Electronic Supplementary Material for CrystEngComm This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'C. Aakeroy' _publ_contact_author_address ; Department of Chemistry Kansas State University Manhattan Manhattan Kansas 66506-3701 UNITED STATES OF AMERICA ; _publ_contact_author_email AAKEROY@KSU.EDU _publ_section_title ; Synthesis and hydrogen-bond capabilities of an amino-pyridine functionalized cavitand ; loop_ _publ_author_name 'C. Aakeroy' 'John Desper' 'Nate Schultheiss' # Attachment 'all.cif' data_6 _database_code_depnum_ccdc_archive 'CCDC 629287' _audit_creation_method SHELXL-97 _chemical_name_systematic ; 3S (aminopyridyl)ethynylcavitand, NO22PhCOOH ; _chemical_name_common '3S (aminopyridyl)ethynylcavitand, NO22PhCOOH' _chemical_melting_point ? _chemical_formula_moiety ; (C80 H80 N8 O8) (C7 H4 N2 O6)4 (C2 H3 N)2.45 (C2 H5 O)0.55 ; _chemical_formula_sum 'C114 H106.10 N18.45 O32.55' _chemical_formula_weight 2255.37 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 14.636(3) _cell_length_b 17.062(3) _cell_length_c 25.079(4) _cell_angle_alpha 76.787(10) _cell_angle_beta 85.972(12) _cell_angle_gamma 64.566(9) _cell_volume 5503.3(16) _cell_formula_units_Z 2 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 1975 _cell_measurement_theta_min 2.25 _cell_measurement_theta_max 26.65 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.361 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2359 _exptl_absorpt_coefficient_mu 0.102 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 143(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 41304 _diffrn_reflns_av_R_equivalents 0.1944 _diffrn_reflns_av_sigmaI/netI 0.6566 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 1.35 _diffrn_reflns_theta_max 27.65 _reflns_number_total 24410 _reflns_number_gt 4410 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1300P)^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 24410 _refine_ls_number_parameters 1471 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.3967 _refine_ls_R_factor_gt 0.1084 _refine_ls_wR_factor_ref 0.3484 _refine_ls_wR_factor_gt 0.2468 _refine_ls_goodness_of_fit_ref 0.762 _refine_ls_restrained_S_all 0.766 _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 N1S N 0.8463(8) 0.8382(7) 0.1293(5) 0.106(4) Uiso 1 1 d D . . C1S C 0.8426(10) 0.9119(8) 0.1129(5) 0.089(4) Uiso 1 1 d D . . C2S C 0.8424(9) 1.0021(7) 0.0973(5) 0.091(4) Uiso 1 1 d D . . H2A H 0.8203 1.0314 0.1283 0.137 Uiso 1 1 calc R . . H2B H 0.7958 1.0380 0.0658 0.137 Uiso 1 1 calc R . . H2C H 0.9108 0.9960 0.0877 0.137 Uiso 1 1 calc R . . N2S N 1.5849(11) 0.1080(9) 0.0344(6) 0.112(4) Uiso 0.804(9) 1 d PD A 1 C3S C 1.5660(15) 0.0514(13) 0.0699(7) 0.112(4) Uiso 0.804(9) 1 d PD A 1 C4S C 1.5571(14) -0.0114(11) 0.1188(7) 0.112(4) Uiso 0.804(9) 1 d PD A 1 H4A H 1.5731 -0.0686 0.1094 0.168 Uiso 0.804(9) 1 calc PR A 1 H4B H 1.4878 0.0126 0.1318 0.168 Uiso 0.804(9) 1 calc PR A 1 H4C H 1.6045 -0.0201 0.1477 0.168 Uiso 0.804(9) 1 calc PR A 1 N3S N 1.412(4) 0.059(4) 0.027(2) 0.112(4) Uiso 0.196(9) 1 d PD A 2 C5S C 1.493(4) 0.019(5) 0.063(2) 0.112(4) Uiso 0.196(9) 1 d PD A 2 C6S C 1.600(4) -0.024(5) 0.086(3) 0.112(4) Uiso 0.196(9) 1 d PD A 2 H6A H 1.6002 -0.0234 0.1246 0.168 Uiso 0.196(9) 1 calc PR A 2 H6B H 1.6374 0.0095 0.0658 0.168 Uiso 0.196(9) 1 calc PR A 2 H6C H 1.6330 -0.0851 0.0809 0.168 Uiso 0.196(9) 1 calc PR A 2 N4S N 0.656(2) -0.0714(17) 0.2957(15) 0.157(12) Uiso 0.45 1 d PD B 1 C7S C 0.717(3) -0.1501(19) 0.2844(18) 0.113(16) Uiso 0.45 1 d PD B 1 C8S C 0.7812(18) -0.2503(15) 0.2944(10) 0.079(8) Uiso 0.45 1 d PD B 1 H8A H 0.7768 -0.2777 0.3328 0.119 Uiso 0.45 1 calc PR B 1 H8B H 0.8519 -0.2623 0.2864 0.119 Uiso 0.45 1 calc PR B 1 H8C H 0.7562 -0.2754 0.2705 0.119 Uiso 0.45 1 calc PR B 1 O1S O 0.7291(12) -0.1038(11) 0.3359(7) 0.101(5) Uiso 0.55 1 d P C 2 C9S C 0.7098(17) -0.1546(14) 0.3081(10) 0.059(7) Uiso 0.55 1 d P C 2 H9A H 0.6459 -0.1589 0.3203 0.070 Uiso 0.55 1 calc PR C 2 H9B H 0.7653 -0.2154 0.3149 0.070 Uiso 0.55 1 calc PR C 2 C10S C 0.700(2) -0.106(2) 0.2402(12) 0.146(12) Uiso 0.55 1 d P C 2 H10A H 0.6324 -0.0569 0.2315 0.219 Uiso 0.55 1 calc PR C 2 H10B H 0.7102 -0.1501 0.2185 0.219 Uiso 0.55 1 calc PR C 2 H10C H 0.7513 -0.0830 0.2313 0.219 Uiso 0.55 1 calc PR C 2 C31_1 C 0.5409(6) 0.6783(6) 0.4209(4) 0.038(2) Uani 1 1 d . D . H31_1 H 0.6150 0.6384 0.4252 0.046 Uiso 1 1 calc R . . C32_1 C 0.5171(6) 0.7367(6) 0.4631(4) 0.041(2) Uani 1 1 d . . . H32A_1 H 0.5283 0.6987 0.5005 0.049 Uiso 1 1 calc R D . H32B_1 H 0.4449 0.7797 0.4588 0.049 Uiso 1 1 calc R . . C33A_1 C 0.5834(6) 0.7881(6) 0.4564(4) 0.048(3) Uani 0.598(6) 1 d PD D -1 H33A_1 H 0.5685 0.8215 0.4858 0.058 Uiso 0.598(6) 1 calc PR D -1 H33B_1 H 0.5658 0.8317 0.4208 0.058 Uiso 0.598(6) 1 calc PR D -1 C34A_1 C 0.6988(9) 0.7256(10) 0.4588(7) 0.062(4) Uani 0.598(6) 1 d PD D -1 H34A_1 H 0.7129 0.6916 0.4297 0.075 Uiso 0.598(6) 1 calc PR D -1 H34B_1 H 0.7158 0.6822 0.4945 0.075 Uiso 0.598(6) 1 calc PR D -1 C35A_1 C 0.7708(12) 0.7743(11) 0.4517(8) 0.099(7) Uani 0.598(6) 1 d PD D -1 H35A_1 H 0.7548 0.8185 0.4164 0.118 Uiso 0.598(6) 1 calc PR D -1 H35B_1 H 0.7611 0.8059 0.4817 0.118 Uiso 0.598(6) 1 calc PR D -1 C36A_1 C 0.8746(10) 0.7079(13) 0.4530(8) 0.081(6) Uani 0.598(6) 1 d PD D -1 H36A_1 H 0.8773 0.6604 0.4362 0.121 Uiso 0.598(6) 1 calc PR D -1 H36B_1 H 0.9001 0.6827 0.4911 0.121 Uiso 0.598(6) 1 calc PR D -1 H36B_1' H 0.9167 0.7356 0.4325 0.121 Uiso 0.598(6) 1 calc PR D -1 C33B_1 C 0.5834(6) 0.7881(6) 0.4564(4) 0.048(3) Uani 0.402(6) 1 d PD D -2 H33C_1 H 0.5923 0.8091 0.4170 0.058 Uiso 0.402(6) 1 calc PR D -2 H33D_1 H 0.6511 0.7488 0.4740 0.058 Uiso 0.402(6) 1 calc PR D -2 C34B_1 C 0.5292(17) 0.8691(13) 0.4842(10) 0.062(4) Uani 0.402(6) 1 d PD D -2 H34C_1 H 0.4599 0.9059 0.4681 0.075 Uiso 0.402(6) 1 calc PR D -2 H34D_1 H 0.5236 0.8474 0.5239 0.075 Uiso 0.402(6) 1 calc PR D -2 C35B_1 C 0.589(2) 0.9263(15) 0.4759(11) 0.099(7) Uani 0.402(6) 1 d PD D -2 H35C_1 H 0.6559 0.8910 0.4955 0.118 Uiso 0.402(6) 1 calc PR D -2 H35D_1 H 0.6019 0.9417 0.4364 0.118 Uiso 0.402(6) 1 calc PR D -2 C36B_1 C 0.5343(16) 1.0113(15) 0.4965(12) 0.081(6) Uani 0.402(6) 1 d PD D -2 H36D_1 H 0.4615 1.0350 0.4888 0.121 Uiso 0.402(6) 1 calc PR D -2 H36E_1 H 0.5590 1.0553 0.4780 0.121 Uiso 0.402(6) 1 calc PR D -2 H36F_1 H 0.5469 0.9986 0.5362 0.121 Uiso 0.402(6) 1 calc PR D -2 C37_1 C 0.6442(7) 0.5350(6) 0.3426(4) 0.042(3) Uani 1 1 d . D . H37A_1 H 0.5824 0.5498 0.3211 0.050 Uiso 1 1 calc R . . H37B_1 H 0.7010 0.4865 0.3295 0.050 Uiso 1 1 calc R . . C31_2 C 0.2299(6) 0.6228(6) 0.4765(4) 0.038(2) Uani 1 1 d . . . H31_2 H 0.2212 0.5681 0.4952 0.045 Uiso 1 1 calc R . . C32_2 C 0.2075(6) 0.6802(7) 0.5180(4) 0.042(3) Uani 1 1 d . . . H32A_2 H 0.2031 0.7395 0.4992 0.051 Uiso 1 1 calc R . . H32B_2 H 0.2636 0.6527 0.5457 0.051 Uiso 1 1 calc R . . C33_2 C 0.1087(7) 0.6911(7) 0.5465(4) 0.052(3) Uani 1 1 d . . . H33A_2 H 0.0530 0.7187 0.5184 0.063 Uiso 1 1 calc R . . H33B_2 H 0.1132 0.6314 0.5643 0.063 Uiso 1 1 calc R . . C34_2 C 0.0826(9) 0.7461(11) 0.5884(5) 0.128(7) Uani 1 1 d . . . H34A_2 H 0.0726 0.8072 0.5697 0.154 Uiso 1 1 calc R . . H34B_2 H 0.1412 0.7215 0.6144 0.154 Uiso 1 1 calc R . . C35_2 C -0.0105(10) 0.7521(14) 0.6210(6) 0.153(8) Uani 1 1 d . . . H35A_2 H -0.0705 0.7979 0.5984 0.184 Uiso 1 1 calc R . . H35B_2 H -0.0146 0.6945 0.6257 0.184 Uiso 1 1 calc R . . C36_2 C -0.0179(12) 0.7705(13) 0.6685(6) 0.155(8) Uani 1 1 d . . . H36A_2 H 0.0406 0.7261 0.6918 0.233 Uiso 1 1 calc R . . H36B_2 H -0.0801 0.7698 0.6852 0.233 Uiso 1 1 calc R . . H36C_2 H -0.0198 0.8297 0.6646 0.233 Uiso 1 1 calc R . . C37_2 C 0.2649(6) 0.4710(6) 0.4071(4) 0.041(2) Uani 1 1 d . . . H37A_2 H 0.2676 0.4144 0.4018 0.049 Uiso 1 1 calc R . . H37B_2 H 0.2806 0.5024 0.3719 0.049 Uiso 1 1 calc R . . C31_3 C 0.0209(6) 0.8942(6) 0.3306(4) 0.036(2) Uani 1 1 d . D . H31_3 H -0.0437 0.9114 0.3103 0.044 Uiso 1 1 calc R . . C32_3 C -0.0048(6) 0.9552(6) 0.3710(4) 0.039(2) Uani 1 1 d . . . H32A_3 H 0.0574 0.9413 0.3916 0.047 Uiso 1 1 calc R . . H32B_3 H -0.0308 1.0178 0.3503 0.047 Uiso 1 1 calc R . . C33_3 C -0.0838(6) 0.9443(6) 0.4110(4) 0.040(2) Uani 1 1 d . . . H33A_3 H -0.0542 0.8843 0.4355 0.048 Uiso 1 1 calc R . . H33B_3 H -0.1420 0.9492 0.3904 0.048 Uiso 1 1 calc R . . C34_3 C -0.1211(7) 1.0149(6) 0.4459(4) 0.045(3) Uani 1 1 d . . . H34A_3 H -0.0617 1.0128 0.4639 0.054 Uiso 1 1 calc R . . H34B_3 H -0.1544 1.0744 0.4213 0.054 Uiso 1 1 calc R . . C35_3 C -0.1931(7) 1.0043(7) 0.4887(4) 0.054(3) Uani 1 1 d . . . H35A_3 H -0.1580 0.9468 0.5150 0.065 Uiso 1 1 calc R . . H35B_3 H -0.2498 1.0016 0.4711 0.065 Uiso 1 1 calc R . . C36_3 C -0.2358(8) 1.0776(7) 0.5198(4) 0.066(3) Uani 1 1 d . . . H36A_3 H -0.2823 1.0660 0.5472 0.099 Uiso 1 1 calc R . . H36B_3 H -0.2724 1.1347 0.4943 0.099 Uiso 1 1 calc R . . H36C_3 H -0.1804 1.0799 0.5383 0.099 Uiso 1 1 calc R . . C37_3 C 0.0189(7) 0.7904(6) 0.2358(4) 0.044(3) Uani 1 1 d . D . H37A_3 H 0.0907 0.7465 0.2397 0.053 Uiso 1 1 calc R . . H37B_3 H -0.0139 0.7792 0.2070 0.053 Uiso 1 1 calc R . . C31_4 C 0.3345(6) 0.9494(6) 0.2758(4) 0.037(2) Uani 1 1 d . D . H31_4 H 0.3528 0.9805 0.2408 0.044 Uiso 1 1 calc R . . C32_4 C 0.3069(6) 1.0131(6) 0.3157(4) 0.041(3) Uani 1 1 d . . . H32A_4 H 0.2442 1.0669 0.3020 0.050 Uiso 1 1 calc R . . H32B_4 H 0.2936 0.9832 0.3521 0.050 Uiso 1 1 calc R . . C33_4 C 0.3916(7) 1.0405(7) 0.3214(5) 0.064(3) Uani 1 1 d . . . H33A_4 H 0.4537 0.9866 0.3360 0.077 Uiso 1 1 calc R . . H33B_4 H 0.4062 1.0685 0.2847 0.077 Uiso 1 1 calc R . . C34_4 C 0.3658(10) 1.1045(10) 0.3587(8) 0.125(7) Uani 1 1 d . . . H34A_4 H 0.3563 1.0727 0.3955 0.151 Uiso 1 1 calc R . . H34B_4 H 0.4268 1.1145 0.3618 0.151 Uiso 1 1 calc R . . C35_4 C 0.2944(13) 1.1773(14) 0.3496(11) 0.220(13) Uani 1 1 d . . . H35A_4 H 0.2323 1.1678 0.3497 0.264 Uiso 1 1 calc R . . H35B_4 H 0.3006 1.2082 0.3119 0.264 Uiso 1 1 calc R . . C36_4 C 0.2771(12) 1.2431(9) 0.3884(6) 0.127(6) Uani 1 1 d . . . H36A_4 H 0.2189 1.2996 0.3745 0.190 Uiso 1 1 calc R . . H36B_4 H 0.3376 1.2538 0.3893 0.190 Uiso 1 1 calc R . . H36C_4 H 0.2642 1.2168 0.4255 0.190 Uiso 1 1 calc R . . C37_4 C 0.4023(7) 0.8589(6) 0.1671(4) 0.042(3) Uani 1 1 d . D . H37A_4 H 0.4238 0.8621 0.1287 0.051 Uiso 1 1 calc R . . H37B_4 H 0.4008 0.8003 0.1813 0.051 Uiso 1 1 calc R . . C41_1 C 1.2563(7) 0.5898(6) 0.1176(5) 0.048(3) Uani 1 1 d . . . C47_1 C 1.1630(7) 0.5832(7) 0.1010(4) 0.046(3) Uani 1 1 d . . . O41_1 O 1.0880(4) 0.6168(4) 0.1304(3) 0.0535(19) Uani 1 1 d . . . H41_1 H 1.0393 0.6081 0.1217 0.064 Uiso 1 1 calc R . . O42_1 O 1.1636(4) 0.5464(4) 0.0633(3) 0.0496(18) Uani 1 1 d . . . C42_1 C 1.3348(7) 0.5725(6) 0.0805(5) 0.058(3) Uani 1 1 d . . . H42_1 H 1.3290 0.5572 0.0471 0.069 Uiso 1 1 calc R . . C43_1 C 1.4209(7) 0.5785(7) 0.0940(5) 0.055(3) Uani 1 1 d . . . N43_1 N 1.5016(7) 0.5615(7) 0.0560(5) 0.070(3) Uani 1 1 d . . . O43_1 O 1.4796(6) 0.5834(6) 0.0065(4) 0.077(3) Uani 1 1 d . . . O44_1 O 1.5893(6) 0.5284(6) 0.0751(4) 0.093(3) Uani 1 1 d . . . C44_1 C 1.4307(7) 0.6017(7) 0.1416(5) 0.053(3) Uani 1 1 d . . . H44_1 H 1.4905 0.6054 0.1506 0.064 Uiso 1 1 calc R . . C45_1 C 1.3506(7) 0.6189(7) 0.1750(4) 0.051(3) Uani 1 1 d . . . N45_1 N 1.3547(8) 0.6483(6) 0.2251(4) 0.064(3) Uani 1 1 d . . . O45_1 O 1.4386(6) 0.6400(5) 0.2393(3) 0.081(3) Uani 1 1 d . . . O46_1 O 1.2792(5) 0.6772(5) 0.2522(3) 0.072(2) Uani 1 1 d . . . C46_1 C 1.2618(7) 0.6147(6) 0.1643(4) 0.047(3) Uani 1 1 d . . . H46_1 H 1.2071 0.6287 0.1885 0.056 Uiso 1 1 calc R . . C41_2 C 1.0165(8) 0.1243(7) 0.1739(5) 0.055(3) Uani 1 1 d . . . C47_2 C 0.9229(10) 0.1314(9) 0.2063(6) 0.077(4) Uani 1 1 d . . . O41_2 O 0.9144(5) 0.1627(5) 0.2501(3) 0.076(2) Uani 1 1 d . . . H41_2 H 0.8611 0.1649 0.2659 0.091 Uiso 1 1 calc R . . O42_2 O 0.8619(6) 0.1092(5) 0.1919(3) 0.080(3) Uani 1 1 d . . . C42_2 C 1.0256(8) 0.0946(7) 0.1249(5) 0.071(4) Uani 1 1 d . . . H42_2 H 0.9748 0.0816 0.1124 0.085 Uiso 1 1 calc R . . C43_2 C 1.1107(9) 0.0855(8) 0.0963(5) 0.066(3) Uani 1 1 d . . . N43_2 N 1.1254(9) 0.0522(7) 0.0466(5) 0.082(3) Uani 1 1 d . . . O43_2 O 1.0557(7) 0.0427(6) 0.0283(3) 0.089(3) Uani 1 1 d . . . O44_2 O 1.2111(7) 0.0321(6) 0.0246(4) 0.108(3) Uani 1 1 d . . . C44_2 C 1.1895(10) 0.1044(7) 0.1133(5) 0.077(4) Uani 1 1 d . . . H44_2 H 1.2500 0.0943 0.0937 0.093 Uiso 1 1 calc R . . C45_2 C 1.1722(8) 0.1374(8) 0.1589(5) 0.062(3) Uani 1 1 d . . . N45_2 N 1.2452(8) 0.1600(7) 0.1769(5) 0.082(4) Uani 1 1 d . . . O45_2 O 1.3289(6) 0.1386(6) 0.1533(4) 0.097(3) Uani 1 1 d . . . O46_2 O 1.2264(7) 0.2009(6) 0.2129(4) 0.098(3) Uani 1 1 d . . . C46_2 C 1.0875(8) 0.1434(7) 0.1914(5) 0.065(3) Uani 1 1 d . . . H46_2 H 1.0809 0.1609 0.2253 0.078 Uiso 1 1 calc R . . C41_3 C -0.3617(7) 0.3573(6) 0.2081(4) 0.044(3) Uani 1 1 d . . . C47_3 C -0.2735(7) 0.3800(7) 0.2000(4) 0.046(3) Uani 1 1 d . . . O41_3 O -0.2675(4) 0.4243(4) 0.2333(3) 0.0489(18) Uani 1 1 d . . . H41_3 H -0.2108 0.4260 0.2309 0.059 Uiso 1 1 calc R . . O42_3 O -0.2177(5) 0.3576(5) 0.1619(3) 0.0510(19) Uani 1 1 d . . . C42_3 C -0.3557(7) 0.2854(6) 0.1865(4) 0.046(3) Uani 1 1 d . . . H42_3 H -0.3013 0.2579 0.1642 0.055 Uiso 1 1 calc R . . C43_3 C -0.4321(7) 0.2558(7) 0.1990(4) 0.052(3) Uani 1 1 d . . . N43_3 N -0.4240(8) 0.1810(7) 0.1778(5) 0.081(3) Uani 1 1 d . . . O43_3 O -0.3616(6) 0.1551(6) 0.1446(4) 0.102(3) Uani 1 1 d . . . O44_3 O -0.4797(7) 0.1472(7) 0.1972(5) 0.133(4) Uani 1 1 d . . . C44_3 C -0.5146(7) 0.2973(7) 0.2302(4) 0.047(3) Uani 1 1 d . . . H44_3 H -0.5652 0.2761 0.2393 0.056 Uiso 1 1 calc R . . C45_3 C -0.5191(7) 0.3687(7) 0.2467(4) 0.047(3) Uani 1 1 d . . . N45_3 N -0.6086(7) 0.4133(7) 0.2765(4) 0.064(3) Uani 1 1 d . . . O45_3 O -0.6661(5) 0.3790(6) 0.2921(3) 0.091(3) Uani 1 1 d . . . C46_3 C -0.4464(6) 0.4007(7) 0.2375(4) 0.046(3) Uani 1 1 d . . . H46_3 H -0.4534 0.4509 0.2507 0.055 Uiso 1 1 calc R . . O46_3 O -0.6193(6) 0.4825(6) 0.2875(3) 0.074(2) Uani 1 1 d . . . C41_4 C -0.1991(7) 0.7075(6) -0.0318(4) 0.042(3) Uani 1 1 d . . . C47_4 C -0.0960(7) 0.7063(7) -0.0311(4) 0.041(3) Uani 1 1 d . . . O41_4 O -0.0813(4) 0.7397(4) 0.0045(3) 0.0505(19) Uani 1 1 d . . . H41_4 H -0.0241 0.7403 0.0006 0.061 Uiso 1 1 calc R . . O42_4 O -0.0352(4) 0.6765(4) -0.0669(3) 0.0452(17) Uani 1 1 d . . . C42_4 C -0.2243(6) 0.6725(6) -0.0706(4) 0.043(3) Uani 1 1 d . . . H42_4 H -0.1777 0.6497 -0.0976 0.051 Uiso 1 1 calc R . . C43_4 C -0.3183(7) 0.6716(7) -0.0689(4) 0.046(3) Uani 1 1 d . . . N43_4 N -0.3461(6) 0.6374(6) -0.1109(4) 0.053(2) Uani 1 1 d . . . O43_4 O -0.2905(5) 0.6224(5) -0.1499(3) 0.0549(19) Uani 1 1 d . . . O44_4 O -0.4245(5) 0.6266(5) -0.1054(3) 0.063(2) Uani 1 1 d . . . C44_4 C -0.3877(7) 0.7011(6) -0.0307(4) 0.047(3) Uani 1 1 d . . . H44_4 H -0.4507 0.6973 -0.0297 0.056 Uiso 1 1 calc R . . C45_4 C -0.3618(7) 0.7364(6) 0.0061(4) 0.046(3) Uani 1 1 d . . . N45_4 N -0.4315(6) 0.7695(6) 0.0496(4) 0.062(3) Uani 1 1 d . . . O45_4 O -0.4968(5) 0.7402(5) 0.0596(3) 0.083(3) Uani 1 1 d . . . O46_4 O -0.4202(5) 0.8176(5) 0.0740(3) 0.070(2) Uani 1 1 d . . . C46_4 C -0.2670(7) 0.7398(7) 0.0073(4) 0.050(3) Uani 1 1 d . . . H46_4 H -0.2508 0.7636 0.0342 0.060 Uiso 1 1 calc R . . C11_1 C 0.5658(6) 0.7377(6) 0.2675(4) 0.036(2) Uani 1 1 d . . . C12_1 C 0.5814(6) 0.6943(6) 0.3209(4) 0.031(2) Uani 1 1 d . D . O12_1 O 0.6649(4) 0.6106(4) 0.3332(2) 0.0398(16) Uani 1 1 d . . . C13_1 C 0.5217(7) 0.7309(6) 0.3618(4) 0.034(2) Uani 1 1 d . . . C14_1 C 0.4431(6) 0.8138(6) 0.3465(4) 0.035(2) Uani 1 1 d . D . H14_1 H 0.3995 0.8393 0.3738 0.042 Uiso 1 1 calc R . . C15_1 C 0.4252(6) 0.8609(6) 0.2933(4) 0.030(2) Uani 1 1 d . . . C16_1 C 0.4852(7) 0.8236(7) 0.2530(4) 0.037(2) Uani 1 1 d . D . O16_1 O 0.4729(4) 0.8678(4) 0.1996(3) 0.0378(16) Uani 1 1 d . . . C17_1 C 0.6294(7) 0.6994(6) 0.2243(4) 0.040(2) Uani 1 1 d . . . C11_2 C 0.4820(7) 0.4826(6) 0.4203(4) 0.038(2) Uani 1 1 d . . . C12_2 C 0.3846(6) 0.5103(6) 0.4410(4) 0.032(2) Uani 1 1 d . . . O12_2 O 0.3388(4) 0.4525(4) 0.4478(2) 0.0420(16) Uani 1 1 d . . . C13_2 C 0.3379(6) 0.5920(6) 0.4563(3) 0.033(2) Uani 1 1 d . . . C14_2 C 0.3897(6) 0.6452(6) 0.4499(3) 0.035(2) Uani 1 1 d . D . H14_2 H 0.3574 0.7017 0.4593 0.042 Uiso 1 1 calc R . . C15_2 C 0.4867(6) 0.6188(6) 0.4304(4) 0.034(2) Uani 1 1 d . . . C16_2 C 0.5299(6) 0.5394(6) 0.4153(4) 0.039(2) Uani 1 1 d . D . O16_2 O 0.6302(4) 0.5056(4) 0.3977(2) 0.0384(16) Uani 1 1 d . . . C17_2 C 0.5306(7) 0.3995(7) 0.4036(4) 0.038(2) Uani 1 1 d . . . C11_3 C 0.0676(7) 0.6523(7) 0.3547(4) 0.038(2) Uani 1 1 d . . . C12_3 C 0.0350(6) 0.7393(6) 0.3324(4) 0.033(2) Uani 1 1 d . . . O12_3 O -0.0293(4) 0.7779(4) 0.2863(2) 0.0387(16) Uani 1 1 d . . . C13_3 C 0.0583(6) 0.7970(6) 0.3569(4) 0.037(2) Uani 1 1 d . . . C14_3 C 0.1206(6) 0.7562(6) 0.4033(4) 0.035(2) Uani 1 1 d . . . H14_3 H 0.1397 0.7918 0.4201 0.042 Uiso 1 1 calc R . . C15_3 C 0.1559(6) 0.6677(6) 0.4265(4) 0.033(2) Uani 1 1 d . . . C16_3 C 0.1306(7) 0.6143(7) 0.4001(4) 0.039(2) Uani 1 1 d . . . O16_3 O 0.1640(4) 0.5252(4) 0.4224(2) 0.0415(17) Uani 1 1 d . . . C17_3 C 0.0432(7) 0.5979(6) 0.3279(4) 0.039(2) Uani 1 1 d . . . C11_4 C 0.1660(6) 0.8920(6) 0.1972(4) 0.035(2) Uani 1 1 d . . . C12_4 C 0.2419(6) 0.9165(6) 0.2103(4) 0.032(2) Uani 1 1 d . D . O12_4 O 0.3035(4) 0.9285(4) 0.1693(2) 0.0365(15) Uani 1 1 d . . . C13_4 C 0.2465(6) 0.9327(6) 0.2613(4) 0.032(2) Uani 1 1 d . . . C14_4 C 0.1759(6) 0.9246(6) 0.2996(4) 0.036(2) Uani 1 1 d . D . H14_4 H 0.1816 0.9325 0.3353 0.043 Uiso 1 1 calc R . . C15_4 C 0.0956(6) 0.9049(6) 0.2877(4) 0.036(2) Uani 1 1 d . . . C16_4 C 0.0939(6) 0.8901(6) 0.2363(4) 0.033(2) Uani 1 1 d . D . O16_4 O 0.0143(4) 0.8762(4) 0.2194(2) 0.0394(16) Uani 1 1 d . . . C17_4 C 0.1659(7) 0.8710(6) 0.1465(4) 0.039(2) Uani 1 1 d . . . N21_1 N 0.9224(5) 0.6057(5) 0.1177(3) 0.0368(19) Uani 1 1 d . . . C22_1 C 0.9176(6) 0.5490(6) 0.0887(4) 0.042(3) Uani 1 1 d . . . N22_1 N 0.9968(5) 0.5112(5) 0.0595(3) 0.049(2) Uani 1 1 d . . . H22A_1 H 1.0497 0.5232 0.0594 0.059 Uiso 1 1 calc R . . H22B_1 H 0.9967 0.4742 0.0403 0.059 Uiso 1 1 calc R . . C23_1 C 0.8306(6) 0.5319(6) 0.0927(4) 0.041(2) Uani 1 1 d . . . H23_1 H 0.8255 0.4925 0.0730 0.050 Uiso 1 1 calc R . . C24_1 C 0.7555(6) 0.5720(6) 0.1248(4) 0.040(2) Uani 1 1 d . . . H24_1 H 0.6976 0.5597 0.1279 0.048 Uiso 1 1 calc R . . C25_1 C 0.7602(6) 0.6313(6) 0.1536(4) 0.037(2) Uani 1 1 d . . . C26_1 C 0.8440(6) 0.6475(6) 0.1476(4) 0.042(3) Uani 1 1 d . . . H26_1 H 0.8472 0.6900 0.1653 0.050 Uiso 1 1 calc R . . C27_1 C 0.6864(7) 0.6705(6) 0.1902(4) 0.041(3) Uani 1 1 d . . . N21_2 N 0.7562(6) 0.1760(6) 0.3068(3) 0.053(2) Uani 1 1 d . . . C22_2 C 0.7183(8) 0.1154(8) 0.3147(4) 0.059(3) Uani 1 1 d . . . N22_2 N 0.7618(6) 0.0510(6) 0.2840(4) 0.071(3) Uani 1 1 d . . . H22A_2 H 0.8104 0.0522 0.2615 0.085 Uiso 1 1 calc R . . H22B_2 H 0.7409 0.0090 0.2871 0.085 Uiso 1 1 calc R . . C23_2 C 0.6437(8) 0.1146(7) 0.3504(5) 0.062(3) Uani 1 1 d . . . H23_2 H 0.6237 0.0672 0.3571 0.074 Uiso 1 1 calc R . . C24_2 C 0.5978(8) 0.1849(7) 0.3765(4) 0.060(3) Uani 1 1 d . . . H24_2 H 0.5446 0.1863 0.4008 0.072 Uiso 1 1 calc R . . C25_2 C 0.6285(7) 0.2535(6) 0.3676(4) 0.042(2) Uani 1 1 d . . . C26_2 C 0.7095(7) 0.2440(7) 0.3339(4) 0.048(3) Uani 1 1 d . . . H26_2 H 0.7349 0.2878 0.3290 0.057 Uiso 1 1 calc R . . C27_2 C 0.5770(7) 0.3329(7) 0.3889(4) 0.044(3) Uani 1 1 d . . . N21_3 N -0.0944(5) 0.4437(5) 0.2367(3) 0.0343(19) Uani 1 1 d . . . C22_3 C -0.0181(7) 0.4010(7) 0.2071(4) 0.045(3) Uani 1 1 d . . . N22_3 N -0.0324(5) 0.3531(5) 0.1759(3) 0.048(2) Uani 1 1 d . . . H22A_3 H -0.0911 0.3505 0.1754 0.058 Uiso 1 1 calc R . . H22B_3 H 0.0169 0.3241 0.1558 0.058 Uiso 1 1 calc R . . C23_3 C 0.0749(7) 0.4057(6) 0.2093(4) 0.046(3) Uani 1 1 d . . . H23_3 H 0.1294 0.3754 0.1880 0.056 Uiso 1 1 calc R . . C24_3 C 0.0858(7) 0.4536(7) 0.2421(4) 0.048(3) Uani 1 1 d . . . H24_3 H 0.1496 0.4545 0.2453 0.058 Uiso 1 1 calc R . . C25_3 C 0.0046(7) 0.5021(6) 0.2715(4) 0.042(3) Uani 1 1 d . . . C26_3 C -0.0838(7) 0.4951(6) 0.2679(4) 0.046(3) Uani 1 1 d . . . H26_3 H -0.1399 0.5270 0.2878 0.055 Uiso 1 1 calc R . . C27_3 C 0.0197(7) 0.5551(7) 0.3044(4) 0.047(3) Uani 1 1 d . . . N21_4 N 0.0851(5) 0.7558(5) 0.0090(3) 0.039(2) Uani 1 1 d . . . C22_4 C 0.1595(7) 0.7403(6) -0.0275(4) 0.038(2) Uani 1 1 d . . . N22_4 N 0.1481(5) 0.6997(5) -0.0656(3) 0.047(2) Uani 1 1 d . . . H22A_4 H 0.0960 0.6865 -0.0646 0.056 Uiso 1 1 calc R . . H22B_4 H 0.1927 0.6867 -0.0913 0.056 Uiso 1 1 calc R . . C23_4 C 0.2392(7) 0.7635(6) -0.0247(4) 0.043(3) Uani 1 1 d . . . H23_4 H 0.2896 0.7545 -0.0516 0.052 Uiso 1 1 calc R . . C24_4 C 0.2421(7) 0.7993(6) 0.0178(4) 0.044(3) Uani 1 1 d . . . H24_4 H 0.2968 0.8141 0.0209 0.053 Uiso 1 1 calc R . . C25_4 C 0.1677(6) 0.8153(6) 0.0571(4) 0.037(2) Uani 1 1 d . . . C26_4 C 0.0904(6) 0.7917(6) 0.0507(4) 0.037(2) Uani 1 1 d . . . H26_4 H 0.0388 0.8012 0.0769 0.045 Uiso 1 1 calc R . . C27_4 C 0.1684(7) 0.8481(6) 0.1060(4) 0.038(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C31_1 0.025(5) 0.034(6) 0.058(7) -0.020(5) 0.005(5) -0.010(5) C32_1 0.026(5) 0.047(7) 0.054(6) -0.022(5) -0.003(5) -0.013(5) C33A_1 0.035(6) 0.045(7) 0.071(8) -0.017(6) -0.002(5) -0.021(5) C34A_1 0.063(11) 0.070(12) 0.070(11) -0.017(9) -0.004(9) -0.040(10) C35A_1 0.17(2) 0.114(17) 0.073(13) 0.004(12) -0.035(13) -0.123(17) C36A_1 0.032(9) 0.148(17) 0.097(13) -0.072(13) 0.042(9) -0.054(11) C33B_1 0.035(6) 0.045(7) 0.071(8) -0.017(6) -0.002(5) -0.021(5) C34B_1 0.063(11) 0.070(12) 0.070(11) -0.017(9) -0.004(9) -0.040(10) C35B_1 0.17(2) 0.114(17) 0.073(13) 0.004(12) -0.035(13) -0.123(17) C36B_1 0.032(9) 0.148(17) 0.097(13) -0.072(13) 0.042(9) -0.054(11) C37_1 0.042(6) 0.032(6) 0.065(7) -0.019(5) 0.010(5) -0.025(5) C31_2 0.023(5) 0.046(6) 0.046(6) -0.018(5) 0.003(4) -0.013(5) C32_2 0.027(5) 0.066(7) 0.041(6) -0.027(6) -0.002(4) -0.020(5) C33_2 0.031(6) 0.078(8) 0.047(7) -0.020(6) 0.004(5) -0.019(6) C34_2 0.059(9) 0.27(2) 0.108(11) -0.140(13) 0.044(8) -0.075(12) C35_2 0.065(10) 0.32(3) 0.141(15) -0.164(17) 0.067(10) -0.100(14) C36_2 0.138(15) 0.27(2) 0.088(13) -0.030(15) 0.037(12) -0.124(17) C37_2 0.023(5) 0.036(6) 0.070(7) -0.022(5) 0.000(5) -0.012(5) C31_3 0.031(5) 0.041(6) 0.043(6) -0.012(5) -0.005(4) -0.018(5) C32_3 0.030(5) 0.043(6) 0.046(6) -0.019(5) 0.003(5) -0.012(5) C33_3 0.022(5) 0.042(6) 0.057(7) -0.024(5) 0.008(5) -0.010(5) C34_3 0.034(6) 0.053(7) 0.057(7) -0.029(6) 0.004(5) -0.019(5) C35_3 0.049(7) 0.060(8) 0.048(7) -0.021(6) 0.004(5) -0.012(6) C36_3 0.057(7) 0.080(9) 0.064(8) -0.038(7) -0.004(6) -0.020(7) C37_3 0.039(6) 0.053(7) 0.055(7) -0.021(6) -0.001(5) -0.028(6) C31_4 0.032(5) 0.040(6) 0.047(6) -0.021(5) 0.004(5) -0.019(5) C32_4 0.029(5) 0.045(6) 0.064(7) -0.026(6) -0.001(5) -0.020(5) C33_4 0.044(7) 0.062(8) 0.108(10) -0.042(7) -0.007(6) -0.030(6) C34_4 0.061(10) 0.093(12) 0.25(2) -0.114(14) -0.008(12) -0.017(9) C35_4 0.099(15) 0.23(2) 0.42(4) -0.27(3) 0.034(19) -0.050(16) C36_4 0.197(17) 0.086(11) 0.126(13) -0.075(10) 0.040(12) -0.066(12) C37_4 0.036(6) 0.035(6) 0.055(7) -0.019(5) 0.009(5) -0.011(5) C41_1 0.028(6) 0.043(7) 0.077(8) -0.012(6) -0.001(5) -0.018(5) C47_1 0.025(5) 0.053(7) 0.070(8) -0.019(6) 0.010(5) -0.025(6) O41_1 0.033(4) 0.070(5) 0.079(5) -0.031(4) 0.003(4) -0.035(4) O42_1 0.030(4) 0.058(5) 0.068(5) -0.028(4) 0.004(3) -0.019(4) C42_1 0.042(6) 0.053(7) 0.089(9) -0.023(7) 0.015(6) -0.028(6) C43_1 0.037(6) 0.060(8) 0.081(9) -0.027(7) 0.020(6) -0.032(6) N43_1 0.041(6) 0.076(8) 0.108(9) -0.036(8) 0.014(7) -0.033(6) O43_1 0.052(5) 0.090(7) 0.103(7) -0.038(6) 0.028(5) -0.038(5) O44_1 0.031(5) 0.116(8) 0.148(8) -0.066(6) 0.011(5) -0.031(5) C44_1 0.034(6) 0.059(8) 0.079(8) -0.022(7) 0.000(6) -0.026(6) C45_1 0.041(6) 0.053(7) 0.070(8) -0.017(6) -0.009(6) -0.028(6) N45_1 0.055(7) 0.048(6) 0.091(8) -0.011(6) -0.012(6) -0.024(6) O45_1 0.072(6) 0.092(7) 0.105(7) -0.027(5) -0.014(5) -0.052(6) O46_1 0.035(4) 0.071(6) 0.114(7) -0.047(5) -0.001(5) -0.013(4) C46_1 0.033(6) 0.037(6) 0.068(8) -0.012(6) -0.006(5) -0.011(5) C41_2 0.043(7) 0.053(8) 0.065(8) -0.011(7) 0.007(6) -0.018(6) C47_2 0.061(9) 0.094(11) 0.072(10) -0.029(9) 0.007(8) -0.025(8) O41_2 0.056(5) 0.083(6) 0.080(6) -0.028(5) 0.012(5) -0.017(5) O42_2 0.063(6) 0.075(6) 0.097(7) -0.038(5) 0.014(5) -0.016(5) C42_2 0.045(7) 0.069(9) 0.080(9) -0.012(8) 0.005(7) -0.009(7) C43_2 0.058(8) 0.055(8) 0.064(9) -0.019(7) 0.014(7) -0.002(7) N43_2 0.092(10) 0.054(7) 0.085(9) -0.009(7) 0.011(8) -0.023(7) O43_2 0.090(7) 0.074(7) 0.084(7) -0.025(5) -0.022(5) -0.011(6) O44_2 0.078(7) 0.114(8) 0.123(8) -0.045(7) 0.040(6) -0.027(6) C44_2 0.081(10) 0.039(8) 0.076(10) -0.004(7) 0.027(8) 0.000(7) C45_2 0.037(7) 0.058(8) 0.073(9) 0.001(7) 0.010(6) -0.014(6) N45_2 0.059(8) 0.071(9) 0.097(10) -0.002(7) 0.016(7) -0.020(7) O45_2 0.060(6) 0.110(8) 0.113(7) -0.009(6) 0.005(5) -0.037(6) O46_2 0.068(6) 0.093(8) 0.119(9) -0.027(7) 0.013(6) -0.021(6) C46_2 0.058(8) 0.051(8) 0.070(8) -0.008(7) 0.010(7) -0.011(7) C41_3 0.033(6) 0.052(7) 0.053(7) -0.019(6) 0.008(5) -0.022(6) C47_3 0.035(6) 0.045(7) 0.065(8) -0.020(6) 0.001(6) -0.020(6) O41_3 0.028(4) 0.057(5) 0.074(5) -0.029(4) 0.013(3) -0.024(4) O42_3 0.042(4) 0.082(5) 0.052(4) -0.035(4) 0.024(4) -0.042(4) C42_3 0.031(5) 0.041(7) 0.069(7) -0.023(6) 0.003(5) -0.013(5) C43_3 0.029(6) 0.058(8) 0.089(8) -0.042(7) 0.002(6) -0.023(6) N43_3 0.054(7) 0.081(8) 0.137(10) -0.056(8) 0.013(7) -0.042(7) O43_3 0.066(6) 0.131(8) 0.161(9) -0.106(8) 0.044(6) -0.059(6) O44_3 0.095(7) 0.134(9) 0.235(12) -0.109(9) 0.069(8) -0.084(7) C44_3 0.035(6) 0.059(8) 0.055(7) -0.006(6) -0.005(5) -0.031(6) C45_3 0.027(5) 0.065(8) 0.053(7) -0.021(6) 0.013(5) -0.019(6) N45_3 0.054(6) 0.072(8) 0.072(7) -0.019(6) 0.021(5) -0.034(6) O45_3 0.056(5) 0.134(8) 0.120(7) -0.069(6) 0.049(5) -0.061(6) C46_3 0.034(6) 0.060(7) 0.052(7) -0.017(6) 0.008(5) -0.026(6) O46_3 0.059(5) 0.074(6) 0.086(6) -0.017(5) 0.029(4) -0.029(5) C41_4 0.025(5) 0.050(7) 0.049(6) -0.012(6) 0.005(5) -0.015(5) C47_4 0.030(6) 0.049(7) 0.051(7) -0.014(6) 0.006(5) -0.023(5) O41_4 0.032(4) 0.073(5) 0.061(5) -0.030(4) 0.010(3) -0.029(4) O42_4 0.033(4) 0.058(5) 0.055(4) -0.024(4) 0.009(3) -0.024(4) C42_4 0.028(5) 0.043(6) 0.057(7) -0.013(6) 0.002(5) -0.013(5) C43_4 0.037(6) 0.065(8) 0.052(7) -0.023(6) 0.003(5) -0.031(6) N43_4 0.044(6) 0.057(6) 0.057(6) -0.016(5) 0.007(5) -0.021(5) O43_4 0.045(4) 0.070(5) 0.064(5) -0.025(4) -0.001(4) -0.032(4) O44_4 0.049(5) 0.081(6) 0.078(5) -0.022(5) 0.003(4) -0.042(5) C44_4 0.024(5) 0.047(7) 0.073(8) -0.023(6) 0.002(5) -0.013(5) C45_4 0.032(6) 0.048(7) 0.056(7) -0.022(6) 0.018(5) -0.012(5) N45_4 0.034(5) 0.072(7) 0.080(7) -0.020(6) 0.022(5) -0.024(5) O45_4 0.054(5) 0.096(7) 0.120(7) -0.059(6) 0.044(5) -0.041(5) O46_4 0.044(5) 0.091(7) 0.090(6) -0.060(5) 0.023(4) -0.027(5) C46_4 0.038(6) 0.066(8) 0.059(7) -0.021(6) 0.000(5) -0.029(6) C11_1 0.017(5) 0.042(7) 0.050(7) -0.014(6) 0.007(5) -0.014(5) C12_1 0.013(4) 0.029(6) 0.051(7) -0.008(5) 0.000(4) -0.008(4) O12_1 0.024(3) 0.039(4) 0.058(4) -0.013(3) 0.007(3) -0.014(3) C13_1 0.031(5) 0.045(7) 0.036(6) -0.012(5) 0.001(5) -0.024(5) C14_1 0.025(5) 0.033(6) 0.052(7) -0.015(5) 0.003(5) -0.015(5) C15_1 0.018(5) 0.031(6) 0.045(6) -0.013(5) 0.003(4) -0.011(5) C16_1 0.037(6) 0.047(7) 0.045(7) -0.016(6) 0.003(5) -0.031(6) O16_1 0.029(3) 0.049(4) 0.043(4) -0.017(4) 0.001(3) -0.019(3) C17_1 0.029(5) 0.036(6) 0.057(7) -0.006(5) 0.002(5) -0.018(5) C11_2 0.030(5) 0.035(6) 0.051(6) -0.016(5) 0.004(5) -0.013(5) C12_2 0.023(5) 0.028(6) 0.054(6) -0.015(5) 0.011(4) -0.017(5) O12_2 0.026(3) 0.039(4) 0.060(4) -0.008(4) -0.007(3) -0.013(3) C13_2 0.025(5) 0.035(6) 0.039(6) -0.013(5) -0.001(4) -0.010(5) C14_2 0.025(5) 0.044(6) 0.041(6) -0.016(5) 0.001(4) -0.017(5) C15_2 0.025(5) 0.038(6) 0.043(6) -0.009(5) 0.001(4) -0.017(5) C16_2 0.017(5) 0.041(6) 0.060(7) -0.016(5) 0.006(5) -0.012(5) O16_2 0.020(3) 0.038(4) 0.054(4) -0.014(3) 0.006(3) -0.008(3) C17_2 0.019(5) 0.049(7) 0.047(7) -0.003(6) -0.003(5) -0.018(5) C11_3 0.033(6) 0.045(7) 0.046(7) -0.020(6) 0.003(5) -0.021(5) C12_3 0.028(5) 0.037(6) 0.038(6) -0.018(5) 0.003(5) -0.013(5) O12_3 0.031(4) 0.048(4) 0.040(4) -0.013(3) -0.006(3) -0.017(3) C13_3 0.024(5) 0.035(6) 0.049(7) -0.019(5) 0.008(5) -0.006(5) C14_3 0.028(5) 0.043(7) 0.034(6) -0.015(5) 0.009(5) -0.014(5) C15_3 0.020(5) 0.036(6) 0.046(6) -0.015(5) 0.000(4) -0.012(5) C16_3 0.040(6) 0.032(6) 0.046(7) -0.010(5) 0.004(5) -0.017(5) O16_3 0.022(3) 0.049(5) 0.053(4) -0.019(4) 0.008(3) -0.012(3) C17_3 0.032(5) 0.039(6) 0.053(7) -0.021(5) 0.007(5) -0.018(5) C11_4 0.033(5) 0.039(6) 0.036(6) -0.009(5) -0.006(4) -0.016(5) C12_4 0.027(5) 0.029(6) 0.038(6) -0.007(5) 0.002(4) -0.009(5) O12_4 0.025(3) 0.038(4) 0.044(4) -0.012(3) 0.000(3) -0.010(3) C13_4 0.019(5) 0.032(6) 0.045(6) -0.018(5) -0.005(4) -0.005(4) C14_4 0.029(5) 0.047(6) 0.042(6) -0.022(5) -0.004(4) -0.017(5) C15_4 0.029(5) 0.035(6) 0.042(6) -0.017(5) -0.002(4) -0.008(5) C16_4 0.016(4) 0.044(6) 0.043(6) -0.016(5) -0.003(4) -0.012(5) O16_4 0.027(3) 0.045(4) 0.053(4) -0.018(4) -0.004(3) -0.018(3) C17_4 0.031(5) 0.042(7) 0.037(6) -0.008(5) 0.001(5) -0.009(5) N21_1 0.032(4) 0.040(5) 0.044(5) -0.015(4) 0.007(4) -0.018(4) C22_1 0.025(5) 0.053(7) 0.059(7) -0.028(6) 0.016(5) -0.020(5) N22_1 0.034(5) 0.063(6) 0.070(6) -0.043(5) 0.013(4) -0.026(5) C23_1 0.029(5) 0.040(6) 0.059(7) -0.015(5) -0.001(5) -0.015(5) C24_1 0.031(5) 0.051(7) 0.053(6) -0.021(6) 0.006(5) -0.028(5) C25_1 0.028(5) 0.048(7) 0.038(6) -0.008(5) 0.004(4) -0.018(5) C26_1 0.030(5) 0.047(7) 0.051(6) -0.024(5) 0.021(5) -0.016(5) C27_1 0.029(5) 0.048(7) 0.047(6) -0.005(6) 0.005(5) -0.020(5) N21_2 0.042(5) 0.045(6) 0.070(6) -0.026(5) 0.001(5) -0.011(5) C22_2 0.053(7) 0.054(8) 0.063(8) -0.020(7) -0.011(6) -0.009(7) N22_2 0.053(6) 0.060(7) 0.088(7) -0.036(6) 0.004(5) -0.004(5) C23_2 0.069(8) 0.043(7) 0.087(9) -0.028(7) 0.017(7) -0.031(7) C24_2 0.064(8) 0.041(7) 0.076(8) -0.008(6) 0.007(6) -0.028(7) C25_2 0.040(6) 0.036(6) 0.044(6) -0.005(5) -0.007(5) -0.012(5) C26_2 0.044(6) 0.049(7) 0.054(7) -0.015(6) -0.012(5) -0.020(6) C27_2 0.034(6) 0.046(7) 0.051(7) -0.010(6) 0.000(5) -0.015(6) N21_3 0.026(4) 0.045(5) 0.041(5) -0.020(4) 0.000(4) -0.017(4) C22_3 0.040(6) 0.054(7) 0.057(7) -0.022(6) 0.003(5) -0.030(6) N22_3 0.033(5) 0.052(6) 0.068(6) -0.026(5) 0.006(4) -0.019(4) C23_3 0.025(5) 0.058(7) 0.068(7) -0.032(6) 0.009(5) -0.020(5) C24_3 0.045(6) 0.059(7) 0.061(7) -0.030(6) 0.009(5) -0.033(6) C25_3 0.041(6) 0.050(7) 0.043(6) -0.011(5) -0.003(5) -0.028(6) C26_3 0.039(6) 0.047(7) 0.062(7) -0.029(6) 0.006(5) -0.021(6) C27_3 0.038(6) 0.045(7) 0.052(7) -0.007(6) 0.000(5) -0.014(6) N21_4 0.038(5) 0.043(5) 0.034(5) -0.012(4) 0.003(4) -0.013(4) C22_4 0.042(6) 0.039(6) 0.043(6) -0.008(5) -0.011(5) -0.025(5) N22_4 0.037(5) 0.071(6) 0.042(5) -0.024(5) 0.007(4) -0.027(5) C23_4 0.035(6) 0.059(7) 0.045(6) -0.019(6) 0.006(5) -0.026(6) C24_4 0.037(6) 0.058(7) 0.047(6) -0.021(6) 0.009(5) -0.025(6) C25_4 0.033(5) 0.036(6) 0.041(6) -0.012(5) -0.003(5) -0.013(5) C26_4 0.028(5) 0.044(6) 0.045(6) -0.020(5) -0.001(5) -0.016(5) C27_4 0.037(6) 0.047(7) 0.037(6) -0.005(5) 0.003(5) -0.026(5) _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 N1S C1S 1.208(11) . ? C1S C2S 1.498(11) . ? C2S H2A 0.9800 . ? C2S H2B 0.9800 . ? C2S H2C 0.9800 . ? N2S C3S 1.267(13) . ? C3S C4S 1.471(14) . ? C4S H4A 0.9800 . ? C4S H4B 0.9800 . ? C4S H4C 0.9800 . ? N3S C5S 1.366(18) . ? C5S C6S 1.501(18) . ? C6S H6A 0.9800 . ? C6S H6B 0.9800 . ? C6S H6C 0.9800 . ? N4S C7S 1.337(17) . ? C7S C8S 1.525(17) . ? C8S H8A 0.9800 . ? C8S H8B 0.9800 . ? C8S H8C 0.9800 . ? O1S C9S 1.35(2) . ? C9S C10S 1.70(4) . ? C9S H9A 0.9900 . ? C9S H9B 0.9900 . ? C10S H10A 0.9800 . ? C10S H10B 0.9800 . ? C10S H10C 0.9800 . ? C31_1 C15_2 1.509(10) . ? C31_1 C13_1 1.521(12) . ? C31_1 C32_1 1.538(11) . ? C31_1 H31_1 1.0000 . ? C32_1 C33A_1 1.542(10) . ? C32_1 H32A_1 0.9900 . ? C32_1 H32B_1 0.9900 . ? C33A_1 C34A_1 1.559(13) . ? C33A_1 H33A_1 0.9900 . ? C33A_1 H33B_1 0.9900 . ? C34A_1 C35A_1 1.578(14) . ? C34A_1 H34A_1 0.9900 . ? C34A_1 H34B_1 0.9900 . ? C35A_1 C36A_1 1.452(15) . ? C35A_1 H35A_1 0.9900 . ? C35A_1 H35B_1 0.9900 . ? C36A_1 H36A_1 0.9800 . ? C36A_1 H36B_1 0.9800 . ? C36A_1 H36B_1 0.9800 . ? C34B_1 C35B_1 1.547(16) . ? C34B_1 H34C_1 0.9900 . ? C34B_1 H34D_1 0.9900 . ? C35B_1 C36B_1 1.518(17) . ? C35B_1 H35C_1 0.9900 . ? C35B_1 H35D_1 0.9900 . ? C36B_1 H36D_1 0.9800 . ? C36B_1 H36E_1 0.9800 . ? C36B_1 H36F_1 0.9800 . ? C37_1 O16_2 1.390(10) . ? C37_1 O12_1 1.413(9) . ? C37_1 H37A_1 0.9900 . ? C37_1 H37B_1 0.9900 . ? C31_2 C32_2 1.513(11) . ? C31_2 C13_2 1.525(10) . ? C31_2 C15_3 1.540(12) . ? C31_2 H31_2 1.0000 . ? C32_2 C33_2 1.523(10) . ? C32_2 H32A_2 0.9900 . ? C32_2 H32B_2 0.9900 . ? C33_2 C34_2 1.490(13) . ? C33_2 H33A_2 0.9900 . ? C33_2 H33B_2 0.9900 . ? C34_2 C35_2 1.515(14) . ? C34_2 H34A_2 0.9900 . ? C34_2 H34B_2 0.9900 . ? C35_2 C36_2 1.286(16) . ? C35_2 H35A_2 0.9900 . ? C35_2 H35B_2 0.9900 . ? C36_2 H36A_2 0.9800 . ? C36_2 H36B_2 0.9800 . ? C36_2 H36C_2 0.9800 . ? C37_2 O12_2 1.422(9) . ? C37_2 O16_3 1.446(9) . ? C37_2 H37A_2 0.9900 . ? C37_2 H37B_2 0.9900 . ? C31_3 C13_3 1.502(12) . ? C31_3 C15_4 1.519(11) . ? C31_3 C32_3 1.529(11) . ? C31_3 H31_3 1.0000 . ? C32_3 C33_3 1.522(10) . ? C32_3 H32A_3 0.9900 . ? C32_3 H32B_3 0.9900 . ? C33_3 C34_3 1.537(11) . ? C33_3 H33A_3 0.9900 . ? C33_3 H33B_3 0.9900 . ? C34_3 C35_3 1.486(11) . ? C34_3 H34A_3 0.9900 . ? C34_3 H34B_3 0.9900 . ? C35_3 C36_3 1.509(12) . ? C35_3 H35A_3 0.9900 . ? C35_3 H35B_3 0.9900 . ? C36_3 H36A_3 0.9800 . ? C36_3 H36B_3 0.9800 . ? C36_3 H36C_3 0.9800 . ? C37_3 O16_4 1.400(9) . ? C37_3 O12_3 1.426(9) . ? C37_3 H37A_3 0.9900 . ? C37_3 H37B_3 0.9900 . ? C31_4 C15_1 1.514(12) . ? C31_4 C13_4 1.515(10) . ? C31_4 C32_4 1.551(11) . ? C31_4 H31_4 1.0000 . ? C32_4 C33_4 1.527(11) . ? C32_4 H32A_4 0.9900 . ? C32_4 H32B_4 0.9900 . ? C33_4 C34_4 1.507(15) . ? C33_4 H33A_4 0.9900 . ? C33_4 H33B_4 0.9900 . ? C34_4 C35_4 1.22(2) . ? C34_4 H34A_4 0.9900 . ? C34_4 H34B_4 0.9900 . ? C35_4 C36_4 1.580(17) . ? C35_4 H35A_4 0.9900 . ? C35_4 H35B_4 0.9900 . ? C36_4 H36A_4 0.9800 . ? C36_4 H36B_4 0.9800 . ? C36_4 H36C_4 0.9800 . ? C37_4 O12_4 1.431(9) . ? C37_4 O16_1 1.436(10) . ? C37_4 H37A_4 0.9900 . ? C37_4 H37B_4 0.9900 . ? C41_1 C46_1 1.351(12) . ? C41_1 C42_1 1.400(12) . ? C41_1 C47_1 1.512(12) . ? C47_1 O42_1 1.245(10) . ? C47_1 O41_1 1.273(10) . ? O41_1 H41_1 0.8400 . ? C42_1 C43_1 1.379(12) . ? C42_1 H42_1 0.9500 . ? C43_1 C44_1 1.374(13) . ? C43_1 N43_1 1.436(12) . ? N43_1 O43_1 1.234(11) . ? N43_1 O44_1 1.240(11) . ? C44_1 C45_1 1.358(12) . ? C44_1 H44_1 0.9500 . ? C45_1 C46_1 1.380(12) . ? C45_1 N45_1 1.469(12) . ? N45_1 O46_1 1.227(10) . ? N45_1 O45_1 1.242(10) . ? C46_1 H46_1 0.9500 . ? C41_2 C46_2 1.343(13) . ? C41_2 C42_2 1.411(14) . ? C41_2 C47_2 1.515(14) . ? C47_2 O42_2 1.214(13) . ? C47_2 O41_2 1.304(13) . ? O41_2 H41_2 0.8400 . ? C42_2 C43_2 1.360(13) . ? C42_2 H42_2 0.9500 . ? C43_2 C44_2 1.439(15) . ? C43_2 N43_2 1.450(14) . ? N43_2 O43_2 1.234(12) . ? N43_2 O44_2 1.271(11) . ? C44_2 C45_2 1.348(14) . ? C44_2 H44_2 0.9500 . ? C45_2 N45_2 1.411(14) . ? C45_2 C46_2 1.413(13) . ? N45_2 O46_2 1.211(12) . ? N45_2 O45_2 1.262(11) . ? C46_2 H46_2 0.9500 . ? C41_3 C46_3 1.401(11) . ? C41_3 C42_3 1.418(12) . ? C41_3 C47_3 1.488(11) . ? C47_3 O42_3 1.231(10) . ? C47_3 O41_3 1.276(10) . ? O41_3 H41_3 0.8400 . ? C42_3 C43_3 1.402(11) . ? C42_3 H42_3 0.9500 . ? C43_3 C44_3 1.398(12) . ? C43_3 N43_3 1.450(12) . ? N43_3 O43_3 1.199(11) . ? N43_3 O44_3 1.205(10) . ? C44_3 C45_3 1.348(12) . ? C44_3 H44_3 0.9500 . ? C45_3 C46_3 1.376(11) . ? C45_3 N45_3 1.456(11) . ? N45_3 O45_3 1.214(9) . ? N45_3 O46_3 1.217(10) . ? C46_3 H46_3 0.9500 . ? C41_4 C46_4 1.378(12) . ? C41_4 C42_4 1.393(12) . ? C41_4 C47_4 1.501(11) . ? C47_4 O41_4 1.238(10) . ? C47_4 O42_4 1.250(10) . ? O41_4 H41_4 0.8400 . ? C42_4 C43_4 1.381(11) . ? C42_4 H42_4 0.9500 . ? C43_4 C44_4 1.359(12) . ? C43_4 N43_4 1.470(11) . ? N43_4 O43_4 1.227(9) . ? N43_4 O44_4 1.231(9) . ? C44_4 C45_4 1.363(12) . ? C44_4 H44_4 0.9500 . ? C45_4 C46_4 1.418(11) . ? C45_4 N45_4 1.477(11) . ? N45_4 O46_4 1.198(10) . ? N45_4 O45_4 1.242(9) . ? C46_4 H46_4 0.9500 . ? C11_1 C12_1 1.357(11) . ? C11_1 C16_1 1.415(12) . ? C11_1 C17_1 1.458(12) . ? C12_1 C13_1 1.379(11) . ? C12_1 O12_1 1.407(9) . ? C13_1 C14_1 1.375(12) . ? C14_1 C15_1 1.368(11) . ? C14_1 H14_1 0.9500 . ? C15_1 C16_1 1.373(11) . ? C16_1 O16_1 1.362(10) . ? C17_1 C27_1 1.188(11) . ? C11_2 C12_2 1.399(10) . ? C11_2 C16_2 1.401(11) . ? C11_2 C17_2 1.433(13) . ? C12_2 O12_2 1.387(9) . ? C12_2 C13_2 1.396(11) . ? C13_2 C14_2 1.390(10) . ? C14_2 C15_2 1.382(10) . ? C14_2 H14_2 0.9500 . ? C15_2 C16_2 1.358(11) . ? C16_2 O16_2 1.408(9) . ? C17_2 C27_2 1.176(12) . ? C11_3 C12_3 1.339(12) . ? C11_3 C16_3 1.367(12) . ? C11_3 C17_3 1.430(12) . ? C12_3 O12_3 1.388(10) . ? C12_3 C13_3 1.435(11) . ? C13_3 C14_3 1.381(12) . ? C14_3 C15_3 1.362(11) . ? C14_3 H14_3 0.9500 . ? C15_3 C16_3 1.416(11) . ? C16_3 O16_3 1.369(10) . ? C17_3 C27_3 1.199(12) . ? C11_4 C16_4 1.395(11) . ? C11_4 C17_4 1.399(12) . ? C11_4 C12_4 1.424(11) . ? C12_4 O12_4 1.358(9) . ? C12_4 C13_4 1.381(11) . ? C13_4 C14_4 1.391(10) . ? C14_4 C15_4 1.421(10) . ? C14_4 H14_4 0.9500 . ? C15_4 C16_4 1.370(11) . ? C16_4 O16_4 1.396(9) . ? C17_4 C27_4 1.162(11) . ? N21_1 C26_1 1.346(9) . ? N21_1 C22_1 1.363(10) . ? C22_1 N22_1 1.322(10) . ? C22_1 C23_1 1.416(11) . ? N22_1 H22A_1 0.8800 . ? N22_1 H22B_1 0.8800 . ? C23_1 C24_1 1.344(11) . ? C23_1 H23_1 0.9500 . ? C24_1 C25_1 1.397(11) . ? C24_1 H24_1 0.9500 . ? C25_1 C26_1 1.360(10) . ? C25_1 C27_1 1.406(12) . ? C26_1 H26_1 0.9500 . ? N21_2 C22_2 1.342(12) . ? N21_2 C26_2 1.374(11) . ? C22_2 C23_2 1.364(13) . ? C22_2 N22_2 1.386(12) . ? N22_2 H22A_2 0.8800 . ? N22_2 H22B_2 0.8800 . ? C23_2 C24_2 1.388(13) . ? C23_2 H23_2 0.9500 . ? C24_2 C25_2 1.393(12) . ? C24_2 H24_2 0.9500 . ? C25_2 C26_2 1.379(12) . ? C25_2 C27_2 1.444(13) . ? C26_2 H26_2 0.9500 . ? N21_3 C22_3 1.327(10) . ? N21_3 C26_3 1.361(10) . ? C22_3 N22_3 1.338(10) . ? C22_3 C23_3 1.403(11) . ? N22_3 H22A_3 0.8800 . ? N22_3 H22B_3 0.8800 . ? C23_3 C24_3 1.344(11) . ? C23_3 H23_3 0.9500 . ? C24_3 C25_3 1.398(12) . ? C24_3 H24_3 0.9500 . ? C25_3 C26_3 1.360(11) . ? C25_3 C27_3 1.445(13) . ? C26_3 H26_3 0.9500 . ? N21_4 C22_4 1.347(10) . ? N21_4 C26_4 1.350(10) . ? C22_4 N22_4 1.358(10) . ? C22_4 C23_4 1.395(11) . ? N22_4 H22A_4 0.8800 . ? N22_4 H22B_4 0.8800 . ? C23_4 C24_4 1.356(11) . ? C23_4 H23_4 0.9500 . ? C24_4 C25_4 1.397(11) . ? C24_4 H24_4 0.9500 . ? C25_4 C26_4 1.383(11) . ? C25_4 C27_4 1.461(12) . ? C26_4 H26_4 0.9500 . ? 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 N1S C1S C2S 174.9(15) . . ? C1S C2S H2A 109.5 . . ? C1S C2S H2B 109.5 . . ? H2A C2S H2B 109.5 . . ? C1S C2S H2C 109.5 . . ? H2A C2S H2C 109.5 . . ? H2B C2S H2C 109.5 . . ? N2S C3S C4S 168.0(19) . . ? C3S C4S H4A 109.5 . . ? C3S C4S H4B 109.5 . . ? H4A C4S H4B 109.5 . . ? C3S C4S H4C 109.5 . . ? H4A C4S H4C 109.5 . . ? H4B C4S H4C 109.5 . . ? N3S C5S C6S 161(6) . . ? C5S C6S H6A 109.5 . . ? C5S C6S H6B 109.5 . . ? H6A C6S H6B 109.5 . . ? C5S C6S H6C 109.5 . . ? H6A C6S H6C 109.5 . . ? H6B C6S H6C 109.5 . . ? N4S C7S C8S 158(4) . . ? C7S C8S H8A 109.5 . . ? C7S C8S H8B 109.5 . . ? H8A C8S H8B 109.5 . . ? C7S C8S H8C 109.5 . . ? H8A C8S H8C 109.5 . . ? H8B C8S H8C 109.5 . . ? O1S C9S C10S 107.9(18) . . ? O1S C9S H9A 110.1 . . ? C10S C9S H9A 110.1 . . ? O1S C9S H9B 110.1 . . ? C10S C9S H9B 110.1 . . ? H9A C9S H9B 108.4 . . ? C9S C10S H10A 109.5 . . ? C9S C10S H10B 109.5 . . ? H10A C10S H10B 109.5 . . ? C9S C10S H10C 109.5 . . ? H10A C10S H10C 109.5 . . ? H10B C10S H10C 109.5 . . ? C15_2 C31_1 C13_1 109.1(7) . . ? C15_2 C31_1 C32_1 113.6(7) . . ? C13_1 C31_1 C32_1 113.6(8) . . ? C15_2 C31_1 H31_1 106.7 . . ? C13_1 C31_1 H31_1 106.7 . . ? C32_1 C31_1 H31_1 106.7 . . ? C31_1 C32_1 C33A_1 112.0(7) . . ? C31_1 C32_1 H32A_1 109.2 . . ? C33A_1 C32_1 H32A_1 109.2 . . ? C31_1 C32_1 H32B_1 109.2 . . ? C33A_1 C32_1 H32B_1 109.2 . . ? H32A_1 C32_1 H32B_1 107.9 . . ? C32_1 C33A_1 C34A_1 112.6(8) . . ? C32_1 C33A_1 H33A_1 109.1 . . ? C34A_1 C33A_1 H33A_1 109.1 . . ? C32_1 C33A_1 H33B_1 109.1 . . ? C34A_1 C33A_1 H33B_1 109.1 . . ? H33A_1 C33A_1 H33B_1 107.8 . . ? C33A_1 C34A_1 C35A_1 115.0(11) . . ? C33A_1 C34A_1 H34A_1 108.5 . . ? C35A_1 C34A_1 H34A_1 108.5 . . ? C33A_1 C34A_1 H34B_1 108.5 . . ? C35A_1 C34A_1 H34B_1 108.5 . . ? H34A_1 C34A_1 H34B_1 107.5 . . ? C36A_1 C35A_1 C34A_1 108.2(12) . . ? C36A_1 C35A_1 H35A_1 110.0 . . ? C34A_1 C35A_1 H35A_1 110.0 . . ? C36A_1 C35A_1 H35B_1 110.0 . . ? C34A_1 C35A_1 H35B_1 110.0 . . ? H35A_1 C35A_1 H35B_1 108.4 . . ? C35A_1 C36A_1 H36A_1 109.5 . . ? C35A_1 C36A_1 H36B_1 109.5 . . ? H36A_1 C36A_1 H36B_1 109.5 . . ? C35A_1 C36A_1 H36B_1 109.5 . . ? H36A_1 C36A_1 H36B_1 109.5 . . ? H36B_1 C36A_1 H36B_1 109.5 . . ? C35B_1 C34B_1 H34C_1 109.6 . . ? C35B_1 C34B_1 H34D_1 109.6 . . ? H34C_1 C34B_1 H34D_1 108.1 . . ? C36B_1 C35B_1 C34B_1 112.5(16) . . ? C36B_1 C35B_1 H35C_1 109.1 . . ? C34B_1 C35B_1 H35C_1 109.1 . . ? C36B_1 C35B_1 H35D_1 109.1 . . ? C34B_1 C35B_1 H35D_1 109.1 . . ? H35C_1 C35B_1 H35D_1 107.8 . . ? C35B_1 C36B_1 H36D_1 109.5 . . ? C35B_1 C36B_1 H36E_1 109.5 . . ? H36D_1 C36B_1 H36E_1 109.5 . . ? C35B_1 C36B_1 H36F_1 109.5 . . ? H36D_1 C36B_1 H36F_1 109.5 . . ? H36E_1 C36B_1 H36F_1 109.5 . . ? O16_2 C37_1 O12_1 112.3(7) . . ? O16_2 C37_1 H37A_1 109.1 . . ? O12_1 C37_1 H37A_1 109.1 . . ? O16_2 C37_1 H37B_1 109.1 . . ? O12_1 C37_1 H37B_1 109.1 . . ? H37A_1 C37_1 H37B_1 107.9 . . ? C32_2 C31_2 C13_2 113.8(7) . . ? C32_2 C31_2 C15_3 113.0(8) . . ? C13_2 C31_2 C15_3 108.7(7) . . ? C32_2 C31_2 H31_2 107.0 . . ? C13_2 C31_2 H31_2 107.0 . . ? C15_3 C31_2 H31_2 107.0 . . ? C31_2 C32_2 C33_2 111.6(7) . . ? C31_2 C32_2 H32A_2 109.3 . . ? C33_2 C32_2 H32A_2 109.3 . . ? C31_2 C32_2 H32B_2 109.3 . . ? C33_2 C32_2 H32B_2 109.3 . . ? H32A_2 C32_2 H32B_2 108.0 . . ? C34_2 C33_2 C32_2 114.4(8) . . ? C34_2 C33_2 H33A_2 108.7 . . ? C32_2 C33_2 H33A_2 108.7 . . ? C34_2 C33_2 H33B_2 108.7 . . ? C32_2 C33_2 H33B_2 108.7 . . ? H33A_2 C33_2 H33B_2 107.6 . . ? C33_2 C34_2 C35_2 115.9(11) . . ? C33_2 C34_2 H34A_2 108.3 . . ? C35_2 C34_2 H34A_2 108.3 . . ? C33_2 C34_2 H34B_2 108.3 . . ? C35_2 C34_2 H34B_2 108.3 . . ? H34A_2 C34_2 H34B_2 107.4 . . ? C36_2 C35_2 C34_2 118.5(13) . . ? C36_2 C35_2 H35A_2 107.7 . . ? C34_2 C35_2 H35A_2 107.7 . . ? C36_2 C35_2 H35B_2 107.7 . . ? C34_2 C35_2 H35B_2 107.7 . . ? H35A_2 C35_2 H35B_2 107.1 . . ? C35_2 C36_2 H36A_2 109.5 . . ? C35_2 C36_2 H36B_2 109.5 . . ? H36A_2 C36_2 H36B_2 109.5 . . ? C35_2 C36_2 H36C_2 109.5 . . ? H36A_2 C36_2 H36C_2 109.5 . . ? H36B_2 C36_2 H36C_2 109.5 . . ? O12_2 C37_2 O16_3 111.6(7) . . ? O12_2 C37_2 H37A_2 109.3 . . ? O16_3 C37_2 H37A_2 109.3 . . ? O12_2 C37_2 H37B_2 109.3 . . ? O16_3 C37_2 H37B_2 109.3 . . ? H37A_2 C37_2 H37B_2 108.0 . . ? C13_3 C31_3 C15_4 108.0(7) . . ? C13_3 C31_3 C32_3 114.7(8) . . ? C15_4 C31_3 C32_3 114.5(7) . . ? C13_3 C31_3 H31_3 106.4 . . ? C15_4 C31_3 H31_3 106.4 . . ? C32_3 C31_3 H31_3 106.4 . . ? C33_3 C32_3 C31_3 111.7(7) . . ? C33_3 C32_3 H32A_3 109.3 . . ? C31_3 C32_3 H32A_3 109.3 . . ? C33_3 C32_3 H32B_3 109.3 . . ? C31_3 C32_3 H32B_3 109.3 . . ? H32A_3 C32_3 H32B_3 107.9 . . ? C32_3 C33_3 C34_3 111.6(7) . . ? C32_3 C33_3 H33A_3 109.3 . . ? C34_3 C33_3 H33A_3 109.3 . . ? C32_3 C33_3 H33B_3 109.3 . . ? C34_3 C33_3 H33B_3 109.3 . . ? H33A_3 C33_3 H33B_3 108.0 . . ? C35_3 C34_3 C33_3 114.4(7) . . ? C35_3 C34_3 H34A_3 108.7 . . ? C33_3 C34_3 H34A_3 108.7 . . ? C35_3 C34_3 H34B_3 108.7 . . ? C33_3 C34_3 H34B_3 108.7 . . ? H34A_3 C34_3 H34B_3 107.6 . . ? C34_3 C35_3 C36_3 114.3(9) . . ? C34_3 C35_3 H35A_3 108.7 . . ? C36_3 C35_3 H35A_3 108.7 . . ? C34_3 C35_3 H35B_3 108.7 . . ? C36_3 C35_3 H35B_3 108.7 . . ? H35A_3 C35_3 H35B_3 107.6 . . ? C35_3 C36_3 H36A_3 109.5 . . ? C35_3 C36_3 H36B_3 109.5 . . ? H36A_3 C36_3 H36B_3 109.5 . . ? C35_3 C36_3 H36C_3 109.5 . . ? H36A_3 C36_3 H36C_3 109.5 . . ? H36B_3 C36_3 H36C_3 109.5 . . ? O16_4 C37_3 O12_3 112.5(7) . . ? O16_4 C37_3 H37A_3 109.1 . . ? O12_3 C37_3 H37A_3 109.1 . . ? O16_4 C37_3 H37B_3 109.1 . . ? O12_3 C37_3 H37B_3 109.1 . . ? H37A_3 C37_3 H37B_3 107.8 . . ? C15_1 C31_4 C13_4 108.9(7) . . ? C15_1 C31_4 C32_4 115.5(8) . . ? C13_4 C31_4 C32_4 113.6(7) . . ? C15_1 C31_4 H31_4 106.0 . . ? C13_4 C31_4 H31_4 106.0 . . ? C32_4 C31_4 H31_4 106.0 . . ? C33_4 C32_4 C31_4 111.7(7) . . ? C33_4 C32_4 H32A_4 109.3 . . ? C31_4 C32_4 H32A_4 109.3 . . ? C33_4 C32_4 H32B_4 109.3 . . ? C31_4 C32_4 H32B_4 109.3 . . ? H32A_4 C32_4 H32B_4 107.9 . . ? C34_4 C33_4 C32_4 112.9(9) . . ? C34_4 C33_4 H33A_4 109.0 . . ? C32_4 C33_4 H33A_4 109.0 . . ? C34_4 C33_4 H33B_4 109.0 . . ? C32_4 C33_4 H33B_4 109.0 . . ? H33A_4 C33_4 H33B_4 107.8 . . ? C35_4 C34_4 C33_4 122.8(18) . . ? C35_4 C34_4 H34A_4 106.6 . . ? C33_4 C34_4 H34A_4 106.6 . . ? C35_4 C34_4 H34B_4 106.6 . . ? C33_4 C34_4 H34B_4 106.6 . . ? H34A_4 C34_4 H34B_4 106.6 . . ? C34_4 C35_4 C36_4 120(2) . . ? C34_4 C35_4 H35A_4 107.4 . . ? C36_4 C35_4 H35A_4 107.4 . . ? C34_4 C35_4 H35B_4 107.4 . . ? C36_4 C35_4 H35B_4 107.4 . . ? H35A_4 C35_4 H35B_4 106.9 . . ? C35_4 C36_4 H36A_4 109.5 . . ? C35_4 C36_4 H36B_4 109.5 . . ? H36A_4 C36_4 H36B_4 109.5 . . ? C35_4 C36_4 H36C_4 109.5 . . ? H36A_4 C36_4 H36C_4 109.5 . . ? H36B_4 C36_4 H36C_4 109.5 . . ? O12_4 C37_4 O16_1 109.8(7) . . ? O12_4 C37_4 H37A_4 109.7 . . ? O16_1 C37_4 H37A_4 109.7 . . ? O12_4 C37_4 H37B_4 109.7 . . ? O16_1 C37_4 H37B_4 109.7 . . ? H37A_4 C37_4 H37B_4 108.2 . . ? C46_1 C41_1 C42_1 122.1(9) . . ? C46_1 C41_1 C47_1 122.1(9) . . ? C42_1 C41_1 C47_1 115.8(10) . . ? O42_1 C47_1 O41_1 125.7(8) . . ? O42_1 C47_1 C41_1 122.0(9) . . ? O41_1 C47_1 C41_1 112.3(9) . . ? C47_1 O41_1 H41_1 109.5 . . ? C43_1 C42_1 C41_1 117.5(10) . . ? C43_1 C42_1 H42_1 121.3 . . ? C41_1 C42_1 H42_1 121.3 . . ? C44_1 C43_1 C42_1 122.4(9) . . ? C44_1 C43_1 N43_1 119.6(10) . . ? C42_1 C43_1 N43_1 118.0(10) . . ? O43_1 N43_1 O44_1 124.1(10) . . ? O43_1 N43_1 C43_1 118.4(10) . . ? O44_1 N43_1 C43_1 117.5(11) . . ? C45_1 C44_1 C43_1 116.6(9) . . ? C45_1 C44_1 H44_1 121.7 . . ? C43_1 C44_1 H44_1 121.7 . . ? C44_1 C45_1 C46_1 124.5(10) . . ? C44_1 C45_1 N45_1 119.0(9) . . ? C46_1 C45_1 N45_1 116.4(10) . . ? O46_1 N45_1 O45_1 122.0(10) . . ? O46_1 N45_1 C45_1 121.2(9) . . ? O45_1 N45_1 C45_1 116.7(10) . . ? C41_1 C46_1 C45_1 116.9(10) . . ? C41_1 C46_1 H46_1 121.5 . . ? C45_1 C46_1 H46_1 121.5 . . ? C46_2 C41_2 C42_2 121.9(10) . . ? C46_2 C41_2 C47_2 121.9(12) . . ? C42_2 C41_2 C47_2 116.2(11) . . ? O42_2 C47_2 O41_2 123.8(12) . . ? O42_2 C47_2 C41_2 121.5(12) . . ? O41_2 C47_2 C41_2 114.7(12) . . ? C47_2 O41_2 H41_2 109.5 . . ? C43_2 C42_2 C41_2 116.6(12) . . ? C43_2 C42_2 H42_2 121.7 . . ? C41_2 C42_2 H42_2 121.7 . . ? C42_2 C43_2 C44_2 123.8(12) . . ? C42_2 C43_2 N43_2 118.7(13) . . ? C44_2 C43_2 N43_2 117.4(11) . . ? O43_2 N43_2 O44_2 122.9(12) . . ? O43_2 N43_2 C43_2 119.0(12) . . ? O44_2 N43_2 C43_2 118.1(12) . . ? C45_2 C44_2 C43_2 115.8(11) . . ? C45_2 C44_2 H44_2 122.1 . . ? C43_2 C44_2 H44_2 122.1 . . ? C44_2 C45_2 N45_2 118.7(11) . . ? C44_2 C45_2 C46_2 122.0(12) . . ? N45_2 C45_2 C46_2 119.2(12) . . ? O46_2 N45_2 O45_2 121.3(13) . . ? O46_2 N45_2 C45_2 120.4(11) . . ? O45_2 N45_2 C45_2 118.2(12) . . ? C41_2 C46_2 C45_2 119.5(12) . . ? C41_2 C46_2 H46_2 120.2 . . ? C45_2 C46_2 H46_2 120.2 . . ? C46_3 C41_3 C42_3 119.7(8) . . ? C46_3 C41_3 C47_3 123.2(9) . . ? C42_3 C41_3 C47_3 117.1(8) . . ? O42_3 C47_3 O41_3 127.6(8) . . ? O42_3 C47_3 C41_3 118.0(9) . . ? O41_3 C47_3 C41_3 114.4(9) . . ? C47_3 O41_3 H41_3 109.5 . . ? C43_3 C42_3 C41_3 118.2(8) . . ? C43_3 C42_3 H42_3 120.9 . . ? C41_3 C42_3 H42_3 120.9 . . ? C44_3 C43_3 C42_3 121.7(9) . . ? C44_3 C43_3 N43_3 120.5(9) . . ? C42_3 C43_3 N43_3 117.8(9) . . ? O43_3 N43_3 O44_3 125.0(11) . . ? O43_3 N43_3 C43_3 119.2(9) . . ? O44_3 N43_3 C43_3 115.7(10) . . ? C45_3 C44_3 C43_3 117.2(8) . . ? C45_3 C44_3 H44_3 121.4 . . ? C43_3 C44_3 H44_3 121.4 . . ? C44_3 C45_3 C46_3 124.8(9) . . ? C44_3 C45_3 N45_3 115.9(9) . . ? C46_3 C45_3 N45_3 119.3(9) . . ? O45_3 N45_3 O46_3 122.4(9) . . ? O45_3 N45_3 C45_3 120.2(10) . . ? O46_3 N45_3 C45_3 117.3(9) . . ? C45_3 C46_3 C41_3 118.1(9) . . ? C45_3 C46_3 H46_3 120.9 . . ? C41_3 C46_3 H46_3 120.9 . . ? C46_4 C41_4 C42_4 120.2(8) . . ? C46_4 C41_4 C47_4 119.7(9) . . ? C42_4 C41_4 C47_4 120.0(8) . . ? O41_4 C47_4 O42_4 125.9(8) . . ? O41_4 C47_4 C41_4 115.1(8) . . ? O42_4 C47_4 C41_4 118.9(9) . . ? C47_4 O41_4 H41_4 109.5 . . ? C43_4 C42_4 C41_4 118.6(9) . . ? C43_4 C42_4 H42_4 120.7 . . ? C41_4 C42_4 H42_4 120.7 . . ? C44_4 C43_4 C42_4 123.9(9) . . ? C44_4 C43_4 N43_4 117.5(8) . . ? C42_4 C43_4 N43_4 118.5(8) . . ? O43_4 N43_4 O44_4 123.8(9) . . ? O43_4 N43_4 C43_4 118.1(8) . . ? O44_4 N43_4 C43_4 118.1(8) . . ? C43_4 C44_4 C45_4 116.2(8) . . ? C43_4 C44_4 H44_4 121.9 . . ? C45_4 C44_4 H44_4 121.9 . . ? C44_4 C45_4 C46_4 123.5(8) . . ? C44_4 C45_4 N45_4 120.5(9) . . ? C46_4 C45_4 N45_4 115.9(9) . . ? O46_4 N45_4 O45_4 124.8(9) . . ? O46_4 N45_4 C45_4 120.4(8) . . ? O45_4 N45_4 C45_4 114.7(9) . . ? C41_4 C46_4 C45_4 117.5(9) . . ? C41_4 C46_4 H46_4 121.2 . . ? C45_4 C46_4 H46_4 121.2 . . ? C12_1 C11_1 C16_1 118.9(9) . . ? C12_1 C11_1 C17_1 122.4(9) . . ? C16_1 C11_1 C17_1 118.6(9) . . ? C11_1 C12_1 C13_1 122.4(9) . . ? C11_1 C12_1 O12_1 116.5(8) . . ? C13_1 C12_1 O12_1 121.0(9) . . ? C12_1 O12_1 C37_1 116.8(6) . . ? C14_1 C13_1 C12_1 117.3(9) . . ? C14_1 C13_1 C31_1 122.3(8) . . ? C12_1 C13_1 C31_1 120.3(9) . . ? C15_1 C14_1 C13_1 122.5(9) . . ? C15_1 C14_1 H14_1 118.8 . . ? C13_1 C14_1 H14_1 118.8 . . ? C14_1 C15_1 C16_1 119.4(9) . . ? C14_1 C15_1 C31_4 122.4(8) . . ? C16_1 C15_1 C31_4 117.8(9) . . ? O16_1 C16_1 C15_1 122.3(9) . . ? O16_1 C16_1 C11_1 118.3(8) . . ? C15_1 C16_1 C11_1 119.3(9) . . ? C16_1 O16_1 C37_4 115.8(6) . . ? C27_1 C17_1 C11_1 174.8(9) . . ? C12_2 C11_2 C16_2 118.0(8) . . ? C12_2 C11_2 C17_2 121.1(8) . . ? C16_2 C11_2 C17_2 121.0(8) . . ? O12_2 C12_2 C13_2 121.9(7) . . ? O12_2 C12_2 C11_2 117.8(8) . . ? C13_2 C12_2 C11_2 120.2(7) . . ? C12_2 O12_2 C37_2 116.6(7) . . ? C14_2 C13_2 C12_2 118.7(7) . . ? C14_2 C13_2 C31_2 121.8(8) . . ? C12_2 C13_2 C31_2 119.4(7) . . ? C15_2 C14_2 C13_2 122.2(8) . . ? C15_2 C14_2 H14_2 118.9 . . ? C13_2 C14_2 H14_2 118.9 . . ? C16_2 C15_2 C14_2 117.9(8) . . ? C16_2 C15_2 C31_1 119.7(7) . . ? C14_2 C15_2 C31_1 122.1(8) . . ? C15_2 C16_2 C11_2 123.0(8) . . ? C15_2 C16_2 O16_2 121.4(7) . . ? C11_2 C16_2 O16_2 115.5(8) . . ? C37_1 O16_2 C16_2 116.4(7) . . ? C27_2 C17_2 C11_2 174.6(9) . . ? C12_3 C11_3 C16_3 120.3(9) . . ? C12_3 C11_3 C17_3 119.5(9) . . ? C16_3 C11_3 C17_3 120.0(10) . . ? C11_3 C12_3 O12_3 120.3(8) . . ? C11_3 C12_3 C13_3 122.1(9) . . ? O12_3 C12_3 C13_3 117.5(9) . . ? C12_3 O12_3 C37_3 114.9(6) . . ? C14_3 C13_3 C12_3 115.6(9) . . ? C14_3 C13_3 C31_3 123.6(9) . . ? C12_3 C13_3 C31_3 120.7(9) . . ? C15_3 C14_3 C13_3 123.5(9) . . ? C15_3 C14_3 H14_3 118.2 . . ? C13_3 C14_3 H14_3 118.2 . . ? C14_3 C15_3 C16_3 118.0(9) . . ? C14_3 C15_3 C31_2 122.6(8) . . ? C16_3 C15_3 C31_2 119.1(9) . . ? C11_3 C16_3 O16_3 119.9(9) . . ? C11_3 C16_3 C15_3 120.2(9) . . ? O16_3 C16_3 C15_3 119.7(9) . . ? C16_3 O16_3 C37_2 114.3(6) . . ? C27_3 C17_3 C11_3 177.5(11) . . ? C16_4 C11_4 C17_4 122.6(8) . . ? C16_4 C11_4 C12_4 117.8(8) . . ? C17_4 C11_4 C12_4 119.7(8) . . ? O12_4 C12_4 C13_4 122.7(8) . . ? O12_4 C12_4 C11_4 116.6(8) . . ? C13_4 C12_4 C11_4 120.5(8) . . ? C12_4 O12_4 C37_4 119.4(7) . . ? C12_4 C13_4 C14_4 118.8(8) . . ? C12_4 C13_4 C31_4 119.1(7) . . ? C14_4 C13_4 C31_4 121.8(8) . . ? C13_4 C14_4 C15_4 122.8(8) . . ? C13_4 C14_4 H14_4 118.6 . . ? C15_4 C14_4 H14_4 118.6 . . ? C16_4 C15_4 C14_4 116.0(8) . . ? C16_4 C15_4 C31_3 122.1(8) . . ? C14_4 C15_4 C31_3 121.8(8) . . ? C15_4 C16_4 C11_4 123.9(8) . . ? C15_4 C16_4 O16_4 120.3(7) . . ? C11_4 C16_4 O16_4 115.7(8) . . ? C16_4 O16_4 C37_3 117.5(7) . . ? C27_4 C17_4 C11_4 175.9(11) . . ? C26_1 N21_1 C22_1 120.4(7) . . ? N22_1 C22_1 N21_1 117.2(7) . . ? N22_1 C22_1 C23_1 124.0(9) . . ? N21_1 C22_1 C23_1 118.8(8) . . ? C22_1 N22_1 H22A_1 120.0 . . ? C22_1 N22_1 H22B_1 120.0 . . ? H22A_1 N22_1 H22B_1 120.0 . . ? C24_1 C23_1 C22_1 119.2(9) . . ? C24_1 C23_1 H23_1 120.4 . . ? C22_1 C23_1 H23_1 120.4 . . ? C23_1 C24_1 C25_1 121.8(8) . . ? C23_1 C24_1 H24_1 119.1 . . ? C25_1 C24_1 H24_1 119.1 . . ? C26_1 C25_1 C24_1 117.2(8) . . ? C26_1 C25_1 C27_1 119.0(8) . . ? C24_1 C25_1 C27_1 123.7(8) . . ? N21_1 C26_1 C25_1 122.5(9) . . ? N21_1 C26_1 H26_1 118.7 . . ? C25_1 C26_1 H26_1 118.7 . . ? C17_1 C27_1 C25_1 174.8(11) . . ? C22_2 N21_2 C26_2 115.7(9) . . ? N21_2 C22_2 C23_2 124.0(10) . . ? N21_2 C22_2 N22_2 114.8(10) . . ? C23_2 C22_2 N22_2 121.2(11) . . ? C22_2 N22_2 H22A_2 120.0 . . ? C22_2 N22_2 H22B_2 120.0 . . ? H22A_2 N22_2 H22B_2 120.0 . . ? C22_2 C23_2 C24_2 118.2(10) . . ? C22_2 C23_2 H23_2 120.9 . . ? C24_2 C23_2 H23_2 120.9 . . ? C23_2 C24_2 C25_2 120.9(10) . . ? C23_2 C24_2 H24_2 119.5 . . ? C25_2 C24_2 H24_2 119.5 . . ? C26_2 C25_2 C24_2 115.7(10) . . ? C26_2 C25_2 C27_2 120.7(9) . . ? C24_2 C25_2 C27_2 123.6(9) . . ? N21_2 C26_2 C25_2 125.1(9) . . ? N21_2 C26_2 H26_2 117.5 . . ? C25_2 C26_2 H26_2 117.5 . . ? C17_2 C27_2 C25_2 175.9(11) . . ? C22_3 N21_3 C26_3 119.9(7) . . ? N21_3 C22_3 N22_3 118.0(8) . . ? N21_3 C22_3 C23_3 120.5(9) . . ? N22_3 C22_3 C23_3 121.5(9) . . ? C22_3 N22_3 H22A_3 120.0 . . ? C22_3 N22_3 H22B_3 120.0 . . ? H22A_3 N22_3 H22B_3 120.0 . . ? C24_3 C23_3 C22_3 119.1(9) . . ? C24_3 C23_3 H23_3 120.5 . . ? C22_3 C23_3 H23_3 120.5 . . ? C23_3 C24_3 C25_3 120.9(9) . . ? C23_3 C24_3 H24_3 119.5 . . ? C25_3 C24_3 H24_3 119.5 . . ? C26_3 C25_3 C24_3 117.5(9) . . ? C26_3 C25_3 C27_3 124.1(9) . . ? C24_3 C25_3 C27_3 118.4(8) . . ? C25_3 C26_3 N21_3 122.0(9) . . ? C25_3 C26_3 H26_3 119.0 . . ? N21_3 C26_3 H26_3 119.0 . . ? C17_3 C27_3 C25_3 171.6(10) . . ? C22_4 N21_4 C26_4 118.7(8) . . ? N21_4 C22_4 N22_4 112.9(7) . . ? N21_4 C22_4 C23_4 122.0(8) . . ? N22_4 C22_4 C23_4 125.1(9) . . ? C22_4 N22_4 H22A_4 120.0 . . ? C22_4 N22_4 H22B_4 120.0 . . ? H22A_4 N22_4 H22B_4 120.0 . . ? C24_4 C23_4 C22_4 117.5(8) . . ? C24_4 C23_4 H23_4 121.2 . . ? C22_4 C23_4 H23_4 121.2 . . ? C23_4 C24_4 C25_4 122.5(9) . . ? C23_4 C24_4 H24_4 118.8 . . ? C25_4 C24_4 H24_4 118.8 . . ? C26_4 C25_4 C24_4 116.2(9) . . ? C26_4 C25_4 C27_4 117.7(8) . . ? C24_4 C25_4 C27_4 126.0(8) . . ? N21_4 C26_4 C25_4 123.0(8) . . ? N21_4 C26_4 H26_4 118.5 . . ? C25_4 C26_4 H26_4 118.5 . . ? C17_4 C27_4 C25_4 175.7(9) . . ? 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 C15_2 C31_1 C32_1 C33A_1 173.0(7) . . . . ? C13_1 C31_1 C32_1 C33A_1 -61.4(10) . . . . ? C31_1 C32_1 C33A_1 C34A_1 -55.2(12) . . . . ? C32_1 C33A_1 C34A_1 C35A_1 179.5(12) . . . . ? C33A_1 C34A_1 C35A_1 C36A_1 -178.1(15) . . . . ? C13_2 C31_2 C32_2 C33_2 -166.8(8) . . . . ? C15_3 C31_2 C32_2 C33_2 68.7(10) . . . . ? C31_2 C32_2 C33_2 C34_2 179.3(10) . . . . ? C32_2 C33_2 C34_2 C35_2 -175.1(12) . . . . ? C33_2 C34_2 C35_2 C36_2 156.2(19) . . . . ? C13_3 C31_3 C32_3 C33_3 -57.2(10) . . . . ? C15_4 C31_3 C32_3 C33_3 177.2(8) . . . . ? C31_3 C32_3 C33_3 C34_3 -171.6(8) . . . . ? C32_3 C33_3 C34_3 C35_3 -175.9(8) . . . . ? C33_3 C34_3 C35_3 C36_3 -175.5(8) . . . . ? C15_1 C31_4 C32_4 C33_4 62.9(10) . . . . ? C13_4 C31_4 C32_4 C33_4 -170.2(8) . . . . ? C31_4 C32_4 C33_4 C34_4 178.4(11) . . . . ? C32_4 C33_4 C34_4 C35_4 -61(2) . . . . ? C33_4 C34_4 C35_4 C36_4 -175.6(13) . . . . ? C46_1 C41_1 C47_1 O42_1 -167.7(10) . . . . ? C42_1 C41_1 C47_1 O42_1 15.1(14) . . . . ? C46_1 C41_1 C47_1 O41_1 10.5(14) . . . . ? C42_1 C41_1 C47_1 O41_1 -166.6(9) . . . . ? C46_1 C41_1 C42_1 C43_1 2.4(15) . . . . ? C47_1 C41_1 C42_1 C43_1 179.5(9) . . . . ? C41_1 C42_1 C43_1 C44_1 -0.9(16) . . . . ? C41_1 C42_1 C43_1 N43_1 -179.5(10) . . . . ? C44_1 C43_1 N43_1 O43_1 -144.9(11) . . . . ? C42_1 C43_1 N43_1 O43_1 33.8(15) . . . . ? C44_1 C43_1 N43_1 O44_1 32.6(15) . . . . ? C42_1 C43_1 N43_1 O44_1 -148.7(10) . . . . ? C42_1 C43_1 C44_1 C45_1 -0.3(16) . . . . ? N43_1 C43_1 C44_1 C45_1 178.4(10) . . . . ? C43_1 C44_1 C45_1 C46_1 0.0(16) . . . . ? C43_1 C44_1 C45_1 N45_1 -177.0(9) . . . . ? C44_1 C45_1 N45_1 O46_1 169.1(10) . . . . ? C46_1 C45_1 N45_1 O46_1 -8.2(14) . . . . ? C44_1 C45_1 N45_1 O45_1 -12.9(14) . . . . ? C46_1 C45_1 N45_1 O45_1 169.9(9) . . . . ? C42_1 C41_1 C46_1 C45_1 -2.6(15) . . . . ? C47_1 C41_1 C46_1 C45_1 -179.6(9) . . . . ? C44_1 C45_1 C46_1 C41_1 1.4(16) . . . . ? N45_1 C45_1 C46_1 C41_1 178.5(9) . . . . ? C46_2 C41_2 C47_2 O42_2 -175.7(12) . . . . ? C42_2 C41_2 C47_2 O42_2 3.1(18) . . . . ? C46_2 C41_2 C47_2 O41_2 4.1(17) . . . . ? C42_2 C41_2 C47_2 O41_2 -177.1(11) . . . . ? C46_2 C41_2 C42_2 C43_2 0.6(17) . . . . ? C47_2 C41_2 C42_2 C43_2 -178.2(10) . . . . ? C41_2 C42_2 C43_2 C44_2 -0.1(18) . . . . ? C41_2 C42_2 C43_2 N43_2 177.8(10) . . . . ? C42_2 C43_2 N43_2 O43_2 8.2(17) . . . . ? C44_2 C43_2 N43_2 O43_2 -173.8(11) . . . . ? C42_2 C43_2 N43_2 O44_2 -170.2(11) . . . . ? C44_2 C43_2 N43_2 O44_2 7.8(16) . . . . ? C42_2 C43_2 C44_2 C45_2 -3.7(18) . . . . ? N43_2 C43_2 C44_2 C45_2 178.4(10) . . . . ? C43_2 C44_2 C45_2 N45_2 -178.1(10) . . . . ? C43_2 C44_2 C45_2 C46_2 7.0(17) . . . . ? C44_2 C45_2 N45_2 O46_2 169.8(12) . . . . ? C46_2 C45_2 N45_2 O46_2 -15.2(17) . . . . ? C44_2 C45_2 N45_2 O45_2 -8.2(17) . . . . ? C46_2 C45_2 N45_2 O45_2 166.9(10) . . . . ? C42_2 C41_2 C46_2 C45_2 2.6(17) . . . . ? C47_2 C41_2 C46_2 C45_2 -178.6(10) . . . . ? C44_2 C45_2 C46_2 C41_2 -6.8(17) . . . . ? N45_2 C45_2 C46_2 C41_2 178.3(11) . . . . ? C46_3 C41_3 C47_3 O42_3 -159.7(10) . . . . ? C42_3 C41_3 C47_3 O42_3 23.1(14) . . . . ? C46_3 C41_3 C47_3 O41_3 17.9(14) . . . . ? C42_3 C41_3 C47_3 O41_3 -159.4(9) . . . . ? C46_3 C41_3 C42_3 C43_3 -4.7(14) . . . . ? C47_3 C41_3 C42_3 C43_3 172.7(9) . . . . ? C41_3 C42_3 C43_3 C44_3 2.2(15) . . . . ? C41_3 C42_3 C43_3 N43_3 -178.6(9) . . . . ? C44_3 C43_3 N43_3 O43_3 168.9(11) . . . . ? C42_3 C43_3 N43_3 O43_3 -10.3(17) . . . . ? C44_3 C43_3 N43_3 O44_3 -13.9(17) . . . . ? C42_3 C43_3 N43_3 O44_3 166.9(11) . . . . ? C42_3 C43_3 C44_3 C45_3 1.7(16) . . . . ? N43_3 C43_3 C44_3 C45_3 -177.4(10) . . . . ? C43_3 C44_3 C45_3 C46_3 -3.4(16) . . . . ? C43_3 C44_3 C45_3 N45_3 176.8(9) . . . . ? C44_3 C45_3 N45_3 O45_3 10.7(15) . . . . ? C46_3 C45_3 N45_3 O45_3 -169.2(10) . . . . ? C44_3 C45_3 N45_3 O46_3 -173.4(10) . . . . ? C46_3 C45_3 N45_3 O46_3 6.7(15) . . . . ? C44_3 C45_3 C46_3 C41_3 1.0(16) . . . . ? N45_3 C45_3 C46_3 C41_3 -179.2(9) . . . . ? C42_3 C41_3 C46_3 C45_3 3.2(14) . . . . ? C47_3 C41_3 C46_3 C45_3 -174.0(9) . . . . ? C46_4 C41_4 C47_4 O41_4 -3.4(14) . . . . ? C42_4 C41_4 C47_4 O41_4 179.3(9) . . . . ? C46_4 C41_4 C47_4 O42_4 179.9(9) . . . . ? C42_4 C41_4 C47_4 O42_4 2.6(14) . . . . ? C46_4 C41_4 C42_4 C43_4 0.4(15) . . . . ? C47_4 C41_4 C42_4 C43_4 177.7(9) . . . . ? C41_4 C42_4 C43_4 C44_4 -1.6(15) . . . . ? C41_4 C42_4 C43_4 N43_4 178.0(9) . . . . ? C44_4 C43_4 N43_4 O43_4 169.9(9) . . . . ? C42_4 C43_4 N43_4 O43_4 -9.8(14) . . . . ? C44_4 C43_4 N43_4 O44_4 -9.0(14) . . . . ? C42_4 C43_4 N43_4 O44_4 171.3(9) . . . . ? C42_4 C43_4 C44_4 C45_4 2.6(16) . . . . ? N43_4 C43_4 C44_4 C45_4 -177.0(9) . . . . ? C43_4 C44_4 C45_4 C46_4 -2.6(15) . . . . ? C43_4 C44_4 C45_4 N45_4 -179.4(9) . . . . ? C44_4 C45_4 N45_4 O46_4 -163.3(10) . . . . ? C46_4 C45_4 N45_4 O46_4 19.7(14) . . . . ? C44_4 C45_4 N45_4 O45_4 19.7(14) . . . . ? C46_4 C45_4 N45_4 O45_4 -157.2(9) . . . . ? C42_4 C41_4 C46_4 C45_4 -0.4(15) . . . . ? C47_4 C41_4 C46_4 C45_4 -177.7(9) . . . . ? C44_4 C45_4 C46_4 C41_4 1.6(15) . . . . ? N45_4 C45_4 C46_4 C41_4 178.4(9) . . . . ? C16_1 C11_1 C12_1 C13_1 -0.3(12) . . . . ? C17_1 C11_1 C12_1 C13_1 179.5(8) . . . . ? C16_1 C11_1 C12_1 O12_1 -177.7(7) . . . . ? C17_1 C11_1 C12_1 O12_1 2.1(12) . . . . ? C11_1 C12_1 O12_1 C37_1 -102.3(8) . . . . ? C13_1 C12_1 O12_1 C37_1 80.2(10) . . . . ? O16_2 C37_1 O12_1 C12_1 -91.7(9) . . . . ? C11_1 C12_1 C13_1 C14_1 1.2(12) . . . . ? O12_1 C12_1 C13_1 C14_1 178.5(7) . . . . ? C11_1 C12_1 C13_1 C31_1 178.6(7) . . . . ? O12_1 C12_1 C13_1 C31_1 -4.2(11) . . . . ? C15_2 C31_1 C13_1 C14_1 92.2(9) . . . . ? C32_1 C31_1 C13_1 C14_1 -35.6(11) . . . . ? C15_2 C31_1 C13_1 C12_1 -85.0(9) . . . . ? C32_1 C31_1 C13_1 C12_1 147.2(7) . . . . ? C12_1 C13_1 C14_1 C15_1 -2.3(12) . . . . ? C31_1 C13_1 C14_1 C15_1 -179.6(7) . . . . ? C13_1 C14_1 C15_1 C16_1 2.4(12) . . . . ? C13_1 C14_1 C15_1 C31_4 175.7(7) . . . . ? C13_4 C31_4 C15_1 C14_1 -88.9(10) . . . . ? C32_4 C31_4 C15_1 C14_1 40.3(11) . . . . ? C13_4 C31_4 C15_1 C16_1 84.5(9) . . . . ? C32_4 C31_4 C15_1 C16_1 -146.3(7) . . . . ? C14_1 C15_1 C16_1 O16_1 -178.4(7) . . . . ? C31_4 C15_1 C16_1 O16_1 8.0(11) . . . . ? C14_1 C15_1 C16_1 C11_1 -1.4(12) . . . . ? C31_4 C15_1 C16_1 C11_1 -175.0(7) . . . . ? C12_1 C11_1 C16_1 O16_1 177.5(7) . . . . ? C17_1 C11_1 C16_1 O16_1 -2.3(11) . . . . ? C12_1 C11_1 C16_1 C15_1 0.4(12) . . . . ? C17_1 C11_1 C16_1 C15_1 -179.4(7) . . . . ? C15_1 C16_1 O16_1 C37_4 -88.2(9) . . . . ? C11_1 C16_1 O16_1 C37_4 94.8(9) . . . . ? O12_4 C37_4 O16_1 C16_1 90.6(9) . . . . ? C16_2 C11_2 C12_2 O12_2 -177.7(8) . . . . ? C17_2 C11_2 C12_2 O12_2 3.5(13) . . . . ? C16_2 C11_2 C12_2 C13_2 -0.3(13) . . . . ? C17_2 C11_2 C12_2 C13_2 -179.2(8) . . . . ? C13_2 C12_2 O12_2 C37_2 80.8(10) . . . . ? C11_2 C12_2 O12_2 C37_2 -101.8(9) . . . . ? O16_3 C37_2 O12_2 C12_2 -92.9(8) . . . . ? O12_2 C12_2 C13_2 C14_2 177.9(8) . . . . ? C11_2 C12_2 C13_2 C14_2 0.7(13) . . . . ? O12_2 C12_2 C13_2 C31_2 -5.4(13) . . . . ? C11_2 C12_2 C13_2 C31_2 177.4(8) . . . . ? C32_2 C31_2 C13_2 C14_2 -34.3(12) . . . . ? C15_3 C31_2 C13_2 C14_2 92.6(10) . . . . ? C32_2 C31_2 C13_2 C12_2 149.2(9) . . . . ? C15_3 C31_2 C13_2 C12_2 -84.0(10) . . . . ? C12_2 C13_2 C14_2 C15_2 -1.8(13) . . . . ? C31_2 C13_2 C14_2 C15_2 -178.4(8) . . . . ? C13_2 C14_2 C15_2 C16_2 2.5(13) . . . . ? C13_2 C14_2 C15_2 C31_1 177.0(8) . . . . ? C13_1 C31_1 C15_2 C16_2 81.9(10) . . . . ? C32_1 C31_1 C15_2 C16_2 -150.2(9) . . . . ? C13_1 C31_1 C15_2 C14_2 -92.4(10) . . . . ? C32_1 C31_1 C15_2 C14_2 35.5(12) . . . . ? C14_2 C15_2 C16_2 C11_2 -2.1(14) . . . . ? C31_1 C15_2 C16_2 C11_2 -176.7(9) . . . . ? C14_2 C15_2 C16_2 O16_2 -176.7(8) . . . . ? C31_1 C15_2 C16_2 O16_2 8.7(14) . . . . ? C12_2 C11_2 C16_2 C15_2 1.0(14) . . . . ? C17_2 C11_2 C16_2 C15_2 179.9(9) . . . . ? C12_2 C11_2 C16_2 O16_2 176.0(8) . . . . ? C17_2 C11_2 C16_2 O16_2 -5.2(13) . . . . ? O12_1 C37_1 O16_2 C16_2 92.6(9) . . . . ? C15_2 C16_2 O16_2 C37_1 -84.9(10) . . . . ? C11_2 C16_2 O16_2 C37_1 100.1(9) . . . . ? C16_3 C11_3 C12_3 O12_3 -179.8(7) . . . . ? C17_3 C11_3 C12_3 O12_3 5.7(12) . . . . ? C16_3 C11_3 C12_3 C13_3 -4.5(13) . . . . ? C17_3 C11_3 C12_3 C13_3 -179.1(7) . . . . ? C11_3 C12_3 O12_3 C37_3 -99.5(9) . . . . ? C13_3 C12_3 O12_3 C37_3 85.1(9) . . . . ? O16_4 C37_3 O12_3 C12_3 -95.8(9) . . . . ? C11_3 C12_3 C13_3 C14_3 3.1(12) . . . . ? O12_3 C12_3 C13_3 C14_3 178.5(7) . . . . ? C11_3 C12_3 C13_3 C31_3 179.7(8) . . . . ? O12_3 C12_3 C13_3 C31_3 -4.9(11) . . . . ? C15_4 C31_3 C13_3 C14_3 91.5(9) . . . . ? C32_3 C31_3 C13_3 C14_3 -37.4(11) . . . . ? C15_4 C31_3 C13_3 C12_3 -84.9(9) . . . . ? C32_3 C31_3 C13_3 C12_3 146.3(7) . . . . ? C12_3 C13_3 C14_3 C15_3 -2.2(12) . . . . ? C31_3 C13_3 C14_3 C15_3 -178.7(8) . . . . ? C13_3 C14_3 C15_3 C16_3 2.6(12) . . . . ? C13_3 C14_3 C15_3 C31_2 176.6(7) . . . . ? C32_2 C31_2 C15_3 C14_3 38.4(11) . . . . ? C13_2 C31_2 C15_3 C14_3 -88.9(9) . . . . ? C32_2 C31_2 C15_3 C16_3 -147.6(8) . . . . ? C13_2 C31_2 C15_3 C16_3 85.1(9) . . . . ? C12_3 C11_3 C16_3 O16_3 -179.6(8) . . . . ? C17_3 C11_3 C16_3 O16_3 -5.1(12) . . . . ? C12_3 C11_3 C16_3 C15_3 4.8(13) . . . . ? C17_3 C11_3 C16_3 C15_3 179.3(7) . . . . ? C14_3 C15_3 C16_3 C11_3 -3.8(12) . . . . ? C31_2 C15_3 C16_3 C11_3 -178.0(7) . . . . ? C14_3 C15_3 C16_3 O16_3 -179.4(7) . . . . ? C31_2 C15_3 C16_3 O16_3 6.4(11) . . . . ? C11_3 C16_3 O16_3 C37_2 99.3(9) . . . . ? C15_3 C16_3 O16_3 C37_2 -85.1(9) . . . . ? O12_2 C37_2 O16_3 C16_3 96.8(9) . . . . ? C16_4 C11_4 C12_4 O12_4 -172.2(8) . . . . ? C17_4 C11_4 C12_4 O12_4 7.8(12) . . . . ? C16_4 C11_4 C12_4 C13_4 3.6(13) . . . . ? C17_4 C11_4 C12_4 C13_4 -176.4(9) . . . . ? C13_4 C12_4 O12_4 C37_4 84.4(10) . . . . ? C11_4 C12_4 O12_4 C37_4 -100.0(9) . . . . ? O16_1 C37_4 O12_4 C12_4 -87.5(9) . . . . ? O12_4 C12_4 C13_4 C14_4 175.6(8) . . . . ? C11_4 C12_4 C13_4 C14_4 0.1(13) . . . . ? O12_4 C12_4 C13_4 C31_4 -10.7(13) . . . . ? C11_4 C12_4 C13_4 C31_4 173.8(8) . . . . ? C15_1 C31_4 C13_4 C12_4 -80.9(10) . . . . ? C32_4 C31_4 C13_4 C12_4 148.9(8) . . . . ? C15_1 C31_4 C13_4 C14_4 92.6(10) . . . . ? C32_4 C31_4 C13_4 C14_4 -37.6(12) . . . . ? C12_4 C13_4 C14_4 C15_4 -3.5(13) . . . . ? C31_4 C13_4 C14_4 C15_4 -177.0(8) . . . . ? C13_4 C14_4 C15_4 C16_4 2.9(13) . . . . ? C13_4 C14_4 C15_4 C31_3 178.6(8) . . . . ? C13_3 C31_3 C15_4 C16_4 81.3(11) . . . . ? C32_3 C31_3 C15_4 C16_4 -149.7(9) . . . . ? C13_3 C31_3 C15_4 C14_4 -94.2(10) . . . . ? C32_3 C31_3 C15_4 C14_4 34.8(12) . . . . ? C14_4 C15_4 C16_4 C11_4 1.2(14) . . . . ? C31_3 C15_4 C16_4 C11_4 -174.5(8) . . . . ? C14_4 C15_4 C16_4 O16_4 -175.7(8) . . . . ? C31_3 C15_4 C16_4 O16_4 8.6(13) . . . . ? C17_4 C11_4 C16_4 C15_4 175.7(9) . . . . ? C12_4 C11_4 C16_4 C15_4 -4.3(14) . . . . ? C17_4 C11_4 C16_4 O16_4 -7.3(13) . . . . ? C12_4 C11_4 C16_4 O16_4 172.7(8) . . . . ? C15_4 C16_4 O16_4 C37_3 -82.0(10) . . . . ? C11_4 C16_4 O16_4 C37_3 100.8(9) . . . . ? O12_3 C37_3 O16_4 C16_4 91.0(8) . . . . ? C26_1 N21_1 C22_1 N22_1 179.0(8) . . . . ? C26_1 N21_1 C22_1 C23_1 -2.8(14) . . . . ? N22_1 C22_1 C23_1 C24_1 178.2(9) . . . . ? N21_1 C22_1 C23_1 C24_1 0.1(14) . . . . ? C22_1 C23_1 C24_1 C25_1 1.0(15) . . . . ? C23_1 C24_1 C25_1 C26_1 0.5(14) . . . . ? C23_1 C24_1 C25_1 C27_1 -175.9(9) . . . . ? C22_1 N21_1 C26_1 C25_1 4.5(14) . . . . ? C24_1 C25_1 C26_1 N21_1 -3.3(14) . . . . ? C27_1 C25_1 C26_1 N21_1 173.3(9) . . . . ? C26_2 N21_2 C22_2 C23_2 -5.1(16) . . . . ? C26_2 N21_2 C22_2 N22_2 175.6(8) . . . . ? N21_2 C22_2 C23_2 C24_2 5.9(18) . . . . ? N22_2 C22_2 C23_2 C24_2 -174.9(10) . . . . ? C22_2 C23_2 C24_2 C25_2 -1.4(17) . . . . ? C23_2 C24_2 C25_2 C26_2 -3.2(15) . . . . ? C23_2 C24_2 C25_2 C27_2 173.2(10) . . . . ? C22_2 N21_2 C26_2 C25_2 -0.1(15) . . . . ? C24_2 C25_2 C26_2 N21_2 4.1(15) . . . . ? C27_2 C25_2 C26_2 N21_2 -172.4(9) . . . . ? C26_3 N21_3 C22_3 N22_3 -178.4(8) . . . . ? C26_3 N21_3 C22_3 C23_3 2.5(14) . . . . ? N21_3 C22_3 C23_3 C24_3 0.3(15) . . . . ? N22_3 C22_3 C23_3 C24_3 -178.8(10) . . . . ? C22_3 C23_3 C24_3 C25_3 -3.3(15) . . . . ? C23_3 C24_3 C25_3 C26_3 3.4(15) . . . . ? C23_3 C24_3 C25_3 C27_3 -177.6(9) . . . . ? C24_3 C25_3 C26_3 N21_3 -0.5(14) . . . . ? C27_3 C25_3 C26_3 N21_3 -179.5(9) . . . . ? C22_3 N21_3 C26_3 C25_3 -2.3(14) . . . . ? C26_4 N21_4 C22_4 N22_4 176.7(8) . . . . ? C26_4 N21_4 C22_4 C23_4 -2.6(14) . . . . ? N21_4 C22_4 C23_4 C24_4 2.7(14) . . . . ? N22_4 C22_4 C23_4 C24_4 -176.5(9) . . . . ? C22_4 C23_4 C24_4 C25_4 -1.6(15) . . . . ? C23_4 C24_4 C25_4 C26_4 0.6(14) . . . . ? C23_4 C24_4 C25_4 C27_4 175.7(10) . . . . ? C22_4 N21_4 C26_4 C25_4 1.5(13) . . . . ? C24_4 C25_4 C26_4 N21_4 -0.5(14) . . . . ? C27_4 C25_4 C26_4 N21_4 -176.0(8) . . . . ? 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 O41_1 H41_1 N21_1 0.84 1.74 2.558(8) 164.2 . O41_2 H41_2 N21_2 0.84 1.75 2.582(10) 170.6 . O41_3 H41_3 N21_3 0.84 1.88 2.703(8) 168.0 . O41_4 H41_4 N21_4 0.84 1.76 2.579(9) 163.5 . N22_1 H22A_1 O42_1 0.88 1.89 2.765(9) 176.8 . N22_2 H22A_2 O42_2 0.88 2.06 2.863(12) 151.7 . N22_3 H22A_3 O42_3 0.88 1.85 2.724(9) 169.7 . N22_4 H22A_4 O42_4 0.88 2.01 2.878(9) 171.1 . N22_1 H22B_1 O42_4 0.88 2.32 2.967(10) 130.2 2_665 N22_2 H22B_2 N4S 0.88 2.18 3.04(3) 167.3 . N22_3 H22B_3 O42_4 0.88 2.23 2.919(10) 135.2 2_565 N22_4 H22B_4 O42_3 0.88 2.03 2.776(9) 141.9 2_565 _diffrn_measured_fraction_theta_max 0.952 _diffrn_reflns_theta_full 27.65 _diffrn_measured_fraction_theta_full 0.952 _refine_diff_density_max 0.700 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.099 #END data_7 _database_code_depnum_ccdc_archive 'CCDC 629288' _audit_creation_method SHELXL-97 _chemical_name_systematic ; NS6S (6-amino-3-pyridyl)ethynyl cavitand, glutaric acid ; _chemical_name_common 'NS6S (6-amino-3-pyridyl)ethynyl cavitand, glutaric acid' _chemical_melting_point ? _chemical_formula_moiety ; (C5 H8 O4)2 (C80 H80 N8 O8) (C8 H10)1.2 (C2 H3 N) ; _chemical_formula_sum 'C101.60 H111 N9 O16' _chemical_formula_weight 1714.19 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 Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 12.7783(9) _cell_length_b 24.5634(18) _cell_length_c 29.317(2) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9202.1(11) _cell_formula_units_Z 4 _cell_measurement_temperature 85(2) _cell_measurement_reflns_used 9387 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 26.90 _exptl_crystal_description prism _exptl_crystal_colour orange _exptl_crystal_size_min 0.14 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_max 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.237 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3646 _exptl_absorpt_coefficient_mu 0.084 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 85(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 48646 _diffrn_reflns_av_R_equivalents 0.0618 _diffrn_reflns_av_sigmaI/netI 0.0623 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 37 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 28.37 _reflns_number_total 11429 _reflns_number_gt 6279 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker XSCANS' _computing_cell_refinement 'Bruker XSCANS' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.1600P)^2^+10.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 11429 _refine_ls_number_parameters 651 _refine_ls_number_restraints 86 _refine_ls_R_factor_all 0.1589 _refine_ls_R_factor_gt 0.0945 _refine_ls_wR_factor_ref 0.3114 _refine_ls_wR_factor_gt 0.2654 _refine_ls_goodness_of_fit_ref 1.020 _refine_ls_restrained_S_all 1.029 _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 C81 C 0.0695(6) 0.2365(6) 0.24783(13) 0.240(6) Uiso 0.35 1 d PD A -1 C82 C 0.1455(7) 0.1972(6) 0.25578(15) 0.240(6) Uiso 0.35 1 d PD A -1 H82A H 0.1276 0.1597 0.2548 0.288 Uiso 0.35 1 calc PR A -1 C83 C 0.2475(7) 0.2128(5) 0.26512(19) 0.240(6) Uiso 0.35 1 d PD A -1 H83A H 0.2999 0.1862 0.2706 0.288 Uiso 0.35 1 calc PR A -1 C84 C 0.2726(8) 0.2682(5) 0.2664(2) 0.240(6) Uiso 0.35 1 d PD A -1 C85 C 0.1974(8) 0.3070(5) 0.2586(3) 0.240(6) Uiso 0.35 1 d PD A -1 H85A H 0.2176 0.3442 0.2598 0.288 Uiso 0.35 1 calc PR A -1 C86 C 0.0941(8) 0.2949(8) 0.2490(3) 0.240(6) Uiso 0.35 1 d PD A -1 H86A H 0.0429 0.3223 0.2436 0.288 Uiso 0.35 1 calc PR A -1 C87 C -0.0402(7) 0.2216(8) 0.2377(3) 0.240(6) Uiso 0.35 1 d PD A -1 H87A H -0.0484 0.1820 0.2401 0.359 Uiso 0.35 1 calc PR A -1 H87B H -0.0581 0.2333 0.2068 0.359 Uiso 0.35 1 calc PR A -1 H87C H -0.0868 0.2395 0.2596 0.359 Uiso 0.35 1 calc PR A -1 C88 C 0.3839(8) 0.2844(8) 0.2766(4) 0.240(6) Uiso 0.35 1 d PD A -1 H88A H 0.3896 0.3242 0.2765 0.359 Uiso 0.35 1 calc PR A -1 H88B H 0.4304 0.2692 0.2533 0.359 Uiso 0.35 1 calc PR A -1 H88C H 0.4041 0.2704 0.3066 0.359 Uiso 0.35 1 calc PR A -1 C91 C -0.0060(7) 0.25296(14) 0.5310(3) 0.150 Uiso 0.25 1 d PD B -1 C92 C -0.0529(8) 0.22383(14) 0.4961(3) 0.150 Uiso 0.25 1 d PD B -1 H92 H -0.0109 0.2052 0.4743 0.180 Uiso 0.25 1 calc PR B -1 C93 C -0.1611(8) 0.2218(3) 0.4927(3) 0.150 Uiso 0.25 1 d PD B -1 H93 H -0.1932 0.2019 0.4688 0.180 Uiso 0.25 1 calc PR B -1 C94 C -0.2224(7) 0.2491(4) 0.5245(4) 0.150 Uiso 0.50 2 d SPD B -1 C95 C -0.1766(8) 0.2783(4) 0.5595(4) 0.150 Uiso 0.25 1 d PD B -1 H95 H -0.2191 0.2968 0.5810 0.180 Uiso 0.25 1 calc PR B -1 C96 C -0.0676(8) 0.2805(5) 0.5632(5) 0.150 Uiso 0.25 1 d PD B -1 H96 H -0.0357 0.3005 0.5872 0.180 Uiso 0.25 1 calc PR B -1 C97 C 0.1115(8) 0.2554(5) 0.5350(6) 0.150 Uiso 0.25 1 d PD B -1 H97A H 0.1432 0.2349 0.5098 0.225 Uiso 0.25 1 calc PR B -1 H97B H 0.1332 0.2394 0.5641 0.225 Uiso 0.25 1 calc PR B -1 H97C H 0.1345 0.2934 0.5336 0.225 Uiso 0.25 1 calc PR B -1 C98 C -0.3395(8) 0.2468(7) 0.5207(6) 0.150 Uiso 0.25 1 d PD B -1 H98A H -0.3710 0.2668 0.5462 0.225 Uiso 0.25 1 calc PR B -1 H98B H -0.3626 0.2088 0.5217 0.225 Uiso 0.25 1 calc PR B -1 H98C H -0.3615 0.2634 0.4919 0.225 Uiso 0.25 1 calc PR B -1 N1S N -0.3661(7) 0.2500 0.5191(4) 0.058(2) Uiso 0.50 2 d SPD C 2 C1S C -0.2733(10) 0.2500 0.5413(5) 0.077(4) Uiso 0.50 2 d SPD C 2 C2S C -0.1808(13) 0.2500 0.5693(7) 0.157(10) Uiso 0.50 2 d SPD C 2 H2C H -0.1154(15) 0.2500 0.5501(13) 0.236 Uiso 0.50 2 d SPD D 2 H2D H -0.180(3) 0.2835(11) 0.5895(12) 0.236 Uiso 0.25 1 d PD E 2 H2E H -0.180(3) 0.2165(12) 0.5895(12) 0.236 Uiso 0.25 1 d PD F 2 N2S N 0.2279(6) 0.2500 0.5376(3) 0.0380(18) Uiso 0.50 2 d SPD G 2 C3S C 0.1326(7) 0.2500 0.5440(4) 0.039(2) Uiso 0.50 2 d SPD G 2 C4S C 0.0146(9) 0.2500 0.5499(5) 0.097(5) Uiso 0.50 2 d SPD G 2 H4C H -0.018(2) 0.2500 0.5195(9) 0.145 Uiso 0.50 2 d SPD H 2 H4D H -0.002(2) 0.2835(11) 0.5680(12) 0.145 Uiso 0.25 1 d PD I 2 H4E H -0.002(2) 0.2165(12) 0.5680(12) 0.145 Uiso 0.25 1 d PD J 2 C11 C 0.6046(2) 0.35928(18) 0.42720(13) 0.0498(10) Uani 1 1 d . . . C12 C 0.5681(2) 0.38314(16) 0.46734(12) 0.0424(9) Uani 1 1 d . . . O12 O 0.62385(17) 0.42624(11) 0.48514(9) 0.0484(7) Uani 1 1 d . . . C13 C 0.4732(2) 0.36670(15) 0.48718(11) 0.0377(8) Uani 1 1 d . . . C14 C 0.4195(2) 0.32419(15) 0.46631(11) 0.0372(8) Uani 1 1 d . . . H14 H 0.3567 0.3117 0.4801 0.045 Uiso 1 1 calc R . . C15 C 0.4525(2) 0.29906(17) 0.42644(11) 0.0434(9) Uani 1 1 d . . . C16 C 0.5460(3) 0.31780(19) 0.40700(12) 0.0493(10) Uani 1 1 d . . . O16 O 0.57991(19) 0.29795(15) 0.36551(8) 0.0631(9) Uani 1 1 d . . . C17 C 0.7005(3) 0.37613(19) 0.40554(14) 0.0561(11) Uani 1 1 d . . . C21 C 0.6339(2) 0.36001(14) 0.62475(11) 0.0332(7) Uani 1 1 d . . . C22 C 0.5825(2) 0.31852(13) 0.64767(10) 0.0301(7) Uani 1 1 d . . . O22 O 0.62780(16) 0.29775(9) 0.68697(7) 0.0336(5) Uani 1 1 d . . . C23 C 0.4843(2) 0.29938(13) 0.63306(10) 0.0281(6) Uani 1 1 d . . . C24 C 0.4396(2) 0.32389(13) 0.59529(10) 0.0288(7) Uani 1 1 d . . . H24 H 0.3734 0.3113 0.5851 0.035 Uiso 1 1 calc R . . C25 C 0.4876(2) 0.36631(14) 0.57158(11) 0.0324(7) Uani 1 1 d . . . C26 C 0.5865(2) 0.38294(14) 0.58607(12) 0.0344(7) Uani 1 1 d . . . O26 O 0.63754(17) 0.42594(10) 0.56519(9) 0.0429(6) Uani 1 1 d . . . C27 C 0.7337(2) 0.37850(14) 0.64123(11) 0.0363(7) Uani 1 1 d . . . C31 C 0.4358(2) 0.39344(14) 0.53072(11) 0.0347(7) Uani 1 1 d . . . H31 H 0.4610 0.4320 0.5300 0.042 Uiso 1 1 calc R . . C32 C 0.3157(2) 0.39558(14) 0.53527(12) 0.0355(7) Uani 1 1 d . L . H32A H 0.2869 0.3585 0.5313 0.043 Uiso 1 1 calc R . . H32B H 0.2972 0.4081 0.5663 0.043 Uiso 1 1 calc R . . C33 C 0.2662(2) 0.43333(16) 0.50051(14) 0.0457(9) Uani 1 1 d D . . H33A H 0.2765 0.4176 0.4697 0.055 Uiso 1 1 calc R K 1 H33B H 0.3034 0.4687 0.5014 0.055 Uiso 1 1 calc R K 1 C34A C 0.1495(5) 0.4437(4) 0.5077(3) 0.045(2) Uani 0.550(7) 1 d PD L 1 H34A H 0.1377 0.4573 0.5390 0.054 Uiso 0.550(7) 1 calc PR L 1 H34B H 0.1254 0.4720 0.4861 0.054 Uiso 0.550(7) 1 calc PR L 1 C35A C 0.0867(5) 0.3921(3) 0.5003(3) 0.062(3) Uani 0.550(7) 1 d PD L 1 H35A H 0.1085 0.3648 0.5233 0.075 Uiso 0.550(7) 1 calc PR L 1 H35B H 0.1039 0.3772 0.4699 0.075 Uiso 0.550(7) 1 calc PR L 1 C36A C -0.0315(5) 0.3997(5) 0.5035(4) 0.079(3) Uani 0.550(7) 1 d PD L 1 H36A H -0.0664 0.3648 0.4980 0.119 Uiso 0.550(7) 1 calc PR L 1 H36B H -0.0542 0.4262 0.4806 0.119 Uiso 0.550(7) 1 calc PR L 1 H36C H -0.0498 0.4130 0.5340 0.119 Uiso 0.550(7) 1 calc PR L 1 C34B C 0.1488(7) 0.4232(5) 0.4946(4) 0.045(2) Uani 0.450(7) 1 d PD L 2 H34C H 0.1220 0.4483 0.4710 0.054 Uiso 0.450(7) 1 calc PR L 2 H34D H 0.1388 0.3856 0.4832 0.054 Uiso 0.450(7) 1 calc PR L 2 C35B C 0.0835(5) 0.4302(5) 0.5372(3) 0.057(3) Uani 0.450(7) 1 d PD L 2 H35C H 0.0967 0.4669 0.5501 0.068 Uiso 0.450(7) 1 calc PR L 2 H35D H 0.1058 0.4030 0.5602 0.068 Uiso 0.450(7) 1 calc PR L 2 C36B C -0.0331(6) 0.4238(7) 0.5286(3) 0.077(5) Uani 0.450(7) 1 d PD L 2 H36D H -0.0714 0.4297 0.5571 0.116 Uiso 0.450(7) 1 calc PR L 2 H36E H -0.0472 0.3870 0.5173 0.116 Uiso 0.450(7) 1 calc PR L 2 H36F H -0.0558 0.4505 0.5059 0.116 Uiso 0.450(7) 1 calc PR L 2 C37 C 0.6884(2) 0.41513(17) 0.52344(13) 0.0461(9) Uani 1 1 d . . . H37A H 0.7097 0.3764 0.5227 0.055 Uiso 1 1 calc R . . H37B H 0.7525 0.4376 0.5215 0.055 Uiso 1 1 calc R . . C41 C 0.4364(3) 0.2500 0.65616(14) 0.0284(9) Uani 1 2 d S . . H41 H 0.4604 0.2500 0.6886 0.034 Uiso 1 2 calc SR . . C42 C 0.3164(3) 0.2500 0.65655(14) 0.0309(10) Uani 1 2 d S . . H42A H 0.2911 0.2567 0.6251 0.037 Uiso 0.50 1 calc PR M . H42B H 0.2918 0.2134 0.6658 0.037 Uiso 0.50 1 calc PR . . C43 C 0.2696(5) 0.2904(3) 0.6868(2) 0.0339(14) Uani 0.50 1 d P M -1 H43A H 0.2999 0.3265 0.6796 0.041 Uiso 0.50 1 calc PR M -1 H43B H 0.2891 0.2815 0.7187 0.041 Uiso 0.50 1 calc PR M -1 C44 C 0.1503(5) 0.2945(3) 0.6839(3) 0.0441(17) Uani 0.50 1 d P M -1 H44A H 0.1280 0.3235 0.7052 0.053 Uiso 0.50 1 calc PR M -1 H44B H 0.1329 0.3072 0.6527 0.053 Uiso 0.50 1 calc PR M -1 C45 C 0.0898(4) 0.2500 0.6925(2) 0.0548(15) Uani 1 2 d S . . H45A H 0.1128 0.2359 0.7225 0.066 Uiso 0.50 1 calc PR M . H45B H 0.1102 0.2223 0.6696 0.066 Uiso 0.50 1 calc PR . . C46 C -0.0282(4) 0.2500 0.6936(2) 0.0588(16) Uani 1 2 d S M . H46A H -0.0534 0.2133 0.7006 0.088 Uiso 0.50 1 calc PR . . H46B H -0.0552 0.2614 0.6638 0.088 Uiso 0.50 1 calc PR . . H46C H -0.0525 0.2753 0.7171 0.088 Uiso 0.50 1 calc PR . . C47 C 0.6878(3) 0.2500 0.68168(15) 0.0349(10) Uani 1 2 d S . . H47A H 0.7201 0.2500 0.6510 0.042 Uiso 1 2 calc SR . . H47B H 0.7449 0.2500 0.7045 0.042 Uiso 1 2 calc SR . . C51 C 0.3989(3) 0.2500 0.40624(16) 0.0464(14) Uani 1 2 d S . . H51 H 0.4141 0.2500 0.3728 0.056 Uiso 1 2 calc SR . . C52 C 0.2789(4) 0.2500 0.41185(18) 0.0520(15) Uani 1 2 d S . . H52A H 0.2525 0.2133 0.4039 0.062 Uiso 0.50 1 d PR . . H52B H 0.2625 0.2565 0.4444 0.062 Uiso 0.50 1 d PR . . C53 C 0.2244(5) 0.2876(4) 0.3860(3) 0.056(2) Uani 0.50 1 d PD . . H53A H 0.2449 0.2823 0.3538 0.068 Uiso 0.50 1 calc PR N . H53B H 0.2489 0.3243 0.3951 0.068 Uiso 0.50 1 calc PR . . C54A C 0.1064(7) 0.2878(5) 0.3881(4) 0.093(3) Uiso 0.300(5) 1 d PD N -1 H54A H 0.0852 0.2926 0.4203 0.112 Uiso 0.300(5) 1 calc PR N -1 H54B H 0.0809 0.3200 0.3710 0.112 Uiso 0.300(5) 1 calc PR N -1 C55A C 0.0533(9) 0.2401(7) 0.3703(5) 0.079(4) Uiso 0.300(5) 1 d PD N -1 H55A H 0.0688 0.2088 0.3905 0.095 Uiso 0.300(5) 1 calc PR N -1 H55B H 0.0827 0.2315 0.3398 0.095 Uiso 0.300(5) 1 calc PR N -1 C56A C -0.0670(8) 0.2457(14) 0.3658(4) 0.074(3) Uiso 0.300(5) 1 d PD N -1 H56A H -0.0957 0.2127 0.3517 0.110 Uiso 0.300(5) 1 calc PR N -1 H56B H -0.0835 0.2772 0.3466 0.110 Uiso 0.300(5) 1 calc PR N -1 H56C H -0.0978 0.2507 0.3961 0.110 Uiso 0.599(9) 2 calc SPR N -1 C54B C 0.1064(7) 0.2878(5) 0.3881(4) 0.093(3) Uiso 0.200(5) 1 d PD N -2 H54C H 0.0846 0.3262 0.3840 0.112 Uiso 0.200(5) 1 calc PR N -2 H54D H 0.0821 0.2680 0.3606 0.112 Uiso 0.200(5) 1 calc PR N -2 C55B C 0.0449(11) 0.2666(10) 0.4264(6) 0.079(4) Uiso 0.200(5) 1 d PD N -2 H55C H 0.0546 0.2914 0.4527 0.095 Uiso 0.200(5) 1 calc PR N -2 H55D H 0.0740 0.2307 0.4351 0.095 Uiso 0.200(5) 1 calc PR N -2 C56B C -0.0751(11) 0.2597(11) 0.4180(7) 0.074(3) Uiso 0.200(5) 1 d PD N -2 H56D H -0.0893 0.2605 0.3852 0.110 Uiso 0.200(5) 1 calc PR N -2 H56E H -0.1130 0.2895 0.4330 0.110 Uiso 0.200(5) 1 calc PR N -2 H56F H -0.0983 0.2248 0.4307 0.110 Uiso 0.200(5) 1 calc PR N -2 C57 C 0.6417(4) 0.2500 0.3672(2) 0.0661(19) Uani 1 2 d S . . H57A H 0.6911 0.2500 0.3412 0.079 Uiso 1 2 calc SR . . H57B H 0.6833 0.2500 0.3957 0.079 Uiso 1 2 calc SR . . N61 N 1.0403(2) 0.42724(17) 0.34323(11) 0.0600(10) Uani 1 1 d . . . C62 C 1.0218(3) 0.43522(19) 0.29862(13) 0.0537(11) Uani 1 1 d . . . N62 N 1.1030(2) 0.45071(19) 0.27308(11) 0.0714(12) Uani 1 1 d . . . H62A H 1.1649 0.4552 0.2856 0.086 Uiso 1 1 calc R . . H62B H 1.0946 0.4564 0.2437 0.086 Uiso 1 1 calc R . . C63 C 0.9219(3) 0.4266(2) 0.28024(13) 0.0562(11) Uani 1 1 d . . . H63 H 0.9096 0.4318 0.2486 0.067 Uiso 1 1 calc R . . C64 C 0.8429(3) 0.41084(18) 0.30840(14) 0.0533(10) Uani 1 1 d . . . H64 H 0.7750 0.4047 0.2962 0.064 Uiso 1 1 calc R . . C65 C 0.8604(3) 0.40359(18) 0.35491(13) 0.0514(10) Uani 1 1 d . . . C66 C 0.9606(3) 0.4119(2) 0.36991(15) 0.0645(13) Uani 1 1 d . . . H66 H 0.9746 0.4064 0.4014 0.077 Uiso 1 1 calc R . . C67 C 0.7762(3) 0.3882(2) 0.38448(14) 0.0577(11) Uani 1 1 d . . . N71 N 1.0849(2) 0.43823(15) 0.68330(10) 0.0487(8) Uani 1 1 d . . . C72 C 1.0889(3) 0.42968(17) 0.72878(12) 0.0440(9) Uani 1 1 d . . . N72 N 1.1784(2) 0.44303(16) 0.75033(11) 0.0572(9) Uani 1 1 d . . . H72A H 1.2312 0.4567 0.7348 0.069 Uiso 1 1 calc R . . H72B H 1.1842 0.4381 0.7800 0.069 Uiso 1 1 calc R . . C73 C 1.0044(3) 0.40669(16) 0.75236(13) 0.0455(9) Uani 1 1 d . . . H73 H 1.0091 0.4001 0.7842 0.055 Uiso 1 1 calc R . . C74 C 0.9159(3) 0.39400(16) 0.72930(12) 0.0437(9) Uani 1 1 d . . . H74 H 0.8583 0.3784 0.7450 0.052 Uiso 1 1 calc R . . C75 C 0.9089(2) 0.40381(16) 0.68219(12) 0.0414(8) Uani 1 1 d . . . C76 C 0.9961(3) 0.42555(17) 0.66135(12) 0.0444(9) Uani 1 1 d . . . H76 H 0.9931 0.4320 0.6294 0.053 Uiso 1 1 calc R . . C77 C 0.8155(2) 0.39046(15) 0.65757(12) 0.0395(8) Uani 1 1 d . . . C1 C 1.3028(3) 0.4511(2) 0.35980(13) 0.0558(11) Uani 1 1 d . . . O1 O 1.22405(18) 0.43538(13) 0.38472(9) 0.0586(8) Uani 1 1 d . . . H1 H 1.1703 0.4329 0.3684 0.070 Uiso 1 1 calc R . . O2 O 1.2934(2) 0.4640(3) 0.32007(11) 0.127(2) Uani 1 1 d . . . C2 C 1.4031(2) 0.45652(16) 0.38437(12) 0.0418(8) Uani 1 1 d . . . H2A H 1.4185 0.4216 0.3999 0.050 Uiso 1 1 calc R . . H2B H 1.3952 0.4847 0.4082 0.050 Uiso 1 1 calc R . . C3 C 1.4952(3) 0.4713(2) 0.35479(13) 0.0537(11) Uani 1 1 d . . . H3A H 1.5214 0.4377 0.3401 0.064 Uiso 1 1 calc R . . H3B H 1.4704 0.4958 0.3303 0.064 Uiso 1 1 calc R . . C4 C 1.5840(3) 0.49810(17) 0.37860(12) 0.0435(9) Uani 1 1 d . . . H4A H 1.6092 0.4737 0.4031 0.052 Uiso 1 1 calc R . . H4B H 1.5582 0.5319 0.3932 0.052 Uiso 1 1 calc R . . C5 C 1.6741(2) 0.51216(16) 0.34846(12) 0.0422(9) Uani 1 1 d . . . O5 O 1.75507(18) 0.53245(12) 0.36952(8) 0.0524(7) Uani 1 1 d . . . H5 H 1.8045 0.5364 0.3509 0.063 Uiso 1 1 calc R . . O6 O 1.67076(19) 0.50441(15) 0.30777(9) 0.0638(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C11 0.0177(14) 0.089(3) 0.043(2) 0.029(2) 0.0043(14) 0.0016(17) C12 0.0196(14) 0.064(2) 0.044(2) 0.0226(18) -0.0010(13) -0.0033(15) O12 0.0205(10) 0.0683(17) 0.0564(16) 0.0297(13) -0.0027(10) -0.0073(11) C13 0.0166(13) 0.061(2) 0.0357(17) 0.0196(16) -0.0005(12) 0.0025(14) C14 0.0150(13) 0.067(2) 0.0301(16) 0.0164(16) 0.0007(12) -0.0003(14) C15 0.0183(14) 0.084(3) 0.0277(16) 0.0133(17) -0.0009(12) 0.0012(16) C16 0.0217(15) 0.096(3) 0.0298(17) 0.0181(19) 0.0059(13) 0.0053(18) O16 0.0316(13) 0.130(3) 0.0277(13) 0.0132(15) 0.0117(10) 0.0015(15) C17 0.0241(16) 0.093(3) 0.051(2) 0.033(2) 0.0077(15) -0.0003(18) C21 0.0186(13) 0.0451(18) 0.0359(17) -0.0035(14) -0.0048(12) -0.0017(13) C22 0.0186(13) 0.0471(18) 0.0245(15) -0.0030(13) -0.0009(11) -0.0002(12) O22 0.0241(10) 0.0512(14) 0.0253(11) -0.0016(10) -0.0056(8) -0.0001(10) C23 0.0177(12) 0.0440(17) 0.0227(14) -0.0069(13) 0.0017(11) -0.0004(12) C24 0.0142(12) 0.0428(17) 0.0293(15) -0.0016(13) 0.0010(11) -0.0003(12) C25 0.0187(13) 0.0468(19) 0.0317(16) 0.0032(14) -0.0012(12) 0.0000(13) C26 0.0186(13) 0.0421(18) 0.0424(18) 0.0041(15) 0.0000(13) -0.0045(12) O26 0.0223(10) 0.0489(14) 0.0576(16) 0.0139(12) -0.0050(10) -0.0094(10) C27 0.0250(15) 0.0468(19) 0.0371(18) 0.0003(15) -0.0035(13) -0.0041(14) C31 0.0175(13) 0.0460(18) 0.0406(18) 0.0124(15) -0.0038(12) -0.0020(13) C32 0.0191(13) 0.0469(19) 0.0404(18) 0.0078(15) -0.0028(13) 0.0009(13) C33 0.0230(15) 0.057(2) 0.057(2) 0.0195(18) -0.0030(15) -0.0005(15) C34A 0.0283(19) 0.062(6) 0.043(5) 0.007(3) 0.001(3) 0.016(3) C35A 0.020(3) 0.069(5) 0.099(7) 0.025(5) -0.004(3) -0.002(3) C36A 0.020(3) 0.132(9) 0.086(7) 0.043(7) 0.000(4) 0.008(4) C34B 0.0283(19) 0.062(6) 0.043(5) 0.007(3) 0.001(3) 0.016(3) C35B 0.029(4) 0.101(8) 0.041(5) 0.017(5) -0.005(3) 0.015(4) C36B 0.021(4) 0.170(14) 0.041(6) 0.033(7) 0.003(4) 0.018(6) C37 0.0178(14) 0.062(2) 0.058(2) 0.0229(19) -0.0013(14) -0.0080(15) C41 0.0180(18) 0.047(3) 0.0204(19) 0.000 0.0003(15) 0.000 C42 0.0201(19) 0.051(3) 0.022(2) 0.000 0.0008(16) 0.000 C43 0.028(3) 0.046(4) 0.028(3) -0.007(3) 0.006(2) -0.006(3) C44 0.029(3) 0.050(4) 0.054(4) -0.009(3) 0.018(3) 0.003(3) C45 0.031(3) 0.088(4) 0.045(3) 0.000 0.010(2) 0.000 C46 0.029(3) 0.071(4) 0.076(4) 0.000 0.009(3) 0.000 C47 0.0216(19) 0.059(3) 0.023(2) 0.000 -0.0036(17) 0.000 C51 0.021(2) 0.098(4) 0.021(2) 0.000 0.0024(17) 0.000 C52 0.022(2) 0.103(5) 0.032(3) 0.000 -0.0030(19) 0.000 C53 0.034(4) 0.085(6) 0.050(5) 0.004(4) -0.010(3) 0.003(4) C57 0.025(2) 0.134(6) 0.040(3) 0.000 0.011(2) 0.000 N61 0.0238(14) 0.118(3) 0.0387(17) 0.0239(19) 0.0041(13) -0.0128(17) C62 0.0280(17) 0.092(3) 0.041(2) 0.015(2) 0.0072(15) -0.0117(19) N62 0.0311(16) 0.145(4) 0.0377(18) 0.025(2) 0.0045(13) -0.022(2) C63 0.0339(18) 0.099(3) 0.0354(19) 0.013(2) 0.0013(15) -0.006(2) C64 0.0282(17) 0.084(3) 0.048(2) 0.010(2) 0.0039(16) -0.0077(18) C65 0.0245(16) 0.082(3) 0.048(2) 0.025(2) 0.0089(15) -0.0006(17) C66 0.0257(17) 0.121(4) 0.047(2) 0.034(2) 0.0060(16) -0.006(2) C67 0.0238(16) 0.096(3) 0.053(2) 0.029(2) 0.0068(16) 0.0012(18) N71 0.0268(14) 0.082(2) 0.0378(16) 0.0040(16) -0.0050(12) -0.0205(15) C72 0.0251(15) 0.069(2) 0.0378(19) -0.0013(17) -0.0058(14) -0.0078(16) N72 0.0291(14) 0.108(3) 0.0343(16) 0.0059(18) -0.0078(12) -0.0225(17) C73 0.0307(17) 0.071(2) 0.0352(18) 0.0060(18) -0.0034(14) -0.0053(17) C74 0.0243(15) 0.067(2) 0.0398(19) 0.0045(17) 0.0005(14) -0.0095(16) C75 0.0222(14) 0.061(2) 0.0414(19) 0.0012(17) -0.0062(14) -0.0095(15) C76 0.0283(16) 0.071(2) 0.0340(18) 0.0015(17) -0.0056(14) -0.0163(16) C77 0.0271(15) 0.053(2) 0.0389(18) 0.0028(16) 0.0013(14) -0.0075(15) C1 0.0270(17) 0.102(3) 0.038(2) 0.016(2) 0.0037(15) -0.0118(19) O1 0.0247(12) 0.111(2) 0.0403(14) 0.0215(15) 0.0004(10) -0.0155(14) O2 0.0345(16) 0.295(6) 0.0506(19) 0.045(3) -0.0028(14) -0.050(3) C2 0.0284(16) 0.061(2) 0.0360(18) 0.0039(17) -0.0004(14) -0.0094(15) C3 0.0278(17) 0.094(3) 0.039(2) 0.004(2) 0.0003(15) -0.0171(19) C4 0.0309(16) 0.065(2) 0.0349(18) 0.0099(17) -0.0025(14) -0.0120(16) C5 0.0256(15) 0.066(2) 0.0355(19) -0.0031(17) -0.0047(14) -0.0080(15) O5 0.0281(12) 0.094(2) 0.0355(13) -0.0033(13) -0.0024(10) -0.0215(13) O6 0.0312(13) 0.127(3) 0.0334(14) -0.0082(15) 0.0017(11) -0.0297(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C81 C82 1.390(9) . ? C81 C86 1.47(2) . ? C81 C87 1.479(8) . ? C82 C83 1.386(8) . ? C82 H82A 0.9500 . ? C83 C84 1.398(8) . ? C83 H83A 0.9500 . ? C84 C85 1.373(8) . ? C84 C88 1.507(8) . ? C85 C86 1.383(8) . ? C85 H85A 0.9500 . ? C86 H86A 0.9500 . ? C87 H87A 0.9800 . ? C87 H87B 0.9800 . ? C87 H87C 0.9800 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C91 C92 1.386(7) . ? C91 C96 1.403(16) . ? C91 C97 1.506(8) . ? C92 C93 1.386(8) . ? C92 H92 0.9500 . ? C93 C94 1.391(8) . ? C93 H93 0.9500 . ? C94 C95 1.380(8) . ? C94 C98 1.501(8) . ? C95 C96 1.398(8) . ? C95 H95 0.9500 . ? C96 H96 0.9500 . ? C97 H97A 0.9800 . ? C97 H97B 0.9800 . ? C97 H97C 0.9800 . ? C98 H98A 0.9800 . ? C98 H98B 0.9800 . ? C98 H98C 0.9800 . ? N1S C1S 1.353(12) . ? C1S C2S 1.439(14) . ? C2S H2C 1.008(17) . ? C2S H2D 1.013(16) . ? C2S H2E 1.013(16) . ? N2S C3S 1.232(10) . ? C3S C4S 1.517(12) . ? C4S H4C 0.979(16) . ? C4S H4D 1.000(16) . ? C4S H4E 1.000(16) . ? C11 C12 1.395(5) . ? C11 C16 1.396(6) . ? C11 C17 1.442(4) . ? C12 O12 1.379(5) . ? C12 C13 1.404(4) . ? O12 C37 1.420(4) . ? C13 C14 1.392(5) . ? C13 C31 1.513(5) . ? C14 C15 1.388(5) . ? C14 H14 0.9500 . ? C15 C16 1.402(5) . ? C15 C51 1.507(5) . ? C16 O16 1.380(4) . ? O16 C57 1.419(4) . ? C17 C67 1.185(5) . ? C21 C22 1.386(5) . ? C21 C26 1.404(4) . ? C21 C27 1.438(4) . ? C22 O22 1.386(4) . ? C22 C23 1.407(4) . ? O22 C47 1.410(3) . ? C23 C24 1.384(4) . ? C23 C41 1.518(4) . ? C24 C25 1.395(4) . ? C24 H24 0.9500 . ? C25 C26 1.394(4) . ? C25 C31 1.523(4) . ? C26 O26 1.384(4) . ? O26 C37 1.411(4) . ? C27 C77 1.186(4) . ? C31 C32 1.541(4) . ? C31 H31 1.0000 . ? C32 C33 1.516(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34A 1.527(8) . ? C33 C34B 1.532(10) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34A C35A 1.516(10) . ? C34A H34A 0.9900 . ? C34A H34B 0.9900 . ? C35A C36A 1.524(9) . ? C35A H35A 0.9900 . ? C35A H35B 0.9900 . ? C36A H36A 0.9800 . ? C36A H36B 0.9800 . ? C36A H36C 0.9800 . ? C34B C35B 1.513(11) . ? C34B H34C 0.9900 . ? C34B H34D 0.9900 . ? C35B C36B 1.519(10) . ? C35B H35C 0.9900 . ? C35B H35D 0.9900 . ? C36B H36D 0.9800 . ? C36B H36E 0.9800 . ? C36B H36F 0.9800 . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C41 C23 1.518(4) 7_565 ? C41 C42 1.533(5) . ? C41 H41 1.0000 . ? C42 C43 1.460(7) . ? C42 C43 1.460(7) 7_565 ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.531(9) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.361(8) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C44 1.361(8) 7_565 ? C45 C46 1.508(7) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 O22 1.410(3) 7_565 ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C51 C15 1.507(5) 7_565 ? C51 C52 1.542(6) . ? C51 H51 1.0000 . ? C52 C53 1.382(9) . ? C52 C53 1.382(9) 7_565 ? C52 H52A 0.9900 . ? C52 H52B 0.9900 . ? C53 C54A 1.509(9) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54A C55A 1.452(14) . ? C54A H54A 0.9900 . ? C54A H54B 0.9900 . ? C55A C56A 1.549(13) . ? C55A H55A 0.9900 . ? C55A H55B 0.9900 . ? C56A H56A 0.9800 . ? C56A H56B 0.9800 . ? C56A H56C 0.9800 . ? C55B C56B 1.562(15) . ? C55B H55C 0.9900 . ? C55B H55D 0.9900 . ? C56B H56D 0.9800 . ? C56B H56E 0.9800 . ? C56B H56F 0.9800 . ? C57 O16 1.419(4) 7_565 ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? N61 C66 1.338(5) . ? N61 C62 1.343(5) . ? C62 N62 1.335(4) . ? C62 C63 1.401(5) . ? N62 H62A 0.8800 . ? N62 H62B 0.8800 . ? C63 C64 1.361(5) . ? C63 H63 0.9500 . ? C64 C65 1.393(5) . ? C64 H64 0.9500 . ? C65 C66 1.370(5) . ? C65 C67 1.432(5) . ? C66 H66 0.9500 . ? C67 O16 5.245(6) 7_565 ? N71 C76 1.342(4) . ? N71 C72 1.351(5) . ? C72 N72 1.347(4) . ? C72 C73 1.402(5) . ? N72 H72A 0.8800 . ? N72 H72B 0.8800 . ? C73 C74 1.353(5) . ? C73 H73 0.9500 . ? C74 C75 1.405(5) . ? C74 H74 0.9500 . ? C75 C76 1.378(5) . ? C75 C77 1.433(4) . ? C76 H76 0.9500 . ? C1 O2 1.213(5) . ? C1 O1 1.303(4) . ? C1 C2 1.476(5) . ? O1 H1 0.8400 . ? C2 C3 1.505(5) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 C4 1.487(5) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.492(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 O6 1.209(4) . ? C5 O5 1.304(4) . ? O5 H5 0.8400 . ? 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 C82 C81 C86 121.7(8) . . ? C82 C81 C87 121.5(10) . . ? C86 C81 C87 116.8(10) . . ? C83 C82 C81 119.8(8) . . ? C83 C82 H82A 120.1 . . ? C81 C82 H82A 120.1 . . ? C82 C83 C84 119.4(7) . . ? C82 C83 H83A 120.3 . . ? C84 C83 H83A 120.3 . . ? C85 C84 C83 120.7(7) . . ? C85 C84 C88 120.7(8) . . ? C83 C84 C88 118.6(8) . . ? C84 C85 C86 123.6(9) . . ? C84 C85 H85A 118.2 . . ? C86 C85 H85A 118.2 . . ? C85 C86 C81 114.7(12) . . ? C85 C86 H86A 122.6 . . ? C81 C86 H86A 122.6 . . ? C81 C87 H87A 109.5 . . ? C81 C87 H87B 109.5 . . ? H87A C87 H87B 109.5 . . ? C81 C87 H87C 109.5 . . ? H87A C87 H87C 109.5 . . ? H87B C87 H87C 109.5 . . ? C84 C88 H88A 109.5 . . ? C84 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C84 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C92 C91 C96 120.2(8) . . ? C92 C91 C97 120.6(8) . . ? C96 C91 C97 119.2(9) . . ? H2C C91 H4C 88(5) . . ? H2C C91 H4D 76.2(18) . . ? H4C C91 H4D 150(3) . . ? H2C C91 H4E 73.7(17) . . ? H4C C91 H4E 126(2) . . ? H4D C91 H4E 74.1(17) . . ? C91 C92 C93 120.1(7) . . ? C91 C92 H92 119.9 . . ? C93 C92 H92 119.9 . . ? C92 C93 C94 119.9(6) . . ? C92 C93 H93 120.1 . . ? C94 C93 H93 120.1 . . ? C95 C94 C93 120.6(6) . . ? C95 C94 C98 119.8(8) . . ? C93 C94 C98 119.6(8) . . ? C94 C95 C96 120.0(8) . . ? C94 C95 H95 120.0 . . ? C96 C95 H95 120.0 . . ? H2C C95 H2D 112(3) . . ? C95 C96 C91 119.2(11) . . ? C95 C96 H96 120.4 . . ? C91 C96 H96 120.4 . . ? H2C C96 H4D 134(2) . . ? C91 C97 H97A 109.5 . . ? C91 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? C91 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? C94 C98 H98A 109.5 . . ? C94 C98 H98B 109.5 . . ? H98A C98 H98B 109.5 . . ? C94 C98 H98C 109.5 . . ? H98A C98 H98C 109.5 . . ? H98B C98 H98C 109.5 . . ? N1S C1S C2S 173.9(16) . . ? C1S C2S H2C 111.2(19) . . ? C1S C2S H2D 110.2(18) . . ? H2C C2S H2D 108(2) . . ? C1S C2S H2E 110.2(18) . . ? H2C C2S H2E 108(2) . . ? H2D C2S H2E 108(2) . . ? N2S C3S C4S 177.7(11) . . ? C3S C4S H4C 108.3(18) . . ? C3S C4S H4D 105.5(17) . . ? H4C C4S H4D 113(2) . . ? C3S C4S H4E 105.5(17) . . ? H4C C4S H4E 113(2) . . ? H4D C4S H4E 111(2) . . ? C12 C11 C16 119.1(3) . . ? C12 C11 C17 122.4(4) . . ? C16 C11 C17 118.6(4) . . ? O12 C12 C11 118.0(3) . . ? O12 C12 C13 120.7(3) . . ? C11 C12 C13 121.1(4) . . ? C12 O12 C37 116.9(3) . . ? C14 C13 C12 117.4(3) . . ? C14 C13 C31 122.7(3) . . ? C12 C13 C31 119.8(3) . . ? C15 C14 C13 123.6(3) . . ? C15 C14 H14 118.2 . . ? C13 C14 H14 118.2 . . ? C14 C15 C16 117.1(4) . . ? C14 C15 C51 123.3(3) . . ? C16 C15 C51 119.4(4) . . ? O16 C16 C11 117.6(3) . . ? O16 C16 C15 120.7(4) . . ? C11 C16 C15 121.6(3) . . ? C16 O16 C57 115.9(3) . . ? C67 C17 C11 174.6(5) . . ? C22 C21 C26 118.8(3) . . ? C22 C21 C27 119.3(3) . . ? C26 C21 C27 121.8(3) . . ? C21 C22 O22 118.4(3) . . ? C21 C22 C23 121.4(3) . . ? O22 C22 C23 120.1(3) . . ? C22 O22 C47 116.2(3) . . ? C24 C23 C22 117.8(3) . . ? C24 C23 C41 122.6(3) . . ? C22 C23 C41 119.4(3) . . ? C23 C24 C25 122.9(3) . . ? C23 C24 H24 118.6 . . ? C25 C24 H24 118.6 . . ? C26 C25 C24 117.8(3) . . ? C26 C25 C31 120.4(3) . . ? C24 C25 C31 121.8(3) . . ? O26 C26 C25 121.1(3) . . ? O26 C26 C21 117.4(3) . . ? C25 C26 C21 121.3(3) . . ? C26 O26 C37 117.2(3) . . ? C77 C27 C21 174.5(4) . . ? C13 C31 C25 109.6(3) . . ? C13 C31 C32 113.7(3) . . ? C25 C31 C32 112.3(3) . . ? C13 C31 H31 106.9 . . ? C25 C31 H31 106.9 . . ? C32 C31 H31 106.9 . . ? C33 C32 C31 112.2(3) . . ? C33 C32 H32A 109.2 . . ? C31 C32 H32A 109.2 . . ? C33 C32 H32B 109.2 . . ? C31 C32 H32B 109.2 . . ? H32A C32 H32B 107.9 . . ? C32 C33 C34A 114.6(4) . . ? C32 C33 C34B 112.6(5) . . ? C32 C33 H33A 108.6 . . ? C34A C33 H33A 108.6 . . ? C34B C33 H33A 87.9 . . ? C32 C33 H33B 108.6 . . ? C34A C33 H33B 108.6 . . ? C34B C33 H33B 128.0 . . ? H33A C33 H33B 107.6 . . ? C35A C34A C33 111.0(6) . . ? C35A C34A H34A 109.4 . . ? C33 C34A H34A 109.4 . . ? C35A C34A H34B 109.4 . . ? C33 C34A H34B 109.4 . . ? H34A C34A H34B 108.0 . . ? C34A C35A C36A 114.4(7) . . ? C34A C35A H35A 108.7 . . ? C36A C35A H35A 108.7 . . ? C34A C35A H35B 108.7 . . ? C36A C35A H35B 108.7 . . ? H35A C35A H35B 107.6 . . ? C35A C36A H36A 109.5 . . ? C35A C36A H36B 109.5 . . ? H36A C36A H36B 109.5 . . ? C35A C36A H36C 109.5 . . ? H36A C36A H36C 109.5 . . ? H36B C36A H36C 109.5 . . ? C35B C34B C33 115.4(8) . . ? C35B C34B H34C 108.4 . . ? C33 C34B H34C 108.4 . . ? C35B C34B H34D 108.4 . . ? C33 C34B H34D 108.4 . . ? H34C C34B H34D 107.5 . . ? C34B C35B C36B 113.1(8) . . ? C34B C35B H35C 109.0 . . ? C36B C35B H35C 109.0 . . ? C34B C35B H35D 109.0 . . ? C36B C35B H35D 109.0 . . ? H35C C35B H35D 107.8 . . ? C35B C36B H36D 109.5 . . ? C35B C36B H36E 109.5 . . ? H36D C36B H36E 109.5 . . ? C35B C36B H36F 109.5 . . ? H36D C36B H36F 109.5 . . ? H36E C36B H36F 109.5 . . ? O26 C37 O12 112.5(3) . . ? O26 C37 H37A 109.1 . . ? O12 C37 H37A 109.1 . . ? O26 C37 H37B 109.1 . . ? O12 C37 H37B 109.1 . . ? H37A C37 H37B 107.8 . . ? C23 C41 C23 106.1(3) 7_565 . ? C23 C41 C42 114.0(2) 7_565 . ? C23 C41 C42 114.0(2) . . ? C23 C41 H41 107.5 7_565 . ? C23 C41 H41 107.5 . . ? C42 C41 H41 107.5 . . ? C43 C42 C43 85.7(6) . 7_565 ? C43 C42 C41 114.4(3) . . ? C43 C42 C41 114.4(3) 7_565 . ? C43 C42 H42A 108.6 . . ? C43 C42 H42A 123.0 7_565 . ? C41 C42 H42A 108.6 . . ? C43 C42 H42B 108.6 . . ? C41 C42 H42B 108.6 . . ? H42A C42 H42B 107.6 . . ? C42 C43 C44 114.6(5) . . ? C42 C43 H43A 108.6 . . ? C44 C43 H43A 108.6 . . ? C42 C43 H43B 108.6 . . ? C44 C43 H43B 108.6 . . ? H43A C43 H43B 107.6 . . ? C45 C44 C43 120.2(6) . . ? C45 C44 H44A 107.3 . . ? C43 C44 H44A 107.3 . . ? C45 C44 H44B 107.3 . . ? C43 C44 H44B 107.3 . . ? H44A C44 H44B 106.9 . . ? C44 C45 C44 106.7(7) 7_565 . ? C44 C45 C46 124.9(4) 7_565 . ? C44 C45 C46 124.9(4) . . ? C44 C45 H45A 73.4 7_565 . ? C44 C45 H45A 106.1 . . ? C46 C45 H45A 106.1 . . ? C44 C45 H45B 106.1 . . ? C46 C45 H45B 106.1 . . ? H45A C45 H45B 106.3 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O22 C47 O22 112.6(3) 7_565 . ? O22 C47 H47A 109.1 7_565 . ? O22 C47 H47A 109.1 . . ? O22 C47 H47B 109.1 7_565 . ? O22 C47 H47B 109.1 . . ? H47A C47 H47B 107.8 . . ? C15 C51 C15 106.2(4) . 7_565 ? C15 C51 C52 114.2(2) . . ? C15 C51 C52 114.2(2) 7_565 . ? C15 C51 H51 107.3 . . ? C15 C51 H51 107.3 7_565 . ? C52 C51 H51 107.3 . . ? C53 C52 C51 116.3(4) . . ? C53 C52 C51 116.3(4) 7_565 . ? C53 C52 H52A 107.9 . . ? C51 C52 H52A 108.3 . . ? C53 C52 H52B 108.3 . . ? C53 C52 H52B 121.9 7_565 . ? C51 C52 H52B 108.3 . . ? H52A C52 H52B 107.4 . . ? C52 C53 C54A 119.0(8) . . ? C52 C53 H53A 107.6 . . ? C54A C53 H53A 107.6 . . ? C52 C53 H53B 107.6 . . ? C54A C53 H53B 107.6 . . ? H53A C53 H53B 107.0 . . ? C55A C54A C53 116.7(10) . . ? C55A C54A H54A 108.1 . . ? C53 C54A H54A 108.1 . . ? C55A C54A H54B 108.1 . . ? C53 C54A H54B 108.1 . . ? H54A C54A H54B 107.3 . . ? C54A C55A C56A 115.0(15) . . ? C54A C55A H55A 108.5 . . ? C56A C55A H55A 108.5 . . ? C54A C55A H55B 108.5 . . ? C56A C55A H55B 108.5 . . ? H55A C55A H55B 107.5 . . ? C55A C56A H56A 109.5 . . ? C55A C56A H56B 109.5 . . ? H56A C56A H56B 109.5 . . ? C55A C56A H56C 109.5 . . ? H56A C56A H56C 109.5 . . ? H56B C56A H56C 109.5 . . ? C56B C55B H55C 108.2 . . ? C56B C55B H55D 108.2 . . ? H55C C55B H55D 107.3 . . ? C55B C56B H56D 109.5 . . ? C55B C56B H56E 109.5 . . ? H56D C56B H56E 109.5 . . ? C55B C56B H56F 109.5 . . ? H56D C56B H56F 109.5 . . ? H56E C56B H56F 109.5 . . ? O16 C57 O16 112.2(4) 7_565 . ? O16 C57 H57A 109.2 7_565 . ? O16 C57 H57A 109.2 . . ? O16 C57 H57B 109.2 7_565 . ? O16 C57 H57B 109.2 . . ? H57A C57 H57B 107.9 . . ? C66 N61 C62 118.5(3) . . ? N62 C62 N61 116.8(3) . . ? N62 C62 C63 122.3(4) . . ? N61 C62 C63 120.9(3) . . ? C62 N62 H62A 120.0 . . ? C62 N62 H62B 120.0 . . ? H62A N62 H62B 120.0 . . ? C64 C63 C62 119.0(4) . . ? C64 C63 H63 120.5 . . ? C62 C63 H63 120.5 . . ? C63 C64 C65 120.7(4) . . ? C63 C64 H64 119.6 . . ? C65 C64 H64 119.6 . . ? C66 C65 C64 116.4(3) . . ? C66 C65 C67 123.2(4) . . ? C64 C65 C67 120.4(3) . . ? N61 C66 C65 124.5(4) . . ? N61 C66 H66 117.8 . . ? C65 C66 H66 117.8 . . ? C17 C67 C65 173.9(4) . . ? C17 C67 O16 56.4(3) . 7_565 ? C65 C67 O16 121.6(3) . 7_565 ? C76 N71 C72 118.0(3) . . ? N72 C72 N71 117.2(3) . . ? N72 C72 C73 121.4(3) . . ? N71 C72 C73 121.3(3) . . ? C72 N72 H72A 120.0 . . ? C72 N72 H72B 120.0 . . ? H72A N72 H72B 120.0 . . ? C74 C73 C72 119.4(3) . . ? C74 C73 H73 120.3 . . ? C72 C73 H73 120.3 . . ? C73 C74 C75 120.3(3) . . ? C73 C74 H74 119.8 . . ? C75 C74 H74 119.8 . . ? C76 C75 C74 116.8(3) . . ? C76 C75 C77 122.6(3) . . ? C74 C75 C77 120.6(3) . . ? N71 C76 C75 124.1(3) . . ? N71 C76 H76 117.9 . . ? C75 C76 H76 117.9 . . ? C27 C77 C75 173.6(4) . . ? O2 C1 O1 122.6(3) . . ? O2 C1 C2 122.1(3) . . ? O1 C1 C2 115.1(3) . . ? C1 O1 H1 109.5 . . ? C1 C2 C3 114.8(3) . . ? C1 C2 H2A 108.6 . . ? C3 C2 H2A 108.6 . . ? C1 C2 H2B 108.6 . . ? C3 C2 H2B 108.6 . . ? H2A C2 H2B 107.6 . . ? C4 C3 C2 115.6(3) . . ? C4 C3 H3A 108.4 . . ? C2 C3 H3A 108.4 . . ? C4 C3 H3B 108.4 . . ? C2 C3 H3B 108.4 . . ? H3A C3 H3B 107.4 . . ? C3 C4 C5 114.4(3) . . ? C3 C4 H4A 108.7 . . ? C5 C4 H4A 108.7 . . ? C3 C4 H4B 108.7 . . ? C5 C4 H4B 108.7 . . ? H4A C4 H4B 107.6 . . ? O6 C5 O5 123.7(3) . . ? O6 C5 C4 121.4(3) . . ? O5 C5 C4 114.8(3) . . ? C5 O5 H5 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 C86 C81 C82 C83 0.02(14) . . . . ? C87 C81 C82 C83 179.99(14) . . . . ? C81 C82 C83 C84 0.01(14) . . . . ? C82 C83 C84 C85 0.0(3) . . . . ? C82 C83 C84 C88 -179.96(19) . . . . ? C83 C84 C85 C86 -0.1(5) . . . . ? C88 C84 C85 C86 179.9(3) . . . . ? C84 C85 C86 C81 0.1(4) . . . . ? C82 C81 C86 C85 -0.1(3) . . . . ? C87 C81 C86 C85 180.0(2) . . . . ? C96 C91 C92 C93 0.00(15) . . . . ? C97 C91 C92 C93 179.99(14) . . . . ? C91 C92 C93 C94 -0.01(15) . . . . ? C92 C93 C94 C95 0.0(3) . . . . ? C92 C93 C94 C98 180.00(19) . . . . ? C93 C94 C95 C96 -0.1(4) . . . . ? C98 C94 C95 C96 180.0(3) . . . . ? C94 C95 C96 C91 0.1(4) . . . . ? C92 C91 C96 C95 0.0(3) . . . . ? C97 C91 C96 C95 180.0(2) . . . . ? C16 C11 C12 O12 -176.1(3) . . . . ? C17 C11 C12 O12 3.5(5) . . . . ? C16 C11 C12 C13 -1.0(5) . . . . ? C17 C11 C12 C13 178.7(3) . . . . ? C11 C12 O12 C37 -103.2(4) . . . . ? C13 C12 O12 C37 81.6(4) . . . . ? O12 C12 C13 C14 177.7(3) . . . . ? C11 C12 C13 C14 2.7(5) . . . . ? O12 C12 C13 C31 -4.9(5) . . . . ? C11 C12 C13 C31 -179.9(3) . . . . ? C12 C13 C14 C15 -2.6(5) . . . . ? C31 C13 C14 C15 -179.9(3) . . . . ? C13 C14 C15 C16 0.7(5) . . . . ? C13 C14 C15 C51 174.6(3) . . . . ? C12 C11 C16 O16 175.1(3) . . . . ? C17 C11 C16 O16 -4.6(5) . . . . ? C12 C11 C16 C15 -1.0(6) . . . . ? C17 C11 C16 C15 179.4(3) . . . . ? C14 C15 C16 O16 -174.8(3) . . . . ? C51 C15 C16 O16 11.0(5) . . . . ? C14 C15 C16 C11 1.1(5) . . . . ? C51 C15 C16 C11 -173.1(3) . . . . ? C11 C16 O16 C57 96.5(4) . . . . ? C15 C16 O16 C57 -87.4(4) . . . . ? C26 C21 C22 O22 -177.2(3) . . . . ? C27 C21 C22 O22 2.6(4) . . . . ? C26 C21 C22 C23 -0.3(5) . . . . ? C27 C21 C22 C23 179.4(3) . . . . ? C21 C22 O22 C47 -96.6(3) . . . . ? C23 C22 O22 C47 86.4(3) . . . . ? C21 C22 C23 C24 -0.9(4) . . . . ? O22 C22 C23 C24 176.0(3) . . . . ? C21 C22 C23 C41 173.6(3) . . . . ? O22 C22 C23 C41 -9.6(4) . . . . ? C22 C23 C24 C25 -0.1(4) . . . . ? C41 C23 C24 C25 -174.4(3) . . . . ? C23 C24 C25 C26 2.3(5) . . . . ? C23 C24 C25 C31 -178.6(3) . . . . ? C24 C25 C26 O26 -177.8(3) . . . . ? C31 C25 C26 O26 3.1(5) . . . . ? C24 C25 C26 C21 -3.6(5) . . . . ? C31 C25 C26 C21 177.4(3) . . . . ? C22 C21 C26 O26 177.1(3) . . . . ? C27 C21 C26 O26 -2.7(5) . . . . ? C22 C21 C26 C25 2.6(5) . . . . ? C27 C21 C26 C25 -177.2(3) . . . . ? C25 C26 O26 C37 -79.6(4) . . . . ? C21 C26 O26 C37 105.9(3) . . . . ? C14 C13 C31 C25 93.7(3) . . . . ? C12 C13 C31 C25 -83.6(4) . . . . ? C14 C13 C31 C32 -33.0(4) . . . . ? C12 C13 C31 C32 149.7(3) . . . . ? C26 C25 C31 C13 84.9(4) . . . . ? C24 C25 C31 C13 -94.1(3) . . . . ? C26 C25 C31 C32 -147.6(3) . . . . ? C24 C25 C31 C32 33.4(4) . . . . ? C13 C31 C32 C33 -67.7(4) . . . . ? C25 C31 C32 C33 167.0(3) . . . . ? C31 C32 C33 C34A -171.5(4) . . . . ? C31 C32 C33 C34B 162.5(5) . . . . ? C32 C33 C34A C35A -66.0(8) . . . . ? C34B C33 C34A C35A 24.6(14) . . . . ? C33 C34A C35A C36A -175.9(7) . . . . ? C32 C33 C34B C35B 59.8(10) . . . . ? C34A C33 C34B C35B -40.2(13) . . . . ? C33 C34B C35B C36B 175.7(10) . . . . ? C26 O26 C37 O12 93.4(3) . . . . ? C12 O12 C37 O26 -94.3(4) . . . . ? C24 C23 C41 C23 90.6(4) . . . 7_565 ? C22 C23 C41 C23 -83.6(4) . . . 7_565 ? C24 C23 C41 C42 -35.7(4) . . . . ? C22 C23 C41 C42 150.1(3) . . . . ? C23 C41 C42 C43 167.3(4) 7_565 . . . ? C23 C41 C42 C43 -70.7(5) . . . . ? C23 C41 C42 C43 70.7(5) 7_565 . . 7_565 ? C23 C41 C42 C43 -167.3(4) . . . 7_565 ? C43 C42 C43 C44 -70.8(7) 7_565 . . . ? C41 C42 C43 C44 174.2(5) . . . . ? C42 C43 C44 C45 58.5(9) . . . . ? C43 C44 C45 C44 -24.9(11) . . . 7_565 ? C43 C44 C45 C46 175.8(6) . . . . ? C22 O22 C47 O22 -90.1(4) . . . 7_565 ? C14 C15 C51 C15 -90.7(4) . . . 7_565 ? C16 C15 C51 C15 83.0(4) . . . 7_565 ? C14 C15 C51 C52 36.0(5) . . . . ? C16 C15 C51 C52 -150.2(4) . . . . ? C15 C51 C52 C53 70.6(6) . . . . ? C15 C51 C52 C53 -166.9(5) 7_565 . . . ? C15 C51 C52 C53 166.9(5) . . . 7_565 ? C15 C51 C52 C53 -70.6(6) 7_565 . . 7_565 ? C53 C52 C53 C54A 60.5(10) 7_565 . . . ? C51 C52 C53 C54A 176.9(7) . . . . ? C51 C52 C53 C53 116.3(6) . . . 7_565 ? C52 C53 C54A C55A -65.4(14) . . . . ? C53 C53 C54A C55A -25.0(11) 7_565 . . . ? C53 C54A C55A C56A -170.6(12) . . . . ? C16 O16 C57 O16 88.9(5) . . . 7_565 ? C66 N61 C62 N62 179.7(5) . . . . ? C66 N61 C62 C63 -1.3(7) . . . . ? N62 C62 C63 C64 180.0(5) . . . . ? N61 C62 C63 C64 1.0(7) . . . . ? C62 C63 C64 C65 0.4(7) . . . . ? C63 C64 C65 C66 -1.6(7) . . . . ? C63 C64 C65 C67 178.5(5) . . . . ? C62 N61 C66 C65 0.1(8) . . . . ? C64 C65 C66 N61 1.3(8) . . . . ? C67 C65 C66 N61 -178.7(5) . . . . ? C66 C65 C67 O16 -117.0(4) . . . 7_565 ? C64 C65 C67 O16 62.9(5) . . . 7_565 ? C76 N71 C72 N72 -179.5(4) . . . . ? C76 N71 C72 C73 2.0(6) . . . . ? N72 C72 C73 C74 179.9(4) . . . . ? N71 C72 C73 C74 -1.6(6) . . . . ? C72 C73 C74 C75 -0.1(6) . . . . ? C73 C74 C75 C76 1.2(6) . . . . ? C73 C74 C75 C77 180.0(4) . . . . ? C72 N71 C76 C75 -0.7(6) . . . . ? C74 C75 C76 N71 -0.9(6) . . . . ? C77 C75 C76 N71 -179.6(4) . . . . ? O2 C1 C2 C3 -8.6(7) . . . . ? O1 C1 C2 C3 176.3(4) . . . . ? C1 C2 C3 C4 156.5(4) . . . . ? C2 C3 C4 C5 179.9(4) . . . . ? C3 C4 C5 O6 3.5(6) . . . . ? C3 C4 C5 O5 -175.7(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O1 H1 N61 0.84 1.82 2.652(4) 169.0 . O5 H5 N71 0.84 1.84 2.664(4) 165.7 5_866 N62 H62A O2 0.88 1.94 2.815(4) 173.4 . N62 H62B O6 0.88 2.15 2.847(4) 136.1 6_556 N72 H72A O6 0.88 2.01 2.878(4) 168.6 5_866 _diffrn_measured_fraction_theta_max 0.971 _diffrn_reflns_theta_full 28.37 _diffrn_measured_fraction_theta_full 0.971 _refine_diff_density_max 1.222 _refine_diff_density_min -0.659 _refine_diff_density_rms 0.076 #END