# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Thomas Weyhermuller' _publ_contact_author_email weyherm@mpi-muelheim.mpg.de loop_ _publ_author_name 'P. Chaudhuri' 'T. Weyhermuller' 'R. Wagner' # Attachment '- Wagner6_Vanadium.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 824885' #TrackingRef '- Wagner6_Vanadium.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H70 N O4 V' _chemical_formula_sum 'C46 H70 N O4 V' _chemical_formula_weight 751.97 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 'P 21/n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 13.8025(4) _cell_length_b 11.7564(3) _cell_length_c 26.8735(6) _cell_angle_alpha 90.00 _cell_angle_beta 93.667(5) _cell_angle_gamma 90.00 _cell_volume 4351.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 132116 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 31.00 _exptl_crystal_description 'transparent parallelepiped' _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.148 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1632 _exptl_absorpt_coefficient_mu 0.269 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.9453 _exptl_absorpt_correction_T_max 0.9892 _exptl_absorpt_process_details 'SADABS 2008/1, Bruker AXS (2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '313 images at 1.0 deg. in phi, 707 images at 1.0 deg in \w, 60 sec./frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 115758 _diffrn_reflns_av_R_equivalents 0.0477 _diffrn_reflns_av_sigmaI/netI 0.0292 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -38 _diffrn_reflns_limit_l_max 38 _diffrn_reflns_theta_min 3.15 _diffrn_reflns_theta_max 31.02 _reflns_number_total 13834 _reflns_number_gt 12235 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect Software' _computing_cell_refinement 'Nonius Collect Software' _computing_data_reduction 'Nonius Collect Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0374P)^2^+2.5366P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 13834 _refine_ls_number_parameters 634 _refine_ls_number_restraints 160 _refine_ls_R_factor_all 0.0560 _refine_ls_R_factor_gt 0.0478 _refine_ls_wR_factor_ref 0.1145 _refine_ls_wR_factor_gt 0.1110 _refine_ls_goodness_of_fit_ref 1.145 _refine_ls_restrained_S_all 1.142 _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 0.61765(11) 0.64340(13) 0.17753(4) 0.01104(13) Uani 0.7073(6) 1 d PD A 1 N1 N 0.52843(19) 0.7513(2) 0.13186(8) 0.0119(3) Uani 0.7073(6) 1 d PD A 1 O70 O 0.6972(3) 0.5215(3) 0.22236(10) 0.0199(5) Uani 0.7073(6) 1 d PD A 1 H70 H 0.704(2) 0.4579(14) 0.2085(10) 0.024 Uiso 0.7073(6) 1 d PD A 1 C71 C 0.7794(7) 0.5365(9) 0.2572(3) 0.0366(5) Uani 0.7073(6) 1 d PD A 1 H71A H 0.8388 0.5400 0.2391 0.055 Uiso 0.7073(6) 1 calc PR A 1 H71B H 0.7835 0.4723 0.2805 0.055 Uiso 0.7073(6) 1 calc PR A 1 H71C H 0.7721 0.6074 0.2757 0.055 Uiso 0.7073(6) 1 calc PR A 1 C10 C 0.53442(12) 0.87052(13) 0.15137(6) 0.0139(3) Uani 0.7073(6) 1 d PD A 1 H10A H 0.4991 0.9220 0.1274 0.017 Uiso 0.7073(6) 1 calc PR A 1 H10B H 0.6032 0.8948 0.1545 0.017 Uiso 0.7073(6) 1 calc PR A 1 C11 C 0.49183(11) 0.88018(13) 0.20130(6) 0.0132(3) Uani 0.7073(6) 1 d PD A 1 C12 C 0.52989(11) 0.81331(14) 0.24122(6) 0.0134(3) Uani 0.7073(6) 1 d PD A 1 O12 O 0.60052(9) 0.73611(10) 0.23345(4) 0.0149(2) Uani 0.7073(6) 1 d PD A 1 C13 C 0.49312(15) 0.8263(2) 0.28892(8) 0.0148(4) Uani 0.7073(6) 1 d PD A 1 C14 C 0.4142(4) 0.8997(5) 0.29271(13) 0.0156(6) Uani 0.7073(6) 1 d PD A 1 H14 H 0.3885 0.9082 0.3244 0.019 Uiso 0.7073(6) 1 calc PR A 1 C15 C 0.37081(13) 0.96138(17) 0.25267(8) 0.0157(4) Uani 0.7073(6) 1 d PD A 1 C16 C 0.41306(12) 0.95232(14) 0.20713(6) 0.0148(3) Uani 0.7073(6) 1 d PD A 1 H16 H 0.3878 0.9960 0.1795 0.018 Uiso 0.7073(6) 1 calc PR A 1 C17 C 0.5412(2) 0.7656(3) 0.33477(9) 0.0169(4) Uani 0.7073(6) 1 d PD A 1 C18 C 0.5368(6) 0.6356(4) 0.3292(3) 0.0230(5) Uani 0.7073(6) 1 d PD A 1 H18A H 0.4688 0.6113 0.3248 0.034 Uiso 0.7073(6) 1 calc PR A 1 H18B H 0.5673 0.5999 0.3592 0.034 Uiso 0.7073(6) 1 calc PR A 1 H18C H 0.5713 0.6126 0.3001 0.034 Uiso 0.7073(6) 1 calc PR A 1 C19 C 0.4921(2) 0.7973(3) 0.38286(10) 0.0286(6) Uani 0.7073(6) 1 d PD A 1 H19A H 0.4936 0.8801 0.3872 0.043 Uiso 0.7073(6) 1 calc PR A 1 H19B H 0.5270 0.7610 0.4115 0.043 Uiso 0.7073(6) 1 calc PR A 1 H19C H 0.4246 0.7710 0.3804 0.043 Uiso 0.7073(6) 1 calc PR A 1 C20 C 0.64804(14) 0.80371(17) 0.34166(8) 0.0215(4) Uani 0.7073(6) 1 d PD A 1 H20A H 0.6509 0.8866 0.3453 0.032 Uiso 0.7073(6) 1 calc PR A 1 H20B H 0.6825 0.7809 0.3125 0.032 Uiso 0.7073(6) 1 calc PR A 1 H20C H 0.6787 0.7679 0.3716 0.032 Uiso 0.7073(6) 1 calc PR A 1 C21 C 0.2809(2) 1.0348(3) 0.25937(17) 0.0180(6) Uani 0.7073(6) 1 d PD A 1 C22 C 0.2432(7) 1.0934(10) 0.2107(3) 0.0336(5) Uani 0.7073(6) 1 d PD A 1 H22A H 0.1861 1.1396 0.2169 0.050 Uiso 0.7073(6) 1 calc PR A 1 H22B H 0.2253 1.0356 0.1855 0.050 Uiso 0.7073(6) 1 calc PR A 1 H22C H 0.2942 1.1424 0.1986 0.050 Uiso 0.7073(6) 1 calc PR A 1 C23 C 0.3074(6) 1.1313(6) 0.2970(4) 0.0316(5) Uani 0.7073(6) 1 d PD A 1 H23A H 0.3328 1.0983 0.3286 0.047 Uiso 0.7073(6) 1 calc PR A 1 H23B H 0.2493 1.1763 0.3025 0.047 Uiso 0.7073(6) 1 calc PR A 1 H23C H 0.3568 1.1804 0.2836 0.047 Uiso 0.7073(6) 1 calc PR A 1 C24 C 0.19914(18) 0.9631(4) 0.27835(16) 0.0319(6) Uani 0.7073(6) 1 d PD A 1 H24A H 0.2215 0.9264 0.3098 0.048 Uiso 0.7073(6) 1 calc PR A 1 H24B H 0.1800 0.9047 0.2536 0.048 Uiso 0.7073(6) 1 calc PR A 1 H24C H 0.1433 1.0119 0.2839 0.048 Uiso 0.7073(6) 1 calc PR A 1 C30 C 0.56102(12) 0.74792(14) 0.07991(6) 0.0145(3) Uani 0.7073(6) 1 d PD A 1 H30A H 0.5136 0.7895 0.0575 0.017 Uiso 0.7073(6) 1 calc PR A 1 H30B H 0.5625 0.6679 0.0685 0.017 Uiso 0.7073(6) 1 calc PR A 1 C31 C 0.66029(11) 0.79988(14) 0.07617(6) 0.0137(3) Uani 0.7073(6) 1 d PD A 1 C32 C 0.73895(11) 0.76162(14) 0.10744(6) 0.0133(3) Uani 0.7073(6) 1 d PD A 1 O32 O 0.72503(8) 0.68033(11) 0.14186(5) 0.0146(2) Uani 0.7073(6) 1 d PD A 1 C33 C 0.83263(17) 0.8086(2) 0.10301(9) 0.0132(5) Uani 0.7073(6) 1 d PD A 1 C34 C 0.8421(3) 0.8919(4) 0.06668(17) 0.0139(7) Uani 0.7073(6) 1 d PD A 1 H34 H 0.9050 0.9219 0.0625 0.017 Uiso 0.7073(6) 1 calc PR A 1 C35 C 0.76433(17) 0.93423(19) 0.03593(8) 0.0152(4) Uani 0.7073(6) 1 d PD A 1 C36 C 0.67340(12) 0.88628(14) 0.04146(6) 0.0154(3) Uani 0.7073(6) 1 d PD A 1 H36 H 0.6191 0.9128 0.0212 0.018 Uiso 0.7073(6) 1 calc PR A 1 C37 C 0.9199(3) 0.7695(4) 0.13712(15) 0.0147(3) Uani 0.7073(6) 1 d PD A 1 C38 C 0.9345(3) 0.6399(4) 0.1332(3) 0.0175(7) Uani 0.7073(6) 1 d PD A 1 H38A H 0.8745 0.6008 0.1408 0.026 Uiso 0.7073(6) 1 calc PR A 1 H38B H 0.9873 0.6161 0.1570 0.026 Uiso 0.7073(6) 1 calc PR A 1 H38C H 0.9510 0.6205 0.0993 0.026 Uiso 0.7073(6) 1 calc PR A 1 C39 C 1.0152(3) 0.8263(4) 0.1236(2) 0.0184(7) Uani 0.7073(6) 1 d PD A 1 H39A H 1.0082 0.9092 0.1251 0.028 Uiso 0.7073(6) 1 calc PR A 1 H39B H 1.0301 0.8038 0.0898 0.028 Uiso 0.7073(6) 1 calc PR A 1 H39C H 1.0681 0.8022 0.1473 0.028 Uiso 0.7073(6) 1 calc PR A 1 C40 C 0.90336(16) 0.8029(3) 0.19155(12) 0.0199(5) Uani 0.7073(6) 1 d PD A 1 H40A H 0.8430 0.7683 0.2015 0.030 Uiso 0.7073(6) 1 calc PR A 1 H40B H 0.8987 0.8858 0.1941 0.030 Uiso 0.7073(6) 1 calc PR A 1 H40C H 0.9579 0.7757 0.2135 0.030 Uiso 0.7073(6) 1 calc PR A 1 C41 C 0.7821(4) 1.0230(4) -0.00416(16) 0.0184(6) Uani 0.7073(6) 1 d PD A 1 C42 C 0.8465(6) 1.1196(6) 0.0177(3) 0.0298(7) Uani 0.7073(6) 1 d PD A 1 H42A H 0.8596 1.1739 -0.0087 0.045 Uiso 0.7073(6) 1 calc PR A 1 H42B H 0.9080 1.0879 0.0318 0.045 Uiso 0.7073(6) 1 calc PR A 1 H42C H 0.8132 1.1585 0.0440 0.045 Uiso 0.7073(6) 1 calc PR A 1 C43 C 0.6875(6) 1.0763(8) -0.0260(4) 0.0294(9) Uani 0.7073(6) 1 d PD A 1 H43A H 0.6428 1.0160 -0.0379 0.044 Uiso 0.7073(6) 1 calc PR A 1 H43B H 0.7015 1.1261 -0.0539 0.044 Uiso 0.7073(6) 1 calc PR A 1 H43C H 0.6577 1.1208 -0.0002 0.044 Uiso 0.7073(6) 1 calc PR A 1 C44 C 0.8331(10) 0.9649(9) -0.0467(3) 0.0325(9) Uani 0.7073(6) 1 d PD A 1 H44A H 0.7940 0.9002 -0.0593 0.049 Uiso 0.7073(6) 1 calc PR A 1 H44B H 0.8973 0.9379 -0.0341 0.049 Uiso 0.7073(6) 1 calc PR A 1 H44C H 0.8406 1.0195 -0.0737 0.049 Uiso 0.7073(6) 1 calc PR A 1 C50 C 0.42640(12) 0.71086(15) 0.13341(7) 0.0134(3) Uani 0.7073(6) 1 d PD A 1 H50A H 0.3828 0.7677 0.1165 0.016 Uiso 0.7073(6) 1 calc PR A 1 H50B H 0.4098 0.7066 0.1687 0.016 Uiso 0.7073(6) 1 calc PR A 1 C51 C 0.40727(12) 0.59708(14) 0.10950(6) 0.0140(3) Uani 0.7073(6) 1 d PD A 1 C52 C 0.46460(11) 0.50259(14) 0.12399(6) 0.0135(3) Uani 0.7073(6) 1 d PD A 1 O52 O 0.54153(8) 0.51638(10) 0.15740(5) 0.0150(2) Uani 0.7073(6) 1 d PD A 1 C53 C 0.43973(14) 0.39422(17) 0.10382(7) 0.0134(4) Uani 0.7073(6) 1 d PD A 1 C54 C 0.35624(18) 0.3868(2) 0.07130(10) 0.0146(6) Uani 0.7073(6) 1 d PD A 1 H54 H 0.3382 0.3141 0.0583 0.017 Uiso 0.7073(6) 1 calc PR A 1 C55 C 0.29812(13) 0.47958(14) 0.05685(7) 0.0151(3) Uani 0.7073(6) 1 d PD A 1 C56 C 0.32664(12) 0.58515(14) 0.07623(6) 0.0154(3) Uani 0.7073(6) 1 d PD A 1 H56 H 0.2900 0.6507 0.0664 0.018 Uiso 0.7073(6) 1 calc PR A 1 C57 C 0.5021(3) 0.2892(3) 0.11702(16) 0.0172(3) Uani 0.7073(6) 1 d PD A 1 C58 C 0.5083(4) 0.2674(2) 0.17358(13) 0.0241(6) Uani 0.7073(6) 1 d PD A 1 H58A H 0.5360 0.3343 0.1910 0.036 Uiso 0.7073(6) 1 calc PR A 1 H58B H 0.5497 0.2012 0.1812 0.036 Uiso 0.7073(6) 1 calc PR A 1 H58C H 0.4431 0.2529 0.1846 0.036 Uiso 0.7073(6) 1 calc PR A 1 C59 C 0.4613(3) 0.1802(3) 0.09188(12) 0.0254(7) Uani 0.7073(6) 1 d PD A 1 H59A H 0.4583 0.1897 0.0556 0.038 Uiso 0.7073(6) 1 calc PR A 1 H59B H 0.3960 0.1657 0.1027 0.038 Uiso 0.7073(6) 1 calc PR A 1 H59C H 0.5037 0.1159 0.1013 0.038 Uiso 0.7073(6) 1 calc PR A 1 C60 C 0.60454(17) 0.3069(2) 0.09875(11) 0.0268(5) Uani 0.7073(6) 1 d PD A 1 H60A H 0.6002 0.3163 0.0624 0.040 Uiso 0.7073(6) 1 calc PR A 1 H60B H 0.6450 0.2406 0.1078 0.040 Uiso 0.7073(6) 1 calc PR A 1 H60C H 0.6336 0.3752 0.1144 0.040 Uiso 0.7073(6) 1 calc PR A 1 C61 C 0.20743(17) 0.4714(3) 0.02101(12) 0.0186(5) Uani 0.7073(6) 1 d PD A 1 C62 C 0.1745(6) 0.3479(4) 0.0124(4) 0.0263(4) Uani 0.7073(6) 1 d PD A 1 H62A H 0.1162 0.3465 -0.0104 0.039 Uiso 0.7073(6) 1 calc PR A 1 H62B H 0.1597 0.3136 0.0443 0.039 Uiso 0.7073(6) 1 calc PR A 1 H62C H 0.2264 0.3047 -0.0021 0.039 Uiso 0.7073(6) 1 calc PR A 1 C63 C 0.2294(4) 0.5251(6) -0.02938(12) 0.0300(6) Uani 0.7073(6) 1 d PD A 1 H63A H 0.1717 0.5200 -0.0525 0.045 Uiso 0.7073(6) 1 calc PR A 1 H63B H 0.2833 0.4843 -0.0434 0.045 Uiso 0.7073(6) 1 calc PR A 1 H63C H 0.2473 0.6051 -0.0243 0.045 Uiso 0.7073(6) 1 calc PR A 1 C64 C 0.12389(16) 0.5374(2) 0.04251(10) 0.0284(4) Uani 0.7073(6) 1 d PD A 1 H64A H 0.0658 0.5315 0.0197 0.043 Uiso 0.7073(6) 1 calc PR A 1 H64B H 0.1423 0.6175 0.0466 0.043 Uiso 0.7073(6) 1 calc PR A 1 H64C H 0.1102 0.5053 0.0750 0.043 Uiso 0.7073(6) 1 calc PR A 1 V1X V 0.6169(3) 0.6394(3) 0.16978(12) 0.01104(13) Uani 0.2927(6) 1 d PD A 2 N1X N 0.5276(5) 0.7462(5) 0.1234(2) 0.0119(3) Uani 0.2927(6) 1 d PD A 2 O70X O 0.7034(8) 0.5200(8) 0.2124(3) 0.0199(5) Uani 0.2927(6) 1 d PD A 2 H70X H 0.672(4) 0.468(4) 0.226(2) 0.024 Uiso 0.2927(6) 1 d PD A 2 C71X C 0.7708(17) 0.535(2) 0.2549(8) 0.0366(5) Uani 0.2927(6) 1 d PD A 2 H71D H 0.8213 0.4766 0.2547 0.055 Uiso 0.2927(6) 1 calc PR A 2 H71E H 0.7364 0.5287 0.2856 0.055 Uiso 0.2927(6) 1 calc PR A 2 H71F H 0.8008 0.6106 0.2534 0.055 Uiso 0.2927(6) 1 calc PR A 2 C10X C 0.4272(3) 0.7497(4) 0.14259(16) 0.0139(3) Uani 0.2927(6) 1 d PD A 2 H10C H 0.3837 0.7927 0.1186 0.017 Uiso 0.2927(6) 1 calc PR A 2 H10D H 0.4020 0.6711 0.1442 0.017 Uiso 0.2927(6) 1 calc PR A 2 C11X C 0.4242(3) 0.8034(3) 0.19313(13) 0.0132(3) Uani 0.2927(6) 1 d PD A 2 C12X C 0.4835(3) 0.7625(3) 0.23346(13) 0.0134(3) Uani 0.2927(6) 1 d PD A 2 O12X O 0.5490(2) 0.6791(2) 0.22575(10) 0.0149(2) Uani 0.2927(6) 1 d PD A 2 C13X C 0.4743(5) 0.8085(6) 0.2815(2) 0.0148(4) Uani 0.2927(6) 1 d PD A 2 C14X C 0.4042(11) 0.8933(14) 0.2861(3) 0.0156(6) Uani 0.2927(6) 1 d PD A 2 H14X H 0.3958 0.9224 0.3185 0.019 Uiso 0.2927(6) 1 calc PR A 2 C15X C 0.3459(4) 0.9381(5) 0.2465(2) 0.0157(4) Uani 0.2927(6) 1 d PD A 2 C16X C 0.3574(3) 0.8904(3) 0.19995(15) 0.0148(3) Uani 0.2927(6) 1 d PD A 2 H16X H 0.3187 0.9177 0.1720 0.018 Uiso 0.2927(6) 1 calc PR A 2 C17X C 0.5393(5) 0.7657(9) 0.3258(3) 0.0169(4) Uani 0.2927(6) 1 d PD A 2 C18X C 0.5316(15) 0.6358(8) 0.3316(8) 0.0230(5) Uani 0.2927(6) 1 d PD A 2 H18D H 0.5708 0.6115 0.3614 0.034 Uiso 0.2927(6) 1 calc PR A 2 H18E H 0.5554 0.5985 0.3022 0.034 Uiso 0.2927(6) 1 calc PR A 2 H18F H 0.4636 0.6147 0.3350 0.034 Uiso 0.2927(6) 1 calc PR A 2 C19X C 0.5113(7) 0.8189(8) 0.3749(3) 0.0286(6) Uani 0.2927(6) 1 d PD A 2 H19D H 0.5502 0.7847 0.4027 0.043 Uiso 0.2927(6) 1 calc PR A 2 H19E H 0.4422 0.8051 0.3791 0.043 Uiso 0.2927(6) 1 calc PR A 2 H19F H 0.5234 0.9010 0.3742 0.043 Uiso 0.2927(6) 1 calc PR A 2 C20X C 0.6455(3) 0.7994(5) 0.3188(2) 0.0215(4) Uani 0.2927(6) 1 d PD A 2 H20D H 0.6873 0.7699 0.3467 0.032 Uiso 0.2927(6) 1 calc PR A 2 H20E H 0.6508 0.8824 0.3177 0.032 Uiso 0.2927(6) 1 calc PR A 2 H20F H 0.6658 0.7672 0.2874 0.032 Uiso 0.2927(6) 1 calc PR A 2 C21X C 0.2680(7) 1.0282(9) 0.2543(5) 0.0180(6) Uani 0.2927(6) 1 d PD A 2 C22X C 0.2423(18) 1.097(2) 0.2063(9) 0.0336(5) Uani 0.2927(6) 1 d PD A 2 H22D H 0.3002 1.1366 0.1962 0.050 Uiso 0.2927(6) 1 calc PR A 2 H22E H 0.1915 1.1522 0.2126 0.050 Uiso 0.2927(6) 1 calc PR A 2 H22F H 0.2188 1.0448 0.1797 0.050 Uiso 0.2927(6) 1 calc PR A 2 C23X C 0.3046(15) 1.1161(17) 0.2937(10) 0.0316(5) Uani 0.2927(6) 1 d PD A 2 H23D H 0.3663 1.1482 0.2843 0.047 Uiso 0.2927(6) 1 calc PR A 2 H23E H 0.3141 1.0788 0.3263 0.047 Uiso 0.2927(6) 1 calc PR A 2 H23F H 0.2565 1.1770 0.2956 0.047 Uiso 0.2927(6) 1 calc PR A 2 C24X C 0.1763(6) 0.9715(11) 0.2707(5) 0.0319(6) Uani 0.2927(6) 1 d PD A 2 H24D H 0.1557 0.9122 0.2467 0.048 Uiso 0.2927(6) 1 calc PR A 2 H24E H 0.1247 1.0285 0.2722 0.048 Uiso 0.2927(6) 1 calc PR A 2 H24F H 0.1894 0.9374 0.3037 0.048 Uiso 0.2927(6) 1 calc PR A 2 C30X C 0.5666(3) 0.8644(3) 0.12250(14) 0.0145(3) Uani 0.2927(6) 1 d PD A 2 H30C H 0.5702 0.8954 0.1568 0.017 Uiso 0.2927(6) 1 calc PR A 2 H30D H 0.5211 0.9126 0.1018 0.017 Uiso 0.2927(6) 1 calc PR A 2 C31X C 0.6653(3) 0.8714(3) 0.10232(14) 0.0137(3) Uani 0.2927(6) 1 d PD A 2 C32X C 0.7426(3) 0.8096(3) 0.12565(15) 0.0133(3) Uani 0.2927(6) 1 d PD A 2 O32X O 0.7250(2) 0.7327(3) 0.16167(11) 0.0146(2) Uani 0.2927(6) 1 d PD A 2 C33X C 0.8383(4) 0.8287(6) 0.1114(3) 0.0132(5) Uani 0.2927(6) 1 d PD A 2 C34X C 0.8501(7) 0.9036(13) 0.0720(5) 0.0139(7) Uani 0.2927(6) 1 d PD A 2 H34X H 0.9142 0.9191 0.0630 0.017 Uiso 0.2927(6) 1 calc PR A 2 C35X C 0.7730(5) 0.9573(6) 0.0450(2) 0.0152(4) Uani 0.2927(6) 1 d PD A 2 C36X C 0.6808(3) 0.9422(3) 0.06173(14) 0.0154(3) Uani 0.2927(6) 1 d PD A 2 H36X H 0.6273 0.9806 0.0453 0.018 Uiso 0.2927(6) 1 calc PR A 2 C37X C 0.9256(6) 0.7728(10) 0.1404(4) 0.0147(3) Uani 0.2927(6) 1 d PD A 2 C38X C 0.9198(11) 0.6419(9) 0.1363(7) 0.0175(7) Uani 0.2927(6) 1 d PD A 2 H38D H 0.9721 0.6077 0.1578 0.026 Uiso 0.2927(6) 1 calc PR A 2 H38E H 0.9267 0.6190 0.1017 0.026 Uiso 0.2927(6) 1 calc PR A 2 H38F H 0.8569 0.6158 0.1470 0.026 Uiso 0.2927(6) 1 calc PR A 2 C39X C 1.0225(8) 0.8085(12) 0.1196(6) 0.0184(7) Uani 0.2927(6) 1 d PD A 2 H39D H 1.0765 0.7753 0.1402 0.028 Uiso 0.2927(6) 1 calc PR A 2 H39E H 1.0280 0.8916 0.1202 0.028 Uiso 0.2927(6) 1 calc PR A 2 H39F H 1.0248 0.7813 0.0852 0.028 Uiso 0.2927(6) 1 calc PR A 2 C40X C 0.9283(6) 0.8089(10) 0.1959(3) 0.0199(5) Uani 0.2927(6) 1 d PD A 2 H40D H 0.9823 0.7704 0.2144 0.030 Uiso 0.2927(6) 1 calc PR A 2 H40E H 0.8671 0.7876 0.2099 0.030 Uiso 0.2927(6) 1 calc PR A 2 H40F H 0.9372 0.8914 0.1984 0.030 Uiso 0.2927(6) 1 calc PR A 2 C41X C 0.7917(10) 1.0334(12) 0.0002(4) 0.0184(6) Uani 0.2927(6) 1 d PD A 2 C42X C 0.8603(16) 1.1306(17) 0.0165(9) 0.0298(7) Uani 0.2927(6) 1 d PD A 2 H42D H 0.9189 1.0993 0.0340 0.045 Uiso 0.2927(6) 1 calc PR A 2 H42E H 0.8276 1.1815 0.0390 0.045 Uiso 0.2927(6) 1 calc PR A 2 H42F H 0.8782 1.1732 -0.0128 0.045 Uiso 0.2927(6) 1 calc PR A 2 C43X C 0.6977(14) 1.086(2) -0.0229(10) 0.0294(9) Uani 0.2927(6) 1 d PD A 2 H43D H 0.6629 1.1237 0.0031 0.044 Uiso 0.2927(6) 1 calc PR A 2 H43E H 0.6567 1.0263 -0.0385 0.044 Uiso 0.2927(6) 1 calc PR A 2 H43F H 0.7134 1.1422 -0.0482 0.044 Uiso 0.2927(6) 1 calc PR A 2 C44X C 0.837(2) 0.962(2) -0.0405(7) 0.0325(9) Uani 0.2927(6) 1 d PD A 2 H44D H 0.8963 0.9255 -0.0265 0.049 Uiso 0.2927(6) 1 calc PR A 2 H44E H 0.8528 1.0121 -0.0681 0.049 Uiso 0.2927(6) 1 calc PR A 2 H44F H 0.7907 0.9041 -0.0529 0.049 Uiso 0.2927(6) 1 calc PR A 2 C50X C 0.5203(3) 0.6989(3) 0.07151(14) 0.0134(3) Uani 0.2927(6) 1 d PD A 2 H50C H 0.5864 0.6886 0.0599 0.016 Uiso 0.2927(6) 1 calc PR A 2 H50D H 0.4855 0.7539 0.0489 0.016 Uiso 0.2927(6) 1 calc PR A 2 C51X C 0.4678(3) 0.5871(3) 0.06891(14) 0.0140(3) Uani 0.2927(6) 1 d PD A 2 C52X C 0.5054(3) 0.4953(3) 0.09718(14) 0.0135(3) Uani 0.2927(6) 1 d PD A 2 O52X O 0.5839(2) 0.5123(2) 0.12960(11) 0.0150(2) Uani 0.2927(6) 1 d PD A 2 C53X C 0.4593(4) 0.3883(4) 0.0928(2) 0.0134(4) Uani 0.2927(6) 1 d PD A 2 C54X C 0.3707(5) 0.3833(7) 0.0637(3) 0.0146(6) Uani 0.2927(6) 1 d PD A 2 H54X H 0.3393 0.3116 0.0600 0.017 Uiso 0.2927(6) 1 calc PR A 2 C55X C 0.3264(3) 0.4771(4) 0.04007(17) 0.0151(3) Uani 0.2927(6) 1 d PD A 2 C56X C 0.3795(3) 0.5781(3) 0.04115(15) 0.0154(3) Uani 0.2927(6) 1 d PD A 2 H56X H 0.3550 0.6418 0.0226 0.018 Uiso 0.2927(6) 1 calc PR A 2 C57X C 0.5038(6) 0.2819(7) 0.1179(4) 0.0172(3) Uani 0.2927(6) 1 d PD A 2 C58X C 0.5063(11) 0.2928(9) 0.1751(3) 0.0241(6) Uani 0.2927(6) 1 d PD A 2 H58D H 0.5381 0.2258 0.1904 0.036 Uiso 0.2927(6) 1 calc PR A 2 H58E H 0.4399 0.2984 0.1857 0.036 Uiso 0.2927(6) 1 calc PR A 2 H58F H 0.5427 0.3613 0.1855 0.036 Uiso 0.2927(6) 1 calc PR A 2 C59X C 0.4445(8) 0.1752(8) 0.1027(4) 0.0254(7) Uani 0.2927(6) 1 d PD A 2 H59D H 0.4758 0.1080 0.1182 0.038 Uiso 0.2927(6) 1 calc PR A 2 H59E H 0.4414 0.1671 0.0664 0.038 Uiso 0.2927(6) 1 calc PR A 2 H59F H 0.3787 0.1827 0.1139 0.038 Uiso 0.2927(6) 1 calc PR A 2 C60X C 0.6070(5) 0.2642(5) 0.1006(3) 0.0268(5) Uani 0.2927(6) 1 d PD A 2 H60D H 0.6361 0.1968 0.1170 0.040 Uiso 0.2927(6) 1 calc PR A 2 H60E H 0.6468 0.3312 0.1094 0.040 Uiso 0.2927(6) 1 calc PR A 2 H60F H 0.6037 0.2535 0.0644 0.040 Uiso 0.2927(6) 1 calc PR A 2 C61X C 0.2232(5) 0.4753(9) 0.0152(3) 0.0186(5) Uani 0.2927(6) 1 d PD A 2 C62X C 0.1800(14) 0.3545(11) 0.0138(9) 0.0263(4) Uani 0.2927(6) 1 d PD A 2 H62D H 0.1797 0.3246 0.0479 0.039 Uiso 0.2927(6) 1 calc PR A 2 H62E H 0.2195 0.3049 -0.0061 0.039 Uiso 0.2927(6) 1 calc PR A 2 H62F H 0.1134 0.3570 -0.0011 0.039 Uiso 0.2927(6) 1 calc PR A 2 C63X C 0.2210(12) 0.5218(17) -0.0381(4) 0.0300(6) Uani 0.2927(6) 1 d PD A 2 H63D H 0.2494 0.5983 -0.0377 0.045 Uiso 0.2927(6) 1 calc PR A 2 H63E H 0.1537 0.5254 -0.0520 0.045 Uiso 0.2927(6) 1 calc PR A 2 H63F H 0.2586 0.4716 -0.0587 0.045 Uiso 0.2927(6) 1 calc PR A 2 C64X C 0.1584(4) 0.5477(6) 0.0471(3) 0.0284(4) Uani 0.2927(6) 1 d PD A 2 H64D H 0.1600 0.5167 0.0810 0.043 Uiso 0.2927(6) 1 calc PR A 2 H64E H 0.0915 0.5464 0.0324 0.043 Uiso 0.2927(6) 1 calc PR A 2 H64F H 0.1822 0.6262 0.0482 0.043 Uiso 0.2927(6) 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 0.01065(9) 0.01034(14) 0.0121(4) 0.0001(2) 0.0002(3) 0.00019(9) N1 0.0120(4) 0.0105(5) 0.0133(10) -0.0010(6) 0.0007(6) -0.0006(4) O70 0.0189(7) 0.0162(4) 0.0241(14) 0.0039(9) -0.0042(10) 0.0020(4) C71 0.0273(17) 0.0333(9) 0.0466(13) 0.0069(8) -0.0193(8) 0.0012(12) C10 0.0152(6) 0.0097(6) 0.0166(7) -0.0004(5) -0.0009(5) -0.0005(5) C11 0.0131(6) 0.0116(6) 0.0149(6) -0.0006(5) -0.0001(5) -0.0003(5) C12 0.0122(6) 0.0125(6) 0.0152(6) -0.0010(5) -0.0012(5) 0.0000(5) O12 0.0148(5) 0.0151(5) 0.0145(5) -0.0010(4) -0.0005(4) 0.0039(4) C13 0.0158(11) 0.0146(10) 0.0139(9) -0.0002(6) -0.0001(7) 0.0004(8) C14 0.0148(14) 0.0159(9) 0.0161(11) -0.0016(10) 0.0016(9) 0.0000(11) C15 0.0131(10) 0.0149(10) 0.0189(8) -0.0030(6) -0.0004(7) 0.0013(7) C16 0.0135(6) 0.0123(6) 0.0184(7) 0.0004(5) -0.0006(5) 0.0010(5) C17 0.0196(6) 0.0176(6) 0.0132(12) 0.0010(9) -0.0005(7) 0.0018(5) C18 0.0266(11) 0.0174(6) 0.0244(10) 0.0049(5) -0.0023(8) -0.0001(5) C19 0.0347(16) 0.0389(17) 0.0125(11) 0.0042(9) 0.0039(8) 0.0138(11) C20 0.0222(7) 0.0230(8) 0.0185(9) -0.0033(9) -0.0046(8) 0.0001(6) C21 0.0119(11) 0.0205(7) 0.0215(12) -0.0025(7) -0.0003(9) 0.0031(8) C22 0.0294(8) 0.0375(10) 0.0340(18) 0.0044(10) 0.0032(10) 0.0158(7) C23 0.0246(9) 0.026(2) 0.0430(17) -0.0107(12) -0.0044(9) 0.0070(13) C24 0.0164(15) 0.0320(11) 0.0478(18) 0.0003(11) 0.0042(13) -0.0002(13) C30 0.0148(6) 0.0157(7) 0.0127(6) 0.0011(5) -0.0004(5) 0.0008(5) C31 0.0136(6) 0.0131(6) 0.0143(6) -0.0009(5) 0.0006(5) 0.0002(5) C32 0.0143(6) 0.0125(7) 0.0131(7) 0.0007(5) 0.0013(5) 0.0014(6) O32 0.0131(5) 0.0148(5) 0.0159(6) 0.0045(4) 0.0016(4) 0.0008(4) C33 0.0143(6) 0.0118(11) 0.0137(11) -0.0009(8) 0.0009(6) 0.0005(6) C34 0.0159(8) 0.0119(13) 0.0139(13) -0.0008(12) 0.0007(7) -0.0018(7) C35 0.0192(7) 0.0128(11) 0.0137(10) 0.0006(7) 0.0006(7) -0.0005(7) C36 0.0176(7) 0.0144(7) 0.0139(7) 0.0004(5) -0.0007(5) 0.0021(5) C37 0.0139(6) 0.0145(6) 0.0156(7) 0.0012(5) 0.0005(5) 0.0001(5) C38 0.0129(18) 0.0155(6) 0.0239(11) 0.0015(6) 0.0000(12) 0.0017(8) C39 0.0148(9) 0.0161(18) 0.0242(12) 0.0019(11) 0.0016(7) -0.0002(9) C40 0.0204(15) 0.0225(8) 0.0165(9) -0.0009(7) -0.0007(10) 0.0010(13) C41 0.0243(12) 0.0141(11) 0.0164(10) 0.0033(9) -0.0011(8) -0.0037(8) C42 0.039(3) 0.0176(16) 0.0312(9) 0.0079(11) -0.0073(15) -0.0108(10) C43 0.0343(18) 0.0232(18) 0.0294(15) 0.0120(15) -0.0077(12) -0.0017(14) C44 0.0473(15) 0.0280(9) 0.023(2) 0.0030(15) 0.013(2) -0.0033(8) C50 0.0111(6) 0.0105(6) 0.0184(7) -0.0006(5) -0.0012(5) -0.0002(5) C51 0.0139(6) 0.0123(6) 0.0156(7) 0.0000(5) -0.0002(5) -0.0007(5) C52 0.0128(6) 0.0128(6) 0.0148(7) 0.0004(5) 0.0002(5) -0.0009(5) O52 0.0139(5) 0.0125(5) 0.0181(5) 0.0009(4) -0.0037(4) -0.0004(4) C53 0.0131(9) 0.0117(6) 0.0154(10) 0.0013(6) 0.0014(6) -0.0007(6) C54 0.0153(10) 0.0126(5) 0.0158(12) -0.0008(7) 0.0008(9) -0.0008(6) C55 0.0139(8) 0.0143(6) 0.0167(9) 0.0002(6) -0.0011(5) -0.0022(6) C56 0.0154(6) 0.0135(6) 0.0168(7) 0.0007(5) -0.0021(5) 0.0002(5) C57 0.0183(5) 0.0123(6) 0.0206(6) 0.0008(5) -0.0028(4) 0.0010(5) C58 0.0343(8) 0.0153(17) 0.0219(7) 0.0053(10) -0.0053(6) -0.0021(14) C59 0.0283(16) 0.0134(7) 0.0332(19) -0.0025(10) -0.0081(11) 0.0025(8) C60 0.0193(7) 0.0241(12) 0.0370(9) -0.0074(13) 0.0026(6) 0.0044(11) C61 0.0171(10) 0.0151(6) 0.0226(11) -0.0010(7) -0.0065(9) -0.0010(8) C62 0.0234(11) 0.0186(8) 0.0351(9) -0.0034(8) -0.0125(8) -0.0027(6) C63 0.0378(14) 0.0286(9) 0.0221(15) -0.0006(15) -0.0093(13) -0.0060(10) C64 0.0168(11) 0.0235(9) 0.0440(11) -0.0059(8) -0.0057(11) 0.0000(10) V1X 0.01065(9) 0.01034(14) 0.0121(4) 0.0001(2) 0.0002(3) 0.00019(9) N1X 0.0120(4) 0.0105(5) 0.0133(10) -0.0010(6) 0.0007(6) -0.0006(4) O70X 0.0189(7) 0.0162(4) 0.0241(14) 0.0039(9) -0.0042(10) 0.0020(4) C71X 0.0273(17) 0.0333(9) 0.0466(13) 0.0069(8) -0.0193(8) 0.0012(12) C10X 0.0152(6) 0.0097(6) 0.0166(7) -0.0004(5) -0.0009(5) -0.0005(5) C11X 0.0131(6) 0.0116(6) 0.0149(6) -0.0006(5) -0.0001(5) -0.0003(5) C12X 0.0122(6) 0.0125(6) 0.0152(6) -0.0010(5) -0.0012(5) 0.0000(5) O12X 0.0148(5) 0.0151(5) 0.0145(5) -0.0010(4) -0.0005(4) 0.0039(4) C13X 0.0158(11) 0.0146(10) 0.0139(9) -0.0002(6) -0.0001(7) 0.0004(8) C14X 0.0148(14) 0.0159(9) 0.0161(11) -0.0016(10) 0.0016(9) 0.0000(11) C15X 0.0131(10) 0.0149(10) 0.0189(8) -0.0030(6) -0.0004(7) 0.0013(7) C16X 0.0135(6) 0.0123(6) 0.0184(7) 0.0004(5) -0.0006(5) 0.0010(5) C17X 0.0196(6) 0.0176(6) 0.0132(12) 0.0010(9) -0.0005(7) 0.0018(5) C18X 0.0266(11) 0.0174(6) 0.0244(10) 0.0049(5) -0.0023(8) -0.0001(5) C19X 0.0347(16) 0.0389(17) 0.0125(11) 0.0042(9) 0.0039(8) 0.0138(11) C20X 0.0222(7) 0.0230(8) 0.0185(9) -0.0033(9) -0.0046(8) 0.0001(6) C21X 0.0119(11) 0.0205(7) 0.0215(12) -0.0025(7) -0.0003(9) 0.0031(8) C22X 0.0294(8) 0.0375(10) 0.0340(18) 0.0044(10) 0.0032(10) 0.0158(7) C23X 0.0246(9) 0.026(2) 0.0430(17) -0.0107(12) -0.0044(9) 0.0070(13) C24X 0.0164(15) 0.0320(11) 0.0478(18) 0.0003(11) 0.0042(13) -0.0002(13) C30X 0.0148(6) 0.0157(7) 0.0127(6) 0.0011(5) -0.0004(5) 0.0008(5) C31X 0.0136(6) 0.0131(6) 0.0143(6) -0.0009(5) 0.0006(5) 0.0002(5) C32X 0.0143(6) 0.0125(7) 0.0131(7) 0.0007(5) 0.0013(5) 0.0014(6) O32X 0.0131(5) 0.0148(5) 0.0159(6) 0.0045(4) 0.0016(4) 0.0008(4) C33X 0.0143(6) 0.0118(11) 0.0137(11) -0.0009(8) 0.0009(6) 0.0005(6) C34X 0.0159(8) 0.0119(13) 0.0139(13) -0.0008(12) 0.0007(7) -0.0018(7) C35X 0.0192(7) 0.0128(11) 0.0137(10) 0.0006(7) 0.0006(7) -0.0005(7) C36X 0.0176(7) 0.0144(7) 0.0139(7) 0.0004(5) -0.0007(5) 0.0021(5) C37X 0.0139(6) 0.0145(6) 0.0156(7) 0.0012(5) 0.0005(5) 0.0001(5) C38X 0.0129(18) 0.0155(6) 0.0239(11) 0.0015(6) 0.0000(12) 0.0017(8) C39X 0.0148(9) 0.0161(18) 0.0242(12) 0.0019(11) 0.0016(7) -0.0002(9) C40X 0.0204(15) 0.0225(8) 0.0165(9) -0.0009(7) -0.0007(10) 0.0010(13) C41X 0.0243(12) 0.0141(11) 0.0164(10) 0.0033(9) -0.0011(8) -0.0037(8) C42X 0.039(3) 0.0176(16) 0.0312(9) 0.0079(11) -0.0073(15) -0.0108(10) C43X 0.0343(18) 0.0232(18) 0.0294(15) 0.0120(15) -0.0077(12) -0.0017(14) C44X 0.0473(15) 0.0280(9) 0.023(2) 0.0030(15) 0.013(2) -0.0033(8) C50X 0.0111(6) 0.0105(6) 0.0184(7) -0.0006(5) -0.0012(5) -0.0002(5) C51X 0.0139(6) 0.0123(6) 0.0156(7) 0.0000(5) -0.0002(5) -0.0007(5) C52X 0.0128(6) 0.0128(6) 0.0148(7) 0.0004(5) 0.0002(5) -0.0009(5) O52X 0.0139(5) 0.0125(5) 0.0181(5) 0.0009(4) -0.0037(4) -0.0004(4) C53X 0.0131(9) 0.0117(6) 0.0154(10) 0.0013(6) 0.0014(6) -0.0007(6) C54X 0.0153(10) 0.0126(5) 0.0158(12) -0.0008(7) 0.0008(9) -0.0008(6) C55X 0.0139(8) 0.0143(6) 0.0167(9) 0.0002(6) -0.0011(5) -0.0022(6) C56X 0.0154(6) 0.0135(6) 0.0168(7) 0.0007(5) -0.0021(5) 0.0002(5) C57X 0.0183(5) 0.0123(6) 0.0206(6) 0.0008(5) -0.0028(4) 0.0010(5) C58X 0.0343(8) 0.0153(17) 0.0219(7) 0.0053(10) -0.0053(6) -0.0021(14) C59X 0.0283(16) 0.0134(7) 0.0332(19) -0.0025(10) -0.0081(11) 0.0025(8) C60X 0.0193(7) 0.0241(12) 0.0370(9) -0.0074(13) 0.0026(6) 0.0044(11) C61X 0.0171(10) 0.0151(6) 0.0226(11) -0.0010(7) -0.0065(9) -0.0010(8) C62X 0.0234(11) 0.0186(8) 0.0351(9) -0.0034(8) -0.0125(8) -0.0027(6) C63X 0.0378(14) 0.0286(9) 0.0221(15) -0.0006(15) -0.0093(13) -0.0060(10) C64X 0.0168(11) 0.0235(9) 0.0440(11) -0.0059(8) -0.0057(11) 0.0000(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 O32 1.8669(18) . ? V1 O12 1.8836(15) . ? V1 O52 1.8852(18) . ? V1 N1 2.107(2) . ? V1 O70 2.131(2) . ? N1 C50 1.490(3) . ? N1 C30 1.494(3) . ? N1 C10 1.497(3) . ? O70 C71 1.435(4) . ? C10 C11 1.503(2) . ? C11 C16 1.396(2) . ? C11 C12 1.405(2) . ? C12 O12 1.3578(19) . ? C12 C13 1.417(3) . ? C13 C14 1.398(3) . ? C13 C17 1.537(3) . ? C14 C15 1.400(3) . ? C15 C16 1.393(3) . ? C15 C21 1.532(3) . ? C17 C18 1.536(3) . ? C17 C20 1.541(3) . ? C17 C19 1.543(3) . ? C21 C24 1.523(3) . ? C21 C22 1.540(4) . ? C21 C23 1.547(3) . ? C30 C31 1.509(2) . ? C31 C36 1.399(2) . ? C31 C32 1.404(2) . ? C32 O32 1.3524(19) . ? C32 C33 1.418(3) . ? C33 C34 1.395(3) . ? C33 C37 1.537(3) . ? C34 C35 1.403(3) . ? C35 C36 1.392(3) . ? C35 C41 1.531(3) . ? C37 C39 1.539(3) . ? C37 C38 1.541(3) . ? C37 C40 1.546(3) . ? C41 C43 1.531(3) . ? C41 C42 1.535(3) . ? C41 C44 1.540(3) . ? C50 C51 1.500(2) . ? C51 C56 1.389(2) . ? C51 C52 1.404(2) . ? C52 O52 1.3557(19) . ? C52 C53 1.418(2) . ? C53 C54 1.404(3) . ? C53 C57 1.534(3) . ? C54 C55 1.395(3) . ? C55 C56 1.393(2) . ? C55 C61 1.533(3) . ? C57 C59 1.538(3) . ? C57 C58 1.538(3) . ? C57 C60 1.540(3) . ? C61 C64 1.533(3) . ? C61 C62 1.534(3) . ? C61 C63 1.542(4) . ? V1X O32X 1.875(4) . ? V1X O12X 1.881(4) . ? V1X O52X 1.883(4) . ? V1X N1X 2.111(6) . ? V1X O70X 2.129(6) . ? N1X C30X 1.491(7) . ? N1X C50X 1.498(7) . ? N1X C10X 1.509(7) . ? O70X C71X 1.437(8) . ? C10X C11X 1.501(5) . ? C11X C16X 1.397(5) . ? C11X C12X 1.400(5) . ? C12X O12X 1.358(4) . ? C12X C13X 1.412(6) . ? C13X C14X 1.400(7) . ? C13X C17X 1.531(7) . ? C14X C15X 1.395(7) . ? C15X C16X 1.390(5) . ? C15X C21X 1.533(6) . ? C17X C19X 1.531(7) . ? C17X C18X 1.540(7) . ? C17X C20X 1.541(7) . ? C21X C24X 1.520(7) . ? C21X C23X 1.541(7) . ? C21X C22X 1.542(7) . ? C30X C31X 1.501(5) . ? C31X C36X 1.399(5) . ? C31X C32X 1.404(5) . ? C32X O32X 1.358(4) . ? C32X C33X 1.417(6) . ? C33X C34X 1.395(7) . ? C33X C37X 1.539(6) . ? C34X C35X 1.399(7) . ? C35X C36X 1.387(6) . ? C35X C41X 1.537(6) . ? C37X C39X 1.541(7) . ? C37X C38X 1.545(7) . ? C37X C40X 1.548(7) . ? C41X C42X 1.530(7) . ? C41X C43X 1.533(7) . ? C41X C44X 1.540(7) . ? C50X C51X 1.500(5) . ? C51X C56X 1.392(5) . ? C51X C52X 1.400(5) . ? C52X O52X 1.360(4) . ? C52X C53X 1.411(5) . ? C53X C54X 1.410(6) . ? C53X C57X 1.532(6) . ? C54X C55X 1.395(6) . ? C55X C56X 1.394(5) . ? C55X C61X 1.535(6) . ? C57X C59X 1.537(7) . ? C57X C58X 1.539(7) . ? C57X C60X 1.541(7) . ? C61X C63X 1.532(7) . ? C61X C64X 1.536(7) . ? C61X C62X 1.539(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 O32 V1 O12 114.79(9) . . ? O32 V1 O52 118.89(8) . . ? O12 V1 O52 126.24(9) . . ? O32 V1 N1 90.84(10) . . ? O12 V1 N1 91.02(9) . . ? O52 V1 N1 90.90(10) . . ? O32 V1 O70 92.84(12) . . ? O12 V1 O70 91.39(11) . . ? O52 V1 O70 83.52(14) . . ? N1 V1 O70 174.30(16) . . ? C50 N1 C30 111.05(17) . . ? C50 N1 C10 108.69(18) . . ? C30 N1 C10 109.83(18) . . ? C50 N1 V1 108.05(16) . . ? C30 N1 V1 109.17(15) . . ? C10 N1 V1 110.04(14) . . ? C71 O70 V1 130.1(4) . . ? N1 C10 C11 111.56(15) . . ? C16 C11 C12 120.69(15) . . ? C16 C11 C10 119.87(14) . . ? C12 C11 C10 119.40(14) . . ? O12 C12 C11 119.59(14) . . ? O12 C12 C13 120.89(16) . . ? C11 C12 C13 119.51(16) . . ? C12 O12 V1 129.60(11) . . ? C14 C13 C12 117.3(2) . . ? C14 C13 C17 121.8(2) . . ? C12 C13 C17 120.93(19) . . ? C13 C14 C15 124.1(3) . . ? C16 C15 C14 116.9(2) . . ? C16 C15 C21 122.3(2) . . ? C14 C15 C21 120.8(3) . . ? C15 C16 C11 121.20(16) . . ? C18 C17 C13 111.8(4) . . ? C18 C17 C20 109.4(4) . . ? C13 C17 C20 108.8(2) . . ? C18 C17 C19 107.8(3) . . ? C13 C17 C19 111.7(2) . . ? C20 C17 C19 107.3(2) . . ? C24 C21 C15 110.5(3) . . ? C24 C21 C22 108.4(4) . . ? C15 C21 C22 112.6(4) . . ? C24 C21 C23 109.7(3) . . ? C15 C21 C23 109.3(3) . . ? C22 C21 C23 106.3(4) . . ? N1 C30 C31 112.34(16) . . ? C36 C31 C32 120.25(15) . . ? C36 C31 C30 119.67(14) . . ? C32 C31 C30 120.08(14) . . ? O32 C32 C31 119.84(14) . . ? O32 C32 C33 120.21(16) . . ? C31 C32 C33 119.95(17) . . ? C32 O32 V1 131.89(11) . . ? C34 C33 C32 117.3(2) . . ? C34 C33 C37 121.5(2) . . ? C32 C33 C37 121.2(2) . . ? C33 C34 C35 124.0(3) . . ? C36 C35 C34 117.0(2) . . ? C36 C35 C41 122.5(2) . . ? C34 C35 C41 120.3(3) . . ? C35 C36 C31 121.41(17) . . ? C33 C37 C39 112.3(3) . . ? C33 C37 C38 110.9(3) . . ? C39 C37 C38 107.2(3) . . ? C33 C37 C40 109.3(3) . . ? C39 C37 C40 107.0(3) . . ? C38 C37 C40 110.1(3) . . ? C43 C41 C35 112.2(3) . . ? C43 C41 C42 107.7(3) . . ? C35 C41 C42 110.5(3) . . ? C43 C41 C44 108.4(4) . . ? C35 C41 C44 108.7(3) . . ? C42 C41 C44 109.3(4) . . ? N1 C50 C51 114.44(16) . . ? C56 C51 C52 120.83(15) . . ? C56 C51 C50 118.52(14) . . ? C52 C51 C50 120.39(14) . . ? O52 C52 C51 119.51(14) . . ? O52 C52 C53 121.39(15) . . ? C51 C52 C53 119.10(15) . . ? C52 O52 V1 133.10(11) . . ? C54 C53 C52 117.58(19) . . ? C54 C53 C57 121.3(2) . . ? C52 C53 C57 121.1(2) . . ? C55 C54 C53 124.0(2) . . ? C56 C55 C54 116.69(18) . . ? C56 C55 C61 119.41(19) . . ? C54 C55 C61 123.9(2) . . ? C51 C56 C55 121.75(15) . . ? C53 C57 C59 112.6(3) . . ? C53 C57 C58 110.9(3) . . ? C59 C57 C58 106.9(3) . . ? C53 C57 C60 109.3(2) . . ? C59 C57 C60 106.9(3) . . ? C58 C57 C60 110.1(3) . . ? C55 C61 C64 109.6(2) . . ? C55 C61 C62 112.1(4) . . ? C64 C61 C62 108.2(3) . . ? C55 C61 C63 109.1(2) . . ? C64 C61 C63 108.6(3) . . ? C62 C61 C63 109.2(4) . . ? O32X V1X O12X 112.9(2) . . ? O32X V1X O52X 124.2(2) . . ? O12X V1X O52X 122.7(2) . . ? O32X V1X N1X 91.3(3) . . ? O12X V1X N1X 91.3(3) . . ? O52X V1X N1X 91.3(2) . . ? O32X V1X O70X 91.5(4) . . ? O12X V1X O70X 91.4(3) . . ? O52X V1X O70X 83.8(3) . . ? N1X V1X O70X 175.1(4) . . ? C30X N1X C50X 109.5(5) . . ? C30X N1X C10X 108.7(4) . . ? C50X N1X C10X 108.7(4) . . ? C30X N1X V1X 111.4(4) . . ? C50X N1X V1X 109.3(4) . . ? C10X N1X V1X 109.2(4) . . ? C71X O70X V1X 131.1(11) . . ? C11X C10X N1X 113.6(4) . . ? C16X C11X C12X 120.5(3) . . ? C16X C11X C10X 118.9(3) . . ? C12X C11X C10X 120.5(3) . . ? O12X C12X C11X 119.4(3) . . ? O12X C12X C13X 121.0(4) . . ? C11X C12X C13X 119.6(4) . . ? C12X O12X V1X 132.2(3) . . ? C14X C13X C12X 117.2(6) . . ? C14X C13X C17X 122.6(6) . . ? C12X C13X C17X 120.2(5) . . ? C15X C14X C13X 124.7(7) . . ? C16X C15X C14X 116.2(5) . . ? C16X C15X C21X 121.5(6) . . ? C14X C15X C21X 122.1(6) . . ? C15X C16X C11X 121.8(4) . . ? C19X C17X C13X 111.6(6) . . ? C19X C17X C18X 107.2(9) . . ? C13X C17X C18X 111.3(9) . . ? C19X C17X C20X 107.2(6) . . ? C13X C17X C20X 109.5(6) . . ? C18X C17X C20X 109.9(9) . . ? C24X C21X C15X 109.9(7) . . ? C24X C21X C23X 109.7(9) . . ? C15X C21X C23X 110.8(9) . . ? C24X C21X C22X 108.6(9) . . ? C15X C21X C22X 111.9(9) . . ? C23X C21X C22X 105.8(9) . . ? N1X C30X C31X 113.2(4) . . ? C36X C31X C32X 120.4(3) . . ? C36X C31X C30X 120.1(3) . . ? C32X C31X C30X 119.4(3) . . ? O32X C32X C31X 119.8(3) . . ? O32X C32X C33X 120.7(4) . . ? C31X C32X C33X 119.5(4) . . ? C32X O32X V1X 130.7(3) . . ? C34X C33X C32X 117.4(6) . . ? C34X C33X C37X 121.9(6) . . ? C32X C33X C37X 120.6(6) . . ? C33X C34X C35X 123.8(7) . . ? C36X C35X C34X 117.2(6) . . ? C36X C35X C41X 122.1(7) . . ? C34X C35X C41X 120.6(7) . . ? C35X C36X C31X 121.2(4) . . ? C33X C37X C39X 111.7(8) . . ? C33X C37X C38X 110.7(8) . . ? C39X C37X C38X 106.7(8) . . ? C33X C37X C40X 109.9(7) . . ? C39X C37X C40X 107.9(8) . . ? C38X C37X C40X 109.8(8) . . ? C42X C41X C43X 107.8(9) . . ? C42X C41X C35X 109.9(8) . . ? C43X C41X C35X 111.9(9) . . ? C42X C41X C44X 109.7(9) . . ? C43X C41X C44X 107.7(9) . . ? C35X C41X C44X 109.7(9) . . ? N1X C50X C51X 111.9(4) . . ? C56X C51X C52X 120.9(3) . . ? C56X C51X C50X 119.7(3) . . ? C52X C51X C50X 119.3(3) . . ? O52X C52X C51X 119.1(3) . . ? O52X C52X C53X 121.4(4) . . ? C51X C52X C53X 119.5(4) . . ? C52X O52X V1X 129.6(3) . . ? C54X C53X C52X 117.0(5) . . ? C54X C53X C57X 121.2(5) . . ? C52X C53X C57X 121.7(5) . . ? C55X C54X C53X 123.9(6) . . ? C56X C55X C54X 116.7(5) . . ? C56X C55X C61X 119.5(5) . . ? C54X C55X C61X 123.7(6) . . ? C51X C56X C55X 121.1(4) . . ? C53X C57X C59X 111.0(7) . . ? C53X C57X C58X 110.8(7) . . ? C59X C57X C58X 108.2(7) . . ? C53X C57X C60X 109.1(6) . . ? C59X C57X C60X 107.2(7) . . ? C58X C57X C60X 110.5(7) . . ? C63X C61X C55X 111.3(7) . . ? C63X C61X C64X 110.3(8) . . ? C55X C61X C64X 107.9(5) . . ? C63X C61X C62X 108.8(9) . . ? C55X C61X C62X 111.7(9) . . ? C64X C61X C62X 106.7(9) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 31.02 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.682 _refine_diff_density_min -0.315 _refine_diff_density_rms 0.050 #===END data_2 _database_code_depnum_ccdc_archive 'CCDC 824886' #TrackingRef '- Wagner6_Vanadium.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H69 N O4 V' _chemical_formula_sum 'C46 H69 N O4 V' _chemical_formula_weight 750.96 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 'P 21/m' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 10.7177(4) _cell_length_b 18.7454(6) _cell_length_c 10.9784(4) _cell_angle_alpha 90.00 _cell_angle_beta 99.288(2) _cell_angle_gamma 90.00 _cell_volume 2176.73(13) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 95190 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 33.14 _exptl_crystal_description 'transparent parallelepiped' _exptl_crystal_colour red _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.49 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.146 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 814 _exptl_absorpt_coefficient_mu 0.268 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.8730 _exptl_absorpt_correction_T_max 0.9384 _exptl_absorpt_process_details 'SADABS 2006/1, Bruker AXS (2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '991 images at 1.0 deg. in \w and 10 sec.' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 61370 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_av_sigmaI/netI 0.0250 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.10 _diffrn_reflns_theta_max 33.22 _reflns_number_total 8540 _reflns_number_gt 7656 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'DENZO, Nonius Collect Software' _computing_cell_refinement 'DENZO, Nonius Collect Software' _computing_data_reduction 'DENZO, Nonius Collect Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0817P)^2^+2.1283P] 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 8540 _refine_ls_number_parameters 296 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.0740 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.1805 _refine_ls_wR_factor_gt 0.1757 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.085 _refine_ls_shift/su_max 0.014 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.52261(4) 0.7554(3) -0.48372(4) 0.0168(4) Uani 0.50 1 d PD . . N1 N 0.73478(16) 0.7500 -0.48543(15) 0.0182(3) Uani 1 2 d SD . . C2 C 0.7999(3) 0.69408(15) -0.3924(2) 0.0164(4) Uani 0.50 1 d PD . . H2A H 0.8879 0.6905 -0.4001 0.021 Uiso 0.50 1 d P . . H2B H 0.7619 0.6483 -0.4107 0.021 Uiso 0.50 1 d P . . O4 O 0.56633(18) 0.71996(12) -0.32146(18) 0.0184(4) Uani 0.50 1 d PD . . C3 C 0.78878(14) 0.71474(11) -0.26237(11) 0.0150(4) Uani 0.50 1 d PGD . . C4 C 0.66946(11) 0.72422(13) -0.23064(11) 0.0144(4) Uani 0.50 1 d PG . . C5 C 0.65728(9) 0.7408(2) -0.10972(13) 0.0231(9) Uani 0.50 1 d PG . . C6 C 0.76442(12) 0.7493(2) -0.02051(10) 0.0182(3) Uani 1 2 d SG . . H6 H 0.7562 0.7624 0.0614 0.022 Uiso 0.50 1 calc PR . . C7 C 0.88374(10) 0.73844(14) -0.05225(12) 0.0166(8) Uani 0.50 1 d PG . . C8 C 0.89592(11) 0.72184(11) -0.17318(14) 0.0162(4) Uani 0.50 1 d PG . . H8 H 0.9775 0.7154 -0.1949 0.019 Uiso 0.50 1 calc PR . . C9 C 0.52366(17) 0.7500 -0.06932(18) 0.0181(3) Uani 1 2 d S . . C10 C 0.5335(2) 0.7500 0.0710(2) 0.0288(5) Uani 1 2 d S . . H10A H 0.5799 0.7925 0.1051 0.043 Uiso 0.50 1 calc PR . . H10B H 0.5784 0.7071 0.1050 0.043 Uiso 0.50 1 calc PR . . H10C H 0.4484 0.7505 0.0930 0.043 Uiso 1 2 calc SR . . C11 C 0.44976(18) 0.68334(13) -0.1179(2) 0.0417(5) Uani 1 1 d . . . H11A H 0.4972 0.6407 -0.0864 0.063 Uiso 1 1 calc R . . H11B H 0.4374 0.6832 -0.2083 0.063 Uiso 1 1 calc R . . H11C H 0.3673 0.6834 -0.0902 0.063 Uiso 1 1 calc R . . C12 C 1.00007(18) 0.7500 0.05115(19) 0.0217(4) Uani 1 2 d S . . C13 C 1.1256(2) 0.7500 0.0019(2) 0.0319(5) Uani 1 2 d S . . H13A H 1.1957 0.7500 0.0713 0.048 Uiso 1 2 calc SR . . H13B H 1.1307 0.7927 -0.0486 0.048 Uiso 0.50 1 calc PR . . H13C H 1.1307 0.7073 -0.0486 0.048 Uiso 0.50 1 calc PR . . C14 C 0.99557(18) 0.68382(12) 0.1308(2) 0.0387(4) Uani 1 1 d . . . H14A H 1.0684 0.6838 0.1974 0.058 Uiso 1 1 calc R . . H14B H 0.9981 0.6410 0.0799 0.058 Uiso 1 1 calc R . . H14C H 0.9173 0.6840 0.1662 0.058 Uiso 1 1 calc R . . O17 O 0.51222(19) 0.82195(11) -0.6075(2) 0.0189(3) Uani 0.50 1 d PD . 1 C15 C 0.7611(2) 0.77785(14) -0.6084(2) 0.0161(3) Uani 0.50 1 d PD . 1 H15A H 0.7208 0.7500 -0.6723 0.021 Uiso 1 2 d S A 1 H15B H 0.8506 0.7750 -0.6091 0.021 Uiso 0.50 1 d P B 1 C16 C 0.71814(15) 0.85315(8) -0.64043(19) 0.0149(3) Uani 0.50 1 d PGD . 1 C17 C 0.59079(14) 0.87028(10) -0.64944(19) 0.0156(3) Uani 0.50 1 d PGD . 1 C18 C 0.54838(16) 0.93772(13) -0.6893(3) 0.0188(3) Uani 0.50 1 d PGD . 1 C19 C 0.6333(2) 0.98803(13) -0.7201(4) 0.0158(3) Uani 0.50 1 d PGD . 1 H19 H 0.6043 1.0341 -0.7474 0.019 Uiso 0.50 1 calc PR . 1 C20 C 0.7607(2) 0.97090(12) -0.7111(3) 0.0190(5) Uani 0.50 1 d PGD . 1 C21 C 0.80307(13) 0.90346(11) -0.67126(19) 0.0158(3) Uani 0.50 1 d PGD . 1 H21 H 0.8901 0.8917 -0.6651 0.019 Uiso 0.50 1 calc PR . 1 C22 C 0.4023(4) 0.9546(3) -0.7128(7) 0.0185(5) Uani 0.50 1 d PD . 1 C23 C 0.3478(13) 0.9507(9) -0.5918(10) 0.0271(5) Uani 0.50 1 d PD . 1 H23A H 0.3923 0.9847 -0.5323 0.041 Uiso 0.50 1 calc PR . 1 H23B H 0.3588 0.9023 -0.5580 0.041 Uiso 0.50 1 calc PR . 1 H23C H 0.2576 0.9625 -0.6081 0.041 Uiso 0.50 1 calc PR . 1 C24 C 0.3755(7) 1.0297(3) -0.7667(7) 0.0287(9) Uani 0.50 1 d PD . 1 H24A H 0.4094 1.0337 -0.8441 0.043 Uiso 0.50 1 calc PR . 1 H24B H 0.4160 1.0652 -0.7077 0.043 Uiso 0.50 1 calc PR . 1 H24C H 0.2841 1.0380 -0.7825 0.043 Uiso 0.50 1 calc PR . 1 C25 C 0.3321(4) 0.9015(2) -0.8063(4) 0.0254(6) Uani 0.50 1 d PD . 1 H25A H 0.3671 0.9038 -0.8833 0.038 Uiso 0.50 1 calc PR . 1 H25B H 0.2420 0.9137 -0.8228 0.038 Uiso 0.50 1 calc PR . 1 H25C H 0.3424 0.8531 -0.7724 0.038 Uiso 0.50 1 calc PR . 1 C26 C 0.8536(10) 1.0286(6) -0.7458(12) 0.0204(6) Uani 0.50 1 d PD . 1 C27 C 0.9925(8) 1.0055(15) -0.715(2) 0.0265(16) Uani 0.50 1 d PD . 1 H27A H 1.0145 0.9967 -0.6266 0.040 Uiso 0.50 1 calc PR . 1 H27B H 1.0467 1.0434 -0.7395 0.040 Uiso 0.50 1 calc PR . 1 H27C H 1.0051 0.9617 -0.7607 0.040 Uiso 0.50 1 calc PR . 1 C28 C 0.838(3) 1.0977(7) -0.674(2) 0.0266(6) Uani 0.50 1 d PD . 1 H28A H 0.7501 1.1138 -0.6919 0.040 Uiso 0.50 1 calc PR . 1 H28B H 0.8937 1.1347 -0.6981 0.040 Uiso 0.50 1 calc PR . 1 H28C H 0.8606 1.0885 -0.5849 0.040 Uiso 0.50 1 calc PR . 1 C29 C 0.8228(17) 1.0430(7) -0.8854(12) 0.0299(14) Uani 0.50 1 d PD . 1 H29A H 0.7339 1.0571 -0.9071 0.045 Uiso 0.50 1 calc PR . 1 H29B H 0.8378 0.9996 -0.9307 0.045 Uiso 0.50 1 calc PR . 1 H29C H 0.8770 1.0815 -0.9073 0.045 Uiso 0.50 1 calc PR . 1 O17X O 0.52521(19) 0.83607(11) -0.5359(2) 0.0189(3) Uani 0.50 1 d PD . 2 C15X C 0.7855(2) 0.81825(14) -0.4568(3) 0.0161(3) Uani 0.50 1 d PD . 2 H15C H 0.8762 0.8165 -0.4498 0.021 Uiso 0.50 1 d P C 2 H15D H 0.7666 0.8329 -0.3771 0.021 Uiso 0.50 1 d P D 2 C16X C 0.73318(14) 0.87246(10) -0.55238(15) 0.0149(3) Uani 0.50 1 d PGD . 2 C17X C 0.60342(13) 0.88010(10) -0.58803(19) 0.0156(3) Uani 0.50 1 d PGD . 2 C18X C 0.55631(15) 0.93256(15) -0.6726(3) 0.0188(3) Uani 0.50 1 d PGD . 2 C19X C 0.6390(2) 0.97738(17) -0.7215(4) 0.0158(3) Uani 0.50 1 d PGD . 2 H19X H 0.6068 1.0132 -0.7793 0.019 Uiso 0.50 1 calc PR . 2 C20X C 0.7687(2) 0.96973(14) -0.6858(3) 0.0190(5) Uani 0.50 1 d PGD . 2 C21X C 0.81583(13) 0.91728(10) -0.60127(19) 0.0158(3) Uani 0.50 1 d PGD . 2 H21X H 0.9045 0.9121 -0.5769 0.019 Uiso 0.50 1 calc PR . 2 C22X C 0.4096(4) 0.9448(3) -0.7083(7) 0.0185(5) Uani 0.50 1 d PD . 2 C23X C 0.3472(13) 0.9548(9) -0.5932(10) 0.0271(5) Uani 0.50 1 d PD . 2 H23D H 0.3838 0.9966 -0.5470 0.041 Uiso 0.50 1 calc PR . 2 H23E H 0.3620 0.9123 -0.5408 0.041 Uiso 0.50 1 calc PR . 2 H23F H 0.2561 0.9619 -0.6181 0.041 Uiso 0.50 1 calc PR . 2 C24X C 0.3786(7) 1.0108(3) -0.7902(6) 0.0287(9) Uani 0.50 1 d PD . 2 H24D H 0.4175 1.0059 -0.8646 0.043 Uiso 0.50 1 calc PR . 2 H24E H 0.4118 1.0535 -0.7446 0.043 Uiso 0.50 1 calc PR . 2 H24F H 0.2868 1.0151 -0.8136 0.043 Uiso 0.50 1 calc PR . 2 C25X C 0.3532(4) 0.8798(2) -0.7822(4) 0.0254(6) Uani 0.50 1 d PD . 2 H25D H 0.3934 0.8741 -0.8557 0.038 Uiso 0.50 1 calc PR . 2 H25E H 0.2620 0.8868 -0.8074 0.038 Uiso 0.50 1 calc PR . 2 H25F H 0.3680 0.8369 -0.7308 0.038 Uiso 0.50 1 calc PR . 2 C26X C 0.8580(10) 1.0249(6) -0.7343(12) 0.0204(6) Uani 0.50 1 d PD . 2 C27X C 0.9983(8) 1.0057(15) -0.698(2) 0.0265(16) Uani 0.50 1 d PD . 2 H27D H 1.0198 1.0027 -0.6084 0.040 Uiso 0.50 1 calc PR . 2 H27E H 1.0501 1.0425 -0.7292 0.040 Uiso 0.50 1 calc PR . 2 H27F H 1.0145 0.9595 -0.7349 0.040 Uiso 0.50 1 calc PR . 2 C28X C 0.838(3) 1.0989(7) -0.679(2) 0.0266(6) Uani 0.50 1 d PD . 2 H28D H 0.7484 1.1123 -0.7001 0.040 Uiso 0.50 1 calc PR . 2 H28E H 0.8898 1.1342 -0.7138 0.040 Uiso 0.50 1 calc PR . 2 H28F H 0.8622 1.0973 -0.5895 0.040 Uiso 0.50 1 calc PR . 2 C29X C 0.8259(17) 1.0280(7) -0.8759(12) 0.0299(14) Uani 0.50 1 d PD . 2 H29D H 0.7368 1.0411 -0.9002 0.045 Uiso 0.50 1 calc PR . 2 H29E H 0.8411 0.9812 -0.9105 0.045 Uiso 0.50 1 calc PR . 2 H29F H 0.8794 1.0638 -0.9073 0.045 Uiso 0.50 1 calc PR . 2 O30 O 0.35911(18) 0.7500 -0.47004(18) 0.0394(5) Uani 1 2 d S . . C31 C 0.2431(4) 0.7500 -0.5556(4) 0.0596(10) Uani 1 2 d S . . H31A H 0.1716 0.7500 -0.5102 0.089 Uiso 1 2 calc SR . . H31B H 0.2392 0.7073 -0.6077 0.089 Uiso 0.50 1 calc PR . . H31C H 0.2392 0.7927 -0.6077 0.089 Uiso 0.50 1 calc PR . . 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 0.01414(15) 0.0219(13) 0.01410(15) -0.0004(3) 0.00187(11) -0.0009(3) N1 0.0144(7) 0.0278(8) 0.0126(6) 0.000 0.0032(5) 0.000 C2 0.0165(10) 0.0180(11) 0.0156(11) 0.0012(9) 0.0059(9) 0.0043(9) O4 0.0127(8) 0.0281(10) 0.0142(8) 0.0022(7) 0.0019(6) -0.0009(7) C3 0.0126(9) 0.0181(11) 0.0151(10) 0.0010(8) 0.0047(8) 0.0023(8) C4 0.0119(9) 0.0180(9) 0.0136(9) 0.0010(8) 0.0033(7) 0.0001(8) C5 0.0121(8) 0.043(3) 0.0144(8) 0.0056(13) 0.0033(6) -0.0071(12) C6 0.0104(7) 0.0292(10) 0.0158(7) 0.000 0.0041(6) 0.000 C7 0.0122(8) 0.021(3) 0.0167(9) 0.0008(8) 0.0033(7) 0.0038(8) C8 0.0108(9) 0.0217(11) 0.0169(10) -0.0001(9) 0.0046(8) 0.0018(8) C9 0.0103(7) 0.0291(9) 0.0159(7) 0.000 0.0047(6) 0.000 C10 0.0152(8) 0.0540(15) 0.0187(9) 0.000 0.0072(7) 0.000 C11 0.0222(8) 0.0460(11) 0.0552(12) -0.0236(10) 0.0005(8) -0.0050(7) C12 0.0107(7) 0.0355(11) 0.0189(8) 0.000 0.0025(6) 0.000 C13 0.0118(8) 0.0581(17) 0.0260(10) 0.000 0.0034(7) 0.000 C14 0.0207(7) 0.0439(11) 0.0519(11) 0.0167(9) 0.0068(7) 0.0047(7) O17 0.0149(6) 0.0197(7) 0.0230(6) 0.0012(6) 0.0051(6) -0.0003(5) C15 0.0160(7) 0.0176(8) 0.0149(8) 0.0005(6) 0.0033(6) 0.0022(6) C16 0.0134(7) 0.0165(7) 0.0149(7) -0.0007(6) 0.0025(5) 0.0009(6) C17 0.0126(7) 0.0166(8) 0.0179(8) -0.0020(7) 0.0036(7) -0.0004(6) C18 0.0134(6) 0.0162(7) 0.0272(10) -0.0029(6) 0.0045(6) 0.0021(5) C19 0.0119(5) 0.0127(9) 0.0233(6) -0.0044(7) 0.0040(5) 0.0022(5) C20 0.0141(6) 0.0178(6) 0.0256(15) 0.0026(7) 0.0043(7) 0.0021(5) C21 0.0113(7) 0.0188(8) 0.0175(7) 0.0008(6) 0.0026(6) 0.0029(6) C22 0.0106(6) 0.0225(15) 0.0222(7) -0.0037(10) 0.0022(5) 0.0008(7) C23 0.0159(6) 0.0400(16) 0.0262(7) -0.0066(8) 0.0057(5) 0.0054(8) C24 0.0140(7) 0.029(3) 0.042(2) 0.0048(17) 0.0015(13) 0.0040(17) C25 0.0157(14) 0.032(2) 0.0274(17) -0.0074(13) -0.0009(11) -0.0018(12) C26 0.0136(7) 0.0208(10) 0.0269(19) 0.0045(9) 0.0039(10) 0.0008(7) C27 0.0130(8) 0.0259(7) 0.041(5) 0.006(3) 0.0062(14) 0.0002(10) C28 0.0207(6) 0.0191(7) 0.0398(17) 0.0021(8) 0.0041(12) -0.0011(6) C29 0.0265(11) 0.035(5) 0.0292(18) 0.008(2) 0.0073(14) -0.002(3) O17X 0.0149(6) 0.0197(7) 0.0230(6) 0.0012(6) 0.0051(6) -0.0003(5) C15X 0.0160(7) 0.0176(8) 0.0149(8) 0.0005(6) 0.0033(6) 0.0022(6) C16X 0.0134(7) 0.0165(7) 0.0149(7) -0.0007(6) 0.0025(5) 0.0009(6) C17X 0.0126(7) 0.0166(8) 0.0179(8) -0.0020(7) 0.0036(7) -0.0004(6) C18X 0.0134(6) 0.0162(7) 0.0272(10) -0.0029(6) 0.0045(6) 0.0021(5) C19X 0.0119(5) 0.0127(9) 0.0233(6) -0.0044(7) 0.0040(5) 0.0022(5) C20X 0.0141(6) 0.0178(6) 0.0256(15) 0.0026(7) 0.0043(7) 0.0021(5) C21X 0.0113(7) 0.0188(8) 0.0175(7) 0.0008(6) 0.0026(6) 0.0029(6) C22X 0.0106(6) 0.0225(15) 0.0222(7) -0.0037(10) 0.0022(5) 0.0008(7) C23X 0.0159(6) 0.0400(16) 0.0262(7) -0.0066(8) 0.0057(5) 0.0054(8) C24X 0.0140(7) 0.029(3) 0.042(2) 0.0048(17) 0.0015(13) 0.0040(17) C25X 0.0157(14) 0.032(2) 0.0274(17) -0.0074(13) -0.0009(11) -0.0018(12) C26X 0.0136(7) 0.0208(10) 0.0269(19) 0.0045(9) 0.0039(10) 0.0008(7) C27X 0.0130(8) 0.0259(7) 0.041(5) 0.006(3) 0.0062(14) 0.0002(10) C28X 0.0207(6) 0.0191(7) 0.0398(17) 0.0021(8) 0.0041(12) -0.0011(6) C29X 0.0265(11) 0.035(5) 0.0292(18) 0.008(2) 0.0073(14) -0.002(3) O30 0.0197(8) 0.0704(15) 0.0260(8) 0.000 -0.0021(6) 0.000 C31 0.0410(18) 0.074(3) 0.060(2) 0.000 -0.0036(16) 0.000 _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 O30 1.786(2) . ? V1 O17X 1.810(5) 4_575 ? V1 O17 1.834(4) . ? V1 O4 1.888(3) . ? V1 N1 2.2794(17) . ? N1 C15X 1.406(3) . ? N1 C15X 1.406(3) 4_575 ? N1 C15 1.516(3) 4_575 ? N1 C15 1.516(3) . ? N1 C2 1.549(3) 4_575 ? N1 C2 1.549(3) . ? N1 V1 2.2794(17) 4_575 ? C2 C3 1.502(3) . ? O4 C4 1.366(2) . ? O4 C4 1.719(3) 4_575 ? O4 V1 1.827(2) 4_575 ? C3 C3 1.322(4) 4_575 ? C3 C4 1.3900 . ? C3 C8 1.3900 . ? C4 C5 1.3900 . ? C4 C5 1.505(3) 4_575 ? C5 C5 0.344(8) 4_575 ? C5 C6 1.3928 . ? C5 C4 1.505(2) 4_575 ? C5 C9 1.576(2) . ? C6 C7 1.3936 . ? C7 C8 1.3900 . ? C7 C8 1.546(2) 4_575 ? C7 C12 1.560(2) . ? C9 C10 1.527(3) . ? C9 C11 1.529(2) 4_575 ? C9 C11 1.529(2) . ? C9 C5 1.576(2) 4_575 ? C12 C14 1.523(2) 4_575 ? C12 C14 1.523(2) . ? C12 C13 1.528(3) . ? C12 C7 1.560(2) 4_575 ? O17 C17 1.366(2) . ? C15 C15 1.044(5) 4_575 ? C15 C16 1.508(3) . ? C16 C17 1.3900 . ? C16 C21 1.3900 . ? C17 C18 1.3900 . ? C18 C19 1.3900 . ? C18 C22 1.577(4) . ? C19 C20 1.3900 . ? C20 C21 1.3900 . ? C20 C26 1.559(5) . ? C22 C24 1.536(5) . ? C22 C23 1.536(5) . ? C22 C25 1.537(5) . ? C26 C27 1.535(5) . ? C26 C29 1.538(5) . ? C26 C28 1.542(5) . ? O17X C17X 1.366(2) . ? O17X V1 1.810(5) 4_575 ? C15X C16X 1.503(3) . ? C16X C17X 1.3900 . ? C16X C21X 1.3900 . ? C17X C18X 1.3900 . ? C18X C19X 1.3900 . ? C18X C22X 1.575(4) . ? C19X C20X 1.3900 . ? C20X C21X 1.3900 . ? C20X C26X 1.559(5) . ? C22X C24X 1.533(6) . ? C22X C23X 1.534(5) . ? C22X C25X 1.534(5) . ? C26X C27X 1.534(5) . ? C26X C29X 1.538(6) . ? C26X C28X 1.542(6) . ? O30 C31 1.432(4) . ? O30 V1 1.786(2) 4_575 ? 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 V1 V1 O17X 159.07(11) 4_575 . ? V1 V1 O30 86.72(17) 4_575 . ? O17X V1 O30 98.99(19) . . ? O30 V1 O17X 92.17(19) . 4_575 ? V1 V1 O4 104.63(18) 4_575 4_575 ? O17X V1 O4 95.3(3) . 4_575 ? O30 V1 O4 91.90(10) . 4_575 ? O17X V1 O4 122.2(2) 4_575 4_575 ? O30 V1 O17 99.10(15) . . ? O17X V1 O17 114.31(13) 4_575 . ? O4 V1 O17 121.8(3) 4_575 . ? O17X V1 O4 130.3(2) . . ? O30 V1 O4 89.88(11) . . ? O17X V1 O4 87.2(2) 4_575 . ? O17 V1 O4 156.1(3) . . ? O17X V1 O17 116.35(12) . 4_575 ? O30 V1 O17 93.94(16) . 4_575 ? O4 V1 O17 146.3(3) 4_575 4_575 ? O17 V1 O17 89.96(14) . 4_575 ? O4 V1 O17 111.6(3) . 4_575 ? V1 V1 N1 87.44(14) 4_575 . ? O17X V1 N1 87.98(13) . . ? O30 V1 N1 172.7(2) . . ? O17X V1 N1 83.61(13) 4_575 . ? O4 V1 N1 85.42(8) 4_575 . ? O17 V1 N1 88.03(11) . . ? O4 V1 N1 84.03(9) . . ? O17 V1 N1 84.67(11) 4_575 . ? C15X N1 C15X 131.0(2) . 4_575 ? C15X N1 C15 113.08(18) . 4_575 ? C15X N1 C2 110.58(19) 4_575 4_575 ? C15 N1 C2 133.76(17) 4_575 4_575 ? C15 N1 C2 103.04(15) . 4_575 ? C15X N1 C2 110.58(19) . . ? C15 N1 C2 103.04(15) 4_575 . ? C15 N1 C2 133.76(17) . . ? C2 N1 C2 85.2(2) 4_575 . ? C15X N1 V1 107.92(18) . . ? C15X N1 V1 112.90(18) 4_575 . ? C15 N1 V1 110.60(14) 4_575 . ? C15 N1 V1 108.72(14) . . ? C2 N1 V1 107.95(16) 4_575 . ? C2 N1 V1 111.64(15) . . ? C15X N1 V1 112.91(18) . 4_575 ? C15X N1 V1 107.92(18) 4_575 4_575 ? C15 N1 V1 108.72(14) 4_575 4_575 ? C15 N1 V1 110.60(14) . 4_575 ? C2 N1 V1 111.64(16) 4_575 4_575 ? C2 N1 V1 107.95(15) . 4_575 ? C3 C2 N1 110.84(18) . . ? C4 O4 V1 138.33(17) . 4_575 ? C4 O4 V1 116.86(19) 4_575 4_575 ? C4 O4 V1 135.74(17) . . ? C4 O4 V1 111.79(18) 4_575 . ? C4 C3 C8 120.0 . . ? C3 C3 C2 104.93(13) 4_575 . ? C4 C3 C2 119.24(14) . . ? C8 C3 C2 120.72(14) . . ? C8 C3 C4 109.64(5) . 4_575 ? C2 C3 C4 121.20(16) . 4_575 ? C4 C3 C8 107.9 . 4_575 ? C2 C3 C8 122.57(18) . 4_575 ? O4 C4 C3 118.58(13) . . ? O4 C4 C5 121.36(13) . . ? C3 C4 C5 120.0 . . ? O4 C4 C5 119.60(16) . 4_575 ? C3 C4 C5 119.4 . 4_575 ? C3 C4 O4 117.64(13) . 4_575 ? C5 C4 O4 105.48(11) . 4_575 ? O4 C4 C3 114.47(15) . 4_575 ? C5 C4 C3 102.87(11) . 4_575 ? C5 C5 C4 102.9 4_575 . ? C6 C5 C4 120.2 . . ? C6 C5 C4 113.04(6) . 4_575 ? C6 C5 C9 118.24(11) . . ? C4 C5 C9 121.54(11) . . ? C4 C5 C9 114.4(2) 4_575 . ? C5 C6 C7 119.5 . . ? C8 C7 C6 120.2 . . ? C6 C7 C8 110.64(5) . 4_575 ? C8 C7 C12 122.61(11) . . ? C6 C7 C12 117.11(11) . . ? C8 C7 C12 112.93(17) 4_575 . ? C7 C8 C3 120.0 . . ? C10 C9 C11 107.43(14) . 4_575 ? C10 C9 C11 107.43(14) . . ? C11 C9 C11 109.6(2) 4_575 . ? C10 C9 C5 111.49(15) . 4_575 ? C11 C9 C5 104.81(16) 4_575 4_575 ? C11 C9 C5 115.74(18) . 4_575 ? C10 C9 C5 111.49(15) . . ? C11 C9 C5 115.74(18) 4_575 . ? C11 C9 C5 104.81(16) . . ? C14 C12 C14 109.1(2) 4_575 . ? C14 C12 C13 108.32(12) 4_575 . ? C14 C12 C13 108.32(12) . . ? C14 C12 C7 115.81(15) 4_575 . ? C14 C12 C7 102.06(15) . . ? C13 C12 C7 112.84(16) . . ? C14 C12 C7 102.06(15) 4_575 4_575 ? C14 C12 C7 115.80(15) . 4_575 ? C13 C12 C7 112.84(17) . 4_575 ? C17 O17 V1 137.15(17) . . ? C17 O17 V1 138.42(16) . 4_575 ? C16 C15 N1 115.85(18) . . ? C17 C16 C21 120.0 . . ? C17 C16 C15 119.47(15) . . ? C21 C16 C15 120.30(15) . . ? O17 C17 C16 118.32(15) . . ? O17 C17 C18 121.40(15) . . ? C16 C17 C18 120.0 . . ? C19 C18 C17 120.0 . . ? C19 C18 C22 119.7(3) . . ? C17 C18 C22 120.0(3) . . ? C18 C19 C20 120.0 . . ? C21 C20 C19 120.0 . . ? C21 C20 C26 121.2(5) . . ? C19 C20 C26 118.8(5) . . ? C20 C21 C16 120.0 . . ? C24 C22 C23 107.7(6) . . ? C24 C22 C25 107.2(4) . . ? C23 C22 C25 109.4(6) . . ? C24 C22 C18 111.5(4) . . ? C23 C22 C18 110.8(6) . . ? C25 C22 C18 110.2(4) . . ? C27 C26 C29 108.1(6) . . ? C27 C26 C28 107.9(7) . . ? C29 C26 C28 109.9(7) . . ? C27 C26 C20 112.8(7) . . ? C29 C26 C20 108.8(6) . . ? C28 C26 C20 109.3(7) . . ? C17X O17X V1 139.41(17) . . ? C17X O17X V1 138.32(16) . 4_575 ? N1 C15X C16X 111.8(2) . . ? C17X C16X C21X 120.0 . . ? C17X C16X C15X 120.66(15) . . ? C21X C16X C15X 119.28(15) . . ? O17X C17X C16X 118.26(15) . . ? O17X C17X C18X 121.73(15) . . ? C16X C17X C18X 120.0 . . ? C17X C18X C19X 120.0 . . ? C17X C18X C22X 120.7(3) . . ? C19X C18X C22X 119.2(3) . . ? C20X C19X C18X 120.0 . . ? C21X C20X C19X 120.0 . . ? C21X C20X C26X 121.3(4) . . ? C19X C20X C26X 118.5(4) . . ? C20X C21X C16X 120.0 . . ? C24X C22X C23X 107.6(6) . . ? C24X C22X C25X 107.5(5) . . ? C23X C22X C25X 110.3(6) . . ? C24X C22X C18X 112.1(5) . . ? C23X C22X C18X 111.3(6) . . ? C25X C22X C18X 108.0(4) . . ? C27X C26X C29X 108.5(6) . . ? C27X C26X C28X 107.7(7) . . ? C29X C26X C28X 109.7(7) . . ? C27X C26X C20X 112.7(7) . . ? C29X C26X C20X 108.7(6) . . ? C28X C26X C20X 109.3(7) . . ? C31 O30 V1 134.8(2) . 4_575 ? C31 O30 V1 134.8(2) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 33.22 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.533 _refine_diff_density_min -1.153 _refine_diff_density_rms 0.076 #===END data_3 _database_code_depnum_ccdc_archive 'CCDC 824887' #TrackingRef '- Wagner6_Vanadium.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_formula_moiety 'C50 H73 N O5 V' _chemical_formula_sum 'C50 H73 N O5 V' _chemical_formula_weight 819.03 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 'P n' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y, z+1/2' _cell_length_a 14.2584(9) _cell_length_b 19.0279(12) _cell_length_c 17.548(2) _cell_angle_alpha 90.00 _cell_angle_beta 91.14(1) _cell_angle_gamma 90.00 _cell_volume 4760.0(7) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 82567 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 30.03 _exptl_crystal_description 'transparent parallelepiped' _exptl_crystal_colour 'dark violet' _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.143 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1772 _exptl_absorpt_coefficient_mu 0.252 _exptl_absorpt_correction_type Gaussian _exptl_absorpt_correction_T_min 0.952 _exptl_absorpt_correction_T_max 0.989 _exptl_absorpt_process_details 'SADABS 2008/1, Bruker AXS (2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Nonius Kappa-CCD' _diffrn_measurement_method '379 images at 1 deg. in \w, 160 sec./frame' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 32678 _diffrn_reflns_av_R_equivalents 0.0774 _diffrn_reflns_av_sigmaI/netI 0.1036 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.21 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13092 _reflns_number_gt 10086 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect Software' _computing_cell_refinement 'Nonius Collect Software' _computing_data_reduction 'Nonius Collect Software' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0485P)^2^+4.9908P] 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(3) _refine_ls_number_reflns 13092 _refine_ls_number_parameters 1067 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0953 _refine_ls_R_factor_gt 0.0670 _refine_ls_wR_factor_ref 0.1443 _refine_ls_wR_factor_gt 0.1319 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 0.44789(6) 0.58361(5) 0.75283(6) 0.0234(2) Uani 1 1 d . . . N1 N 0.5768(3) 0.5380(2) 0.7102(3) 0.0207(11) Uani 1 1 d . . . C2 C 0.5872(4) 0.5573(3) 0.6281(3) 0.0235(14) Uani 1 1 d . . . H2A H 0.6459 0.5360 0.6098 0.028 Uiso 1 1 calc R . . H2B H 0.5942 0.6089 0.6247 0.028 Uiso 1 1 calc R . . C3 C 0.5084(4) 0.5354(3) 0.5751(3) 0.0206(13) Uani 1 1 d . . . O4 O 0.3969(2) 0.53508(19) 0.6719(2) 0.0247(9) Uani 1 1 d . . . C4 C 0.4174(4) 0.5236(3) 0.5985(3) 0.0219(13) Uani 1 1 d . . . C5 C 0.3492(4) 0.4952(3) 0.5494(4) 0.0288(15) Uani 1 1 d . . . C6 C 0.3730(4) 0.4890(3) 0.4731(4) 0.0273(14) Uani 1 1 d . . . H6 H 0.3262 0.4729 0.4380 0.033 Uiso 1 1 calc R . . C7 C 0.4609(4) 0.5049(3) 0.4451(4) 0.0236(13) Uani 1 1 d . . . C8 C 0.5282(4) 0.5266(3) 0.4980(4) 0.0248(14) Uani 1 1 d . . . H8 H 0.5900 0.5359 0.4813 0.030 Uiso 1 1 calc R . . C9 C 0.2534(4) 0.4693(3) 0.5787(4) 0.0320(15) Uani 1 1 d . . . C10 C 0.1968(4) 0.5300(3) 0.6107(4) 0.0389(17) Uani 1 1 d . . . H10A H 0.1860 0.5653 0.5708 0.058 Uiso 1 1 calc R . . H10B H 0.2317 0.5514 0.6535 0.058 Uiso 1 1 calc R . . H10C H 0.1364 0.5125 0.6284 0.058 Uiso 1 1 calc R . . C11 C 0.2713(4) 0.4126(3) 0.6413(4) 0.0375(17) Uani 1 1 d . . . H11A H 0.3089 0.4330 0.6831 0.056 Uiso 1 1 calc R . . H11B H 0.3053 0.3728 0.6194 0.056 Uiso 1 1 calc R . . H11C H 0.2112 0.3962 0.6608 0.056 Uiso 1 1 calc R . . C12 C 0.1943(4) 0.4341(4) 0.5150(4) 0.0452(18) Uani 1 1 d . . . H12A H 0.1339 0.4192 0.5354 0.068 Uiso 1 1 calc R . . H12B H 0.2278 0.3930 0.4958 0.068 Uiso 1 1 calc R . . H12C H 0.1834 0.4677 0.4734 0.068 Uiso 1 1 calc R . . C13 C 0.4806(4) 0.4957(3) 0.3600(4) 0.0295(15) Uani 1 1 d . . . C14 C 0.4643(4) 0.4174(3) 0.3375(4) 0.0385(17) Uani 1 1 d . . . H14A H 0.4792 0.4108 0.2837 0.058 Uiso 1 1 calc R . . H14B H 0.3986 0.4049 0.3455 0.058 Uiso 1 1 calc R . . H14C H 0.5050 0.3873 0.3691 0.058 Uiso 1 1 calc R . . C15 C 0.5782(4) 0.5154(4) 0.3378(4) 0.0447(18) Uani 1 1 d . . . H15A H 0.5852 0.5082 0.2829 0.067 Uiso 1 1 calc R . . H15B H 0.6235 0.4860 0.3659 0.067 Uiso 1 1 calc R . . H15C H 0.5895 0.5650 0.3502 0.067 Uiso 1 1 calc R . . C16 C 0.4103(5) 0.5386(4) 0.3132(4) 0.050(2) Uani 1 1 d . . . H16A H 0.4210 0.5887 0.3225 0.075 Uiso 1 1 calc R . . H16B H 0.3465 0.5262 0.3281 0.075 Uiso 1 1 calc R . . H16C H 0.4180 0.5284 0.2590 0.075 Uiso 1 1 calc R . . C22 C 0.6642(4) 0.5603(3) 0.7514(3) 0.0209(13) Uani 1 1 d . . . H22A H 0.7188 0.5426 0.7230 0.025 Uiso 1 1 calc R . . H22B H 0.6659 0.5378 0.8022 0.025 Uiso 1 1 calc R . . C23 C 0.6748(4) 0.6383(3) 0.7617(3) 0.0199(13) Uani 1 1 d . . . O24 O 0.5248(2) 0.63739(19) 0.8140(2) 0.0267(10) Uani 1 1 d . . . C24 C 0.6036(4) 0.6734(3) 0.7988(3) 0.0231(13) Uani 1 1 d . . . C25 C 0.6164(4) 0.7446(3) 0.8214(3) 0.0254(14) Uani 1 1 d . . . C26 C 0.7005(4) 0.7750(3) 0.8041(4) 0.0297(15) Uani 1 1 d . . . H26 H 0.7104 0.8220 0.8207 0.036 Uiso 1 1 calc R . . C27 C 0.7732(4) 0.7431(3) 0.7642(4) 0.0270(14) Uani 1 1 d . . . C28 C 0.7568(4) 0.6727(3) 0.7444(3) 0.0234(13) Uani 1 1 d . . . H28 H 0.8039 0.6478 0.7181 0.028 Uiso 1 1 calc R . . C29 C 0.5421(4) 0.7830(3) 0.8698(4) 0.0345(16) Uani 1 1 d . . . C30 C 0.5254(4) 0.7423(3) 0.9439(4) 0.0359(16) Uani 1 1 d . . . H30A H 0.4752 0.7651 0.9722 0.054 Uiso 1 1 calc R . . H30B H 0.5832 0.7419 0.9751 0.054 Uiso 1 1 calc R . . H30C H 0.5071 0.6939 0.9316 0.054 Uiso 1 1 calc R . . C31 C 0.5736(5) 0.8576(3) 0.8919(4) 0.0400(17) Uani 1 1 d . . . H31A H 0.5833 0.8854 0.8456 0.060 Uiso 1 1 calc R . . H31B H 0.6325 0.8552 0.9216 0.060 Uiso 1 1 calc R . . H31C H 0.5253 0.8799 0.9226 0.060 Uiso 1 1 calc R . . C32 C 0.4497(4) 0.7881(3) 0.8249(4) 0.0404(18) Uani 1 1 d . . . H32A H 0.4253 0.7408 0.8151 0.061 Uiso 1 1 calc R . . H32B H 0.4602 0.8120 0.7764 0.061 Uiso 1 1 calc R . . H32C H 0.4043 0.8148 0.8545 0.061 Uiso 1 1 calc R . . C33 C 0.8656(4) 0.7794(3) 0.7509(4) 0.0307(15) Uani 1 1 d . . . C34 C 0.8513(4) 0.8573(3) 0.7263(4) 0.0354(16) Uani 1 1 d . . . H34A H 0.8174 0.8589 0.6771 0.053 Uiso 1 1 calc R . . H34B H 0.9125 0.8801 0.7213 0.053 Uiso 1 1 calc R . . H34C H 0.8149 0.8820 0.7648 0.053 Uiso 1 1 calc R . . C35 C 0.9243(4) 0.7441(3) 0.6907(4) 0.0405(17) Uani 1 1 d . . . H35A H 0.9392 0.6960 0.7068 0.061 Uiso 1 1 calc R . . H35B H 0.9827 0.7705 0.6843 0.061 Uiso 1 1 calc R . . H35C H 0.8891 0.7429 0.6422 0.061 Uiso 1 1 calc R . . C36 C 0.9220(5) 0.7793(3) 0.8280(4) 0.0427(18) Uani 1 1 d . . . H36A H 0.8876 0.8062 0.8660 0.064 Uiso 1 1 calc R . . H36B H 0.9836 0.8009 0.8207 0.064 Uiso 1 1 calc R . . H36C H 0.9302 0.7309 0.8457 0.064 Uiso 1 1 calc R . . C42 C 0.5708(4) 0.4586(3) 0.7178(4) 0.0253(14) Uani 1 1 d . . . H42A H 0.5151 0.4417 0.6887 0.030 Uiso 1 1 calc R . . H42B H 0.6270 0.4373 0.6949 0.030 Uiso 1 1 calc R . . C43 C 0.5642(4) 0.4339(3) 0.7996(3) 0.0232(14) Uani 1 1 d . . . O44 O 0.4353(2) 0.5111(2) 0.8231(2) 0.0262(10) Uani 1 1 d . . . C44 C 0.4938(4) 0.4602(3) 0.8472(3) 0.0214(13) Uani 1 1 d . . . C45 C 0.4830(4) 0.4321(3) 0.9213(4) 0.0245(14) Uani 1 1 d . . . C46 C 0.5451(4) 0.3786(3) 0.9441(4) 0.0254(14) Uani 1 1 d . . . H46 H 0.5381 0.3589 0.9934 0.031 Uiso 1 1 calc R . . C47 C 0.6160(4) 0.3526(3) 0.8991(4) 0.0235(14) Uani 1 1 d . . . C48 C 0.6246(4) 0.3816(3) 0.8263(3) 0.0244(14) Uani 1 1 d . . . H48 H 0.6729 0.3651 0.7944 0.029 Uiso 1 1 calc R . . C49 C 0.4045(4) 0.4581(3) 0.9732(4) 0.0280(15) Uani 1 1 d . . . C50 C 0.4171(4) 0.5376(3) 0.9895(4) 0.0374(16) Uani 1 1 d . . . H50A H 0.4123 0.5639 0.9416 0.056 Uiso 1 1 calc R . . H50B H 0.4788 0.5458 1.0134 0.056 Uiso 1 1 calc R . . H50C H 0.3681 0.5535 1.0239 0.056 Uiso 1 1 calc R . . C51 C 0.3092(4) 0.4450(3) 0.9349(4) 0.0350(16) Uani 1 1 d . . . H51A H 0.3045 0.4720 0.8874 0.053 Uiso 1 1 calc R . . H51B H 0.2594 0.4597 0.9691 0.053 Uiso 1 1 calc R . . H51C H 0.3023 0.3948 0.9235 0.053 Uiso 1 1 calc R . . C52 C 0.4052(4) 0.4192(4) 1.0497(4) 0.0372(16) Uani 1 1 d . . . H52A H 0.3539 0.4367 1.0808 0.056 Uiso 1 1 calc R . . H52B H 0.4652 0.4273 1.0764 0.056 Uiso 1 1 calc R . . H52C H 0.3969 0.3687 1.0407 0.056 Uiso 1 1 calc R . . C53 C 0.6832(4) 0.2939(3) 0.9261(4) 0.0279(14) Uani 1 1 d . . . C54 C 0.7826(4) 0.3231(3) 0.9354(4) 0.0320(15) Uani 1 1 d . . . H54A H 0.7849 0.3566 0.9777 0.048 Uiso 1 1 calc R . . H54B H 0.8004 0.3469 0.8883 0.048 Uiso 1 1 calc R . . H54C H 0.8264 0.2844 0.9460 0.048 Uiso 1 1 calc R . . C55 C 0.6534(4) 0.2619(3) 1.0020(4) 0.0366(16) Uani 1 1 d . . . H55A H 0.6969 0.2241 1.0166 0.055 Uiso 1 1 calc R . . H55B H 0.5898 0.2427 0.9964 0.055 Uiso 1 1 calc R . . H55C H 0.6544 0.2983 1.0415 0.055 Uiso 1 1 calc R . . C56 C 0.6845(4) 0.2341(3) 0.8656(4) 0.0389(17) Uani 1 1 d . . . H56A H 0.7287 0.1974 0.8823 0.058 Uiso 1 1 calc R . . H56B H 0.7042 0.2532 0.8166 0.058 Uiso 1 1 calc R . . H56C H 0.6215 0.2139 0.8599 0.058 Uiso 1 1 calc R . . C61 C 0.1772(4) 0.6731(4) 0.7799(5) 0.049(2) Uani 1 1 d . . . H61A H 0.1422 0.6296 0.7702 0.074 Uiso 1 1 calc R . . H61B H 0.1449 0.7124 0.7546 0.074 Uiso 1 1 calc R . . H61C H 0.1810 0.6818 0.8350 0.074 Uiso 1 1 calc R . . O62 O 0.3263(3) 0.6213(2) 0.7846(2) 0.0296(10) Uani 1 1 d . . . C62 C 0.2741(4) 0.6662(3) 0.7494(4) 0.0287(15) Uani 1 1 d . . . C63 C 0.3010(4) 0.7084(3) 0.6888(4) 0.0296(15) Uani 1 1 d . . . H63 H 0.2552 0.7387 0.6664 0.036 Uiso 1 1 calc R . . O64 O 0.4564(2) 0.6670(2) 0.6785(2) 0.0247(10) Uani 1 1 d . . . C64 C 0.3910(4) 0.7090(3) 0.6590(3) 0.0217(13) Uani 1 1 d . . . C65 C 0.4164(4) 0.7632(3) 0.6014(4) 0.0372(17) Uani 1 1 d . . . H65A H 0.4707 0.7902 0.6202 0.056 Uiso 1 1 calc R . . H65B H 0.3632 0.7950 0.5926 0.056 Uiso 1 1 calc R . . H65C H 0.4321 0.7401 0.5534 0.056 Uiso 1 1 calc R . . V2 V 0.48354(6) 1.09468(5) 0.64735(6) 0.0236(2) Uani 1 1 d . . . N101 N 0.6050(3) 1.0393(2) 0.6957(3) 0.0190(10) Uani 1 1 d . . . C102 C 0.5887(4) 0.9607(3) 0.6905(3) 0.0201(13) Uani 1 1 d . . . H10D H 0.5313 0.9486 0.7184 0.024 Uiso 1 1 calc R . . H10E H 0.6421 0.9360 0.7156 0.024 Uiso 1 1 calc R . . C103 C 0.5784(3) 0.9350(3) 0.6089(3) 0.0193(13) Uani 1 1 d . . . O104 O 0.4660(2) 1.02284(18) 0.5772(2) 0.0244(9) Uani 1 1 d . . . C104 C 0.5147(3) 0.9654(3) 0.5577(4) 0.0221(13) Uani 1 1 d . . . C105 C 0.4982(4) 0.9363(3) 0.4844(3) 0.0218(13) Uani 1 1 d . . . C106 C 0.5516(4) 0.8780(3) 0.4650(4) 0.0259(14) Uani 1 1 d . . . H106 H 0.5414 0.8580 0.4160 0.031 Uiso 1 1 calc R . . C107 C 0.6186(4) 0.8473(3) 0.5126(3) 0.0226(13) Uani 1 1 d . . . C108 C 0.6299(4) 0.8769(3) 0.5857(3) 0.0216(13) Uani 1 1 d . . . H108 H 0.6742 0.8566 0.6204 0.026 Uiso 1 1 calc R . . C109 C 0.4210(4) 0.9666(3) 0.4324(4) 0.0290(15) Uani 1 1 d . . . C110 C 0.4387(4) 1.0454(3) 0.4153(4) 0.0392(17) Uani 1 1 d . . . H11D H 0.5010 1.0510 0.3935 0.059 Uiso 1 1 calc R . . H11E H 0.4355 1.0724 0.4627 0.059 Uiso 1 1 calc R . . H11F H 0.3909 1.0625 0.3790 0.059 Uiso 1 1 calc R . . C111 C 0.3254(4) 0.9591(3) 0.4700(4) 0.0404(18) Uani 1 1 d . . . H11G H 0.2758 0.9748 0.4344 0.061 Uiso 1 1 calc R . . H11H H 0.3243 0.9880 0.5162 0.061 Uiso 1 1 calc R . . H11I H 0.3150 0.9098 0.4834 0.061 Uiso 1 1 calc R . . C112 C 0.4159(5) 0.9295(4) 0.3559(4) 0.053(2) Uani 1 1 d . . . H11J H 0.4753 0.9359 0.3295 0.079 Uiso 1 1 calc R . . H11K H 0.3645 0.9494 0.3249 0.079 Uiso 1 1 calc R . . H11L H 0.4047 0.8793 0.3638 0.079 Uiso 1 1 calc R . . C113 C 0.6793(4) 0.7840(3) 0.4892(3) 0.0229(13) Uani 1 1 d . . . C114 C 0.7815(4) 0.8071(3) 0.4859(4) 0.0337(16) Uani 1 1 d . . . H11M H 0.8209 0.7666 0.4735 0.050 Uiso 1 1 calc R . . H11N H 0.8014 0.8264 0.5354 0.050 Uiso 1 1 calc R . . H11O H 0.7880 0.8433 0.4465 0.050 Uiso 1 1 calc R . . C115 C 0.6494(4) 0.7547(3) 0.4117(4) 0.0361(16) Uani 1 1 d . . . H11P H 0.6596 0.7903 0.3724 0.054 Uiso 1 1 calc R . . H11Q H 0.5827 0.7422 0.4124 0.054 Uiso 1 1 calc R . . H11R H 0.6865 0.7127 0.4006 0.054 Uiso 1 1 calc R . . C116 C 0.6703(4) 0.7250(3) 0.5485(4) 0.0368(16) Uani 1 1 d . . . H11S H 0.6049 0.7095 0.5502 0.055 Uiso 1 1 calc R . . H11T H 0.6902 0.7426 0.5988 0.055 Uiso 1 1 calc R . . H11U H 0.7102 0.6854 0.5343 0.055 Uiso 1 1 calc R . . C122 C 0.6955(4) 1.0531(3) 0.6582(3) 0.0208(13) Uani 1 1 d . . . H12D H 0.6929 1.0325 0.6064 0.025 Uiso 1 1 calc R . . H12E H 0.7462 1.0289 0.6873 0.025 Uiso 1 1 calc R . . C123 C 0.7203(4) 1.1302(3) 0.6518(3) 0.0229(13) Uani 1 1 d . . . O124 O 0.5713(2) 1.14605(18) 0.5955(2) 0.0237(9) Uani 1 1 d . . . C124 C 0.6559(4) 1.1738(3) 0.6137(3) 0.0232(13) Uani 1 1 d . . . C125 C 0.6820(4) 1.2440(3) 0.5926(3) 0.0231(13) Uani 1 1 d . . . C126 C 0.7711(4) 1.2644(3) 0.6153(3) 0.0246(14) Uani 1 1 d . . . H126 H 0.7904 1.3104 0.6017 0.029 Uiso 1 1 calc R . . C127 C 0.8351(4) 1.2237(3) 0.6564(3) 0.0251(14) Uani 1 1 d . . . C128 C 0.8071(4) 1.1552(3) 0.6735(3) 0.0198(12) Uani 1 1 d . . . H128 H 0.8492 1.1253 0.7009 0.024 Uiso 1 1 calc R . . C129 C 0.6173(4) 1.2878(3) 0.5423(4) 0.0305(15) Uani 1 1 d . . . C130 C 0.6629(4) 1.3583(3) 0.5214(4) 0.0383(17) Uani 1 1 d . . . H13A H 0.6788 1.3844 0.5681 0.057 Uiso 1 1 calc R . . H13B H 0.6190 1.3859 0.4900 0.057 Uiso 1 1 calc R . . H13C H 0.7201 1.3495 0.4929 0.057 Uiso 1 1 calc R . . C131 C 0.5972(5) 1.2483(3) 0.4676(4) 0.0447(19) Uani 1 1 d . . . H13D H 0.6566 1.2363 0.4436 0.067 Uiso 1 1 calc R . . H13E H 0.5598 1.2781 0.4332 0.067 Uiso 1 1 calc R . . H13F H 0.5624 1.2051 0.4784 0.067 Uiso 1 1 calc R . . C132 C 0.5255(4) 1.3035(3) 0.5826(4) 0.0428(19) Uani 1 1 d . . . H13G H 0.4887 1.2602 0.5867 0.064 Uiso 1 1 calc R . . H13H H 0.4895 1.3384 0.5533 0.064 Uiso 1 1 calc R . . H13I H 0.5394 1.3219 0.6338 0.064 Uiso 1 1 calc R . . C133 C 0.9316(4) 1.2514(3) 0.6833(4) 0.0251(14) Uani 1 1 d . . . C134 C 0.9281(4) 1.2645(3) 0.7695(4) 0.0347(16) Uani 1 1 d . . . H13J H 0.9899 1.2800 0.7884 0.052 Uiso 1 1 calc R . . H13K H 0.9105 1.2210 0.7955 0.052 Uiso 1 1 calc R . . H13L H 0.8815 1.3010 0.7798 0.052 Uiso 1 1 calc R . . C135 C 0.9575(4) 1.3209(3) 0.6456(4) 0.0337(15) Uani 1 1 d . . . H13M H 0.9134 1.3575 0.6611 0.051 Uiso 1 1 calc R . . H13N H 0.9542 1.3155 0.5900 0.051 Uiso 1 1 calc R . . H13O H 1.0213 1.3343 0.6614 0.051 Uiso 1 1 calc R . . C136 C 1.0087(4) 1.1976(3) 0.6682(4) 0.0378(17) Uani 1 1 d . . . H13P H 1.0104 1.1876 0.6135 0.057 Uiso 1 1 calc R . . H13Q H 0.9956 1.1542 0.6961 0.057 Uiso 1 1 calc R . . H13R H 1.0694 1.2167 0.6853 0.057 Uiso 1 1 calc R . . C142 C 0.6152(4) 1.0605(3) 0.7770(3) 0.0222(13) Uani 1 1 d . . . H14D H 0.6282 1.1116 0.7787 0.027 Uiso 1 1 calc R . . H14E H 0.6707 1.0362 0.7991 0.027 Uiso 1 1 calc R . . C143 C 0.5323(4) 1.0458(3) 0.8273(4) 0.0220(14) Uani 1 1 d . . . O144 O 0.4238(2) 1.0478(2) 0.7239(2) 0.0275(10) Uani 1 1 d . . . C144 C 0.4407(4) 1.0379(3) 0.7988(3) 0.0206(13) Uani 1 1 d . . . C145 C 0.3686(4) 1.0155(3) 0.8464(4) 0.0276(15) Uani 1 1 d . . . C146 C 0.3894(4) 1.0117(3) 0.9243(4) 0.0285(15) Uani 1 1 d . . . H146 H 0.3403 0.9996 0.9576 0.034 Uiso 1 1 calc R . . C147 C 0.4779(4) 1.0246(3) 0.9561(4) 0.0247(14) Uani 1 1 d . . . C148 C 0.5481(4) 1.0409(3) 0.9054(4) 0.0243(14) Uani 1 1 d . . . H148 H 0.6097 1.0491 0.9251 0.029 Uiso 1 1 calc R . . C149 C 0.2708(4) 0.9973(3) 0.8144(4) 0.0329(15) Uani 1 1 d . . . C150 C 0.2787(4) 0.9397(3) 0.7503(4) 0.0406(17) Uani 1 1 d . . . H15D H 0.3140 0.9587 0.7076 0.061 Uiso 1 1 calc R . . H15E H 0.2157 0.9261 0.7324 0.061 Uiso 1 1 calc R . . H15F H 0.3113 0.8983 0.7710 0.061 Uiso 1 1 calc R . . C151 C 0.2235(4) 1.0621(4) 0.7803(4) 0.0466(19) Uani 1 1 d . . . H15G H 0.2233 1.0999 0.8182 0.070 Uiso 1 1 calc R . . H15H H 0.1588 1.0506 0.7651 0.070 Uiso 1 1 calc R . . H15I H 0.2580 1.0776 0.7355 0.070 Uiso 1 1 calc R . . C152 C 0.2069(5) 0.9661(4) 0.8747(5) 0.058(2) Uani 1 1 d . . . H15J H 0.2366 0.9242 0.8969 0.087 Uiso 1 1 calc R . . H15K H 0.1466 0.9531 0.8509 0.087 Uiso 1 1 calc R . . H15L H 0.1966 1.0009 0.9148 0.087 Uiso 1 1 calc R . . C153 C 0.4990(4) 1.0229(3) 1.0424(4) 0.0269(14) Uani 1 1 d . . . C154 C 0.5315(4) 1.0972(3) 1.0682(4) 0.0356(16) Uani 1 1 d . . . H15M H 0.4809 1.1310 1.0584 0.053 Uiso 1 1 calc R . . H15N H 0.5869 1.1109 1.0395 0.053 Uiso 1 1 calc R . . H15O H 0.5473 1.0964 1.1228 0.053 Uiso 1 1 calc R . . C155 C 0.4136(4) 1.0026(3) 1.0875(4) 0.0357(16) Uani 1 1 d . . . H15P H 0.3910 0.9564 1.0706 0.054 Uiso 1 1 calc R . . H15Q H 0.3640 1.0376 1.0792 0.054 Uiso 1 1 calc R . . H15R H 0.4305 1.0006 1.1419 0.054 Uiso 1 1 calc R . . C156 C 0.5792(4) 0.9717(4) 1.0601(4) 0.0398(17) Uani 1 1 d . . . H15S H 0.5952 0.9735 1.1146 0.060 Uiso 1 1 calc R . . H15T H 0.6342 0.9849 1.0307 0.060 Uiso 1 1 calc R . . H15U H 0.5597 0.9239 1.0463 0.060 Uiso 1 1 calc R . . C161 C 0.2412(4) 1.2080(3) 0.5708(4) 0.0406(18) Uani 1 1 d . . . H16D H 0.2660 1.2263 0.5231 0.061 Uiso 1 1 calc R . . H16E H 0.2016 1.2437 0.5943 0.061 Uiso 1 1 calc R . . H16F H 0.2039 1.1657 0.5603 0.061 Uiso 1 1 calc R . . O162 O 0.3736(3) 1.1392(2) 0.5991(2) 0.0294(10) Uani 1 1 d . . . C162 C 0.3219(4) 1.1898(3) 0.6248(4) 0.0274(15) Uani 1 1 d . . . C163 C 0.3355(4) 1.2234(3) 0.6928(4) 0.0327(16) Uani 1 1 d . . . H163 H 0.2876 1.2540 0.7096 0.039 Uiso 1 1 calc R . . O164 O 0.4846(2) 1.17540(19) 0.7252(2) 0.0254(9) Uani 1 1 d . . . C164 C 0.4165(4) 1.2155(3) 0.7400(4) 0.0270(14) Uani 1 1 d . . . C165 C 0.4246(4) 1.2593(3) 0.8113(4) 0.0333(16) Uani 1 1 d . . . H16G H 0.4416 1.2291 0.8546 0.050 Uiso 1 1 calc R . . H16H H 0.3644 1.2823 0.8207 0.050 Uiso 1 1 calc R . . H16I H 0.4732 1.2952 0.8049 0.050 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 0.0263(5) 0.0191(5) 0.0249(6) 0.0029(5) 0.0033(4) 0.0023(4) N1 0.020(2) 0.017(2) 0.025(3) 0.006(2) 0.000(2) -0.0007(19) C2 0.022(3) 0.017(3) 0.032(4) -0.007(3) 0.008(2) 0.000(2) C3 0.026(3) 0.012(3) 0.024(4) 0.005(3) 0.000(2) 0.002(2) O4 0.024(2) 0.022(2) 0.028(3) 0.0024(19) 0.0073(17) -0.0012(16) C4 0.034(3) 0.007(3) 0.024(4) 0.002(3) -0.001(3) 0.004(2) C5 0.025(3) 0.021(3) 0.041(4) 0.006(3) 0.001(3) 0.002(2) C6 0.029(3) 0.024(3) 0.028(4) 0.001(3) -0.009(3) -0.004(3) C7 0.030(3) 0.013(3) 0.028(4) -0.001(3) -0.003(3) 0.001(2) C8 0.027(3) 0.017(3) 0.031(4) 0.000(3) 0.008(3) 0.004(2) C9 0.026(3) 0.029(3) 0.042(4) -0.002(3) 0.001(3) -0.002(3) C10 0.030(3) 0.043(4) 0.043(5) 0.012(4) 0.004(3) 0.003(3) C11 0.032(3) 0.032(4) 0.048(5) 0.010(3) 0.005(3) -0.007(3) C12 0.030(3) 0.056(5) 0.050(5) -0.001(4) 0.005(3) -0.014(3) C13 0.033(3) 0.026(3) 0.029(4) -0.001(3) -0.001(3) 0.003(3) C14 0.039(4) 0.027(3) 0.050(5) -0.011(3) -0.002(3) 0.006(3) C15 0.057(4) 0.049(4) 0.028(4) -0.006(4) 0.006(3) -0.010(3) C16 0.071(5) 0.047(5) 0.032(5) -0.002(4) -0.002(4) 0.018(4) C22 0.028(3) 0.012(3) 0.024(4) 0.008(3) 0.001(2) 0.002(2) C23 0.025(3) 0.020(3) 0.015(3) -0.003(3) -0.005(2) -0.001(2) O24 0.030(2) 0.020(2) 0.030(3) -0.0006(19) -0.0006(18) 0.0043(17) C24 0.029(3) 0.018(3) 0.022(4) 0.005(3) -0.007(3) 0.001(2) C25 0.036(3) 0.019(3) 0.021(4) 0.003(3) -0.006(3) 0.005(3) C26 0.040(4) 0.019(3) 0.030(4) -0.004(3) -0.007(3) -0.002(3) C27 0.040(3) 0.017(3) 0.023(4) 0.007(3) -0.012(3) 0.001(3) C28 0.025(3) 0.029(3) 0.015(3) 0.006(3) -0.004(2) 0.002(2) C29 0.047(4) 0.022(3) 0.034(4) -0.010(3) -0.001(3) 0.004(3) C30 0.048(4) 0.035(4) 0.025(4) -0.007(3) 0.001(3) 0.008(3) C31 0.069(4) 0.023(3) 0.028(4) -0.009(3) -0.001(3) 0.004(3) C32 0.054(4) 0.027(4) 0.041(5) -0.010(3) -0.006(3) 0.017(3) C33 0.034(3) 0.019(3) 0.039(4) 0.004(3) -0.008(3) -0.004(3) C34 0.039(4) 0.031(4) 0.036(4) -0.001(3) -0.009(3) -0.006(3) C35 0.037(4) 0.034(4) 0.051(5) 0.006(4) -0.003(3) -0.005(3) C36 0.050(4) 0.025(4) 0.052(5) 0.006(3) -0.025(3) -0.007(3) C42 0.024(3) 0.016(3) 0.036(4) -0.003(3) 0.002(3) -0.002(2) C43 0.025(3) 0.013(3) 0.032(4) -0.003(3) 0.006(3) 0.000(2) O44 0.028(2) 0.023(2) 0.028(3) 0.0002(19) 0.0059(18) 0.0065(17) C44 0.026(3) 0.019(3) 0.019(4) 0.001(3) 0.000(2) 0.002(2) C45 0.026(3) 0.016(3) 0.032(4) -0.005(3) 0.002(3) -0.006(2) C46 0.031(3) 0.022(3) 0.023(4) 0.003(3) -0.002(3) -0.007(3) C47 0.025(3) 0.013(3) 0.033(4) 0.001(3) -0.002(3) -0.008(2) C48 0.027(3) 0.019(3) 0.028(4) -0.001(3) 0.003(3) -0.003(2) C49 0.030(3) 0.027(3) 0.028(4) 0.006(3) 0.011(3) 0.002(3) C50 0.037(4) 0.038(4) 0.038(5) -0.005(3) 0.012(3) 0.006(3) C51 0.027(3) 0.037(4) 0.041(5) 0.012(3) 0.006(3) -0.003(3) C52 0.035(3) 0.047(4) 0.030(4) 0.005(3) 0.008(3) 0.004(3) C53 0.033(3) 0.020(3) 0.031(4) 0.000(3) -0.001(3) 0.005(2) C54 0.036(3) 0.026(3) 0.033(4) 0.004(3) -0.007(3) 0.003(3) C55 0.035(4) 0.029(4) 0.046(5) 0.007(3) -0.001(3) 0.002(3) C56 0.041(4) 0.017(3) 0.059(5) 0.001(3) -0.008(3) 0.006(3) C61 0.039(4) 0.042(4) 0.068(6) 0.009(4) 0.011(4) 0.008(3) O62 0.031(2) 0.026(2) 0.032(3) 0.003(2) 0.0085(19) 0.0067(18) C62 0.028(3) 0.023(3) 0.035(4) -0.004(3) 0.009(3) 0.007(3) C63 0.027(3) 0.025(3) 0.037(4) 0.001(3) -0.003(3) 0.006(3) O64 0.026(2) 0.022(2) 0.026(3) 0.0028(19) 0.0036(17) -0.0002(17) C64 0.027(3) 0.016(3) 0.021(4) -0.004(3) -0.008(2) 0.003(2) C65 0.033(3) 0.031(4) 0.048(5) 0.007(3) -0.002(3) 0.002(3) V2 0.0247(5) 0.0167(5) 0.0291(7) -0.0022(5) -0.0043(4) 0.0025(4) N101 0.023(2) 0.012(2) 0.021(3) -0.001(2) -0.004(2) 0.0049(19) C102 0.023(3) 0.014(3) 0.023(4) 0.002(3) -0.002(2) 0.005(2) C103 0.023(3) 0.009(3) 0.026(4) -0.002(3) 0.001(2) 0.002(2) O104 0.031(2) 0.016(2) 0.027(3) -0.0079(19) -0.0039(17) 0.0028(17) C104 0.018(3) 0.017(3) 0.031(4) 0.000(3) -0.001(2) -0.003(2) C105 0.022(3) 0.018(3) 0.026(4) -0.007(3) -0.002(2) 0.002(2) C106 0.027(3) 0.024(3) 0.027(4) 0.000(3) -0.002(3) -0.004(2) C107 0.023(3) 0.019(3) 0.026(4) 0.003(3) -0.005(2) 0.004(2) C108 0.025(3) 0.014(3) 0.026(4) 0.006(3) -0.004(2) -0.003(2) C109 0.026(3) 0.030(3) 0.030(4) -0.007(3) -0.007(3) 0.011(3) C110 0.043(4) 0.034(4) 0.041(5) 0.017(3) 0.001(3) 0.014(3) C111 0.033(4) 0.034(4) 0.054(5) -0.002(4) -0.011(3) 0.001(3) C112 0.067(5) 0.055(5) 0.036(5) -0.012(4) -0.024(4) 0.027(4) C113 0.031(3) 0.017(3) 0.021(4) 0.002(3) 0.002(2) 0.003(2) C114 0.037(3) 0.024(3) 0.041(4) 0.001(3) 0.008(3) 0.011(3) C115 0.044(4) 0.023(3) 0.041(5) -0.004(3) 0.001(3) 0.014(3) C116 0.044(4) 0.027(4) 0.040(5) -0.005(3) 0.007(3) 0.007(3) C122 0.028(3) 0.007(3) 0.027(4) -0.002(3) -0.003(2) 0.001(2) C123 0.025(3) 0.021(3) 0.023(4) -0.002(3) -0.001(2) 0.005(2) O124 0.027(2) 0.017(2) 0.027(3) 0.0021(18) -0.0050(17) 0.0009(16) C124 0.029(3) 0.024(3) 0.018(4) 0.000(3) 0.005(2) 0.001(3) C125 0.030(3) 0.021(3) 0.018(4) 0.000(3) 0.006(2) 0.003(2) C126 0.040(3) 0.015(3) 0.019(4) -0.001(3) 0.005(3) 0.001(3) C127 0.036(3) 0.020(3) 0.020(4) -0.005(3) 0.005(3) 0.000(3) C128 0.027(3) 0.020(3) 0.012(3) 0.001(3) -0.001(2) 0.004(2) C129 0.035(3) 0.019(3) 0.037(4) 0.003(3) -0.007(3) 0.003(3) C130 0.041(4) 0.027(4) 0.047(5) 0.014(3) -0.006(3) 0.002(3) C131 0.055(4) 0.029(4) 0.049(5) 0.019(4) -0.019(3) -0.003(3) C132 0.039(4) 0.027(4) 0.061(6) 0.012(4) -0.006(3) 0.005(3) C133 0.021(3) 0.025(3) 0.029(4) 0.002(3) 0.003(2) -0.002(2) C134 0.039(4) 0.030(3) 0.035(4) 0.004(3) -0.005(3) -0.010(3) C135 0.037(3) 0.033(4) 0.031(4) 0.006(3) -0.004(3) -0.010(3) C136 0.031(3) 0.032(4) 0.050(5) 0.004(3) -0.001(3) -0.006(3) C142 0.027(3) 0.021(3) 0.019(4) 0.001(3) -0.008(2) 0.000(2) C143 0.023(3) 0.011(3) 0.032(4) -0.006(3) 0.004(3) 0.005(2) O144 0.024(2) 0.028(2) 0.030(3) -0.001(2) -0.0045(18) 0.0005(17) C144 0.029(3) 0.006(3) 0.026(4) -0.009(3) 0.002(3) 0.003(2) C145 0.028(3) 0.019(3) 0.036(4) -0.004(3) 0.002(3) 0.004(2) C146 0.022(3) 0.024(3) 0.040(5) 0.002(3) 0.012(3) 0.004(2) C147 0.026(3) 0.008(3) 0.041(4) -0.001(3) 0.008(3) 0.001(2) C148 0.019(3) 0.016(3) 0.038(4) -0.012(3) -0.001(3) 0.002(2) C149 0.026(3) 0.033(4) 0.039(4) 0.001(3) 0.004(3) -0.003(3) C150 0.031(3) 0.040(4) 0.050(5) -0.005(4) -0.011(3) -0.004(3) C151 0.023(3) 0.048(4) 0.069(6) -0.009(4) -0.004(3) 0.006(3) C152 0.035(4) 0.071(5) 0.066(6) 0.002(5) -0.002(4) -0.015(4) C153 0.029(3) 0.019(3) 0.032(4) -0.001(3) 0.008(3) -0.007(2) C154 0.043(4) 0.028(4) 0.036(4) -0.003(3) 0.006(3) -0.001(3) C155 0.042(4) 0.026(3) 0.039(5) 0.002(3) 0.003(3) -0.003(3) C156 0.045(4) 0.046(4) 0.028(4) 0.007(3) -0.001(3) 0.003(3) C161 0.030(3) 0.028(4) 0.063(5) -0.002(4) -0.007(3) 0.004(3) O162 0.025(2) 0.024(2) 0.039(3) -0.006(2) -0.0084(18) 0.0048(18) C162 0.018(3) 0.021(3) 0.043(5) 0.007(3) 0.000(3) 0.005(2) C163 0.028(3) 0.023(3) 0.046(5) -0.006(3) 0.001(3) 0.001(3) O164 0.030(2) 0.020(2) 0.026(3) -0.0059(19) -0.0040(18) 0.0032(18) C164 0.028(3) 0.021(3) 0.032(4) 0.009(3) 0.004(3) 0.003(3) C165 0.040(4) 0.030(4) 0.031(4) -0.005(3) 0.004(3) 0.003(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 O24 1.832(4) . ? V1 O4 1.832(4) . ? V1 O44 1.861(4) . ? V1 O62 1.967(4) . ? V1 O64 2.059(4) . ? V1 N1 2.178(4) . ? N1 C22 1.490(7) . ? N1 C2 1.497(7) . ? N1 C42 1.520(7) . ? C2 C3 1.503(8) . ? C3 C4 1.387(7) . ? C3 C8 1.398(8) . ? O4 C4 1.345(7) . ? C4 C5 1.396(8) . ? C5 C6 1.393(8) . ? C5 C9 1.550(8) . ? C6 C7 1.388(8) . ? C7 C8 1.386(8) . ? C7 C13 1.535(8) . ? C9 C10 1.524(8) . ? C9 C12 1.538(9) . ? C9 C11 1.557(8) . ? C13 C15 1.500(8) . ? C13 C16 1.519(9) . ? C13 C14 1.557(8) . ? C22 C23 1.503(7) . ? C23 C28 1.379(7) . ? C23 C24 1.388(8) . ? O24 C24 1.347(6) . ? C24 C25 1.422(8) . ? C25 C26 1.371(8) . ? C25 C29 1.554(8) . ? C26 C27 1.400(8) . ? C27 C28 1.403(8) . ? C27 C33 1.510(8) . ? C29 C32 1.524(8) . ? C29 C30 1.537(9) . ? C29 C31 1.537(8) . ? C33 C35 1.518(9) . ? C33 C34 1.555(8) . ? C33 C36 1.560(9) . ? C42 C43 1.514(8) . ? C43 C48 1.392(7) . ? C43 C44 1.411(7) . ? O44 C44 1.342(6) . ? C44 C45 1.417(8) . ? C45 C46 1.402(8) . ? C45 C49 1.538(7) . ? C46 C47 1.387(8) . ? C47 C48 1.398(8) . ? C47 C53 1.541(8) . ? C49 C51 1.525(8) . ? C49 C52 1.533(8) . ? C49 C50 1.550(8) . ? C53 C54 1.528(8) . ? C53 C55 1.532(8) . ? C53 C56 1.557(8) . ? C61 C62 1.498(8) . ? O62 C62 1.283(7) . ? C62 C63 1.392(8) . ? C63 C64 1.395(8) . ? O64 C64 1.271(6) . ? C64 C65 1.494(8) . ? V2 O144 1.836(4) . ? V2 O124 1.843(4) . ? V2 O104 1.854(4) . ? V2 O162 1.960(4) . ? V2 O164 2.056(4) . ? V2 N101 2.185(4) . ? N101 C122 1.484(7) . ? N101 C142 1.486(7) . ? N101 C102 1.517(6) . ? C102 C103 1.519(8) . ? C103 C104 1.390(7) . ? C103 C108 1.392(7) . ? O104 C104 1.342(6) . ? C104 C105 1.417(8) . ? C105 C106 1.392(7) . ? C105 C109 1.528(8) . ? C106 C107 1.385(8) . ? C107 C108 1.408(8) . ? C107 C113 1.544(7) . ? C109 C112 1.517(9) . ? C109 C111 1.533(8) . ? C109 C110 1.550(8) . ? C113 C115 1.523(8) . ? C113 C114 1.525(8) . ? C113 C116 1.538(8) . ? C122 C123 1.513(7) . ? C123 C128 1.374(7) . ? C123 C124 1.396(8) . ? O124 C124 1.349(6) . ? C124 C125 1.438(8) . ? C125 C126 1.380(8) . ? C125 C129 1.514(8) . ? C126 C127 1.387(8) . ? C127 C128 1.396(7) . ? C127 C133 1.540(8) . ? C129 C132 1.530(8) . ? C129 C131 1.533(9) . ? C129 C130 1.539(8) . ? C133 C136 1.527(8) . ? C133 C135 1.528(8) . ? C133 C134 1.536(9) . ? C142 C143 1.515(7) . ? C143 C148 1.387(8) . ? C143 C144 1.398(7) . ? O144 C144 1.346(7) . ? C144 C145 1.403(8) . ? C145 C146 1.394(9) . ? C145 C149 1.533(8) . ? C146 C147 1.390(8) . ? C147 C148 1.387(8) . ? C147 C153 1.540(9) . ? C149 C151 1.523(9) . ? C149 C152 1.530(9) . ? C149 C150 1.578(9) . ? C153 C155 1.516(8) . ? C153 C156 1.530(8) . ? C153 C154 1.551(8) . ? C161 C162 1.515(8) . ? O162 C162 1.299(7) . ? C162 C163 1.364(9) . ? C163 C164 1.415(8) . ? O164 C164 1.266(6) . ? C164 C165 1.506(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 O24 V1 O4 163.64(17) . . ? O24 V1 O44 95.19(18) . . ? O4 V1 O44 95.61(18) . . ? O24 V1 O62 98.69(17) . . ? O4 V1 O62 93.72(17) . . ? O44 V1 O62 89.15(16) . . ? O24 V1 O64 84.19(17) . . ? O4 V1 O64 85.69(17) . . ? O44 V1 O64 176.78(16) . . ? O62 V1 O64 87.82(16) . . ? O24 V1 N1 85.64(17) . . ? O4 V1 N1 81.83(17) . . ? O44 V1 N1 91.47(16) . . ? O62 V1 N1 175.55(19) . . ? O64 V1 N1 91.64(16) . . ? C22 N1 C2 107.4(4) . . ? C22 N1 C42 106.8(4) . . ? C2 N1 C42 109.5(4) . . ? C22 N1 V1 115.1(3) . . ? C2 N1 V1 109.5(3) . . ? C42 N1 V1 108.5(3) . . ? N1 C2 C3 116.2(4) . . ? C4 C3 C8 118.4(5) . . ? C4 C3 C2 123.6(5) . . ? C8 C3 C2 118.0(5) . . ? C4 O4 V1 137.2(3) . . ? O4 C4 C3 118.7(5) . . ? O4 C4 C5 119.5(5) . . ? C3 C4 C5 121.7(6) . . ? C6 C5 C4 116.5(5) . . ? C6 C5 C9 121.7(5) . . ? C4 C5 C9 121.8(6) . . ? C7 C6 C5 124.1(5) . . ? C8 C7 C6 116.5(6) . . ? C8 C7 C13 123.3(5) . . ? C6 C7 C13 120.2(5) . . ? C7 C8 C3 122.3(5) . . ? C10 C9 C12 108.2(5) . . ? C10 C9 C5 110.9(5) . . ? C12 C9 C5 111.8(5) . . ? C10 C9 C11 110.3(5) . . ? C12 C9 C11 106.9(5) . . ? C5 C9 C11 108.7(5) . . ? C15 C13 C16 109.4(6) . . ? C15 C13 C7 114.3(5) . . ? C16 C13 C7 109.5(5) . . ? C15 C13 C14 107.9(5) . . ? C16 C13 C14 106.5(5) . . ? C7 C13 C14 109.0(5) . . ? N1 C22 C23 114.9(4) . . ? C28 C23 C24 120.4(5) . . ? C28 C23 C22 121.7(5) . . ? C24 C23 C22 117.3(5) . . ? C24 O24 V1 131.3(4) . . ? O24 C24 C23 118.0(5) . . ? O24 C24 C25 122.2(5) . . ? C23 C24 C25 119.8(5) . . ? C26 C25 C24 116.6(5) . . ? C26 C25 C29 122.1(5) . . ? C24 C25 C29 121.0(5) . . ? C25 C26 C27 126.0(5) . . ? C26 C27 C28 114.6(5) . . ? C26 C27 C33 122.4(5) . . ? C28 C27 C33 122.7(5) . . ? C23 C28 C27 122.5(5) . . ? C32 C29 C30 108.8(5) . . ? C32 C29 C31 108.5(5) . . ? C30 C29 C31 107.6(5) . . ? C32 C29 C25 109.9(5) . . ? C30 C29 C25 110.1(5) . . ? C31 C29 C25 111.9(5) . . ? C27 C33 C35 113.6(5) . . ? C27 C33 C34 111.6(5) . . ? C35 C33 C34 107.5(5) . . ? C27 C33 C36 107.5(5) . . ? C35 C33 C36 108.7(5) . . ? C34 C33 C36 107.7(5) . . ? C43 C42 N1 113.3(5) . . ? C48 C43 C44 119.7(6) . . ? C48 C43 C42 119.5(5) . . ? C44 C43 C42 120.7(5) . . ? C44 O44 V1 132.6(3) . . ? O44 C44 C43 120.9(5) . . ? O44 C44 C45 118.9(5) . . ? C43 C44 C45 120.1(5) . . ? C46 C45 C44 117.2(5) . . ? C46 C45 C49 121.8(5) . . ? C44 C45 C49 121.0(5) . . ? C47 C46 C45 124.0(6) . . ? C46 C47 C48 117.3(5) . . ? C46 C47 C53 122.6(5) . . ? C48 C47 C53 120.1(5) . . ? C43 C48 C47 121.7(5) . . ? C51 C49 C52 107.3(5) . . ? C51 C49 C45 109.9(5) . . ? C52 C49 C45 111.8(5) . . ? C51 C49 C50 109.9(5) . . ? C52 C49 C50 108.1(5) . . ? C45 C49 C50 109.9(4) . . ? C54 C53 C55 109.0(5) . . ? C54 C53 C47 109.8(5) . . ? C55 C53 C47 111.9(5) . . ? C54 C53 C56 108.4(5) . . ? C55 C53 C56 108.0(5) . . ? C47 C53 C56 109.7(5) . . ? C62 O62 V1 127.8(4) . . ? O62 C62 C63 125.8(5) . . ? O62 C62 C61 114.6(6) . . ? C63 C62 C61 119.5(5) . . ? C62 C63 C64 124.2(5) . . ? C64 O64 V1 127.1(3) . . ? O64 C64 C63 124.7(5) . . ? O64 C64 C65 115.4(5) . . ? C63 C64 C65 119.9(5) . . ? O144 V2 O124 161.56(17) . . ? O144 V2 O104 93.95(18) . . ? O124 V2 O104 98.46(17) . . ? O144 V2 O162 98.47(17) . . ? O124 V2 O162 95.90(17) . . ? O104 V2 O162 86.30(17) . . ? O144 V2 O164 82.78(17) . . ? O124 V2 O164 86.33(16) . . ? O104 V2 O164 172.66(15) . . ? O162 V2 O164 87.68(16) . . ? O144 V2 N101 81.81(16) . . ? O124 V2 N101 84.63(16) . . ? O104 V2 N101 89.89(16) . . ? O162 V2 N101 176.19(17) . . ? O164 V2 N101 96.12(16) . . ? C122 N101 C142 108.0(4) . . ? C122 N101 C102 106.4(4) . . ? C142 N101 C102 109.7(4) . . ? C122 N101 V2 115.6(3) . . ? C142 N101 V2 107.6(3) . . ? C102 N101 V2 109.5(3) . . ? N101 C102 C103 112.7(4) . . ? C104 C103 C108 119.0(5) . . ? C104 C103 C102 121.6(5) . . ? C108 C103 C102 119.3(5) . . ? C104 O104 V2 134.9(4) . . ? O104 C104 C103 120.7(5) . . ? O104 C104 C105 118.1(5) . . ? C103 C104 C105 121.2(5) . . ? C106 C105 C104 116.9(5) . . ? C106 C105 C109 123.1(5) . . ? C104 C105 C109 120.0(5) . . ? C107 C106 C105 124.3(6) . . ? C106 C107 C108 116.5(5) . . ? C106 C107 C113 123.6(5) . . ? C108 C107 C113 119.9(5) . . ? C103 C108 C107 122.1(5) . . ? C112 C109 C105 112.0(5) . . ? C112 C109 C111 108.1(5) . . ? C105 C109 C111 110.1(5) . . ? C112 C109 C110 106.5(6) . . ? C105 C109 C110 111.2(5) . . ? C111 C109 C110 108.8(5) . . ? C115 C113 C114 108.8(5) . . ? C115 C113 C116 108.1(5) . . ? C114 C113 C116 109.2(5) . . ? C115 C113 C107 112.0(5) . . ? C114 C113 C107 109.1(4) . . ? C116 C113 C107 109.6(5) . . ? N101 C122 C123 114.3(4) . . ? C128 C123 C124 120.4(5) . . ? C128 C123 C122 121.7(5) . . ? C124 C123 C122 117.3(5) . . ? C124 O124 V2 134.7(4) . . ? O124 C124 C123 117.2(5) . . ? O124 C124 C125 122.5(5) . . ? C123 C124 C125 120.3(5) . . ? C126 C125 C124 115.4(5) . . ? C126 C125 C129 124.1(5) . . ? C124 C125 C129 120.3(5) . . ? C125 C126 C127 125.8(5) . . ? C126 C127 C128 116.5(5) . . ? C126 C127 C133 122.9(5) . . ? C128 C127 C133 120.6(5) . . ? C123 C128 C127 121.5(5) . . ? C125 C129 C132 110.8(5) . . ? C125 C129 C131 109.3(5) . . ? C132 C129 C131 110.1(5) . . ? C125 C129 C130 111.3(5) . . ? C132 C129 C130 108.0(5) . . ? C131 C129 C130 107.3(5) . . ? C136 C133 C135 108.9(5) . . ? C136 C133 C134 108.6(5) . . ? C135 C133 C134 107.4(5) . . ? C136 C133 C127 111.1(5) . . ? C135 C133 C127 112.6(5) . . ? C134 C133 C127 108.1(4) . . ? N101 C142 C143 116.6(4) . . ? C148 C143 C144 118.5(5) . . ? C148 C143 C142 118.4(5) . . ? C144 C143 C142 123.1(5) . . ? C144 O144 V2 134.9(3) . . ? O144 C144 C143 118.8(5) . . ? O144 C144 C145 120.3(5) . . ? C143 C144 C145 120.7(6) . . ? C146 C145 C144 117.1(5) . . ? C146 C145 C149 121.4(5) . . ? C144 C145 C149 121.5(6) . . ? C147 C146 C145 123.9(5) . . ? C148 C147 C146 116.3(6) . . ? C148 C147 C153 120.4(5) . . ? C146 C147 C153 123.3(5) . . ? C147 C148 C143 122.9(5) . . ? C151 C149 C152 108.8(5) . . ? C151 C149 C145 110.7(5) . . ? C152 C149 C145 112.6(6) . . ? C151 C149 C150 108.7(6) . . ? C152 C149 C150 105.9(5) . . ? C145 C149 C150 109.9(5) . . ? C155 C153 C156 109.7(5) . . ? C155 C153 C147 112.1(5) . . ? C156 C153 C147 110.0(5) . . ? C155 C153 C154 108.6(5) . . ? C156 C153 C154 107.7(5) . . ? C147 C153 C154 108.6(5) . . ? C162 O162 V2 128.7(4) . . ? O162 C162 C163 125.4(5) . . ? O162 C162 C161 112.4(6) . . ? C163 C162 C161 122.2(5) . . ? C162 C163 C164 124.3(5) . . ? C164 O164 V2 126.2(4) . . ? O164 C164 C163 124.3(6) . . ? O164 C164 C165 117.2(5) . . ? C163 C164 C165 118.4(5) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.852 _refine_diff_density_min -0.418 _refine_diff_density_rms 0.065 #===END