# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email cprao@iitb.ac.in _publ_contact_author_name 'Chebrolu Rao' _publ_author_name 'Chebrolu Rao' data_cpr108a _database_code_depnum_ccdc_archive 'CCDC 836001' #TrackingRef '- L_with_solvent_atoms.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C73.50 H75 N7.50 O6' _chemical_formula_weight 1159.41 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.6535(4) _cell_length_b 12.0093(4) _cell_length_c 22.2811(13) _cell_angle_alpha 87.280(4) _cell_angle_beta 83.524(4) _cell_angle_gamma 86.494(3) _cell_volume 3090.0(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5934 _cell_measurement_theta_min 3.2964 _cell_measurement_theta_max 32.7888 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.246 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1233 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_T_min 0.9741 _exptl_absorpt_correction_T_max 0.9834 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OXFORD DIFFRACTION XCALIBUR-S' _diffrn_measurement_method \w/q-scan _diffrn_detector_area_resol_mean 15.9948 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22396 _diffrn_reflns_av_R_equivalents 0.0677 _diffrn_reflns_av_sigmaI/netI 0.1396 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 3.30 _diffrn_reflns_theta_max 25.00 _reflns_number_total 10860 _reflns_number_gt 5056 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd.,' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd.,' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics Ortep3 _computing_publication_material Shelx97 _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^)+(0.1376P)^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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10860 _refine_ls_number_parameters 804 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1600 _refine_ls_R_factor_gt 0.0933 _refine_ls_wR_factor_ref 0.2536 _refine_ls_wR_factor_gt 0.2309 _refine_ls_goodness_of_fit_ref 0.927 _refine_ls_restrained_S_all 0.927 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.6861(2) 0.8939(3) 0.33740(13) 0.0309(8) Uani 1 1 d . . . O2 O 0.6101(3) 0.6634(3) 0.34562(15) 0.0336(8) Uani 1 1 d . . . O3 O 0.8790(2) 0.6359(2) 0.33609(13) 0.0308(7) Uani 1 1 d . . . O4 O 0.9504(3) 0.8642(3) 0.34553(13) 0.0340(8) Uani 1 1 d . . . H4 H 0.9767 0.8025 0.3591 0.051 Uiso 1 1 calc R . . O5 O 0.5509(3) 0.8173(3) 0.43322(15) 0.0468(9) Uani 1 1 d . . . O6 O 0.9766(3) 0.6949(3) 0.43207(15) 0.0466(9) Uani 1 1 d . . . N1 N 0.6433(3) 0.9082(3) 0.49854(17) 0.0378(10) Uani 1 1 d . . . H1 H 0.6939 0.9593 0.5000 0.045 Uiso 1 1 calc R . . N2 N 0.7490(3) 0.9495(4) 0.59525(18) 0.0440(11) Uani 1 1 d . . . N4 N 0.7118(4) 0.5340(4) 0.59481(18) 0.0451(11) Uani 1 1 d . . . C1 C 0.6686(4) 0.9618(4) 0.28705(19) 0.0257(10) Uani 1 1 d . . . C2 C 0.7456(3) 1.0402(4) 0.26252(19) 0.0264(10) Uani 1 1 d . . . C3 C 0.7202(4) 1.0990(4) 0.2097(2) 0.0287(11) Uani 1 1 d . . . H3 H 0.7711 1.1544 0.1934 0.034 Uiso 1 1 calc R . . C4 C 0.6257(4) 1.0819(4) 0.1794(2) 0.0292(11) Uani 1 1 d . . . C5 C 0.5517(3) 1.0024(4) 0.20606(19) 0.0268(10) Uani 1 1 d . . . H5 H 0.4856 0.9885 0.1868 0.032 Uiso 1 1 calc R . . C6 C 0.5694(4) 0.9424(4) 0.25916(19) 0.0257(10) Uani 1 1 d . . . C7 C 0.6015(4) 1.1430(4) 0.1197(2) 0.0320(11) Uani 1 1 d . . . C8 C 0.6982(4) 1.2202(4) 0.0969(2) 0.0413(13) Uani 1 1 d . . . H8A H 0.7024 1.2773 0.1265 0.062 Uiso 1 1 calc R . . H8B H 0.6820 1.2565 0.0582 0.062 Uiso 1 1 calc R . . H8C H 0.7722 1.1765 0.0915 0.062 Uiso 1 1 calc R . . C9 C 0.5933(4) 1.0581(4) 0.0722(2) 0.0423(13) Uani 1 1 d . . . H9A H 0.6656 1.0117 0.0670 0.063 Uiso 1 1 calc R . . H9B H 0.5802 1.0970 0.0338 0.063 Uiso 1 1 calc R . . H9C H 0.5289 1.0106 0.0853 0.063 Uiso 1 1 calc R . . C10 C 0.4893(4) 1.2153(4) 0.1291(2) 0.0416(13) Uani 1 1 d . . . H10A H 0.4248 1.1677 0.1418 0.062 Uiso 1 1 calc R . . H10B H 0.4756 1.2559 0.0911 0.062 Uiso 1 1 calc R . . H10C H 0.4952 1.2688 0.1603 0.062 Uiso 1 1 calc R . . C11 C 0.4876(4) 0.8527(4) 0.2834(2) 0.0296(11) Uani 1 1 d . . . H11A H 0.4853 0.8450 0.3279 0.035 Uiso 1 1 calc R . . H11B H 0.4085 0.8745 0.2733 0.035 Uiso 1 1 calc R . . C12 C 0.5941(3) 0.6607(4) 0.28665(19) 0.0254(10) Uani 1 1 d . . . C13 C 0.5280(3) 0.7422(4) 0.25593(19) 0.0256(10) Uani 1 1 d . . . C14 C 0.5077(4) 0.7246(4) 0.19808(19) 0.0278(10) Uani 1 1 d . . . H14 H 0.4609 0.7794 0.1785 0.033 Uiso 1 1 calc R . . C15 C 0.5511(4) 0.6315(4) 0.1659(2) 0.0291(10) Uani 1 1 d . . . C16 C 0.6203(4) 0.5545(4) 0.1967(2) 0.0278(10) Uani 1 1 d . . . H16 H 0.6534 0.4908 0.1762 0.033 Uiso 1 1 calc R . . C17 C 0.6430(3) 0.5663(4) 0.2557(2) 0.0273(10) Uani 1 1 d . . . C18 C 0.5191(4) 0.6137(4) 0.1028(2) 0.0344(11) Uani 1 1 d . . . C19 C 0.5128(6) 0.7245(5) 0.0651(2) 0.0611(17) Uani 1 1 d . . . H19A H 0.4547 0.7765 0.0855 0.092 Uiso 1 1 calc R . . H19B H 0.4913 0.7103 0.0250 0.092 Uiso 1 1 calc R . . H19C H 0.5885 0.7572 0.0608 0.092 Uiso 1 1 calc R . . C20 C 0.4005(5) 0.5657(6) 0.1093(3) 0.070(2) Uani 1 1 d . . . H20A H 0.4035 0.4938 0.1319 0.106 Uiso 1 1 calc R . . H20B H 0.3775 0.5549 0.0691 0.106 Uiso 1 1 calc R . . H20C H 0.3441 0.6175 0.1310 0.106 Uiso 1 1 calc R . . C21 C 0.6060(5) 0.5336(5) 0.0681(2) 0.0505(14) Uani 1 1 d . . . H21A H 0.6842 0.5591 0.0685 0.076 Uiso 1 1 calc R . . H21B H 0.5881 0.5316 0.0263 0.076 Uiso 1 1 calc R . . H21C H 0.6016 0.4586 0.0874 0.076 Uiso 1 1 calc R . . C22 C 0.7252(4) 0.4840(4) 0.28413(19) 0.0296(11) Uani 1 1 d . . . H22A H 0.7073 0.4073 0.2753 0.036 Uiso 1 1 calc R . . H22B H 0.7143 0.4908 0.3285 0.036 Uiso 1 1 calc R . . C23 C 0.9183(4) 0.5769(4) 0.28518(19) 0.0281(10) Uani 1 1 d . . . C24 C 0.8512(4) 0.5032(4) 0.2606(2) 0.0274(10) Uani 1 1 d . . . C25 C 0.8964(4) 0.4526(4) 0.2071(2) 0.0297(11) Uani 1 1 d . . . H25 H 0.8519 0.4004 0.1906 0.036 Uiso 1 1 calc R . . C26 C 1.0046(4) 0.4758(4) 0.1771(2) 0.0303(11) Uani 1 1 d . . . C27 C 1.0696(4) 0.5505(4) 0.20306(19) 0.0257(10) Uani 1 1 d . . . H27 H 1.1438 0.5674 0.1837 0.031 Uiso 1 1 calc R . . C28 C 1.0284(4) 0.6004(3) 0.2563(2) 0.0264(10) Uani 1 1 d . . . C29 C 1.0530(4) 0.4223(4) 0.1174(2) 0.0350(11) Uani 1 1 d . . . C30 C 0.9647(4) 0.3547(4) 0.0920(2) 0.0426(13) Uani 1 1 d . . . H30A H 0.9425 0.2934 0.1207 0.064 Uiso 1 1 calc R . . H30B H 0.9987 0.3241 0.0536 0.064 Uiso 1 1 calc R . . H30C H 0.8961 0.4030 0.0852 0.064 Uiso 1 1 calc R . . C31 C 1.1596(4) 0.3447(4) 0.1270(2) 0.0427(13) Uani 1 1 d . . . H31A H 1.1372 0.2839 0.1561 0.064 Uiso 1 1 calc R . . H31B H 1.2182 0.3872 0.1427 0.064 Uiso 1 1 calc R . . H31C H 1.1915 0.3135 0.0884 0.064 Uiso 1 1 calc R . . C32 C 1.0888(4) 0.5157(4) 0.0690(2) 0.0437(13) Uani 1 1 d . . . H32A H 1.1179 0.4816 0.0308 0.066 Uiso 1 1 calc R . . H32B H 1.1495 0.5578 0.0829 0.066 Uiso 1 1 calc R . . H32C H 1.0214 0.5663 0.0630 0.066 Uiso 1 1 calc R . . C33 C 1.0977(4) 0.6859(3) 0.2814(2) 0.0257(10) Uani 1 1 d . . . H33A H 1.1812 0.6660 0.2719 0.031 Uiso 1 1 calc R . . H33B H 1.0801 0.6855 0.3260 0.031 Uiso 1 1 calc R . . C34 C 0.9912(3) 0.8786(4) 0.2863(2) 0.0258(10) Uani 1 1 d . . . C35 C 1.0702(4) 0.8020(4) 0.25510(19) 0.0261(10) Uani 1 1 d . . . C36 C 1.1146(3) 0.8303(4) 0.19731(19) 0.0267(10) Uani 1 1 d . . . H36 H 1.1702 0.7796 0.1772 0.032 Uiso 1 1 calc R . . C37 C 1.0834(4) 0.9290(4) 0.1659(2) 0.0291(11) Uani 1 1 d . . . C38 C 1.0021(4) 1.0018(4) 0.19787(19) 0.0277(10) Uani 1 1 d . . . H38 H 0.9783 1.0699 0.1783 0.033 Uiso 1 1 calc R . . C39 C 0.9552(3) 0.9784(4) 0.2567(2) 0.0268(10) Uani 1 1 d . . . C40 C 1.1390(4) 0.9571(4) 0.1023(2) 0.0362(12) Uani 1 1 d . . . C41 C 1.1524(5) 0.8551(5) 0.0637(2) 0.0511(14) Uani 1 1 d . . . H41A H 1.2054 0.7989 0.0808 0.077 Uiso 1 1 calc R . . H41B H 1.1836 0.8768 0.0224 0.077 Uiso 1 1 calc R . . H41C H 1.0767 0.8240 0.0630 0.077 Uiso 1 1 calc R . . C42 C 1.2579(4) 1.0004(6) 0.1057(2) 0.0572(16) Uani 1 1 d . . . H42A H 1.2499 1.0686 0.1287 0.086 Uiso 1 1 calc R . . H42B H 1.2947 1.0170 0.0648 0.086 Uiso 1 1 calc R . . H42C H 1.3058 0.9436 0.1259 0.086 Uiso 1 1 calc R . . C43 C 1.0646(5) 1.0463(5) 0.0700(2) 0.0561(16) Uani 1 1 d . . . H43A H 0.9869 1.0198 0.0690 0.084 Uiso 1 1 calc R . . H43B H 1.1003 1.0601 0.0285 0.084 Uiso 1 1 calc R . . H43C H 1.0591 1.1157 0.0918 0.084 Uiso 1 1 calc R . . C44 C 0.8601(4) 1.0574(4) 0.2860(2) 0.0298(11) Uani 1 1 d . . . H44A H 0.8525 1.0439 0.3304 0.036 Uiso 1 1 calc R . . H44B H 0.8811 1.1356 0.2771 0.036 Uiso 1 1 calc R . . C45 C 0.6926(4) 0.9447(4) 0.3924(2) 0.0346(11) Uani 1 1 d . . . H45A H 0.6630 1.0235 0.3894 0.041 Uiso 1 1 calc R . . H45B H 0.7743 0.9435 0.4008 0.041 Uiso 1 1 calc R . . C46 C 0.6228(4) 0.8841(4) 0.4430(2) 0.0319(11) Uani 1 1 d . . . C47 C 0.5968(4) 0.8648(4) 0.5547(2) 0.0370(12) Uani 1 1 d . . . C48 C 0.4995(4) 0.8043(4) 0.5632(2) 0.0417(13) Uani 1 1 d . . . H48 H 0.4612 0.7881 0.5294 0.050 Uiso 1 1 calc R . . C49 C 0.4565(5) 0.7666(4) 0.6212(2) 0.0440(13) Uani 1 1 d . . . H49 H 0.3885 0.7259 0.6262 0.053 Uiso 1 1 calc R . . C50 C 0.5095(4) 0.7867(4) 0.6707(2) 0.0419(13) Uani 1 1 d . . . H50 H 0.4791 0.7595 0.7096 0.050 Uiso 1 1 calc R . . C51 C 0.6117(4) 0.8493(4) 0.6636(2) 0.0367(12) Uani 1 1 d . . . C52 C 0.6703(5) 0.8731(4) 0.7118(2) 0.0432(13) Uani 1 1 d . . . H52 H 0.6436 0.8473 0.7516 0.052 Uiso 1 1 calc R . . C53 C 0.7664(5) 0.9336(5) 0.7018(2) 0.0474(14) Uani 1 1 d . . . H53 H 0.8081 0.9504 0.7342 0.057 Uiso 1 1 calc R . . C54 C 0.8016(5) 0.9701(5) 0.6429(2) 0.0518(15) Uani 1 1 d . . . H54 H 0.8681 1.0128 0.6363 0.062 Uiso 1 1 calc R . . C55 C 0.6528(4) 0.8884(4) 0.6058(2) 0.0348(12) Uani 1 1 d . . . C56 C 0.8499(4) 0.5747(4) 0.3914(2) 0.0363(12) Uani 1 1 d . . . H56A H 0.8807 0.4964 0.3878 0.044 Uiso 1 1 calc R . . H56B H 0.7648 0.5747 0.4004 0.044 Uiso 1 1 calc R . . C57 C 0.9000(4) 0.6266(4) 0.4416(2) 0.0338(11) Uani 1 1 d . . . N3 N 0.8570(3) 0.5923(4) 0.49737(17) 0.0406(11) Uani 1 1 d . . . H3A H 0.8046 0.5422 0.4986 0.049 Uiso 1 1 calc R . . C58 C 0.8826(4) 0.6240(4) 0.5538(2) 0.0365(12) Uani 1 1 d . . . C59 C 0.9768(4) 0.6840(4) 0.5621(2) 0.0400(12) Uani 1 1 d . . . H59 H 1.0281 0.7075 0.5283 0.048 Uiso 1 1 calc R . . C60 C 0.9958(5) 0.7097(4) 0.6205(2) 0.0476(14) Uani 1 1 d . . . H60 H 1.0618 0.7494 0.6257 0.057 Uiso 1 1 calc R . . C61 C 0.9245(5) 0.6805(4) 0.6698(2) 0.0419(13) Uani 1 1 d . . . H61 H 0.9399 0.7001 0.7088 0.050 Uiso 1 1 calc R . . C62 C 0.8260(4) 0.6201(4) 0.6628(2) 0.0388(12) Uani 1 1 d . . . C63 C 0.7461(4) 0.5880(4) 0.7123(2) 0.0435(13) Uani 1 1 d . . . H63 H 0.7558 0.6074 0.7522 0.052 Uiso 1 1 calc R . . C64 C 0.6538(5) 0.5278(5) 0.7014(2) 0.0482(14) Uani 1 1 d . . . H64 H 0.5999 0.5028 0.7337 0.058 Uiso 1 1 calc R . . C65 C 0.6418(4) 0.5052(5) 0.6426(2) 0.0484(14) Uani 1 1 d . . . H65 H 0.5769 0.4650 0.6359 0.058 Uiso 1 1 calc R . . C66 C 0.8056(4) 0.5918(4) 0.6046(2) 0.0361(12) Uani 1 1 d . . . C111 C 0.8166(4) 0.7800(5) 0.1657(2) 0.0487(14) Uani 1 1 d . . . H11C H 0.7882 0.7115 0.1864 0.073 Uiso 1 1 calc R . . H11D H 0.7619 0.8430 0.1764 0.073 Uiso 1 1 calc R . . H11E H 0.8923 0.7939 0.1781 0.073 Uiso 1 1 calc R . . C222 C 0.8270(5) 0.7678(6) 0.1028(3) 0.0609(18) Uani 1 1 d . . . C333 C 1.0000 1.0000 0.5000 0.30(2) Uani 1 2 d S . . C444 C 0.9063(16) 1.0663(12) 0.4817(6) 0.175(6) Uani 1 1 d . . . C555 C 0.7145(14) 1.3872(12) 0.4641(6) 0.136(6) Uani 1 1 d . . . C666 C 0.596(3) 1.4404(13) 0.4820(8) 0.237(11) Uani 1 1 d . . . N222 N 0.8003(13) 1.1228(11) 0.4638(5) 0.168(6) Uani 1 1 d . . . N333 N 0.5000 1.5000 0.5000 0.44(3) Uani 1 2 d S . . N111 N 0.8368(6) 0.7523(7) 0.0523(3) 0.116(3) Uani 1 1 d . . . N555 N 0.7319(8) 1.2438(7) 0.5776(4) 0.120(3) Uani 1 1 d . . . C888 C 0.7632(12) 1.1824(17) 0.5181(9) 0.208(7) Uani 1 1 d . . . C777 C 0.7282(11) 1.3224(14) 0.5112(15) 0.281(15) Uani 1 1 d . . . H102 H 0.606(5) 0.725(6) 0.363(3) 0.07(2) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0298(17) 0.0303(19) 0.0319(18) 0.0009(14) -0.0015(13) -0.0005(14) O2 0.041(2) 0.027(2) 0.033(2) -0.0015(15) -0.0062(15) 0.0014(16) O3 0.0332(17) 0.0282(18) 0.0303(18) 0.0015(14) -0.0020(14) -0.0007(14) O4 0.0345(18) 0.0273(18) 0.038(2) 0.0038(14) -0.0009(15) 0.0033(14) O5 0.049(2) 0.049(2) 0.043(2) -0.0014(17) 0.0004(17) -0.0191(19) O6 0.052(2) 0.045(2) 0.046(2) 0.0078(17) -0.0110(17) -0.0177(19) N1 0.035(2) 0.049(3) 0.031(2) -0.0004(19) -0.0027(18) -0.016(2) N2 0.037(2) 0.049(3) 0.046(3) -0.001(2) -0.003(2) -0.008(2) N4 0.042(3) 0.050(3) 0.044(3) 0.004(2) -0.007(2) -0.010(2) C1 0.023(2) 0.024(2) 0.028(2) 0.0015(19) 0.0032(19) 0.0044(19) C2 0.023(2) 0.023(2) 0.033(3) -0.008(2) -0.0004(19) 0.0043(19) C3 0.026(2) 0.021(2) 0.037(3) 0.000(2) 0.003(2) -0.0002(19) C4 0.022(2) 0.024(3) 0.039(3) 0.000(2) 0.001(2) 0.002(2) C5 0.015(2) 0.030(3) 0.034(3) 0.001(2) 0.0001(18) 0.0000(19) C6 0.022(2) 0.023(2) 0.031(3) -0.0053(19) 0.0023(19) 0.0005(19) C7 0.027(2) 0.029(3) 0.037(3) 0.002(2) 0.003(2) 0.001(2) C8 0.034(3) 0.040(3) 0.050(3) 0.012(2) -0.007(2) -0.008(2) C9 0.047(3) 0.040(3) 0.039(3) 0.005(2) -0.004(2) -0.003(3) C10 0.038(3) 0.035(3) 0.051(3) 0.011(2) -0.007(2) 0.001(2) C11 0.027(2) 0.032(3) 0.031(3) 0.002(2) -0.0018(19) -0.010(2) C12 0.019(2) 0.029(3) 0.029(3) 0.0019(19) -0.0029(18) -0.0057(19) C13 0.017(2) 0.023(2) 0.035(3) 0.0008(19) -0.0006(19) 0.0015(18) C14 0.021(2) 0.029(3) 0.033(3) 0.004(2) -0.0038(19) 0.0021(19) C15 0.026(2) 0.027(3) 0.033(3) 0.003(2) -0.001(2) -0.003(2) C16 0.022(2) 0.023(2) 0.038(3) 0.002(2) -0.002(2) -0.0009(19) C17 0.019(2) 0.023(2) 0.039(3) -0.003(2) 0.0002(19) -0.0024(19) C18 0.033(3) 0.036(3) 0.035(3) -0.005(2) -0.007(2) 0.003(2) C19 0.085(4) 0.061(4) 0.036(3) 0.002(3) -0.017(3) 0.019(3) C20 0.041(3) 0.116(6) 0.059(4) -0.019(4) -0.014(3) -0.021(4) C21 0.058(3) 0.054(4) 0.039(3) -0.010(3) -0.009(3) 0.014(3) C22 0.031(2) 0.027(3) 0.032(3) 0.002(2) -0.006(2) -0.007(2) C23 0.032(3) 0.022(2) 0.030(3) 0.0015(19) -0.006(2) 0.004(2) C24 0.024(2) 0.023(3) 0.036(3) 0.005(2) -0.0052(19) -0.001(2) C25 0.027(2) 0.022(3) 0.041(3) 0.002(2) -0.007(2) -0.001(2) C26 0.026(2) 0.024(3) 0.039(3) 0.004(2) -0.002(2) 0.004(2) C27 0.023(2) 0.022(2) 0.032(3) 0.0035(19) -0.0075(19) 0.0008(19) C28 0.026(2) 0.016(2) 0.037(3) 0.0053(19) -0.007(2) -0.0012(19) C29 0.033(3) 0.031(3) 0.041(3) -0.004(2) -0.003(2) 0.005(2) C30 0.034(3) 0.041(3) 0.052(3) -0.005(3) -0.004(2) 0.002(2) C31 0.034(3) 0.038(3) 0.056(3) -0.011(2) -0.005(2) 0.008(2) C32 0.047(3) 0.050(4) 0.033(3) -0.003(2) -0.005(2) 0.002(3) C33 0.021(2) 0.020(2) 0.036(3) -0.0004(19) -0.0029(19) -0.0022(18) C34 0.019(2) 0.026(3) 0.034(3) 0.000(2) -0.0064(19) -0.0041(19) C35 0.023(2) 0.021(2) 0.036(3) -0.0012(19) -0.0083(19) -0.0023(19) C36 0.020(2) 0.022(2) 0.037(3) -0.002(2) -0.0011(19) 0.0044(19) C37 0.021(2) 0.026(3) 0.040(3) 0.000(2) -0.0023(19) -0.004(2) C38 0.027(2) 0.019(2) 0.036(3) 0.0020(19) -0.002(2) -0.0008(19) C39 0.021(2) 0.018(2) 0.043(3) -0.001(2) -0.012(2) 0.0002(18) C40 0.033(3) 0.038(3) 0.034(3) 0.005(2) 0.005(2) 0.005(2) C41 0.064(4) 0.048(4) 0.036(3) 0.001(2) 0.006(3) 0.005(3) C42 0.042(3) 0.086(5) 0.044(3) -0.002(3) 0.002(3) -0.018(3) C43 0.070(4) 0.050(4) 0.042(3) 0.013(3) 0.008(3) 0.012(3) C44 0.027(2) 0.021(2) 0.041(3) -0.001(2) -0.002(2) -0.002(2) C45 0.035(3) 0.034(3) 0.033(3) -0.002(2) 0.003(2) -0.001(2) C46 0.027(3) 0.031(3) 0.037(3) 0.000(2) -0.001(2) 0.001(2) C47 0.037(3) 0.036(3) 0.036(3) -0.002(2) 0.003(2) 0.003(2) C48 0.043(3) 0.034(3) 0.047(3) -0.006(2) 0.006(2) -0.008(2) C49 0.044(3) 0.036(3) 0.048(3) 0.004(2) 0.011(3) -0.004(2) C50 0.047(3) 0.035(3) 0.039(3) 0.004(2) 0.009(3) 0.007(2) C51 0.038(3) 0.033(3) 0.035(3) -0.003(2) 0.004(2) 0.015(2) C52 0.048(3) 0.042(3) 0.035(3) 0.003(2) 0.001(2) 0.016(3) C53 0.046(3) 0.056(4) 0.040(3) -0.010(3) -0.008(2) 0.009(3) C54 0.048(3) 0.064(4) 0.045(4) -0.004(3) -0.009(3) -0.006(3) C55 0.033(3) 0.029(3) 0.041(3) -0.003(2) 0.002(2) 0.006(2) C56 0.038(3) 0.037(3) 0.035(3) 0.003(2) -0.007(2) -0.004(2) C57 0.035(3) 0.027(3) 0.039(3) 0.008(2) -0.008(2) 0.002(2) N3 0.045(3) 0.047(3) 0.031(2) 0.0050(19) -0.0043(19) -0.019(2) C58 0.042(3) 0.035(3) 0.032(3) 0.004(2) -0.009(2) 0.004(2) C59 0.039(3) 0.037(3) 0.045(3) 0.007(2) -0.012(2) -0.006(2) C60 0.054(3) 0.038(3) 0.055(4) -0.004(3) -0.022(3) -0.005(3) C61 0.058(3) 0.036(3) 0.033(3) -0.003(2) -0.013(3) 0.008(3) C62 0.047(3) 0.028(3) 0.041(3) 0.005(2) -0.012(2) 0.012(2) C63 0.049(3) 0.041(3) 0.036(3) 0.003(2) 0.002(2) 0.020(3) C64 0.039(3) 0.055(4) 0.047(4) 0.009(3) 0.000(3) 0.013(3) C65 0.040(3) 0.063(4) 0.040(3) 0.010(3) 0.000(3) -0.004(3) C66 0.043(3) 0.030(3) 0.036(3) 0.003(2) -0.010(2) 0.006(2) C111 0.031(3) 0.053(4) 0.062(4) 0.001(3) 0.000(3) -0.011(3) C222 0.039(3) 0.092(5) 0.049(4) 0.007(3) 0.004(3) -0.007(3) C333 0.089(11) 0.39(4) 0.34(3) 0.25(3) 0.065(14) 0.157(18) C444 0.239(17) 0.136(12) 0.139(11) -0.020(9) 0.076(12) -0.090(12) C555 0.150(11) 0.101(10) 0.151(10) -0.048(8) 0.070(9) -0.089(10) C666 0.44(3) 0.140(13) 0.182(14) 0.065(12) -0.234(19) -0.117(17) N222 0.229(13) 0.142(9) 0.165(9) 0.066(7) -0.134(10) -0.122(9) N333 0.145(16) 0.59(6) 0.60(6) -0.27(4) -0.15(2) 0.28(3) N111 0.085(5) 0.184(8) 0.079(5) -0.012(5) 0.008(4) -0.035(5) N555 0.163(8) 0.084(6) 0.114(6) 0.001(5) -0.011(5) -0.016(5) C888 0.132(11) 0.26(2) 0.247(18) -0.079(17) -0.049(12) -0.025(12) C777 0.083(8) 0.095(12) 0.65(5) -0.067(18) 0.056(18) -0.003(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.381(5) . ? O1 C45 1.406(5) . ? O2 C12 1.350(5) . ? O2 H102 0.84(7) . ? O3 C23 1.385(5) . ? O3 C56 1.423(5) . ? O4 C34 1.358(5) . ? O4 H4 0.8400 . ? O5 C46 1.239(5) . ? O6 C57 1.243(5) . ? N1 C46 1.334(6) . ? N1 C47 1.397(6) . ? N1 H1 0.8800 . ? N2 C54 1.324(7) . ? N2 C55 1.370(6) . ? N4 C65 1.312(6) . ? N4 C66 1.373(6) . ? C1 C2 1.391(6) . ? C1 C6 1.409(6) . ? C2 C3 1.395(6) . ? C2 C44 1.516(6) . ? C3 C4 1.386(6) . ? C3 H3 0.9500 . ? C4 C5 1.392(6) . ? C4 C7 1.534(6) . ? C5 C6 1.385(6) . ? C5 H5 0.9500 . ? C6 C11 1.522(6) . ? C7 C9 1.518(7) . ? C7 C10 1.525(6) . ? C7 C8 1.530(6) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 C13 1.514(6) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.408(6) . ? C12 C17 1.412(6) . ? C13 C14 1.365(6) . ? C14 C15 1.396(6) . ? C14 H14 0.9500 . ? C15 C16 1.396(6) . ? C15 C18 1.522(6) . ? C16 C17 1.385(6) . ? C16 H16 0.9500 . ? C17 C22 1.502(6) . ? C18 C20 1.519(7) . ? C18 C21 1.524(7) . ? C18 C19 1.542(7) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.530(6) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.386(6) . ? C23 C28 1.408(6) . ? C24 C25 1.398(6) . ? C25 C26 1.396(6) . ? C25 H25 0.9500 . ? C26 C27 1.395(6) . ? C26 C29 1.538(6) . ? C27 C28 1.379(6) . ? C27 H27 0.9500 . ? C28 C33 1.509(6) . ? C29 C30 1.522(7) . ? C29 C31 1.536(7) . ? C29 C32 1.561(7) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 C35 1.516(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 C39 1.404(6) . ? C34 C35 1.411(6) . ? C35 C36 1.368(6) . ? C36 C37 1.397(6) . ? C36 H36 0.9500 . ? C37 C38 1.405(6) . ? C37 C40 1.523(6) . ? C38 C39 1.386(6) . ? C38 H38 0.9500 . ? C39 C44 1.523(6) . ? C40 C41 1.519(7) . ? C40 C42 1.521(7) . ? C40 C43 1.540(7) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.500(6) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C47 C48 1.375(7) . ? C47 C55 1.421(7) . ? C48 C49 1.397(6) . ? C48 H48 0.9500 . ? C49 C50 1.361(7) . ? C49 H49 0.9500 . ? C50 C51 1.437(7) . ? C50 H50 0.9500 . ? C51 C52 1.386(7) . ? C51 C55 1.392(6) . ? C52 C53 1.364(7) . ? C52 H52 0.9500 . ? C53 C54 1.390(7) . ? C53 H53 0.9500 . ? C54 H54 0.9500 . ? C56 C57 1.496(7) . ? C56 H56A 0.9900 . ? C56 H56B 0.9900 . ? C57 N3 1.341(6) . ? N3 C58 1.400(6) . ? N3 H3A 0.8800 . ? C58 C59 1.384(7) . ? C58 C66 1.416(6) . ? C59 C60 1.396(7) . ? C59 H59 0.9500 . ? C60 C61 1.346(7) . ? C60 H60 0.9500 . ? C61 C62 1.422(7) . ? C61 H61 0.9500 . ? C62 C66 1.406(7) . ? C62 C63 1.415(7) . ? C63 C64 1.382(7) . ? C63 H63 0.9500 . ? C64 C65 1.374(7) . ? C64 H64 0.9500 . ? C65 H65 0.9500 . ? C111 C222 1.406(8) . ? C111 H11C 0.9800 . ? C111 H11D 0.9800 . ? C111 H11E 0.9800 . ? C222 N111 1.142(8) . ? C333 C444 1.40(2) 2_776 ? C333 C444 1.40(2) . ? C444 N222 1.46(2) . ? C555 C777 1.29(3) . ? C555 C666 1.50(3) . ? C666 N333 1.33(3) . ? N222 C888 1.446(19) . ? N333 C666 1.33(3) 2_686 ? N555 C888 1.543(19) . ? N555 C777 1.72(3) . ? C888 C777 1.71(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 O1 C45 118.3(4) . . ? C12 O2 H102 120(4) . . ? C23 O3 C56 118.3(4) . . ? C34 O4 H4 109.5 . . ? C46 N1 C47 129.9(4) . . ? C46 N1 H1 115.1 . . ? C47 N1 H1 115.1 . . ? C54 N2 C55 116.7(4) . . ? C65 N4 C66 116.9(4) . . ? O1 C1 C2 123.5(4) . . ? O1 C1 C6 115.5(3) . . ? C2 C1 C6 121.0(4) . . ? C1 C2 C3 117.4(4) . . ? C1 C2 C44 124.1(4) . . ? C3 C2 C44 118.2(4) . . ? C4 C3 C2 124.3(4) . . ? C4 C3 H3 117.9 . . ? C2 C3 H3 117.9 . . ? C3 C4 C5 115.7(4) . . ? C3 C4 C7 123.9(4) . . ? C5 C4 C7 120.4(4) . . ? C6 C5 C4 123.5(4) . . ? C6 C5 H5 118.3 . . ? C4 C5 H5 118.3 . . ? C5 C6 C1 118.1(4) . . ? C5 C6 C11 120.0(4) . . ? C1 C6 C11 121.8(4) . . ? C9 C7 C10 110.3(4) . . ? C9 C7 C8 108.7(4) . . ? C10 C7 C8 107.4(4) . . ? C9 C7 C4 109.4(4) . . ? C10 C7 C4 109.9(4) . . ? C8 C7 C4 111.1(4) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C7 C10 H10A 109.5 . . ? C7 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C7 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C13 C11 C6 110.0(3) . . ? C13 C11 H11A 109.7 . . ? C6 C11 H11A 109.7 . . ? C13 C11 H11B 109.7 . . ? C6 C11 H11B 109.7 . . ? H11A C11 H11B 108.2 . . ? O2 C12 C13 124.3(4) . . ? O2 C12 C17 116.4(4) . . ? C13 C12 C17 119.2(4) . . ? C14 C13 C12 119.0(4) . . ? C14 C13 C11 119.1(4) . . ? C12 C13 C11 121.7(4) . . ? C13 C14 C15 124.2(4) . . ? C13 C14 H14 117.9 . . ? C15 C14 H14 117.9 . . ? C14 C15 C16 115.3(4) . . ? C14 C15 C18 121.5(4) . . ? C16 C15 C18 123.1(4) . . ? C17 C16 C15 123.5(4) . . ? C17 C16 H16 118.3 . . ? C15 C16 H16 118.3 . . ? C16 C17 C12 118.7(4) . . ? C16 C17 C22 120.1(4) . . ? C12 C17 C22 121.1(4) . . ? C20 C18 C15 108.1(4) . . ? C20 C18 C21 109.1(4) . . ? C15 C18 C21 111.9(4) . . ? C20 C18 C19 108.3(5) . . ? C15 C18 C19 111.5(4) . . ? C21 C18 C19 107.8(4) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C17 C22 C24 111.8(3) . . ? C17 C22 H22A 109.3 . . ? C24 C22 H22A 109.3 . . ? C17 C22 H22B 109.3 . . ? C24 C22 H22B 109.3 . . ? H22A C22 H22B 107.9 . . ? O3 C23 C24 122.7(4) . . ? O3 C23 C28 116.8(4) . . ? C24 C23 C28 120.4(4) . . ? C23 C24 C25 118.2(4) . . ? C23 C24 C22 123.9(4) . . ? C25 C24 C22 117.4(4) . . ? C26 C25 C24 122.5(4) . . ? C26 C25 H25 118.7 . . ? C24 C25 H25 118.7 . . ? C27 C26 C25 117.7(4) . . ? C27 C26 C29 119.9(4) . . ? C25 C26 C29 122.5(4) . . ? C28 C27 C26 121.3(4) . . ? C28 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C27 C28 C23 119.9(4) . . ? C27 C28 C33 120.1(4) . . ? C23 C28 C33 119.9(4) . . ? C30 C29 C31 108.3(4) . . ? C30 C29 C26 112.5(4) . . ? C31 C29 C26 110.2(4) . . ? C30 C29 C32 107.4(4) . . ? C31 C29 C32 108.9(4) . . ? C26 C29 C32 109.5(4) . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C29 C32 H32A 109.5 . . ? C29 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C29 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C28 C33 C35 111.2(4) . . ? C28 C33 H33A 109.4 . . ? C35 C33 H33A 109.4 . . ? C28 C33 H33B 109.4 . . ? C35 C33 H33B 109.4 . . ? H33A C33 H33B 108.0 . . ? O4 C34 C39 116.6(4) . . ? O4 C34 C35 123.4(4) . . ? C39 C34 C35 119.9(4) . . ? C36 C35 C34 118.4(4) . . ? C36 C35 C33 119.4(4) . . ? C34 C35 C33 121.9(4) . . ? C35 C36 C37 124.2(4) . . ? C35 C36 H36 117.9 . . ? C37 C36 H36 117.9 . . ? C36 C37 C38 115.7(4) . . ? C36 C37 C40 121.5(4) . . ? C38 C37 C40 122.7(4) . . ? C39 C38 C37 122.8(4) . . ? C39 C38 H38 118.6 . . ? C37 C38 H38 118.6 . . ? C38 C39 C34 118.9(4) . . ? C38 C39 C44 119.1(4) . . ? C34 C39 C44 121.8(4) . . ? C41 C40 C42 108.8(4) . . ? C41 C40 C37 111.3(4) . . ? C42 C40 C37 109.2(4) . . ? C41 C40 C43 107.0(4) . . ? C42 C40 C43 109.2(4) . . ? C37 C40 C43 111.2(4) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C2 C44 C39 110.7(4) . . ? C2 C44 H44A 109.5 . . ? C39 C44 H44A 109.5 . . ? C2 C44 H44B 109.5 . . ? C39 C44 H44B 109.5 . . ? H44A C44 H44B 108.1 . . ? O1 C45 C46 110.3(4) . . ? O1 C45 H45A 109.6 . . ? C46 C45 H45A 109.6 . . ? O1 C45 H45B 109.6 . . ? C46 C45 H45B 109.6 . . ? H45A C45 H45B 108.1 . . ? O5 C46 N1 123.1(4) . . ? O5 C46 C45 121.6(4) . . ? N1 C46 C45 115.3(4) . . ? C48 C47 N1 123.9(5) . . ? C48 C47 C55 119.0(4) . . ? N1 C47 C55 117.1(4) . . ? C47 C48 C49 120.3(5) . . ? C47 C48 H48 119.9 . . ? C49 C48 H48 119.9 . . ? C50 C49 C48 121.8(5) . . ? C50 C49 H49 119.1 . . ? C48 C49 H49 119.1 . . ? C49 C50 C51 119.5(4) . . ? C49 C50 H50 120.3 . . ? C51 C50 H50 120.3 . . ? C52 C51 C55 118.8(5) . . ? C52 C51 C50 122.8(4) . . ? C55 C51 C50 118.4(5) . . ? C53 C52 C51 119.7(5) . . ? C53 C52 H52 120.1 . . ? C51 C52 H52 120.1 . . ? C52 C53 C54 118.0(5) . . ? C52 C53 H53 121.0 . . ? C54 C53 H53 121.0 . . ? N2 C54 C53 124.7(5) . . ? N2 C54 H54 117.7 . . ? C53 C54 H54 117.7 . . ? N2 C55 C51 122.0(5) . . ? N2 C55 C47 117.0(4) . . ? C51 C55 C47 121.0(4) . . ? O3 C56 C57 109.8(4) . . ? O3 C56 H56A 109.7 . . ? C57 C56 H56A 109.7 . . ? O3 C56 H56B 109.7 . . ? C57 C56 H56B 109.7 . . ? H56A C56 H56B 108.2 . . ? O6 C57 N3 123.0(4) . . ? O6 C57 C56 122.2(4) . . ? N3 C57 C56 114.8(4) . . ? C57 N3 C58 129.9(4) . . ? C57 N3 H3A 115.0 . . ? C58 N3 H3A 115.0 . . ? C59 C58 N3 123.9(4) . . ? C59 C58 C66 119.5(4) . . ? N3 C58 C66 116.6(4) . . ? C58 C59 C60 119.4(5) . . ? C58 C59 H59 120.3 . . ? C60 C59 H59 120.3 . . ? C61 C60 C59 122.7(5) . . ? C61 C60 H60 118.6 . . ? C59 C60 H60 118.6 . . ? C60 C61 C62 119.3(5) . . ? C60 C61 H61 120.4 . . ? C62 C61 H61 120.4 . . ? C66 C62 C63 118.2(5) . . ? C66 C62 C61 119.2(4) . . ? C63 C62 C61 122.6(5) . . ? C64 C63 C62 118.6(5) . . ? C64 C63 H63 120.7 . . ? C62 C63 H63 120.7 . . ? C65 C64 C63 118.3(5) . . ? C65 C64 H64 120.9 . . ? C63 C64 H64 120.9 . . ? N4 C65 C64 126.0(5) . . ? N4 C65 H65 117.0 . . ? C64 C65 H65 117.0 . . ? N4 C66 C62 122.0(4) . . ? N4 C66 C58 118.1(4) . . ? C62 C66 C58 119.9(5) . . ? C222 C111 H11C 109.5 . . ? C222 C111 H11D 109.5 . . ? H11C C111 H11D 109.5 . . ? C222 C111 H11E 109.5 . . ? H11C C111 H11E 109.5 . . ? H11D C111 H11E 109.5 . . ? N111 C222 C111 176.5(8) . . ? C444 C333 C444 180.0(11) 2_776 . ? C333 C444 N222 172.7(10) . . ? C777 C555 C666 100.9(11) . . ? N333 C666 C555 171.7(12) . . ? C888 N222 C444 99.3(10) . . ? C666 N333 C666 180.000(5) 2_686 . ? C888 N555 C777 62.9(9) . . ? N222 C888 N555 176.0(15) . . ? N222 C888 C777 118.4(19) . . ? N555 C888 C777 63.6(14) . . ? C555 C777 C888 131(2) . . ? C555 C777 N555 173.4(16) . . ? C888 C777 N555 53.5(11) . . ? 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 C45 O1 C1 C2 61.8(5) . . . . ? C45 O1 C1 C6 -121.7(4) . . . . ? O1 C1 C2 C3 176.7(4) . . . . ? C6 C1 C2 C3 0.3(6) . . . . ? O1 C1 C2 C44 2.9(6) . . . . ? C6 C1 C2 C44 -173.4(4) . . . . ? C1 C2 C3 C4 -1.9(6) . . . . ? C44 C2 C3 C4 172.2(4) . . . . ? C2 C3 C4 C5 1.9(6) . . . . ? C2 C3 C4 C7 -177.0(4) . . . . ? C3 C4 C5 C6 -0.4(6) . . . . ? C7 C4 C5 C6 178.6(4) . . . . ? C4 C5 C6 C1 -1.1(7) . . . . ? C4 C5 C6 C11 -176.8(4) . . . . ? O1 C1 C6 C5 -175.5(4) . . . . ? C2 C1 C6 C5 1.1(6) . . . . ? O1 C1 C6 C11 0.1(6) . . . . ? C2 C1 C6 C11 176.7(4) . . . . ? C3 C4 C7 C9 122.7(5) . . . . ? C5 C4 C7 C9 -56.1(5) . . . . ? C3 C4 C7 C10 -116.0(5) . . . . ? C5 C4 C7 C10 65.1(6) . . . . ? C3 C4 C7 C8 2.7(6) . . . . ? C5 C4 C7 C8 -176.1(4) . . . . ? C5 C6 C11 C13 87.5(5) . . . . ? C1 C6 C11 C13 -88.0(5) . . . . ? O2 C12 C13 C14 -173.0(4) . . . . ? C17 C12 C13 C14 3.5(6) . . . . ? O2 C12 C13 C11 12.2(6) . . . . ? C17 C12 C13 C11 -171.2(4) . . . . ? C6 C11 C13 C14 -77.2(5) . . . . ? C6 C11 C13 C12 97.5(5) . . . . ? C12 C13 C14 C15 -1.9(6) . . . . ? C11 C13 C14 C15 173.0(4) . . . . ? C13 C14 C15 C16 -0.7(6) . . . . ? C13 C14 C15 C18 176.3(4) . . . . ? C14 C15 C16 C17 1.7(6) . . . . ? C18 C15 C16 C17 -175.2(4) . . . . ? C15 C16 C17 C12 0.0(6) . . . . ? C15 C16 C17 C22 -175.6(4) . . . . ? O2 C12 C17 C16 174.2(4) . . . . ? C13 C12 C17 C16 -2.6(6) . . . . ? O2 C12 C17 C22 -10.3(5) . . . . ? C13 C12 C17 C22 172.9(4) . . . . ? C14 C15 C18 C20 -80.2(5) . . . . ? C16 C15 C18 C20 96.5(5) . . . . ? C14 C15 C18 C21 159.6(4) . . . . ? C16 C15 C18 C21 -23.7(6) . . . . ? C14 C15 C18 C19 38.8(6) . . . . ? C16 C15 C18 C19 -144.6(4) . . . . ? C16 C17 C22 C24 75.3(5) . . . . ? C12 C17 C22 C24 -100.1(5) . . . . ? C56 O3 C23 C24 62.3(6) . . . . ? C56 O3 C23 C28 -121.7(4) . . . . ? O3 C23 C24 C25 176.4(4) . . . . ? C28 C23 C24 C25 0.6(7) . . . . ? O3 C23 C24 C22 4.0(7) . . . . ? C28 C23 C24 C22 -171.9(4) . . . . ? C17 C22 C24 C23 86.7(5) . . . . ? C17 C22 C24 C25 -85.7(5) . . . . ? C23 C24 C25 C26 -1.7(7) . . . . ? C22 C24 C25 C26 171.3(4) . . . . ? C24 C25 C26 C27 1.6(7) . . . . ? C24 C25 C26 C29 -178.5(4) . . . . ? C25 C26 C27 C28 -0.4(7) . . . . ? C29 C26 C27 C28 179.6(4) . . . . ? C26 C27 C28 C23 -0.6(7) . . . . ? C26 C27 C28 C33 -176.4(4) . . . . ? O3 C23 C28 C27 -175.5(4) . . . . ? C24 C23 C28 C27 0.5(7) . . . . ? O3 C23 C28 C33 0.3(6) . . . . ? C24 C23 C28 C33 176.4(4) . . . . ? C27 C26 C29 C30 -172.9(4) . . . . ? C25 C26 C29 C30 7.1(6) . . . . ? C27 C26 C29 C31 66.2(6) . . . . ? C25 C26 C29 C31 -113.8(5) . . . . ? C27 C26 C29 C32 -53.6(6) . . . . ? C25 C26 C29 C32 126.4(5) . . . . ? C27 C28 C33 C35 87.0(5) . . . . ? C23 C28 C33 C35 -88.9(5) . . . . ? O4 C34 C35 C36 -173.4(4) . . . . ? C39 C34 C35 C36 3.5(6) . . . . ? O4 C34 C35 C33 12.6(6) . . . . ? C39 C34 C35 C33 -170.5(4) . . . . ? C28 C33 C35 C36 -75.9(5) . . . . ? C28 C33 C35 C34 98.1(5) . . . . ? C34 C35 C36 C37 -2.6(6) . . . . ? C33 C35 C36 C37 171.5(4) . . . . ? C35 C36 C37 C38 0.8(6) . . . . ? C35 C36 C37 C40 178.1(4) . . . . ? C36 C37 C38 C39 0.1(6) . . . . ? C40 C37 C38 C39 -177.1(4) . . . . ? C37 C38 C39 C34 0.9(6) . . . . ? C37 C38 C39 C44 -174.9(4) . . . . ? O4 C34 C39 C38 174.4(4) . . . . ? C35 C34 C39 C38 -2.7(6) . . . . ? O4 C34 C39 C44 -9.9(6) . . . . ? C35 C34 C39 C44 172.9(4) . . . . ? C36 C37 C40 C41 41.8(6) . . . . ? C38 C37 C40 C41 -141.2(5) . . . . ? C36 C37 C40 C42 -78.4(6) . . . . ? C38 C37 C40 C42 98.6(5) . . . . ? C36 C37 C40 C43 161.0(5) . . . . ? C38 C37 C40 C43 -22.0(6) . . . . ? C1 C2 C44 C39 86.8(5) . . . . ? C3 C2 C44 C39 -86.9(5) . . . . ? C38 C39 C44 C2 76.5(5) . . . . ? C34 C39 C44 C2 -99.2(5) . . . . ? C1 O1 C45 C46 135.6(4) . . . . ? C47 N1 C46 O5 2.7(8) . . . . ? C47 N1 C46 C45 -177.7(5) . . . . ? O1 C45 C46 O5 -15.1(6) . . . . ? O1 C45 C46 N1 165.3(4) . . . . ? C46 N1 C47 C48 -15.2(8) . . . . ? C46 N1 C47 C55 166.8(5) . . . . ? N1 C47 C48 C49 -178.1(5) . . . . ? C55 C47 C48 C49 -0.1(7) . . . . ? C47 C48 C49 C50 -0.9(8) . . . . ? C48 C49 C50 C51 0.7(8) . . . . ? C49 C50 C51 C52 180.0(5) . . . . ? C49 C50 C51 C55 0.5(7) . . . . ? C55 C51 C52 C53 -0.1(7) . . . . ? C50 C51 C52 C53 -179.6(5) . . . . ? C51 C52 C53 C54 0.4(8) . . . . ? C55 N2 C54 C53 0.4(8) . . . . ? C52 C53 C54 N2 -0.6(9) . . . . ? C54 N2 C55 C51 -0.1(7) . . . . ? C54 N2 C55 C47 -179.2(5) . . . . ? C52 C51 C55 N2 -0.1(7) . . . . ? C50 C51 C55 N2 179.4(4) . . . . ? C52 C51 C55 C47 179.0(4) . . . . ? C50 C51 C55 C47 -1.5(7) . . . . ? C48 C47 C55 N2 -179.6(4) . . . . ? N1 C47 C55 N2 -1.4(7) . . . . ? C48 C47 C55 C51 1.3(7) . . . . ? N1 C47 C55 C51 179.4(4) . . . . ? C23 O3 C56 C57 134.7(4) . . . . ? O3 C56 C57 O6 -15.4(7) . . . . ? O3 C56 C57 N3 165.5(4) . . . . ? O6 C57 N3 C58 1.8(8) . . . . ? C56 C57 N3 C58 -179.1(5) . . . . ? C57 N3 C58 C59 -13.1(8) . . . . ? C57 N3 C58 C66 166.7(5) . . . . ? N3 C58 C59 C60 -178.8(5) . . . . ? C66 C58 C59 C60 1.4(7) . . . . ? C58 C59 C60 C61 -1.5(8) . . . . ? C59 C60 C61 C62 0.6(8) . . . . ? C60 C61 C62 C66 0.3(7) . . . . ? C60 C61 C62 C63 -179.0(5) . . . . ? C66 C62 C63 C64 1.8(7) . . . . ? C61 C62 C63 C64 -179.0(5) . . . . ? C62 C63 C64 C65 -2.1(7) . . . . ? C66 N4 C65 C64 0.2(8) . . . . ? C63 C64 C65 N4 1.2(9) . . . . ? C65 N4 C66 C62 -0.5(7) . . . . ? C65 N4 C66 C58 -180.0(5) . . . . ? C63 C62 C66 N4 -0.4(7) . . . . ? C61 C62 C66 N4 -179.7(5) . . . . ? C63 C62 C66 C58 179.0(4) . . . . ? C61 C62 C66 C58 -0.3(7) . . . . ? C59 C58 C66 N4 178.9(5) . . . . ? N3 C58 C66 N4 -0.9(7) . . . . ? C59 C58 C66 C62 -0.6(7) . . . . ? N3 C58 C66 C62 179.6(4) . . . . ? C444 C333 C444 N222 0(100) 2_776 . . . ? C777 C555 C666 N333 99(10) . . . . ? C333 C444 N222 C888 103(10) . . . . ? C555 C666 N333 C666 0(100) . . . 2_686 ? C444 N222 C888 N555 11(23) . . . . ? C444 N222 C888 C777 129.3(12) . . . . ? C777 N555 C888 N222 120(23) . . . . ? C666 C555 C777 C888 126.7(15) . . . . ? C666 C555 C777 N555 -8(15) . . . . ? N222 C888 C777 C555 10(2) . . . . ? N555 C888 C777 C555 -174.1(19) . . . . ? N222 C888 C777 N555 -176.1(15) . . . . ? C888 N555 C777 C555 138(15) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.662 _refine_diff_density_min -0.494 _refine_diff_density_rms 0.086