# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_global _publ_contact_author_email ATWOODJ@MISSOURI.EDU _publ_contact_author_name 'Prof Jerry L. Atwood' _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? loop_ _publ_author_name J.L.Atwood A.Szumna data_3xTMACl _database_code_CSD 203670 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C126.50 H118.50 Cl N13.50 O21' _chemical_formula_weight 2199.30 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P21/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 18.891(7) _cell_length_b 15.913(6) _cell_length_c 37.075(14) _cell_angle_alpha 90.00 _cell_angle_beta 99.032(7) _cell_angle_gamma 90.00 _cell_volume 11007(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 28678 _cell_measurement_theta_min 1.40 _cell_measurement_theta_max 22.58 _exptl_crystal_description ? _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.327 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4628 _exptl_absorpt_coefficient_mu 0.115 _exptl_absorpt_correction_type experimental _exptl_absorpt_correction_T_min 0.520 _exptl_absorpt_correction_T_max 0.962 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'SMART CCD' _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28678 _diffrn_reflns_av_R_equivalents 0.1671 _diffrn_reflns_av_sigmaI/netI 0.3035 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -40 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.40 _diffrn_reflns_theta_max 22.58 _reflns_number_total 14428 _reflns_number_gt 5261 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Bruker-Nonius)' _computing_cell_refinement 'SMART (Bruker-Nonius)' _computing_data_reduction 'SAINT (Bruker-Nonius)' _computing_structure_solution ; DIRDIF-99 (P.T. Beurskens, G. P.T. Beurskens, R. de Gelder, S. Garcia-Granda, I. Israel, R.O. Gould, J. M. M. Smits) ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (L. Barbour)' _computing_publication_material 'X-Seed (L. Barbour)' _refine_special_details ; Of the five nitrobenzene molecules one is disordered. Owing to disorder, this molecule was refined isotropically and hydrogen atoms were not assigned. A second nitrobenzene molecule was also refined isotropically, since anisotropic refinement resulted in non-positive definite thermal parameters. Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14428 _refine_ls_number_parameters 1385 _refine_ls_number_restraints 10 _refine_ls_R_factor_all 0.2923 _refine_ls_R_factor_gt 0.1307 _refine_ls_wR_factor_ref 0.3429 _refine_ls_wR_factor_gt 0.2865 _refine_ls_goodness_of_fit_ref 1.199 _refine_ls_restrained_S_all 1.200 _refine_ls_shift/su_max 0.275 _refine_ls_shift/su_mean 0.006 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 Cl1 Cl 0.27179(16) 0.48021(17) 0.33331(9) 0.0413(9) Uani 1 1 d . . . O1 O 0.1047(4) 0.2060(4) 0.15010(19) 0.0283(19) Uiso 1 1 d . . . N1 N 0.0531(6) 0.2335(6) 0.2042(3) 0.039(3) Uani 1 1 d . . . C1 C 0.1138(6) 0.3144(6) 0.1074(3) 0.027(3) Uani 1 1 d . . . O2 O -0.0306(4) 0.4554(4) 0.1563(2) 0.044(2) Uani 1 1 d . . . H2 H -0.0408 0.5016 0.1458 0.053 Uiso 1 1 calc R . . N2 N 0.2673(6) 0.2697(5) 0.3268(3) 0.038(3) Uani 1 1 d . . . H1 H 0.2668 0.3186 0.3378 0.046 Uiso 1 1 calc R . . C2 C 0.0842(5) 0.2872(6) 0.1370(3) 0.025(3) Uani 1 1 d . . . O3 O -0.0153(4) 0.6242(4) 0.1488(2) 0.0275(19) Uani 1 1 d . . . N3 N 0.0179(5) 0.7097(6) 0.2019(3) 0.034(3) Uani 1 1 d . . . C3 C 0.0392(6) 0.3332(7) 0.1539(3) 0.028(3) Uani 1 1 d . . . O4 O 0.1948(4) 0.7934(4) 0.15775(19) 0.035(2) Uani 1 1 d . . . H4 H 0.2313 0.8019 0.1479 0.042 Uiso 1 1 calc R . . N4 N 0.0894(5) 0.4998(5) 0.3244(2) 0.032(2) Uani 1 1 d . . . H3 H 0.1354 0.4943 0.3328 0.038 Uiso 1 1 calc R . . C4 C 0.0175(6) 0.4122(7) 0.1384(3) 0.035(3) Uani 1 1 d . . . O5 O 0.3386(4) 0.7620(4) 0.1551(2) 0.035(2) Uani 1 1 d . . . N5 N 0.4228(5) 0.7323(6) 0.2081(3) 0.043(3) Uani 1 1 d . . . C5 C 0.0425(5) 0.4432(6) 0.1079(3) 0.025(3) Uani 1 1 d . . . O6 O 0.4777(4) 0.5126(4) 0.1585(2) 0.047(2) Uani 1 1 d . . . H6 H 0.4819 0.4675 0.1472 0.056 Uiso 1 1 calc R . . N6 N 0.2763(5) 0.6914(5) 0.3286(3) 0.040(3) Uani 1 1 d . . . H5 H 0.2820 0.6416 0.3391 0.048 Uiso 1 1 calc R . . C6 C 0.0164(6) 0.5290(6) 0.0911(3) 0.029(3) Uani 1 1 d . . . O7 O 0.4559(4) 0.3462(5) 0.1504(2) 0.038(2) Uani 1 1 d . . . N7 N 0.4498(5) 0.2615(6) 0.2032(3) 0.034(3) Uani 1 1 d . . . C7 C 0.0668(5) 0.5989(6) 0.1072(3) 0.020(3) Uani 1 1 d . . . O8 O 0.2497(4) 0.1768(4) 0.1541(2) 0.037(2) Uani 1 1 d . . . H8 H 0.2074 0.1686 0.1437 0.044 Uiso 1 1 calc R . . N8 N 0.4475(6) 0.4658(6) 0.3266(3) 0.043(3) Uani 1 1 d . . . H7 H 0.4069 0.4663 0.3354 0.051 Uiso 1 1 calc R . . C8 C 0.0487(6) 0.6447(7) 0.1366(3) 0.025(3) Uani 1 1 d . . . O9 O 0.3268(6) 0.1438(5) 0.3281(3) 0.073(3) Uani 1 1 d . . . C9 C 0.0936(6) 0.7088(6) 0.1544(3) 0.026(3) Uani 1 1 d . . . O10 O -0.0238(5) 0.4679(5) 0.3326(3) 0.060(3) Uani 1 1 d . . . N10 N 0.3723(9) 0.8050(14) 0.4815(5) 0.101(6) Uani 1 1 d . . . C10 C 0.1546(5) 0.7287(6) 0.1396(3) 0.018(3) Uiso 1 1 d . . . O11 O 0.2257(5) 0.8202(5) 0.3315(2) 0.069(3) Uani 1 1 d . . . N11 N 0.1751(7) 0.9825(9) 0.4905(4) 0.069(4) Uani 1 1 d . . . C11 C 0.1746(6) 0.6867(6) 0.1095(3) 0.024(3) Uani 1 1 d . . . O12 O 0.5595(5) 0.5165(6) 0.3330(3) 0.070(3) Uani 1 1 d . . . N12 N 0.3022(10) 0.0693(12) 0.0017(6) 0.109(6) Uani 1 1 d . . . C12 C 0.2415(6) 0.7126(6) 0.0943(3) 0.030(3) Uani 1 1 d . . . O13 O 0.3466(10) 0.7349(9) 0.4764(4) 0.164(8) Uani 1 1 d . . . N13 N 0.1637(10) 0.9507(11) 0.2769(5) 0.122(6) Uiso 1 1 d . . . C13 C 0.3034(6) 0.6580(6) 0.1096(3) 0.029(3) Uani 1 1 d . . . O14 O 0.3947(8) 0.8330(10) 0.5121(4) 0.130(5) Uani 1 1 d . . . C14 C 0.3522(6) 0.6827(6) 0.1404(4) 0.033(3) Uani 1 1 d . . . O15 O 0.1415(7) 0.9151(7) 0.4893(3) 0.093(4) Uani 1 1 d . . . C15 C 0.4089(6) 0.6342(7) 0.1574(3) 0.031(3) Uani 1 1 d . . . O16 O 0.1897(6) 1.0206(7) 0.5194(3) 0.087(4) Uani 1 1 d . . . C16 C 0.4202(6) 0.5555(7) 0.1416(4) 0.036(3) Uani 1 1 d . . . O17 O 0.3090(9) 0.0336(9) -0.0259(4) 0.146(6) Uani 1 1 d . . . C17 C 0.3755(6) 0.5284(6) 0.1106(3) 0.027(3) Uani 1 1 d . . . O18 O 0.2838(8) 0.1451(10) 0.0020(4) 0.132(5) Uani 1 1 d . . . C18 C 0.3928(6) 0.4433(6) 0.0916(3) 0.026(3) Uani 1 1 d . . . O19 O 0.1138(8) 0.8968(9) 0.2688(4) 0.138(5) Uiso 1 1 d . . . C19 C 0.3506(6) 0.3725(7) 0.1063(3) 0.027(3) Uani 1 1 d . . . O20 O 0.1627(7) 0.9895(8) 0.3075(4) 0.125(4) Uiso 1 1 d . . . C20 C 0.3840(6) 0.3247(7) 0.1368(3) 0.028(3) Uani 1 1 d . . . C21 C 0.3499(6) 0.2602(6) 0.1522(3) 0.028(3) Uani 1 1 d . . . C22 C 0.2800(6) 0.2429(6) 0.1367(3) 0.026(3) Uani 1 1 d . . . C23 C 0.2437(6) 0.2841(6) 0.1064(3) 0.027(3) Uani 1 1 d . . . C24 C 0.1673(6) 0.2598(6) 0.0897(3) 0.027(3) Uani 1 1 d . . . C25 C 0.0927(5) 0.3914(6) 0.0932(3) 0.029(3) Uani 1 1 d . . . H25 H 0.1124 0.4113 0.0727 0.035 Uiso 1 1 calc R . . C26 C 0.1293(6) 0.6207(6) 0.0953(3) 0.026(3) Uani 1 1 d . . . H26 H 0.1432 0.5887 0.0759 0.031 Uiso 1 1 calc R . . C27 C 0.3176(6) 0.5788(6) 0.0950(3) 0.028(3) Uani 1 1 d . . . H27 H 0.2870 0.5590 0.0739 0.034 Uiso 1 1 calc R . . C28 C 0.2808(6) 0.3497(6) 0.0930(3) 0.027(3) Uani 1 1 d . . . H28 H 0.2563 0.3813 0.0732 0.032 Uiso 1 1 calc R . . C29 C 0.0595(6) 0.1767(7) 0.1767(3) 0.039(3) Uani 1 1 d . . . H29A H 0.0111 0.1638 0.1635 0.047 Uiso 1 1 calc R . . H29B H 0.0800 0.1238 0.1879 0.047 Uiso 1 1 calc R . . C30 C 0.0137(7) 0.3066(7) 0.1880(3) 0.044(4) Uani 1 1 d . . . H30A H 0.0196 0.3536 0.2057 0.052 Uiso 1 1 calc R . . H30B H -0.0380 0.2928 0.1825 0.052 Uiso 1 1 calc R . . C31 C 0.1100(7) 0.2427(7) 0.2330(4) 0.036(3) Uani 1 1 d . . . C32 C 0.1031(7) 0.3015(7) 0.2621(4) 0.038(3) Uani 1 1 d . . . H32 H 0.0618 0.3361 0.2607 0.045 Uiso 1 1 calc R . . C33 C 0.1558(7) 0.3067(7) 0.2914(4) 0.044(4) Uani 1 1 d . . . H33 H 0.1507 0.3471 0.3096 0.053 Uiso 1 1 calc R . . C34 C 0.2169(7) 0.2569(7) 0.2964(4) 0.033(3) Uani 1 1 d . . . C35 C 0.2249(7) 0.2024(6) 0.2675(4) 0.036(3) Uani 1 1 d . . . H35 H 0.2669 0.1691 0.2689 0.044 Uiso 1 1 calc R . . C36 C 0.1720(7) 0.1966(7) 0.2372(4) 0.040(3) Uani 1 1 d . . . H36 H 0.1791 0.1587 0.2182 0.047 Uiso 1 1 calc R . . C37 C 0.3185(7) 0.2130(8) 0.3416(4) 0.041(3) Uani 1 1 d . . . C38 C 0.3698(7) 0.2431(8) 0.3737(4) 0.042(3) Uani 1 1 d . . . C39 C 0.3567(9) 0.3082(8) 0.3960(4) 0.065(4) Uani 1 1 d . . . H39 H 0.3133 0.3394 0.3910 0.079 Uiso 1 1 calc R . . C40 C 0.4080(10) 0.3281(10) 0.4262(5) 0.083(6) Uani 1 1 d . . . H40 H 0.3989 0.3744 0.4410 0.099 Uiso 1 1 calc R . . C41 C 0.4703(10) 0.2848(10) 0.4355(4) 0.080(5) Uani 1 1 d . . . H41 H 0.5032 0.2989 0.4568 0.096 Uiso 1 1 calc R . . C42 C 0.4845(9) 0.2176(11) 0.4124(4) 0.078(5) Uani 1 1 d . . . H42 H 0.5283 0.1874 0.4175 0.093 Uiso 1 1 calc R . . C43 C 0.4349(8) 0.1963(8) 0.3828(4) 0.057(4) Uani 1 1 d . . . H43 H 0.4438 0.1498 0.3680 0.068 Uiso 1 1 calc R . . C44 C -0.0364(6) 0.6890(7) 0.1740(3) 0.033(3) Uani 1 1 d . . . H44A H -0.0517 0.7403 0.1598 0.040 Uiso 1 1 calc R . . H44B H -0.0779 0.6681 0.1846 0.040 Uiso 1 1 calc R . . C45 C 0.0762(6) 0.7542(6) 0.1867(3) 0.031(3) Uani 1 1 d . . . H45A H 0.0606 0.8122 0.1797 0.037 Uiso 1 1 calc R . . H45B H 0.1194 0.7577 0.2056 0.037 Uiso 1 1 calc R . . C46 C 0.0378(6) 0.6532(7) 0.2316(3) 0.029(3) Uani 1 1 d . . . C47 C 0.0912(6) 0.6759(7) 0.2597(3) 0.031(3) Uani 1 1 d . . . H47 H 0.1164 0.7270 0.2581 0.037 Uiso 1 1 calc R . . C48 C 0.1086(6) 0.6247(7) 0.2905(3) 0.035(3) Uani 1 1 d . . . H48 H 0.1453 0.6411 0.3098 0.042 Uiso 1 1 calc R . . C49 C 0.0712(7) 0.5487(7) 0.2927(4) 0.029(3) Uani 1 1 d . . . C50 C 0.0181(7) 0.5287(8) 0.2652(4) 0.042(3) Uani 1 1 d . . . H50 H -0.0089 0.4792 0.2675 0.050 Uiso 1 1 calc R . . C51 C 0.0012(6) 0.5772(7) 0.2339(3) 0.031(3) Uani 1 1 d . . . H51 H -0.0344 0.5592 0.2144 0.037 Uiso 1 1 calc R . . C52 C 0.0428(9) 0.4600(7) 0.3434(4) 0.046(4) Uani 1 1 d . . . C53 C 0.0718(9) 0.4133(7) 0.3762(4) 0.043(4) Uani 1 1 d . . . C54 C 0.1417(9) 0.4096(8) 0.3899(4) 0.062(4) Uani 1 1 d . . . H54 H 0.1753 0.4405 0.3786 0.075 Uiso 1 1 calc R . . C55 C 0.1662(10) 0.3593(11) 0.4216(4) 0.089(6) Uani 1 1 d . . . H55 H 0.2157 0.3573 0.4315 0.107 Uiso 1 1 calc R . . C56 C 0.1183(12) 0.3152(11) 0.4372(5) 0.086(6) Uani 1 1 d . . . H56 H 0.1338 0.2819 0.4582 0.104 Uiso 1 1 calc R . . C57 C 0.0467(14) 0.3185(10) 0.4224(5) 0.102(7) Uani 1 1 d . . . H57 H 0.0136 0.2863 0.4335 0.122 Uiso 1 1 calc R . . C58 C 0.0216(8) 0.3662(9) 0.3926(4) 0.067(5) Uani 1 1 d . . . H58 H -0.0281 0.3678 0.3831 0.080 Uiso 1 1 calc R . . C59 C 0.3995(7) 0.7918(7) 0.1794(4) 0.050(4) Uani 1 1 d . . . H59A H 0.3873 0.8456 0.1904 0.060 Uiso 1 1 calc R . . H59B H 0.4392 0.8026 0.1655 0.060 Uiso 1 1 calc R . . C60 C 0.4536(6) 0.6601(7) 0.1929(3) 0.039(3) Uani 1 1 d . . . H60A H 0.4565 0.6128 0.2105 0.047 Uiso 1 1 calc R . . H60B H 0.5028 0.6736 0.1888 0.047 Uiso 1 1 calc R . . C61 C 0.3827(7) 0.7203(7) 0.2374(4) 0.040(3) Uani 1 1 d . . . C62 C 0.4055(6) 0.6644(7) 0.2660(4) 0.040(3) Uani 1 1 d . . . H62 H 0.4475 0.6320 0.2653 0.048 Uiso 1 1 calc R . . C63 C 0.3697(6) 0.6552(7) 0.2942(4) 0.041(3) Uani 1 1 d . . . H63 H 0.3852 0.6133 0.3119 0.049 Uiso 1 1 calc R . . C64 C 0.3110(7) 0.7044(7) 0.2986(4) 0.042(4) Uani 1 1 d . . . C65 C 0.2872(7) 0.7621(7) 0.2700(4) 0.047(4) Uani 1 1 d . . . H65 H 0.2472 0.7971 0.2717 0.056 Uiso 1 1 calc R . . C66 C 0.3209(6) 0.7681(7) 0.2402(4) 0.040(3) Uani 1 1 d . . . H66 H 0.3024 0.8051 0.2209 0.047 Uiso 1 1 calc R . . C67 C 0.2344(7) 0.7472(8) 0.3436(4) 0.048(4) Uani 1 1 d . . . C68 C 0.1991(7) 0.7189(8) 0.3748(4) 0.044(4) Uani 1 1 d . . . C69 C 0.2197(10) 0.6486(8) 0.3960(4) 0.080(5) Uani 1 1 d . . . H69 H 0.2584 0.6150 0.3908 0.096 Uiso 1 1 calc R . . C70 C 0.1838(12) 0.6265(10) 0.4251(4) 0.097(7) Uani 1 1 d . . . H70 H 0.1999 0.5797 0.4401 0.117 Uiso 1 1 calc R . . C71 C 0.1280(10) 0.6703(11) 0.4316(5) 0.083(6) Uani 1 1 d . . . H71 H 0.1024 0.6532 0.4505 0.100 Uiso 1 1 calc R . . C72 C 0.1074(9) 0.7392(13) 0.4118(4) 0.086(6) Uani 1 1 d . . . H72 H 0.0680 0.7711 0.4174 0.104 Uiso 1 1 calc R . . C73 C 0.1415(7) 0.7650(8) 0.3835(4) 0.053(4) Uani 1 1 d . . . H73 H 0.1258 0.8141 0.3700 0.063 Uiso 1 1 calc R . . C74 C 0.4900(6) 0.2832(8) 0.1755(3) 0.042(3) Uani 1 1 d . . . H74A H 0.4980 0.2319 0.1615 0.050 Uiso 1 1 calc R . . H74B H 0.5375 0.3044 0.1870 0.050 Uiso 1 1 calc R . . C75 C 0.3825(7) 0.2174(7) 0.1862(3) 0.041(3) Uani 1 1 d . . . H75A H 0.3938 0.1585 0.1806 0.050 Uiso 1 1 calc R . . H75B H 0.3479 0.2165 0.2036 0.050 Uiso 1 1 calc R . . C76 C 0.4459(6) 0.3170(7) 0.2323(3) 0.029(3) Uani 1 1 d . . . C77 C 0.4080(6) 0.2956(7) 0.2602(4) 0.039(3) Uani 1 1 d . . . H77 H 0.3800 0.2457 0.2581 0.047 Uiso 1 1 calc R . . C78 C 0.4100(6) 0.3441(7) 0.2902(4) 0.039(3) Uani 1 1 d . . . H78 H 0.3838 0.3268 0.3088 0.047 Uiso 1 1 calc R . . C79 C 0.4489(6) 0.4180(7) 0.2949(3) 0.033(3) Uani 1 1 d . . . C80 C 0.4869(6) 0.4411(7) 0.2665(4) 0.040(3) Uani 1 1 d . . . H80 H 0.5138 0.4917 0.2687 0.047 Uiso 1 1 calc R . . C81 C 0.4861(6) 0.3929(7) 0.2361(3) 0.033(3) Uani 1 1 d . . . H81 H 0.5122 0.4100 0.2174 0.040 Uiso 1 1 calc R . . C82 C 0.5018(8) 0.5107(8) 0.3449(4) 0.043(4) Uani 1 1 d . . . C83 C 0.4915(8) 0.5539(7) 0.3793(4) 0.045(4) Uani 1 1 d . . . C84 C 0.4324(9) 0.5427(11) 0.3964(5) 0.083(5) Uani 1 1 d . . . H84 H 0.3957 0.5055 0.3857 0.100 Uiso 1 1 calc R . . C85 C 0.4244(11) 0.5834(14) 0.4286(6) 0.118(8) Uani 1 1 d . . . H85 H 0.3825 0.5759 0.4395 0.141 Uiso 1 1 calc R . . C86 C 0.4785(14) 0.6344(14) 0.4441(6) 0.117(8) Uani 1 1 d . . . H86 H 0.4758 0.6590 0.4672 0.140 Uiso 1 1 calc R . . C87 C 0.5387(14) 0.6521(10) 0.4269(6) 0.109(8) Uani 1 1 d . . . H87 H 0.5738 0.6920 0.4368 0.131 Uiso 1 1 calc R . . C88 C 0.5442(9) 0.6082(10) 0.3947(5) 0.080(5) Uani 1 1 d . . . H88 H 0.5853 0.6162 0.3833 0.096 Uiso 1 1 calc R . . C89 C 0.0090(6) 0.5255(6) 0.0489(3) 0.034(3) Uani 1 1 d . . . H89A H 0.0567 0.5174 0.0416 0.041 Uiso 1 1 calc R . . H89B H -0.0218 0.4775 0.0395 0.041 Uiso 1 1 calc R . . C90 C -0.0242(7) 0.6074(7) 0.0326(3) 0.046(4) Uani 1 1 d . . . H90A H -0.0683 0.6191 0.0425 0.069 Uiso 1 1 calc R . . H90B H -0.0353 0.6020 0.0060 0.069 Uiso 1 1 calc R . . H90C H 0.0098 0.6536 0.0388 0.069 Uiso 1 1 calc R . . C91 C 0.2288(7) 0.7123(7) 0.0518(3) 0.044(4) Uani 1 1 d . . . H91A H 0.2744 0.7260 0.0431 0.053 Uiso 1 1 calc R . . H91B H 0.2144 0.6551 0.0430 0.053 Uiso 1 1 calc R . . C92 C 0.1714(7) 0.7748(8) 0.0353(4) 0.062(4) Uani 1 1 d . . . H92A H 0.1255 0.7597 0.0427 0.093 Uiso 1 1 calc R . . H92B H 0.1668 0.7733 0.0086 0.093 Uiso 1 1 calc R . . H92C H 0.1852 0.8315 0.0441 0.093 Uiso 1 1 calc R . . C93 C 0.3786(7) 0.4504(7) 0.0506(4) 0.054(4) Uani 1 1 d . . . H93A H 0.4060 0.4986 0.0430 0.065 Uiso 1 1 calc R . . H93B H 0.3271 0.4621 0.0427 0.065 Uiso 1 1 calc R . . C94 C 0.3995(7) 0.3694(7) 0.0307(4) 0.061(4) Uani 1 1 d . . . H94A H 0.4457 0.3483 0.0431 0.091 Uiso 1 1 calc R . . H94B H 0.4031 0.3829 0.0053 0.091 Uiso 1 1 calc R . . H94C H 0.3627 0.3263 0.0313 0.091 Uiso 1 1 calc R . . C95 C 0.1519(6) 0.2623(6) 0.0486(3) 0.037(3) Uani 1 1 d . . . H95A H 0.1880 0.2281 0.0386 0.045 Uiso 1 1 calc R . . H95B H 0.1559 0.3209 0.0402 0.045 Uiso 1 1 calc R . . C96 C 0.0776(8) 0.2290(8) 0.0342(4) 0.069(4) Uani 1 1 d . . . H96A H 0.0699 0.1761 0.0465 0.103 Uiso 1 1 calc R . . H96B H 0.0734 0.2192 0.0078 0.103 Uiso 1 1 calc R . . H96C H 0.0416 0.2702 0.0389 0.103 Uiso 1 1 calc R . . N100 N 0.2343(5) 0.4824(5) 0.2054(3) 0.035(3) Uani 1 1 d D . . C101 C 0.2300(10) 0.4862(11) 0.1667(4) 0.145(8) Uiso 1 1 d D . . H10A H 0.2070 0.5390 0.1576 0.218 Uiso 1 1 calc R . . H10B H 0.2018 0.4386 0.1555 0.218 Uiso 1 1 calc R . . H10C H 0.2784 0.4837 0.1603 0.218 Uiso 1 1 calc R . . C102 C 0.1606(9) 0.4971(12) 0.2122(5) 0.151(8) Uiso 1 1 d D . . H10D H 0.1571 0.4824 0.2375 0.226 Uiso 1 1 calc R . . H10E H 0.1274 0.4621 0.1956 0.226 Uiso 1 1 calc R . . H10F H 0.1483 0.5565 0.2080 0.226 Uiso 1 1 calc R . . C103 C 0.2400(14) 0.3924(12) 0.2137(6) 0.233(14) Uiso 1 1 d D . . H10G H 0.2859 0.3711 0.2083 0.349 Uiso 1 1 calc R . . H10H H 0.2006 0.3624 0.1988 0.349 Uiso 1 1 calc R . . H10I H 0.2374 0.3835 0.2396 0.349 Uiso 1 1 calc R . . C104 C 0.2711(18) 0.554(2) 0.2206(8) 0.40(3) Uiso 1 1 d D . . H10J H 0.2430 0.6045 0.2126 0.602 Uiso 1 1 calc R . . H10K H 0.3178 0.5577 0.2123 0.602 Uiso 1 1 calc R . . H10L H 0.2781 0.5505 0.2473 0.602 Uiso 1 1 calc R . . C105 C 0.3804(9) 0.8647(13) 0.4521(5) 0.073(5) Uani 1 1 d . . . C106 C 0.3664(8) 0.8333(12) 0.4170(6) 0.090(6) Uani 1 1 d . . . H106 H 0.3517 0.7766 0.4128 0.109 Uiso 1 1 calc R . . C107 C 0.3741(9) 0.8859(15) 0.3881(6) 0.096(6) Uani 1 1 d . . . H107 H 0.3677 0.8640 0.3640 0.115 Uiso 1 1 calc R . . C108 C 0.3900(9) 0.9646(14) 0.3934(6) 0.087(6) Uani 1 1 d . . . H108 H 0.3897 1.0010 0.3731 0.105 Uiso 1 1 calc R . . C109 C 0.4073(10) 0.9954(11) 0.4279(6) 0.101(6) Uani 1 1 d . . . H109 H 0.4232 1.0519 0.4314 0.121 Uiso 1 1 calc R . . C110 C 0.4018(10) 0.9455(12) 0.4581(5) 0.091(6) Uani 1 1 d . . . H110 H 0.4127 0.9673 0.4821 0.110 Uiso 1 1 calc R . . C111 C 0.1948(8) 1.0162(10) 0.4564(5) 0.060(4) Uani 1 1 d . . . C112 C 0.2228(9) 1.0958(12) 0.4582(6) 0.096(6) Uani 1 1 d . . . H112 H 0.2324 1.1272 0.4802 0.115 Uiso 1 1 calc R . . C113 C 0.2362(13) 1.1270(14) 0.4238(10) 0.170(14) Uani 1 1 d . . . H113 H 0.2533 1.1827 0.4220 0.204 Uiso 1 1 calc R . . C114 C 0.2239(14) 1.0746(17) 0.3921(8) 0.162(12) Uani 1 1 d . . . H114 H 0.2336 1.0946 0.3692 0.195 Uiso 1 1 calc R . . C115 C 0.1985(8) 0.9974(14) 0.3951(5) 0.096(6) Uani 1 1 d . . . H115 H 0.1901 0.9626 0.3741 0.115 Uiso 1 1 calc R . . C116 C 0.1844(9) 0.9672(12) 0.4270(5) 0.086(6) Uani 1 1 d . . . H116 H 0.1672 0.9114 0.4285 0.104 Uiso 1 1 calc R . . C117 C 0.3084(9) 0.0219(13) 0.0362(6) 0.085(5) Uani 1 1 d . . . C118 C 0.2860(10) 0.0611(12) 0.0660(6) 0.114(7) Uani 1 1 d . . . H118 H 0.2658 0.1159 0.0643 0.137 Uiso 1 1 calc R . . C119 C 0.2952(12) 0.0147(14) 0.0985(5) 0.129(8) Uani 1 1 d . . . H119 H 0.2825 0.0398 0.1199 0.155 Uiso 1 1 calc R . . C120 C 0.3210(12) -0.0627(12) 0.1005(8) 0.138(10) Uani 1 1 d . . . H120 H 0.3243 -0.0958 0.1221 0.166 Uiso 1 1 calc R . . C121 C 0.3449(11) -0.0947(15) 0.0661(12) 0.181(17) Uani 1 1 d . . . H121 H 0.3634 -0.1502 0.0661 0.217 Uiso 1 1 calc R . . C122 C 0.3415(16) -0.0486(13) 0.0350(10) 0.199(18) Uani 1 1 d . . . H122 H 0.3616 -0.0665 0.0143 0.239 Uiso 1 1 calc R . . C123 C 0.2130(8) 0.9650(9) 0.2565(4) 0.065(4) Uiso 1 1 d . . . C124 C 0.2791(8) 0.9924(9) 0.2703(4) 0.076(5) Uiso 1 1 d . . . H124 H 0.2863 0.9967 0.2962 0.091 Uiso 1 1 calc R . . C125 C 0.3359(11) 1.0146(11) 0.2565(5) 0.109(6) Uiso 1 1 d . . . H125 H 0.3821 1.0314 0.2682 0.131 Uiso 1 1 calc R . . C126 C 0.3064(8) 1.0056(8) 0.2162(4) 0.066(4) Uiso 1 1 d . . . H126 H 0.3398 1.0199 0.2005 0.079 Uiso 1 1 calc R . . C127 C 0.2396(8) 0.9803(9) 0.1975(4) 0.078(5) Uiso 1 1 d . . . H127 H 0.2312 0.9779 0.1716 0.094 Uiso 1 1 calc R . . C128 C 0.1843(8) 0.9584(8) 0.2178(4) 0.065(4) Uiso 1 1 d . . . H128 H 0.1369 0.9421 0.2078 0.077 Uiso 1 1 calc R . . O130 O 0.0831(16) -0.0170(18) 0.0429(9) 0.117(11) Uiso 0.50 1 d P . . C130 C 0.1165(17) 0.0006(19) 0.0487(9) 0.052(9) Uiso 0.50 1 d P . . C133 C -0.0169(19) 0.008(2) 0.0433(11) 0.096(11) Uiso 0.50 1 d P . . C134 C 0.056(3) 0.012(3) 0.0717(13) 0.145(16) Uiso 0.50 1 d P . . O135 O 0.1386(15) -0.0053(16) -0.0025(7) 0.130(10) Uiso 0.50 1 d P . . C135 C 0.0331(9) -0.0034(11) -0.0073(6) 0.105(6) Uiso 1 1 d . . . N136 N 0.1000(12) -0.0039(12) 0.0139(6) 0.040(5) Uiso 0.50 1 d P . . 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 Cl1 0.044(2) 0.0227(16) 0.059(2) -0.0015(16) 0.0138(18) -0.0003(15) N1 0.048(7) 0.020(6) 0.052(8) 0.005(6) 0.013(6) 0.003(5) C1 0.036(7) 0.004(6) 0.041(8) -0.005(6) 0.010(7) 0.006(5) O2 0.046(5) 0.017(4) 0.073(6) 0.012(4) 0.020(5) 0.006(4) N2 0.051(7) 0.015(6) 0.053(8) -0.002(6) 0.021(6) 0.008(6) C2 0.019(7) 0.010(6) 0.045(8) 0.005(6) 0.002(6) 0.003(5) O3 0.028(5) 0.012(4) 0.048(5) -0.011(4) 0.020(4) -0.002(4) N3 0.024(6) 0.029(6) 0.047(7) 0.003(6) 0.002(6) 0.003(5) C3 0.042(8) 0.014(6) 0.032(8) -0.005(6) 0.016(7) -0.020(6) O4 0.045(5) 0.020(4) 0.042(5) -0.008(4) 0.017(4) -0.010(4) N4 0.034(6) 0.032(6) 0.035(6) 0.001(5) 0.020(5) -0.008(5) C4 0.027(7) 0.027(7) 0.057(9) -0.007(7) 0.027(7) -0.009(6) O5 0.041(5) 0.008(4) 0.060(6) -0.011(4) 0.014(5) 0.001(4) N5 0.052(7) 0.031(6) 0.049(8) -0.008(6) 0.018(6) -0.007(6) C5 0.013(6) 0.016(6) 0.044(8) -0.014(6) -0.004(6) 0.002(5) O6 0.037(5) 0.021(4) 0.079(7) -0.009(5) 0.004(5) 0.008(4) N6 0.052(7) 0.014(5) 0.055(8) 0.000(5) 0.010(6) 0.005(5) C6 0.050(8) 0.007(6) 0.027(8) 0.005(6) -0.008(6) -0.006(6) O7 0.031(5) 0.036(5) 0.049(6) 0.002(4) 0.012(5) 0.011(4) N7 0.026(6) 0.036(6) 0.042(7) 0.009(6) 0.010(6) 0.004(5) C7 0.018(7) 0.008(6) 0.033(8) 0.009(6) 0.003(6) 0.003(5) O8 0.044(5) 0.015(4) 0.050(6) 0.008(4) 0.000(4) -0.004(4) N8 0.043(7) 0.027(6) 0.058(8) 0.003(6) 0.010(6) -0.002(6) C8 0.028(7) 0.022(7) 0.024(7) 0.003(6) 0.003(6) 0.005(6) O9 0.126(9) 0.024(5) 0.068(7) -0.001(5) 0.010(7) 0.022(6) C9 0.038(8) 0.003(6) 0.039(8) -0.001(6) 0.012(6) 0.006(6) O10 0.060(7) 0.056(6) 0.069(7) 0.006(5) 0.029(6) -0.007(6) N10 0.088(13) 0.141(18) 0.080(14) -0.037(16) 0.029(11) 0.013(12) O11 0.111(9) 0.025(5) 0.065(7) -0.010(5) 0.000(6) 0.020(5) N11 0.079(10) 0.066(10) 0.057(10) -0.017(9) -0.010(8) 0.001(8) C11 0.023(7) 0.020(6) 0.029(7) 0.010(6) 0.007(6) 0.006(6) O12 0.056(7) 0.084(7) 0.066(7) -0.002(6) -0.005(6) -0.023(6) N12 0.131(15) 0.090(14) 0.114(17) -0.019(14) 0.047(13) 0.004(12) C12 0.039(8) 0.021(6) 0.031(8) 0.005(6) 0.005(6) 0.011(6) O13 0.28(2) 0.073(9) 0.158(16) -0.023(10) 0.093(15) -0.043(12) C13 0.036(8) 0.011(6) 0.041(8) 0.003(6) 0.008(7) -0.005(6) O14 0.139(13) 0.144(13) 0.112(12) 0.024(11) 0.033(11) 0.017(10) C14 0.033(8) 0.017(7) 0.054(9) 0.007(7) 0.028(8) -0.006(6) O15 0.126(11) 0.063(8) 0.086(9) 0.002(7) 0.001(8) -0.015(7) C15 0.010(6) 0.034(8) 0.051(9) -0.005(7) 0.008(6) -0.001(6) O16 0.093(9) 0.105(9) 0.062(8) -0.026(7) 0.006(7) 0.007(7) C16 0.020(8) 0.025(8) 0.069(11) 0.004(8) 0.025(8) -0.003(6) O17 0.196(16) 0.144(13) 0.123(13) -0.039(11) 0.099(12) -0.039(11) C17 0.039(8) 0.012(6) 0.036(8) 0.008(6) 0.026(7) -0.002(6) O18 0.172(14) 0.114(11) 0.114(12) 0.024(10) 0.029(10) 0.038(11) C18 0.043(8) 0.013(6) 0.026(8) -0.002(6) 0.018(6) -0.002(6) C19 0.033(8) 0.024(7) 0.025(8) 0.000(6) 0.005(6) 0.013(6) C20 0.021(7) 0.021(7) 0.044(9) -0.015(7) 0.011(7) 0.001(6) C21 0.034(8) 0.015(6) 0.036(8) 0.003(6) 0.006(7) 0.008(6) C22 0.034(8) 0.015(6) 0.029(8) 0.008(6) 0.010(6) 0.007(6) C23 0.038(8) 0.007(6) 0.038(8) -0.009(6) 0.016(7) 0.001(6) C24 0.044(8) 0.027(7) 0.007(7) -0.005(5) -0.002(6) -0.005(6) C25 0.024(7) 0.020(7) 0.042(8) 0.000(6) 0.004(6) -0.003(6) C26 0.031(7) 0.009(6) 0.038(8) 0.001(6) 0.008(6) 0.010(6) C27 0.043(8) 0.014(6) 0.033(8) 0.006(6) 0.019(7) 0.010(6) C28 0.039(8) 0.015(6) 0.029(8) 0.007(6) 0.009(7) 0.023(6) C29 0.047(9) 0.025(7) 0.045(9) 0.005(7) 0.009(7) -0.007(6) C30 0.044(8) 0.030(8) 0.061(10) 0.016(7) 0.022(8) -0.006(7) C31 0.027(8) 0.025(7) 0.059(10) 0.018(7) 0.019(8) -0.001(7) C32 0.034(8) 0.033(8) 0.051(10) 0.008(7) 0.022(8) 0.003(7) C33 0.058(10) 0.018(7) 0.063(11) 0.001(7) 0.030(9) -0.018(7) C34 0.041(9) 0.014(7) 0.043(9) 0.005(7) 0.008(7) 0.007(7) C35 0.045(9) 0.012(6) 0.054(10) -0.004(7) 0.015(8) 0.015(6) C36 0.059(10) 0.024(7) 0.039(9) -0.005(7) 0.018(8) 0.003(7) C37 0.059(10) 0.023(8) 0.044(10) 0.013(8) 0.018(8) -0.004(8) C38 0.061(10) 0.029(8) 0.038(9) 0.003(7) 0.013(8) 0.010(8) C39 0.079(12) 0.057(10) 0.062(11) -0.007(9) 0.013(10) 0.032(9) C40 0.093(14) 0.080(12) 0.067(13) -0.028(10) -0.013(11) 0.045(11) C41 0.096(15) 0.076(12) 0.062(12) -0.031(10) -0.006(11) -0.002(11) C42 0.074(13) 0.108(14) 0.054(12) 0.000(11) 0.017(10) 0.017(11) C43 0.069(11) 0.053(10) 0.047(10) 0.000(8) 0.005(9) 0.022(9) C44 0.028(8) 0.024(7) 0.052(9) -0.004(7) 0.015(7) 0.009(6) C45 0.038(8) 0.008(6) 0.047(8) 0.012(6) 0.003(7) -0.009(6) C46 0.028(7) 0.028(7) 0.036(8) -0.003(7) 0.020(7) 0.006(6) C47 0.032(8) 0.024(7) 0.041(9) -0.011(7) 0.021(7) -0.015(6) C48 0.041(8) 0.037(8) 0.027(8) -0.016(7) 0.004(7) -0.012(7) C49 0.036(8) 0.021(7) 0.036(9) -0.010(7) 0.021(7) -0.001(6) C50 0.038(9) 0.040(8) 0.055(10) -0.014(8) 0.029(8) -0.004(7) C51 0.032(8) 0.027(7) 0.032(8) 0.000(7) 0.004(6) 0.001(6) C52 0.067(11) 0.023(7) 0.054(10) -0.007(7) 0.025(9) -0.003(8) C53 0.074(11) 0.022(7) 0.034(9) 0.001(7) 0.013(9) -0.009(8) C54 0.086(13) 0.046(9) 0.060(12) 0.023(8) 0.031(10) 0.030(9) C55 0.094(14) 0.109(14) 0.075(13) 0.036(12) 0.049(12) 0.020(12) C56 0.114(17) 0.064(12) 0.089(15) 0.010(11) 0.041(15) 0.036(13) C57 0.19(2) 0.061(12) 0.070(15) 0.018(11) 0.060(16) -0.043(15) C58 0.091(12) 0.064(10) 0.048(10) 0.003(9) 0.017(9) -0.045(10) C59 0.036(8) 0.020(7) 0.096(12) -0.003(8) 0.017(9) -0.014(7) C60 0.026(7) 0.039(8) 0.055(9) 0.003(7) 0.013(7) 0.000(6) C61 0.036(8) 0.026(7) 0.053(10) -0.003(7) -0.009(7) -0.004(7) C62 0.027(8) 0.022(7) 0.067(10) -0.004(7) -0.005(8) 0.000(6) C63 0.027(8) 0.027(7) 0.066(10) 0.008(7) 0.001(8) 0.001(6) C64 0.042(9) 0.019(7) 0.066(11) -0.014(7) 0.008(8) -0.013(7) C65 0.058(10) 0.017(7) 0.065(10) 0.018(7) 0.010(8) 0.007(7) C66 0.040(8) 0.025(7) 0.053(10) 0.000(7) 0.004(7) 0.013(7) C67 0.065(10) 0.026(8) 0.050(10) -0.016(8) -0.006(8) 0.006(8) C68 0.063(10) 0.024(8) 0.041(9) -0.007(7) -0.006(8) -0.003(7) C69 0.138(16) 0.030(9) 0.069(13) -0.021(9) 0.011(12) 0.022(10) C70 0.19(2) 0.061(11) 0.050(12) 0.004(9) 0.047(13) 0.036(13) C71 0.135(18) 0.058(11) 0.064(13) 0.004(10) 0.035(12) 0.035(11) C72 0.076(12) 0.131(17) 0.058(12) -0.033(12) 0.030(10) 0.003(12) C73 0.070(11) 0.043(8) 0.042(9) 0.000(7) 0.000(8) 0.030(8) C74 0.013(7) 0.049(8) 0.064(10) 0.003(8) 0.007(7) 0.009(6) C75 0.054(9) 0.018(7) 0.051(9) 0.011(7) 0.002(8) -0.003(7) C76 0.023(7) 0.023(7) 0.037(8) 0.005(7) -0.006(6) 0.010(6) C77 0.037(8) 0.021(7) 0.057(10) 0.002(7) 0.003(8) -0.008(6) C78 0.019(7) 0.034(8) 0.065(10) 0.009(8) 0.009(7) 0.001(6) C79 0.030(8) 0.031(8) 0.036(9) 0.017(7) 0.002(7) 0.002(6) C80 0.019(7) 0.025(7) 0.070(10) 0.002(8) -0.005(7) 0.003(6) C81 0.031(7) 0.028(7) 0.043(9) -0.002(7) 0.012(7) -0.001(6) C82 0.046(10) 0.026(8) 0.057(11) 0.024(8) 0.006(9) 0.003(8) C83 0.050(10) 0.022(7) 0.060(11) -0.001(8) -0.002(9) -0.008(7) C84 0.075(13) 0.098(14) 0.070(13) -0.011(11) -0.011(11) -0.027(11) C85 0.092(16) 0.16(2) 0.100(17) -0.082(15) 0.008(13) -0.028(14) C86 0.13(2) 0.098(17) 0.12(2) -0.043(15) -0.006(18) 0.028(16) C87 0.17(2) 0.031(10) 0.112(19) -0.014(12) -0.040(17) -0.002(13) C88 0.099(14) 0.051(11) 0.079(14) 0.021(10) -0.014(11) -0.016(10) C89 0.047(8) 0.012(6) 0.041(8) 0.009(6) 0.002(7) 0.007(6) C90 0.065(10) 0.033(8) 0.034(8) -0.005(7) -0.011(7) 0.002(7) C91 0.068(10) 0.013(6) 0.056(10) 0.021(7) 0.022(8) 0.015(6) C92 0.081(11) 0.054(9) 0.057(10) 0.014(8) 0.029(9) 0.004(8) C93 0.077(10) 0.018(7) 0.080(11) 0.014(7) 0.053(9) -0.001(7) C94 0.081(11) 0.038(8) 0.071(11) -0.026(8) 0.036(9) 0.010(8) C95 0.052(9) 0.012(6) 0.049(9) -0.007(6) 0.014(7) 0.005(6) C96 0.090(13) 0.055(10) 0.057(10) 0.003(8) -0.002(9) 0.000(9) N100 0.046(7) 0.024(5) 0.039(7) 0.001(5) 0.019(5) 0.000(5) C105 0.067(12) 0.095(16) 0.063(14) 0.014(13) 0.031(11) 0.021(11) C106 0.069(12) 0.105(15) 0.101(17) -0.009(15) 0.026(12) -0.033(11) C107 0.073(13) 0.124(18) 0.093(17) -0.007(15) 0.021(12) -0.034(13) C108 0.079(13) 0.102(16) 0.088(16) 0.004(14) 0.037(12) -0.022(12) C109 0.156(19) 0.079(13) 0.075(14) 0.013(13) 0.038(14) -0.013(13) C110 0.128(17) 0.074(13) 0.085(15) -0.012(12) 0.055(13) 0.000(12) C111 0.055(10) 0.058(11) 0.069(13) 0.004(11) 0.015(9) 0.006(9) C112 0.068(12) 0.084(14) 0.143(19) -0.024(14) 0.039(13) -0.014(11) C113 0.16(2) 0.063(15) 0.33(4) 0.04(2) 0.17(3) -0.003(15) C114 0.18(3) 0.11(2) 0.23(3) 0.04(2) 0.14(3) -0.01(2) C115 0.057(11) 0.16(2) 0.071(14) 0.012(14) 0.017(10) -0.024(12) C116 0.086(13) 0.129(16) 0.040(11) -0.008(13) -0.001(10) -0.015(12) C117 0.076(13) 0.083(15) 0.097(16) 0.006(13) 0.014(12) -0.006(11) C118 0.121(17) 0.111(16) 0.116(18) -0.031(15) 0.033(15) 0.068(13) C119 0.20(2) 0.117(19) 0.058(13) 0.012(14) -0.020(14) 0.046(17) C120 0.108(18) 0.034(12) 0.26(3) 0.024(16) -0.001(19) -0.002(11) C121 0.058(14) 0.070(17) 0.43(6) -0.09(3) 0.09(2) -0.016(13) C122 0.21(3) 0.018(13) 0.38(5) 0.028(19) 0.09(3) 0.024(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C2 1.412(11) . ? O1 C29 1.478(12) . ? N1 C29 1.383(13) . ? N1 C31 1.399(14) . ? N1 C30 1.459(13) . ? C1 C25 1.368(13) . ? C1 C2 1.378(14) . ? C1 C24 1.554(14) . ? O2 C4 1.389(12) . ? N2 C34 1.372(14) . ? N2 C37 1.373(14) . ? C2 C3 1.349(14) . ? O3 C8 1.396(12) . ? O3 C44 1.486(11) . ? N3 C44 1.378(13) . ? N3 C46 1.423(13) . ? N3 C45 1.492(13) . ? C3 C4 1.416(15) . ? C3 C30 1.482(14) . ? O4 C10 1.390(11) . ? N4 C52 1.369(14) . ? N4 C49 1.406(14) . ? C4 C5 1.380(14) . ? O5 C14 1.413(12) . ? O5 C59 1.426(13) . ? N5 C61 1.432(15) . ? N5 C59 1.438(14) . ? N5 C60 1.442(13) . ? C5 C25 1.429(13) . ? C5 C6 1.548(14) . ? O6 C16 1.351(13) . ? N6 C67 1.364(14) . ? N6 C64 1.393(15) . ? C6 C7 1.522(13) . ? C6 C89 1.551(14) . ? O7 C20 1.414(12) . ? O7 C74 1.449(13) . ? N7 C76 1.406(13) . ? N7 C74 1.413(13) . ? N7 C75 1.502(14) . ? C7 C26 1.370(13) . ? C7 C8 1.396(14) . ? O8 C22 1.402(12) . ? N8 C82 1.344(15) . ? N8 C79 1.403(14) . ? C8 C9 1.421(14) . ? O9 C37 1.230(14) . ? C9 C10 1.389(13) . ? C9 C45 1.481(14) . ? O10 C52 1.264(15) . ? N10 O13 1.219(19) . ? N10 O14 1.231(17) . ? N10 C105 1.47(2) . ? C10 C11 1.400(13) . ? O11 C67 1.247(13) . ? N11 O16 1.224(13) . ? N11 O15 1.244(14) . ? N11 C111 1.472(19) . ? C11 C26 1.404(13) . ? C11 C12 1.519(14) . ? O12 C82 1.242(14) . ? N12 O17 1.195(17) . ? N12 O18 1.255(17) . ? N12 C117 1.48(2) . ? C12 C13 1.494(15) . ? C12 C91 1.558(15) . ? N13 O19 1.276(18) . ? N13 O20 1.294(17) . ? N13 C123 1.306(18) . ? C13 C14 1.406(15) . ? C13 C27 1.414(14) . ? C14 C15 1.390(15) . ? C15 C16 1.412(15) . ? C15 C60 1.506(15) . ? C16 C17 1.385(15) . ? C17 C27 1.405(14) . ? C17 C18 1.584(14) . ? C18 C93 1.506(15) . ? C18 C19 1.531(14) . ? C19 C28 1.382(14) . ? C19 C20 1.423(15) . ? C20 C21 1.382(14) . ? C21 C22 1.382(15) . ? C21 C75 1.479(15) . ? C22 C23 1.386(14) . ? C23 C28 1.391(14) . ? C23 C24 1.527(15) . ? C24 C95 1.507(14) . ? C31 C36 1.369(15) . ? C31 C32 1.449(16) . ? C32 C33 1.356(16) . ? C33 C34 1.388(16) . ? C34 C35 1.403(15) . ? C35 C36 1.386(15) . ? C37 C38 1.491(17) . ? C38 C39 1.373(16) . ? C38 C43 1.431(17) . ? C39 C40 1.396(19) . ? C40 C41 1.362(19) . ? C41 C42 1.422(19) . ? C42 C43 1.371(18) . ? C46 C47 1.380(15) . ? C46 C51 1.402(14) . ? C47 C48 1.400(15) . ? C48 C49 1.410(14) . ? C49 C50 1.349(15) . ? C50 C51 1.391(15) . ? C52 C53 1.457(18) . ? C53 C54 1.339(17) . ? C53 C58 1.419(17) . ? C54 C55 1.438(19) . ? C55 C56 1.34(2) . ? C56 C57 1.38(2) . ? C57 C58 1.36(2) . ? C61 C62 1.397(16) . ? C61 C66 1.410(15) . ? C62 C63 1.340(16) . ? C63 C64 1.389(15) . ? C64 C65 1.420(16) . ? C65 C66 1.363(15) . ? C67 C68 1.494(17) . ? C68 C69 1.388(17) . ? C68 C73 1.392(16) . ? C69 C70 1.40(2) . ? C70 C71 1.32(2) . ? C71 C72 1.34(2) . ? C72 C73 1.377(19) . ? C76 C77 1.389(15) . ? C76 C81 1.423(14) . ? C77 C78 1.349(15) . ? C78 C79 1.383(15) . ? C79 C80 1.412(15) . ? C80 C81 1.361(15) . ? C82 C83 1.489(18) . ? C83 C88 1.374(18) . ? C83 C84 1.378(19) . ? C84 C85 1.39(2) . ? C85 C86 1.36(2) . ? C86 C87 1.42(3) . ? C87 C88 1.40(2) . ? C89 C90 1.529(14) . ? C91 C92 1.527(15) . ? C93 C94 1.565(14) . ? C95 C96 1.517(16) . ? N100 C104 1.408(18) . ? N100 C101 1.428(15) . ? N100 C103 1.464(16) . ? N100 C102 1.472(15) . ? C105 C110 1.36(2) . ? C105 C106 1.38(2) . ? C106 C107 1.39(2) . ? C107 C108 1.29(2) . ? C108 C109 1.36(2) . ? C109 C110 1.39(2) . ? C111 C116 1.331(19) . ? C111 C112 1.37(2) . ? C112 C113 1.43(3) . ? C113 C114 1.43(3) . ? C114 C115 1.33(3) . ? C115 C116 1.34(2) . ? C117 C122 1.29(3) . ? C117 C118 1.39(2) . ? C118 C119 1.40(2) . ? C119 C120 1.32(2) . ? C120 C121 1.51(3) . ? C121 C122 1.36(4) . ? C123 C124 1.347(18) . ? C123 C128 1.458(18) . ? C124 C125 1.31(2) . ? C125 C126 1.52(2) . ? C126 C127 1.400(18) . ? C127 C128 1.422(17) . ? O130 C130 0.69(4) . ? O130 N136 1.19(3) . ? O130 C134 1.33(5) . ? C130 N136 1.28(4) . ? C130 C134 1.54(6) . ? C133 C135 1.33(4) 3 ? C133 C134 1.60(5) . ? O135 N136 1.02(3) . ? C135 C133 1.33(4) 3 ? C135 N136 1.38(2) . ? C135 C135 1.44(3) 3 ? 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 O1 C29 111.3(8) . . ? C29 N1 C31 119.0(10) . . ? C29 N1 C30 108.3(10) . . ? C31 N1 C30 120.9(10) . . ? C25 C1 C2 117.3(10) . . ? C25 C1 C24 120.6(10) . . ? C2 C1 C24 122.2(9) . . ? C34 N2 C37 125.9(10) . . ? C3 C2 C1 124.3(10) . . ? C3 C2 O1 119.7(10) . . ? C1 C2 O1 116.0(9) . . ? C8 O3 C44 111.9(8) . . ? C44 N3 C46 120.3(10) . . ? C44 N3 C45 109.6(10) . . ? C46 N3 C45 118.0(9) . . ? C2 C3 C4 117.1(10) . . ? C2 C3 C30 123.6(11) . . ? C4 C3 C30 119.3(10) . . ? C52 N4 C49 126.5(11) . . ? C5 C4 O2 123.1(10) . . ? C5 C4 C3 122.5(10) . . ? O2 C4 C3 114.4(10) . . ? C14 O5 C59 111.4(9) . . ? C61 N5 C59 120.8(10) . . ? C61 N5 C60 118.9(10) . . ? C59 N5 C60 109.4(10) . . ? C4 C5 C25 116.0(10) . . ? C4 C5 C6 121.1(10) . . ? C25 C5 C6 122.9(10) . . ? C67 N6 C64 127.1(11) . . ? C7 C6 C5 110.3(8) . . ? C7 C6 C89 112.0(9) . . ? C5 C6 C89 110.3(8) . . ? C20 O7 C74 111.5(8) . . ? C76 N7 C74 120.3(10) . . ? C76 N7 C75 118.3(9) . . ? C74 N7 C75 109.0(9) . . ? C26 C7 C8 116.6(10) . . ? C26 C7 C6 125.2(10) . . ? C8 C7 C6 118.2(9) . . ? C82 N8 C79 126.8(11) . . ? O3 C8 C7 117.6(9) . . ? O3 C8 C9 120.0(9) . . ? C7 C8 C9 122.4(10) . . ? C10 C9 C8 116.8(10) . . ? C10 C9 C45 120.8(10) . . ? C8 C9 C45 122.3(10) . . ? O13 N10 O14 123(2) . . ? O13 N10 C105 124.0(19) . . ? O14 N10 C105 113(2) . . ? C9 C10 O4 113.7(9) . . ? C9 C10 C11 123.4(10) . . ? O4 C10 C11 122.9(9) . . ? O16 N11 O15 120.1(15) . . ? O16 N11 C111 121.3(15) . . ? O15 N11 C111 118.6(14) . . ? C10 C11 C26 115.5(10) . . ? C10 C11 C12 120.7(10) . . ? C26 C11 C12 123.8(10) . . ? O17 N12 O18 122(2) . . ? O17 N12 C117 119.7(18) . . ? O18 N12 C117 117.9(18) . . ? C13 C12 C11 110.5(9) . . ? C13 C12 C91 111.6(9) . . ? C11 C12 C91 111.7(10) . . ? O19 N13 O20 114.5(18) . . ? O19 N13 C123 123.3(19) . . ? O20 N13 C123 122.2(18) . . ? C14 C13 C27 114.9(11) . . ? C14 C13 C12 121.2(10) . . ? C27 C13 C12 123.9(11) . . ? C15 C14 C13 125.0(10) . . ? C15 C14 O5 119.5(11) . . ? C13 C14 O5 115.4(10) . . ? C14 C15 C16 117.3(12) . . ? C14 C15 C60 122.2(10) . . ? C16 C15 C60 120.3(11) . . ? O6 C16 C17 124.6(11) . . ? O6 C16 C15 114.7(12) . . ? C17 C16 C15 120.6(11) . . ? C16 C17 C27 119.8(10) . . ? C16 C17 C18 119.6(10) . . ? C27 C17 C18 120.4(11) . . ? C93 C18 C19 113.3(9) . . ? C93 C18 C17 111.6(9) . . ? C19 C18 C17 108.4(8) . . ? C28 C19 C20 115.0(10) . . ? C28 C19 C18 125.9(10) . . ? C20 C19 C18 119.1(10) . . ? C21 C20 O7 121.1(11) . . ? C21 C20 C19 123.1(11) . . ? O7 C20 C19 115.8(10) . . ? C22 C21 C20 117.0(11) . . ? C22 C21 C75 120.3(10) . . ? C20 C21 C75 122.4(11) . . ? C21 C22 C23 124.2(10) . . ? C21 C22 O8 113.0(10) . . ? C23 C22 O8 122.7(10) . . ? C22 C23 C28 115.5(11) . . ? C22 C23 C24 121.7(10) . . ? C28 C23 C24 122.9(11) . . ? C95 C24 C23 115.0(10) . . ? C95 C24 C1 112.1(9) . . ? C23 C24 C1 108.9(8) . . ? C1 C25 C5 122.8(11) . . ? C7 C26 C11 125.1(10) . . ? C17 C27 C13 122.2(11) . . ? C19 C28 C23 125.2(11) . . ? N1 C29 O1 114.4(9) . . ? N1 C30 C3 111.5(10) . . ? C36 C31 N1 124.8(12) . . ? C36 C31 C32 116.0(12) . . ? N1 C31 C32 119.1(11) . . ? C33 C32 C31 119.6(12) . . ? C32 C33 C34 124.3(12) . . ? N2 C34 C33 118.7(11) . . ? N2 C34 C35 125.0(11) . . ? C33 C34 C35 116.0(12) . . ? C36 C35 C34 120.7(11) . . ? C31 C36 C35 123.3(12) . . ? O9 C37 N2 123.5(13) . . ? O9 C37 C38 120.3(12) . . ? N2 C37 C38 115.9(11) . . ? C39 C38 C43 118.8(13) . . ? C39 C38 C37 124.5(13) . . ? C43 C38 C37 116.5(12) . . ? C38 C39 C40 119.0(14) . . ? C41 C40 C39 123.5(14) . . ? C40 C41 C42 117.7(15) . . ? C43 C42 C41 120.0(15) . . ? C42 C43 C38 120.9(13) . . ? N3 C44 O3 113.4(9) . . ? C9 C45 N3 110.2(9) . . ? C47 C46 C51 119.2(11) . . ? C47 C46 N3 119.4(10) . . ? C51 C46 N3 121.2(11) . . ? C46 C47 C48 121.0(10) . . ? C47 C48 C49 119.3(11) . . ? C50 C49 N4 123.7(11) . . ? C50 C49 C48 118.6(12) . . ? N4 C49 C48 117.6(12) . . ? C49 C50 C51 123.1(12) . . ? C50 C51 C46 118.6(12) . . ? O10 C52 N4 118.7(13) . . ? O10 C52 C53 122.7(13) . . ? N4 C52 C53 118.5(13) . . ? C54 C53 C58 120.0(14) . . ? C54 C53 C52 124.0(13) . . ? C58 C53 C52 116.0(15) . . ? C53 C54 C55 120.4(15) . . ? C56 C55 C54 119.4(18) . . ? C55 C56 C57 119.7(19) . . ? C58 C57 C56 122.4(18) . . ? C57 C58 C53 118.2(16) . . ? O5 C59 N5 111.8(9) . . ? N5 C60 C15 110.7(10) . . ? C62 C61 C66 116.6(12) . . ? C62 C61 N5 121.6(11) . . ? C66 C61 N5 121.7(12) . . ? C63 C62 C61 121.9(12) . . ? C62 C63 C64 122.7(13) . . ? C63 C64 N6 119.7(13) . . ? C63 C64 C65 116.2(12) . . ? N6 C64 C65 124.0(12) . . ? C66 C65 C64 121.1(12) . . ? C65 C66 C61 121.3(12) . . ? O11 C67 N6 120.8(13) . . ? O11 C67 C68 120.7(12) . . ? N6 C67 C68 118.5(12) . . ? C69 C68 C73 117.0(13) . . ? C69 C68 C67 124.3(14) . . ? C73 C68 C67 118.7(12) . . ? C68 C69 C70 120.7(15) . . ? C71 C70 C69 120.4(17) . . ? C70 C71 C72 120.1(17) . . ? C71 C72 C73 122.0(16) . . ? C72 C73 C68 119.7(14) . . ? N7 C74 O7 113.6(9) . . ? C21 C75 N7 110.7(9) . . ? C77 C76 N7 120.9(10) . . ? C77 C76 C81 117.7(11) . . ? N7 C76 C81 121.2(11) . . ? C78 C77 C76 121.4(11) . . ? C77 C78 C79 122.4(12) . . ? C78 C79 N8 119.1(11) . . ? C78 C79 C80 116.7(12) . . ? N8 C79 C80 124.2(11) . . ? C81 C80 C79 122.0(11) . . ? C80 C81 C76 119.7(11) . . ? O12 C82 N8 120.2(13) . . ? O12 C82 C83 120.7(14) . . ? N8 C82 C83 119.1(13) . . ? C88 C83 C84 118.5(15) . . ? C88 C83 C82 117.6(15) . . ? C84 C83 C82 123.9(14) . . ? C83 C84 C85 122.7(16) . . ? C86 C85 C84 118(2) . . ? C85 C86 C87 122(2) . . ? C88 C87 C86 117.2(19) . . ? C83 C88 C87 121.5(18) . . ? C90 C89 C6 109.6(9) . . ? C92 C91 C12 112.9(10) . . ? C18 C93 C94 113.3(10) . . ? C24 C95 C96 111.6(10) . . ? C104 N100 C101 108.2(13) . . ? C104 N100 C103 134(2) . . ? C101 N100 C103 104.1(11) . . ? C104 N100 C102 102.9(14) . . ? C101 N100 C102 105.0(11) . . ? C103 N100 C102 99.2(12) . . ? C110 C105 C106 120.3(18) . . ? C110 C105 N10 123.7(19) . . ? C106 C105 N10 116(2) . . ? C105 C106 C107 118.9(18) . . ? C108 C107 C106 121(2) . . ? C107 C108 C109 121(2) . . ? C108 C109 C110 120.9(18) . . ? C105 C110 C109 118.0(18) . . ? C116 C111 C112 125.9(18) . . ? C116 C111 N11 117.7(16) . . ? C112 C111 N11 116.4(18) . . ? C111 C112 C113 113.7(19) . . ? C112 C113 C114 120(2) . . ? C115 C114 C113 119(2) . . ? C114 C115 C116 122(2) . . ? C111 C116 C115 119.3(19) . . ? C122 C117 C118 129(2) . . ? C122 C117 N12 113(2) . . ? C118 C117 N12 117.8(19) . . ? C117 C118 C119 115.7(18) . . ? C120 C119 C118 122(2) . . ? C119 C120 C121 115(2) . . ? C122 C121 C120 124(2) . . ? C117 C122 C121 113(3) . . ? N13 C123 C124 122.7(17) . . ? N13 C123 C128 111.7(15) . . ? C124 C123 C128 125.2(15) . . ? C125 C124 C123 135.0(18) . . ? C124 C125 C126 99.4(16) . . ? C127 C126 C125 132.7(15) . . ? C126 C127 C128 119.3(15) . . ? C127 C128 C123 108.3(14) . . ? C130 O130 N136 81(5) . . ? C130 O130 C134 93(5) . . ? N136 O130 C134 149(4) . . ? O130 C130 N136 66(4) . . ? O130 C130 C134 60(4) . . ? N136 C130 C134 119(3) . . ? C135 C133 C134 135(3) 3 . ? O130 C134 C130 27(2) . . ? O130 C134 C133 82(3) . . ? C130 C134 C133 106(3) . . ? C133 C135 N136 128(2) 3 . ? C133 C135 C135 108(3) 3 3 ? N136 C135 C135 124(3) . 3 ? O135 N136 O130 149(3) . . ? O135 N136 C130 121(3) . . ? O130 N136 C130 32.3(19) . . ? O135 N136 C135 110(3) . . ? O130 N136 C135 99(2) . . ? C130 N136 C135 129(3) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 22.58 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.220 _refine_diff_density_min -0.608 _refine_diff_density_rms 0.099