Electronic Supplementary MAterial for CrystEngComm This Journal is © The Royal SOciety of Chemistry 2003 data_global _publ_contact_author_email M.R.J.ELSEGOOD@LBORO.AC.UK _publ_contact_author_name 'Dr Mark Robert James Elsegood' _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_address ; Department of Chemistry Loughborough University Loughborough Leicestershire LE11 3TU UNITED KINGDOM ; _publ_section_title ; Polymorphism and Pseudopolymorphism in Calixarenes: Acetonitrile Clathrates of p-But-calix[n]arenes (n = 6 and 8) ; loop_ _publ_author_name 'Mark Robert James Elsegood' 'Sophie H. Dale' 'Carl Redshaw' data_1 _database_code_CSD 215817 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C69 H88.50 N1.50 O6' _chemical_formula_weight 1034.91 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 9.6509(12) _cell_length_b 16.0236(19) _cell_length_c 21.118(3) _cell_angle_alpha 110.872(2) _cell_angle_beta 95.888(3) _cell_angle_gamma 97.949(2) _cell_volume 2981.2(6) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 1685 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 26.46 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.44 _exptl_crystal_size_mid 0.04 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.153 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1122 _exptl_absorpt_coefficient_mu 0.072 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.969 _exptl_absorpt_correction_T_max 0.999 _exptl_absorpt_process_details 'SADABS v2.03 (Sheldrick, 2001)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 14523 _diffrn_reflns_av_R_equivalents 0.0901 _diffrn_reflns_av_sigmaI/netI 0.2579 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 2.03 _diffrn_reflns_theta_max 25.00 _reflns_number_total 9864 _reflns_number_gt 3080 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0445P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'All non-H atoms found by direct methods' _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0059(5) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 9864 _refine_ls_number_parameters 755 _refine_ls_number_restraints 113 _refine_ls_R_factor_all 0.2246 _refine_ls_R_factor_gt 0.0614 _refine_ls_wR_factor_ref 0.1658 _refine_ls_wR_factor_gt 0.1074 _refine_ls_goodness_of_fit_ref 0.835 _refine_ls_restrained_S_all 0.838 _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 -0.0025(4) 0.5893(2) 0.35546(17) 0.0372(10) Uani 1 1 d . . . H1 H 0.0554 0.5551 0.3565 0.056 Uiso 1 1 calc R . . O2 O 0.0784(4) 0.6041(2) 0.23987(18) 0.0433(10) Uani 1 1 d . . . H2 H 0.0277 0.6025 0.2696 0.065 Uiso 1 1 calc R . . O3 O 0.0874(4) 0.4683(2) 0.12277(17) 0.0408(10) Uani 1 1 d . . . H3 H 0.1047 0.5146 0.1594 0.061 Uiso 1 1 calc R . . O4 O 0.0911(4) 0.3063(2) 0.12371(17) 0.0357(10) Uani 1 1 d . . . H4 H 0.0662 0.3509 0.1167 0.054 Uiso 1 1 calc R . . O5 O 0.2796(4) 0.3944(3) 0.23447(17) 0.0440(10) Uani 1 1 d . . . H5 H 0.2315 0.3661 0.1951 0.066 Uiso 1 1 calc R . . O6 O 0.2378(4) 0.5215(2) 0.34769(17) 0.0433(10) Uani 1 1 d . . . H6 H 0.2620 0.4901 0.3108 0.065 Uiso 1 1 calc R . . C1 C 0.0526(6) 0.6777(4) 0.4044(3) 0.0334(14) Uani 1 1 d . . . C2 C 0.1397(6) 0.6895(4) 0.4642(3) 0.0326(14) Uani 1 1 d . . . C3 C 0.1960(5) 0.7785(3) 0.5092(3) 0.0333(14) Uani 1 1 d . . . H3A H 0.2550 0.7882 0.5510 0.040 Uiso 1 1 calc R . . C4 C 0.1687(5) 0.8540(3) 0.4949(2) 0.0293(13) Uani 1 1 d . . . C5 C 0.0782(5) 0.8376(3) 0.4352(2) 0.0340(14) Uani 1 1 d . . . H5A H 0.0559 0.8881 0.4253 0.041 Uiso 1 1 calc R . . C6 C 0.0176(5) 0.7501(4) 0.3884(2) 0.0316(14) Uani 1 1 d . . . C7 C 0.2399(6) 0.9501(3) 0.5468(3) 0.0337(14) Uani 1 1 d . . . C8 C 0.2291(6) 1.0223(3) 0.5153(3) 0.0469(16) Uani 1 1 d . . . H8A H 0.1291 1.0249 0.5040 0.070 Uiso 1 1 calc R . . H8B H 0.2717 1.0062 0.4734 0.070 Uiso 1 1 calc R . . H8C H 0.2795 1.0818 0.5483 0.070 Uiso 1 1 calc R . . C9 C 0.1659(6) 0.9746(3) 0.6095(3) 0.0486(17) Uani 1 1 d . . . H9A H 0.0663 0.9753 0.5955 0.073 Uiso 1 1 calc R . . H9B H 0.2126 1.0348 0.6428 0.073 Uiso 1 1 calc R . . H9C H 0.1713 0.9294 0.6306 0.073 Uiso 1 1 calc R . . C10 C 0.3974(6) 0.9541(4) 0.5690(3) 0.0540(18) Uani 1 1 d . . . H10A H 0.4423 1.0167 0.5984 0.081 Uiso 1 1 calc R . . H10B H 0.4432 0.9339 0.5282 0.081 Uiso 1 1 calc R . . H10C H 0.4075 0.9142 0.5945 0.081 Uiso 1 1 calc R . . C11 C -0.0732(5) 0.7365(3) 0.3210(2) 0.0332(14) Uani 1 1 d . . . H11A H -0.1288 0.6737 0.3007 0.040 Uiso 1 1 calc R . . H11B H -0.1408 0.7790 0.3299 0.040 Uiso 1 1 calc R . . C12 C 0.0904(6) 0.6891(4) 0.2343(3) 0.0338(14) Uani 1 1 d . . . C13 C 0.0169(5) 0.7528(4) 0.2711(2) 0.0306(13) Uani 1 1 d . . . C14 C 0.0356(6) 0.8373(4) 0.2647(3) 0.0375(15) Uani 1 1 d . . . H14 H -0.0178 0.8808 0.2881 0.045 Uiso 1 1 calc R . . C15 C 0.1303(6) 0.8596(4) 0.2250(3) 0.0371(15) Uani 1 1 d . . . C16 C 0.2035(6) 0.7918(3) 0.1896(3) 0.0355(14) Uani 1 1 d . . . H16 H 0.2679 0.8048 0.1617 0.043 Uiso 1 1 calc R . . C17 C 0.1852(5) 0.7068(3) 0.1938(3) 0.0324(14) Uani 1 1 d . . . C18 C 0.1605(6) 0.9539(4) 0.2207(3) 0.0423(16) Uani 1 1 d . . . C19 C 0.3161(7) 0.9969(4) 0.2506(3) 0.067(2) Uani 1 1 d . . . H19A H 0.3349 1.0023 0.2985 0.101 Uiso 1 1 calc R . . H19B H 0.3362 1.0575 0.2485 0.101 Uiso 1 1 calc R . . H19C H 0.3770 0.9586 0.2239 0.101 Uiso 1 1 calc R . . C20 C 0.0696(7) 1.0181(4) 0.2621(3) 0.068(2) Uani 1 1 d . . . H20A H -0.0309 0.9897 0.2469 0.102 Uiso 1 1 calc R . . H20B H 0.0862 1.0755 0.2548 0.102 Uiso 1 1 calc R . . H20C H 0.0954 1.0301 0.3111 0.102 Uiso 1 1 calc R . . C21 C 0.1317(6) 0.9447(4) 0.1458(3) 0.0532(17) Uani 1 1 d . . . H21A H 0.1926 0.9062 0.1194 0.080 Uiso 1 1 calc R . . H21B H 0.1521 1.0051 0.1433 0.080 Uiso 1 1 calc R . . H21C H 0.0320 0.9171 0.1266 0.080 Uiso 1 1 calc R . . C22 C 0.2809(5) 0.6418(3) 0.1610(2) 0.0353(14) Uani 1 1 d . . . H22A H 0.2978 0.6064 0.1902 0.042 Uiso 1 1 calc R . . H22B H 0.3735 0.6788 0.1630 0.042 Uiso 1 1 calc R . . C23 C 0.1473(5) 0.4891(4) 0.0721(3) 0.0310(13) Uani 1 1 d . . . C24 C 0.2330(6) 0.5736(3) 0.0865(3) 0.0326(14) Uani 1 1 d . . . C25 C 0.2890(5) 0.5893(3) 0.0332(3) 0.0323(14) Uani 1 1 d . . . H25 H 0.3458 0.6471 0.0426 0.039 Uiso 1 1 calc R . . C26 C 0.2668(5) 0.5256(4) -0.0329(2) 0.0310(13) Uani 1 1 d . . . C27 C 0.1811(5) 0.4418(3) -0.0451(3) 0.0320(14) Uani 1 1 d . . . H27 H 0.1622 0.3967 -0.0902 0.038 Uiso 1 1 calc R . . C28 C 0.1230(5) 0.4226(3) 0.0066(3) 0.0297(13) Uani 1 1 d . . . C29 C 0.3364(5) 0.5462(4) -0.0884(3) 0.0333(14) Uani 1 1 d . . . C30 C 0.2798(6) 0.6229(4) -0.1031(3) 0.0530(18) Uani 1 1 d . . . H30A H 0.1777 0.6041 -0.1203 0.079 Uiso 1 1 calc R . . H30B H 0.3284 0.6368 -0.1377 0.079 Uiso 1 1 calc R . . H30C H 0.2969 0.6772 -0.0607 0.079 Uiso 1 1 calc R . . C31 C 0.4966(5) 0.5766(4) -0.0642(3) 0.0469(16) Uani 1 1 d . . . H31A H 0.5420 0.5864 -0.1011 0.070 Uiso 1 1 calc R . . H31B H 0.5347 0.5295 -0.0524 0.070 Uiso 1 1 calc R . . H31C H 0.5158 0.6334 -0.0237 0.070 Uiso 1 1 calc R . . C32 C 0.3118(7) 0.4632(4) -0.1558(3) 0.070(2) Uani 1 1 d . . . H32A H 0.2098 0.4419 -0.1723 0.105 Uiso 1 1 calc R . . H32B H 0.3534 0.4146 -0.1479 0.105 Uiso 1 1 calc R . . H32C H 0.3566 0.4800 -0.1902 0.105 Uiso 1 1 calc R . . C33 C 0.0426(5) 0.3267(3) -0.0077(2) 0.0338(14) Uani 1 1 d . . . H33A H -0.0336 0.3309 0.0207 0.041 Uiso 1 1 calc R . . H33B H -0.0025 0.2983 -0.0566 0.041 Uiso 1 1 calc R . . C34 C 0.1625(6) 0.2611(3) 0.0718(3) 0.0303(13) Uani 1 1 d . . . C35 C 0.1387(5) 0.2671(3) 0.0078(3) 0.0297(13) Uani 1 1 d . . . C36 C 0.2119(5) 0.2191(3) -0.0421(3) 0.0356(14) Uani 1 1 d . . . H36 H 0.1973 0.2230 -0.0860 0.043 Uiso 1 1 calc R . . C37 C 0.3064(6) 0.1651(3) -0.0304(3) 0.0358(14) Uani 1 1 d . A . C38 C 0.3252(5) 0.1617(3) 0.0345(3) 0.0351(14) Uani 1 1 d . . . H38 H 0.3888 0.1258 0.0438 0.042 Uiso 1 1 calc R . . C39 C 0.2555(5) 0.2084(3) 0.0864(3) 0.0300(13) Uani 1 1 d . . . C40 C 0.3831(6) 0.1126(4) -0.0864(3) 0.0481(16) Uani 1 1 d DU . . C41 C 0.4870(14) 0.1739(7) -0.1044(7) 0.067(5) Uani 0.529(8) 1 d PDU A 1 H41A H 0.5348 0.1376 -0.1405 0.101 Uiso 0.529(8) 1 calc PR A 1 H41B H 0.5574 0.2111 -0.0637 0.101 Uiso 0.529(8) 1 calc PR A 1 H41C H 0.4378 0.2135 -0.1211 0.101 Uiso 0.529(8) 1 calc PR A 1 C42 C 0.2711(11) 0.0528(7) -0.1514(5) 0.052(4) Uani 0.529(8) 1 d PDU A 1 H42A H 0.2048 0.0104 -0.1398 0.078 Uiso 0.529(8) 1 calc PR A 1 H42B H 0.3194 0.0185 -0.1880 0.078 Uiso 0.529(8) 1 calc PR A 1 H42C H 0.2188 0.0920 -0.1670 0.078 Uiso 0.529(8) 1 calc PR A 1 C43 C 0.4564(13) 0.0394(7) -0.0687(6) 0.058(4) Uani 0.529(8) 1 d PDU A 1 H43A H 0.3871 0.0010 -0.0551 0.087 Uiso 0.529(8) 1 calc PR A 1 H43B H 0.5358 0.0704 -0.0307 0.087 Uiso 0.529(8) 1 calc PR A 1 H43C H 0.4916 0.0016 -0.1091 0.087 Uiso 0.529(8) 1 calc PR A 1 C41X C 0.3818(15) 0.1530(9) -0.1453(6) 0.052(4) Uani 0.471(8) 1 d PDU A 2 H41D H 0.4192 0.2186 -0.1248 0.078 Uiso 0.471(8) 1 calc PR A 2 H41E H 0.2843 0.1421 -0.1689 0.078 Uiso 0.471(8) 1 calc PR A 2 H41F H 0.4409 0.1232 -0.1783 0.078 Uiso 0.471(8) 1 calc PR A 2 C42X C 0.3289(15) 0.0162(7) -0.1135(8) 0.070(5) Uani 0.471(8) 1 d PDU A 2 H42D H 0.3817 -0.0144 -0.1495 0.104 Uiso 0.471(8) 1 calc PR A 2 H42E H 0.2282 0.0045 -0.1330 0.104 Uiso 0.471(8) 1 calc PR A 2 H42F H 0.3399 -0.0070 -0.0765 0.104 Uiso 0.471(8) 1 calc PR A 2 C43X C 0.5478(10) 0.1359(9) -0.0560(6) 0.055(4) Uani 0.471(8) 1 d PDU A 2 H43D H 0.5809 0.2019 -0.0382 0.083 Uiso 0.471(8) 1 calc PR A 2 H43E H 0.6007 0.1064 -0.0923 0.083 Uiso 0.471(8) 1 calc PR A 2 H43F H 0.5632 0.1137 -0.0186 0.083 Uiso 0.471(8) 1 calc PR A 2 C44 C 0.2841(5) 0.2045(3) 0.1573(2) 0.0343(14) Uani 1 1 d . . . H44A H 0.2987 0.1425 0.1520 0.041 Uiso 1 1 calc R . . H44B H 0.1992 0.2151 0.1794 0.041 Uiso 1 1 calc R . . C45 C 0.4060(6) 0.3641(4) 0.2379(2) 0.0315(14) Uani 1 1 d . . . C46 C 0.4121(6) 0.2729(4) 0.2045(3) 0.0328(14) Uani 1 1 d . . . C47 C 0.5406(6) 0.2462(3) 0.2117(2) 0.0320(14) Uani 1 1 d . . . H47 H 0.5456 0.1841 0.1886 0.038 Uiso 1 1 calc R . . C48 C 0.6648(6) 0.3071(4) 0.2517(2) 0.0316(14) Uani 1 1 d . . . C49 C 0.6525(6) 0.3977(3) 0.2829(2) 0.0323(14) Uani 1 1 d . . . H49 H 0.7347 0.4409 0.3093 0.039 Uiso 1 1 calc R . . C50 C 0.5254(6) 0.4277(3) 0.2772(3) 0.0332(14) Uani 1 1 d . . . C51 C 0.8041(6) 0.2730(4) 0.2576(3) 0.0340(14) Uani 1 1 d . . . C52 C 0.8292(6) 0.2123(4) 0.1868(3) 0.0459(16) Uani 1 1 d . . . H52A H 0.9202 0.1927 0.1914 0.069 Uiso 1 1 calc R . . H52B H 0.8309 0.2466 0.1566 0.069 Uiso 1 1 calc R . . H52C H 0.7526 0.1589 0.1672 0.069 Uiso 1 1 calc R . . C53 C 0.9317(5) 0.3520(3) 0.2881(3) 0.0480(17) Uani 1 1 d . . . H53A H 0.9248 0.3881 0.3357 0.072 Uiso 1 1 calc R . . H53B H 0.9321 0.3906 0.2610 0.072 Uiso 1 1 calc R . . H53C H 1.0197 0.3278 0.2870 0.072 Uiso 1 1 calc R . . C54 C 0.7966(6) 0.2183(4) 0.3033(3) 0.0507(17) Uani 1 1 d . . . H54A H 0.7859 0.2577 0.3495 0.076 Uiso 1 1 calc R . . H54B H 0.8839 0.1940 0.3058 0.076 Uiso 1 1 calc R . . H54C H 0.7151 0.1679 0.2841 0.076 Uiso 1 1 calc R . . C55 C 0.5202(6) 0.5284(3) 0.3082(2) 0.0347(14) Uani 1 1 d . . . H55A H 0.6115 0.5632 0.3060 0.042 Uiso 1 1 calc R . . H55B H 0.4449 0.5407 0.2792 0.042 Uiso 1 1 calc R . . C56 C 0.3588(6) 0.5618(3) 0.3989(3) 0.0320(14) Uani 1 1 d . . . C57 C 0.4936(6) 0.5645(3) 0.3816(3) 0.0300(13) Uani 1 1 d . . . C58 C 0.6063(6) 0.6074(3) 0.4349(3) 0.0343(14) Uani 1 1 d . . . H58 H 0.6998 0.6095 0.4244 0.041 Uiso 1 1 calc R . . C59 C 0.5897(6) 0.6476(3) 0.5029(2) 0.0313(14) Uani 1 1 d . . . C60 C 0.4525(6) 0.6444(3) 0.5162(3) 0.0319(14) Uani 1 1 d . . . H60 H 0.4383 0.6719 0.5624 0.038 Uiso 1 1 calc R . . C61 C 0.3331(6) 0.6027(3) 0.4650(3) 0.0287(13) Uani 1 1 d . . . C62 C 0.7202(6) 0.6977(3) 0.5588(3) 0.0342(14) Uani 1 1 d . . . C63 C 0.8328(6) 0.6383(4) 0.5519(3) 0.0504(17) Uani 1 1 d . . . H63A H 0.9182 0.6725 0.5855 0.076 Uiso 1 1 calc R . . H63B H 0.8563 0.6206 0.5054 0.076 Uiso 1 1 calc R . . H63C H 0.7962 0.5837 0.5603 0.076 Uiso 1 1 calc R . . C64 C 0.6839(6) 0.7241(4) 0.6308(3) 0.0502(17) Uani 1 1 d . . . H64A H 0.6166 0.7658 0.6367 0.075 Uiso 1 1 calc R . . H64B H 0.7705 0.7541 0.6645 0.075 Uiso 1 1 calc R . . H64C H 0.6411 0.6694 0.6375 0.075 Uiso 1 1 calc R . . C65 C 0.7832(6) 0.7849(4) 0.5481(3) 0.0570(18) Uani 1 1 d . . . H65A H 0.7111 0.8229 0.5504 0.086 Uiso 1 1 calc R . . H65B H 0.8134 0.7683 0.5030 0.086 Uiso 1 1 calc R . . H65C H 0.8651 0.8188 0.5841 0.086 Uiso 1 1 calc R . . C66 C 0.1872(5) 0.6113(3) 0.4812(3) 0.0312(14) Uani 1 1 d . . . H66A H 0.1869 0.6231 0.5305 0.037 Uiso 1 1 calc R . . H66B H 0.1202 0.5537 0.4539 0.037 Uiso 1 1 calc R . . N1 N 0.5859(6) 0.7883(4) 0.2922(3) 0.087(2) Uani 1 1 d D . . C67 C 0.5031(7) 0.7782(4) 0.3239(3) 0.0565(19) Uani 1 1 d D . . C68 C 0.3968(7) 0.7666(4) 0.3649(3) 0.070(2) Uani 1 1 d D . . H68A H 0.4431 0.7695 0.4094 0.105 Uiso 1 1 calc R . . H68B H 0.3340 0.7073 0.3410 0.105 Uiso 1 1 calc R . . H68C H 0.3412 0.8150 0.3722 0.105 Uiso 1 1 calc R . . N2 N -0.028(10) 1.017(7) 0.013(5) 0.46(3) Uani 0.50 1 d PDU B -1 C69 C 0.044(2) 0.9672(13) -0.0112(7) 0.078(8) Uani 0.50 1 d PDU B -1 C70 C 0.151(2) 0.9138(13) -0.0205(8) 0.136(10) Uani 0.50 1 d PDU B -1 H70A H 0.1642 0.8922 -0.0687 0.204 Uiso 0.50 1 calc PR B -1 H70B H 0.1237 0.8616 -0.0076 0.204 Uiso 0.50 1 calc PR B -1 H70C H 0.2407 0.9508 0.0086 0.204 Uiso 0.50 1 calc 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 O1 0.047(3) 0.026(2) 0.032(2) 0.0030(19) 0.0068(19) 0.0078(19) O2 0.064(3) 0.031(2) 0.037(2) 0.0097(19) 0.023(2) 0.013(2) O3 0.060(3) 0.032(2) 0.028(2) 0.0043(18) 0.021(2) 0.009(2) O4 0.042(2) 0.030(2) 0.035(2) 0.0085(19) 0.0136(19) 0.012(2) O5 0.042(3) 0.046(3) 0.031(2) -0.001(2) -0.0008(19) 0.014(2) O6 0.047(3) 0.040(3) 0.033(2) 0.001(2) 0.007(2) 0.012(2) C1 0.040(4) 0.028(3) 0.025(3) -0.002(3) 0.011(3) 0.007(3) C2 0.041(4) 0.031(4) 0.026(3) 0.007(3) 0.014(3) 0.009(3) C3 0.037(4) 0.037(4) 0.025(3) 0.008(3) 0.010(3) 0.013(3) C4 0.034(3) 0.029(3) 0.018(3) -0.002(3) 0.009(3) 0.007(3) C5 0.040(4) 0.030(4) 0.029(3) 0.003(3) 0.013(3) 0.015(3) C6 0.038(4) 0.031(3) 0.021(3) 0.002(3) 0.009(3) 0.009(3) C7 0.037(4) 0.026(3) 0.029(3) 0.000(3) 0.006(3) 0.005(3) C8 0.055(4) 0.031(4) 0.050(4) 0.012(3) 0.005(3) 0.002(3) C9 0.070(5) 0.028(4) 0.036(4) -0.001(3) 0.013(3) 0.003(3) C10 0.042(4) 0.044(4) 0.066(5) 0.012(3) -0.001(3) 0.004(3) C11 0.043(4) 0.025(3) 0.028(3) 0.003(3) 0.013(3) 0.009(3) C12 0.042(4) 0.028(4) 0.027(3) 0.006(3) 0.005(3) 0.007(3) C13 0.032(3) 0.034(4) 0.022(3) 0.004(3) 0.004(3) 0.010(3) C14 0.043(4) 0.032(4) 0.033(3) 0.004(3) 0.008(3) 0.015(3) C15 0.041(4) 0.037(4) 0.033(3) 0.007(3) 0.012(3) 0.013(3) C16 0.045(4) 0.037(4) 0.027(3) 0.012(3) 0.015(3) 0.008(3) C17 0.036(4) 0.033(4) 0.027(3) 0.006(3) 0.013(3) 0.009(3) C18 0.060(4) 0.026(4) 0.041(4) 0.011(3) 0.013(3) 0.012(3) C19 0.085(6) 0.034(4) 0.071(5) 0.009(4) 0.010(4) 0.003(4) C20 0.102(6) 0.038(4) 0.071(5) 0.015(4) 0.041(4) 0.031(4) C21 0.074(5) 0.039(4) 0.044(4) 0.015(3) 0.015(4) 0.002(3) C22 0.041(4) 0.035(4) 0.029(3) 0.007(3) 0.012(3) 0.011(3) C23 0.038(4) 0.032(4) 0.027(3) 0.011(3) 0.016(3) 0.012(3) C24 0.042(4) 0.025(3) 0.026(3) 0.003(3) 0.006(3) 0.009(3) C25 0.038(4) 0.028(3) 0.031(3) 0.010(3) 0.010(3) 0.007(3) C26 0.037(4) 0.031(3) 0.023(3) 0.007(3) 0.008(3) 0.009(3) C27 0.038(4) 0.032(4) 0.024(3) 0.006(3) 0.007(3) 0.008(3) C28 0.036(4) 0.026(3) 0.027(3) 0.008(3) 0.008(3) 0.010(3) C29 0.033(4) 0.038(4) 0.029(3) 0.011(3) 0.011(3) 0.007(3) C30 0.053(4) 0.067(5) 0.059(4) 0.045(4) 0.019(3) 0.015(4) C31 0.042(4) 0.060(4) 0.043(4) 0.023(3) 0.011(3) 0.010(3) C32 0.101(6) 0.060(5) 0.035(4) 0.003(3) 0.040(4) -0.010(4) C33 0.037(4) 0.032(3) 0.025(3) 0.003(3) 0.006(3) 0.003(3) C34 0.038(4) 0.020(3) 0.024(3) -0.002(3) 0.010(3) 0.003(3) C35 0.032(3) 0.022(3) 0.025(3) -0.002(3) 0.004(3) 0.000(3) C36 0.039(4) 0.029(3) 0.030(3) 0.004(3) 0.003(3) 0.000(3) C37 0.034(4) 0.030(3) 0.033(4) 0.000(3) 0.009(3) 0.002(3) C38 0.037(4) 0.028(3) 0.032(3) 0.002(3) 0.007(3) 0.006(3) C39 0.032(3) 0.024(3) 0.028(3) 0.005(3) 0.008(3) -0.005(3) C40 0.049(4) 0.056(4) 0.037(4) 0.008(3) 0.018(3) 0.018(3) C41 0.080(11) 0.048(8) 0.065(11) 0.001(7) 0.051(9) 0.010(7) C42 0.081(9) 0.030(7) 0.038(7) -0.002(5) 0.021(5) 0.022(6) C43 0.060(9) 0.046(8) 0.058(8) 0.001(6) 0.018(6) 0.020(7) C41X 0.062(11) 0.056(9) 0.040(9) 0.012(7) 0.028(7) 0.018(9) C42X 0.078(11) 0.042(7) 0.086(13) 0.015(8) 0.030(10) 0.013(7) C43X 0.048(7) 0.064(10) 0.050(9) 0.011(7) 0.016(6) 0.021(7) C44 0.037(4) 0.034(4) 0.030(3) 0.009(3) 0.011(3) 0.006(3) C45 0.032(4) 0.038(4) 0.021(3) 0.004(3) 0.007(3) 0.010(3) C46 0.037(4) 0.033(4) 0.025(3) 0.008(3) 0.006(3) 0.005(3) C47 0.043(4) 0.026(3) 0.024(3) 0.006(3) 0.006(3) 0.006(3) C48 0.042(4) 0.035(4) 0.022(3) 0.013(3) 0.012(3) 0.012(3) C49 0.036(4) 0.032(4) 0.027(3) 0.008(3) 0.008(3) 0.008(3) C50 0.044(4) 0.028(3) 0.027(3) 0.007(3) 0.010(3) 0.012(3) C51 0.032(4) 0.035(4) 0.032(3) 0.009(3) 0.005(3) 0.007(3) C52 0.048(4) 0.049(4) 0.043(4) 0.015(3) 0.019(3) 0.017(3) C53 0.036(4) 0.043(4) 0.055(4) 0.010(3) -0.002(3) 0.007(3) C54 0.053(4) 0.050(4) 0.053(4) 0.025(3) 0.003(3) 0.010(3) C55 0.040(4) 0.033(3) 0.029(3) 0.008(3) 0.010(3) 0.007(3) C56 0.035(4) 0.026(3) 0.028(3) 0.001(3) 0.004(3) 0.009(3) C57 0.036(4) 0.029(3) 0.027(3) 0.009(3) 0.012(3) 0.011(3) C58 0.039(4) 0.029(3) 0.035(4) 0.009(3) 0.009(3) 0.012(3) C59 0.047(4) 0.024(3) 0.018(3) 0.001(3) 0.006(3) 0.007(3) C60 0.048(4) 0.024(3) 0.025(3) 0.005(3) 0.012(3) 0.013(3) C61 0.036(4) 0.028(3) 0.025(3) 0.009(3) 0.016(3) 0.014(3) C62 0.041(4) 0.029(3) 0.029(3) 0.006(3) 0.010(3) 0.006(3) C63 0.050(4) 0.051(4) 0.042(4) 0.008(3) -0.001(3) 0.012(3) C64 0.060(4) 0.053(4) 0.032(4) 0.008(3) 0.010(3) 0.011(3) C65 0.071(5) 0.040(4) 0.052(4) 0.015(3) 0.002(4) -0.003(4) C66 0.038(4) 0.026(3) 0.029(3) 0.008(3) 0.013(3) 0.007(3) N1 0.058(5) 0.104(5) 0.077(5) 0.012(4) 0.012(4) -0.003(4) C67 0.050(5) 0.051(5) 0.046(5) -0.003(4) -0.002(4) 0.001(4) C68 0.064(5) 0.069(5) 0.073(5) 0.019(4) 0.020(4) 0.010(4) N2 0.46(5) 0.47(5) 0.42(5) 0.22(4) 0.01(4) -0.06(3) C69 0.099(18) 0.083(16) 0.006(9) -0.002(10) 0.003(9) -0.078(12) C70 0.123(18) 0.16(2) 0.045(11) -0.013(12) 0.037(12) -0.104(16) _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 1.411(5) . ? O2 C12 1.398(6) . ? O3 C23 1.383(5) . ? O4 C34 1.388(5) . ? O5 C45 1.379(5) . ? O6 C56 1.409(6) . ? C1 C2 1.380(7) . ? C1 C6 1.393(7) . ? C2 C3 1.395(6) . ? C2 C66 1.534(6) . ? C3 C4 1.400(6) . ? C4 C5 1.377(6) . ? C4 C7 1.547(6) . ? C5 C6 1.397(6) . ? C6 C11 1.521(6) . ? C7 C9 1.522(6) . ? C7 C10 1.529(7) . ? C7 C8 1.537(7) . ? C11 C13 1.503(6) . ? C12 C13 1.377(6) . ? C12 C17 1.383(7) . ? C13 C14 1.396(6) . ? C14 C15 1.396(7) . ? C15 C16 1.408(6) . ? C15 C18 1.535(7) . ? C16 C17 1.384(6) . ? C17 C22 1.518(6) . ? C18 C21 1.529(7) . ? C18 C19 1.529(7) . ? C18 C20 1.536(7) . ? C22 C24 1.539(6) . ? C23 C28 1.386(6) . ? C23 C24 1.398(6) . ? C24 C25 1.384(6) . ? C25 C26 1.377(6) . ? C26 C27 1.398(6) . ? C26 C29 1.521(7) . ? C27 C28 1.384(6) . ? C28 C33 1.531(6) . ? C29 C30 1.526(7) . ? C29 C31 1.530(6) . ? C29 C32 1.531(7) . ? C33 C35 1.512(6) . ? C34 C35 1.388(6) . ? C34 C39 1.397(7) . ? C35 C36 1.387(6) . ? C36 C37 1.402(7) . ? C37 C38 1.384(7) . ? C37 C40 1.517(7) . ? C38 C39 1.386(6) . ? C39 C44 1.520(6) . ? C40 C42X 1.439(11) . ? C40 C41 1.478(10) . ? C40 C42 1.562(10) . ? C40 C43 1.583(10) . ? C40 C41X 1.592(10) . ? C40 C43X 1.592(10) . ? C44 C46 1.522(6) . ? C45 C46 1.390(6) . ? C45 C50 1.390(6) . ? C46 C47 1.378(6) . ? C47 C48 1.408(6) . ? C48 C49 1.393(6) . ? C48 C51 1.530(7) . ? C49 C50 1.387(6) . ? C50 C55 1.520(6) . ? C51 C54 1.518(7) . ? C51 C52 1.529(6) . ? C51 C53 1.537(6) . ? C55 C57 1.512(6) . ? C56 C61 1.380(6) . ? C56 C57 1.385(6) . ? C57 C58 1.384(7) . ? C58 C59 1.386(6) . ? C59 C60 1.379(6) . ? C59 C62 1.537(7) . ? C60 C61 1.400(6) . ? C61 C66 1.496(6) . ? C62 C64 1.518(6) . ? C62 C63 1.525(6) . ? C62 C65 1.546(7) . ? N1 C67 1.125(7) . ? C67 C68 1.443(8) . ? N2 C69 1.15(2) . ? C69 C70 1.419(16) . ? 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 C2 C1 C6 122.9(5) . . ? C2 C1 O1 120.1(5) . . ? C6 C1 O1 117.0(5) . . ? C1 C2 C3 117.5(5) . . ? C1 C2 C66 124.0(5) . . ? C3 C2 C66 118.4(5) . . ? C2 C3 C4 122.3(5) . . ? C5 C4 C3 117.3(5) . . ? C5 C4 C7 124.2(5) . . ? C3 C4 C7 118.5(5) . . ? C4 C5 C6 123.0(5) . . ? C1 C6 C5 117.0(5) . . ? C1 C6 C11 122.5(5) . . ? C5 C6 C11 120.3(5) . . ? C9 C7 C10 109.7(5) . . ? C9 C7 C8 107.9(4) . . ? C10 C7 C8 107.5(4) . . ? C9 C7 C4 109.6(4) . . ? C10 C7 C4 110.8(4) . . ? C8 C7 C4 111.2(4) . . ? C13 C11 C6 111.1(4) . . ? C13 C12 C17 122.6(5) . . ? C13 C12 O2 120.7(5) . . ? C17 C12 O2 116.5(5) . . ? C12 C13 C14 118.1(5) . . ? C12 C13 C11 122.2(5) . . ? C14 C13 C11 119.6(5) . . ? C15 C14 C13 122.0(5) . . ? C14 C15 C16 116.9(5) . . ? C14 C15 C18 123.2(5) . . ? C16 C15 C18 119.8(5) . . ? C17 C16 C15 122.4(5) . . ? C12 C17 C16 117.9(5) . . ? C12 C17 C22 122.8(5) . . ? C16 C17 C22 119.0(5) . . ? C21 C18 C19 109.4(5) . . ? C21 C18 C15 109.8(4) . . ? C19 C18 C15 108.9(5) . . ? C21 C18 C20 108.9(5) . . ? C19 C18 C20 107.6(5) . . ? C15 C18 C20 112.2(5) . . ? C17 C22 C24 119.1(4) . . ? O3 C23 C28 118.0(5) . . ? O3 C23 C24 121.5(5) . . ? C28 C23 C24 120.5(5) . . ? C25 C24 C23 118.1(5) . . ? C25 C24 C22 120.5(5) . . ? C23 C24 C22 120.8(5) . . ? C26 C25 C24 123.4(5) . . ? C25 C26 C27 116.7(5) . . ? C25 C26 C29 120.6(5) . . ? C27 C26 C29 122.6(4) . . ? C28 C27 C26 122.1(5) . . ? C27 C28 C23 119.1(5) . . ? C27 C28 C33 120.1(5) . . ? C23 C28 C33 120.6(5) . . ? C26 C29 C30 110.7(4) . . ? C26 C29 C31 109.6(4) . . ? C30 C29 C31 108.0(4) . . ? C26 C29 C32 112.4(4) . . ? C30 C29 C32 108.3(5) . . ? C31 C29 C32 107.7(5) . . ? C35 C33 C28 112.2(4) . . ? C35 C34 O4 120.6(5) . . ? C35 C34 C39 122.0(5) . . ? O4 C34 C39 117.4(5) . . ? C36 C35 C34 117.7(5) . . ? C36 C35 C33 119.8(5) . . ? C34 C35 C33 122.4(5) . . ? C35 C36 C37 122.8(5) . . ? C38 C37 C36 116.8(5) . . ? C38 C37 C40 121.9(5) . . ? C36 C37 C40 121.4(5) . . ? C37 C38 C39 123.0(5) . . ? C38 C39 C34 117.8(5) . . ? C38 C39 C44 120.6(5) . . ? C34 C39 C44 121.6(5) . . ? C42X C40 C41 135.2(8) . . ? C42X C40 C37 112.7(7) . . ? C41 C40 C37 111.8(6) . . ? C42X C40 C42 50.1(7) . . ? C41 C40 C42 109.6(7) . . ? C37 C40 C42 108.7(6) . . ? C42X C40 C43 54.5(7) . . ? C41 C40 C43 110.5(8) . . ? C37 C40 C43 113.1(6) . . ? C42 C40 C43 102.6(7) . . ? C42X C40 C41X 112.0(8) . . ? C37 C40 C41X 110.4(6) . . ? C42X C40 C43X 111.8(8) . . ? C37 C40 C43X 107.9(6) . . ? C41X C40 C43X 101.4(8) . . ? C39 C44 C46 114.4(4) . . ? O5 C45 C46 120.9(5) . . ? O5 C45 C50 117.4(5) . . ? C46 C45 C50 121.7(5) . . ? C47 C46 C45 118.2(5) . . ? C47 C46 C44 119.9(5) . . ? C45 C46 C44 121.8(5) . . ? C46 C47 C48 122.8(5) . . ? C49 C48 C47 116.3(5) . . ? C49 C48 C51 123.5(5) . . ? C47 C48 C51 120.2(5) . . ? C50 C49 C48 122.9(5) . . ? C49 C50 C45 118.0(5) . . ? C49 C50 C55 120.6(5) . . ? C45 C50 C55 121.1(5) . . ? C54 C51 C52 109.0(4) . . ? C54 C51 C48 108.9(4) . . ? C52 C51 C48 110.6(4) . . ? C54 C51 C53 109.2(4) . . ? C52 C51 C53 107.4(4) . . ? C48 C51 C53 111.6(4) . . ? C57 C55 C50 116.5(4) . . ? C61 C56 C57 123.4(5) . . ? C61 C56 O6 115.8(5) . . ? C57 C56 O6 120.7(5) . . ? C58 C57 C56 116.8(5) . . ? C58 C57 C55 120.0(5) . . ? C56 C57 C55 123.1(5) . . ? C57 C58 C59 123.3(5) . . ? C60 C59 C58 116.8(5) . . ? C60 C59 C62 123.1(5) . . ? C58 C59 C62 120.0(5) . . ? C59 C60 C61 123.3(5) . . ? C56 C61 C60 116.4(5) . . ? C56 C61 C66 122.6(5) . . ? C60 C61 C66 120.8(5) . . ? C64 C62 C63 108.9(4) . . ? C64 C62 C59 112.4(4) . . ? C63 C62 C59 110.1(4) . . ? C64 C62 C65 108.9(4) . . ? C63 C62 C65 108.2(5) . . ? C59 C62 C65 108.3(4) . . ? C61 C66 C2 109.8(4) . . ? N1 C67 C68 179.2(8) . . ? N2 C69 C70 163(5) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 -1.3(8) . . . . ? O1 C1 C2 C3 177.2(4) . . . . ? C6 C1 C2 C66 -176.2(5) . . . . ? O1 C1 C2 C66 2.2(8) . . . . ? C1 C2 C3 C4 -1.0(8) . . . . ? C66 C2 C3 C4 174.2(4) . . . . ? C2 C3 C4 C5 2.6(7) . . . . ? C2 C3 C4 C7 -178.1(5) . . . . ? C3 C4 C5 C6 -2.0(8) . . . . ? C7 C4 C5 C6 178.7(5) . . . . ? C2 C1 C6 C5 1.8(8) . . . . ? O1 C1 C6 C5 -176.7(4) . . . . ? C2 C1 C6 C11 177.2(5) . . . . ? O1 C1 C6 C11 -1.2(7) . . . . ? C4 C5 C6 C1 -0.1(8) . . . . ? C4 C5 C6 C11 -175.6(5) . . . . ? C5 C4 C7 C9 104.4(6) . . . . ? C3 C4 C7 C9 -75.0(6) . . . . ? C5 C4 C7 C10 -134.4(5) . . . . ? C3 C4 C7 C10 46.2(6) . . . . ? C5 C4 C7 C8 -14.9(7) . . . . ? C3 C4 C7 C8 165.8(4) . . . . ? C1 C6 C11 C13 -100.3(6) . . . . ? C5 C6 C11 C13 75.0(6) . . . . ? C17 C12 C13 C14 2.6(8) . . . . ? O2 C12 C13 C14 178.5(5) . . . . ? C17 C12 C13 C11 -173.0(5) . . . . ? O2 C12 C13 C11 3.0(8) . . . . ? C6 C11 C13 C12 78.1(6) . . . . ? C6 C11 C13 C14 -97.4(6) . . . . ? C12 C13 C14 C15 -2.9(8) . . . . ? C11 C13 C14 C15 172.8(5) . . . . ? C13 C14 C15 C16 2.0(8) . . . . ? C13 C14 C15 C18 -175.8(5) . . . . ? C14 C15 C16 C17 -0.7(8) . . . . ? C18 C15 C16 C17 177.2(5) . . . . ? C13 C12 C17 C16 -1.4(8) . . . . ? O2 C12 C17 C16 -177.5(5) . . . . ? C13 C12 C17 C22 171.5(5) . . . . ? O2 C12 C17 C22 -4.7(7) . . . . ? C15 C16 C17 C12 0.4(8) . . . . ? C15 C16 C17 C22 -172.7(5) . . . . ? C14 C15 C18 C21 -124.0(6) . . . . ? C16 C15 C18 C21 58.2(7) . . . . ? C14 C15 C18 C19 116.2(6) . . . . ? C16 C15 C18 C19 -61.5(6) . . . . ? C14 C15 C18 C20 -2.8(8) . . . . ? C16 C15 C18 C20 179.5(5) . . . . ? C12 C17 C22 C24 95.2(6) . . . . ? C16 C17 C22 C24 -92.1(6) . . . . ? O3 C23 C24 C25 -180.0(5) . . . . ? C28 C23 C24 C25 1.8(8) . . . . ? O3 C23 C24 C22 8.5(7) . . . . ? C28 C23 C24 C22 -169.7(5) . . . . ? C17 C22 C24 C25 102.1(6) . . . . ? C17 C22 C24 C23 -86.6(6) . . . . ? C23 C24 C25 C26 -1.2(8) . . . . ? C22 C24 C25 C26 170.3(5) . . . . ? C24 C25 C26 C27 0.9(8) . . . . ? C24 C25 C26 C29 -177.6(5) . . . . ? C25 C26 C27 C28 -1.1(7) . . . . ? C29 C26 C27 C28 177.3(5) . . . . ? C26 C27 C28 C23 1.7(8) . . . . ? C26 C27 C28 C33 -173.8(5) . . . . ? O3 C23 C28 C27 179.7(5) . . . . ? C24 C23 C28 C27 -2.0(8) . . . . ? O3 C23 C28 C33 -4.9(7) . . . . ? C24 C23 C28 C33 173.4(5) . . . . ? C25 C26 C29 C30 -65.1(6) . . . . ? C27 C26 C29 C30 116.5(5) . . . . ? C25 C26 C29 C31 53.9(6) . . . . ? C27 C26 C29 C31 -124.5(5) . . . . ? C25 C26 C29 C32 173.6(5) . . . . ? C27 C26 C29 C32 -4.8(7) . . . . ? C27 C28 C33 C35 90.8(6) . . . . ? C23 C28 C33 C35 -84.6(6) . . . . ? O4 C34 C35 C36 -179.0(4) . . . . ? C39 C34 C35 C36 -0.5(7) . . . . ? O4 C34 C35 C33 3.8(7) . . . . ? C39 C34 C35 C33 -177.7(5) . . . . ? C28 C33 C35 C36 -86.6(6) . . . . ? C28 C33 C35 C34 90.5(6) . . . . ? C34 C35 C36 C37 0.5(7) . . . . ? C33 C35 C36 C37 177.8(5) . . . . ? C35 C36 C37 C38 -0.4(8) . . . . ? C35 C36 C37 C40 179.2(5) . . . . ? C36 C37 C38 C39 0.2(8) . . . . ? C40 C37 C38 C39 -179.4(5) . . . . ? C37 C38 C39 C34 -0.1(7) . . . . ? C37 C38 C39 C44 -178.0(5) . . . . ? C35 C34 C39 C38 0.3(7) . . . . ? O4 C34 C39 C38 178.9(4) . . . . ? C35 C34 C39 C44 178.1(5) . . . . ? O4 C34 C39 C44 -3.3(7) . . . . ? C38 C37 C40 C42X 72.3(9) . . . . ? C36 C37 C40 C42X -107.2(9) . . . . ? C38 C37 C40 C41 -112.8(9) . . . . ? C36 C37 C40 C41 67.6(9) . . . . ? C38 C37 C40 C42 126.0(7) . . . . ? C36 C37 C40 C42 -53.6(8) . . . . ? C38 C37 C40 C43 12.7(9) . . . . ? C36 C37 C40 C43 -166.9(7) . . . . ? C38 C37 C40 C41X -161.6(7) . . . . ? C36 C37 C40 C41X 18.8(9) . . . . ? C38 C37 C40 C43X -51.6(8) . . . . ? C36 C37 C40 C43X 128.8(7) . . . . ? C38 C39 C44 C46 84.8(6) . . . . ? C34 C39 C44 C46 -93.0(6) . . . . ? O5 C45 C46 C47 -177.9(4) . . . . ? C50 C45 C46 C47 0.4(8) . . . . ? O5 C45 C46 C44 6.2(7) . . . . ? C50 C45 C46 C44 -175.5(5) . . . . ? C39 C44 C46 C47 -98.0(6) . . . . ? C39 C44 C46 C45 77.9(6) . . . . ? C45 C46 C47 C48 0.6(7) . . . . ? C44 C46 C47 C48 176.6(4) . . . . ? C46 C47 C48 C49 -1.6(7) . . . . ? C46 C47 C48 C51 179.9(5) . . . . ? C47 C48 C49 C50 1.6(7) . . . . ? C51 C48 C49 C50 -180.0(5) . . . . ? C48 C49 C50 C45 -0.6(8) . . . . ? C48 C49 C50 C55 -175.7(5) . . . . ? O5 C45 C50 C49 177.9(4) . . . . ? C46 C45 C50 C49 -0.4(7) . . . . ? O5 C45 C50 C55 -7.0(7) . . . . ? C46 C45 C50 C55 174.6(5) . . . . ? C49 C48 C51 C54 108.3(6) . . . . ? C47 C48 C51 C54 -73.3(6) . . . . ? C49 C48 C51 C52 -131.8(5) . . . . ? C47 C48 C51 C52 46.6(6) . . . . ? C49 C48 C51 C53 -12.3(7) . . . . ? C47 C48 C51 C53 166.1(4) . . . . ? C49 C50 C55 C57 -89.9(6) . . . . ? C45 C50 C55 C57 95.2(6) . . . . ? C61 C56 C57 C58 3.0(8) . . . . ? O6 C56 C57 C58 178.4(4) . . . . ? C61 C56 C57 C55 -173.3(5) . . . . ? O6 C56 C57 C55 2.1(7) . . . . ? C50 C55 C57 C58 97.4(6) . . . . ? C50 C55 C57 C56 -86.4(6) . . . . ? C56 C57 C58 C59 -0.8(7) . . . . ? C55 C57 C58 C59 175.6(5) . . . . ? C57 C58 C59 C60 -0.9(7) . . . . ? C57 C58 C59 C62 -177.2(5) . . . . ? C58 C59 C60 C61 0.5(7) . . . . ? C62 C59 C60 C61 176.7(5) . . . . ? C57 C56 C61 C60 -3.3(7) . . . . ? O6 C56 C61 C60 -178.9(4) . . . . ? C57 C56 C61 C66 170.5(5) . . . . ? O6 C56 C61 C66 -5.1(7) . . . . ? C59 C60 C61 C56 1.5(7) . . . . ? C59 C60 C61 C66 -172.4(5) . . . . ? C60 C59 C62 C64 13.0(7) . . . . ? C58 C59 C62 C64 -171.0(5) . . . . ? C60 C59 C62 C63 134.6(5) . . . . ? C58 C59 C62 C63 -49.4(6) . . . . ? C60 C59 C62 C65 -107.3(5) . . . . ? C58 C59 C62 C65 68.7(6) . . . . ? C56 C61 C66 C2 -78.0(6) . . . . ? C60 C61 C66 C2 95.5(5) . . . . ? C1 C2 C66 C61 98.8(6) . . . . ? C3 C2 C66 C61 -76.0(6) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O6 0.84 1.92 2.690(5) 152.2 . O2 H2 O1 0.84 1.94 2.716(5) 152.2 . O3 H3 O2 0.84 1.86 2.668(5) 160.7 . O4 H4 O3 0.84 1.82 2.608(5) 155.5 . O5 H5 O4 0.84 1.79 2.615(5) 164.9 . O6 H6 O5 0.84 1.83 2.643(5) 162.6 . _diffrn_measured_fraction_theta_max 0.939 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.939 _refine_diff_density_max 0.224 _refine_diff_density_min -0.252 _refine_diff_density_rms 0.055 #===END data_2 _database_code_CSD 215818 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C70 H90 N2 O6' _chemical_formula_weight 1055.44 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 monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.9380(9) _cell_length_b 16.9178(11) _cell_length_c 27.9606(18) _cell_angle_alpha 90.00 _cell_angle_beta 99.621(2) _cell_angle_gamma 90.00 _cell_volume 6500.4(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4701 _cell_measurement_theta_min 2.82 _cell_measurement_theta_max 26.33 _exptl_crystal_description 'thick needle' _exptl_crystal_colour colourless _exptl_crystal_size_max 0.47 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.078 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2288 _exptl_absorpt_coefficient_mu 0.067 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.969 _exptl_absorpt_correction_T_max 0.996 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 45775 _diffrn_reflns_av_R_equivalents 0.0738 _diffrn_reflns_av_sigmaI/netI 0.0984 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 25.00 _reflns_number_total 11441 _reflns_number_gt 5467 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0231P)^2^+8.7596P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00159(19) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 11441 _refine_ls_number_parameters 857 _refine_ls_number_restraints 437 _refine_ls_R_factor_all 0.1560 _refine_ls_R_factor_gt 0.0606 _refine_ls_wR_factor_ref 0.1945 _refine_ls_wR_factor_gt 0.1304 _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_restrained_S_all 1.038 _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 0.60065(18) 0.75109(14) 0.25532(8) 0.0412(6) Uani 1 1 d . . . H1 H 0.5677 0.7883 0.2641 0.062 Uiso 1 1 calc R . . O2 O 0.47608(18) 0.85927(15) 0.27468(9) 0.0460(7) Uani 1 1 d . . . H2 H 0.4391 0.8582 0.2955 0.069 Uiso 1 1 calc R . . O3 O 0.3815(2) 0.84227(16) 0.34779(10) 0.0560(8) Uani 1 1 d . . . H3 H 0.3956 0.8198 0.3748 0.084 Uiso 1 1 calc R . . O4 O 0.41673(17) 0.73574(15) 0.41705(8) 0.0418(6) Uani 1 1 d . . . H4 H 0.4117 0.7045 0.3934 0.063 Uiso 1 1 calc R . . O5 O 0.35974(19) 0.65262(16) 0.33718(9) 0.0502(7) Uani 1 1 d . . . H5 H 0.3830 0.6533 0.3113 0.075 Uiso 1 1 calc R . . O6 O 0.44792(18) 0.65829(15) 0.26029(9) 0.0464(7) Uani 1 1 d . . . H6 H 0.5062 0.6706 0.2599 0.070 Uiso 1 1 calc R . . C1 C 0.6018(2) 0.7571(2) 0.20575(12) 0.0358(9) Uani 1 1 d . . . C2 C 0.5963(2) 0.6881(2) 0.17833(13) 0.0359(8) Uani 1 1 d . . . C3 C 0.5955(2) 0.6944(2) 0.12865(12) 0.0376(9) Uani 1 1 d . . . H3A H 0.5913 0.6475 0.1098 0.045 Uiso 1 1 calc R . . C4 C 0.6005(2) 0.7667(2) 0.10555(12) 0.0381(9) Uani 1 1 d . . . C5 C 0.6081(2) 0.8341(2) 0.13497(12) 0.0390(9) Uani 1 1 d . . . H5A H 0.6140 0.8841 0.1204 0.047 Uiso 1 1 calc R . . C6 C 0.6075(2) 0.8311(2) 0.18449(12) 0.0357(8) Uani 1 1 d . . . C7 C 0.5967(3) 0.7756(2) 0.05086(13) 0.0447(10) Uani 1 1 d . . . C8 C 0.5163(3) 0.8350(3) 0.03038(14) 0.0603(12) Uani 1 1 d . . . H8A H 0.4533 0.8156 0.0366 0.090 Uiso 1 1 calc R . . H8B H 0.5143 0.8407 -0.0047 0.090 Uiso 1 1 calc R . . H8C H 0.5303 0.8864 0.0462 0.090 Uiso 1 1 calc R . . C9 C 0.6949(3) 0.8070(3) 0.04048(14) 0.0578(12) Uani 1 1 d . . . H9A H 0.7078 0.8591 0.0555 0.087 Uiso 1 1 calc R . . H9B H 0.6925 0.8115 0.0054 0.087 Uiso 1 1 calc R . . H9C H 0.7469 0.7703 0.0539 0.087 Uiso 1 1 calc R . . C10 C 0.5751(4) 0.6972(3) 0.02419(14) 0.0658(13) Uani 1 1 d . . . H10A H 0.6287 0.6602 0.0344 0.099 Uiso 1 1 calc R . . H10B H 0.5680 0.7061 -0.0109 0.099 Uiso 1 1 calc R . . H10C H 0.5146 0.6749 0.0319 0.099 Uiso 1 1 calc R . . C11 C 0.6045(2) 0.9082(2) 0.21249(13) 0.0381(9) Uani 1 1 d . . . H11A H 0.6310 0.8995 0.2472 0.046 Uiso 1 1 calc R . . H11B H 0.6452 0.9485 0.1998 0.046 Uiso 1 1 calc R . . C12 C 0.4379(3) 0.9096(2) 0.23731(12) 0.0361(9) Uani 1 1 d . . . C13 C 0.5006(3) 0.9373(2) 0.20727(12) 0.0362(8) Uani 1 1 d . . . C14 C 0.4626(3) 0.9877(2) 0.16946(13) 0.0432(9) Uani 1 1 d . . . H14 H 0.5050 1.0079 0.1491 0.052 Uiso 1 1 calc R . . C15 C 0.3649(3) 1.0095(2) 0.16024(14) 0.0454(10) Uani 1 1 d . A . C16 C 0.3054(3) 0.9788(2) 0.19076(13) 0.0436(9) Uani 1 1 d . . . H16 H 0.2384 0.9924 0.1851 0.052 Uiso 1 1 calc R . . C17 C 0.3399(3) 0.9285(2) 0.22951(12) 0.0375(9) Uani 1 1 d . . . C18 C 0.3253(3) 1.0624(3) 0.11692(16) 0.0598(12) Uani 1 1 d DU . . C19 C 0.3753(7) 1.1406(4) 0.1203(3) 0.068(2) Uani 0.721(8) 1 d PDU A 1 H19A H 0.4459 1.1326 0.1273 0.101 Uiso 0.721(8) 1 calc PR A 1 H19B H 0.3550 1.1717 0.1465 0.101 Uiso 0.721(8) 1 calc PR A 1 H19C H 0.3580 1.1689 0.0895 0.101 Uiso 0.721(8) 1 calc PR A 1 C20 C 0.3532(6) 1.0214(4) 0.0688(2) 0.076(2) Uani 0.721(8) 1 d PDU A 1 H20A H 0.3221 0.9694 0.0642 0.115 Uiso 0.721(8) 1 calc PR A 1 H20B H 0.4240 1.0152 0.0726 0.115 Uiso 0.721(8) 1 calc PR A 1 H20C H 0.3304 1.0547 0.0405 0.115 Uiso 0.721(8) 1 calc PR A 1 C21 C 0.2171(5) 1.0673(6) 0.1065(3) 0.095(3) Uani 0.721(8) 1 d PDU A 1 H21A H 0.1895 1.0139 0.1050 0.142 Uiso 0.721(8) 1 calc PR A 1 H21B H 0.1967 1.0939 0.0753 0.142 Uiso 0.721(8) 1 calc PR A 1 H21C H 0.1938 1.0974 0.1322 0.142 Uiso 0.721(8) 1 calc PR A 1 C19X C 0.4012(16) 1.1122(17) 0.1003(11) 0.132(11) Uani 0.279(8) 1 d PDU A 2 H19D H 0.4395 1.1390 0.1282 0.197 Uiso 0.279(8) 1 calc PR A 2 H19E H 0.3701 1.1517 0.0771 0.197 Uiso 0.279(8) 1 calc PR A 2 H19F H 0.4442 1.0788 0.0846 0.197 Uiso 0.279(8) 1 calc PR A 2 C20X C 0.2543(14) 1.0182(12) 0.0811(6) 0.089(6) Uani 0.279(8) 1 d PDU A 2 H20D H 0.2072 0.9914 0.0979 0.134 Uiso 0.279(8) 1 calc PR A 2 H20E H 0.2890 0.9789 0.0646 0.134 Uiso 0.279(8) 1 calc PR A 2 H20F H 0.2200 1.0551 0.0571 0.134 Uiso 0.279(8) 1 calc PR A 2 C21X C 0.2587(13) 1.1262(9) 0.1401(6) 0.076(5) Uani 0.279(8) 1 d PDU A 2 H21D H 0.3003 1.1587 0.1641 0.114 Uiso 0.279(8) 1 calc PR A 2 H21E H 0.2108 1.0982 0.1557 0.114 Uiso 0.279(8) 1 calc PR A 2 H21F H 0.2249 1.1603 0.1143 0.114 Uiso 0.279(8) 1 calc PR A 2 C22 C 0.2694(3) 0.8914(2) 0.25849(13) 0.0418(9) Uani 1 1 d . . . H22A H 0.2884 0.8354 0.2643 0.050 Uiso 1 1 calc R . . H22B H 0.2042 0.8918 0.2381 0.050 Uiso 1 1 calc R . . C23 C 0.3119(3) 0.8994(2) 0.35025(13) 0.0412(9) Uani 1 1 d . . . C24 C 0.2601(3) 0.9281(2) 0.30709(13) 0.0394(9) Uani 1 1 d . . . C25 C 0.1930(3) 0.9885(2) 0.30936(14) 0.0413(9) Uani 1 1 d . . . H25 H 0.1591 1.0101 0.2800 0.050 Uiso 1 1 calc R . . C26 C 0.1740(3) 1.0182(2) 0.35336(15) 0.0431(9) Uani 1 1 d . . . C27 C 0.2251(3) 0.9842(2) 0.39569(14) 0.0464(10) Uani 1 1 d . . . H27 H 0.2121 1.0024 0.4261 0.056 Uiso 1 1 calc R . . C28 C 0.2936(3) 0.9254(2) 0.39519(13) 0.0420(9) Uani 1 1 d . . . C29 C 0.0977(3) 1.0823(2) 0.35620(15) 0.0494(10) Uani 1 1 d . . . C30 C 0.0634(4) 1.1221(3) 0.30728(17) 0.0769(15) Uani 1 1 d . . . H30A H 0.1192 1.1460 0.2956 0.115 Uiso 1 1 calc R . . H30B H 0.0158 1.1633 0.3111 0.115 Uiso 1 1 calc R . . H30C H 0.0331 1.0827 0.2839 0.115 Uiso 1 1 calc R . . C31 C 0.1409(3) 1.1463(2) 0.39266(16) 0.0630(12) Uani 1 1 d . . . H31A H 0.1617 1.1222 0.4246 0.094 Uiso 1 1 calc R . . H31B H 0.0915 1.1867 0.3950 0.094 Uiso 1 1 calc R . . H31C H 0.1971 1.1708 0.3816 0.094 Uiso 1 1 calc R . . C32 C 0.0096(3) 1.0452(3) 0.3735(2) 0.0888(18) Uani 1 1 d . . . H32A H -0.0177 1.0038 0.3507 0.133 Uiso 1 1 calc R . . H32B H -0.0397 1.0860 0.3751 0.133 Uiso 1 1 calc R . . H32C H 0.0297 1.0221 0.4057 0.133 Uiso 1 1 calc R . . C33 C 0.3411(3) 0.8849(2) 0.44184(13) 0.0472(10) Uani 1 1 d . . . H33A H 0.4109 0.8762 0.4407 0.057 Uiso 1 1 calc R . . H33B H 0.3365 0.9200 0.4697 0.057 Uiso 1 1 calc R . . C34 C 0.3307(3) 0.7351(2) 0.43619(12) 0.0392(9) Uani 1 1 d . . . C35 C 0.2935(3) 0.8063(2) 0.44947(12) 0.0412(9) Uani 1 1 d . . . C36 C 0.2067(3) 0.8049(3) 0.46818(13) 0.0501(11) Uani 1 1 d . . . H36 H 0.1809 0.8533 0.4777 0.060 Uiso 1 1 calc R . . C37 C 0.1564(3) 0.7350(3) 0.47332(13) 0.0511(11) Uani 1 1 d . B . C38 C 0.1984(3) 0.6652(3) 0.46018(13) 0.0474(10) Uani 1 1 d . . . H38 H 0.1667 0.6166 0.4642 0.057 Uiso 1 1 calc R . . C39 C 0.2845(3) 0.6637(2) 0.44154(12) 0.0416(9) Uani 1 1 d . . . C40 C 0.0591(3) 0.7352(3) 0.49196(16) 0.0651(12) Uani 1 1 d DU . . C41 C 0.0330(11) 0.8155(6) 0.5103(7) 0.143(7) Uani 0.620(13) 1 d PDU B 1 H41A H 0.0839 0.8325 0.5368 0.214 Uiso 0.620(13) 1 calc PR B 1 H41B H -0.0293 0.8119 0.5220 0.214 Uiso 0.620(13) 1 calc PR B 1 H41C H 0.0275 0.8540 0.4838 0.214 Uiso 0.620(13) 1 calc PR B 1 C42 C -0.0192(6) 0.7093(9) 0.4520(4) 0.114(5) Uani 0.620(13) 1 d PDU B 1 H42A H -0.0022 0.6577 0.4398 0.171 Uiso 0.620(13) 1 calc PR B 1 H42B H -0.0260 0.7481 0.4256 0.171 Uiso 0.620(13) 1 calc PR B 1 H42C H -0.0808 0.7050 0.4643 0.171 Uiso 0.620(13) 1 calc PR B 1 C43 C 0.0631(7) 0.6756(7) 0.5334(4) 0.110(5) Uani 0.620(13) 1 d PDU B 1 H43A H 0.1145 0.6909 0.5601 0.165 Uiso 0.620(13) 1 calc PR B 1 H43B H 0.0770 0.6229 0.5217 0.165 Uiso 0.620(13) 1 calc PR B 1 H43C H 0.0004 0.6749 0.5448 0.165 Uiso 0.620(13) 1 calc PR B 1 C41X C 0.0761(13) 0.7684(17) 0.5423(5) 0.127(9) Uani 0.380(13) 1 d PDU B 2 H41D H 0.1220 0.7346 0.5635 0.190 Uiso 0.380(13) 1 calc PR B 2 H41E H 0.0143 0.7706 0.5546 0.190 Uiso 0.380(13) 1 calc PR B 2 H41F H 0.1031 0.8218 0.5418 0.190 Uiso 0.380(13) 1 calc PR B 2 C42X C -0.0125(11) 0.7865(14) 0.4590(8) 0.125(8) Uani 0.380(13) 1 d PDU B 2 H42D H -0.0236 0.7642 0.4262 0.187 Uiso 0.380(13) 1 calc PR B 2 H42E H 0.0140 0.8400 0.4581 0.187 Uiso 0.380(13) 1 calc PR B 2 H42F H -0.0742 0.7886 0.4714 0.187 Uiso 0.380(13) 1 calc PR B 2 C43X C 0.0116(12) 0.6533(8) 0.4911(8) 0.107(7) Uani 0.380(13) 1 d PDU B 2 H43D H -0.0013 0.6336 0.4576 0.160 Uiso 0.380(13) 1 calc PR B 2 H43E H -0.0497 0.6573 0.5036 0.160 Uiso 0.380(13) 1 calc PR B 2 H43F H 0.0555 0.6168 0.5113 0.160 Uiso 0.380(13) 1 calc PR B 2 C44 C 0.3229(3) 0.5856(2) 0.42570(13) 0.0449(10) Uani 1 1 d . . . H44A H 0.3932 0.5910 0.4245 0.054 Uiso 1 1 calc R . . H44B H 0.3153 0.5445 0.4500 0.054 Uiso 1 1 calc R . . C45 C 0.2878(3) 0.5953(2) 0.33401(13) 0.0377(9) Uani 1 1 d . . . C46 C 0.2703(3) 0.5593(2) 0.37633(13) 0.0381(9) Uani 1 1 d . . . C47 C 0.1992(3) 0.5016(2) 0.37232(14) 0.0414(9) Uani 1 1 d . . . H47 H 0.1867 0.4766 0.4011 0.050 Uiso 1 1 calc R . . C48 C 0.1450(3) 0.4782(2) 0.32814(13) 0.0391(9) Uani 1 1 d . C . C49 C 0.1640(2) 0.5175(2) 0.28707(13) 0.0385(9) Uani 1 1 d . . . H49 H 0.1276 0.5035 0.2564 0.046 Uiso 1 1 calc R . . C50 C 0.2339(3) 0.5764(2) 0.28898(12) 0.0367(9) Uani 1 1 d . . . C51 C 0.0660(3) 0.4156(2) 0.32566(15) 0.0507(10) Uani 1 1 d DU . . C52 C -0.0234(4) 0.4538(3) 0.3434(2) 0.0632(18) Uani 0.786(7) 1 d PDU C 1 H52A H -0.0453 0.4997 0.3231 0.076 Uiso 0.786(7) 1 calc PR C 1 H52B H -0.0051 0.4706 0.3772 0.076 Uiso 0.786(7) 1 calc PR C 1 H52C H -0.0763 0.4150 0.3409 0.076 Uiso 0.786(7) 1 calc PR C 1 C53 C 0.0288(4) 0.3856(4) 0.27366(19) 0.0638(18) Uani 0.786(7) 1 d PDU C 1 H53A H 0.0078 0.4306 0.2524 0.077 Uiso 0.786(7) 1 calc PR C 1 H53B H -0.0263 0.3497 0.2741 0.077 Uiso 0.786(7) 1 calc PR C 1 H53C H 0.0812 0.3573 0.2615 0.077 Uiso 0.786(7) 1 calc PR C 1 C54 C 0.0979(5) 0.3452(3) 0.3571(3) 0.068(2) Uani 0.786(7) 1 d PDU C 1 H54A H 0.0448 0.3067 0.3542 0.081 Uiso 0.786(7) 1 calc PR C 1 H54B H 0.1151 0.3622 0.3909 0.081 Uiso 0.786(7) 1 calc PR C 1 H54C H 0.1547 0.3209 0.3466 0.081 Uiso 0.786(7) 1 calc PR C 1 C52X C 0.0540(16) 0.3921(15) 0.3790(5) 0.079(7) Uani 0.214(7) 1 d PDU C 2 H52D H 0.1173 0.3766 0.3973 0.094 Uiso 0.214(7) 1 calc PR C 2 H52E H 0.0085 0.3477 0.3778 0.094 Uiso 0.214(7) 1 calc PR C 2 H52F H 0.0286 0.4374 0.3948 0.094 Uiso 0.214(7) 1 calc PR C 2 C53X C -0.0234(12) 0.4395(14) 0.2951(9) 0.086(9) Uani 0.214(7) 1 d PDU C 2 H53D H -0.0720 0.3975 0.2945 0.103 Uiso 0.214(7) 1 calc PR C 2 H53E H -0.0111 0.4492 0.2621 0.103 Uiso 0.214(7) 1 calc PR C 2 H53F H -0.0477 0.4880 0.3081 0.103 Uiso 0.214(7) 1 calc PR C 2 C54X C 0.1162(15) 0.3408(10) 0.3087(10) 0.083(7) Uani 0.214(7) 1 d PDU C 2 H54D H 0.1765 0.3302 0.3313 0.099 Uiso 0.214(7) 1 calc PR C 2 H54E H 0.1313 0.3498 0.2762 0.099 Uiso 0.214(7) 1 calc PR C 2 H54F H 0.0724 0.2954 0.3081 0.099 Uiso 0.214(7) 1 calc PR C 2 C55 C 0.2463(3) 0.6215(2) 0.24330(12) 0.0388(9) Uani 1 1 d . . . H55A H 0.1818 0.6254 0.2223 0.047 Uiso 1 1 calc R . . H55B H 0.2676 0.6759 0.2528 0.047 Uiso 1 1 calc R . . C56 C 0.4156(3) 0.6074(2) 0.22195(12) 0.0358(8) Uani 1 1 d . . . C57 C 0.3177(3) 0.5868(2) 0.21343(12) 0.0364(9) Uani 1 1 d . . . C58 C 0.2858(3) 0.5359(2) 0.17495(12) 0.0408(9) Uani 1 1 d . . . H58 H 0.2192 0.5210 0.1689 0.049 Uiso 1 1 calc R . . C59 C 0.3467(3) 0.5061(2) 0.14505(13) 0.0414(9) Uani 1 1 d . D . C60 C 0.4442(3) 0.5295(2) 0.15491(13) 0.0399(9) Uani 1 1 d . . . H60 H 0.4875 0.5101 0.1348 0.048 Uiso 1 1 calc R . . C61 C 0.4803(3) 0.5799(2) 0.19276(12) 0.0372(9) Uani 1 1 d . . . C62 C 0.3094(3) 0.4513(3) 0.10237(14) 0.0546(11) Uani 1 1 d DU . . C63 C 0.2013(5) 0.4390(8) 0.0930(4) 0.098(4) Uani 0.610(10) 1 d PDU D 1 H63A H 0.1838 0.4030 0.0654 0.118 Uiso 0.610(10) 1 calc PR D 1 H63B H 0.1686 0.4899 0.0856 0.118 Uiso 0.610(10) 1 calc PR D 1 H63C H 0.1808 0.4160 0.1219 0.118 Uiso 0.610(10) 1 calc PR D 1 C64 C 0.3584(7) 0.3686(4) 0.1120(3) 0.069(3) Uani 0.610(10) 1 d PDU D 1 H64A H 0.4293 0.3748 0.1179 0.083 Uiso 0.610(10) 1 calc PR D 1 H64B H 0.3391 0.3346 0.0836 0.083 Uiso 0.610(10) 1 calc PR D 1 H64C H 0.3377 0.3444 0.1404 0.083 Uiso 0.610(10) 1 calc PR D 1 C65 C 0.3412(9) 0.4822(5) 0.0560(3) 0.082(3) Uani 0.610(10) 1 d PDU D 1 H65A H 0.4117 0.4908 0.0619 0.098 Uiso 0.610(10) 1 calc PR D 1 H65B H 0.3080 0.5323 0.0466 0.098 Uiso 0.610(10) 1 calc PR D 1 H65C H 0.3243 0.4435 0.0299 0.098 Uiso 0.610(10) 1 calc PR D 1 C63X C 0.2282(10) 0.4976(9) 0.0698(4) 0.078(4) Uani 0.390(10) 1 d PDU D 2 H63D H 0.2563 0.5438 0.0562 0.093 Uiso 0.390(10) 1 calc PR D 2 H63E H 0.1795 0.5150 0.0891 0.093 Uiso 0.390(10) 1 calc PR D 2 H63F H 0.1971 0.4634 0.0434 0.093 Uiso 0.390(10) 1 calc PR D 2 C64X C 0.2649(14) 0.3800(8) 0.1240(5) 0.109(6) Uani 0.390(10) 1 d PDU D 2 H64D H 0.2402 0.3425 0.0981 0.131 Uiso 0.390(10) 1 calc PR D 2 H64E H 0.2113 0.3975 0.1400 0.131 Uiso 0.390(10) 1 calc PR D 2 H64F H 0.3147 0.3541 0.1478 0.131 Uiso 0.390(10) 1 calc PR D 2 C65X C 0.3877(9) 0.4309(12) 0.0734(6) 0.106(7) Uani 0.390(10) 1 d PDU D 2 H65D H 0.4110 0.4794 0.0599 0.127 Uiso 0.390(10) 1 calc PR D 2 H65E H 0.3613 0.3951 0.0469 0.127 Uiso 0.390(10) 1 calc PR D 2 H65F H 0.4419 0.4051 0.0945 0.127 Uiso 0.390(10) 1 calc PR D 2 C66 C 0.5854(2) 0.6074(2) 0.20039(13) 0.0395(9) Uani 1 1 d . . . H66A H 0.6109 0.6095 0.2356 0.047 Uiso 1 1 calc R . . H66B H 0.6249 0.5685 0.1856 0.047 Uiso 1 1 calc R . . N1 N 0.1783(3) 0.7651(3) 0.16330(15) 0.0794(12) Uani 1 1 d D . . C67 C 0.2498(4) 0.7662(3) 0.14832(17) 0.0620(12) Uani 1 1 d D . . C68 C 0.3398(4) 0.7682(3) 0.1295(2) 0.0886(17) Uani 1 1 d D . . H68A H 0.3814 0.7243 0.1433 0.133 Uiso 1 1 calc R . . H68B H 0.3732 0.8184 0.1384 0.133 Uiso 1 1 calc R . . H68C H 0.3262 0.7632 0.0941 0.133 Uiso 1 1 calc R . . N2 N -0.0386(10) 0.6683(7) 0.3191(4) 0.189(6) Uani 0.640(7) 1 d PDU E 1 C69 C 0.0285(9) 0.7086(7) 0.3252(3) 0.106(4) Uani 0.640(7) 1 d PDU E 1 C70 C 0.1133(11) 0.7578(11) 0.3336(11) 0.074(4) Uani 0.640(7) 1 d PDU E 1 H70A H 0.1439 0.7586 0.3045 0.112 Uiso 0.640(7) 1 calc PR E 1 H70B H 0.1595 0.7368 0.3610 0.112 Uiso 0.640(7) 1 calc PR E 1 H70C H 0.0946 0.8117 0.3411 0.112 Uiso 0.640(7) 1 calc PR E 1 N2X N -0.0270(17) 0.8436(11) 0.3411(8) 0.192(11) Uani 0.360(7) 1 d PDU E 2 C69X C 0.0344(14) 0.8011(12) 0.3360(6) 0.107(6) Uani 0.360(7) 1 d PDU E 2 C70X C 0.109(2) 0.749(2) 0.326(2) 0.096(13) Uani 0.360(7) 1 d PDU E 2 H70D H 0.1363 0.7194 0.3550 0.144 Uiso 0.360(7) 1 calc PR E 2 H70E H 0.1612 0.7799 0.3148 0.144 Uiso 0.360(7) 1 calc PR E 2 H70F H 0.0821 0.7119 0.3000 0.144 Uiso 0.360(7) 1 calc PR E 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0447(16) 0.0462(16) 0.0337(14) 0.0004(12) 0.0096(11) 0.0053(12) O2 0.0534(17) 0.0505(16) 0.0374(15) 0.0101(13) 0.0172(13) 0.0094(13) O3 0.0693(19) 0.0560(18) 0.0496(17) 0.0155(14) 0.0298(15) 0.0219(15) O4 0.0414(15) 0.0521(17) 0.0330(15) -0.0054(12) 0.0091(11) 0.0006(12) O5 0.0540(17) 0.0585(18) 0.0433(16) -0.0111(14) 0.0233(13) -0.0172(14) O6 0.0493(16) 0.0495(16) 0.0427(15) -0.0064(13) 0.0145(13) -0.0109(14) C1 0.034(2) 0.045(2) 0.030(2) 0.0005(17) 0.0091(16) -0.0021(17) C2 0.0312(19) 0.038(2) 0.040(2) 0.0025(17) 0.0100(16) 0.0055(16) C3 0.036(2) 0.040(2) 0.038(2) -0.0034(17) 0.0085(16) 0.0006(17) C4 0.036(2) 0.046(2) 0.033(2) -0.0018(18) 0.0061(16) -0.0023(17) C5 0.036(2) 0.045(2) 0.036(2) 0.0036(18) 0.0054(16) -0.0057(17) C6 0.0308(19) 0.042(2) 0.034(2) 0.0002(17) 0.0054(16) -0.0026(17) C7 0.044(2) 0.057(3) 0.032(2) -0.0009(19) 0.0058(17) -0.003(2) C8 0.062(3) 0.079(3) 0.037(2) 0.001(2) -0.001(2) 0.014(2) C9 0.058(3) 0.081(3) 0.036(2) 0.013(2) 0.011(2) -0.001(2) C10 0.098(4) 0.064(3) 0.034(2) -0.010(2) 0.009(2) -0.004(3) C11 0.040(2) 0.038(2) 0.036(2) 0.0027(17) 0.0052(17) -0.0067(17) C12 0.044(2) 0.034(2) 0.031(2) 0.0008(16) 0.0095(17) 0.0000(17) C13 0.041(2) 0.034(2) 0.033(2) -0.0038(16) 0.0062(16) -0.0028(17) C14 0.045(2) 0.045(2) 0.039(2) 0.0080(18) 0.0063(18) -0.0094(19) C15 0.043(2) 0.050(2) 0.044(2) 0.0083(19) 0.0056(19) -0.0031(19) C16 0.041(2) 0.045(2) 0.045(2) 0.0019(19) 0.0067(18) -0.0028(18) C17 0.042(2) 0.038(2) 0.034(2) -0.0018(17) 0.0102(17) -0.0050(17) C18 0.047(2) 0.071(3) 0.058(3) 0.026(2) 0.000(2) -0.001(2) C19 0.085(6) 0.050(4) 0.063(6) 0.020(3) 0.000(4) 0.006(4) C20 0.113(6) 0.072(5) 0.041(4) 0.015(3) 0.003(4) 0.013(4) C21 0.057(4) 0.145(9) 0.078(6) 0.055(6) -0.002(4) 0.013(4) C19X 0.073(14) 0.19(3) 0.13(3) 0.12(2) 0.008(11) -0.013(14) C20X 0.089(15) 0.123(16) 0.050(11) -0.003(9) -0.005(10) 0.017(10) C21X 0.083(13) 0.075(12) 0.061(11) 0.027(8) -0.016(8) 0.011(9) C22 0.044(2) 0.040(2) 0.044(2) -0.0020(18) 0.0154(18) -0.0057(18) C23 0.048(2) 0.035(2) 0.044(2) -0.0013(18) 0.0191(19) 0.0026(18) C24 0.043(2) 0.038(2) 0.039(2) -0.0017(17) 0.0136(18) -0.0089(18) C25 0.038(2) 0.040(2) 0.047(2) -0.0033(18) 0.0107(18) -0.0047(18) C26 0.037(2) 0.037(2) 0.057(3) -0.0041(19) 0.0126(19) -0.0031(17) C27 0.050(2) 0.045(2) 0.048(2) -0.0085(19) 0.018(2) 0.000(2) C28 0.045(2) 0.042(2) 0.040(2) -0.0042(18) 0.0111(18) -0.0018(18) C29 0.044(2) 0.041(2) 0.066(3) -0.007(2) 0.015(2) 0.0008(19) C30 0.079(3) 0.071(3) 0.076(3) -0.009(3) 0.000(3) 0.031(3) C31 0.062(3) 0.053(3) 0.076(3) -0.015(2) 0.016(2) 0.006(2) C32 0.048(3) 0.069(3) 0.156(5) -0.002(3) 0.037(3) 0.003(3) C33 0.052(2) 0.053(3) 0.039(2) -0.0085(19) 0.0123(19) 0.002(2) C34 0.038(2) 0.053(2) 0.027(2) 0.0005(17) 0.0062(16) -0.0014(19) C35 0.044(2) 0.052(2) 0.0282(19) -0.0023(18) 0.0079(17) 0.0017(19) C36 0.053(3) 0.064(3) 0.035(2) -0.006(2) 0.0154(19) 0.010(2) C37 0.050(2) 0.072(3) 0.034(2) -0.002(2) 0.0141(19) -0.001(2) C38 0.051(2) 0.061(3) 0.032(2) 0.0022(19) 0.0120(18) -0.002(2) C39 0.045(2) 0.053(2) 0.0266(19) 0.0025(18) 0.0067(17) 0.0003(19) C40 0.054(3) 0.095(4) 0.053(3) -0.008(2) 0.027(2) -0.002(2) C41 0.117(12) 0.127(8) 0.220(17) -0.066(9) 0.129(12) -0.020(7) C42 0.043(5) 0.213(16) 0.087(6) -0.029(8) 0.013(4) -0.004(8) C43 0.081(7) 0.186(11) 0.075(7) 0.030(8) 0.047(6) -0.011(8) C41X 0.085(13) 0.24(3) 0.075(9) -0.062(12) 0.059(8) -0.021(14) C42X 0.043(9) 0.184(19) 0.153(15) 0.064(16) 0.034(10) 0.036(12) C43X 0.077(12) 0.128(10) 0.128(18) 0.004(10) 0.054(13) -0.017(9) C44 0.046(2) 0.048(2) 0.041(2) 0.0055(19) 0.0089(18) -0.0015(19) C45 0.037(2) 0.038(2) 0.040(2) -0.0009(17) 0.0123(17) -0.0022(17) C46 0.038(2) 0.040(2) 0.038(2) 0.0035(17) 0.0099(17) 0.0057(17) C47 0.045(2) 0.039(2) 0.044(2) 0.0050(18) 0.0150(19) 0.0033(18) C48 0.035(2) 0.036(2) 0.047(2) 0.0017(18) 0.0109(18) 0.0016(17) C49 0.035(2) 0.039(2) 0.042(2) -0.0016(17) 0.0084(17) 0.0037(17) C50 0.037(2) 0.038(2) 0.036(2) -0.0003(17) 0.0125(17) 0.0032(17) C51 0.044(2) 0.046(2) 0.060(3) 0.007(2) 0.005(2) -0.0074(19) C52 0.042(3) 0.066(4) 0.084(5) -0.004(3) 0.016(3) -0.008(3) C53 0.061(4) 0.061(4) 0.067(4) -0.004(3) 0.006(3) -0.019(3) C54 0.062(4) 0.050(4) 0.085(5) 0.017(3) -0.007(4) -0.009(3) C52X 0.058(15) 0.095(19) 0.078(10) 0.031(11) 0.000(9) -0.050(13) C53X 0.050(11) 0.089(17) 0.106(19) 0.047(16) -0.019(12) -0.023(10) C54X 0.079(15) 0.041(11) 0.13(2) -0.008(12) 0.009(14) -0.025(8) C55 0.039(2) 0.042(2) 0.037(2) 0.0025(17) 0.0098(17) 0.0039(17) C56 0.043(2) 0.035(2) 0.0300(19) -0.0010(16) 0.0086(17) -0.0014(17) C57 0.038(2) 0.037(2) 0.035(2) 0.0027(17) 0.0084(16) 0.0041(17) C58 0.045(2) 0.044(2) 0.033(2) -0.0004(18) 0.0051(17) 0.0001(18) C59 0.047(2) 0.044(2) 0.035(2) -0.0024(17) 0.0107(18) 0.0059(19) C60 0.048(2) 0.038(2) 0.036(2) 0.0008(17) 0.0145(18) 0.0091(18) C61 0.042(2) 0.035(2) 0.037(2) 0.0048(17) 0.0139(17) 0.0065(17) C62 0.054(3) 0.065(3) 0.044(2) -0.017(2) 0.0038(19) 0.002(2) C63 0.059(5) 0.141(11) 0.093(8) -0.073(8) 0.007(5) -0.011(5) C64 0.099(7) 0.048(4) 0.056(5) -0.014(4) 0.001(5) -0.007(4) C65 0.131(9) 0.074(6) 0.038(4) -0.008(4) 0.012(5) -0.014(6) C63X 0.060(8) 0.114(11) 0.053(8) -0.027(7) -0.008(6) 0.011(7) C64X 0.154(18) 0.061(8) 0.101(11) -0.030(7) -0.011(9) -0.034(10) C65X 0.075(9) 0.157(18) 0.079(11) -0.079(12) -0.004(7) 0.023(8) C66 0.040(2) 0.039(2) 0.041(2) 0.0042(17) 0.0102(17) 0.0068(17) N1 0.079(3) 0.083(3) 0.077(3) 0.017(2) 0.016(2) 0.015(3) C67 0.060(3) 0.064(3) 0.059(3) 0.009(2) -0.001(2) 0.013(3) C68 0.060(3) 0.105(4) 0.100(4) 0.011(3) 0.014(3) 0.005(3) N2 0.228(13) 0.182(12) 0.177(11) -0.021(8) 0.091(10) -0.109(10) C69 0.139(10) 0.108(9) 0.081(6) -0.005(6) 0.047(6) -0.032(6) C70 0.084(9) 0.084(9) 0.053(8) 0.012(8) 0.006(6) 0.010(6) N2X 0.25(2) 0.123(16) 0.24(2) -0.018(15) 0.131(19) 0.063(14) C69X 0.126(15) 0.105(14) 0.092(12) -0.010(10) 0.020(11) 0.025(10) C70X 0.078(19) 0.13(2) 0.09(3) -0.007(16) 0.020(15) 0.005(14) _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 1.393(4) . ? O2 C12 1.384(4) . ? O3 C23 1.379(4) . ? O4 C34 1.393(4) . ? O5 C45 1.387(4) . ? O6 C56 1.390(4) . ? C1 C2 1.391(5) . ? C1 C6 1.393(5) . ? C2 C3 1.391(5) . ? C2 C66 1.517(5) . ? C3 C4 1.391(5) . ? C4 C5 1.398(5) . ? C4 C7 1.529(5) . ? C5 C6 1.387(5) . ? C6 C11 1.526(5) . ? C7 C10 1.527(5) . ? C7 C9 1.540(5) . ? C7 C8 1.542(5) . ? C11 C13 1.514(5) . ? C12 C17 1.385(5) . ? C12 C13 1.390(5) . ? C13 C14 1.391(5) . ? C14 C15 1.393(5) . ? C15 C16 1.387(5) . ? C15 C18 1.533(5) . ? C16 C17 1.397(5) . ? C17 C22 1.510(5) . ? C18 C20X 1.487(14) . ? C18 C19X 1.487(13) . ? C18 C21 1.490(7) . ? C18 C19 1.492(7) . ? C18 C20 1.618(7) . ? C18 C21X 1.626(12) . ? C22 C24 1.519(5) . ? C23 C24 1.386(5) . ? C23 C28 1.394(5) . ? C24 C25 1.395(5) . ? C25 C26 1.395(5) . ? C26 C27 1.399(5) . ? C26 C29 1.529(5) . ? C27 C28 1.381(5) . ? C28 C33 1.523(5) . ? C29 C32 1.528(6) . ? C29 C30 1.528(6) . ? C29 C31 1.539(5) . ? C33 C35 1.516(5) . ? C34 C35 1.386(5) . ? C34 C39 1.388(5) . ? C35 C36 1.397(5) . ? C36 C37 1.395(6) . ? C37 C38 1.394(5) . ? C37 C40 1.531(5) . ? C38 C39 1.386(5) . ? C39 C44 1.520(5) . ? C40 C42 1.492(9) . ? C40 C41X 1.498(11) . ? C40 C42X 1.514(12) . ? C40 C41 1.518(9) . ? C40 C43 1.528(8) . ? C40 C43X 1.533(11) . ? C44 C46 1.517(5) . ? C45 C46 1.388(5) . ? C45 C50 1.391(5) . ? C46 C47 1.383(5) . ? C47 C48 1.393(5) . ? C48 C49 1.390(5) . ? C48 C51 1.521(5) . ? C49 C50 1.388(5) . ? C50 C55 1.523(5) . ? C51 C53X 1.445(14) . ? C51 C54 1.502(6) . ? C51 C53 1.546(6) . ? C51 C52 1.556(6) . ? C51 C54X 1.557(13) . ? C51 C52X 1.578(13) . ? C55 C57 1.520(5) . ? C56 C57 1.390(5) . ? C56 C61 1.394(5) . ? C57 C58 1.391(5) . ? C58 C59 1.382(5) . ? C59 C60 1.398(5) . ? C59 C62 1.533(5) . ? C60 C61 1.386(5) . ? C61 C66 1.519(5) . ? C62 C63 1.500(8) . ? C62 C65X 1.505(10) . ? C62 C64X 1.527(12) . ? C62 C65 1.531(7) . ? C62 C63X 1.543(10) . ? C62 C64 1.560(8) . ? N1 C67 1.144(5) . ? C67 C68 1.439(7) . ? N2 C69 1.147(11) . ? C69 C70 1.432(17) . ? N2X C69X 1.145(14) . ? C69X C70X 1.434(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 C2 C1 O1 118.6(3) . . ? C2 C1 C6 121.3(3) . . ? O1 C1 C6 120.1(3) . . ? C3 C2 C1 118.5(3) . . ? C3 C2 C66 119.4(3) . . ? C1 C2 C66 122.1(3) . . ? C4 C3 C2 122.6(3) . . ? C3 C4 C5 116.6(3) . . ? C3 C4 C7 123.7(3) . . ? C5 C4 C7 119.7(3) . . ? C6 C5 C4 123.0(3) . . ? C5 C6 C1 118.0(3) . . ? C5 C6 C11 119.1(3) . . ? C1 C6 C11 122.7(3) . . ? C10 C7 C4 112.0(3) . . ? C10 C7 C9 108.4(3) . . ? C4 C7 C9 109.8(3) . . ? C10 C7 C8 108.2(3) . . ? C4 C7 C8 109.7(3) . . ? C9 C7 C8 108.6(3) . . ? C13 C11 C6 109.7(3) . . ? O2 C12 C17 120.4(3) . . ? O2 C12 C13 117.6(3) . . ? C17 C12 C13 122.0(3) . . ? C12 C13 C14 117.9(3) . . ? C12 C13 C11 121.3(3) . . ? C14 C13 C11 120.6(3) . . ? C13 C14 C15 122.6(3) . . ? C16 C15 C14 116.9(3) . . ? C16 C15 C18 122.1(3) . . ? C14 C15 C18 120.9(3) . . ? C15 C16 C17 122.8(4) . . ? C12 C17 C16 117.7(3) . . ? C12 C17 C22 122.2(3) . . ? C16 C17 C22 119.9(3) . . ? C20X C18 C19X 120.2(13) . . ? C21 C18 C19 114.3(6) . . ? C20X C18 C15 110.5(9) . . ? C19X C18 C15 113.3(12) . . ? C21 C18 C15 114.0(4) . . ? C19 C18 C15 111.4(5) . . ? C21 C18 C20 103.7(5) . . ? C19 C18 C20 105.0(5) . . ? C15 C18 C20 107.5(4) . . ? C20X C18 C21X 104.1(10) . . ? C19X C18 C21X 103.4(14) . . ? C15 C18 C21X 103.2(6) . . ? C17 C22 C24 118.1(3) . . ? O3 C23 C24 118.0(3) . . ? O3 C23 C28 120.1(3) . . ? C24 C23 C28 121.8(3) . . ? C23 C24 C25 118.2(3) . . ? C23 C24 C22 121.8(3) . . ? C25 C24 C22 119.9(3) . . ? C26 C25 C24 122.1(4) . . ? C25 C26 C27 117.0(3) . . ? C25 C26 C29 122.5(4) . . ? C27 C26 C29 120.5(4) . . ? C28 C27 C26 122.9(4) . . ? C27 C28 C23 117.9(4) . . ? C27 C28 C33 121.2(3) . . ? C23 C28 C33 120.7(3) . . ? C32 C29 C30 108.4(4) . . ? C32 C29 C26 109.2(3) . . ? C30 C29 C26 112.5(3) . . ? C32 C29 C31 109.0(4) . . ? C30 C29 C31 108.2(3) . . ? C26 C29 C31 109.5(3) . . ? C35 C33 C28 112.2(3) . . ? C35 C34 C39 121.8(3) . . ? C35 C34 O4 118.7(3) . . ? C39 C34 O4 119.5(3) . . ? C34 C35 C36 118.1(4) . . ? C34 C35 C33 122.2(3) . . ? C36 C35 C33 119.6(4) . . ? C37 C36 C35 122.3(4) . . ? C38 C37 C36 116.8(4) . . ? C38 C37 C40 121.8(4) . . ? C36 C37 C40 121.5(4) . . ? C39 C38 C37 122.9(4) . . ? C38 C39 C34 118.1(4) . . ? C38 C39 C44 119.6(4) . . ? C34 C39 C44 122.2(3) . . ? C41X C40 C42X 109.9(11) . . ? C42 C40 C41 109.2(8) . . ? C42 C40 C43 107.7(7) . . ? C41 C40 C43 108.4(8) . . ? C42 C40 C37 108.8(5) . . ? C41X C40 C37 108.1(7) . . ? C42X C40 C37 109.0(7) . . ? C41 C40 C37 113.1(5) . . ? C43 C40 C37 109.5(5) . . ? C41X C40 C43X 110.8(11) . . ? C42X C40 C43X 105.6(10) . . ? C37 C40 C43X 113.4(7) . . ? C46 C44 C39 112.3(3) . . ? O5 C45 C46 118.7(3) . . ? O5 C45 C50 119.6(3) . . ? C46 C45 C50 121.7(3) . . ? C47 C46 C45 117.8(3) . . ? C47 C46 C44 120.8(3) . . ? C45 C46 C44 121.3(3) . . ? C46 C47 C48 123.2(3) . . ? C49 C48 C47 116.6(3) . . ? C49 C48 C51 122.1(3) . . ? C47 C48 C51 121.3(3) . . ? C50 C49 C48 122.7(3) . . ? C49 C50 C45 118.0(3) . . ? C49 C50 C55 120.3(3) . . ? C45 C50 C55 121.6(3) . . ? C53X C51 C48 112.2(9) . . ? C54 C51 C48 112.6(4) . . ? C54 C51 C53 108.0(4) . . ? C48 C51 C53 113.5(4) . . ? C54 C51 C52 108.5(4) . . ? C48 C51 C52 108.0(3) . . ? C53 C51 C52 106.0(4) . . ? C53X C51 C54X 115.8(13) . . ? C48 C51 C54X 102.8(8) . . ? C53X C51 C52X 114.2(12) . . ? C48 C51 C52X 108.8(8) . . ? C54X C51 C52X 101.9(13) . . ? C57 C55 C50 116.3(3) . . ? C57 C56 O6 118.1(3) . . ? C57 C56 C61 121.9(3) . . ? O6 C56 C61 120.0(3) . . ? C56 C57 C58 117.7(3) . . ? C56 C57 C55 121.5(3) . . ? C58 C57 C55 120.7(3) . . ? C59 C58 C57 123.0(4) . . ? C58 C59 C60 116.9(3) . . ? C58 C59 C62 121.9(3) . . ? C60 C59 C62 121.1(3) . . ? C61 C60 C59 122.8(3) . . ? C60 C61 C56 117.7(3) . . ? C60 C61 C66 120.9(3) . . ? C56 C61 C66 121.3(3) . . ? C65X C62 C64X 114.4(10) . . ? C63 C62 C65 108.9(7) . . ? C63 C62 C59 114.8(4) . . ? C65X C62 C59 112.1(6) . . ? C64X C62 C59 106.1(6) . . ? C65 C62 C59 110.1(4) . . ? C65X C62 C63X 109.0(9) . . ? C64X C62 C63X 109.2(9) . . ? C59 C62 C63X 105.8(6) . . ? C63 C62 C64 107.7(6) . . ? C65 C62 C64 105.8(5) . . ? C59 C62 C64 109.1(4) . . ? C2 C66 C61 112.3(3) . . ? N1 C67 C68 179.7(6) . . ? N2 C69 C70 178.8(18) . . ? N2X C69X C70X 175(3) . . ? 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 O1 C1 C2 C3 178.7(3) . . . . ? C6 C1 C2 C3 -0.8(5) . . . . ? O1 C1 C2 C66 2.3(5) . . . . ? C6 C1 C2 C66 -177.2(3) . . . . ? C1 C2 C3 C4 0.4(5) . . . . ? C66 C2 C3 C4 176.9(3) . . . . ? C2 C3 C4 C5 1.0(5) . . . . ? C2 C3 C4 C7 -178.1(3) . . . . ? C3 C4 C5 C6 -2.2(5) . . . . ? C7 C4 C5 C6 177.0(3) . . . . ? C4 C5 C6 C1 1.9(5) . . . . ? C4 C5 C6 C11 -173.1(3) . . . . ? C2 C1 C6 C5 -0.3(5) . . . . ? O1 C1 C6 C5 -179.8(3) . . . . ? C2 C1 C6 C11 174.4(3) . . . . ? O1 C1 C6 C11 -5.1(5) . . . . ? C3 C4 C7 C10 6.6(5) . . . . ? C5 C4 C7 C10 -172.5(3) . . . . ? C3 C4 C7 C9 -113.9(4) . . . . ? C5 C4 C7 C9 67.0(4) . . . . ? C3 C4 C7 C8 126.8(4) . . . . ? C5 C4 C7 C8 -52.3(4) . . . . ? C5 C6 C11 C13 82.6(4) . . . . ? C1 C6 C11 C13 -92.1(4) . . . . ? O2 C12 C13 C14 179.7(3) . . . . ? C17 C12 C13 C14 2.2(5) . . . . ? O2 C12 C13 C11 5.1(5) . . . . ? C17 C12 C13 C11 -172.4(3) . . . . ? C6 C11 C13 C12 84.3(4) . . . . ? C6 C11 C13 C14 -90.1(4) . . . . ? C12 C13 C14 C15 -1.4(5) . . . . ? C11 C13 C14 C15 173.3(3) . . . . ? C13 C14 C15 C16 0.1(6) . . . . ? C13 C14 C15 C18 -177.5(4) . . . . ? C14 C15 C16 C17 0.5(6) . . . . ? C18 C15 C16 C17 178.0(4) . . . . ? O2 C12 C17 C16 -179.1(3) . . . . ? C13 C12 C17 C16 -1.7(5) . . . . ? O2 C12 C17 C22 -4.4(5) . . . . ? C13 C12 C17 C22 173.0(3) . . . . ? C15 C16 C17 C12 0.3(5) . . . . ? C15 C16 C17 C22 -174.5(3) . . . . ? C16 C15 C18 C20X -63.1(10) . . . . ? C14 C15 C18 C20X 114.3(10) . . . . ? C16 C15 C18 C19X 158.7(15) . . . . ? C14 C15 C18 C19X -23.9(15) . . . . ? C16 C15 C18 C21 -8.8(7) . . . . ? C14 C15 C18 C21 168.6(6) . . . . ? C16 C15 C18 C19 122.3(5) . . . . ? C14 C15 C18 C19 -60.3(6) . . . . ? C16 C15 C18 C20 -123.2(5) . . . . ? C14 C15 C18 C20 54.2(5) . . . . ? C16 C15 C18 C21X 47.6(9) . . . . ? C14 C15 C18 C21X -135.0(8) . . . . ? C12 C17 C22 C24 84.8(4) . . . . ? C16 C17 C22 C24 -100.6(4) . . . . ? O3 C23 C24 C25 -177.0(3) . . . . ? C28 C23 C24 C25 4.6(5) . . . . ? O3 C23 C24 C22 7.6(5) . . . . ? C28 C23 C24 C22 -170.9(3) . . . . ? C17 C22 C24 C23 -95.7(4) . . . . ? C17 C22 C24 C25 88.9(4) . . . . ? C23 C24 C25 C26 -2.6(5) . . . . ? C22 C24 C25 C26 172.9(3) . . . . ? C24 C25 C26 C27 -0.5(5) . . . . ? C24 C25 C26 C29 -177.6(3) . . . . ? C25 C26 C27 C28 1.8(6) . . . . ? C29 C26 C27 C28 179.0(3) . . . . ? C26 C27 C28 C23 0.1(6) . . . . ? C26 C27 C28 C33 -174.5(3) . . . . ? O3 C23 C28 C27 178.2(3) . . . . ? C24 C23 C28 C27 -3.4(6) . . . . ? O3 C23 C28 C33 -7.1(5) . . . . ? C24 C23 C28 C33 171.3(3) . . . . ? C25 C26 C29 C32 107.2(4) . . . . ? C27 C26 C29 C32 -69.8(5) . . . . ? C25 C26 C29 C30 -13.2(5) . . . . ? C27 C26 C29 C30 169.8(4) . . . . ? C25 C26 C29 C31 -133.5(4) . . . . ? C27 C26 C29 C31 49.4(5) . . . . ? C27 C28 C33 C35 98.5(4) . . . . ? C23 C28 C33 C35 -76.0(4) . . . . ? C39 C34 C35 C36 -0.7(5) . . . . ? O4 C34 C35 C36 179.4(3) . . . . ? C39 C34 C35 C33 -177.4(3) . . . . ? O4 C34 C35 C33 2.7(5) . . . . ? C28 C33 C35 C34 96.5(4) . . . . ? C28 C33 C35 C36 -80.2(4) . . . . ? C34 C35 C36 C37 -0.7(6) . . . . ? C33 C35 C36 C37 176.1(3) . . . . ? C35 C36 C37 C38 1.9(6) . . . . ? C35 C36 C37 C40 -177.5(4) . . . . ? C36 C37 C38 C39 -1.8(6) . . . . ? C40 C37 C38 C39 177.6(4) . . . . ? C37 C38 C39 C34 0.5(5) . . . . ? C37 C38 C39 C44 -176.9(3) . . . . ? C35 C34 C39 C38 0.8(5) . . . . ? O4 C34 C39 C38 -179.3(3) . . . . ? C35 C34 C39 C44 178.1(3) . . . . ? O4 C34 C39 C44 -2.0(5) . . . . ? C38 C37 C40 C42 -65.9(8) . . . . ? C36 C37 C40 C42 113.4(8) . . . . ? C38 C37 C40 C41X 119.2(13) . . . . ? C36 C37 C40 C41X -61.5(13) . . . . ? C38 C37 C40 C42X -121.3(12) . . . . ? C36 C37 C40 C42X 58.0(13) . . . . ? C38 C37 C40 C41 172.6(10) . . . . ? C36 C37 C40 C41 -8.1(11) . . . . ? C38 C37 C40 C43 51.6(7) . . . . ? C36 C37 C40 C43 -129.1(7) . . . . ? C38 C37 C40 C43X -4.0(11) . . . . ? C36 C37 C40 C43X 175.3(10) . . . . ? C38 C39 C44 C46 78.7(4) . . . . ? C34 C39 C44 C46 -98.5(4) . . . . ? O5 C45 C46 C47 -179.2(3) . . . . ? C50 C45 C46 C47 2.2(5) . . . . ? O5 C45 C46 C44 4.4(5) . . . . ? C50 C45 C46 C44 -174.3(3) . . . . ? C39 C44 C46 C47 -101.7(4) . . . . ? C39 C44 C46 C45 74.6(4) . . . . ? C45 C46 C47 C48 -0.1(5) . . . . ? C44 C46 C47 C48 176.4(3) . . . . ? C46 C47 C48 C49 -1.4(5) . . . . ? C46 C47 C48 C51 -178.7(3) . . . . ? C47 C48 C49 C50 0.9(5) . . . . ? C51 C48 C49 C50 178.1(3) . . . . ? C48 C49 C50 C45 1.1(5) . . . . ? C48 C49 C50 C55 -175.4(3) . . . . ? O5 C45 C50 C49 178.7(3) . . . . ? C46 C45 C50 C49 -2.7(5) . . . . ? O5 C45 C50 C55 -4.8(5) . . . . ? C46 C45 C50 C55 173.8(3) . . . . ? C49 C48 C51 C53X -44.6(13) . . . . ? C47 C48 C51 C53X 132.5(13) . . . . ? C49 C48 C51 C54 137.8(5) . . . . ? C47 C48 C51 C54 -45.2(6) . . . . ? C49 C48 C51 C53 14.7(5) . . . . ? C47 C48 C51 C53 -168.2(4) . . . . ? C49 C48 C51 C52 -102.5(5) . . . . ? C47 C48 C51 C52 74.6(5) . . . . ? C49 C48 C51 C54X 80.4(11) . . . . ? C47 C48 C51 C54X -102.5(11) . . . . ? C49 C48 C51 C52X -172.1(11) . . . . ? C47 C48 C51 C52X 5.0(12) . . . . ? C49 C50 C55 C57 -89.9(4) . . . . ? C45 C50 C55 C57 93.7(4) . . . . ? O6 C56 C57 C58 179.9(3) . . . . ? C61 C56 C57 C58 1.2(5) . . . . ? O6 C56 C57 C55 3.0(5) . . . . ? C61 C56 C57 C55 -175.8(3) . . . . ? C50 C55 C57 C56 -89.7(4) . . . . ? C50 C55 C57 C58 93.4(4) . . . . ? C56 C57 C58 C59 -0.6(5) . . . . ? C55 C57 C58 C59 176.4(3) . . . . ? C57 C58 C59 C60 -0.1(5) . . . . ? C57 C58 C59 C62 -179.0(3) . . . . ? C58 C59 C60 C61 0.3(5) . . . . ? C62 C59 C60 C61 179.1(3) . . . . ? C59 C60 C61 C56 0.3(5) . . . . ? C59 C60 C61 C66 -176.5(3) . . . . ? C57 C56 C61 C60 -1.0(5) . . . . ? O6 C56 C61 C60 -179.8(3) . . . . ? C57 C56 C61 C66 175.8(3) . . . . ? O6 C56 C61 C66 -3.0(5) . . . . ? C58 C59 C62 C63 5.5(8) . . . . ? C60 C59 C62 C63 -173.3(7) . . . . ? C58 C59 C62 C65X 176.3(10) . . . . ? C60 C59 C62 C65X -2.5(11) . . . . ? C58 C59 C62 C64X -58.2(9) . . . . ? C60 C59 C62 C64X 123.0(9) . . . . ? C58 C59 C62 C65 128.8(6) . . . . ? C60 C59 C62 C65 -50.0(7) . . . . ? C58 C59 C62 C63X 57.7(8) . . . . ? C60 C59 C62 C63X -121.1(8) . . . . ? C58 C59 C62 C64 -115.5(5) . . . . ? C60 C59 C62 C64 65.7(6) . . . . ? C3 C2 C66 C61 -79.4(4) . . . . ? C1 C2 C66 C61 97.0(4) . . . . ? C60 C61 C66 C2 97.0(4) . . . . ? C56 C61 C66 C2 -79.7(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O2 0.84 1.81 2.640(3) 168.1 . O2 H2 O3 0.84 1.80 2.627(3) 166.9 . O3 H3 O4 0.84 1.84 2.631(4) 156.2 . O4 H4 O5 0.84 1.84 2.646(3) 160.4 . O5 H5 O6 0.84 1.82 2.650(3) 172.6 . O6 H6 O1 0.84 1.91 2.667(3) 148.7 . _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.304 _refine_diff_density_min -0.244 _refine_diff_density_rms 0.048 #===END data_3 _database_code_CSD 215819 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C96 H124 N4 O8' _chemical_formula_weight 1461.99 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 38.419(2) _cell_length_b 21.8067(14) _cell_length_c 21.1486(13) _cell_angle_alpha 90.00 _cell_angle_beta 92.251(2) _cell_angle_gamma 90.00 _cell_volume 17704.7(19) _cell_formula_units_Z 8 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7547 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 26.47 _exptl_crystal_description 'octahedral prism' _exptl_crystal_colour orange _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.097 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 6336 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.984 _exptl_absorpt_correction_T_max 0.988 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 63586 _diffrn_reflns_av_R_equivalents 0.0847 _diffrn_reflns_av_sigmaI/netI 0.0968 _diffrn_reflns_limit_h_min -45 _diffrn_reflns_limit_h_max 45 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.85 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15584 _reflns_number_gt 7431 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0707P)^2^+66.3018P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00055(6) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 15584 _refine_ls_number_parameters 1063 _refine_ls_number_restraints 283 _refine_ls_R_factor_all 0.1669 _refine_ls_R_factor_gt 0.0694 _refine_ls_wR_factor_ref 0.2365 _refine_ls_wR_factor_gt 0.1635 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.045 _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 O1 O 0.29604(7) 0.01950(14) 0.50090(15) 0.0439(8) Uani 1 1 d . . . H1 H 0.2767 0.0078 0.4856 0.066 Uiso 1 1 calc R . . O2 O 0.31109(7) 0.13080(13) 0.54994(16) 0.0446(8) Uani 1 1 d D . . H2 H 0.3035 0.0987 0.5323 0.067 Uiso 1 1 calc R . . O3 O 0.27908(7) 0.23023(14) 0.59001(15) 0.0434(8) Uani 1 1 d . . . H3 H 0.2900 0.1995 0.5772 0.065 Uiso 1 1 calc RD . . O4 O 0.21438(7) 0.26469(14) 0.59653(17) 0.0473(8) Uani 1 1 d . . . H4 H 0.2356 0.2590 0.5907 0.071 Uiso 1 1 calc R . . O5 O 0.15662(7) 0.22440(14) 0.54127(16) 0.0465(8) Uani 1 1 d D . . H5 H 0.1743 0.2391 0.5603 0.070 Uiso 1 1 calc R . . O6 O 0.13526(7) 0.11991(14) 0.48538(16) 0.0456(8) Uani 1 1 d . . . H6 H 0.1410 0.1547 0.4992 0.068 Uiso 1 1 calc RD . . O7 O 0.16747(7) 0.01813(14) 0.43879(16) 0.0452(8) Uani 1 1 d . . . H7 H 0.1566 0.0484 0.4525 0.068 Uiso 1 1 calc R . . O8 O 0.23461(8) -0.02727(14) 0.44848(17) 0.0479(8) Uani 1 1 d . . . H8 H 0.2140 -0.0144 0.4463 0.072 Uiso 1 1 calc R . . C1 C 0.32192(10) -0.01913(19) 0.4808(2) 0.0326(10) Uani 1 1 d . . . C2 C 0.31712(10) -0.0820(2) 0.4804(2) 0.0352(10) Uani 1 1 d . . . C3 C 0.34363(11) -0.1191(2) 0.4589(2) 0.0363(10) Uani 1 1 d . . . H3A H 0.3402 -0.1622 0.4580 0.044 Uiso 1 1 calc R . . C4 C 0.37492(11) -0.0957(2) 0.4386(2) 0.0374(11) Uani 1 1 d . . . C5 C 0.37899(11) -0.03220(19) 0.4419(2) 0.0352(10) Uani 1 1 d . . . H5A H 0.4003 -0.0149 0.4294 0.042 Uiso 1 1 calc R . . C6 C 0.35330(11) 0.00675(19) 0.4627(2) 0.0356(10) Uani 1 1 d . . . C7 C 0.40284(12) -0.1385(2) 0.4136(2) 0.0448(12) Uani 1 1 d . . . C8 C 0.38893(15) -0.1656(3) 0.3513(3) 0.085(2) Uani 1 1 d . . . H8A H 0.3685 -0.1910 0.3590 0.127 Uiso 1 1 calc R . . H8B H 0.4070 -0.1909 0.3329 0.127 Uiso 1 1 calc R . . H8C H 0.3823 -0.1324 0.3220 0.127 Uiso 1 1 calc R . . C9 C 0.41065(17) -0.1905(3) 0.4609(4) 0.091(2) Uani 1 1 d . . . H9A H 0.4194 -0.1731 0.5012 0.136 Uiso 1 1 calc R . . H9B H 0.4283 -0.2178 0.4441 0.136 Uiso 1 1 calc R . . H9C H 0.3893 -0.2137 0.4676 0.136 Uiso 1 1 calc R . . C10 C 0.43674(14) -0.1055(3) 0.4027(4) 0.084(2) Uani 1 1 d . . . H10A H 0.4328 -0.0735 0.3706 0.126 Uiso 1 1 calc R . . H10B H 0.4540 -0.1349 0.3880 0.126 Uiso 1 1 calc R . . H10C H 0.4454 -0.0867 0.4423 0.126 Uiso 1 1 calc R . . C11 C 0.35991(11) 0.07480(19) 0.4676(2) 0.0357(10) Uani 1 1 d . . . H11A H 0.3792 0.0860 0.4402 0.043 Uiso 1 1 calc R . . H11B H 0.3388 0.0973 0.4523 0.043 Uiso 1 1 calc R . . C12 C 0.34482(10) 0.12081(19) 0.5734(2) 0.0336(10) Uani 1 1 d . . . C13 C 0.36907(11) 0.09348(19) 0.5347(2) 0.0338(10) Uani 1 1 d . . . C14 C 0.40257(11) 0.08301(19) 0.5609(2) 0.0359(10) Uani 1 1 d . . . H14 H 0.4194 0.0646 0.5352 0.043 Uiso 1 1 calc R . . C15 C 0.41236(11) 0.09828(19) 0.6225(2) 0.0357(10) Uani 1 1 d . . . C16 C 0.38731(11) 0.12676(19) 0.6586(2) 0.0370(11) Uani 1 1 d . . . H16 H 0.3936 0.1388 0.7006 0.044 Uiso 1 1 calc R . . C17 C 0.35357(11) 0.13817(19) 0.6354(2) 0.0349(10) Uani 1 1 d . . . C18 C 0.44870(11) 0.0865(2) 0.6518(2) 0.0443(12) Uani 1 1 d . . . C19 C 0.46696(13) 0.1478(2) 0.6648(3) 0.0640(16) Uani 1 1 d . . . H19A H 0.4701 0.1693 0.6247 0.096 Uiso 1 1 calc R . . H19B H 0.4897 0.1405 0.6859 0.096 Uiso 1 1 calc R . . H19C H 0.4527 0.1730 0.6921 0.096 Uiso 1 1 calc R . . C20 C 0.44577(13) 0.0511(3) 0.7140(3) 0.0666(16) Uani 1 1 d . . . H20A H 0.4325 0.0755 0.7436 0.100 Uiso 1 1 calc R . . H20B H 0.4691 0.0432 0.7324 0.100 Uiso 1 1 calc R . . H20C H 0.4338 0.0120 0.7057 0.100 Uiso 1 1 calc R . . C21 C 0.47128(12) 0.0485(3) 0.6082(3) 0.0613(15) Uani 1 1 d . . . H21A H 0.4597 0.0093 0.5987 0.092 Uiso 1 1 calc R . . H21B H 0.4940 0.0408 0.6294 0.092 Uiso 1 1 calc R . . H21C H 0.4745 0.0711 0.5688 0.092 Uiso 1 1 calc R . . C22 C 0.32752(11) 0.16783(19) 0.6769(2) 0.0375(11) Uani 1 1 d . . . H22A H 0.3338 0.1578 0.7216 0.045 Uiso 1 1 calc R . . H22B H 0.3043 0.1499 0.6669 0.045 Uiso 1 1 calc R . . C23 C 0.30092(10) 0.26500(19) 0.6293(2) 0.0329(10) Uani 1 1 d . . . C24 C 0.32502(10) 0.23693(19) 0.6704(2) 0.0336(10) Uani 1 1 d . . . C25 C 0.34644(11) 0.27421(19) 0.7091(2) 0.0359(10) Uani 1 1 d . . . H25 H 0.3635 0.2553 0.7364 0.043 Uiso 1 1 calc R . . C26 C 0.34390(11) 0.3378(2) 0.7092(2) 0.0364(10) Uani 1 1 d . . . C27 C 0.31847(11) 0.3634(2) 0.6682(2) 0.0371(10) Uani 1 1 d . . . H27 H 0.3160 0.4067 0.6675 0.044 Uiso 1 1 calc R . . C28 C 0.29664(10) 0.32866(19) 0.6284(2) 0.0338(10) Uani 1 1 d . . . C29 C 0.36727(12) 0.3785(2) 0.7520(2) 0.0415(11) Uani 1 1 d . . . C30 C 0.34630(18) 0.4302(3) 0.7798(3) 0.091(2) Uani 1 1 d . . . H30A H 0.3255 0.4133 0.7987 0.136 Uiso 1 1 calc R . . H30B H 0.3393 0.4592 0.7463 0.136 Uiso 1 1 calc R . . H30C H 0.3605 0.4514 0.8125 0.136 Uiso 1 1 calc R . . C31 C 0.38276(18) 0.3437(3) 0.8077(3) 0.088(2) Uani 1 1 d . . . H31A H 0.3642 0.3224 0.8294 0.132 Uiso 1 1 calc R . . H31B H 0.3945 0.3725 0.8371 0.132 Uiso 1 1 calc R . . H31C H 0.3996 0.3138 0.7930 0.132 Uiso 1 1 calc R . . C32 C 0.39525(19) 0.4063(4) 0.7128(3) 0.115(3) Uani 1 1 d . . . H32A H 0.4086 0.4362 0.7384 0.172 Uiso 1 1 calc R . . H32B H 0.3844 0.4268 0.6758 0.172 Uiso 1 1 calc R . . H32C H 0.4108 0.3739 0.6988 0.172 Uiso 1 1 calc R . . C33 C 0.26781(10) 0.3589(2) 0.5890(2) 0.0348(10) Uani 1 1 d . . . H33A H 0.2628 0.3340 0.5506 0.042 Uiso 1 1 calc R . . H33B H 0.2757 0.3998 0.5753 0.042 Uiso 1 1 calc R . . C34 C 0.21009(10) 0.31955(19) 0.6283(2) 0.0341(10) Uani 1 1 d . . . C35 C 0.23464(10) 0.36612(19) 0.6248(2) 0.0334(10) Uani 1 1 d . . . C36 C 0.22844(11) 0.42011(19) 0.6583(2) 0.0351(10) Uani 1 1 d . . . H36 H 0.2449 0.4525 0.6562 0.042 Uiso 1 1 calc R . . C37 C 0.19936(11) 0.42865(19) 0.6946(2) 0.0360(10) Uani 1 1 d . A . C38 C 0.17561(11) 0.38055(19) 0.6960(2) 0.0358(10) Uani 1 1 d . . . H38 H 0.1553 0.3852 0.7198 0.043 Uiso 1 1 calc R . . C39 C 0.18064(10) 0.32582(19) 0.6637(2) 0.0340(10) Uani 1 1 d . . . C40 C 0.19410(11) 0.4880(2) 0.7323(2) 0.0429(11) Uani 1 1 d DU . . C41 C 0.2043(3) 0.4770(4) 0.8007(4) 0.088(4) Uani 0.683(11) 1 d PDU A 1 H41A H 0.2010 0.5148 0.8249 0.132 Uiso 0.683(11) 1 calc PR A 1 H41B H 0.2289 0.4647 0.8044 0.132 Uiso 0.683(11) 1 calc PR A 1 H41C H 0.1898 0.4444 0.8175 0.132 Uiso 0.683(11) 1 calc PR A 1 C42 C 0.2120(4) 0.5424(4) 0.7053(7) 0.112(5) Uani 0.683(11) 1 d PDU A 1 H42A H 0.2051 0.5466 0.6604 0.169 Uiso 0.683(11) 1 calc PR A 1 H42B H 0.2373 0.5367 0.7097 0.169 Uiso 0.683(11) 1 calc PR A 1 H42C H 0.2053 0.5794 0.7281 0.169 Uiso 0.683(11) 1 calc PR A 1 C43 C 0.15428(18) 0.5041(4) 0.7314(5) 0.063(3) Uani 0.683(11) 1 d PDU A 1 H43A H 0.1461 0.5132 0.6879 0.095 Uiso 0.683(11) 1 calc PR A 1 H43B H 0.1506 0.5400 0.7582 0.095 Uiso 0.683(11) 1 calc PR A 1 H43C H 0.1412 0.4692 0.7474 0.095 Uiso 0.683(11) 1 calc PR A 1 C41X C 0.2286(4) 0.4938(8) 0.7764(8) 0.052(5) Uiso 0.317(11) 1 d PDU A 2 H41D H 0.2491 0.4928 0.7501 0.078 Uiso 0.317(11) 1 calc PR A 2 H41E H 0.2298 0.4596 0.8064 0.078 Uiso 0.317(11) 1 calc PR A 2 H41F H 0.2282 0.5327 0.7997 0.078 Uiso 0.317(11) 1 calc PR A 2 C42X C 0.1957(4) 0.5420(8) 0.6884(8) 0.043(5) Uiso 0.317(11) 1 d PDU A 2 H42D H 0.2178 0.5412 0.6667 0.065 Uiso 0.317(11) 1 calc PR A 2 H42E H 0.1942 0.5800 0.7128 0.065 Uiso 0.317(11) 1 calc PR A 2 H42F H 0.1763 0.5399 0.6571 0.065 Uiso 0.317(11) 1 calc PR A 2 C43X C 0.1648(4) 0.4858(8) 0.7751(8) 0.057(5) Uiso 0.317(11) 1 d PDU A 2 H43D H 0.1634 0.5248 0.7979 0.086 Uiso 0.317(11) 1 calc PR A 2 H43E H 0.1685 0.4523 0.8055 0.086 Uiso 0.317(11) 1 calc PR A 2 H43F H 0.1431 0.4789 0.7503 0.086 Uiso 0.317(11) 1 calc PR A 2 C44 C 0.15412(11) 0.27453(19) 0.6689(2) 0.0377(11) Uani 1 1 d . . . H44A H 0.1660 0.2346 0.6640 0.045 Uiso 1 1 calc R . . H44B H 0.1444 0.2756 0.7116 0.045 Uiso 1 1 calc R . . C45 C 0.12727(10) 0.25637(19) 0.5587(2) 0.0354(10) Uani 1 1 d . . . C46 C 0.12456(11) 0.27956(19) 0.6196(2) 0.0354(10) Uani 1 1 d . . . C47 C 0.09386(10) 0.30890(19) 0.6349(2) 0.0364(10) Uani 1 1 d . . . H47 H 0.0918 0.3248 0.6764 0.044 Uiso 1 1 calc R . . C48 C 0.06583(11) 0.3157(2) 0.5908(2) 0.0388(11) Uani 1 1 d . . . C49 C 0.06987(10) 0.29275(19) 0.5307(2) 0.0370(11) Uani 1 1 d . . . H49 H 0.0514 0.2974 0.4999 0.044 Uiso 1 1 calc R . . C50 C 0.10039(11) 0.26295(19) 0.5135(2) 0.0365(10) Uani 1 1 d . . . C51 C 0.03267(11) 0.3477(2) 0.6114(2) 0.0430(12) Uani 1 1 d . . . C52 C 0.01925(13) 0.3162(3) 0.6700(3) 0.0610(15) Uani 1 1 d . . . H52A H 0.0149 0.2728 0.6608 0.091 Uiso 1 1 calc R . . H52B H -0.0024 0.3358 0.6821 0.091 Uiso 1 1 calc R . . H52C H 0.0367 0.3197 0.7049 0.091 Uiso 1 1 calc R . . C53 C 0.00346(13) 0.3451(3) 0.5598(3) 0.0654(16) Uani 1 1 d . . . H53A H 0.0108 0.3672 0.5222 0.098 Uiso 1 1 calc R . . H53B H -0.0176 0.3642 0.5755 0.098 Uiso 1 1 calc R . . H53C H -0.0015 0.3022 0.5487 0.098 Uiso 1 1 calc R . . C54 C 0.04076(14) 0.4146(2) 0.6272(3) 0.0721(18) Uani 1 1 d . . . H54A H 0.0601 0.4166 0.6587 0.108 Uiso 1 1 calc R . . H54B H 0.0201 0.4341 0.6441 0.108 Uiso 1 1 calc R . . H54C H 0.0473 0.4361 0.5887 0.108 Uiso 1 1 calc R . . C55 C 0.10315(12) 0.2362(2) 0.4477(2) 0.0410(11) Uani 1 1 d . . . H55A H 0.0926 0.2649 0.4162 0.049 Uiso 1 1 calc R . . H55B H 0.1280 0.2309 0.4382 0.049 Uiso 1 1 calc R . . C56 C 0.10055(11) 0.1210(2) 0.4641(2) 0.0377(11) Uani 1 1 d . . . C57 C 0.08486(11) 0.1752(2) 0.4430(2) 0.0395(11) Uani 1 1 d . . . C58 C 0.05038(12) 0.1722(2) 0.4203(2) 0.0452(12) Uani 1 1 d . . . H58 H 0.0395 0.2088 0.4052 0.054 Uiso 1 1 calc R . . C59 C 0.03126(12) 0.1184(2) 0.4188(2) 0.0477(12) Uani 1 1 d . B . C60 C 0.04777(11) 0.0658(2) 0.4423(2) 0.0454(12) Uani 1 1 d . . . H60 H 0.0351 0.0283 0.4424 0.054 Uiso 1 1 calc R . . C61 C 0.08213(11) 0.0662(2) 0.4655(2) 0.0394(11) Uani 1 1 d . . . C62 C -0.00655(13) 0.1169(3) 0.3925(3) 0.0616(14) Uani 1 1 d DU . . C63 C -0.0291(4) 0.1475(9) 0.4416(8) 0.085(5) Uani 0.54(2) 1 d PDU B 1 H63A H -0.0259 0.1263 0.4823 0.127 Uiso 0.54(2) 1 calc PR B 1 H63B H -0.0537 0.1453 0.4274 0.127 Uiso 0.54(2) 1 calc PR B 1 H63C H -0.0222 0.1905 0.4467 0.127 Uiso 0.54(2) 1 calc PR B 1 C64 C -0.0093(4) 0.1455(12) 0.3297(7) 0.111(7) Uani 0.54(2) 1 d PDU B 1 H64A H -0.0336 0.1443 0.3137 0.166 Uiso 0.54(2) 1 calc PR B 1 H64B H 0.0054 0.1232 0.3006 0.166 Uiso 0.54(2) 1 calc PR B 1 H64C H -0.0015 0.1883 0.3327 0.166 Uiso 0.54(2) 1 calc PR B 1 C65 C -0.0210(3) 0.0488(5) 0.3882(11) 0.088(5) Uani 0.54(2) 1 d PDU B 1 H65A H -0.0191 0.0296 0.4301 0.132 Uiso 0.54(2) 1 calc PR B 1 H65B H -0.0073 0.0252 0.3585 0.132 Uiso 0.54(2) 1 calc PR B 1 H65C H -0.0454 0.0494 0.3732 0.132 Uiso 0.54(2) 1 calc PR B 1 C63X C -0.0303(5) 0.1082(13) 0.4462(9) 0.101(7) Uani 0.46(2) 1 d PDU B 2 H63D H -0.0545 0.1074 0.4298 0.151 Uiso 0.46(2) 1 calc PR B 2 H63E H -0.0272 0.1421 0.4763 0.151 Uiso 0.46(2) 1 calc PR B 2 H63F H -0.0248 0.0694 0.4676 0.151 Uiso 0.46(2) 1 calc PR B 2 C64X C -0.0168(4) 0.1792(7) 0.3600(11) 0.080(5) Uani 0.46(2) 1 d PDU B 2 H64D H -0.0022 0.1859 0.3236 0.120 Uiso 0.46(2) 1 calc PR B 2 H64E H -0.0131 0.2128 0.3904 0.120 Uiso 0.46(2) 1 calc PR B 2 H64F H -0.0413 0.1780 0.3458 0.120 Uiso 0.46(2) 1 calc PR B 2 C65X C -0.0098(5) 0.0684(11) 0.3391(12) 0.114(9) Uani 0.46(2) 1 d PDU B 2 H65D H 0.0072 0.0773 0.3070 0.170 Uiso 0.46(2) 1 calc PR B 2 H65E H -0.0334 0.0696 0.3197 0.170 Uiso 0.46(2) 1 calc PR B 2 H65F H -0.0052 0.0275 0.3569 0.170 Uiso 0.46(2) 1 calc PR B 2 C66 C 0.09866(12) 0.0076(2) 0.4903(2) 0.0420(11) Uani 1 1 d . . . H66A H 0.0814 -0.0156 0.5144 0.050 Uiso 1 1 calc R . . H66B H 0.1185 0.0178 0.5196 0.050 Uiso 1 1 calc R . . C67 C 0.14393(11) -0.02431(19) 0.4129(2) 0.0361(10) Uani 1 1 d . . . C68 C 0.11136(11) -0.0322(2) 0.4374(2) 0.0382(11) Uani 1 1 d . . . C69 C 0.08967(12) -0.0773(2) 0.4106(2) 0.0450(12) Uani 1 1 d . . . H69 H 0.0672 -0.0828 0.4271 0.054 Uiso 1 1 calc R . . C70 C 0.09937(11) -0.1143(2) 0.3609(2) 0.0428(11) Uani 1 1 d . . . C71 C 0.13207(11) -0.1041(2) 0.3373(2) 0.0410(11) Uani 1 1 d . . . H71 H 0.1394 -0.1283 0.3029 0.049 Uiso 1 1 calc R . . C72 C 0.15474(11) -0.0591(2) 0.3627(2) 0.0364(10) Uani 1 1 d . . . C73 C 0.07483(13) -0.1641(3) 0.3347(3) 0.0594(15) Uani 1 1 d . . . C74 C 0.0654(2) -0.2072(3) 0.3883(4) 0.106(3) Uani 1 1 d . . . H74A H 0.0504 -0.1856 0.4174 0.159 Uiso 1 1 calc R . . H74B H 0.0867 -0.2207 0.4112 0.159 Uiso 1 1 calc R . . H74C H 0.0530 -0.2429 0.3706 0.159 Uiso 1 1 calc R . . C75 C 0.09143(15) -0.2021(3) 0.2831(3) 0.0783(19) Uani 1 1 d . . . H75A H 0.0753 -0.2347 0.2691 0.117 Uiso 1 1 calc R . . H75B H 0.1131 -0.2205 0.3001 0.117 Uiso 1 1 calc R . . H75C H 0.0965 -0.1756 0.2472 0.117 Uiso 1 1 calc R . . C76 C 0.04229(16) -0.1336(4) 0.3054(4) 0.116(3) Uani 1 1 d . . . H76A H 0.0491 -0.1033 0.2740 0.175 Uiso 1 1 calc R . . H76B H 0.0295 -0.1132 0.3386 0.175 Uiso 1 1 calc R . . H76C H 0.0274 -0.1648 0.2848 0.175 Uiso 1 1 calc R . . C77 C 0.19058(11) -0.0533(2) 0.3367(2) 0.0401(11) Uani 1 1 d . . . H77A H 0.1891 -0.0602 0.2904 0.048 Uiso 1 1 calc R . . H77B H 0.1994 -0.0112 0.3443 0.048 Uiso 1 1 calc R . . C78 C 0.23609(10) -0.0854(2) 0.4209(2) 0.0368(11) Uani 1 1 d . . . C79 C 0.21579(11) -0.0986(2) 0.3668(2) 0.0371(11) Uani 1 1 d . . . C80 C 0.21876(11) -0.1568(2) 0.3409(2) 0.0385(11) Uani 1 1 d . . . H80 H 0.2052 -0.1663 0.3037 0.046 Uiso 1 1 calc R . . C81 C 0.24065(11) -0.2020(2) 0.3667(2) 0.0373(10) Uani 1 1 d . . . C82 C 0.26083(11) -0.1857(2) 0.4198(2) 0.0363(10) Uani 1 1 d . . . H82 H 0.2764 -0.2152 0.4381 0.044 Uiso 1 1 calc R . . C83 C 0.25930(11) -0.1277(2) 0.4475(2) 0.0360(10) Uani 1 1 d . . . C84 C 0.24181(12) -0.2651(2) 0.3353(2) 0.0440(12) Uani 1 1 d . . . C85 C 0.25267(16) -0.2584(3) 0.2667(2) 0.0651(16) Uani 1 1 d . . . H85A H 0.2358 -0.2325 0.2434 0.098 Uiso 1 1 calc R . . H85B H 0.2534 -0.2989 0.2469 0.098 Uiso 1 1 calc R . . H85C H 0.2758 -0.2394 0.2662 0.098 Uiso 1 1 calc R . . C86 C 0.26774(13) -0.3078(2) 0.3699(3) 0.0584(14) Uani 1 1 d . . . H86A H 0.2913 -0.2912 0.3671 0.088 Uiso 1 1 calc R . . H86B H 0.2667 -0.3485 0.3502 0.088 Uiso 1 1 calc R . . H86C H 0.2618 -0.3111 0.4144 0.088 Uiso 1 1 calc R . . C87 C 0.20548(13) -0.2941(2) 0.3355(3) 0.0586(14) Uani 1 1 d . . . H87A H 0.1986 -0.2998 0.3793 0.088 Uiso 1 1 calc R . . H87B H 0.2059 -0.3339 0.3141 0.088 Uiso 1 1 calc R . . H87C H 0.1887 -0.2671 0.3133 0.088 Uiso 1 1 calc R . . C88 C 0.28372(11) -0.1115(2) 0.5027(2) 0.0385(11) Uani 1 1 d . . . H88A H 0.2896 -0.1491 0.5271 0.046 Uiso 1 1 calc R . . H88B H 0.2719 -0.0828 0.5311 0.046 Uiso 1 1 calc R . . N1 N 0.3329(4) -0.2945(9) 0.5130(8) 0.334(11) Uani 1 1 d DU . . C89 C 0.3353(9) -0.3410(11) 0.4919(18) 0.412(15) Uani 1 1 d DU . . C90 C 0.3251(4) -0.3967(8) 0.4607(6) 0.321(12) Uani 1 1 d DU . . H90A H 0.3018 -0.3916 0.4405 0.482 Uiso 1 1 calc R . . H90B H 0.3245 -0.4301 0.4917 0.482 Uiso 1 1 calc R . . H90C H 0.3418 -0.4067 0.4285 0.482 Uiso 1 1 calc R . . N2 N 0.1063(5) 0.0777(8) 0.6456(5) 0.283(10) Uani 0.825(7) 1 d PDU C 1 C91 C 0.0834(3) 0.1072(5) 0.6292(5) 0.134(5) Uani 0.825(7) 1 d PDU C 1 C92 C 0.0563(2) 0.1448(3) 0.6092(3) 0.086(2) Uani 0.825(7) 1 d PDU C 1 N2X N 0.0130(8) 0.0726(16) 0.5824(16) 0.086(10) Uani 0.175(7) 1 d PDU C 2 C91X C 0.0349(9) 0.1044(15) 0.5935(17) 0.065(8) Uani 0.175(7) 1 d PDU C 2 C92X C 0.0563(2) 0.1448(3) 0.6092(3) 0.086(2) Uani 0.17 1 d PU C 2 N3 N 0.4128(2) -0.1285(3) 0.7032(3) 0.122(2) Uani 1 1 d DU . . C93 C 0.39916(17) -0.1088(3) 0.6603(3) 0.0731(17) Uani 1 1 d DU . . C94 C 0.3822(2) -0.0806(5) 0.6072(3) 0.136(4) Uani 1 1 d DU . . H94A H 0.3708 -0.0428 0.6206 0.204 Uiso 1 1 calc R . . H94B H 0.3646 -0.1086 0.5888 0.204 Uiso 1 1 calc R . . H94C H 0.3993 -0.0708 0.5756 0.204 Uiso 1 1 calc R . . N4 N 0.2290(4) 0.0824(9) 0.5579(6) 0.291(8) Uani 1 1 d DU . . C95 C 0.2126(3) 0.0804(5) 0.5975(5) 0.129(3) Uani 1 1 d DU . . C96 C 0.1911(4) 0.0940(7) 0.6467(6) 0.288(10) Uani 1 1 d DU . . H96A H 0.2045 0.1158 0.6800 0.432 Uiso 1 1 calc R . . H96B H 0.1818 0.0558 0.6639 0.432 Uiso 1 1 calc R . . H96C H 0.1718 0.1198 0.6309 0.432 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0301(16) 0.0439(19) 0.058(2) -0.0106(16) 0.0013(15) 0.0023(14) O2 0.0303(16) 0.0393(18) 0.063(2) -0.0109(16) -0.0119(15) 0.0034(14) O3 0.0287(16) 0.0417(19) 0.059(2) -0.0163(16) -0.0045(15) 0.0037(14) O4 0.0275(16) 0.0410(18) 0.073(2) -0.0191(17) -0.0033(16) 0.0035(14) O5 0.0269(16) 0.048(2) 0.065(2) -0.0188(17) -0.0006(15) 0.0012(14) O6 0.0309(17) 0.0459(19) 0.059(2) -0.0127(17) -0.0069(15) -0.0028(14) O7 0.0345(17) 0.0372(18) 0.064(2) -0.0092(16) -0.0011(16) -0.0034(14) O8 0.0343(17) 0.0372(18) 0.072(2) -0.0101(17) -0.0006(17) 0.0015(14) C1 0.026(2) 0.035(2) 0.037(3) -0.003(2) -0.0002(18) 0.0011(19) C2 0.028(2) 0.040(3) 0.037(3) -0.001(2) -0.0021(19) -0.0013(19) C3 0.034(2) 0.035(2) 0.039(3) 0.000(2) -0.006(2) -0.001(2) C4 0.033(2) 0.038(3) 0.041(3) -0.004(2) -0.002(2) 0.002(2) C5 0.031(2) 0.038(3) 0.037(3) -0.001(2) -0.0018(19) -0.0012(19) C6 0.035(2) 0.034(2) 0.038(3) -0.003(2) -0.003(2) 0.000(2) C7 0.037(3) 0.044(3) 0.053(3) -0.005(2) 0.002(2) 0.002(2) C8 0.059(4) 0.103(5) 0.094(5) -0.051(4) 0.009(3) 0.002(4) C9 0.071(4) 0.077(5) 0.125(6) 0.025(4) 0.024(4) 0.034(4) C10 0.046(3) 0.075(4) 0.132(6) -0.027(4) 0.026(4) 0.000(3) C11 0.030(2) 0.033(2) 0.044(3) 0.000(2) 0.000(2) -0.0009(19) C12 0.024(2) 0.031(2) 0.045(3) 0.002(2) -0.0073(19) 0.0028(18) C13 0.031(2) 0.030(2) 0.040(3) -0.001(2) -0.003(2) -0.0023(19) C14 0.027(2) 0.037(2) 0.044(3) 0.002(2) 0.000(2) 0.0022(19) C15 0.030(2) 0.031(2) 0.045(3) 0.004(2) -0.005(2) 0.0028(19) C16 0.035(2) 0.033(2) 0.042(3) 0.001(2) -0.004(2) 0.000(2) C17 0.031(2) 0.030(2) 0.044(3) 0.002(2) -0.002(2) 0.0025(19) C18 0.033(2) 0.046(3) 0.054(3) 0.002(2) -0.006(2) 0.003(2) C19 0.040(3) 0.062(4) 0.089(4) -0.011(3) -0.016(3) 0.001(3) C20 0.043(3) 0.085(4) 0.071(4) 0.023(3) -0.012(3) 0.010(3) C21 0.034(3) 0.070(4) 0.079(4) -0.007(3) -0.011(3) 0.014(3) C22 0.033(2) 0.033(2) 0.047(3) 0.001(2) 0.003(2) -0.0026(19) C23 0.025(2) 0.034(2) 0.040(3) -0.005(2) 0.0018(19) -0.0007(18) C24 0.028(2) 0.033(2) 0.041(3) 0.000(2) 0.005(2) 0.0021(19) C25 0.030(2) 0.036(3) 0.042(3) 0.003(2) 0.000(2) 0.0049(19) C26 0.031(2) 0.036(3) 0.042(3) -0.001(2) -0.002(2) 0.0017(19) C27 0.032(2) 0.034(2) 0.046(3) 0.000(2) -0.001(2) 0.0027(19) C28 0.029(2) 0.035(2) 0.037(3) 0.000(2) 0.0018(19) -0.0005(19) C29 0.039(3) 0.041(3) 0.044(3) -0.002(2) -0.004(2) -0.004(2) C30 0.103(5) 0.067(4) 0.098(5) -0.040(4) -0.048(4) 0.026(4) C31 0.112(5) 0.057(4) 0.089(5) 0.002(3) -0.065(4) -0.004(4) C32 0.097(5) 0.163(8) 0.084(5) -0.042(5) 0.017(4) -0.087(5) C33 0.030(2) 0.035(2) 0.039(3) -0.003(2) -0.0036(19) 0.0020(19) C34 0.027(2) 0.033(2) 0.042(3) -0.005(2) -0.0053(19) 0.0028(19) C35 0.024(2) 0.035(2) 0.041(3) 0.001(2) -0.0022(19) 0.0047(18) C36 0.032(2) 0.033(2) 0.040(3) 0.000(2) -0.001(2) -0.0018(19) C37 0.035(2) 0.032(2) 0.040(3) -0.002(2) -0.002(2) 0.002(2) C38 0.031(2) 0.035(2) 0.042(3) -0.001(2) -0.001(2) 0.0036(19) C39 0.027(2) 0.030(2) 0.044(3) -0.001(2) -0.003(2) 0.0001(18) C40 0.050(3) 0.034(3) 0.046(3) -0.006(2) 0.005(2) -0.002(2) C41 0.119(10) 0.080(7) 0.063(5) -0.040(5) -0.026(6) 0.037(6) C42 0.135(11) 0.043(5) 0.167(11) -0.042(6) 0.102(10) -0.039(7) C43 0.055(4) 0.046(5) 0.089(7) -0.028(5) 0.004(4) 0.012(4) C44 0.031(2) 0.034(2) 0.047(3) -0.002(2) 0.000(2) -0.0010(19) C45 0.025(2) 0.031(2) 0.050(3) -0.003(2) 0.002(2) -0.0010(18) C46 0.031(2) 0.030(2) 0.045(3) -0.001(2) -0.003(2) -0.0053(19) C47 0.030(2) 0.036(2) 0.043(3) -0.003(2) 0.000(2) -0.0023(19) C48 0.030(2) 0.036(3) 0.050(3) 0.002(2) 0.004(2) -0.0013(19) C49 0.025(2) 0.040(3) 0.045(3) 0.001(2) -0.005(2) -0.0014(19) C50 0.033(2) 0.034(2) 0.043(3) 0.002(2) 0.002(2) -0.0034(19) C51 0.028(2) 0.046(3) 0.055(3) -0.001(2) 0.003(2) 0.004(2) C52 0.042(3) 0.082(4) 0.059(4) 0.007(3) 0.012(3) 0.008(3) C53 0.037(3) 0.098(5) 0.061(4) -0.002(3) -0.001(3) 0.019(3) C54 0.051(3) 0.046(3) 0.121(5) -0.011(3) 0.010(3) 0.015(3) C55 0.036(2) 0.043(3) 0.044(3) -0.001(2) 0.000(2) 0.000(2) C56 0.027(2) 0.042(3) 0.044(3) -0.005(2) -0.001(2) 0.000(2) C57 0.035(2) 0.043(3) 0.041(3) -0.007(2) 0.004(2) -0.001(2) C58 0.037(3) 0.053(3) 0.045(3) -0.011(2) -0.002(2) 0.003(2) C59 0.033(3) 0.058(3) 0.052(3) -0.012(3) -0.001(2) -0.001(2) C60 0.033(3) 0.052(3) 0.051(3) -0.013(2) 0.002(2) -0.010(2) C61 0.035(3) 0.042(3) 0.042(3) -0.007(2) 0.002(2) -0.001(2) C62 0.035(3) 0.074(4) 0.075(4) -0.011(3) -0.010(3) -0.002(3) C63 0.029(6) 0.116(12) 0.109(10) -0.033(9) -0.007(6) 0.006(9) C64 0.050(9) 0.203(19) 0.075(8) 0.029(11) -0.036(7) -0.038(12) C65 0.047(7) 0.093(7) 0.121(14) -0.030(7) -0.025(8) -0.010(6) C63X 0.034(8) 0.15(2) 0.120(12) 0.031(12) 0.006(7) -0.019(13) C64X 0.036(8) 0.100(9) 0.100(13) 0.018(8) -0.029(9) 0.000(8) C65X 0.087(13) 0.120(14) 0.129(16) -0.052(14) -0.065(11) 0.014(11) C66 0.040(3) 0.044(3) 0.042(3) -0.004(2) 0.007(2) -0.006(2) C67 0.031(2) 0.032(2) 0.046(3) 0.000(2) -0.003(2) -0.0039(19) C68 0.037(3) 0.035(3) 0.042(3) -0.003(2) 0.000(2) -0.001(2) C69 0.031(2) 0.047(3) 0.057(3) -0.005(2) 0.003(2) -0.003(2) C70 0.034(3) 0.045(3) 0.049(3) -0.007(2) -0.002(2) -0.003(2) C71 0.032(2) 0.046(3) 0.044(3) -0.005(2) -0.003(2) 0.003(2) C72 0.031(2) 0.036(2) 0.042(3) 0.004(2) 0.000(2) 0.0033(19) C73 0.039(3) 0.066(4) 0.072(4) -0.023(3) 0.002(3) -0.010(3) C74 0.128(6) 0.084(5) 0.109(6) -0.025(4) 0.033(5) -0.072(5) C75 0.071(4) 0.077(4) 0.087(5) -0.039(4) 0.010(3) -0.023(3) C76 0.052(4) 0.131(7) 0.161(8) -0.075(6) -0.043(4) 0.008(4) C77 0.033(2) 0.040(3) 0.047(3) 0.004(2) 0.000(2) 0.000(2) C78 0.026(2) 0.035(3) 0.049(3) -0.003(2) 0.005(2) 0.0004(19) C79 0.027(2) 0.037(3) 0.047(3) 0.004(2) 0.001(2) 0.0001(19) C80 0.032(2) 0.041(3) 0.042(3) 0.001(2) 0.000(2) 0.001(2) C81 0.035(2) 0.038(3) 0.039(3) 0.000(2) 0.004(2) 0.000(2) C82 0.031(2) 0.038(3) 0.040(3) 0.005(2) 0.003(2) 0.0002(19) C83 0.030(2) 0.041(3) 0.037(3) 0.002(2) 0.0015(19) -0.002(2) C84 0.044(3) 0.045(3) 0.043(3) -0.004(2) -0.002(2) 0.005(2) C85 0.080(4) 0.064(4) 0.052(3) -0.012(3) 0.009(3) 0.014(3) C86 0.057(3) 0.045(3) 0.072(4) -0.011(3) -0.009(3) 0.008(3) C87 0.060(3) 0.046(3) 0.068(4) -0.004(3) -0.015(3) -0.008(3) C88 0.032(2) 0.043(3) 0.041(3) 0.003(2) 0.002(2) -0.001(2) N1 0.087(7) 0.70(3) 0.214(14) 0.244(18) 0.055(8) 0.036(16) C89 0.20(2) 0.63(4) 0.40(4) 0.31(2) 0.01(2) 0.12(2) C90 0.187(15) 0.57(3) 0.219(14) 0.316(15) 0.141(12) 0.248(17) N2 0.42(2) 0.327(18) 0.106(9) 0.030(10) 0.041(11) 0.282(17) C91 0.207(13) 0.131(9) 0.066(6) 0.000(6) 0.033(7) 0.073(8) C92 0.104(5) 0.070(5) 0.083(5) -0.009(4) 0.024(4) -0.004(4) N2X 0.07(2) 0.10(2) 0.09(2) -0.026(19) 0.018(18) 0.010(12) C91X 0.07(2) 0.06(2) 0.06(2) -0.005(17) 0.018(18) 0.017(11) C92X 0.104(5) 0.070(5) 0.083(5) -0.009(4) 0.024(4) -0.004(4) N3 0.154(6) 0.110(5) 0.099(5) 0.020(4) -0.026(5) 0.035(5) C93 0.084(5) 0.079(4) 0.056(4) 0.001(3) -0.002(3) 0.010(4) C94 0.130(7) 0.227(11) 0.050(4) 0.019(5) -0.015(4) 0.038(7) N4 0.249(15) 0.48(2) 0.148(11) 0.051(13) 0.051(8) 0.073(15) C95 0.117(8) 0.190(10) 0.080(6) 0.014(7) 0.001(5) 0.017(7) C96 0.45(3) 0.254(16) 0.168(12) 0.114(12) 0.146(13) 0.154(16) _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 1.383(5) . ? O2 C12 1.387(5) . ? O3 C23 1.384(5) . ? O4 C34 1.385(5) . ? O5 C45 1.388(5) . ? O6 C56 1.391(5) . ? O7 C67 1.391(5) . ? O8 C78 1.398(5) . ? C1 C2 1.384(6) . ? C1 C6 1.398(6) . ? C2 C3 1.390(6) . ? C2 C88 1.527(6) . ? C3 C4 1.389(6) . ? C4 C5 1.396(6) . ? C4 C7 1.531(6) . ? C5 C6 1.387(6) . ? C6 C11 1.509(6) . ? C7 C10 1.513(7) . ? C7 C8 1.521(7) . ? C7 C9 1.535(7) . ? C11 C13 1.505(6) . ? C12 C17 1.392(6) . ? C12 C13 1.398(6) . ? C13 C14 1.400(6) . ? C14 C15 1.383(6) . ? C15 C16 1.397(6) . ? C15 C18 1.526(6) . ? C16 C17 1.390(6) . ? C17 C22 1.504(6) . ? C18 C19 1.531(7) . ? C18 C21 1.533(7) . ? C18 C20 1.534(7) . ? C22 C24 1.516(6) . ? C23 C24 1.387(6) . ? C23 C28 1.398(6) . ? C24 C25 1.397(6) . ? C25 C26 1.390(6) . ? C26 C27 1.396(6) . ? C26 C29 1.533(6) . ? C27 C28 1.390(6) . ? C28 C33 1.511(6) . ? C29 C31 1.503(7) . ? C29 C32 1.511(7) . ? C29 C30 1.518(7) . ? C33 C35 1.515(6) . ? C34 C39 1.388(6) . ? C34 C35 1.390(6) . ? C35 C36 1.400(6) . ? C36 C37 1.393(6) . ? C37 C38 1.391(6) . ? C37 C40 1.537(6) . ? C38 C39 1.393(6) . ? C39 C44 1.520(6) . ? C40 C43X 1.471(12) . ? C40 C42 1.495(9) . ? C40 C42X 1.502(14) . ? C40 C41 1.504(8) . ? C40 C43 1.569(7) . ? C40 C41X 1.596(11) . ? C44 C46 1.515(6) . ? C45 C50 1.386(6) . ? C45 C46 1.393(6) . ? C46 C47 1.391(6) . ? C47 C48 1.405(6) . ? C48 C49 1.381(6) . ? C48 C51 1.531(6) . ? C49 C50 1.401(6) . ? C50 C55 1.516(6) . ? C51 C52 1.524(7) . ? C51 C54 1.526(7) . ? C51 C53 1.536(7) . ? C55 C57 1.506(6) . ? C56 C61 1.389(6) . ? C56 C57 1.393(6) . ? C57 C58 1.392(6) . ? C58 C59 1.386(7) . ? C59 C60 1.392(7) . ? C59 C62 1.535(6) . ? C60 C61 1.390(6) . ? C61 C66 1.512(6) . ? C62 C64 1.468(12) . ? C62 C63X 1.497(12) . ? C62 C63 1.532(11) . ? C62 C65X 1.549(11) . ? C62 C64X 1.565(13) . ? C62 C65 1.587(10) . ? C66 C68 1.512(6) . ? C67 C72 1.383(6) . ? C67 C68 1.384(6) . ? C68 C69 1.394(6) . ? C69 C70 1.389(6) . ? C70 C71 1.388(6) . ? C70 C73 1.527(6) . ? C71 C72 1.404(6) . ? C72 C77 1.507(6) . ? C73 C74 1.526(9) . ? C73 C76 1.526(8) . ? C73 C75 1.529(7) . ? C77 C79 1.506(6) . ? C78 C83 1.388(6) . ? C78 C79 1.388(6) . ? C79 C80 1.390(6) . ? C80 C81 1.392(6) . ? C81 C82 1.386(6) . ? C81 C84 1.530(6) . ? C82 C83 1.395(6) . ? C83 C88 1.510(6) . ? C84 C86 1.528(6) . ? C84 C85 1.531(7) . ? C84 C87 1.532(7) . ? N1 C89 1.114(16) . ? C89 C90 1.431(16) . ? N2 C91 1.133(11) . ? C91 C92 1.378(11) . ? N2X C91X 1.110(17) . ? N3 C93 1.115(7) . ? C93 C94 1.417(8) . ? N4 C95 1.068(10) . ? C95 C96 1.386(11) . ? 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 O1 C1 C2 120.6(4) . . ? O1 C1 C6 118.5(4) . . ? C2 C1 C6 121.0(4) . . ? C1 C2 C3 118.6(4) . . ? C1 C2 C88 121.9(4) . . ? C3 C2 C88 119.5(4) . . ? C4 C3 C2 122.8(4) . . ? C3 C4 C5 116.4(4) . . ? C3 C4 C7 120.7(4) . . ? C5 C4 C7 122.9(4) . . ? C6 C5 C4 123.0(4) . . ? C5 C6 C1 118.2(4) . . ? C5 C6 C11 120.3(4) . . ? C1 C6 C11 121.5(4) . . ? C10 C7 C8 109.2(5) . . ? C10 C7 C4 112.5(4) . . ? C8 C7 C4 108.0(4) . . ? C10 C7 C9 107.6(5) . . ? C8 C7 C9 109.2(5) . . ? C4 C7 C9 110.3(4) . . ? C13 C11 C6 111.3(4) . . ? O2 C12 C17 118.8(4) . . ? O2 C12 C13 119.5(4) . . ? C17 C12 C13 121.7(4) . . ? C12 C13 C14 117.5(4) . . ? C12 C13 C11 122.1(4) . . ? C14 C13 C11 120.4(4) . . ? C15 C14 C13 123.0(4) . . ? C14 C15 C16 117.0(4) . . ? C14 C15 C18 123.5(4) . . ? C16 C15 C18 119.5(4) . . ? C17 C16 C15 122.7(4) . . ? C16 C17 C12 118.1(4) . . ? C16 C17 C22 120.2(4) . . ? C12 C17 C22 121.7(4) . . ? C15 C18 C19 109.3(4) . . ? C15 C18 C21 112.2(4) . . ? C19 C18 C21 108.3(4) . . ? C15 C18 C20 109.6(4) . . ? C19 C18 C20 109.5(4) . . ? C21 C18 C20 107.8(4) . . ? C17 C22 C24 114.6(4) . . ? O3 C23 C24 120.6(4) . . ? O3 C23 C28 117.9(4) . . ? C24 C23 C28 121.5(4) . . ? C23 C24 C25 118.2(4) . . ? C23 C24 C22 122.3(4) . . ? C25 C24 C22 119.4(4) . . ? C26 C25 C24 122.8(4) . . ? C25 C26 C27 116.4(4) . . ? C25 C26 C29 122.6(4) . . ? C27 C26 C29 121.0(4) . . ? C28 C27 C26 123.3(4) . . ? C27 C28 C23 117.7(4) . . ? C27 C28 C33 120.5(4) . . ? C23 C28 C33 121.7(4) . . ? C31 C29 C32 111.4(5) . . ? C31 C29 C30 105.7(5) . . ? C32 C29 C30 108.3(5) . . ? C31 C29 C26 112.1(4) . . ? C32 C29 C26 108.7(4) . . ? C30 C29 C26 110.6(4) . . ? C28 C33 C35 112.5(4) . . ? O4 C34 C39 117.5(4) . . ? O4 C34 C35 120.8(4) . . ? C39 C34 C35 121.7(4) . . ? C34 C35 C36 117.3(4) . . ? C34 C35 C33 122.4(4) . . ? C36 C35 C33 120.2(4) . . ? C37 C36 C35 123.2(4) . . ? C38 C37 C36 116.9(4) . . ? C38 C37 C40 121.6(4) . . ? C36 C37 C40 121.5(4) . . ? C37 C38 C39 122.1(4) . . ? C34 C39 C38 118.8(4) . . ? C34 C39 C44 122.0(4) . . ? C38 C39 C44 119.2(4) . . ? C43X C40 C42X 117.2(10) . . ? C42 C40 C41 112.8(7) . . ? C43X C40 C37 114.3(8) . . ? C42 C40 C37 113.5(5) . . ? C42X C40 C37 109.3(9) . . ? C41 C40 C37 109.3(5) . . ? C42 C40 C43 106.2(7) . . ? C41 C40 C43 105.4(6) . . ? C37 C40 C43 109.3(4) . . ? C43X C40 C41X 106.3(10) . . ? C42X C40 C41X 104.1(9) . . ? C37 C40 C41X 104.3(7) . . ? C46 C44 C39 112.5(4) . . ? C50 C45 O5 117.4(4) . . ? C50 C45 C46 121.3(4) . . ? O5 C45 C46 121.2(4) . . ? C47 C46 C45 118.5(4) . . ? C47 C46 C44 119.5(4) . . ? C45 C46 C44 122.0(4) . . ? C46 C47 C48 121.9(4) . . ? C49 C48 C47 117.5(4) . . ? C49 C48 C51 123.5(4) . . ? C47 C48 C51 118.9(4) . . ? C48 C49 C50 122.1(4) . . ? C45 C50 C49 118.6(4) . . ? C45 C50 C55 121.0(4) . . ? C49 C50 C55 120.4(4) . . ? C52 C51 C54 109.1(4) . . ? C52 C51 C48 109.8(4) . . ? C54 C51 C48 109.5(4) . . ? C52 C51 C53 107.5(4) . . ? C54 C51 C53 109.1(4) . . ? C48 C51 C53 112.0(4) . . ? C57 C55 C50 110.6(4) . . ? C61 C56 O6 117.5(4) . . ? C61 C56 C57 121.5(4) . . ? O6 C56 C57 121.1(4) . . ? C58 C57 C56 117.7(4) . . ? C58 C57 C55 119.9(4) . . ? C56 C57 C55 122.2(4) . . ? C59 C58 C57 122.9(5) . . ? C58 C59 C60 117.2(4) . . ? C58 C59 C62 121.3(5) . . ? C60 C59 C62 121.6(4) . . ? C61 C60 C59 122.2(4) . . ? C56 C61 C60 118.4(4) . . ? C56 C61 C66 121.8(4) . . ? C60 C61 C66 119.8(4) . . ? C64 C62 C63 114.0(10) . . ? C64 C62 C59 110.6(7) . . ? C63X C62 C59 108.9(10) . . ? C63 C62 C59 107.3(7) . . ? C63X C62 C65X 115.6(12) . . ? C59 C62 C65X 109.0(7) . . ? C63X C62 C64X 107.0(10) . . ? C59 C62 C64X 111.0(7) . . ? C65X C62 C64X 105.1(10) . . ? C64 C62 C65 109.5(9) . . ? C63 C62 C65 104.0(9) . . ? C59 C62 C65 111.3(6) . . ? C61 C66 C68 111.9(4) . . ? C72 C67 C68 121.5(4) . . ? C72 C67 O7 117.2(4) . . ? C68 C67 O7 121.3(4) . . ? C67 C68 C69 118.1(4) . . ? C67 C68 C66 121.9(4) . . ? C69 C68 C66 120.0(4) . . ? C70 C69 C68 123.0(4) . . ? C71 C70 C69 116.9(4) . . ? C71 C70 C73 122.6(4) . . ? C69 C70 C73 120.5(4) . . ? C70 C71 C72 122.1(4) . . ? C67 C72 C71 118.5(4) . . ? C67 C72 C77 122.7(4) . . ? C71 C72 C77 118.8(4) . . ? C74 C73 C76 110.8(6) . . ? C74 C73 C70 109.3(5) . . ? C76 C73 C70 108.7(5) . . ? C74 C73 C75 108.3(5) . . ? C76 C73 C75 107.7(5) . . ? C70 C73 C75 112.0(4) . . ? C79 C77 C72 111.9(4) . . ? C83 C78 C79 121.9(4) . . ? C83 C78 O8 118.0(4) . . ? C79 C78 O8 120.1(4) . . ? C78 C79 C80 117.5(4) . . ? C78 C79 C77 122.9(4) . . ? C80 C79 C77 119.6(4) . . ? C79 C80 C81 123.4(4) . . ? C82 C81 C80 116.4(4) . . ? C82 C81 C84 123.9(4) . . ? C80 C81 C84 119.6(4) . . ? C81 C82 C83 122.9(4) . . ? C78 C83 C82 117.9(4) . . ? C78 C83 C88 121.9(4) . . ? C82 C83 C88 120.2(4) . . ? C86 C84 C81 111.7(4) . . ? C86 C84 C85 108.3(4) . . ? C81 C84 C85 109.7(4) . . ? C86 C84 C87 108.9(4) . . ? C81 C84 C87 109.1(4) . . ? C85 C84 C87 108.9(4) . . ? C83 C88 C2 111.3(4) . . ? N1 C89 C90 159(4) . . ? N2 C91 C92 178.1(18) . . ? N3 C93 C94 176.9(9) . . ? N4 C95 C96 165.3(18) . . ? 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 O1 C1 C2 C3 179.1(4) . . . . ? C6 C1 C2 C3 -2.9(6) . . . . ? O1 C1 C2 C88 -0.8(6) . . . . ? C6 C1 C2 C88 177.2(4) . . . . ? C1 C2 C3 C4 0.9(7) . . . . ? C88 C2 C3 C4 -179.2(4) . . . . ? C2 C3 C4 C5 1.2(6) . . . . ? C2 C3 C4 C7 -178.2(4) . . . . ? C3 C4 C5 C6 -1.6(7) . . . . ? C7 C4 C5 C6 177.9(4) . . . . ? C4 C5 C6 C1 -0.3(7) . . . . ? C4 C5 C6 C11 177.6(4) . . . . ? O1 C1 C6 C5 -179.4(4) . . . . ? C2 C1 C6 C5 2.5(6) . . . . ? O1 C1 C6 C11 2.8(6) . . . . ? C2 C1 C6 C11 -175.3(4) . . . . ? C3 C4 C7 C10 -171.9(5) . . . . ? C5 C4 C7 C10 8.7(7) . . . . ? C3 C4 C7 C8 67.6(6) . . . . ? C5 C4 C7 C8 -111.9(5) . . . . ? C3 C4 C7 C9 -51.7(6) . . . . ? C5 C4 C7 C9 128.9(5) . . . . ? C5 C6 C11 C13 -99.9(5) . . . . ? C1 C6 C11 C13 77.9(5) . . . . ? O2 C12 C13 C14 -178.6(4) . . . . ? C17 C12 C13 C14 1.2(6) . . . . ? O2 C12 C13 C11 0.5(6) . . . . ? C17 C12 C13 C11 -179.7(4) . . . . ? C6 C11 C13 C12 -101.1(5) . . . . ? C6 C11 C13 C14 78.0(5) . . . . ? C12 C13 C14 C15 0.1(6) . . . . ? C11 C13 C14 C15 -179.0(4) . . . . ? C13 C14 C15 C16 -1.6(6) . . . . ? C13 C14 C15 C18 179.4(4) . . . . ? C14 C15 C16 C17 1.9(6) . . . . ? C18 C15 C16 C17 -179.1(4) . . . . ? C15 C16 C17 C12 -0.6(6) . . . . ? C15 C16 C17 C22 178.7(4) . . . . ? O2 C12 C17 C16 178.8(4) . . . . ? C13 C12 C17 C16 -0.9(6) . . . . ? O2 C12 C17 C22 -0.5(6) . . . . ? C13 C12 C17 C22 179.7(4) . . . . ? C14 C15 C18 C19 112.7(5) . . . . ? C16 C15 C18 C19 -66.4(5) . . . . ? C14 C15 C18 C21 -7.5(6) . . . . ? C16 C15 C18 C21 173.4(4) . . . . ? C14 C15 C18 C20 -127.3(5) . . . . ? C16 C15 C18 C20 53.7(6) . . . . ? C16 C17 C22 C24 94.1(5) . . . . ? C12 C17 C22 C24 -86.6(5) . . . . ? O3 C23 C24 C25 179.9(4) . . . . ? C28 C23 C24 C25 -3.2(6) . . . . ? O3 C23 C24 C22 -3.2(6) . . . . ? C28 C23 C24 C22 173.6(4) . . . . ? C17 C22 C24 C23 93.3(5) . . . . ? C17 C22 C24 C25 -89.8(5) . . . . ? C23 C24 C25 C26 1.8(6) . . . . ? C22 C24 C25 C26 -175.2(4) . . . . ? C24 C25 C26 C27 0.1(6) . . . . ? C24 C25 C26 C29 179.5(4) . . . . ? C25 C26 C27 C28 -0.6(7) . . . . ? C29 C26 C27 C28 180.0(4) . . . . ? C26 C27 C28 C23 -0.7(6) . . . . ? C26 C27 C28 C33 175.2(4) . . . . ? O3 C23 C28 C27 179.6(4) . . . . ? C24 C23 C28 C27 2.7(6) . . . . ? O3 C23 C28 C33 3.8(6) . . . . ? C24 C23 C28 C33 -173.1(4) . . . . ? C25 C26 C29 C31 -20.8(7) . . . . ? C27 C26 C29 C31 158.6(5) . . . . ? C25 C26 C29 C32 102.7(6) . . . . ? C27 C26 C29 C32 -77.9(6) . . . . ? C25 C26 C29 C30 -138.5(5) . . . . ? C27 C26 C29 C30 40.9(6) . . . . ? C27 C28 C33 C35 -86.1(5) . . . . ? C23 C28 C33 C35 89.6(5) . . . . ? O4 C34 C35 C36 -179.9(4) . . . . ? C39 C34 C35 C36 -0.3(6) . . . . ? O4 C34 C35 C33 -2.7(6) . . . . ? C39 C34 C35 C33 176.9(4) . . . . ? C28 C33 C35 C34 -84.9(5) . . . . ? C28 C33 C35 C36 92.2(5) . . . . ? C34 C35 C36 C37 0.4(6) . . . . ? C33 C35 C36 C37 -176.8(4) . . . . ? C35 C36 C37 C38 -0.7(6) . . . . ? C35 C36 C37 C40 178.2(4) . . . . ? C36 C37 C38 C39 1.0(6) . . . . ? C40 C37 C38 C39 -178.0(4) . . . . ? O4 C34 C39 C38 -179.9(4) . . . . ? C35 C34 C39 C38 0.5(6) . . . . ? O4 C34 C39 C44 1.1(6) . . . . ? C35 C34 C39 C44 -178.6(4) . . . . ? C37 C38 C39 C34 -0.9(6) . . . . ? C37 C38 C39 C44 178.2(4) . . . . ? C38 C37 C40 C43X 7.3(10) . . . . ? C36 C37 C40 C43X -171.6(9) . . . . ? C38 C37 C40 C42 -155.2(8) . . . . ? C36 C37 C40 C42 25.9(9) . . . . ? C38 C37 C40 C42X -126.2(8) . . . . ? C36 C37 C40 C42X 54.9(8) . . . . ? C38 C37 C40 C41 78.0(7) . . . . ? C36 C37 C40 C41 -100.9(7) . . . . ? C38 C37 C40 C43 -36.8(7) . . . . ? C36 C37 C40 C43 144.3(6) . . . . ? C38 C37 C40 C41X 123.0(8) . . . . ? C36 C37 C40 C41X -55.9(9) . . . . ? C34 C39 C44 C46 -92.8(5) . . . . ? C38 C39 C44 C46 88.2(5) . . . . ? C50 C45 C46 C47 1.0(6) . . . . ? O5 C45 C46 C47 -177.3(4) . . . . ? C50 C45 C46 C44 -178.1(4) . . . . ? O5 C45 C46 C44 3.7(6) . . . . ? C39 C44 C46 C47 -94.8(5) . . . . ? C39 C44 C46 C45 84.3(5) . . . . ? C45 C46 C47 C48 0.0(6) . . . . ? C44 C46 C47 C48 179.1(4) . . . . ? C46 C47 C48 C49 -0.9(6) . . . . ? C46 C47 C48 C51 179.1(4) . . . . ? C47 C48 C49 C50 0.9(6) . . . . ? C51 C48 C49 C50 -179.1(4) . . . . ? O5 C45 C50 C49 177.3(4) . . . . ? C46 C45 C50 C49 -1.0(6) . . . . ? O5 C45 C50 C55 -0.1(6) . . . . ? C46 C45 C50 C55 -178.5(4) . . . . ? C48 C49 C50 C45 0.1(6) . . . . ? C48 C49 C50 C55 177.5(4) . . . . ? C49 C48 C51 C52 125.3(5) . . . . ? C47 C48 C51 C52 -54.7(5) . . . . ? C49 C48 C51 C54 -115.1(5) . . . . ? C47 C48 C51 C54 64.9(6) . . . . ? C49 C48 C51 C53 6.0(6) . . . . ? C47 C48 C51 C53 -174.0(4) . . . . ? C45 C50 C55 C57 97.6(5) . . . . ? C49 C50 C55 C57 -79.8(5) . . . . ? C61 C56 C57 C58 -3.0(7) . . . . ? O6 C56 C57 C58 177.8(4) . . . . ? C61 C56 C57 C55 173.2(4) . . . . ? O6 C56 C57 C55 -6.0(7) . . . . ? C50 C55 C57 C58 94.1(5) . . . . ? C50 C55 C57 C56 -82.0(5) . . . . ? C56 C57 C58 C59 0.9(7) . . . . ? C55 C57 C58 C59 -175.4(4) . . . . ? C57 C58 C59 C60 1.0(7) . . . . ? C57 C58 C59 C62 -179.0(5) . . . . ? C58 C59 C60 C61 -0.9(7) . . . . ? C62 C59 C60 C61 179.1(5) . . . . ? O6 C56 C61 C60 -177.7(4) . . . . ? C57 C56 C61 C60 3.1(7) . . . . ? O6 C56 C61 C66 1.2(6) . . . . ? C57 C56 C61 C66 -178.1(4) . . . . ? C59 C60 C61 C56 -1.1(7) . . . . ? C59 C60 C61 C66 -179.9(4) . . . . ? C58 C59 C62 C64 50.9(13) . . . . ? C60 C59 C62 C64 -129.1(13) . . . . ? C58 C59 C62 C63X -108.8(13) . . . . ? C60 C59 C62 C63X 71.1(13) . . . . ? C58 C59 C62 C63 -74.0(11) . . . . ? C60 C59 C62 C63 105.9(10) . . . . ? C58 C59 C62 C65X 124.2(14) . . . . ? C60 C59 C62 C65X -55.9(15) . . . . ? C58 C59 C62 C64X 8.8(12) . . . . ? C60 C59 C62 C64X -171.3(11) . . . . ? C58 C59 C62 C65 172.9(10) . . . . ? C60 C59 C62 C65 -7.2(11) . . . . ? C56 C61 C66 C68 -97.4(5) . . . . ? C60 C61 C66 C68 81.4(5) . . . . ? C72 C67 C68 C69 1.0(7) . . . . ? O7 C67 C68 C69 -177.5(4) . . . . ? C72 C67 C68 C66 -177.1(4) . . . . ? O7 C67 C68 C66 4.3(7) . . . . ? C61 C66 C68 C67 85.8(5) . . . . ? C61 C66 C68 C69 -92.3(5) . . . . ? C67 C68 C69 C70 0.2(7) . . . . ? C66 C68 C69 C70 178.4(4) . . . . ? C68 C69 C70 C71 -1.1(7) . . . . ? C68 C69 C70 C73 178.3(5) . . . . ? C69 C70 C71 C72 0.9(7) . . . . ? C73 C70 C71 C72 -178.5(5) . . . . ? C68 C67 C72 C71 -1.2(6) . . . . ? O7 C67 C72 C71 177.4(4) . . . . ? C68 C67 C72 C77 -177.5(4) . . . . ? O7 C67 C72 C77 1.1(6) . . . . ? C70 C71 C72 C67 0.2(7) . . . . ? C70 C71 C72 C77 176.6(4) . . . . ? C71 C70 C73 C74 122.9(6) . . . . ? C69 C70 C73 C74 -56.4(7) . . . . ? C71 C70 C73 C76 -116.0(6) . . . . ? C69 C70 C73 C76 64.7(7) . . . . ? C71 C70 C73 C75 2.9(7) . . . . ? C69 C70 C73 C75 -176.4(5) . . . . ? C67 C72 C77 C79 93.1(5) . . . . ? C71 C72 C77 C79 -83.2(5) . . . . ? C83 C78 C79 C80 1.8(6) . . . . ? O8 C78 C79 C80 179.0(4) . . . . ? C83 C78 C79 C77 -179.6(4) . . . . ? O8 C78 C79 C77 -2.4(6) . . . . ? C72 C77 C79 C78 -90.5(5) . . . . ? C72 C77 C79 C80 88.1(5) . . . . ? C78 C79 C80 C81 0.5(7) . . . . ? C77 C79 C80 C81 -178.1(4) . . . . ? C79 C80 C81 C82 -1.9(6) . . . . ? C79 C80 C81 C84 179.2(4) . . . . ? C80 C81 C82 C83 1.2(6) . . . . ? C84 C81 C82 C83 -180.0(4) . . . . ? C79 C78 C83 C82 -2.5(6) . . . . ? O8 C78 C83 C82 -179.8(4) . . . . ? C79 C78 C83 C88 174.3(4) . . . . ? O8 C78 C83 C88 -3.0(6) . . . . ? C81 C82 C83 C78 1.0(6) . . . . ? C81 C82 C83 C88 -175.9(4) . . . . ? C82 C81 C84 C86 0.3(6) . . . . ? C80 C81 C84 C86 179.1(4) . . . . ? C82 C81 C84 C85 -119.9(5) . . . . ? C80 C81 C84 C85 58.9(6) . . . . ? C82 C81 C84 C87 120.8(5) . . . . ? C80 C81 C84 C87 -60.4(5) . . . . ? C78 C83 C88 C2 -85.4(5) . . . . ? C82 C83 C88 C2 91.3(5) . . . . ? C1 C2 C88 C83 98.9(5) . . . . ? C3 C2 C88 C83 -81.0(5) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O8 0.84 1.93 2.763(4) 173.8 . O2 H2 O1 0.84 1.87 2.693(4) 166.7 . O3 H3 O2 0.84 1.81 2.648(4) 176.7 . O4 H4 O3 0.84 1.78 2.606(4) 165.6 . O5 H5 O4 0.84 1.78 2.619(4) 174.3 . O6 H6 O5 0.84 1.85 2.681(4) 170.5 . O7 H7 O6 0.84 1.90 2.743(4) 175.5 . O8 H8 O7 0.84 1.92 2.763(4) 177.2 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.712 _refine_diff_density_min -0.551 _refine_diff_density_rms 0.058 #===END data_4 _database_code_CSD 219745 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C92 H118 N2 O8' _chemical_formula_weight 1379.88 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 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 monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 20.1552(9) _cell_length_b 22.9575(10) _cell_length_c 19.7543(9) _cell_angle_alpha 90.00 _cell_angle_beta 112.455(2) _cell_angle_gamma 90.00 _cell_volume 8447.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 17612 _cell_measurement_theta_min 2.15 _cell_measurement_theta_max 28.04 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.44 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.085 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2992 _exptl_absorpt_coefficient_mu 0.068 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.964 _exptl_absorpt_correction_T_max 0.985 _exptl_absorpt_process_details 'SADABS v2.08 (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1000 CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 73214 _diffrn_reflns_av_R_equivalents 0.0496 _diffrn_reflns_av_sigmaI/netI 0.0422 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 25.00 _reflns_number_total 14882 _reflns_number_gt 10177 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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. Platon Squeeze applied. R1 (before Squeeze with 1.5 MeCN only) was 6.58%. Void space calculated with volume 585.3 ang cubed, 44 electrons recovered, close to 40 electrons in two MeCN. Thus half of an MecN per calixarene - this has been added to the formula. ; _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^)+(0.0995P)^2^+0.6345P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary 'All non-H atoms found by direct methods' _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14882 _refine_ls_number_parameters 1047 _refine_ls_number_restraints 342 _refine_ls_R_factor_all 0.0831 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1783 _refine_ls_wR_factor_gt 0.1629 _refine_ls_goodness_of_fit_ref 1.134 _refine_ls_restrained_S_all 1.175 _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 0.37521(8) 0.10379(7) 0.31832(9) 0.0343(4) Uani 1 1 d . . . H1 H 0.3365 0.1178 0.2888 0.051 Uiso 1 1 calc R . . O2 O 0.43756(8) -0.00384(7) 0.34591(9) 0.0336(4) Uani 1 1 d . . . H2 H 0.4225 0.0303 0.3461 0.050 Uiso 1 1 calc R . . O3 O 0.36425(8) -0.10600(7) 0.32244(9) 0.0331(4) Uani 1 1 d . . . H3 H 0.3851 -0.0735 0.3316 0.050 Uiso 1 1 calc R . . O4 O 0.22333(8) -0.13735(7) 0.25112(9) 0.0341(4) Uani 1 1 d . . . H4 H 0.2661 -0.1266 0.2732 0.051 Uiso 1 1 calc R . . O5 O 0.08085(8) -0.10001(7) 0.18609(8) 0.0319(4) Uani 1 1 d . . . H5 H 0.1223 -0.1135 0.1963 0.048 Uiso 1 1 calc R . . O6 O 0.03389(8) 0.01163(7) 0.15360(9) 0.0372(4) Uani 1 1 d . . . H6 H 0.0462 -0.0228 0.1672 0.056 Uiso 1 1 calc R . . O7 O 0.11130(8) 0.10772(7) 0.19020(10) 0.0370(4) Uani 1 1 d . . . H7 H 0.0886 0.0761 0.1796 0.056 Uiso 1 1 calc R . . O8 O 0.24499(8) 0.14305(7) 0.24324(9) 0.0366(4) Uani 1 1 d . . . H8 H 0.2016 0.1331 0.2275 0.055 Uiso 1 1 calc R . . C1 C 0.43130(11) 0.14009(9) 0.32257(12) 0.0262(5) Uani 1 1 d . . . C2 C 0.42531(11) 0.18118(9) 0.26800(12) 0.0264(5) Uani 1 1 d . . . C3 C 0.48643(12) 0.21194(10) 0.27351(12) 0.0292(5) Uani 1 1 d . . . H3A H 0.4829 0.2396 0.2365 0.035 Uiso 1 1 calc R . . C4 C 0.55268(12) 0.20421(10) 0.33077(12) 0.0310(5) Uani 1 1 d . A . C5 C 0.55483(12) 0.16551(10) 0.38593(12) 0.0286(5) Uani 1 1 d . . . H5A H 0.5986 0.1608 0.4270 0.034 Uiso 1 1 calc R . . C6 C 0.49518(11) 0.13365(9) 0.38303(12) 0.0251(5) Uani 1 1 d . . . C7 C 0.61905(13) 0.23621(12) 0.32976(15) 0.0445(6) Uani 1 1 d DU . . C8 C 0.60407(19) 0.30210(14) 0.3233(2) 0.0585(10) Uani 0.856(4) 1 d PDU A 1 H8A H 0.5972 0.3159 0.3671 0.088 Uiso 0.856(4) 1 calc PR A 1 H8B H 0.5606 0.3099 0.2799 0.088 Uiso 0.856(4) 1 calc PR A 1 H8C H 0.6449 0.3225 0.3188 0.088 Uiso 0.856(4) 1 calc PR A 1 C9 C 0.62992(18) 0.21775(16) 0.25915(19) 0.0551(10) Uani 0.856(4) 1 d PDU A 1 H9A H 0.6730 0.2367 0.2578 0.083 Uiso 0.856(4) 1 calc PR A 1 H9B H 0.5880 0.2295 0.2161 0.083 Uiso 0.856(4) 1 calc PR A 1 H9C H 0.6356 0.1754 0.2589 0.083 Uiso 0.856(4) 1 calc PR A 1 C10 C 0.68533(18) 0.2233(2) 0.3948(2) 0.0799(16) Uani 0.856(4) 1 d PDU A 1 H10A H 0.7262 0.2436 0.3902 0.120 Uiso 0.856(4) 1 calc PR A 1 H10B H 0.6943 0.1812 0.3980 0.120 Uiso 0.856(4) 1 calc PR A 1 H10C H 0.6792 0.2366 0.4393 0.120 Uiso 0.856(4) 1 calc PR A 1 C8X C 0.6514(10) 0.2702(8) 0.4053(7) 0.056(4) Uani 0.144(4) 1 d PDU A 2 H8X1 H 0.6959 0.2898 0.4091 0.083 Uiso 0.144(4) 1 calc PR A 2 H8X2 H 0.6617 0.2425 0.4458 0.083 Uiso 0.144(4) 1 calc PR A 2 H8X3 H 0.6167 0.2991 0.4076 0.083 Uiso 0.144(4) 1 calc PR A 2 C9X C 0.6202(12) 0.2793(7) 0.2725(8) 0.065(5) Uani 0.144(4) 1 d PDU A 2 H9X1 H 0.6355 0.3175 0.2953 0.097 Uiso 0.144(4) 1 calc PR A 2 H9X2 H 0.5719 0.2825 0.2342 0.097 Uiso 0.144(4) 1 calc PR A 2 H9X3 H 0.6538 0.2659 0.2508 0.097 Uiso 0.144(4) 1 calc PR A 2 C10X C 0.6797(8) 0.1906(7) 0.3419(12) 0.059(4) Uani 0.144(4) 1 d PDU A 2 H10D H 0.6647 0.1628 0.3012 0.088 Uiso 0.144(4) 1 calc PR A 2 H10E H 0.6891 0.1697 0.3879 0.088 Uiso 0.144(4) 1 calc PR A 2 H10F H 0.7235 0.2105 0.3442 0.088 Uiso 0.144(4) 1 calc PR A 2 C11 C 0.50034(11) 0.09221(9) 0.44510(12) 0.0262(5) Uani 1 1 d . . . H11A H 0.5251 0.1121 0.4926 0.031 Uiso 1 1 calc R . . H11B H 0.4514 0.0819 0.4414 0.031 Uiso 1 1 calc R . . C12 C 0.50899(11) -0.00734(9) 0.39365(11) 0.0255(5) Uani 1 1 d . . . C13 C 0.54069(11) 0.03712(9) 0.44307(11) 0.0252(5) Uani 1 1 d . . . C14 C 0.61191(12) 0.03078(10) 0.48990(13) 0.0310(5) Uani 1 1 d . . . H14 H 0.6334 0.0608 0.5245 0.037 Uiso 1 1 calc R . . C15 C 0.65354(12) -0.01752(10) 0.48866(13) 0.0334(5) Uani 1 1 d . B . C16 C 0.61940(12) -0.06022(10) 0.43700(13) 0.0318(5) Uani 1 1 d . . . H16 H 0.6462 -0.0935 0.4342 0.038 Uiso 1 1 calc R . . C17 C 0.54788(11) -0.05650(9) 0.38921(12) 0.0272(5) Uani 1 1 d . . . C18 C 0.73234(13) -0.02291(11) 0.53926(15) 0.0462(6) Uani 1 1 d DU . . C19 C 0.7454(3) -0.0834(2) 0.5762(3) 0.0486(12) Uani 0.651(6) 1 d PDU B 1 H19A H 0.7273 -0.1137 0.5387 0.073 Uiso 0.651(6) 1 calc PR B 1 H19B H 0.7202 -0.0858 0.6099 0.073 Uiso 0.651(6) 1 calc PR B 1 H19C H 0.7970 -0.0890 0.6036 0.073 Uiso 0.651(6) 1 calc PR B 1 C20 C 0.7602(3) 0.0242(2) 0.5935(4) 0.086(2) Uani 0.651(6) 1 d PDU B 1 H20A H 0.8109 0.0171 0.6233 0.130 Uiso 0.651(6) 1 calc PR B 1 H20B H 0.7328 0.0254 0.6251 0.130 Uiso 0.651(6) 1 calc PR B 1 H20C H 0.7553 0.0616 0.5680 0.130 Uiso 0.651(6) 1 calc PR B 1 C21 C 0.7778(2) -0.0235(2) 0.4895(3) 0.0638(15) Uani 0.651(6) 1 d PDU B 1 H21A H 0.7604 -0.0546 0.4530 0.096 Uiso 0.651(6) 1 calc PR B 1 H21B H 0.8285 -0.0304 0.5200 0.096 Uiso 0.651(6) 1 calc PR B 1 H21C H 0.7729 0.0141 0.4645 0.096 Uiso 0.651(6) 1 calc PR B 1 C19X C 0.7658(6) -0.0803(4) 0.5426(7) 0.087(4) Uani 0.349(6) 1 d PDU B 2 H19D H 0.8168 -0.0753 0.5520 0.131 Uiso 0.349(6) 1 calc PR B 2 H19E H 0.7420 -0.1006 0.4959 0.131 Uiso 0.349(6) 1 calc PR B 2 H19F H 0.7607 -0.1033 0.5822 0.131 Uiso 0.349(6) 1 calc PR B 2 C20X C 0.7367(4) -0.0071(4) 0.6199(4) 0.048(2) Uani 0.349(6) 1 d PDU B 2 H20D H 0.7459 0.0346 0.6288 0.072 Uiso 0.349(6) 1 calc PR B 2 H20E H 0.7757 -0.0293 0.6562 0.072 Uiso 0.349(6) 1 calc PR B 2 H20F H 0.6911 -0.0171 0.6240 0.072 Uiso 0.349(6) 1 calc PR B 2 C21X C 0.7709(5) 0.0301(4) 0.5225(6) 0.076(3) Uani 0.349(6) 1 d PDU B 2 H21D H 0.7728 0.0619 0.5563 0.113 Uiso 0.349(6) 1 calc PR B 2 H21E H 0.7446 0.0430 0.4720 0.113 Uiso 0.349(6) 1 calc PR B 2 H21F H 0.8199 0.0190 0.5287 0.113 Uiso 0.349(6) 1 calc PR B 2 C22 C 0.51340(12) -0.10605(10) 0.33672(12) 0.0296(5) Uani 1 1 d . . . H22A H 0.4752 -0.0903 0.2922 0.036 Uiso 1 1 calc R . . H22B H 0.5499 -0.1248 0.3218 0.036 Uiso 1 1 calc R . . C23 C 0.41001(11) -0.14858(9) 0.36508(11) 0.0263(5) Uani 1 1 d . . . C24 C 0.48148(11) -0.15108(9) 0.37161(11) 0.0258(5) Uani 1 1 d . . . C25 C 0.52469(11) -0.19461(10) 0.41524(12) 0.0284(5) Uani 1 1 d . . . H25 H 0.5731 -0.1969 0.4192 0.034 Uiso 1 1 calc R . . C26 C 0.50097(12) -0.23508(10) 0.45356(12) 0.0291(5) Uani 1 1 d . . . C27 C 0.42893(12) -0.23075(10) 0.44475(12) 0.0285(5) Uani 1 1 d . . . H27 H 0.4105 -0.2581 0.4692 0.034 Uiso 1 1 calc R . . C28 C 0.38305(11) -0.18811(9) 0.40166(11) 0.0253(5) Uani 1 1 d . . . C29 C 0.55237(12) -0.28088(11) 0.50245(13) 0.0352(6) Uani 1 1 d . . . C30 C 0.51919(17) -0.31361(15) 0.54884(18) 0.0652(9) Uani 1 1 d . . . H30A H 0.4762 -0.3343 0.5167 0.098 Uiso 1 1 calc R . . H30B H 0.5061 -0.2859 0.5793 0.098 Uiso 1 1 calc R . . H30C H 0.5540 -0.3417 0.5803 0.098 Uiso 1 1 calc R . . C31 C 0.61968(16) -0.25010(14) 0.55648(17) 0.0619(9) Uani 1 1 d . . . H31A H 0.6523 -0.2791 0.5886 0.093 Uiso 1 1 calc R . . H31B H 0.6055 -0.2222 0.5861 0.093 Uiso 1 1 calc R . . H31C H 0.6440 -0.2294 0.5291 0.093 Uiso 1 1 calc R . . C32 C 0.5738(2) -0.32315(14) 0.45576(17) 0.0701(10) Uani 1 1 d . . . H32A H 0.6100 -0.3501 0.4874 0.105 Uiso 1 1 calc R . . H32B H 0.5937 -0.3016 0.4250 0.105 Uiso 1 1 calc R . . H32C H 0.5315 -0.3451 0.4245 0.105 Uiso 1 1 calc R . . C33 C 0.30622(11) -0.18557(10) 0.39528(12) 0.0273(5) Uani 1 1 d . . . H33A H 0.2903 -0.1444 0.3891 0.033 Uiso 1 1 calc R . . H33B H 0.3037 -0.2000 0.4415 0.033 Uiso 1 1 calc R . . C34 C 0.21739(11) -0.19632(9) 0.26387(12) 0.0257(5) Uani 1 1 d . . . C35 C 0.25493(11) -0.22097(9) 0.33194(11) 0.0252(5) Uani 1 1 d . . . C36 C 0.24374(12) -0.27934(10) 0.34191(13) 0.0311(5) Uani 1 1 d . . . H36 H 0.2699 -0.2965 0.3882 0.037 Uiso 1 1 calc R . . C37 C 0.19583(13) -0.31386(10) 0.28705(13) 0.0345(6) Uani 1 1 d . C . C38 C 0.16046(12) -0.28739(10) 0.21965(13) 0.0312(5) Uani 1 1 d . . . H38 H 0.1282 -0.3101 0.1808 0.037 Uiso 1 1 calc R . . C39 C 0.17013(11) -0.22936(10) 0.20661(12) 0.0267(5) Uani 1 1 d . . . C40 C 0.18017(15) -0.37763(11) 0.29863(16) 0.0518(7) Uani 1 1 d DU . . C41 C 0.2159(3) -0.39641(17) 0.3782(2) 0.0802(14) Uani 0.877(4) 1 d PDU C 1 H41A H 0.1998 -0.4357 0.3839 0.120 Uiso 0.877(4) 1 calc PR C 1 H41B H 0.2028 -0.3693 0.4093 0.120 Uiso 0.877(4) 1 calc PR C 1 H41C H 0.2681 -0.3964 0.3926 0.120 Uiso 0.877(4) 1 calc PR C 1 C42 C 0.2028(3) -0.41579(15) 0.2491(2) 0.0791(13) Uani 0.877(4) 1 d PDU C 1 H42A H 0.2551 -0.4137 0.2641 0.119 Uiso 0.877(4) 1 calc PR C 1 H42B H 0.1795 -0.4023 0.1984 0.119 Uiso 0.877(4) 1 calc PR C 1 H42C H 0.1886 -0.4561 0.2527 0.119 Uiso 0.877(4) 1 calc PR C 1 C43 C 0.09746(19) -0.38480(16) 0.2774(2) 0.0664(11) Uani 0.877(4) 1 d PDU C 1 H43A H 0.0870 -0.4249 0.2872 0.100 Uiso 0.877(4) 1 calc PR C 1 H43B H 0.0722 -0.3761 0.2252 0.100 Uiso 0.877(4) 1 calc PR C 1 H43C H 0.0814 -0.3579 0.3065 0.100 Uiso 0.877(4) 1 calc PR C 1 C41X C 0.2562(7) -0.4059(11) 0.3313(15) 0.081(5) Uani 0.123(4) 1 d PDU C 2 H41D H 0.2519 -0.4463 0.3452 0.121 Uiso 0.123(4) 1 calc PR C 2 H41E H 0.2864 -0.3840 0.3747 0.121 Uiso 0.123(4) 1 calc PR C 2 H41F H 0.2779 -0.4053 0.2947 0.121 Uiso 0.123(4) 1 calc PR C 2 C42X C 0.1347(12) -0.4078(11) 0.2289(9) 0.082(6) Uani 0.123(4) 1 d PDU C 2 H42D H 0.1593 -0.4071 0.1946 0.123 Uiso 0.123(4) 1 calc PR C 2 H42E H 0.0884 -0.3877 0.2069 0.123 Uiso 0.123(4) 1 calc PR C 2 H42F H 0.1266 -0.4483 0.2395 0.123 Uiso 0.123(4) 1 calc PR C 2 C43X C 0.1487(13) -0.3797(10) 0.3577(11) 0.069(4) Uani 0.123(4) 1 d PDU C 2 H43D H 0.1010 -0.3617 0.3390 0.104 Uiso 0.123(4) 1 calc PR C 2 H43E H 0.1802 -0.3585 0.4011 0.104 Uiso 0.123(4) 1 calc PR C 2 H43F H 0.1447 -0.4204 0.3709 0.104 Uiso 0.123(4) 1 calc PR C 2 C44 C 0.12804(11) -0.20318(10) 0.13208(12) 0.0298(5) Uani 1 1 d . . . H44A H 0.1512 -0.1663 0.1272 0.036 Uiso 1 1 calc R . . H44B H 0.1298 -0.2302 0.0937 0.036 Uiso 1 1 calc R . . C45 C 0.03024(11) -0.14155(9) 0.14768(11) 0.0262(5) Uani 1 1 d . . . C46 C 0.05033(11) -0.19114(9) 0.11943(11) 0.0261(5) Uani 1 1 d . . . C47 C -0.00274(12) -0.22931(10) 0.07819(12) 0.0288(5) Uani 1 1 d . . . H47 H 0.0109 -0.2631 0.0590 0.035 Uiso 1 1 calc R . . C48 C -0.07583(11) -0.22050(9) 0.06336(12) 0.0267(5) Uani 1 1 d . . . C49 C -0.09275(12) -0.17135(9) 0.09411(11) 0.0271(5) Uani 1 1 d . . . H49 H -0.1416 -0.1646 0.0864 0.032 Uiso 1 1 calc R . . C50 C -0.04150(11) -0.13127(9) 0.13579(11) 0.0257(5) Uani 1 1 d . . . C51 C -0.13220(12) -0.26119(10) 0.01080(12) 0.0320(5) Uani 1 1 d . . . C52 C -0.13441(14) -0.25063(13) -0.06713(13) 0.0448(7) Uani 1 1 d . . . H52A H -0.1492 -0.2104 -0.0818 0.067 Uiso 1 1 calc R . . H52B H -0.1689 -0.2775 -0.1014 0.067 Uiso 1 1 calc R . . H52C H -0.0866 -0.2573 -0.0677 0.067 Uiso 1 1 calc R . . C53 C -0.20772(13) -0.25000(12) 0.00961(14) 0.0425(6) Uani 1 1 d . . . H53A H -0.2073 -0.2553 0.0590 0.064 Uiso 1 1 calc R . . H53B H -0.2416 -0.2775 -0.0240 0.064 Uiso 1 1 calc R . . H53C H -0.2224 -0.2101 -0.0069 0.064 Uiso 1 1 calc R . . C54 C -0.11237(15) -0.32476(11) 0.03150(15) 0.0435(6) Uani 1 1 d . . . H54A H -0.0655 -0.3331 0.0295 0.065 Uiso 1 1 calc R . . H54B H -0.1488 -0.3502 -0.0030 0.065 Uiso 1 1 calc R . . H54C H -0.1101 -0.3318 0.0812 0.065 Uiso 1 1 calc R . . C55 C -0.06532(12) -0.07560(10) 0.16102(12) 0.0302(5) Uani 1 1 d . . . H55A H -0.1076 -0.0837 0.1734 0.036 Uiso 1 1 calc R . . H55B H -0.0262 -0.0611 0.2057 0.036 Uiso 1 1 calc R . . C56 C -0.03518(11) 0.01180(9) 0.10001(12) 0.0277(5) Uani 1 1 d . . . C57 C -0.08439(12) -0.02944(9) 0.10206(12) 0.0277(5) Uani 1 1 d . . . C58 C -0.15218(12) -0.02956(10) 0.04537(13) 0.0327(5) Uani 1 1 d . . . H58 H -0.1863 -0.0579 0.0460 0.039 Uiso 1 1 calc R . . C59 C -0.17155(13) 0.01021(10) -0.01185(13) 0.0341(6) Uani 1 1 d . . . C60 C -0.12071(13) 0.05216(10) -0.00976(13) 0.0335(6) Uani 1 1 d . . . H60 H -0.1331 0.0803 -0.0478 0.040 Uiso 1 1 calc R . . C61 C -0.05279(12) 0.05448(9) 0.04549(12) 0.0287(5) Uani 1 1 d . . . C62 C -0.24489(14) 0.00851(11) -0.07629(15) 0.0470(7) Uani 1 1 d . . . C63 C -0.29275(19) -0.03933(16) -0.0681(2) 0.0932(14) Uani 1 1 d . . . H63A H -0.3031 -0.0322 -0.0242 0.140 Uiso 1 1 calc R . . H63B H -0.2684 -0.0769 -0.0634 0.140 Uiso 1 1 calc R . . H63C H -0.3378 -0.0399 -0.1113 0.140 Uiso 1 1 calc R . . C64 C -0.2316(2) -0.00266(18) -0.14794(19) 0.0834(12) Uani 1 1 d . . . H64A H -0.2774 -0.0007 -0.1902 0.125 Uiso 1 1 calc R . . H64B H -0.2103 -0.0413 -0.1457 0.125 Uiso 1 1 calc R . . H64C H -0.1989 0.0270 -0.1530 0.125 Uiso 1 1 calc R . . C65 C -0.28193(17) 0.06695(14) -0.0855(2) 0.0787(12) Uani 1 1 d . . . H65A H -0.2909 0.0761 -0.0413 0.118 Uiso 1 1 calc R . . H65B H -0.3276 0.0655 -0.1279 0.118 Uiso 1 1 calc R . . H65C H -0.2512 0.0971 -0.0934 0.118 Uiso 1 1 calc R . . C66 C 0.00024(12) 0.10130(10) 0.04578(12) 0.0307(5) Uani 1 1 d . . . H66A H -0.0144 0.1171 -0.0045 0.037 Uiso 1 1 calc R . . H66B H 0.0480 0.0830 0.0586 0.037 Uiso 1 1 calc R . . C67 C 0.06364(12) 0.15380(9) 0.16654(12) 0.0281(5) Uani 1 1 d . . . C68 C 0.00752(11) 0.15174(9) 0.09812(12) 0.0263(5) Uani 1 1 d . . . C69 C -0.03925(11) 0.19905(9) 0.07761(12) 0.0271(5) Uani 1 1 d . . . H69 H -0.0787 0.1976 0.0318 0.033 Uiso 1 1 calc R . . C70 C -0.03090(12) 0.24845(10) 0.12122(12) 0.0275(5) Uani 1 1 d . . . C71 C 0.02765(11) 0.24860(10) 0.18823(12) 0.0282(5) Uani 1 1 d . . . H71 H 0.0352 0.2818 0.2191 0.034 Uiso 1 1 calc R . . C72 C 0.07519(11) 0.20225(10) 0.21158(12) 0.0276(5) Uani 1 1 d . . . C73 C -0.07903(12) 0.30223(10) 0.09654(12) 0.0313(5) Uani 1 1 d . . . C74 C -0.04441(16) 0.34607(12) 0.06183(17) 0.0535(8) Uani 1 1 d . . . H74A H -0.0402 0.3287 0.0183 0.080 Uiso 1 1 calc R . . H74B H 0.0034 0.3564 0.0972 0.080 Uiso 1 1 calc R . . H74C H -0.0743 0.3812 0.0477 0.080 Uiso 1 1 calc R . . C75 C -0.08829(14) 0.33185(12) 0.16185(13) 0.0413(6) Uani 1 1 d . . . H75A H -0.1254 0.3620 0.1441 0.062 Uiso 1 1 calc R . . H75B H -0.0428 0.3497 0.1933 0.062 Uiso 1 1 calc R . . H75C H -0.1027 0.3028 0.1900 0.062 Uiso 1 1 calc R . . C76 C -0.15344(14) 0.28678(13) 0.04137(14) 0.0469(7) Uani 1 1 d . . . H76A H -0.1497 0.2724 -0.0038 0.070 Uiso 1 1 calc R . . H76B H -0.1840 0.3215 0.0304 0.070 Uiso 1 1 calc R . . H76C H -0.1745 0.2565 0.0619 0.070 Uiso 1 1 calc R . . C77 C 0.14044(11) 0.20776(10) 0.28210(12) 0.0294(5) Uani 1 1 d . . . H77A H 0.1550 0.1687 0.3039 0.035 Uiso 1 1 calc R . . H77B H 0.1283 0.2317 0.3174 0.035 Uiso 1 1 calc R . . C78 C 0.24992(11) 0.20287(9) 0.24766(11) 0.0274(5) Uani 1 1 d . . . C79 C 0.20255(11) 0.23569(10) 0.26850(11) 0.0276(5) Uani 1 1 d . . . C80 C 0.21095(12) 0.29572(10) 0.27210(12) 0.0290(5) Uani 1 1 d . . . H80 H 0.1791 0.3183 0.2866 0.035 Uiso 1 1 calc R . . C81 C 0.26391(12) 0.32456(10) 0.25547(12) 0.0303(5) Uani 1 1 d . . . C82 C 0.30986(12) 0.28969(10) 0.23513(12) 0.0291(5) Uani 1 1 d . . . H82 H 0.3468 0.3079 0.2240 0.035 Uiso 1 1 calc R . . C83 C 0.30370(11) 0.22946(10) 0.23053(11) 0.0276(5) Uani 1 1 d . . . C84 C 0.26689(14) 0.39110(11) 0.25716(15) 0.0402(6) Uani 1 1 d . . . C85 C 0.27752(15) 0.41293(12) 0.33418(16) 0.0507(7) Uani 1 1 d . . . H85A H 0.2800 0.4556 0.3352 0.076 Uiso 1 1 calc R . . H85B H 0.3223 0.3970 0.3699 0.076 Uiso 1 1 calc R . . H85C H 0.2371 0.4002 0.3465 0.076 Uiso 1 1 calc R . . C86 C 0.32871(18) 0.41451(12) 0.2376(2) 0.0664(9) Uani 1 1 d . . . H86A H 0.3217 0.4024 0.1877 0.100 Uiso 1 1 calc R . . H86B H 0.3744 0.3990 0.2721 0.100 Uiso 1 1 calc R . . H86C H 0.3295 0.4571 0.2403 0.100 Uiso 1 1 calc R . . C87 C 0.19619(16) 0.41470(12) 0.20131(17) 0.0543(8) Uani 1 1 d . . . H87A H 0.1880 0.3985 0.1529 0.081 Uiso 1 1 calc R . . H87B H 0.1987 0.4573 0.1995 0.081 Uiso 1 1 calc R . . H87C H 0.1566 0.4034 0.2158 0.081 Uiso 1 1 calc R . . C88 C 0.35413(12) 0.19373(10) 0.20618(12) 0.0295(5) Uani 1 1 d . . . H88A H 0.3306 0.1564 0.1854 0.035 Uiso 1 1 calc R . . H88B H 0.3631 0.2150 0.1669 0.035 Uiso 1 1 calc R . . N1 N 0.4802(4) -0.0297(4) 0.1688(6) 0.141(3) Uani 0.50 1 d PDU D 1 C89 C 0.5115(5) 0.0118(4) 0.2068(5) 0.094(2) Uani 0.50 1 d PDU D 1 C90 C 0.5491(3) 0.0558(2) 0.2506(3) 0.1147(16) Uani 1 1 d DU . . N1X N 0.5926(6) 0.0660(5) 0.1490(5) 0.143(3) Uani 0.50 1 d PDU D 2 C89X C 0.5672(5) 0.0595(4) 0.1923(5) 0.101(2) Uani 0.50 1 d PDU D 2 N2 N 0.5969(8) 0.0577(7) 0.0968(8) 0.209(5) Uani 0.50 1 d PDU E 1 C91 C 0.5536(12) 0.0260(9) 0.0523(11) 0.288(8) Uani 0.50 1 d PDU E 1 C92 C 0.5000 0.0000 0.0000 0.313(8) Uani 1 2 d SDU . 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 O1 0.0233(8) 0.0264(9) 0.0478(10) 0.0049(7) 0.0076(7) -0.0008(7) O2 0.0266(8) 0.0235(9) 0.0415(9) 0.0022(7) 0.0027(7) 0.0010(7) O3 0.0319(9) 0.0213(8) 0.0374(9) 0.0026(7) 0.0036(7) -0.0012(7) O4 0.0287(8) 0.0227(9) 0.0428(10) 0.0056(7) 0.0046(7) -0.0033(7) O5 0.0271(8) 0.0262(9) 0.0341(9) 0.0005(7) 0.0025(7) -0.0028(7) O6 0.0312(9) 0.0242(9) 0.0419(10) 0.0047(7) -0.0021(7) -0.0001(7) O7 0.0301(9) 0.0196(8) 0.0517(11) 0.0031(8) 0.0049(8) 0.0007(7) O8 0.0262(8) 0.0226(9) 0.0523(11) -0.0045(7) 0.0052(8) -0.0017(7) C1 0.0256(11) 0.0178(11) 0.0349(12) -0.0031(9) 0.0114(10) -0.0012(9) C2 0.0256(11) 0.0234(12) 0.0282(11) -0.0012(9) 0.0082(9) 0.0052(9) C3 0.0314(12) 0.0261(12) 0.0299(12) 0.0043(10) 0.0116(10) 0.0023(10) C4 0.0321(12) 0.0281(13) 0.0336(13) 0.0024(10) 0.0133(10) -0.0017(10) C5 0.0260(11) 0.0271(12) 0.0298(12) 0.0016(10) 0.0076(10) 0.0000(9) C6 0.0275(11) 0.0191(11) 0.0297(12) -0.0008(9) 0.0118(10) 0.0011(9) C7 0.0327(13) 0.0518(16) 0.0485(15) 0.0103(13) 0.0149(12) -0.0108(12) C8 0.059(2) 0.051(2) 0.060(2) 0.0032(16) 0.0168(18) -0.0272(16) C9 0.0451(19) 0.066(2) 0.065(2) 0.0092(17) 0.0325(17) -0.0107(16) C10 0.0324(18) 0.123(4) 0.065(2) 0.050(3) -0.0022(17) -0.027(2) C8X 0.041(9) 0.067(10) 0.068(6) 0.001(6) 0.032(7) -0.026(7) C9X 0.067(9) 0.060(9) 0.064(7) 0.012(6) 0.021(8) -0.022(7) C10X 0.034(7) 0.073(8) 0.072(9) 0.005(7) 0.022(7) -0.006(5) C11 0.0271(11) 0.0230(12) 0.0272(11) -0.0001(9) 0.0090(9) -0.0032(9) C12 0.0229(11) 0.0250(12) 0.0262(11) 0.0045(9) 0.0066(9) -0.0029(9) C13 0.0276(11) 0.0213(12) 0.0262(11) 0.0026(9) 0.0098(9) -0.0017(9) C14 0.0329(12) 0.0230(12) 0.0338(12) -0.0024(10) 0.0090(10) -0.0050(10) C15 0.0276(12) 0.0263(13) 0.0420(14) -0.0003(11) 0.0085(11) -0.0021(10) C16 0.0288(12) 0.0246(12) 0.0413(13) 0.0018(10) 0.0128(11) 0.0031(10) C17 0.0295(12) 0.0218(12) 0.0304(12) 0.0006(9) 0.0116(10) -0.0037(9) C18 0.0286(13) 0.0425(15) 0.0538(16) -0.0031(12) 0.0005(12) 0.0022(11) C19 0.030(2) 0.062(3) 0.048(3) 0.008(2) 0.0084(19) 0.016(2) C20 0.045(3) 0.063(3) 0.105(5) -0.044(3) -0.024(3) 0.014(3) C21 0.027(2) 0.069(4) 0.091(3) 0.016(3) 0.017(2) -0.001(2) C19X 0.041(6) 0.077(5) 0.108(9) -0.038(6) -0.011(6) 0.025(4) C20X 0.024(4) 0.048(5) 0.054(4) -0.003(4) -0.006(3) 0.002(3) C21X 0.044(5) 0.096(6) 0.081(6) -0.009(5) 0.017(4) -0.028(4) C22 0.0302(12) 0.0247(12) 0.0327(12) -0.0020(10) 0.0108(10) -0.0022(9) C23 0.0265(11) 0.0216(12) 0.0235(11) -0.0031(9) 0.0013(9) -0.0012(9) C24 0.0286(12) 0.0207(11) 0.0256(11) -0.0038(9) 0.0076(9) -0.0026(9) C25 0.0219(11) 0.0296(13) 0.0297(12) -0.0046(10) 0.0054(9) -0.0004(9) C26 0.0298(12) 0.0263(12) 0.0264(12) -0.0028(10) 0.0055(10) -0.0001(10) C27 0.0311(12) 0.0258(12) 0.0249(11) 0.0004(9) 0.0066(10) -0.0019(10) C28 0.0247(11) 0.0237(12) 0.0224(11) -0.0036(9) 0.0031(9) -0.0031(9) C29 0.0316(13) 0.0340(14) 0.0382(13) 0.0066(11) 0.0113(11) 0.0092(10) C30 0.0549(18) 0.072(2) 0.074(2) 0.0455(18) 0.0301(17) 0.0282(16) C31 0.0489(18) 0.063(2) 0.0549(19) 0.0126(15) -0.0009(15) 0.0101(15) C32 0.104(3) 0.054(2) 0.0528(18) 0.0101(15) 0.0311(19) 0.0418(19) C33 0.0261(11) 0.0277(12) 0.0252(11) 0.0004(9) 0.0065(9) 0.0017(9) C34 0.0255(11) 0.0205(12) 0.0319(12) 0.0003(9) 0.0119(10) -0.0005(9) C35 0.0238(11) 0.0245(12) 0.0266(11) 0.0005(9) 0.0088(9) 0.0012(9) C36 0.0334(12) 0.0286(13) 0.0311(12) 0.0052(10) 0.0120(10) 0.0027(10) C37 0.0392(14) 0.0238(13) 0.0404(14) -0.0001(10) 0.0152(11) -0.0001(10) C38 0.0321(12) 0.0248(13) 0.0352(13) -0.0070(10) 0.0111(10) -0.0037(10) C39 0.0252(11) 0.0277(12) 0.0266(11) -0.0017(9) 0.0092(9) 0.0013(9) C40 0.0673(18) 0.0239(14) 0.0623(17) 0.0028(12) 0.0228(15) -0.0036(12) C41 0.113(3) 0.041(2) 0.072(2) 0.0252(18) 0.019(2) -0.015(2) C42 0.120(4) 0.0232(18) 0.106(3) -0.0060(19) 0.055(3) 0.010(2) C43 0.072(2) 0.044(2) 0.085(3) 0.0001(19) 0.032(2) -0.0242(18) C41X 0.087(7) 0.037(9) 0.106(11) 0.018(9) 0.024(6) 0.012(8) C42X 0.103(10) 0.040(10) 0.086(8) -0.012(8) 0.018(7) -0.015(9) C43X 0.092(9) 0.045(9) 0.074(8) 0.032(8) 0.035(7) -0.015(9) C44 0.0283(12) 0.0310(13) 0.0272(12) -0.0025(10) 0.0074(10) -0.0021(10) C45 0.0293(12) 0.0212(12) 0.0227(11) 0.0017(9) 0.0037(9) -0.0037(9) C46 0.0264(11) 0.0255(12) 0.0214(11) 0.0032(9) 0.0033(9) -0.0006(9) C47 0.0314(12) 0.0260(12) 0.0255(11) -0.0005(9) 0.0070(10) 0.0014(10) C48 0.0274(12) 0.0237(12) 0.0249(11) 0.0049(9) 0.0055(9) -0.0011(9) C49 0.0247(11) 0.0268(12) 0.0263(11) 0.0051(9) 0.0059(9) -0.0013(9) C50 0.0289(12) 0.0230(12) 0.0234(11) 0.0050(9) 0.0078(9) 0.0008(9) C51 0.0274(12) 0.0361(14) 0.0275(12) -0.0032(10) 0.0050(10) -0.0077(10) C52 0.0404(15) 0.0565(18) 0.0317(13) -0.0050(12) 0.0072(12) -0.0157(13) C53 0.0347(14) 0.0472(16) 0.0401(14) -0.0070(12) 0.0082(11) -0.0112(12) C54 0.0483(16) 0.0331(15) 0.0470(15) -0.0082(12) 0.0159(13) -0.0126(12) C55 0.0320(12) 0.0273(13) 0.0322(12) -0.0018(10) 0.0133(10) -0.0020(10) C56 0.0268(12) 0.0211(12) 0.0290(12) -0.0032(9) 0.0037(10) -0.0004(9) C57 0.0304(12) 0.0209(12) 0.0308(12) -0.0027(9) 0.0105(10) 0.0003(9) C58 0.0294(12) 0.0230(12) 0.0427(14) -0.0034(10) 0.0103(11) -0.0007(10) C59 0.0328(13) 0.0215(12) 0.0375(13) -0.0035(10) 0.0017(11) 0.0009(10) C60 0.0385(14) 0.0211(12) 0.0330(13) -0.0012(10) 0.0047(11) 0.0005(10) C61 0.0317(12) 0.0194(12) 0.0314(12) -0.0013(9) 0.0080(10) 0.0008(9) C62 0.0355(14) 0.0309(15) 0.0542(17) -0.0012(12) -0.0057(12) -0.0027(11) C63 0.051(2) 0.073(3) 0.107(3) 0.027(2) -0.024(2) -0.0233(18) C64 0.066(2) 0.099(3) 0.056(2) -0.024(2) -0.0097(17) -0.001(2) C65 0.0435(18) 0.056(2) 0.097(3) -0.0030(19) -0.0173(17) 0.0114(15) C66 0.0348(13) 0.0243(12) 0.0298(12) 0.0028(10) 0.0089(10) -0.0014(10) C67 0.0268(11) 0.0209(12) 0.0359(13) 0.0044(10) 0.0112(10) -0.0024(9) C68 0.0267(11) 0.0218(12) 0.0302(12) 0.0019(9) 0.0105(10) -0.0040(9) C69 0.0241(11) 0.0273(12) 0.0262(11) 0.0031(9) 0.0055(9) -0.0032(9) C70 0.0268(11) 0.0254(12) 0.0301(12) -0.0005(9) 0.0106(10) -0.0017(9) C71 0.0253(11) 0.0282(13) 0.0294(12) -0.0046(10) 0.0085(10) -0.0015(9) C72 0.0238(11) 0.0288(12) 0.0287(12) 0.0030(10) 0.0083(9) -0.0035(9) C73 0.0285(12) 0.0318(13) 0.0332(13) 0.0016(10) 0.0110(10) 0.0059(10) C74 0.0600(18) 0.0406(17) 0.073(2) 0.0211(15) 0.0405(16) 0.0163(14) C75 0.0361(14) 0.0454(16) 0.0388(14) -0.0062(12) 0.0101(11) 0.0096(12) C76 0.0380(15) 0.0537(18) 0.0386(14) -0.0076(13) 0.0029(12) 0.0164(13) C77 0.0294(12) 0.0290(13) 0.0267(12) 0.0021(10) 0.0073(10) 0.0020(10) C78 0.0256(11) 0.0218(12) 0.0268(12) -0.0007(9) 0.0009(9) 0.0015(9) C79 0.0258(11) 0.0279(13) 0.0222(11) -0.0010(9) 0.0016(9) 0.0002(9) C80 0.0293(12) 0.0261(12) 0.0276(12) -0.0019(9) 0.0066(10) 0.0057(10) C81 0.0309(12) 0.0239(12) 0.0313(12) -0.0025(10) 0.0064(10) -0.0005(10) C82 0.0279(12) 0.0258(13) 0.0307(12) 0.0013(10) 0.0079(10) 0.0000(9) C83 0.0239(11) 0.0294(13) 0.0229(11) -0.0008(9) 0.0016(9) 0.0031(9) C84 0.0417(14) 0.0245(13) 0.0545(16) -0.0025(11) 0.0183(13) 0.0000(11) C85 0.0479(16) 0.0310(15) 0.0646(19) -0.0152(13) 0.0118(14) -0.0013(12) C86 0.075(2) 0.0267(15) 0.113(3) 0.0031(16) 0.054(2) -0.0051(14) C87 0.0628(19) 0.0283(15) 0.0618(19) 0.0039(13) 0.0128(15) 0.0101(13) C88 0.0293(12) 0.0276(13) 0.0291(12) -0.0008(10) 0.0082(10) 0.0024(10) N1 0.072(5) 0.138(7) 0.171(8) 0.065(5) -0.002(5) -0.011(5) C89 0.113(6) 0.083(5) 0.110(5) 0.044(3) 0.072(4) 0.035(4) C90 0.191(5) 0.084(3) 0.115(3) 0.008(2) 0.111(3) 0.029(3) N1X 0.179(8) 0.189(8) 0.083(6) -0.009(6) 0.074(5) -0.011(7) C89X 0.140(6) 0.090(5) 0.100(5) 0.024(4) 0.074(4) 0.036(4) N2 0.237(12) 0.222(12) 0.157(11) -0.009(9) 0.063(9) -0.009(9) C91 0.347(18) 0.200(13) 0.214(15) -0.050(10) -0.008(12) 0.025(11) C92 0.386(19) 0.192(12) 0.232(15) -0.083(9) -0.026(12) 0.034(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.381(3) . ? O2 C12 1.390(2) . ? O3 C23 1.386(3) . ? O4 C34 1.391(3) . ? O5 C45 1.391(2) . ? O6 C56 1.390(3) . ? O7 C67 1.385(3) . ? O8 C78 1.377(3) . ? C1 C6 1.390(3) . ? C1 C2 1.402(3) . ? C2 C3 1.388(3) . ? C2 C88 1.515(3) . ? C3 C4 1.393(3) . ? C4 C5 1.394(3) . ? C4 C7 1.533(3) . ? C5 C6 1.389(3) . ? C6 C11 1.524(3) . ? C7 C10 1.488(4) . ? C7 C9X 1.510(10) . ? C7 C8 1.538(4) . ? C7 C9 1.551(4) . ? C7 C10X 1.557(8) . ? C7 C8X 1.586(8) . ? C11 C13 1.513(3) . ? C12 C13 1.388(3) . ? C12 C17 1.396(3) . ? C13 C14 1.387(3) . ? C14 C15 1.396(3) . ? C15 C16 1.392(3) . ? C15 C18 1.525(3) . ? C16 C17 1.392(3) . ? C17 C22 1.517(3) . ? C18 C19X 1.470(6) . ? C18 C20 1.474(5) . ? C18 C19 1.544(5) . ? C18 C21X 1.546(6) . ? C18 C21 1.580(5) . ? C18 C20X 1.603(7) . ? C22 C24 1.515(3) . ? C23 C28 1.393(3) . ? C23 C24 1.398(3) . ? C24 C25 1.388(3) . ? C25 C26 1.393(3) . ? C26 C27 1.398(3) . ? C26 C29 1.532(3) . ? C27 C28 1.391(3) . ? C28 C33 1.506(3) . ? C29 C32 1.511(4) . ? C29 C30 1.523(4) . ? C29 C31 1.540(4) . ? C33 C35 1.519(3) . ? C34 C35 1.387(3) . ? C34 C39 1.392(3) . ? C35 C36 1.385(3) . ? C36 C37 1.391(3) . ? C37 C38 1.387(3) . ? C37 C40 1.533(3) . ? C38 C39 1.385(3) . ? C39 C44 1.515(3) . ? C40 C42X 1.501(10) . ? C40 C42 1.508(5) . ? C40 C41 1.520(4) . ? C40 C43X 1.526(8) . ? C40 C41X 1.559(8) . ? C40 C43 1.564(4) . ? C44 C46 1.514(3) . ? C45 C50 1.394(3) . ? C45 C46 1.394(3) . ? C46 C47 1.382(3) . ? C47 C48 1.403(3) . ? C48 C49 1.384(3) . ? C48 C51 1.530(3) . ? C49 C50 1.394(3) . ? C50 C55 1.515(3) . ? C51 C54 1.527(3) . ? C51 C53 1.535(3) . ? C51 C52 1.542(3) . ? C55 C57 1.512(3) . ? C56 C57 1.383(3) . ? C56 C61 1.398(3) . ? C57 C58 1.397(3) . ? C58 C59 1.388(3) . ? C59 C60 1.395(3) . ? C59 C62 1.539(3) . ? C60 C61 1.388(3) . ? C61 C66 1.514(3) . ? C62 C63 1.511(4) . ? C62 C65 1.512(4) . ? C62 C64 1.559(5) . ? C66 C68 1.522(3) . ? C67 C72 1.387(3) . ? C67 C68 1.393(3) . ? C68 C69 1.393(3) . ? C69 C70 1.395(3) . ? C70 C71 1.397(3) . ? C70 C73 1.530(3) . ? C71 C72 1.387(3) . ? C72 C77 1.512(3) . ? C73 C76 1.521(3) . ? C73 C74 1.528(3) . ? C73 C75 1.532(3) . ? C77 C79 1.519(3) . ? C78 C83 1.394(3) . ? C78 C79 1.396(3) . ? C79 C80 1.387(3) . ? C80 C81 1.398(3) . ? C81 C82 1.394(3) . ? C81 C84 1.529(3) . ? C82 C83 1.388(3) . ? C83 C88 1.520(3) . ? C84 C87 1.530(4) . ? C84 C86 1.536(4) . ? C84 C85 1.537(4) . ? N1 C89 1.228(11) . ? C89 C90 1.356(10) . ? C90 C89X 1.337(8) . ? N1X C89X 1.161(10) . ? N2 C91 1.216(13) . ? C91 C92 1.318(14) . ? C92 C91 1.318(14) 3_655 ? 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 O1 C1 C6 117.15(19) . . ? O1 C1 C2 122.08(19) . . ? C6 C1 C2 120.76(19) . . ? C3 C2 C1 118.0(2) . . ? C3 C2 C88 120.4(2) . . ? C1 C2 C88 121.65(19) . . ? C2 C3 C4 123.1(2) . . ? C3 C4 C5 116.7(2) . . ? C3 C4 C7 119.9(2) . . ? C5 C4 C7 123.3(2) . . ? C6 C5 C4 122.4(2) . . ? C5 C6 C1 118.8(2) . . ? C5 C6 C11 120.23(19) . . ? C1 C6 C11 120.92(19) . . ? C10 C7 C4 113.2(2) . . ? C9X C7 C4 125.9(8) . . ? C10 C7 C8 110.5(3) . . ? C4 C7 C8 109.1(2) . . ? C10 C7 C9 109.5(3) . . ? C4 C7 C9 107.7(2) . . ? C8 C7 C9 106.5(2) . . ? C9X C7 C10X 108.7(9) . . ? C4 C7 C10X 108.3(7) . . ? C9X C7 C8X 105.3(8) . . ? C4 C7 C8X 105.7(6) . . ? C10X C7 C8X 99.7(9) . . ? C13 C11 C6 111.89(17) . . ? C13 C12 O2 120.92(19) . . ? C13 C12 C17 121.34(19) . . ? O2 C12 C17 117.73(19) . . ? C14 C13 C12 118.2(2) . . ? C14 C13 C11 120.01(19) . . ? C12 C13 C11 121.73(19) . . ? C13 C14 C15 123.2(2) . . ? C16 C15 C14 116.1(2) . . ? C16 C15 C18 121.5(2) . . ? C14 C15 C18 122.4(2) . . ? C17 C16 C15 123.2(2) . . ? C16 C17 C12 117.9(2) . . ? C16 C17 C22 120.2(2) . . ? C12 C17 C22 121.84(19) . . ? C19X C18 C15 116.6(4) . . ? C20 C18 C15 115.4(3) . . ? C20 C18 C19 111.6(4) . . ? C15 C18 C19 109.3(3) . . ? C19X C18 C21X 117.2(7) . . ? C15 C18 C21X 106.2(4) . . ? C20 C18 C21 108.0(4) . . ? C15 C18 C21 107.4(2) . . ? C19 C18 C21 104.6(3) . . ? C19X C18 C20X 107.9(6) . . ? C15 C18 C20X 106.3(3) . . ? C21X C18 C20X 101.2(5) . . ? C24 C22 C17 111.34(18) . . ? O3 C23 C28 118.28(19) . . ? O3 C23 C24 120.54(19) . . ? C28 C23 C24 121.2(2) . . ? C25 C24 C23 117.8(2) . . ? C25 C24 C22 119.93(19) . . ? C23 C24 C22 122.12(19) . . ? C24 C25 C26 123.6(2) . . ? C25 C26 C27 116.1(2) . . ? C25 C26 C29 120.7(2) . . ? C27 C26 C29 123.2(2) . . ? C28 C27 C26 122.8(2) . . ? C27 C28 C23 118.4(2) . . ? C27 C28 C33 120.0(2) . . ? C23 C28 C33 121.57(19) . . ? C32 C29 C30 110.1(3) . . ? C32 C29 C26 109.8(2) . . ? C30 C29 C26 111.8(2) . . ? C32 C29 C31 109.7(3) . . ? C30 C29 C31 106.4(2) . . ? C26 C29 C31 109.1(2) . . ? C28 C33 C35 113.76(18) . . ? C35 C34 O4 121.33(19) . . ? C35 C34 C39 121.1(2) . . ? O4 C34 C39 117.57(19) . . ? C36 C35 C34 118.3(2) . . ? C36 C35 C33 119.80(19) . . ? C34 C35 C33 121.88(19) . . ? C35 C36 C37 122.9(2) . . ? C38 C37 C36 116.6(2) . . ? C38 C37 C40 120.1(2) . . ? C36 C37 C40 123.3(2) . . ? C39 C38 C37 122.9(2) . . ? C38 C39 C34 118.3(2) . . ? C38 C39 C44 119.8(2) . . ? C34 C39 C44 121.9(2) . . ? C42 C40 C41 111.4(3) . . ? C42X C40 C43X 113.6(10) . . ? C42X C40 C37 113.1(11) . . ? C42 C40 C37 109.1(3) . . ? C41 C40 C37 112.5(2) . . ? C43X C40 C37 108.3(9) . . ? C42X C40 C41X 110.3(10) . . ? C43X C40 C41X 107.4(11) . . ? C37 C40 C41X 103.5(10) . . ? C42 C40 C43 108.7(3) . . ? C41 C40 C43 106.4(3) . . ? C37 C40 C43 108.6(2) . . ? C46 C44 C39 113.12(18) . . ? O5 C45 C50 118.26(19) . . ? O5 C45 C46 120.91(19) . . ? C50 C45 C46 120.79(19) . . ? C47 C46 C45 118.4(2) . . ? C47 C46 C44 120.0(2) . . ? C45 C46 C44 121.54(19) . . ? C46 C47 C48 123.1(2) . . ? C49 C48 C47 116.2(2) . . ? C49 C48 C51 123.5(2) . . ? C47 C48 C51 120.1(2) . . ? C48 C49 C50 123.1(2) . . ? C49 C50 C45 118.4(2) . . ? C49 C50 C55 119.65(19) . . ? C45 C50 C55 121.74(19) . . ? C54 C51 C48 110.56(19) . . ? C54 C51 C53 108.7(2) . . ? C48 C51 C53 112.5(2) . . ? C54 C51 C52 108.8(2) . . ? C48 C51 C52 108.19(19) . . ? C53 C51 C52 107.9(2) . . ? C57 C55 C50 110.92(18) . . ? C57 C56 O6 119.77(19) . . ? C57 C56 C61 121.9(2) . . ? O6 C56 C61 118.32(19) . . ? C56 C57 C58 118.1(2) . . ? C56 C57 C55 121.9(2) . . ? C58 C57 C55 120.0(2) . . ? C59 C58 C57 122.4(2) . . ? C58 C59 C60 117.1(2) . . ? C58 C59 C62 122.6(2) . . ? C60 C59 C62 120.3(2) . . ? C61 C60 C59 122.9(2) . . ? C60 C61 C56 117.6(2) . . ? C60 C61 C66 120.9(2) . . ? C56 C61 C66 121.57(19) . . ? C63 C62 C65 110.6(3) . . ? C63 C62 C59 112.4(2) . . ? C65 C62 C59 110.6(2) . . ? C63 C62 C64 108.4(3) . . ? C65 C62 C64 106.5(3) . . ? C59 C62 C64 108.1(2) . . ? C61 C66 C68 115.30(19) . . ? O7 C67 C72 118.11(19) . . ? O7 C67 C68 120.2(2) . . ? C72 C67 C68 121.6(2) . . ? C69 C68 C67 117.7(2) . . ? C69 C68 C66 121.12(19) . . ? C67 C68 C66 121.13(19) . . ? C68 C69 C70 123.1(2) . . ? C69 C70 C71 116.5(2) . . ? C69 C70 C73 123.2(2) . . ? C71 C70 C73 120.2(2) . . ? C72 C71 C70 122.6(2) . . ? C67 C72 C71 118.4(2) . . ? C67 C72 C77 122.1(2) . . ? C71 C72 C77 119.3(2) . . ? C76 C73 C74 109.0(2) . . ? C76 C73 C70 111.8(2) . . ? C74 C73 C70 109.37(19) . . ? C76 C73 C75 107.64(19) . . ? C74 C73 C75 108.0(2) . . ? C70 C73 C75 110.87(19) . . ? C72 C77 C79 110.97(18) . . ? O8 C78 C83 117.73(19) . . ? O8 C78 C79 121.1(2) . . ? C83 C78 C79 121.2(2) . . ? C80 C79 C78 117.9(2) . . ? C80 C79 C77 120.2(2) . . ? C78 C79 C77 121.8(2) . . ? C79 C80 C81 123.2(2) . . ? C82 C81 C80 116.5(2) . . ? C82 C81 C84 123.7(2) . . ? C80 C81 C84 119.7(2) . . ? C83 C82 C81 122.6(2) . . ? C82 C83 C78 118.6(2) . . ? C82 C83 C88 120.3(2) . . ? C78 C83 C88 121.1(2) . . ? C81 C84 C87 108.7(2) . . ? C81 C84 C86 111.9(2) . . ? C87 C84 C86 108.4(2) . . ? C81 C84 C85 109.7(2) . . ? C87 C84 C85 109.7(2) . . ? C86 C84 C85 108.4(2) . . ? C2 C88 C83 112.92(18) . . ? N1 C89 C90 177.0(10) . . ? N1X C89X C90 169.8(12) . . ? N2 C91 C92 170(2) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 C3 -174.1(2) . . . . ? C6 C1 C2 C3 4.7(3) . . . . ? O1 C1 C2 C88 8.2(3) . . . . ? C6 C1 C2 C88 -173.00(19) . . . . ? C1 C2 C3 C4 -0.6(3) . . . . ? C88 C2 C3 C4 177.1(2) . . . . ? C2 C3 C4 C5 -3.2(3) . . . . ? C2 C3 C4 C7 175.1(2) . . . . ? C3 C4 C5 C6 3.2(3) . . . . ? C7 C4 C5 C6 -175.0(2) . . . . ? C4 C5 C6 C1 0.7(3) . . . . ? C4 C5 C6 C11 -179.6(2) . . . . ? O1 C1 C6 C5 174.09(19) . . . . ? C2 C1 C6 C5 -4.8(3) . . . . ? O1 C1 C6 C11 -5.6(3) . . . . ? C2 C1 C6 C11 175.55(19) . . . . ? C3 C4 C7 C10 179.9(3) . . . . ? C5 C4 C7 C10 -2.0(4) . . . . ? C3 C4 C7 C9X 3.0(10) . . . . ? C5 C4 C7 C9X -178.9(10) . . . . ? C3 C4 C7 C8 56.4(3) . . . . ? C5 C4 C7 C8 -125.5(3) . . . . ? C3 C4 C7 C9 -58.9(3) . . . . ? C5 C4 C7 C9 119.2(3) . . . . ? C3 C4 C7 C10X -128.0(9) . . . . ? C5 C4 C7 C10X 50.1(9) . . . . ? C3 C4 C7 C8X 125.8(8) . . . . ? C5 C4 C7 C8X -56.0(8) . . . . ? C5 C6 C11 C13 -74.7(3) . . . . ? C1 C6 C11 C13 105.0(2) . . . . ? O2 C12 C13 C14 179.2(2) . . . . ? C17 C12 C13 C14 -1.9(3) . . . . ? O2 C12 C13 C11 -2.7(3) . . . . ? C17 C12 C13 C11 176.16(19) . . . . ? C6 C11 C13 C14 100.8(2) . . . . ? C6 C11 C13 C12 -77.2(2) . . . . ? C12 C13 C14 C15 1.4(3) . . . . ? C11 C13 C14 C15 -176.8(2) . . . . ? C13 C14 C15 C16 -0.1(3) . . . . ? C13 C14 C15 C18 178.3(2) . . . . ? C14 C15 C16 C17 -0.7(3) . . . . ? C18 C15 C16 C17 -179.1(2) . . . . ? C15 C16 C17 C12 0.1(3) . . . . ? C15 C16 C17 C22 -177.2(2) . . . . ? C13 C12 C17 C16 1.2(3) . . . . ? O2 C12 C17 C16 -179.90(19) . . . . ? C13 C12 C17 C22 178.50(19) . . . . ? O2 C12 C17 C22 -2.6(3) . . . . ? C16 C15 C18 C19X -13.4(8) . . . . ? C14 C15 C18 C19X 168.3(7) . . . . ? C16 C15 C18 C20 -177.2(4) . . . . ? C14 C15 C18 C20 4.5(5) . . . . ? C16 C15 C18 C19 -50.5(4) . . . . ? C14 C15 C18 C19 131.1(3) . . . . ? C16 C15 C18 C21X 119.2(5) . . . . ? C14 C15 C18 C21X -59.1(5) . . . . ? C16 C15 C18 C21 62.4(3) . . . . ? C14 C15 C18 C21 -116.0(3) . . . . ? C16 C15 C18 C20X -133.6(4) . . . . ? C14 C15 C18 C20X 48.0(5) . . . . ? C16 C17 C22 C24 88.3(2) . . . . ? C12 C17 C22 C24 -88.9(2) . . . . ? O3 C23 C24 C25 179.82(19) . . . . ? C28 C23 C24 C25 0.6(3) . . . . ? O3 C23 C24 C22 3.6(3) . . . . ? C28 C23 C24 C22 -175.60(19) . . . . ? C17 C22 C24 C25 -84.2(2) . . . . ? C17 C22 C24 C23 91.9(2) . . . . ? C23 C24 C25 C26 -1.1(3) . . . . ? C22 C24 C25 C26 175.2(2) . . . . ? C24 C25 C26 C27 1.4(3) . . . . ? C24 C25 C26 C29 -178.2(2) . . . . ? C25 C26 C27 C28 -1.3(3) . . . . ? C29 C26 C27 C28 178.4(2) . . . . ? C26 C27 C28 C23 0.8(3) . . . . ? C26 C27 C28 C33 -179.3(2) . . . . ? O3 C23 C28 C27 -179.73(18) . . . . ? C24 C23 C28 C27 -0.5(3) . . . . ? O3 C23 C28 C33 0.4(3) . . . . ? C24 C23 C28 C33 179.68(19) . . . . ? C25 C26 C29 C32 -67.2(3) . . . . ? C27 C26 C29 C32 113.1(3) . . . . ? C25 C26 C29 C30 170.3(2) . . . . ? C27 C26 C29 C30 -9.3(3) . . . . ? C25 C26 C29 C31 52.9(3) . . . . ? C27 C26 C29 C31 -126.7(3) . . . . ? C27 C28 C33 C35 -90.7(2) . . . . ? C23 C28 C33 C35 89.1(2) . . . . ? O4 C34 C35 C36 176.77(19) . . . . ? C39 C34 C35 C36 -0.6(3) . . . . ? O4 C34 C35 C33 -2.1(3) . . . . ? C39 C34 C35 C33 -179.46(19) . . . . ? C28 C33 C35 C36 87.7(2) . . . . ? C28 C33 C35 C34 -93.5(2) . . . . ? C34 C35 C36 C37 -1.0(3) . . . . ? C33 C35 C36 C37 177.9(2) . . . . ? C35 C36 C37 C38 2.0(3) . . . . ? C35 C36 C37 C40 -176.8(2) . . . . ? C36 C37 C38 C39 -1.4(3) . . . . ? C40 C37 C38 C39 177.4(2) . . . . ? C37 C38 C39 C34 -0.1(3) . . . . ? C37 C38 C39 C44 -178.4(2) . . . . ? C35 C34 C39 C38 1.1(3) . . . . ? O4 C34 C39 C38 -176.34(19) . . . . ? C35 C34 C39 C44 179.37(19) . . . . ? O4 C34 C39 C44 1.9(3) . . . . ? C38 C37 C40 C42X 9.3(12) . . . . ? C36 C37 C40 C42X -172.0(11) . . . . ? C38 C37 C40 C42 63.8(3) . . . . ? C36 C37 C40 C42 -117.5(3) . . . . ? C38 C37 C40 C41 -172.1(3) . . . . ? C36 C37 C40 C41 6.6(4) . . . . ? C38 C37 C40 C43X -117.5(11) . . . . ? C36 C37 C40 C43X 61.2(11) . . . . ? C38 C37 C40 C41X 128.7(11) . . . . ? C36 C37 C40 C41X -52.6(11) . . . . ? C38 C37 C40 C43 -54.5(3) . . . . ? C36 C37 C40 C43 124.2(3) . . . . ? C38 C39 C44 C46 75.6(3) . . . . ? C34 C39 C44 C46 -102.6(2) . . . . ? O5 C45 C46 C47 -176.38(19) . . . . ? C50 C45 C46 C47 1.2(3) . . . . ? O5 C45 C46 C44 2.7(3) . . . . ? C50 C45 C46 C44 -179.7(2) . . . . ? C39 C44 C46 C47 -100.5(2) . . . . ? C39 C44 C46 C45 80.4(3) . . . . ? C45 C46 C47 C48 0.1(3) . . . . ? C44 C46 C47 C48 -179.0(2) . . . . ? C46 C47 C48 C49 -1.5(3) . . . . ? C46 C47 C48 C51 173.6(2) . . . . ? C47 C48 C49 C50 1.9(3) . . . . ? C51 C48 C49 C50 -173.1(2) . . . . ? C48 C49 C50 C45 -0.7(3) . . . . ? C48 C49 C50 C55 173.88(19) . . . . ? O5 C45 C50 C49 176.75(18) . . . . ? C46 C45 C50 C49 -0.9(3) . . . . ? O5 C45 C50 C55 2.3(3) . . . . ? C46 C45 C50 C55 -175.36(19) . . . . ? C49 C48 C51 C54 -134.9(2) . . . . ? C47 C48 C51 C54 50.3(3) . . . . ? C49 C48 C51 C53 -13.1(3) . . . . ? C47 C48 C51 C53 172.1(2) . . . . ? C49 C48 C51 C52 106.1(3) . . . . ? C47 C48 C51 C52 -68.7(3) . . . . ? C49 C50 C55 C57 -84.2(2) . . . . ? C45 C50 C55 C57 90.2(2) . . . . ? O6 C56 C57 C58 -177.07(19) . . . . ? C61 C56 C57 C58 3.4(3) . . . . ? O6 C56 C57 C55 -0.5(3) . . . . ? C61 C56 C57 C55 180.0(2) . . . . ? C50 C55 C57 C56 -94.2(2) . . . . ? C50 C55 C57 C58 82.3(3) . . . . ? C56 C57 C58 C59 -0.5(3) . . . . ? C55 C57 C58 C59 -177.2(2) . . . . ? C57 C58 C59 C60 -1.7(3) . . . . ? C57 C58 C59 C62 177.1(2) . . . . ? C58 C59 C60 C61 1.3(4) . . . . ? C62 C59 C60 C61 -177.6(2) . . . . ? C59 C60 C61 C56 1.4(3) . . . . ? C59 C60 C61 C66 -179.3(2) . . . . ? C57 C56 C61 C60 -3.8(3) . . . . ? O6 C56 C61 C60 176.7(2) . . . . ? C57 C56 C61 C66 176.9(2) . . . . ? O6 C56 C61 C66 -2.7(3) . . . . ? C58 C59 C62 C63 2.0(4) . . . . ? C60 C59 C62 C63 -179.2(3) . . . . ? C58 C59 C62 C65 126.1(3) . . . . ? C60 C59 C62 C65 -55.1(4) . . . . ? C58 C59 C62 C64 -117.6(3) . . . . ? C60 C59 C62 C64 61.2(3) . . . . ? C60 C61 C66 C68 101.5(2) . . . . ? C56 C61 C66 C68 -79.2(3) . . . . ? O7 C67 C68 C69 179.2(2) . . . . ? C72 C67 C68 C69 -3.1(3) . . . . ? O7 C67 C68 C66 -4.4(3) . . . . ? C72 C67 C68 C66 173.2(2) . . . . ? C61 C66 C68 C69 -85.1(3) . . . . ? C61 C66 C68 C67 98.7(2) . . . . ? C67 C68 C69 C70 2.1(3) . . . . ? C66 C68 C69 C70 -174.3(2) . . . . ? C68 C69 C70 C71 -0.2(3) . . . . ? C68 C69 C70 C73 175.6(2) . . . . ? C69 C70 C71 C72 -0.7(3) . . . . ? C73 C70 C71 C72 -176.6(2) . . . . ? O7 C67 C72 C71 180.0(2) . . . . ? C68 C67 C72 C71 2.3(3) . . . . ? O7 C67 C72 C77 4.5(3) . . . . ? C68 C67 C72 C77 -173.2(2) . . . . ? C70 C71 C72 C67 -0.4(3) . . . . ? C70 C71 C72 C77 175.3(2) . . . . ? C69 C70 C73 C76 27.6(3) . . . . ? C71 C70 C73 C76 -156.8(2) . . . . ? C69 C70 C73 C74 -93.3(3) . . . . ? C71 C70 C73 C74 82.4(3) . . . . ? C69 C70 C73 C75 147.7(2) . . . . ? C71 C70 C73 C75 -36.6(3) . . . . ? C67 C72 C77 C79 88.7(3) . . . . ? C71 C72 C77 C79 -86.7(2) . . . . ? O8 C78 C79 C80 179.68(19) . . . . ? C83 C78 C79 C80 -0.4(3) . . . . ? O8 C78 C79 C77 -4.3(3) . . . . ? C83 C78 C79 C77 175.59(19) . . . . ? C72 C77 C79 C80 89.7(2) . . . . ? C72 C77 C79 C78 -86.2(2) . . . . ? C78 C79 C80 C81 0.5(3) . . . . ? C77 C79 C80 C81 -175.6(2) . . . . ? C79 C80 C81 C82 -0.6(3) . . . . ? C79 C80 C81 C84 176.9(2) . . . . ? C80 C81 C82 C83 0.7(3) . . . . ? C84 C81 C82 C83 -176.7(2) . . . . ? C81 C82 C83 C78 -0.7(3) . . . . ? C81 C82 C83 C88 178.4(2) . . . . ? O8 C78 C83 C82 -179.57(18) . . . . ? C79 C78 C83 C82 0.5(3) . . . . ? O8 C78 C83 C88 1.3(3) . . . . ? C79 C78 C83 C88 -178.59(19) . . . . ? C82 C81 C84 C87 116.9(3) . . . . ? C80 C81 C84 C87 -60.4(3) . . . . ? C82 C81 C84 C86 -2.8(4) . . . . ? C80 C81 C84 C86 179.9(2) . . . . ? C82 C81 C84 C85 -123.2(2) . . . . ? C80 C81 C84 C85 59.5(3) . . . . ? C3 C2 C88 C83 -103.4(2) . . . . ? C1 C2 C88 C83 74.2(3) . . . . ? C82 C83 C88 C2 83.3(3) . . . . ? C78 C83 C88 C2 -97.6(2) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 O8 0.84 1.81 2.632(2) 165.4 . O2 H2 O1 0.84 1.91 2.731(2) 164.2 . O3 H3 O2 0.84 1.88 2.716(2) 173.6 . O4 H4 O3 0.84 1.90 2.741(2) 177.2 . O5 H5 O4 0.84 1.98 2.795(2) 162.2 . O6 H6 O5 0.84 1.89 2.723(2) 170.6 . O7 H7 O6 0.84 1.80 2.638(2) 175.7 . O8 H8 O7 0.84 1.78 2.619(2) 175.5 . _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.552 _refine_diff_density_min -0.335 _refine_diff_density_rms 0.050 #===END