# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_f70315b _database_code_depnum_ccdc_archive 'CCDC 703853' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H63 Dy2 N13' _chemical_formula_weight 1002.99 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' Dy Dy -0.1892 4.4098 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.048(4) _cell_length_b 36.093(13) _cell_length_c 12.195(4) _cell_angle_alpha 90.00 _cell_angle_beta 107.660(5) _cell_angle_gamma 90.00 _cell_volume 4214(3) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 990 _cell_measurement_theta_min 2.377 _cell_measurement_theta_max 25.631 _exptl_crystal_description block _exptl_crystal_colour pale-yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.581 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2008 _exptl_absorpt_coefficient_mu 3.560 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5362 _exptl_absorpt_correction_T_max 0.6173 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16809 _diffrn_reflns_av_R_equivalents 0.0390 _diffrn_reflns_av_sigmaI/netI 0.0645 _diffrn_reflns_limit_h_min -5 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -41 _diffrn_reflns_limit_k_max 44 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 26.01 _reflns_number_total 8248 _reflns_number_gt 6014 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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. ; _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^)+(0.0158P)^2^+50.0000P] 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 8248 _refine_ls_number_parameters 460 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0932 _refine_ls_R_factor_gt 0.0641 _refine_ls_wR_factor_ref 0.1219 _refine_ls_wR_factor_gt 0.1114 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.054 _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 Dy1 Dy 0.16306(4) 0.116652(13) 0.48955(4) 0.03377(13) Uani 1 1 d . . . Dy2 Dy 0.11341(4) 0.120589(13) 0.18047(4) 0.03517(13) Uani 1 1 d . . . N1 N 0.3799(11) 0.2171(3) 0.6170(11) 0.070(3) Uani 1 1 d . . . N2 N 0.4826(12) 0.1737(4) 0.7603(10) 0.085(4) Uani 1 1 d . . . N3 N 0.3281(8) 0.1541(2) 0.5840(8) 0.047(2) Uani 1 1 d . . . N4 N -0.0819(10) 0.1775(3) 0.6419(9) 0.061(3) Uani 1 1 d . . . N5 N -0.2574(9) 0.1633(3) 0.4718(9) 0.060(3) Uani 1 1 d . . . N6 N -0.0176(8) 0.1653(2) 0.4815(7) 0.0378(19) Uani 1 1 d . . . N7 N -0.1124(9) 0.1996(2) 0.3069(8) 0.051(2) Uani 1 1 d . . . N8 N 0.0195(8) 0.1439(2) 0.3145(7) 0.0364(18) Uani 1 1 d . . . N9 N 0.2535(8) 0.0935(2) 0.3541(7) 0.0379(19) Uani 1 1 d . . . N10 N 0.4661(9) 0.0610(3) 0.3861(9) 0.059(3) Uani 1 1 d . . . N11 N 0.3112(8) 0.0701(2) 0.1961(7) 0.040(2) Uani 1 1 d . . . N12 N 0.3372(11) 0.0388(3) 0.0411(9) 0.058(3) Uani 1 1 d . . . N13 N 0.2938(9) 0.0046(2) 0.1851(8) 0.051(2) Uani 1 1 d . . . C1 C -0.0197(15) 0.0795(4) 0.5797(15) 0.077(5) Uani 1 1 d . . . H1A H -0.1039 0.0914 0.5726 0.093 Uiso 1 1 calc R . . C2 C 0.0058(16) 0.0546(4) 0.5020(13) 0.070(4) Uani 1 1 d . . . H2A H -0.0585 0.0465 0.4339 0.084 Uiso 1 1 calc R . . C3 C 0.1428(17) 0.0439(3) 0.5436(14) 0.073(4) Uani 1 1 d . . . H3A H 0.1876 0.0275 0.5077 0.088 Uiso 1 1 calc R . . C4 C 0.2033(16) 0.0613(4) 0.6467(12) 0.076(4) Uani 1 1 d . . . H4A H 0.2953 0.0587 0.6930 0.092 Uiso 1 1 calc R . . C5 C 0.1020(17) 0.0834(4) 0.6692(12) 0.071(4) Uani 1 1 d . . . H5A H 0.1140 0.0983 0.7336 0.085 Uiso 1 1 calc R . . C6 C 0.3922(10) 0.1795(4) 0.6486(10) 0.053(3) Uani 1 1 d . . . C7 C 0.5087(17) 0.1363(6) 0.7934(14) 0.126(8) Uani 1 1 d . . . H7A H 0.5279 0.1226 0.7323 0.188 Uiso 1 1 calc R . . H7B H 0.4283 0.1260 0.8090 0.188 Uiso 1 1 calc R . . H7C H 0.5878 0.1348 0.8614 0.188 Uiso 1 1 calc R . . C8 C 0.4537(19) 0.1949(7) 0.8542(15) 0.149(10) Uani 1 1 d . . . H8A H 0.4355 0.2203 0.8312 0.223 Uiso 1 1 calc R . . H8B H 0.5332 0.1936 0.9219 0.223 Uiso 1 1 calc R . . H8C H 0.3736 0.1846 0.8706 0.223 Uiso 1 1 calc R . . C9 C 0.4926(14) 0.2432(4) 0.6579(16) 0.104(6) Uani 1 1 d . . . H9A H 0.4627 0.2672 0.6258 0.156 Uiso 1 1 calc R . . H9B H 0.5712 0.2353 0.6347 0.156 Uiso 1 1 calc R . . H9C H 0.5189 0.2446 0.7403 0.156 Uiso 1 1 calc R . . C10 C 0.2869(15) 0.2269(4) 0.5098(15) 0.083(5) Uani 1 1 d . . . H10A H 0.2145 0.2086 0.4865 0.124 Uiso 1 1 calc R . . H10B H 0.3364 0.2282 0.4538 0.124 Uiso 1 1 calc R . . H10C H 0.2461 0.2506 0.5156 0.124 Uiso 1 1 calc R . . C11 C -0.1177(10) 0.1687(3) 0.5278(10) 0.047(3) Uani 1 1 d . . . C12 C 0.0589(13) 0.1912(4) 0.6987(11) 0.077(4) Uani 1 1 d . . . H12A H 0.0957 0.2024 0.6428 0.116 Uiso 1 1 calc R . . H12B H 0.1177 0.1709 0.7349 0.116 Uiso 1 1 calc R . . H12C H 0.0557 0.2092 0.7558 0.116 Uiso 1 1 calc R . . C13 C -0.1489(16) 0.1600(5) 0.7180(13) 0.093(5) Uani 1 1 d . . . H13A H -0.2408 0.1519 0.6744 0.139 Uiso 1 1 calc R . . H13B H -0.1558 0.1774 0.7755 0.139 Uiso 1 1 calc R . . H13C H -0.0947 0.1390 0.7546 0.139 Uiso 1 1 calc R . . C14 C -0.3646(13) 0.1860(5) 0.4979(14) 0.094(5) Uani 1 1 d . . . H14A H -0.3240 0.1994 0.5681 0.141 Uiso 1 1 calc R . . H14B H -0.4380 0.1703 0.5063 0.141 Uiso 1 1 calc R . . H14C H -0.4022 0.2032 0.4362 0.141 Uiso 1 1 calc R . . C15 C -0.3055(12) 0.1415(4) 0.3688(12) 0.072(4) Uani 1 1 d . . . H15A H -0.2290 0.1276 0.3583 0.108 Uiso 1 1 calc R . . H15B H -0.3425 0.1576 0.3040 0.108 Uiso 1 1 calc R . . H15C H -0.3772 0.1249 0.3753 0.108 Uiso 1 1 calc R . . C16 C -0.0378(9) 0.1681(3) 0.3610(9) 0.035(2) Uani 1 1 d . . . C17 C -0.1304(15) 0.2323(3) 0.3690(13) 0.077(4) Uani 1 1 d . . . H17A H -0.0941 0.2278 0.4502 0.116 Uiso 1 1 calc R . . H17B H -0.2279 0.2382 0.3495 0.116 Uiso 1 1 calc R . . H17C H -0.0810 0.2526 0.3486 0.116 Uiso 1 1 calc R . . C18 C -0.1616(13) 0.2018(4) 0.1847(11) 0.070(4) Uani 1 1 d . . . H18A H -0.1452 0.1786 0.1523 0.105 Uiso 1 1 calc R . . H18B H -0.1130 0.2212 0.1590 0.105 Uiso 1 1 calc R . . H18C H -0.2599 0.2070 0.1604 0.105 Uiso 1 1 calc R . . C19 C -0.0928(13) 0.0685(4) 0.1329(11) 0.065(4) Uani 1 1 d . . . H19A H -0.0974 0.0544 0.1954 0.077 Uiso 1 1 calc R . . C20 C -0.1607(11) 0.1019(4) 0.0969(11) 0.061(3) Uani 1 1 d . . . H20A H -0.2189 0.1141 0.1317 0.073 Uiso 1 1 calc R . . C21 C -0.1275(11) 0.1142(4) 0.0008(11) 0.065(3) Uani 1 1 d . . . H21A H -0.1591 0.1357 -0.0411 0.078 Uiso 1 1 calc R . . C22 C -0.0362(12) 0.0875(4) -0.0206(11) 0.065(4) Uani 1 1 d . . . H22A H 0.0044 0.0885 -0.0797 0.078 Uiso 1 1 calc R . . C23 C -0.0170(12) 0.0603(4) 0.0584(12) 0.062(3) Uani 1 1 d . . . H23A H 0.0383 0.0394 0.0622 0.075 Uiso 1 1 calc R . . C24 C 0.1780(13) 0.1936(3) 0.1856(12) 0.061(3) Uani 1 1 d . . . H24A H 0.1369 0.2085 0.2284 0.073 Uiso 1 1 calc R . . C25 C 0.1202(15) 0.1848(4) 0.0653(13) 0.070(4) Uani 1 1 d . . . H25A H 0.0356 0.1931 0.0158 0.084 Uiso 1 1 calc R . . C26 C 0.2144(15) 0.1620(4) 0.0377(12) 0.068(4) Uani 1 1 d . . . H26A H 0.2037 0.1517 -0.0345 0.082 Uiso 1 1 calc R . . C27 C 0.3280(13) 0.1566(3) 0.1345(12) 0.058(3) Uani 1 1 d . . . H27A H 0.4066 0.1425 0.1379 0.070 Uiso 1 1 calc R . . C28 C 0.3045(12) 0.1759(3) 0.2259(12) 0.061(3) Uani 1 1 d . . . H28A H 0.3641 0.1766 0.3010 0.073 Uiso 1 1 calc R . . C29 C 0.3385(9) 0.0742(3) 0.3160(9) 0.036(2) Uani 1 1 d . . . C30 C 0.5707(12) 0.0436(4) 0.3445(12) 0.073(4) Uani 1 1 d . . . H30A H 0.5347 0.0404 0.2626 0.109 Uiso 1 1 calc R . . H30B H 0.5943 0.0198 0.3806 0.109 Uiso 1 1 calc R . . H30C H 0.6526 0.0589 0.3625 0.109 Uiso 1 1 calc R . . C31 C 0.5030(13) 0.0678(4) 0.5081(11) 0.078(4) Uani 1 1 d . . . H31A H 0.4263 0.0796 0.5256 0.117 Uiso 1 1 calc R . . H31B H 0.5834 0.0837 0.5310 0.117 Uiso 1 1 calc R . . H31C H 0.5241 0.0447 0.5488 0.117 Uiso 1 1 calc R . . C32 C 0.3145(10) 0.0383(3) 0.1456(10) 0.044(3) Uani 1 1 d . . . C33 C 0.2573(16) 0.0154(4) -0.0560(12) 0.082(4) Uani 1 1 d . . . H33A H 0.2231 -0.0061 -0.0267 0.122 Uiso 1 1 calc R . . H33B H 0.3169 0.0078 -0.1003 0.122 Uiso 1 1 calc R . . H33C H 0.1799 0.0292 -0.1040 0.122 Uiso 1 1 calc R . . C34 C 0.3950(17) 0.0723(4) 0.0063(13) 0.085(5) Uani 1 1 d . . . H34A H 0.4452 0.0860 0.0735 0.127 Uiso 1 1 calc R . . H34B H 0.3205 0.0872 -0.0409 0.127 Uiso 1 1 calc R . . H34C H 0.4573 0.0656 -0.0365 0.127 Uiso 1 1 calc R . . C35 C 0.3614(14) -0.0288(3) 0.1610(12) 0.069(4) Uani 1 1 d . . . H35A H 0.4075 -0.0233 0.1045 0.104 Uiso 1 1 calc R . . H35B H 0.2926 -0.0477 0.1322 0.104 Uiso 1 1 calc R . . H35C H 0.4288 -0.0372 0.2305 0.104 Uiso 1 1 calc R . . C36 C 0.2196(13) 0.0001(3) 0.2708(11) 0.063(3) Uani 1 1 d . . . H36A H 0.1785 0.0234 0.2813 0.094 Uiso 1 1 calc R . . H36B H 0.2842 -0.0077 0.3425 0.094 Uiso 1 1 calc R . . H36C H 0.1476 -0.0182 0.2446 0.094 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 Dy1 0.0300(2) 0.0364(3) 0.0347(3) 0.0031(2) 0.00948(19) 0.0044(2) Dy2 0.0320(2) 0.0385(3) 0.0337(3) 0.0025(2) 0.0080(2) 0.0029(2) N1 0.055(6) 0.061(7) 0.094(9) -0.031(6) 0.022(6) -0.018(5) N2 0.061(7) 0.135(12) 0.057(8) -0.017(8) 0.015(6) -0.027(8) N3 0.032(4) 0.053(6) 0.052(6) -0.011(5) 0.007(4) -0.002(4) N4 0.051(6) 0.088(8) 0.052(6) -0.001(6) 0.028(5) 0.011(5) N5 0.032(5) 0.078(7) 0.076(7) 0.005(6) 0.028(5) 0.007(5) N6 0.033(4) 0.044(5) 0.040(5) 0.003(4) 0.016(4) 0.013(4) N7 0.053(5) 0.042(5) 0.059(6) 0.008(5) 0.020(5) 0.021(4) N8 0.032(4) 0.035(5) 0.042(5) 0.004(4) 0.010(4) 0.002(4) N9 0.033(4) 0.038(5) 0.042(5) 0.003(4) 0.010(4) 0.013(4) N10 0.043(5) 0.073(7) 0.057(7) 0.004(5) 0.008(5) 0.024(5) N11 0.045(5) 0.037(5) 0.041(5) -0.001(4) 0.019(4) 0.007(4) N12 0.073(7) 0.049(6) 0.061(7) -0.013(5) 0.035(6) -0.004(5) N13 0.054(6) 0.036(5) 0.064(6) -0.002(4) 0.021(5) 0.009(4) C1 0.068(9) 0.069(10) 0.113(13) 0.042(9) 0.054(10) 0.006(7) C2 0.078(10) 0.052(8) 0.076(10) 0.017(7) 0.018(8) -0.023(7) C3 0.105(12) 0.040(7) 0.093(12) 0.020(7) 0.057(10) 0.010(7) C4 0.081(10) 0.083(11) 0.062(9) 0.037(8) 0.017(8) 0.013(8) C5 0.106(12) 0.070(9) 0.057(9) 0.017(7) 0.053(9) 0.018(9) C6 0.024(5) 0.081(9) 0.054(7) -0.018(6) 0.014(5) -0.011(5) C7 0.083(11) 0.19(2) 0.070(11) 0.055(13) -0.033(9) -0.026(13) C8 0.111(15) 0.28(3) 0.070(12) -0.061(15) 0.045(11) -0.040(17) C9 0.070(9) 0.071(10) 0.183(19) -0.065(11) 0.056(11) -0.024(8) C10 0.072(9) 0.047(8) 0.132(15) -0.007(9) 0.037(10) -0.002(7) C11 0.036(6) 0.046(6) 0.060(8) 0.006(5) 0.016(5) 0.010(5) C12 0.070(9) 0.116(12) 0.046(8) -0.017(8) 0.018(7) 0.019(8) C13 0.087(11) 0.129(15) 0.079(11) 0.012(10) 0.051(9) 0.026(10) C14 0.041(7) 0.135(15) 0.114(13) 0.003(11) 0.037(8) 0.028(8) C15 0.044(7) 0.088(10) 0.080(10) -0.013(8) 0.013(7) -0.027(7) C16 0.024(4) 0.036(5) 0.046(6) 0.007(4) 0.013(4) 0.007(4) C17 0.099(11) 0.035(7) 0.104(12) 0.001(7) 0.041(9) 0.018(7) C18 0.066(8) 0.076(9) 0.066(9) 0.019(7) 0.020(7) 0.034(7) C19 0.066(8) 0.069(9) 0.053(8) -0.010(7) 0.010(7) -0.030(7) C20 0.027(5) 0.087(10) 0.063(8) -0.030(7) 0.007(5) -0.002(6) C21 0.038(6) 0.088(10) 0.052(7) 0.008(7) -0.009(6) 0.003(7) C22 0.050(7) 0.096(11) 0.044(7) -0.020(7) 0.005(6) -0.007(7) C23 0.050(7) 0.059(8) 0.068(9) -0.012(7) 0.004(7) -0.004(6) C24 0.071(8) 0.042(7) 0.081(10) 0.001(6) 0.039(8) -0.005(6) C25 0.074(9) 0.060(8) 0.085(11) 0.035(8) 0.035(8) 0.012(7) C26 0.095(11) 0.057(8) 0.064(9) 0.003(7) 0.042(8) -0.013(7) C27 0.055(8) 0.048(7) 0.079(10) 0.004(6) 0.031(7) -0.011(6) C28 0.049(7) 0.056(8) 0.073(9) -0.004(7) 0.014(7) -0.013(6) C29 0.030(5) 0.035(5) 0.038(6) 0.001(4) 0.002(4) 0.007(4) C30 0.045(7) 0.070(9) 0.099(11) -0.010(8) 0.015(7) 0.018(6) C31 0.051(7) 0.118(12) 0.053(8) 0.008(8) -0.003(6) 0.024(8) C32 0.037(5) 0.041(6) 0.056(7) -0.003(5) 0.015(5) 0.004(5) C33 0.107(12) 0.068(10) 0.075(10) -0.021(8) 0.036(9) -0.008(8) C34 0.121(13) 0.067(9) 0.092(11) -0.015(8) 0.069(11) -0.005(9) C35 0.080(9) 0.041(7) 0.084(9) -0.005(7) 0.021(7) 0.018(7) C36 0.077(9) 0.040(7) 0.075(9) 0.011(6) 0.030(7) -0.003(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Dy1 N3 2.178(8) . ? Dy1 N9 2.272(8) . ? Dy1 N8 2.395(8) . ? Dy1 N6 2.506(7) . ? Dy1 C4 2.714(12) . ? Dy1 C5 2.726(11) . ? Dy1 C3 2.731(12) . ? Dy1 C1 2.758(12) . ? Dy1 C2 2.773(12) . ? Dy1 C16 2.839(9) . ? Dy1 Dy2 3.6517(15) . ? Dy2 N8 2.282(8) . ? Dy2 N9 2.369(8) . ? Dy2 N11 2.660(8) . ? Dy2 C28 2.707(11) . ? Dy2 C24 2.709(11) . ? Dy2 C26 2.714(12) . ? Dy2 C20 2.716(10) . ? Dy2 C27 2.718(11) . ? Dy2 C25 2.723(11) . ? Dy2 C19 2.726(11) . ? Dy2 C22 2.732(11) . ? Dy2 C23 2.735(12) . ? N1 C10 1.403(17) . ? N1 C6 1.406(16) . ? N1 C9 1.440(15) . ? N2 C6 1.406(16) . ? N2 C7 1.41(2) . ? N2 C8 1.479(19) . ? N3 C6 1.253(13) . ? N4 C11 1.363(14) . ? N4 C13 1.447(16) . ? N4 C12 1.460(16) . ? N5 C11 1.376(13) . ? N5 C15 1.435(15) . ? N5 C14 1.463(14) . ? N6 C11 1.301(12) . ? N6 C16 1.425(12) . ? N7 C16 1.409(12) . ? N7 C18 1.423(14) . ? N7 C17 1.444(14) . ? N8 C16 1.269(11) . ? N9 C29 1.293(11) . ? N10 C29 1.392(12) . ? N10 C31 1.440(15) . ? N10 C30 1.443(14) . ? N11 C32 1.307(12) . ? N11 C29 1.411(12) . ? N12 C32 1.362(14) . ? N12 C34 1.456(15) . ? N12 C33 1.479(15) . ? N13 C32 1.349(13) . ? N13 C35 1.454(13) . ? N13 C36 1.465(14) . ? C1 C5 1.377(19) . ? C1 C2 1.385(19) . ? C1 H1A 0.9300 . ? C2 C3 1.370(18) . ? C2 H2A 0.9300 . ? C3 C4 1.372(19) . ? C3 H3A 0.9300 . ? C4 C5 1.385(18) . ? C4 H4A 0.9300 . ? C5 H5A 0.9300 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C23 1.383(17) . ? C19 C20 1.389(17) . ? C19 H19A 0.9300 . ? C20 C21 1.385(17) . ? C20 H20A 0.9300 . ? C21 C22 1.409(17) . ? C21 H21A 0.9300 . ? C22 C23 1.348(17) . ? C22 H22A 0.9300 . ? C23 H23A 0.9300 . ? C24 C28 1.374(16) . ? C24 C25 1.440(18) . ? C24 H24A 0.9300 . ? C25 C26 1.372(17) . ? C25 H25A 0.9300 . ? C26 C27 1.384(17) . ? C26 H26A 0.9300 . ? C27 C28 1.394(16) . ? C27 H27A 0.9300 . ? C28 H28A 0.9300 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? 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 Dy1 N9 101.8(3) . . ? N3 Dy1 N8 111.8(3) . . ? N9 Dy1 N8 76.6(3) . . ? N3 Dy1 N6 90.7(3) . . ? N9 Dy1 N6 132.4(3) . . ? N8 Dy1 N6 56.2(3) . . ? N3 Dy1 C4 99.0(4) . . ? N9 Dy1 C4 103.6(4) . . ? N8 Dy1 C4 148.5(4) . . ? N6 Dy1 C4 119.7(4) . . ? N3 Dy1 C5 99.7(4) . . ? N9 Dy1 C5 131.2(3) . . ? N8 Dy1 C5 132.5(4) . . ? N6 Dy1 C5 90.2(3) . . ? C4 Dy1 C5 29.5(4) . . ? N3 Dy1 C3 124.7(4) . . ? N9 Dy1 C3 84.1(4) . . ? N8 Dy1 C3 122.8(4) . . ? N6 Dy1 C3 125.3(4) . . ? C4 Dy1 C3 29.2(4) . . ? C5 Dy1 C3 48.0(4) . . ? N3 Dy1 C1 125.7(5) . . ? N9 Dy1 C1 124.9(4) . . ? N8 Dy1 C1 105.2(4) . . ? N6 Dy1 C1 78.2(4) . . ? C4 Dy1 C1 48.3(4) . . ? C5 Dy1 C1 29.1(4) . . ? C3 Dy1 C1 47.8(4) . . ? N3 Dy1 C2 145.9(4) . . ? N9 Dy1 C2 95.9(4) . . ? N8 Dy1 C2 100.5(4) . . ? N6 Dy1 C2 98.7(4) . . ? C4 Dy1 C2 48.0(4) . . ? C5 Dy1 C2 47.9(4) . . ? C3 Dy1 C2 28.8(4) . . ? C1 Dy1 C2 29.0(4) . . ? N3 Dy1 C16 100.7(3) . . ? N9 Dy1 C16 102.3(3) . . ? N8 Dy1 C16 26.4(3) . . ? N6 Dy1 C16 30.1(3) . . ? C4 Dy1 C16 143.2(4) . . ? C5 Dy1 C16 115.9(4) . . ? C3 Dy1 C16 132.1(4) . . ? C1 Dy1 C16 95.2(4) . . ? C2 Dy1 C16 103.7(4) . . ? N3 Dy1 Dy2 111.4(2) . . ? N9 Dy1 Dy2 39.07(19) . . ? N8 Dy1 Dy2 37.58(19) . . ? N6 Dy1 Dy2 93.54(19) . . ? C4 Dy1 Dy2 134.6(4) . . ? C5 Dy1 Dy2 148.5(3) . . ? C3 Dy1 Dy2 106.8(3) . . ? C1 Dy1 Dy2 122.1(4) . . ? C2 Dy1 Dy2 100.7(3) . . ? C16 Dy1 Dy2 63.4(2) . . ? N8 Dy2 N9 77.0(3) . . ? N8 Dy2 N11 131.6(3) . . ? N9 Dy2 N11 54.9(3) . . ? N8 Dy2 C28 90.2(3) . . ? N9 Dy2 C28 85.9(3) . . ? N11 Dy2 C28 91.3(3) . . ? N8 Dy2 C24 76.8(3) . . ? N9 Dy2 C24 107.9(4) . . ? N11 Dy2 C24 119.7(3) . . ? C28 Dy2 C24 29.4(3) . . ? N8 Dy2 C26 124.9(4) . . ? N9 Dy2 C26 124.3(4) . . ? N11 Dy2 C26 90.4(4) . . ? C28 Dy2 C26 49.1(4) . . ? C24 Dy2 C26 49.2(4) . . ? N8 Dy2 C20 76.6(3) . . ? N9 Dy2 C20 119.5(4) . . ? N11 Dy2 C20 120.5(3) . . ? C28 Dy2 C20 146.6(4) . . ? C24 Dy2 C20 117.3(4) . . ? C26 Dy2 C20 115.5(4) . . ? N8 Dy2 C27 119.8(3) . . ? N9 Dy2 C27 95.1(3) . . ? N11 Dy2 C27 73.7(3) . . ? C28 Dy2 C27 29.8(3) . . ? C24 Dy2 C27 48.7(4) . . ? C26 Dy2 C27 29.5(4) . . ? C20 Dy2 C27 145.0(4) . . ? N8 Dy2 C25 97.8(4) . . ? N9 Dy2 C25 135.4(4) . . ? N11 Dy2 C25 119.0(3) . . ? C28 Dy2 C25 49.5(4) . . ? C24 Dy2 C25 30.7(4) . . ? C26 Dy2 C25 29.2(4) . . ? C20 Dy2 C25 101.5(4) . . ? C27 Dy2 C25 48.8(4) . . ? N8 Dy2 C19 87.4(4) . . ? N9 Dy2 C19 96.5(4) . . ? N11 Dy2 C19 92.6(4) . . ? C28 Dy2 C19 176.1(4) . . ? C24 Dy2 C19 146.8(4) . . ? C26 Dy2 C19 130.6(4) . . ? C20 Dy2 C19 29.6(4) . . ? C27 Dy2 C19 152.3(4) . . ? C25 Dy2 C19 127.9(4) . . ? N8 Dy2 C22 124.8(3) . . ? N9 Dy2 C22 129.7(4) . . ? N11 Dy2 C22 87.7(3) . . ? C28 Dy2 C22 132.0(4) . . ? C24 Dy2 C22 120.5(4) . . ? C26 Dy2 C22 82.8(4) . . ? C20 Dy2 C22 48.4(4) . . ? C27 Dy2 C22 106.2(4) . . ? C25 Dy2 C22 90.1(5) . . ? C19 Dy2 C22 48.1(4) . . ? N8 Dy2 C23 116.7(3) . . ? N9 Dy2 C23 102.4(4) . . ? N11 Dy2 C23 73.6(3) . . ? C28 Dy2 C23 152.9(4) . . ? C24 Dy2 C23 149.0(4) . . ? C26 Dy2 C23 107.4(4) . . ? C20 Dy2 C23 48.3(4) . . ? C27 Dy2 C23 123.2(4) . . ? C25 Dy2 C23 118.6(5) . . ? C19 Dy2 C23 29.3(4) . . ? C22 Dy2 C23 28.5(4) . . ? C10 N1 C6 118.5(10) . . ? C10 N1 C9 112.9(13) . . ? C6 N1 C9 122.8(12) . . ? C6 N2 C7 115.6(12) . . ? C6 N2 C8 116.9(14) . . ? C7 N2 C8 109.8(15) . . ? C6 N3 Dy1 162.0(8) . . ? C11 N4 C13 121.6(12) . . ? C11 N4 C12 118.7(9) . . ? C13 N4 C12 114.6(11) . . ? C11 N5 C15 122.3(9) . . ? C11 N5 C14 121.3(11) . . ? C15 N5 C14 114.9(10) . . ? C11 N6 C16 123.7(8) . . ? C11 N6 Dy1 134.1(7) . . ? C16 N6 Dy1 88.0(5) . . ? C16 N7 C18 120.1(9) . . ? C16 N7 C17 123.2(10) . . ? C18 N7 C17 116.4(10) . . ? C16 N8 Dy2 156.3(7) . . ? C16 N8 Dy1 96.7(6) . . ? Dy2 N8 Dy1 102.6(3) . . ? C29 N9 Dy1 155.9(7) . . ? C29 N9 Dy2 100.3(6) . . ? Dy1 N9 Dy2 103.8(3) . . ? C29 N10 C31 118.5(9) . . ? C29 N10 C30 124.5(10) . . ? C31 N10 C30 116.8(10) . . ? C32 N11 C29 123.7(9) . . ? C32 N11 Dy2 133.9(7) . . ? C29 N11 Dy2 84.8(5) . . ? C32 N12 C34 118.6(10) . . ? C32 N12 C33 122.5(10) . . ? C34 N12 C33 114.1(11) . . ? C32 N13 C35 122.9(10) . . ? C32 N13 C36 121.3(9) . . ? C35 N13 C36 115.1(10) . . ? C5 C1 C2 107.8(13) . . ? C5 C1 Dy1 74.2(7) . . ? C2 C1 Dy1 76.1(7) . . ? C5 C1 H1A 126.1 . . ? C2 C1 H1A 126.1 . . ? Dy1 C1 H1A 115.8 . . ? C3 C2 C1 107.6(14) . . ? C3 C2 Dy1 73.9(7) . . ? C1 C2 Dy1 74.9(7) . . ? C3 C2 H2A 126.2 . . ? C1 C2 H2A 126.2 . . ? Dy1 C2 H2A 117.1 . . ? C2 C3 C4 109.1(13) . . ? C2 C3 Dy1 77.3(7) . . ? C4 C3 Dy1 74.7(8) . . ? C2 C3 H3A 125.5 . . ? C4 C3 H3A 125.5 . . ? Dy1 C3 H3A 114.6 . . ? C3 C4 C5 107.3(13) . . ? C3 C4 Dy1 76.1(7) . . ? C5 C4 Dy1 75.8(7) . . ? C3 C4 H4A 126.4 . . ? C5 C4 H4A 126.4 . . ? Dy1 C4 H4A 114.2 . . ? C1 C5 C4 108.2(13) . . ? C1 C5 Dy1 76.7(7) . . ? C4 C5 Dy1 74.7(7) . . ? C1 C5 H5A 125.9 . . ? C4 C5 H5A 125.9 . . ? Dy1 C5 H5A 114.9 . . ? N3 C6 N2 123.8(13) . . ? N3 C6 N1 123.3(11) . . ? N2 C6 N1 112.9(11) . . ? N2 C7 H7A 109.5 . . ? N2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N2 C8 H8A 109.5 . . ? N2 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N2 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 C10 H10A 109.5 . . ? N1 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N1 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N6 C11 N4 117.7(10) . . ? N6 C11 N5 125.3(11) . . ? N4 C11 N5 116.9(10) . . ? N4 C12 H12A 109.5 . . ? N4 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N4 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N4 C13 H13A 109.5 . . ? N4 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N4 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N5 C14 H14A 109.5 . . ? N5 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N5 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N5 C15 H15A 109.5 . . ? N5 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N5 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N8 C16 N7 126.4(9) . . ? N8 C16 N6 118.0(8) . . ? N7 C16 N6 115.4(8) . . ? N8 C16 Dy1 56.9(5) . . ? N7 C16 Dy1 166.8(7) . . ? N6 C16 Dy1 61.9(4) . . ? N7 C17 H17A 109.5 . . ? N7 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? N7 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? N7 C18 H18A 109.5 . . ? N7 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N7 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C23 C19 C20 107.0(12) . . ? C23 C19 Dy2 75.7(7) . . ? C20 C19 Dy2 74.8(7) . . ? C23 C19 H19A 126.5 . . ? C20 C19 H19A 126.5 . . ? Dy2 C19 H19A 115.4 . . ? C21 C20 C19 108.9(11) . . ? C21 C20 Dy2 76.2(6) . . ? C19 C20 Dy2 75.6(6) . . ? C21 C20 H20A 125.5 . . ? C19 C20 H20A 125.5 . . ? Dy2 C20 H20A 114.8 . . ? C20 C21 C22 106.0(12) . . ? C20 C21 Dy2 74.4(6) . . ? C22 C21 Dy2 74.8(6) . . ? C20 C21 H21A 127.0 . . ? C22 C21 H21A 127.0 . . ? Dy2 C21 H21A 116.2 . . ? C23 C22 C21 109.0(12) . . ? C23 C22 Dy2 75.9(7) . . ? C21 C22 Dy2 75.3(7) . . ? C23 C22 H22A 125.5 . . ? C21 C22 H22A 125.5 . . ? Dy2 C22 H22A 115.4 . . ? C22 C23 C19 109.1(12) . . ? C22 C23 Dy2 75.6(7) . . ? C19 C23 Dy2 75.0(7) . . ? C22 C23 H23A 125.5 . . ? C19 C23 H23A 125.5 . . ? Dy2 C23 H23A 116.0 . . ? C28 C24 C25 107.8(12) . . ? C28 C24 Dy2 75.2(7) . . ? C25 C24 Dy2 75.2(7) . . ? C28 C24 H24A 126.1 . . ? C25 C24 H24A 126.1 . . ? Dy2 C24 H24A 115.7 . . ? C26 C25 C24 106.7(12) . . ? C26 C25 Dy2 75.0(7) . . ? C24 C25 Dy2 74.1(6) . . ? C26 C25 H25A 126.7 . . ? C24 C25 H25A 126.7 . . ? Dy2 C25 H25A 116.5 . . ? C25 C26 C27 109.1(13) . . ? C25 C26 Dy2 75.8(7) . . ? C27 C26 Dy2 75.4(7) . . ? C25 C26 H26A 125.4 . . ? C27 C26 H26A 125.4 . . ? Dy2 C26 H26A 115.4 . . ? C26 C27 C28 108.4(12) . . ? C26 C27 Dy2 75.1(7) . . ? C28 C27 Dy2 74.7(6) . . ? C26 C27 H27A 125.8 . . ? C28 C27 H27A 125.8 . . ? Dy2 C27 H27A 116.5 . . ? C24 C28 C27 108.0(12) . . ? C24 C28 Dy2 75.4(7) . . ? C27 C28 Dy2 75.5(7) . . ? C24 C28 H28A 126.0 . . ? C27 C28 H28A 126.0 . . ? Dy2 C28 H28A 115.3 . . ? N9 C29 N10 123.3(9) . . ? N9 C29 N11 119.1(8) . . ? N10 C29 N11 117.0(9) . . ? N9 C29 Dy2 53.6(5) . . ? N10 C29 Dy2 164.4(7) . . ? N11 C29 Dy2 66.2(5) . . ? N10 C30 H30A 109.5 . . ? N10 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? N10 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? N10 C31 H31A 109.5 . . ? N10 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? N10 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? N11 C32 N13 126.6(10) . . ? N11 C32 N12 117.7(10) . . ? N13 C32 N12 115.7(10) . . ? N12 C33 H33A 109.5 . . ? N12 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? N12 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? N12 C34 H34A 109.5 . . ? N12 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? N12 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N13 C35 H35A 109.5 . . ? N13 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? N13 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? N13 C36 H36A 109.5 . . ? N13 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? N13 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.714 _refine_diff_density_min -3.176 _refine_diff_density_rms 0.131 data_f90115a _database_code_depnum_ccdc_archive 'CCDC 800248' #TrackingRef 'f90115a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C51 H120 N31 Y3' _chemical_formula_weight 1434.51 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 31.010(12) _cell_length_b 13.292(5) _cell_length_c 19.176(7) _cell_angle_alpha 90.00 _cell_angle_beta 101.978(6) _cell_angle_gamma 90.00 _cell_volume 7732(5) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 800 _cell_measurement_theta_min 2.686 _cell_measurement_theta_max 24.295 _exptl_crystal_description sheet _exptl_crystal_colour colorless _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.03 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.232 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3040 _exptl_absorpt_coefficient_mu 2.285 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8383 _exptl_absorpt_correction_T_max 0.9346 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15541 _diffrn_reflns_av_R_equivalents 0.0819 _diffrn_reflns_av_sigmaI/netI 0.1651 _diffrn_reflns_limit_h_min -36 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.34 _diffrn_reflns_theta_max 25.01 _reflns_number_total 6801 _reflns_number_gt 2747 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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. ; _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^)+(0.0159P)^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 6801 _refine_ls_number_parameters 385 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1375 _refine_ls_R_factor_gt 0.0475 _refine_ls_wR_factor_ref 0.0846 _refine_ls_wR_factor_gt 0.0777 _refine_ls_goodness_of_fit_ref 0.976 _refine_ls_restrained_S_all 0.976 _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 Y1 Y 0.0000 0.18355(5) 0.2500 0.0554(3) Uani 1 2 d S . . Y2 Y 0.110941(19) 0.27798(4) 0.26136(3) 0.05669(19) Uani 1 1 d . . . N1 N 0.06536(14) 0.1976(3) 0.3312(2) 0.0520(13) Uani 1 1 d . . . N2 N 0.09066(17) 0.1390(4) 0.4486(3) 0.0771(15) Uani 1 1 d . . . N3 N 0.14092(19) 0.2013(3) 0.3807(2) 0.0582(13) Uani 1 1 d . . . N4 N 0.17023(19) 0.0382(5) 0.4057(3) 0.0876(17) Uani 1 1 d . . . N5 N 0.2149(2) 0.1756(5) 0.4074(2) 0.0795(16) Uani 1 1 d . . . N6 N 0.0000 0.0208(5) 0.2500 0.071(2) Uani 1 2 d S . . N7 N 0.02632(17) -0.1346(4) 0.2137(3) 0.0804(16) Uani 1 1 d . . . N8 N 0.04463(13) 0.2650(3) 0.1824(2) 0.0514(12) Uani 1 1 d . . . N9 N 0.00632(18) 0.3803(4) 0.0974(3) 0.0764(15) Uani 1 1 d . . . N10 N 0.05127(16) 0.2618(4) 0.0618(2) 0.0735(15) Uani 1 1 d . . . N11 N 0.16266(16) 0.2034(3) 0.2187(2) 0.0687(15) Uani 1 1 d . . . N12 N 0.19952(18) 0.0787(4) 0.1659(2) 0.0766(15) Uani 1 1 d . . . N13 N 0.21985(18) 0.2441(4) 0.1598(3) 0.0961(19) Uani 1 1 d . . . N14 N 0.12229(15) 0.4370(4) 0.2747(2) 0.0813(17) Uani 1 1 d . . . N15 N 0.13957(19) 0.5855(5) 0.3401(4) 0.1009(19) Uani 1 1 d . . . N16 N 0.12228(19) 0.5959(4) 0.2184(4) 0.0971(19) Uani 1 1 d . . . C1 C 0.0971(2) 0.1795(4) 0.3843(3) 0.0596(18) Uani 1 1 d . . . C2 C 0.0470(2) 0.1037(4) 0.4532(3) 0.095(2) Uani 1 1 d . . . H2A H 0.0294 0.0956 0.4061 0.143 Uiso 1 1 calc R . . H2B H 0.0333 0.1520 0.4789 0.143 Uiso 1 1 calc R . . H2C H 0.0494 0.0403 0.4777 0.143 Uiso 1 1 calc R . . C3 C 0.1218(2) 0.1554(5) 0.5159(3) 0.113(2) Uani 1 1 d . . . H3A H 0.1493 0.1790 0.5066 0.169 Uiso 1 1 calc R . . H3B H 0.1265 0.0933 0.5420 0.169 Uiso 1 1 calc R . . H3C H 0.1100 0.2046 0.5436 0.169 Uiso 1 1 calc R . . C4 C 0.1736(3) 0.1391(6) 0.3973(3) 0.0631(18) Uani 1 1 d . . . C5 C 0.1332(2) -0.0190(4) 0.3690(3) 0.105(2) Uani 1 1 d . . . H5A H 0.1154 0.0222 0.3330 0.158 Uiso 1 1 calc R . . H5B H 0.1159 -0.0408 0.4023 0.158 Uiso 1 1 calc R . . H5C H 0.1435 -0.0766 0.3470 0.158 Uiso 1 1 calc R . . C6 C 0.2003(2) -0.0161(5) 0.4610(3) 0.138(3) Uani 1 1 d . . . H6A H 0.2244 0.0269 0.4817 0.207 Uiso 1 1 calc R . . H6B H 0.2113 -0.0742 0.4407 0.207 Uiso 1 1 calc R . . H6C H 0.1850 -0.0369 0.4972 0.207 Uiso 1 1 calc R . . C7 C 0.22031(19) 0.2832(5) 0.4101(3) 0.106(2) Uani 1 1 d . . . H7A H 0.1978 0.3128 0.4312 0.159 Uiso 1 1 calc R . . H7B H 0.2179 0.3088 0.3627 0.159 Uiso 1 1 calc R . . H7C H 0.2488 0.2996 0.4383 0.159 Uiso 1 1 calc R . . C8 C 0.2486(2) 0.1244(5) 0.3770(3) 0.127(3) Uani 1 1 d . . . H8A H 0.2433 0.0532 0.3761 0.191 Uiso 1 1 calc R . . H8B H 0.2772 0.1382 0.4057 0.191 Uiso 1 1 calc R . . H8C H 0.2473 0.1482 0.3294 0.191 Uiso 1 1 calc R . . C9 C 0.0000 -0.0728(7) 0.2500 0.062(2) Uani 1 2 d S . . C10 C 0.05638(19) -0.0799(4) 0.1802(3) 0.104(2) Uani 1 1 d . . . H10A H 0.0707 -0.0285 0.2120 0.156 Uiso 1 1 calc R . . H10B H 0.0405 -0.0495 0.1371 0.156 Uiso 1 1 calc R . . H10C H 0.0781 -0.1252 0.1692 0.156 Uiso 1 1 calc R . . C11 C 0.0045(2) -0.2130(5) 0.1691(4) 0.172(4) Uani 1 1 d . . . H11A H -0.0153 -0.2477 0.1933 0.259 Uiso 1 1 calc R . . H11B H 0.0259 -0.2595 0.1585 0.259 Uiso 1 1 calc R . . H11C H -0.0119 -0.1846 0.1256 0.259 Uiso 1 1 calc R . . C12 C 0.03414(19) 0.2996(4) 0.1187(3) 0.0573(16) Uani 1 1 d . . . C13 C -0.00795(19) 0.4383(4) 0.1522(3) 0.099(2) Uani 1 1 d . . . H13A H 0.0151 0.4395 0.1943 0.149 Uiso 1 1 calc R . . H13B H -0.0339 0.4081 0.1632 0.149 Uiso 1 1 calc R . . H13C H -0.0145 0.5058 0.1356 0.149 Uiso 1 1 calc R . . C14 C -0.0276(2) 0.3768(4) 0.0318(3) 0.110(2) Uani 1 1 d . . . H14A H -0.0172 0.3380 -0.0035 0.165 Uiso 1 1 calc R . . H14B H -0.0342 0.4440 0.0144 0.165 Uiso 1 1 calc R . . H14C H -0.0538 0.3463 0.0416 0.165 Uiso 1 1 calc R . . C15 C 0.07410(19) 0.1663(4) 0.0713(3) 0.088(2) Uani 1 1 d . . . H15A H 0.0619 0.1252 0.1035 0.132 Uiso 1 1 calc R . . H15B H 0.1048 0.1776 0.0907 0.132 Uiso 1 1 calc R . . H15C H 0.0708 0.1329 0.0262 0.132 Uiso 1 1 calc R . . C16 C 0.0676(2) 0.3287(4) 0.0140(3) 0.109(2) Uani 1 1 d . . . H16A H 0.0512 0.3904 0.0096 0.163 Uiso 1 1 calc R . . H16B H 0.0643 0.2976 -0.0320 0.163 Uiso 1 1 calc R . . H16C H 0.0982 0.3427 0.0326 0.163 Uiso 1 1 calc R . . C17 C 0.1911(2) 0.1790(5) 0.1852(3) 0.0653(18) Uani 1 1 d . . . C18 C 0.17192(19) 0.0029(4) 0.1875(3) 0.097(2) Uani 1 1 d . . . H18A H 0.1425 0.0284 0.1824 0.145 Uiso 1 1 calc R . . H18B H 0.1832 -0.0146 0.2365 0.145 Uiso 1 1 calc R . . H18C H 0.1716 -0.0557 0.1582 0.145 Uiso 1 1 calc R . . C19 C 0.2437(2) 0.0434(5) 0.1727(3) 0.120(3) Uani 1 1 d . . . H19A H 0.2613 0.0951 0.1575 0.181 Uiso 1 1 calc R . . H19B H 0.2438 -0.0152 0.1435 0.181 Uiso 1 1 calc R . . H19C H 0.2556 0.0266 0.2215 0.181 Uiso 1 1 calc R . . C20 C 0.2211(2) 0.2406(5) 0.0858(3) 0.147(3) Uani 1 1 d . . . H20A H 0.2218 0.1718 0.0710 0.221 Uiso 1 1 calc R . . H20B H 0.2470 0.2747 0.0781 0.221 Uiso 1 1 calc R . . H20C H 0.1953 0.2729 0.0587 0.221 Uiso 1 1 calc R . . C21 C 0.2188(2) 0.3445(5) 0.1845(4) 0.168(4) Uani 1 1 d . . . H21A H 0.2187 0.3440 0.2346 0.252 Uiso 1 1 calc R . . H21B H 0.1927 0.3774 0.1591 0.252 Uiso 1 1 calc R . . H21C H 0.2443 0.3800 0.1768 0.252 Uiso 1 1 calc R . . C22 C 0.12665(19) 0.5296(6) 0.2777(4) 0.073(2) Uani 1 1 d . . . C23 C 0.1486(2) 0.5277(5) 0.4053(3) 0.123(3) Uani 1 1 d . . . H23A H 0.1662 0.4703 0.3994 0.185 Uiso 1 1 calc R . . H23B H 0.1213 0.5057 0.4164 0.185 Uiso 1 1 calc R . . H23C H 0.1642 0.5689 0.4435 0.185 Uiso 1 1 calc R . . C24 C 0.1162(3) 0.6755(5) 0.3461(4) 0.187(4) Uani 1 1 d . . . H24A H 0.1120 0.7120 0.3020 0.280 Uiso 1 1 calc R . . H24B H 0.1327 0.7160 0.3838 0.280 Uiso 1 1 calc R . . H24C H 0.0880 0.6595 0.3566 0.280 Uiso 1 1 calc R . . C25 C 0.1541(3) 0.6700(6) 0.2123(4) 0.170(4) Uani 1 1 d . . . H25A H 0.1644 0.7014 0.2578 0.255 Uiso 1 1 calc R . . H25B H 0.1410 0.7198 0.1782 0.255 Uiso 1 1 calc R . . H25C H 0.1784 0.6390 0.1968 0.255 Uiso 1 1 calc R . . C26 C 0.1070(3) 0.5503(5) 0.1502(4) 0.158(3) Uani 1 1 d . . . H26A H 0.0855 0.4998 0.1537 0.237 Uiso 1 1 calc R . . H26B H 0.1314 0.5199 0.1344 0.237 Uiso 1 1 calc R . . H26C H 0.0939 0.6007 0.1165 0.237 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 Y1 0.0657(7) 0.0531(6) 0.0500(5) 0.000 0.0184(5) 0.000 Y2 0.0677(4) 0.0483(3) 0.0555(3) 0.0028(3) 0.0161(3) -0.0002(3) N1 0.055(3) 0.049(3) 0.051(3) 0.006(2) 0.008(3) -0.002(2) N2 0.069(4) 0.097(4) 0.065(4) 0.021(3) 0.015(3) 0.000(3) N3 0.054(4) 0.068(4) 0.053(3) 0.001(3) 0.011(3) 0.000(3) N4 0.105(6) 0.064(5) 0.091(4) 0.002(4) 0.012(4) 0.017(4) N5 0.060(5) 0.096(5) 0.076(4) 0.003(4) 0.000(3) 0.005(4) N6 0.099(6) 0.047(5) 0.066(5) 0.000 0.015(4) 0.000 N7 0.101(5) 0.054(4) 0.098(4) -0.025(3) 0.048(4) -0.013(3) N8 0.064(3) 0.046(3) 0.045(3) 0.008(2) 0.013(2) -0.002(2) N9 0.098(5) 0.067(4) 0.066(4) 0.011(3) 0.020(3) 0.021(3) N10 0.105(4) 0.070(4) 0.052(3) 0.007(3) 0.030(3) 0.006(3) N11 0.067(4) 0.078(4) 0.065(3) -0.006(3) 0.022(3) 0.001(3) N12 0.068(4) 0.065(4) 0.103(4) -0.003(3) 0.031(3) -0.009(3) N13 0.130(5) 0.081(5) 0.096(4) -0.031(4) 0.068(4) -0.041(4) N14 0.101(5) 0.041(3) 0.105(4) -0.003(3) 0.030(3) -0.008(3) N15 0.104(5) 0.069(5) 0.132(6) -0.024(5) 0.031(4) 0.023(4) N16 0.105(5) 0.070(5) 0.114(5) 0.005(4) 0.018(4) -0.033(4) C1 0.088(6) 0.045(4) 0.048(4) 0.009(3) 0.018(4) 0.006(4) C2 0.123(7) 0.103(5) 0.063(4) 0.030(4) 0.026(4) 0.013(5) C3 0.132(6) 0.161(7) 0.041(4) 0.005(4) 0.005(4) 0.028(5) C4 0.070(6) 0.074(6) 0.042(4) -0.002(4) 0.004(4) 0.019(5) C5 0.142(7) 0.061(5) 0.115(6) -0.002(4) 0.033(5) 0.001(5) C6 0.171(8) 0.098(6) 0.130(6) 0.033(5) -0.001(6) 0.063(6) C7 0.094(6) 0.111(7) 0.099(5) 0.009(5) -0.009(4) -0.026(5) C8 0.076(6) 0.181(8) 0.127(6) -0.015(5) 0.027(5) 0.032(6) C9 0.070(7) 0.061(7) 0.053(6) 0.000 0.006(5) 0.000 C10 0.106(6) 0.105(6) 0.118(5) -0.008(4) 0.061(5) -0.018(5) C11 0.180(9) 0.134(7) 0.235(9) -0.117(7) 0.116(7) -0.061(6) C12 0.060(5) 0.045(4) 0.065(4) 0.000(4) 0.011(4) 0.001(3) C13 0.121(6) 0.072(5) 0.111(5) 0.027(4) 0.038(5) 0.032(4) C14 0.122(6) 0.098(6) 0.095(5) 0.033(4) -0.013(5) 0.010(5) C15 0.108(6) 0.083(5) 0.076(4) -0.013(4) 0.027(4) 0.013(4) C16 0.159(7) 0.106(5) 0.075(5) 0.006(4) 0.056(5) -0.023(5) C17 0.073(6) 0.056(5) 0.067(4) -0.013(4) 0.015(4) -0.012(4) C18 0.103(6) 0.078(5) 0.108(5) -0.002(4) 0.016(4) -0.003(5) C19 0.098(6) 0.139(7) 0.131(6) -0.024(5) 0.039(5) 0.031(6) C20 0.212(9) 0.129(7) 0.126(6) -0.014(5) 0.094(6) -0.059(6) C21 0.244(10) 0.092(6) 0.206(8) -0.061(6) 0.131(8) -0.081(6) C22 0.068(5) 0.067(6) 0.090(6) 0.000(6) 0.034(4) 0.008(4) C23 0.148(7) 0.130(7) 0.087(5) -0.024(5) 0.011(5) 0.031(5) C24 0.292(13) 0.093(7) 0.208(9) -0.028(6) 0.128(9) 0.025(7) C25 0.151(9) 0.182(9) 0.175(8) 0.068(7) 0.026(7) -0.027(7) C26 0.204(10) 0.125(8) 0.140(8) 0.040(6) 0.027(7) -0.018(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 Y1 N6 2.163(7) . ? Y1 N1 2.293(4) 2 ? Y1 N1 2.293(4) . ? Y1 N8 2.348(4) 2 ? Y1 N8 2.348(4) . ? Y1 Y2 3.6258(14) 2 ? Y1 Y2 3.6259(14) . ? Y2 N14 2.149(5) . ? Y2 N11 2.184(5) . ? Y2 N8 2.293(4) . ? Y2 N1 2.392(4) . ? Y2 N3 2.501(4) . ? Y2 C1 2.806(6) . ? N1 C1 1.283(6) . ? N2 C1 1.399(6) . ? N2 C2 1.452(6) . ? N2 C3 1.458(6) . ? N3 C4 1.295(6) . ? N3 C1 1.405(6) . ? N4 C4 1.358(7) . ? N4 C5 1.434(6) . ? N4 C6 1.450(6) . ? N5 C4 1.346(7) . ? N5 C7 1.439(6) . ? N5 C8 1.465(6) . ? N6 C9 1.245(8) . ? N7 C11 1.427(7) . ? N7 C10 1.434(6) . ? N7 C9 1.435(6) . ? N8 C12 1.283(6) . ? N9 C12 1.383(6) . ? N9 C13 1.446(6) . ? N9 C14 1.463(6) . ? N10 C12 1.402(6) . ? N10 C16 1.442(5) . ? N10 C15 1.446(6) . ? N11 C17 1.236(6) . ? N12 C17 1.422(6) . ? N12 C19 1.428(6) . ? N12 C18 1.438(6) . ? N13 C17 1.402(6) . ? N13 C21 1.419(6) . ? N13 C20 1.428(6) . ? N14 C22 1.238(7) . ? N15 C22 1.395(7) . ? N15 C24 1.416(7) . ? N15 C23 1.444(7) . ? N16 C25 1.415(7) . ? N16 C22 1.422(7) . ? N16 C26 1.431(7) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 N7 1.435(6) 2 ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 H16A 0.9600 . ? C16 H16B 0.9600 . ? C16 H16C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? 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 Y1 N1 94.67(10) . 2 ? N6 Y1 N1 94.67(10) . . ? N1 Y1 N1 170.67(19) 2 . ? N6 Y1 N8 117.45(9) . 2 ? N1 Y1 N8 78.37(14) 2 2 ? N1 Y1 N8 97.27(14) . 2 ? N6 Y1 N8 117.46(9) . . ? N1 Y1 N8 97.27(14) 2 . ? N1 Y1 N8 78.37(14) . . ? N8 Y1 N8 125.09(19) 2 . ? N6 Y1 Y2 110.253(17) . 2 ? N1 Y1 Y2 40.29(10) 2 2 ? N1 Y1 Y2 134.95(10) . 2 ? N8 Y1 Y2 38.09(10) 2 2 ? N8 Y1 Y2 117.89(10) . 2 ? N6 Y1 Y2 110.253(17) . . ? N1 Y1 Y2 134.95(10) 2 . ? N1 Y1 Y2 40.29(10) . . ? N8 Y1 Y2 117.89(10) 2 . ? N8 Y1 Y2 38.09(10) . . ? Y2 Y1 Y2 139.49(3) 2 . ? N14 Y2 N11 112.10(17) . . ? N14 Y2 N8 104.78(16) . . ? N11 Y2 N8 110.26(16) . . ? N14 Y2 N1 118.27(15) . . ? N11 Y2 N1 124.91(15) . . ? N8 Y2 N1 77.47(14) . . ? N14 Y2 N3 105.71(16) . . ? N11 Y2 N3 89.73(17) . . ? N8 Y2 N3 133.28(15) . . ? N1 Y2 N3 57.05(15) . . ? N14 Y2 C1 114.09(16) . . ? N11 Y2 C1 110.81(17) . . ? N8 Y2 C1 104.30(18) . . ? N1 Y2 C1 27.10(15) . . ? N3 Y2 C1 30.01(14) . . ? N14 Y2 Y1 118.52(13) . . ? N11 Y2 Y1 125.58(12) . . ? N8 Y2 Y1 39.17(10) . . ? N1 Y2 Y1 38.31(10) . . ? N3 Y2 Y1 94.69(12) . . ? C1 Y2 Y1 65.18(15) . . ? C1 N1 Y1 161.4(4) . . ? C1 N1 Y2 94.7(4) . . ? Y1 N1 Y2 101.40(16) . . ? C1 N2 C2 118.9(5) . . ? C1 N2 C3 122.3(5) . . ? C2 N2 C3 116.6(5) . . ? C4 N3 C1 124.8(6) . . ? C4 N3 Y2 127.5(4) . . ? C1 N3 Y2 87.1(3) . . ? C4 N4 C5 122.6(6) . . ? C4 N4 C6 121.6(6) . . ? C5 N4 C6 115.0(6) . . ? C4 N5 C7 117.6(6) . . ? C4 N5 C8 120.8(6) . . ? C7 N5 C8 112.9(6) . . ? C9 N6 Y1 180.000(1) . . ? C11 N7 C10 112.0(5) . . ? C11 N7 C9 117.5(5) . . ? C10 N7 C9 114.5(5) . . ? C12 N8 Y2 128.1(4) . . ? C12 N8 Y1 129.0(4) . . ? Y2 N8 Y1 102.74(15) . . ? C12 N9 C13 117.7(5) . . ? C12 N9 C14 121.6(5) . . ? C13 N9 C14 111.5(5) . . ? C12 N10 C16 120.8(5) . . ? C12 N10 C15 118.1(5) . . ? C16 N10 C15 113.3(5) . . ? C17 N11 Y2 166.3(5) . . ? C17 N12 C19 120.6(5) . . ? C17 N12 C18 115.4(5) . . ? C19 N12 C18 111.1(5) . . ? C17 N13 C21 113.8(5) . . ? C17 N13 C20 118.4(5) . . ? C21 N13 C20 111.8(6) . . ? C22 N14 Y2 175.3(5) . . ? C22 N15 C24 117.4(7) . . ? C22 N15 C23 115.4(6) . . ? C24 N15 C23 112.9(6) . . ? C25 N16 C22 123.0(6) . . ? C25 N16 C26 108.8(7) . . ? C22 N16 C26 115.3(6) . . ? N1 C1 N2 123.1(6) . . ? N1 C1 N3 120.9(5) . . ? N2 C1 N3 116.0(6) . . ? N1 C1 Y2 58.2(3) . . ? N2 C1 Y2 174.8(4) . . ? N3 C1 Y2 62.9(3) . . ? N2 C2 H2A 109.5 . . ? N2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N3 C4 N5 118.6(7) . . ? N3 C4 N4 125.8(7) . . ? N5 C4 N4 115.6(7) . . ? N4 C5 H5A 109.5 . . ? N4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N4 C6 H6A 109.5 . . ? N4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N5 C7 H7A 109.5 . . ? N5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N5 C8 H8A 109.5 . . ? N5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N6 C9 N7 124.9(4) . 2 ? N6 C9 N7 124.9(4) . . ? N7 C9 N7 110.2(8) 2 . ? N7 C10 H10A 109.5 . . ? N7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N7 C11 H11A 109.5 . . ? N7 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N7 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N8 C12 N9 125.4(6) . . ? N8 C12 N10 123.4(5) . . ? N9 C12 N10 111.2(5) . . ? N9 C13 H13A 109.5 . . ? N9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N9 C14 H14A 109.5 . . ? N9 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N9 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N10 C15 H15A 109.5 . . ? N10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N10 C16 H16A 109.5 . . ? N10 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? N10 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N11 C17 N13 126.3(6) . . ? N11 C17 N12 124.9(6) . . ? N13 C17 N12 108.9(6) . . ? N12 C18 H18A 109.5 . . ? N12 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? N12 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N12 C19 H19A 109.5 . . ? N12 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? N12 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N13 C20 H20A 109.5 . . ? N13 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? N13 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N13 C21 H21A 109.5 . . ? N13 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? N13 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? N14 C22 N15 125.3(7) . . ? N14 C22 N16 126.0(7) . . ? N15 C22 N16 108.5(7) . . ? N15 C23 H23A 109.5 . . ? N15 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? N15 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? N15 C24 H24A 109.5 . . ? N15 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? N15 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N16 C25 H25A 109.5 . . ? N16 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? N16 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N16 C26 H26A 109.5 . . ? N16 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? N16 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.579 _refine_diff_density_min -0.282 _refine_diff_density_rms 0.059 data_f91015a _database_code_depnum_ccdc_archive 'CCDC 800249' #TrackingRef 'f91015a.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H56 N10 Y2' _chemical_formula_weight 806.73 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' Y Y -2.7962 3.5667 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.003(6) _cell_length_b 12.179(5) _cell_length_c 21.055(8) _cell_angle_alpha 90.00 _cell_angle_beta 95.119(5) _cell_angle_gamma 90.00 _cell_volume 3832(2) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 4717 _cell_measurement_theta_min 2.726 _cell_measurement_theta_max 24.211 _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1680 _exptl_absorpt_coefficient_mu 3.053 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4611 _exptl_absorpt_correction_T_max 0.5803 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16973 _diffrn_reflns_av_R_equivalents 0.0649 _diffrn_reflns_av_sigmaI/netI 0.1003 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.36 _diffrn_reflns_theta_max 26.01 _reflns_number_total 7516 _reflns_number_gt 4479 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _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. ; _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^)+(0.0150P)^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 7516 _refine_ls_number_parameters 433 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_gt 0.0414 _refine_ls_wR_factor_ref 0.0683 _refine_ls_wR_factor_gt 0.0640 _refine_ls_goodness_of_fit_ref 0.983 _refine_ls_restrained_S_all 0.983 _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 Y1 Y 0.21795(2) 0.37456(3) 0.131369(17) 0.03048(10) Uani 1 1 d . . . Y2 Y 0.21864(2) 0.67079(3) 0.160721(16) 0.03153(10) Uani 1 1 d . . . N1 N 0.21299(18) 0.5068(2) 0.21383(13) 0.0300(7) Uani 1 1 d . . . N2 N 0.23139(19) 0.3282(2) 0.25014(13) 0.0305(7) Uani 1 1 d . . . N3 N 0.18076(19) 0.4623(2) 0.31967(14) 0.0408(8) Uani 1 1 d . . . N4 N 0.2829(2) 0.1613(2) 0.29010(13) 0.0409(8) Uani 1 1 d . . . N5 N 0.3501(2) 0.3175(2) 0.33248(14) 0.0374(8) Uani 1 1 d . . . N6 N 0.22527(17) 0.5394(2) 0.07841(13) 0.0276(7) Uani 1 1 d . . . N7 N 0.25321(18) 0.7162(2) 0.04535(13) 0.0313(7) Uani 1 1 d . . . N8 N 0.21225(19) 0.5807(2) -0.03253(14) 0.0395(8) Uani 1 1 d . . . N9 N 0.3132(2) 0.8824(2) 0.01925(14) 0.0412(8) Uani 1 1 d . . . N10 N 0.38447(19) 0.7260(2) -0.00961(14) 0.0376(8) Uani 1 1 d . . . C1 C 0.2092(2) 0.4404(3) 0.26070(17) 0.0296(9) Uani 1 1 d . . . C2 C 0.1456(3) 0.3789(3) 0.35984(17) 0.0540(12) Uani 1 1 d . . . H2A H 0.1657 0.3078 0.3474 0.081 Uiso 1 1 calc R . . H2B H 0.0814 0.3811 0.3551 0.081 Uiso 1 1 calc R . . H2C H 0.1665 0.3925 0.4036 0.081 Uiso 1 1 calc R . . C3 C 0.1555(3) 0.5727(3) 0.33531(18) 0.0661(14) Uani 1 1 d . . . H3A H 0.1814 0.6236 0.3074 0.099 Uiso 1 1 calc R . . H3B H 0.1768 0.5886 0.3787 0.099 Uiso 1 1 calc R . . H3C H 0.0915 0.5793 0.3303 0.099 Uiso 1 1 calc R . . C4 C 0.2870(3) 0.2737(3) 0.29043(18) 0.0349(9) Uani 1 1 d . . . C5 C 0.2041(3) 0.1060(3) 0.26360(18) 0.0511(11) Uani 1 1 d . . . H5A H 0.1549 0.1567 0.2597 0.077 Uiso 1 1 calc R . . H5B H 0.1905 0.0465 0.2911 0.077 Uiso 1 1 calc R . . H5C H 0.2140 0.0777 0.2223 0.077 Uiso 1 1 calc R . . C6 C 0.3642(3) 0.0947(3) 0.29867(19) 0.0624(13) Uani 1 1 d . . . H6A H 0.4128 0.1390 0.3169 0.094 Uiso 1 1 calc R . . H6B H 0.3783 0.0670 0.2581 0.094 Uiso 1 1 calc R . . H6C H 0.3548 0.0344 0.3266 0.094 Uiso 1 1 calc R . . C7 C 0.3698(3) 0.2733(3) 0.39623(18) 0.0592(12) Uani 1 1 d . . . H7A H 0.3411 0.2032 0.3991 0.089 Uiso 1 1 calc R . . H7B H 0.3480 0.3228 0.4268 0.089 Uiso 1 1 calc R . . H7C H 0.4333 0.2646 0.4049 0.089 Uiso 1 1 calc R . . C8 C 0.3899(3) 0.4226(3) 0.32237(18) 0.0533(11) Uani 1 1 d . . . H8A H 0.3738 0.4461 0.2794 0.080 Uiso 1 1 calc R . . H8B H 0.4538 0.4168 0.3295 0.080 Uiso 1 1 calc R . . H8C H 0.3686 0.4751 0.3515 0.080 Uiso 1 1 calc R . . C9 C 0.2304(2) 0.6043(3) 0.03163(18) 0.0302(9) Uani 1 1 d . . . C10 C 0.1869(3) 0.4711(3) -0.05238(17) 0.0517(11) Uani 1 1 d . . . H10A H 0.2033 0.4206 -0.0183 0.077 Uiso 1 1 calc R . . H10B H 0.2171 0.4515 -0.0891 0.077 Uiso 1 1 calc R . . H10C H 0.1234 0.4682 -0.0630 0.077 Uiso 1 1 calc R . . C11 C 0.1920(3) 0.6645(3) -0.08051(16) 0.0560(12) Uani 1 1 d . . . H11A H 0.2115 0.7347 -0.0638 0.084 Uiso 1 1 calc R . . H11B H 0.1286 0.6664 -0.0919 0.084 Uiso 1 1 calc R . . H11C H 0.2223 0.6479 -0.1176 0.084 Uiso 1 1 calc R . . C12 C 0.2307(3) 0.9384(3) 0.02829(18) 0.0551(12) Uani 1 1 d . . . H12A H 0.1814 0.8884 0.0204 0.083 Uiso 1 1 calc R . . H12B H 0.2232 0.9991 -0.0008 0.083 Uiso 1 1 calc R . . H12C H 0.2324 0.9650 0.0713 0.083 Uiso 1 1 calc R . . C13 C 0.3940(3) 0.9479(3) 0.02992(19) 0.0601(13) Uani 1 1 d . . . H13A H 0.4450 0.9034 0.0230 0.090 Uiso 1 1 calc R . . H13B H 0.3995 0.9747 0.0730 0.090 Uiso 1 1 calc R . . H13C H 0.3909 1.0088 0.0009 0.090 Uiso 1 1 calc R . . C14 C 0.4167(2) 0.6163(3) 0.00532(18) 0.0467(11) Uani 1 1 d . . . H14A H 0.3928 0.5912 0.0435 0.070 Uiso 1 1 calc R . . H14B H 0.4809 0.6170 0.0116 0.070 Uiso 1 1 calc R . . H14C H 0.3979 0.5678 -0.0293 0.070 Uiso 1 1 calc R . . C15 C 0.4169(3) 0.7724(3) -0.06713(18) 0.0570(12) Uani 1 1 d . . . H15A H 0.3931 0.8451 -0.0739 0.085 Uiso 1 1 calc R . . H15B H 0.3980 0.7270 -0.1031 0.085 Uiso 1 1 calc R . . H15C H 0.4811 0.7759 -0.0622 0.085 Uiso 1 1 calc R . . C16 C 0.3154(2) 0.7695(3) 0.01881(17) 0.0351(9) Uani 1 1 d . . . C17 C 0.0883(3) 0.2789(4) 0.0512(2) 0.0552(12) Uani 1 1 d . . . H17A H 0.1044 0.2592 0.0111 0.066 Uiso 1 1 calc R . . C18 C 0.0940(3) 0.2127(3) 0.1051(2) 0.0545(12) Uani 1 1 d . . . H18A H 0.1147 0.1407 0.1074 0.065 Uiso 1 1 calc R . . C19 C 0.0633(2) 0.2721(4) 0.1548(2) 0.0519(12) Uani 1 1 d . . . H19A H 0.0592 0.2471 0.1962 0.062 Uiso 1 1 calc R . . C20 C 0.0398(2) 0.3758(4) 0.1317(2) 0.0514(11) Uani 1 1 d . . . H20A H 0.0179 0.4329 0.1552 0.062 Uiso 1 1 calc R . . C21 C 0.0542(3) 0.3802(4) 0.0680(2) 0.0515(11) Uani 1 1 d . . . H21A H 0.0432 0.4401 0.0411 0.062 Uiso 1 1 calc R . . C22 C 0.3180(3) 0.2406(3) 0.06424(19) 0.0500(12) Uani 1 1 d . . . H22A H 0.2859 0.2014 0.0319 0.060 Uiso 1 1 calc R . . C23 C 0.3378(3) 0.2059(3) 0.1273(2) 0.0566(13) Uani 1 1 d . . . H23A H 0.3201 0.1401 0.1447 0.068 Uiso 1 1 calc R . . C24 C 0.3889(3) 0.2880(4) 0.15942(19) 0.0510(11) Uani 1 1 d . . . H24A H 0.4123 0.2855 0.2018 0.061 Uiso 1 1 calc R . . C25 C 0.3988(2) 0.3733(3) 0.1175(2) 0.0437(10) Uani 1 1 d . . . H25A H 0.4293 0.4386 0.1269 0.052 Uiso 1 1 calc R . . C26 C 0.3553(2) 0.3448(3) 0.05859(19) 0.0426(10) Uani 1 1 d . . . H26A H 0.3517 0.3877 0.0219 0.051 Uiso 1 1 calc R . . C27 C 0.0409(2) 0.6781(3) 0.1247(2) 0.0497(11) Uani 1 1 d . . . H27A H 0.0189 0.6217 0.0980 0.060 Uiso 1 1 calc R . . C28 C 0.0478(3) 0.6764(3) 0.1910(2) 0.0521(11) Uani 1 1 d . . . H28A H 0.0311 0.6189 0.2165 0.063 Uiso 1 1 calc R . . C29 C 0.0843(3) 0.7766(3) 0.2123(2) 0.0552(12) Uani 1 1 d . . . H29A H 0.0965 0.7975 0.2546 0.066 Uiso 1 1 calc R . . C30 C 0.0993(3) 0.8396(3) 0.1593(2) 0.0541(12) Uani 1 1 d . . . H30A H 0.1230 0.9102 0.1599 0.065 Uiso 1 1 calc R . . C31 C 0.0725(3) 0.7786(4) 0.1055(2) 0.0532(12) Uani 1 1 d . . . H31A H 0.0753 0.8012 0.0636 0.064 Uiso 1 1 calc R . . C32 C 0.3448(3) 0.6999(3) 0.26079(19) 0.0560(12) Uani 1 1 d . . . H32A H 0.3366 0.6592 0.2972 0.067 Uiso 1 1 calc R . . C33 C 0.3930(3) 0.6664(3) 0.2110(2) 0.0511(11) Uani 1 1 d . . . H33A H 0.4221 0.5995 0.2080 0.061 Uiso 1 1 calc R . . C34 C 0.3899(3) 0.7503(4) 0.1668(2) 0.0543(12) Uani 1 1 d . . . H34A H 0.4174 0.7506 0.1289 0.065 Uiso 1 1 calc R . . C35 C 0.3382(3) 0.8341(3) 0.1892(2) 0.0535(12) Uani 1 1 d . . . H35A H 0.3242 0.9001 0.1684 0.064 Uiso 1 1 calc R . . C36 C 0.3110(3) 0.8032(3) 0.2474(2) 0.0526(12) Uani 1 1 d . . . H36A H 0.2763 0.8445 0.2730 0.063 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 Y1 0.0322(2) 0.0329(2) 0.0270(2) -0.00248(17) 0.00624(16) -0.00204(17) Y2 0.0321(2) 0.0333(2) 0.0299(2) -0.00307(17) 0.00617(16) 0.00073(17) N1 0.0313(19) 0.0421(19) 0.017(2) -0.0009(15) 0.0034(14) -0.0020(14) N2 0.0334(19) 0.0325(17) 0.0257(18) 0.0007(15) 0.0029(14) -0.0010(15) N3 0.054(2) 0.040(2) 0.032(2) -0.0030(16) 0.0230(17) -0.0033(16) N4 0.044(2) 0.0345(19) 0.043(2) 0.0020(16) -0.0011(16) -0.0007(17) N5 0.041(2) 0.0367(19) 0.034(2) 0.0030(16) -0.0033(15) -0.0049(16) N6 0.0279(18) 0.0343(18) 0.0211(19) 0.0037(14) 0.0046(14) 0.0014(14) N7 0.034(2) 0.0306(17) 0.0304(19) 0.0019(14) 0.0081(15) -0.0009(15) N8 0.050(2) 0.043(2) 0.024(2) 0.0054(16) -0.0032(15) -0.0075(16) N9 0.037(2) 0.0351(19) 0.053(2) 0.0035(17) 0.0134(16) 0.0005(17) N10 0.038(2) 0.0367(19) 0.040(2) 0.0088(15) 0.0152(16) 0.0036(16) C1 0.021(2) 0.040(2) 0.027(2) -0.004(2) 0.0005(17) -0.0029(17) C2 0.058(3) 0.061(3) 0.046(3) 0.005(2) 0.022(2) -0.009(2) C3 0.105(4) 0.055(3) 0.043(3) -0.004(2) 0.032(3) 0.012(3) C4 0.038(3) 0.037(2) 0.032(3) -0.005(2) 0.015(2) -0.006(2) C5 0.057(3) 0.040(3) 0.055(3) 0.005(2) -0.002(2) -0.008(2) C6 0.066(3) 0.047(3) 0.073(4) 0.004(2) 0.000(3) 0.004(2) C7 0.068(3) 0.070(3) 0.038(3) 0.008(2) -0.008(2) -0.010(2) C8 0.052(3) 0.055(3) 0.051(3) -0.004(2) -0.006(2) -0.007(2) C9 0.020(2) 0.038(3) 0.033(3) -0.0053(19) 0.0041(17) 0.0000(17) C10 0.061(3) 0.057(3) 0.037(3) -0.007(2) 0.001(2) -0.011(2) C11 0.069(3) 0.068(3) 0.029(3) 0.010(2) -0.008(2) -0.011(2) C12 0.061(3) 0.037(2) 0.069(3) 0.007(2) 0.013(2) 0.010(2) C13 0.061(3) 0.046(3) 0.075(4) 0.005(2) 0.014(3) -0.006(2) C14 0.040(3) 0.045(2) 0.058(3) 0.003(2) 0.016(2) 0.007(2) C15 0.056(3) 0.067(3) 0.051(3) 0.014(2) 0.022(2) 0.007(2) C16 0.034(3) 0.035(2) 0.036(3) 0.0012(19) 0.0044(19) 0.003(2) C17 0.059(3) 0.070(3) 0.036(3) -0.009(3) 0.001(2) -0.020(3) C18 0.055(3) 0.048(3) 0.060(3) -0.003(3) -0.002(2) -0.018(2) C19 0.037(3) 0.071(3) 0.048(3) 0.010(3) 0.006(2) -0.018(2) C20 0.024(3) 0.064(3) 0.066(3) -0.004(3) 0.000(2) -0.004(2) C21 0.040(3) 0.071(3) 0.041(3) 0.012(2) -0.008(2) -0.004(2) C22 0.062(3) 0.049(3) 0.041(3) -0.013(2) 0.017(2) 0.005(2) C23 0.067(3) 0.040(3) 0.067(4) 0.012(2) 0.031(3) 0.015(2) C24 0.040(3) 0.075(3) 0.039(3) 0.002(3) 0.008(2) 0.023(2) C25 0.032(3) 0.047(2) 0.053(3) -0.008(2) 0.011(2) 0.001(2) C26 0.043(3) 0.045(3) 0.044(3) 0.005(2) 0.024(2) 0.007(2) C27 0.032(3) 0.060(3) 0.058(3) -0.011(3) 0.008(2) 0.007(2) C28 0.039(3) 0.062(3) 0.059(3) 0.008(3) 0.022(2) 0.007(2) C29 0.054(3) 0.063(3) 0.051(3) -0.012(3) 0.019(2) 0.014(2) C30 0.049(3) 0.044(3) 0.071(4) -0.001(3) 0.017(2) 0.009(2) C31 0.037(3) 0.068(3) 0.057(3) 0.012(3) 0.015(2) 0.011(2) C32 0.072(3) 0.060(3) 0.031(3) 0.004(2) -0.017(2) -0.021(3) C33 0.042(3) 0.048(3) 0.061(3) -0.011(3) -0.011(2) 0.002(2) C34 0.035(3) 0.077(3) 0.050(3) -0.012(3) 0.002(2) -0.023(2) C35 0.065(3) 0.038(2) 0.054(3) 0.005(2) -0.012(2) -0.018(2) C36 0.067(3) 0.045(3) 0.045(3) -0.011(2) 0.003(2) -0.006(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 Y1 N6 2.304(3) . ? Y1 N1 2.374(3) . ? Y1 N2 2.554(3) . ? Y1 C20 2.673(4) . ? Y1 C21 2.689(4) . ? Y1 C26 2.700(3) . ? Y1 C22 2.700(3) . ? Y1 C19 2.718(4) . ? Y1 C17 2.721(4) . ? Y1 C18 2.733(4) . ? Y1 C23 2.736(4) . ? Y1 C25 2.755(4) . ? Y2 N1 2.294(3) . ? Y2 N6 2.367(3) . ? Y2 N7 2.589(3) . ? Y2 C28 2.697(4) . ? Y2 C29 2.700(4) . ? Y2 C27 2.708(4) . ? Y2 C35 2.709(4) . ? Y2 C36 2.721(4) . ? Y2 C31 2.725(4) . ? Y2 C30 2.725(4) . ? Y2 C32 2.727(4) . ? Y2 C33 2.733(4) . ? N1 C1 1.281(4) . ? N2 C4 1.316(4) . ? N2 C1 1.428(4) . ? N3 C1 1.375(4) . ? N3 C3 1.443(4) . ? N3 C2 1.451(4) . ? N4 C4 1.370(4) . ? N4 C5 1.430(4) . ? N4 C6 1.463(4) . ? N5 C4 1.348(4) . ? N5 C8 1.436(4) . ? N5 C7 1.452(4) . ? N6 C9 1.270(4) . ? N7 C16 1.303(4) . ? N7 C9 1.429(4) . ? N8 C9 1.384(4) . ? N8 C10 1.439(4) . ? N8 C11 1.449(4) . ? N9 C16 1.376(4) . ? N9 C12 1.441(4) . ? N9 C13 1.452(4) . ? N10 C16 1.350(4) . ? N10 C14 1.446(4) . ? N10 C15 1.459(4) . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C10 H10A 0.9600 . ? C10 H10B 0.9600 . ? C10 H10C 0.9600 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C17 C18 1.388(5) . ? C17 C21 1.393(5) . ? C17 H17A 0.9300 . ? C18 C19 1.385(5) . ? C18 H18A 0.9300 . ? C19 C20 1.388(5) . ? C19 H19A 0.9300 . ? C20 C21 1.377(5) . ? C20 H20A 0.9300 . ? C21 H21A 0.9300 . ? C22 C26 1.396(5) . ? C22 C23 1.400(5) . ? C22 H22A 0.9300 . ? C23 C24 1.397(5) . ? C23 H23A 0.9300 . ? C24 C25 1.380(5) . ? C24 H24A 0.9300 . ? C25 C26 1.393(5) . ? C25 H25A 0.9300 . ? C26 H26A 0.9300 . ? C27 C31 1.386(5) . ? C27 C28 1.389(5) . ? C27 H27A 0.9300 . ? C28 C29 1.395(5) . ? C28 H28A 0.9300 . ? C29 C30 1.388(5) . ? C29 H29A 0.9300 . ? C30 C31 1.383(5) . ? C30 H30A 0.9300 . ? C31 H31A 0.9300 . ? C32 C36 1.376(5) . ? C32 C33 1.386(5) . ? C32 H32A 0.9300 . ? C33 C34 1.380(5) . ? C33 H33A 0.9300 . ? C34 C35 1.391(5) . ? C34 H34A 0.9300 . ? C35 C36 1.379(5) . ? C35 H35A 0.9300 . ? C36 H36A 0.9300 . ? 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 Y1 N1 76.62(10) . . ? N6 Y1 N2 131.56(9) . . ? N1 Y1 N2 55.86(9) . . ? N6 Y1 C20 94.99(12) . . ? N1 Y1 C20 84.13(11) . . ? N2 Y1 C20 89.45(12) . . ? N6 Y1 C21 79.55(11) . . ? N1 Y1 C21 104.98(12) . . ? N2 Y1 C21 118.68(11) . . ? C20 Y1 C21 29.77(11) . . ? N6 Y1 C26 76.74(10) . . ? N1 Y1 C26 125.56(11) . . ? N2 Y1 C26 121.91(11) . . ? C20 Y1 C26 144.69(13) . . ? C21 Y1 C26 115.57(13) . . ? N6 Y1 C22 102.73(11) . . ? N1 Y1 C22 147.97(11) . . ? N2 Y1 C22 112.34(11) . . ? C20 Y1 C22 127.41(13) . . ? C21 Y1 C22 106.37(13) . . ? C26 Y1 C22 29.96(10) . . ? N6 Y1 C19 124.49(11) . . ? N1 Y1 C19 95.48(12) . . ? N2 Y1 C19 73.43(11) . . ? C20 Y1 C19 29.82(10) . . ? C21 Y1 C19 49.09(12) . . ? C26 Y1 C19 138.47(13) . . ? C22 Y1 C19 109.96(13) . . ? N6 Y1 C17 97.77(12) . . ? N1 Y1 C17 132.59(12) . . ? N2 Y1 C17 120.16(11) . . ? C20 Y1 C17 49.05(13) . . ? C21 Y1 C17 29.84(11) . . ? C26 Y1 C17 97.46(13) . . ? C22 Y1 C17 79.43(13) . . ? C19 Y1 C17 48.83(13) . . ? N6 Y1 C18 126.27(11) . . ? N1 Y1 C18 124.91(12) . . ? N2 Y1 C18 91.82(11) . . ? C20 Y1 C18 48.86(12) . . ? C21 Y1 C18 48.92(13) . . ? C26 Y1 C18 109.17(13) . . ? C22 Y1 C18 81.86(13) . . ? C19 Y1 C18 29.44(11) . . ? C17 Y1 C18 29.49(10) . . ? N6 Y1 C23 125.40(11) . . ? N1 Y1 C23 126.55(12) . . ? N2 Y1 C23 82.53(11) . . ? C20 Y1 C23 131.63(13) . . ? C21 Y1 C23 125.27(14) . . ? C26 Y1 C23 49.05(11) . . ? C22 Y1 C23 29.84(11) . . ? C19 Y1 C23 103.60(14) . . ? C17 Y1 C23 95.43(15) . . ? C18 Y1 C23 83.66(14) . . ? N6 Y1 C25 82.16(11) . . ? N1 Y1 C25 100.18(10) . . ? N2 Y1 C25 96.32(11) . . ? C20 Y1 C25 174.08(13) . . ? C21 Y1 C25 144.32(13) . . ? C26 Y1 C25 29.58(10) . . ? C22 Y1 C25 48.88(11) . . ? C19 Y1 C25 151.83(13) . . ? C17 Y1 C25 126.03(13) . . ? C18 Y1 C25 129.31(12) . . ? C23 Y1 C25 48.42(12) . . ? N1 Y2 N6 76.95(9) . . ? N1 Y2 N7 131.50(9) . . ? N6 Y2 N7 55.41(9) . . ? N1 Y2 C28 80.18(11) . . ? N6 Y2 C28 107.03(12) . . ? N7 Y2 C28 119.37(11) . . ? N1 Y2 C29 99.10(12) . . ? N6 Y2 C29 134.29(11) . . ? N7 Y2 C29 119.63(11) . . ? C28 Y2 C29 29.97(10) . . ? N1 Y2 C27 94.97(11) . . ? N6 Y2 C27 85.52(11) . . ? N7 Y2 C27 90.30(11) . . ? C28 Y2 C27 29.79(11) . . ? C29 Y2 C27 49.08(12) . . ? N1 Y2 C35 125.72(11) . . ? N6 Y2 C35 126.01(12) . . ? N7 Y2 C35 82.34(11) . . ? C28 Y2 C35 123.62(14) . . ? C29 Y2 C35 93.66(14) . . ? C27 Y2 C35 130.82(13) . . ? N1 Y2 C36 103.16(12) . . ? N6 Y2 C36 147.10(11) . . ? N7 Y2 C36 111.74(11) . . ? C28 Y2 C36 105.35(13) . . ? C29 Y2 C36 78.55(13) . . ? C27 Y2 C36 126.75(12) . . ? C35 Y2 C36 29.41(10) . . ? N1 Y2 C31 124.34(11) . . ? N6 Y2 C31 95.64(12) . . ? N7 Y2 C31 73.60(11) . . ? C28 Y2 C31 48.94(12) . . ? C29 Y2 C31 48.74(13) . . ? C27 Y2 C31 29.57(10) . . ? C35 Y2 C31 103.41(14) . . ? C36 Y2 C31 110.05(14) . . ? N1 Y2 C30 127.54(11) . . ? N6 Y2 C30 124.92(12) . . ? N7 Y2 C30 90.86(11) . . ? C28 Y2 C30 49.15(12) . . ? C29 Y2 C30 29.65(11) . . ? C27 Y2 C30 48.88(12) . . ? C35 Y2 C30 82.53(14) . . ? C36 Y2 C30 81.68(14) . . ? C31 Y2 C30 29.41(11) . . ? N1 Y2 C32 77.86(11) . . ? N6 Y2 C32 125.58(12) . . ? N7 Y2 C32 120.93(12) . . ? C28 Y2 C32 115.03(14) . . ? C29 Y2 C32 96.84(14) . . ? C27 Y2 C32 144.12(13) . . ? C35 Y2 C32 48.21(12) . . ? C36 Y2 C32 29.26(10) . . ? C31 Y2 C32 138.03(14) . . ? C30 Y2 C32 108.71(14) . . ? N1 Y2 C33 82.52(11) . . ? N6 Y2 C33 99.74(11) . . ? N7 Y2 C33 95.91(12) . . ? C28 Y2 C33 143.69(14) . . ? C29 Y2 C33 125.20(13) . . ? C27 Y2 C33 173.44(13) . . ? C35 Y2 C33 48.47(12) . . ? C36 Y2 C33 48.62(12) . . ? C31 Y2 C33 151.67(13) . . ? C30 Y2 C33 128.63(13) . . ? C32 Y2 C33 29.41(11) . . ? C1 N1 Y2 158.6(2) . . ? C1 N1 Y1 98.2(2) . . ? Y2 N1 Y1 103.25(11) . . ? C4 N2 C1 121.7(3) . . ? C4 N2 Y1 137.1(2) . . ? C1 N2 Y1 86.7(2) . . ? C1 N3 C3 119.7(3) . . ? C1 N3 C2 123.3(3) . . ? C3 N3 C2 113.8(3) . . ? C4 N4 C5 120.5(3) . . ? C4 N4 C6 121.1(3) . . ? C5 N4 C6 116.0(3) . . ? C4 N5 C8 122.2(3) . . ? C4 N5 C7 122.2(3) . . ? C8 N5 C7 114.5(3) . . ? C9 N6 Y1 157.8(2) . . ? C9 N6 Y2 99.0(2) . . ? Y1 N6 Y2 103.17(10) . . ? C16 N7 C9 123.8(3) . . ? C16 N7 Y2 136.1(3) . . ? C9 N7 Y2 85.49(19) . . ? C9 N8 C10 120.0(3) . . ? C9 N8 C11 123.0(3) . . ? C10 N8 C11 114.6(3) . . ? C16 N9 C12 119.7(3) . . ? C16 N9 C13 122.0(3) . . ? C12 N9 C13 115.8(3) . . ? C16 N10 C14 121.4(3) . . ? C16 N10 C15 122.8(3) . . ? C14 N10 C15 114.1(3) . . ? N1 C1 N3 127.8(3) . . ? N1 C1 N2 117.2(3) . . ? N3 C1 N2 114.9(3) . . ? N1 C1 Y1 55.47(18) . . ? N3 C1 Y1 163.9(2) . . ? N2 C1 Y1 63.33(17) . . ? N3 C2 H2A 109.5 . . ? N3 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N3 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N3 C3 H3A 109.5 . . ? N3 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N3 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C4 N5 126.3(3) . . ? N2 C4 N4 118.4(3) . . ? N5 C4 N4 115.3(4) . . ? N4 C5 H5A 109.5 . . ? N4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N4 C6 H6A 109.5 . . ? N4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N5 C7 H7A 109.5 . . ? N5 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N5 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N5 C8 H8A 109.5 . . ? N5 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N5 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N6 C9 N8 127.4(3) . . ? N6 C9 N7 117.8(3) . . ? N8 C9 N7 114.7(3) . . ? N6 C9 Y2 54.92(18) . . ? N8 C9 Y2 164.6(2) . . ? N7 C9 Y2 64.60(17) . . ? N8 C10 H10A 109.5 . . ? N8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? N8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N8 C11 H11A 109.5 . . ? N8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? N8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? N9 C12 H12A 109.5 . . ? N9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? N9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N9 C13 H13A 109.5 . . ? N9 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? N9 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? N10 C14 H14A 109.5 . . ? N10 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? N10 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N10 C15 H15A 109.5 . . ? N10 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? N10 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N7 C16 N10 127.0(3) . . ? N7 C16 N9 118.4(3) . . ? N10 C16 N9 114.5(3) . . ? C18 C17 C21 107.7(4) . . ? C18 C17 Y1 75.8(2) . . ? C21 C17 Y1 73.8(2) . . ? C18 C17 H17A 126.2 . . ? C21 C17 H17A 126.2 . . ? Y1 C17 H17A 116.4 . . ? C19 C18 C17 108.3(4) . . ? C19 C18 Y1 74.7(2) . . ? C17 C18 Y1 74.7(2) . . ? C19 C18 H18A 125.9 . . ? C17 C18 H18A 125.9 . . ? Y1 C18 H18A 116.8 . . ? C18 C19 C20 107.5(4) . . ? C18 C19 Y1 75.9(2) . . ? C20 C19 Y1 73.3(2) . . ? C18 C19 H19A 126.2 . . ? C20 C19 H19A 126.2 . . ? Y1 C19 H19A 116.7 . . ? C21 C20 C19 108.6(4) . . ? C21 C20 Y1 75.7(2) . . ? C19 C20 Y1 76.9(2) . . ? C21 C20 H20A 125.7 . . ? C19 C20 H20A 125.7 . . ? Y1 C20 H20A 113.9 . . ? C20 C21 C17 107.8(4) . . ? C20 C21 Y1 74.5(2) . . ? C17 C21 Y1 76.3(2) . . ? C20 C21 H21A 126.1 . . ? C17 C21 H21A 126.1 . . ? Y1 C21 H21A 115.3 . . ? C26 C22 C23 107.6(4) . . ? C26 C22 Y1 75.0(2) . . ? C23 C22 Y1 76.5(2) . . ? C26 C22 H22A 126.2 . . ? C23 C22 H22A 126.2 . . ? Y1 C22 H22A 114.7 . . ? C24 C23 C22 107.7(4) . . ? C24 C23 Y1 77.4(2) . . ? C22 C23 Y1 73.7(2) . . ? C24 C23 H23A 126.2 . . ? C22 C23 H23A 126.2 . . ? Y1 C23 H23A 115.0 . . ? C25 C24 C23 108.4(4) . . ? C25 C24 Y1 74.3(2) . . ? C23 C24 Y1 73.3(2) . . ? C25 C24 H24A 125.8 . . ? C23 C24 H24A 125.8 . . ? Y1 C24 H24A 118.5 . . ? C24 C25 C26 108.2(4) . . ? C24 C25 Y1 76.9(2) . . ? C26 C25 Y1 73.0(2) . . ? C24 C25 H25A 125.9 . . ? C26 C25 H25A 125.9 . . ? Y1 C25 H25A 116.3 . . ? C25 C26 C22 108.1(4) . . ? C25 C26 Y1 77.4(2) . . ? C22 C26 Y1 75.0(2) . . ? C25 C26 H26A 126.0 . . ? C22 C26 H26A 126.0 . . ? Y1 C26 H26A 113.9 . . ? C31 C27 C28 108.0(4) . . ? C31 C27 Y2 75.9(2) . . ? C28 C27 Y2 74.6(2) . . ? C31 C27 H27A 126.0 . . ? C28 C27 H27A 126.0 . . ? Y2 C27 H27A 115.7 . . ? C27 C28 C29 107.5(4) . . ? C27 C28 Y2 75.6(2) . . ? C29 C28 Y2 75.2(2) . . ? C27 C28 H28A 126.2 . . ? C29 C28 H28A 126.2 . . ? Y2 C28 H28A 115.3 . . ? C30 C29 C28 108.2(4) . . ? C30 C29 Y2 76.2(2) . . ? C28 C29 Y2 74.9(2) . . ? C30 C29 H29A 125.9 . . ? C28 C29 H29A 125.9 . . ? Y2 C29 H29A 115.2 . . ? C31 C30 C29 107.7(4) . . ? C31 C30 Y2 75.3(2) . . ? C29 C30 Y2 74.2(2) . . ? C31 C30 H30A 126.1 . . ? C29 C30 H30A 126.1 . . ? Y2 C30 H30A 116.5 . . ? C30 C31 C27 108.5(4) . . ? C30 C31 Y2 75.3(2) . . ? C27 C31 Y2 74.6(2) . . ? C30 C31 H31A 125.7 . . ? C27 C31 H31A 125.7 . . ? Y2 C31 H31A 116.4 . . ? C36 C32 C33 108.8(4) . . ? C36 C32 Y2 75.1(2) . . ? C33 C32 Y2 75.6(2) . . ? C36 C32 H32A 125.6 . . ? C33 C32 H32A 125.6 . . ? Y2 C32 H32A 115.7 . . ? C34 C33 C32 107.7(4) . . ? C34 C33 Y2 75.6(2) . . ? C32 C33 Y2 75.0(2) . . ? C34 C33 H33A 126.1 . . ? C32 C33 H33A 126.1 . . ? Y2 C33 H33A 115.5 . . ? C33 C34 C35 107.5(4) . . ? C33 C34 Y2 75.2(2) . . ? C35 C34 Y2 74.1(2) . . ? C33 C34 H34A 126.3 . . ? C35 C34 H34A 126.3 . . ? Y2 C34 H34A 116.6 . . ? C36 C35 C34 108.6(4) . . ? C36 C35 Y2 75.7(2) . . ? C34 C35 Y2 76.4(2) . . ? C36 C35 H35A 125.7 . . ? C34 C35 H35A 125.7 . . ? Y2 C35 H35A 114.4 . . ? C32 C36 C35 107.4(4) . . ? C32 C36 Y2 75.6(2) . . ? C35 C36 Y2 74.8(2) . . ? C32 C36 H36A 126.3 . . ? C35 C36 H36A 126.3 . . ? Y2 C36 H36A 115.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.01 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.689 _refine_diff_density_min -0.535 _refine_diff_density_rms 0.072