Supplementary Material (ESI) for Chemical Communications This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Kyle A. Williams' _publ_contact_author_email kyle.williams@mail.utexas.edu loop_ _publ_author_name 'Kyle A. Williams' 'Christopher W. Bielawski' # Attachment 'cif.CIF.txt' data_9,10-dihexylanthracene _database_code_depnum_ccdc_archive 'CCDC 774042' #TrackingRef 'cif.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H34' _chemical_formula_weight 346.53 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 7.8785(5) _cell_length_b 17.1725(9) _cell_length_c 8.2929(6) _cell_angle_alpha 90.00 _cell_angle_beta 117.057(2) _cell_angle_gamma 90.00 _cell_volume 999.18(11) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 2295 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description prisms _exptl_crystal_colour yellow _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.152 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 380 _exptl_absorpt_coefficient_mu 0.064 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(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 'Nonius Kappa CCD' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4350 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0329 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -10 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.48 _reflns_number_total 2283 _reflns_number_gt 1844 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. An Integrated System of Windows Programs for the Solution, Refinement and Analysis of Single Crystal X-ray Diffraction Data. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (2008). SHELXL-97. Acat Cryst., A64, 112-122. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction ; DENZO and Scalepack (Otwinoski and Minor, 1997) ; _computing_structure_solution ; SIR97 - Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The molecule sits around a crystallographic inversion center at 1/2, 1/2, 1/2. ; _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^)+(0.0743P)^2^+0.2485P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2283 _refine_ls_number_parameters 186 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0587 _refine_ls_R_factor_gt 0.0443 _refine_ls_wR_factor_ref 0.1274 _refine_ls_wR_factor_gt 0.1161 _refine_ls_goodness_of_fit_ref 0.992 _refine_ls_restrained_S_all 0.992 _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 C1 C 0.58401(16) 0.53760(6) 0.67055(14) 0.0176(3) Uani 1 1 d . . . C2 C 0.45037(15) 0.57818(6) 0.51104(15) 0.0173(3) Uani 1 1 d . . . C3 C 0.41010(17) 0.65832(7) 0.52980(16) 0.0215(3) Uani 1 1 d . . . C4 C 0.49060(18) 0.69513(7) 0.69291(16) 0.0238(3) Uani 1 1 d . . . C5 C 0.61521(18) 0.65418(7) 0.85099(16) 0.0246(3) Uani 1 1 d . . . C6 C 0.65985(17) 0.57843(7) 0.84015(15) 0.0215(3) Uani 1 1 d . . . C7 C 0.63542(15) 0.45992(7) 0.65829(15) 0.0179(3) Uani 1 1 d . . . C8 C 0.77758(17) 0.41736(7) 0.82499(15) 0.0198(3) Uani 1 1 d . . . C9 C 0.68389(17) 0.37093(7) 0.92114(15) 0.0217(3) Uani 1 1 d . . . C10 C 0.82822(18) 0.33353(7) 1.09792(15) 0.0219(3) Uani 1 1 d . . . C11 C 0.91697(17) 0.39002(7) 1.25657(15) 0.0197(3) Uani 1 1 d . . . C12 C 1.05828(18) 0.35001(7) 1.43016(16) 0.0231(3) Uani 1 1 d . . . C13 C 1.1365(2) 0.40348(9) 1.59461(17) 0.0294(3) Uani 1 1 d . . . H11B H 0.812(2) 0.4140(8) 1.2775(18) 0.023(3) Uiso 1 1 d . . . H9A H 0.597(2) 0.4055(8) 0.9453(18) 0.024(3) Uiso 1 1 d . . . H8A H 0.873(2) 0.4539(8) 0.9112(19) 0.023(3) Uiso 1 1 d . . . H4 H 0.462(2) 0.7491(9) 0.7026(19) 0.028(4) Uiso 1 1 d . . . H6 H 0.742(2) 0.5508(8) 0.951(2) 0.027(3) Uiso 1 1 d . . . H10B H 0.764(2) 0.2920(9) 1.1348(18) 0.029(4) Uiso 1 1 d . . . H3 H 0.324(2) 0.6872(9) 0.422(2) 0.032(4) Uiso 1 1 d . . . H9B H 0.600(2) 0.3304(9) 0.8368(19) 0.028(4) Uiso 1 1 d . . . H12A H 1.164(2) 0.3287(8) 1.4112(18) 0.024(3) Uiso 1 1 d . . . H10A H 0.931(2) 0.3100(9) 1.0774(18) 0.027(4) Uiso 1 1 d . . . H8B H 0.853(2) 0.3811(8) 0.7914(18) 0.027(4) Uiso 1 1 d . . . H5 H 0.666(2) 0.6791(9) 0.968(2) 0.034(4) Uiso 1 1 d . . . H12B H 0.991(2) 0.3057(9) 1.4533(19) 0.034(4) Uiso 1 1 d . . . H13A H 1.204(2) 0.4475(9) 1.575(2) 0.037(4) Uiso 1 1 d . . . H11A H 0.9834(18) 0.4340(9) 1.2250(18) 0.024(3) Uiso 1 1 d . . . H13B H 1.031(2) 0.4245(10) 1.618(2) 0.042(4) Uiso 1 1 d . . . H13C H 1.226(3) 0.3761(10) 1.708(2) 0.051(5) 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 C1 0.0166(5) 0.0204(6) 0.0162(5) 0.0014(4) 0.0078(4) -0.0030(4) C2 0.0164(6) 0.0187(6) 0.0180(6) 0.0017(4) 0.0088(5) -0.0016(4) C3 0.0226(6) 0.0205(6) 0.0222(6) 0.0028(5) 0.0111(5) 0.0005(5) C4 0.0275(7) 0.0184(6) 0.0277(6) -0.0019(5) 0.0145(5) -0.0013(5) C5 0.0269(7) 0.0263(7) 0.0202(6) -0.0056(5) 0.0105(5) -0.0056(5) C6 0.0204(6) 0.0255(6) 0.0162(6) 0.0004(4) 0.0063(5) -0.0034(5) C7 0.0165(6) 0.0213(6) 0.0164(5) 0.0023(4) 0.0078(4) -0.0018(4) C8 0.0185(6) 0.0215(6) 0.0169(5) 0.0019(4) 0.0059(5) -0.0001(5) C9 0.0226(6) 0.0221(6) 0.0177(6) 0.0017(5) 0.0068(5) -0.0031(5) C10 0.0280(7) 0.0179(6) 0.0179(6) 0.0021(4) 0.0088(5) -0.0008(5) C11 0.0226(6) 0.0185(6) 0.0168(5) 0.0012(4) 0.0077(5) -0.0001(5) C12 0.0232(6) 0.0240(6) 0.0192(6) 0.0030(5) 0.0072(5) 0.0013(5) C13 0.0287(7) 0.0370(8) 0.0188(6) -0.0008(5) 0.0074(5) -0.0025(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 C1 C7 1.4110(17) . ? C1 C6 1.4360(15) . ? C1 C2 1.4412(15) . ? C2 C7 1.4119(15) 3_666 ? C2 C3 1.4364(16) . ? C3 C4 1.3605(17) . ? C3 H3 0.978(15) . ? C4 C5 1.4163(17) . ? C4 H4 0.967(15) . ? C5 C6 1.3612(18) . ? C5 H5 0.966(16) . ? C6 H6 0.972(15) . ? C7 C2 1.4119(15) 3_666 ? C7 C8 1.5136(15) . ? C8 C9 1.5336(16) . ? C8 H8A 0.990(14) . ? C8 H8B 0.986(14) . ? C9 C10 1.5291(16) . ? C9 H9A 0.994(15) . ? C9 H9B 0.995(15) . ? C10 C11 1.5244(16) . ? C10 H10B 1.001(15) . ? C10 H10A 0.990(15) . ? C11 C12 1.5250(16) . ? C11 H11B 1.006(14) . ? C11 H11A 1.019(15) . ? C12 C13 1.5226(18) . ? C12 H12A 0.988(14) . ? C12 H12B 0.993(16) . ? C13 H13A 0.980(17) . ? C13 H13B 1.001(17) . ? C13 H13C 1.000(18) . ? 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 C6 121.80(10) . . ? C7 C1 C2 120.32(10) . . ? C6 C1 C2 117.88(10) . . ? C7 C2 C3 121.49(10) 3_666 . ? C7 C2 C1 120.54(10) 3_666 . ? C3 C2 C1 117.97(10) . . ? C4 C3 C2 121.79(11) . . ? C4 C3 H3 119.4(9) . . ? C2 C3 H3 118.8(9) . . ? C3 C4 C5 120.19(11) . . ? C3 C4 H4 120.5(9) . . ? C5 C4 H4 119.3(9) . . ? C6 C5 C4 120.30(11) . . ? C6 C5 H5 119.2(9) . . ? C4 C5 H5 120.5(9) . . ? C5 C6 C1 121.76(11) . . ? C5 C6 H6 119.1(8) . . ? C1 C6 H6 119.1(8) . . ? C1 C7 C2 119.11(10) . 3_666 ? C1 C7 C8 120.53(10) . . ? C2 C7 C8 120.34(10) 3_666 . ? C7 C8 C9 113.25(10) . . ? C7 C8 H8A 110.9(8) . . ? C9 C8 H8A 109.9(8) . . ? C7 C8 H8B 109.8(8) . . ? C9 C8 H8B 108.4(8) . . ? H8A C8 H8B 104.3(11) . . ? C10 C9 C8 113.14(10) . . ? C10 C9 H9A 109.8(8) . . ? C8 C9 H9A 109.5(8) . . ? C10 C9 H9B 110.3(8) . . ? C8 C9 H9B 108.8(8) . . ? H9A C9 H9B 105.0(11) . . ? C11 C10 C9 114.16(10) . . ? C11 C10 H10B 106.7(8) . . ? C9 C10 H10B 109.4(8) . . ? C11 C10 H10A 108.6(8) . . ? C9 C10 H10A 108.5(8) . . ? H10B C10 H10A 109.4(12) . . ? C10 C11 C12 112.30(10) . . ? C10 C11 H11B 108.6(8) . . ? C12 C11 H11B 109.0(8) . . ? C10 C11 H11A 109.7(8) . . ? C12 C11 H11A 109.7(7) . . ? H11B C11 H11A 107.4(11) . . ? C13 C12 C11 113.46(11) . . ? C13 C12 H12A 109.8(8) . . ? C11 C12 H12A 108.9(8) . . ? C13 C12 H12B 108.8(8) . . ? C11 C12 H12B 107.7(9) . . ? H12A C12 H12B 108.0(12) . . ? C12 C13 H13A 110.4(9) . . ? C12 C13 H13B 111.1(9) . . ? H13A C13 H13B 108.4(13) . . ? C12 C13 H13C 112.5(10) . . ? H13A C13 H13C 108.1(13) . . ? H13B C13 H13C 106.3(13) . . ? 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 C7 2.05(18) . . . 3_666 ? C6 C1 C2 C7 -177.25(10) . . . 3_666 ? C7 C1 C2 C3 -177.07(10) . . . . ? C6 C1 C2 C3 3.63(16) . . . . ? C7 C2 C3 C4 179.24(11) 3_666 . . . ? C1 C2 C3 C4 -1.65(17) . . . . ? C2 C3 C4 C5 -1.19(19) . . . . ? C3 C4 C5 C6 1.98(19) . . . . ? C4 C5 C6 C1 0.16(19) . . . . ? C7 C1 C6 C5 177.74(11) . . . . ? C2 C1 C6 C5 -2.97(17) . . . . ? C6 C1 C7 C2 177.25(10) . . . 3_666 ? C2 C1 C7 C2 -2.02(18) . . . 3_666 ? C6 C1 C7 C8 -1.50(17) . . . . ? C2 C1 C7 C8 179.23(9) . . . . ? C1 C7 C8 C9 92.29(13) . . . . ? C2 C7 C8 C9 -86.45(13) 3_666 . . . ? C7 C8 C9 C10 -175.22(10) . . . . ? C8 C9 C10 C11 77.38(13) . . . . ? C9 C10 C11 C12 179.42(10) . . . . ? C10 C11 C12 C13 -175.06(11) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.292 _refine_diff_density_min -0.175 _refine_diff_density_rms 0.040 #===END data_9,10-dihexyltriptycene _database_code_depnum_ccdc_archive 'CCDC 774043' #TrackingRef 'cif.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common 9,10-dihexyl-triptycene _chemical_melting_point ? _chemical_formula_moiety 9,10-(C6H13)2-C20H12 _chemical_formula_sum 'C32 H38' _chemical_formula_weight 422.62 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' _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 69.417(14) _cell_length_b 8.3391(17) _cell_length_c 33.478(7) _cell_angle_alpha 90.00 _cell_angle_beta 117.24(3) _cell_angle_gamma 90.00 _cell_volume 17231(6) _cell_formula_units_Z 28 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.28 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.140 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6440 _exptl_absorpt_coefficient_mu 0.064 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _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 'CCD area detector' _diffrn_measurement_method 'phi scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29014 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0689 _diffrn_reflns_limit_h_min -81 _diffrn_reflns_limit_h_max 82 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_limit_l_max 39 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15111 _reflns_number_gt 9689 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect software, Nonius B.V. 1998' _computing_cell_refinement 'Collect software, Nonius B.V. 1998' _computing_data_reduction 'DENZO and Scalepack (Otwinoski and Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0555P)^2^+57.1491P] 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 15111 _refine_ls_number_parameters 1036 _refine_ls_number_restraints 62 _refine_ls_R_factor_all 0.1245 _refine_ls_R_factor_gt 0.0753 _refine_ls_wR_factor_ref 0.1857 _refine_ls_wR_factor_gt 0.1613 _refine_ls_goodness_of_fit_ref 0.994 _refine_ls_restrained_S_all 1.004 _refine_ls_shift/su_max 0.038 _refine_ls_shift/su_mean 0.001 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.07525(5) 0.4160(3) 0.40896(9) 0.0247(6) Uani 1 1 d . . . C2 C 0.06173(5) 0.3246(3) 0.42768(9) 0.0255(7) Uani 1 1 d . . . C3 C 0.07490(4) 0.1705(3) 0.44690(9) 0.0238(6) Uani 1 1 d . . . C4 C 0.09692(5) 0.4419(3) 0.44046(9) 0.0255(7) Uani 1 1 d . . . C5 C 0.08627(5) 0.4564(3) 0.49933(9) 0.0255(7) Uani 1 1 d . . . C6 C 0.08174(5) -0.1129(4) 0.44938(10) 0.0315(7) Uani 1 1 d . . . H6A H 0.0767 -0.2165 0.4400 0.038 Uiso 1 1 calc R . . C9 C 0.06463(5) 0.4320(3) 0.46746(9) 0.0257(7) Uani 1 1 d . . . C12 C 0.06778(5) 0.0161(4) 0.43260(10) 0.0274(7) Uani 1 1 d . . . H12A H 0.0535 -0.0011 0.4115 0.033 Uiso 1 1 calc R . . C14 C 0.10306(5) -0.0877(4) 0.48007(10) 0.0318(7) Uani 1 1 d . . . H14A H 0.1124 -0.1746 0.4913 0.038 Uiso 1 1 calc R . . C20 C 0.04822(5) 0.5156(4) 0.47104(10) 0.0308(7) Uani 1 1 d . . . H20A H 0.0339 0.5015 0.4496 0.037 Uiso 1 1 calc R . . C21 C 0.09661(5) 0.1961(4) 0.47838(9) 0.0250(7) Uani 1 1 d . . . C24 C 0.10295(5) 0.3738(3) 0.48776(9) 0.0257(7) Uani 1 1 d . . . C26 C 0.03808(5) 0.2988(4) 0.39272(10) 0.0293(7) Uani 1 1 d . . . H26A H 0.0381 0.2403 0.3677 0.035 Uiso 1 1 calc R . . H26B H 0.0317 0.4031 0.3815 0.035 Uiso 1 1 calc R . . C28 C 0.08164(5) 0.5538(4) 0.35341(10) 0.0340(8) Uani 1 1 d . . . H28A H 0.0766 0.5918 0.3242 0.041 Uiso 1 1 calc R . . C30 C 0.07441(5) 0.6423(4) 0.53825(11) 0.0369(8) Uani 1 1 d . . . H30A H 0.0777 0.7112 0.5623 0.044 Uiso 1 1 calc R . . C32 C 0.06768(5) 0.4725(4) 0.36556(10) 0.0285(7) Uani 1 1 d . . . H32A H 0.0533 0.4560 0.3446 0.034 Uiso 1 1 calc R . . C34 C 0.12677(5) 0.4032(4) 0.52174(9) 0.0301(7) Uani 1 1 d . . . H34A H 0.1294 0.5178 0.5233 0.036 Uiso 1 1 calc R . . H34B H 0.1358 0.3543 0.5099 0.036 Uiso 1 1 calc R . . C38 C 0.11069(5) 0.5224(4) 0.42787(10) 0.0299(7) Uani 1 1 d . . . H38A H 0.1251 0.5386 0.4486 0.036 Uiso 1 1 calc R . . C39 C 0.13449(5) 0.3413(4) 0.57006(10) 0.0358(8) Uani 1 1 d . . . H39A H 0.1265 0.3965 0.5832 0.043 Uiso 1 1 calc R . . H39B H 0.1312 0.2280 0.5689 0.043 Uiso 1 1 calc R . . C48 C 0.09096(5) 0.5622(4) 0.53436(10) 0.0317(7) Uani 1 1 d . . . H48A H 0.1053 0.5796 0.5554 0.038 Uiso 1 1 calc R . . C49 C 0.02323(5) 0.2095(4) 0.40794(11) 0.0336(7) Uani 1 1 d . . . H49A H 0.0252 0.0950 0.4064 0.040 Uiso 1 1 calc R . . H49B H 0.0275 0.2364 0.4391 0.040 Uiso 1 1 calc R . . C52 C 0.05319(5) 0.6206(4) 0.50667(10) 0.0364(8) Uani 1 1 d . . . H52A H 0.0422 0.6762 0.5092 0.044 Uiso 1 1 calc R . . C55 C 0.11065(5) 0.0663(4) 0.49433(10) 0.0278(7) Uani 1 1 d . . . H55A H 0.1251 0.0826 0.5146 0.033 Uiso 1 1 calc R . . C61 C 0.10296(5) 0.5789(4) 0.38415(11) 0.0329(8) Uani 1 1 d . . . H61A H 0.1122 0.6336 0.3757 0.040 Uiso 1 1 calc R . . C70 C -0.00058(5) 0.2493(5) 0.37982(11) 0.0421(9) Uani 1 1 d . . . H70A H -0.0044 0.2347 0.3483 0.050 Uiso 1 1 calc R . . H70B H -0.0029 0.3611 0.3843 0.050 Uiso 1 1 calc R . . C90 C -0.01533(5) 0.1452(5) 0.39163(13) 0.0548(11) Uani 1 1 d . . . H90A H -0.0127 0.0337 0.3874 0.066 Uiso 1 1 calc R . . H90B H -0.0113 0.1601 0.4232 0.066 Uiso 1 1 calc R . . C97 C 0.17540(6) 0.3324(8) 0.59733(14) 0.0911(18) Uani 1 1 d . . . H97A H 0.1736 0.3917 0.5709 0.109 Uiso 1 1 calc R . . H97B H 0.1734 0.2209 0.5880 0.109 Uiso 1 1 calc R . . C98 C 0.15771(7) 0.3640(12) 0.59914(17) 0.171(4) Uani 1 1 d . . . H98A H 0.1588 0.4782 0.6052 0.205 Uiso 1 1 calc R . . H98B H 0.1599 0.3137 0.6270 0.205 Uiso 1 1 calc R . . C101 C -0.03942(6) 0.1777(7) 0.36481(15) 0.0865(18) Uani 1 1 d . . . H10A H -0.0428 0.1930 0.3336 0.104 Uiso 1 1 calc R . . H10B H -0.0473 0.0838 0.3664 0.104 Uiso 1 1 calc R . . C105 C -0.04707(7) 0.3159(7) 0.37967(17) 0.0921(17) Uani 1 1 d . . . H10C H -0.0624 0.3287 0.3610 0.138 Uiso 1 1 calc R . . H10D H -0.0396 0.4101 0.3776 0.138 Uiso 1 1 calc R . . H10E H -0.0443 0.3005 0.4103 0.138 Uiso 1 1 calc R . . C108 C 0.19761(7) 0.3408(11) 0.62441(18) 0.151(4) Uani 1 1 d . . . H10F H 0.1987 0.4488 0.6360 0.182 Uiso 1 1 calc R . . H10Q H 0.1989 0.2727 0.6490 0.182 Uiso 1 1 calc R . . C112 C 0.21612(9) 0.3259(16) 0.6283(2) 0.239(7) Uani 1 1 d . . . H11A H 0.2265 0.3567 0.6581 0.358 Uiso 1 1 calc R . . H11B H 0.2177 0.3934 0.6067 0.358 Uiso 1 1 calc R . . H11C H 0.2185 0.2162 0.6231 0.358 Uiso 1 1 calc R . . C7 C 0.01685(4) 0.9180(3) 0.29337(9) 0.0228(6) Uani 1 1 d . . . C8 C 0.03236(5) 0.8334(3) 0.32946(9) 0.0268(7) Uani 1 1 d . . . H8A H 0.0466 0.8301 0.3340 0.032 Uiso 1 1 calc R . . C15 C -0.00471(5) 0.9184(3) 0.28634(9) 0.0251(7) Uani 1 1 d . . . C17 C 0.10075(5) 1.1031(4) 0.36419(10) 0.0311(7) Uani 1 1 d . . . H17A H 0.1033 1.1941 0.3491 0.037 Uiso 1 1 calc R . . H17B H 0.0958 1.1444 0.3851 0.037 Uiso 1 1 calc R . . C18 C 0.00547(5) 0.7568(4) 0.35221(10) 0.0305(7) Uani 1 1 d . . . H18A H 0.0018 0.7041 0.3722 0.037 Uiso 1 1 calc R . . C19 C 0.08283(5) 1.0009(4) 0.32935(10) 0.0303(7) Uani 1 1 d . . . H19A H 0.0870 0.9680 0.3067 0.036 Uiso 1 1 calc R . . H19B H 0.0811 0.9049 0.3438 0.036 Uiso 1 1 calc R . . C22 C 0.02058(5) 1.0058(3) 0.25689(9) 0.0259(7) Uani 1 1 d . . . C23 C 0.02653(5) 0.7535(4) 0.35884(10) 0.0297(7) Uani 1 1 d . . . H23A H 0.0370 0.6975 0.3831 0.036 Uiso 1 1 calc R . . C25 C 0.04410(5) 1.0007(4) 0.26499(10) 0.0284(7) Uani 1 1 d . . . H25A H 0.0446 1.0453 0.2387 0.034 Uiso 1 1 calc R . . H25B H 0.0484 0.8890 0.2670 0.034 Uiso 1 1 calc R . . C29 C 0.12206(5) 1.0161(4) 0.39067(10) 0.0338(8) Uani 1 1 d . . . H29A H 0.1263 0.9647 0.3699 0.041 Uiso 1 1 calc R . . H29B H 0.1201 0.9328 0.4087 0.041 Uiso 1 1 calc R . . C33 C -0.01027(5) 0.8384(4) 0.31577(9) 0.0280(7) Uani 1 1 d . . . H33A H -0.0245 0.8393 0.3111 0.034 Uiso 1 1 calc R . . C37 C 0.01060(5) 1.1739(3) 0.25267(9) 0.0260(7) Uani 1 1 d . . . C51 C 0.01020(5) 1.4619(4) 0.25119(11) 0.0399(8) Uani 1 1 d . . . H51A H 0.0169 1.5584 0.2514 0.048 Uiso 1 1 calc R . . C64 C 0.06124(5) 1.0880(4) 0.30665(10) 0.0301(7) Uani 1 1 d . . . H64A H 0.0636 1.1940 0.2978 0.036 Uiso 1 1 calc R . . H64B H 0.0556 1.1015 0.3282 0.036 Uiso 1 1 calc R . . C65 C 0.02063(5) 1.3179(4) 0.25332(10) 0.0330(8) Uani 1 1 d . . . H65A H 0.0344 1.3182 0.2552 0.040 Uiso 1 1 calc R . . C77 C 0.14009(5) 1.1273(4) 0.42125(11) 0.0436(9) Uani 1 1 d . . . H77A H 0.1532 1.0669 0.4373 0.065 Uiso 1 1 calc R . . H77B H 0.1361 1.1771 0.4423 0.065 Uiso 1 1 calc R . . H77C H 0.1424 1.2085 0.4035 0.065 Uiso 1 1 calc R . . C10 C 0.15299(5) 0.8590(4) 0.21801(10) 0.0296(7) Uani 1 1 d . . . C11 C 0.11713(5) 0.9755(4) 0.20044(10) 0.0312(7) Uani 1 1 d . . . C13 C 0.15144(5) 0.9633(4) 0.17878(10) 0.0330(8) Uani 1 1 d . . . C27 C 0.08927(5) 0.9372(4) 0.11858(10) 0.0380(8) Uani 1 1 d . . . H27A H 0.0798 0.8904 0.1296 0.046 Uiso 1 1 calc R . . H27B H 0.0869 1.0522 0.1169 0.046 Uiso 1 1 calc R . . C31 C 0.11265(5) 0.9067(4) 0.15397(10) 0.0326(8) Uani 1 1 d . . . C36 C 0.13014(5) 0.9871(4) 0.14488(10) 0.0325(7) Uani 1 1 d . . . C41 C 0.11260(5) 0.4449(4) 0.16183(11) 0.0414(9) Uani 1 1 d . . . H41A H 0.1033 0.3580 0.1497 0.050 Uiso 1 1 calc R . . C43 C 0.11889(5) 0.7290(4) 0.16432(10) 0.0318(7) Uani 1 1 d . . . C44 C 0.14026(5) 0.7043(4) 0.19767(10) 0.0313(7) Uani 1 1 d . . . C46 C 0.13849(5) 0.9508(4) 0.23399(10) 0.0294(7) Uani 1 1 d . . . C47 C 0.12664(5) 1.0891(4) 0.10936(10) 0.0381(8) Uani 1 1 d . . . H47A H 0.1126 1.1072 0.0870 0.046 Uiso 1 1 calc R . . C53 C 0.14736(5) 0.5500(4) 0.21233(10) 0.0340(8) Uani 1 1 d . . . H53A H 0.1615 0.5336 0.2346 0.041 Uiso 1 1 calc R . . C59 C 0.12978(5) 1.0866(4) 0.28687(10) 0.0363(8) Uani 1 1 d . . . H59A H 0.1340 1.1246 0.3158 0.044 Uiso 1 1 calc R . . C60 C 0.17611(5) 0.8348(4) 0.25561(10) 0.0329(7) Uani 1 1 d . . . H60A H 0.1820 0.9398 0.2673 0.040 Uiso 1 1 calc R . . H60B H 0.1751 0.7765 0.2797 0.040 Uiso 1 1 calc R . . C62 C 0.10249(5) 1.0538(4) 0.21075(10) 0.0340(8) Uani 1 1 d . . . H62A H 0.0883 1.0695 0.1886 0.041 Uiso 1 1 calc R . . C63 C 0.10519(5) 0.5991(4) 0.14720(10) 0.0374(8) Uani 1 1 d . . . H63A H 0.0909 0.6151 0.1257 0.045 Uiso 1 1 calc R . . C66 C 0.10882(5) 1.1091(4) 0.25405(10) 0.0365(8) Uani 1 1 d . . . H66A H 0.0989 1.1615 0.2609 0.044 Uiso 1 1 calc R . . C68 C 0.14467(5) 1.0073(4) 0.27696(10) 0.0331(7) Uani 1 1 d . . . H68A H 0.1588 0.9923 0.2992 0.040 Uiso 1 1 calc R . . C69 C 0.08178(5) 0.8763(5) 0.07059(10) 0.0433(9) Uani 1 1 d . . . H69A H 0.0897 0.9323 0.0573 0.052 Uiso 1 1 calc R . . H69B H 0.0851 0.7630 0.0715 0.052 Uiso 1 1 calc R . . C73 C 0.16839(5) 1.0429(4) 0.17652(11) 0.0386(8) Uani 1 1 d . . . H73A H 0.1824 1.0295 0.1993 0.046 Uiso 1 1 calc R . . C74 C 0.14379(6) 1.1639(5) 0.10689(11) 0.0448(9) Uani 1 1 d . . . H74A H 0.1413 1.2290 0.0824 0.054 Uiso 1 1 calc R . . C75 C 0.19248(5) 0.7473(4) 0.24450(11) 0.0409(8) Uani 1 1 d . . . H75A H 0.1911 0.6326 0.2473 0.049 Uiso 1 1 calc R . . H75B H 0.1892 0.7697 0.2136 0.049 Uiso 1 1 calc R . . C80 C 0.13365(5) 0.4196(4) 0.19419(11) 0.0395(8) Uani 1 1 d . . . H80A H 0.1386 0.3162 0.2038 0.047 Uiso 1 1 calc R . . C84 C 0.16458(6) 1.1426(5) 0.14045(11) 0.0461(9) Uani 1 1 d . . . H84A H 0.1761 1.1949 0.1390 0.055 Uiso 1 1 calc R . . C85 C 0.05797(6) 0.9003(5) 0.04163(12) 0.0506(10) Uani 1 1 d . . . H85A H 0.0545 0.8837 0.0104 0.061 Uiso 1 1 calc R . . H85B H 0.0541 1.0095 0.0449 0.061 Uiso 1 1 calc R . . C88 C 0.21546(5) 0.7979(5) 0.27516(12) 0.0472(9) Uani 1 1 d . . . H88A H 0.2182 0.7819 0.3060 0.057 Uiso 1 1 calc R . . H88B H 0.2168 0.9117 0.2710 0.057 Uiso 1 1 calc R . . C92 C 0.23258(5) 0.7089(5) 0.26776(13) 0.0554(11) Uani 1 1 d . . . H92A H 0.2322 0.5966 0.2749 0.066 Uiso 1 1 calc R . . H92B H 0.2291 0.7159 0.2362 0.066 Uiso 1 1 calc R . . C99 C 0.02209(9) 0.7753(8) 0.03128(17) 0.105(2) Uani 1 1 d . . . H99A H 0.0186 0.7433 0.0008 0.126 Uiso 1 1 calc R . . H99B H 0.0170 0.8847 0.0297 0.126 Uiso 1 1 calc R . . C100 C 0.04436(7) 0.7777(7) 0.05556(14) 0.0800(15) Uani 1 1 d . . . H10G H 0.0496 0.6705 0.0546 0.096 Uiso 1 1 calc R . . H10H H 0.0479 0.7993 0.0866 0.096 Uiso 1 1 calc R . . C102 C 0.25517(6) 0.7724(8) 0.29548(18) 0.104(2) Uani 1 1 d . . . H10I H 0.2586 0.7680 0.3270 0.125 Uiso 1 1 calc R . . H10J H 0.2556 0.8839 0.2877 0.125 Uiso 1 1 calc R . . C103 C 0.27239(7) 0.6802(9) 0.28888(19) 0.126(3) Uani 1 1 d . . . H10K H 0.2863 0.7272 0.3071 0.189 Uiso 1 1 calc R . . H10L H 0.2693 0.6848 0.2578 0.189 Uiso 1 1 calc R . . H10M H 0.2725 0.5704 0.2976 0.189 Uiso 1 1 calc R . . C107 C 0.00966(8) 0.6770(11) 0.0458(2) 0.159(4) Uani 1 1 d . . . H10N H -0.0055 0.6935 0.0263 0.238 Uiso 1 1 calc R . . H10O H 0.0129 0.7050 0.0760 0.238 Uiso 1 1 calc R . . H10P H 0.0132 0.5664 0.0447 0.238 Uiso 1 1 calc R . . C16 C 0.18315(5) 0.5562(4) 0.38697(10) 0.0287(7) Uani 1 1 d . . . C35 C 0.12261(5) 0.5256(4) 0.29899(10) 0.0357(8) Uani 1 1 d . . . H35A H 0.1175 0.4829 0.3193 0.043 Uiso 1 1 calc R . . H35B H 0.1256 0.4356 0.2843 0.043 Uiso 1 1 calc R . . C40 C 0.15878(4) 0.5362(4) 0.37073(10) 0.0313(7) Uani 1 1 d . . . H40A H 0.1554 0.5777 0.3939 0.038 Uiso 1 1 calc R . . H40B H 0.1556 0.4223 0.3680 0.038 Uiso 1 1 calc R . . C42 C 0.14348(5) 0.6168(4) 0.32606(10) 0.0332(7) Uani 1 1 d . . . H42A H 0.1399 0.7234 0.3323 0.040 Uiso 1 1 calc R . . H42B H 0.1510 0.6289 0.3080 0.040 Uiso 1 1 calc R . . C45 C 0.19714(5) 0.4799(4) 0.43344(10) 0.0312(7) Uani 1 1 d . . . C50 C 0.19134(5) 0.4716(4) 0.35676(10) 0.0283(7) Uani 1 1 d . . . C54 C 0.17902(5) 0.3776(4) 0.31984(10) 0.0333(7) Uani 1 1 d . . . H54A H 0.1642 0.3673 0.3102 0.040 Uiso 1 1 calc R . . C56 C 0.21368(5) 0.4846(4) 0.37161(11) 0.0352(8) Uani 1 1 d . . . C57 C 0.17927(5) 0.8664(4) 0.38940(10) 0.0353(8) Uani 1 1 d . . . H57A H 0.1647 0.8573 0.3824 0.042 Uiso 1 1 calc R . . C58 C 0.19134(5) 0.7293(4) 0.39293(9) 0.0294(7) Uani 1 1 d . . . C67 C 0.21951(5) 0.4938(4) 0.44808(11) 0.0371(8) Uani 1 1 d . . . C71 C 0.18941(6) 0.4018(4) 0.45963(11) 0.0385(8) Uani 1 1 d . . . H71A H 0.1746 0.3925 0.4498 0.046 Uiso 1 1 calc R . . C72 C 0.18858(6) 0.2987(4) 0.29706(12) 0.0463(9) Uani 1 1 d . . . H72A H 0.1801 0.2374 0.2718 0.056 Uiso 1 1 calc R . . C76 C 0.22565(5) 0.5824(4) 0.41506(11) 0.0380(8) Uani 1 1 d D C . C78 C 0.20397(6) 0.3371(4) 0.50072(12) 0.0501(10) Uani 1 1 d . . . H78A H 0.1989 0.2852 0.5186 0.060 Uiso 1 1 calc R . . C79 C 0.22317(6) 0.4024(4) 0.34914(14) 0.0507(10) Uani 1 1 d . . . H79A H 0.2381 0.4086 0.3592 0.061 Uiso 1 1 calc R . . C81 C 0.21356(5) 0.7432(4) 0.40611(10) 0.0371(8) Uani 1 1 d . . . C82 C 0.10492(5) 0.6272(4) 0.26377(11) 0.0416(9) Uani 1 1 d . . . H82A H 0.1021 0.7176 0.2786 0.050 Uiso 1 1 calc R . . H82B H 0.1102 0.6697 0.2436 0.050 Uiso 1 1 calc R . . C83 C 0.18876(6) 1.0159(4) 0.39627(11) 0.0457(9) Uani 1 1 d . . . H83A H 0.1806 1.1070 0.3938 0.055 Uiso 1 1 calc R . . C86 C 0.21045(7) 0.3109(5) 0.31166(14) 0.0567(11) Uani 1 1 d . . . H86A H 0.2168 0.2575 0.2963 0.068 Uiso 1 1 calc R . . C87 C 0.23375(6) 0.4271(4) 0.48871(12) 0.0497(10) Uani 1 1 d . . . H87A H 0.2486 0.4339 0.4985 0.060 Uiso 1 1 calc R . . C89 C 0.08376(5) 0.5410(5) 0.23609(11) 0.0514(10) Uani 1 1 d . . . H89A H 0.0789 0.4906 0.2561 0.062 Uiso 1 1 calc R . . H89B H 0.0861 0.4572 0.2187 0.062 Uiso 1 1 calc R . . C91 C 0.22263(6) 0.8948(5) 0.41218(15) 0.0674(13) Uani 1 1 d . . . H91A H 0.2373 0.9056 0.4200 0.081 Uiso 1 1 calc R . . C93 C 0.21015(6) 1.0308(5) 0.40669(15) 0.0690(13) Uani 1 1 d . . . H93A H 0.2163 1.1320 0.4101 0.083 Uiso 1 1 calc R . . C94 C 0.06611(6) 0.6542(6) 0.20430(15) 0.0817(16) Uani 1 1 d . . . H94A H 0.0530 0.5948 0.1874 0.123 Uiso 1 1 calc R . . H94B H 0.0707 0.7030 0.1841 0.123 Uiso 1 1 calc R . . H94C H 0.0635 0.7360 0.2214 0.123 Uiso 1 1 calc R . . C95 C 0.22587(6) 0.3497(5) 0.51500(12) 0.0565(11) Uani 1 1 d . . . H95A H 0.2355 0.3061 0.5425 0.068 Uiso 1 1 calc R . . C410 C 0.25007(6) 0.5953(5) 0.43043(14) 0.0656(12) Uani 1 1 d DU . . H41E H 0.2551 0.4866 0.4343 0.079 Uiso 1 1 d R C . H41D H 0.2516 0.6372 0.4053 0.079 Uiso 0.50 1 d PR A 1 H41C H 0.2568 0.6345 0.4607 0.079 Uiso 0.50 1 d PR B 2 C420 C 0.26541(9) 0.6759(9) 0.4669(2) 0.0478(18) Uani 0.50 1 d PDU C 1 H42C H 0.2644 0.6354 0.4928 0.057 Uiso 0.50 1 d PR C 1 H42D H 0.2611 0.7864 0.4635 0.057 Uiso 0.50 1 d PR C 1 C450 C 0.28812(11) 0.6635(14) 0.4760(3) 0.095(3) Uani 0.50 1 d PDU C 1 H45A H 0.2947 0.5994 0.5027 0.114 Uiso 0.50 1 d PR C 1 H45B H 0.2931 0.7708 0.4856 0.114 Uiso 0.50 1 d PR C 1 C460 C 0.29811(14) 0.7122(15) 0.4528(6) 0.104(5) Uani 0.50 1 d PDU C 1 H46B H 0.2957 0.6997 0.4786 0.124 Uiso 0.50 1 d PR C 1 H46C H 0.2977 0.8248 0.4465 0.124 Uiso 0.50 1 d PR C 1 C430 C 0.25851(10) 0.6866(9) 0.4068(3) 0.054(2) Uani 0.50 1 d PDU C 2 H43A H 0.2578 0.7978 0.4134 0.065 Uiso 0.50 1 d PR C 2 H43B H 0.2494 0.6706 0.3753 0.065 Uiso 0.50 1 d PR C 2 C440 C 0.28117(11) 0.6417(14) 0.4173(3) 0.098(3) Uani 0.50 1 d PDU C 2 H44A H 0.2832 0.6631 0.3913 0.117 Uiso 0.50 1 d PR C 2 H44B H 0.2828 0.5282 0.4226 0.117 Uiso 0.50 1 d PR C 2 C465 C 0.29806(13) 0.6356(19) 0.4583(6) 0.097(4) Uani 0.50 1 d PDU C 2 H46A H 0.2898 0.6839 0.4294 0.116 Uiso 0.50 1 d PR C 2 H46D H 0.2951 0.5228 0.4535 0.116 Uiso 0.50 1 d PR C 2 C470 C 0.32131(7) 0.6471(8) 0.46544(17) 0.0938(17) Uani 1 1 d DU . . H47D H 0.3273 0.5411 0.4698 0.113 Uiso 0.50 1 d PR C 1 H47E H 0.3208 0.6886 0.4383 0.113 Uiso 0.50 1 d PR C 1 H47C H 0.3226 0.5364 0.4741 0.113 Uiso 0.50 1 d PR C 2 H47B H 0.3242 0.6574 0.4402 0.113 Uiso 0.50 1 d PR C 2 C480 C 0.33633(7) 0.7423(7) 0.50227(19) 0.0936(17) Uani 1 1 d U C . H48B H 0.3510 0.7094 0.5116 0.140 Uiso 1 1 d R . . H48C H 0.3346 0.8524 0.4929 0.140 Uiso 1 1 d R . . H48D H 0.3330 0.7311 0.5270 0.140 Uiso 1 1 d 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 C1 0.0331(16) 0.0162(15) 0.0284(16) -0.0022(13) 0.0171(14) 0.0016(13) C2 0.0313(16) 0.0227(16) 0.0242(15) 0.0002(13) 0.0141(13) -0.0001(13) C3 0.0287(16) 0.0246(16) 0.0226(15) -0.0006(13) 0.0156(13) -0.0025(13) C4 0.0370(17) 0.0163(15) 0.0284(16) -0.0026(13) 0.0194(14) -0.0001(13) C5 0.0349(17) 0.0209(16) 0.0251(15) 0.0019(13) 0.0176(14) -0.0007(13) C6 0.0397(18) 0.0207(17) 0.0358(18) -0.0027(14) 0.0188(16) -0.0032(14) C9 0.0346(17) 0.0203(16) 0.0254(15) 0.0014(13) 0.0163(14) -0.0009(13) C12 0.0300(16) 0.0265(17) 0.0265(16) -0.0013(13) 0.0136(14) -0.0011(14) C14 0.0367(18) 0.0252(17) 0.0352(18) 0.0044(14) 0.0179(16) 0.0050(14) C20 0.0371(18) 0.0300(18) 0.0285(17) 0.0007(14) 0.0177(15) 0.0004(15) C21 0.0300(16) 0.0264(17) 0.0242(15) 0.0000(13) 0.0171(14) -0.0029(13) C24 0.0286(16) 0.0246(16) 0.0237(15) -0.0004(13) 0.0118(13) -0.0029(13) C26 0.0317(17) 0.0269(17) 0.0266(16) -0.0008(14) 0.0109(14) -0.0006(14) C28 0.052(2) 0.0267(18) 0.0292(17) 0.0041(14) 0.0233(16) 0.0022(15) C30 0.055(2) 0.0304(18) 0.0318(18) -0.0074(15) 0.0254(17) -0.0025(16) C32 0.0367(17) 0.0240(17) 0.0277(16) -0.0020(13) 0.0174(14) 0.0021(14) C34 0.0328(17) 0.0287(17) 0.0297(16) -0.0009(14) 0.0152(14) -0.0043(14) C38 0.0362(17) 0.0239(17) 0.0343(18) -0.0032(14) 0.0202(15) -0.0020(14) C39 0.0371(18) 0.0373(19) 0.0312(17) 0.0009(15) 0.0142(15) -0.0021(15) C48 0.0393(18) 0.0290(18) 0.0269(16) 0.0003(14) 0.0153(15) -0.0039(15) C49 0.0314(17) 0.0296(18) 0.0403(19) 0.0010(15) 0.0168(15) 0.0011(14) C52 0.045(2) 0.0355(19) 0.0365(18) -0.0031(16) 0.0251(17) 0.0039(16) C55 0.0285(16) 0.0290(18) 0.0261(16) 0.0018(14) 0.0128(14) 0.0003(14) C61 0.048(2) 0.0223(17) 0.0423(19) -0.0005(15) 0.0328(17) -0.0013(15) C70 0.0305(18) 0.057(2) 0.0345(18) -0.0076(17) 0.0111(15) 0.0008(17) C90 0.0349(19) 0.072(3) 0.064(3) -0.020(2) 0.0287(19) -0.0076(19) C97 0.049(3) 0.174(6) 0.043(2) 0.015(3) 0.014(2) -0.009(3) C98 0.038(3) 0.400(13) 0.080(4) 0.130(6) 0.032(3) 0.061(5) C101 0.038(2) 0.164(6) 0.062(3) -0.027(3) 0.026(2) -0.016(3) C105 0.064(3) 0.127(5) 0.091(4) 0.033(4) 0.040(3) 0.040(3) C108 0.035(3) 0.332(11) 0.087(4) 0.098(6) 0.028(3) 0.055(4) C112 0.065(4) 0.58(2) 0.070(4) 0.010(8) 0.027(3) -0.026(8) C7 0.0320(16) 0.0160(15) 0.0203(15) -0.0033(12) 0.0118(13) -0.0014(13) C8 0.0312(16) 0.0223(16) 0.0258(16) -0.0015(13) 0.0121(14) -0.0009(13) C15 0.0351(17) 0.0180(15) 0.0222(15) -0.0015(13) 0.0131(13) -0.0007(13) C17 0.0341(17) 0.0286(18) 0.0335(17) -0.0031(14) 0.0179(15) -0.0034(14) C18 0.0417(19) 0.0257(17) 0.0255(16) 0.0051(14) 0.0166(15) -0.0021(15) C19 0.0344(17) 0.0261(17) 0.0349(17) -0.0022(14) 0.0198(15) -0.0027(14) C22 0.0334(17) 0.0226(16) 0.0242(15) 0.0004(13) 0.0155(14) -0.0028(13) C23 0.0356(18) 0.0250(17) 0.0220(15) 0.0021(13) 0.0075(14) -0.0001(14) C25 0.0342(17) 0.0256(17) 0.0279(16) -0.0028(13) 0.0163(14) -0.0032(14) C29 0.0346(17) 0.0357(19) 0.0334(18) -0.0014(15) 0.0176(15) -0.0048(15) C33 0.0331(17) 0.0267(17) 0.0280(16) -0.0005(14) 0.0174(14) -0.0008(14) C37 0.0368(16) 0.0240(16) 0.0150(14) -0.0010(13) 0.0100(13) -0.0013(13) C51 0.053(2) 0.0207(17) 0.0319(18) 0.0016(15) 0.0074(17) -0.0072(15) C64 0.0335(17) 0.0250(17) 0.0341(17) -0.0026(14) 0.0174(15) -0.0046(14) C65 0.0398(18) 0.0257(18) 0.0255(16) 0.0015(14) 0.0081(15) -0.0051(15) C77 0.0355(19) 0.046(2) 0.044(2) -0.0003(18) 0.0137(16) -0.0055(17) C10 0.0285(16) 0.0350(18) 0.0246(16) 0.0015(14) 0.0115(14) 0.0030(14) C11 0.0349(17) 0.0337(18) 0.0255(16) -0.0003(14) 0.0143(14) 0.0015(15) C13 0.0332(17) 0.039(2) 0.0273(17) -0.0032(15) 0.0139(15) 0.0042(15) C27 0.0330(18) 0.054(2) 0.0278(17) -0.0026(16) 0.0141(15) 0.0074(16) C31 0.0302(17) 0.043(2) 0.0215(16) -0.0034(15) 0.0094(14) 0.0042(15) C36 0.0327(17) 0.040(2) 0.0250(16) -0.0051(15) 0.0136(14) 0.0071(15) C41 0.042(2) 0.046(2) 0.0362(19) -0.0138(17) 0.0178(17) -0.0092(17) C43 0.0315(17) 0.044(2) 0.0231(16) -0.0070(15) 0.0148(14) 0.0016(16) C44 0.0308(17) 0.039(2) 0.0255(16) -0.0057(15) 0.0138(14) 0.0021(15) C46 0.0323(17) 0.0297(18) 0.0255(16) 0.0022(14) 0.0126(14) 0.0015(14) C47 0.0368(18) 0.048(2) 0.0265(17) 0.0010(16) 0.0121(15) 0.0104(17) C53 0.0324(17) 0.040(2) 0.0297(17) -0.0027(15) 0.0141(15) 0.0023(15) C59 0.051(2) 0.0329(19) 0.0279(17) -0.0042(15) 0.0207(17) -0.0013(16) C60 0.0320(17) 0.0335(18) 0.0284(17) 0.0004(14) 0.0094(14) 0.0010(15) C62 0.0350(17) 0.039(2) 0.0286(17) -0.0005(15) 0.0149(15) 0.0053(15) C63 0.0299(17) 0.054(2) 0.0276(17) -0.0108(17) 0.0124(15) -0.0036(17) C66 0.0414(19) 0.038(2) 0.0355(19) -0.0029(16) 0.0221(16) 0.0029(16) C68 0.0373(18) 0.0346(19) 0.0236(16) -0.0010(14) 0.0107(14) -0.0031(15) C69 0.0317(18) 0.071(3) 0.0273(17) -0.0030(18) 0.0136(15) 0.0012(18) C73 0.0322(18) 0.050(2) 0.0330(18) 0.0012(17) 0.0141(15) 0.0019(16) C74 0.052(2) 0.053(2) 0.0324(19) 0.0095(17) 0.0220(18) 0.0053(19) C75 0.0325(18) 0.043(2) 0.043(2) 0.0014(17) 0.0136(16) 0.0046(16) C80 0.048(2) 0.034(2) 0.0387(19) -0.0057(16) 0.0219(17) 0.0005(17) C84 0.044(2) 0.059(2) 0.041(2) 0.0066(19) 0.0237(18) -0.0019(18) C85 0.049(2) 0.049(2) 0.036(2) -0.0086(18) 0.0037(17) 0.0075(19) C88 0.0335(19) 0.060(3) 0.048(2) 0.0037(19) 0.0182(17) 0.0039(18) C92 0.039(2) 0.075(3) 0.052(2) 0.011(2) 0.0210(18) 0.011(2) C99 0.101(4) 0.153(6) 0.077(4) -0.025(4) 0.055(3) -0.039(4) C100 0.064(3) 0.130(5) 0.053(3) -0.029(3) 0.034(2) -0.009(3) C102 0.038(2) 0.165(6) 0.106(4) -0.024(4) 0.030(3) 0.007(3) C103 0.044(3) 0.223(8) 0.110(4) -0.022(5) 0.035(3) 0.025(4) C107 0.061(3) 0.332(12) 0.099(4) 0.003(6) 0.050(3) -0.031(5) C16 0.0306(16) 0.0273(17) 0.0275(16) -0.0005(14) 0.0127(14) -0.0009(14) C35 0.0319(17) 0.042(2) 0.0337(18) -0.0039(16) 0.0157(15) -0.0015(15) C40 0.0297(17) 0.0293(18) 0.0341(17) -0.0025(14) 0.0139(14) -0.0026(14) C42 0.0308(17) 0.0301(18) 0.0366(18) -0.0006(15) 0.0137(15) 0.0008(14) C45 0.0380(18) 0.0213(16) 0.0298(17) -0.0043(14) 0.0115(15) -0.0044(14) C50 0.0302(16) 0.0225(16) 0.0316(17) 0.0013(14) 0.0136(14) 0.0015(13) C54 0.0376(18) 0.0270(18) 0.0341(18) -0.0018(15) 0.0153(15) -0.0016(15) C56 0.0346(18) 0.0255(18) 0.045(2) 0.0042(15) 0.0177(16) 0.0000(15) C57 0.0404(19) 0.0316(19) 0.0270(17) -0.0032(14) 0.0095(15) 0.0011(16) C58 0.0341(18) 0.0261(17) 0.0227(16) -0.0009(13) 0.0085(14) -0.0048(14) C67 0.0357(18) 0.0253(18) 0.0360(19) -0.0011(15) 0.0041(15) -0.0065(15) C71 0.047(2) 0.0304(19) 0.0351(19) -0.0039(16) 0.0157(16) -0.0096(16) C72 0.065(3) 0.032(2) 0.049(2) -0.0076(17) 0.033(2) -0.0009(18) C76 0.0262(17) 0.0318(19) 0.046(2) 0.0037(16) 0.0081(15) -0.0031(14) C78 0.073(3) 0.036(2) 0.034(2) 0.0046(17) 0.017(2) -0.0107(19) C79 0.043(2) 0.040(2) 0.080(3) 0.000(2) 0.037(2) 0.0048(18) C81 0.0346(18) 0.0297(19) 0.0334(18) 0.0022(15) 0.0037(15) -0.0073(15) C82 0.0323(18) 0.047(2) 0.041(2) -0.0090(17) 0.0125(16) 0.0057(16) C83 0.054(2) 0.0247(19) 0.037(2) -0.0023(16) 0.0020(17) 0.0023(17) C86 0.074(3) 0.039(2) 0.084(3) -0.012(2) 0.060(3) 0.000(2) C87 0.045(2) 0.035(2) 0.046(2) 0.0062(18) 0.0009(18) -0.0088(17) C89 0.0355(19) 0.079(3) 0.0359(19) -0.014(2) 0.0126(16) 0.0007(19) C91 0.035(2) 0.039(2) 0.087(3) 0.013(2) -0.007(2) -0.0109(18) C93 0.053(3) 0.028(2) 0.082(3) 0.006(2) -0.007(2) -0.0111(19) C94 0.043(2) 0.094(4) 0.073(3) -0.037(3) -0.004(2) 0.026(2) C95 0.062(3) 0.042(2) 0.037(2) 0.0085(18) -0.0020(19) -0.008(2) C410 0.035(2) 0.050(2) 0.089(3) 0.021(2) 0.008(2) -0.0031(19) C420 0.048(4) 0.040(4) 0.050(4) -0.011(3) 0.018(3) -0.008(3) C450 0.053(5) 0.154(8) 0.102(6) -0.065(6) 0.056(5) -0.031(5) C460 0.073(7) 0.097(8) 0.112(8) -0.004(7) 0.017(6) -0.034(6) C430 0.038(4) 0.060(5) 0.072(5) 0.008(4) 0.032(4) -0.006(3) C440 0.070(6) 0.116(7) 0.102(7) 0.027(6) 0.035(5) -0.008(5) C465 0.050(6) 0.122(9) 0.111(8) -0.013(8) 0.031(5) -0.042(6) C470 0.057(3) 0.131(5) 0.092(4) -0.016(3) 0.033(3) -0.011(3) C480 0.053(3) 0.098(4) 0.127(4) -0.013(3) 0.038(3) -0.017(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 C32 1.382(4) . ? C1 C4 1.403(4) . ? C1 C2 1.547(4) . ? C2 C26 1.534(4) . ? C2 C3 1.538(4) . ? C2 C9 1.539(4) . ? C3 C12 1.384(4) . ? C3 C21 1.405(4) . ? C4 C38 1.382(4) . ? C4 C24 1.549(4) . ? C5 C48 1.382(4) . ? C5 C9 1.404(4) . ? C5 C24 1.541(4) . ? C6 C14 1.378(4) . ? C6 C12 1.383(4) . ? C6 H6A 0.9300 . ? C9 C20 1.387(4) . ? C12 H12A 0.9300 . ? C14 C55 1.387(4) . ? C14 H14A 0.9300 . ? C20 C52 1.390(4) . ? C20 H20A 0.9300 . ? C21 C55 1.389(4) . ? C21 C24 1.537(4) . ? C24 C34 1.538(4) . ? C26 C49 1.536(4) . ? C26 H26A 0.9700 . ? C26 H26B 0.9700 . ? C28 C61 1.378(4) . ? C28 C32 1.387(4) . ? C28 H28A 0.9300 . ? C30 C52 1.377(5) . ? C30 C48 1.386(4) . ? C30 H30A 0.9300 . ? C32 H32A 0.9300 . ? C34 C39 1.541(4) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C38 C61 1.391(4) . ? C38 H38A 0.9300 . ? C39 C98 1.464(6) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C48 H48A 0.9300 . ? C49 C70 1.518(4) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C52 H52A 0.9300 . ? C55 H55A 0.9300 . ? C61 H61A 0.9300 . ? C70 C90 1.525(5) . ? C70 H70A 0.9700 . ? C70 H70B 0.9700 . ? C90 C101 1.517(5) . ? C90 H90A 0.9700 . ? C90 H90B 0.9700 . ? C97 C98 1.284(6) . ? C97 C108 1.387(6) . ? C97 H97A 0.9700 . ? C97 H97B 0.9700 . ? C98 H98A 0.9700 . ? C98 H98B 0.9700 . ? C101 C105 1.449(7) . ? C101 H10A 0.9700 . ? C101 H10B 0.9700 . ? C105 H10C 0.9600 . ? C105 H10D 0.9600 . ? C105 H10E 0.9600 . ? C108 C112 1.237(7) . ? C108 H10F 0.9700 . ? C108 H10Q 0.9700 . ? C112 H11A 0.9600 . ? C112 H11B 0.9600 . ? C112 H11C 0.9600 . ? C7 C8 1.388(4) . ? C7 C15 1.405(4) . ? C7 C22 1.544(4) . ? C8 C23 1.392(4) . ? C8 H8A 0.9300 . ? C15 C33 1.383(4) . ? C15 C22 1.542(4) 2 ? C17 C29 1.517(4) . ? C17 C19 1.518(4) . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C18 C23 1.375(4) . ? C18 C33 1.388(4) . ? C18 H18A 0.9300 . ? C19 C64 1.519(4) . ? C19 H19A 0.9700 . ? C19 H19B 0.9700 . ? C22 C25 1.529(4) . ? C22 C15 1.542(4) 2 ? C22 C37 1.541(4) . ? C23 H23A 0.9300 . ? C25 C64 1.540(4) . ? C25 H25A 0.9700 . ? C25 H25B 0.9700 . ? C29 C77 1.517(4) . ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? C33 H33A 0.9300 . ? C37 C65 1.384(4) . ? C37 C37 1.398(6) 2 ? C51 C51 1.382(7) 2 ? C51 C65 1.386(4) . ? C51 H51A 0.9300 . ? C64 H64A 0.9700 . ? C64 H64B 0.9700 . ? C65 H65A 0.9300 . ? C77 H77A 0.9600 . ? C77 H77B 0.9600 . ? C77 H77C 0.9600 . ? C10 C13 1.537(4) . ? C10 C44 1.536(4) . ? C10 C60 1.533(4) . ? C10 C46 1.542(4) . ? C11 C62 1.378(4) . ? C11 C46 1.406(4) . ? C11 C31 1.550(4) . ? C13 C73 1.383(4) . ? C13 C36 1.406(4) . ? C27 C69 1.531(4) . ? C27 C31 1.530(4) . ? C27 H27A 0.9700 . ? C27 H27B 0.9700 . ? C31 C43 1.538(5) . ? C31 C36 1.535(4) . ? C36 C47 1.390(4) . ? C41 C80 1.380(5) . ? C41 C63 1.389(5) . ? C41 H41A 0.9300 . ? C43 C63 1.381(4) . ? C43 C44 1.405(4) . ? C44 C53 1.384(4) . ? C46 C68 1.382(4) . ? C47 C74 1.380(5) . ? C47 H47A 0.9300 . ? C53 C80 1.389(5) . ? C53 H53A 0.9300 . ? C59 C66 1.377(4) . ? C59 C68 1.389(4) . ? C59 H59A 0.9300 . ? C60 C75 1.533(4) . ? C60 H60A 0.9700 . ? C60 H60B 0.9700 . ? C62 C66 1.387(4) . ? C62 H62A 0.9300 . ? C63 H63A 0.9300 . ? C66 H66A 0.9300 . ? C68 H68A 0.9300 . ? C69 C85 1.498(4) . ? C69 H69A 0.9700 . ? C69 H69B 0.9700 . ? C73 C84 1.388(5) . ? C73 H73A 0.9300 . ? C74 C84 1.376(5) . ? C74 H74A 0.9300 . ? C75 C88 1.509(4) . ? C75 H75A 0.9700 . ? C75 H75B 0.9700 . ? C80 H80A 0.9300 . ? C84 H84A 0.9300 . ? C85 C100 1.600(6) . ? C85 H85A 0.9700 . ? C85 H85B 0.9700 . ? C88 C92 1.515(5) . ? C88 H88A 0.9700 . ? C88 H88B 0.9700 . ? C92 C102 1.506(6) . ? C92 H92A 0.9700 . ? C92 H92B 0.9700 . ? C99 C100 1.378(6) . ? C99 C107 1.427(8) . ? C99 H99A 0.9700 . ? C99 H99B 0.9700 . ? C100 H10G 0.9700 . ? C100 H10H 0.9700 . ? C102 C103 1.520(6) . ? C102 H10I 0.9700 . ? C102 H10J 0.9700 . ? C103 H10K 0.9600 . ? C103 H10L 0.9600 . ? C103 H10M 0.9600 . ? C107 H10N 0.9600 . ? C107 H10O 0.9600 . ? C107 H10P 0.9600 . ? C16 C50 1.540(4) . ? C16 C40 1.531(4) . ? C16 C45 1.544(4) . ? C16 C58 1.531(4) . ? C35 C42 1.515(4) . ? C35 C82 1.513(4) . ? C35 H35A 0.9700 . ? C35 H35B 0.9700 . ? C40 C42 1.537(4) . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? C42 H42A 0.9700 . ? C42 H42B 0.9700 . ? C45 C71 1.383(4) . ? C45 C67 1.403(4) . ? C50 C54 1.381(4) . ? C50 C56 1.399(4) . ? C54 C72 1.385(4) . ? C54 H54A 0.9300 . ? C56 C79 1.387(5) . ? C56 C76 1.538(5) . ? C57 C83 1.379(5) . ? C57 C58 1.391(4) . ? C57 H57A 0.9300 . ? C58 C81 1.402(4) . ? C67 C87 1.381(5) . ? C67 C76 1.543(5) . ? C71 C78 1.390(5) . ? C71 H71A 0.9300 . ? C72 C86 1.370(5) . ? C72 H72A 0.9300 . ? C76 C81 1.536(5) . ? C76 C410 1.534(5) . ? C78 C95 1.373(5) . ? C78 H78A 0.9300 . ? C79 C86 1.386(5) . ? C79 H79A 0.9300 . ? C81 C91 1.386(5) . ? C82 C89 1.512(5) . ? C82 H82A 0.9700 . ? C82 H82B 0.9700 . ? C83 C93 1.367(5) . ? C83 H83A 0.9300 . ? C86 H86A 0.9300 . ? C87 C95 1.389(5) . ? C87 H87A 0.9300 . ? C89 C94 1.527(5) . ? C89 H89A 0.9700 . ? C89 H89B 0.9700 . ? C91 C93 1.387(6) . ? C91 H91A 0.9300 . ? C93 H93A 0.9300 . ? C94 H94A 0.9600 . ? C94 H94B 0.9600 . ? C94 H94C 0.9600 . ? C95 H95A 0.9300 . ? C410 C420 1.374(6) . ? C410 C430 1.403(6) . ? C410 H41E 0.9599 . ? C410 H41D 0.9598 . ? C410 H41C 0.9599 . ? C420 C450 1.467(8) . ? C420 H41C 0.6393 . ? C420 H42C 0.9602 . ? C420 H42D 0.9600 . ? C450 C460 1.320(16) . ? C450 H45A 0.9601 . ? C450 H45B 0.9599 . ? C450 H46B 0.5761 . ? C460 C470 1.563(9) . ? C460 H45B 1.3856 . ? C460 H46B 0.9598 . ? C460 H46C 0.9599 . ? C460 H46A 0.7684 . ? C430 C440 1.494(9) . ? C430 H41D 0.6150 . ? C430 H43A 0.9600 . ? C430 H43B 0.9600 . ? C440 C465 1.336(16) . ? C440 H44A 0.9602 . ? C440 H44B 0.9600 . ? C440 H46A 0.6491 . ? C440 H46D 1.5216 . ? C465 C470 1.522(8) . ? C465 H46B 0.9372 . ? C465 H44B 1.4810 . ? C465 H46A 0.9600 . ? C465 H46D 0.9600 . ? C470 C480 1.436(6) . ? C470 H47D 0.9599 . ? C470 H47E 0.9600 . ? C470 H47C 0.9599 . ? C470 H47B 0.9601 . ? C480 H48B 0.9595 . ? C480 H48C 0.9600 . ? C480 H48D 0.9604 . ? 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 C32 C1 C4 119.9(3) . . ? C32 C1 C2 125.8(3) . . ? C4 C1 C2 114.3(2) . . ? C26 C2 C3 115.2(2) . . ? C26 C2 C9 114.4(2) . . ? C3 C2 C9 107.9(2) . . ? C26 C2 C1 113.3(2) . . ? C3 C2 C1 103.1(2) . . ? C9 C2 C1 101.6(2) . . ? C12 C3 C21 119.4(3) . . ? C12 C3 C2 125.7(3) . . ? C21 C3 C2 114.5(2) . . ? C38 C4 C1 119.9(3) . . ? C38 C4 C24 126.1(3) . . ? C1 C4 C24 114.0(2) . . ? C48 C5 C9 119.5(3) . . ? C48 C5 C24 125.9(3) . . ? C9 C5 C24 114.2(2) . . ? C14 C6 C12 119.9(3) . . ? C14 C6 H6A 120.1 . . ? C12 C6 H6A 120.1 . . ? C20 C9 C5 119.8(3) . . ? C20 C9 C2 125.4(3) . . ? C5 C9 C2 114.4(2) . . ? C3 C12 C6 120.7(3) . . ? C3 C12 H12A 119.7 . . ? C6 C12 H12A 119.7 . . ? C6 C14 C55 120.5(3) . . ? C6 C14 H14A 119.8 . . ? C55 C14 H14A 119.8 . . ? C52 C20 C9 120.0(3) . . ? C52 C20 H20A 120.0 . . ? C9 C20 H20A 120.0 . . ? C55 C21 C3 119.5(3) . . ? C55 C21 C24 126.0(3) . . ? C3 C21 C24 114.1(3) . . ? C5 C24 C21 107.7(2) . . ? C5 C24 C34 114.8(2) . . ? C21 C24 C34 114.5(2) . . ? C5 C24 C4 102.2(2) . . ? C21 C24 C4 103.1(2) . . ? C34 C24 C4 113.2(2) . . ? C2 C26 C49 117.5(2) . . ? C2 C26 H26A 107.9 . . ? C49 C26 H26A 107.9 . . ? C2 C26 H26B 107.9 . . ? C49 C26 H26B 107.9 . . ? H26A C26 H26B 107.2 . . ? C61 C28 C32 120.7(3) . . ? C61 C28 H28A 119.6 . . ? C32 C28 H28A 119.6 . . ? C52 C30 C48 120.4(3) . . ? C52 C30 H30A 119.8 . . ? C48 C30 H30A 119.8 . . ? C1 C32 C28 119.6(3) . . ? C1 C32 H32A 120.2 . . ? C28 C32 H32A 120.2 . . ? C24 C34 C39 117.6(2) . . ? C24 C34 H34A 107.9 . . ? C39 C34 H34A 107.9 . . ? C24 C34 H34B 107.9 . . ? C39 C34 H34B 107.9 . . ? H34A C34 H34B 107.2 . . ? C4 C38 C61 119.9(3) . . ? C4 C38 H38A 120.1 . . ? C61 C38 H38A 120.1 . . ? C98 C39 C34 113.8(3) . . ? C98 C39 H39A 108.8 . . ? C34 C39 H39A 108.8 . . ? C98 C39 H39B 108.8 . . ? C34 C39 H39B 108.8 . . ? H39A C39 H39B 107.7 . . ? C5 C48 C30 120.3(3) . . ? C5 C48 H48A 119.9 . . ? C30 C48 H48A 119.9 . . ? C70 C49 C26 113.2(3) . . ? C70 C49 H49A 108.9 . . ? C26 C49 H49A 108.9 . . ? C70 C49 H49B 108.9 . . ? C26 C49 H49B 108.9 . . ? H49A C49 H49B 107.8 . . ? C30 C52 C20 120.0(3) . . ? C30 C52 H52A 120.0 . . ? C20 C52 H52A 120.0 . . ? C14 C55 C21 120.0(3) . . ? C14 C55 H55A 120.0 . . ? C21 C55 H55A 120.0 . . ? C28 C61 C38 120.0(3) . . ? C28 C61 H61A 120.0 . . ? C38 C61 H61A 120.0 . . ? C49 C70 C90 112.6(3) . . ? C49 C70 H70A 109.1 . . ? C90 C70 H70A 109.1 . . ? C49 C70 H70B 109.1 . . ? C90 C70 H70B 109.1 . . ? H70A C70 H70B 107.8 . . ? C101 C90 C70 115.7(4) . . ? C101 C90 H90A 108.3 . . ? C70 C90 H90A 108.3 . . ? C101 C90 H90B 108.3 . . ? C70 C90 H90B 108.3 . . ? H90A C90 H90B 107.4 . . ? C98 C97 C108 139.4(6) . . ? C98 C97 H97A 102.2 . . ? C108 C97 H97A 102.2 . . ? C98 C97 H97B 102.2 . . ? C108 C97 H97B 102.2 . . ? H97A C97 H97B 104.8 . . ? C97 C98 C39 136.7(6) . . ? C97 C98 H98A 103.0 . . ? C39 C98 H98A 103.0 . . ? C97 C98 H98B 103.0 . . ? C39 C98 H98B 103.0 . . ? H98A C98 H98B 105.1 . . ? C105 C101 C90 114.6(4) . . ? C105 C101 H10A 108.6 . . ? C90 C101 H10A 108.6 . . ? C105 C101 H10B 108.6 . . ? C90 C101 H10B 108.6 . . ? H10A C101 H10B 107.6 . . ? C101 C105 H10C 109.5 . . ? C101 C105 H10D 109.5 . . ? H10C C105 H10D 109.5 . . ? C101 C105 H10E 109.5 . . ? H10C C105 H10E 109.5 . . ? H10D C105 H10E 109.5 . . ? C112 C108 C97 148.6(7) . . ? C112 C108 H10F 99.6 . . ? C97 C108 H10F 99.6 . . ? C112 C108 H10Q 99.6 . . ? C97 C108 H10Q 99.6 . . ? H10F C108 H10Q 104.1 . . ? C108 C112 H11A 109.5 . . ? C108 C112 H11B 109.5 . . ? H11A C112 H11B 109.5 . . ? C108 C112 H11C 109.5 . . ? H11A C112 H11C 109.5 . . ? H11B C112 H11C 109.5 . . ? C8 C7 C15 119.3(3) . . ? C8 C7 C22 125.8(3) . . ? C15 C7 C22 114.7(2) . . ? C7 C8 C23 119.9(3) . . ? C7 C8 H8A 120.1 . . ? C23 C8 H8A 120.1 . . ? C33 C15 C7 120.2(3) . . ? C33 C15 C22 125.8(3) . 2 ? C7 C15 C22 114.0(2) . 2 ? C29 C17 C19 114.7(3) . . ? C29 C17 H17A 108.6 . . ? C19 C17 H17A 108.6 . . ? C29 C17 H17B 108.6 . . ? C19 C17 H17B 108.6 . . ? H17A C17 H17B 107.6 . . ? C23 C18 C33 120.2(3) . . ? C23 C18 H18A 119.9 . . ? C33 C18 H18A 119.9 . . ? C64 C19 C17 112.9(3) . . ? C64 C19 H19A 109.0 . . ? C17 C19 H19A 109.0 . . ? C64 C19 H19B 109.0 . . ? C17 C19 H19B 109.0 . . ? H19A C19 H19B 107.8 . . ? C25 C22 C15 113.5(2) . 2 ? C25 C22 C37 116.1(2) . . ? C15 C22 C37 104.2(2) 2 . ? C25 C22 C7 113.5(2) . . ? C15 C22 C7 102.3(2) 2 . ? C37 C22 C7 105.8(2) . . ? C18 C23 C8 120.5(3) . . ? C18 C23 H23A 119.7 . . ? C8 C23 H23A 119.7 . . ? C22 C25 C64 117.8(2) . . ? C22 C25 H25A 107.8 . . ? C64 C25 H25A 107.8 . . ? C22 C25 H25B 107.8 . . ? C64 C25 H25B 107.8 . . ? H25A C25 H25B 107.2 . . ? C17 C29 C77 112.6(3) . . ? C17 C29 H29A 109.1 . . ? C77 C29 H29A 109.1 . . ? C17 C29 H29B 109.1 . . ? C77 C29 H29B 109.1 . . ? H29A C29 H29B 107.8 . . ? C15 C33 C18 119.9(3) . . ? C15 C33 H33A 120.0 . . ? C18 C33 H33A 120.0 . . ? C65 C37 C37 119.62(18) . 2 ? C65 C37 C22 125.9(3) . . ? C37 C37 C22 114.46(15) 2 . ? C51 C51 C65 120.01(19) 2 . ? C51 C51 H51A 120.0 2 . ? C65 C51 H51A 120.0 . . ? C19 C64 C25 113.8(3) . . ? C19 C64 H64A 108.8 . . ? C25 C64 H64A 108.8 . . ? C19 C64 H64B 108.8 . . ? C25 C64 H64B 108.8 . . ? H64A C64 H64B 107.7 . . ? C51 C65 C37 120.3(3) . . ? C51 C65 H65A 119.9 . . ? C37 C65 H65A 119.9 . . ? C29 C77 H77A 109.5 . . ? C29 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C29 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C13 C10 C44 107.2(2) . . ? C13 C10 C60 114.4(2) . . ? C44 C10 C60 115.3(3) . . ? C13 C10 C46 102.4(2) . . ? C44 C10 C46 103.7(2) . . ? C60 C10 C46 112.6(2) . . ? C62 C11 C46 119.9(3) . . ? C62 C11 C31 126.5(3) . . ? C46 C11 C31 113.7(3) . . ? C73 C13 C36 119.7(3) . . ? C73 C13 C10 126.1(3) . . ? C36 C13 C10 114.0(3) . . ? C69 C27 C31 119.2(3) . . ? C69 C27 H27A 107.5 . . ? C31 C27 H27A 107.5 . . ? C69 C27 H27B 107.5 . . ? C31 C27 H27B 107.5 . . ? H27A C27 H27B 107.0 . . ? C27 C31 C43 115.1(3) . . ? C27 C31 C36 115.4(3) . . ? C43 C31 C36 107.4(2) . . ? C27 C31 C11 111.7(2) . . ? C43 C31 C11 103.0(2) . . ? C36 C31 C11 102.9(2) . . ? C47 C36 C13 119.0(3) . . ? C47 C36 C31 126.3(3) . . ? C13 C36 C31 114.4(3) . . ? C80 C41 C63 120.4(3) . . ? C80 C41 H41A 119.8 . . ? C63 C41 H41A 119.8 . . ? C63 C43 C44 119.4(3) . . ? C63 C43 C31 126.3(3) . . ? C44 C43 C31 114.0(3) . . ? C53 C44 C43 119.5(3) . . ? C53 C44 C10 125.7(3) . . ? C43 C44 C10 114.4(3) . . ? C68 C46 C11 119.5(3) . . ? C68 C46 C10 126.1(3) . . ? C11 C46 C10 114.4(3) . . ? C74 C47 C36 120.7(3) . . ? C74 C47 H47A 119.7 . . ? C36 C47 H47A 119.7 . . ? C44 C53 C80 120.7(3) . . ? C44 C53 H53A 119.6 . . ? C80 C53 H53A 119.6 . . ? C66 C59 C68 120.3(3) . . ? C66 C59 H59A 119.9 . . ? C68 C59 H59A 119.9 . . ? C75 C60 C10 118.5(3) . . ? C75 C60 H60A 107.7 . . ? C10 C60 H60A 107.7 . . ? C75 C60 H60B 107.7 . . ? C10 C60 H60B 107.7 . . ? H60A C60 H60B 107.1 . . ? C66 C62 C11 120.1(3) . . ? C66 C62 H62A 119.9 . . ? C11 C62 H62A 119.9 . . ? C43 C63 C41 120.4(3) . . ? C43 C63 H63A 119.8 . . ? C41 C63 H63A 119.8 . . ? C59 C66 C62 120.2(3) . . ? C59 C66 H66A 119.9 . . ? C62 C66 H66A 119.9 . . ? C46 C68 C59 120.0(3) . . ? C46 C68 H68A 120.0 . . ? C59 C68 H68A 120.0 . . ? C85 C69 C27 112.3(3) . . ? C85 C69 H69A 109.2 . . ? C27 C69 H69A 109.2 . . ? C85 C69 H69B 109.2 . . ? C27 C69 H69B 109.2 . . ? H69A C69 H69B 107.9 . . ? C13 C73 C84 120.5(3) . . ? C13 C73 H73A 119.8 . . ? C84 C73 H73A 119.8 . . ? C84 C74 C47 120.3(3) . . ? C84 C74 H74A 119.9 . . ? C47 C74 H74A 119.9 . . ? C88 C75 C60 111.8(3) . . ? C88 C75 H75A 109.2 . . ? C60 C75 H75A 109.2 . . ? C88 C75 H75B 109.2 . . ? C60 C75 H75B 109.2 . . ? H75A C75 H75B 107.9 . . ? C41 C80 C53 119.4(3) . . ? C41 C80 H80A 120.3 . . ? C53 C80 H80A 120.3 . . ? C74 C84 C73 119.9(3) . . ? C74 C84 H84A 120.0 . . ? C73 C84 H84A 120.0 . . ? C69 C85 C100 110.5(3) . . ? C69 C85 H85A 109.6 . . ? C100 C85 H85A 109.6 . . ? C69 C85 H85B 109.6 . . ? C100 C85 H85B 109.6 . . ? H85A C85 H85B 108.1 . . ? C75 C88 C92 114.6(3) . . ? C75 C88 H88A 108.6 . . ? C92 C88 H88A 108.6 . . ? C75 C88 H88B 108.6 . . ? C92 C88 H88B 108.6 . . ? H88A C88 H88B 107.6 . . ? C102 C92 C88 113.6(4) . . ? C102 C92 H92A 108.8 . . ? C88 C92 H92A 108.8 . . ? C102 C92 H92B 108.8 . . ? C88 C92 H92B 108.8 . . ? H92A C92 H92B 107.7 . . ? C100 C99 C107 119.8(6) . . ? C100 C99 H99A 107.4 . . ? C107 C99 H99A 107.4 . . ? C100 C99 H99B 107.4 . . ? C107 C99 H99B 107.4 . . ? H99A C99 H99B 106.9 . . ? C99 C100 C85 119.3(5) . . ? C99 C100 H10G 107.5 . . ? C85 C100 H10G 107.5 . . ? C99 C100 H10H 107.5 . . ? C85 C100 H10H 107.5 . . ? H10G C100 H10H 107.0 . . ? C92 C102 C103 113.5(5) . . ? C92 C102 H10I 108.9 . . ? C103 C102 H10I 108.9 . . ? C92 C102 H10J 108.9 . . ? C103 C102 H10J 108.9 . . ? H10I C102 H10J 107.7 . . ? C102 C103 H10K 109.5 . . ? C102 C103 H10L 109.5 . . ? H10K C103 H10L 109.5 . . ? C102 C103 H10M 109.5 . . ? H10K C103 H10M 109.5 . . ? H10L C103 H10M 109.5 . . ? C99 C107 H10N 109.5 . . ? C99 C107 H10O 109.5 . . ? H10N C107 H10O 109.5 . . ? C99 C107 H10P 109.5 . . ? H10N C107 H10P 109.5 . . ? H10O C107 H10P 109.5 . . ? C50 C16 C40 113.4(2) . . ? C50 C16 C45 102.8(2) . . ? C40 C16 C45 113.3(2) . . ? C50 C16 C58 106.9(2) . . ? C40 C16 C58 115.7(3) . . ? C45 C16 C58 103.4(2) . . ? C42 C35 C82 113.4(3) . . ? C42 C35 H35A 108.9 . . ? C82 C35 H35A 108.9 . . ? C42 C35 H35B 108.9 . . ? C82 C35 H35B 108.9 . . ? H35A C35 H35B 107.7 . . ? C16 C40 C42 117.2(3) . . ? C16 C40 H40A 108.0 . . ? C42 C40 H40A 108.0 . . ? C16 C40 H40B 108.0 . . ? C42 C40 H40B 108.0 . . ? H40A C40 H40B 107.2 . . ? C35 C42 C40 114.1(3) . . ? C35 C42 H42A 108.7 . . ? C40 C42 H42A 108.7 . . ? C35 C42 H42B 108.7 . . ? C40 C42 H42B 108.7 . . ? H42A C42 H42B 107.6 . . ? C71 C45 C67 120.4(3) . . ? C71 C45 C16 125.8(3) . . ? C67 C45 C16 113.8(3) . . ? C54 C50 C56 119.6(3) . . ? C54 C50 C16 125.8(3) . . ? C56 C50 C16 114.4(3) . . ? C50 C54 C72 120.4(3) . . ? C50 C54 H54A 119.8 . . ? C72 C54 H54A 119.8 . . ? C79 C56 C50 119.5(3) . . ? C79 C56 C76 126.2(3) . . ? C50 C56 C76 114.1(3) . . ? C83 C57 C58 120.4(3) . . ? C83 C57 H57A 119.8 . . ? C58 C57 H57A 119.8 . . ? C57 C58 C81 119.5(3) . . ? C57 C58 C16 126.2(3) . . ? C81 C58 C16 114.1(3) . . ? C87 C67 C45 119.4(3) . . ? C87 C67 C76 126.2(3) . . ? C45 C67 C76 114.4(3) . . ? C78 C71 C45 119.5(3) . . ? C78 C71 H71A 120.2 . . ? C45 C71 H71A 120.2 . . ? C86 C72 C54 120.0(3) . . ? C86 C72 H72A 120.0 . . ? C54 C72 H72A 120.0 . . ? C56 C76 C81 105.5(2) . . ? C56 C76 C67 102.5(2) . . ? C81 C76 C67 104.6(3) . . ? C56 C76 C410 113.0(3) . . ? C81 C76 C410 115.2(3) . . ? C67 C76 C410 114.8(3) . . ? C95 C78 C71 120.2(3) . . ? C95 C78 H78A 119.9 . . ? C71 C78 H78A 119.9 . . ? C56 C79 C86 120.0(3) . . ? C56 C79 H79A 120.0 . . ? C86 C79 H79A 120.0 . . ? C91 C81 C58 118.8(3) . . ? C91 C81 C76 126.7(3) . . ? C58 C81 C76 114.4(3) . . ? C89 C82 C35 115.2(3) . . ? C89 C82 H82A 108.5 . . ? C35 C82 H82A 108.5 . . ? C89 C82 H82B 108.5 . . ? C35 C82 H82B 108.5 . . ? H82A C82 H82B 107.5 . . ? C93 C83 C57 120.3(3) . . ? C93 C83 H83A 119.8 . . ? C57 C83 H83A 119.8 . . ? C72 C86 C79 120.4(3) . . ? C72 C86 H86A 119.8 . . ? C79 C86 H86A 119.8 . . ? C67 C87 C95 119.9(3) . . ? C67 C87 H87A 120.0 . . ? C95 C87 H87A 120.0 . . ? C82 C89 C94 112.2(4) . . ? C82 C89 H89A 109.2 . . ? C94 C89 H89A 109.2 . . ? C82 C89 H89B 109.2 . . ? C94 C89 H89B 109.2 . . ? H89A C89 H89B 107.9 . . ? C93 C91 C81 120.8(4) . . ? C93 C91 H91A 119.6 . . ? C81 C91 H91A 119.6 . . ? C83 C93 C91 119.9(4) . . ? C83 C93 H93A 120.0 . . ? C91 C93 H93A 120.0 . . ? C89 C94 H94A 109.5 . . ? C89 C94 H94B 109.5 . . ? H94A C94 H94B 109.5 . . ? C89 C94 H94C 109.5 . . ? H94A C94 H94C 109.5 . . ? H94B C94 H94C 109.5 . . ? C78 C95 C87 120.6(3) . . ? C78 C95 H95A 119.7 . . ? C87 C95 H95A 119.7 . . ? C420 C410 C430 83.3(5) . . ? C420 C410 C76 128.3(4) . . ? C430 C410 C76 122.1(4) . . ? C420 C410 H41E 104.8 . . ? C430 C410 H41E 111.5 . . ? C76 C410 H41E 105.1 . . ? C420 C410 H41D 104.4 . . ? C430 C410 H41D 21.2 . . ? C76 C410 H41D 106.3 . . ? H41E C410 H41D 106.3 . . ? C420 C410 H41C 24.5 . . ? C430 C410 H41C 106.6 . . ? C76 C410 H41C 107.7 . . ? H41E C410 H41C 102.1 . . ? H41D C410 H41C 127.4 . . ? C410 C420 C450 118.1(6) . . ? C410 C420 H41C 38.5 . . ? C450 C420 H41C 142.2 . . ? C410 C420 H42C 106.5 . . ? C450 C420 H42C 107.7 . . ? H41C C420 H42C 70.0 . . ? C410 C420 H42D 106.9 . . ? C450 C420 H42D 109.9 . . ? H41C C420 H42D 106.4 . . ? H42C C420 H42D 107.2 . . ? C460 C450 C420 131.4(10) . . ? C460 C450 H45A 124.6 . . ? C420 C450 H45A 103.7 . . ? C460 C450 H45B 72.9 . . ? C420 C450 H45B 101.0 . . ? H45A C450 H45B 105.1 . . ? C460 C450 H46B 40.7 . . ? C420 C450 H46B 144.4 . . ? H45A C450 H46B 97.9 . . ? H45B C450 H46B 45.5 . . ? C450 C460 C470 119.2(11) . . ? C450 C460 H45B 41.5 . . ? C470 C460 H45B 120.6 . . ? C450 C460 H46B 23.0 . . ? C470 C460 H46B 107.6 . . ? H45B C460 H46B 27.3 . . ? C450 C460 H46C 117.4 . . ? C470 C460 H46C 108.7 . . ? H45B C460 H46C 80.6 . . ? H46B C460 H46C 107.7 . . ? C450 C460 H46A 98.7 . . ? C470 C460 H46A 111.9 . . ? H45B C460 H46A 124.9 . . ? H46B C460 H46A 121.6 . . ? H46C C460 H46A 98.4 . . ? C410 C430 C440 113.4(6) . . ? C410 C430 H41D 34.3 . . ? C440 C430 H41D 123.1 . . ? C410 C430 H43A 108.5 . . ? C440 C430 H43A 110.2 . . ? H41D C430 H43A 123.2 . . ? C410 C430 H43B 108.0 . . ? C440 C430 H43B 108.5 . . ? H41D C430 H43B 73.8 . . ? H43A C430 H43B 108.0 . . ? C465 C440 C430 125.9(10) . . ? C465 C440 H44A 121.0 . . ? C430 C440 H44A 108.3 . . ? C465 C440 H44B 78.4 . . ? C430 C440 H44B 108.3 . . ? H44A C440 H44B 107.1 . . ? C465 C440 H46A 42.2 . . ? C430 C440 H46A 125.5 . . ? H44A C440 H46A 89.3 . . ? H44B C440 H46A 114.9 . . ? C465 C440 H46D 38.6 . . ? C430 C440 H46D 124.7 . . ? H44A C440 H46D 122.7 . . ? H44B C440 H46D 39.9 . . ? H46A C440 H46D 77.9 . . ? C440 C465 C470 121.9(12) . . ? C440 C465 H46B 111.1 . . ? C470 C465 H46B 112.1 . . ? C440 C465 H44B 39.4 . . ? C470 C465 H44B 118.6 . . ? H46B C465 H44B 129.2 . . ? C440 C465 H46A 27.0 . . ? C470 C465 H46A 103.6 . . ? H46B C465 H46A 105.7 . . ? H44B C465 H46A 64.0 . . ? C440 C465 H46D 81.2 . . ? C470 C465 H46D 102.5 . . ? H46B C465 H46D 125.8 . . ? H44B C465 H46D 41.8 . . ? H46A C465 H46D 105.0 . . ? C480 C470 C465 118.1(8) . . ? C480 C470 C460 107.1(7) . . ? C465 C470 C460 24.9(8) . . ? C480 C470 H47D 106.6 . . ? C465 C470 H47D 108.7 . . ? C460 C470 H47D 133.1 . . ? C480 C470 H47E 108.1 . . ? C465 C470 H47E 107.5 . . ? C460 C470 H47E 92.0 . . ? H47D C470 H47E 107.4 . . ? C480 C470 H47C 110.0 . . ? C465 C470 H47C 86.1 . . ? C460 C470 H47C 110.9 . . ? H47D C470 H47C 25.1 . . ? H47E C470 H47C 126.3 . . ? C480 C470 H47B 110.1 . . ? C465 C470 H47B 120.2 . . ? C460 C470 H47B 109.7 . . ? H47D C470 H47B 87.9 . . ? H47E C470 H47B 20.2 . . ? H47C C470 H47B 109.0 . . ? C470 C480 H48B 111.5 . . ? C470 C480 H48C 108.4 . . ? H48B C480 H48C 109.5 . . ? C470 C480 H48D 108.5 . . ? H48B C480 H48D 109.5 . . ? H48C C480 H48D 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.208 _refine_diff_density_min -0.990 _refine_diff_density_rms 0.050 #===END data_TrisNHC _database_code_depnum_ccdc_archive 'CCDC 774044' #TrackingRef 'cif.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common tricarbene _chemical_melting_point ? _chemical_formula_moiety triscarbene _chemical_formula_sum 'C107 H134 N6' _chemical_formula_weight 1504.20 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 27.7357(15) _cell_length_b 20.3898(13) _cell_length_c 16.5894(11) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9381.7(10) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.065 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3272 _exptl_absorpt_coefficient_mu 0.061 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _exptl_special_details ; 'Squeeze' ; _diffrn_ambient_temperature 293(2) _diffrn_radiation_wavelength 0.71075 _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 80592 _diffrn_reflns_av_R_equivalents 0.1369 _diffrn_reflns_av_sigmaI/netI 0.1002 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_h_max 32 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 3.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8490 _reflns_number_gt 6303 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SHELXL-97 (Sheldrick, 1997)' _computing_cell_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_data_reduction 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_solution 'SHELXL-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 8490 _refine_ls_number_parameters 336 _refine_ls_number_restraints 242 _refine_ls_R_factor_all 0.1577 _refine_ls_R_factor_gt 0.1398 _refine_ls_wR_factor_ref 0.3314 _refine_ls_wR_factor_gt 0.3217 _refine_ls_goodness_of_fit_ref 1.962 _refine_ls_restrained_S_all 1.968 _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 C1 C 0.29970(9) 0.21599(12) 0.08096(16) 0.0334(6) Uani 1 1 d U . . N1 N 0.15454(9) 0.19724(13) 0.49562(15) 0.0421(6) Uani 1 1 d U . . C2 C 0.26221(9) 0.18060(13) 0.11687(17) 0.0349(6) Uani 1 1 d U . . H2A H 0.2620 0.1350 0.1164 0.042 Uiso 1 1 calc R . . N2 N 0.02862(7) 0.19654(11) 0.01155(14) 0.0345(5) Uani 1 1 d U . . C3 C 0.06908(9) 0.21598(12) 0.05563(16) 0.0309(6) Uani 1 1 d U . . N3 N 0.34032(7) 0.19678(12) 0.03436(15) 0.0355(6) Uani 1 1 d U . . C5 C 0.10488(9) 0.18087(13) 0.09727(16) 0.0318(6) Uani 1 1 d U . . H5A H 0.1052 0.1353 0.0965 0.038 Uiso 1 1 calc R . . C6 C 0.13932(9) 0.21502(12) 0.13905(16) 0.0314(6) Uani 1 1 d U . . C8 C 0.22615(9) 0.21517(12) 0.15241(16) 0.0331(6) Uani 1 1 d U . . C9 C 0.16049(9) 0.21538(13) 0.41589(17) 0.0364(7) Uani 1 1 d U . . C11 C 0.17413(9) 0.21562(12) 0.27318(17) 0.0337(6) Uani 1 1 d U . . C12 C 0.18040(9) 0.18450(13) 0.18967(18) 0.0348(6) Uani 1 1 d U . . C13 C 0.16759(9) 0.18060(13) 0.34446(16) 0.0318(6) Uani 1 1 d U . . H13A H 0.1679 0.1350 0.3444 0.038 Uiso 1 1 calc R . . C15 C 0.00291(13) 0.2500 -0.0157(3) 0.0410(10) Uani 1 2 d SU . . C16 C 0.35341(11) 0.12723(14) 0.0189(2) 0.0455(7) Uani 1 1 d U . . C17 C 0.14997(15) 0.2500 0.5451(3) 0.0446(10) Uani 1 2 d SU . . C18 C 0.36329(12) 0.09293(17) 0.0985(2) 0.0543(8) Uani 1 1 d U . . H18A H 0.3336 0.0877 0.1276 0.081 Uiso 1 1 calc R . . H18B H 0.3853 0.1188 0.1298 0.081 Uiso 1 1 calc R . . H18C H 0.3772 0.0506 0.0882 0.081 Uiso 1 1 calc R . . C19 C 0.31407(10) 0.09582(17) -0.0318(2) 0.0516(8) Uani 1 1 d U . . H19A H 0.2854 0.0911 0.0001 0.077 Uiso 1 1 calc R . . H19B H 0.3246 0.0534 -0.0498 0.077 Uiso 1 1 calc R . . H19C H 0.3074 0.1231 -0.0776 0.077 Uiso 1 1 calc R . . C20 C 0.15323(12) 0.12766(15) 0.5245(2) 0.0490(8) Uani 1 1 d U . . C21 C 0.36521(14) 0.2500 0.0043(3) 0.0422(9) Uani 1 2 d SU . . C22 C 0.01513(11) 0.12852(14) -0.0061(2) 0.0444(7) Uani 1 1 d U . . C23 C -0.03102(11) 0.12685(16) -0.0564(2) 0.0561(9) Uani 1 1 d U . . H23A H -0.0245 0.1440 -0.1092 0.084 Uiso 1 1 calc R . . H23B H -0.0553 0.1531 -0.0307 0.084 Uiso 1 1 calc R . . H23C H -0.0422 0.0824 -0.0609 0.084 Uiso 1 1 calc R . . C24 C 0.05497(11) 0.09570(15) -0.0544(2) 0.0513(8) Uani 1 1 d U . . H24A H 0.0578 0.1167 -0.1060 0.077 Uiso 1 1 calc R . . H24B H 0.0473 0.0502 -0.0620 0.077 Uiso 1 1 calc R . . H24C H 0.0849 0.0994 -0.0258 0.077 Uiso 1 1 calc R . . C25 C 0.11071(11) 0.09315(17) 0.4838(2) 0.0538(8) Uani 1 1 d U . . H25A H 0.1126 0.0994 0.4265 0.081 Uiso 1 1 calc R . . H25B H 0.0810 0.1113 0.5035 0.081 Uiso 1 1 calc R . . H25C H 0.1118 0.0471 0.4958 0.081 Uiso 1 1 calc R . . C28 C 0.00535(11) 0.09295(17) 0.0745(2) 0.0530(8) Uani 1 1 d U . . H28A H -0.0260 0.1049 0.0941 0.080 Uiso 1 1 calc R . . H28B H 0.0294 0.1054 0.1133 0.080 Uiso 1 1 calc R . . H28C H 0.0066 0.0464 0.0662 0.080 Uiso 1 1 calc R . . C29 C 0.40022(11) 0.12607(16) -0.0324(2) 0.0541(9) Uani 1 1 d U . . H29A H 0.4263 0.1445 -0.0017 0.081 Uiso 1 1 calc R . . H29B H 0.3955 0.1514 -0.0805 0.081 Uiso 1 1 calc R . . H29C H 0.4079 0.0816 -0.0465 0.081 Uiso 1 1 calc R . . C31 C 0.20142(13) 0.09554(17) 0.5044(2) 0.0573(8) Uani 1 1 d U . . H31A H 0.2052 0.0932 0.4470 0.086 Uiso 1 1 calc R . . H31B H 0.2023 0.0521 0.5267 0.086 Uiso 1 1 calc R . . H31C H 0.2272 0.1211 0.5269 0.086 Uiso 1 1 calc R . . C35 C 0.14390(16) 0.12658(19) 0.6164(2) 0.0655(10) Uani 1 1 d U . . H35A H 0.1726 0.1399 0.6443 0.098 Uiso 1 1 calc R . . H35B H 0.1352 0.0830 0.6327 0.098 Uiso 1 1 calc R . . H35C H 0.1181 0.1562 0.6291 0.098 Uiso 1 1 calc R . . C250 C 0.18064(10) 0.10971(13) 0.18938(18) 0.0379(6) Uani 1 1 d DU B . H25D H 0.1816 0.0953 0.1337 0.046 Uiso 1 1 calc R . . H25E H 0.1502 0.0949 0.2118 0.046 Uiso 1 1 calc R . . C251 C 0.22137(13) 0.07461(18) 0.2348(2) 0.0637(10) Uani 1 1 d DU . . H25H H 0.2327 0.1026 0.2773 0.076 Uiso 0.50 1 d PR A 2 H25I H 0.2478 0.0667 0.1986 0.076 Uiso 0.50 1 d PR A 2 H25F H 0.2121 0.0684 0.2900 0.076 Uiso 0.50 1 d PR A 1 H25G H 0.2498 0.1015 0.2338 0.076 Uiso 0.50 1 d PR A 1 C252 C 0.2322(2) 0.0083(3) 0.1981(5) 0.071(2) Uani 0.50 1 d PDU B 1 H25J H 0.2391 0.0144 0.1419 0.085 Uiso 0.50 1 d PR B 1 H25K H 0.2603 -0.0101 0.2232 0.085 Uiso 0.50 1 d PR B 1 C253 C 0.2050(3) 0.0103(3) 0.2693(5) 0.075(2) Uani 0.50 1 d PDU B 2 H25L H 0.2303 -0.0079 0.3019 0.090 Uiso 0.50 1 d PR B 2 H25M H 0.1777 0.0182 0.3036 0.090 Uiso 0.50 1 d PR B 2 C254 C 0.19117(18) -0.0388(2) 0.2056(4) 0.0999(17) Uani 1 1 d DU . . H25P H 0.2188 -0.0473 0.1724 0.120 Uiso 0.59 1 d PR B 2 H25N H 0.1672 -0.0260 0.1668 0.120 Uiso 1 1 d R . . H25O H 0.1774 -0.0313 0.2579 0.120 Uiso 0.41 1 d PR B 1 C255 C 0.1967(4) -0.1117(4) 0.1979(10) 0.101(4) Uani 0.41 1 d PDU B 1 H25Q H 0.2064 -0.1218 0.1437 0.121 Uiso 0.41 1 d PR B 1 H25R H 0.2218 -0.1261 0.2337 0.121 Uiso 0.41 1 d PR B 1 C256 C 0.1726(4) -0.1023(4) 0.2377(6) 0.111(3) Uani 0.59 1 d PDU B 2 H25S H 0.1956 -0.1200 0.2750 0.133 Uiso 0.59 1 d PR B 2 H25T H 0.1430 -0.0948 0.2663 0.133 Uiso 0.59 1 d PR B 2 C257 C 0.1637(4) -0.1528(4) 0.1690(7) 0.105(3) Uani 0.59 1 d PDU B 2 H25U H 0.1517 -0.1928 0.1920 0.157 Uiso 0.59 1 d PR B 2 H25X H 0.1405 -0.1357 0.1316 0.157 Uiso 0.59 1 d PR B 2 H25V H 0.1935 -0.1613 0.1414 0.157 Uiso 0.59 1 d PR B 2 C258 C 0.1485(5) -0.1467(7) 0.2196(11) 0.118(5) Uani 0.41 1 d PDU B 1 H25W H 0.1528 -0.1933 0.2144 0.177 Uiso 0.41 1 d PR B 1 H25Y H 0.1392 -0.1365 0.2739 0.177 Uiso 0.41 1 d PR B 1 H25Z H 0.1238 -0.1323 0.1831 0.177 Uiso 0.41 1 d PR B 1 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 0.0477(14) 0.0205(14) 0.0321(14) -0.0026(11) -0.0095(11) -0.0006(10) N1 0.0659(15) 0.0273(12) 0.0332(13) 0.0035(11) 0.0027(10) 0.0016(10) C2 0.0497(14) 0.0212(13) 0.0338(14) -0.0023(11) -0.0118(11) 0.0033(11) N2 0.0434(12) 0.0234(11) 0.0366(13) -0.0029(10) -0.0016(9) -0.0049(9) C3 0.0408(13) 0.0203(14) 0.0315(14) -0.0019(10) 0.0030(10) -0.0022(9) N3 0.0417(12) 0.0265(12) 0.0384(13) -0.0066(10) -0.0053(9) 0.0024(9) C5 0.0467(14) 0.0184(12) 0.0303(13) 0.0032(10) -0.0007(11) 0.0018(10) C6 0.0472(14) 0.0186(14) 0.0284(13) 0.0028(10) -0.0020(10) 0.0007(10) C8 0.0495(14) 0.0173(14) 0.0323(14) -0.0026(11) -0.0080(11) -0.0059(10) C9 0.0484(15) 0.0257(15) 0.0352(15) 0.0063(12) -0.0053(11) -0.0003(10) C11 0.0475(14) 0.0204(14) 0.0331(14) -0.0030(11) -0.0058(11) -0.0004(10) C12 0.0526(15) 0.0184(14) 0.0333(15) 0.0034(11) -0.0073(11) 0.0042(10) C13 0.0449(14) 0.0204(12) 0.0301(14) 0.0019(10) -0.0080(10) 0.0000(10) C15 0.045(2) 0.032(2) 0.046(2) 0.000 0.0000(17) 0.000 C16 0.0622(17) 0.0260(16) 0.0484(18) -0.0007(13) -0.0020(13) 0.0100(12) C17 0.067(2) 0.029(2) 0.037(2) 0.000 -0.0021(18) 0.000 C18 0.0674(18) 0.0392(19) 0.056(2) 0.0100(16) 0.0006(15) 0.0114(14) C19 0.0634(19) 0.0383(18) 0.053(2) -0.0167(15) 0.0016(14) -0.0048(13) C20 0.081(2) 0.0288(17) 0.0375(17) 0.0082(13) 0.0071(14) 0.0035(14) C21 0.053(2) 0.032(2) 0.042(2) 0.000 -0.0049(17) 0.000 C22 0.0594(16) 0.0273(16) 0.0464(18) -0.0018(13) -0.0007(13) -0.0098(12) C23 0.0611(17) 0.0387(19) 0.068(2) -0.0035(16) -0.0170(16) -0.0071(13) C24 0.0627(17) 0.0323(17) 0.059(2) -0.0155(15) -0.0046(15) -0.0043(13) C25 0.0692(19) 0.0410(19) 0.051(2) 0.0071(15) 0.0097(15) -0.0024(14) C28 0.0622(17) 0.0378(18) 0.059(2) 0.0083(16) -0.0022(15) -0.0145(14) C29 0.0642(18) 0.0388(19) 0.059(2) -0.0020(15) 0.0128(15) 0.0062(14) C31 0.083(2) 0.0410(19) 0.0479(19) 0.0085(16) -0.0041(16) 0.0028(16) C35 0.113(3) 0.043(2) 0.0404(19) 0.0118(16) 0.0035(18) -0.0013(18) C250 0.0585(16) 0.0154(14) 0.0399(15) -0.0011(12) -0.0014(12) -0.0004(11) C251 0.080(2) 0.051(2) 0.060(2) -0.0027(18) -0.0019(18) -0.0042(16) C252 0.077(4) 0.060(5) 0.076(5) -0.007(4) -0.014(4) 0.008(4) C253 0.074(4) 0.070(5) 0.080(5) 0.003(4) 0.004(4) -0.010(4) C254 0.115(3) 0.074(3) 0.111(4) -0.002(3) -0.026(3) 0.008(3) C255 0.116(7) 0.085(7) 0.101(8) -0.007(7) 0.007(6) -0.003(6) C256 0.125(6) 0.101(7) 0.105(7) 0.010(6) 0.010(5) 0.011(5) C257 0.109(5) 0.079(6) 0.127(7) -0.020(5) 0.004(5) -0.022(5) C258 0.125(8) 0.116(9) 0.113(9) 0.004(8) -0.005(7) -0.037(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 C1 C1 1.387(5) 8_565 ? C1 C2 1.399(4) . ? C1 N3 1.421(4) . ? N1 C17 1.359(4) . ? N1 C9 1.383(4) . ? N1 C20 1.498(4) . ? C2 C8 1.358(4) . ? C2 H2A 0.9300 . ? N2 C15 1.379(3) . ? N2 C3 1.397(3) . ? N2 C22 1.466(3) . ? C3 C3 1.387(5) 8_565 ? C3 C5 1.405(4) . ? N3 C21 1.379(3) . ? N3 C16 1.486(3) . ? C5 C6 1.370(4) . ? C5 H5A 0.9300 . ? C6 C6 1.426(5) 8_565 ? C6 C12 1.546(4) . ? C8 C8 1.420(5) 8_565 ? C8 C12 1.544(4) . ? C9 C13 1.395(4) . ? C9 C9 1.412(5) 8_565 ? C11 C13 1.393(4) . ? C11 C11 1.402(5) 8_565 ? C11 C12 1.534(4) . ? C12 C250 1.525(4) . ? C13 H13A 0.9300 . ? C15 N2 1.379(3) 8_565 ? C16 C18 1.518(5) . ? C16 C19 1.519(4) . ? C16 C29 1.552(4) . ? C17 N1 1.359(4) 8_565 ? 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 C31 1.525(5) . ? C20 C25 1.531(5) . ? C20 C35 1.546(5) . ? C21 N3 1.379(3) 8_565 ? C22 C24 1.520(4) . ? C22 C23 1.528(4) . ? C22 C28 1.545(4) . ? 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 . ? C28 H28A 0.9600 . ? C28 H28B 0.9600 . ? C28 H28C 0.9600 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C31 H31A 0.9600 . ? C31 H31B 0.9600 . ? C31 H31C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C250 C251 1.535(5) . ? C250 H25D 0.9700 . ? C250 H25E 0.9700 . ? C251 C253 1.501(6) . ? C251 C252 1.512(6) . ? C251 H25H 0.9599 . ? C251 H25I 0.9600 . ? C251 H25F 0.9599 . ? C251 H25G 0.9600 . ? C252 C254 1.494(6) . ? C252 H25I 1.2658 . ? C252 H25J 0.9600 . ? C252 H25K 0.9602 . ? C252 H25P 1.2678 . ? C253 C254 1.505(7) . ? C253 H25F 1.2483 . ? C253 H25L 0.9601 . ? C253 H25M 0.9602 . ? C253 H25O 1.1581 . ? C254 C256 1.492(7) . ? C254 C255 1.500(8) . ? C254 H25P 0.9601 . ? C254 H25N 0.9599 . ? C254 H25O 0.9600 . ? C255 C258 1.560(11) . ? C255 H25Q 0.9600 . ? C255 H25R 0.9599 . ? C255 H25S 1.2920 . ? C256 C257 1.556(10) . ? C256 H25S 0.9599 . ? C256 H25T 0.9601 . ? C257 H25U 0.9598 . ? C257 H25X 0.9600 . ? C257 H25V 0.9600 . ? C257 H25W 1.1572 . ? C257 H25Z 1.2061 . ? C258 H25U 1.0492 . ? C258 H25W 0.9600 . ? C258 H25Y 0.9599 . ? C258 H25Z 0.9599 . ? 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 C1 C1 C2 121.05(15) 8_565 . ? C1 C1 N3 106.00(14) 8_565 . ? C2 C1 N3 132.7(2) . . ? C17 N1 C9 112.1(3) . . ? C17 N1 C20 123.7(3) . . ? C9 N1 C20 124.2(3) . . ? C8 C2 C1 117.7(3) . . ? C8 C2 H2A 121.2 . . ? C1 C2 H2A 121.2 . . ? C15 N2 C3 111.3(2) . . ? C15 N2 C22 123.4(2) . . ? C3 N2 C22 125.3(2) . . ? C3 C3 N2 106.48(14) 8_565 . ? C3 C3 C5 120.62(15) 8_565 . ? N2 C3 C5 132.9(2) . . ? C21 N3 C1 112.1(2) . . ? C21 N3 C16 124.5(2) . . ? C1 N3 C16 123.4(2) . . ? C6 C5 C3 118.8(2) . . ? C6 C5 H5A 120.6 . . ? C3 C5 H5A 120.6 . . ? C5 C6 C6 120.54(15) . 8_565 ? C5 C6 C12 125.7(2) . . ? C6 C6 C12 113.73(14) 8_565 . ? C2 C8 C8 121.26(16) . 8_565 ? C2 C8 C12 124.7(2) . . ? C8 C8 C12 113.89(14) 8_565 . ? N1 C9 C13 133.9(3) . . ? N1 C9 C9 105.51(16) . 8_565 ? C13 C9 C9 120.56(16) . 8_565 ? C13 C11 C11 120.83(16) . 8_565 ? C13 C11 C12 124.7(2) . . ? C11 C11 C12 114.44(14) 8_565 . ? C250 C12 C11 114.7(2) . . ? C250 C12 C8 113.6(2) . . ? C11 C12 C8 106.7(2) . . ? C250 C12 C6 113.8(2) . . ? C11 C12 C6 103.9(2) . . ? C8 C12 C6 103.0(2) . . ? C11 C13 C9 118.6(2) . . ? C11 C13 H13A 120.7 . . ? C9 C13 H13A 120.7 . . ? N2 C15 N2 104.5(3) 8_565 . ? N3 C16 C18 109.5(3) . . ? N3 C16 C19 108.8(2) . . ? C18 C16 C19 114.6(3) . . ? N3 C16 C29 108.3(2) . . ? C18 C16 C29 108.6(3) . . ? C19 C16 C29 106.9(3) . . ? N1 C17 N1 104.7(4) 8_565 . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C16 C19 H19A 109.5 . . ? C16 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C16 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? N1 C20 C31 108.4(2) . . ? N1 C20 C25 108.2(3) . . ? C31 C20 C25 112.4(3) . . ? N1 C20 C35 109.4(3) . . ? C31 C20 C35 110.8(3) . . ? C25 C20 C35 107.4(3) . . ? N3 C21 N3 103.8(3) 8_565 . ? N2 C22 C24 109.6(2) . . ? N2 C22 C23 110.1(2) . . ? C24 C22 C23 108.1(3) . . ? N2 C22 C28 108.4(3) . . ? C24 C22 C28 112.1(3) . . ? C23 C22 C28 108.4(3) . . ? 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 . . ? C20 C25 H25A 109.5 . . ? C20 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C20 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C22 C28 H28A 109.5 . . ? C22 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C22 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C16 C29 H29A 109.5 . . ? C16 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C16 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C20 C31 H31A 109.5 . . ? C20 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C20 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C20 C35 H35A 109.5 . . ? C20 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C20 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C12 C250 C251 117.9(2) . . ? C12 C250 H25D 107.8 . . ? C251 C250 H25D 107.8 . . ? C12 C250 H25E 107.8 . . ? C251 C250 H25E 107.8 . . ? H25D C250 H25E 107.2 . . ? C253 C251 C252 55.4(5) . . ? C253 C251 C250 111.9(3) . . ? C252 C251 C250 111.4(4) . . ? C253 C251 H25H 109.7 . . ? C252 C251 H25H 139.6 . . ? C250 C251 H25H 108.9 . . ? C253 C251 H25I 108.8 . . ? C252 C251 H25I 56.4 . . ? C250 C251 H25I 109.5 . . ? H25H C251 H25I 108.0 . . ? C253 C251 H25F 55.9 . . ? C252 C251 H25F 108.6 . . ? C250 C251 H25F 109.4 . . ? H25H C251 H25F 57.6 . . ? H25I C251 H25F 141.1 . . ? C253 C251 H25G 138.8 . . ? C252 C251 H25G 110.0 . . ? C250 C251 H25G 109.2 . . ? H25H C251 H25G 53.4 . . ? H25I C251 H25G 57.3 . . ? H25F C251 H25G 108.1 . . ? C254 C252 C251 113.0(5) . . ? C254 C252 H25I 149.7 . . ? C251 C252 H25I 39.2 . . ? C254 C252 H25J 108.4 . . ? C251 C252 H25J 108.4 . . ? H25I C252 H25J 79.5 . . ? C254 C252 H25K 109.3 . . ? C251 C252 H25K 109.7 . . ? H25I C252 H25K 95.1 . . ? H25J C252 H25K 108.0 . . ? C254 C252 H25P 39.6 . . ? C251 C252 H25P 151.3 . . ? H25I C252 H25P 160.7 . . ? H25J C252 H25P 81.2 . . ? H25K C252 H25P 91.8 . . ? C251 C253 C254 112.9(5) . . ? C251 C253 H25F 39.5 . . ? C254 C253 H25F 149.7 . . ? C251 C253 H25L 109.4 . . ? C254 C253 H25L 108.9 . . ? H25F C253 H25L 95.6 . . ? C251 C253 H25M 108.6 . . ? C254 C253 H25M 109.0 . . ? H25F C253 H25M 78.6 . . ? H25L C253 H25M 107.9 . . ? C251 C253 H25O 141.0 . . ? C254 C253 H25O 39.6 . . ? H25F C253 H25O 147.5 . . ? H25L C253 H25O 107.0 . . ? H25M C253 H25O 72.4 . . ? C256 C254 C252 148.3(7) . . ? C256 C254 C255 37.4(6) . . ? C252 C254 C255 123.5(6) . . ? C256 C254 C253 114.5(6) . . ? C252 C254 C253 55.7(4) . . ? C255 C254 C253 133.8(8) . . ? C256 C254 H25P 108.8 . . ? C252 C254 H25P 57.4 . . ? C255 C254 H25P 71.8 . . ? C253 C254 H25P 108.6 . . ? C256 C254 H25N 103.6 . . ? C252 C254 H25N 107.3 . . ? C255 C254 H25N 106.4 . . ? C253 C254 H25N 117.9 . . ? H25P C254 H25N 102.5 . . ? C256 C254 H25O 71.2 . . ? C252 C254 H25O 106.0 . . ? C255 C254 H25O 106.0 . . ? C253 C254 H25O 50.3 . . ? H25P C254 H25O 149.8 . . ? H25N C254 H25O 106.8 . . ? C254 C255 C258 110.2(8) . . ? C254 C255 H25P 37.2 . . ? C258 C255 H25P 144.3 . . ? C254 C255 H25Q 108.8 . . ? C258 C255 H25Q 110.8 . . ? H25P C255 H25Q 79.2 . . ? C254 C255 H25R 108.9 . . ? C258 C255 H25R 109.8 . . ? H25P C255 H25R 98.3 . . ? H25Q C255 H25R 108.2 . . ? C254 C255 H25S 92.5 . . ? C258 C255 H25S 71.9 . . ? H25P C255 H25S 113.7 . . ? H25Q C255 H25S 155.0 . . ? H25R C255 H25S 50.5 . . ? C254 C255 H25V 141.0 . . ? C258 C255 H25V 76.4 . . ? H25P C255 H25V 118.3 . . ? H25Q C255 H25V 39.2 . . ? H25R C255 H25V 104.1 . . ? H25S C255 H25V 125.0 . . ? C254 C256 C257 111.6(7) . . ? C254 C256 H25O 37.5 . . ? C257 C256 H25O 145.2 . . ? C254 C256 H25R 87.1 . . ? C257 C256 H25R 83.9 . . ? H25O C256 H25R 104.5 . . ? C254 C256 H25S 109.1 . . ? C257 C256 H25S 109.1 . . ? H25O C256 H25S 99.3 . . ? H25R C256 H25S 43.8 . . ? C254 C256 H25T 109.5 . . ? C257 C256 H25T 109.3 . . ? H25O C256 H25T 79.2 . . ? H25R C256 H25T 151.8 . . ? H25S C256 H25T 108.1 . . ? C254 C256 H25Y 150.8 . . ? C257 C256 H25Y 82.6 . . ? H25O C256 H25Y 118.6 . . ? H25R C256 H25Y 120.7 . . ? H25S C256 H25Y 88.5 . . ? H25T C256 H25Y 41.5 . . ? C256 C257 H25Q 77.8 . . ? C256 C257 H25U 109.1 . . ? H25Q C257 H25U 142.4 . . ? C256 C257 H25X 109.8 . . ? H25Q C257 H25X 102.0 . . ? H25U C257 H25X 109.5 . . ? C256 C257 H25V 109.5 . . ? H25Q C257 H25V 38.2 . . ? H25U C257 H25V 109.5 . . ? H25X C257 H25V 109.5 . . ? C256 C257 H25W 92.2 . . ? H25Q C257 H25W 137.4 . . ? H25U C257 H25W 17.3 . . ? H25X C257 H25W 120.2 . . ? H25V C257 H25W 114.1 . . ? C256 C257 H25Z 77.0 . . ? H25Q C257 H25Z 132.5 . . ? H25U C257 H25Z 84.2 . . ? H25X C257 H25Z 52.0 . . ? H25V C257 H25Z 160.8 . . ? H25W C257 H25Z 83.1 . . ? C255 C258 H25T 82.4 . . ? C255 C258 H25U 103.6 . . ? H25T C258 H25U 169.7 . . ? C255 C258 H25X 80.3 . . ? H25T C258 H25X 115.8 . . ? H25U C258 H25X 73.8 . . ? C255 C258 H25W 109.0 . . ? H25T C258 H25W 149.2 . . ? H25U C258 H25W 20.8 . . ? H25X C258 H25W 94.6 . . ? C255 C258 H25Y 110.3 . . ? H25T C258 H25Y 40.8 . . ? H25U C258 H25Y 128.9 . . ? H25X C258 H25Y 147.6 . . ? H25W C258 H25Y 109.5 . . ? C255 C258 H25Z 109.1 . . ? H25T C258 H25Z 92.5 . . ? H25U C258 H25Z 93.4 . . ? H25X C258 H25Z 39.8 . . ? H25W C258 H25Z 109.5 . . ? H25Y C258 H25Z 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.435 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.082 #===END data_TrisThiourea _database_code_depnum_ccdc_archive 'CCDC 774045' #TrackingRef 'cif.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common Triscarbene-thiourea _chemical_melting_point ? _chemical_formula_moiety 'C59 H86 N6 S3, 2 C6 H6' _chemical_formula_sum 'C71 H98 N6 S3' _chemical_formula_weight 1131.73 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' _cell_length_a 23.074(3) _cell_length_b 19.486(2) _cell_length_c 14.463(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6502.9(14) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 50941 _cell_measurement_theta_min 2.0 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.07 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.156 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2456 _exptl_absorpt_coefficient_mu 0.159 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details none _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Rigaku AFC-12 with Saturn 724+ CCD' _diffrn_measurement_method \w-scans _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13457 _diffrn_reflns_av_R_equivalents 0.0920 _diffrn_reflns_av_sigmaI/netI 0.2235 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.77 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5870 _reflns_number_gt 3234 _reflns_threshold_expression >2sigma(I) _publ_section_references ; Altomare A., Burla M.C., Camalli M., Cascarano G.L., Giacovazzo C., Guagliardi A., Moliterni A.G.G., Polidori G.,Spagna R. Sir97. (1999) J. Appl. Cryst. 32, 115-119. Farrugia, L. J. (1999) J. Appl. Cryst., 32, 837-838. An Integrated System of Windows Programs for the Solution, Refinement and Analysis of Single Crystal X-ray Diffraction Data. Otwinowski, Z. and Minor, W. (1997). Methods in Enzymology, 276, Macromolecular Crystallography, part A, 307-326, C. W. Carter, Jr. and R. M. Sweets, Eds., Academic Press. Sheldrick, G. M. (2008). SHELXL-97. Acat Cryst., A64, 112-122. Spek, A. L. (1998) PLATON, A Multipurpose Crystallographic Tool, Utrecht University, Utrecht, The Netherlands. ; _publ_section_acknowledgements ; ; _computing_data_collection 'CrystalClear (Rigaku Inc., 2008)' _computing_cell_refinement 'CrystalClear (Rigaku Inc., 2008)' _computing_data_reduction 'CrystalClear (Rigaku Inc., 2008)' _computing_structure_solution ; ; _computing_structure_refinement 'XL SHELXTL/PC, Siemens Analytical' _computing_molecular_graphics 'XP SHELXTL/PC, Siemens Analytical' _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The space group was either the non-centrosymmetric space group, Pna21, or the centrosymmetric space group, Pnma. The intensity statistics indicated that the space group was Pna21. The refinement model in Pna21 revealed a disorder molecule where one of the three benzimidazole thione moities was disordered about two positions. The disorder model resulted in a pyramidal carbon atom bound to the sulfur atom. Such a result was chemically unlikely. The model was refined in the centrosymmetric space group, Pnma. In this space group, the disordered benzimidazole thione group in Pna21 was disordered by symmetry across the mirror plane of symmetry at y=1/4. In addition, the n-hexyl side chains were also disordered where C19, C21, C25 and C27 lie out of the mirror plane. The geometry of the disordered moiety was restrained so that equivalent bond lengths and angles were set so that they would not deviate too greatly from equivalency. The non-H atoms were refined anisotropically with their displacement parameters restrained to be approximately isotropic. ; _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^)+(0.0811P)^2^+24.8650P] 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 5870 _refine_ls_number_parameters 481 _refine_ls_number_restraints 418 _refine_ls_R_factor_all 0.2224 _refine_ls_R_factor_gt 0.1391 _refine_ls_wR_factor_ref 0.3295 _refine_ls_wR_factor_gt 0.2730 _refine_ls_goodness_of_fit_ref 1.162 _refine_ls_restrained_S_all 1.158 _refine_ls_shift/su_max 0.030 _refine_ls_shift/su_mean 0.007 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 S2 S 0.58208(10) -0.09392(11) 0.72847(15) 0.0489(6) Uani 1 1 d U . . N3 N 0.6400(2) 0.0165(3) 0.8001(4) 0.0276(14) Uani 1 1 d U . . N4 N 0.6380(2) 0.0128(3) 0.6457(4) 0.0275(14) Uani 1 1 d U . . C5 C 0.7447(3) 0.2500 0.8003(6) 0.017(2) Uani 1 2 d SU . . C6 C 0.7134(2) 0.1869(3) 0.7625(4) 0.0212(15) Uani 1 1 d U . . C7 C 0.6926(3) 0.1330(4) 0.8148(5) 0.0244(16) Uani 1 1 d U . . H7 H 0.6956 0.1335 0.8804 0.029 Uiso 1 1 calc R . . C8 C 0.6666(3) 0.0768(3) 0.7680(5) 0.0214(15) Uani 1 1 d U . . C9 C 0.6204(3) -0.0207(4) 0.7248(5) 0.0297(16) Uani 1 1 d U . . C10 C 0.6661(3) 0.0753(3) 0.6710(5) 0.0230(15) Uani 1 1 d U . . C11 C 0.6870(2) 0.1304(3) 0.6199(4) 0.0177(14) Uani 1 1 d U . . H11 H 0.6860 0.1292 0.5543 0.021 Uiso 1 1 calc R . . C12 C 0.7091(2) 0.1869(3) 0.6650(4) 0.0175(14) Uani 1 1 d U . . C13 C 0.7364(3) 0.2500 0.6179(6) 0.020(2) Uani 1 2 d SU . . C17 C 0.7512(4) 0.2500 0.9069(6) 0.023(2) Uani 1 2 d SU . . H17A H 0.7747 0.2093 0.9233 0.027 Uiso 0.50 1 d PR . . H17B H 0.7747 0.2908 0.9233 0.027 Uiso 0.50 1 d PR . . C18 C 0.6994(4) 0.2500 0.9709(7) 0.035(3) Uani 1 2 d SU . . H18A H 0.6673 0.2287 0.9399 0.042 Uiso 0.50 1 d PR . . H18B H 0.6888 0.2965 0.9849 0.042 Uiso 0.50 1 d PR . . C19 C 0.7117(7) 0.2116(8) 1.0636(10) 0.041(4) Uani 0.50 1 d PU . . H19A H 0.7250 0.1660 1.0502 0.049 Uiso 0.50 1 d PR . . H19B H 0.6769 0.2083 1.0996 0.049 Uiso 0.50 1 d PR . . C20 C 0.7582(5) 0.2500 1.1211(8) 0.046(3) Uani 1 2 d SU . . H20A H 0.7447 0.2950 1.1377 0.056 Uiso 0.50 1 d PR . . H20B H 0.7931 0.2500 1.0855 0.056 Uiso 1 2 d SR . . C21 C 0.7712(7) 0.2078(8) 1.2089(11) 0.047(4) Uani 0.50 1 d PU . . H21A H 0.7868 0.1638 1.1926 0.057 Uiso 0.50 1 d PR . . H21B H 0.7359 0.2013 1.2429 0.057 Uiso 0.50 1 d PR . . C22 C 0.8163(5) 0.2500 1.2675(8) 0.051(3) Uani 1 2 d SU . . H22C H 0.8525 0.2500 1.2351 0.077 Uiso 1 2 d SR . . H22A H 0.8220 0.2293 1.3271 0.077 Uiso 0.50 1 d PR . . H22B H 0.8026 0.2961 1.2763 0.077 Uiso 0.50 1 d PR . . C23 C 0.7320(4) 0.2500 0.5119(6) 0.019(2) Uani 1 2 d SU . . H23A H 0.7528 0.2091 0.4885 0.023 Uiso 0.50 1 d PR . . H23B H 0.7528 0.2909 0.4885 0.023 Uiso 0.50 1 d PR . . C24 C 0.6705(4) 0.2500 0.4690(6) 0.021(2) Uani 1 2 d SU . . H24A H 0.6444 0.2724 0.5108 0.025 Uiso 0.50 1 d PR . . H24B H 0.6577 0.2035 0.4616 0.025 Uiso 0.50 1 d PR . . C25 C 0.6667(5) 0.2840(7) 0.3764(9) 0.031(3) Uani 0.50 1 d PU . . H25A H 0.7026 0.2779 0.3440 0.038 Uiso 0.50 1 d PR . . H25B H 0.6602 0.3323 0.3848 0.038 Uiso 0.50 1 d PR . . C26 C 0.6130(5) 0.2500 0.3195(8) 0.055(3) Uani 1 2 d SU . . H26A H 0.6294 0.2136 0.2832 0.065 Uiso 0.50 1 d PR . . H26B H 0.5999 0.2843 0.2767 0.065 Uiso 0.50 1 d PR . . C27 C 0.5587(5) 0.2223(7) 0.3608(9) 0.029(3) Uani 0.50 1 d PU . . H27A H 0.5558 0.2376 0.4237 0.035 Uiso 0.50 1 d PR . . H27B H 0.5591 0.1730 0.3600 0.035 Uiso 0.50 1 d PR . . C28 C 0.5056(5) 0.2500 0.3029(9) 0.051(3) Uani 1 2 d SU . . H28C H 0.4705 0.2500 0.3384 0.076 Uiso 1 2 d SR . . H28A H 0.5009 0.2222 0.2486 0.076 Uiso 0.50 1 d PR . . H28B H 0.5144 0.2959 0.2835 0.076 Uiso 0.50 1 d PR . . C33 C 0.6319(3) -0.0068(4) 0.9002(5) 0.0369(19) Uani 1 1 d U . . C36 C 0.5657(3) -0.0089(5) 0.9216(6) 0.054(2) Uani 1 1 d U . . H36A H 0.5486 0.0362 0.9093 0.082 Uiso 1 1 calc R . . H36B H 0.5598 -0.0209 0.9867 0.082 Uiso 1 1 calc R . . H36C H 0.5471 -0.0435 0.8823 0.082 Uiso 1 1 calc R . . C34 C 0.6622(4) -0.0753(4) 0.9117(6) 0.055(2) Uani 1 1 d U . . H34A H 0.6481 -0.1074 0.8646 0.082 Uiso 1 1 calc R . . H34B H 0.6539 -0.0938 0.9733 0.082 Uiso 1 1 calc R . . H34C H 0.7041 -0.0690 0.9045 0.082 Uiso 1 1 calc R . . C35 C 0.6569(4) 0.0436(4) 0.9685(5) 0.044(2) Uani 1 1 d U . . H35A H 0.6984 0.0492 0.9567 0.066 Uiso 1 1 calc R . . H35B H 0.6510 0.0264 1.0315 0.066 Uiso 1 1 calc R . . H35C H 0.6374 0.0880 0.9616 0.066 Uiso 1 1 calc R . . C37 C 0.6313(3) -0.0146(4) 0.5478(5) 0.0343(18) Uani 1 1 d U . . C40 C 0.5655(5) -0.0203(7) 0.5292(8) 0.097(4) Uani 1 1 d U . . H40A H 0.5475 0.0250 0.5361 0.146 Uiso 1 1 calc R . . H40B H 0.5481 -0.0522 0.5736 0.146 Uiso 1 1 calc R . . H40C H 0.5591 -0.0372 0.4663 0.146 Uiso 1 1 calc R . . C38 C 0.6610(4) -0.0865(5) 0.5410(7) 0.073(3) Uani 1 1 d U . . H38A H 0.6589 -0.1032 0.4772 0.109 Uiso 1 1 calc R . . H38B H 0.6411 -0.1189 0.5819 0.109 Uiso 1 1 calc R . . H38C H 0.7017 -0.0826 0.5598 0.109 Uiso 1 1 calc R . . C39 C 0.6611(5) 0.0251(6) 0.4779(7) 0.093(4) Uani 1 1 d U . . H39A H 0.6458 0.0720 0.4774 0.140 Uiso 1 1 calc R . . H39B H 0.6550 0.0040 0.4172 0.140 Uiso 1 1 calc R . . H39C H 0.7027 0.0262 0.4918 0.140 Uiso 1 1 calc R . . C1A C 0.8306(5) 0.0520(6) 0.7182(7) 0.069(3) Uani 1 1 d U . . H1A H 0.8048 0.0900 0.7152 0.083 Uiso 1 1 calc R . . C2A C 0.8097(4) -0.0108(6) 0.7177(6) 0.062(3) Uani 1 1 d U . . H2A H 0.7690 -0.0182 0.7140 0.074 Uiso 1 1 calc R . . C3A C 0.8472(4) -0.0663(5) 0.7228(6) 0.053(2) Uani 1 1 d U . . H3A H 0.8321 -0.1116 0.7215 0.063 Uiso 1 1 calc R . . C4A C 0.9050(4) -0.0567(5) 0.7297(6) 0.052(2) Uani 1 1 d U . . H4A H 0.9301 -0.0951 0.7350 0.063 Uiso 1 1 calc R . . C5A C 0.9278(4) 0.0089(5) 0.7290(6) 0.062(3) Uani 1 1 d U . . H5A H 0.9684 0.0165 0.7325 0.074 Uiso 1 1 calc R . . C6A C 0.8890(5) 0.0634(5) 0.7230(7) 0.072(3) Uani 1 1 d U . . H6A H 0.9033 0.1091 0.7222 0.086 Uiso 1 1 calc R . . C14 C 0.7998(3) 0.2500 0.6548(6) 0.022(2) Uani 1 2 d SDU . . C4 C 0.8024(3) 0.2500 0.7505(6) 0.020(2) Uani 1 2 d SDU . . S1 S 1.06806(15) 0.2857(3) 0.6762(3) 0.0528(13) Uani 0.50 1 d PDU . -1 N2 N 0.9595(3) 0.2593(10) 0.6083(5) 0.024(3) Uani 0.50 1 d PDU . -1 N1 N 0.9665(3) 0.2611(6) 0.7620(5) 0.020(3) Uani 0.50 1 d PDU . -1 C15 C 0.8479(4) 0.252(2) 0.6004(7) 0.029(3) Uani 1 2 d SDU . -1 H15 H 0.8443 0.2503 0.5351 0.035 Uiso 1 2 calc SR . -1 C16 C 0.9029(3) 0.2565(13) 0.6415(6) 0.017(3) Uani 0.50 1 d PDU . -1 C1 C 0.9972(5) 0.2676(5) 0.6805(5) 0.025(4) Uani 0.50 1 d PDU . -1 C2 C 0.9076(3) 0.2582(7) 0.7438(5) 0.018(3) Uani 0.50 1 d PDU . -1 C3 C 0.8561(3) 0.2528(12) 0.7900(6) 0.026(2) Uani 0.50 1 d PDU . -1 H3 H 0.8578 0.2509 0.8556 0.031 Uiso 1 2 calc SR . -1 C41 C 0.9809(3) 0.2520(7) 0.5073(6) 0.030(2) Uani 1 2 d SDU . -1 C42 C 1.0081(6) 0.3197(8) 0.4773(9) 0.030(4) Uani 0.50 1 d PDU . -1 H42A H 1.0281 0.3135 0.4181 0.044 Uiso 0.50 1 calc PR . -1 H42B H 1.0361 0.3348 0.5242 0.044 Uiso 0.50 1 calc PR . -1 H42C H 0.9778 0.3545 0.4705 0.044 Uiso 0.50 1 calc PR . -1 C43 C 1.0253(5) 0.1942(8) 0.5027(11) 0.047(6) Uani 0.50 1 d PDU . -1 H43A H 1.0084 0.1522 0.5284 0.070 Uiso 0.50 1 calc PR . -1 H43B H 1.0597 0.2069 0.5386 0.070 Uiso 0.50 1 calc PR . -1 H43C H 1.0364 0.1863 0.4382 0.070 Uiso 0.50 1 calc PR . -1 C44 C 0.9294(4) 0.2350(7) 0.4451(6) 0.029(4) Uani 0.50 1 d PDU . -1 H44A H 0.9014 0.2728 0.4469 0.043 Uiso 0.50 1 calc PR . -1 H44B H 0.9108 0.1927 0.4669 0.043 Uiso 0.50 1 calc PR . -1 H44C H 0.9430 0.2284 0.3814 0.043 Uiso 0.50 1 calc PR . -1 C29 C 0.9944(3) 0.2516(6) 0.8585(6) 0.038(3) Uani 1 2 d SDU . -1 C30 C 1.0229(6) 0.3192(8) 0.8869(10) 0.047(5) Uani 0.50 1 d PDU . -1 H30A H 0.9948 0.3566 0.8814 0.071 Uiso 0.50 1 calc PR . -1 H30B H 1.0561 0.3284 0.8465 0.071 Uiso 0.50 1 calc PR . -1 H30C H 1.0362 0.3159 0.9511 0.071 Uiso 0.50 1 calc PR . -1 C31 C 1.0403(5) 0.1950(8) 0.8518(10) 0.049(5) Uani 0.50 1 d PDU . -1 H31A H 1.0542 0.1835 0.9139 0.074 Uiso 0.50 1 calc PR . -1 H31B H 1.0729 0.2113 0.8141 0.074 Uiso 0.50 1 calc PR . -1 H31C H 1.0233 0.1542 0.8230 0.074 Uiso 0.50 1 calc PR . -1 C32 C 0.9485(5) 0.2313(7) 0.9287(6) 0.040(5) Uani 0.50 1 d PDU . -1 H32A H 0.9672 0.2192 0.9874 0.060 Uiso 0.50 1 calc PR . -1 H32B H 0.9267 0.1916 0.9056 0.060 Uiso 0.50 1 calc PR . -1 H32C H 0.9219 0.2698 0.9386 0.060 Uiso 0.50 1 calc PR . -1 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 S2 0.0641(14) 0.0401(12) 0.0425(12) -0.0074(11) 0.0091(11) -0.0293(11) N3 0.033(3) 0.022(3) 0.028(3) -0.005(3) 0.008(3) -0.007(3) N4 0.033(3) 0.027(3) 0.023(3) -0.006(3) 0.002(3) -0.004(3) C5 0.014(4) 0.021(5) 0.016(4) 0.000 -0.004(3) 0.000 C6 0.016(3) 0.024(4) 0.024(3) 0.000(3) -0.007(3) 0.000(3) C7 0.023(3) 0.028(4) 0.023(3) -0.004(3) -0.002(3) 0.002(3) C8 0.019(3) 0.022(3) 0.024(3) 0.001(3) 0.005(3) 0.003(3) C9 0.031(3) 0.029(4) 0.029(4) -0.004(3) 0.007(3) 0.001(3) C10 0.021(3) 0.019(3) 0.028(4) -0.002(3) -0.009(3) 0.003(3) C11 0.013(3) 0.023(3) 0.017(3) -0.001(3) 0.004(3) 0.003(3) C12 0.008(3) 0.021(4) 0.023(3) 0.002(3) 0.001(3) -0.002(3) C13 0.009(4) 0.033(5) 0.018(4) 0.000 0.002(4) 0.000 C17 0.013(4) 0.026(5) 0.030(5) 0.000 0.001(4) 0.000 C18 0.031(5) 0.039(6) 0.035(5) 0.000 -0.007(4) 0.000 C19 0.046(7) 0.036(7) 0.039(7) 0.004(6) -0.003(6) -0.008(6) C20 0.053(6) 0.045(6) 0.041(6) 0.000 0.007(5) 0.000 C21 0.049(7) 0.056(8) 0.037(7) 0.001(7) -0.016(6) 0.002(7) C22 0.042(6) 0.063(7) 0.048(6) 0.000 0.002(5) 0.000 C23 0.019(4) 0.021(5) 0.018(4) 0.000 -0.006(4) 0.000 C24 0.019(4) 0.022(5) 0.023(5) 0.000 -0.002(4) 0.000 C25 0.022(6) 0.039(7) 0.034(7) 0.003(6) -0.001(5) -0.003(5) C26 0.044(6) 0.087(8) 0.033(6) 0.000 -0.006(5) 0.000 C27 0.027(5) 0.034(5) 0.027(5) -0.004(4) -0.007(4) -0.002(4) C28 0.047(6) 0.047(6) 0.059(7) 0.000 -0.019(5) 0.000 C33 0.050(4) 0.028(4) 0.033(4) 0.005(3) 0.002(3) -0.004(4) C36 0.053(5) 0.068(6) 0.043(5) -0.001(4) 0.019(4) -0.018(4) C34 0.075(5) 0.043(5) 0.046(5) 0.004(4) -0.013(4) -0.009(5) C35 0.069(5) 0.035(4) 0.027(4) 0.009(3) -0.010(4) -0.023(4) C37 0.036(4) 0.039(4) 0.028(4) -0.010(4) 0.000(3) -0.010(4) C40 0.097(7) 0.111(8) 0.084(7) -0.014(6) -0.025(6) 0.001(6) C38 0.079(6) 0.065(6) 0.074(6) -0.018(5) 0.020(5) 0.002(5) C39 0.122(7) 0.095(7) 0.063(6) -0.030(6) 0.021(6) -0.042(6) C1A 0.092(6) 0.068(6) 0.048(5) -0.003(5) 0.000(5) 0.042(6) C2A 0.054(5) 0.082(6) 0.049(5) 0.002(5) -0.008(4) 0.014(5) C3A 0.064(5) 0.055(5) 0.040(4) 0.010(4) -0.002(4) -0.005(4) C4A 0.054(5) 0.051(5) 0.052(5) 0.001(4) 0.001(4) 0.015(4) C5A 0.061(5) 0.074(6) 0.051(5) 0.001(5) 0.006(4) -0.001(5) C6A 0.108(7) 0.040(5) 0.067(6) 0.001(5) 0.020(6) 0.004(5) C14 0.016(4) 0.023(5) 0.027(5) 0.000 0.003(4) 0.000 C4 0.010(4) 0.019(4) 0.030(5) 0.000 -0.007(4) 0.000 S1 0.0186(17) 0.094(4) 0.046(2) 0.001(2) 0.0019(17) -0.0144(19) N2 0.018(4) 0.026(9) 0.028(4) 0.003(6) 0.004(3) 0.001(6) N1 0.016(3) 0.020(5) 0.024(4) 0.001(4) -0.007(3) -0.001(3) C15 0.024(5) 0.031(6) 0.033(5) 0.002(10) -0.004(4) -0.001(10) C16 0.012(3) 0.015(6) 0.024(4) -0.003(4) -0.002(3) -0.003(4) C1 0.015(5) 0.024(9) 0.034(6) -0.007(5) 0.004(5) 0.000(5) C2 0.018(4) 0.015(5) 0.023(4) 0.007(4) 0.002(3) 0.003(4) C3 0.028(5) 0.025(6) 0.025(5) -0.010(9) 0.004(4) -0.005(9) C41 0.025(5) 0.027(5) 0.038(5) -0.002(10) 0.009(4) -0.003(10) C42 0.027(7) 0.039(8) 0.023(7) 0.004(6) 0.010(6) -0.010(7) C43 0.042(8) 0.046(9) 0.051(9) -0.001(7) -0.002(7) -0.001(7) C44 0.034(6) 0.023(10) 0.030(6) -0.017(5) 0.000(5) 0.003(5) C29 0.032(5) 0.043(6) 0.039(6) 0.002(10) 0.001(5) 0.005(10) C30 0.037(8) 0.052(9) 0.052(9) -0.007(7) -0.014(7) -0.001(7) C31 0.045(8) 0.061(9) 0.041(8) -0.008(7) -0.016(7) 0.001(7) C32 0.040(6) 0.043(10) 0.038(6) 0.013(6) -0.004(5) 0.006(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 S2 C9 1.679(7) . ? N3 C9 1.386(9) . ? N3 C8 1.404(8) . ? N3 C33 1.529(9) . ? N4 C9 1.378(9) . ? N4 C10 1.427(8) . ? N4 C37 1.521(8) . ? C5 C4 1.513(12) . ? C5 C6 1.528(8) 8_565 ? C5 C6 1.528(8) . ? C5 C17 1.549(12) . ? C6 C7 1.380(9) . ? C6 C12 1.414(9) . ? C7 C8 1.421(9) . ? C7 H7 0.9500 . ? C8 C10 1.404(9) . ? C10 C11 1.390(9) . ? C11 C12 1.377(9) . ? C11 H11 0.9500 . ? C12 C13 1.541(8) . ? C13 C23 1.536(12) . ? C13 C12 1.541(8) 8_565 ? C13 C14 1.558(11) . ? C17 C18 1.511(13) . ? C17 H17A 0.9901 . ? C17 H17B 0.9901 . ? C18 C19 1.561(16) 8_565 ? C18 C19 1.561(16) . ? C18 H18A 0.9601 . ? C18 H18B 0.9601 . ? C19 C19 1.50(3) 8_565 ? C19 C20 1.550(17) . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C20 C19 1.550(17) 8_565 ? C20 C21 1.542(17) 8_565 ? C20 C21 1.542(17) . ? C20 H20A 0.9601 . ? C20 H20B 0.9560 . ? C21 C22 1.572(17) . ? C21 C21 1.64(3) 8_565 ? C21 H21A 0.9599 . ? C21 H21B 0.9601 . ? C22 C21 1.572(17) 8_565 ? C22 H22C 0.9596 . ? C22 H22A 0.9600 . ? C22 H22B 0.9600 . ? C23 C24 1.547(12) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 C25 1.497(15) 8_565 ? C24 C25 1.497(15) . ? C24 H24A 0.9599 . ? C24 H24B 0.9600 . ? C25 C25 1.33(3) 8_565 ? C25 C26 1.627(16) . ? C25 H25A 0.9600 . ? C25 H25B 0.9599 . ? C26 C27 1.491(16) . ? C26 C27 1.491(16) 8_565 ? C26 C25 1.627(16) 8_565 ? C26 H26A 0.9601 . ? C26 H26B 0.9601 . ? C27 C27 1.08(3) 8_565 ? C27 C28 1.579(15) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C28 C27 1.579(15) 8_565 ? C28 H28C 0.9599 . ? C28 H28A 0.9599 . ? C28 H28B 0.9600 . ? C33 C35 1.507(10) . ? C33 C34 1.517(11) . ? C33 C36 1.558(11) . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 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 . ? C37 C39 1.447(12) . ? C37 C40 1.546(12) . ? C37 C38 1.564(11) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 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 . ? C1A C2A 1.317(13) . ? C1A C6A 1.367(14) . ? C1A H1A 0.9500 . ? C2A C3A 1.387(12) . ? C2A H2A 0.9500 . ? C3A C4A 1.350(11) . ? C3A H3A 0.9500 . ? C4A C5A 1.382(12) . ? C4A H4A 0.9500 . ? C5A C6A 1.391(13) . ? C5A H5A 0.9500 . ? C6A H6A 0.9500 . ? C14 C15 1.360(9) . ? C14 C4 1.385(13) . ? C4 C3 1.366(8) 8_565 ? C4 C3 1.366(8) . ? S1 C1 1.673(11) . ? N2 C1 1.369(10) . ? N2 C16 1.394(9) . ? N2 C41 1.549(10) . ? N1 C1 1.380(10) . ? N1 C2 1.386(9) . ? N1 C29 1.547(10) . ? C15 C16 1.403(13) . ? C15 H15 0.9500 . ? C16 C2 1.485(12) . ? C2 C3 1.367(8) . ? C3 H3 0.9500 . ? C41 C43 1.524(8) . ? C41 C42 1.524(8) . ? C41 C44 1.527(8) . ? 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 . ? C29 C32 1.521(8) . ? C29 C30 1.529(8) . ? C29 C31 1.532(8) . ? 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 . ? 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 C9 N3 C8 108.7(6) . . ? C9 N3 C33 123.3(6) . . ? C8 N3 C33 128.0(6) . . ? C9 N4 C10 109.0(6) . . ? C9 N4 C37 125.2(6) . . ? C10 N4 C37 125.7(6) . . ? C4 C5 C6 104.2(5) . 8_565 ? C4 C5 C6 104.2(5) . . ? C6 C5 C6 107.2(7) 8_565 . ? C4 C5 C17 112.9(7) . . ? C6 C5 C17 113.7(5) 8_565 . ? C6 C5 C17 113.7(5) . . ? C7 C6 C12 121.5(6) . . ? C7 C6 C5 125.4(6) . . ? C12 C6 C5 113.0(6) . . ? C6 C7 C8 118.1(6) . . ? C6 C7 H7 120.9 . . ? C8 C7 H7 120.9 . . ? C10 C8 N3 108.0(6) . . ? C10 C8 C7 119.8(6) . . ? N3 C8 C7 132.2(6) . . ? N4 C9 N3 108.0(6) . . ? N4 C9 S2 125.7(6) . . ? N3 C9 S2 126.3(5) . . ? C11 C10 C8 120.8(6) . . ? C11 C10 N4 132.9(6) . . ? C8 C10 N4 106.1(6) . . ? C12 C11 C10 119.6(6) . . ? C12 C11 H11 120.2 . . ? C10 C11 H11 120.2 . . ? C11 C12 C6 119.9(6) . . ? C11 C12 C13 125.4(6) . . ? C6 C12 C13 114.4(6) . . ? C23 C13 C12 114.5(5) . 8_565 ? C23 C13 C12 114.5(5) . . ? C12 C13 C12 105.9(7) 8_565 . ? C23 C13 C14 113.9(7) . . ? C12 C13 C14 103.5(5) 8_565 . ? C12 C13 C14 103.5(5) . . ? C18 C17 C5 122.2(7) . . ? C18 C17 H17A 106.6 . . ? C5 C17 H17A 106.9 . . ? C18 C17 H17B 106.6 . . ? C5 C17 H17B 106.9 . . ? H17A C17 H17B 106.6 . . ? C17 C18 C19 112.5(9) . 8_565 ? C17 C18 C19 112.5(9) . . ? C19 C18 C19 57.3(12) 8_565 . ? C17 C18 H18A 108.9 . . ? C19 C18 H18A 138.4 8_565 . ? C19 C18 H18A 109.5 . . ? C17 C18 H18B 109.3 . . ? C19 C18 H18B 54.1 8_565 . ? C19 C18 H18B 108.6 . . ? H18A C18 H18B 107.9 . . ? C19 C19 C20 61.2(6) 8_565 . ? C19 C19 C18 61.4(6) 8_565 . ? C20 C19 C18 110.8(10) . . ? C19 C19 H19A 157.8 8_565 . ? C20 C19 H19A 109.5 . . ? C18 C19 H19A 109.1 . . ? C19 C19 H19B 93.9 8_565 . ? C20 C19 H19B 108.7 . . ? C18 C19 H19B 110.3 . . ? H19A C19 H19B 108.3 . . ? C19 C20 C19 57.7(12) . 8_565 ? C19 C20 C21 146.5(12) . 8_565 ? C19 C20 C21 108.7(9) 8_565 8_565 ? C19 C20 C21 108.7(9) . . ? C19 C20 C21 146.5(12) 8_565 . ? C21 C20 C21 64.4(13) 8_565 . ? C19 C20 H20A 110.5 . . ? C19 C20 H20A 58.0 8_565 . ? C21 C20 H20A 51.0 8_565 . ? C21 C20 H20A 110.1 . . ? C19 C20 H20B 107.1 . . ? C19 C20 H20B 107.1 8_565 . ? C21 C20 H20B 106.3 8_565 . ? C21 C20 H20B 106.3 . . ? H20A C20 H20B 114.1 . . ? C20 C21 C22 107.1(11) . . ? C20 C21 C21 57.8(7) . 8_565 ? C22 C21 C21 58.5(6) . 8_565 ? C20 C21 H21A 110.3 . . ? C22 C21 H21A 110.7 . . ? C21 C21 H21A 153.4 8_565 . ? C20 C21 H21B 109.0 . . ? C22 C21 H21B 110.7 . . ? C21 C21 H21B 97.6 8_565 . ? H21A C21 H21B 108.9 . . ? C21 C22 C21 63.0(12) 8_565 . ? C21 C22 H22C 108.3 8_565 . ? C21 C22 H22C 108.3 . . ? C21 C22 H22A 142.5 8_565 . ? C21 C22 H22A 110.8 . . ? H22C C22 H22A 108.6 . . ? C21 C22 H22B 50.7 8_565 . ? C21 C22 H22B 110.1 . . ? H22C C22 H22B 110.5 . . ? H22A C22 H22B 108.6 . . ? C13 C23 C24 117.5(7) . . ? C13 C23 H23A 108.0 . . ? C24 C23 H23A 107.9 . . ? C13 C23 H23B 108.0 . . ? C24 C23 H23B 107.9 . . ? H23A C23 H23B 107.3 . . ? C25 C24 C25 52.6(11) 8_565 . ? C25 C24 C23 114.4(8) 8_565 . ? C25 C24 C23 114.4(8) . . ? C25 C24 H24A 136.7 8_565 . ? C25 C24 H24A 108.9 . . ? C23 C24 H24A 108.9 . . ? C25 C24 H24B 57.5 8_565 . ? C25 C24 H24B 107.4 . . ? C23 C24 H24B 109.1 . . ? H24A C24 H24B 107.9 . . ? C25 C25 C24 63.7(6) 8_565 . ? C25 C25 C26 66.0(5) 8_565 . ? C24 C25 C26 108.5(9) . . ? C25 C25 H25A 82.8 8_565 . ? C24 C25 H25A 109.2 . . ? C26 C25 H25A 111.0 . . ? C25 C25 H25B 168.4 8_565 . ? C24 C25 H25B 109.3 . . ? C26 C25 H25B 110.1 . . ? H25A C25 H25B 108.6 . . ? C27 C26 C27 42.5(11) . 8_565 ? C27 C26 C25 125.8(11) . . ? C27 C26 C25 106.8(9) 8_565 . ? C27 C26 C25 106.8(9) . 8_565 ? C27 C26 C25 125.8(11) 8_565 8_565 ? C25 C26 C25 48.1(10) . 8_565 ? C27 C26 H26A 106.4 . . ? C27 C26 H26A 145.0 8_565 . ? C25 C26 H26A 106.1 . . ? C25 C26 H26A 71.1 8_565 . ? C27 C26 H26B 104.1 . . ? C27 C26 H26B 74.9 8_565 . ? C25 C26 H26B 106.5 . . ? C25 C26 H26B 148.3 8_565 . ? H26A C26 H26B 106.6 . . ? C27 C27 C26 68.7(5) 8_565 . ? C27 C27 C28 70.0(5) 8_565 . ? C26 C27 C28 108.4(10) . . ? C27 C27 H27A 71.8 8_565 . ? C26 C27 H27A 108.9 . . ? C28 C27 H27A 110.0 . . ? C27 C27 H27B 179.0 8_565 . ? C26 C27 H27B 110.3 . . ? C28 C27 H27B 110.1 . . ? H27A C27 H27B 109.0 . . ? C27 C28 C27 40.1(10) 8_565 . ? C27 C28 H28C 111.8 8_565 . ? C27 C28 H28C 111.8 . . ? C27 C28 H28A 135.6 8_565 . ? C27 C28 H28A 109.2 . . ? H28C C28 H28A 110.1 . . ? C27 C28 H28B 70.8 8_565 . ? C27 C28 H28B 108.0 . . ? H28C C28 H28B 109.6 . . ? H28A C28 H28B 108.1 . . ? C35 C33 C34 109.0(7) . . ? C35 C33 N3 112.3(6) . . ? C34 C33 N3 107.9(6) . . ? C35 C33 C36 105.3(7) . . ? C34 C33 C36 114.0(7) . . ? N3 C33 C36 108.5(6) . . ? 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 . . ? 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 . . ? C39 C37 N4 114.5(7) . . ? C39 C37 C40 112.6(9) . . ? N4 C37 C40 106.7(6) . . ? C39 C37 C38 103.1(8) . . ? N4 C37 C38 109.1(7) . . ? C40 C37 C38 110.8(8) . . ? 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 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C2A C1A C6A 120.8(10) . . ? C2A C1A H1A 119.6 . . ? C6A C1A H1A 119.6 . . ? C1A C2A C3A 119.7(9) . . ? C1A C2A H2A 120.2 . . ? C3A C2A H2A 120.2 . . ? C4A C3A C2A 120.9(9) . . ? C4A C3A H3A 119.6 . . ? C2A C3A H3A 119.6 . . ? C3A C4A C5A 120.2(9) . . ? C3A C4A H4A 119.9 . . ? C5A C4A H4A 119.9 . . ? C4A C5A C6A 117.5(9) . . ? C4A C5A H5A 121.3 . . ? C6A C5A H5A 121.3 . . ? C1A C6A C5A 120.9(10) . . ? C1A C6A H6A 119.5 . . ? C5A C6A H6A 119.5 . . ? C15 C14 C4 122.8(8) . . ? C15 C14 C13 124.6(8) . . ? C4 C14 C13 112.5(6) . . ? C3 C4 C3 5(2) 8_565 . ? C3 C4 C14 117.2(8) 8_565 . ? C3 C4 C14 117.2(8) . . ? C3 C4 C5 126.7(8) 8_565 . ? C3 C4 C5 126.7(8) . . ? C14 C4 C5 116.0(6) . . ? C1 N2 C16 109.8(8) . . ? C1 N2 C41 121.9(7) . . ? C16 N2 C41 128.3(7) . . ? C1 N1 C2 110.2(7) . . ? C1 N1 C29 124.6(7) . . ? C2 N1 C29 125.0(6) . . ? C14 C15 C16 119.6(9) . . ? C14 C15 H15 120.2 . . ? C16 C15 H15 120.2 . . ? N2 C16 C15 134.8(9) . . ? N2 C16 C2 105.9(7) . . ? C15 C16 C2 119.3(7) . . ? N2 C1 N1 108.3(9) . . ? N2 C1 S1 128.1(7) . . ? N1 C1 S1 123.5(6) . . ? C3 C2 N1 139.8(7) . . ? C3 C2 C16 114.9(6) . . ? N1 C2 C16 105.2(6) . . ? C4 C3 C2 126.0(8) . . ? C4 C3 H3 117.0 . . ? C2 C3 H3 117.0 . . ? C43 C41 C42 110.6(6) . . ? C43 C41 C44 109.7(6) . . ? C42 C41 C44 110.0(6) . . ? C43 C41 N2 108.9(6) . . ? C42 C41 N2 108.6(6) . . ? C44 C41 N2 109.1(5) . . ? C32 C29 C30 110.1(6) . . ? C32 C29 C31 109.7(6) . . ? C30 C29 C31 109.8(6) . . ? C32 C29 N1 110.2(6) . . ? C30 C29 N1 108.6(6) . . ? C31 C29 N1 108.5(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 C4 C5 C6 C7 122.5(7) . . . . ? C6 C5 C6 C7 -127.4(6) 8_565 . . . ? C17 C5 C6 C7 -0.9(9) . . . . ? C4 C5 C6 C12 -55.2(7) . . . . ? C6 C5 C6 C12 54.9(8) 8_565 . . . ? C17 C5 C6 C12 -178.6(6) . . . . ? C12 C6 C7 C8 0.1(9) . . . . ? C5 C6 C7 C8 -177.4(6) . . . . ? C9 N3 C8 C10 -3.1(7) . . . . ? C33 N3 C8 C10 177.7(6) . . . . ? C9 N3 C8 C7 178.6(7) . . . . ? C33 N3 C8 C7 -0.5(11) . . . . ? C6 C7 C8 C10 4.3(9) . . . . ? C6 C7 C8 N3 -177.6(6) . . . . ? C10 N4 C9 N3 -3.9(7) . . . . ? C37 N4 C9 N3 173.1(6) . . . . ? C10 N4 C9 S2 176.1(5) . . . . ? C37 N4 C9 S2 -6.8(10) . . . . ? C8 N3 C9 N4 4.3(7) . . . . ? C33 N3 C9 N4 -176.4(6) . . . . ? C8 N3 C9 S2 -175.7(5) . . . . ? C33 N3 C9 S2 3.5(10) . . . . ? N3 C8 C10 C11 176.6(5) . . . . ? C7 C8 C10 C11 -4.9(9) . . . . ? N3 C8 C10 N4 0.6(7) . . . . ? C7 C8 C10 N4 179.2(5) . . . . ? C9 N4 C10 C11 -173.2(7) . . . . ? C37 N4 C10 C11 9.8(11) . . . . ? C9 N4 C10 C8 2.0(7) . . . . ? C37 N4 C10 C8 -175.0(6) . . . . ? C8 C10 C11 C12 0.9(9) . . . . ? N4 C10 C11 C12 175.6(6) . . . . ? C10 C11 C12 C6 3.5(9) . . . . ? C10 C11 C12 C13 176.8(6) . . . . ? C7 C6 C12 C11 -4.0(9) . . . . ? C5 C6 C12 C11 173.7(5) . . . . ? C7 C6 C12 C13 -178.0(6) . . . . ? C5 C6 C12 C13 -0.2(8) . . . . ? C11 C12 C13 C23 6.2(9) . . . . ? C6 C12 C13 C23 179.8(6) . . . . ? C11 C12 C13 C12 133.3(5) . . . 8_565 ? C6 C12 C13 C12 -53.1(8) . . . 8_565 ? C11 C12 C13 C14 -118.2(7) . . . . ? C6 C12 C13 C14 55.3(7) . . . . ? C4 C5 C17 C18 180.000(2) . . . . ? C6 C5 C17 C18 61.5(5) 8_565 . . . ? C6 C5 C17 C18 -61.5(5) . . . . ? C5 C17 C18 C19 -148.8(7) . . . 8_565 ? C5 C17 C18 C19 148.8(7) . . . . ? C17 C18 C19 C19 103.1(6) . . . 8_565 ? C17 C18 C19 C20 65.7(11) . . . . ? C19 C18 C19 C20 -37.3(13) 8_565 . . . ? C18 C19 C20 C19 37.4(13) . . . 8_565 ? C19 C19 C20 C21 74.3(15) 8_565 . . 8_565 ? C18 C19 C20 C21 111.7(17) . . . 8_565 ? C19 C19 C20 C21 145.9(12) 8_565 . . . ? C18 C19 C20 C21 -176.7(11) . . . . ? C19 C20 C21 C22 -177.4(11) . . . . ? C19 C20 C21 C22 -118.2(16) 8_565 . . . ? C21 C20 C21 C22 -32.9(13) 8_565 . . . ? C19 C20 C21 C21 -144.5(12) . . . 8_565 ? C19 C20 C21 C21 -85.3(17) 8_565 . . 8_565 ? C20 C21 C22 C21 32.6(14) . . . 8_565 ? C12 C13 C23 C24 -61.2(5) 8_565 . . . ? C12 C13 C23 C24 61.2(5) . . . . ? C14 C13 C23 C24 180.000(1) . . . . ? C13 C23 C24 C25 -150.9(7) . . . 8_565 ? C13 C23 C24 C25 150.9(7) . . . . ? C23 C24 C25 C25 103.0(6) . . . 8_565 ? C25 C24 C25 C26 49.9(10) 8_565 . . . ? C23 C24 C25 C26 152.8(6) . . . . ? C25 C25 C26 C27 80.3(8) 8_565 . . . ? C24 C25 C26 C27 31.7(13) . . . . ? C25 C25 C26 C27 123.3(8) 8_565 . . 8_565 ? C24 C25 C26 C27 74.7(11) . . . 8_565 ? C24 C25 C26 C25 -48.6(10) . . . 8_565 ? C25 C26 C27 C27 75.0(8) . . . 8_565 ? C25 C26 C27 C27 125.1(8) 8_565 . . 8_565 ? C27 C26 C27 C28 58.9(9) 8_565 . . . ? C25 C26 C27 C28 133.9(9) . . . . ? C25 C26 C27 C28 -176.0(8) 8_565 . . . ? C26 C27 C28 C27 -58.1(9) . . . 8_565 ? C9 N3 C33 C35 -179.6(6) . . . . ? C8 N3 C33 C35 -0.5(10) . . . . ? C9 N3 C33 C34 60.3(9) . . . . ? C8 N3 C33 C34 -120.7(7) . . . . ? C9 N3 C33 C36 -63.6(9) . . . . ? C8 N3 C33 C36 115.4(8) . . . . ? C9 N4 C37 C39 -170.9(8) . . . . ? C10 N4 C37 C39 5.6(11) . . . . ? C9 N4 C37 C40 63.9(10) . . . . ? C10 N4 C37 C40 -119.6(8) . . . . ? C9 N4 C37 C38 -55.9(9) . . . . ? C10 N4 C37 C38 120.6(7) . . . . ? C6A C1A C2A C3A 0.5(16) . . . . ? C1A C2A C3A C4A 1.0(14) . . . . ? C2A C3A C4A C5A -1.9(14) . . . . ? C3A C4A C5A C6A 1.3(14) . . . . ? C2A C1A C6A C5A -1.0(16) . . . . ? C4A C5A C6A C1A 0.2(15) . . . . ? C23 C13 C14 C15 2(2) . . . . ? C12 C13 C14 C15 -123(2) 8_565 . . . ? C12 C13 C14 C15 127(2) . . . . ? C23 C13 C14 C4 180.000(1) . . . . ? C12 C13 C14 C4 55.1(4) 8_565 . . . ? C12 C13 C14 C4 -55.1(4) . . . . ? C15 C14 C4 C3 -5(2) . . . 8_565 ? C13 C14 C4 C3 177.4(11) . . . 8_565 ? C15 C14 C4 C3 1(3) . . . . ? C13 C14 C4 C3 -177.4(11) . . . . ? C15 C14 C4 C5 178(2) . . . . ? C13 C14 C4 C5 0.000(2) . . . . ? C6 C5 C4 C3 126.8(13) 8_565 . . 8_565 ? C6 C5 C4 C3 -121.0(13) . . . 8_565 ? C17 C5 C4 C3 2.9(13) . . . 8_565 ? C6 C5 C4 C3 121.0(13) 8_565 . . . ? C6 C5 C4 C3 -126.8(13) . . . . ? C17 C5 C4 C3 -2.9(13) . . . . ? C6 C5 C4 C14 -56.1(4) 8_565 . . . ? C6 C5 C4 C14 56.1(4) . . . . ? C17 C5 C4 C14 180.000(2) . . . . ? C4 C14 C15 C16 -2(4) . . . . ? C13 C14 C15 C16 176(2) . . . . ? C1 N2 C16 C15 177(3) . . . . ? C41 N2 C16 C15 -6(4) . . . . ? C1 N2 C16 C2 -4(2) . . . . ? C41 N2 C16 C2 173.4(14) . . . . ? C14 C15 C16 N2 180(3) . . . . ? C14 C15 C16 C2 1(4) . . . . ? C16 N2 C1 N1 7.8(18) . . . . ? C41 N2 C1 N1 -170.1(12) . . . . ? C16 N2 C1 S1 -169.7(13) . . . . ? C41 N2 C1 S1 12.3(19) . . . . ? C2 N1 C1 N2 -8.3(15) . . . . ? C29 N1 C1 N2 166.4(12) . . . . ? C2 N1 C1 S1 169.4(8) . . . . ? C29 N1 C1 S1 -15.9(15) . . . . ? C1 N1 C2 C3 -179.3(2) . . . . ? C29 N1 C2 C3 6.1(16) . . . . ? C1 N1 C2 C16 5.4(17) . . . . ? C29 N1 C2 C16 -169.3(14) . . . . ? N2 C16 C2 C3 -177.3(12) . . . . ? C15 C16 C2 C3 2(3) . . . . ? N2 C16 C2 N1 -1(2) . . . . ? C15 C16 C2 N1 179(2) . . . . ? C3 C4 C3 C2 93.7(13) 8_565 . . . ? C14 C4 C3 C2 2.5(18) . . . . ? C5 C4 C3 C2 -174.5(5) . . . . ? N1 C2 C3 C4 -179(2) . . . . ? C16 C2 C3 C4 -3.7(15) . . . . ? C1 N2 C41 C43 53.5(14) . . . . ? C16 N2 C41 C43 -124.1(19) . . . . ? C1 N2 C41 C42 -66.9(14) . . . . ? C16 N2 C41 C42 115.5(19) . . . . ? C1 N2 C41 C44 173.2(13) . . . . ? C16 N2 C41 C44 -4(2) . . . . ? C1 N1 C29 C32 -168.0(11) . . . . ? C2 N1 C29 C32 5.8(13) . . . . ? C1 N1 C29 C30 71.3(12) . . . . ? C2 N1 C29 C30 -114.8(12) . . . . ? C1 N1 C29 C31 -47.9(12) . . . . ? C2 N1 C29 C31 125.9(12) . . . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.668 _refine_diff_density_min -0.329 _refine_diff_density_rms 0.083 #===END