# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2006 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'Carl Redshaw' 'Sophie H. Dale' 'Mark R.J. Elsegood' 'Damien M. Hamden' 'Sadahiko Matsuura' 'Shigekazu Matsui' 'Michael Rowan' _publ_contact_author_name 'Carl Redshaw' _publ_contact_author_address ; School of Chemical Sciences & Pharmacy The University of East Anglia Norwich NR4 7TJ UNITED KINGDOM ; _publ_contact_author_email CARL.REDSHAW@UEA.AC.UK _publ_requested_journal 'Chemical Communications' _publ_section_title ; Vanadyl C and N-capped tris(phenolate) complexes: influence of pro-catalyst geometry on catalytic activity. ; data_1 _database_code_depnum_ccdc_archive 'CCDC 607716' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C86 H122 O8 V2' _chemical_formula_weight 1385.72 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' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1275(8) _cell_length_b 13.7705(10) _cell_length_c 13.8307(10) _cell_angle_alpha 104.984(2) _cell_angle_beta 104.898(2) _cell_angle_gamma 105.394(2) _cell_volume 2015.3(2) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4386 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 28.56 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.142 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 0.284 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.932 _exptl_absorpt_correction_T_max 0.989 _exptl_absorpt_process_details 'SADABS, v.2.10, Shedlrick, G.M., 2003' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 17569 _diffrn_reflns_av_R_equivalents 0.0343 _diffrn_reflns_av_sigmaI/netI 0.0680 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8979 _reflns_number_gt 5954 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0480P)^2^+1.9681P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _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 8979 _refine_ls_number_parameters 476 _refine_ls_number_restraints 86 _refine_ls_R_factor_all 0.0955 _refine_ls_R_factor_gt 0.0567 _refine_ls_wR_factor_ref 0.1467 _refine_ls_wR_factor_gt 0.1243 _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_restrained_S_all 1.068 _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 0.55218(4) 0.65148(4) 0.45388(4) 0.02191(13) Uani 1 1 d . . . O1 O 0.51006(18) 0.71102(17) 0.37533(16) 0.0333(5) Uani 1 1 d . . . O2 O 0.42073(16) 0.53746(14) 0.42434(14) 0.0226(4) Uani 1 1 d . . . O3 O 0.66886(17) 0.60947(14) 0.42179(14) 0.0242(4) Uani 1 1 d . . . O4 O 0.38800(17) 0.26274(14) 0.40903(14) 0.0231(4) Uani 1 1 d . . . C1 C 0.5128(2) 0.3925(2) 0.3169(2) 0.0205(6) Uani 1 1 d . . . H1 H 0.5449 0.4366 0.3947 0.025 Uiso 1 1 calc R . . C2 C 0.3382(2) 0.4613(2) 0.3282(2) 0.0210(6) Uani 1 1 d . . . C3 C 0.2158(2) 0.4557(2) 0.2919(2) 0.0225(6) Uani 1 1 d . . . C4 C 0.1415(3) 0.3751(2) 0.1950(2) 0.0249(6) Uani 1 1 d . . . H4 H 0.0591 0.3700 0.1672 0.030 Uiso 1 1 calc R . . C5 C 0.1798(2) 0.3005(2) 0.1351(2) 0.0232(6) Uani 1 1 d . . . C6 C 0.2994(2) 0.3076(2) 0.1761(2) 0.0224(6) Uani 1 1 d . . . H6 H 0.3272 0.2574 0.1374 0.027 Uiso 1 1 calc R . . C7 C 0.3802(2) 0.3868(2) 0.2729(2) 0.0190(5) Uani 1 1 d . . . C8 C 0.1641(3) 0.5319(2) 0.3537(2) 0.0259(6) Uani 1 1 d . . . C9 C 0.2268(3) 0.6479(3) 0.3653(4) 0.0551(11) Uani 1 1 d . . . H9A H 0.3130 0.6729 0.4101 0.083 Uiso 1 1 calc R . . H9B H 0.1871 0.6933 0.3988 0.083 Uiso 1 1 calc R . . H9C H 0.2206 0.6523 0.2946 0.083 Uiso 1 1 calc R . . C10 C 0.0271(3) 0.5009(3) 0.2969(3) 0.0444(9) Uani 1 1 d . . . H10A H 0.0128 0.5097 0.2271 0.067 Uiso 1 1 calc R . . H10B H -0.0041 0.5475 0.3402 0.067 Uiso 1 1 calc R . . H10C H -0.0152 0.4258 0.2868 0.067 Uiso 1 1 calc R . . C11 C 0.1801(4) 0.5238(3) 0.4643(3) 0.0511(10) Uani 1 1 d . . . H11A H 0.1394 0.4491 0.4567 0.077 Uiso 1 1 calc R . . H11B H 0.1439 0.5700 0.5017 0.077 Uiso 1 1 calc R . . H11C H 0.2673 0.5470 0.5054 0.077 Uiso 1 1 calc R . . C12 C 0.0868(2) 0.2145(2) 0.0303(2) 0.0267(6) Uani 1 1 d . . . C13 C -0.0063(3) 0.1358(3) 0.0565(3) 0.0410(8) Uani 1 1 d . . . H13A H 0.0357 0.1021 0.1007 0.061 Uiso 1 1 calc R . . H13B H -0.0668 0.0801 -0.0099 0.061 Uiso 1 1 calc R . . H13C H -0.0475 0.1748 0.0956 0.061 Uiso 1 1 calc R . . C14 C 0.0194(3) 0.2656(3) -0.0395(2) 0.0363(7) Uani 1 1 d . . . H14A H -0.0285 0.2983 -0.0036 0.054 Uiso 1 1 calc R . . H14B H -0.0352 0.2102 -0.1085 0.054 Uiso 1 1 calc R . . H14C H 0.0788 0.3210 -0.0513 0.054 Uiso 1 1 calc R . . C15 C 0.1488(3) 0.1527(2) -0.0339(2) 0.0357(7) Uani 1 1 d . . . H15A H 0.2118 0.2035 -0.0471 0.054 Uiso 1 1 calc R . . H15B H 0.0876 0.1012 -0.1023 0.054 Uiso 1 1 calc R . . H15C H 0.1863 0.1139 0.0067 0.054 Uiso 1 1 calc R . . C16 C 0.6718(2) 0.5594(2) 0.3226(2) 0.0214(6) Uani 1 1 d . . . C17 C 0.7538(2) 0.6151(2) 0.2823(2) 0.0231(6) Uani 1 1 d . . . C18 C 0.7446(3) 0.5608(2) 0.1787(2) 0.0246(6) Uani 1 1 d . . . H18 H 0.7990 0.5958 0.1493 0.030 Uiso 1 1 calc R . . C19 C 0.6598(2) 0.4576(2) 0.1154(2) 0.0233(6) Uani 1 1 d . . . C20 C 0.5852(2) 0.4056(2) 0.1611(2) 0.0218(6) Uani 1 1 d . . . H20 H 0.5279 0.3351 0.1200 0.026 Uiso 1 1 calc R . . C21 C 0.5912(2) 0.4533(2) 0.2657(2) 0.0201(5) Uani 1 1 d . . . C22 C 0.8466(3) 0.7304(2) 0.3469(2) 0.0300(7) Uani 1 1 d . . . C23 C 0.9401(3) 0.7631(2) 0.2940(3) 0.0354(7) Uani 1 1 d . . . H23A H 0.9810 0.7106 0.2845 0.053 Uiso 1 1 calc R . . H23B H 1.0008 0.8344 0.3395 0.053 Uiso 1 1 calc R . . H23C H 0.8984 0.7653 0.2242 0.053 Uiso 1 1 calc R . . C24 C 0.7783(3) 0.8099(3) 0.3497(4) 0.0560(11) Uani 1 1 d . . . H24A H 0.7360 0.8038 0.2765 0.084 Uiso 1 1 calc R . . H24B H 0.8368 0.8834 0.3895 0.084 Uiso 1 1 calc R . . H24C H 0.7187 0.7933 0.3847 0.084 Uiso 1 1 calc R . . C25 C 0.9189(3) 0.7418(3) 0.4602(2) 0.0445(9) Uani 1 1 d . . . H25A H 0.8632 0.7296 0.4997 0.067 Uiso 1 1 calc R . . H25B H 0.9805 0.8144 0.4968 0.067 Uiso 1 1 calc R . . H25C H 0.9593 0.6887 0.4567 0.067 Uiso 1 1 calc R . . C26 C 0.6538(3) 0.4049(2) 0.0001(2) 0.0291(6) Uani 1 1 d . . . C27 C 0.6375(4) 0.4809(3) -0.0632(3) 0.0508(9) Uani 1 1 d . . . H27A H 0.7065 0.5493 -0.0279 0.076 Uiso 1 1 calc R . . H27B H 0.5614 0.4938 -0.0657 0.076 Uiso 1 1 calc R . . H27C H 0.6344 0.4475 -0.1361 0.076 Uiso 1 1 calc R . . C28 C 0.7730(3) 0.3872(3) 0.0036(3) 0.0539(10) Uani 1 1 d . . . H28A H 0.7837 0.3373 0.0414 0.081 Uiso 1 1 calc R . . H28B H 0.8412 0.4561 0.0411 0.081 Uiso 1 1 calc R . . H28C H 0.7712 0.3569 -0.0694 0.081 Uiso 1 1 calc R . . C29 C 0.5472(4) 0.2998(3) -0.0601(3) 0.0604(12) Uani 1 1 d . . . H29A H 0.5455 0.2710 -0.1334 0.091 Uiso 1 1 calc R . . H29B H 0.4709 0.3122 -0.0618 0.091 Uiso 1 1 calc R . . H29C H 0.5561 0.2481 -0.0243 0.091 Uiso 1 1 calc R . . C30 C 0.4456(2) 0.2150(2) 0.3469(2) 0.0221(6) Uani 1 1 d . . . C31 C 0.4290(3) 0.1053(2) 0.3234(2) 0.0255(6) Uani 1 1 d . . . C32 C 0.5100(3) 0.0715(2) 0.2797(2) 0.0304(7) Uani 1 1 d . . . H32 H 0.5029 -0.0017 0.2640 0.037 Uiso 1 1 calc R . . C33 C 0.5998(3) 0.1385(2) 0.2580(2) 0.0318(7) Uani 1 1 d . A . C34 C 0.5994(3) 0.2421(2) 0.2682(2) 0.0276(6) Uani 1 1 d . . . H34 H 0.6549 0.2871 0.2467 0.033 Uiso 1 1 calc R . . C35 C 0.5196(2) 0.2810(2) 0.3092(2) 0.0211(6) Uani 1 1 d . . . C36 C 0.3239(3) 0.0249(2) 0.3372(2) 0.0309(7) Uani 1 1 d . . . C37 C 0.2037(3) 0.0382(3) 0.2846(3) 0.0502(10) Uani 1 1 d . . . H37A H 0.2071 0.1107 0.3211 0.075 Uiso 1 1 calc R . . H37B H 0.1358 -0.0151 0.2900 0.075 Uiso 1 1 calc R . . H37C H 0.1914 0.0274 0.2092 0.075 Uiso 1 1 calc R . . C38 C 0.3443(4) 0.0405(3) 0.4555(3) 0.0573(11) Uani 1 1 d . . . H38A H 0.3396 0.1099 0.4913 0.086 Uiso 1 1 calc R . . H38B H 0.4250 0.0391 0.4899 0.086 Uiso 1 1 calc R . . H38C H 0.2813 -0.0175 0.4606 0.086 Uiso 1 1 calc R . . C39 C 0.3108(3) -0.0919(2) 0.2823(3) 0.0419(8) Uani 1 1 d . . . H39A H 0.2397 -0.1410 0.2880 0.063 Uiso 1 1 calc R . . H39B H 0.3844 -0.1043 0.3171 0.063 Uiso 1 1 calc R . . H39C H 0.2999 -0.1050 0.2068 0.063 Uiso 1 1 calc R . . C40 C 0.6962(3) 0.1016(3) 0.2204(3) 0.0453(8) Uani 1 1 d DU . . C41 C 0.6668(10) -0.0198(6) 0.1935(11) 0.092(4) Uani 0.600(11) 1 d PDU A 1 H41A H 0.5819 -0.0586 0.1454 0.138 Uiso 0.600(11) 1 calc PR A 1 H41B H 0.6785 -0.0363 0.2594 0.138 Uiso 0.600(11) 1 calc PR A 1 H41C H 0.7214 -0.0420 0.1585 0.138 Uiso 0.600(11) 1 calc PR A 1 C42 C 0.6826(7) 0.1135(8) 0.1055(5) 0.0532(19) Uani 0.600(11) 1 d PDU A 1 H42A H 0.6005 0.0678 0.0547 0.080 Uiso 0.600(11) 1 calc PR A 1 H42B H 0.7433 0.0914 0.0797 0.080 Uiso 0.600(11) 1 calc PR A 1 H42C H 0.6958 0.1887 0.1121 0.080 Uiso 0.600(11) 1 calc PR A 1 C43 C 0.8177(8) 0.1689(10) 0.2927(8) 0.077(3) Uani 0.600(11) 1 d PDU A 1 H43A H 0.8771 0.1440 0.2672 0.115 Uiso 0.600(11) 1 calc PR A 1 H43B H 0.8269 0.1653 0.3640 0.115 Uiso 0.600(11) 1 calc PR A 1 H43C H 0.8319 0.2434 0.2961 0.115 Uiso 0.600(11) 1 calc PR A 1 C41X C 0.6565(13) 0.0447(14) 0.1101(9) 0.089(5) Uani 0.400(11) 1 d PDU A 2 H41D H 0.7222 0.0237 0.0927 0.134 Uiso 0.400(11) 1 calc PR A 2 H41E H 0.6349 0.0906 0.0706 0.134 Uiso 0.400(11) 1 calc PR A 2 H41F H 0.5849 -0.0198 0.0901 0.134 Uiso 0.400(11) 1 calc PR A 2 C42X C 0.8198(11) 0.2029(9) 0.2604(11) 0.047(3) Uani 0.400(11) 1 d PDU A 2 H42D H 0.8466 0.2377 0.3380 0.070 Uiso 0.400(11) 1 calc PR A 2 H42E H 0.8052 0.2543 0.2257 0.070 Uiso 0.400(11) 1 calc PR A 2 H42F H 0.8831 0.1787 0.2418 0.070 Uiso 0.400(11) 1 calc PR A 2 C43X C 0.7439(13) 0.0399(14) 0.2948(15) 0.092(5) Uani 0.400(11) 1 d PDU A 2 H43D H 0.7659 0.0837 0.3698 0.138 Uiso 0.400(11) 1 calc PR A 2 H43E H 0.8158 0.0269 0.2829 0.138 Uiso 0.400(11) 1 calc PR A 2 H43F H 0.6795 -0.0290 0.2775 0.138 Uiso 0.400(11) 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0239(3) 0.0204(2) 0.0203(2) 0.00519(19) 0.00779(19) 0.00789(19) O1 0.0310(11) 0.0376(12) 0.0332(12) 0.0177(10) 0.0090(9) 0.0121(10) O2 0.0227(10) 0.0225(10) 0.0205(9) 0.0046(8) 0.0072(8) 0.0081(8) O3 0.0253(10) 0.0223(10) 0.0221(10) 0.0035(8) 0.0112(8) 0.0053(8) O4 0.0279(10) 0.0177(9) 0.0222(10) 0.0049(8) 0.0100(8) 0.0066(8) C1 0.0221(14) 0.0195(13) 0.0197(13) 0.0051(11) 0.0068(11) 0.0096(11) C2 0.0238(14) 0.0162(13) 0.0203(13) 0.0049(11) 0.0056(11) 0.0062(11) C3 0.0236(14) 0.0233(14) 0.0226(14) 0.0084(11) 0.0090(11) 0.0103(11) C4 0.0217(14) 0.0270(15) 0.0268(15) 0.0088(12) 0.0086(12) 0.0105(12) C5 0.0237(14) 0.0215(14) 0.0222(14) 0.0061(11) 0.0088(11) 0.0057(11) C6 0.0232(14) 0.0197(13) 0.0227(14) 0.0047(11) 0.0099(11) 0.0060(11) C7 0.0201(13) 0.0161(12) 0.0223(13) 0.0079(11) 0.0089(11) 0.0063(10) C8 0.0245(15) 0.0238(14) 0.0281(15) 0.0058(12) 0.0076(12) 0.0115(12) C9 0.050(2) 0.0298(18) 0.095(3) 0.017(2) 0.036(2) 0.0224(17) C10 0.0338(18) 0.043(2) 0.047(2) -0.0026(16) 0.0100(16) 0.0201(16) C11 0.057(2) 0.081(3) 0.0381(19) 0.0223(19) 0.0252(18) 0.050(2) C12 0.0230(14) 0.0237(14) 0.0260(15) 0.0030(12) 0.0071(12) 0.0040(12) C13 0.0401(19) 0.0291(17) 0.0377(18) 0.0021(14) 0.0129(15) -0.0025(14) C14 0.0318(17) 0.0413(19) 0.0265(16) 0.0044(14) 0.0046(13) 0.0116(15) C15 0.0318(17) 0.0333(17) 0.0275(16) -0.0038(13) 0.0054(13) 0.0081(14) C16 0.0251(14) 0.0211(13) 0.0199(13) 0.0067(11) 0.0089(11) 0.0106(11) C17 0.0233(14) 0.0203(13) 0.0272(14) 0.0092(12) 0.0093(12) 0.0085(11) C18 0.0257(15) 0.0265(15) 0.0270(15) 0.0133(12) 0.0126(12) 0.0105(12) C19 0.0242(14) 0.0262(14) 0.0231(14) 0.0094(12) 0.0090(11) 0.0130(12) C20 0.0204(13) 0.0189(13) 0.0236(14) 0.0054(11) 0.0050(11) 0.0078(11) C21 0.0214(13) 0.0179(13) 0.0242(14) 0.0084(11) 0.0091(11) 0.0100(11) C22 0.0284(16) 0.0249(15) 0.0347(17) 0.0073(13) 0.0153(13) 0.0051(13) C23 0.0330(17) 0.0283(16) 0.0384(18) 0.0073(14) 0.0157(14) 0.0019(13) C24 0.047(2) 0.0213(17) 0.101(3) 0.0145(19) 0.039(2) 0.0090(16) C25 0.0407(19) 0.0369(19) 0.0307(17) -0.0025(14) 0.0113(15) -0.0097(15) C26 0.0290(16) 0.0359(17) 0.0230(15) 0.0081(13) 0.0106(12) 0.0132(13) C27 0.061(2) 0.061(2) 0.0359(19) 0.0216(18) 0.0195(18) 0.024(2) C28 0.055(2) 0.075(3) 0.038(2) 0.0118(19) 0.0206(18) 0.037(2) C29 0.062(3) 0.056(2) 0.0333(19) -0.0071(18) 0.0218(18) -0.007(2) C30 0.0242(14) 0.0206(13) 0.0199(13) 0.0047(11) 0.0063(11) 0.0090(11) C31 0.0317(16) 0.0203(14) 0.0208(14) 0.0045(11) 0.0067(12) 0.0085(12) C32 0.0379(17) 0.0205(14) 0.0352(17) 0.0089(13) 0.0135(14) 0.0141(13) C33 0.0393(18) 0.0309(16) 0.0391(18) 0.0174(14) 0.0211(15) 0.0216(14) C34 0.0285(15) 0.0281(15) 0.0324(16) 0.0122(13) 0.0145(13) 0.0145(13) C35 0.0217(14) 0.0200(13) 0.0207(13) 0.0056(11) 0.0057(11) 0.0094(11) C36 0.0375(17) 0.0177(14) 0.0335(16) 0.0063(12) 0.0130(14) 0.0055(13) C37 0.0307(18) 0.0286(18) 0.084(3) 0.0181(19) 0.0184(19) 0.0019(15) C38 0.089(3) 0.0299(19) 0.046(2) 0.0122(17) 0.034(2) 0.0026(19) C39 0.053(2) 0.0189(15) 0.048(2) 0.0080(14) 0.0177(17) 0.0071(15) C40 0.0488(19) 0.0384(18) 0.071(2) 0.0231(17) 0.0365(18) 0.0301(16) C41 0.127(7) 0.052(4) 0.166(10) 0.048(5) 0.113(7) 0.067(4) C42 0.052(4) 0.067(5) 0.049(3) 0.009(3) 0.025(3) 0.038(4) C43 0.049(4) 0.112(7) 0.060(5) 0.005(5) 0.009(4) 0.050(4) C41X 0.074(8) 0.081(10) 0.087(5) -0.022(6) 0.030(6) 0.038(7) C42X 0.039(5) 0.050(5) 0.070(8) 0.022(4) 0.031(5) 0.030(3) C43X 0.090(9) 0.106(10) 0.181(12) 0.111(10) 0.094(9) 0.086(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O1 1.585(2) . ? V1 O3 1.7774(19) . ? V1 O2 1.7828(19) . ? V1 O4 1.7877(18) 2_666 ? O2 C2 1.381(3) . ? O3 C16 1.382(3) . ? O4 C30 1.385(3) . ? O4 V1 1.7877(18) 2_666 ? C1 C21 1.528(4) . ? C1 C35 1.537(3) . ? C1 C7 1.539(4) . ? C2 C7 1.404(4) . ? C2 C3 1.413(4) . ? C3 C4 1.386(4) . ? C3 C8 1.545(4) . ? C4 C5 1.403(4) . ? C5 C6 1.381(4) . ? C5 C12 1.529(4) . ? C6 C7 1.395(3) . ? C8 C9 1.522(4) . ? C8 C11 1.529(4) . ? C8 C10 1.530(4) . ? C12 C13 1.532(4) . ? C12 C14 1.533(4) . ? C12 C15 1.539(4) . ? C16 C21 1.400(4) . ? C16 C17 1.410(4) . ? C17 C18 1.395(4) . ? C17 C22 1.545(4) . ? C18 C19 1.401(4) . ? C19 C20 1.383(4) . ? C19 C26 1.545(4) . ? C20 C21 1.400(4) . ? C22 C25 1.530(4) . ? C22 C23 1.533(4) . ? C22 C24 1.537(4) . ? C26 C29 1.513(4) . ? C26 C28 1.519(4) . ? C26 C27 1.548(5) . ? C30 C35 1.399(4) . ? C30 C31 1.407(4) . ? C31 C32 1.397(4) . ? C31 C36 1.540(4) . ? C32 C33 1.379(4) . ? C33 C34 1.398(4) . ? C33 C40 1.544(4) . ? C34 C35 1.394(4) . ? C36 C37 1.533(5) . ? C36 C39 1.536(4) . ? C36 C38 1.538(4) . ? C40 C41X 1.406(10) . ? C40 C43 1.438(9) . ? C40 C41 1.534(7) . ? C40 C43X 1.588(9) . ? C40 C42X 1.602(11) . ? C40 C42 1.611(7) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 V1 O3 107.19(10) . . ? O1 V1 O2 105.37(10) . . ? O3 V1 O2 110.23(8) . . ? O1 V1 O4 112.37(10) . 2_666 ? O3 V1 O4 108.69(9) . 2_666 ? O2 V1 O4 112.82(8) . 2_666 ? C2 O2 V1 131.29(16) . . ? C16 O3 V1 128.92(17) . . ? C30 O4 V1 129.85(16) . 2_666 ? C21 C1 C35 114.6(2) . . ? C21 C1 C7 110.2(2) . . ? C35 C1 C7 111.8(2) . . ? O2 C2 C7 116.7(2) . . ? O2 C2 C3 120.9(2) . . ? C7 C2 C3 122.3(2) . . ? C4 C3 C2 115.5(2) . . ? C4 C3 C8 120.5(2) . . ? C2 C3 C8 124.0(2) . . ? C3 C4 C5 124.4(3) . . ? C6 C5 C4 117.7(2) . . ? C6 C5 C12 123.7(2) . . ? C4 C5 C12 118.6(2) . . ? C5 C6 C7 121.5(2) . . ? C6 C7 C2 118.6(2) . . ? C6 C7 C1 120.4(2) . . ? C2 C7 C1 121.1(2) . . ? C9 C8 C11 109.5(3) . . ? C9 C8 C10 107.9(3) . . ? C11 C8 C10 106.5(3) . . ? C9 C8 C3 111.3(2) . . ? C11 C8 C3 110.0(2) . . ? C10 C8 C3 111.4(2) . . ? C5 C12 C13 108.4(2) . . ? C5 C12 C14 110.6(2) . . ? C13 C12 C14 108.7(3) . . ? C5 C12 C15 111.5(2) . . ? C13 C12 C15 109.5(2) . . ? C14 C12 C15 108.1(2) . . ? O3 C16 C21 117.4(2) . . ? O3 C16 C17 120.0(2) . . ? C21 C16 C17 122.6(2) . . ? C18 C17 C16 115.9(2) . . ? C18 C17 C22 121.4(2) . . ? C16 C17 C22 122.6(2) . . ? C17 C18 C19 123.8(3) . . ? C20 C19 C18 117.4(2) . . ? C20 C19 C26 122.4(2) . . ? C18 C19 C26 120.2(2) . . ? C19 C20 C21 122.3(2) . . ? C16 C21 C20 117.7(2) . . ? C16 C21 C1 120.7(2) . . ? C20 C21 C1 121.6(2) . . ? C25 C22 C23 106.8(3) . . ? C25 C22 C24 110.8(3) . . ? C23 C22 C24 106.5(3) . . ? C25 C22 C17 112.0(2) . . ? C23 C22 C17 111.6(2) . . ? C24 C22 C17 109.0(2) . . ? C29 C26 C28 110.3(3) . . ? C29 C26 C19 112.5(3) . . ? C28 C26 C19 109.2(2) . . ? C29 C26 C27 106.9(3) . . ? C28 C26 C27 108.3(3) . . ? C19 C26 C27 109.6(2) . . ? O4 C30 C35 116.7(2) . . ? O4 C30 C31 120.9(2) . . ? C35 C30 C31 122.4(2) . . ? C32 C31 C30 115.5(3) . . ? C32 C31 C36 121.3(2) . . ? C30 C31 C36 123.1(3) . . ? C33 C32 C31 123.7(3) . . ? C32 C33 C34 117.6(3) . . ? C32 C33 C40 122.4(3) . . ? C34 C33 C40 120.0(3) . . ? C35 C34 C33 121.7(3) . . ? C34 C35 C30 117.2(2) . . ? C34 C35 C1 123.1(2) . . ? C30 C35 C1 119.7(2) . . ? C37 C36 C39 107.5(3) . . ? C37 C36 C38 110.3(3) . . ? C39 C36 C38 106.6(3) . . ? C37 C36 C31 108.9(2) . . ? C39 C36 C31 111.5(2) . . ? C38 C36 C31 112.0(2) . . ? C41X C40 C43 128.7(8) . . ? C41X C40 C41 67.1(8) . . ? C43 C40 C41 115.5(6) . . ? C41X C40 C33 114.4(6) . . ? C43 C40 C33 111.0(5) . . ? C41 C40 C33 112.0(4) . . ? C41X C40 C43X 115.0(8) . . ? C33 C40 C43X 106.7(5) . . ? C41X C40 C42X 112.1(8) . . ? C33 C40 C42X 109.3(6) . . ? C43X C40 C42X 98.0(7) . . ? C43 C40 C42 108.1(6) . . ? C41 C40 C42 102.0(5) . . ? C33 C40 C42 107.4(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 V1 O2 C2 46.7(2) . . . . ? O3 V1 O2 C2 -68.6(2) . . . . ? O4 V1 O2 C2 169.7(2) 2_666 . . . ? O1 V1 O3 C16 -45.6(2) . . . . ? O2 V1 O3 C16 68.6(2) . . . . ? O4 V1 O3 C16 -167.3(2) 2_666 . . . ? V1 O2 C2 C7 71.6(3) . . . . ? V1 O2 C2 C3 -112.2(3) . . . . ? O2 C2 C3 C4 -179.3(2) . . . . ? C7 C2 C3 C4 -3.3(4) . . . . ? O2 C2 C3 C8 0.3(4) . . . . ? C7 C2 C3 C8 176.3(2) . . . . ? C2 C3 C4 C5 1.6(4) . . . . ? C8 C3 C4 C5 -178.1(3) . . . . ? C3 C4 C5 C6 0.4(4) . . . . ? C3 C4 C5 C12 178.9(3) . . . . ? C4 C5 C6 C7 -0.8(4) . . . . ? C12 C5 C6 C7 -179.1(2) . . . . ? C5 C6 C7 C2 -0.9(4) . . . . ? C5 C6 C7 C1 179.7(2) . . . . ? O2 C2 C7 C6 179.2(2) . . . . ? C3 C2 C7 C6 3.1(4) . . . . ? O2 C2 C7 C1 -1.4(3) . . . . ? C3 C2 C7 C1 -177.5(2) . . . . ? C21 C1 C7 C6 83.1(3) . . . . ? C35 C1 C7 C6 -45.6(3) . . . . ? C21 C1 C7 C2 -96.3(3) . . . . ? C35 C1 C7 C2 135.1(2) . . . . ? C4 C3 C8 C9 -117.4(3) . . . . ? C2 C3 C8 C9 63.0(4) . . . . ? C4 C3 C8 C11 121.0(3) . . . . ? C2 C3 C8 C11 -58.6(4) . . . . ? C4 C3 C8 C10 3.0(4) . . . . ? C2 C3 C8 C10 -176.5(3) . . . . ? C6 C5 C12 C13 109.0(3) . . . . ? C4 C5 C12 C13 -69.4(3) . . . . ? C6 C5 C12 C14 -131.9(3) . . . . ? C4 C5 C12 C14 49.8(3) . . . . ? C6 C5 C12 C15 -11.6(4) . . . . ? C4 C5 C12 C15 170.1(3) . . . . ? V1 O3 C16 C21 -68.8(3) . . . . ? V1 O3 C16 C17 111.1(3) . . . . ? O3 C16 C17 C18 -175.8(2) . . . . ? C21 C16 C17 C18 4.2(4) . . . . ? O3 C16 C17 C22 2.7(4) . . . . ? C21 C16 C17 C22 -177.3(3) . . . . ? C16 C17 C18 C19 0.5(4) . . . . ? C22 C17 C18 C19 -178.0(3) . . . . ? C17 C18 C19 C20 -3.0(4) . . . . ? C17 C18 C19 C26 178.3(3) . . . . ? C18 C19 C20 C21 1.0(4) . . . . ? C26 C19 C20 C21 179.6(2) . . . . ? O3 C16 C21 C20 173.9(2) . . . . ? C17 C16 C21 C20 -6.1(4) . . . . ? O3 C16 C21 C1 -6.0(4) . . . . ? C17 C16 C21 C1 174.1(2) . . . . ? C19 C20 C21 C16 3.4(4) . . . . ? C19 C20 C21 C1 -176.8(2) . . . . ? C35 C1 C21 C16 -129.0(3) . . . . ? C7 C1 C21 C16 103.9(3) . . . . ? C35 C1 C21 C20 51.1(3) . . . . ? C7 C1 C21 C20 -76.0(3) . . . . ? C18 C17 C22 C25 -132.3(3) . . . . ? C16 C17 C22 C25 49.2(4) . . . . ? C18 C17 C22 C23 -12.6(4) . . . . ? C16 C17 C22 C23 168.9(3) . . . . ? C18 C17 C22 C24 104.7(3) . . . . ? C16 C17 C22 C24 -73.7(4) . . . . ? C20 C19 C26 C29 8.4(4) . . . . ? C18 C19 C26 C29 -173.0(3) . . . . ? C20 C19 C26 C28 -114.4(3) . . . . ? C18 C19 C26 C28 64.2(4) . . . . ? C20 C19 C26 C27 127.2(3) . . . . ? C18 C19 C26 C27 -54.2(3) . . . . ? V1 O4 C30 C35 -77.4(3) 2_666 . . . ? V1 O4 C30 C31 102.8(3) 2_666 . . . ? O4 C30 C31 C32 -167.2(2) . . . . ? C35 C30 C31 C32 13.0(4) . . . . ? O4 C30 C31 C36 16.7(4) . . . . ? C35 C30 C31 C36 -163.0(3) . . . . ? C30 C31 C32 C33 -1.3(4) . . . . ? C36 C31 C32 C33 174.9(3) . . . . ? C31 C32 C33 C34 -8.1(5) . . . . ? C31 C32 C33 C40 173.7(3) . . . . ? C32 C33 C34 C35 6.4(4) . . . . ? C40 C33 C34 C35 -175.3(3) . . . . ? C33 C34 C35 C30 4.4(4) . . . . ? C33 C34 C35 C1 -177.2(3) . . . . ? O4 C30 C35 C34 165.6(2) . . . . ? C31 C30 C35 C34 -14.6(4) . . . . ? O4 C30 C35 C1 -12.8(4) . . . . ? C31 C30 C35 C1 166.9(2) . . . . ? C21 C1 C35 C34 5.9(4) . . . . ? C7 C1 C35 C34 132.2(3) . . . . ? C21 C1 C35 C30 -175.8(2) . . . . ? C7 C1 C35 C30 -49.5(3) . . . . ? C32 C31 C36 C37 -127.2(3) . . . . ? C30 C31 C36 C37 48.6(4) . . . . ? C32 C31 C36 C39 -8.8(4) . . . . ? C30 C31 C36 C39 167.1(3) . . . . ? C32 C31 C36 C38 110.6(3) . . . . ? C30 C31 C36 C38 -73.6(4) . . . . ? C32 C33 C40 C41X 83.1(10) . . . . ? C34 C33 C40 C41X -95.1(10) . . . . ? C32 C33 C40 C43 -121.5(6) . . . . ? C34 C33 C40 C43 60.3(7) . . . . ? C32 C33 C40 C41 9.2(7) . . . . ? C34 C33 C40 C41 -168.9(6) . . . . ? C32 C33 C40 C43X -45.2(8) . . . . ? C34 C33 C40 C43X 136.6(8) . . . . ? C32 C33 C40 C42X -150.2(6) . . . . ? C34 C33 C40 C42X 31.6(7) . . . . ? C32 C33 C40 C42 120.5(5) . . . . ? C34 C33 C40 C42 -57.7(5) . . . . ? _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.748 _refine_diff_density_min -0.673 _refine_diff_density_rms 0.070 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 607717' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C104 H144 N2 O7 V' _chemical_formula_weight 1585.15 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.4639(8) _cell_length_b 30.6728(17) _cell_length_c 21.4928(9) _cell_angle_alpha 90.00 _cell_angle_beta 107.107(3) _cell_angle_gamma 90.00 _cell_volume 9743.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 17672 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.48 _exptl_crystal_description plate _exptl_crystal_colour 'pale green' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.081 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3444 _exptl_absorpt_coefficient_mu 0.154 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.958 _exptl_absorpt_correction_T_max 0.995 _exptl_absorpt_process_details 'SADABS v2.10, Sheldrick, G.M., (2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Bruker-Nonius FR591 rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker-Nonius 95mm CCD camera on \k-goniostat' _diffrn_measurement_method '\f & \w scans' _diffrn_detector_area_resol_mean 9.091 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 64432 _diffrn_reflns_av_R_equivalents 0.2112 _diffrn_reflns_av_sigmaI/netI 0.1870 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.81 _diffrn_reflns_theta_max 22.50 _reflns_number_total 12660 _reflns_number_gt 6643 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'COLLECT (Hooft, R.W.W., 1998)' _computing_cell_refinement 'DENZO (Ottowinowski & Minor, 1997) & COLLECT' _computing_data_reduction 'DENZO & COLLECT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0223P)^2^+19.8098P] 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 SHELXL _refine_ls_extinction_coef 0.00042(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 12660 _refine_ls_number_parameters 1140 _refine_ls_number_restraints 149 _refine_ls_R_factor_all 0.1983 _refine_ls_R_factor_gt 0.1009 _refine_ls_wR_factor_ref 0.1859 _refine_ls_wR_factor_gt 0.1511 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.040 _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 0.26184(7) 0.84196(4) 0.83503(5) 0.0322(3) Uani 1 1 d . . . O1 O 0.1661(3) 0.88415(13) 0.80221(19) 0.0313(11) Uani 1 1 d . . . O2 O 0.2472(3) 0.94866(17) 0.8923(2) 0.0364(18) Uani 0.847(9) 1 d P A 1 H2 H 0.2210 0.9328 0.8605 0.055 Uiso 0.847(9) 1 calc PR A 1 O2X O -0.0196(17) 1.0391(10) 0.8139(15) 0.048(10) Uani 0.153(9) 1 d PU A 2 O3 O 0.1658(3) 1.05222(16) 0.7685(2) 0.0480(13) Uani 1 1 d . . . H3 H 0.1709 1.0387 0.8034 0.072 Uiso 1 1 calc R . . O4 O 0.3323(3) 0.78957(13) 0.83864(19) 0.0345(11) Uani 1 1 d . . . O5 O 0.4613(4) 0.8146(2) 0.9606(3) 0.046(2) Uani 0.768(10) 1 d P B 1 H5 H 0.4260 0.8045 0.9261 0.069 Uiso 0.768(10) 1 calc PR B 1 O5X O 0.6313(11) 0.6854(6) 0.9528(8) 0.033(7) Uani 0.232(10) 1 d P B 2 O6 O 0.4644(3) 0.68425(14) 1.0291(2) 0.0385(12) Uani 1 1 d . . . H6 H 0.4946 0.7066 1.0267 0.058 Uiso 1 1 calc R . . O7 O 0.3169(3) 0.86458(15) 0.9009(2) 0.0465(13) Uani 1 1 d . . . N1 N 0.1611(4) 0.79981(17) 0.8476(2) 0.0336(14) Uani 1 1 d . . . N2 N 0.3078(3) 0.86060(16) 0.7563(2) 0.0305(13) Uani 1 1 d . . . C1 C 0.1832(4) 0.7554(2) 0.8687(4) 0.0385(19) Uani 1 1 d . . . C2 C 0.1767(4) 0.7233(2) 0.8216(4) 0.0438(19) Uani 1 1 d . . . C3 C 0.1961(5) 0.6805(2) 0.8432(4) 0.052(2) Uani 1 1 d . . . H3A H 0.1894 0.6575 0.8124 0.062 Uiso 1 1 calc R . . C4 C 0.2251(5) 0.6711(3) 0.9094(4) 0.055(2) Uani 1 1 d . . . H4 H 0.2391 0.6419 0.9234 0.066 Uiso 1 1 calc R . . C5 C 0.2339(5) 0.7035(2) 0.9547(4) 0.047(2) Uani 1 1 d . . . H5A H 0.2535 0.6965 0.9998 0.056 Uiso 1 1 calc R . . C6 C 0.2140(4) 0.7471(2) 0.9351(3) 0.0406(19) Uani 1 1 d . . . C7 C 0.1512(5) 0.7337(2) 0.7492(3) 0.050(2) Uani 1 1 d . . . H7 H 0.1599 0.7658 0.7450 0.060 Uiso 1 1 calc R . . C8 C 0.2117(5) 0.7104(2) 0.7146(3) 0.064(2) Uani 1 1 d . . . H8A H 0.2754 0.7152 0.7388 0.096 Uiso 1 1 calc R . . H8B H 0.1998 0.7220 0.6704 0.096 Uiso 1 1 calc R . . H8C H 0.1987 0.6791 0.7125 0.096 Uiso 1 1 calc R . . C9 C 0.0518(5) 0.7238(3) 0.7159(4) 0.078(3) Uani 1 1 d . . . H9A H 0.0400 0.6929 0.7217 0.117 Uiso 1 1 calc R . . H9B H 0.0375 0.7303 0.6693 0.117 Uiso 1 1 calc R . . H9C H 0.0140 0.7418 0.7352 0.117 Uiso 1 1 calc R . . C10 C 0.2244(5) 0.7833(2) 0.9853(4) 0.056(2) Uani 1 1 d . . . H10 H 0.2349 0.8109 0.9639 0.067 Uiso 1 1 calc R . . C11 C 0.1362(5) 0.7896(3) 1.0038(4) 0.075(3) Uani 1 1 d . . . H11A H 0.0866 0.7964 0.9646 0.112 Uiso 1 1 calc R . . H11B H 0.1437 0.8136 1.0350 0.112 Uiso 1 1 calc R . . H11C H 0.1220 0.7627 1.0235 0.112 Uiso 1 1 calc R . . C12 C 0.3036(5) 0.7781(3) 1.0464(4) 0.069(3) Uani 1 1 d . . . H12A H 0.2937 0.7526 1.0708 0.103 Uiso 1 1 calc R . . H12B H 0.3088 0.8042 1.0736 0.103 Uiso 1 1 calc R . . H12C H 0.3595 0.7743 1.0343 0.103 Uiso 1 1 calc R . . C13 C 0.0764(5) 0.8102(2) 0.8357(3) 0.0368(18) Uani 1 1 d . . . H13 H 0.0380 0.7874 0.8414 0.044 Uiso 1 1 calc R . . C14 C 0.0808(4) 0.8873(2) 0.8032(3) 0.0295(17) Uani 1 1 d . . . C15 C 0.0328(4) 0.8509(2) 0.8153(3) 0.0300(16) Uani 1 1 d . . . C16 C -0.0594(4) 0.8548(2) 0.8112(3) 0.0352(17) Uani 1 1 d . . . H16 H -0.0914 0.8297 0.8180 0.042 Uiso 1 1 calc R . . C17 C -0.1049(4) 0.8940(2) 0.7977(3) 0.0314(17) Uani 1 1 d . . . C18 C -0.0536(4) 0.9303(2) 0.7901(3) 0.0316(17) Uani 1 1 d . . . H18 H -0.0821 0.9581 0.7841 0.038 Uiso 1 1 calc R . . C19 C 0.0373(4) 0.9280(2) 0.7909(3) 0.0277(16) Uani 1 1 d . . . C20 C -0.2060(4) 0.8962(2) 0.7895(3) 0.0299(16) Uani 1 1 d . . . C24 C 0.0898(4) 0.9690(2) 0.7864(3) 0.0307(16) Uani 1 1 d . . . H24 H 0.1488 0.9590 0.7812 0.037 Uiso 1 1 calc R . . C21 C -0.2276(4) 0.8786(2) 0.8499(3) 0.047(2) Uani 1 1 d . . . H21A H -0.2046 0.8488 0.8586 0.071 Uiso 1 1 calc R . . H21B H -0.2933 0.8787 0.8424 0.071 Uiso 1 1 calc R . . H21C H -0.1988 0.8972 0.8874 0.071 Uiso 1 1 calc R . . C22 C -0.2561(4) 0.8678(2) 0.7308(3) 0.051(2) Uani 1 1 d . . . H22A H -0.2473 0.8799 0.6910 0.076 Uiso 1 1 calc R . . H22B H -0.3209 0.8673 0.7270 0.076 Uiso 1 1 calc R . . H22C H -0.2321 0.8380 0.7373 0.076 Uiso 1 1 calc R . . C23 C -0.2432(4) 0.9424(2) 0.7764(3) 0.047(2) Uani 1 1 d . . . H23A H -0.2118 0.9614 0.8127 0.071 Uiso 1 1 calc R . . H23B H -0.3081 0.9423 0.7719 0.071 Uiso 1 1 calc R . . H23C H -0.2335 0.9533 0.7361 0.071 Uiso 1 1 calc R . . C25 C 0.1880(4) 0.9789(2) 0.9021(3) 0.0286(16) Uani 1 1 d . . . H25X H 0.2258 0.9568 0.8934 0.034 Uiso 0.153(9) 1 calc PR A 2 C26 C 0.2100(4) 0.9970(2) 0.9648(3) 0.0300(16) Uani 1 1 d . A . C27 C 0.1531(4) 1.0297(2) 0.9745(3) 0.0335(17) Uani 1 1 d . . . H27 H 0.1678 1.0434 1.0160 0.040 Uiso 1 1 calc R A . C28 C 0.0763(4) 1.0435(2) 0.9270(3) 0.0326(17) Uani 1 1 d . A . C29 C 0.0566(4) 1.0240(2) 0.8665(3) 0.0335(17) Uani 1 1 d U . . H29 H 0.0034 1.0325 0.8335 0.040 Uiso 0.847(9) 1 calc PR A 1 C30 C 0.1126(4) 0.9922(2) 0.8523(3) 0.0285(16) Uani 1 1 d . A . C31 C 0.2912(4) 0.9798(2) 1.0198(3) 0.0352(17) Uani 1 1 d . . . C32 C 0.2779(5) 0.9310(2) 1.0332(3) 0.048(2) Uani 1 1 d . A . H32A H 0.2220 0.9274 1.0453 0.071 Uiso 1 1 calc R . . H32B H 0.3293 0.9208 1.0688 0.071 Uiso 1 1 calc R . . H32C H 0.2739 0.9139 0.9939 0.071 Uiso 1 1 calc R . . C33 C 0.3805(4) 0.9851(2) 1.0024(3) 0.0430(19) Uani 1 1 d . A . H33A H 0.3798 0.9660 0.9656 0.064 Uiso 1 1 calc R . . H33B H 0.4315 0.9771 1.0400 0.064 Uiso 1 1 calc R . . H33C H 0.3871 1.0155 0.9904 0.064 Uiso 1 1 calc R . . C34 C 0.3024(5) 1.0042(2) 1.0843(3) 0.049(2) Uani 1 1 d . A . H34A H 0.3123 1.0353 1.0782 0.073 Uiso 1 1 calc R . . H34B H 0.3544 0.9924 1.1179 0.073 Uiso 1 1 calc R . . H34C H 0.2475 1.0006 1.0978 0.073 Uiso 1 1 calc R . . C35 C 0.0163(4) 1.0800(2) 0.9415(3) 0.0387(18) Uani 1 1 d . . . C36 C -0.0086(5) 1.0692(3) 1.0049(4) 0.077(3) Uani 1 1 d . A . H36A H 0.0468 1.0671 1.0415 0.115 Uiso 1 1 calc R . . H36B H -0.0409 1.0413 0.9996 0.115 Uiso 1 1 calc R . . H36C H -0.0473 1.0923 1.0135 0.115 Uiso 1 1 calc R . . C37 C -0.0726(5) 1.0843(3) 0.8884(4) 0.077(3) Uani 1 1 d . A . H37A H -0.1072 1.1086 0.8987 0.116 Uiso 1 1 calc R . . H37B H -0.1073 1.0573 0.8855 0.116 Uiso 1 1 calc R . . H37C H -0.0609 1.0899 0.8468 0.116 Uiso 1 1 calc R . . C38 C 0.0659(5) 1.1228(3) 0.9504(5) 0.086(3) Uani 1 1 d . A . H38A H 0.0796 1.1305 0.9101 0.128 Uiso 1 1 calc R . . H38B H 0.1224 1.1203 0.9860 0.128 Uiso 1 1 calc R . . H38C H 0.0279 1.1455 0.9610 0.128 Uiso 1 1 calc R . . C39 C 0.0885(5) 1.0392(2) 0.7225(3) 0.0392(18) Uani 1 1 d . . . C40 C 0.0549(5) 1.0659(2) 0.6683(3) 0.0423(19) Uani 1 1 d . . . C41 C -0.0195(5) 1.0510(2) 0.6197(3) 0.046(2) Uani 1 1 d . . . H41 H -0.0433 1.0689 0.5825 0.056 Uiso 1 1 calc R . . C42 C -0.0608(4) 1.0114(2) 0.6226(3) 0.0404(19) Uani 1 1 d . . . C43 C -0.0258(4) 0.9860(2) 0.6780(3) 0.0332(17) Uani 1 1 d . . . H43 H -0.0535 0.9587 0.6811 0.040 Uiso 1 1 calc R . . C44 C 0.0481(4) 0.9989(2) 0.7288(3) 0.0338(17) Uani 1 1 d . . . C45 C 0.0987(6) 1.1105(3) 0.6639(4) 0.059(2) Uani 1 1 d . . . C46 C 0.0933(6) 1.1392(2) 0.7207(4) 0.078(3) Uani 1 1 d . . . H46A H 0.1290 1.1260 0.7618 0.117 Uiso 1 1 calc R . . H46B H 0.0301 1.1418 0.7206 0.117 Uiso 1 1 calc R . . H46C H 0.1174 1.1682 0.7163 0.117 Uiso 1 1 calc R . . C47 C 0.0468(6) 1.1349(3) 0.6003(4) 0.088(3) Uani 1 1 d . . . H47A H -0.0167 1.1385 0.5989 0.132 Uiso 1 1 calc R . . H47B H 0.0501 1.1178 0.5625 0.132 Uiso 1 1 calc R . . H47C H 0.0743 1.1635 0.5993 0.132 Uiso 1 1 calc R . . C48 C 0.1959(5) 1.1050(2) 0.6626(4) 0.064(2) Uani 1 1 d . . . H48A H 0.2216 1.1336 0.6583 0.096 Uiso 1 1 calc R . . H48B H 0.1970 1.0866 0.6256 0.096 Uiso 1 1 calc R . . H48C H 0.2316 1.0912 0.7032 0.096 Uiso 1 1 calc R . . C49 C -0.1417(5) 0.9947(3) 0.5663(3) 0.050(2) Uani 1 1 d . . . C50 C -0.2102(6) 0.9713(4) 0.5929(4) 0.137(5) Uani 1 1 d . . . H50A H -0.2627 0.9628 0.5567 0.205 Uiso 1 1 calc R . . H50B H -0.2298 0.9909 0.6222 0.205 Uiso 1 1 calc R . . H50C H -0.1823 0.9452 0.6169 0.205 Uiso 1 1 calc R . . C51 C -0.1086(6) 0.9639(3) 0.5241(4) 0.104(4) Uani 1 1 d . . . H51A H -0.0747 0.9401 0.5508 0.155 Uiso 1 1 calc R . . H51B H -0.0691 0.9796 0.5035 0.155 Uiso 1 1 calc R . . H51C H -0.1604 0.9520 0.4904 0.155 Uiso 1 1 calc R . . C52 C -0.1910(6) 1.0317(3) 0.5230(4) 0.085(3) Uani 1 1 d . . . H52A H -0.1478 1.0483 0.5069 0.128 Uiso 1 1 calc R . . H52B H -0.2185 1.0510 0.5482 0.128 Uiso 1 1 calc R . . H52C H -0.2382 1.0196 0.4861 0.128 Uiso 1 1 calc R . . C53 C 0.2729(4) 0.9002(2) 0.7202(3) 0.0288(16) Uani 1 1 d . . . C54 C 0.1923(4) 0.8977(2) 0.6691(3) 0.0276(16) Uani 1 1 d . . . C55 C 0.1615(5) 0.9356(2) 0.6352(3) 0.0390(18) Uani 1 1 d . . . H55 H 0.1072 0.9351 0.6001 0.047 Uiso 1 1 calc R . . C56 C 0.2090(5) 0.9742(2) 0.6518(3) 0.0411(19) Uani 1 1 d . . . H56 H 0.1877 0.9998 0.6273 0.049 Uiso 1 1 calc R . . C57 C 0.2874(5) 0.9759(2) 0.7040(3) 0.0382(18) Uani 1 1 d . . . H57 H 0.3183 1.0029 0.7154 0.046 Uiso 1 1 calc R . . C58 C 0.3211(4) 0.9390(2) 0.7394(3) 0.0313(17) Uani 1 1 d . . . C59 C 0.1418(4) 0.8550(2) 0.6513(3) 0.0373(18) Uani 1 1 d . . . H59 H 0.1599 0.8357 0.6904 0.045 Uiso 1 1 calc R . . C60 C 0.1673(5) 0.8323(2) 0.5967(4) 0.060(2) Uani 1 1 d . . . H60A H 0.1538 0.8515 0.5585 0.090 Uiso 1 1 calc R . . H60B H 0.1326 0.8053 0.5854 0.090 Uiso 1 1 calc R . . H60C H 0.2321 0.8256 0.6108 0.090 Uiso 1 1 calc R . . C61 C 0.0393(4) 0.8607(2) 0.6323(3) 0.049(2) Uani 1 1 d . . . H61A H 0.0185 0.8755 0.5901 0.073 Uiso 1 1 calc R . . H61B H 0.0232 0.8783 0.6653 0.073 Uiso 1 1 calc R . . H61C H 0.0103 0.8321 0.6291 0.073 Uiso 1 1 calc R . . C62 C 0.4058(4) 0.9406(2) 0.7967(3) 0.0381(18) Uani 1 1 d . . . H62 H 0.4002 0.9175 0.8280 0.046 Uiso 1 1 calc R . . C63 C 0.4900(4) 0.9306(2) 0.7764(3) 0.052(2) Uani 1 1 d . . . H63A H 0.4853 0.9012 0.7580 0.077 Uiso 1 1 calc R . . H63B H 0.5435 0.9324 0.8145 0.077 Uiso 1 1 calc R . . H63C H 0.4954 0.9518 0.7436 0.077 Uiso 1 1 calc R . . C64 C 0.4175(5) 0.9842(2) 0.8327(3) 0.052(2) Uani 1 1 d . . . H64A H 0.4305 1.0071 0.8050 0.079 Uiso 1 1 calc R . . H64B H 0.4679 0.9821 0.8729 0.079 Uiso 1 1 calc R . . H64C H 0.3618 0.9914 0.8434 0.079 Uiso 1 1 calc R . . C65 C 0.3630(4) 0.8383(2) 0.7336(3) 0.0291(16) Uani 1 1 d . . . H65 H 0.3728 0.8491 0.6948 0.035 Uiso 1 1 calc R . . C66 C 0.3979(4) 0.7779(2) 0.8145(3) 0.0311(17) Uani 1 1 d . . . C67 C 0.4112(4) 0.7991(2) 0.7600(3) 0.0286(16) Uani 1 1 d . . . C68 C 0.4784(4) 0.7844(2) 0.7320(3) 0.0353(17) Uani 1 1 d . . . H68 H 0.4840 0.7980 0.6937 0.042 Uiso 1 1 calc R . . C69 C 0.5354(4) 0.7508(2) 0.7593(3) 0.0323(17) Uani 1 1 d . . . C70 C 0.5246(4) 0.7328(2) 0.8164(3) 0.0326(17) Uani 1 1 d . . . H70 H 0.5657 0.7107 0.8375 0.039 Uiso 1 1 calc R . . C71 C 0.4584(4) 0.7449(2) 0.8444(3) 0.0287(16) Uani 1 1 d . . . C72 C 0.6113(5) 0.7339(2) 0.7329(3) 0.045(2) Uani 1 1 d . . . C73 C 0.6033(5) 0.7533(2) 0.6659(3) 0.052(2) Uani 1 1 d . . . H73A H 0.5425 0.7476 0.6366 0.078 Uiso 1 1 calc R . . H73B H 0.6484 0.7397 0.6481 0.078 Uiso 1 1 calc R . . H73C H 0.6138 0.7848 0.6699 0.078 Uiso 1 1 calc R . . C74 C 0.7027(5) 0.7455(3) 0.7810(4) 0.060(2) Uani 1 1 d . . . H74A H 0.7087 0.7773 0.7846 0.091 Uiso 1 1 calc R . . H74B H 0.7513 0.7336 0.7654 0.091 Uiso 1 1 calc R . . H74C H 0.7066 0.7331 0.8237 0.091 Uiso 1 1 calc R . . C75 C 0.6039(5) 0.6843(2) 0.7261(4) 0.058(2) Uani 1 1 d . . . H75A H 0.6111 0.6711 0.7689 0.087 Uiso 1 1 calc R . . H75B H 0.6514 0.6734 0.7084 0.087 Uiso 1 1 calc R . . H75C H 0.5445 0.6765 0.6966 0.087 Uiso 1 1 calc R . . C76 C 0.4577(4) 0.72677(19) 0.9101(3) 0.0319(17) Uani 1 1 d . . . H76 H 0.4030 0.7391 0.9195 0.038 Uiso 1 1 calc R . . C77 C 0.5371(5) 0.7907(2) 0.9782(3) 0.0340(17) Uani 1 1 d . . . H77X H 0.4805 0.8053 0.9653 0.041 Uiso 0.232(10) 1 calc PR B 2 C78 C 0.6136(5) 0.8138(2) 1.0154(3) 0.0410(19) Uani 1 1 d . B . C79 C 0.6930(5) 0.7899(2) 1.0345(3) 0.047(2) Uani 1 1 d . . . H79 H 0.7461 0.8042 1.0599 0.056 Uiso 1 1 calc R B . C80 C 0.7004(5) 0.7462(2) 1.0190(3) 0.0400(18) Uani 1 1 d . B . C81 C 0.6231(5) 0.7261(2) 0.9804(3) 0.0425(19) Uani 1 1 d . . . H81 H 0.6268 0.6966 0.9677 0.051 Uiso 0.768(10) 1 calc PR B 1 C82 C 0.5405(4) 0.7474(2) 0.9595(3) 0.0340(17) Uani 1 1 d . B . C83 C 0.6079(6) 0.8623(2) 1.0276(4) 0.056(2) Uani 1 1 d . . . C84 C 0.5879(6) 0.8860(3) 0.9613(4) 0.081(3) Uani 1 1 d . B . H84A H 0.5831 0.9174 0.9679 0.122 Uiso 1 1 calc R . . H84B H 0.5308 0.8752 0.9319 0.122 Uiso 1 1 calc R . . H84C H 0.6371 0.8804 0.9422 0.122 Uiso 1 1 calc R . . C85 C 0.5334(6) 0.8735(2) 1.0591(4) 0.072(3) Uani 1 1 d . B . H85A H 0.5405 0.8553 1.0977 0.108 Uiso 1 1 calc R . . H85B H 0.4740 0.8681 1.0278 0.108 Uiso 1 1 calc R . . H85C H 0.5382 0.9043 1.0718 0.108 Uiso 1 1 calc R . . C86 C 0.6964(6) 0.8798(3) 1.0736(4) 0.079(3) Uani 1 1 d . B . H86A H 0.7100 0.8645 1.1154 0.119 Uiso 1 1 calc R . . H86B H 0.6902 0.9111 1.0806 0.119 Uiso 1 1 calc R . . H86C H 0.7458 0.8751 1.0544 0.119 Uiso 1 1 calc R . . C87 C 0.7926(5) 0.7222(2) 1.0436(3) 0.050(2) Uani 1 1 d D . . C88 C 0.8250(7) 0.7218(4) 1.1202(4) 0.064(4) Uani 0.730(12) 1 d PDU B 1 H88A H 0.7790 0.7076 1.1364 0.096 Uiso 0.730(12) 1 calc PR B 1 H88B H 0.8341 0.7518 1.1365 0.096 Uiso 0.730(12) 1 calc PR B 1 H88C H 0.8821 0.7057 1.1355 0.096 Uiso 0.730(12) 1 calc PR B 1 C89 C 0.7848(7) 0.6737(3) 1.0237(6) 0.065(4) Uani 0.730(12) 1 d PDU B 1 H89A H 0.7373 0.6598 1.0386 0.097 Uiso 0.730(12) 1 calc PR B 1 H89B H 0.8426 0.6591 1.0437 0.097 Uiso 0.730(12) 1 calc PR B 1 H89C H 0.7694 0.6714 0.9763 0.097 Uiso 0.730(12) 1 calc PR B 1 C90 C 0.8657(7) 0.7440(4) 1.0204(6) 0.066(4) Uani 0.730(12) 1 d PDU B 1 H90A H 0.8705 0.7748 1.0331 0.099 Uiso 0.730(12) 1 calc PR B 1 H90B H 0.8502 0.7417 0.9729 0.099 Uiso 0.730(12) 1 calc PR B 1 H90C H 0.9238 0.7294 1.0403 0.099 Uiso 0.730(12) 1 calc PR B 1 C88X C 0.781(2) 0.6818(8) 1.0801(17) 0.083(12) Uani 0.270(12) 1 d PDU B 2 H88D H 0.7636 0.6901 1.1189 0.124 Uiso 0.270(12) 1 calc PR B 2 H88E H 0.8376 0.6655 1.0932 0.124 Uiso 0.270(12) 1 calc PR B 2 H88F H 0.7330 0.6635 1.0520 0.124 Uiso 0.270(12) 1 calc PR B 2 C89X C 0.8209(19) 0.7123(11) 0.9821(11) 0.074(11) Uani 0.270(12) 1 d PDU B 2 H89D H 0.8316 0.7398 0.9622 0.110 Uiso 0.270(12) 1 calc PR B 2 H89E H 0.7726 0.6960 0.9510 0.110 Uiso 0.270(12) 1 calc PR B 2 H89F H 0.8765 0.6949 0.9940 0.110 Uiso 0.270(12) 1 calc PR B 2 C90X C 0.8588(15) 0.7554(8) 1.0853(16) 0.076(13) Uani 0.270(12) 1 d PDU B 2 H90D H 0.8644 0.7803 1.0583 0.114 Uiso 0.270(12) 1 calc PR B 2 H90E H 0.9181 0.7416 1.1033 0.114 Uiso 0.270(12) 1 calc PR B 2 H90F H 0.8362 0.7653 1.1209 0.114 Uiso 0.270(12) 1 calc PR B 2 C91 C 0.4556(4) 0.6584(2) 0.9747(3) 0.0303(16) Uani 1 1 d . . . C92 C 0.4487(4) 0.6137(2) 0.9823(3) 0.0355(18) Uani 1 1 d . . . C93 C 0.4331(4) 0.5889(2) 0.9260(3) 0.0410(19) Uani 1 1 d . . . H93 H 0.4276 0.5582 0.9296 0.049 Uiso 1 1 calc R . . C94 C 0.4250(5) 0.6061(2) 0.8644(3) 0.045(2) Uani 1 1 d . C . C95 C 0.4351(4) 0.6505(2) 0.8611(3) 0.0390(18) Uani 1 1 d . . . H95 H 0.4304 0.6632 0.8199 0.047 Uiso 1 1 calc R . . C96 C 0.4519(4) 0.6781(2) 0.9154(3) 0.0353(17) Uani 1 1 d . . . C97 C 0.4564(4) 0.5930(2) 1.0483(3) 0.0362(18) Uani 1 1 d . . . C98 C 0.5471(5) 0.6040(2) 1.0978(3) 0.052(2) Uani 1 1 d . . . H98A H 0.5512 0.5895 1.1392 0.078 Uiso 1 1 calc R . . H98B H 0.5518 0.6356 1.1044 0.078 Uiso 1 1 calc R . . H98C H 0.5965 0.5939 1.0815 0.078 Uiso 1 1 calc R . . C99 C 0.4524(5) 0.5434(2) 1.0452(3) 0.049(2) Uani 1 1 d . . . H99A H 0.5035 0.5324 1.0316 0.074 Uiso 1 1 calc R . . H99B H 0.3955 0.5343 1.0137 0.074 Uiso 1 1 calc R . . H99C H 0.4557 0.5318 1.0883 0.074 Uiso 1 1 calc R . . C100 C 0.3787(4) 0.6083(2) 1.0735(3) 0.0398(18) Uani 1 1 d . . . H10A H 0.3209 0.5993 1.0429 0.060 Uiso 1 1 calc R . . H10B H 0.3804 0.6401 1.0775 0.060 Uiso 1 1 calc R . . H10C H 0.3850 0.5952 1.1162 0.060 Uiso 1 1 calc R . . C101 C 0.4095(6) 0.5770(2) 0.8047(3) 0.066(2) Uani 1 1 d DU . . C102 C 0.3573(13) 0.5374(5) 0.8079(8) 0.091(6) Uani 0.525(10) 1 d PDU C 1 H10D H 0.3502 0.5200 0.7685 0.136 Uiso 0.525(10) 1 calc PR C 1 H10E H 0.2975 0.5456 0.8112 0.136 Uiso 0.525(10) 1 calc PR C 1 H10F H 0.3894 0.5202 0.8462 0.136 Uiso 0.525(10) 1 calc PR C 1 C103 C 0.3675(13) 0.6028(7) 0.7389(8) 0.097(6) Uani 0.525(10) 1 d PDU C 1 H10G H 0.4059 0.6279 0.7370 0.146 Uiso 0.525(10) 1 calc PR C 1 H10H H 0.3067 0.6130 0.7369 0.146 Uiso 0.525(10) 1 calc PR C 1 H10I H 0.3639 0.5835 0.7019 0.146 Uiso 0.525(10) 1 calc PR C 1 C104 C 0.5045(8) 0.5631(5) 0.8054(8) 0.093(5) Uani 0.525(10) 1 d PDU C 1 H10J H 0.5406 0.5890 0.8032 0.140 Uiso 0.525(10) 1 calc PR C 1 H10K H 0.5007 0.5443 0.7678 0.140 Uiso 0.525(10) 1 calc PR C 1 H10L H 0.5332 0.5470 0.8456 0.140 Uiso 0.525(10) 1 calc PR C 1 C1X C 0.4307(14) 0.5296(4) 0.8131(9) 0.070(5) Uani 0.475(10) 1 d PDU C 2 H1X1 H 0.4134 0.5186 0.8505 0.106 Uiso 0.475(10) 1 calc PR C 2 H1X2 H 0.4957 0.5252 0.8206 0.106 Uiso 0.475(10) 1 calc PR C 2 H1X3 H 0.3970 0.5139 0.7737 0.106 Uiso 0.475(10) 1 calc PR C 2 C2X C 0.2988(10) 0.5761(6) 0.7767(9) 0.110(7) Uani 0.475(10) 1 d PDU C 2 H2X1 H 0.2759 0.6060 0.7681 0.165 Uiso 0.475(10) 1 calc PR C 2 H2X2 H 0.2738 0.5626 0.8089 0.165 Uiso 0.475(10) 1 calc PR C 2 H2X3 H 0.2805 0.5592 0.7362 0.165 Uiso 0.475(10) 1 calc PR C 2 C3X C 0.4361(15) 0.5967(7) 0.7496(8) 0.103(7) Uani 0.475(10) 1 d PDU C 2 H3X1 H 0.4218 0.6279 0.7468 0.154 Uiso 0.475(10) 1 calc PR C 2 H3X2 H 0.4028 0.5823 0.7089 0.154 Uiso 0.475(10) 1 calc PR C 2 H3X3 H 0.5012 0.5927 0.7569 0.154 Uiso 0.475(10) 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0309(7) 0.0305(8) 0.0364(7) 0.0045(6) 0.0117(5) 0.0033(6) O1 0.026(3) 0.024(3) 0.045(3) 0.004(2) 0.012(2) 0.004(2) O2 0.034(4) 0.032(4) 0.039(4) -0.014(3) 0.005(3) 0.003(3) O2X 0.009(15) 0.05(2) 0.08(2) 0.017(16) -0.004(11) 0.002(14) O3 0.052(3) 0.042(4) 0.049(3) 0.001(3) 0.014(3) -0.016(3) O4 0.033(3) 0.037(3) 0.039(3) 0.012(2) 0.018(2) 0.009(2) O5 0.049(5) 0.035(4) 0.046(4) -0.008(3) 0.003(3) 0.012(4) O5X 0.024(12) 0.032(14) 0.042(13) 0.000(10) 0.006(9) 0.004(9) O6 0.050(3) 0.030(3) 0.039(3) -0.004(2) 0.018(2) -0.008(2) O7 0.047(3) 0.056(4) 0.034(3) -0.008(2) 0.006(2) 0.000(3) N1 0.032(4) 0.028(4) 0.044(4) 0.010(3) 0.016(3) 0.006(3) N2 0.025(3) 0.024(4) 0.042(3) 0.002(3) 0.008(3) 0.000(3) C1 0.040(5) 0.023(5) 0.057(5) 0.020(4) 0.021(4) 0.007(3) C2 0.037(5) 0.028(5) 0.066(6) 0.004(4) 0.015(4) 0.007(4) C3 0.052(5) 0.034(5) 0.068(6) 0.002(4) 0.013(4) 0.002(4) C4 0.043(5) 0.049(6) 0.073(6) 0.017(5) 0.017(5) 0.006(4) C5 0.049(5) 0.039(6) 0.056(5) 0.024(4) 0.021(4) 0.011(4) C6 0.037(5) 0.040(5) 0.051(5) 0.011(4) 0.022(4) 0.003(4) C7 0.056(5) 0.035(5) 0.049(5) 0.010(4) 0.000(4) 0.004(4) C8 0.082(6) 0.053(6) 0.056(5) -0.003(4) 0.019(5) 0.010(5) C9 0.056(6) 0.091(8) 0.069(6) 0.011(5) -0.012(5) 0.013(5) C10 0.085(6) 0.043(6) 0.052(5) 0.019(4) 0.040(5) 0.006(4) C11 0.090(7) 0.088(7) 0.057(6) 0.020(5) 0.038(5) 0.040(5) C12 0.087(7) 0.070(7) 0.054(5) 0.007(5) 0.029(5) 0.014(5) C13 0.045(5) 0.027(5) 0.042(4) 0.012(3) 0.017(4) -0.005(4) C14 0.030(4) 0.040(5) 0.019(4) 0.001(3) 0.007(3) 0.006(4) C15 0.036(4) 0.018(4) 0.039(4) 0.002(3) 0.015(3) 0.000(3) C16 0.036(4) 0.029(5) 0.043(4) 0.002(3) 0.015(3) 0.000(4) C17 0.034(4) 0.033(5) 0.028(4) -0.003(3) 0.011(3) 0.003(4) C18 0.044(5) 0.022(4) 0.028(4) -0.001(3) 0.010(3) 0.005(4) C19 0.029(4) 0.028(5) 0.025(4) -0.001(3) 0.007(3) 0.003(3) C20 0.029(4) 0.027(4) 0.035(4) -0.001(3) 0.012(3) 0.000(3) C24 0.026(4) 0.027(4) 0.036(4) -0.001(3) 0.005(3) 0.001(3) C21 0.042(5) 0.049(5) 0.058(5) 0.006(4) 0.024(4) 0.003(4) C22 0.034(5) 0.061(6) 0.053(5) 0.000(4) 0.006(4) 0.002(4) C23 0.038(5) 0.048(5) 0.059(5) -0.004(4) 0.020(4) 0.002(4) C25 0.027(4) 0.019(4) 0.043(5) -0.009(3) 0.014(4) -0.001(3) C26 0.029(4) 0.024(4) 0.036(4) -0.002(3) 0.008(3) 0.004(3) C27 0.036(4) 0.026(4) 0.037(4) -0.006(3) 0.008(4) -0.002(4) C28 0.037(5) 0.024(4) 0.040(4) -0.003(3) 0.016(4) -0.003(3) C29 0.029(4) 0.026(4) 0.044(5) 0.006(3) 0.008(3) 0.003(3) C30 0.024(4) 0.026(4) 0.034(4) 0.003(3) 0.006(3) -0.003(3) C31 0.032(4) 0.034(5) 0.039(4) -0.010(3) 0.011(3) -0.006(3) C32 0.052(5) 0.036(5) 0.055(5) 0.001(4) 0.017(4) 0.002(4) C33 0.043(5) 0.041(5) 0.039(4) -0.004(4) 0.004(4) 0.002(4) C34 0.051(5) 0.057(6) 0.035(4) -0.007(4) 0.007(4) 0.001(4) C35 0.032(4) 0.040(5) 0.043(4) -0.002(4) 0.009(4) 0.004(4) C36 0.081(7) 0.088(8) 0.066(6) -0.008(5) 0.030(5) 0.010(5) C37 0.060(6) 0.067(7) 0.098(7) -0.031(5) 0.013(6) 0.023(5) C38 0.067(6) 0.044(6) 0.159(9) -0.019(6) 0.054(6) 0.004(5) C39 0.039(5) 0.039(5) 0.040(5) 0.000(4) 0.011(4) -0.013(4) C40 0.048(5) 0.041(5) 0.041(5) 0.007(4) 0.017(4) -0.003(4) C41 0.054(5) 0.040(5) 0.043(5) 0.024(4) 0.011(4) 0.012(4) C42 0.033(5) 0.049(6) 0.041(5) 0.007(4) 0.015(4) 0.006(4) C43 0.036(5) 0.029(4) 0.038(4) 0.011(4) 0.015(4) 0.005(3) C44 0.028(4) 0.036(5) 0.036(4) 0.003(3) 0.007(4) 0.005(4) C45 0.071(6) 0.035(6) 0.072(6) 0.005(4) 0.022(5) -0.017(4) C46 0.107(8) 0.028(5) 0.113(7) -0.008(5) 0.053(6) -0.017(5) C47 0.105(8) 0.064(7) 0.098(7) 0.043(6) 0.033(6) -0.006(6) C48 0.071(6) 0.048(6) 0.072(6) 0.007(4) 0.020(5) -0.028(5) C49 0.047(5) 0.062(6) 0.040(5) 0.021(4) 0.012(4) 0.010(4) C50 0.083(8) 0.245(15) 0.059(6) 0.054(8) -0.015(6) -0.075(8) C51 0.074(7) 0.102(9) 0.103(8) -0.042(6) -0.025(6) 0.032(6) C52 0.090(7) 0.086(8) 0.061(6) 0.014(5) -0.007(5) 0.021(6) C53 0.029(4) 0.029(5) 0.033(4) 0.005(3) 0.017(4) 0.004(3) C54 0.031(4) 0.030(5) 0.020(4) -0.001(3) 0.005(3) 0.004(3) C55 0.039(5) 0.042(5) 0.033(4) 0.011(4) 0.008(3) 0.008(4) C56 0.058(5) 0.033(5) 0.034(4) 0.016(4) 0.017(4) 0.015(4) C57 0.045(5) 0.028(5) 0.041(5) 0.005(4) 0.011(4) -0.005(4) C58 0.036(4) 0.026(5) 0.036(4) 0.007(3) 0.016(4) 0.000(4) C59 0.034(4) 0.030(5) 0.046(4) 0.004(3) 0.008(4) 0.005(3) C60 0.046(5) 0.054(6) 0.073(6) -0.029(4) 0.007(4) -0.003(4) C61 0.034(5) 0.046(5) 0.059(5) -0.009(4) 0.004(4) -0.003(4) C62 0.030(4) 0.048(5) 0.030(4) 0.004(4) 0.001(3) -0.009(4) C63 0.041(5) 0.060(6) 0.051(5) -0.008(4) 0.009(4) -0.015(4) C64 0.054(5) 0.053(6) 0.051(5) -0.013(4) 0.016(4) -0.019(4) C65 0.030(4) 0.036(5) 0.021(4) 0.009(3) 0.006(3) 0.003(4) C66 0.030(4) 0.033(5) 0.031(4) -0.002(3) 0.010(3) 0.001(3) C67 0.033(4) 0.025(4) 0.028(4) 0.005(3) 0.012(3) 0.005(3) C68 0.036(4) 0.042(5) 0.030(4) 0.006(3) 0.011(3) 0.004(4) C69 0.030(4) 0.028(4) 0.039(4) 0.005(3) 0.010(3) 0.003(3) C70 0.035(4) 0.022(4) 0.038(4) 0.009(3) 0.007(3) 0.013(3) C71 0.030(4) 0.023(4) 0.035(4) 0.004(3) 0.012(3) 0.003(3) C72 0.046(5) 0.054(6) 0.044(5) 0.007(4) 0.027(4) 0.011(4) C73 0.058(5) 0.055(6) 0.053(5) 0.003(4) 0.033(4) 0.010(4) C74 0.043(5) 0.074(7) 0.071(6) 0.007(5) 0.027(5) 0.016(4) C75 0.077(6) 0.037(5) 0.075(6) 0.002(4) 0.045(5) 0.009(4) C76 0.039(4) 0.017(4) 0.042(4) 0.006(3) 0.015(4) 0.008(3) C77 0.041(5) 0.034(5) 0.031(4) 0.013(4) 0.017(4) 0.017(4) C78 0.055(6) 0.025(5) 0.052(5) -0.002(4) 0.030(4) -0.009(4) C79 0.051(5) 0.036(5) 0.062(5) 0.000(4) 0.031(4) -0.006(4) C80 0.046(5) 0.037(5) 0.042(4) 0.004(4) 0.020(4) 0.010(4) C81 0.048(5) 0.034(5) 0.047(5) -0.010(4) 0.016(4) -0.006(4) C82 0.026(4) 0.036(5) 0.042(4) 0.004(4) 0.013(4) 0.005(4) C83 0.085(7) 0.032(5) 0.059(5) -0.001(4) 0.035(5) -0.002(5) C84 0.138(9) 0.039(6) 0.078(7) 0.004(5) 0.050(6) -0.003(5) C85 0.118(8) 0.039(6) 0.069(6) 0.003(4) 0.041(6) 0.024(5) C86 0.093(7) 0.040(6) 0.108(8) -0.023(5) 0.033(6) -0.019(5) C87 0.038(5) 0.048(6) 0.063(6) -0.011(4) 0.015(4) 0.005(4) C88 0.058(8) 0.070(11) 0.065(8) 0.012(7) 0.019(6) 0.012(7) C89 0.044(7) 0.055(9) 0.086(10) -0.015(7) 0.004(7) 0.016(6) C90 0.044(8) 0.068(10) 0.094(11) 0.011(8) 0.034(8) 0.005(7) C88X 0.08(2) 0.09(3) 0.08(3) 0.03(2) 0.02(2) 0.03(2) C89X 0.027(18) 0.09(3) 0.11(3) 0.03(2) 0.035(18) 0.023(18) C90X 0.019(17) 0.06(2) 0.12(3) -0.05(2) -0.010(18) -0.004(15) C91 0.039(4) 0.021(4) 0.032(4) -0.001(4) 0.012(3) 0.003(3) C92 0.041(5) 0.027(5) 0.040(5) -0.001(4) 0.014(4) 0.006(3) C93 0.061(5) 0.020(4) 0.046(5) 0.000(4) 0.023(4) -0.004(4) C94 0.078(6) 0.026(5) 0.042(5) 0.005(4) 0.034(4) 0.009(4) C95 0.054(5) 0.030(5) 0.033(4) 0.004(4) 0.012(4) 0.007(4) C96 0.044(5) 0.027(5) 0.036(4) 0.003(4) 0.013(4) 0.004(3) C97 0.046(5) 0.029(5) 0.032(4) 0.004(3) 0.009(4) 0.009(4) C98 0.058(5) 0.053(6) 0.036(4) 0.006(4) 0.000(4) 0.010(4) C99 0.071(6) 0.030(5) 0.048(5) 0.006(4) 0.020(4) 0.011(4) C100 0.053(5) 0.029(5) 0.038(4) -0.001(3) 0.015(4) -0.004(4) C101 0.122(6) 0.036(4) 0.049(4) -0.019(4) 0.040(5) -0.004(4) C102 0.166(14) 0.057(10) 0.053(10) -0.029(8) 0.039(13) -0.041(10) C103 0.179(17) 0.064(12) 0.044(9) -0.012(7) 0.025(12) -0.014(14) C104 0.147(10) 0.066(13) 0.089(11) -0.035(9) 0.070(10) 0.011(8) C1X 0.119(14) 0.037(6) 0.055(10) -0.021(7) 0.026(12) 0.003(9) C2X 0.128(8) 0.070(14) 0.114(16) -0.062(12) 0.007(10) 0.025(10) C3X 0.216(18) 0.067(12) 0.017(9) -0.023(7) 0.021(12) -0.049(16) _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 O7 1.582(4) . ? V1 O4 1.930(4) . ? V1 O1 1.936(4) . ? V1 N2 2.097(5) . ? V1 N1 2.102(5) . ? O1 C14 1.331(6) . ? O2 C25 1.363(7) . ? O2X C29 1.45(3) . ? O3 C39 1.368(7) . ? O4 C66 1.318(6) . ? O5 C77 1.340(8) . ? O5X C81 1.402(18) . ? O6 C91 1.388(7) . ? N1 C13 1.298(7) . ? N1 C1 1.445(8) . ? N2 C65 1.296(7) . ? N2 C53 1.456(7) . ? C1 C6 1.389(9) . ? C1 C2 1.394(9) . ? C2 C3 1.396(9) . ? C2 C7 1.522(9) . ? C3 C4 1.391(9) . ? C4 C5 1.370(9) . ? C5 C6 1.408(9) . ? C6 C10 1.525(10) . ? C7 C9 1.523(9) . ? C7 C8 1.532(9) . ? C10 C12 1.518(10) . ? C10 C11 1.541(9) . ? C13 C15 1.425(8) . ? C14 C15 1.406(8) . ? C14 C19 1.406(8) . ? C15 C16 1.407(8) . ? C16 C17 1.380(8) . ? C17 C18 1.404(8) . ? C17 C20 1.523(8) . ? C18 C19 1.403(8) . ? C19 C24 1.516(8) . ? C20 C23 1.524(8) . ? C20 C21 1.531(8) . ? C20 C22 1.541(8) . ? C24 C44 1.524(8) . ? C24 C30 1.530(8) . ? C25 C30 1.391(8) . ? C25 C26 1.402(8) . ? C26 C27 1.391(8) . ? C26 C31 1.542(9) . ? C27 C28 1.385(8) . ? C28 C29 1.383(8) . ? C28 C35 1.543(8) . ? C29 C30 1.397(8) . ? C31 C34 1.541(8) . ? C31 C33 1.543(8) . ? C31 C32 1.548(8) . ? C35 C38 1.505(9) . ? C35 C37 1.513(9) . ? C35 C36 1.556(9) . ? C39 C40 1.393(9) . ? C39 C44 1.409(9) . ? C40 C41 1.384(9) . ? C40 C45 1.544(9) . ? C41 C42 1.382(9) . ? C42 C43 1.393(8) . ? C42 C49 1.550(9) . ? C43 C44 1.385(8) . ? C45 C48 1.521(10) . ? C45 C46 1.528(10) . ? C45 C47 1.557(10) . ? C49 C51 1.499(10) . ? C49 C50 1.523(10) . ? C49 C52 1.523(9) . ? C53 C54 1.401(8) . ? C53 C58 1.402(8) . ? C54 C55 1.379(8) . ? C54 C59 1.514(8) . ? C55 C56 1.384(9) . ? C56 C57 1.390(9) . ? C57 C58 1.377(8) . ? C58 C62 1.511(8) . ? C59 C60 1.513(8) . ? C59 C61 1.526(8) . ? C62 C63 1.522(8) . ? C62 C64 1.529(8) . ? C65 C67 1.440(8) . ? C66 C71 1.398(8) . ? C66 C67 1.408(8) . ? C67 C68 1.420(8) . ? C68 C69 1.370(8) . ? C69 C70 1.399(8) . ? C69 C72 1.535(8) . ? C70 C71 1.382(8) . ? C71 C76 1.520(8) . ? C72 C74 1.527(9) . ? C72 C73 1.530(9) . ? C72 C75 1.531(9) . ? C76 C96 1.501(8) . ? C76 C82 1.539(9) . ? C77 C82 1.394(9) . ? C77 C78 1.409(9) . ? C78 C79 1.386(9) . ? C78 C83 1.515(9) . ? C79 C80 1.392(9) . ? C80 C81 1.385(9) . ? C80 C87 1.552(9) . ? C81 C82 1.387(9) . ? C83 C86 1.532(10) . ? C83 C85 1.538(9) . ? C83 C84 1.546(10) . ? C87 C88X 1.506(15) . ? C87 C90 1.519(10) . ? C87 C90X 1.531(15) . ? C87 C89X 1.541(18) . ? C87 C89 1.543(11) . ? C87 C88 1.573(10) . ? C91 C92 1.387(8) . ? C91 C96 1.397(8) . ? C92 C93 1.390(8) . ? C92 C97 1.527(8) . ? C93 C94 1.395(8) . ? C94 C95 1.377(8) . ? C94 C101 1.521(9) . ? C95 C96 1.404(8) . ? C97 C99 1.520(8) . ? C97 C98 1.529(9) . ? C97 C100 1.530(8) . ? C101 C102 1.472(10) . ? C101 C1X 1.490(10) . ? C101 C3X 1.491(10) . ? C101 C104 1.526(10) . ? C101 C103 1.585(14) . ? C101 C2X 1.639(15) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O7 V1 O4 100.4(2) . . ? O7 V1 O1 100.7(2) . . ? O4 V1 O1 158.91(18) . . ? O7 V1 N2 112.4(2) . . ? O4 V1 N2 86.48(18) . . ? O1 V1 N2 85.86(18) . . ? O7 V1 N1 112.3(2) . . ? O4 V1 N1 85.03(19) . . ? O1 V1 N1 86.67(19) . . ? N2 V1 N1 135.3(2) . . ? C14 O1 V1 134.3(4) . . ? C66 O4 V1 134.6(4) . . ? C13 N1 C1 115.2(5) . . ? C13 N1 V1 124.5(4) . . ? C1 N1 V1 120.3(4) . . ? C65 N2 C53 114.8(5) . . ? C65 N2 V1 125.2(4) . . ? C53 N2 V1 119.8(4) . . ? C6 C1 C2 123.1(6) . . ? C6 C1 N1 118.2(6) . . ? C2 C1 N1 118.6(6) . . ? C1 C2 C3 117.4(7) . . ? C1 C2 C7 122.4(6) . . ? C3 C2 C7 120.2(7) . . ? C4 C3 C2 120.6(7) . . ? C5 C4 C3 120.8(7) . . ? C4 C5 C6 120.6(7) . . ? C1 C6 C5 117.4(7) . . ? C1 C6 C10 121.8(7) . . ? C5 C6 C10 120.8(7) . . ? C2 C7 C9 111.2(6) . . ? C2 C7 C8 112.7(6) . . ? C9 C7 C8 110.7(6) . . ? C12 C10 C6 115.3(6) . . ? C12 C10 C11 110.0(6) . . ? C6 C10 C11 110.9(7) . . ? N1 C13 C15 129.4(6) . . ? O1 C14 C15 121.7(6) . . ? O1 C14 C19 118.9(6) . . ? C15 C14 C19 119.4(6) . . ? C14 C15 C16 120.0(6) . . ? C14 C15 C13 121.6(6) . . ? C16 C15 C13 118.3(6) . . ? C17 C16 C15 122.2(6) . . ? C16 C17 C18 116.4(6) . . ? C16 C17 C20 120.4(6) . . ? C18 C17 C20 123.2(6) . . ? C19 C18 C17 123.8(6) . . ? C18 C19 C14 118.0(6) . . ? C18 C19 C24 120.7(6) . . ? C14 C19 C24 120.9(5) . . ? C17 C20 C23 112.4(5) . . ? C17 C20 C21 111.0(5) . . ? C23 C20 C21 108.6(5) . . ? C17 C20 C22 108.8(5) . . ? C23 C20 C22 107.7(6) . . ? C21 C20 C22 108.1(5) . . ? C19 C24 C44 116.4(5) . . ? C19 C24 C30 108.0(5) . . ? C44 C24 C30 113.6(5) . . ? O2 C25 C30 121.9(6) . . ? O2 C25 C26 115.7(6) . . ? C30 C25 C26 122.4(6) . . ? C27 C26 C25 116.4(6) . . ? C27 C26 C31 122.7(6) . . ? C25 C26 C31 120.9(6) . . ? C28 C27 C26 123.5(6) . . ? C29 C28 C27 117.8(6) . . ? C29 C28 C35 121.7(6) . . ? C27 C28 C35 120.6(6) . . ? C28 C29 C30 121.9(6) . . ? C28 C29 O2X 119.9(14) . . ? C30 C29 O2X 118.0(13) . . ? C25 C30 C29 118.0(6) . . ? C25 C30 C24 119.3(6) . . ? C29 C30 C24 122.5(6) . . ? C34 C31 C26 111.9(5) . . ? C34 C31 C33 107.2(5) . . ? C26 C31 C33 111.3(5) . . ? C34 C31 C32 106.8(5) . . ? C26 C31 C32 110.5(5) . . ? C33 C31 C32 108.9(5) . . ? C38 C35 C37 109.5(7) . . ? C38 C35 C28 110.2(5) . . ? C37 C35 C28 112.3(6) . . ? C38 C35 C36 108.9(6) . . ? C37 C35 C36 106.0(6) . . ? C28 C35 C36 109.9(6) . . ? O3 C39 C40 117.7(6) . . ? O3 C39 C44 120.3(6) . . ? C40 C39 C44 121.9(6) . . ? C41 C40 C39 117.5(7) . . ? C41 C40 C45 121.9(7) . . ? C39 C40 C45 120.7(7) . . ? C42 C41 C40 123.2(6) . . ? C41 C42 C43 117.5(7) . . ? C41 C42 C49 122.2(6) . . ? C43 C42 C49 120.2(7) . . ? C44 C43 C42 122.4(6) . . ? C43 C44 C39 117.5(6) . . ? C43 C44 C24 121.4(6) . . ? C39 C44 C24 120.8(6) . . ? C48 C45 C46 111.4(7) . . ? C48 C45 C40 110.9(6) . . ? C46 C45 C40 109.5(6) . . ? C48 C45 C47 107.1(6) . . ? C46 C45 C47 106.9(7) . . ? C40 C45 C47 110.9(7) . . ? C51 C49 C50 109.3(8) . . ? C51 C49 C52 107.3(6) . . ? C50 C49 C52 107.6(7) . . ? C51 C49 C42 109.9(6) . . ? C50 C49 C42 110.7(6) . . ? C52 C49 C42 111.9(7) . . ? C54 C53 C58 123.4(6) . . ? C54 C53 N2 118.5(6) . . ? C58 C53 N2 118.0(6) . . ? C55 C54 C53 117.2(6) . . ? C55 C54 C59 121.5(6) . . ? C53 C54 C59 121.2(6) . . ? C54 C55 C56 120.7(7) . . ? C55 C56 C57 120.7(6) . . ? C58 C57 C56 120.9(6) . . ? C57 C58 C53 117.0(6) . . ? C57 C58 C62 121.3(6) . . ? C53 C58 C62 121.7(6) . . ? C60 C59 C54 111.1(5) . . ? C60 C59 C61 109.4(5) . . ? C54 C59 C61 112.7(5) . . ? C58 C62 C63 111.6(5) . . ? C58 C62 C64 112.8(6) . . ? C63 C62 C64 109.7(5) . . ? N2 C65 C67 127.9(5) . . ? O4 C66 C71 120.3(5) . . ? O4 C66 C67 121.2(6) . . ? C71 C66 C67 118.4(5) . . ? C66 C67 C68 120.6(6) . . ? C66 C67 C65 122.0(5) . . ? C68 C67 C65 117.3(5) . . ? C69 C68 C67 121.1(6) . . ? C68 C69 C70 116.4(5) . . ? C68 C69 C72 124.1(6) . . ? C70 C69 C72 119.5(6) . . ? C71 C70 C69 124.8(6) . . ? C70 C71 C66 118.4(5) . . ? C70 C71 C76 120.9(6) . . ? C66 C71 C76 120.3(5) . . ? C74 C72 C73 110.4(6) . . ? C74 C72 C75 109.0(6) . . ? C73 C72 C75 108.2(6) . . ? C74 C72 C69 109.1(6) . . ? C73 C72 C69 111.0(6) . . ? C75 C72 C69 109.1(5) . . ? C96 C76 C71 116.9(5) . . ? C96 C76 C82 114.3(5) . . ? C71 C76 C82 105.0(5) . . ? O5 C77 C82 123.0(7) . . ? O5 C77 C78 113.8(7) . . ? C82 C77 C78 123.2(6) . . ? C79 C78 C77 115.0(7) . . ? C79 C78 C83 124.1(7) . . ? C77 C78 C83 120.7(7) . . ? C78 C79 C80 124.6(7) . . ? C81 C80 C79 117.1(7) . . ? C81 C80 C87 122.4(7) . . ? C79 C80 C87 120.4(7) . . ? C80 C81 C82 122.3(7) . . ? C80 C81 O5X 118.8(9) . . ? C82 C81 O5X 118.1(9) . . ? C81 C82 C77 117.7(6) . . ? C81 C82 C76 122.0(6) . . ? C77 C82 C76 119.8(6) . . ? C78 C83 C86 111.7(7) . . ? C78 C83 C85 112.6(6) . . ? C86 C83 C85 106.2(6) . . ? C78 C83 C84 107.9(6) . . ? C86 C83 C84 109.2(7) . . ? C85 C83 C84 109.1(7) . . ? C88X C87 C90 138.5(14) . . ? C88X C87 C90X 113.9(18) . . ? C90 C87 C90X 57.7(12) . . ? C88X C87 C89X 113.2(16) . . ? C90 C87 C89X 51.5(11) . . ? C90X C87 C89X 108.8(14) . . ? C88X C87 C89 48.7(13) . . ? C90 C87 C89 109.7(8) . . ? C90X C87 C89 141.9(13) . . ? C89X C87 C89 65.9(12) . . ? C88X C87 C80 109.1(13) . . ? C90 C87 C80 112.1(7) . . ? C90X C87 C80 105.9(12) . . ? C89X C87 C80 105.3(11) . . ? C89 C87 C80 112.0(7) . . ? C88X C87 C88 59.9(14) . . ? C90 C87 C88 108.0(8) . . ? C90X C87 C88 56.0(14) . . ? C89X C87 C88 144.4(12) . . ? C89 C87 C88 104.9(7) . . ? C80 C87 C88 109.8(6) . . ? C92 C91 O6 117.2(5) . . ? C92 C91 C96 123.6(6) . . ? O6 C91 C96 119.2(6) . . ? C91 C92 C93 116.0(6) . . ? C91 C92 C97 122.3(6) . . ? C93 C92 C97 121.7(6) . . ? C92 C93 C94 124.2(6) . . ? C95 C94 C93 116.4(6) . . ? C95 C94 C101 121.8(6) . . ? C93 C94 C101 121.7(6) . . ? C94 C95 C96 123.4(6) . . ? C91 C96 C95 116.4(6) . . ? C91 C96 C76 121.0(6) . . ? C95 C96 C76 122.5(6) . . ? C99 C97 C92 112.6(5) . . ? C99 C97 C98 105.6(5) . . ? C92 C97 C98 111.1(5) . . ? C99 C97 C100 107.2(5) . . ? C92 C97 C100 110.3(5) . . ? C98 C97 C100 109.9(5) . . ? C102 C101 C1X 45.0(8) . . ? C102 C101 C3X 130.8(12) . . ? C1X C101 C3X 112.8(12) . . ? C102 C101 C94 113.4(8) . . ? C1X C101 C94 119.7(9) . . ? C3X C101 C94 115.0(10) . . ? C102 C101 C104 107.9(11) . . ? C1X C101 C104 63.1(10) . . ? C3X C101 C104 68.3(9) . . ? C94 C101 C104 104.1(8) . . ? C102 C101 C103 111.6(10) . . ? C1X C101 C103 127.8(12) . . ? C94 C101 C103 112.5(10) . . ? C104 C101 C103 106.7(8) . . ? C102 C101 C2X 58.4(9) . . ? C1X C101 C2X 101.3(8) . . ? C3X C101 C2X 102.5(9) . . ? C94 C101 C2X 102.1(8) . . ? C104 C101 C2X 153.7(9) . . ? C103 C101 C2X 64.6(9) . . ? 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 O7 V1 O1 C14 -98.1(5) . . . . ? O4 V1 O1 C14 80.9(7) . . . . ? N2 V1 O1 C14 149.8(5) . . . . ? N1 V1 O1 C14 13.9(5) . . . . ? O7 V1 O4 C66 -95.8(6) . . . . ? O1 V1 O4 C66 85.2(7) . . . . ? N2 V1 O4 C66 16.4(6) . . . . ? N1 V1 O4 C66 152.4(6) . . . . ? O7 V1 N1 C13 97.5(5) . . . . ? O4 V1 N1 C13 -163.2(5) . . . . ? O1 V1 N1 C13 -2.6(5) . . . . ? N2 V1 N1 C13 -83.3(6) . . . . ? O7 V1 N1 C1 -84.7(5) . . . . ? O4 V1 N1 C1 14.5(5) . . . . ? O1 V1 N1 C1 175.1(5) . . . . ? N2 V1 N1 C1 94.4(5) . . . . ? O7 V1 N2 C65 98.2(5) . . . . ? O4 V1 N2 C65 -1.6(5) . . . . ? O1 V1 N2 C65 -161.9(5) . . . . ? N1 V1 N2 C65 -80.9(6) . . . . ? O7 V1 N2 C53 -85.7(5) . . . . ? O4 V1 N2 C53 174.5(5) . . . . ? O1 V1 N2 C53 14.2(4) . . . . ? N1 V1 N2 C53 95.2(5) . . . . ? C13 N1 C1 C6 -94.8(7) . . . . ? V1 N1 C1 C6 87.3(6) . . . . ? C13 N1 C1 C2 88.1(7) . . . . ? V1 N1 C1 C2 -89.8(7) . . . . ? C6 C1 C2 C3 4.8(10) . . . . ? N1 C1 C2 C3 -178.3(6) . . . . ? C6 C1 C2 C7 -174.2(6) . . . . ? N1 C1 C2 C7 2.7(10) . . . . ? C1 C2 C3 C4 -3.2(10) . . . . ? C7 C2 C3 C4 175.8(6) . . . . ? C2 C3 C4 C5 1.1(11) . . . . ? C3 C4 C5 C6 -0.3(11) . . . . ? C2 C1 C6 C5 -4.0(10) . . . . ? N1 C1 C6 C5 179.0(5) . . . . ? C2 C1 C6 C10 177.1(6) . . . . ? N1 C1 C6 C10 0.2(9) . . . . ? C4 C5 C6 C1 1.7(10) . . . . ? C4 C5 C6 C10 -179.5(6) . . . . ? C1 C2 C7 C9 -100.0(8) . . . . ? C3 C2 C7 C9 81.0(8) . . . . ? C1 C2 C7 C8 135.0(7) . . . . ? C3 C2 C7 C8 -44.0(9) . . . . ? C1 C6 C10 C12 -144.9(6) . . . . ? C5 C6 C10 C12 36.3(9) . . . . ? C1 C6 C10 C11 89.4(7) . . . . ? C5 C6 C10 C11 -89.4(8) . . . . ? C1 N1 C13 C15 179.0(6) . . . . ? V1 N1 C13 C15 -3.1(10) . . . . ? V1 O1 C14 C15 -18.8(9) . . . . ? V1 O1 C14 C19 162.3(4) . . . . ? O1 C14 C15 C16 -175.3(5) . . . . ? C19 C14 C15 C16 3.6(9) . . . . ? O1 C14 C15 C13 8.7(9) . . . . ? C19 C14 C15 C13 -172.4(6) . . . . ? N1 C13 C15 C14 1.6(10) . . . . ? N1 C13 C15 C16 -174.4(6) . . . . ? C14 C15 C16 C17 -2.2(9) . . . . ? C13 C15 C16 C17 173.9(6) . . . . ? C15 C16 C17 C18 -1.8(9) . . . . ? C15 C16 C17 C20 176.0(5) . . . . ? C16 C17 C18 C19 4.7(9) . . . . ? C20 C17 C18 C19 -173.1(5) . . . . ? C17 C18 C19 C14 -3.3(9) . . . . ? C17 C18 C19 C24 -176.2(5) . . . . ? O1 C14 C19 C18 178.0(5) . . . . ? C15 C14 C19 C18 -0.9(8) . . . . ? O1 C14 C19 C24 -9.1(8) . . . . ? C15 C14 C19 C24 172.0(5) . . . . ? C16 C17 C20 C23 178.7(5) . . . . ? C18 C17 C20 C23 -3.6(8) . . . . ? C16 C17 C20 C21 56.8(8) . . . . ? C18 C17 C20 C21 -125.5(6) . . . . ? C16 C17 C20 C22 -62.1(7) . . . . ? C18 C17 C20 C22 115.6(6) . . . . ? C18 C19 C24 C44 -54.2(8) . . . . ? C14 C19 C24 C44 133.1(6) . . . . ? C18 C19 C24 C30 74.9(7) . . . . ? C14 C19 C24 C30 -97.8(6) . . . . ? O2 C25 C26 C27 176.3(5) . . . . ? C30 C25 C26 C27 -1.1(9) . . . . ? O2 C25 C26 C31 -5.8(8) . . . . ? C30 C25 C26 C31 176.7(6) . . . . ? C25 C26 C27 C28 2.4(9) . . . . ? C31 C26 C27 C28 -175.3(6) . . . . ? C26 C27 C28 C29 -1.2(9) . . . . ? C26 C27 C28 C35 179.9(6) . . . . ? C27 C28 C29 C30 -1.5(9) . . . . ? C35 C28 C29 C30 177.4(6) . . . . ? C27 C28 C29 O2X -176.0(13) . . . . ? C35 C28 C29 O2X 2.9(16) . . . . ? O2 C25 C30 C29 -178.7(5) . . . . ? C26 C25 C30 C29 -1.4(9) . . . . ? O2 C25 C30 C24 6.4(9) . . . . ? C26 C25 C30 C24 -176.3(5) . . . . ? C28 C29 C30 C25 2.8(9) . . . . ? O2X C29 C30 C25 177.4(13) . . . . ? C28 C29 C30 C24 177.5(6) . . . . ? O2X C29 C30 C24 -7.9(15) . . . . ? C19 C24 C30 C25 83.1(7) . . . . ? C44 C24 C30 C25 -146.2(6) . . . . ? C19 C24 C30 C29 -91.6(7) . . . . ? C44 C24 C30 C29 39.1(8) . . . . ? C27 C26 C31 C34 -2.1(9) . . . . ? C25 C26 C31 C34 -179.7(6) . . . . ? C27 C26 C31 C33 -122.0(6) . . . . ? C25 C26 C31 C33 60.3(8) . . . . ? C27 C26 C31 C32 116.8(6) . . . . ? C25 C26 C31 C32 -60.9(7) . . . . ? C29 C28 C35 C38 -110.4(7) . . . . ? C27 C28 C35 C38 68.4(8) . . . . ? C29 C28 C35 C37 12.0(9) . . . . ? C27 C28 C35 C37 -169.2(6) . . . . ? C29 C28 C35 C36 129.6(7) . . . . ? C27 C28 C35 C36 -51.5(8) . . . . ? O3 C39 C40 C41 175.4(6) . . . . ? C44 C39 C40 C41 -1.1(10) . . . . ? O3 C39 C40 C45 -5.6(10) . . . . ? C44 C39 C40 C45 177.9(6) . . . . ? C39 C40 C41 C42 -0.2(10) . . . . ? C45 C40 C41 C42 -179.3(6) . . . . ? C40 C41 C42 C43 1.0(10) . . . . ? C40 C41 C42 C49 -177.5(6) . . . . ? C41 C42 C43 C44 -0.4(9) . . . . ? C49 C42 C43 C44 178.1(6) . . . . ? C42 C43 C44 C39 -0.8(9) . . . . ? C42 C43 C44 C24 -175.1(6) . . . . ? O3 C39 C44 C43 -174.8(6) . . . . ? C40 C39 C44 C43 1.6(10) . . . . ? O3 C39 C44 C24 -0.4(9) . . . . ? C40 C39 C44 C24 176.0(6) . . . . ? C19 C24 C44 C43 -10.0(8) . . . . ? C30 C24 C44 C43 -136.4(6) . . . . ? C19 C24 C44 C39 175.9(5) . . . . ? C30 C24 C44 C39 49.5(8) . . . . ? C41 C40 C45 C48 -117.6(8) . . . . ? C39 C40 C45 C48 63.4(9) . . . . ? C41 C40 C45 C46 119.0(8) . . . . ? C39 C40 C45 C46 -60.0(9) . . . . ? C41 C40 C45 C47 1.2(10) . . . . ? C39 C40 C45 C47 -177.8(7) . . . . ? C41 C42 C49 C51 97.1(9) . . . . ? C43 C42 C49 C51 -81.3(8) . . . . ? C41 C42 C49 C50 -142.0(8) . . . . ? C43 C42 C49 C50 39.6(10) . . . . ? C41 C42 C49 C52 -22.0(9) . . . . ? C43 C42 C49 C52 159.6(6) . . . . ? C65 N2 C53 C54 90.6(7) . . . . ? V1 N2 C53 C54 -85.9(6) . . . . ? C65 N2 C53 C58 -90.6(7) . . . . ? V1 N2 C53 C58 92.9(5) . . . . ? C58 C53 C54 C55 2.1(9) . . . . ? N2 C53 C54 C55 -179.2(5) . . . . ? C58 C53 C54 C59 -178.7(5) . . . . ? N2 C53 C54 C59 0.0(8) . . . . ? C53 C54 C55 C56 -0.2(9) . . . . ? C59 C54 C55 C56 -179.4(5) . . . . ? C54 C55 C56 C57 -1.6(9) . . . . ? C55 C56 C57 C58 1.7(9) . . . . ? C56 C57 C58 C53 0.1(9) . . . . ? C56 C57 C58 C62 -179.2(6) . . . . ? C54 C53 C58 C57 -2.0(9) . . . . ? N2 C53 C58 C57 179.2(5) . . . . ? C54 C53 C58 C62 177.3(5) . . . . ? N2 C53 C58 C62 -1.4(8) . . . . ? C55 C54 C59 C60 84.1(7) . . . . ? C53 C54 C59 C60 -95.1(7) . . . . ? C55 C54 C59 C61 -39.1(8) . . . . ? C53 C54 C59 C61 141.7(6) . . . . ? C57 C58 C62 C63 -92.4(7) . . . . ? C53 C58 C62 C63 88.3(7) . . . . ? C57 C58 C62 C64 31.7(8) . . . . ? C53 C58 C62 C64 -147.6(6) . . . . ? C53 N2 C65 C67 177.1(6) . . . . ? V1 N2 C65 C67 -6.7(9) . . . . ? V1 O4 C66 C71 155.4(5) . . . . ? V1 O4 C66 C67 -22.0(9) . . . . ? O4 C66 C67 C68 -175.9(6) . . . . ? C71 C66 C67 C68 6.5(9) . . . . ? O4 C66 C67 C65 9.0(10) . . . . ? C71 C66 C67 C65 -168.5(6) . . . . ? N2 C65 C67 C66 4.7(10) . . . . ? N2 C65 C67 C68 -170.6(6) . . . . ? C66 C67 C68 C69 -3.8(10) . . . . ? C65 C67 C68 C69 171.6(6) . . . . ? C67 C68 C69 C70 -1.3(10) . . . . ? C67 C68 C69 C72 -178.3(6) . . . . ? C68 C69 C70 C71 3.6(10) . . . . ? C72 C69 C70 C71 -179.2(6) . . . . ? C69 C70 C71 C66 -0.8(10) . . . . ? C69 C70 C71 C76 -173.8(6) . . . . ? O4 C66 C71 C70 178.2(6) . . . . ? C67 C66 C71 C70 -4.3(9) . . . . ? O4 C66 C71 C76 -8.8(9) . . . . ? C67 C66 C71 C76 168.8(6) . . . . ? C68 C69 C72 C74 111.0(7) . . . . ? C70 C69 C72 C74 -65.9(8) . . . . ? C68 C69 C72 C73 -10.8(10) . . . . ? C70 C69 C72 C73 172.2(6) . . . . ? C68 C69 C72 C75 -130.0(7) . . . . ? C70 C69 C72 C75 53.1(8) . . . . ? C70 C71 C76 C96 -58.7(8) . . . . ? C66 C71 C76 C96 128.4(7) . . . . ? C70 C71 C76 C82 69.1(7) . . . . ? C66 C71 C76 C82 -103.7(7) . . . . ? O5 C77 C78 C79 179.8(6) . . . . ? C82 C77 C78 C79 -2.4(9) . . . . ? O5 C77 C78 C83 -4.9(9) . . . . ? C82 C77 C78 C83 172.8(6) . . . . ? C77 C78 C79 C80 0.5(9) . . . . ? C83 C78 C79 C80 -174.5(6) . . . . ? C78 C79 C80 C81 1.7(10) . . . . ? C78 C79 C80 C87 -179.2(6) . . . . ? C79 C80 C81 C82 -2.3(9) . . . . ? C87 C80 C81 C82 178.7(6) . . . . ? C79 C80 C81 O5X 167.1(10) . . . . ? C87 C80 C81 O5X -11.9(12) . . . . ? C80 C81 C82 C77 0.5(9) . . . . ? O5X C81 C82 C77 -168.9(9) . . . . ? C80 C81 C82 C76 172.5(6) . . . . ? O5X C81 C82 C76 3.1(12) . . . . ? O5 C77 C82 C81 179.5(6) . . . . ? C78 C77 C82 C81 1.9(9) . . . . ? O5 C77 C82 C76 7.3(9) . . . . ? C78 C77 C82 C76 -170.2(5) . . . . ? C96 C76 C82 C81 33.9(8) . . . . ? C71 C76 C82 C81 -95.5(7) . . . . ? C96 C76 C82 C77 -154.3(5) . . . . ? C71 C76 C82 C77 76.3(7) . . . . ? C79 C78 C83 C86 -10.0(9) . . . . ? C77 C78 C83 C86 175.2(6) . . . . ? C79 C78 C83 C85 -129.5(7) . . . . ? C77 C78 C83 C85 55.7(9) . . . . ? C79 C78 C83 C84 110.0(8) . . . . ? C77 C78 C83 C84 -64.8(8) . . . . ? C81 C80 C87 C88X -55.8(17) . . . . ? C79 C80 C87 C88X 125.2(17) . . . . ? C81 C80 C87 C90 120.2(9) . . . . ? C79 C80 C87 C90 -58.9(10) . . . . ? C81 C80 C87 C90X -178.8(16) . . . . ? C79 C80 C87 C90X 2.2(17) . . . . ? C81 C80 C87 C89X 66.0(15) . . . . ? C79 C80 C87 C89X -113.0(14) . . . . ? C81 C80 C87 C89 -3.7(10) . . . . ? C79 C80 C87 C89 177.3(7) . . . . ? C81 C80 C87 C88 -119.8(8) . . . . ? C79 C80 C87 C88 61.2(9) . . . . ? O6 C91 C92 C93 175.3(5) . . . . ? C96 C91 C92 C93 -3.0(9) . . . . ? O6 C91 C92 C97 -3.9(9) . . . . ? C96 C91 C92 C97 177.8(6) . . . . ? C91 C92 C93 C94 0.4(10) . . . . ? C97 C92 C93 C94 179.6(6) . . . . ? C92 C93 C94 C95 1.2(11) . . . . ? C92 C93 C94 C101 179.0(7) . . . . ? C93 C94 C95 C96 -0.5(10) . . . . ? C101 C94 C95 C96 -178.2(7) . . . . ? C92 C91 C96 C95 3.7(9) . . . . ? O6 C91 C96 C95 -174.6(5) . . . . ? C92 C91 C96 C76 178.6(6) . . . . ? O6 C91 C96 C76 0.3(9) . . . . ? C94 C95 C96 C91 -1.8(10) . . . . ? C94 C95 C96 C76 -176.7(6) . . . . ? C71 C76 C96 C91 176.6(6) . . . . ? C82 C76 C96 C91 53.4(8) . . . . ? C71 C76 C96 C95 -8.7(9) . . . . ? C82 C76 C96 C95 -131.9(6) . . . . ? C91 C92 C97 C99 -176.5(6) . . . . ? C93 C92 C97 C99 4.4(9) . . . . ? C91 C92 C97 C98 -58.3(8) . . . . ? C93 C92 C97 C98 122.6(7) . . . . ? C91 C92 C97 C100 63.8(8) . . . . ? C93 C92 C97 C100 -115.4(7) . . . . ? C95 C94 C101 C102 -151.2(11) . . . . ? C93 C94 C101 C102 31.2(14) . . . . ? C95 C94 C101 C1X 158.7(11) . . . . ? C93 C94 C101 C1X -18.9(14) . . . . ? C95 C94 C101 C3X 19.5(14) . . . . ? C93 C94 C101 C3X -158.1(12) . . . . ? C95 C94 C101 C104 91.8(10) . . . . ? C93 C94 C101 C104 -85.8(10) . . . . ? C95 C94 C101 C103 -23.4(12) . . . . ? C93 C94 C101 C103 159.0(9) . . . . ? C95 C94 C101 C2X -90.6(10) . . . . ? C93 C94 C101 C2X 91.8(10) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 O1 0.84 1.97 2.795(6) 165.7 . O5 H5 O4 0.84 2.06 2.892(7) 170.9 . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 22.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.447 _refine_diff_density_min -0.372 _refine_diff_density_rms 0.059 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 607718' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H15 N2 O4 V' _chemical_formula_weight 398.28 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 9.6923(18) _cell_length_b 11.754(2) _cell_length_c 16.214(3) _cell_angle_alpha 90.00 _cell_angle_beta 107.213(4) _cell_angle_gamma 90.00 _cell_volume 1764.5(6) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5618 _cell_measurement_theta_min 2.55 _cell_measurement_theta_max 29.20 _exptl_crystal_description Block _exptl_crystal_colour Blue _exptl_crystal_size_max 0.05 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.499 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 816 _exptl_absorpt_coefficient_mu 0.591 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.971 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_process_details 'SADABS v2.03 (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.6892 _diffrn_radiation_type Synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 19 _diffrn_reflns_number 12369 _diffrn_reflns_av_R_equivalents 0.0466 _diffrn_reflns_av_sigmaI/netI 0.0639 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 29.43 _reflns_number_total 4942 _reflns_number_gt 4077 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0511P)^2^+0.6533P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'All non-H atoms found by direct methods' _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4942 _refine_ls_number_parameters 245 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0544 _refine_ls_R_factor_gt 0.0432 _refine_ls_wR_factor_ref 0.1179 _refine_ls_wR_factor_gt 0.1104 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 0.41081(3) 0.44663(2) 0.126753(18) 0.01678(9) Uani 1 1 d . . . O1 O 0.49470(13) 0.49172(11) 0.24099(8) 0.0213(3) Uani 1 1 d . . . O2 O 0.53900(13) 0.32704(11) 0.13123(8) 0.0220(3) Uani 1 1 d . . . O3 O 0.22456(13) 0.49366(10) 0.11711(8) 0.0194(2) Uani 1 1 d . . . O4 O 0.46968(15) 0.55044(11) 0.08416(9) 0.0275(3) Uani 1 1 d . . . N1 N 0.32556(14) 0.30076(12) 0.20073(9) 0.0154(3) Uani 1 1 d . . . C1 C 0.39980(17) 0.32687(14) 0.29122(10) 0.0171(3) Uani 1 1 d . . . C2 C 0.48656(18) 0.42442(15) 0.30645(11) 0.0194(3) Uani 1 1 d . . . C3 C 0.5654(2) 0.45126(16) 0.39104(12) 0.0265(4) Uani 1 1 d . . . H3 H 0.6253 0.5169 0.4024 0.032 Uiso 1 1 calc R . . C4 C 0.5564(2) 0.38225(18) 0.45833(12) 0.0301(4) Uani 1 1 d . . . H4 H 0.6110 0.4007 0.5158 0.036 Uiso 1 1 calc R . . C5 C 0.4689(2) 0.28666(17) 0.44309(12) 0.0281(4) Uani 1 1 d . . . H5 H 0.4626 0.2406 0.4900 0.034 Uiso 1 1 calc R . . C6 C 0.3899(2) 0.25805(16) 0.35874(11) 0.0221(3) Uani 1 1 d . . . H6 H 0.3303 0.1923 0.3477 0.026 Uiso 1 1 calc R . . C7 C 0.49388(18) 0.21938(15) 0.13546(11) 0.0193(3) Uani 1 1 d . . . C8 C 0.38113(18) 0.19805(14) 0.17116(10) 0.0175(3) Uani 1 1 d . . . C9 C 0.3367(2) 0.08735(15) 0.17853(11) 0.0231(4) Uani 1 1 d . . . H9 H 0.2616 0.0731 0.2039 0.028 Uiso 1 1 calc R . . C10 C 0.4021(2) -0.00301(16) 0.14875(13) 0.0293(4) Uani 1 1 d . . . H10 H 0.3715 -0.0789 0.1535 0.035 Uiso 1 1 calc R . . C11 C 0.5118(2) 0.01817(18) 0.11233(13) 0.0304(4) Uani 1 1 d . . . H11 H 0.5563 -0.0436 0.0922 0.036 Uiso 1 1 calc R . . C12 C 0.5578(2) 0.12854(17) 0.10490(12) 0.0264(4) Uani 1 1 d . . . H12 H 0.6324 0.1422 0.0791 0.032 Uiso 1 1 calc R . . C13 C 0.12588(17) 0.42167(14) 0.13155(10) 0.0164(3) Uani 1 1 d . . . C14 C 0.17034(17) 0.31923(14) 0.17559(10) 0.0159(3) Uani 1 1 d . . . C15 C 0.06949(19) 0.24873(15) 0.19556(11) 0.0208(3) Uani 1 1 d . . . H15 H 0.0993 0.1806 0.2273 0.025 Uiso 1 1 calc R . . C16 C -0.07575(19) 0.27938(17) 0.16835(12) 0.0243(4) Uani 1 1 d . . . H16 H -0.1452 0.2315 0.1817 0.029 Uiso 1 1 calc R . . C17 C -0.12064(19) 0.37893(17) 0.12197(12) 0.0252(4) Uani 1 1 d . . . H17 H -0.2204 0.3979 0.1029 0.030 Uiso 1 1 calc R . . C18 C -0.02004(19) 0.45058(15) 0.10357(12) 0.0218(3) Uani 1 1 d . . . H18 H -0.0503 0.5189 0.0721 0.026 Uiso 1 1 calc R . . N2 N 0.30614(16) 0.36506(13) 0.00445(10) 0.0219(3) Uani 1 1 d . . . C19 C 0.27978(19) 0.34038(16) -0.06601(12) 0.0230(4) Uani 1 1 d . . . C20 C 0.2463(2) 0.3121(2) -0.15710(13) 0.0375(5) Uani 1 1 d . . . H20A H 0.1657 0.3593 -0.1905 0.056 Uiso 1 1 calc R . . H20B H 0.2193 0.2316 -0.1656 0.056 Uiso 1 1 calc R . . H20C H 0.3312 0.3263 -0.1767 0.056 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 0.01461(15) 0.01979(16) 0.01627(15) -0.00070(10) 0.00508(10) -0.00404(10) O1 0.0222(6) 0.0216(6) 0.0187(6) -0.0036(5) 0.0035(5) -0.0048(5) O2 0.0147(5) 0.0265(6) 0.0249(6) -0.0043(5) 0.0061(5) -0.0023(5) O3 0.0175(6) 0.0193(6) 0.0227(6) 0.0046(5) 0.0077(5) -0.0006(4) O4 0.0284(7) 0.0294(7) 0.0276(7) -0.0003(5) 0.0127(6) -0.0110(5) N1 0.0141(6) 0.0180(6) 0.0126(6) -0.0010(5) 0.0018(5) -0.0001(5) C1 0.0163(7) 0.0198(8) 0.0135(7) -0.0024(6) 0.0018(5) 0.0035(6) C2 0.0182(8) 0.0213(8) 0.0168(7) -0.0031(6) 0.0021(6) 0.0034(6) C3 0.0258(9) 0.0272(9) 0.0208(8) -0.0078(7) -0.0017(7) 0.0026(7) C4 0.0335(10) 0.0353(10) 0.0161(8) -0.0058(7) -0.0012(7) 0.0109(8) C5 0.0362(10) 0.0320(10) 0.0154(8) 0.0028(7) 0.0063(7) 0.0125(8) C6 0.0256(8) 0.0225(8) 0.0181(8) 0.0019(6) 0.0066(6) 0.0045(6) C7 0.0155(7) 0.0245(8) 0.0155(7) -0.0031(6) 0.0010(6) 0.0007(6) C8 0.0173(7) 0.0201(8) 0.0135(7) -0.0019(6) 0.0022(6) 0.0014(6) C9 0.0288(9) 0.0207(8) 0.0188(8) 0.0009(6) 0.0057(7) 0.0013(7) C10 0.0428(11) 0.0180(9) 0.0254(9) -0.0013(7) 0.0076(8) 0.0034(8) C11 0.0361(11) 0.0276(10) 0.0262(10) -0.0053(7) 0.0072(8) 0.0102(8) C12 0.0232(9) 0.0327(10) 0.0233(9) -0.0054(7) 0.0066(7) 0.0053(7) C13 0.0157(7) 0.0195(7) 0.0144(7) 0.0000(6) 0.0050(6) -0.0013(6) C14 0.0144(7) 0.0194(7) 0.0132(7) -0.0005(6) 0.0032(5) -0.0011(6) C15 0.0218(8) 0.0213(8) 0.0193(8) 0.0024(6) 0.0058(6) -0.0050(6) C16 0.0185(8) 0.0325(10) 0.0237(9) -0.0022(7) 0.0090(7) -0.0087(7) C17 0.0152(8) 0.0347(10) 0.0249(9) -0.0014(7) 0.0047(6) -0.0012(7) C18 0.0174(8) 0.0262(9) 0.0214(8) 0.0024(6) 0.0052(6) 0.0030(6) N2 0.0176(7) 0.0280(8) 0.0204(7) 0.0021(6) 0.0060(5) -0.0030(6) C19 0.0174(8) 0.0302(9) 0.0210(8) -0.0017(7) 0.0050(6) -0.0070(7) C20 0.0355(11) 0.0564(14) 0.0214(9) -0.0124(9) 0.0097(8) -0.0201(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 O1 1.8658(13) . ? V1 O2 1.8632(13) . ? V1 O3 1.8498(13) . ? V1 O4 1.5889(13) . ? V1 N1 2.3765(14) . ? V1 N2 2.1657(16) . ? O1 C2 1.345(2) . ? O2 C7 1.347(2) . ? O3 C13 1.348(2) . ? N1 C1 1.463(2) . ? N1 C8 1.460(2) . ? N1 C14 1.454(2) . ? C1 C2 1.400(2) . ? C1 C6 1.387(2) . ? C2 C3 1.395(2) . ? C3 C4 1.383(3) . ? C4 C5 1.385(3) . ? C5 C6 1.396(2) . ? C7 C8 1.402(2) . ? C7 C12 1.397(2) . ? C8 C9 1.387(2) . ? C9 C10 1.395(3) . ? C10 C11 1.383(3) . ? C11 C12 1.388(3) . ? C13 C14 1.401(2) . ? C13 C18 1.393(2) . ? C14 C15 1.391(2) . ? C15 C16 1.392(3) . ? C16 C17 1.389(3) . ? C17 C18 1.386(3) . ? N2 C19 1.132(2) . ? C19 C20 1.454(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 V1 O2 94.93(6) . . ? O1 V1 O3 97.28(6) . . ? O1 V1 O4 96.10(7) . . ? O1 V1 N1 79.53(5) . . ? O1 V1 N2 169.47(6) . . ? O2 V1 O3 148.39(6) . . ? O2 V1 O4 105.98(7) . . ? O2 V1 N1 76.32(5) . . ? O2 V1 N2 80.09(6) . . ? O3 V1 O4 101.58(7) . . ? O3 V1 N1 77.40(5) . . ? O3 V1 N2 82.76(6) . . ? O4 V1 N1 175.30(6) . . ? O4 V1 N2 94.19(7) . . ? N1 V1 N2 90.24(5) . . ? V1 O1 C2 120.42(11) . . ? V1 O2 C7 119.20(10) . . ? V1 O3 C13 121.49(11) . . ? V1 N1 C1 102.34(10) . . ? V1 N1 C8 102.35(10) . . ? V1 N1 C14 103.67(9) . . ? C1 N1 C8 112.53(12) . . ? C1 N1 C14 114.26(13) . . ? C8 N1 C14 118.90(13) . . ? N1 C1 C2 116.11(14) . . ? N1 C1 C6 122.75(15) . . ? C2 C1 C6 121.10(15) . . ? O1 C2 C1 121.00(15) . . ? O1 C2 C3 120.01(16) . . ? C1 C2 C3 118.98(17) . . ? C2 C3 C4 119.94(18) . . ? C3 C4 C5 120.89(17) . . ? C4 C5 C6 119.94(18) . . ? C1 C6 C5 119.14(18) . . ? O2 C7 C8 119.56(15) . . ? O2 C7 C12 121.01(16) . . ? C8 C7 C12 119.43(17) . . ? N1 C8 C7 113.33(14) . . ? N1 C8 C9 126.41(15) . . ? C7 C8 C9 120.22(16) . . ? C8 C9 C10 119.98(18) . . ? C9 C10 C11 119.79(18) . . ? C10 C11 C12 120.81(18) . . ? C7 C12 C11 119.74(18) . . ? O3 C13 C14 120.05(14) . . ? O3 C13 C18 119.62(15) . . ? C14 C13 C18 120.32(15) . . ? N1 C14 C13 114.07(14) . . ? N1 C14 C15 125.87(15) . . ? C13 C14 C15 119.96(15) . . ? C14 C15 C16 119.10(16) . . ? C15 C16 C17 120.98(16) . . ? C16 C17 C18 120.04(17) . . ? C13 C18 C17 119.51(17) . . ? V1 N2 C19 160.41(14) . . ? N2 C19 C20 178.4(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 V1 O1 C2 -67.85(13) . . . . ? O3 V1 O1 C2 82.92(13) . . . . ? O4 V1 O1 C2 -174.54(13) . . . . ? N1 V1 O1 C2 7.23(12) . . . . ? N2 V1 O1 C2 -6.6(4) . . . . ? O1 V1 O2 C7 105.13(12) . . . . ? O3 V1 O2 C7 -7.37(19) . . . . ? O4 V1 O2 C7 -157.07(12) . . . . ? N1 V1 O2 C7 27.17(12) . . . . ? N2 V1 O2 C7 -65.51(12) . . . . ? O1 V1 O3 C13 -94.27(12) . . . . ? O2 V1 O3 C13 17.62(18) . . . . ? O4 V1 O3 C13 167.94(12) . . . . ? N1 V1 O3 C13 -16.75(12) . . . . ? N2 V1 O3 C13 75.12(12) . . . . ? O1 V1 N1 C1 -5.02(9) . . . . ? O1 V1 N1 C8 -121.72(10) . . . . ? O1 V1 N1 C14 114.06(10) . . . . ? O2 V1 N1 C1 92.73(10) . . . . ? O2 V1 N1 C8 -23.97(9) . . . . ? O2 V1 N1 C14 -148.18(10) . . . . ? O3 V1 N1 C1 -105.00(10) . . . . ? O3 V1 N1 C8 138.30(10) . . . . ? O3 V1 N1 C14 14.09(9) . . . . ? N2 V1 N1 C1 172.48(10) . . . . ? N2 V1 N1 C8 55.78(10) . . . . ? N2 V1 N1 C14 -68.44(10) . . . . ? V1 N1 C1 C2 2.53(16) . . . . ? V1 N1 C1 C6 -175.44(14) . . . . ? C8 N1 C1 C2 111.65(16) . . . . ? C8 N1 C1 C6 -66.3(2) . . . . ? C14 N1 C1 C2 -108.81(16) . . . . ? C14 N1 C1 C6 73.2(2) . . . . ? V1 O1 C2 C1 -8.4(2) . . . . ? V1 O1 C2 C3 171.44(13) . . . . ? N1 C1 C2 O1 2.8(2) . . . . ? N1 C1 C2 C3 -177.13(15) . . . . ? C6 C1 C2 O1 -179.24(16) . . . . ? C6 C1 C2 C3 0.9(2) . . . . ? O1 C2 C3 C4 179.69(17) . . . . ? C1 C2 C3 C4 -0.4(3) . . . . ? C2 C3 C4 C5 -0.5(3) . . . . ? C3 C4 C5 C6 0.9(3) . . . . ? N1 C1 C6 C5 177.45(15) . . . . ? C2 C1 C6 C5 -0.4(3) . . . . ? C4 C5 C6 C1 -0.5(3) . . . . ? V1 O2 C7 C8 -26.1(2) . . . . ? V1 O2 C7 C12 153.95(13) . . . . ? O2 C7 C8 N1 -0.2(2) . . . . ? O2 C7 C8 C9 -177.90(15) . . . . ? C12 C7 C8 N1 179.69(15) . . . . ? C12 C7 C8 C9 2.0(2) . . . . ? V1 N1 C8 C7 18.26(15) . . . . ? V1 N1 C8 C9 -164.26(15) . . . . ? C1 N1 C8 C7 -90.86(16) . . . . ? C1 N1 C8 C9 86.6(2) . . . . ? C14 N1 C8 C7 131.66(15) . . . . ? C14 N1 C8 C9 -50.9(2) . . . . ? N1 C8 C9 C10 -178.64(16) . . . . ? C7 C8 C9 C10 -1.3(3) . . . . ? C8 C9 C10 C11 0.3(3) . . . . ? C9 C10 C11 C12 -0.1(3) . . . . ? C10 C11 C12 C7 0.8(3) . . . . ? O2 C7 C12 C11 178.17(16) . . . . ? C8 C7 C12 C11 -1.8(3) . . . . ? V1 O3 C13 C14 16.8(2) . . . . ? V1 O3 C13 C18 -164.20(13) . . . . ? O3 C13 C14 N1 -0.9(2) . . . . ? O3 C13 C14 C15 175.65(15) . . . . ? C18 C13 C14 N1 -179.97(15) . . . . ? C18 C13 C14 C15 -3.4(2) . . . . ? V1 N1 C14 C13 -10.21(15) . . . . ? V1 N1 C14 C15 173.44(14) . . . . ? C1 N1 C14 C13 100.32(16) . . . . ? C1 N1 C14 C15 -76.0(2) . . . . ? C8 N1 C14 C13 -122.89(16) . . . . ? C8 N1 C14 C15 60.8(2) . . . . ? N1 C14 C15 C16 178.58(16) . . . . ? C13 C14 C15 C16 2.4(3) . . . . ? C14 C15 C16 C17 -0.1(3) . . . . ? C15 C16 C17 C18 -1.3(3) . . . . ? C16 C17 C18 C13 0.3(3) . . . . ? O3 C13 C18 C17 -177.04(16) . . . . ? C14 C13 C18 C17 2.0(3) . . . . ? O1 V1 N2 C19 -145.0(4) . . . . ? O2 V1 N2 C19 -82.5(5) . . . . ? O3 V1 N2 C19 124.2(5) . . . . ? O4 V1 N2 C19 23.0(5) . . . . ? N1 V1 N2 C19 -158.6(5) . . . . ? _diffrn_measured_fraction_theta_max 0.921 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.607 _refine_diff_density_min -0.342 _refine_diff_density_rms 0.119 #===END data_4 _database_code_depnum_ccdc_archive 'CCDC 607719' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C24.50 H24 N O5 V' _chemical_formula_weight 463.39 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 23.7193(13) _cell_length_b 9.6174(5) _cell_length_c 21.0836(12) _cell_angle_alpha 90.00 _cell_angle_beta 116.030(2) _cell_angle_gamma 90.00 _cell_volume 4321.7(4) _cell_formula_units_Z 8 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 3222 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 22.69 _exptl_crystal_description plate _exptl_crystal_colour blue _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1928 _exptl_absorpt_coefficient_mu 0.496 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.957 _exptl_absorpt_correction_T_max 0.995 _exptl_absorpt_process_details 'SADABS v2.10, Sheldrick, G.M., (2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.6751 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker Apex II' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 3 _diffrn_reflns_number 25481 _diffrn_reflns_av_R_equivalents 0.0680 _diffrn_reflns_av_sigmaI/netI 0.0657 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 23.28 _reflns_number_total 7242 _reflns_number_gt 4922 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0425P)^2^+3.1275P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary heavy _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens 'geom except OH coords freely refined' _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7242 _refine_ls_number_parameters 586 _refine_ls_number_restraints 53 _refine_ls_R_factor_all 0.0801 _refine_ls_R_factor_gt 0.0439 _refine_ls_wR_factor_ref 0.1063 _refine_ls_wR_factor_gt 0.0922 _refine_ls_goodness_of_fit_ref 1.004 _refine_ls_restrained_S_all 1.007 _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 0.17496(2) 0.20338(6) 0.72800(3) 0.01605(15) Uani 1 1 d . . . O1 O 0.16043(9) 0.2001(2) 0.80988(11) 0.0186(5) Uani 1 1 d . . . O2 O 0.10001(9) 0.1162(2) 0.66980(11) 0.0184(5) Uani 1 1 d . . . O3 O 0.22264(9) 0.3635(2) 0.75017(11) 0.0179(5) Uani 1 1 d . . . O4 O 0.22587(10) 0.0824(2) 0.75507(11) 0.0217(5) Uani 1 1 d . . . N1 N 0.09859(11) 0.3819(3) 0.70088(13) 0.0163(6) Uani 1 1 d . . . C1 C 0.11208(14) 0.2746(3) 0.81106(16) 0.0179(7) Uani 1 1 d . . . C2 C 0.09532(15) 0.2565(3) 0.86628(17) 0.0205(8) Uani 1 1 d . . . H2 H 0.1183 0.1943 0.9038 0.025 Uiso 1 1 calc R . . C3 C 0.04514(15) 0.3299(4) 0.86588(18) 0.0232(8) Uani 1 1 d . . . H3 H 0.0338 0.3172 0.9035 0.028 Uiso 1 1 calc R . . C4 C 0.01116(15) 0.4211(4) 0.81221(18) 0.0254(8) Uani 1 1 d . . . H4 H -0.0233 0.4706 0.8127 0.030 Uiso 1 1 calc R . . C5 C 0.02806(15) 0.4397(4) 0.75707(17) 0.0227(8) Uani 1 1 d . . . H5A H 0.0049 0.5016 0.7194 0.027 Uiso 1 1 calc R . . C6 C 0.07878(14) 0.3677(3) 0.75757(16) 0.0177(7) Uani 1 1 d . . . C7 C 0.05239(14) 0.1932(3) 0.62136(16) 0.0173(7) Uani 1 1 d . . . C8 C 0.00719(15) 0.1314(4) 0.56095(17) 0.0221(8) Uani 1 1 d . . . H8 H 0.0083 0.0341 0.5537 0.027 Uiso 1 1 calc R . . C9 C -0.03917(15) 0.2122(4) 0.51167(18) 0.0253(8) Uani 1 1 d . . . H9 H -0.0697 0.1704 0.4699 0.030 Uiso 1 1 calc R . . C10 C -0.04200(15) 0.3537(4) 0.52208(18) 0.0256(8) Uani 1 1 d . . . H10A H -0.0741 0.4086 0.4876 0.031 Uiso 1 1 calc R . . C11 C 0.00247(15) 0.4148(4) 0.58329(17) 0.0222(8) Uani 1 1 d . . . H11 H 0.0004 0.5116 0.5910 0.027 Uiso 1 1 calc R . . C12 C 0.04984(14) 0.3353(3) 0.63308(16) 0.0184(7) Uani 1 1 d . . . C13 C 0.19733(14) 0.4904(3) 0.72820(16) 0.0170(7) Uani 1 1 d . . . C14 C 0.23535(16) 0.6038(4) 0.73271(17) 0.0230(8) Uani 1 1 d . . . H14 H 0.2792 0.5918 0.7488 0.028 Uiso 1 1 calc R . . C15 C 0.20861(16) 0.7339(4) 0.71356(17) 0.0249(8) Uani 1 1 d . . . H15 H 0.2345 0.8115 0.7168 0.030 Uiso 1 1 calc R . . C16 C 0.14484(17) 0.7533(4) 0.68979(18) 0.0260(8) Uani 1 1 d . . . H16 H 0.1271 0.8435 0.6770 0.031 Uiso 1 1 calc R . . C17 C 0.10706(15) 0.6410(3) 0.68480(17) 0.0210(8) Uani 1 1 d . . . H17 H 0.0633 0.6541 0.6690 0.025 Uiso 1 1 calc R . . C18 C 0.13244(14) 0.5094(3) 0.70258(16) 0.0181(7) Uani 1 1 d . . . O5 O 0.17757(10) 0.2397(2) 0.63113(11) 0.0195(5) Uani 1 1 d . . . H5 H 0.2053(16) 0.288(4) 0.6357(19) 0.029 Uiso 1 1 d . . . C19 C 0.16662(15) 0.1351(4) 0.57662(17) 0.0229(8) Uani 1 1 d . . . H19A H 0.1589 0.1826 0.5319 0.027 Uiso 1 1 calc R . . H19B H 0.1285 0.0813 0.5687 0.027 Uiso 1 1 calc R . . C20 C 0.22086(17) 0.0370(4) 0.59598(19) 0.0282(9) Uani 1 1 d . . . H20A H 0.2288 -0.0108 0.6407 0.034 Uiso 1 1 calc R . . H20B H 0.2590 0.0902 0.6034 0.034 Uiso 1 1 calc R . . C21 C 0.20734(18) -0.0701(4) 0.5382(2) 0.0407(11) Uani 1 1 d . . . H21A H 0.1680 -0.1182 0.5286 0.061 Uiso 1 1 calc R . . H21B H 0.2417 -0.1378 0.5536 0.061 Uiso 1 1 calc R . . H21C H 0.2036 -0.0235 0.4952 0.061 Uiso 1 1 calc R . . V2 V 0.24817(2) 0.43295(6) 0.52375(3) 0.01879(15) Uani 1 1 d . . . O6 O 0.27270(9) 0.3743(2) 0.61826(11) 0.0187(5) Uani 1 1 d . . . O7 O 0.24661(10) 0.2573(2) 0.48735(11) 0.0200(5) Uani 1 1 d . . . O8 O 0.28631(10) 0.6050(2) 0.54347(11) 0.0209(5) Uani 1 1 d . . . O9 O 0.17774(10) 0.4597(2) 0.51029(11) 0.0251(6) Uani 1 1 d . . . N2 N 0.35752(12) 0.3783(3) 0.56338(13) 0.0177(6) Uani 1 1 d . . . C22 C 0.33202(14) 0.3336(3) 0.66102(17) 0.0190(7) Uani 1 1 d . . . C23 C 0.34785(15) 0.2941(4) 0.73012(17) 0.0246(8) Uani 1 1 d . . . H23 H 0.3171 0.2946 0.7475 0.029 Uiso 1 1 calc R . . C24 C 0.40860(16) 0.2541(4) 0.77332(19) 0.0322(9) Uani 1 1 d . . . H24 H 0.4195 0.2275 0.8207 0.039 Uiso 1 1 calc R . . C25 C 0.45409(16) 0.2519(4) 0.74864(19) 0.0341(10) Uani 1 1 d . . . H25 H 0.4957 0.2238 0.7789 0.041 Uiso 1 1 calc R . . C26 C 0.43853(15) 0.2909(4) 0.67998(18) 0.0280(9) Uani 1 1 d . . . H26 H 0.4695 0.2900 0.6628 0.034 Uiso 1 1 calc R . . C27 C 0.37761(14) 0.3313(3) 0.63614(16) 0.0173(7) Uani 1 1 d . . . C28 C 0.29548(14) 0.2116(3) 0.47588(16) 0.0190(7) Uani 1 1 d . . . C29 C 0.28634(16) 0.1090(4) 0.42595(17) 0.0241(8) Uani 1 1 d . . . H29 H 0.2457 0.0709 0.3993 0.029 Uiso 1 1 calc R . . C30 C 0.33655(16) 0.0628(4) 0.41535(18) 0.0279(8) Uani 1 1 d . . . H30 H 0.3304 -0.0068 0.3810 0.033 Uiso 1 1 calc R . . C31 C 0.39568(17) 0.1173(4) 0.45445(19) 0.0302(9) Uani 1 1 d . . . H31 H 0.4301 0.0839 0.4472 0.036 Uiso 1 1 calc R . . C32 C 0.40525(16) 0.2199(4) 0.50407(18) 0.0255(8) Uani 1 1 d . . . H32 H 0.4461 0.2562 0.5311 0.031 Uiso 1 1 calc R . . C33 C 0.35492(15) 0.2695(3) 0.51425(16) 0.0193(7) Uani 1 1 d . . . C34 C 0.34405(16) 0.6253(4) 0.54714(16) 0.0214(8) Uani 1 1 d . . . C35 C 0.36413(17) 0.7590(4) 0.54132(17) 0.0262(8) Uani 1 1 d . . . H35 H 0.3367 0.8361 0.5327 0.031 Uiso 1 1 calc R . . C36 C 0.42434(17) 0.7788(4) 0.54813(18) 0.0302(9) Uani 1 1 d . . . H36 H 0.4380 0.8697 0.5440 0.036 Uiso 1 1 calc R . . C37 C 0.46470(17) 0.6679(4) 0.56081(18) 0.0292(9) Uani 1 1 d . . . H37 H 0.5059 0.6828 0.5653 0.035 Uiso 1 1 calc R . . C38 C 0.44524(15) 0.5339(4) 0.56702(17) 0.0251(8) Uani 1 1 d . . . H38 H 0.4734 0.4578 0.5770 0.030 Uiso 1 1 calc R . . C39 C 0.38422(15) 0.5124(4) 0.55853(16) 0.0196(8) Uani 1 1 d . . . O10 O 0.23426(11) 0.4838(2) 0.41998(12) 0.0224(5) Uani 1 1 d U A . H10 H 0.2149(17) 0.428(4) 0.391(2) 0.034 Uiso 1 1 d . . . C40 C 0.21015(19) 0.6184(4) 0.38790(19) 0.0385(10) Uani 1 1 d DU . . H40A H 0.2178 0.6299 0.3457 0.046 Uiso 0.902(7) 1 calc PR A 1 H40B H 0.2333 0.6928 0.4218 0.046 Uiso 0.902(7) 1 calc PR A 1 H40C H 0.2478 0.6561 0.3851 0.046 Uiso 0.098(7) 1 calc PR A 2 H40D H 0.1826 0.5887 0.3390 0.046 Uiso 0.098(7) 1 calc PR A 2 C41 C 0.1385(2) 0.6350(5) 0.3659(3) 0.0572(16) Uani 0.902(7) 1 d PDU A 1 H41A H 0.1149 0.5773 0.3236 0.069 Uiso 0.902(7) 1 calc PR A 1 H41B H 0.1294 0.5993 0.4045 0.069 Uiso 0.902(7) 1 calc PR A 1 C42 C 0.1166(2) 0.7778(5) 0.3506(2) 0.0592(13) Uani 1 1 d DU . . H42A H 0.0715 0.7811 0.3373 0.089 Uiso 0.902(7) 1 calc PR A 1 H42B H 0.1245 0.8133 0.3117 0.089 Uiso 0.902(7) 1 calc PR A 1 H42C H 0.1390 0.8353 0.3927 0.089 Uiso 0.902(7) 1 calc PR A 1 H42D H 0.1083 0.8705 0.3639 0.089 Uiso 0.098(7) 1 calc PR A 2 H42E H 0.0905 0.7091 0.3597 0.089 Uiso 0.098(7) 1 calc PR A 2 H42F H 0.1067 0.7771 0.3004 0.089 Uiso 0.098(7) 1 calc PR A 2 C41X C 0.1799(10) 0.745(3) 0.3905(18) 0.036(3) Uani 0.098(7) 1 d PDU A 2 H41C H 0.1880 0.7560 0.4405 0.043 Uiso 0.098(7) 1 calc PR A 2 H41D H 0.2038 0.8195 0.3809 0.043 Uiso 0.098(7) 1 calc PR A 2 C43 C 0.36962(18) 0.9668(4) 0.8776(2) 0.0391(10) Uani 1 1 d . . . H43A H 0.4093 1.0101 0.9099 0.059 Uiso 1 1 calc R . . H43B H 0.3501 0.9228 0.9049 0.059 Uiso 1 1 calc R . . H43C H 0.3414 1.0379 0.8465 0.059 Uiso 1 1 calc R . . C44 C 0.38204(16) 0.8583(4) 0.83369(19) 0.0303(9) Uani 1 1 d . . . C45 C 0.41050(17) 0.7337(4) 0.8627(2) 0.0334(9) Uani 1 1 d . . . H45 H 0.4232 0.7166 0.9115 0.040 Uiso 1 1 calc R . . C46 C 0.42087(18) 0.6334(4) 0.8223(2) 0.0388(10) Uani 1 1 d . . . H46 H 0.4403 0.5481 0.8433 0.047 Uiso 1 1 calc R . . C47 C 0.40320(18) 0.6565(5) 0.7513(2) 0.0424(11) Uani 1 1 d . . . H47 H 0.4099 0.5872 0.7233 0.051 Uiso 1 1 calc R . . C48 C 0.37578(19) 0.7814(5) 0.7219(2) 0.0440(11) Uani 1 1 d . . . H48 H 0.3639 0.7988 0.6734 0.053 Uiso 1 1 calc R . . C49 C 0.36547(17) 0.8813(4) 0.76262(19) 0.0366(10) Uani 1 1 d . . . H49 H 0.3468 0.9673 0.7417 0.044 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 V1 0.0177(3) 0.0173(3) 0.0160(3) 0.0004(2) 0.0101(2) 0.0008(2) O1 0.0210(11) 0.0205(13) 0.0180(12) 0.0035(10) 0.0120(10) 0.0042(10) O2 0.0206(12) 0.0175(13) 0.0198(12) 0.0021(10) 0.0114(10) -0.0003(10) O3 0.0184(11) 0.0179(13) 0.0196(12) 0.0020(10) 0.0103(10) 0.0016(10) O4 0.0237(12) 0.0240(13) 0.0211(12) 0.0021(11) 0.0133(10) 0.0050(10) N1 0.0185(14) 0.0171(15) 0.0165(14) -0.0025(12) 0.0107(12) -0.0029(12) C1 0.0151(16) 0.0186(19) 0.0192(18) -0.0034(15) 0.0070(14) -0.0012(14) C2 0.0253(18) 0.0218(19) 0.0178(17) -0.0005(15) 0.0126(15) -0.0023(15) C3 0.0267(19) 0.028(2) 0.0227(19) -0.0053(16) 0.0180(16) -0.0036(16) C4 0.0227(18) 0.030(2) 0.030(2) -0.0045(17) 0.0170(16) 0.0018(16) C5 0.0220(18) 0.022(2) 0.0247(19) -0.0017(16) 0.0111(15) 0.0003(15) C6 0.0187(17) 0.0200(19) 0.0183(17) -0.0022(15) 0.0116(14) -0.0017(14) C7 0.0171(17) 0.023(2) 0.0180(17) 0.0029(15) 0.0130(14) 0.0005(15) C8 0.0259(19) 0.022(2) 0.0226(19) -0.0019(16) 0.0143(16) -0.0043(16) C9 0.0182(17) 0.038(2) 0.0207(19) -0.0022(17) 0.0093(15) -0.0040(17) C10 0.0205(18) 0.036(2) 0.0195(19) 0.0065(17) 0.0083(15) 0.0033(16) C11 0.0255(19) 0.0198(19) 0.0258(19) 0.0023(16) 0.0153(16) 0.0014(15) C12 0.0172(17) 0.027(2) 0.0141(17) 0.0012(15) 0.0098(14) -0.0013(15) C13 0.0223(18) 0.0184(19) 0.0141(17) -0.0020(14) 0.0113(14) -0.0010(15) C14 0.0233(18) 0.026(2) 0.0215(18) -0.0002(16) 0.0110(15) -0.0038(16) C15 0.033(2) 0.019(2) 0.0238(19) -0.0011(16) 0.0135(16) -0.0078(16) C16 0.037(2) 0.0147(19) 0.0254(19) 0.0053(15) 0.0132(17) 0.0023(16) C17 0.0237(18) 0.022(2) 0.0194(18) 0.0012(15) 0.0114(15) 0.0047(15) C18 0.0232(18) 0.0177(19) 0.0167(17) -0.0002(14) 0.0118(15) -0.0030(15) O5 0.0235(13) 0.0215(14) 0.0193(12) -0.0020(10) 0.0148(11) -0.0038(10) C19 0.0293(19) 0.027(2) 0.0188(18) -0.0068(16) 0.0166(16) -0.0048(16) C20 0.041(2) 0.022(2) 0.029(2) -0.0004(16) 0.0223(18) 0.0025(17) C21 0.043(2) 0.032(2) 0.065(3) -0.019(2) 0.039(2) -0.008(2) V2 0.0197(3) 0.0223(3) 0.0159(3) 0.0001(3) 0.0092(2) 0.0025(3) O6 0.0177(12) 0.0244(13) 0.0160(12) -0.0011(10) 0.0094(10) 0.0008(10) O7 0.0216(12) 0.0201(13) 0.0200(12) -0.0002(10) 0.0106(10) 0.0010(10) O8 0.0234(12) 0.0207(13) 0.0212(12) -0.0001(10) 0.0122(10) 0.0014(10) O9 0.0207(12) 0.0329(15) 0.0215(13) -0.0001(11) 0.0091(10) 0.0048(11) N2 0.0204(14) 0.0199(16) 0.0155(14) 0.0005(12) 0.0103(12) 0.0010(12) C22 0.0174(17) 0.0175(19) 0.0211(18) -0.0006(15) 0.0075(15) -0.0009(14) C23 0.0258(19) 0.033(2) 0.0193(18) 0.0030(16) 0.0144(16) -0.0005(17) C24 0.0254(19) 0.052(3) 0.0219(19) 0.0105(18) 0.0133(16) 0.0041(18) C25 0.0230(19) 0.055(3) 0.023(2) 0.0132(19) 0.0092(16) 0.0110(18) C26 0.0234(19) 0.040(2) 0.026(2) 0.0074(18) 0.0155(16) 0.0026(17) C27 0.0205(17) 0.0201(19) 0.0150(17) 0.0021(14) 0.0111(14) -0.0002(14) C28 0.0231(18) 0.0197(19) 0.0181(17) 0.0041(15) 0.0125(15) 0.0068(15) C29 0.0261(19) 0.025(2) 0.0202(18) 0.0021(16) 0.0091(15) 0.0000(16) C30 0.035(2) 0.029(2) 0.0192(19) -0.0036(17) 0.0120(17) 0.0072(18) C31 0.038(2) 0.032(2) 0.032(2) 0.0003(18) 0.0255(19) 0.0093(18) C32 0.0277(19) 0.025(2) 0.029(2) -0.0001(17) 0.0180(16) 0.0025(16) C33 0.0248(18) 0.0212(19) 0.0147(17) 0.0008(14) 0.0113(15) 0.0017(15) C34 0.030(2) 0.022(2) 0.0129(17) -0.0008(15) 0.0095(15) 0.0001(16) C35 0.042(2) 0.022(2) 0.0150(18) -0.0014(15) 0.0128(16) 0.0001(17) C36 0.041(2) 0.029(2) 0.0206(19) -0.0046(17) 0.0133(17) -0.0176(19) C37 0.029(2) 0.037(2) 0.0223(19) -0.0001(17) 0.0117(16) -0.0118(18) C38 0.0247(19) 0.034(2) 0.0167(18) -0.0019(16) 0.0088(15) -0.0009(16) C39 0.0244(18) 0.024(2) 0.0119(17) -0.0014(15) 0.0090(14) -0.0056(15) O10 0.0285(14) 0.0228(14) 0.0154(13) 0.0007(10) 0.0092(11) 0.0006(11) C40 0.060(2) 0.025(2) 0.019(2) 0.0073(17) 0.0067(19) 0.0024(18) C41 0.061(3) 0.039(3) 0.089(4) 0.025(3) 0.049(3) 0.015(2) C42 0.067(3) 0.060(3) 0.045(3) 0.013(2) 0.020(2) 0.024(2) C41X 0.036(3) 0.035(3) 0.035(3) 0.0001(10) 0.0159(16) 0.0000(10) C43 0.036(2) 0.056(3) 0.029(2) -0.002(2) 0.0177(19) 0.001(2) C44 0.0248(19) 0.042(2) 0.027(2) -0.0030(19) 0.0138(17) -0.0058(18) C45 0.033(2) 0.044(3) 0.027(2) -0.0030(19) 0.0162(18) -0.0134(19) C46 0.036(2) 0.039(3) 0.048(3) -0.002(2) 0.024(2) -0.0092(19) C47 0.043(2) 0.053(3) 0.046(3) -0.026(2) 0.033(2) -0.029(2) C48 0.052(3) 0.059(3) 0.027(2) -0.008(2) 0.024(2) -0.015(2) C49 0.038(2) 0.048(3) 0.024(2) 0.0006(19) 0.0130(18) -0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O4 1.591(2) . ? V1 O3 1.845(2) . ? V1 O2 1.859(2) . ? V1 O1 1.903(2) . ? V1 O5 2.100(2) . ? V1 N1 2.377(3) . ? O1 C1 1.362(4) . ? O2 C7 1.362(4) . ? O3 C13 1.350(4) . ? N1 C18 1.457(4) . ? N1 C12 1.460(4) . ? N1 C6 1.470(4) . ? C1 C6 1.384(4) . ? C1 C2 1.396(4) . ? C2 C3 1.380(4) . ? C3 C4 1.378(5) . ? C4 C5 1.398(4) . ? C5 C6 1.385(4) . ? C7 C8 1.388(4) . ? C7 C12 1.395(5) . ? C8 C9 1.375(5) . ? C9 C10 1.385(5) . ? C10 C11 1.389(5) . ? C11 C12 1.383(4) . ? C13 C14 1.391(4) . ? C13 C18 1.402(4) . ? C14 C15 1.381(5) . ? C15 C16 1.381(5) . ? C16 C17 1.378(5) . ? C17 C18 1.381(5) . ? O5 C19 1.462(4) . ? C19 C20 1.500(5) . ? C20 C21 1.518(5) . ? V2 O9 1.588(2) . ? V2 O8 1.843(2) . ? V2 O7 1.849(2) . ? V2 O6 1.900(2) . ? V2 O10 2.122(2) . ? V2 N2 2.408(3) . ? O6 C22 1.353(4) . ? O7 C28 1.357(4) . ? O8 C34 1.352(4) . ? N2 C33 1.454(4) . ? N2 C39 1.460(4) . ? N2 C27 1.464(4) . ? C22 C23 1.389(4) . ? C22 C27 1.394(4) . ? C23 C24 1.379(5) . ? C24 C25 1.388(5) . ? C25 C26 1.380(5) . ? C26 C27 1.386(4) . ? C28 C29 1.389(5) . ? C28 C33 1.397(4) . ? C29 C30 1.378(5) . ? C30 C31 1.381(5) . ? C31 C32 1.382(5) . ? C32 C33 1.387(4) . ? C34 C39 1.394(5) . ? C34 C35 1.396(5) . ? C35 C36 1.384(5) . ? C36 C37 1.378(5) . ? C37 C38 1.394(5) . ? C38 C39 1.394(4) . ? O10 C40 1.456(4) . ? C40 C41X 1.423(18) . ? C40 C41 1.560(6) . ? C41 C42 1.455(6) . ? C42 C41X 1.399(18) . ? C43 C44 1.507(5) . ? C44 C45 1.380(5) . ? C44 C49 1.390(5) . ? C45 C46 1.378(5) . ? C46 C47 1.384(5) . ? C47 C48 1.377(6) . ? C48 C49 1.380(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 V1 O3 103.59(11) . . ? O4 V1 O2 105.20(11) . . ? O3 V1 O2 147.80(10) . . ? O4 V1 O1 94.22(10) . . ? O3 V1 O1 96.83(9) . . ? O2 V1 O1 95.16(9) . . ? O4 V1 O5 97.41(10) . . ? O3 V1 O5 80.27(9) . . ? O2 V1 O5 82.00(9) . . ? O1 V1 O5 168.37(9) . . ? O4 V1 N1 173.13(10) . . ? O3 V1 N1 77.04(9) . . ? O2 V1 N1 76.12(9) . . ? O1 V1 N1 78.93(9) . . ? O5 V1 N1 89.44(9) . . ? C1 O1 V1 119.81(19) . . ? C7 O2 V1 119.20(19) . . ? C13 O3 V1 122.48(19) . . ? C18 N1 C12 118.3(2) . . ? C18 N1 C6 115.3(2) . . ? C12 N1 C6 111.7(2) . . ? C18 N1 V1 104.38(17) . . ? C12 N1 V1 101.90(18) . . ? C6 N1 V1 102.63(18) . . ? O1 C1 C6 120.6(3) . . ? O1 C1 C2 120.0(3) . . ? C6 C1 C2 119.4(3) . . ? C3 C2 C1 119.5(3) . . ? C4 C3 C2 121.5(3) . . ? C3 C4 C5 119.1(3) . . ? C6 C5 C4 119.7(3) . . ? C1 C6 C5 120.9(3) . . ? C1 C6 N1 116.8(3) . . ? C5 C6 N1 122.3(3) . . ? O2 C7 C8 120.5(3) . . ? O2 C7 C12 119.1(3) . . ? C8 C7 C12 120.4(3) . . ? C9 C8 C7 119.4(3) . . ? C8 C9 C10 120.9(3) . . ? C9 C10 C11 119.5(3) . . ? C12 C11 C10 120.3(3) . . ? C11 C12 C7 119.4(3) . . ? C11 C12 N1 127.1(3) . . ? C7 C12 N1 113.4(3) . . ? O3 C13 C14 120.5(3) . . ? O3 C13 C18 119.9(3) . . ? C14 C13 C18 119.6(3) . . ? C15 C14 C13 119.3(3) . . ? C14 C15 C16 121.2(3) . . ? C17 C16 C15 119.6(3) . . ? C16 C17 C18 120.4(3) . . ? C17 C18 C13 119.9(3) . . ? C17 C18 N1 126.5(3) . . ? C13 C18 N1 113.6(3) . . ? C19 O5 V1 125.39(19) . . ? O5 C19 C20 112.5(3) . . ? C19 C20 C21 110.8(3) . . ? O9 V2 O8 105.57(11) . . ? O9 V2 O7 104.24(11) . . ? O8 V2 O7 146.31(10) . . ? O9 V2 O6 92.84(10) . . ? O8 V2 O6 97.81(10) . . ? O7 V2 O6 96.03(10) . . ? O9 V2 O10 95.91(10) . . ? O8 V2 O10 82.21(10) . . ? O7 V2 O10 79.46(9) . . ? O6 V2 O10 170.91(9) . . ? O9 V2 N2 170.34(10) . . ? O8 V2 N2 76.73(9) . . ? O7 V2 N2 76.53(9) . . ? O6 V2 N2 77.51(9) . . ? O10 V2 N2 93.70(9) . . ? C22 O6 V2 122.33(19) . . ? C28 O7 V2 120.4(2) . . ? C34 O8 V2 121.8(2) . . ? C33 N2 C39 118.0(2) . . ? C33 N2 C27 114.6(3) . . ? C39 N2 C27 113.2(2) . . ? C33 N2 V2 101.96(18) . . ? C39 N2 V2 102.54(18) . . ? C27 N2 V2 103.69(17) . . ? O6 C22 C23 120.1(3) . . ? O6 C22 C27 120.4(3) . . ? C23 C22 C27 119.6(3) . . ? C24 C23 C22 119.5(3) . . ? C23 C24 C25 121.0(3) . . ? C26 C25 C24 119.7(3) . . ? C25 C26 C27 119.8(3) . . ? C26 C27 C22 120.5(3) . . ? C26 C27 N2 123.4(3) . . ? C22 C27 N2 116.1(3) . . ? O7 C28 C29 120.2(3) . . ? O7 C28 C33 119.4(3) . . ? C29 C28 C33 120.3(3) . . ? C30 C29 C28 119.6(3) . . ? C29 C30 C31 120.3(3) . . ? C30 C31 C32 120.6(3) . . ? C31 C32 C33 119.7(3) . . ? C32 C33 C28 119.4(3) . . ? C32 C33 N2 126.0(3) . . ? C28 C33 N2 114.6(3) . . ? O8 C34 C39 119.7(3) . . ? O8 C34 C35 120.3(3) . . ? C39 C34 C35 120.0(3) . . ? C36 C35 C34 119.6(3) . . ? C37 C36 C35 120.8(3) . . ? C36 C37 C38 120.2(3) . . ? C39 C38 C37 119.5(3) . . ? C38 C39 C34 119.9(3) . . ? C38 C39 N2 125.5(3) . . ? C34 C39 N2 114.6(3) . . ? C40 O10 V2 122.4(2) . . ? C41X C40 O10 147.3(17) . . ? C41X C40 C41 54.8(11) . . ? O10 C40 C41 112.5(3) . . ? C42 C41 C40 113.5(4) . . ? C41X C42 C41 57.7(12) . . ? C42 C41X C40 126.7(19) . . ? C45 C44 C49 117.9(4) . . ? C45 C44 C43 121.2(3) . . ? C49 C44 C43 120.9(4) . . ? C46 C45 C44 121.2(4) . . ? C45 C46 C47 120.3(4) . . ? C48 C47 C46 119.0(4) . . ? C47 C48 C49 120.4(4) . . ? C48 C49 C44 121.1(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 V1 O1 C1 -170.7(2) . . . . ? O3 V1 O1 C1 85.0(2) . . . . ? O2 V1 O1 C1 -65.0(2) . . . . ? O5 V1 O1 C1 10.2(6) . . . . ? N1 V1 O1 C1 9.7(2) . . . . ? O4 V1 O2 C7 -159.2(2) . . . . ? O3 V1 O2 C7 -6.6(3) . . . . ? O1 V1 O2 C7 105.0(2) . . . . ? O5 V1 O2 C7 -63.7(2) . . . . ? N1 V1 O2 C7 27.7(2) . . . . ? O4 V1 O3 C13 171.8(2) . . . . ? O2 V1 O3 C13 18.9(3) . . . . ? O1 V1 O3 C13 -92.2(2) . . . . ? O5 V1 O3 C13 76.4(2) . . . . ? N1 V1 O3 C13 -15.3(2) . . . . ? O3 V1 N1 C18 12.28(17) . . . . ? O2 V1 N1 C18 -149.77(19) . . . . ? O1 V1 N1 C18 112.03(18) . . . . ? O5 V1 N1 C18 -67.87(18) . . . . ? O3 V1 N1 C12 135.90(19) . . . . ? O2 V1 N1 C12 -26.14(17) . . . . ? O1 V1 N1 C12 -124.35(18) . . . . ? O5 V1 N1 C12 55.76(18) . . . . ? O3 V1 N1 C6 -108.40(19) . . . . ? O2 V1 N1 C6 89.56(18) . . . . ? O1 V1 N1 C6 -8.65(18) . . . . ? O5 V1 N1 C6 171.46(18) . . . . ? V1 O1 C1 C6 -9.1(4) . . . . ? V1 O1 C1 C2 170.4(2) . . . . ? O1 C1 C2 C3 -178.3(3) . . . . ? C6 C1 C2 C3 1.2(5) . . . . ? C1 C2 C3 C4 -0.2(5) . . . . ? C2 C3 C4 C5 -0.1(5) . . . . ? C3 C4 C5 C6 -0.6(5) . . . . ? O1 C1 C6 C5 177.5(3) . . . . ? C2 C1 C6 C5 -1.9(5) . . . . ? O1 C1 C6 N1 -0.5(4) . . . . ? C2 C1 C6 N1 -179.9(3) . . . . ? C4 C5 C6 C1 1.7(5) . . . . ? C4 C5 C6 N1 179.5(3) . . . . ? C18 N1 C6 C1 -105.8(3) . . . . ? C12 N1 C6 C1 115.4(3) . . . . ? V1 N1 C6 C1 7.0(3) . . . . ? C18 N1 C6 C5 76.2(4) . . . . ? C12 N1 C6 C5 -62.5(4) . . . . ? V1 N1 C6 C5 -170.9(3) . . . . ? V1 O2 C7 C8 154.9(2) . . . . ? V1 O2 C7 C12 -24.7(3) . . . . ? O2 C7 C8 C9 -177.8(3) . . . . ? C12 C7 C8 C9 1.9(5) . . . . ? C7 C8 C9 C10 -1.1(5) . . . . ? C8 C9 C10 C11 -0.3(5) . . . . ? C9 C10 C11 C12 1.0(5) . . . . ? C10 C11 C12 C7 -0.2(5) . . . . ? C10 C11 C12 N1 -177.6(3) . . . . ? O2 C7 C12 C11 178.5(3) . . . . ? C8 C7 C12 C11 -1.2(5) . . . . ? O2 C7 C12 N1 -3.8(4) . . . . ? C8 C7 C12 N1 176.6(3) . . . . ? C18 N1 C12 C11 -47.2(4) . . . . ? C6 N1 C12 C11 90.2(4) . . . . ? V1 N1 C12 C11 -160.9(3) . . . . ? C18 N1 C12 C7 135.3(3) . . . . ? C6 N1 C12 C7 -87.3(3) . . . . ? V1 N1 C12 C7 21.6(3) . . . . ? V1 O3 C13 C14 -166.1(2) . . . . ? V1 O3 C13 C18 15.8(4) . . . . ? O3 C13 C14 C15 -176.4(3) . . . . ? C18 C13 C14 C15 1.7(5) . . . . ? C13 C14 C15 C16 -0.3(5) . . . . ? C14 C15 C16 C17 -0.2(5) . . . . ? C15 C16 C17 C18 -0.8(5) . . . . ? C16 C17 C18 C13 2.2(5) . . . . ? C16 C17 C18 N1 179.1(3) . . . . ? O3 C13 C18 C17 175.4(3) . . . . ? C14 C13 C18 C17 -2.7(5) . . . . ? O3 C13 C18 N1 -1.8(4) . . . . ? C14 C13 C18 N1 -179.9(3) . . . . ? C12 N1 C18 C17 62.3(4) . . . . ? C6 N1 C18 C17 -73.6(4) . . . . ? V1 N1 C18 C17 174.6(3) . . . . ? C12 N1 C18 C13 -120.7(3) . . . . ? C6 N1 C18 C13 103.4(3) . . . . ? V1 N1 C18 C13 -8.4(3) . . . . ? O4 V1 O5 C19 56.1(2) . . . . ? O3 V1 O5 C19 158.7(2) . . . . ? O2 V1 O5 C19 -48.3(2) . . . . ? O1 V1 O5 C19 -124.9(5) . . . . ? N1 V1 O5 C19 -124.3(2) . . . . ? V1 O5 C19 C20 -74.3(3) . . . . ? O5 C19 C20 C21 179.6(3) . . . . ? O9 V2 O6 C22 179.6(2) . . . . ? O8 V2 O6 C22 -74.2(2) . . . . ? O7 V2 O6 C22 75.0(2) . . . . ? N2 V2 O6 C22 0.2(2) . . . . ? O9 V2 O7 C28 165.8(2) . . . . ? O8 V2 O7 C28 14.1(3) . . . . ? O6 V2 O7 C28 -99.8(2) . . . . ? O10 V2 O7 C28 72.3(2) . . . . ? N2 V2 O7 C28 -24.2(2) . . . . ? O9 V2 O8 C34 -169.7(2) . . . . ? O7 V2 O8 C34 -18.3(3) . . . . ? O6 V2 O8 C34 95.1(2) . . . . ? O10 V2 O8 C34 -75.7(2) . . . . ? N2 V2 O8 C34 20.0(2) . . . . ? O8 V2 N2 C33 -138.86(19) . . . . ? O7 V2 N2 C33 20.47(18) . . . . ? O6 V2 N2 C33 119.89(19) . . . . ? O10 V2 N2 C33 -57.76(19) . . . . ? O8 V2 N2 C39 -16.25(17) . . . . ? O7 V2 N2 C39 143.08(19) . . . . ? O6 V2 N2 C39 -117.50(19) . . . . ? O10 V2 N2 C39 64.85(18) . . . . ? O8 V2 N2 C27 101.8(2) . . . . ? O7 V2 N2 C27 -98.9(2) . . . . ? O6 V2 N2 C27 0.53(19) . . . . ? O10 V2 N2 C27 -177.12(19) . . . . ? V2 O6 C22 C23 178.8(2) . . . . ? V2 O6 C22 C27 -1.1(4) . . . . ? O6 C22 C23 C24 -179.4(3) . . . . ? C27 C22 C23 C24 0.5(5) . . . . ? C22 C23 C24 C25 -0.4(6) . . . . ? C23 C24 C25 C26 0.2(6) . . . . ? C24 C25 C26 C27 -0.2(6) . . . . ? C25 C26 C27 C22 0.4(5) . . . . ? C25 C26 C27 N2 178.0(3) . . . . ? O6 C22 C27 C26 179.4(3) . . . . ? C23 C22 C27 C26 -0.5(5) . . . . ? O6 C22 C27 N2 1.6(4) . . . . ? C23 C22 C27 N2 -178.3(3) . . . . ? C33 N2 C27 C26 70.8(4) . . . . ? C39 N2 C27 C26 -68.6(4) . . . . ? V2 N2 C27 C26 -179.0(3) . . . . ? C33 N2 C27 C22 -111.5(3) . . . . ? C39 N2 C27 C22 109.2(3) . . . . ? V2 N2 C27 C22 -1.2(3) . . . . ? V2 O7 C28 C29 -155.3(2) . . . . ? V2 O7 C28 C33 24.2(4) . . . . ? O7 C28 C29 C30 -179.4(3) . . . . ? C33 C28 C29 C30 1.1(5) . . . . ? C28 C29 C30 C31 0.5(5) . . . . ? C29 C30 C31 C32 -0.8(5) . . . . ? C30 C31 C32 C33 -0.6(5) . . . . ? C31 C32 C33 C28 2.2(5) . . . . ? C31 C32 C33 N2 -178.9(3) . . . . ? O7 C28 C33 C32 178.0(3) . . . . ? C29 C28 C33 C32 -2.5(5) . . . . ? O7 C28 C33 N2 -1.0(4) . . . . ? C29 C28 C33 N2 178.5(3) . . . . ? C39 N2 C33 C32 54.8(4) . . . . ? C27 N2 C33 C32 -82.5(4) . . . . ? V2 N2 C33 C32 166.2(3) . . . . ? C39 N2 C33 C28 -126.3(3) . . . . ? C27 N2 C33 C28 96.4(3) . . . . ? V2 N2 C33 C28 -14.9(3) . . . . ? V2 O8 C34 C39 -20.5(4) . . . . ? V2 O8 C34 C35 161.1(2) . . . . ? O8 C34 C35 C36 177.3(3) . . . . ? C39 C34 C35 C36 -1.1(5) . . . . ? C34 C35 C36 C37 -0.2(5) . . . . ? C35 C36 C37 C38 -0.1(5) . . . . ? C36 C37 C38 C39 1.6(5) . . . . ? C37 C38 C39 C34 -2.9(5) . . . . ? C37 C38 C39 N2 179.8(3) . . . . ? O8 C34 C39 C38 -175.8(3) . . . . ? C35 C34 C39 C38 2.7(5) . . . . ? O8 C34 C39 N2 1.8(4) . . . . ? C35 C34 C39 N2 -179.8(3) . . . . ? C33 N2 C39 C38 -60.2(4) . . . . ? C27 N2 C39 C38 77.7(4) . . . . ? V2 N2 C39 C38 -171.3(3) . . . . ? C33 N2 C39 C34 122.4(3) . . . . ? C27 N2 C39 C34 -99.7(3) . . . . ? V2 N2 C39 C34 11.4(3) . . . . ? O9 V2 O10 C40 57.6(3) . . . . ? O8 V2 O10 C40 -47.4(2) . . . . ? O7 V2 O10 C40 161.0(3) . . . . ? N2 V2 O10 C40 -123.4(3) . . . . ? V2 O10 C40 C41X -14(2) . . . . ? V2 O10 C40 C41 -73.7(4) . . . . ? C41X C40 C41 C42 19.9(19) . . . . ? O10 C40 C41 C42 165.3(4) . . . . ? C40 C41 C42 C41X -19.5(19) . . . . ? C41 C42 C41X C40 25(2) . . . . ? O10 C40 C41X C42 -100(3) . . . . ? C41 C40 C41X C42 -24(2) . . . . ? C49 C44 C45 C46 -1.6(5) . . . . ? C43 C44 C45 C46 178.9(3) . . . . ? C44 C45 C46 C47 0.5(5) . . . . ? C45 C46 C47 C48 0.7(6) . . . . ? C46 C47 C48 C49 -0.7(6) . . . . ? C47 C48 C49 C44 -0.4(6) . . . . ? C45 C44 C49 C48 1.5(5) . . . . ? C43 C44 C49 C48 -178.9(3) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5 O6 0.78(4) 1.97(4) 2.716(3) 160(4) . O10 H10 O1 0.79(4) 2.04(4) 2.831(3) 174(4) 4_565 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.732 _refine_diff_density_min -0.355 _refine_diff_density_rms 0.065 #===END data_5 _database_code_depnum_ccdc_archive 'CCDC 607720' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C27 H24 N3 O4 V' _chemical_formula_weight 505.43 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 9.2526(7) _cell_length_b 25.7210(18) _cell_length_c 9.8995(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.085(2) _cell_angle_gamma 90.00 _cell_volume 2355.9(3) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 4951 _cell_measurement_theta_min 2.86 _cell_measurement_theta_max 24.07 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.425 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1048 _exptl_absorpt_coefficient_mu 0.461 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.973 _exptl_absorpt_correction_T_max 0.986 _exptl_absorpt_process_details 'SADABS v2.10, Sheldrick, G.M., (2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.6751 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 9.8' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker Apex II' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 4 _diffrn_reflns_number 17474 _diffrn_reflns_av_R_equivalents 0.0453 _diffrn_reflns_av_sigmaI/netI 0.0659 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.09 _diffrn_reflns_theta_max 23.50 _reflns_number_total 8056 _reflns_number_gt 7594 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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. Data were twinned with 180 degree rotation about b, swapping a and c, with raceamic twinning. 3 batch scale factors refined. ; _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^)+(0.1911P)^2^+59.2875P] 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 0.00 _refine_ls_number_reflns 8056 _refine_ls_number_parameters 638 _refine_ls_number_restraints 747 _refine_ls_R_factor_all 0.1472 _refine_ls_R_factor_gt 0.1423 _refine_ls_wR_factor_ref 0.3814 _refine_ls_wR_factor_gt 0.3770 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.018 _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 1.0368(3) 0.70378(9) 0.5568(3) 0.0192(5) Uani 1 1 d U . . O1 O 1.1410(11) 0.7466(4) 0.4331(11) 0.0225(18) Uani 1 1 d U . . O2 O 0.8749(12) 0.7463(4) 0.5597(11) 0.0222(17) Uani 1 1 d U . . O3 O 1.1196(11) 0.6418(4) 0.5028(11) 0.0223(18) Uani 1 1 d U . . O4 O 1.1216(12) 0.7179(4) 0.6918(11) 0.024(2) Uani 1 1 d U . . N1 N 0.9175(14) 0.6840(5) 0.3497(13) 0.0202(15) Uani 1 1 d U . . V2 V 0.4190(3) 0.41040(10) 0.2985(3) 0.0211(6) Uani 1 1 d U . . O5 O 0.3134(12) 0.3742(4) 0.1638(12) 0.0255(18) Uani 1 1 d U . . O6 O 0.5587(11) 0.3581(4) 0.3078(11) 0.0197(17) Uani 1 1 d U . . O7 O 0.3653(12) 0.4761(4) 0.2470(12) 0.0269(19) Uani 1 1 d U . . O8 O 0.3194(11) 0.3999(4) 0.4246(11) 0.027(2) Uani 1 1 d U . . N3 N 0.5678(13) 0.4248(5) 0.1037(12) 0.0170(15) Uani 1 1 d U . . C1 C 1.1053(15) 0.7463(6) 0.3023(15) 0.016(2) Uani 1 1 d U . . C2 C 1.1843(15) 0.7792(6) 0.2135(16) 0.020(2) Uani 1 1 d U . . H2 H 1.2641 0.7988 0.2457 0.025 Uiso 1 1 calc R . . C3 C 1.1429(17) 0.7821(6) 0.0798(17) 0.026(3) Uani 1 1 d U . . H3 H 1.1916 0.8054 0.0211 0.031 Uiso 1 1 calc R . . C4 C 1.0313(18) 0.7515(6) 0.0294(17) 0.026(3) Uani 1 1 d U . . H4 H 1.0057 0.7528 -0.0635 0.032 Uiso 1 1 calc R . . C5 C 0.9581(15) 0.7191(5) 0.1184(15) 0.017(2) Uani 1 1 d U . . H5 H 0.8836 0.6979 0.0818 0.020 Uiso 1 1 calc R . . C6 C 0.9836(16) 0.7152(5) 0.2516(15) 0.020(2) Uani 1 1 d U . . C7 C 0.7563(17) 0.7349(6) 0.4861(17) 0.026(3) Uani 1 1 d U . . C8 C 0.6213(17) 0.7564(7) 0.518(2) 0.031(3) Uani 1 1 d U . . H8 H 0.6105 0.7804 0.5904 0.038 Uiso 1 1 calc R . . C9 C 0.5037(17) 0.7410(6) 0.4396(18) 0.026(3) Uani 1 1 d U . . H9 H 0.4098 0.7520 0.4658 0.032 Uiso 1 1 calc R . . C10 C 0.5177(17) 0.7099(7) 0.3231(17) 0.027(3) Uani 1 1 d U . . H10 H 0.4359 0.7028 0.2680 0.032 Uiso 1 1 calc R . . C11 C 0.6445(16) 0.6909(6) 0.2918(16) 0.022(2) Uani 1 1 d U . . H11 H 0.6539 0.6693 0.2146 0.026 Uiso 1 1 calc R . . C12 C 0.7693(15) 0.7024(6) 0.3723(15) 0.022(2) Uani 1 1 d U . . C13 C 1.0587(17) 0.6099(6) 0.4159(16) 0.022(3) Uani 1 1 d U . . C14 C 1.095(2) 0.5586(6) 0.3993(17) 0.030(3) Uani 1 1 d U . . H14 H 1.1647 0.5449 0.4603 0.036 Uiso 1 1 calc R . . C15 C 1.0438(16) 0.5264(6) 0.3083(15) 0.019(2) Uani 1 1 d U . . H15 H 1.0847 0.4928 0.2964 0.023 Uiso 1 1 calc R . . C16 C 0.9236(16) 0.5434(6) 0.2271(16) 0.020(3) Uani 1 1 d U . . H16 H 0.8731 0.5206 0.1681 0.024 Uiso 1 1 calc R . . C17 C 0.8852(15) 0.5972(5) 0.2411(14) 0.015(2) Uani 1 1 d U . . H17 H 0.8123 0.6109 0.1835 0.018 Uiso 1 1 calc R . . C18 C 0.9483(16) 0.6298(5) 0.3330(14) 0.016(2) Uani 1 1 d U . . N2 N 0.8811(15) 0.6509(5) 0.6615(13) 0.023(2) Uani 1 1 d U . . H2A H 0.8278 0.6705 0.7211 0.028 Uiso 1 1 calc R . . H2B H 0.8181 0.6380 0.5979 0.028 Uiso 1 1 calc R . . C19 C 0.9415(15) 0.6078(6) 0.7342(15) 0.018(2) Uani 1 1 d U . . C20 C 1.0226(17) 0.6140(6) 0.8477(16) 0.023(3) Uani 1 1 d U . . H20 H 1.0335 0.6483 0.8823 0.027 Uiso 1 1 calc R . . C21 C 1.0898(19) 0.5744(6) 0.9156(17) 0.027(3) Uani 1 1 d U . . H21 H 1.1526 0.5814 0.9894 0.032 Uiso 1 1 calc R . . C22 C 1.0630(19) 0.5224(7) 0.8729(17) 0.029(3) Uani 1 1 d U . . C23 C 0.970(2) 0.5162(7) 0.7582(16) 0.030(3) Uani 1 1 d U . . H23 H 0.9483 0.4821 0.7274 0.036 Uiso 1 1 calc R . . C24 C 0.9119(16) 0.5584(6) 0.6909(15) 0.018(2) Uani 1 1 d U . . H24 H 0.8512 0.5531 0.6146 0.022 Uiso 1 1 calc R . . C25 C 1.1455(19) 0.4777(7) 0.935(2) 0.039(4) Uani 1 1 d U . . H25A H 1.2491 0.4824 0.9184 0.058 Uiso 1 1 calc R . . H25B H 1.1133 0.4450 0.8942 0.058 Uiso 1 1 calc R . . H25C H 1.1276 0.4768 1.0325 0.058 Uiso 1 1 calc R . . C26 C 0.3589(16) 0.3707(6) 0.0444(17) 0.023(2) Uani 1 1 d U . . C27 C 0.2901(17) 0.3375(6) -0.0562(17) 0.025(2) Uani 1 1 d U . . H27 H 0.2044 0.3191 -0.0337 0.031 Uiso 1 1 calc R . . C28 C 0.3474(17) 0.3327(7) -0.1824(16) 0.026(3) Uani 1 1 d U . . H28 H 0.2961 0.3119 -0.2457 0.031 Uiso 1 1 calc R . . C29 C 0.4677(17) 0.3545(6) -0.2234(16) 0.020(2) Uani 1 1 d U . . H29 H 0.5026 0.3487 -0.3123 0.024 Uiso 1 1 calc R . . C30 C 0.5455(18) 0.3873(6) -0.1319(16) 0.024(2) Uani 1 1 d U . . H30 H 0.6321 0.4043 -0.1582 0.028 Uiso 1 1 calc R . . C31 C 0.4881(16) 0.3932(5) -0.0012(15) 0.019(2) Uani 1 1 d U . . C32 C 0.6930(17) 0.3670(6) 0.2486(16) 0.023(2) Uani 1 1 d U . . C33 C 0.8093(17) 0.3385(7) 0.2983(17) 0.027(3) Uani 1 1 d U . . H33 H 0.7974 0.3125 0.3654 0.032 Uiso 1 1 calc R . . C34 C 0.9430(17) 0.3502(6) 0.2444(16) 0.024(2) Uani 1 1 d U . . H34 H 1.0253 0.3325 0.2787 0.028 Uiso 1 1 calc R . . C35 C 0.9619(17) 0.3851(6) 0.1469(16) 0.022(2) Uani 1 1 d U . . H35 H 1.0561 0.3928 0.1145 0.026 Uiso 1 1 calc R . . C36 C 0.8341(15) 0.4116(6) 0.0897(15) 0.021(2) Uani 1 1 d U . . H36 H 0.8418 0.4349 0.0155 0.025 Uiso 1 1 calc R . . C37 C 0.7050(14) 0.4010(5) 0.1490(14) 0.016(2) Uani 1 1 d U . . C38 C 0.4431(16) 0.5049(6) 0.1555(15) 0.021(2) Uani 1 1 d U . . C39 C 0.4202(18) 0.5566(6) 0.1496(17) 0.026(3) Uani 1 1 d U . . H39 H 0.3518 0.5722 0.2083 0.031 Uiso 1 1 calc R . . C40 C 0.5001(18) 0.5888(6) 0.0531(16) 0.024(3) Uani 1 1 d U . . H40 H 0.4828 0.6251 0.0456 0.029 Uiso 1 1 calc R . . C41 C 0.6071(18) 0.5629(7) -0.0307(18) 0.028(3) Uani 1 1 d U . . H41 H 0.6578 0.5819 -0.0979 0.034 Uiso 1 1 calc R . . C42 C 0.6354(17) 0.5095(6) -0.0122(16) 0.022(2) Uani 1 1 d U . . H42 H 0.7085 0.4930 -0.0639 0.026 Uiso 1 1 calc R . . C43 C 0.5572(16) 0.4811(6) 0.0809(14) 0.0171(19) Uani 1 1 d U . . N4 N 0.5859(15) 0.4537(6) 0.4162(14) 0.027(2) Uani 1 1 d U . . H4A H 0.6251 0.4308 0.4776 0.032 Uiso 1 1 calc R . . H4B H 0.6585 0.4626 0.3572 0.032 Uiso 1 1 calc R . . C44 C 0.5472(16) 0.4992(6) 0.4880(15) 0.021(2) Uani 1 1 d U . . C45 C 0.5841(17) 0.5481(6) 0.4533(16) 0.023(2) Uani 1 1 d U . . H45 H 0.6460 0.5525 0.3777 0.027 Uiso 1 1 calc R . . C46 C 0.5405(18) 0.5903(7) 0.5171(16) 0.026(3) Uani 1 1 d U . . H46 H 0.5684 0.6236 0.4845 0.032 Uiso 1 1 calc R . . C47 C 0.4544(17) 0.5866(6) 0.6311(15) 0.023(3) Uani 1 1 d U . . C48 C 0.407(2) 0.5356(7) 0.6721(18) 0.034(3) Uani 1 1 d U . . H48 H 0.3406 0.5314 0.7440 0.041 Uiso 1 1 calc R . . C49 C 0.4623(19) 0.4928(6) 0.6040(16) 0.026(3) Uani 1 1 d U . . H49 H 0.4420 0.4588 0.6364 0.032 Uiso 1 1 calc R . . C50 C 0.4008(19) 0.6334(7) 0.7008(18) 0.030(3) Uani 1 1 d U . . H50A H 0.4191 0.6640 0.6447 0.045 Uiso 1 1 calc R . . H50B H 0.4510 0.6372 0.7875 0.045 Uiso 1 1 calc R . . H50C H 0.2967 0.6299 0.7167 0.045 Uiso 1 1 calc R . . N5 N 0.7004(18) 0.7031(7) 0.8713(15) 0.040(3) Uani 1 1 d U . . C51 C 0.5886(18) 0.7254(6) 0.8877(17) 0.026(3) Uani 1 1 d U . . C52 C 0.462(2) 0.7516(8) 0.905(2) 0.047(5) Uani 1 1 d U . . H52A H 0.4753 0.7783 0.9745 0.070 Uiso 1 1 calc R . . H52B H 0.3868 0.7272 0.9335 0.070 Uiso 1 1 calc R . . H52C H 0.4341 0.7680 0.8198 0.070 Uiso 1 1 calc R . . N6 N 0.7822(14) 0.4009(5) 0.6160(13) 0.026(3) Uani 1 1 d U . . C53 C 0.8975(18) 0.3843(7) 0.6069(17) 0.027(3) Uani 1 1 d U . . C54 C 1.0411(18) 0.3657(8) 0.609(2) 0.039(4) Uani 1 1 d U . . H54A H 1.0704 0.3587 0.7020 0.059 Uiso 1 1 calc R . . H54B H 1.1053 0.3920 0.5695 0.059 Uiso 1 1 calc R . . H54C H 1.0471 0.3336 0.5557 0.059 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 0.0151(11) 0.0201(12) 0.0224(12) -0.0014(10) -0.0059(9) 0.0001(10) O1 0.018(4) 0.025(4) 0.024(3) -0.003(4) -0.002(3) -0.002(3) O2 0.021(3) 0.017(4) 0.029(5) 0.005(3) 0.005(3) 0.002(3) O3 0.014(4) 0.023(4) 0.030(5) -0.010(3) -0.007(3) 0.001(3) O4 0.030(5) 0.016(5) 0.026(4) -0.005(3) -0.007(4) -0.004(4) N1 0.021(4) 0.015(4) 0.024(3) 0.001(3) -0.004(3) 0.003(3) V2 0.0158(12) 0.0220(12) 0.0257(12) -0.0015(11) 0.0032(10) 0.0003(10) O5 0.017(4) 0.030(5) 0.030(4) 0.001(4) -0.007(3) -0.004(4) O6 0.014(3) 0.015(4) 0.030(5) 0.005(3) -0.008(3) -0.007(3) O7 0.020(5) 0.022(3) 0.039(6) 0.003(3) 0.007(3) 0.003(3) O8 0.020(4) 0.034(6) 0.027(4) 0.006(4) -0.001(3) -0.006(4) N3 0.013(3) 0.018(3) 0.020(3) 0.000(2) -0.005(2) 0.002(2) C1 0.013(4) 0.016(4) 0.020(3) -0.004(3) 0.002(3) 0.005(3) C2 0.011(6) 0.018(6) 0.033(5) 0.003(5) 0.002(4) 0.006(4) C3 0.025(7) 0.024(7) 0.028(5) 0.000(5) 0.015(5) -0.004(5) C4 0.028(7) 0.027(7) 0.025(5) -0.005(5) 0.008(5) -0.003(5) C5 0.012(6) 0.016(6) 0.023(4) -0.002(4) 0.000(4) 0.005(4) C6 0.022(5) 0.016(5) 0.023(3) -0.004(4) 0.001(4) 0.000(4) C7 0.017(4) 0.028(7) 0.032(6) 0.003(5) 0.003(4) 0.005(4) C8 0.017(4) 0.026(7) 0.051(8) -0.004(6) 0.008(5) 0.000(5) C9 0.015(4) 0.023(7) 0.040(7) 0.006(5) 0.008(5) 0.001(5) C10 0.021(3) 0.027(5) 0.033(4) 0.007(4) 0.001(3) -0.002(4) C11 0.020(3) 0.021(4) 0.024(4) 0.007(3) 0.005(3) -0.001(3) C12 0.021(4) 0.021(6) 0.024(5) 0.011(4) 0.001(3) 0.004(4) C13 0.023(6) 0.019(4) 0.025(6) -0.002(4) -0.012(4) 0.003(4) C14 0.046(8) 0.014(5) 0.029(7) 0.002(5) -0.014(6) 0.004(5) C15 0.020(6) 0.020(5) 0.019(6) 0.000(4) 0.000(5) 0.009(5) C16 0.021(6) 0.017(5) 0.023(6) 0.000(5) -0.001(5) 0.002(5) C17 0.012(4) 0.016(3) 0.017(4) 0.002(3) -0.002(3) 0.001(3) C18 0.020(6) 0.016(4) 0.011(5) 0.004(3) -0.002(4) 0.002(4) N2 0.031(5) 0.015(4) 0.024(5) -0.004(4) 0.004(4) -0.001(3) C19 0.008(5) 0.024(4) 0.023(5) -0.001(4) 0.006(4) -0.001(4) C20 0.021(7) 0.023(5) 0.024(6) -0.003(5) -0.001(5) -0.009(5) C21 0.029(7) 0.031(5) 0.021(6) 0.006(5) 0.006(5) -0.006(5) C22 0.034(5) 0.029(4) 0.025(4) 0.007(4) -0.006(4) 0.002(4) C23 0.041(8) 0.028(5) 0.021(7) 0.011(5) -0.005(5) 0.002(6) C24 0.017(6) 0.019(4) 0.019(6) 0.000(4) -0.006(5) 0.000(5) C25 0.019(8) 0.035(6) 0.062(11) 0.022(8) -0.011(7) -0.002(6) C26 0.017(4) 0.023(4) 0.029(3) -0.002(3) -0.005(3) -0.001(3) C27 0.019(4) 0.027(4) 0.031(4) -0.002(3) -0.003(3) -0.006(3) C28 0.023(6) 0.031(7) 0.024(5) 0.006(5) -0.014(5) -0.002(5) C29 0.023(4) 0.017(4) 0.019(4) -0.004(3) -0.004(3) 0.002(3) C30 0.026(4) 0.021(4) 0.024(3) -0.008(3) 0.000(3) -0.002(3) C31 0.018(4) 0.017(4) 0.020(3) -0.005(3) -0.004(3) 0.001(3) C32 0.019(4) 0.021(6) 0.027(6) 0.000(4) 0.002(4) 0.010(4) C33 0.019(4) 0.035(7) 0.027(7) 0.000(5) -0.001(5) 0.013(5) C34 0.020(3) 0.023(4) 0.028(4) -0.008(3) -0.003(4) 0.005(4) C35 0.016(4) 0.018(6) 0.032(7) -0.011(4) -0.006(5) 0.001(5) C36 0.015(3) 0.022(4) 0.026(4) -0.007(3) 0.001(3) 0.003(3) C37 0.014(3) 0.016(5) 0.017(5) -0.008(4) -0.002(3) 0.000(4) C38 0.021(6) 0.022(4) 0.019(6) -0.001(4) -0.005(4) 0.007(4) C39 0.028(7) 0.020(4) 0.029(7) -0.001(5) 0.004(5) 0.002(5) C40 0.025(4) 0.023(4) 0.024(4) -0.003(3) -0.004(4) -0.004(3) C41 0.020(7) 0.033(5) 0.032(7) 0.016(5) 0.002(5) 0.004(5) C42 0.020(6) 0.021(4) 0.023(6) -0.005(4) -0.004(4) -0.009(4) C43 0.019(4) 0.017(3) 0.016(4) -0.001(3) -0.006(3) 0.001(3) N4 0.023(5) 0.033(5) 0.024(5) -0.011(4) 0.002(4) -0.006(4) C44 0.018(6) 0.030(4) 0.016(5) -0.002(4) -0.003(4) -0.004(4) C45 0.019(4) 0.029(3) 0.020(4) 0.003(3) 0.004(3) -0.002(4) C46 0.026(7) 0.031(5) 0.022(6) -0.005(5) 0.003(5) -0.015(6) C47 0.025(7) 0.024(5) 0.020(6) -0.008(5) 0.000(5) -0.006(5) C48 0.050(9) 0.030(5) 0.024(7) -0.011(5) 0.018(6) -0.017(6) C49 0.039(8) 0.022(5) 0.018(6) 0.006(4) 0.005(5) -0.001(6) C50 0.025(8) 0.028(6) 0.036(8) -0.007(6) -0.005(6) 0.011(6) N5 0.052(8) 0.036(8) 0.031(7) -0.011(7) -0.006(6) 0.017(7) C51 0.030(4) 0.024(5) 0.025(5) -0.004(4) 0.001(4) -0.005(4) C52 0.028(8) 0.039(10) 0.073(14) 0.013(10) 0.011(9) -0.002(6) N6 0.021(4) 0.028(5) 0.028(4) 0.000(4) 0.005(4) -0.002(3) C53 0.026(4) 0.028(5) 0.026(5) -0.006(4) 0.002(4) 0.003(4) C54 0.017(6) 0.044(10) 0.057(12) -0.003(9) 0.007(8) -0.002(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O4 1.591(11) . ? V1 O3 1.847(10) . ? V1 O2 1.855(11) . ? V1 O1 1.909(11) . ? V1 N2 2.238(13) . ? V1 N1 2.382(13) . ? O1 C1 1.336(18) . ? O2 C7 1.35(2) . ? O3 C13 1.316(18) . ? N1 C6 1.40(2) . ? N1 C18 1.433(19) . ? N1 C12 1.468(19) . ? V2 O8 1.576(11) . ? V2 O7 1.834(11) . ? V2 O6 1.868(11) . ? V2 O5 1.896(11) . ? V2 N4 2.231(13) . ? V2 N3 2.400(13) . ? O5 C26 1.26(2) . ? O6 C32 1.394(19) . ? O7 C38 1.37(2) . ? N3 C43 1.471(18) . ? N3 C37 1.478(18) . ? N3 C31 1.509(18) . ? C1 C2 1.42(2) . ? C1 C6 1.47(2) . ? C2 C3 1.38(2) . ? C3 C4 1.39(2) . ? C4 C5 1.39(2) . ? C5 C6 1.34(2) . ? C7 C8 1.40(2) . ? C7 C12 1.41(2) . ? C8 C9 1.39(3) . ? C9 C10 1.41(2) . ? C10 C11 1.31(2) . ? C11 C12 1.43(2) . ? C13 C14 1.37(2) . ? C13 C18 1.41(2) . ? C14 C15 1.31(2) . ? C15 C16 1.44(2) . ? C16 C17 1.44(2) . ? C17 C18 1.37(2) . ? N2 C19 1.43(2) . ? C19 C20 1.36(2) . ? C19 C24 1.37(2) . ? C20 C21 1.37(2) . ? C21 C22 1.43(2) . ? C22 C23 1.43(2) . ? C22 C25 1.51(2) . ? C23 C24 1.38(2) . ? C26 C31 1.40(2) . ? C26 C27 1.46(2) . ? C27 C28 1.36(2) . ? C28 C29 1.31(2) . ? C29 C30 1.43(2) . ? C30 C31 1.41(2) . ? C32 C37 1.32(2) . ? C32 C33 1.39(2) . ? C33 C34 1.38(2) . ? C34 C35 1.33(2) . ? C35 C36 1.48(2) . ? C36 C37 1.36(2) . ? C38 C39 1.35(2) . ? C38 C43 1.43(2) . ? C39 C40 1.47(2) . ? C40 C41 1.45(2) . ? C41 C42 1.41(2) . ? C42 C43 1.38(2) . ? N4 C44 1.42(2) . ? C44 C45 1.35(2) . ? C44 C49 1.40(2) . ? C45 C46 1.32(2) . ? C46 C47 1.39(2) . ? C47 C48 1.44(2) . ? C47 C50 1.47(2) . ? C48 C49 1.39(2) . ? N5 C51 1.19(2) . ? C51 C52 1.36(3) . ? N6 C53 1.15(2) . ? C53 C54 1.41(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O4 V1 O3 103.6(5) . . ? O4 V1 O2 104.5(5) . . ? O3 V1 O2 148.0(5) . . ? O4 V1 O1 99.1(5) . . ? O3 V1 O1 95.9(5) . . ? O2 V1 O1 94.5(5) . . ? O4 V1 N2 93.8(5) . . ? O3 V1 N2 82.9(5) . . ? O2 V1 N2 80.3(5) . . ? O1 V1 N2 166.9(5) . . ? O4 V1 N1 177.8(6) . . ? O3 V1 N1 76.0(4) . . ? O2 V1 N1 76.5(5) . . ? O1 V1 N1 78.8(4) . . ? N2 V1 N1 88.3(5) . . ? C1 O1 V1 119.6(9) . . ? C7 O2 V1 121.4(10) . . ? C13 O3 V1 123.4(9) . . ? C6 N1 C18 113.0(12) . . ? C6 N1 C12 109.2(11) . . ? C18 N1 C12 121.1(13) . . ? C6 N1 V1 105.8(9) . . ? C18 N1 V1 102.4(8) . . ? C12 N1 V1 103.4(9) . . ? O8 V2 O7 102.7(6) . . ? O8 V2 O6 104.1(5) . . ? O7 V2 O6 149.9(5) . . ? O8 V2 O5 99.9(5) . . ? O7 V2 O5 96.7(5) . . ? O6 V2 O5 92.1(5) . . ? O8 V2 N4 94.4(5) . . ? O7 V2 N4 82.7(6) . . ? O6 V2 N4 81.7(5) . . ? O5 V2 N4 165.4(5) . . ? O8 V2 N3 178.7(5) . . ? O7 V2 N3 77.9(4) . . ? O6 V2 N3 75.7(4) . . ? O5 V2 N3 78.8(4) . . ? N4 V2 N3 86.9(5) . . ? C26 O5 V2 121.6(10) . . ? C32 O6 V2 118.6(9) . . ? C38 O7 V2 122.5(9) . . ? C43 N3 C37 120.7(11) . . ? C43 N3 C31 113.1(11) . . ? C37 N3 C31 113.9(11) . . ? C43 N3 V2 103.7(8) . . ? C37 N3 V2 100.7(8) . . ? C31 N3 V2 100.9(8) . . ? O1 C1 C2 117.9(13) . . ? O1 C1 C6 121.6(13) . . ? C2 C1 C6 120.4(13) . . ? C3 C2 C1 118.9(14) . . ? C2 C3 C4 121.2(15) . . ? C5 C4 C3 118.3(15) . . ? C6 C5 C4 125.6(14) . . ? C5 C6 N1 130.3(14) . . ? C5 C6 C1 115.4(13) . . ? N1 C6 C1 114.2(13) . . ? O2 C7 C8 121.1(15) . . ? O2 C7 C12 119.3(13) . . ? C8 C7 C12 119.5(15) . . ? C9 C8 C7 117.2(16) . . ? C8 C9 C10 123.1(15) . . ? C11 C10 C9 119.3(15) . . ? C10 C11 C12 120.9(15) . . ? C7 C12 C11 119.8(14) . . ? C7 C12 N1 113.2(13) . . ? C11 C12 N1 127.0(14) . . ? O3 C13 C14 125.0(14) . . ? O3 C13 C18 117.7(13) . . ? C14 C13 C18 117.3(14) . . ? C15 C14 C13 126.9(16) . . ? C14 C15 C16 118.0(14) . . ? C17 C16 C15 115.5(13) . . ? C18 C17 C16 123.3(13) . . ? C17 C18 C13 118.3(13) . . ? C17 C18 N1 126.0(13) . . ? C13 C18 N1 115.6(13) . . ? C19 N2 V1 116.9(10) . . ? C20 C19 C24 118.6(14) . . ? C20 C19 N2 122.5(14) . . ? C24 C19 N2 118.8(13) . . ? C19 C20 C21 124.5(15) . . ? C20 C21 C22 118.4(15) . . ? C21 C22 C23 116.3(15) . . ? C21 C22 C25 120.4(16) . . ? C23 C22 C25 122.7(16) . . ? C24 C23 C22 121.9(16) . . ? C19 C24 C23 119.9(14) . . ? O5 C26 C31 123.9(14) . . ? O5 C26 C27 122.6(14) . . ? C31 C26 C27 113.2(14) . . ? C28 C27 C26 120.6(15) . . ? C29 C28 C27 125.2(16) . . ? C28 C29 C30 118.8(15) . . ? C31 C30 C29 117.2(14) . . ? C26 C31 C30 125.0(14) . . ? C26 C31 N3 114.6(13) . . ? C30 C31 N3 120.4(13) . . ? C37 C32 C33 123.1(15) . . ? C37 C32 O6 119.9(13) . . ? C33 C32 O6 117.0(14) . . ? C34 C33 C32 116.2(16) . . ? C35 C34 C33 123.1(15) . . ? C34 C35 C36 118.9(14) . . ? C37 C36 C35 116.4(14) . . ? C32 C37 C36 122.0(14) . . ? C32 C37 N3 115.3(13) . . ? C36 C37 N3 122.7(13) . . ? C39 C38 O7 118.5(14) . . ? C39 C38 C43 121.1(15) . . ? O7 C38 C43 119.9(13) . . ? C38 C39 C40 120.5(15) . . ? C41 C40 C39 117.2(15) . . ? C42 C41 C40 119.9(15) . . ? C43 C42 C41 120.3(15) . . ? C42 C43 C38 120.5(14) . . ? C42 C43 N3 126.1(13) . . ? C38 C43 N3 113.1(13) . . ? C44 N4 V2 120.0(10) . . ? C45 C44 C49 117.4(15) . . ? C45 C44 N4 125.5(14) . . ? C49 C44 N4 117.1(14) . . ? C46 C45 C44 124.6(15) . . ? C45 C46 C47 120.6(16) . . ? C46 C47 C48 117.8(14) . . ? C46 C47 C50 121.3(16) . . ? C48 C47 C50 120.7(15) . . ? C49 C48 C47 118.4(15) . . ? C48 C49 C44 120.7(15) . . ? N5 C51 C52 179(2) . . ? N6 C53 C54 174.4(19) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O4 V1 O1 C1 179.1(10) . . . . ? O3 V1 O1 C1 74.2(10) . . . . ? O2 V1 O1 C1 -75.5(11) . . . . ? N2 V1 O1 C1 -10(3) . . . . ? N1 V1 O1 C1 -0.2(10) . . . . ? O4 V1 O2 C7 -159.3(11) . . . . ? O3 V1 O2 C7 -8.5(17) . . . . ? O1 V1 O2 C7 100.1(12) . . . . ? N2 V1 O2 C7 -67.8(12) . . . . ? N1 V1 O2 C7 22.8(11) . . . . ? O4 V1 O3 C13 162.2(12) . . . . ? O2 V1 O3 C13 11.3(18) . . . . ? O1 V1 O3 C13 -97.0(12) . . . . ? N2 V1 O3 C13 69.9(12) . . . . ? N1 V1 O3 C13 -20.1(12) . . . . ? O3 V1 N1 C6 -101.0(10) . . . . ? O2 V1 N1 C6 95.5(9) . . . . ? O1 V1 N1 C6 -2.0(9) . . . . ? N2 V1 N1 C6 175.9(9) . . . . ? O3 V1 N1 C18 17.6(9) . . . . ? O2 V1 N1 C18 -145.9(10) . . . . ? O1 V1 N1 C18 116.6(9) . . . . ? N2 V1 N1 C18 -65.6(9) . . . . ? O3 V1 N1 C12 144.2(10) . . . . ? O2 V1 N1 C12 -19.3(9) . . . . ? O1 V1 N1 C12 -116.7(9) . . . . ? N2 V1 N1 C12 61.1(9) . . . . ? O8 V2 O5 C26 -177.1(12) . . . . ? O7 V2 O5 C26 78.8(12) . . . . ? O6 V2 O5 C26 -72.4(12) . . . . ? N4 V2 O5 C26 -8(3) . . . . ? N3 V2 O5 C26 2.6(12) . . . . ? O8 V2 O6 C32 -154.3(11) . . . . ? O7 V2 O6 C32 -2.4(17) . . . . ? O5 V2 O6 C32 104.9(11) . . . . ? N4 V2 O6 C32 -61.9(11) . . . . ? N3 V2 O6 C32 27.0(10) . . . . ? O8 V2 O7 C38 167.7(11) . . . . ? O6 V2 O7 C38 15.7(18) . . . . ? O5 V2 O7 C38 -90.5(12) . . . . ? N4 V2 O7 C38 74.9(12) . . . . ? N3 V2 O7 C38 -13.5(11) . . . . ? O7 V2 N3 C43 14.5(8) . . . . ? O6 V2 N3 C43 -150.8(9) . . . . ? O5 V2 N3 C43 114.0(9) . . . . ? N4 V2 N3 C43 -68.7(9) . . . . ? O7 V2 N3 C37 140.1(9) . . . . ? O6 V2 N3 C37 -25.3(8) . . . . ? O5 V2 N3 C37 -120.4(8) . . . . ? N4 V2 N3 C37 56.9(8) . . . . ? O7 V2 N3 C31 -102.8(9) . . . . ? O6 V2 N3 C31 91.9(8) . . . . ? O5 V2 N3 C31 -3.3(8) . . . . ? N4 V2 N3 C31 174.1(9) . . . . ? V1 O1 C1 C2 179.3(9) . . . . ? V1 O1 C1 C6 2.5(17) . . . . ? O1 C1 C2 C3 -175.6(13) . . . . ? C6 C1 C2 C3 1(2) . . . . ? C1 C2 C3 C4 -4(2) . . . . ? C2 C3 C4 C5 2(2) . . . . ? C3 C4 C5 C6 1(2) . . . . ? C4 C5 C6 N1 -179.7(15) . . . . ? C4 C5 C6 C1 -4(2) . . . . ? C18 N1 C6 C5 68(2) . . . . ? C12 N1 C6 C5 -70(2) . . . . ? V1 N1 C6 C5 179.6(14) . . . . ? C18 N1 C6 C1 -107.8(14) . . . . ? C12 N1 C6 C1 114.3(14) . . . . ? V1 N1 C6 C1 3.5(14) . . . . ? O1 C1 C6 C5 178.9(13) . . . . ? C2 C1 C6 C5 2(2) . . . . ? O1 C1 C6 N1 -4.4(19) . . . . ? C2 C1 C6 N1 179.0(12) . . . . ? V1 O2 C7 C8 159.8(13) . . . . ? V1 O2 C7 C12 -22.5(19) . . . . ? O2 C7 C8 C9 -177.8(15) . . . . ? C12 C7 C8 C9 5(2) . . . . ? C7 C8 C9 C10 -7(3) . . . . ? C8 C9 C10 C11 6(2) . . . . ? C9 C10 C11 C12 -2(2) . . . . ? O2 C7 C12 C11 -178.7(13) . . . . ? C8 C7 C12 C11 -1(2) . . . . ? O2 C7 C12 N1 1(2) . . . . ? C8 C7 C12 N1 178.5(14) . . . . ? C10 C11 C12 C7 -1(2) . . . . ? C10 C11 C12 N1 180.0(15) . . . . ? C6 N1 C12 C7 -98.1(15) . . . . ? C18 N1 C12 C7 128.0(15) . . . . ? V1 N1 C12 C7 14.2(14) . . . . ? C6 N1 C12 C11 81.3(18) . . . . ? C18 N1 C12 C11 -53(2) . . . . ? V1 N1 C12 C11 -166.4(13) . . . . ? V1 O3 C13 C14 -162.0(14) . . . . ? V1 O3 C13 C18 18(2) . . . . ? O3 C13 C14 C15 -175.2(17) . . . . ? C18 C13 C14 C15 4(3) . . . . ? C13 C14 C15 C16 -9(3) . . . . ? C14 C15 C16 C17 9(2) . . . . ? C15 C16 C17 C18 -6(2) . . . . ? C16 C17 C18 C13 2(2) . . . . ? C16 C17 C18 N1 178.3(14) . . . . ? O3 C13 C18 C17 179.2(14) . . . . ? C14 C13 C18 C17 0(2) . . . . ? O3 C13 C18 N1 2(2) . . . . ? C14 C13 C18 N1 -177.6(15) . . . . ? C6 N1 C18 C17 -78.1(19) . . . . ? C12 N1 C18 C17 54(2) . . . . ? V1 N1 C18 C17 168.6(13) . . . . ? C6 N1 C18 C13 98.8(16) . . . . ? C12 N1 C18 C13 -128.8(15) . . . . ? V1 N1 C18 C13 -14.5(15) . . . . ? O4 V1 N2 C19 -58.4(11) . . . . ? O3 V1 N2 C19 44.9(10) . . . . ? O2 V1 N2 C19 -162.4(11) . . . . ? O1 V1 N2 C19 130(2) . . . . ? N1 V1 N2 C19 121.0(10) . . . . ? V1 N2 C19 C20 67.6(16) . . . . ? V1 N2 C19 C24 -115.0(13) . . . . ? C24 C19 C20 C21 7(2) . . . . ? N2 C19 C20 C21 -175.8(14) . . . . ? C19 C20 C21 C22 -6(2) . . . . ? C20 C21 C22 C23 2(2) . . . . ? C20 C21 C22 C25 173.9(16) . . . . ? C21 C22 C23 C24 1(3) . . . . ? C25 C22 C23 C24 -170.6(17) . . . . ? C20 C19 C24 C23 -3(2) . . . . ? N2 C19 C24 C23 179.1(14) . . . . ? C22 C23 C24 C19 0(3) . . . . ? V2 O5 C26 C31 -1(2) . . . . ? V2 O5 C26 C27 171.7(12) . . . . ? O5 C26 C27 C28 -176.5(15) . . . . ? C31 C26 C27 C28 -3(2) . . . . ? C26 C27 C28 C29 3(3) . . . . ? C27 C28 C29 C30 -2(3) . . . . ? C28 C29 C30 C31 1(2) . . . . ? O5 C26 C31 C30 176.1(16) . . . . ? C27 C26 C31 C30 3(2) . . . . ? O5 C26 C31 N3 -3(2) . . . . ? C27 C26 C31 N3 -175.9(13) . . . . ? C29 C30 C31 C26 -2(2) . . . . ? C29 C30 C31 N3 176.7(13) . . . . ? C43 N3 C31 C26 -106.4(15) . . . . ? C37 N3 C31 C26 110.8(14) . . . . ? V2 N3 C31 C26 3.7(14) . . . . ? C43 N3 C31 C30 74.8(17) . . . . ? C37 N3 C31 C30 -68.0(18) . . . . ? V2 N3 C31 C30 -175.0(12) . . . . ? V2 O6 C32 C37 -24.6(19) . . . . ? V2 O6 C32 C33 156.0(12) . . . . ? C37 C32 C33 C34 5(2) . . . . ? O6 C32 C33 C34 -176.0(14) . . . . ? C32 C33 C34 C35 -3(2) . . . . ? C33 C34 C35 C36 -2(2) . . . . ? C34 C35 C36 C37 5(2) . . . . ? C33 C32 C37 C36 -2(2) . . . . ? O6 C32 C37 C36 178.9(13) . . . . ? C33 C32 C37 N3 175.8(14) . . . . ? O6 C32 C37 N3 -4(2) . . . . ? C35 C36 C37 C32 -3(2) . . . . ? C35 C36 C37 N3 179.7(12) . . . . ? C43 N3 C37 C32 134.3(14) . . . . ? C31 N3 C37 C32 -86.0(16) . . . . ? V2 N3 C37 C32 21.1(14) . . . . ? C43 N3 C37 C36 -48.2(19) . . . . ? C31 N3 C37 C36 91.5(16) . . . . ? V2 N3 C37 C36 -161.3(12) . . . . ? V2 O7 C38 C39 -162.7(12) . . . . ? V2 O7 C38 C43 9.9(19) . . . . ? O7 C38 C39 C40 -179.7(14) . . . . ? C43 C38 C39 C40 8(2) . . . . ? C38 C39 C40 C41 -2(2) . . . . ? C39 C40 C41 C42 -3(2) . . . . ? C40 C41 C42 C43 3(2) . . . . ? C41 C42 C43 C38 3(2) . . . . ? C41 C42 C43 N3 175.3(14) . . . . ? C39 C38 C43 C42 -8(2) . . . . ? O7 C38 C43 C42 179.4(13) . . . . ? C39 C38 C43 N3 178.2(14) . . . . ? O7 C38 C43 N3 5.9(19) . . . . ? C37 N3 C43 C42 61.7(19) . . . . ? C31 N3 C43 C42 -78.3(17) . . . . ? V2 N3 C43 C42 173.2(12) . . . . ? C37 N3 C43 C38 -125.2(14) . . . . ? C31 N3 C43 C38 94.8(14) . . . . ? V2 N3 C43 C38 -13.6(13) . . . . ? O8 V2 N4 C44 -59.2(13) . . . . ? O7 V2 N4 C44 43.1(12) . . . . ? O6 V2 N4 C44 -162.8(12) . . . . ? O5 V2 N4 C44 131.7(19) . . . . ? N3 V2 N4 C44 121.2(12) . . . . ? V2 N4 C44 C45 -108.0(16) . . . . ? V2 N4 C44 C49 71.3(17) . . . . ? C49 C44 C45 C46 -3(2) . . . . ? N4 C44 C45 C46 176.0(16) . . . . ? C44 C45 C46 C47 2(3) . . . . ? C45 C46 C47 C48 -4(3) . . . . ? C45 C46 C47 C50 -178.0(16) . . . . ? C46 C47 C48 C49 6(3) . . . . ? C50 C47 C48 C49 -179.4(17) . . . . ? C47 C48 C49 C44 -8(3) . . . . ? C45 C44 C49 C48 6(2) . . . . ? N4 C44 C49 C48 -173.3(16) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N2 H2A N5 0.92 2.08 2.99(2) 170.6 . N4 H4A N6 0.92 2.14 3.01(2) 156.9 . _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 23.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 1.418 _refine_diff_density_min -1.310 _refine_diff_density_rms 0.212 #===END data_LH~3~3 _database_code_depnum_ccdc_archive 'CCDC 607721' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C52 H73 N O3' _chemical_formula_weight 760.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.452(2) _cell_length_b 14.819(3) _cell_length_c 14.999(3) _cell_angle_alpha 116.865(2) _cell_angle_beta 116.214(2) _cell_angle_gamma 91.421(3) _cell_volume 2467.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1797 _cell_measurement_theta_min 3.63 _cell_measurement_theta_max 24.50 _exptl_crystal_description block _exptl_crystal_colour yellow/green _exptl_crystal_size_max 0.06 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.023 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 0.062 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.996 _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_process_details 'SADABS v2.10, Sheldrick, G.M., (2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.8464 _diffrn_radiation_type synchrotron _diffrn_radiation_source 'Daresbury SRS station 16.2' _diffrn_radiation_monochromator 'silicon 111' _diffrn_measurement_device_type 'Bruker Apex II' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 6 _diffrn_reflns_number 12956 _diffrn_reflns_av_R_equivalents 0.0577 _diffrn_reflns_av_sigmaI/netI 0.0931 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.62 _diffrn_reflns_theta_max 27.00 _reflns_number_total 6318 _reflns_number_gt 4298 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker Apex II' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.1006P)^2^+1.7153P] 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 SHELXL _refine_ls_extinction_coef 0.026(4) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 6318 _refine_ls_number_parameters 623 _refine_ls_number_restraints 318 _refine_ls_R_factor_all 0.1094 _refine_ls_R_factor_gt 0.0776 _refine_ls_wR_factor_ref 0.2253 _refine_ls_wR_factor_gt 0.1975 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.192 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.0838(3) 0.6650(3) 0.4907(4) 0.0460(11) Uani 1 1 d . . . C2 C 0.0654(4) 0.6272(4) 0.3782(4) 0.0573(13) Uani 1 1 d . A . C3 C -0.0392(5) 0.5994(4) 0.2898(5) 0.0707(16) Uani 1 1 d . . . H3 H -0.0535 0.5736 0.2130 0.085 Uiso 1 1 calc R . . C4 C -0.1222(5) 0.6085(4) 0.3110(5) 0.0786(18) Uani 1 1 d . . . H4 H -0.1933 0.5885 0.2489 0.094 Uiso 1 1 calc R . . C5 C -0.1037(4) 0.6466(4) 0.4222(5) 0.0697(16) Uani 1 1 d . . . H5 H -0.1622 0.6532 0.4356 0.084 Uiso 1 1 calc R . . C6 C -0.0004(4) 0.6753(3) 0.5144(4) 0.0527(13) Uani 1 1 d . B . C7 C 0.1586(5) 0.6185(5) 0.3546(5) 0.0834(18) Uani 1 1 d DU . . H7 H 0.2221 0.6683 0.4331 0.100 Uiso 0.515(16) 1 calc PR A 1 H7X H 0.2208 0.6136 0.4164 0.100 Uiso 0.485(16) 1 calc PR A 2 C8 C 0.1601(17) 0.6660(12) 0.2834(14) 0.093(5) Uani 0.515(16) 1 d PDU A 1 H8A H 0.1422 0.7332 0.3101 0.140 Uiso 0.515(16) 1 calc PR A 1 H8B H 0.1071 0.6173 0.2013 0.140 Uiso 0.515(16) 1 calc PR A 1 H8C H 0.2318 0.6780 0.2932 0.140 Uiso 0.515(16) 1 calc PR A 1 C9 C 0.1887(14) 0.5199(10) 0.3219(16) 0.092(5) Uani 0.515(16) 1 d PDU A 1 H9A H 0.2504 0.5274 0.3118 0.138 Uiso 0.515(16) 1 calc PR A 1 H9B H 0.1280 0.4629 0.2490 0.138 Uiso 0.515(16) 1 calc PR A 1 H9C H 0.2079 0.5033 0.3831 0.138 Uiso 0.515(16) 1 calc PR A 1 C8X C 0.1928(19) 0.7065(15) 0.345(2) 0.143(8) Uani 0.485(16) 1 d PDU A 2 H8X1 H 0.2536 0.6983 0.3320 0.214 Uiso 0.485(16) 1 calc PR A 2 H8X2 H 0.2145 0.7732 0.4169 0.214 Uiso 0.485(16) 1 calc PR A 2 H8X3 H 0.1329 0.7067 0.2797 0.214 Uiso 0.485(16) 1 calc PR A 2 C9X C 0.1114(14) 0.5101(11) 0.2303(15) 0.111(7) Uani 0.485(16) 1 d PDU A 2 H9X1 H 0.0905 0.4505 0.2362 0.166 Uiso 0.485(16) 1 calc PR A 2 H9X2 H 0.1667 0.4999 0.2085 0.166 Uiso 0.485(16) 1 calc PR A 2 H9X3 H 0.0485 0.5144 0.1711 0.166 Uiso 0.485(16) 1 calc PR A 2 C10 C 0.0214(4) 0.7206(4) 0.6378(4) 0.0624(14) Uani 1 1 d DU . . H10 H 0.0801 0.6936 0.6757 0.075 Uiso 0.50(3) 1 calc PR B 1 H10X H 0.0986 0.7300 0.6899 0.075 Uiso 0.50(3) 1 calc PR B 2 C11 C 0.0639(14) 0.8390(6) 0.7079(12) 0.058(4) Uani 0.50(3) 1 d PDU B 1 H11A H 0.0783 0.8649 0.7869 0.087 Uiso 0.50(3) 1 calc PR B 1 H11B H 0.0104 0.8693 0.6716 0.087 Uiso 0.50(3) 1 calc PR B 1 H11C H 0.1305 0.8599 0.7109 0.087 Uiso 0.50(3) 1 calc PR B 1 C12 C -0.071(2) 0.6876(19) 0.648(3) 0.115(9) Uani 0.50(3) 1 d PDU B 1 H12A H -0.0484 0.7200 0.7300 0.172 Uiso 0.50(3) 1 calc PR B 1 H12B H -0.0920 0.6107 0.6105 0.172 Uiso 0.50(3) 1 calc PR B 1 H12C H -0.1313 0.7105 0.6098 0.172 Uiso 0.50(3) 1 calc PR B 1 C11X C -0.001(3) 0.8286(12) 0.677(2) 0.104(7) Uani 0.50(3) 1 d PDU B 2 H11D H 0.0140 0.8602 0.7564 0.155 Uiso 0.50(3) 1 calc PR B 2 H11E H -0.0758 0.8201 0.6251 0.155 Uiso 0.50(3) 1 calc PR B 2 H11F H 0.0463 0.8745 0.6733 0.155 Uiso 0.50(3) 1 calc PR B 2 C12X C -0.0469(18) 0.6519(18) 0.646(2) 0.099(7) Uani 0.50(3) 1 d PDU B 2 H12D H -0.0289 0.6836 0.7274 0.149 Uiso 0.50(3) 1 calc PR B 2 H12E H -0.0342 0.5823 0.6197 0.149 Uiso 0.50(3) 1 calc PR B 2 H12F H -0.1228 0.6447 0.5980 0.149 Uiso 0.50(3) 1 calc PR B 2 N1 N 0.1918(3) 0.6984(3) 0.5850(3) 0.0445(9) Uani 1 1 d . . . C13 C 0.2313(3) 0.6317(3) 0.6115(4) 0.0444(11) Uani 1 1 d . . . H13 H 0.1871 0.5617 0.5693 0.053 Uiso 1 1 calc R . . C14 C 0.3407(3) 0.6587(3) 0.7031(4) 0.0387(10) Uani 1 1 d . . . C15 C 0.4072(3) 0.7622(3) 0.7731(4) 0.0372(10) Uani 1 1 d . . . O1 O 0.3702(2) 0.8419(2) 0.7611(2) 0.0415(8) Uani 1 1 d . . . H1 H 0.3091 0.8167 0.7013 0.062 Uiso 1 1 calc R . . C16 C 0.5136(3) 0.7867(3) 0.8598(3) 0.0360(10) Uani 1 1 d . . . C17 C 0.5498(3) 0.7046(3) 0.8728(4) 0.0390(10) Uani 1 1 d . . . H17 H 0.6222 0.7205 0.9304 0.047 Uiso 1 1 calc R . . C18 C 0.4854(3) 0.5999(3) 0.8059(4) 0.0397(11) Uani 1 1 d . . . C19 C 0.3809(3) 0.5801(3) 0.7216(4) 0.0441(11) Uani 1 1 d . . . H19 H 0.3347 0.5103 0.6746 0.053 Uiso 1 1 calc R . . C20 C 0.5332(3) 0.5167(3) 0.8283(4) 0.0449(11) Uani 1 1 d . . . C21 C 0.6152(4) 0.4956(4) 0.7876(5) 0.0689(15) Uani 1 1 d . . . H21A H 0.5789 0.4690 0.7041 0.103 Uiso 1 1 calc R . . H21B H 0.6474 0.4431 0.8030 0.103 Uiso 1 1 calc R . . H21C H 0.6716 0.5612 0.8296 0.103 Uiso 1 1 calc R . . C22 C 0.5916(4) 0.5570(4) 0.9596(4) 0.0650(15) Uani 1 1 d . . . H22A H 0.6522 0.6190 1.0013 0.097 Uiso 1 1 calc R . . H22B H 0.6181 0.5014 0.9728 0.097 Uiso 1 1 calc R . . H22C H 0.5414 0.5760 0.9880 0.097 Uiso 1 1 calc R . . C23 C 0.4474(4) 0.4136(4) 0.7657(5) 0.0651(15) Uani 1 1 d . . . H23A H 0.3935 0.4274 0.7892 0.098 Uiso 1 1 calc R . . H23B H 0.4810 0.3639 0.7860 0.098 Uiso 1 1 calc R . . H23C H 0.4128 0.3833 0.6817 0.098 Uiso 1 1 calc R . . C24 C 0.5847(3) 0.9007(3) 0.9418(3) 0.0333(10) Uani 1 1 d . . . H24 H 0.5430 0.9421 0.9755 0.040 Uiso 1 1 calc R . . C25 C 0.6081(3) 0.9517(3) 0.8825(3) 0.0345(10) Uani 1 1 d . . . C26 C 0.6480(3) 1.0613(3) 0.9415(3) 0.0337(10) Uani 1 1 d . . . O2 O 0.6660(2) 1.1228(2) 1.0524(2) 0.0446(8) Uani 1 1 d . . . H2 H 0.6717 1.0857 1.0825 0.067 Uiso 1 1 calc R . . C27 C 0.6680(3) 1.1123(3) 0.8905(4) 0.0396(10) Uani 1 1 d . . . C28 C 0.6504(3) 1.0478(4) 0.7789(4) 0.0465(12) Uani 1 1 d . . . H28 H 0.6639 1.0805 0.7425 0.056 Uiso 1 1 calc R . . C29 C 0.6141(3) 0.9385(4) 0.7179(4) 0.0472(12) Uani 1 1 d . . . C30 C 0.5928(3) 0.8927(3) 0.7717(4) 0.0418(11) Uani 1 1 d . . . H30 H 0.5668 0.8181 0.7314 0.050 Uiso 1 1 calc R . . C31 C 0.7081(4) 1.2335(3) 0.9549(4) 0.0510(12) Uani 1 1 d . . . C32 C 0.6273(4) 1.2839(4) 0.9872(5) 0.0662(15) Uani 1 1 d . . . H32A H 0.5581 1.2604 0.9163 0.099 Uiso 1 1 calc R . . H32B H 0.6546 1.3608 1.0293 0.099 Uiso 1 1 calc R . . H32C H 0.6178 1.2626 1.0363 0.099 Uiso 1 1 calc R . . C33 C 0.8182(4) 1.2738(4) 1.0650(5) 0.0650(14) Uani 1 1 d . . . H33A H 0.8120 1.2534 1.1163 0.098 Uiso 1 1 calc R . . H33B H 0.8433 1.3507 1.1052 0.098 Uiso 1 1 calc R . . H33C H 0.8697 1.2429 1.0437 0.098 Uiso 1 1 calc R . . C34 C 0.7211(5) 1.2712(4) 0.8792(5) 0.0756(17) Uani 1 1 d . . . H34A H 0.7745 1.2431 0.8598 0.113 Uiso 1 1 calc R . . H34B H 0.7450 1.3484 0.9223 0.113 Uiso 1 1 calc R . . H34C H 0.6520 1.2462 0.8077 0.113 Uiso 1 1 calc R . . C35 C 0.5979(4) 0.8685(5) 0.5971(4) 0.0716(16) Uani 1 1 d . . . C36 C 0.6269(7) 0.9346(7) 0.5523(6) 0.135(3) Uani 1 1 d . . . H36A H 0.5848 0.9857 0.5541 0.202 Uiso 1 1 calc R . . H36B H 0.6105 0.8878 0.4725 0.202 Uiso 1 1 calc R . . H36C H 0.7037 0.9722 0.6020 0.202 Uiso 1 1 calc R . . C37 C 0.4819(5) 0.8052(5) 0.5120(5) 0.097(2) Uani 1 1 d . . . H37A H 0.4618 0.7597 0.5355 0.146 Uiso 1 1 calc R . . H37B H 0.4720 0.7617 0.4344 0.146 Uiso 1 1 calc R . . H37C H 0.4364 0.8531 0.5106 0.146 Uiso 1 1 calc R . . C38 C 0.6730(7) 0.7992(7) 0.6018(6) 0.140(4) Uani 1 1 d . . . H38A H 0.7472 0.8434 0.6590 0.210 Uiso 1 1 calc R . . H38B H 0.6658 0.7576 0.5253 0.210 Uiso 1 1 calc R . . H38C H 0.6545 0.7517 0.6241 0.210 Uiso 1 1 calc R . . C39 C 0.6860(3) 0.9099(3) 1.0440(3) 0.0326(10) Uani 1 1 d . C . C40 C 0.7763(3) 0.8910(3) 1.0360(4) 0.0409(11) Uani 1 1 d . . . H40 H 0.7786 0.8822 0.9703 0.049 Uiso 0.517(8) 1 calc PR C 1 O3X O 0.7825(5) 0.8558(5) 0.9403(5) 0.049(2) Uani 0.483(8) 1 d P C 2 H3X H 0.7383 0.8739 0.8967 0.073 Uiso 0.483(8) 1 calc PR C 2 C41 C 0.8640(3) 0.8848(3) 1.1221(4) 0.0496(12) Uani 1 1 d . C . C42 C 0.8556(4) 0.9002(4) 1.2166(5) 0.0642(15) Uani 1 1 d . . . H42 H 0.9144 0.8967 1.2765 0.077 Uiso 1 1 calc R C . C43 C 0.7687(4) 0.9203(4) 1.2300(4) 0.0576(14) Uani 1 1 d . C . C44 C 0.6843(3) 0.9253(3) 1.1421(4) 0.0414(11) Uani 1 1 d . . . H44X H 0.6232 0.9397 1.1486 0.050 Uiso 0.483(8) 1 calc PR C 2 O3 O 0.5982(5) 0.9292(4) 1.1533(5) 0.048(2) Uani 0.517(8) 1 d P C 1 H3A H 0.5867 0.9881 1.1669 0.072 Uiso 0.517(8) 1 calc PR C 1 C45 C 0.9604(4) 0.8557(4) 1.1104(5) 0.0831(18) Uani 1 1 d DU . . C46 C 1.0116(10) 0.9291(7) 1.0920(14) 0.111(4) Uani 0.700(16) 1 d PDU C 1 H46A H 1.0279 1.0019 1.1529 0.167 Uiso 0.700(16) 1 calc PR C 1 H46B H 0.9623 0.9197 1.0160 0.167 Uiso 0.700(16) 1 calc PR C 1 H46C H 1.0782 0.9140 1.0951 0.167 Uiso 0.700(16) 1 calc PR C 1 C47 C 0.931(2) 0.7393(7) 1.0238(13) 0.078(4) Uani 0.700(16) 1 d PDU C 1 H47A H 0.8975 0.6982 1.0430 0.116 Uiso 0.700(16) 1 calc PR C 1 H47B H 0.9964 0.7197 1.0268 0.116 Uiso 0.700(16) 1 calc PR C 1 H47C H 0.8810 0.7246 0.9456 0.116 Uiso 0.700(16) 1 calc PR C 1 C48 C 1.0495(8) 0.8747(11) 1.2342(7) 0.119(5) Uani 0.700(16) 1 d PDU C 1 H48A H 1.0741 0.9499 1.2927 0.179 Uiso 0.700(16) 1 calc PR C 1 H48B H 1.1106 0.8509 1.2291 0.179 Uiso 0.700(16) 1 calc PR C 1 H48C H 1.0182 0.8348 1.2563 0.179 Uiso 0.700(16) 1 calc PR C 1 C46X C 0.951(2) 0.869(3) 1.002(2) 0.110(7) Uani 0.300(16) 1 d PDU C 2 H46D H 0.9592 0.9436 1.0250 0.165 Uiso 0.300(16) 1 calc PR C 2 H46E H 0.8804 0.8265 0.9329 0.165 Uiso 0.300(16) 1 calc PR C 2 H46F H 1.0074 0.8460 0.9863 0.165 Uiso 0.300(16) 1 calc PR C 2 C47X C 0.939(5) 0.7382(12) 1.055(3) 0.065(8) Uani 0.300(16) 1 d PDU C 2 H47D H 1.0002 0.7177 1.0466 0.098 Uiso 0.300(16) 1 calc PR C 2 H47E H 0.8739 0.7036 0.9785 0.098 Uiso 0.300(16) 1 calc PR C 2 H47F H 0.9300 0.7165 1.1041 0.098 Uiso 0.300(16) 1 calc PR C 2 C48X C 1.0765(13) 0.918(2) 1.203(2) 0.116(8) Uani 0.300(16) 1 d PDU C 2 H48D H 1.0826 0.9931 1.2395 0.173 Uiso 0.300(16) 1 calc PR C 2 H48E H 1.1217 0.9019 1.1682 0.173 Uiso 0.300(16) 1 calc PR C 2 H48F H 1.1003 0.8977 1.2623 0.173 Uiso 0.300(16) 1 calc PR C 2 C49 C 0.7655(5) 0.9393(6) 1.3379(5) 0.099(2) Uani 1 1 d DU . . C50 C 0.8730(10) 0.9062(11) 1.4071(11) 0.110(4) Uani 0.533(9) 1 d PDU C 1 H50A H 0.8752 0.8392 1.3514 0.166 Uiso 0.533(9) 1 calc PR C 1 H50B H 0.8684 0.8989 1.4668 0.166 Uiso 0.533(9) 1 calc PR C 1 H50C H 0.9385 0.9612 1.4435 0.166 Uiso 0.533(9) 1 calc PR C 1 C51 C 0.7691(14) 1.0384(10) 1.4179(13) 0.107(5) Uani 0.533(9) 1 d PDU C 1 H51A H 0.7651 1.0347 1.4798 0.160 Uiso 0.533(9) 1 calc PR C 1 H51B H 0.7083 1.0606 1.3788 0.160 Uiso 0.533(9) 1 calc PR C 1 H51C H 0.8365 1.0893 1.4513 0.160 Uiso 0.533(9) 1 calc PR C 1 C52 C 0.6902(9) 0.8298(7) 1.2951(9) 0.074(3) Uani 0.533(9) 1 d PDU C 1 H52A H 0.6948 0.7720 1.2320 0.111 Uiso 0.533(9) 1 calc PR C 1 H52B H 0.6156 0.8329 1.2674 0.111 Uiso 0.533(9) 1 calc PR C 1 H52C H 0.7143 0.8177 1.3599 0.111 Uiso 0.533(9) 1 calc PR C 1 C50X C 0.7821(10) 0.8637(9) 1.3723(11) 0.072(3) Uani 0.467(9) 1 d PDU C 2 H50D H 0.7356 0.7938 1.3055 0.108 Uiso 0.467(9) 1 calc PR C 2 H50E H 0.7649 0.8820 1.4335 0.108 Uiso 0.467(9) 1 calc PR C 2 H50F H 0.8574 0.8629 1.4016 0.108 Uiso 0.467(9) 1 calc PR C 2 C51X C 0.8376(12) 1.0527(8) 1.4370(11) 0.087(4) Uani 0.467(9) 1 d PDU C 2 H51D H 0.8253 1.1001 1.4064 0.131 Uiso 0.467(9) 1 calc PR C 2 H51E H 0.9133 1.0529 1.4686 0.131 Uiso 0.467(9) 1 calc PR C 2 H51F H 0.8199 1.0767 1.4985 0.131 Uiso 0.467(9) 1 calc PR C 2 C52X C 0.6517(10) 0.9675(11) 1.3296(11) 0.087(4) Uani 0.467(9) 1 d PDU C 2 H52D H 0.5912 0.9037 1.2706 0.131 Uiso 0.467(9) 1 calc PR C 2 H52E H 0.6402 1.0215 1.3083 0.131 Uiso 0.467(9) 1 calc PR C 2 H52F H 0.6570 0.9938 1.4050 0.131 Uiso 0.467(9) 1 calc PR C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.039(3) 0.041(3) 0.048(3) 0.021(2) 0.016(2) 0.013(2) C2 0.058(3) 0.055(3) 0.055(3) 0.030(3) 0.024(3) 0.022(3) C3 0.070(4) 0.069(4) 0.051(3) 0.027(3) 0.018(3) 0.027(3) C4 0.052(4) 0.070(4) 0.065(4) 0.020(3) 0.009(3) 0.015(3) C5 0.040(3) 0.062(3) 0.072(4) 0.017(3) 0.020(3) 0.007(3) C6 0.041(3) 0.039(3) 0.058(3) 0.014(2) 0.022(3) 0.006(2) C7 0.080(4) 0.132(5) 0.067(4) 0.063(4) 0.045(3) 0.055(4) C8 0.125(14) 0.076(10) 0.090(11) 0.051(9) 0.056(10) 0.014(9) C9 0.096(11) 0.118(9) 0.136(13) 0.095(10) 0.083(10) 0.059(8) C8X 0.111(15) 0.089(10) 0.19(2) 0.023(12) 0.107(16) -0.018(10) C9X 0.108(12) 0.090(8) 0.134(13) 0.026(8) 0.095(11) 0.022(8) C10 0.044(3) 0.056(3) 0.060(3) 0.010(3) 0.026(2) 0.005(2) C11 0.050(8) 0.042(5) 0.054(7) 0.013(5) 0.019(7) 0.003(5) C12 0.105(13) 0.080(13) 0.116(14) 0.003(11) 0.075(12) -0.030(10) C11X 0.145(18) 0.048(7) 0.099(13) 0.006(8) 0.083(14) -0.001(9) C12X 0.114(14) 0.083(12) 0.056(10) 0.032(10) 0.016(9) -0.023(10) N1 0.040(2) 0.045(2) 0.048(2) 0.0246(19) 0.0209(19) 0.0151(18) C13 0.043(3) 0.039(3) 0.049(3) 0.021(2) 0.022(2) 0.011(2) C14 0.036(2) 0.038(2) 0.044(3) 0.021(2) 0.021(2) 0.014(2) C15 0.039(3) 0.036(2) 0.046(3) 0.025(2) 0.024(2) 0.016(2) O1 0.0373(17) 0.0374(17) 0.0513(19) 0.0256(15) 0.0207(14) 0.0138(13) C16 0.036(2) 0.033(2) 0.044(2) 0.021(2) 0.023(2) 0.0132(19) C17 0.035(2) 0.036(3) 0.047(3) 0.021(2) 0.022(2) 0.012(2) C18 0.041(3) 0.033(2) 0.045(3) 0.018(2) 0.023(2) 0.010(2) C19 0.042(3) 0.032(2) 0.050(3) 0.016(2) 0.022(2) 0.009(2) C20 0.044(3) 0.031(2) 0.060(3) 0.024(2) 0.027(2) 0.016(2) C21 0.075(4) 0.057(3) 0.102(4) 0.048(3) 0.058(3) 0.037(3) C22 0.080(4) 0.048(3) 0.067(3) 0.038(3) 0.029(3) 0.026(3) C23 0.060(3) 0.039(3) 0.086(4) 0.037(3) 0.025(3) 0.015(2) C24 0.036(2) 0.030(2) 0.042(2) 0.022(2) 0.024(2) 0.0140(18) C25 0.033(2) 0.034(2) 0.039(2) 0.018(2) 0.021(2) 0.0130(19) C26 0.040(2) 0.034(2) 0.033(2) 0.018(2) 0.022(2) 0.0167(19) O2 0.067(2) 0.0312(16) 0.0446(18) 0.0189(14) 0.0358(16) 0.0171(15) C27 0.044(3) 0.041(3) 0.046(3) 0.027(2) 0.026(2) 0.017(2) C28 0.043(3) 0.064(3) 0.051(3) 0.039(3) 0.028(2) 0.018(2) C29 0.040(3) 0.059(3) 0.038(3) 0.019(2) 0.022(2) 0.010(2) C30 0.040(3) 0.037(2) 0.039(3) 0.010(2) 0.022(2) 0.010(2) C31 0.059(3) 0.043(3) 0.071(3) 0.037(3) 0.040(3) 0.019(2) C32 0.086(4) 0.047(3) 0.100(4) 0.047(3) 0.063(4) 0.035(3) C33 0.066(4) 0.044(3) 0.076(4) 0.026(3) 0.035(3) 0.005(3) C34 0.105(5) 0.063(3) 0.108(5) 0.062(4) 0.072(4) 0.036(3) C35 0.063(4) 0.093(4) 0.041(3) 0.017(3) 0.031(3) 0.007(3) C36 0.137(7) 0.185(8) 0.060(4) 0.038(5) 0.061(4) -0.014(6) C37 0.086(5) 0.109(5) 0.047(3) 0.008(3) 0.031(3) 0.001(4) C38 0.140(7) 0.183(8) 0.068(4) 0.027(5) 0.067(5) 0.101(6) C39 0.034(2) 0.027(2) 0.039(2) 0.0169(19) 0.020(2) 0.0087(18) C40 0.041(3) 0.036(2) 0.043(3) 0.017(2) 0.023(2) 0.010(2) O3X 0.049(4) 0.060(4) 0.040(4) 0.024(3) 0.027(3) 0.024(3) C41 0.032(3) 0.039(3) 0.065(3) 0.026(2) 0.016(2) 0.009(2) C42 0.043(3) 0.066(3) 0.071(4) 0.051(3) 0.004(3) 0.000(3) C43 0.055(3) 0.059(3) 0.044(3) 0.029(3) 0.013(3) -0.011(3) C44 0.042(3) 0.036(2) 0.044(3) 0.016(2) 0.025(2) 0.004(2) O3 0.050(4) 0.045(4) 0.058(4) 0.022(3) 0.039(3) 0.014(3) C45 0.044(3) 0.062(3) 0.119(5) 0.034(3) 0.037(3) 0.024(3) C46 0.064(7) 0.069(6) 0.182(12) 0.025(7) 0.091(8) 0.005(5) C47 0.075(9) 0.072(5) 0.086(9) 0.027(5) 0.055(9) 0.027(5) C48 0.036(5) 0.131(10) 0.109(7) 0.018(6) 0.019(5) 0.042(6) C46X 0.056(13) 0.127(19) 0.205(16) 0.108(16) 0.085(13) 0.052(12) C47X 0.067(14) 0.062(8) 0.051(14) 0.011(8) 0.036(14) 0.016(10) C48X 0.045(10) 0.093(13) 0.176(16) 0.051(13) 0.052(10) -0.013(9) C49 0.078(4) 0.151(5) 0.062(4) 0.068(4) 0.022(3) -0.015(4) C50 0.128(9) 0.128(11) 0.084(8) 0.080(8) 0.035(7) 0.012(8) C51 0.127(13) 0.135(8) 0.080(9) 0.057(7) 0.067(10) 0.030(9) C52 0.104(8) 0.088(7) 0.071(7) 0.056(6) 0.059(7) 0.031(6) C50X 0.042(7) 0.095(8) 0.079(8) 0.049(7) 0.027(7) 0.011(6) C51X 0.147(11) 0.103(7) 0.063(8) 0.055(6) 0.076(9) 0.075(7) C52X 0.136(9) 0.113(10) 0.073(8) 0.064(8) 0.079(8) 0.070(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C2 1.405(6) . ? C1 C6 1.405(6) . ? C1 N1 1.435(5) . ? C2 C3 1.386(7) . ? C2 C7 1.531(7) . ? C3 C4 1.365(8) . ? C4 C5 1.385(8) . ? C5 C6 1.391(7) . ? C6 C10 1.525(7) . ? C7 C9 1.462(8) . ? C7 C8X 1.472(14) . ? C7 C8 1.528(9) . ? C7 C9X 1.624(12) . ? C10 C12X 1.486(10) . ? C10 C12 1.496(10) . ? C10 C11 1.507(9) . ? C10 C11X 1.532(10) . ? N1 C13 1.282(5) . ? C13 C14 1.449(6) . ? C14 C19 1.399(6) . ? C14 C15 1.400(6) . ? C15 O1 1.361(5) . ? C15 C16 1.401(6) . ? C16 C17 1.395(5) . ? C16 C24 1.531(5) . ? C17 C18 1.406(6) . ? C18 C19 1.386(6) . ? C18 C20 1.525(6) . ? C20 C23 1.527(6) . ? C20 C21 1.537(6) . ? C20 C22 1.546(7) . ? C24 C39 1.526(5) . ? C24 C25 1.529(5) . ? C25 C30 1.389(5) . ? C25 C26 1.399(5) . ? C26 O2 1.378(4) . ? C26 C27 1.396(6) . ? C27 C28 1.395(6) . ? C27 C31 1.542(6) . ? C28 C29 1.390(6) . ? C29 C30 1.381(6) . ? C29 C35 1.527(6) . ? C31 C33 1.535(7) . ? C31 C32 1.540(6) . ? C31 C34 1.547(7) . ? C35 C37 1.507(8) . ? C35 C38 1.513(9) . ? C35 C36 1.553(9) . ? C39 C40 1.387(6) . ? C39 C44 1.395(6) . ? C40 O3X 1.333(7) . ? C40 C41 1.397(6) . ? C41 C42 1.391(7) . ? C41 C45 1.528(7) . ? C42 C43 1.377(7) . ? C43 C44 1.380(6) . ? C43 C49 1.535(7) . ? C44 O3 1.327(6) . ? C45 C46 1.489(9) . ? C45 C47X 1.503(17) . ? C45 C47 1.515(9) . ? C45 C48X 1.517(14) . ? C45 C48 1.608(9) . ? C45 C46X 1.667(15) . ? C49 C51 1.395(10) . ? C49 C50X 1.416(9) . ? C49 C51X 1.551(11) . ? C49 C52 1.607(9) . ? C49 C52X 1.671(10) . ? C49 C50 1.675(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 C1 C6 121.7(4) . . ? C2 C1 N1 119.4(4) . . ? C6 C1 N1 118.9(4) . . ? C3 C2 C1 118.0(5) . . ? C3 C2 C7 121.1(5) . . ? C1 C2 C7 120.9(4) . . ? C4 C3 C2 121.2(5) . . ? C3 C4 C5 120.7(5) . . ? C4 C5 C6 120.8(5) . . ? C5 C6 C1 117.7(5) . . ? C5 C6 C10 121.2(4) . . ? C1 C6 C10 121.1(4) . . ? C9 C7 C8 112.1(9) . . ? C9 C7 C2 119.3(7) . . ? C8X C7 C2 112.7(10) . . ? C8 C7 C2 114.8(9) . . ? C8X C7 C9X 108.6(11) . . ? C2 C7 C9X 104.8(7) . . ? C12 C10 C11 109.7(9) . . ? C12X C10 C6 112.6(10) . . ? C12 C10 C6 115.7(12) . . ? C11 C10 C6 111.9(7) . . ? C12X C10 C11X 109.6(10) . . ? C6 C10 C11X 107.6(9) . . ? C13 N1 C1 119.5(4) . . ? N1 C13 C14 122.7(4) . . ? C19 C14 C15 119.3(4) . . ? C19 C14 C13 119.6(4) . . ? C15 C14 C13 121.1(4) . . ? O1 C15 C14 121.3(4) . . ? O1 C15 C16 118.3(3) . . ? C14 C15 C16 120.5(4) . . ? C17 C16 C15 117.7(4) . . ? C17 C16 C24 121.4(4) . . ? C15 C16 C24 120.8(3) . . ? C16 C17 C18 123.9(4) . . ? C19 C18 C17 116.1(4) . . ? C19 C18 C20 124.5(4) . . ? C17 C18 C20 119.4(4) . . ? C18 C19 C14 122.6(4) . . ? C18 C20 C23 112.2(4) . . ? C18 C20 C21 108.8(4) . . ? C23 C20 C21 109.4(4) . . ? C18 C20 C22 110.0(3) . . ? C23 C20 C22 107.7(4) . . ? C21 C20 C22 108.7(4) . . ? C39 C24 C25 113.1(3) . . ? C39 C24 C16 110.5(3) . . ? C25 C24 C16 114.6(3) . . ? C30 C25 C26 118.2(4) . . ? C30 C25 C24 122.2(4) . . ? C26 C25 C24 119.5(3) . . ? O2 C26 C27 117.8(3) . . ? O2 C26 C25 120.2(3) . . ? C27 C26 C25 122.0(4) . . ? C28 C27 C26 116.4(4) . . ? C28 C27 C31 122.1(4) . . ? C26 C27 C31 121.5(4) . . ? C29 C28 C27 123.8(4) . . ? C30 C29 C28 117.1(4) . . ? C30 C29 C35 119.5(4) . . ? C28 C29 C35 123.4(4) . . ? C29 C30 C25 122.4(4) . . ? C33 C31 C32 109.9(4) . . ? C33 C31 C27 109.9(4) . . ? C32 C31 C27 110.4(4) . . ? C33 C31 C34 107.5(4) . . ? C32 C31 C34 107.1(4) . . ? C27 C31 C34 111.9(4) . . ? C37 C35 C38 112.2(6) . . ? C37 C35 C29 110.1(4) . . ? C38 C35 C29 109.6(5) . . ? C37 C35 C36 107.3(5) . . ? C38 C35 C36 106.0(6) . . ? C29 C35 C36 111.7(5) . . ? C40 C39 C44 118.7(4) . . ? C40 C39 C24 121.0(4) . . ? C44 C39 C24 119.8(3) . . ? O3X C40 C39 125.5(5) . . ? O3X C40 C41 111.3(4) . . ? C39 C40 C41 121.7(4) . . ? C42 C41 C40 115.9(4) . . ? C42 C41 C45 121.6(5) . . ? C40 C41 C45 122.4(5) . . ? C43 C42 C41 125.0(4) . . ? C42 C43 C44 116.5(4) . . ? C42 C43 C49 122.5(5) . . ? C44 C43 C49 121.0(5) . . ? O3 C44 C43 112.4(5) . . ? O3 C44 C39 124.7(5) . . ? C43 C44 C39 122.1(4) . . ? C46 C45 C47 116.1(10) . . ? C47X C45 C48X 114(2) . . ? C46 C45 C41 111.6(5) . . ? C47X C45 C41 108(3) . . ? C47 C45 C41 110.6(11) . . ? C48X C45 C41 124.1(12) . . ? C46 C45 C48 105.1(7) . . ? C47 C45 C48 106.3(9) . . ? C41 C45 C48 106.3(6) . . ? C47X C45 C46X 100.1(16) . . ? C48X C45 C46X 100.9(12) . . ? C41 C45 C46X 105.5(8) . . ? C51 C49 C43 121.4(8) . . ? C50X C49 C43 120.3(8) . . ? C50X C49 C51X 113.6(9) . . ? C43 C49 C51X 106.9(7) . . ? C51 C49 C52 124.5(9) . . ? C43 C49 C52 103.9(5) . . ? C50X C49 C52X 108.4(7) . . ? C43 C49 C52X 110.2(6) . . ? C51X C49 C52X 94.2(8) . . ? C51 C49 C50 107.9(9) . . ? C43 C49 C50 103.3(6) . . ? C52 C49 C50 89.0(7) . . ? 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 C6 C1 C2 C3 -0.3(7) . . . . ? N1 C1 C2 C3 -177.5(4) . . . . ? C6 C1 C2 C7 178.8(5) . . . . ? N1 C1 C2 C7 1.6(7) . . . . ? C1 C2 C3 C4 0.0(8) . . . . ? C7 C2 C3 C4 -179.1(5) . . . . ? C2 C3 C4 C5 0.4(9) . . . . ? C3 C4 C5 C6 -0.7(9) . . . . ? C4 C5 C6 C1 0.5(8) . . . . ? C4 C5 C6 C10 178.1(5) . . . . ? C2 C1 C6 C5 0.0(7) . . . . ? N1 C1 C6 C5 177.3(4) . . . . ? C2 C1 C6 C10 -177.6(4) . . . . ? N1 C1 C6 C10 -0.3(6) . . . . ? C3 C2 C7 C9 -89.4(10) . . . . ? C1 C2 C7 C9 91.5(10) . . . . ? C3 C2 C7 C8X 78.7(13) . . . . ? C1 C2 C7 C8X -100.4(13) . . . . ? C3 C2 C7 C8 47.9(10) . . . . ? C1 C2 C7 C8 -131.2(9) . . . . ? C3 C2 C7 C9X -39.3(11) . . . . ? C1 C2 C7 C9X 141.6(10) . . . . ? C5 C6 C10 C12X 53.9(14) . . . . ? C1 C6 C10 C12X -128.6(13) . . . . ? C5 C6 C10 C12 27.1(16) . . . . ? C1 C6 C10 C12 -155.3(15) . . . . ? C5 C6 C10 C11 -99.5(9) . . . . ? C1 C6 C10 C11 78.1(9) . . . . ? C5 C6 C10 C11X -67.0(14) . . . . ? C1 C6 C10 C11X 110.5(14) . . . . ? C2 C1 N1 C13 -90.4(5) . . . . ? C6 C1 N1 C13 92.3(5) . . . . ? C1 N1 C13 C14 178.0(4) . . . . ? N1 C13 C14 C19 -175.4(4) . . . . ? N1 C13 C14 C15 4.3(6) . . . . ? C19 C14 C15 O1 -177.4(4) . . . . ? C13 C14 C15 O1 2.9(6) . . . . ? C19 C14 C15 C16 1.0(6) . . . . ? C13 C14 C15 C16 -178.6(4) . . . . ? O1 C15 C16 C17 178.6(3) . . . . ? C14 C15 C16 C17 0.1(6) . . . . ? O1 C15 C16 C24 2.4(6) . . . . ? C14 C15 C16 C24 -176.1(4) . . . . ? C15 C16 C17 C18 -1.2(6) . . . . ? C24 C16 C17 C18 175.0(4) . . . . ? C16 C17 C18 C19 1.1(6) . . . . ? C16 C17 C18 C20 -179.5(4) . . . . ? C17 C18 C19 C14 0.1(6) . . . . ? C20 C18 C19 C14 -179.3(4) . . . . ? C15 C14 C19 C18 -1.2(6) . . . . ? C13 C14 C19 C18 178.5(4) . . . . ? C19 C18 C20 C23 -12.0(6) . . . . ? C17 C18 C20 C23 168.6(4) . . . . ? C19 C18 C20 C21 109.2(5) . . . . ? C17 C18 C20 C21 -70.2(5) . . . . ? C19 C18 C20 C22 -131.9(5) . . . . ? C17 C18 C20 C22 48.8(5) . . . . ? C17 C16 C24 C39 -9.1(5) . . . . ? C15 C16 C24 C39 167.0(3) . . . . ? C17 C16 C24 C25 120.2(4) . . . . ? C15 C16 C24 C25 -63.8(5) . . . . ? C39 C24 C25 C30 110.6(4) . . . . ? C16 C24 C25 C30 -17.3(5) . . . . ? C39 C24 C25 C26 -68.3(5) . . . . ? C16 C24 C25 C26 163.8(3) . . . . ? C30 C25 C26 O2 -178.9(3) . . . . ? C24 C25 C26 O2 0.0(5) . . . . ? C30 C25 C26 C27 2.9(6) . . . . ? C24 C25 C26 C27 -178.2(4) . . . . ? O2 C26 C27 C28 179.1(3) . . . . ? C25 C26 C27 C28 -2.6(6) . . . . ? O2 C26 C27 C31 -0.5(6) . . . . ? C25 C26 C27 C31 177.8(4) . . . . ? C26 C27 C28 C29 0.5(6) . . . . ? C31 C27 C28 C29 -179.9(4) . . . . ? C27 C28 C29 C30 1.3(6) . . . . ? C27 C28 C29 C35 -178.3(4) . . . . ? C28 C29 C30 C25 -1.0(6) . . . . ? C35 C29 C30 C25 178.6(4) . . . . ? C26 C25 C30 C29 -1.0(6) . . . . ? C24 C25 C30 C29 -179.9(4) . . . . ? C28 C27 C31 C33 -117.3(5) . . . . ? C26 C27 C31 C33 62.3(5) . . . . ? C28 C27 C31 C32 121.3(5) . . . . ? C26 C27 C31 C32 -59.1(6) . . . . ? C28 C27 C31 C34 2.1(6) . . . . ? C26 C27 C31 C34 -178.3(4) . . . . ? C30 C29 C35 C37 61.4(7) . . . . ? C28 C29 C35 C37 -119.0(6) . . . . ? C30 C29 C35 C38 -62.4(7) . . . . ? C28 C29 C35 C38 117.2(6) . . . . ? C30 C29 C35 C36 -179.6(5) . . . . ? C28 C29 C35 C36 0.0(7) . . . . ? C25 C24 C39 C40 -44.0(5) . . . . ? C16 C24 C39 C40 86.1(4) . . . . ? C25 C24 C39 C44 143.6(4) . . . . ? C16 C24 C39 C44 -86.4(4) . . . . ? C44 C39 C40 O3X 166.8(5) . . . . ? C24 C39 C40 O3X -5.8(7) . . . . ? C44 C39 C40 C41 1.5(6) . . . . ? C24 C39 C40 C41 -171.0(4) . . . . ? O3X C40 C41 C42 -168.1(5) . . . . ? C39 C40 C41 C42 -1.0(6) . . . . ? O3X C40 C41 C45 8.0(6) . . . . ? C39 C40 C41 C45 175.1(4) . . . . ? C40 C41 C42 C43 0.3(7) . . . . ? C45 C41 C42 C43 -175.9(5) . . . . ? C41 C42 C43 C44 -0.1(7) . . . . ? C41 C42 C43 C49 -178.5(5) . . . . ? C42 C43 C44 O3 170.6(5) . . . . ? C49 C43 C44 O3 -10.9(7) . . . . ? C42 C43 C44 C39 0.6(7) . . . . ? C49 C43 C44 C39 179.1(4) . . . . ? C40 C39 C44 O3 -170.1(5) . . . . ? C24 C39 C44 O3 2.5(6) . . . . ? C40 C39 C44 C43 -1.3(6) . . . . ? C24 C39 C44 C43 171.3(4) . . . . ? C42 C41 C45 C46 -126.6(8) . . . . ? C40 C41 C45 C46 57.5(8) . . . . ? C42 C41 C45 C47X 85.0(16) . . . . ? C40 C41 C45 C47X -90.9(16) . . . . ? C42 C41 C45 C47 102.5(9) . . . . ? C40 C41 C45 C47 -73.4(9) . . . . ? C42 C41 C45 C48X -53.4(16) . . . . ? C40 C41 C45 C48X 130.7(16) . . . . ? C42 C41 C45 C48 -12.5(8) . . . . ? C40 C41 C45 C48 171.5(7) . . . . ? C42 C41 C45 C46X -168.6(13) . . . . ? C40 C41 C45 C46X 15.5(14) . . . . ? C42 C43 C49 C51 110.6(11) . . . . ? C44 C43 C49 C51 -67.8(11) . . . . ? C42 C43 C49 C50X -55.6(9) . . . . ? C44 C43 C49 C50X 126.0(8) . . . . ? C42 C43 C49 C51X 75.9(9) . . . . ? C44 C43 C49 C51X -102.5(8) . . . . ? C42 C43 C49 C52 -102.8(7) . . . . ? C44 C43 C49 C52 78.9(7) . . . . ? C42 C43 C49 C52X 177.0(7) . . . . ? C44 C43 C49 C52X -1.3(9) . . . . ? C42 C43 C49 C50 -10.4(8) . . . . ? C44 C43 C49 C50 171.2(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 N1 0.84 1.86 2.604(4) 146.5 . O3 H3A O1 0.84 2.18 2.971(6) 156.0 2_677 _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.491 _refine_diff_density_min -0.441 _refine_diff_density_rms 0.047 #===END