# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2011 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Prof. Zi, Guofu' _publ_contact_author_email ziguofu@hotmail.com _publ_section_title ; Synthesis and catalytic activity of group 5 metal amides with chiral biaryldiamine-based ligands ; loop_ _publ_author_name 'Furen Zhang' 'Haibin Song' 'Guofu Zi' # Attachment '- compound 3.cif' data_compound3 _database_code_depnum_ccdc_archive 'CCDC 739122' #TrackingRef '- compound 3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H36 N2 O2' _chemical_formula_sum 'C34 H36 N2 O2' _chemical_formula_weight 504.65 _chemical_absolute_configuration rm 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 0.0000 '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 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 8.6919(10) _cell_length_b 17.638(2) _cell_length_c 18.832(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2886.9(6) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 9616 _cell_measurement_theta_min 2.5 _cell_measurement_theta_max 27.8 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.161 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 0.072 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9830 _exptl_absorpt_correction_T_max 0.9872 _exptl_absorpt_process_details crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 30162 _diffrn_reflns_av_R_equivalents 0.0440 _diffrn_reflns_av_sigmaI/netI 0.0484 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.31 _diffrn_reflns_theta_max 27.85 _reflns_number_total 3858 _reflns_number_gt 3661 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear(Rigaku/MSC Inc., 2005)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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. The absolute structure was assigned refering starting material, no Flack parameter provided. ; _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^)+(0.0581P)^2^+0.3620P] 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 SHELXL _refine_ls_extinction_coef 0.020(2) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'None, Fiedel Pairs merged' _refine_ls_abs_structure_Flack ? _refine_ls_number_reflns 3858 _refine_ls_number_parameters 360 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0409 _refine_ls_R_factor_gt 0.0383 _refine_ls_wR_factor_ref 0.0971 _refine_ls_wR_factor_gt 0.0953 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _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 O1 O 0.43225(15) 0.45000(6) 0.79458(7) 0.0315(3) Uani 1 1 d . . . O2 O 0.55808(17) 0.67694(7) 0.65537(7) 0.0334(3) Uani 1 1 d . . . N1 N 0.46142(17) 0.57156(7) 0.75679(7) 0.0248(3) Uani 1 1 d . . . N2 N 0.56310(18) 0.78850(8) 0.71598(8) 0.0266(3) Uani 1 1 d . . . C1 C 0.5529(2) 0.67491(9) 0.82976(8) 0.0241(3) Uani 1 1 d . . . C2 C 0.5674(2) 0.59867(9) 0.80825(8) 0.0233(3) Uani 1 1 d . . . C3 C 0.6845(2) 0.55326(9) 0.83535(9) 0.0266(3) Uani 1 1 d . . . H3 H 0.6933 0.5018 0.8209 0.032 Uiso 1 1 calc R . . C4 C 0.7882(2) 0.58347(10) 0.88364(9) 0.0297(4) Uani 1 1 d . . . H4 H 0.8674 0.5525 0.9028 0.036 Uiso 1 1 calc R . . C5 C 0.7767(2) 0.65883(11) 0.90411(9) 0.0304(4) Uani 1 1 d . . . H5 H 0.8491 0.6791 0.9368 0.036 Uiso 1 1 calc R . . C6 C 0.6610(2) 0.70516(10) 0.87752(9) 0.0289(4) Uani 1 1 d . . . C7 C 0.6507(3) 0.78736(11) 0.90008(11) 0.0417(5) Uani 1 1 d . . . H7A H 0.7314 0.7982 0.9349 0.063 Uiso 1 1 calc R . . H7B H 0.5497 0.7969 0.9214 0.063 Uiso 1 1 calc R . . H7C H 0.6643 0.8201 0.8585 0.063 Uiso 1 1 calc R . . C8 C 0.4160(2) 0.72080(9) 0.80771(8) 0.0249(3) Uani 1 1 d . . . C9 C 0.4228(2) 0.77584(9) 0.75424(9) 0.0262(3) Uani 1 1 d . . . C10 C 0.2960(2) 0.82094(10) 0.73835(10) 0.0323(4) Uani 1 1 d . . . H10 H 0.3026 0.8580 0.7019 0.039 Uiso 1 1 calc R . . C11 C 0.1602(3) 0.81172(11) 0.77572(11) 0.0369(4) Uani 1 1 d . . . H11 H 0.0736 0.8425 0.7652 0.044 Uiso 1 1 calc R . . C12 C 0.1514(2) 0.75706(11) 0.82890(10) 0.0358(4) Uani 1 1 d . . . H12 H 0.0581 0.7510 0.8545 0.043 Uiso 1 1 calc R . . C13 C 0.2766(2) 0.71113(10) 0.84520(9) 0.0297(4) Uani 1 1 d . . . C14 C 0.2639(2) 0.65309(11) 0.90375(10) 0.0365(4) Uani 1 1 d . . . H14A H 0.1585 0.6527 0.9222 0.055 Uiso 1 1 calc R . . H14B H 0.3354 0.6661 0.9421 0.055 Uiso 1 1 calc R . . H14C H 0.2895 0.6028 0.8850 0.055 Uiso 1 1 calc R . . C15 C 0.4039(2) 0.50073(8) 0.75149(8) 0.0231(3) Uani 1 1 d . . . C16 C 0.2948(2) 0.48936(9) 0.69074(9) 0.0243(3) Uani 1 1 d . . . C17 C 0.1373(2) 0.48202(9) 0.70649(9) 0.0283(4) Uani 1 1 d . . . C18 C 0.0346(2) 0.47299(10) 0.65061(10) 0.0317(4) Uani 1 1 d . . . H18 H -0.0721 0.4687 0.6609 0.038 Uiso 1 1 calc R . . C19 C 0.0824(2) 0.47001(10) 0.58000(10) 0.0318(4) Uani 1 1 d . . . C20 C 0.2397(2) 0.47579(9) 0.56605(9) 0.0308(4) Uani 1 1 d . . . H20 H 0.2743 0.4731 0.5183 0.037 Uiso 1 1 calc R . . C21 C 0.3478(2) 0.48543(9) 0.62036(9) 0.0276(4) Uani 1 1 d . . . C22 C 0.0797(2) 0.48530(13) 0.78215(10) 0.0396(5) Uani 1 1 d . . . H22A H -0.0328 0.4818 0.7824 0.059 Uiso 1 1 calc R . . H22B H 0.1114 0.5333 0.8039 0.059 Uiso 1 1 calc R . . H22C H 0.1232 0.4430 0.8092 0.059 Uiso 1 1 calc R . . C23 C -0.0344(3) 0.46015(13) 0.52130(11) 0.0455(5) Uani 1 1 d . . . H23A H -0.0775 0.4089 0.5234 0.068 Uiso 1 1 calc R . . H23B H 0.0157 0.4678 0.4752 0.068 Uiso 1 1 calc R . . H23C H -0.1171 0.4974 0.5272 0.068 Uiso 1 1 calc R . . C24 C 0.5177(2) 0.48878(11) 0.60359(10) 0.0341(4) Uani 1 1 d . . . H24A H 0.5559 0.5403 0.6119 0.051 Uiso 1 1 calc R . . H24B H 0.5342 0.4750 0.5538 0.051 Uiso 1 1 calc R . . H24C H 0.5733 0.4532 0.6343 0.051 Uiso 1 1 calc R . . C25 C 0.6177(2) 0.73909(9) 0.66641(9) 0.0267(4) Uani 1 1 d . . . C26 C 0.7590(2) 0.76583(9) 0.62830(9) 0.0262(4) Uani 1 1 d . . . C27 C 0.9011(2) 0.73179(10) 0.64459(9) 0.0309(4) Uani 1 1 d . . . C28 C 1.0325(2) 0.75798(11) 0.61041(9) 0.0325(4) Uani 1 1 d . . . H28 H 1.1290 0.7355 0.6214 0.039 Uiso 1 1 calc R . . C29 C 1.0267(2) 0.81665(11) 0.56014(9) 0.0316(4) Uani 1 1 d . . . C30 C 0.8833(2) 0.84647(10) 0.54268(9) 0.0303(4) Uani 1 1 d . . . H30 H 0.8770 0.8844 0.5070 0.036 Uiso 1 1 calc R . . C31 C 0.7487(2) 0.82238(9) 0.57597(9) 0.0277(4) Uani 1 1 d . . . C32 C 0.9113(3) 0.66795(11) 0.69793(11) 0.0407(5) Uani 1 1 d . . . H32A H 1.0196 0.6561 0.7072 0.061 Uiso 1 1 calc R . . H32B H 0.8595 0.6230 0.6789 0.061 Uiso 1 1 calc R . . H32C H 0.8614 0.6834 0.7423 0.061 Uiso 1 1 calc R . . C33 C 1.1720(3) 0.84589(13) 0.52615(11) 0.0405(5) Uani 1 1 d . . . H33A H 1.2516 0.8066 0.5281 0.061 Uiso 1 1 calc R . . H33B H 1.2076 0.8910 0.5518 0.061 Uiso 1 1 calc R . . H33C H 1.1514 0.8592 0.4765 0.061 Uiso 1 1 calc R . . C34 C 0.5946(2) 0.85439(11) 0.55393(10) 0.0343(4) Uani 1 1 d . . . H34A H 0.6030 0.8766 0.5064 0.051 Uiso 1 1 calc R . . H34B H 0.5630 0.8936 0.5878 0.051 Uiso 1 1 calc R . . H34C H 0.5178 0.8137 0.5534 0.051 Uiso 1 1 calc R . . H2 H 0.595(3) 0.8392(12) 0.7107(12) 0.036(6) Uiso 1 1 d . . . H1 H 0.434(3) 0.6058(14) 0.7211(13) 0.048(7) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0389(7) 0.0193(5) 0.0364(6) 0.0058(5) -0.0070(6) -0.0028(5) O2 0.0482(8) 0.0204(5) 0.0317(6) -0.0022(5) 0.0070(6) -0.0068(5) N1 0.0303(7) 0.0182(6) 0.0259(6) 0.0009(5) -0.0027(6) -0.0015(6) N2 0.0355(8) 0.0172(6) 0.0271(6) -0.0001(5) 0.0021(6) -0.0015(6) C1 0.0277(9) 0.0216(7) 0.0230(7) 0.0003(6) 0.0022(7) -0.0018(7) C2 0.0271(8) 0.0203(7) 0.0225(7) 0.0015(6) 0.0010(7) -0.0032(6) C3 0.0284(9) 0.0230(7) 0.0284(7) 0.0013(6) 0.0024(7) -0.0004(7) C4 0.0265(9) 0.0344(9) 0.0283(8) 0.0050(7) -0.0012(7) 0.0000(7) C5 0.0297(9) 0.0372(9) 0.0244(8) -0.0008(7) -0.0015(7) -0.0077(8) C6 0.0352(10) 0.0267(8) 0.0247(7) -0.0025(7) 0.0018(7) -0.0055(7) C7 0.0565(13) 0.0311(9) 0.0375(9) -0.0098(8) -0.0074(10) -0.0053(9) C8 0.0301(9) 0.0203(7) 0.0243(7) -0.0050(6) 0.0003(7) -0.0005(7) C9 0.0344(9) 0.0185(7) 0.0257(7) -0.0033(6) 0.0009(7) -0.0002(7) C10 0.0394(10) 0.0239(7) 0.0336(8) 0.0000(7) -0.0010(8) 0.0039(7) C11 0.0376(11) 0.0306(9) 0.0423(10) -0.0018(8) 0.0010(9) 0.0091(8) C12 0.0335(10) 0.0358(9) 0.0382(9) -0.0041(8) 0.0055(8) 0.0037(8) C13 0.0338(10) 0.0276(8) 0.0276(8) -0.0032(7) 0.0026(7) -0.0012(7) C14 0.0369(10) 0.0394(10) 0.0332(9) 0.0031(8) 0.0072(8) -0.0006(8) C15 0.0252(8) 0.0176(7) 0.0264(7) -0.0010(6) 0.0016(7) 0.0015(6) C16 0.0300(9) 0.0150(6) 0.0278(7) -0.0006(6) -0.0016(7) 0.0003(6) C17 0.0295(9) 0.0216(7) 0.0336(8) -0.0035(7) 0.0013(7) -0.0006(7) C18 0.0294(9) 0.0246(8) 0.0412(9) -0.0037(7) -0.0043(8) 0.0007(7) C19 0.0373(10) 0.0218(8) 0.0362(9) -0.0008(7) -0.0109(8) -0.0012(7) C20 0.0423(10) 0.0236(7) 0.0266(8) -0.0004(7) -0.0024(8) -0.0010(8) C21 0.0351(9) 0.0190(7) 0.0287(8) -0.0002(6) -0.0003(7) 0.0003(7) C22 0.0332(10) 0.0486(11) 0.0368(9) -0.0078(9) 0.0051(9) -0.0029(9) C23 0.0474(12) 0.0454(11) 0.0438(10) -0.0011(9) -0.0167(10) -0.0016(10) C24 0.0347(10) 0.0365(10) 0.0312(8) -0.0037(8) 0.0053(8) -0.0034(8) C25 0.0372(10) 0.0187(7) 0.0240(7) 0.0025(6) 0.0006(7) 0.0003(7) C26 0.0342(9) 0.0191(7) 0.0252(7) -0.0019(6) 0.0009(7) -0.0012(7) C27 0.0410(10) 0.0252(8) 0.0264(8) -0.0010(7) -0.0015(8) 0.0026(8) C28 0.0332(9) 0.0350(9) 0.0294(8) -0.0032(7) -0.0014(8) 0.0043(8) C29 0.0347(10) 0.0328(9) 0.0272(8) -0.0038(7) 0.0015(8) -0.0031(8) C30 0.0368(10) 0.0270(8) 0.0271(8) 0.0024(7) 0.0006(7) -0.0031(8) C31 0.0344(9) 0.0220(7) 0.0266(7) -0.0003(6) -0.0010(7) -0.0028(7) C32 0.0496(12) 0.0316(9) 0.0409(10) 0.0085(8) -0.0004(10) 0.0070(9) C33 0.0349(11) 0.0494(11) 0.0372(10) -0.0009(9) 0.0039(9) -0.0036(10) C34 0.0367(10) 0.0343(9) 0.0319(9) 0.0073(7) -0.0014(8) 0.0022(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C15 1.2327(19) . ? O2 C25 1.230(2) . ? N1 C15 1.349(2) . ? N1 C2 1.420(2) . ? N1 H1 0.93(2) . ? N2 C25 1.362(2) . ? N2 C9 1.434(2) . ? N2 H2 0.94(2) . ? C1 C6 1.406(2) . ? C1 C2 1.410(2) . ? C1 C8 1.498(2) . ? C2 C3 1.392(2) . ? C3 C4 1.387(2) . ? C3 H3 0.9500 . ? C4 C5 1.388(3) . ? C4 H4 0.9500 . ? C5 C6 1.389(3) . ? C5 H5 0.9500 . ? C6 C7 1.513(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.400(2) . ? C8 C13 1.412(3) . ? C9 C10 1.392(3) . ? C10 C11 1.383(3) . ? C10 H10 0.9500 . ? C11 C12 1.392(3) . ? C11 H11 0.9500 . ? C12 C13 1.391(3) . ? C12 H12 0.9500 . ? C13 C14 1.509(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.500(2) . ? C16 C21 1.405(2) . ? C16 C17 1.406(3) . ? C17 C18 1.389(3) . ? C17 C22 1.511(3) . ? C18 C19 1.394(3) . ? C18 H18 0.9500 . ? C19 C20 1.395(3) . ? C19 C23 1.511(3) . ? C20 C21 1.399(3) . ? C20 H20 0.9500 . ? C21 C24 1.511(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.499(3) . ? C26 C31 1.405(2) . ? C26 C27 1.407(3) . ? C27 C28 1.390(3) . ? C27 C32 1.511(2) . ? C28 C29 1.403(3) . ? C28 H28 0.9500 . ? C29 C30 1.392(3) . ? C29 C33 1.507(3) . ? C30 C31 1.393(3) . ? C30 H30 0.9500 . ? C31 C34 1.512(3) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C15 N1 C2 127.05(14) . . ? C15 N1 H1 116.9(15) . . ? C2 N1 H1 115.9(15) . . ? C25 N2 C9 122.75(15) . . ? C25 N2 H2 115.7(14) . . ? C9 N2 H2 116.7(14) . . ? C6 C1 C2 119.05(16) . . ? C6 C1 C8 120.22(14) . . ? C2 C1 C8 120.47(15) . . ? C3 C2 C1 120.61(15) . . ? C3 C2 N1 122.06(14) . . ? C1 C2 N1 117.31(15) . . ? C4 C3 C2 119.64(15) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 120.22(17) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C6 121.03(17) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C1 119.42(15) . . ? C5 C6 C7 120.35(17) . . ? C1 C6 C7 120.23(17) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C13 118.66(16) . . ? C9 C8 C1 122.71(16) . . ? C13 C8 C1 118.53(14) . . ? C10 C9 C8 121.15(17) . . ? C10 C9 N2 118.47(15) . . ? C8 C9 N2 120.36(15) . . ? C11 C10 C9 119.94(17) . . ? C11 C10 H10 120.0 . . ? C9 C10 H10 120.0 . . ? C10 C11 C12 119.63(18) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C13 C12 C11 121.25(18) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C12 C13 C8 119.37(16) . . ? C12 C13 C14 119.93(17) . . ? C8 C13 C14 120.68(17) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O1 C15 N1 123.32(15) . . ? O1 C15 C16 122.11(14) . . ? N1 C15 C16 114.49(14) . . ? C21 C16 C17 120.91(16) . . ? C21 C16 C15 121.24(16) . . ? C17 C16 C15 117.84(15) . . ? C18 C17 C16 118.46(17) . . ? C18 C17 C22 120.36(17) . . ? C16 C17 C22 121.18(16) . . ? C17 C18 C19 122.33(19) . . ? C17 C18 H18 118.8 . . ? C19 C18 H18 118.8 . . ? C18 C19 C20 117.97(17) . . ? C18 C19 C23 120.10(19) . . ? C20 C19 C23 121.93(19) . . ? C19 C20 C21 121.96(17) . . ? C19 C20 H20 119.0 . . ? C21 C20 H20 119.0 . . ? C20 C21 C16 118.35(17) . . ? C20 C21 C24 120.57(16) . . ? C16 C21 C24 121.05(16) . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O2 C25 N2 122.61(17) . . ? O2 C25 C26 123.00(15) . . ? N2 C25 C26 114.36(15) . . ? C31 C26 C27 120.79(17) . . ? C31 C26 C25 120.45(16) . . ? C27 C26 C25 118.73(14) . . ? C28 C27 C26 118.58(15) . . ? C28 C27 C32 120.47(18) . . ? C26 C27 C32 120.95(17) . . ? C27 C28 C29 121.86(18) . . ? C27 C28 H28 119.1 . . ? C29 C28 H28 119.1 . . ? C30 C29 C28 118.04(17) . . ? C30 C29 C33 121.38(17) . . ? C28 C29 C33 120.58(18) . . ? C29 C30 C31 122.01(16) . . ? C29 C30 H30 119.0 . . ? C31 C30 H30 119.0 . . ? C30 C31 C26 118.58(17) . . ? C30 C31 C34 120.44(15) . . ? C26 C31 C34 120.94(16) . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C33 H33A 109.5 . . ? C29 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C29 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 1.8(2) . . . . ? C8 C1 C2 C3 -172.33(15) . . . . ? C6 C1 C2 N1 -176.36(15) . . . . ? C8 C1 C2 N1 9.5(2) . . . . ? C15 N1 C2 C3 34.9(3) . . . . ? C15 N1 C2 C1 -146.97(17) . . . . ? C1 C2 C3 C4 -0.4(2) . . . . ? N1 C2 C3 C4 177.70(15) . . . . ? C2 C3 C4 C5 -0.9(3) . . . . ? C3 C4 C5 C6 0.7(3) . . . . ? C4 C5 C6 C1 0.8(3) . . . . ? C4 C5 C6 C7 -179.65(18) . . . . ? C2 C1 C6 C5 -2.0(2) . . . . ? C8 C1 C6 C5 172.17(15) . . . . ? C2 C1 C6 C7 178.44(16) . . . . ? C8 C1 C6 C7 -7.4(3) . . . . ? C6 C1 C8 C9 81.8(2) . . . . ? C2 C1 C8 C9 -104.12(19) . . . . ? C6 C1 C8 C13 -94.47(19) . . . . ? C2 C1 C8 C13 79.6(2) . . . . ? C13 C8 C9 C10 0.6(2) . . . . ? C1 C8 C9 C10 -175.68(16) . . . . ? C13 C8 C9 N2 178.69(14) . . . . ? C1 C8 C9 N2 2.4(2) . . . . ? C25 N2 C9 C10 -108.64(19) . . . . ? C25 N2 C9 C8 73.2(2) . . . . ? C8 C9 C10 C11 0.0(3) . . . . ? N2 C9 C10 C11 -178.09(15) . . . . ? C9 C10 C11 C12 -0.2(3) . . . . ? C10 C11 C12 C13 -0.2(3) . . . . ? C11 C12 C13 C8 0.8(3) . . . . ? C11 C12 C13 C14 179.23(18) . . . . ? C9 C8 C13 C12 -1.0(2) . . . . ? C1 C8 C13 C12 175.43(15) . . . . ? C9 C8 C13 C14 -179.41(15) . . . . ? C1 C8 C13 C14 -3.0(2) . . . . ? C2 N1 C15 O1 3.7(3) . . . . ? C2 N1 C15 C16 -179.47(15) . . . . ? O1 C15 C16 C21 -109.7(2) . . . . ? N1 C15 C16 C21 73.5(2) . . . . ? O1 C15 C16 C17 69.7(2) . . . . ? N1 C15 C16 C17 -107.10(18) . . . . ? C21 C16 C17 C18 -1.8(3) . . . . ? C15 C16 C17 C18 178.73(14) . . . . ? C21 C16 C17 C22 179.29(17) . . . . ? C15 C16 C17 C22 -0.1(2) . . . . ? C16 C17 C18 C19 0.8(3) . . . . ? C22 C17 C18 C19 179.70(18) . . . . ? C17 C18 C19 C20 0.5(3) . . . . ? C17 C18 C19 C23 -179.96(17) . . . . ? C18 C19 C20 C21 -0.9(3) . . . . ? C23 C19 C20 C21 179.56(17) . . . . ? C19 C20 C21 C16 0.0(3) . . . . ? C19 C20 C21 C24 177.88(17) . . . . ? C17 C16 C21 C20 1.5(2) . . . . ? C15 C16 C21 C20 -179.13(15) . . . . ? C17 C16 C21 C24 -176.45(16) . . . . ? C15 C16 C21 C24 3.0(2) . . . . ? C9 N2 C25 O2 -6.6(3) . . . . ? C9 N2 C25 C26 175.22(15) . . . . ? O2 C25 C26 C31 107.0(2) . . . . ? N2 C25 C26 C31 -74.9(2) . . . . ? O2 C25 C26 C27 -71.3(2) . . . . ? N2 C25 C26 C27 106.81(18) . . . . ? C31 C26 C27 C28 3.3(2) . . . . ? C25 C26 C27 C28 -178.45(15) . . . . ? C31 C26 C27 C32 -176.59(16) . . . . ? C25 C26 C27 C32 1.7(2) . . . . ? C26 C27 C28 C29 -0.5(3) . . . . ? C32 C27 C28 C29 179.39(17) . . . . ? C27 C28 C29 C30 -2.7(3) . . . . ? C27 C28 C29 C33 177.55(17) . . . . ? C28 C29 C30 C31 3.2(3) . . . . ? C33 C29 C30 C31 -177.06(18) . . . . ? C29 C30 C31 C26 -0.5(3) . . . . ? C29 C30 C31 C34 -178.09(18) . . . . ? C27 C26 C31 C30 -2.8(2) . . . . ? C25 C26 C31 C30 178.95(15) . . . . ? C27 C26 C31 C34 174.78(16) . . . . ? C25 C26 C31 C34 -3.5(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A N1 H1 O2 0.93(2) 2.06(2) 2.7942(19) 134(2) . N2 H2 O1 0.94(2) 1.97(2) 2.8557(18) 156(2) 3_656 N1 H1 O2 0.93(2) 2.06(2) 2.7942(19) 134(2) . _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.85 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.167 _refine_diff_density_min -0.183 _refine_diff_density_rms 0.038 data_compound12 _database_code_depnum_ccdc_archive 'CCDC 775657' #TrackingRef '- compound 12.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H52 N5 Nb O2' _chemical_formula_sum 'C46 H52 N5 Nb O2' _chemical_formula_weight 799.84 _chemical_absolute_configuration rmad 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' Nb Nb -2.0727 0.6215 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.6800(18) _cell_length_b 13.465(2) _cell_length_c 13.696(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.561(2) _cell_angle_gamma 90.00 _cell_volume 2041.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 6935 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.9 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.301 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 0.338 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8709 _exptl_absorpt_correction_T_max 0.8879 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Rigaku Saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 26215 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.0648 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 27.88 _reflns_number_total 9650 _reflns_number_gt 8460 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.8' _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^)+(0.0277P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0470(9) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.025(18) _refine_ls_number_reflns 9650 _refine_ls_number_parameters 500 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0682 _refine_ls_wR_factor_gt 0.0673 _refine_ls_goodness_of_fit_ref 1.014 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.003 _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 Nb1 Nb 1.145192(15) 0.151981(16) 0.904740(12) 0.01791(6) Uani 1 1 d . . . O2 O 1.05070(13) 0.02501(12) 0.83794(11) 0.0199(3) Uani 1 1 d . . . O1 O 0.97351(13) 0.21894(13) 0.90106(11) 0.0209(3) Uani 1 1 d . . . N2 N 0.95870(17) -0.05707(14) 0.68472(14) 0.0193(4) Uani 1 1 d . . . N1 N 1.00989(16) 0.21033(14) 0.75448(13) 0.0177(4) Uani 1 1 d . . . N3 N 1.29467(17) 0.10924(15) 0.87895(15) 0.0256(4) Uani 1 1 d . . . N4 N 1.15234(16) 0.10631(15) 1.04262(13) 0.0219(4) Uani 1 1 d . . . N5 N 1.22122(16) 0.28585(15) 0.95100(14) 0.0217(4) Uani 1 1 d . . . C1 C 0.81290(19) 0.07718(17) 0.61818(16) 0.0180(5) Uani 1 1 d . . . C2 C 0.8459(2) -0.01233(17) 0.66871(16) 0.0183(5) Uani 1 1 d . . . C3 C 0.7571(2) -0.0719(2) 0.6929(2) 0.0237(6) Uani 1 1 d . . . H3 H 0.7806 -0.1329 0.7285 0.028 Uiso 1 1 calc R . . C4 C 0.6397(2) -0.04280(19) 0.66589(18) 0.0256(5) Uani 1 1 d . . . H4 H 0.5829 -0.0831 0.6841 0.031 Uiso 1 1 calc R . . C5 C 0.6009(2) 0.04672(18) 0.61089(17) 0.0228(5) Uani 1 1 d . . . C6 C 0.6879(2) 0.10745(18) 0.58581(17) 0.0208(5) Uani 1 1 d . . . C7 C 0.6469(2) 0.19527(19) 0.52899(17) 0.0238(5) Uani 1 1 d . . . H7 H 0.7033 0.2365 0.5113 0.029 Uiso 1 1 calc R . . C8 C 0.5278(2) 0.2223(2) 0.49893(18) 0.0318(6) Uani 1 1 d . . . H8 H 0.5025 0.2818 0.4610 0.038 Uiso 1 1 calc R . . C9 C 0.4421(2) 0.1618(3) 0.52419(17) 0.0349(6) Uani 1 1 d . . . H9 H 0.3595 0.1807 0.5031 0.042 Uiso 1 1 calc R . . C10 C 0.4781(2) 0.0774(2) 0.57829(18) 0.0306(6) Uani 1 1 d . . . H10 H 0.4199 0.0375 0.5950 0.037 Uiso 1 1 calc R . . C11 C 0.90141(18) 0.1387(2) 0.58358(15) 0.0186(5) Uani 1 1 d . . . C12 C 0.98708(19) 0.20130(17) 0.64640(16) 0.0189(5) Uani 1 1 d . . . C13 C 1.0650(2) 0.25682(18) 0.60596(17) 0.0222(5) Uani 1 1 d . . . H13 H 1.1248 0.2981 0.6510 0.027 Uiso 1 1 calc R . . C14 C 1.0568(2) 0.25282(18) 0.50523(17) 0.0235(5) Uani 1 1 d . . . H14 H 1.1076 0.2932 0.4797 0.028 Uiso 1 1 calc R . . C15 C 0.9718(2) 0.18796(17) 0.43793(16) 0.0206(5) Uani 1 1 d . . . C16 C 0.89606(18) 0.12925(15) 0.47679(15) 0.0185(5) Uani 1 1 d . . . C17 C 0.8163(2) 0.06156(18) 0.40923(17) 0.0237(5) Uani 1 1 d . . . H17 H 0.7673 0.0192 0.4347 0.028 Uiso 1 1 calc R . . C18 C 0.8090(2) 0.0565(2) 0.30761(18) 0.0282(6) Uani 1 1 d . . . H18 H 0.7550 0.0106 0.2634 0.034 Uiso 1 1 calc R . . C19 C 0.8808(2) 0.11869(19) 0.26780(18) 0.0283(6) Uani 1 1 d . . . H19 H 0.8730 0.1163 0.1966 0.034 Uiso 1 1 calc R . . C20 C 0.9608(2) 0.18181(17) 0.33137(17) 0.0250(6) Uani 1 1 d . . . H20 H 1.0102 0.2225 0.3046 0.030 Uiso 1 1 calc R . . C31 C 1.0508(2) -0.03711(17) 0.76319(16) 0.0188(5) Uani 1 1 d . . . C22 C 1.1645(2) -0.09297(17) 0.77178(17) 0.0204(5) Uani 1 1 d . . . C23 C 1.20955(19) -0.09461(17) 0.68711(16) 0.0213(5) Uani 1 1 d . . . C24 C 1.3102(2) -0.15295(18) 0.69447(18) 0.0246(5) Uani 1 1 d . . . H24 H 1.3414 -0.1537 0.6383 0.029 Uiso 1 1 calc R . . C25 C 1.3669(2) -0.21023(19) 0.78068(19) 0.0286(5) Uani 1 1 d . . . C26 C 1.3212(2) -0.2070(2) 0.86207(19) 0.0297(6) Uani 1 1 d . . . H26 H 1.3588 -0.2457 0.9217 0.036 Uiso 1 1 calc R . . C27 C 1.2213(2) -0.14869(19) 0.85929(18) 0.0257(5) Uani 1 1 d . . . C28 C 1.1517(2) -0.0369(2) 0.58940(17) 0.0261(5) Uani 1 1 d . . . H28A H 1.2097 -0.0294 0.5515 0.039 Uiso 1 1 calc R . . H28B H 1.1277 0.0288 0.6066 0.039 Uiso 1 1 calc R . . H28C H 1.0803 -0.0727 0.5466 0.039 Uiso 1 1 calc R . . C29 C 1.4706(2) -0.2768(2) 0.7825(2) 0.0418(7) Uani 1 1 d . . . H29A H 1.5014 -0.3092 0.8499 0.063 Uiso 1 1 calc R . . H29B H 1.5351 -0.2372 0.7701 0.063 Uiso 1 1 calc R . . H29C H 1.4431 -0.3274 0.7287 0.063 Uiso 1 1 calc R . . C30 C 1.1750(3) -0.1512(2) 0.9512(2) 0.0446(8) Uani 1 1 d . . . H30A H 1.2022 -0.0915 0.9931 0.067 Uiso 1 1 calc R . . H30B H 1.2065 -0.2103 0.9928 0.067 Uiso 1 1 calc R . . H30C H 1.0866 -0.1534 0.9268 0.067 Uiso 1 1 calc R . . C21 C 0.93308(19) 0.23568(17) 0.80274(16) 0.0182(5) Uani 1 1 d . . . C32 C 0.8132(2) 0.28419(17) 0.76122(16) 0.0195(5) Uani 1 1 d . . . C33 C 0.7150(2) 0.24311(18) 0.78673(17) 0.0215(5) Uani 1 1 d . . . C34 C 0.6055(2) 0.2932(2) 0.75408(19) 0.0288(6) Uani 1 1 d . . . H34 H 0.5385 0.2660 0.7699 0.035 Uiso 1 1 calc R . . C35 C 0.5902(2) 0.3814(2) 0.6992(2) 0.0318(6) Uani 1 1 d . . . C36 C 0.6892(2) 0.4217(2) 0.67772(18) 0.0290(6) Uani 1 1 d . . . H36 H 0.6802 0.4826 0.6411 0.035 Uiso 1 1 calc R . . C37 C 0.8007(2) 0.3749(2) 0.70852(18) 0.0226(6) Uani 1 1 d . . . C38 C 0.72546(18) 0.1475(3) 0.84501(15) 0.0241(4) Uani 1 1 d . . . H38A H 0.7657 0.1598 0.9185 0.036 Uiso 1 1 calc R . . H38B H 0.7728 0.0999 0.8197 0.036 Uiso 1 1 calc R . . H38C H 0.6446 0.1204 0.8349 0.036 Uiso 1 1 calc R . . C39 C 0.4683(3) 0.4325(2) 0.6622(2) 0.0486(8) Uani 1 1 d . . . H39A H 0.4767 0.4969 0.6318 0.073 Uiso 1 1 calc R . . H39B H 0.4382 0.4427 0.7205 0.073 Uiso 1 1 calc R . . H39C H 0.4113 0.3910 0.6102 0.073 Uiso 1 1 calc R . . C40 C 0.9069(2) 0.42599(18) 0.68778(18) 0.0272(5) Uani 1 1 d . . . H40A H 0.9796 0.4177 0.7475 0.041 Uiso 1 1 calc R . . H40B H 0.8892 0.4969 0.6755 0.041 Uiso 1 1 calc R . . H40C H 0.9202 0.3963 0.6270 0.041 Uiso 1 1 calc R . . C41 C 1.3968(2) 0.0602(2) 0.9531(2) 0.0391(7) Uani 1 1 d . . . H41A H 1.4124 -0.0033 0.9247 0.059 Uiso 1 1 calc R . . H41B H 1.3783 0.0482 1.0171 0.059 Uiso 1 1 calc R . . H41C H 1.4685 0.1026 0.9675 0.059 Uiso 1 1 calc R . . C42 C 1.3188(2) 0.1271(2) 0.78207(19) 0.0361(7) Uani 1 1 d . . . H42A H 1.3875 0.1725 0.7942 0.054 Uiso 1 1 calc R . . H42B H 1.2473 0.1568 0.7321 0.054 Uiso 1 1 calc R . . H42C H 1.3376 0.0640 0.7549 0.054 Uiso 1 1 calc R . . C43 C 1.0552(2) 0.0433(2) 1.05623(18) 0.0309(6) Uani 1 1 d . . . H43A H 1.0908 -0.0120 1.1024 0.046 Uiso 1 1 calc R . . H43B H 1.0060 0.0172 0.9892 0.046 Uiso 1 1 calc R . . H43C H 1.0043 0.0829 1.0861 0.046 Uiso 1 1 calc R . . C44 C 1.2180(2) 0.1534(3) 1.14059(16) 0.0425(6) Uani 1 1 d . . . H44A H 1.1608 0.1882 1.1677 0.064 Uiso 1 1 calc R . . H44B H 1.2763 0.2011 1.1299 0.064 Uiso 1 1 calc R . . H44C H 1.2609 0.1026 1.1899 0.064 Uiso 1 1 calc R . . C45 C 1.1617(2) 0.3661(2) 0.9886(2) 0.0429(7) Uani 1 1 d . . . H45A H 1.2158 0.3907 1.0545 0.064 Uiso 1 1 calc R . . H45B H 1.0872 0.3410 0.9982 0.064 Uiso 1 1 calc R . . H45C H 1.1421 0.4203 0.9383 0.064 Uiso 1 1 calc R . . C46 C 1.3355(2) 0.3250(2) 0.9443(2) 0.0330(6) Uani 1 1 d . . . H46A H 1.3189 0.3763 0.8909 0.050 Uiso 1 1 calc R . . H46B H 1.3818 0.2711 0.9269 0.050 Uiso 1 1 calc R . . H46C H 1.3821 0.3539 1.0108 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 Nb1 0.01633(9) 0.02000(9) 0.01781(9) -0.00147(11) 0.00603(6) -0.00157(11) O2 0.0232(8) 0.0181(8) 0.0193(8) -0.0040(7) 0.0080(6) -0.0035(7) O1 0.0175(8) 0.0274(9) 0.0189(8) -0.0016(7) 0.0072(6) -0.0001(7) N2 0.0222(10) 0.0160(10) 0.0213(10) 0.0021(8) 0.0090(8) 0.0003(8) N1 0.0182(9) 0.0173(10) 0.0176(9) 0.0002(8) 0.0059(7) -0.0028(8) N3 0.0212(10) 0.0253(10) 0.0331(11) -0.0063(9) 0.0126(8) -0.0034(8) N4 0.0206(10) 0.0273(11) 0.0172(9) -0.0002(8) 0.0050(7) -0.0039(8) N5 0.0191(10) 0.0217(11) 0.0232(10) -0.0045(8) 0.0051(8) -0.0033(8) C1 0.0188(11) 0.0188(11) 0.0167(10) -0.0038(9) 0.0060(9) -0.0038(9) C2 0.0211(12) 0.0182(12) 0.0156(11) -0.0054(9) 0.0060(9) -0.0030(9) C3 0.0314(15) 0.0176(13) 0.0241(13) -0.0024(10) 0.0116(11) -0.0061(11) C4 0.0246(13) 0.0277(14) 0.0271(13) -0.0056(11) 0.0119(10) -0.0100(11) C5 0.0202(12) 0.0250(13) 0.0223(12) -0.0071(10) 0.0058(9) -0.0066(10) C6 0.0215(12) 0.0241(12) 0.0180(11) -0.0026(10) 0.0078(9) -0.0009(10) C7 0.0261(13) 0.0270(13) 0.0181(12) -0.0008(10) 0.0066(10) 0.0002(10) C8 0.0300(14) 0.0364(15) 0.0259(13) 0.0033(12) 0.0045(10) 0.0105(12) C9 0.0185(11) 0.0498(19) 0.0329(12) -0.0047(16) 0.0034(9) 0.0082(15) C10 0.0202(13) 0.0412(16) 0.0308(13) -0.0076(12) 0.0087(10) -0.0074(11) C11 0.0169(9) 0.0199(15) 0.0205(9) 0.0035(10) 0.0083(7) 0.0040(10) C12 0.0187(12) 0.0187(12) 0.0197(11) 0.0016(9) 0.0064(9) 0.0024(9) C13 0.0229(12) 0.0183(12) 0.0269(12) 0.0010(10) 0.0099(10) -0.0044(9) C14 0.0271(12) 0.0190(12) 0.0293(13) 0.0030(10) 0.0160(10) -0.0012(10) C15 0.0222(12) 0.0187(11) 0.0220(11) 0.0027(9) 0.0086(9) 0.0067(9) C16 0.0163(10) 0.0198(15) 0.0187(10) 0.0029(8) 0.0045(8) 0.0046(8) C17 0.0231(12) 0.0242(13) 0.0255(12) -0.0026(10) 0.0102(10) -0.0001(10) C18 0.0247(13) 0.0342(15) 0.0243(12) -0.0079(11) 0.0056(10) 0.0013(11) C19 0.0290(13) 0.0380(16) 0.0192(11) 0.0008(10) 0.0096(10) 0.0092(10) C20 0.0285(13) 0.0256(14) 0.0253(12) 0.0066(9) 0.0147(10) 0.0078(9) C31 0.0241(12) 0.0159(11) 0.0180(11) 0.0026(9) 0.0091(9) -0.0025(9) C22 0.0222(11) 0.0164(11) 0.0219(11) -0.0002(9) 0.0060(9) -0.0010(9) C23 0.0206(12) 0.0223(13) 0.0201(12) -0.0032(10) 0.0054(9) -0.0027(10) C24 0.0213(12) 0.0259(13) 0.0265(13) -0.0037(10) 0.0075(10) -0.0018(10) C25 0.0238(13) 0.0237(13) 0.0355(14) -0.0028(11) 0.0054(10) 0.0015(10) C26 0.0305(14) 0.0248(14) 0.0284(13) 0.0071(11) 0.0020(10) 0.0053(11) C27 0.0308(13) 0.0218(13) 0.0251(12) 0.0024(10) 0.0097(10) 0.0024(10) C28 0.0245(13) 0.0349(15) 0.0198(12) 0.0012(11) 0.0083(10) 0.0007(11) C29 0.0329(16) 0.0411(17) 0.0488(17) 0.0004(15) 0.0094(13) 0.0129(13) C30 0.062(2) 0.0446(18) 0.0325(15) 0.0204(14) 0.0221(14) 0.0248(16) C21 0.0168(11) 0.0160(11) 0.0213(11) -0.0013(9) 0.0053(9) -0.0051(9) C32 0.0216(11) 0.0180(11) 0.0191(11) -0.0044(9) 0.0068(9) -0.0009(9) C33 0.0214(12) 0.0213(12) 0.0219(11) -0.0062(10) 0.0071(9) -0.0033(9) C34 0.0213(12) 0.0332(15) 0.0327(13) -0.0053(12) 0.0098(10) -0.0011(11) C35 0.0253(13) 0.0314(15) 0.0342(14) -0.0064(12) 0.0031(11) 0.0087(11) C36 0.0343(14) 0.0232(14) 0.0257(13) -0.0024(11) 0.0041(10) 0.0042(12) C37 0.0280(14) 0.0206(13) 0.0175(12) -0.0027(10) 0.0049(10) -0.0013(11) C38 0.0229(10) 0.0260(11) 0.0260(10) -0.0022(15) 0.0114(8) 0.0001(15) C39 0.0329(16) 0.050(2) 0.059(2) 0.0027(16) 0.0097(14) 0.0192(15) C40 0.0343(14) 0.0208(13) 0.0266(13) 0.0020(10) 0.0101(11) -0.0018(11) C41 0.0232(14) 0.0440(18) 0.0494(17) -0.0040(14) 0.0105(12) 0.0043(12) C42 0.0294(13) 0.043(2) 0.0442(14) -0.0067(12) 0.0232(11) -0.0092(11) C43 0.0352(14) 0.0371(16) 0.0239(12) 0.0009(11) 0.0143(11) -0.0086(12) C44 0.0425(14) 0.0577(17) 0.0220(11) 0.0024(19) 0.0030(10) -0.017(2) C45 0.0309(16) 0.0329(17) 0.067(2) -0.0227(15) 0.0179(14) -0.0052(12) C46 0.0289(14) 0.0273(14) 0.0450(16) -0.0044(12) 0.0146(12) -0.0068(11) _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 Nb1 N4 1.9623(18) . ? Nb1 N3 1.9740(19) . ? Nb1 N5 2.020(2) . ? Nb1 O2 2.0821(15) . ? Nb1 O1 2.1845(15) . ? Nb1 N1 2.2977(18) . ? Nb1 C21 2.675(2) . ? O2 C31 1.322(3) . ? O1 C21 1.297(2) . ? N2 C31 1.284(3) . ? N2 C2 1.401(3) . ? N1 C21 1.317(3) . ? N1 C12 1.423(3) . ? N3 C41 1.456(3) . ? N3 C42 1.461(3) . ? N4 C44 1.461(3) . ? N4 C43 1.475(3) . ? N5 C45 1.464(3) . ? N5 C46 1.465(3) . ? C1 C2 1.382(3) . ? C1 C6 1.443(3) . ? C1 C11 1.514(3) . ? C2 C3 1.432(3) . ? C3 C4 1.359(4) . ? C3 H3 0.9500 . ? C4 C5 1.417(3) . ? C4 H4 0.9500 . ? C5 C10 1.421(3) . ? C5 C6 1.429(3) . ? C6 C7 1.413(3) . ? C7 C8 1.369(3) . ? C7 H7 0.9500 . ? C8 C9 1.416(4) . ? C8 H8 0.9500 . ? C9 C10 1.348(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.380(3) . ? C11 C16 1.449(3) . ? C12 C13 1.420(3) . ? C13 C14 1.353(3) . ? C13 H13 0.9500 . ? C14 C15 1.419(3) . ? C14 H14 0.9500 . ? C15 C16 1.411(3) . ? C15 C20 1.426(3) . ? C16 C17 1.416(3) . ? C17 C18 1.369(3) . ? C17 H17 0.9500 . ? C18 C19 1.412(3) . ? C18 H18 0.9500 . ? C19 C20 1.355(3) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C31 C22 1.498(3) . ? C22 C27 1.391(3) . ? C22 C23 1.418(3) . ? C23 C24 1.391(3) . ? C23 C28 1.508(3) . ? C24 C25 1.389(3) . ? C24 H24 0.9500 . ? C25 C26 1.382(3) . ? C25 C29 1.501(3) . ? C26 C27 1.397(3) . ? C26 H26 0.9500 . ? C27 C30 1.520(3) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C21 C32 1.485(3) . ? C32 C37 1.402(3) . ? C32 C33 1.413(3) . ? C33 C34 1.388(3) . ? C33 C38 1.499(4) . ? C34 C35 1.386(4) . ? C34 H34 0.9500 . ? C35 C36 1.391(4) . ? C35 C39 1.516(3) . ? C36 C37 1.386(3) . ? C36 H36 0.9500 . ? C37 C40 1.522(3) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Nb1 N3 108.16(8) . . ? N4 Nb1 N5 95.63(8) . . ? N3 Nb1 N5 89.47(8) . . ? N4 Nb1 O2 91.13(7) . . ? N3 Nb1 O2 93.29(7) . . ? N5 Nb1 O2 171.53(7) . . ? N4 Nb1 O1 84.78(7) . . ? N3 Nb1 O1 166.87(7) . . ? N5 Nb1 O1 87.00(7) . . ? O2 Nb1 O1 88.54(6) . . ? N4 Nb1 N1 140.85(7) . . ? N3 Nb1 N1 109.56(7) . . ? N5 Nb1 N1 94.82(7) . . ? O2 Nb1 N1 76.70(6) . . ? O1 Nb1 N1 58.24(6) . . ? N4 Nb1 C21 112.53(7) . . ? N3 Nb1 C21 138.96(7) . . ? N5 Nb1 C21 91.68(7) . . ? O2 Nb1 C21 80.98(7) . . ? O1 Nb1 C21 28.76(6) . . ? N1 Nb1 C21 29.49(6) . . ? C31 O2 Nb1 136.77(14) . . ? C21 O1 Nb1 97.11(12) . . ? C31 N2 C2 122.45(19) . . ? C21 N1 C12 127.73(18) . . ? C21 N1 Nb1 91.34(13) . . ? C12 N1 Nb1 138.58(14) . . ? C41 N3 C42 110.9(2) . . ? C41 N3 Nb1 125.61(16) . . ? C42 N3 Nb1 123.47(17) . . ? C44 N4 C43 109.47(18) . . ? C44 N4 Nb1 126.64(18) . . ? C43 N4 Nb1 120.20(14) . . ? C45 N5 C46 107.5(2) . . ? C45 N5 Nb1 123.92(16) . . ? C46 N5 Nb1 128.32(16) . . ? C2 C1 C6 119.6(2) . . ? C2 C1 C11 121.6(2) . . ? C6 C1 C11 118.3(2) . . ? C1 C2 N2 123.52(19) . . ? C1 C2 C3 119.8(2) . . ? N2 C2 C3 115.9(2) . . ? C4 C3 C2 121.2(2) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 121.0(2) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C4 C5 C10 122.3(2) . . ? C4 C5 C6 118.8(2) . . ? C10 C5 C6 118.8(2) . . ? C7 C6 C5 118.0(2) . . ? C7 C6 C1 122.5(2) . . ? C5 C6 C1 119.5(2) . . ? C8 C7 C6 121.4(2) . . ? C8 C7 H7 119.3 . . ? C6 C7 H7 119.3 . . ? C7 C8 C9 120.2(3) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C10 C9 C8 119.9(2) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C5 121.6(2) . . ? C9 C10 H10 119.2 . . ? C5 C10 H10 119.2 . . ? C12 C11 C16 118.19(19) . . ? C12 C11 C1 124.83(18) . . ? C16 C11 C1 116.97(19) . . ? C11 C12 C13 120.42(19) . . ? C11 C12 N1 124.00(19) . . ? C13 C12 N1 115.45(19) . . ? C14 C13 C12 122.0(2) . . ? C14 C13 H13 119.0 . . ? C12 C13 H13 119.0 . . ? C13 C14 C15 119.7(2) . . ? C13 C14 H14 120.2 . . ? C15 C14 H14 120.2 . . ? C16 C15 C14 119.50(19) . . ? C16 C15 C20 119.4(2) . . ? C14 C15 C20 121.1(2) . . ? C15 C16 C17 118.37(19) . . ? C15 C16 C11 120.0(2) . . ? C17 C16 C11 121.6(2) . . ? C18 C17 C16 120.8(2) . . ? C18 C17 H17 119.6 . . ? C16 C17 H17 119.6 . . ? C17 C18 C19 120.7(2) . . ? C17 C18 H18 119.7 . . ? C19 C18 H18 119.7 . . ? C20 C19 C18 119.8(2) . . ? C20 C19 H19 120.1 . . ? C18 C19 H19 120.1 . . ? C19 C20 C15 120.9(2) . . ? C19 C20 H20 119.6 . . ? C15 C20 H20 119.6 . . ? N2 C31 O2 125.0(2) . . ? N2 C31 C22 116.5(2) . . ? O2 C31 C22 118.43(19) . . ? C27 C22 C23 119.8(2) . . ? C27 C22 C31 120.4(2) . . ? C23 C22 C31 119.61(19) . . ? C24 C23 C22 118.3(2) . . ? C24 C23 C28 119.0(2) . . ? C22 C23 C28 122.7(2) . . ? C25 C24 C23 122.6(2) . . ? C25 C24 H24 118.7 . . ? C23 C24 H24 118.7 . . ? C26 C25 C24 117.8(2) . . ? C26 C25 C29 121.5(2) . . ? C24 C25 C29 120.6(2) . . ? C25 C26 C27 122.0(2) . . ? C25 C26 H26 119.0 . . ? C27 C26 H26 119.0 . . ? C22 C27 C26 119.5(2) . . ? C22 C27 C30 121.9(2) . . ? C26 C27 C30 118.6(2) . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O1 C21 N1 113.25(19) . . ? O1 C21 C32 117.48(18) . . ? N1 C21 C32 129.18(19) . . ? O1 C21 Nb1 54.13(10) . . ? N1 C21 Nb1 59.17(11) . . ? C32 C21 Nb1 171.58(15) . . ? C37 C32 C33 120.6(2) . . ? C37 C32 C21 120.7(2) . . ? C33 C32 C21 118.3(2) . . ? C34 C33 C32 117.8(2) . . ? C34 C33 C38 119.9(2) . . ? C32 C33 C38 122.2(2) . . ? C35 C34 C33 122.5(2) . . ? C35 C34 H34 118.7 . . ? C33 C34 H34 118.7 . . ? C34 C35 C36 118.4(2) . . ? C34 C35 C39 121.0(3) . . ? C36 C35 C39 120.5(3) . . ? C37 C36 C35 121.5(3) . . ? C37 C36 H36 119.2 . . ? C35 C36 H36 119.2 . . ? C36 C37 C32 119.1(2) . . ? C36 C37 C40 118.7(2) . . ? C32 C37 C40 122.2(2) . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C35 C39 H39A 109.5 . . ? C35 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C35 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N3 C41 H41A 109.5 . . ? N3 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N3 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N3 C42 H42A 109.5 . . ? N3 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N3 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N4 C43 H43A 109.5 . . ? N4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N4 C44 H44A 109.5 . . ? N4 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N4 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N5 C45 H45A 109.5 . . ? N5 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N5 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N5 C46 H46A 109.5 . . ? N5 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N5 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Nb1 O2 C31 -139.7(2) . . . . ? N3 Nb1 O2 C31 -31.4(2) . . . . ? N5 Nb1 O2 C31 77.4(5) . . . . ? O1 Nb1 O2 C31 135.6(2) . . . . ? N1 Nb1 O2 C31 77.9(2) . . . . ? C21 Nb1 O2 C31 107.7(2) . . . . ? N4 Nb1 O1 C21 -165.04(14) . . . . ? N3 Nb1 O1 C21 24.4(4) . . . . ? N5 Nb1 O1 C21 99.02(14) . . . . ? O2 Nb1 O1 C21 -73.77(13) . . . . ? N1 Nb1 O1 C21 1.46(12) . . . . ? N4 Nb1 N1 C21 20.16(19) . . . . ? N3 Nb1 N1 C21 -176.03(13) . . . . ? N5 Nb1 N1 C21 -84.88(14) . . . . ? O2 Nb1 N1 C21 95.20(13) . . . . ? O1 Nb1 N1 C21 -1.43(12) . . . . ? N4 Nb1 N1 C12 -142.0(2) . . . . ? N3 Nb1 N1 C12 21.8(2) . . . . ? N5 Nb1 N1 C12 113.0(2) . . . . ? O2 Nb1 N1 C12 -66.9(2) . . . . ? O1 Nb1 N1 C12 -163.6(2) . . . . ? C21 Nb1 N1 C12 -162.1(3) . . . . ? N4 Nb1 N3 C41 -5.0(2) . . . . ? N5 Nb1 N3 C41 90.8(2) . . . . ? O2 Nb1 N3 C41 -97.2(2) . . . . ? O1 Nb1 N3 C41 165.1(3) . . . . ? N1 Nb1 N3 C41 -174.3(2) . . . . ? C21 Nb1 N3 C41 -177.27(18) . . . . ? N4 Nb1 N3 C42 177.66(18) . . . . ? N5 Nb1 N3 C42 -86.59(19) . . . . ? O2 Nb1 N3 C42 85.39(18) . . . . ? O1 Nb1 N3 C42 -12.3(4) . . . . ? N1 Nb1 N3 C42 8.3(2) . . . . ? C21 Nb1 N3 C42 5.4(2) . . . . ? N3 Nb1 N4 C44 80.1(2) . . . . ? N5 Nb1 N4 C44 -11.2(2) . . . . ? O2 Nb1 N4 C44 174.0(2) . . . . ? O1 Nb1 N4 C44 -97.6(2) . . . . ? N1 Nb1 N4 C44 -115.9(2) . . . . ? C21 Nb1 N4 C44 -105.3(2) . . . . ? N3 Nb1 N4 C43 -123.89(18) . . . . ? N5 Nb1 N4 C43 144.82(18) . . . . ? O2 Nb1 N4 C43 -30.06(18) . . . . ? O1 Nb1 N4 C43 58.37(18) . . . . ? N1 Nb1 N4 C43 40.1(2) . . . . ? C21 Nb1 N4 C43 50.6(2) . . . . ? N4 Nb1 N5 C45 -70.0(2) . . . . ? N3 Nb1 N5 C45 -178.2(2) . . . . ? O2 Nb1 N5 C45 72.7(5) . . . . ? O1 Nb1 N5 C45 14.5(2) . . . . ? N1 Nb1 N5 C45 72.2(2) . . . . ? C21 Nb1 N5 C45 42.8(2) . . . . ? N4 Nb1 N5 C46 116.8(2) . . . . ? N3 Nb1 N5 C46 8.6(2) . . . . ? O2 Nb1 N5 C46 -100.5(5) . . . . ? O1 Nb1 N5 C46 -158.8(2) . . . . ? N1 Nb1 N5 C46 -101.0(2) . . . . ? C21 Nb1 N5 C46 -130.4(2) . . . . ? C6 C1 C2 N2 166.8(2) . . . . ? C11 C1 C2 N2 -5.2(3) . . . . ? C6 C1 C2 C3 -3.0(3) . . . . ? C11 C1 C2 C3 -175.1(2) . . . . ? C31 N2 C2 C1 87.3(3) . . . . ? C31 N2 C2 C3 -102.5(3) . . . . ? C1 C2 C3 C4 0.9(4) . . . . ? N2 C2 C3 C4 -169.7(2) . . . . ? C2 C3 C4 C5 1.3(4) . . . . ? C3 C4 C5 C10 177.7(2) . . . . ? C3 C4 C5 C6 -1.2(3) . . . . ? C4 C5 C6 C7 178.6(2) . . . . ? C10 C5 C6 C7 -0.3(3) . . . . ? C4 C5 C6 C1 -0.9(3) . . . . ? C10 C5 C6 C1 -179.9(2) . . . . ? C2 C1 C6 C7 -176.48(19) . . . . ? C11 C1 C6 C7 -4.1(3) . . . . ? C2 C1 C6 C5 3.0(3) . . . . ? C11 C1 C6 C5 175.37(19) . . . . ? C5 C6 C7 C8 0.3(3) . . . . ? C1 C6 C7 C8 179.8(2) . . . . ? C6 C7 C8 C9 -0.2(4) . . . . ? C7 C8 C9 C10 0.2(4) . . . . ? C8 C9 C10 C5 -0.2(4) . . . . ? C4 C5 C10 C9 -178.6(2) . . . . ? C6 C5 C10 C9 0.3(3) . . . . ? C2 C1 C11 C12 -80.9(3) . . . . ? C6 C1 C11 C12 106.9(3) . . . . ? C2 C1 C11 C16 98.1(2) . . . . ? C6 C1 C11 C16 -74.1(3) . . . . ? C16 C11 C12 C13 1.8(3) . . . . ? C1 C11 C12 C13 -179.2(2) . . . . ? C16 C11 C12 N1 -173.77(19) . . . . ? C1 C11 C12 N1 5.2(4) . . . . ? C21 N1 C12 C11 -58.2(3) . . . . ? Nb1 N1 C12 C11 99.0(3) . . . . ? C21 N1 C12 C13 126.0(2) . . . . ? Nb1 N1 C12 C13 -76.8(3) . . . . ? C11 C12 C13 C14 1.7(3) . . . . ? N1 C12 C13 C14 177.7(2) . . . . ? C12 C13 C14 C15 -3.0(4) . . . . ? C13 C14 C15 C16 0.7(3) . . . . ? C13 C14 C15 C20 -179.9(2) . . . . ? C14 C15 C16 C17 -176.9(2) . . . . ? C20 C15 C16 C17 3.7(3) . . . . ? C14 C15 C16 C11 2.8(3) . . . . ? C20 C15 C16 C11 -176.6(2) . . . . ? C12 C11 C16 C15 -4.0(3) . . . . ? C1 C11 C16 C15 176.9(2) . . . . ? C12 C11 C16 C17 175.7(2) . . . . ? C1 C11 C16 C17 -3.4(3) . . . . ? C15 C16 C17 C18 -2.9(3) . . . . ? C11 C16 C17 C18 177.4(2) . . . . ? C16 C17 C18 C19 -0.1(4) . . . . ? C17 C18 C19 C20 2.3(4) . . . . ? C18 C19 C20 C15 -1.4(4) . . . . ? C16 C15 C20 C19 -1.6(3) . . . . ? C14 C15 C20 C19 179.0(2) . . . . ? C2 N2 C31 O2 1.3(3) . . . . ? C2 N2 C31 C22 178.22(19) . . . . ? Nb1 O2 C31 N2 -123.2(2) . . . . ? Nb1 O2 C31 C22 59.9(3) . . . . ? N2 C31 C22 C27 -123.5(2) . . . . ? O2 C31 C22 C27 53.7(3) . . . . ? N2 C31 C22 C23 52.1(3) . . . . ? O2 C31 C22 C23 -130.8(2) . . . . ? C27 C22 C23 C24 0.2(3) . . . . ? C31 C22 C23 C24 -175.4(2) . . . . ? C27 C22 C23 C28 179.3(2) . . . . ? C31 C22 C23 C28 3.8(3) . . . . ? C22 C23 C24 C25 0.8(4) . . . . ? C28 C23 C24 C25 -178.4(2) . . . . ? C23 C24 C25 C26 -0.9(4) . . . . ? C23 C24 C25 C29 176.3(2) . . . . ? C24 C25 C26 C27 0.0(4) . . . . ? C29 C25 C26 C27 -177.1(3) . . . . ? C23 C22 C27 C26 -1.0(4) . . . . ? C31 C22 C27 C26 174.5(2) . . . . ? C23 C22 C27 C30 -178.7(2) . . . . ? C31 C22 C27 C30 -3.2(4) . . . . ? C25 C26 C27 C22 0.9(4) . . . . ? C25 C26 C27 C30 178.7(3) . . . . ? Nb1 O1 C21 N1 -2.4(2) . . . . ? Nb1 O1 C21 C32 -179.29(17) . . . . ? C12 N1 C21 O1 167.4(2) . . . . ? Nb1 N1 C21 O1 2.23(19) . . . . ? C12 N1 C21 C32 -16.2(4) . . . . ? Nb1 N1 C21 C32 178.7(2) . . . . ? C12 N1 C21 Nb1 165.1(2) . . . . ? N4 Nb1 C21 O1 16.16(15) . . . . ? N3 Nb1 C21 O1 -171.77(14) . . . . ? N5 Nb1 C21 O1 -80.64(13) . . . . ? O2 Nb1 C21 O1 103.62(13) . . . . ? N1 Nb1 C21 O1 -177.5(2) . . . . ? N4 Nb1 C21 N1 -166.37(13) . . . . ? N3 Nb1 C21 N1 5.70(19) . . . . ? N5 Nb1 C21 N1 96.83(14) . . . . ? O2 Nb1 C21 N1 -78.91(13) . . . . ? O1 Nb1 C21 N1 177.5(2) . . . . ? N4 Nb1 C21 C32 20.5(11) . . . . ? N3 Nb1 C21 C32 -167.4(11) . . . . ? N5 Nb1 C21 C32 -76.3(11) . . . . ? O2 Nb1 C21 C32 108.0(11) . . . . ? O1 Nb1 C21 C32 4.3(10) . . . . ? N1 Nb1 C21 C32 -173.1(12) . . . . ? O1 C21 C32 C37 121.1(2) . . . . ? N1 C21 C32 C37 -55.3(3) . . . . ? Nb1 C21 C32 C37 117.1(10) . . . . ? O1 C21 C32 C33 -51.4(3) . . . . ? N1 C21 C32 C33 132.2(2) . . . . ? Nb1 C21 C32 C33 -55.4(12) . . . . ? C37 C32 C33 C34 2.7(3) . . . . ? C21 C32 C33 C34 175.2(2) . . . . ? C37 C32 C33 C38 -178.6(2) . . . . ? C21 C32 C33 C38 -6.1(3) . . . . ? C32 C33 C34 C35 -0.8(3) . . . . ? C38 C33 C34 C35 -179.5(2) . . . . ? C33 C34 C35 C36 -1.0(4) . . . . ? C33 C34 C35 C39 178.2(2) . . . . ? C34 C35 C36 C37 1.0(4) . . . . ? C39 C35 C36 C37 -178.3(2) . . . . ? C35 C36 C37 C32 0.9(4) . . . . ? C35 C36 C37 C40 -176.6(2) . . . . ? C33 C32 C37 C36 -2.8(3) . . . . ? C21 C32 C37 C36 -175.1(2) . . . . ? C33 C32 C37 C40 174.6(2) . . . . ? C21 C32 C37 C40 2.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.779 _refine_diff_density_min -0.539 _refine_diff_density_rms 0.065 # Attachment 'compound-5.cif.txt' data_compound5 _database_code_depnum_ccdc_archive 'CCDC 775658' #TrackingRef 'compound-5.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H52 N5 O2 Ta' _chemical_formula_sum 'C46 H52 N5 O2 Ta' _chemical_formula_weight 887.88 _chemical_absolute_configuration rmad 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' Ta Ta -0.7052 6.5227 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.687(2) _cell_length_b 13.451(3) _cell_length_c 13.686(3) _cell_angle_alpha 90.00 _cell_angle_beta 108.63(3) _cell_angle_gamma 90.00 _cell_volume 2038.8(7) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 8175 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.9 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.446 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 2.739 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5840 _exptl_absorpt_correction_T_max 0.7003 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Rigaku Saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 18042 _diffrn_reflns_av_R_equivalents 0.0397 _diffrn_reflns_av_sigmaI/netI 0.0396 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 27.92 _reflns_number_total 9255 _reflns_number_gt 9010 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.8' _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. The sample crystal was a twinned crystal and one domain was used for refinement and a high residual electron density was observed near H39A. ; _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^)+(0.0562P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0447(10) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.001(7) _refine_ls_number_reflns 9255 _refine_ls_number_parameters 500 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0359 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0849 _refine_ls_wR_factor_gt 0.0843 _refine_ls_goodness_of_fit_ref 1.116 _refine_ls_restrained_S_all 1.116 _refine_ls_shift/su_max 0.110 _refine_ls_shift/su_mean 0.005 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ta1 Ta 0.356771(10) 0.25329(2) 0.096430(9) 0.01923(7) Uani 1 1 d . . . N1 N 0.4909(3) 0.3113(2) 0.2469(3) 0.0200(6) Uani 1 1 d . . . N2 N 0.5412(3) 0.0448(2) 0.3159(3) 0.0213(7) Uani 1 1 d . . . N3 N 0.3473(3) 0.2059(3) -0.0416(3) 0.0249(7) Uani 1 1 d . . . N4 N 0.2082(3) 0.2117(3) 0.1258(3) 0.0281(8) Uani 1 1 d . . . N5 N 0.2822(3) 0.3875(3) 0.0499(3) 0.0240(7) Uani 1 1 d . . . O1 O 0.5266(2) 0.3186(2) 0.1004(2) 0.0227(6) Uani 1 1 d . . . O2 O 0.4493(3) 0.1265(2) 0.1612(2) 0.0221(6) Uani 1 1 d . . . C1 C 0.5992(3) 0.2395(3) 0.4177(3) 0.0195(8) Uani 1 1 d . . . C2 C 0.5139(4) 0.3014(3) 0.3546(3) 0.0208(7) Uani 1 1 d . . . C3 C 0.4360(4) 0.3575(3) 0.3958(3) 0.0246(8) Uani 1 1 d . . . H3A H 0.3765 0.3991 0.3509 0.030 Uiso 1 1 calc R . . C4 C 0.4442(4) 0.3532(3) 0.4967(3) 0.0259(8) Uani 1 1 d . . . H4A H 0.3932 0.3932 0.5223 0.031 Uiso 1 1 calc R . . C5 C 0.5288(4) 0.2888(3) 0.5632(3) 0.0232(8) Uani 1 1 d . . . C6 C 0.6040(3) 0.2297(3) 0.5240(3) 0.0219(8) Uani 1 1 d . . . C7 C 0.6854(4) 0.1623(3) 0.5918(3) 0.0267(8) Uani 1 1 d . . . H7 H 0.7356 0.1212 0.5663 0.032 Uiso 1 1 calc R . . C8 C 0.6920(4) 0.1559(4) 0.6938(4) 0.0314(9) Uani 1 1 d . . . H8 H 0.7448 0.1090 0.7377 0.038 Uiso 1 1 calc R . . C9 C 0.6205(4) 0.2189(4) 0.7336(4) 0.0301(9) Uani 1 1 d . . . H9 H 0.6294 0.2172 0.8050 0.036 Uiso 1 1 calc R . . C10 C 0.5391(4) 0.2820(3) 0.6701(4) 0.0278(10) Uani 1 1 d . . . H10 H 0.4889 0.3217 0.6969 0.033 Uiso 1 1 calc R . . C11 C 0.6867(4) 0.1783(3) 0.3820(3) 0.0207(7) Uani 1 1 d . . . C12 C 0.6543(3) 0.0890(3) 0.3317(3) 0.0194(7) Uani 1 1 d . . . C13 C 0.7414(5) 0.0291(4) 0.3068(4) 0.0260(10) Uani 1 1 d . . . H13 H 0.7172 -0.0319 0.2711 0.031 Uiso 1 1 calc R . . C14 C 0.8599(4) 0.0585(3) 0.3337(4) 0.0285(9) Uani 1 1 d . . . H14 H 0.9165 0.0186 0.3147 0.034 Uiso 1 1 calc R . . C15 C 0.8986(4) 0.1476(3) 0.3892(3) 0.0260(9) Uani 1 1 d . . . C16 C 0.8115(4) 0.2088(3) 0.4132(3) 0.0238(8) Uani 1 1 d . . . C17 C 0.8531(4) 0.2957(3) 0.4715(4) 0.0273(8) Uani 1 1 d . . . H17 H 0.7972 0.3369 0.4899 0.033 Uiso 1 1 calc R . . C18 C 0.9736(4) 0.3218(4) 0.5022(4) 0.0350(10) Uani 1 1 d . . . H18 H 0.9997 0.3810 0.5409 0.042 Uiso 1 1 calc R . . C19 C 1.0578(4) 0.2617(6) 0.4767(4) 0.0375(11) Uani 1 1 d . . . H19 H 1.1406 0.2801 0.4982 0.045 Uiso 1 1 calc R . . C20 C 1.0214(4) 0.1774(4) 0.4216(4) 0.0338(10) Uani 1 1 d . . . H20 H 1.0792 0.1375 0.4043 0.041 Uiso 1 1 calc R . . C21 C 0.5672(4) 0.3356(3) 0.1998(3) 0.0213(7) Uani 1 1 d . . . C22 C 0.6862(3) 0.3845(3) 0.2397(3) 0.0222(8) Uani 1 1 d . . . C23 C 0.7844(4) 0.3441(3) 0.2142(3) 0.0241(8) Uani 1 1 d . . . C24 C 0.8940(4) 0.3942(4) 0.2470(4) 0.0319(10) Uani 1 1 d . . . H24 H 0.9612 0.3670 0.2314 0.038 Uiso 1 1 calc R . . C25 C 0.9083(4) 0.4822(4) 0.3017(4) 0.0353(10) Uani 1 1 d . . . C26 C 0.8102(5) 0.5221(4) 0.3237(4) 0.0321(10) Uani 1 1 d . . . H26 H 0.8194 0.5828 0.3609 0.039 Uiso 1 1 calc R . . C27 C 0.6984(5) 0.4752(4) 0.2926(4) 0.0264(10) Uani 1 1 d . . . C28 C 0.7743(3) 0.2497(5) 0.1554(3) 0.0270(7) Uani 1 1 d . . . H28A H 0.7384 0.2632 0.0815 0.040 Uiso 1 1 calc R . . H28B H 0.7229 0.2029 0.1772 0.040 Uiso 1 1 calc R . . H28C H 0.8547 0.2207 0.1686 0.040 Uiso 1 1 calc R . . C29 C 1.0310(5) 0.5328(5) 0.3395(5) 0.0536(16) Uani 1 1 d . . . H29A H 1.0212 0.6008 0.3615 0.080 Uiso 1 1 calc R . . H29B H 1.0664 0.5348 0.2836 0.080 Uiso 1 1 calc R . . H29C H 1.0843 0.4955 0.3979 0.080 Uiso 1 1 calc R . . C30 C 0.5935(4) 0.5266(3) 0.3126(4) 0.0297(9) Uani 1 1 d . . . H30A H 0.5202 0.5161 0.2538 0.045 Uiso 1 1 calc R . . H30B H 0.6102 0.5980 0.3218 0.045 Uiso 1 1 calc R . . H30C H 0.5819 0.4992 0.3751 0.045 Uiso 1 1 calc R . . C31 C 0.4489(4) 0.0648(3) 0.2365(3) 0.0218(8) Uani 1 1 d . . . C32 C 0.3355(4) 0.0084(3) 0.2284(3) 0.0228(8) Uani 1 1 d . . . C33 C 0.2910(4) 0.0064(3) 0.3124(3) 0.0251(8) Uani 1 1 d . . . C34 C 0.1898(4) -0.0514(3) 0.3053(4) 0.0282(9) Uani 1 1 d . . . H34 H 0.1585 -0.0517 0.3613 0.034 Uiso 1 1 calc R . . C35 C 0.1336(4) -0.1082(3) 0.2197(4) 0.0333(10) Uani 1 1 d . . . C36 C 0.1793(5) -0.1045(4) 0.1377(4) 0.0353(10) Uani 1 1 d . . . H36 H 0.1410 -0.1427 0.0778 0.042 Uiso 1 1 calc R . . C37 C 0.2785(4) -0.0472(3) 0.1398(4) 0.0309(9) Uani 1 1 d . . . C38 C 0.3483(4) 0.0643(4) 0.4100(3) 0.0289(9) Uani 1 1 d . . . H38A H 0.2923 0.0677 0.4501 0.043 Uiso 1 1 calc R . . H38B H 0.3669 0.1318 0.3925 0.043 Uiso 1 1 calc R . . H38C H 0.4229 0.0312 0.4508 0.043 Uiso 1 1 calc R . . C39 C 0.0316(5) -0.1741(5) 0.2182(5) 0.0458(13) Uani 1 1 d . . . H39A H 0.0608 -0.2282 0.2680 0.069 Uiso 1 1 calc R . . H39B H -0.0039 -0.2021 0.1489 0.069 Uiso 1 1 calc R . . H39C H -0.0298 -0.1357 0.2366 0.069 Uiso 1 1 calc R . . C40 C 0.3237(6) -0.0481(5) 0.0492(5) 0.0474(14) Uani 1 1 d . . . H40A H 0.2936 -0.1075 0.0075 0.071 Uiso 1 1 calc R . . H40B H 0.4122 -0.0488 0.0735 0.071 Uiso 1 1 calc R . . H40C H 0.2950 0.0115 0.0073 0.071 Uiso 1 1 calc R . . C41 C 0.2752(5) 0.2479(7) -0.1398(3) 0.0456(12) Uani 1 1 d . . . H41A H 0.3282 0.2816 -0.1720 0.068 Uiso 1 1 calc R . . H41B H 0.2175 0.2957 -0.1284 0.068 Uiso 1 1 calc R . . H41C H 0.2312 0.1945 -0.1851 0.068 Uiso 1 1 calc R . . C42 C 0.4407(5) 0.1433(4) -0.0582(4) 0.0347(10) Uani 1 1 d . . . H42A H 0.4034 0.0859 -0.1005 0.052 Uiso 1 1 calc R . . H42B H 0.4950 0.1203 0.0084 0.052 Uiso 1 1 calc R . . H42C H 0.4868 0.1816 -0.0938 0.052 Uiso 1 1 calc R . . C43 C 0.1050(5) 0.1652(5) 0.0503(5) 0.0445(13) Uani 1 1 d . . . H43A H 0.0884 0.1009 0.0768 0.067 Uiso 1 1 calc R . . H43B H 0.1229 0.1549 -0.0143 0.067 Uiso 1 1 calc R . . H43C H 0.0342 0.2084 0.0374 0.067 Uiso 1 1 calc R . . C44 C 0.1847(5) 0.2305(4) 0.2220(4) 0.0403(13) Uani 1 1 d . . . H44A H 0.1180 0.2780 0.2100 0.060 Uiso 1 1 calc R . . H44B H 0.2572 0.2581 0.2725 0.060 Uiso 1 1 calc R . . H44C H 0.1628 0.1681 0.2484 0.060 Uiso 1 1 calc R . . C45 C 0.1709(5) 0.4275(4) 0.0584(4) 0.0374(11) Uani 1 1 d . . . H45A H 0.1894 0.4792 0.1116 0.056 Uiso 1 1 calc R . . H45B H 0.1248 0.3741 0.0772 0.056 Uiso 1 1 calc R . . H45C H 0.1232 0.4562 -0.0079 0.056 Uiso 1 1 calc R . . C46 C 0.3390(5) 0.4642(4) 0.0066(6) 0.0555(18) Uani 1 1 d . . . H46A H 0.2851 0.4828 -0.0619 0.083 Uiso 1 1 calc R . . H46B H 0.4152 0.4390 0.0007 0.083 Uiso 1 1 calc R . . H46C H 0.3551 0.5227 0.0517 0.083 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 Ta1 0.01603(9) 0.02317(9) 0.01937(9) 0.00163(8) 0.00687(5) 0.00202(8) N1 0.0177(15) 0.0233(16) 0.0198(17) 0.0017(12) 0.0072(13) 0.0040(12) N2 0.0200(16) 0.0208(15) 0.0240(17) -0.0017(13) 0.0082(13) 0.0006(12) N3 0.0236(18) 0.0312(17) 0.0208(17) -0.0018(14) 0.0085(14) 0.0028(13) N4 0.0198(17) 0.0324(17) 0.035(2) 0.0067(15) 0.0136(15) 0.0038(13) N5 0.0202(16) 0.0232(16) 0.0271(19) 0.0067(14) 0.0053(14) 0.0044(12) O1 0.0152(13) 0.0320(15) 0.0208(14) 0.0021(11) 0.0057(11) -0.0015(10) O2 0.0251(14) 0.0216(13) 0.0208(14) 0.0029(11) 0.0091(11) 0.0028(10) C1 0.0196(15) 0.023(3) 0.0168(15) -0.0004(15) 0.0072(12) -0.0016(15) C2 0.0169(18) 0.0243(19) 0.020(2) -0.0014(15) 0.0045(15) -0.0010(14) C3 0.029(2) 0.0191(17) 0.028(2) 0.0013(15) 0.0123(17) 0.0039(15) C4 0.029(2) 0.0214(18) 0.031(2) -0.0026(16) 0.0154(18) 0.0032(15) C5 0.026(2) 0.0235(16) 0.024(2) -0.0037(15) 0.0131(16) -0.0058(14) C6 0.0189(17) 0.024(2) 0.0222(18) -0.0029(13) 0.0062(14) -0.0039(12) C7 0.022(2) 0.031(2) 0.028(2) 0.0038(17) 0.0081(17) -0.0002(15) C8 0.030(2) 0.040(2) 0.023(2) 0.0083(18) 0.0077(18) 0.0008(18) C9 0.036(2) 0.035(2) 0.022(2) 0.0021(16) 0.0133(18) -0.0086(17) C10 0.034(2) 0.032(2) 0.024(2) -0.0056(15) 0.0184(18) -0.0090(15) C11 0.0218(19) 0.0196(17) 0.022(2) 0.0031(15) 0.0087(15) 0.0036(14) C12 0.0205(18) 0.0186(17) 0.0188(18) 0.0028(14) 0.0057(15) 0.0024(13) C13 0.032(3) 0.0195(19) 0.029(2) 0.0022(17) 0.014(2) 0.0063(19) C14 0.025(2) 0.035(2) 0.028(2) 0.0075(18) 0.0119(18) 0.0147(17) C15 0.0167(19) 0.033(2) 0.028(2) 0.0095(17) 0.0077(17) 0.0060(15) C16 0.020(2) 0.0281(18) 0.024(2) 0.0062(17) 0.0080(17) 0.0050(15) C17 0.023(2) 0.0301(19) 0.030(2) 0.0028(18) 0.0094(18) -0.0017(16) C18 0.026(2) 0.044(3) 0.030(2) 0.000(2) 0.0026(19) -0.0080(18) C19 0.0192(17) 0.054(3) 0.037(2) 0.012(3) 0.0048(15) -0.005(3) C20 0.018(2) 0.044(3) 0.038(3) 0.014(2) 0.0088(18) 0.0057(18) C21 0.0184(18) 0.0198(18) 0.024(2) 0.0031(14) 0.0045(15) 0.0050(13) C22 0.0186(18) 0.0233(18) 0.024(2) 0.0031(15) 0.0053(15) 0.0003(14) C23 0.0227(19) 0.0263(19) 0.023(2) 0.0079(16) 0.0070(16) 0.0027(15) C24 0.021(2) 0.038(2) 0.038(3) 0.010(2) 0.0106(18) 0.0011(17) C25 0.027(2) 0.032(2) 0.042(3) 0.007(2) 0.004(2) -0.0082(18) C26 0.035(2) 0.028(2) 0.030(2) 0.0012(18) 0.0050(19) -0.0062(19) C27 0.028(3) 0.026(2) 0.023(2) 0.0031(17) 0.0052(19) -0.0010(18) C28 0.0250(16) 0.0311(18) 0.0286(18) -0.003(3) 0.0137(14) 0.002(3) C29 0.038(3) 0.054(3) 0.063(4) 0.005(3) 0.007(3) -0.021(3) C30 0.039(2) 0.0217(19) 0.030(2) 0.0002(16) 0.0129(19) 0.0019(17) C31 0.026(2) 0.0174(16) 0.024(2) -0.0026(14) 0.0109(16) 0.0023(13) C32 0.025(2) 0.0191(17) 0.023(2) -0.0001(14) 0.0065(16) 0.0008(14) C33 0.021(2) 0.026(2) 0.027(2) 0.0011(17) 0.0071(17) 0.0026(15) C34 0.023(2) 0.033(2) 0.031(2) 0.0059(18) 0.0112(18) 0.0015(16) C35 0.024(2) 0.029(2) 0.043(3) 0.0028(19) 0.0062(19) -0.0024(16) C36 0.040(3) 0.032(2) 0.030(2) -0.0047(19) 0.005(2) -0.0093(19) C37 0.030(2) 0.028(2) 0.033(2) -0.0024(17) 0.0075(19) -0.0027(17) C38 0.023(2) 0.044(2) 0.020(2) -0.0032(18) 0.0073(16) -0.0005(17) C39 0.036(3) 0.050(3) 0.050(3) -0.003(3) 0.012(2) -0.012(2) C40 0.060(3) 0.051(3) 0.037(3) -0.021(2) 0.024(3) -0.024(3) C41 0.045(3) 0.059(3) 0.027(2) -0.001(3) 0.0032(18) 0.017(4) C42 0.037(3) 0.043(3) 0.029(2) 0.000(2) 0.018(2) 0.010(2) C43 0.027(3) 0.055(3) 0.051(3) 0.001(3) 0.013(2) -0.010(2) C44 0.033(2) 0.053(4) 0.043(3) 0.006(2) 0.025(2) 0.0046(19) C45 0.034(2) 0.030(2) 0.052(3) 0.008(2) 0.019(2) 0.0096(18) C46 0.035(3) 0.045(3) 0.091(5) 0.039(3) 0.026(3) 0.012(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 N3 1.963(3) . ? Ta1 N4 1.983(3) . ? Ta1 N5 2.017(3) . ? Ta1 O2 2.062(3) . ? Ta1 O1 2.155(3) . ? Ta1 N1 2.291(3) . ? Ta1 C21 2.656(4) . ? N1 C21 1.299(5) . ? N1 C2 1.417(5) . ? N2 C31 1.291(5) . ? N2 C12 1.402(5) . ? N3 C42 1.453(5) . ? N3 C41 1.452(6) . ? N4 C44 1.451(6) . ? N4 C43 1.455(7) . ? N5 C45 1.445(6) . ? N5 C46 1.453(6) . ? O1 C21 1.310(5) . ? O2 C31 1.324(5) . ? C1 C2 1.372(6) . ? C1 C6 1.443(5) . ? C1 C11 1.510(5) . ? C2 C3 1.430(6) . ? C3 C4 1.354(6) . ? C3 H3A 0.9500 . ? C4 C5 1.408(6) . ? C4 H4A 0.9500 . ? C5 C6 1.412(6) . ? C5 C10 1.432(6) . ? C6 C7 1.423(6) . ? C7 C8 1.376(6) . ? C7 H7 0.9500 . ? C8 C9 1.416(7) . ? C8 H8 0.9500 . ? C9 C10 1.360(7) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.376(6) . ? C11 C16 1.442(6) . ? C12 C13 1.422(6) . ? C13 C14 1.373(7) . ? C13 H13 0.9500 . ? C14 C15 1.413(7) . ? C14 H14 0.9500 . ? C15 C16 1.427(6) . ? C15 C20 1.418(6) . ? C16 C17 1.411(6) . ? C17 C18 1.381(6) . ? C17 H17 0.9500 . ? C18 C19 1.401(8) . ? C18 H18 0.9500 . ? C19 C20 1.354(9) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 C22 1.476(5) . ? C22 C27 1.402(6) . ? C22 C23 1.410(5) . ? C23 C24 1.389(6) . ? C23 C28 1.489(7) . ? C24 C25 1.382(7) . ? C24 H24 0.9500 . ? C25 C26 1.385(7) . ? C25 C29 1.520(7) . ? C26 C27 1.389(6) . ? C26 H26 0.9500 . ? C27 C30 1.508(7) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.500(5) . ? C32 C37 1.399(6) . ? C32 C33 1.405(6) . ? C33 C34 1.393(6) . ? C33 C38 1.506(6) . ? C34 C35 1.377(7) . ? C34 H34 0.9500 . ? C35 C36 1.388(7) . ? C35 C39 1.481(7) . ? C36 C37 1.385(7) . ? C36 H36 0.9500 . ? C37 C40 1.495(7) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ta1 N4 108.61(16) . . ? N3 Ta1 N5 95.80(15) . . ? N4 Ta1 N5 89.89(15) . . ? N3 Ta1 O2 90.34(14) . . ? N4 Ta1 O2 93.00(14) . . ? N5 Ta1 O2 172.02(13) . . ? N3 Ta1 O1 85.70(13) . . ? N4 Ta1 O1 165.59(14) . . ? N5 Ta1 O1 86.85(13) . . ? O2 Ta1 O1 88.52(11) . . ? N3 Ta1 N1 142.02(13) . . ? N4 Ta1 N1 107.82(14) . . ? N5 Ta1 N1 94.67(13) . . ? O2 Ta1 N1 77.36(11) . . ? O1 Ta1 N1 58.56(11) . . ? N3 Ta1 C21 113.95(14) . . ? N4 Ta1 C21 137.01(15) . . ? N5 Ta1 C21 91.63(13) . . ? O2 Ta1 C21 81.18(12) . . ? O1 Ta1 C21 29.30(12) . . ? N1 Ta1 C21 29.27(12) . . ? C21 N1 C2 127.4(3) . . ? C21 N1 Ta1 91.2(3) . . ? C2 N1 Ta1 138.7(3) . . ? C31 N2 C12 122.3(4) . . ? C42 N3 C41 108.9(4) . . ? C42 N3 Ta1 121.6(3) . . ? C41 N3 Ta1 127.0(3) . . ? C44 N4 C43 111.4(4) . . ? C44 N4 Ta1 124.5(3) . . ? C43 N4 Ta1 123.9(3) . . ? C45 N5 C46 108.0(4) . . ? C45 N5 Ta1 128.1(3) . . ? C46 N5 Ta1 123.8(3) . . ? C21 O1 Ta1 97.1(2) . . ? C31 O2 Ta1 136.2(2) . . ? C2 C1 C6 118.4(4) . . ? C2 C1 C11 123.9(4) . . ? C6 C1 C11 117.7(4) . . ? C1 C2 N1 124.8(4) . . ? C1 C2 C3 119.9(4) . . ? N1 C2 C3 115.3(4) . . ? C4 C3 C2 122.2(4) . . ? C4 C3 H3A 118.9 . . ? C2 C3 H3A 118.9 . . ? C3 C4 C5 119.5(4) . . ? C3 C4 H4A 120.3 . . ? C5 C4 H4A 120.3 . . ? C4 C5 C6 119.6(4) . . ? C4 C5 C10 120.9(4) . . ? C6 C5 C10 119.5(4) . . ? C5 C6 C7 118.6(4) . . ? C5 C6 C1 120.3(4) . . ? C7 C6 C1 121.2(4) . . ? C8 C7 C6 120.7(4) . . ? C8 C7 H7 119.6 . . ? C6 C7 H7 119.6 . . ? C7 C8 C9 120.3(4) . . ? C7 C8 H8 119.9 . . ? C9 C8 H8 119.9 . . ? C10 C9 C8 120.4(4) . . ? C10 C9 H9 119.8 . . ? C8 C9 H9 119.8 . . ? C9 C10 C5 120.4(4) . . ? C9 C10 H10 119.8 . . ? C5 C10 H10 119.8 . . ? C12 C11 C16 119.1(4) . . ? C12 C11 C1 122.0(4) . . ? C16 C11 C1 118.3(4) . . ? C11 C12 N2 122.9(3) . . ? C11 C12 C13 120.7(4) . . ? N2 C12 C13 115.7(4) . . ? C14 C13 C12 120.7(4) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C13 C14 C15 120.6(4) . . ? C13 C14 H14 119.7 . . ? C15 C14 H14 119.7 . . ? C14 C15 C16 119.0(4) . . ? C14 C15 C20 121.7(4) . . ? C16 C15 C20 119.3(4) . . ? C17 C16 C15 117.8(4) . . ? C17 C16 C11 122.4(4) . . ? C15 C16 C11 119.7(4) . . ? C18 C17 C16 121.1(4) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 120.4(5) . . ? C17 C18 H18 119.8 . . ? C19 C18 H18 119.8 . . ? C20 C19 C18 120.1(4) . . ? C20 C19 H19 119.9 . . ? C18 C19 H19 119.9 . . ? C19 C20 C15 121.2(4) . . ? C19 C20 H20 119.4 . . ? C15 C20 H20 119.4 . . ? N1 C21 O1 113.2(4) . . ? N1 C21 C22 130.0(4) . . ? O1 C21 C22 116.6(4) . . ? N1 C21 Ta1 59.6(2) . . ? O1 C21 Ta1 53.64(19) . . ? C22 C21 Ta1 170.2(3) . . ? C27 C22 C23 120.4(4) . . ? C27 C22 C21 120.5(4) . . ? C23 C22 C21 118.8(4) . . ? C24 C23 C22 118.2(4) . . ? C24 C23 C28 119.6(4) . . ? C22 C23 C28 122.2(4) . . ? C25 C24 C23 122.0(4) . . ? C25 C24 H24 119.0 . . ? C23 C24 H24 119.0 . . ? C26 C25 C24 119.0(4) . . ? C26 C25 C29 120.6(5) . . ? C24 C25 C29 120.4(5) . . ? C25 C26 C27 121.3(5) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C26 C27 C22 119.0(5) . . ? C26 C27 C30 118.4(4) . . ? C22 C27 C30 122.5(4) . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N2 C31 O2 125.2(4) . . ? N2 C31 C32 116.0(4) . . ? O2 C31 C32 118.8(4) . . ? C37 C32 C33 120.0(4) . . ? C37 C32 C31 120.0(4) . . ? C33 C32 C31 119.9(4) . . ? C34 C33 C32 118.8(4) . . ? C34 C33 C38 118.6(4) . . ? C32 C33 C38 122.7(4) . . ? C35 C34 C33 122.2(4) . . ? C35 C34 H34 118.9 . . ? C33 C34 H34 118.9 . . ? C34 C35 C36 117.7(4) . . ? C34 C35 C39 120.5(5) . . ? C36 C35 C39 121.7(5) . . ? C37 C36 C35 122.6(4) . . ? C37 C36 H36 118.7 . . ? C35 C36 H36 118.7 . . ? C36 C37 C32 118.6(4) . . ? C36 C37 C40 119.6(4) . . ? C32 C37 C40 121.7(4) . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C35 C39 H39A 109.5 . . ? C35 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C35 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N3 C41 H41A 109.5 . . ? N3 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N3 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N3 C42 H42A 109.5 . . ? N3 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N3 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N4 C43 H43A 109.5 . . ? N4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N4 C44 H44A 109.5 . . ? N4 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N4 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N5 C45 H45A 109.5 . . ? N5 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N5 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N5 C46 H46A 109.5 . . ? N5 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N5 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Ta1 N1 C21 20.6(3) . . . . ? N4 Ta1 N1 C21 -176.4(2) . . . . ? N5 Ta1 N1 C21 -85.0(2) . . . . ? O2 Ta1 N1 C21 94.5(2) . . . . ? O1 Ta1 N1 C21 -1.6(2) . . . . ? N3 Ta1 N1 C2 -140.1(4) . . . . ? N4 Ta1 N1 C2 22.9(4) . . . . ? N5 Ta1 N1 C2 114.3(4) . . . . ? O2 Ta1 N1 C2 -66.2(4) . . . . ? O1 Ta1 N1 C2 -162.3(4) . . . . ? C21 Ta1 N1 C2 -160.7(5) . . . . ? N4 Ta1 N3 C42 -124.0(4) . . . . ? N5 Ta1 N3 C42 144.2(4) . . . . ? O2 Ta1 N3 C42 -30.7(4) . . . . ? O1 Ta1 N3 C42 57.8(4) . . . . ? N1 Ta1 N3 C42 38.9(5) . . . . ? C21 Ta1 N3 C42 49.8(4) . . . . ? N4 Ta1 N3 C41 76.1(5) . . . . ? N5 Ta1 N3 C41 -15.7(5) . . . . ? O2 Ta1 N3 C41 169.4(5) . . . . ? O1 Ta1 N3 C41 -102.1(5) . . . . ? N1 Ta1 N3 C41 -121.0(4) . . . . ? C21 Ta1 N3 C41 -110.1(4) . . . . ? N3 Ta1 N4 C44 177.9(3) . . . . ? N5 Ta1 N4 C44 -86.1(4) . . . . ? O2 Ta1 N4 C44 86.5(4) . . . . ? O1 Ta1 N4 C44 -9.2(8) . . . . ? N1 Ta1 N4 C44 8.8(4) . . . . ? C21 Ta1 N4 C44 6.2(5) . . . . ? N3 Ta1 N4 C43 -7.1(4) . . . . ? N5 Ta1 N4 C43 89.0(4) . . . . ? O2 Ta1 N4 C43 -98.5(4) . . . . ? O1 Ta1 N4 C43 165.8(5) . . . . ? N1 Ta1 N4 C43 -176.2(4) . . . . ? C21 Ta1 N4 C43 -178.7(3) . . . . ? N3 Ta1 N5 C45 117.3(4) . . . . ? N4 Ta1 N5 C45 8.6(4) . . . . ? O2 Ta1 N5 C45 -102.6(9) . . . . ? O1 Ta1 N5 C45 -157.3(4) . . . . ? N1 Ta1 N5 C45 -99.2(4) . . . . ? C21 Ta1 N5 C45 -128.4(4) . . . . ? N3 Ta1 N5 C46 -66.8(5) . . . . ? N4 Ta1 N5 C46 -175.5(5) . . . . ? O2 Ta1 N5 C46 73.2(11) . . . . ? O1 Ta1 N5 C46 18.6(5) . . . . ? N1 Ta1 N5 C46 76.7(5) . . . . ? C21 Ta1 N5 C46 47.5(5) . . . . ? N3 Ta1 O1 C21 -164.9(2) . . . . ? N4 Ta1 O1 C21 21.8(6) . . . . ? N5 Ta1 O1 C21 99.0(2) . . . . ? O2 Ta1 O1 C21 -74.5(2) . . . . ? N1 Ta1 O1 C21 1.6(2) . . . . ? N3 Ta1 O2 C31 -139.7(4) . . . . ? N4 Ta1 O2 C31 -31.0(4) . . . . ? N5 Ta1 O2 C31 80.1(10) . . . . ? O1 Ta1 O2 C31 134.6(4) . . . . ? N1 Ta1 O2 C31 76.6(4) . . . . ? C21 Ta1 O2 C31 106.1(4) . . . . ? C6 C1 C2 N1 -173.8(4) . . . . ? C11 C1 C2 N1 4.5(7) . . . . ? C6 C1 C2 C3 2.6(6) . . . . ? C11 C1 C2 C3 -179.1(4) . . . . ? C21 N1 C2 C1 -56.8(6) . . . . ? Ta1 N1 C2 C1 98.7(5) . . . . ? C21 N1 C2 C3 126.7(4) . . . . ? Ta1 N1 C2 C3 -77.8(5) . . . . ? C1 C2 C3 C4 1.1(6) . . . . ? N1 C2 C3 C4 177.8(4) . . . . ? C2 C3 C4 C5 -2.4(7) . . . . ? C3 C4 C5 C6 0.0(6) . . . . ? C3 C4 C5 C10 -179.6(4) . . . . ? C4 C5 C6 C7 -177.4(4) . . . . ? C10 C5 C6 C7 2.2(6) . . . . ? C4 C5 C6 C1 3.6(6) . . . . ? C10 C5 C6 C1 -176.8(4) . . . . ? C2 C1 C6 C5 -4.9(6) . . . . ? C11 C1 C6 C5 176.7(4) . . . . ? C2 C1 C6 C7 176.2(4) . . . . ? C11 C1 C6 C7 -2.2(6) . . . . ? C5 C6 C7 C8 -1.0(6) . . . . ? C1 C6 C7 C8 177.9(4) . . . . ? C6 C7 C8 C9 -2.1(7) . . . . ? C7 C8 C9 C10 4.1(7) . . . . ? C8 C9 C10 C5 -3.0(7) . . . . ? C4 C5 C10 C9 179.4(4) . . . . ? C6 C5 C10 C9 -0.2(6) . . . . ? C2 C1 C11 C12 -81.2(6) . . . . ? C6 C1 C11 C12 97.2(5) . . . . ? C2 C1 C11 C16 106.9(5) . . . . ? C6 C1 C11 C16 -74.8(5) . . . . ? C16 C11 C12 N2 167.6(4) . . . . ? C1 C11 C12 N2 -4.3(6) . . . . ? C16 C11 C12 C13 -2.7(6) . . . . ? C1 C11 C12 C13 -174.6(4) . . . . ? C31 N2 C12 C11 87.6(5) . . . . ? C31 N2 C12 C13 -101.6(5) . . . . ? C11 C12 C13 C14 1.0(7) . . . . ? N2 C12 C13 C14 -170.0(4) . . . . ? C12 C13 C14 C15 1.7(7) . . . . ? C13 C14 C15 C16 -2.6(7) . . . . ? C13 C14 C15 C20 177.3(4) . . . . ? C14 C15 C16 C17 178.1(4) . . . . ? C20 C15 C16 C17 -1.8(6) . . . . ? C14 C15 C16 C11 0.8(6) . . . . ? C20 C15 C16 C11 -179.1(4) . . . . ? C12 C11 C16 C17 -175.3(4) . . . . ? C1 C11 C16 C17 -3.1(6) . . . . ? C12 C11 C16 C15 1.8(6) . . . . ? C1 C11 C16 C15 174.0(4) . . . . ? C15 C16 C17 C18 1.4(6) . . . . ? C11 C16 C17 C18 178.6(4) . . . . ? C16 C17 C18 C19 -0.6(7) . . . . ? C17 C18 C19 C20 0.1(8) . . . . ? C18 C19 C20 C15 -0.5(7) . . . . ? C14 C15 C20 C19 -178.5(5) . . . . ? C16 C15 C20 C19 1.4(7) . . . . ? C2 N1 C21 O1 166.5(4) . . . . ? Ta1 N1 C21 O1 2.4(3) . . . . ? C2 N1 C21 C22 -18.2(7) . . . . ? Ta1 N1 C21 C22 177.7(4) . . . . ? C2 N1 C21 Ta1 164.1(4) . . . . ? Ta1 O1 C21 N1 -2.6(3) . . . . ? Ta1 O1 C21 C22 -178.6(3) . . . . ? N3 Ta1 C21 N1 -166.3(2) . . . . ? N4 Ta1 C21 N1 5.1(3) . . . . ? N5 Ta1 C21 N1 96.7(2) . . . . ? O2 Ta1 C21 N1 -79.8(2) . . . . ? O1 Ta1 C21 N1 177.3(4) . . . . ? N3 Ta1 C21 O1 16.5(3) . . . . ? N4 Ta1 C21 O1 -172.2(2) . . . . ? N5 Ta1 C21 O1 -80.6(2) . . . . ? O2 Ta1 C21 O1 102.9(2) . . . . ? N1 Ta1 C21 O1 -177.3(4) . . . . ? N3 Ta1 C21 C22 23.9(17) . . . . ? N4 Ta1 C21 C22 -164.7(16) . . . . ? N5 Ta1 C21 C22 -73.1(16) . . . . ? O2 Ta1 C21 C22 110.4(16) . . . . ? O1 Ta1 C21 C22 7.5(15) . . . . ? N1 Ta1 C21 C22 -169.8(18) . . . . ? N1 C21 C22 C27 -53.6(6) . . . . ? O1 C21 C22 C27 121.6(4) . . . . ? Ta1 C21 C22 C27 114.9(16) . . . . ? N1 C21 C22 C23 133.1(4) . . . . ? O1 C21 C22 C23 -51.7(5) . . . . ? Ta1 C21 C22 C23 -58.4(18) . . . . ? C27 C22 C23 C24 2.9(6) . . . . ? C21 C22 C23 C24 176.2(4) . . . . ? C27 C22 C23 C28 -178.1(4) . . . . ? C21 C22 C23 C28 -4.8(6) . . . . ? C22 C23 C24 C25 -1.1(7) . . . . ? C28 C23 C24 C25 179.9(4) . . . . ? C23 C24 C25 C26 -0.5(7) . . . . ? C23 C24 C25 C29 177.8(5) . . . . ? C24 C25 C26 C27 0.4(8) . . . . ? C29 C25 C26 C27 -178.0(5) . . . . ? C25 C26 C27 C22 1.4(7) . . . . ? C25 C26 C27 C30 -175.7(5) . . . . ? C23 C22 C27 C26 -3.1(7) . . . . ? C21 C22 C27 C26 -176.2(4) . . . . ? C23 C22 C27 C30 173.9(4) . . . . ? C21 C22 C27 C30 0.7(7) . . . . ? C12 N2 C31 O2 1.0(6) . . . . ? C12 N2 C31 C32 177.7(3) . . . . ? Ta1 O2 C31 N2 -122.1(4) . . . . ? Ta1 O2 C31 C32 61.4(5) . . . . ? N2 C31 C32 C37 -124.1(4) . . . . ? O2 C31 C32 C37 52.7(5) . . . . ? N2 C31 C32 C33 51.7(5) . . . . ? O2 C31 C32 C33 -131.5(4) . . . . ? C37 C32 C33 C34 -0.2(6) . . . . ? C31 C32 C33 C34 -176.0(4) . . . . ? C37 C32 C33 C38 179.8(4) . . . . ? C31 C32 C33 C38 4.0(6) . . . . ? C32 C33 C34 C35 1.4(6) . . . . ? C38 C33 C34 C35 -178.6(4) . . . . ? C33 C34 C35 C36 -1.6(7) . . . . ? C33 C34 C35 C39 175.7(5) . . . . ? C34 C35 C36 C37 0.6(7) . . . . ? C39 C35 C36 C37 -176.6(5) . . . . ? C35 C36 C37 C32 0.5(7) . . . . ? C35 C36 C37 C40 179.1(5) . . . . ? C33 C32 C37 C36 -0.7(6) . . . . ? C31 C32 C37 C36 175.1(4) . . . . ? C33 C32 C37 C40 -179.3(5) . . . . ? C31 C32 C37 C40 -3.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.982 _diffrn_reflns_theta_full 27.92 _diffrn_measured_fraction_theta_full 0.982 _refine_diff_density_max 3.342 _refine_diff_density_min -1.805 _refine_diff_density_rms 0.154 # Attachment 'CCDC_775659.cif' data_compound15 _database_code_depnum_ccdc_archive 'CCDC 775659' #TrackingRef 'CCDC_775659.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H60 N5 Nb O2' _chemical_formula_sum 'C46 H60 N5 Nb O2' _chemical_formula_weight 807.90 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -0.1121 2.4826 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.934(2) _cell_length_b 14.079(3) _cell_length_c 13.534(2) _cell_angle_alpha 90.00 _cell_angle_beta 111.011(9) _cell_angle_gamma 90.00 _cell_volume 2122.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 2763 _cell_measurement_theta_min 27.70 _cell_measurement_theta_max 72.00 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.264 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 856 _exptl_absorpt_coefficient_mu 2.633 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5950 _exptl_absorpt_correction_T_max 0.6210 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Rigaku Saturn944 CCD camera' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 21782 _diffrn_reflns_av_R_equivalents 0.0448 _diffrn_reflns_av_sigmaI/netI 0.0543 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.50 _diffrn_reflns_theta_max 72.09 _reflns_number_total 6900 _reflns_number_gt 6542 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r4' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure 4.0' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2009)' _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. One hydronaphthyl ring is disordered in two positions, the c-c bonds distances were restrained to 1.54%A. The thermal parameters of disordered atoms were also restrained. ; _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^)+(0.0666P)^2^+0.7288P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0022(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.001(11) _refine_ls_number_reflns 6900 _refine_ls_number_parameters 513 _refine_ls_number_restraints 47 _refine_ls_R_factor_all 0.0396 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.1236 _refine_ls_wR_factor_gt 0.0997 _refine_ls_goodness_of_fit_ref 1.180 _refine_ls_restrained_S_all 1.180 _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 Nb1 Nb 1.13703(2) 0.98421(3) 0.40776(2) 0.02405(12) Uani 1 1 d . . . N1 N 0.9919(3) 1.0410(3) 0.2564(3) 0.0246(8) Uani 1 1 d . . . N2 N 0.9547(3) 0.7827(3) 0.1792(3) 0.0250(8) Uani 1 1 d . . . N3 N 1.2054(3) 1.1151(3) 0.4551(3) 0.0298(9) Uani 1 1 d . . . N4 N 1.1580(3) 0.9375(3) 0.5507(3) 0.0322(9) Uani 1 1 d . . . N5 N 1.2834(3) 0.9515(3) 0.3761(3) 0.0337(9) Uani 1 1 d . . . O1 O 0.9657(3) 1.0390(3) 0.4079(2) 0.0274(7) Uani 1 1 d . . . O2 O 1.0479(3) 0.8608(2) 0.3387(2) 0.0278(7) Uani 1 1 d . . . C1 C 0.8865(3) 0.9680(3) 0.0788(3) 0.0229(10) Uani 1 1 d . . . C2 C 0.9675(4) 1.0354(3) 0.1459(3) 0.0223(9) Uani 1 1 d . . . C3 C 1.0373(4) 1.0896(4) 0.1056(4) 0.0305(10) Uani 1 1 d . . . H3 H 1.0910 1.1344 0.1509 0.037 Uiso 1 1 calc R . . C4 C 1.0330(5) 1.0818(4) 0.0030(4) 0.0330(11) Uani 1 1 d . . . H4 H 1.0806 1.1218 -0.0226 0.040 Uiso 1 1 calc R . . C5 C 0.9562(4) 1.0128(3) -0.0637(3) 0.0295(10) Uani 1 1 d . . . C6 C 0.8854(4) 0.9566(3) -0.0264(3) 0.0253(10) Uani 1 1 d . . . C7 C 0.8090(4) 0.8799(4) -0.0939(4) 0.0317(10) Uani 1 1 d . . . H7A H 0.7242 0.9010 -0.1202 0.038 Uiso 1 1 calc R . . H7B H 0.8150 0.8226 -0.0498 0.038 Uiso 1 1 calc R . . C8 C 0.8444(5) 0.8533(4) -0.1889(4) 0.0402(12) Uani 1 1 d . . . H8A H 0.9218 0.8188 -0.1641 0.048 Uiso 1 1 calc R . . H8B H 0.7826 0.8112 -0.2375 0.048 Uiso 1 1 calc R . . C9 C 0.8557(6) 0.9423(5) -0.2463(4) 0.0476(14) Uani 1 1 d . . . H9A H 0.8711 0.9253 -0.3113 0.057 Uiso 1 1 calc R . . H9B H 0.7797 0.9787 -0.2674 0.057 Uiso 1 1 calc R . . C10 C 0.9566(5) 1.0019(4) -0.1758(3) 0.0381(13) Uani 1 1 d . . . H10A H 0.9518 1.0657 -0.2078 0.046 Uiso 1 1 calc R . . H10B H 1.0337 0.9729 -0.1719 0.046 Uiso 1 1 calc R . . C11 C 0.8024(4) 0.9095(4) 0.1113(3) 0.0246(9) Uani 1 1 d . . . C12 C 0.8398(4) 0.8223(4) 0.1633(3) 0.0272(10) Uani 1 1 d . . . C13 C 0.7561(6) 0.7649(4) 0.1867(4) 0.0384(13) Uani 1 1 d . . . H13 H 0.7815 0.7066 0.2232 0.046 Uiso 1 1 calc R . . C14 C 0.6368(5) 0.7924(4) 0.1569(4) 0.0399(12) Uani 1 1 d . A . H14 H 0.5820 0.7534 0.1749 0.048 Uiso 1 1 calc R . . C15 C 0.5963(4) 0.8761(4) 0.1013(4) 0.0362(12) Uani 1 1 d D . . C16 C 0.6790(4) 0.9357(3) 0.0776(3) 0.0308(10) Uani 1 1 d D A . C17 C 0.6247(10) 1.0214(14) 0.010(3) 0.033(2) Uani 0.532(6) 1 d PD A 1 H17A H 0.6649 1.0315 -0.0415 0.040 Uiso 0.532(6) 1 calc PR A 1 H17B H 0.6389 1.0783 0.0559 0.040 Uiso 0.532(6) 1 calc PR A 1 C18 C 0.4887(8) 1.0092(8) -0.0497(7) 0.0395(18) Uani 0.532(6) 1 d PDU A 1 H18A H 0.4554 1.0692 -0.0868 0.047 Uiso 0.532(6) 1 calc PR A 1 H18B H 0.4755 0.9590 -0.1039 0.047 Uiso 0.532(6) 1 calc PR A 1 C19 C 0.4213(7) 0.9829(9) 0.0231(7) 0.0411(16) Uani 0.532(6) 1 d PDU A 1 H19A H 0.3339 0.9827 -0.0178 0.049 Uiso 0.532(6) 1 calc PR A 1 H19B H 0.4375 1.0312 0.0798 0.049 Uiso 0.532(6) 1 calc PR A 1 C20 C 0.4602(7) 0.8843(8) 0.0731(11) 0.031(2) Uani 0.532(6) 1 d PDU A 1 H20A H 0.4399 0.8774 0.1376 0.037 Uiso 0.532(6) 1 calc PR A 1 H20B H 0.4182 0.8338 0.0225 0.037 Uiso 0.532(6) 1 calc PR A 1 C17' C 0.6464(13) 1.0286(16) 0.018(3) 0.033(2) Uani 0.468(6) 1 d PD A 2 H17C H 0.6572 1.0210 -0.0504 0.040 Uiso 0.468(6) 1 calc PR A 2 H17D H 0.7045 1.0773 0.0591 0.040 Uiso 0.468(6) 1 calc PR A 2 C18' C 0.5189(9) 1.0672(8) -0.0036(9) 0.0395(18) Uani 0.468(6) 1 d PDU A 2 H18C H 0.5153 1.0991 0.0604 0.047 Uiso 0.468(6) 1 calc PR A 2 H18D H 0.4978 1.1142 -0.0618 0.047 Uiso 0.468(6) 1 calc PR A 2 C19' C 0.4301(8) 0.9840(9) -0.0342(8) 0.0411(16) Uani 0.468(6) 1 d PDU A 2 H19C H 0.3475 1.0069 -0.0478 0.049 Uiso 0.468(6) 1 calc PR A 2 H19D H 0.4320 0.9527 -0.0991 0.049 Uiso 0.468(6) 1 calc PR A 2 C20' C 0.4687(8) 0.9144(10) 0.0587(12) 0.031(2) Uani 0.468(6) 1 d PDU A 2 H20C H 0.4538 0.9457 0.1183 0.037 Uiso 0.468(6) 1 calc PR A 2 H20D H 0.4140 0.8591 0.0378 0.037 Uiso 0.468(6) 1 calc PR A 2 C21 C 0.9213(4) 1.0588(3) 0.3076(3) 0.0229(9) Uani 1 1 d . . . C22 C 0.7983(4) 1.1002(3) 0.2707(3) 0.0255(9) Uani 1 1 d . . . C23 C 0.7074(4) 1.0579(4) 0.3026(4) 0.0303(10) Uani 1 1 d . . . C24 C 0.5996(4) 1.1042(4) 0.2809(4) 0.0394(12) Uani 1 1 d . . . H24 H 0.5387 1.0751 0.3003 0.047 Uiso 1 1 calc R . . C25 C 0.5775(6) 1.1923(5) 0.2314(6) 0.0531(15) Uani 1 1 d . . . C26 C 0.6666(5) 1.2336(5) 0.2016(4) 0.0443(13) Uani 1 1 d . . . H26 H 0.6518 1.2937 0.1674 0.053 Uiso 1 1 calc R . . C27 C 0.7750(4) 1.1902(4) 0.2201(4) 0.0275(10) Uani 1 1 d . . . C28 C 0.7271(4) 0.9625(4) 0.3581(4) 0.0335(12) Uani 1 1 d . . . H28A H 0.7738 0.9714 0.4335 0.050 Uiso 1 1 calc R . . H28B H 0.7709 0.9205 0.3269 0.050 Uiso 1 1 calc R . . H28C H 0.6493 0.9341 0.3497 0.050 Uiso 1 1 calc R . . C29 C 0.4564(7) 1.2426(7) 0.2100(9) 0.090(3) Uani 1 1 d . . . H29A H 0.4702 1.3105 0.2255 0.135 Uiso 1 1 calc R . . H29B H 0.4165 1.2151 0.2553 0.135 Uiso 1 1 calc R . . H29C H 0.4053 1.2342 0.1355 0.135 Uiso 1 1 calc R . . C30 C 0.8683(5) 1.2404(4) 0.1885(4) 0.0331(10) Uani 1 1 d . . . H30A H 0.8697 1.2132 0.1222 0.050 Uiso 1 1 calc R . . H30B H 0.9473 1.2324 0.2442 0.050 Uiso 1 1 calc R . . H30C H 0.8488 1.3081 0.1784 0.050 Uiso 1 1 calc R . . C31 C 1.0464(4) 0.8032(3) 0.2611(3) 0.0277(9) Uani 1 1 d . . . C32 C 1.1603(4) 0.7517(3) 0.2711(3) 0.0257(9) Uani 1 1 d . . . C33 C 1.2031(4) 0.7517(4) 0.1868(3) 0.0295(10) Uani 1 1 d . . . C34 C 1.3074(4) 0.6992(4) 0.1976(4) 0.0339(11) Uani 1 1 d . . . H34 H 1.3370 0.6997 0.1411 0.041 Uiso 1 1 calc R . . C35 C 1.3680(4) 0.6470(4) 0.2876(4) 0.0351(11) Uani 1 1 d . . . C36 C 1.3243(5) 0.6484(4) 0.3699(4) 0.0371(11) Uani 1 1 d . . . H36 H 1.3654 0.6133 0.4325 0.044 Uiso 1 1 calc R . . C37 C 1.2224(4) 0.6995(4) 0.3635(3) 0.0307(10) Uani 1 1 d . . . C38 C 1.1419(4) 0.8055(4) 0.0851(3) 0.0339(11) Uani 1 1 d . . . H38A H 1.0766 0.7668 0.0373 0.051 Uiso 1 1 calc R . . H38B H 1.2002 0.8194 0.0513 0.051 Uiso 1 1 calc R . . H38C H 1.1091 0.8651 0.1006 0.051 Uiso 1 1 calc R . . C39 C 1.4748(5) 0.5882(6) 0.2955(5) 0.0530(17) Uani 1 1 d . . . H39A H 1.4492 0.5329 0.2488 0.079 Uiso 1 1 calc R . . H39B H 1.5144 0.5668 0.3687 0.079 Uiso 1 1 calc R . . H39C H 1.5311 0.6263 0.2743 0.079 Uiso 1 1 calc R . . C40 C 1.1772(5) 0.6926(4) 0.4539(4) 0.0426(13) Uani 1 1 d . . . H40A H 1.2055 0.6332 0.4925 0.064 Uiso 1 1 calc R . . H40B H 1.0892 0.6936 0.4261 0.064 Uiso 1 1 calc R . . H40C H 1.2075 0.7465 0.5019 0.064 Uiso 1 1 calc R . . C41 C 1.1471(6) 1.1860(6) 0.4996(7) 0.071(2) Uani 1 1 d . . . H41A H 1.2043 1.2086 0.5674 0.106 Uiso 1 1 calc R . . H41B H 1.0778 1.1572 0.5107 0.106 Uiso 1 1 calc R . . H41C H 1.1204 1.2395 0.4505 0.106 Uiso 1 1 calc R . . C42 C 1.3056(5) 1.1613(4) 0.4381(4) 0.0412(12) Uani 1 1 d . . . H42A H 1.2752 1.2078 0.3807 0.062 Uiso 1 1 calc R . . H42B H 1.3541 1.1137 0.4189 0.062 Uiso 1 1 calc R . . H42C H 1.3552 1.1938 0.5031 0.062 Uiso 1 1 calc R . . C43 C 1.0677(5) 0.8770(4) 0.5660(4) 0.0361(11) Uani 1 1 d . . . H43A H 1.1068 0.8242 0.6130 0.054 Uiso 1 1 calc R . . H43B H 1.0152 0.8518 0.4976 0.054 Uiso 1 1 calc R . . H43C H 1.0198 0.9139 0.5980 0.054 Uiso 1 1 calc R . . C44 C 1.2333(5) 0.9795(7) 0.6505(3) 0.0555(16) Uani 1 1 d . . . H44A H 1.1825 1.0099 0.6844 0.083 Uiso 1 1 calc R . . H44B H 1.2863 1.0270 0.6374 0.083 Uiso 1 1 calc R . . H44C H 1.2818 0.9298 0.6970 0.083 Uiso 1 1 calc R . . C45 C 1.2957(4) 0.9698(5) 0.2744(4) 0.0430(15) Uani 1 1 d . . . H45A H 1.3500 1.0236 0.2813 0.064 Uiso 1 1 calc R . . H45B H 1.2168 0.9847 0.2214 0.064 Uiso 1 1 calc R . . H45C H 1.3284 0.9133 0.2522 0.064 Uiso 1 1 calc R . . C46 C 1.3910(4) 0.9122(5) 0.4524(4) 0.0441(13) Uani 1 1 d . . . H46A H 1.4118 0.8533 0.4244 0.066 Uiso 1 1 calc R . . H46B H 1.3775 0.8985 0.5183 0.066 Uiso 1 1 calc R . . H46C H 1.4568 0.9579 0.4665 0.066 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 Nb1 0.02146(16) 0.0299(2) 0.02247(16) -0.00384(16) 0.00986(11) -0.00369(17) N1 0.0229(17) 0.034(2) 0.0199(16) 0.0010(15) 0.0111(13) -0.0065(16) N2 0.0260(18) 0.025(2) 0.0264(17) 0.0018(15) 0.0118(14) 0.0008(15) N3 0.0226(17) 0.034(2) 0.0334(19) -0.0061(17) 0.0106(15) -0.0092(16) N4 0.0296(19) 0.036(2) 0.0302(18) -0.0026(17) 0.0100(15) -0.0083(17) N5 0.0276(19) 0.039(2) 0.0357(19) -0.0081(16) 0.0130(15) -0.0042(16) O1 0.0249(14) 0.040(2) 0.0214(13) -0.0061(13) 0.0130(12) 0.0076(14) O2 0.0312(16) 0.0318(18) 0.0225(14) -0.0027(13) 0.0122(12) -0.0035(14) C1 0.0231(17) 0.022(3) 0.0269(17) 0.0009(17) 0.0133(14) 0.0053(17) C2 0.0234(19) 0.022(2) 0.028(2) 0.0000(17) 0.0174(17) 0.0027(17) C3 0.036(2) 0.025(2) 0.037(2) -0.0031(19) 0.021(2) -0.004(2) C4 0.040(3) 0.030(3) 0.042(2) 0.000(2) 0.030(2) 0.004(2) C5 0.042(2) 0.022(3) 0.032(2) 0.0034(16) 0.0224(19) 0.0106(18) C6 0.027(2) 0.028(3) 0.0216(17) 0.0024(15) 0.0102(15) 0.0048(16) C7 0.037(2) 0.032(3) 0.030(2) -0.003(2) 0.0163(19) 0.002(2) C8 0.044(3) 0.047(3) 0.031(2) -0.012(2) 0.014(2) 0.005(2) C9 0.067(4) 0.055(4) 0.025(2) 0.001(2) 0.023(2) 0.017(3) C10 0.059(3) 0.035(4) 0.033(2) 0.005(2) 0.032(2) 0.006(2) C11 0.0217(19) 0.032(2) 0.0215(18) -0.0047(17) 0.0090(15) 0.0023(18) C12 0.029(2) 0.034(3) 0.0186(18) -0.0055(18) 0.0076(16) -0.0041(19) C13 0.050(3) 0.032(3) 0.034(3) -0.003(2) 0.017(2) -0.019(3) C14 0.037(3) 0.042(3) 0.045(3) -0.014(2) 0.019(2) -0.012(2) C15 0.026(2) 0.054(4) 0.028(2) -0.016(2) 0.0088(18) -0.012(2) C16 0.030(2) 0.040(3) 0.0194(19) -0.0058(19) 0.0061(17) 0.001(2) C17 0.025(4) 0.045(4) 0.024(4) -0.007(4) 0.002(5) 0.016(4) C18 0.035(3) 0.042(5) 0.036(3) 0.003(3) 0.006(3) 0.001(3) C19 0.025(2) 0.052(4) 0.052(4) -0.006(5) 0.020(3) -0.001(4) C20 0.019(2) 0.043(6) 0.038(4) 0.001(4) 0.021(2) -0.011(3) C17' 0.025(4) 0.045(4) 0.024(4) -0.007(4) 0.002(5) 0.016(4) C18' 0.035(3) 0.042(5) 0.036(3) 0.003(3) 0.006(3) 0.001(3) C19' 0.025(2) 0.052(4) 0.052(4) -0.006(5) 0.020(3) -0.001(4) C20' 0.019(2) 0.043(6) 0.038(4) 0.001(4) 0.021(2) -0.011(3) C21 0.023(2) 0.026(2) 0.0253(19) -0.0077(17) 0.0154(16) -0.0056(17) C22 0.024(2) 0.029(3) 0.0255(19) -0.0034(17) 0.0114(16) -0.0001(18) C23 0.033(2) 0.030(3) 0.028(2) -0.0039(19) 0.0103(18) -0.007(2) C24 0.024(2) 0.045(3) 0.063(3) -0.004(3) 0.033(2) -0.004(2) C25 0.046(3) 0.046(4) 0.072(4) 0.005(3) 0.027(3) 0.014(3) C26 0.041(3) 0.044(4) 0.047(3) 0.011(3) 0.014(2) 0.011(3) C27 0.027(2) 0.030(3) 0.031(2) -0.0062(19) 0.0167(19) 0.0013(19) C28 0.030(2) 0.038(4) 0.034(2) -0.004(2) 0.0140(17) -0.005(2) C29 0.055(4) 0.082(6) 0.140(8) 0.033(6) 0.043(5) 0.029(4) C30 0.044(3) 0.031(3) 0.034(2) 0.001(2) 0.025(2) -0.006(2) C31 0.035(2) 0.026(2) 0.0216(19) 0.0045(17) 0.0092(17) 0.0001(19) C32 0.027(2) 0.026(2) 0.0253(19) -0.0038(17) 0.0114(17) 0.0039(18) C33 0.032(2) 0.031(3) 0.025(2) 0.0010(18) 0.0095(17) 0.000(2) C34 0.034(2) 0.042(3) 0.026(2) -0.003(2) 0.0113(18) 0.012(2) C35 0.035(2) 0.037(3) 0.034(2) -0.001(2) 0.012(2) 0.004(2) C36 0.045(3) 0.033(3) 0.029(2) 0.004(2) 0.009(2) 0.005(2) C37 0.036(2) 0.033(3) 0.023(2) 0.0027(18) 0.0111(18) 0.006(2) C38 0.033(2) 0.045(3) 0.023(2) 0.005(2) 0.0102(18) 0.004(2) C39 0.044(3) 0.070(5) 0.042(3) 0.002(3) 0.012(2) 0.026(3) C40 0.058(3) 0.043(3) 0.032(2) 0.014(2) 0.023(2) 0.016(3) C41 0.048(3) 0.061(5) 0.120(6) -0.060(5) 0.051(4) -0.016(3) C42 0.050(3) 0.033(3) 0.040(3) 0.000(2) 0.015(2) -0.008(2) C43 0.040(3) 0.044(3) 0.027(2) 0.003(2) 0.0157(19) -0.010(2) C44 0.055(3) 0.082(5) 0.0250(19) -0.011(4) 0.0100(19) -0.025(4) C45 0.035(2) 0.055(5) 0.046(2) -0.013(3) 0.0244(19) -0.002(3) C46 0.018(2) 0.063(4) 0.056(3) -0.002(3) 0.019(2) -0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 N4 1.972(4) . ? Nb1 N5 1.996(4) . ? Nb1 N3 2.024(4) . ? Nb1 O2 2.076(3) . ? Nb1 O1 2.186(3) . ? Nb1 N1 2.301(3) . ? Nb1 C21 2.658(4) . ? N1 C21 1.293(5) . ? N1 C2 1.419(5) . ? N2 C31 1.280(6) . ? N2 C12 1.424(6) . ? N3 C42 1.451(7) . ? N3 C41 1.463(7) . ? N4 C43 1.446(6) . ? N4 C44 1.453(6) . ? N5 C46 1.438(7) . ? N5 C45 1.458(6) . ? O1 C21 1.298(5) . ? O2 C31 1.322(6) . ? C1 C2 1.424(6) . ? C1 C6 1.428(5) . ? C1 C11 1.482(6) . ? C2 C3 1.378(6) . ? C3 C4 1.376(6) . ? C3 H3 0.9500 . ? C4 C5 1.415(7) . ? C4 H4 0.9500 . ? C5 C6 1.379(6) . ? C5 C10 1.526(6) . ? C6 C7 1.495(7) . ? C7 C8 1.538(6) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.505(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.497(8) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.406(7) . ? C11 C16 1.425(6) . ? C12 C13 1.406(7) . ? C13 C14 1.389(9) . ? C13 H13 0.9500 . ? C14 C15 1.388(9) . ? C14 H14 0.9500 . ? C15 C16 1.417(7) . ? C15 C20' 1.522(9) . ? C15 C20 1.535(8) . ? C16 C17' 1.511(9) . ? C16 C17 1.511(9) . ? C17 C18 1.543(10) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C18 C19 1.524(8) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 C20 1.541(9) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C17' C18' 1.540(10) . ? C17' H17C 0.9900 . ? C17' H17D 0.9900 . ? C18' C19' 1.534(9) . ? C18' H18C 0.9900 . ? C18' H18D 0.9900 . ? C19' C20' 1.529(9) . ? C19' H19C 0.9900 . ? C19' H19D 0.9900 . ? C20' H20C 0.9900 . ? C20' H20D 0.9900 . ? C21 C22 1.490(6) . ? C22 C27 1.419(7) . ? C22 C23 1.434(6) . ? C23 C24 1.376(7) . ? C23 C28 1.515(7) . ? C24 C25 1.389(9) . ? C24 H24 0.9500 . ? C25 C26 1.393(9) . ? C25 C29 1.541(9) . ? C26 C27 1.371(7) . ? C26 H26 0.9500 . ? C27 C30 1.505(7) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.503(6) . ? C32 C33 1.407(6) . ? C32 C37 1.409(6) . ? C33 C34 1.409(7) . ? C33 C38 1.511(6) . ? C34 C35 1.384(7) . ? C34 H34 0.9500 . ? C35 C36 1.390(7) . ? C35 C39 1.491(8) . ? C36 C37 1.389(7) . ? C36 H36 0.9500 . ? C37 C40 1.507(7) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Nb1 N5 108.70(17) . . ? N4 Nb1 N3 95.62(17) . . ? N5 Nb1 N3 89.62(16) . . ? N4 Nb1 O2 91.55(15) . . ? N5 Nb1 O2 93.29(15) . . ? N3 Nb1 O2 170.97(14) . . ? N4 Nb1 O1 84.62(14) . . ? N5 Nb1 O1 166.54(15) . . ? N3 Nb1 O1 87.10(15) . . ? O2 Nb1 O1 88.11(13) . . ? N4 Nb1 N1 141.21(14) . . ? N5 Nb1 N1 109.06(14) . . ? N3 Nb1 N1 93.16(15) . . ? O2 Nb1 N1 77.81(13) . . ? O1 Nb1 N1 58.16(11) . . ? N4 Nb1 C21 113.00(15) . . ? N5 Nb1 C21 138.08(14) . . ? N3 Nb1 C21 90.49(15) . . ? O2 Nb1 C21 81.64(13) . . ? O1 Nb1 C21 29.06(11) . . ? N1 Nb1 C21 29.11(12) . . ? C21 N1 C2 130.5(4) . . ? C21 N1 Nb1 90.9(3) . . ? C2 N1 Nb1 136.3(3) . . ? C31 N2 C12 121.3(4) . . ? C42 N3 C41 107.4(5) . . ? C42 N3 Nb1 128.3(3) . . ? C41 N3 Nb1 123.7(3) . . ? C43 N4 C44 110.5(4) . . ? C43 N4 Nb1 119.9(3) . . ? C44 N4 Nb1 126.5(4) . . ? C46 N5 C45 112.3(4) . . ? C46 N5 Nb1 124.0(3) . . ? C45 N5 Nb1 123.6(3) . . ? C21 O1 Nb1 96.1(2) . . ? C31 O2 Nb1 136.9(3) . . ? C2 C1 C6 118.2(4) . . ? C2 C1 C11 123.9(3) . . ? C6 C1 C11 117.9(4) . . ? C3 C2 N1 117.5(4) . . ? C3 C2 C1 119.0(4) . . ? N1 C2 C1 123.0(4) . . ? C4 C3 C2 123.1(5) . . ? C4 C3 H3 118.5 . . ? C2 C3 H3 118.5 . . ? C3 C4 C5 118.7(4) . . ? C3 C4 H4 120.6 . . ? C5 C4 H4 120.6 . . ? C6 C5 C4 120.1(4) . . ? C6 C5 C10 121.8(4) . . ? C4 C5 C10 118.1(4) . . ? C5 C6 C1 120.8(4) . . ? C5 C6 C7 120.7(4) . . ? C1 C6 C7 118.4(4) . . ? C6 C7 C8 113.3(4) . . ? C6 C7 H7A 108.9 . . ? C8 C7 H7A 108.9 . . ? C6 C7 H7B 108.9 . . ? C8 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C9 C8 C7 109.4(4) . . ? C9 C8 H8A 109.8 . . ? C7 C8 H8A 109.8 . . ? C9 C8 H8B 109.8 . . ? C7 C8 H8B 109.8 . . ? H8A C8 H8B 108.2 . . ? C10 C9 C8 109.7(4) . . ? C10 C9 H9A 109.7 . . ? C8 C9 H9A 109.7 . . ? C10 C9 H9B 109.7 . . ? C8 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? C9 C10 C5 113.7(4) . . ? C9 C10 H10A 108.8 . . ? C5 C10 H10A 108.8 . . ? C9 C10 H10B 108.8 . . ? C5 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C12 C11 C16 119.5(4) . . ? C12 C11 C1 120.4(4) . . ? C16 C11 C1 119.6(4) . . ? C11 C12 C13 119.4(5) . . ? C11 C12 N2 122.2(4) . . ? C13 C12 N2 117.7(5) . . ? C14 C13 C12 120.8(6) . . ? C14 C13 H13 119.6 . . ? C12 C13 H13 119.6 . . ? C15 C14 C13 121.0(5) . . ? C15 C14 H14 119.5 . . ? C13 C14 H14 119.5 . . ? C14 C15 C16 119.4(4) . . ? C14 C15 C20' 127.8(6) . . ? C16 C15 C20' 112.9(6) . . ? C14 C15 C20 109.2(6) . . ? C16 C15 C20 131.4(6) . . ? C20' C15 C20 18.5(6) . . ? C15 C16 C11 119.9(4) . . ? C15 C16 C17' 124.4(7) . . ? C11 C16 C17' 115.7(7) . . ? C15 C16 C17 115.2(6) . . ? C11 C16 C17 124.7(7) . . ? C17' C16 C17 10.0(13) . . ? C16 C17 C18 111.8(9) . . ? C16 C17 H17A 109.3 . . ? C18 C17 H17A 109.3 . . ? C16 C17 H17B 109.3 . . ? C18 C17 H17B 109.3 . . ? H17A C17 H17B 107.9 . . ? C19 C18 C17 112.8(12) . . ? C19 C18 H18A 109.0 . . ? C17 C18 H18A 109.0 . . ? C19 C18 H18B 109.0 . . ? C17 C18 H18B 109.0 . . ? H18A C18 H18B 107.8 . . ? C18 C19 C20 110.9(8) . . ? C18 C19 H19A 109.5 . . ? C20 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? C20 C19 H19B 109.5 . . ? H19A C19 H19B 108.0 . . ? C15 C20 C19 107.6(6) . . ? C15 C20 H20A 110.2 . . ? C19 C20 H20A 110.2 . . ? C15 C20 H20B 110.2 . . ? C19 C20 H20B 110.2 . . ? H20A C20 H20B 108.5 . . ? C16 C17' C18' 117.2(12) . . ? C16 C17' H17C 108.0 . . ? C18' C17' H17C 108.0 . . ? C16 C17' H17D 108.0 . . ? C18' C17' H17D 108.0 . . ? H17C C17' H17D 107.2 . . ? C19' C18' C17' 108.8(12) . . ? C19' C18' H18C 109.9 . . ? C17' C18' H18C 109.9 . . ? C19' C18' H18D 109.9 . . ? C17' C18' H18D 109.9 . . ? H18C C18' H18D 108.3 . . ? C20' C19' C18' 107.0(9) . . ? C20' C19' H19C 110.3 . . ? C18' C19' H19C 110.3 . . ? C20' C19' H19D 110.3 . . ? C18' C19' H19D 110.3 . . ? H19C C19' H19D 108.6 . . ? C15 C20' C19' 120.3(9) . . ? C15 C20' H20C 107.3 . . ? C19' C20' H20C 107.3 . . ? C15 C20' H20D 107.3 . . ? C19' C20' H20D 107.3 . . ? H20C C20' H20D 106.9 . . ? N1 C21 O1 114.8(4) . . ? N1 C21 C22 130.4(4) . . ? O1 C21 C22 114.7(3) . . ? N1 C21 Nb1 59.9(2) . . ? O1 C21 Nb1 54.9(2) . . ? C22 C21 Nb1 169.6(3) . . ? C27 C22 C23 118.5(4) . . ? C27 C22 C21 120.7(4) . . ? C23 C22 C21 119.9(4) . . ? C24 C23 C22 119.3(5) . . ? C24 C23 C28 119.5(4) . . ? C22 C23 C28 121.2(4) . . ? C23 C24 C25 121.8(5) . . ? C23 C24 H24 119.1 . . ? C25 C24 H24 119.1 . . ? C24 C25 C26 118.7(5) . . ? C24 C25 C29 120.3(6) . . ? C26 C25 C29 121.0(6) . . ? C27 C26 C25 122.0(6) . . ? C27 C26 H26 119.0 . . ? C25 C26 H26 119.0 . . ? C26 C27 C22 119.7(5) . . ? C26 C27 C30 119.0(5) . . ? C22 C27 C30 121.3(4) . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N2 C31 O2 126.1(4) . . ? N2 C31 C32 115.7(4) . . ? O2 C31 C32 118.0(4) . . ? C33 C32 C37 119.3(4) . . ? C33 C32 C31 120.4(4) . . ? C37 C32 C31 120.2(4) . . ? C32 C33 C34 118.7(4) . . ? C32 C33 C38 122.8(4) . . ? C34 C33 C38 118.5(4) . . ? C35 C34 C33 122.2(4) . . ? C35 C34 H34 118.9 . . ? C33 C34 H34 118.9 . . ? C34 C35 C36 118.0(5) . . ? C34 C35 C39 121.5(5) . . ? C36 C35 C39 120.5(5) . . ? C37 C36 C35 121.9(5) . . ? C37 C36 H36 119.0 . . ? C35 C36 H36 119.0 . . ? C36 C37 C32 119.8(4) . . ? C36 C37 C40 118.4(4) . . ? C32 C37 C40 121.8(4) . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C35 C39 H39A 109.5 . . ? C35 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C35 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N3 C41 H41A 109.5 . . ? N3 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N3 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N3 C42 H42A 109.5 . . ? N3 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N3 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N4 C43 H43A 109.5 . . ? N4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N4 C44 H44A 109.5 . . ? N4 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N4 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N5 C45 H45A 109.5 . . ? N5 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N5 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N5 C46 H46A 109.5 . . ? N5 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N5 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Nb1 N1 C21 17.7(4) . . . . ? N5 Nb1 N1 C21 -176.0(3) . . . . ? N3 Nb1 N1 C21 -85.3(3) . . . . ? O2 Nb1 N1 C21 94.7(3) . . . . ? O1 Nb1 N1 C21 -0.7(3) . . . . ? N4 Nb1 N1 C2 -145.6(4) . . . . ? N5 Nb1 N1 C2 20.7(4) . . . . ? N3 Nb1 N1 C2 111.4(4) . . . . ? O2 Nb1 N1 C2 -68.6(4) . . . . ? O1 Nb1 N1 C2 -164.0(5) . . . . ? C21 Nb1 N1 C2 -163.3(6) . . . . ? N4 Nb1 N3 C42 122.8(4) . . . . ? N5 Nb1 N3 C42 14.0(4) . . . . ? O2 Nb1 N3 C42 -94.8(10) . . . . ? O1 Nb1 N3 C42 -152.9(4) . . . . ? N1 Nb1 N3 C42 -95.0(4) . . . . ? C21 Nb1 N3 C42 -124.0(4) . . . . ? N4 Nb1 N3 C41 -67.4(5) . . . . ? N5 Nb1 N3 C41 -176.2(5) . . . . ? O2 Nb1 N3 C41 75.0(11) . . . . ? O1 Nb1 N3 C41 16.9(5) . . . . ? N1 Nb1 N3 C41 74.8(5) . . . . ? C21 Nb1 N3 C41 45.8(5) . . . . ? N5 Nb1 N4 C43 -126.6(4) . . . . ? N3 Nb1 N4 C43 141.9(4) . . . . ? O2 Nb1 N4 C43 -32.6(4) . . . . ? O1 Nb1 N4 C43 55.3(4) . . . . ? N1 Nb1 N4 C43 39.7(5) . . . . ? C21 Nb1 N4 C43 48.9(4) . . . . ? N5 Nb1 N4 C44 75.2(5) . . . . ? N3 Nb1 N4 C44 -16.3(5) . . . . ? O2 Nb1 N4 C44 169.2(5) . . . . ? O1 Nb1 N4 C44 -102.9(5) . . . . ? N1 Nb1 N4 C44 -118.5(5) . . . . ? C21 Nb1 N4 C44 -109.3(5) . . . . ? N4 Nb1 N5 C46 -7.7(5) . . . . ? N3 Nb1 N5 C46 88.1(4) . . . . ? O2 Nb1 N5 C46 -100.4(4) . . . . ? O1 Nb1 N5 C46 163.9(6) . . . . ? N1 Nb1 N5 C46 -178.7(4) . . . . ? C21 Nb1 N5 C46 178.4(4) . . . . ? N4 Nb1 N5 C45 175.8(4) . . . . ? N3 Nb1 N5 C45 -88.4(4) . . . . ? O2 Nb1 N5 C45 83.0(4) . . . . ? O1 Nb1 N5 C45 -12.6(9) . . . . ? N1 Nb1 N5 C45 4.8(5) . . . . ? C21 Nb1 N5 C45 1.9(5) . . . . ? N4 Nb1 O1 C21 -167.8(3) . . . . ? N5 Nb1 O1 C21 20.1(8) . . . . ? N3 Nb1 O1 C21 96.2(3) . . . . ? O2 Nb1 O1 C21 -76.1(3) . . . . ? N1 Nb1 O1 C21 0.7(3) . . . . ? N4 Nb1 O2 C31 -138.9(4) . . . . ? N5 Nb1 O2 C31 -30.1(4) . . . . ? N3 Nb1 O2 C31 78.5(10) . . . . ? O1 Nb1 O2 C31 136.5(4) . . . . ? N1 Nb1 O2 C31 78.7(4) . . . . ? C21 Nb1 O2 C31 108.0(4) . . . . ? C21 N1 C2 C3 127.2(5) . . . . ? Nb1 N1 C2 C3 -75.0(6) . . . . ? C21 N1 C2 C1 -61.4(7) . . . . ? Nb1 N1 C2 C1 96.4(5) . . . . ? C6 C1 C2 C3 2.8(6) . . . . ? C11 C1 C2 C3 -176.6(4) . . . . ? C6 C1 C2 N1 -168.5(4) . . . . ? C11 C1 C2 N1 12.1(7) . . . . ? N1 C2 C3 C4 171.7(4) . . . . ? C1 C2 C3 C4 -0.1(7) . . . . ? C2 C3 C4 C5 -2.1(8) . . . . ? C3 C4 C5 C6 1.6(7) . . . . ? C3 C4 C5 C10 -177.3(4) . . . . ? C4 C5 C6 C1 1.1(7) . . . . ? C10 C5 C6 C1 179.9(4) . . . . ? C4 C5 C6 C7 -176.6(4) . . . . ? C10 C5 C6 C7 2.2(7) . . . . ? C2 C1 C6 C5 -3.3(6) . . . . ? C11 C1 C6 C5 176.1(4) . . . . ? C2 C1 C6 C7 174.4(4) . . . . ? C11 C1 C6 C7 -6.1(6) . . . . ? C5 C6 C7 C8 16.2(6) . . . . ? C1 C6 C7 C8 -161.5(4) . . . . ? C6 C7 C8 C9 -49.2(6) . . . . ? C7 C8 C9 C10 64.5(6) . . . . ? C8 C9 C10 C5 -46.1(6) . . . . ? C6 C5 C10 C9 13.0(7) . . . . ? C4 C5 C10 C9 -168.1(5) . . . . ? C2 C1 C11 C12 -86.7(5) . . . . ? C6 C1 C11 C12 93.9(5) . . . . ? C2 C1 C11 C16 101.5(5) . . . . ? C6 C1 C11 C16 -77.9(5) . . . . ? C16 C11 C12 C13 -3.7(6) . . . . ? C1 C11 C12 C13 -175.5(4) . . . . ? C16 C11 C12 N2 166.5(4) . . . . ? C1 C11 C12 N2 -5.3(6) . . . . ? C31 N2 C12 C11 88.3(5) . . . . ? C31 N2 C12 C13 -101.3(5) . . . . ? C11 C12 C13 C14 1.4(7) . . . . ? N2 C12 C13 C14 -169.2(4) . . . . ? C12 C13 C14 C15 1.5(8) . . . . ? C13 C14 C15 C16 -2.0(7) . . . . ? C13 C14 C15 C20' 177.1(10) . . . . ? C13 C14 C15 C20 176.2(7) . . . . ? C14 C15 C16 C11 -0.3(7) . . . . ? C20' C15 C16 C11 -179.6(8) . . . . ? C20 C15 C16 C11 -178.1(8) . . . . ? C14 C15 C16 C17' -180(2) . . . . ? C20' C15 C16 C17' 1(2) . . . . ? C20 C15 C16 C17' 3(2) . . . . ? C14 C15 C16 C17 175.8(16) . . . . ? C20' C15 C16 C17 -3.4(18) . . . . ? C20 C15 C16 C17 -2.0(19) . . . . ? C12 C11 C16 C15 3.2(6) . . . . ? C1 C11 C16 C15 175.0(4) . . . . ? C12 C11 C16 C17' -177.5(18) . . . . ? C1 C11 C16 C17' -5.7(19) . . . . ? C12 C11 C16 C17 -172.6(18) . . . . ? C1 C11 C16 C17 -0.7(18) . . . . ? C15 C16 C17 C18 -19(3) . . . . ? C11 C16 C17 C18 156.6(12) . . . . ? C17' C16 C17 C18 -177(19) . . . . ? C16 C17 C18 C19 53(3) . . . . ? C17 C18 C19 C20 -65.1(14) . . . . ? C14 C15 C20 C19 173.6(8) . . . . ? C16 C15 C20 C19 -8.4(14) . . . . ? C20' C15 C20 C19 -4(3) . . . . ? C18 C19 C20 C15 39.6(12) . . . . ? C15 C16 C17' C18' 9(4) . . . . ? C11 C16 C17' C18' -170.4(19) . . . . ? C17 C16 C17' C18' 34(14) . . . . ? C16 C17' C18' C19' -40(3) . . . . ? C17' C18' C19' C20' 59.2(18) . . . . ? C14 C15 C20' C19' -156.2(10) . . . . ? C16 C15 C20' C19' 23.0(16) . . . . ? C20 C15 C20' C19' -154(5) . . . . ? C18' C19' C20' C15 -54.5(17) . . . . ? C2 N1 C21 O1 166.0(4) . . . . ? Nb1 N1 C21 O1 1.1(4) . . . . ? C2 N1 C21 C22 -15.5(8) . . . . ? Nb1 N1 C21 C22 179.7(5) . . . . ? C2 N1 C21 Nb1 164.9(5) . . . . ? Nb1 O1 C21 N1 -1.2(4) . . . . ? Nb1 O1 C21 C22 -180.0(3) . . . . ? N4 Nb1 C21 N1 -168.1(3) . . . . ? N5 Nb1 C21 N1 5.6(4) . . . . ? N3 Nb1 C21 N1 95.6(3) . . . . ? O2 Nb1 C21 N1 -79.9(3) . . . . ? O1 Nb1 C21 N1 178.8(4) . . . . ? N4 Nb1 C21 O1 13.2(3) . . . . ? N5 Nb1 C21 O1 -173.1(3) . . . . ? N3 Nb1 C21 O1 -83.1(3) . . . . ? O2 Nb1 C21 O1 101.3(3) . . . . ? N1 Nb1 C21 O1 -178.8(4) . . . . ? N4 Nb1 C21 C22 13.3(18) . . . . ? N5 Nb1 C21 C22 -172.9(17) . . . . ? N3 Nb1 C21 C22 -83.0(18) . . . . ? O2 Nb1 C21 C22 101.5(18) . . . . ? O1 Nb1 C21 C22 0.2(17) . . . . ? N1 Nb1 C21 C22 -178.6(19) . . . . ? N1 C21 C22 C27 -56.1(7) . . . . ? O1 C21 C22 C27 122.4(5) . . . . ? Nb1 C21 C22 C27 122.3(17) . . . . ? N1 C21 C22 C23 135.0(5) . . . . ? O1 C21 C22 C23 -46.4(6) . . . . ? Nb1 C21 C22 C23 -47(2) . . . . ? C27 C22 C23 C24 1.7(7) . . . . ? C21 C22 C23 C24 170.8(4) . . . . ? C27 C22 C23 C28 -179.3(4) . . . . ? C21 C22 C23 C28 -10.3(6) . . . . ? C22 C23 C24 C25 -1.8(8) . . . . ? C28 C23 C24 C25 179.2(5) . . . . ? C23 C24 C25 C26 1.1(9) . . . . ? C23 C24 C25 C29 -179.1(7) . . . . ? C24 C25 C26 C27 -0.3(10) . . . . ? C29 C25 C26 C27 179.9(7) . . . . ? C25 C26 C27 C22 0.2(9) . . . . ? C25 C26 C27 C30 -178.3(5) . . . . ? C23 C22 C27 C26 -0.9(7) . . . . ? C21 C22 C27 C26 -169.9(4) . . . . ? C23 C22 C27 C30 177.5(4) . . . . ? C21 C22 C27 C30 8.5(6) . . . . ? C12 N2 C31 O2 0.0(7) . . . . ? C12 N2 C31 C32 176.4(4) . . . . ? Nb1 O2 C31 N2 -121.5(5) . . . . ? Nb1 O2 C31 C32 62.2(6) . . . . ? N2 C31 C32 C33 52.2(6) . . . . ? O2 C31 C32 C33 -131.1(4) . . . . ? N2 C31 C32 C37 -125.0(5) . . . . ? O2 C31 C32 C37 51.7(6) . . . . ? C37 C32 C33 C34 -0.1(7) . . . . ? C31 C32 C33 C34 -177.3(5) . . . . ? C37 C32 C33 C38 179.9(5) . . . . ? C31 C32 C33 C38 2.7(7) . . . . ? C32 C33 C34 C35 0.8(8) . . . . ? C38 C33 C34 C35 -179.2(5) . . . . ? C33 C34 C35 C36 -1.0(8) . . . . ? C33 C34 C35 C39 177.1(6) . . . . ? C34 C35 C36 C37 0.5(8) . . . . ? C39 C35 C36 C37 -177.6(6) . . . . ? C35 C36 C37 C32 0.1(8) . . . . ? C35 C36 C37 C40 176.5(5) . . . . ? C33 C32 C37 C36 -0.4(7) . . . . ? C31 C32 C37 C36 176.8(5) . . . . ? C33 C32 C37 C40 -176.6(5) . . . . ? C31 C32 C37 C40 0.6(7) . . . . ? _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 72.09 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 0.865 _refine_diff_density_min -1.011 _refine_diff_density_rms 0.095 # Attachment 'compound-7.cif.txt' data_compound7 _database_code_depnum_ccdc_archive 'CCDC 775660' #TrackingRef 'compound-7.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H60 N5 O2 Ta' _chemical_formula_sum 'C46 H60 N5 O2 Ta' _chemical_formula_weight 895.94 _chemical_absolute_configuration rmad 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' Ta Ta -0.7052 6.5227 '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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.832(2) _cell_length_b 14.325(3) _cell_length_c 13.481(3) _cell_angle_alpha 90.00 _cell_angle_beta 111.28(3) _cell_angle_gamma 90.00 _cell_volume 2129.1(7) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 8198 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.9 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 920 _exptl_absorpt_coefficient_mu 2.624 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4873 _exptl_absorpt_correction_T_max 0.5270 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Rigaku Saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 22072 _diffrn_reflns_av_R_equivalents 0.0529 _diffrn_reflns_av_sigmaI/netI 0.1250 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.62 _diffrn_reflns_theta_max 27.88 _reflns_number_total 9882 _reflns_number_gt 7509 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.8' _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. One hydronaphthyl ring is disordered in two positions, the c-c bonds distances were restrained to 1.54%A. The thermal parameters of disordered atoms were also restrained. The sample crystal was a twinned crystal and one domain was used for refinement and a high residual electron density was observed near H39A. ; _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^)+(0.0155P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0450(7) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.016(7) _refine_ls_number_reflns 9882 _refine_ls_number_parameters 519 _refine_ls_number_restraints 31 _refine_ls_R_factor_all 0.0398 _refine_ls_R_factor_gt 0.0349 _refine_ls_wR_factor_ref 0.0860 _refine_ls_wR_factor_gt 0.0849 _refine_ls_goodness_of_fit_ref 0.936 _refine_ls_restrained_S_all 0.938 _refine_ls_shift/su_max 0.005 _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 Ta1 Ta 0.634157(17) 0.75146(3) 0.908588(16) 0.01958(8) Uani 1 1 d . . . N1 N 0.4911(4) 0.8083(3) 0.7572(4) 0.0176(11) Uani 1 1 d . . . N2 N 0.4505(4) 0.5564(3) 0.6773(4) 0.0202(12) Uani 1 1 d . . . N3 N 0.6565(4) 0.7050(4) 1.0512(4) 0.0241(12) Uani 1 1 d . . . N4 N 0.7016(5) 0.8803(3) 0.9605(4) 0.0208(12) Uani 1 1 d . . . N5 N 0.7786(4) 0.7245(3) 0.8726(4) 0.0246(13) Uani 1 1 d . . . O1 O 0.4621(3) 0.8046(3) 0.9064(3) 0.0208(10) Uani 1 1 d . . . O2 O 0.5447(4) 0.6314(3) 0.8372(3) 0.0224(10) Uani 1 1 d . . . C1 C 0.3854(4) 0.7420(8) 0.5771(4) 0.0185(14) Uani 1 1 d . . . C2 C 0.4671(5) 0.8035(4) 0.6446(5) 0.0193(14) Uani 1 1 d . . . C3 C 0.5406(5) 0.8583(4) 0.6083(5) 0.0249(15) Uani 1 1 d . . . H3 H 0.5961 0.9010 0.6551 0.030 Uiso 1 1 calc R . . C4 C 0.5332(6) 0.8510(4) 0.5038(6) 0.0276(16) Uani 1 1 d . . . H4 H 0.5807 0.8911 0.4785 0.033 Uiso 1 1 calc R . . C5 C 0.4571(5) 0.7857(4) 0.4353(5) 0.0235(14) Uani 1 1 d . . . C6 C 0.3843(5) 0.7304(4) 0.4717(5) 0.0229(18) Uani 1 1 d . . . C7 C 0.3059(6) 0.6540(5) 0.4021(5) 0.0259(15) Uani 1 1 d . . . H7A H 0.3140 0.5969 0.4455 0.031 Uiso 1 1 calc R . . H7B H 0.2200 0.6739 0.3774 0.031 Uiso 1 1 calc R . . C8 C 0.3384(6) 0.6309(5) 0.3063(6) 0.0341(18) Uani 1 1 d . . . H8A H 0.2736 0.5920 0.2560 0.041 Uiso 1 1 calc R . . H8B H 0.4147 0.5946 0.3292 0.041 Uiso 1 1 calc R . . C9 C 0.3539(7) 0.7204(5) 0.2499(5) 0.044(2) Uani 1 1 d . . . H9A H 0.3697 0.7041 0.1848 0.053 Uiso 1 1 calc R . . H9B H 0.2783 0.7577 0.2286 0.053 Uiso 1 1 calc R . . C10 C 0.4572(6) 0.7767(5) 0.3227(5) 0.0370(19) Uani 1 1 d . . . H10A H 0.4539 0.8400 0.2922 0.044 Uiso 1 1 calc R . . H10B H 0.5343 0.7474 0.3261 0.044 Uiso 1 1 calc R . . C11 C 0.2982(5) 0.6824(4) 0.6084(5) 0.0175(13) Uani 1 1 d . . . C12 C 0.3343(5) 0.5976(4) 0.6601(5) 0.0209(14) Uani 1 1 d . . . C13 C 0.2491(7) 0.5423(6) 0.6835(6) 0.028(2) Uani 1 1 d . . . H13 H 0.2737 0.4857 0.7221 0.033 Uiso 1 1 calc R . . C14 C 0.1302(6) 0.5702(5) 0.6505(6) 0.0336(18) Uani 1 1 d . . . H14 H 0.0728 0.5316 0.6652 0.040 Uiso 1 1 calc R . . C15 C 0.0922(6) 0.6526(5) 0.5966(6) 0.0318(17) Uani 1 1 d . A . C16 C 0.1733(6) 0.7066(5) 0.5753(5) 0.0280(16) Uani 1 1 d . A . C17 C 0.1306(6) 0.7991(5) 0.5084(6) 0.0352(19) Uani 1 1 d D . . H17A H 0.1417 0.7906 0.4419 0.042 Uiso 0.555(16) 1 d PR A 1 H17B H 0.1855 0.8476 0.5460 0.042 Uiso 0.555(16) 1 d PR A 1 H17C H 0.1730 0.8084 0.4605 0.042 Uiso 0.445(16) 1 d PR A 2 H17D H 0.1435 0.8523 0.5545 0.042 Uiso 0.445(16) 1 d PR A 2 C20 C -0.0451(7) 0.6752(7) 0.5596(6) 0.057(3) Uani 1 1 d D . . H20A H -0.0639 0.7017 0.6172 0.069 Uiso 0.555(16) 1 d PR A 1 H20B H -0.0918 0.6193 0.5360 0.069 Uiso 0.555(16) 1 d PR A 1 H20C H -0.0692 0.6661 0.6196 0.069 Uiso 0.445(16) 1 d PR A 2 H20D H -0.0885 0.6307 0.5061 0.069 Uiso 0.445(16) 1 d PR A 2 C18 C 0.0060(9) 0.8381(8) 0.4863(13) 0.046(5) Uani 0.555(16) 1 d PDU A 1 H18C H -0.0199 0.8784 0.4222 0.056 Uiso 0.555(16) 1 calc PR A 1 H18D H 0.0029 0.8746 0.5476 0.056 Uiso 0.555(16) 1 calc PR A 1 C19 C -0.0736(10) 0.7494(9) 0.4679(10) 0.037(4) Uani 0.555(16) 1 d PDU A 1 H19C H -0.0692 0.7172 0.4044 0.044 Uiso 0.555(16) 1 calc PR A 1 H19D H -0.1586 0.7699 0.4498 0.044 Uiso 0.555(16) 1 calc PR A 1 C18' C -0.0091(9) 0.7823(13) 0.4480(11) 0.036(5) Uani 0.445(16) 1 d PDU A 2 H18A H -0.0421 0.8351 0.3986 0.043 Uiso 0.445(16) 1 calc PR A 2 H18B H -0.0195 0.7251 0.4044 0.043 Uiso 0.445(16) 1 calc PR A 2 C19' C -0.0853(15) 0.7719(9) 0.5187(15) 0.040(6) Uani 0.445(16) 1 d PDU A 2 H19A H -0.0632 0.8188 0.5767 0.047 Uiso 0.445(16) 1 calc PR A 2 H19B H -0.1734 0.7751 0.4771 0.047 Uiso 0.445(16) 1 calc PR A 2 C21 C 0.4173(5) 0.8256(4) 0.8058(5) 0.0175(13) Uani 1 1 d . . . C22 C 0.2945(5) 0.8698(4) 0.7692(5) 0.0200(13) Uani 1 1 d . . . C23 C 0.2038(6) 0.8284(5) 0.7997(5) 0.0254(15) Uani 1 1 d . . . C24 C 0.0947(6) 0.8753(5) 0.7772(6) 0.0355(18) Uani 1 1 d . . . H24 H 0.0327 0.8473 0.7963 0.043 Uiso 1 1 calc R . . C25 C 0.0735(7) 0.9620(6) 0.7273(7) 0.045(2) Uani 1 1 d . . . C26 C 0.1637(7) 1.0023(5) 0.6987(6) 0.0386(19) Uani 1 1 d . . . H26 H 0.1493 1.0610 0.6636 0.046 Uiso 1 1 calc R . . C27 C 0.2752(7) 0.9582(6) 0.7205(6) 0.026(2) Uani 1 1 d . . . C28 C 0.2198(5) 0.7371(7) 0.8549(5) 0.029(2) Uani 1 1 d . . . H28A H 0.2620 0.6939 0.8237 0.044 Uiso 1 1 calc R . . H28B H 0.1402 0.7114 0.8468 0.044 Uiso 1 1 calc R . . H28C H 0.2678 0.7456 0.9307 0.044 Uiso 1 1 calc R . . C29 C -0.0466(7) 1.0141(7) 0.7016(8) 0.072(3) Uani 1 1 d . . . H29A H -0.0315 1.0815 0.7065 0.108 Uiso 1 1 calc R . . H29B H -0.0843 0.9959 0.7526 0.108 Uiso 1 1 calc R . . H29C H -0.1011 0.9982 0.6293 0.108 Uiso 1 1 calc R . . C30 C 0.3712(6) 1.0059(4) 0.6901(6) 0.0353(18) Uani 1 1 d . . . H30A H 0.4498 1.0003 0.7487 0.053 Uiso 1 1 calc R . . H30B H 0.3506 1.0720 0.6759 0.053 Uiso 1 1 calc R . . H30C H 0.3759 0.9764 0.6261 0.053 Uiso 1 1 calc R . . C31 C 0.5437(5) 0.5748(4) 0.7590(5) 0.0198(13) Uani 1 1 d . . . C32 C 0.6584(5) 0.5237(4) 0.7700(5) 0.0205(14) Uani 1 1 d . . . C33 C 0.7212(6) 0.4762(5) 0.8633(6) 0.0278(16) Uani 1 1 d . . . C34 C 0.8270(6) 0.4250(5) 0.8712(5) 0.0300(16) Uani 1 1 d . . . H34 H 0.8689 0.3914 0.9347 0.036 Uiso 1 1 calc R . . C35 C 0.8702(6) 0.4230(5) 0.7893(6) 0.0325(17) Uani 1 1 d . . . C36 C 0.8052(6) 0.4716(5) 0.6960(5) 0.0274(15) Uani 1 1 d . . . H36 H 0.8338 0.4703 0.6387 0.033 Uiso 1 1 calc R . . C37 C 0.7008(6) 0.5214(4) 0.6838(5) 0.0250(15) Uani 1 1 d . . . C38 C 0.6780(7) 0.4699(5) 0.9570(6) 0.0356(18) Uani 1 1 d . . . H38A H 0.6961 0.5286 0.9971 0.053 Uiso 1 1 calc R . . H38B H 0.7198 0.4184 1.0037 0.053 Uiso 1 1 calc R . . H38C H 0.5903 0.4587 0.9303 0.053 Uiso 1 1 calc R . . C39 C 0.9828(6) 0.3687(5) 0.7982(6) 0.041(2) Uani 1 1 d . . . H39A H 0.9597 0.3064 0.7674 0.061 Uiso 1 1 calc R . . H39B H 1.0350 0.3628 0.8733 0.061 Uiso 1 1 calc R . . H39C H 1.0268 0.4017 0.7596 0.061 Uiso 1 1 calc R . . C40 C 0.6354(6) 0.5715(5) 0.5780(5) 0.0318(17) Uani 1 1 d . . . H40A H 0.6942 0.5885 0.5453 0.048 Uiso 1 1 calc R . . H40B H 0.5963 0.6281 0.5909 0.048 Uiso 1 1 calc R . . H40C H 0.5738 0.5300 0.5300 0.048 Uiso 1 1 calc R . . C41 C 0.5639(6) 0.6447(5) 1.0681(5) 0.0313(17) Uani 1 1 d . . . H41A H 0.6015 0.5859 1.1012 0.047 Uiso 1 1 calc R . . H41B H 0.4994 0.6315 0.9995 0.047 Uiso 1 1 calc R . . H41C H 0.5294 0.6765 1.1149 0.047 Uiso 1 1 calc R . . C42 C 0.7472(6) 0.7353(7) 1.1541(5) 0.043(2) Uani 1 1 d . . . H42A H 0.7062 0.7680 1.1954 0.064 Uiso 1 1 calc R . . H42B H 0.8057 0.7774 1.1412 0.064 Uiso 1 1 calc R . . H42C H 0.7898 0.6806 1.1940 0.064 Uiso 1 1 calc R . . C43 C 0.6495(7) 0.9388(5) 1.0210(7) 0.048(2) Uani 1 1 d . . . H43A H 0.7144 0.9632 1.0840 0.072 Uiso 1 1 calc R . . H43B H 0.5933 0.9017 1.0434 0.072 Uiso 1 1 calc R . . H43C H 0.6056 0.9909 0.9765 0.072 Uiso 1 1 calc R . . C44 C 0.7883(6) 0.9319(5) 0.9290(6) 0.0343(18) Uani 1 1 d . . . H44A H 0.7456 0.9790 0.8760 0.051 Uiso 1 1 calc R . . H44B H 0.8311 0.8889 0.8982 0.051 Uiso 1 1 calc R . . H44C H 0.8469 0.9626 0.9914 0.051 Uiso 1 1 calc R . . C45 C 0.8953(6) 0.6929(6) 0.9538(6) 0.050(2) Uani 1 1 d . . . H45A H 0.9141 0.6299 0.9361 0.074 Uiso 1 1 calc R . . H45B H 0.8883 0.6923 1.0240 0.074 Uiso 1 1 calc R . . H45C H 0.9602 0.7357 0.9547 0.074 Uiso 1 1 calc R . . C46 C 0.7885(5) 0.7360(7) 0.7669(5) 0.034(2) Uani 1 1 d . . . H46A H 0.8364 0.7919 0.7672 0.051 Uiso 1 1 calc R . . H46B H 0.7072 0.7426 0.7124 0.051 Uiso 1 1 calc R . . H46C H 0.8284 0.6811 0.7510 0.051 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 Ta1 0.01882(13) 0.02371(12) 0.01785(13) -0.00268(19) 0.00862(9) -0.00287(18) N1 0.019(3) 0.018(3) 0.019(3) -0.004(2) 0.010(2) -0.008(2) N2 0.021(3) 0.017(3) 0.023(3) 0.004(2) 0.009(3) 0.003(2) N3 0.022(3) 0.033(3) 0.018(3) -0.001(2) 0.008(2) 0.002(2) N4 0.020(3) 0.019(3) 0.021(3) -0.009(2) 0.005(2) -0.006(2) N5 0.017(2) 0.030(3) 0.030(3) -0.010(2) 0.011(2) -0.007(2) O1 0.013(2) 0.038(3) 0.015(2) -0.002(2) 0.0096(18) -0.0006(19) O2 0.028(3) 0.022(2) 0.019(3) -0.005(2) 0.010(2) -0.007(2) C1 0.021(3) 0.021(4) 0.015(3) 0.001(4) 0.009(2) 0.005(4) C2 0.024(3) 0.020(3) 0.016(3) 0.003(3) 0.010(3) 0.006(3) C3 0.024(3) 0.025(3) 0.028(4) -0.003(3) 0.012(3) -0.003(3) C4 0.039(4) 0.018(3) 0.038(4) 0.004(3) 0.030(4) 0.002(3) C5 0.029(3) 0.027(3) 0.017(3) 0.003(3) 0.010(3) 0.013(3) C6 0.023(3) 0.035(5) 0.011(3) 0.004(3) 0.007(2) 0.009(3) C7 0.030(4) 0.030(4) 0.018(4) -0.004(3) 0.008(3) -0.001(3) C8 0.033(4) 0.044(4) 0.026(4) -0.014(4) 0.012(3) -0.002(4) C9 0.050(4) 0.070(7) 0.014(4) -0.002(4) 0.014(3) 0.017(4) C10 0.058(5) 0.036(5) 0.032(4) 0.005(3) 0.034(4) 0.009(3) C11 0.018(3) 0.018(3) 0.014(3) -0.007(3) 0.003(3) -0.006(3) C12 0.020(3) 0.028(3) 0.012(3) -0.002(3) 0.003(3) -0.004(3) C13 0.035(5) 0.022(4) 0.032(5) 0.005(4) 0.019(4) -0.001(3) C14 0.026(4) 0.044(4) 0.038(5) -0.016(4) 0.020(4) -0.019(4) C15 0.020(4) 0.048(5) 0.028(4) -0.011(4) 0.008(3) -0.009(3) C16 0.041(4) 0.026(4) 0.019(4) 0.001(3) 0.013(3) 0.000(3) C17 0.037(4) 0.041(4) 0.018(4) 0.001(3) 0.000(3) 0.023(4) C20 0.029(5) 0.116(9) 0.026(5) -0.015(5) 0.008(4) -0.002(5) C18 0.049(8) 0.042(7) 0.052(8) 0.003(6) 0.023(6) 0.020(6) C19 0.016(5) 0.027(5) 0.051(7) -0.003(8) -0.008(5) 0.009(7) C18' 0.035(8) 0.044(9) 0.035(8) 0.008(6) 0.020(6) 0.020(6) C19' 0.023(7) 0.047(10) 0.047(9) -0.009(7) 0.011(7) 0.012(6) C21 0.023(3) 0.015(3) 0.017(3) -0.003(3) 0.011(3) -0.005(3) C22 0.019(3) 0.025(3) 0.015(3) -0.003(3) 0.005(3) -0.001(3) C23 0.029(4) 0.027(4) 0.022(4) -0.009(3) 0.012(3) -0.003(3) C24 0.022(4) 0.044(4) 0.043(5) -0.010(4) 0.015(4) -0.003(3) C25 0.033(4) 0.049(5) 0.051(6) -0.005(4) 0.013(4) 0.008(4) C26 0.041(5) 0.040(4) 0.038(5) 0.006(4) 0.018(4) 0.010(4) C27 0.026(4) 0.028(4) 0.025(5) -0.011(3) 0.011(4) -0.003(3) C28 0.022(3) 0.043(6) 0.027(3) 0.002(4) 0.013(3) -0.005(4) C29 0.039(5) 0.079(7) 0.104(9) 0.011(7) 0.033(6) 0.024(5) C30 0.056(5) 0.022(3) 0.036(5) 0.003(3) 0.026(4) 0.000(3) C31 0.023(3) 0.020(3) 0.017(3) -0.001(3) 0.008(3) -0.005(3) C32 0.021(3) 0.021(3) 0.016(3) 0.001(3) 0.002(3) -0.004(3) C33 0.033(4) 0.024(3) 0.027(4) 0.001(3) 0.012(3) -0.003(3) C34 0.037(4) 0.028(4) 0.022(4) 0.005(3) 0.007(3) 0.004(3) C35 0.031(4) 0.030(4) 0.033(4) 0.001(3) 0.007(4) 0.008(3) C36 0.030(4) 0.034(4) 0.019(4) -0.001(3) 0.009(3) 0.001(3) C37 0.027(4) 0.026(3) 0.020(4) -0.002(3) 0.005(3) 0.002(3) C38 0.050(5) 0.031(4) 0.030(4) 0.006(3) 0.019(4) 0.003(4) C39 0.034(4) 0.048(5) 0.038(5) -0.007(4) 0.011(4) 0.012(4) C40 0.031(4) 0.043(4) 0.027(4) 0.006(4) 0.017(3) -0.001(4) C41 0.034(4) 0.036(4) 0.025(4) 0.002(3) 0.012(3) -0.011(3) C42 0.047(4) 0.058(7) 0.019(3) -0.004(4) 0.007(3) -0.028(5) C43 0.045(5) 0.035(4) 0.071(6) -0.033(4) 0.030(5) -0.006(4) C44 0.050(5) 0.023(4) 0.036(5) -0.001(3) 0.023(4) -0.010(3) C45 0.036(4) 0.067(6) 0.049(6) 0.005(5) 0.020(4) 0.011(4) C46 0.034(3) 0.043(6) 0.032(4) -0.002(4) 0.022(3) -0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ta1 N3 1.960(5) . ? Ta1 N5 1.977(4) . ? Ta1 N4 2.031(5) . ? Ta1 O2 2.065(4) . ? Ta1 O1 2.163(4) . ? Ta1 N1 2.278(5) . ? Ta1 C21 2.655(6) . ? N1 C21 1.291(7) . ? N1 C2 1.441(7) . ? N2 C31 1.272(8) . ? N2 C12 1.436(7) . ? N3 C41 1.476(7) . ? N3 C42 1.478(7) . ? N4 C44 1.447(7) . ? N4 C43 1.454(7) . ? N5 C46 1.481(7) . ? N5 C45 1.486(8) . ? O1 C21 1.301(7) . ? O2 C31 1.327(7) . ? C1 C2 1.378(9) . ? C1 C6 1.425(7) . ? C1 C11 1.512(10) . ? C2 C3 1.387(8) . ? C3 C4 1.383(8) . ? C3 H3 0.9500 . ? C4 C5 1.390(8) . ? C4 H4 0.9500 . ? C5 C6 1.385(8) . ? C5 C10 1.524(8) . ? C6 C7 1.519(8) . ? C7 C8 1.512(8) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.535(9) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.495(9) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.389(8) . ? C11 C16 1.422(8) . ? C12 C13 1.405(10) . ? C13 C14 1.372(10) . ? C13 H13 0.9500 . ? C14 C15 1.374(10) . ? C14 H14 0.9500 . ? C15 C16 1.343(9) . ? C15 C20 1.551(9) . ? C16 C17 1.579(8) . ? C17 C18 1.502(8) . ? C17 C18' 1.574(9) . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9599 . ? C17 H17D 0.9600 . ? C20 C19' 1.503(9) . ? C20 C19 1.571(9) . ? C20 H20A 0.9600 . ? C20 H20B 0.9599 . ? C20 H20C 0.9599 . ? C20 H20D 0.9600 . ? C18 C19 1.547(9) . ? C18 H17D 1.5648 . ? C18 H18C 0.9900 . ? C18 H18D 0.9900 . ? C19 H19C 0.9900 . ? C19 H19D 0.9900 . ? C18' C19' 1.538(9) . ? C18' H18A 0.9900 . ? C18' H18B 0.9900 . ? C19' H19A 0.9900 . ? C19' H19B 0.9900 . ? C21 C22 1.495(8) . ? C22 C27 1.405(10) . ? C22 C23 1.412(8) . ? C23 C24 1.387(8) . ? C23 C28 1.483(10) . ? C24 C25 1.391(10) . ? C24 H24 0.9500 . ? C25 C26 1.385(10) . ? C25 C29 1.529(10) . ? C26 C27 1.395(10) . ? C26 H26 0.9500 . ? C27 C30 1.505(10) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 C32 1.501(8) . ? C32 C33 1.385(9) . ? C32 C37 1.424(8) . ? C33 C34 1.420(9) . ? C33 C38 1.528(9) . ? C34 C35 1.375(9) . ? C34 H34 0.9500 . ? C35 C36 1.398(9) . ? C35 C39 1.509(9) . ? C36 C37 1.383(8) . ? C36 H36 0.9500 . ? C37 C40 1.532(9) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ta1 N5 110.7(2) . . ? N3 Ta1 N4 94.3(2) . . ? N5 Ta1 N4 89.7(2) . . ? N3 Ta1 O2 92.19(19) . . ? N5 Ta1 O2 93.75(18) . . ? N4 Ta1 O2 171.06(19) . . ? N3 Ta1 O1 85.62(18) . . ? N5 Ta1 O1 163.45(19) . . ? N4 Ta1 O1 86.29(18) . . ? O2 Ta1 O1 88.06(16) . . ? N3 Ta1 N1 142.41(18) . . ? N5 Ta1 N1 106.12(19) . . ? N4 Ta1 N1 93.15(19) . . ? O2 Ta1 N1 77.98(18) . . ? O1 Ta1 N1 58.17(15) . . ? N3 Ta1 C21 114.12(18) . . ? N5 Ta1 C21 135.0(2) . . ? N4 Ta1 C21 90.04(19) . . ? O2 Ta1 C21 81.69(17) . . ? O1 Ta1 C21 29.10(15) . . ? N1 Ta1 C21 29.07(16) . . ? C21 N1 C2 129.2(5) . . ? C21 N1 Ta1 91.9(4) . . ? C2 N1 Ta1 136.5(4) . . ? C31 N2 C12 122.2(5) . . ? C41 N3 C42 110.7(5) . . ? C41 N3 Ta1 120.5(4) . . ? C42 N3 Ta1 127.9(4) . . ? C44 N4 C43 111.1(5) . . ? C44 N4 Ta1 126.5(4) . . ? C43 N4 Ta1 121.6(4) . . ? C46 N5 C45 111.5(5) . . ? C46 N5 Ta1 126.3(4) . . ? C45 N5 Ta1 122.2(4) . . ? C21 O1 Ta1 96.9(3) . . ? C31 O2 Ta1 137.3(4) . . ? C2 C1 C6 118.9(7) . . ? C2 C1 C11 124.2(5) . . ? C6 C1 C11 116.8(7) . . ? C1 C2 C3 120.5(6) . . ? C1 C2 N1 123.3(5) . . ? C3 C2 N1 115.8(5) . . ? C4 C3 C2 120.0(6) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C3 C4 C5 121.0(6) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C6 C5 C4 119.0(6) . . ? C6 C5 C10 122.0(6) . . ? C4 C5 C10 119.0(6) . . ? C5 C6 C1 120.3(7) . . ? C5 C6 C7 120.8(5) . . ? C1 C6 C7 118.9(6) . . ? C8 C7 C6 113.4(5) . . ? C8 C7 H7A 108.9 . . ? C6 C7 H7A 108.9 . . ? C8 C7 H7B 108.9 . . ? C6 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C7 C8 C9 110.7(5) . . ? C7 C8 H8A 109.5 . . ? C9 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? C9 C8 H8B 109.5 . . ? H8A C8 H8B 108.1 . . ? C10 C9 C8 110.0(6) . . ? C10 C9 H9A 109.7 . . ? C8 C9 H9A 109.7 . . ? C10 C9 H9B 109.7 . . ? C8 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? C9 C10 C5 113.8(6) . . ? C9 C10 H10A 108.8 . . ? C5 C10 H10A 108.8 . . ? C9 C10 H10B 108.8 . . ? C5 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C12 C11 C16 117.7(6) . . ? C12 C11 C1 121.2(6) . . ? C16 C11 C1 120.8(6) . . ? C11 C12 C13 119.4(6) . . ? C11 C12 N2 122.9(5) . . ? C13 C12 N2 117.1(6) . . ? C14 C13 C12 119.9(7) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C13 C14 C15 121.4(7) . . ? C13 C14 H14 119.3 . . ? C15 C14 H14 119.3 . . ? C16 C15 C14 119.1(6) . . ? C16 C15 C20 123.9(7) . . ? C14 C15 C20 116.9(6) . . ? C15 C16 C11 122.3(7) . . ? C15 C16 C17 120.0(7) . . ? C11 C16 C17 117.6(6) . . ? C18 C17 C18' 35.2(7) . . ? C18 C17 C16 120.9(8) . . ? C18' C17 C16 103.0(8) . . ? C18 C17 H17A 108.5 . . ? C18' C17 H17A 88.3 . . ? C16 C17 H17A 107.6 . . ? C18 C17 H17B 105.2 . . ? C18' C17 H17B 140.0 . . ? C16 C17 H17B 106.9 . . ? H17A C17 H17B 106.9 . . ? C18 C17 H17C 122.0 . . ? C18' C17 H17C 112.3 . . ? C16 C17 H17C 111.3 . . ? H17A C17 H17C 26.8 . . ? H17B C17 H17C 80.7 . . ? C18 C17 H17D 75.4 . . ? C18' C17 H17D 110.3 . . ? C16 C17 H17D 110.7 . . ? H17A C17 H17D 131.5 . . ? H17B C17 H17D 33.5 . . ? H17C C17 H17D 109.1 . . ? C19' C20 C15 117.7(10) . . ? C19' C20 C19 30.6(7) . . ? C15 C20 C19 107.1(7) . . ? C19' C20 H20A 78.3 . . ? C15 C20 H20A 110.2 . . ? C19 C20 H20A 108.8 . . ? C19' C20 H20B 125.6 . . ? C15 C20 H20B 110.0 . . ? C19 C20 H20B 111.8 . . ? H20A C20 H20B 108.9 . . ? C19' C20 H20C 106.5 . . ? C15 C20 H20C 107.3 . . ? C19 C20 H20C 135.4 . . ? H20A C20 H20C 31.2 . . ? H20B C20 H20C 81.6 . . ? C19' C20 H20D 109.0 . . ? C15 C20 H20D 108.4 . . ? C19 C20 H20D 87.4 . . ? H20A C20 H20D 130.7 . . ? H20B C20 H20D 27.1 . . ? H20C C20 H20D 107.5 . . ? C17 C18 C19 102.9(9) . . ? C17 C18 H17D 36.4 . . ? C19 C18 H17D 130.0 . . ? C17 C18 H18C 111.2 . . ? C19 C18 H18C 111.2 . . ? H17D C18 H18C 111.3 . . ? C17 C18 H18D 111.2 . . ? C19 C18 H18D 111.2 . . ? H17D C18 H18D 77.7 . . ? H18C C18 H18D 109.1 . . ? C18 C19 C20 119.1(10) . . ? C18 C19 H19C 107.6 . . ? C20 C19 H19C 107.6 . . ? C18 C19 H19D 107.6 . . ? C20 C19 H19D 107.6 . . ? H19C C19 H19D 107.0 . . ? C19' C18' C17 115.9(11) . . ? C19' C18' H18A 108.3 . . ? C17 C18' H18A 108.3 . . ? C19' C18' H18B 108.3 . . ? C17 C18' H18B 108.3 . . ? H18A C18' H18B 107.4 . . ? C20 C19' C18' 97.9(11) . . ? C20 C19' H19A 112.2 . . ? C18' C19' H19A 112.2 . . ? C20 C19' H19B 112.2 . . ? C18' C19' H19B 112.2 . . ? H19A C19' H19B 109.8 . . ? N1 C21 O1 113.0(5) . . ? N1 C21 C22 132.0(6) . . ? O1 C21 C22 114.9(5) . . ? N1 C21 Ta1 59.0(3) . . ? O1 C21 Ta1 54.0(3) . . ? C22 C21 Ta1 168.7(4) . . ? C27 C22 C23 120.2(6) . . ? C27 C22 C21 120.6(6) . . ? C23 C22 C21 118.4(6) . . ? C24 C23 C22 118.5(6) . . ? C24 C23 C28 118.4(6) . . ? C22 C23 C28 123.1(6) . . ? C23 C24 C25 121.9(7) . . ? C23 C24 H24 119.0 . . ? C25 C24 H24 119.0 . . ? C26 C25 C24 119.0(7) . . ? C26 C25 C29 118.7(8) . . ? C24 C25 C29 122.4(8) . . ? C25 C26 C27 121.2(7) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C26 C27 C22 119.2(7) . . ? C26 C27 C30 119.1(7) . . ? C22 C27 C30 121.7(7) . . ? C23 C28 H28A 109.5 . . ? C23 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C23 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C25 C29 H29A 109.5 . . ? C25 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C25 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N2 C31 O2 124.7(6) . . ? N2 C31 C32 116.9(6) . . ? O2 C31 C32 118.2(5) . . ? C33 C32 C37 119.9(6) . . ? C33 C32 C31 119.8(6) . . ? C37 C32 C31 120.3(6) . . ? C32 C33 C34 119.3(6) . . ? C32 C33 C38 123.3(6) . . ? C34 C33 C38 117.2(6) . . ? C35 C34 C33 121.7(6) . . ? C35 C34 H34 119.2 . . ? C33 C34 H34 119.2 . . ? C34 C35 C36 117.9(6) . . ? C34 C35 C39 121.5(7) . . ? C36 C35 C39 120.6(7) . . ? C37 C36 C35 122.7(6) . . ? C37 C36 H36 118.6 . . ? C35 C36 H36 118.7 . . ? C36 C37 C32 118.6(6) . . ? C36 C37 C40 118.7(6) . . ? C32 C37 C40 122.7(6) . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C35 C39 H39A 109.5 . . ? C35 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C35 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N3 C41 H41A 109.5 . . ? N3 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N3 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N3 C42 H42A 109.5 . . ? N3 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N3 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N4 C43 H43A 109.5 . . ? N4 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N4 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N4 C44 H44A 109.5 . . ? N4 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N4 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N5 C45 H45A 109.5 . . ? N5 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N5 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N5 C46 H46A 109.5 . . ? N5 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N5 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Ta1 N1 C21 16.8(5) . . . . ? N5 Ta1 N1 C21 -175.0(3) . . . . ? N4 Ta1 N1 C21 -84.4(4) . . . . ? O2 Ta1 N1 C21 94.5(3) . . . . ? O1 Ta1 N1 C21 -0.7(3) . . . . ? N3 Ta1 N1 C2 -145.8(5) . . . . ? N5 Ta1 N1 C2 22.4(6) . . . . ? N4 Ta1 N1 C2 113.0(5) . . . . ? O2 Ta1 N1 C2 -68.0(5) . . . . ? O1 Ta1 N1 C2 -163.3(6) . . . . ? C21 Ta1 N1 C2 -162.6(7) . . . . ? N5 Ta1 N3 C41 -128.4(4) . . . . ? N4 Ta1 N3 C41 140.3(5) . . . . ? O2 Ta1 N3 C41 -33.5(5) . . . . ? O1 Ta1 N3 C41 54.4(5) . . . . ? N1 Ta1 N3 C41 39.5(6) . . . . ? C21 Ta1 N3 C41 48.4(5) . . . . ? N5 Ta1 N3 C42 63.6(6) . . . . ? N4 Ta1 N3 C42 -27.7(6) . . . . ? O2 Ta1 N3 C42 158.5(6) . . . . ? O1 Ta1 N3 C42 -113.6(6) . . . . ? N1 Ta1 N3 C42 -128.5(5) . . . . ? C21 Ta1 N3 C42 -119.6(6) . . . . ? N3 Ta1 N4 C44 134.3(5) . . . . ? N5 Ta1 N4 C44 23.5(5) . . . . ? O2 Ta1 N4 C44 -89.5(12) . . . . ? O1 Ta1 N4 C44 -140.4(5) . . . . ? N1 Ta1 N4 C44 -82.6(5) . . . . ? C21 Ta1 N4 C44 -111.5(5) . . . . ? N3 Ta1 N4 C43 -57.2(6) . . . . ? N5 Ta1 N4 C43 -167.9(6) . . . . ? O2 Ta1 N4 C43 79.1(13) . . . . ? O1 Ta1 N4 C43 28.1(6) . . . . ? N1 Ta1 N4 C43 85.9(6) . . . . ? C21 Ta1 N4 C43 57.0(6) . . . . ? N3 Ta1 N5 C46 170.2(6) . . . . ? N4 Ta1 N5 C46 -95.3(6) . . . . ? O2 Ta1 N5 C46 76.4(6) . . . . ? O1 Ta1 N5 C46 -19.4(10) . . . . ? N1 Ta1 N5 C46 -2.1(6) . . . . ? C21 Ta1 N5 C46 -5.5(7) . . . . ? N3 Ta1 N5 C45 -12.5(5) . . . . ? N4 Ta1 N5 C45 82.0(5) . . . . ? O2 Ta1 N5 C45 -106.3(5) . . . . ? O1 Ta1 N5 C45 157.9(6) . . . . ? N1 Ta1 N5 C45 175.2(5) . . . . ? C21 Ta1 N5 C45 171.8(5) . . . . ? N3 Ta1 O1 C21 -168.7(4) . . . . ? N5 Ta1 O1 C21 20.3(8) . . . . ? N4 Ta1 O1 C21 96.8(4) . . . . ? O2 Ta1 O1 C21 -76.3(4) . . . . ? N1 Ta1 O1 C21 0.7(3) . . . . ? N3 Ta1 O2 C31 -137.9(6) . . . . ? N5 Ta1 O2 C31 -27.0(6) . . . . ? N4 Ta1 O2 C31 85.7(13) . . . . ? O1 Ta1 O2 C31 136.5(6) . . . . ? N1 Ta1 O2 C31 78.7(6) . . . . ? C21 Ta1 O2 C31 108.0(6) . . . . ? C6 C1 C2 C3 4.9(10) . . . . ? C11 C1 C2 C3 -177.4(7) . . . . ? C6 C1 C2 N1 -168.4(6) . . . . ? C11 C1 C2 N1 9.3(11) . . . . ? C21 N1 C2 C1 -59.3(9) . . . . ? Ta1 N1 C2 C1 98.0(7) . . . . ? C21 N1 C2 C3 127.2(6) . . . . ? Ta1 N1 C2 C3 -75.6(7) . . . . ? C1 C2 C3 C4 -0.6(9) . . . . ? N1 C2 C3 C4 173.1(5) . . . . ? C2 C3 C4 C5 -3.3(9) . . . . ? C3 C4 C5 C6 2.8(9) . . . . ? C3 C4 C5 C10 -176.8(6) . . . . ? C4 C5 C6 C1 1.6(9) . . . . ? C10 C5 C6 C1 -178.9(6) . . . . ? C4 C5 C6 C7 -176.1(5) . . . . ? C10 C5 C6 C7 3.5(9) . . . . ? C2 C1 C6 C5 -5.4(10) . . . . ? C11 C1 C6 C5 176.8(6) . . . . ? C2 C1 C6 C7 172.3(6) . . . . ? C11 C1 C6 C7 -5.6(9) . . . . ? C5 C6 C7 C8 13.8(8) . . . . ? C1 C6 C7 C8 -163.8(6) . . . . ? C6 C7 C8 C9 -46.3(8) . . . . ? C7 C8 C9 C10 63.0(7) . . . . ? C8 C9 C10 C5 -45.4(7) . . . . ? C6 C5 C10 C9 13.2(8) . . . . ? C4 C5 C10 C9 -167.2(6) . . . . ? C2 C1 C11 C12 -83.7(10) . . . . ? C6 C1 C11 C12 94.0(8) . . . . ? C2 C1 C11 C16 103.3(8) . . . . ? C6 C1 C11 C16 -78.9(9) . . . . ? C16 C11 C12 C13 -3.9(9) . . . . ? C1 C11 C12 C13 -177.1(6) . . . . ? C16 C11 C12 N2 166.6(6) . . . . ? C1 C11 C12 N2 -6.6(9) . . . . ? C31 N2 C12 C11 88.0(8) . . . . ? C31 N2 C12 C13 -101.3(8) . . . . ? C11 C12 C13 C14 3.3(11) . . . . ? N2 C12 C13 C14 -167.8(6) . . . . ? C12 C13 C14 C15 -1.5(12) . . . . ? C13 C14 C15 C16 0.5(11) . . . . ? C13 C14 C15 C20 177.8(7) . . . . ? C14 C15 C16 C11 -1.3(11) . . . . ? C20 C15 C16 C11 -178.4(6) . . . . ? C14 C15 C16 C17 176.9(6) . . . . ? C20 C15 C16 C17 -0.3(10) . . . . ? C12 C11 C16 C15 3.0(10) . . . . ? C1 C11 C16 C15 176.2(6) . . . . ? C12 C11 C16 C17 -175.2(5) . . . . ? C1 C11 C16 C17 -2.0(9) . . . . ? C15 C16 C17 C18 12.1(11) . . . . ? C11 C16 C17 C18 -169.6(9) . . . . ? C15 C16 C17 C18' -20.8(9) . . . . ? C11 C16 C17 C18' 157.4(7) . . . . ? C16 C15 C20 C19' -13.8(14) . . . . ? C14 C15 C20 C19' 169.0(10) . . . . ? C16 C15 C20 C19 17.4(12) . . . . ? C14 C15 C20 C19 -159.8(9) . . . . ? C18' C17 C18 C19 29.2(10) . . . . ? C16 C17 C18 C19 -37.7(14) . . . . ? C17 C18 C19 C20 59.7(17) . . . . ? C19' C20 C19 C18 65.1(16) . . . . ? C15 C20 C19 C18 -50.7(15) . . . . ? C18 C17 C18' C19' -62.7(14) . . . . ? C16 C17 C18' C19' 63.3(14) . . . . ? C15 C20 C19' C18' 44.5(15) . . . . ? C19 C20 C19' C18' -31.9(10) . . . . ? C17 C18' C19' C20 -74.3(17) . . . . ? C2 N1 C21 O1 165.7(5) . . . . ? Ta1 N1 C21 O1 1.1(5) . . . . ? C2 N1 C21 C22 -18.3(10) . . . . ? Ta1 N1 C21 C22 177.1(6) . . . . ? C2 N1 C21 Ta1 164.5(7) . . . . ? Ta1 O1 C21 N1 -1.2(5) . . . . ? Ta1 O1 C21 C22 -177.9(4) . . . . ? N3 Ta1 C21 N1 -168.9(3) . . . . ? N5 Ta1 C21 N1 6.8(5) . . . . ? N4 Ta1 C21 N1 96.4(4) . . . . ? O2 Ta1 C21 N1 -80.2(3) . . . . ? O1 Ta1 C21 N1 178.7(6) . . . . ? N3 Ta1 C21 O1 12.4(4) . . . . ? N5 Ta1 C21 O1 -171.9(3) . . . . ? N4 Ta1 C21 O1 -82.3(4) . . . . ? O2 Ta1 C21 O1 101.1(4) . . . . ? N1 Ta1 C21 O1 -178.7(6) . . . . ? N3 Ta1 C21 C22 22(2) . . . . ? N5 Ta1 C21 C22 -162(2) . . . . ? N4 Ta1 C21 C22 -73(2) . . . . ? O2 Ta1 C21 C22 111(2) . . . . ? O1 Ta1 C21 C22 10(2) . . . . ? N1 Ta1 C21 C22 -169(2) . . . . ? N1 C21 C22 C27 -53.6(10) . . . . ? O1 C21 C22 C27 122.3(6) . . . . ? Ta1 C21 C22 C27 114(2) . . . . ? N1 C21 C22 C23 136.4(7) . . . . ? O1 C21 C22 C23 -47.6(8) . . . . ? Ta1 C21 C22 C23 -56(2) . . . . ? C27 C22 C23 C24 2.2(9) . . . . ? C21 C22 C23 C24 172.2(6) . . . . ? C27 C22 C23 C28 -177.7(6) . . . . ? C21 C22 C23 C28 -7.7(9) . . . . ? C22 C23 C24 C25 -1.1(11) . . . . ? C28 C23 C24 C25 178.8(7) . . . . ? C23 C24 C25 C26 0.5(12) . . . . ? C23 C24 C25 C29 179.7(7) . . . . ? C24 C25 C26 C27 -1.0(12) . . . . ? C29 C25 C26 C27 179.7(8) . . . . ? C25 C26 C27 C22 2.1(12) . . . . ? C25 C26 C27 C30 -178.5(7) . . . . ? C23 C22 C27 C26 -2.7(10) . . . . ? C21 C22 C27 C26 -172.5(6) . . . . ? C23 C22 C27 C30 178.0(6) . . . . ? C21 C22 C27 C30 8.2(10) . . . . ? C12 N2 C31 O2 1.3(9) . . . . ? C12 N2 C31 C32 177.3(5) . . . . ? Ta1 O2 C31 N2 -121.9(6) . . . . ? Ta1 O2 C31 C32 62.2(8) . . . . ? N2 C31 C32 C33 -127.4(7) . . . . ? O2 C31 C32 C33 48.8(8) . . . . ? N2 C31 C32 C37 50.7(8) . . . . ? O2 C31 C32 C37 -133.1(6) . . . . ? C37 C32 C33 C34 -0.6(10) . . . . ? C31 C32 C33 C34 177.5(6) . . . . ? C37 C32 C33 C38 -176.1(6) . . . . ? C31 C32 C33 C38 2.0(10) . . . . ? C32 C33 C34 C35 1.4(10) . . . . ? C38 C33 C34 C35 177.2(6) . . . . ? C33 C34 C35 C36 -1.3(11) . . . . ? C33 C34 C35 C39 179.8(6) . . . . ? C34 C35 C36 C37 0.5(11) . . . . ? C39 C35 C36 C37 179.3(6) . . . . ? C35 C36 C37 C32 0.4(11) . . . . ? C35 C36 C37 C40 -179.4(6) . . . . ? C33 C32 C37 C36 -0.3(10) . . . . ? C31 C32 C37 C36 -178.4(6) . . . . ? C33 C32 C37 C40 179.5(6) . . . . ? C31 C32 C37 C40 1.4(9) . . . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 4.002 _refine_diff_density_min -1.416 _refine_diff_density_rms 0.131 # Attachment 'compound-8.cif.txt' data_compound8 _database_code_depnum_ccdc_archive 'CCDC 775661' #TrackingRef 'compound-8.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H52 N5 Nb O2' _chemical_formula_sum 'C40 H52 N5 Nb O2' _chemical_formula_weight 727.78 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' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.757(2) _cell_length_b 12.302(3) _cell_length_c 15.936(3) _cell_angle_alpha 98.091(3) _cell_angle_beta 103.416(4) _cell_angle_gamma 90.473(4) _cell_volume 1840.3(6) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 7593 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 31.3 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.313 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 768 _exptl_absorpt_coefficient_mu 0.368 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9104 _exptl_absorpt_correction_T_max 0.9301 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 31741 _diffrn_reflns_av_R_equivalents 0.0402 _diffrn_reflns_av_sigmaI/netI 0.0463 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 27.88 _reflns_number_total 8743 _reflns_number_gt 7881 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.8' _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^)+(0.0419P)^2^+0.0316P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0221(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8743 _refine_ls_number_parameters 448 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0343 _refine_ls_R_factor_gt 0.0309 _refine_ls_wR_factor_ref 0.0827 _refine_ls_wR_factor_gt 0.0814 _refine_ls_goodness_of_fit_ref 1.094 _refine_ls_restrained_S_all 1.094 _refine_ls_shift/su_max 0.003 _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 Nb1 Nb 0.190841(15) 0.993758(12) 0.298012(9) 0.01340(6) Uani 1 1 d . . . O1 O 0.27870(12) 0.86086(9) 0.36827(7) 0.0173(2) Uani 1 1 d . . . O2 O -0.01205(11) 0.94864(9) 0.30195(7) 0.0155(2) Uani 1 1 d . . . N1 N 0.17357(15) 0.81640(11) 0.23103(9) 0.0155(3) Uani 1 1 d . . . N2 N -0.20732(15) 0.83573(11) 0.23203(9) 0.0163(3) Uani 1 1 d . . . N3 N 0.38752(14) 1.01873(12) 0.28557(9) 0.0176(3) Uani 1 1 d . . . N4 N 0.22226(15) 1.08689(11) 0.41182(9) 0.0170(3) Uani 1 1 d . . . N5 N 0.12519(14) 1.07888(11) 0.20129(9) 0.0161(3) Uani 1 1 d . . . C1 C -0.02292(18) 0.68661(13) 0.15244(11) 0.0172(3) Uani 1 1 d . . . C2 C 0.09647(17) 0.75184(13) 0.15396(10) 0.0154(3) Uani 1 1 d . . . C3 C 0.13320(18) 0.76441(14) 0.07595(11) 0.0184(4) Uani 1 1 d . . . H3 H 0.2135 0.8094 0.0772 0.022 Uiso 1 1 calc R . . C4 C 0.05373(19) 0.71198(14) -0.00267(11) 0.0209(4) Uani 1 1 d . . . H4 H 0.0805 0.7196 -0.0553 0.025 Uiso 1 1 calc R . . C5 C -0.06496(19) 0.64823(14) -0.00498(11) 0.0219(4) Uani 1 1 d . . . H5 H -0.1195 0.6124 -0.0594 0.026 Uiso 1 1 calc R . . C6 C -0.10532(18) 0.63596(14) 0.07133(11) 0.0198(4) Uani 1 1 d . . . C7 C -0.2402(2) 0.57147(16) 0.06501(13) 0.0287(4) Uani 1 1 d . . . H7A H -0.2227 0.5181 0.1061 0.043 Uiso 1 1 calc R . . H7B H -0.2740 0.5326 0.0055 0.043 Uiso 1 1 calc R . . H7C H -0.3116 0.6218 0.0793 0.043 Uiso 1 1 calc R . . C8 C -0.06887(17) 0.66804(13) 0.23341(11) 0.0163(3) Uani 1 1 d . . . C9 C -0.15447(17) 0.74369(13) 0.27033(10) 0.0158(3) Uani 1 1 d . . . C10 C -0.20780(18) 0.71724(14) 0.33989(11) 0.0202(4) Uani 1 1 d . . . H10 H -0.2651 0.7675 0.3655 0.024 Uiso 1 1 calc R . . C11 C -0.1781(2) 0.61932(15) 0.37154(12) 0.0240(4) Uani 1 1 d . . . H11 H -0.2140 0.6030 0.4191 0.029 Uiso 1 1 calc R . . C12 C -0.0964(2) 0.54483(14) 0.33430(12) 0.0242(4) Uani 1 1 d . . . H12 H -0.0774 0.4771 0.3560 0.029 Uiso 1 1 calc R . . C13 C -0.04147(19) 0.56805(14) 0.26497(11) 0.0203(4) Uani 1 1 d . . . C14 C 0.0405(2) 0.48155(14) 0.22335(12) 0.0263(4) Uani 1 1 d . . . H14A H 0.0803 0.4326 0.2655 0.039 Uiso 1 1 calc R . . H14B H 0.1170 0.5171 0.2053 0.039 Uiso 1 1 calc R . . H14C H -0.0225 0.4387 0.1722 0.039 Uiso 1 1 calc R . . C15 C 0.24794(17) 0.78389(13) 0.30219(11) 0.0161(3) Uani 1 1 d . . . C16 C 0.30985(18) 0.67503(14) 0.31283(11) 0.0172(3) Uani 1 1 d . . . C17 C 0.29292(18) 0.62432(14) 0.38370(11) 0.0201(4) Uani 1 1 d . . . C18 C 0.35969(19) 0.52625(14) 0.39638(12) 0.0224(4) Uani 1 1 d . . . H18 H 0.3466 0.4901 0.4430 0.027 Uiso 1 1 calc R . . C19 C 0.44442(19) 0.47951(14) 0.34361(12) 0.0231(4) Uani 1 1 d . . . C20 C 0.46232(19) 0.53334(15) 0.27590(12) 0.0231(4) Uani 1 1 d . . . H20 H 0.5209 0.5026 0.2395 0.028 Uiso 1 1 calc R . . C21 C 0.39749(18) 0.63086(14) 0.25954(11) 0.0202(4) Uani 1 1 d . . . C22 C 0.2099(2) 0.67503(15) 0.44693(12) 0.0243(4) Uani 1 1 d . . . H22A H 0.2682 0.7328 0.4890 0.036 Uiso 1 1 calc R . . H22B H 0.1821 0.6184 0.4780 0.036 Uiso 1 1 calc R . . H22C H 0.1253 0.7069 0.4149 0.036 Uiso 1 1 calc R . . C23 C 0.5199(2) 0.37525(15) 0.35970(14) 0.0307(5) Uani 1 1 d . . . H23A H 0.5184 0.3596 0.4181 0.046 Uiso 1 1 calc R . . H23B H 0.6178 0.3842 0.3554 0.046 Uiso 1 1 calc R . . H23C H 0.4725 0.3142 0.3160 0.046 Uiso 1 1 calc R . . C24 C 0.4336(2) 0.68746(16) 0.18869(12) 0.0274(4) Uani 1 1 d . . . H24A H 0.5321 0.6753 0.1869 0.041 Uiso 1 1 calc R . . H24B H 0.4204 0.7665 0.2010 0.041 Uiso 1 1 calc R . . H24C H 0.3718 0.6573 0.1323 0.041 Uiso 1 1 calc R . . C25 C -0.13732(17) 0.92805(13) 0.24791(10) 0.0148(3) Uani 1 1 d . . . C26 C -0.20393(16) 1.02124(13) 0.20361(10) 0.0149(3) Uani 1 1 d . . . C27 C -0.27538(17) 1.00265(14) 0.11472(11) 0.0167(3) Uani 1 1 d . . . C28 C -0.33520(18) 1.09018(15) 0.07508(11) 0.0196(4) Uani 1 1 d . . . H28 H -0.3826 1.0770 0.0151 0.023 Uiso 1 1 calc R . . C29 C -0.32834(18) 1.19639(14) 0.11980(12) 0.0201(4) Uani 1 1 d . . . C30 C -0.25705(18) 1.21314(14) 0.20696(12) 0.0201(4) Uani 1 1 d . . . H30 H -0.2495 1.2853 0.2384 0.024 Uiso 1 1 calc R . . C31 C -0.19618(17) 1.12837(14) 0.25008(11) 0.0167(3) Uani 1 1 d . . . C32 C -0.28956(19) 0.89106(14) 0.05947(11) 0.0219(4) Uani 1 1 d . . . H32A H -0.3547 0.8433 0.0777 0.033 Uiso 1 1 calc R . . H32B H -0.1970 0.8585 0.0668 0.033 Uiso 1 1 calc R . . H32C H -0.3263 0.8989 -0.0020 0.033 Uiso 1 1 calc R . . C33 C -0.3996(2) 1.28902(15) 0.07655(13) 0.0293(4) Uani 1 1 d . . . H33A H -0.5010 1.2839 0.0737 0.044 Uiso 1 1 calc R . . H33B H -0.3849 1.2839 0.0174 0.044 Uiso 1 1 calc R . . H33C H -0.3595 1.3595 0.1104 0.044 Uiso 1 1 calc R . . C34 C -0.12834(18) 1.15593(14) 0.34595(11) 0.0216(4) Uani 1 1 d . . . H34A H -0.0263 1.1673 0.3541 0.032 Uiso 1 1 calc R . . H34B H -0.1472 1.0953 0.3761 0.032 Uiso 1 1 calc R . . H34C H -0.1674 1.2232 0.3701 0.032 Uiso 1 1 calc R . . C35 C 0.51403(19) 1.00115(17) 0.35245(13) 0.0290(4) Uani 1 1 d . . . H35A H 0.5585 0.9344 0.3325 0.043 Uiso 1 1 calc R . . H35B H 0.4871 0.9930 0.4069 0.043 Uiso 1 1 calc R . . H35C H 0.5807 1.0643 0.3626 0.043 Uiso 1 1 calc R . . C36 C 0.43180(19) 1.03689(17) 0.20673(12) 0.0278(4) Uani 1 1 d . . . H36A H 0.4924 1.1039 0.2192 0.042 Uiso 1 1 calc R . . H36B H 0.3485 1.0448 0.1603 0.042 Uiso 1 1 calc R . . H36C H 0.4842 0.9741 0.1879 0.042 Uiso 1 1 calc R . . C37 C 0.16168(19) 1.05173(15) 0.47991(11) 0.0226(4) Uani 1 1 d . . . H37A H 0.2376 1.0339 0.5275 0.034 Uiso 1 1 calc R . . H37B H 0.0992 0.9866 0.4555 0.034 Uiso 1 1 calc R . . H37C H 0.1077 1.1111 0.5024 0.034 Uiso 1 1 calc R . . C38 C 0.3224(2) 1.18017(16) 0.44681(12) 0.0285(4) Uani 1 1 d . . . H38A H 0.2718 1.2449 0.4640 0.043 Uiso 1 1 calc R . . H38B H 0.3710 1.1955 0.4021 0.043 Uiso 1 1 calc R . . H38C H 0.3917 1.1627 0.4978 0.043 Uiso 1 1 calc R . . C39 C 0.1532(2) 1.19713(15) 0.21245(13) 0.0328(5) Uani 1 1 d . . . H39A H 0.2105 1.2139 0.1725 0.049 Uiso 1 1 calc R . . H39B H 0.2042 1.2229 0.2727 0.049 Uiso 1 1 calc R . . H39C H 0.0637 1.2341 0.1996 0.049 Uiso 1 1 calc R . . C40 C 0.05799(18) 1.03664(15) 0.11075(11) 0.0199(4) Uani 1 1 d . . . H40A H -0.0260 1.0781 0.0914 0.030 Uiso 1 1 calc R . . H40B H 0.0305 0.9588 0.1059 0.030 Uiso 1 1 calc R . . H40C H 0.1243 1.0446 0.0741 0.030 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 Nb1 0.01237(9) 0.01495(9) 0.01324(8) 0.00256(6) 0.00348(6) 0.00012(6) O1 0.0196(6) 0.0170(6) 0.0150(6) 0.0027(5) 0.0033(5) 0.0020(5) O2 0.0100(6) 0.0174(6) 0.0183(6) 0.0024(5) 0.0023(5) -0.0008(5) N1 0.0172(7) 0.0152(7) 0.0147(7) 0.0017(5) 0.0057(6) 0.0019(6) N2 0.0165(7) 0.0164(7) 0.0165(7) 0.0010(6) 0.0058(6) -0.0007(6) N3 0.0126(7) 0.0249(8) 0.0161(7) 0.0058(6) 0.0033(6) 0.0000(6) N4 0.0178(7) 0.0189(7) 0.0147(7) 0.0019(6) 0.0048(6) -0.0009(6) N5 0.0151(7) 0.0175(7) 0.0161(7) 0.0043(6) 0.0031(6) -0.0011(6) C1 0.0211(9) 0.0149(8) 0.0173(8) 0.0016(6) 0.0084(7) 0.0043(7) C2 0.0170(8) 0.0140(8) 0.0152(8) 0.0016(6) 0.0041(7) 0.0047(6) C3 0.0199(9) 0.0190(8) 0.0188(8) 0.0035(7) 0.0092(7) 0.0033(7) C4 0.0275(10) 0.0212(9) 0.0157(8) 0.0018(7) 0.0093(7) 0.0051(8) C5 0.0270(10) 0.0216(9) 0.0151(8) -0.0027(7) 0.0042(7) 0.0029(8) C6 0.0228(9) 0.0167(8) 0.0194(8) -0.0013(7) 0.0062(7) 0.0010(7) C7 0.0289(11) 0.0290(10) 0.0256(10) -0.0028(8) 0.0053(8) -0.0078(8) C8 0.0177(9) 0.0153(8) 0.0159(8) 0.0004(6) 0.0051(7) -0.0019(7) C9 0.0156(8) 0.0147(8) 0.0157(8) -0.0021(6) 0.0034(7) -0.0046(6) C10 0.0220(9) 0.0197(8) 0.0202(9) -0.0006(7) 0.0097(7) -0.0012(7) C11 0.0298(10) 0.0249(9) 0.0202(9) 0.0050(7) 0.0110(8) -0.0044(8) C12 0.0338(11) 0.0162(8) 0.0245(9) 0.0056(7) 0.0090(8) -0.0021(8) C13 0.0249(10) 0.0157(8) 0.0201(9) -0.0012(7) 0.0070(8) -0.0009(7) C14 0.0369(11) 0.0161(9) 0.0273(10) 0.0020(7) 0.0111(9) 0.0056(8) C15 0.0156(8) 0.0174(8) 0.0172(8) 0.0030(6) 0.0073(7) 0.0010(7) C16 0.0168(8) 0.0171(8) 0.0177(8) 0.0026(7) 0.0036(7) 0.0021(7) C17 0.0201(9) 0.0209(9) 0.0203(9) 0.0046(7) 0.0056(7) 0.0030(7) C18 0.0241(10) 0.0209(9) 0.0243(9) 0.0084(7) 0.0070(8) 0.0023(7) C19 0.0210(9) 0.0178(9) 0.0297(10) 0.0035(7) 0.0042(8) 0.0031(7) C20 0.0206(9) 0.0233(9) 0.0261(9) -0.0001(7) 0.0087(8) 0.0054(7) C21 0.0189(9) 0.0214(9) 0.0203(8) 0.0023(7) 0.0052(7) 0.0011(7) C22 0.0284(10) 0.0269(9) 0.0219(9) 0.0083(8) 0.0116(8) 0.0077(8) C23 0.0329(11) 0.0207(9) 0.0410(12) 0.0076(9) 0.0114(9) 0.0074(8) C24 0.0263(10) 0.0335(11) 0.0287(10) 0.0103(8) 0.0151(8) 0.0102(8) C25 0.0144(8) 0.0172(8) 0.0144(8) -0.0004(6) 0.0080(7) 0.0010(6) C26 0.0101(8) 0.0173(8) 0.0185(8) 0.0031(7) 0.0053(7) -0.0013(6) C27 0.0126(8) 0.0189(8) 0.0195(8) 0.0022(7) 0.0059(7) -0.0013(7) C28 0.0142(8) 0.0258(9) 0.0198(8) 0.0064(7) 0.0043(7) 0.0002(7) C29 0.0137(8) 0.0212(9) 0.0282(9) 0.0090(7) 0.0075(7) 0.0007(7) C30 0.0174(9) 0.0165(8) 0.0279(9) 0.0023(7) 0.0088(8) 0.0001(7) C31 0.0120(8) 0.0179(8) 0.0215(8) 0.0022(7) 0.0072(7) 0.0001(6) C32 0.0234(10) 0.0240(9) 0.0165(8) 0.0009(7) 0.0026(7) 0.0013(8) C33 0.0305(11) 0.0236(10) 0.0357(11) 0.0112(8) 0.0074(9) 0.0029(8) C34 0.0226(9) 0.0201(9) 0.0212(9) -0.0023(7) 0.0061(8) 0.0031(7) C35 0.0156(9) 0.0438(12) 0.0277(10) 0.0119(9) 0.0015(8) -0.0003(8) C36 0.0169(9) 0.0449(12) 0.0246(10) 0.0098(9) 0.0081(8) -0.0028(9) C37 0.0217(9) 0.0313(10) 0.0146(8) 0.0027(7) 0.0042(7) -0.0038(8) C38 0.0341(11) 0.0281(10) 0.0230(9) -0.0019(8) 0.0094(9) -0.0101(9) C39 0.0414(12) 0.0210(10) 0.0294(10) 0.0084(8) -0.0074(9) -0.0035(9) C40 0.0188(9) 0.0250(9) 0.0167(8) 0.0050(7) 0.0044(7) 0.0015(7) _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 Nb1 N4 1.9614(14) . ? Nb1 N5 1.9723(14) . ? Nb1 N3 2.0000(14) . ? Nb1 O2 2.0688(12) . ? Nb1 O1 2.1804(12) . ? Nb1 N1 2.2766(14) . ? Nb1 C15 2.6524(17) . ? O1 C15 1.2898(19) . ? O2 C25 1.321(2) . ? N1 C15 1.313(2) . ? N1 C2 1.411(2) . ? N2 C25 1.283(2) . ? N2 C9 1.407(2) . ? N3 C36 1.464(2) . ? N3 C35 1.471(2) . ? N4 C38 1.460(2) . ? N4 C37 1.463(2) . ? N5 C39 1.456(2) . ? N5 C40 1.458(2) . ? C1 C2 1.403(2) . ? C1 C6 1.410(2) . ? C1 C8 1.506(2) . ? C2 C3 1.399(2) . ? C3 C4 1.378(2) . ? C3 H3 0.9500 . ? C4 C5 1.384(2) . ? C4 H4 0.9500 . ? C5 C6 1.389(2) . ? C5 H5 0.9500 . ? C6 C7 1.507(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C13 1.398(2) . ? C8 C9 1.413(2) . ? C9 C10 1.404(2) . ? C10 C11 1.378(2) . ? C10 H10 0.9500 . ? C11 C12 1.380(3) . ? C11 H11 0.9500 . ? C12 C13 1.397(2) . ? C12 H12 0.9500 . ? C13 C14 1.508(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.489(2) . ? C16 C21 1.401(2) . ? C16 C17 1.405(2) . ? C17 C18 1.393(2) . ? C17 C22 1.507(2) . ? C18 C19 1.384(2) . ? C18 H18 0.9500 . ? C19 C20 1.386(2) . ? C19 C23 1.508(2) . ? C20 C21 1.390(2) . ? C20 H20 0.9500 . ? C21 C24 1.512(2) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.504(2) . ? C26 C31 1.410(2) . ? C26 C27 1.412(2) . ? C27 C28 1.389(2) . ? C27 C32 1.510(2) . ? C28 C29 1.391(2) . ? C28 H28 0.9500 . ? C29 C30 1.387(2) . ? C29 C33 1.506(2) . ? C30 C31 1.391(2) . ? C30 H30 0.9500 . ? C31 C34 1.506(2) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Nb1 N5 111.67(6) . . ? N4 Nb1 N3 94.07(6) . . ? N5 Nb1 N3 88.03(6) . . ? N4 Nb1 O2 92.10(5) . . ? N5 Nb1 O2 93.15(5) . . ? N3 Nb1 O2 172.80(5) . . ? N4 Nb1 O1 87.15(5) . . ? N5 Nb1 O1 160.34(5) . . ? N3 Nb1 O1 84.85(5) . . ? O2 Nb1 O1 91.76(4) . . ? N4 Nb1 N1 143.82(5) . . ? N5 Nb1 N1 103.87(6) . . ? N3 Nb1 N1 93.70(5) . . ? O2 Nb1 N1 79.12(5) . . ? O1 Nb1 N1 58.48(5) . . ? N4 Nb1 C15 115.70(5) . . ? N5 Nb1 C15 132.62(5) . . ? N3 Nb1 C15 87.59(5) . . ? O2 Nb1 C15 86.39(5) . . ? O1 Nb1 C15 28.90(5) . . ? N1 Nb1 C15 29.66(5) . . ? C15 O1 Nb1 96.30(10) . . ? C25 O2 Nb1 138.72(10) . . ? C15 N1 C2 128.62(14) . . ? C15 N1 Nb1 91.24(10) . . ? C2 N1 Nb1 139.00(11) . . ? C25 N2 C9 122.20(14) . . ? C36 N3 C35 108.24(14) . . ? C36 N3 Nb1 127.48(11) . . ? C35 N3 Nb1 123.43(11) . . ? C38 N4 C37 111.16(14) . . ? C38 N4 Nb1 128.43(11) . . ? C37 N4 Nb1 119.32(11) . . ? C39 N5 C40 110.85(14) . . ? C39 N5 Nb1 121.32(11) . . ? C40 N5 Nb1 127.58(11) . . ? C2 C1 C6 118.85(15) . . ? C2 C1 C8 123.32(15) . . ? C6 C1 C8 117.83(15) . . ? C3 C2 C1 120.01(15) . . ? C3 C2 N1 117.46(15) . . ? C1 C2 N1 122.14(14) . . ? C4 C3 C2 120.46(16) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C5 120.00(16) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 120.74(16) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 119.91(16) . . ? C5 C6 C7 118.76(16) . . ? C1 C6 C7 121.30(15) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C13 C8 C9 119.93(15) . . ? C13 C8 C1 118.92(14) . . ? C9 C8 C1 120.62(14) . . ? C10 C9 N2 117.73(15) . . ? C10 C9 C8 118.71(15) . . ? N2 C9 C8 122.76(14) . . ? C11 C10 C9 120.90(16) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C10 C11 C12 120.19(16) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C13 120.65(16) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C12 C13 C8 119.60(16) . . ? C12 C13 C14 118.64(16) . . ? C8 C13 C14 121.70(15) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O1 C15 N1 113.70(15) . . ? O1 C15 C16 117.72(14) . . ? N1 C15 C16 128.32(15) . . ? O1 C15 Nb1 54.79(8) . . ? N1 C15 Nb1 59.11(9) . . ? C16 C15 Nb1 168.31(12) . . ? C21 C16 C17 120.61(16) . . ? C21 C16 C15 120.25(15) . . ? C17 C16 C15 118.69(15) . . ? C18 C17 C16 118.08(16) . . ? C18 C17 C22 119.98(16) . . ? C16 C17 C22 121.91(15) . . ? C19 C18 C17 122.48(17) . . ? C19 C18 H18 118.8 . . ? C17 C18 H18 118.8 . . ? C18 C19 C20 117.97(16) . . ? C18 C19 C23 122.02(17) . . ? C20 C19 C23 119.98(17) . . ? C19 C20 C21 122.19(17) . . ? C19 C20 H20 118.9 . . ? C21 C20 H20 118.9 . . ? C20 C21 C16 118.60(16) . . ? C20 C21 C24 117.76(16) . . ? C16 C21 C24 123.50(16) . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N2 C25 O2 125.02(15) . . ? N2 C25 C26 117.83(14) . . ? O2 C25 C26 117.12(14) . . ? C31 C26 C27 118.97(15) . . ? C31 C26 C25 120.63(14) . . ? C27 C26 C25 120.39(14) . . ? C28 C27 C26 119.33(16) . . ? C28 C27 C32 117.70(15) . . ? C26 C27 C32 122.97(15) . . ? C27 C28 C29 122.50(16) . . ? C27 C28 H28 118.8 . . ? C29 C28 H28 118.8 . . ? C30 C29 C28 117.32(16) . . ? C30 C29 C33 121.09(16) . . ? C28 C29 C33 121.55(17) . . ? C29 C30 C31 122.59(16) . . ? C29 C30 H30 118.7 . . ? C31 C30 H30 118.7 . . ? C30 C31 C26 119.27(16) . . ? C30 C31 C34 117.54(15) . . ? C26 C31 C34 123.16(15) . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C33 H33A 109.5 . . ? C29 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C29 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N3 C35 H35A 109.5 . . ? N3 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N3 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N3 C36 H36A 109.5 . . ? N3 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N3 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N4 C37 H37A 109.5 . . ? N4 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N4 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N4 C38 H38A 109.5 . . ? N4 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N4 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N5 C39 H39A 109.5 . . ? N5 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N5 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N5 C40 H40A 109.5 . . ? N5 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N5 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Nb1 O1 C15 171.31(10) . . . . ? N5 Nb1 O1 C15 -25.13(19) . . . . ? N3 Nb1 O1 C15 -94.34(10) . . . . ? O2 Nb1 O1 C15 79.29(10) . . . . ? N1 Nb1 O1 C15 3.21(9) . . . . ? N4 Nb1 O2 C25 142.99(16) . . . . ? N5 Nb1 O2 C25 31.15(16) . . . . ? N3 Nb1 O2 C25 -68.0(4) . . . . ? O1 Nb1 O2 C25 -129.80(15) . . . . ? N1 Nb1 O2 C25 -72.38(16) . . . . ? C15 Nb1 O2 C25 -101.38(16) . . . . ? N4 Nb1 N1 C15 -23.54(14) . . . . ? N5 Nb1 N1 C15 167.40(9) . . . . ? N3 Nb1 N1 C15 78.52(10) . . . . ? O2 Nb1 N1 C15 -102.02(10) . . . . ? O1 Nb1 N1 C15 -3.13(9) . . . . ? N4 Nb1 N1 C2 144.04(15) . . . . ? N5 Nb1 N1 C2 -25.02(17) . . . . ? N3 Nb1 N1 C2 -113.90(16) . . . . ? O2 Nb1 N1 C2 65.56(16) . . . . ? O1 Nb1 N1 C2 164.45(18) . . . . ? C15 Nb1 N1 C2 167.6(2) . . . . ? N4 Nb1 N3 C36 -139.07(15) . . . . ? N5 Nb1 N3 C36 -27.48(15) . . . . ? O2 Nb1 N3 C36 72.0(4) . . . . ? O1 Nb1 N3 C36 134.17(15) . . . . ? N1 Nb1 N3 C36 76.29(15) . . . . ? C15 Nb1 N3 C36 105.33(15) . . . . ? N4 Nb1 N3 C35 52.77(15) . . . . ? N5 Nb1 N3 C35 164.36(15) . . . . ? O2 Nb1 N3 C35 -96.1(4) . . . . ? O1 Nb1 N3 C35 -33.99(14) . . . . ? N1 Nb1 N3 C35 -91.86(15) . . . . ? C15 Nb1 N3 C35 -62.83(15) . . . . ? N5 Nb1 N4 C38 -62.33(16) . . . . ? N3 Nb1 N4 C38 27.16(15) . . . . ? O2 Nb1 N4 C38 -156.55(15) . . . . ? O1 Nb1 N4 C38 111.79(15) . . . . ? N1 Nb1 N4 C38 129.11(14) . . . . ? C15 Nb1 N4 C38 116.44(15) . . . . ? N5 Nb1 N4 C37 130.77(12) . . . . ? N3 Nb1 N4 C37 -139.74(13) . . . . ? O2 Nb1 N4 C37 36.54(13) . . . . ? O1 Nb1 N4 C37 -55.11(12) . . . . ? N1 Nb1 N4 C37 -37.80(17) . . . . ? C15 Nb1 N4 C37 -50.47(14) . . . . ? N4 Nb1 N5 C39 23.00(15) . . . . ? N3 Nb1 N5 C39 -70.59(14) . . . . ? O2 Nb1 N5 C39 116.52(14) . . . . ? O1 Nb1 N5 C39 -139.29(16) . . . . ? N1 Nb1 N5 C39 -163.92(14) . . . . ? C15 Nb1 N5 C39 -155.49(13) . . . . ? N4 Nb1 N5 C40 -163.32(13) . . . . ? N3 Nb1 N5 C40 103.08(14) . . . . ? O2 Nb1 N5 C40 -69.80(14) . . . . ? O1 Nb1 N5 C40 34.4(2) . . . . ? N1 Nb1 N5 C40 9.75(14) . . . . ? C15 Nb1 N5 C40 18.19(17) . . . . ? C6 C1 C2 C3 -1.0(2) . . . . ? C8 C1 C2 C3 179.42(15) . . . . ? C6 C1 C2 N1 171.65(15) . . . . ? C8 C1 C2 N1 -8.0(2) . . . . ? C15 N1 C2 C3 -121.34(18) . . . . ? Nb1 N1 C2 C3 74.6(2) . . . . ? C15 N1 C2 C1 65.9(2) . . . . ? Nb1 N1 C2 C1 -98.15(19) . . . . ? C1 C2 C3 C4 -0.8(2) . . . . ? N1 C2 C3 C4 -173.73(15) . . . . ? C2 C3 C4 C5 1.4(3) . . . . ? C3 C4 C5 C6 -0.2(3) . . . . ? C4 C5 C6 C1 -1.6(3) . . . . ? C4 C5 C6 C7 176.28(16) . . . . ? C2 C1 C6 C5 2.1(2) . . . . ? C8 C1 C6 C5 -178.23(15) . . . . ? C2 C1 C6 C7 -175.69(16) . . . . ? C8 C1 C6 C7 4.0(2) . . . . ? C2 C1 C8 C13 -103.00(19) . . . . ? C6 C1 C8 C13 77.4(2) . . . . ? C2 C1 C8 C9 85.4(2) . . . . ? C6 C1 C8 C9 -94.27(19) . . . . ? C25 N2 C9 C10 102.91(18) . . . . ? C25 N2 C9 C8 -87.5(2) . . . . ? C13 C8 C9 C10 1.4(2) . . . . ? C1 C8 C9 C10 173.00(15) . . . . ? C13 C8 C9 N2 -168.04(15) . . . . ? C1 C8 C9 N2 3.5(2) . . . . ? N2 C9 C10 C11 169.72(16) . . . . ? C8 C9 C10 C11 -0.3(3) . . . . ? C9 C10 C11 C12 -0.8(3) . . . . ? C10 C11 C12 C13 0.8(3) . . . . ? C11 C12 C13 C8 0.4(3) . . . . ? C11 C12 C13 C14 -176.73(17) . . . . ? C9 C8 C13 C12 -1.5(3) . . . . ? C1 C8 C13 C12 -173.19(16) . . . . ? C9 C8 C13 C14 175.53(16) . . . . ? C1 C8 C13 C14 3.8(3) . . . . ? Nb1 O1 C15 N1 -5.18(14) . . . . ? Nb1 O1 C15 C16 169.46(12) . . . . ? C2 N1 C15 O1 -164.66(15) . . . . ? Nb1 N1 C15 O1 4.93(14) . . . . ? C2 N1 C15 C16 21.4(3) . . . . ? Nb1 N1 C15 C16 -169.02(16) . . . . ? C2 N1 C15 Nb1 -169.60(18) . . . . ? N4 Nb1 C15 O1 -9.64(11) . . . . ? N5 Nb1 C15 O1 168.80(9) . . . . ? N3 Nb1 C15 O1 83.72(10) . . . . ? O2 Nb1 C15 O1 -100.24(9) . . . . ? N1 Nb1 C15 O1 -174.47(15) . . . . ? N4 Nb1 C15 N1 164.83(9) . . . . ? N5 Nb1 C15 N1 -16.73(13) . . . . ? N3 Nb1 C15 N1 -101.81(10) . . . . ? O2 Nb1 C15 N1 74.23(10) . . . . ? O1 Nb1 C15 N1 174.47(15) . . . . ? N4 Nb1 C15 C16 -62.7(6) . . . . ? N5 Nb1 C15 C16 115.7(6) . . . . ? N3 Nb1 C15 C16 30.6(6) . . . . ? O2 Nb1 C15 C16 -153.3(6) . . . . ? O1 Nb1 C15 C16 -53.1(5) . . . . ? N1 Nb1 C15 C16 132.4(6) . . . . ? O1 C15 C16 C21 -119.97(18) . . . . ? N1 C15 C16 C21 53.8(3) . . . . ? Nb1 C15 C16 C21 -72.4(6) . . . . ? O1 C15 C16 C17 52.3(2) . . . . ? N1 C15 C16 C17 -133.93(18) . . . . ? Nb1 C15 C16 C17 99.9(6) . . . . ? C21 C16 C17 C18 -3.3(3) . . . . ? C15 C16 C17 C18 -175.59(16) . . . . ? C21 C16 C17 C22 174.49(17) . . . . ? C15 C16 C17 C22 2.2(3) . . . . ? C16 C17 C18 C19 1.9(3) . . . . ? C22 C17 C18 C19 -175.91(18) . . . . ? C17 C18 C19 C20 0.0(3) . . . . ? C17 C18 C19 C23 178.00(17) . . . . ? C18 C19 C20 C21 -0.5(3) . . . . ? C23 C19 C20 C21 -178.62(17) . . . . ? C19 C20 C21 C16 -0.8(3) . . . . ? C19 C20 C21 C24 175.11(17) . . . . ? C17 C16 C21 C20 2.8(3) . . . . ? C15 C16 C21 C20 174.94(16) . . . . ? C17 C16 C21 C24 -172.90(17) . . . . ? C15 C16 C21 C24 -0.7(3) . . . . ? C9 N2 C25 O2 -1.5(2) . . . . ? C9 N2 C25 C26 -179.85(14) . . . . ? Nb1 O2 C25 N2 118.48(17) . . . . ? Nb1 O2 C25 C26 -63.2(2) . . . . ? N2 C25 C26 C31 137.19(16) . . . . ? O2 C25 C26 C31 -41.3(2) . . . . ? N2 C25 C26 C27 -42.7(2) . . . . ? O2 C25 C26 C27 138.78(15) . . . . ? C31 C26 C27 C28 0.5(2) . . . . ? C25 C26 C27 C28 -179.55(14) . . . . ? C31 C26 C27 C32 -179.93(15) . . . . ? C25 C26 C27 C32 0.0(2) . . . . ? C26 C27 C28 C29 -0.4(2) . . . . ? C32 C27 C28 C29 -179.96(15) . . . . ? C27 C28 C29 C30 0.7(2) . . . . ? C27 C28 C29 C33 -177.17(16) . . . . ? C28 C29 C30 C31 -1.2(2) . . . . ? C33 C29 C30 C31 176.67(16) . . . . ? C29 C30 C31 C26 1.4(2) . . . . ? C29 C30 C31 C34 -176.82(15) . . . . ? C27 C26 C31 C30 -1.0(2) . . . . ? C25 C26 C31 C30 179.07(14) . . . . ? C27 C26 C31 C34 177.11(15) . . . . ? C25 C26 C31 C34 -2.8(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.609 _refine_diff_density_min -0.487 _refine_diff_density_rms 0.073 # Attachment 'compound-9.cif.txt' data_compound9 _database_code_depnum_ccdc_archive 'CCDC 775662' #TrackingRef 'compound-9.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H52 N5 O2 Ta' _chemical_formula_sum 'C40 H52 N5 O2 Ta' _chemical_formula_weight 815.82 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' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.7613(18) _cell_length_b 12.259(2) _cell_length_c 15.969(3) _cell_angle_alpha 82.373(6) _cell_angle_beta 77.151(5) _cell_angle_gamma 89.891(6) _cell_volume 1845.7(6) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 7008 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 27.9 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.468 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 3.018 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5311 _exptl_absorpt_correction_T_max 0.5835 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 22062 _diffrn_reflns_av_R_equivalents 0.0344 _diffrn_reflns_av_sigmaI/netI 0.0295 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.32 _diffrn_reflns_theta_max 27.89 _reflns_number_total 8670 _reflns_number_gt 8385 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.8' _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^)+(0.0589P)^2^+0.3703P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0504(11) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 8670 _refine_ls_number_parameters 449 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0350 _refine_ls_wR_factor_ref 0.0889 _refine_ls_wR_factor_gt 0.0863 _refine_ls_goodness_of_fit_ref 1.212 _refine_ls_restrained_S_all 1.212 _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 Ta1 Ta 0.190096(9) 0.991424(7) 0.203050(6) 0.01279(7) Uani 1 1 d . . . O1 O 0.2724(2) 0.85791(17) 0.13230(13) 0.0174(4) Uani 1 1 d . . . O2 O -0.0116(2) 0.94883(18) 0.19988(15) 0.0165(4) Uani 1 1 d . . . N1 N 0.1744(2) 0.8149(2) 0.26867(15) 0.0157(5) Uani 1 1 d . . . N2 N -0.2048(2) 0.8364(2) 0.26729(16) 0.0168(5) Uani 1 1 d . . . N3 N 0.1272(3) 1.0762(2) 0.30123(16) 0.0171(5) Uani 1 1 d . . . N4 N 0.3879(3) 1.0143(2) 0.21424(18) 0.0176(5) Uani 1 1 d . . . N5 N 0.2174(3) 1.0863(2) 0.09080(15) 0.0171(5) Uani 1 1 d . . . C1 C -0.0203(3) 0.6855(2) 0.34677(18) 0.0160(5) Uani 1 1 d . . . C2 C 0.0990(3) 0.7506(2) 0.34537(18) 0.0149(5) Uani 1 1 d . . . C3 C 0.1371(3) 0.7635(2) 0.4237(2) 0.0188(6) Uani 1 1 d . . . H3A H 0.2165 0.8086 0.4229 0.023 Uiso 1 1 calc R . . C4 C 0.0595(3) 0.7107(3) 0.5014(2) 0.0209(6) Uani 1 1 d . . . H4A H 0.0873 0.7177 0.5538 0.025 Uiso 1 1 calc R . . C5 C -0.0594(3) 0.6474(2) 0.50301(19) 0.0211(6) Uani 1 1 d . . . H5A H -0.1129 0.6121 0.5569 0.025 Uiso 1 1 calc R . . C6 C -0.1007(3) 0.6352(2) 0.42726(19) 0.0186(6) Uani 1 1 d . . . C7 C -0.2348(4) 0.5708(3) 0.4330(2) 0.0281(7) Uani 1 1 d . . . H7A H -0.2691 0.5342 0.4924 0.042 Uiso 1 1 calc R . . H7B H -0.2165 0.5153 0.3932 0.042 Uiso 1 1 calc R . . H7C H -0.3059 0.6210 0.4171 0.042 Uiso 1 1 calc R . . C8 C -0.0669(3) 0.6675(2) 0.26589(18) 0.0158(5) Uani 1 1 d . . . C9 C -0.1528(3) 0.7434(2) 0.22880(18) 0.0153(5) Uani 1 1 d . . . C10 C -0.2065(3) 0.7179(2) 0.1595(2) 0.0201(6) Uani 1 1 d . . . H10 H -0.2633 0.7693 0.1339 0.024 Uiso 1 1 calc R . . C11 C -0.1782(4) 0.6185(3) 0.1275(2) 0.0241(6) Uani 1 1 d . . . H11 H -0.2150 0.6022 0.0801 0.029 Uiso 1 1 calc R . . C12 C -0.0960(4) 0.5430(3) 0.1649(2) 0.0240(6) Uani 1 1 d . . . H12 H -0.0780 0.4745 0.1433 0.029 Uiso 1 1 calc R . . C13 C -0.0396(3) 0.5658(2) 0.23317(19) 0.0194(6) Uani 1 1 d . . . C14 C 0.0429(4) 0.4787(3) 0.2747(2) 0.0261(7) Uani 1 1 d . . . H14A H -0.0198 0.4356 0.3245 0.039 Uiso 1 1 calc R . . H14B H 0.1181 0.5139 0.2941 0.039 Uiso 1 1 calc R . . H14C H 0.0839 0.4299 0.2323 0.039 Uiso 1 1 calc R . . C15 C 0.2452(3) 0.7808(2) 0.19756(18) 0.0159(5) Uani 1 1 d . . . C16 C 0.3083(3) 0.6719(2) 0.18611(18) 0.0167(5) Uani 1 1 d . . . C17 C 0.3984(3) 0.6278(2) 0.23876(19) 0.0188(6) Uani 1 1 d . . . C18 C 0.4647(3) 0.5297(3) 0.2216(2) 0.0216(6) Uani 1 1 d . . . H18 H 0.5245 0.4990 0.2575 0.026 Uiso 1 1 calc R . . C19 C 0.4464(3) 0.4757(3) 0.1539(2) 0.0224(6) Uani 1 1 d . . . C20 C 0.3587(3) 0.5223(3) 0.1016(2) 0.0210(6) Uani 1 1 d . . . H20 H 0.3444 0.4858 0.0553 0.025 Uiso 1 1 calc R . . C21 C 0.2914(3) 0.6208(2) 0.11538(19) 0.0189(6) Uani 1 1 d . . . C22 C 0.4357(3) 0.6852(3) 0.3090(2) 0.0258(7) Uani 1 1 d . . . H22A H 0.3747 0.6565 0.3650 0.039 Uiso 1 1 calc R . . H22B H 0.4226 0.7645 0.2965 0.039 Uiso 1 1 calc R . . H22C H 0.5340 0.6720 0.3110 0.039 Uiso 1 1 calc R . . C23 C 0.5239(4) 0.3716(3) 0.1370(3) 0.0300(7) Uani 1 1 d . . . H23A H 0.6240 0.3840 0.1343 0.045 Uiso 1 1 calc R . . H23B H 0.5120 0.3508 0.0819 0.045 Uiso 1 1 calc R . . H23C H 0.4860 0.3124 0.1841 0.045 Uiso 1 1 calc R . . C24 C 0.2057(3) 0.6714(3) 0.0528(2) 0.0229(6) Uani 1 1 d . . . H24A H 0.1203 0.7019 0.0851 0.034 Uiso 1 1 calc R . . H24B H 0.1800 0.6148 0.0206 0.034 Uiso 1 1 calc R . . H24C H 0.2615 0.7304 0.0120 0.034 Uiso 1 1 calc R . . C25 C -0.1364(3) 0.9286(2) 0.25270(18) 0.0141(5) Uani 1 1 d . . . C26 C -0.2040(3) 1.0220(2) 0.29766(17) 0.0141(5) Uani 1 1 d . . . C27 C -0.1981(3) 1.1299(2) 0.25232(19) 0.0164(5) Uani 1 1 d . . . C28 C -0.2612(3) 1.2151(2) 0.2957(2) 0.0192(6) Uani 1 1 d . . . H28 H -0.2555 1.2874 0.2651 0.023 Uiso 1 1 calc R . . C29 C -0.3319(3) 1.1976(3) 0.3820(2) 0.0202(6) Uani 1 1 d . . . C30 C -0.3376(3) 1.0914(3) 0.4265(2) 0.0184(6) Uani 1 1 d . . . H30 H -0.3844 1.0784 0.4859 0.022 Uiso 1 1 calc R . . C31 C -0.2760(3) 1.0032(2) 0.38566(19) 0.0165(5) Uani 1 1 d . . . C32 C -0.1317(3) 1.1577(3) 0.1573(2) 0.0218(6) Uani 1 1 d . . . H32A H -0.1746 1.2234 0.1333 0.033 Uiso 1 1 calc R . . H32B H -0.1466 1.0958 0.1270 0.033 Uiso 1 1 calc R . . H32C H -0.0306 1.1719 0.1497 0.033 Uiso 1 1 calc R . . C33 C -0.4058(4) 1.2906(3) 0.4262(2) 0.0275(7) Uani 1 1 d . . . H33A H -0.3652 1.3614 0.3947 0.041 Uiso 1 1 calc R . . H33B H -0.3938 1.2838 0.4860 0.041 Uiso 1 1 calc R . . H33C H -0.5062 1.2868 0.4265 0.041 Uiso 1 1 calc R . . C34 C -0.2884(3) 0.8913(3) 0.4402(2) 0.0203(6) Uani 1 1 d . . . H34A H -0.3285 0.8991 0.5010 0.030 Uiso 1 1 calc R . . H34B H -0.1951 0.8597 0.4350 0.030 Uiso 1 1 calc R . . H34C H -0.3498 0.8425 0.4199 0.030 Uiso 1 1 calc R . . C35 C 0.1593(5) 1.1932(3) 0.2936(3) 0.0392(10) Uani 1 1 d . . . H35A H 0.0719 1.2328 0.3088 0.059 Uiso 1 1 calc R . . H35B H 0.2079 1.2202 0.2338 0.059 Uiso 1 1 calc R . . H35C H 0.2200 1.2056 0.3330 0.059 Uiso 1 1 calc R . . C36 C 0.0579(3) 1.0341(3) 0.38978(18) 0.0192(6) Uani 1 1 d . . . H36A H 0.1226 1.0405 0.4280 0.029 Uiso 1 1 calc R . . H36B H 0.0302 0.9566 0.3931 0.029 Uiso 1 1 calc R . . H36C H -0.0259 1.0768 0.4081 0.029 Uiso 1 1 calc R . . C37 C 0.5102(3) 0.9986(3) 0.1455(2) 0.0297(7) Uani 1 1 d . . . H37A H 0.5762 1.0614 0.1364 0.044 Uiso 1 1 calc R . . H37B H 0.4798 0.9929 0.0917 0.044 Uiso 1 1 calc R . . H37C H 0.5566 0.9308 0.1624 0.044 Uiso 1 1 calc R . . C38 C 0.4350(3) 1.0288(3) 0.2925(2) 0.0269(7) Uani 1 1 d . . . H38A H 0.4932 0.9670 0.3070 0.040 Uiso 1 1 calc R . . H38B H 0.3531 1.0314 0.3405 0.040 Uiso 1 1 calc R . . H38C H 0.4903 1.0978 0.2827 0.040 Uiso 1 1 calc R . . C39 C 0.1560(3) 1.0525(3) 0.0223(2) 0.0229(6) Uani 1 1 d . . . H39A H 0.0985 1.1116 0.0022 0.034 Uiso 1 1 calc R . . H39B H 0.0970 0.9858 0.0450 0.034 Uiso 1 1 calc R . . H39C H 0.2313 1.0373 -0.0263 0.034 Uiso 1 1 calc R . . C40 C 0.3126(4) 1.1815(3) 0.0584(2) 0.0300(7) Uani 1 1 d . . . H40A H 0.3775 1.1685 0.0045 0.045 Uiso 1 1 calc R . . H40B H 0.3661 1.1931 0.1018 0.045 Uiso 1 1 calc R . . H40C H 0.2581 1.2469 0.0471 0.045 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ta1 0.01181(9) 0.01434(9) 0.01279(9) -0.00129(5) -0.00430(5) 0.00067(5) O1 0.0204(10) 0.0165(10) 0.0152(10) -0.0015(8) -0.0039(8) 0.0032(8) O2 0.0123(9) 0.0176(10) 0.0197(11) -0.0017(8) -0.0043(8) 0.0012(8) N1 0.0185(11) 0.0167(11) 0.0127(11) -0.0011(9) -0.0057(9) 0.0018(9) N2 0.0162(11) 0.0170(11) 0.0180(12) 0.0000(9) -0.0070(9) 0.0005(9) N3 0.0181(11) 0.0177(12) 0.0153(12) -0.0025(9) -0.0034(9) -0.0002(9) N4 0.0114(11) 0.0256(14) 0.0180(12) -0.0069(10) -0.0059(9) 0.0008(9) N5 0.0202(11) 0.0190(12) 0.0127(11) 0.0008(9) -0.0068(9) -0.0013(9) C1 0.0207(13) 0.0158(13) 0.0133(12) -0.0009(10) -0.0081(10) 0.0041(10) C2 0.0164(12) 0.0150(13) 0.0139(13) -0.0002(10) -0.0058(10) 0.0040(10) C3 0.0174(13) 0.0193(14) 0.0218(15) -0.0021(11) -0.0094(11) 0.0036(10) C4 0.0265(15) 0.0221(15) 0.0166(14) -0.0012(11) -0.0110(12) 0.0078(12) C5 0.0270(15) 0.0202(14) 0.0144(13) 0.0031(11) -0.0047(11) 0.0015(11) C6 0.0220(14) 0.0155(13) 0.0188(14) 0.0017(10) -0.0078(11) 0.0019(10) C7 0.0280(16) 0.0284(17) 0.0271(17) 0.0018(13) -0.0078(13) -0.0061(13) C8 0.0177(13) 0.0139(13) 0.0165(13) 0.0001(10) -0.0066(10) -0.0018(10) C9 0.0145(12) 0.0144(12) 0.0169(13) 0.0017(10) -0.0060(10) -0.0019(10) C10 0.0216(14) 0.0198(14) 0.0204(14) 0.0017(11) -0.0107(11) -0.0003(11) C11 0.0318(16) 0.0244(15) 0.0196(15) -0.0033(12) -0.0131(12) -0.0027(12) C12 0.0348(17) 0.0171(14) 0.0228(15) -0.0055(11) -0.0108(13) 0.0001(12) C13 0.0255(15) 0.0149(13) 0.0177(14) 0.0015(11) -0.0070(11) 0.0003(11) C14 0.0347(18) 0.0168(14) 0.0286(17) 0.0010(12) -0.0137(14) 0.0068(12) C15 0.0157(12) 0.0180(13) 0.0164(13) -0.0035(10) -0.0079(10) 0.0018(10) C16 0.0171(13) 0.0185(13) 0.0156(13) -0.0028(10) -0.0057(10) 0.0038(10) C17 0.0214(14) 0.0199(14) 0.0178(13) -0.0033(11) -0.0095(11) 0.0035(11) C18 0.0198(14) 0.0223(15) 0.0242(15) -0.0003(11) -0.0104(11) 0.0062(11) C19 0.0201(14) 0.0165(14) 0.0308(17) -0.0028(12) -0.0063(12) 0.0030(11) C20 0.0239(15) 0.0205(15) 0.0208(15) -0.0073(12) -0.0072(12) 0.0020(12) C21 0.0210(13) 0.0216(14) 0.0161(13) -0.0052(11) -0.0069(11) 0.0028(11) C22 0.0262(15) 0.0327(17) 0.0251(16) -0.0106(13) -0.0160(13) 0.0100(13) C23 0.0282(16) 0.0191(15) 0.044(2) -0.0076(14) -0.0096(15) 0.0080(13) C24 0.0276(15) 0.0278(16) 0.0179(14) -0.0073(12) -0.0120(12) 0.0077(12) C25 0.0112(11) 0.0160(13) 0.0165(13) -0.0004(10) -0.0073(10) 0.0024(10) C26 0.0123(12) 0.0162(13) 0.0144(14) -0.0013(11) -0.0050(10) 0.0001(10) C27 0.0130(12) 0.0168(13) 0.0205(14) 0.0003(10) -0.0078(10) 0.0003(10) C28 0.0176(13) 0.0160(13) 0.0255(15) -0.0014(11) -0.0085(11) 0.0013(10) C29 0.0142(12) 0.0217(14) 0.0266(15) -0.0071(12) -0.0063(11) 0.0012(10) C30 0.0155(13) 0.0244(15) 0.0171(14) -0.0037(11) -0.0067(11) 0.0015(11) C31 0.0134(12) 0.0201(14) 0.0175(13) -0.0013(11) -0.0072(10) 0.0012(10) C32 0.0230(15) 0.0200(15) 0.0207(15) 0.0042(11) -0.0054(12) 0.0027(11) C33 0.0280(16) 0.0230(16) 0.0330(18) -0.0102(13) -0.0060(13) 0.0035(12) C34 0.0227(14) 0.0199(15) 0.0168(14) 0.0019(11) -0.0041(11) -0.0002(11) C35 0.058(2) 0.0185(16) 0.0322(19) -0.0088(14) 0.0111(17) -0.0069(16) C36 0.0216(14) 0.0230(15) 0.0131(13) -0.0022(11) -0.0042(11) 0.0013(11) C37 0.0133(14) 0.048(2) 0.0270(17) -0.0092(15) -0.0008(12) 0.0007(14) C38 0.0189(14) 0.0392(19) 0.0258(16) -0.0061(14) -0.0104(12) -0.0025(13) C39 0.0217(14) 0.0326(17) 0.0155(14) -0.0011(12) -0.0078(11) -0.0035(12) C40 0.0378(19) 0.0311(18) 0.0209(16) 0.0046(13) -0.0108(14) -0.0137(15) _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 Ta1 N5 1.968(2) . ? Ta1 N3 1.979(2) . ? Ta1 N4 2.002(3) . ? Ta1 O2 2.051(2) . ? Ta1 O1 2.164(2) . ? Ta1 N1 2.266(2) . ? Ta1 C15 2.645(3) . ? O1 C15 1.291(4) . ? O2 C25 1.322(4) . ? N1 C15 1.310(4) . ? N1 C2 1.417(4) . ? N2 C25 1.281(4) . ? N2 C9 1.407(4) . ? N3 C36 1.451(4) . ? N3 C35 1.452(4) . ? N4 C38 1.456(4) . ? N4 C37 1.463(4) . ? N5 C40 1.457(4) . ? N5 C39 1.463(4) . ? C1 C2 1.407(4) . ? C1 C6 1.411(4) . ? C1 C8 1.503(4) . ? C2 C3 1.409(4) . ? C3 C4 1.379(4) . ? C3 H3A 0.9500 . ? C4 C5 1.391(4) . ? C4 H4A 0.9500 . ? C5 C6 1.384(4) . ? C5 H5A 0.9500 . ? C6 C7 1.509(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.412(4) . ? C8 C13 1.416(4) . ? C9 C10 1.396(4) . ? C10 C11 1.387(4) . ? C10 H10 0.9500 . ? C11 C12 1.386(5) . ? C11 H11 0.9500 . ? C12 C13 1.386(4) . ? C12 H12 0.9500 . ? C13 C14 1.509(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.485(4) . ? C16 C21 1.402(4) . ? C16 C17 1.407(4) . ? C17 C18 1.395(4) . ? C17 C22 1.509(4) . ? C18 C19 1.385(5) . ? C18 H18 0.9500 . ? C19 C20 1.395(4) . ? C19 C23 1.506(4) . ? C20 C21 1.393(4) . ? C20 H20 0.9500 . ? C21 C24 1.513(4) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.505(4) . ? C26 C31 1.413(4) . ? C26 C27 1.416(4) . ? C27 C28 1.397(4) . ? C27 C32 1.505(4) . ? C28 C29 1.386(4) . ? C28 H28 0.9500 . ? C29 C30 1.393(4) . ? C29 C33 1.518(4) . ? C30 C31 1.402(4) . ? C30 H30 0.9500 . ? C31 C34 1.515(4) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Ta1 N3 111.60(11) . . ? N5 Ta1 N4 93.99(11) . . ? N3 Ta1 N4 88.26(11) . . ? N5 Ta1 O2 92.09(10) . . ? N3 Ta1 O2 92.98(10) . . ? N4 Ta1 O2 172.86(9) . . ? N5 Ta1 O1 87.79(9) . . ? N3 Ta1 O1 159.98(10) . . ? N4 Ta1 O1 85.35(10) . . ? O2 Ta1 O1 91.16(8) . . ? N5 Ta1 N1 144.68(9) . . ? N3 Ta1 N1 103.05(10) . . ? N4 Ta1 N1 93.68(10) . . ? O2 Ta1 N1 79.18(9) . . ? O1 Ta1 N1 58.59(8) . . ? N5 Ta1 C15 116.49(9) . . ? N3 Ta1 C15 131.91(10) . . ? N4 Ta1 C15 87.73(10) . . ? O2 Ta1 C15 86.20(9) . . ? O1 Ta1 C15 28.99(8) . . ? N1 Ta1 C15 29.68(9) . . ? C15 O1 Ta1 96.67(17) . . ? C25 O2 Ta1 140.0(2) . . ? C15 N1 C2 128.1(3) . . ? C15 N1 Ta1 91.41(17) . . ? C2 N1 Ta1 139.19(19) . . ? C25 N2 C9 123.0(2) . . ? C36 N3 C35 110.3(3) . . ? C36 N3 Ta1 127.7(2) . . ? C35 N3 Ta1 121.8(2) . . ? C38 N4 C37 109.1(3) . . ? C38 N4 Ta1 127.3(2) . . ? C37 N4 Ta1 122.8(2) . . ? C40 N5 C39 111.3(2) . . ? C40 N5 Ta1 128.3(2) . . ? C39 N5 Ta1 119.59(19) . . ? C2 C1 C6 119.0(3) . . ? C2 C1 C8 122.8(3) . . ? C6 C1 C8 118.2(3) . . ? C1 C2 C3 119.8(3) . . ? C1 C2 N1 122.2(2) . . ? C3 C2 N1 117.6(3) . . ? C4 C3 C2 120.2(3) . . ? C4 C3 H3A 119.9 . . ? C2 C3 H3A 119.9 . . ? C3 C4 C5 120.1(3) . . ? C3 C4 H4A 120.0 . . ? C5 C4 H4A 120.0 . . ? C6 C5 C4 120.9(3) . . ? C6 C5 H5A 119.6 . . ? C4 C5 H5A 119.6 . . ? C5 C6 C1 120.0(3) . . ? C5 C6 C7 118.8(3) . . ? C1 C6 C7 121.2(3) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C13 119.2(3) . . ? C9 C8 C1 121.2(3) . . ? C13 C8 C1 119.1(2) . . ? C10 C9 N2 117.6(2) . . ? C10 C9 C8 119.4(3) . . ? N2 C9 C8 122.2(3) . . ? C11 C10 C9 120.9(3) . . ? C11 C10 H10 119.6 . . ? C9 C10 H10 119.6 . . ? C12 C11 C10 119.8(3) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C13 C12 C11 120.9(3) . . ? C13 C12 H12 119.5 . . ? C11 C12 H12 119.5 . . ? C12 C13 C8 119.7(3) . . ? C12 C13 C14 118.9(3) . . ? C8 C13 C14 121.2(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O1 C15 N1 113.0(2) . . ? O1 C15 C16 118.0(2) . . ? N1 C15 C16 128.7(3) . . ? O1 C15 Ta1 54.34(14) . . ? N1 C15 Ta1 58.90(15) . . ? C16 C15 Ta1 167.3(2) . . ? C21 C16 C17 120.4(3) . . ? C21 C16 C15 119.0(3) . . ? C17 C16 C15 120.2(3) . . ? C18 C17 C16 118.6(3) . . ? C18 C17 C22 117.9(3) . . ? C16 C17 C22 123.4(3) . . ? C19 C18 C17 122.2(3) . . ? C19 C18 H18 118.9 . . ? C17 C18 H18 118.9 . . ? C18 C19 C20 118.0(3) . . ? C18 C19 C23 119.8(3) . . ? C20 C19 C23 122.2(3) . . ? C21 C20 C19 122.0(3) . . ? C21 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? C20 C21 C16 118.7(3) . . ? C20 C21 C24 119.6(3) . . ? C16 C21 C24 121.7(3) . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N2 C25 O2 125.0(3) . . ? N2 C25 C26 117.8(2) . . ? O2 C25 C26 117.2(2) . . ? C31 C26 C27 118.8(3) . . ? C31 C26 C25 120.6(2) . . ? C27 C26 C25 120.6(2) . . ? C28 C27 C26 119.4(3) . . ? C28 C27 C32 117.4(3) . . ? C26 C27 C32 123.1(3) . . ? C29 C28 C27 122.2(3) . . ? C29 C28 H28 118.9 . . ? C27 C28 H28 118.9 . . ? C28 C29 C30 118.2(3) . . ? C28 C29 C33 121.0(3) . . ? C30 C29 C33 120.7(3) . . ? C29 C30 C31 121.6(3) . . ? C29 C30 H30 119.2 . . ? C31 C30 H30 119.2 . . ? C30 C31 C26 119.7(3) . . ? C30 C31 C34 117.2(3) . . ? C26 C31 C34 123.1(3) . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C33 H33A 109.5 . . ? C29 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C29 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N3 C35 H35A 109.5 . . ? N3 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N3 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N3 C36 H36A 109.5 . . ? N3 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N3 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N4 C37 H37A 109.5 . . ? N4 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N4 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N4 C38 H38A 109.5 . . ? N4 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N4 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N5 C39 H39A 109.5 . . ? N5 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N5 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N5 C40 H40A 109.5 . . ? N5 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N5 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Ta1 O1 C15 -172.08(17) . . . . ? N3 Ta1 O1 C15 21.9(3) . . . . ? N4 Ta1 O1 C15 93.73(18) . . . . ? O2 Ta1 O1 C15 -80.03(17) . . . . ? N1 Ta1 O1 C15 -3.47(16) . . . . ? N5 Ta1 O2 C25 -142.7(3) . . . . ? N3 Ta1 O2 C25 -31.0(3) . . . . ? N4 Ta1 O2 C25 68.9(7) . . . . ? O1 Ta1 O2 C25 129.4(3) . . . . ? N1 Ta1 O2 C25 71.8(3) . . . . ? C15 Ta1 O2 C25 100.9(3) . . . . ? N5 Ta1 N1 C15 23.3(3) . . . . ? N3 Ta1 N1 C15 -167.94(17) . . . . ? N4 Ta1 N1 C15 -78.87(18) . . . . ? O2 Ta1 N1 C15 101.49(18) . . . . ? O1 Ta1 N1 C15 3.39(15) . . . . ? N5 Ta1 N1 C2 -143.4(3) . . . . ? N3 Ta1 N1 C2 25.3(3) . . . . ? N4 Ta1 N1 C2 114.4(3) . . . . ? O2 Ta1 N1 C2 -65.2(3) . . . . ? O1 Ta1 N1 C2 -163.3(3) . . . . ? C15 Ta1 N1 C2 -166.7(4) . . . . ? N5 Ta1 N3 C36 160.4(2) . . . . ? N4 Ta1 N3 C36 -106.0(3) . . . . ? O2 Ta1 N3 C36 67.0(2) . . . . ? O1 Ta1 N3 C36 -34.7(4) . . . . ? N1 Ta1 N3 C36 -12.6(3) . . . . ? C15 Ta1 N3 C36 -20.6(3) . . . . ? N5 Ta1 N3 C35 -25.9(3) . . . . ? N4 Ta1 N3 C35 67.8(3) . . . . ? O2 Ta1 N3 C35 -119.3(3) . . . . ? O1 Ta1 N3 C35 139.1(3) . . . . ? N1 Ta1 N3 C35 161.1(3) . . . . ? C15 Ta1 N3 C35 153.1(3) . . . . ? N5 Ta1 N4 C38 140.2(3) . . . . ? N3 Ta1 N4 C38 28.7(3) . . . . ? O2 Ta1 N4 C38 -71.4(7) . . . . ? O1 Ta1 N4 C38 -132.3(3) . . . . ? N1 Ta1 N4 C38 -74.3(3) . . . . ? C15 Ta1 N4 C38 -103.4(3) . . . . ? N5 Ta1 N4 C37 -51.3(3) . . . . ? N3 Ta1 N4 C37 -162.9(3) . . . . ? O2 Ta1 N4 C37 97.0(7) . . . . ? O1 Ta1 N4 C37 36.1(3) . . . . ? N1 Ta1 N4 C37 94.2(3) . . . . ? C15 Ta1 N4 C37 65.1(3) . . . . ? N3 Ta1 N5 C40 59.9(3) . . . . ? N4 Ta1 N5 C40 -29.8(3) . . . . ? O2 Ta1 N5 C40 154.0(3) . . . . ? O1 Ta1 N5 C40 -115.0(3) . . . . ? N1 Ta1 N5 C40 -131.9(3) . . . . ? C15 Ta1 N5 C40 -119.2(3) . . . . ? N3 Ta1 N5 C39 -131.4(2) . . . . ? N4 Ta1 N5 C39 138.9(2) . . . . ? O2 Ta1 N5 C39 -37.4(2) . . . . ? O1 Ta1 N5 C39 53.7(2) . . . . ? N1 Ta1 N5 C39 36.8(3) . . . . ? C15 Ta1 N5 C39 49.4(2) . . . . ? C6 C1 C2 C3 0.7(4) . . . . ? C8 C1 C2 C3 -179.6(3) . . . . ? C6 C1 C2 N1 -171.8(3) . . . . ? C8 C1 C2 N1 7.8(4) . . . . ? C15 N1 C2 C1 -64.6(4) . . . . ? Ta1 N1 C2 C1 98.4(3) . . . . ? C15 N1 C2 C3 122.7(3) . . . . ? Ta1 N1 C2 C3 -74.3(4) . . . . ? C1 C2 C3 C4 1.3(4) . . . . ? N1 C2 C3 C4 174.1(3) . . . . ? C2 C3 C4 C5 -2.0(4) . . . . ? C3 C4 C5 C6 0.8(5) . . . . ? C4 C5 C6 C1 1.3(4) . . . . ? C4 C5 C6 C7 -176.7(3) . . . . ? C2 C1 C6 C5 -2.0(4) . . . . ? C8 C1 C6 C5 178.4(3) . . . . ? C2 C1 C6 C7 175.9(3) . . . . ? C8 C1 C6 C7 -3.7(4) . . . . ? C2 C1 C8 C9 -85.1(4) . . . . ? C6 C1 C8 C9 94.6(3) . . . . ? C2 C1 C8 C13 103.4(3) . . . . ? C6 C1 C8 C13 -77.0(4) . . . . ? C25 N2 C9 C10 -102.6(3) . . . . ? C25 N2 C9 C8 87.4(4) . . . . ? C13 C8 C9 C10 -1.4(4) . . . . ? C1 C8 C9 C10 -172.9(3) . . . . ? C13 C8 C9 N2 168.4(3) . . . . ? C1 C8 C9 N2 -3.2(4) . . . . ? N2 C9 C10 C11 -169.4(3) . . . . ? C8 C9 C10 C11 0.9(4) . . . . ? C9 C10 C11 C12 0.3(5) . . . . ? C10 C11 C12 C13 -1.0(5) . . . . ? C11 C12 C13 C8 0.4(5) . . . . ? C11 C12 C13 C14 176.9(3) . . . . ? C9 C8 C13 C12 0.8(4) . . . . ? C1 C8 C13 C12 172.5(3) . . . . ? C9 C8 C13 C14 -175.6(3) . . . . ? C1 C8 C13 C14 -3.9(4) . . . . ? Ta1 O1 C15 N1 5.6(3) . . . . ? Ta1 O1 C15 C16 -168.2(2) . . . . ? C2 N1 C15 O1 163.7(3) . . . . ? Ta1 N1 C15 O1 -5.3(2) . . . . ? C2 N1 C15 C16 -23.4(5) . . . . ? Ta1 N1 C15 C16 167.6(3) . . . . ? C2 N1 C15 Ta1 169.0(3) . . . . ? N5 Ta1 C15 O1 8.85(19) . . . . ? N3 Ta1 C15 O1 -170.11(16) . . . . ? N4 Ta1 C15 O1 -84.48(18) . . . . ? O2 Ta1 C15 O1 99.30(17) . . . . ? N1 Ta1 C15 O1 174.0(3) . . . . ? N5 Ta1 C15 N1 -165.17(16) . . . . ? N3 Ta1 C15 N1 15.9(2) . . . . ? N4 Ta1 C15 N1 101.50(18) . . . . ? O2 Ta1 C15 N1 -74.72(17) . . . . ? O1 Ta1 C15 N1 -174.0(3) . . . . ? N5 Ta1 C15 C16 64.7(9) . . . . ? N3 Ta1 C15 C16 -114.3(9) . . . . ? N4 Ta1 C15 C16 -28.7(9) . . . . ? O2 Ta1 C15 C16 155.1(9) . . . . ? O1 Ta1 C15 C16 55.8(9) . . . . ? N1 Ta1 C15 C16 -130.1(10) . . . . ? O1 C15 C16 C21 -51.7(4) . . . . ? N1 C15 C16 C21 135.7(3) . . . . ? Ta1 C15 C16 C21 -101.2(9) . . . . ? O1 C15 C16 C17 120.2(3) . . . . ? N1 C15 C16 C17 -52.4(4) . . . . ? Ta1 C15 C16 C17 70.6(10) . . . . ? C21 C16 C17 C18 -3.1(4) . . . . ? C15 C16 C17 C18 -174.9(3) . . . . ? C21 C16 C17 C22 172.3(3) . . . . ? C15 C16 C17 C22 0.5(5) . . . . ? C16 C17 C18 C19 1.0(5) . . . . ? C22 C17 C18 C19 -174.6(3) . . . . ? C17 C18 C19 C20 0.3(5) . . . . ? C17 C18 C19 C23 178.4(3) . . . . ? C18 C19 C20 C21 0.6(5) . . . . ? C23 C19 C20 C21 -177.5(3) . . . . ? C19 C20 C21 C16 -2.6(5) . . . . ? C19 C20 C21 C24 175.7(3) . . . . ? C17 C16 C21 C20 3.9(4) . . . . ? C15 C16 C21 C20 175.7(3) . . . . ? C17 C16 C21 C24 -174.4(3) . . . . ? C15 C16 C21 C24 -2.5(4) . . . . ? C9 N2 C25 O2 0.9(4) . . . . ? C9 N2 C25 C26 179.8(2) . . . . ? Ta1 O2 C25 N2 -117.6(3) . . . . ? Ta1 O2 C25 C26 63.6(4) . . . . ? N2 C25 C26 C31 42.0(4) . . . . ? O2 C25 C26 C31 -139.1(3) . . . . ? N2 C25 C26 C27 -137.2(3) . . . . ? O2 C25 C26 C27 41.7(4) . . . . ? C31 C26 C27 C28 1.0(4) . . . . ? C25 C26 C27 C28 -179.8(2) . . . . ? C31 C26 C27 C32 -176.3(3) . . . . ? C25 C26 C27 C32 2.9(4) . . . . ? C26 C27 C28 C29 -1.0(4) . . . . ? C32 C27 C28 C29 176.5(3) . . . . ? C27 C28 C29 C30 1.0(4) . . . . ? C27 C28 C29 C33 -176.9(3) . . . . ? C28 C29 C30 C31 -1.0(4) . . . . ? C33 C29 C30 C31 176.8(3) . . . . ? C29 C30 C31 C26 1.1(4) . . . . ? C29 C30 C31 C34 180.0(3) . . . . ? C27 C26 C31 C30 -1.1(4) . . . . ? C25 C26 C31 C30 179.7(3) . . . . ? C27 C26 C31 C34 -179.9(3) . . . . ? C25 C26 C31 C34 0.9(4) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 27.89 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 3.181 _refine_diff_density_min -2.665 _refine_diff_density_rms 0.201 # Attachment 'compound-10.cif.txt' data_compound10 _database_code_depnum_ccdc_archive 'CCDC 775663' #TrackingRef 'compound-10.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C21 H23 N O' _chemical_formula_sum 'C21 H23 N O' _chemical_formula_weight 305.40 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.388(16) _cell_length_b 9.44(2) _cell_length_c 9.484(17) _cell_angle_alpha 88.28(9) _cell_angle_beta 81.19(5) _cell_angle_gamma 89.14(9) _cell_volume 830(3) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 581 _cell_measurement_theta_min 4.7 _cell_measurement_theta_max 45.7 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 328 _exptl_absorpt_coefficient_mu 0.574 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8842 _exptl_absorpt_correction_T_max 0.9343 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Rigaku Saturn70 CCD camera' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 11805 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0485 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 4.69 _diffrn_reflns_theta_max 72.54 _reflns_number_total 4974 _reflns_number_gt 4582 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r4' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure 4.0' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2009)' _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^)+(0.0661P)^2^+0.1704P] 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 0.2(3) _refine_ls_number_reflns 4974 _refine_ls_number_parameters 415 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0457 _refine_ls_R_factor_gt 0.0420 _refine_ls_wR_factor_ref 0.1280 _refine_ls_wR_factor_gt 0.1115 _refine_ls_goodness_of_fit_ref 1.123 _refine_ls_restrained_S_all 1.123 _refine_ls_shift/su_max 0.003 _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 O1 O 0.2049(2) 0.2271(2) 0.7636(2) 0.0358(5) Uani 1 1 d . . . N2 N 0.8664(2) 0.7337(2) 0.3480(2) 0.0240(5) Uani 1 1 d . . . O2 O 0.6437(2) 0.7258(2) 0.2831(2) 0.0415(5) Uani 1 1 d . . . N1 N 0.2380(2) 0.2312(2) 0.9962(2) 0.0232(5) Uani 1 1 d . . . C5 C 0.1590(3) 0.4479(3) 0.8749(3) 0.0228(5) Uani 1 1 d . . . C6 C 0.3801(3) 0.4167(3) 1.0837(3) 0.0255(5) Uani 1 1 d . . . H6 H 0.4254 0.4359 0.9886 0.031 Uiso 1 1 calc R . . C7 C 0.9424(3) 0.9175(3) 0.4998(3) 0.0297(6) Uani 1 1 d . . . H7 H 0.8444 0.9331 0.5393 0.036 Uiso 1 1 calc R . . C8 C 0.2775(3) 0.3106(3) 1.1107(3) 0.0230(5) Uani 1 1 d . . . C9 C 0.8658(3) 1.1490(3) 0.1207(3) 0.0316(6) Uani 1 1 d . . . H9 H 0.9454 1.1885 0.0588 0.038 Uiso 1 1 calc R . . C10 C 0.7505(3) 0.7953(3) 0.2997(3) 0.0287(6) Uani 1 1 d . . . C11 C 0.9783(3) 0.8149(3) 0.3967(3) 0.0248(5) Uani 1 1 d . . . C12 C 0.1973(3) 0.5312(3) 0.7517(3) 0.0291(6) Uani 1 1 d . . . H12 H 0.2602 0.4938 0.6733 0.035 Uiso 1 1 calc R . . C13 C 0.4169(3) 0.4948(3) 1.1936(3) 0.0303(6) Uani 1 1 d . . . H13 H 0.4855 0.5685 1.1736 0.036 Uiso 1 1 calc R . . C14 C 0.2155(3) 0.2803(3) 1.2517(3) 0.0269(6) Uani 1 1 d . . . H14 H 0.1470 0.2065 1.2722 0.032 Uiso 1 1 calc R . . C15 C 0.0478(3) 0.7220(3) 0.8541(3) 0.0327(6) Uani 1 1 d . . . H15 H 0.0100 0.8154 0.8465 0.039 Uiso 1 1 calc R . . C16 C 0.4027(3) 0.0174(3) 0.9919(3) 0.0247(5) Uani 1 1 d . . . H16 H 0.4534 0.0620 1.0645 0.030 Uiso 1 1 calc R . . C17 C 1.1219(3) 0.7897(3) 0.3420(3) 0.0283(6) Uani 1 1 d . . . H17 H 1.1471 0.7195 0.2725 0.034 Uiso 1 1 calc R . . C18 C 0.0626(3) 0.5030(3) 0.9872(3) 0.0266(6) Uani 1 1 d . . . H18 H 0.0350 0.4470 1.0716 0.032 Uiso 1 1 calc R . . C19 C 0.6538(3) -0.1553(3) 0.8921(3) 0.0386(7) Uani 1 1 d . . . H19A H 0.7246 -0.2048 0.8216 0.046 Uiso 1 1 calc R . . H19B H 0.6776 -0.1751 0.9890 0.046 Uiso 1 1 calc R . . C20 C 0.6274(3) 1.1728(3) 0.2514(3) 0.0336(6) Uani 1 1 d . . . H20 H 0.5442 1.2294 0.2806 0.040 Uiso 1 1 calc R . . C21 C 0.6315(3) 1.0321(3) 0.2970(3) 0.0326(6) Uani 1 1 d . . . H21 H 0.5501 0.9918 0.3556 0.039 Uiso 1 1 calc R . . C22 C 0.7549(3) 0.9495(3) 0.2571(3) 0.0277(6) Uani 1 1 d . . . C23 C 0.4033(3) -0.1463(3) 1.0153(3) 0.0314(6) Uani 1 1 d . . . H23A H 0.4436 -0.1737 1.1029 0.038 Uiso 1 1 calc R . . H23B H 0.3047 -0.1844 1.0230 0.038 Uiso 1 1 calc R . . C24 C 1.0495(3) 0.9963(3) 0.5445(3) 0.0327(6) Uani 1 1 d . . . H24 H 1.0248 1.0674 0.6131 0.039 Uiso 1 1 calc R . . C25 C 0.2493(3) 0.0752(3) 1.0049(3) 0.0258(5) Uani 1 1 d . . . H25A H 0.2026 0.0356 0.9282 0.031 Uiso 1 1 calc R . . H25B H 0.1950 0.0415 1.0974 0.031 Uiso 1 1 calc R . . C26 C 0.3532(3) 0.4651(3) 1.3336(3) 0.0331(6) Uani 1 1 d . . . H26 H 0.3779 0.5185 1.4095 0.040 Uiso 1 1 calc R . . C27 C 0.8379(3) 0.5355(3) 0.5294(3) 0.0326(6) Uani 1 1 d . . . H27 H 0.9100 0.5793 0.5818 0.039 Uiso 1 1 calc R . . C28 C 0.7446(3) 1.2310(3) 0.1632(3) 0.0340(6) Uani 1 1 d . . . H28 H 0.7416 1.3275 0.1319 0.041 Uiso 1 1 calc R . . C29 C 0.2056(3) 0.2947(3) 0.8727(3) 0.0262(6) Uani 1 1 d . . . C30 C 0.6514(3) 0.0065(3) 0.8580(3) 0.0344(6) Uani 1 1 d . . . H30A H 0.6801 0.0608 0.9367 0.041 Uiso 1 1 calc R . . H30B H 0.7165 0.0306 0.7685 0.041 Uiso 1 1 calc R . . C31 C 0.2538(3) 0.3574(3) 1.3614(3) 0.0312(6) Uani 1 1 d . . . H31 H 0.2114 0.3361 1.4571 0.037 Uiso 1 1 calc R . . C32 C 0.8715(3) 1.0085(3) 0.1686(3) 0.0287(6) Uani 1 1 d . . . H32 H 0.9556 0.9528 0.1406 0.034 Uiso 1 1 calc R . . C33 C 0.8378(3) 0.3747(3) 0.5575(4) 0.0432(8) Uani 1 1 d . . . H33 H 0.9080 0.3195 0.4896 0.052 Uiso 1 1 calc R . . C34 C 1.2284(3) 0.8678(3) 0.3895(3) 0.0363(7) Uani 1 1 d . . . H34 H 1.3268 0.8497 0.3531 0.044 Uiso 1 1 calc R . . C35 C 0.8714(3) 0.5790(3) 0.3715(3) 0.0301(6) Uani 1 1 d . . . H35A H 0.9685 0.5430 0.3321 0.036 Uiso 1 1 calc R . . H35B H 0.8009 0.5346 0.3194 0.036 Uiso 1 1 calc R . . C36 C 0.0067(3) 0.6392(3) 0.9762(3) 0.0310(6) Uani 1 1 d . . . H36 H -0.0598 0.6757 1.0526 0.037 Uiso 1 1 calc R . . C37 C 0.4940(3) 0.0361(3) 0.8425(3) 0.0277(6) Uani 1 1 d . . . H37 H 0.4769 0.1276 0.7914 0.033 Uiso 1 1 calc R . . C38 C 1.1932(3) 0.9713(3) 0.4891(3) 0.0370(7) Uani 1 1 d . . . H38 H 1.2669 1.0253 0.5197 0.044 Uiso 1 1 calc R . . C39 C 0.1445(3) 0.6678(3) 0.7428(3) 0.0325(6) Uani 1 1 d . . . H39 H 0.1746 0.7252 0.6599 0.039 Uiso 1 1 calc R . . C40 C 0.4572(3) -0.0964(3) 0.7672(3) 0.0301(6) Uani 1 1 d . . . H40A H 0.5175 -0.1077 0.6729 0.036 Uiso 1 1 calc R . . H40B H 0.3537 -0.1011 0.7580 0.036 Uiso 1 1 calc R . . C41 C 0.6236(3) 0.4411(4) 0.6706(4) 0.0491(9) Uani 1 1 d . . . H41 H 0.5162 0.4422 0.6965 0.059 Uiso 1 1 calc R . . C42 C 0.7028(4) 0.3995(4) 0.7928(3) 0.0434(8) Uani 1 1 d . . . H42A H 0.6531 0.3220 0.8526 0.052 Uiso 1 1 calc R . . H42B H 0.7128 0.4814 0.8533 0.052 Uiso 1 1 calc R . . C43 C 0.8496(4) 0.3502(5) 0.7155(4) 0.0598(12) Uani 1 1 d . . . H43A H 0.9284 0.4068 0.7429 0.072 Uiso 1 1 calc R . . H43B H 0.8671 0.2487 0.7373 0.072 Uiso 1 1 calc R . . C44 C 0.4996(3) -0.2002(3) 0.8822(3) 0.0320(6) Uani 1 1 d . . . H44 H 0.4884 -0.3028 0.8631 0.038 Uiso 1 1 calc R . . C45 C 0.6859(4) 0.5787(4) 0.5989(4) 0.0557(11) Uani 1 1 d . . . H45A H 0.6895 0.6527 0.6700 0.067 Uiso 1 1 calc R . . H45B H 0.6279 0.6145 0.5263 0.067 Uiso 1 1 calc R . . C46 C 0.6793(4) 0.3392(4) 0.5589(3) 0.0513(9) Uani 1 1 d . . . H46A H 0.6462 0.3617 0.4665 0.062 Uiso 1 1 calc R . . H46B H 0.6569 0.2396 0.5888 0.062 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 O1 0.0447(11) 0.0354(11) 0.0294(10) -0.0085(8) -0.0117(8) 0.0104(9) N2 0.0248(11) 0.0232(11) 0.0254(10) -0.0018(8) -0.0076(8) -0.0034(9) O2 0.0411(12) 0.0356(12) 0.0520(12) 0.0067(10) -0.0210(9) -0.0141(9) N1 0.0262(11) 0.0208(11) 0.0232(10) -0.0017(8) -0.0056(8) 0.0024(9) C5 0.0247(12) 0.0244(13) 0.0211(11) 0.0006(9) -0.0092(9) -0.0009(10) C6 0.0306(13) 0.0220(12) 0.0254(12) 0.0020(10) -0.0093(10) 0.0009(10) C7 0.0333(14) 0.0279(14) 0.0285(12) -0.0010(11) -0.0070(11) 0.0042(11) C8 0.0255(12) 0.0189(11) 0.0252(11) -0.0005(9) -0.0064(9) 0.0050(9) C9 0.0332(14) 0.0268(15) 0.0355(14) 0.0073(11) -0.0088(11) -0.0056(11) C10 0.0325(14) 0.0275(14) 0.0265(12) -0.0006(10) -0.0058(10) -0.0050(11) C11 0.0320(13) 0.0190(12) 0.0231(11) 0.0047(9) -0.0039(10) -0.0023(10) C12 0.0320(13) 0.0340(15) 0.0230(12) 0.0005(11) -0.0090(10) -0.0058(11) C13 0.0357(14) 0.0178(12) 0.0397(14) -0.0021(11) -0.0128(12) 0.0025(11) C14 0.0261(13) 0.0274(13) 0.0262(12) 0.0027(10) -0.0019(10) 0.0024(11) C15 0.0380(15) 0.0228(13) 0.0402(15) 0.0042(11) -0.0161(12) 0.0016(11) C16 0.0272(12) 0.0224(13) 0.0251(12) -0.0018(10) -0.0059(10) 0.0007(10) C17 0.0274(13) 0.0331(14) 0.0247(12) 0.0026(10) -0.0056(10) -0.0013(11) C18 0.0297(13) 0.0261(13) 0.0247(12) 0.0027(10) -0.0072(10) 0.0003(11) C19 0.0334(15) 0.0401(17) 0.0440(17) -0.0079(13) -0.0114(13) 0.0115(13) C20 0.0305(14) 0.0358(16) 0.0386(15) -0.0101(12) -0.0167(11) 0.0077(12) C21 0.0307(14) 0.0372(16) 0.0313(14) -0.0028(12) -0.0094(11) 0.0014(12) C22 0.0332(14) 0.0249(14) 0.0273(12) -0.0023(10) -0.0113(10) -0.0028(11) C23 0.0379(15) 0.0262(14) 0.0285(13) 0.0016(10) -0.0014(11) 0.0076(11) C24 0.0439(16) 0.0266(14) 0.0316(13) -0.0011(11) -0.0179(12) -0.0026(12) C25 0.0256(12) 0.0202(12) 0.0311(13) -0.0009(10) -0.0029(10) 0.0004(10) C26 0.0429(15) 0.0297(14) 0.0302(13) -0.0075(11) -0.0166(11) 0.0097(12) C27 0.0441(16) 0.0276(14) 0.0284(13) 0.0018(11) -0.0128(11) -0.0082(12) C28 0.0394(15) 0.0251(14) 0.0418(15) -0.0023(12) -0.0196(12) 0.0007(12) C29 0.0251(12) 0.0297(14) 0.0236(12) -0.0036(10) -0.0035(10) 0.0035(10) C30 0.0251(14) 0.0359(16) 0.0428(15) -0.0084(12) -0.0061(11) -0.0012(11) C31 0.0354(14) 0.0370(15) 0.0218(12) -0.0024(10) -0.0070(10) 0.0075(12) C32 0.0265(13) 0.0271(14) 0.0336(13) -0.0005(11) -0.0081(11) 0.0008(11) C33 0.0401(17) 0.0341(16) 0.0482(18) 0.0085(14) 0.0132(14) 0.0095(13) C34 0.0330(15) 0.0440(17) 0.0318(14) 0.0125(13) -0.0062(11) -0.0047(12) C35 0.0351(14) 0.0239(14) 0.0301(13) -0.0023(11) -0.0013(11) -0.0021(11) C36 0.0297(14) 0.0319(15) 0.0323(13) -0.0012(11) -0.0079(11) 0.0057(11) C37 0.0284(13) 0.0254(13) 0.0299(12) -0.0003(10) -0.0061(10) -0.0007(10) C38 0.0493(18) 0.0317(15) 0.0338(14) 0.0111(12) -0.0198(13) -0.0121(13) C39 0.0374(15) 0.0316(14) 0.0305(13) 0.0086(11) -0.0127(11) -0.0083(12) C40 0.0299(13) 0.0363(15) 0.0242(13) -0.0036(11) -0.0048(10) 0.0032(11) C41 0.0297(15) 0.070(2) 0.0434(17) 0.0164(17) 0.0033(13) 0.0122(15) C42 0.063(2) 0.0420(18) 0.0258(14) 0.0004(12) -0.0069(13) -0.0090(15) C43 0.0355(17) 0.068(3) 0.076(3) 0.041(2) -0.0182(16) -0.0107(16) C44 0.0419(15) 0.0205(13) 0.0333(14) -0.0028(11) -0.0046(12) 0.0040(12) C45 0.077(3) 0.047(2) 0.0346(16) 0.0073(15) 0.0167(16) 0.0224(19) C46 0.061(2) 0.064(2) 0.0299(15) -0.0011(15) -0.0072(14) -0.0346(18) _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 O1 C29 1.233(4) . ? N2 C10 1.360(4) . ? N2 C11 1.449(4) . ? N2 C35 1.471(4) . ? O2 C10 1.238(4) . ? N1 C29 1.373(4) . ? N1 C8 1.435(4) . ? N1 C25 1.475(4) . ? C5 C12 1.391(4) . ? C5 C18 1.396(4) . ? C5 C29 1.504(5) . ? C6 C13 1.383(5) . ? C6 C8 1.391(4) . ? C6 H6 0.9500 . ? C7 C24 1.384(5) . ? C7 C11 1.398(4) . ? C7 H7 0.9500 . ? C8 C14 1.398(4) . ? C9 C28 1.382(4) . ? C9 C32 1.391(5) . ? C9 H9 0.9500 . ? C10 C22 1.498(5) . ? C11 C17 1.388(4) . ? C12 C39 1.378(5) . ? C12 H12 0.9500 . ? C13 C26 1.392(5) . ? C13 H13 0.9500 . ? C14 C31 1.382(5) . ? C14 H14 0.9500 . ? C15 C36 1.385(4) . ? C15 C39 1.387(5) . ? C15 H15 0.9500 . ? C16 C25 1.521(4) . ? C16 C37 1.546(4) . ? C16 C23 1.554(5) . ? C16 H16 1.0000 . ? C17 C34 1.388(5) . ? C17 H17 0.9500 . ? C18 C36 1.388(4) . ? C18 H18 0.9500 . ? C19 C44 1.532(5) . ? C19 C30 1.551(5) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.386(5) . ? C20 C28 1.386(5) . ? C20 H20 0.9500 . ? C21 C22 1.397(4) . ? C21 H21 0.9500 . ? C22 C32 1.386(4) . ? C23 C44 1.531(4) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C38 1.390(5) . ? C24 H24 0.9500 . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C26 C31 1.382(5) . ? C26 H26 0.9500 . ? C27 C35 1.526(4) . ? C27 C45 1.532(5) . ? C27 C33 1.533(5) . ? C27 H27 1.0000 . ? C28 H28 0.9500 . ? C30 C37 1.528(4) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C46 1.528(6) . ? C33 C43 1.530(6) . ? C33 H33 1.0000 . ? C34 C38 1.381(5) . ? C34 H34 0.9500 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36 0.9500 . ? C37 C40 1.528(5) . ? C37 H37 1.0000 . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C44 1.538(4) . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C46 1.482(6) . ? C41 C42 1.509(5) . ? C41 C45 1.529(6) . ? C41 H41 1.0000 . ? C42 C43 1.531(6) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 H44 1.0000 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? 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 C10 N2 C11 122.7(2) . . ? C10 N2 C35 119.8(2) . . ? C11 N2 C35 116.9(2) . . ? C29 N1 C8 122.5(2) . . ? C29 N1 C25 118.7(2) . . ? C8 N1 C25 118.3(2) . . ? C12 C5 C18 119.0(3) . . ? C12 C5 C29 118.1(2) . . ? C18 C5 C29 122.2(2) . . ? C13 C6 C8 120.8(3) . . ? C13 C6 H6 119.6 . . ? C8 C6 H6 119.6 . . ? C24 C7 C11 120.1(3) . . ? C24 C7 H7 120.0 . . ? C11 C7 H7 120.0 . . ? C6 C8 C14 118.9(3) . . ? C6 C8 N1 120.7(2) . . ? C14 C8 N1 120.4(3) . . ? C28 C9 C32 120.0(3) . . ? C28 C9 H9 120.0 . . ? C32 C9 H9 120.0 . . ? O2 C10 N2 121.8(3) . . ? O2 C10 C22 118.7(3) . . ? N2 C10 C22 119.4(3) . . ? C17 C11 C7 119.8(3) . . ? C17 C11 N2 119.9(3) . . ? C7 C11 N2 120.2(2) . . ? C39 C12 C5 120.4(3) . . ? C39 C12 H12 119.8 . . ? C5 C12 H12 119.8 . . ? C6 C13 C26 119.9(3) . . ? C6 C13 H13 120.1 . . ? C26 C13 H13 120.1 . . ? C31 C14 C8 120.1(3) . . ? C31 C14 H14 120.0 . . ? C8 C14 H14 120.0 . . ? C36 C15 C39 119.6(3) . . ? C36 C15 H15 120.2 . . ? C39 C15 H15 120.2 . . ? C25 C16 C37 115.3(2) . . ? C25 C16 C23 110.8(2) . . ? C37 C16 C23 102.2(2) . . ? C25 C16 H16 109.4 . . ? C37 C16 H16 109.4 . . ? C23 C16 H16 109.4 . . ? C34 C17 C11 119.5(3) . . ? C34 C17 H17 120.2 . . ? C11 C17 H17 120.2 . . ? C36 C18 C5 120.3(2) . . ? C36 C18 H18 119.8 . . ? C5 C18 H18 119.8 . . ? C44 C19 C30 103.2(2) . . ? C44 C19 H19A 111.1 . . ? C30 C19 H19A 111.1 . . ? C44 C19 H19B 111.1 . . ? C30 C19 H19B 111.1 . . ? H19A C19 H19B 109.1 . . ? C21 C20 C28 120.1(3) . . ? C21 C20 H20 120.0 . . ? C28 C20 H20 120.0 . . ? C20 C21 C22 120.1(3) . . ? C20 C21 H21 119.9 . . ? C22 C21 H21 119.9 . . ? C32 C22 C21 119.4(3) . . ? C32 C22 C10 122.1(2) . . ? C21 C22 C10 118.2(3) . . ? C44 C23 C16 104.0(2) . . ? C44 C23 H23A 111.0 . . ? C16 C23 H23A 111.0 . . ? C44 C23 H23B 111.0 . . ? C16 C23 H23B 111.0 . . ? H23A C23 H23B 109.0 . . ? C7 C24 C38 120.0(3) . . ? C7 C24 H24 120.0 . . ? C38 C24 H24 120.0 . . ? N1 C25 C16 114.5(2) . . ? N1 C25 H25A 108.6 . . ? C16 C25 H25A 108.6 . . ? N1 C25 H25B 108.6 . . ? C16 C25 H25B 108.6 . . ? H25A C25 H25B 107.6 . . ? C31 C26 C13 119.6(3) . . ? C31 C26 H26 120.2 . . ? C13 C26 H26 120.2 . . ? C35 C27 C45 113.3(2) . . ? C35 C27 C33 113.8(3) . . ? C45 C27 C33 102.1(3) . . ? C35 C27 H27 109.1 . . ? C45 C27 H27 109.1 . . ? C33 C27 H27 109.1 . . ? C9 C28 C20 120.1(3) . . ? C9 C28 H28 120.0 . . ? C20 C28 H28 120.0 . . ? O1 C29 N1 121.7(3) . . ? O1 C29 C5 119.5(2) . . ? N1 C29 C5 118.7(2) . . ? C37 C30 C19 103.1(2) . . ? C37 C30 H30A 111.1 . . ? C19 C30 H30A 111.1 . . ? C37 C30 H30B 111.1 . . ? C19 C30 H30B 111.1 . . ? H30A C30 H30B 109.1 . . ? C14 C31 C26 120.7(3) . . ? C14 C31 H31 119.6 . . ? C26 C31 H31 119.6 . . ? C22 C32 C9 120.3(3) . . ? C22 C32 H32 119.9 . . ? C9 C32 H32 119.9 . . ? C46 C33 C43 100.3(2) . . ? C46 C33 C27 101.9(3) . . ? C43 C33 C27 106.9(3) . . ? C46 C33 H33 115.3 . . ? C43 C33 H33 115.3 . . ? C27 C33 H33 115.3 . . ? C38 C34 C17 120.8(3) . . ? C38 C34 H34 119.6 . . ? C17 C34 H34 119.6 . . ? N2 C35 C27 112.4(2) . . ? N2 C35 H35A 109.1 . . ? C27 C35 H35A 109.1 . . ? N2 C35 H35B 109.1 . . ? C27 C35 H35B 109.1 . . ? H35A C35 H35B 107.9 . . ? C15 C36 C18 120.1(3) . . ? C15 C36 H36 120.0 . . ? C18 C36 H36 120.0 . . ? C40 C37 C30 101.4(2) . . ? C40 C37 C16 102.5(2) . . ? C30 C37 C16 107.7(2) . . ? C40 C37 H37 114.6 . . ? C30 C37 H37 114.6 . . ? C16 C37 H37 114.6 . . ? C34 C38 C24 119.7(3) . . ? C34 C38 H38 120.1 . . ? C24 C38 H38 120.1 . . ? C12 C39 C15 120.5(3) . . ? C12 C39 H39 119.8 . . ? C15 C39 H39 119.8 . . ? C37 C40 C44 94.5(3) . . ? C37 C40 H40A 112.8 . . ? C44 C40 H40A 112.8 . . ? C37 C40 H40B 112.8 . . ? C44 C40 H40B 112.8 . . ? H40A C40 H40B 110.3 . . ? C46 C41 C42 103.6(3) . . ? C46 C41 C45 99.9(3) . . ? C42 C41 C45 109.6(4) . . ? C46 C41 H41 114.1 . . ? C42 C41 H41 114.1 . . ? C45 C41 H41 114.1 . . ? C41 C42 C43 102.5(3) . . ? C41 C42 H42A 111.3 . . ? C43 C42 H42A 111.3 . . ? C41 C42 H42B 111.3 . . ? C43 C42 H42B 111.3 . . ? H42A C42 H42B 109.2 . . ? C33 C43 C42 103.7(3) . . ? C33 C43 H43A 111.0 . . ? C42 C43 H43A 111.0 . . ? C33 C43 H43B 111.0 . . ? C42 C43 H43B 111.0 . . ? H43A C43 H43B 109.0 . . ? C23 C44 C19 107.0(3) . . ? C23 C44 C40 100.8(2) . . ? C19 C44 C40 102.4(2) . . ? C23 C44 H44 115.0 . . ? C19 C44 H44 115.0 . . ? C40 C44 H44 115.0 . . ? C41 C45 C27 103.7(3) . . ? C41 C45 H45A 111.0 . . ? C27 C45 H45A 111.0 . . ? C41 C45 H45B 111.0 . . ? C27 C45 H45B 111.0 . . ? H45A C45 H45B 109.0 . . ? C41 C46 C33 95.0(3) . . ? C41 C46 H46A 112.7 . . ? C33 C46 H46A 112.7 . . ? C41 C46 H46B 112.7 . . ? C33 C46 H46B 112.7 . . ? H46A C46 H46B 110.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C13 C6 C8 C14 -2.3(3) . . . . ? C13 C6 C8 N1 179.1(2) . . . . ? C29 N1 C8 C6 -47.5(3) . . . . ? C25 N1 C8 C6 125.2(3) . . . . ? C29 N1 C8 C14 133.9(3) . . . . ? C25 N1 C8 C14 -53.4(3) . . . . ? C11 N2 C10 O2 -166.7(3) . . . . ? C35 N2 C10 O2 4.6(4) . . . . ? C11 N2 C10 C22 17.0(4) . . . . ? C35 N2 C10 C22 -171.7(2) . . . . ? C24 C7 C11 C17 1.7(3) . . . . ? C24 C7 C11 N2 -179.1(2) . . . . ? C10 N2 C11 C17 -128.5(3) . . . . ? C35 N2 C11 C17 59.9(3) . . . . ? C10 N2 C11 C7 52.3(3) . . . . ? C35 N2 C11 C7 -119.3(3) . . . . ? C18 C5 C12 C39 2.2(4) . . . . ? C29 C5 C12 C39 173.0(2) . . . . ? C8 C6 C13 C26 1.4(4) . . . . ? C6 C8 C14 C31 1.5(3) . . . . ? N1 C8 C14 C31 -179.9(2) . . . . ? C7 C11 C17 C34 -0.6(3) . . . . ? N2 C11 C17 C34 -179.8(2) . . . . ? C12 C5 C18 C36 -0.5(4) . . . . ? C29 C5 C18 C36 -170.9(3) . . . . ? C28 C20 C21 C22 1.5(4) . . . . ? C20 C21 C22 C32 -1.7(4) . . . . ? C20 C21 C22 C10 -175.5(3) . . . . ? O2 C10 C22 C32 -128.5(3) . . . . ? N2 C10 C22 C32 47.9(4) . . . . ? O2 C10 C22 C21 45.1(4) . . . . ? N2 C10 C22 C21 -138.4(3) . . . . ? C25 C16 C23 C44 126.1(2) . . . . ? C37 C16 C23 C44 2.8(3) . . . . ? C11 C7 C24 C38 -1.4(4) . . . . ? C29 N1 C25 C16 104.7(3) . . . . ? C8 N1 C25 C16 -68.2(3) . . . . ? C37 C16 C25 N1 -69.5(3) . . . . ? C23 C16 C25 N1 175.1(2) . . . . ? C6 C13 C26 C31 0.2(4) . . . . ? C32 C9 C28 C20 -1.2(5) . . . . ? C21 C20 C28 C9 -0.1(5) . . . . ? C8 N1 C29 O1 162.8(2) . . . . ? C25 N1 C29 O1 -9.8(4) . . . . ? C8 N1 C29 C5 -22.0(3) . . . . ? C25 N1 C29 C5 165.4(2) . . . . ? C12 C5 C29 O1 -37.7(4) . . . . ? C18 C5 C29 O1 132.8(3) . . . . ? C12 C5 C29 N1 147.0(3) . . . . ? C18 C5 C29 N1 -42.5(4) . . . . ? C44 C19 C30 C37 3.6(3) . . . . ? C8 C14 C31 C26 0.1(4) . . . . ? C13 C26 C31 C14 -0.9(4) . . . . ? C21 C22 C32 C9 0.4(4) . . . . ? C10 C22 C32 C9 173.9(3) . . . . ? C28 C9 C32 C22 1.1(4) . . . . ? C35 C27 C33 C46 -92.3(3) . . . . ? C45 C27 C33 C46 30.2(3) . . . . ? C35 C27 C33 C43 162.9(3) . . . . ? C45 C27 C33 C43 -74.6(3) . . . . ? C11 C17 C34 C38 -0.8(4) . . . . ? C10 N2 C35 C27 -103.2(3) . . . . ? C11 N2 C35 C27 68.6(3) . . . . ? C45 C27 C35 N2 62.2(4) . . . . ? C33 C27 C35 N2 178.3(2) . . . . ? C39 C15 C36 C18 0.2(5) . . . . ? C5 C18 C36 C15 -0.7(4) . . . . ? C19 C30 C37 C40 -37.9(3) . . . . ? C19 C30 C37 C16 69.2(3) . . . . ? C25 C16 C37 C40 -87.2(3) . . . . ? C23 C16 C37 C40 33.1(3) . . . . ? C25 C16 C37 C30 166.4(2) . . . . ? C23 C16 C37 C30 -73.4(3) . . . . ? C17 C34 C38 C24 1.1(4) . . . . ? C7 C24 C38 C34 0.0(4) . . . . ? C5 C12 C39 C15 -2.8(4) . . . . ? C36 C15 C39 C12 1.5(5) . . . . ? C30 C37 C40 C44 56.2(2) . . . . ? C16 C37 C40 C44 -55.1(3) . . . . ? C46 C41 C42 C43 33.8(4) . . . . ? C45 C41 C42 C43 -72.1(4) . . . . ? C46 C33 C43 C42 -35.4(4) . . . . ? C27 C33 C43 C42 70.5(4) . . . . ? C41 C42 C43 C33 1.9(4) . . . . ? C16 C23 C44 C19 69.4(3) . . . . ? C16 C23 C44 C40 -37.3(3) . . . . ? C30 C19 C44 C23 -73.7(3) . . . . ? C30 C19 C44 C40 31.8(3) . . . . ? C37 C40 C44 C23 56.3(3) . . . . ? C37 C40 C44 C19 -53.9(2) . . . . ? C46 C41 C45 C27 -40.5(3) . . . . ? C42 C41 C45 C27 67.8(4) . . . . ? C35 C27 C45 C41 128.4(3) . . . . ? C33 C27 C45 C41 5.5(3) . . . . ? C42 C41 C46 C33 -55.1(3) . . . . ? C45 C41 C46 C33 57.9(3) . . . . ? C43 C33 C46 C41 54.8(3) . . . . ? C27 C33 C46 C41 -55.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.938 _diffrn_reflns_theta_full 67.50 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 0.239 _refine_diff_density_min -0.265 _refine_diff_density_rms 0.060 # Attachment '- compound 17.cif' data_compound17 _database_code_depnum_ccdc_archive 'CCDC 791864' #TrackingRef '- compound 17.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H46 N4 O2 V' _chemical_formula_sum 'C38 H46 N4 O2 V' _chemical_formula_weight 641.73 _chemical_absolute_configuration rmad 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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.605(3) _cell_length_b 10.657(2) _cell_length_c 13.937(2) _cell_angle_alpha 90.00 _cell_angle_beta 92.275(14) _cell_angle_gamma 90.00 _cell_volume 1722.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 4168 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.0 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.237 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 682 _exptl_absorpt_coefficient_mu 0.326 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9142 _exptl_absorpt_correction_T_max 0.9258 _exptl_absorpt_process_details Crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8487 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0079 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8487 _reflns_number_gt 8413 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalStructure _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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. The twin crystal was used for data collection and the platon programm was used to create HKL5 data file. So the number of all and unique data are the same. ; _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^)+(0.0986P)^2^+1.9344P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.205(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.08(3) _refine_ls_number_reflns 8487 _refine_ls_number_parameters 422 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0598 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1945 _refine_ls_wR_factor_gt 0.1941 _refine_ls_goodness_of_fit_ref 1.213 _refine_ls_restrained_S_all 1.213 _refine_ls_shift/su_max 0.007 _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 0.22242(6) 1.02334(7) 0.56135(5) 0.0162(2) Uani 1 1 d . . . O1 O 0.1223(3) 0.8612(3) 0.5765(2) 0.0193(7) Uani 1 1 d . . . O2 O 0.3485(3) 1.1553(3) 0.5958(2) 0.0194(7) Uani 1 1 d . . . N1 N 0.1890(3) 0.9540(4) 0.7065(3) 0.0185(8) Uani 1 1 d . . . N2 N 0.3935(3) 0.9566(4) 0.6118(3) 0.0157(8) Uani 1 1 d . . . N3 N 0.2304(3) 0.9947(4) 0.4303(3) 0.0213(9) Uani 1 1 d . . . N4 N 0.1092(3) 1.1458(4) 0.5632(3) 0.0239(9) Uani 1 1 d . . . C1 C 0.3540(4) 0.9115(4) 0.8184(3) 0.0170(9) Uani 1 1 d . . . C2 C 0.2439(4) 0.9661(4) 0.7986(3) 0.0167(9) Uani 1 1 d . . . C3 C 0.1957(4) 1.0463(4) 0.8655(3) 0.0238(11) Uani 1 1 d . . . H3 H 0.1223 1.0827 0.8514 0.029 Uiso 1 1 calc R . . C4 C 0.2534(4) 1.0739(5) 0.9521(3) 0.0271(11) Uani 1 1 d . . . H4 H 0.2177 1.1239 0.9989 0.033 Uiso 1 1 calc R . . C5 C 0.3646(4) 1.0273(6) 0.9695(3) 0.0244(9) Uani 1 1 d . . . H5 H 0.4062 1.0497 1.0270 0.029 Uiso 1 1 calc R . . C6 C 0.4159(4) 0.9480(5) 0.9036(3) 0.0196(9) Uani 1 1 d . . . C7 C 0.5413(4) 0.9094(5) 0.9214(3) 0.0226(10) Uani 1 1 d . . . H7A H 0.5858 0.9813 0.9463 0.034 Uiso 1 1 calc R . . H7B H 0.5732 0.8812 0.8610 0.034 Uiso 1 1 calc R . . H7C H 0.5457 0.8409 0.9683 0.034 Uiso 1 1 calc R . . C8 C 0.4049(4) 0.8169(4) 0.7535(3) 0.0171(9) Uani 1 1 d . . . C9 C 0.4332(4) 0.8463(4) 0.6581(3) 0.0176(9) Uani 1 1 d . . . C10 C 0.4898(4) 0.7565(5) 0.6029(4) 0.0228(10) Uani 1 1 d . . . H10 H 0.5081 0.7761 0.5388 0.027 Uiso 1 1 calc R . . C11 C 0.5190(4) 0.6404(5) 0.6404(4) 0.0261(11) Uani 1 1 d . . . H11 H 0.5613 0.5824 0.6039 0.031 Uiso 1 1 calc R . . C12 C 0.4855(4) 0.6093(5) 0.7324(4) 0.0249(11) Uani 1 1 d . . . H12 H 0.5035 0.5285 0.7575 0.030 Uiso 1 1 calc R . . C13 C 0.4260(4) 0.6944(5) 0.7882(4) 0.0223(10) Uani 1 1 d . . . C14 C 0.3790(4) 0.6532(5) 0.8826(4) 0.0255(11) Uani 1 1 d . . . H14A H 0.3770 0.5613 0.8852 0.038 Uiso 1 1 calc R . . H14B H 0.3008 0.6863 0.8882 0.038 Uiso 1 1 calc R . . H14C H 0.4286 0.6851 0.9356 0.038 Uiso 1 1 calc R . . C15 C 0.1403(4) 0.8540(4) 0.6685(3) 0.0194(9) Uani 1 1 d . . . C16 C 0.1089(4) 0.7384(5) 0.7245(3) 0.0207(10) Uani 1 1 d . . . C17 C 0.1563(4) 0.6224(5) 0.7019(3) 0.0212(10) Uani 1 1 d . . . C18 C 0.1401(4) 0.5222(6) 0.7635(3) 0.0282(10) Uani 1 1 d . . . H18 H 0.1743 0.4437 0.7493 0.034 Uiso 1 1 calc R . . C19 C 0.0751(4) 0.5323(6) 0.8460(3) 0.0304(11) Uani 1 1 d . . . C20 C 0.0203(4) 0.6442(6) 0.8617(4) 0.0310(12) Uani 1 1 d . . . H20 H -0.0282 0.6512 0.9147 0.037 Uiso 1 1 calc R . . C21 C 0.0337(4) 0.7484(5) 0.8017(4) 0.0276(11) Uani 1 1 d . . . C22 C 0.2202(4) 0.6004(5) 0.6126(4) 0.0249(10) Uani 1 1 d . . . H22A H 0.2650 0.5227 0.6193 0.037 Uiso 1 1 calc R . . H22B H 0.2724 0.6710 0.6022 0.037 Uiso 1 1 calc R . . H22C H 0.1651 0.5931 0.5578 0.037 Uiso 1 1 calc R . . C23 C 0.0702(6) 0.4223(7) 0.9145(5) 0.0515(18) Uani 1 1 d . . . H23A H 0.1369 0.4253 0.9599 0.077 Uiso 1 1 calc R . . H23B H 0.0716 0.3437 0.8781 0.077 Uiso 1 1 calc R . . H23C H -0.0009 0.4267 0.9499 0.077 Uiso 1 1 calc R . . C24 C -0.0376(5) 0.8642(6) 0.8173(5) 0.0390(14) Uani 1 1 d . . . H24A H -0.0018 0.9143 0.8694 0.058 Uiso 1 1 calc R . . H24B H -0.1155 0.8396 0.8345 0.058 Uiso 1 1 calc R . . H24C H -0.0420 0.9141 0.7582 0.058 Uiso 1 1 calc R . . C25 C 0.4206(4) 1.0733(5) 0.6333(3) 0.0167(9) Uani 1 1 d . . . C26 C 0.5191(4) 1.1188(4) 0.6976(3) 0.0164(9) Uani 1 1 d . . . C27 C 0.6312(4) 1.0734(4) 0.6880(3) 0.0191(9) Uani 1 1 d . . . C28 C 0.7184(4) 1.1142(5) 0.7525(4) 0.0238(10) Uani 1 1 d . . . H28 H 0.7946 1.0834 0.7461 0.029 Uiso 1 1 calc R . . C29 C 0.6974(4) 1.1986(5) 0.8259(4) 0.0282(11) Uani 1 1 d . . . C30 C 0.5866(4) 1.2479(5) 0.8310(4) 0.0259(11) Uani 1 1 d . . . H30 H 0.5718 1.3086 0.8788 0.031 Uiso 1 1 calc R . . C31 C 0.4971(4) 1.2106(4) 0.7680(3) 0.0201(10) Uani 1 1 d . . . C32 C 0.6659(4) 0.9867(5) 0.6080(4) 0.0257(11) Uani 1 1 d . . . H32A H 0.6697 0.9002 0.6318 0.038 Uiso 1 1 calc R . . H32B H 0.7418 1.0117 0.5860 0.038 Uiso 1 1 calc R . . H32C H 0.6089 0.9922 0.5544 0.038 Uiso 1 1 calc R . . C33 C 0.7951(5) 1.2398(7) 0.8944(5) 0.0480(17) Uani 1 1 d . . . H33A H 0.7648 1.2953 0.9435 0.072 Uiso 1 1 calc R . . H33B H 0.8533 1.2847 0.8587 0.072 Uiso 1 1 calc R . . H33C H 0.8304 1.1658 0.9254 0.072 Uiso 1 1 calc R . . C34 C 0.3813(4) 1.2739(5) 0.7777(4) 0.0264(11) Uani 1 1 d . . . H34A H 0.3783 1.3132 0.8411 0.040 Uiso 1 1 calc R . . H34B H 0.3197 1.2113 0.7703 0.040 Uiso 1 1 calc R . . H34C H 0.3709 1.3382 0.7278 0.040 Uiso 1 1 calc R . . C35 C 0.1683(5) 1.0582(7) 0.3513(4) 0.0432(16) Uani 1 1 d . . . H35A H 0.2210 1.0745 0.2995 0.065 Uiso 1 1 calc R . . H35B H 0.1372 1.1378 0.3741 0.065 Uiso 1 1 calc R . . H35C H 0.1048 1.0048 0.3271 0.065 Uiso 1 1 calc R . . C36 C 0.2783(5) 0.8759(5) 0.3987(4) 0.0306(12) Uani 1 1 d . . . H36A H 0.2161 0.8226 0.3722 0.046 Uiso 1 1 calc R . . H36B H 0.3169 0.8336 0.4535 0.046 Uiso 1 1 calc R . . H36C H 0.3342 0.8918 0.3492 0.046 Uiso 1 1 calc R . . C37 C -0.0001(4) 1.1358(6) 0.6105(4) 0.0331(12) Uani 1 1 d . . . H37A H 0.0094 1.1664 0.6766 0.050 Uiso 1 1 calc R . . H37B H -0.0247 1.0478 0.6110 0.050 Uiso 1 1 calc R . . H37C H -0.0585 1.1863 0.5756 0.050 Uiso 1 1 calc R . . C38 C 0.1322(5) 1.2762(5) 0.5383(5) 0.0365(14) Uani 1 1 d . . . H38A H 0.0688 1.3083 0.4967 0.055 Uiso 1 1 calc R . . H38B H 0.2044 1.2812 0.5045 0.055 Uiso 1 1 calc R . . H38C H 0.1387 1.3268 0.5970 0.055 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 0.0152(4) 0.0179(4) 0.0152(3) 0.0007(3) -0.0017(2) -0.0007(3) O1 0.0193(17) 0.0241(18) 0.0145(15) -0.0014(14) -0.0005(12) -0.0028(13) O2 0.0165(16) 0.0203(16) 0.0210(16) 0.0014(14) -0.0037(12) 0.0015(12) N1 0.0163(19) 0.021(2) 0.0177(18) -0.0005(16) 0.0005(14) -0.0003(15) N2 0.021(2) 0.0105(18) 0.0156(18) 0.0000(15) 0.0006(14) -0.0013(15) N3 0.0232(19) 0.022(2) 0.0180(17) -0.0003(15) -0.0029(14) -0.0036(15) N4 0.016(2) 0.029(2) 0.027(2) 0.0029(19) -0.0049(16) 0.0019(16) C1 0.020(2) 0.016(2) 0.015(2) -0.0009(17) 0.0019(17) -0.0025(17) C2 0.021(2) 0.014(2) 0.015(2) -0.0005(17) 0.0018(17) -0.0022(18) C3 0.022(2) 0.025(3) 0.024(2) -0.0027(19) 0.0031(18) 0.0051(19) C4 0.033(3) 0.030(3) 0.020(2) -0.008(2) 0.009(2) -0.006(2) C5 0.029(2) 0.028(2) 0.0161(19) -0.006(2) -0.0022(16) -0.002(2) C6 0.022(2) 0.021(2) 0.016(2) 0.0017(18) 0.0006(17) -0.0050(18) C7 0.023(3) 0.025(3) 0.019(2) -0.001(2) -0.0057(18) -0.0033(19) C8 0.013(2) 0.021(2) 0.017(2) -0.0003(19) -0.0032(16) -0.0011(17) C9 0.015(2) 0.020(2) 0.018(2) -0.0023(19) -0.0010(16) -0.0019(17) C10 0.018(2) 0.023(2) 0.027(2) -0.003(2) 0.0057(18) 0.0005(19) C11 0.024(3) 0.019(3) 0.035(3) -0.005(2) 0.004(2) 0.0045(19) C12 0.020(2) 0.018(2) 0.036(3) 0.002(2) -0.0042(19) 0.0038(18) C13 0.014(2) 0.025(2) 0.027(3) 0.002(2) -0.0097(18) -0.0016(17) C14 0.032(3) 0.019(2) 0.025(2) 0.006(2) -0.0073(19) -0.004(2) C15 0.012(2) 0.023(2) 0.023(2) -0.002(2) 0.0032(17) 0.0016(17) C16 0.016(2) 0.025(2) 0.021(2) 0.000(2) -0.0003(17) -0.0037(18) C17 0.014(2) 0.024(2) 0.025(2) -0.001(2) -0.0069(17) -0.0036(17) C18 0.026(2) 0.027(2) 0.032(2) 0.004(3) -0.0058(18) -0.010(2) C19 0.027(2) 0.033(3) 0.031(2) 0.011(3) -0.0077(18) -0.015(2) C20 0.022(3) 0.049(3) 0.022(2) -0.001(2) 0.0073(19) -0.010(2) C21 0.019(3) 0.038(3) 0.026(3) -0.003(2) 0.0021(19) -0.008(2) C22 0.026(3) 0.018(2) 0.030(3) -0.004(2) -0.0013(19) 0.0002(19) C23 0.057(4) 0.056(4) 0.042(4) 0.021(3) -0.003(3) -0.017(3) C24 0.037(3) 0.041(3) 0.039(3) -0.008(3) 0.013(2) 0.005(3) C25 0.017(2) 0.023(2) 0.011(2) -0.0017(18) 0.0030(16) 0.0017(17) C26 0.019(2) 0.015(2) 0.015(2) 0.0031(18) 0.0015(16) -0.0043(17) C27 0.020(2) 0.019(2) 0.018(2) 0.0071(18) 0.0039(17) -0.0028(18) C28 0.016(2) 0.029(3) 0.027(2) 0.006(2) -0.0019(18) -0.0016(18) C29 0.025(3) 0.035(3) 0.024(3) 0.003(2) -0.005(2) -0.013(2) C30 0.033(3) 0.022(3) 0.023(2) -0.002(2) 0.000(2) -0.009(2) C31 0.022(3) 0.017(2) 0.021(2) 0.0022(19) -0.0007(18) -0.0012(18) C32 0.017(2) 0.028(3) 0.032(2) 0.000(2) 0.0041(18) -0.0021(18) C33 0.026(3) 0.072(5) 0.045(4) -0.017(3) -0.010(3) -0.011(3) C34 0.026(3) 0.021(3) 0.033(3) -0.008(2) 0.004(2) -0.002(2) C35 0.033(3) 0.071(5) 0.025(3) 0.012(3) -0.008(2) -0.001(3) C36 0.031(3) 0.034(3) 0.028(3) -0.008(2) 0.007(2) -0.012(2) C37 0.020(3) 0.033(3) 0.046(3) 0.004(3) 0.000(2) 0.003(2) C38 0.028(3) 0.026(3) 0.054(4) 0.011(3) -0.016(2) 0.001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V1 N4 1.852(4) . ? V1 N3 1.858(4) . ? V1 O2 2.072(3) . ? V1 O1 2.098(3) . ? V1 N2 2.198(4) . ? V1 N1 2.202(4) . ? V1 C25 2.529(5) . ? V1 C15 2.551(5) . ? O1 C15 1.293(6) . ? O2 C25 1.305(6) . ? N1 C15 1.307(6) . ? N1 C2 1.416(6) . ? N2 C25 1.315(6) . ? N2 C9 1.410(6) . ? N3 C36 1.457(7) . ? N3 C35 1.458(6) . ? N4 C37 1.456(7) . ? N4 C38 1.460(7) . ? C1 C6 1.417(6) . ? C1 C2 1.421(6) . ? C1 C8 1.492(6) . ? C2 C3 1.398(6) . ? C3 C4 1.389(7) . ? C3 H3 0.9500 . ? C4 C5 1.395(7) . ? C4 H4 0.9500 . ? C5 C6 1.398(7) . ? C5 H5 0.9500 . ? C6 C7 1.524(7) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C13 1.410(7) . ? C8 C9 1.416(6) . ? C9 C10 1.407(7) . ? C10 C11 1.380(7) . ? C10 H10 0.9500 . ? C11 C12 1.394(8) . ? C11 H11 0.9500 . ? C12 C13 1.395(7) . ? C12 H12 0.9500 . ? C13 C14 1.510(7) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.510(7) . ? C16 C17 1.394(7) . ? C16 C21 1.417(7) . ? C17 C18 1.387(7) . ? C17 C22 1.492(7) . ? C18 C19 1.404(7) . ? C18 H18 0.9500 . ? C19 C20 1.373(9) . ? C19 C23 1.515(8) . ? C20 C21 1.402(8) . ? C20 H20 0.9500 . ? C21 C24 1.507(8) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.505(6) . ? C26 C27 1.399(7) . ? C26 C31 1.416(7) . ? C27 C28 1.396(7) . ? C27 C32 1.515(7) . ? C28 C29 1.390(8) . ? C28 H28 0.9500 . ? C29 C30 1.393(8) . ? C29 C33 1.519(7) . ? C30 C31 1.391(7) . ? C30 H30 0.9500 . ? C31 C34 1.515(7) . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 V1 N3 101.12(18) . . ? N4 V1 O2 90.74(16) . . ? N3 V1 O2 106.09(15) . . ? N4 V1 O1 100.53(16) . . ? N3 V1 O1 90.77(15) . . ? O2 V1 O1 157.61(12) . . ? N4 V1 N2 148.81(17) . . ? N3 V1 N2 100.44(16) . . ? O2 V1 N2 61.64(14) . . ? O1 V1 N2 101.44(14) . . ? N4 V1 N1 94.15(17) . . ? N3 V1 N1 149.91(16) . . ? O2 V1 N1 99.40(13) . . ? O1 V1 N1 60.81(14) . . ? N2 V1 N1 77.75(14) . . ? N4 V1 C25 118.69(17) . . ? N3 V1 C25 110.14(16) . . ? O2 V1 C25 30.96(14) . . ? O1 V1 C25 129.22(14) . . ? N2 V1 C25 31.31(15) . . ? N1 V1 C25 84.10(14) . . ? N4 V1 C15 102.04(17) . . ? N3 V1 C15 119.59(16) . . ? O2 V1 C15 128.38(14) . . ? O1 V1 C15 30.35(14) . . ? N2 V1 C15 86.42(14) . . ? N1 V1 C15 30.83(14) . . ? C25 V1 C15 105.76(15) . . ? C15 O1 V1 94.6(3) . . ? C25 O2 V1 94.2(3) . . ? C15 N1 C2 127.7(4) . . ? C15 N1 V1 89.5(3) . . ? C2 N1 V1 135.4(3) . . ? C25 N2 C9 127.8(4) . . ? C25 N2 V1 88.3(3) . . ? C9 N2 V1 133.7(3) . . ? C36 N3 C35 111.0(4) . . ? C36 N3 V1 118.3(3) . . ? C35 N3 V1 128.6(4) . . ? C37 N4 C38 110.4(4) . . ? C37 N4 V1 125.8(4) . . ? C38 N4 V1 122.1(3) . . ? C6 C1 C2 118.2(4) . . ? C6 C1 C8 119.6(4) . . ? C2 C1 C8 122.2(4) . . ? C3 C2 N1 118.9(4) . . ? C3 C2 C1 120.0(4) . . ? N1 C2 C1 120.5(4) . . ? C4 C3 C2 121.2(4) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 119.1(5) . . ? C3 C4 H4 120.5 . . ? C5 C4 H4 120.5 . . ? C4 C5 C6 121.1(4) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C1 120.1(4) . . ? C5 C6 C7 119.0(4) . . ? C1 C6 C7 120.7(4) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C13 C8 C9 118.9(4) . . ? C13 C8 C1 119.0(4) . . ? C9 C8 C1 122.1(4) . . ? C10 C9 N2 117.9(4) . . ? C10 C9 C8 119.5(4) . . ? N2 C9 C8 122.1(4) . . ? C11 C10 C9 121.1(5) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C10 C11 C12 119.2(5) . . ? C10 C11 H11 120.4 . . ? C12 C11 H11 120.4 . . ? C11 C12 C13 121.4(5) . . ? C11 C12 H12 119.3 . . ? C13 C12 H12 119.3 . . ? C12 C13 C8 119.5(5) . . ? C12 C13 C14 120.0(4) . . ? C8 C13 C14 120.3(5) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O1 C15 N1 113.8(4) . . ? O1 C15 C16 121.8(4) . . ? N1 C15 C16 124.4(4) . . ? O1 C15 V1 55.0(2) . . ? N1 C15 V1 59.7(2) . . ? C16 C15 V1 169.3(3) . . ? C17 C16 C21 119.9(5) . . ? C17 C16 C15 120.1(4) . . ? C21 C16 C15 120.0(4) . . ? C18 C17 C16 118.6(5) . . ? C18 C17 C22 118.6(5) . . ? C16 C17 C22 122.7(4) . . ? C17 C18 C19 122.5(6) . . ? C17 C18 H18 118.8 . . ? C19 C18 H18 118.8 . . ? C20 C19 C18 117.7(5) . . ? C20 C19 C23 122.9(5) . . ? C18 C19 C23 119.4(6) . . ? C19 C20 C21 122.0(5) . . ? C19 C20 H20 119.0 . . ? C21 C20 H20 119.0 . . ? C20 C21 C16 118.7(5) . . ? C20 C21 C24 119.2(5) . . ? C16 C21 C24 122.0(5) . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? O2 C25 N2 113.5(4) . . ? O2 C25 C26 118.9(4) . . ? N2 C25 C26 127.6(4) . . ? O2 C25 V1 54.8(2) . . ? N2 C25 V1 60.3(2) . . ? C26 C25 V1 164.1(3) . . ? C27 C26 C31 119.9(4) . . ? C27 C26 C25 121.3(4) . . ? C31 C26 C25 118.8(4) . . ? C28 C27 C26 118.9(4) . . ? C28 C27 C32 117.2(4) . . ? C26 C27 C32 123.8(4) . . ? C29 C28 C27 122.0(4) . . ? C29 C28 H28 119.0 . . ? C27 C28 H28 119.0 . . ? C28 C29 C30 118.1(4) . . ? C28 C29 C33 120.0(5) . . ? C30 C29 C33 121.8(5) . . ? C31 C30 C29 121.8(5) . . ? C31 C30 H30 119.1 . . ? C29 C30 H30 119.1 . . ? C30 C31 C26 118.9(4) . . ? C30 C31 C34 117.4(5) . . ? C26 C31 C34 123.7(4) . . ? C27 C32 H32A 109.5 . . ? C27 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C27 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C29 C33 H33A 109.5 . . ? C29 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C29 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N3 C35 H35A 109.5 . . ? N3 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N3 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N3 C36 H36A 109.5 . . ? N3 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N3 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N4 C37 H37A 109.5 . . ? N4 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N4 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N4 C38 H38A 109.5 . . ? N4 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N4 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 V1 O1 C15 -95.9(3) . . . . ? N3 V1 O1 C15 162.7(3) . . . . ? O2 V1 O1 C15 23.2(5) . . . . ? N2 V1 O1 C15 61.8(3) . . . . ? N1 V1 O1 C15 -7.0(2) . . . . ? C25 V1 O1 C15 45.6(3) . . . . ? N4 V1 O2 C25 155.7(3) . . . . ? N3 V1 O2 C25 -102.5(3) . . . . ? O1 V1 O2 C25 35.0(5) . . . . ? N2 V1 O2 C25 -9.1(3) . . . . ? N1 V1 O2 C25 61.4(3) . . . . ? C15 V1 O2 C25 49.7(3) . . . . ? N4 V1 N1 C15 106.6(3) . . . . ? N3 V1 N1 C15 -14.1(4) . . . . ? O2 V1 N1 C15 -161.9(3) . . . . ? O1 V1 N1 C15 6.9(2) . . . . ? N2 V1 N1 C15 -103.8(3) . . . . ? C25 V1 N1 C15 -134.9(3) . . . . ? N4 V1 N1 C2 -103.7(4) . . . . ? N3 V1 N1 C2 135.6(4) . . . . ? O2 V1 N1 C2 -12.2(4) . . . . ? O1 V1 N1 C2 156.6(5) . . . . ? N2 V1 N1 C2 45.9(4) . . . . ? C25 V1 N1 C2 14.8(4) . . . . ? C15 V1 N1 C2 149.7(6) . . . . ? N4 V1 N2 C25 -21.3(5) . . . . ? N3 V1 N2 C25 111.8(3) . . . . ? O2 V1 N2 C25 9.0(3) . . . . ? O1 V1 N2 C25 -155.3(3) . . . . ? N1 V1 N2 C25 -98.9(3) . . . . ? C15 V1 N2 C25 -128.8(3) . . . . ? N4 V1 N2 C9 123.9(4) . . . . ? N3 V1 N2 C9 -103.0(4) . . . . ? O2 V1 N2 C9 154.2(5) . . . . ? O1 V1 N2 C9 -10.1(4) . . . . ? N1 V1 N2 C9 46.3(4) . . . . ? C25 V1 N2 C9 145.2(6) . . . . ? C15 V1 N2 C9 16.4(4) . . . . ? N4 V1 N3 C36 -158.5(3) . . . . ? O2 V1 N3 C36 107.5(3) . . . . ? O1 V1 N3 C36 -57.6(3) . . . . ? N2 V1 N3 C36 44.2(3) . . . . ? N1 V1 N3 C36 -39.4(5) . . . . ? C25 V1 N3 C36 75.1(4) . . . . ? C15 V1 N3 C36 -47.6(4) . . . . ? N4 V1 N3 C35 3.2(5) . . . . ? O2 V1 N3 C35 -90.8(4) . . . . ? O1 V1 N3 C35 104.1(4) . . . . ? N2 V1 N3 C35 -154.1(4) . . . . ? N1 V1 N3 C35 122.3(5) . . . . ? C25 V1 N3 C35 -123.2(4) . . . . ? C15 V1 N3 C35 114.1(4) . . . . ? N3 V1 N4 C37 120.0(4) . . . . ? O2 V1 N4 C37 -133.4(4) . . . . ? O1 V1 N4 C37 27.1(4) . . . . ? N2 V1 N4 C37 -107.0(5) . . . . ? N1 V1 N4 C37 -33.9(4) . . . . ? C25 V1 N4 C37 -119.5(4) . . . . ? C15 V1 N4 C37 -3.8(5) . . . . ? N3 V1 N4 C38 -76.3(4) . . . . ? O2 V1 N4 C38 30.3(4) . . . . ? O1 V1 N4 C38 -169.2(4) . . . . ? N2 V1 N4 C38 56.6(6) . . . . ? N1 V1 N4 C38 129.7(4) . . . . ? C25 V1 N4 C38 44.2(5) . . . . ? C15 V1 N4 C38 159.9(4) . . . . ? C15 N1 C2 C3 -115.3(5) . . . . ? V1 N1 C2 C3 104.4(5) . . . . ? C15 N1 C2 C1 73.4(6) . . . . ? V1 N1 C2 C1 -67.0(6) . . . . ? C6 C1 C2 C3 -4.5(6) . . . . ? C8 C1 C2 C3 174.6(4) . . . . ? C6 C1 C2 N1 166.8(4) . . . . ? C8 C1 C2 N1 -14.1(6) . . . . ? N1 C2 C3 C4 -171.8(4) . . . . ? C1 C2 C3 C4 -0.4(7) . . . . ? C2 C3 C4 C5 4.4(8) . . . . ? C3 C4 C5 C6 -3.5(8) . . . . ? C4 C5 C6 C1 -1.4(8) . . . . ? C4 C5 C6 C7 174.4(5) . . . . ? C2 C1 C6 C5 5.3(7) . . . . ? C8 C1 C6 C5 -173.8(5) . . . . ? C2 C1 C6 C7 -170.3(4) . . . . ? C8 C1 C6 C7 10.5(7) . . . . ? C6 C1 C8 C13 62.7(6) . . . . ? C2 C1 C8 C13 -116.4(5) . . . . ? C6 C1 C8 C9 -117.0(5) . . . . ? C2 C1 C8 C9 63.9(6) . . . . ? C25 N2 C9 C10 -122.0(5) . . . . ? V1 N2 C9 C10 104.2(5) . . . . ? C25 N2 C9 C8 66.4(6) . . . . ? V1 N2 C9 C8 -67.3(6) . . . . ? C13 C8 C9 C10 -4.9(6) . . . . ? C1 C8 C9 C10 174.7(4) . . . . ? C13 C8 C9 N2 166.6(4) . . . . ? C1 C8 C9 N2 -13.8(6) . . . . ? N2 C9 C10 C11 -172.4(4) . . . . ? C8 C9 C10 C11 -0.6(7) . . . . ? C9 C10 C11 C12 4.0(7) . . . . ? C10 C11 C12 C13 -1.8(7) . . . . ? C11 C12 C13 C8 -3.6(7) . . . . ? C11 C12 C13 C14 172.9(4) . . . . ? C9 C8 C13 C12 6.9(6) . . . . ? C1 C8 C13 C12 -172.7(4) . . . . ? C9 C8 C13 C14 -169.6(4) . . . . ? C1 C8 C13 C14 10.8(6) . . . . ? V1 O1 C15 N1 11.3(4) . . . . ? V1 O1 C15 C16 -167.8(4) . . . . ? C2 N1 C15 O1 -164.1(4) . . . . ? V1 N1 C15 O1 -10.7(4) . . . . ? C2 N1 C15 C16 14.9(7) . . . . ? V1 N1 C15 C16 168.3(4) . . . . ? C2 N1 C15 V1 -153.4(5) . . . . ? N4 V1 C15 O1 90.3(3) . . . . ? N3 V1 C15 O1 -20.0(3) . . . . ? O2 V1 C15 O1 -169.0(2) . . . . ? N2 V1 C15 O1 -120.0(3) . . . . ? N1 V1 C15 O1 168.0(4) . . . . ? C25 V1 C15 O1 -144.9(3) . . . . ? N4 V1 C15 N1 -77.7(3) . . . . ? N3 V1 C15 N1 171.9(3) . . . . ? O2 V1 C15 N1 23.0(3) . . . . ? O1 V1 C15 N1 -168.0(4) . . . . ? N2 V1 C15 N1 72.0(3) . . . . ? C25 V1 C15 N1 47.1(3) . . . . ? N4 V1 C15 C16 166.7(17) . . . . ? N3 V1 C15 C16 56.4(18) . . . . ? O2 V1 C15 C16 -92.6(18) . . . . ? O1 V1 C15 C16 76.4(17) . . . . ? N2 V1 C15 C16 -43.6(18) . . . . ? N1 V1 C15 C16 -115.6(18) . . . . ? C25 V1 C15 C16 -68.5(18) . . . . ? O1 C15 C16 C17 58.4(6) . . . . ? N1 C15 C16 C17 -120.5(5) . . . . ? V1 C15 C16 C17 -11(2) . . . . ? O1 C15 C16 C21 -123.4(5) . . . . ? N1 C15 C16 C21 57.7(6) . . . . ? V1 C15 C16 C21 167.0(15) . . . . ? C21 C16 C17 C18 -8.0(6) . . . . ? C15 C16 C17 C18 170.2(4) . . . . ? C21 C16 C17 C22 169.8(4) . . . . ? C15 C16 C17 C22 -12.0(7) . . . . ? C16 C17 C18 C19 1.9(7) . . . . ? C22 C17 C18 C19 -176.0(4) . . . . ? C17 C18 C19 C20 4.1(7) . . . . ? C17 C18 C19 C23 -174.5(5) . . . . ? C18 C19 C20 C21 -4.1(7) . . . . ? C23 C19 C20 C21 174.5(5) . . . . ? C19 C20 C21 C16 -1.9(7) . . . . ? C19 C20 C21 C24 174.2(5) . . . . ? C17 C16 C21 C20 8.1(7) . . . . ? C15 C16 C21 C20 -170.1(4) . . . . ? C17 C16 C21 C24 -167.9(5) . . . . ? C15 C16 C21 C24 13.9(7) . . . . ? V1 O2 C25 N2 14.7(4) . . . . ? V1 O2 C25 C26 -162.7(3) . . . . ? C9 N2 C25 O2 -162.3(4) . . . . ? V1 N2 C25 O2 -13.8(4) . . . . ? C9 N2 C25 C26 14.9(8) . . . . ? V1 N2 C25 C26 163.4(4) . . . . ? C9 N2 C25 V1 -148.5(5) . . . . ? N4 V1 C25 O2 -27.9(3) . . . . ? N3 V1 C25 O2 87.9(3) . . . . ? O1 V1 C25 O2 -163.6(2) . . . . ? N2 V1 C25 O2 164.5(4) . . . . ? N1 V1 C25 O2 -119.4(3) . . . . ? C15 V1 C25 O2 -141.6(3) . . . . ? N4 V1 C25 N2 167.6(3) . . . . ? N3 V1 C25 N2 -76.6(3) . . . . ? O2 V1 C25 N2 -164.5(4) . . . . ? O1 V1 C25 N2 31.9(3) . . . . ? N1 V1 C25 N2 76.1(3) . . . . ? C15 V1 C25 N2 53.9(3) . . . . ? N4 V1 C25 C26 43.5(12) . . . . ? N3 V1 C25 C26 159.3(12) . . . . ? O2 V1 C25 C26 71.4(12) . . . . ? O1 V1 C25 C26 -92.2(12) . . . . ? N2 V1 C25 C26 -124.1(13) . . . . ? N1 V1 C25 C26 -48.0(12) . . . . ? C15 V1 C25 C26 -70.2(12) . . . . ? O2 C25 C26 C27 -134.7(4) . . . . ? N2 C25 C26 C27 48.2(7) . . . . ? V1 C25 C26 C27 163.1(10) . . . . ? O2 C25 C26 C31 44.4(6) . . . . ? N2 C25 C26 C31 -132.6(5) . . . . ? V1 C25 C26 C31 -17.8(14) . . . . ? C31 C26 C27 C28 3.9(6) . . . . ? C25 C26 C27 C28 -177.0(4) . . . . ? C31 C26 C27 C32 -172.7(4) . . . . ? C25 C26 C27 C32 6.4(7) . . . . ? C26 C27 C28 C29 0.0(7) . . . . ? C32 C27 C28 C29 176.8(4) . . . . ? C27 C28 C29 C30 -3.4(7) . . . . ? C27 C28 C29 C33 179.8(5) . . . . ? C28 C29 C30 C31 2.9(7) . . . . ? C33 C29 C30 C31 179.8(5) . . . . ? C29 C30 C31 C26 0.8(7) . . . . ? C29 C30 C31 C34 -177.7(5) . . . . ? C27 C26 C31 C30 -4.3(7) . . . . ? C25 C26 C31 C30 176.5(4) . . . . ? C27 C26 C31 C34 174.2(4) . . . . ? C25 C26 C31 C34 -5.0(7) . . . . ? _diffrn_measured_fraction_theta_max 0.958 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.962 _refine_diff_density_max 0.484 _refine_diff_density_min -0.552 _refine_diff_density_rms 0.118 # Attachment '- compound 20.cif' data_compound20 _database_code_depnum_ccdc_archive 'CCDC 791865' #TrackingRef '- compound 20.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H52 N5 Nb O4 S2' _chemical_formula_sum 'C38 H52 N5 Nb O4 S2' _chemical_formula_weight 799.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Nb Nb -0.1121 2.4826 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.1360(15) _cell_length_b 16.0630(18) _cell_length_c 17.379(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.527(6) _cell_angle_gamma 90.00 _cell_volume 3874.1(7) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 5057 _cell_measurement_theta_min 27.70 _cell_measurement_theta_max 72.40 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.371 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 3.900 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4808 _exptl_absorpt_correction_T_max 0.5742 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Rigaku Saturn70 CCD camera' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 41218 _diffrn_reflns_av_R_equivalents 0.0458 _diffrn_reflns_av_sigmaI/netI 0.0263 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.18 _diffrn_reflns_theta_max 72.57 _reflns_number_total 7536 _reflns_number_gt 7174 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r4' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure 4.0' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2009)' _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^)+(0.0536P)^2^+3.7033P] 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 7536 _refine_ls_number_parameters 465 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0342 _refine_ls_R_factor_gt 0.0316 _refine_ls_wR_factor_ref 0.0988 _refine_ls_wR_factor_gt 0.0821 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Nb1 Nb 0.179685(12) 0.495312(11) 0.276155(11) 0.01463(8) Uani 1 1 d . . . S1 S 0.37439(4) 0.55646(3) 0.25470(3) 0.01696(12) Uani 1 1 d . . . S2 S 0.08674(4) 0.29567(3) 0.22609(3) 0.01895(12) Uani 1 1 d . . . O1 O 0.30485(11) 0.60735(10) 0.19099(10) 0.0213(3) Uani 1 1 d . . . O2 O 0.42992(12) 0.59720(10) 0.33266(10) 0.0227(3) Uani 1 1 d . . . O3 O 0.02637(12) 0.33066(11) 0.26404(11) 0.0250(4) Uani 1 1 d . . . O4 O 0.14748(12) 0.22752(11) 0.27072(11) 0.0242(4) Uani 1 1 d . . . N1 N 0.31329(13) 0.47760(12) 0.26641(12) 0.0160(4) Uani 1 1 d . . . N2 N 0.14944(13) 0.36987(12) 0.20947(12) 0.0167(4) Uani 1 1 d . . . N3 N 0.15655(15) 0.45085(13) 0.36993(12) 0.0215(4) Uani 1 1 d . . . N4 N 0.07231(14) 0.55094(12) 0.18823(12) 0.0200(4) Uani 1 1 d . . . N5 N 0.21746(14) 0.60446(12) 0.33720(13) 0.0214(4) Uani 1 1 d . . . C1 C 0.35134(15) 0.33053(14) 0.29445(14) 0.0176(4) Uani 1 1 d . . . C2 C 0.36325(15) 0.41259(14) 0.32489(14) 0.0176(4) Uani 1 1 d . . . C3 C 0.41365(17) 0.42924(15) 0.41021(15) 0.0212(5) Uani 1 1 d . . . H3A H 0.4203 0.4849 0.4303 0.025 Uiso 1 1 calc R . . C4 C 0.45406(17) 0.36401(16) 0.46561(15) 0.0240(5) Uani 1 1 d . . . H4A H 0.4903 0.3749 0.5235 0.029 Uiso 1 1 calc R . . C5 C 0.44117(17) 0.28307(16) 0.43582(16) 0.0241(5) Uani 1 1 d . . . H5A H 0.4689 0.2387 0.4741 0.029 Uiso 1 1 calc R . . C6 C 0.38857(16) 0.26460(15) 0.35109(15) 0.0210(5) Uani 1 1 d . . . C7 C 0.37139(19) 0.17444(15) 0.32464(18) 0.0279(5) Uani 1 1 d . . . H7A H 0.3244 0.1504 0.3441 0.042 Uiso 1 1 calc R . . H7B H 0.4322 0.1436 0.3493 0.042 Uiso 1 1 calc R . . H7C H 0.3464 0.1708 0.2633 0.042 Uiso 1 1 calc R . . C8 C 0.29994(16) 0.31843(14) 0.20221(15) 0.0179(4) Uani 1 1 d . . . C9 C 0.20253(17) 0.34101(14) 0.16154(14) 0.0185(4) Uani 1 1 d . . . C10 C 0.15718(17) 0.33693(14) 0.07422(15) 0.0211(5) Uani 1 1 d . . . H10 H 0.0920 0.3542 0.0466 0.025 Uiso 1 1 calc R . . C11 C 0.20648(18) 0.30799(15) 0.02786(16) 0.0240(5) Uani 1 1 d . . . H11 H 0.1749 0.3046 -0.0315 0.029 Uiso 1 1 calc R . . C12 C 0.30197(18) 0.28383(15) 0.06774(16) 0.0245(5) Uani 1 1 d . . . H12 H 0.3348 0.2623 0.0355 0.029 Uiso 1 1 calc R . . C13 C 0.35030(17) 0.29064(14) 0.15432(16) 0.0209(5) Uani 1 1 d . . . C14 C 0.45678(18) 0.27102(16) 0.19521(17) 0.0272(5) Uani 1 1 d . . . H14A H 0.4815 0.2617 0.1517 0.041 Uiso 1 1 calc R . . H14B H 0.4667 0.2208 0.2297 0.041 Uiso 1 1 calc R . . H14C H 0.4911 0.3179 0.2307 0.041 Uiso 1 1 calc R . . C15 C 0.45616(17) 0.51243(14) 0.21472(16) 0.0191(5) Uani 1 1 d . . . C16 C 0.42018(19) 0.48992(14) 0.12968(17) 0.0215(5) Uani 1 1 d . . . C17 C 0.48401(19) 0.45623(16) 0.09813(17) 0.0258(5) Uani 1 1 d . . . H17 H 0.4603 0.4410 0.0406 0.031 Uiso 1 1 calc R . . C18 C 0.5803(2) 0.44437(17) 0.14782(18) 0.0310(6) Uani 1 1 d . . . C19 C 0.61390(19) 0.46745(17) 0.23121(18) 0.0299(6) Uani 1 1 d . . . H19 H 0.6803 0.4594 0.2654 0.036 Uiso 1 1 calc R . . C20 C 0.55561(19) 0.50175(15) 0.26770(17) 0.0239(5) Uani 1 1 d . . . C21 C 0.31733(19) 0.49961(15) 0.06936(16) 0.0239(5) Uani 1 1 d . . . H21A H 0.3027 0.5588 0.0573 0.036 Uiso 1 1 calc R . . H21B H 0.2749 0.4762 0.0941 0.036 Uiso 1 1 calc R . . H21C H 0.3071 0.4701 0.0171 0.036 Uiso 1 1 calc R . . C22 C 0.6469(3) 0.4055(2) 0.1122(2) 0.0496(9) Uani 1 1 d . . . H22A H 0.6661 0.3499 0.1364 0.074 Uiso 1 1 calc R . . H22B H 0.7043 0.4404 0.1260 0.074 Uiso 1 1 calc R . . H22C H 0.6133 0.4009 0.0511 0.074 Uiso 1 1 calc R . . C23 C 0.6037(2) 0.5246(2) 0.35947(18) 0.0346(6) Uani 1 1 d . . . H23A H 0.6704 0.5046 0.3824 0.052 Uiso 1 1 calc R . . H23B H 0.5687 0.4987 0.3901 0.052 Uiso 1 1 calc R . . H23C H 0.6032 0.5852 0.3655 0.052 Uiso 1 1 calc R . . C24 C 0.00844(17) 0.25725(16) 0.12460(16) 0.0233(5) Uani 1 1 d . . . C25 C 0.0308(2) 0.18459(17) 0.09057(17) 0.0287(6) Uani 1 1 d . . . C26 C -0.0336(2) 0.16062(18) 0.01045(18) 0.0367(7) Uani 1 1 d . . . H26 H -0.0201 0.1115 -0.0132 0.044 Uiso 1 1 calc R . . C27 C -0.1162(3) 0.2050(2) -0.03613(18) 0.0432(8) Uani 1 1 d . . . C28 C -0.1345(2) 0.27656(19) -0.00095(18) 0.0371(7) Uani 1 1 d . . . H28 H -0.1907 0.3079 -0.0323 0.045 Uiso 1 1 calc R . . C29 C -0.07439(18) 0.30469(17) 0.07827(17) 0.0283(6) Uani 1 1 d . . . C30 C 0.1198(2) 0.13186(18) 0.1320(2) 0.0364(6) Uani 1 1 d . . . H30A H 0.1192 0.0862 0.0943 0.055 Uiso 1 1 calc R . . H30B H 0.1208 0.1089 0.1845 0.055 Uiso 1 1 calc R . . H30C H 0.1773 0.1662 0.1439 0.055 Uiso 1 1 calc R . . C31 C -0.1844(4) 0.1747(3) -0.1215(2) 0.0726(14) Uani 1 1 d . . . H31A H -0.1478 0.1607 -0.1552 0.109 Uiso 1 1 calc R . . H31B H -0.2311 0.2186 -0.1497 0.109 Uiso 1 1 calc R . . H31C H -0.2186 0.1252 -0.1150 0.109 Uiso 1 1 calc R . . C32 C -0.10140(19) 0.38494(18) 0.1083(2) 0.0357(6) Uani 1 1 d . . . H32A H -0.1468 0.4159 0.0601 0.053 Uiso 1 1 calc R . . H32B H -0.0434 0.4185 0.1367 0.053 Uiso 1 1 calc R . . H32C H -0.1316 0.3726 0.1475 0.053 Uiso 1 1 calc R . . C33 C 0.0842(2) 0.48768(19) 0.3953(2) 0.0365(7) Uani 1 1 d . . . H33A H 0.0282 0.4507 0.3789 0.055 Uiso 1 1 calc R . . H33B H 0.0643 0.5418 0.3677 0.055 Uiso 1 1 calc R . . H33C H 0.1116 0.4953 0.4563 0.055 Uiso 1 1 calc R . . C34 C 0.20150(18) 0.37834(16) 0.42066(15) 0.0235(5) Uani 1 1 d . . . H34A H 0.2410 0.3960 0.4782 0.035 Uiso 1 1 calc R . . H34B H 0.2423 0.3503 0.3968 0.035 Uiso 1 1 calc R . . H34C H 0.1514 0.3399 0.4211 0.035 Uiso 1 1 calc R . . C35 C -0.00181(18) 0.60594(18) 0.19235(17) 0.0297(6) Uani 1 1 d . . . H35A H 0.0017 0.6597 0.1671 0.045 Uiso 1 1 calc R . . H35B H 0.0082 0.6142 0.2511 0.045 Uiso 1 1 calc R . . H35C H -0.0653 0.5810 0.1616 0.045 Uiso 1 1 calc R . . C36 C 0.07097(18) 0.54448(17) 0.10435(15) 0.0254(5) Uani 1 1 d . . . H36A H 0.0099 0.5197 0.0665 0.038 Uiso 1 1 calc R . . H36B H 0.1246 0.5093 0.1059 0.038 Uiso 1 1 calc R . . H36C H 0.0776 0.6001 0.0841 0.038 Uiso 1 1 calc R . . C37 C 0.2692(2) 0.61266(18) 0.42789(17) 0.0322(6) Uani 1 1 d . . . H37A H 0.3341 0.6343 0.4406 0.048 Uiso 1 1 calc R . . H37B H 0.2740 0.5580 0.4544 0.048 Uiso 1 1 calc R . . H37C H 0.2344 0.6511 0.4496 0.048 Uiso 1 1 calc R . . C38 C 0.2091(2) 0.68640(16) 0.29882(19) 0.0307(6) Uani 1 1 d . . . H38A H 0.1744 0.7239 0.3215 0.046 Uiso 1 1 calc R . . H38B H 0.1737 0.6816 0.2379 0.046 Uiso 1 1 calc R . . H38C H 0.2736 0.7088 0.3112 0.046 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 Nb1 0.01639(12) 0.01293(11) 0.01644(12) 0.00029(6) 0.00851(8) 0.00138(6) S1 0.0182(3) 0.0140(3) 0.0202(3) 0.00072(19) 0.0094(2) -0.00061(19) S2 0.0192(3) 0.0169(3) 0.0233(3) -0.0006(2) 0.0112(2) -0.0027(2) O1 0.0206(8) 0.0177(8) 0.0254(8) 0.0036(7) 0.0092(7) 0.0041(6) O2 0.0233(8) 0.0194(8) 0.0252(8) -0.0032(7) 0.0095(7) -0.0067(6) O3 0.0231(8) 0.0286(9) 0.0297(9) -0.0038(7) 0.0174(7) -0.0038(7) O4 0.0237(8) 0.0191(8) 0.0293(9) 0.0032(7) 0.0099(7) -0.0020(7) N1 0.0154(9) 0.0150(9) 0.0197(9) -0.0007(7) 0.0092(7) -0.0012(7) N2 0.0164(9) 0.0139(9) 0.0216(9) -0.0029(7) 0.0095(7) -0.0026(7) N3 0.0252(10) 0.0203(10) 0.0219(10) 0.0009(8) 0.0124(8) 0.0042(8) N4 0.0220(9) 0.0192(10) 0.0206(10) 0.0014(8) 0.0104(8) 0.0031(8) N5 0.0216(9) 0.0189(10) 0.0255(10) -0.0050(8) 0.0113(8) -0.0012(8) C1 0.0147(10) 0.0185(11) 0.0225(11) 0.0009(9) 0.0104(9) 0.0021(8) C2 0.0172(10) 0.0163(11) 0.0217(11) 0.0017(9) 0.0103(9) 0.0010(8) C3 0.0238(11) 0.0194(11) 0.0221(11) -0.0020(9) 0.0110(9) -0.0027(9) C4 0.0222(11) 0.0290(13) 0.0202(11) 0.0029(10) 0.0079(9) -0.0002(10) C5 0.0209(11) 0.0241(12) 0.0281(12) 0.0078(10) 0.0106(10) 0.0035(9) C6 0.0184(11) 0.0178(11) 0.0297(12) 0.0025(9) 0.0125(9) 0.0028(9) C7 0.0316(13) 0.0161(12) 0.0381(14) 0.0030(10) 0.0161(11) 0.0037(10) C8 0.0218(11) 0.0116(10) 0.0231(11) -0.0009(8) 0.0118(9) -0.0004(8) C9 0.0259(11) 0.0119(10) 0.0228(11) -0.0020(8) 0.0153(9) -0.0024(9) C10 0.0248(11) 0.0174(11) 0.0238(12) -0.0009(9) 0.0125(9) -0.0020(9) C11 0.0306(12) 0.0210(12) 0.0231(12) -0.0059(9) 0.0135(10) -0.0072(10) C12 0.0309(13) 0.0193(12) 0.0306(13) -0.0077(10) 0.0199(11) -0.0052(10) C13 0.0223(11) 0.0137(11) 0.0307(12) -0.0037(9) 0.0148(10) -0.0027(9) C14 0.0287(13) 0.0241(13) 0.0363(14) 0.0004(10) 0.0210(11) 0.0047(10) C15 0.0150(11) 0.0165(11) 0.0272(12) 0.0057(9) 0.0099(9) 0.0017(8) C16 0.0271(13) 0.0151(11) 0.0279(13) 0.0044(9) 0.0168(11) 0.0004(9) C17 0.0313(13) 0.0237(12) 0.0305(13) 0.0055(10) 0.0209(11) 0.0041(10) C18 0.0341(14) 0.0269(14) 0.0435(16) 0.0160(12) 0.0277(12) 0.0109(11) C19 0.0229(12) 0.0278(14) 0.0427(15) 0.0159(12) 0.0169(11) 0.0075(10) C20 0.0221(13) 0.0222(13) 0.0289(14) 0.0089(9) 0.0117(11) 0.0012(9) C21 0.0268(13) 0.0259(14) 0.0220(13) -0.0021(9) 0.0127(11) -0.0010(9) C22 0.0503(19) 0.054(2) 0.063(2) 0.0205(17) 0.0416(17) 0.0249(16) C23 0.0239(13) 0.0435(17) 0.0308(14) 0.0052(13) 0.0051(11) -0.0014(12) C24 0.0195(11) 0.0224(12) 0.0282(12) -0.0019(10) 0.0098(9) -0.0098(9) C25 0.0378(14) 0.0241(13) 0.0320(13) -0.0031(10) 0.0222(11) -0.0120(11) C26 0.0600(19) 0.0284(14) 0.0314(14) -0.0078(11) 0.0284(14) -0.0216(13) C27 0.0574(19) 0.0427(18) 0.0250(14) 0.0022(12) 0.0117(13) -0.0292(15) C28 0.0326(14) 0.0387(16) 0.0310(14) 0.0103(12) 0.0033(11) -0.0179(12) C29 0.0215(11) 0.0297(14) 0.0323(13) 0.0042(11) 0.0090(10) -0.0113(10) C30 0.0465(16) 0.0231(13) 0.0502(17) -0.0104(12) 0.0306(14) -0.0049(12) C31 0.097(3) 0.063(3) 0.0309(17) -0.0004(16) -0.0028(18) -0.050(2) C32 0.0198(12) 0.0321(15) 0.0484(17) 0.0087(13) 0.0065(11) 0.0033(11) C33 0.0483(18) 0.0345(15) 0.0432(17) 0.0119(12) 0.0357(15) 0.0154(13) C34 0.0284(12) 0.0223(12) 0.0217(11) 0.0057(9) 0.0120(10) 0.0047(10) C35 0.0249(12) 0.0343(15) 0.0295(13) 0.0036(11) 0.0103(10) 0.0148(11) C36 0.0253(12) 0.0284(13) 0.0221(12) 0.0036(10) 0.0090(9) 0.0025(10) C37 0.0305(13) 0.0316(14) 0.0289(13) -0.0142(11) 0.0061(11) 0.0024(11) C38 0.0394(14) 0.0154(12) 0.0429(15) -0.0053(11) 0.0223(12) -0.0022(11) _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 Nb1 N3 1.935(2) . ? Nb1 N4 1.9474(19) . ? Nb1 N5 2.010(2) . ? Nb1 N1 2.1149(18) . ? Nb1 N2 2.2780(18) . ? S1 O2 1.4357(17) . ? S1 O1 1.4393(17) . ? S1 N1 1.6283(19) . ? S1 C15 1.789(2) . ? S2 O3 1.4376(17) . ? S2 O4 1.4408(18) . ? S2 N2 1.6198(19) . ? S2 C24 1.797(2) . ? N1 C2 1.443(3) . ? N2 C9 1.445(3) . ? N3 C34 1.455(3) . ? N3 C33 1.459(3) . ? N4 C35 1.452(3) . ? N4 C36 1.453(3) . ? N5 C38 1.458(3) . ? N5 C37 1.459(3) . ? C1 C6 1.402(3) . ? C1 C2 1.405(3) . ? C1 C8 1.489(3) . ? C2 C3 1.396(3) . ? C3 C4 1.389(3) . ? C3 H3A 0.9500 . ? C4 C5 1.384(4) . ? C4 H4A 0.9500 . ? C5 C6 1.398(4) . ? C5 H5A 0.9500 . ? C6 C7 1.510(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.405(3) . ? C8 C13 1.407(3) . ? C9 C10 1.395(3) . ? C10 C11 1.379(3) . ? C10 H10 0.9500 . ? C11 C12 1.386(4) . ? C11 H11 0.9500 . ? C12 C13 1.390(4) . ? C12 H12 0.9500 . ? C13 C14 1.512(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.403(4) . ? C15 C20 1.427(3) . ? C16 C17 1.396(3) . ? C16 C21 1.498(4) . ? C17 C18 1.379(4) . ? C17 H17 0.9500 . ? C18 C19 1.381(4) . ? C18 C22 1.512(4) . ? C19 C20 1.390(4) . ? C19 H19 0.9500 . ? C20 C23 1.510(4) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.409(4) . ? C24 C29 1.412(4) . ? C25 C26 1.398(4) . ? C25 C30 1.509(4) . ? C26 C27 1.385(5) . ? C26 H26 0.9500 . ? C27 C28 1.381(5) . ? C27 C31 1.510(4) . ? C28 C29 1.388(4) . ? C28 H28 0.9500 . ? C29 C32 1.507(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Nb1 N4 117.09(8) . . ? N3 Nb1 N5 89.22(8) . . ? N4 Nb1 N5 89.22(8) . . ? N3 Nb1 N1 121.20(8) . . ? N4 Nb1 N1 121.61(8) . . ? N5 Nb1 N1 94.58(8) . . ? N3 Nb1 N2 91.99(8) . . ? N4 Nb1 N2 94.09(8) . . ? N5 Nb1 N2 175.48(7) . . ? N1 Nb1 N2 81.06(7) . . ? O2 S1 O1 116.10(10) . . ? O2 S1 N1 112.61(10) . . ? O1 S1 N1 105.10(10) . . ? O2 S1 C15 108.15(11) . . ? O1 S1 C15 109.42(11) . . ? N1 S1 C15 104.86(10) . . ? O3 S2 O4 115.85(11) . . ? O3 S2 N2 108.61(10) . . ? O4 S2 N2 111.20(10) . . ? O3 S2 C24 107.08(11) . . ? O4 S2 C24 107.25(11) . . ? N2 S2 C24 106.35(10) . . ? C2 N1 S1 119.14(15) . . ? C2 N1 Nb1 106.86(13) . . ? S1 N1 Nb1 120.95(11) . . ? C9 N2 S2 111.53(14) . . ? C9 N2 Nb1 122.13(13) . . ? S2 N2 Nb1 124.97(10) . . ? C34 N3 C33 111.5(2) . . ? C34 N3 Nb1 127.43(15) . . ? C33 N3 Nb1 120.99(17) . . ? C35 N4 C36 113.03(19) . . ? C35 N4 Nb1 131.28(16) . . ? C36 N4 Nb1 115.30(15) . . ? C38 N5 C37 108.9(2) . . ? C38 N5 Nb1 126.26(17) . . ? C37 N5 Nb1 124.44(17) . . ? C6 C1 C2 119.3(2) . . ? C6 C1 C8 123.2(2) . . ? C2 C1 C8 117.5(2) . . ? C3 C2 C1 120.9(2) . . ? C3 C2 N1 121.3(2) . . ? C1 C2 N1 117.5(2) . . ? C4 C3 C2 119.6(2) . . ? C4 C3 H3A 120.2 . . ? C2 C3 H3A 120.2 . . ? C5 C4 C3 119.5(2) . . ? C5 C4 H4A 120.3 . . ? C3 C4 H4A 120.3 . . ? C4 C5 C6 121.9(2) . . ? C4 C5 H5A 119.0 . . ? C6 C5 H5A 119.0 . . ? C5 C6 C1 118.7(2) . . ? C5 C6 C7 118.7(2) . . ? C1 C6 C7 122.6(2) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C13 119.5(2) . . ? C9 C8 C1 120.0(2) . . ? C13 C8 C1 120.3(2) . . ? C10 C9 C8 119.8(2) . . ? C10 C9 N2 119.8(2) . . ? C8 C9 N2 120.4(2) . . ? C11 C10 C9 120.3(2) . . ? C11 C10 H10 119.8 . . ? C9 C10 H10 119.8 . . ? C10 C11 C12 120.1(2) . . ? C10 C11 H11 119.9 . . ? C12 C11 H11 119.9 . . ? C11 C12 C13 120.8(2) . . ? C11 C12 H12 119.6 . . ? C13 C12 H12 119.6 . . ? C12 C13 C8 119.3(2) . . ? C12 C13 C14 119.6(2) . . ? C8 C13 C14 121.0(2) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 121.0(2) . . ? C16 C15 S1 118.23(18) . . ? C20 C15 S1 120.8(2) . . ? C17 C16 C15 118.4(2) . . ? C17 C16 C21 117.0(2) . . ? C15 C16 C21 124.6(2) . . ? C18 C17 C16 122.1(3) . . ? C18 C17 H17 118.9 . . ? C16 C17 H17 118.9 . . ? C17 C18 C19 118.3(2) . . ? C17 C18 C22 120.7(3) . . ? C19 C18 C22 121.0(3) . . ? C18 C19 C20 123.4(2) . . ? C18 C19 H19 118.3 . . ? C20 C19 H19 118.3 . . ? C19 C20 C15 116.8(3) . . ? C19 C20 C23 116.9(2) . . ? C15 C20 C23 126.3(2) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C25 C24 C29 121.0(2) . . ? C25 C24 S2 121.5(2) . . ? C29 C24 S2 117.5(2) . . ? C26 C25 C24 117.2(3) . . ? C26 C25 C30 117.1(3) . . ? C24 C25 C30 125.7(2) . . ? C27 C26 C25 123.2(3) . . ? C27 C26 H26 118.4 . . ? C25 C26 H26 118.4 . . ? C28 C27 C26 117.6(3) . . ? C28 C27 C31 121.6(4) . . ? C26 C27 C31 120.8(4) . . ? C27 C28 C29 122.8(3) . . ? C27 C28 H28 118.6 . . ? C29 C28 H28 118.6 . . ? C28 C29 C24 118.1(3) . . ? C28 C29 C32 117.4(3) . . ? C24 C29 C32 124.5(2) . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C27 C31 H31A 109.5 . . ? C27 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C27 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N3 C33 H33A 109.5 . . ? N3 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N3 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N3 C34 H34A 109.5 . . ? N3 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N3 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N4 C35 H35A 109.5 . . ? N4 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N4 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N4 C36 H36A 109.5 . . ? N4 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N4 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N5 C37 H37A 109.5 . . ? N5 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N5 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N5 C38 H38A 109.5 . . ? N5 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N5 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 S1 N1 C2 -54.62(19) . . . . ? O1 S1 N1 C2 178.07(16) . . . . ? C15 S1 N1 C2 62.73(19) . . . . ? O2 S1 N1 Nb1 81.56(13) . . . . ? O1 S1 N1 Nb1 -45.75(14) . . . . ? C15 S1 N1 Nb1 -161.09(12) . . . . ? N3 Nb1 N1 C2 15.05(17) . . . . ? N4 Nb1 N1 C2 -161.17(13) . . . . ? N5 Nb1 N1 C2 106.92(15) . . . . ? N2 Nb1 N1 C2 -71.85(14) . . . . ? N3 Nb1 N1 S1 -125.76(12) . . . . ? N4 Nb1 N1 S1 58.02(15) . . . . ? N5 Nb1 N1 S1 -33.89(13) . . . . ? N2 Nb1 N1 S1 147.34(13) . . . . ? O3 S2 N2 C9 -172.51(15) . . . . ? O4 S2 N2 C9 58.88(18) . . . . ? C24 S2 N2 C9 -57.57(18) . . . . ? O3 S2 N2 Nb1 20.66(15) . . . . ? O4 S2 N2 Nb1 -107.95(13) . . . . ? C24 S2 N2 Nb1 135.60(13) . . . . ? N3 Nb1 N2 C9 -143.20(17) . . . . ? N4 Nb1 N2 C9 99.46(17) . . . . ? N5 Nb1 N2 C9 -37.6(10) . . . . ? N1 Nb1 N2 C9 -21.92(17) . . . . ? N3 Nb1 N2 S2 22.30(13) . . . . ? N4 Nb1 N2 S2 -95.04(13) . . . . ? N5 Nb1 N2 S2 127.9(9) . . . . ? N1 Nb1 N2 S2 143.59(13) . . . . ? N4 Nb1 N3 C34 149.27(19) . . . . ? N5 Nb1 N3 C34 -122.0(2) . . . . ? N1 Nb1 N3 C34 -27.1(2) . . . . ? N2 Nb1 N3 C34 53.6(2) . . . . ? N4 Nb1 N3 C33 -27.8(2) . . . . ? N5 Nb1 N3 C33 60.9(2) . . . . ? N1 Nb1 N3 C33 155.8(2) . . . . ? N2 Nb1 N3 C33 -123.4(2) . . . . ? N3 Nb1 N4 C35 38.9(3) . . . . ? N5 Nb1 N4 C35 -49.8(2) . . . . ? N1 Nb1 N4 C35 -144.7(2) . . . . ? N2 Nb1 N4 C35 133.3(2) . . . . ? N3 Nb1 N4 C36 -148.86(16) . . . . ? N5 Nb1 N4 C36 122.41(17) . . . . ? N1 Nb1 N4 C36 27.5(2) . . . . ? N2 Nb1 N4 C36 -54.52(17) . . . . ? N3 Nb1 N5 C38 -152.4(2) . . . . ? N4 Nb1 N5 C38 -35.3(2) . . . . ? N1 Nb1 N5 C38 86.4(2) . . . . ? N2 Nb1 N5 C38 101.9(10) . . . . ? N3 Nb1 N5 C37 35.8(2) . . . . ? N4 Nb1 N5 C37 152.9(2) . . . . ? N1 Nb1 N5 C37 -85.5(2) . . . . ? N2 Nb1 N5 C37 -69.9(10) . . . . ? C6 C1 C2 C3 1.6(3) . . . . ? C8 C1 C2 C3 -177.7(2) . . . . ? C6 C1 C2 N1 -172.09(19) . . . . ? C8 C1 C2 N1 8.6(3) . . . . ? S1 N1 C2 C3 60.6(3) . . . . ? Nb1 N1 C2 C3 -81.1(2) . . . . ? S1 N1 C2 C1 -125.69(19) . . . . ? Nb1 N1 C2 C1 92.7(2) . . . . ? C1 C2 C3 C4 1.2(3) . . . . ? N1 C2 C3 C4 174.7(2) . . . . ? C2 C3 C4 C5 -2.1(4) . . . . ? C3 C4 C5 C6 0.1(4) . . . . ? C4 C5 C6 C1 2.6(4) . . . . ? C4 C5 C6 C7 -175.4(2) . . . . ? C2 C1 C6 C5 -3.5(3) . . . . ? C8 C1 C6 C5 175.8(2) . . . . ? C2 C1 C6 C7 174.5(2) . . . . ? C8 C1 C6 C7 -6.2(3) . . . . ? C6 C1 C8 C9 116.3(3) . . . . ? C2 C1 C8 C9 -64.4(3) . . . . ? C6 C1 C8 C13 -68.7(3) . . . . ? C2 C1 C8 C13 110.6(2) . . . . ? C13 C8 C9 C10 -1.0(3) . . . . ? C1 C8 C9 C10 174.0(2) . . . . ? C13 C8 C9 N2 -179.9(2) . . . . ? C1 C8 C9 N2 -4.9(3) . . . . ? S2 N2 C9 C10 83.5(2) . . . . ? Nb1 N2 C9 C10 -109.3(2) . . . . ? S2 N2 C9 C8 -97.6(2) . . . . ? Nb1 N2 C9 C8 69.6(2) . . . . ? C8 C9 C10 C11 2.3(3) . . . . ? N2 C9 C10 C11 -178.7(2) . . . . ? C9 C10 C11 C12 -0.9(4) . . . . ? C10 C11 C12 C13 -2.0(4) . . . . ? C11 C12 C13 C8 3.3(4) . . . . ? C11 C12 C13 C14 -174.6(2) . . . . ? C9 C8 C13 C12 -1.8(3) . . . . ? C1 C8 C13 C12 -176.7(2) . . . . ? C9 C8 C13 C14 176.1(2) . . . . ? C1 C8 C13 C14 1.1(3) . . . . ? O2 S1 C15 C16 -162.61(18) . . . . ? O1 S1 C15 C16 -35.3(2) . . . . ? N1 S1 C15 C16 77.0(2) . . . . ? O2 S1 C15 C20 16.4(2) . . . . ? O1 S1 C15 C20 143.77(18) . . . . ? N1 S1 C15 C20 -103.9(2) . . . . ? C20 C15 C16 C17 0.4(3) . . . . ? S1 C15 C16 C17 179.44(18) . . . . ? C20 C15 C16 C21 -179.4(2) . . . . ? S1 C15 C16 C21 -0.4(3) . . . . ? C15 C16 C17 C18 0.2(4) . . . . ? C21 C16 C17 C18 -180.0(2) . . . . ? C16 C17 C18 C19 -0.5(4) . . . . ? C16 C17 C18 C22 178.2(3) . . . . ? C17 C18 C19 C20 0.2(4) . . . . ? C22 C18 C19 C20 -178.5(3) . . . . ? C18 C19 C20 C15 0.4(4) . . . . ? C18 C19 C20 C23 -179.3(3) . . . . ? C16 C15 C20 C19 -0.7(3) . . . . ? S1 C15 C20 C19 -179.69(18) . . . . ? C16 C15 C20 C23 179.0(2) . . . . ? S1 C15 C20 C23 0.0(3) . . . . ? O3 S2 C24 C25 -144.75(19) . . . . ? O4 S2 C24 C25 -19.8(2) . . . . ? N2 S2 C24 C25 99.3(2) . . . . ? O3 S2 C24 C29 38.1(2) . . . . ? O4 S2 C24 C29 163.06(18) . . . . ? N2 S2 C24 C29 -77.9(2) . . . . ? C29 C24 C25 C26 -1.6(4) . . . . ? S2 C24 C25 C26 -178.70(18) . . . . ? C29 C24 C25 C30 176.3(2) . . . . ? S2 C24 C25 C30 -0.8(4) . . . . ? C24 C25 C26 C27 0.7(4) . . . . ? C30 C25 C26 C27 -177.4(3) . . . . ? C25 C26 C27 C28 0.3(4) . . . . ? C25 C26 C27 C31 -178.4(3) . . . . ? C26 C27 C28 C29 -0.4(4) . . . . ? C31 C27 C28 C29 178.3(3) . . . . ? C27 C28 C29 C24 -0.6(4) . . . . ? C27 C28 C29 C32 178.4(3) . . . . ? C25 C24 C29 C28 1.6(4) . . . . ? S2 C24 C29 C28 178.77(19) . . . . ? C25 C24 C29 C32 -177.3(2) . . . . ? S2 C24 C29 C32 -0.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 72.57 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.489 _refine_diff_density_min -0.865 _refine_diff_density_rms 0.084 # Attachment '- compound 21.cif' data_compound21 _database_code_depnum_ccdc_archive 'CCDC 791866' #TrackingRef '- compound 21.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C38 H52 N5 O4 S2 Ta' _chemical_formula_sum 'C38 H52 N5 O4 S2 Ta' _chemical_formula_weight 887.92 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ta Ta -5.7959 5.2718 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.1810(16) _cell_length_b 16.0520(18) _cell_length_c 17.371(2) _cell_angle_alpha 90.00 _cell_angle_beta 113.3250(10) _cell_angle_gamma 90.00 _cell_volume 3887.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 5069 _cell_measurement_theta_min 27.50 _cell_measurement_theta_max 72.20 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.517 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 6.583 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3253 _exptl_absorpt_correction_T_max 0.3837 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Rigaku Saturn70 CCD camera' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 40234 _diffrn_reflns_av_R_equivalents 0.0456 _diffrn_reflns_av_sigmaI/netI 0.0283 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.17 _diffrn_reflns_theta_max 72.26 _reflns_number_total 7532 _reflns_number_gt 7251 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear-SM Expert 2.0 r4 (Rigaku, 2009)' _computing_cell_refinement 'CrystalClear-SM Expert 2.0 r4' _computing_data_reduction 'CrystalClear-SM Expert 2.0 r4' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure 4.0' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2009)' _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^)+(0.0438P)^2^+1.7090P] 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 7532 _refine_ls_number_parameters 465 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0306 _refine_ls_R_factor_gt 0.0296 _refine_ls_wR_factor_ref 0.0781 _refine_ls_wR_factor_gt 0.0771 _refine_ls_goodness_of_fit_ref 1.144 _refine_ls_restrained_S_all 1.144 _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 Ta1 Ta 0.180395(8) 0.495767(6) 0.276758(7) 0.01228(6) Uani 1 1 d . . . S1 S 0.37417(4) 0.55598(4) 0.25466(4) 0.01496(12) Uani 1 1 d . . . S2 S 0.08723(4) 0.29706(4) 0.22758(4) 0.01663(13) Uani 1 1 d . . . O1 O 0.30467(13) 0.60663(11) 0.19095(11) 0.0194(4) Uani 1 1 d . . . O2 O 0.42995(13) 0.59675(11) 0.33237(11) 0.0208(4) Uani 1 1 d . . . O3 O 0.02702(13) 0.33243(12) 0.26561(12) 0.0232(4) Uani 1 1 d . . . O4 O 0.14768(14) 0.22905(11) 0.27208(12) 0.0222(4) Uani 1 1 d . . . N1 N 0.31339(15) 0.47771(14) 0.26759(13) 0.0140(4) Uani 1 1 d . . . N2 N 0.15088(14) 0.37119(13) 0.21096(13) 0.0143(4) Uani 1 1 d . . . N3 N 0.15796(16) 0.45207(14) 0.37148(14) 0.0198(5) Uani 1 1 d . . . N4 N 0.07308(15) 0.55038(14) 0.18845(13) 0.0174(4) Uani 1 1 d . . . N5 N 0.21761(16) 0.60534(14) 0.33670(14) 0.0199(5) Uani 1 1 d . . . C1 C 0.35186(17) 0.33002(16) 0.29517(16) 0.0158(5) Uani 1 1 d . . . C2 C 0.36287(17) 0.41190(15) 0.32607(16) 0.0153(5) Uani 1 1 d . . . C3 C 0.41314(18) 0.42887(17) 0.41116(16) 0.0187(5) Uani 1 1 d . . . H3A H 0.4197 0.4845 0.4313 0.022 Uiso 1 1 calc R . . C4 C 0.45356(19) 0.36315(18) 0.46611(17) 0.0224(5) Uani 1 1 d . . . H4A H 0.4895 0.3738 0.5240 0.027 Uiso 1 1 calc R . . C5 C 0.44133(19) 0.28215(18) 0.43623(17) 0.0217(5) Uani 1 1 d . . . H5A H 0.4691 0.2378 0.4744 0.026 Uiso 1 1 calc R . . C6 C 0.38925(18) 0.26376(16) 0.35149(17) 0.0186(5) Uani 1 1 d . . . C7 C 0.3714(2) 0.17388(17) 0.32511(19) 0.0262(6) Uani 1 1 d . . . H7A H 0.3234 0.1506 0.3436 0.039 Uiso 1 1 calc R . . H7B H 0.4314 0.1424 0.3506 0.039 Uiso 1 1 calc R . . H7C H 0.3479 0.1701 0.2639 0.039 Uiso 1 1 calc R . . C8 C 0.30011(18) 0.31823(15) 0.20268(16) 0.0162(5) Uani 1 1 d . . . C9 C 0.20315(18) 0.34193(15) 0.16248(16) 0.0149(5) Uani 1 1 d . . . C10 C 0.15768(19) 0.33815(16) 0.07557(16) 0.0185(5) Uani 1 1 d . . . H10 H 0.0931 0.3563 0.0485 0.022 Uiso 1 1 calc R . . C11 C 0.2058(2) 0.30810(17) 0.02810(17) 0.0225(6) Uani 1 1 d . . . H11 H 0.1738 0.3043 -0.0311 0.027 Uiso 1 1 calc R . . C12 C 0.3008(2) 0.28365(17) 0.06740(17) 0.0223(6) Uani 1 1 d . . . H12 H 0.3331 0.2622 0.0347 0.027 Uiso 1 1 calc R . . C13 C 0.34990(19) 0.29001(15) 0.15430(17) 0.0188(5) Uani 1 1 d . . . C14 C 0.4553(2) 0.26956(18) 0.19418(19) 0.0257(6) Uani 1 1 d . . . H14A H 0.4795 0.2599 0.1503 0.039 Uiso 1 1 calc R . . H14B H 0.4649 0.2193 0.2286 0.039 Uiso 1 1 calc R . . H14C H 0.4902 0.3162 0.2296 0.039 Uiso 1 1 calc R . . C15 C 0.4552(2) 0.51100(16) 0.21449(19) 0.0173(5) Uani 1 1 d . . . C16 C 0.4195(2) 0.48895(16) 0.1292(2) 0.0194(6) Uani 1 1 d . . . C17 C 0.4826(2) 0.45501(18) 0.09678(18) 0.0239(6) Uani 1 1 d . . . H17 H 0.4588 0.4402 0.0392 0.029 Uiso 1 1 calc R . . C18 C 0.5782(2) 0.44241(19) 0.1461(2) 0.0298(7) Uani 1 1 d . . . C19 C 0.6120(2) 0.46511(19) 0.2301(2) 0.0281(6) Uani 1 1 d . . . H19 H 0.6781 0.4569 0.2640 0.034 Uiso 1 1 calc R . . C20 C 0.5536(2) 0.49941(15) 0.2673(2) 0.0215(6) Uani 1 1 d . . . C21 C 0.3163(2) 0.49984(16) 0.0687(2) 0.0218(6) Uani 1 1 d . . . H21A H 0.3024 0.5593 0.0573 0.033 Uiso 1 1 calc R . . H21B H 0.2738 0.4766 0.0934 0.033 Uiso 1 1 calc R . . H21C H 0.3058 0.4707 0.0162 0.033 Uiso 1 1 calc R . . C22 C 0.6439(3) 0.4030(2) 0.1103(3) 0.0463(9) Uani 1 1 d . . . H22A H 0.6580 0.3456 0.1305 0.069 Uiso 1 1 calc R . . H22B H 0.7038 0.4348 0.1281 0.069 Uiso 1 1 calc R . . H22C H 0.6126 0.4030 0.0489 0.069 Uiso 1 1 calc R . . C23 C 0.6017(2) 0.5217(2) 0.3590(2) 0.0322(7) Uani 1 1 d . . . H23A H 0.6670 0.4991 0.3821 0.048 Uiso 1 1 calc R . . H23B H 0.5651 0.4979 0.3892 0.048 Uiso 1 1 calc R . . H23C H 0.6043 0.5824 0.3652 0.048 Uiso 1 1 calc R . . C24 C 0.00971(19) 0.25874(17) 0.12614(17) 0.0215(5) Uani 1 1 d . . . C25 C 0.0325(2) 0.18600(18) 0.09184(18) 0.0266(6) Uani 1 1 d . . . C26 C -0.0306(3) 0.1616(2) 0.01223(19) 0.0342(7) Uani 1 1 d . . . H26 H -0.0162 0.1127 -0.0113 0.041 Uiso 1 1 calc R . . C27 C -0.1134(3) 0.2051(2) -0.03437(19) 0.0405(9) Uani 1 1 d . . . C28 C -0.1333(2) 0.2770(2) 0.0003(2) 0.0359(8) Uani 1 1 d . . . H28 H -0.1896 0.3079 -0.0310 0.043 Uiso 1 1 calc R . . C29 C -0.0731(2) 0.30535(18) 0.07957(18) 0.0254(6) Uani 1 1 d . . . C30 C 0.1214(2) 0.13318(19) 0.1334(2) 0.0326(7) Uani 1 1 d . . . H30A H 0.1215 0.0879 0.0956 0.049 Uiso 1 1 calc R . . H30B H 0.1217 0.1097 0.1856 0.049 Uiso 1 1 calc R . . H30C H 0.1787 0.1678 0.1460 0.049 Uiso 1 1 calc R . . C31 C -0.1804(4) 0.1744(3) -0.1195(2) 0.0690(16) Uani 1 1 d . . . H31A H -0.1444 0.1660 -0.1549 0.103 Uiso 1 1 calc R . . H31B H -0.2311 0.2157 -0.1456 0.103 Uiso 1 1 calc R . . H31C H -0.2093 0.1215 -0.1134 0.103 Uiso 1 1 calc R . . C32 C -0.1012(2) 0.3855(2) 0.1096(2) 0.0325(7) Uani 1 1 d . . . H32A H -0.1486 0.4151 0.0618 0.049 Uiso 1 1 calc R . . H32B H -0.0443 0.4206 0.1360 0.049 Uiso 1 1 calc R . . H32C H -0.1289 0.3728 0.1505 0.049 Uiso 1 1 calc R . . C33 C 0.0876(3) 0.4901(2) 0.3987(2) 0.0338(8) Uani 1 1 d . . . H33A H 0.0315 0.4535 0.3837 0.051 Uiso 1 1 calc R . . H33B H 0.0677 0.5441 0.3710 0.051 Uiso 1 1 calc R . . H33C H 0.1163 0.4980 0.4596 0.051 Uiso 1 1 calc R . . C34 C 0.2011(2) 0.37842(17) 0.42150(17) 0.0218(5) Uani 1 1 d . . . H34A H 0.2408 0.3953 0.4791 0.033 Uiso 1 1 calc R . . H34B H 0.2412 0.3498 0.3973 0.033 Uiso 1 1 calc R . . H34C H 0.1504 0.3407 0.4216 0.033 Uiso 1 1 calc R . . C35 C -0.0010(2) 0.60510(19) 0.19370(19) 0.0281(6) Uani 1 1 d . . . H35A H 0.0008 0.6586 0.1672 0.042 Uiso 1 1 calc R . . H35B H 0.0104 0.6142 0.2527 0.042 Uiso 1 1 calc R . . H35C H -0.0641 0.5792 0.1647 0.042 Uiso 1 1 calc R . . C36 C 0.0692(2) 0.54337(18) 0.10374(17) 0.0229(6) Uani 1 1 d . . . H36A H 0.0082 0.5180 0.0674 0.034 Uiso 1 1 calc R . . H36B H 0.1224 0.5085 0.1042 0.034 Uiso 1 1 calc R . . H36C H 0.0745 0.5989 0.0826 0.034 Uiso 1 1 calc R . . C37 C 0.2706(2) 0.6143(2) 0.42730(19) 0.0307(7) Uani 1 1 d . . . H37A H 0.3354 0.6347 0.4389 0.046 Uiso 1 1 calc R . . H37B H 0.2744 0.5602 0.4545 0.046 Uiso 1 1 calc R . . H37C H 0.2373 0.6542 0.4492 0.046 Uiso 1 1 calc R . . C38 C 0.2082(2) 0.68692(17) 0.2971(2) 0.0283(6) Uani 1 1 d . . . H38A H 0.1743 0.7248 0.3203 0.042 Uiso 1 1 calc R . . H38B H 0.1719 0.6814 0.2365 0.042 Uiso 1 1 calc R . . H38C H 0.2721 0.7093 0.3081 0.042 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 Ta1 0.01533(9) 0.01223(8) 0.01098(9) 0.00022(4) 0.00703(6) 0.00136(4) S1 0.0171(3) 0.0135(3) 0.0155(3) 0.0006(2) 0.0079(2) -0.0006(2) S2 0.0179(3) 0.0164(3) 0.0183(3) -0.0007(2) 0.0101(2) -0.0029(2) O1 0.0218(9) 0.0177(9) 0.0194(9) 0.0033(7) 0.0089(7) 0.0039(7) O2 0.0215(9) 0.0205(9) 0.0200(9) -0.0015(7) 0.0079(8) -0.0061(7) O3 0.0227(9) 0.0277(10) 0.0263(10) -0.0038(8) 0.0172(8) -0.0040(8) O4 0.0255(9) 0.0167(9) 0.0250(10) 0.0023(7) 0.0107(8) -0.0014(8) N1 0.0154(10) 0.0139(10) 0.0153(11) 0.0007(8) 0.0089(8) -0.0012(8) N2 0.0177(10) 0.0125(10) 0.0151(10) -0.0021(8) 0.0090(8) -0.0011(8) N3 0.0261(11) 0.0185(11) 0.0178(11) 0.0013(9) 0.0121(9) 0.0050(9) N4 0.0204(10) 0.0187(11) 0.0139(10) 0.0023(8) 0.0075(8) 0.0042(8) N5 0.0222(11) 0.0182(11) 0.0210(11) -0.0042(9) 0.0101(9) 0.0004(9) C1 0.0166(11) 0.0152(12) 0.0186(13) 0.0011(10) 0.0103(10) 0.0006(9) C2 0.0144(11) 0.0165(12) 0.0172(12) 0.0007(10) 0.0087(10) 0.0004(9) C3 0.0229(12) 0.0195(12) 0.0151(12) -0.0014(10) 0.0089(10) -0.0015(10) C4 0.0209(12) 0.0260(14) 0.0188(13) 0.0024(11) 0.0063(10) -0.0014(11) C5 0.0221(13) 0.0246(14) 0.0195(13) 0.0078(11) 0.0096(11) 0.0042(11) C6 0.0182(12) 0.0183(13) 0.0222(13) 0.0028(10) 0.0112(10) 0.0026(10) C7 0.0320(15) 0.0160(13) 0.0329(16) 0.0048(11) 0.0152(13) 0.0053(11) C8 0.0208(12) 0.0115(11) 0.0194(13) -0.0023(9) 0.0111(10) -0.0028(9) C9 0.0203(12) 0.0102(11) 0.0179(12) -0.0024(9) 0.0114(10) -0.0034(9) C10 0.0224(12) 0.0158(12) 0.0192(13) -0.0020(10) 0.0104(10) -0.0039(10) C11 0.0321(14) 0.0212(13) 0.0173(13) -0.0050(10) 0.0130(11) -0.0074(11) C12 0.0327(14) 0.0182(13) 0.0247(14) -0.0064(11) 0.0206(12) -0.0026(11) C13 0.0253(13) 0.0121(12) 0.0243(14) -0.0031(10) 0.0156(11) -0.0015(10) C14 0.0273(14) 0.0226(14) 0.0350(16) 0.0007(12) 0.0205(13) 0.0038(11) C15 0.0173(13) 0.0170(12) 0.0213(15) 0.0054(10) 0.0117(12) 0.0010(9) C16 0.0237(15) 0.0171(12) 0.0226(15) 0.0066(10) 0.0146(12) 0.0019(10) C17 0.0320(14) 0.0235(14) 0.0238(14) 0.0055(11) 0.0191(12) 0.0048(11) C18 0.0332(15) 0.0261(15) 0.0415(18) 0.0160(13) 0.0271(14) 0.0092(12) C19 0.0207(13) 0.0295(16) 0.0375(17) 0.0170(13) 0.0153(12) 0.0083(12) C20 0.0190(15) 0.0218(15) 0.0234(16) 0.0099(10) 0.0081(13) 0.0009(9) C21 0.0254(16) 0.0250(16) 0.0173(15) -0.0017(9) 0.0110(13) -0.0012(9) C22 0.049(2) 0.051(2) 0.057(2) 0.0214(18) 0.0410(19) 0.0245(17) C23 0.0227(15) 0.0441(17) 0.0254(16) 0.0084(14) 0.0048(12) 0.0009(14) C24 0.0234(13) 0.0221(13) 0.0210(13) -0.0002(10) 0.0111(11) -0.0087(10) C25 0.0361(15) 0.0258(14) 0.0257(15) -0.0032(11) 0.0205(13) -0.0130(12) C26 0.056(2) 0.0294(16) 0.0258(16) -0.0079(12) 0.0248(15) -0.0231(15) C27 0.054(2) 0.043(2) 0.0197(15) -0.0005(14) 0.0089(14) -0.0321(17) C28 0.0309(16) 0.0387(18) 0.0279(16) 0.0122(14) 0.0006(13) -0.0178(14) C29 0.0225(13) 0.0273(15) 0.0263(15) 0.0054(12) 0.0093(11) -0.0093(11) C30 0.0403(17) 0.0205(14) 0.0454(19) -0.0100(13) 0.0258(15) -0.0055(12) C31 0.095(3) 0.062(3) 0.0243(19) -0.0009(18) -0.003(2) -0.049(3) C32 0.0201(13) 0.0327(16) 0.0407(18) 0.0071(14) 0.0078(13) 0.0011(12) C33 0.045(2) 0.0350(17) 0.036(2) 0.0135(13) 0.0320(17) 0.0168(14) C34 0.0283(14) 0.0219(13) 0.0171(13) 0.0043(10) 0.0110(11) 0.0032(11) C35 0.0280(14) 0.0318(16) 0.0244(15) 0.0024(12) 0.0101(12) 0.0137(12) C36 0.0260(13) 0.0273(14) 0.0158(13) 0.0035(11) 0.0088(11) 0.0029(11) C37 0.0312(15) 0.0328(16) 0.0231(15) -0.0136(12) 0.0054(12) 0.0036(13) C38 0.0396(16) 0.0142(13) 0.0374(17) -0.0044(12) 0.0221(14) -0.0011(12) _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 Ta1 N3 1.939(2) . ? Ta1 N4 1.948(2) . ? Ta1 N5 2.008(2) . ? Ta1 N1 2.107(2) . ? Ta1 N2 2.258(2) . ? S1 O2 1.4361(19) . ? S1 O1 1.4403(18) . ? S1 N1 1.626(2) . ? S1 C15 1.789(3) . ? S2 O4 1.4386(19) . ? S2 O3 1.4396(19) . ? S2 N2 1.629(2) . ? S2 C24 1.796(3) . ? N1 C2 1.452(3) . ? N2 C9 1.445(3) . ? N3 C34 1.460(3) . ? N3 C33 1.462(4) . ? N4 C36 1.454(3) . ? N4 C35 1.458(3) . ? N5 C38 1.459(4) . ? N5 C37 1.464(4) . ? C1 C6 1.404(4) . ? C1 C2 1.404(3) . ? C1 C8 1.495(4) . ? C2 C3 1.396(4) . ? C3 C4 1.392(4) . ? C3 H3A 0.9500 . ? C4 C5 1.385(4) . ? C4 H4A 0.9500 . ? C5 C6 1.399(4) . ? C5 H5A 0.9500 . ? C6 C7 1.505(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.409(4) . ? C8 C13 1.409(4) . ? C9 C10 1.391(4) . ? C10 C11 1.387(4) . ? C10 H10 0.9500 . ? C11 C12 1.385(4) . ? C11 H11 0.9500 . ? C12 C13 1.398(4) . ? C12 H12 0.9500 . ? C13 C14 1.507(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.407(4) . ? C15 C20 1.422(4) . ? C16 C17 1.399(4) . ? C16 C21 1.511(4) . ? C17 C18 1.378(4) . ? C17 H17 0.9500 . ? C18 C19 1.390(5) . ? C18 C22 1.508(4) . ? C19 C20 1.400(4) . ? C19 H19 0.9500 . ? C20 C23 1.509(5) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C29 1.411(4) . ? C24 C25 1.415(4) . ? C25 C26 1.391(4) . ? C25 C30 1.514(5) . ? C26 C27 1.385(5) . ? C26 H26 0.9500 . ? C27 C28 1.389(5) . ? C27 C31 1.508(4) . ? C28 C29 1.393(4) . ? C28 H28 0.9500 . ? C29 C32 1.512(4) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Ta1 N4 117.24(9) . . ? N3 Ta1 N5 89.12(9) . . ? N4 Ta1 N5 89.43(9) . . ? N3 Ta1 N1 120.65(9) . . ? N4 Ta1 N1 122.00(9) . . ? N5 Ta1 N1 94.50(9) . . ? N3 Ta1 N2 92.46(8) . . ? N4 Ta1 N2 93.63(8) . . ? N5 Ta1 N2 175.45(8) . . ? N1 Ta1 N2 81.02(8) . . ? O2 S1 O1 116.43(11) . . ? O2 S1 N1 112.20(11) . . ? O1 S1 N1 105.01(11) . . ? O2 S1 C15 108.07(13) . . ? O1 S1 C15 109.61(12) . . ? N1 S1 C15 104.91(12) . . ? O4 S2 O3 116.01(12) . . ? O4 S2 N2 110.65(11) . . ? O3 S2 N2 108.79(11) . . ? O4 S2 C24 107.34(12) . . ? O3 S2 C24 107.26(12) . . ? N2 S2 C24 106.29(11) . . ? C2 N1 S1 119.61(16) . . ? C2 N1 Ta1 107.04(14) . . ? S1 N1 Ta1 121.14(12) . . ? C9 N2 S2 111.52(16) . . ? C9 N2 Ta1 122.55(15) . . ? S2 N2 Ta1 124.74(11) . . ? C34 N3 C33 111.0(2) . . ? C34 N3 Ta1 127.56(17) . . ? C33 N3 Ta1 121.32(18) . . ? C36 N4 C35 112.8(2) . . ? C36 N4 Ta1 116.61(17) . . ? C35 N4 Ta1 130.31(18) . . ? C38 N5 C37 109.1(2) . . ? C38 N5 Ta1 125.94(18) . . ? C37 N5 Ta1 124.47(19) . . ? C6 C1 C2 119.2(2) . . ? C6 C1 C8 123.3(2) . . ? C2 C1 C8 117.5(2) . . ? C3 C2 C1 121.3(2) . . ? C3 C2 N1 120.9(2) . . ? C1 C2 N1 117.6(2) . . ? C4 C3 C2 119.1(2) . . ? C4 C3 H3A 120.5 . . ? C2 C3 H3A 120.5 . . ? C5 C4 C3 119.8(3) . . ? C5 C4 H4A 120.1 . . ? C3 C4 H4A 120.1 . . ? C4 C5 C6 121.9(2) . . ? C4 C5 H5A 119.0 . . ? C6 C5 H5A 119.0 . . ? C5 C6 C1 118.5(2) . . ? C5 C6 C7 118.8(2) . . ? C1 C6 C7 122.7(2) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C13 119.5(2) . . ? C9 C8 C1 120.0(2) . . ? C13 C8 C1 120.3(2) . . ? C10 C9 C8 119.9(2) . . ? C10 C9 N2 119.7(2) . . ? C8 C9 N2 120.4(2) . . ? C11 C10 C9 120.6(2) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C12 C11 C10 119.7(2) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 121.2(2) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C12 C13 C8 119.0(2) . . ? C12 C13 C14 119.7(2) . . ? C8 C13 C14 121.2(2) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C16 C15 C20 120.9(3) . . ? C16 C15 S1 118.4(2) . . ? C20 C15 S1 120.7(2) . . ? C17 C16 C15 118.8(3) . . ? C17 C16 C21 116.9(3) . . ? C15 C16 C21 124.3(3) . . ? C18 C17 C16 121.8(3) . . ? C18 C17 H17 119.1 . . ? C16 C17 H17 119.1 . . ? C17 C18 C19 118.4(3) . . ? C17 C18 C22 120.7(3) . . ? C19 C18 C22 120.9(3) . . ? C18 C19 C20 123.3(3) . . ? C18 C19 H19 118.4 . . ? C20 C19 H19 118.4 . . ? C19 C20 C15 116.8(3) . . ? C19 C20 C23 116.7(3) . . ? C15 C20 C23 126.5(3) . . ? C16 C21 H21A 109.5 . . ? C16 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C16 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C18 C22 H22A 109.5 . . ? C18 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C18 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C20 C23 H23A 109.5 . . ? C20 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C20 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C29 C24 C25 120.5(3) . . ? C29 C24 S2 118.0(2) . . ? C25 C24 S2 121.4(2) . . ? C26 C25 C24 117.7(3) . . ? C26 C25 C30 116.7(3) . . ? C24 C25 C30 125.6(3) . . ? C27 C26 C25 123.2(3) . . ? C27 C26 H26 118.4 . . ? C25 C26 H26 118.4 . . ? C26 C27 C28 118.0(3) . . ? C26 C27 C31 120.8(4) . . ? C28 C27 C31 121.3(4) . . ? C27 C28 C29 122.0(3) . . ? C27 C28 H28 119.0 . . ? C29 C28 H28 119.0 . . ? C28 C29 C24 118.7(3) . . ? C28 C29 C32 117.0(3) . . ? C24 C29 C32 124.2(3) . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C27 C31 H31A 109.5 . . ? C27 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C27 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N3 C33 H33A 109.5 . . ? N3 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N3 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N3 C34 H34A 109.5 . . ? N3 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N3 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N4 C35 H35A 109.5 . . ? N4 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N4 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N4 C36 H36A 109.5 . . ? N4 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N4 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N5 C37 H37A 109.5 . . ? N5 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N5 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N5 C38 H38A 109.5 . . ? N5 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N5 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O2 S1 N1 C2 -55.0(2) . . . . ? O1 S1 N1 C2 177.64(18) . . . . ? C15 S1 N1 C2 62.1(2) . . . . ? O2 S1 N1 Ta1 82.52(15) . . . . ? O1 S1 N1 Ta1 -44.86(15) . . . . ? C15 S1 N1 Ta1 -160.39(14) . . . . ? N3 Ta1 N1 C2 16.07(19) . . . . ? N4 Ta1 N1 C2 -160.13(15) . . . . ? N5 Ta1 N1 C2 107.72(16) . . . . ? N2 Ta1 N1 C2 -71.45(16) . . . . ? N3 Ta1 N1 S1 -126.02(13) . . . . ? N4 Ta1 N1 S1 57.78(17) . . . . ? N5 Ta1 N1 S1 -34.37(14) . . . . ? N2 Ta1 N1 S1 146.46(14) . . . . ? O4 S2 N2 C9 59.4(2) . . . . ? O3 S2 N2 C9 -172.07(17) . . . . ? C24 S2 N2 C9 -56.9(2) . . . . ? O4 S2 N2 Ta1 -108.38(14) . . . . ? O3 S2 N2 Ta1 20.18(17) . . . . ? C24 S2 N2 Ta1 135.39(14) . . . . ? N3 Ta1 N2 C9 -143.31(19) . . . . ? N4 Ta1 N2 C9 99.18(19) . . . . ? N5 Ta1 N2 C9 -33.1(11) . . . . ? N1 Ta1 N2 C9 -22.66(18) . . . . ? N3 Ta1 N2 S2 23.15(14) . . . . ? N4 Ta1 N2 S2 -94.36(14) . . . . ? N5 Ta1 N2 S2 133.4(10) . . . . ? N1 Ta1 N2 S2 143.80(15) . . . . ? N4 Ta1 N3 C34 147.2(2) . . . . ? N5 Ta1 N3 C34 -123.9(2) . . . . ? N1 Ta1 N3 C34 -29.2(3) . . . . ? N2 Ta1 N3 C34 51.8(2) . . . . ? N4 Ta1 N3 C33 -29.4(3) . . . . ? N5 Ta1 N3 C33 59.5(3) . . . . ? N1 Ta1 N3 C33 154.2(2) . . . . ? N2 Ta1 N3 C33 -124.8(2) . . . . ? N3 Ta1 N4 C36 -148.24(18) . . . . ? N5 Ta1 N4 C36 123.0(2) . . . . ? N1 Ta1 N4 C36 28.1(2) . . . . ? N2 Ta1 N4 C36 -53.59(19) . . . . ? N3 Ta1 N4 C35 38.5(3) . . . . ? N5 Ta1 N4 C35 -50.2(3) . . . . ? N1 Ta1 N4 C35 -145.2(2) . . . . ? N2 Ta1 N4 C35 133.2(2) . . . . ? N3 Ta1 N5 C38 -152.2(2) . . . . ? N4 Ta1 N5 C38 -34.9(2) . . . . ? N1 Ta1 N5 C38 87.1(2) . . . . ? N2 Ta1 N5 C38 97.4(10) . . . . ? N3 Ta1 N5 C37 36.6(2) . . . . ? N4 Ta1 N5 C37 153.8(2) . . . . ? N1 Ta1 N5 C37 -84.1(2) . . . . ? N2 Ta1 N5 C37 -73.8(11) . . . . ? C6 C1 C2 C3 2.3(4) . . . . ? C8 C1 C2 C3 -177.7(2) . . . . ? C6 C1 C2 N1 -172.7(2) . . . . ? C8 C1 C2 N1 7.3(3) . . . . ? S1 N1 C2 C3 61.1(3) . . . . ? Ta1 N1 C2 C3 -81.7(2) . . . . ? S1 N1 C2 C1 -123.9(2) . . . . ? Ta1 N1 C2 C1 93.3(2) . . . . ? C1 C2 C3 C4 0.5(4) . . . . ? N1 C2 C3 C4 175.3(2) . . . . ? C2 C3 C4 C5 -1.7(4) . . . . ? C3 C4 C5 C6 0.2(4) . . . . ? C4 C5 C6 C1 2.6(4) . . . . ? C4 C5 C6 C7 -174.5(3) . . . . ? C2 C1 C6 C5 -3.7(4) . . . . ? C8 C1 C6 C5 176.3(2) . . . . ? C2 C1 C6 C7 173.2(2) . . . . ? C8 C1 C6 C7 -6.8(4) . . . . ? C6 C1 C8 C9 117.2(3) . . . . ? C2 C1 C8 C9 -62.8(3) . . . . ? C6 C1 C8 C13 -68.2(3) . . . . ? C2 C1 C8 C13 111.9(3) . . . . ? C13 C8 C9 C10 -0.7(4) . . . . ? C1 C8 C9 C10 174.0(2) . . . . ? C13 C8 C9 N2 -179.9(2) . . . . ? C1 C8 C9 N2 -5.2(3) . . . . ? S2 N2 C9 C10 83.2(2) . . . . ? Ta1 N2 C9 C10 -108.7(2) . . . . ? S2 N2 C9 C8 -97.6(2) . . . . ? Ta1 N2 C9 C8 70.5(3) . . . . ? C8 C9 C10 C11 2.6(4) . . . . ? N2 C9 C10 C11 -178.2(2) . . . . ? C9 C10 C11 C12 -1.7(4) . . . . ? C10 C11 C12 C13 -1.1(4) . . . . ? C11 C12 C13 C8 3.0(4) . . . . ? C11 C12 C13 C14 -174.9(2) . . . . ? C9 C8 C13 C12 -2.0(4) . . . . ? C1 C8 C13 C12 -176.8(2) . . . . ? C9 C8 C13 C14 175.8(2) . . . . ? C1 C8 C13 C14 1.1(4) . . . . ? O2 S1 C15 C16 -161.9(2) . . . . ? O1 S1 C15 C16 -34.1(2) . . . . ? N1 S1 C15 C16 78.2(2) . . . . ? O2 S1 C15 C20 16.9(2) . . . . ? O1 S1 C15 C20 144.7(2) . . . . ? N1 S1 C15 C20 -103.0(2) . . . . ? C20 C15 C16 C17 0.2(4) . . . . ? S1 C15 C16 C17 179.0(2) . . . . ? C20 C15 C16 C21 -179.5(2) . . . . ? S1 C15 C16 C21 -0.7(4) . . . . ? C15 C16 C17 C18 0.2(4) . . . . ? C21 C16 C17 C18 179.9(2) . . . . ? C16 C17 C18 C19 -0.6(4) . . . . ? C16 C17 C18 C22 177.9(3) . . . . ? C17 C18 C19 C20 0.6(4) . . . . ? C22 C18 C19 C20 -177.9(3) . . . . ? C18 C19 C20 C15 -0.2(4) . . . . ? C18 C19 C20 C23 -179.3(3) . . . . ? C16 C15 C20 C19 -0.2(4) . . . . ? S1 C15 C20 C19 -178.9(2) . . . . ? C16 C15 C20 C23 178.8(3) . . . . ? S1 C15 C20 C23 0.0(4) . . . . ? O4 S2 C24 C29 162.8(2) . . . . ? O3 S2 C24 C29 37.4(2) . . . . ? N2 S2 C24 C29 -78.8(2) . . . . ? O4 S2 C24 C25 -19.9(2) . . . . ? O3 S2 C24 C25 -145.3(2) . . . . ? N2 S2 C24 C25 98.5(2) . . . . ? C29 C24 C25 C26 -1.6(4) . . . . ? S2 C24 C25 C26 -178.8(2) . . . . ? C29 C24 C25 C30 176.7(3) . . . . ? S2 C24 C25 C30 -0.5(4) . . . . ? C24 C25 C26 C27 0.3(4) . . . . ? C30 C25 C26 C27 -178.1(3) . . . . ? C25 C26 C27 C28 0.7(5) . . . . ? C25 C26 C27 C31 -178.5(3) . . . . ? C26 C27 C28 C29 -0.4(5) . . . . ? C31 C27 C28 C29 178.7(3) . . . . ? C27 C28 C29 C24 -0.8(4) . . . . ? C27 C28 C29 C32 178.6(3) . . . . ? C25 C24 C29 C28 1.8(4) . . . . ? S2 C24 C29 C28 179.1(2) . . . . ? C25 C24 C29 C32 -177.5(3) . . . . ? S2 C24 C29 C32 -0.2(4) . . . . ? _diffrn_measured_fraction_theta_max 0.980 _diffrn_reflns_theta_full 72.26 _diffrn_measured_fraction_theta_full 0.980 _refine_diff_density_max 0.986 _refine_diff_density_min -1.452 _refine_diff_density_rms 0.107 # Attachment '- compound 22.cif' data_compound22 _database_code_depnum_ccdc_archive 'CCDC 791867' #TrackingRef '- compound 22.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H44 N4 P2 S2 V' _chemical_formula_sum 'C48 H44 N4 P2 S2 V' _chemical_formula_weight 853.87 _chemical_absolute_configuration rmad 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 9.7371(7) _cell_length_b 19.029(2) _cell_length_c 22.878(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4239.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 11935 _cell_measurement_theta_min 1.4 _cell_measurement_theta_max 27.9 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.338 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1780 _exptl_absorpt_coefficient_mu 0.447 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9002 _exptl_absorpt_correction_T_max 0.9158 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 34533 _diffrn_reflns_av_R_equivalents 0.0438 _diffrn_reflns_av_sigmaI/netI 0.0458 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8312 _reflns_number_gt 7694 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.8' _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. N3, N4, C28' and C48 were isotropic restrained. The phenyl groups, dimethyamino groups and S2 and P2 atoms are disordered in two positions. The phenyl ring were constrained as a hexgon, the P-C distances and N-C distances of disordered atoms were restrained. ; _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^)+(0.0372P)^2^+10.4411P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0147(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.03(4) _refine_ls_number_reflns 8312 _refine_ls_number_parameters 687 _refine_ls_number_restraints 934 _refine_ls_R_factor_all 0.0792 _refine_ls_R_factor_gt 0.0734 _refine_ls_wR_factor_ref 0.1618 _refine_ls_wR_factor_gt 0.1576 _refine_ls_goodness_of_fit_ref 1.110 _refine_ls_restrained_S_all 1.101 _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 0.29679(11) 0.07995(5) 0.91401(5) 0.0491(3) Uani 1 1 d D . . S1 S -0.08914(16) 0.12348(8) 0.98042(9) 0.0610(5) Uani 1 1 d . A . P1 P 0.05232(13) 0.05838(6) 1.00775(6) 0.0315(3) Uani 1 1 d D . . N1 N 0.1599(4) 0.02456(19) 0.95838(15) 0.0273(8) Uani 1 1 d . A . N2 N 0.4060(4) 0.02733(19) 0.85610(17) 0.0316(9) Uani 1 1 d . A . C1 C 0.2173(4) -0.0752(2) 0.89730(17) 0.0227(9) Uani 1 1 d . A . C2 C 0.1200(4) -0.0296(2) 0.91913(18) 0.0234(9) Uani 1 1 d . . . C3 C -0.0198(5) -0.0377(3) 0.9001(2) 0.0385(12) Uani 1 1 d . A . H3A H -0.0875 -0.0061 0.9145 0.046 Uiso 1 1 calc R . . C4 C -0.0580(5) -0.0887(3) 0.8625(2) 0.0431(13) Uani 1 1 d . . . H4A H -0.1516 -0.0925 0.8513 0.052 Uiso 1 1 calc R A . C5 C 0.0401(5) -0.1369(3) 0.8394(2) 0.0332(11) Uani 1 1 d . A . C6 C 0.1798(5) -0.1292(2) 0.85644(18) 0.0250(9) Uani 1 1 d . . . C7 C 0.2761(6) -0.1771(2) 0.8328(2) 0.0338(11) Uani 1 1 d . A . H7A H 0.3704 -0.1728 0.8428 0.041 Uiso 1 1 calc R . . C8 C 0.2353(6) -0.2298(3) 0.7956(2) 0.0387(12) Uani 1 1 d . . . H8A H 0.3019 -0.2612 0.7800 0.046 Uiso 1 1 calc R A . C9 C 0.0969(6) -0.2380(3) 0.7802(2) 0.0446(14) Uani 1 1 d . A . H9A H 0.0697 -0.2753 0.7551 0.053 Uiso 1 1 calc R . . C10 C 0.0006(6) -0.1918(3) 0.8016(2) 0.0447(13) Uani 1 1 d . . . H10A H -0.0931 -0.1970 0.7908 0.054 Uiso 1 1 calc R A . C11 C 0.3630(4) -0.0734(2) 0.91740(19) 0.0239(9) Uani 1 1 d . . . C12 C 0.4552(5) -0.0258(2) 0.89431(18) 0.0273(9) Uani 1 1 d . A . C13 C 0.5978(5) -0.0287(3) 0.9125(2) 0.0323(10) Uani 1 1 d . . . H13A H 0.6623 0.0034 0.8966 0.039 Uiso 1 1 calc R A . C14 C 0.6392(5) -0.0773(3) 0.9523(2) 0.0376(11) Uani 1 1 d . A . H14A H 0.7332 -0.0787 0.9633 0.045 Uiso 1 1 calc R . . C15 C 0.5474(5) -0.1255(2) 0.9777(2) 0.0319(10) Uani 1 1 d . . . C16 C 0.4081(5) -0.1240(2) 0.95995(18) 0.0247(9) Uani 1 1 d . A . C17 C 0.3183(5) -0.1750(2) 0.98451(19) 0.0305(10) Uani 1 1 d . . . H17A H 0.2254 -0.1766 0.9719 0.037 Uiso 1 1 calc R A . C18 C 0.3621(6) -0.2219(2) 1.0259(2) 0.0337(11) Uani 1 1 d . A . H18A H 0.3000 -0.2555 1.0416 0.040 Uiso 1 1 calc R . . C19 C 0.5003(6) -0.2203(3) 1.0452(2) 0.0419(13) Uani 1 1 d . . . H19A H 0.5303 -0.2514 1.0751 0.050 Uiso 1 1 calc R A . C20 C 0.5891(6) -0.1744(3) 1.0209(2) 0.0406(12) Uani 1 1 d . A . H20A H 0.6824 -0.1748 1.0330 0.049 Uiso 1 1 calc R . . C21 C -0.0212(5) -0.0161(2) 1.04643(19) 0.0330(11) Uani 1 1 d . A . C22 C 0.0460(6) -0.0797(3) 1.0497(2) 0.0389(11) Uani 1 1 d . . . H22A H 0.1317 -0.0852 1.0304 0.047 Uiso 1 1 calc R A . C23 C -0.0087(8) -0.1357(3) 1.0805(3) 0.0597(18) Uani 1 1 d . A . H23A H 0.0362 -0.1800 1.0806 0.072 Uiso 1 1 calc R . . C24 C -0.1301(8) -0.1260(4) 1.1110(2) 0.062(2) Uani 1 1 d . . . H24A H -0.1668 -0.1632 1.1339 0.075 Uiso 1 1 calc R A . C25 C -0.1974(7) -0.0628(4) 1.1084(3) 0.066(2) Uani 1 1 d . A . H25A H -0.2814 -0.0569 1.1289 0.079 Uiso 1 1 calc R . . C26 C -0.1445(6) -0.0073(3) 1.0762(2) 0.0474(14) Uani 1 1 d . . . H26A H -0.1919 0.0363 1.0745 0.057 Uiso 1 1 calc R A . C27 C 0.1559(5) 0.1051(2) 1.0594(2) 0.0362(18) Uani 0.727(5) 1 d PGDU A 1 C28 C 0.2038(6) 0.0725(2) 1.1098(2) 0.054(2) Uani 0.727(5) 1 d PGU A 1 H28A H 0.1831 0.0245 1.1169 0.065 Uiso 0.727(5) 1 calc PR A 1 C29 C 0.2818(6) 0.1102(3) 1.14985(19) 0.069(3) Uani 0.727(5) 1 d PGU A 1 H29A H 0.3146 0.0880 1.1843 0.083 Uiso 0.727(5) 1 calc PR A 1 C30 C 0.3121(6) 0.1805(3) 1.1395(2) 0.056(2) Uani 0.727(5) 1 d PGU A 1 H30A H 0.3654 0.2063 1.1668 0.067 Uiso 0.727(5) 1 calc PR A 1 C31 C 0.2642(6) 0.21311(18) 1.0891(2) 0.051(2) Uani 0.727(5) 1 d PGU A 1 H31A H 0.2849 0.2612 1.0820 0.061 Uiso 0.727(5) 1 calc PR A 1 C32 C 0.1861(5) 0.1754(2) 1.04903(18) 0.0401(17) Uani 0.727(5) 1 d PGU A 1 H32A H 0.1534 0.1977 1.0146 0.048 Uiso 0.727(5) 1 calc PR A 1 P2 P 0.4790(5) 0.0663(3) 0.8029(3) 0.0322(11) Uani 0.540(6) 1 d PDU A 1 C33 C 0.5862(9) -0.0032(5) 0.7698(5) 0.038(2) Uani 0.540(6) 1 d PGDU A 1 C34 C 0.5197(7) -0.0637(6) 0.7508(6) 0.051(3) Uani 0.540(6) 1 d PGU A 1 H34A H 0.4240 -0.0693 0.7575 0.062 Uiso 0.540(6) 1 calc PR A 1 C35 C 0.5930(9) -0.1159(5) 0.7220(5) 0.069(4) Uani 0.540(6) 1 d PGU A 1 H35A H 0.5475 -0.1572 0.7090 0.083 Uiso 0.540(6) 1 calc PR A 1 C36 C 0.7330(9) -0.1077(5) 0.7122(4) 0.066(4) Uani 0.540(6) 1 d PGU A 1 H36A H 0.7832 -0.1434 0.6925 0.080 Uiso 0.540(6) 1 calc PR A 1 C37 C 0.7996(7) -0.0472(5) 0.7312(4) 0.066(3) Uani 0.540(6) 1 d PGU A 1 H37A H 0.8953 -0.0416 0.7245 0.080 Uiso 0.540(6) 1 calc PR A 1 C38 C 0.7262(9) 0.0050(4) 0.7600(4) 0.052(3) Uani 0.540(6) 1 d PGU A 1 H38A H 0.7717 0.0463 0.7730 0.062 Uiso 0.540(6) 1 calc PR A 1 S2 S 0.5931(5) 0.15004(19) 0.81835(14) 0.0572(12) Uani 0.540(6) 1 d PDU A 1 C39 C 0.3412(6) 0.0859(4) 0.7526(3) 0.036(2) Uani 0.540(6) 1 d PGDU A 1 C40 C 0.3504(7) 0.1443(4) 0.7163(3) 0.057(3) Uani 0.540(6) 1 d PGU A 1 H40A H 0.4275 0.1747 0.7189 0.068 Uiso 0.540(6) 1 calc PR A 1 C41 C 0.2468(9) 0.1582(4) 0.6761(3) 0.077(4) Uani 0.540(6) 1 d PGU A 1 H41A H 0.2531 0.1981 0.6513 0.092 Uiso 0.540(6) 1 calc PR A 1 C42 C 0.1340(8) 0.1136(5) 0.6723(3) 0.077(4) Uani 0.540(6) 1 d PGU A 1 H42A H 0.0631 0.1231 0.6448 0.092 Uiso 0.540(6) 1 calc PR A 1 C43 C 0.1248(7) 0.0553(4) 0.7086(4) 0.069(3) Uani 0.540(6) 1 d PGU A 1 H43A H 0.0477 0.0248 0.7059 0.083 Uiso 0.540(6) 1 calc PR A 1 C44 C 0.2284(7) 0.0414(3) 0.7487(3) 0.049(3) Uani 0.540(6) 1 d PGU A 1 H44A H 0.2221 0.0015 0.7735 0.059 Uiso 0.540(6) 1 calc PR A 1 C45 C 0.5083(11) 0.1778(4) 0.9636(5) 0.102(4) Uani 0.727(5) 1 d PDU A 1 H45A H 0.4973 0.2055 0.9994 0.154 Uiso 0.727(5) 1 calc PR A 1 H45B H 0.4753 0.2051 0.9301 0.154 Uiso 0.727(5) 1 calc PR A 1 H45C H 0.6056 0.1664 0.9580 0.154 Uiso 0.727(5) 1 calc PR A 1 C46 C 0.4786(8) 0.0673(4) 1.0174(4) 0.064(2) Uani 0.727(5) 1 d PDU A 1 H46A H 0.4760 0.0944 1.0539 0.097 Uiso 0.727(5) 1 calc PR A 1 H46B H 0.5732 0.0527 1.0093 0.097 Uiso 0.727(5) 1 calc PR A 1 H46C H 0.4202 0.0256 1.0213 0.097 Uiso 0.727(5) 1 calc PR A 1 C47 C 0.1142(11) 0.1399(6) 0.8472(4) 0.084(4) Uani 0.727(5) 1 d PDU A 1 H47A H 0.1271 0.1655 0.8104 0.126 Uiso 0.727(5) 1 calc PR A 1 H47B H 0.0241 0.1514 0.8637 0.126 Uiso 0.727(5) 1 calc PR A 1 H47C H 0.1193 0.0892 0.8396 0.126 Uiso 0.727(5) 1 calc PR A 1 C48 C 0.2395(15) 0.2334(5) 0.9010(6) 0.105(4) Uani 0.727(5) 1 d PDU A 1 H48A H 0.2049 0.2620 0.8686 0.158 Uiso 0.727(5) 1 calc PR A 1 H48B H 0.3376 0.2428 0.9067 0.158 Uiso 0.727(5) 1 calc PR A 1 H48C H 0.1894 0.2453 0.9368 0.158 Uiso 0.727(5) 1 calc PR A 1 N3 N 0.4274(6) 0.1117(3) 0.9685(3) 0.050(2) Uani 0.727(5) 1 d PDU A 1 N4 N 0.2197(9) 0.1595(4) 0.8878(4) 0.071(2) Uani 0.727(5) 1 d PDU A 1 C27' C 0.1798(13) 0.0844(8) 1.0643(6) 0.039(4) Uani 0.273(5) 1 d PGDU A 2 C28' C 0.2969(14) 0.0455(6) 1.0769(6) 0.044(4) Uani 0.273(5) 1 d PGU A 2 H28B H 0.3141 0.0027 1.0567 0.053 Uiso 0.273(5) 1 calc PR A 2 C29' C 0.3890(12) 0.0692(7) 1.1189(6) 0.047(4) Uani 0.273(5) 1 d PGU A 2 H29B H 0.4691 0.0426 1.1275 0.057 Uiso 0.273(5) 1 calc PR A 2 C30' C 0.3639(14) 0.1317(8) 1.1484(6) 0.066(5) Uani 0.273(5) 1 d PGU A 2 H30B H 0.4269 0.1479 1.1772 0.079 Uiso 0.273(5) 1 calc PR A 2 C31' C 0.2468(17) 0.1706(7) 1.1359(8) 0.073(6) Uani 0.273(5) 1 d PGU A 2 H31B H 0.2296 0.2134 1.1560 0.087 Uiso 0.273(5) 1 calc PR A 2 C32' C 0.1547(14) 0.1470(8) 1.0938(8) 0.073(5) Uani 0.273(5) 1 d PGU A 2 H32B H 0.0746 0.1736 1.0852 0.087 Uiso 0.273(5) 1 calc PR A 2 C45' C 0.295(3) 0.2201(10) 0.9743(11) 0.074(7) Uani 0.273(5) 1 d PDU A 2 H45D H 0.3370 0.2599 0.9539 0.111 Uiso 0.273(5) 1 calc PR A 2 H45E H 0.3099 0.2249 1.0165 0.111 Uiso 0.273(5) 1 calc PR A 2 H45F H 0.1958 0.2195 0.9663 0.111 Uiso 0.273(5) 1 calc PR A 2 C46' C 0.481(2) 0.1304(13) 0.9791(10) 0.049(5) Uani 0.273(5) 1 d PDU A 2 H46D H 0.4777 0.1352 1.0217 0.074 Uiso 0.273(5) 1 calc PR A 2 H46E H 0.5586 0.1579 0.9638 0.074 Uiso 0.273(5) 1 calc PR A 2 H46F H 0.4940 0.0808 0.9688 0.074 Uiso 0.273(5) 1 calc PR A 2 C47' C 0.081(3) 0.1008(11) 0.8244(11) 0.072(7) Uani 0.273(5) 1 d PDU A 2 H47D H 0.0744 0.1312 0.7900 0.107 Uiso 0.273(5) 1 calc PR A 2 H47E H -0.0096 0.0965 0.8427 0.107 Uiso 0.273(5) 1 calc PR A 2 H47F H 0.1136 0.0542 0.8127 0.107 Uiso 0.273(5) 1 calc PR A 2 C48' C 0.167(3) 0.2100(7) 0.8697(12) 0.063(6) Uani 0.273(5) 1 d PDU A 2 H48D H 0.1020 0.2262 0.8399 0.095 Uiso 0.273(5) 1 calc PR A 2 H48E H 0.2572 0.2311 0.8626 0.095 Uiso 0.273(5) 1 calc PR A 2 H48F H 0.1340 0.2238 0.9085 0.095 Uiso 0.273(5) 1 calc PR A 2 N3' N 0.3554(17) 0.1556(7) 0.9540(8) 0.061(5) Uani 0.273(5) 1 d PDU A 2 N4' N 0.1788(17) 0.1319(7) 0.8668(7) 0.036(4) Uani 0.273(5) 1 d PDU A 2 S2' S 0.6705(4) 0.1209(3) 0.82954(16) 0.0579(12) Uani 0.460(6) 1 d PDU A 2 C33' C 0.5754(16) -0.0172(8) 0.7624(8) 0.052(4) Uani 0.460(6) 1 d PGDU A 2 C34' C 0.4901(13) -0.0740(9) 0.7502(10) 0.072(5) Uani 0.460(6) 1 d PGU A 2 H34B H 0.3983 -0.0743 0.7642 0.086 Uiso 0.460(6) 1 calc PR A 2 C35' C 0.5393(16) -0.1302(7) 0.7176(9) 0.092(5) Uani 0.460(6) 1 d PGU A 2 H35B H 0.4810 -0.1690 0.7093 0.110 Uiso 0.460(6) 1 calc PR A 2 C36' C 0.6737(18) -0.1297(7) 0.6971(7) 0.107(5) Uani 0.460(6) 1 d PGU A 2 H36B H 0.7073 -0.1681 0.6748 0.128 Uiso 0.460(6) 1 calc PR A 2 C37' C 0.7589(14) -0.0730(8) 0.7092(7) 0.091(5) Uani 0.460(6) 1 d PGU A 2 H37B H 0.8507 -0.0726 0.6952 0.109 Uiso 0.460(6) 1 calc PR A 2 C38' C 0.7098(15) -0.0167(6) 0.7419(7) 0.072(4) Uani 0.460(6) 1 d PGU A 2 H38B H 0.7680 0.0221 0.7502 0.087 Uiso 0.460(6) 1 calc PR A 2 P2' P 0.5238(5) 0.0595(4) 0.8040(3) 0.0326(13) Uani 0.460(6) 1 d PDU A 2 C39' C 0.4096(8) 0.1032(3) 0.7536(3) 0.030(2) Uani 0.460(6) 1 d PGDU A 2 C40' C 0.4129(7) 0.1762(3) 0.7512(3) 0.034(2) Uani 0.460(6) 1 d PGU A 2 H40B H 0.4741 0.2016 0.7757 0.041 Uiso 0.460(6) 1 calc PR A 2 C41' C 0.3266(9) 0.2119(3) 0.7131(4) 0.049(3) Uani 0.460(6) 1 d PGU A 2 H41B H 0.3288 0.2618 0.7115 0.059 Uiso 0.460(6) 1 calc PR A 2 C42' C 0.2370(9) 0.1747(5) 0.6773(4) 0.055(3) Uani 0.460(6) 1 d PGU A 2 H42B H 0.1780 0.1992 0.6512 0.066 Uiso 0.460(6) 1 calc PR A 2 C43' C 0.2338(9) 0.1018(5) 0.6797(4) 0.060(3) Uani 0.460(6) 1 d PGU A 2 H43B H 0.1726 0.0763 0.6552 0.072 Uiso 0.460(6) 1 calc PR A 2 C44' C 0.3201(10) 0.0660(3) 0.7178(4) 0.049(3) Uani 0.460(6) 1 d PGU A 2 H44B H 0.3179 0.0161 0.7194 0.059 Uiso 0.460(6) 1 calc PRU 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 0.0519(6) 0.0282(4) 0.0672(7) 0.0126(4) 0.0280(5) -0.0013(4) S1 0.0444(8) 0.0453(8) 0.0934(13) 0.0124(8) 0.0176(9) 0.0193(7) P1 0.0301(6) 0.0273(6) 0.0371(7) -0.0030(5) 0.0053(5) -0.0003(5) N1 0.031(2) 0.0273(19) 0.0237(19) 0.0021(15) -0.0003(16) -0.0012(16) N2 0.031(2) 0.0261(19) 0.037(2) 0.0097(16) -0.0026(18) -0.0082(17) C1 0.026(2) 0.0196(19) 0.023(2) 0.0081(16) -0.0024(17) -0.0030(18) C2 0.022(2) 0.028(2) 0.020(2) 0.0042(17) -0.0017(17) -0.0029(17) C3 0.023(2) 0.056(3) 0.037(3) -0.011(2) -0.003(2) -0.002(2) C4 0.027(3) 0.070(4) 0.032(3) -0.008(2) -0.006(2) -0.014(3) C5 0.033(3) 0.040(3) 0.026(2) 0.0035(19) 0.000(2) -0.006(2) C6 0.032(2) 0.025(2) 0.018(2) 0.0056(16) -0.0039(18) -0.0067(19) C7 0.047(3) 0.025(2) 0.029(3) 0.0029(18) -0.001(2) 0.003(2) C8 0.055(3) 0.030(2) 0.031(3) -0.001(2) 0.001(2) 0.003(2) C9 0.060(4) 0.042(3) 0.032(3) -0.004(2) -0.005(3) -0.013(3) C10 0.041(3) 0.057(3) 0.035(3) -0.004(2) 0.001(2) -0.014(3) C11 0.022(2) 0.025(2) 0.025(2) 0.0019(18) -0.0041(17) -0.0001(17) C12 0.030(2) 0.033(2) 0.019(2) 0.0018(17) -0.0010(18) 0.000(2) C13 0.027(2) 0.047(3) 0.023(2) 0.002(2) 0.0006(19) -0.003(2) C14 0.024(2) 0.061(3) 0.028(2) 0.003(2) -0.0014(19) 0.005(2) C15 0.033(2) 0.036(2) 0.027(2) -0.0020(19) -0.002(2) 0.011(2) C16 0.029(2) 0.022(2) 0.024(2) 0.0015(16) -0.0013(18) 0.0037(18) C17 0.041(3) 0.025(2) 0.026(2) 0.0037(17) 0.000(2) 0.003(2) C18 0.045(3) 0.025(2) 0.031(2) 0.0005(18) 0.002(2) 0.002(2) C19 0.056(3) 0.042(3) 0.028(2) 0.003(2) -0.006(2) 0.023(3) C20 0.043(3) 0.051(3) 0.029(3) 0.002(2) -0.005(2) 0.024(2) C21 0.038(3) 0.038(3) 0.023(2) -0.0022(18) 0.004(2) -0.010(2) C22 0.049(3) 0.036(3) 0.032(2) 0.004(2) 0.003(2) -0.003(2) C23 0.095(5) 0.046(3) 0.039(3) 0.010(3) -0.015(4) -0.019(3) C24 0.088(5) 0.068(4) 0.030(3) 0.010(3) -0.002(3) -0.043(4) C25 0.060(4) 0.093(5) 0.044(3) -0.011(3) 0.017(3) -0.041(4) C26 0.046(3) 0.052(3) 0.044(3) -0.017(3) 0.019(3) -0.012(3) C27 0.049(5) 0.025(3) 0.035(4) -0.006(3) 0.010(3) -0.012(3) C28 0.065(5) 0.046(4) 0.051(4) 0.010(3) -0.010(4) -0.033(4) C29 0.100(7) 0.071(5) 0.036(4) 0.005(4) -0.011(5) -0.046(5) C30 0.057(6) 0.058(5) 0.052(5) -0.022(4) 0.004(4) -0.030(4) C31 0.066(5) 0.032(4) 0.054(4) -0.021(3) 0.021(4) -0.023(3) C32 0.051(4) 0.022(3) 0.047(4) -0.010(3) 0.016(3) -0.009(3) P2 0.034(3) 0.0385(19) 0.0243(15) 0.0024(13) 0.0051(19) -0.0083(18) C33 0.046(5) 0.055(6) 0.013(5) 0.009(4) 0.005(4) 0.000(4) C34 0.051(6) 0.063(7) 0.040(6) -0.020(6) 0.000(5) 0.014(5) C35 0.063(7) 0.079(8) 0.065(7) -0.041(7) 0.003(7) 0.016(6) C36 0.056(6) 0.096(9) 0.047(7) -0.018(7) -0.002(6) 0.026(7) C37 0.040(6) 0.113(9) 0.046(7) -0.005(6) -0.014(5) 0.024(5) C38 0.039(5) 0.084(8) 0.032(6) 0.008(5) -0.014(5) 0.013(5) S2 0.071(3) 0.0553(19) 0.0454(17) 0.0106(14) 0.0070(17) -0.0387(19) C39 0.038(5) 0.041(5) 0.029(5) 0.002(4) 0.011(4) 0.018(4) C40 0.050(5) 0.068(6) 0.053(6) 0.024(5) 0.022(4) 0.019(5) C41 0.080(8) 0.104(10) 0.047(8) 0.029(7) 0.012(6) 0.046(6) C42 0.066(7) 0.110(9) 0.054(7) 0.008(6) -0.007(6) 0.056(6) C43 0.055(7) 0.082(8) 0.070(8) -0.011(6) -0.031(6) 0.033(6) C44 0.047(6) 0.052(6) 0.049(6) -0.001(4) -0.016(5) 0.011(4) C45 0.073(7) 0.062(6) 0.172(12) -0.063(6) 0.052(8) -0.038(6) C46 0.037(4) 0.078(6) 0.079(6) -0.045(4) -0.017(4) 0.011(4) C47 0.070(7) 0.134(10) 0.048(6) 0.038(6) 0.015(5) -0.014(7) C48 0.121(6) 0.089(5) 0.106(6) 0.006(4) 0.005(4) 0.011(4) N3 0.032(3) 0.039(3) 0.081(5) -0.030(3) 0.022(3) -0.017(3) N4 0.065(5) 0.061(4) 0.088(6) 0.026(4) 0.015(4) 0.019(4) C27' 0.039(7) 0.040(7) 0.039(8) 0.000(6) 0.012(6) -0.009(6) C28' 0.044(5) 0.046(5) 0.043(5) -0.001(4) -0.005(4) -0.005(4) C29' 0.048(7) 0.050(7) 0.045(7) -0.002(6) -0.007(6) -0.013(6) C30' 0.068(8) 0.069(8) 0.060(8) -0.019(7) -0.004(7) -0.003(7) C31' 0.077(9) 0.069(8) 0.071(9) -0.020(7) -0.013(7) 0.001(7) C32' 0.070(8) 0.065(8) 0.083(9) -0.018(7) -0.009(7) 0.006(7) C45' 0.085(10) 0.065(9) 0.073(11) -0.008(8) 0.002(9) 0.013(8) C46' 0.051(9) 0.058(9) 0.039(8) -0.012(8) -0.005(7) 0.006(7) C47' 0.083(10) 0.064(9) 0.068(10) 0.019(7) -0.027(8) -0.010(8) C48' 0.061(9) 0.029(6) 0.101(10) 0.017(7) -0.008(8) 0.016(7) N3' 0.056(8) 0.051(7) 0.077(9) 0.003(7) -0.008(7) 0.000(7) N4' 0.052(8) 0.022(6) 0.033(7) -0.005(6) 0.006(6) 0.005(6) S2' 0.037(2) 0.085(3) 0.052(2) 0.0313(19) -0.0097(16) -0.026(2) C33' 0.054(6) 0.060(6) 0.042(7) 0.006(5) 0.007(6) 0.013(5) C34' 0.089(8) 0.053(6) 0.073(8) -0.006(6) -0.003(7) 0.004(6) C35' 0.100(8) 0.075(7) 0.100(9) -0.014(6) 0.010(7) 0.013(7) C36' 0.115(8) 0.099(8) 0.107(9) -0.006(7) 0.021(7) 0.014(7) C37' 0.089(8) 0.093(8) 0.092(9) 0.001(7) 0.024(7) 0.021(6) C38' 0.068(7) 0.079(7) 0.069(8) 0.012(6) 0.015(6) 0.021(6) P2' 0.032(3) 0.041(2) 0.0247(17) 0.0117(14) 0.007(2) -0.001(2) C39' 0.037(5) 0.031(4) 0.022(4) 0.005(3) 0.000(4) 0.003(4) C40' 0.040(5) 0.030(4) 0.032(5) 0.001(4) 0.005(4) 0.001(4) C41' 0.055(6) 0.041(5) 0.052(6) 0.017(4) 0.009(5) 0.017(4) C42' 0.059(7) 0.063(5) 0.043(7) 0.006(5) 0.004(5) 0.027(5) C43' 0.064(7) 0.065(5) 0.051(6) -0.007(5) -0.023(5) 0.005(5) C44' 0.062(6) 0.043(5) 0.042(5) -0.005(4) -0.007(5) -0.001(5) _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 N4 1.794(6) . ? V1 N3' 1.799(8) . ? V1 N4' 1.862(8) . ? V1 N3 1.881(6) . ? V1 N2 1.972(4) . ? V1 N1 1.979(4) . ? V1 C12 2.576(5) . ? S1 P1 1.955(2) . ? P1 N1 1.670(4) . ? P1 C27 1.790(3) . ? P1 C21 1.818(5) . ? P1 C27' 1.860(7) . ? N1 C2 1.421(5) . ? N2 C12 1.420(6) . ? N2 P2 1.593(7) . ? N2 P2' 1.764(8) . ? C1 C2 1.379(6) . ? C1 C6 1.435(6) . ? C1 C11 1.492(6) . ? C2 C3 1.437(6) . ? C3 C4 1.350(7) . ? C3 H3A 0.9500 . ? C4 C5 1.427(7) . ? C4 H4A 0.9500 . ? C5 C10 1.410(7) . ? C5 C6 1.423(6) . ? C6 C7 1.416(7) . ? C7 C8 1.374(7) . ? C7 H7A 0.9500 . ? C8 C9 1.402(8) . ? C8 H8A 0.9500 . ? C9 C10 1.374(8) . ? C9 H9A 0.9500 . ? C10 H10A 0.9500 . ? C11 C12 1.380(6) . ? C11 C16 1.438(6) . ? C12 C13 1.450(6) . ? C13 C14 1.357(7) . ? C13 H13A 0.9500 . ? C14 C15 1.407(7) . ? C14 H14A 0.9500 . ? C15 C20 1.416(6) . ? C15 C16 1.416(6) . ? C16 C17 1.423(6) . ? C17 C18 1.369(6) . ? C17 H17A 0.9500 . ? C18 C19 1.416(8) . ? C18 H18A 0.9500 . ? C19 C20 1.351(8) . ? C19 H19A 0.9500 . ? C20 H20A 0.9500 . ? C21 C22 1.377(7) . ? C21 C26 1.391(7) . ? C22 C23 1.384(7) . ? C22 H22A 0.9500 . ? C23 C24 1.386(10) . ? C23 H23A 0.9500 . ? C24 C25 1.371(10) . ? C24 H24A 0.9500 . ? C25 C26 1.387(8) . ? C25 H25A 0.9500 . ? C26 H26A 0.9500 . ? C27 C28 1.3900 . ? C27 C32 1.3900 . ? C28 C29 1.3900 . ? C28 H28A 0.9500 . ? C29 C30 1.3900 . ? C29 H29A 0.9500 . ? C30 C31 1.3900 . ? C30 H30A 0.9500 . ? C31 C32 1.3900 . ? C31 H31A 0.9500 . ? C32 H32A 0.9500 . ? P2 C39 1.806(6) . ? P2 C33 1.848(6) . ? P2 S2 1.975(5) . ? C33 C34 1.3900 . ? C33 C38 1.3900 . ? C34 C35 1.3900 . ? C34 H34A 0.9500 . ? C35 C36 1.3900 . ? C35 H35A 0.9500 . ? C36 C37 1.3900 . ? C36 H36A 0.9500 . ? C37 C38 1.3900 . ? C37 H37A 0.9500 . ? C38 H38A 0.9500 . ? C39 C40 1.3900 . ? C39 C44 1.3900 . ? C40 C41 1.3900 . ? C40 H40A 0.9500 . ? C41 C42 1.3900 . ? C41 H41A 0.9500 . ? C42 C43 1.3900 . ? C42 H42A 0.9500 . ? C43 C44 1.3900 . ? C43 H43A 0.9500 . ? C44 H44A 0.9500 . ? C45 N3 1.488(7) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 N3 1.488(8) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 N4 1.435(8) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 N4 1.451(8) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C27' C28' 1.3900 . ? C27' C32' 1.3900 . ? C28' C29' 1.3900 . ? C28' H28B 0.9500 . ? C29' C30' 1.3900 . ? C29' H29B 0.9500 . ? C30' C31' 1.3900 . ? C30' H30B 0.9500 . ? C31' C32' 1.3900 . ? C31' H31B 0.9500 . ? C32' H32B 0.9500 . ? C45' N3' 1.439(9) . ? C45' H45D 0.9800 . ? C45' H45E 0.9800 . ? C45' H45F 0.9800 . ? C46' N3' 1.437(9) . ? C46' H46D 0.9800 . ? C46' H46E 0.9800 . ? C46' H46F 0.9800 . ? C47' N4' 1.481(9) . ? C47' H47D 0.9800 . ? C47' H47E 0.9800 . ? C47' H47F 0.9800 . ? C48' N4' 1.491(9) . ? C48' H48D 0.9800 . ? C48' H48E 0.9800 . ? C48' H48F 0.9800 . ? S2' P2' 1.937(6) . ? C33' C34' 1.3900 . ? C33' C38' 1.3900 . ? C33' P2' 1.814(8) . ? C34' C35' 1.3900 . ? C34' H34B 0.9500 . ? C35' C36' 1.3900 . ? C35' H35B 0.9500 . ? C36' C37' 1.3900 . ? C36' H36B 0.9500 . ? C37' C38' 1.3900 . ? C37' H37B 0.9500 . ? C38' H38B 0.9500 . ? P2' C39' 1.804(7) . ? C39' C40' 1.3900 . ? C39' C44' 1.3900 . ? C40' C41' 1.3900 . ? C40' H40B 0.9500 . ? C41' C42' 1.3900 . ? C41' H41B 0.9500 . ? C42' C43' 1.3900 . ? C42' H42B 0.9500 . ? C43' C44' 1.3900 . ? C43' H43B 0.9500 . ? C44' H44B 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 V1 N3' 68.1(6) . . ? N4 V1 N4' 25.7(4) . . ? N3' V1 N4' 93.8(7) . . ? N4 V1 N3 103.5(4) . . ? N3' V1 N3 36.0(6) . . ? N4' V1 N3 129.2(5) . . ? N4 V1 N2 115.4(3) . . ? N3' V1 N2 125.3(6) . . ? N4' V1 N2 102.3(5) . . ? N3 V1 N2 104.1(2) . . ? N4 V1 N1 109.9(3) . . ? N3' V1 N1 112.2(7) . . ? N4' V1 N1 99.5(6) . . ? N3 V1 N1 106.7(2) . . ? N2 V1 N1 115.92(16) . . ? N4 V1 C12 148.4(3) . . ? N3' V1 C12 121.6(5) . . ? N4' V1 C12 133.1(5) . . ? N3 V1 C12 87.8(2) . . ? N2 V1 C12 33.14(14) . . ? N1 V1 C12 94.40(15) . . ? N1 P1 C27 106.5(2) . . ? N1 P1 C21 106.0(2) . . ? C27 P1 C21 106.7(2) . . ? N1 P1 C27' 98.9(5) . . ? C27 P1 C27' 14.7(5) . . ? C21 P1 C27' 97.5(6) . . ? N1 P1 S1 118.04(15) . . ? C27 P1 S1 107.04(19) . . ? C21 P1 S1 111.87(18) . . ? C27' P1 S1 121.6(5) . . ? C2 N1 P1 122.4(3) . . ? C2 N1 V1 104.3(3) . . ? P1 N1 V1 124.3(2) . . ? C12 N2 P2 130.6(4) . . ? C12 N2 P2' 116.3(4) . . ? P2 N2 P2' 14.5(3) . . ? C12 N2 V1 97.5(3) . . ? P2 N2 V1 121.2(3) . . ? P2' N2 V1 128.9(3) . . ? C2 C1 C6 120.8(4) . . ? C2 C1 C11 121.8(4) . . ? C6 C1 C11 117.3(4) . . ? C1 C2 N1 119.8(4) . . ? C1 C2 C3 118.3(4) . . ? N1 C2 C3 121.9(4) . . ? C4 C3 C2 122.1(5) . . ? C4 C3 H3A 119.0 . . ? C2 C3 H3A 119.0 . . ? C3 C4 C5 121.0(5) . . ? C3 C4 H4A 119.5 . . ? C5 C4 H4A 119.5 . . ? C10 C5 C6 120.4(5) . . ? C10 C5 C4 121.4(5) . . ? C6 C5 C4 118.2(4) . . ? C7 C6 C5 117.5(4) . . ? C7 C6 C1 122.8(4) . . ? C5 C6 C1 119.7(4) . . ? C8 C7 C6 121.1(5) . . ? C8 C7 H7A 119.5 . . ? C6 C7 H7A 119.5 . . ? C7 C8 C9 120.9(5) . . ? C7 C8 H8A 119.5 . . ? C9 C8 H8A 119.5 . . ? C10 C9 C8 119.7(5) . . ? C10 C9 H9A 120.1 . . ? C8 C9 H9A 120.1 . . ? C9 C10 C5 120.4(5) . . ? C9 C10 H10A 119.8 . . ? C5 C10 H10A 119.8 . . ? C12 C11 C16 120.0(4) . . ? C12 C11 C1 121.0(4) . . ? C16 C11 C1 118.9(4) . . ? C11 C12 N2 118.9(4) . . ? C11 C12 C13 119.2(4) . . ? N2 C12 C13 121.8(4) . . ? C11 C12 V1 93.2(3) . . ? N2 C12 V1 49.4(2) . . ? C13 C12 V1 123.5(3) . . ? C14 C13 C12 120.2(4) . . ? C14 C13 H13A 119.9 . . ? C12 C13 H13A 119.9 . . ? C13 C14 C15 122.2(4) . . ? C13 C14 H14A 118.9 . . ? C15 C14 H14A 118.9 . . ? C14 C15 C20 122.3(5) . . ? C14 C15 C16 118.4(4) . . ? C20 C15 C16 119.2(5) . . ? C15 C16 C17 117.5(4) . . ? C15 C16 C11 120.0(4) . . ? C17 C16 C11 122.4(4) . . ? C18 C17 C16 121.8(5) . . ? C18 C17 H17A 119.1 . . ? C16 C17 H17A 119.1 . . ? C17 C18 C19 119.9(5) . . ? C17 C18 H18A 120.1 . . ? C19 C18 H18A 120.1 . . ? C20 C19 C18 119.6(5) . . ? C20 C19 H19A 120.2 . . ? C18 C19 H19A 120.2 . . ? C19 C20 C15 121.9(5) . . ? C19 C20 H20A 119.0 . . ? C15 C20 H20A 119.0 . . ? C22 C21 C26 119.3(5) . . ? C22 C21 P1 121.6(4) . . ? C26 C21 P1 118.9(4) . . ? C21 C22 C23 121.4(6) . . ? C21 C22 H22A 119.3 . . ? C23 C22 H22A 119.3 . . ? C22 C23 C24 118.9(6) . . ? C22 C23 H23A 120.6 . . ? C24 C23 H23A 120.6 . . ? C25 C24 C23 120.1(6) . . ? C25 C24 H24A 119.9 . . ? C23 C24 H24A 119.9 . . ? C24 C25 C26 120.9(6) . . ? C24 C25 H25A 119.5 . . ? C26 C25 H25A 119.5 . . ? C25 C26 C21 119.3(6) . . ? C25 C26 H26A 120.4 . . ? C21 C26 H26A 120.4 . . ? C28 C27 C32 120.0 . . ? C28 C27 P1 121.0(3) . . ? C32 C27 P1 119.0(3) . . ? C29 C28 C27 120.0 . . ? C29 C28 H28A 120.0 . . ? C27 C28 H28A 120.0 . . ? C28 C29 C30 120.0 . . ? C28 C29 H29A 120.0 . . ? C30 C29 H29A 120.0 . . ? C31 C30 C29 120.0 . . ? C31 C30 H30A 120.0 . . ? C29 C30 H30A 120.0 . . ? C30 C31 C32 120.0 . . ? C30 C31 H31A 120.0 . . ? C32 C31 H31A 120.0 . . ? C31 C32 C27 120.0 . . ? C31 C32 H32A 120.0 . . ? C27 C32 H32A 120.0 . . ? N2 P2 C39 104.6(4) . . ? N2 P2 C33 103.4(5) . . ? C39 P2 C33 107.8(5) . . ? N2 P2 S2 119.3(4) . . ? C39 P2 S2 111.4(4) . . ? C33 P2 S2 109.4(4) . . ? C34 C33 C38 120.0 . . ? C34 C33 P2 117.2(6) . . ? C38 C33 P2 122.7(6) . . ? C35 C34 C33 120.0 . . ? C35 C34 H34A 120.0 . . ? C33 C34 H34A 120.0 . . ? C34 C35 C36 120.0 . . ? C34 C35 H35A 120.0 . . ? C36 C35 H35A 120.0 . . ? C35 C36 C37 120.0 . . ? C35 C36 H36A 120.0 . . ? C37 C36 H36A 120.0 . . ? C38 C37 C36 120.0 . . ? C38 C37 H37A 120.0 . . ? C36 C37 H37A 120.0 . . ? C37 C38 C33 120.0 . . ? C37 C38 H38A 120.0 . . ? C33 C38 H38A 120.0 . . ? C40 C39 C44 120.0 . . ? C40 C39 P2 119.9(4) . . ? C44 C39 P2 120.1(4) . . ? C41 C40 C39 120.0 . . ? C41 C40 H40A 120.0 . . ? C39 C40 H40A 120.0 . . ? C40 C41 C42 120.0 . . ? C40 C41 H41A 120.0 . . ? C42 C41 H41A 120.0 . . ? C41 C42 C43 120.0 . . ? C41 C42 H42A 120.0 . . ? C43 C42 H42A 120.0 . . ? C44 C43 C42 120.0 . . ? C44 C43 H43A 120.0 . . ? C42 C43 H43A 120.0 . . ? C43 C44 C39 120.0 . . ? C43 C44 H44A 120.0 . . ? C39 C44 H44A 120.0 . . ? C45 N3 C46 111.0(6) . . ? C45 N3 V1 125.4(6) . . ? C46 N3 V1 122.8(4) . . ? C47 N4 C48 118.9(7) . . ? C47 N4 V1 107.2(7) . . ? C48 N4 V1 133.8(8) . . ? C28' C27' C32' 120.0 . . ? C28' C27' P1 123.3(8) . . ? C32' C27' P1 116.7(8) . . ? C29' C28' C27' 120.0 . . ? C29' C28' H28B 120.0 . . ? C27' C28' H28B 120.0 . . ? C28' C29' C30' 120.0 . . ? C28' C29' H29B 120.0 . . ? C30' C29' H29B 120.0 . . ? C31' C30' C29' 120.0 . . ? C31' C30' H30B 120.0 . . ? C29' C30' H30B 120.0 . . ? C32' C31' C30' 120.0 . . ? C32' C31' H31B 120.0 . . ? C30' C31' H31B 120.0 . . ? C31' C32' C27' 120.0 . . ? C31' C32' H32B 120.0 . . ? C27' C32' H32B 120.0 . . ? N3' C45' H45D 109.5 . . ? N3' C45' H45E 109.5 . . ? H45D C45' H45E 109.5 . . ? N3' C45' H45F 109.5 . . ? H45D C45' H45F 109.5 . . ? H45E C45' H45F 109.5 . . ? N3' C46' H46D 109.5 . . ? N3' C46' H46E 109.5 . . ? H46D C46' H46E 109.5 . . ? N3' C46' H46F 109.5 . . ? H46D C46' H46F 109.5 . . ? H46E C46' H46F 109.5 . . ? N4' C47' H47D 109.5 . . ? N4' C47' H47E 109.5 . . ? H47D C47' H47E 109.5 . . ? N4' C47' H47F 109.5 . . ? H47D C47' H47F 109.5 . . ? H47E C47' H47F 109.5 . . ? N4' C48' H48D 109.5 . . ? N4' C48' H48E 109.5 . . ? H48D C48' H48E 109.5 . . ? N4' C48' H48F 109.5 . . ? H48D C48' H48F 109.5 . . ? H48E C48' H48F 109.5 . . ? C46' N3' C45' 120.5(10) . . ? C46' N3' V1 101.9(12) . . ? C45' N3' V1 135.8(14) . . ? C47' N4' C48' 112.2(9) . . ? C47' N4' V1 124.3(11) . . ? C48' N4' V1 123.4(11) . . ? C34' C33' C38' 120.0 . . ? C34' C33' P2' 124.4(9) . . ? C38' C33' P2' 115.6(9) . . ? C35' C34' C33' 120.0 . . ? C35' C34' H34B 120.0 . . ? C33' C34' H34B 120.0 . . ? C34' C35' C36' 120.0 . . ? C34' C35' H35B 120.0 . . ? C36' C35' H35B 120.0 . . ? C37' C36' C35' 120.0 . . ? C37' C36' H36B 120.0 . . ? C35' C36' H36B 120.0 . . ? C38' C37' C36' 120.0 . . ? C38' C37' H37B 120.0 . . ? C36' C37' H37B 120.0 . . ? C37' C38' C33' 120.0 . . ? C37' C38' H38B 120.0 . . ? C33' C38' H38B 120.0 . . ? N2 P2' C39' 101.0(4) . . ? N2 P2' C33' 104.8(7) . . ? C39' P2' C33' 101.9(8) . . ? N2 P2' S2' 119.0(4) . . ? C39' P2' S2' 111.7(4) . . ? C33' P2' S2' 116.1(6) . . ? C40' C39' C44' 120.0 . . ? C40' C39' P2' 118.1(5) . . ? C44' C39' P2' 121.9(5) . . ? C39' C40' C41' 120.0 . . ? C39' C40' H40B 120.0 . . ? C41' C40' H40B 120.0 . . ? C42' C41' C40' 120.0 . . ? C42' C41' H41B 120.0 . . ? C40' C41' H41B 120.0 . . ? C41' C42' C43' 120.0 . . ? C41' C42' H42B 120.0 . . ? C43' C42' H42B 120.0 . . ? C42' C43' C44' 120.0 . . ? C42' C43' H43B 120.0 . . ? C44' C43' H43B 120.0 . . ? C43' C44' C39' 120.0 . . ? C43' C44' H44B 120.0 . . ? C39' C44' H44B 120.0 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C27 P1 N1 C2 164.2(3) . . . . ? C21 P1 N1 C2 50.8(4) . . . . ? C27' P1 N1 C2 151.4(6) . . . . ? S1 P1 N1 C2 -75.5(3) . . . . ? C27 P1 N1 V1 -53.9(3) . . . . ? C21 P1 N1 V1 -167.4(2) . . . . ? C27' P1 N1 V1 -66.8(6) . . . . ? S1 P1 N1 V1 66.4(3) . . . . ? N4 V1 N1 C2 102.8(4) . . . . ? N3' V1 N1 C2 176.6(6) . . . . ? N4' V1 N1 C2 78.5(5) . . . . ? N3 V1 N1 C2 -145.6(3) . . . . ? N2 V1 N1 C2 -30.3(3) . . . . ? C12 V1 N1 C2 -56.6(3) . . . . ? N4 V1 N1 P1 -44.6(4) . . . . ? N3' V1 N1 P1 29.2(6) . . . . ? N4' V1 N1 P1 -69.0(5) . . . . ? N3 V1 N1 P1 67.0(3) . . . . ? N2 V1 N1 P1 -177.7(2) . . . . ? C12 V1 N1 P1 156.0(2) . . . . ? N4 V1 N2 C12 175.6(4) . . . . ? N3' V1 N2 C12 95.3(8) . . . . ? N4' V1 N2 C12 -161.0(6) . . . . ? N3 V1 N2 C12 62.9(3) . . . . ? N1 V1 N2 C12 -54.0(3) . . . . ? N4 V1 N2 P2 27.6(5) . . . . ? N3' V1 N2 P2 -52.6(8) . . . . ? N4' V1 N2 P2 51.1(7) . . . . ? N3 V1 N2 P2 -85.1(4) . . . . ? N1 V1 N2 P2 158.1(3) . . . . ? C12 V1 N2 P2 -147.9(5) . . . . ? N4 V1 N2 P2' 42.6(5) . . . . ? N3' V1 N2 P2' -37.7(8) . . . . ? N4' V1 N2 P2' 66.0(7) . . . . ? N3 V1 N2 P2' -70.1(4) . . . . ? N1 V1 N2 P2' 173.1(3) . . . . ? C12 V1 N2 P2' -133.0(5) . . . . ? C6 C1 C2 N1 -178.4(4) . . . . ? C11 C1 C2 N1 5.1(6) . . . . ? C6 C1 C2 C3 0.3(6) . . . . ? C11 C1 C2 C3 -176.2(4) . . . . ? P1 N1 C2 C1 -153.0(3) . . . . ? V1 N1 C2 C1 58.8(4) . . . . ? P1 N1 C2 C3 28.4(6) . . . . ? V1 N1 C2 C3 -119.8(4) . . . . ? C1 C2 C3 C4 0.9(7) . . . . ? N1 C2 C3 C4 179.5(5) . . . . ? C2 C3 C4 C5 -0.5(8) . . . . ? C3 C4 C5 C10 177.9(5) . . . . ? C3 C4 C5 C6 -0.9(7) . . . . ? C10 C5 C6 C7 1.7(6) . . . . ? C4 C5 C6 C7 -179.6(4) . . . . ? C10 C5 C6 C1 -176.8(4) . . . . ? C4 C5 C6 C1 2.0(6) . . . . ? C2 C1 C6 C7 179.9(4) . . . . ? C11 C1 C6 C7 -3.4(6) . . . . ? C2 C1 C6 C5 -1.7(6) . . . . ? C11 C1 C6 C5 175.0(4) . . . . ? C5 C6 C7 C8 -1.1(6) . . . . ? C1 C6 C7 C8 177.4(4) . . . . ? C6 C7 C8 C9 -0.4(7) . . . . ? C7 C8 C9 C10 1.4(8) . . . . ? C8 C9 C10 C5 -0.8(8) . . . . ? C6 C5 C10 C9 -0.8(8) . . . . ? C4 C5 C10 C9 -179.5(5) . . . . ? C2 C1 C11 C12 -82.2(5) . . . . ? C6 C1 C11 C12 101.2(5) . . . . ? C2 C1 C11 C16 100.1(5) . . . . ? C6 C1 C11 C16 -76.5(5) . . . . ? C16 C11 C12 N2 -174.8(4) . . . . ? C1 C11 C12 N2 7.6(6) . . . . ? C16 C11 C12 C13 1.4(6) . . . . ? C1 C11 C12 C13 -176.3(4) . . . . ? C16 C11 C12 V1 -130.3(4) . . . . ? C1 C11 C12 V1 52.0(4) . . . . ? P2 N2 C12 C11 -149.7(5) . . . . ? P2' N2 C12 C11 -152.3(4) . . . . ? V1 N2 C12 C11 67.1(4) . . . . ? P2 N2 C12 C13 34.3(7) . . . . ? P2' N2 C12 C13 31.6(6) . . . . ? V1 N2 C12 C13 -109.0(4) . . . . ? P2 N2 C12 V1 143.2(5) . . . . ? P2' N2 C12 V1 140.6(4) . . . . ? N4 V1 C12 C11 -133.8(6) . . . . ? N3' V1 C12 C11 126.6(8) . . . . ? N4' V1 C12 C11 -100.3(8) . . . . ? N3 V1 C12 C11 113.6(3) . . . . ? N2 V1 C12 C11 -126.1(4) . . . . ? N1 V1 C12 C11 7.0(3) . . . . ? N4 V1 C12 N2 -7.7(7) . . . . ? N3' V1 C12 N2 -107.3(8) . . . . ? N4' V1 C12 N2 25.8(9) . . . . ? N3 V1 C12 N2 -120.3(3) . . . . ? N1 V1 C12 N2 133.2(3) . . . . ? N4 V1 C12 C13 97.6(7) . . . . ? N3' V1 C12 C13 -2.0(9) . . . . ? N4' V1 C12 C13 131.1(9) . . . . ? N3 V1 C12 C13 -15.0(4) . . . . ? N2 V1 C12 C13 105.3(5) . . . . ? N1 V1 C12 C13 -121.5(4) . . . . ? C11 C12 C13 C14 -0.7(7) . . . . ? N2 C12 C13 C14 175.4(4) . . . . ? V1 C12 C13 C14 115.9(5) . . . . ? C12 C13 C14 C15 -0.8(7) . . . . ? C13 C14 C15 C20 -177.5(5) . . . . ? C13 C14 C15 C16 1.5(7) . . . . ? C14 C15 C16 C17 177.6(4) . . . . ? C20 C15 C16 C17 -3.4(6) . . . . ? C14 C15 C16 C11 -0.8(7) . . . . ? C20 C15 C16 C11 178.2(4) . . . . ? C12 C11 C16 C15 -0.7(6) . . . . ? C1 C11 C16 C15 177.0(4) . . . . ? C12 C11 C16 C17 -178.9(4) . . . . ? C1 C11 C16 C17 -1.2(6) . . . . ? C15 C16 C17 C18 3.1(7) . . . . ? C11 C16 C17 C18 -178.6(4) . . . . ? C16 C17 C18 C19 -0.1(7) . . . . ? C17 C18 C19 C20 -2.7(7) . . . . ? C18 C19 C20 C15 2.3(8) . . . . ? C14 C15 C20 C19 179.8(5) . . . . ? C16 C15 C20 C19 0.8(7) . . . . ? N1 P1 C21 C22 24.5(5) . . . . ? C27 P1 C21 C22 -88.7(4) . . . . ? C27' P1 C21 C22 -77.0(6) . . . . ? S1 P1 C21 C22 154.5(4) . . . . ? N1 P1 C21 C26 -159.2(4) . . . . ? C27 P1 C21 C26 87.5(5) . . . . ? C27' P1 C21 C26 99.2(6) . . . . ? S1 P1 C21 C26 -29.3(4) . . . . ? C26 C21 C22 C23 2.1(8) . . . . ? P1 C21 C22 C23 178.3(4) . . . . ? C21 C22 C23 C24 -3.4(8) . . . . ? C22 C23 C24 C25 2.9(9) . . . . ? C23 C24 C25 C26 -1.2(10) . . . . ? C24 C25 C26 C21 -0.2(9) . . . . ? C22 C21 C26 C25 -0.2(8) . . . . ? P1 C21 C26 C25 -176.6(4) . . . . ? N1 P1 C27 C28 -92.3(3) . . . . ? C21 P1 C27 C28 20.7(4) . . . . ? C27' P1 C27 C28 -32(2) . . . . ? S1 P1 C27 C28 140.6(3) . . . . ? N1 P1 C27 C32 89.0(3) . . . . ? C21 P1 C27 C32 -158.1(3) . . . . ? C27' P1 C27 C32 149(3) . . . . ? S1 P1 C27 C32 -38.2(3) . . . . ? C32 C27 C28 C29 0.0 . . . . ? P1 C27 C28 C29 -178.8(4) . . . . ? C27 C28 C29 C30 0.0 . . . . ? C28 C29 C30 C31 0.0 . . . . ? C29 C30 C31 C32 0.0 . . . . ? C30 C31 C32 C27 0.0 . . . . ? C28 C27 C32 C31 0.0 . . . . ? P1 C27 C32 C31 178.8(4) . . . . ? C12 N2 P2 C39 148.4(5) . . . . ? P2' N2 P2 C39 157.9(18) . . . . ? V1 N2 P2 C39 -75.5(4) . . . . ? C12 N2 P2 C33 35.6(6) . . . . ? P2' N2 P2 C33 45.1(14) . . . . ? V1 N2 P2 C33 171.7(4) . . . . ? C12 N2 P2 S2 -86.1(5) . . . . ? P2' N2 P2 S2 -76.6(15) . . . . ? V1 N2 P2 S2 49.9(4) . . . . ? N2 P2 C33 C34 57.9(6) . . . . ? C39 P2 C33 C34 -52.6(7) . . . . ? S2 P2 C33 C34 -173.9(5) . . . . ? N2 P2 C33 C38 -126.6(7) . . . . ? C39 P2 C33 C38 123.0(7) . . . . ? S2 P2 C33 C38 1.7(9) . . . . ? C38 C33 C34 C35 0.0 . . . . ? P2 C33 C34 C35 175.7(9) . . . . ? C33 C34 C35 C36 0.0 . . . . ? C34 C35 C36 C37 0.0 . . . . ? C35 C36 C37 C38 0.0 . . . . ? C36 C37 C38 C33 0.0 . . . . ? C34 C33 C38 C37 0.0 . . . . ? P2 C33 C38 C37 -175.5(9) . . . . ? N2 P2 C39 C40 150.7(4) . . . . ? C33 P2 C39 C40 -99.7(6) . . . . ? S2 P2 C39 C40 20.5(6) . . . . ? N2 P2 C39 C44 -31.4(5) . . . . ? C33 P2 C39 C44 78.2(6) . . . . ? S2 P2 C39 C44 -161.7(4) . . . . ? C44 C39 C40 C41 0.0 . . . . ? P2 C39 C40 C41 177.8(6) . . . . ? C39 C40 C41 C42 0.0 . . . . ? C40 C41 C42 C43 0.0 . . . . ? C41 C42 C43 C44 0.0 . . . . ? C42 C43 C44 C39 0.0 . . . . ? C40 C39 C44 C43 0.0 . . . . ? P2 C39 C44 C43 -177.8(6) . . . . ? N4 V1 N3 C45 -34.5(8) . . . . ? N3' V1 N3 C45 -45.3(13) . . . . ? N4' V1 N3 C45 -32.6(11) . . . . ? N2 V1 N3 C45 86.6(7) . . . . ? N1 V1 N3 C45 -150.4(6) . . . . ? C12 V1 N3 C45 115.7(7) . . . . ? N4 V1 N3 C46 155.7(6) . . . . ? N3' V1 N3 C46 144.9(14) . . . . ? N4' V1 N3 C46 157.6(9) . . . . ? N2 V1 N3 C46 -83.3(6) . . . . ? N1 V1 N3 C46 39.8(6) . . . . ? C12 V1 N3 C46 -54.2(6) . . . . ? N3' V1 N4 C47 -171.1(10) . . . . ? N4' V1 N4 C47 5.5(16) . . . . ? N3 V1 N4 C47 -177.9(6) . . . . ? N2 V1 N4 C47 69.0(7) . . . . ? N1 V1 N4 C47 -64.3(7) . . . . ? C12 V1 N4 C47 73.7(9) . . . . ? N3' V1 N4 C48 6.0(13) . . . . ? N4' V1 N4 C48 -177(2) . . . . ? N3 V1 N4 C48 -0.8(13) . . . . ? N2 V1 N4 C48 -113.9(12) . . . . ? N1 V1 N4 C48 112.8(12) . . . . ? C12 V1 N4 C48 -109.2(13) . . . . ? N1 P1 C27' C28' -36.3(10) . . . . ? C27 P1 C27' C28' -159(3) . . . . ? C21 P1 C27' C28' 71.3(10) . . . . ? S1 P1 C27' C28' -167.2(7) . . . . ? N1 P1 C27' C32' 142.4(8) . . . . ? C27 P1 C27' C32' 20(2) . . . . ? C21 P1 C27' C32' -110.0(8) . . . . ? S1 P1 C27' C32' 11.5(10) . . . . ? C32' C27' C28' C29' 0.0 . . . . ? P1 C27' C28' C29' 178.6(13) . . . . ? C27' C28' C29' C30' 0.0 . . . . ? C28' C29' C30' C31' 0.0 . . . . ? C29' C30' C31' C32' 0.0 . . . . ? C30' C31' C32' C27' 0.0 . . . . ? C28' C27' C32' C31' 0.0 . . . . ? P1 C27' C32' C31' -178.7(12) . . . . ? N4 V1 N3' C46' -159.4(17) . . . . ? N4' V1 N3' C46' -160.9(16) . . . . ? N3 V1 N3' C46' 9.3(12) . . . . ? N2 V1 N3' C46' -52.9(17) . . . . ? N1 V1 N3' C46' 97.3(15) . . . . ? C12 V1 N3' C46' -13.2(18) . . . . ? N4 V1 N3' C45' 37(2) . . . . ? N4' V1 N3' C45' 35(3) . . . . ? N3 V1 N3' C45' -154(3) . . . . ? N2 V1 N3' C45' 143(2) . . . . ? N1 V1 N3' C45' -66(3) . . . . ? C12 V1 N3' C45' -177(2) . . . . ? N4 V1 N4' C47' -177(3) . . . . ? N3' V1 N4' C47' -174(2) . . . . ? N3 V1 N4' C47' 178.9(19) . . . . ? N2 V1 N4' C47' 59(2) . . . . ? N1 V1 N4' C47' -60(2) . . . . ? C12 V1 N4' C47' 45(2) . . . . ? N4 V1 N4' C48' -0.2(15) . . . . ? N3' V1 N4' C48' 3(2) . . . . ? N3 V1 N4' C48' -4(2) . . . . ? N2 V1 N4' C48' -124.4(18) . . . . ? N1 V1 N4' C48' 116.3(18) . . . . ? C12 V1 N4' C48' -138.4(16) . . . . ? C38' C33' C34' C35' 0.0 . . . . ? P2' C33' C34' C35' 179.6(15) . . . . ? C33' C34' C35' C36' 0.0 . . . . ? C34' C35' C36' C37' 0.0 . . . . ? C35' C36' C37' C38' 0.0 . . . . ? C36' C37' C38' C33' 0.0 . . . . ? C34' C33' C38' C37' 0.0 . . . . ? P2' C33' C38' C37' -179.6(14) . . . . ? C12 N2 P2' C39' 163.8(4) . . . . ? P2 N2 P2' C39' -8.2(13) . . . . ? V1 N2 P2' C39' -70.3(5) . . . . ? C12 N2 P2' C33' 58.1(8) . . . . ? P2 N2 P2' C33' -113.8(18) . . . . ? V1 N2 P2' C33' -175.9(7) . . . . ? C12 N2 P2' S2' -73.7(5) . . . . ? P2 N2 P2' S2' 114.3(17) . . . . ? V1 N2 P2' S2' 52.2(5) . . . . ? C34' C33' P2' N2 33.3(11) . . . . ? C38' C33' P2' N2 -147.1(9) . . . . ? C34' C33' P2' C39' -71.7(10) . . . . ? C38' C33' P2' C39' 108.0(10) . . . . ? C34' C33' P2' S2' 166.8(8) . . . . ? C38' C33' P2' S2' -13.6(14) . . . . ? N2 P2' C39' C40' 110.1(5) . . . . ? C33' P2' C39' C40' -142.0(7) . . . . ? S2' P2' C39' C40' -17.4(7) . . . . ? N2 P2' C39' C44' -69.9(6) . . . . ? C33' P2' C39' C44' 38.1(8) . . . . ? S2' P2' C39' C44' 162.6(4) . . . . ? C44' C39' C40' C41' 0.0 . . . . ? P2' C39' C40' C41' -180.0(7) . . . . ? C39' C40' C41' C42' 0.0 . . . . ? C40' C41' C42' C43' 0.0 . . . . ? C41' C42' C43' C44' 0.0 . . . . ? C42' C43' C44' C39' 0.0 . . . . ? C40' C39' C44' C43' 0.0 . . . . ? P2' C39' C44' C43' 180.0(7) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.556 _refine_diff_density_min -0.737 _refine_diff_density_rms 0.078 # Attachment '- compound 23.cif' data_compound23 _database_code_depnum_ccdc_archive 'CCDC 791868' #TrackingRef '- compound 23.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C40 H50 N4 O2 V' _chemical_formula_sum 'C40 H50 N4 O2 V' _chemical_formula_weight 669.78 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 11.0271(11) _cell_length_b 11.4224(12) _cell_length_c 14.9238(16) _cell_angle_alpha 85.963(9) _cell_angle_beta 85.289(11) _cell_angle_gamma 83.182(9) _cell_volume 1856.6(3) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 8354 _cell_measurement_theta_min 1.80 _cell_measurement_theta_max 32.78 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 714 _exptl_absorpt_coefficient_mu 0.305 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9248 _exptl_absorpt_correction_T_max 0.9415 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Rigaku Saturn70 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 28339 _diffrn_reflns_av_R_equivalents 0.0361 _diffrn_reflns_av_sigmaI/netI 0.1042 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 32.87 _reflns_number_total 21065 _reflns_number_gt 14747 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure 4.0' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2009)' _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^)+(0.0214P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0485(8) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.005(8) _refine_ls_number_reflns 21065 _refine_ls_number_parameters 872 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0524 _refine_ls_R_factor_gt 0.0371 _refine_ls_wR_factor_ref 0.0825 _refine_ls_wR_factor_gt 0.0766 _refine_ls_goodness_of_fit_ref 0.929 _refine_ls_restrained_S_all 0.929 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V1 V 0.79017(3) 0.21470(2) 0.062109(19) 0.01377(7) Uani 1 1 d . . . V2 V 0.04032(3) 0.70119(2) 0.563508(19) 0.01454(7) Uani 1 1 d . . . N1 N 0.70337(14) 0.33329(13) -0.04264(10) 0.0146(3) Uani 1 1 d . . . N2 N 0.79995(14) 0.38647(13) 0.11563(10) 0.0153(3) Uani 1 1 d . . . N3 N 0.88264(15) 0.13962(14) 0.15502(10) 0.0175(3) Uani 1 1 d . . . N4 N 0.75330(15) 0.07923(14) 0.00978(10) 0.0169(3) Uani 1 1 d . . . N5 N 0.12540(14) 0.79779(14) 0.44494(10) 0.0170(3) Uani 1 1 d . . . N6 N 0.01586(14) 0.58501(14) 0.45645(10) 0.0165(3) Uani 1 1 d . . . N7 N -0.04714(14) 0.60473(14) 0.64691(10) 0.0178(3) Uani 1 1 d . . . N8 N 0.08661(15) 0.80403(14) 0.64470(10) 0.0192(3) Uani 1 1 d . . . O1 O 0.93647(11) 0.23512(11) -0.01978(8) 0.0157(3) Uani 1 1 d . . . O2 O 0.63286(12) 0.22783(11) 0.13546(8) 0.0164(3) Uani 1 1 d . . . O3 O -0.10639(12) 0.80366(11) 0.52838(8) 0.0178(3) Uani 1 1 d . . . O4 O 0.19751(11) 0.60034(11) 0.56754(8) 0.0173(3) Uani 1 1 d . . . C1 C 0.63473(17) 0.53026(16) 0.00864(12) 0.0162(4) Uani 1 1 d . . . C2 C 0.60533(17) 0.42395(16) -0.02116(12) 0.0153(4) Uani 1 1 d . . . C3 C 0.48413(18) 0.40454(18) -0.02916(13) 0.0209(4) Uani 1 1 d . . . H3 H 0.4660 0.3329 -0.0509 0.025 Uiso 1 1 calc R . . C4 C 0.39078(19) 0.49127(19) -0.00499(14) 0.0253(4) Uani 1 1 d . . . H4 H 0.3081 0.4803 -0.0118 0.030 Uiso 1 1 calc R . . C5 C 0.41799(19) 0.59432(19) 0.02925(14) 0.0253(4) Uani 1 1 d . . . H5 H 0.3530 0.6520 0.0474 0.030 Uiso 1 1 calc R . . C6 C 0.53851(19) 0.61513(17) 0.03755(13) 0.0208(4) Uani 1 1 d . . . C7 C 0.5615(2) 0.72689(19) 0.07815(14) 0.0280(5) Uani 1 1 d . . . H7A H 0.5336 0.7953 0.0387 0.042 Uiso 1 1 calc R . . H7B H 0.6494 0.7256 0.0848 0.042 Uiso 1 1 calc R . . H7C H 0.5166 0.7324 0.1374 0.042 Uiso 1 1 calc R . . C8 C 0.76700(17) 0.55232(16) 0.00562(12) 0.0160(4) Uani 1 1 d . . . C9 C 0.84845(17) 0.48088(16) 0.05972(12) 0.0158(4) Uani 1 1 d . . . C10 C 0.97098(18) 0.49754(17) 0.05789(13) 0.0196(4) Uani 1 1 d . . . H10 H 1.0247 0.4483 0.0948 0.024 Uiso 1 1 calc R . . C11 C 1.01411(18) 0.58800(18) 0.00079(13) 0.0220(4) Uani 1 1 d . . . H11 H 1.0976 0.6015 -0.0007 0.026 Uiso 1 1 calc R . . C12 C 0.93519(18) 0.65822(17) -0.05383(13) 0.0209(4) Uani 1 1 d . . . H12 H 0.9655 0.7197 -0.0924 0.025 Uiso 1 1 calc R . . C13 C 0.81255(18) 0.64036(16) -0.05324(12) 0.0180(4) Uani 1 1 d . . . C14 C 0.73233(19) 0.71320(18) -0.12012(13) 0.0242(4) Uani 1 1 d . . . H14A H 0.6792 0.6624 -0.1447 0.036 Uiso 1 1 calc R . . H14B H 0.7844 0.7470 -0.1693 0.036 Uiso 1 1 calc R . . H14C H 0.6818 0.7770 -0.0894 0.036 Uiso 1 1 calc R . . C15 C 0.74033(17) 0.32612(16) -0.12690(12) 0.0169(4) Uani 1 1 d . . . H15 H 0.6916 0.3711 -0.1695 0.020 Uiso 1 1 calc R . . C16 C 0.84865(17) 0.25605(17) -0.16161(12) 0.0164(4) Uani 1 1 d . . . C17 C 0.94904(17) 0.22089(16) -0.10794(12) 0.0155(4) Uani 1 1 d . . . C18 C 1.06366(17) 0.17417(17) -0.15090(12) 0.0174(4) Uani 1 1 d . . . C19 C 1.06849(19) 0.15726(19) -0.24231(13) 0.0228(4) Uani 1 1 d . . . H19 H 1.1437 0.1241 -0.2708 0.027 Uiso 1 1 calc R . . C20 C 0.96789(19) 0.18667(19) -0.29499(13) 0.0247(4) Uani 1 1 d . . . H20 H 0.9745 0.1710 -0.3570 0.030 Uiso 1 1 calc R . . C21 C 0.86038(18) 0.23822(18) -0.25537(12) 0.0205(4) Uani 1 1 d . . . H21 H 0.7930 0.2623 -0.2908 0.025 Uiso 1 1 calc R . . C22 C 1.17832(18) 0.14519(18) -0.09767(13) 0.0226(4) Uani 1 1 d . . . C23 C 1.20648(19) 0.2584(2) -0.05704(15) 0.0276(5) Uani 1 1 d . . . H23A H 1.2262 0.3168 -0.1057 0.041 Uiso 1 1 calc R . . H23B H 1.2764 0.2397 -0.0200 0.041 Uiso 1 1 calc R . . H23C H 1.1348 0.2907 -0.0196 0.041 Uiso 1 1 calc R . . C24 C 1.1575(2) 0.0486(2) -0.02287(15) 0.0269(5) Uani 1 1 d . . . H24A H 1.0867 0.0756 0.0176 0.040 Uiso 1 1 calc R . . H24B H 1.2304 0.0323 0.0114 0.040 Uiso 1 1 calc R . . H24C H 1.1422 -0.0235 -0.0498 0.040 Uiso 1 1 calc R . . C25 C 1.2920(2) 0.0997(2) -0.15705(15) 0.0363(6) Uani 1 1 d . . . H25A H 1.2773 0.0270 -0.1834 0.054 Uiso 1 1 calc R . . H25B H 1.3625 0.0835 -0.1203 0.054 Uiso 1 1 calc R . . H25C H 1.3088 0.1597 -0.2053 0.054 Uiso 1 1 calc R . . C26 C 0.75068(18) 0.41441(17) 0.19456(12) 0.0178(4) Uani 1 1 d . . . H26 H 0.7680 0.4869 0.2154 0.021 Uiso 1 1 calc R . . C27 C 0.67224(17) 0.34559(16) 0.25334(12) 0.0169(4) Uani 1 1 d . . . C28 C 0.60782(17) 0.25980(16) 0.21895(12) 0.0172(4) Uani 1 1 d . . . C29 C 0.51146(18) 0.21112(17) 0.27567(12) 0.0197(4) Uani 1 1 d . . . C30 C 0.4905(2) 0.24930(19) 0.36295(13) 0.0249(4) Uani 1 1 d . . . H30 H 0.4278 0.2176 0.4013 0.030 Uiso 1 1 calc R . . C31 C 0.5559(2) 0.33117(18) 0.39739(13) 0.0247(5) Uani 1 1 d . . . H31 H 0.5394 0.3526 0.4579 0.030 Uiso 1 1 calc R . . C32 C 0.64396(19) 0.37978(17) 0.34236(12) 0.0214(4) Uani 1 1 d . . . H32 H 0.6871 0.4377 0.3644 0.026 Uiso 1 1 calc R . . C33 C 0.4361(2) 0.12139(19) 0.24117(13) 0.0255(5) Uani 1 1 d . . . C34 C 0.3675(2) 0.1763(2) 0.15942(15) 0.0308(5) Uani 1 1 d . . . H34A H 0.3239 0.1166 0.1358 0.046 Uiso 1 1 calc R . . H34B H 0.4265 0.2043 0.1124 0.046 Uiso 1 1 calc R . . H34C H 0.3087 0.2429 0.1782 0.046 Uiso 1 1 calc R . . C35 C 0.5197(2) 0.00968(19) 0.21410(16) 0.0315(5) Uani 1 1 d . . . H35A H 0.5646 -0.0240 0.2656 0.047 Uiso 1 1 calc R . . H35B H 0.5779 0.0304 0.1640 0.047 Uiso 1 1 calc R . . H35C H 0.4696 -0.0485 0.1955 0.047 Uiso 1 1 calc R . . C36 C 0.3401(2) 0.0813(2) 0.31334(16) 0.0396(6) Uani 1 1 d . . . H36A H 0.3813 0.0397 0.3641 0.059 Uiso 1 1 calc R . . H36B H 0.2905 0.0282 0.2876 0.059 Uiso 1 1 calc R . . H36C H 0.2870 0.1505 0.3345 0.059 Uiso 1 1 calc R . . C37 C 0.98962(19) 0.18706(18) 0.18347(13) 0.0248(4) Uani 1 1 d . . . H37A H 0.9663 0.2305 0.2377 0.037 Uiso 1 1 calc R . . H37B H 1.0212 0.2405 0.1352 0.037 Uiso 1 1 calc R . . H37C H 1.0532 0.1220 0.1966 0.037 Uiso 1 1 calc R . . C38 C 0.8446(2) 0.04505(18) 0.21789(13) 0.0258(5) Uani 1 1 d . . . H38A H 0.9161 -0.0110 0.2314 0.039 Uiso 1 1 calc R . . H38B H 0.7848 0.0040 0.1909 0.039 Uiso 1 1 calc R . . H38C H 0.8071 0.0786 0.2737 0.039 Uiso 1 1 calc R . . C39 C 0.63709(19) 0.07240(19) -0.02939(14) 0.0240(5) Uani 1 1 d . . . H39A H 0.6491 0.0810 -0.0952 0.036 Uiso 1 1 calc R . . H39B H 0.5762 0.1358 -0.0079 0.036 Uiso 1 1 calc R . . H39C H 0.6081 -0.0042 -0.0113 0.036 Uiso 1 1 calc R . . C40 C 0.83906(19) -0.02417(18) -0.00866(14) 0.0257(5) Uani 1 1 d . . . H40A H 0.8013 -0.0956 0.0124 0.038 Uiso 1 1 calc R . . H40B H 0.9132 -0.0214 0.0228 0.038 Uiso 1 1 calc R . . H40C H 0.8606 -0.0254 -0.0736 0.038 Uiso 1 1 calc R . . C41 C 0.18215(17) 0.66651(17) 0.32302(12) 0.0180(4) Uani 1 1 d . . . C42 C 0.21954(17) 0.73632(17) 0.38685(12) 0.0180(4) Uani 1 1 d . . . C43 C 0.34248(18) 0.7404(2) 0.39742(13) 0.0252(5) Uani 1 1 d . . . H43 H 0.3669 0.7918 0.4382 0.030 Uiso 1 1 calc R . . C44 C 0.42927(19) 0.6689(2) 0.34807(14) 0.0317(5) Uani 1 1 d . . . H44 H 0.5138 0.6721 0.3544 0.038 Uiso 1 1 calc R . . C45 C 0.39427(19) 0.5924(2) 0.28942(14) 0.0303(5) Uani 1 1 d . . . H45 H 0.4549 0.5414 0.2578 0.036 Uiso 1 1 calc R . . C46 C 0.27061(19) 0.58961(18) 0.27636(13) 0.0231(4) Uani 1 1 d . . . C47 C 0.2334(2) 0.5001(2) 0.21741(15) 0.0331(5) Uani 1 1 d . . . H47A H 0.1838 0.4460 0.2539 0.050 Uiso 1 1 calc R . . H47B H 0.3068 0.4551 0.1903 0.050 Uiso 1 1 calc R . . H47C H 0.1854 0.5409 0.1697 0.050 Uiso 1 1 calc R . . C48 C 0.04789(17) 0.67555(17) 0.30697(12) 0.0170(4) Uani 1 1 d . . . C49 C -0.03432(18) 0.63445(16) 0.37386(12) 0.0174(4) Uani 1 1 d . . . C50 C -0.16005(18) 0.64586(17) 0.36355(13) 0.0213(4) Uani 1 1 d . . . H50 H -0.2155 0.6185 0.4103 0.026 Uiso 1 1 calc R . . C51 C -0.20223(19) 0.69831(18) 0.28303(14) 0.0236(4) Uani 1 1 d . . . H51 H -0.2871 0.7055 0.2740 0.028 Uiso 1 1 calc R . . C52 C -0.12062(18) 0.74008(17) 0.21598(13) 0.0220(4) Uani 1 1 d . . . H52 H -0.1509 0.7754 0.1615 0.026 Uiso 1 1 calc R . . C53 C 0.00496(18) 0.73159(17) 0.22643(12) 0.0190(4) Uani 1 1 d . . . C54 C 0.0890(2) 0.78724(19) 0.15607(14) 0.0268(5) Uani 1 1 d . . . H54A H 0.0467 0.8069 0.1008 0.040 Uiso 1 1 calc R . . H54B H 0.1622 0.7318 0.1434 0.040 Uiso 1 1 calc R . . H54C H 0.1128 0.8594 0.1780 0.040 Uiso 1 1 calc R . . C55 C 0.08516(18) 0.90474(17) 0.41957(13) 0.0187(4) Uani 1 1 d . . . H55 H 0.1299 0.9415 0.3705 0.022 Uiso 1 1 calc R . . C56 C -0.02153(18) 0.97344(17) 0.45901(12) 0.0180(4) Uani 1 1 d . . . C57 C -0.11815(18) 0.91890(17) 0.50824(12) 0.0182(4) Uani 1 1 d . . . C58 C -0.23015(19) 0.99059(18) 0.53174(13) 0.0221(4) Uani 1 1 d . . . C59 C -0.2348(2) 1.11141(18) 0.51018(14) 0.0266(5) Uani 1 1 d . . . H59 H -0.3073 1.1602 0.5283 0.032 Uiso 1 1 calc R . . C60 C -0.1391(2) 1.16513(18) 0.46348(14) 0.0284(5) Uani 1 1 d . . . H60 H -0.1461 1.2482 0.4508 0.034 Uiso 1 1 calc R . . C61 C -0.03475(19) 1.09485(17) 0.43630(13) 0.0226(4) Uani 1 1 d . . . H61 H 0.0295 1.1293 0.4015 0.027 Uiso 1 1 calc R . . C62 C -0.34311(19) 0.93562(19) 0.57557(14) 0.0275(5) Uani 1 1 d . . . C63 C -0.4530(2) 1.0294(2) 0.59676(18) 0.0458(7) Uani 1 1 d . . . H63A H -0.5256 0.9898 0.6167 0.069 Uiso 1 1 calc R . . H63B H -0.4692 1.0804 0.5425 0.069 Uiso 1 1 calc R . . H63C H -0.4339 1.0773 0.6446 0.069 Uiso 1 1 calc R . . C64 C -0.3150(2) 0.8667(2) 0.66486(15) 0.0343(6) Uani 1 1 d . . . H64A H -0.2940 0.9210 0.7077 0.052 Uiso 1 1 calc R . . H64B H -0.2459 0.8057 0.6543 0.052 Uiso 1 1 calc R . . H64C H -0.3871 0.8294 0.6896 0.052 Uiso 1 1 calc R . . C65 C -0.3833(2) 0.8522(2) 0.50890(16) 0.0357(6) Uani 1 1 d . . . H65A H -0.3166 0.7895 0.4964 0.054 Uiso 1 1 calc R . . H65B H -0.4028 0.8973 0.4526 0.054 Uiso 1 1 calc R . . H65C H -0.4558 0.8171 0.5355 0.054 Uiso 1 1 calc R . . C66 C 0.06354(18) 0.47677(17) 0.45639(13) 0.0182(4) Uani 1 1 d . . . H66 H 0.0406 0.4308 0.4113 0.022 Uiso 1 1 calc R . . C67 C 0.14901(17) 0.41786(17) 0.51855(12) 0.0175(4) Uani 1 1 d . . . C68 C 0.21997(17) 0.48428(16) 0.56686(12) 0.0162(4) Uani 1 1 d . . . C69 C 0.32039(18) 0.42296(18) 0.61301(12) 0.0196(4) Uani 1 1 d . . . C70 C 0.33753(19) 0.30038(18) 0.61096(13) 0.0225(4) Uani 1 1 d . . . H70 H 0.4023 0.2585 0.6425 0.027 Uiso 1 1 calc R . . C71 C 0.26549(19) 0.23528(18) 0.56554(14) 0.0247(5) Uani 1 1 d . . . H71 H 0.2797 0.1515 0.5674 0.030 Uiso 1 1 calc R . . C72 C 0.17369(18) 0.29502(17) 0.51810(13) 0.0216(4) Uani 1 1 d . . . H72 H 0.1262 0.2524 0.4844 0.026 Uiso 1 1 calc R . . C73 C 0.40492(19) 0.48931(19) 0.66188(14) 0.0257(5) Uani 1 1 d . . . C74 C 0.3317(2) 0.5589(2) 0.73846(14) 0.0352(6) Uani 1 1 d . . . H74A H 0.2698 0.6175 0.7126 0.053 Uiso 1 1 calc R . . H74B H 0.3878 0.5991 0.7700 0.053 Uiso 1 1 calc R . . H74C H 0.2913 0.5040 0.7811 0.053 Uiso 1 1 calc R . . C75 C 0.5078(2) 0.4076(2) 0.70434(18) 0.0443(7) Uani 1 1 d . . . H75A H 0.4722 0.3509 0.7482 0.066 Uiso 1 1 calc R . . H75B H 0.5588 0.4547 0.7348 0.066 Uiso 1 1 calc R . . H75C H 0.5581 0.3649 0.6572 0.066 Uiso 1 1 calc R . . C76 C 0.4686(2) 0.5769(2) 0.59449(15) 0.0308(5) Uani 1 1 d . . . H76A H 0.5207 0.5327 0.5490 0.046 Uiso 1 1 calc R . . H76B H 0.5190 0.6222 0.6271 0.046 Uiso 1 1 calc R . . H76C H 0.4063 0.6311 0.5649 0.046 Uiso 1 1 calc R . . C77 C -0.15820(18) 0.55757(19) 0.62610(14) 0.0269(5) Uani 1 1 d . . . H77A H -0.1390 0.4738 0.6143 0.040 Uiso 1 1 calc R . . H77B H -0.1907 0.6012 0.5727 0.040 Uiso 1 1 calc R . . H77C H -0.2195 0.5660 0.6773 0.040 Uiso 1 1 calc R . . C78 C -0.00100(19) 0.54640(19) 0.72957(13) 0.0249(4) Uani 1 1 d . . . H78A H -0.0687 0.5433 0.7762 0.037 Uiso 1 1 calc R . . H78B H 0.0612 0.5908 0.7501 0.037 Uiso 1 1 calc R . . H78C H 0.0354 0.4659 0.7179 0.037 Uiso 1 1 calc R . . C79 C 0.0054(2) 0.8539(2) 0.71831(14) 0.0288(5) Uani 1 1 d . . . H79A H 0.0512 0.8538 0.7719 0.043 Uiso 1 1 calc R . . H79B H -0.0628 0.8063 0.7320 0.043 Uiso 1 1 calc R . . H79C H -0.0266 0.9352 0.7004 0.043 Uiso 1 1 calc R . . C80 C 0.2011(2) 0.8563(2) 0.63301(15) 0.0280(5) Uani 1 1 d . . . H80A H 0.1857 0.9383 0.6091 0.042 Uiso 1 1 calc R . . H80B H 0.2583 0.8114 0.5908 0.042 Uiso 1 1 calc R . . H80C H 0.2366 0.8543 0.6913 0.042 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 0.01638(16) 0.01385(16) 0.01115(14) -0.00046(11) -0.00014(12) -0.00279(12) V2 0.01629(16) 0.01358(15) 0.01352(15) 0.00064(12) -0.00104(12) -0.00170(12) N1 0.0132(7) 0.0157(8) 0.0153(7) -0.0008(6) -0.0012(6) -0.0034(6) N2 0.0185(8) 0.0138(8) 0.0137(7) 0.0015(6) -0.0020(6) -0.0031(6) N3 0.0196(8) 0.0181(8) 0.0141(7) 0.0013(6) -0.0009(6) -0.0013(6) N4 0.0181(8) 0.0160(8) 0.0173(8) -0.0028(6) -0.0006(6) -0.0045(6) N5 0.0147(8) 0.0204(8) 0.0166(7) -0.0012(6) -0.0022(6) -0.0038(6) N6 0.0135(8) 0.0206(8) 0.0153(7) -0.0002(6) -0.0007(6) -0.0026(6) N7 0.0192(8) 0.0179(8) 0.0161(7) 0.0007(6) -0.0006(7) -0.0027(7) N8 0.0235(9) 0.0175(8) 0.0170(8) -0.0028(6) -0.0014(7) -0.0035(7) O1 0.0168(7) 0.0198(7) 0.0107(6) -0.0021(5) -0.0004(5) -0.0028(5) O2 0.0166(7) 0.0196(7) 0.0131(6) -0.0030(5) 0.0021(5) -0.0033(5) O3 0.0183(7) 0.0138(7) 0.0204(6) 0.0029(5) -0.0010(6) -0.0010(5) O4 0.0162(7) 0.0153(7) 0.0207(7) -0.0012(5) -0.0035(6) -0.0013(5) C1 0.0164(9) 0.0167(9) 0.0151(8) 0.0020(7) -0.0004(7) -0.0023(7) C2 0.0148(9) 0.0166(9) 0.0134(8) 0.0013(7) 0.0003(7) 0.0005(7) C3 0.0182(10) 0.0229(10) 0.0214(9) -0.0021(8) 0.0008(8) -0.0027(8) C4 0.0143(9) 0.0313(12) 0.0301(11) -0.0051(9) -0.0002(8) -0.0010(8) C5 0.0188(10) 0.0255(11) 0.0298(11) -0.0030(9) 0.0037(9) 0.0017(8) C6 0.0222(10) 0.0189(10) 0.0207(9) -0.0021(8) 0.0026(8) -0.0029(8) C7 0.0308(12) 0.0224(11) 0.0297(11) -0.0053(9) 0.0036(10) -0.0005(9) C8 0.0177(9) 0.0164(9) 0.0143(8) -0.0020(7) -0.0009(7) -0.0036(7) C9 0.0193(9) 0.0137(9) 0.0147(8) -0.0012(7) -0.0001(7) -0.0039(7) C10 0.0187(10) 0.0187(10) 0.0226(9) -0.0013(8) -0.0047(8) -0.0041(8) C11 0.0170(10) 0.0243(11) 0.0258(10) -0.0006(8) 0.0005(8) -0.0087(8) C12 0.0210(10) 0.0197(10) 0.0223(10) -0.0002(8) 0.0027(8) -0.0077(8) C13 0.0218(10) 0.0158(9) 0.0160(8) -0.0011(7) 0.0025(8) -0.0026(8) C14 0.0277(11) 0.0230(11) 0.0212(10) 0.0046(8) -0.0020(9) -0.0037(9) C15 0.0166(9) 0.0204(10) 0.0144(8) -0.0004(7) -0.0037(7) -0.0033(7) C16 0.0153(9) 0.0202(10) 0.0136(8) 0.0005(7) -0.0007(7) -0.0029(7) C17 0.0177(9) 0.0147(9) 0.0140(8) 0.0011(7) 0.0004(7) -0.0036(7) C18 0.0154(9) 0.0207(10) 0.0160(8) -0.0022(7) 0.0019(7) -0.0033(7) C19 0.0201(10) 0.0277(11) 0.0188(9) -0.0032(8) 0.0058(8) 0.0003(9) C20 0.0264(11) 0.0329(12) 0.0144(9) -0.0041(8) -0.0005(8) -0.0012(9) C21 0.0230(10) 0.0264(11) 0.0122(8) -0.0017(7) -0.0017(8) -0.0025(8) C22 0.0155(9) 0.0284(11) 0.0239(10) -0.0011(8) -0.0021(8) -0.0023(8) C23 0.0200(11) 0.0362(13) 0.0288(11) -0.0004(9) -0.0028(9) -0.0125(9) C24 0.0237(11) 0.0274(12) 0.0288(11) 0.0022(9) -0.0052(9) 0.0001(9) C25 0.0216(11) 0.0518(16) 0.0326(12) -0.0013(11) 0.0031(10) 0.0030(11) C26 0.0199(10) 0.0174(10) 0.0169(9) -0.0036(7) -0.0041(8) -0.0023(8) C27 0.0209(10) 0.0160(9) 0.0135(8) -0.0003(7) -0.0015(7) -0.0015(7) C28 0.0190(10) 0.0171(9) 0.0142(8) 0.0008(7) 0.0004(7) 0.0019(7) C29 0.0209(10) 0.0219(10) 0.0154(9) 0.0027(7) 0.0014(8) -0.0031(8) C30 0.0264(11) 0.0285(11) 0.0173(9) 0.0023(8) 0.0049(8) 0.0001(9) C31 0.0362(12) 0.0235(11) 0.0130(9) -0.0006(8) 0.0018(9) -0.0004(9) C32 0.0273(11) 0.0210(10) 0.0162(9) -0.0039(7) -0.0042(8) -0.0013(8) C33 0.0254(11) 0.0286(12) 0.0224(10) 0.0010(8) 0.0063(9) -0.0095(9) C34 0.0246(11) 0.0340(13) 0.0351(12) -0.0023(10) -0.0016(10) -0.0095(10) C35 0.0363(13) 0.0228(11) 0.0359(12) -0.0021(9) 0.0042(10) -0.0105(10) C36 0.0404(14) 0.0454(15) 0.0341(12) -0.0036(11) 0.0151(11) -0.0212(12) C37 0.0296(12) 0.0246(11) 0.0209(10) 0.0012(8) -0.0088(9) -0.0031(9) C38 0.0319(12) 0.0211(11) 0.0231(10) 0.0073(8) -0.0049(9) -0.0008(9) C39 0.0226(11) 0.0233(11) 0.0280(11) -0.0052(9) -0.0048(9) -0.0067(9) C40 0.0299(12) 0.0200(10) 0.0274(11) -0.0058(8) -0.0042(9) 0.0000(9) C41 0.0171(9) 0.0208(10) 0.0143(8) 0.0029(7) 0.0006(7) 0.0014(8) C42 0.0171(9) 0.0211(10) 0.0148(8) 0.0038(7) 0.0011(7) -0.0025(8) C43 0.0189(10) 0.0351(12) 0.0218(10) 0.0048(9) -0.0028(8) -0.0070(9) C44 0.0144(10) 0.0502(15) 0.0281(11) 0.0069(10) 0.0017(9) -0.0009(10) C45 0.0220(11) 0.0406(13) 0.0230(10) 0.0052(9) 0.0042(9) 0.0100(10) C46 0.0244(11) 0.0245(11) 0.0182(9) 0.0013(8) 0.0019(8) 0.0026(8) C47 0.0348(13) 0.0354(13) 0.0260(11) -0.0065(10) 0.0042(10) 0.0063(10) C48 0.0171(9) 0.0182(9) 0.0159(8) -0.0015(7) -0.0025(7) -0.0014(7) C49 0.0199(10) 0.0174(9) 0.0160(8) -0.0031(7) -0.0060(7) -0.0025(7) C50 0.0207(10) 0.0230(10) 0.0217(9) -0.0017(8) -0.0042(8) -0.0064(8) C51 0.0197(10) 0.0256(11) 0.0271(10) -0.0030(8) -0.0096(9) -0.0026(8) C52 0.0261(11) 0.0198(10) 0.0204(9) -0.0004(8) -0.0101(8) 0.0011(8) C53 0.0217(10) 0.0190(10) 0.0160(8) -0.0033(7) -0.0017(7) 0.0002(8) C54 0.0280(12) 0.0300(12) 0.0203(10) 0.0020(9) 0.0008(9) 0.0009(9) C55 0.0197(10) 0.0203(10) 0.0180(9) 0.0019(7) -0.0037(8) -0.0097(8) C56 0.0214(10) 0.0170(9) 0.0172(8) 0.0005(7) -0.0063(8) -0.0062(8) C57 0.0214(10) 0.0171(9) 0.0168(8) -0.0009(7) -0.0049(8) -0.0023(8) C58 0.0205(10) 0.0236(11) 0.0209(9) 0.0021(8) -0.0033(8) 0.0021(8) C59 0.0280(12) 0.0195(11) 0.0301(11) -0.0001(9) -0.0026(9) 0.0059(9) C60 0.0381(13) 0.0158(10) 0.0318(11) 0.0007(8) -0.0080(10) -0.0019(9) C61 0.0287(11) 0.0183(10) 0.0221(10) 0.0013(8) -0.0056(9) -0.0071(8) C62 0.0191(10) 0.0276(12) 0.0318(11) 0.0069(9) 0.0018(9) 0.0062(9) C63 0.0302(13) 0.0437(15) 0.0540(16) 0.0183(13) 0.0110(12) 0.0132(11) C64 0.0295(13) 0.0353(14) 0.0325(12) 0.0091(10) 0.0080(10) 0.0064(10) C65 0.0224(12) 0.0409(14) 0.0438(14) 0.0085(11) -0.0079(10) -0.0060(10) C66 0.0174(9) 0.0185(10) 0.0194(9) -0.0028(8) 0.0002(8) -0.0051(8) C67 0.0167(9) 0.0198(10) 0.0157(8) -0.0007(7) -0.0002(7) -0.0019(7) C68 0.0179(9) 0.0161(9) 0.0135(8) 0.0016(7) 0.0018(7) -0.0017(7) C69 0.0188(10) 0.0228(10) 0.0154(8) 0.0046(7) 0.0000(8) -0.0001(8) C70 0.0212(11) 0.0228(11) 0.0205(9) 0.0053(8) 0.0027(8) 0.0032(8) C71 0.0263(11) 0.0174(11) 0.0272(10) 0.0036(8) 0.0066(9) 0.0024(8) C72 0.0234(10) 0.0183(10) 0.0229(9) -0.0015(8) 0.0031(8) -0.0040(8) C73 0.0234(11) 0.0281(12) 0.0256(10) 0.0077(9) -0.0112(9) -0.0026(9) C74 0.0422(14) 0.0414(14) 0.0246(11) -0.0003(10) -0.0142(11) -0.0080(11) C75 0.0394(15) 0.0433(15) 0.0511(16) 0.0111(12) -0.0272(13) -0.0002(12) C76 0.0227(11) 0.0333(13) 0.0379(12) 0.0051(10) -0.0078(10) -0.0097(10) C77 0.0234(11) 0.0288(12) 0.0294(11) 0.0011(9) 0.0006(9) -0.0102(9) C78 0.0296(12) 0.0260(11) 0.0175(9) 0.0014(8) 0.0015(8) -0.0010(9) C79 0.0368(13) 0.0250(11) 0.0250(10) -0.0070(9) 0.0065(10) -0.0077(9) C80 0.0303(12) 0.0297(12) 0.0266(11) -0.0048(9) -0.0052(10) -0.0108(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 N4 1.8819(16) . ? V1 N3 1.8855(16) . ? V1 O1 1.9687(13) . ? V1 O2 1.9696(13) . ? V1 N2 2.1873(15) . ? V1 N1 2.1988(15) . ? V2 N8 1.8849(16) . ? V2 N7 1.8855(15) . ? V2 O3 1.9660(13) . ? V2 O4 1.9668(13) . ? V2 N6 2.2002(16) . ? V2 N5 2.2197(16) . ? N1 C15 1.295(2) . ? N1 C2 1.438(2) . ? N2 C26 1.300(2) . ? N2 C9 1.443(2) . ? N3 C38 1.457(2) . ? N3 C37 1.460(2) . ? N4 C40 1.450(2) . ? N4 C39 1.464(2) . ? N5 C55 1.291(2) . ? N5 C42 1.445(2) . ? N6 C66 1.285(2) . ? N6 C49 1.444(2) . ? N7 C77 1.459(2) . ? N7 C78 1.460(2) . ? N8 C80 1.452(2) . ? N8 C79 1.463(3) . ? O1 C17 1.331(2) . ? O2 C28 1.321(2) . ? O3 C57 1.323(2) . ? O4 C68 1.320(2) . ? C1 C2 1.404(3) . ? C1 C6 1.411(3) . ? C1 C8 1.506(2) . ? C2 C3 1.396(3) . ? C3 C4 1.385(3) . ? C3 H3 0.9500 . ? C4 C5 1.389(3) . ? C4 H4 0.9500 . ? C5 C6 1.394(3) . ? C5 H5 0.9500 . ? C6 C7 1.507(3) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C13 1.399(2) . ? C8 C9 1.406(2) . ? C9 C10 1.384(3) . ? C10 C11 1.395(3) . ? C10 H10 0.9500 . ? C11 C12 1.387(3) . ? C11 H11 0.9500 . ? C12 C13 1.391(3) . ? C12 H12 0.9500 . ? C13 C14 1.525(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.437(3) . ? C15 H15 0.9500 . ? C16 C21 1.421(2) . ? C16 C17 1.422(3) . ? C17 C18 1.431(3) . ? C18 C19 1.387(3) . ? C18 C22 1.539(3) . ? C19 C20 1.407(3) . ? C19 H19 0.9500 . ? C20 C21 1.367(3) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C25 1.534(3) . ? C22 C24 1.536(3) . ? C22 C23 1.540(3) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.441(3) . ? C26 H26 0.9500 . ? C27 C32 1.411(2) . ? C27 C28 1.423(3) . ? C28 C29 1.443(3) . ? C29 C30 1.395(3) . ? C29 C33 1.534(3) . ? C30 C31 1.395(3) . ? C30 H30 0.9500 . ? C31 C32 1.363(3) . ? C31 H31 0.9500 . ? C32 H32 0.9500 . ? C33 C36 1.532(3) . ? C33 C35 1.540(3) . ? C33 C34 1.544(3) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.401(3) . ? C41 C46 1.407(3) . ? C41 C48 1.509(3) . ? C42 C43 1.384(3) . ? C43 C44 1.382(3) . ? C43 H43 0.9500 . ? C44 C45 1.386(3) . ? C44 H44 0.9500 . ? C45 C46 1.397(3) . ? C45 H45 0.9500 . ? C46 C47 1.508(3) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 C49 1.387(3) . ? C48 C53 1.411(2) . ? C49 C50 1.397(3) . ? C50 C51 1.394(3) . ? C50 H50 0.9500 . ? C51 C52 1.388(3) . ? C51 H51 0.9500 . ? C52 C53 1.397(3) . ? C52 H52 0.9500 . ? C53 C54 1.500(3) . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.442(3) . ? C55 H55 0.9500 . ? C56 C61 1.398(3) . ? C56 C57 1.424(3) . ? C57 C58 1.431(3) . ? C58 C59 1.391(3) . ? C58 C62 1.539(3) . ? C59 C60 1.396(3) . ? C59 H59 0.9500 . ? C60 C61 1.373(3) . ? C60 H60 0.9500 . ? C61 H61 0.9500 . ? C62 C64 1.534(3) . ? C62 C63 1.547(3) . ? C62 C65 1.549(3) . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 C67 1.451(3) . ? C66 H66 0.9500 . ? C67 C72 1.398(3) . ? C67 C68 1.421(3) . ? C68 C69 1.437(3) . ? C69 C70 1.393(3) . ? C69 C73 1.527(3) . ? C70 C71 1.394(3) . ? C70 H70 0.9500 . ? C71 C72 1.370(3) . ? C71 H71 0.9500 . ? C72 H72 0.9500 . ? C73 C75 1.530(3) . ? C73 C74 1.554(3) . ? C73 C76 1.554(3) . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 H75A 0.9800 . ? C75 H75B 0.9800 . ? C75 H75C 0.9800 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 H79A 0.9800 . ? C79 H79B 0.9800 . ? C79 H79C 0.9800 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 V1 N3 98.62(7) . . ? N4 V1 O1 94.84(6) . . ? N3 V1 O1 93.21(6) . . ? N4 V1 O2 91.90(6) . . ? N3 V1 O2 95.28(6) . . ? O1 V1 O2 168.25(6) . . ? N4 V1 N2 169.46(7) . . ? N3 V1 N2 90.23(6) . . ? O1 V1 N2 90.35(6) . . ? O2 V1 N2 81.52(6) . . ? N4 V1 N1 92.30(6) . . ? N3 V1 N1 168.13(6) . . ? O1 V1 N1 81.21(6) . . ? O2 V1 N1 88.93(6) . . ? N2 V1 N1 79.41(6) . . ? N8 V2 N7 98.32(7) . . ? N8 V2 O3 95.69(6) . . ? N7 V2 O3 94.41(6) . . ? N8 V2 O4 92.19(6) . . ? N7 V2 O4 95.50(6) . . ? O3 V2 O4 166.32(5) . . ? N8 V2 N6 170.44(7) . . ? N7 V2 N6 89.62(6) . . ? O3 V2 N6 88.95(6) . . ? O4 V2 N6 81.71(6) . . ? N8 V2 N5 92.80(6) . . ? N7 V2 N5 168.55(6) . . ? O3 V2 N5 81.73(6) . . ? O4 V2 N5 86.74(6) . . ? N6 V2 N5 79.57(6) . . ? C15 N1 C2 116.79(15) . . ? C15 N1 V1 121.21(13) . . ? C2 N1 V1 121.99(11) . . ? C26 N2 C9 115.88(16) . . ? C26 N2 V1 122.81(13) . . ? C9 N2 V1 120.85(11) . . ? C38 N3 C37 111.53(15) . . ? C38 N3 V1 125.10(13) . . ? C37 N3 V1 122.26(12) . . ? C40 N4 C39 110.82(16) . . ? C40 N4 V1 125.50(13) . . ? C39 N4 V1 123.16(13) . . ? C55 N5 C42 117.43(16) . . ? C55 N5 V2 122.35(13) . . ? C42 N5 V2 119.80(12) . . ? C66 N6 C49 116.16(16) . . ? C66 N6 V2 122.70(13) . . ? C49 N6 V2 120.03(12) . . ? C77 N7 C78 110.68(15) . . ? C77 N7 V2 122.69(12) . . ? C78 N7 V2 125.25(13) . . ? C80 N8 C79 111.96(16) . . ? C80 N8 V2 123.26(14) . . ? C79 N8 V2 124.20(14) . . ? C17 O1 V1 126.82(11) . . ? C28 O2 V1 129.54(12) . . ? C57 O3 V2 128.23(12) . . ? C68 O4 V2 129.29(11) . . ? C2 C1 C6 118.63(17) . . ? C2 C1 C8 119.31(16) . . ? C6 C1 C8 122.02(17) . . ? C3 C2 C1 121.56(17) . . ? C3 C2 N1 119.96(17) . . ? C1 C2 N1 118.47(16) . . ? C4 C3 C2 119.07(19) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? C3 C4 C5 120.07(19) . . ? C3 C4 H4 120.0 . . ? C5 C4 H4 120.0 . . ? C4 C5 C6 121.6(2) . . ? C4 C5 H5 119.2 . . ? C6 C5 H5 119.2 . . ? C5 C6 C1 118.92(18) . . ? C5 C6 C7 118.86(19) . . ? C1 C6 C7 122.22(18) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C13 C8 C9 118.67(16) . . ? C13 C8 C1 121.11(16) . . ? C9 C8 C1 120.17(15) . . ? C10 C9 C8 121.79(16) . . ? C10 C9 N2 121.00(16) . . ? C8 C9 N2 117.18(16) . . ? C9 C10 C11 118.78(18) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? C12 C11 C10 120.08(18) . . ? C12 C11 H11 120.0 . . ? C10 C11 H11 120.0 . . ? C11 C12 C13 121.24(17) . . ? C11 C12 H12 119.4 . . ? C13 C12 H12 119.4 . . ? C12 C13 C8 119.38(17) . . ? C12 C13 C14 119.08(17) . . ? C8 C13 C14 121.46(17) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N1 C15 C16 125.73(17) . . ? N1 C15 H15 117.1 . . ? C16 C15 H15 117.1 . . ? C21 C16 C17 120.28(17) . . ? C21 C16 C15 117.55(17) . . ? C17 C16 C15 121.48(16) . . ? O1 C17 C16 119.97(17) . . ? O1 C17 C18 121.15(16) . . ? C16 C17 C18 118.85(16) . . ? C19 C18 C17 117.88(17) . . ? C19 C18 C22 121.04(17) . . ? C17 C18 C22 121.07(16) . . ? C18 C19 C20 123.44(19) . . ? C18 C19 H19 118.3 . . ? C20 C19 H19 118.3 . . ? C21 C20 C19 118.82(18) . . ? C21 C20 H20 120.6 . . ? C19 C20 H20 120.6 . . ? C20 C21 C16 120.51(18) . . ? C20 C21 H21 119.7 . . ? C16 C21 H21 119.7 . . ? C25 C22 C24 107.14(18) . . ? C25 C22 C18 112.59(16) . . ? C24 C22 C18 110.27(16) . . ? C25 C22 C23 107.46(17) . . ? C24 C22 C23 110.40(17) . . ? C18 C22 C23 108.94(17) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N2 C26 C27 126.03(18) . . ? N2 C26 H26 117.0 . . ? C27 C26 H26 117.0 . . ? C32 C27 C28 120.20(17) . . ? C32 C27 C26 117.89(17) . . ? C28 C27 C26 120.97(16) . . ? O2 C28 C27 120.71(16) . . ? O2 C28 C29 120.32(17) . . ? C27 C28 C29 118.94(17) . . ? C30 C29 C28 116.91(18) . . ? C30 C29 C33 121.85(18) . . ? C28 C29 C33 121.24(17) . . ? C31 C30 C29 124.10(19) . . ? C31 C30 H30 118.0 . . ? C29 C30 H30 118.0 . . ? C32 C31 C30 118.62(19) . . ? C32 C31 H31 120.7 . . ? C30 C31 H31 120.7 . . ? C31 C32 C27 121.19(18) . . ? C31 C32 H32 119.4 . . ? C27 C32 H32 119.4 . . ? C36 C33 C29 111.94(17) . . ? C36 C33 C35 106.84(18) . . ? C29 C33 C35 110.50(18) . . ? C36 C33 C34 107.51(18) . . ? C29 C33 C34 110.35(16) . . ? C35 C33 C34 109.57(18) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C33 C35 H35A 109.5 . . ? C33 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C33 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C33 C36 H36A 109.5 . . ? C33 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C33 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? N3 C37 H37A 109.5 . . ? N3 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? N3 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N3 C38 H38A 109.5 . . ? N3 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? N3 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N4 C39 H39A 109.5 . . ? N4 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? N4 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? N4 C40 H40A 109.5 . . ? N4 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? N4 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C46 119.06(17) . . ? C42 C41 C48 118.89(17) . . ? C46 C41 C48 122.04(17) . . ? C43 C42 C41 121.05(19) . . ? C43 C42 N5 121.24(18) . . ? C41 C42 N5 117.60(16) . . ? C44 C43 C42 119.3(2) . . ? C44 C43 H43 120.4 . . ? C42 C43 H43 120.4 . . ? C43 C44 C45 120.7(2) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C44 C45 C46 120.6(2) . . ? C44 C45 H45 119.7 . . ? C46 C45 H45 119.7 . . ? C45 C46 C41 118.97(19) . . ? C45 C46 C47 119.9(2) . . ? C41 C46 C47 120.99(18) . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C49 C48 C53 119.97(17) . . ? C49 C48 C41 119.70(16) . . ? C53 C48 C41 120.22(16) . . ? C48 C49 C50 121.65(17) . . ? C48 C49 N6 116.60(16) . . ? C50 C49 N6 121.67(17) . . ? C51 C50 C49 118.43(18) . . ? C51 C50 H50 120.8 . . ? C49 C50 H50 120.8 . . ? C52 C51 C50 120.24(18) . . ? C52 C51 H51 119.9 . . ? C50 C51 H51 119.9 . . ? C51 C52 C53 121.80(17) . . ? C51 C52 H52 119.1 . . ? C53 C52 H52 119.1 . . ? C52 C53 C48 117.87(18) . . ? C52 C53 C54 120.30(17) . . ? C48 C53 C54 121.73(18) . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N5 C55 C56 125.88(18) . . ? N5 C55 H55 117.1 . . ? C56 C55 H55 117.1 . . ? C61 C56 C57 120.66(19) . . ? C61 C56 C55 117.09(18) . . ? C57 C56 C55 121.65(17) . . ? O3 C57 C56 120.63(17) . . ? O3 C57 C58 120.79(17) . . ? C56 C57 C58 118.52(17) . . ? C59 C58 C57 117.54(19) . . ? C59 C58 C62 121.10(19) . . ? C57 C58 C62 121.31(17) . . ? C58 C59 C60 123.8(2) . . ? C58 C59 H59 118.1 . . ? C60 C59 H59 118.1 . . ? C61 C60 C59 118.32(19) . . ? C61 C60 H60 120.8 . . ? C59 C60 H60 120.8 . . ? C60 C61 C56 121.00(19) . . ? C60 C61 H61 119.5 . . ? C56 C61 H61 119.5 . . ? C64 C62 C58 111.32(17) . . ? C64 C62 C63 106.81(19) . . ? C58 C62 C63 112.58(18) . . ? C64 C62 C65 110.07(19) . . ? C58 C62 C65 108.37(17) . . ? C63 C62 C65 107.63(19) . . ? C62 C63 H63A 109.5 . . ? C62 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C62 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C62 C64 H64A 109.5 . . ? C62 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C62 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? C62 C65 H65A 109.5 . . ? C62 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C62 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? N6 C66 C67 126.36(18) . . ? N6 C66 H66 116.8 . . ? C67 C66 H66 116.8 . . ? C72 C67 C68 120.85(17) . . ? C72 C67 C66 117.75(17) . . ? C68 C67 C66 120.58(17) . . ? O4 C68 C67 121.29(16) . . ? O4 C68 C69 120.07(16) . . ? C67 C68 C69 118.61(17) . . ? C70 C69 C68 117.08(18) . . ? C70 C69 C73 121.45(18) . . ? C68 C69 C73 121.47(18) . . ? C69 C70 C71 124.05(19) . . ? C69 C70 H70 118.0 . . ? C71 C70 H70 118.0 . . ? C72 C71 C70 118.41(19) . . ? C72 C71 H71 120.8 . . ? C70 C71 H71 120.8 . . ? C71 C72 C67 120.89(19) . . ? C71 C72 H72 119.6 . . ? C67 C72 H72 119.6 . . ? C69 C73 C75 113.00(18) . . ? C69 C73 C74 110.73(18) . . ? C75 C73 C74 107.43(18) . . ? C69 C73 C76 110.12(16) . . ? C75 C73 C76 106.21(18) . . ? C74 C73 C76 109.19(19) . . ? C73 C74 H74A 109.5 . . ? C73 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C73 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C73 C75 H75A 109.5 . . ? C73 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C73 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C73 C76 H76A 109.5 . . ? C73 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C73 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? N7 C77 H77A 109.5 . . ? N7 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? N7 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? N7 C78 H78A 109.5 . . ? N7 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? N7 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? N8 C79 H79A 109.5 . . ? N8 C79 H79B 109.5 . . ? H79A C79 H79B 109.5 . . ? N8 C79 H79C 109.5 . . ? H79A C79 H79C 109.5 . . ? H79B C79 H79C 109.5 . . ? N8 C80 H80A 109.5 . . ? N8 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? N8 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 V1 N1 C15 -58.75(15) . . . . ? N3 V1 N1 C15 98.3(3) . . . . ? O1 V1 N1 C15 35.79(14) . . . . ? O2 V1 N1 C15 -150.61(14) . . . . ? N2 V1 N1 C15 127.81(15) . . . . ? N4 V1 N1 C2 122.74(14) . . . . ? N3 V1 N1 C2 -80.2(4) . . . . ? O1 V1 N1 C2 -142.72(14) . . . . ? O2 V1 N1 C2 30.88(13) . . . . ? N2 V1 N1 C2 -50.70(13) . . . . ? N4 V1 N2 C26 83.2(4) . . . . ? N3 V1 N2 C26 -64.05(15) . . . . ? O1 V1 N2 C26 -157.26(15) . . . . ? O2 V1 N2 C26 31.26(15) . . . . ? N1 V1 N2 C26 121.76(16) . . . . ? N4 V1 N2 C9 -88.7(4) . . . . ? N3 V1 N2 C9 124.06(14) . . . . ? O1 V1 N2 C9 30.85(13) . . . . ? O2 V1 N2 C9 -140.63(14) . . . . ? N1 V1 N2 C9 -50.14(13) . . . . ? N4 V1 N3 C38 -49.93(17) . . . . ? O1 V1 N3 C38 -145.32(16) . . . . ? O2 V1 N3 C38 42.81(16) . . . . ? N2 V1 N3 C38 124.32(16) . . . . ? N1 V1 N3 C38 153.2(3) . . . . ? N4 V1 N3 C37 143.16(15) . . . . ? O1 V1 N3 C37 47.77(15) . . . . ? O2 V1 N3 C37 -124.11(15) . . . . ? N2 V1 N3 C37 -42.60(15) . . . . ? N1 V1 N3 C37 -13.7(4) . . . . ? N3 V1 N4 C40 -44.10(16) . . . . ? O1 V1 N4 C40 49.89(16) . . . . ? O2 V1 N4 C40 -139.73(15) . . . . ? N2 V1 N4 C40 169.1(3) . . . . ? N1 V1 N4 C40 131.26(16) . . . . ? N3 V1 N4 C39 144.94(15) . . . . ? O1 V1 N4 C39 -121.06(15) . . . . ? O2 V1 N4 C39 49.31(15) . . . . ? N2 V1 N4 C39 -1.8(4) . . . . ? N1 V1 N4 C39 -39.70(15) . . . . ? N8 V2 N5 C55 -65.90(15) . . . . ? N7 V2 N5 C55 100.4(4) . . . . ? O3 V2 N5 C55 29.45(14) . . . . ? O4 V2 N5 C55 -157.94(15) . . . . ? N6 V2 N5 C55 119.90(15) . . . . ? N8 V2 N5 C42 121.74(13) . . . . ? N7 V2 N5 C42 -72.0(4) . . . . ? O3 V2 N5 C42 -142.92(13) . . . . ? O4 V2 N5 C42 29.70(13) . . . . ? N6 V2 N5 C42 -52.46(13) . . . . ? N8 V2 N6 C66 81.4(4) . . . . ? N7 V2 N6 C66 -64.93(15) . . . . ? O3 V2 N6 C66 -159.34(15) . . . . ? O4 V2 N6 C66 30.69(15) . . . . ? N5 V2 N6 C66 118.88(16) . . . . ? N8 V2 N6 C49 -86.0(4) . . . . ? N7 V2 N6 C49 127.60(14) . . . . ? O3 V2 N6 C49 33.18(13) . . . . ? O4 V2 N6 C49 -136.79(14) . . . . ? N5 V2 N6 C49 -48.60(13) . . . . ? N8 V2 N7 C77 143.00(16) . . . . ? O3 V2 N7 C77 46.59(16) . . . . ? O4 V2 N7 C77 -123.96(16) . . . . ? N6 V2 N7 C77 -42.33(16) . . . . ? N5 V2 N7 C77 -23.1(4) . . . . ? N8 V2 N7 C78 -51.64(16) . . . . ? O3 V2 N7 C78 -148.06(15) . . . . ? O4 V2 N7 C78 41.39(16) . . . . ? N6 V2 N7 C78 123.02(16) . . . . ? N5 V2 N7 C78 142.2(3) . . . . ? N7 V2 N8 C80 146.98(16) . . . . ? O3 V2 N8 C80 -117.70(15) . . . . ? O4 V2 N8 C80 51.10(16) . . . . ? N6 V2 N8 C80 1.0(5) . . . . ? N5 V2 N8 C80 -35.75(16) . . . . ? N7 V2 N8 C79 -42.45(17) . . . . ? O3 V2 N8 C79 52.87(16) . . . . ? O4 V2 N8 C79 -138.33(16) . . . . ? N6 V2 N8 C79 171.6(3) . . . . ? N5 V2 N8 C79 134.83(16) . . . . ? N4 V1 O1 C17 40.51(15) . . . . ? N3 V1 O1 C17 139.45(15) . . . . ? O2 V1 O1 C17 -84.3(3) . . . . ? N2 V1 O1 C17 -130.30(15) . . . . ? N1 V1 O1 C17 -51.08(15) . . . . ? N4 V1 O2 C28 142.47(15) . . . . ? N3 V1 O2 C28 43.63(16) . . . . ? O1 V1 O2 C28 -92.5(3) . . . . ? N2 V1 O2 C28 -45.81(15) . . . . ? N1 V1 O2 C28 -125.26(15) . . . . ? N8 V2 O3 C57 44.41(15) . . . . ? N7 V2 O3 C57 143.25(15) . . . . ? O4 V2 O3 C57 -80.4(3) . . . . ? N6 V2 O3 C57 -127.21(15) . . . . ? N5 V2 O3 C57 -47.60(15) . . . . ? N8 V2 O4 C68 142.10(15) . . . . ? N7 V2 O4 C68 43.52(15) . . . . ? O3 V2 O4 C68 -92.7(3) . . . . ? N6 V2 O4 C68 -45.29(14) . . . . ? N5 V2 O4 C68 -125.22(15) . . . . ? C6 C1 C2 C3 4.9(3) . . . . ? C8 C1 C2 C3 -172.81(16) . . . . ? C6 C1 C2 N1 -174.33(16) . . . . ? C8 C1 C2 N1 7.9(2) . . . . ? C15 N1 C2 C3 82.3(2) . . . . ? V1 N1 C2 C3 -99.12(18) . . . . ? C15 N1 C2 C1 -98.4(2) . . . . ? V1 N1 C2 C1 80.15(18) . . . . ? C1 C2 C3 C4 -1.6(3) . . . . ? N1 C2 C3 C4 177.65(17) . . . . ? C2 C3 C4 C5 -1.9(3) . . . . ? C3 C4 C5 C6 2.1(3) . . . . ? C4 C5 C6 C1 1.3(3) . . . . ? C4 C5 C6 C7 -177.95(19) . . . . ? C2 C1 C6 C5 -4.7(3) . . . . ? C8 C1 C6 C5 172.96(17) . . . . ? C2 C1 C6 C7 174.54(17) . . . . ? C8 C1 C6 C7 -7.8(3) . . . . ? C2 C1 C8 C13 112.4(2) . . . . ? C6 C1 C8 C13 -65.3(2) . . . . ? C2 C1 C8 C9 -64.9(2) . . . . ? C6 C1 C8 C9 117.4(2) . . . . ? C13 C8 C9 C10 1.7(3) . . . . ? C1 C8 C9 C10 179.16(18) . . . . ? C13 C8 C9 N2 -176.39(16) . . . . ? C1 C8 C9 N2 1.0(2) . . . . ? C26 N2 C9 C10 94.7(2) . . . . ? V1 N2 C9 C10 -92.83(18) . . . . ? C26 N2 C9 C8 -87.1(2) . . . . ? V1 N2 C9 C8 85.32(18) . . . . ? C8 C9 C10 C11 0.1(3) . . . . ? N2 C9 C10 C11 178.20(17) . . . . ? C9 C10 C11 C12 -1.0(3) . . . . ? C10 C11 C12 C13 -0.1(3) . . . . ? C11 C12 C13 C8 2.0(3) . . . . ? C11 C12 C13 C14 -174.96(19) . . . . ? C9 C8 C13 C12 -2.8(3) . . . . ? C1 C8 C13 C12 179.82(17) . . . . ? C9 C8 C13 C14 174.12(17) . . . . ? C1 C8 C13 C14 -3.3(3) . . . . ? C2 N1 C15 C16 169.21(17) . . . . ? V1 N1 C15 C16 -9.4(3) . . . . ? N1 C15 C16 C21 166.26(18) . . . . ? N1 C15 C16 C17 -23.2(3) . . . . ? V1 O1 C17 C16 37.1(2) . . . . ? V1 O1 C17 C18 -144.99(14) . . . . ? C21 C16 C17 O1 -178.32(17) . . . . ? C15 C16 C17 O1 11.4(3) . . . . ? C21 C16 C17 C18 3.8(3) . . . . ? C15 C16 C17 C18 -166.48(17) . . . . ? O1 C17 C18 C19 177.37(17) . . . . ? C16 C17 C18 C19 -4.7(3) . . . . ? O1 C17 C18 C22 -3.4(3) . . . . ? C16 C17 C18 C22 174.46(17) . . . . ? C17 C18 C19 C20 1.9(3) . . . . ? C22 C18 C19 C20 -177.35(19) . . . . ? C18 C19 C20 C21 2.2(3) . . . . ? C19 C20 C21 C16 -3.3(3) . . . . ? C17 C16 C21 C20 0.3(3) . . . . ? C15 C16 C21 C20 170.93(18) . . . . ? C19 C18 C22 C25 0.9(3) . . . . ? C17 C18 C22 C25 -178.25(18) . . . . ? C19 C18 C22 C24 -118.7(2) . . . . ? C17 C18 C22 C24 62.1(2) . . . . ? C19 C18 C22 C23 120.0(2) . . . . ? C17 C18 C22 C23 -59.2(2) . . . . ? C9 N2 C26 C27 164.67(17) . . . . ? V1 N2 C26 C27 -7.6(3) . . . . ? N2 C26 C27 C32 169.57(18) . . . . ? N2 C26 C27 C28 -21.5(3) . . . . ? V1 O2 C28 C27 33.4(2) . . . . ? V1 O2 C28 C29 -148.86(14) . . . . ? C32 C27 C28 O2 179.45(17) . . . . ? C26 C27 C28 O2 10.8(3) . . . . ? C32 C27 C28 C29 1.6(3) . . . . ? C26 C27 C28 C29 -167.03(18) . . . . ? O2 C28 C29 C30 -179.96(17) . . . . ? C27 C28 C29 C30 -2.1(3) . . . . ? O2 C28 C29 C33 0.2(3) . . . . ? C27 C28 C29 C33 177.98(17) . . . . ? C28 C29 C30 C31 0.5(3) . . . . ? C33 C29 C30 C31 -179.6(2) . . . . ? C29 C30 C31 C32 1.7(3) . . . . ? C30 C31 C32 C27 -2.2(3) . . . . ? C28 C27 C32 C31 0.6(3) . . . . ? C26 C27 C32 C31 169.62(18) . . . . ? C30 C29 C33 C36 -0.4(3) . . . . ? C28 C29 C33 C36 179.46(19) . . . . ? C30 C29 C33 C35 -119.4(2) . . . . ? C28 C29 C33 C35 60.5(2) . . . . ? C30 C29 C33 C34 119.3(2) . . . . ? C28 C29 C33 C34 -60.8(2) . . . . ? C46 C41 C42 C43 7.2(3) . . . . ? C48 C41 C42 C43 -173.28(17) . . . . ? C46 C41 C42 N5 -168.99(16) . . . . ? C48 C41 C42 N5 10.6(2) . . . . ? C55 N5 C42 C43 90.8(2) . . . . ? V2 N5 C42 C43 -96.46(19) . . . . ? C55 N5 C42 C41 -93.0(2) . . . . ? V2 N5 C42 C41 79.69(18) . . . . ? C41 C42 C43 C44 -4.0(3) . . . . ? N5 C42 C43 C44 172.01(18) . . . . ? C42 C43 C44 C45 -0.9(3) . . . . ? C43 C44 C45 C46 2.6(3) . . . . ? C44 C45 C46 C41 0.6(3) . . . . ? C44 C45 C46 C47 -175.7(2) . . . . ? C42 C41 C46 C45 -5.4(3) . . . . ? C48 C41 C46 C45 175.08(18) . . . . ? C42 C41 C46 C47 170.89(18) . . . . ? C48 C41 C46 C47 -8.6(3) . . . . ? C42 C41 C48 C49 -68.3(2) . . . . ? C46 C41 C48 C49 111.2(2) . . . . ? C42 C41 C48 C53 108.1(2) . . . . ? C46 C41 C48 C53 -72.4(3) . . . . ? C53 C48 C49 C50 0.7(3) . . . . ? C41 C48 C49 C50 177.06(18) . . . . ? C53 C48 C49 N6 -176.17(17) . . . . ? C41 C48 C49 N6 0.2(3) . . . . ? C66 N6 C49 C48 -82.4(2) . . . . ? V2 N6 C49 C48 85.85(19) . . . . ? C66 N6 C49 C50 100.8(2) . . . . ? V2 N6 C49 C50 -90.97(19) . . . . ? C48 C49 C50 C51 1.1(3) . . . . ? N6 C49 C50 C51 177.73(17) . . . . ? C49 C50 C51 C52 -1.3(3) . . . . ? C50 C51 C52 C53 -0.1(3) . . . . ? C51 C52 C53 C48 1.8(3) . . . . ? C51 C52 C53 C54 -174.5(2) . . . . ? C49 C48 C53 C52 -2.1(3) . . . . ? C41 C48 C53 C52 -178.46(17) . . . . ? C49 C48 C53 C54 174.25(18) . . . . ? C41 C48 C53 C54 -2.1(3) . . . . ? C42 N5 C55 C56 168.65(17) . . . . ? V2 N5 C55 C56 -3.9(3) . . . . ? N5 C55 C56 C61 165.90(18) . . . . ? N5 C55 C56 C57 -23.0(3) . . . . ? V2 O3 C57 C56 37.8(2) . . . . ? V2 O3 C57 C58 -145.13(14) . . . . ? C61 C56 C57 O3 178.84(17) . . . . ? C55 C56 C57 O3 8.0(3) . . . . ? C61 C56 C57 C58 1.7(3) . . . . ? C55 C56 C57 C58 -169.11(17) . . . . ? O3 C57 C58 C59 178.59(18) . . . . ? C56 C57 C58 C59 -4.3(3) . . . . ? O3 C57 C58 C62 -4.0(3) . . . . ? C56 C57 C58 C62 173.19(17) . . . . ? C57 C58 C59 C60 3.2(3) . . . . ? C62 C58 C59 C60 -174.3(2) . . . . ? C58 C59 C60 C61 0.7(3) . . . . ? C59 C60 C61 C56 -3.5(3) . . . . ? C57 C56 C61 C60 2.3(3) . . . . ? C55 C56 C61 C60 173.51(18) . . . . ? C59 C58 C62 C64 -123.6(2) . . . . ? C57 C58 C62 C64 59.1(3) . . . . ? C59 C58 C62 C63 -3.7(3) . . . . ? C57 C58 C62 C63 178.97(19) . . . . ? C59 C58 C62 C65 115.3(2) . . . . ? C57 C58 C62 C65 -62.1(2) . . . . ? C49 N6 C66 C67 161.01(17) . . . . ? V2 N6 C66 C67 -6.9(3) . . . . ? N6 C66 C67 C72 168.73(19) . . . . ? N6 C66 C67 C68 -21.6(3) . . . . ? V2 O4 C68 C67 33.3(2) . . . . ? V2 O4 C68 C69 -148.87(13) . . . . ? C72 C67 C68 O4 179.87(17) . . . . ? C66 C67 C68 O4 10.5(3) . . . . ? C72 C67 C68 C69 2.0(3) . . . . ? C66 C67 C68 C69 -167.41(17) . . . . ? O4 C68 C69 C70 178.86(17) . . . . ? C67 C68 C69 C70 -3.2(3) . . . . ? O4 C68 C69 C73 -1.4(3) . . . . ? C67 C68 C69 C73 176.56(17) . . . . ? C68 C69 C70 C71 1.5(3) . . . . ? C73 C69 C70 C71 -178.24(19) . . . . ? C69 C70 C71 C72 1.6(3) . . . . ? C70 C71 C72 C67 -2.9(3) . . . . ? C68 C67 C72 C71 1.2(3) . . . . ? C66 C67 C72 C71 170.87(18) . . . . ? C70 C69 C73 C75 1.3(3) . . . . ? C68 C69 C73 C75 -178.47(18) . . . . ? C70 C69 C73 C74 -119.3(2) . . . . ? C68 C69 C73 C74 61.0(2) . . . . ? C70 C69 C73 C76 119.9(2) . . . . ? C68 C69 C73 C76 -59.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.890 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.320 _refine_diff_density_min -0.405 _refine_diff_density_rms 0.056 # Attachment '- compound 24.cif' data_compound24 _database_code_depnum_ccdc_archive 'CCDC 791869' #TrackingRef '- compound 24.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C48 H66 N4 O2 V' _chemical_formula_sum 'C48 H66 N4 O2 V' _chemical_formula_weight 781.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.3005 0.5294 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.433(4) _cell_length_b 15.427(5) _cell_length_c 15.628(5) _cell_angle_alpha 98.603(6) _cell_angle_beta 112.406(6) _cell_angle_gamma 94.668(6) _cell_volume 2708.5(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2060 _cell_measurement_theta_min 2.30 _cell_measurement_theta_max 22.50 _exptl_crystal_description block _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.959 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 842 _exptl_absorpt_coefficient_mu 0.217 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9538 _exptl_absorpt_correction_T_max 0.9620 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 15957 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.1159 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 27.56 _reflns_number_total 15957 _reflns_number_gt 9327 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The structure is a non-merohedral twin. PLATON (Spek, 2003) was used to de-twin the structure. The twin component refined to 20%.The twinning crystal was used for data collection. The t-butyl groups are disordered in two positions. The C-C distances were restrained in 1.54%A, and the thermal parameters of disordered atoms were restrained. The disorders solvents were removed by SQEEZE programm. ; _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^)+(0.1422P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15957 _refine_ls_number_parameters 577 _refine_ls_number_restraints 117 _refine_ls_R_factor_all 0.1230 _refine_ls_R_factor_gt 0.0831 _refine_ls_wR_factor_ref 0.2451 _refine_ls_wR_factor_gt 0.2190 _refine_ls_goodness_of_fit_ref 0.954 _refine_ls_restrained_S_all 0.960 _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 C1 C 1.0317(3) 0.6897(2) 0.8772(2) 0.0313(8) Uani 1 1 d . . . C2 C 1.1074(3) 0.6283(2) 0.8746(3) 0.0385(9) Uani 1 1 d . . . H2 H 1.1345 0.6194 0.8252 0.046 Uiso 1 1 calc R . . C3 C 1.1421(4) 0.5801(2) 0.9473(3) 0.0467(11) Uani 1 1 d . . . H3 H 1.1941 0.5381 0.9475 0.056 Uiso 1 1 calc R . . C4 C 1.1030(4) 0.5923(3) 1.0172(3) 0.0467(11) Uani 1 1 d . . . H4 H 1.1263 0.5578 1.0649 0.056 Uiso 1 1 calc R . . C5 C 1.0283(3) 0.6551(2) 1.0207(2) 0.0399(9) Uani 1 1 d . . . C6 C 0.9860(4) 0.6646(3) 1.0992(3) 0.0543(12) Uani 1 1 d . . . H6A H 1.0481 0.7002 1.1568 0.081 Uiso 1 1 calc R . . H6B H 0.9665 0.6057 1.1106 0.081 Uiso 1 1 calc R . . H6C H 0.9159 0.6939 1.0815 0.081 Uiso 1 1 calc R . . C7 C 0.9951(3) 0.7066(2) 0.9505(2) 0.0319(8) Uani 1 1 d . . . C8 C 0.9156(3) 0.7751(2) 0.9503(2) 0.0346(8) Uani 1 1 d . . . C9 C 0.9535(4) 0.8547(2) 1.0166(3) 0.0430(10) Uani 1 1 d . . . C10 C 1.0787(4) 0.8780(3) 1.0888(3) 0.0626(13) Uani 1 1 d . . . H10A H 1.0977 0.9424 1.1114 0.094 Uiso 1 1 calc R . . H10B H 1.1321 0.8581 1.0600 0.094 Uiso 1 1 calc R . . H10C H 1.0875 0.8487 1.1421 0.094 Uiso 1 1 calc R . . C11 C 0.8745(4) 0.9144(3) 1.0138(3) 0.0505(11) Uani 1 1 d . . . H11 H 0.9001 0.9689 1.0582 0.061 Uiso 1 1 calc R . . C12 C 0.7603(4) 0.8961(3) 0.9479(3) 0.0495(11) Uani 1 1 d . . . H12 H 0.7069 0.9365 0.9493 0.059 Uiso 1 1 calc R . . C13 C 0.7224(4) 0.8186(2) 0.8791(3) 0.0416(9) Uani 1 1 d . . . H13 H 0.6442 0.8064 0.8323 0.050 Uiso 1 1 calc R . . C14 C 0.8008(3) 0.7600(2) 0.8806(2) 0.0298(8) Uani 1 1 d . . . C15 C 0.7294(3) 0.6100(2) 0.8218(2) 0.0298(8) Uani 1 1 d . . . H15 H 0.7070 0.6139 0.8738 0.036 Uiso 1 1 calc R . . C16 C 0.7161(3) 0.5229(2) 0.7675(2) 0.0250(7) Uani 1 1 d . A . C17 C 0.6506(3) 0.4535(2) 0.7851(2) 0.0292(8) Uani 1 1 d . . . H17 H 0.6105 0.4675 0.8251 0.035 Uiso 1 1 calc R . . C18 C 0.6437(3) 0.3660(2) 0.7455(2) 0.0302(8) Uani 1 1 d . A . C19 C 0.5708(3) 0.2901(2) 0.7617(2) 0.0374(9) Uani 1 1 d D . . C20 C 0.5137(7) 0.3239(4) 0.8296(5) 0.056(2) Uani 0.639(8) 1 d PDU A 1 H20A H 0.5741 0.3605 0.8875 0.084 Uiso 0.639(8) 1 calc PR A 1 H20B H 0.4772 0.2733 0.8453 0.084 Uiso 0.639(8) 1 calc PR A 1 H20C H 0.4536 0.3595 0.7993 0.084 Uiso 0.639(8) 1 calc PR A 1 C21 C 0.6583(5) 0.2281(4) 0.8104(5) 0.053(2) Uani 0.639(8) 1 d PDU A 1 H21A H 0.6141 0.1737 0.8130 0.079 Uiso 0.639(8) 1 calc PR A 1 H21B H 0.7101 0.2587 0.8747 0.079 Uiso 0.639(8) 1 calc PR A 1 H21C H 0.7058 0.2130 0.7742 0.079 Uiso 0.639(8) 1 calc PR A 1 C22 C 0.4806(6) 0.2398(5) 0.6695(4) 0.057(2) Uani 0.639(8) 1 d PDU A 1 H22A H 0.5138 0.2362 0.6216 0.085 Uiso 0.639(8) 1 calc PR A 1 H22B H 0.4117 0.2704 0.6501 0.085 Uiso 0.639(8) 1 calc PR A 1 H22C H 0.4571 0.1799 0.6762 0.085 Uiso 0.639(8) 1 calc PR A 1 C20' C 0.5781(10) 0.3030(7) 0.8616(5) 0.040(3) Uani 0.361(8) 1 d PDU A 2 H20D H 0.5437 0.3557 0.8746 0.060 Uiso 0.361(8) 1 calc PR A 2 H20E H 0.6607 0.3108 0.9058 0.060 Uiso 0.361(8) 1 calc PR A 2 H20F H 0.5347 0.2508 0.8693 0.060 Uiso 0.361(8) 1 calc PR A 2 C21' C 0.5969(11) 0.1961(5) 0.7331(8) 0.053(4) Uani 0.361(8) 1 d PDU A 2 H21D H 0.5794 0.1839 0.6654 0.079 Uiso 0.361(8) 1 calc PR A 2 H21E H 0.5478 0.1520 0.7471 0.079 Uiso 0.361(8) 1 calc PR A 2 H21F H 0.6802 0.1929 0.7688 0.079 Uiso 0.361(8) 1 calc PR A 2 C22' C 0.4392(7) 0.2908(7) 0.6939(7) 0.046(3) Uani 0.361(8) 1 d PDU A 2 H22D H 0.3905 0.2360 0.6903 0.069 Uiso 0.361(8) 1 calc PR A 2 H22E H 0.4350 0.2949 0.6308 0.069 Uiso 0.361(8) 1 calc PR A 2 H22F H 0.4102 0.3419 0.7185 0.069 Uiso 0.361(8) 1 calc PR A 2 C23 C 0.7081(3) 0.3494(2) 0.6899(2) 0.0329(8) Uani 1 1 d . . . H23 H 0.7046 0.2895 0.6621 0.039 Uiso 1 1 calc R A . C24 C 0.7770(3) 0.4149(2) 0.6725(2) 0.0259(7) Uani 1 1 d . A . C25 C 0.8463(3) 0.3889(2) 0.6114(2) 0.0337(8) Uani 1 1 d . . . C26 C 0.9791(3) 0.4187(2) 0.6704(3) 0.0398(9) Uani 1 1 d . A . H26A H 1.0220 0.4095 0.6294 0.060 Uiso 1 1 calc R . . H26B H 1.0065 0.3838 0.7200 0.060 Uiso 1 1 calc R . . H26C H 0.9931 0.4817 0.6993 0.060 Uiso 1 1 calc R . . C27 C 0.8279(4) 0.2883(2) 0.5750(3) 0.0479(11) Uani 1 1 d . A . H27A H 0.8713 0.2756 0.5348 0.072 Uiso 1 1 calc R . . H27B H 0.7439 0.2668 0.5383 0.072 Uiso 1 1 calc R . . H27C H 0.8570 0.2583 0.6286 0.072 Uiso 1 1 calc R . . C28 C 0.8075(4) 0.4318(3) 0.5242(3) 0.0406(9) Uani 1 1 d . A . H28A H 0.8474 0.4103 0.4837 0.061 Uiso 1 1 calc R . . H28B H 0.8282 0.4964 0.5441 0.061 Uiso 1 1 calc R . . H28C H 0.7222 0.4161 0.4891 0.061 Uiso 1 1 calc R . . C29 C 0.7792(3) 0.5047(2) 0.7106(2) 0.0244(7) Uani 1 1 d . . . C30 C 0.8858(3) 0.8820(2) 0.7093(2) 0.0291(8) Uani 1 1 d . . . C31 C 0.8523(3) 0.9586(2) 0.6715(2) 0.0314(8) Uani 1 1 d . . . C32 C 0.7213(3) 0.9703(2) 0.6267(3) 0.0425(10) Uani 1 1 d . . . C33 C 0.6682(4) 0.9718(3) 0.7003(3) 0.0476(10) Uani 1 1 d . . . H33A H 0.6733 0.9155 0.7226 0.071 Uiso 1 1 calc R . . H33B H 0.5855 0.9800 0.6719 0.071 Uiso 1 1 calc R . . H33C H 0.7117 1.0208 0.7537 0.071 Uiso 1 1 calc R . . C34 C 0.6522(4) 0.8963(3) 0.5421(3) 0.0497(11) Uani 1 1 d . . . H34A H 0.6800 0.9007 0.4919 0.074 Uiso 1 1 calc R . . H34B H 0.5684 0.9016 0.5192 0.074 Uiso 1 1 calc R . . H34C H 0.6638 0.8387 0.5609 0.074 Uiso 1 1 calc R . . C35 C 0.7053(4) 1.0598(3) 0.5916(4) 0.0634(14) Uani 1 1 d . . . H35A H 0.7452 1.1093 0.6452 0.095 Uiso 1 1 calc R . . H35B H 0.6212 1.0641 0.5629 0.095 Uiso 1 1 calc R . . H35C H 0.7394 1.0623 0.5448 0.095 Uiso 1 1 calc R . . C36 C 0.9412(3) 1.0228(2) 0.6754(3) 0.0382(9) Uani 1 1 d . . . H36 H 0.9177 1.0727 0.6480 0.046 Uiso 1 1 calc R . . C37 C 1.0612(3) 1.0194(2) 0.7163(3) 0.0380(9) Uani 1 1 d D B . C38 C 1.1522(3) 1.0902(2) 0.7135(3) 0.0506(11) Uani 1 1 d D . . C39 C 1.0938(7) 1.1716(5) 0.6815(9) 0.056(4) Uani 0.430(10) 1 d PDU B 1 H39A H 1.0495 1.1584 0.6129 0.084 Uiso 0.430(10) 1 calc PR B 1 H39B H 1.1549 1.2231 0.6989 0.084 Uiso 0.430(10) 1 calc PR B 1 H39C H 1.0402 1.1848 0.7126 0.084 Uiso 0.430(10) 1 calc PR B 1 C40 C 1.2555(8) 1.1190(7) 0.8070(5) 0.067(4) Uani 0.430(10) 1 d PDU B 1 H40A H 1.2763 1.0672 0.8359 0.101 Uiso 0.430(10) 1 calc PR B 1 H40B H 1.2347 1.1620 0.8487 0.101 Uiso 0.430(10) 1 calc PR B 1 H40C H 1.3228 1.1464 0.7972 0.101 Uiso 0.430(10) 1 calc PR B 1 C41 C 1.1930(9) 1.0501(6) 0.6357(7) 0.057(3) Uani 0.430(10) 1 d PDU B 1 H41A H 1.2305 0.9982 0.6527 0.086 Uiso 0.430(10) 1 calc PR B 1 H41B H 1.2495 1.0946 0.6299 0.086 Uiso 0.430(10) 1 calc PR B 1 H41C H 1.1248 1.0323 0.5753 0.086 Uiso 0.430(10) 1 calc PR B 1 C39' C 1.1409(8) 1.1815(4) 0.7618(8) 0.079(3) Uani 0.570(10) 1 d PDU B 2 H39D H 1.1022 1.2157 0.7137 0.119 Uiso 0.570(10) 1 calc PR B 2 H39E H 1.2193 1.2134 0.8035 0.119 Uiso 0.570(10) 1 calc PR B 2 H39F H 1.0939 1.1735 0.7988 0.119 Uiso 0.570(10) 1 calc PR B 2 C40' C 1.1411(9) 1.0879(7) 0.6143(4) 0.080(4) Uani 0.570(10) 1 d PDU B 2 H40D H 1.2018 1.1325 0.6142 0.120 Uiso 0.570(10) 1 calc PR B 2 H40E H 1.0631 1.1006 0.5761 0.120 Uiso 0.570(10) 1 calc PR B 2 H40F H 1.1512 1.0289 0.5877 0.120 Uiso 0.570(10) 1 calc PR B 2 C41' C 1.2807(5) 1.0734(6) 0.7730(7) 0.064(3) Uani 0.570(10) 1 d PDU B 2 H41D H 1.2911 1.0137 0.7489 0.096 Uiso 0.570(10) 1 calc PR B 2 H41E H 1.2925 1.0788 0.8394 0.096 Uiso 0.570(10) 1 calc PR B 2 H41F H 1.3381 1.1174 0.7676 0.096 Uiso 0.570(10) 1 calc PR B 2 C42 C 1.0929(3) 0.9468(2) 0.7579(3) 0.0368(9) Uani 1 1 d . . . H42 H 1.1740 0.9429 0.7895 0.044 Uiso 1 1 calc R B . C43 C 1.0080(3) 0.8789(2) 0.7545(2) 0.0295(8) Uani 1 1 d . B . C44 C 1.0488(3) 0.8129(2) 0.8109(2) 0.0291(8) Uani 1 1 d . . . H44 H 1.1262 0.8260 0.8589 0.035 Uiso 1 1 calc R B . C45 C 0.6165(3) 0.5932(2) 0.5116(3) 0.0408(9) Uani 1 1 d . . . H45A H 0.5447 0.6072 0.4648 0.061 Uiso 1 1 calc R . . H45B H 0.5995 0.5354 0.5264 0.061 Uiso 1 1 calc R . . H45C H 0.6773 0.5912 0.4862 0.061 Uiso 1 1 calc R . . C46 C 0.5611(3) 0.6901(3) 0.6170(3) 0.0412(9) Uani 1 1 d . . . H46A H 0.5897 0.7455 0.6641 0.062 Uiso 1 1 calc R . . H46B H 0.5285 0.6448 0.6419 0.062 Uiso 1 1 calc R . . H46C H 0.4998 0.7002 0.5591 0.062 Uiso 1 1 calc R . . C47 C 0.9947(3) 0.6600(3) 0.6085(3) 0.0412(9) Uani 1 1 d . . . H47A H 0.9862 0.6219 0.5496 0.062 Uiso 1 1 calc R . . H47B H 1.0152 0.6260 0.6592 0.062 Uiso 1 1 calc R . . H47C H 1.0570 0.7104 0.6250 0.062 Uiso 1 1 calc R . . C48 C 0.8474(4) 0.7368(3) 0.5156(3) 0.0448(10) Uani 1 1 d . . . H48A H 0.9057 0.7887 0.5274 0.067 Uiso 1 1 calc R . . H48B H 0.7711 0.7557 0.5066 0.067 Uiso 1 1 calc R . . H48C H 0.8399 0.6956 0.4587 0.067 Uiso 1 1 calc R . . N1 N 0.9882(2) 0.73756(17) 0.80126(19) 0.0258(6) Uani 1 1 d . A . N2 N 0.7690(2) 0.68294(17) 0.80628(19) 0.0269(6) Uani 1 1 d . A . N3 N 0.6577(2) 0.66050(18) 0.5965(2) 0.0313(7) Uani 1 1 d . A . N4 N 0.8855(2) 0.69217(18) 0.59654(19) 0.0295(6) Uani 1 1 d . A . O1 O 0.84376(19) 0.56883(14) 0.69670(15) 0.0272(5) Uani 1 1 d . A . O2 O 0.80610(19) 0.81715(14) 0.70368(16) 0.0290(5) Uani 1 1 d . A . V1 V 0.81598(5) 0.69067(4) 0.68424(4) 0.02581(17) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.0295(19) 0.0199(17) 0.034(2) 0.0087(15) 0.0024(15) -0.0045(14) C2 0.033(2) 0.031(2) 0.040(2) 0.0097(17) 0.0031(17) 0.0024(16) C3 0.046(2) 0.030(2) 0.046(3) 0.0124(19) -0.004(2) 0.0108(18) C4 0.052(3) 0.034(2) 0.033(2) 0.0174(18) -0.0076(19) -0.0042(18) C5 0.046(2) 0.031(2) 0.026(2) 0.0103(16) -0.0021(17) -0.0063(17) C6 0.071(3) 0.048(3) 0.033(2) 0.017(2) 0.010(2) -0.007(2) C7 0.037(2) 0.0223(17) 0.0271(19) 0.0085(14) 0.0021(15) -0.0027(14) C8 0.048(2) 0.0237(18) 0.032(2) 0.0088(15) 0.0162(18) -0.0029(16) C9 0.068(3) 0.0244(19) 0.032(2) 0.0064(16) 0.018(2) -0.0079(18) C10 0.080(3) 0.037(2) 0.044(3) -0.004(2) 0.004(2) -0.015(2) C11 0.079(3) 0.026(2) 0.042(2) -0.0009(18) 0.023(2) 0.002(2) C12 0.077(3) 0.031(2) 0.047(3) 0.0050(19) 0.032(3) 0.014(2) C13 0.049(2) 0.034(2) 0.046(2) 0.0114(18) 0.022(2) 0.0087(18) C14 0.039(2) 0.0209(17) 0.035(2) 0.0080(14) 0.0203(17) 0.0013(15) C15 0.035(2) 0.0283(18) 0.0276(18) 0.0097(15) 0.0136(16) 0.0022(15) C16 0.0305(18) 0.0194(16) 0.0256(18) 0.0059(13) 0.0116(15) 0.0011(13) C17 0.035(2) 0.0275(18) 0.0259(18) 0.0062(14) 0.0137(16) -0.0006(15) C18 0.037(2) 0.0260(18) 0.0269(18) 0.0089(15) 0.0124(16) -0.0020(15) C19 0.054(2) 0.0207(18) 0.040(2) 0.0042(16) 0.0233(19) -0.0048(16) C20 0.063(5) 0.043(4) 0.063(5) 0.007(3) 0.031(4) -0.015(3) C21 0.074(5) 0.038(4) 0.049(4) 0.019(3) 0.027(4) -0.009(3) C22 0.061(5) 0.053(5) 0.050(4) 0.009(3) 0.022(3) -0.027(4) C20' 0.045(6) 0.043(6) 0.031(5) 0.014(4) 0.016(5) -0.017(5) C21' 0.067(7) 0.035(6) 0.061(7) 0.019(5) 0.029(6) -0.002(5) C22' 0.039(6) 0.037(6) 0.055(7) 0.015(5) 0.011(5) -0.010(4) C23 0.042(2) 0.0226(18) 0.0291(19) 0.0081(15) 0.0104(17) -0.0053(15) C24 0.0310(18) 0.0290(18) 0.0232(17) 0.0081(14) 0.0151(15) 0.0073(14) C25 0.048(2) 0.0236(18) 0.034(2) 0.0083(15) 0.0193(18) 0.0070(16) C26 0.046(2) 0.036(2) 0.044(2) 0.0144(18) 0.021(2) 0.0172(18) C27 0.077(3) 0.030(2) 0.051(3) 0.0080(19) 0.041(2) 0.009(2) C28 0.048(2) 0.044(2) 0.034(2) 0.0117(18) 0.0199(19) 0.0051(18) C29 0.0308(18) 0.0212(16) 0.0211(17) 0.0091(13) 0.0095(14) -0.0020(13) C30 0.036(2) 0.0222(17) 0.0268(18) 0.0049(14) 0.0118(16) -0.0016(14) C31 0.036(2) 0.0192(17) 0.037(2) 0.0075(15) 0.0115(17) 0.0040(15) C32 0.040(2) 0.030(2) 0.057(3) 0.0259(19) 0.012(2) 0.0089(17) C33 0.041(2) 0.032(2) 0.069(3) 0.017(2) 0.017(2) 0.0104(18) C34 0.049(3) 0.048(3) 0.039(2) 0.017(2) 0.001(2) 0.009(2) C35 0.069(3) 0.042(3) 0.076(3) 0.040(3) 0.013(3) 0.018(2) C36 0.048(2) 0.031(2) 0.035(2) 0.0151(17) 0.0135(18) 0.0021(17) C37 0.044(2) 0.0273(19) 0.047(2) 0.0141(17) 0.0228(19) -0.0056(16) C38 0.053(3) 0.034(2) 0.072(3) 0.026(2) 0.030(2) -0.0078(19) C39 0.057(6) 0.033(5) 0.080(7) 0.020(5) 0.031(5) -0.017(4) C40 0.080(7) 0.052(7) 0.061(6) 0.016(5) 0.023(5) -0.027(5) C41 0.055(6) 0.067(7) 0.065(7) 0.014(5) 0.041(5) -0.002(5) C39' 0.073(6) 0.056(5) 0.102(8) 0.021(5) 0.030(5) -0.005(4) C40' 0.074(6) 0.102(7) 0.072(6) 0.051(5) 0.030(5) -0.007(5) C41' 0.059(5) 0.059(5) 0.069(6) 0.026(4) 0.019(4) -0.016(4) C42 0.040(2) 0.0274(19) 0.042(2) 0.0109(17) 0.0149(18) -0.0042(16) C43 0.0321(19) 0.0223(17) 0.035(2) 0.0114(15) 0.0129(16) -0.0010(14) C44 0.0273(18) 0.0265(18) 0.0298(19) 0.0097(15) 0.0067(15) -0.0002(14) C45 0.040(2) 0.035(2) 0.039(2) 0.0059(17) 0.0089(18) -0.0011(17) C46 0.030(2) 0.044(2) 0.045(2) 0.0082(19) 0.0105(18) 0.0039(17) C47 0.045(2) 0.044(2) 0.044(2) 0.0161(19) 0.025(2) 0.0099(19) C48 0.060(3) 0.049(2) 0.031(2) 0.0195(19) 0.021(2) 0.002(2) N1 0.0284(15) 0.0200(14) 0.0281(15) 0.0094(12) 0.0086(12) 0.0030(11) N2 0.0293(15) 0.0198(14) 0.0307(16) 0.0067(12) 0.0117(13) -0.0020(11) N3 0.0267(15) 0.0297(16) 0.0348(17) 0.0113(13) 0.0078(13) 0.0029(12) N4 0.0290(15) 0.0275(15) 0.0339(17) 0.0121(13) 0.0127(13) 0.0025(12) O1 0.0326(13) 0.0209(12) 0.0301(13) 0.0109(10) 0.0126(11) 0.0036(10) O2 0.0287(13) 0.0221(12) 0.0375(14) 0.0099(10) 0.0136(11) 0.0010(10) V1 0.0270(3) 0.0222(3) 0.0270(3) 0.0097(2) 0.0085(2) 0.0001(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C7 1.383(5) . ? C1 C2 1.397(5) . ? C1 N1 1.443(4) . ? C2 C3 1.401(5) . ? C2 H2 0.9500 . ? C3 C4 1.350(6) . ? C3 H3 0.9500 . ? C4 C5 1.404(6) . ? C4 H4 0.9500 . ? C5 C7 1.406(4) . ? C5 C6 1.501(6) . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.504(5) . ? C8 C9 1.399(5) . ? C8 C14 1.401(5) . ? C9 C11 1.393(6) . ? C9 C10 1.508(6) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C12 1.374(6) . ? C11 H11 0.9500 . ? C12 C13 1.395(5) . ? C12 H12 0.9500 . ? C13 C14 1.379(5) . ? C13 H13 0.9500 . ? C14 N2 1.441(4) . ? C15 N2 1.285(4) . ? C15 C16 1.438(5) . ? C15 H15 0.9500 . ? C16 C29 1.407(4) . ? C16 C17 1.414(4) . ? C17 C18 1.380(5) . ? C17 H17 0.9500 . ? C18 C23 1.400(5) . ? C18 C19 1.533(4) . ? C19 C22 1.492(6) . ? C19 C20' 1.510(7) . ? C19 C20 1.540(6) . ? C19 C21' 1.549(7) . ? C19 C21 1.559(5) . ? C19 C22' 1.577(7) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C20' H20D 0.9800 . ? C20' H20E 0.9800 . ? C20' H20F 0.9800 . ? C21' H21D 0.9800 . ? C21' H21E 0.9800 . ? C21' H21F 0.9800 . ? C22' H22D 0.9800 . ? C22' H22E 0.9800 . ? C22' H22F 0.9800 . ? C23 C24 1.395(4) . ? C23 H23 0.9500 . ? C24 C29 1.417(4) . ? C24 C25 1.545(5) . ? C25 C28 1.532(4) . ? C25 C27 1.538(5) . ? C25 C26 1.542(5) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 O1 1.319(3) . ? C30 O2 1.318(4) . ? C30 C43 1.419(5) . ? C30 C31 1.421(4) . ? C31 C36 1.399(5) . ? C31 C32 1.546(5) . ? C32 C34 1.520(6) . ? C32 C33 1.528(6) . ? C32 C35 1.560(4) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 C37 1.391(5) . ? C36 H36 0.9500 . ? C37 C42 1.389(4) . ? C37 C38 1.525(4) . ? C38 C40' 1.497(6) . ? C38 C40 1.505(5) . ? C38 C39' 1.539(6) . ? C38 C39 1.554(5) . ? C38 C41 1.554(5) . ? C38 C41' 1.578(6) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C39' H39D 0.9800 . ? C39' H39E 0.9800 . ? C39' H39F 0.9800 . ? C40' H40D 0.9800 . ? C40' H40E 0.9800 . ? C40' H40F 0.9800 . ? C41' H41D 0.9800 . ? C41' H41E 0.9800 . ? C41' H41F 0.9800 . ? C42 C43 1.405(4) . ? C42 H42 0.9500 . ? C43 C44 1.443(4) . ? C44 N1 1.288(4) . ? C44 H44 0.9500 . ? C45 N3 1.443(5) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 N3 1.447(4) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 N4 1.438(4) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 N4 1.468(4) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? N1 V1 2.195(3) . ? N2 V1 2.214(3) . ? N3 V1 1.891(3) . ? N4 V1 1.880(3) . ? O1 V1 1.963(2) . ? O2 V1 1.951(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C7 C1 C2 122.2(3) . . ? C7 C1 N1 117.8(3) . . ? C2 C1 N1 119.9(3) . . ? C1 C2 C3 117.8(4) . . ? C1 C2 H2 121.1 . . ? C3 C2 H2 121.1 . . ? C4 C3 C2 121.0(4) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 121.3(3) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C4 C5 C7 119.0(4) . . ? C4 C5 C6 118.8(3) . . ? C7 C5 C6 122.2(4) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? C1 C7 C5 118.5(3) . . ? C1 C7 C8 119.7(3) . . ? C5 C7 C8 121.7(3) . . ? C9 C8 C14 118.7(3) . . ? C9 C8 C7 122.0(3) . . ? C14 C8 C7 119.3(3) . . ? C11 C9 C8 119.1(4) . . ? C11 C9 C10 119.6(4) . . ? C8 C9 C10 121.3(4) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C12 C11 C9 121.3(4) . . ? C12 C11 H11 119.4 . . ? C9 C11 H11 119.4 . . ? C11 C12 C13 120.4(4) . . ? C11 C12 H12 119.8 . . ? C13 C12 H12 119.8 . . ? C14 C13 C12 118.5(4) . . ? C14 C13 H13 120.7 . . ? C12 C13 H13 120.7 . . ? C13 C14 C8 121.9(3) . . ? C13 C14 N2 120.5(3) . . ? C8 C14 N2 117.5(3) . . ? N2 C15 C16 125.8(3) . . ? N2 C15 H15 117.1 . . ? C16 C15 H15 117.1 . . ? C29 C16 C17 120.9(3) . . ? C29 C16 C15 121.8(3) . . ? C17 C16 C15 116.6(3) . . ? C18 C17 C16 121.6(3) . . ? C18 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? C17 C18 C23 116.5(3) . . ? C17 C18 C19 122.4(3) . . ? C23 C18 C19 121.1(3) . . ? C22 C19 C20' 133.1(5) . . ? C22 C19 C18 110.0(3) . . ? C20' C19 C18 112.9(5) . . ? C22 C19 C20 111.3(4) . . ? C20' C19 C20 33.7(4) . . ? C18 C19 C20 111.7(4) . . ? C22 C19 C21' 66.7(5) . . ? C20' C19 C21' 109.4(5) . . ? C18 C19 C21' 115.1(5) . . ? C20 C19 C21' 130.4(5) . . ? C22 C19 C21 109.9(4) . . ? C20' C19 C21 74.9(5) . . ? C18 C19 C21 106.7(3) . . ? C20 C19 C21 107.1(4) . . ? C21' C19 C21 43.8(4) . . ? C22 C19 C22' 40.9(4) . . ? C20' C19 C22' 108.0(5) . . ? C18 C19 C22' 105.6(4) . . ? C20 C19 C22' 76.4(5) . . ? C21' C19 C22' 105.3(5) . . ? C21 C19 C22' 143.1(5) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? C19 C20' H20D 109.5 . . ? C19 C20' H20E 109.5 . . ? H20D C20' H20E 109.5 . . ? C19 C20' H20F 109.5 . . ? H20D C20' H20F 109.5 . . ? H20E C20' H20F 109.5 . . ? C19 C21' H21D 109.5 . . ? C19 C21' H21E 109.5 . . ? H21D C21' H21E 109.5 . . ? C19 C21' H21F 109.5 . . ? H21D C21' H21F 109.5 . . ? H21E C21' H21F 109.5 . . ? C19 C22' H22D 109.5 . . ? C19 C22' H22E 109.5 . . ? H22D C22' H22E 109.5 . . ? C19 C22' H22F 109.5 . . ? H22D C22' H22F 109.5 . . ? H22E C22' H22F 109.5 . . ? C24 C23 C18 124.3(3) . . ? C24 C23 H23 117.8 . . ? C18 C23 H23 117.8 . . ? C23 C24 C29 118.4(3) . . ? C23 C24 C25 120.0(3) . . ? C29 C24 C25 121.6(3) . . ? C28 C25 C27 106.6(3) . . ? C28 C25 C26 109.5(3) . . ? C27 C25 C26 107.3(3) . . ? C28 C25 C24 110.9(3) . . ? C27 C25 C24 112.8(3) . . ? C26 C25 C24 109.6(3) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C25 C28 H28A 109.5 . . ? C25 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C25 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O1 C29 C16 121.2(3) . . ? O1 C29 C24 120.5(3) . . ? C16 C29 C24 118.2(3) . . ? O2 C30 C43 121.5(3) . . ? O2 C30 C31 121.1(3) . . ? C43 C30 C31 117.4(3) . . ? C36 C31 C30 118.1(3) . . ? C36 C31 C32 121.0(3) . . ? C30 C31 C32 120.9(3) . . ? C34 C32 C33 110.0(3) . . ? C34 C32 C31 111.1(3) . . ? C33 C32 C31 109.7(3) . . ? C34 C32 C35 107.3(3) . . ? C33 C32 C35 106.5(3) . . ? C31 C32 C35 112.1(3) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C37 C36 C31 125.2(3) . . ? C37 C36 H36 117.4 . . ? C31 C36 H36 117.4 . . ? C42 C37 C36 116.0(3) . . ? C42 C37 C38 122.1(3) . . ? C36 C37 C38 121.9(3) . . ? C40' C38 C40 131.8(6) . . ? C40' C38 C37 110.7(4) . . ? C40 C38 C37 112.4(4) . . ? C40' C38 C39' 113.0(5) . . ? C40 C38 C39' 71.0(5) . . ? C37 C38 C39' 109.6(4) . . ? C40' C38 C39 73.2(5) . . ? C40 C38 C39 110.1(4) . . ? C37 C38 C39 110.1(4) . . ? C39' C38 C39 43.4(4) . . ? C40' C38 C41 34.5(4) . . ? C40 C38 C41 110.6(4) . . ? C37 C38 C41 106.9(4) . . ? C39' C38 C41 139.2(5) . . ? C39 C38 C41 106.4(4) . . ? C40' C38 C41' 107.6(5) . . ? C40 C38 C41' 36.2(4) . . ? C37 C38 C41' 110.4(3) . . ? C39' C38 C41' 105.5(5) . . ? C39 C38 C41' 135.9(5) . . ? C41 C38 C41' 77.5(5) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? C38 C41 H41A 109.5 . . ? C38 C41 H41B 109.5 . . ? C38 C41 H41C 109.5 . . ? C38 C39' H39D 109.5 . . ? C38 C39' H39E 109.5 . . ? H39D C39' H39E 109.5 . . ? C38 C39' H39F 109.5 . . ? H39D C39' H39F 109.5 . . ? H39E C39' H39F 109.5 . . ? C38 C40' H40D 109.5 . . ? C38 C40' H40E 109.5 . . ? H40D C40' H40E 109.5 . . ? C38 C40' H40F 109.5 . . ? H40D C40' H40F 109.5 . . ? H40E C40' H40F 109.5 . . ? C38 C41' H41D 109.5 . . ? C38 C41' H41E 109.5 . . ? H41D C41' H41E 109.5 . . ? C38 C41' H41F 109.5 . . ? H41D C41' H41F 109.5 . . ? H41E C41' H41F 109.5 . . ? C37 C42 C43 121.6(3) . . ? C37 C42 H42 119.2 . . ? C43 C42 H42 119.2 . . ? C42 C43 C30 121.4(3) . . ? C42 C43 C44 117.5(3) . . ? C30 C43 C44 120.4(3) . . ? N1 C44 C43 125.0(3) . . ? N1 C44 H44 117.5 . . ? C43 C44 H44 117.5 . . ? N3 C45 H45A 109.5 . . ? N3 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N3 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? N3 C46 H46A 109.5 . . ? N3 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N3 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? N4 C47 H47A 109.5 . . ? N4 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? N4 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? N4 C48 H48A 109.5 . . ? N4 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? N4 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C44 N1 C1 116.8(3) . . ? C44 N1 V1 122.1(2) . . ? C1 N1 V1 120.74(19) . . ? C15 N2 C14 116.8(3) . . ? C15 N2 V1 123.3(2) . . ? C14 N2 V1 119.15(19) . . ? C45 N3 C46 111.7(3) . . ? C45 N3 V1 124.8(2) . . ? C46 N3 V1 122.4(2) . . ? C47 N4 C48 110.5(3) . . ? C47 N4 V1 123.3(2) . . ? C48 N4 V1 125.7(2) . . ? C29 O1 V1 129.7(2) . . ? C30 O2 V1 126.5(2) . . ? N4 V1 N3 97.47(12) . . ? N4 V1 O2 95.95(10) . . ? N3 V1 O2 92.95(11) . . ? N4 V1 O1 92.33(10) . . ? N3 V1 O1 96.27(11) . . ? O2 V1 O1 166.71(10) . . ? N4 V1 N1 90.51(12) . . ? N3 V1 N1 170.67(12) . . ? O2 V1 N1 81.37(10) . . ? O1 V1 N1 88.18(10) . . ? N4 V1 N2 168.41(11) . . ? N3 V1 N2 92.98(11) . . ? O2 V1 N2 88.46(9) . . ? O1 V1 N2 81.54(9) . . ? N1 V1 N2 79.54(10) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 C1 C2 C3 2.9(5) . . . . ? N1 C1 C2 C3 -176.6(3) . . . . ? C1 C2 C3 C4 0.4(6) . . . . ? C2 C3 C4 C5 -1.5(6) . . . . ? C3 C4 C5 C7 -0.6(6) . . . . ? C3 C4 C5 C6 178.9(4) . . . . ? C2 C1 C7 C5 -5.0(5) . . . . ? N1 C1 C7 C5 174.5(3) . . . . ? C2 C1 C7 C8 178.6(3) . . . . ? N1 C1 C7 C8 -1.9(5) . . . . ? C4 C5 C7 C1 3.8(5) . . . . ? C6 C5 C7 C1 -175.8(3) . . . . ? C4 C5 C7 C8 -179.9(3) . . . . ? C6 C5 C7 C8 0.5(6) . . . . ? C1 C7 C8 C9 -112.4(4) . . . . ? C5 C7 C8 C9 71.3(5) . . . . ? C1 C7 C8 C14 66.2(4) . . . . ? C5 C7 C8 C14 -110.1(4) . . . . ? C14 C8 C9 C11 2.8(5) . . . . ? C7 C8 C9 C11 -178.6(3) . . . . ? C14 C8 C9 C10 -175.3(3) . . . . ? C7 C8 C9 C10 3.3(5) . . . . ? C8 C9 C11 C12 0.7(6) . . . . ? C10 C9 C11 C12 178.9(4) . . . . ? C9 C11 C12 C13 -3.1(6) . . . . ? C11 C12 C13 C14 1.9(6) . . . . ? C12 C13 C14 C8 1.7(5) . . . . ? C12 C13 C14 N2 -174.6(3) . . . . ? C9 C8 C14 C13 -4.1(5) . . . . ? C7 C8 C14 C13 177.3(3) . . . . ? C9 C8 C14 N2 172.3(3) . . . . ? C7 C8 C14 N2 -6.3(4) . . . . ? N2 C15 C16 C29 21.1(5) . . . . ? N2 C15 C16 C17 -168.3(3) . . . . ? C29 C16 C17 C18 -1.7(5) . . . . ? C15 C16 C17 C18 -172.3(3) . . . . ? C16 C17 C18 C23 2.2(5) . . . . ? C16 C17 C18 C19 -178.5(3) . . . . ? C17 C18 C19 C22 121.5(5) . . . . ? C23 C18 C19 C22 -59.2(5) . . . . ? C17 C18 C19 C20' -39.1(6) . . . . ? C23 C18 C19 C20' 140.3(6) . . . . ? C17 C18 C19 C20 -2.6(5) . . . . ? C23 C18 C19 C20 176.7(4) . . . . ? C17 C18 C19 C21' -165.6(6) . . . . ? C23 C18 C19 C21' 13.7(6) . . . . ? C17 C18 C19 C21 -119.4(4) . . . . ? C23 C18 C19 C21 60.0(5) . . . . ? C17 C18 C19 C22' 78.7(6) . . . . ? C23 C18 C19 C22' -101.9(6) . . . . ? C17 C18 C23 C24 -0.1(5) . . . . ? C19 C18 C23 C24 -179.5(3) . . . . ? C18 C23 C24 C29 -2.4(5) . . . . ? C18 C23 C24 C25 178.9(3) . . . . ? C23 C24 C25 C28 120.0(3) . . . . ? C29 C24 C25 C28 -58.7(4) . . . . ? C23 C24 C25 C27 0.6(5) . . . . ? C29 C24 C25 C27 -178.1(3) . . . . ? C23 C24 C25 C26 -118.9(3) . . . . ? C29 C24 C25 C26 62.4(4) . . . . ? C17 C16 C29 O1 -177.6(3) . . . . ? C15 C16 C29 O1 -7.5(5) . . . . ? C17 C16 C29 C24 -0.9(5) . . . . ? C15 C16 C29 C24 169.2(3) . . . . ? C23 C24 C29 O1 179.5(3) . . . . ? C25 C24 C29 O1 -1.8(5) . . . . ? C23 C24 C29 C16 2.8(5) . . . . ? C25 C24 C29 C16 -178.5(3) . . . . ? O2 C30 C31 C36 -176.6(3) . . . . ? C43 C30 C31 C36 4.3(5) . . . . ? O2 C30 C31 C32 2.9(5) . . . . ? C43 C30 C31 C32 -176.2(3) . . . . ? C36 C31 C32 C34 118.5(4) . . . . ? C30 C31 C32 C34 -61.0(4) . . . . ? C36 C31 C32 C33 -119.7(4) . . . . ? C30 C31 C32 C33 60.8(4) . . . . ? C36 C31 C32 C35 -1.6(5) . . . . ? C30 C31 C32 C35 178.9(3) . . . . ? C30 C31 C36 C37 -2.2(6) . . . . ? C32 C31 C36 C37 178.3(4) . . . . ? C31 C36 C37 C42 -1.6(6) . . . . ? C31 C36 C37 C38 177.1(4) . . . . ? C42 C37 C38 C40' 112.6(6) . . . . ? C36 C37 C38 C40' -66.1(6) . . . . ? C42 C37 C38 C40 -45.3(7) . . . . ? C36 C37 C38 C40 136.0(6) . . . . ? C42 C37 C38 C39' -122.2(6) . . . . ? C36 C37 C38 C39' 59.2(6) . . . . ? C42 C37 C38 C39 -168.5(6) . . . . ? C36 C37 C38 C39 12.9(6) . . . . ? C42 C37 C38 C41 76.3(6) . . . . ? C36 C37 C38 C41 -102.4(6) . . . . ? C42 C37 C38 C41' -6.4(6) . . . . ? C36 C37 C38 C41' 175.0(5) . . . . ? C36 C37 C42 C43 3.1(5) . . . . ? C38 C37 C42 C43 -175.6(3) . . . . ? C37 C42 C43 C30 -0.8(6) . . . . ? C37 C42 C43 C44 -171.4(3) . . . . ? O2 C30 C43 C42 178.0(3) . . . . ? C31 C30 C43 C42 -3.0(5) . . . . ? O2 C30 C43 C44 -11.7(5) . . . . ? C31 C30 C43 C44 167.3(3) . . . . ? C42 C43 C44 N1 -164.6(4) . . . . ? C30 C43 C44 N1 24.7(5) . . . . ? C43 C44 N1 C1 -165.7(3) . . . . ? C43 C44 N1 V1 7.0(5) . . . . ? C7 C1 N1 C44 88.9(4) . . . . ? C2 C1 N1 C44 -91.6(4) . . . . ? C7 C1 N1 V1 -83.9(3) . . . . ? C2 C1 N1 V1 95.7(3) . . . . ? C16 C15 N2 C14 -166.1(3) . . . . ? C16 C15 N2 V1 3.9(5) . . . . ? C13 C14 N2 C15 -96.0(4) . . . . ? C8 C14 N2 C15 87.5(4) . . . . ? C13 C14 N2 V1 93.6(3) . . . . ? C8 C14 N2 V1 -82.9(3) . . . . ? C16 C29 O1 V1 -35.4(4) . . . . ? C24 C29 O1 V1 148.0(3) . . . . ? C43 C30 O2 V1 -37.0(4) . . . . ? C31 C30 O2 V1 144.0(3) . . . . ? C47 N4 V1 N3 -141.8(3) . . . . ? C48 N4 V1 N3 47.7(3) . . . . ? C47 N4 V1 O2 124.4(3) . . . . ? C48 N4 V1 O2 -46.1(3) . . . . ? C47 N4 V1 O1 -45.2(3) . . . . ? C48 N4 V1 O1 144.3(3) . . . . ? C47 N4 V1 N1 43.0(3) . . . . ? C48 N4 V1 N1 -127.5(3) . . . . ? C47 N4 V1 N2 12.5(7) . . . . ? C48 N4 V1 N2 -158.0(5) . . . . ? C45 N3 V1 N4 44.1(3) . . . . ? C46 N3 V1 N4 -148.8(3) . . . . ? C45 N3 V1 O2 140.5(3) . . . . ? C46 N3 V1 O2 -52.4(3) . . . . ? C45 N3 V1 O1 -49.1(3) . . . . ? C46 N3 V1 O1 118.0(3) . . . . ? C45 N3 V1 N1 -167.3(5) . . . . ? C46 N3 V1 N1 -0.2(8) . . . . ? C45 N3 V1 N2 -130.9(3) . . . . ? C46 N3 V1 N2 36.2(3) . . . . ? C30 O2 V1 N4 -39.3(3) . . . . ? C30 O2 V1 N3 -137.2(3) . . . . ? C30 O2 V1 O1 88.9(5) . . . . ? C30 O2 V1 N1 50.3(3) . . . . ? C30 O2 V1 N2 129.9(3) . . . . ? C29 O1 V1 N4 -145.6(3) . . . . ? C29 O1 V1 N3 -47.8(3) . . . . ? C29 O1 V1 O2 85.9(5) . . . . ? C29 O1 V1 N1 124.0(3) . . . . ? C29 O1 V1 N2 44.3(2) . . . . ? C44 N1 V1 N4 61.5(3) . . . . ? C1 N1 V1 N4 -126.2(3) . . . . ? C44 N1 V1 N3 -87.4(7) . . . . ? C1 N1 V1 N3 84.9(7) . . . . ? C44 N1 V1 O2 -34.5(3) . . . . ? C1 N1 V1 O2 137.9(3) . . . . ? C44 N1 V1 O1 153.8(3) . . . . ? C1 N1 V1 O1 -33.9(2) . . . . ? C44 N1 V1 N2 -124.5(3) . . . . ? C1 N1 V1 N2 47.9(2) . . . . ? C15 N2 V1 N4 -85.9(6) . . . . ? C14 N2 V1 N4 83.8(6) . . . . ? C15 N2 V1 N3 68.6(3) . . . . ? C14 N2 V1 N3 -121.7(2) . . . . ? C15 N2 V1 O2 161.5(3) . . . . ? C14 N2 V1 O2 -28.8(2) . . . . ? C15 N2 V1 O1 -27.3(3) . . . . ? C14 N2 V1 O1 142.4(2) . . . . ? C15 N2 V1 N1 -117.0(3) . . . . ? C14 N2 V1 N1 52.7(2) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.826 1.000 668 164 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.949 _diffrn_reflns_theta_full 27.56 _diffrn_measured_fraction_theta_full 0.949 _refine_diff_density_max 1.183 _refine_diff_density_min -0.490 _refine_diff_density_rms 0.084 # Attachment '- compound 25.cif' data_compound25 _database_code_depnum_ccdc_archive 'CCDC 791870' #TrackingRef '- compound 25.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C55 H64 N5 Nb O2' _chemical_formula_sum 'C55 H64 N5 Nb O2' _chemical_formula_weight 920.02 _chemical_absolute_configuration rmad 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' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.5500(10) _cell_length_b 10.9436(12) _cell_length_c 11.4253(14) _cell_angle_alpha 97.974(6) _cell_angle_beta 93.029(14) _cell_angle_gamma 99.572(9) _cell_volume 1162.5(2) _cell_formula_units_Z 1 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 6108 _cell_measurement_theta_min 1.91 _cell_measurement_theta_max 34.82 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.314 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 486 _exptl_absorpt_coefficient_mu 0.307 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9245 _exptl_absorpt_correction_T_max 0.9412 _exptl_absorpt_process_details Crystalclear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Rigaku Saturn70 CCD' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.314 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 20069 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0779 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.91 _diffrn_reflns_theta_max 35.12 _reflns_number_total 15623 _reflns_number_gt 14011 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'CrystalStructure 4.0' _computing_publication_material 'CrystalStructure 4.0 (Rigaku, 2009)' _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^)+(0.0285P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0609(14) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.003(14) _refine_ls_number_reflns 15623 _refine_ls_number_parameters 582 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0442 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.0804 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 1.010 _refine_ls_restrained_S_all 1.010 _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 Nb1 Nb 1.004353(9) -0.003726(9) 1.001823(9) 0.01332(4) Uani 1 1 d . . . O2 O 0.98752(14) 0.16744(12) 1.08245(12) 0.0153(2) Uani 1 1 d . . . N3 N 1.08456(17) 0.13990(16) 0.86542(15) 0.0162(3) Uani 1 1 d . . . O1 O 0.97281(15) -0.07907(14) 1.15397(12) 0.0167(3) Uani 1 1 d . . . N2 N 0.94253(16) -0.12305(14) 0.87487(14) 0.0148(3) Uani 1 1 d . . . N1 N 0.75522(16) -0.04481(15) 1.00754(14) 0.0143(3) Uani 1 1 d . . . N5 N 1.20590(17) -0.02335(16) 1.02037(16) 0.0190(3) Uani 1 1 d . . . C37 C 0.95749(19) 0.31412(17) 0.95113(16) 0.0143(3) Uani 1 1 d . . . N4 N 0.98600(18) 0.27975(16) 0.73752(15) 0.0188(3) Uani 1 1 d . . . C11 C 0.66908(19) -0.06110(16) 0.79807(16) 0.0137(3) Uani 1 1 d . . . C32 C 0.95887(19) 0.28046(16) 1.06537(16) 0.0132(3) Uani 1 1 d . . . C22 C 0.73019(19) -0.16563(17) 1.17086(17) 0.0161(3) Uani 1 1 d . . . C1 C 0.70953(19) -0.18623(16) 0.76571(16) 0.0142(3) Uani 1 1 d . . . C23 C 0.87600(19) -0.14010(17) 1.21286(17) 0.0142(3) Uani 1 1 d . . . C42 C 0.97387(19) 0.22052(17) 0.84203(16) 0.0141(3) Uani 1 1 d . . . H42 H 0.8810 0.1611 0.8281 0.017 Uiso 1 1 calc R . . C2 C 0.84600(19) -0.20700(16) 0.79870(16) 0.0137(3) Uani 1 1 d . . . C29 C 1.1231(3) -0.0105(2) 1.3958(2) 0.0259(4) Uani 1 1 d . . . H29A H 1.1100 0.0242 1.3223 0.039 Uiso 1 1 calc R . . H29B H 1.2242 0.0077 1.4239 0.039 Uiso 1 1 calc R . . H29C H 1.0677 0.0275 1.4562 0.039 Uiso 1 1 calc R . . C52 C 0.5134(3) 0.5260(3) -0.0439(3) 0.0405(8) Uani 1 1 d . . . H52 H 0.5806 0.5329 -0.1021 0.049 Uiso 1 1 calc R . . C51 C 0.5366(3) 0.4622(3) 0.0501(3) 0.0334(7) Uani 1 1 d . . . H51 H 0.6191 0.4247 0.0555 0.040 Uiso 1 1 calc R . . C6 C 0.6096(2) -0.28735(16) 0.69794(16) 0.0150(3) Uani 1 1 d . . . C12 C 0.68550(19) 0.00108(18) 0.91349(17) 0.0140(3) Uani 1 1 d . . . C47 C 1.2999(2) 0.0469(2) 1.1215(2) 0.0258(4) Uani 1 1 d . . . H47A H 1.3272 -0.0113 1.1729 0.039 Uiso 1 1 calc R . . H47B H 1.2499 0.1069 1.1666 0.039 Uiso 1 1 calc R . . H47C H 1.3856 0.0922 1.0928 0.039 Uiso 1 1 calc R . . C5 C 0.6550(2) -0.40161(17) 0.65381(17) 0.0166(3) Uani 1 1 d . . . C24 C 0.9156(2) -0.18141(17) 1.32131(17) 0.0165(3) Uani 1 1 d . . . C25 C 0.8094(2) -0.24686(18) 1.37805(18) 0.0201(4) Uani 1 1 d . . . H25 H 0.8350 -0.2738 1.4505 0.024 Uiso 1 1 calc R . . C21 C 0.67924(19) -0.11767(17) 1.06816(17) 0.0161(3) Uani 1 1 d . . . H21 H 0.5809 -0.1421 1.0431 0.019 Uiso 1 1 calc R . . C13 C 0.64195(19) 0.11871(17) 0.94479(18) 0.0165(3) Uani 1 1 d . . . H13 H 0.6553 0.1591 1.0247 0.020 Uiso 1 1 calc R . . C16 C 0.61398(19) 0.00161(17) 0.70695(17) 0.0158(3) Uani 1 1 d . . . C7 C 0.4631(2) -0.28097(19) 0.67532(18) 0.0201(4) Uani 1 1 d . . . H7 H 0.4286 -0.2073 0.7059 0.024 Uiso 1 1 calc R . . C14 C 0.5810(2) 0.17338(17) 0.85962(18) 0.0177(3) Uani 1 1 d . . . H14 H 0.5478 0.2499 0.8815 0.021 Uiso 1 1 calc R . . C36 C 0.9262(2) 0.43079(18) 0.93575(18) 0.0188(4) Uani 1 1 d . . . H36 H 0.9216 0.4530 0.8583 0.023 Uiso 1 1 calc R . . C35 C 0.9015(2) 0.51508(19) 1.03088(19) 0.0213(4) Uani 1 1 d . . . H35 H 0.8830 0.5954 1.0193 0.026 Uiso 1 1 calc R . . C38 C 0.9269(2) 0.32683(18) 1.28904(17) 0.0186(4) Uani 1 1 d . . . C27 C 0.6275(2) -0.23443(19) 1.23124(19) 0.0205(4) Uani 1 1 d . . . H27 H 0.5306 -0.2527 1.2006 0.025 Uiso 1 1 calc R . . C28 C 1.0720(2) -0.15302(19) 1.37262(18) 0.0199(4) Uani 1 1 d . . . C45 C 0.9108(2) 0.2156(2) 0.62700(19) 0.0251(4) Uani 1 1 d . . . H45A H 0.9775 0.1786 0.5766 0.038 Uiso 1 1 calc R . . H45B H 0.8687 0.2754 0.5863 0.038 Uiso 1 1 calc R . . H45C H 0.8352 0.1491 0.6433 0.038 Uiso 1 1 calc R . . C34 C 0.9040(2) 0.48110(18) 1.14375(18) 0.0190(4) Uani 1 1 d . . . H34 H 0.8874 0.5395 1.2089 0.023 Uiso 1 1 calc R . . C33 C 0.9300(2) 0.36387(17) 1.16422(17) 0.0160(3) Uani 1 1 d . . . C39 C 0.8198(2) 0.2058(2) 1.29019(19) 0.0237(4) Uani 1 1 d . . . H39A H 0.8498 0.1365 1.2396 0.036 Uiso 1 1 calc R . . H39B H 0.7253 0.2167 1.2602 0.036 Uiso 1 1 calc R . . H39C H 0.8158 0.1870 1.3715 0.036 Uiso 1 1 calc R . . C17 C 0.6112(2) -0.04425(19) 0.58455(18) 0.0199(4) Uani 1 1 d . . . H17 H 0.6443 -0.1204 0.5607 0.024 Uiso 1 1 calc R . . C26 C 0.6668(2) -0.27536(19) 1.33438(19) 0.0223(4) Uani 1 1 d . . . H26 H 0.5979 -0.3223 1.3753 0.027 Uiso 1 1 calc R . . C46 C 1.1055(2) 0.3745(2) 0.7223(2) 0.0247(4) Uani 1 1 d . . . H46A H 1.1432 0.4221 0.7997 0.037 Uiso 1 1 calc R . . H46B H 1.0744 0.4313 0.6712 0.037 Uiso 1 1 calc R . . H46C H 1.1801 0.3343 0.6856 0.037 Uiso 1 1 calc R . . C4 C 0.7971(2) -0.41491(17) 0.68207(18) 0.0188(4) Uani 1 1 d . . . H4 H 0.8293 -0.4894 0.6505 0.023 Uiso 1 1 calc R . . C50 C 0.4397(2) 0.4528(2) 0.1364(2) 0.0253(4) Uani 1 1 d . . . C18 C 0.5621(3) 0.0182(2) 0.4998(2) 0.0257(4) Uani 1 1 d . . . H18 H 0.5629 -0.0140 0.4183 0.031 Uiso 1 1 calc R . . C19 C 0.5103(2) 0.1306(2) 0.5329(2) 0.0269(4) Uani 1 1 d . . . H19 H 0.4736 0.1727 0.4740 0.032 Uiso 1 1 calc R . . C40 C 1.0767(2) 0.3095(2) 1.33152(19) 0.0242(4) Uani 1 1 d . . . H40A H 1.1419 0.3900 1.3401 0.036 Uiso 1 1 calc R . . H40B H 1.1103 0.2485 1.2734 0.036 Uiso 1 1 calc R . . H40C H 1.0734 0.2790 1.4082 0.036 Uiso 1 1 calc R . . C8 C 0.3705(2) -0.3796(2) 0.6100(2) 0.0251(4) Uani 1 1 d . . . H8 H 0.2731 -0.3733 0.5966 0.030 Uiso 1 1 calc R . . C55 C 0.3194(2) 0.5079(2) 0.1264(2) 0.0272(5) Uani 1 1 d . . . H55 H 0.2525 0.5023 0.1850 0.033 Uiso 1 1 calc R . . C53 C 0.3930(3) 0.5797(3) -0.0533(2) 0.0378(6) Uani 1 1 d . . . H53 H 0.3769 0.6227 -0.1181 0.045 Uiso 1 1 calc R . . C41 C 0.8836(3) 0.4296(2) 1.3782(2) 0.0308(5) Uani 1 1 d . . . H41A H 0.8801 0.4025 1.4564 0.046 Uiso 1 1 calc R . . H41B H 0.7895 0.4450 1.3522 0.046 Uiso 1 1 calc R . . H41C H 0.9536 0.5069 1.3830 0.046 Uiso 1 1 calc R . . C30 C 1.1653(2) -0.2160(2) 1.2855(2) 0.0265(4) Uani 1 1 d . . . H30A H 1.1387 -0.3073 1.2787 0.040 Uiso 1 1 calc R . . H30B H 1.2657 -0.1904 1.3149 0.040 Uiso 1 1 calc R . . H30C H 1.1510 -0.1903 1.2076 0.040 Uiso 1 1 calc R . . C54 C 0.2959(3) 0.5706(2) 0.0322(2) 0.0320(5) Uani 1 1 d . . . H54 H 0.2130 0.6075 0.0261 0.038 Uiso 1 1 calc R . . C31 C 1.0901(3) -0.2009(2) 1.4912(2) 0.0301(5) Uani 1 1 d . . . H31A H 1.0321 -0.1613 1.5483 0.045 Uiso 1 1 calc R . . H31B H 1.1905 -0.1801 1.5213 0.045 Uiso 1 1 calc R . . H31C H 1.0593 -0.2921 1.4799 0.045 Uiso 1 1 calc R . . C49 C 0.4667(3) 0.3861(3) 0.2395(3) 0.0405(6) Uani 1 1 d . . . H49A H 0.5173 0.4466 0.3057 0.061 Uiso 1 1 calc R . . H49B H 0.5248 0.3222 0.2160 0.061 Uiso 1 1 calc R . . H49C H 0.3757 0.3460 0.2640 0.061 Uiso 1 1 calc R . . C3 C 0.8879(2) -0.32327(17) 0.75326(18) 0.0174(3) Uani 1 1 d . . . H3 H 0.9816 -0.3362 0.7736 0.021 Uiso 1 1 calc R . . C10 C 0.5568(2) -0.49964(18) 0.58456(18) 0.0223(4) Uani 1 1 d . . . H10 H 0.5886 -0.5742 0.5526 0.027 Uiso 1 1 calc R . . C44 C 1.2234(2) 0.21816(19) 0.91503(19) 0.0207(4) Uani 1 1 d . . . H44A H 1.2947 0.1642 0.9223 0.031 Uiso 1 1 calc R . . H44B H 1.2121 0.2630 0.9934 0.031 Uiso 1 1 calc R . . H44C H 1.2549 0.2787 0.8620 0.031 Uiso 1 1 calc R . . C43 C 1.1107(2) 0.0672(2) 0.75232(19) 0.0227(4) Uani 1 1 d . . . H43A H 1.1544 0.1246 0.7005 0.034 Uiso 1 1 calc R . . H43B H 1.0202 0.0197 0.7135 0.034 Uiso 1 1 calc R . . H43C H 1.1749 0.0092 0.7678 0.034 Uiso 1 1 calc R . . C48 C 1.2786(2) -0.1123(2) 0.9513(2) 0.0267(5) Uani 1 1 d . . . H48A H 1.3585 -0.0665 0.9157 0.040 Uiso 1 1 calc R . . H48B H 1.2117 -0.1639 0.8885 0.040 Uiso 1 1 calc R . . H48C H 1.3144 -0.1663 1.0032 0.040 Uiso 1 1 calc R . . C9 C 0.4182(3) -0.4897(2) 0.5627(2) 0.0265(4) Uani 1 1 d . . . H9 H 0.3541 -0.5565 0.5159 0.032 Uiso 1 1 calc R . . C15 C 0.5665(2) 0.11778(17) 0.73938(18) 0.0178(3) Uani 1 1 d . . . C20 C 0.5132(2) 0.1784(2) 0.6499(2) 0.0239(4) Uani 1 1 d . . . H20 H 0.4786 0.2542 0.6716 0.029 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 Nb1 0.01135(6) 0.01277(7) 0.01509(7) -0.00013(5) 0.00087(5) 0.00187(4) O2 0.0189(6) 0.0133(6) 0.0138(6) 0.0001(5) 0.0015(5) 0.0047(5) N3 0.0143(7) 0.0156(7) 0.0184(8) 0.0015(6) 0.0021(6) 0.0023(6) O1 0.0146(6) 0.0182(7) 0.0168(6) 0.0039(5) 0.0003(5) 0.0010(5) N2 0.0134(7) 0.0130(7) 0.0168(7) -0.0016(5) 0.0010(5) 0.0022(5) N1 0.0130(7) 0.0149(7) 0.0150(7) 0.0003(6) 0.0019(5) 0.0035(5) N5 0.0121(7) 0.0208(8) 0.0237(9) 0.0016(6) 0.0006(6) 0.0034(6) C37 0.0129(7) 0.0142(8) 0.0151(8) 0.0014(6) 0.0015(6) 0.0013(6) N4 0.0220(8) 0.0189(8) 0.0142(7) 0.0039(6) 0.0024(6) -0.0019(6) C11 0.0132(7) 0.0110(7) 0.0168(8) 0.0015(6) 0.0007(6) 0.0019(6) C32 0.0138(7) 0.0108(7) 0.0144(8) 0.0002(6) 0.0017(6) 0.0015(6) C22 0.0143(8) 0.0158(8) 0.0171(8) 0.0010(6) 0.0014(6) 0.0006(6) C1 0.0145(7) 0.0131(7) 0.0146(8) 0.0005(6) 0.0006(6) 0.0027(6) C23 0.0164(8) 0.0103(7) 0.0151(8) -0.0012(6) 0.0023(6) 0.0019(6) C42 0.0138(7) 0.0164(8) 0.0120(8) 0.0025(6) 0.0020(6) 0.0018(6) C2 0.0148(7) 0.0140(7) 0.0120(8) 0.0004(6) -0.0001(6) 0.0034(6) C29 0.0288(10) 0.0183(9) 0.0272(11) -0.0022(8) -0.0068(8) 0.0014(8) C52 0.0391(17) 0.0391(16) 0.0377(16) -0.0083(12) 0.0126(13) -0.0004(12) C51 0.0258(13) 0.0290(12) 0.0409(16) -0.0096(11) 0.0056(11) 0.0032(10) C6 0.0190(8) 0.0110(7) 0.0146(8) 0.0038(6) -0.0014(6) 0.0004(6) C12 0.0104(7) 0.0139(8) 0.0173(8) 0.0016(6) 0.0013(6) 0.0017(6) C47 0.0177(9) 0.0311(12) 0.0257(11) -0.0005(9) -0.0021(8) 0.0007(8) C5 0.0237(9) 0.0126(8) 0.0126(8) 0.0022(6) -0.0014(7) 0.0013(6) C24 0.0190(8) 0.0126(8) 0.0168(9) -0.0007(6) -0.0008(7) 0.0031(6) C25 0.0286(10) 0.0148(8) 0.0176(9) 0.0029(7) 0.0012(8) 0.0053(7) C21 0.0114(7) 0.0156(8) 0.0201(9) 0.0011(6) 0.0018(6) 0.0002(6) C13 0.0148(8) 0.0138(8) 0.0204(9) -0.0010(6) 0.0045(7) 0.0028(6) C16 0.0147(7) 0.0132(7) 0.0186(9) 0.0012(6) -0.0015(6) 0.0019(6) C7 0.0168(8) 0.0181(9) 0.0236(10) 0.0027(7) -0.0025(7) -0.0002(7) C14 0.0151(8) 0.0134(8) 0.0254(10) 0.0025(7) 0.0037(7) 0.0047(6) C36 0.0194(8) 0.0196(9) 0.0192(9) 0.0067(7) 0.0017(7) 0.0050(7) C35 0.0246(9) 0.0184(9) 0.0234(10) 0.0046(7) 0.0043(8) 0.0087(7) C38 0.0247(9) 0.0173(8) 0.0130(8) -0.0015(6) 0.0031(7) 0.0040(7) C27 0.0180(8) 0.0209(9) 0.0215(10) 0.0042(7) 0.0029(7) -0.0010(7) C28 0.0228(9) 0.0169(9) 0.0191(9) 0.0008(7) -0.0037(7) 0.0042(7) C45 0.0295(11) 0.0282(11) 0.0163(9) 0.0042(8) 0.0015(8) 0.0010(9) C34 0.0227(9) 0.0142(8) 0.0204(9) 0.0004(7) 0.0040(7) 0.0049(7) C33 0.0168(8) 0.0141(8) 0.0165(8) -0.0001(6) 0.0019(6) 0.0026(6) C39 0.0268(10) 0.0229(10) 0.0201(10) 0.0014(8) 0.0066(8) 0.0004(8) C17 0.0231(9) 0.0161(8) 0.0193(9) 0.0029(7) -0.0029(7) 0.0012(7) C26 0.0244(10) 0.0191(9) 0.0227(10) 0.0055(7) 0.0056(8) -0.0007(7) C46 0.0262(10) 0.0237(10) 0.0251(10) 0.0102(8) 0.0073(8) -0.0003(8) C4 0.0253(9) 0.0123(8) 0.0180(9) -0.0018(6) 0.0004(7) 0.0050(7) C50 0.0230(10) 0.0193(9) 0.0295(11) -0.0039(8) 0.0005(8) -0.0010(8) C18 0.0319(11) 0.0215(10) 0.0218(10) 0.0056(8) -0.0056(8) -0.0008(8) C19 0.0286(11) 0.0235(10) 0.0299(11) 0.0137(8) -0.0078(9) 0.0035(8) C40 0.0298(11) 0.0241(10) 0.0175(9) 0.0034(7) -0.0021(8) 0.0026(8) C8 0.0202(9) 0.0238(10) 0.0281(11) 0.0065(8) -0.0074(8) -0.0048(8) C55 0.0208(9) 0.0237(10) 0.0341(12) -0.0021(9) 0.0067(9) -0.0007(8) C53 0.0453(15) 0.0310(13) 0.0336(14) 0.0031(10) 0.0003(11) -0.0008(11) C41 0.0508(15) 0.0251(11) 0.0185(10) -0.0009(8) 0.0083(10) 0.0140(10) C30 0.0203(9) 0.0274(11) 0.0320(12) 0.0004(9) -0.0018(8) 0.0090(8) C54 0.0246(11) 0.0240(11) 0.0442(14) 0.0004(10) -0.0015(10) 0.0006(8) C31 0.0352(12) 0.0277(11) 0.0267(11) 0.0071(9) -0.0103(9) 0.0046(9) C49 0.0420(15) 0.0333(13) 0.0435(16) 0.0035(11) -0.0065(12) 0.0034(11) C3 0.0194(8) 0.0131(8) 0.0201(9) -0.0003(6) 0.0009(7) 0.0060(6) C10 0.0306(10) 0.0153(8) 0.0180(9) -0.0012(7) -0.0003(8) -0.0012(7) C44 0.0137(8) 0.0207(9) 0.0270(10) 0.0051(7) 0.0025(7) -0.0005(7) C43 0.0286(10) 0.0234(10) 0.0181(9) 0.0018(8) 0.0090(8) 0.0091(8) C48 0.0159(9) 0.0254(10) 0.0389(13) -0.0018(9) 0.0029(8) 0.0095(8) C9 0.0320(11) 0.0183(9) 0.0236(10) 0.0023(8) -0.0073(9) -0.0076(8) C15 0.0151(8) 0.0145(8) 0.0241(10) 0.0040(7) -0.0003(7) 0.0029(6) C20 0.0225(9) 0.0177(9) 0.0329(12) 0.0085(8) -0.0019(8) 0.0045(7) _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 Nb1 N2 1.8125(15) . ? Nb1 N5 1.9756(16) . ? Nb1 O2 2.0051(13) . ? Nb1 O1 2.0402(14) . ? Nb1 N1 2.3528(16) . ? Nb1 N3 2.4272(17) . ? O2 C32 1.348(2) . ? N3 C43 1.476(3) . ? N3 C44 1.491(2) . ? N3 C42 1.521(2) . ? O1 C23 1.319(2) . ? N2 C2 1.365(2) . ? N1 C21 1.287(3) . ? N1 C12 1.427(2) . ? N5 C48 1.456(3) . ? N5 C47 1.466(3) . ? C37 C36 1.391(3) . ? C37 C32 1.404(3) . ? C37 C42 1.532(2) . ? N4 C42 1.437(2) . ? N4 C46 1.444(3) . ? N4 C45 1.447(3) . ? C11 C12 1.386(3) . ? C11 C16 1.446(3) . ? C11 C1 1.487(2) . ? C32 C33 1.420(2) . ? C22 C27 1.405(3) . ? C22 C23 1.418(3) . ? C22 C21 1.444(3) . ? C1 C2 1.401(2) . ? C1 C6 1.438(2) . ? C23 C24 1.430(3) . ? C42 H42 1.0000 . ? C2 C3 1.434(2) . ? C29 C28 1.536(3) . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C52 C53 1.382(4) . ? C52 C51 1.388(4) . ? C52 H52 0.9500 . ? C51 C50 1.390(4) . ? C51 H51 0.9500 . ? C6 C7 1.424(3) . ? C6 C5 1.426(3) . ? C12 C13 1.423(3) . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C5 C4 1.414(3) . ? C5 C10 1.417(3) . ? C24 C25 1.385(3) . ? C24 C28 1.541(3) . ? C25 C26 1.394(3) . ? C25 H25 0.9500 . ? C21 H21 0.9500 . ? C13 C14 1.364(3) . ? C13 H13 0.9500 . ? C16 C17 1.416(3) . ? C16 C15 1.428(3) . ? C7 C8 1.376(3) . ? C7 H7 0.9500 . ? C14 C15 1.413(3) . ? C14 H14 0.9500 . ? C36 C35 1.382(3) . ? C36 H36 0.9500 . ? C35 C34 1.391(3) . ? C35 H35 0.9500 . ? C38 C41 1.535(3) . ? C38 C39 1.535(3) . ? C38 C40 1.536(3) . ? C38 C33 1.536(3) . ? C27 C26 1.373(3) . ? C27 H27 0.9500 . ? C28 C31 1.531(3) . ? C28 C30 1.538(3) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C34 C33 1.395(3) . ? C34 H34 0.9500 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C17 C18 1.367(3) . ? C17 H17 0.9500 . ? C26 H26 0.9500 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C4 C3 1.353(3) . ? C4 H4 0.9500 . ? C50 C55 1.390(3) . ? C50 C49 1.502(4) . ? C18 C19 1.412(3) . ? C18 H18 0.9500 . ? C19 C20 1.363(3) . ? C19 H19 0.9500 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C8 C9 1.407(3) . ? C8 H8 0.9500 . ? C55 C54 1.383(4) . ? C55 H55 0.9500 . ? C53 C54 1.383(4) . ? C53 H53 0.9500 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C54 H54 0.9500 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C3 H3 0.9500 . ? C10 C9 1.359(3) . ? C10 H10 0.9500 . ? C44 H44A 0.9800 . ? C44 H44B 0.9800 . ? C44 H44C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C9 H9 0.9500 . ? C15 C20 1.410(3) . ? C20 H20 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Nb1 N5 99.92(7) . . ? N2 Nb1 O2 145.03(6) . . ? N5 Nb1 O2 108.26(6) . . ? N2 Nb1 O1 109.48(7) . . ? N5 Nb1 O1 88.27(7) . . ? O2 Nb1 O1 91.96(6) . . ? N2 Nb1 N1 75.37(6) . . ? N5 Nb1 N1 160.26(6) . . ? O2 Nb1 N1 84.08(6) . . ? O1 Nb1 N1 75.68(6) . . ? N2 Nb1 N3 88.43(7) . . ? N5 Nb1 N3 85.36(7) . . ? O2 Nb1 N3 73.99(6) . . ? O1 Nb1 N3 161.80(5) . . ? N1 Nb1 N3 113.33(6) . . ? C32 O2 Nb1 144.63(12) . . ? C43 N3 C44 106.99(16) . . ? C43 N3 C42 109.15(15) . . ? C44 N3 C42 111.45(15) . . ? C43 N3 Nb1 109.13(12) . . ? C44 N3 Nb1 108.88(12) . . ? C42 N3 Nb1 111.12(11) . . ? C23 O1 Nb1 143.85(13) . . ? C2 N2 Nb1 156.90(13) . . ? C21 N1 C12 118.40(16) . . ? C21 N1 Nb1 128.88(13) . . ? C12 N1 Nb1 111.55(11) . . ? C48 N5 C47 110.46(17) . . ? C48 N5 Nb1 128.50(14) . . ? C47 N5 Nb1 120.70(14) . . ? C36 C37 C32 118.90(16) . . ? C36 C37 C42 119.28(17) . . ? C32 C37 C42 121.49(16) . . ? C42 N4 C46 123.00(17) . . ? C42 N4 C45 119.37(16) . . ? C46 N4 C45 113.61(17) . . ? C12 C11 C16 117.60(16) . . ? C12 C11 C1 122.43(17) . . ? C16 C11 C1 119.95(16) . . ? O2 C32 C37 120.06(15) . . ? O2 C32 C33 118.97(16) . . ? C37 C32 C33 120.97(16) . . ? C27 C22 C23 121.05(18) . . ? C27 C22 C21 116.92(17) . . ? C23 C22 C21 121.96(17) . . ? C2 C1 C6 118.94(16) . . ? C2 C1 C11 120.73(16) . . ? C6 C1 C11 120.32(16) . . ? O1 C23 C22 120.94(17) . . ? O1 C23 C24 120.69(17) . . ? C22 C23 C24 118.37(17) . . ? N4 C42 N3 116.38(15) . . ? N4 C42 C37 111.46(15) . . ? N3 C42 C37 112.50(14) . . ? N4 C42 H42 105.1 . . ? N3 C42 H42 105.1 . . ? C37 C42 H42 105.1 . . ? N2 C2 C1 123.58(16) . . ? N2 C2 C3 117.07(16) . . ? C1 C2 C3 119.34(16) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C53 C52 C51 120.3(3) . . ? C53 C52 H52 119.9 . . ? C51 C52 H52 119.9 . . ? C52 C51 C50 120.3(3) . . ? C52 C51 H51 119.8 . . ? C50 C51 H51 119.8 . . ? C7 C6 C5 117.28(17) . . ? C7 C6 C1 122.81(17) . . ? C5 C6 C1 119.88(17) . . ? C11 C12 C13 122.27(17) . . ? C11 C12 N1 122.17(16) . . ? C13 C12 N1 115.45(17) . . ? N5 C47 H47A 109.5 . . ? N5 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? N5 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C4 C5 C10 121.52(18) . . ? C4 C5 C6 118.91(17) . . ? C10 C5 C6 119.56(18) . . ? C25 C24 C23 117.97(18) . . ? C25 C24 C28 121.56(18) . . ? C23 C24 C28 120.48(17) . . ? C24 C25 C26 123.46(19) . . ? C24 C25 H25 118.3 . . ? C26 C25 H25 118.3 . . ? N1 C21 C22 125.80(17) . . ? N1 C21 H21 117.1 . . ? C22 C21 H21 117.1 . . ? C14 C13 C12 119.78(17) . . ? C14 C13 H13 120.1 . . ? C12 C13 H13 120.1 . . ? C17 C16 C15 117.61(18) . . ? C17 C16 C11 122.64(17) . . ? C15 C16 C11 119.68(17) . . ? C8 C7 C6 121.16(19) . . ? C8 C7 H7 119.4 . . ? C6 C7 H7 119.4 . . ? C13 C14 C15 120.93(16) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C35 C36 C37 121.29(19) . . ? C35 C36 H36 119.4 . . ? C37 C36 H36 119.4 . . ? C36 C35 C34 119.30(18) . . ? C36 C35 H35 120.4 . . ? C34 C35 H35 120.4 . . ? C41 C38 C39 107.60(18) . . ? C41 C38 C40 107.42(18) . . ? C39 C38 C40 110.05(18) . . ? C41 C38 C33 111.27(17) . . ? C39 C38 C33 111.13(16) . . ? C40 C38 C33 109.30(16) . . ? C26 C27 C22 120.15(19) . . ? C26 C27 H27 119.9 . . ? C22 C27 H27 119.9 . . ? C31 C28 C29 107.00(17) . . ? C31 C28 C30 108.12(18) . . ? C29 C28 C30 110.43(19) . . ? C31 C28 C24 111.99(18) . . ? C29 C28 C24 109.30(16) . . ? C30 C28 C24 109.96(16) . . ? N4 C45 H45A 109.5 . . ? N4 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? N4 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C35 C34 C33 122.05(17) . . ? C35 C34 H34 119.0 . . ? C33 C34 H34 119.0 . . ? C34 C33 C32 117.42(17) . . ? C34 C33 C38 121.05(16) . . ? C32 C33 C38 121.52(16) . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C18 C17 C16 121.69(19) . . ? C18 C17 H17 119.2 . . ? C16 C17 H17 119.2 . . ? C27 C26 C25 118.95(19) . . ? C27 C26 H26 120.5 . . ? C25 C26 H26 120.5 . . ? N4 C46 H46A 109.5 . . ? N4 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? N4 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C3 C4 C5 121.07(17) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C51 C50 C55 118.9(2) . . ? C51 C50 C49 120.2(2) . . ? C55 C50 C49 120.9(2) . . ? C17 C18 C19 120.3(2) . . ? C17 C18 H18 119.9 . . ? C19 C18 H18 119.9 . . ? C20 C19 C18 119.6(2) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C38 C40 H40A 109.5 . . ? C38 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C38 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C7 C8 C9 120.9(2) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C54 C55 C50 120.7(2) . . ? C54 C55 H55 119.7 . . ? C50 C55 H55 119.7 . . ? C52 C53 C54 119.7(3) . . ? C52 C53 H53 120.1 . . ? C54 C53 H53 120.1 . . ? C38 C41 H41A 109.5 . . ? C38 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C38 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C55 C54 C53 120.1(2) . . ? C55 C54 H54 120.0 . . ? C53 C54 H54 120.0 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C50 C49 H49A 109.5 . . ? C50 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C50 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C4 C3 C2 121.43(18) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C9 C10 C5 121.66(19) . . ? C9 C10 H10 119.2 . . ? C5 C10 H10 119.2 . . ? N3 C44 H44A 109.5 . . ? N3 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? N3 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? N3 C43 H43A 109.5 . . ? N3 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? N3 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? N5 C48 H48A 109.5 . . ? N5 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? N5 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C10 C9 C8 119.35(19) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C20 C15 C14 121.17(18) . . ? C20 C15 C16 119.25(19) . . ? C14 C15 C16 119.48(17) . . ? C19 C20 C15 121.5(2) . . ? C19 C20 H20 119.2 . . ? C15 C20 H20 119.2 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Nb1 O2 C32 -28.8(3) . . . . ? N5 Nb1 O2 C32 113.3(2) . . . . ? O1 Nb1 O2 C32 -157.9(2) . . . . ? N1 Nb1 O2 C32 -82.5(2) . . . . ? N3 Nb1 O2 C32 33.8(2) . . . . ? N2 Nb1 N3 C43 -24.37(13) . . . . ? N5 Nb1 N3 C43 75.72(13) . . . . ? O2 Nb1 N3 C43 -173.76(14) . . . . ? O1 Nb1 N3 C43 145.62(17) . . . . ? N1 Nb1 N3 C43 -97.68(13) . . . . ? N2 Nb1 N3 C44 -140.83(12) . . . . ? N5 Nb1 N3 C44 -40.74(12) . . . . ? O2 Nb1 N3 C44 69.77(12) . . . . ? O1 Nb1 N3 C44 29.2(2) . . . . ? N1 Nb1 N3 C44 145.85(11) . . . . ? N2 Nb1 N3 C42 96.05(12) . . . . ? N5 Nb1 N3 C42 -163.86(12) . . . . ? O2 Nb1 N3 C42 -53.35(11) . . . . ? O1 Nb1 N3 C42 -94.0(2) . . . . ? N1 Nb1 N3 C42 22.73(13) . . . . ? N2 Nb1 O1 C23 -55.3(2) . . . . ? N5 Nb1 O1 C23 -155.2(2) . . . . ? O2 Nb1 O1 C23 96.6(2) . . . . ? N1 Nb1 O1 C23 13.2(2) . . . . ? N3 Nb1 O1 C23 135.3(2) . . . . ? N5 Nb1 N2 C2 159.0(4) . . . . ? O2 Nb1 N2 C2 -57.3(4) . . . . ? O1 Nb1 N2 C2 67.3(4) . . . . ? N1 Nb1 N2 C2 -1.3(4) . . . . ? N3 Nb1 N2 C2 -116.0(4) . . . . ? N2 Nb1 N1 C21 96.85(17) . . . . ? N5 Nb1 N1 C21 18.4(3) . . . . ? O2 Nb1 N1 C21 -111.68(16) . . . . ? O1 Nb1 N1 C21 -18.13(16) . . . . ? N3 Nb1 N1 C21 178.61(15) . . . . ? N2 Nb1 N1 C12 -70.35(12) . . . . ? N5 Nb1 N1 C12 -148.80(18) . . . . ? O2 Nb1 N1 C12 81.12(12) . . . . ? O1 Nb1 N1 C12 174.67(13) . . . . ? N3 Nb1 N1 C12 11.40(13) . . . . ? N2 Nb1 N5 C48 -1.4(2) . . . . ? O2 Nb1 N5 C48 -160.45(18) . . . . ? O1 Nb1 N5 C48 108.05(19) . . . . ? N1 Nb1 N5 C48 72.8(3) . . . . ? N3 Nb1 N5 C48 -89.01(19) . . . . ? N2 Nb1 N5 C47 -174.06(17) . . . . ? O2 Nb1 N5 C47 26.91(18) . . . . ? O1 Nb1 N5 C47 -64.58(17) . . . . ? N1 Nb1 N5 C47 -99.8(2) . . . . ? N3 Nb1 N5 C47 98.35(17) . . . . ? Nb1 O2 C32 C37 -14.7(3) . . . . ? Nb1 O2 C32 C33 165.19(15) . . . . ? C36 C37 C32 O2 179.34(17) . . . . ? C42 C37 C32 O2 5.9(3) . . . . ? C36 C37 C32 C33 -0.5(3) . . . . ? C42 C37 C32 C33 -173.90(16) . . . . ? C12 C11 C1 C2 -52.9(3) . . . . ? C16 C11 C1 C2 125.32(19) . . . . ? C12 C11 C1 C6 128.2(2) . . . . ? C16 C11 C1 C6 -53.5(2) . . . . ? Nb1 O1 C23 C22 -5.3(3) . . . . ? Nb1 O1 C23 C24 175.16(14) . . . . ? C27 C22 C23 O1 177.77(17) . . . . ? C21 C22 C23 O1 -5.2(3) . . . . ? C27 C22 C23 C24 -2.7(3) . . . . ? C21 C22 C23 C24 174.33(16) . . . . ? C46 N4 C42 N3 -65.1(2) . . . . ? C45 N4 C42 N3 90.9(2) . . . . ? C46 N4 C42 C37 65.8(2) . . . . ? C45 N4 C42 C37 -138.25(18) . . . . ? C43 N3 C42 N4 -40.6(2) . . . . ? C44 N3 C42 N4 77.33(19) . . . . ? Nb1 N3 C42 N4 -161.03(12) . . . . ? C43 N3 C42 C37 -170.99(16) . . . . ? C44 N3 C42 C37 -53.0(2) . . . . ? Nb1 N3 C42 C37 68.61(16) . . . . ? C36 C37 C42 N4 13.4(2) . . . . ? C32 C37 C42 N4 -173.20(16) . . . . ? C36 C37 C42 N3 146.24(17) . . . . ? C32 C37 C42 N3 -40.4(2) . . . . ? Nb1 N2 C2 C1 36.5(5) . . . . ? Nb1 N2 C2 C3 -142.1(3) . . . . ? C6 C1 C2 N2 -171.61(18) . . . . ? C11 C1 C2 N2 9.5(3) . . . . ? C6 C1 C2 C3 6.9(3) . . . . ? C11 C1 C2 C3 -171.92(17) . . . . ? C53 C52 C51 C50 -0.7(4) . . . . ? C2 C1 C6 C7 170.56(18) . . . . ? C11 C1 C6 C7 -10.6(3) . . . . ? C2 C1 C6 C5 -7.2(3) . . . . ? C11 C1 C6 C5 171.62(17) . . . . ? C16 C11 C12 C13 4.0(3) . . . . ? C1 C11 C12 C13 -177.69(16) . . . . ? C16 C11 C12 N1 -171.98(16) . . . . ? C1 C11 C12 N1 6.3(3) . . . . ? C21 N1 C12 C11 -91.5(2) . . . . ? Nb1 N1 C12 C11 77.24(19) . . . . ? C21 N1 C12 C13 92.3(2) . . . . ? Nb1 N1 C12 C13 -99.03(15) . . . . ? C7 C6 C5 C4 -175.32(18) . . . . ? C1 C6 C5 C4 2.6(3) . . . . ? C7 C6 C5 C10 3.7(3) . . . . ? C1 C6 C5 C10 -178.40(18) . . . . ? O1 C23 C24 C25 -178.96(17) . . . . ? C22 C23 C24 C25 1.5(3) . . . . ? O1 C23 C24 C28 1.2(3) . . . . ? C22 C23 C24 C28 -178.36(16) . . . . ? C23 C24 C25 C26 0.6(3) . . . . ? C28 C24 C25 C26 -179.53(18) . . . . ? C12 N1 C21 C22 -175.53(17) . . . . ? Nb1 N1 C21 C22 18.0(3) . . . . ? C27 C22 C21 N1 174.18(18) . . . . ? C23 C22 C21 N1 -2.9(3) . . . . ? C11 C12 C13 C14 0.4(3) . . . . ? N1 C12 C13 C14 176.65(17) . . . . ? C12 C11 C16 C17 170.96(18) . . . . ? C1 C11 C16 C17 -7.4(3) . . . . ? C12 C11 C16 C15 -5.8(3) . . . . ? C1 C11 C16 C15 175.84(17) . . . . ? C5 C6 C7 C8 -2.2(3) . . . . ? C1 C6 C7 C8 179.9(2) . . . . ? C12 C13 C14 C15 -3.1(3) . . . . ? C32 C37 C36 C35 2.3(3) . . . . ? C42 C37 C36 C35 175.83(18) . . . . ? C37 C36 C35 C34 -1.9(3) . . . . ? C23 C22 C27 C26 1.7(3) . . . . ? C21 C22 C27 C26 -175.41(18) . . . . ? C25 C24 C28 C31 -2.1(3) . . . . ? C23 C24 C28 C31 177.78(17) . . . . ? C25 C24 C28 C29 -120.5(2) . . . . ? C23 C24 C28 C29 59.4(2) . . . . ? C25 C24 C28 C30 118.2(2) . . . . ? C23 C24 C28 C30 -62.0(2) . . . . ? C36 C35 C34 C33 -0.3(3) . . . . ? C35 C34 C33 C32 2.0(3) . . . . ? C35 C34 C33 C38 -177.78(19) . . . . ? O2 C32 C33 C34 178.59(17) . . . . ? C37 C32 C33 C34 -1.6(3) . . . . ? O2 C32 C33 C38 -1.6(3) . . . . ? C37 C32 C33 C38 178.21(17) . . . . ? C41 C38 C33 C34 3.6(3) . . . . ? C39 C38 C33 C34 123.5(2) . . . . ? C40 C38 C33 C34 -114.9(2) . . . . ? C41 C38 C33 C32 -176.19(19) . . . . ? C39 C38 C33 C32 -56.3(2) . . . . ? C40 C38 C33 C32 65.4(2) . . . . ? C15 C16 C17 C18 -1.4(3) . . . . ? C11 C16 C17 C18 -178.24(19) . . . . ? C22 C27 C26 C25 0.4(3) . . . . ? C24 C25 C26 C27 -1.6(3) . . . . ? C10 C5 C4 C3 -176.6(2) . . . . ? C6 C5 C4 C3 2.4(3) . . . . ? C52 C51 C50 C55 0.3(3) . . . . ? C52 C51 C50 C49 -178.6(2) . . . . ? C16 C17 C18 C19 -1.0(3) . . . . ? C17 C18 C19 C20 1.8(3) . . . . ? C6 C7 C8 C9 -0.5(3) . . . . ? C51 C50 C55 C54 0.2(3) . . . . ? C49 C50 C55 C54 179.1(2) . . . . ? C51 C52 C53 C54 0.6(4) . . . . ? C50 C55 C54 C53 -0.3(3) . . . . ? C52 C53 C54 C55 -0.1(4) . . . . ? C5 C4 C3 C2 -2.7(3) . . . . ? N2 C2 C3 C4 176.58(19) . . . . ? C1 C2 C3 C4 -2.0(3) . . . . ? C4 C5 C10 C9 176.4(2) . . . . ? C6 C5 C10 C9 -2.6(3) . . . . ? C5 C10 C9 C8 -0.1(3) . . . . ? C7 C8 C9 C10 1.7(3) . . . . ? C13 C14 C15 C20 -175.27(19) . . . . ? C13 C14 C15 C16 1.1(3) . . . . ? C17 C16 C15 C20 2.9(3) . . . . ? C11 C16 C15 C20 179.86(18) . . . . ? C17 C16 C15 C14 -173.58(18) . . . . ? C11 C16 C15 C14 3.4(3) . . . . ? C18 C19 C20 C15 -0.3(3) . . . . ? C14 C15 C20 C19 174.3(2) . . . . ? C16 C15 C20 C19 -2.1(3) . . . . ? _diffrn_measured_fraction_theta_max 0.897 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.519 _refine_diff_density_min -1.052 _refine_diff_density_rms 0.082 # Attachment '- compound 27.cif' data_compound27 _database_code_depnum_ccdc_archive 'CCDC 791871' #TrackingRef '- compound 27.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C89 H94 N6 O2 V' _chemical_formula_sum 'C89 H94 N6 O2 V' _chemical_formula_weight 1330.64 _chemical_absolute_configuration rmad 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' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 16.237(5) _cell_length_b 10.878(3) _cell_length_c 21.013(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.074(6) _cell_angle_gamma 90.00 _cell_volume 3674.5(18) _cell_formula_units_Z 2 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 12041 _cell_measurement_theta_min 1.7 _cell_measurement_theta_max 27.9 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.203 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1418 _exptl_absorpt_coefficient_mu 0.189 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9597 _exptl_absorpt_correction_T_max 0.9705 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator confocal _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 7.31 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 45257 _diffrn_reflns_av_R_equivalents 0.0449 _diffrn_reflns_av_sigmaI/netI 0.0663 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.71 _diffrn_reflns_theta_max 27.87 _reflns_number_total 17377 _reflns_number_gt 15026 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.7.0' _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^)+(0.0718P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0333(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.004(15) _refine_ls_number_reflns 17377 _refine_ls_number_parameters 901 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0629 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1330 _refine_ls_wR_factor_gt 0.1265 _refine_ls_goodness_of_fit_ref 1.044 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group V V 0.69393(2) 0.38091(4) 0.701391(16) 0.02195(10) Uani 1 1 d . . . O1 O 0.80629(9) 0.29273(15) 0.68213(7) 0.0239(3) Uani 1 1 d . . . O2 O 0.77457(9) 0.52466(15) 0.74356(7) 0.0234(3) Uani 1 1 d . . . N1 N 0.73754(11) 0.42255(17) 0.61515(8) 0.0216(4) Uani 1 1 d . . . N2 N 0.58244(11) 0.32765(18) 0.49714(9) 0.0257(4) Uani 1 1 d . . . N3 N 0.73403(10) 0.37414(19) 0.80024(8) 0.0225(4) Uani 1 1 d . . . N4 N 0.54105(13) 0.3907(3) 0.85999(11) 0.0417(5) Uani 1 1 d . . . N5 N 0.63492(12) 0.2324(2) 0.69354(9) 0.0277(4) Uani 1 1 d . . . N6 N 0.60355(11) 0.48832(19) 0.69040(9) 0.0270(4) Uani 1 1 d . . . C1 C 0.71083(12) 0.5125(2) 0.50483(10) 0.0201(4) Uani 1 1 d . . . C2 C 0.72457(12) 0.5225(2) 0.57133(10) 0.0197(4) Uani 1 1 d . . . C3 C 0.72202(13) 0.6402(2) 0.60145(11) 0.0248(5) Uani 1 1 d . . . H3 H 0.7313 0.6454 0.6470 0.030 Uiso 1 1 calc R . . C4 C 0.70657(13) 0.7448(2) 0.56626(12) 0.0265(5) Uani 1 1 d . . . H4 H 0.7058 0.8218 0.5875 0.032 Uiso 1 1 calc R . . C5 C 0.69156(13) 0.7400(2) 0.49808(12) 0.0249(5) Uani 1 1 d . . . C6 C 0.69302(12) 0.6230(2) 0.46740(11) 0.0230(5) Uani 1 1 d . . . C7 C 0.67608(13) 0.6190(2) 0.39928(11) 0.0270(5) Uani 1 1 d . . . H7 H 0.6742 0.5421 0.3777 0.032 Uiso 1 1 calc R . . C8 C 0.66237(14) 0.7262(2) 0.36416(12) 0.0315(5) Uani 1 1 d . . . H8 H 0.6515 0.7220 0.3186 0.038 Uiso 1 1 calc R . . C9 C 0.66428(14) 0.8414(2) 0.39462(13) 0.0321(6) Uani 1 1 d . . . H9 H 0.6564 0.9144 0.3697 0.039 Uiso 1 1 calc R . . C10 C 0.67756(13) 0.8480(2) 0.46041(12) 0.0299(5) Uani 1 1 d . . . H10 H 0.6774 0.9258 0.4810 0.036 Uiso 1 1 calc R . . C11 C 0.71649(12) 0.3940(2) 0.46989(9) 0.0212(4) Uani 1 1 d . . . C12 C 0.65481(13) 0.3056(2) 0.46664(10) 0.0232(4) Uani 1 1 d . . . C13 C 0.66285(14) 0.1951(2) 0.43174(11) 0.0281(5) Uani 1 1 d . . . H13 H 0.6211 0.1337 0.4307 0.034 Uiso 1 1 calc R . . C14 C 0.72860(15) 0.1756(2) 0.40009(11) 0.0286(5) Uani 1 1 d . . . H14 H 0.7324 0.1007 0.3775 0.034 Uiso 1 1 calc R . . C15 C 0.79211(14) 0.2653(2) 0.40010(11) 0.0256(5) Uani 1 1 d . . . C16 C 0.78645(12) 0.3752(2) 0.43606(9) 0.0219(4) Uani 1 1 d . . . C17 C 0.85099(13) 0.4637(2) 0.43608(11) 0.0257(5) Uani 1 1 d . . . H17 H 0.8495 0.5370 0.4605 0.031 Uiso 1 1 calc R . . C18 C 0.91549(15) 0.4448(2) 0.40132(12) 0.0290(5) Uani 1 1 d . . . H18 H 0.9574 0.5057 0.4015 0.035 Uiso 1 1 calc R . . C19 C 0.92035(15) 0.3366(2) 0.36544(12) 0.0309(5) Uani 1 1 d . . . H19 H 0.9651 0.3248 0.3415 0.037 Uiso 1 1 calc R . . C20 C 0.86041(15) 0.2486(2) 0.36523(12) 0.0304(5) Uani 1 1 d . . . H20 H 0.8643 0.1751 0.3415 0.036 Uiso 1 1 calc R . . C21 C 0.54179(15) 0.2173(2) 0.51744(13) 0.0330(5) Uani 1 1 d . . . H21A H 0.5118 0.1760 0.4797 0.049 Uiso 1 1 calc R . . H21B H 0.5025 0.2404 0.5468 0.049 Uiso 1 1 calc R . . H21C H 0.5838 0.1615 0.5395 0.049 Uiso 1 1 calc R . . C22 C 0.52194(15) 0.4072(2) 0.45958(13) 0.0366(6) Uani 1 1 d . . . H22A H 0.5496 0.4822 0.4478 0.055 Uiso 1 1 calc R . . H22B H 0.4780 0.4287 0.4851 0.055 Uiso 1 1 calc R . . H22C H 0.4975 0.3641 0.4205 0.055 Uiso 1 1 calc R . . C23 C 0.80639(13) 0.3582(2) 0.63139(10) 0.0218(4) Uani 1 1 d . . . C24 C 0.88132(12) 0.3541(2) 0.59703(10) 0.0231(5) Uani 1 1 d . . . C25 C 0.89614(14) 0.2452(2) 0.56433(11) 0.0257(5) Uani 1 1 d . . . C26 C 0.96797(14) 0.2384(2) 0.53534(11) 0.0294(5) Uani 1 1 d . . . H26 H 0.9782 0.1659 0.5125 0.035 Uiso 1 1 calc R . . C27 C 1.02519(14) 0.3338(2) 0.53872(12) 0.0322(5) Uani 1 1 d . . . C28 C 1.01012(14) 0.4393(2) 0.57247(12) 0.0302(5) Uani 1 1 d . . . H28 H 1.0493 0.5046 0.5757 0.036 Uiso 1 1 calc R . . C29 C 0.93837(14) 0.4514(2) 0.60180(11) 0.0261(5) Uani 1 1 d . . . C30 C 0.83755(15) 0.1382(2) 0.56074(12) 0.0307(5) Uani 1 1 d . . . H30A H 0.8427 0.0896 0.5222 0.046 Uiso 1 1 calc R . . H30B H 0.7803 0.1683 0.5586 0.046 Uiso 1 1 calc R . . H30C H 0.8513 0.0867 0.5990 0.046 Uiso 1 1 calc R . . C31 C 1.10295(17) 0.3220(3) 0.50727(16) 0.0469(7) Uani 1 1 d . . . H31A H 1.1165 0.2348 0.5032 0.070 Uiso 1 1 calc R . . H31B H 1.1492 0.3636 0.5337 0.070 Uiso 1 1 calc R . . H31C H 1.0936 0.3598 0.4645 0.070 Uiso 1 1 calc R . . C32 C 0.92601(15) 0.5647(2) 0.64057(13) 0.0331(6) Uani 1 1 d . . . H32A H 0.9803 0.6003 0.6571 0.050 Uiso 1 1 calc R . . H32B H 0.8967 0.5425 0.6767 0.050 Uiso 1 1 calc R . . H32C H 0.8930 0.6249 0.6132 0.050 Uiso 1 1 calc R . . C33 C 0.70971(14) 0.2997(2) 0.90763(11) 0.0264(5) Uani 1 1 d . . . C34 C 0.73853(13) 0.2827(2) 0.84910(11) 0.0243(5) Uani 1 1 d . . . C35 C 0.77171(14) 0.1676(2) 0.83378(12) 0.0283(5) Uani 1 1 d . . . H35 H 0.7883 0.1565 0.7926 0.034 Uiso 1 1 calc R . . C36 C 0.78052(16) 0.0724(2) 0.87634(12) 0.0309(5) Uani 1 1 d . . . H36 H 0.8043 -0.0030 0.8651 0.037 Uiso 1 1 calc R . . C37 C 0.75412(15) 0.0862(2) 0.93753(12) 0.0312(5) Uani 1 1 d . . . C38 C 0.71728(15) 0.1995(2) 0.95286(12) 0.0300(5) Uani 1 1 d . . . C39 C 0.68993(19) 0.2100(3) 1.01376(13) 0.0389(6) Uani 1 1 d . . . H39 H 0.6630 0.2834 1.0242 0.047 Uiso 1 1 calc R . . C40 C 0.7015(2) 0.1170(3) 1.05780(13) 0.0456(7) Uani 1 1 d . . . H40 H 0.6831 0.1270 1.0985 0.055 Uiso 1 1 calc R . . C41 C 0.7401(2) 0.0068(3) 1.04371(14) 0.0490(8) Uani 1 1 d . . . H41 H 0.7489 -0.0566 1.0750 0.059 Uiso 1 1 calc R . . C42 C 0.76512(19) -0.0090(3) 0.98439(13) 0.0393(6) Uani 1 1 d . . . H42 H 0.7901 -0.0843 0.9746 0.047 Uiso 1 1 calc R . . C43 C 0.67575(16) 0.4193(2) 0.92808(11) 0.0305(5) Uani 1 1 d . . . C44 C 0.59569(16) 0.4610(3) 0.90480(13) 0.0370(6) Uani 1 1 d . . . C45 C 0.5684(2) 0.5759(3) 0.92799(16) 0.0488(8) Uani 1 1 d . . . H45 H 0.5149 0.6062 0.9113 0.059 Uiso 1 1 calc R . . C46 C 0.6172(2) 0.6422(3) 0.97310(15) 0.0489(8) Uani 1 1 d . . . H46 H 0.5971 0.7180 0.9873 0.059 Uiso 1 1 calc R . . C47 C 0.6974(2) 0.6010(3) 0.99955(14) 0.0418(7) Uani 1 1 d . . . C48 C 0.72762(17) 0.4893(2) 0.97575(12) 0.0329(6) Uani 1 1 d . . . C49 C 0.80925(18) 0.4516(2) 1.00139(12) 0.0355(6) Uani 1 1 d . . . H49 H 0.8313 0.3785 0.9858 0.043 Uiso 1 1 calc R . . C50 C 0.8568(2) 0.5179(3) 1.04793(13) 0.0453(7) Uani 1 1 d . . . H50 H 0.9112 0.4904 1.0642 0.054 Uiso 1 1 calc R . . C51 C 0.8257(3) 0.6272(3) 1.07216(14) 0.0556(9) Uani 1 1 d . . . H51 H 0.8586 0.6724 1.1051 0.067 Uiso 1 1 calc R . . C52 C 0.7487(3) 0.6669(3) 1.04787(15) 0.0562(9) Uani 1 1 d . . . H52 H 0.7285 0.7412 1.0637 0.067 Uiso 1 1 calc R . . C53 C 0.5149(2) 0.2737(4) 0.88371(17) 0.0568(9) Uani 1 1 d . . . H53A H 0.5638 0.2287 0.9044 0.085 Uiso 1 1 calc R . . H53B H 0.4869 0.2252 0.8477 0.085 Uiso 1 1 calc R . . H53C H 0.4765 0.2881 0.9150 0.085 Uiso 1 1 calc R . . C54 C 0.46901(18) 0.4559(4) 0.82730(17) 0.0591(9) Uani 1 1 d . . . H54A H 0.4264 0.4618 0.8559 0.089 Uiso 1 1 calc R . . H54B H 0.4465 0.4110 0.7883 0.089 Uiso 1 1 calc R . . H54C H 0.4856 0.5386 0.8157 0.089 Uiso 1 1 calc R . . C55 C 0.78481(13) 0.4691(2) 0.79818(10) 0.0236(4) Uani 1 1 d . . . C56 C 0.84997(13) 0.5167(2) 0.84979(10) 0.0226(4) Uani 1 1 d . . . C57 C 0.83640(14) 0.6314(2) 0.87673(11) 0.0261(5) Uani 1 1 d . . . C58 C 0.89986(15) 0.6805(2) 0.92131(12) 0.0311(5) Uani 1 1 d . . . H58 H 0.8910 0.7577 0.9403 0.037 Uiso 1 1 calc R . . C59 C 0.97508(15) 0.6213(3) 0.93890(12) 0.0341(6) Uani 1 1 d . . . C60 C 0.98723(15) 0.5088(3) 0.91036(12) 0.0320(5) Uani 1 1 d . . . H60 H 1.0387 0.4674 0.9216 0.038 Uiso 1 1 calc R . . C61 C 0.92626(14) 0.4545(2) 0.86561(11) 0.0269(5) Uani 1 1 d . . . C62 C 0.75732(15) 0.7011(2) 0.85861(12) 0.0300(5) Uani 1 1 d . . . H62A H 0.7529 0.7658 0.8904 0.045 Uiso 1 1 calc R . . H62B H 0.7100 0.6449 0.8575 0.045 Uiso 1 1 calc R . . H62C H 0.7572 0.7382 0.8161 0.045 Uiso 1 1 calc R . . C63 C 1.04168(18) 0.6767(3) 0.98822(14) 0.0481(7) Uani 1 1 d . . . H63A H 1.0406 0.6365 1.0298 0.072 Uiso 1 1 calc R . . H63B H 1.0312 0.7648 0.9923 0.072 Uiso 1 1 calc R . . H63C H 1.0963 0.6644 0.9745 0.072 Uiso 1 1 calc R . . C64 C 0.94447(15) 0.3354(2) 0.83365(12) 0.0334(6) Uani 1 1 d . . . H64A H 0.9273 0.2662 0.8586 0.050 Uiso 1 1 calc R . . H64B H 1.0043 0.3296 0.8315 0.050 Uiso 1 1 calc R . . H64C H 0.9137 0.3330 0.7901 0.050 Uiso 1 1 calc R . . C65 C 0.55552(18) 0.2151(3) 0.71737(19) 0.0542(9) Uani 1 1 d . . . H65A H 0.5153 0.1786 0.6835 0.081 Uiso 1 1 calc R . . H65B H 0.5346 0.2947 0.7299 0.081 Uiso 1 1 calc R . . H65C H 0.5633 0.1602 0.7547 0.081 Uiso 1 1 calc R . . C66 C 0.66686(16) 0.1129(2) 0.67726(13) 0.0344(6) Uani 1 1 d . . . H66A H 0.6757 0.0612 0.7158 0.052 Uiso 1 1 calc R . . H66B H 0.7197 0.1239 0.6605 0.052 Uiso 1 1 calc R . . H66C H 0.6266 0.0732 0.6445 0.052 Uiso 1 1 calc R . . C67 C 0.53710(17) 0.4763(3) 0.63651(14) 0.0482(8) Uani 1 1 d . . . H67A H 0.4831 0.4808 0.6522 0.072 Uiso 1 1 calc R . . H67B H 0.5421 0.3971 0.6152 0.072 Uiso 1 1 calc R . . H67C H 0.5413 0.5431 0.6058 0.072 Uiso 1 1 calc R . . C68 C 0.59797(17) 0.6072(3) 0.72033(16) 0.0464(7) Uani 1 1 d . . . H68A H 0.6036 0.6721 0.6889 0.070 Uiso 1 1 calc R . . H68B H 0.6426 0.6151 0.7567 0.070 Uiso 1 1 calc R . . H68C H 0.5439 0.6149 0.7357 0.070 Uiso 1 1 calc R . . C69 C 1.1187(3) 0.7765(4) 0.82636(17) 0.0701(11) Uani 1 1 d . . . H69A H 1.1072 0.7004 0.8485 0.105 Uiso 1 1 calc R . . H69B H 1.1487 0.8338 0.8573 0.105 Uiso 1 1 calc R . . H69C H 1.1527 0.7579 0.7925 0.105 Uiso 1 1 calc R . . C70 C 1.0367(2) 0.8347(3) 0.79638(13) 0.0451(7) Uani 1 1 d . . . C71 C 0.9682(2) 0.7608(3) 0.77665(14) 0.0466(7) Uani 1 1 d . . . H71 H 0.9716 0.6749 0.7848 0.056 Uiso 1 1 calc R . . C72 C 0.8954(2) 0.8098(3) 0.74543(15) 0.0518(8) Uani 1 1 d . . . H72 H 0.8494 0.7578 0.7317 0.062 Uiso 1 1 calc R . . C73 C 0.8895(2) 0.9352(4) 0.73409(16) 0.0570(9) Uani 1 1 d . . . H73 H 0.8393 0.9695 0.7126 0.068 Uiso 1 1 calc R . . C74 C 0.9577(3) 1.0111(3) 0.75445(17) 0.0617(10) Uani 1 1 d . . . H74 H 0.9543 1.0972 0.7471 0.074 Uiso 1 1 calc R . . C75 C 1.0304(2) 0.9588(3) 0.78563(16) 0.0521(8) Uani 1 1 d . . . H75 H 1.0768 1.0100 0.7998 0.063 Uiso 1 1 calc R . . C76 C 0.3785(3) 0.7938(5) 0.7450(2) 0.0862(14) Uani 1 1 d . . . H76A H 0.3933 0.8271 0.7047 0.129 Uiso 1 1 calc R . . H76B H 0.3211 0.8166 0.7491 0.129 Uiso 1 1 calc R . . H76C H 0.3836 0.7040 0.7447 0.129 Uiso 1 1 calc R . . C77 C 0.4353(2) 0.8445(3) 0.79978(18) 0.0621(9) Uani 1 1 d . . . C78 C 0.5150(2) 0.8772(4) 0.79444(19) 0.0643(9) Uani 1 1 d . . . H78 H 0.5350 0.8669 0.7544 0.077 Uiso 1 1 calc R . . C79 C 0.5681(2) 0.9259(3) 0.8469(2) 0.0627(9) Uani 1 1 d . . . H79 H 0.6242 0.9445 0.8424 0.075 Uiso 1 1 calc R . . C80 C 0.5410(2) 0.9463(4) 0.9027(2) 0.0663(10) Uani 1 1 d . . . H80 H 0.5776 0.9800 0.9376 0.080 Uiso 1 1 calc R . . C81 C 0.4589(2) 0.9187(3) 0.91041(17) 0.0610(9) Uani 1 1 d . . . H81 H 0.4392 0.9337 0.9502 0.073 Uiso 1 1 calc R . . C82 C 0.4068(2) 0.8690(4) 0.85907(16) 0.0606(9) Uani 1 1 d . . . H82 H 0.3507 0.8511 0.8638 0.073 Uiso 1 1 calc R . . C83 C 0.2712(4) 0.0869(6) 0.7783(3) 0.128(3) Uani 1 1 d . . . H83A H 0.2781 0.0457 0.7379 0.193 Uiso 1 1 calc R . . H83B H 0.2419 0.0322 0.8046 0.193 Uiso 1 1 calc R . . H83C H 0.3261 0.1073 0.8017 0.193 Uiso 1 1 calc R . . C84 C 0.2225(2) 0.2009(4) 0.76429(18) 0.0612(9) Uani 1 1 d . . . C85 C 0.1489(3) 0.2025(4) 0.72376(18) 0.0751(12) Uani 1 1 d . . . H85 H 0.1291 0.1293 0.7022 0.090 Uiso 1 1 calc R . . C86 C 0.1033(3) 0.3084(6) 0.7138(2) 0.0897(16) Uani 1 1 d . . . H86 H 0.0506 0.3056 0.6877 0.108 Uiso 1 1 calc R . . C87 C 0.1307(3) 0.4157(5) 0.7399(2) 0.0860(14) Uani 1 1 d . . . H87 H 0.0985 0.4884 0.7317 0.103 Uiso 1 1 calc R . . C88 C 0.2056(3) 0.4185(4) 0.77824(19) 0.0779(12) Uani 1 1 d . . . H88 H 0.2265 0.4945 0.7960 0.093 Uiso 1 1 calc R . . C89 C 0.2525(2) 0.3102(4) 0.79203(16) 0.0631(10) Uani 1 1 d . . . H89 H 0.3039 0.3123 0.8199 0.076 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 V 0.01917(16) 0.02379(19) 0.02229(18) 0.00215(15) 0.00076(12) -0.00163(15) O1 0.0248(7) 0.0210(8) 0.0249(8) 0.0029(6) 0.0002(6) 0.0002(6) O2 0.0254(8) 0.0214(8) 0.0229(8) 0.0027(6) 0.0012(6) -0.0020(6) N1 0.0186(8) 0.0232(9) 0.0226(9) 0.0020(7) 0.0016(6) 0.0005(7) N2 0.0226(9) 0.0239(10) 0.0309(10) 0.0006(8) 0.0041(7) -0.0032(8) N3 0.0225(8) 0.0239(9) 0.0213(8) 0.0040(8) 0.0032(6) -0.0015(8) N4 0.0300(10) 0.0557(15) 0.0412(12) 0.0135(12) 0.0108(9) 0.0027(11) N5 0.0225(9) 0.0312(11) 0.0285(10) 0.0035(9) 0.0003(7) -0.0037(8) N6 0.0221(9) 0.0330(12) 0.0255(10) 0.0002(8) 0.0023(7) -0.0018(8) C1 0.0153(9) 0.0178(10) 0.0275(11) 0.0030(9) 0.0046(8) 0.0012(8) C2 0.0150(9) 0.0168(10) 0.0275(11) 0.0029(8) 0.0036(8) 0.0002(8) C3 0.0215(10) 0.0255(12) 0.0275(11) -0.0033(9) 0.0036(8) 0.0010(9) C4 0.0235(11) 0.0202(11) 0.0358(13) -0.0036(9) 0.0039(9) 0.0008(9) C5 0.0169(10) 0.0202(11) 0.0382(13) 0.0032(9) 0.0059(8) 0.0007(8) C6 0.0148(9) 0.0236(11) 0.0306(12) 0.0038(9) 0.0030(8) 0.0009(8) C7 0.0237(11) 0.0284(12) 0.0287(12) 0.0081(10) 0.0028(9) 0.0018(9) C8 0.0226(11) 0.0382(14) 0.0342(13) 0.0142(11) 0.0054(9) 0.0048(10) C9 0.0217(11) 0.0274(13) 0.0475(15) 0.0146(11) 0.0054(10) 0.0032(9) C10 0.0204(10) 0.0217(12) 0.0485(15) 0.0075(10) 0.0078(9) 0.0037(8) C11 0.0231(9) 0.0212(11) 0.0183(9) 0.0035(9) -0.0003(7) 0.0021(9) C12 0.0226(10) 0.0210(11) 0.0255(11) 0.0027(9) 0.0019(8) 0.0011(8) C13 0.0287(11) 0.0231(12) 0.0313(12) -0.0015(10) -0.0002(9) -0.0039(9) C14 0.0343(12) 0.0215(12) 0.0290(12) -0.0022(9) 0.0004(9) 0.0011(10) C15 0.0270(11) 0.0253(12) 0.0243(11) 0.0019(9) 0.0023(8) 0.0034(9) C16 0.0221(9) 0.0214(10) 0.0215(10) 0.0048(9) 0.0001(7) 0.0014(9) C17 0.0248(11) 0.0213(11) 0.0306(12) 0.0011(9) 0.0028(9) 0.0020(9) C18 0.0292(12) 0.0287(13) 0.0299(12) 0.0038(10) 0.0072(9) 0.0028(10) C19 0.0304(12) 0.0345(13) 0.0292(12) 0.0030(10) 0.0095(9) 0.0066(10) C20 0.0331(12) 0.0288(13) 0.0301(13) -0.0005(10) 0.0073(10) 0.0098(10) C21 0.0311(12) 0.0307(14) 0.0375(13) 0.0015(11) 0.0064(10) -0.0074(10) C22 0.0267(12) 0.0334(15) 0.0508(15) 0.0072(12) 0.0090(10) 0.0022(10) C23 0.0222(10) 0.0211(12) 0.0210(10) 0.0004(8) -0.0011(7) -0.0016(8) C24 0.0187(9) 0.0257(12) 0.0243(11) 0.0041(9) 0.0006(8) 0.0026(8) C25 0.0261(11) 0.0236(11) 0.0262(12) 0.0029(9) -0.0001(9) 0.0056(9) C26 0.0277(11) 0.0287(13) 0.0317(13) 0.0004(10) 0.0039(9) 0.0096(10) C27 0.0242(11) 0.0349(13) 0.0374(13) 0.0057(11) 0.0039(9) 0.0068(10) C28 0.0233(11) 0.0283(13) 0.0391(14) 0.0031(11) 0.0041(9) -0.0024(9) C29 0.0246(11) 0.0246(12) 0.0284(12) 0.0005(9) 0.0012(9) 0.0001(9) C30 0.0331(12) 0.0238(12) 0.0355(13) -0.0002(10) 0.0055(10) 0.0037(10) C31 0.0353(14) 0.0409(17) 0.070(2) 0.0019(15) 0.0256(13) 0.0091(12) C32 0.0282(12) 0.0287(13) 0.0436(15) -0.0062(11) 0.0089(10) -0.0066(10) C33 0.0301(11) 0.0225(12) 0.0266(12) 0.0035(9) 0.0044(9) -0.0027(9) C34 0.0218(10) 0.0234(11) 0.0271(11) 0.0030(9) 0.0009(8) -0.0030(9) C35 0.0285(11) 0.0270(12) 0.0291(12) -0.0008(10) 0.0031(9) -0.0014(9) C36 0.0390(13) 0.0220(12) 0.0312(13) 0.0014(10) 0.0029(10) 0.0010(10) C37 0.0403(13) 0.0208(12) 0.0306(12) 0.0033(10) -0.0018(10) -0.0075(10) C38 0.0350(13) 0.0268(13) 0.0284(12) 0.0028(10) 0.0049(10) -0.0059(10) C39 0.0575(17) 0.0281(14) 0.0337(14) 0.0037(11) 0.0148(12) -0.0053(12) C40 0.076(2) 0.0330(15) 0.0299(14) 0.0061(12) 0.0159(13) -0.0087(14) C41 0.085(2) 0.0250(14) 0.0356(15) 0.0070(12) 0.0044(14) -0.0082(15) C42 0.0607(17) 0.0245(13) 0.0316(13) 0.0063(11) 0.0030(12) -0.0029(12) C43 0.0382(13) 0.0265(12) 0.0294(12) 0.0064(10) 0.0138(10) 0.0021(10) C44 0.0361(13) 0.0418(16) 0.0367(14) 0.0107(12) 0.0175(11) 0.0068(12) C45 0.0515(17) 0.0476(18) 0.0537(18) 0.0183(15) 0.0303(15) 0.0199(15) C46 0.073(2) 0.0341(15) 0.0468(17) 0.0099(14) 0.0351(16) 0.0167(15) C47 0.0696(19) 0.0263(14) 0.0342(15) 0.0038(11) 0.0237(13) 0.0037(13) C48 0.0514(15) 0.0245(13) 0.0250(12) 0.0055(10) 0.0130(10) 0.0016(11) C49 0.0542(16) 0.0275(13) 0.0251(12) 0.0050(10) 0.0070(11) -0.0038(12) C50 0.0678(19) 0.0367(16) 0.0291(14) 0.0035(12) -0.0009(12) -0.0137(14) C51 0.100(3) 0.0388(17) 0.0268(14) -0.0027(13) 0.0044(15) -0.0183(18) C52 0.112(3) 0.0243(15) 0.0374(16) -0.0043(12) 0.0294(18) -0.0079(17) C53 0.0426(16) 0.070(2) 0.058(2) 0.0138(18) 0.0084(14) -0.0131(16) C54 0.0348(15) 0.081(3) 0.063(2) 0.0191(19) 0.0114(13) 0.0158(16) C55 0.0250(10) 0.0229(11) 0.0232(11) -0.0008(9) 0.0046(8) 0.0021(9) C56 0.0247(10) 0.0228(11) 0.0199(10) 0.0038(9) 0.0018(8) -0.0034(9) C57 0.0286(11) 0.0262(12) 0.0235(11) 0.0000(9) 0.0044(9) -0.0042(9) C58 0.0338(13) 0.0275(13) 0.0318(13) -0.0045(10) 0.0042(10) -0.0053(10) C59 0.0335(13) 0.0343(14) 0.0331(13) -0.0033(11) -0.0006(10) -0.0072(11) C60 0.0283(12) 0.0346(14) 0.0311(13) 0.0012(11) -0.0032(9) -0.0011(10) C61 0.0259(11) 0.0273(12) 0.0273(12) 0.0028(10) 0.0033(9) -0.0001(9) C62 0.0328(12) 0.0237(12) 0.0336(13) -0.0021(10) 0.0052(10) -0.0014(10) C63 0.0424(15) 0.055(2) 0.0423(16) -0.0106(14) -0.0086(12) -0.0091(14) C64 0.0302(12) 0.0324(13) 0.0356(13) -0.0045(11) -0.0026(10) 0.0022(10) C65 0.0382(15) 0.0364(17) 0.093(3) 0.0083(17) 0.0279(16) -0.0081(13) C66 0.0365(13) 0.0266(13) 0.0395(14) -0.0012(11) 0.0035(11) -0.0072(11) C67 0.0381(15) 0.0484(18) 0.0511(17) -0.0075(14) -0.0187(12) 0.0144(13) C68 0.0306(13) 0.0433(17) 0.0638(19) -0.0205(15) 0.0014(12) 0.0076(12) C69 0.084(3) 0.077(3) 0.048(2) -0.0042(19) 0.0028(18) 0.008(2) C70 0.0578(18) 0.0494(18) 0.0297(14) -0.0071(13) 0.0122(12) -0.0073(14) C71 0.065(2) 0.0437(18) 0.0337(15) -0.0016(13) 0.0174(14) -0.0128(15) C72 0.0533(18) 0.060(2) 0.0471(18) -0.0111(16) 0.0241(14) -0.0115(16) C73 0.056(2) 0.070(2) 0.0487(19) -0.0012(17) 0.0194(15) 0.0153(18) C74 0.097(3) 0.0353(17) 0.060(2) -0.0054(16) 0.037(2) 0.0020(19) C75 0.068(2) 0.0439(19) 0.0469(18) -0.0130(15) 0.0169(15) -0.0173(16) C76 0.082(3) 0.095(3) 0.075(3) -0.020(3) -0.015(2) 0.010(3) C77 0.069(2) 0.0414(19) 0.070(2) -0.0036(16) -0.0096(17) 0.0087(16) C78 0.074(2) 0.0468(19) 0.077(2) -0.002(2) 0.0285(18) 0.003(2) C79 0.060(2) 0.049(2) 0.082(3) 0.0003(19) 0.0182(18) -0.0063(16) C80 0.068(2) 0.050(2) 0.075(3) 0.0059(19) -0.0127(19) -0.0113(18) C81 0.074(2) 0.055(2) 0.055(2) 0.0034(17) 0.0116(17) 0.0009(18) C82 0.0499(17) 0.081(3) 0.0522(18) 0.006(2) 0.0107(14) 0.0079(19) C83 0.164(6) 0.108(4) 0.137(5) 0.055(4) 0.102(4) 0.069(4) C84 0.076(2) 0.060(2) 0.055(2) 0.0067(18) 0.0352(18) 0.0110(19) C85 0.099(3) 0.078(3) 0.048(2) -0.002(2) 0.005(2) -0.034(3) C86 0.078(3) 0.112(4) 0.074(3) 0.050(3) -0.011(2) -0.010(3) C87 0.109(4) 0.071(3) 0.079(3) 0.039(3) 0.017(3) 0.020(3) C88 0.120(4) 0.060(3) 0.054(2) 0.0026(19) 0.014(2) -0.008(2) C89 0.057(2) 0.089(3) 0.0416(18) 0.0112(19) 0.0001(14) -0.017(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag V N6 1.865(2) . ? V N5 1.873(2) . ? V N1 2.0858(19) . ? V N3 2.0889(18) . ? V O2 2.1491(16) . ? V O1 2.1493(16) . ? V C23 2.513(2) . ? V C55 2.528(2) . ? O1 C23 1.282(3) . ? O2 C55 1.287(3) . ? N1 C23 1.323(3) . ? N1 C2 1.421(3) . ? N2 C12 1.435(3) . ? N2 C22 1.455(3) . ? N2 C21 1.462(3) . ? N3 C55 1.326(3) . ? N3 C34 1.424(3) . ? N4 C44 1.423(4) . ? N4 C53 1.452(4) . ? N4 C54 1.455(4) . ? N5 C66 1.459(3) . ? N5 C65 1.459(3) . ? N6 C68 1.446(3) . ? N6 C67 1.456(3) . ? C1 C2 1.388(3) . ? C1 C6 1.443(3) . ? C1 C11 1.493(3) . ? C2 C3 1.432(3) . ? C3 C4 1.361(3) . ? C3 H3 0.9500 . ? C4 C5 1.420(3) . ? C4 H4 0.9500 . ? C5 C10 1.416(3) . ? C5 C6 1.428(3) . ? C6 C7 1.420(3) . ? C7 C8 1.381(3) . ? C7 H7 0.9500 . ? C8 C9 1.405(4) . ? C8 H8 0.9500 . ? C9 C10 1.371(4) . ? C9 H9 0.9500 . ? C10 H10 0.9500 . ? C11 C12 1.383(3) . ? C11 C16 1.437(3) . ? C12 C13 1.424(3) . ? C13 C14 1.351(3) . ? C13 H13 0.9500 . ? C14 C15 1.420(3) . ? C14 H14 0.9500 . ? C15 C20 1.424(3) . ? C15 C16 1.424(3) . ? C16 C17 1.423(3) . ? C17 C18 1.374(3) . ? C17 H17 0.9500 . ? C18 C19 1.406(3) . ? C18 H18 0.9500 . ? C19 C20 1.364(4) . ? C19 H19 0.9500 . ? C20 H20 0.9500 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 C24 1.500(3) . ? C24 C29 1.400(3) . ? C24 C25 1.407(3) . ? C25 C26 1.392(3) . ? C25 C30 1.499(3) . ? C26 C27 1.389(4) . ? C26 H26 0.9500 . ? C27 C28 1.389(4) . ? C27 C31 1.511(3) . ? C28 C29 1.399(3) . ? C28 H28 0.9500 . ? C29 C32 1.506(3) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C34 1.388(3) . ? C33 C38 1.440(3) . ? C33 C43 1.500(3) . ? C34 C35 1.418(3) . ? C35 C36 1.362(3) . ? C35 H35 0.9500 . ? C36 C37 1.419(4) . ? C36 H36 0.9500 . ? C37 C42 1.422(3) . ? C37 C38 1.426(4) . ? C38 C39 1.417(4) . ? C39 C40 1.366(4) . ? C39 H39 0.9500 . ? C40 C41 1.403(4) . ? C40 H40 0.9500 . ? C41 C42 1.375(4) . ? C41 H41 0.9500 . ? C42 H42 0.9500 . ? C43 C44 1.399(4) . ? C43 C48 1.433(4) . ? C44 C45 1.433(4) . ? C45 C46 1.355(5) . ? C45 H45 0.9500 . ? C46 C47 1.415(4) . ? C46 H46 0.9500 . ? C47 C52 1.415(5) . ? C47 C48 1.427(4) . ? C48 C49 1.419(4) . ? C49 C50 1.364(4) . ? C49 H49 0.9500 . ? C50 C51 1.414(5) . ? C50 H50 0.9500 . ? C51 C52 1.353(5) . ? C51 H51 0.9500 . ? C52 H52 0.9500 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.497(3) . ? C56 C57 1.400(3) . ? C56 C61 1.410(3) . ? C57 C58 1.397(3) . ? C57 C62 1.493(3) . ? C58 C59 1.384(4) . ? C58 H58 0.9500 . ? C59 C60 1.389(4) . ? C59 C63 1.514(3) . ? C60 C61 1.397(3) . ? C60 H60 0.9500 . ? C61 C64 1.508(3) . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 H67A 0.9800 . ? C67 H67B 0.9800 . ? C67 H67C 0.9800 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 C70 1.528(5) . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 C75 1.369(5) . ? C70 C71 1.388(4) . ? C71 C72 1.375(5) . ? C71 H71 0.9500 . ? C72 C73 1.386(5) . ? C72 H72 0.9500 . ? C73 C74 1.400(5) . ? C73 H73 0.9500 . ? C74 C75 1.390(5) . ? C74 H74 0.9500 . ? C75 H75 0.9500 . ? C76 C77 1.477(5) . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 C78 1.362(5) . ? C77 C82 1.413(5) . ? C78 C79 1.405(5) . ? C78 H78 0.9500 . ? C79 C80 1.327(5) . ? C79 H79 0.9500 . ? C80 C81 1.398(5) . ? C80 H80 0.9500 . ? C81 C82 1.383(5) . ? C81 H81 0.9500 . ? C82 H82 0.9500 . ? C83 C84 1.478(6) . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 C85 1.367(6) . ? C84 C89 1.383(6) . ? C85 C86 1.369(7) . ? C85 H85 0.9500 . ? C86 C87 1.338(7) . ? C86 H86 0.9500 . ? C87 C88 1.362(7) . ? C87 H87 0.9500 . ? C88 C89 1.411(6) . ? C88 H88 0.9500 . ? C89 H89 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N6 V N5 98.37(10) . . ? N6 V N1 96.53(8) . . ? N5 V N1 110.04(8) . . ? N6 V N3 105.97(8) . . ? N5 V N3 98.12(8) . . ? N1 V N3 140.81(7) . . ? N6 V O2 91.06(8) . . ? N5 V O2 159.72(7) . . ? N1 V O2 86.49(7) . . ? N3 V O2 61.89(7) . . ? N6 V O1 158.50(7) . . ? N5 V O1 92.05(8) . . ? N1 V O1 62.13(6) . . ? N3 V O1 90.99(7) . . ? O2 V O1 85.31(6) . . ? N6 V C23 127.83(8) . . ? N5 V C23 105.56(8) . . ? N1 V C23 31.74(7) . . ? N3 V C23 115.33(7) . . ? O2 V C23 82.08(6) . . ? O1 V C23 30.68(6) . . ? N6 V C55 102.84(8) . . ? N5 V C55 129.16(8) . . ? N1 V C55 112.67(7) . . ? N3 V C55 31.59(7) . . ? O2 V C55 30.60(7) . . ? O1 V C55 84.59(7) . . ? C23 V C55 96.79(7) . . ? C23 O1 V 90.52(12) . . ? C55 O2 V 91.20(13) . . ? C23 N1 C2 127.97(18) . . ? C23 N1 V 92.21(13) . . ? C2 N1 V 133.76(14) . . ? C12 N2 C22 112.93(19) . . ? C12 N2 C21 115.13(19) . . ? C22 N2 C21 110.38(19) . . ? C55 N3 C34 126.75(18) . . ? C55 N3 V 92.79(13) . . ? C34 N3 V 135.95(16) . . ? C44 N4 C53 115.4(2) . . ? C44 N4 C54 115.9(3) . . ? C53 N4 C54 109.6(2) . . ? C66 N5 C65 109.0(2) . . ? C66 N5 V 126.52(15) . . ? C65 N5 V 123.16(19) . . ? C68 N6 C67 109.5(2) . . ? C68 N6 V 127.06(16) . . ? C67 N6 V 121.64(18) . . ? C2 C1 C6 118.4(2) . . ? C2 C1 C11 123.37(19) . . ? C6 C1 C11 118.20(18) . . ? C1 C2 N1 125.5(2) . . ? C1 C2 C3 120.3(2) . . ? N1 C2 C3 114.11(19) . . ? C4 C3 C2 121.5(2) . . ? C4 C3 H3 119.3 . . ? C2 C3 H3 119.3 . . ? C3 C4 C5 120.6(2) . . ? C3 C4 H4 119.7 . . ? C5 C4 H4 119.7 . . ? C10 C5 C4 121.6(2) . . ? C10 C5 C6 119.9(2) . . ? C4 C5 C6 118.5(2) . . ? C7 C6 C5 118.0(2) . . ? C7 C6 C1 121.3(2) . . ? C5 C6 C1 120.7(2) . . ? C8 C7 C6 120.4(2) . . ? C8 C7 H7 119.8 . . ? C6 C7 H7 119.8 . . ? C7 C8 C9 121.2(2) . . ? C7 C8 H8 119.4 . . ? C9 C8 H8 119.4 . . ? C10 C9 C8 119.7(2) . . ? C10 C9 H9 120.1 . . ? C8 C9 H9 120.1 . . ? C9 C10 C5 120.7(2) . . ? C9 C10 H10 119.6 . . ? C5 C10 H10 119.6 . . ? C12 C11 C16 119.6(2) . . ? C12 C11 C1 122.03(18) . . ? C16 C11 C1 118.29(19) . . ? C11 C12 C13 119.6(2) . . ? C11 C12 N2 119.6(2) . . ? C13 C12 N2 120.71(19) . . ? C14 C13 C12 121.4(2) . . ? C14 C13 H13 119.3 . . ? C12 C13 H13 119.3 . . ? C13 C14 C15 121.1(2) . . ? C13 C14 H14 119.5 . . ? C15 C14 H14 119.5 . . ? C14 C15 C20 122.1(2) . . ? C14 C15 C16 118.4(2) . . ? C20 C15 C16 119.5(2) . . ? C17 C16 C15 117.76(19) . . ? C17 C16 C11 122.5(2) . . ? C15 C16 C11 119.8(2) . . ? C18 C17 C16 121.0(2) . . ? C18 C17 H17 119.5 . . ? C16 C17 H17 119.5 . . ? C17 C18 C19 121.0(2) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C20 C19 C18 119.7(2) . . ? C20 C19 H19 120.2 . . ? C18 C19 H19 120.2 . . ? C19 C20 C15 121.1(2) . . ? C19 C20 H20 119.5 . . ? C15 C20 H20 119.5 . . ? N2 C21 H21A 109.5 . . ? N2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N2 C22 H22A 109.5 . . ? N2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? N2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? O1 C23 N1 114.13(19) . . ? O1 C23 C24 118.68(18) . . ? N1 C23 C24 127.19(19) . . ? O1 C23 V 58.80(11) . . ? N1 C23 V 56.05(11) . . ? C24 C23 V 171.84(15) . . ? C29 C24 C25 120.9(2) . . ? C29 C24 C23 121.1(2) . . ? C25 C24 C23 117.76(19) . . ? C26 C25 C24 118.1(2) . . ? C26 C25 C30 120.1(2) . . ? C24 C25 C30 121.8(2) . . ? C27 C26 C25 122.2(2) . . ? C27 C26 H26 118.9 . . ? C25 C26 H26 118.9 . . ? C26 C27 C28 118.7(2) . . ? C26 C27 C31 120.5(2) . . ? C28 C27 C31 120.8(2) . . ? C27 C28 C29 121.3(2) . . ? C27 C28 H28 119.3 . . ? C29 C28 H28 119.3 . . ? C28 C29 C24 118.8(2) . . ? C28 C29 C32 119.8(2) . . ? C24 C29 C32 121.3(2) . . ? C25 C30 H30A 109.5 . . ? C25 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C25 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C27 C31 H31A 109.5 . . ? C27 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C27 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C34 C33 C38 118.4(2) . . ? C34 C33 C43 123.5(2) . . ? C38 C33 C43 117.9(2) . . ? C33 C34 C35 120.3(2) . . ? C33 C34 N3 123.8(2) . . ? C35 C34 N3 115.8(2) . . ? C36 C35 C34 122.0(2) . . ? C36 C35 H35 119.0 . . ? C34 C35 H35 119.0 . . ? C35 C36 C37 119.8(2) . . ? C35 C36 H36 120.1 . . ? C37 C36 H36 120.1 . . ? C36 C37 C42 121.7(2) . . ? C36 C37 C38 119.0(2) . . ? C42 C37 C38 119.2(2) . . ? C39 C38 C37 118.0(2) . . ? C39 C38 C33 121.7(2) . . ? C37 C38 C33 120.3(2) . . ? C40 C39 C38 121.4(3) . . ? C40 C39 H39 119.3 . . ? C38 C39 H39 119.3 . . ? C39 C40 C41 120.8(3) . . ? C39 C40 H40 119.6 . . ? C41 C40 H40 119.6 . . ? C42 C41 C40 119.7(3) . . ? C42 C41 H41 120.1 . . ? C40 C41 H41 120.1 . . ? C41 C42 C37 120.8(3) . . ? C41 C42 H42 119.6 . . ? C37 C42 H42 119.6 . . ? C44 C43 C48 119.9(2) . . ? C44 C43 C33 122.8(2) . . ? C48 C43 C33 117.2(2) . . ? C43 C44 N4 121.3(3) . . ? C43 C44 C45 118.7(3) . . ? N4 C44 C45 120.0(3) . . ? C46 C45 C44 121.6(3) . . ? C46 C45 H45 119.2 . . ? C44 C45 H45 119.2 . . ? C45 C46 C47 121.4(3) . . ? C45 C46 H46 119.3 . . ? C47 C46 H46 119.3 . . ? C52 C47 C46 122.6(3) . . ? C52 C47 C48 119.1(3) . . ? C46 C47 C48 118.4(3) . . ? C49 C48 C47 117.5(3) . . ? C49 C48 C43 122.6(2) . . ? C47 C48 C43 120.0(3) . . ? C50 C49 C48 121.6(3) . . ? C50 C49 H49 119.2 . . ? C48 C49 H49 119.2 . . ? C49 C50 C51 120.6(3) . . ? C49 C50 H50 119.7 . . ? C51 C50 H50 119.7 . . ? C52 C51 C50 119.3(3) . . ? C52 C51 H51 120.4 . . ? C50 C51 H51 120.4 . . ? C51 C52 C47 122.0(3) . . ? C51 C52 H52 119.0 . . ? C47 C52 H52 119.0 . . ? N4 C53 H53A 109.5 . . ? N4 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N4 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N4 C54 H54A 109.5 . . ? N4 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? N4 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? O2 C55 N3 113.07(19) . . ? O2 C55 C56 118.2(2) . . ? N3 C55 C56 128.7(2) . . ? O2 C55 V 58.21(11) . . ? N3 C55 V 55.62(11) . . ? C56 C55 V 170.86(16) . . ? C57 C56 C61 121.0(2) . . ? C57 C56 C55 117.8(2) . . ? C61 C56 C55 120.8(2) . . ? C58 C57 C56 117.9(2) . . ? C58 C57 C62 120.3(2) . . ? C56 C57 C62 121.8(2) . . ? C59 C58 C57 122.8(2) . . ? C59 C58 H58 118.6 . . ? C57 C58 H58 118.6 . . ? C58 C59 C60 117.9(2) . . ? C58 C59 C63 121.1(3) . . ? C60 C59 C63 121.0(2) . . ? C59 C60 C61 122.2(2) . . ? C59 C60 H60 118.9 . . ? C61 C60 H60 118.9 . . ? C60 C61 C56 118.2(2) . . ? C60 C61 C64 119.9(2) . . ? C56 C61 C64 121.9(2) . . ? C57 C62 H62A 109.5 . . ? C57 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C57 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C59 C63 H63A 109.5 . . ? C59 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C59 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C61 C64 H64A 109.5 . . ? C61 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C61 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? N5 C65 H65A 109.5 . . ? N5 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? N5 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? N5 C66 H66A 109.5 . . ? N5 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? N5 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? N6 C67 H67A 109.5 . . ? N6 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? N6 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? N6 C68 H68A 109.5 . . ? N6 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? N6 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C70 C69 H69A 109.5 . . ? C70 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C70 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C75 C70 C71 118.9(3) . . ? C75 C70 C69 121.1(3) . . ? C71 C70 C69 119.9(3) . . ? C72 C71 C70 121.1(3) . . ? C72 C71 H71 119.5 . . ? C70 C71 H71 119.5 . . ? C71 C72 C73 119.9(3) . . ? C71 C72 H72 120.1 . . ? C73 C72 H72 120.1 . . ? C72 C73 C74 119.6(4) . . ? C72 C73 H73 120.2 . . ? C74 C73 H73 120.2 . . ? C75 C74 C73 119.1(3) . . ? C75 C74 H74 120.4 . . ? C73 C74 H74 120.4 . . ? C70 C75 C74 121.3(3) . . ? C70 C75 H75 119.3 . . ? C74 C75 H75 119.3 . . ? C77 C76 H76A 109.5 . . ? C77 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C77 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C78 C77 C82 117.1(3) . . ? C78 C77 C76 121.9(4) . . ? C82 C77 C76 120.8(4) . . ? C77 C78 C79 121.3(4) . . ? C77 C78 H78 119.3 . . ? C79 C78 H78 119.3 . . ? C80 C79 C78 120.9(4) . . ? C80 C79 H79 119.6 . . ? C78 C79 H79 119.6 . . ? C79 C80 C81 120.4(4) . . ? C79 C80 H80 119.8 . . ? C81 C80 H80 119.8 . . ? C82 C81 C80 118.8(3) . . ? C82 C81 H81 120.6 . . ? C80 C81 H81 120.6 . . ? C81 C82 C77 121.4(3) . . ? C81 C82 H82 119.3 . . ? C77 C82 H82 119.3 . . ? C84 C83 H83A 109.5 . . ? C84 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C84 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C85 C84 C89 118.5(4) . . ? C85 C84 C83 122.2(5) . . ? C89 C84 C83 119.3(5) . . ? C84 C85 C86 120.9(4) . . ? C84 C85 H85 119.6 . . ? C86 C85 H85 119.6 . . ? C87 C86 C85 122.0(4) . . ? C87 C86 H86 119.0 . . ? C85 C86 H86 119.0 . . ? C86 C87 C88 118.6(4) . . ? C86 C87 H87 120.7 . . ? C88 C87 H87 120.7 . . ? C87 C88 C89 121.0(4) . . ? C87 C88 H88 119.5 . . ? C89 C88 H88 119.5 . . ? C84 C89 C88 118.9(3) . . ? C84 C89 H89 120.6 . . ? C88 C89 H89 120.6 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 V O1 C23 -1.5(3) . . . . ? N5 V O1 C23 117.76(13) . . . . ? N1 V O1 C23 6.12(12) . . . . ? N3 V O1 C23 -144.07(13) . . . . ? O2 V O1 C23 -82.38(12) . . . . ? C55 V O1 C23 -113.09(13) . . . . ? N6 V O2 C55 113.92(13) . . . . ? N5 V O2 C55 -4.1(3) . . . . ? N1 V O2 C55 -149.61(13) . . . . ? N3 V O2 C55 6.33(12) . . . . ? O1 V O2 C55 -87.31(13) . . . . ? C23 V O2 C55 -118.01(13) . . . . ? N6 V N1 C23 171.28(13) . . . . ? N5 V N1 C23 -87.33(14) . . . . ? N3 V N1 C23 45.93(19) . . . . ? O2 V N1 C23 80.62(13) . . . . ? O1 V N1 C23 -5.93(12) . . . . ? C55 V N1 C23 64.41(14) . . . . ? N6 V N1 C2 18.5(2) . . . . ? N5 V N1 C2 119.88(19) . . . . ? N3 V N1 C2 -106.9(2) . . . . ? O2 V N1 C2 -72.18(19) . . . . ? O1 V N1 C2 -158.7(2) . . . . ? C23 V N1 C2 -152.8(3) . . . . ? C55 V N1 C2 -88.38(19) . . . . ? N6 V N3 C55 -88.61(14) . . . . ? N5 V N3 C55 170.22(14) . . . . ? N1 V N3 C55 33.95(19) . . . . ? O2 V N3 C55 -6.15(12) . . . . ? O1 V N3 C55 78.01(13) . . . . ? C23 V N3 C55 58.66(15) . . . . ? N6 V N3 C34 115.6(2) . . . . ? N5 V N3 C34 14.4(2) . . . . ? N1 V N3 C34 -121.84(19) . . . . ? O2 V N3 C34 -161.9(2) . . . . ? O1 V N3 C34 -77.8(2) . . . . ? C23 V N3 C34 -97.1(2) . . . . ? C55 V N3 C34 -155.8(3) . . . . ? N6 V N5 C66 159.1(2) . . . . ? N1 V N5 C66 59.0(2) . . . . ? N3 V N5 C66 -93.3(2) . . . . ? O2 V N5 C66 -84.1(3) . . . . ? O1 V N5 C66 -2.0(2) . . . . ? C23 V N5 C66 25.9(2) . . . . ? C55 V N5 C66 -86.7(2) . . . . ? N6 V N5 C65 -35.6(2) . . . . ? N1 V N5 C65 -135.7(2) . . . . ? N3 V N5 C65 72.0(2) . . . . ? O2 V N5 C65 81.3(3) . . . . ? O1 V N5 C65 163.3(2) . . . . ? C23 V N5 C65 -168.7(2) . . . . ? C55 V N5 C65 78.6(2) . . . . ? N5 V N6 C68 146.6(2) . . . . ? N1 V N6 C68 -102.0(2) . . . . ? N3 V N6 C68 45.6(2) . . . . ? O2 V N6 C68 -15.4(2) . . . . ? O1 V N6 C68 -95.3(3) . . . . ? C23 V N6 C68 -96.2(2) . . . . ? C55 V N6 C68 13.1(2) . . . . ? N5 V N6 C67 -50.5(2) . . . . ? N1 V N6 C67 60.9(2) . . . . ? N3 V N6 C67 -151.5(2) . . . . ? O2 V N6 C67 147.5(2) . . . . ? O1 V N6 C67 67.7(3) . . . . ? C23 V N6 C67 66.7(2) . . . . ? C55 V N6 C67 176.0(2) . . . . ? C6 C1 C2 N1 175.75(18) . . . . ? C11 C1 C2 N1 -6.5(3) . . . . ? C6 C1 C2 C3 -0.8(3) . . . . ? C11 C1 C2 C3 176.96(19) . . . . ? C23 N1 C2 C1 78.4(3) . . . . ? V N1 C2 C1 -136.96(18) . . . . ? C23 N1 C2 C3 -104.8(2) . . . . ? V N1 C2 C3 39.8(3) . . . . ? C1 C2 C3 C4 -0.3(3) . . . . ? N1 C2 C3 C4 -177.2(2) . . . . ? C2 C3 C4 C5 0.7(3) . . . . ? C3 C4 C5 C10 -178.3(2) . . . . ? C3 C4 C5 C6 0.0(3) . . . . ? C10 C5 C6 C7 -3.1(3) . . . . ? C4 C5 C6 C7 178.61(19) . . . . ? C10 C5 C6 C1 177.24(19) . . . . ? C4 C5 C6 C1 -1.1(3) . . . . ? C2 C1 C6 C7 -178.23(19) . . . . ? C11 C1 C6 C7 3.9(3) . . . . ? C2 C1 C6 C5 1.5(3) . . . . ? C11 C1 C6 C5 -176.39(18) . . . . ? C5 C6 C7 C8 2.8(3) . . . . ? C1 C6 C7 C8 -177.5(2) . . . . ? C6 C7 C8 C9 -0.4(3) . . . . ? C7 C8 C9 C10 -1.9(3) . . . . ? C8 C9 C10 C5 1.7(3) . . . . ? C4 C5 C10 C9 179.1(2) . . . . ? C6 C5 C10 C9 0.8(3) . . . . ? C2 C1 C11 C12 75.7(3) . . . . ? C6 C1 C11 C12 -106.6(2) . . . . ? C2 C1 C11 C16 -107.6(2) . . . . ? C6 C1 C11 C16 70.2(2) . . . . ? C16 C11 C12 C13 2.3(3) . . . . ? C1 C11 C12 C13 178.97(19) . . . . ? C16 C11 C12 N2 -176.20(18) . . . . ? C1 C11 C12 N2 0.5(3) . . . . ? C22 N2 C12 C11 79.2(3) . . . . ? C21 N2 C12 C11 -152.8(2) . . . . ? C22 N2 C12 C13 -99.3(3) . . . . ? C21 N2 C12 C13 28.8(3) . . . . ? C11 C12 C13 C14 -1.8(3) . . . . ? N2 C12 C13 C14 176.7(2) . . . . ? C12 C13 C14 C15 -0.4(4) . . . . ? C13 C14 C15 C20 -177.7(2) . . . . ? C13 C14 C15 C16 2.0(3) . . . . ? C14 C15 C16 C17 179.4(2) . . . . ? C20 C15 C16 C17 -0.8(3) . . . . ? C14 C15 C16 C11 -1.5(3) . . . . ? C20 C15 C16 C11 178.3(2) . . . . ? C12 C11 C16 C17 178.4(2) . . . . ? C1 C11 C16 C17 1.6(3) . . . . ? C12 C11 C16 C15 -0.7(3) . . . . ? C1 C11 C16 C15 -177.49(18) . . . . ? C15 C16 C17 C18 1.5(3) . . . . ? C11 C16 C17 C18 -177.6(2) . . . . ? C16 C17 C18 C19 -1.0(3) . . . . ? C17 C18 C19 C20 -0.3(4) . . . . ? C18 C19 C20 C15 0.9(4) . . . . ? C14 C15 C20 C19 179.4(2) . . . . ? C16 C15 C20 C19 -0.4(3) . . . . ? V O1 C23 N1 -9.37(18) . . . . ? V O1 C23 C24 171.04(17) . . . . ? C2 N1 C23 O1 164.90(19) . . . . ? V N1 C23 O1 9.66(19) . . . . ? C2 N1 C23 C24 -15.5(3) . . . . ? V N1 C23 C24 -170.8(2) . . . . ? C2 N1 C23 V 155.2(2) . . . . ? N6 V C23 O1 179.32(12) . . . . ? N5 V C23 O1 -66.63(13) . . . . ? N1 V C23 O1 -169.7(2) . . . . ? N3 V C23 O1 40.47(14) . . . . ? O2 V C23 O1 94.16(12) . . . . ? C55 V C23 O1 67.26(13) . . . . ? N6 V C23 N1 -10.99(17) . . . . ? N5 V C23 N1 103.05(14) . . . . ? N3 V C23 N1 -149.85(13) . . . . ? O2 V C23 N1 -96.15(13) . . . . ? O1 V C23 N1 169.7(2) . . . . ? C55 V C23 N1 -123.06(13) . . . . ? N6 V C23 C24 105.0(11) . . . . ? N5 V C23 C24 -140.9(11) . . . . ? N1 V C23 C24 116.0(11) . . . . ? N3 V C23 C24 -33.8(11) . . . . ? O2 V C23 C24 19.9(11) . . . . ? O1 V C23 C24 -74.3(11) . . . . ? C55 V C23 C24 -7.0(11) . . . . ? O1 C23 C24 C29 -104.7(2) . . . . ? N1 C23 C24 C29 75.8(3) . . . . ? V C23 C24 C29 -34.8(12) . . . . ? O1 C23 C24 C25 70.1(3) . . . . ? N1 C23 C24 C25 -109.4(3) . . . . ? V C23 C24 C25 139.9(10) . . . . ? C29 C24 C25 C26 -1.8(3) . . . . ? C23 C24 C25 C26 -176.52(19) . . . . ? C29 C24 C25 C30 177.7(2) . . . . ? C23 C24 C25 C30 2.9(3) . . . . ? C24 C25 C26 C27 1.1(3) . . . . ? C30 C25 C26 C27 -178.3(2) . . . . ? C25 C26 C27 C28 0.3(4) . . . . ? C25 C26 C27 C31 179.2(2) . . . . ? C26 C27 C28 C29 -1.1(4) . . . . ? C31 C27 C28 C29 -180.0(2) . . . . ? C27 C28 C29 C24 0.4(3) . . . . ? C27 C28 C29 C32 177.2(2) . . . . ? C25 C24 C29 C28 1.0(3) . . . . ? C23 C24 C29 C28 175.6(2) . . . . ? C25 C24 C29 C32 -175.7(2) . . . . ? C23 C24 C29 C32 -1.1(3) . . . . ? C38 C33 C34 C35 2.3(3) . . . . ? C43 C33 C34 C35 178.4(2) . . . . ? C38 C33 C34 N3 179.5(2) . . . . ? C43 C33 C34 N3 -4.4(4) . . . . ? C55 N3 C34 C33 79.7(3) . . . . ? V N3 C34 C33 -131.1(2) . . . . ? C55 N3 C34 C35 -103.0(3) . . . . ? V N3 C34 C35 46.3(3) . . . . ? C33 C34 C35 C36 -3.4(3) . . . . ? N3 C34 C35 C36 179.2(2) . . . . ? C34 C35 C36 C37 1.6(4) . . . . ? C35 C36 C37 C42 -177.5(2) . . . . ? C35 C36 C37 C38 1.1(4) . . . . ? C36 C37 C38 C39 178.8(2) . . . . ? C42 C37 C38 C39 -2.6(4) . . . . ? C36 C37 C38 C33 -2.1(3) . . . . ? C42 C37 C38 C33 176.5(2) . . . . ? C34 C33 C38 C39 179.5(2) . . . . ? C43 C33 C38 C39 3.1(4) . . . . ? C34 C33 C38 C37 0.4(3) . . . . ? C43 C33 C38 C37 -176.0(2) . . . . ? C37 C38 C39 C40 2.8(4) . . . . ? C33 C38 C39 C40 -176.4(3) . . . . ? C38 C39 C40 C41 -0.8(5) . . . . ? C39 C40 C41 C42 -1.4(5) . . . . ? C40 C41 C42 C37 1.5(5) . . . . ? C36 C37 C42 C41 179.1(3) . . . . ? C38 C37 C42 C41 0.6(4) . . . . ? C34 C33 C43 C44 77.3(3) . . . . ? C38 C33 C43 C44 -106.5(3) . . . . ? C34 C33 C43 C48 -105.6(3) . . . . ? C38 C33 C43 C48 70.6(3) . . . . ? C48 C43 C44 N4 -176.7(2) . . . . ? C33 C43 C44 N4 0.4(4) . . . . ? C48 C43 C44 C45 2.0(3) . . . . ? C33 C43 C44 C45 179.1(2) . . . . ? C53 N4 C44 C43 65.0(3) . . . . ? C54 N4 C44 C43 -165.0(2) . . . . ? C53 N4 C44 C45 -113.7(3) . . . . ? C54 N4 C44 C45 16.3(3) . . . . ? C43 C44 C45 C46 -2.1(4) . . . . ? N4 C44 C45 C46 176.6(3) . . . . ? C44 C45 C46 C47 -0.1(4) . . . . ? C45 C46 C47 C52 -178.4(3) . . . . ? C45 C46 C47 C48 2.4(4) . . . . ? C52 C47 C48 C49 -1.3(4) . . . . ? C46 C47 C48 C49 178.0(2) . . . . ? C52 C47 C48 C43 178.3(2) . . . . ? C46 C47 C48 C43 -2.5(4) . . . . ? C44 C43 C48 C49 179.8(2) . . . . ? C33 C43 C48 C49 2.6(3) . . . . ? C44 C43 C48 C47 0.3(4) . . . . ? C33 C43 C48 C47 -176.9(2) . . . . ? C47 C48 C49 C50 1.3(4) . . . . ? C43 C48 C49 C50 -178.3(2) . . . . ? C48 C49 C50 C51 -0.1(4) . . . . ? C49 C50 C51 C52 -1.1(4) . . . . ? C50 C51 C52 C47 1.1(5) . . . . ? C46 C47 C52 C51 -179.1(3) . . . . ? C48 C47 C52 C51 0.1(4) . . . . ? V O2 C55 N3 -9.58(18) . . . . ? V O2 C55 C56 170.28(18) . . . . ? C34 N3 C55 O2 169.0(2) . . . . ? V N3 C55 O2 9.87(19) . . . . ? C34 N3 C55 C56 -10.8(4) . . . . ? V N3 C55 C56 -170.0(2) . . . . ? C34 N3 C55 V 159.1(2) . . . . ? N6 V C55 O2 -69.62(13) . . . . ? N5 V C55 O2 178.17(12) . . . . ? N1 V C55 O2 33.18(14) . . . . ? N3 V C55 O2 -169.3(2) . . . . ? O1 V C55 O2 89.93(12) . . . . ? C23 V C55 O2 61.72(13) . . . . ? N6 V C55 N3 99.69(14) . . . . ? N5 V C55 N3 -12.52(17) . . . . ? N1 V C55 N3 -157.51(13) . . . . ? O2 V C55 N3 169.3(2) . . . . ? O1 V C55 N3 -100.77(13) . . . . ? C23 V C55 N3 -128.97(13) . . . . ? N6 V C55 C56 -139.1(11) . . . . ? N5 V C55 C56 108.6(10) . . . . ? N1 V C55 C56 -36.3(11) . . . . ? N3 V C55 C56 121.2(11) . . . . ? O2 V C55 C56 -69.5(10) . . . . ? O1 V C55 C56 20.4(11) . . . . ? C23 V C55 C56 -7.8(11) . . . . ? O2 C55 C56 C57 68.4(3) . . . . ? N3 C55 C56 C57 -111.7(3) . . . . ? V C55 C56 C57 133.1(10) . . . . ? O2 C55 C56 C61 -104.7(3) . . . . ? N3 C55 C56 C61 75.1(3) . . . . ? V C55 C56 C61 -40.1(12) . . . . ? C61 C56 C57 C58 -2.0(3) . . . . ? C55 C56 C57 C58 -175.1(2) . . . . ? C61 C56 C57 C62 177.5(2) . . . . ? C55 C56 C57 C62 4.3(3) . . . . ? C56 C57 C58 C59 0.9(4) . . . . ? C62 C57 C58 C59 -178.6(2) . . . . ? C57 C58 C59 C60 0.4(4) . . . . ? C57 C58 C59 C63 -179.0(3) . . . . ? C58 C59 C60 C61 -0.6(4) . . . . ? C63 C59 C60 C61 178.8(3) . . . . ? C59 C60 C61 C56 -0.5(4) . . . . ? C59 C60 C61 C64 176.9(2) . . . . ? C57 C56 C61 C60 1.8(3) . . . . ? C55 C56 C61 C60 174.8(2) . . . . ? C57 C56 C61 C64 -175.5(2) . . . . ? C55 C56 C61 C64 -2.6(3) . . . . ? C75 C70 C71 C72 1.5(4) . . . . ? C69 C70 C71 C72 -175.4(3) . . . . ? C70 C71 C72 C73 -0.9(5) . . . . ? C71 C72 C73 C74 0.1(5) . . . . ? C72 C73 C74 C75 0.2(5) . . . . ? C71 C70 C75 C74 -1.2(5) . . . . ? C69 C70 C75 C74 175.6(3) . . . . ? C73 C74 C75 C70 0.4(5) . . . . ? C82 C77 C78 C79 4.0(6) . . . . ? C76 C77 C78 C79 179.7(4) . . . . ? C77 C78 C79 C80 -2.9(6) . . . . ? C78 C79 C80 C81 0.5(6) . . . . ? C79 C80 C81 C82 0.4(6) . . . . ? C80 C81 C82 C77 0.9(6) . . . . ? C78 C77 C82 C81 -3.0(6) . . . . ? C76 C77 C82 C81 -178.8(4) . . . . ? C89 C84 C85 C86 -3.9(6) . . . . ? C83 C84 C85 C86 177.1(4) . . . . ? C84 C85 C86 C87 4.1(7) . . . . ? C85 C86 C87 C88 -1.1(7) . . . . ? C86 C87 C88 C89 -1.9(7) . . . . ? C85 C84 C89 C88 0.9(5) . . . . ? C83 C84 C89 C88 179.9(3) . . . . ? C87 C88 C89 C84 2.0(6) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.554 _refine_diff_density_min -0.385 _refine_diff_density_rms 0.076 # Attachment '- compound 28.cif' data_compound28 _database_code_depnum_ccdc_archive 'CCDC 791872' #TrackingRef '- compound 28.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H70 N6 O2 V' _chemical_formula_sum 'C56 H70 N6 O2 V' _chemical_formula_weight 910.12 _chemical_absolute_configuration rmad 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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 13.7092(19) _cell_length_b 18.865(3) _cell_length_c 19.441(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5027.9(13) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 16945 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 27.9 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.202 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1948 _exptl_absorpt_coefficient_mu 0.244 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9259 _exptl_absorpt_correction_T_max 0.9437 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 52617 _diffrn_reflns_av_R_equivalents 0.0479 _diffrn_reflns_av_sigmaI/netI 0.0511 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 27.86 _reflns_number_total 11984 _reflns_number_gt 11267 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.8' _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^)+(0.0392P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00125(15) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.000(12) _refine_ls_number_reflns 11984 _refine_ls_number_parameters 605 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0844 _refine_ls_wR_factor_gt 0.0827 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _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 0.67724(2) 0.839464(14) 0.759268(14) 0.01677(7) Uani 1 1 d . . . N1 N 0.57318(10) 0.77711(7) 0.70890(7) 0.0168(3) Uani 1 1 d . . . N2 N 0.40645(11) 0.90333(8) 0.65923(8) 0.0231(3) Uani 1 1 d . . . N3 N 0.82443(10) 0.83719(7) 0.78835(6) 0.0162(3) Uani 1 1 d . . . N4 N 0.84593(11) 0.97639(7) 0.90181(8) 0.0235(3) Uani 1 1 d . . . N5 N 0.68010(11) 0.92623(7) 0.71373(7) 0.0218(3) Uani 1 1 d . . . N6 N 0.60193(11) 0.86793(8) 0.83485(8) 0.0237(3) Uani 1 1 d . . . O1 O 0.72075(8) 0.78433(6) 0.66802(6) 0.0181(2) Uani 1 1 d . . . O2 O 0.72978(8) 0.74754(6) 0.81312(6) 0.0197(3) Uani 1 1 d . . . C1 C 0.39741(12) 0.75129(8) 0.68514(8) 0.0176(3) Uani 1 1 d . . . C2 C 0.48088(12) 0.74755(9) 0.72714(8) 0.0174(3) Uani 1 1 d . . . C3 C 0.47377(13) 0.71912(9) 0.79321(9) 0.0227(4) Uani 1 1 d . . . H3 H 0.5303 0.7171 0.8214 0.027 Uiso 1 1 calc R . . C4 C 0.38610(13) 0.69382(10) 0.81839(9) 0.0269(4) Uani 1 1 d . . . H4 H 0.3825 0.6742 0.8633 0.032 Uiso 1 1 calc R . . C5 C 0.30350(13) 0.69737(9) 0.77746(9) 0.0228(4) Uani 1 1 d . . . H5 H 0.2432 0.6800 0.7947 0.027 Uiso 1 1 calc R . . C6 C 0.30746(12) 0.72589(9) 0.71152(9) 0.0204(4) Uani 1 1 d . . . C7 C 0.21401(13) 0.73338(10) 0.67149(10) 0.0278(4) Uani 1 1 d . . . H7A H 0.1597 0.7148 0.6988 0.042 Uiso 1 1 calc R . . H7B H 0.2191 0.7067 0.6284 0.042 Uiso 1 1 calc R . . H7C H 0.2025 0.7835 0.6612 0.042 Uiso 1 1 calc R . . C8 C 0.39832(12) 0.78150(9) 0.61365(9) 0.0194(4) Uani 1 1 d . . . C9 C 0.39902(12) 0.85571(9) 0.60236(9) 0.0210(4) Uani 1 1 d . . . C10 C 0.39463(14) 0.88088(10) 0.53481(10) 0.0279(4) Uani 1 1 d . . . H10 H 0.3966 0.9305 0.5266 0.033 Uiso 1 1 calc R . . C11 C 0.38753(14) 0.83487(11) 0.47973(9) 0.0310(4) Uani 1 1 d . . . H11 H 0.3835 0.8530 0.4342 0.037 Uiso 1 1 calc R . . C12 C 0.38622(13) 0.76293(11) 0.49056(9) 0.0288(4) Uani 1 1 d . . . H12 H 0.3817 0.7316 0.4524 0.035 Uiso 1 1 calc R . . C13 C 0.39147(12) 0.73536(10) 0.55719(9) 0.0235(4) Uani 1 1 d . . . C14 C 0.38863(14) 0.65549(10) 0.56669(10) 0.0308(4) Uani 1 1 d . . . H14A H 0.3232 0.6411 0.5814 0.046 Uiso 1 1 calc R . . H14B H 0.4362 0.6416 0.6018 0.046 Uiso 1 1 calc R . . H14C H 0.4047 0.6322 0.5231 0.046 Uiso 1 1 calc R . . C15 C 0.63895(12) 0.75125(9) 0.66590(8) 0.0171(3) Uani 1 1 d . . . C16 C 0.63166(12) 0.68869(9) 0.61926(9) 0.0188(4) Uani 1 1 d . . . C17 C 0.63151(12) 0.69969(9) 0.54754(9) 0.0204(4) Uani 1 1 d . . . C18 C 0.63610(13) 0.64113(10) 0.50461(9) 0.0242(4) Uani 1 1 d . . . H18 H 0.6347 0.6482 0.4562 0.029 Uiso 1 1 calc R . . C19 C 0.64272(13) 0.57224(10) 0.53009(10) 0.0267(4) Uani 1 1 d . . . C20 C 0.64366(13) 0.56334(9) 0.60099(10) 0.0250(4) Uani 1 1 d . . . H20 H 0.6484 0.5167 0.6192 0.030 Uiso 1 1 calc R . . C21 C 0.63792(12) 0.61988(9) 0.64608(9) 0.0213(4) Uani 1 1 d . . . C22 C 0.63015(13) 0.77352(9) 0.51817(9) 0.0238(4) Uani 1 1 d . . . H22A H 0.6959 0.7937 0.5202 0.036 Uiso 1 1 calc R . . H22B H 0.5854 0.8031 0.5450 0.036 Uiso 1 1 calc R . . H22C H 0.6082 0.7718 0.4702 0.036 Uiso 1 1 calc R . . C23 C 0.65166(17) 0.50942(11) 0.48219(11) 0.0402(5) Uani 1 1 d . . . H23A H 0.5868 0.4893 0.4737 0.060 Uiso 1 1 calc R . . H23B H 0.6935 0.4734 0.5033 0.060 Uiso 1 1 calc R . . H23C H 0.6804 0.5248 0.4385 0.060 Uiso 1 1 calc R . . C24 C 0.64138(15) 0.60707(9) 0.72283(9) 0.0285(4) Uani 1 1 d . . . H24A H 0.5748 0.6048 0.7410 0.043 Uiso 1 1 calc R . . H24B H 0.6766 0.6459 0.7452 0.043 Uiso 1 1 calc R . . H24C H 0.6750 0.5622 0.7321 0.043 Uiso 1 1 calc R . . C25 C 0.32205(15) 0.90425(10) 0.70536(10) 0.0310(4) Uani 1 1 d . . . H25A H 0.2643 0.9200 0.6799 0.047 Uiso 1 1 calc R . . H25B H 0.3346 0.9369 0.7436 0.047 Uiso 1 1 calc R . . H25C H 0.3108 0.8565 0.7235 0.047 Uiso 1 1 calc R . . C26 C 0.43260(15) 0.97632(10) 0.64107(11) 0.0336(5) Uani 1 1 d . . . H26A H 0.4878 0.9758 0.6090 0.050 Uiso 1 1 calc R . . H26B H 0.4509 1.0023 0.6828 0.050 Uiso 1 1 calc R . . H26C H 0.3766 0.9996 0.6193 0.050 Uiso 1 1 calc R . . C27 C 0.97825(12) 0.90730(9) 0.80602(9) 0.0184(3) Uani 1 1 d . . . C28 C 0.90852(11) 0.87404(8) 0.76396(9) 0.0166(3) Uani 1 1 d . . . C29 C 0.91570(12) 0.88049(9) 0.69214(9) 0.0202(4) Uani 1 1 d . . . H29 H 0.8704 0.8562 0.6637 0.024 Uiso 1 1 calc R . . C30 C 0.98729(13) 0.92139(10) 0.66239(9) 0.0254(4) Uani 1 1 d . . . H30 H 0.9919 0.9247 0.6137 0.030 Uiso 1 1 calc R . . C31 C 1.05268(13) 0.95777(9) 0.70368(10) 0.0241(4) Uani 1 1 d . . . H31 H 1.0999 0.9879 0.6831 0.029 Uiso 1 1 calc R . . C32 C 1.05017(13) 0.95071(9) 0.77495(9) 0.0222(4) Uani 1 1 d . . . C33 C 1.12437(14) 0.99082(10) 0.81778(10) 0.0296(4) Uani 1 1 d . . . H33A H 1.1807 0.9602 0.8268 0.044 Uiso 1 1 calc R . . H33B H 1.0946 1.0050 0.8615 0.044 Uiso 1 1 calc R . . H33C H 1.1457 1.0331 0.7927 0.044 Uiso 1 1 calc R . . C34 C 0.98428(13) 0.89667(9) 0.88278(9) 0.0202(4) Uani 1 1 d . . . C35 C 0.92170(13) 0.93212(9) 0.92859(9) 0.0219(4) Uani 1 1 d . . . C36 C 0.93472(14) 0.92359(9) 0.99950(9) 0.0267(4) Uani 1 1 d . . . H36 H 0.8926 0.9473 1.0307 0.032 Uiso 1 1 calc R . . C37 C 1.00869(15) 0.88072(10) 1.02446(10) 0.0313(5) Uani 1 1 d . . . H37 H 1.0172 0.8754 1.0727 0.038 Uiso 1 1 calc R . . C38 C 1.07005(14) 0.84574(10) 0.97982(9) 0.0282(4) Uani 1 1 d . . . H38 H 1.1203 0.8162 0.9975 0.034 Uiso 1 1 calc R . . C39 C 1.05913(13) 0.85324(9) 0.90858(9) 0.0242(4) Uani 1 1 d . . . C40 C 1.12802(14) 0.81317(10) 0.86165(10) 0.0298(4) Uani 1 1 d . . . H40A H 1.1793 0.8452 0.8454 0.045 Uiso 1 1 calc R . . H40B H 1.0917 0.7946 0.8222 0.045 Uiso 1 1 calc R . . H40C H 1.1576 0.7738 0.8870 0.045 Uiso 1 1 calc R . . C41 C 0.81760(13) 0.77129(8) 0.81008(8) 0.0174(3) Uani 1 1 d . . . C42 C 0.89921(12) 0.72318(8) 0.83093(8) 0.0172(3) Uani 1 1 d . . . C43 C 0.95547(13) 0.68727(9) 0.78167(9) 0.0194(4) Uani 1 1 d . . . C44 C 1.02705(13) 0.64022(9) 0.80412(9) 0.0211(4) Uani 1 1 d . . . H44 H 1.0650 0.6156 0.7710 0.025 Uiso 1 1 calc R . . C45 C 1.04448(14) 0.62835(9) 0.87361(9) 0.0239(4) Uani 1 1 d . . . C46 C 0.98491(13) 0.66253(9) 0.92099(9) 0.0235(4) Uani 1 1 d . . . H46 H 0.9945 0.6535 0.9686 0.028 Uiso 1 1 calc R . . C47 C 0.91178(13) 0.70939(9) 0.90138(8) 0.0196(4) Uani 1 1 d . . . C48 C 0.93864(14) 0.69805(10) 0.70517(9) 0.0252(4) Uani 1 1 d . . . H48A H 0.8691 0.7065 0.6967 0.038 Uiso 1 1 calc R . . H48B H 0.9595 0.6556 0.6801 0.038 Uiso 1 1 calc R . . H48C H 0.9764 0.7390 0.6893 0.038 Uiso 1 1 calc R . . C49 C 1.12539(15) 0.58047(10) 0.89729(10) 0.0332(5) Uani 1 1 d . . . H49A H 1.1837 0.6088 0.9070 0.050 Uiso 1 1 calc R . . H49B H 1.1402 0.5459 0.8612 0.050 Uiso 1 1 calc R . . H49C H 1.1051 0.5555 0.9391 0.050 Uiso 1 1 calc R . . C50 C 0.84721(13) 0.74303(10) 0.95485(9) 0.0260(4) Uani 1 1 d . . . H50A H 0.8408 0.7938 0.9452 0.039 Uiso 1 1 calc R . . H50B H 0.8762 0.7364 1.0005 0.039 Uiso 1 1 calc R . . H50C H 0.7827 0.7208 0.9536 0.039 Uiso 1 1 calc R . . C51 C 0.88042(15) 1.04499(9) 0.87605(11) 0.0326(5) Uani 1 1 d . . . H51A H 0.9050 1.0734 0.9145 0.049 Uiso 1 1 calc R . . H51B H 0.8264 1.0701 0.8538 0.049 Uiso 1 1 calc R . . H51C H 0.9329 1.0373 0.8426 0.049 Uiso 1 1 calc R . . C52 C 0.76263(15) 0.98632(11) 0.94729(11) 0.0344(5) Uani 1 1 d . . . H52A H 0.7427 0.9404 0.9662 0.052 Uiso 1 1 calc R . . H52B H 0.7084 1.0070 0.9213 0.052 Uiso 1 1 calc R . . H52C H 0.7808 1.0182 0.9849 0.052 Uiso 1 1 calc R . . C53 C 0.68383(15) 0.93524(10) 0.63937(9) 0.0277(4) Uani 1 1 d . . . H53A H 0.6519 0.9798 0.6267 0.042 Uiso 1 1 calc R . . H53B H 0.6501 0.8956 0.6171 0.042 Uiso 1 1 calc R . . H53C H 0.7520 0.9363 0.6243 0.042 Uiso 1 1 calc R . . C54 C 0.70659(16) 0.99141(10) 0.74943(10) 0.0357(5) Uani 1 1 d . . . H54A H 0.7730 1.0052 0.7365 0.054 Uiso 1 1 calc R . . H54B H 0.7035 0.9836 0.7992 0.054 Uiso 1 1 calc R . . H54C H 0.6611 1.0292 0.7366 0.054 Uiso 1 1 calc R . . C55 C 0.52165(16) 0.91817(11) 0.82997(11) 0.0410(5) Uani 1 1 d . . . H55A H 0.4596 0.8929 0.8352 0.061 Uiso 1 1 calc R . . H55B H 0.5234 0.9416 0.7850 0.061 Uiso 1 1 calc R . . H55C H 0.5279 0.9538 0.8664 0.061 Uiso 1 1 calc R . . C56 C 0.59887(15) 0.83326(12) 0.90197(9) 0.0355(5) Uani 1 1 d . . . H56A H 0.6085 0.8687 0.9382 0.053 Uiso 1 1 calc R . . H56B H 0.6507 0.7976 0.9046 0.053 Uiso 1 1 calc R . . H56C H 0.5354 0.8102 0.9081 0.053 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 0.01405(13) 0.01982(14) 0.01646(13) 0.00083(11) 0.00102(11) -0.00046(12) N1 0.0133(7) 0.0204(7) 0.0166(7) 0.0014(6) 0.0011(5) -0.0008(6) N2 0.0202(8) 0.0237(8) 0.0254(8) 0.0006(7) 0.0047(6) 0.0016(6) N3 0.0134(6) 0.0188(7) 0.0163(6) -0.0003(6) 0.0004(5) -0.0005(6) N4 0.0231(8) 0.0223(8) 0.0250(8) -0.0020(6) 0.0071(6) 0.0000(6) N5 0.0207(7) 0.0214(8) 0.0232(7) 0.0023(6) -0.0006(6) 0.0002(7) N6 0.0192(8) 0.0292(8) 0.0227(7) -0.0024(7) 0.0054(6) 0.0015(6) O1 0.0143(6) 0.0232(6) 0.0169(5) 0.0020(5) 0.0013(5) -0.0026(5) O2 0.0173(6) 0.0249(6) 0.0170(6) 0.0036(5) 0.0001(5) -0.0028(5) C1 0.0156(8) 0.0180(8) 0.0191(8) -0.0019(7) 0.0001(7) -0.0004(7) C2 0.0139(8) 0.0187(8) 0.0196(8) -0.0005(7) 0.0027(6) -0.0004(7) C3 0.0182(9) 0.0275(10) 0.0224(9) 0.0040(8) -0.0009(7) -0.0001(7) C4 0.0252(10) 0.0319(10) 0.0238(9) 0.0081(8) 0.0057(8) 0.0000(8) C5 0.0171(9) 0.0240(9) 0.0271(9) 0.0027(7) 0.0052(7) -0.0036(7) C6 0.0164(9) 0.0203(9) 0.0244(8) -0.0019(7) 0.0018(7) -0.0006(7) C7 0.0165(9) 0.0364(11) 0.0307(10) 0.0025(9) -0.0003(8) -0.0042(8) C8 0.0108(8) 0.0290(10) 0.0184(8) 0.0010(7) -0.0008(6) 0.0005(7) C9 0.0154(8) 0.0268(10) 0.0209(8) 0.0011(7) 0.0028(7) 0.0015(7) C10 0.0231(10) 0.0324(10) 0.0281(10) 0.0066(8) 0.0033(8) 0.0045(8) C11 0.0240(10) 0.0516(13) 0.0176(8) 0.0062(9) 0.0019(7) 0.0044(9) C12 0.0192(9) 0.0476(13) 0.0195(9) -0.0069(8) -0.0018(7) -0.0005(9) C13 0.0131(8) 0.0348(10) 0.0225(9) -0.0033(8) 0.0025(7) -0.0016(8) C14 0.0243(10) 0.0359(11) 0.0323(10) -0.0108(9) 0.0009(8) -0.0068(9) C15 0.0165(8) 0.0192(8) 0.0155(7) 0.0057(7) -0.0020(6) 0.0007(7) C16 0.0134(8) 0.0219(9) 0.0212(8) 0.0001(7) 0.0015(7) 0.0001(7) C17 0.0117(8) 0.0276(10) 0.0218(8) -0.0002(7) 0.0024(7) -0.0008(7) C18 0.0199(9) 0.0326(11) 0.0202(8) -0.0046(8) 0.0004(7) 0.0004(8) C19 0.0219(9) 0.0288(10) 0.0294(10) -0.0083(8) -0.0016(8) 0.0010(8) C20 0.0199(9) 0.0208(9) 0.0343(10) -0.0026(8) -0.0017(8) 0.0014(7) C21 0.0181(8) 0.0210(9) 0.0248(9) 0.0010(7) 0.0017(7) -0.0007(7) C22 0.0216(9) 0.0310(10) 0.0188(8) 0.0033(8) 0.0025(7) 0.0008(8) C23 0.0463(14) 0.0355(12) 0.0387(12) -0.0123(10) -0.0067(10) 0.0036(10) C24 0.0374(11) 0.0212(9) 0.0270(10) 0.0053(8) 0.0013(8) 0.0027(8) C25 0.0313(10) 0.0295(10) 0.0323(10) -0.0026(8) 0.0105(9) 0.0039(9) C26 0.0340(11) 0.0258(10) 0.0410(12) 0.0001(9) 0.0077(10) 0.0001(9) C27 0.0174(8) 0.0188(9) 0.0190(8) -0.0009(7) 0.0024(7) 0.0011(7) C28 0.0141(8) 0.0166(8) 0.0192(8) -0.0002(7) 0.0014(7) 0.0006(6) C29 0.0177(8) 0.0239(9) 0.0191(8) -0.0008(7) 0.0011(7) -0.0002(7) C30 0.0239(9) 0.0329(10) 0.0193(8) 0.0049(8) 0.0047(7) 0.0018(8) C31 0.0199(9) 0.0257(10) 0.0266(9) 0.0042(8) 0.0068(8) -0.0026(8) C32 0.0179(9) 0.0214(9) 0.0273(10) -0.0013(7) 0.0032(7) -0.0024(7) C33 0.0252(10) 0.0324(11) 0.0314(10) -0.0024(9) 0.0031(8) -0.0090(8) C34 0.0212(9) 0.0204(9) 0.0189(8) -0.0042(7) 0.0008(7) -0.0060(7) C35 0.0226(9) 0.0206(9) 0.0226(9) -0.0022(7) 0.0017(7) -0.0061(7) C36 0.0304(10) 0.0276(10) 0.0222(9) -0.0054(8) 0.0025(8) -0.0045(8) C37 0.0388(12) 0.0347(11) 0.0203(9) -0.0005(8) -0.0043(8) -0.0074(9) C38 0.0283(10) 0.0267(10) 0.0296(10) 0.0007(8) -0.0081(8) -0.0013(8) C39 0.0212(9) 0.0249(10) 0.0267(9) -0.0027(8) -0.0029(7) -0.0034(8) C40 0.0219(10) 0.0303(10) 0.0373(11) -0.0033(9) -0.0047(8) 0.0026(8) C41 0.0190(8) 0.0225(9) 0.0106(7) -0.0011(6) -0.0003(7) -0.0014(7) C42 0.0158(8) 0.0177(8) 0.0181(8) 0.0015(7) 0.0000(7) -0.0021(7) C43 0.0187(8) 0.0220(9) 0.0173(8) -0.0010(7) -0.0031(7) -0.0007(7) C44 0.0223(9) 0.0202(9) 0.0207(8) -0.0016(7) -0.0001(7) 0.0014(7) C45 0.0250(9) 0.0199(9) 0.0267(9) 0.0002(7) -0.0068(8) 0.0018(8) C46 0.0276(9) 0.0249(9) 0.0180(8) 0.0031(8) -0.0046(7) -0.0016(8) C47 0.0210(9) 0.0200(9) 0.0178(8) 0.0008(7) -0.0013(7) -0.0020(7) C48 0.0244(10) 0.0317(10) 0.0194(9) -0.0029(8) 0.0010(7) 0.0062(8) C49 0.0334(11) 0.0348(11) 0.0314(10) 0.0013(9) -0.0063(9) 0.0109(9) C50 0.0271(10) 0.0336(10) 0.0174(8) 0.0014(8) -0.0005(7) 0.0009(8) C51 0.0357(12) 0.0224(10) 0.0398(11) 0.0002(9) 0.0044(9) 0.0002(9) C52 0.0302(11) 0.0407(11) 0.0323(11) -0.0057(9) 0.0093(9) 0.0025(9) C53 0.0327(10) 0.0256(9) 0.0248(9) 0.0064(8) -0.0063(9) -0.0008(9) C54 0.0520(13) 0.0264(10) 0.0287(10) -0.0007(9) 0.0001(10) -0.0050(9) C55 0.0325(11) 0.0475(13) 0.0430(12) 0.0043(10) 0.0131(10) 0.0161(10) C56 0.0325(11) 0.0532(13) 0.0209(9) -0.0015(9) 0.0065(8) 0.0031(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 N5 1.8614(14) . ? V1 N6 1.8745(14) . ? V1 N1 2.0924(14) . ? V1 N3 2.0959(14) . ? V1 O1 2.1411(12) . ? V1 O2 2.1499(12) . ? V1 C41 2.5163(17) . ? V1 C15 2.5178(17) . ? N1 C15 1.323(2) . ? N1 C2 1.428(2) . ? N2 C9 1.428(2) . ? N2 C25 1.464(2) . ? N2 C26 1.466(2) . ? N3 C41 1.316(2) . ? N3 C28 1.427(2) . ? N4 C35 1.431(2) . ? N4 C52 1.456(2) . ? N4 C51 1.466(2) . ? N5 C53 1.456(2) . ? N5 C54 1.458(2) . ? N6 C55 1.455(2) . ? N6 C56 1.460(2) . ? O1 C15 1.2840(19) . ? O2 C41 1.286(2) . ? C1 C2 1.408(2) . ? C1 C6 1.419(2) . ? C1 C8 1.502(2) . ? C2 C3 1.395(2) . ? C3 C4 1.383(2) . ? C3 H3 0.9500 . ? C4 C5 1.386(3) . ? C4 H4 0.9500 . ? C5 C6 1.391(2) . ? C5 H5 0.9500 . ? C6 C7 1.506(2) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C13 1.404(2) . ? C8 C9 1.417(3) . ? C9 C10 1.398(2) . ? C10 C11 1.382(3) . ? C10 H10 0.9500 . ? C11 C12 1.374(3) . ? C11 H11 0.9500 . ? C12 C13 1.398(2) . ? C12 H12 0.9500 . ? C13 C14 1.518(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 C16 1.492(2) . ? C16 C21 1.402(2) . ? C16 C17 1.410(2) . ? C17 C18 1.386(2) . ? C17 C22 1.505(2) . ? C18 C19 1.394(3) . ? C18 H18 0.9500 . ? C19 C20 1.389(3) . ? C19 C23 1.512(3) . ? C20 C21 1.383(2) . ? C20 H20 0.9500 . ? C21 C24 1.512(2) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.406(2) . ? C27 C32 1.417(2) . ? C27 C34 1.508(2) . ? C28 C29 1.405(2) . ? C29 C30 1.376(2) . ? C29 H29 0.9500 . ? C30 C31 1.385(3) . ? C30 H30 0.9500 . ? C31 C32 1.392(2) . ? C31 H31 0.9500 . ? C32 C33 1.517(3) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C39 1.406(2) . ? C34 C35 1.406(2) . ? C35 C36 1.399(2) . ? C36 C37 1.385(3) . ? C36 H36 0.9500 . ? C37 C38 1.377(3) . ? C37 H37 0.9500 . ? C38 C39 1.400(2) . ? C38 H38 0.9500 . ? C39 C40 1.515(3) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.497(2) . ? C42 C43 1.404(2) . ? C42 C47 1.405(2) . ? C43 C44 1.393(2) . ? C43 C48 1.519(2) . ? C44 C45 1.390(2) . ? C44 H44 0.9500 . ? C45 C46 1.390(3) . ? C45 C49 1.503(2) . ? C46 C47 1.390(2) . ? C46 H46 0.9500 . ? C47 C50 1.506(2) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 V1 N6 97.61(7) . . ? N5 V1 N1 106.63(6) . . ? N6 V1 N1 98.76(6) . . ? N5 V1 N3 97.24(6) . . ? N6 V1 N3 108.95(6) . . ? N1 V1 N3 140.46(5) . . ? N5 V1 O1 91.56(5) . . ? N6 V1 O1 160.40(6) . . ? N1 V1 O1 61.91(5) . . ? N3 V1 O1 86.87(5) . . ? N5 V1 O2 159.05(6) . . ? N6 V1 O2 91.94(6) . . ? N1 V1 O2 90.16(5) . . ? N3 V1 O2 61.94(5) . . ? O1 V1 O2 85.31(5) . . ? N5 V1 C41 128.32(6) . . ? N6 V1 C41 105.07(6) . . ? N1 V1 C41 114.69(5) . . ? N3 V1 C41 31.52(5) . . ? O1 V1 C41 82.18(5) . . ? O2 V1 C41 30.73(5) . . ? N5 V1 C15 104.05(6) . . ? N6 V1 C15 129.76(6) . . ? N1 V1 C15 31.66(5) . . ? N3 V1 C15 112.44(5) . . ? O1 V1 C15 30.66(5) . . ? O2 V1 C15 83.56(5) . . ? C41 V1 C15 96.01(5) . . ? C15 N1 C2 128.11(14) . . ? C15 N1 V1 92.19(10) . . ? C2 N1 V1 135.05(11) . . ? C9 N2 C25 115.17(15) . . ? C9 N2 C26 114.95(15) . . ? C25 N2 C26 109.25(14) . . ? C41 N3 C28 128.61(14) . . ? C41 N3 V1 92.15(10) . . ? C28 N3 V1 132.69(10) . . ? C35 N4 C52 115.04(15) . . ? C35 N4 C51 113.92(15) . . ? C52 N4 C51 110.29(15) . . ? C53 N5 C54 111.44(14) . . ? C53 N5 V1 125.13(11) . . ? C54 N5 V1 121.36(12) . . ? C55 N6 C56 109.16(15) . . ? C55 N6 V1 123.51(13) . . ? C56 N6 V1 126.01(12) . . ? C15 O1 V1 91.11(10) . . ? C41 O2 V1 90.58(9) . . ? C2 C1 C6 118.68(15) . . ? C2 C1 C8 123.30(15) . . ? C6 C1 C8 118.02(15) . . ? C3 C2 C1 119.77(15) . . ? C3 C2 N1 116.16(15) . . ? C1 C2 N1 123.84(14) . . ? C4 C3 C2 121.28(17) . . ? C4 C3 H3 119.4 . . ? C2 C3 H3 119.4 . . ? C3 C4 C5 119.37(16) . . ? C3 C4 H4 120.3 . . ? C5 C4 H4 120.3 . . ? C4 C5 C6 121.06(16) . . ? C4 C5 H5 119.5 . . ? C6 C5 H5 119.5 . . ? C5 C6 C1 119.84(16) . . ? C5 C6 C7 118.64(16) . . ? C1 C6 C7 121.40(15) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C13 C8 C9 119.46(16) . . ? C13 C8 C1 119.19(15) . . ? C9 C8 C1 121.20(15) . . ? C10 C9 C8 118.74(16) . . ? C10 C9 N2 121.11(16) . . ? C8 C9 N2 120.13(15) . . ? C11 C10 C9 121.18(17) . . ? C11 C10 H10 119.4 . . ? C9 C10 H10 119.4 . . ? C12 C11 C10 120.19(17) . . ? C12 C11 H11 119.9 . . ? C10 C11 H11 119.9 . . ? C11 C12 C13 120.60(17) . . ? C11 C12 H12 119.7 . . ? C13 C12 H12 119.7 . . ? C12 C13 C8 119.82(17) . . ? C12 C13 C14 118.72(16) . . ? C8 C13 C14 121.45(16) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O1 C15 N1 113.32(15) . . ? O1 C15 C16 117.55(14) . . ? N1 C15 C16 129.07(15) . . ? O1 C15 V1 58.23(8) . . ? N1 C15 V1 56.14(9) . . ? C16 C15 V1 167.19(12) . . ? C21 C16 C17 120.30(16) . . ? C21 C16 C15 120.17(15) . . ? C17 C16 C15 119.00(15) . . ? C18 C17 C16 118.57(16) . . ? C18 C17 C22 120.64(16) . . ? C16 C17 C22 120.75(15) . . ? C17 C18 C19 122.15(17) . . ? C17 C18 H18 118.9 . . ? C19 C18 H18 118.9 . . ? C20 C19 C18 117.79(17) . . ? C20 C19 C23 121.04(18) . . ? C18 C19 C23 121.15(17) . . ? C21 C20 C19 122.36(17) . . ? C21 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? C20 C21 C16 118.82(16) . . ? C20 C21 C24 120.02(16) . . ? C16 C21 C24 121.13(15) . . ? C17 C22 H22A 109.5 . . ? C17 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C17 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N2 C25 H25A 109.5 . . ? N2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N2 C26 H26A 109.5 . . ? N2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C32 118.90(15) . . ? C28 C27 C34 123.61(15) . . ? C32 C27 C34 117.42(15) . . ? C29 C28 C27 119.46(16) . . ? C29 C28 N3 115.40(14) . . ? C27 C28 N3 124.99(15) . . ? C30 C29 C28 121.09(17) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C29 C30 C31 119.72(17) . . ? C29 C30 H30 120.1 . . ? C31 C30 H30 120.1 . . ? C30 C31 C32 120.88(17) . . ? C30 C31 H31 119.6 . . ? C32 C31 H31 119.6 . . ? C31 C32 C27 119.78(16) . . ? C31 C32 C33 118.81(17) . . ? C27 C32 C33 121.41(16) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C39 C34 C35 119.78(16) . . ? C39 C34 C27 118.08(15) . . ? C35 C34 C27 122.02(16) . . ? C36 C35 C34 119.44(17) . . ? C36 C35 N4 121.22(16) . . ? C34 C35 N4 119.34(16) . . ? C37 C36 C35 120.39(17) . . ? C37 C36 H36 119.8 . . ? C35 C36 H36 119.8 . . ? C38 C37 C36 120.42(18) . . ? C38 C37 H37 119.8 . . ? C36 C37 H37 119.8 . . ? C37 C38 C39 120.64(18) . . ? C37 C38 H38 119.7 . . ? C39 C38 H38 119.7 . . ? C38 C39 C34 119.33(17) . . ? C38 C39 C40 118.59(17) . . ? C34 C39 C40 122.07(16) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O2 C41 N3 114.23(15) . . ? O2 C41 C42 118.43(14) . . ? N3 C41 C42 127.33(15) . . ? O2 C41 V1 58.69(8) . . ? N3 C41 V1 56.34(9) . . ? C42 C41 V1 171.09(11) . . ? C43 C42 C47 120.55(15) . . ? C43 C42 C41 121.24(15) . . ? C47 C42 C41 117.91(14) . . ? C44 C43 C42 118.73(15) . . ? C44 C43 C48 119.94(15) . . ? C42 C43 C48 121.33(16) . . ? C45 C44 C43 121.88(16) . . ? C45 C44 H44 119.1 . . ? C43 C44 H44 119.1 . . ? C46 C45 C44 117.93(16) . . ? C46 C45 C49 120.64(16) . . ? C44 C45 C49 121.43(17) . . ? C45 C46 C47 122.49(16) . . ? C45 C46 H46 118.8 . . ? C47 C46 H46 118.8 . . ? C46 C47 C42 118.28(15) . . ? C46 C47 C50 120.18(15) . . ? C42 C47 C50 121.54(15) . . ? C43 C48 H48A 109.5 . . ? C43 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C43 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C45 C49 H49A 109.5 . . ? C45 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C45 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C47 C50 H50A 109.5 . . ? C47 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C47 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N4 C51 H51A 109.5 . . ? N4 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N4 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N4 C52 H52A 109.5 . . ? N4 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N4 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N5 C53 H53A 109.5 . . ? N5 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? N5 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? N5 C54 H54A 109.5 . . ? N5 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? N5 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N6 C55 H55A 109.5 . . ? N6 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? N6 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N6 C56 H56A 109.5 . . ? N6 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N6 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 V1 N1 C15 89.90(10) . . . . ? N6 V1 N1 C15 -169.38(10) . . . . ? N3 V1 N1 C15 -34.73(13) . . . . ? O1 V1 N1 C15 7.21(9) . . . . ? O2 V1 N1 C15 -77.39(10) . . . . ? C41 V1 N1 C15 -58.26(11) . . . . ? N5 V1 N1 C2 -114.24(15) . . . . ? N6 V1 N1 C2 -13.52(16) . . . . ? N3 V1 N1 C2 121.13(15) . . . . ? O1 V1 N1 C2 163.07(16) . . . . ? O2 V1 N1 C2 78.47(15) . . . . ? C41 V1 N1 C2 97.60(15) . . . . ? C15 V1 N1 C2 155.9(2) . . . . ? N5 V1 N3 C41 -171.31(9) . . . . ? N6 V1 N3 C41 88.04(10) . . . . ? N1 V1 N3 C41 -43.94(13) . . . . ? O1 V1 N3 C41 -80.13(9) . . . . ? O2 V1 N3 C41 6.23(8) . . . . ? C15 V1 N3 C41 -62.82(10) . . . . ? N5 V1 N3 C28 -19.16(15) . . . . ? N6 V1 N3 C28 -119.81(14) . . . . ? N1 V1 N3 C28 108.21(14) . . . . ? O1 V1 N3 C28 72.02(14) . . . . ? O2 V1 N3 C28 158.38(15) . . . . ? C41 V1 N3 C28 152.15(19) . . . . ? C15 V1 N3 C28 89.33(14) . . . . ? N6 V1 N5 C53 -148.03(15) . . . . ? N1 V1 N5 C53 -46.48(16) . . . . ? N3 V1 N5 C53 101.65(15) . . . . ? O1 V1 N5 C53 14.61(15) . . . . ? O2 V1 N5 C53 95.5(2) . . . . ? C41 V1 N5 C53 95.87(16) . . . . ? C15 V1 N5 C53 -13.72(16) . . . . ? N6 V1 N5 C54 49.77(15) . . . . ? N1 V1 N5 C54 151.33(14) . . . . ? N3 V1 N5 C54 -60.55(15) . . . . ? O1 V1 N5 C54 -147.59(14) . . . . ? O2 V1 N5 C54 -66.6(2) . . . . ? C41 V1 N5 C54 -66.33(16) . . . . ? C15 V1 N5 C54 -175.91(14) . . . . ? N5 V1 N6 C55 36.92(16) . . . . ? N1 V1 N6 C55 -71.31(16) . . . . ? N3 V1 N6 C55 137.31(15) . . . . ? O1 V1 N6 C55 -80.3(2) . . . . ? O2 V1 N6 C55 -161.77(15) . . . . ? C41 V1 N6 C55 170.06(15) . . . . ? C15 V1 N6 C55 -78.54(17) . . . . ? N5 V1 N6 C56 -157.67(15) . . . . ? N1 V1 N6 C56 94.11(15) . . . . ? N3 V1 N6 C56 -57.28(16) . . . . ? O1 V1 N6 C56 85.1(2) . . . . ? O2 V1 N6 C56 3.64(15) . . . . ? C41 V1 N6 C56 -24.53(16) . . . . ? C15 V1 N6 C56 86.88(16) . . . . ? N5 V1 O1 C15 -115.48(10) . . . . ? N6 V1 O1 C15 2.7(2) . . . . ? N1 V1 O1 C15 -7.42(9) . . . . ? N3 V1 O1 C15 147.35(9) . . . . ? O2 V1 O1 C15 85.27(9) . . . . ? C41 V1 O1 C15 116.03(10) . . . . ? N5 V1 O2 C41 0.5(2) . . . . ? N6 V1 O2 C41 -116.86(10) . . . . ? N1 V1 O2 C41 144.36(9) . . . . ? N3 V1 O2 C41 -6.37(9) . . . . ? O1 V1 O2 C41 82.57(9) . . . . ? C15 V1 O2 C41 113.33(9) . . . . ? C6 C1 C2 C3 0.1(2) . . . . ? C8 C1 C2 C3 179.58(15) . . . . ? C6 C1 C2 N1 -174.08(14) . . . . ? C8 C1 C2 N1 5.4(3) . . . . ? C15 N1 C2 C3 107.77(19) . . . . ? V1 N1 C2 C3 -40.9(2) . . . . ? C15 N1 C2 C1 -77.8(2) . . . . ? V1 N1 C2 C1 133.44(15) . . . . ? C1 C2 C3 C4 0.5(3) . . . . ? N1 C2 C3 C4 175.14(16) . . . . ? C2 C3 C4 C5 -0.6(3) . . . . ? C3 C4 C5 C6 0.0(3) . . . . ? C4 C5 C6 C1 0.6(3) . . . . ? C4 C5 C6 C7 -175.46(17) . . . . ? C2 C1 C6 C5 -0.6(2) . . . . ? C8 C1 C6 C5 179.86(15) . . . . ? C2 C1 C6 C7 175.28(16) . . . . ? C8 C1 C6 C7 -4.2(2) . . . . ? C2 C1 C8 C13 106.64(19) . . . . ? C6 C1 C8 C13 -73.9(2) . . . . ? C2 C1 C8 C9 -77.8(2) . . . . ? C6 C1 C8 C9 101.62(19) . . . . ? C13 C8 C9 C10 -1.2(2) . . . . ? C1 C8 C9 C10 -176.66(15) . . . . ? C13 C8 C9 N2 -179.68(15) . . . . ? C1 C8 C9 N2 4.8(2) . . . . ? C25 N2 C9 C10 114.21(19) . . . . ? C26 N2 C9 C10 -14.1(2) . . . . ? C25 N2 C9 C8 -67.3(2) . . . . ? C26 N2 C9 C8 164.35(16) . . . . ? C8 C9 C10 C11 1.4(3) . . . . ? N2 C9 C10 C11 179.94(17) . . . . ? C9 C10 C11 C12 -1.0(3) . . . . ? C10 C11 C12 C13 0.4(3) . . . . ? C11 C12 C13 C8 -0.1(3) . . . . ? C11 C12 C13 C14 179.32(17) . . . . ? C9 C8 C13 C12 0.5(2) . . . . ? C1 C8 C13 C12 176.10(16) . . . . ? C9 C8 C13 C14 -178.89(15) . . . . ? C1 C8 C13 C14 -3.3(2) . . . . ? V1 O1 C15 N1 11.32(14) . . . . ? V1 O1 C15 C16 -166.06(13) . . . . ? C2 N1 C15 O1 -170.05(14) . . . . ? V1 N1 C15 O1 -11.60(14) . . . . ? C2 N1 C15 C16 7.0(3) . . . . ? V1 N1 C15 C16 165.42(15) . . . . ? C2 N1 C15 V1 -158.46(18) . . . . ? N5 V1 C15 O1 68.47(10) . . . . ? N6 V1 C15 O1 -178.84(9) . . . . ? N1 V1 C15 O1 167.46(15) . . . . ? N3 V1 C15 O1 -35.65(10) . . . . ? O2 V1 C15 O1 -91.68(9) . . . . ? C41 V1 C15 O1 -63.52(9) . . . . ? N5 V1 C15 N1 -98.99(10) . . . . ? N6 V1 C15 N1 13.71(13) . . . . ? N3 V1 C15 N1 156.90(9) . . . . ? O1 V1 C15 N1 -167.46(15) . . . . ? O2 V1 C15 N1 100.87(10) . . . . ? C41 V1 C15 N1 129.02(10) . . . . ? N5 V1 C15 C16 142.8(5) . . . . ? N6 V1 C15 C16 -104.5(5) . . . . ? N1 V1 C15 C16 -118.2(6) . . . . ? N3 V1 C15 C16 38.7(5) . . . . ? O1 V1 C15 C16 74.4(5) . . . . ? O2 V1 C15 C16 -17.3(5) . . . . ? C41 V1 C15 C16 10.8(5) . . . . ? O1 C15 C16 C21 101.45(18) . . . . ? N1 C15 C16 C21 -75.5(2) . . . . ? V1 C15 C16 C21 34.0(6) . . . . ? O1 C15 C16 C17 -70.2(2) . . . . ? N1 C15 C16 C17 112.9(2) . . . . ? V1 C15 C16 C17 -137.6(5) . . . . ? C21 C16 C17 C18 1.0(2) . . . . ? C15 C16 C17 C18 172.65(15) . . . . ? C21 C16 C17 C22 -176.76(16) . . . . ? C15 C16 C17 C22 -5.1(2) . . . . ? C16 C17 C18 C19 -1.3(3) . . . . ? C22 C17 C18 C19 176.51(17) . . . . ? C17 C18 C19 C20 0.6(3) . . . . ? C17 C18 C19 C23 -177.55(17) . . . . ? C18 C19 C20 C21 0.3(3) . . . . ? C23 C19 C20 C21 178.45(18) . . . . ? C19 C20 C21 C16 -0.5(3) . . . . ? C19 C20 C21 C24 -178.73(17) . . . . ? C17 C16 C21 C20 -0.2(2) . . . . ? C15 C16 C21 C20 -171.70(16) . . . . ? C17 C16 C21 C24 178.06(16) . . . . ? C15 C16 C21 C24 6.5(2) . . . . ? C32 C27 C28 C29 4.4(2) . . . . ? C34 C27 C28 C29 -172.47(16) . . . . ? C32 C27 C28 N3 -170.83(15) . . . . ? C34 C27 C28 N3 12.3(3) . . . . ? C41 N3 C28 C29 101.28(19) . . . . ? V1 N3 C28 C29 -42.0(2) . . . . ? C41 N3 C28 C27 -83.3(2) . . . . ? V1 N3 C28 C27 133.38(15) . . . . ? C27 C28 C29 C30 -2.9(3) . . . . ? N3 C28 C29 C30 172.77(15) . . . . ? C28 C29 C30 C31 -1.0(3) . . . . ? C29 C30 C31 C32 3.3(3) . . . . ? C30 C31 C32 C27 -1.7(3) . . . . ? C30 C31 C32 C33 179.08(17) . . . . ? C28 C27 C32 C31 -2.2(3) . . . . ? C34 C27 C32 C31 174.92(17) . . . . ? C28 C27 C32 C33 177.03(16) . . . . ? C34 C27 C32 C33 -5.9(2) . . . . ? C28 C27 C34 C39 104.4(2) . . . . ? C32 C27 C34 C39 -72.5(2) . . . . ? C28 C27 C34 C35 -79.6(2) . . . . ? C32 C27 C34 C35 103.48(19) . . . . ? C39 C34 C35 C36 -0.1(3) . . . . ? C27 C34 C35 C36 -176.00(16) . . . . ? C39 C34 C35 N4 179.80(15) . . . . ? C27 C34 C35 N4 3.9(2) . . . . ? C52 N4 C35 C36 -24.9(2) . . . . ? C51 N4 C35 C36 103.82(19) . . . . ? C52 N4 C35 C34 155.18(16) . . . . ? C51 N4 C35 C34 -76.1(2) . . . . ? C34 C35 C36 C37 0.1(3) . . . . ? N4 C35 C36 C37 -179.77(16) . . . . ? C35 C36 C37 C38 -0.3(3) . . . . ? C36 C37 C38 C39 0.4(3) . . . . ? C37 C38 C39 C34 -0.4(3) . . . . ? C37 C38 C39 C40 -179.53(17) . . . . ? C35 C34 C39 C38 0.2(3) . . . . ? C27 C34 C39 C38 176.27(16) . . . . ? C35 C34 C39 C40 179.35(16) . . . . ? C27 C34 C39 C40 -4.6(3) . . . . ? V1 O2 C41 N3 9.84(13) . . . . ? V1 O2 C41 C42 -170.27(12) . . . . ? C28 N3 C41 O2 -164.04(14) . . . . ? V1 N3 C41 O2 -10.10(13) . . . . ? C28 N3 C41 C42 16.1(3) . . . . ? V1 N3 C41 C42 170.01(14) . . . . ? C28 N3 C41 V1 -153.93(17) . . . . ? N5 V1 C41 O2 -179.78(9) . . . . ? N6 V1 C41 O2 67.41(10) . . . . ? N1 V1 C41 O2 -39.89(10) . . . . ? N3 V1 C41 O2 169.21(15) . . . . ? O1 V1 C41 O2 -93.99(9) . . . . ? C15 V1 C41 O2 -66.56(9) . . . . ? N5 V1 C41 N3 11.01(12) . . . . ? N6 V1 C41 N3 -101.79(10) . . . . ? N1 V1 C41 N3 150.90(9) . . . . ? O1 V1 C41 N3 96.80(9) . . . . ? O2 V1 C41 N3 -169.21(15) . . . . ? C15 V1 C41 N3 124.23(9) . . . . ? N5 V1 C41 C42 -106.1(8) . . . . ? N6 V1 C41 C42 141.1(8) . . . . ? N1 V1 C41 C42 33.8(8) . . . . ? N3 V1 C41 C42 -117.1(8) . . . . ? O1 V1 C41 C42 -20.3(8) . . . . ? O2 V1 C41 C42 73.6(8) . . . . ? C15 V1 C41 C42 7.1(8) . . . . ? O2 C41 C42 C43 100.00(19) . . . . ? N3 C41 C42 C43 -80.1(2) . . . . ? V1 C41 C42 C43 31.2(9) . . . . ? O2 C41 C42 C47 -73.7(2) . . . . ? N3 C41 C42 C47 106.13(19) . . . . ? V1 C41 C42 C47 -142.5(7) . . . . ? C47 C42 C43 C44 -3.0(3) . . . . ? C41 C42 C43 C44 -176.57(15) . . . . ? C47 C42 C43 C48 176.15(16) . . . . ? C41 C42 C43 C48 2.6(3) . . . . ? C42 C43 C44 C45 -0.4(3) . . . . ? C48 C43 C44 C45 -179.55(17) . . . . ? C43 C44 C45 C46 3.0(3) . . . . ? C43 C44 C45 C49 -176.69(17) . . . . ? C44 C45 C46 C47 -2.3(3) . . . . ? C49 C45 C46 C47 177.41(17) . . . . ? C45 C46 C47 C42 -1.0(3) . . . . ? C45 C46 C47 C50 177.94(17) . . . . ? C43 C42 C47 C46 3.7(3) . . . . ? C41 C42 C47 C46 177.45(15) . . . . ? C43 C42 C47 C50 -175.27(16) . . . . ? C41 C42 C47 C50 -1.5(2) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 27.86 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.206 _refine_diff_density_min -0.264 _refine_diff_density_rms 0.040 # Attachment '- compound 29.cif' data_compound29 _database_code_depnum_ccdc_archive 'CCDC 791873' #TrackingRef '- compound 29.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H69 N6 Nb O2' _chemical_formula_sum 'C56 H69 N6 Nb O2' _chemical_formula_weight 951.08 _chemical_absolute_configuration rmad 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' Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 13.1691(3) _cell_length_b 13.4302(4) _cell_length_c 32.5935(9) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5764.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 14984 _cell_measurement_theta_min 1.2 _cell_measurement_theta_max 27.9 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.096 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2016 _exptl_absorpt_coefficient_mu 0.250 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9379 _exptl_absorpt_correction_T_max 0.9471 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Rigaku Saturn CCD area detector' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 41838 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_sigmaI/netI 0.0562 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -41 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 27.88 _reflns_number_total 13705 _reflns_number_gt 12696 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.8' _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^)+(0.0617P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.02(2) _refine_ls_number_reflns 13705 _refine_ls_number_parameters 603 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0466 _refine_ls_R_factor_gt 0.0433 _refine_ls_wR_factor_ref 0.1153 _refine_ls_wR_factor_gt 0.1132 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _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 Nb1 Nb 0.633694(16) 0.880205(15) 0.061200(7) 0.02425(7) Uani 1 1 d . . . O1 O 0.55322(16) 0.96217(13) 0.11001(6) 0.0317(4) Uani 1 1 d . . . O2 O 0.76029(14) 0.91040(13) 0.10177(6) 0.0290(4) Uani 1 1 d . . . N1 N 0.53390(17) 0.80045(16) 0.10474(7) 0.0246(5) Uani 1 1 d . . . N2 N 0.70842(19) 0.65667(17) 0.14478(8) 0.0369(6) Uani 1 1 d . . . N3 N 0.72191(16) 1.02555(14) 0.05722(7) 0.0244(4) Uani 1 1 d . . . N4 N 0.54114(19) 1.20124(18) 0.08682(8) 0.0370(6) Uani 1 1 d . . . N5 N 0.67700(18) 0.75371(17) 0.03910(7) 0.0313(5) Uani 1 1 d . . . N6 N 0.53351(18) 0.91791(19) 0.01877(8) 0.0341(5) Uani 1 1 d . . . C1 C 0.4917(2) 0.64442(19) 0.14254(8) 0.0263(5) Uani 1 1 d . . . C2 C 0.48564(19) 0.70583(18) 0.10786(8) 0.0249(5) Uani 1 1 d . . . C3 C 0.4361(2) 0.6726(2) 0.07263(8) 0.0285(6) Uani 1 1 d . . . H3 H 0.4332 0.7140 0.0490 0.034 Uiso 1 1 calc R . . C4 C 0.3914(2) 0.5797(2) 0.07194(9) 0.0330(6) Uani 1 1 d . . . H4 H 0.3573 0.5575 0.0479 0.040 Uiso 1 1 calc R . . C5 C 0.3961(2) 0.5190(2) 0.10606(9) 0.0354(6) Uani 1 1 d . . . H5 H 0.3644 0.4554 0.1056 0.042 Uiso 1 1 calc R . . C6 C 0.4468(2) 0.5501(2) 0.14102(9) 0.0319(6) Uani 1 1 d . . . C7 C 0.4521(3) 0.4778(2) 0.17678(10) 0.0443(8) Uani 1 1 d . . . H7A H 0.4049 0.4992 0.1983 0.066 Uiso 1 1 calc R . . H7B H 0.5214 0.4767 0.1878 0.066 Uiso 1 1 calc R . . H7C H 0.4334 0.4110 0.1674 0.066 Uiso 1 1 calc R . . C8 C 0.5474(2) 0.67707(19) 0.18014(8) 0.0318(6) Uani 1 1 d . . . C9 C 0.6542(2) 0.6837(2) 0.18034(9) 0.0346(6) Uani 1 1 d . . . C10 C 0.7036(3) 0.7169(2) 0.21594(11) 0.0468(8) Uani 1 1 d . . . H10 H 0.7754 0.7234 0.2158 0.056 Uiso 1 1 calc R . . C11 C 0.6509(3) 0.7400(3) 0.25069(11) 0.0544(10) Uani 1 1 d . . . H11 H 0.6859 0.7613 0.2746 0.065 Uiso 1 1 calc R . . C12 C 0.5447(3) 0.7322(3) 0.25091(11) 0.0501(9) Uani 1 1 d . . . H12 H 0.5083 0.7483 0.2752 0.060 Uiso 1 1 calc R . . C13 C 0.4916(3) 0.7012(2) 0.21626(9) 0.0377(7) Uani 1 1 d . . . C14 C 0.3790(2) 0.6952(2) 0.21777(9) 0.0390(7) Uani 1 1 d . . . H14A H 0.3518 0.6953 0.1898 0.059 Uiso 1 1 calc R . . H14B H 0.3522 0.7527 0.2328 0.059 Uiso 1 1 calc R . . H14C H 0.3587 0.6337 0.2317 0.059 Uiso 1 1 calc R . . C15 C 0.8105(3) 0.6979(3) 0.14063(12) 0.0484(8) Uani 1 1 d . . . H15A H 0.8077 0.7704 0.1439 0.073 Uiso 1 1 calc R . . H15B H 0.8375 0.6816 0.1134 0.073 Uiso 1 1 calc R . . H15C H 0.8546 0.6695 0.1618 0.073 Uiso 1 1 calc R . . C16 C 0.7135(3) 0.5472(2) 0.13924(11) 0.0458(8) Uani 1 1 d . . . H16A H 0.7549 0.5180 0.1611 0.069 Uiso 1 1 calc R . . H16B H 0.7442 0.5320 0.1126 0.069 Uiso 1 1 calc R . . H16C H 0.6448 0.5193 0.1404 0.069 Uiso 1 1 calc R . . C17 C 0.5030(2) 0.8842(2) 0.12182(8) 0.0284(5) Uani 1 1 d . . . C18 C 0.4190(2) 0.90065(19) 0.15125(8) 0.0298(6) Uani 1 1 d . . . C19 C 0.4435(2) 0.9405(2) 0.19006(9) 0.0319(6) Uani 1 1 d . . . C20 C 0.3656(3) 0.9625(2) 0.21702(9) 0.0367(6) Uani 1 1 d . . . H20 H 0.3816 0.9887 0.2433 0.044 Uiso 1 1 calc R . . C21 C 0.2642(3) 0.9473(2) 0.20656(10) 0.0412(7) Uani 1 1 d . . . C22 C 0.2414(2) 0.9119(2) 0.16773(10) 0.0409(7) Uani 1 1 d . . . H22 H 0.1723 0.9024 0.1603 0.049 Uiso 1 1 calc R . . C23 C 0.3168(2) 0.8897(2) 0.13921(9) 0.0339(6) Uani 1 1 d . . . C24 C 0.5517(2) 0.9598(2) 0.20210(10) 0.0406(7) Uani 1 1 d . . . H24A H 0.5951 0.9068 0.1912 0.061 Uiso 1 1 calc R . . H24B H 0.5571 0.9611 0.2321 0.061 Uiso 1 1 calc R . . H24C H 0.5735 1.0241 0.1909 0.061 Uiso 1 1 calc R . . C25 C 0.1801(3) 0.9714(3) 0.23650(11) 0.0575(10) Uani 1 1 d . . . H25A H 0.1690 0.9144 0.2547 0.086 Uiso 1 1 calc R . . H25B H 0.1175 0.9857 0.2213 0.086 Uiso 1 1 calc R . . H25C H 0.1992 1.0297 0.2528 0.086 Uiso 1 1 calc R . . C26 C 0.2880(3) 0.8616(3) 0.09572(10) 0.0479(8) Uani 1 1 d . . . H26A H 0.2847 0.7889 0.0933 0.072 Uiso 1 1 calc R . . H26B H 0.3391 0.8875 0.0766 0.072 Uiso 1 1 calc R . . H26C H 0.2215 0.8902 0.0891 0.072 Uiso 1 1 calc R . . C27 C 0.73187(19) 1.20866(19) 0.04247(9) 0.0256(5) Uani 1 1 d . . . C28 C 0.72831(18) 1.1087(2) 0.03032(8) 0.0262(5) Uani 1 1 d . . . C29 C 0.7223(2) 1.0838(2) -0.01152(9) 0.0327(6) Uani 1 1 d . . . H29 H 0.7151 1.0162 -0.0195 0.039 Uiso 1 1 calc R . . C30 C 0.7268(2) 1.1582(2) -0.04116(9) 0.0389(7) Uani 1 1 d . . . H30 H 0.7239 1.1417 -0.0695 0.047 Uiso 1 1 calc R . . C31 C 0.7357(2) 1.2575(2) -0.02889(10) 0.0392(7) Uani 1 1 d . . . H31 H 0.7412 1.3081 -0.0491 0.047 Uiso 1 1 calc R . . C32 C 0.7365(2) 1.2830(2) 0.01180(9) 0.0317(6) Uani 1 1 d . . . C33 C 0.7352(2) 1.3926(2) 0.02271(10) 0.0370(7) Uani 1 1 d . . . H33A H 0.7375 1.4324 -0.0025 0.056 Uiso 1 1 calc R . . H33B H 0.7943 1.4083 0.0398 0.056 Uiso 1 1 calc R . . H33C H 0.6729 1.4080 0.0379 0.056 Uiso 1 1 calc R . . C34 C 0.7236(2) 1.24071(18) 0.08673(9) 0.0294(6) Uani 1 1 d . . . C35 C 0.6286(3) 1.23412(19) 0.10741(9) 0.0359(6) Uani 1 1 d . . . C36 C 0.6247(3) 1.2604(2) 0.14850(10) 0.0467(8) Uani 1 1 d . . . H36 H 0.5626 1.2547 0.1631 0.056 Uiso 1 1 calc R . . C37 C 0.7121(3) 1.2957(2) 0.16885(11) 0.0532(10) Uani 1 1 d . . . H37 H 0.7084 1.3129 0.1971 0.064 Uiso 1 1 calc R . . C38 C 0.8016(3) 1.3052(2) 0.14837(10) 0.0425(8) Uani 1 1 d . . . H38 H 0.8597 1.3296 0.1624 0.051 Uiso 1 1 calc R . . C39 C 0.8089(2) 1.27953(19) 0.10720(9) 0.0323(6) Uani 1 1 d . . . C40 C 0.9093(2) 1.2935(2) 0.08593(10) 0.0390(7) Uani 1 1 d . . . H40A H 0.9186 1.3641 0.0793 0.059 Uiso 1 1 calc R . . H40B H 0.9104 1.2542 0.0606 0.059 Uiso 1 1 calc R . . H40C H 0.9642 1.2715 0.1041 0.059 Uiso 1 1 calc R . . C41 C 0.5049(2) 1.2661(2) 0.05377(12) 0.0490(9) Uani 1 1 d . . . H41A H 0.4953 1.3337 0.0644 0.073 Uiso 1 1 calc R . . H41B H 0.4402 1.2407 0.0433 0.073 Uiso 1 1 calc R . . H41C H 0.5551 1.2672 0.0316 0.073 Uiso 1 1 calc R . . C42 C 0.4555(3) 1.1727(3) 0.11240(12) 0.0525(9) Uani 1 1 d . . . H42A H 0.4800 1.1344 0.1360 0.079 Uiso 1 1 calc R . . H42B H 0.4084 1.1317 0.0964 0.079 Uiso 1 1 calc R . . H42C H 0.4204 1.2326 0.1220 0.079 Uiso 1 1 calc R . . C43 C 0.7853(2) 0.99526(18) 0.08597(8) 0.0244(5) Uani 1 1 d . . . C44 C 0.88352(19) 1.03839(17) 0.09998(8) 0.0248(5) Uani 1 1 d . . . C45 C 0.8930(2) 1.06324(18) 0.14165(8) 0.0273(6) Uani 1 1 d . . . C46 C 0.9877(2) 1.0984(2) 0.15544(9) 0.0323(6) Uani 1 1 d . . . H46 H 0.9946 1.1176 0.1834 0.039 Uiso 1 1 calc R . . C47 C 1.0706(2) 1.1060(2) 0.12993(9) 0.0340(6) Uani 1 1 d . . . C48 C 1.0598(2) 1.0748(2) 0.08945(10) 0.0358(6) Uani 1 1 d . . . H48 H 1.1175 1.0754 0.0720 0.043 Uiso 1 1 calc R . . C49 C 0.9669(2) 1.0424(2) 0.07365(9) 0.0295(6) Uani 1 1 d . . . C50 C 0.8056(2) 1.0525(2) 0.17070(8) 0.0326(6) Uani 1 1 d . . . H50A H 0.7427 1.0729 0.1570 0.049 Uiso 1 1 calc R . . H50B H 0.8169 1.0947 0.1948 0.049 Uiso 1 1 calc R . . H50C H 0.7998 0.9829 0.1794 0.049 Uiso 1 1 calc R . . C51 C 1.1687(2) 1.1507(3) 0.14516(11) 0.0456(8) Uani 1 1 d . . . H51A H 1.1701 1.2219 0.1387 0.068 Uiso 1 1 calc R . . H51B H 1.2261 1.1175 0.1318 0.068 Uiso 1 1 calc R . . H51C H 1.1736 1.1417 0.1749 0.068 Uiso 1 1 calc R . . C52 C 0.9612(2) 1.0132(2) 0.02914(10) 0.0402(7) Uani 1 1 d . . . H52A H 0.9278 1.0662 0.0135 0.060 Uiso 1 1 calc R . . H52B H 0.9222 0.9514 0.0265 0.060 Uiso 1 1 calc R . . H52C H 1.0300 1.0029 0.0185 0.060 Uiso 1 1 calc R . . C53 C 0.7450(2) 0.8172(2) 0.01804(10) 0.0352(7) Uani 1 1 d . . . H53A H 0.7335 0.8280 -0.0116 0.042 Uiso 1 1 calc R . . H53B H 0.8172 0.8163 0.0265 0.042 Uiso 1 1 calc R . . C54 C 0.6787(3) 0.6462(2) 0.03674(11) 0.0432(8) Uani 1 1 d . . . H54A H 0.6683 0.6254 0.0082 0.065 Uiso 1 1 calc R . . H54B H 0.6244 0.6188 0.0539 0.065 Uiso 1 1 calc R . . H54C H 0.7445 0.6216 0.0464 0.065 Uiso 1 1 calc R . . C55 C 0.4869(2) 1.0162(3) 0.01927(11) 0.0473(8) Uani 1 1 d . . . H55A H 0.5013 1.0504 -0.0067 0.071 Uiso 1 1 calc R . . H55B H 0.5148 1.0551 0.0421 0.071 Uiso 1 1 calc R . . H55C H 0.4133 1.0094 0.0227 0.071 Uiso 1 1 calc R . . C56 C 0.5042(3) 0.8604(3) -0.01782(11) 0.0560(10) Uani 1 1 d . . . H56A H 0.4309 0.8474 -0.0171 0.084 Uiso 1 1 calc R . . H56B H 0.5410 0.7970 -0.0181 0.084 Uiso 1 1 calc R . . H56C H 0.5210 0.8984 -0.0426 0.084 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 Nb1 0.02332(10) 0.02150(10) 0.02795(12) -0.00360(9) 0.00094(9) -0.00016(9) O1 0.0384(11) 0.0213(9) 0.0354(11) -0.0044(8) 0.0114(9) -0.0015(8) O2 0.0306(10) 0.0234(9) 0.0331(10) 0.0029(7) -0.0042(8) -0.0053(7) N1 0.0265(11) 0.0232(10) 0.0241(11) -0.0014(8) 0.0025(9) -0.0014(9) N2 0.0331(12) 0.0258(11) 0.0517(16) -0.0008(11) -0.0019(12) 0.0059(10) N3 0.0249(10) 0.0188(9) 0.0294(12) -0.0002(9) 0.0028(10) 0.0014(8) N4 0.0300(12) 0.0281(12) 0.0528(16) 0.0026(11) 0.0173(12) 0.0042(10) N5 0.0324(12) 0.0263(11) 0.0351(13) -0.0075(10) 0.0038(10) -0.0028(10) N6 0.0284(11) 0.0402(13) 0.0336(13) 0.0051(10) -0.0033(10) -0.0030(10) C1 0.0299(13) 0.0265(13) 0.0224(13) -0.0048(10) -0.0003(10) 0.0015(10) C2 0.0236(12) 0.0226(11) 0.0285(13) -0.0062(10) 0.0013(10) 0.0004(10) C3 0.0296(13) 0.0306(13) 0.0253(14) -0.0037(10) 0.0002(10) -0.0012(11) C4 0.0312(14) 0.0373(14) 0.0307(15) -0.0097(11) -0.0001(11) -0.0054(12) C5 0.0392(16) 0.0303(13) 0.0366(15) -0.0081(12) 0.0027(13) -0.0106(12) C6 0.0379(15) 0.0260(12) 0.0317(15) -0.0050(11) 0.0056(12) -0.0034(12) C7 0.063(2) 0.0260(13) 0.0436(18) 0.0005(13) 0.0054(16) 0.0005(14) C8 0.0467(16) 0.0225(12) 0.0262(14) -0.0032(10) -0.0053(12) 0.0033(12) C9 0.0409(16) 0.0252(12) 0.0378(16) -0.0055(11) -0.0099(13) 0.0096(12) C10 0.0459(18) 0.0425(17) 0.052(2) -0.0062(15) -0.0202(16) 0.0127(15) C11 0.067(3) 0.058(2) 0.0384(18) -0.0178(16) -0.0235(18) 0.0104(19) C12 0.071(2) 0.0472(19) 0.0322(17) -0.0082(14) -0.0053(17) 0.0108(18) C13 0.0525(19) 0.0302(14) 0.0305(15) -0.0022(12) -0.0040(14) 0.0098(14) C14 0.0475(18) 0.0361(14) 0.0334(15) -0.0021(12) 0.0072(14) 0.0008(14) C15 0.0384(17) 0.0391(17) 0.068(2) -0.0012(17) -0.0067(17) 0.0025(14) C16 0.0498(19) 0.0296(15) 0.058(2) -0.0055(14) 0.0031(17) 0.0076(14) C17 0.0279(12) 0.0262(12) 0.0311(13) -0.0032(12) -0.0002(10) -0.0012(12) C18 0.0316(14) 0.0259(13) 0.0321(14) -0.0016(10) 0.0047(11) 0.0039(11) C19 0.0353(15) 0.0253(12) 0.0352(16) -0.0018(11) 0.0051(12) 0.0023(11) C20 0.0435(16) 0.0304(13) 0.0363(15) -0.0029(11) 0.0058(14) 0.0080(14) C21 0.0425(17) 0.0388(16) 0.0422(18) 0.0072(14) 0.0103(14) 0.0148(14) C22 0.0323(15) 0.0427(17) 0.0476(19) 0.0033(14) 0.0051(13) 0.0123(13) C23 0.0329(14) 0.0296(14) 0.0392(16) 0.0005(13) -0.0004(12) 0.0090(12) C24 0.0409(17) 0.0383(16) 0.0425(18) -0.0137(13) 0.0033(14) -0.0069(14) C25 0.0451(19) 0.078(3) 0.050(2) 0.0085(19) 0.0186(17) 0.0255(19) C26 0.0365(15) 0.062(2) 0.0451(18) -0.0063(16) -0.0047(14) 0.0178(16) C27 0.0190(11) 0.0225(12) 0.0354(14) 0.0003(10) 0.0033(11) 0.0049(10) C28 0.0217(11) 0.0273(12) 0.0295(13) 0.0029(11) 0.0038(10) 0.0066(10) C29 0.0302(14) 0.0331(14) 0.0348(15) -0.0012(11) 0.0067(12) 0.0086(12) C30 0.0343(15) 0.0506(18) 0.0319(15) 0.0051(13) 0.0056(13) 0.0143(14) C31 0.0363(15) 0.0413(16) 0.0399(17) 0.0170(13) 0.0119(13) 0.0195(14) C32 0.0287(13) 0.0261(13) 0.0404(16) 0.0092(11) 0.0066(12) 0.0084(11) C33 0.0355(14) 0.0252(13) 0.0503(18) 0.0100(13) 0.0085(13) 0.0074(12) C34 0.0345(14) 0.0157(11) 0.0380(16) 0.0024(10) 0.0081(12) 0.0052(11) C35 0.0427(16) 0.0223(12) 0.0426(16) 0.0002(11) 0.0184(15) 0.0052(13) C36 0.055(2) 0.0344(15) 0.0503(19) -0.0056(14) 0.0228(17) 0.0008(16) C37 0.094(3) 0.0308(16) 0.0346(18) -0.0029(13) 0.0103(19) -0.0005(18) C38 0.060(2) 0.0225(13) 0.0452(19) -0.0043(12) -0.0043(16) -0.0060(14) C39 0.0401(16) 0.0190(11) 0.0379(16) -0.0006(11) 0.0014(13) 0.0008(11) C40 0.0378(15) 0.0279(13) 0.0515(19) 0.0050(13) -0.0025(14) -0.0030(12) C41 0.0342(15) 0.0424(17) 0.070(3) 0.0127(17) 0.0100(16) 0.0097(14) C42 0.0414(18) 0.0440(18) 0.072(2) 0.0040(17) 0.0334(18) 0.0067(15) C43 0.0267(12) 0.0189(11) 0.0276(13) -0.0013(9) 0.0015(11) 0.0018(10) C44 0.0251(13) 0.0191(10) 0.0303(13) 0.0020(9) -0.0014(10) -0.0002(10) C45 0.0293(14) 0.0216(11) 0.0310(14) 0.0023(10) -0.0018(11) -0.0018(10) C46 0.0351(14) 0.0309(14) 0.0309(15) 0.0046(11) -0.0066(12) -0.0038(12) C47 0.0290(13) 0.0316(14) 0.0412(16) 0.0065(12) -0.0058(12) -0.0035(12) C48 0.0289(14) 0.0341(14) 0.0444(17) 0.0016(13) 0.0032(13) -0.0021(12) C49 0.0276(13) 0.0252(12) 0.0356(15) 0.0002(11) -0.0001(11) 0.0000(11) C50 0.0337(15) 0.0350(14) 0.0289(15) -0.0021(11) -0.0026(12) -0.0050(12) C51 0.0348(15) 0.0462(17) 0.056(2) 0.0097(15) -0.0098(15) -0.0125(14) C52 0.0352(16) 0.0443(17) 0.0411(17) -0.0052(14) 0.0095(14) -0.0014(14) C53 0.0348(15) 0.0289(14) 0.0420(17) -0.0083(12) 0.0146(13) -0.0012(12) C54 0.0443(17) 0.0303(15) 0.055(2) -0.0101(14) 0.0081(15) -0.0023(13) C55 0.0290(15) 0.055(2) 0.058(2) 0.0159(17) -0.0035(15) 0.0074(15) C56 0.063(2) 0.061(2) 0.0444(19) 0.0020(17) -0.0194(17) -0.018(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Nb1 N5 1.931(2) . ? Nb1 N6 1.977(2) . ? Nb1 O2 2.1663(18) . ? Nb1 C53 2.201(3) . ? Nb1 O1 2.2058(18) . ? Nb1 N1 2.211(2) . ? Nb1 N3 2.275(2) . ? Nb1 C17 2.621(3) . ? Nb1 C43 2.650(3) . ? O1 C17 1.296(3) . ? O2 C43 1.293(3) . ? N1 C17 1.320(3) . ? N1 C2 1.424(3) . ? N2 C9 1.409(4) . ? N2 C15 1.460(4) . ? N2 C16 1.482(4) . ? N3 C43 1.319(3) . ? N3 C28 1.422(3) . ? N4 C35 1.405(4) . ? N4 C42 1.454(4) . ? N4 C41 1.465(4) . ? N5 C53 1.415(4) . ? N5 C54 1.446(4) . ? N6 C55 1.456(4) . ? N6 C56 1.473(4) . ? C1 C6 1.399(4) . ? C1 C2 1.402(4) . ? C1 C8 1.494(4) . ? C2 C3 1.394(4) . ? C3 C4 1.379(4) . ? C3 H3 0.9500 . ? C4 C5 1.381(4) . ? C4 H4 0.9500 . ? C5 C6 1.385(4) . ? C5 H5 0.9500 . ? C6 C7 1.518(4) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.410(4) . ? C8 C13 1.424(4) . ? C9 C10 1.403(4) . ? C10 C11 1.364(5) . ? C10 H10 0.9500 . ? C11 C12 1.402(6) . ? C11 H11 0.9500 . ? C12 C13 1.392(5) . ? C12 H12 0.9500 . ? C13 C14 1.486(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.481(4) . ? C18 C23 1.410(4) . ? C18 C19 1.410(4) . ? C19 C20 1.383(4) . ? C19 C24 1.501(4) . ? C20 C21 1.392(5) . ? C20 H20 0.9500 . ? C21 C22 1.385(5) . ? C21 C25 1.512(4) . ? C22 C23 1.393(4) . ? C22 H22 0.9500 . ? C23 C26 1.515(4) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.400(4) . ? C27 C32 1.414(4) . ? C27 C34 1.509(4) . ? C28 C29 1.407(4) . ? C29 C30 1.391(4) . ? C29 H29 0.9500 . ? C30 C31 1.396(5) . ? C30 H30 0.9500 . ? C31 C32 1.370(4) . ? C31 H31 0.9500 . ? C32 C33 1.515(4) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C39 1.407(4) . ? C34 C35 1.424(4) . ? C35 C36 1.386(4) . ? C36 C37 1.410(5) . ? C36 H36 0.9500 . ? C37 C38 1.361(5) . ? C37 H37 0.9500 . ? C38 C39 1.389(4) . ? C38 H38 0.9500 . ? C39 C40 1.504(4) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.489(4) . ? C44 C49 1.394(4) . ? C44 C45 1.404(4) . ? C45 C46 1.407(4) . ? C45 C50 1.498(4) . ? C46 C47 1.376(4) . ? C46 H46 0.9500 . ? C47 C48 1.392(4) . ? C47 C51 1.508(4) . ? C48 C49 1.397(4) . ? C48 H48 0.9500 . ? C49 C52 1.505(4) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Nb1 N6 99.30(11) . . ? N5 Nb1 O2 99.50(9) . . ? N6 Nb1 O2 153.19(9) . . ? N5 Nb1 C53 39.35(10) . . ? N6 Nb1 C53 95.51(12) . . ? O2 Nb1 C53 87.10(10) . . ? N5 Nb1 O1 148.19(9) . . ? N6 Nb1 O1 93.21(9) . . ? O2 Nb1 O1 80.57(8) . . ? C53 Nb1 O1 166.62(10) . . ? N5 Nb1 N1 89.36(9) . . ? N6 Nb1 N1 100.16(9) . . ? O2 Nb1 N1 98.99(8) . . ? C53 Nb1 N1 128.31(10) . . ? O1 Nb1 N1 59.55(7) . . ? N5 Nb1 N3 125.63(9) . . ? N6 Nb1 N3 94.65(9) . . ? O2 Nb1 N3 58.75(7) . . ? C53 Nb1 N3 87.32(9) . . ? O1 Nb1 N3 81.85(7) . . ? N1 Nb1 N3 139.09(8) . . ? N5 Nb1 C17 119.55(9) . . ? N6 Nb1 C17 94.81(9) . . ? O2 Nb1 C17 92.36(8) . . ? C53 Nb1 C17 158.00(10) . . ? O1 Nb1 C17 29.60(8) . . ? N1 Nb1 C17 30.21(8) . . ? N3 Nb1 C17 111.13(8) . . ? N5 Nb1 C43 113.83(9) . . ? N6 Nb1 C43 124.49(9) . . ? O2 Nb1 C43 28.98(7) . . ? C53 Nb1 C43 85.25(10) . . ? O1 Nb1 C43 81.44(8) . . ? N1 Nb1 C43 122.32(8) . . ? N3 Nb1 C43 29.85(7) . . ? C17 Nb1 C43 104.65(8) . . ? C17 O1 Nb1 93.23(15) . . ? C43 O2 Nb1 96.75(16) . . ? C17 N1 C2 126.4(2) . . ? C17 N1 Nb1 92.34(16) . . ? C2 N1 Nb1 138.00(17) . . ? C9 N2 C15 116.4(3) . . ? C9 N2 C16 112.2(3) . . ? C15 N2 C16 108.9(3) . . ? C43 N3 C28 130.0(2) . . ? C43 N3 Nb1 91.02(15) . . ? C28 N3 Nb1 137.67(17) . . ? C35 N4 C42 116.4(3) . . ? C35 N4 C41 115.6(2) . . ? C42 N4 C41 109.0(3) . . ? C53 N5 C54 124.5(2) . . ? C53 N5 Nb1 80.68(15) . . ? C54 N5 Nb1 154.5(2) . . ? C55 N6 C56 112.0(3) . . ? C55 N6 Nb1 120.4(2) . . ? C56 N6 Nb1 127.4(2) . . ? C6 C1 C2 118.7(2) . . ? C6 C1 C8 120.2(2) . . ? C2 C1 C8 121.1(2) . . ? C3 C2 C1 120.2(2) . . ? C3 C2 N1 115.8(2) . . ? C1 C2 N1 123.8(2) . . ? C4 C3 C2 120.2(3) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 120.1(3) . . ? C3 C4 H4 119.9 . . ? C5 C4 H4 119.9 . . ? C4 C5 C6 120.4(3) . . ? C4 C5 H5 119.8 . . ? C6 C5 H5 119.8 . . ? C5 C6 C1 120.4(3) . . ? C5 C6 C7 117.4(3) . . ? C1 C6 C7 122.1(3) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C13 119.7(3) . . ? C9 C8 C1 120.8(3) . . ? C13 C8 C1 119.5(3) . . ? C10 C9 N2 121.8(3) . . ? C10 C9 C8 119.1(3) . . ? N2 C9 C8 119.1(3) . . ? C11 C10 C9 121.6(3) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C10 C11 C12 119.6(3) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C13 C12 C11 121.3(3) . . ? C13 C12 H12 119.4 . . ? C11 C12 H12 119.4 . . ? C12 C13 C8 118.7(3) . . ? C12 C13 C14 119.4(3) . . ? C8 C13 C14 122.0(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N2 C15 H15A 109.5 . . ? N2 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N2 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N2 C16 H16A 109.5 . . ? N2 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N2 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O1 C17 N1 114.0(2) . . ? O1 C17 C18 117.0(2) . . ? N1 C17 C18 129.1(2) . . ? O1 C17 Nb1 57.18(12) . . ? N1 C17 Nb1 57.45(13) . . ? C18 C17 Nb1 169.13(19) . . ? C23 C18 C19 120.5(2) . . ? C23 C18 C17 121.2(2) . . ? C19 C18 C17 117.8(2) . . ? C20 C19 C18 118.8(3) . . ? C20 C19 C24 120.1(3) . . ? C18 C19 C24 121.1(3) . . ? C19 C20 C21 121.6(3) . . ? C19 C20 H20 119.2 . . ? C21 C20 H20 119.2 . . ? C22 C21 C20 118.8(3) . . ? C22 C21 C25 120.3(3) . . ? C20 C21 C25 120.9(3) . . ? C21 C22 C23 121.9(3) . . ? C21 C22 H22 119.1 . . ? C23 C22 H22 119.1 . . ? C22 C23 C18 118.2(3) . . ? C22 C23 C26 119.9(3) . . ? C18 C23 C26 121.7(3) . . ? C19 C24 H24A 109.5 . . ? C19 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C19 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C21 C25 H25A 109.5 . . ? C21 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C21 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C32 118.6(3) . . ? C28 C27 C34 122.8(2) . . ? C32 C27 C34 118.5(2) . . ? C27 C28 C29 120.3(2) . . ? C27 C28 N3 125.5(2) . . ? C29 C28 N3 114.0(2) . . ? C30 C29 C28 120.0(3) . . ? C30 C29 H29 120.0 . . ? C28 C29 H29 120.0 . . ? C29 C30 C31 119.4(3) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C32 C31 C30 121.1(3) . . ? C32 C31 H31 119.5 . . ? C30 C31 H31 119.5 . . ? C31 C32 C27 120.5(3) . . ? C31 C32 C33 118.0(3) . . ? C27 C32 C33 121.3(3) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C39 C34 C35 120.0(3) . . ? C39 C34 C27 120.1(3) . . ? C35 C34 C27 119.9(3) . . ? C36 C35 N4 120.7(3) . . ? C36 C35 C34 118.3(3) . . ? N4 C35 C34 120.9(3) . . ? C35 C36 C37 120.6(3) . . ? C35 C36 H36 119.7 . . ? C37 C36 H36 119.7 . . ? C38 C37 C36 120.5(3) . . ? C38 C37 H37 119.7 . . ? C36 C37 H37 119.7 . . ? C37 C38 C39 120.7(3) . . ? C37 C38 H38 119.6 . . ? C39 C38 H38 119.6 . . ? C38 C39 C34 119.7(3) . . ? C38 C39 C40 118.4(3) . . ? C34 C39 C40 122.0(3) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N4 C41 H41A 109.5 . . ? N4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N4 C42 H42A 109.5 . . ? N4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? O2 C43 N3 113.2(2) . . ? O2 C43 C44 116.2(2) . . ? N3 C43 C44 130.3(2) . . ? O2 C43 Nb1 54.27(13) . . ? N3 C43 Nb1 59.13(13) . . ? C44 C43 Nb1 167.03(17) . . ? C49 C44 C45 121.1(2) . . ? C49 C44 C43 120.7(2) . . ? C45 C44 C43 117.8(2) . . ? C44 C45 C46 117.9(2) . . ? C44 C45 C50 121.3(2) . . ? C46 C45 C50 120.8(2) . . ? C47 C46 C45 122.3(3) . . ? C47 C46 H46 118.8 . . ? C45 C46 H46 118.8 . . ? C46 C47 C48 118.0(3) . . ? C46 C47 C51 120.7(3) . . ? C48 C47 C51 121.3(3) . . ? C47 C48 C49 122.2(3) . . ? C47 C48 H48 118.9 . . ? C49 C48 H48 118.9 . . ? C44 C49 C48 118.4(3) . . ? C44 C49 C52 123.0(3) . . ? C48 C49 C52 118.7(3) . . ? C45 C50 H50A 109.5 . . ? C45 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C45 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C47 C51 H51A 109.5 . . ? C47 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C47 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C49 C52 H52A 109.5 . . ? C49 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C49 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N5 C53 Nb1 59.97(13) . . ? N5 C53 H53A 117.8 . . ? Nb1 C53 H53A 117.8 . . ? N5 C53 H53B 117.8 . . ? Nb1 C53 H53B 117.8 . . ? H53A C53 H53B 114.9 . . ? N5 C54 H54A 109.5 . . ? N5 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? N5 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N6 C55 H55A 109.5 . . ? N6 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? N6 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N6 C56 H56A 109.5 . . ? N6 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? N6 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Nb1 O1 C17 -19.3(3) . . . . ? N6 Nb1 O1 C17 94.09(17) . . . . ? O2 Nb1 O1 C17 -112.16(16) . . . . ? C53 Nb1 O1 C17 -135.3(4) . . . . ? N1 Nb1 O1 C17 -5.81(15) . . . . ? N3 Nb1 O1 C17 -171.67(17) . . . . ? C43 Nb1 O1 C17 -141.50(16) . . . . ? N5 Nb1 O2 C43 122.91(16) . . . . ? N6 Nb1 O2 C43 -11.1(3) . . . . ? C53 Nb1 O2 C43 85.42(17) . . . . ? O1 Nb1 O2 C43 -89.35(15) . . . . ? N1 Nb1 O2 C43 -146.24(15) . . . . ? N3 Nb1 O2 C43 -3.21(14) . . . . ? C17 Nb1 O2 C43 -116.60(16) . . . . ? N5 Nb1 N1 C17 178.63(17) . . . . ? N6 Nb1 N1 C17 -82.04(17) . . . . ? O2 Nb1 N1 C17 79.11(16) . . . . ? C53 Nb1 N1 C17 172.55(17) . . . . ? O1 Nb1 N1 C17 5.70(14) . . . . ? N3 Nb1 N1 C17 27.4(2) . . . . ? C43 Nb1 N1 C17 60.53(18) . . . . ? N5 Nb1 N1 C2 -22.5(3) . . . . ? N6 Nb1 N1 C2 76.8(3) . . . . ? O2 Nb1 N1 C2 -122.0(3) . . . . ? C53 Nb1 N1 C2 -28.6(3) . . . . ? O1 Nb1 N1 C2 164.5(3) . . . . ? N3 Nb1 N1 C2 -173.8(2) . . . . ? C17 Nb1 N1 C2 158.8(4) . . . . ? C43 Nb1 N1 C2 -140.6(2) . . . . ? N5 Nb1 N3 C43 -75.49(18) . . . . ? N6 Nb1 N3 C43 179.57(16) . . . . ? O2 Nb1 N3 C43 3.12(14) . . . . ? C53 Nb1 N3 C43 -85.11(17) . . . . ? O1 Nb1 N3 C43 86.99(15) . . . . ? N1 Nb1 N3 C43 68.23(19) . . . . ? C17 Nb1 N3 C43 82.59(16) . . . . ? N5 Nb1 N3 C28 91.3(3) . . . . ? N6 Nb1 N3 C28 -13.6(3) . . . . ? O2 Nb1 N3 C28 170.0(3) . . . . ? C53 Nb1 N3 C28 81.7(3) . . . . ? O1 Nb1 N3 C28 -106.2(2) . . . . ? N1 Nb1 N3 C28 -124.9(2) . . . . ? C17 Nb1 N3 C28 -110.6(2) . . . . ? C43 Nb1 N3 C28 166.8(3) . . . . ? N6 Nb1 N5 C53 87.35(18) . . . . ? O2 Nb1 N5 C53 -73.45(18) . . . . ? O1 Nb1 N5 C53 -160.84(18) . . . . ? N1 Nb1 N5 C53 -172.46(17) . . . . ? N3 Nb1 N5 C53 -15.3(2) . . . . ? C17 Nb1 N5 C53 -171.67(16) . . . . ? C43 Nb1 N5 C53 -47.05(19) . . . . ? N6 Nb1 N5 C54 -101.2(5) . . . . ? O2 Nb1 N5 C54 98.0(5) . . . . ? C53 Nb1 N5 C54 171.4(6) . . . . ? O1 Nb1 N5 C54 10.6(6) . . . . ? N1 Nb1 N5 C54 -1.1(5) . . . . ? N3 Nb1 N5 C54 156.1(5) . . . . ? C17 Nb1 N5 C54 -0.3(6) . . . . ? C43 Nb1 N5 C54 124.4(5) . . . . ? N5 Nb1 N6 C55 -172.7(2) . . . . ? O2 Nb1 N6 C55 -38.7(3) . . . . ? C53 Nb1 N6 C55 -133.2(2) . . . . ? O1 Nb1 N6 C55 36.6(2) . . . . ? N1 Nb1 N6 C55 96.3(2) . . . . ? N3 Nb1 N6 C55 -45.5(2) . . . . ? C17 Nb1 N6 C55 66.3(2) . . . . ? C43 Nb1 N6 C55 -45.2(3) . . . . ? N5 Nb1 N6 C56 0.8(3) . . . . ? O2 Nb1 N6 C56 134.8(3) . . . . ? C53 Nb1 N6 C56 40.4(3) . . . . ? O1 Nb1 N6 C56 -149.8(3) . . . . ? N1 Nb1 N6 C56 -90.2(3) . . . . ? N3 Nb1 N6 C56 128.1(3) . . . . ? C17 Nb1 N6 C56 -120.2(3) . . . . ? C43 Nb1 N6 C56 128.4(2) . . . . ? C6 C1 C2 C3 -0.4(4) . . . . ? C8 C1 C2 C3 177.9(3) . . . . ? C6 C1 C2 N1 -175.8(2) . . . . ? C8 C1 C2 N1 2.6(4) . . . . ? C17 N1 C2 C3 107.5(3) . . . . ? Nb1 N1 C2 C3 -45.9(4) . . . . ? C17 N1 C2 C1 -76.9(4) . . . . ? Nb1 N1 C2 C1 129.7(3) . . . . ? C1 C2 C3 C4 1.1(4) . . . . ? N1 C2 C3 C4 176.8(2) . . . . ? C2 C3 C4 C5 -0.5(4) . . . . ? C3 C4 C5 C6 -0.8(4) . . . . ? C4 C5 C6 C1 1.5(4) . . . . ? C4 C5 C6 C7 -177.8(3) . . . . ? C2 C1 C6 C5 -0.9(4) . . . . ? C8 C1 C6 C5 -179.2(3) . . . . ? C2 C1 C6 C7 178.4(3) . . . . ? C8 C1 C6 C7 0.0(4) . . . . ? C6 C1 C8 C9 107.4(3) . . . . ? C2 C1 C8 C9 -70.9(4) . . . . ? C6 C1 C8 C13 -72.2(3) . . . . ? C2 C1 C8 C13 109.5(3) . . . . ? C15 N2 C9 C10 -22.0(4) . . . . ? C16 N2 C9 C10 104.4(3) . . . . ? C15 N2 C9 C8 158.0(3) . . . . ? C16 N2 C9 C8 -75.6(3) . . . . ? C13 C8 C9 C10 -1.9(4) . . . . ? C1 C8 C9 C10 178.5(3) . . . . ? C13 C8 C9 N2 178.1(2) . . . . ? C1 C8 C9 N2 -1.5(4) . . . . ? N2 C9 C10 C11 -178.0(3) . . . . ? C8 C9 C10 C11 2.0(5) . . . . ? C9 C10 C11 C12 -1.1(6) . . . . ? C10 C11 C12 C13 0.0(6) . . . . ? C11 C12 C13 C8 0.1(5) . . . . ? C11 C12 C13 C14 -179.2(3) . . . . ? C9 C8 C13 C12 0.9(4) . . . . ? C1 C8 C13 C12 -179.5(3) . . . . ? C9 C8 C13 C14 -179.8(3) . . . . ? C1 C8 C13 C14 -0.2(4) . . . . ? Nb1 O1 C17 N1 9.2(2) . . . . ? Nb1 O1 C17 C18 -169.4(2) . . . . ? C2 N1 C17 O1 -171.7(2) . . . . ? Nb1 N1 C17 O1 -9.2(2) . . . . ? C2 N1 C17 C18 6.7(4) . . . . ? Nb1 N1 C17 C18 169.3(3) . . . . ? C2 N1 C17 Nb1 -162.5(3) . . . . ? N5 Nb1 C17 O1 168.43(16) . . . . ? N6 Nb1 C17 O1 -88.03(17) . . . . ? O2 Nb1 C17 O1 66.12(16) . . . . ? C53 Nb1 C17 O1 154.2(3) . . . . ? N1 Nb1 C17 O1 170.0(3) . . . . ? N3 Nb1 C17 O1 8.85(18) . . . . ? C43 Nb1 C17 O1 39.52(17) . . . . ? N5 Nb1 C17 N1 -1.58(19) . . . . ? N6 Nb1 C17 N1 101.96(17) . . . . ? O2 Nb1 C17 N1 -103.89(16) . . . . ? C53 Nb1 C17 N1 -15.8(4) . . . . ? O1 Nb1 C17 N1 -170.0(3) . . . . ? N3 Nb1 C17 N1 -161.16(15) . . . . ? C43 Nb1 C17 N1 -130.49(16) . . . . ? N5 Nb1 C17 C18 -131.5(10) . . . . ? N6 Nb1 C17 C18 -28.0(10) . . . . ? O2 Nb1 C17 C18 126.2(10) . . . . ? C53 Nb1 C17 C18 -145.7(10) . . . . ? O1 Nb1 C17 C18 60.1(10) . . . . ? N1 Nb1 C17 C18 -129.9(11) . . . . ? N3 Nb1 C17 C18 68.9(10) . . . . ? C43 Nb1 C17 C18 99.6(10) . . . . ? O1 C17 C18 C23 109.5(3) . . . . ? N1 C17 C18 C23 -68.9(4) . . . . ? Nb1 C17 C18 C23 54.7(11) . . . . ? O1 C17 C18 C19 -62.2(3) . . . . ? N1 C17 C18 C19 119.4(3) . . . . ? Nb1 C17 C18 C19 -117.0(10) . . . . ? C23 C18 C19 C20 4.1(4) . . . . ? C17 C18 C19 C20 175.8(2) . . . . ? C23 C18 C19 C24 -175.3(3) . . . . ? C17 C18 C19 C24 -3.6(4) . . . . ? C18 C19 C20 C21 -0.7(4) . . . . ? C24 C19 C20 C21 178.8(3) . . . . ? C19 C20 C21 C22 -1.9(5) . . . . ? C19 C20 C21 C25 179.7(3) . . . . ? C20 C21 C22 C23 1.0(5) . . . . ? C25 C21 C22 C23 179.4(3) . . . . ? C21 C22 C23 C18 2.3(5) . . . . ? C21 C22 C23 C26 -173.5(3) . . . . ? C19 C18 C23 C22 -4.9(4) . . . . ? C17 C18 C23 C22 -176.3(3) . . . . ? C19 C18 C23 C26 170.9(3) . . . . ? C17 C18 C23 C26 -0.6(4) . . . . ? C32 C27 C28 C29 -4.4(4) . . . . ? C34 C27 C28 C29 171.2(3) . . . . ? C32 C27 C28 N3 -178.9(2) . . . . ? C34 C27 C28 N3 -3.3(4) . . . . ? C43 N3 C28 C27 -61.3(4) . . . . ? Nb1 N3 C28 C27 136.0(2) . . . . ? C43 N3 C28 C29 123.8(3) . . . . ? Nb1 N3 C28 C29 -38.9(3) . . . . ? C27 C28 C29 C30 4.4(4) . . . . ? N3 C28 C29 C30 179.5(2) . . . . ? C28 C29 C30 C31 -1.0(4) . . . . ? C29 C30 C31 C32 -2.3(5) . . . . ? C30 C31 C32 C27 2.2(4) . . . . ? C30 C31 C32 C33 -173.7(3) . . . . ? C28 C27 C32 C31 1.1(4) . . . . ? C34 C27 C32 C31 -174.7(3) . . . . ? C28 C27 C32 C33 176.9(3) . . . . ? C34 C27 C32 C33 1.1(4) . . . . ? C28 C27 C34 C39 109.7(3) . . . . ? C32 C27 C34 C39 -74.7(3) . . . . ? C28 C27 C34 C35 -72.1(3) . . . . ? C32 C27 C34 C35 103.5(3) . . . . ? C42 N4 C35 C36 -15.0(4) . . . . ? C41 N4 C35 C36 114.9(3) . . . . ? C42 N4 C35 C34 164.6(3) . . . . ? C41 N4 C35 C34 -65.5(3) . . . . ? C39 C34 C35 C36 -4.2(4) . . . . ? C27 C34 C35 C36 177.5(2) . . . . ? C39 C34 C35 N4 176.1(2) . . . . ? C27 C34 C35 N4 -2.2(4) . . . . ? N4 C35 C36 C37 -178.5(3) . . . . ? C34 C35 C36 C37 1.9(4) . . . . ? C35 C36 C37 C38 0.5(5) . . . . ? C36 C37 C38 C39 -0.6(5) . . . . ? C37 C38 C39 C34 -1.8(4) . . . . ? C37 C38 C39 C40 178.8(3) . . . . ? C35 C34 C39 C38 4.2(4) . . . . ? C27 C34 C39 C38 -177.5(2) . . . . ? C35 C34 C39 C40 -176.4(2) . . . . ? C27 C34 C39 C40 1.9(4) . . . . ? Nb1 O2 C43 N3 5.1(2) . . . . ? Nb1 O2 C43 C44 -169.71(19) . . . . ? C28 N3 C43 O2 -173.3(2) . . . . ? Nb1 N3 C43 O2 -4.9(2) . . . . ? C28 N3 C43 C44 0.6(4) . . . . ? Nb1 N3 C43 C44 169.1(3) . . . . ? C28 N3 C43 Nb1 -168.5(3) . . . . ? N5 Nb1 C43 O2 -64.85(17) . . . . ? N6 Nb1 C43 O2 173.97(15) . . . . ? C53 Nb1 C43 O2 -92.60(17) . . . . ? O1 Nb1 C43 O2 85.96(15) . . . . ? N1 Nb1 C43 O2 40.51(18) . . . . ? N3 Nb1 C43 O2 174.5(2) . . . . ? C17 Nb1 C43 O2 67.43(16) . . . . ? N5 Nb1 C43 N3 120.67(16) . . . . ? N6 Nb1 C43 N3 -0.52(19) . . . . ? O2 Nb1 C43 N3 -174.5(2) . . . . ? C53 Nb1 C43 N3 92.91(17) . . . . ? O1 Nb1 C43 N3 -88.53(15) . . . . ? N1 Nb1 C43 N3 -133.98(15) . . . . ? C17 Nb1 C43 N3 -107.06(15) . . . . ? N5 Nb1 C43 C44 -19.3(9) . . . . ? N6 Nb1 C43 C44 -140.5(8) . . . . ? O2 Nb1 C43 C44 45.6(8) . . . . ? C53 Nb1 C43 C44 -47.0(8) . . . . ? O1 Nb1 C43 C44 131.5(8) . . . . ? N1 Nb1 C43 C44 86.1(8) . . . . ? N3 Nb1 C43 C44 -140.0(9) . . . . ? C17 Nb1 C43 C44 113.0(8) . . . . ? O2 C43 C44 C49 109.3(3) . . . . ? N3 C43 C44 C49 -64.5(4) . . . . ? Nb1 C43 C44 C49 69.0(9) . . . . ? O2 C43 C44 C45 -63.1(3) . . . . ? N3 C43 C44 C45 123.1(3) . . . . ? Nb1 C43 C44 C45 -103.3(8) . . . . ? C49 C44 C45 C46 4.0(4) . . . . ? C43 C44 C45 C46 176.3(2) . . . . ? C49 C44 C45 C50 -175.8(2) . . . . ? C43 C44 C45 C50 -3.5(4) . . . . ? C44 C45 C46 C47 -2.0(4) . . . . ? C50 C45 C46 C47 177.8(3) . . . . ? C45 C46 C47 C48 -1.9(4) . . . . ? C45 C46 C47 C51 175.7(3) . . . . ? C46 C47 C48 C49 4.1(4) . . . . ? C51 C47 C48 C49 -173.5(3) . . . . ? C45 C44 C49 C48 -1.9(4) . . . . ? C43 C44 C49 C48 -174.0(2) . . . . ? C45 C44 C49 C52 177.8(3) . . . . ? C43 C44 C49 C52 5.7(4) . . . . ? C47 C48 C49 C44 -2.3(4) . . . . ? C47 C48 C49 C52 178.0(3) . . . . ? C54 N5 C53 Nb1 -175.5(3) . . . . ? N6 Nb1 C53 N5 -97.95(17) . . . . ? O2 Nb1 C53 N5 108.80(17) . . . . ? O1 Nb1 C53 N5 131.6(4) . . . . ? N1 Nb1 C53 N5 9.6(2) . . . . ? N3 Nb1 C53 N5 167.63(17) . . . . ? C17 Nb1 C53 N5 19.7(4) . . . . ? C43 Nb1 C53 N5 137.79(17) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.772 0.250 689 153 ' ' 2 0.500 0.605 0.750 689 153 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.321 _refine_diff_density_min -0.970 _refine_diff_density_rms 0.101 # Attachment '- compound 30.cif' data_compound30 _database_code_depnum_ccdc_archive 'CCDC 791874' #TrackingRef '- compound 30.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C56 H69 N6 O2 Ta' _chemical_formula_sum 'C56 H69 N6 O2 Ta' _chemical_formula_weight 1039.12 _chemical_absolute_configuration rmad 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' Ta Ta -0.7052 6.5227 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' _cell_length_a 13.1663(19) _cell_length_b 13.4684(19) _cell_length_c 32.490(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5761.4(14) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 16382 _cell_measurement_theta_min 1.3 _cell_measurement_theta_max 27.9 _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.198 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2144 _exptl_absorpt_coefficient_mu 1.949 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5571 _exptl_absorpt_correction_T_max 0.6966 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 0.71075 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator multilayer _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method '\w and \f scans' _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 40645 _diffrn_reflns_av_R_equivalents 0.0395 _diffrn_reflns_av_sigmaI/netI 0.0566 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 1.25 _diffrn_reflns_theta_max 27.87 _reflns_number_total 13699 _reflns_number_gt 13138 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.8' _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^)+(0.0317P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.000(6) _refine_ls_number_reflns 13699 _refine_ls_number_parameters 603 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0285 _refine_ls_wR_factor_ref 0.0775 _refine_ls_wR_factor_gt 0.0767 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.007 _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 Ta1 Ta 0.631572(10) 0.620871(11) 0.939504(4) 0.02120(4) Uani 1 1 d . . . N1 N 0.5325(2) 0.6991(2) 0.89590(9) 0.0206(7) Uani 1 1 d . . . N2 N 0.7092(3) 0.8429(3) 0.85671(11) 0.0339(8) Uani 1 1 d . . . N3 N 0.7174(2) 0.4751(2) 0.94291(10) 0.0208(6) Uani 1 1 d . . . N4 N 0.5366(3) 0.3003(3) 0.91344(11) 0.0323(8) Uani 1 1 d . . . N6 N 0.5303(3) 0.5824(3) 0.98190(10) 0.0305(8) Uani 1 1 d . . . N5 N 0.6738(3) 0.7473(2) 0.96137(10) 0.0265(7) Uani 1 1 d . . . O1 O 0.5489(2) 0.5380(2) 0.89163(8) 0.0277(6) Uani 1 1 d . . . O2 O 0.7552(2) 0.5895(2) 0.89795(8) 0.0257(6) Uani 1 1 d . . . C1 C 0.4921(3) 0.8541(3) 0.85758(11) 0.0243(8) Uani 1 1 d . . . C2 C 0.4850(3) 0.7942(3) 0.89275(11) 0.0238(8) Uani 1 1 d . . . C3 C 0.4349(3) 0.8279(3) 0.92770(11) 0.0259(8) Uani 1 1 d . . . H3 H 0.4315 0.7869 0.9515 0.031 Uiso 1 1 calc R . . C4 C 0.3897(3) 0.9213(3) 0.92815(11) 0.0296(9) Uani 1 1 d . . . H4 H 0.3548 0.9438 0.9520 0.036 Uiso 1 1 calc R . . C5 C 0.3961(3) 0.9809(3) 0.89360(12) 0.0312(9) Uani 1 1 d . . . H5A H 0.3651 1.0446 0.8940 0.037 Uiso 1 1 calc R . . C6 C 0.4465(3) 0.9501(3) 0.85858(12) 0.0283(9) Uani 1 1 d . . . C7 C 0.4523(4) 1.0210(3) 0.82257(13) 0.0391(11) Uani 1 1 d . . . H7A H 0.4032 1.0009 0.8015 0.059 Uiso 1 1 calc R . . H7B H 0.5209 1.0197 0.8109 0.059 Uiso 1 1 calc R . . H7C H 0.4364 1.0884 0.8320 0.059 Uiso 1 1 calc R . . C8 C 0.5486(3) 0.8214(3) 0.81971(12) 0.0280(8) Uani 1 1 d . . . C9 C 0.6556(3) 0.8154(3) 0.82027(12) 0.0307(9) Uani 1 1 d . . . C10 C 0.7074(4) 0.7817(4) 0.78575(15) 0.0450(12) Uani 1 1 d . . . H10 H 0.7792 0.7744 0.7862 0.054 Uiso 1 1 calc R . . C11 C 0.6514(5) 0.7584(4) 0.74985(14) 0.0560(15) Uani 1 1 d . . . H11 H 0.6860 0.7367 0.7258 0.067 Uiso 1 1 calc R . . C12 C 0.5481(4) 0.7667(4) 0.74936(14) 0.0472(13) Uani 1 1 d . . . H12 H 0.5118 0.7504 0.7250 0.057 Uiso 1 1 calc R . . C13 C 0.4956(3) 0.7985(3) 0.78365(12) 0.0328(10) Uani 1 1 d . . . C14 C 0.3801(4) 0.8029(3) 0.78135(12) 0.0397(10) Uani 1 1 d . . . H14A H 0.3597 0.8520 0.7607 0.060 Uiso 1 1 calc R . . H14B H 0.3527 0.8219 0.8083 0.060 Uiso 1 1 calc R . . H14C H 0.3536 0.7375 0.7736 0.060 Uiso 1 1 calc R . . C17 C 0.5006(3) 0.6157(3) 0.87919(10) 0.0242(7) Uani 1 1 d . . . C16 C 0.4163(3) 0.5991(3) 0.84907(11) 0.0259(8) Uani 1 1 d . . . C15 C 0.4415(3) 0.5590(3) 0.81051(12) 0.0290(9) Uani 1 1 d . . . C18 C 0.3654(4) 0.5364(3) 0.78341(12) 0.0355(9) Uani 1 1 d . . . H18 H 0.3825 0.5091 0.7574 0.043 Uiso 1 1 calc R . . C19 C 0.2634(3) 0.5523(4) 0.79295(14) 0.0386(11) Uani 1 1 d . . . C20 C 0.2401(3) 0.5880(3) 0.83182(13) 0.0360(10) Uani 1 1 d . . . H20 H 0.1708 0.5972 0.8390 0.043 Uiso 1 1 calc R . . C21 C 0.3152(3) 0.6110(4) 0.86086(12) 0.0322(9) Uani 1 1 d . . . C22 C 0.5512(3) 0.5385(4) 0.79903(13) 0.0358(10) Uani 1 1 d . . . H22A H 0.5723 0.4748 0.8108 0.054 Uiso 1 1 calc R . . H22B H 0.5945 0.5916 0.8098 0.054 Uiso 1 1 calc R . . H22C H 0.5576 0.5359 0.7690 0.054 Uiso 1 1 calc R . . C23 C 0.1803(4) 0.5279(5) 0.76259(15) 0.0578(16) Uani 1 1 d . . . H23A H 0.1153 0.5229 0.7771 0.087 Uiso 1 1 calc R . . H23B H 0.1955 0.4644 0.7492 0.087 Uiso 1 1 calc R . . H23C H 0.1762 0.5804 0.7418 0.087 Uiso 1 1 calc R . . C24 C 0.2838(3) 0.6412(4) 0.90357(13) 0.0456(13) Uani 1 1 d . . . H24A H 0.3345 0.6178 0.9234 0.068 Uiso 1 1 calc R . . H24B H 0.2176 0.6118 0.9101 0.068 Uiso 1 1 calc R . . H24C H 0.2789 0.7137 0.9051 0.068 Uiso 1 1 calc R . . C25 C 0.8111(3) 0.8011(4) 0.86116(16) 0.0427(11) Uani 1 1 d . . . H25A H 0.8088 0.7294 0.8560 0.064 Uiso 1 1 calc R . . H25B H 0.8360 0.8132 0.8891 0.064 Uiso 1 1 calc R . . H25C H 0.8570 0.8326 0.8413 0.064 Uiso 1 1 calc R . . C26 C 0.7125(4) 0.9535(3) 0.86191(16) 0.0434(12) Uani 1 1 d . . . H26A H 0.7555 0.9826 0.8404 0.065 Uiso 1 1 calc R . . H26B H 0.7406 0.9698 0.8890 0.065 Uiso 1 1 calc R . . H26C H 0.6436 0.9805 0.8596 0.065 Uiso 1 1 calc R . . C27 C 0.7269(3) 0.2928(3) 0.95813(12) 0.0237(8) Uani 1 1 d . . . C28 C 0.7238(3) 0.3923(3) 0.97014(11) 0.0233(8) Uani 1 1 d . . . C29 C 0.7177(3) 0.4170(3) 1.01186(12) 0.0275(9) Uani 1 1 d . . . H29 H 0.7107 0.4846 1.0197 0.033 Uiso 1 1 calc R . . C30 C 0.7217(3) 0.3439(3) 1.04190(12) 0.0337(10) Uani 1 1 d . . . H30 H 0.7187 0.3613 1.0702 0.040 Uiso 1 1 calc R . . C31 C 0.7302(3) 0.2449(3) 1.03018(13) 0.0333(10) Uani 1 1 d . . . H31 H 0.7355 0.1947 1.0506 0.040 Uiso 1 1 calc R . . C32 C 0.7310(3) 0.2189(3) 0.98892(13) 0.0282(9) Uani 1 1 d . . . C33 C 0.7294(3) 0.1087(3) 0.97785(14) 0.0339(10) Uani 1 1 d . . . H33A H 0.7240 0.0691 1.0031 0.051 Uiso 1 1 calc R . . H33B H 0.7921 0.0913 0.9633 0.051 Uiso 1 1 calc R . . H33C H 0.6709 0.0950 0.9601 0.051 Uiso 1 1 calc R . . C34 C 0.7193(3) 0.2618(3) 0.91381(12) 0.0235(8) Uani 1 1 d . . . C35 C 0.6249(3) 0.2664(3) 0.89279(12) 0.0309(9) Uani 1 1 d . . . C36 C 0.6223(4) 0.2384(3) 0.85162(14) 0.0418(11) Uani 1 1 d . . . H36 H 0.5603 0.2436 0.8368 0.050 Uiso 1 1 calc R . . C37 C 0.7076(4) 0.2031(4) 0.83177(14) 0.0455(12) Uani 1 1 d . . . H37 H 0.7039 0.1848 0.8036 0.055 Uiso 1 1 calc R . . C38 C 0.7972(4) 0.1945(3) 0.85247(14) 0.0395(11) Uani 1 1 d . . . H38 H 0.8553 0.1699 0.8384 0.047 Uiso 1 1 calc R . . C39 C 0.8054(3) 0.2210(3) 0.89376(13) 0.0307(9) Uani 1 1 d . . . C40 C 0.9057(3) 0.2075(3) 0.91530(13) 0.0342(10) Uani 1 1 d . . . H40A H 0.9194 0.1365 0.9188 0.051 Uiso 1 1 calc R . . H40B H 0.9031 0.2396 0.9424 0.051 Uiso 1 1 calc R . . H40C H 0.9598 0.2377 0.8988 0.051 Uiso 1 1 calc R . . C43 C 0.7807(3) 0.5043(3) 0.91414(11) 0.0218(8) Uani 1 1 d . . . C42 C 0.8786(3) 0.4614(3) 0.90017(11) 0.0231(7) Uani 1 1 d . . . C41 C 0.9620(3) 0.4586(3) 0.92692(12) 0.0257(8) Uani 1 1 d . . . C44 C 1.0555(3) 0.4258(3) 0.91096(13) 0.0320(9) Uani 1 1 d . . . H44 H 1.1130 0.4245 0.9286 0.038 Uiso 1 1 calc R . . C45 C 1.0673(3) 0.3948(3) 0.87000(13) 0.0301(9) Uani 1 1 d . . . C46 C 0.9830(3) 0.4023(3) 0.84436(12) 0.0287(9) Uani 1 1 d . . . H46 H 0.9896 0.3830 0.8164 0.034 Uiso 1 1 calc R . . C47 C 0.8902(3) 0.4367(3) 0.85798(11) 0.0253(8) Uani 1 1 d . . . C48 C 0.9557(3) 0.4883(4) 0.97095(13) 0.0353(10) Uani 1 1 d . . . H48A H 0.9110 0.5461 0.9737 0.053 Uiso 1 1 calc R . . H48B H 1.0237 0.5052 0.9810 0.053 Uiso 1 1 calc R . . H48C H 0.9283 0.4331 0.9872 0.053 Uiso 1 1 calc R . . C49 C 1.1655(3) 0.3516(3) 0.85548(14) 0.0397(11) Uani 1 1 d . . . H49A H 1.2221 0.3894 0.8672 0.060 Uiso 1 1 calc R . . H49B H 1.1685 0.3547 0.8254 0.060 Uiso 1 1 calc R . . H49C H 1.1702 0.2822 0.8644 0.060 Uiso 1 1 calc R . . C50 C 0.8009(3) 0.4468(3) 0.82888(12) 0.0306(9) Uani 1 1 d . . . H50A H 0.7922 0.5168 0.8213 0.046 Uiso 1 1 calc R . . H50B H 0.7392 0.4228 0.8424 0.046 Uiso 1 1 calc R . . H50C H 0.8136 0.4075 0.8040 0.046 Uiso 1 1 calc R . . C51 C 0.4996(3) 0.2361(3) 0.94722(14) 0.0413(11) Uani 1 1 d . . . H51A H 0.4839 0.1700 0.9363 0.062 Uiso 1 1 calc R . . H51B H 0.4383 0.2652 0.9593 0.062 Uiso 1 1 calc R . . H51C H 0.5523 0.2305 0.9684 0.062 Uiso 1 1 calc R . . C52 C 0.4515(3) 0.3286(4) 0.88747(16) 0.0443(12) Uani 1 1 d . . . H52A H 0.4750 0.3747 0.8662 0.066 Uiso 1 1 calc R . . H52B H 0.3993 0.3609 0.9043 0.066 Uiso 1 1 calc R . . H52C H 0.4229 0.2692 0.8745 0.066 Uiso 1 1 calc R . . C55 C 0.4823(3) 0.4846(4) 0.98173(15) 0.0423(12) Uani 1 1 d . . . H53A H 0.4981 0.4500 1.0075 0.063 Uiso 1 1 calc R . . H53B H 0.5080 0.4458 0.9584 0.063 Uiso 1 1 calc R . . H53C H 0.4085 0.4923 0.9792 0.063 Uiso 1 1 calc R . . C56 C 0.5022(4) 0.6401(4) 1.01804(13) 0.0479(13) Uani 1 1 d . . . H54A H 0.4284 0.6492 1.0186 0.072 Uiso 1 1 calc R . . H54B H 0.5356 0.7051 1.0169 0.072 Uiso 1 1 calc R . . H54C H 0.5238 0.6048 1.0429 0.072 Uiso 1 1 calc R . . C53 C 0.7436(3) 0.6837(3) 0.98217(13) 0.0297(9) Uani 1 1 d . . . H55A H 0.7332 0.6725 1.0120 0.036 Uiso 1 1 calc R . . H55B H 0.8155 0.6852 0.9733 0.036 Uiso 1 1 calc R . . C54 C 0.6756(3) 0.8551(3) 0.96502(14) 0.0370(10) Uani 1 1 d . . . H56A H 0.6578 0.8741 0.9932 0.056 Uiso 1 1 calc R . . H56B H 0.6265 0.8840 0.9458 0.056 Uiso 1 1 calc R . . H56C H 0.7438 0.8796 0.9585 0.056 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ta1 0.02151(6) 0.01941(7) 0.02269(6) -0.00236(6) -0.00064(6) 0.00008(6) N1 0.0223(16) 0.0199(17) 0.0197(15) 0.0013(13) -0.0016(12) 0.0009(13) N2 0.0338(19) 0.027(2) 0.041(2) 0.0002(16) 0.0030(16) -0.0057(15) N3 0.0258(15) 0.0157(15) 0.0209(14) -0.0009(13) -0.0007(14) 0.0003(11) N4 0.0268(18) 0.0235(19) 0.047(2) 0.0054(16) -0.0150(15) -0.0037(15) N6 0.0267(17) 0.036(2) 0.0291(17) 0.0008(15) 0.0031(14) 0.0025(15) N5 0.0319(17) 0.0184(17) 0.0292(17) -0.0074(14) -0.0067(14) 0.0017(13) O1 0.0311(15) 0.0223(16) 0.0297(15) -0.0052(12) -0.0112(12) 0.0002(12) O2 0.0272(14) 0.0233(15) 0.0266(13) 0.0010(11) 0.0044(11) 0.0023(11) C1 0.0274(19) 0.023(2) 0.0226(17) -0.0026(15) -0.0002(14) -0.0012(15) C2 0.0227(18) 0.024(2) 0.0244(18) -0.0026(15) -0.0006(14) -0.0023(15) C3 0.0250(19) 0.031(2) 0.0221(18) -0.0022(15) 0.0013(14) 0.0005(16) C4 0.030(2) 0.034(2) 0.0249(18) -0.0073(15) -0.0006(15) 0.0074(17) C5 0.037(2) 0.020(2) 0.037(2) -0.0083(17) -0.0049(17) 0.0069(16) C6 0.034(2) 0.024(2) 0.028(2) -0.0010(17) -0.0045(16) 0.0023(17) C7 0.062(3) 0.024(2) 0.032(2) 0.0058(19) -0.005(2) -0.003(2) C8 0.036(2) 0.020(2) 0.0276(19) -0.0001(16) 0.0043(17) -0.0014(16) C9 0.044(3) 0.020(2) 0.0276(19) -0.0003(16) 0.0086(17) -0.0070(16) C10 0.049(3) 0.041(3) 0.045(3) -0.009(2) 0.020(2) -0.013(2) C11 0.086(4) 0.051(3) 0.031(2) -0.013(2) 0.028(3) -0.006(3) C12 0.061(3) 0.053(3) 0.028(2) -0.006(2) 0.008(2) -0.013(3) C13 0.047(3) 0.028(2) 0.0228(19) -0.0024(17) 0.0030(18) -0.0035(19) C14 0.053(3) 0.036(2) 0.030(2) -0.0018(18) -0.008(2) -0.001(2) C17 0.0258(17) 0.0224(19) 0.0245(16) -0.0018(17) 0.0020(13) -0.0002(17) C16 0.032(2) 0.018(2) 0.0279(18) -0.0012(15) -0.0057(15) -0.0032(15) C15 0.032(2) 0.025(2) 0.030(2) -0.0032(17) -0.0043(16) -0.0021(17) C18 0.043(2) 0.032(2) 0.032(2) -0.0028(17) -0.010(2) -0.006(2) C19 0.036(2) 0.041(3) 0.038(2) 0.002(2) -0.0114(19) -0.015(2) C20 0.024(2) 0.041(3) 0.042(2) 0.003(2) -0.0045(17) -0.0051(18) C21 0.032(2) 0.030(2) 0.035(2) 0.001(2) -0.0034(16) -0.0068(19) C22 0.035(2) 0.040(3) 0.033(2) -0.010(2) -0.0051(18) 0.006(2) C23 0.049(3) 0.081(4) 0.043(3) 0.004(3) -0.015(2) -0.029(3) C24 0.030(2) 0.064(4) 0.043(2) -0.007(2) 0.0036(18) -0.016(2) C25 0.035(2) 0.035(3) 0.059(3) 0.003(2) 0.002(2) 0.000(2) C26 0.048(3) 0.030(3) 0.052(3) -0.006(2) -0.004(2) -0.010(2) C27 0.0165(17) 0.024(2) 0.0303(19) 0.0020(16) -0.0012(15) -0.0008(15) C28 0.0189(16) 0.025(2) 0.0261(17) 0.0019(16) -0.0028(13) -0.0042(15) C29 0.0243(19) 0.028(2) 0.030(2) -0.0007(17) -0.0030(16) -0.0073(16) C30 0.034(2) 0.043(3) 0.0245(19) 0.0050(18) -0.0046(17) -0.0135(19) C31 0.031(2) 0.033(3) 0.035(2) 0.0122(19) -0.0097(18) -0.0117(18) C32 0.0237(19) 0.025(2) 0.036(2) 0.0083(18) -0.0051(16) -0.0056(16) C33 0.032(2) 0.023(2) 0.047(2) 0.011(2) -0.0069(18) -0.0026(19) C34 0.027(2) 0.0119(19) 0.032(2) 0.0033(16) -0.0046(16) -0.0040(15) C35 0.039(2) 0.0164(18) 0.037(2) 0.0007(15) -0.0143(19) -0.0066(18) C36 0.055(3) 0.028(2) 0.043(2) -0.0024(19) -0.021(2) -0.001(2) C37 0.073(4) 0.032(3) 0.032(2) -0.006(2) -0.011(2) 0.000(2) C38 0.058(3) 0.023(2) 0.038(2) -0.0037(19) 0.002(2) 0.001(2) C39 0.043(2) 0.012(2) 0.037(2) 0.0031(17) 0.0008(18) -0.0032(17) C40 0.031(2) 0.026(2) 0.045(2) 0.0075(19) 0.0041(18) 0.0027(17) C43 0.0234(19) 0.020(2) 0.0223(18) -0.0006(15) -0.0025(14) -0.0028(15) C42 0.0244(18) 0.0192(18) 0.0258(17) 0.0019(14) 0.0023(15) -0.0002(16) C41 0.0258(19) 0.025(2) 0.0260(19) 0.0004(16) -0.0015(15) 0.0007(16) C44 0.025(2) 0.028(2) 0.043(2) 0.0058(19) -0.0037(17) 0.0035(17) C45 0.0227(18) 0.027(2) 0.040(2) 0.0031(18) 0.0043(16) 0.0022(16) C46 0.034(2) 0.025(2) 0.0271(19) 0.0066(16) 0.0060(16) 0.0016(16) C47 0.029(2) 0.021(2) 0.0260(18) 0.0015(15) 0.0003(15) -0.0008(15) C48 0.026(2) 0.047(3) 0.033(2) -0.006(2) -0.0070(17) 0.0030(19) C49 0.030(2) 0.041(3) 0.049(3) 0.005(2) 0.0096(18) 0.0108(18) C50 0.034(2) 0.032(2) 0.026(2) -0.0018(17) -0.0010(16) 0.0024(18) C51 0.031(2) 0.039(3) 0.055(3) 0.008(2) -0.007(2) -0.0103(19) C52 0.038(2) 0.030(3) 0.065(3) 0.004(2) -0.027(2) -0.008(2) C55 0.028(2) 0.050(3) 0.048(3) 0.014(2) 0.005(2) -0.010(2) C56 0.058(3) 0.053(4) 0.033(2) 0.002(2) 0.019(2) 0.021(3) C53 0.028(2) 0.029(2) 0.032(2) -0.0070(18) -0.0139(17) 0.0009(17) C54 0.040(2) 0.023(2) 0.048(3) -0.0074(19) -0.0081(19) 0.0022(18) _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 Ta1 N5 1.927(3) . ? Ta1 N6 1.986(3) . ? Ta1 O2 2.157(3) . ? Ta1 C53 2.194(4) . ? Ta1 N1 2.195(3) . ? Ta1 O1 2.202(3) . ? Ta1 N3 2.268(3) . ? Ta1 C17 2.611(3) . ? Ta1 C43 2.645(4) . ? N1 C17 1.316(5) . ? N1 C2 1.429(5) . ? N2 C9 1.428(5) . ? N2 C25 1.462(6) . ? N2 C26 1.500(6) . ? N3 C43 1.313(4) . ? N3 C28 1.426(5) . ? N4 C35 1.418(6) . ? N4 C52 1.453(5) . ? N4 C51 1.480(5) . ? N6 C56 1.456(5) . ? N6 C55 1.461(6) . ? N5 C53 1.426(5) . ? N5 C54 1.456(5) . ? O1 C17 1.289(5) . ? O2 C43 1.306(4) . ? C1 C2 1.402(5) . ? C1 C6 1.426(5) . ? C1 C8 1.504(5) . ? C2 C3 1.389(5) . ? C3 C4 1.391(5) . ? C3 H3 0.9500 . ? C4 C5 1.383(6) . ? C4 H4 0.9500 . ? C5 C6 1.381(5) . ? C5 H5A 0.9500 . ? C6 C7 1.512(6) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C13 1.399(6) . ? C8 C9 1.410(6) . ? C9 C10 1.389(6) . ? C10 C11 1.416(7) . ? C10 H10 0.9500 . ? C11 C12 1.364(7) . ? C11 H11 0.9500 . ? C12 C13 1.380(6) . ? C12 H12 0.9500 . ? C13 C14 1.523(6) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C17 C16 1.496(5) . ? C16 C21 1.395(5) . ? C16 C15 1.404(5) . ? C15 C18 1.368(5) . ? C15 C22 1.516(5) . ? C18 C19 1.395(6) . ? C18 H18 0.9500 . ? C19 C20 1.385(6) . ? C19 C23 1.509(6) . ? C20 C21 1.401(5) . ? C20 H20 0.9500 . ? C21 C24 1.504(6) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C28 1.397(6) . ? C27 C32 1.413(5) . ? C27 C34 1.503(5) . ? C28 C29 1.398(5) . ? C29 C30 1.387(5) . ? C29 H29 0.9500 . ? C30 C31 1.392(6) . ? C30 H30 0.9500 . ? C31 C32 1.385(6) . ? C31 H31 0.9500 . ? C32 C33 1.527(6) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C39 1.418(6) . ? C34 C35 1.420(5) . ? C35 C36 1.390(6) . ? C36 C37 1.380(7) . ? C36 H36 0.9500 . ? C37 C38 1.363(7) . ? C37 H37 0.9500 . ? C38 C39 1.392(6) . ? C38 H38 0.9500 . ? C39 C40 1.506(6) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C43 C42 1.484(5) . ? C42 C41 1.401(5) . ? C42 C47 1.419(5) . ? C41 C44 1.408(5) . ? C41 C48 1.487(5) . ? C44 C45 1.403(6) . ? C44 H44 0.9500 . ? C45 C46 1.392(5) . ? C45 C49 1.494(5) . ? C46 C47 1.379(5) . ? C46 H46 0.9500 . ? C47 C50 1.515(5) . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 H49A 0.9800 . ? C49 H49B 0.9800 . ? C49 H49C 0.9800 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C55 H53A 0.9800 . ? C55 H53B 0.9800 . ? C55 H53C 0.9800 . ? C56 H54A 0.9800 . ? C56 H54B 0.9800 . ? C56 H54C 0.9800 . ? C53 H55A 0.9900 . ? C53 H55B 0.9900 . ? C54 H56A 0.9800 . ? C54 H56B 0.9800 . ? C54 H56C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N5 Ta1 N6 99.72(15) . . ? N5 Ta1 O2 100.71(13) . . ? N6 Ta1 O2 152.86(13) . . ? N5 Ta1 C53 39.84(14) . . ? N6 Ta1 C53 96.53(16) . . ? O2 Ta1 C53 87.91(14) . . ? N5 Ta1 N1 89.15(13) . . ? N6 Ta1 N1 100.04(13) . . ? O2 Ta1 N1 97.95(11) . . ? C53 Ta1 N1 128.46(14) . . ? N5 Ta1 O1 148.29(12) . . ? N6 Ta1 O1 91.47(13) . . ? O2 Ta1 O1 80.33(11) . . ? C53 Ta1 O1 166.94(13) . . ? N1 Ta1 O1 59.57(10) . . ? N5 Ta1 N3 127.10(12) . . ? N6 Ta1 N3 94.28(13) . . ? O2 Ta1 N3 59.00(10) . . ? C53 Ta1 N3 88.18(13) . . ? N1 Ta1 N3 137.99(11) . . ? O1 Ta1 N3 80.92(11) . . ? N5 Ta1 C17 119.39(14) . . ? N6 Ta1 C17 94.02(13) . . ? O2 Ta1 C17 91.36(10) . . ? C53 Ta1 C17 158.18(15) . . ? N1 Ta1 C17 30.24(12) . . ? O1 Ta1 C17 29.54(12) . . ? N3 Ta1 C17 110.03(12) . . ? N5 Ta1 C43 115.15(13) . . ? N6 Ta1 C43 124.02(13) . . ? O2 Ta1 C43 29.38(10) . . ? C53 Ta1 C43 85.81(14) . . ? N1 Ta1 C43 121.64(11) . . ? O1 Ta1 C43 81.16(11) . . ? N3 Ta1 C43 29.74(11) . . ? C17 Ta1 C43 103.92(11) . . ? C17 N1 C2 126.5(3) . . ? C17 N1 Ta1 92.7(2) . . ? C2 N1 Ta1 137.4(2) . . ? C9 N2 C25 115.8(4) . . ? C9 N2 C26 111.5(4) . . ? C25 N2 C26 110.2(4) . . ? C43 N3 C28 129.7(3) . . ? C43 N3 Ta1 91.3(2) . . ? C28 N3 Ta1 137.4(2) . . ? C35 N4 C52 116.2(4) . . ? C35 N4 C51 115.6(3) . . ? C52 N4 C51 109.3(3) . . ? C56 N6 C55 112.0(4) . . ? C56 N6 Ta1 126.2(3) . . ? C55 N6 Ta1 121.6(3) . . ? C53 N5 C54 123.3(3) . . ? C53 N5 Ta1 80.2(2) . . ? C54 N5 Ta1 156.3(3) . . ? C17 O1 Ta1 93.1(2) . . ? C43 O2 Ta1 96.5(2) . . ? C2 C1 C6 118.4(3) . . ? C2 C1 C8 122.1(3) . . ? C6 C1 C8 119.5(3) . . ? C3 C2 C1 120.6(4) . . ? C3 C2 N1 116.2(3) . . ? C1 C2 N1 123.0(3) . . ? C2 C3 C4 120.5(4) . . ? C2 C3 H3 119.8 . . ? C4 C3 H3 119.8 . . ? C5 C4 C3 119.4(4) . . ? C5 C4 H4 120.3 . . ? C3 C4 H4 120.3 . . ? C6 C5 C4 121.6(4) . . ? C6 C5 H5A 119.2 . . ? C4 C5 H5A 119.2 . . ? C5 C6 C1 119.6(4) . . ? C5 C6 C7 118.2(4) . . ? C1 C6 C7 122.3(4) . . ? C6 C7 H7A 109.5 . . ? C6 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C6 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C13 C8 C9 119.8(4) . . ? C13 C8 C1 120.1(4) . . ? C9 C8 C1 120.0(4) . . ? C10 C9 C8 119.9(4) . . ? C10 C9 N2 120.7(4) . . ? C8 C9 N2 119.3(4) . . ? C9 C10 C11 118.8(5) . . ? C9 C10 H10 120.6 . . ? C11 C10 H10 120.6 . . ? C12 C11 C10 120.8(4) . . ? C12 C11 H11 119.6 . . ? C10 C11 H11 119.6 . . ? C11 C12 C13 121.1(5) . . ? C11 C12 H12 119.5 . . ? C13 C12 H12 119.5 . . ? C12 C13 C8 119.6(4) . . ? C12 C13 C14 118.2(4) . . ? C8 C13 C14 122.1(4) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O1 C17 N1 113.9(3) . . ? O1 C17 C16 116.7(4) . . ? N1 C17 C16 129.4(4) . . ? O1 C17 Ta1 57.37(18) . . ? N1 C17 Ta1 57.09(19) . . ? C16 C17 Ta1 169.9(3) . . ? C21 C16 C15 121.0(3) . . ? C21 C16 C17 120.7(3) . . ? C15 C16 C17 117.8(3) . . ? C18 C15 C16 119.1(4) . . ? C18 C15 C22 119.9(4) . . ? C16 C15 C22 121.0(4) . . ? C15 C18 C19 121.9(4) . . ? C15 C18 H18 119.1 . . ? C19 C18 H18 119.1 . . ? C20 C19 C18 118.0(4) . . ? C20 C19 C23 120.7(4) . . ? C18 C19 C23 121.3(4) . . ? C19 C20 C21 122.3(4) . . ? C19 C20 H20 118.9 . . ? C21 C20 H20 118.9 . . ? C16 C21 C20 117.6(4) . . ? C16 C21 C24 123.1(3) . . ? C20 C21 C24 119.2(4) . . ? C15 C22 H22A 109.5 . . ? C15 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C15 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C19 C23 H23A 109.5 . . ? C19 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C19 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C21 C24 H24A 109.5 . . ? C21 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C21 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N2 C25 H25A 109.5 . . ? N2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N2 C26 H26A 109.5 . . ? N2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 C32 118.7(4) . . ? C28 C27 C34 122.2(3) . . ? C32 C27 C34 119.0(4) . . ? C27 C28 C29 120.1(4) . . ? C27 C28 N3 125.4(3) . . ? C29 C28 N3 114.4(3) . . ? C30 C29 C28 120.8(4) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C29 C30 C31 119.4(4) . . ? C29 C30 H30 120.3 . . ? C31 C30 H30 120.3 . . ? C32 C31 C30 120.5(4) . . ? C32 C31 H31 119.8 . . ? C30 C31 H31 119.8 . . ? C31 C32 C27 120.5(4) . . ? C31 C32 C33 118.3(4) . . ? C27 C32 C33 121.2(4) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C39 C34 C35 119.7(4) . . ? C39 C34 C27 119.6(4) . . ? C35 C34 C27 120.5(4) . . ? C36 C35 N4 121.5(4) . . ? C36 C35 C34 118.2(4) . . ? N4 C35 C34 120.3(3) . . ? C37 C36 C35 121.5(5) . . ? C37 C36 H36 119.2 . . ? C35 C36 H36 119.2 . . ? C38 C37 C36 120.2(4) . . ? C38 C37 H37 119.9 . . ? C36 C37 H37 119.9 . . ? C37 C38 C39 121.4(5) . . ? C37 C38 H38 119.3 . . ? C39 C38 H38 119.3 . . ? C38 C39 C34 118.7(4) . . ? C38 C39 C40 119.0(4) . . ? C34 C39 C40 122.3(4) . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? O2 C43 N3 112.8(3) . . ? O2 C43 C42 116.2(3) . . ? N3 C43 C42 130.7(3) . . ? O2 C43 Ta1 54.10(18) . . ? N3 C43 Ta1 59.00(19) . . ? C42 C43 Ta1 166.2(3) . . ? C41 C42 C47 120.6(3) . . ? C41 C42 C43 120.1(3) . . ? C47 C42 C43 118.7(3) . . ? C42 C41 C44 117.7(4) . . ? C42 C41 C48 123.1(3) . . ? C44 C41 C48 119.2(4) . . ? C45 C44 C41 122.7(4) . . ? C45 C44 H44 118.7 . . ? C41 C44 H44 118.7 . . ? C46 C45 C44 117.2(4) . . ? C46 C45 C49 122.0(4) . . ? C44 C45 C49 120.7(4) . . ? C47 C46 C45 122.6(4) . . ? C47 C46 H46 118.7 . . ? C45 C46 H46 118.7 . . ? C46 C47 C42 118.9(3) . . ? C46 C47 C50 121.1(3) . . ? C42 C47 C50 119.9(3) . . ? C41 C48 H48A 109.5 . . ? C41 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C41 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C45 C49 H49A 109.5 . . ? C45 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C45 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C47 C50 H50A 109.5 . . ? C47 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C47 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? N4 C51 H51A 109.5 . . ? N4 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? N4 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? N4 C52 H52A 109.5 . . ? N4 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? N4 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N6 C55 H53A 109.5 . . ? N6 C55 H53B 109.5 . . ? H53A C55 H53B 109.5 . . ? N6 C55 H53C 109.5 . . ? H53A C55 H53C 109.5 . . ? H53B C55 H53C 109.5 . . ? N6 C56 H54A 109.5 . . ? N6 C56 H54B 109.5 . . ? H54A C56 H54B 109.5 . . ? N6 C56 H54C 109.5 . . ? H54A C56 H54C 109.5 . . ? H54B C56 H54C 109.5 . . ? N5 C53 Ta1 59.95(18) . . ? N5 C53 H55A 117.8 . . ? Ta1 C53 H55A 117.8 . . ? N5 C53 H55B 117.8 . . ? Ta1 C53 H55B 117.8 . . ? H55A C53 H55B 114.9 . . ? N5 C54 H56A 109.5 . . ? N5 C54 H56B 109.5 . . ? H56A C54 H56B 109.5 . . ? N5 C54 H56C 109.5 . . ? H56A C54 H56C 109.5 . . ? H56B C54 H56C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Ta1 N1 C17 179.6(2) . . . . ? N6 Ta1 N1 C17 -80.7(2) . . . . ? O2 Ta1 N1 C17 78.9(2) . . . . ? C53 Ta1 N1 C17 172.6(2) . . . . ? O1 Ta1 N1 C17 5.10(19) . . . . ? N3 Ta1 N1 C17 27.4(3) . . . . ? C43 Ta1 N1 C17 60.3(2) . . . . ? N5 Ta1 N1 C2 -21.7(4) . . . . ? N6 Ta1 N1 C2 78.0(4) . . . . ? O2 Ta1 N1 C2 -122.4(4) . . . . ? C53 Ta1 N1 C2 -28.8(4) . . . . ? O1 Ta1 N1 C2 163.8(4) . . . . ? N3 Ta1 N1 C2 -174.0(3) . . . . ? C17 Ta1 N1 C2 158.7(5) . . . . ? C43 Ta1 N1 C2 -141.1(3) . . . . ? N5 Ta1 N3 C43 -75.6(3) . . . . ? N6 Ta1 N3 C43 178.9(2) . . . . ? O2 Ta1 N3 C43 3.9(2) . . . . ? C53 Ta1 N3 C43 -84.7(2) . . . . ? N1 Ta1 N3 C43 68.7(3) . . . . ? O1 Ta1 N3 C43 88.0(2) . . . . ? C17 Ta1 N3 C43 83.0(2) . . . . ? N5 Ta1 N3 C28 90.1(4) . . . . ? N6 Ta1 N3 C28 -15.5(4) . . . . ? O2 Ta1 N3 C28 169.6(4) . . . . ? C53 Ta1 N3 C28 80.9(4) . . . . ? N1 Ta1 N3 C28 -125.6(3) . . . . ? O1 Ta1 N3 C28 -106.3(3) . . . . ? C17 Ta1 N3 C28 -111.4(3) . . . . ? C43 Ta1 N3 C28 165.6(5) . . . . ? N5 Ta1 N6 C56 0.1(4) . . . . ? O2 Ta1 N6 C56 138.5(3) . . . . ? C53 Ta1 N6 C56 40.2(4) . . . . ? N1 Ta1 N6 C56 -90.8(3) . . . . ? O1 Ta1 N6 C56 -150.1(3) . . . . ? N3 Ta1 N6 C56 128.9(3) . . . . ? C17 Ta1 N6 C56 -120.6(3) . . . . ? C43 Ta1 N6 C56 129.6(3) . . . . ? N5 Ta1 N6 C55 -173.5(3) . . . . ? O2 Ta1 N6 C55 -35.2(5) . . . . ? C53 Ta1 N6 C55 -133.4(3) . . . . ? N1 Ta1 N6 C55 95.6(3) . . . . ? O1 Ta1 N6 C55 36.2(3) . . . . ? N3 Ta1 N6 C55 -44.8(3) . . . . ? C17 Ta1 N6 C55 65.7(3) . . . . ? C43 Ta1 N6 C55 -44.1(4) . . . . ? N6 Ta1 N5 C53 88.6(2) . . . . ? O2 Ta1 N5 C53 -73.5(2) . . . . ? N1 Ta1 N5 C53 -171.4(2) . . . . ? O1 Ta1 N5 C53 -162.4(2) . . . . ? N3 Ta1 N5 C53 -14.4(3) . . . . ? C17 Ta1 N5 C53 -171.2(2) . . . . ? C43 Ta1 N5 C53 -46.5(3) . . . . ? N6 Ta1 N5 C54 -98.7(8) . . . . ? O2 Ta1 N5 C54 99.2(8) . . . . ? C53 Ta1 N5 C54 172.7(9) . . . . ? N1 Ta1 N5 C54 1.3(8) . . . . ? O1 Ta1 N5 C54 10.3(9) . . . . ? N3 Ta1 N5 C54 158.3(7) . . . . ? C17 Ta1 N5 C54 1.5(8) . . . . ? C43 Ta1 N5 C54 126.2(7) . . . . ? N5 Ta1 O1 C17 -15.7(4) . . . . ? N6 Ta1 O1 C17 95.6(2) . . . . ? O2 Ta1 O1 C17 -110.5(2) . . . . ? C53 Ta1 O1 C17 -136.5(6) . . . . ? N1 Ta1 O1 C17 -5.2(2) . . . . ? N3 Ta1 O1 C17 -170.3(2) . . . . ? C43 Ta1 O1 C17 -140.2(2) . . . . ? N5 Ta1 O2 C43 123.1(2) . . . . ? N6 Ta1 O2 C43 -15.1(4) . . . . ? C53 Ta1 O2 C43 85.2(2) . . . . ? N1 Ta1 O2 C43 -146.3(2) . . . . ? O1 Ta1 O2 C43 -89.1(2) . . . . ? N3 Ta1 O2 C43 -4.0(2) . . . . ? C17 Ta1 O2 C43 -116.6(2) . . . . ? C6 C1 C2 C3 -0.1(6) . . . . ? C8 C1 C2 C3 177.9(4) . . . . ? C6 C1 C2 N1 -176.5(3) . . . . ? C8 C1 C2 N1 1.5(6) . . . . ? C17 N1 C2 C3 106.2(4) . . . . ? Ta1 N1 C2 C3 -46.9(5) . . . . ? C17 N1 C2 C1 -77.3(5) . . . . ? Ta1 N1 C2 C1 129.6(4) . . . . ? C1 C2 C3 C4 0.9(6) . . . . ? N1 C2 C3 C4 177.5(3) . . . . ? C2 C3 C4 C5 -0.8(6) . . . . ? C3 C4 C5 C6 -0.1(6) . . . . ? C4 C5 C6 C1 0.8(6) . . . . ? C4 C5 C6 C7 -178.4(4) . . . . ? C2 C1 C6 C5 -0.7(6) . . . . ? C8 C1 C6 C5 -178.8(4) . . . . ? C2 C1 C6 C7 178.5(4) . . . . ? C8 C1 C6 C7 0.4(6) . . . . ? C2 C1 C8 C13 110.5(5) . . . . ? C6 C1 C8 C13 -71.4(5) . . . . ? C2 C1 C8 C9 -70.6(5) . . . . ? C6 C1 C8 C9 107.4(4) . . . . ? C13 C8 C9 C10 -3.5(6) . . . . ? C1 C8 C9 C10 177.7(4) . . . . ? C13 C8 C9 N2 177.3(4) . . . . ? C1 C8 C9 N2 -1.5(6) . . . . ? C25 N2 C9 C10 -21.5(6) . . . . ? C26 N2 C9 C10 105.5(5) . . . . ? C25 N2 C9 C8 157.7(4) . . . . ? C26 N2 C9 C8 -75.3(5) . . . . ? C8 C9 C10 C11 2.9(7) . . . . ? N2 C9 C10 C11 -177.9(4) . . . . ? C9 C10 C11 C12 -1.4(8) . . . . ? C10 C11 C12 C13 0.4(9) . . . . ? C11 C12 C13 C8 -0.9(8) . . . . ? C11 C12 C13 C14 -178.0(5) . . . . ? C9 C8 C13 C12 2.4(7) . . . . ? C1 C8 C13 C12 -178.7(4) . . . . ? C9 C8 C13 C14 179.5(4) . . . . ? C1 C8 C13 C14 -1.7(6) . . . . ? Ta1 O1 C17 N1 8.2(3) . . . . ? Ta1 O1 C17 C16 -170.6(3) . . . . ? C2 N1 C17 O1 -170.4(3) . . . . ? Ta1 N1 C17 O1 -8.2(3) . . . . ? C2 N1 C17 C16 8.2(6) . . . . ? Ta1 N1 C17 C16 170.4(3) . . . . ? C2 N1 C17 Ta1 -162.2(4) . . . . ? N5 Ta1 C17 O1 170.6(2) . . . . ? N6 Ta1 C17 O1 -85.9(2) . . . . ? O2 Ta1 C17 O1 67.5(2) . . . . ? C53 Ta1 C17 O1 155.3(4) . . . . ? N1 Ta1 C17 O1 171.0(3) . . . . ? N3 Ta1 C17 O1 10.2(2) . . . . ? C43 Ta1 C17 O1 40.6(2) . . . . ? N5 Ta1 C17 N1 -0.4(3) . . . . ? N6 Ta1 C17 N1 103.1(2) . . . . ? O2 Ta1 C17 N1 -103.5(2) . . . . ? C53 Ta1 C17 N1 -15.8(5) . . . . ? O1 Ta1 C17 N1 -171.0(3) . . . . ? N3 Ta1 C17 N1 -160.9(2) . . . . ? C43 Ta1 C17 N1 -130.4(2) . . . . ? N5 Ta1 C17 C16 -133.0(16) . . . . ? N6 Ta1 C17 C16 -29.5(16) . . . . ? O2 Ta1 C17 C16 123.9(16) . . . . ? C53 Ta1 C17 C16 -148.3(15) . . . . ? N1 Ta1 C17 C16 -132.5(17) . . . . ? O1 Ta1 C17 C16 56.4(16) . . . . ? N3 Ta1 C17 C16 66.6(16) . . . . ? C43 Ta1 C17 C16 97.1(16) . . . . ? O1 C17 C16 C21 108.9(4) . . . . ? N1 C17 C16 C21 -69.7(6) . . . . ? Ta1 C17 C16 C21 57.1(18) . . . . ? O1 C17 C16 C15 -63.1(5) . . . . ? N1 C17 C16 C15 118.4(4) . . . . ? Ta1 C17 C16 C15 -114.8(15) . . . . ? C21 C16 C15 C18 3.5(6) . . . . ? C17 C16 C15 C18 175.4(4) . . . . ? C21 C16 C15 C22 -175.1(4) . . . . ? C17 C16 C15 C22 -3.2(6) . . . . ? C16 C15 C18 C19 0.2(7) . . . . ? C22 C15 C18 C19 178.9(4) . . . . ? C15 C18 C19 C20 -2.9(7) . . . . ? C15 C18 C19 C23 179.5(5) . . . . ? C18 C19 C20 C21 2.0(7) . . . . ? C23 C19 C20 C21 179.6(5) . . . . ? C15 C16 C21 C20 -4.3(7) . . . . ? C17 C16 C21 C20 -176.0(4) . . . . ? C15 C16 C21 C24 172.0(4) . . . . ? C17 C16 C21 C24 0.3(7) . . . . ? C19 C20 C21 C16 1.5(7) . . . . ? C19 C20 C21 C24 -174.9(5) . . . . ? C32 C27 C28 C29 -4.4(5) . . . . ? C34 C27 C28 C29 171.6(3) . . . . ? C32 C27 C28 N3 -178.6(3) . . . . ? C34 C27 C28 N3 -2.6(6) . . . . ? C43 N3 C28 C27 -61.5(5) . . . . ? Ta1 N3 C28 C27 137.3(3) . . . . ? C43 N3 C28 C29 124.0(4) . . . . ? Ta1 N3 C28 C29 -37.2(5) . . . . ? C27 C28 C29 C30 4.5(6) . . . . ? N3 C28 C29 C30 179.3(3) . . . . ? C28 C29 C30 C31 -1.1(6) . . . . ? C29 C30 C31 C32 -2.3(6) . . . . ? C30 C31 C32 C27 2.3(6) . . . . ? C30 C31 C32 C33 -173.7(4) . . . . ? C28 C27 C32 C31 1.1(6) . . . . ? C34 C27 C32 C31 -175.0(4) . . . . ? C28 C27 C32 C33 177.0(4) . . . . ? C34 C27 C32 C33 0.9(6) . . . . ? C28 C27 C34 C39 110.7(4) . . . . ? C32 C27 C34 C39 -73.3(5) . . . . ? C28 C27 C34 C35 -73.8(5) . . . . ? C32 C27 C34 C35 102.2(4) . . . . ? C52 N4 C35 C36 -15.4(6) . . . . ? C51 N4 C35 C36 114.6(4) . . . . ? C52 N4 C35 C34 163.6(4) . . . . ? C51 N4 C35 C34 -66.4(5) . . . . ? C39 C34 C35 C36 -5.5(6) . . . . ? C27 C34 C35 C36 179.0(4) . . . . ? C39 C34 C35 N4 175.4(3) . . . . ? C27 C34 C35 N4 -0.1(6) . . . . ? N4 C35 C36 C37 -178.4(4) . . . . ? C34 C35 C36 C37 2.6(6) . . . . ? C35 C36 C37 C38 0.4(7) . . . . ? C36 C37 C38 C39 -0.3(7) . . . . ? C37 C38 C39 C34 -2.7(7) . . . . ? C37 C38 C39 C40 178.5(4) . . . . ? C35 C34 C39 C38 5.7(6) . . . . ? C27 C34 C39 C38 -178.8(4) . . . . ? C35 C34 C39 C40 -175.7(4) . . . . ? C27 C34 C39 C40 -0.1(6) . . . . ? Ta1 O2 C43 N3 6.4(3) . . . . ? Ta1 O2 C43 C42 -168.5(3) . . . . ? C28 N3 C43 O2 -173.4(3) . . . . ? Ta1 N3 C43 O2 -6.0(3) . . . . ? C28 N3 C43 C42 0.5(6) . . . . ? Ta1 N3 C43 C42 167.9(4) . . . . ? C28 N3 C43 Ta1 -167.4(4) . . . . ? N5 Ta1 C43 O2 -65.4(2) . . . . ? N6 Ta1 C43 O2 171.8(2) . . . . ? C53 Ta1 C43 O2 -93.2(2) . . . . ? N1 Ta1 C43 O2 40.2(2) . . . . ? O1 Ta1 C43 O2 86.0(2) . . . . ? N3 Ta1 C43 O2 173.1(3) . . . . ? C17 Ta1 C43 O2 67.0(2) . . . . ? N5 Ta1 C43 N3 121.4(2) . . . . ? N6 Ta1 C43 N3 -1.4(3) . . . . ? O2 Ta1 C43 N3 -173.1(3) . . . . ? C53 Ta1 C43 N3 93.7(2) . . . . ? N1 Ta1 C43 N3 -132.9(2) . . . . ? O1 Ta1 C43 N3 -87.2(2) . . . . ? C17 Ta1 C43 N3 -106.1(2) . . . . ? N5 Ta1 C43 C42 -16.8(11) . . . . ? N6 Ta1 C43 C42 -139.6(10) . . . . ? O2 Ta1 C43 C42 48.7(10) . . . . ? C53 Ta1 C43 C42 -44.5(11) . . . . ? N1 Ta1 C43 C42 88.9(11) . . . . ? O1 Ta1 C43 C42 134.6(11) . . . . ? N3 Ta1 C43 C42 -138.2(12) . . . . ? C17 Ta1 C43 C42 115.7(11) . . . . ? O2 C43 C42 C41 109.0(4) . . . . ? N3 C43 C42 C41 -64.8(6) . . . . ? Ta1 C43 C42 C41 66.3(12) . . . . ? O2 C43 C42 C47 -62.1(5) . . . . ? N3 C43 C42 C47 124.1(4) . . . . ? Ta1 C43 C42 C47 -104.8(10) . . . . ? C47 C42 C41 C44 -3.2(6) . . . . ? C43 C42 C41 C44 -174.2(3) . . . . ? C47 C42 C41 C48 177.0(4) . . . . ? C43 C42 C41 C48 6.0(6) . . . . ? C42 C41 C44 C45 -1.0(6) . . . . ? C48 C41 C44 C45 178.8(4) . . . . ? C41 C44 C45 C46 3.2(6) . . . . ? C41 C44 C45 C49 -174.2(4) . . . . ? C44 C45 C46 C47 -1.2(6) . . . . ? C49 C45 C46 C47 176.2(4) . . . . ? C45 C46 C47 C42 -2.8(6) . . . . ? C45 C46 C47 C50 178.1(4) . . . . ? C41 C42 C47 C46 5.1(6) . . . . ? C43 C42 C47 C46 176.2(3) . . . . ? C41 C42 C47 C50 -175.9(4) . . . . ? C43 C42 C47 C50 -4.8(5) . . . . ? C54 N5 C53 Ta1 -176.5(4) . . . . ? N6 Ta1 C53 N5 -97.3(2) . . . . ? O2 Ta1 C53 N5 109.5(2) . . . . ? N1 Ta1 C53 N5 11.0(3) . . . . ? O1 Ta1 C53 N5 135.2(6) . . . . ? N3 Ta1 C53 N5 168.6(2) . . . . ? C17 Ta1 C53 N5 21.1(5) . . . . ? C43 Ta1 C53 N5 138.9(2) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.000 0.245 0.750 560 169 ' ' 2 0.500 0.963 0.250 560 169 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.87 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.740 _refine_diff_density_min -1.338 _refine_diff_density_rms 0.126 # Attachment '- compound 26.cif' data_compound26 _database_code_depnum_ccdc_archive 'CCDC 800129' #TrackingRef '- compound 26.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C84 H96 N6 O4 V2' _chemical_formula_sum 'C84 H96 N6 O4 V2' _chemical_formula_weight 1355.55 _chemical_absolute_configuration rmad loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' V V 0.0687 2.1097 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 24.254(5) _cell_length_b 21.750(3) _cell_length_c 21.964(4) _cell_angle_alpha 90.00 _cell_angle_beta 115.942(4) _cell_angle_gamma 90.00 _cell_volume 10419(3) _cell_formula_units_Z 4 _cell_measurement_temperature 113(2) _cell_measurement_reflns_used 6630 _cell_measurement_theta_min 27.6 _cell_measurement_theta_max 72.5 _exptl_crystal_description prism _exptl_crystal_colour red _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 0.864 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2880 _exptl_absorpt_coefficient_mu 1.799 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5798 _exptl_absorpt_correction_T_max 0.6327 _exptl_absorpt_process_details CrystalClear _exptl_special_details ; ? ; _diffrn_ambient_temperature 113(2) _diffrn_radiation_wavelength 1.54187 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku Saturn' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean 14.63 _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 72632 _diffrn_reflns_av_R_equivalents 0.0507 _diffrn_reflns_av_sigmaI/netI 0.0559 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.24 _diffrn_reflns_theta_max 72.68 _reflns_number_total 19202 _reflns_number_gt 16455 _reflns_threshold_expression >2sigma(I) _computing_data_collection CrystalClear _computing_cell_refinement CrystalClear _computing_data_reduction CrystalClear _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material 'CrystalStructure 3.8' _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. The disorders solvents were removed by SQEEZE programm. C81 was isotropic restrained. ; _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^)+(0.0362P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.033(3) _refine_ls_number_reflns 19202 _refine_ls_number_parameters 883 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0404 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0885 _refine_ls_wR_factor_gt 0.0853 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 1.002 _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 0.5000 0.515954(18) 0.5000 0.02858(12) Uani 1 2 d S . . V2 V 0.5000 0.647323(18) 0.5000 0.02893(12) Uani 1 2 d S . . V3 V 0.500672(18) 0.077087(19) 0.065892(19) 0.03960(9) Uani 1 1 d . . . N1 N 0.46645(7) 0.44303(6) 0.43158(9) 0.0265(4) Uani 1 1 d . . . N2 N 0.54026(8) 0.72093(6) 0.47107(9) 0.0276(4) Uani 1 1 d . . . N3 N 0.50175(7) 0.58114(8) 0.43258(8) 0.0298(3) Uani 1 1 d . . . N4 N 0.53794(8) 0.12872(7) 0.15550(9) 0.0341(4) Uani 1 1 d . . . N5 N 0.46518(9) 0.02675(7) 0.12220(10) 0.0384(4) Uani 1 1 d . . . N6 N 0.5000 0.14581(12) 0.0000 0.0410(7) Uani 1 2 d S . . N7 N 0.5000 0.00795(12) 0.0000 0.0467(7) Uani 1 2 d S . . O1 O 0.40550(6) 0.50378(6) 0.45336(8) 0.0320(3) Uani 1 1 d . . . O2 O 0.59295(6) 0.65954(6) 0.55531(8) 0.0333(4) Uani 1 1 d . . . O3 O 0.59436(7) 0.07224(7) 0.12335(7) 0.0410(4) Uani 1 1 d . . . O4 O 0.40635(7) 0.08095(9) 0.03434(7) 0.0479(4) Uani 1 1 d . . . C1 C 0.51050(10) 0.34123(8) 0.47238(11) 0.0284(5) Uani 1 1 d . . . C2 C 0.49342(9) 0.38845(8) 0.42366(11) 0.0286(5) Uani 1 1 d . . . C3 C 0.51151(10) 0.38598(8) 0.37101(12) 0.0302(5) Uani 1 1 d . . . H3 H 0.4998 0.4179 0.3382 0.036 Uiso 1 1 calc R . . C4 C 0.54627(10) 0.33734(8) 0.36694(11) 0.0327(5) Uani 1 1 d . . . H4 H 0.5562 0.3349 0.3297 0.039 Uiso 1 1 calc R . . C5 C 0.56698(10) 0.29181(8) 0.41655(11) 0.0315(5) Uani 1 1 d . . . C6 C 0.55018(9) 0.29374(8) 0.47034(11) 0.0299(5) Uani 1 1 d . . . C7 C 0.57793(11) 0.24850(8) 0.52773(12) 0.0353(5) Uani 1 1 d . . . H7A H 0.5462 0.2360 0.5421 0.042 Uiso 1 1 calc R . . H7B H 0.6112 0.2692 0.5666 0.042 Uiso 1 1 calc R . . C8 C 0.60400(11) 0.19076(9) 0.50998(13) 0.0399(6) Uani 1 1 d . . . H8A H 0.6275 0.1665 0.5515 0.048 Uiso 1 1 calc R . . H8B H 0.5700 0.1648 0.4782 0.048 Uiso 1 1 calc R . . C9 C 0.64581(11) 0.20913(9) 0.47749(12) 0.0394(5) Uani 1 1 d . . . H9A H 0.6788 0.2364 0.5085 0.047 Uiso 1 1 calc R . . H9B H 0.6650 0.1720 0.4690 0.047 Uiso 1 1 calc R . . C10 C 0.60865(11) 0.24224(9) 0.41135(13) 0.0393(6) Uani 1 1 d . . . H10A H 0.5834 0.2118 0.3770 0.047 Uiso 1 1 calc R . . H10B H 0.6371 0.2611 0.3954 0.047 Uiso 1 1 calc R . . C11 C 0.41017(9) 0.45344(8) 0.42417(11) 0.0304(5) Uani 1 1 d . . . C12 C 0.35548(10) 0.41355(9) 0.38911(13) 0.0353(5) Uani 1 1 d . . . C13 C 0.33687(10) 0.39526(9) 0.32217(13) 0.0388(5) Uani 1 1 d . . . C14 C 0.28558(11) 0.35711(11) 0.29183(14) 0.0493(6) Uani 1 1 d . . . H14 H 0.2732 0.3442 0.2464 0.059 Uiso 1 1 calc R . . C15 C 0.25248(12) 0.33764(11) 0.32517(16) 0.0552(7) Uani 1 1 d . . . C16 C 0.27024(11) 0.35774(11) 0.39064(15) 0.0505(7) Uani 1 1 d . . . H16 H 0.2470 0.3451 0.4138 0.061 Uiso 1 1 calc R . . C17 C 0.32133(10) 0.39621(9) 0.42462(13) 0.0398(5) Uani 1 1 d . . . C18 C 0.36598(12) 0.41743(12) 0.27760(14) 0.0527(6) Uani 1 1 d . . . H18A H 0.3935 0.4519 0.2997 0.079 Uiso 1 1 calc R . . H18B H 0.3339 0.4310 0.2339 0.079 Uiso 1 1 calc R . . H18C H 0.3894 0.3838 0.2704 0.079 Uiso 1 1 calc R . . C19 C 0.19607(15) 0.29791(15) 0.2895(2) 0.0852(11) Uani 1 1 d . . . H19A H 0.1971 0.2788 0.2496 0.128 Uiso 1 1 calc R . . H19B H 0.1592 0.3234 0.2754 0.128 Uiso 1 1 calc R . . H19C H 0.1954 0.2658 0.3205 0.128 Uiso 1 1 calc R . . C20 C 0.33594(11) 0.41731(11) 0.49411(13) 0.0467(6) Uani 1 1 d . . . H20A H 0.3176 0.4578 0.4921 0.070 Uiso 1 1 calc R . . H20B H 0.3805 0.4201 0.5205 0.070 Uiso 1 1 calc R . . H20C H 0.3194 0.3880 0.5157 0.070 Uiso 1 1 calc R . . C21 C 0.49305(9) 0.82223(8) 0.46320(11) 0.0263(4) Uani 1 1 d . . . C22 C 0.51500(9) 0.77611(8) 0.43541(11) 0.0284(5) Uani 1 1 d . . . C23 C 0.50317(10) 0.77849(9) 0.36732(12) 0.0318(5) Uani 1 1 d . . . H23 H 0.5188 0.7473 0.3488 0.038 Uiso 1 1 calc R . . C24 C 0.46904(10) 0.82582(9) 0.32682(12) 0.0333(5) Uani 1 1 d . . . H24 H 0.4629 0.8281 0.2811 0.040 Uiso 1 1 calc R . . C25 C 0.44311(10) 0.87088(8) 0.35219(11) 0.0317(5) Uani 1 1 d . . . C26 C 0.45461(9) 0.86869(8) 0.41941(11) 0.0283(4) Uani 1 1 d . . . C27 C 0.42333(10) 0.91397(8) 0.44704(12) 0.0315(5) Uani 1 1 d . . . H27A H 0.4526 0.9262 0.4934 0.038 Uiso 1 1 calc R . . H27B H 0.3882 0.8933 0.4500 0.038 Uiso 1 1 calc R . . C28 C 0.40038(10) 0.97177(8) 0.40327(11) 0.0335(5) Uani 1 1 d . . . H28A H 0.3749 0.9965 0.4191 0.040 Uiso 1 1 calc R . . H28B H 0.4358 0.9972 0.4075 0.040 Uiso 1 1 calc R . . C29 C 0.36259(10) 0.95371(9) 0.32951(12) 0.0367(5) Uani 1 1 d . . . H29A H 0.3453 0.9910 0.3019 0.044 Uiso 1 1 calc R . . H29B H 0.3281 0.9270 0.3256 0.044 Uiso 1 1 calc R . . C30 C 0.40277(11) 0.91957(9) 0.30326(12) 0.0360(5) Uani 1 1 d . . . H30A H 0.3762 0.8997 0.2596 0.043 Uiso 1 1 calc R . . H30B H 0.4292 0.9496 0.2946 0.043 Uiso 1 1 calc R . . C31 C 0.59150(9) 0.71160(8) 0.52515(11) 0.0279(5) Uani 1 1 d . . . C32 C 0.64530(9) 0.75336(8) 0.55605(12) 0.0318(5) Uani 1 1 d . . . C33 C 0.67221(10) 0.77871(9) 0.51598(13) 0.0375(5) Uani 1 1 d . . . C34 C 0.72037(11) 0.82025(10) 0.54641(15) 0.0497(7) Uani 1 1 d . . . H34 H 0.7388 0.8372 0.5199 0.060 Uiso 1 1 calc R . . C35 C 0.74251(11) 0.83792(10) 0.61371(16) 0.0508(7) Uani 1 1 d . . . C36 C 0.71660(10) 0.81012(9) 0.65235(14) 0.0415(6) Uani 1 1 d . . . H36 H 0.7317 0.8208 0.6988 0.050 Uiso 1 1 calc R . . C37 C 0.66953(10) 0.76748(9) 0.62519(13) 0.0365(5) Uani 1 1 d . . . C38 C 0.65458(11) 0.75867(10) 0.44536(14) 0.0462(6) Uani 1 1 d . . . H38A H 0.6297 0.7907 0.4140 0.069 Uiso 1 1 calc R . . H38B H 0.6308 0.7205 0.4365 0.069 Uiso 1 1 calc R . . H38C H 0.6916 0.7516 0.4390 0.069 Uiso 1 1 calc R . . C39 C 0.79319(13) 0.88475(13) 0.64545(18) 0.0700(9) Uani 1 1 d . . . H39A H 0.7846 0.9108 0.6767 0.105 Uiso 1 1 calc R . . H39B H 0.7954 0.9104 0.6099 0.105 Uiso 1 1 calc R . . H39C H 0.8324 0.8635 0.6703 0.105 Uiso 1 1 calc R . . C40 C 0.64898(11) 0.73610(10) 0.67357(13) 0.0432(6) Uani 1 1 d . . . H40A H 0.6656 0.6943 0.6829 0.065 Uiso 1 1 calc R . . H40B H 0.6041 0.7344 0.6530 0.065 Uiso 1 1 calc R . . H40C H 0.6640 0.7594 0.7160 0.065 Uiso 1 1 calc R . . C41 C 0.44894(9) 0.58292(10) 0.36556(11) 0.0368(5) Uani 1 1 d . . . H41A H 0.4497 0.6213 0.3426 0.055 Uiso 1 1 calc R . . H41B H 0.4109 0.5807 0.3708 0.055 Uiso 1 1 calc R . . H41C H 0.4510 0.5479 0.3385 0.055 Uiso 1 1 calc R . . C42 C 0.55830(9) 0.58057(11) 0.42220(11) 0.0376(5) Uani 1 1 d . . . H42A H 0.5594 0.5429 0.3983 0.056 Uiso 1 1 calc R . . H42B H 0.5943 0.5820 0.4662 0.056 Uiso 1 1 calc R . . H42C H 0.5584 0.6164 0.3953 0.056 Uiso 1 1 calc R . . C43 C 0.49223(10) 0.11293(9) 0.23513(11) 0.0295(5) Uani 1 1 d . . . C44 C 0.51152(10) 0.15181(9) 0.19700(11) 0.0325(5) Uani 1 1 d . . . C45 C 0.49607(11) 0.21413(9) 0.19084(12) 0.0347(5) Uani 1 1 d . . . H45 H 0.5088 0.2402 0.1647 0.042 Uiso 1 1 calc R . . C46 C 0.46274(10) 0.23807(9) 0.22221(12) 0.0370(5) Uani 1 1 d . . . H46 H 0.4549 0.2810 0.2198 0.044 Uiso 1 1 calc R . . C47 C 0.44019(10) 0.20012(9) 0.25756(11) 0.0327(5) Uani 1 1 d . . . C48 C 0.45447(10) 0.13692(8) 0.26282(11) 0.0301(5) Uani 1 1 d . . . C49 C 0.42416(10) 0.09399(8) 0.29411(12) 0.0364(5) Uani 1 1 d . . . H49A H 0.4543 0.0626 0.3215 0.044 Uiso 1 1 calc R . . H49B H 0.3897 0.0724 0.2573 0.044 Uiso 1 1 calc R . . C50 C 0.39986(11) 0.12710(9) 0.33899(12) 0.0379(5) Uani 1 1 d . . . H50A H 0.3750 0.0982 0.3516 0.045 Uiso 1 1 calc R . . H50B H 0.4347 0.1412 0.3811 0.045 Uiso 1 1 calc R . . C51 C 0.36073(11) 0.18199(10) 0.30179(13) 0.0410(5) Uani 1 1 d . . . H51A H 0.3427 0.2011 0.3298 0.049 Uiso 1 1 calc R . . H51B H 0.3268 0.1682 0.2587 0.049 Uiso 1 1 calc R . . C52 C 0.40027(11) 0.22909(9) 0.28717(13) 0.0387(5) Uani 1 1 d . . . H52A H 0.3732 0.2602 0.2551 0.046 Uiso 1 1 calc R . . H52B H 0.4268 0.2505 0.3297 0.046 Uiso 1 1 calc R . . C53 C 0.51147(10) 0.04605(8) 0.24571(11) 0.0307(5) Uani 1 1 d . . . C54 C 0.49287(11) 0.00590(9) 0.19019(11) 0.0332(5) Uani 1 1 d . . . C55 C 0.51077(11) -0.05692(9) 0.20092(13) 0.0386(6) Uani 1 1 d . . . H55 H 0.4987 -0.0843 0.1636 0.046 Uiso 1 1 calc R . . C56 C 0.54512(11) -0.07762(9) 0.26477(12) 0.0385(5) Uani 1 1 d . . . H56 H 0.5552 -0.1201 0.2716 0.046 Uiso 1 1 calc R . . C57 C 0.56604(10) -0.03855(8) 0.32052(11) 0.0326(5) Uani 1 1 d . . . C58 C 0.54966(9) 0.02401(8) 0.31094(11) 0.0297(5) Uani 1 1 d . . . C59 C 0.57743(9) 0.06765(8) 0.36989(10) 0.0326(5) Uani 1 1 d . . . H59A H 0.5462 0.0984 0.3666 0.039 Uiso 1 1 calc R . . H59B H 0.6117 0.0899 0.3668 0.039 Uiso 1 1 calc R . . C60 C 0.60126(11) 0.03600(9) 0.43888(12) 0.0363(5) Uani 1 1 d . . . H60A H 0.6244 0.0660 0.4750 0.044 Uiso 1 1 calc R . . H60B H 0.5662 0.0211 0.4464 0.044 Uiso 1 1 calc R . . C61 C 0.64282(10) -0.01806(9) 0.44271(12) 0.0353(5) Uani 1 1 d . . . H61A H 0.6777 -0.0034 0.4346 0.042 Uiso 1 1 calc R . . H61B H 0.6594 -0.0368 0.4884 0.042 Uiso 1 1 calc R . . C62 C 0.60643(10) -0.06553(9) 0.38988(12) 0.0354(5) Uani 1 1 d . . . H62A H 0.5802 -0.0886 0.4061 0.043 Uiso 1 1 calc R . . H62B H 0.6353 -0.0951 0.3852 0.043 Uiso 1 1 calc R . . C63 C 0.59134(10) 0.10257(9) 0.17237(11) 0.0349(5) Uani 1 1 d . . . C64 C 0.64420(10) 0.10289(9) 0.24094(11) 0.0342(5) Uani 1 1 d . . . C65 C 0.66427(10) 0.15818(9) 0.27815(12) 0.0352(5) Uani 1 1 d . . . C66 C 0.70914(10) 0.15619(10) 0.34461(12) 0.0364(5) Uani 1 1 d . . . H66 H 0.7220 0.1934 0.3695 0.044 Uiso 1 1 calc R . . C67 C 0.73612(10) 0.10033(10) 0.37616(12) 0.0381(5) Uani 1 1 d . . . C68 C 0.71876(11) 0.04782(10) 0.33663(13) 0.0420(6) Uani 1 1 d . . . H68 H 0.7382 0.0102 0.3564 0.050 Uiso 1 1 calc R . . C69 C 0.67429(10) 0.04709(9) 0.26936(12) 0.0370(5) Uani 1 1 d . . . C70 C 0.64175(11) 0.22058(10) 0.24603(13) 0.0437(6) Uani 1 1 d . . . H70A H 0.6132 0.2375 0.2624 0.066 Uiso 1 1 calc R . . H70B H 0.6208 0.2161 0.1967 0.066 Uiso 1 1 calc R . . H70C H 0.6767 0.2485 0.2583 0.066 Uiso 1 1 calc R . . C71 C 0.78107(10) 0.09795(11) 0.44750(13) 0.0484(6) Uani 1 1 d . . . H71A H 0.7632 0.0764 0.4738 0.073 Uiso 1 1 calc R . . H71B H 0.7922 0.1399 0.4649 0.073 Uiso 1 1 calc R . . H71C H 0.8178 0.0760 0.4514 0.073 Uiso 1 1 calc R . . C72 C 0.66110(12) -0.01272(10) 0.23037(14) 0.0482(6) Uani 1 1 d . . . H72A H 0.6770 -0.0105 0.1964 0.072 Uiso 1 1 calc R . . H72B H 0.6167 -0.0197 0.2078 0.072 Uiso 1 1 calc R . . H72C H 0.6810 -0.0467 0.2617 0.072 Uiso 1 1 calc R . . C73 C 0.41157(12) 0.05092(10) 0.08781(12) 0.0415(5) Uani 1 1 d . . . C74 C 0.35725(12) 0.04886(13) 0.10403(13) 0.0509(6) Uani 1 1 d . . . C75 C 0.32720(13) 0.10283(14) 0.10470(15) 0.0612(7) Uani 1 1 d . . . C76 C 0.27931(14) 0.09996(18) 0.12503(17) 0.0810(10) Uani 1 1 d . . . H76 H 0.2598 0.1370 0.1278 0.097 Uiso 1 1 calc R . . C77 C 0.26001(16) 0.0454(2) 0.1409(2) 0.0902(11) Uani 1 1 d . . . C78 C 0.28784(16) -0.00686(19) 0.13651(18) 0.0848(11) Uani 1 1 d . . . H78 H 0.2741 -0.0447 0.1467 0.102 Uiso 1 1 calc R . . C79 C 0.33722(13) -0.00810(15) 0.11723(15) 0.0628(8) Uani 1 1 d . . . C80 C 0.34252(14) 0.16521(13) 0.08456(16) 0.0642(8) Uani 1 1 d . . . H80A H 0.3867 0.1678 0.0985 0.096 Uiso 1 1 calc R . . H80B H 0.3302 0.1978 0.1069 0.096 Uiso 1 1 calc R . . H80C H 0.3204 0.1702 0.0353 0.096 Uiso 1 1 calc R . . C81 C 0.20953(19) 0.0442(2) 0.1626(2) 0.1289(16) Uani 1 1 d U . . H81A H 0.2083 0.0037 0.1815 0.193 Uiso 1 1 calc R . . H81B H 0.1703 0.0522 0.1235 0.193 Uiso 1 1 calc R . . H81C H 0.2170 0.0758 0.1971 0.193 Uiso 1 1 calc R . . C82 C 0.36210(14) -0.06876(13) 0.10884(16) 0.0667(8) Uani 1 1 d . . . H82A H 0.3770 -0.0652 0.0741 0.100 Uiso 1 1 calc R . . H82B H 0.3296 -0.0998 0.0950 0.100 Uiso 1 1 calc R . . H82C H 0.3960 -0.0810 0.1519 0.100 Uiso 1 1 calc R . . C83 C 0.55452(14) 0.18514(12) 0.02454(14) 0.0531(7) Uani 1 1 d . . . H83A H 0.5546 0.2089 -0.0133 0.080 Uiso 1 1 calc R . . H83B H 0.5914 0.1595 0.0442 0.080 Uiso 1 1 calc R . . H83C H 0.5540 0.2133 0.0591 0.080 Uiso 1 1 calc R . . C84 C 0.55582(16) -0.03110(12) 0.02773(14) 0.0613(9) Uani 1 1 d . . . H84A H 0.5558 -0.0566 0.0645 0.092 Uiso 1 1 calc R . . H84B H 0.5923 -0.0049 0.0452 0.092 Uiso 1 1 calc R . . H84C H 0.5562 -0.0576 -0.0082 0.092 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 0.0323(3) 0.0167(2) 0.0418(4) 0.000 0.0209(3) 0.000 V2 0.0333(3) 0.0174(2) 0.0436(4) 0.000 0.0238(3) 0.000 V3 0.0576(2) 0.03843(18) 0.0288(2) -0.00146(19) 0.0244(2) -0.0039(2) N1 0.0349(9) 0.0165(7) 0.0344(11) -0.0014(7) 0.0207(9) -0.0007(6) N2 0.0356(9) 0.0172(7) 0.0406(12) 0.0001(7) 0.0264(9) -0.0005(6) N3 0.0380(8) 0.0223(7) 0.0364(10) -0.0030(8) 0.0231(8) -0.0023(8) N4 0.0499(11) 0.0269(8) 0.0318(11) 0.0020(7) 0.0237(10) -0.0024(7) N5 0.0580(12) 0.0288(9) 0.0344(12) -0.0023(8) 0.0257(11) -0.0065(8) N6 0.0642(19) 0.0391(14) 0.0227(17) 0.000 0.0219(15) 0.000 N7 0.072(2) 0.0366(15) 0.040(2) 0.000 0.0328(17) 0.000 O1 0.0326(8) 0.0212(7) 0.0456(10) -0.0031(6) 0.0201(8) 0.0009(5) O2 0.0345(8) 0.0213(7) 0.0501(11) 0.0052(6) 0.0240(8) 0.0019(6) O3 0.0545(9) 0.0447(9) 0.0329(9) -0.0018(7) 0.0274(8) -0.0008(7) O4 0.0560(9) 0.0570(9) 0.0310(9) 0.0028(9) 0.0192(8) -0.0031(9) C1 0.0401(11) 0.0173(8) 0.0360(14) -0.0033(8) 0.0241(11) -0.0027(8) C2 0.0359(11) 0.0183(8) 0.0381(14) 0.0010(8) 0.0222(11) -0.0014(8) C3 0.0409(12) 0.0235(9) 0.0326(14) 0.0014(8) 0.0220(11) -0.0002(8) C4 0.0443(12) 0.0267(9) 0.0356(14) -0.0005(9) 0.0254(11) -0.0033(9) C5 0.0449(12) 0.0203(8) 0.0401(14) -0.0053(9) 0.0286(11) -0.0028(8) C6 0.0407(12) 0.0199(8) 0.0378(14) 0.0004(8) 0.0252(11) -0.0005(8) C7 0.0493(13) 0.0230(9) 0.0454(16) 0.0034(9) 0.0317(13) 0.0062(9) C8 0.0560(14) 0.0252(9) 0.0527(16) 0.0019(10) 0.0370(13) 0.0058(9) C9 0.0505(13) 0.0313(10) 0.0496(16) 0.0029(10) 0.0339(13) 0.0071(9) C10 0.0538(14) 0.0246(9) 0.0554(17) 0.0011(10) 0.0386(14) 0.0057(9) C11 0.0358(11) 0.0194(8) 0.0391(14) 0.0011(8) 0.0191(11) -0.0025(8) C12 0.0355(12) 0.0214(9) 0.0507(16) 0.0021(9) 0.0205(12) -0.0022(8) C13 0.0375(12) 0.0295(10) 0.0480(17) 0.0003(10) 0.0174(12) -0.0011(9) C14 0.0461(14) 0.0458(13) 0.0506(18) -0.0098(12) 0.0163(14) -0.0093(11) C15 0.0501(15) 0.0443(13) 0.069(2) -0.0059(13) 0.0246(16) -0.0153(11) C16 0.0430(14) 0.0462(13) 0.064(2) 0.0000(13) 0.0255(14) -0.0132(11) C17 0.0400(12) 0.0292(10) 0.0525(17) 0.0048(10) 0.0225(13) -0.0042(9) C18 0.0525(15) 0.0566(15) 0.0524(19) -0.0038(13) 0.0262(14) -0.0079(12) C19 0.074(2) 0.082(2) 0.099(3) -0.016(2) 0.038(2) -0.0394(18) C20 0.0469(14) 0.0478(13) 0.0527(18) 0.0028(12) 0.0284(14) -0.0089(11) C21 0.0356(11) 0.0139(8) 0.0341(13) -0.0002(8) 0.0196(10) -0.0038(7) C22 0.0370(11) 0.0178(8) 0.0382(14) -0.0005(8) 0.0238(11) -0.0053(8) C23 0.0444(12) 0.0240(9) 0.0362(15) -0.0053(9) 0.0261(12) -0.0033(9) C24 0.0471(13) 0.0278(9) 0.0306(13) -0.0024(9) 0.0223(11) -0.0070(9) C25 0.0427(12) 0.0206(8) 0.0350(14) -0.0009(8) 0.0199(11) -0.0042(8) C26 0.0331(10) 0.0212(8) 0.0336(13) -0.0003(8) 0.0174(10) -0.0026(8) C27 0.0391(11) 0.0240(9) 0.0357(14) 0.0043(9) 0.0203(11) 0.0023(8) C28 0.0451(12) 0.0236(9) 0.0352(14) 0.0030(9) 0.0207(11) 0.0036(8) C29 0.0444(13) 0.0287(10) 0.0370(15) 0.0057(9) 0.0178(12) 0.0010(9) C30 0.0481(13) 0.0300(10) 0.0310(14) 0.0018(9) 0.0183(12) -0.0017(9) C31 0.0323(11) 0.0198(8) 0.0401(14) 0.0014(8) 0.0236(11) 0.0011(8) C32 0.0317(11) 0.0199(9) 0.0481(16) -0.0036(9) 0.0214(11) -0.0026(8) C33 0.0346(11) 0.0280(10) 0.0575(17) -0.0035(10) 0.0271(12) -0.0033(9) C34 0.0479(14) 0.0356(11) 0.082(2) -0.0142(12) 0.0436(16) -0.0136(10) C35 0.0458(14) 0.0353(12) 0.079(2) -0.0191(12) 0.0351(15) -0.0105(10) C36 0.0379(12) 0.0308(10) 0.0561(18) -0.0091(10) 0.0209(13) 0.0009(9) C37 0.0353(12) 0.0274(10) 0.0498(16) -0.0006(10) 0.0212(12) 0.0064(9) C38 0.0513(14) 0.0349(11) 0.073(2) -0.0061(11) 0.0463(15) -0.0080(10) C39 0.0633(18) 0.0623(17) 0.099(3) -0.0411(17) 0.0488(19) -0.0342(14) C40 0.0472(14) 0.0344(11) 0.0513(17) 0.0001(11) 0.0246(13) 0.0030(10) C41 0.0479(12) 0.0242(8) 0.0449(14) -0.0007(11) 0.0263(11) -0.0036(10) C42 0.0413(11) 0.0293(9) 0.0541(14) -0.0025(12) 0.0319(11) 0.0011(10) C43 0.0426(12) 0.0243(9) 0.0219(13) 0.0002(8) 0.0143(10) -0.0013(8) C44 0.0458(12) 0.0262(9) 0.0290(14) -0.0005(9) 0.0195(11) -0.0042(9) C45 0.0493(13) 0.0244(10) 0.0326(15) 0.0045(9) 0.0200(12) -0.0008(9) C46 0.0525(14) 0.0210(9) 0.0411(15) 0.0049(9) 0.0238(12) 0.0019(9) C47 0.0441(12) 0.0261(9) 0.0280(13) 0.0004(8) 0.0159(11) 0.0025(8) C48 0.0401(11) 0.0230(9) 0.0302(13) -0.0007(8) 0.0183(11) 0.0000(8) C49 0.0501(12) 0.0254(11) 0.0458(15) 0.0000(9) 0.0322(12) -0.0011(8) C50 0.0523(13) 0.0280(9) 0.0441(15) -0.0014(10) 0.0310(12) -0.0013(9) C51 0.0460(13) 0.0383(11) 0.0440(16) -0.0005(10) 0.0246(13) 0.0036(10) C52 0.0513(14) 0.0249(10) 0.0435(16) 0.0013(9) 0.0241(13) 0.0042(9) C53 0.0453(12) 0.0224(9) 0.0324(14) 0.0008(9) 0.0245(11) -0.0031(8) C54 0.0503(13) 0.0285(10) 0.0254(13) -0.0025(9) 0.0208(11) -0.0053(9) C55 0.0620(15) 0.0253(10) 0.0375(16) -0.0064(10) 0.0300(13) -0.0065(10) C56 0.0565(14) 0.0228(9) 0.0470(16) -0.0007(10) 0.0326(13) -0.0009(9) C57 0.0442(12) 0.0242(9) 0.0371(14) 0.0028(9) 0.0249(11) 0.0027(8) C58 0.0425(11) 0.0233(9) 0.0320(13) -0.0007(8) 0.0243(11) -0.0018(8) C59 0.0445(11) 0.0217(10) 0.0381(13) 0.0012(8) 0.0239(11) 0.0006(8) C60 0.0523(13) 0.0257(9) 0.0353(14) -0.0004(9) 0.0233(12) -0.0011(9) C61 0.0433(12) 0.0291(10) 0.0341(14) 0.0031(9) 0.0175(11) 0.0014(9) C62 0.0471(13) 0.0228(9) 0.0432(15) 0.0022(9) 0.0260(12) 0.0026(9) C63 0.0487(13) 0.0306(9) 0.0340(14) 0.0036(9) 0.0259(12) -0.0029(9) C64 0.0425(12) 0.0335(10) 0.0308(14) 0.0020(9) 0.0199(11) 0.0002(9) C65 0.0399(12) 0.0309(10) 0.0418(15) 0.0017(10) 0.0243(12) -0.0039(9) C66 0.0352(11) 0.0339(10) 0.0430(16) 0.0021(10) 0.0198(12) -0.0031(9) C67 0.0340(11) 0.0449(12) 0.0382(15) 0.0084(10) 0.0183(11) -0.0021(9) C68 0.0434(13) 0.0334(11) 0.0593(19) 0.0052(11) 0.0319(14) 0.0036(9) C69 0.0417(13) 0.0359(11) 0.0397(16) 0.0037(10) 0.0238(12) 0.0011(9) C70 0.0524(14) 0.0335(11) 0.0426(16) 0.0048(10) 0.0185(13) -0.0036(10) C71 0.0383(12) 0.0528(15) 0.0507(17) 0.0067(12) 0.0163(13) -0.0045(10) C72 0.0609(16) 0.0359(12) 0.0519(18) -0.0018(11) 0.0286(14) 0.0028(11) C73 0.0545(14) 0.0412(12) 0.0284(14) -0.0051(10) 0.0178(12) -0.0107(11) C74 0.0487(15) 0.0712(17) 0.0353(16) -0.0028(13) 0.0206(13) -0.0099(13) C75 0.0559(16) 0.0803(19) 0.0470(18) -0.0078(14) 0.0220(15) -0.0058(14) C76 0.0610(18) 0.112(3) 0.074(2) -0.006(2) 0.0337(18) 0.0043(18) C77 0.068(2) 0.116(3) 0.103(3) 0.005(2) 0.052(2) -0.008(2) C78 0.072(2) 0.115(3) 0.075(3) 0.002(2) 0.039(2) -0.034(2) C79 0.0565(17) 0.088(2) 0.0409(18) -0.0021(15) 0.0188(15) -0.0239(15) C80 0.0616(18) 0.0677(18) 0.060(2) -0.0072(15) 0.0239(17) 0.0032(14) C81 0.101(2) 0.153(3) 0.153(3) 0.013(2) 0.074(2) -0.005(2) C82 0.078(2) 0.0653(18) 0.056(2) -0.0038(15) 0.0277(17) -0.0316(16) C83 0.083(2) 0.0436(14) 0.0399(18) -0.0005(12) 0.0332(17) -0.0121(13) C84 0.114(3) 0.0418(14) 0.0407(19) 0.0077(12) 0.0453(19) 0.0208(15) _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 N3 2.0640(17) . ? V1 N3 2.0640(17) 2_656 ? V1 O1 2.0782(15) 2_656 ? V1 O1 2.0782(15) . ? V1 N1 2.0897(16) . ? V1 N1 2.0897(16) 2_656 ? V1 C11 2.489(2) 2_656 ? V1 C11 2.489(2) . ? V1 V2 2.8573(7) . ? V2 O2 2.0573(15) . ? V2 O2 2.0573(15) 2_656 ? V2 N3 2.0788(16) . ? V2 N3 2.0788(17) 2_656 ? V2 N2 2.1126(14) . ? V2 N2 2.1126(14) 2_656 ? V2 C31 2.4722(19) . ? V2 C31 2.4722(19) 2_656 ? V3 O3 2.0635(16) . ? V3 N6 2.076(2) . ? V3 O4 2.0818(16) . ? V3 N7 2.082(2) . ? V3 N4 2.0965(18) . ? V3 N5 2.0977(17) . ? V3 C63 2.472(2) . ? V3 C73 2.477(2) . ? V3 V3 2.8804(9) 2_655 ? N1 C11 1.322(2) . ? N1 C2 1.402(2) . ? N2 C31 1.306(3) . ? N2 C22 1.418(2) . ? N3 C41 1.469(3) . ? N3 C42 1.486(2) . ? N4 C63 1.311(3) . ? N4 C44 1.416(2) . ? N5 C73 1.295(3) . ? N5 C54 1.418(3) . ? N6 C83 1.465(3) . ? N6 C83 1.465(3) 2_655 ? N6 V3 2.076(2) 2_655 ? N7 C84 1.485(3) . ? N7 C84 1.485(3) 2_655 ? N7 V3 2.082(2) 2_655 ? O1 C11 1.299(2) . ? O2 C31 1.304(2) . ? O3 C63 1.292(2) . ? O4 C73 1.301(3) . ? C1 C2 1.409(3) . ? C1 C6 1.426(2) . ? C1 C1 1.507(4) 2_656 ? C2 C3 1.406(3) . ? C3 C4 1.380(3) . ? C3 H3 0.9500 . ? C4 C5 1.393(3) . ? C4 H4 0.9500 . ? C5 C6 1.409(3) . ? C5 C10 1.516(3) . ? C6 C7 1.506(3) . ? C7 C8 1.531(2) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.526(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 C10 1.515(3) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.487(3) . ? C12 C13 1.394(3) . ? C12 C17 1.415(3) . ? C13 C14 1.398(3) . ? C13 C18 1.515(3) . ? C14 C15 1.369(3) . ? C14 H14 0.9500 . ? C15 C16 1.379(4) . ? C15 C19 1.515(4) . ? C16 C17 1.408(3) . ? C16 H16 0.9500 . ? C17 C20 1.481(3) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 C22 1.395(2) . ? C21 C26 1.425(3) . ? C21 C21 1.500(4) 2_656 ? C22 C23 1.395(3) . ? C23 C24 1.376(3) . ? C23 H23 0.9500 . ? C24 C25 1.405(3) . ? C24 H24 0.9500 . ? C25 C26 1.378(3) . ? C25 C30 1.521(3) . ? C26 C27 1.522(2) . ? C27 C28 1.532(3) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C28 C29 1.523(3) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 C30 1.525(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.488(3) . ? C32 C37 1.402(3) . ? C32 C33 1.417(3) . ? C33 C34 1.394(3) . ? C33 C38 1.483(3) . ? C34 C35 1.388(4) . ? C34 H34 0.9500 . ? C35 C36 1.396(3) . ? C35 C39 1.511(3) . ? C36 C37 1.387(3) . ? C36 H36 0.9500 . ? C37 C40 1.519(3) . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C48 1.403(3) . ? C43 C44 1.407(3) . ? C43 C53 1.514(2) . ? C44 C45 1.397(3) . ? C45 C46 1.373(3) . ? C45 H45 0.9500 . ? C46 C47 1.398(3) . ? C46 H46 0.9500 . ? C47 C48 1.410(3) . ? C47 C52 1.519(3) . ? C48 C49 1.525(2) . ? C49 C50 1.532(3) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.521(3) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.530(3) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54 1.404(3) . ? C53 C58 1.407(3) . ? C54 C55 1.422(3) . ? C55 C56 1.357(3) . ? C55 H55 0.9500 . ? C56 C57 1.391(3) . ? C56 H56 0.9500 . ? C57 C58 1.407(2) . ? C57 C62 1.523(3) . ? C58 C59 1.506(3) . ? C59 C60 1.529(3) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 C61 1.527(3) . ? C60 H60A 0.9900 . ? C60 H60B 0.9900 . ? C61 C62 1.515(3) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.491(3) . ? C64 C69 1.413(3) . ? C64 C65 1.415(3) . ? C65 C66 1.388(3) . ? C65 C70 1.517(3) . ? C66 C67 1.410(3) . ? C66 H66 0.9500 . ? C67 C68 1.384(3) . ? C67 C71 1.467(3) . ? C68 C69 1.397(3) . ? C68 H68 0.9500 . ? C69 C72 1.513(3) . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 H72A 0.9800 . ? C72 H72B 0.9800 . ? C72 H72C 0.9800 . ? C73 C74 1.508(3) . ? C74 C75 1.385(4) . ? C74 C79 1.406(4) . ? C75 C76 1.416(4) . ? C75 C80 1.523(4) . ? C76 C77 1.375(5) . ? C76 H76 0.9500 . ? C77 C78 1.347(5) . ? C77 C81 1.496(5) . ? C78 C79 1.435(4) . ? C78 H78 0.9500 . ? C79 C82 1.495(4) . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 H82A 0.9800 . ? C82 H82B 0.9800 . ? C82 H82C 0.9800 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 V1 N3 93.22(9) . 2_656 ? N3 V1 O1 94.41(6) . 2_656 ? N3 V1 O1 95.64(6) 2_656 2_656 ? N3 V1 O1 95.64(6) . . ? N3 V1 O1 94.41(6) 2_656 . ? O1 V1 O1 165.36(7) 2_656 . ? N3 V1 N1 97.42(6) . . ? N3 V1 N1 156.02(6) 2_656 . ? O1 V1 N1 104.85(6) 2_656 . ? O1 V1 N1 63.27(5) . . ? N3 V1 N1 156.02(6) . 2_656 ? N3 V1 N1 97.42(6) 2_656 2_656 ? O1 V1 N1 63.27(5) 2_656 2_656 ? O1 V1 N1 104.85(6) . 2_656 ? N1 V1 N1 81.24(9) . 2_656 ? N3 V1 C11 124.66(6) . 2_656 ? N3 V1 C11 100.48(7) 2_656 2_656 ? O1 V1 C11 31.43(5) 2_656 2_656 ? O1 V1 C11 135.57(6) . 2_656 ? N1 V1 C11 91.03(7) . 2_656 ? N1 V1 C11 32.07(6) 2_656 2_656 ? N3 V1 C11 100.48(7) . . ? N3 V1 C11 124.66(6) 2_656 . ? O1 V1 C11 135.57(6) 2_656 . ? O1 V1 C11 31.43(5) . . ? N1 V1 C11 32.07(6) . . ? N1 V1 C11 91.03(7) 2_656 . ? C11 V1 C11 113.77(9) 2_656 . ? N3 V1 V2 46.61(5) . . ? N3 V1 V2 46.61(5) 2_656 . ? O1 V1 V2 97.32(4) 2_656 . ? O1 V1 V2 97.32(4) . . ? N1 V1 V2 139.38(5) . . ? N1 V1 V2 139.38(5) 2_656 . ? C11 V1 V2 123.11(4) 2_656 . ? C11 V1 V2 123.11(4) . . ? O2 V2 O2 165.16(7) . 2_656 ? O2 V2 N3 98.71(6) . . ? O2 V2 N3 91.57(6) 2_656 . ? O2 V2 N3 91.57(6) . 2_656 ? O2 V2 N3 98.71(6) 2_656 2_656 ? N3 V2 N3 92.36(9) . 2_656 ? O2 V2 N2 63.16(6) . . ? O2 V2 N2 104.82(6) 2_656 . ? N3 V2 N2 98.88(6) . . ? N3 V2 N2 153.52(7) 2_656 . ? O2 V2 N2 104.82(6) . 2_656 ? O2 V2 N2 63.16(6) 2_656 2_656 ? N3 V2 N2 153.52(7) . 2_656 ? N3 V2 N2 98.88(6) 2_656 2_656 ? N2 V2 N2 81.46(8) . 2_656 ? O2 V2 C31 31.83(6) . . ? O2 V2 C31 134.72(6) 2_656 . ? N3 V2 C31 104.75(6) . . ? N3 V2 C31 121.90(7) 2_656 . ? N2 V2 C31 31.88(7) . . ? N2 V2 C31 89.55(6) 2_656 . ? O2 V2 C31 134.72(6) . 2_656 ? O2 V2 C31 31.83(6) 2_656 2_656 ? N3 V2 C31 121.90(7) . 2_656 ? N3 V2 C31 104.75(6) 2_656 2_656 ? N2 V2 C31 89.55(6) . 2_656 ? N2 V2 C31 31.88(7) 2_656 2_656 ? C31 V2 C31 111.13(8) . 2_656 ? O2 V2 V1 97.42(4) . . ? O2 V2 V1 97.42(4) 2_656 . ? N3 V2 V1 46.18(5) . . ? N3 V2 V1 46.18(5) 2_656 . ? N2 V2 V1 139.27(4) . . ? N2 V2 V1 139.27(4) 2_656 . ? C31 V2 V1 124.44(4) . . ? C31 V2 V1 124.44(4) 2_656 . ? O3 V3 N6 97.69(4) . . ? O3 V3 O4 164.03(6) . . ? N6 V3 O4 93.81(5) . . ? O3 V3 N7 93.43(4) . . ? N6 V3 N7 92.30(7) . . ? O4 V3 N7 97.15(5) . . ? O3 V3 N4 63.00(6) . . ? N6 V3 N4 97.90(7) . . ? O4 V3 N4 104.51(7) . . ? N7 V3 N4 155.29(6) . . ? O3 V3 N5 103.82(7) . . ? N6 V3 N5 155.07(6) . . ? O4 V3 N5 62.79(7) . . ? N7 V3 N5 98.77(7) . . ? N4 V3 N5 81.13(7) . . ? O3 V3 C63 31.48(6) . . ? N6 V3 C63 103.33(5) . . ? O4 V3 C63 134.35(6) . . ? N7 V3 C63 123.55(5) . . ? N4 V3 C63 32.02(6) . . ? N5 V3 C63 89.08(7) . . ? O3 V3 C73 133.66(7) . . ? N6 V3 C73 124.02(6) . . ? O4 V3 C73 31.67(7) . . ? N7 V3 C73 103.12(6) . . ? N4 V3 C73 89.72(7) . . ? N5 V3 C73 31.53(7) . . ? C63 V3 C73 110.99(7) . . ? O3 V3 V3 98.04(4) . 2_655 ? N6 V3 V3 46.07(5) . 2_655 ? O4 V3 V3 97.92(4) . 2_655 ? N7 V3 V3 46.23(5) . 2_655 ? N4 V3 V3 138.94(4) . 2_655 ? N5 V3 V3 139.93(5) . 2_655 ? C63 V3 V3 124.40(5) . 2_655 ? C73 V3 V3 124.61(6) . 2_655 ? C11 N1 C2 129.97(15) . . ? C11 N1 V1 90.84(11) . . ? C2 N1 V1 132.51(14) . . ? C31 N2 C22 130.06(16) . . ? C31 N2 V2 89.42(11) . . ? C22 N2 V2 131.52(12) . . ? C41 N3 C42 107.76(14) . . ? C41 N3 V1 117.02(12) . . ? C42 N3 V1 114.48(13) . . ? C41 N3 V2 114.52(12) . . ? C42 N3 V2 115.03(13) . . ? V1 N3 V2 87.21(6) . . ? C63 N4 C44 129.9(2) . . ? C63 N4 V3 89.99(13) . . ? C44 N4 V3 131.58(15) . . ? C73 N5 C54 129.50(18) . . ? C73 N5 V3 90.61(14) . . ? C54 N5 V3 131.34(15) . . ? C83 N6 C83 108.6(3) . 2_655 ? C83 N6 V3 114.04(11) . 2_655 ? C83 N6 V3 115.68(11) 2_655 2_655 ? C83 N6 V3 115.68(11) . . ? C83 N6 V3 114.04(11) 2_655 . ? V3 N6 V3 87.87(10) 2_655 . ? C84 N7 C84 110.2(3) . 2_655 ? C84 N7 V3 113.55(12) . . ? C84 N7 V3 115.26(11) 2_655 . ? C84 N7 V3 115.26(11) . 2_655 ? C84 N7 V3 113.55(12) 2_655 2_655 ? V3 N7 V3 87.53(10) . 2_655 ? C11 O1 V1 92.01(11) . . ? C31 O2 V2 91.89(12) . . ? C63 O3 V3 92.00(13) . . ? C73 O4 V3 91.17(14) . . ? C2 C1 C6 118.86(17) . . ? C2 C1 C1 121.39(15) . 2_656 ? C6 C1 C1 119.72(17) . 2_656 ? N1 C2 C3 117.68(17) . . ? N1 C2 C1 121.41(17) . . ? C3 C2 C1 120.21(17) . . ? C4 C3 C2 120.13(19) . . ? C4 C3 H3 119.9 . . ? C2 C3 H3 119.9 . . ? C3 C4 C5 121.05(18) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C4 C5 C6 119.81(17) . . ? C4 C5 C10 118.09(17) . . ? C6 C5 C10 122.09(18) . . ? C5 C6 C1 119.65(18) . . ? C5 C6 C7 119.69(16) . . ? C1 C6 C7 120.50(17) . . ? C6 C7 C8 113.95(18) . . ? C6 C7 H7A 108.8 . . ? C8 C7 H7A 108.8 . . ? C6 C7 H7B 108.8 . . ? C8 C7 H7B 108.8 . . ? H7A C7 H7B 107.7 . . ? C9 C8 C7 109.70(16) . . ? C9 C8 H8A 109.7 . . ? C7 C8 H8A 109.7 . . ? C9 C8 H8B 109.7 . . ? C7 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C10 C9 C8 109.54(18) . . ? C10 C9 H9A 109.8 . . ? C8 C9 H9A 109.8 . . ? C10 C9 H9B 109.8 . . ? C8 C9 H9B 109.8 . . ? H9A C9 H9B 108.2 . . ? C9 C10 C5 113.74(18) . . ? C9 C10 H10A 108.8 . . ? C5 C10 H10A 108.8 . . ? C9 C10 H10B 108.8 . . ? C5 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? O1 C11 N1 113.10(17) . . ? O1 C11 C12 119.79(17) . . ? N1 C11 C12 127.08(17) . . ? O1 C11 V1 56.56(10) . . ? N1 C11 V1 57.09(10) . . ? C12 C11 V1 170.62(15) . . ? C13 C12 C17 120.5(2) . . ? C13 C12 C11 121.11(18) . . ? C17 C12 C11 118.3(2) . . ? C12 C13 C14 118.8(2) . . ? C12 C13 C18 124.3(2) . . ? C14 C13 C18 116.7(2) . . ? C15 C14 C13 122.4(3) . . ? C15 C14 H14 118.8 . . ? C13 C14 H14 118.8 . . ? C14 C15 C16 118.1(2) . . ? C14 C15 C19 120.6(3) . . ? C16 C15 C19 121.3(2) . . ? C15 C16 C17 122.8(2) . . ? C15 C16 H16 118.6 . . ? C17 C16 H16 118.6 . . ? C16 C17 C12 117.2(2) . . ? C16 C17 C20 119.3(2) . . ? C12 C17 C20 123.5(2) . . ? C13 C18 H18A 109.5 . . ? C13 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C13 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C15 C19 H19A 109.5 . . ? C15 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C15 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C17 C20 H20A 109.5 . . ? C17 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C17 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C22 C21 C26 118.48(19) . . ? C22 C21 C21 121.51(17) . 2_656 ? C26 C21 C21 119.97(15) . 2_656 ? C23 C22 C21 120.23(19) . . ? C23 C22 N2 117.40(17) . . ? C21 C22 N2 121.50(18) . . ? C24 C23 C22 120.28(18) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C25 120.9(2) . . ? C23 C24 H24 119.6 . . ? C25 C24 H24 119.6 . . ? C26 C25 C24 119.02(19) . . ? C26 C25 C30 123.17(17) . . ? C24 C25 C30 117.81(19) . . ? C25 C26 C21 120.89(17) . . ? C25 C26 C27 120.15(18) . . ? C21 C26 C27 118.86(18) . . ? C26 C27 C28 112.86(16) . . ? C26 C27 H27A 109.0 . . ? C28 C27 H27A 109.0 . . ? C26 C27 H27B 109.0 . . ? C28 C27 H27B 109.0 . . ? H27A C27 H27B 107.8 . . ? C29 C28 C27 109.90(17) . . ? C29 C28 H28A 109.7 . . ? C27 C28 H28A 109.7 . . ? C29 C28 H28B 109.7 . . ? C27 C28 H28B 109.7 . . ? H28A C28 H28B 108.2 . . ? C28 C29 C30 109.94(18) . . ? C28 C29 H29A 109.7 . . ? C30 C29 H29A 109.7 . . ? C28 C29 H29B 109.7 . . ? C30 C29 H29B 109.7 . . ? H29A C29 H29B 108.2 . . ? C25 C30 C29 113.07(18) . . ? C25 C30 H30A 109.0 . . ? C29 C30 H30A 109.0 . . ? C25 C30 H30B 109.0 . . ? C29 C30 H30B 109.0 . . ? H30A C30 H30B 107.8 . . ? O2 C31 N2 113.60(17) . . ? O2 C31 C32 118.35(19) . . ? N2 C31 C32 128.01(17) . . ? O2 C31 V2 56.28(9) . . ? N2 C31 V2 58.70(9) . . ? C32 C31 V2 165.84(15) . . ? C37 C32 C33 119.94(19) . . ? C37 C32 C31 119.75(18) . . ? C33 C32 C31 120.3(2) . . ? C34 C33 C32 118.1(2) . . ? C34 C33 C38 119.32(19) . . ? C32 C33 C38 122.34(18) . . ? C35 C34 C33 122.9(2) . . ? C35 C34 H34 118.6 . . ? C33 C34 H34 118.6 . . ? C34 C35 C36 117.4(2) . . ? C34 C35 C39 122.4(2) . . ? C36 C35 C39 120.2(3) . . ? C37 C36 C35 122.2(2) . . ? C37 C36 H36 118.9 . . ? C35 C36 H36 118.9 . . ? C36 C37 C32 119.2(2) . . ? C36 C37 C40 117.4(2) . . ? C32 C37 C40 123.32(19) . . ? C33 C38 H38A 109.5 . . ? C33 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C33 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C35 C39 H39A 109.5 . . ? C35 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C35 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? N3 C41 H41A 109.5 . . ? N3 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N3 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N3 C42 H42A 109.5 . . ? N3 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N3 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C48 C43 C44 119.01(17) . . ? C48 C43 C53 120.44(17) . . ? C44 C43 C53 120.55(18) . . ? C45 C44 C43 119.73(18) . . ? C45 C44 N4 117.36(17) . . ? C43 C44 N4 122.16(17) . . ? C46 C45 C44 120.73(18) . . ? C46 C45 H45 119.6 . . ? C44 C45 H45 119.6 . . ? C45 C46 C47 120.93(18) . . ? C45 C46 H46 119.5 . . ? C47 C46 H46 119.5 . . ? C46 C47 C48 118.63(18) . . ? C46 C47 C52 118.06(17) . . ? C48 C47 C52 123.29(17) . . ? C43 C48 C47 120.70(17) . . ? C43 C48 C49 120.16(15) . . ? C47 C48 C49 118.96(16) . . ? C48 C49 C50 113.53(15) . . ? C48 C49 H49A 108.9 . . ? C50 C49 H49A 108.9 . . ? C48 C49 H49B 108.9 . . ? C50 C49 H49B 108.9 . . ? H49A C49 H49B 107.7 . . ? C51 C50 C49 110.40(18) . . ? C51 C50 H50A 109.6 . . ? C49 C50 H50A 109.6 . . ? C51 C50 H50B 109.6 . . ? C49 C50 H50B 109.6 . . ? H50A C50 H50B 108.1 . . ? C50 C51 C52 109.70(18) . . ? C50 C51 H51A 109.7 . . ? C52 C51 H51A 109.7 . . ? C50 C51 H51B 109.7 . . ? C52 C51 H51B 109.7 . . ? H51A C51 H51B 108.2 . . ? C47 C52 C51 112.80(17) . . ? C47 C52 H52A 109.0 . . ? C51 C52 H52A 109.0 . . ? C47 C52 H52B 109.0 . . ? C51 C52 H52B 109.0 . . ? H52A C52 H52B 107.8 . . ? C54 C53 C58 119.38(18) . . ? C54 C53 C43 120.2(2) . . ? C58 C53 C43 120.34(19) . . ? C53 C54 N5 122.69(18) . . ? C53 C54 C55 119.7(2) . . ? N5 C54 C55 116.85(19) . . ? C56 C55 C54 119.7(2) . . ? C56 C55 H55 120.2 . . ? C54 C55 H55 120.2 . . ? C55 C56 C57 121.99(19) . . ? C55 C56 H56 119.0 . . ? C57 C56 H56 119.0 . . ? C56 C57 C58 119.2(2) . . ? C56 C57 C62 118.21(17) . . ? C58 C57 C62 122.55(19) . . ? C57 C58 C53 119.93(19) . . ? C57 C58 C59 119.34(19) . . ? C53 C58 C59 120.55(16) . . ? C58 C59 C60 113.66(15) . . ? C58 C59 H59A 108.8 . . ? C60 C59 H59A 108.8 . . ? C58 C59 H59B 108.8 . . ? C60 C59 H59B 108.8 . . ? H59A C59 H59B 107.7 . . ? C61 C60 C59 110.83(17) . . ? C61 C60 H60A 109.5 . . ? C59 C60 H60A 109.5 . . ? C61 C60 H60B 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 108.1 . . ? C62 C61 C60 109.47(18) . . ? C62 C61 H61A 109.8 . . ? C60 C61 H61A 109.8 . . ? C62 C61 H61B 109.8 . . ? C60 C61 H61B 109.8 . . ? H61A C61 H61B 108.2 . . ? C61 C62 C57 114.07(16) . . ? C61 C62 H62A 108.7 . . ? C57 C62 H62A 108.7 . . ? C61 C62 H62B 108.7 . . ? C57 C62 H62B 108.7 . . ? H62A C62 H62B 107.6 . . ? O3 C63 N4 113.3(2) . . ? O3 C63 C64 120.48(19) . . ? N4 C63 C64 126.17(18) . . ? O3 C63 V3 56.52(11) . . ? N4 C63 V3 57.99(12) . . ? C64 C63 V3 166.55(14) . . ? C69 C64 C65 119.6(2) . . ? C69 C64 C63 119.46(18) . . ? C65 C64 C63 120.93(19) . . ? C66 C65 C64 119.62(19) . . ? C66 C65 C70 118.30(19) . . ? C64 C65 C70 121.9(2) . . ? C65 C66 C67 121.7(2) . . ? C65 C66 H66 119.2 . . ? C67 C66 H66 119.2 . . ? C68 C67 C66 117.0(2) . . ? C68 C67 C71 121.4(2) . . ? C66 C67 C71 121.6(2) . . ? C67 C68 C69 123.7(2) . . ? C67 C68 H68 118.1 . . ? C69 C68 H68 118.1 . . ? C68 C69 C64 117.9(2) . . ? C68 C69 C72 118.9(2) . . ? C64 C69 C72 123.2(2) . . ? C65 C70 H70A 109.5 . . ? C65 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C65 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C67 C71 H71A 109.5 . . ? C67 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C67 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C69 C72 H72A 109.5 . . ? C69 C72 H72B 109.5 . . ? H72A C72 H72B 109.5 . . ? C69 C72 H72C 109.5 . . ? H72A C72 H72C 109.5 . . ? H72B C72 H72C 109.5 . . ? N5 C73 O4 114.0(2) . . ? N5 C73 C74 127.4(2) . . ? O4 C73 C74 118.6(2) . . ? N5 C73 V3 57.86(11) . . ? O4 C73 V3 57.17(11) . . ? C74 C73 V3 168.27(17) . . ? C75 C74 C79 120.9(2) . . ? C75 C74 C73 119.7(2) . . ? C79 C74 C73 119.4(2) . . ? C74 C75 C76 118.3(3) . . ? C74 C75 C80 123.8(2) . . ? C76 C75 C80 118.0(3) . . ? C77 C76 C75 122.3(3) . . ? C77 C76 H76 118.8 . . ? C75 C76 H76 118.8 . . ? C78 C77 C76 118.3(3) . . ? C78 C77 C81 120.8(4) . . ? C76 C77 C81 120.9(4) . . ? C77 C78 C79 123.1(3) . . ? C77 C78 H78 118.5 . . ? C79 C78 H78 118.5 . . ? C74 C79 C78 116.9(3) . . ? C74 C79 C82 123.9(2) . . ? C78 C79 C82 119.1(3) . . ? C75 C80 H80A 109.5 . . ? C75 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C75 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C77 C81 H81A 109.5 . . ? C77 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C77 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C79 C82 H82A 109.5 . . ? C79 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C79 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? N6 C83 H83A 109.5 . . ? N6 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? N6 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? N7 C84 H84A 109.5 . . ? N7 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? N7 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 V1 V2 O2 -94.98(7) . . . . ? N3 V1 V2 O2 85.02(7) 2_656 . . . ? O1 V1 V2 O2 -5.83(6) 2_656 . . . ? O1 V1 V2 O2 174.17(6) . . . . ? N1 V1 V2 O2 -128.97(7) . . . . ? N1 V1 V2 O2 51.03(7) 2_656 . . . ? C11 V1 V2 O2 13.55(7) 2_656 . . . ? C11 V1 V2 O2 -166.45(7) . . . . ? N3 V1 V2 O2 85.02(7) . . . 2_656 ? N3 V1 V2 O2 -94.98(7) 2_656 . . 2_656 ? O1 V1 V2 O2 174.17(6) 2_656 . . 2_656 ? O1 V1 V2 O2 -5.83(6) . . . 2_656 ? N1 V1 V2 O2 51.03(7) . . . 2_656 ? N1 V1 V2 O2 -128.97(7) 2_656 . . 2_656 ? C11 V1 V2 O2 -166.45(7) 2_656 . . 2_656 ? C11 V1 V2 O2 13.55(7) . . . 2_656 ? N3 V1 V2 N3 180.0 2_656 . . . ? O1 V1 V2 N3 89.15(7) 2_656 . . . ? O1 V1 V2 N3 -90.85(7) . . . . ? N1 V1 V2 N3 -33.99(8) . . . . ? N1 V1 V2 N3 146.01(8) 2_656 . . . ? C11 V1 V2 N3 108.53(8) 2_656 . . . ? C11 V1 V2 N3 -71.47(8) . . . . ? N3 V1 V2 N3 180.000(1) . . . 2_656 ? O1 V1 V2 N3 -90.85(7) 2_656 . . 2_656 ? O1 V1 V2 N3 89.15(7) . . . 2_656 ? N1 V1 V2 N3 146.01(8) . . . 2_656 ? N1 V1 V2 N3 -33.99(8) 2_656 . . 2_656 ? C11 V1 V2 N3 -71.47(8) 2_656 . . 2_656 ? C11 V1 V2 N3 108.53(8) . . . 2_656 ? N3 V1 V2 N2 -38.12(10) . . . . ? N3 V1 V2 N2 141.88(10) 2_656 . . . ? O1 V1 V2 N2 51.03(9) 2_656 . . . ? O1 V1 V2 N2 -128.97(9) . . . . ? N1 V1 V2 N2 -72.11(10) . . . . ? N1 V1 V2 N2 107.89(10) 2_656 . . . ? C11 V1 V2 N2 70.41(10) 2_656 . . . ? C11 V1 V2 N2 -109.59(10) . . . . ? N3 V1 V2 N2 141.88(10) . . . 2_656 ? N3 V1 V2 N2 -38.12(10) 2_656 . . 2_656 ? O1 V1 V2 N2 -128.97(9) 2_656 . . 2_656 ? O1 V1 V2 N2 51.03(9) . . . 2_656 ? N1 V1 V2 N2 107.89(10) . . . 2_656 ? N1 V1 V2 N2 -72.11(10) 2_656 . . 2_656 ? C11 V1 V2 N2 -109.59(10) 2_656 . . 2_656 ? C11 V1 V2 N2 70.41(10) . . . 2_656 ? N3 V1 V2 C31 -76.70(8) . . . . ? N3 V1 V2 C31 103.30(8) 2_656 . . . ? O1 V1 V2 C31 12.45(7) 2_656 . . . ? O1 V1 V2 C31 -167.55(7) . . . . ? N1 V1 V2 C31 -110.70(8) . . . . ? N1 V1 V2 C31 69.30(8) 2_656 . . . ? C11 V1 V2 C31 31.82(8) 2_656 . . . ? C11 V1 V2 C31 -148.18(8) . . . . ? N3 V1 V2 C31 103.30(8) . . . 2_656 ? N3 V1 V2 C31 -76.70(8) 2_656 . . 2_656 ? O1 V1 V2 C31 -167.55(7) 2_656 . . 2_656 ? O1 V1 V2 C31 12.45(7) . . . 2_656 ? N1 V1 V2 C31 69.30(8) . . . 2_656 ? N1 V1 V2 C31 -110.70(8) 2_656 . . 2_656 ? C11 V1 V2 C31 -148.18(8) 2_656 . . 2_656 ? C11 V1 V2 C31 31.82(8) . . . 2_656 ? N3 V1 N1 C11 -97.91(12) . . . . ? N3 V1 N1 C11 17.7(2) 2_656 . . . ? O1 V1 N1 C11 165.51(11) 2_656 . . . ? O1 V1 N1 C11 -5.31(11) . . . . ? N1 V1 N1 C11 106.28(12) 2_656 . . . ? C11 V1 N1 C11 136.93(11) 2_656 . . . ? V2 V1 N1 C11 -73.72(12) . . . . ? N3 V1 N1 C2 109.85(16) . . . . ? N3 V1 N1 C2 -134.54(18) 2_656 . . . ? O1 V1 N1 C2 13.26(17) 2_656 . . . ? O1 V1 N1 C2 -157.56(18) . . . . ? N1 V1 N1 C2 -45.96(14) 2_656 . . . ? C11 V1 N1 C2 -15.32(16) 2_656 . . . ? C11 V1 N1 C2 -152.2(2) . . . . ? V2 V1 N1 C2 134.04(14) . . . . ? O2 V2 N2 C31 -8.38(10) . . . . ? O2 V2 N2 C31 162.29(10) 2_656 . . . ? N3 V2 N2 C31 -103.70(11) . . . . ? N3 V2 N2 C31 10.31(19) 2_656 . . . ? N2 V2 N2 C31 103.09(13) 2_656 . . . ? C31 V2 N2 C31 134.05(10) 2_656 . . . ? V1 V2 N2 C31 -76.91(13) . . . . ? O2 V2 N2 C22 -156.65(19) . . . . ? O2 V2 N2 C22 14.01(19) 2_656 . . . ? N3 V2 N2 C22 108.02(18) . . . . ? N3 V2 N2 C22 -137.96(18) 2_656 . . . ? N2 V2 N2 C22 -45.19(14) 2_656 . . . ? C31 V2 N2 C22 -148.3(2) . . . . ? C31 V2 N2 C22 -14.23(18) 2_656 . . . ? V1 V2 N2 C22 134.81(14) . . . . ? N3 V1 N3 C41 -116.20(14) 2_656 . . . ? O1 V1 N3 C41 147.89(13) 2_656 . . . ? O1 V1 N3 C41 -21.45(13) . . . . ? N1 V1 N3 C41 42.26(14) . . . . ? N1 V1 N3 C41 127.39(16) 2_656 . . . ? C11 V1 N3 C41 138.71(12) 2_656 . . . ? C11 V1 N3 C41 9.93(14) . . . . ? V2 V1 N3 C41 -116.20(14) . . . . ? N3 V1 N3 C42 116.31(15) 2_656 . . . ? O1 V1 N3 C42 20.40(14) 2_656 . . . ? O1 V1 N3 C42 -148.94(13) . . . . ? N1 V1 N3 C42 -85.23(14) . . . . ? N1 V1 N3 C42 -0.1(2) 2_656 . . . ? C11 V1 N3 C42 11.22(17) 2_656 . . . ? C11 V1 N3 C42 -117.56(14) . . . . ? V2 V1 N3 C42 116.31(15) . . . . ? N3 V1 N3 V2 0.0 2_656 . . . ? O1 V1 N3 V2 -95.91(6) 2_656 . . . ? O1 V1 N3 V2 94.75(6) . . . . ? N1 V1 N3 V2 158.47(5) . . . . ? N1 V1 N3 V2 -116.41(15) 2_656 . . . ? C11 V1 N3 V2 -105.09(7) 2_656 . . . ? C11 V1 N3 V2 126.13(6) . . . . ? O2 V2 N3 C41 -149.51(12) . . . . ? O2 V2 N3 C41 19.75(13) 2_656 . . . ? N3 V2 N3 C41 118.54(13) 2_656 . . . ? N2 V2 N3 C41 -85.51(13) . . . . ? N2 V2 N3 C41 3.1(2) 2_656 . . . ? C31 V2 N3 C41 -117.56(13) . . . . ? C31 V2 N3 C41 9.52(15) 2_656 . . . ? V1 V2 N3 C41 118.54(13) . . . . ? O2 V2 N3 C42 -23.85(14) . . . . ? O2 V2 N3 C42 145.41(14) 2_656 . . . ? N3 V2 N3 C42 -115.80(15) 2_656 . . . ? N2 V2 N3 C42 40.15(15) . . . . ? N2 V2 N3 C42 128.79(15) 2_656 . . . ? C31 V2 N3 C42 8.10(15) . . . . ? C31 V2 N3 C42 135.19(13) 2_656 . . . ? V1 V2 N3 C42 -115.80(15) . . . . ? O2 V2 N3 V1 91.95(6) . . . . ? O2 V2 N3 V1 -98.79(6) 2_656 . . . ? N3 V2 N3 V1 0.0 2_656 . . . ? N2 V2 N3 V1 155.94(6) . . . . ? N2 V2 N3 V1 -115.41(12) 2_656 . . . ? C31 V2 N3 V1 123.90(6) . . . . ? C31 V2 N3 V1 -109.02(7) 2_656 . . . ? O3 V3 N4 C63 -7.90(10) . . . . ? N6 V3 N4 C63 -102.54(11) . . . . ? O4 V3 N4 C63 161.42(11) . . . . ? N7 V3 N4 C63 10.9(2) . . . . ? N5 V3 N4 C63 102.65(12) . . . . ? C73 V3 N4 C63 133.11(12) . . . . ? V3 V3 N4 C63 -77.66(13) 2_655 . . . ? O3 V3 N4 C44 -156.90(19) . . . . ? N6 V3 N4 C44 108.45(17) . . . . ? O4 V3 N4 C44 12.41(18) . . . . ? N7 V3 N4 C44 -138.07(19) . . . . ? N5 V3 N4 C44 -46.36(17) . . . . ? C63 V3 N4 C44 -149.0(2) . . . . ? C73 V3 N4 C44 -15.90(18) . . . . ? V3 V3 N4 C44 133.33(15) 2_655 . . . ? O3 V3 N5 C73 163.42(13) . . . . ? N6 V3 N5 C73 14.5(2) . . . . ? O4 V3 N5 C73 -7.25(13) . . . . ? N7 V3 N5 C73 -100.83(13) . . . . ? N4 V3 N5 C73 104.18(14) . . . . ? C63 V3 N5 C73 135.34(13) . . . . ? V3 V3 N5 C73 -75.50(15) 2_655 . . . ? O3 V3 N5 C54 14.47(18) . . . . ? N6 V3 N5 C54 -134.43(19) . . . . ? O4 V3 N5 C54 -156.19(19) . . . . ? N7 V3 N5 C54 110.23(17) . . . . ? N4 V3 N5 C54 -44.76(17) . . . . ? C63 V3 N5 C54 -13.60(17) . . . . ? C73 V3 N5 C54 -148.9(2) . . . . ? V3 V3 N5 C54 135.55(15) 2_655 . . . ? O3 V3 N6 C83 -21.97(16) . . . . ? O4 V3 N6 C83 146.92(16) . . . . ? N7 V3 N6 C83 -115.75(15) . . . . ? N4 V3 N6 C83 41.69(16) . . . . ? N5 V3 N6 C83 127.62(17) . . . . ? C63 V3 N6 C83 9.55(17) . . . . ? C73 V3 N6 C83 136.72(15) . . . . ? V3 V3 N6 C83 -115.75(15) 2_655 . . . ? O3 V3 N6 C83 -148.95(16) . . . 2_655 ? O4 V3 N6 C83 19.94(16) . . . 2_655 ? N7 V3 N6 C83 117.27(15) . . . 2_655 ? N4 V3 N6 C83 -85.30(16) . . . 2_655 ? N5 V3 N6 C83 0.6(3) . . . 2_655 ? C63 V3 N6 C83 -117.43(16) . . . 2_655 ? C73 V3 N6 C83 9.74(19) . . . 2_655 ? V3 V3 N6 C83 117.27(15) 2_655 . . 2_655 ? O3 V3 N6 V3 93.78(4) . . . 2_655 ? O4 V3 N6 V3 -97.33(5) . . . 2_655 ? N7 V3 N6 V3 0.0 . . . 2_655 ? N4 V3 N6 V3 157.44(5) . . . 2_655 ? N5 V3 N6 V3 -116.63(16) . . . 2_655 ? C63 V3 N6 V3 125.30(5) . . . 2_655 ? C73 V3 N6 V3 -107.53(7) . . . 2_655 ? O3 V3 N7 C84 18.71(16) . . . . ? N6 V3 N7 C84 116.56(15) . . . . ? O4 V3 N7 C84 -149.30(16) . . . . ? N4 V3 N7 C84 2.0(3) . . . . ? N5 V3 N7 C84 -85.85(16) . . . . ? C63 V3 N7 C84 8.90(18) . . . . ? C73 V3 N7 C84 -117.68(16) . . . . ? V3 V3 N7 C84 116.56(15) 2_655 . . . ? O3 V3 N7 C84 147.20(16) . . . 2_655 ? N6 V3 N7 C84 -114.95(16) . . . 2_655 ? O4 V3 N7 C84 -20.82(17) . . . 2_655 ? N4 V3 N7 C84 130.44(17) . . . 2_655 ? N5 V3 N7 C84 42.63(17) . . . 2_655 ? C63 V3 N7 C84 137.38(15) . . . 2_655 ? C73 V3 N7 C84 10.80(18) . . . 2_655 ? V3 V3 N7 C84 -114.95(16) 2_655 . . 2_655 ? O3 V3 N7 V3 -97.85(4) . . . 2_655 ? N6 V3 N7 V3 0.0 . . . 2_655 ? O4 V3 N7 V3 94.14(5) . . . 2_655 ? N4 V3 N7 V3 -114.60(15) . . . 2_655 ? N5 V3 N7 V3 157.59(6) . . . 2_655 ? C63 V3 N7 V3 -107.67(6) . . . 2_655 ? C73 V3 N7 V3 125.76(6) . . . 2_655 ? N3 V1 O1 C11 100.90(12) . . . . ? N3 V1 O1 C11 -165.42(12) 2_656 . . . ? O1 V1 O1 C11 -32.20(11) 2_656 . . . ? N1 V1 O1 C11 5.41(11) . . . . ? N1 V1 O1 C11 -66.53(12) 2_656 . . . ? C11 V1 O1 C11 -55.59(18) 2_656 . . . ? V2 V1 O1 C11 147.80(11) . . . . ? O2 V2 O2 C31 -29.37(10) 2_656 . . . ? N3 V2 O2 C31 103.98(11) . . . . ? N3 V2 O2 C31 -163.39(11) 2_656 . . . ? N2 V2 O2 C31 8.39(11) . . . . ? N2 V2 O2 C31 -63.78(12) 2_656 . . . ? C31 V2 O2 C31 -50.71(17) 2_656 . . . ? V1 V2 O2 C31 150.63(10) . . . . ? N6 V3 O3 C63 103.00(12) . . . . ? O4 V3 O3 C63 -32.7(3) . . . . ? N7 V3 O3 C63 -164.21(12) . . . . ? N4 V3 O3 C63 8.02(11) . . . . ? N5 V3 O3 C63 -64.31(12) . . . . ? C73 V3 O3 C63 -52.40(15) . . . . ? V3 V3 O3 C63 149.53(10) 2_655 . . . ? O3 V3 O4 C73 -27.7(3) . . . . ? N6 V3 O4 C73 -163.76(14) . . . . ? N7 V3 O4 C73 103.43(14) . . . . ? N4 V3 O4 C73 -64.58(14) . . . . ? N5 V3 O4 C73 7.22(12) . . . . ? C63 V3 O4 C73 -50.92(17) . . . . ? V3 V3 O4 C73 150.09(12) 2_655 . . . ? C11 N1 C2 C3 114.7(2) . . . . ? V1 N1 C2 C3 -102.7(2) . . . . ? C11 N1 C2 C1 -74.8(3) . . . . ? V1 N1 C2 C1 67.8(2) . . . . ? C6 C1 C2 N1 -165.43(19) . . . . ? C1 C1 C2 N1 12.4(3) 2_656 . . . ? C6 C1 C2 C3 4.8(3) . . . . ? C1 C1 C2 C3 -177.3(2) 2_656 . . . ? N1 C2 C3 C4 170.40(19) . . . . ? C1 C2 C3 C4 -0.2(3) . . . . ? C2 C3 C4 C5 -3.7(3) . . . . ? C3 C4 C5 C6 2.7(3) . . . . ? C3 C4 C5 C10 -175.8(2) . . . . ? C4 C5 C6 C1 2.0(3) . . . . ? C10 C5 C6 C1 -179.6(2) . . . . ? C4 C5 C6 C7 -173.5(2) . . . . ? C10 C5 C6 C7 4.9(3) . . . . ? C2 C1 C6 C5 -5.7(3) . . . . ? C1 C1 C6 C5 176.4(2) 2_656 . . . ? C2 C1 C6 C7 169.79(19) . . . . ? C1 C1 C6 C7 -8.1(3) 2_656 . . . ? C5 C6 C7 C8 -20.8(3) . . . . ? C1 C6 C7 C8 163.69(19) . . . . ? C6 C7 C8 C9 49.9(3) . . . . ? C7 C8 C9 C10 -63.4(2) . . . . ? C8 C9 C10 C5 47.3(2) . . . . ? C4 C5 C10 C9 159.78(19) . . . . ? C6 C5 C10 C9 -18.7(3) . . . . ? V1 O1 C11 N1 -8.32(17) . . . . ? V1 O1 C11 C12 169.85(17) . . . . ? C2 N1 C11 O1 161.7(2) . . . . ? V1 N1 C11 O1 8.27(17) . . . . ? C2 N1 C11 C12 -16.3(4) . . . . ? V1 N1 C11 C12 -169.7(2) . . . . ? C2 N1 C11 V1 153.4(2) . . . . ? N3 V1 C11 O1 -83.62(12) . . . . ? N3 V1 C11 O1 17.76(14) 2_656 . . . ? O1 V1 C11 O1 168.91(7) 2_656 . . . ? N1 V1 C11 O1 -170.88(19) . . . . ? N1 V1 C11 O1 117.53(12) 2_656 . . . ? C11 V1 C11 O1 140.87(13) 2_656 . . . ? V2 V1 C11 O1 -39.13(13) . . . . ? N3 V1 C11 N1 87.26(12) . . . . ? N3 V1 C11 N1 -171.36(11) 2_656 . . . ? O1 V1 C11 N1 -20.21(15) 2_656 . . . ? O1 V1 C11 N1 170.88(19) . . . . ? N1 V1 C11 N1 -71.60(13) 2_656 . . . ? C11 V1 C11 N1 -48.25(10) 2_656 . . . ? V2 V1 C11 N1 131.75(10) . . . . ? N3 V1 C11 C12 -153.5(8) . . . . ? N3 V1 C11 C12 -52.1(9) 2_656 . . . ? O1 V1 C11 C12 99.0(8) 2_656 . . . ? O1 V1 C11 C12 -69.9(8) . . . . ? N1 V1 C11 C12 119.2(9) . . . . ? N1 V1 C11 C12 47.6(9) 2_656 . . . ? C11 V1 C11 C12 71.0(8) 2_656 . . . ? V2 V1 C11 C12 -109.0(8) . . . . ? O1 C11 C12 C13 126.9(2) . . . . ? N1 C11 C12 C13 -55.2(3) . . . . ? V1 C11 C12 C13 -168.5(7) . . . . ? O1 C11 C12 C17 -50.9(3) . . . . ? N1 C11 C12 C17 127.0(2) . . . . ? V1 C11 C12 C17 13.7(10) . . . . ? C17 C12 C13 C14 -3.0(3) . . . . ? C11 C12 C13 C14 179.2(2) . . . . ? C17 C12 C13 C18 172.6(2) . . . . ? C11 C12 C13 C18 -5.1(3) . . . . ? C12 C13 C14 C15 0.8(4) . . . . ? C18 C13 C14 C15 -175.1(2) . . . . ? C13 C14 C15 C16 1.3(4) . . . . ? C13 C14 C15 C19 178.1(3) . . . . ? C14 C15 C16 C17 -1.2(4) . . . . ? C19 C15 C16 C17 -178.0(3) . . . . ? C15 C16 C17 C12 -0.9(4) . . . . ? C15 C16 C17 C20 178.0(2) . . . . ? C13 C12 C17 C16 3.0(3) . . . . ? C11 C12 C17 C16 -179.15(19) . . . . ? C13 C12 C17 C20 -175.8(2) . . . . ? C11 C12 C17 C20 2.0(3) . . . . ? C26 C21 C22 C23 4.8(3) . . . . ? C21 C21 C22 C23 -177.7(2) 2_656 . . . ? C26 C21 C22 N2 -164.20(17) . . . . ? C21 C21 C22 N2 13.3(3) 2_656 . . . ? C31 N2 C22 C23 121.2(2) . . . . ? V2 N2 C22 C23 -102.17(19) . . . . ? C31 N2 C22 C21 -69.5(3) . . . . ? V2 N2 C22 C21 67.1(3) . . . . ? C21 C22 C23 C24 -0.9(3) . . . . ? N2 C22 C23 C24 168.51(18) . . . . ? C22 C23 C24 C25 -3.0(3) . . . . ? C23 C24 C25 C26 2.9(3) . . . . ? C23 C24 C25 C30 -176.37(19) . . . . ? C24 C25 C26 C21 1.1(3) . . . . ? C30 C25 C26 C21 -179.66(18) . . . . ? C24 C25 C26 C27 -175.42(18) . . . . ? C30 C25 C26 C27 3.8(3) . . . . ? C22 C21 C26 C25 -4.9(3) . . . . ? C21 C21 C26 C25 177.56(19) 2_656 . . . ? C22 C21 C26 C27 171.65(17) . . . . ? C21 C21 C26 C27 -5.9(3) 2_656 . . . ? C25 C26 C27 C28 -21.1(3) . . . . ? C21 C26 C27 C28 162.32(18) . . . . ? C26 C27 C28 C29 50.6(2) . . . . ? C27 C28 C29 C30 -63.4(2) . . . . ? C26 C25 C30 C29 -16.3(3) . . . . ? C24 C25 C30 C29 162.97(18) . . . . ? C28 C29 C30 C25 45.4(2) . . . . ? V2 O2 C31 N2 -13.29(16) . . . . ? V2 O2 C31 C32 164.68(14) . . . . ? C22 N2 C31 O2 161.97(17) . . . . ? V2 N2 C31 O2 12.93(15) . . . . ? C22 N2 C31 C32 -15.8(3) . . . . ? V2 N2 C31 C32 -164.81(18) . . . . ? C22 N2 C31 V2 149.0(2) . . . . ? O2 V2 C31 O2 169.82(6) 2_656 . . . ? N3 V2 C31 O2 -82.69(12) . . . . ? N3 V2 C31 O2 19.67(13) 2_656 . . . ? N2 V2 C31 O2 -165.73(17) . . . . ? N2 V2 C31 O2 119.86(11) 2_656 . . . ? C31 V2 C31 O2 143.87(13) 2_656 . . . ? V1 V2 C31 O2 -36.13(13) . . . . ? O2 V2 C31 N2 165.73(17) . . . . ? O2 V2 C31 N2 -24.45(14) 2_656 . . . ? N3 V2 C31 N2 83.04(11) . . . . ? N3 V2 C31 N2 -174.61(10) 2_656 . . . ? N2 V2 C31 N2 -74.42(13) 2_656 . . . ? C31 V2 C31 N2 -50.40(9) 2_656 . . . ? V1 V2 C31 N2 129.60(9) . . . . ? O2 V2 C31 C32 -71.8(6) . . . . ? O2 V2 C31 C32 98.0(6) 2_656 . . . ? N3 V2 C31 C32 -154.5(6) . . . . ? N3 V2 C31 C32 -52.2(6) 2_656 . . . ? N2 V2 C31 C32 122.4(6) . . . . ? N2 V2 C31 C32 48.0(6) 2_656 . . . ? C31 V2 C31 C32 72.0(6) 2_656 . . . ? V1 V2 C31 C32 -108.0(6) . . . . ? O2 C31 C32 C37 -49.0(2) . . . . ? N2 C31 C32 C37 128.6(2) . . . . ? V2 C31 C32 C37 14.9(7) . . . . ? O2 C31 C32 C33 130.8(2) . . . . ? N2 C31 C32 C33 -51.6(3) . . . . ? V2 C31 C32 C33 -165.3(5) . . . . ? C37 C32 C33 C34 -3.7(3) . . . . ? C31 C32 C33 C34 176.50(18) . . . . ? C37 C32 C33 C38 171.00(19) . . . . ? C31 C32 C33 C38 -8.8(3) . . . . ? C32 C33 C34 C35 -0.5(3) . . . . ? C38 C33 C34 C35 -175.3(2) . . . . ? C33 C34 C35 C36 3.0(4) . . . . ? C33 C34 C35 C39 -177.7(2) . . . . ? C34 C35 C36 C37 -1.5(3) . . . . ? C39 C35 C36 C37 179.2(2) . . . . ? C35 C36 C37 C32 -2.5(3) . . . . ? C35 C36 C37 C40 174.6(2) . . . . ? C33 C32 C37 C36 5.1(3) . . . . ? C31 C32 C37 C36 -175.05(17) . . . . ? C33 C32 C37 C40 -171.80(18) . . . . ? C31 C32 C37 C40 8.0(3) . . . . ? C48 C43 C44 C45 3.9(3) . . . . ? C53 C43 C44 C45 -176.5(2) . . . . ? C48 C43 C44 N4 -165.9(2) . . . . ? C53 C43 C44 N4 13.6(3) . . . . ? C63 N4 C44 C45 120.3(2) . . . . ? V3 N4 C44 C45 -101.9(2) . . . . ? C63 N4 C44 C43 -69.7(3) . . . . ? V3 N4 C44 C43 68.2(3) . . . . ? C43 C44 C45 C46 0.7(4) . . . . ? N4 C44 C45 C46 171.0(2) . . . . ? C44 C45 C46 C47 -4.0(4) . . . . ? C45 C46 C47 C48 2.6(3) . . . . ? C45 C46 C47 C52 -176.2(2) . . . . ? C44 C43 C48 C47 -5.3(3) . . . . ? C53 C43 C48 C47 175.1(2) . . . . ? C44 C43 C48 C49 169.8(2) . . . . ? C53 C43 C48 C49 -9.8(3) . . . . ? C46 C47 C48 C43 2.1(3) . . . . ? C52 C47 C48 C43 -179.2(2) . . . . ? C46 C47 C48 C49 -173.0(2) . . . . ? C52 C47 C48 C49 5.6(3) . . . . ? C43 C48 C49 C50 163.8(2) . . . . ? C47 C48 C49 C50 -21.0(3) . . . . ? C48 C49 C50 C51 50.1(3) . . . . ? C49 C50 C51 C52 -63.7(2) . . . . ? C46 C47 C52 C51 159.7(2) . . . . ? C48 C47 C52 C51 -19.0(3) . . . . ? C50 C51 C52 C47 47.1(3) . . . . ? C48 C43 C53 C54 116.3(2) . . . . ? C44 C43 C53 C54 -63.2(3) . . . . ? C48 C43 C53 C58 -65.7(3) . . . . ? C44 C43 C53 C58 114.8(2) . . . . ? C58 C53 C54 N5 -166.91(18) . . . . ? C43 C53 C54 N5 11.2(3) . . . . ? C58 C53 C54 C55 2.5(3) . . . . ? C43 C53 C54 C55 -179.38(19) . . . . ? C73 N5 C54 C53 -69.2(3) . . . . ? V3 N5 C54 C53 68.8(3) . . . . ? C73 N5 C54 C55 121.1(2) . . . . ? V3 N5 C54 C55 -100.9(2) . . . . ? C53 C54 C55 C56 0.7(3) . . . . ? N5 C54 C55 C56 170.74(19) . . . . ? C54 C55 C56 C57 -3.0(3) . . . . ? C55 C56 C57 C58 2.0(3) . . . . ? C55 C56 C57 C62 -177.60(19) . . . . ? C56 C57 C58 C53 1.3(3) . . . . ? C62 C57 C58 C53 -179.10(17) . . . . ? C56 C57 C58 C59 -173.74(17) . . . . ? C62 C57 C58 C59 5.8(3) . . . . ? C54 C53 C58 C57 -3.5(3) . . . . ? C43 C53 C58 C57 178.39(17) . . . . ? C54 C53 C58 C59 171.49(17) . . . . ? C43 C53 C58 C59 -6.6(3) . . . . ? C57 C58 C59 C60 -22.1(2) . . . . ? C53 C58 C59 C60 162.85(17) . . . . ? C58 C59 C60 C61 50.5(2) . . . . ? C59 C60 C61 C62 -62.2(2) . . . . ? C60 C61 C62 C57 45.1(2) . . . . ? C56 C57 C62 C61 161.62(18) . . . . ? C58 C57 C62 C61 -17.9(3) . . . . ? V3 O3 C63 N4 -12.50(16) . . . . ? V3 O3 C63 C64 164.53(15) . . . . ? C44 N4 C63 O3 162.16(18) . . . . ? V3 N4 C63 O3 12.29(16) . . . . ? C44 N4 C63 C64 -14.7(3) . . . . ? V3 N4 C63 C64 -164.54(17) . . . . ? C44 N4 C63 V3 149.9(2) . . . . ? N6 V3 C63 O3 -82.90(12) . . . . ? O4 V3 C63 O3 168.00(12) . . . . ? N7 V3 C63 O3 19.02(14) . . . . ? N4 V3 C63 O3 -166.44(18) . . . . ? N5 V3 C63 O3 118.94(12) . . . . ? C73 V3 C63 O3 142.12(12) . . . . ? V3 V3 C63 O3 -37.49(13) 2_655 . . . ? O3 V3 C63 N4 166.44(18) . . . . ? N6 V3 C63 N4 83.54(12) . . . . ? O4 V3 C63 N4 -25.56(15) . . . . ? N7 V3 C63 N4 -174.54(11) . . . . ? N5 V3 C63 N4 -74.62(12) . . . . ? C73 V3 C63 N4 -51.44(13) . . . . ? V3 V3 C63 N4 128.96(10) 2_655 . . . ? O3 V3 C63 C64 -81.3(6) . . . . ? N6 V3 C63 C64 -164.2(6) . . . . ? O4 V3 C63 C64 86.7(6) . . . . ? N7 V3 C63 C64 -62.3(6) . . . . ? N4 V3 C63 C64 112.2(6) . . . . ? N5 V3 C63 C64 37.6(6) . . . . ? C73 V3 C63 C64 60.8(6) . . . . ? V3 V3 C63 C64 -118.8(6) 2_655 . . . ? O3 C63 C64 C69 -45.4(3) . . . . ? N4 C63 C64 C69 131.2(2) . . . . ? V3 C63 C64 C69 27.7(7) . . . . ? O3 C63 C64 C65 135.12(19) . . . . ? N4 C63 C64 C65 -48.3(3) . . . . ? V3 C63 C64 C65 -151.8(5) . . . . ? C69 C64 C65 C66 -6.4(3) . . . . ? C63 C64 C65 C66 173.04(17) . . . . ? C69 C64 C65 C70 168.86(19) . . . . ? C63 C64 C65 C70 -11.7(3) . . . . ? C64 C65 C66 C67 0.8(3) . . . . ? C70 C65 C66 C67 -174.59(18) . . . . ? C65 C66 C67 C68 4.0(3) . . . . ? C65 C66 C67 C71 -176.61(18) . . . . ? C66 C67 C68 C69 -3.5(3) . . . . ? C71 C67 C68 C69 177.15(18) . . . . ? C67 C68 C69 C64 -1.9(3) . . . . ? C67 C68 C69 C72 177.46(19) . . . . ? C65 C64 C69 C68 6.9(3) . . . . ? C63 C64 C69 C68 -172.58(17) . . . . ? C65 C64 C69 C72 -172.49(19) . . . . ? C63 C64 C69 C72 8.1(3) . . . . ? C54 N5 C73 O4 161.21(19) . . . . ? V3 N5 C73 O4 11.34(19) . . . . ? C54 N5 C73 C74 -17.4(4) . . . . ? V3 N5 C73 C74 -167.2(2) . . . . ? C54 N5 C73 V3 149.9(2) . . . . ? V3 O4 C73 N5 -11.43(19) . . . . ? V3 O4 C73 C74 167.29(18) . . . . ? O3 V3 C73 N5 -22.52(17) . . . . ? N6 V3 C73 N5 -172.68(12) . . . . ? O4 V3 C73 N5 167.7(2) . . . . ? N7 V3 C73 N5 85.37(13) . . . . ? N4 V3 C73 N5 -73.32(13) . . . . ? C63 V3 C73 N5 -48.83(14) . . . . ? V3 V3 C73 N5 130.78(11) 2_655 . . . ? O3 V3 C73 O4 169.82(12) . . . . ? N6 V3 C73 O4 19.67(16) . . . . ? N7 V3 C73 O4 -82.28(14) . . . . ? N4 V3 C73 O4 119.02(14) . . . . ? N5 V3 C73 O4 -167.7(2) . . . . ? C63 V3 C73 O4 143.52(13) . . . . ? V3 V3 C73 O4 -36.88(15) 2_655 . . . ? O3 V3 C73 C74 97.8(9) . . . . ? N6 V3 C73 C74 -52.3(9) . . . . ? O4 V3 C73 C74 -72.0(9) . . . . ? N7 V3 C73 C74 -154.3(9) . . . . ? N4 V3 C73 C74 47.0(9) . . . . ? N5 V3 C73 C74 120.4(9) . . . . ? C63 V3 C73 C74 71.5(9) . . . . ? V3 V3 C73 C74 -108.9(9) 2_655 . . . ? N5 C73 C74 C75 129.1(3) . . . . ? O4 C73 C74 C75 -49.4(3) . . . . ? V3 C73 C74 C75 16.1(10) . . . . ? N5 C73 C74 C79 -51.9(4) . . . . ? O4 C73 C74 C79 129.6(3) . . . . ? V3 C73 C74 C79 -164.9(8) . . . . ? C79 C74 C75 C76 5.7(4) . . . . ? C73 C74 C75 C76 -175.4(2) . . . . ? C79 C74 C75 C80 -174.1(3) . . . . ? C73 C74 C75 C80 4.9(4) . . . . ? C74 C75 C76 C77 -3.1(5) . . . . ? C80 C75 C76 C77 176.7(3) . . . . ? C75 C76 C77 C78 -0.2(6) . . . . ? C75 C76 C77 C81 179.6(3) . . . . ? C76 C77 C78 C79 1.1(6) . . . . ? C81 C77 C78 C79 -178.7(3) . . . . ? C75 C74 C79 C78 -4.8(4) . . . . ? C73 C74 C79 C78 176.2(3) . . . . ? C75 C74 C79 C82 171.9(3) . . . . ? C73 C74 C79 C82 -7.1(4) . . . . ? C77 C78 C79 C74 1.4(5) . . . . ? C77 C78 C79 C82 -175.5(4) . . . . ? loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 -0.004 -0.013 0.000 4178 1368 ' ' 2 0.500 0.082 0.500 14 0 ' ' 3 0.000 0.582 0.500 14 0 ' ' _platon_squeeze_details ; ; _diffrn_measured_fraction_theta_max 0.955 _diffrn_reflns_theta_full 72.68 _diffrn_measured_fraction_theta_full 0.955 _refine_diff_density_max 0.238 _refine_diff_density_min -0.524 _refine_diff_density_rms 0.040