# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 182 loop_ _publ_author_name 'John Ripmeester' 'Philip Brown' 'Gary D. Enright' 'Konstantin A. Udachin' _publ_contact_author_name 'John A. Ripmeester' _publ_contact_author_address ; Steacie Institute for Molecular Sciences National Research Council Functional Materials Group 100 Sussex Dr Ottawa ON K1A 0R6 CANADA ; _publ_contact_author_email JOHN.RIPMEESTER@NRC-CNRC.GC.CA _publ_requested_journal 'Chemical Communications' _publ_section_title ; Extending the chemistry of p-t-butylcalix[4]arene with H-bonding and secondary coordination ; data_compound_1(ku79) _database_code_depnum_ccdc_archive 'CCDC 192202' _audit_creation_method SHELXL-97 _chemical_name_systematic ; t-butyl-calix[4]arene*3n-butylamine*2H2O ; _chemical_name_common t-butyl-calix[4]arene*3n-butylamine*2H2O _chemical_melting_point ? _chemical_formula_moiety 'C44H56O4 C4H9NH2' _chemical_formula_sum 'C56 H93 N3 O6' _chemical_formula_weight 904.33 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.9000(10) _cell_length_b 22.2170(17) _cell_length_c 19.4755(15) _cell_angle_alpha 90.00 _cell_angle_beta 94.224(2) _cell_angle_gamma 90.00 _cell_volume 5566.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.079 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1992 _exptl_absorpt_coefficient_mu 0.069 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 65010 _diffrn_reflns_av_R_equivalents 0.0602 _diffrn_reflns_av_sigmaI/netI 0.0656 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 28.76 _reflns_number_total 14320 _reflns_number_gt 6779 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1074P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 14320 _refine_ls_number_parameters 803 _refine_ls_number_restraints 179 _refine_ls_R_factor_all 0.1352 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1829 _refine_ls_wR_factor_gt 0.1462 _refine_ls_goodness_of_fit_ref 0.869 _refine_ls_restrained_S_all 0.901 _refine_ls_shift/su_max 0.601 _refine_ls_shift/su_mean 0.011 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.12643(10) 0.62594(6) 0.43342(6) 0.0418(3) Uani 1 1 d D . . H1 H 0.0683 0.6296 0.4497 0.050 Uiso 0.50 1 calc PRD . . H1X H 0.1100 0.6000 0.4008 0.050 Uiso 0.50 1 d PRD . . O2 O -0.06281(12) 0.60794(7) 0.39917(8) 0.0517(4) Uani 1 1 d D . . H2 H 0.0066(15) 0.6181(13) 0.4145(14) 0.013(7) Uiso 0.50 1 d PD . . H2X H -0.084(3) 0.5704(13) 0.421(2) 0.059(14) Uiso 0.50 1 d PD . . O3 O -0.04313(11) 0.49808(6) 0.31875(7) 0.0495(4) Uani 1 1 d . . . H3 H 0.0135 0.5047 0.3348 0.050 Uiso 0.50 1 d P . . H3X H -0.0550 0.5032 0.3597 0.050 Uiso 0.50 1 d P . . O4 O 0.15068(11) 0.54456(7) 0.34553(8) 0.0446(3) Uani 1 1 d . . . H4 H 0.150(2) 0.5722(14) 0.3744(15) 0.004(7) Uiso 0.50 1 d P . . H4X H 0.0854 0.5254 0.3404 0.050 Uiso 0.50 1 d P . . C1 C 0.15792(14) 0.68011(9) 0.41102(9) 0.0348(4) Uani 1 1 d . . . C2 C 0.09561(14) 0.73126(9) 0.41734(9) 0.0366(4) Uani 1 1 d . . . C3 C 0.13139(15) 0.78651(9) 0.39573(10) 0.0407(5) Uani 1 1 d . . . H3A H 0.0892 0.8211 0.4006 0.049 Uiso 1 1 calc R . . C4 C 0.22668(15) 0.79344(9) 0.36724(10) 0.0404(4) Uani 1 1 d D F . C5 C 0.28566(14) 0.74168(9) 0.36059(10) 0.0372(4) Uani 1 1 d . . . H5 H 0.3507 0.7449 0.3410 0.045 Uiso 1 1 calc R . . C6 C 0.25325(14) 0.68541(9) 0.38150(9) 0.0346(4) Uani 1 1 d . . . C7 C 0.32122(15) 0.63001(9) 0.37479(10) 0.0386(4) Uani 1 1 d . . . H7A H 0.3099 0.6025 0.4135 0.046 Uiso 1 1 calc R . . H7B H 0.3949 0.6428 0.3796 0.046 Uiso 1 1 calc R . . C8 C 0.26546(19) 0.85600(10) 0.34810(13) 0.0586(6) Uani 1 1 d D . . C12 C 0.21853(15) 0.55534(8) 0.29645(10) 0.0372(4) Uani 1 1 d . . . C13 C 0.30296(14) 0.59485(8) 0.30765(10) 0.0355(4) Uani 1 1 d . . . C14 C 0.37281(15) 0.59962(8) 0.25745(10) 0.0376(4) Uani 1 1 d . . . H14 H 0.4299 0.6264 0.2651 0.045 Uiso 1 1 calc R . . C15 C 0.36378(14) 0.56694(8) 0.19585(10) 0.0379(4) Uani 1 1 d D G . C16 C 0.27679(15) 0.52989(9) 0.18606(10) 0.0402(5) Uani 1 1 d . . . H16 H 0.2670 0.5078 0.1443 0.048 Uiso 1 1 calc R . . C17 C 0.20395(15) 0.52369(8) 0.23429(10) 0.0387(4) Uani 1 1 d . . . C18 C 0.10942(16) 0.48340(9) 0.21975(12) 0.0452(5) Uani 1 1 d . . . H18A H 0.1212 0.4573 0.1799 0.054 Uiso 1 1 calc R . . H18B H 0.1020 0.4570 0.2601 0.054 Uiso 1 1 calc R . . C19 C 0.44902(16) 0.56764(10) 0.14534(10) 0.0447(5) Uani 1 1 d D . . C23 C -0.06091(15) 0.52587(8) 0.25568(10) 0.0379(4) Uani 1 1 d . . . C24 C 0.00928(15) 0.51790(8) 0.20471(10) 0.0392(4) Uani 1 1 d . . . C25 C -0.01549(15) 0.54215(8) 0.13989(10) 0.0386(4) Uani 1 1 d . . . H25 H 0.0317 0.5366 0.1052 0.046 Uiso 1 1 calc R . . C26 C -0.10645(15) 0.57426(8) 0.12366(9) 0.0356(4) Uani 1 1 d . . . C27 C -0.17169(14) 0.58306(8) 0.17648(9) 0.0346(4) Uani 1 1 d . . . H27 H -0.2339 0.6053 0.1669 0.041 Uiso 1 1 calc R . . C28 C -0.15014(14) 0.56078(8) 0.24265(10) 0.0358(4) Uani 1 1 d . . . C29 C -0.22001(15) 0.57750(9) 0.29913(10) 0.0398(5) Uani 1 1 d . . . H29A H -0.2936 0.5728 0.2817 0.048 Uiso 1 1 calc R . . H29B H -0.2067 0.5497 0.3385 0.048 Uiso 1 1 calc R . . C30 C -0.13749(16) 0.59750(9) 0.05085(10) 0.0424(5) Uani 1 1 d . . . C31 C -0.0474(2) 0.59630(11) 0.00422(12) 0.0568(6) Uani 1 1 d . . . H31A H 0.0102 0.6205 0.0249 0.085 Uiso 1 1 calc R . . H31B H -0.0705 0.6129 -0.0410 0.085 Uiso 1 1 calc R . . H31C H -0.0241 0.5547 -0.0012 0.085 Uiso 1 1 calc R . . C32 C -0.2247(2) 0.55695(14) 0.01878(13) 0.0763(8) Uani 1 1 d . . . H32A H -0.1989 0.5156 0.0157 0.114 Uiso 1 1 calc R . . H32B H -0.2468 0.5716 -0.0274 0.114 Uiso 1 1 calc R . . H32C H -0.2838 0.5577 0.0476 0.114 Uiso 1 1 calc R . . C33 C -0.17746(19) 0.66228(11) 0.05303(11) 0.0521(6) Uani 1 1 d . . . H33A H -0.2404 0.6635 0.0783 0.078 Uiso 1 1 calc R . . H33B H -0.1936 0.6768 0.0060 0.078 Uiso 1 1 calc R . . H33C H -0.1240 0.6880 0.0762 0.078 Uiso 1 1 calc R . . C34 C -0.11961(15) 0.65461(10) 0.37218(9) 0.0392(5) Uani 1 1 d . . . C35 C -0.20175(14) 0.64153(9) 0.32335(9) 0.0380(4) Uani 1 1 d . . . C36 C -0.26216(14) 0.68886(9) 0.29681(9) 0.0376(4) Uani 1 1 d . . . H36 H -0.3184 0.6801 0.2640 0.045 Uiso 1 1 calc R . . C37 C -0.24445(14) 0.74842(9) 0.31587(10) 0.0393(5) Uani 1 1 d D H . C38 C -0.16093(15) 0.75928(10) 0.36444(10) 0.0406(5) Uani 1 1 d . . . H38 H -0.1463 0.7996 0.3781 0.049 Uiso 1 1 calc R . . C39 C -0.09893(14) 0.71367(10) 0.39328(9) 0.0392(5) Uani 1 1 d . . . C40 C -0.00973(15) 0.72754(10) 0.44675(10) 0.0428(5) Uani 1 1 d . . . H40A H -0.0241 0.7663 0.4692 0.051 Uiso 1 1 calc R . . H40B H -0.0072 0.6959 0.4826 0.051 Uiso 1 1 calc R . . C41 C -0.30910(17) 0.80099(10) 0.28510(11) 0.0492(5) Uani 1 1 d D . . N1A N 0.0221(10) 0.7567(5) 0.2305(6) 0.062(2) Uani 0.50 1 d PD A -1 H1A1 H 0.0776 0.7779 0.2492 0.093 Uiso 0.25 1 calc PR A -1 H1A2 H -0.0279 0.7552 0.2610 0.093 Uiso 0.25 1 calc PR A -1 H1A3 H -0.0038 0.7751 0.1912 0.093 Uiso 0.50 1 calc PR A -1 C1A C 0.0534(10) 0.6985(5) 0.2154(6) 0.084(5) Uani 0.50 1 d PD A -1 H1A4 H -0.0094 0.6731 0.2078 0.101 Uiso 0.50 1 calc PR A -1 H1A5 H 0.0948 0.6824 0.2561 0.101 Uiso 0.50 1 calc PR A -1 C2A C 0.1172(8) 0.6924(4) 0.1532(6) 0.091(3) Uani 0.50 1 d PD A -1 H2A1 H 0.1422 0.6504 0.1509 0.110 Uiso 0.50 1 calc PR A -1 H2A2 H 0.0710 0.6999 0.1111 0.110 Uiso 0.50 1 calc PR A -1 C3A C 0.2078(6) 0.7332(3) 0.1524(4) 0.0752(17) Uani 0.50 1 d PD A -1 H3A1 H 0.2610 0.7213 0.1891 0.090 Uiso 0.50 1 calc PR A -1 H3A2 H 0.1859 0.7749 0.1617 0.090 Uiso 0.50 1 calc PR A -1 C4A C 0.255(2) 0.730(2) 0.0816(15) 0.106(4) Uani 0.50 1 d PD A -1 H4A1 H 0.3259 0.7461 0.0860 0.160 Uiso 0.50 1 calc PR A -1 H4A2 H 0.2124 0.7547 0.0483 0.160 Uiso 0.50 1 calc PR A -1 H4A3 H 0.2556 0.6885 0.0658 0.160 Uiso 0.50 1 calc PR A -1 N1B N -0.0032(11) 0.7418(6) 0.2265(9) 0.104(5) Uani 0.50 1 d PD B -2 H1B1 H -0.0525 0.7289 0.2542 0.156 Uiso 0.25 1 calc PR B -2 H1B2 H -0.0347 0.7581 0.1874 0.156 Uiso 0.25 1 calc PR B -2 H1B3 H 0.0374 0.7701 0.2490 0.156 Uiso 0.50 1 calc PR B -2 C1B C 0.0588(8) 0.6926(6) 0.2090(7) 0.085(5) Uani 0.50 1 d PD B -2 H1B4 H 0.0151 0.6669 0.1770 0.102 Uiso 0.50 1 calc PR B -2 H1B5 H 0.0738 0.6689 0.2516 0.102 Uiso 0.50 1 calc PR B -2 C2B C 0.1585(8) 0.7013(4) 0.1780(4) 0.078(3) Uani 0.50 1 d PD B -2 H2B1 H 0.2066 0.7217 0.2124 0.094 Uiso 0.50 1 calc PR B -2 H2B2 H 0.1879 0.6610 0.1698 0.094 Uiso 0.50 1 calc PR B -2 C3B C 0.1584(5) 0.7353(3) 0.1136(3) 0.0722(17) Uani 0.50 1 d PD B -2 H3B1 H 0.1325 0.7764 0.1217 0.087 Uiso 0.50 1 calc PR B -2 H3B2 H 0.1093 0.7159 0.0789 0.087 Uiso 0.50 1 calc PR B -2 C4B C 0.265(2) 0.740(3) 0.0840(16) 0.106(4) Uani 0.50 1 d PD B -2 H4B1 H 0.3168 0.7540 0.1199 0.160 Uiso 0.50 1 calc PR B -2 H4B2 H 0.2613 0.7685 0.0455 0.160 Uiso 0.50 1 calc PR B -2 H4B3 H 0.2858 0.7003 0.0676 0.160 Uiso 0.50 1 calc PR B -2 N1C N 0.14078(17) 0.59201(10) 0.56940(9) 0.0639(6) Uani 1 1 d D . . H1C1 H 0.1552 0.6136 0.5300 0.050 Uiso 1 1 d . . . H1C2 H 0.0957 0.6148 0.5924 0.050 Uiso 0.50 1 d P . . H1C3 H 0.1204 0.5563 0.5604 0.050 Uiso 0.50 1 d P . . C1C C 0.2401(2) 0.59097(13) 0.61227(13) 0.0693(7) Uani 1 1 d D C -1 H1C4 H 0.2274 0.5746 0.6582 0.083 Uiso 1 1 calc R C -1 H1C5 H 0.2655 0.6328 0.6188 0.083 Uiso 1 1 calc R C -1 C2C C 0.3222(2) 0.55459(14) 0.58251(13) 0.0719(8) Uani 1 1 d D C -1 H2C1 H 0.3382 0.5726 0.5380 0.086 Uiso 1 1 calc R C -1 H2C2 H 0.2950 0.5135 0.5730 0.086 Uiso 1 1 calc R C -1 C3C C 0.4215(3) 0.55000(17) 0.62830(17) 0.0948(10) Uani 1 1 d D C -1 H3C1 H 0.4534 0.5905 0.6320 0.114 Uiso 1 1 calc R C -1 H3C2 H 0.4034 0.5382 0.6749 0.114 Uiso 1 1 calc R C -1 C4C C 0.4996(3) 0.5077(2) 0.6062(2) 0.1279(15) Uani 1 1 d D C -1 H4C1 H 0.4707 0.4668 0.6048 0.192 Uiso 1 1 calc R C -1 H4C2 H 0.5612 0.5089 0.6389 0.192 Uiso 1 1 calc R C -1 H4C3 H 0.5193 0.5189 0.5603 0.192 Uiso 1 1 calc R C -1 N1E N 0.2044(11) 0.4176(12) 0.4188(11) 0.074(3) Uani 0.50 1 d PD D -1 H1E1 H 0.2510 0.4325 0.3904 0.112 Uiso 0.25 1 calc PR D -1 H1E2 H 0.1672 0.4484 0.4355 0.112 Uiso 0.25 1 calc PR D -1 H1E3 H 0.1604 0.3917 0.3949 0.112 Uiso 0.50 1 calc PR D -1 C1E C 0.2603(7) 0.3852(6) 0.4768(5) 0.120(4) Uani 0.50 1 d PD D -1 H1E4 H 0.3039 0.4146 0.5040 0.144 Uiso 0.50 1 calc PR D -1 H1E5 H 0.2083 0.3693 0.5070 0.144 Uiso 0.50 1 calc PR D -1 C2E C 0.3250(5) 0.3366(3) 0.4586(3) 0.0649(17) Uani 0.50 1 d PD D -1 H2E1 H 0.3534 0.3469 0.4142 0.078 Uiso 0.50 1 calc PR D -1 H2E2 H 0.2801 0.3008 0.4504 0.078 Uiso 0.50 1 calc PR D -1 C3E C 0.4141(11) 0.3186(6) 0.5074(9) 0.160(9) Uani 0.50 1 d PD D -1 H3E1 H 0.4714 0.3473 0.5011 0.193 Uiso 0.50 1 calc PR D -1 H3E2 H 0.3923 0.3249 0.5546 0.193 Uiso 0.50 1 calc PR D -1 C4E C 0.457(2) 0.2594(9) 0.5052(11) 0.131(4) Uani 0.50 1 d PD D -1 H4E1 H 0.4648 0.2427 0.5519 0.197 Uiso 0.50 1 calc PR D -1 H4E2 H 0.5250 0.2611 0.4860 0.197 Uiso 0.50 1 calc PR D -1 H4E3 H 0.4102 0.2336 0.4761 0.197 Uiso 0.50 1 calc PR D -1 N1F N 0.1788(12) 0.4123(13) 0.4276(13) 0.091(5) Uani 0.50 1 d PD E -2 H1F1 H 0.1472 0.3782 0.4107 0.136 Uiso 0.25 1 calc PR E -2 H1F2 H 0.1737 0.4415 0.3948 0.136 Uiso 0.25 1 calc PR E -2 H1F3 H 0.1472 0.4249 0.4653 0.136 Uiso 0.50 1 calc PR E -2 C1F C 0.2891(8) 0.3997(4) 0.4469(6) 0.108(3) Uani 0.50 1 d PD E -2 H1F4 H 0.3269 0.3956 0.4047 0.130 Uiso 0.50 1 calc PR E -2 H1F5 H 0.3198 0.4339 0.4740 0.130 Uiso 0.50 1 calc PR E -2 C2F C 0.3007(10) 0.3476(7) 0.4852(7) 0.194(8) Uani 0.50 1 d PD E -2 H2F1 H 0.2614 0.3181 0.4555 0.233 Uiso 0.50 1 calc PR E -2 H2F2 H 0.2559 0.3556 0.5233 0.233 Uiso 0.50 1 calc PR E -2 C3F C 0.3829(11) 0.3101(7) 0.5190(8) 0.133(6) Uani 0.50 1 d PD E -2 H3F1 H 0.4189 0.3359 0.5547 0.160 Uiso 0.50 1 calc PR E -2 H3F2 H 0.3468 0.2785 0.5440 0.160 Uiso 0.50 1 calc PR E -2 C4F C 0.4650(19) 0.2792(9) 0.4852(11) 0.131(4) Uani 0.50 1 d PD E -2 H4F1 H 0.4341 0.2485 0.4539 0.197 Uiso 0.50 1 calc PR E -2 H4F2 H 0.5129 0.2600 0.5199 0.197 Uiso 0.50 1 calc PR E -2 H4F3 H 0.5031 0.3084 0.4589 0.197 Uiso 0.50 1 calc PR E -2 C9 C 0.1729(4) 0.8881(3) 0.3024(3) 0.093(2) Uani 0.59 1 d PD F -1 H9A H 0.1120 0.8917 0.3293 0.139 Uiso 0.59 1 calc PR F -1 H9B H 0.1549 0.8639 0.2611 0.139 Uiso 0.59 1 calc PR F -1 H9C H 0.1953 0.9282 0.2888 0.139 Uiso 0.59 1 calc PR F -1 C10 C 0.2888(8) 0.8908(3) 0.4104(3) 0.116(3) Uani 0.59 1 d PD F -1 H10A H 0.2910 0.9337 0.3988 0.175 Uiso 0.59 1 calc PR F -1 H10B H 0.3564 0.8784 0.4321 0.175 Uiso 0.59 1 calc PR F -1 H10C H 0.2348 0.8838 0.4423 0.175 Uiso 0.59 1 calc PR F -1 C11 C 0.3509(4) 0.8539(3) 0.3000(3) 0.0554(14) Uani 0.59 1 d PD F -1 H11A H 0.3317 0.8261 0.2621 0.083 Uiso 0.59 1 calc PR F -1 H11B H 0.4152 0.8400 0.3250 0.083 Uiso 0.59 1 calc PR F -1 H11C H 0.3617 0.8942 0.2815 0.083 Uiso 0.59 1 calc PR F -1 C9K C 0.1943(8) 0.9063(3) 0.3645(9) 0.148(6) Uani 0.41 1 d PD F -2 H9K1 H 0.1815 0.9048 0.4134 0.222 Uiso 0.41 1 calc PR F -2 H9K2 H 0.1282 0.9021 0.3366 0.222 Uiso 0.41 1 calc PR F -2 H9K3 H 0.2265 0.9449 0.3541 0.222 Uiso 0.41 1 calc PR F -2 C10K C 0.3666(7) 0.8677(4) 0.4028(4) 0.085(3) Uani 0.41 1 d PD F -2 H10D H 0.3893 0.9096 0.3993 0.127 Uiso 0.41 1 calc PR F -2 H10E H 0.4233 0.8408 0.3920 0.127 Uiso 0.41 1 calc PR F -2 H10F H 0.3474 0.8598 0.4497 0.127 Uiso 0.41 1 calc PR F -2 C11K C 0.3075(8) 0.8571(5) 0.2806(4) 0.097(4) Uani 0.41 1 d PD F -2 H11D H 0.2526 0.8465 0.2452 0.145 Uiso 0.41 1 calc PR F -2 H11E H 0.3645 0.8281 0.2798 0.145 Uiso 0.41 1 calc PR F -2 H11F H 0.3335 0.8976 0.2716 0.145 Uiso 0.41 1 calc PR F -2 C20 C 0.5337(7) 0.5244(5) 0.1759(7) 0.073(3) Uani 0.54 1 d PD G -1 H20A H 0.5050 0.4837 0.1783 0.109 Uiso 0.54 1 calc PR G -1 H20B H 0.5578 0.5379 0.2223 0.109 Uiso 0.54 1 calc PR G -1 H20C H 0.5923 0.5242 0.1466 0.109 Uiso 0.54 1 calc PR G -1 C21 C 0.4979(10) 0.6292(4) 0.1398(8) 0.088(5) Uani 0.54 1 d PD G -1 H21A H 0.5181 0.6446 0.1860 0.131 Uiso 0.54 1 calc PR G -1 H21B H 0.4477 0.6567 0.1162 0.131 Uiso 0.54 1 calc PR G -1 H21C H 0.5596 0.6261 0.1135 0.131 Uiso 0.54 1 calc PR G -1 C22 C 0.4105(9) 0.5453(8) 0.0755(4) 0.106(5) Uani 0.54 1 d PD G -1 H22A H 0.4593 0.5573 0.0417 0.159 Uiso 0.54 1 calc PR G -1 H22B H 0.3420 0.5627 0.0626 0.159 Uiso 0.54 1 calc PR G -1 H22C H 0.4050 0.5013 0.0764 0.159 Uiso 0.54 1 calc PR G -1 C20K C 0.5244(9) 0.5170(5) 0.1607(9) 0.089(6) Uani 0.46 1 d PD G -2 H20D H 0.5544 0.5206 0.2082 0.133 Uiso 0.46 1 calc PR G -2 H20E H 0.5799 0.5190 0.1290 0.133 Uiso 0.46 1 calc PR G -2 H20F H 0.4879 0.4785 0.1548 0.133 Uiso 0.46 1 calc PR G -2 C21K C 0.5089(9) 0.6278(4) 0.1487(7) 0.045(3) Uani 0.46 1 d PD G -2 H21D H 0.5518 0.6302 0.1923 0.068 Uiso 0.46 1 calc PR G -2 H21E H 0.4594 0.6613 0.1457 0.068 Uiso 0.46 1 calc PR G -2 H21F H 0.5536 0.6300 0.1102 0.068 Uiso 0.46 1 calc PR G -2 C22K C 0.4029(11) 0.5618(9) 0.0708(5) 0.108(6) Uani 0.46 1 d PD G -2 H22D H 0.4591 0.5622 0.0396 0.163 Uiso 0.46 1 calc PR G -2 H22E H 0.3556 0.5956 0.0599 0.163 Uiso 0.46 1 calc PR G -2 H22F H 0.3644 0.5238 0.0654 0.163 Uiso 0.46 1 calc PR G -2 C42 C -0.2442(8) 0.8381(5) 0.2359(6) 0.091(5) Uani 0.58 1 d PD H -1 H42A H -0.1780 0.8497 0.2602 0.137 Uiso 0.58 1 calc PR H -1 H42B H -0.2829 0.8743 0.2210 0.137 Uiso 0.58 1 calc PR H -1 H42C H -0.2309 0.8136 0.1957 0.137 Uiso 0.58 1 calc PR H -1 C43 C -0.4074(7) 0.7795(5) 0.2446(6) 0.126(5) Uani 0.58 1 d PD H -1 H43A H -0.3887 0.7555 0.2052 0.189 Uiso 0.58 1 calc PR H -1 H43B H -0.4486 0.8144 0.2281 0.189 Uiso 0.58 1 calc PR H -1 H43C H -0.4484 0.7549 0.2744 0.189 Uiso 0.58 1 calc PR H -1 C44 C -0.3387(9) 0.8432(4) 0.3425(4) 0.082(4) Uani 0.58 1 d PD H -1 H44A H -0.3788 0.8208 0.3749 0.124 Uiso 0.58 1 calc PR H -1 H44B H -0.3809 0.8764 0.3225 0.124 Uiso 0.58 1 calc PR H -1 H44C H -0.2755 0.8593 0.3668 0.124 Uiso 0.58 1 calc PR H -1 C42K C -0.2393(9) 0.8401(5) 0.2436(7) 0.081(6) Uani 0.42 1 d PD H -2 H42D H -0.1803 0.8547 0.2737 0.122 Uiso 0.42 1 calc PR H -2 H42E H -0.2791 0.8745 0.2243 0.122 Uiso 0.42 1 calc PR H -2 H42F H -0.2135 0.8163 0.2061 0.122 Uiso 0.42 1 calc PR H -2 C43K C -0.4029(5) 0.7806(4) 0.2387(3) 0.035(2) Uani 0.42 1 d PD H -2 H43D H -0.3791 0.7601 0.1982 0.052 Uiso 0.42 1 calc PR H -2 H43E H -0.4447 0.8158 0.2239 0.052 Uiso 0.42 1 calc PR H -2 H43F H -0.4452 0.7530 0.2641 0.052 Uiso 0.42 1 calc PR H -2 C44K C -0.3523(12) 0.8395(6) 0.3426(6) 0.109(8) Uani 0.42 1 d PD H -2 H44D H -0.4067 0.8170 0.3641 0.163 Uiso 0.42 1 calc PR H -2 H44E H -0.3817 0.8769 0.3228 0.163 Uiso 0.42 1 calc PR H -2 H44F H -0.2960 0.8491 0.3774 0.163 Uiso 0.42 1 calc PR H -2 O1W O 0.0901(2) 0.01755(10) 0.01757(11) 0.1036(8) Uani 1 1 d . . . H1W1 H 0.0188 0.0036 0.0036 0.050 Uiso 0.50 1 d P . . H1W2 H 0.1048 -0.0195 0.0389 0.050 Uiso 1 1 d . . . H1W3 H 0.1188 0.0455 -0.0095 0.050 Uiso 0.50 1 d P . . O2W O -0.0130(4) 0.6608(3) 0.6225(2) 0.0750(13) Uani 0.50 1 d PD . . O2W1 O 0.0023(5) 0.6391(2) 0.6569(3) 0.0627(12) Uani 0.50 1 d P . . H2W H -0.0031(18) 0.6777(11) 0.6689(10) 0.050 Uiso 1 1 d D . . H2V H 0.025(3) 0.6271(12) 0.6491(16) 0.050 Uiso 1 1 d D . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.0414(7) 0.0500(9) 0.0334(7) 0.0048(6) -0.0008(6) -0.0031(6) O2 0.0441(9) 0.0578(10) 0.0515(9) 0.0006(7) -0.0091(7) -0.0012(8) O3 0.0516(9) 0.0438(8) 0.0515(8) 0.0169(7) -0.0064(7) -0.0123(7) O4 0.0438(8) 0.0380(8) 0.0519(9) -0.0018(7) 0.0027(7) -0.0056(6) C1 0.0342(10) 0.0422(11) 0.0272(9) -0.0008(8) -0.0026(7) -0.0007(8) C2 0.0317(10) 0.0466(12) 0.0309(9) -0.0087(8) -0.0013(8) 0.0005(8) C3 0.0337(10) 0.0423(12) 0.0455(11) -0.0083(9) -0.0013(8) 0.0062(9) C4 0.0382(10) 0.0385(11) 0.0442(11) -0.0028(9) 0.0012(9) 0.0012(9) C5 0.0304(10) 0.0418(11) 0.0391(10) -0.0051(8) 0.0011(8) -0.0006(8) C6 0.0332(10) 0.0394(11) 0.0301(9) -0.0053(8) -0.0057(7) 0.0034(8) C7 0.0324(10) 0.0395(11) 0.0422(10) -0.0026(8) -0.0079(8) 0.0018(8) C8 0.0622(15) 0.0383(12) 0.0779(17) -0.0014(11) 0.0215(13) -0.0014(11) C12 0.0350(10) 0.0281(10) 0.0473(11) 0.0015(8) -0.0041(8) 0.0041(8) C13 0.0335(10) 0.0288(10) 0.0426(10) -0.0013(8) -0.0069(8) 0.0063(8) C14 0.0323(10) 0.0334(10) 0.0454(11) -0.0024(8) -0.0080(8) 0.0038(8) C15 0.0344(10) 0.0336(10) 0.0444(11) -0.0039(8) -0.0063(8) 0.0061(8) C16 0.0392(11) 0.0326(10) 0.0471(11) -0.0104(8) -0.0085(9) 0.0072(8) C17 0.0359(10) 0.0253(9) 0.0535(12) -0.0036(8) -0.0065(9) 0.0042(8) C18 0.0441(12) 0.0281(10) 0.0622(13) -0.0072(9) -0.0037(10) 0.0000(8) C19 0.0406(11) 0.0463(12) 0.0466(12) -0.0088(9) -0.0013(9) -0.0005(9) C23 0.0383(10) 0.0277(10) 0.0466(11) 0.0046(8) -0.0040(9) -0.0117(8) C24 0.0375(10) 0.0248(9) 0.0545(12) -0.0039(8) -0.0016(9) -0.0080(8) C25 0.0403(11) 0.0309(10) 0.0448(11) -0.0069(8) 0.0033(9) -0.0066(8) C26 0.0375(10) 0.0296(10) 0.0395(10) -0.0043(8) 0.0011(8) -0.0098(8) C27 0.0331(10) 0.0306(10) 0.0397(10) 0.0006(8) 0.0009(8) -0.0055(8) C28 0.0349(10) 0.0311(10) 0.0409(10) 0.0025(8) -0.0005(8) -0.0112(8) C29 0.0340(10) 0.0472(12) 0.0381(10) 0.0059(8) 0.0010(8) -0.0114(9) C30 0.0497(12) 0.0413(12) 0.0360(10) 0.0003(8) 0.0010(9) -0.0117(9) C31 0.0736(16) 0.0491(14) 0.0495(13) 0.0022(10) 0.0170(12) 0.0063(12) C32 0.093(2) 0.086(2) 0.0462(13) 0.0096(12) -0.0170(13) -0.0441(16) C33 0.0562(14) 0.0565(14) 0.0440(12) 0.0119(10) 0.0071(10) 0.0103(11) C34 0.0318(10) 0.0554(13) 0.0309(9) 0.0002(9) 0.0055(8) -0.0026(9) C35 0.0317(10) 0.0506(12) 0.0323(9) 0.0019(8) 0.0077(8) -0.0099(9) C36 0.0299(10) 0.0497(12) 0.0333(9) -0.0017(8) 0.0026(8) -0.0080(8) C37 0.0301(9) 0.0523(13) 0.0361(10) -0.0029(9) 0.0055(8) -0.0051(9) C38 0.0339(10) 0.0512(12) 0.0372(10) -0.0083(9) 0.0061(8) -0.0060(9) C39 0.0296(9) 0.0578(13) 0.0309(9) -0.0082(9) 0.0064(8) -0.0043(9) C40 0.0357(10) 0.0590(13) 0.0336(10) -0.0127(9) 0.0022(8) -0.0020(9) C41 0.0453(12) 0.0512(13) 0.0497(12) -0.0043(10) -0.0051(10) -0.0028(10) N1A 0.072(4) 0.062(6) 0.055(4) 0.027(3) 0.030(3) 0.002(3) C1A 0.112(11) 0.055(7) 0.087(7) 0.015(5) 0.028(6) -0.032(7) C2A 0.085(6) 0.077(5) 0.112(8) -0.046(6) 0.004(6) -0.011(4) C3A 0.086(5) 0.068(4) 0.071(4) 0.010(3) -0.003(4) -0.001(4) C4A 0.102(5) 0.133(12) 0.084(3) 0.001(4) 0.012(3) 0.051(5) N1B 0.137(12) 0.060(7) 0.124(7) 0.038(5) 0.067(7) 0.029(7) C1B 0.065(7) 0.077(7) 0.106(9) -0.045(6) -0.032(6) 0.022(5) C2B 0.100(8) 0.063(5) 0.068(5) -0.001(4) -0.021(5) 0.034(5) C3B 0.061(4) 0.089(5) 0.064(4) 0.003(3) -0.014(3) 0.020(3) C4B 0.102(5) 0.133(12) 0.084(3) 0.001(4) 0.012(3) 0.051(5) N1C 0.0802(15) 0.0719(14) 0.0398(10) 0.0124(9) 0.0054(10) 0.0235(11) C1C 0.0791(18) 0.0753(18) 0.0526(14) 0.0048(12) -0.0015(13) 0.0151(14) C2C 0.0786(19) 0.0774(19) 0.0599(15) 0.0181(13) 0.0067(14) 0.0170(15) C3C 0.094(2) 0.106(3) 0.085(2) 0.0138(18) 0.0054(18) 0.026(2) C4C 0.110(3) 0.152(4) 0.121(3) 0.021(3) 0.007(2) 0.060(3) N1E 0.049(6) 0.095(8) 0.077(5) 0.009(4) -0.005(5) 0.007(6) C1E 0.079(5) 0.159(10) 0.127(7) 0.089(7) 0.046(5) 0.041(5) C2E 0.060(4) 0.077(4) 0.058(4) -0.006(3) 0.004(3) 0.004(3) C3E 0.079(8) 0.135(10) 0.26(2) -0.109(12) -0.053(10) 0.014(7) C4E 0.127(6) 0.137(13) 0.128(11) 0.030(7) -0.005(7) 0.011(9) N1F 0.064(8) 0.096(6) 0.111(10) 0.000(7) -0.006(7) -0.007(7) C1F 0.111(8) 0.093(6) 0.116(7) -0.013(5) -0.017(6) -0.019(6) C2F 0.201(13) 0.199(13) 0.200(14) 0.114(11) 0.141(11) 0.125(11) C3F 0.097(9) 0.174(13) 0.130(8) 0.049(8) 0.020(7) 0.059(8) C4F 0.127(6) 0.137(13) 0.128(11) 0.030(7) -0.005(7) 0.011(9) C9 0.082(4) 0.059(4) 0.141(5) 0.046(4) 0.042(4) 0.030(3) C10 0.190(9) 0.066(4) 0.101(5) -0.044(4) 0.063(6) -0.059(5) C11 0.057(3) 0.043(3) 0.066(4) 0.004(3) 0.010(3) -0.002(2) C9K 0.095(8) 0.034(4) 0.32(2) 0.021(8) 0.073(12) 0.016(5) C10K 0.118(7) 0.065(5) 0.068(5) 0.000(4) -0.015(5) -0.052(5) C11K 0.149(12) 0.077(6) 0.061(5) 0.024(4) -0.016(6) -0.049(8) C20 0.036(4) 0.088(7) 0.095(5) -0.008(4) 0.015(3) 0.019(4) C21 0.096(9) 0.088(8) 0.084(8) -0.009(5) 0.046(7) 0.001(6) C22 0.055(5) 0.205(13) 0.059(6) -0.033(6) 0.021(4) -0.020(6) C20K 0.099(9) 0.034(4) 0.139(12) 0.014(6) 0.057(8) 0.021(5) C21K 0.041(4) 0.032(5) 0.062(5) 0.002(4) -0.002(4) -0.007(3) C22K 0.099(11) 0.182(13) 0.044(6) -0.032(6) -0.001(5) -0.090(10) C42 0.085(8) 0.101(9) 0.089(6) -0.001(5) 0.021(5) -0.010(6) C43 0.094(8) 0.082(9) 0.193(11) -0.003(7) -0.054(8) 0.019(7) C44 0.090(7) 0.074(6) 0.082(7) 0.006(5) -0.003(5) 0.035(5) C42K 0.075(9) 0.051(7) 0.111(10) 0.052(7) -0.045(7) -0.017(6) C43K 0.027(4) 0.038(5) 0.037(3) 0.002(3) -0.015(3) -0.007(4) C44K 0.091(9) 0.134(14) 0.093(10) -0.086(9) -0.049(8) 0.061(9) O1W 0.157(2) 0.0758(14) 0.0799(14) 0.0097(11) 0.0224(14) 0.0241(14) O2W 0.068(3) 0.095(4) 0.063(3) -0.021(3) 0.010(2) 0.010(3) O2W1 0.073(3) 0.052(3) 0.066(3) -0.011(2) 0.029(3) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C1 1.353(2) . ? O2 C34 1.353(2) . ? O3 C23 1.379(2) . ? O4 C12 1.364(2) . ? C1 C6 1.400(3) . ? C1 C2 1.403(3) . ? C2 C3 1.388(3) . ? C2 C40 1.515(3) . ? C3 C4 1.394(3) . ? C4 C5 1.390(3) . ? C4 C8 1.533(3) . ? C5 C6 1.389(3) . ? C6 C7 1.522(3) . ? C7 C13 1.526(3) . ? C8 C10 1.451(5) . ? C8 C11K 1.458(8) . ? C8 C9K 1.496(7) . ? C8 C11 1.499(5) . ? C8 C9 1.603(6) . ? C8 C10K 1.643(7) . ? C12 C17 1.401(3) . ? C12 C13 1.403(3) . ? C13 C14 1.382(3) . ? C14 C15 1.400(3) . ? C15 C16 1.393(3) . ? C15 C19 1.529(3) . ? C16 C17 1.384(3) . ? C17 C18 1.522(3) . ? C18 C24 1.512(3) . ? C19 C22 1.499(8) . ? C19 C20K 1.502(8) . ? C19 C21 1.513(8) . ? C19 C22K 1.533(8) . ? C19 C20 1.541(8) . ? C19 C21K 1.542(7) . ? C23 C28 1.396(3) . ? C23 C24 1.403(3) . ? C24 C25 1.388(3) . ? C25 C26 1.390(3) . ? C26 C27 1.390(3) . ? C26 C30 1.534(3) . ? C27 C28 1.389(3) . ? C28 C29 1.519(3) . ? C29 C35 1.512(3) . ? C30 C31 1.527(3) . ? C30 C33 1.530(3) . ? C30 C32 1.537(3) . ? C34 C39 1.395(3) . ? C34 C35 1.401(3) . ? C35 C36 1.386(3) . ? C36 C37 1.389(3) . ? C37 C38 1.401(3) . ? C37 C41 1.531(3) . ? C38 C39 1.384(3) . ? C39 C40 1.525(3) . ? C41 C43 1.520(8) . ? C41 C43K 1.525(6) . ? C41 C42K 1.526(8) . ? C41 C44 1.528(7) . ? C41 C44K 1.547(8) . ? C41 C42 1.553(7) . ? N1A C1A 1.392(13) . ? C1A C2A 1.520(12) . ? C2A C3A 1.480(10) . ? C3A C4A 1.547(18) . ? N1B C1B 1.411(13) . ? C1B C2B 1.473(12) . ? C2B C3B 1.463(10) . ? C3B C4B 1.537(18) . ? N1C C1C 1.477(3) . ? C1C C2C 1.484(4) . ? C2C C3C 1.509(4) . ? C3C C4C 1.466(5) . ? N1E C1E 1.481(15) . ? C1E C2E 1.424(11) . ? C2E C3E 1.491(13) . ? C3E C4E 1.429(15) . ? N1F C1F 1.472(14) . ? C1F C2F 1.379(12) . ? C2F C3F 1.466(13) . ? C3F C4F 1.459(16) . ? O2W O2W1 0.835(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 C6 120.05(17) . . ? O1 C1 C2 120.33(17) . . ? C6 C1 C2 119.62(17) . . ? C3 C2 C1 118.99(17) . . ? C3 C2 C40 119.37(17) . . ? C1 C2 C40 121.64(18) . . ? C2 C3 C4 122.76(18) . . ? C5 C4 C3 116.78(18) . . ? C5 C4 C8 122.47(18) . . ? C3 C4 C8 120.67(18) . . ? C6 C5 C4 122.59(18) . . ? C5 C6 C1 119.24(17) . . ? C5 C6 C7 120.98(17) . . ? C1 C6 C7 119.74(17) . . ? C6 C7 C13 115.71(15) . . ? C10 C8 C11K 132.6(5) . . ? C10 C8 C9K 61.1(6) . . ? C11K C8 C9K 117.0(7) . . ? C10 C8 C11 114.9(4) . . ? C11K C8 C11 25.6(4) . . ? C9K C8 C11 130.4(5) . . ? C10 C8 C4 109.3(3) . . ? C11K C8 C4 112.6(5) . . ? C9K C8 C4 114.1(4) . . ? C11 C8 C4 113.1(3) . . ? C10 C8 C9 109.1(4) . . ? C11K C8 C9 78.6(5) . . ? C9K C8 C9 48.9(6) . . ? C11 C8 C9 102.6(3) . . ? C4 C8 C9 107.2(3) . . ? C10 C8 C10K 42.9(4) . . ? C11K C8 C10K 104.6(5) . . ? C9K C8 C10K 102.3(6) . . ? C11 C8 C10K 79.9(4) . . ? C4 C8 C10K 104.1(3) . . ? C9 C8 C10K 144.4(4) . . ? O4 C12 C17 117.73(17) . . ? O4 C12 C13 122.11(17) . . ? C17 C12 C13 120.11(18) . . ? C14 C13 C12 118.50(17) . . ? C14 C13 C7 119.96(17) . . ? C12 C13 C7 121.49(17) . . ? C13 C14 C15 123.31(18) . . ? C16 C15 C14 116.05(18) . . ? C16 C15 C19 121.88(17) . . ? C14 C15 C19 121.86(17) . . ? C17 C16 C15 123.11(18) . . ? C16 C17 C12 118.82(17) . . ? C16 C17 C18 120.47(18) . . ? C12 C17 C18 120.71(18) . . ? C24 C18 C17 113.52(16) . . ? C22 C19 C20K 95.7(12) . . ? C22 C19 C21 110.3(7) . . ? C20K C19 C21 115.1(9) . . ? C22 C19 C15 112.0(4) . . ? C20K C19 C15 110.5(5) . . ? C21 C19 C15 112.3(5) . . ? C22 C19 C22K 14.7(14) . . ? C20K C19 C22K 109.0(7) . . ? C21 C19 C22K 98.3(11) . . ? C15 C19 C22K 111.1(6) . . ? C22 C19 C20 108.8(7) . . ? C20K C19 C20 13.2(12) . . ? C21 C19 C20 107.6(6) . . ? C15 C19 C20 105.6(5) . . ? C22K C19 C20 121.9(11) . . ? C22 C19 C21K 117.2(10) . . ? C20K C19 C21K 109.0(6) . . ? C21 C19 C21K 8.1(10) . . ? C15 C19 C21K 111.3(5) . . ? C22K C19 C21K 105.8(7) . . ? C20 C19 C21K 100.6(8) . . ? O3 C23 C28 119.45(17) . . ? O3 C23 C24 120.01(17) . . ? C28 C23 C24 120.53(17) . . ? C25 C24 C23 118.49(18) . . ? C25 C24 C18 120.61(18) . . ? C23 C24 C18 120.90(18) . . ? C24 C25 C26 122.70(18) . . ? C25 C26 C27 116.80(17) . . ? C25 C26 C30 122.79(17) . . ? C27 C26 C30 120.37(17) . . ? C28 C27 C26 123.07(18) . . ? C27 C28 C23 118.21(18) . . ? C27 C28 C29 119.72(17) . . ? C23 C28 C29 121.99(17) . . ? C35 C29 C28 111.65(14) . . ? C31 C30 C33 107.80(17) . . ? C31 C30 C26 112.67(18) . . ? C33 C30 C26 110.88(16) . . ? C31 C30 C32 108.30(19) . . ? C33 C30 C32 108.9(2) . . ? C26 C30 C32 108.16(16) . . ? O2 C34 C39 121.33(18) . . ? O2 C34 C35 117.74(18) . . ? C39 C34 C35 120.91(19) . . ? C36 C35 C34 118.17(18) . . ? C36 C35 C29 121.81(17) . . ? C34 C35 C29 119.98(18) . . ? C35 C36 C37 123.12(18) . . ? C36 C37 C38 116.60(19) . . ? C36 C37 C41 123.23(18) . . ? C38 C37 C41 120.15(18) . . ? C39 C38 C37 122.71(19) . . ? C38 C39 C34 118.48(18) . . ? C38 C39 C40 120.89(19) . . ? C34 C39 C40 120.63(19) . . ? C2 C40 C39 113.91(15) . . ? C43 C41 C43K 5.1(7) . . ? C43 C41 C42K 114.0(8) . . ? C43K C41 C42K 109.2(5) . . ? C43 C41 C44 109.1(6) . . ? C43K C41 C44 112.6(6) . . ? C42K C41 C44 103.2(9) . . ? C43 C41 C37 111.9(5) . . ? C43K C41 C37 113.1(4) . . ? C42K C41 C37 108.4(5) . . ? C44 C41 C37 109.9(4) . . ? C43 C41 C44K 102.6(9) . . ? C43K C41 C44K 106.3(6) . . ? C42K C41 C44K 109.1(7) . . ? C44 C41 C44K 7.2(11) . . ? C37 C41 C44K 110.7(6) . . ? C43 C41 C42 108.2(6) . . ? C43K C41 C42 103.4(6) . . ? C42K C41 C42 6.0(10) . . ? C44 C41 C42 107.5(5) . . ? C37 C41 C42 110.1(4) . . ? C44K C41 C42 113.1(10) . . ? N1A C1A C2A 115.7(8) . . ? C3A C2A C1A 115.3(8) . . ? C2A C3A C4A 110.2(15) . . ? N1B C1B C2B 121.7(10) . . ? C3B C2B C1B 118.3(8) . . ? C2B C3B C4B 114.4(19) . . ? N1C C1C C2C 113.7(2) . . ? C1C C2C C3C 113.9(2) . . ? C4C C3C C2C 116.2(3) . . ? C2E C1E N1E 116.2(12) . . ? C1E C2E C3E 118.9(8) . . ? C4E C3E C2E 120.6(14) . . ? C2F C1F N1F 111.3(13) . . ? C1F C2F C3F 140.0(13) . . ? C4F C3F C2F 126.1(13) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.76 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.320 _refine_diff_density_min -0.390 _refine_diff_density_rms 0.040 data_compound_3_(ku82) _database_code_depnum_ccdc_archive 'CCDC 192203' _audit_creation_method SHELXL-97 _chemical_name_systematic ; t-butyl-calix[4]arene*2(Zn(n-butylamine)3) 2Cl ; _chemical_name_common 't-butyl-calix[4]arene*2(Zn(n-butylamine)3) 2Cl' _chemical_melting_point ? _chemical_formula_moiety 'C44H56O4 C4H9NH2' _chemical_formula_sum 'C36 H66.11 Cl1.16 N3.50 O2.50 Zn' _chemical_formula_weight 694.53 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' Zn Zn 0.2839 1.4301 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5854(15) _cell_length_b 16.2134(19) _cell_length_c 20.695(2) _cell_angle_alpha 77.408(2) _cell_angle_beta 86.846(2) _cell_angle_gamma 79.320(2) _cell_volume 4049.5(8) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.139 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1505 _exptl_absorpt_coefficient_mu 0.716 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71070 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48385 _diffrn_reflns_av_R_equivalents 0.0611 _diffrn_reflns_av_sigmaI/netI 0.0782 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 28.78 _reflns_number_total 20806 _reflns_number_gt 12305 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1561P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 20806 _refine_ls_number_parameters 996 _refine_ls_number_restraints 82 _refine_ls_R_factor_all 0.1257 _refine_ls_R_factor_gt 0.0736 _refine_ls_wR_factor_ref 0.2491 _refine_ls_wR_factor_gt 0.2077 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.561 _refine_ls_shift/su_mean 0.018 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 N1A N 0.19297(3) 0.32791(3) 0.35572(2) 0.00503(10) Uani 0.68 1 d PDU A -11 H1A1 H 0.2649 0.3132 0.3467 0.050 Uiso 0.68 1 d P B -11 H1A2 H 0.1571 0.3494 0.3168 0.050 Uiso 0.68 1 d P C -11 C1A C 0.15487(5) 0.25930(3) 0.38930(3) 0.01282(13) Uani 0.68 1 d PD A -11 H1A3 H 0.0751 0.2719 0.3860 0.015 Uiso 0.68 1 calc PR A -11 H1A4 H 0.1724 0.2515 0.4366 0.015 Uiso 0.68 1 calc PR A -11 C2A C 0.19378(7) 0.17809(4) 0.36915(3) 0.0339(2) Uani 0.68 1 d PD A -11 H2A1 H 0.1321 0.1472 0.3727 0.041 Uiso 0.68 1 calc PR A -11 H2A2 H 0.2478 0.1433 0.4018 0.041 Uiso 0.68 1 calc PR A -11 C3A C 0.24376(7) 0.17956(6) 0.30148(4) 0.0457(3) Uani 0.68 1 d PD A -11 H3A1 H 0.3129 0.1383 0.3048 0.055 Uiso 0.68 1 calc PR A -11 H3A2 H 0.2593 0.2376 0.2821 0.055 Uiso 0.68 1 calc PR A -11 C4A C 0.16575(7) 0.15541(5) 0.25621(4) 0.0420(2) Uani 0.68 1 d PD A -11 H4A1 H 0.1434 0.1012 0.2781 0.063 Uiso 0.68 1 calc PR A -11 H4A2 H 0.2026 0.1488 0.2142 0.063 Uiso 0.68 1 calc PR A -11 H4A3 H 0.1019 0.2009 0.2476 0.063 Uiso 0.68 1 calc PR A -11 Cl3 Cl 0.09763(3) 0.26130(2) 0.439400(18) 0.03025(11) Uani 0.32 1 d P D -18 N1H N 0.17499(7) 0.19752(5) 0.36285(4) 0.00503(10) Uani 0.32 1 d PDU E -12 H1H1 H 0.1038 0.2156 0.3528 0.008 Uiso 0.32 1 calc PR E -12 H1H2 H 0.2009 0.2397 0.3764 0.008 Uiso 0.32 1 calc PR E -12 H1H3 H 0.1825 0.1496 0.3958 0.008 Uiso 0.32 1 calc PR E -12 C1H C 0.23590(8) 0.17775(7) 0.30395(4) 0.01282(13) Uani 0.32 1 d PD E -12 H1H4 H 0.2941 0.1276 0.3178 0.015 Uiso 0.32 1 calc PR E -12 H1H5 H 0.2704 0.2272 0.2826 0.015 Uiso 0.32 1 calc PR E -12 C2H C 0.16570(9) 0.15833(7) 0.25390(6) 0.0339(2) Uani 0.32 1 d PD E -12 H2H1 H 0.1496 0.0998 0.2703 0.041 Uiso 0.32 1 calc PR E -12 H2H2 H 0.2072 0.1585 0.2118 0.041 Uiso 0.32 1 calc PR E -12 C3H C 0.05981(10) 0.22092(7) 0.23995(9) 0.0457(3) Uani 0.32 1 d PD E -12 H3H1 H 0.0138 0.1984 0.2131 0.055 Uiso 0.32 1 calc PR E -12 H3H2 H 0.0212 0.2256 0.2823 0.055 Uiso 0.32 1 calc PR E -12 C4H C 0.07686(15) 0.30874(7) 0.20369(8) 0.0420(2) Uani 0.32 1 d PD E -12 H4H1 H 0.1200 0.3322 0.2309 0.063 Uiso 0.32 1 calc PR E -12 H4H2 H 0.0066 0.3467 0.1949 0.063 Uiso 0.32 1 calc PR E -12 H4H3 H 0.1150 0.3044 0.1616 0.063 Uiso 0.32 1 calc PR E -12 Zn1 Zn 0.141037(5) 0.425652(4) 0.394939(3) 0.03057(2) Uani 1 1 d . F -12 N1B N -0.02087(6) 0.45641(5) 0.39853(3) 0.0264(2) Uani 0.55 1 d PD G -1 H1B1 H -0.0507 0.5130 0.3993 0.050 Uiso 0.55 1 d P H -1 H1B2 H -0.0312 0.4225 0.4368 0.050 Uiso 0.55 1 d P I -1 C1B C -0.06714(7) 0.43061(7) 0.34199(4) 0.0344(3) Uani 0.55 1 d PD G -1 H1B1' H -0.0299 0.4546 0.3007 0.041 Uiso 0.55 1 calc PR G -1 H1B2' H -0.0496 0.3673 0.3487 0.041 Uiso 0.55 1 calc PR G -1 C2B C -0.18646(7) 0.45756(7) 0.33188(5) 0.0366(3) Uani 0.55 1 d PD G -1 H2B1 H -0.2067 0.5201 0.3297 0.044 Uiso 0.55 1 calc PR G -1 H2B2 H -0.2252 0.4277 0.3703 0.044 Uiso 0.55 1 calc PR G -1 C3B C -0.22212(9) 0.43713(8) 0.26813(5) 0.0467(3) Uani 0.55 1 d PD G -1 C4B C -0.34245(10) 0.47090(11) 0.25470(7) 0.0732(5) Uani 0.55 1 d PD G -1 H4B1 H -0.3593 0.5320 0.2560 0.110 Uiso 0.55 1 calc PR G -1 H4B2 H -0.3856 0.4389 0.2886 0.110 Uiso 0.55 1 calc PR G -1 H4B3 H -0.3595 0.4635 0.2109 0.110 Uiso 0.55 1 calc PR G -1 N1J N -0.02517(11) 0.45386(8) 0.40240(6) 0.0541(4) Uani 0.45 1 d PD J -2 H1J1 H -0.0506 0.5024 0.4156 0.050 Uiso 0.45 1 d P K -2 H1J2 H -0.0458 0.4083 0.4383 0.050 Uiso 0.45 1 d P L -2 C1J C -0.09110(10) 0.44922(9) 0.34462(6) 0.0442(4) Uani 0.45 1 d PD J -2 H1J1' H -0.0639 0.4829 0.3033 0.053 Uiso 0.45 1 calc PR J -2 H1J2' H -0.0823 0.3888 0.3401 0.053 Uiso 0.45 1 calc PR J -2 C2J C -0.20841(9) 0.48346(9) 0.35401(6) 0.0401(4) Uani 0.45 1 d PD J -2 H2J1 H -0.2186 0.5447 0.3564 0.048 Uiso 0.45 1 calc PR J -2 H2J2 H -0.2361 0.4512 0.3958 0.048 Uiso 0.45 1 calc PR J -2 C3J C -0.26990(11) 0.47349(10) 0.29477(6) 0.0519(5) Uani 0.45 1 d PD J -2 H3J1 H -0.2414 0.5056 0.2532 0.062 Uiso 0.45 1 calc PR J -2 H3J2 H -0.2590 0.4121 0.2924 0.062 Uiso 0.45 1 calc PR J -2 C4J C -0.39056(11) 0.50783(13) 0.30227(9) 0.0678(6) Uani 0.45 1 d PD J -2 H4J1 H -0.4239 0.4648 0.3334 0.102 Uiso 0.45 1 calc PR J -2 H4J2 H -0.4251 0.5199 0.2591 0.102 Uiso 0.45 1 calc PR J -2 H4J3 H -0.4000 0.5608 0.3191 0.102 Uiso 0.45 1 calc PR J -2 N1C N 0.18879(4) 0.53176(3) 0.33296(2) 0.03439(13) Uani 1 1 d . M -2 H1C1 H 0.1309 0.5557 0.3069 0.050 Uiso 1 1 d . N -2 H1C2 H 0.1966 0.5668 0.3609 0.050 Uiso 1 1 d . O -2 C1C C 0.28665(5) 0.52101(4) 0.29157(3) 0.04606(19) Uani 1 1 d . M -2 H1C1' H 0.3484 0.4895 0.3198 0.055 Uiso 1 1 calc R M -2 H1C2' H 0.3031 0.5782 0.2703 0.055 Uiso 1 1 calc R M -2 C2C C 0.27324(5) 0.47224(4) 0.23849(3) 0.04072(18) Uani 1 1 d . M -2 H2C1 H 0.2600 0.4143 0.2604 0.049 Uiso 1 1 calc R M -2 H2C2 H 0.2084 0.5023 0.2125 0.049 Uiso 1 1 calc R M -2 C3C C 0.36608(8) 0.46280(7) 0.19262(4) 0.0877(3) Uani 1 1 d . M -2 H3C1 H 0.3807 0.5208 0.1723 0.105 Uiso 1 1 calc R M -2 H3C2 H 0.4302 0.4314 0.2188 0.105 Uiso 1 1 calc R M -2 C4C C 0.35563(9) 0.41876(7) 0.13950(4) 0.0993(4) Uani 1 1 d . M -2 H4C1 H 0.3615 0.3571 0.1578 0.149 Uiso 1 1 calc R M -2 H4C2 H 0.4133 0.4284 0.1064 0.149 Uiso 1 1 calc R M -2 H4C3 H 0.2851 0.4413 0.1186 0.149 Uiso 1 1 calc R M -2 N1D N 0.20469(5) 0.41626(4) 0.48607(3) 0.02244(17) Uani 0.62 1 d PD P -1 H1D1 H 0.2248 0.4654 0.4810 0.050 Uiso 0.62 1 d P Q -1 H1D2 H 0.1573 0.4055 0.5202 0.050 Uiso 0.62 1 d P R -1 C1D C 0.30312(7) 0.34768(6) 0.50292(5) 0.0360(3) Uani 0.62 1 d PD P -1 H1D1' H 0.2863 0.2924 0.4974 0.043 Uiso 0.62 1 calc PR P -1 H1D2' H 0.3203 0.3414 0.5501 0.043 Uiso 0.62 1 calc PR P -1 C2D C 0.40152(7) 0.36606(7) 0.46093(6) 0.0479(3) Uani 0.62 1 d PD P -1 H2D1 H 0.4614 0.3165 0.4718 0.057 Uiso 0.62 1 calc PR P -1 H2D2 H 0.3846 0.3744 0.4135 0.057 Uiso 0.62 1 calc PR P -1 C3D C 0.43590(9) 0.44492(8) 0.47303(6) 0.0599(4) Uani 0.62 1 d PD P -1 H3D1 H 0.4374 0.4415 0.5213 0.072 Uiso 0.62 1 calc PR P -1 H3D2 H 0.3823 0.4960 0.4536 0.072 Uiso 0.62 1 calc PR P -1 C4D C 0.54845(10) 0.45546(11) 0.44268(9) 0.0918(7) Uani 0.62 1 d PD P -1 H4D1 H 0.6005 0.4029 0.4587 0.138 Uiso 0.62 1 calc PR P -1 H4D2 H 0.5714 0.5040 0.4557 0.138 Uiso 0.62 1 calc PR P -1 H4D3 H 0.5450 0.4662 0.3943 0.138 Uiso 0.62 1 calc PR P -1 N1K N 0.20683(12) 0.40871(9) 0.48081(9) 0.0619(5) Uani 0.38 1 d PD S -2 H1K1 H 0.2142 0.4627 0.4979 0.050 Uiso 0.38 1 d P T -2 H1K2 H 0.1478 0.3943 0.4889(9) 0.050 Uiso 0.38 1 d P U -2 C1K C 0.30957(14) 0.34552(18) 0.49821(10) 0.1046(10) Uani 0.38 1 d PD S -2 H1K1' H 0.2952 0.2865 0.5026 0.125 Uiso 0.38 1 calc PR S -2 H1K2' H 0.3350 0.3503 0.5414 0.125 Uiso 0.38 1 calc PR S -2 C2K C 0.39685(17) 0.36117(16) 0.44611(15) 0.1491(16) Uani 0.38 1 d PD S -2 H2K1 H 0.4257 0.4124 0.4507 0.179 Uiso 0.38 1 calc PR S -2 H2K2 H 0.3645 0.3737 0.4017 0.179 Uiso 0.38 1 calc PR S -2 C3K C 0.49040(15) 0.28468(13) 0.45093(12) 0.1149(13) Uani 0.38 1 d PD S -2 H3K1 H 0.5559 0.3044 0.4290 0.138 Uiso 0.38 1 calc PR S -2 H3K2 H 0.5069 0.2588 0.4980 0.138 Uiso 0.38 1 calc PR S -2 C4K C 0.4585(2) 0.21776(13) 0.41729(11) 0.1017(11) Uani 0.38 1 d PD S -2 H4K1 H 0.4445 0.1681 0.4511 0.153 Uiso 0.38 1 calc PR S -2 H4K2 H 0.5175 0.1992 0.3879 0.153 Uiso 0.38 1 calc PR S -2 H4K3 H 0.3931 0.2431 0.3914 0.153 Uiso 0.38 1 calc PR S -2 O1 O 1.09493(3) -0.31552(2) 0.213890(16) 0.02920(10) Uani 1 1 d . . . O2 O 1.08732(3) -0.17426(2) 0.239409(16) 0.02747(10) Uani 1 1 d . . . H2 H 1.1173(12) -0.2556(10) 0.2571(7) 0.202(6) Uiso 1 1 d . . . O3 O 0.90439(3) -0.17647(2) 0.297108(17) 0.03147(11) Uani 1 1 d . . . H3 H 0.9588(6) -0.1706(5) 0.2800(4) 0.069(2) Uiso 1 1 d . . . O4 O 0.91825(3) -0.34972(3) 0.271507(17) 0.03308(11) Uani 1 1 d . . . H4 H 0.9889(5) -0.3441(4) 0.2429(3) 0.0364(16) Uiso 1 1 d . . . C1 C 1.11696(4) -0.32058(3) 0.14889(2) 0.02506(13) Uani 1 1 d . . . C2 C 1.06581(4) -0.37405(3) 0.12073(2) 0.02708(14) Uani 1 1 d . . . C3 C 1.09417(4) -0.38240(3) 0.05609(2) 0.02725(13) Uani 1 1 d . . . H3A H 1.0600 -0.4188 0.0371 0.033 Uiso 1 1 calc R . . C4 C 1.16982(4) -0.34004(3) 0.01833(2) 0.02798(14) Uani 1 1 d . . . C5 C 1.21588(4) -0.28518(3) 0.04752(2) 0.02678(14) Uani 1 1 d . . . H5 H 1.2660 -0.2536 0.0221 0.032 Uiso 1 1 calc R . . C6 C 1.19184(4) -0.27468(3) 0.11176(2) 0.02460(13) Uani 1 1 d . . . C7 C 1.24411(4) -0.21467(3) 0.14083(2) 0.02715(13) Uani 1 1 d . . . H7A H 1.3140 -0.2085 0.1176 0.033 Uiso 1 1 calc R . . H7B H 1.2598 -0.2409 0.1880 0.033 Uiso 1 1 calc R . . C8 C 1.20308(5) -0.34979(4) -0.05247(3) 0.03444(15) Uani 1 1 d . . . C9 C 1.15187(5) -0.41991(4) -0.07171(3) 0.04524(18) Uani 1 1 d . . . H9A H 1.1769 -0.4268 -0.1162 0.054 Uiso 1 1 calc R . . H9B H 1.0729 -0.4033 -0.0712 0.054 Uiso 1 1 calc R . . H9C H 1.1732 -0.4743 -0.0400 0.054 Uiso 1 1 calc R . . C10 C 1.32594(5) -0.37421(4) -0.05868(3) 0.04485(19) Uani 1 1 d . . . H10A H 1.3598 -0.3273 -0.0512 0.054 Uiso 1 1 calc R . . H10B H 1.3453 -0.3844 -0.1031 0.054 Uiso 1 1 calc R . . H10C H 1.3515 -0.4265 -0.0256 0.054 Uiso 1 1 calc R . . C11 C 1.16440(6) -0.26505(4) -0.10053(3) 0.04296(19) Uani 1 1 d . . . H11A H 1.1935 -0.2191 -0.0876 0.052 Uiso 1 1 calc R . . H11B H 1.0852 -0.2518 -0.0994 0.052 Uiso 1 1 calc R . . H11C H 1.1896 -0.2698 -0.1454 0.052 Uiso 1 1 calc R . . C12 C 1.09843(4) -0.11008(3) 0.18564(2) 0.02587(13) Uani 1 1 d . . . C13 C 1.17581(4) -0.12570(3) 0.13643(2) 0.02597(13) Uani 1 1 d . . . C14 C 1.18908(4) -0.05915(3) 0.08282(2) 0.02655(13) Uani 1 1 d . . . H14 H 1.2424 -0.0700 0.0500 0.032 Uiso 1 1 calc R . . C15 C 1.12705(4) 0.02235(3) 0.07586(2) 0.02703(13) Uani 1 1 d . . . C16 C 1.04932(4) 0.03504(3) 0.12524(2) 0.02803(14) Uani 1 1 d . . . H16 H 1.0050 0.0901 0.1212 0.034 Uiso 1 1 calc R . . C17 C 1.03344(4) -0.02878(3) 0.18014(2) 0.02551(13) Uani 1 1 d . . . C18 C 0.94984(4) -0.00852(3) 0.23282(2) 0.02958(14) Uani 1 1 d . . . H18A H 0.9360 0.0543 0.2298 0.036 Uiso 1 1 calc R . . H18B H 0.9812 -0.0360 0.2768 0.036 Uiso 1 1 calc R . . C19 C 1.13980(4) 0.09637(3) 0.01699(3) 0.03046(15) Uani 1 1 d . . . C20 C 1.23022(5) 0.07084(4) -0.03039(3) 0.04341(19) Uani 1 1 d . . . H20A H 1.2138 0.0241 -0.0490 0.052 Uiso 1 1 calc R . . H20B H 1.2985 0.0516 -0.0065 0.052 Uiso 1 1 calc R . . H20C H 1.2368 0.1204 -0.0662 0.052 Uiso 1 1 calc R . . C21 C 1.16774(5) 0.17164(4) 0.04300(3) 0.04207(18) Uani 1 1 d . . . H21A H 1.2374 0.1535 0.0654 0.050 Uiso 1 1 calc R . . H21B H 1.1113 0.1892 0.0743 0.050 Uiso 1 1 calc R . . H21C H 1.1722 0.2201 0.0058 0.050 Uiso 1 1 calc R . . C22 C 1.03413(5) 0.12700(4) -0.02142(3) 0.04261(18) Uani 1 1 d . . . H22A H 1.0398 0.1791 -0.0549 0.051 Uiso 1 1 calc R . . H22B H 0.9742 0.1395 0.0093 0.051 Uiso 1 1 calc R . . H22C H 1.0209 0.0820 -0.0432 0.051 Uiso 1 1 calc R . . C23 C 0.82532(4) -0.11957(3) 0.26044(2) 0.02688(14) Uani 1 1 d . . . C24 C 0.84107(4) -0.03705(3) 0.22931(2) 0.02704(14) Uani 1 1 d . . . C25 C 0.75436(4) 0.02022(3) 0.19595(2) 0.02936(14) Uani 1 1 d . . . H25 H 0.7648 0.0762 0.1743 0.035 Uiso 1 1 calc R . . C26 C 0.65309(4) -0.00214(4) 0.19346(2) 0.03036(15) Uani 1 1 d . . . C27 C 0.64162(4) -0.08548(3) 0.22448(2) 0.03150(15) Uani 1 1 d . . . H27 H 0.5734 -0.1022 0.2234 0.038 Uiso 1 1 calc R . . C28 C 0.72598(4) -0.14499(3) 0.25694(2) 0.02812(14) Uani 1 1 d . . . C29 C 0.71266(5) -0.23851(3) 0.28363(2) 0.03168(15) Uani 1 1 d . . . H29A H 0.7606 -0.2645 0.3219 0.038 Uiso 1 1 calc R . . H29B H 0.6370 -0.2408 0.2987 0.038 Uiso 1 1 calc R . . C30 C 0.55469(5) 0.06165(4) 0.16041(3) 0.03725(17) Uani 1 1 d . . . C31 C 0.50274(6) 0.02144(5) 0.11268(3) 0.0573(2) Uani 1 1 d . . . H31A H 0.4444 0.0640 0.0889 0.069 Uiso 1 1 calc R . . H31B H 0.4731 -0.0281 0.1377 0.069 Uiso 1 1 calc R . . H31C H 0.5574 0.0026 0.0808 0.069 Uiso 1 1 calc R . . C32 C 0.47261(6) 0.08325(5) 0.21408(4) 0.0582(2) Uani 1 1 d . . . H32A H 0.5075 0.1055 0.2462 0.070 Uiso 1 1 calc R . . H32B H 0.4455 0.0313 0.2366 0.070 Uiso 1 1 calc R . . H32C H 0.4122 0.1268 0.1938 0.070 Uiso 1 1 calc R . . C33 C 0.58571(6) 0.14566(4) 0.12180(3) 0.0494(2) Uani 1 1 d . . . H33A H 0.6204 0.1718 0.1515 0.059 Uiso 1 1 calc R . . H33B H 0.5206 0.1851 0.1034 0.059 Uiso 1 1 calc R . . H33C H 0.6361 0.1340 0.0857 0.059 Uiso 1 1 calc R . . C34 C 0.84334(4) -0.33560(3) 0.22264(2) 0.02786(14) Uani 1 1 d . . . C35 C 0.74156(4) -0.28804(3) 0.22916(2) 0.02823(14) Uani 1 1 d . . . C36 C 0.66468(4) -0.28141(3) 0.18101(3) 0.03008(15) Uani 1 1 d . . . H36 H 0.5936 -0.2514 0.1866 0.036 Uiso 1 1 calc R . . C37 C 0.68815(4) -0.31688(3) 0.12544(3) 0.02981(14) Uani 1 1 d . . . C38 C 0.79303(4) -0.36144(3) 0.11898(3) 0.03003(14) Uani 1 1 d . . . H38 H 0.8113 -0.3854 0.0810 0.036 Uiso 1 1 calc R . . C39 C 0.87266(4) -0.37216(3) 0.16679(2) 0.02690(13) Uani 1 1 d . . . C40 C 0.98253(4) -0.42359(3) 0.15874(3) 0.02927(14) Uani 1 1 d . . . H40A H 0.9745 -0.4697 0.1359 0.035 Uiso 1 1 calc R . . H40B H 1.0111 -0.4516 0.2033 0.035 Uiso 1 1 calc R . . C41 C 0.59813(4) -0.31018(4) 0.07673(3) 0.03355(15) Uani 1 1 d . . . C42 C 0.54102(5) -0.21654(4) 0.05505(3) 0.04121(18) Uani 1 1 d . . . H42A H 0.5124 -0.1944 0.0942 0.049 Uiso 1 1 calc R . . H42B H 0.4814 -0.2137 0.0256 0.049 Uiso 1 1 calc R . . H42C H 0.5928 -0.1818 0.0315 0.049 Uiso 1 1 calc R . . C43 C 0.51473(5) -0.36380(4) 0.11192(3) 0.04448(19) Uani 1 1 d . . . H43A H 0.5498 -0.4239 0.1257 0.053 Uiso 1 1 calc R . . H43B H 0.4561 -0.3597 0.0815 0.053 Uiso 1 1 calc R . . H43C H 0.4852 -0.3419 0.1509 0.053 Uiso 1 1 calc R . . C44 C 0.63883(5) -0.34282(4) 0.01494(3) 0.04551(19) Uani 1 1 d . . . H44A H 0.6920 -0.3092 -0.0082 0.055 Uiso 1 1 calc R . . H44B H 0.5780 -0.3369 -0.0143 0.055 Uiso 1 1 calc R . . H44C H 0.6728 -0.4034 0.0274 0.055 Uiso 1 1 calc R . . Zn2 Zn 0.061258(5) 0.876131(4) 0.434823(3) 0.03160(2) Uani 1 1 d . . . N1E N -0.08897(4) 0.85216(3) 0.43126(2) 0.02967(12) Uani 1 1 d D V -14 H1E1 H -0.0911 0.8249 0.3969 0.036 Uiso 1 1 calc R V -14 H1E2 H -0.1020 0.8144 0.4698 0.036 Uiso 1 1 calc R V -14 C1E C -0.17863(5) 0.92760(4) 0.42268(3) 0.03650(16) Uani 1 1 d D V -14 H1E1' H -0.1693 0.9661 0.3793 0.044 Uiso 1 1 calc R V -14 H1E2' H -0.1740 0.9599 0.4576 0.044 Uiso 1 1 calc R V -14 C2E C -0.28948(5) 0.90344(4) 0.42608(3) 0.03965(17) Uani 1 1 d D V -14 H2E1 H -0.3032 0.8723 0.4716 0.048 Uiso 1 1 calc R V -14 H2E2 H -0.2908 0.8640 0.3958 0.048 Uiso 1 1 calc R V -14 C3E C -0.37920(6) 0.98076(5) 0.40744(4) 0.0617(3) Uani 1 1 d D V -14 H3E1 H -0.3764 1.0209 0.4369 0.074 Uiso 1 1 calc R V -14 H3E2 H -0.3662 1.0110 0.3615 0.074 Uiso 1 1 calc R V -14 C4E C -0.49101(6) 0.95780(7) 0.41233(5) 0.0837(4) Uani 1 1 d D V -14 H4E1 H -0.4954 0.9196 0.3822 0.126 Uiso 1 1 calc R V -14 H4E2 H -0.5450 1.0103 0.4001 0.126 Uiso 1 1 calc R V -14 H4E3 H -0.5050 0.9286 0.4578 0.126 Uiso 1 1 calc R V -14 N1F N 0.16960(3) 0.82577(3) 0.37062(2) 0.02993(12) Uani 1 1 d D V -15 H1F1 H 0.1864 0.7673 0.3858 0.036 Uiso 1 1 calc R V -15 H1F2 H 0.1374 0.8357 0.3302 0.036 Uiso 1 1 calc R V -15 C1F C 0.27100(5) 0.86095(4) 0.36131(3) 0.04993(19) Uani 1 1 d D V -15 H1F1' H 0.3121 0.8418 0.4030 0.060 Uiso 1 1 calc R V -15 H1F2' H 0.2528 0.9244 0.3522 0.060 Uiso 1 1 calc R V -15 C2F C 0.34343(5) 0.83352(4) 0.30465(3) 0.04642(19) Uani 1 1 d D V -15 H2F1 H 0.3048 0.8577 0.2624 0.056 Uiso 1 1 calc R V -15 H2F2 H 0.4097 0.8589 0.3020 0.056 Uiso 1 1 calc R V -15 C3F C 0.37592(6) 0.73800(5) 0.31140(3) 0.0522(2) Uani 1 1 d D V -15 H3F1 H 0.3104 0.7130 0.3095 0.063 Uiso 1 1 calc R V -15 H3F2 H 0.4236 0.7265 0.2735 0.063 Uiso 1 1 calc R V -15 C4F C 0.43373(7) 0.69456(7) 0.37464(4) 0.0873(4) Uani 1 1 d D V -15 H4F1 H 0.4924 0.7245 0.3801 0.131 Uiso 1 1 calc R V -15 H4F2 H 0.4638 0.6348 0.3731 0.131 Uiso 1 1 calc R V -15 H4F3 H 0.3827 0.6960 0.4121 0.131 Uiso 1 1 calc R V -15 N1G N 0.09772(7) 0.83126(6) 0.52980(4) 0.0371(3) Uani 0.55 1 d PD V -1 H1G1 H 0.0664 0.8721 0.5530 0.044 Uiso 0.55 1 calc PR V -1 H1G2 H 0.0664 0.7835 0.5449 0.044 Uiso 0.55 1 calc PR V -1 C1G C 0.21608(9) 0.80732(7) 0.54617(5) 0.0402(3) Uani 0.55 1 d PD V -1 H1G1' H 0.2534 0.8560 0.5270 0.048 Uiso 0.55 1 calc PR V -1 H1G2' H 0.2498 0.7573 0.5274 0.048 Uiso 0.55 1 calc PR V -1 C2G C 0.22637(10) 0.78537(11) 0.62054(5) 0.0651(5) Uani 0.55 1 d PD V -1 H2G1 H 0.1501 0.7972 0.6356 0.078 Uiso 0.55 1 calc PR V -1 H2G2 H 0.2460 0.7220 0.6298 0.078 Uiso 0.55 1 calc PR V -1 C3G C 0.28527(14) 0.80787(11) 0.67365(8) 0.1032(7) Uani 0.55 1 d PD V -1 H3G1 H 0.2312 0.8463 0.6952 0.124 Uiso 0.55 1 calc PR V -1 H3G2 H 0.3377 0.8433 0.6505 0.124 Uiso 0.55 1 calc PR V -1 C4G C 0.34612(14) 0.74338(12) 0.72864(7) 0.1119(6) Uani 0.55 1 d PD V -1 H4G1 H 0.2975 0.7315 0.7668 0.168 Uiso 0.55 1 calc PR V -1 H4G2 H 0.4066 0.7665 0.7415 0.168 Uiso 0.55 1 calc PR V -1 H4G3 H 0.3740 0.6901 0.7135 0.168 Uiso 0.55 1 calc PR V -1 N1N N 0.11327(8) 0.80281(6) 0.52768(4) 0.0305(3) Uani 0.45 1 d PD V -2 H1N1 H 0.0521 0.7934 0.5525 0.037 Uiso 0.45 1 calc PR V -2 H1N2 H 0.1482 0.7502 0.5210 0.037 Uiso 0.45 1 calc PR V -2 C1N C 0.18325(11) 0.83153(8) 0.56896(6) 0.0412(4) Uani 0.45 1 d PD V -2 H1N1' H 0.1426 0.8859 0.5787 0.049 Uiso 0.45 1 calc PR V -2 H1N2' H 0.2456 0.8467 0.5405 0.049 Uiso 0.45 1 calc PR V -2 C2N C 0.22903(13) 0.77985(11) 0.63256(6) 0.0822(6) Uani 0.45 1 d PD V -2 H2N1 H 0.2102 0.7219 0.6393 0.099 Uiso 0.45 1 calc PR V -2 H2N2 H 0.1939 0.8066 0.6688 0.099 Uiso 0.45 1 calc PR V -2 C3N C 0.35426(11) 0.76969(10) 0.63853(6) 0.0571(5) Uani 0.45 1 d PD V -2 H3N1 H 0.3921 0.7146 0.6285 0.069 Uiso 0.45 1 calc PR V -2 H3N2 H 0.3826 0.8177 0.6089 0.069 Uiso 0.45 1 calc PR V -2 C4N C 0.3652(3) 0.7717(2) 0.71225(9) 0.2556(13) Uani 0.45 1 d PD V -2 H4N1 H 0.3881 0.8252 0.7154 0.383 Uiso 0.45 1 calc PR V -2 H4N2 H 0.4191 0.7227 0.7330 0.383 Uiso 0.45 1 calc PR V -2 H4N3 H 0.2952 0.7685 0.7350 0.383 Uiso 0.45 1 calc PR V -2 O1W O 0.93768(3) -0.35343(3) 0.406242(19) 0.04358(13) Uani 1 1 d . . . H1W H 0.9968(7) -0.3550(6) 0.4188(4) 0.088(3) Uiso 1 1 d . . . Cl1 Cl 1.168431(12) -0.369670(9) 0.461929(7) 0.03774(4) Uani 1 1 d . . . Cl2 Cl 0.067777(16) 1.016558(10) 0.413993(9) 0.05679(5) Uani 1 1 d . V . 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 N1A 0.00952(16) 0.00001(15) 0.00628(15) -0.00105(12) 0.00463(13) -0.00362(13) C1A 0.0191(2) 0.0089(2) 0.0099(2) -0.00046(16) -0.00212(18) -0.00231(18) C2A 0.0528(4) 0.0102(3) 0.0313(3) -0.0033(2) 0.0006(3) 0.0115(3) C3A 0.0524(4) 0.0455(4) 0.0456(4) -0.0206(3) 0.0008(4) -0.0129(3) C4A 0.0608(4) 0.0355(3) 0.0363(3) -0.0163(3) -0.0072(3) -0.0133(3) Cl3 0.04128(19) 0.02588(16) 0.02402(15) -0.00542(13) 0.00417(15) -0.00830(15) N1H 0.00952(16) 0.00001(15) 0.00628(15) -0.00105(12) 0.00463(13) -0.00362(13) C1H 0.0191(2) 0.0089(2) 0.0099(2) -0.00046(16) -0.00212(18) -0.00231(18) C2H 0.0528(4) 0.0102(3) 0.0313(3) -0.0033(2) 0.0006(3) 0.0115(3) C3H 0.0524(4) 0.0455(4) 0.0456(4) -0.0206(3) 0.0008(4) -0.0129(3) C4H 0.0608(4) 0.0355(3) 0.0363(3) -0.0163(3) -0.0072(3) -0.0133(3) Zn1 0.03684(3) 0.02920(3) 0.02651(3) -0.00556(2) -0.00049(2) -0.00837(2) N1B 0.0253(3) 0.0408(4) 0.0123(3) 0.0030(3) 0.0046(3) -0.0151(3) C1B 0.0321(4) 0.0443(5) 0.0253(4) 0.0005(4) -0.0082(4) -0.0101(4) C2B 0.0322(4) 0.0392(5) 0.0338(5) 0.0072(4) -0.0065(4) -0.0103(4) C3B 0.0552(6) 0.0572(6) 0.0291(5) 0.0014(4) -0.0120(4) -0.0224(5) C4B 0.0659(7) 0.0920(10) 0.0613(8) 0.0074(7) -0.0239(6) -0.0341(6) N1J 0.0595(7) 0.0301(6) 0.0694(8) -0.0083(5) -0.0125(6) 0.0006(6) C1J 0.0512(7) 0.0326(6) 0.0394(7) 0.0154(5) -0.0064(6) -0.0089(6) C2J 0.0432(7) 0.0417(7) 0.0318(6) 0.0009(5) -0.0038(5) -0.0075(6) C3J 0.0739(8) 0.0522(7) 0.0321(6) 0.0040(6) -0.0079(6) -0.0308(6) C4J 0.0501(7) 0.0859(12) 0.0604(9) 0.0161(9) -0.0252(7) -0.0248(7) N1C 0.0512(3) 0.0259(2) 0.02613(19) -0.00494(16) -0.00650(19) -0.00613(19) C1C 0.0583(3) 0.0497(3) 0.0351(3) -0.0054(2) 0.0050(3) -0.0279(2) C2C 0.0469(3) 0.0380(3) 0.0379(3) -0.0053(2) -0.0005(2) -0.0126(2) C3C 0.0868(5) 0.1317(6) 0.0683(4) -0.0522(4) 0.0311(4) -0.0523(4) C4C 0.0953(6) 0.1468(7) 0.0794(4) -0.0695(4) 0.0268(5) -0.0362(6) N1D 0.0350(3) 0.0217(3) 0.0095(2) -0.0003(2) -0.0087(2) -0.0032(2) C1D 0.0360(4) 0.0275(4) 0.0411(4) -0.0029(4) -0.0007(4) -0.0021(4) C2D 0.0270(4) 0.0501(6) 0.0641(6) -0.0133(5) 0.0082(4) -0.0016(4) C3D 0.0512(6) 0.0615(7) 0.0613(7) -0.0050(6) -0.0006(6) -0.0050(6) C4D 0.0614(8) 0.1023(12) 0.1060(12) -0.0074(10) 0.0137(8) -0.0222(8) N1K 0.0772(9) 0.0334(6) 0.0864(10) -0.0290(6) 0.0312(8) -0.0287(6) C1K 0.0926(11) 0.120(2) 0.0867(11) 0.0333(13) -0.0758(8) -0.0254(13) C2K 0.1132(18) 0.098(2) 0.229(4) 0.024(2) -0.076(2) -0.0479(15) C3K 0.0297(9) 0.196(3) 0.0931(17) -0.0233(19) -0.0038(11) 0.0391(14) C4K 0.1031(18) 0.0924(17) 0.0845(15) -0.0201(13) 0.0142(14) 0.0435(14) O1 0.03859(18) 0.02775(16) 0.02062(14) -0.00204(13) -0.00344(14) -0.00703(14) O2 0.03443(17) 0.02781(16) 0.02022(14) -0.00412(12) -0.00342(13) -0.00590(14) O3 0.03210(17) 0.03514(18) 0.02464(16) -0.00044(14) -0.00130(14) -0.00628(15) O4 0.03741(18) 0.03837(19) 0.02189(15) -0.00246(14) -0.00461(14) -0.00621(16) C1 0.0271(2) 0.0215(2) 0.0247(2) -0.00372(17) -0.00477(18) 0.00039(18) C2 0.0311(2) 0.0214(2) 0.0262(2) -0.00009(18) -0.00560(19) -0.00256(19) C3 0.0286(2) 0.0238(2) 0.0298(2) -0.00756(17) -0.00478(19) -0.00233(18) C4 0.0291(2) 0.0259(2) 0.0270(2) -0.00628(18) -0.00436(19) 0.0020(2) C5 0.0250(2) 0.0228(2) 0.0304(2) -0.00331(18) -0.00154(19) -0.00150(18) C6 0.0263(2) 0.0204(2) 0.0258(2) -0.00422(17) -0.00522(18) -0.00016(18) C7 0.0256(2) 0.0286(2) 0.0279(2) -0.00826(17) -0.00147(18) -0.00347(18) C8 0.0397(3) 0.0361(2) 0.0309(2) -0.01386(19) -0.0008(2) -0.0073(2) C9 0.0576(3) 0.0480(3) 0.0399(3) -0.0267(2) 0.0043(3) -0.0151(2) C10 0.0428(3) 0.0548(3) 0.0395(3) -0.0207(2) 0.0069(2) -0.0047(3) C11 0.0553(3) 0.0438(3) 0.0281(2) -0.0066(2) -0.0015(2) -0.0055(3) C12 0.0294(2) 0.0280(2) 0.02171(19) -0.00531(17) -0.00385(17) -0.00795(18) C13 0.0252(2) 0.0283(2) 0.0262(2) -0.00733(17) -0.00356(17) -0.00640(18) C14 0.0252(2) 0.0320(2) 0.0254(2) -0.00916(17) -0.00365(17) -0.00783(18) C15 0.0272(2) 0.0298(2) 0.0260(2) -0.00638(17) -0.00530(17) -0.00825(18) C16 0.0300(2) 0.0236(2) 0.0312(2) -0.00667(17) -0.00317(19) -0.00490(18) C17 0.0256(2) 0.0255(2) 0.0266(2) -0.00599(17) -0.00269(18) -0.00598(17) C18 0.0355(2) 0.0297(2) 0.0260(2) -0.01078(17) 0.00003(19) -0.0062(2) C19 0.0357(2) 0.0272(2) 0.0286(2) -0.00553(18) -0.0003(2) -0.0065(2) C20 0.0478(3) 0.0439(3) 0.0356(3) -0.0029(2) 0.0093(3) -0.0104(3) C21 0.0509(3) 0.0351(3) 0.0433(3) -0.0058(2) 0.0023(3) -0.0195(2) C22 0.0444(3) 0.0421(3) 0.0389(3) 0.0041(2) -0.0105(2) -0.0137(2) C23 0.0285(2) 0.0328(2) 0.01790(19) -0.00586(17) 0.00085(18) -0.0014(2) C24 0.0261(2) 0.0314(2) 0.0253(2) -0.01074(17) 0.00402(18) -0.00482(19) C25 0.0337(2) 0.0279(2) 0.0252(2) -0.00560(18) 0.0005(2) -0.0028(2) C26 0.0326(2) 0.0358(3) 0.0224(2) -0.00668(19) 0.00186(19) -0.0055(2) C27 0.0346(2) 0.0340(2) 0.0279(2) -0.00923(19) 0.0014(2) -0.0087(2) C28 0.0342(2) 0.0314(2) 0.02011(19) -0.00636(17) 0.00347(19) -0.00931(19) C29 0.0364(3) 0.0335(3) 0.0235(2) -0.00200(19) 0.0044(2) -0.0085(2) C30 0.0325(3) 0.0402(3) 0.0365(3) -0.0072(2) -0.0026(2) -0.0005(2) C31 0.0488(3) 0.0648(4) 0.0578(3) -0.0136(3) -0.0249(3) -0.0011(3) C32 0.0486(4) 0.0611(4) 0.0517(4) -0.0058(3) 0.0115(3) 0.0128(3) C33 0.0500(3) 0.0447(4) 0.0447(3) 0.0046(3) -0.0074(3) -0.0006(3) C34 0.0336(2) 0.0242(2) 0.0250(2) 0.00065(18) -0.00268(19) -0.00949(18) C35 0.0342(2) 0.0279(2) 0.0221(2) 0.00035(18) 0.00226(19) -0.01159(19) C36 0.0319(2) 0.0260(2) 0.0308(2) -0.00189(19) 0.0000(2) -0.0061(2) C37 0.0334(2) 0.0266(2) 0.0292(2) -0.00220(19) -0.0017(2) -0.00879(19) C38 0.0348(2) 0.0291(2) 0.0286(2) -0.00557(18) 0.0011(2) -0.01279(19) C39 0.0314(2) 0.0231(2) 0.0263(2) -0.00111(17) 0.00136(19) -0.01053(18) C40 0.0338(2) 0.0231(2) 0.0293(2) -0.00044(19) -0.0012(2) -0.00669(19) C41 0.0333(2) 0.0340(2) 0.0344(2) -0.0079(2) -0.0083(2) -0.0057(2) C42 0.0442(3) 0.0356(3) 0.0419(3) -0.0005(2) -0.0104(2) -0.0086(2) C43 0.0391(3) 0.0450(3) 0.0490(3) -0.0030(3) -0.0085(3) -0.0127(2) C44 0.0463(3) 0.0507(3) 0.0428(3) -0.0164(2) -0.0127(2) -0.0058(3) Zn2 0.04080(3) 0.02918(3) 0.02655(3) -0.00461(2) 0.00099(2) -0.01254(2) N1E 0.0411(2) 0.02497(19) 0.02312(18) -0.00327(15) -0.00152(17) -0.00806(17) C1E 0.0497(3) 0.0293(2) 0.0307(2) -0.0062(2) 0.0003(2) -0.0079(2) C2E 0.0430(3) 0.0423(3) 0.0365(3) -0.0131(2) 0.0015(2) -0.0098(2) C3E 0.0518(4) 0.0588(4) 0.0723(4) -0.0143(3) -0.0170(3) 0.0007(3) C4E 0.0492(4) 0.1101(7) 0.0932(6) -0.0318(5) -0.0099(4) -0.0033(5) N1F 0.0322(2) 0.0306(2) 0.02835(19) -0.00457(16) -0.00219(17) -0.01072(16) C1F 0.0516(3) 0.0653(3) 0.0464(3) -0.0250(2) 0.0048(3) -0.0308(2) C2F 0.0391(3) 0.0587(3) 0.0468(3) -0.0164(3) 0.0054(3) -0.0179(3) C3F 0.0419(3) 0.0685(4) 0.0443(3) -0.0145(3) -0.0005(3) -0.0022(3) C4F 0.0579(5) 0.1063(7) 0.0705(5) 0.0265(5) -0.0072(4) 0.0030(5) N1G 0.0465(4) 0.0326(4) 0.0356(4) -0.0105(3) -0.0045(4) -0.0109(3) C1G 0.0486(6) 0.0404(5) 0.0295(4) -0.0081(4) -0.0029(4) -0.0013(5) C2G 0.0486(6) 0.1052(11) 0.0381(5) -0.0095(6) -0.0239(5) -0.0052(7) C3G 0.1215(12) 0.0776(10) 0.1208(13) -0.0157(9) -0.0455(10) -0.0372(8) C4G 0.1302(10) 0.1191(11) 0.0899(6) -0.0608(6) -0.0858(6) 0.0394(9) N1N 0.0433(5) 0.0270(4) 0.0208(4) -0.0042(3) -0.0019(4) -0.0058(4) C1N 0.0517(7) 0.0357(6) 0.0394(6) -0.0108(5) -0.0027(6) -0.0125(5) C2N 0.1123(12) 0.0891(8) 0.0411(5) -0.0532(5) -0.0395(6) 0.0506(9) C3N 0.0735(9) 0.0462(8) 0.0488(7) -0.0055(6) -0.0356(6) 0.0015(7) C4N 0.521(3) 0.162(2) 0.1098(10) 0.0576(12) -0.2143(10) -0.1670(18) O1W 0.0478(2) 0.0512(2) 0.02859(18) 0.00074(17) -0.00099(17) -0.01164(19) Cl1 0.05084(7) 0.03079(6) 0.03224(6) -0.00423(5) -0.00229(5) -0.01133(5) Cl2 0.08266(10) 0.03264(6) 0.06096(9) -0.01491(6) 0.02371(8) -0.02657(6) _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 N1A C1A 1.3320(7) . ? C1A C2A 1.4580(9) . ? C2A C3A 1.5005(10) . ? C3A C4A 1.5489(13) . ? N1H C1H 1.4673(12) . ? C1H C2H 1.5160(17) . ? C2H C3H 1.5174(15) . ? C3H C4H 1.5055(17) . ? N1B C1B 1.5040(13) . ? C1B C2B 1.4972(13) . ? C2B C3B 1.5371(16) . ? C3B C4B 1.5306(16) . ? N1J C1J 1.515(2) . ? C1J C2J 1.4958(17) . ? C2J C3J 1.538(2) . ? C3J C4J 1.5292(19) . ? N1C C1C 1.4664(8) . ? C1C C2C 1.5195(10) . ? C2C C3C 1.4714(11) . ? C3C C4C 1.4591(15) . ? N1D C1D 1.5035(10) . ? C1D C2D 1.5111(13) . ? C2D C3D 1.4971(18) . ? C3D C4D 1.5411(18) . ? N1K C1K 1.500(2) . ? C1K C2K 1.512(3) . ? C2K C3K 1.534(3) . ? C3K C4K 1.531(4) . ? O1 C1 1.3754(6) . ? O2 C12 1.3684(6) . ? O3 C23 1.3619(6) . ? O4 C34 1.3740(7) . ? C1 C6 1.4012(7) . ? C1 C2 1.4050(8) . ? C2 C3 1.3941(7) . ? C2 C40 1.5193(7) . ? C3 C4 1.3839(7) . ? C4 C5 1.3987(8) . ? C4 C8 1.5349(8) . ? C5 C6 1.3868(7) . ? C6 C7 1.5092(8) . ? C7 C13 1.5229(7) . ? C8 C11 1.5242(8) . ? C8 C10 1.5289(9) . ? C8 C9 1.5374(10) . ? C12 C13 1.4005(7) . ? C12 C17 1.4016(7) . ? C13 C14 1.3957(7) . ? C14 C15 1.3869(7) . ? C15 C16 1.3968(7) . ? C15 C19 1.5370(7) . ? C16 C17 1.3930(7) . ? C17 C18 1.5184(7) . ? C18 C24 1.5341(8) . ? C19 C20 1.5191(8) . ? C19 C22 1.5319(8) . ? C19 C21 1.5391(9) . ? C23 C28 1.3973(8) . ? C23 C24 1.3975(7) . ? C24 C25 1.3990(7) . ? C25 C26 1.3948(8) . ? C26 C27 1.3938(8) . ? C26 C30 1.5431(7) . ? C27 C28 1.3876(7) . ? C28 C29 1.5333(8) . ? C29 C35 1.5132(8) . ? C30 C32 1.5274(9) . ? C30 C33 1.5279(9) . ? C30 C31 1.5290(11) . ? C34 C35 1.3833(7) . ? C34 C39 1.4122(8) . ? C35 C36 1.4005(8) . ? C36 C37 1.3887(8) . ? C37 C38 1.3970(7) . ? C37 C41 1.5311(8) . ? C38 C39 1.4082(8) . ? C39 C40 1.4976(7) . ? C41 C44 1.5167(9) . ? C41 C42 1.5351(8) . ? C41 C43 1.5381(9) . ? Zn2 N1G 1.9889(8) . ? Zn2 N1E 2.0078(5) . ? Zn2 N1F 2.0378(5) . ? Zn2 N1N 2.0948(9) . ? Zn2 Cl2 2.2391(3) . ? N1E C1E 1.4889(7) . ? C1E C2E 1.5114(9) . ? C2E C3E 1.5190(9) . ? C3E C4E 1.5136(12) . ? N1F C1F 1.4784(8) . ? C1F C2F 1.5373(9) . ? C2F C3F 1.5042(10) . ? C3F C4F 1.5004(11) . ? N1G C1G 1.5061(14) . ? C1G C2G 1.5094(14) . ? C2G C3G 1.502(2) . ? C3G C4G 1.502(2) . ? N1N C1N 1.4596(18) . ? C1N C2N 1.4799(17) . ? C2N C3N 1.563(2) . ? C3N C4N 1.547(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1A C1A C2A 117.20(5) . . ? C1A C2A C3A 118.89(6) . . ? C2A C3A C4A 109.96(7) . . ? N1H C1H C2H 112.91(9) . . ? C1H C2H C3H 114.37(11) . . ? C4H C3H C2H 112.12(12) . . ? C2B C1B N1B 116.84(8) . . ? C1B C2B C3B 112.06(8) . . ? C4B C3B C2B 112.27(10) . . ? C2J C1J N1J 111.38(11) . . ? C1J C2J C3J 108.12(11) . . ? C4J C3J C2J 109.93(12) . . ? N1C C1C C2C 111.56(6) . . ? C3C C2C C1C 114.82(7) . . ? C4C C3C C2C 116.83(9) . . ? N1D C1D C2D 113.64(7) . . ? C3D C2D C1D 110.35(9) . . ? C2D C3D C4D 111.94(11) . . ? N1K C1K C2K 111.46(17) . . ? C1K C2K C3K 113.0(2) . . ? C4K C3K C2K 109.32(19) . . ? O1 C1 C6 120.29(5) . . ? O1 C1 C2 119.28(4) . . ? C6 C1 C2 120.41(5) . . ? C3 C2 C1 118.41(5) . . ? C3 C2 C40 119.43(5) . . ? C1 C2 C40 122.15(5) . . ? C4 C3 C2 123.02(5) . . ? C3 C4 C5 116.60(5) . . ? C3 C4 C8 123.54(5) . . ? C5 C4 C8 119.86(5) . . ? C6 C5 C4 123.13(5) . . ? C5 C6 C1 118.36(5) . . ? C5 C6 C7 120.91(4) . . ? C1 C6 C7 120.72(5) . . ? C6 C7 C13 114.20(4) . . ? C11 C8 C10 109.38(5) . . ? C11 C8 C4 109.19(5) . . ? C10 C8 C4 110.59(5) . . ? C11 C8 C9 108.43(5) . . ? C10 C8 C9 108.26(5) . . ? C4 C8 C9 110.94(5) . . ? O2 C12 C13 119.71(4) . . ? O2 C12 C17 120.17(4) . . ? C13 C12 C17 120.11(4) . . ? C14 C13 C12 119.38(4) . . ? C14 C13 C7 120.16(4) . . ? C12 C13 C7 120.45(4) . . ? C15 C14 C13 122.25(4) . . ? C14 C15 C16 116.72(4) . . ? C14 C15 C19 123.10(4) . . ? C16 C15 C19 120.18(4) . . ? C17 C16 C15 123.42(4) . . ? C16 C17 C12 118.10(4) . . ? C16 C17 C18 119.96(4) . . ? C12 C17 C18 121.92(4) . . ? C17 C18 C24 116.05(5) . . ? C20 C19 C22 108.68(5) . . ? C20 C19 C15 112.40(4) . . ? C22 C19 C15 110.18(5) . . ? C20 C19 C21 107.35(5) . . ? C22 C19 C21 108.95(5) . . ? C15 C19 C21 109.19(5) . . ? O3 C23 C28 117.92(5) . . ? O3 C23 C24 121.32(5) . . ? C28 C23 C24 120.72(4) . . ? C23 C24 C25 118.53(5) . . ? C23 C24 C18 121.12(4) . . ? C25 C24 C18 120.33(5) . . ? C26 C25 C24 122.18(5) . . ? C27 C26 C25 117.23(5) . . ? C27 C26 C30 119.76(5) . . ? C25 C26 C30 122.98(5) . . ? C28 C27 C26 122.56(5) . . ? C27 C28 C23 118.71(5) . . ? C27 C28 C29 120.37(5) . . ? C23 C28 C29 120.75(4) . . ? C35 C29 C28 108.96(4) . . ? C32 C30 C33 107.74(6) . . ? C32 C30 C31 109.63(6) . . ? C33 C30 C31 108.43(5) . . ? C32 C30 C26 108.93(5) . . ? C33 C30 C26 112.19(5) . . ? C31 C30 C26 109.87(5) . . ? O4 C34 C35 120.33(5) . . ? O4 C34 C39 118.20(4) . . ? C35 C34 C39 121.46(5) . . ? C34 C35 C36 118.45(5) . . ? C34 C35 C29 122.53(5) . . ? C36 C35 C29 118.90(5) . . ? C37 C36 C35 122.69(5) . . ? C36 C37 C38 117.34(5) . . ? C36 C37 C41 119.40(5) . . ? C38 C37 C41 123.17(5) . . ? C37 C38 C39 122.36(5) . . ? C38 C39 C34 117.57(4) . . ? C38 C39 C40 120.13(5) . . ? C34 C39 C40 122.25(5) . . ? C39 C40 C2 116.04(4) . . ? C44 C41 C37 113.07(5) . . ? C44 C41 C42 107.94(5) . . ? C37 C41 C42 110.46(5) . . ? C44 C41 C43 108.38(6) . . ? C37 C41 C43 108.39(4) . . ? C42 C41 C43 108.48(5) . . ? N1G Zn2 N1E 102.57(3) . . ? N1G Zn2 N1F 114.34(3) . . ? N1E Zn2 N1F 114.80(2) . . ? N1G Zn2 N1N 13.08(4) . . ? N1E Zn2 N1N 102.28(3) . . ? N1F Zn2 N1N 103.42(3) . . ? N1G Zn2 Cl2 106.19(3) . . ? N1E Zn2 Cl2 113.150(13) . . ? N1F Zn2 Cl2 105.673(15) . . ? N1N Zn2 Cl2 117.48(3) . . ? C1E N1E Zn2 116.68(4) . . ? N1E C1E C2E 113.34(5) . . ? C1E C2E C3E 112.87(5) . . ? C4E C3E C2E 113.50(7) . . ? C1F N1F Zn2 114.36(4) . . ? N1F C1F C2F 113.54(6) . . ? C3F C2F C1F 114.67(5) . . ? C4F C3F C2F 112.97(7) . . ? C1G N1G Zn2 116.73(6) . . ? N1G C1G C2G 108.38(8) . . ? C3G C2G C1G 139.56(14) . . ? C2G C3G C4G 124.52(16) . . ? C1N N1N Zn2 122.10(7) . . ? N1N C1N C2N 124.49(12) . . ? C1N C2N C3N 115.47(12) . . ? C4N C3N C2N 101.55(16) . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 28.78 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 3.452 _refine_diff_density_min -0.733 _refine_diff_density_rms 0.123 data_compound_4_(pob34) _database_code_depnum_ccdc_archive 'CCDC 192204' _audit_creation_method SHELXL-97 _chemical_name_systematic ; t-butyl-calix[4]arene*(Ag(isopropylamine)3) ; _chemical_name_common t-butyl-calix[4]arene*(Ag(isopropylamine)3) _chemical_melting_point ? _chemical_formula_moiety 'C44H56O4 C3H7NH2' _chemical_formula_sum 'C120 H149.50 Ag2 N7 O10' _chemical_formula_weight 2065.71 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 22.133(3) _cell_length_b 20.811(3) _cell_length_c 23.420(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.438(2) _cell_angle_gamma 90.00 _cell_volume 10492(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.5 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.2 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4370 _exptl_absorpt_coefficient_mu 0.437 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 63280 _diffrn_reflns_av_R_equivalents 0.0966 _diffrn_reflns_av_sigmaI/netI 0.0598 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.33 _diffrn_reflns_theta_max 21.15 _reflns_number_total 63527 _reflns_number_gt 34885 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.1234P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 63527 _refine_ls_number_parameters 1250 _refine_ls_number_restraints 66 _refine_ls_R_factor_all 0.1480 _refine_ls_R_factor_gt 0.0771 _refine_ls_wR_factor_ref 0.2342 _refine_ls_wR_factor_gt 0.1916 _refine_ls_goodness_of_fit_ref 0.979 _refine_ls_restrained_S_all 0.980 _refine_ls_shift/su_max 6.033 _refine_ls_shift/su_mean 0.200 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 Ag1 Ag 0.392745(15) 0.314610(16) 0.260075(14) 0.07214(11) Uani 0.8951(4) 1 d P . . Ag2 Ag 0.115208(16) 0.046711(18) 0.275625(17) 0.08540(13) Uani 0.87 1 d P . . Ag01 Ag 0.14183(16) 0.08014(15) 0.27511(13) 0.0983(12) Uani 0.1049(4) 1 d P A -3 Ag02 Ag 0.37979(13) 0.34856(14) 0.25950(13) 0.0339(7) Uiso 0.08 1 d P B -3 Ag03 Ag 0.3577(4) 0.2805(4) 0.2734(4) 0.0339(7) Uiso 0.03 1 d P B -3 O1 O 0.37664(9) 0.13774(8) 0.21272(8) 0.0509(6) Uani 1 1 d . . . O2 O 0.40618(10) 0.13731(9) 0.32270(9) 0.0543(7) Uani 1 1 d . . . O3 O 0.31326(9) 0.06346(9) 0.33661(10) 0.0613(7) Uani 1 1 d . . . O4 O 0.28363(10) 0.06301(10) 0.20834(10) 0.0623(8) Uani 1 1 d . . . O5 O 0.10435(9) 0.23901(9) 0.20172(9) 0.0550(7) Uani 1 1 d . . . O6 O 0.14278(9) 0.22924(10) 0.31379(9) 0.0642(7) Uani 1 1 d . . . O7 O 0.23654(10) 0.31526(9) 0.31339(9) 0.0604(7) Uani 1 1 d . . . O8 O 0.18632(9) 0.31940(9) 0.19547(9) 0.0594(7) Uani 1 1 d . . . C1 C 0.42152(14) 0.11839(13) 0.18556(13) 0.0455(9) Uani 1 1 d . . . C2 C 0.40715(14) 0.07991(14) 0.13601(13) 0.0485(10) Uani 1 1 d . . . C3 C 0.45499(16) 0.06032(14) 0.11111(13) 0.0579(11) Uani 1 1 d . . . H3 H 0.4446 0.0343 0.0769 0.069 Uiso 1 1 calc R . . C4 C 0.51727(15) 0.07608(14) 0.13277(14) 0.0524(10) Uani 1 1 d . . . C5 C 0.52908(14) 0.11463(12) 0.18267(13) 0.0462(10) Uani 1 1 d . . . H5 H 0.5708 0.1266 0.1996 0.055 Uiso 1 1 calc R . . C6 C 0.48246(14) 0.13656(12) 0.20895(12) 0.0401(9) Uani 1 1 d . . . C7 C 0.56717(16) 0.05448(16) 0.10337(15) 0.0672(11) Uani 1 1 d . . . C8 C 0.34122(15) 0.05890(15) 0.10934(13) 0.0601(11) Uani 1 1 d . C . H8A H 0.3374 0.0498 0.0672 0.072 Uiso 1 1 calc R . . H8B H 0.3129 0.0950 0.1121 0.072 Uiso 1 1 calc R . . C9 C 0.5649(2) -0.01908(16) 0.09399(19) 0.1092(16) Uani 1 1 d . . . H9A H 0.5985 -0.0321 0.0756 0.164 Uiso 1 1 calc R . . H9B H 0.5248 -0.0311 0.0685 0.164 Uiso 1 1 calc R . . H9C H 0.5700 -0.0407 0.1320 0.164 Uiso 1 1 calc R . . C10 C 0.63259(18) 0.0729(2) 0.13786(19) 0.1106(17) Uani 1 1 d . . . H10A H 0.6633 0.0568 0.1172 0.166 Uiso 1 1 calc R . . H10B H 0.6404 0.0539 0.1772 0.166 Uiso 1 1 calc R . . H10C H 0.6358 0.1198 0.1412 0.166 Uiso 1 1 calc R . . C11 C 0.55778(19) 0.08777(18) 0.04327(16) 0.0990(15) Uani 1 1 d . . . H11A H 0.5903 0.0739 0.0239 0.149 Uiso 1 1 calc R . . H11B H 0.5601 0.1345 0.0488 0.149 Uiso 1 1 calc R . . H11C H 0.5170 0.0762 0.0188 0.149 Uiso 1 1 calc R . . C21 C 0.46464(13) 0.11858(12) 0.34577(13) 0.0401(9) Uani 1 1 d . . . C22 C 0.51270(14) 0.13707(12) 0.31986(12) 0.0429(9) Uani 1 1 d . . . C23 C 0.57269(14) 0.11558(12) 0.34349(12) 0.0443(9) Uani 1 1 d . . . H23 H 0.6051 0.1283 0.3255 0.053 Uiso 1 1 calc R . . C24 C 0.58702(14) 0.07600(14) 0.39269(13) 0.0443(9) Uani 1 1 d . . . C25 C 0.53996(14) 0.06122(13) 0.41898(13) 0.0475(10) Uani 1 1 d . . . H25 H 0.5491 0.0362 0.4539 0.057 Uiso 1 1 calc R . . C26 C 0.47853(14) 0.08148(13) 0.39648(12) 0.0423(9) Uani 1 1 d . . . C27 C 0.65363(15) 0.05234(16) 0.41809(14) 0.0619(11) Uani 1 1 d . . . C28 C 0.50095(14) 0.17665(13) 0.26420(12) 0.0506(10) Uani 1 1 d . . . H28A H 0.5390 0.2011 0.2631 0.061 Uiso 1 1 calc R . . H28B H 0.4676 0.2081 0.2649 0.061 Uiso 1 1 calc R . . C29 C 0.6500(2) -0.01861(19) 0.4368(2) 0.138(2) Uani 1 1 d . . . H29A H 0.6297 -0.0443 0.4026 0.208 Uiso 1 1 calc R . . H29B H 0.6259 -0.0214 0.4669 0.208 Uiso 1 1 calc R . . H29C H 0.6920 -0.0351 0.4526 0.208 Uiso 1 1 calc R . . C30 C 0.6839(2) 0.0886(2) 0.47030(19) 0.149(2) Uani 1 1 d . . . H30A H 0.6579 0.0877 0.4989 0.224 Uiso 1 1 calc R . . H30B H 0.6898 0.1332 0.4593 0.224 Uiso 1 1 calc R . . H30C H 0.7244 0.0693 0.4877 0.224 Uiso 1 1 calc R . . C31 C 0.69359(17) 0.0529(2) 0.37426(17) 0.1062(17) Uani 1 1 d . . . H31A H 0.6731 0.0285 0.3394 0.159 Uiso 1 1 calc R . . H31B H 0.7339 0.0333 0.3918 0.159 Uiso 1 1 calc R . . H31C H 0.6999 0.0973 0.3631 0.159 Uiso 1 1 calc R . . C41 C 0.34074(14) 0.00441(14) 0.35164(13) 0.0468(10) Uani 1 1 d . . . C42 C 0.39449(13) 0.00048(13) 0.39579(12) 0.0433(9) Uani 1 1 d . . . C43 C 0.41868(14) -0.05998(13) 0.41153(12) 0.0477(10) Uani 1 1 d . . . H43 H 0.4556 -0.0634 0.4417 0.057 Uiso 1 1 calc R . . C44 C 0.39115(14) -0.11623(13) 0.38493(12) 0.0454(9) Uani 1 1 d . . . C45 C 0.33866(14) -0.10993(13) 0.34157(13) 0.0477(10) Uani 1 1 d . . . H45 H 0.3193 -0.1477 0.3230 0.057 Uiso 1 1 calc R . . C46 C 0.31172(13) -0.05011(14) 0.32294(13) 0.0463(10) Uani 1 1 d . . . C47 C 0.41815(16) -0.18413(15) 0.40350(14) 0.0628(11) Uani 1 1 d . . . C48 C 0.42781(14) 0.05911(13) 0.42545(13) 0.0484(10) Uani 1 1 d . . . H48A H 0.4463 0.0491 0.4672 0.058 Uiso 1 1 calc R . . H48B H 0.3974 0.0943 0.4242 0.058 Uiso 1 1 calc R . . C49 C 0.4825(2) -0.18034(19) 0.4442(2) 0.129(2) Uani 1 1 d . . . H49A H 0.4979 -0.2239 0.4551 0.194 Uiso 1 1 calc R . . H49B H 0.4803 -0.1563 0.4797 0.194 Uiso 1 1 calc R . . H49C H 0.5108 -0.1584 0.4241 0.194 Uiso 1 1 calc R . . C50 C 0.3780(2) -0.21733(18) 0.4355(2) 0.1552(19) Uani 1 1 d . . . H50A H 0.3950 -0.2601 0.4473 0.233 Uiso 1 1 calc R . . H50B H 0.3362 -0.2217 0.4102 0.233 Uiso 1 1 calc R . . H50C H 0.3759 -0.1925 0.4706 0.233 Uiso 1 1 calc R . . C51 C 0.4262(2) -0.22146(17) 0.35135(17) 0.1253(19) Uani 1 1 d . . . H51A H 0.4431 -0.2640 0.3640 0.188 Uiso 1 1 calc R . . H51B H 0.4549 -0.1986 0.3323 0.188 Uiso 1 1 calc R . . H51C H 0.3859 -0.2263 0.3236 0.188 Uiso 1 1 calc R . . C61 C 0.29487(14) 0.00375(15) 0.18678(14) 0.0510(10) Uani 1 1 d . C . C62 C 0.27722(12) -0.05065(14) 0.21338(14) 0.0489(10) Uani 1 1 d . . . C63 C 0.28617(14) -0.10916(15) 0.18861(15) 0.0579(11) Uani 1 1 d . C . H63 H 0.2746 -0.1468 0.2064 0.070 Uiso 1 1 calc R . . C64 C 0.31065(14) -0.11694(13) 0.14016(14) 0.0567(11) Uani 1 1 d D . . C65 C 0.32844(14) -0.06124(15) 0.11551(14) 0.0584(11) Uani 1 1 d . C . H65 H 0.3468 -0.0645 0.0828 0.070 Uiso 1 1 calc R . . C66 C 0.31982(15) -0.00049(15) 0.13798(14) 0.0530(11) Uani 1 1 d . . . C68 C 0.25719(13) -0.04687(15) 0.27055(13) 0.0528(10) Uani 1 1 d . . . H68A H 0.2284 -0.0828 0.2726 0.063 Uiso 1 1 calc R . . H68B H 0.2345 -0.0061 0.2719 0.063 Uiso 1 1 calc R . . C67A C 0.3202(3) -0.1814(3) 0.1131(2) 0.0738(13) Uani 0.632(3) 1 d PD C -1 C69 C 0.3625(3) -0.2213(3) 0.1625(2) 0.112(3) Uani 0.632(3) 1 d PD C -1 H69A H 0.3692 -0.2640 0.1475 0.168 Uiso 0.632(3) 1 calc PR C -1 H69B H 0.3425 -0.2257 0.1955 0.168 Uiso 0.632(3) 1 calc PR C -1 H69C H 0.4025 -0.1994 0.1758 0.168 Uiso 0.632(3) 1 calc PR C -1 C70 C 0.2562(2) -0.2132(3) 0.0908(3) 0.091(3) Uani 0.632(3) 1 d PD C -1 H70A H 0.2615 -0.2550 0.0735 0.137 Uiso 0.632(3) 1 calc PR C -1 H70B H 0.2302 -0.1856 0.0611 0.137 Uiso 0.632(3) 1 calc PR C -1 H70C H 0.2363 -0.2190 0.1237 0.137 Uiso 0.632(3) 1 calc PR C -1 C71 C 0.3515(3) -0.1782(3) 0.0612(2) 0.108(3) Uani 0.632(3) 1 d PD C -1 H71A H 0.3547 -0.2216 0.0460 0.162 Uiso 0.632(3) 1 calc PR C -1 H71B H 0.3931 -0.1597 0.0743 0.162 Uiso 0.632(3) 1 calc PR C -1 H71C H 0.3266 -0.1513 0.0301 0.162 Uiso 0.632(3) 1 calc PR C -1 C67B C 0.3163(4) -0.1855(4) 0.1167(4) 0.0738(13) Uani 0.368(3) 1 d PD C -2 C72 C 0.3856(3) -0.2016(4) 0.1198(5) 0.092(5) Uani 0.368(3) 1 d PD C -2 H72A H 0.4106 -0.1915 0.1591 0.138 Uiso 0.368(3) 1 calc PR C -2 H72B H 0.4002 -0.1761 0.0905 0.138 Uiso 0.368(3) 1 calc PR C -2 H72C H 0.3896 -0.2474 0.1117 0.138 Uiso 0.368(3) 1 calc PR C -2 C73 C 0.2909(5) -0.2402(4) 0.1500(4) 0.118(5) Uani 0.368(3) 1 d PD C -2 H73A H 0.3162 -0.2430 0.1903 0.177 Uiso 0.368(3) 1 calc PR C -2 H73B H 0.2930 -0.2812 0.1298 0.177 Uiso 0.368(3) 1 calc PR C -2 H73C H 0.2477 -0.2310 0.1508 0.177 Uiso 0.368(3) 1 calc PR C -2 C74 C 0.2795(4) -0.1878(4) 0.0519(3) 0.100(4) Uani 0.368(3) 1 d PD C -2 H74A H 0.2854 -0.2298 0.0351 0.150 Uiso 0.368(3) 1 calc PR C -2 H74B H 0.2946 -0.1540 0.0296 0.150 Uiso 0.368(3) 1 calc PR C -2 H74C H 0.2352 -0.1812 0.0500 0.150 Uiso 0.368(3) 1 calc PR C -2 C81 C 0.04532(13) 0.25903(13) 0.18187(13) 0.0419(9) Uani 1 1 d . . . C82 C 0.02949(14) 0.29870(14) 0.13222(13) 0.0457(10) Uani 1 1 d . . . C83 C -0.03262(13) 0.31715(14) 0.11321(12) 0.0485(10) Uani 1 1 d . . . H83 H -0.0434 0.3444 0.0798 0.058 Uiso 1 1 calc R . . C84 C -0.07960(14) 0.29841(14) 0.13971(13) 0.0442(9) Uani 1 1 d . . . C85 C -0.06144(13) 0.25986(13) 0.18828(13) 0.0427(9) Uani 1 1 d . . . H85 H -0.0920 0.2464 0.2083 0.051 Uiso 1 1 calc R . . C86 C -0.00034(14) 0.23955(12) 0.20961(12) 0.0427(9) Uani 1 1 d . . . C87 C -0.14671(14) 0.31717(15) 0.11434(13) 0.0535(10) Uani 1 1 d . . . C88 C 0.07777(15) 0.32134(15) 0.10137(12) 0.0546(10) Uani 1 1 d . D . H88A H 0.0574 0.3294 0.0597 0.066 Uiso 1 1 calc R . . H88B H 0.1083 0.2864 0.1024 0.066 Uiso 1 1 calc R . . C89 C -0.19063(16) 0.29586(18) 0.15259(15) 0.0827(14) Uani 1 1 d . . . H89A H -0.2331 0.3091 0.1340 0.124 Uiso 1 1 calc R . . H89B H -0.1778 0.3158 0.1914 0.124 Uiso 1 1 calc R . . H89C H -0.1890 0.2490 0.1568 0.124 Uiso 1 1 calc R . . C90 C -0.16908(15) 0.28735(15) 0.05417(13) 0.0649(12) Uani 1 1 d . . . H90A H -0.2125 0.2994 0.0380 0.097 Uiso 1 1 calc R . . H90B H -0.1658 0.2405 0.0574 0.097 Uiso 1 1 calc R . . H90C H -0.1434 0.3029 0.0281 0.097 Uiso 1 1 calc R . . C91 C -0.15186(16) 0.39145(14) 0.10772(15) 0.0739(13) Uani 1 1 d . . . H91A H -0.1953 0.4034 0.0914 0.111 Uiso 1 1 calc R . . H91B H -0.1263 0.4061 0.0813 0.111 Uiso 1 1 calc R . . H91C H -0.1373 0.4116 0.1463 0.111 Uiso 1 1 calc R . . C101 C 0.10041(14) 0.25156(14) 0.34227(13) 0.0473(10) Uani 1 1 d . . . C102 C 0.03732(14) 0.23749(12) 0.32161(13) 0.0457(9) Uani 1 1 d . . . C103 C -0.00506(14) 0.26291(13) 0.35115(13) 0.0497(10) Uani 1 1 d . . . H103 H -0.0480 0.2549 0.3358 0.060 Uiso 1 1 calc R . . C104 C 0.01233(15) 0.29916(14) 0.40165(14) 0.0532(10) Uani 1 1 d . . . C105 C 0.07526(15) 0.31073(14) 0.42112(13) 0.0551(10) Uani 1 1 d . . . H105 H 0.0889 0.3353 0.4559 0.066 Uiso 1 1 calc R . . C106 C 0.11887(15) 0.28868(14) 0.39304(14) 0.0515(10) Uani 1 1 d . . . C107 C -0.03364(17) 0.32690(17) 0.43481(16) 0.0782(13) Uani 1 1 d . . . C108 C 0.01511(14) 0.19828(13) 0.26533(12) 0.0497(10) Uani 1 1 d . . . H10D H -0.0223 0.1736 0.2682 0.060 Uiso 1 1 calc R . . H10E H 0.0478 0.1670 0.2620 0.060 Uiso 1 1 calc R . . C109 C -0.02151(18) 0.39868(16) 0.44697(17) 0.0887(14) Uani 1 1 d . . . H10F H -0.0507 0.4153 0.4691 0.133 Uiso 1 1 calc R . . H10G H -0.0272 0.4219 0.4097 0.133 Uiso 1 1 calc R . . H10H H 0.0211 0.4048 0.4699 0.133 Uiso 1 1 calc R . . C110 C -0.0252(2) 0.29149(19) 0.49382(18) 0.1246(17) Uani 1 1 d . . . H11D H -0.0543 0.3088 0.5156 0.187 Uiso 1 1 calc R . . H11E H 0.0175 0.2976 0.5168 0.187 Uiso 1 1 calc R . . H11F H -0.0332 0.2455 0.4866 0.187 Uiso 1 1 calc R . . C111 C -0.0995(2) 0.3186(2) 0.4019(2) 0.144(2) Uani 1 1 d . . . H11G H -0.1272 0.3360 0.4251 0.216 Uiso 1 1 calc R . . H11H H -0.1083 0.2728 0.3945 0.216 Uiso 1 1 calc R . . H11I H -0.1062 0.3416 0.3644 0.216 Uiso 1 1 calc R . . C121 C 0.22087(13) 0.37209(14) 0.33574(13) 0.0454(10) Uani 1 1 d . D . C122 C 0.19954(14) 0.37103(15) 0.38681(13) 0.0497(10) Uani 1 1 d . . . C123 C 0.18578(15) 0.42895(16) 0.40986(15) 0.0675(12) Uani 1 1 d . D . H123 H 0.1713 0.4287 0.4450 0.081 Uiso 1 1 calc R . . C124 C 0.19237(15) 0.48723(14) 0.38349(15) 0.0663(12) Uani 1 1 d D . . C125 C 0.21344(14) 0.48523(15) 0.33266(15) 0.0570(11) Uani 1 1 d . D . H125 H 0.2179 0.5246 0.3136 0.068 Uiso 1 1 calc R . . C126 C 0.22838(13) 0.42897(14) 0.30802(14) 0.0461(10) Uani 1 1 d . . . C128 C 0.18663(15) 0.30800(16) 0.41526(13) 0.0629(11) Uani 1 1 d . . . H12A H 0.2138 0.2738 0.4058 0.076 Uiso 1 1 calc R . . H12B H 0.1961 0.3132 0.4584 0.076 Uiso 1 1 calc R . . C127 C 0.1747(3) 0.5539(3) 0.4060(3) 0.0939(16) Uani 0.625(3) 1 d PD D -1 C129 C 0.2320(3) 0.5977(3) 0.4208(4) 0.165(4) Uani 0.625(3) 1 d PD D -1 H12C H 0.2485 0.6036 0.3858 0.247 Uiso 0.625(3) 1 calc PR D -1 H12D H 0.2639 0.5780 0.4520 0.247 Uiso 0.625(3) 1 calc PR D -1 H12E H 0.2203 0.6395 0.4342 0.247 Uiso 0.625(3) 1 calc PR D -1 C130 C 0.1247(3) 0.5863(3) 0.3574(3) 0.147(4) Uani 0.625(3) 1 d PD D -1 H13A H 0.1388 0.5871 0.3207 0.220 Uiso 0.625(3) 1 calc PR D -1 H13B H 0.1178 0.6304 0.3692 0.220 Uiso 0.625(3) 1 calc PR D -1 H13C H 0.0858 0.5620 0.3515 0.220 Uiso 0.625(3) 1 calc PR D -1 C131 C 0.1487(4) 0.5461(3) 0.4602(3) 0.208(4) Uani 0.625(3) 1 d PD D -1 H13D H 0.1395 0.5886 0.4742 0.312 Uiso 0.625(3) 1 calc PR D -1 H13E H 0.1792 0.5242 0.4910 0.312 Uiso 0.625(3) 1 calc PR D -1 H13F H 0.1104 0.5206 0.4502 0.312 Uiso 0.625(3) 1 calc PR D -1 C527 C 0.1808(4) 0.5461(4) 0.4197(4) 0.0939(16) Uani 0.375(3) 1 d PD D -2 C132 C 0.1147(3) 0.5406(5) 0.4282(4) 0.100(4) Uani 0.375(3) 1 d PD D -2 H13G H 0.1118 0.5035 0.4532 0.150 Uiso 0.375(3) 1 calc PR D -2 H13H H 0.0857 0.5351 0.3900 0.150 Uiso 0.375(3) 1 calc PR D -2 H13I H 0.1041 0.5798 0.4470 0.150 Uiso 0.375(3) 1 calc PR D -2 C133 C 0.1904(5) 0.6051(3) 0.3838(4) 0.101(4) Uani 0.375(3) 1 d PD D -2 H13J H 0.2316 0.6031 0.3753 0.152 Uiso 0.375(3) 1 calc PR D -2 H13K H 0.1871 0.6442 0.4063 0.152 Uiso 0.375(3) 1 calc PR D -2 H13L H 0.1586 0.6058 0.3469 0.152 Uiso 0.375(3) 1 calc PR D -2 C134 C 0.2269(4) 0.5473(5) 0.4789(3) 0.103(4) Uani 0.375(3) 1 d PD D -2 H13M H 0.2205 0.5095 0.5017 0.155 Uiso 0.375(3) 1 calc PR D -2 H13N H 0.2206 0.5864 0.5002 0.155 Uiso 0.375(3) 1 calc PR D -2 H13O H 0.2693 0.5469 0.4730 0.155 Uiso 0.375(3) 1 calc PR D -2 C141 C 0.16352(14) 0.37647(15) 0.17315(14) 0.0528(10) Uani 1 1 d . D . C142 C 0.19438(14) 0.43359(15) 0.19814(14) 0.0537(10) Uani 1 1 d . . . C143 C 0.17176(15) 0.49205(15) 0.17297(14) 0.0595(11) Uani 1 1 d . D . H143 H 0.1925 0.5303 0.1887 0.071 Uiso 1 1 calc R . . C144 C 0.12039(15) 0.49736(14) 0.12595(14) 0.0576(10) Uani 1 1 d D . . C145 C 0.09221(15) 0.44158(15) 0.10426(14) 0.0613(11) Uani 1 1 d . D . H145 H 0.0569 0.4437 0.0722 0.074 Uiso 1 1 calc R . . C146 C 0.11261(14) 0.38192(14) 0.12671(12) 0.0463(9) Uani 1 1 d . . . C148 C 0.24781(14) 0.43082(16) 0.25121(14) 0.0601(11) Uani 1 1 d . D . H14A H 0.2730 0.3921 0.2484 0.072 Uiso 1 1 calc R . . H14B H 0.2746 0.4689 0.2510 0.072 Uiso 1 1 calc R . . C147 C 0.1020(2) 0.5646(2) 0.1003(2) 0.0693(13) Uani 0.674(3) 1 d PD D -1 C149 C 0.1372(3) 0.6213(2) 0.1367(3) 0.105(3) Uani 0.674(3) 1 d PD D -1 H14C H 0.1818 0.6174 0.1387 0.157 Uiso 0.674(3) 1 calc PR D -1 H14D H 0.1301 0.6202 0.1764 0.157 Uiso 0.674(3) 1 calc PR D -1 H14E H 0.1218 0.6621 0.1178 0.157 Uiso 0.674(3) 1 calc PR D -1 C150 C 0.1124(3) 0.5675(2) 0.0387(2) 0.097(2) Uani 0.674(3) 1 d PD D -1 H15A H 0.1565 0.5604 0.0400 0.145 Uiso 0.674(3) 1 calc PR D -1 H15B H 0.1000 0.6099 0.0217 0.145 Uiso 0.674(3) 1 calc PR D -1 H15C H 0.0875 0.5343 0.0144 0.145 Uiso 0.674(3) 1 calc PR D -1 C151 C 0.0329(2) 0.5736(3) 0.0980(3) 0.106(3) Uani 0.674(3) 1 d PD D -1 H15D H 0.0192 0.6156 0.0808 0.159 Uiso 0.674(3) 1 calc PR D -1 H15E H 0.0261 0.5713 0.1378 0.159 Uiso 0.674(3) 1 calc PR D -1 H15F H 0.0090 0.5396 0.0739 0.159 Uiso 0.674(3) 1 calc PR D -1 C547 C 0.0906(4) 0.5596(4) 0.0957(4) 0.0693(13) Uani 0.326(3) 1 d PD D -2 C152 C 0.1446(4) 0.5971(4) 0.0793(4) 0.070(3) Uiso 0.326(3) 1 d PD D -2 H15G H 0.1295 0.6391 0.0630 0.105 Uiso 0.326(3) 1 calc PR D -2 H15H H 0.1603 0.5727 0.0500 0.105 Uiso 0.326(3) 1 calc PR D -2 H15I H 0.1780 0.6032 0.1145 0.105 Uiso 0.326(3) 1 calc PR D -2 C153 C 0.0398(4) 0.5501(5) 0.0395(3) 0.078(4) Uiso 0.326(3) 1 d PD D -2 H15J H 0.0043 0.5280 0.0490 0.117 Uiso 0.326(3) 1 calc PR D -2 H15K H 0.0562 0.5241 0.0116 0.117 Uiso 0.326(3) 1 calc PR D -2 H15L H 0.0265 0.5920 0.0220 0.117 Uiso 0.326(3) 1 calc PR D -2 C154 C 0.0648(4) 0.5978(4) 0.1416(3) 0.067(3) Uiso 0.326(3) 1 d PD D -2 H15M H 0.0356 0.5708 0.1566 0.101 Uiso 0.326(3) 1 calc PR D -2 H15N H 0.0431 0.6363 0.1231 0.101 Uiso 0.326(3) 1 calc PR D -2 H15O H 0.0991 0.6106 0.1741 0.101 Uiso 0.326(3) 1 calc PR D -2 N201 N 0.14708(12) 0.09682(12) 0.19783(11) 0.0596(9) Uani 1 1 d . A . H20A H 0.1392 0.1402 0.1943 0.072 Uiso 1 1 calc R . . H20B H 0.1890 0.0930 0.2002 0.072 Uiso 1 1 calc R . . C202 C 0.11927(17) 0.07286(17) 0.13728(15) 0.0734(13) Uani 1 1 d . . . H202 H 0.1254 0.0252 0.1380 0.088 Uiso 1 1 calc R A . C203 C 0.1493(2) 0.0985(2) 0.09235(18) 0.1207(19) Uani 1 1 d . A . H20A' H 0.1938 0.0884 0.1030 0.181 Uiso 1 1 calc R . . H20B' H 0.1437 0.1453 0.0898 0.181 Uiso 1 1 calc R . . H20C' H 0.1305 0.0791 0.0543 0.181 Uiso 1 1 calc R . . C204 C 0.05028(15) 0.08460(19) 0.12441(16) 0.0842(14) Uani 1 1 d . A . H20D H 0.0334 0.0665 0.1561 0.126 Uiso 1 1 calc R . . H20E H 0.0303 0.0640 0.0872 0.126 Uiso 1 1 calc R . . H20F H 0.0422 0.1309 0.1216 0.126 Uiso 1 1 calc R . . N211 N 0.0272(3) -0.0074(3) 0.2780(2) 0.144(2) Uani 0.626(3) 1 d PD A -1 H21A H 0.0342 -0.0317 0.3117 0.172 Uiso 0.626(3) 1 calc PR A -1 H21B H -0.0035 0.0218 0.2798 0.172 Uiso 0.626(3) 1 calc PR A -1 C212 C 0.0055(3) -0.0489(3) 0.2283(3) 0.089(2) Uani 0.626(3) 1 d PD A -1 H212 H -0.0033 -0.0209 0.1927 0.107 Uiso 0.626(3) 1 calc PR A -1 C213 C -0.0502(3) -0.0884(3) 0.2253(3) 0.069(2) Uani 0.626(3) 1 d PD A -1 C214 C 0.0601(3) -0.0922(3) 0.2236(3) 0.090(2) Uani 0.626(3) 1 d PD A -1 N212 N 0.0567(3) -0.0521(4) 0.2497(4) 0.094(4) Uani 0.374(3) 1 d PD A -2 H21C H 0.0607 -0.0654 0.2134 0.113 Uiso 0.374(3) 1 calc PR A -2 H21D H 0.0734 -0.0835 0.2764 0.113 Uiso 0.374(3) 1 calc PR A -2 C512 C -0.0083(4) -0.0453(4) 0.2486(6) 0.089(2) Uani 0.374(3) 1 d PD A -2 H512 H -0.0008 -0.0476 0.2923 0.107 Uiso 0.374(3) 1 calc PR A -2 C513 C -0.0535(5) -0.1000(5) 0.2400(6) 0.076(4) Uani 0.374(3) 1 d PD A -2 C515 C -0.0401(4) 0.0187(3) 0.2461(5) 0.070(3) Uani 0.374(3) 1 d PD A -2 N221 N 0.18400(12) 0.09344(13) 0.34972(13) 0.0780(11) Uani 1 1 d . A . H22A H 0.2236 0.0826 0.3472 0.094 Uiso 1 1 calc R . . H22B H 0.1843 0.1376 0.3512 0.094 Uiso 1 1 calc R . . C222 C 0.18662(19) 0.07728(19) 0.41288(16) 0.0878(14) Uani 1 1 d . . . H222 H 0.2007 0.0318 0.4206 0.105 Uiso 1 1 calc R A . C223 C 0.1244(2) 0.0848(2) 0.4253(2) 0.141(2) Uani 1 1 d . A . H22A' H 0.0950 0.0557 0.3999 0.212 Uiso 1 1 calc R . . H22B' H 0.1104 0.1293 0.4176 0.212 Uiso 1 1 calc R . . H22C' H 0.1267 0.0742 0.4665 0.212 Uiso 1 1 calc R . . C224 C 0.2319(2) 0.1212(2) 0.4526(2) 0.133(2) Uani 1 1 d . A . H22D H 0.2734 0.1154 0.4453 0.199 Uiso 1 1 calc R . . H22E H 0.2331 0.1107 0.4937 0.199 Uiso 1 1 calc R . . H22F H 0.2188 0.1659 0.4448 0.199 Uiso 1 1 calc R . . N231 N 0.36984(12) 0.27612(12) 0.34220(10) 0.0598(9) Uani 1 1 d . B . H23A H 0.3294 0.2753 0.3460 0.072 Uiso 1 1 calc R . . H23B H 0.3824 0.2340 0.3472 0.072 Uiso 1 1 calc R . . C232 C 0.40032(18) 0.30142(17) 0.40088(14) 0.0724(13) Uani 1 1 d . . . H232 H 0.3927 0.3488 0.4009 0.087 Uiso 1 1 calc R B . C233 C 0.46895(17) 0.29066(19) 0.41139(17) 0.0905(15) Uani 1 1 d . B . H23A' H 0.4846 0.3112 0.3800 0.136 Uiso 1 1 calc R . . H23B' H 0.4774 0.2444 0.4117 0.136 Uiso 1 1 calc R . . H23C' H 0.4897 0.3093 0.4493 0.136 Uiso 1 1 calc R . . C234 C 0.3743(2) 0.2720(2) 0.44792(17) 0.1164(19) Uani 1 1 d . B . H23D H 0.3296 0.2805 0.4400 0.175 Uiso 1 1 calc R . . H23E H 0.3948 0.2906 0.4859 0.175 Uiso 1 1 calc R . . H23F H 0.3814 0.2255 0.4488 0.175 Uiso 1 1 calc R . . N241 N 0.4870(2) 0.36600(17) 0.2616(2) 0.170(2) Uani 1 1 d . B -1 H24A H 0.5080 0.3695 0.3003 0.204 Uiso 1 1 calc R B -1 H24B H 0.5099 0.3390 0.2438 0.204 Uiso 1 1 calc R B -1 C242 C 0.4876(2) 0.42232(17) 0.2379(2) 0.1219(19) Uani 1 1 d . B -1 H242 H 0.4784 0.4087 0.1958 0.146 Uiso 1 1 calc R B -1 C243 C 0.54133(16) 0.46263(16) 0.23801(16) 0.0810(13) Uani 1 1 d . B -1 H24A' H 0.5771 0.4354 0.2365 0.121 Uiso 1 1 calc R B -1 H24B' H 0.5509 0.4886 0.2739 0.121 Uiso 1 1 calc R B -1 H24C' H 0.5322 0.4910 0.2037 0.121 Uiso 1 1 calc R B -1 C244 C 0.43084(18) 0.4550(2) 0.2371(2) 0.135(2) Uani 1 1 d . B -1 H24D H 0.3975 0.4236 0.2351 0.202 Uiso 1 1 calc R B -1 H24E H 0.4206 0.4832 0.2027 0.202 Uiso 1 1 calc R B -1 H24F H 0.4354 0.4808 0.2729 0.202 Uiso 1 1 calc R B -1 N251 N 0.31904(12) 0.27209(11) 0.18783(10) 0.0571(9) Uani 1 1 d . B -1 H25A H 0.3255 0.2284 0.1889 0.069 Uiso 1 1 calc R B -1 H25B H 0.2817 0.2788 0.1978 0.069 Uiso 1 1 calc R B -1 C252 C 0.31054(17) 0.29198(16) 0.12607(15) 0.0696(13) Uani 1 1 d . B -1 H252 H 0.2968 0.3379 0.1228 0.084 Uiso 1 1 calc R B -1 C253 C 0.26105(19) 0.25216(18) 0.08547(16) 0.0948(16) Uani 1 1 d . B -1 H25A' H 0.2216 0.2563 0.0974 0.142 Uiso 1 1 calc R B -1 H25B' H 0.2738 0.2070 0.0877 0.142 Uiso 1 1 calc R B -1 H25C' H 0.2558 0.2675 0.0450 0.142 Uiso 1 1 calc R B -1 C254 C 0.3720(2) 0.2880(2) 0.10972(17) 0.1147(18) Uani 1 1 d . B -1 H25D H 0.4026 0.3140 0.1370 0.172 Uiso 1 1 calc R B -1 H25E H 0.3676 0.3041 0.0697 0.172 Uiso 1 1 calc R B -1 H25F H 0.3859 0.2431 0.1118 0.172 Uiso 1 1 calc R B -1 O30 O 0.2578(4) 0.1860(4) 0.2746(4) 0.100 Uiso 0.293(4) 1 d P E -1 H05 H 0.128(2) 0.253(2) 0.2371(19) 0.20(2) Uiso 1 1 d . . . H04 H 0.3092(15) 0.0755(15) 0.2184(14) 0.075(12) Uiso 1 1 d . . . H07 H 0.2162(18) 0.3090(18) 0.2843(16) 0.130(16) Uiso 1 1 d . . . H02 H 0.3965(17) 0.1443(17) 0.2961(15) 0.099(14) Uiso 1 1 d . . . H03 H 0.3404(15) 0.0896(15) 0.3317(14) 0.086(12) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.0649(2) 0.0696(2) 0.0818(2) 0.00791(19) 0.01670(17) -0.00807(18) Ag2 0.0500(2) 0.1024(3) 0.0927(3) 0.0104(2) -0.0061(2) -0.0207(2) Ag01 0.138(2) 0.094(2) 0.0646(19) -0.0087(16) 0.0257(19) 0.0865(19) O1 0.0462(13) 0.0350(11) 0.0690(14) 0.0001(10) 0.0085(11) 0.0048(10) O2 0.0494(13) 0.0457(12) 0.0647(15) 0.0056(11) 0.0075(12) 0.0004(11) O3 0.0422(13) 0.0452(13) 0.0949(17) 0.0117(12) 0.0127(12) 0.0074(11) O4 0.0450(14) 0.0547(14) 0.0824(16) -0.0074(12) 0.0050(12) -0.0032(11) O5 0.0399(13) 0.0529(13) 0.0700(14) 0.0016(11) 0.0082(11) 0.0110(10) O6 0.0421(13) 0.0824(15) 0.0687(14) -0.0038(12) 0.0143(12) 0.0143(11) O7 0.0621(14) 0.0485(13) 0.0689(15) -0.0015(12) 0.0117(12) 0.0125(11) O8 0.0496(13) 0.0519(13) 0.0714(15) 0.0165(11) 0.0031(12) 0.0106(11) C1 0.0431(19) 0.0378(18) 0.053(2) 0.0124(16) 0.0054(17) 0.0020(15) C2 0.047(2) 0.0497(19) 0.046(2) 0.0118(17) 0.0047(17) 0.0015(16) C3 0.074(2) 0.046(2) 0.048(2) 0.0009(16) 0.0051(19) -0.0062(18) C4 0.054(2) 0.0415(19) 0.058(2) 0.0063(17) 0.0062(18) -0.0008(16) C5 0.0455(19) 0.0382(18) 0.050(2) 0.0097(16) 0.0014(17) -0.0019(15) C6 0.057(2) 0.0181(15) 0.0428(18) 0.0082(14) 0.0075(17) -0.0069(15) C7 0.058(2) 0.066(2) 0.080(2) -0.006(2) 0.021(2) 0.004(2) C8 0.062(2) 0.062(2) 0.049(2) 0.0002(18) -0.0028(18) 0.0070(18) C9 0.117(3) 0.068(3) 0.159(4) -0.006(3) 0.066(3) 0.016(2) C10 0.083(3) 0.123(4) 0.133(4) -0.017(3) 0.041(3) 0.008(3) C11 0.111(3) 0.099(3) 0.100(3) 0.013(2) 0.051(3) -0.002(3) C21 0.0385(18) 0.0306(17) 0.052(2) -0.0078(15) 0.0130(16) -0.0018(14) C22 0.048(2) 0.0257(16) 0.0525(19) -0.0058(15) 0.0075(17) -0.0076(14) C23 0.0485(19) 0.0373(17) 0.0515(19) -0.0106(15) 0.0206(16) -0.0115(15) C24 0.0436(19) 0.0500(19) 0.0421(19) -0.0006(16) 0.0154(16) -0.0027(16) C25 0.050(2) 0.0462(19) 0.0441(19) 0.0021(16) 0.0057(17) 0.0055(16) C26 0.054(2) 0.0380(17) 0.0395(18) -0.0069(15) 0.0210(16) -0.0103(16) C27 0.051(2) 0.076(2) 0.060(2) 0.0130(19) 0.0158(19) 0.0139(19) C28 0.0510(19) 0.0307(16) 0.067(2) 0.0089(17) 0.0078(18) -0.0028(15) C29 0.093(3) 0.115(4) 0.213(5) 0.068(3) 0.048(4) 0.037(3) C30 0.072(3) 0.228(5) 0.124(4) -0.080(4) -0.025(3) 0.043(3) C31 0.064(3) 0.161(4) 0.097(3) 0.013(3) 0.024(2) 0.035(3) C41 0.0430(19) 0.0375(18) 0.065(2) 0.0055(16) 0.0223(17) 0.0032(15) C42 0.0347(17) 0.0461(18) 0.0520(19) 0.0034(16) 0.0157(16) 0.0149(15) C43 0.0409(19) 0.056(2) 0.0451(19) -0.0064(16) 0.0076(16) 0.0079(16) C44 0.0450(19) 0.0485(19) 0.0439(19) 0.0029(16) 0.0128(16) 0.0107(16) C45 0.049(2) 0.0373(18) 0.057(2) -0.0021(16) 0.0129(17) -0.0059(15) C46 0.0309(17) 0.0481(19) 0.061(2) 0.0114(17) 0.0128(16) 0.0025(16) C47 0.073(2) 0.0469(19) 0.067(2) 0.0143(19) 0.013(2) 0.0283(18) C48 0.0450(19) 0.0479(19) 0.0531(19) -0.0091(16) 0.0127(17) 0.0043(16) C49 0.115(4) 0.078(3) 0.165(5) -0.002(3) -0.030(3) 0.047(3) C50 0.148(4) 0.093(3) 0.267(5) 0.120(3) 0.135(3) 0.069(3) C51 0.182(4) 0.077(3) 0.105(3) -0.013(3) 0.007(3) 0.070(3) C61 0.040(2) 0.052(2) 0.053(2) -0.0071(18) -0.0055(17) 0.0013(17) C62 0.0234(17) 0.0517(19) 0.066(2) 0.0043(18) -0.0021(16) 0.0001(16) C63 0.044(2) 0.041(2) 0.078(3) 0.0030(19) -0.0050(19) -0.0016(16) C64 0.044(2) 0.051(2) 0.066(2) 0.0052(19) -0.0069(19) 0.0081(17) C65 0.040(2) 0.073(2) 0.053(2) -0.0087(19) -0.0070(18) 0.0077(18) C66 0.040(2) 0.049(2) 0.058(2) 0.0000(18) -0.0108(18) -0.0022(17) C68 0.0253(18) 0.058(2) 0.070(2) 0.0109(18) 0.0022(17) -0.0009(15) C67A 0.061(3) 0.063(2) 0.090(3) -0.018(2) 0.002(2) 0.004(2) C69 0.139(6) 0.075(4) 0.104(5) -0.017(4) -0.007(5) 0.058(4) C70 0.083(5) 0.069(4) 0.116(5) -0.037(4) 0.011(4) -0.019(4) C71 0.118(6) 0.069(4) 0.146(6) -0.046(4) 0.049(5) 0.020(4) C67B 0.061(3) 0.063(2) 0.090(3) -0.018(2) 0.002(2) 0.004(2) C72 0.079(8) 0.053(7) 0.131(11) 0.005(7) -0.001(8) 0.018(6) C73 0.191(12) 0.045(7) 0.151(10) -0.002(6) 0.105(9) -0.025(7) C74 0.094(9) 0.082(7) 0.117(9) -0.057(7) 0.012(8) -0.017(7) C81 0.0310(18) 0.0404(18) 0.056(2) -0.0044(16) 0.0148(16) 0.0022(15) C82 0.0436(19) 0.0472(19) 0.0473(19) -0.0031(16) 0.0122(16) 0.0043(16) C83 0.046(2) 0.0541(19) 0.0454(19) -0.0013(16) 0.0101(16) 0.0136(16) C84 0.0368(18) 0.052(2) 0.0425(19) -0.0034(16) 0.0073(16) 0.0093(16) C85 0.0300(17) 0.0425(18) 0.055(2) -0.0139(16) 0.0100(15) 0.0062(14) C86 0.045(2) 0.0241(16) 0.053(2) -0.0087(15) 0.0013(17) 0.0053(15) C87 0.0390(19) 0.063(2) 0.055(2) -0.0025(18) 0.0031(17) 0.0106(17) C88 0.054(2) 0.071(2) 0.0407(18) 0.0045(18) 0.0144(17) 0.0136(18) C89 0.063(3) 0.109(3) 0.076(3) 0.002(2) 0.016(2) 0.027(2) C90 0.056(2) 0.069(2) 0.063(2) -0.0029(19) -0.001(2) 0.0053(19) C91 0.066(2) 0.066(2) 0.078(2) -0.011(2) -0.008(2) 0.017(2) C101 0.041(2) 0.0468(19) 0.052(2) 0.0153(17) 0.0070(17) 0.0013(16) C102 0.050(2) 0.0279(16) 0.059(2) 0.0175(15) 0.0119(18) 0.0025(15) C103 0.0359(19) 0.0459(19) 0.067(2) 0.0166(17) 0.0109(17) 0.0014(16) C104 0.057(2) 0.0448(19) 0.062(2) -0.0028(17) 0.0209(19) -0.0007(17) C105 0.065(2) 0.057(2) 0.0426(19) 0.0042(17) 0.0110(18) -0.0074(19) C106 0.052(2) 0.051(2) 0.046(2) 0.0208(17) 0.0004(18) 0.0067(17) C107 0.079(3) 0.078(3) 0.086(3) -0.014(2) 0.036(2) -0.009(2) C108 0.0397(18) 0.0400(18) 0.069(2) 0.0073(17) 0.0123(17) 0.0011(15) C109 0.097(3) 0.066(3) 0.111(3) -0.021(2) 0.039(3) -0.003(2) C110 0.173(4) 0.084(3) 0.156(4) 0.010(3) 0.117(3) 0.000(3) C111 0.090(3) 0.152(4) 0.203(5) -0.093(4) 0.058(3) -0.009(3) C121 0.0319(18) 0.0455(19) 0.055(2) -0.0104(17) 0.0026(16) 0.0088(15) C122 0.044(2) 0.055(2) 0.045(2) 0.0043(17) 0.0004(17) 0.0066(17) C123 0.050(2) 0.092(3) 0.064(2) -0.025(2) 0.0201(18) -0.016(2) C124 0.042(2) 0.058(2) 0.101(3) -0.019(2) 0.021(2) -0.0023(18) C125 0.044(2) 0.045(2) 0.079(2) -0.0007(19) 0.0089(19) -0.0024(16) C126 0.0328(18) 0.0430(19) 0.063(2) -0.0017(17) 0.0111(16) -0.0007(15) C128 0.056(2) 0.078(2) 0.049(2) 0.0108(19) 0.0002(18) 0.005(2) C127 0.055(2) 0.080(3) 0.151(4) -0.049(3) 0.033(3) 0.004(2) C129 0.094(6) 0.078(5) 0.313(11) -0.099(6) 0.029(7) 0.010(4) C130 0.089(6) 0.089(5) 0.260(10) -0.040(6) 0.036(6) 0.029(5) C131 0.281(8) 0.103(6) 0.327(9) -0.044(6) 0.247(7) 0.013(6) C527 0.055(2) 0.080(3) 0.151(4) -0.049(3) 0.033(3) 0.004(2) C132 0.120(8) 0.108(8) 0.071(7) -0.008(6) 0.020(7) 0.096(7) C133 0.166(11) 0.051(6) 0.115(8) -0.002(6) 0.089(8) 0.053(7) C134 0.094(9) 0.114(8) 0.102(8) -0.080(7) 0.022(7) -0.014(7) C141 0.0435(19) 0.062(2) 0.060(2) 0.0082(18) 0.0269(17) 0.0035(17) C142 0.0407(19) 0.055(2) 0.072(2) 0.0096(18) 0.0265(17) -0.0022(16) C143 0.060(2) 0.048(2) 0.084(2) 0.0113(18) 0.0431(19) 0.0054(17) C144 0.052(2) 0.061(2) 0.068(2) 0.0150(18) 0.0301(18) 0.0137(18) C145 0.052(2) 0.069(2) 0.067(2) 0.0231(19) 0.0226(18) 0.0157(18) C146 0.0445(19) 0.057(2) 0.0397(18) 0.0039(16) 0.0151(17) 0.0007(17) C148 0.0369(19) 0.060(2) 0.085(2) 0.0060(19) 0.0177(19) -0.0044(16) C147 0.047(2) 0.059(2) 0.103(3) 0.023(2) 0.019(2) 0.012(2) C149 0.095(5) 0.075(4) 0.129(6) 0.008(4) -0.003(4) 0.014(4) C150 0.120(5) 0.080(4) 0.098(4) 0.055(3) 0.039(4) 0.022(4) C151 0.074(4) 0.085(4) 0.167(6) 0.038(4) 0.042(4) 0.036(3) C547 0.047(2) 0.059(2) 0.103(3) 0.023(2) 0.019(2) 0.012(2) N201 0.0406(16) 0.0581(17) 0.0708(19) -0.0089(15) -0.0059(15) 0.0057(13) C202 0.067(3) 0.071(2) 0.077(3) 0.009(2) 0.007(2) -0.006(2) C203 0.071(3) 0.209(5) 0.080(3) 0.018(3) 0.014(3) 0.003(3) C204 0.047(2) 0.128(3) 0.075(3) 0.006(2) 0.008(2) -0.020(2) N211 0.076(4) 0.167(5) 0.190(5) -0.139(4) 0.035(4) -0.036(4) C212 0.142(5) 0.054(3) 0.087(5) -0.026(3) 0.057(4) -0.008(3) C213 0.062(4) 0.039(3) 0.108(5) 0.019(3) 0.027(4) -0.027(3) C214 0.083(4) 0.093(5) 0.105(5) -0.010(4) 0.042(4) 0.009(4) N212 0.056(6) 0.095(7) 0.096(7) 0.025(6) -0.052(5) 0.003(5) C512 0.142(5) 0.054(3) 0.087(5) -0.026(3) 0.057(4) -0.008(3) C513 0.068(8) 0.094(9) 0.075(8) 0.007(7) 0.032(6) -0.036(6) C515 0.039(5) 0.041(5) 0.141(9) -0.036(5) 0.042(6) -0.020(4) N221 0.0424(18) 0.080(2) 0.110(2) -0.0080(19) 0.0155(17) -0.0057(16) C222 0.091(3) 0.098(3) 0.068(3) 0.001(2) 0.005(2) 0.005(3) C223 0.109(4) 0.188(5) 0.137(4) 0.048(4) 0.049(3) 0.010(4) C224 0.134(4) 0.103(4) 0.140(4) -0.013(3) -0.010(4) 0.003(3) N231 0.0486(17) 0.0592(17) 0.0711(19) -0.0052(15) 0.0127(15) 0.0026(14) C232 0.091(3) 0.065(2) 0.061(2) -0.0055(19) 0.018(2) -0.004(2) C233 0.063(3) 0.120(3) 0.083(3) -0.012(2) 0.005(2) -0.033(2) C234 0.079(3) 0.196(5) 0.072(3) 0.012(3) 0.013(3) 0.008(3) N241 0.160(4) 0.106(3) 0.230(5) 0.051(3) 0.017(4) -0.001(3) C242 0.105(3) 0.042(2) 0.223(5) 0.029(3) 0.045(4) -0.007(2) C243 0.073(3) 0.079(3) 0.094(3) -0.018(2) 0.025(2) -0.030(2) C244 0.045(3) 0.206(5) 0.154(4) -0.045(4) 0.024(3) -0.019(3) N251 0.0759(19) 0.0384(15) 0.0630(17) 0.0059(13) 0.0280(15) -0.0008(14) C252 0.088(3) 0.059(2) 0.064(2) 0.0006(19) 0.023(2) 0.002(2) C253 0.097(3) 0.098(3) 0.078(3) -0.013(2) -0.004(2) -0.013(3) C254 0.120(4) 0.165(4) 0.075(3) -0.003(3) 0.053(3) -0.020(3) _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 Ag1 Ag02 0.762(3) . ? Ag1 Ag03 1.147(9) . ? Ag1 N251 2.241(2) . ? Ag1 N231 2.248(3) . ? Ag1 N241 2.337(4) . ? Ag2 Ag01 0.914(4) . ? Ag2 N221 2.246(3) . ? Ag2 N211 2.262(6) . ? Ag2 N201 2.346(3) . ? Ag2 N212 2.430(8) . ? Ag01 N221 1.801(4) . ? Ag01 N201 1.873(4) . ? Ag02 Ag03 1.557(9) . ? Ag02 N231 2.504(4) . ? Ag03 N231 1.574(9) . ? O1 C1 1.359(4) . ? O2 C21 1.339(3) . ? O3 C41 1.380(3) . ? O4 C61 1.377(4) . ? O5 C81 1.347(3) . ? O6 C101 1.353(4) . ? O7 C121 1.370(3) . ? O8 C141 1.348(3) . ? C1 C2 1.385(4) . ? C1 C6 1.385(4) . ? C2 C3 1.384(5) . ? C2 C8 1.512(4) . ? C3 C4 1.393(4) . ? C4 C5 1.391(4) . ? C4 C7 1.500(5) . ? C5 C6 1.395(4) . ? C6 C28 1.514(4) . ? C7 C10 1.534(5) . ? C7 C11 1.539(5) . ? C7 C9 1.546(4) . ? C8 C66 1.533(4) . ? C21 C26 1.390(4) . ? C21 C22 1.396(4) . ? C22 C23 1.388(4) . ? C22 C28 1.513(4) . ? C23 C24 1.392(4) . ? C24 C25 1.363(4) . ? C24 C27 1.537(4) . ? C25 C26 1.404(4) . ? C26 C48 1.514(4) . ? C27 C30 1.461(5) . ? C27 C31 1.503(5) . ? C27 C29 1.547(5) . ? C41 C42 1.385(4) . ? C41 C46 1.397(4) . ? C42 C43 1.384(4) . ? C42 C48 1.509(4) . ? C43 C44 1.398(4) . ? C44 C45 1.360(4) . ? C44 C47 1.556(4) . ? C45 C46 1.405(4) . ? C46 C68 1.509(4) . ? C47 C50 1.462(5) . ? C47 C51 1.493(5) . ? C47 C49 1.521(5) . ? C61 C66 1.383(5) . ? C61 C62 1.391(4) . ? C62 C63 1.383(4) . ? C62 C68 1.507(4) . ? C63 C64 1.376(5) . ? C64 C65 1.392(4) . ? C64 C67A 1.520(6) . ? C64 C67B 1.544(9) . ? C65 C66 1.399(4) . ? C67A C71 1.534(8) . ? C67A C70 1.540(7) . ? C67A C69 1.549(7) . ? C67B C74 1.547(10) . ? C67B C72 1.556(10) . ? C67B C73 1.557(11) . ? C81 C86 1.383(4) . ? C81 C82 1.403(4) . ? C82 C83 1.397(4) . ? C82 C88 1.498(4) . ? C83 C84 1.385(4) . ? C84 C85 1.374(4) . ? C84 C87 1.517(4) . ? C85 C86 1.394(4) . ? C86 C108 1.533(4) . ? C87 C90 1.514(4) . ? C87 C89 1.533(5) . ? C87 C91 1.555(4) . ? C88 C146 1.524(4) . ? C101 C102 1.399(4) . ? C101 C106 1.397(4) . ? C102 C103 1.393(4) . ? C102 C108 1.531(4) . ? C103 C104 1.380(4) . ? C104 C105 1.382(4) . ? C104 C107 1.529(5) . ? C105 C106 1.367(5) . ? C106 C128 1.523(4) . ? C107 C111 1.492(5) . ? C107 C109 1.533(5) . ? C107 C110 1.539(5) . ? C121 C126 1.378(4) . ? C121 C122 1.384(4) . ? C122 C123 1.383(4) . ? C122 C128 1.528(4) . ? C123 C124 1.384(4) . ? C124 C125 1.376(5) . ? C124 C527 1.545(9) . ? C124 C127 1.565(6) . ? C125 C126 1.379(4) . ? C126 C148 1.491(4) . ? C127 C131 1.520(9) . ? C127 C129 1.536(8) . ? C127 C130 1.545(8) . ? C527 C134 1.518(10) . ? C527 C132 1.525(11) . ? C527 C133 1.531(11) . ? C141 C146 1.377(4) . ? C141 C142 1.427(4) . ? C142 C143 1.393(4) . ? C142 C148 1.504(4) . ? C143 C144 1.391(4) . ? C144 C145 1.359(4) . ? C144 C147 1.539(5) . ? C144 C547 1.549(9) . ? C145 C146 1.383(4) . ? C147 C150 1.514(7) . ? C147 C151 1.530(7) . ? C147 C149 1.555(6) . ? C547 C153 1.532(10) . ? C547 C152 1.548(11) . ? C547 C154 1.549(11) . ? N201 C202 1.494(4) . ? C202 C203 1.470(5) . ? C202 C204 1.506(5) . ? N211 C212 1.440(7) . ? C212 C213 1.468(8) . ? C212 C214 1.531(8) . ? N212 C512 1.439(11) . ? C512 C513 1.498(12) . ? C512 C515 1.502(10) . ? N221 C222 1.505(4) . ? C222 C223 1.480(6) . ? C222 C224 1.508(5) . ? N231 C232 1.480(4) . ? C232 C234 1.488(5) . ? C232 C233 1.498(5) . ? N241 C242 1.299(5) . ? C242 C244 1.424(6) . ? C242 C243 1.455(5) . ? N251 C252 1.474(4) . ? C252 C254 1.498(5) . ? C252 C253 1.519(5) . ? 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 Ag02 Ag1 Ag03 107.6(5) . . ? Ag02 Ag1 N251 98.5(2) . . ? Ag03 Ag1 N251 62.7(4) . . ? Ag02 Ag1 N231 100.8(2) . . ? Ag03 Ag1 N231 41.0(4) . . ? N251 Ag1 N231 103.64(9) . . ? Ag02 Ag1 N241 84.7(2) . . ? Ag03 Ag1 N241 159.5(4) . . ? N251 Ag1 N241 133.08(14) . . ? N231 Ag1 N241 121.85(13) . . ? Ag01 Ag2 N221 50.0(2) . . ? Ag01 Ag2 N211 160.3(2) . . ? N221 Ag2 N211 128.99(16) . . ? Ag01 Ag2 N201 48.7(2) . . ? N221 Ag2 N201 97.78(10) . . ? N211 Ag2 N201 131.06(16) . . ? Ag01 Ag2 N212 161.6(3) . . ? N221 Ag2 N212 141.7(2) . . ? N211 Ag2 N212 34.2(2) . . ? N201 Ag2 N212 114.9(2) . . ? Ag2 Ag01 N221 107.1(3) . . ? Ag2 Ag01 N201 109.8(2) . . ? N221 Ag01 N201 140.8(3) . . ? Ag1 Ag02 Ag03 44.6(4) . . ? Ag1 Ag02 N231 61.9(2) . . ? Ag03 Ag02 N231 37.1(3) . . ? Ag1 Ag03 Ag02 27.8(2) . . ? Ag1 Ag03 N231 110.4(6) . . ? Ag02 Ag03 N231 106.2(5) . . ? O1 C1 C2 120.9(3) . . ? O1 C1 C6 119.0(3) . . ? C2 C1 C6 120.1(3) . . ? C1 C2 C3 118.3(3) . . ? C1 C2 C8 121.7(3) . . ? C3 C2 C8 120.0(3) . . ? C2 C3 C4 124.5(3) . . ? C5 C4 C3 114.7(3) . . ? C5 C4 C7 122.9(3) . . ? C3 C4 C7 122.3(3) . . ? C4 C5 C6 123.0(3) . . ? C1 C6 C5 119.2(3) . . ? C1 C6 C28 122.2(3) . . ? C5 C6 C28 118.5(3) . . ? C4 C7 C10 112.9(3) . . ? C4 C7 C11 109.1(3) . . ? C10 C7 C11 106.2(3) . . ? C4 C7 C9 111.1(3) . . ? C10 C7 C9 108.5(3) . . ? C11 C7 C9 108.8(3) . . ? C2 C8 C66 114.8(2) . . ? O2 C21 C26 120.5(3) . . ? O2 C21 C22 120.5(3) . . ? C26 C21 C22 119.0(3) . . ? C23 C22 C21 119.5(3) . . ? C23 C22 C28 118.4(3) . . ? C21 C22 C28 121.9(3) . . ? C22 C23 C24 122.2(3) . . ? C25 C24 C23 117.2(3) . . ? C25 C24 C27 121.2(3) . . ? C23 C24 C27 121.6(3) . . ? C24 C25 C26 122.5(3) . . ? C21 C26 C25 119.3(3) . . ? C21 C26 C48 120.9(3) . . ? C25 C26 C48 119.6(3) . . ? C30 C27 C31 109.8(3) . . ? C30 C27 C24 111.8(3) . . ? C31 C27 C24 113.4(3) . . ? C30 C27 C29 107.5(3) . . ? C31 C27 C29 106.2(3) . . ? C24 C27 C29 107.9(3) . . ? C22 C28 C6 113.2(2) . . ? O3 C41 C42 119.6(3) . . ? O3 C41 C46 118.3(2) . . ? C42 C41 C46 122.0(3) . . ? C43 C42 C41 117.7(3) . . ? C43 C42 C48 119.7(2) . . ? C41 C42 C48 122.6(2) . . ? C42 C43 C44 122.8(3) . . ? C45 C44 C43 117.4(3) . . ? C45 C44 C47 120.1(3) . . ? C43 C44 C47 122.4(3) . . ? C44 C45 C46 123.0(3) . . ? C41 C46 C45 117.1(3) . . ? C41 C46 C68 123.1(3) . . ? C45 C46 C68 119.6(3) . . ? C50 C47 C51 112.1(3) . . ? C50 C47 C49 107.1(3) . . ? C51 C47 C49 105.5(3) . . ? C50 C47 C44 109.4(3) . . ? C51 C47 C44 110.8(3) . . ? C49 C47 C44 111.8(3) . . ? C42 C48 C26 112.1(2) . . ? O4 C61 C66 120.1(3) . . ? O4 C61 C62 118.1(3) . . ? C66 C61 C62 121.7(3) . . ? C63 C62 C61 116.5(3) . . ? C63 C62 C68 121.3(3) . . ? C61 C62 C68 121.8(3) . . ? C64 C63 C62 124.9(3) . . ? C63 C64 C65 116.6(3) . . ? C63 C64 C67A 124.6(3) . . ? C65 C64 C67A 118.9(4) . . ? C63 C64 C67B 118.8(4) . . ? C65 C64 C67B 124.6(5) . . ? C67A C64 C67B 5.9(5) . . ? C64 C65 C66 121.3(3) . . ? C61 C66 C65 118.9(3) . . ? C61 C66 C8 122.3(3) . . ? C65 C66 C8 118.7(3) . . ? C62 C68 C46 112.0(2) . . ? C64 C67A C71 115.1(4) . . ? C64 C67A C70 108.3(4) . . ? C71 C67A C70 107.4(5) . . ? C64 C67A C69 106.3(4) . . ? C71 C67A C69 108.1(5) . . ? C70 C67A C69 111.9(5) . . ? C74 C67B C64 108.1(6) . . ? C74 C67B C72 109.1(8) . . ? C64 C67B C72 110.1(6) . . ? C74 C67B C73 107.4(7) . . ? C64 C67B C73 115.5(7) . . ? C72 C67B C73 106.5(7) . . ? O5 C81 C86 120.2(3) . . ? O5 C81 C82 120.2(3) . . ? C86 C81 C82 119.5(3) . . ? C83 C82 C81 117.6(3) . . ? C83 C82 C88 121.3(3) . . ? C81 C82 C88 121.1(3) . . ? C84 C83 C82 124.4(3) . . ? C85 C84 C83 115.5(3) . . ? C85 C84 C87 123.1(3) . . ? C83 C84 C87 121.4(3) . . ? C84 C85 C86 123.1(3) . . ? C81 C86 C85 119.8(3) . . ? C81 C86 C108 121.4(3) . . ? C85 C86 C108 118.7(3) . . ? C90 C87 C84 109.7(3) . . ? C90 C87 C89 108.1(3) . . ? C84 C87 C89 113.1(3) . . ? C90 C87 C91 108.3(2) . . ? C84 C87 C91 109.7(3) . . ? C89 C87 C91 107.7(3) . . ? C82 C88 C146 115.2(3) . . ? O6 C101 C102 120.5(3) . . ? O6 C101 C106 120.7(3) . . ? C102 C101 C106 118.8(3) . . ? C103 C102 C101 118.8(3) . . ? C103 C102 C108 120.8(3) . . ? C101 C102 C108 120.3(3) . . ? C104 C103 C102 123.2(3) . . ? C103 C104 C105 115.9(3) . . ? C103 C104 C107 123.8(3) . . ? C105 C104 C107 120.3(3) . . ? C106 C105 C104 123.6(3) . . ? C105 C106 C101 119.7(3) . . ? C105 C106 C128 119.8(3) . . ? C101 C106 C128 120.5(3) . . ? C111 C107 C104 112.3(3) . . ? C111 C107 C109 108.4(3) . . ? C104 C107 C109 110.7(3) . . ? C111 C107 C110 108.0(4) . . ? C104 C107 C110 108.6(3) . . ? C109 C107 C110 108.7(3) . . ? C102 C108 C86 113.4(2) . . ? O7 C121 C126 119.5(3) . . ? O7 C121 C122 118.9(3) . . ? C126 C121 C122 121.5(3) . . ? C123 C122 C121 118.3(3) . . ? C123 C122 C128 119.8(3) . . ? C121 C122 C128 121.8(3) . . ? C122 C123 C124 122.3(3) . . ? C125 C124 C123 116.8(3) . . ? C125 C124 C527 129.2(5) . . ? C123 C124 C527 113.7(5) . . ? C125 C124 C127 118.6(4) . . ? C123 C124 C127 124.5(4) . . ? C527 C124 C127 13.2(5) . . ? C124 C125 C126 123.4(3) . . ? C121 C126 C125 117.7(3) . . ? C121 C126 C148 122.3(3) . . ? C125 C126 C148 119.9(3) . . ? C106 C128 C122 110.3(2) . . ? C131 C127 C129 109.1(6) . . ? C131 C127 C130 108.3(5) . . ? C129 C127 C130 108.7(5) . . ? C131 C127 C124 111.1(5) . . ? C129 C127 C124 110.2(4) . . ? C130 C127 C124 109.3(5) . . ? C134 C527 C132 110.1(8) . . ? C134 C527 C133 109.7(7) . . ? C132 C527 C133 113.0(8) . . ? C134 C527 C124 110.6(7) . . ? C132 C527 C124 107.4(6) . . ? C133 C527 C124 105.8(7) . . ? O8 C141 C146 122.9(3) . . ? O8 C141 C142 118.3(3) . . ? C146 C141 C142 118.8(3) . . ? C143 C142 C141 117.6(3) . . ? C143 C142 C148 121.3(3) . . ? C141 C142 C148 121.1(3) . . ? C144 C143 C142 123.5(3) . . ? C145 C144 C143 116.6(3) . . ? C145 C144 C147 125.0(3) . . ? C143 C144 C147 118.3(3) . . ? C145 C144 C547 115.7(4) . . ? C143 C144 C547 127.7(4) . . ? C147 C144 C547 10.0(4) . . ? C144 C145 C146 123.0(3) . . ? C141 C146 C145 120.6(3) . . ? C141 C146 C88 119.1(3) . . ? C145 C146 C88 120.2(3) . . ? C126 C148 C142 113.8(3) . . ? C150 C147 C151 109.5(4) . . ? C150 C147 C144 109.0(4) . . ? C151 C147 C144 107.2(4) . . ? C150 C147 C149 108.9(4) . . ? C151 C147 C149 107.2(4) . . ? C144 C147 C149 115.0(4) . . ? C153 C547 C152 107.9(8) . . ? C153 C547 C154 110.3(7) . . ? C152 C547 C154 110.2(7) . . ? C153 C547 C144 115.7(7) . . ? C152 C547 C144 105.3(6) . . ? C154 C547 C144 107.4(7) . . ? C202 N201 Ag01 138.7(2) . . ? C202 N201 Ag2 117.2(2) . . ? Ag01 N201 Ag2 21.50(11) . . ? C203 C202 N201 113.8(3) . . ? C203 C202 C204 113.8(3) . . ? N201 C202 C204 108.1(3) . . ? C212 N211 Ag2 114.0(4) . . ? N211 C212 C213 119.5(6) . . ? N211 C212 C214 106.9(5) . . ? C213 C212 C214 109.6(5) . . ? C512 N212 Ag2 113.2(6) . . ? N212 C512 C513 124.2(9) . . ? N212 C512 C515 123.1(8) . . ? C513 C512 C515 112.1(8) . . ? C222 N221 Ag01 144.3(3) . . ? C222 N221 Ag2 121.8(2) . . ? Ag01 N221 Ag2 22.87(12) . . ? C223 C222 N221 110.1(3) . . ? C223 C222 C224 109.3(4) . . ? N221 C222 C224 109.9(3) . . ? C232 N231 Ag03 149.6(4) . . ? C232 N231 Ag1 121.5(2) . . ? Ag03 N231 Ag1 28.6(3) . . ? C232 N231 Ag02 113.6(2) . . ? Ag03 N231 Ag02 36.7(3) . . ? Ag1 N231 Ag02 17.38(7) . . ? N231 C232 C234 111.7(3) . . ? N231 C232 C233 109.0(3) . . ? C234 C232 C233 111.6(3) . . ? C242 N241 Ag1 120.3(3) . . ? N241 C242 C244 109.9(4) . . ? N241 C242 C243 127.5(4) . . ? C244 C242 C243 116.3(3) . . ? C252 N251 Ag1 122.3(2) . . ? N251 C252 C254 108.6(3) . . ? N251 C252 C253 111.7(3) . . ? C254 C252 C253 112.0(3) . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 21.15 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.576 _refine_diff_density_min -0.653 _refine_diff_density_rms 0.068