N3 120.5(5) . . ? C20 C19 N3 118.4(4) . . ? C21 C20 C19 119.0(5) . . ? C21 C20 H20 120.5 . . ? C19 C20 H20 120.5 . . ? C20 C21 C22 120.7(5) . . ? C20 C21 H21 119.7 . . ? C22 C21 H21 119.7 . . ? C23 C22 C21 119.6(5) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C22 C23 C24 121.1(5) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C19 C24 C23 118.7(5) . . ? C19 C24 H24 120.7 . . ? C23 C24 H24 120.7 . . ? C26 C25 C30 121.4(5) . . ? C26 C25 N3 118.7(5) . . ? C30 C25 N3 119.9(5) . . ? C25 C26 C27 118.6(5) . . ? C25 C26 H26 120.7 . . ? C27 C26 H26 120.7 . . ? C28 C27 C26 121.0(6) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 119.5(6) . . ? C27 C28 H28 120.2 . . ? C29 C28 H28 120.2 . . ? C30 C29 C28 120.6(5) . . ? C30 C29 H29 119.7 . . ? C28 C29 H29 119.7 . . ? C29 C30 C25 118.9(5) . . ? C29 C30 H30 120.6 . . ? C25 C30 H30 120.6 . . ? C32 C31 C36 119.3(5) . . ? C32 C31 N4 114.7(4) . . ? C36 C31 N4 126.0(5) . . ? O4 C32 C33 121.2(5) . . ? O4 C32 C31 118.4(5) . . ? C33 C32 C31 120.4(5) . . ? C34 C33 C32 119.5(5) . . ? C34 C33 H33 120.3 . . ? C32 C33 H33 120.3 . . ? C33 C34 C35 121.1(5) . . ? C33 C34 H34 119.4 . . ? C35 C34 H34 119.4 . . ? C34 C35 C36 119.7(5) . . ? C34 C35 H35 120.2 . . ? C36 C35 H35 120.2 . . ? C35 C36 C31 119.9(5) . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? C42 C37 C38 119.0(5) . . ? C42 C37 N4 125.7(5) . . ? C38 C37 N4 115.2(4) . . ? O5 C38 C39 120.1(5) . . ? O5 C38 C37 119.4(4) . . ? C39 C38 C37 120.5(4) . . ? C38 C39 C40 119.4(5) . . ? C38 C39 H39 120.3 . . ? C40 C39 H39 120.3 . . ? C41 C40 C39 120.3(5) . . ? C41 C40 H40 119.9 . . ? C39 C40 H40 119.9 . . ? C40 C41 C42 120.2(5) . . ? C40 C41 H41 119.9 . . ? C42 C41 H41 119.9 . . ? C37 C42 C41 120.6(5) . . ? C37 C42 H42 119.7 . . ? C41 C42 H42 119.7 . . ? C44 C43 C48 119.6(5) . . ? C44 C43 N4 115.6(4) . . ? C48 C43 N4 124.8(4) . . ? O6 C44 C45 120.4(5) . . ? O6 C44 C43 119.5(4) . . ? C45 C44 C43 120.1(5) . . ? C46 C45 C44 119.5(5) . . ? C46 C45 H45 120.2 . . ? C44 C45 H45 120.2 . . ? C45 C46 C47 121.1(5) . . ? C45 C46 H46 119.4 . . ? C47 C46 H46 119.4 . . ? C46 C47 C48 119.6(5) . . ? C46 C47 H47 120.2 . . ? C48 C47 H47 120.2 . . ? C47 C48 C43 120.0(5) . . ? C47 C48 H48 120.0 . . ? C43 C48 H48 120.0 . . ? C54 C49 C50 121.5(5) . . ? C54 C49 N6 119.8(5) . . ? C50 C49 N6 118.6(5) . . ? C49 C50 C51 119.2(5) . . ? C49 C50 H50 120.4 . . ? C51 C50 H50 120.4 . . ? C52 C51 C50 119.5(5) . . ? C52 C51 H51 120.2 . . ? C50 C51 H51 120.2 . . ? C51 C52 C53 120.5(6) . . ? C51 C52 H52 119.7 . . ? C53 C52 H52 119.7 . . ? C52 C53 C54 120.3(5) . . ? C52 C53 H53 119.8 . . ? C54 C53 H53 119.8 . . ? C49 C54 C53 119.0(5) . . ? C49 C54 H54 120.5 . . ? C53 C54 H54 120.5 . . ? C56 C55 C60 121.1(5) . . ? C56 C55 N6 119.5(4) . . ? C60 C55 N6 119.4(4) . . ? C55 C56 C57 119.5(5) . . ? C55 C56 H56 120.3 . . ? C57 C56 H56 120.3 . . ? C56 C57 C58 120.6(5) . . ? C56 C57 H57 119.7 . . ? C58 C57 H57 119.7 . . ? C57 C58 C59 119.3(5) . . ? C57 C58 H58 120.4 . . ? C59 C58 H58 120.4 . . ? C60 C59 C58 120.4(5) . . ? C60 C59 H59 119.8 . . ? C58 C59 H59 119.8 . . ? C55 C60 C59 119.0(5) . . ? C55 C60 H60 120.5 . . ? C59 C60 H60 120.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 V1 O1 C2 165.5(3) . . . . ? O2 V1 O1 C2 60.1(4) . . . . ? O3 V1 O1 C2 -88.3(3) . . . . ? N1 V1 O1 C2 -11.7(3) . . . . ? N2 V1 O2 C8 171.3(4) . . . . ? O1 V1 O2 C8 -79.8(4) . . . . ? O3 V1 O2 C8 68.2(4) . . . . ? N1 V1 O2 C8 -7.6(3) . . . . ? N2 V1 O3 C14 172.9(3) . . . . ? O1 V1 O3 C14 64.9(4) . . . . ? O2 V1 O3 C14 -86.3(3) . . . . ? N1 V1 O3 C14 -11.4(3) . . . . ? N5 V2 O4 C32 -175.7(4) . . . . ? O6 V2 O4 C32 -65.8(4) . . . . ? O5 V2 O4 C32 81.9(4) . . . . ? N4 V2 O4 C32 7.4(3) . . . . ? N5 V2 O5 C38 -174.5(3) . . . . ? O4 V2 O5 C38 -73.9(4) . . . . ? O6 V2 O5 C38 77.3(3) . . . . ? N4 V2 O5 C38 0.0(3) . . . . ? N5 V2 O6 C44 176.3(3) . . . . ? O4 V2 O6 C44 70.6(4) . . . . ? O5 V2 O6 C44 -78.5(4) . . . . ? N4 V2 O6 C44 -1.8(3) . . . . ? O1 V1 N1 C7 134.6(3) . . . . ? O2 V1 N1 C7 7.9(3) . . . . ? O3 V1 N1 C7 -109.5(3) . . . . ? O1 V1 N1 C1 12.4(3) . . . . ? O2 V1 N1 C1 -114.4(3) . . . . ? O3 V1 N1 C1 128.2(3) . . . . ? O1 V1 N1 C13 -105.5(3) . . . . ? O2 V1 N1 C13 127.8(3) . . . . ? O3 V1 N1 C13 10.3(3) . . . . ? O4 V2 N4 C37 117.4(3) . . . . ? O6 V2 N4 C37 -116.5(3) . . . . ? O5 V2 N4 C37 -2.3(3) . . . . ? O4 V2 N4 C31 -5.0(3) . . . . ? O6 V2 N4 C31 121.1(3) . . . . ? O5 V2 N4 C31 -124.7(3) . . . . ? O4 V2 N4 C43 -124.3(3) . . . . ? O6 V2 N4 C43 1.9(3) . . . . ? O5 V2 N4 C43 116.0(3) . . . . ? O4 V2 N5 N6 -16.7(12) . . . . ? O6 V2 N5 N6 -143.0(11) . . . . ? O5 V2 N5 N6 101.7(12) . . . . ? V2 N5 N6 C55 172.9(9) . . . . ? V2 N5 N6 C49 1.1(14) . . . . ? C7 N1 C1 C2 -126.4(5) . . . . ? C13 N1 C1 C2 100.4(5) . . . . ? V1 N1 C1 C2 -11.5(5) . . . . ? C7 N1 C1 C6 52.9(6) . . . . ? C13 N1 C1 C6 -80.3(6) . . . . ? V1 N1 C1 C6 167.7(4) . . . . ? V1 O1 C2 C3 -171.6(4) . . . . ? V1 O1 C2 C1 8.6(6) . . . . ? C6 C1 C2 C3 5.0(8) . . . . ? N1 C1 C2 C3 -175.7(4) . . . . ? C6 C1 C2 O1 -175.2(4) . . . . ? N1 C1 C2 O1 4.1(7) . . . . ? O1 C2 C3 C4 177.1(4) . . . . ? C1 C2 C3 C4 -3.2(8) . . . . ? C2 C3 C4 C5 0.0(7) . . . . ? C3 C4 C5 C6 1.3(8) . . . . ? C4 C5 C6 C1 0.6(8) . . . . ? C2 C1 C6 C5 -3.7(7) . . . . ? N1 C1 C6 C5 177.1(4) . . . . ? C1 N1 C7 C8 106.9(5) . . . . ? C13 N1 C7 C8 -120.6(5) . . . . ? V1 N1 C7 C8 -7.3(5) . . . . ? C1 N1 C7 C12 -74.6(6) . . . . ? C13 N1 C7 C12 57.9(6) . . . . ? V1 N1 C7 C12 171.2(4) . . . . ? V1 O2 C8 C9 -173.6(4) . . . . ? V1 O2 C8 C7 5.7(6) . . . . ? C12 C7 C8 O2 -176.1(4) . . . . ? N1 C7 C8 O2 2.5(6) . . . . ? C12 C7 C8 C9 3.2(8) . . . . ? N1 C7 C8 C9 -178.2(4) . . . . ? O2 C8 C9 C10 177.1(5) . . . . ? C7 C8 C9 C10 -2.2(8) . . . . ? C8 C9 C10 C11 0.2(8) . . . . ? C9 C10 C11 C12 0.8(8) . . . . ? C10 C11 C12 C7 0.2(8) . . . . ? C8 C7 C12 C11 -2.2(7) . . . . ? N1 C7 C12 C11 179.4(5) . . . . ? C7 N1 C13 C18 -75.2(6) . . . . ? C1 N1 C13 C18 59.1(6) . . . . ? V1 N1 C13 C18 170.9(4) . . . . ? C7 N1 C13 C14 105.8(5) . . . . ? C1 N1 C13 C14 -120.0(5) . . . . ? V1 N1 C13 C14 -8.1(5) . . . . ? V1 O3 C14 C15 -169.2(4) . . . . ? V1 O3 C14 C13 10.3(6) . . . . ? C18 C13 C14 O3 -178.7(4) . . . . ? N1 C13 C14 O3 0.3(7) . . . . ? C18 C13 C14 C15 0.8(7) . . . . ? N1 C13 C14 C15 179.8(4) . . . . ? O3 C14 C15 C16 179.8(4) . . . . ? C13 C14 C15 C16 0.3(7) . . . . ? C14 C15 C16 C17 -0.6(8) . . . . ? C15 C16 C17 C18 -0.1(8) . . . . ? C14 C13 C18 C17 -1.5(8) . . . . ? N1 C13 C18 C17 179.6(5) . . . . ? C16 C17 C18 C13 1.2(8) . . . . ? N2 N3 C19 C24 -145.2(5) . . . . ? C25 N3 C19 C24 21.4(7) . . . . ? N2 N3 C19 C20 30.6(6) . . . . ? C25 N3 C19 C20 -162.8(4) . . . . ? C24 C19 C20 C21 1.5(7) . . . . ? N3 C19 C20 C21 -174.4(4) . . . . ? C19 C20 C21 C22 -0.5(8) . . . . ? C20 C21 C22 C23 -0.2(8) . . . . ? C21 C22 C23 C24 0.0(8) . . . . ? C20 C19 C24 C23 -1.7(7) . . . . ? N3 C19 C24 C23 174.0(4) . . . . ? C22 C23 C24 C19 1.0(8) . . . . ? N2 N3 C25 C26 34.4(6) . . . . ? C19 N3 C25 C26 -132.2(5) . . . . ? N2 N3 C25 C30 -144.2(5) . . . . ? C19 N3 C25 C30 49.2(6) . . . . ? C30 C25 C26 C27 0.2(8) . . . . ? N3 C25 C26 C27 -178.4(5) . . . . ? C25 C26 C27 C28 0.2(8) . . . . ? C26 C27 C28 C29 -1.0(9) . . . . ? C27 C28 C29 C30 1.4(9) . . . . ? C28 C29 C30 C25 -1.0(8) . . . . ? C26 C25 C30 C29 0.2(7) . . . . ? N3 C25 C30 C29 178.7(4) . . . . ? C37 N4 C31 C32 -112.3(5) . . . . ? C43 N4 C31 C32 114.8(5) . . . . ? V2 N4 C31 C32 2.4(5) . . . . ? C37 N4 C31 C36 68.1(6) . . . . ? C43 N4 C31 C36 -64.8(6) . . . . ? V2 N4 C31 C36 -177.2(4) . . . . ? V2 O4 C32 C33 169.8(4) . . . . ? V2 O4 C32 C31 -8.5(6) . . . . ? C36 C31 C32 O4 -177.5(4) . . . . ? N4 C31 C32 O4 2.9(6) . . . . ? C36 C31 C32 C33 4.2(7) . . . . ? N4 C31 C32 C33 -175.4(4) . . . . ? O4 C32 C33 C34 178.4(5) . . . . ? C31 C32 C33 C34 -3.3(8) . . . . ? C32 C33 C34 C35 0.3(8) . . . . ? C33 C34 C35 C36 1.7(9) . . . . ? C34 C35 C36 C31 -0.7(8) . . . . ? C32 C31 C36 C35 -2.2(8) . . . . ? N4 C31 C36 C35 177.4(5) . . . . ? C31 N4 C37 C42 -63.4(6) . . . . ? C43 N4 C37 C42 69.8(6) . . . . ? V2 N4 C37 C42 -178.2(4) . . . . ? C31 N4 C37 C38 119.0(5) . . . . ? C43 N4 C37 C38 -107.8(5) . . . . ? V2 N4 C37 C38 4.2(5) . . . . ? V2 O5 C38 C39 -177.6(3) . . . . ? V2 O5 C38 C37 2.7(6) . . . . ? C42 C37 C38 O5 177.4(4) . . . . ? N4 C37 C38 O5 -4.9(6) . . . . ? C42 C37 C38 C39 -2.4(7) . . . . ? N4 C37 C38 C39 175.3(4) . . . . ? O5 C38 C39 C40 -177.6(4) . . . . ? C37 C38 C39 C40 2.2(7) . . . . ? C38 C39 C40 C41 -0.2(7) . . . . ? C39 C40 C41 C42 -1.5(8) . . . . ? C38 C37 C42 C41 0.7(8) . . . . ? N4 C37 C42 C41 -176.8(5) . . . . ? C40 C41 C42 C37 1.2(8) . . . . ? C37 N4 C43 C44 110.8(5) . . . . ? C31 N4 C43 C44 -114.8(5) . . . . ? V2 N4 C43 C44 -1.7(5) . . . . ? C37 N4 C43 C48 -68.6(6) . . . . ? C31 N4 C43 C48 65.8(6) . . . . ? V2 N4 C43 C48 178.9(4) . . . . ? V2 O6 C44 C45 -177.2(4) . . . . ? V2 O6 C44 C43 1.4(6) . . . . ? C48 C43 C44 O6 -180.0(4) . . . . ? N4 C43 C44 O6 0.6(7) . . . . ? C48 C43 C44 C45 -1.4(8) . . . . ? N4 C43 C44 C45 179.2(4) . . . . ? O6 C44 C45 C46 -179.6(5) . . . . ? C43 C44 C45 C46 1.8(8) . . . . ? C44 C45 C46 C47 -1.4(9) . . . . ? C45 C46 C47 C48 0.6(9) . . . . ? C46 C47 C48 C43 -0.2(8) . . . . ? C44 C43 C48 C47 0.6(8) . . . . ? N4 C43 C48 C47 179.9(5) . . . . ? N5 N6 C49 C54 115.0(5) . . . . ? C55 N6 C49 C54 -56.4(7) . . . . ? N5 N6 C49 C50 -61.0(6) . . . . ? C55 N6 C49 C50 127.7(5) . . . . ? C54 C49 C50 C51 0.3(8) . . . . ? N6 C49 C50 C51 176.2(5) . . . . ? C49 C50 C51 C52 -0.1(9) . . . . ? C50 C51 C52 C53 0.5(9) . . . . ? C51 C52 C53 C54 -1.0(8) . . . . ? C50 C49 C54 C53 -0.8(8) . . . . ? N6 C49 C54 C53 -176.7(5) . . . . ? C52 C53 C54 C49 1.1(8) . . . . ? N5 N6 C55 C56 -11.2(7) . . . . ? C49 N6 C55 C56 159.9(5) . . . . ? N5 N6 C55 C60 166.7(4) . . . . ? C49 N6 C55 C60 -22.2(7) . . . . ? C60 C55 C56 C57 1.2(7) . . . . ? N6 C55 C56 C57 179.0(5) . . . . ? C55 C56 C57 C58 0.7(8) . . . . ? C56 C57 C58 C59 -0.9(8) . . . . ? C57 C58 C59 C60 -0.7(8) . . . . ? C56 C55 C60 C59 -2.8(8) . . . . ? N6 C55 C60 C59 179.3(5) . . . . ? C58 C59 C60 C55 2.5(8) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.600 _refine_diff_density_min -0.923 _refine_diff_density_rms 0.092 # start Validation Reply Form _vrf_RINTA01_5b ; PROBLEM: The value of Rint is greater than 0.18 Rint given 0.216 RESPONSE: The overall quality of the data may be poor due to the crystal quality. ; # end Validation Reply Form