# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email NOCERA@MIT.EDU _publ_contact_author_name D.Nocera loop_ _publ_author_name 'Stanislav Groysman' 'Dino Villagran' 'Danna Freedman' D.Nocera data_10158final _database_code_depnum_ccdc_archive 'CCDC 832149' #TrackingRef '- CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common (RO)3VNNV(OR)3 _chemical_melting_point 'not measured' _chemical_formula_moiety 'C30 H63 N O3 V' _chemical_formula_sum 'C30 H63 N O3 V' _chemical_formula_weight 536.75 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 triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1590(8) _cell_length_b 15.1818(9) _cell_length_c 17.6527(11) _cell_angle_alpha 82.4180(10) _cell_angle_beta 82.0610(10) _cell_angle_gamma 79.7960(10) _cell_volume 3157.0(3) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour 'dark brown' _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.129 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1188 _exptl_absorpt_coefficient_mu 0.342 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9193 _exptl_absorpt_correction_T_max 0.9504 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 66384 _diffrn_reflns_av_R_equivalents 0.0641 _diffrn_reflns_av_sigmaI/netI 0.0610 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 28.29 _reflns_number_total 15604 _reflns_number_gt 11183 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0612P)^2^+1.7637P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15604 _refine_ls_number_parameters 864 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0823 _refine_ls_R_factor_gt 0.0521 _refine_ls_wR_factor_ref 0.1384 _refine_ls_wR_factor_gt 0.1206 _refine_ls_goodness_of_fit_ref 1.025 _refine_ls_restrained_S_all 1.025 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.42383(3) 0.36347(2) 0.031813(19) 0.01439(9) Uani 1 1 d . . . O1 O 0.52305(12) 0.27495(9) 0.07207(8) 0.0187(3) Uani 1 1 d . . . O2 O 0.30234(12) 0.38198(9) 0.10070(8) 0.0180(3) Uani 1 1 d . B . O3 O 0.38127(13) 0.32494(9) -0.04894(8) 0.0188(3) Uani 1 1 d . . . N1 N 0.48106(14) 0.46440(11) 0.00783(9) 0.0151(3) Uani 1 1 d . . . C21 C 0.40590(19) 0.29693(14) -0.12508(12) 0.0202(4) Uani 1 1 d . . . C22 C 0.33693(19) 0.36919(14) -0.18164(12) 0.0206(4) Uani 1 1 d . . . C1 C 0.1963(2) 0.43772(14) 0.12221(12) 0.0227(5) Uani 1 1 d D . . C13 C 0.5440(2) 0.17304(16) 0.18710(13) 0.0284(5) Uani 1 1 d . . . C23 C 0.3394(2) 0.46352(16) -0.16031(15) 0.0346(6) Uani 1 1 d . . . H23A H 0.3064 0.5090 -0.1991 0.052 Uiso 1 1 calc R . . H23B H 0.4175 0.4707 -0.1583 0.052 Uiso 1 1 calc R . . H23C H 0.2960 0.4711 -0.1099 0.052 Uiso 1 1 calc R . . C24 C 0.2123(2) 0.36147(17) -0.17797(14) 0.0287(5) Uani 1 1 d . . . H24A H 0.1772 0.3614 -0.1245 0.043 Uiso 1 1 calc R . . H24B H 0.2056 0.3053 -0.1974 0.043 Uiso 1 1 calc R . . H24C H 0.1743 0.4128 -0.2096 0.043 Uiso 1 1 calc R . . C11 C 0.6033(2) 0.24132(14) 0.12601(13) 0.0243(5) Uani 1 1 d . . . C25 C 0.3888(2) 0.36791(18) -0.26646(13) 0.0306(5) Uani 1 1 d . . . H25A H 0.3401 0.4101 -0.2994 0.046 Uiso 1 1 calc R . . H25B H 0.3959 0.3070 -0.2813 0.046 Uiso 1 1 calc R . . H25C H 0.4634 0.3858 -0.2725 0.046 Uiso 1 1 calc R . . C3 C 0.2080(2) 0.48096(17) 0.19668(14) 0.0332(6) Uani 1 1 d . B . C26 C 0.5316(2) 0.2966(2) -0.14903(14) 0.0409(7) Uani 1 1 d . . . H26A H 0.5465 0.3587 -0.1582 0.061 Uiso 1 1 calc R . . H26B H 0.5549 0.2674 -0.1963 0.061 Uiso 1 1 calc R . . H26C H 0.5741 0.2635 -0.1079 0.061 Uiso 1 1 calc R . . C27 C 0.3808(3) 0.19620(16) -0.11541(14) 0.0349(6) Uani 1 1 d . . . C12 C 0.6207(4) 0.32180(18) 0.1632(2) 0.0705(13) Uani 1 1 d . . . H12A H 0.6660 0.3591 0.1264 0.106 Uiso 1 1 calc R . . H12B H 0.6598 0.3007 0.2088 0.106 Uiso 1 1 calc R . . H12C H 0.5475 0.3576 0.1784 0.106 Uiso 1 1 calc R . . C28 C 0.2683(3) 0.18409(19) -0.06841(16) 0.0516(9) Uani 1 1 d . . . H28A H 0.2069 0.2208 -0.0945 0.077 Uiso 1 1 calc R . . H28B H 0.2662 0.2031 -0.0172 0.077 Uiso 1 1 calc R . . H28C H 0.2596 0.1206 -0.0633 0.077 Uiso 1 1 calc R . . C14 C 0.4877(2) 0.11054(19) 0.14963(17) 0.0445(7) Uani 1 1 d . . . H14A H 0.5437 0.0773 0.1139 0.067 Uiso 1 1 calc R . . H14B H 0.4278 0.1462 0.1215 0.067 Uiso 1 1 calc R . . H14C H 0.4555 0.0679 0.1895 0.067 Uiso 1 1 calc R . . C16 C 0.6226(2) 0.11558(18) 0.24245(14) 0.0385(6) Uani 1 1 d . . . H16A H 0.5782 0.0828 0.2837 0.058 Uiso 1 1 calc R . . H16B H 0.6624 0.1548 0.2647 0.058 Uiso 1 1 calc R . . H16C H 0.6774 0.0725 0.2142 0.058 Uiso 1 1 calc R . . C29 C 0.4700(3) 0.13425(19) -0.06961(18) 0.0618(11) Uani 1 1 d . . . H29A H 0.4757 0.1605 -0.0227 0.093 Uiso 1 1 calc R . . H29B H 0.5431 0.1283 -0.1014 0.093 Uiso 1 1 calc R . . H29C H 0.4477 0.0747 -0.0557 0.093 Uiso 1 1 calc R . . C17 C 0.7186(2) 0.20198(19) 0.07881(16) 0.0390(7) Uani 1 1 d . . . C15 C 0.4481(3) 0.2271(3) 0.23695(16) 0.0728(13) Uani 1 1 d . . . H15A H 0.3991 0.2683 0.2035 0.109 Uiso 1 1 calc R . . H15B H 0.4800 0.2618 0.2690 0.109 Uiso 1 1 calc R . . H15C H 0.4041 0.1856 0.2700 0.109 Uiso 1 1 calc R . . C30 C 0.3889(3) 0.15895(18) -0.19335(16) 0.0507(9) Uani 1 1 d . . . H30A H 0.3815 0.0951 -0.1846 0.076 Uiso 1 1 calc R . . H30B H 0.4619 0.1657 -0.2228 0.076 Uiso 1 1 calc R . . H30C H 0.3284 0.1923 -0.2222 0.076 Uiso 1 1 calc R . . C19 C 0.7201(3) 0.1124(2) 0.04841(16) 0.0521(9) Uani 1 1 d . . . H19A H 0.6577 0.1178 0.0175 0.078 Uiso 1 1 calc R . . H19B H 0.7119 0.0656 0.0917 0.078 Uiso 1 1 calc R . . H19C H 0.7916 0.0962 0.0164 0.078 Uiso 1 1 calc R . . C2 C 0.1810(3) 0.5134(2) 0.05621(17) 0.0668(12) Uani 1 1 d . B . H2A H 0.2400 0.5506 0.0530 0.100 Uiso 1 1 calc R . . H2B H 0.1071 0.5507 0.0657 0.100 Uiso 1 1 calc R . . H2C H 0.1862 0.4874 0.0077 0.100 Uiso 1 1 calc R . . C20 C 0.8200(3) 0.1906(3) 0.1258(2) 0.0755(14) Uani 1 1 d . . . H20A H 0.8074 0.1492 0.1725 0.113 Uiso 1 1 calc R . . H20B H 0.8277 0.2492 0.1400 0.113 Uiso 1 1 calc R . . H20C H 0.8889 0.1661 0.0945 0.113 Uiso 1 1 calc R . . C18 C 0.7443(3) 0.2698(3) 0.0083(2) 0.0762(14) Uani 1 1 d . . . H18A H 0.8174 0.2478 -0.0195 0.114 Uiso 1 1 calc R . . H18B H 0.7463 0.3283 0.0255 0.114 Uiso 1 1 calc R . . H18C H 0.6856 0.2765 -0.0258 0.114 Uiso 1 1 calc R . . V2 V 0.02687(3) 0.86408(2) 0.440887(19) 0.01417(8) Uani 1 1 d . . . O6 O 0.12782(12) 0.77719(9) 0.48125(8) 0.0182(3) Uani 1 1 d . . . O4 O 0.07119(12) 0.88645(9) 0.34076(8) 0.0169(3) Uani 1 1 d . A . O5 O -0.10312(12) 0.82271(9) 0.44921(8) 0.0187(3) Uani 1 1 d . C . N2 N 0.00798(14) 0.96490(11) 0.48504(9) 0.0159(3) Uani 1 1 d . . . C41 C 0.23622(18) 0.73424(14) 0.50244(12) 0.0198(4) Uani 1 1 d . . . C57 C -0.30695(18) 0.87093(14) 0.47813(13) 0.0206(4) Uani 1 1 d . C . C51 C -0.20134(18) 0.79674(14) 0.49576(12) 0.0198(4) Uani 1 1 d . . . C47 C 0.28201(18) 0.66370(15) 0.44187(12) 0.0212(4) Uani 1 1 d . . . C49 C 0.1941(2) 0.60913(16) 0.42831(15) 0.0305(5) Uani 1 1 d . . . H49A H 0.2278 0.5659 0.3916 0.046 Uiso 1 1 calc R . . H49B H 0.1307 0.6498 0.4074 0.046 Uiso 1 1 calc R . . H49C H 0.1673 0.5766 0.4771 0.046 Uiso 1 1 calc R . . C31 C 0.05928(19) 0.94506(15) 0.27003(12) 0.0235(5) Uani 1 1 d D . . C60 C -0.4048(2) 0.86877(17) 0.54382(14) 0.0303(5) Uani 1 1 d . . . H60A H -0.3816 0.8847 0.5906 0.045 Uiso 1 1 calc R C . H60B H -0.4246 0.8081 0.5536 0.045 Uiso 1 1 calc R . . H60C H -0.4702 0.9121 0.5290 0.045 Uiso 1 1 calc R . . C43 C 0.2208(2) 0.69640(16) 0.59056(13) 0.0320(6) Uani 1 1 d . . . C52 C -0.1819(2) 0.7949(2) 0.57936(14) 0.0369(6) Uani 1 1 d . C . H52A H -0.1068 0.7615 0.5871 0.055 Uiso 1 1 calc R . . H52B H -0.2388 0.7653 0.6130 0.055 Uiso 1 1 calc R . . H52C H -0.1874 0.8566 0.5918 0.055 Uiso 1 1 calc R . . C58 C -0.2724(2) 0.96444(15) 0.47213(17) 0.0335(6) Uani 1 1 d . . . H58A H -0.2181 0.9725 0.4263 0.050 Uiso 1 1 calc R C . H58B H -0.2380 0.9695 0.5181 0.050 Uiso 1 1 calc R . . H58C H -0.3391 1.0109 0.4682 0.050 Uiso 1 1 calc R . . C50 C 0.3884(2) 0.59779(16) 0.46169(14) 0.0297(5) Uani 1 1 d . . . H50A H 0.3692 0.5562 0.5070 0.045 Uiso 1 1 calc R . . H50B H 0.4448 0.6316 0.4727 0.045 Uiso 1 1 calc R . . H50C H 0.4190 0.5636 0.4180 0.045 Uiso 1 1 calc R . . C42 C 0.3118(2) 0.80697(17) 0.49189(18) 0.0407(7) Uani 1 1 d . . . H42A H 0.3009 0.8451 0.4433 0.061 Uiso 1 1 calc R . . H42B H 0.3907 0.7783 0.4909 0.061 Uiso 1 1 calc R . . H42C H 0.2919 0.8440 0.5347 0.061 Uiso 1 1 calc R . . C59 C -0.3544(2) 0.8668(2) 0.40286(14) 0.0364(6) Uani 1 1 d . . . H59A H -0.4138 0.9186 0.3944 0.055 Uiso 1 1 calc R C . H59B H -0.3857 0.8110 0.4061 0.055 Uiso 1 1 calc R . . H59C H -0.2941 0.8681 0.3599 0.055 Uiso 1 1 calc R . . C33 C 0.1737(2) 0.98042(17) 0.24393(14) 0.0330(6) Uani 1 1 d . A . C48 C 0.3128(2) 0.7152(2) 0.36270(14) 0.0420(7) Uani 1 1 d . . . H48A H 0.3287 0.6733 0.3233 0.063 Uiso 1 1 calc R . . H48B H 0.3795 0.7426 0.3642 0.063 Uiso 1 1 calc R . . H48C H 0.2497 0.7624 0.3503 0.063 Uiso 1 1 calc R . . C46 C 0.1641(3) 0.61239(19) 0.60813(15) 0.0459(8) Uani 1 1 d . . . H46A H 0.1498 0.5977 0.6640 0.069 Uiso 1 1 calc R . . H46B H 0.2136 0.5617 0.5857 0.069 Uiso 1 1 calc R . . H46C H 0.0927 0.6240 0.5859 0.069 Uiso 1 1 calc R . . C44 C 0.1446(3) 0.7694(2) 0.63600(15) 0.0513(9) Uani 1 1 d . . . H44A H 0.0690 0.7801 0.6198 0.077 Uiso 1 1 calc R . . H44B H 0.1764 0.8254 0.6257 0.077 Uiso 1 1 calc R . . H44C H 0.1403 0.7490 0.6912 0.077 Uiso 1 1 calc R . . C45 C 0.3335(3) 0.6750(2) 0.62551(17) 0.0532(9) Uani 1 1 d . . . H45A H 0.3206 0.6491 0.6792 0.080 Uiso 1 1 calc R . . H45B H 0.3650 0.7306 0.6233 0.080 Uiso 1 1 calc R . . H45C H 0.3865 0.6318 0.5962 0.080 Uiso 1 1 calc R . . C38 C 0.0036(6) 0.9482(5) 0.1337(4) 0.0313(13) Uani 0.604(3) 1 d P A 3 H38A H -0.0313 1.0115 0.1346 0.047 Uiso 0.604(3) 1 calc PR A 3 H38B H -0.0394 0.9177 0.1053 0.047 Uiso 0.604(3) 1 calc PR A 3 H38C H 0.0810 0.9449 0.1084 0.047 Uiso 0.604(3) 1 calc PR A 3 C39 C 0.0561(4) 0.8024(3) 0.2133(2) 0.0307(10) Uani 0.604(3) 1 d P A 3 H39A H 0.1309 0.7977 0.1837 0.046 Uiso 0.604(3) 1 calc PR A 3 H39B H 0.0075 0.7726 0.1886 0.046 Uiso 0.604(3) 1 calc PR A 3 H39C H 0.0625 0.7732 0.2658 0.046 Uiso 0.604(3) 1 calc PR A 3 C32 C -0.0178(4) 1.0368(3) 0.2942(3) 0.0314(10) Uani 0.604(3) 1 d P A 3 H32A H -0.0848 1.0227 0.3280 0.047 Uiso 0.604(3) 1 calc PR A 3 H32B H -0.0407 1.0749 0.2480 0.047 Uiso 0.604(3) 1 calc PR A 3 H32C H 0.0252 1.0688 0.3214 0.047 Uiso 0.604(3) 1 calc PR A 3 C40 C -0.1204(3) 0.9017(3) 0.2487(2) 0.0314(10) Uani 0.604(3) 1 d P A 3 H40A H -0.1251 0.8785 0.3034 0.047 Uiso 0.604(3) 1 calc PR A 3 H40B H -0.1529 0.8631 0.2205 0.047 Uiso 0.604(3) 1 calc PR A 3 H40C H -0.1623 0.9631 0.2429 0.047 Uiso 0.604(3) 1 calc PR A 3 C68 C 0.1778(6) 1.0618(5) 0.1873(4) 0.0519(19) Uani 0.604(3) 1 d P A 3 H68A H 0.1478 1.1158 0.2131 0.078 Uiso 0.604(3) 1 calc PR A 3 H68B H 0.1325 1.0592 0.1461 0.078 Uiso 0.604(3) 1 calc PR A 3 H68C H 0.2560 1.0641 0.1653 0.078 Uiso 0.604(3) 1 calc PR A 3 C35 C 0.2633(3) 0.9008(3) 0.2014(2) 0.0345(11) Uani 0.604(3) 1 d P A 3 H35A H 0.3392 0.9164 0.1944 0.052 Uiso 0.604(3) 1 calc PR A 3 H35B H 0.2407 0.8961 0.1511 0.052 Uiso 0.604(3) 1 calc PR A 3 H35C H 0.2630 0.8431 0.2335 0.052 Uiso 0.604(3) 1 calc PR A 3 C36 C 0.2389(4) 0.9876(3) 0.3116(3) 0.0399(11) Uani 0.604(3) 1 d P A 3 H36A H 0.2597 0.9276 0.3387 0.060 Uiso 0.604(3) 1 calc PR A 3 H36B H 0.1911 1.0266 0.3473 0.060 Uiso 0.604(3) 1 calc PR A 3 H36C H 0.3071 1.0132 0.2917 0.060 Uiso 0.604(3) 1 calc PR A 3 C37 C 0.0047(5) 0.9024(4) 0.2160(3) 0.0230(10) Uani 0.604(3) 1 d P A 3 C64 C 0.1506(5) 0.8097(4) 0.1787(4) 0.0266(14) Uani 0.396(3) 1 d P A 4 H64A H 0.1910 0.7789 0.2216 0.040 Uiso 0.396(3) 1 calc PR A 4 H64B H 0.1980 0.8485 0.1453 0.040 Uiso 0.396(3) 1 calc PR A 4 H64C H 0.1328 0.7649 0.1490 0.040 Uiso 0.396(3) 1 calc PR A 4 C65 C -0.0323(6) 0.8005(4) 0.2540(3) 0.0317(15) Uani 0.396(3) 1 d P A 4 H65A H -0.0515 0.7638 0.2176 0.047 Uiso 0.396(3) 1 calc PR A 4 H65B H -0.1015 0.8329 0.2795 0.047 Uiso 0.396(3) 1 calc PR A 4 H65C H 0.0098 0.7615 0.2926 0.047 Uiso 0.396(3) 1 calc PR A 4 C34 C 0.1697(8) 1.0347(6) 0.1621(4) 0.0244(17) Uani 0.396(3) 1 d P A 4 H34A H 0.2284 1.0728 0.1527 0.037 Uiso 0.396(3) 1 calc PR A 4 H34B H 0.0959 1.0725 0.1594 0.037 Uiso 0.396(3) 1 calc PR A 4 H34C H 0.1825 0.9926 0.1230 0.037 Uiso 0.396(3) 1 calc PR A 4 C63 C -0.0518(6) 1.0029(5) 0.2815(4) 0.0267(14) Uani 0.396(3) 1 d P A 4 H63A H -0.1113 0.9657 0.2874 0.040 Uiso 0.396(3) 1 calc PR A 4 H63B H -0.0610 1.0481 0.2368 0.040 Uiso 0.396(3) 1 calc PR A 4 H63C H -0.0568 1.0331 0.3279 0.040 Uiso 0.396(3) 1 calc PR A 4 C66 C 0.2745(5) 0.9295(4) 0.2599(3) 0.0247(13) Uani 0.396(3) 1 d P A 4 H66A H 0.3351 0.9651 0.2435 0.037 Uiso 0.396(3) 1 calc PR A 4 H66B H 0.2889 0.8759 0.2322 0.037 Uiso 0.396(3) 1 calc PR A 4 H66C H 0.2716 0.9109 0.3154 0.037 Uiso 0.396(3) 1 calc PR A 4 C67 C 0.1485(6) 1.0643(4) 0.2989(3) 0.0281(14) Uani 0.396(3) 1 d P A 4 H67A H 0.1316 1.0404 0.3528 0.042 Uiso 0.396(3) 1 calc PR A 4 H67B H 0.0840 1.1080 0.2830 0.042 Uiso 0.396(3) 1 calc PR A 4 H67C H 0.2149 1.0940 0.2934 0.042 Uiso 0.396(3) 1 calc PR A 4 C69 C -0.0189(10) 0.9163(7) 0.1418(6) 0.035(2) Uani 0.396(3) 1 d P A 4 H69A H -0.0295 0.8718 0.1090 0.052 Uiso 0.396(3) 1 calc PR A 4 H69B H 0.0277 0.9583 0.1120 0.052 Uiso 0.396(3) 1 calc PR A 4 H69C H -0.0923 0.9496 0.1600 0.052 Uiso 0.396(3) 1 calc PR A 4 C70 C 0.0395(7) 0.8681(5) 0.2107(4) 0.0175(14) Uani 0.396(3) 1 d PD A 4 C7 C 0.1040(7) 0.3828(5) 0.1193(4) 0.0237(13) Uani 0.653(5) 1 d P B 1 C8 C 0.0947(3) 0.3713(3) 0.0345(2) 0.0336(10) Uani 0.653(5) 1 d P B 1 H8A H 0.0668 0.4299 0.0074 0.050 Uiso 0.653(5) 1 calc PR B 1 H8B H 0.0424 0.3294 0.0333 0.050 Uiso 0.653(5) 1 calc PR B 1 H8C H 0.1690 0.3474 0.0094 0.050 Uiso 0.653(5) 1 calc PR B 1 C9 C -0.0133(9) 0.4274(6) 0.1525(5) 0.0380(19) Uani 0.653(5) 1 d P B 1 H9A H -0.0303 0.4887 0.1268 0.057 Uiso 0.653(5) 1 calc PR B 1 H9B H -0.0146 0.4296 0.2078 0.057 Uiso 0.653(5) 1 calc PR B 1 H9C H -0.0698 0.3922 0.1439 0.057 Uiso 0.653(5) 1 calc PR B 1 C10 C 0.1291(3) 0.2871(3) 0.1601(2) 0.0324(10) Uani 0.653(5) 1 d P B 1 H10A H 0.0716 0.2526 0.1521 0.049 Uiso 0.653(5) 1 calc PR B 1 H10B H 0.1284 0.2898 0.2153 0.049 Uiso 0.653(5) 1 calc PR B 1 H10C H 0.2033 0.2577 0.1389 0.049 Uiso 0.653(5) 1 calc PR B 1 C61 C 0.1357(6) 0.2937(5) 0.0816(4) 0.0268(17) Uani 0.347(5) 1 d P B 2 H61A H 0.2062 0.2539 0.0914 0.040 Uiso 0.347(5) 1 calc PR B 2 H61B H 0.1447 0.3263 0.0300 0.040 Uiso 0.347(5) 1 calc PR B 2 H61C H 0.0754 0.2577 0.0851 0.040 Uiso 0.347(5) 1 calc PR B 2 C62 C 0.1069(6) 0.3061(4) 0.2209(4) 0.0242(16) Uani 0.347(5) 1 d P B 2 H62A H 0.0565 0.2615 0.2254 0.036 Uiso 0.347(5) 1 calc PR B 2 H62B H 0.0816 0.3466 0.2610 0.036 Uiso 0.347(5) 1 calc PR B 2 H62C H 0.1836 0.2752 0.2270 0.036 Uiso 0.347(5) 1 calc PR B 2 C81 C 0.1056(12) 0.3611(9) 0.1413(7) 0.018(2) Uani 0.347(5) 1 d PD B 2 C80 C -0.0180(17) 0.4063(10) 0.1354(9) 0.029(3) Uani 0.347(5) 1 d P B 2 H80A H -0.0240 0.4393 0.0842 0.043 Uiso 0.347(5) 1 calc PR B 2 H80B H -0.0415 0.4482 0.1745 0.043 Uiso 0.347(5) 1 calc PR B 2 H80C H -0.0666 0.3600 0.1438 0.043 Uiso 0.347(5) 1 calc PR B 2 C6 C 0.1957(4) 0.4080(3) 0.2717(2) 0.0390(13) Uani 0.654(5) 1 d P B 5 H6A H 0.2453 0.3513 0.2620 0.059 Uiso 0.654(5) 1 calc PR B 5 H6B H 0.1175 0.3975 0.2825 0.059 Uiso 0.654(5) 1 calc PR B 5 H6C H 0.2168 0.4310 0.3161 0.059 Uiso 0.654(5) 1 calc PR B 5 C4 C 0.1269(7) 0.5635(4) 0.2125(4) 0.060(2) Uani 0.654(5) 1 d P B 5 H4A H 0.1364 0.5811 0.2624 0.091 Uiso 0.654(5) 1 calc PR B 5 H4B H 0.0500 0.5517 0.2136 0.091 Uiso 0.654(5) 1 calc PR B 5 H4C H 0.1407 0.6124 0.1719 0.091 Uiso 0.654(5) 1 calc PR B 5 C5 C 0.3301(4) 0.4984(3) 0.1970(2) 0.0438(13) Uani 0.654(5) 1 d P B 5 H5A H 0.3341 0.5278 0.2425 0.066 Uiso 0.654(5) 1 calc PR B 5 H5B H 0.3514 0.5374 0.1505 0.066 Uiso 0.654(5) 1 calc PR B 5 H5C H 0.3818 0.4409 0.1983 0.066 Uiso 0.654(5) 1 calc PR B 5 C71 C 0.0888(8) 0.5348(6) 0.2321(5) 0.0245(18) Uani 0.346(5) 1 d P B 6 H71A H 0.0424 0.4916 0.2600 0.037 Uiso 0.346(5) 1 calc PR B 6 H71B H 0.0497 0.5700 0.1903 0.037 Uiso 0.346(5) 1 calc PR B 6 H71C H 0.1022 0.5753 0.2675 0.037 Uiso 0.346(5) 1 calc PR B 6 C73 C 0.2713(6) 0.4340(5) 0.2518(4) 0.0244(17) Uani 0.346(5) 1 d P B 6 H73A H 0.2701 0.4718 0.2929 0.037 Uiso 0.346(5) 1 calc PR B 6 H73B H 0.3490 0.4171 0.2287 0.037 Uiso 0.346(5) 1 calc PR B 6 H73C H 0.2399 0.3796 0.2733 0.037 Uiso 0.346(5) 1 calc PR B 6 C72 C 0.2666(6) 0.5675(4) 0.1585(4) 0.0288(18) Uani 0.346(5) 1 d P B 6 H72A H 0.2866 0.5975 0.1993 0.043 Uiso 0.346(5) 1 calc PR B 6 H72B H 0.2137 0.6098 0.1287 0.043 Uiso 0.346(5) 1 calc PR B 6 H72C H 0.3346 0.5473 0.1245 0.043 Uiso 0.346(5) 1 calc PR B 6 C85 C -0.3116(10) 0.6622(8) 0.5306(9) 0.035(2) Uani 0.44(2) 1 d P C 7 H85A H -0.3057 0.5971 0.5298 0.052 Uiso 0.44(2) 1 calc PR C 7 H85B H -0.3727 0.6938 0.5014 0.052 Uiso 0.44(2) 1 calc PR C 7 H85C H -0.3275 0.6767 0.5839 0.052 Uiso 0.44(2) 1 calc PR C 7 C86 C -0.1040(6) 0.6347(6) 0.5348(9) 0.031(2) Uani 0.44(2) 1 d P C 7 H86A H -0.0938 0.5728 0.5215 0.046 Uiso 0.44(2) 1 calc PR C 7 H86B H -0.1234 0.6348 0.5905 0.046 Uiso 0.44(2) 1 calc PR C 7 H86C H -0.0340 0.6592 0.5188 0.046 Uiso 0.44(2) 1 calc PR C 7 C87 C -0.1782(7) 0.6717(7) 0.4092(9) 0.032(2) Uani 0.44(2) 1 d P C 7 H87A H -0.1047 0.6860 0.3859 0.048 Uiso 0.44(2) 1 calc PR C 7 H87B H -0.2372 0.7080 0.3806 0.048 Uiso 0.44(2) 1 calc PR C 7 H87C H -0.1797 0.6076 0.4075 0.048 Uiso 0.44(2) 1 calc PR C 7 C88 C -0.1988(11) 0.6927(9) 0.4935(8) 0.024(2) Uani 0.44(2) 1 d P C 7 C53 C -0.2053(7) 0.7000(6) 0.4664(6) 0.0164(15) Uani 0.56(2) 1 d P C 8 C54 C -0.1840(5) 0.6991(6) 0.3783(5) 0.0263(15) Uani 0.56(2) 1 d P C 8 H54A H -0.1850 0.6384 0.3654 0.039 Uiso 0.56(2) 1 calc PR C 8 H54B H -0.1105 0.7166 0.3592 0.039 Uiso 0.56(2) 1 calc PR C 8 H54C H -0.2430 0.7417 0.3542 0.039 Uiso 0.56(2) 1 calc PR C 8 C55 C -0.3138(7) 0.6624(6) 0.4971(7) 0.0296(17) Uani 0.56(2) 1 d P C 8 H55A H -0.3068 0.6009 0.4835 0.044 Uiso 0.56(2) 1 calc PR C 8 H55B H -0.3774 0.7005 0.4743 0.044 Uiso 0.56(2) 1 calc PR C 8 H55C H -0.3266 0.6616 0.5532 0.044 Uiso 0.56(2) 1 calc PR C 8 C56 C -0.1074(5) 0.6330(4) 0.4976(7) 0.0264(16) Uani 0.56(2) 1 d P C 8 H56A H -0.1255 0.6177 0.5531 0.040 Uiso 0.56(2) 1 calc PR C 8 H56B H -0.0389 0.6604 0.4881 0.040 Uiso 0.56(2) 1 calc PR C 8 H56C H -0.0953 0.5783 0.4717 0.040 Uiso 0.56(2) 1 calc PR C 8 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 0.01826(19) 0.01186(16) 0.01412(16) -0.00128(12) -0.00395(13) -0.00387(13) O1 0.0224(8) 0.0144(7) 0.0200(7) 0.0003(6) -0.0070(6) -0.0033(6) O2 0.0201(8) 0.0162(7) 0.0179(7) -0.0025(6) -0.0020(6) -0.0036(6) O3 0.0244(8) 0.0177(7) 0.0161(7) -0.0056(6) -0.0034(6) -0.0050(6) N1 0.0168(9) 0.0148(8) 0.0136(7) -0.0028(6) -0.0013(6) -0.0017(7) C21 0.0234(12) 0.0211(10) 0.0165(9) -0.0060(8) -0.0026(8) -0.0014(9) C22 0.0228(12) 0.0212(10) 0.0180(10) -0.0039(8) -0.0032(8) -0.0020(8) C1 0.0296(13) 0.0174(10) 0.0181(10) -0.0032(8) -0.0036(9) 0.0057(9) C13 0.0305(13) 0.0300(12) 0.0186(10) 0.0021(9) -0.0011(9) 0.0061(10) C23 0.0534(17) 0.0191(11) 0.0337(13) 0.0018(10) -0.0167(12) -0.0069(11) C24 0.0240(13) 0.0321(13) 0.0301(12) -0.0092(10) -0.0047(10) 0.0008(10) C11 0.0334(13) 0.0123(10) 0.0308(12) -0.0001(8) -0.0191(10) -0.0036(9) C25 0.0321(14) 0.0392(14) 0.0187(10) 0.0024(10) -0.0035(9) -0.0052(11) C3 0.0429(16) 0.0318(13) 0.0267(12) -0.0157(10) -0.0026(11) -0.0031(11) C26 0.0236(14) 0.072(2) 0.0240(12) -0.0070(12) -0.0032(10) 0.0028(13) C27 0.0661(19) 0.0179(11) 0.0245(11) -0.0080(9) -0.0203(12) -0.0012(11) C12 0.112(3) 0.0195(13) 0.098(3) -0.0139(15) -0.085(3) 0.0031(16) C28 0.098(3) 0.0328(15) 0.0364(15) 0.0052(12) -0.0188(16) -0.0418(16) C14 0.0411(17) 0.0382(15) 0.0547(17) 0.0241(13) -0.0144(13) -0.0222(13) C16 0.0484(17) 0.0366(14) 0.0243(12) 0.0075(11) -0.0086(11) 0.0056(12) C29 0.119(3) 0.0267(14) 0.0436(17) -0.0123(12) -0.0497(19) 0.0157(17) C17 0.0202(13) 0.0451(16) 0.0454(15) 0.0260(13) -0.0086(11) -0.0070(11) C15 0.072(2) 0.094(3) 0.0216(13) 0.0071(15) 0.0059(14) 0.048(2) C30 0.094(3) 0.0225(13) 0.0391(15) -0.0174(11) -0.0380(16) 0.0144(14) C19 0.0501(19) 0.0548(19) 0.0331(14) 0.0010(13) 0.0071(13) 0.0276(15) C2 0.095(3) 0.0491(19) 0.0315(15) 0.0115(14) -0.0018(16) 0.0385(19) C20 0.0361(18) 0.082(3) 0.105(3) 0.062(2) -0.0422(19) -0.0280(17) C18 0.0265(16) 0.098(3) 0.086(3) 0.070(2) -0.0124(16) -0.0161(17) V2 0.01396(18) 0.01368(16) 0.01598(16) -0.00405(12) -0.00170(13) -0.00351(13) O6 0.0179(8) 0.0173(7) 0.0199(7) -0.0052(6) -0.0040(6) -0.0005(6) O4 0.0176(8) 0.0167(7) 0.0166(7) -0.0031(5) -0.0005(5) -0.0033(6) O5 0.0170(8) 0.0185(7) 0.0225(7) -0.0066(6) 0.0008(6) -0.0074(6) N2 0.0133(8) 0.0181(8) 0.0170(8) -0.0045(6) -0.0008(6) -0.0032(7) C41 0.0209(11) 0.0168(10) 0.0237(10) -0.0033(8) -0.0094(8) -0.0031(8) C57 0.0183(11) 0.0170(10) 0.0275(11) -0.0033(8) -0.0044(9) -0.0035(8) C51 0.0160(11) 0.0161(10) 0.0268(11) -0.0026(8) 0.0017(8) -0.0043(8) C47 0.0183(11) 0.0241(11) 0.0196(10) -0.0020(8) -0.0011(8) 0.0000(9) C49 0.0291(13) 0.0288(12) 0.0362(13) -0.0192(10) -0.0116(10) 0.0058(10) C31 0.0193(11) 0.0263(11) 0.0211(10) 0.0037(9) -0.0019(8) 0.0017(9) C60 0.0182(12) 0.0333(13) 0.0383(13) -0.0083(11) 0.0005(10) -0.0010(10) C43 0.0474(16) 0.0277(12) 0.0203(11) -0.0079(9) -0.0106(10) 0.0045(11) C52 0.0225(13) 0.0577(17) 0.0245(12) 0.0078(12) -0.0002(10) -0.0015(12) C58 0.0252(13) 0.0162(11) 0.0591(17) -0.0022(11) -0.0111(12) -0.0002(9) C50 0.0218(12) 0.0293(12) 0.0357(13) -0.0024(10) -0.0051(10) 0.0027(10) C42 0.0334(15) 0.0221(12) 0.072(2) 0.0049(12) -0.0280(14) -0.0101(11) C59 0.0321(15) 0.0515(16) 0.0304(13) 0.0026(12) -0.0112(11) -0.0190(12) C33 0.0393(15) 0.0341(13) 0.0291(12) 0.0054(10) -0.0048(11) -0.0216(11) C48 0.0296(14) 0.0563(18) 0.0257(12) 0.0100(12) 0.0080(10) 0.0127(12) C46 0.063(2) 0.0358(15) 0.0276(13) 0.0055(11) 0.0144(13) 0.0003(14) C44 0.081(2) 0.0456(17) 0.0238(13) -0.0170(12) -0.0163(14) 0.0163(16) C45 0.077(2) 0.0445(17) 0.0414(16) -0.0170(13) -0.0414(16) 0.0171(16) C38 0.029(3) 0.042(4) 0.021(2) 0.005(3) -0.005(2) -0.003(2) C39 0.042(3) 0.033(3) 0.0193(18) -0.0086(17) -0.0043(17) -0.0055(19) C32 0.030(3) 0.019(2) 0.041(3) -0.0065(19) -0.003(2) 0.0087(18) C40 0.022(2) 0.041(2) 0.031(2) 0.0036(18) -0.0081(16) -0.0066(17) C68 0.037(3) 0.045(4) 0.071(5) 0.032(3) -0.015(4) -0.020(3) C35 0.019(2) 0.049(3) 0.029(2) 0.0036(19) 0.0050(16) 0.0001(18) C36 0.036(3) 0.033(2) 0.054(3) -0.001(2) -0.010(2) -0.016(2) C37 0.027(3) 0.016(3) 0.025(2) 0.002(2) -0.004(2) -0.0021(19) C64 0.035(4) 0.020(3) 0.024(3) -0.007(2) -0.001(2) -0.002(2) C65 0.040(4) 0.037(3) 0.027(3) -0.016(3) -0.002(3) -0.023(3) C34 0.031(4) 0.029(4) 0.015(3) -0.002(2) 0.000(3) -0.011(3) C63 0.031(4) 0.025(4) 0.022(3) -0.001(3) -0.004(3) 0.002(3) C66 0.018(3) 0.030(3) 0.027(3) 0.001(2) -0.006(2) -0.008(2) C67 0.048(4) 0.020(3) 0.021(3) -0.004(2) 0.000(3) -0.018(3) C69 0.037(5) 0.044(6) 0.027(4) -0.006(4) -0.008(4) -0.009(4) C70 0.028(5) 0.014(4) 0.015(3) -0.005(3) -0.005(3) -0.010(3) C7 0.021(2) 0.024(4) 0.022(3) -0.001(2) -0.003(3) 0.007(2) C8 0.024(2) 0.045(2) 0.031(2) -0.0137(17) -0.0069(15) 0.0052(17) C9 0.026(3) 0.052(5) 0.031(3) -0.012(3) -0.002(2) 0.011(4) C10 0.022(2) 0.032(2) 0.042(2) -0.0017(18) -0.0009(16) -0.0064(16) C61 0.027(4) 0.031(4) 0.026(3) -0.009(3) 0.001(3) -0.011(3) C62 0.028(4) 0.020(3) 0.023(3) 0.003(3) 0.004(3) -0.009(3) C81 0.017(4) 0.020(7) 0.017(6) 0.002(4) -0.002(4) -0.006(4) C80 0.024(5) 0.026(5) 0.038(7) -0.010(5) 0.000(6) -0.007(4) C6 0.046(3) 0.046(3) 0.0188(17) -0.0093(17) -0.0065(18) 0.017(2) C4 0.090(6) 0.044(4) 0.043(4) -0.027(3) -0.024(3) 0.032(3) C5 0.068(3) 0.033(2) 0.037(2) -0.0196(18) -0.013(2) -0.008(2) C71 0.022(4) 0.026(5) 0.022(4) -0.003(3) 0.005(3) 0.000(3) C73 0.028(4) 0.028(4) 0.018(3) -0.012(3) 0.001(3) -0.002(3) C72 0.033(4) 0.022(3) 0.031(4) -0.010(3) 0.009(3) -0.009(3) C85 0.023(4) 0.024(4) 0.057(7) 0.010(5) -0.006(5) -0.011(3) C86 0.018(3) 0.025(3) 0.049(7) 0.004(4) -0.007(4) -0.002(2) C87 0.036(4) 0.016(4) 0.048(6) -0.012(4) -0.004(4) -0.010(3) C88 0.025(4) 0.022(4) 0.026(5) 0.005(4) -0.009(4) -0.008(3) C53 0.014(2) 0.008(2) 0.027(4) -0.003(3) -0.005(3) -0.0019(17) C54 0.032(3) 0.021(3) 0.029(3) -0.011(3) -0.002(2) -0.006(2) C55 0.024(3) 0.018(2) 0.048(5) -0.003(3) 0.000(3) -0.0088(19) C56 0.024(3) 0.018(2) 0.037(4) -0.002(3) -0.004(3) -0.0031(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 N1 1.7712(16) . ? V1 O3 1.7814(14) . ? V1 O1 1.7823(14) . ? V1 O2 1.7852(15) . ? O1 C11 1.440(2) . ? O2 C1 1.444(3) . ? O3 C21 1.439(2) . ? N1 N1 1.232(3) 2_665 ? C21 C26 1.528(3) . ? C21 C22 1.587(3) . ? C21 C27 1.595(3) . ? C22 C24 1.533(3) . ? C22 C23 1.534(3) . ? C22 C25 1.544(3) . ? C1 C7 1.521(9) . ? C1 C2 1.531(3) . ? C1 C3 1.579(3) . ? C1 C81 1.713(13) . ? C13 C14 1.525(4) . ? C13 C16 1.539(3) . ? C13 C15 1.542(4) . ? C13 C11 1.585(3) . ? C11 C12 1.520(3) . ? C11 C17 1.590(4) . ? C3 C73 1.369(7) . ? C3 C4 1.483(6) . ? C3 C5 1.554(5) . ? C3 C6 1.620(5) . ? C3 C71 1.620(10) . ? C3 C72 1.629(7) . ? C27 C28 1.525(4) . ? C27 C30 1.540(3) . ? C27 C29 1.548(4) . ? C17 C19 1.523(4) . ? C17 C18 1.541(3) . ? C17 C20 1.551(4) . ? V2 N2 1.7731(17) . ? V2 O4 1.7814(14) . ? V2 O6 1.7817(14) . ? V2 O5 1.7826(14) . ? O6 C41 1.439(2) . ? O4 C31 1.443(2) . ? O5 C51 1.438(2) . ? N2 N2 1.225(3) 2_576 ? C41 C42 1.535(3) . ? C41 C43 1.583(3) . ? C41 C47 1.590(3) . ? C57 C59 1.533(3) . ? C57 C58 1.537(3) . ? C57 C60 1.544(3) . ? C57 C51 1.587(3) . ? C51 C52 1.522(3) . ? C51 C88 1.580(13) . ? C51 C53 1.631(8) . ? C47 C49 1.524(3) . ? C47 C50 1.540(3) . ? C47 C48 1.541(3) . ? C31 C63 1.479(7) . ? C31 C37 1.503(6) . ? C31 C33 1.568(3) . ? C31 C32 1.608(5) . ? C31 C70 1.735(7) . ? C43 C46 1.532(4) . ? C43 C45 1.545(4) . ? C43 C44 1.548(4) . ? C33 C66 1.372(6) . ? C33 C68 1.487(6) . ? C33 C36 1.548(5) . ? C33 C34 1.568(8) . ? C33 C35 1.661(5) . ? C33 C67 1.662(6) . ? C38 C37 1.527(8) . ? C39 C37 1.541(6) . ? C40 C37 1.551(7) . ? C64 C70 1.558(10) . ? C65 C70 1.524(9) . ? C69 C70 1.530(13) . ? C7 C10 1.533(7) . ? C7 C9 1.539(13) . ? C7 C8 1.551(8) . ? C61 C81 1.529(17) . ? C62 C81 1.536(10) . ? C81 C80 1.55(2) . ? C85 C88 1.555(17) . ? C86 C88 1.530(12) . ? C87 C88 1.541(11) . ? C53 C55 1.533(12) . ? C53 C56 1.537(9) . ? C53 C54 1.542(8) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 V1 O3 112.90(7) . . ? N1 V1 O1 111.21(7) . . ? O3 V1 O1 107.29(7) . . ? N1 V1 O2 109.30(7) . . ? O3 V1 O2 107.36(7) . . ? O1 V1 O2 108.61(7) . . ? C11 O1 V1 150.67(13) . . ? C1 O2 V1 147.50(13) . . ? C21 O3 V1 150.82(14) . . ? N1 N1 V1 178.6(2) 2_665 . ? O3 C21 C26 106.81(18) . . ? O3 C21 C22 108.41(16) . . ? C26 C21 C22 109.00(18) . . ? O3 C21 C27 105.06(16) . . ? C26 C21 C27 109.3(2) . . ? C22 C21 C27 117.66(18) . . ? C24 C22 C23 105.97(19) . . ? C24 C22 C25 107.65(18) . . ? C23 C22 C25 106.43(19) . . ? C24 C22 C21 114.96(18) . . ? C23 C22 C21 108.69(17) . . ? C25 C22 C21 112.61(18) . . ? O2 C1 C7 107.1(3) . . ? O2 C1 C2 105.9(2) . . ? C7 C1 C2 104.7(3) . . ? O2 C1 C3 107.74(18) . . ? C7 C1 C3 122.2(3) . . ? C2 C1 C3 108.2(2) . . ? O2 C1 C81 102.3(5) . . ? C7 C1 C81 15.5(4) . . ? C2 C1 C81 120.1(4) . . ? C3 C1 C81 111.8(5) . . ? C14 C13 C16 108.7(2) . . ? C14 C13 C15 105.4(3) . . ? C16 C13 C15 106.9(2) . . ? C14 C13 C11 112.63(19) . . ? C16 C13 C11 114.0(2) . . ? C15 C13 C11 108.7(2) . . ? O1 C11 C12 106.62(18) . . ? O1 C11 C13 104.86(17) . . ? C12 C11 C13 110.8(2) . . ? O1 C11 C17 107.88(18) . . ? C12 C11 C17 108.9(2) . . ? C13 C11 C17 117.18(18) . . ? C73 C3 C4 121.2(4) . . ? C73 C3 C5 60.7(4) . . ? C4 C3 C5 109.8(4) . . ? C73 C3 C1 121.0(3) . . ? C4 C3 C1 116.2(3) . . ? C5 C3 C1 111.2(2) . . ? C73 C3 C6 40.5(3) . . ? C4 C3 C6 107.4(3) . . ? C5 C3 C6 101.2(3) . . ? C1 C3 C6 109.9(2) . . ? C73 C3 C71 113.3(5) . . ? C4 C3 C71 26.2(4) . . ? C5 C3 C71 130.5(4) . . ? C1 C3 C71 111.8(4) . . ? C6 C3 C71 86.1(4) . . ? C73 C3 C72 108.3(5) . . ? C4 C3 C72 72.1(4) . . ? C5 C3 C72 50.2(3) . . ? C1 C3 C72 100.8(3) . . ? C6 C3 C72 144.9(4) . . ? C71 C3 C72 98.3(4) . . ? C28 C27 C30 109.8(2) . . ? C28 C27 C29 104.7(2) . . ? C30 C27 C29 106.7(2) . . ? C28 C27 C21 113.8(2) . . ? C30 C27 C21 112.2(2) . . ? C29 C27 C21 109.1(2) . . ? C19 C17 C18 106.7(3) . . ? C19 C17 C20 107.5(3) . . ? C18 C17 C20 105.6(2) . . ? C19 C17 C11 115.2(2) . . ? C18 C17 C11 108.8(2) . . ? C20 C17 C11 112.4(3) . . ? N2 V2 O4 109.55(7) . . ? N2 V2 O6 113.14(7) . . ? O4 V2 O6 108.47(7) . . ? N2 V2 O5 110.30(7) . . ? O4 V2 O5 107.03(7) . . ? O6 V2 O5 108.15(7) . . ? C41 O6 V2 157.12(13) . . ? C31 O4 V2 148.26(13) . . ? C51 O5 V2 150.01(13) . . ? N2 N2 V2 178.2(2) 2_576 . ? O6 C41 C42 107.31(17) . . ? O6 C41 C43 108.12(18) . . ? C42 C41 C43 108.8(2) . . ? O6 C41 C47 104.98(16) . . ? C42 C41 C47 109.6(2) . . ? C43 C41 C47 117.57(17) . . ? C59 C57 C58 106.21(19) . . ? C59 C57 C60 107.54(19) . . ? C58 C57 C60 106.35(19) . . ? C59 C57 C51 115.53(19) . . ? C58 C57 C51 108.66(17) . . ? C60 C57 C51 112.02(17) . . ? O5 C51 C52 106.84(18) . . ? O5 C51 C88 108.7(5) . . ? C52 C51 C88 99.0(5) . . ? O5 C51 C57 108.63(16) . . ? C52 C51 C57 109.16(18) . . ? C88 C51 C57 123.3(5) . . ? O5 C51 C53 101.6(3) . . ? C52 C51 C53 116.5(4) . . ? C88 C51 C53 17.5(3) . . ? C57 C51 C53 113.4(4) . . ? C49 C47 C50 108.36(19) . . ? C49 C47 C48 104.6(2) . . ? C50 C47 C48 106.79(19) . . ? C49 C47 C41 113.33(18) . . ? C50 C47 C41 114.14(18) . . ? C48 C47 C41 108.96(19) . . ? O4 C31 C63 106.2(3) . . ? O4 C31 C37 110.2(3) . . ? C63 C31 C37 84.4(4) . . ? O4 C31 C33 107.59(17) . . ? C63 C31 C33 124.9(4) . . ? C37 C31 C33 121.3(3) . . ? O4 C31 C32 105.8(2) . . ? C63 C31 C32 29.2(3) . . ? C37 C31 C32 111.1(3) . . ? C33 C31 C32 99.4(3) . . ? O4 C31 C70 99.8(3) . . ? C63 C31 C70 104.3(4) . . ? C37 C31 C70 20.5(3) . . ? C33 C31 C70 111.1(3) . . ? C32 C31 C70 131.6(4) . . ? C46 C43 C45 107.9(2) . . ? C46 C43 C44 106.1(2) . . ? C45 C43 C44 106.6(2) . . ? C46 C43 C41 114.8(2) . . ? C45 C43 C41 112.2(2) . . ? C44 C43 C41 108.77(19) . . ? C66 C33 C68 117.2(4) . . ? C66 C33 C36 53.8(3) . . ? C68 C33 C36 109.4(4) . . ? C66 C33 C31 121.7(3) . . ? C68 C33 C31 119.9(3) . . ? C36 C33 C31 113.6(2) . . ? C66 C33 C34 117.3(5) . . ? C68 C33 C34 25.3(3) . . ? C36 C33 C34 131.8(4) . . ? C31 C33 C34 109.3(4) . . ? C66 C33 C35 45.6(3) . . ? C68 C33 C35 103.5(4) . . ? C36 C33 C35 99.4(3) . . ? C31 C33 C35 108.5(2) . . ? C34 C33 C35 86.8(4) . . ? C66 C33 C67 107.0(4) . . ? C68 C33 C67 76.6(4) . . ? C36 C33 C67 54.3(3) . . ? C31 C33 C67 96.4(3) . . ? C34 C33 C67 100.6(4) . . ? C35 C33 C67 150.1(3) . . ? C31 C37 C38 116.8(4) . . ? C31 C37 C39 111.2(4) . . ? C38 C37 C39 108.7(5) . . ? C31 C37 C40 108.5(4) . . ? C38 C37 C40 106.1(4) . . ? C39 C37 C40 104.8(4) . . ? C65 C70 C69 108.3(6) . . ? C65 C70 C64 104.9(6) . . ? C69 C70 C64 107.5(7) . . ? C65 C70 C31 111.2(5) . . ? C69 C70 C31 110.6(6) . . ? C64 C70 C31 113.9(5) . . ? C1 C7 C10 112.5(5) . . ? C1 C7 C9 113.5(6) . . ? C10 C7 C9 108.7(6) . . ? C1 C7 C8 109.8(4) . . ? C10 C7 C8 105.7(6) . . ? C9 C7 C8 106.1(5) . . ? C61 C81 C62 106.9(8) . . ? C61 C81 C80 107.1(10) . . ? C62 C81 C80 106.4(10) . . ? C61 C81 C1 108.9(8) . . ? C62 C81 C1 115.2(8) . . ? C80 C81 C1 111.9(9) . . ? C86 C88 C87 107.0(9) . . ? C86 C88 C85 107.9(7) . . ? C87 C88 C85 108.1(8) . . ? C86 C88 C51 112.3(8) . . ? C87 C88 C51 109.3(6) . . ? C85 C88 C51 112.0(10) . . ? C55 C53 C56 107.2(6) . . ? C55 C53 C54 109.3(5) . . ? C56 C53 C54 105.0(6) . . ? C55 C53 C51 113.4(6) . . ? C56 C53 C51 106.7(5) . . ? C54 C53 C51 114.5(5) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 28.29 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.863 _refine_diff_density_min -0.493 _refine_diff_density_rms 0.068 #============================================END data_10252_0m _database_code_depnum_ccdc_archive 'CCDC 832150' #TrackingRef '- CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[V(OR)3N](TBA)' _chemical_melting_point 'not measured' _chemical_formula_moiety 'C46 H80 N2 O3 V' _chemical_formula_sum 'C46 H80 N2 O3 V' _chemical_formula_weight 760.06 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 P21 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 12.8888(8) _cell_length_b 15.7816(10) _cell_length_c 24.2559(16) _cell_angle_alpha 90.00 _cell_angle_beta 89.9820(10) _cell_angle_gamma 90.00 _cell_volume 4933.8(5) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prisms _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.023 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1668 _exptl_absorpt_coefficient_mu 0.236 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.9542 _exptl_absorpt_correction_T_max 0.9929 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63464 _diffrn_reflns_av_R_equivalents 0.0818 _diffrn_reflns_av_sigmaI/netI 0.0790 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 24.00 _reflns_number_total 15515 _reflns_number_gt 12086 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1065P)^2^+24.8610P] 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 0.19(4) _refine_ls_number_reflns 15515 _refine_ls_number_parameters 1130 _refine_ls_number_restraints 1886 _refine_ls_R_factor_all 0.1339 _refine_ls_R_factor_gt 0.1080 _refine_ls_wR_factor_ref 0.2836 _refine_ls_wR_factor_gt 0.2664 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.151 _refine_ls_shift/su_mean 0.005 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 N2 N 0.2536(5) 0.9364(4) 0.0402(3) 0.0279(15) Uani 1 1 d U . . O6 O 0.1439(4) 0.9511(4) 0.1397(2) 0.0324(14) Uani 1 1 d U . . O5 O 0.3730(4) 0.9632(4) 0.1361(2) 0.0270(12) Uani 1 1 d U . . O4 O 0.2680(4) 0.8012(3) 0.1144(2) 0.0305(13) Uani 1 1 d U . . V1 V 0.25869(9) 0.57790(7) 0.39502(5) 0.0223(3) Uani 1 1 d U . . O1 O 0.2659(4) 0.6926(4) 0.3867(2) 0.0276(12) Uani 1 1 d U . . O3 O 0.1443(4) 0.5394(4) 0.3600(2) 0.0293(13) Uani 1 1 d U . . O2 O 0.3729(4) 0.5287(3) 0.3629(2) 0.0269(12) Uani 1 1 d U . . C115 C 0.0361(7) 0.5104(6) 0.3640(4) 0.0387(18) Uani 1 1 d U . . C118 C 0.2930(7) 0.7704(5) 0.4090(3) 0.0345(17) Uani 1 1 d U . . C112 C 0.4463(7) 0.4642(5) 0.3671(3) 0.0344(17) Uani 1 1 d U . . V2 V 0.25809(9) 0.91430(7) 0.10488(5) 0.0209(3) Uani 1 1 d U . . C47 C 0.2941(7) 0.7196(5) 0.0904(4) 0.0332(17) Uani 1 1 d U . . C66 C 0.3968(10) 1.1056(7) 0.1029(4) 0.061(3) Uani 1 1 d U . . H66A H 0.3651 1.0859 0.0685 0.092 Uiso 1 1 calc R . . H66B H 0.4515 1.1467 0.0946 0.092 Uiso 1 1 calc R . . H66C H 0.3437 1.1324 0.1260 0.092 Uiso 1 1 calc R . . C60 C 0.5752(7) 0.9056(9) 0.1150(5) 0.070(3) Uani 1 1 d U . . H60A H 0.5138 0.8719 0.1244 0.105 Uiso 1 1 calc R . . H60B H 0.6211 0.9091 0.1471 0.105 Uiso 1 1 calc R . . H60C H 0.6121 0.8786 0.0844 0.105 Uiso 1 1 calc R . . C62 C 0.4665(8) 1.0594(6) 0.1957(4) 0.044(2) Uani 1 1 d U . . C58 C 0.4425(7) 1.0318(6) 0.1330(3) 0.0372(18) Uani 1 1 d U . . C65 C 0.5308(8) 0.9935(7) 0.2289(4) 0.050(2) Uani 1 1 d U . . H65A H 0.5349 1.0111 0.2675 0.074 Uiso 1 1 calc R . . H65B H 0.6010 0.9898 0.2134 0.074 Uiso 1 1 calc R . . H65C H 0.4972 0.9379 0.2265 0.074 Uiso 1 1 calc R . . C69 C -0.0186(9) 0.9466(7) 0.1914(5) 0.062(3) Uani 1 1 d U . . C48 C 0.1977(8) 0.6843(6) 0.0604(5) 0.057(2) Uani 1 1 d U . . C64 C 0.5198(10) 1.1460(7) 0.2002(4) 0.070(3) Uani 1 1 d U . . H64A H 0.4874 1.1856 0.1743 0.105 Uiso 1 1 calc R . . H64B H 0.5936 1.1400 0.1913 0.105 Uiso 1 1 calc R . . H64C H 0.5124 1.1676 0.2379 0.105 Uiso 1 1 calc R . . C53 C 0.3412(10) 0.6673(6) 0.1424(4) 0.056(2) Uani 1 1 d U . . C73 C 0.0381(8) 1.0747(7) 0.1223(4) 0.055(2) Uani 1 1 d U . . C56 C 0.2564(13) 0.6412(7) 0.1861(5) 0.087(4) Uani 1 1 d U . . H56A H 0.2735 0.5855 0.2014 0.131 Uiso 1 1 calc R . . H56B H 0.1883 0.6388 0.1683 0.131 Uiso 1 1 calc R . . H56C H 0.2548 0.6833 0.2158 0.131 Uiso 1 1 calc R . . C51 C 0.2069(10) 0.5879(7) 0.0442(6) 0.078(4) Uani 1 1 d U . . H51A H 0.2029 0.5529 0.0775 0.117 Uiso 1 1 calc R . . H51B H 0.2736 0.5780 0.0257 0.117 Uiso 1 1 calc R . . H51C H 0.1502 0.5728 0.0191 0.117 Uiso 1 1 calc R . . C68 C -0.0116(7) 0.9311(8) 0.0860(4) 0.058(3) Uani 1 1 d U . . H68A H 0.0337 0.9379 0.0538 0.087 Uiso 1 1 calc R . . H68B H -0.0805 0.9539 0.0775 0.087 Uiso 1 1 calc R . . H68C H -0.0175 0.8708 0.0951 0.087 Uiso 1 1 calc R . . C110 C 0.0713(9) 1.0924(7) 0.0614(5) 0.061(3) Uani 1 1 d U . . H76A H 0.1372 1.0637 0.0537 0.091 Uiso 1 1 calc R . . H76B H 0.0797 1.1535 0.0559 0.091 Uiso 1 1 calc R . . H76C H 0.0178 1.0710 0.0363 0.091 Uiso 1 1 calc R . . C71 C -0.1302(9) 0.9549(8) 0.1932(6) 0.080(4) Uani 1 1 d U . . H71A H -0.1598 0.9361 0.1580 0.121 Uiso 1 1 calc R . . H71B H -0.1487 1.0143 0.1996 0.121 Uiso 1 1 calc R . . H71C H -0.1579 0.9199 0.2232 0.121 Uiso 1 1 calc R . . C70 C 0.0127(8) 0.8528(8) 0.2007(5) 0.068(3) Uani 1 1 d U . . H70A H -0.0104 0.8345 0.2373 0.102 Uiso 1 1 calc R . . H70B H 0.0883 0.8474 0.1982 0.102 Uiso 1 1 calc R . . H70C H -0.0199 0.8172 0.1725 0.102 Uiso 1 1 calc R . . C75 C -0.0763(9) 1.1153(8) 0.1257(5) 0.074(4) Uani 1 1 d U . . H75A H -0.1213 1.0881 0.0984 0.111 Uiso 1 1 calc R . . H75B H -0.0724 1.1762 0.1181 0.111 Uiso 1 1 calc R . . H75C H -0.1049 1.1063 0.1627 0.111 Uiso 1 1 calc R . . C55 C 0.4164(9) 0.7255(7) 0.1727(4) 0.064(3) Uani 1 1 d U . . H55A H 0.4565 0.6925 0.1994 0.096 Uiso 1 1 calc R . . H55B H 0.3773 0.7698 0.1920 0.096 Uiso 1 1 calc R . . H55C H 0.4637 0.7519 0.1460 0.096 Uiso 1 1 calc R . . C57 C 0.5412(8) 0.9957(9) 0.0979(4) 0.061(3) Uani 1 1 d U . . C67 C 0.0340(6) 0.9784(6) 0.1346(4) 0.0383(19) Uani 1 1 d U . . C74 C 0.1124(11) 1.1256(7) 0.1587(6) 0.078(3) Uani 1 1 d U . . H74A H 0.0890 1.1229 0.1971 0.116 Uiso 1 1 calc R . . H74B H 0.1135 1.1847 0.1464 0.116 Uiso 1 1 calc R . . H74C H 0.1824 1.1016 0.1559 0.116 Uiso 1 1 calc R . . C63 C 0.3651(8) 1.0647(7) 0.2269(4) 0.054(2) Uani 1 1 d U . . H63A H 0.3310 1.0092 0.2265 0.082 Uiso 1 1 calc R . . H63B H 0.3199 1.1067 0.2094 0.082 Uiso 1 1 calc R . . H63C H 0.3787 1.0815 0.2651 0.082 Uiso 1 1 calc R . . C54 C 0.3969(12) 0.5868(8) 0.1239(5) 0.084(4) Uani 1 1 d U . . H54A H 0.4465 0.6007 0.0946 0.126 Uiso 1 1 calc R . . H54B H 0.3460 0.5460 0.1099 0.126 Uiso 1 1 calc R . . H54C H 0.4341 0.5620 0.1552 0.126 Uiso 1 1 calc R . . C59 C 0.5093(9) 0.9928(10) 0.0369(4) 0.084(4) Uani 1 1 d U . . H59A H 0.5140 1.0498 0.0211 0.126 Uiso 1 1 calc R . . H59B H 0.4378 0.9722 0.0339 0.126 Uiso 1 1 calc R . . H59C H 0.5558 0.9545 0.0169 0.126 Uiso 1 1 calc R . . C52 C 0.3819(7) 0.7359(6) 0.0481(4) 0.042(2) Uani 1 1 d U . . H52A H 0.3640 0.7851 0.0253 0.063 Uiso 1 1 calc R . . H52B H 0.3902 0.6860 0.0245 0.063 Uiso 1 1 calc R . . H52C H 0.4469 0.7470 0.0677 0.063 Uiso 1 1 calc R . . C114 C 0.4693(8) 0.4351(5) 0.3036(3) 0.040(2) Uani 1 1 d U . . C116 C 0.0399(8) 0.4131(7) 0.3765(4) 0.055(2) Uani 1 1 d U . . C32 C 0.3642(8) 0.4272(7) 0.2736(4) 0.054(2) Uani 1 1 d U . . H32A H 0.3749 0.4009 0.2375 0.081 Uiso 1 1 calc R . . H32B H 0.3340 0.4837 0.2687 0.081 Uiso 1 1 calc R . . H32C H 0.3170 0.3921 0.2956 0.081 Uiso 1 1 calc R . . C117 C -0.0133(7) 0.5449(7) 0.3084(4) 0.051(2) Uani 1 1 d U . . C30 C 0.5321(8) 0.5003(7) 0.2730(4) 0.048(2) Uani 1 1 d U . . H30A H 0.6051 0.4955 0.2837 0.071 Uiso 1 1 calc R . . H30B H 0.5065 0.5571 0.2821 0.071 Uiso 1 1 calc R . . H30C H 0.5254 0.4907 0.2332 0.071 Uiso 1 1 calc R . . C35 C 0.5730(7) 0.5865(9) 0.3859(5) 0.068(3) Uani 1 1 d U . . H35A H 0.5103 0.6215 0.3834 0.101 Uiso 1 1 calc R . . H35B H 0.6075 0.5850 0.3499 0.101 Uiso 1 1 calc R . . H35C H 0.6201 0.6107 0.4134 0.101 Uiso 1 1 calc R . . C40 C 0.0126(9) 0.6383(8) 0.2991(5) 0.074(3) Uani 1 1 d U . . H40A H 0.0073 0.6514 0.2597 0.110 Uiso 1 1 calc R . . H40B H 0.0834 0.6497 0.3118 0.110 Uiso 1 1 calc R . . H40C H -0.0363 0.6737 0.3197 0.110 Uiso 1 1 calc R . . C44 C 0.0764(9) 0.4007(8) 0.4380(5) 0.067(3) Uani 1 1 d U . . H44A H 0.0925 0.3408 0.4444 0.101 Uiso 1 1 calc R . . H44B H 0.0210 0.4185 0.4631 0.101 Uiso 1 1 calc R . . H44C H 0.1385 0.4349 0.4447 0.101 Uiso 1 1 calc R . . C113 C 0.5442(8) 0.4998(8) 0.4024(4) 0.057(2) Uani 1 1 d U . . N1 N 0.2541(5) 0.5523(4) 0.4582(3) 0.0280(15) Uani 1 1 d U . . C120 C 0.3352(10) 0.8274(6) 0.3588(4) 0.058(3) Uani 1 1 d U . . C119 C 0.1977(9) 0.8095(7) 0.4412(5) 0.062(3) Uani 1 1 d U . . C28 C 0.3951(10) 0.3880(6) 0.3979(4) 0.063(3) Uani 1 1 d U . . H28A H 0.3594 0.4087 0.4309 0.095 Uiso 1 1 calc R . . H28B H 0.4488 0.3473 0.4086 0.095 Uiso 1 1 calc R . . H28C H 0.3450 0.3603 0.3735 0.095 Uiso 1 1 calc R . . C72 C 0.0222(12) 0.9967(10) 0.2419(5) 0.087(4) Uani 1 1 d U . . H72A H -0.0095 1.0531 0.2425 0.130 Uiso 1 1 calc R . . H72B H 0.0978 1.0023 0.2393 0.130 Uiso 1 1 calc R . . H72C H 0.0042 0.9663 0.2758 0.130 Uiso 1 1 calc R . . C38 C -0.0136(6) 0.5576(7) 0.4124(4) 0.049(2) Uani 1 1 d U . . H38A H 0.0389 0.5683 0.4408 0.073 Uiso 1 1 calc R . . H38B H -0.0695 0.5230 0.4280 0.073 Uiso 1 1 calc R . . H38C H -0.0421 0.6116 0.3994 0.073 Uiso 1 1 calc R . . C50 C 0.0991(9) 0.6932(8) 0.0962(7) 0.089(4) Uani 1 1 d U . . H50A H 0.0410 0.7114 0.0730 0.134 Uiso 1 1 calc R . . H50B H 0.1112 0.7355 0.1251 0.134 Uiso 1 1 calc R . . H50C H 0.0827 0.6385 0.1132 0.134 Uiso 1 1 calc R . . C34 C 0.5111(9) 0.5009(9) 0.4635(4) 0.071(3) Uani 1 1 d U . . H34A H 0.5664 0.5261 0.4859 0.106 Uiso 1 1 calc R . . H34B H 0.4981 0.4428 0.4760 0.106 Uiso 1 1 calc R . . H34C H 0.4476 0.5345 0.4676 0.106 Uiso 1 1 calc R . . C49 C 0.1820(9) 0.7325(7) 0.0053(5) 0.068(3) Uani 1 1 d U . . H49A H 0.1117 0.7221 -0.0085 0.102 Uiso 1 1 calc R . . H49B H 0.2327 0.7124 -0.0219 0.102 Uiso 1 1 calc R . . H49C H 0.1917 0.7933 0.0114 0.102 Uiso 1 1 calc R . . C26 C 0.1827(10) 0.7591(8) 0.4950(5) 0.074(3) Uani 1 1 d U . . H26A H 0.1854 0.6983 0.4869 0.110 Uiso 1 1 calc R . . H26B H 0.1152 0.7732 0.5112 0.110 Uiso 1 1 calc R . . H26C H 0.2380 0.7738 0.5210 0.110 Uiso 1 1 calc R . . C31 C 0.5187(10) 0.3467(6) 0.2997(4) 0.063(3) Uani 1 1 d U . . H31A H 0.5360 0.3345 0.2612 0.095 Uiso 1 1 calc R . . H31B H 0.4697 0.3042 0.3134 0.095 Uiso 1 1 calc R . . H31C H 0.5820 0.3452 0.3221 0.095 Uiso 1 1 calc R . . C20 C 0.3961(10) 0.9067(7) 0.3769(5) 0.073(3) Uani 1 1 d U . . H20A H 0.4637 0.9074 0.3584 0.110 Uiso 1 1 calc R . . H20B H 0.4063 0.9053 0.4169 0.110 Uiso 1 1 calc R . . H20C H 0.3569 0.9576 0.3668 0.110 Uiso 1 1 calc R . . C36 C 0.6411(10) 0.4389(11) 0.3988(5) 0.093(5) Uani 1 1 d U . . H36A H 0.6917 0.4546 0.4272 0.140 Uiso 1 1 calc R . . H36B H 0.6732 0.4439 0.3623 0.140 Uiso 1 1 calc R . . H36C H 0.6187 0.3802 0.4047 0.140 Uiso 1 1 calc R . . C61 C 0.6394(9) 1.0536(11) 0.1004(5) 0.098(5) Uani 1 1 d U . . H61A H 0.6923 1.0318 0.0751 0.146 Uiso 1 1 calc R . . H61B H 0.6670 1.0540 0.1381 0.146 Uiso 1 1 calc R . . H61C H 0.6205 1.1115 0.0896 0.146 Uiso 1 1 calc R . . C46 C -0.0706(10) 0.3722(8) 0.3734(5) 0.085(4) Uani 1 1 d U . . H46A H -0.0782 0.3422 0.3383 0.128 Uiso 1 1 calc R . . H46B H -0.1234 0.4167 0.3760 0.128 Uiso 1 1 calc R . . H46C H -0.0793 0.3322 0.4039 0.128 Uiso 1 1 calc R . . C21 C 0.2479(14) 0.8534(10) 0.3195(6) 0.114(5) Uani 1 1 d U . . H21A H 0.2059 0.8980 0.3366 0.171 Uiso 1 1 calc R . . H21B H 0.2040 0.8041 0.3116 0.171 Uiso 1 1 calc R . . H21C H 0.2779 0.8746 0.2850 0.171 Uiso 1 1 calc R . . C42 C 0.0254(11) 0.4951(9) 0.2590(5) 0.083(4) Uani 1 1 d U . . H42A H 0.0090 0.5260 0.2251 0.125 Uiso 1 1 calc R . . H42B H -0.0084 0.4395 0.2583 0.125 Uiso 1 1 calc R . . H42C H 0.1007 0.4875 0.2619 0.125 Uiso 1 1 calc R . . C18 C 0.3810(7) 0.7577(6) 0.4506(3) 0.038(2) Uani 1 1 d U . . H18A H 0.3670 0.7072 0.4729 0.057 Uiso 1 1 calc R . . H18B H 0.3856 0.8074 0.4747 0.057 Uiso 1 1 calc R . . H18C H 0.4467 0.7504 0.4308 0.057 Uiso 1 1 calc R . . C25 C 0.0932(10) 0.7953(10) 0.4076(8) 0.110(5) Uani 1 1 d U . . H25A H 0.0844 0.7348 0.3999 0.164 Uiso 1 1 calc R . . H25B H 0.0967 0.8267 0.3728 0.164 Uiso 1 1 calc R . . H25C H 0.0343 0.8158 0.4294 0.164 Uiso 1 1 calc R . . C22 C 0.4156(10) 0.7706(8) 0.3267(4) 0.073(3) Uani 1 1 d U . . H22A H 0.4255 0.7932 0.2895 0.110 Uiso 1 1 calc R . . H22B H 0.3892 0.7125 0.3244 0.110 Uiso 1 1 calc R . . H22C H 0.4820 0.7708 0.3464 0.110 Uiso 1 1 calc R . . C45 C 0.1191(11) 0.3646(8) 0.3423(5) 0.076(3) Uani 1 1 d U . . H45A H 0.1831 0.3979 0.3395 0.114 Uiso 1 1 calc R . . H45B H 0.0911 0.3545 0.3053 0.114 Uiso 1 1 calc R . . H45C H 0.1341 0.3102 0.3601 0.114 Uiso 1 1 calc R . . N7 N 0.2571(8) 0.4541(8) 0.6126(5) 0.081(3) Uani 1 1 d DU . . C24 C 0.2063(9) 0.9027(7) 0.4575(6) 0.072(3) Uani 1 1 d U . . H24A H 0.1653 0.9129 0.4909 0.108 Uiso 1 1 calc R . . H24B H 0.1799 0.9381 0.4274 0.108 Uiso 1 1 calc R . . H24C H 0.2791 0.9168 0.4646 0.108 Uiso 1 1 calc R . . C41 C -0.1334(8) 0.5393(8) 0.3081(6) 0.083(4) Uani 1 1 d U . . H41A H -0.1615 0.5736 0.3382 0.124 Uiso 1 1 calc R . . H41B H -0.1546 0.4801 0.3130 0.124 Uiso 1 1 calc R . . H41C H -0.1599 0.5605 0.2728 0.124 Uiso 1 1 calc R . . C1 C 0.2404(10) 0.8975(7) 0.8233(5) 0.067(3) Uani 1 1 d U . . H1A H 0.1794 0.9227 0.8046 0.080 Uiso 1 1 calc R . . H1B H 0.3032 0.9186 0.8042 0.080 Uiso 1 1 calc R . . N6 N 0.2428(8) 0.9299(8) 0.8843(4) 0.075(2) Uani 1 1 d U . . C9 C 0.2557(10) 1.0341(9) 0.8854(5) 0.071(3) Uani 1 1 d U . . H9A H 0.3177 1.0484 0.8631 0.086 Uiso 1 1 calc R . . H9B H 0.1950 1.0585 0.8661 0.086 Uiso 1 1 calc R . . C6 C 0.4310(11) 0.8763(14) 0.8975(6) 0.117(6) Uani 1 1 d U . . H6A H 0.4246 0.8501 0.8605 0.140 Uiso 1 1 calc R . . H6B H 0.4522 0.9355 0.8902 0.140 Uiso 1 1 calc R . . C4 C 0.2076(10) 0.7038(8) 0.7409(4) 0.067(3) Uani 1 1 d U . . H4A H 0.2606 0.6702 0.7599 0.100 Uiso 1 1 calc R . . H4B H 0.2219 0.7041 0.7012 0.100 Uiso 1 1 calc R . . H4C H 0.1391 0.6788 0.7475 0.100 Uiso 1 1 calc R . . C5 C 0.3294(10) 0.8858(9) 0.9126(6) 0.076(3) Uani 1 1 d U . . H5A H 0.3322 0.9119 0.9496 0.091 Uiso 1 1 calc R . . H5B H 0.3039 0.8273 0.9183 0.091 Uiso 1 1 calc R . . C13 C 0.1451(10) 0.9053(10) 0.9170(6) 0.081(3) Uani 1 1 d U . . H13A H 0.1549 0.9213 0.9561 0.098 Uiso 1 1 calc R . . H13B H 0.1363 0.8430 0.9154 0.098 Uiso 1 1 calc R . . C10 C 0.2647(12) 1.0740(10) 0.9332(6) 0.094(4) Uani 1 1 d U . . H10A H 0.3223 1.0478 0.9541 0.113 Uiso 1 1 calc R . . H10B H 0.2002 1.0647 0.9546 0.113 Uiso 1 1 calc R . . C2 C 0.2354(11) 0.7998(7) 0.8163(5) 0.071(3) Uani 1 1 d U . . H2A H 0.3033 0.7737 0.8249 0.085 Uiso 1 1 calc R . . H2B H 0.1821 0.7751 0.8409 0.085 Uiso 1 1 calc R . . C3 C 0.2093(10) 0.7863(8) 0.7608(4) 0.069(3) Uani 1 1 d U . . H3A H 0.1397 0.8111 0.7546 0.083 Uiso 1 1 calc R . . H3B H 0.2588 0.8190 0.7380 0.083 Uiso 1 1 calc R . . C8 C 0.6256(10) 0.8512(9) 0.9054(9) 0.118(6) Uani 1 1 d U . . H8A H 0.6401 0.8431 0.8660 0.177 Uiso 1 1 calc R . . H8B H 0.6622 0.8078 0.9268 0.177 Uiso 1 1 calc R . . H8C H 0.6495 0.9075 0.9168 0.177 Uiso 1 1 calc R . . C7 C 0.5141(10) 0.8440(10) 0.9151(7) 0.101(5) Uani 1 1 d U . . H7A H 0.5016 0.7826 0.9100 0.122 Uiso 1 1 calc R . . H7B H 0.5088 0.8533 0.9554 0.122 Uiso 1 1 calc R . . C12 C 0.2850(14) 1.2260(10) 0.9847(7) 0.120(6) Uani 1 1 d U . . H12A H 0.2491 1.1956 1.0144 0.180 Uiso 1 1 calc R . . H12B H 0.2495 1.2798 0.9776 0.180 Uiso 1 1 calc R . . H12C H 0.3568 1.2372 0.9958 0.180 Uiso 1 1 calc R . . C11 C 0.2844(18) 1.1690(11) 0.9296(9) 0.146(7) Uani 1 1 d U . . H11A H 0.2312 1.1930 0.9047 0.176 Uiso 1 1 calc R . . H11B H 0.3523 1.1769 0.9113 0.176 Uiso 1 1 calc R . . C14 C 0.0456(14) 0.9481(12) 0.8950(9) 0.126(6) Uani 1 1 d U . . H14A H 0.0304 0.9983 0.9181 0.151 Uiso 1 1 calc R . . H14B H 0.0591 0.9686 0.8570 0.151 Uiso 1 1 calc R . . C99 C 0.2034(18) 0.3901(17) 0.6582(9) 0.069(5) Uani 0.50 1 d PU A 1 H99A H 0.1666 0.4249 0.6859 0.082 Uiso 0.50 1 calc PR A 1 H99B H 0.1510 0.3549 0.6391 0.082 Uiso 0.50 1 calc PR A 1 C39 C 0.314(2) 0.290(2) 0.7363(11) 0.041(6) Uani 0.33 1 d PU A 1 H39A H 0.2875 0.3270 0.7661 0.049 Uiso 0.33 1 calc PR A 1 H39B H 0.3894 0.2998 0.7353 0.049 Uiso 0.33 1 calc PR A 1 C43 C 0.306(2) 0.2085(19) 0.7598(10) 0.062(6) Uani 0.50 1 d PU A 1 H43A H 0.2776 0.1690 0.7326 0.093 Uiso 0.50 1 calc PR A 1 H43B H 0.2604 0.2106 0.7921 0.093 Uiso 0.50 1 calc PR A 1 H43C H 0.3753 0.1893 0.7711 0.093 Uiso 0.50 1 calc PR A 1 C84 C 0.249(2) 0.383(2) 0.5648(12) 0.077(5) Uani 0.50 1 d PDU A 1 H84A H 0.1862 0.3491 0.5724 0.092 Uiso 0.50 1 calc PR A 1 H84B H 0.2369 0.4132 0.5297 0.092 Uiso 0.50 1 calc PR A 1 C87 C 0.330(2) 0.3249(17) 0.5549(11) 0.083(5) Uani 0.50 1 d PDU A 1 H87A H 0.3584 0.3040 0.5901 0.100 Uiso 0.50 1 calc PR A 1 H87B H 0.3860 0.3523 0.5337 0.100 Uiso 0.50 1 calc PR A 1 C91 C 0.221(2) 0.1779(16) 0.5081(15) 0.117(10) Uani 0.50 1 d PDU A 1 H91A H 0.1658 0.1695 0.5355 0.176 Uiso 0.50 1 calc PR A 1 H91B H 0.2654 0.1277 0.5070 0.176 Uiso 0.50 1 calc PR A 1 H91C H 0.1895 0.1868 0.4717 0.176 Uiso 0.50 1 calc PR A 1 C93 C 0.1457(19) 0.4849(18) 0.5802(11) 0.071(5) Uani 0.50 1 d PU A 1 H93A H 0.1663 0.5182 0.5474 0.085 Uiso 0.50 1 calc PR A 1 H93B H 0.1113 0.4329 0.5665 0.085 Uiso 0.50 1 calc PR A 1 C94 C 0.056(2) 0.541(2) 0.6140(13) 0.074(6) Uani 0.50 1 d PU A 1 C96 C -0.034(3) 0.612(2) 0.6163(15) 0.108(9) Uani 0.50 1 d PDU A 1 H96A H -0.0084 0.6543 0.6430 0.130 Uiso 0.50 1 calc PR A 1 H96B H -0.0316 0.6395 0.5798 0.130 Uiso 0.50 1 calc PR A 1 C89 C 0.286(3) 0.256(2) 0.5238(15) 0.089(8) Uani 0.50 1 d PDU A 1 H89A H 0.3533 0.2315 0.5122 0.107 Uiso 0.50 1 calc PR A 1 H89B H 0.2650 0.2906 0.4917 0.107 Uiso 0.50 1 calc PR A 1 C111 C 0.3335(15) 0.5120(14) 0.5866(8) 0.053(4) Uani 0.50 1 d PU A 1 C79 C 0.335(2) 0.5970(17) 0.6243(11) 0.077(5) Uani 0.50 1 d PU A 1 H79A H 0.2647 0.6216 0.6263 0.093 Uiso 0.50 1 calc PR A 1 H79B H 0.3579 0.5828 0.6622 0.093 Uiso 0.50 1 calc PR A 1 C81 C 0.4127(18) 0.6637(17) 0.5980(10) 0.069(5) Uani 0.50 1 d PU A 1 H81A H 0.4048 0.6653 0.5574 0.083 Uiso 0.50 1 calc PR A 1 H81B H 0.3994 0.7211 0.6128 0.083 Uiso 0.50 1 calc PR A 1 C82 C 0.521(2) 0.6338(18) 0.6137(14) 0.079(7) Uani 0.50 1 d PU A 1 H82A H 0.5239 0.6232 0.6535 0.118 Uiso 0.50 1 calc PR A 1 H82B H 0.5719 0.6775 0.6039 0.118 Uiso 0.50 1 calc PR A 1 H82C H 0.5373 0.5814 0.5938 0.118 Uiso 0.50 1 calc PR A 1 C97 C -0.149(3) 0.601(4) 0.629(2) 0.183(19) Uiso 0.50 1 d PDU A 1 C33 C 0.279(2) 0.331(2) 0.6882(14) 0.060(6) Uani 0.50 1 d PU A 1 H33A H 0.2738 0.2817 0.6635 0.072 Uiso 0.50 1 calc PR A 1 H33B H 0.3446 0.3589 0.6773 0.072 Uiso 0.50 1 calc PR A 1 C83 C 0.5159(14) 0.6574(10) 0.5768(8) 0.033(4) Uani 0.50 1 d PU A 2 H83A H 0.5035 0.6531 0.5371 0.049 Uiso 0.50 1 calc PR A 2 H83B H 0.5880 0.6420 0.5848 0.049 Uiso 0.50 1 calc PR A 2 H83C H 0.5030 0.7157 0.5890 0.049 Uiso 0.50 1 calc PR A 2 C37 C 0.262(3) 0.260(2) 0.7258(15) 0.057(7) Uani 0.33 1 d PU A 2 H37A H 0.2529 0.2089 0.7026 0.068 Uiso 0.33 1 calc PR A 2 H37B H 0.3377 0.2684 0.7269 0.068 Uiso 0.33 1 calc PR A 2 C85 C 0.285(2) 0.4203(18) 0.5642(10) 0.076(5) Uani 0.50 1 d PDU A 2 H85A H 0.3569 0.4349 0.5535 0.091 Uiso 0.50 1 calc PR A 2 H85B H 0.2363 0.4348 0.5340 0.091 Uiso 0.50 1 calc PR A 2 C17 C 0.252(4) 0.225(2) 0.772(2) 0.049(10) Uani 0.25 1 d PU A 2 H17A H 0.2016 0.2563 0.7942 0.073 Uiso 0.25 1 calc PR A 2 H17B H 0.3191 0.2241 0.7907 0.073 Uiso 0.25 1 calc PR A 2 H17C H 0.2274 0.1666 0.7667 0.073 Uiso 0.25 1 calc PR A 2 C86 C 0.274(2) 0.3283(17) 0.5836(11) 0.076(5) Uani 0.50 1 d PDU A 2 H86A H 0.3426 0.3036 0.5920 0.091 Uiso 0.50 1 calc PR A 2 H86B H 0.2300 0.3252 0.6171 0.091 Uiso 0.50 1 calc PR A 2 C88 C 0.231(2) 0.289(2) 0.5435(11) 0.087(6) Uani 0.50 1 d PDU A 2 H88A H 0.1796 0.3277 0.5264 0.104 Uiso 0.50 1 calc PR A 2 H88B H 0.1924 0.2403 0.5587 0.104 Uiso 0.50 1 calc PR A 2 C90 C 0.298(3) 0.259(2) 0.5007(13) 0.084(9) Uani 0.50 1 d PDU A 2 H90A H 0.3360 0.2086 0.5140 0.126 Uiso 0.50 1 calc PR A 2 H90B H 0.3480 0.3029 0.4906 0.126 Uiso 0.50 1 calc PR A 2 H90C H 0.2570 0.2431 0.4683 0.126 Uiso 0.50 1 calc PR A 2 C92 C 0.1455(18) 0.4848(17) 0.6284(12) 0.073(5) Uani 0.50 1 d PU A 2 H92A H 0.1515 0.5245 0.6598 0.087 Uiso 0.50 1 calc PR A 2 H92B H 0.1054 0.4351 0.6413 0.087 Uiso 0.50 1 calc PR A 2 C95 C 0.083(2) 0.5286(18) 0.5828(14) 0.069(5) Uani 0.50 1 d PU A 2 H95A H 0.1311 0.5644 0.5609 0.083 Uiso 0.50 1 calc PR A 2 H95B H 0.0548 0.4847 0.5579 0.083 Uiso 0.50 1 calc PR A 2 C80 C 0.4405(12) 0.5951(9) 0.6084(7) 0.029(3) Uani 0.50 1 d PU A 2 H80A H 0.4652 0.5362 0.6037 0.034 Uiso 0.50 1 calc PR A 2 H80B H 0.4416 0.6086 0.6482 0.034 Uiso 0.50 1 calc PR A 2 C109 C 0.009(3) 0.5747(19) 0.6000(13) 0.087(7) Uani 0.50 1 d PDU A 2 C77 C 0.2420(11) 0.5659(10) 0.6189(6) 0.021(3) Uiso 0.50 1 d PU A 2 H77A H 0.1746 0.5844 0.6036 0.025 Uiso 0.50 1 calc PR A 2 H77B H 0.2459 0.5835 0.6581 0.025 Uiso 0.50 1 calc PR A 2 C78 C 0.3293(12) 0.6022(10) 0.5869(7) 0.026(3) Uiso 0.50 1 d PU A 2 H78A H 0.3144 0.6632 0.5816 0.031 Uiso 0.50 1 calc PR A 2 H78B H 0.3278 0.5756 0.5499 0.031 Uiso 0.50 1 calc PR A 2 C27 C 0.3059(17) 0.3989(19) 0.6551(10) 0.076(6) Uani 0.50 1 d PU A 2 H27A H 0.3306 0.4358 0.6855 0.091 Uiso 0.50 1 calc PR A 2 H27B H 0.3678 0.3721 0.6384 0.091 Uiso 0.50 1 calc PR A 2 C98 C -0.0621(18) 0.629(2) 0.5610(13) 0.113(11) Uani 0.50 1 d PDU A 2 H98A H -0.0313 0.6302 0.5241 0.169 Uiso 0.50 1 calc PR A 2 H98B H -0.0680 0.6863 0.5755 0.169 Uiso 0.50 1 calc PR A 2 H98C H -0.1311 0.6027 0.5590 0.169 Uiso 0.50 1 calc PR A 2 C29 C 0.237(2) 0.326(2) 0.6814(13) 0.056(6) Uani 0.50 1 d PU A 2 H29A H 0.1748 0.3559 0.6954 0.067 Uiso 0.50 1 calc PR A 2 H29B H 0.2131 0.2925 0.6494 0.067 Uiso 0.50 1 calc PR A 2 C214 C 0.1389(14) 0.5852(13) 0.5859(9) 0.048(4) Uani 0.50 1 d PU B 3 C16 C -0.0860(18) 0.8561(18) 0.9288(11) 0.189(12) Uani 1 1 d U . . H16A H -0.0372 0.8500 0.9595 0.284 Uiso 1 1 calc R . . H16B H -0.1060 0.7998 0.9154 0.284 Uiso 1 1 calc R . . H16C H -0.1479 0.8865 0.9414 0.284 Uiso 1 1 calc R . . C15 C -0.0474(14) 0.8932(17) 0.8940(12) 0.171(9) Uani 1 1 d U . . H15A H -0.1031 0.9294 0.8788 0.205 Uiso 1 1 calc R . . H15B H -0.0325 0.8503 0.8652 0.205 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 N2 0.024(3) 0.033(4) 0.027(3) -0.006(3) 0.004(3) 0.003(3) O6 0.021(3) 0.043(3) 0.033(3) -0.004(3) 0.005(2) 0.017(2) O5 0.024(3) 0.038(3) 0.019(3) 0.003(2) -0.002(2) -0.013(2) O4 0.026(3) 0.021(3) 0.044(4) -0.005(2) 0.000(3) 0.000(2) V1 0.0205(6) 0.0240(7) 0.0223(7) -0.0014(6) 0.0007(5) -0.0013(6) O1 0.023(3) 0.029(3) 0.030(3) -0.004(2) -0.003(2) -0.006(2) O3 0.022(3) 0.038(3) 0.028(3) 0.004(3) -0.002(2) -0.010(2) O2 0.028(3) 0.028(3) 0.024(3) 0.004(2) 0.004(2) 0.008(2) C115 0.028(4) 0.044(4) 0.044(4) 0.012(4) -0.003(3) -0.017(3) C118 0.048(5) 0.022(4) 0.033(4) -0.004(3) -0.007(3) 0.000(3) C112 0.055(5) 0.029(4) 0.019(4) 0.004(3) 0.007(3) 0.021(3) V2 0.0179(6) 0.0219(7) 0.0229(7) -0.0021(6) 0.0026(5) 0.0010(5) C47 0.037(4) 0.023(4) 0.039(4) 0.002(3) 0.013(3) 0.007(3) C66 0.105(9) 0.055(6) 0.024(5) 0.013(4) -0.003(5) -0.031(5) C60 0.029(5) 0.105(7) 0.075(7) -0.040(6) 0.002(5) -0.005(5) C62 0.056(5) 0.041(5) 0.036(4) -0.001(4) -0.007(4) -0.014(4) C58 0.050(5) 0.035(4) 0.027(4) 0.008(3) -0.002(3) -0.024(3) C65 0.046(5) 0.079(6) 0.023(5) 0.018(5) -0.003(4) -0.015(5) C69 0.057(6) 0.065(6) 0.064(5) 0.028(5) 0.034(5) 0.027(5) C48 0.052(5) 0.040(5) 0.079(7) -0.027(4) 0.005(4) -0.011(4) C64 0.103(9) 0.062(6) 0.045(6) -0.009(5) -0.018(6) -0.035(6) C53 0.096(8) 0.035(5) 0.036(5) 0.009(4) 0.019(4) 0.024(5) C73 0.059(6) 0.037(4) 0.070(6) 0.020(4) 0.025(5) 0.024(4) C56 0.165(12) 0.029(5) 0.068(8) 0.009(5) 0.065(8) 0.004(6) C51 0.091(9) 0.038(5) 0.104(10) -0.030(5) 0.037(7) -0.012(6) C68 0.029(5) 0.077(7) 0.069(6) 0.018(5) -0.006(4) -0.007(5) C110 0.060(7) 0.057(7) 0.064(6) 0.023(5) 0.024(5) 0.021(5) C71 0.053(5) 0.074(8) 0.115(10) 0.044(7) 0.047(6) 0.033(5) C70 0.051(6) 0.080(6) 0.073(7) 0.047(5) 0.035(6) 0.033(6) C75 0.070(6) 0.076(8) 0.076(8) 0.043(6) 0.027(6) 0.050(6) C55 0.080(7) 0.071(7) 0.041(6) 0.004(5) -0.016(5) 0.041(5) C57 0.038(5) 0.115(7) 0.029(5) -0.004(5) 0.007(4) -0.041(5) C67 0.025(4) 0.044(4) 0.046(4) 0.024(4) 0.010(3) 0.019(3) C74 0.100(8) 0.046(6) 0.087(8) 0.012(6) -0.002(7) 0.017(6) C63 0.077(6) 0.054(6) 0.033(5) -0.015(5) -0.004(4) 0.001(5) C54 0.144(12) 0.055(6) 0.052(7) 0.004(5) 0.011(7) 0.063(7) C59 0.046(6) 0.174(13) 0.032(5) -0.019(6) 0.010(4) -0.054(7) C52 0.054(5) 0.040(5) 0.032(5) -0.011(4) 0.012(4) 0.000(4) C114 0.063(5) 0.028(4) 0.031(4) -0.003(3) 0.010(4) 0.017(4) C116 0.059(6) 0.043(5) 0.065(6) 0.028(5) -0.015(5) -0.016(4) C32 0.080(6) 0.051(6) 0.031(5) -0.009(4) 0.001(4) 0.005(5) C117 0.031(4) 0.057(5) 0.066(5) 0.028(4) -0.020(4) -0.022(4) C30 0.062(6) 0.063(6) 0.018(4) 0.014(4) 0.009(4) 0.021(5) C35 0.026(5) 0.115(7) 0.061(6) -0.023(6) -0.004(5) -0.013(5) C40 0.064(7) 0.069(6) 0.088(8) 0.044(6) -0.037(6) -0.034(6) C44 0.060(7) 0.068(8) 0.074(6) 0.028(6) -0.025(5) -0.030(6) C113 0.048(5) 0.100(7) 0.024(4) 0.004(5) -0.002(4) 0.036(5) N1 0.019(3) 0.036(4) 0.029(3) 0.004(3) 0.003(3) 0.000(3) C120 0.107(8) 0.034(5) 0.032(5) 0.005(4) -0.030(4) -0.016(5) C119 0.057(6) 0.041(5) 0.088(7) -0.023(5) -0.008(5) 0.026(5) C28 0.116(9) 0.044(5) 0.030(5) 0.021(4) 0.021(6) 0.027(5) C72 0.105(9) 0.111(9) 0.044(6) 0.017(6) 0.036(6) 0.031(8) C38 0.016(4) 0.065(6) 0.066(5) 0.018(5) 0.012(4) 0.004(4) C50 0.043(6) 0.053(7) 0.171(12) -0.045(8) 0.040(7) -0.017(5) C34 0.066(7) 0.115(10) 0.031(5) -0.017(5) -0.005(4) 0.038(7) C49 0.067(7) 0.054(6) 0.083(7) -0.031(5) -0.041(5) 0.006(5) C26 0.074(8) 0.064(6) 0.082(7) -0.035(5) 0.041(6) -0.016(6) C31 0.107(9) 0.040(5) 0.043(6) -0.004(4) 0.024(6) 0.033(6) C20 0.102(9) 0.040(5) 0.078(8) 0.019(5) -0.015(6) -0.029(6) C36 0.063(7) 0.170(12) 0.048(7) -0.023(8) -0.004(5) 0.059(8) C61 0.059(7) 0.185(13) 0.049(7) -0.005(8) -0.004(5) -0.088(9) C46 0.094(7) 0.080(8) 0.081(9) 0.044(7) -0.051(6) -0.060(7) C21 0.189(13) 0.079(10) 0.075(9) 0.028(8) -0.087(10) -0.015(9) C42 0.104(9) 0.100(9) 0.045(6) -0.001(6) -0.038(6) -0.034(8) C18 0.043(5) 0.040(5) 0.030(4) -0.007(4) -0.006(4) -0.008(4) C25 0.055(7) 0.102(11) 0.171(13) -0.070(10) -0.034(8) 0.024(7) C22 0.109(8) 0.079(7) 0.032(6) 0.002(5) 0.026(5) -0.061(6) C45 0.104(8) 0.051(6) 0.073(7) 0.008(6) -0.027(6) 0.004(6) N7 0.056(5) 0.110(6) 0.077(6) 0.050(5) 0.026(5) 0.031(5) C24 0.069(7) 0.044(5) 0.103(10) -0.023(5) -0.002(6) 0.011(5) C41 0.041(5) 0.082(8) 0.124(11) 0.040(7) -0.043(6) -0.033(5) C1 0.072(7) 0.068(6) 0.061(5) 0.013(5) -0.005(5) 0.002(6) N6 0.076(5) 0.086(6) 0.063(5) 0.010(4) 0.001(4) 0.012(5) C9 0.070(7) 0.086(6) 0.059(6) 0.049(5) -0.030(6) -0.024(6) C6 0.072(6) 0.217(17) 0.062(8) -0.032(10) -0.023(6) 0.035(9) C4 0.073(8) 0.087(7) 0.040(6) 0.005(5) 0.015(6) 0.018(7) C5 0.060(5) 0.084(8) 0.085(8) -0.010(7) -0.012(6) 0.016(6) C13 0.075(6) 0.095(9) 0.074(7) 0.004(7) 0.000(5) -0.028(6) C10 0.100(10) 0.094(7) 0.088(8) 0.029(6) 0.012(8) -0.004(9) C2 0.102(9) 0.064(6) 0.047(5) 0.011(5) 0.008(6) 0.004(7) C3 0.075(8) 0.089(7) 0.042(6) 0.001(5) 0.003(6) -0.010(7) C8 0.061(6) 0.066(9) 0.23(2) 0.038(11) -0.006(10) -0.024(7) C7 0.053(6) 0.097(10) 0.155(13) -0.060(10) -0.007(7) 0.018(7) C12 0.140(15) 0.082(9) 0.138(13) 0.039(7) 0.070(12) 0.007(10) C11 0.184(18) 0.081(8) 0.174(15) -0.009(9) 0.087(14) 0.007(11) C14 0.110(8) 0.118(13) 0.149(14) 0.022(11) 0.010(10) 0.059(9) C99 0.061(11) 0.096(13) 0.048(9) 0.023(8) -0.007(8) -0.002(9) C39 0.045(15) 0.058(12) 0.019(10) -0.034(8) -0.010(10) 0.026(11) C43 0.071(17) 0.082(14) 0.032(12) -0.010(9) 0.006(11) -0.005(14) C84 0.073(13) 0.100(11) 0.056(9) 0.058(8) 0.024(10) 0.009(8) C87 0.069(12) 0.112(12) 0.069(12) 0.039(9) 0.015(10) 0.010(8) C91 0.064(16) 0.078(14) 0.21(3) 0.103(15) -0.034(17) -0.005(12) C93 0.057(8) 0.091(13) 0.065(12) 0.035(10) 0.018(8) 0.000(8) C94 0.046(10) 0.096(13) 0.079(13) 0.032(11) 0.039(10) 0.005(8) C96 0.098(17) 0.115(18) 0.112(17) 0.088(14) 0.031(14) 0.044(12) C89 0.048(14) 0.115(15) 0.10(2) 0.031(14) 0.016(16) 0.006(11) C111 0.037(7) 0.076(8) 0.045(9) 0.027(7) 0.020(7) 0.042(6) C79 0.068(10) 0.094(10) 0.070(12) 0.008(9) -0.011(10) 0.041(8) C81 0.063(11) 0.083(11) 0.061(12) -0.026(10) -0.006(9) 0.026(8) C82 0.073(10) 0.060(15) 0.10(2) -0.031(16) -0.010(14) 0.036(11) C33 0.050(14) 0.073(12) 0.057(11) 0.002(8) -0.015(11) 0.000(11) C83 0.033(9) 0.017(9) 0.048(11) 0.008(8) -0.009(8) -0.010(7) C37 0.089(19) 0.044(13) 0.038(13) 0.002(10) 0.005(13) 0.010(13) C85 0.060(12) 0.116(11) 0.053(8) 0.048(10) 0.000(9) 0.011(11) C17 0.09(3) 0.011(16) 0.049(17) 0.003(13) 0.00(2) 0.015(18) C86 0.065(13) 0.101(10) 0.062(12) 0.042(9) 0.012(10) 0.032(11) C88 0.083(15) 0.100(12) 0.076(13) 0.033(11) 0.008(11) 0.035(11) C90 0.10(2) 0.074(16) 0.076(16) 0.045(12) 0.024(15) 0.033(14) C92 0.051(9) 0.086(13) 0.081(13) 0.020(11) 0.001(9) 0.002(8) C95 0.038(10) 0.064(12) 0.105(14) 0.025(12) 0.000(10) 0.004(8) C80 0.024(8) 0.009(7) 0.053(9) 0.013(6) -0.009(7) 0.006(6) C109 0.090(14) 0.062(14) 0.108(15) 0.053(12) 0.058(11) 0.028(10) C27 0.052(10) 0.120(14) 0.056(9) 0.048(10) -0.010(9) -0.005(9) C98 0.028(12) 0.18(3) 0.13(2) 0.01(2) 0.021(13) 0.057(15) C29 0.053(15) 0.073(12) 0.042(11) 0.014(8) -0.015(11) 0.009(11) C214 0.030(8) 0.040(9) 0.072(11) 0.033(9) 0.009(8) 0.018(8) C16 0.144(18) 0.19(2) 0.23(3) -0.022(19) 0.114(18) 0.030(14) C15 0.062(8) 0.20(2) 0.25(2) 0.054(16) 0.037(11) 0.062(9) _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 N2 V2 1.609(7) . ? O6 C67 1.487(9) . ? O6 V2 1.793(5) . ? O5 C58 1.407(10) . ? O5 V2 1.834(5) . ? O4 C47 1.453(10) . ? O4 V2 1.804(6) . ? V1 N1 1.587(7) . ? V1 O3 1.807(5) . ? V1 O1 1.823(6) . ? V1 O2 1.837(5) . ? O1 C118 1.387(10) . ? O3 C115 1.472(10) . ? O2 C112 1.394(10) . ? C115 C38 1.531(14) . ? C115 C116 1.566(13) . ? C115 C117 1.588(13) . ? C118 C18 1.531(12) . ? C118 C119 1.580(14) . ? C118 C120 1.608(13) . ? C112 C28 1.561(13) . ? C112 C113 1.625(15) . ? C112 C114 1.635(11) . ? C47 C48 1.544(14) . ? C47 C52 1.549(12) . ? C47 C53 1.624(13) . ? C66 C58 1.495(14) . ? C60 C57 1.545(18) . ? C62 C63 1.512(14) . ? C62 C64 1.532(13) . ? C62 C65 1.555(14) . ? C62 C58 1.613(12) . ? C58 C57 1.633(15) . ? C69 C71 1.445(15) . ? C69 C72 1.550(19) . ? C69 C70 1.551(15) . ? C69 C67 1.616(13) . ? C48 C50 1.545(15) . ? C48 C49 1.552(17) . ? C48 C51 1.577(13) . ? C53 C54 1.527(13) . ? C53 C55 1.525(16) . ? C53 C56 1.577(15) . ? C73 C74 1.530(17) . ? C73 C67 1.549(13) . ? C73 C110 1.564(14) . ? C73 C75 1.609(13) . ? C68 C67 1.515(15) . ? C57 C59 1.536(14) . ? C57 C61 1.562(13) . ? C114 C30 1.505(13) . ? C114 C31 1.536(12) . ? C114 C32 1.543(14) . ? C116 C45 1.521(17) . ? C116 C46 1.564(14) . ? C116 C44 1.577(14) . ? C117 C42 1.517(18) . ? C117 C40 1.527(14) . ? C117 C41 1.551(14) . ? C35 C113 1.473(17) . ? C113 C34 1.543(13) . ? C113 C36 1.579(15) . ? C120 C21 1.531(16) . ? C120 C20 1.540(14) . ? C120 C22 1.576(17) . ? C119 C24 1.527(14) . ? C119 C26 1.539(17) . ? C119 C25 1.591(17) . ? N7 C85 1.34(3) . ? N7 C111 1.48(2) . ? N7 C27 1.49(2) . ? N7 C92 1.56(3) . ? N7 C84 1.62(4) . ? N7 C99 1.65(2) . ? N7 C93 1.71(3) . ? N7 C77 1.78(2) . ? C1 C2 1.553(16) . ? C1 N6 1.566(15) . ? N6 C5 1.484(15) . ? N6 C13 1.537(16) . ? N6 C9 1.654(18) . ? C9 C10 1.324(19) . ? C6 C7 1.261(18) . ? C6 C5 1.368(18) . ? C4 C3 1.390(16) . ? C13 C14 1.55(2) . ? C10 C11 1.52(2) . ? C2 C3 1.403(15) . ? C8 C7 1.461(18) . ? C12 C11 1.61(3) . ? C14 C15 1.48(3) . ? C99 C33 1.53(4) . ? C39 C33 1.41(4) . ? C39 C43 1.41(4) . ? C84 C87 1.40(3) . ? C87 C89 1.44(3) . ? C91 C89 1.54(3) . ? C93 C94 1.68(4) . ? C94 C96 1.60(4) . ? C96 C97 1.53(3) . ? C111 C79 1.62(4) . ? C79 C81 1.58(4) . ? C81 C82 1.52(3) . ? C83 C80 1.58(2) . ? C37 C17 1.26(5) . ? C37 C29 1.53(4) . ? C85 C86 1.53(3) . ? C86 C88 1.28(3) . ? C88 C90 1.44(3) . ? C92 C95 1.53(4) . ? C95 C109 1.28(4) . ? C80 C78 1.53(2) . ? C109 C98 1.56(3) . ? C77 C78 1.48(2) . ? C27 C29 1.58(4) . ? C16 C15 1.14(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 C67 O6 V2 146.9(5) . . ? C58 O5 V2 144.6(5) . . ? C47 O4 V2 147.3(5) . . ? N1 V1 O3 109.8(3) . . ? N1 V1 O1 111.2(3) . . ? O3 V1 O1 108.9(3) . . ? N1 V1 O2 109.4(3) . . ? O3 V1 O2 108.2(3) . . ? O1 V1 O2 109.4(3) . . ? C118 O1 V1 148.2(5) . . ? C115 O3 V1 147.9(5) . . ? C112 O2 V1 145.1(5) . . ? O3 C115 C38 107.2(7) . . ? O3 C115 C116 106.8(7) . . ? C38 C115 C116 110.0(8) . . ? O3 C115 C117 102.5(6) . . ? C38 C115 C117 108.5(8) . . ? C116 C115 C117 120.9(8) . . ? O1 C118 C18 109.1(7) . . ? O1 C118 C119 110.1(7) . . ? C18 C118 C119 107.5(7) . . ? O1 C118 C120 106.6(7) . . ? C18 C118 C120 108.7(7) . . ? C119 C118 C120 114.8(8) . . ? O2 C112 C28 108.1(7) . . ? O2 C112 C113 108.3(7) . . ? C28 C112 C113 110.0(8) . . ? O2 C112 C114 105.0(6) . . ? C28 C112 C114 108.0(7) . . ? C113 C112 C114 116.9(7) . . ? N2 V2 O6 111.1(3) . . ? N2 V2 O4 110.0(3) . . ? O6 V2 O4 108.6(3) . . ? N2 V2 O5 109.9(3) . . ? O6 V2 O5 109.4(3) . . ? O4 V2 O5 107.8(3) . . ? O4 C47 C48 108.8(7) . . ? O4 C47 C52 106.7(6) . . ? C48 C47 C52 109.6(8) . . ? O4 C47 C53 103.1(7) . . ? C48 C47 C53 118.9(8) . . ? C52 C47 C53 109.0(7) . . ? C63 C62 C64 107.6(9) . . ? C63 C62 C65 103.8(8) . . ? C64 C62 C65 108.7(8) . . ? C63 C62 C58 108.7(7) . . ? C64 C62 C58 113.3(7) . . ? C65 C62 C58 114.1(8) . . ? O5 C58 C66 112.0(8) . . ? O5 C58 C62 106.3(6) . . ? C66 C58 C62 108.9(8) . . ? O5 C58 C57 104.8(7) . . ? C66 C58 C57 108.9(8) . . ? C62 C58 C57 115.8(7) . . ? C71 C69 C72 105.6(10) . . ? C71 C69 C70 110.0(10) . . ? C72 C69 C70 106.4(10) . . ? C71 C69 C67 114.5(9) . . ? C72 C69 C67 111.9(10) . . ? C70 C69 C67 108.2(8) . . ? C47 C48 C50 111.4(9) . . ? C47 C48 C49 109.6(8) . . ? C50 C48 C49 109.4(11) . . ? C47 C48 C51 113.9(10) . . ? C50 C48 C51 106.9(9) . . ? C49 C48 C51 105.5(9) . . ? C54 C53 C55 110.1(11) . . ? C54 C53 C56 107.9(9) . . ? C55 C53 C56 105.9(9) . . ? C54 C53 C47 111.8(8) . . ? C55 C53 C47 107.8(8) . . ? C56 C53 C47 113.3(10) . . ? C74 C73 C67 115.2(9) . . ? C74 C73 C110 106.3(10) . . ? C67 C73 C110 111.4(9) . . ? C74 C73 C75 109.6(10) . . ? C67 C73 C75 110.4(8) . . ? C110 C73 C75 103.2(8) . . ? C59 C57 C60 107.9(11) . . ? C59 C57 C61 105.8(8) . . ? C60 C57 C61 107.4(11) . . ? C59 C57 C58 107.6(9) . . ? C60 C57 C58 113.7(8) . . ? C61 C57 C58 114.0(10) . . ? O6 C67 C68 106.9(7) . . ? O6 C67 C73 105.5(7) . . ? C68 C67 C73 110.4(8) . . ? O6 C67 C69 103.8(7) . . ? C68 C67 C69 110.4(9) . . ? C73 C67 C69 118.9(8) . . ? C30 C114 C31 111.5(8) . . ? C30 C114 C32 107.1(7) . . ? C31 C114 C32 105.2(8) . . ? C30 C114 C112 111.7(7) . . ? C31 C114 C112 112.9(7) . . ? C32 C114 C112 108.0(7) . . ? C45 C116 C46 112.1(11) . . ? C45 C116 C115 114.1(9) . . ? C46 C116 C115 111.5(9) . . ? C45 C116 C44 104.6(9) . . ? C46 C116 C44 105.4(8) . . ? C115 C116 C44 108.3(9) . . ? C42 C117 C40 108.2(10) . . ? C42 C117 C41 107.1(10) . . ? C40 C117 C41 105.8(9) . . ? C42 C117 C115 111.1(9) . . ? C40 C117 C115 111.7(8) . . ? C41 C117 C115 112.6(8) . . ? C35 C113 C34 108.7(10) . . ? C35 C113 C36 110.6(11) . . ? C34 C113 C36 106.2(8) . . ? C35 C113 C112 111.9(8) . . ? C34 C113 C112 107.1(9) . . ? C36 C113 C112 112.0(10) . . ? C21 C120 C20 109.5(10) . . ? C21 C120 C22 109.1(10) . . ? C20 C120 C22 105.5(10) . . ? C21 C120 C118 111.9(11) . . ? C20 C120 C118 114.3(8) . . ? C22 C120 C118 106.1(7) . . ? C24 C119 C26 106.8(10) . . ? C24 C119 C118 116.6(10) . . ? C26 C119 C118 108.3(8) . . ? C24 C119 C25 109.2(9) . . ? C26 C119 C25 104.8(12) . . ? C118 C119 C25 110.4(9) . . ? C85 N7 C111 72.3(15) . . ? C85 N7 C27 105.2(17) . . ? C111 N7 C27 111.9(13) . . ? C85 N7 C92 125.7(19) . . ? C111 N7 C92 121.6(14) . . ? C27 N7 C92 113.6(15) . . ? C85 N7 C84 27.2(13) . . ? C111 N7 C84 99.5(13) . . ? C27 N7 C84 96.6(17) . . ? C92 N7 C84 109.5(16) . . ? C85 N7 C99 117.1(18) . . ? C111 N7 C99 160.0(14) . . ? C27 N7 C99 49.8(11) . . ? C92 N7 C99 68.9(13) . . ? C84 N7 C99 91.7(15) . . ? C85 N7 C93 86.2(16) . . ? C111 N7 C93 100.8(12) . . ? C27 N7 C93 147.1(14) . . ? C92 N7 C93 41.5(12) . . ? C84 N7 C93 79.4(15) . . ? C99 N7 C93 97.5(12) . . ? C85 N7 C77 120.0(14) . . ? C111 N7 C77 60.0(10) . . ? C27 N7 C77 124.4(16) . . ? C92 N7 C77 64.7(12) . . ? C84 N7 C77 138.0(13) . . ? C99 N7 C77 120.2(12) . . ? C93 N7 C77 70.5(12) . . ? C2 C1 N6 115.3(9) . . ? C5 N6 C13 105.0(10) . . ? C5 N6 C1 107.4(10) . . ? C13 N6 C1 112.9(10) . . ? C5 N6 C9 112.5(10) . . ? C13 N6 C9 109.0(10) . . ? C1 N6 C9 110.0(9) . . ? C10 C9 N6 119.7(11) . . ? C7 C6 C5 140.1(18) . . ? C6 C5 N6 130.4(13) . . ? N6 C13 C14 113.0(12) . . ? C9 C10 C11 115.6(15) . . ? C3 C2 C1 105.3(10) . . ? C4 C3 C2 118.6(11) . . ? C6 C7 C8 138.5(19) . . ? C10 C11 C12 120.2(16) . . ? C15 C14 C13 114.9(15) . . ? C33 C99 N7 115.2(19) . . ? C33 C39 C43 137(3) . . ? C87 C84 N7 122(3) . . ? C84 C87 C89 107(3) . . ? C94 C93 N7 121(2) . . ? C96 C94 C93 152(3) . . ? C97 C96 C94 129(3) . . ? C87 C89 C91 162(3) . . ? N7 C111 C79 106.3(15) . . ? C81 C79 C111 109.4(19) . . ? C82 C81 C79 106(2) . . ? C39 C33 C99 152(3) . . ? C17 C37 C29 155(4) . . ? N7 C85 C86 94.8(19) . . ? C88 C86 C85 105(2) . . ? C86 C88 C90 117(3) . . ? N7 C92 C95 116(2) . . ? C109 C95 C92 115(3) . . ? C78 C80 C83 111.5(13) . . ? C95 C109 C98 123(3) . . ? C78 C77 N7 104.7(11) . . ? C77 C78 C80 120.3(14) . . ? N7 C27 C29 117.8(17) . . ? C37 C29 C27 131(3) . . ? C16 C15 C14 130(3) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.954 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.099