# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2011 data_global _journal_name_full Chem.Commun. _journal_coden_cambridge 0182 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_email aakeroy@ksu.edu _publ_contact_author_name C.Aakeroy loop_ _publ_author_name C.Aakeroy 'Arbin Rajbanshi' 'John Desper' data_ar0721m_3 _database_code_depnum_ccdc_archive 'CCDC 833723' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; AI5 cavitand ; _chemical_name_common 'AI5 cavitand' _chemical_melting_point ? _chemical_formula_moiety ; (C70 H74 N4 O10 BR2) (C3 H6 O)2 (C6 H14)0.5 ; _chemical_formula_sum 'C79 H93 Br2 N4 O12' _chemical_formula_weight 1450.39 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' Br Br -0.2901 2.4595 '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)/m loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' '-x, -y, -z' 'x, -y-1/2, z' _cell_length_a 13.3457(7) _cell_length_b 19.5826(9) _cell_length_c 14.0550(8) _cell_angle_alpha 90.00 _cell_angle_beta 99.793(2) _cell_angle_gamma 90.00 _cell_volume 3619.7(3) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9902 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 27.80 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.331 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1522 _exptl_absorpt_coefficient_mu 1.184 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7327 _exptl_absorpt_correction_T_max 0.8907 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 45929 _diffrn_reflns_av_R_equivalents 0.0389 _diffrn_reflns_av_sigmaI/netI 0.0483 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 29.13 _reflns_number_total 9980 _reflns_number_gt 5982 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1500P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9980 _refine_ls_number_parameters 481 _refine_ls_number_restraints 44 _refine_ls_R_factor_all 0.1321 _refine_ls_R_factor_gt 0.0823 _refine_ls_wR_factor_ref 0.2791 _refine_ls_wR_factor_gt 0.2499 _refine_ls_goodness_of_fit_ref 1.251 _refine_ls_restrained_S_all 1.255 _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 Br1_1 Br 0.68616(5) 0.7500 0.14764(3) 0.05987(17) Uani 1 2 d S . . C11_1 C 0.6788(4) 0.7500 0.2797(3) 0.0385(10) Uani 1 2 d S . . C12_1 C 0.6771(2) 0.68871(15) 0.3286(2) 0.0376(7) Uani 1 1 d . . . O12_1 O 0.67956(18) 0.62809(11) 0.27735(15) 0.0411(5) Uani 1 1 d . . . C13_1 C 0.6731(2) 0.68759(15) 0.42742(19) 0.0332(7) Uani 1 1 d . . . C14_1 C 0.6712(3) 0.7500 0.4740(3) 0.0341(9) Uani 1 2 d S . . H14_1 H 0.6683 0.7500 0.5411 0.041 Uiso 1 2 calc SR . . C21_1 C 0.6677(2) 0.61957(15) 0.4799(2) 0.0351(7) Uani 1 1 d . . . H21A_1 H 0.7021 0.5844 0.4451 0.042 Uiso 1 1 calc R . . C22_1 C 0.7242(2) 0.62208(16) 0.5854(2) 0.0372(7) Uani 1 1 d . . . H22A_1 H 0.6972 0.6606 0.6190 0.045 Uiso 1 1 calc R . . H22B_1 H 0.7101 0.5794 0.6185 0.045 Uiso 1 1 calc R . . C23_1 C 0.8374(3) 0.6304(2) 0.5936(2) 0.0514(9) Uani 1 1 d . . . H23A_1 H 0.8520 0.6720 0.5584 0.062 Uiso 1 1 calc R . . H23B_1 H 0.8655 0.5907 0.5633 0.062 Uiso 1 1 calc R . . C24_1 C 0.8889(3) 0.6359(3) 0.6983(3) 0.0628(11) Uani 1 1 d . . . H24A_1 H 0.8587 0.6749 0.7282 0.075 Uiso 1 1 calc R . . H24B_1 H 0.8737 0.5940 0.7326 0.075 Uiso 1 1 calc R . . C25_1 C 1.0023(4) 0.6453(3) 0.7139(4) 0.0893(17) Uani 1 1 d . . . H25A_1 H 1.0189 0.6875 0.6809 0.107 Uiso 1 1 calc R . . H25B_1 H 1.0339 0.6063 0.6854 0.107 Uiso 1 1 calc R . . C26_1 C 1.0464(4) 0.6503(5) 0.8231(4) 0.123(3) Uani 1 1 d . . . H26A_1 H 1.1206 0.6460 0.8326 0.185 Uiso 1 1 calc R . . H26B_1 H 1.0182 0.6136 0.8578 0.185 Uiso 1 1 calc R . . H26C_1 H 1.0282 0.6946 0.8479 0.185 Uiso 1 1 calc R . . C27_1 C 0.5829(3) 0.59460(16) 0.2489(2) 0.0412(7) Uani 1 1 d . . . H27A_1 H 0.5279 0.6291 0.2414 0.049 Uiso 1 1 calc R . . H27B_1 H 0.5815 0.5721 0.1855 0.049 Uiso 1 1 calc R . . C11_2 C 0.4056(3) 0.55158(15) 0.3701(2) 0.0372(7) Uani 1 1 d . . . C12_2 C 0.3484(3) 0.56715(15) 0.4424(2) 0.0374(7) Uani 1 1 d . . . O12_2 O 0.24841(17) 0.54645(11) 0.42886(16) 0.0428(5) Uani 1 1 d . . . C13_2 C 0.3936(2) 0.60058(14) 0.5276(2) 0.0342(7) Uani 1 1 d . B . C14_2 C 0.4958(2) 0.61697(14) 0.5388(2) 0.0347(7) Uani 1 1 d . . . H14_2 H 0.5261 0.6407 0.5954 0.042 Uiso 1 1 calc R . . C15_2 C 0.5566(2) 0.59991(14) 0.4696(2) 0.0354(7) Uani 1 1 d . . . C16_2 C 0.5092(2) 0.56717(15) 0.38672(19) 0.0361(7) Uani 1 1 d . . . O16_2 O 0.56514(17) 0.54592(10) 0.31660(15) 0.0392(5) Uani 1 1 d . . . C17_2 C 0.3575(3) 0.52224(16) 0.2771(2) 0.0397(7) Uani 1 1 d . . . C21_2 C 0.3274(3) 0.61946(15) 0.6008(2) 0.0362(7) Uani 1 1 d D . . H21B_2 H 0.2733 0.5838 0.5976 0.043 Uiso 1 1 calc R A 1 C22A_2 C 0.3857(2) 0.62050(15) 0.7047(2) 0.0379(7) Uani 0.758(4) 1 d PD B 1 H22A_2 H 0.4221 0.5766 0.7177 0.046 Uiso 0.758(4) 1 calc PR B 1 H22B_2 H 0.4375 0.6571 0.7102 0.046 Uiso 0.758(4) 1 calc PR B 1 C23A_2 C 0.3207(4) 0.6317(3) 0.7816(3) 0.0430(10) Uani 0.758(4) 1 d PD B 1 H23A_2 H 0.2699 0.5945 0.7780 0.052 Uiso 0.758(4) 1 calc PR B 1 H23B_2 H 0.2834 0.6753 0.7689 0.052 Uiso 0.758(4) 1 calc PR B 1 C24A_2 C 0.3839(4) 0.6335(3) 0.8831(3) 0.0467(12) Uani 0.758(4) 1 d PD B 1 H24A_2 H 0.4218 0.5900 0.8946 0.056 Uiso 0.758(4) 1 calc PR B 1 H24B_2 H 0.4345 0.6708 0.8858 0.056 Uiso 0.758(4) 1 calc PR B 1 C25A_2 C 0.3245(4) 0.6440(3) 0.9632(3) 0.0561(13) Uani 0.758(4) 1 d PD B 1 H25A_2 H 0.2725 0.6077 0.9606 0.067 Uiso 0.758(4) 1 calc PR B 1 H25B_2 H 0.2889 0.6885 0.9545 0.067 Uiso 0.758(4) 1 calc PR B 1 C26A_2 C 0.3938(5) 0.6425(4) 1.0619(3) 0.0763(19) Uani 0.758(4) 1 d PD B 1 H26A_2 H 0.3521 0.6423 1.1130 0.115 Uiso 0.758(4) 1 calc PR B 1 H26B_2 H 0.4375 0.6830 1.0689 0.115 Uiso 0.758(4) 1 calc PR B 1 H26C_2 H 0.4360 0.6013 1.0670 0.115 Uiso 0.758(4) 1 calc PR B 1 C22B_2 C 0.3857(2) 0.62050(15) 0.7047(2) 0.0379(7) Uani 0.242(4) 1 d PD B 2 H22C_2 H 0.4279 0.6622 0.7165 0.046 Uiso 0.242(4) 1 calc PR B 2 H22D_2 H 0.4304 0.5800 0.7173 0.046 Uiso 0.242(4) 1 calc PR B 2 C23B_2 C 0.3025(8) 0.6196(10) 0.7704(5) 0.0430(10) Uani 0.242(4) 1 d PD B 2 H23C_2 H 0.2648 0.6633 0.7625 0.052 Uiso 0.242(4) 1 calc PR B 2 H23D_2 H 0.2535 0.5825 0.7485 0.052 Uiso 0.242(4) 1 calc PR B 2 C24B_2 C 0.3445(10) 0.6092(6) 0.8769(6) 0.0467(12) Uani 0.242(4) 1 d PD B 2 H24C_2 H 0.3883 0.5680 0.8843 0.056 Uiso 0.242(4) 1 calc PR B 2 H24D_2 H 0.2874 0.6010 0.9120 0.056 Uiso 0.242(4) 1 calc PR B 2 C25B_2 C 0.4063(11) 0.6702(7) 0.9220(7) 0.0561(13) Uani 0.242(4) 1 d PD B 2 H25C_2 H 0.4609 0.6803 0.8844 0.067 Uiso 0.242(4) 1 calc PR B 2 H25D_2 H 0.3615 0.7107 0.9185 0.067 Uiso 0.242(4) 1 calc PR B 2 C26B_2 C 0.4536(15) 0.6571(10) 1.0271(8) 0.0763(19) Uani 0.242(4) 1 d PD B 2 H26D_2 H 0.4025 0.6649 1.0685 0.115 Uiso 0.242(4) 1 calc PR B 2 H26E_2 H 0.5109 0.6883 1.0460 0.115 Uiso 0.242(4) 1 calc PR B 2 H26F_2 H 0.4777 0.6099 1.0343 0.115 Uiso 0.242(4) 1 calc PR B 2 C27_2 C 0.1738(3) 0.59504(18) 0.3963(2) 0.0472(8) Uani 1 1 d . . . H27A_2 H 0.1172 0.5725 0.3530 0.057 Uiso 1 1 calc R . . H27B_2 H 0.2030 0.6301 0.3583 0.057 Uiso 1 1 calc R . . N31_2 N 0.2992(2) 0.44924(15) -0.0526(2) 0.0487(7) Uani 1 1 d . . . C32_2 C 0.1998(3) 0.45363(18) -0.0822(2) 0.0468(8) Uani 1 1 d . . . N32_2 N 0.1720(2) 0.43924(18) -0.1806(2) 0.0568(9) Uani 1 1 d . . . H32_2 H 0.2183 0.4175 -0.2066 0.068 Uiso 1 1 calc R . . C33_2 C 0.1313(3) 0.4720(2) -0.0226(3) 0.0570(10) Uani 1 1 d . . . H33A_2 H 0.0603 0.4740 -0.0466 0.068 Uiso 1 1 calc R . . C34_2 C 0.1695(3) 0.4874(2) 0.0732(3) 0.0534(9) Uani 1 1 d . . . H34A_2 H 0.1246 0.4990 0.1164 0.064 Uiso 1 1 calc R . . C35_2 C 0.2724(3) 0.48569(16) 0.1051(2) 0.0416(8) Uani 1 1 d . . . C36_2 C 0.3339(3) 0.46576(18) 0.0396(2) 0.0438(8) Uani 1 1 d . . . H36A_2 H 0.4052 0.4637 0.0616 0.053 Uiso 1 1 calc R . . C37_2 C 0.3182(3) 0.50618(16) 0.2032(2) 0.0435(8) Uani 1 1 d . . . C38_2 C 0.0844(3) 0.4537(2) -0.2423(3) 0.0579(10) Uani 1 1 d . . . O38_2 O 0.0082(2) 0.4726(2) -0.2156(2) 0.0792(10) Uani 1 1 d . . . C39_2 C 0.0912(3) 0.4435(3) -0.3480(3) 0.0675(12) Uani 1 1 d . . . H39A_2 H 0.0334 0.4660 -0.3882 0.101 Uiso 1 1 calc R . . H39B_2 H 0.0899 0.3945 -0.3627 0.101 Uiso 1 1 calc R . . H39C_2 H 0.1547 0.4634 -0.3614 0.101 Uiso 1 1 calc R . . Br2_3 Br 0.00839(5) 0.7500 0.39269(5) 0.06497(18) Uani 1 2 d S . . C11_3 C 0.1357(4) 0.7500 0.4768(3) 0.0420(11) Uani 1 2 d S . . C12_3 C 0.1832(3) 0.68852(16) 0.5059(2) 0.0394(7) Uani 1 1 d . . . O12_3 O 0.13460(18) 0.62779(11) 0.47314(17) 0.0454(6) Uani 1 1 d . B . C13_3 C 0.2743(2) 0.68736(15) 0.5692(2) 0.0352(7) Uani 1 1 d . B . C14_3 C 0.3194(3) 0.7500 0.6000(3) 0.0325(9) Uani 1 2 d S . . H14_3 H 0.3825 0.7500 0.6431 0.039 Uiso 1 2 calc SR B . C31 C -0.3197(9) 0.6899(4) -0.1449(7) 0.0732(10) Uani 0.50 1 d PD C -1 H31A H -0.3444 0.6494 -0.1828 0.110 Uiso 0.50 1 calc PR C -1 H31B H -0.3447 0.6892 -0.0833 0.110 Uiso 0.50 1 calc PR C -1 H31C H -0.2451 0.6899 -0.1327 0.110 Uiso 0.50 1 calc PR C -1 C32 C -0.3573(5) 0.7527(6) -0.1998(4) 0.0732(10) Uani 0.50 1 d PD C -1 O32 O -0.4065(4) 0.7462(7) -0.2834(3) 0.0732(10) Uani 0.50 1 d PD C -1 C33 C -0.3380(10) 0.8179(5) -0.1552(8) 0.0732(10) Uani 0.50 1 d PD C -1 H33A H -0.2661 0.8297 -0.1519 0.110 Uiso 0.50 1 calc PR C -1 H33B H -0.3542 0.8164 -0.0898 0.110 Uiso 0.50 1 calc PR C -1 H33C H -0.3804 0.8524 -0.1932 0.110 Uiso 0.50 1 calc PR C -1 C41 C 0.0737(17) 0.7968(8) 0.116(3) 0.147(5) Uiso 0.25 1 d PD D -1 H41A H 0.1445 0.7926 0.1070 0.220 Uiso 0.25 1 calc PR D -1 H41B H 0.0721 0.8095 0.1836 0.220 Uiso 0.25 1 calc PR D -1 H41C H 0.0396 0.8321 0.0733 0.220 Uiso 0.25 1 calc PR D -1 C42 C 0.0201(11) 0.7296(7) 0.0943(15) 0.147(5) Uiso 0.25 1 d PD D -1 O42 O 0.0757(14) 0.6770(8) 0.1106(18) 0.147(5) Uiso 0.25 1 d PD D -1 C43 C -0.0646(15) 0.7283(13) 0.0159(18) 0.147(5) Uiso 0.25 1 d PD D -1 H43A H -0.0529 0.7611 -0.0337 0.220 Uiso 0.25 1 calc PR D -1 H43B H -0.1269 0.7405 0.0400 0.220 Uiso 0.25 1 calc PR D -1 H43C H -0.0717 0.6823 -0.0120 0.220 Uiso 0.25 1 calc PR D -1 C51 C 0.216(2) 0.7228(12) 0.167(2) 0.253(12) Uiso 0.25 1 d PD E -2 H51A H 0.1862 0.7523 0.1130 0.379 Uiso 0.50 2 calc SPR E -2 H51B H 0.1617 0.6960 0.1883 0.379 Uiso 0.25 1 calc PR E -2 H51C H 0.2652 0.6918 0.1454 0.379 Uiso 0.25 1 calc PR E -2 C52 C 0.2678(19) 0.7657(8) 0.249(2) 0.253(12) Uiso 0.25 1 d PD E -2 O52 O 0.252(2) 0.8293(9) 0.241(2) 0.253(12) Uiso 0.25 1 d PD E -2 C53 C 0.361(2) 0.742(2) 0.305(3) 0.253(12) Uiso 0.25 1 d PD E -2 H53A H 0.4171 0.7498 0.2686 0.379 Uiso 0.50 2 calc SPR E -2 H53B H 0.3559 0.6932 0.3177 0.379 Uiso 0.25 1 calc PR E -2 H53C H 0.3748 0.7672 0.3658 0.379 Uiso 0.25 1 calc PR E -2 C61 C -0.0316(8) 0.7968(12) 0.0912(17) 0.104(3) Uiso 0.25 1 d PD F -3 H61A H -0.0692 0.7562 0.1060 0.156 Uiso 0.25 1 calc PR F -3 H61B H -0.0666 0.8176 0.0313 0.156 Uiso 0.25 1 calc PR F -3 H61C H -0.0279 0.8297 0.1442 0.156 Uiso 0.25 1 calc PR F -3 C62 C 0.0762(8) 0.7760(10) 0.0789(11) 0.104(3) Uiso 0.25 1 d PD F -3 H62A H 0.0827 0.7258 0.0843 0.125 Uiso 0.25 1 calc PR F -3 H62B H 0.0873 0.7893 0.0135 0.125 Uiso 0.25 1 calc PR F -3 C63 C 0.1578(9) 0.8092(8) 0.1539(14) 0.104(3) Uiso 0.25 1 d PD F -3 H63A H 0.1252 0.8373 0.1986 0.125 Uiso 0.25 1 calc PR F -3 H63B H 0.2006 0.8396 0.1212 0.125 Uiso 0.25 1 calc PR F -3 C64 C 0.2253(8) 0.7536(10) 0.2118(12) 0.104(3) Uiso 0.25 1 d PD F -3 H64A H 0.1984 0.7429 0.2716 0.125 Uiso 0.25 1 calc PR F -3 H64B H 0.2227 0.7114 0.1727 0.125 Uiso 0.25 1 calc PR F -3 C65 C 0.3352(8) 0.7775(10) 0.2380(13) 0.104(3) Uiso 0.25 1 d PD F -3 H65A H 0.3362 0.8280 0.2425 0.125 Uiso 0.25 1 calc PR F -3 H65B H 0.3724 0.7643 0.1857 0.125 Uiso 0.25 1 calc PR F -3 C66 C 0.3902(12) 0.748(3) 0.3331(13) 0.104(3) Uiso 0.50 2 d SPD F -3 H66A H 0.4218 0.7043 0.3208 0.156 Uiso 0.25 1 calc PR F -3 H66B H 0.3413 0.7404 0.3768 0.156 Uiso 0.25 1 calc PR F -3 H66C H 0.4428 0.7799 0.3628 0.156 Uiso 0.25 1 calc PR F -3 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 Br1_1 0.0934(4) 0.0623(3) 0.0292(2) 0.000 0.0256(2) 0.000 C11_1 0.055(3) 0.044(2) 0.0190(16) 0.000 0.0142(17) 0.000 C12_1 0.0547(19) 0.0342(15) 0.0268(13) -0.0045(11) 0.0148(13) 0.0028(13) O12_1 0.0620(13) 0.0372(11) 0.0279(10) -0.0065(9) 0.0183(10) 0.0047(10) C13_1 0.0432(16) 0.0358(15) 0.0222(12) 0.0015(11) 0.0097(12) 0.0011(12) C14_1 0.045(2) 0.037(2) 0.0225(17) 0.000 0.0116(16) 0.000 C21_1 0.0498(17) 0.0300(14) 0.0271(13) -0.0010(11) 0.0117(12) 0.0060(13) C22_1 0.0532(18) 0.0336(15) 0.0259(13) 0.0021(12) 0.0099(13) 0.0028(13) C23_1 0.059(2) 0.059(2) 0.0359(17) 0.0021(16) 0.0066(16) 0.0062(17) C24_1 0.061(2) 0.086(3) 0.0404(19) 0.0000(19) 0.0067(18) 0.007(2) C25_1 0.060(3) 0.142(5) 0.064(3) -0.003(3) 0.004(2) 0.010(3) C26_1 0.073(3) 0.211(8) 0.079(4) -0.025(5) -0.006(3) 0.005(4) C27_1 0.0597(19) 0.0407(16) 0.0253(13) -0.0080(12) 0.0134(13) -0.0002(15) C11_2 0.0578(19) 0.0272(14) 0.0267(13) -0.0028(11) 0.0075(13) -0.0007(13) C12_2 0.0552(19) 0.0280(14) 0.0296(13) -0.0012(12) 0.0088(13) 0.0032(13) O12_2 0.0539(13) 0.0372(11) 0.0384(11) -0.0092(9) 0.0106(10) -0.0068(10) C13_2 0.0536(18) 0.0254(13) 0.0245(12) -0.0014(11) 0.0092(12) -0.0004(13) C14_2 0.0561(19) 0.0268(14) 0.0222(12) 0.0005(11) 0.0098(12) 0.0067(13) C15_2 0.0548(18) 0.0270(14) 0.0249(13) 0.0016(11) 0.0083(13) 0.0041(13) C16_2 0.0583(19) 0.0280(14) 0.0240(12) 0.0005(11) 0.0127(13) 0.0104(13) O16_2 0.0576(13) 0.0327(11) 0.0303(10) -0.0051(8) 0.0162(9) 0.0027(10) C17_2 0.0527(18) 0.0309(15) 0.0376(16) 0.0062(12) 0.0135(14) 0.0003(13) C21_2 0.0524(18) 0.0309(15) 0.0275(13) -0.0008(11) 0.0128(13) -0.0033(13) C22A_2 0.0584(19) 0.0292(14) 0.0279(13) 0.0017(11) 0.0122(13) 0.0050(14) C23A_2 0.062(2) 0.043(2) 0.0263(15) -0.0004(15) 0.0119(16) 0.0021(19) C24A_2 0.062(3) 0.048(3) 0.0308(18) 0.0060(19) 0.010(2) -0.001(2) C25A_2 0.075(3) 0.063(3) 0.030(2) 0.000(2) 0.010(2) -0.002(2) C26A_2 0.103(5) 0.088(4) 0.036(3) -0.003(3) 0.004(3) -0.021(4) C22B_2 0.0584(19) 0.0292(14) 0.0279(13) 0.0017(11) 0.0122(13) 0.0050(14) C23B_2 0.062(2) 0.043(2) 0.0263(15) -0.0004(15) 0.0119(16) 0.0021(19) C24B_2 0.062(3) 0.048(3) 0.0308(18) 0.0060(19) 0.010(2) -0.001(2) C25B_2 0.075(3) 0.063(3) 0.030(2) 0.000(2) 0.010(2) -0.002(2) C26B_2 0.103(5) 0.088(4) 0.036(3) -0.003(3) 0.004(3) -0.021(4) C27_2 0.054(2) 0.0474(19) 0.0379(16) -0.0098(15) 0.0018(15) -0.0017(16) N31_2 0.0573(17) 0.0564(17) 0.0325(13) -0.0129(12) 0.0074(12) 0.0087(14) C32_2 0.0505(19) 0.057(2) 0.0332(15) -0.0153(15) 0.0075(14) 0.0084(16) N32_2 0.0524(17) 0.080(2) 0.0373(14) -0.0253(15) 0.0061(13) 0.0099(16) C33_2 0.051(2) 0.081(3) 0.0390(18) -0.0183(18) 0.0076(16) 0.0087(19) C34_2 0.055(2) 0.071(2) 0.0353(16) -0.0168(16) 0.0130(15) 0.0035(18) C35_2 0.058(2) 0.0385(16) 0.0293(14) -0.0070(13) 0.0096(14) 0.0031(15) C36_2 0.0510(19) 0.0494(19) 0.0304(14) -0.0099(14) 0.0052(14) 0.0004(15) C37_2 0.060(2) 0.0328(16) 0.0409(17) -0.0030(13) 0.0187(16) 0.0019(15) C38_2 0.051(2) 0.081(3) 0.0420(18) -0.0217(19) 0.0092(16) -0.0001(19) O38_2 0.0532(15) 0.137(3) 0.0471(15) -0.0295(17) 0.0073(13) 0.0114(18) C39_2 0.054(2) 0.105(3) 0.045(2) -0.022(2) 0.0094(17) 0.007(2) Br2_3 0.0589(3) 0.0683(4) 0.0626(4) 0.000 -0.0042(3) 0.000 C11_3 0.048(3) 0.042(2) 0.034(2) 0.000 0.002(2) 0.000 C12_3 0.0485(18) 0.0391(17) 0.0315(14) -0.0043(13) 0.0096(13) -0.0036(14) O12_3 0.0517(13) 0.0412(12) 0.0434(12) -0.0109(10) 0.0085(11) -0.0047(10) C13_3 0.0471(17) 0.0333(15) 0.0277(13) -0.0025(11) 0.0134(13) -0.0013(13) C14_3 0.046(2) 0.0279(19) 0.0260(17) 0.000 0.0123(17) 0.000 C31 0.097(2) 0.0645(19) 0.0600(17) 0.029(4) 0.0197(17) 0.017(4) C32 0.097(2) 0.0645(19) 0.0600(17) 0.029(4) 0.0197(17) 0.017(4) O32 0.097(2) 0.0645(19) 0.0600(17) 0.029(4) 0.0197(17) 0.017(4) C33 0.097(2) 0.0645(19) 0.0600(17) 0.029(4) 0.0197(17) 0.017(4) _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 Br1_1 C11_1 1.876(4) . ? C11_1 C12_1 1.385(4) 4_575 ? C11_1 C12_1 1.385(4) . ? C12_1 O12_1 1.392(4) . ? C12_1 C13_1 1.400(4) . ? O12_1 C27_1 1.442(4) . ? C13_1 C14_1 1.389(3) . ? C13_1 C21_1 1.530(4) . ? C14_1 C13_1 1.389(3) 4_575 ? C14_1 H14_1 0.9500 . ? C21_1 C15_2 1.515(5) . ? C21_1 C22_1 1.546(4) . ? C21_1 H21A_1 1.0000 . ? C22_1 C23_1 1.504(5) . ? C22_1 H22A_1 0.9900 . ? C22_1 H22B_1 0.9900 . ? C23_1 C24_1 1.518(5) . ? C23_1 H23A_1 0.9900 . ? C23_1 H23B_1 0.9900 . ? C24_1 C25_1 1.504(6) . ? C24_1 H24A_1 0.9900 . ? C24_1 H24B_1 0.9900 . ? C25_1 C26_1 1.551(7) . ? C25_1 H25A_1 0.9900 . ? C25_1 H25B_1 0.9900 . ? C26_1 H26A_1 0.9800 . ? C26_1 H26B_1 0.9800 . ? C26_1 H26C_1 0.9800 . ? C27_1 O16_2 1.396(4) . ? C27_1 H27A_1 0.9900 . ? C27_1 H27B_1 0.9900 . ? C11_2 C16_2 1.396(5) . ? C11_2 C12_2 1.405(4) . ? C11_2 C17_2 1.472(4) . ? C12_2 O12_2 1.376(4) . ? C12_2 C13_2 1.407(4) . ? O12_2 C27_2 1.397(4) . ? C13_2 C14_2 1.383(4) . ? C13_2 C21_2 1.512(4) . ? C14_2 C15_2 1.408(4) . ? C14_2 H14_2 0.9500 . ? C15_2 C16_2 1.385(4) . ? C16_2 O16_2 1.397(3) . ? C17_2 C37_2 1.125(4) . ? C21_2 C22A_2 1.533(4) . ? C21_2 C13_3 1.536(4) . ? C21_2 H21B_2 1.0000 . ? C22A_2 C23A_2 1.512(5) . ? C22A_2 H22A_2 0.9900 . ? C22A_2 H22B_2 0.9900 . ? C23A_2 C24A_2 1.530(5) . ? C23A_2 H23A_2 0.9900 . ? C23A_2 H23B_2 0.9900 . ? C24A_2 C25A_2 1.497(5) . ? C24A_2 H24A_2 0.9900 . ? C24A_2 H24B_2 0.9900 . ? C25A_2 C26A_2 1.531(6) . ? C25A_2 H25A_2 0.9900 . ? C25A_2 H25B_2 0.9900 . ? C26A_2 H26A_2 0.9800 . ? C26A_2 H26B_2 0.9800 . ? C26A_2 H26C_2 0.9800 . ? C23B_2 C24B_2 1.519(8) . ? C23B_2 H23C_2 0.9900 . ? C23B_2 H23D_2 0.9900 . ? C24B_2 C25B_2 1.527(9) . ? C24B_2 H24C_2 0.9900 . ? C24B_2 H24D_2 0.9900 . ? C25B_2 C26B_2 1.526(9) . ? C25B_2 H25C_2 0.9900 . ? C25B_2 H25D_2 0.9900 . ? C26B_2 H26D_2 0.9800 . ? C26B_2 H26E_2 0.9800 . ? C26B_2 H26F_2 0.9800 . ? C27_2 O12_3 1.429(4) . ? C27_2 H27A_2 0.9900 . ? C27_2 H27B_2 0.9900 . ? N31_2 C32_2 1.324(5) . ? N31_2 C36_2 1.340(4) . ? C32_2 C33_2 1.389(5) . ? C32_2 N32_2 1.398(4) . ? N32_2 C38_2 1.362(5) . ? N32_2 H32_2 0.8800 . ? C33_2 C34_2 1.390(5) . ? C33_2 H33A_2 0.9500 . ? C34_2 C35_2 1.371(5) . ? C34_2 H34A_2 0.9500 . ? C35_2 C36_2 1.390(5) . ? C35_2 C37_2 1.466(5) . ? C36_2 H36A_2 0.9500 . ? C38_2 O38_2 1.201(5) . ? C38_2 C39_2 1.517(5) . ? C39_2 H39A_2 0.9800 . ? C39_2 H39B_2 0.9800 . ? C39_2 H39C_2 0.9800 . ? Br2_3 C11_3 1.897(5) . ? C11_3 C12_3 1.390(4) 4_575 ? C11_3 C12_3 1.390(4) . ? C12_3 C13_3 1.380(4) . ? C12_3 O12_3 1.395(4) . ? C13_3 C14_3 1.402(4) . ? C14_3 C13_3 1.402(4) 4_575 ? C14_3 H14_3 0.9500 . ? C31 C32 1.493(11) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 O32 1.250(8) . ? C32 C33 1.427(14) . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C41 C42 1.505(13) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 O42 1.267(11) . ? C42 C43 1.438(16) . ? C43 H43A 0.9800 . ? C43 H43B 0.9800 . ? C43 H43C 0.9800 . ? C51 C52 1.497(14) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 O52 1.264(11) . ? C52 C53 1.433(16) . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C61 C62 1.532(9) . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 C63 1.526(9) . ? C62 H62A 0.9900 . ? C62 H62B 0.9900 . ? C63 C64 1.553(10) . ? C63 H63A 0.9900 . ? C63 H63B 0.9900 . ? C64 C65 1.524(9) . ? C64 H64A 0.9900 . ? C64 H64B 0.9900 . ? C65 C66 1.526(10) . ? C65 H65A 0.9900 . ? C65 H65B 0.9900 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12_1 C11_1 C12_1 120.2(4) 4_575 . ? C12_1 C11_1 Br1_1 119.91(18) 4_575 . ? C12_1 C11_1 Br1_1 119.91(18) . . ? C11_1 C12_1 O12_1 118.6(3) . . ? C11_1 C12_1 C13_1 120.8(3) . . ? O12_1 C12_1 C13_1 120.5(3) . . ? C12_1 O12_1 C27_1 115.7(2) . . ? C14_1 C13_1 C12_1 117.5(3) . . ? C14_1 C13_1 C21_1 122.2(3) . . ? C12_1 C13_1 C21_1 120.3(3) . . ? C13_1 C14_1 C13_1 123.2(4) . 4_575 ? C13_1 C14_1 H14_1 118.4 . . ? C13_1 C14_1 H14_1 118.4 4_575 . ? C15_2 C21_1 C13_1 107.5(2) . . ? C15_2 C21_1 C22_1 114.2(2) . . ? C13_1 C21_1 C22_1 112.3(2) . . ? C15_2 C21_1 H21A_1 107.5 . . ? C13_1 C21_1 H21A_1 107.5 . . ? C22_1 C21_1 H21A_1 107.5 . . ? C23_1 C22_1 C21_1 113.4(3) . . ? C23_1 C22_1 H22A_1 108.9 . . ? C21_1 C22_1 H22A_1 108.9 . . ? C23_1 C22_1 H22B_1 108.9 . . ? C21_1 C22_1 H22B_1 108.9 . . ? H22A_1 C22_1 H22B_1 107.7 . . ? C22_1 C23_1 C24_1 111.4(3) . . ? C22_1 C23_1 H23A_1 109.3 . . ? C24_1 C23_1 H23A_1 109.3 . . ? C22_1 C23_1 H23B_1 109.3 . . ? C24_1 C23_1 H23B_1 109.3 . . ? H23A_1 C23_1 H23B_1 108.0 . . ? C25_1 C24_1 C23_1 115.4(4) . . ? C25_1 C24_1 H24A_1 108.4 . . ? C23_1 C24_1 H24A_1 108.4 . . ? C25_1 C24_1 H24B_1 108.4 . . ? C23_1 C24_1 H24B_1 108.4 . . ? H24A_1 C24_1 H24B_1 107.5 . . ? C24_1 C25_1 C26_1 110.8(4) . . ? C24_1 C25_1 H25A_1 109.5 . . ? C26_1 C25_1 H25A_1 109.5 . . ? C24_1 C25_1 H25B_1 109.5 . . ? C26_1 C25_1 H25B_1 109.5 . . ? H25A_1 C25_1 H25B_1 108.1 . . ? C25_1 C26_1 H26A_1 109.5 . . ? C25_1 C26_1 H26B_1 109.5 . . ? H26A_1 C26_1 H26B_1 109.5 . . ? C25_1 C26_1 H26C_1 109.5 . . ? H26A_1 C26_1 H26C_1 109.5 . . ? H26B_1 C26_1 H26C_1 109.5 . . ? O16_2 C27_1 O12_1 111.6(2) . . ? O16_2 C27_1 H27A_1 109.3 . . ? O12_1 C27_1 H27A_1 109.3 . . ? O16_2 C27_1 H27B_1 109.3 . . ? O12_1 C27_1 H27B_1 109.3 . . ? H27A_1 C27_1 H27B_1 108.0 . . ? C16_2 C11_2 C12_2 118.5(3) . . ? C16_2 C11_2 C17_2 120.2(3) . . ? C12_2 C11_2 C17_2 121.3(3) . . ? O12_2 C12_2 C11_2 118.0(3) . . ? O12_2 C12_2 C13_2 121.4(3) . . ? C11_2 C12_2 C13_2 120.6(3) . . ? C12_2 O12_2 C27_2 117.7(2) . . ? C14_2 C13_2 C12_2 118.5(3) . . ? C14_2 C13_2 C21_2 123.0(3) . . ? C12_2 C13_2 C21_2 118.5(3) . . ? C13_2 C14_2 C15_2 122.6(3) . . ? C13_2 C14_2 H14_2 118.7 . . ? C15_2 C14_2 H14_2 118.7 . . ? C16_2 C15_2 C14_2 117.2(3) . . ? C16_2 C15_2 C21_1 119.8(3) . . ? C14_2 C15_2 C21_1 122.9(3) . . ? C15_2 C16_2 C11_2 122.6(3) . . ? C15_2 C16_2 O16_2 120.6(3) . . ? C11_2 C16_2 O16_2 116.7(2) . . ? C27_1 O16_2 C16_2 116.8(2) . . ? C37_2 C17_2 C11_2 173.2(3) . . ? C13_2 C21_2 C22A_2 113.0(3) . . ? C13_2 C21_2 C13_3 108.0(2) . . ? C22A_2 C21_2 C13_3 113.5(2) . . ? C13_2 C21_2 H21B_2 107.4 . . ? C22A_2 C21_2 H21B_2 107.4 . . ? C13_3 C21_2 H21B_2 107.4 . . ? C23A_2 C22A_2 C21_2 115.0(3) . . ? C23A_2 C22A_2 H22A_2 108.5 . . ? C21_2 C22A_2 H22A_2 108.5 . . ? C23A_2 C22A_2 H22B_2 108.5 . . ? C21_2 C22A_2 H22B_2 108.5 . . ? H22A_2 C22A_2 H22B_2 107.5 . . ? C22A_2 C23A_2 C24A_2 112.2(4) . . ? C22A_2 C23A_2 H23A_2 109.2 . . ? C24A_2 C23A_2 H23A_2 109.2 . . ? C22A_2 C23A_2 H23B_2 109.2 . . ? C24A_2 C23A_2 H23B_2 109.2 . . ? H23A_2 C23A_2 H23B_2 107.9 . . ? C25A_2 C24A_2 C23A_2 115.2(4) . . ? C25A_2 C24A_2 H24A_2 108.5 . . ? C23A_2 C24A_2 H24A_2 108.5 . . ? C25A_2 C24A_2 H24B_2 108.5 . . ? C23A_2 C24A_2 H24B_2 108.5 . . ? H24A_2 C24A_2 H24B_2 107.5 . . ? C24A_2 C25A_2 C26A_2 111.3(4) . . ? C24A_2 C25A_2 H25A_2 109.4 . . ? C26A_2 C25A_2 H25A_2 109.4 . . ? C24A_2 C25A_2 H25B_2 109.4 . . ? C26A_2 C25A_2 H25B_2 109.4 . . ? H25A_2 C25A_2 H25B_2 108.0 . . ? C24B_2 C23B_2 H23C_2 108.8 . . ? C24B_2 C23B_2 H23D_2 108.8 . . ? H23C_2 C23B_2 H23D_2 107.7 . . ? C23B_2 C24B_2 C25B_2 112.7(9) . . ? C23B_2 C24B_2 H24C_2 109.0 . . ? C25B_2 C24B_2 H24C_2 109.0 . . ? C23B_2 C24B_2 H24D_2 109.0 . . ? C25B_2 C24B_2 H24D_2 109.0 . . ? H24C_2 C24B_2 H24D_2 107.8 . . ? C26B_2 C25B_2 C24B_2 112.1(9) . . ? C26B_2 C25B_2 H25C_2 109.2 . . ? C24B_2 C25B_2 H25C_2 109.2 . . ? C26B_2 C25B_2 H25D_2 109.2 . . ? C24B_2 C25B_2 H25D_2 109.2 . . ? H25C_2 C25B_2 H25D_2 107.9 . . ? C25B_2 C26B_2 H26D_2 109.5 . . ? C25B_2 C26B_2 H26E_2 109.5 . . ? H26D_2 C26B_2 H26E_2 109.5 . . ? C25B_2 C26B_2 H26F_2 109.5 . . ? H26D_2 C26B_2 H26F_2 109.5 . . ? H26E_2 C26B_2 H26F_2 109.5 . . ? O12_2 C27_2 O12_3 113.0(3) . . ? O12_2 C27_2 H27A_2 109.0 . . ? O12_3 C27_2 H27A_2 109.0 . . ? O12_2 C27_2 H27B_2 109.0 . . ? O12_3 C27_2 H27B_2 109.0 . . ? H27A_2 C27_2 H27B_2 107.8 . . ? C32_2 N31_2 C36_2 116.8(3) . . ? N31_2 C32_2 C33_2 123.7(3) . . ? N31_2 C32_2 N32_2 112.4(3) . . ? C33_2 C32_2 N32_2 123.9(3) . . ? C38_2 N32_2 C32_2 130.0(3) . . ? C38_2 N32_2 H32_2 115.0 . . ? C32_2 N32_2 H32_2 115.0 . . ? C32_2 C33_2 C34_2 118.0(3) . . ? C32_2 C33_2 H33A_2 121.0 . . ? C34_2 C33_2 H33A_2 121.0 . . ? C35_2 C34_2 C33_2 119.6(3) . . ? C35_2 C34_2 H34A_2 120.2 . . ? C33_2 C34_2 H34A_2 120.2 . . ? C34_2 C35_2 C36_2 117.5(3) . . ? C34_2 C35_2 C37_2 122.4(3) . . ? C36_2 C35_2 C37_2 120.1(3) . . ? N31_2 C36_2 C35_2 124.2(3) . . ? N31_2 C36_2 H36A_2 117.9 . . ? C35_2 C36_2 H36A_2 117.9 . . ? C17_2 C37_2 C35_2 176.8(4) . . ? O38_2 C38_2 N32_2 123.1(4) . . ? O38_2 C38_2 C39_2 122.8(4) . . ? N32_2 C38_2 C39_2 114.1(3) . . ? C38_2 C39_2 H39A_2 109.5 . . ? C38_2 C39_2 H39B_2 109.5 . . ? H39A_2 C39_2 H39B_2 109.5 . . ? C38_2 C39_2 H39C_2 109.5 . . ? H39A_2 C39_2 H39C_2 109.5 . . ? H39B_2 C39_2 H39C_2 109.5 . . ? C12_3 C11_3 C12_3 120.1(4) 4_575 . ? C12_3 C11_3 Br2_3 119.9(2) 4_575 . ? C12_3 C11_3 Br2_3 119.9(2) . . ? C13_3 C12_3 C11_3 120.8(3) . . ? C13_3 C12_3 O12_3 120.6(3) . . ? C11_3 C12_3 O12_3 118.6(3) . . ? C12_3 O12_3 C27_2 115.0(3) . . ? C12_3 C13_3 C14_3 118.0(3) . . ? C12_3 C13_3 C21_2 120.9(3) . . ? C14_3 C13_3 C21_2 121.0(3) . . ? C13_3 C14_3 C13_3 122.1(4) . 4_575 ? C13_3 C14_3 H14_3 118.9 . . ? C13_3 C14_3 H14_3 118.9 4_575 . ? O32 C32 C33 122.1(9) . . ? O32 C32 C31 118.6(10) . . ? C33 C32 C31 119.3(6) . . ? C42 C41 H41A 109.5 . . ? C42 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C42 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? O42 C42 C43 118.9(15) . . ? O42 C42 C41 115.5(12) . . ? C43 C42 C41 117.3(13) . . ? C42 C43 H43A 109.5 . . ? C42 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C42 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C52 C51 H51A 109.5 . . ? C52 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C52 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? O52 C52 C53 118.8(16) . . ? O52 C52 C51 116.2(16) . . ? C53 C52 C51 119.2(15) . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C63 C62 C61 112.5(10) . . ? C63 C62 H62A 109.1 . . ? C61 C62 H62A 109.1 . . ? C63 C62 H62B 109.1 . . ? C61 C62 H62B 109.1 . . ? H62A C62 H62B 107.8 . . ? C62 C63 C64 110.2(9) . . ? C62 C63 H63A 109.6 . . ? C64 C63 H63A 109.6 . . ? C62 C63 H63B 109.6 . . ? C64 C63 H63B 109.6 . . ? H63A C63 H63B 108.1 . . ? C65 C64 C63 111.1(10) . . ? C65 C64 H64A 109.4 . . ? C63 C64 H64A 109.4 . . ? C65 C64 H64B 109.4 . . ? C63 C64 H64B 109.4 . . ? H64A C64 H64B 108.0 . . ? C64 C65 C66 113.3(11) . . ? C64 C65 H65A 108.9 . . ? C66 C65 H65A 108.9 . . ? C64 C65 H65B 108.9 . . ? C66 C65 H65B 108.9 . . ? H65A C65 H65B 107.7 . . ? 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 C12_1 C11_1 C12_1 O12_1 -179.6(3) 4_575 . . . ? Br1_1 C11_1 C12_1 O12_1 -0.8(5) . . . . ? C12_1 C11_1 C12_1 C13_1 0.3(7) 4_575 . . . ? Br1_1 C11_1 C12_1 C13_1 179.1(3) . . . . ? C11_1 C12_1 O12_1 C27_1 -100.1(4) . . . . ? C13_1 C12_1 O12_1 C27_1 80.0(4) . . . . ? C11_1 C12_1 C13_1 C14_1 -0.1(5) . . . . ? O12_1 C12_1 C13_1 C14_1 179.8(3) . . . . ? C11_1 C12_1 C13_1 C21_1 178.0(3) . . . . ? O12_1 C12_1 C13_1 C21_1 -2.1(5) . . . . ? C12_1 C13_1 C14_1 C13_1 -0.1(6) . . . 4_575 ? C21_1 C13_1 C14_1 C13_1 -178.1(3) . . . 4_575 ? C14_1 C13_1 C21_1 C15_2 90.8(4) . . . . ? C12_1 C13_1 C21_1 C15_2 -87.2(3) . . . . ? C14_1 C13_1 C21_1 C22_1 -35.6(4) . . . . ? C12_1 C13_1 C21_1 C22_1 146.4(3) . . . . ? C15_2 C21_1 C22_1 C23_1 170.6(3) . . . . ? C13_1 C21_1 C22_1 C23_1 -66.6(3) . . . . ? C21_1 C22_1 C23_1 C24_1 177.3(3) . . . . ? C22_1 C23_1 C24_1 C25_1 -179.2(4) . . . . ? C23_1 C24_1 C25_1 C26_1 180.0(5) . . . . ? C12_1 O12_1 C27_1 O16_2 -93.3(3) . . . . ? C16_2 C11_2 C12_2 O12_2 -174.7(3) . . . . ? C17_2 C11_2 C12_2 O12_2 7.9(4) . . . . ? C16_2 C11_2 C12_2 C13_2 2.9(4) . . . . ? C17_2 C11_2 C12_2 C13_2 -174.5(3) . . . . ? C11_2 C12_2 O12_2 C27_2 -100.2(3) . . . . ? C13_2 C12_2 O12_2 C27_2 82.3(4) . . . . ? O12_2 C12_2 C13_2 C14_2 176.8(3) . . . . ? C11_2 C12_2 C13_2 C14_2 -0.7(4) . . . . ? O12_2 C12_2 C13_2 C21_2 -5.6(4) . . . . ? C11_2 C12_2 C13_2 C21_2 176.8(3) . . . . ? C12_2 C13_2 C14_2 C15_2 -1.7(4) . . . . ? C21_2 C13_2 C14_2 C15_2 -179.2(3) . . . . ? C13_2 C14_2 C15_2 C16_2 1.9(4) . . . . ? C13_2 C14_2 C15_2 C21_1 178.1(3) . . . . ? C13_1 C21_1 C15_2 C16_2 83.0(3) . . . . ? C22_1 C21_1 C15_2 C16_2 -151.7(3) . . . . ? C13_1 C21_1 C15_2 C14_2 -93.0(3) . . . . ? C22_1 C21_1 C15_2 C14_2 32.2(4) . . . . ? C14_2 C15_2 C16_2 C11_2 0.5(4) . . . . ? C21_1 C15_2 C16_2 C11_2 -175.8(3) . . . . ? C14_2 C15_2 C16_2 O16_2 -177.2(2) . . . . ? C21_1 C15_2 C16_2 O16_2 6.5(4) . . . . ? C12_2 C11_2 C16_2 C15_2 -2.8(4) . . . . ? C17_2 C11_2 C16_2 C15_2 174.6(3) . . . . ? C12_2 C11_2 C16_2 O16_2 174.9(2) . . . . ? C17_2 C11_2 C16_2 O16_2 -7.6(4) . . . . ? O12_1 C27_1 O16_2 C16_2 94.3(3) . . . . ? C15_2 C16_2 O16_2 C27_1 -84.2(3) . . . . ? C11_2 C16_2 O16_2 C27_1 98.0(3) . . . . ? C14_2 C13_2 C21_2 C22A_2 -32.0(4) . . . . ? C12_2 C13_2 C21_2 C22A_2 150.6(3) . . . . ? C14_2 C13_2 C21_2 C13_3 94.4(3) . . . . ? C12_2 C13_2 C21_2 C13_3 -83.1(3) . . . . ? C13_2 C21_2 C22A_2 C23A_2 -173.8(3) . . . . ? C13_3 C21_2 C22A_2 C23A_2 62.9(4) . . . . ? C21_2 C22A_2 C23A_2 C24A_2 -178.9(3) . . . . ? C22A_2 C23A_2 C24A_2 C25A_2 -179.6(4) . . . . ? C23A_2 C24A_2 C25A_2 C26A_2 177.9(5) . . . . ? C23B_2 C24B_2 C25B_2 C26B_2 -176.4(14) . . . . ? C12_2 O12_2 C27_2 O12_3 -93.7(3) . . . . ? C36_2 N31_2 C32_2 C33_2 -2.1(6) . . . . ? C36_2 N31_2 C32_2 N32_2 176.5(3) . . . . ? N31_2 C32_2 N32_2 C38_2 -162.3(4) . . . . ? C33_2 C32_2 N32_2 C38_2 16.3(7) . . . . ? N31_2 C32_2 C33_2 C34_2 0.7(6) . . . . ? N32_2 C32_2 C33_2 C34_2 -177.7(4) . . . . ? C32_2 C33_2 C34_2 C35_2 1.6(6) . . . . ? C33_2 C34_2 C35_2 C36_2 -2.4(6) . . . . ? C33_2 C34_2 C35_2 C37_2 175.4(4) . . . . ? C32_2 N31_2 C36_2 C35_2 1.2(5) . . . . ? C34_2 C35_2 C36_2 N31_2 1.1(5) . . . . ? C37_2 C35_2 C36_2 N31_2 -176.8(3) . . . . ? C32_2 N32_2 C38_2 O38_2 -12.8(7) . . . . ? C32_2 N32_2 C38_2 C39_2 167.5(4) . . . . ? C12_3 C11_3 C12_3 C13_3 4.7(7) 4_575 . . . ? Br2_3 C11_3 C12_3 C13_3 -178.1(3) . . . . ? C12_3 C11_3 C12_3 O12_3 -178.2(3) 4_575 . . . ? Br2_3 C11_3 C12_3 O12_3 -1.0(5) . . . . ? C13_3 C12_3 O12_3 C27_2 -80.4(4) . . . . ? C11_3 C12_3 O12_3 C27_2 102.5(4) . . . . ? O12_2 C27_2 O12_3 C12_3 92.9(3) . . . . ? C11_3 C12_3 C13_3 C14_3 -2.7(5) . . . . ? O12_3 C12_3 C13_3 C14_3 -179.7(3) . . . . ? C11_3 C12_3 C13_3 C21_2 -179.5(3) . . . . ? O12_3 C12_3 C13_3 C21_2 3.4(4) . . . . ? C13_2 C21_2 C13_3 C12_3 87.2(3) . . . . ? C22A_2 C21_2 C13_3 C12_3 -146.8(3) . . . . ? C13_2 C21_2 C13_3 C14_3 -89.6(3) . . . . ? C22A_2 C21_2 C13_3 C14_3 36.4(4) . . . . ? C12_3 C13_3 C14_3 C13_3 0.7(6) . . . 4_575 ? C21_2 C13_3 C14_3 C13_3 177.5(2) . . . 4_575 ? C61 C62 C63 C64 122.5(17) . . . . ? C62 C63 C64 C65 145.1(15) . . . . ? C63 C64 C65 C66 149(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 N32_2 H32_2 O12_1 0.88 2.03 2.903(4) 175.0 3_665 _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 29.13 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.441 _refine_diff_density_min -1.063 _refine_diff_density_rms 0.122 #END data_ar0712m_4 _database_code_depnum_ccdc_archive 'CCDC 833724' #TrackingRef '- all.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; AR-AI-11 pentyl (6-acetylamino-3-pyridyl)ethynyl cavitand ; _chemical_name_common 'AR-AI-11 pentyl (6-acetylamino-3-pyridyl)ethynyl cavitand' _chemical_melting_point ? _chemical_formula_moiety ; (C88 H88 N8 O12) (C7 H8)0.7 (C2 H5 O1)3.4 (C1 H3 O1)0.9 ( O1)0.5 ; _chemical_formula_sum 'C100.60 H113.30 N8 O16.80' _chemical_formula_weight 1703.29 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 14.7722(7) _cell_length_b 15.9370(8) _cell_length_c 22.1716(11) _cell_angle_alpha 109.733(3) _cell_angle_beta 96.094(3) _cell_angle_gamma 93.890(3) _cell_volume 4855.4(4) _cell_formula_units_Z 2 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used 9857 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 27.55 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.165 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1815 _exptl_absorpt_coefficient_mu 0.080 _exptl_absorpt_correction_type none _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 99701 _diffrn_reflns_av_R_equivalents 0.0575 _diffrn_reflns_av_sigmaI/netI 0.0738 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 0.99 _diffrn_reflns_theta_max 28.40 _reflns_number_total 23980 _reflns_number_gt 12858 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23980 _refine_ls_number_parameters 1136 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.1804 _refine_ls_R_factor_gt 0.1055 _refine_ls_wR_factor_ref 0.3241 _refine_ls_wR_factor_gt 0.2969 _refine_ls_goodness_of_fit_ref 1.806 _refine_ls_restrained_S_all 1.831 _refine_ls_shift/su_max 0.000 _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 C11_1 C 0.1335(2) 0.0864(2) 0.15757(17) 0.0276(8) Uani 1 1 d . . . C12_1 C 0.0776(2) 0.1414(2) 0.19694(17) 0.0273(8) Uani 1 1 d . . . C13_1 C 0.0811(2) 0.1527(2) 0.26172(17) 0.0259(8) Uani 1 1 d . . . C14_1 C 0.1414(2) 0.1054(2) 0.28701(18) 0.0277(8) Uani 1 1 d . . . H14_1 H 0.1442 0.1124 0.3315 0.033 Uiso 1 1 calc R . . C15_1 C 0.1979(2) 0.0479(2) 0.24955(17) 0.0269(8) Uani 1 1 d . B . C16_1 C 0.1932(3) 0.0402(2) 0.18465(18) 0.0298(8) Uani 1 1 d . . . O12_1 O 0.01529(16) 0.18108(16) 0.16709(11) 0.0295(6) Uani 1 1 d . . . O16_1 O 0.24551(17) -0.01658(16) 0.14346(12) 0.0321(6) Uani 1 1 d . . . C17_1 C 0.1338(3) 0.0810(2) 0.09106(19) 0.0317(9) Uani 1 1 d . . . C21_1 C 0.2670(3) 0.0000(2) 0.27697(18) 0.0314(8) Uani 1 1 d . . . H21_1 H 0.2766 -0.0545 0.2404 0.038 Uiso 1 1 calc R A 1 C22A_1 C 0.2357(3) -0.0327(3) 0.3293(2) 0.0398(10) Uiso 0.729(4) 1 d PD B 1 H22A_1 H 0.2147 0.0176 0.3631 0.048 Uiso 0.729(4) 1 calc PR B 1 H22B_1 H 0.2879 -0.0540 0.3497 0.048 Uiso 0.729(4) 1 calc PR B 1 C23A_1 C 0.1577(4) -0.1090(4) 0.3006(3) 0.0418(13) Uiso 0.729(4) 1 d PD B 1 H23A_1 H 0.1718 -0.1506 0.2590 0.050 Uiso 0.729(4) 1 calc PR B 1 H23B_1 H 0.1004 -0.0838 0.2916 0.050 Uiso 0.729(4) 1 calc PR B 1 C24A_1 C 0.1427(4) -0.1613(4) 0.3460(3) 0.0482(14) Uiso 0.729(4) 1 d PD B 1 H24A_1 H 0.1974 -0.1923 0.3508 0.058 Uiso 0.729(4) 1 calc PR B 1 H24B_1 H 0.1360 -0.1185 0.3892 0.058 Uiso 0.729(4) 1 calc PR B 1 C25A_1 C 0.0588(5) -0.2298(5) 0.3218(4) 0.0628(18) Uiso 0.729(4) 1 d PD B 1 H25A_1 H 0.0670 -0.2739 0.2794 0.075 Uiso 0.729(4) 1 calc PR B 1 H25B_1 H 0.0049 -0.1989 0.3148 0.075 Uiso 0.729(4) 1 calc PR B 1 C26A_1 C 0.0395(6) -0.2798(6) 0.3671(4) 0.086(2) Uiso 0.729(4) 1 d PD B 1 H26A_1 H -0.0159 -0.3222 0.3486 0.129 Uiso 0.729(4) 1 calc PR B 1 H26B_1 H 0.0303 -0.2369 0.4091 0.129 Uiso 0.729(4) 1 calc PR B 1 H26C_1 H 0.0915 -0.3126 0.3730 0.129 Uiso 0.729(4) 1 calc PR B 1 C22B_1 C 0.2357(3) -0.0327(3) 0.3293(2) 0.0398(10) Uiso 0.271(4) 1 d PD B 2 H22C_1 H 0.2218 0.0209 0.3641 0.048 Uiso 0.271(4) 1 calc PR B 2 H22D_1 H 0.1767 -0.0706 0.3103 0.048 Uiso 0.271(4) 1 calc PR B 2 C23B_1 C 0.2919(10) -0.0832(8) 0.3613(6) 0.0418(13) Uiso 0.271(4) 1 d PD B 2 H23C_1 H 0.2583 -0.0984 0.3932 0.050 Uiso 0.271(4) 1 calc PR B 2 H23D_1 H 0.3497 -0.0458 0.3846 0.050 Uiso 0.271(4) 1 calc PR B 2 C24B_1 C 0.3136(9) -0.1701(8) 0.3099(7) 0.0482(14) Uiso 0.271(4) 1 d PD B 2 H24C_1 H 0.3546 -0.1542 0.2820 0.058 Uiso 0.271(4) 1 calc PR B 2 H24D_1 H 0.3464 -0.2061 0.3320 0.058 Uiso 0.271(4) 1 calc PR B 2 C25B_1 C 0.2278(11) -0.2264(11) 0.2680(8) 0.0628(18) Uiso 0.271(4) 1 d PD B 2 H25C_1 H 0.2463 -0.2797 0.2353 0.075 Uiso 0.271(4) 1 calc PR B 2 H25D_1 H 0.1971 -0.1909 0.2445 0.075 Uiso 0.271(4) 1 calc PR B 2 C26B_1 C 0.1584(13) -0.2581(15) 0.3045(11) 0.086(2) Uiso 0.271(4) 1 d PD B 2 H26D_1 H 0.1170 -0.3089 0.2742 0.129 Uiso 0.271(4) 1 calc PR B 2 H26E_1 H 0.1228 -0.2089 0.3248 0.129 Uiso 0.271(4) 1 calc PR B 2 H26F_1 H 0.1909 -0.2767 0.3380 0.129 Uiso 0.271(4) 1 calc PR B 2 C27_1 C 0.3386(3) 0.0176(3) 0.14575(19) 0.0360(9) Uani 1 1 d . . . H27A_1 H 0.3572 -0.0066 0.1021 0.043 Uiso 1 1 calc R . . H27B_1 H 0.3431 0.0838 0.1585 0.043 Uiso 1 1 calc R . . N31_1 N 0.2566(3) 0.1202(3) -0.09013(18) 0.0530(10) Uani 1 1 d . . . C32_1 C 0.2281(3) 0.1285(3) -0.0334(2) 0.0492(12) Uani 1 1 d . . . H32_1 H 0.2574 0.1760 0.0039 0.059 Uiso 1 1 calc R . . C33_1 C 0.1584(3) 0.0719(3) -0.02573(18) 0.0356(9) Uani 1 1 d . . . C34_1 C 0.1144(3) 0.0036(3) -0.08171(19) 0.0368(9) Uani 1 1 d . . . H34_1 H 0.0646 -0.0353 -0.0791 0.044 Uiso 1 1 calc R . . C35_1 C 0.1435(3) -0.0068(3) -0.14035(19) 0.0392(10) Uani 1 1 d . . . H35_1 H 0.1147 -0.0528 -0.1787 0.047 Uiso 1 1 calc R . . C36_1 C 0.2163(3) 0.0519(3) -0.1418(2) 0.0404(10) Uani 1 1 d . . . N36_1 N 0.2555(3) 0.0455(3) -0.19740(17) 0.0496(10) Uani 1 1 d . . . H36_1 H 0.2944 0.0914 -0.1945 0.060 Uiso 1 1 calc R . . C37_1 C 0.1410(3) 0.0783(3) 0.03777(19) 0.0338(9) Uani 1 1 d . . . C38_1 C 0.2413(3) -0.0226(4) -0.2558(2) 0.0506(12) Uani 1 1 d . . . O38_1 O 0.1888(2) -0.0895(3) -0.26618(16) 0.0666(10) Uani 1 1 d . . . C39_1 C 0.2957(4) -0.0068(4) -0.3058(2) 0.0665(15) Uani 1 1 d . . . H39A_1 H 0.3545 0.0281 -0.2843 0.100 Uiso 1 1 calc R . . H39B_1 H 0.2612 0.0263 -0.3288 0.100 Uiso 1 1 calc R . . H39C_1 H 0.3064 -0.0647 -0.3367 0.100 Uiso 1 1 calc R . . C11_2 C 0.1212(2) 0.4451(2) 0.29860(17) 0.0259(8) Uani 1 1 d . . . C12_2 C 0.1774(2) 0.4812(2) 0.35901(17) 0.0250(8) Uani 1 1 d . . . C13_2 C 0.1830(2) 0.4350(2) 0.40206(16) 0.0237(8) Uani 1 1 d . . . C14_2 C 0.1331(2) 0.3511(2) 0.38322(16) 0.0236(7) Uani 1 1 d . . . H14_2 H 0.1391 0.3178 0.4115 0.028 Uiso 1 1 calc R . . C15_2 C 0.0747(2) 0.3131(2) 0.32467(16) 0.0235(7) Uani 1 1 d . . . C16_2 C 0.0691(2) 0.3628(2) 0.28372(16) 0.0254(8) Uani 1 1 d . . . O12_2 O 0.22330(16) 0.56599(16) 0.37420(12) 0.0280(6) Uani 1 1 d . . . O16_2 O 0.00925(16) 0.33233(16) 0.22583(11) 0.0286(6) Uani 1 1 d . . . C17_2 C 0.1211(3) 0.4848(2) 0.24950(18) 0.0306(8) Uani 1 1 d . . . C21_2 C 0.0237(2) 0.2187(2) 0.30367(16) 0.0248(8) Uani 1 1 d . . . H21_2 H -0.0335 0.2185 0.2751 0.030 Uiso 1 1 calc R . . C22_2 C -0.0065(2) 0.1924(2) 0.35966(17) 0.0264(8) Uani 1 1 d . . . H22A_2 H -0.0348 0.1293 0.3424 0.032 Uiso 1 1 calc R . . H22B_2 H 0.0482 0.1961 0.3907 0.032 Uiso 1 1 calc R . . C23_2 C -0.0745(3) 0.2515(2) 0.39532(18) 0.0313(9) Uani 1 1 d . . . H23A_2 H -0.0416 0.3106 0.4226 0.038 Uiso 1 1 calc R . . H23B_2 H -0.1206 0.2614 0.3633 0.038 Uiso 1 1 calc R . . C24_2 C -0.1231(3) 0.2111(3) 0.4376(2) 0.0370(9) Uani 1 1 d . . . H24A_2 H -0.0767 0.2013 0.4695 0.044 Uiso 1 1 calc R . . H24B_2 H -0.1554 0.1518 0.4101 0.044 Uiso 1 1 calc R . . C25_2 C -0.1922(3) 0.2689(3) 0.4739(2) 0.0391(10) Uani 1 1 d . . . H25A_2 H -0.1586 0.3234 0.5073 0.047 Uiso 1 1 calc R . . H25B_2 H -0.2317 0.2881 0.4431 0.047 Uiso 1 1 calc R . . C26_2 C -0.2518(3) 0.2210(3) 0.5057(2) 0.0557(13) Uani 1 1 d . . . H26A_2 H -0.2961 0.2603 0.5266 0.083 Uiso 1 1 calc R . . H26B_2 H -0.2136 0.2051 0.5383 0.083 Uiso 1 1 calc R . . H26C_2 H -0.2846 0.1663 0.4730 0.083 Uiso 1 1 calc R . . C27_2 C 0.0411(3) 0.2708(2) 0.17257(17) 0.0300(8) Uani 1 1 d . . . H27A_2 H 0.1087 0.2816 0.1774 0.036 Uiso 1 1 calc R . . H27B_2 H 0.0159 0.2804 0.1325 0.036 Uiso 1 1 calc R . . N31_2 N 0.1063(2) 0.6028(2) 0.07077(16) 0.0380(8) Uani 1 1 d . . . C32_2 C 0.1078(3) 0.5928(3) 0.12855(19) 0.0390(10) Uani 1 1 d . . . H32_2 H 0.1015 0.6441 0.1647 0.047 Uiso 1 1 calc R . . C33_2 C 0.1180(3) 0.5135(3) 0.13927(18) 0.0326(9) Uani 1 1 d . . . C34_2 C 0.1235(3) 0.4386(3) 0.0850(2) 0.0405(10) Uani 1 1 d . . . H34_2 H 0.1284 0.3819 0.0897 0.049 Uiso 1 1 calc R . . C35_2 C 0.1219(3) 0.4454(3) 0.0249(2) 0.0402(10) Uani 1 1 d . . . H35_2 H 0.1261 0.3946 -0.0121 0.048 Uiso 1 1 calc R . . C36_2 C 0.1140(3) 0.5296(3) 0.02004(18) 0.0333(9) Uani 1 1 d . . . N36_2 N 0.1110(2) 0.5468(2) -0.03811(14) 0.0334(7) Uani 1 1 d . . . H36_2 H 0.0985 0.6007 -0.0362 0.040 Uiso 1 1 calc R . . C37_2 C 0.1204(3) 0.5041(3) 0.20147(19) 0.0333(9) Uani 1 1 d . . . C38_2 C 0.1249(3) 0.4904(3) -0.0971(2) 0.0360(9) Uani 1 1 d . . . O38_2 O 0.1401(2) 0.4137(2) -0.10705(14) 0.0484(8) Uani 1 1 d . . . C39_2 C 0.1201(3) 0.5296(3) -0.15002(19) 0.0448(11) Uani 1 1 d . . . H39A_2 H 0.1054 0.5916 -0.1330 0.067 Uiso 1 1 calc R . . H39B_2 H 0.0724 0.4941 -0.1854 0.067 Uiso 1 1 calc R . . H39C_2 H 0.1794 0.5287 -0.1662 0.067 Uiso 1 1 calc R . . C11_3 C 0.4842(2) 0.4697(2) 0.40975(17) 0.0278(8) Uani 1 1 d . . . C12_3 C 0.5123(2) 0.3920(2) 0.41832(16) 0.0271(8) Uani 1 1 d . . . C13_3 C 0.4566(2) 0.3388(2) 0.44124(16) 0.0252(8) Uani 1 1 d . B . C14_3 C 0.3722(2) 0.3661(2) 0.45631(16) 0.0240(7) Uani 1 1 d . . . H14_3 H 0.3331 0.3297 0.4711 0.029 Uiso 1 1 calc R . . C15_3 C 0.3421(2) 0.4445(2) 0.45081(16) 0.0232(7) Uani 1 1 d . . . C16_3 C 0.3993(2) 0.4957(2) 0.42709(16) 0.0257(8) Uani 1 1 d . . . O12_3 O 0.60094(16) 0.37370(17) 0.40700(12) 0.0318(6) Uani 1 1 d . B . O16_3 O 0.37621(16) 0.57601(17) 0.42218(12) 0.0302(6) Uani 1 1 d . . . C17_3 C 0.5396(2) 0.5200(3) 0.38080(18) 0.0308(8) Uani 1 1 d . . . C21_3 C 0.2474(2) 0.4726(2) 0.46481(16) 0.0221(7) Uani 1 1 d . . . H21_3 H 0.2527 0.5394 0.4775 0.026 Uiso 1 1 calc R . . C22_3 C 0.2134(2) 0.4501(2) 0.52165(17) 0.0258(8) Uani 1 1 d . . . H22A_3 H 0.2012 0.3842 0.5094 0.031 Uiso 1 1 calc R . . H22B_3 H 0.2618 0.4720 0.5596 0.031 Uiso 1 1 calc R . . C23_3 C 0.1266(3) 0.4928(3) 0.53966(18) 0.0321(9) Uani 1 1 d . . . H23A_3 H 0.0820 0.4769 0.4999 0.039 Uiso 1 1 calc R . . H23B_3 H 0.1416 0.5588 0.5562 0.039 Uiso 1 1 calc R . . C24_3 C 0.0807(3) 0.4664(3) 0.5899(2) 0.0465(11) Uani 1 1 d . . . H24A_3 H 0.0269 0.5002 0.5979 0.056 Uiso 1 1 calc R . . H24B_3 H 0.0569 0.4022 0.5695 0.056 Uiso 1 1 calc R . . C25_3 C 0.1305(4) 0.4776(4) 0.6524(3) 0.0651(14) Uani 1 1 d . . . H25A_3 H 0.1808 0.4388 0.6463 0.078 Uiso 1 1 calc R . . H25B_3 H 0.0888 0.4577 0.6783 0.078 Uiso 1 1 calc R . . C26_3 C 0.1698(4) 0.5726(4) 0.6892(3) 0.0728(16) Uani 1 1 d . . . H26A_3 H 0.2008 0.5769 0.7317 0.109 Uiso 1 1 calc R . . H26B_3 H 0.1204 0.6115 0.6950 0.109 Uiso 1 1 calc R . . H26C_3 H 0.2140 0.5917 0.6651 0.109 Uiso 1 1 calc R . . C27_3 C 0.3171(2) 0.5704(3) 0.36574(18) 0.0320(9) Uani 1 1 d . . . H27A_3 H 0.3330 0.6235 0.3538 0.038 Uiso 1 1 calc R . . H27B_3 H 0.3270 0.5164 0.3296 0.038 Uiso 1 1 calc R . . N31_3 N 0.7148(3) 0.5928(2) 0.22948(17) 0.0440(9) Uani 1 1 d . . . C32_3 C 0.6600(3) 0.5577(3) 0.2611(2) 0.0439(11) Uani 1 1 d . . . H32_3 H 0.6315 0.4982 0.2396 0.053 Uiso 1 1 calc R . . C33_3 C 0.6422(3) 0.6024(3) 0.32309(19) 0.0357(9) Uani 1 1 d . . . C34_3 C 0.6827(3) 0.6884(3) 0.3529(2) 0.0456(11) Uani 1 1 d . . . H34_3 H 0.6709 0.7217 0.3952 0.055 Uiso 1 1 calc R . . C35_3 C 0.7404(3) 0.7280(3) 0.3227(2) 0.0464(11) Uani 1 1 d . . . H35_3 H 0.7692 0.7875 0.3435 0.056 Uiso 1 1 calc R . . C36_3 C 0.7544(3) 0.6764(3) 0.2604(2) 0.0370(10) Uani 1 1 d . . . N36_3 N 0.8127(2) 0.7071(2) 0.22427(17) 0.0422(9) Uani 1 1 d . . . H36_3 H 0.8239 0.6665 0.1884 0.051 Uiso 1 1 calc R . . C37_3 C 0.5836(3) 0.5572(3) 0.35444(19) 0.0348(9) Uani 1 1 d . . . C38_3 C 0.8540(3) 0.7915(3) 0.2375(2) 0.0492(12) Uani 1 1 d . . . O38_3 O 0.8463(3) 0.8543(2) 0.28513(18) 0.0634(10) Uani 1 1 d . . . C39_3 C 0.9122(4) 0.7993(3) 0.1868(3) 0.0624(15) Uani 1 1 d . . . H39A_3 H 0.9559 0.7545 0.1801 0.094 Uiso 1 1 calc R . . H39B_3 H 0.9457 0.8595 0.2016 0.094 Uiso 1 1 calc R . . H39C_3 H 0.8727 0.7890 0.1461 0.094 Uiso 1 1 calc R . . C11_4 C 0.5006(3) 0.1122(3) 0.26909(18) 0.0320(9) Uani 1 1 d . B . C12_4 C 0.4172(3) 0.0567(3) 0.25307(18) 0.0324(9) Uani 1 1 d . . . C13_4 C 0.3582(2) 0.0599(2) 0.29775(18) 0.0286(8) Uani 1 1 d . B . C14_4 C 0.3822(2) 0.1222(2) 0.35968(17) 0.0290(8) Uani 1 1 d . . . H14_4 H 0.3413 0.1262 0.3906 0.035 Uiso 1 1 calc R B . C15_4 C 0.4639(2) 0.1793(2) 0.37850(18) 0.0293(8) Uani 1 1 d . B . C16_4 C 0.5227(2) 0.1721(3) 0.33227(18) 0.0310(8) Uani 1 1 d . . . O12_4 O 0.39881(17) -0.00548(17) 0.18985(12) 0.0372(7) Uani 1 1 d . B . O16_4 O 0.60815(17) 0.22126(18) 0.34863(12) 0.0357(6) Uani 1 1 d . B . C17_4 C 0.5588(3) 0.1117(3) 0.22101(19) 0.0354(9) Uani 1 1 d . . . C21_4 C 0.4880(2) 0.2518(2) 0.44564(17) 0.0282(8) Uani 1 1 d . . . H21_4 H 0.5564 0.2616 0.4550 0.034 Uiso 1 1 calc R B . C22_4 C 0.4540(3) 0.2259(3) 0.50041(17) 0.0306(8) Uani 1 1 d . B . H22A_4 H 0.4701 0.2775 0.5413 0.037 Uiso 1 1 calc R . . H22B_4 H 0.3864 0.2139 0.4918 0.037 Uiso 1 1 calc R . . C23_4 C 0.4929(3) 0.1442(3) 0.5094(2) 0.0462(11) Uani 1 1 d . . . H23A_4 H 0.4724 0.0917 0.4696 0.055 Uiso 1 1 calc R B 1 H23B_4 H 0.5605 0.1542 0.5140 0.055 Uiso 1 1 calc R B 1 C24A_4 C 0.4669(4) 0.1220(3) 0.5659(2) 0.0597(13) Uiso 0.50 1 d PD B 1 H24A_4 H 0.4735 0.0582 0.5595 0.072 Uiso 0.50 1 calc PR B 1 H24B_4 H 0.4025 0.1324 0.5713 0.072 Uiso 0.50 1 calc PR B 1 C25A_4 C 0.5341(9) 0.1857(8) 0.6279(5) 0.085(3) Uiso 0.50 1 d PD B 1 H25A_4 H 0.5983 0.1783 0.6201 0.102 Uiso 0.50 1 calc PR B 1 H25B_4 H 0.5243 0.2490 0.6348 0.102 Uiso 0.50 1 calc PR B 1 C26A_4 C 0.5184(12) 0.1648(11) 0.6892(6) 0.129(4) Uiso 0.50 1 d PD B 1 H26A_4 H 0.5468 0.2150 0.7276 0.193 Uiso 0.50 1 calc PR B 1 H26B_4 H 0.5460 0.1102 0.6884 0.193 Uiso 0.50 1 calc PR B 1 H26C_4 H 0.4525 0.1558 0.6907 0.193 Uiso 0.50 1 calc PR B 1 O1A_4 O 0.1012(16) 0.1694(16) 0.5291(13) 0.298(12) Uiso 0.50 1 d PD C 1 C1A_4 C 0.1761(11) 0.1435(10) 0.4957(8) 0.110(5) Uiso 0.50 1 d PD C 1 H1A_4 H 0.2234 0.1956 0.5086 0.132 Uiso 0.50 1 calc PR C 1 H1B_4 H 0.1557 0.1267 0.4488 0.132 Uiso 0.50 1 calc PR C 1 C2A_4 C 0.2187(14) 0.0666(13) 0.5074(11) 0.169(8) Uiso 0.50 1 d PD C 1 H2A_4 H 0.2123 0.0156 0.4667 0.254 Uiso 0.50 1 calc PR C 1 H2B_4 H 0.1878 0.0492 0.5391 0.254 Uiso 0.50 1 calc PR C 1 H2C_4 H 0.2838 0.0848 0.5241 0.254 Uiso 0.50 1 calc PR C 1 C24B_4 C 0.4669(4) 0.1220(3) 0.5659(2) 0.0597(13) Uiso 0.50 1 d PD B -2 H24C_4 H 0.4589 0.1755 0.6031 0.072 Uiso 0.50 1 calc PR B -2 H24D_4 H 0.5090 0.0842 0.5799 0.072 Uiso 0.50 1 calc PR B -2 C25B_4 C 0.3704(8) 0.0662(8) 0.5253(6) 0.085(3) Uiso 0.50 1 d PD B -2 H25C_4 H 0.3318 0.1072 0.5122 0.102 Uiso 0.50 1 calc PR B -2 H25D_4 H 0.3826 0.0189 0.4856 0.102 Uiso 0.50 1 calc PR B -2 C26B_4 C 0.3206(11) 0.0244(11) 0.5643(8) 0.129(4) Uiso 0.50 1 d PD B -2 H26D_4 H 0.3193 0.0688 0.6073 0.193 Uiso 0.50 1 calc PR B -2 H26E_4 H 0.3516 -0.0261 0.5686 0.193 Uiso 0.50 1 calc PR B -2 H26F_4 H 0.2577 0.0027 0.5428 0.193 Uiso 0.50 1 calc PR B -2 O1B_4 O 0.0707(7) 0.0588(7) 0.4983(5) 0.127(4) Uiso 0.50 1 d PD D -2 C1B_4 C 0.0100(7) 0.0143(6) 0.4421(5) 0.055(2) Uiso 0.50 1 d PD D -2 H1C_4 H 0.0472 -0.0182 0.4088 0.066 Uiso 0.50 1 calc PR D -2 H1D_4 H -0.0158 0.0610 0.4275 0.066 Uiso 0.50 1 calc PR D -2 C2B_4 C -0.0674(6) -0.0496(6) 0.4402(5) 0.049(2) Uiso 0.50 1 d PD D -2 H2D_4 H -0.0944 -0.0817 0.3952 0.074 Uiso 0.50 1 calc PR D -2 H2E_4 H -0.1136 -0.0172 0.4644 0.074 Uiso 0.50 1 calc PR D -2 H2F_4 H -0.0458 -0.0926 0.4597 0.074 Uiso 0.50 1 calc PR D -2 C27_4 C 0.6106(3) 0.3090(3) 0.34670(18) 0.0364(10) Uani 1 1 d . . . H27A_4 H 0.5607 0.3107 0.3137 0.044 Uiso 1 1 calc R B . H27B_4 H 0.6695 0.3246 0.3334 0.044 Uiso 1 1 calc R . . N31_4 N 0.6967(2) 0.0827(2) 0.02600(15) 0.0368(8) Uani 1 1 d . . . C32_4 C 0.6455(3) 0.0756(3) 0.07089(19) 0.0380(10) Uani 1 1 d . B . H32_4 H 0.5940 0.0313 0.0573 0.046 Uiso 1 1 calc R . . C33_4 C 0.6629(3) 0.1287(3) 0.13583(18) 0.0343(9) Uani 1 1 d . . . C34_4 C 0.7380(3) 0.1939(3) 0.15454(19) 0.0358(9) Uani 1 1 d . B . H34_4 H 0.7526 0.2321 0.1985 0.043 Uiso 1 1 calc R . . C35_4 C 0.7911(3) 0.2030(3) 0.10915(19) 0.0350(9) Uani 1 1 d . . . H35_4 H 0.8423 0.2475 0.1211 0.042 Uiso 1 1 calc R B . C36_4 C 0.7679(3) 0.1455(3) 0.04548(18) 0.0316(9) Uani 1 1 d . B . N36_4 N 0.8196(2) 0.1438(2) -0.00439(15) 0.0335(8) Uani 1 1 d . . . H36_4 H 0.8057 0.0968 -0.0401 0.040 Uiso 1 1 calc R B . C37_4 C 0.6050(3) 0.1176(3) 0.18167(19) 0.0363(9) Uani 1 1 d . B . C38_4 C 0.8886(3) 0.2052(3) -0.00523(19) 0.0325(9) Uani 1 1 d . B . O38_4 O 0.91366(19) 0.27423(18) 0.04075(13) 0.0388(7) Uani 1 1 d . . . C39_4 C 0.9316(3) 0.1817(3) -0.0664(2) 0.0433(10) Uani 1 1 d . . . H39A_4 H 0.9023 0.1238 -0.0969 0.065 Uiso 1 1 calc R B . H39B_4 H 0.9972 0.1780 -0.0565 0.065 Uiso 1 1 calc R . . H39C_4 H 0.9235 0.2281 -0.0858 0.065 Uiso 1 1 calc R . . O1A_6 O 0.6553(12) 0.2934(10) -0.0087(7) 0.221(6) Uiso 0.60 1 d PD E 1 C1A_6 C 0.6765(8) 0.3185(7) -0.0565(5) 0.081(3) Uiso 0.60 1 d PD E 1 H1A_6 H 0.7341 0.3596 -0.0408 0.097 Uiso 0.60 1 calc PR E 1 H1B_6 H 0.6281 0.3540 -0.0662 0.097 Uiso 0.60 1 calc PR E 1 C2A_6 C 0.6898(14) 0.2430(11) -0.1235(7) 0.172(7) Uiso 0.60 1 d PD E 1 H2A_6 H 0.6832 0.2678 -0.1584 0.258 Uiso 0.60 1 calc PR E 1 H2B_6 H 0.6433 0.1916 -0.1332 0.258 Uiso 0.60 1 calc PR E 1 H2C_6 H 0.7510 0.2234 -0.1197 0.258 Uiso 0.60 1 calc PR E 1 O1B_6 O 0.6443(15) 0.3894(13) 0.0495(11) 0.193(8) Uiso 0.40 1 d PD F 2 C1B_6 C 0.5964(15) 0.2982(13) 0.0455(11) 0.122(7) Uiso 0.40 1 d PD F 2 H1D_6 H 0.6316 0.2501 0.0228 0.183 Uiso 0.40 1 calc PR F 2 H1E_6 H 0.5345 0.2888 0.0220 0.183 Uiso 0.40 1 calc PR F 2 H1F_6 H 0.5929 0.2979 0.0893 0.183 Uiso 0.40 1 calc PR F 2 O1A_7 O 0.3920(5) 0.2036(4) -0.1782(3) 0.066(2) Uani 0.50 1 d PD G -1 C1A_7 C 0.4393(9) 0.2127(9) -0.1116(6) 0.084(4) Uiso 0.50 1 d PD G -1 H1A_7 H 0.4891 0.2617 -0.1033 0.101 Uiso 0.50 1 calc PR G -1 H1B_7 H 0.3940 0.2399 -0.0831 0.101 Uiso 0.50 1 calc PR G -1 C2A_7 C 0.4813(10) 0.1552(9) -0.0790(7) 0.088(4) Uiso 0.50 1 d PD G -1 H2A_7 H 0.4660 0.1723 -0.0348 0.131 Uiso 0.50 1 calc PR G -1 H2B_7 H 0.5479 0.1627 -0.0776 0.131 Uiso 0.50 1 calc PR G -1 H2C_7 H 0.4577 0.0923 -0.1030 0.131 Uiso 0.50 1 calc PR G -1 O1E_7 O 0.4928(16) 0.6819(14) 0.2132(11) 0.243(8) Uiso 0.50 1 d P H -1 C1E_7 C 0.4189(12) 0.6066(12) 0.2096(9) 0.129(6) Uiso 0.50 1 d P H -1 H1I_7 H 0.4484 0.5570 0.2168 0.194 Uiso 0.50 1 calc PR H -1 H1J_7 H 0.3821 0.5851 0.1667 0.194 Uiso 0.50 1 calc PR H -1 H1K_7 H 0.3792 0.6298 0.2428 0.194 Uiso 0.50 1 calc PR H -1 O1F_7 O 0.6378(15) 0.4472(13) -0.0158(10) 0.231(8) Uiso 0.50 1 d P I -1 O1B_7 O 0.4338(14) 0.1653(15) -0.1649(10) 0.076(6) Uiso 0.20 1 d PD J 2 C1B_7 C 0.497(10) 0.121(4) -0.133(5) 0.65(16) Uiso 0.20 1 d PD J 2 H1C_7 H 0.5426 0.0962 -0.1620 0.783 Uiso 0.20 1 calc PR J 2 H1D_7 H 0.4618 0.0700 -0.1268 0.783 Uiso 0.20 1 calc PR J 2 C2B_7 C 0.5463(14) 0.1852(14) -0.0674(9) 0.040(5) Uiso 0.20 1 d PD J 2 H2D_7 H 0.5578 0.1517 -0.0381 0.061 Uiso 0.20 1 calc PR J 2 H2E_7 H 0.5079 0.2326 -0.0487 0.061 Uiso 0.20 1 calc PR J 2 H2F_7 H 0.6047 0.2121 -0.0735 0.061 Uiso 0.20 1 calc PR J 2 O1C_7 O 0.5672(6) 0.7055(5) 0.0696(4) 0.0316(19) Uiso 0.30 1 d PD K 3 C1C_7 C 0.6053(13) 0.6420(13) 0.1002(9) 0.071(5) Uiso 0.30 1 d PD K 3 H1E_7 H 0.6688 0.6625 0.1222 0.085 Uiso 0.30 1 calc PR K 3 H1F_7 H 0.6013 0.5798 0.0692 0.085 Uiso 0.30 1 calc PR K 3 C2C_7 C 0.5299(8) 0.6542(8) 0.1514(6) 0.029(3) Uiso 0.30 1 d PD K 3 H2G_7 H 0.5424 0.6170 0.1781 0.044 Uiso 0.30 1 calc PR K 3 H2H_7 H 0.4680 0.6354 0.1273 0.044 Uiso 0.30 1 calc PR K 3 H2I_7 H 0.5343 0.7172 0.1793 0.044 Uiso 0.30 1 calc PR K 3 O1D_7 O 0.6038(16) 0.7211(13) 0.1445(9) 0.250(9) Uiso 0.50 1 d PD L 4 C1D_7 C 0.6330(10) 0.6714(9) 0.0871(7) 0.085(4) Uiso 0.50 1 d PD L 4 H1G_7 H 0.7001 0.6876 0.0943 0.102 Uiso 0.50 1 calc PR L 4 H1H_7 H 0.6085 0.6984 0.0555 0.102 Uiso 0.50 1 calc PR L 4 C2D_7 C 0.6199(15) 0.5723(10) 0.0504(9) 0.163(8) Uiso 0.50 1 d PD L 4 H2J_7 H 0.6393 0.5604 0.0077 0.244 Uiso 0.50 1 calc PR L 4 H2K_7 H 0.5551 0.5498 0.0454 0.244 Uiso 0.50 1 calc PR L 4 H2L_7 H 0.6568 0.5418 0.0743 0.244 Uiso 0.50 1 calc PR L 4 C41_5 C 0.3539(3) 0.3061(4) 0.2065(2) 0.054(2) Uani 0.70 1 d PG M 1 C42_5 C 0.3090(3) 0.3571(4) 0.1754(3) 0.091(3) Uani 0.70 1 d PG M 1 H42_5 H 0.2578 0.3856 0.1917 0.109 Uiso 0.70 1 calc PR M 1 C43_5 C 0.3390(4) 0.3664(4) 0.1204(3) 0.092(3) Uani 0.70 1 d PG M 1 H43_5 H 0.3083 0.4013 0.0991 0.110 Uiso 0.70 1 calc PR M 1 C44_5 C 0.4139(4) 0.3247(5) 0.0966(3) 0.096(3) Uani 0.70 1 d PG M 1 H44_5 H 0.4344 0.3310 0.0590 0.115 Uiso 0.70 1 calc PR M 1 C45_5 C 0.4588(4) 0.2737(4) 0.1277(3) 0.088(3) Uani 0.70 1 d PG M 1 H45_5 H 0.5100 0.2452 0.1114 0.106 Uiso 0.70 1 calc PR M 1 C46_5 C 0.4288(3) 0.2644(4) 0.1827(3) 0.063(2) Uani 0.70 1 d PG M 1 H46_5 H 0.4595 0.2295 0.2040 0.076 Uiso 0.70 1 calc PR M 1 C47_5 C 0.3200(7) 0.2895(6) 0.2644(5) 0.0352(15) Uani 0.70 1 d P M 1 H47A_5 H 0.2660 0.3211 0.2751 0.053 Uiso 0.70 1 calc PR M 1 H47B_5 H 0.3685 0.3116 0.3016 0.053 Uiso 0.70 1 calc PR M 1 H47C_5 H 0.3037 0.2250 0.2538 0.053 Uiso 0.70 1 calc PR M 1 O1A_5 O 0.3833(12) 0.3998(11) 0.2307(8) 0.104(4) Uiso 0.30 1 d PD N 2 C1A_5 C 0.330(2) 0.3151(18) 0.2081(14) 0.104(4) Uiso 0.30 1 d PD N 2 H1A_5 H 0.3597 0.2713 0.1753 0.125 Uiso 0.30 1 calc PR N 2 H1B_5 H 0.2686 0.3203 0.1874 0.125 Uiso 0.30 1 calc PR N 2 C2A_5 C 0.319(3) 0.282(3) 0.265(2) 0.104(4) Uiso 0.30 1 d PD N 2 H2A_5 H 0.2563 0.2530 0.2602 0.156 Uiso 0.30 1 calc PR N 2 H2B_5 H 0.3309 0.3326 0.3061 0.156 Uiso 0.30 1 calc PR N 2 H2C_5 H 0.3625 0.2382 0.2658 0.156 Uiso 0.30 1 calc PR N 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 C11_1 0.0249(19) 0.0315(19) 0.0228(19) 0.0056(15) 0.0046(15) -0.0041(16) C12_1 0.0216(18) 0.0306(19) 0.0256(19) 0.0055(16) 0.0038(15) -0.0025(15) C13_1 0.0204(18) 0.0329(19) 0.0226(18) 0.0070(15) 0.0065(15) -0.0015(15) C14_1 0.0244(19) 0.033(2) 0.0238(19) 0.0069(16) 0.0074(15) -0.0026(16) C15_1 0.0231(18) 0.0282(19) 0.0257(19) 0.0045(15) 0.0056(15) -0.0002(15) C16_1 0.027(2) 0.0295(19) 0.027(2) 0.0014(16) 0.0089(16) -0.0016(16) O12_1 0.0260(13) 0.0377(14) 0.0219(13) 0.0067(11) 0.0026(11) 0.0024(11) O16_1 0.0263(14) 0.0376(14) 0.0259(14) 0.0016(11) 0.0083(11) 0.0026(11) C17_1 0.0244(19) 0.034(2) 0.032(2) 0.0053(17) 0.0046(17) 0.0036(16) C21_1 0.032(2) 0.030(2) 0.029(2) 0.0053(16) 0.0048(17) 0.0027(16) C27_1 0.030(2) 0.047(2) 0.025(2) 0.0035(18) 0.0101(17) 0.0030(18) N31_1 0.065(3) 0.053(2) 0.033(2) 0.0056(18) 0.018(2) -0.009(2) C32_1 0.061(3) 0.051(3) 0.027(2) 0.005(2) 0.010(2) -0.012(2) C33_1 0.038(2) 0.043(2) 0.023(2) 0.0085(17) 0.0076(18) 0.0049(19) C34_1 0.030(2) 0.046(2) 0.030(2) 0.0085(18) 0.0036(18) 0.0029(18) C35_1 0.034(2) 0.053(3) 0.023(2) 0.0044(18) 0.0001(17) 0.005(2) C36_1 0.043(2) 0.049(3) 0.027(2) 0.0102(19) 0.0089(19) 0.007(2) N36_1 0.057(2) 0.062(2) 0.029(2) 0.0127(18) 0.0132(18) 0.007(2) C37_1 0.033(2) 0.039(2) 0.025(2) 0.0044(17) 0.0080(17) 0.0038(17) C38_1 0.038(3) 0.070(3) 0.033(3) 0.003(2) 0.005(2) 0.015(2) O38_1 0.048(2) 0.090(3) 0.0376(19) -0.0084(18) 0.0062(16) 0.003(2) C39_1 0.070(4) 0.096(4) 0.034(3) 0.014(3) 0.023(3) 0.027(3) C11_2 0.0243(18) 0.0326(19) 0.0237(19) 0.0119(16) 0.0066(15) 0.0059(16) C12_2 0.0229(18) 0.0285(19) 0.0249(19) 0.0099(15) 0.0065(15) 0.0031(15) C13_2 0.0167(17) 0.035(2) 0.0220(18) 0.0101(15) 0.0083(14) 0.0061(15) C14_2 0.0187(17) 0.0335(19) 0.0196(17) 0.0093(15) 0.0057(14) 0.0055(15) C15_2 0.0171(17) 0.0326(19) 0.0211(18) 0.0081(15) 0.0072(14) 0.0049(14) C16_2 0.0191(17) 0.038(2) 0.0172(17) 0.0064(15) 0.0028(14) 0.0050(15) O12_2 0.0206(12) 0.0356(14) 0.0283(14) 0.0126(11) 0.0036(11) 0.0000(11) O16_2 0.0238(13) 0.0391(14) 0.0215(13) 0.0098(11) 0.0001(11) 0.0030(11) C17_2 0.026(2) 0.037(2) 0.026(2) 0.0091(17) 0.0015(16) 0.0029(16) C21_2 0.0186(17) 0.0345(19) 0.0214(18) 0.0092(15) 0.0055(14) 0.0021(15) C22_2 0.0250(18) 0.0314(19) 0.0228(18) 0.0081(15) 0.0084(15) 0.0019(15) C23_2 0.027(2) 0.034(2) 0.032(2) 0.0079(17) 0.0120(17) 0.0036(16) C24_2 0.038(2) 0.043(2) 0.033(2) 0.0141(18) 0.0161(19) 0.0034(19) C25_2 0.036(2) 0.052(3) 0.032(2) 0.0133(19) 0.0144(19) 0.007(2) C26_2 0.043(3) 0.064(3) 0.057(3) 0.010(2) 0.029(2) 0.003(2) C27_2 0.0270(19) 0.042(2) 0.0188(18) 0.0076(16) 0.0024(16) 0.0029(17) N31_2 0.048(2) 0.0418(19) 0.0285(18) 0.0160(16) 0.0088(16) 0.0054(16) C32_2 0.049(3) 0.043(2) 0.025(2) 0.0126(18) 0.0039(19) 0.007(2) C33_2 0.029(2) 0.049(2) 0.026(2) 0.0211(18) 0.0041(16) 0.0019(18) C34_2 0.049(3) 0.044(2) 0.035(2) 0.021(2) 0.009(2) 0.006(2) C35_2 0.050(3) 0.042(2) 0.033(2) 0.0156(19) 0.013(2) 0.007(2) C36_2 0.032(2) 0.047(2) 0.025(2) 0.0167(18) 0.0071(17) 0.0028(18) N36_2 0.0405(19) 0.0425(19) 0.0231(16) 0.0167(15) 0.0105(15) 0.0073(15) C37_2 0.029(2) 0.043(2) 0.032(2) 0.0187(18) 0.0053(17) 0.0021(17) C38_2 0.031(2) 0.045(2) 0.035(2) 0.0140(19) 0.0138(18) 0.0053(18) O38_2 0.063(2) 0.0516(19) 0.0385(17) 0.0181(15) 0.0267(16) 0.0158(16) C39_2 0.050(3) 0.063(3) 0.026(2) 0.017(2) 0.013(2) 0.012(2) C11_3 0.0232(18) 0.041(2) 0.0177(18) 0.0087(16) 0.0056(15) 0.0005(16) C12_3 0.0184(17) 0.041(2) 0.0183(18) 0.0047(16) 0.0035(15) 0.0034(16) C13_3 0.0193(17) 0.037(2) 0.0157(17) 0.0042(15) 0.0029(14) 0.0026(15) C14_3 0.0179(17) 0.0343(19) 0.0182(17) 0.0073(15) 0.0030(14) 0.0013(15) C15_3 0.0176(17) 0.0343(19) 0.0143(16) 0.0052(14) 0.0002(14) 0.0006(15) C16_3 0.0204(18) 0.034(2) 0.0202(18) 0.0070(15) 0.0034(15) 0.0007(15) O12_3 0.0179(12) 0.0462(16) 0.0256(14) 0.0041(12) 0.0069(11) 0.0017(11) O16_3 0.0234(13) 0.0381(14) 0.0291(14) 0.0121(12) 0.0049(11) -0.0012(11) C17_3 0.0200(18) 0.045(2) 0.025(2) 0.0090(17) 0.0028(16) 0.0027(17) C21_3 0.0181(17) 0.0286(18) 0.0201(17) 0.0081(15) 0.0066(14) 0.0019(14) C22_3 0.0217(18) 0.037(2) 0.0211(18) 0.0120(16) 0.0063(15) 0.0016(15) C23_3 0.027(2) 0.048(2) 0.028(2) 0.0178(18) 0.0118(16) 0.0081(17) C24_3 0.053(3) 0.059(3) 0.037(2) 0.022(2) 0.025(2) 0.014(2) C25_3 0.065(3) 0.081(4) 0.059(3) 0.032(3) 0.021(3) 0.015(3) C26_3 0.063(4) 0.080(4) 0.078(4) 0.029(3) 0.015(3) 0.015(3) C27_3 0.029(2) 0.043(2) 0.029(2) 0.0188(18) 0.0059(17) 0.0001(17) N31_3 0.053(2) 0.043(2) 0.038(2) 0.0133(17) 0.0228(18) 0.0023(18) C32_3 0.045(3) 0.047(2) 0.042(3) 0.016(2) 0.019(2) -0.002(2) C33_3 0.030(2) 0.051(3) 0.033(2) 0.020(2) 0.0151(18) 0.0107(19) C34_3 0.048(3) 0.057(3) 0.035(2) 0.015(2) 0.023(2) 0.003(2) C35_3 0.049(3) 0.047(3) 0.042(3) 0.010(2) 0.022(2) 0.001(2) C36_3 0.036(2) 0.048(3) 0.036(2) 0.021(2) 0.0174(19) 0.0113(19) N36_3 0.050(2) 0.046(2) 0.040(2) 0.0206(17) 0.0270(18) 0.0095(17) C37_3 0.028(2) 0.049(2) 0.029(2) 0.0144(19) 0.0076(17) 0.0083(18) C38_3 0.061(3) 0.047(3) 0.050(3) 0.023(2) 0.027(2) 0.012(2) O38_3 0.085(3) 0.0461(19) 0.064(2) 0.0197(18) 0.033(2) 0.0075(18) C39_3 0.072(4) 0.059(3) 0.074(4) 0.036(3) 0.043(3) 0.008(3) C11_4 0.026(2) 0.042(2) 0.026(2) 0.0060(17) 0.0106(16) 0.0102(17) C12_4 0.028(2) 0.037(2) 0.026(2) 0.0018(17) 0.0050(16) 0.0061(17) C13_4 0.0261(19) 0.0295(19) 0.029(2) 0.0068(16) 0.0084(16) 0.0069(16) C14_4 0.0259(19) 0.036(2) 0.0239(19) 0.0077(16) 0.0068(16) 0.0071(16) C15_4 0.0216(18) 0.039(2) 0.0255(19) 0.0075(16) 0.0061(16) 0.0091(16) C16_4 0.0222(19) 0.040(2) 0.027(2) 0.0062(17) 0.0045(16) 0.0050(16) O12_4 0.0289(14) 0.0427(16) 0.0298(15) -0.0017(12) 0.0064(12) 0.0067(12) O16_4 0.0219(13) 0.0454(16) 0.0326(15) 0.0028(12) 0.0089(12) 0.0031(12) C17_4 0.024(2) 0.046(2) 0.028(2) 0.0020(18) 0.0037(17) 0.0051(17) C21_4 0.0209(18) 0.038(2) 0.0224(19) 0.0052(16) 0.0036(15) 0.0075(16) C22_4 0.0261(19) 0.042(2) 0.0229(19) 0.0092(16) 0.0041(16) 0.0071(17) C23_4 0.048(3) 0.055(3) 0.047(3) 0.026(2) 0.016(2) 0.022(2) C27_4 0.026(2) 0.052(3) 0.026(2) 0.0049(18) 0.0140(17) -0.0001(18) N31_4 0.0335(19) 0.0438(19) 0.0287(18) 0.0058(15) 0.0104(15) 0.0003(16) C32_4 0.028(2) 0.047(2) 0.033(2) 0.0041(19) 0.0116(18) 0.0004(18) C33_4 0.030(2) 0.041(2) 0.027(2) 0.0037(17) 0.0099(17) 0.0076(18) C34_4 0.034(2) 0.041(2) 0.026(2) 0.0027(17) 0.0070(18) 0.0033(18) C35_4 0.031(2) 0.038(2) 0.030(2) 0.0048(17) 0.0048(18) -0.0008(17) C36_4 0.027(2) 0.036(2) 0.029(2) 0.0072(17) 0.0063(17) 0.0016(17) N36_4 0.0355(18) 0.0347(18) 0.0260(17) 0.0034(14) 0.0118(15) 0.0015(15) C37_4 0.028(2) 0.046(2) 0.027(2) 0.0019(18) 0.0031(18) 0.0050(18) C38_4 0.028(2) 0.039(2) 0.029(2) 0.0100(18) 0.0031(17) 0.0061(17) O38_4 0.0450(17) 0.0395(16) 0.0293(15) 0.0110(13) 0.0015(13) -0.0026(13) C39_4 0.039(2) 0.051(3) 0.042(3) 0.016(2) 0.016(2) 0.000(2) O1A_7 0.072(5) 0.040(4) 0.073(5) -0.004(4) 0.045(4) -0.017(4) C41_5 0.032(4) 0.073(5) 0.055(4) 0.024(4) -0.003(3) -0.010(4) C42_5 0.043(4) 0.155(9) 0.123(8) 0.102(8) 0.030(5) 0.036(5) C43_5 0.076(6) 0.138(8) 0.121(8) 0.098(7) 0.061(6) 0.071(6) C44_5 0.099(7) 0.135(9) 0.078(6) 0.063(7) 0.029(6) 0.029(7) C45_5 0.080(6) 0.114(7) 0.092(7) 0.053(6) 0.026(6) 0.044(6) C46_5 0.063(5) 0.079(5) 0.063(5) 0.036(4) 0.021(4) 0.029(4) C47_5 0.022(3) 0.034(3) 0.043(4) 0.006(3) 0.001(3) 0.004(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C11_1 C12_1 1.396(5) . ? C11_1 C16_1 1.398(5) . ? C11_1 C17_1 1.449(5) . ? C12_1 C13_1 1.381(5) . ? C12_1 O12_1 1.384(4) . ? C13_1 C14_1 1.396(5) . ? C13_1 C21_2 1.523(5) . ? C14_1 C15_1 1.401(5) . ? C14_1 H14_1 0.9500 . ? C15_1 C16_1 1.396(5) . ? C15_1 C21_1 1.510(5) . ? C16_1 O16_1 1.392(4) . ? O12_1 C27_2 1.416(4) . ? O16_1 C27_1 1.434(4) . ? C17_1 C37_1 1.184(5) . ? C21_1 C22A_1 1.523(5) . ? C21_1 C13_4 1.528(5) . ? C21_1 H21_1 1.0000 . ? C22A_1 C23A_1 1.531(7) . ? C22A_1 H22A_1 0.9900 . ? C22A_1 H22B_1 0.9900 . ? C23A_1 C24A_1 1.531(7) . ? C23A_1 H23A_1 0.9900 . ? C23A_1 H23B_1 0.9900 . ? C24A_1 C25A_1 1.515(8) . ? C24A_1 H24A_1 0.9900 . ? C24A_1 H24B_1 0.9900 . ? C25A_1 C26A_1 1.516(9) . ? C25A_1 H25A_1 0.9900 . ? C25A_1 H25B_1 0.9900 . ? C26A_1 H26A_1 0.9800 . ? C26A_1 H26B_1 0.9800 . ? C26A_1 H26C_1 0.9800 . ? C23B_1 C24B_1 1.545(14) . ? C23B_1 H23C_1 0.9900 . ? C23B_1 H23D_1 0.9900 . ? C24B_1 C25B_1 1.519(15) . ? C24B_1 H24C_1 0.9900 . ? C24B_1 H24D_1 0.9900 . ? C25B_1 C26B_1 1.531(16) . ? C25B_1 H25C_1 0.9900 . ? C25B_1 H25D_1 0.9900 . ? C26B_1 H26D_1 0.9800 . ? C26B_1 H26E_1 0.9800 . ? C26B_1 H26F_1 0.9800 . ? C27_1 O12_4 1.409(5) . ? C27_1 H27A_1 0.9900 . ? C27_1 H27B_1 0.9900 . ? N31_1 C36_1 1.333(5) . ? N31_1 C32_1 1.336(5) . ? C32_1 C33_1 1.384(6) . ? C32_1 H32_1 0.9500 . ? C33_1 C34_1 1.403(5) . ? C33_1 C37_1 1.429(5) . ? C34_1 C35_1 1.373(5) . ? C34_1 H34_1 0.9500 . ? C35_1 C36_1 1.387(6) . ? C35_1 H35_1 0.9500 . ? C36_1 N36_1 1.392(5) . ? N36_1 C38_1 1.364(6) . ? N36_1 H36_1 0.8800 . ? C38_1 O38_1 1.215(6) . ? C38_1 C39_1 1.512(7) . ? C39_1 H39A_1 0.9800 . ? C39_1 H39B_1 0.9800 . ? C39_1 H39C_1 0.9800 . ? C11_2 C16_2 1.392(5) . ? C11_2 C12_2 1.412(5) . ? C11_2 C17_2 1.432(5) . ? C12_2 O12_2 1.386(4) . ? C12_2 C13_2 1.387(5) . ? C13_2 C14_2 1.389(5) . ? C13_2 C21_3 1.510(5) . ? C14_2 C15_2 1.399(5) . ? C14_2 H14_2 0.9500 . ? C15_2 C16_2 1.392(5) . ? C15_2 C21_2 1.531(5) . ? C16_2 O16_2 1.395(4) . ? O12_2 C27_3 1.418(4) . ? O16_2 C27_2 1.406(4) . ? C17_2 C37_2 1.204(5) . ? C21_2 C22_2 1.536(5) . ? C21_2 H21_2 1.0000 . ? C22_2 C23_2 1.521(5) . ? C22_2 H22A_2 0.9900 . ? C22_2 H22B_2 0.9900 . ? C23_2 C24_2 1.515(5) . ? C23_2 H23A_2 0.9900 . ? C23_2 H23B_2 0.9900 . ? C24_2 C25_2 1.530(5) . ? C24_2 H24A_2 0.9900 . ? C24_2 H24B_2 0.9900 . ? C25_2 C26_2 1.504(6) . ? C25_2 H25A_2 0.9900 . ? C25_2 H25B_2 0.9900 . ? C26_2 H26A_2 0.9800 . ? C26_2 H26B_2 0.9800 . ? C26_2 H26C_2 0.9800 . ? C27_2 H27A_2 0.9900 . ? C27_2 H27B_2 0.9900 . ? N31_2 C36_2 1.341(5) . ? N31_2 C32_2 1.342(5) . ? C32_2 C33_2 1.377(5) . ? C32_2 H32_2 0.9500 . ? C33_2 C34_2 1.394(6) . ? C33_2 C37_2 1.433(5) . ? C34_2 C35_2 1.371(5) . ? C34_2 H34_2 0.9500 . ? C35_2 C36_2 1.394(6) . ? C35_2 H35_2 0.9500 . ? C36_2 N36_2 1.402(5) . ? N36_2 C38_2 1.359(5) . ? N36_2 H36_2 0.8800 . ? C38_2 O38_2 1.209(5) . ? C38_2 C39_2 1.502(6) . ? C39_2 H39A_2 0.9800 . ? C39_2 H39B_2 0.9800 . ? C39_2 H39C_2 0.9800 . ? C11_3 C12_3 1.397(5) . ? C11_3 C16_3 1.399(5) . ? C11_3 C17_3 1.447(5) . ? C12_3 O12_3 1.392(4) . ? C12_3 C13_3 1.393(5) . ? C13_3 C14_3 1.386(5) . ? C13_3 C21_4 1.521(5) . ? C14_3 C15_3 1.392(5) . ? C14_3 H14_3 0.9500 . ? C15_3 C16_3 1.396(5) . ? C15_3 C21_3 1.529(5) . ? C16_3 O16_3 1.383(4) . ? O12_3 C27_4 1.414(4) . ? O16_3 C27_3 1.421(4) . ? C17_3 C37_3 1.175(5) . ? C21_3 C22_3 1.544(4) . ? C21_3 H21_3 1.0000 . ? C22_3 C23_3 1.521(5) . ? C22_3 H22A_3 0.9900 . ? C22_3 H22B_3 0.9900 . ? C23_3 C24_3 1.521(5) . ? C23_3 H23A_3 0.9900 . ? C23_3 H23B_3 0.9900 . ? C24_3 C25_3 1.448(7) . ? C24_3 H24A_3 0.9900 . ? C24_3 H24B_3 0.9900 . ? C25_3 C26_3 1.498(8) . ? C25_3 H25A_3 0.9900 . ? C25_3 H25B_3 0.9900 . ? C26_3 H26A_3 0.9800 . ? C26_3 H26B_3 0.9800 . ? C26_3 H26C_3 0.9800 . ? C27_3 H27A_3 0.9900 . ? C27_3 H27B_3 0.9900 . ? N31_3 C36_3 1.333(5) . ? N31_3 C32_3 1.335(5) . ? C32_3 C33_3 1.381(6) . ? C32_3 H32_3 0.9500 . ? C33_3 C34_3 1.366(6) . ? C33_3 C37_3 1.460(5) . ? C34_3 C35_3 1.379(6) . ? C34_3 H34_3 0.9500 . ? C35_3 C36_3 1.395(6) . ? C35_3 H35_3 0.9500 . ? C36_3 N36_3 1.406(5) . ? N36_3 C38_3 1.361(6) . ? N36_3 H36_3 0.8800 . ? C38_3 O38_3 1.207(5) . ? C38_3 C39_3 1.518(6) . ? C39_3 H39A_3 0.9800 . ? C39_3 H39B_3 0.9800 . ? C39_3 H39C_3 0.9800 . ? C11_4 C16_4 1.392(5) . ? C11_4 C12_4 1.406(5) . ? C11_4 C17_4 1.437(5) . ? C12_4 C13_4 1.378(5) . ? C12_4 O12_4 1.402(4) . ? C13_4 C14_4 1.387(5) . ? C14_4 C15_4 1.395(5) . ? C14_4 H14_4 0.9500 . ? C15_4 C16_4 1.393(5) . ? C15_4 C21_4 1.532(5) . ? C16_4 O16_4 1.384(4) . ? O16_4 C27_4 1.412(5) . ? C17_4 C37_4 1.186(5) . ? C21_4 C22_4 1.529(5) . ? C21_4 H21_4 1.0000 . ? C22_4 C23_4 1.522(5) . ? C22_4 H22A_4 0.9900 . ? C22_4 H22B_4 0.9900 . ? C23_4 C24A_4 1.493(6) . ? C23_4 H23A_4 0.9900 . ? C23_4 H23B_4 0.9900 . ? C24A_4 C25A_4 1.593(11) . ? C24A_4 H24A_4 0.9900 . ? C24A_4 H24B_4 0.9900 . ? C25A_4 C26A_4 1.542(13) . ? C25A_4 H25A_4 0.9900 . ? C25A_4 H25B_4 0.9900 . ? C26A_4 H26A_4 0.9800 . ? C26A_4 H26B_4 0.9800 . ? C26A_4 H26C_4 0.9800 . ? O1A_4 C1A_4 1.404(15) . ? C1A_4 C2A_4 1.499(15) . ? C1A_4 H1A_4 0.9900 . ? C1A_4 H1B_4 0.9900 . ? C2A_4 H2A_4 0.9800 . ? C2A_4 H2B_4 0.9800 . ? C2A_4 H2C_4 0.9800 . ? C25B_4 C26B_4 1.480(13) . ? C25B_4 H25C_4 0.9900 . ? C25B_4 H25D_4 0.9900 . ? C26B_4 H26D_4 0.9800 . ? C26B_4 H26E_4 0.9800 . ? C26B_4 H26F_4 0.9800 . ? O1B_4 C1B_4 1.393(11) . ? C1B_4 C2B_4 1.465(11) . ? C1B_4 H1C_4 0.9900 . ? C1B_4 H1D_4 0.9900 . ? C2B_4 H2D_4 0.9800 . ? C2B_4 H2E_4 0.9800 . ? C2B_4 H2F_4 0.9800 . ? C27_4 H27A_4 0.9900 . ? C27_4 H27B_4 0.9900 . ? N31_4 C36_4 1.327(5) . ? N31_4 C32_4 1.342(5) . ? C32_4 C33_4 1.387(5) . ? C32_4 H32_4 0.9500 . ? C33_4 C34_4 1.392(5) . ? C33_4 C37_4 1.443(5) . ? C34_4 C35_4 1.378(5) . ? C34_4 H34_4 0.9500 . ? C35_4 C36_4 1.390(5) . ? C35_4 H35_4 0.9500 . ? C36_4 N36_4 1.403(5) . ? N36_4 C38_4 1.370(5) . ? N36_4 H36_4 0.8800 . ? C38_4 O38_4 1.223(4) . ? C38_4 C39_4 1.502(5) . ? C39_4 H39A_4 0.9800 . ? C39_4 H39B_4 0.9800 . ? C39_4 H39C_4 0.9800 . ? O1A_6 C1A_6 1.313(12) . ? C1A_6 C2A_6 1.605(13) . ? C1A_6 H1A_6 0.9900 . ? C1A_6 H1B_6 0.9900 . ? C2A_6 H2A_6 0.9800 . ? C2A_6 H2B_6 0.9800 . ? C2A_6 H2C_6 0.9800 . ? O1B_6 C1B_6 1.544(16) . ? C1B_6 H1D_6 0.9800 . ? C1B_6 H1E_6 0.9800 . ? C1B_6 H1F_6 0.9800 . ? O1A_7 C1A_7 1.521(12) . ? C1A_7 C2A_7 1.474(12) . ? C1A_7 H1A_7 0.9900 . ? C1A_7 H1B_7 0.9900 . ? C2A_7 H2A_7 0.9800 . ? C2A_7 H2B_7 0.9800 . ? C2A_7 H2C_7 0.9800 . ? O1E_7 C1E_7 1.54(2) . ? C1E_7 H1I_7 0.9800 . ? C1E_7 H1J_7 0.9800 . ? C1E_7 H1K_7 0.9800 . ? O1B_7 C1B_7 1.46(2) . ? C1B_7 C2B_7 1.55(2) . ? C1B_7 H1C_7 0.9900 . ? C1B_7 H1D_7 0.9900 . ? C2B_7 H2D_7 0.9800 . ? C2B_7 H2E_7 0.9800 . ? C2B_7 H2F_7 0.9800 . ? O1C_7 C1C_7 1.504(15) . ? C1C_7 C2C_7 1.648(16) . ? C1C_7 H1E_7 0.9900 . ? C1C_7 H1F_7 0.9900 . ? C2C_7 H2G_7 0.9800 . ? C2C_7 H2H_7 0.9800 . ? C2C_7 H2I_7 0.9800 . ? O1D_7 C1D_7 1.384(15) . ? C1D_7 C2D_7 1.501(14) . ? C1D_7 H1G_7 0.9900 . ? C1D_7 H1H_7 0.9900 . ? C2D_7 H2J_7 0.9800 . ? C2D_7 H2K_7 0.9800 . ? C2D_7 H2L_7 0.9800 . ? C41_5 C42_5 1.3900 . ? C41_5 C46_5 1.3900 . ? C41_5 C47_5 1.522(9) . ? C42_5 C43_5 1.3900 . ? C42_5 H42_5 0.9500 . ? C43_5 C44_5 1.3900 . ? C43_5 H43_5 0.9500 . ? C44_5 C45_5 1.3900 . ? C44_5 H44_5 0.9500 . ? C45_5 C46_5 1.3900 . ? C45_5 H45_5 0.9500 . ? C46_5 H46_5 0.9500 . ? C47_5 H47A_5 0.9800 . ? C47_5 H47B_5 0.9800 . ? C47_5 H47C_5 0.9800 . ? O1A_5 C1A_5 1.420(18) . ? C1A_5 C2A_5 1.552(19) . ? C1A_5 H1A_5 0.9900 . ? C1A_5 H1B_5 0.9900 . ? C2A_5 H2A_5 0.9800 . ? C2A_5 H2B_5 0.9800 . ? C2A_5 H2C_5 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C12_1 C11_1 C16_1 118.6(3) . . ? C12_1 C11_1 C17_1 120.9(3) . . ? C16_1 C11_1 C17_1 120.4(3) . . ? C13_1 C12_1 O12_1 121.5(3) . . ? C13_1 C12_1 C11_1 121.9(3) . . ? O12_1 C12_1 C11_1 116.6(3) . . ? C12_1 C13_1 C14_1 117.8(3) . . ? C12_1 C13_1 C21_2 119.8(3) . . ? C14_1 C13_1 C21_2 122.3(3) . . ? C13_1 C14_1 C15_1 122.7(3) . . ? C13_1 C14_1 H14_1 118.6 . . ? C15_1 C14_1 H14_1 118.6 . . ? C16_1 C15_1 C14_1 117.2(3) . . ? C16_1 C15_1 C21_1 119.3(3) . . ? C14_1 C15_1 C21_1 123.3(3) . . ? O16_1 C16_1 C15_1 121.2(3) . . ? O16_1 C16_1 C11_1 117.0(3) . . ? C15_1 C16_1 C11_1 121.7(3) . . ? C12_1 O12_1 C27_2 116.6(3) . . ? C16_1 O16_1 C27_1 116.6(3) . . ? C37_1 C17_1 C11_1 175.0(4) . . ? C15_1 C21_1 C22A_1 114.5(3) . . ? C15_1 C21_1 C13_4 108.1(3) . . ? C22A_1 C21_1 C13_4 113.9(3) . . ? C15_1 C21_1 H21_1 106.6 . . ? C22A_1 C21_1 H21_1 106.6 . . ? C13_4 C21_1 H21_1 106.6 . . ? C21_1 C22A_1 C23A_1 110.7(4) . . ? C21_1 C22A_1 H22A_1 109.5 . . ? C23A_1 C22A_1 H22A_1 109.5 . . ? C21_1 C22A_1 H22B_1 109.5 . . ? C23A_1 C22A_1 H22B_1 109.5 . . ? H22A_1 C22A_1 H22B_1 108.1 . . ? C22A_1 C23A_1 C24A_1 112.2(4) . . ? C22A_1 C23A_1 H23A_1 109.2 . . ? C24A_1 C23A_1 H23A_1 109.2 . . ? C22A_1 C23A_1 H23B_1 109.2 . . ? C24A_1 C23A_1 H23B_1 109.2 . . ? H23A_1 C23A_1 H23B_1 107.9 . . ? C25A_1 C24A_1 C23A_1 112.8(5) . . ? C25A_1 C24A_1 H24A_1 109.0 . . ? C23A_1 C24A_1 H24A_1 109.0 . . ? C25A_1 C24A_1 H24B_1 109.0 . . ? C23A_1 C24A_1 H24B_1 109.0 . . ? H24A_1 C24A_1 H24B_1 107.8 . . ? C24A_1 C25A_1 C26A_1 114.2(6) . . ? C24A_1 C25A_1 H25A_1 108.7 . . ? C26A_1 C25A_1 H25A_1 108.7 . . ? C24A_1 C25A_1 H25B_1 108.7 . . ? C26A_1 C25A_1 H25B_1 108.7 . . ? H25A_1 C25A_1 H25B_1 107.6 . . ? C25A_1 C26A_1 H26A_1 109.5 . . ? C25A_1 C26A_1 H26B_1 109.5 . . ? H26A_1 C26A_1 H26B_1 109.5 . . ? C25A_1 C26A_1 H26C_1 109.5 . . ? H26A_1 C26A_1 H26C_1 109.5 . . ? H26B_1 C26A_1 H26C_1 109.5 . . ? C24B_1 C23B_1 H23C_1 109.8 . . ? C24B_1 C23B_1 H23D_1 109.8 . . ? H23C_1 C23B_1 H23D_1 108.2 . . ? C25B_1 C24B_1 C23B_1 112.4(11) . . ? C25B_1 C24B_1 H24C_1 109.1 . . ? C23B_1 C24B_1 H24C_1 109.1 . . ? C25B_1 C24B_1 H24D_1 109.1 . . ? C23B_1 C24B_1 H24D_1 109.1 . . ? H24C_1 C24B_1 H24D_1 107.9 . . ? C24B_1 C25B_1 C26B_1 115.2(13) . . ? C24B_1 C25B_1 H25C_1 108.5 . . ? C26B_1 C25B_1 H25C_1 108.5 . . ? C24B_1 C25B_1 H25D_1 108.5 . . ? C26B_1 C25B_1 H25D_1 108.5 . . ? H25C_1 C25B_1 H25D_1 107.5 . . ? C25B_1 C26B_1 H26D_1 109.5 . . ? C25B_1 C26B_1 H26E_1 109.5 . . ? H26D_1 C26B_1 H26E_1 109.5 . . ? C25B_1 C26B_1 H26F_1 109.5 . . ? H26D_1 C26B_1 H26F_1 109.5 . . ? H26E_1 C26B_1 H26F_1 109.5 . . ? O12_4 C27_1 O16_1 111.9(3) . . ? O12_4 C27_1 H27A_1 109.2 . . ? O16_1 C27_1 H27A_1 109.2 . . ? O12_4 C27_1 H27B_1 109.2 . . ? O16_1 C27_1 H27B_1 109.2 . . ? H27A_1 C27_1 H27B_1 107.9 . . ? C36_1 N31_1 C32_1 117.3(4) . . ? N31_1 C32_1 C33_1 124.0(4) . . ? N31_1 C32_1 H32_1 118.0 . . ? C33_1 C32_1 H32_1 118.0 . . ? C32_1 C33_1 C34_1 117.1(4) . . ? C32_1 C33_1 C37_1 119.9(4) . . ? C34_1 C33_1 C37_1 122.7(4) . . ? C35_1 C34_1 C33_1 119.9(4) . . ? C35_1 C34_1 H34_1 120.1 . . ? C33_1 C34_1 H34_1 120.1 . . ? C34_1 C35_1 C36_1 117.9(4) . . ? C34_1 C35_1 H35_1 121.0 . . ? C36_1 C35_1 H35_1 121.0 . . ? N31_1 C36_1 C35_1 123.7(4) . . ? N31_1 C36_1 N36_1 112.7(4) . . ? C35_1 C36_1 N36_1 123.6(4) . . ? C38_1 N36_1 C36_1 128.5(4) . . ? C38_1 N36_1 H36_1 115.7 . . ? C36_1 N36_1 H36_1 115.7 . . ? C17_1 C37_1 C33_1 174.3(4) . . ? O38_1 C38_1 N36_1 122.2(4) . . ? O38_1 C38_1 C39_1 123.5(4) . . ? N36_1 C38_1 C39_1 114.3(5) . . ? C38_1 C39_1 H39A_1 109.5 . . ? C38_1 C39_1 H39B_1 109.5 . . ? H39A_1 C39_1 H39B_1 109.5 . . ? C38_1 C39_1 H39C_1 109.5 . . ? H39A_1 C39_1 H39C_1 109.5 . . ? H39B_1 C39_1 H39C_1 109.5 . . ? C16_2 C11_2 C12_2 118.4(3) . . ? C16_2 C11_2 C17_2 118.1(3) . . ? C12_2 C11_2 C17_2 123.3(3) . . ? O12_2 C12_2 C13_2 121.8(3) . . ? O12_2 C12_2 C11_2 116.9(3) . . ? C13_2 C12_2 C11_2 121.2(3) . . ? C12_2 C13_2 C14_2 117.9(3) . . ? C12_2 C13_2 C21_3 120.2(3) . . ? C14_2 C13_2 C21_3 121.7(3) . . ? C13_2 C14_2 C15_2 123.4(3) . . ? C13_2 C14_2 H14_2 118.3 . . ? C15_2 C14_2 H14_2 118.3 . . ? C16_2 C15_2 C14_2 116.8(3) . . ? C16_2 C15_2 C21_2 120.7(3) . . ? C14_2 C15_2 C21_2 122.4(3) . . ? C15_2 C16_2 C11_2 122.2(3) . . ? C15_2 C16_2 O16_2 120.9(3) . . ? C11_2 C16_2 O16_2 116.9(3) . . ? C12_2 O12_2 C27_3 116.7(3) . . ? C16_2 O16_2 C27_2 116.2(3) . . ? C37_2 C17_2 C11_2 169.4(4) . . ? C13_1 C21_2 C15_2 108.5(3) . . ? C13_1 C21_2 C22_2 113.8(3) . . ? C15_2 C21_2 C22_2 114.2(3) . . ? C13_1 C21_2 H21_2 106.6 . . ? C15_2 C21_2 H21_2 106.6 . . ? C22_2 C21_2 H21_2 106.6 . . ? C23_2 C22_2 C21_2 113.2(3) . . ? C23_2 C22_2 H22A_2 108.9 . . ? C21_2 C22_2 H22A_2 108.9 . . ? C23_2 C22_2 H22B_2 108.9 . . ? C21_2 C22_2 H22B_2 108.9 . . ? H22A_2 C22_2 H22B_2 107.8 . . ? C24_2 C23_2 C22_2 112.7(3) . . ? C24_2 C23_2 H23A_2 109.0 . . ? C22_2 C23_2 H23A_2 109.0 . . ? C24_2 C23_2 H23B_2 109.0 . . ? C22_2 C23_2 H23B_2 109.0 . . ? H23A_2 C23_2 H23B_2 107.8 . . ? C23_2 C24_2 C25_2 114.0(3) . . ? C23_2 C24_2 H24A_2 108.8 . . ? C25_2 C24_2 H24A_2 108.8 . . ? C23_2 C24_2 H24B_2 108.8 . . ? C25_2 C24_2 H24B_2 108.8 . . ? H24A_2 C24_2 H24B_2 107.7 . . ? C26_2 C25_2 C24_2 113.2(4) . . ? C26_2 C25_2 H25A_2 108.9 . . ? C24_2 C25_2 H25A_2 108.9 . . ? C26_2 C25_2 H25B_2 108.9 . . ? C24_2 C25_2 H25B_2 108.9 . . ? H25A_2 C25_2 H25B_2 107.7 . . ? C25_2 C26_2 H26A_2 109.5 . . ? C25_2 C26_2 H26B_2 109.5 . . ? H26A_2 C26_2 H26B_2 109.5 . . ? C25_2 C26_2 H26C_2 109.5 . . ? H26A_2 C26_2 H26C_2 109.5 . . ? H26B_2 C26_2 H26C_2 109.5 . . ? O16_2 C27_2 O12_1 111.6(3) . . ? O16_2 C27_2 H27A_2 109.3 . . ? O12_1 C27_2 H27A_2 109.3 . . ? O16_2 C27_2 H27B_2 109.3 . . ? O12_1 C27_2 H27B_2 109.3 . . ? H27A_2 C27_2 H27B_2 108.0 . . ? C36_2 N31_2 C32_2 117.0(3) . . ? N31_2 C32_2 C33_2 124.7(4) . . ? N31_2 C32_2 H32_2 117.6 . . ? C33_2 C32_2 H32_2 117.6 . . ? C32_2 C33_2 C34_2 116.4(3) . . ? C32_2 C33_2 C37_2 124.0(4) . . ? C34_2 C33_2 C37_2 119.6(4) . . ? C35_2 C34_2 C33_2 121.0(4) . . ? C35_2 C34_2 H34_2 119.5 . . ? C33_2 C34_2 H34_2 119.5 . . ? C34_2 C35_2 C36_2 117.6(4) . . ? C34_2 C35_2 H35_2 121.2 . . ? C36_2 C35_2 H35_2 121.2 . . ? N31_2 C36_2 C35_2 123.2(3) . . ? N31_2 C36_2 N36_2 112.7(3) . . ? C35_2 C36_2 N36_2 124.0(4) . . ? C38_2 N36_2 C36_2 128.1(3) . . ? C38_2 N36_2 H36_2 115.9 . . ? C36_2 N36_2 H36_2 115.9 . . ? C17_2 C37_2 C33_2 171.7(4) . . ? O38_2 C38_2 N36_2 122.9(4) . . ? O38_2 C38_2 C39_2 121.5(4) . . ? N36_2 C38_2 C39_2 115.6(4) . . ? C38_2 C39_2 H39A_2 109.5 . . ? C38_2 C39_2 H39B_2 109.5 . . ? H39A_2 C39_2 H39B_2 109.5 . . ? C38_2 C39_2 H39C_2 109.5 . . ? H39A_2 C39_2 H39C_2 109.5 . . ? H39B_2 C39_2 H39C_2 109.5 . . ? C12_3 C11_3 C16_3 118.5(3) . . ? C12_3 C11_3 C17_3 120.8(3) . . ? C16_3 C11_3 C17_3 120.6(3) . . ? O12_3 C12_3 C13_3 121.5(3) . . ? O12_3 C12_3 C11_3 116.7(3) . . ? C13_3 C12_3 C11_3 121.7(3) . . ? C14_3 C13_3 C12_3 117.6(3) . . ? C14_3 C13_3 C21_4 122.8(3) . . ? C12_3 C13_3 C21_4 119.5(3) . . ? C13_3 C14_3 C15_3 123.1(3) . . ? C13_3 C14_3 H14_3 118.4 . . ? C15_3 C14_3 H14_3 118.4 . . ? C14_3 C15_3 C16_3 117.6(3) . . ? C14_3 C15_3 C21_3 123.1(3) . . ? C16_3 C15_3 C21_3 119.1(3) . . ? O16_3 C16_3 C15_3 121.4(3) . . ? O16_3 C16_3 C11_3 117.2(3) . . ? C15_3 C16_3 C11_3 121.3(3) . . ? C12_3 O12_3 C27_4 116.8(3) . . ? C16_3 O16_3 C27_3 116.5(3) . . ? C37_3 C17_3 C11_3 176.7(4) . . ? C13_2 C21_3 C15_3 107.7(3) . . ? C13_2 C21_3 C22_3 114.4(3) . . ? C15_3 C21_3 C22_3 114.1(3) . . ? C13_2 C21_3 H21_3 106.7 . . ? C15_3 C21_3 H21_3 106.7 . . ? C22_3 C21_3 H21_3 106.7 . . ? C23_3 C22_3 C21_3 111.1(3) . . ? C23_3 C22_3 H22A_3 109.4 . . ? C21_3 C22_3 H22A_3 109.4 . . ? C23_3 C22_3 H22B_3 109.4 . . ? C21_3 C22_3 H22B_3 109.4 . . ? H22A_3 C22_3 H22B_3 108.0 . . ? C22_3 C23_3 C24_3 115.6(3) . . ? C22_3 C23_3 H23A_3 108.4 . . ? C24_3 C23_3 H23A_3 108.4 . . ? C22_3 C23_3 H23B_3 108.4 . . ? C24_3 C23_3 H23B_3 108.4 . . ? H23A_3 C23_3 H23B_3 107.4 . . ? C25_3 C24_3 C23_3 121.3(4) . . ? C25_3 C24_3 H24A_3 107.0 . . ? C23_3 C24_3 H24A_3 107.0 . . ? C25_3 C24_3 H24B_3 107.0 . . ? C23_3 C24_3 H24B_3 107.0 . . ? H24A_3 C24_3 H24B_3 106.8 . . ? C24_3 C25_3 C26_3 112.8(5) . . ? C24_3 C25_3 H25A_3 109.0 . . ? C26_3 C25_3 H25A_3 109.0 . . ? C24_3 C25_3 H25B_3 109.0 . . ? C26_3 C25_3 H25B_3 109.0 . . ? H25A_3 C25_3 H25B_3 107.8 . . ? C25_3 C26_3 H26A_3 109.5 . . ? C25_3 C26_3 H26B_3 109.5 . . ? H26A_3 C26_3 H26B_3 109.5 . . ? C25_3 C26_3 H26C_3 109.5 . . ? H26A_3 C26_3 H26C_3 109.5 . . ? H26B_3 C26_3 H26C_3 109.5 . . ? O12_2 C27_3 O16_3 112.7(3) . . ? O12_2 C27_3 H27A_3 109.0 . . ? O16_3 C27_3 H27A_3 109.0 . . ? O12_2 C27_3 H27B_3 109.0 . . ? O16_3 C27_3 H27B_3 109.0 . . ? H27A_3 C27_3 H27B_3 107.8 . . ? C36_3 N31_3 C32_3 117.1(4) . . ? N31_3 C32_3 C33_3 124.2(4) . . ? N31_3 C32_3 H32_3 117.9 . . ? C33_3 C32_3 H32_3 117.9 . . ? C34_3 C33_3 C32_3 117.1(4) . . ? C34_3 C33_3 C37_3 122.8(4) . . ? C32_3 C33_3 C37_3 120.1(4) . . ? C33_3 C34_3 C35_3 121.3(4) . . ? C33_3 C34_3 H34_3 119.3 . . ? C35_3 C34_3 H34_3 119.3 . . ? C34_3 C35_3 C36_3 116.8(4) . . ? C34_3 C35_3 H35_3 121.6 . . ? C36_3 C35_3 H35_3 121.6 . . ? N31_3 C36_3 C35_3 123.5(4) . . ? N31_3 C36_3 N36_3 113.3(3) . . ? C35_3 C36_3 N36_3 123.2(4) . . ? C38_3 N36_3 C36_3 128.5(4) . . ? C38_3 N36_3 H36_3 115.8 . . ? C36_3 N36_3 H36_3 115.8 . . ? C17_3 C37_3 C33_3 177.3(4) . . ? O38_3 C38_3 N36_3 123.7(4) . . ? O38_3 C38_3 C39_3 122.8(4) . . ? N36_3 C38_3 C39_3 113.5(4) . . ? C38_3 C39_3 H39A_3 109.5 . . ? C38_3 C39_3 H39B_3 109.5 . . ? H39A_3 C39_3 H39B_3 109.5 . . ? C38_3 C39_3 H39C_3 109.5 . . ? H39A_3 C39_3 H39C_3 109.5 . . ? H39B_3 C39_3 H39C_3 109.5 . . ? C16_4 C11_4 C12_4 117.9(3) . . ? C16_4 C11_4 C17_4 120.6(3) . . ? C12_4 C11_4 C17_4 121.3(3) . . ? C13_4 C12_4 O12_4 121.4(3) . . ? C13_4 C12_4 C11_4 122.0(3) . . ? O12_4 C12_4 C11_4 116.5(3) . . ? C12_4 C13_4 C14_4 117.9(3) . . ? C12_4 C13_4 C21_1 119.7(3) . . ? C14_4 C13_4 C21_1 122.3(3) . . ? C13_4 C14_4 C15_4 122.8(3) . . ? C13_4 C14_4 H14_4 118.6 . . ? C15_4 C14_4 H14_4 118.6 . . ? C16_4 C15_4 C14_4 117.4(3) . . ? C16_4 C15_4 C21_4 119.6(3) . . ? C14_4 C15_4 C21_4 122.8(3) . . ? O16_4 C16_4 C11_4 117.2(3) . . ? O16_4 C16_4 C15_4 120.8(3) . . ? C11_4 C16_4 C15_4 121.9(3) . . ? C12_4 O12_4 C27_1 116.5(3) . . ? C16_4 O16_4 C27_4 115.8(3) . . ? C37_4 C17_4 C11_4 175.1(4) . . ? C13_3 C21_4 C22_4 114.1(3) . . ? C13_3 C21_4 C15_4 107.8(3) . . ? C22_4 C21_4 C15_4 114.4(3) . . ? C13_3 C21_4 H21_4 106.7 . . ? C22_4 C21_4 H21_4 106.7 . . ? C15_4 C21_4 H21_4 106.7 . . ? C23_4 C22_4 C21_4 114.4(3) . . ? C23_4 C22_4 H22A_4 108.7 . . ? C21_4 C22_4 H22A_4 108.7 . . ? C23_4 C22_4 H22B_4 108.7 . . ? C21_4 C22_4 H22B_4 108.7 . . ? H22A_4 C22_4 H22B_4 107.6 . . ? C24A_4 C23_4 C22_4 115.5(4) . . ? C24A_4 C23_4 H23A_4 108.4 . . ? C22_4 C23_4 H23A_4 108.4 . . ? C24A_4 C23_4 H23B_4 108.4 . . ? C22_4 C23_4 H23B_4 108.4 . . ? H23A_4 C23_4 H23B_4 107.5 . . ? C23_4 C24A_4 C25A_4 106.9(6) . . ? C23_4 C24A_4 H24A_4 110.3 . . ? C25A_4 C24A_4 H24A_4 110.3 . . ? C23_4 C24A_4 H24B_4 110.3 . . ? C25A_4 C24A_4 H24B_4 110.3 . . ? H24A_4 C24A_4 H24B_4 108.6 . . ? C26A_4 C25A_4 C24A_4 112.0(9) . . ? C26A_4 C25A_4 H25A_4 109.2 . . ? C24A_4 C25A_4 H25A_4 109.2 . . ? C26A_4 C25A_4 H25B_4 109.2 . . ? C24A_4 C25A_4 H25B_4 109.2 . . ? H25A_4 C25A_4 H25B_4 107.9 . . ? O1A_4 C1A_4 C2A_4 114.4(14) . . ? O1A_4 C1A_4 H1A_4 108.7 . . ? C2A_4 C1A_4 H1A_4 108.7 . . ? O1A_4 C1A_4 H1B_4 108.7 . . ? C2A_4 C1A_4 H1B_4 108.7 . . ? H1A_4 C1A_4 H1B_4 107.6 . . ? C1A_4 C2A_4 H2A_4 109.5 . . ? C1A_4 C2A_4 H2B_4 109.5 . . ? H2A_4 C2A_4 H2B_4 109.5 . . ? C1A_4 C2A_4 H2C_4 109.5 . . ? H2A_4 C2A_4 H2C_4 109.5 . . ? H2B_4 C2A_4 H2C_4 109.5 . . ? C26B_4 C25B_4 H25C_4 109.4 . . ? C26B_4 C25B_4 H25D_4 109.4 . . ? H25C_4 C25B_4 H25D_4 108.0 . . ? C25B_4 C26B_4 H26D_4 109.5 . . ? C25B_4 C26B_4 H26E_4 109.5 . . ? H26D_4 C26B_4 H26E_4 109.5 . . ? C25B_4 C26B_4 H26F_4 109.5 . . ? H26D_4 C26B_4 H26F_4 109.5 . . ? H26E_4 C26B_4 H26F_4 109.5 . . ? O1B_4 C1B_4 C2B_4 122.2(9) . . ? O1B_4 C1B_4 H1C_4 106.8 . . ? C2B_4 C1B_4 H1C_4 106.8 . . ? O1B_4 C1B_4 H1D_4 106.8 . . ? C2B_4 C1B_4 H1D_4 106.8 . . ? H1C_4 C1B_4 H1D_4 106.6 . . ? C1B_4 C2B_4 H2D_4 109.5 . . ? C1B_4 C2B_4 H2E_4 109.5 . . ? H2D_4 C2B_4 H2E_4 109.5 . . ? C1B_4 C2B_4 H2F_4 109.5 . . ? H2D_4 C2B_4 H2F_4 109.5 . . ? H2E_4 C2B_4 H2F_4 109.5 . . ? O16_4 C27_4 O12_3 112.6(3) . . ? O16_4 C27_4 H27A_4 109.1 . . ? O12_3 C27_4 H27A_4 109.1 . . ? O16_4 C27_4 H27B_4 109.1 . . ? O12_3 C27_4 H27B_4 109.1 . . ? H27A_4 C27_4 H27B_4 107.8 . . ? C36_4 N31_4 C32_4 117.3(3) . . ? N31_4 C32_4 C33_4 124.2(4) . . ? N31_4 C32_4 H32_4 117.9 . . ? C33_4 C32_4 H32_4 117.9 . . ? C32_4 C33_4 C34_4 117.0(4) . . ? C32_4 C33_4 C37_4 121.5(4) . . ? C34_4 C33_4 C37_4 121.6(3) . . ? C35_4 C34_4 C33_4 119.8(3) . . ? C35_4 C34_4 H34_4 120.1 . . ? C33_4 C34_4 H34_4 120.1 . . ? C34_4 C35_4 C36_4 118.4(4) . . ? C34_4 C35_4 H35_4 120.8 . . ? C36_4 C35_4 H35_4 120.8 . . ? N31_4 C36_4 C35_4 123.3(3) . . ? N31_4 C36_4 N36_4 112.6(3) . . ? C35_4 C36_4 N36_4 124.0(3) . . ? C38_4 N36_4 C36_4 129.0(3) . . ? C38_4 N36_4 H36_4 115.5 . . ? C36_4 N36_4 H36_4 115.5 . . ? C17_4 C37_4 C33_4 177.4(4) . . ? O38_4 C38_4 N36_4 122.3(3) . . ? O38_4 C38_4 C39_4 122.2(4) . . ? N36_4 C38_4 C39_4 115.5(3) . . ? C38_4 C39_4 H39A_4 109.5 . . ? C38_4 C39_4 H39B_4 109.5 . . ? H39A_4 C39_4 H39B_4 109.5 . . ? C38_4 C39_4 H39C_4 109.5 . . ? H39A_4 C39_4 H39C_4 109.5 . . ? H39B_4 C39_4 H39C_4 109.5 . . ? O1A_6 C1A_6 C2A_6 118.8(11) . . ? O1A_6 C1A_6 H1A_6 107.6 . . ? C2A_6 C1A_6 H1A_6 107.6 . . ? O1A_6 C1A_6 H1B_6 107.6 . . ? C2A_6 C1A_6 H1B_6 107.6 . . ? H1A_6 C1A_6 H1B_6 107.0 . . ? C1A_6 C2A_6 H2A_6 109.5 . . ? C1A_6 C2A_6 H2B_6 109.5 . . ? H2A_6 C2A_6 H2B_6 109.5 . . ? C1A_6 C2A_6 H2C_6 109.5 . . ? H2A_6 C2A_6 H2C_6 109.5 . . ? H2B_6 C2A_6 H2C_6 109.5 . . ? O1B_6 C1B_6 H1D_6 109.5 . . ? O1B_6 C1B_6 H1E_6 109.5 . . ? H1D_6 C1B_6 H1E_6 109.5 . . ? O1B_6 C1B_6 H1F_6 109.5 . . ? H1D_6 C1B_6 H1F_6 109.5 . . ? H1E_6 C1B_6 H1F_6 109.5 . . ? C2A_7 C1A_7 O1A_7 138.3(11) . . ? C2A_7 C1A_7 H1A_7 102.5 . . ? O1A_7 C1A_7 H1A_7 102.5 . . ? C2A_7 C1A_7 H1B_7 102.5 . . ? O1A_7 C1A_7 H1B_7 102.5 . . ? H1A_7 C1A_7 H1B_7 104.9 . . ? C1A_7 C2A_7 H2A_7 109.5 . . ? C1A_7 C2A_7 H2B_7 109.5 . . ? H2A_7 C2A_7 H2B_7 109.5 . . ? C1A_7 C2A_7 H2C_7 109.5 . . ? H2A_7 C2A_7 H2C_7 109.5 . . ? H2B_7 C2A_7 H2C_7 109.5 . . ? O1E_7 C1E_7 H1I_7 109.5 . . ? O1E_7 C1E_7 H1J_7 109.5 . . ? H1I_7 C1E_7 H1J_7 109.5 . . ? O1E_7 C1E_7 H1K_7 109.5 . . ? H1I_7 C1E_7 H1K_7 109.5 . . ? H1J_7 C1E_7 H1K_7 109.5 . . ? O1B_7 C1B_7 C2B_7 112(2) . . ? O1B_7 C1B_7 H1C_7 109.1 . . ? C2B_7 C1B_7 H1C_7 109.1 . . ? O1B_7 C1B_7 H1D_7 109.1 . . ? C2B_7 C1B_7 H1D_7 109.1 . . ? H1C_7 C1B_7 H1D_7 107.9 . . ? C1B_7 C2B_7 H2D_7 109.5 . . ? C1B_7 C2B_7 H2E_7 109.5 . . ? H2D_7 C2B_7 H2E_7 109.5 . . ? C1B_7 C2B_7 H2F_7 109.5 . . ? H2D_7 C2B_7 H2F_7 109.5 . . ? H2E_7 C2B_7 H2F_7 109.5 . . ? O1C_7 C1C_7 C2C_7 95.1(10) . . ? O1C_7 C1C_7 H1E_7 112.7 . . ? C2C_7 C1C_7 H1E_7 112.7 . . ? O1C_7 C1C_7 H1F_7 112.7 . . ? C2C_7 C1C_7 H1F_7 112.7 . . ? H1E_7 C1C_7 H1F_7 110.2 . . ? C1C_7 C2C_7 H2G_7 109.5 . . ? C1C_7 C2C_7 H2H_7 109.5 . . ? H2G_7 C2C_7 H2H_7 109.5 . . ? C1C_7 C2C_7 H2I_7 109.5 . . ? H2G_7 C2C_7 H2I_7 109.5 . . ? H2H_7 C2C_7 H2I_7 109.5 . . ? O1D_7 C1D_7 C2D_7 130.7(15) . . ? O1D_7 C1D_7 H1G_7 104.6 . . ? C2D_7 C1D_7 H1G_7 104.6 . . ? O1D_7 C1D_7 H1H_7 104.6 . . ? C2D_7 C1D_7 H1H_7 104.6 . . ? H1G_7 C1D_7 H1H_7 105.7 . . ? C1D_7 C2D_7 H2J_7 109.5 . . ? C1D_7 C2D_7 H2K_7 109.5 . . ? H2J_7 C2D_7 H2K_7 109.5 . . ? C1D_7 C2D_7 H2L_7 109.5 . . ? H2J_7 C2D_7 H2L_7 109.5 . . ? H2K_7 C2D_7 H2L_7 109.5 . . ? C42_5 C41_5 C46_5 120.0 . . ? C42_5 C41_5 C47_5 121.8(5) . . ? C46_5 C41_5 C47_5 118.1(5) . . ? C43_5 C42_5 C41_5 120.0 . . ? C43_5 C42_5 H42_5 120.0 . . ? C41_5 C42_5 H42_5 120.0 . . ? C42_5 C43_5 C44_5 120.0 . . ? C42_5 C43_5 H43_5 120.0 . . ? C44_5 C43_5 H43_5 120.0 . . ? C45_5 C44_5 C43_5 120.0 . . ? C45_5 C44_5 H44_5 120.0 . . ? C43_5 C44_5 H44_5 120.0 . . ? C46_5 C45_5 C44_5 120.0 . . ? C46_5 C45_5 H45_5 120.0 . . ? C44_5 C45_5 H45_5 120.0 . . ? C45_5 C46_5 C41_5 120.0 . . ? C45_5 C46_5 H46_5 120.0 . . ? C41_5 C46_5 H46_5 120.0 . . ? C41_5 C47_5 H47A_5 109.5 . . ? C41_5 C47_5 H47B_5 109.5 . . ? H47A_5 C47_5 H47B_5 109.5 . . ? C41_5 C47_5 H47C_5 109.5 . . ? H47A_5 C47_5 H47C_5 109.5 . . ? H47B_5 C47_5 H47C_5 109.5 . . ? O1A_5 C1A_5 C2A_5 110.0(18) . . ? O1A_5 C1A_5 H1A_5 109.7 . . ? C2A_5 C1A_5 H1A_5 109.7 . . ? O1A_5 C1A_5 H1B_5 109.7 . . ? C2A_5 C1A_5 H1B_5 109.7 . . ? H1A_5 C1A_5 H1B_5 108.2 . . ? C1A_5 C2A_5 H2A_5 109.5 . . ? C1A_5 C2A_5 H2B_5 109.5 . . ? H2A_5 C2A_5 H2B_5 109.5 . . ? C1A_5 C2A_5 H2C_5 109.5 . . ? H2A_5 C2A_5 H2C_5 109.5 . . ? H2B_5 C2A_5 H2C_5 109.5 . . ? 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 C16_1 C11_1 C12_1 C13_1 1.3(5) . . . . ? C17_1 C11_1 C12_1 C13_1 -175.1(3) . . . . ? C16_1 C11_1 C12_1 O12_1 -175.8(3) . . . . ? C17_1 C11_1 C12_1 O12_1 7.8(5) . . . . ? O12_1 C12_1 C13_1 C14_1 175.6(3) . . . . ? C11_1 C12_1 C13_1 C14_1 -1.4(5) . . . . ? O12_1 C12_1 C13_1 C21_2 -7.5(5) . . . . ? C11_1 C12_1 C13_1 C21_2 175.6(3) . . . . ? C12_1 C13_1 C14_1 C15_1 0.2(5) . . . . ? C21_2 C13_1 C14_1 C15_1 -176.7(3) . . . . ? C13_1 C14_1 C15_1 C16_1 1.0(5) . . . . ? C13_1 C14_1 C15_1 C21_1 176.7(3) . . . . ? C14_1 C15_1 C16_1 O16_1 -178.8(3) . . . . ? C21_1 C15_1 C16_1 O16_1 5.3(5) . . . . ? C14_1 C15_1 C16_1 C11_1 -1.1(5) . . . . ? C21_1 C15_1 C16_1 C11_1 -177.0(3) . . . . ? C12_1 C11_1 C16_1 O16_1 177.8(3) . . . . ? C17_1 C11_1 C16_1 O16_1 -5.8(5) . . . . ? C12_1 C11_1 C16_1 C15_1 0.0(5) . . . . ? C17_1 C11_1 C16_1 C15_1 176.5(3) . . . . ? C13_1 C12_1 O12_1 C27_2 84.7(4) . . . . ? C11_1 C12_1 O12_1 C27_2 -98.2(4) . . . . ? C15_1 C16_1 O16_1 C27_1 -82.1(4) . . . . ? C11_1 C16_1 O16_1 C27_1 100.1(4) . . . . ? C16_1 C15_1 C21_1 C22A_1 -146.9(3) . . . . ? C14_1 C15_1 C21_1 C22A_1 37.4(5) . . . . ? C16_1 C15_1 C21_1 C13_4 84.9(4) . . . . ? C14_1 C15_1 C21_1 C13_4 -90.7(4) . . . . ? C15_1 C21_1 C22A_1 C23A_1 68.5(5) . . . . ? C13_4 C21_1 C22A_1 C23A_1 -166.4(4) . . . . ? C21_1 C22A_1 C23A_1 C24A_1 163.7(4) . . . . ? C22A_1 C23A_1 C24A_1 C25A_1 173.3(5) . . . . ? C23A_1 C24A_1 C25A_1 C26A_1 -177.3(6) . . . . ? C23B_1 C24B_1 C25B_1 C26B_1 -60(2) . . . . ? C16_1 O16_1 C27_1 O12_4 92.4(4) . . . . ? C36_1 N31_1 C32_1 C33_1 -1.6(7) . . . . ? N31_1 C32_1 C33_1 C34_1 -1.7(7) . . . . ? N31_1 C32_1 C33_1 C37_1 171.4(4) . . . . ? C32_1 C33_1 C34_1 C35_1 2.5(6) . . . . ? C37_1 C33_1 C34_1 C35_1 -170.4(4) . . . . ? C33_1 C34_1 C35_1 C36_1 -0.2(6) . . . . ? C32_1 N31_1 C36_1 C35_1 4.2(7) . . . . ? C32_1 N31_1 C36_1 N36_1 -175.6(4) . . . . ? C34_1 C35_1 C36_1 N31_1 -3.3(7) . . . . ? C34_1 C35_1 C36_1 N36_1 176.4(4) . . . . ? N31_1 C36_1 N36_1 C38_1 169.3(4) . . . . ? C35_1 C36_1 N36_1 C38_1 -10.5(7) . . . . ? C36_1 N36_1 C38_1 O38_1 0.5(8) . . . . ? C36_1 N36_1 C38_1 C39_1 179.9(4) . . . . ? C16_2 C11_2 C12_2 O12_2 -175.6(3) . . . . ? C17_2 C11_2 C12_2 O12_2 10.3(5) . . . . ? C16_2 C11_2 C12_2 C13_2 1.7(5) . . . . ? C17_2 C11_2 C12_2 C13_2 -172.4(3) . . . . ? O12_2 C12_2 C13_2 C14_2 178.7(3) . . . . ? C11_2 C12_2 C13_2 C14_2 1.5(5) . . . . ? O12_2 C12_2 C13_2 C21_3 -6.1(5) . . . . ? C11_2 C12_2 C13_2 C21_3 176.7(3) . . . . ? C12_2 C13_2 C14_2 C15_2 -3.1(5) . . . . ? C21_3 C13_2 C14_2 C15_2 -178.2(3) . . . . ? C13_2 C14_2 C15_2 C16_2 1.3(5) . . . . ? C13_2 C14_2 C15_2 C21_2 177.3(3) . . . . ? C14_2 C15_2 C16_2 C11_2 2.2(5) . . . . ? C21_2 C15_2 C16_2 C11_2 -173.9(3) . . . . ? C14_2 C15_2 C16_2 O16_2 -176.7(3) . . . . ? C21_2 C15_2 C16_2 O16_2 7.2(5) . . . . ? C12_2 C11_2 C16_2 C15_2 -3.6(5) . . . . ? C17_2 C11_2 C16_2 C15_2 170.8(3) . . . . ? C12_2 C11_2 C16_2 O16_2 175.3(3) . . . . ? C17_2 C11_2 C16_2 O16_2 -10.2(5) . . . . ? C13_2 C12_2 O12_2 C27_3 81.9(4) . . . . ? C11_2 C12_2 O12_2 C27_3 -100.8(4) . . . . ? C15_2 C16_2 O16_2 C27_2 -83.6(4) . . . . ? C11_2 C16_2 O16_2 C27_2 97.4(4) . . . . ? C16_2 C11_2 C17_2 C37_2 -36(2) . . . . ? C12_2 C11_2 C17_2 C37_2 139(2) . . . . ? C12_1 C13_1 C21_2 C15_2 -81.9(4) . . . . ? C14_1 C13_1 C21_2 C15_2 94.9(4) . . . . ? C12_1 C13_1 C21_2 C22_2 149.8(3) . . . . ? C14_1 C13_1 C21_2 C22_2 -33.4(5) . . . . ? C16_2 C15_2 C21_2 C13_1 82.3(4) . . . . ? C14_2 C15_2 C21_2 C13_1 -93.6(4) . . . . ? C16_2 C15_2 C21_2 C22_2 -149.6(3) . . . . ? C14_2 C15_2 C21_2 C22_2 34.5(4) . . . . ? C13_1 C21_2 C22_2 C23_2 -172.0(3) . . . . ? C15_2 C21_2 C22_2 C23_2 62.7(4) . . . . ? C21_2 C22_2 C23_2 C24_2 164.5(3) . . . . ? C22_2 C23_2 C24_2 C25_2 -179.8(3) . . . . ? C23_2 C24_2 C25_2 C26_2 169.5(4) . . . . ? C16_2 O16_2 C27_2 O12_1 92.2(3) . . . . ? C12_1 O12_1 C27_2 O16_2 -92.9(3) . . . . ? C36_2 N31_2 C32_2 C33_2 0.9(6) . . . . ? N31_2 C32_2 C33_2 C34_2 -2.4(6) . . . . ? N31_2 C32_2 C33_2 C37_2 179.3(4) . . . . ? C32_2 C33_2 C34_2 C35_2 2.1(6) . . . . ? C37_2 C33_2 C34_2 C35_2 -179.6(4) . . . . ? C33_2 C34_2 C35_2 C36_2 -0.4(6) . . . . ? C32_2 N31_2 C36_2 C35_2 1.0(6) . . . . ? C32_2 N31_2 C36_2 N36_2 179.6(3) . . . . ? C34_2 C35_2 C36_2 N31_2 -1.2(6) . . . . ? C34_2 C35_2 C36_2 N36_2 -179.6(4) . . . . ? N31_2 C36_2 N36_2 C38_2 173.6(4) . . . . ? C35_2 C36_2 N36_2 C38_2 -7.9(6) . . . . ? C36_2 N36_2 C38_2 O38_2 2.1(7) . . . . ? C36_2 N36_2 C38_2 C39_2 -178.0(4) . . . . ? C16_3 C11_3 C12_3 O12_3 -173.4(3) . . . . ? C17_3 C11_3 C12_3 O12_3 9.4(5) . . . . ? C16_3 C11_3 C12_3 C13_3 2.4(5) . . . . ? C17_3 C11_3 C12_3 C13_3 -174.7(3) . . . . ? O12_3 C12_3 C13_3 C14_3 174.7(3) . . . . ? C11_3 C12_3 C13_3 C14_3 -0.9(5) . . . . ? O12_3 C12_3 C13_3 C21_4 -8.2(5) . . . . ? C11_3 C12_3 C13_3 C21_4 176.2(3) . . . . ? C12_3 C13_3 C14_3 C15_3 -1.3(5) . . . . ? C21_4 C13_3 C14_3 C15_3 -178.3(3) . . . . ? C13_3 C14_3 C15_3 C16_3 1.9(5) . . . . ? C13_3 C14_3 C15_3 C21_3 177.4(3) . . . . ? C14_3 C15_3 C16_3 O16_3 -177.7(3) . . . . ? C21_3 C15_3 C16_3 O16_3 6.6(5) . . . . ? C14_3 C15_3 C16_3 C11_3 -0.3(5) . . . . ? C21_3 C15_3 C16_3 C11_3 -176.0(3) . . . . ? C12_3 C11_3 C16_3 O16_3 175.7(3) . . . . ? C17_3 C11_3 C16_3 O16_3 -7.1(5) . . . . ? C12_3 C11_3 C16_3 C15_3 -1.8(5) . . . . ? C17_3 C11_3 C16_3 C15_3 175.4(3) . . . . ? C13_3 C12_3 O12_3 C27_4 83.8(4) . . . . ? C11_3 C12_3 O12_3 C27_4 -100.4(4) . . . . ? C15_3 C16_3 O16_3 C27_3 -83.6(4) . . . . ? C11_3 C16_3 O16_3 C27_3 98.9(4) . . . . ? C12_2 C13_2 C21_3 C15_3 -84.3(4) . . . . ? C14_2 C13_2 C21_3 C15_3 90.7(4) . . . . ? C12_2 C13_2 C21_3 C22_3 147.8(3) . . . . ? C14_2 C13_2 C21_3 C22_3 -37.3(4) . . . . ? C14_3 C15_3 C21_3 C13_2 -91.5(4) . . . . ? C16_3 C15_3 C21_3 C13_2 83.9(4) . . . . ? C14_3 C15_3 C21_3 C22_3 36.7(4) . . . . ? C16_3 C15_3 C21_3 C22_3 -147.9(3) . . . . ? C13_2 C21_3 C22_3 C23_3 -64.4(4) . . . . ? C15_3 C21_3 C22_3 C23_3 171.0(3) . . . . ? C21_3 C22_3 C23_3 C24_3 173.2(3) . . . . ? C22_3 C23_3 C24_3 C25_3 55.3(6) . . . . ? C23_3 C24_3 C25_3 C26_3 57.7(6) . . . . ? C12_2 O12_2 C27_3 O16_3 -90.2(4) . . . . ? C16_3 O16_3 C27_3 O12_2 91.8(4) . . . . ? C36_3 N31_3 C32_3 C33_3 0.2(7) . . . . ? N31_3 C32_3 C33_3 C34_3 0.9(7) . . . . ? N31_3 C32_3 C33_3 C37_3 -178.0(4) . . . . ? C32_3 C33_3 C34_3 C35_3 -1.3(7) . . . . ? C37_3 C33_3 C34_3 C35_3 177.6(4) . . . . ? C33_3 C34_3 C35_3 C36_3 0.7(7) . . . . ? C32_3 N31_3 C36_3 C35_3 -0.9(6) . . . . ? C32_3 N31_3 C36_3 N36_3 178.4(4) . . . . ? C34_3 C35_3 C36_3 N31_3 0.5(7) . . . . ? C34_3 C35_3 C36_3 N36_3 -178.8(4) . . . . ? N31_3 C36_3 N36_3 C38_3 170.8(4) . . . . ? C35_3 C36_3 N36_3 C38_3 -9.9(7) . . . . ? C36_3 N36_3 C38_3 O38_3 0.8(8) . . . . ? C36_3 N36_3 C38_3 C39_3 -179.9(4) . . . . ? C16_4 C11_4 C12_4 C13_4 -0.3(6) . . . . ? C17_4 C11_4 C12_4 C13_4 -176.3(4) . . . . ? C16_4 C11_4 C12_4 O12_4 -177.4(3) . . . . ? C17_4 C11_4 C12_4 O12_4 6.7(5) . . . . ? O12_4 C12_4 C13_4 C14_4 178.8(3) . . . . ? C11_4 C12_4 C13_4 C14_4 1.8(6) . . . . ? O12_4 C12_4 C13_4 C21_1 -5.0(5) . . . . ? C11_4 C12_4 C13_4 C21_1 178.1(3) . . . . ? C15_1 C21_1 C13_4 C12_4 -85.4(4) . . . . ? C22A_1 C21_1 C13_4 C12_4 146.1(4) . . . . ? C15_1 C21_1 C13_4 C14_4 90.7(4) . . . . ? C22A_1 C21_1 C13_4 C14_4 -37.8(5) . . . . ? C12_4 C13_4 C14_4 C15_4 -1.7(6) . . . . ? C21_1 C13_4 C14_4 C15_4 -177.8(3) . . . . ? C13_4 C14_4 C15_4 C16_4 -0.1(5) . . . . ? C13_4 C14_4 C15_4 C21_4 176.4(3) . . . . ? C12_4 C11_4 C16_4 O16_4 175.1(3) . . . . ? C17_4 C11_4 C16_4 O16_4 -8.9(5) . . . . ? C12_4 C11_4 C16_4 C15_4 -1.5(6) . . . . ? C17_4 C11_4 C16_4 C15_4 174.5(4) . . . . ? C14_4 C15_4 C16_4 O16_4 -174.8(3) . . . . ? C21_4 C15_4 C16_4 O16_4 8.6(5) . . . . ? C14_4 C15_4 C16_4 C11_4 1.7(6) . . . . ? C21_4 C15_4 C16_4 C11_4 -174.8(3) . . . . ? C13_4 C12_4 O12_4 C27_1 82.3(4) . . . . ? C11_4 C12_4 O12_4 C27_1 -100.6(4) . . . . ? O16_1 C27_1 O12_4 C12_4 -92.3(4) . . . . ? C11_4 C16_4 O16_4 C27_4 97.7(4) . . . . ? C15_4 C16_4 O16_4 C27_4 -85.6(4) . . . . ? C14_3 C13_3 C21_4 C22_4 -34.0(5) . . . . ? C12_3 C13_3 C21_4 C22_4 149.1(3) . . . . ? C14_3 C13_3 C21_4 C15_4 94.3(4) . . . . ? C12_3 C13_3 C21_4 C15_4 -82.6(4) . . . . ? C16_4 C15_4 C21_4 C13_3 83.3(4) . . . . ? C14_4 C15_4 C21_4 C13_3 -93.1(4) . . . . ? C16_4 C15_4 C21_4 C22_4 -148.6(3) . . . . ? C14_4 C15_4 C21_4 C22_4 35.0(5) . . . . ? C13_3 C21_4 C22_4 C23_4 -174.2(3) . . . . ? C15_4 C21_4 C22_4 C23_4 61.0(4) . . . . ? C21_4 C22_4 C23_4 C24A_4 175.2(4) . . . . ? C22_4 C23_4 C24A_4 C25A_4 -81.7(7) . . . . ? C23_4 C24A_4 C25A_4 C26A_4 -176.1(10) . . . . ? C16_4 O16_4 C27_4 O12_3 91.8(4) . . . . ? C12_3 O12_3 C27_4 O16_4 -90.4(4) . . . . ? C36_4 N31_4 C32_4 C33_4 -0.7(6) . . . . ? N31_4 C32_4 C33_4 C34_4 0.8(6) . . . . ? N31_4 C32_4 C33_4 C37_4 180.0(4) . . . . ? C32_4 C33_4 C34_4 C35_4 -0.2(6) . . . . ? C37_4 C33_4 C34_4 C35_4 -179.4(4) . . . . ? C33_4 C34_4 C35_4 C36_4 -0.5(6) . . . . ? C32_4 N31_4 C36_4 C35_4 -0.1(6) . . . . ? C32_4 N31_4 C36_4 N36_4 176.6(3) . . . . ? C34_4 C35_4 C36_4 N31_4 0.6(6) . . . . ? C34_4 C35_4 C36_4 N36_4 -175.7(4) . . . . ? N31_4 C36_4 N36_4 C38_4 169.5(4) . . . . ? C35_4 C36_4 N36_4 C38_4 -13.8(6) . . . . ? C36_4 N36_4 C38_4 O38_4 -1.3(6) . . . . ? C36_4 N36_4 C38_4 C39_4 178.6(4) . . . . ? C46_5 C41_5 C42_5 C43_5 0.0 . . . . ? C47_5 C41_5 C42_5 C43_5 -176.3(6) . . . . ? C41_5 C42_5 C43_5 C44_5 0.0 . . . . ? C42_5 C43_5 C44_5 C45_5 0.0 . . . . ? C43_5 C44_5 C45_5 C46_5 0.0 . . . . ? C44_5 C45_5 C46_5 C41_5 0.0 . . . . ? C42_5 C41_5 C46_5 C45_5 0.0 . . . . ? C47_5 C41_5 C46_5 C45_5 176.4(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 N36_2 H36_2 O38_4 0.88 2.05 2.920(4) 170.6 2_665 N36_3 H36_3 O38_2 0.88 1.98 2.852(4) 173.1 2_665 N36_4 H36_4 O16_1 0.88 2.23 3.070(4) 159.2 2_655 _diffrn_measured_fraction_theta_max 0.984 _diffrn_reflns_theta_full 28.40 _diffrn_measured_fraction_theta_full 0.984 _refine_diff_density_max 1.223 _refine_diff_density_min -0.708 _refine_diff_density_rms 0.120 #END