# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_C-hexyltetracyanoresorcin[4]arene _database_code_depnum_ccdc_archive 'CCDC 908886' #TrackingRef '15894_web_deposit_cif_file_0_AndrewMossine_1354649190.RESCN.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common C-hexyltetracyanoresorcin(4)arene _chemical_formula_moiety 'C56 H68 N4 O8, 3(C1 H4 O1), 1(H2 O1)' _chemical_formula_sum 'C59 H82 N4 O12' _exptl_crystal_recrystallization_method '8:1 methanol:water' _chemical_melting_point ? _exptl_crystal_description prism _exptl_crystal_colour orange _diffrn_ambient_temperature 173(2) _chemical_formula_weight 1039.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_int_tables_number 14 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 18.167(5) _cell_length_b 16.430(4) _cell_length_c 19.731(5) _cell_angle_alpha 90.00 _cell_angle_beta 93.477(3) _cell_angle_gamma 90.00 _cell_volume 5879(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9841 _cell_measurement_theta_min 4.492 _cell_measurement_theta_max 53.684 _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.174 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2240 _exptl_absorpt_coefficient_mu 0.082 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.88 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_process_details ; Data were corrected for decay and absorption using the program SADABS (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of G\"ottingen, Germany). ; _exptl_special_details ; ? ; _diffrn_radiation_probe ? _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 68252 _diffrn_reflns_av_R_equivalents 0.0376 _diffrn_reflns_av_sigmaI/netI 0.0291 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.57 _diffrn_reflns_theta_max 27.49 _reflns_number_total 13444 _reflns_number_gt 10357 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2008)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2008)' _computing_data_reduction 'APEX2 (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-SEED, Barbour, 2001' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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. Following refinement, the maximum difference density peak was found to be 0.625. This peak appeared to coincide to a potential alternate position of a hydroxyl hydrogen on one of the methanol molecules. However, as this hydrogen does not fit to the overall hydrogen bonding scheme within this structure, it was omitted. Also, It is unlikely that all possible positions of c-hexyl tails and solvent molecules have been accounted for due to a high level of disorder within these parts of the structure. However, all major parts have been modeled to the best of our ability. ; _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^)+(0.0859P)^2^+4.2531P] 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 13444 _refine_ls_number_parameters 753 _refine_ls_number_restraints 3 _refine_ls_R_factor_all 0.0754 _refine_ls_R_factor_gt 0.0572 _refine_ls_wR_factor_ref 0.1734 _refine_ls_wR_factor_gt 0.1582 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 0.29660(9) 0.80011(9) 0.40164(7) 0.0300(3) Uani 1 1 d . . . N1 N 0.24031(10) 0.61300(10) 0.33279(9) 0.0335(4) Uani 1 1 d . . . C1 C 0.21866(9) 0.92384(10) 0.25961(9) 0.0199(3) Uani 1 1 d . . . H1 H 0.2145 0.9789 0.2453 0.024 Uiso 1 1 calc R . . O2 O 0.17021(8) 0.71799(8) 0.20129(7) 0.0263(3) Uani 1 1 d . . . N2 N 0.24675(11) 0.63797(11) -0.05527(10) 0.0377(4) Uani 1 1 d . B . C2 C 0.25456(9) 0.90801(10) 0.32279(9) 0.0195(3) Uani 1 1 d . B . O3 O 0.14169(8) 0.74171(9) 0.06534(7) 0.0285(3) Uani 1 1 d . B . N3 N 0.62917(11) 0.76977(12) 0.12147(10) 0.0415(4) Uani 1 1 d D B . C3 C 0.26167(10) 0.82648(11) 0.34280(9) 0.0213(3) Uani 1 1 d . . . O4 O 0.35153(8) 0.82160(9) -0.05913(7) 0.0308(3) Uani 1 1 d . B . N4 N 0.58438(10) 0.88550(11) 0.49014(9) 0.0315(4) Uani 1 1 d . B . C4 C 0.23126(10) 0.76497(10) 0.30067(9) 0.0212(3) Uani 1 1 d . . . O5 O 0.48413(8) 0.84294(8) 0.01586(7) 0.0299(3) Uani 1 1 d . B . C5 C 0.19554(10) 0.78323(10) 0.23766(9) 0.0207(3) Uani 1 1 d . . . O6 O 0.60754(8) 0.93698(9) 0.21510(7) 0.0310(3) Uani 1 1 d . B . C6 C 0.18847(9) 0.86396(10) 0.21608(8) 0.0193(3) Uani 1 1 d . B . O7 O 0.59590(7) 1.00438(9) 0.33874(7) 0.0286(3) Uani 1 1 d . B . C7 C 0.15051(10) 0.88260(10) 0.14665(9) 0.0212(3) Uani 1 1 d . . . H7 H 0.1083 0.8438 0.1398 0.025 Uiso 1 1 calc R A 1 O8 O 0.39746(8) 0.91042(8) 0.46693(6) 0.0249(3) Uani 1 1 d . B . C8 C 0.26163(10) 0.91741(10) 0.07962(9) 0.0210(3) Uani 1 1 d . . . H8 H 0.2686 0.9634 0.1085 0.025 Uiso 1 1 calc R B . C9 C 0.20367(9) 0.86485(10) 0.09113(8) 0.0204(3) Uani 1 1 d . B . C10 C 0.19660(10) 0.79485(11) 0.05123(9) 0.0226(4) Uani 1 1 d . . . C11 C 0.24696(10) 0.77919(11) 0.00147(9) 0.0232(4) Uani 1 1 d . B . C12 C 0.30215(10) 0.83630(11) -0.01108(9) 0.0234(4) Uani 1 1 d . . . C13 C 0.30996(10) 0.90653(10) 0.02834(9) 0.0209(3) Uani 1 1 d . B . C14 C 0.36837(10) 0.97046(10) 0.01495(8) 0.0208(3) Uani 1 1 d . . . H14 H 0.3876 0.9585 -0.0304 0.025 Uiso 1 1 calc R B . C15 C 0.44114(10) 1.01651(10) 0.12355(8) 0.0204(3) Uani 1 1 d . . . H15 H 0.4055 1.0585 0.1267 0.024 Uiso 1 1 calc R B . C16 C 0.43306(9) 0.96343(10) 0.06832(9) 0.0205(3) Uani 1 1 d . B . C17 C 0.48457(10) 0.90053(11) 0.06513(9) 0.0227(4) Uani 1 1 d . . . C18 C 0.54177(10) 0.89345(11) 0.11613(9) 0.0237(4) Uani 1 1 d . B . C19 C 0.54902(10) 0.94968(11) 0.16966(9) 0.0227(4) Uani 1 1 d . . . C20 C 0.49789(10) 1.01229(10) 0.17458(8) 0.0206(3) Uani 1 1 d . B . C21 C 0.50280(9) 1.07093(10) 0.23464(8) 0.0200(3) Uani 1 1 d . . . H21 H 0.5565 1.0809 0.2457 0.024 Uiso 1 1 calc R B . C22 C 0.39754(9) 1.02228(10) 0.30558(8) 0.0196(3) Uani 1 1 d . . . H22 H 0.3639 1.0430 0.2711 0.024 Uiso 1 1 calc R B . C23 C 0.47299(10) 1.03074(10) 0.29739(8) 0.0201(3) Uani 1 1 d . B . C24 C 0.52181(10) 0.99902(11) 0.34772(9) 0.0219(3) Uani 1 1 d . . . C25 C 0.49520(10) 0.95869(11) 0.40392(9) 0.0215(3) Uani 1 1 d . B . C26 C 0.41912(10) 0.95332(10) 0.41152(9) 0.0208(3) Uani 1 1 d . . . C27 C 0.36891(9) 0.98480(10) 0.36218(8) 0.0195(3) Uani 1 1 d . B . C28 C 0.28618(9) 0.97558(10) 0.36931(8) 0.0197(3) Uani 1 1 d . . . H28 H 0.2802 0.9569 0.4169 0.024 Uiso 1 1 calc R B . C29 C 0.11830(11) 0.96908(12) 0.14063(10) 0.0293(5) Uani 0.706(4) 1 d P B 1 H29A H 0.0858 0.9778 0.1785 0.035 Uiso 0.706(4) 1 calc PR B 1 H29B H 0.1593 1.0086 0.1461 0.035 Uiso 0.706(4) 1 calc PR B 1 C30 C 0.07562(19) 0.9866(2) 0.07576(16) 0.0401(8) Uani 0.706(4) 1 d P B 1 H30A H 0.0313 0.9514 0.0725 0.048 Uiso 0.706(4) 1 calc PR B 1 H30B H 0.1062 0.9724 0.0376 0.048 Uiso 0.706(4) 1 calc PR B 1 C31 C 0.0511(2) 1.0761(2) 0.06799(19) 0.0497(10) Uani 0.706(4) 1 d P B 1 H31A H 0.0943 1.1117 0.0786 0.060 Uiso 0.706(4) 1 calc PR B 1 H31B H 0.0340 1.0859 0.0201 0.060 Uiso 0.706(4) 1 calc PR B 1 C32 C -0.0091(2) 1.0993(3) 0.1126(2) 0.0874(13) Uani 0.706(4) 1 d P B 1 H32A H 0.0090 1.0944 0.1608 0.105 Uiso 0.706(4) 1 calc PR B 1 H32B H -0.0512 1.0616 0.1047 0.105 Uiso 0.706(4) 1 calc PR B 1 C33 C -0.0355(3) 1.1881(3) 0.0984(2) 0.1015(15) Uani 1 1 d . . . H33A H 0.0067 1.2259 0.1056 0.122 Uiso 1 1 calc R B 1 H33B H -0.0546 1.1929 0.0505 0.122 Uiso 1 1 calc R B 1 C34 C -0.0946(3) 1.2107(4) 0.1443(3) 0.132(2) Uani 1 1 d . B . H34A H -0.1344 1.1705 0.1400 0.198 Uiso 1 1 calc R . . H34B H -0.1142 1.2646 0.1316 0.198 Uiso 1 1 calc R . . H34C H -0.0741 1.2120 0.1913 0.198 Uiso 1 1 calc R . . C35 C 0.33363(10) 1.05580(11) 0.01154(9) 0.0236(4) Uani 1 1 d . B . H35A H 0.3142 1.0685 0.0561 0.028 Uiso 1 1 calc R . . H35B H 0.3726 1.0961 0.0033 0.028 Uiso 1 1 calc R . . C36 C 0.27128(11) 1.06532(12) -0.04355(10) 0.0282(4) Uani 1 1 d . . . H36A H 0.2922 1.0666 -0.0887 0.034 Uiso 1 1 calc R B . H36B H 0.2376 1.0180 -0.0423 0.034 Uiso 1 1 calc R . . C37 C 0.22804(12) 1.14343(13) -0.03308(11) 0.0345(5) Uani 1 1 d . B . H37A H 0.2080 1.1414 0.0124 0.041 Uiso 1 1 calc R . . H37B H 0.2627 1.1899 -0.0334 0.041 Uiso 1 1 calc R . . C38 C 0.16489(14) 1.15970(15) -0.08511(12) 0.0430(5) Uani 1 1 d . . . H38A H 0.1303 1.1131 -0.0859 0.052 Uiso 1 1 calc R B . H38B H 0.1846 1.1641 -0.1307 0.052 Uiso 1 1 calc R . . C39 C 0.12287(15) 1.23754(17) -0.07019(15) 0.0547(7) Uani 1 1 d . B . H39A H 0.1024 1.2324 -0.0250 0.066 Uiso 1 1 calc R . . H39B H 0.1579 1.2837 -0.0682 0.066 Uiso 1 1 calc R . . C40 C 0.0608(2) 1.2565(2) -0.1220(2) 0.0811(11) Uani 1 1 d . . . H40A H 0.0805 1.2618 -0.1669 0.122 Uiso 1 1 calc R B . H40B H 0.0371 1.3076 -0.1099 0.122 Uiso 1 1 calc R . . H40C H 0.0245 1.2123 -0.1228 0.122 Uiso 1 1 calc R . . C41 C 0.46761(10) 1.15468(11) 0.21983(9) 0.0223(4) Uani 1 1 d . B . H41A H 0.4156 1.1470 0.2029 0.027 Uiso 1 1 calc R . . H41B H 0.4677 1.1862 0.2626 0.027 Uiso 1 1 calc R . . C42 C 0.50796(12) 1.20337(12) 0.16753(10) 0.0307(4) Uani 1 1 d . . . H42A H 0.5617 1.2002 0.1791 0.037 Uiso 1 1 calc R B . H42B H 0.4983 1.1782 0.1223 0.037 Uiso 1 1 calc R . . C43 C 0.48515(15) 1.29220(14) 0.16369(14) 0.0483(6) Uani 1 1 d . B . H43A H 0.4893 1.3159 0.2099 0.058 Uiso 1 1 calc R . . H43B H 0.4328 1.2957 0.1467 0.058 Uiso 1 1 calc R . . C44 C 0.53220(16) 1.34220(16) 0.11733(16) 0.0546(7) Uani 1 1 d . . . H44A H 0.5849 1.3329 0.1310 0.066 Uiso 1 1 calc R B . H44B H 0.5234 1.3223 0.0702 0.066 Uiso 1 1 calc R . . C45 C 0.5171(2) 1.43259(19) 0.1186(2) 0.0750(10) Uani 1 1 d . B . H45A H 0.5249 1.4527 0.1658 0.090 Uiso 1 1 calc R . . H45B H 0.4649 1.4425 0.1035 0.090 Uiso 1 1 calc R . . C46 C 0.5667(3) 1.4799(3) 0.0731(3) 0.127(2) Uani 1 1 d . . . H46A H 0.6182 1.4641 0.0835 0.190 Uiso 1 1 calc R B . H46B H 0.5611 1.5383 0.0811 0.190 Uiso 1 1 calc R . . H46C H 0.5528 1.4675 0.0254 0.190 Uiso 1 1 calc R . . C47 C 0.24557(10) 1.05741(10) 0.36173(9) 0.0227(4) Uani 1 1 d . B . H47A H 0.2716 1.0982 0.3913 0.027 Uiso 1 1 calc R . . H47B H 0.2471 1.0763 0.3142 0.027 Uiso 1 1 calc R . . C48 C 0.16542(11) 1.05207(13) 0.38020(11) 0.0331(4) Uani 1 1 d . . . H48A H 0.1382 1.0164 0.3469 0.040 Uiso 1 1 calc R B . H48B H 0.1638 1.0262 0.4254 0.040 Uiso 1 1 calc R . . C49 C 0.12622(13) 1.13392(14) 0.38183(12) 0.0407(5) Uani 1 1 d . B . H49A H 0.0753 1.1249 0.3954 0.049 Uiso 1 1 calc R . . H49B H 0.1518 1.1684 0.4171 0.049 Uiso 1 1 calc R . . C50 C 0.12276(14) 1.17951(15) 0.31545(13) 0.0450(6) Uani 1 1 d . . . H50A H 0.1737 1.1921 0.3035 0.054 Uiso 1 1 calc R B . H50B H 0.1005 1.1436 0.2795 0.054 Uiso 1 1 calc R . . C51 C 0.07959(19) 1.25717(19) 0.31585(18) 0.0681(9) Uani 1 1 d . B . H51A H 0.0277 1.2435 0.3238 0.082 Uiso 1 1 calc R . . H51B H 0.0989 1.2904 0.3548 0.082 Uiso 1 1 calc R . . C52 C 0.0801(2) 1.3077(2) 0.2542(2) 0.0951(15) Uani 1 1 d . . . H52A H 0.1270 1.3371 0.2538 0.143 Uiso 1 1 calc R B . H52B H 0.0393 1.3468 0.2539 0.143 Uiso 1 1 calc R . . H52C H 0.0742 1.2728 0.2140 0.143 Uiso 1 1 calc R . . O1A O 0.30642(8) 0.97435(9) 0.55673(7) 0.0260(3) Uani 1 1 d . . . O1B O 0.28689(11) 0.78586(13) -0.17555(9) 0.0527(5) Uani 1 1 d . . . C1B C 0.2778(2) 0.8495(3) -0.2229(2) 0.0897(12) Uani 1 1 d . . . H1B1 H 0.2255 0.8543 -0.2380 0.134 Uiso 1 1 calc R . . H1B2 H 0.3068 0.8380 -0.2621 0.134 Uiso 1 1 calc R . . H1B3 H 0.2946 0.9007 -0.2017 0.134 Uiso 1 1 calc R . . O1C O 0.69819(11) 0.63583(13) 0.05925(13) 0.0725(7) Uani 1 1 d D . . C1C C 0.65275(19) 0.6513(2) -0.00234(19) 0.0746(10) Uani 1 1 d D . . H1C1 H 0.6006 0.6481 0.0075 0.112 Uiso 1 1 calc R . . H1C2 H 0.6634 0.6105 -0.0367 0.112 Uiso 1 1 calc R . . H1C3 H 0.6635 0.7057 -0.0195 0.112 Uiso 1 1 calc R . . O1D O 0.74133(14) 0.84800(16) 0.25761(13) 0.0790(7) Uani 1 1 d . . . C1D C 0.7781(2) 0.9214(3) 0.2676(2) 0.0879(11) Uani 1 1 d . . . H1D1 H 0.7509 0.9557 0.2981 0.132 Uiso 1 1 calc R . . H1D2 H 0.7814 0.9491 0.2239 0.132 Uiso 1 1 calc R . . H1D3 H 0.8278 0.9112 0.2879 0.132 Uiso 1 1 calc R . . C1N C 0.23774(10) 0.68101(11) 0.32011(9) 0.0245(4) Uani 1 1 d . . . C2N C 0.24643(11) 0.70165(12) -0.03207(10) 0.0278(4) Uani 1 1 d . . . C3N C 0.59044(11) 0.82463(12) 0.11746(10) 0.0286(4) Uani 1 1 d . . . C4N C 0.54470(10) 0.91858(11) 0.45252(9) 0.0233(4) Uani 1 1 d . . . H5O H 0.4472(17) 0.8442(18) -0.0122(15) 0.055(8) Uiso 1 1 d . . . H1A H 0.2852(15) 1.0206(18) 0.5515(14) 0.046(7) Uiso 1 1 d . . . H3O H 0.1343(16) 0.7068(19) 0.0393(15) 0.054(9) Uiso 1 1 d . . . H1O H 0.3229(15) 0.8309(16) 0.4190(13) 0.038(7) Uiso 1 1 d . . . H2A H 0.2724(16) 0.9393(18) 0.5637(14) 0.050(8) Uiso 1 1 d . . . H8O H 0.3648(15) 0.9376(16) 0.4908(14) 0.043(7) Uiso 1 1 d . . . H2O H 0.1557(14) 0.7318(16) 0.1618(15) 0.044(7) Uiso 1 1 d . . . H7O H 0.6230(16) 1.0071(18) 0.3766(16) 0.055(8) Uiso 1 1 d . . . H6O H 0.6036(15) 0.9656(17) 0.2514(15) 0.049(8) Uiso 1 1 d . . . H4O H 0.3320(16) 0.8069(18) -0.0955(16) 0.054(8) Uiso 1 1 d . . . H1B H 0.269(2) 0.736(2) -0.1958(18) 0.080(11) Uiso 1 1 d . . . H1D H 0.697(2) 0.861(2) 0.2336(19) 0.087(12) Uiso 1 1 d . . . C30' C 0.0494(5) 0.9799(6) 0.1763(5) 0.053(2) Uani 0.294(4) 1 d P B 2 H30C H 0.0607 0.9737 0.2258 0.064 Uiso 0.294(4) 1 calc PR B 2 H30D H 0.0141 0.9365 0.1616 0.064 Uiso 0.294(4) 1 calc PR B 2 C31' C 0.0140(9) 1.0616(10) 0.1627(9) 0.116(6) Uani 0.294(4) 1 d P B 2 H31C H -0.0289 1.0607 0.1914 0.139 Uiso 0.294(4) 1 calc PR B 2 H31D H 0.0494 1.1000 0.1856 0.139 Uiso 0.294(4) 1 calc PR B 2 C32' C -0.0091(2) 1.0993(3) 0.1126(2) 0.0874(13) Uani 0.29 1 d P B 2 H32C H -0.0511 1.0659 0.0945 0.105 Uiso 0.294(4) 1 calc PR B 2 H32D H 0.0300 1.0915 0.0804 0.105 Uiso 0.294(4) 1 calc PR B 2 C29' C 0.11830(11) 0.96908(12) 0.14063(10) 0.0293(5) Uani 0.29 1 d P B 2 H29C H 0.1556 1.0082 0.1594 0.035 Uiso 0.294(4) 1 calc PR B 2 H29D H 0.1082 0.9822 0.0920 0.035 Uiso 0.294(4) 1 calc PR B 2 H1C H 0.6761(15) 0.6598(14) 0.0965(8) 0.100 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 0.0421(8) 0.0203(7) 0.0263(7) 0.0047(5) -0.0097(6) -0.0037(6) N1 0.0467(10) 0.0203(8) 0.0334(9) 0.0037(7) 0.0026(8) 0.0009(7) C1 0.0215(8) 0.0153(8) 0.0230(8) 0.0018(6) 0.0033(7) 0.0000(6) O2 0.0377(8) 0.0173(6) 0.0237(7) -0.0017(5) 0.0008(6) -0.0057(5) N2 0.0430(10) 0.0274(9) 0.0436(10) -0.0119(8) 0.0092(8) -0.0068(8) C2 0.0213(8) 0.0158(8) 0.0215(8) -0.0005(6) 0.0033(6) -0.0013(6) O3 0.0348(8) 0.0250(7) 0.0259(7) -0.0062(6) 0.0034(6) -0.0127(6) N3 0.0460(11) 0.0347(10) 0.0440(11) -0.0022(8) 0.0043(9) 0.0142(9) C3 0.0237(8) 0.0191(8) 0.0211(8) 0.0015(6) 0.0023(7) 0.0002(7) O4 0.0300(7) 0.0347(8) 0.0283(7) -0.0138(6) 0.0072(6) -0.0065(6) N4 0.0324(9) 0.0327(9) 0.0290(8) 0.0055(7) -0.0007(7) 0.0051(7) C4 0.0249(9) 0.0152(8) 0.0239(8) 0.0015(6) 0.0036(7) -0.0009(6) O5 0.0332(8) 0.0292(7) 0.0274(7) -0.0112(6) 0.0015(6) 0.0027(6) C5 0.0227(8) 0.0180(8) 0.0220(8) -0.0026(6) 0.0049(7) -0.0025(6) O6 0.0293(7) 0.0386(8) 0.0244(7) -0.0053(6) -0.0041(6) 0.0109(6) C6 0.0201(8) 0.0178(8) 0.0203(8) -0.0001(6) 0.0035(6) -0.0003(6) O7 0.0202(6) 0.0448(8) 0.0205(6) 0.0011(6) -0.0004(5) -0.0004(6) C7 0.0222(8) 0.0196(8) 0.0216(8) -0.0004(6) 0.0005(7) -0.0008(6) O8 0.0301(7) 0.0235(6) 0.0214(6) 0.0060(5) 0.0028(5) 0.0011(5) C8 0.0256(9) 0.0170(8) 0.0201(8) -0.0013(6) -0.0015(7) -0.0008(6) C9 0.0233(8) 0.0195(8) 0.0180(8) 0.0003(6) -0.0015(6) -0.0003(6) C10 0.0244(9) 0.0213(8) 0.0217(8) 0.0008(7) -0.0022(7) -0.0038(7) C11 0.0273(9) 0.0194(8) 0.0225(8) -0.0036(7) -0.0016(7) -0.0027(7) C12 0.0245(9) 0.0233(9) 0.0223(8) -0.0037(7) 0.0006(7) -0.0013(7) C13 0.0240(8) 0.0189(8) 0.0196(8) -0.0003(6) -0.0010(7) -0.0018(7) C14 0.0246(8) 0.0199(8) 0.0180(8) -0.0017(6) 0.0013(7) -0.0024(7) C15 0.0223(8) 0.0186(8) 0.0204(8) -0.0002(6) 0.0037(6) -0.0010(6) C16 0.0230(8) 0.0193(8) 0.0193(8) 0.0005(6) 0.0027(7) -0.0032(6) C17 0.0266(9) 0.0213(8) 0.0207(8) -0.0022(6) 0.0052(7) -0.0029(7) C18 0.0257(9) 0.0226(9) 0.0234(8) -0.0001(7) 0.0063(7) 0.0025(7) C19 0.0232(8) 0.0257(9) 0.0194(8) 0.0022(7) 0.0023(7) 0.0006(7) C20 0.0236(8) 0.0193(8) 0.0191(8) 0.0005(6) 0.0035(6) -0.0014(6) C21 0.0196(8) 0.0214(8) 0.0190(8) -0.0011(6) 0.0012(6) -0.0013(6) C22 0.0228(8) 0.0168(8) 0.0188(8) -0.0013(6) -0.0014(6) 0.0007(6) C23 0.0243(8) 0.0178(8) 0.0181(8) -0.0018(6) 0.0005(6) -0.0008(6) C24 0.0226(8) 0.0225(8) 0.0206(8) -0.0035(7) 0.0014(7) -0.0002(7) C25 0.0262(9) 0.0195(8) 0.0183(8) -0.0012(6) -0.0029(7) 0.0031(7) C26 0.0268(9) 0.0165(8) 0.0191(8) -0.0006(6) 0.0018(7) -0.0004(7) C27 0.0232(8) 0.0159(8) 0.0193(8) -0.0031(6) 0.0003(6) -0.0002(6) C28 0.0243(8) 0.0163(8) 0.0186(8) 0.0002(6) 0.0018(6) -0.0009(6) C29 0.0293(10) 0.0272(10) 0.0314(10) 0.0028(8) 0.0010(8) 0.0064(8) C30 0.0454(18) 0.0420(18) 0.0310(15) 0.0026(13) -0.0120(13) 0.0151(14) C31 0.054(2) 0.050(2) 0.0444(19) 0.0162(16) -0.0019(16) 0.0218(17) C32 0.075(2) 0.094(3) 0.094(3) 0.031(2) 0.014(2) 0.036(2) C33 0.110(3) 0.096(3) 0.099(3) 0.032(2) 0.009(3) 0.057(3) C34 0.117(4) 0.141(5) 0.142(4) 0.045(4) 0.038(3) 0.080(4) C35 0.0282(9) 0.0203(8) 0.0221(8) 0.0017(7) -0.0001(7) -0.0022(7) C36 0.0329(10) 0.0257(9) 0.0255(9) 0.0026(7) -0.0034(8) -0.0005(8) C37 0.0367(11) 0.0327(11) 0.0336(11) 0.0019(8) -0.0025(9) 0.0051(9) C38 0.0426(13) 0.0457(13) 0.0396(12) 0.0048(10) -0.0074(10) 0.0071(10) C39 0.0495(15) 0.0514(15) 0.0617(17) 0.0067(13) -0.0087(13) 0.0146(12) C40 0.066(2) 0.087(3) 0.087(2) 0.013(2) -0.0212(18) 0.0289(18) C41 0.0259(9) 0.0200(8) 0.0211(8) -0.0016(6) 0.0020(7) -0.0021(7) C42 0.0340(10) 0.0261(10) 0.0328(10) 0.0038(8) 0.0091(8) -0.0015(8) C43 0.0531(14) 0.0331(12) 0.0605(16) 0.0120(11) 0.0187(12) 0.0048(10) C44 0.0532(15) 0.0442(14) 0.0677(18) 0.0161(13) 0.0141(13) 0.0043(12) C45 0.072(2) 0.0462(17) 0.109(3) 0.0217(17) 0.0247(19) 0.0032(14) C46 0.127(4) 0.072(3) 0.187(5) 0.052(3) 0.057(4) 0.000(3) C47 0.0263(9) 0.0176(8) 0.0243(8) -0.0021(7) 0.0031(7) 0.0004(7) C48 0.0317(10) 0.0297(10) 0.0389(11) 0.0058(8) 0.0113(9) 0.0055(8) C49 0.0394(12) 0.0401(12) 0.0432(12) -0.0030(10) 0.0079(10) 0.0143(10) C50 0.0479(13) 0.0366(12) 0.0522(14) 0.0075(10) 0.0178(11) 0.0129(10) C51 0.074(2) 0.0488(17) 0.082(2) 0.0114(15) 0.0124(17) 0.0278(15) C52 0.098(3) 0.067(2) 0.128(3) 0.054(2) 0.068(3) 0.048(2) O1A 0.0278(7) 0.0219(7) 0.0282(7) 0.0028(5) 0.0011(5) -0.0020(6) O1B 0.0583(11) 0.0583(12) 0.0401(9) -0.0021(8) -0.0084(8) -0.0096(9) C1B 0.077(2) 0.110(3) 0.081(2) 0.041(2) -0.0105(19) -0.015(2) O1C 0.0485(11) 0.0587(12) 0.1089(18) -0.0365(12) -0.0063(11) 0.0198(9) C1C 0.0609(19) 0.078(2) 0.085(2) -0.0315(19) 0.0002(17) 0.0081(16) O1D 0.0686(15) 0.0834(17) 0.0814(16) 0.0160(13) -0.0252(13) 0.0189(13) C1D 0.081(2) 0.096(3) 0.083(3) 0.003(2) -0.021(2) 0.010(2) C1N 0.0294(9) 0.0211(9) 0.0230(8) 0.0004(7) 0.0024(7) -0.0012(7) C2N 0.0287(9) 0.0272(10) 0.0277(9) -0.0046(8) 0.0040(8) -0.0051(8) C3N 0.0321(10) 0.0279(10) 0.0262(9) -0.0014(7) 0.0041(8) 0.0026(8) C4N 0.0259(9) 0.0225(9) 0.0215(8) 0.0002(7) 0.0017(7) 0.0009(7) C30' 0.047(5) 0.046(5) 0.067(6) -0.007(4) 0.010(4) 0.014(4) C31' 0.095(10) 0.105(11) 0.149(15) 0.050(11) 0.021(10) 0.071(9) C32' 0.075(2) 0.094(3) 0.094(3) 0.031(2) 0.014(2) 0.036(2) C29' 0.0293(10) 0.0272(10) 0.0314(10) 0.0028(8) 0.0010(8) 0.0064(8) _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 C3 1.360(2) . ? O1 H1O 0.76(3) . ? N1 C1N 1.145(2) . ? C1 C2 1.396(2) . ? C1 C6 1.396(2) . ? C1 H1 0.9500 . ? O2 C5 1.355(2) . ? O2 H2O 0.84(3) . ? N2 C2N 1.142(3) . ? C2 C3 1.400(2) . ? C2 C28 1.530(2) . ? O3 C10 1.367(2) . ? O3 H3O 0.78(3) . ? N3 C3N 1.143(3) . ? C3 C4 1.401(2) . ? O4 C12 1.366(2) . ? O4 H4O 0.82(3) . ? N4 C4N 1.141(2) . ? C4 C5 1.400(2) . ? C4 C1N 1.435(2) . ? O5 C17 1.356(2) . ? O5 H5O 0.84(3) . ? C5 C6 1.396(2) . ? O6 C19 1.365(2) . ? O6 H6O 0.86(3) . ? C6 C7 1.527(2) . ? O7 C24 1.371(2) . ? O7 H7O 0.87(3) . ? C7 C9 1.532(2) . ? C7 C29 1.538(3) . ? C7 H7 1.0000 . ? O8 C26 1.378(2) . ? O8 H8O 0.90(3) . ? C8 C13 1.391(2) . ? C8 C9 1.391(2) . ? C8 H8 0.9500 . ? C9 C10 1.395(2) . ? C10 C11 1.406(3) . ? C11 C12 1.406(3) . ? C11 C2N 1.435(3) . ? C12 C13 1.394(2) . ? C13 C14 1.528(2) . ? C14 C16 1.534(2) . ? C14 C35 1.537(2) . ? C14 H14 1.0000 . ? C15 C16 1.397(2) . ? C15 C20 1.399(2) . ? C15 H15 0.9500 . ? C16 C17 1.398(3) . ? C17 C18 1.407(3) . ? C18 C19 1.403(3) . ? C18 C3N 1.435(3) . ? C19 C20 1.393(2) . ? C20 C21 1.526(2) . ? C21 C23 1.531(2) . ? C21 C41 1.538(2) . ? C21 H21 1.0000 . ? C22 C23 1.397(2) . ? C22 C27 1.403(2) . ? C22 H22 0.9500 . ? C23 C24 1.392(2) . ? C24 C25 1.403(2) . ? C25 C26 1.402(3) . ? C25 C4N 1.434(2) . ? C26 C27 1.393(2) . ? C27 C28 1.526(2) . ? C28 C47 1.536(2) . ? C28 H28 1.0000 . ? C29 C30 1.484(3) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30 C31 1.541(5) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.495(5) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C32 C33 1.555(5) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C33 C34 1.494(6) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C35 C36 1.530(3) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 C37 1.525(3) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C37 C38 1.516(3) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.527(4) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C39 C40 1.507(4) . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C41 C42 1.528(3) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? C42 C43 1.518(3) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.529(3) . ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C44 C45 1.511(4) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.523(5) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.525(3) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 C49 1.523(3) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.507(3) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.498(3) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? C51 C52 1.473(5) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? O1A H1A 0.86(3) . ? O1A H2A 0.86(3) . ? O1B C1B 1.406(4) . ? O1B H1B 0.96(4) . ? C1B H1B1 0.9800 . ? C1B H1B2 0.9800 . ? C1B H1B3 0.9800 . ? O1C C1C 1.450(4) . ? O1C H1C 0.944(14) . ? C1C H1C1 0.9800 . ? C1C H1C2 0.9800 . ? C1C H1C3 0.9800 . ? O1D C1D 1.386(5) . ? O1D H1D 0.94(4) . ? C1D H1D1 0.9800 . ? C1D H1D2 0.9800 . ? C1D H1D3 0.9800 . ? C30' C31' 1.507(14) . ? C30' H30C 0.9900 . ? C30' H30D 0.9900 . ? C31' H31C 0.9900 . ? C31' H31D 0.9900 . ? 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 C3 O1 H1O 115(2) . . ? C2 C1 C6 124.25(16) . . ? C2 C1 H1 117.9 . . ? C6 C1 H1 117.9 . . ? C5 O2 H2O 110.8(19) . . ? C1 C2 C3 117.41(15) . . ? C1 C2 C28 122.58(15) . . ? C3 C2 C28 120.01(15) . . ? C10 O3 H3O 116(2) . . ? O1 C3 C2 125.16(16) . . ? O1 C3 C4 115.07(15) . . ? C2 C3 C4 119.77(16) . . ? C12 O4 H4O 113(2) . . ? C5 C4 C3 121.16(16) . . ? C5 C4 C1N 118.01(16) . . ? C3 C4 C1N 120.80(16) . . ? C17 O5 H5O 115(2) . . ? O2 C5 C6 124.61(16) . . ? O2 C5 C4 115.16(15) . . ? C6 C5 C4 120.23(16) . . ? C19 O6 H6O 111.2(19) . . ? C1 C6 C5 117.15(16) . . ? C1 C6 C7 123.35(15) . . ? C5 C6 C7 119.48(15) . . ? C24 O7 H7O 113.6(19) . . ? C6 C7 C9 109.47(14) . . ? C6 C7 C29 113.80(15) . . ? C9 C7 C29 111.96(14) . . ? C6 C7 H7 107.1 . . ? C9 C7 H7 107.1 . . ? C29 C7 H7 107.1 . . ? C26 O8 H8O 113.0(17) . . ? C13 C8 C9 123.81(16) . . ? C13 C8 H8 118.1 . . ? C9 C8 H8 118.1 . . ? C8 C9 C10 117.66(16) . . ? C8 C9 C7 120.99(15) . . ? C10 C9 C7 121.34(15) . . ? O3 C10 C9 117.05(16) . . ? O3 C10 C11 122.63(16) . . ? C9 C10 C11 120.23(16) . . ? C10 C11 C12 120.14(16) . . ? C10 C11 C2N 119.87(16) . . ? C12 C11 C2N 119.73(17) . . ? O4 C12 C13 119.01(16) . . ? O4 C12 C11 120.64(16) . . ? C13 C12 C11 120.23(16) . . ? C8 C13 C12 117.71(16) . . ? C8 C13 C14 120.88(15) . . ? C12 C13 C14 121.40(16) . . ? C13 C14 C16 109.93(14) . . ? C13 C14 C35 110.31(14) . . ? C16 C14 C35 113.21(14) . . ? C13 C14 H14 107.7 . . ? C16 C14 H14 107.7 . . ? C35 C14 H14 107.7 . . ? C16 C15 C20 124.67(16) . . ? C16 C15 H15 117.7 . . ? C20 C15 H15 117.7 . . ? C15 C16 C17 117.25(16) . . ? C15 C16 C14 121.90(16) . . ? C17 C16 C14 120.78(15) . . ? O5 C17 C16 124.97(16) . . ? O5 C17 C18 115.27(16) . . ? C16 C17 C18 119.76(16) . . ? C19 C18 C17 121.02(16) . . ? C19 C18 C3N 118.39(17) . . ? C17 C18 C3N 120.40(17) . . ? O6 C19 C20 124.27(16) . . ? O6 C19 C18 115.32(16) . . ? C20 C19 C18 120.40(16) . . ? C19 C20 C15 116.86(16) . . ? C19 C20 C21 120.84(15) . . ? C15 C20 C21 122.26(15) . . ? C20 C21 C23 110.42(14) . . ? C20 C21 C41 114.43(14) . . ? C23 C21 C41 112.10(14) . . ? C20 C21 H21 106.4 . . ? C23 C21 H21 106.4 . . ? C41 C21 H21 106.4 . . ? C23 C22 C27 123.35(16) . . ? C23 C22 H22 118.3 . . ? C27 C22 H22 118.3 . . ? C24 C23 C22 117.87(16) . . ? C24 C23 C21 119.81(15) . . ? C22 C23 C21 122.29(15) . . ? O7 C24 C23 118.15(16) . . ? O7 C24 C25 121.38(16) . . ? C23 C24 C25 120.37(16) . . ? C26 C25 C24 120.24(16) . . ? C26 C25 C4N 118.80(16) . . ? C24 C25 C4N 120.88(16) . . ? O8 C26 C27 122.55(16) . . ? O8 C26 C25 116.60(15) . . ? C27 C26 C25 120.67(16) . . ? C26 C27 C22 117.44(16) . . ? C26 C27 C28 120.39(15) . . ? C22 C27 C28 122.14(15) . . ? C27 C28 C2 110.67(14) . . ? C27 C28 C47 111.97(14) . . ? C2 C28 C47 114.58(14) . . ? C27 C28 H28 106.3 . . ? C2 C28 H28 106.3 . . ? C47 C28 H28 106.3 . . ? C30 C29 C7 115.00(19) . . ? C30 C29 H29A 108.5 . . ? C7 C29 H29A 108.5 . . ? C30 C29 H29B 108.5 . . ? C7 C29 H29B 108.5 . . ? H29A C29 H29B 107.5 . . ? C29 C30 C31 113.8(3) . . ? C29 C30 H30A 108.8 . . ? C31 C30 H30A 108.8 . . ? C29 C30 H30B 108.8 . . ? C31 C30 H30B 108.8 . . ? H30A C30 H30B 107.7 . . ? C32 C31 C30 113.7(3) . . ? C32 C31 H31A 108.8 . . ? C30 C31 H31A 108.8 . . ? C32 C31 H31B 108.8 . . ? C30 C31 H31B 108.8 . . ? H31A C31 H31B 107.7 . . ? C31 C32 C33 111.2(3) . . ? C31 C32 H32A 109.4 . . ? C33 C32 H32A 109.4 . . ? C31 C32 H32B 109.4 . . ? C33 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? C34 C33 C32 110.4(4) . . ? C34 C33 H33A 109.6 . . ? C32 C33 H33A 109.6 . . ? C34 C33 H33B 109.6 . . ? C32 C33 H33B 109.6 . . ? H33A C33 H33B 108.1 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C36 C35 C14 114.12(15) . . ? C36 C35 H35A 108.7 . . ? C14 C35 H35A 108.7 . . ? C36 C35 H35B 108.7 . . ? C14 C35 H35B 108.7 . . ? H35A C35 H35B 107.6 . . ? C37 C36 C35 110.79(16) . . ? C37 C36 H36A 109.5 . . ? C35 C36 H36A 109.5 . . ? C37 C36 H36B 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 108.1 . . ? C38 C37 C36 115.55(18) . . ? C38 C37 H37A 108.4 . . ? C36 C37 H37A 108.4 . . ? C38 C37 H37B 108.4 . . ? C36 C37 H37B 108.4 . . ? H37A C37 H37B 107.5 . . ? C37 C38 C39 112.6(2) . . ? C37 C38 H38A 109.1 . . ? C39 C38 H38A 109.1 . . ? C37 C38 H38B 109.1 . . ? C39 C38 H38B 109.1 . . ? H38A C38 H38B 107.8 . . ? C40 C39 C38 113.8(3) . . ? C40 C39 H39A 108.8 . . ? C38 C39 H39A 108.8 . . ? C40 C39 H39B 108.8 . . ? C38 C39 H39B 108.8 . . ? H39A C39 H39B 107.7 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C21 112.69(15) . . ? C42 C41 H41A 109.1 . . ? C21 C41 H41A 109.1 . . ? C42 C41 H41B 109.1 . . ? C21 C41 H41B 109.1 . . ? H41A C41 H41B 107.8 . . ? C43 C42 C41 113.35(17) . . ? C43 C42 H42A 108.9 . . ? C41 C42 H42A 108.9 . . ? C43 C42 H42B 108.9 . . ? C41 C42 H42B 108.9 . . ? H42A C42 H42B 107.7 . . ? C42 C43 C44 112.7(2) . . ? C42 C43 H43A 109.1 . . ? C44 C43 H43A 109.1 . . ? C42 C43 H43B 109.1 . . ? C44 C43 H43B 109.1 . . ? H43A C43 H43B 107.8 . . ? C45 C44 C43 114.2(2) . . ? C45 C44 H44A 108.7 . . ? C43 C44 H44A 108.7 . . ? C45 C44 H44B 108.7 . . ? C43 C44 H44B 108.7 . . ? H44A C44 H44B 107.6 . . ? C44 C45 C46 112.1(3) . . ? C44 C45 H45A 109.2 . . ? C46 C45 H45A 109.2 . . ? C44 C45 H45B 109.2 . . ? C46 C45 H45B 109.2 . . ? H45A C45 H45B 107.9 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 C28 112.73(15) . . ? C48 C47 H47A 109.0 . . ? C28 C47 H47A 109.0 . . ? C48 C47 H47B 109.0 . . ? C28 C47 H47B 109.0 . . ? H47A C47 H47B 107.8 . . ? C49 C48 C47 114.13(18) . . ? C49 C48 H48A 108.7 . . ? C47 C48 H48A 108.7 . . ? C49 C48 H48B 108.7 . . ? C47 C48 H48B 108.7 . . ? H48A C48 H48B 107.6 . . ? C50 C49 C48 114.55(19) . . ? C50 C49 H49A 108.6 . . ? C48 C49 H49A 108.6 . . ? C50 C49 H49B 108.6 . . ? C48 C49 H49B 108.6 . . ? H49A C49 H49B 107.6 . . ? C51 C50 C49 114.4(2) . . ? C51 C50 H50A 108.7 . . ? C49 C50 H50A 108.7 . . ? C51 C50 H50B 108.7 . . ? C49 C50 H50B 108.7 . . ? H50A C50 H50B 107.6 . . ? C52 C51 C50 116.5(3) . . ? C52 C51 H51A 108.2 . . ? C50 C51 H51A 108.2 . . ? C52 C51 H51B 108.2 . . ? C50 C51 H51B 108.2 . . ? H51A C51 H51B 107.3 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? H1A O1A H2A 107(3) . . ? C1B O1B H1B 109(2) . . ? O1B C1B H1B1 109.5 . . ? O1B C1B H1B2 109.5 . . ? H1B1 C1B H1B2 109.5 . . ? O1B C1B H1B3 109.5 . . ? H1B1 C1B H1B3 109.5 . . ? H1B2 C1B H1B3 109.5 . . ? C1C O1C H1C 109.4(13) . . ? O1C C1C H1C1 109.5 . . ? O1C C1C H1C2 109.5 . . ? H1C1 C1C H1C2 109.5 . . ? O1C C1C H1C3 109.5 . . ? H1C1 C1C H1C3 109.5 . . ? H1C2 C1C H1C3 109.5 . . ? C1D O1D H1D 105(2) . . ? O1D C1D H1D1 109.5 . . ? O1D C1D H1D2 109.5 . . ? H1D1 C1D H1D2 109.5 . . ? O1D C1D H1D3 109.5 . . ? H1D1 C1D H1D3 109.5 . . ? H1D2 C1D H1D3 109.5 . . ? N1 C1N C4 176.4(2) . . ? N2 C2N C11 176.2(2) . . ? N3 C3N C18 177.1(2) . . ? N4 C4N C25 178.6(2) . . ? C31' C30' H30C 109.0 . . ? C31' C30' H30D 109.0 . . ? H30C C30' H30D 107.8 . . ? C30' C31' H31C 103.2 . . ? C30' C31' H31D 103.2 . . ? H31C C31' H31D 105.1 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C6 C1 C2 C3 1.2(3) . . . . ? C6 C1 C2 C28 -179.33(16) . . . . ? C1 C2 C3 O1 178.20(16) . . . . ? C28 C2 C3 O1 -1.3(3) . . . . ? C1 C2 C3 C4 -1.9(3) . . . . ? C28 C2 C3 C4 178.64(15) . . . . ? O1 C3 C4 C5 -178.19(16) . . . . ? C2 C3 C4 C5 1.9(3) . . . . ? O1 C3 C4 C1N 0.0(3) . . . . ? C2 C3 C4 C1N -179.92(17) . . . . ? C3 C4 C5 O2 178.47(16) . . . . ? C1N C4 C5 O2 0.2(2) . . . . ? C3 C4 C5 C6 -1.1(3) . . . . ? C1N C4 C5 C6 -179.34(16) . . . . ? C2 C1 C6 C5 -0.5(3) . . . . ? C2 C1 C6 C7 -178.98(16) . . . . ? O2 C5 C6 C1 -179.17(16) . . . . ? C4 C5 C6 C1 0.4(2) . . . . ? O2 C5 C6 C7 -0.6(3) . . . . ? C4 C5 C6 C7 178.95(15) . . . . ? C1 C6 C7 C9 100.95(19) . . . . ? C5 C6 C7 C9 -77.53(19) . . . . ? C1 C6 C7 C29 -25.2(2) . . . . ? C5 C6 C7 C29 156.35(16) . . . . ? C13 C8 C9 C10 3.9(3) . . . . ? C13 C8 C9 C7 -177.32(16) . . . . ? C6 C7 C9 C8 -75.2(2) . . . . ? C29 C7 C9 C8 51.9(2) . . . . ? C6 C7 C9 C10 103.55(18) . . . . ? C29 C7 C9 C10 -129.29(17) . . . . ? C8 C9 C10 O3 176.80(15) . . . . ? C7 C9 C10 O3 -2.0(2) . . . . ? C8 C9 C10 C11 0.0(3) . . . . ? C7 C9 C10 C11 -178.78(16) . . . . ? O3 C10 C11 C12 179.71(16) . . . . ? C9 C10 C11 C12 -3.7(3) . . . . ? O3 C10 C11 C2N -6.1(3) . . . . ? C9 C10 C11 C2N 170.44(17) . . . . ? C10 C11 C12 O4 179.76(17) . . . . ? C2N C11 C12 O4 5.6(3) . . . . ? C10 C11 C12 C13 3.7(3) . . . . ? C2N C11 C12 C13 -170.44(17) . . . . ? C9 C8 C13 C12 -3.9(3) . . . . ? C9 C8 C13 C14 174.85(16) . . . . ? O4 C12 C13 C8 -176.15(16) . . . . ? C11 C12 C13 C8 0.0(3) . . . . ? O4 C12 C13 C14 5.2(3) . . . . ? C11 C12 C13 C14 -178.74(16) . . . . ? C8 C13 C14 C16 77.6(2) . . . . ? C12 C13 C14 C16 -103.77(19) . . . . ? C8 C13 C14 C35 -48.0(2) . . . . ? C12 C13 C14 C35 130.70(17) . . . . ? C20 C15 C16 C17 1.7(3) . . . . ? C20 C15 C16 C14 178.62(16) . . . . ? C13 C14 C16 C15 -101.24(18) . . . . ? C35 C14 C16 C15 22.6(2) . . . . ? C13 C14 C16 C17 75.6(2) . . . . ? C35 C14 C16 C17 -160.56(16) . . . . ? C15 C16 C17 O5 178.77(16) . . . . ? C14 C16 C17 O5 1.8(3) . . . . ? C15 C16 C17 C18 -0.5(2) . . . . ? C14 C16 C17 C18 -177.50(16) . . . . ? O5 C17 C18 C19 179.27(16) . . . . ? C16 C17 C18 C19 -1.4(3) . . . . ? O5 C17 C18 C3N -5.8(3) . . . . ? C16 C17 C18 C3N 173.54(17) . . . . ? C17 C18 C19 O6 -178.82(16) . . . . ? C3N C18 C19 O6 6.2(2) . . . . ? C17 C18 C19 C20 2.2(3) . . . . ? C3N C18 C19 C20 -172.76(17) . . . . ? O6 C19 C20 C15 -179.97(16) . . . . ? C18 C19 C20 C15 -1.1(2) . . . . ? O6 C19 C20 C21 -2.2(3) . . . . ? C18 C19 C20 C21 176.61(16) . . . . ? C16 C15 C20 C19 -0.9(3) . . . . ? C16 C15 C20 C21 -178.56(16) . . . . ? C19 C20 C21 C23 -77.7(2) . . . . ? C15 C20 C21 C23 99.88(19) . . . . ? C19 C20 C21 C41 154.68(16) . . . . ? C15 C20 C21 C41 -27.7(2) . . . . ? C27 C22 C23 C24 1.0(3) . . . . ? C27 C22 C23 C21 179.19(15) . . . . ? C20 C21 C23 C24 100.56(18) . . . . ? C41 C21 C23 C24 -130.59(17) . . . . ? C20 C21 C23 C22 -77.5(2) . . . . ? C41 C21 C23 C22 51.3(2) . . . . ? C22 C23 C24 O7 177.57(15) . . . . ? C21 C23 C24 O7 -0.6(2) . . . . ? C22 C23 C24 C25 1.2(2) . . . . ? C21 C23 C24 C25 -177.03(15) . . . . ? O7 C24 C25 C26 -179.31(16) . . . . ? C23 C24 C25 C26 -3.0(3) . . . . ? O7 C24 C25 C4N -2.7(3) . . . . ? C23 C24 C25 C4N 173.60(16) . . . . ? C24 C25 C26 O8 177.94(15) . . . . ? C4N C25 C26 O8 1.3(2) . . . . ? C24 C25 C26 C27 2.7(3) . . . . ? C4N C25 C26 C27 -173.99(16) . . . . ? O8 C26 C27 C22 -175.50(15) . . . . ? C25 C26 C27 C22 -0.5(2) . . . . ? O8 C26 C27 C28 2.4(2) . . . . ? C25 C26 C27 C28 177.41(15) . . . . ? C23 C22 C27 C26 -1.4(2) . . . . ? C23 C22 C27 C28 -179.27(15) . . . . ? C26 C27 C28 C2 -102.69(18) . . . . ? C22 C27 C28 C2 75.2(2) . . . . ? C26 C27 C28 C47 128.14(17) . . . . ? C22 C27 C28 C47 -54.0(2) . . . . ? C1 C2 C28 C27 -98.66(19) . . . . ? C3 C2 C28 C27 80.76(19) . . . . ? C1 C2 C28 C47 29.1(2) . . . . ? C3 C2 C28 C47 -151.49(16) . . . . ? C6 C7 C29 C30 -175.1(2) . . . . ? C9 C7 C29 C30 60.1(3) . . . . ? C7 C29 C30 C31 -173.8(2) . . . . ? C29 C30 C31 C32 -72.0(4) . . . . ? C30 C31 C32 C33 -175.5(4) . . . . ? C31 C32 C33 C34 -179.0(4) . . . . ? C13 C14 C35 C36 -58.99(19) . . . . ? C16 C14 C35 C36 177.36(15) . . . . ? C14 C35 C36 C37 166.53(16) . . . . ? C35 C36 C37 C38 179.62(18) . . . . ? C36 C37 C38 C39 178.3(2) . . . . ? C37 C38 C39 C40 178.6(3) . . . . ? C20 C21 C41 C42 -65.7(2) . . . . ? C23 C21 C41 C42 167.57(15) . . . . ? C21 C41 C42 C43 -167.24(19) . . . . ? C41 C42 C43 C44 173.3(2) . . . . ? C42 C43 C44 C45 -173.2(3) . . . . ? C43 C44 C45 C46 178.5(4) . . . . ? C27 C28 C47 C48 -170.49(15) . . . . ? C2 C28 C47 C48 62.4(2) . . . . ? C28 C47 C48 C49 172.75(17) . . . . ? C47 C48 C49 C50 59.9(3) . . . . ? C48 C49 C50 C51 175.9(2) . . . . ? C49 C50 C51 C52 174.7(3) . . . . ? C5 C4 C1N N1 -12(3) . . . . ? C3 C4 C1N N1 170(3) . . . . ? C10 C11 C2N N2 -59(3) . . . . ? C12 C11 C2N N2 115(3) . . . . ? C19 C18 C3N N3 34(4) . . . . ? C17 C18 C3N N3 -141(4) . . . . ? C26 C25 C4N N4 108(9) . . . . ? C24 C25 C4N N4 -68(9) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5O O4 0.84(3) 1.96(3) 2.772(2) 163(3) . O1A H1A N2 0.86(3) 2.02(3) 2.856(2) 167(3) 2 O3 H3O N4 0.78(3) 1.99(3) 2.732(2) 160(3) 4_575 O1 H1O O8 0.76(3) 2.07(3) 2.831(2) 178(3) . O1A H2A O1C 0.86(3) 1.83(3) 2.675(2) 168(3) 4_576 O8 H8O O1A 0.90(3) 1.83(3) 2.708(2) 165(2) . O2 H2O O3 0.84(3) 1.91(3) 2.729(2) 164(3) . O7 H7O O1A 0.87(3) 1.81(3) 2.661(2) 167(3) 3_676 O6 H6O O7 0.86(3) 1.85(3) 2.699(2) 167(3) . O4 H4O O1B 0.82(3) 1.77(3) 2.583(2) 174(3) . O1B H1B O1D 0.96(4) 1.72(4) 2.670(3) 172(3) 4_575 O1D H1D O6 0.94(4) 2.05(4) 2.916(3) 151(3) . O1C H1C N3 0.944(14) 2.071(16) 2.848(3) 138.6(18) . _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.625 _refine_diff_density_min -0.458 _refine_diff_density_rms 0.059 data_C-hexytetracyanoresorcinarene/Ag _database_code_depnum_ccdc_archive 'CCDC 908887' #TrackingRef '15895_web_deposit_cif_file_1_AndrewMossine_1354649190.RESCNAG.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ? _chemical_name_common 'C-hexyltetracyanoresorcin(4)arene silver complex' _chemical_formula_moiety 'C56 H68 N4 O8 Ag1, 3.6(C1H4O1), 0.3(H2O)' _chemical_formula_sum 'C59.60 H83 Ag N4 O11.90' _exptl_crystal_recrystallization_method '8:1 methanol:water' _chemical_melting_point ? _exptl_crystal_description rod _exptl_crystal_colour yellow _diffrn_ambient_temperature 173(2) _chemical_formula_weight 1153.7990 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 orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_int_tables_number 19 _chemical_absolute_configuration ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 15.6936(18) _cell_length_b 15.9984(19) _cell_length_c 26.489(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 6650.6(13) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9901 _cell_measurement_theta_min 2.381 _cell_measurement_theta_max 22.326 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.137 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2439 _exptl_absorpt_coefficient_mu 0.359 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.82 _exptl_absorpt_correction_T_max 0.95 _exptl_absorpt_process_details ; Data were corrected for decay and absorption using the program SADABS (Sheldrick, G. M. (2003). SADABS. Version 2.10. University of G\"ottingen, Germany). ; _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0.0 _diffrn_reflns_number 77688 _diffrn_reflns_av_R_equivalents 0.0467 _diffrn_reflns_av_sigmaI/netI 0.0428 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.49 _diffrn_reflns_theta_max 27.50 _reflns_number_total 15196 _reflns_number_gt 8239 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 (Bruker AXS, 2008)' _computing_cell_refinement 'APEX2 (Bruker AXS, 2008)' _computing_data_reduction 'APEX2 (Bruker AXS, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-SEED, Barbour, 2001' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _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. The crystal was a racemic twin so the TWIN command was used during refinement. It is unlikely that all possible positions of c-hexyl tails and solvent molecules have been accounted for due to a high level of disorder within these parts of the structure. However, all major parts have been modeled to the best of our ability. ; _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^)+(0.2000P)^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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.50(5) _refine_ls_number_reflns 15196 _refine_ls_number_parameters 670 _refine_ls_number_restraints 50 _refine_ls_R_factor_all 0.1634 _refine_ls_R_factor_gt 0.1058 _refine_ls_wR_factor_ref 0.3363 _refine_ls_wR_factor_gt 0.2857 _refine_ls_goodness_of_fit_ref 1.119 _refine_ls_restrained_S_all 1.121 _refine_ls_shift/su_max 0.059 _refine_ls_shift/su_mean 0.002 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 1.01634(5) 0.75528(4) 0.13889(3) 0.1035(3) Uani 1 1 d . . . O6 O 0.8532(4) 0.5926(3) 0.5429(2) 0.0851(16) Uani 1 1 d D . . C8 C 0.6790(5) 0.9158(4) 0.4105(3) 0.067(2) Uani 1 1 d . . . H8 H 0.6354 0.8750 0.4137 0.081 Uiso 1 1 calc R . . O2 O 0.7973(4) 0.8967(3) 0.2512(2) 0.0894(16) Uani 1 1 d D D . C15 C 0.6937(3) 0.7491(4) 0.5032(2) 0.0572(12) Uani 1 1 d . . . H15 H 0.6379 0.7521 0.4894 0.069 Uiso 1 1 calc R . . C20 C 0.7283(5) 0.6679(4) 0.5119(3) 0.0634(18) Uani 1 1 d . . . C17 C 0.8180(4) 0.8162(4) 0.5335(3) 0.0623(16) Uani 1 1 d . . . C2 C 0.6699(6) 0.6803(5) 0.2969(3) 0.078(2) Uani 1 1 d . D . C16 C 0.7346(4) 0.8237(4) 0.5133(3) 0.0593(16) Uani 1 1 d . D . C28 C 0.6282(7) 0.6000(6) 0.3094(3) 0.093(3) Uani 1 1 d . . . H28 H 0.6365 0.5607 0.2804 0.111 Uiso 1 1 calc R . . O5 O 0.8683(3) 0.8839(3) 0.5445(2) 0.0789(14) Uani 1 1 d D . . C21 C 0.6766(4) 0.5897(4) 0.5005(3) 0.070(2) Uani 1 1 d . . . H21 H 0.6977 0.5460 0.5245 0.085 Uiso 1 1 calc R . . N3 N 1.0081(5) 0.7332(5) 0.5775(3) 0.100(2) Uani 1 1 d . . . O1 O 0.7758(4) 0.6052(4) 0.2461(2) 0.0937(18) Uani 1 1 d D D . C3N C 0.9393(5) 0.7328(5) 0.5621(3) 0.081(2) Uani 1 1 d . . . C27 C 0.6730(6) 0.5620(4) 0.3572(4) 0.084(2) Uani 1 1 d . . . O3 O 0.7880(5) 1.0325(3) 0.3117(2) 0.0924(18) Uani 1 1 d D D . C4 C 0.7823(4) 0.7511(5) 0.2501(2) 0.0710(16) Uani 1 1 d . D . C1 C 0.6448(4) 0.7593(4) 0.3111(3) 0.0732(17) Uani 1 1 d . . . H1A H 0.5976 0.7629 0.3335 0.088 Uiso 1 1 calc R . . C23 C 0.6978(5) 0.5589(4) 0.4496(3) 0.072(2) Uani 1 1 d . . . C13 C 0.7200(5) 0.9421(4) 0.4530(3) 0.0628(17) Uani 1 1 d . D . C9 C 0.6993(5) 0.9474(4) 0.3605(3) 0.0664(17) Uani 1 1 d . D . C22 C 0.6602(6) 0.5915(5) 0.4054(3) 0.074(2) Uani 1 1 d . . . H22 H 0.6229 0.6377 0.4093 0.089 Uiso 1 1 calc R . . C11 C 0.8071(5) 1.0307(4) 0.4008(3) 0.0697(19) Uani 1 1 d . D . C41 C 0.5808(6) 0.5979(5) 0.5106(4) 0.082(2) Uani 1 1 d . . . H41A H 0.5578 0.6405 0.4872 0.098 Uiso 1 1 calc R . . H41B H 0.5536 0.5440 0.5018 0.098 Uiso 1 1 calc R . . O4 O 0.8263(4) 1.0229(3) 0.4904(2) 0.0874(16) Uani 1 1 d D D . C7 C 0.6464(5) 0.9176(5) 0.3159(3) 0.077(2) Uani 1 1 d . . . H7 H 0.6587 0.9581 0.2881 0.093 Uiso 1 1 calc R A 1 C26 C 0.7305(7) 0.4961(5) 0.3513(4) 0.103(4) Uani 1 1 d . . . C10 C 0.7631(5) 1.0040(4) 0.3577(3) 0.0718(19) Uani 1 1 d . . . C18 C 0.8549(4) 0.7380(5) 0.5418(2) 0.0668(16) Uani 1 1 d . . . C19 C 0.8114(5) 0.6643(4) 0.5307(3) 0.0664(18) Uani 1 1 d . . . C12 C 0.7849(5) 1.0000(4) 0.4487(3) 0.0701(19) Uani 1 1 d . . . C14 C 0.6952(4) 0.9073(4) 0.5055(3) 0.0591(16) Uani 1 1 d . . . H14 H 0.7200 0.9458 0.5313 0.071 Uiso 1 1 calc R D . C4N C 0.8443(9) 0.4041(5) 0.3863(4) 0.113(4) Uani 1 1 d . . . C25 C 0.7735(6) 0.4620(5) 0.3939(4) 0.086(3) Uani 1 1 d . . . N1 N 0.9130(5) 0.7470(5) 0.1937(3) 0.0970(19) Uani 1 1 d . D . C36 C 0.5689(6) 0.8853(5) 0.5650(3) 0.084(2) Uani 1 1 d . . . H36A H 0.5854 0.8265 0.5713 0.100 Uiso 1 1 calc R D . H36B H 0.6005 0.9205 0.5895 0.100 Uiso 1 1 calc R . . O8 O 0.7489(6) 0.4684(4) 0.3023(3) 0.115(3) Uani 1 1 d D . . O7 O 0.7980(4) 0.4623(3) 0.4818(3) 0.100(2) Uani 1 1 d D . . C5 C 0.7528(6) 0.8280(5) 0.2664(3) 0.075(2) Uani 1 1 d . . . C24 C 0.7576(6) 0.4939(4) 0.4422(3) 0.077(2) Uani 1 1 d . . . C3 C 0.7420(6) 0.6766(5) 0.2646(3) 0.079(2) Uani 1 1 d . . . C42 C 0.5539(6) 0.6207(6) 0.5627(3) 0.085(2) Uani 1 1 d . . . H42A H 0.5767 0.6768 0.5709 0.102 Uiso 1 1 calc R . . H42B H 0.4909 0.6240 0.5638 0.102 Uiso 1 1 calc R . . C1N C 0.8566(5) 0.7463(6) 0.2189(3) 0.0818(19) Uani 1 1 d . . . C35 C 0.5971(5) 0.9090(5) 0.5122(3) 0.0679(18) Uani 1 1 d . D . H35A H 0.5759 0.9659 0.5044 0.082 Uiso 1 1 calc R . . H35B H 0.5710 0.8699 0.4878 0.082 Uiso 1 1 calc R . . C2N C 0.8735(8) 1.0905(6) 0.3952(4) 0.100(3) Uani 1 1 d . . . N4 N 0.8951(6) 0.3577(5) 0.3785(4) 0.117(3) Uani 1 1 d . . . C47 C 0.5299(6) 0.6121(5) 0.3180(4) 0.096(3) Uani 1 1 d D . . H47A H 0.5226 0.6557 0.3442 0.115 Uiso 1 1 calc R . . H47B H 0.5054 0.6345 0.2864 0.115 Uiso 1 1 calc R . . C40 C 0.3552(6) 0.7464(6) 0.6113(3) 0.099(2) Uiso 1 1 d . . . H40A H 0.3031 0.7764 0.6208 0.148 Uiso 1 1 calc R . . H40B H 0.3499 0.6875 0.6209 0.148 Uiso 1 1 calc R . . H40C H 0.3637 0.7507 0.5748 0.148 Uiso 1 1 calc R . . C44 C 0.5413(7) 0.5793(6) 0.6547(3) 0.097(3) Uani 1 1 d . . . H44A H 0.5566 0.6369 0.6650 0.116 Uiso 1 1 calc R . . H44B H 0.4786 0.5772 0.6512 0.116 Uiso 1 1 calc R . . C45 C 0.5666(9) 0.5212(8) 0.6960(4) 0.125(4) Uani 1 1 d . . . H45A H 0.6296 0.5176 0.6970 0.150 Uiso 1 1 calc R . . H45B H 0.5445 0.4647 0.6881 0.150 Uiso 1 1 calc R . . N2 N 0.9295(6) 1.1350(4) 0.3888(3) 0.102(2) Uani 1 1 d . . . C43 C 0.5827(7) 0.5615(6) 0.6010(3) 0.099(3) Uani 1 1 d . . . H43A H 0.6455 0.5647 0.6039 0.119 Uiso 1 1 calc R . . H43B H 0.5677 0.5041 0.5902 0.119 Uiso 1 1 calc R . . C37 C 0.4759(6) 0.8942(9) 0.5753(4) 0.116(4) Uani 1 1 d . D . H37A H 0.4456 0.8611 0.5493 0.139 Uiso 1 1 calc R . . H37B H 0.4611 0.9535 0.5693 0.139 Uiso 1 1 calc R . . C38 C 0.4365(13) 0.8694(8) 0.6278(4) 0.241(13) Uani 1 1 d . . . H38A H 0.4692 0.8986 0.6545 0.289 Uiso 1 1 calc R D . H38B H 0.3775 0.8911 0.6291 0.289 Uiso 1 1 calc R . . C46 C 0.5348(9) 0.5467(8) 0.7479(4) 0.128(4) Uani 1 1 d . . . H46A H 0.5707 0.5918 0.7611 0.193 Uiso 1 1 calc R . . H46B H 0.5373 0.4986 0.7707 0.193 Uiso 1 1 calc R . . H46C H 0.4758 0.5663 0.7452 0.193 Uiso 1 1 calc R . . C48 C 0.4778(8) 0.5386(9) 0.3333(6) 0.175(7) Uani 1 1 d D . . H48A H 0.4922 0.5235 0.3685 0.210 Uiso 1 1 calc R . . H48B H 0.4930 0.4905 0.3115 0.210 Uiso 1 1 calc R . . C49 C 0.3808(8) 0.5538(9) 0.3297(5) 0.150(6) Uani 1 1 d D . . H49A H 0.3645 0.5661 0.2943 0.180 Uiso 1 1 calc R . . H49B H 0.3642 0.6018 0.3511 0.180 Uiso 1 1 calc R . . C50 C 0.3354(10) 0.4719(10) 0.3484(6) 0.176(7) Uani 1 1 d D . . H50A H 0.3422 0.4267 0.3232 0.211 Uiso 1 1 calc R . . H50B H 0.3603 0.4531 0.3808 0.211 Uiso 1 1 calc R . . O1A O 0.8598(8) 1.1784(5) 0.2869(4) 0.109(4) Uani 0.60 1 d PD B 1 C1A C 0.9058(10) 1.1679(9) 0.2413(5) 0.087(4) Uani 0.60 1 d PD B 1 O1B O 0.7472(10) 0.2988(9) 0.3047(6) 0.209(5) Uiso 0.40 1 d PD C 2 C29 C 0.5538(6) 0.9236(5) 0.3246(3) 0.084(2) Uiso 0.60 1 d PD D 1 H29A H 0.5410 0.8915 0.3557 0.101 Uiso 0.60 1 calc PR D 1 H29B H 0.5408 0.9829 0.3321 0.101 Uiso 0.60 1 calc PR D 1 C30' C 0.5203(10) 1.0124(9) 0.3322(7) 0.072(4) Uiso 0.20 1 d PD D 2 H30A H 0.5340 1.0458 0.3018 0.086 Uiso 0.20 1 calc PR D 2 H30B H 0.5507 1.0380 0.3611 0.086 Uiso 0.20 1 calc PR D 2 C31' C 0.4243(10) 1.0177(11) 0.3420(7) 0.074(4) Uiso 0.20 1 d PD D 2 H31A H 0.4083 0.9757 0.3678 0.089 Uiso 0.20 1 calc PR D 2 H31B H 0.3934 1.0040 0.3105 0.089 Uiso 0.20 1 calc PR D 2 C30 C 0.4937(8) 0.8958(9) 0.2855(7) 0.175(10) Uiso 0.60 1 d PD D 1 H30C H 0.5001 0.8343 0.2831 0.211 Uiso 0.60 1 calc PR D 1 H30D H 0.5151 0.9188 0.2532 0.211 Uiso 0.60 1 calc PR D 1 C34 C 0.2390(13) 0.7686(11) 0.3445(7) 0.124(6) Uiso 0.60 1 d PD D 1 H34A H 0.1777 0.7769 0.3495 0.186 Uiso 0.60 1 calc PR D 1 H34B H 0.2666 0.7602 0.3774 0.186 Uiso 0.60 1 calc PR D 1 H34C H 0.2485 0.7194 0.3233 0.186 Uiso 0.60 1 calc PR D 1 C33 C 0.2758(11) 0.8433(12) 0.3197(8) 0.127(6) Uiso 0.60 1 d PD D 1 H33A H 0.2675 0.8933 0.3411 0.152 Uiso 0.60 1 calc PR D 1 H33B H 0.2475 0.8532 0.2868 0.152 Uiso 0.60 1 calc PR D 1 C32 C 0.3692(9) 0.8274(11) 0.3119(8) 0.124(6) Uiso 0.60 1 d PD D 1 H32A H 0.3791 0.7792 0.2892 0.149 Uiso 0.60 1 calc PR D 1 H32B H 0.3990 0.8179 0.3443 0.149 Uiso 0.60 1 calc PR D 1 C32' C 0.3964(15) 1.1065(13) 0.3606(11) 0.119(8) Uiso 0.20 1 d PD D 2 H32C H 0.4311 1.1237 0.3900 0.142 Uiso 0.20 1 calc PR D 2 H32D H 0.4044 1.1481 0.3333 0.142 Uiso 0.20 1 calc PR D 2 C33' C 0.3012(16) 1.1013(19) 0.3755(13) 0.068(8) Uiso 0.20 1 d PD D 2 H33C H 0.2680 1.0975 0.3438 0.082 Uiso 0.20 1 calc PR D 2 H33D H 0.2930 1.0478 0.3935 0.082 Uiso 0.20 1 calc PR D 2 C6 C 0.6802(5) 0.8320(5) 0.2966(3) 0.0675(18) Uani 1 1 d . D . C39 C 0.4342(9) 0.7865(8) 0.6397(5) 0.134(4) Uiso 1 1 d . D . H39A H 0.4280 0.7793 0.6766 0.161 Uiso 1 1 calc R . . H39B H 0.4876 0.7589 0.6289 0.161 Uiso 1 1 calc R . . C51 C 0.2395(10) 0.4937(10) 0.3553(7) 0.166(6) Uiso 1 1 d D . . H51A H 0.2337 0.5399 0.3800 0.199 Uiso 1 1 calc R . . H51B H 0.2155 0.5129 0.3227 0.199 Uiso 1 1 calc R . . C52 C 0.1892(6) 0.4171(7) 0.3741(7) 0.250(12) Uiso 1 1 d D . . H52A H 0.2088 0.3670 0.3562 0.376 Uiso 1 1 calc R . . H52B H 0.1283 0.4255 0.3676 0.376 Uiso 1 1 calc R . . H52C H 0.1985 0.4100 0.4104 0.376 Uiso 1 1 calc R . . H7O H 0.8350 0.4293 0.4893 0.100 Uiso 1 1 d RD . . H1O H 0.7904 0.5617 0.2617 0.100 Uiso 1 1 d RD . . H4O H 0.8508 1.0598 0.4769 0.100 Uiso 1 1 d RD . . H8O H 0.7640 0.4216 0.3005 0.100 Uiso 1 1 d RD . . H5O H 0.8528 0.9283 0.5367 0.100 Uiso 1 1 d RD . . H2O H 0.7840 0.9401 0.2631 0.100 Uiso 1 1 d RD . . H3O H 0.7990 1.0794 0.3196 0.100 Uiso 1 1 d RD . . H6O H 0.8294 0.5678 0.5211 0.100 Uiso 1 1 d RD . . C31 C 0.3977(11) 0.9131(13) 0.2864(10) 0.144(8) Uiso 0.60 1 d PD D 1 H31C H 0.3738 0.9200 0.2520 0.172 Uiso 0.60 1 calc PR D 1 H31D H 0.3831 0.9622 0.3074 0.172 Uiso 0.60 1 calc PR D 1 O1F O 0.997(3) 0.392(3) 0.4912(17) 0.249(17) Uiso 0.40 1 d PD E 2 C29' C 0.5538(6) 0.9236(5) 0.3246(3) 0.084(2) Uiso 0.20 1 d PD D 2 H29C H 0.5393 0.8901 0.3549 0.101 Uiso 0.20 1 calc PR D 2 H29D H 0.5239 0.8984 0.2955 0.101 Uiso 0.20 1 calc PR D 2 O1E O 0.852(2) 0.3042(17) 0.4929(13) 0.276(14) Uiso 0.60 1 d PD F 1 C1G C 1.007(2) 0.107(2) 0.5450(10) 0.205(13) Uiso 0.60 1 d PD G 1 O1D O 0.8839(14) 0.1750(14) 0.5071(8) 0.131(6) Uiso 0.40 1 d PD H 2 O1G O 0.9703(10) 0.1024(10) 0.4954(6) 0.139(5) Uiso 0.60 1 d PD G 1 C1E C 0.7737(18) 0.268(2) 0.4753(11) 0.163(9) Uiso 0.60 1 d PD F 1 C1F C 1.082(3) 0.370(3) 0.5015(17) 0.167(14) Uiso 0.40 1 d PD E 2 C34' C 0.260(3) 1.169(4) 0.4073(18) 0.15(2) Uiso 0.20 1 d PD D 2 H34D H 0.2067 1.1481 0.4214 0.229 Uiso 0.20 1 calc PR D 2 H34E H 0.2489 1.2181 0.3863 0.229 Uiso 0.20 1 calc PR D 2 H34F H 0.2990 1.1845 0.4349 0.229 Uiso 0.20 1 calc PR D 2 C1D C 0.826(2) 0.236(2) 0.4893(12) 0.150(12) Uiso 0.40 1 d PD H 2 C1B C 0.697(2) 0.245(2) 0.3372(13) 0.146(11) Uiso 0.40 1 d PD C 2 C2B C 0.669(2) 0.297(4) 0.333(2) 0.29(3) Uiso 0.60 1 d PD I 1 O2B O 0.7472(10) 0.2988(9) 0.3047(6) 0.209(5) Uiso 0.60 1 d PD I 1 C34" C 0.376(4) 1.2565(19) 0.361(2) 0.14(2) Uiso 0.20 1 d PD D 3 H34G H 0.4006 1.3118 0.3662 0.211 Uiso 0.20 1 calc PR D 3 H34H H 0.3272 1.2486 0.3834 0.211 Uiso 0.20 1 calc PR D 3 H34I H 0.3561 1.2522 0.3255 0.211 Uiso 0.20 1 calc PR D 3 C33" C 0.443(4) 1.189(2) 0.371(5) 0.24(5) Uiso 0.20 1 d PD D 3 H33E H 0.4925 1.1953 0.3479 0.291 Uiso 0.20 1 calc PR D 3 H33F H 0.4632 1.1914 0.4062 0.291 Uiso 0.20 1 calc PR D 3 C32" C 0.3964(15) 1.1065(13) 0.3606(11) 0.119(8) Uiso 0.20 1 d PD D 3 H32E H 0.3511 1.1226 0.3364 0.142 Uiso 0.20 1 calc PR D 3 H32F H 0.3665 1.0950 0.3927 0.142 Uiso 0.20 1 calc PR D 3 C31" C 0.4243(10) 1.0177(11) 0.3420(7) 0.074(4) Uiso 0.20 1 d P D 3 H31E H 0.4083 0.9757 0.3678 0.089 Uiso 0.20 1 calc PR D 3 H31F H 0.3934 1.0040 0.3105 0.089 Uiso 0.20 1 calc PR D 3 C30" C 0.5203(10) 1.0124(9) 0.3322(7) 0.072(4) Uiso 0.20 1 d P D 3 H30E H 0.5340 1.0458 0.3018 0.086 Uiso 0.20 1 calc PR D 3 H30F H 0.5507 1.0380 0.3611 0.086 Uiso 0.20 1 calc PR D 3 C29" C 0.5538(6) 0.9236(5) 0.3246(3) 0.084(2) Uiso 0.20 1 d P D 3 H29E H 0.5393 0.8901 0.3549 0.101 Uiso 0.20 1 calc PR D 3 H29F H 0.5239 0.8984 0.2955 0.101 Uiso 0.20 1 calc PR D 3 O1C O 1.076(3) 0.2546(19) 0.4484(17) 0.220(17) Uiso 0.30 1 d P J 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ag1 0.1140(5) 0.0686(4) 0.1280(6) 0.0029(4) 0.0533(4) 0.0033(4) O6 0.092(4) 0.070(3) 0.092(4) 0.017(3) 0.007(3) 0.029(3) C8 0.070(4) 0.043(3) 0.089(5) -0.003(3) 0.012(4) 0.006(3) O2 0.113(4) 0.078(3) 0.077(3) 0.003(3) 0.019(3) -0.003(3) C15 0.050(3) 0.055(3) 0.067(3) 0.008(3) 0.013(2) 0.003(3) C20 0.066(4) 0.058(4) 0.066(4) 0.011(3) 0.025(4) 0.017(3) C17 0.065(4) 0.060(4) 0.062(4) 0.001(3) 0.010(3) -0.003(3) C2 0.090(6) 0.064(4) 0.078(5) -0.006(4) 0.010(4) -0.012(4) C16 0.059(4) 0.064(4) 0.055(4) 0.008(3) 0.016(3) 0.013(3) C28 0.112(7) 0.089(6) 0.077(6) -0.020(4) 0.031(5) -0.024(5) O5 0.082(3) 0.062(3) 0.093(4) 0.000(3) -0.003(3) 0.003(2) C21 0.082(5) 0.048(3) 0.082(5) 0.012(3) 0.019(4) 0.005(3) N3 0.076(4) 0.102(5) 0.121(5) 0.007(4) -0.020(4) 0.028(4) O1 0.120(5) 0.077(3) 0.084(3) -0.008(3) 0.040(3) 0.017(3) C3N 0.071(5) 0.078(5) 0.096(5) 0.005(4) 0.006(4) 0.011(4) C27 0.102(6) 0.058(4) 0.092(6) -0.009(4) 0.044(5) -0.006(4) O3 0.130(5) 0.064(3) 0.083(4) 0.010(3) 0.021(3) -0.016(3) C4 0.082(4) 0.076(4) 0.054(3) 0.001(4) 0.013(3) -0.012(4) C1 0.069(4) 0.074(4) 0.077(4) -0.014(4) 0.014(3) 0.013(4) C23 0.070(4) 0.047(3) 0.098(6) 0.006(4) 0.029(4) -0.004(3) C13 0.072(4) 0.046(3) 0.071(4) 0.002(3) 0.014(3) 0.008(3) C9 0.091(5) 0.045(3) 0.063(4) 0.005(3) 0.005(4) 0.010(3) C22 0.092(5) 0.056(4) 0.075(5) -0.013(3) 0.028(4) 0.001(4) C11 0.076(5) 0.047(3) 0.087(5) 0.007(3) 0.017(4) 0.001(3) C41 0.087(5) 0.058(4) 0.100(6) 0.001(4) 0.028(5) -0.006(4) O4 0.110(4) 0.060(3) 0.093(4) 0.008(3) -0.003(3) -0.020(3) C7 0.095(5) 0.072(5) 0.064(4) 0.006(3) 0.001(4) 0.014(4) C26 0.132(8) 0.061(4) 0.116(8) -0.023(5) 0.061(7) -0.024(5) C10 0.095(5) 0.052(3) 0.068(5) 0.014(3) 0.011(4) 0.000(3) C18 0.058(3) 0.077(5) 0.065(3) 0.006(3) 0.003(3) 0.016(4) C19 0.067(4) 0.058(4) 0.074(4) 0.011(3) 0.025(4) 0.017(3) C12 0.077(5) 0.057(4) 0.077(5) 0.001(3) 0.000(4) -0.003(3) C14 0.054(3) 0.058(3) 0.066(4) 0.004(3) 0.012(3) 0.010(3) C4N 0.174(11) 0.053(4) 0.112(7) 0.007(4) 0.058(8) 0.011(6) C25 0.110(7) 0.049(4) 0.098(6) 0.005(4) 0.033(5) 0.000(4) N1 0.100(5) 0.096(5) 0.095(4) -0.018(5) 0.027(4) 0.011(5) C36 0.096(6) 0.074(5) 0.080(5) 0.020(4) 0.029(5) 0.017(4) O8 0.173(7) 0.058(3) 0.113(5) -0.022(3) 0.048(5) 0.006(4) O7 0.120(5) 0.055(3) 0.124(5) 0.009(3) 0.047(4) 0.013(3) C5 0.089(5) 0.081(5) 0.056(4) 0.000(4) 0.012(4) -0.016(4) C24 0.090(5) 0.047(3) 0.095(6) 0.017(4) 0.039(5) 0.011(3) C3 0.082(5) 0.088(5) 0.067(5) -0.015(4) 0.013(4) -0.011(4) C42 0.080(5) 0.089(5) 0.087(6) 0.016(4) 0.022(4) 0.006(4) C1N 0.084(4) 0.092(5) 0.070(4) 0.012(5) 0.020(3) 0.003(5) C35 0.066(4) 0.068(4) 0.070(4) 0.004(3) 0.016(3) 0.017(3) C2N 0.136(9) 0.071(5) 0.092(6) 0.007(4) 0.017(6) -0.014(6) N4 0.149(8) 0.062(4) 0.141(7) 0.006(4) 0.056(6) 0.016(5) C47 0.085(6) 0.097(6) 0.106(6) -0.029(5) 0.011(5) -0.026(5) C44 0.112(7) 0.092(6) 0.085(5) 0.025(4) 0.001(5) -0.005(5) C45 0.141(9) 0.146(10) 0.087(7) 0.034(6) 0.000(6) -0.012(8) N2 0.133(7) 0.063(4) 0.110(6) 0.001(4) 0.025(5) -0.023(4) C43 0.102(6) 0.106(7) 0.089(6) 0.005(5) -0.007(5) -0.001(5) C37 0.094(6) 0.177(11) 0.077(6) 0.031(6) 0.022(5) -0.003(7) C38 0.44(3) 0.206(16) 0.072(7) -0.013(8) -0.043(12) 0.20(2) C46 0.145(10) 0.154(10) 0.086(6) 0.029(6) -0.018(7) 0.012(8) C48 0.131(11) 0.186(15) 0.209(16) -0.012(12) 0.013(11) -0.083(11) C49 0.170(12) 0.179(13) 0.101(8) -0.035(8) 0.038(8) -0.083(11) C50 0.188(15) 0.183(15) 0.157(13) -0.057(12) -0.012(11) -0.033(13) O1A 0.162(10) 0.048(4) 0.118(7) 0.013(5) 0.068(7) 0.005(5) C1A 0.111(11) 0.083(9) 0.068(7) 0.013(6) -0.001(7) -0.013(8) C6 0.065(4) 0.078(4) 0.059(4) 0.012(3) 0.003(3) 0.000(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 N1 2.180(7) . ? Ag1 N4 2.196(8) 4_755 ? Ag1 N2 2.229(7) 4_745 ? O6 C19 1.361(8) . ? O6 H6O 0.7952 . ? C8 C13 1.364(11) . ? C8 C9 1.452(11) . ? C8 H8 0.9500 . ? O2 C5 1.363(10) . ? O2 H2O 0.7914 . ? C15 C16 1.381(10) . ? C15 C20 1.427(10) . ? C15 H15 0.9500 . ? C20 C19 1.398(11) . ? C20 C21 1.521(11) . ? C17 O5 1.372(8) . ? C17 C18 1.396(9) . ? C17 C16 1.419(10) . ? C2 C1 1.376(10) . ? C2 C3 1.421(12) . ? C2 C28 1.479(12) . ? C16 C14 1.489(9) . ? C28 C47 1.572(14) . ? C28 C27 1.571(14) . ? C28 H28 1.0000 . ? O5 H5O 0.7786 . ? C21 C23 1.475(12) . ? C21 C41 1.533(11) . ? C21 H21 1.0000 . ? N3 C3N 1.155(10) . ? O1 C3 1.350(10) . ? O1 H1O 0.8408 . ? C3N C18 1.430(11) . ? C27 C22 1.375(12) . ? C27 C26 1.396(13) . ? O3 C10 1.359(10) . ? O3 H3O 0.7970 . ? C4 C5 1.384(11) . ? C4 C3 1.404(11) . ? C4 C1N 1.430(10) . ? C1 C6 1.345(10) . ? C1 H1A 0.9500 . ? C23 C24 1.414(10) . ? C23 C22 1.409(12) . ? C13 C12 1.381(11) . ? C13 C14 1.547(10) . ? C9 C10 1.352(11) . ? C9 C7 1.521(11) . ? C22 H22 0.9500 . ? C11 C10 1.400(11) . ? C11 C12 1.406(11) . ? C11 C2N 1.422(13) . ? C41 C42 1.489(13) . ? C41 H41A 0.9900 . ? C41 H41B 0.9900 . ? O4 C12 1.333(10) . ? O4 H4O 0.7896 . ? C7 C29 1.475(12) . ? C7 C6 1.555(11) . ? C7 H7 1.0000 . ? C26 O8 1.403(12) . ? C26 C25 1.424(15) . ? C18 C19 1.393(11) . ? C14 C35 1.551(10) . ? C14 H14 1.0000 . ? C4N N4 1.110(13) . ? C4N C25 1.461(15) . ? C25 C24 1.399(12) . ? N1 C1N 1.109(9) . ? C36 C37 1.492(13) . ? C36 C35 1.515(11) . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? O8 H8O 0.7870 . ? O7 C24 1.326(11) . ? O7 H7O 0.8088 . ? C5 C6 1.392(11) . ? C42 C43 1.459(12) . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C2N N2 1.143(12) . ? N4 Ag1 2.196(8) 4_745 ? C47 C48 1.488(12) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C40 C39 1.586(15) . ? C40 H40A 0.9800 . ? C40 H40B 0.9800 . ? C40 H40C 0.9800 . ? C44 C45 1.490(13) . ? C44 C43 1.590(14) . ? C44 H44A 0.9900 . ? C44 H44B 0.9900 . ? C45 C46 1.517(16) . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? N2 Ag1 2.229(7) 4_755 ? C43 H43A 0.9900 . ? C43 H43B 0.9900 . ? C37 C38 1.573(16) . ? C37 H37A 0.9900 . ? C37 H37B 0.9900 . ? C38 C39 1.363(10) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C48 C49 1.544(15) . ? C48 H48A 0.9900 . ? C48 H48B 0.9900 . ? C49 C50 1.572(15) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 C51 1.556(16) . ? C50 H50A 0.9900 . ? C50 H50B 0.9900 . ? O1A C1A 1.416(13) . ? O1B C1B 1.448(18) . ? C29 C30 1.472(15) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C30' C31' 1.531(16) . ? C30' H30A 0.9900 . ? C30' H30B 0.9900 . ? C31' C32' 1.566(17) . ? C31' H31A 0.9900 . ? C31' H31B 0.9900 . ? C30 C31 1.532(16) . ? C30 H30C 0.9900 . ? C30 H30D 0.9900 . ? C34 C33 1.481(16) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? C33 C32 1.501(16) . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C32 C31 1.592(17) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C32' C33' 1.548(18) . ? C32' H32C 0.9900 . ? C32' H32D 0.9900 . ? C33' C34' 1.515(19) . ? C33' H33C 0.9900 . ? C33' H33D 0.9900 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C51 C52 1.540(14) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C31 H31C 0.9900 . ? C31 H31D 0.9900 . ? O1F C1F 1.414(19) . ? O1E C1E 1.436(18) . ? C1G O1G 1.436(18) . ? O1D C1D 1.412(19) . ? C34' H34D 0.9800 . ? C34' H34E 0.9800 . ? C34' H34F 0.9800 . ? C34" C33" 1.54(2) . ? C34" H34G 0.9800 . ? C34" H34H 0.9800 . ? C34" H34I 0.9800 . ? C33" H33E 0.9900 . ? C33" H33F 0.9900 . ? 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 N1 Ag1 N4 130.9(3) . 4_755 ? N1 Ag1 N2 116.8(3) . 4_745 ? N4 Ag1 N2 109.5(3) 4_755 4_745 ? C19 O6 H6O 91.3 . . ? C13 C8 C9 122.8(7) . . ? C13 C8 H8 118.6 . . ? C9 C8 H8 118.6 . . ? C5 O2 H2O 117.1 . . ? C16 C15 C20 125.3(5) . . ? C16 C15 H15 117.3 . . ? C20 C15 H15 117.3 . . ? C19 C20 C15 116.7(7) . . ? C19 C20 C21 122.3(6) . . ? C15 C20 C21 121.0(6) . . ? O5 C17 C18 115.8(6) . . ? O5 C17 C16 122.9(6) . . ? C18 C17 C16 121.2(6) . . ? C1 C2 C3 115.5(7) . . ? C1 C2 C28 127.6(8) . . ? C3 C2 C28 116.8(7) . . ? C15 C16 C17 115.4(6) . . ? C15 C16 C14 123.8(6) . . ? C17 C16 C14 120.8(7) . . ? C2 C28 C47 111.1(8) . . ? C2 C28 C27 108.5(8) . . ? C47 C28 C27 111.6(7) . . ? C2 C28 H28 108.5 . . ? C47 C28 H28 108.5 . . ? C27 C28 H28 108.5 . . ? C17 O5 H5O 119.0 . . ? C23 C21 C20 109.6(6) . . ? C23 C21 C41 114.1(8) . . ? C20 C21 C41 114.7(6) . . ? C23 C21 H21 105.9 . . ? C20 C21 H21 105.9 . . ? C41 C21 H21 105.9 . . ? C3 O1 H1O 129.1 . . ? N3 C3N C18 176.2(9) . . ? C22 C27 C26 117.1(10) . . ? C22 C27 C28 123.5(7) . . ? C26 C27 C28 119.4(8) . . ? C10 O3 H3O 98.1 . . ? C5 C4 C3 121.2(6) . . ? C5 C4 C1N 120.1(7) . . ? C3 C4 C1N 118.7(8) . . ? C6 C1 C2 126.7(6) . . ? C6 C1 H1A 116.7 . . ? C2 C1 H1A 116.7 . . ? C24 C23 C22 115.8(8) . . ? C24 C23 C21 121.4(8) . . ? C22 C23 C21 122.8(6) . . ? C8 C13 C12 119.1(7) . . ? C8 C13 C14 120.8(6) . . ? C12 C13 C14 120.1(7) . . ? C10 C9 C8 116.5(7) . . ? C10 C9 C7 124.8(7) . . ? C8 C9 C7 118.7(7) . . ? C27 C22 C23 125.6(8) . . ? C27 C22 H22 117.2 . . ? C23 C22 H22 117.2 . . ? C10 C11 C12 120.4(7) . . ? C10 C11 C2N 118.8(7) . . ? C12 C11 C2N 120.7(8) . . ? C42 C41 C21 117.4(9) . . ? C42 C41 H41A 108.0 . . ? C21 C41 H41A 108.0 . . ? C42 C41 H41B 108.0 . . ? C21 C41 H41B 108.0 . . ? H41A C41 H41B 107.2 . . ? C12 O4 H4O 93.9 . . ? C29 C7 C9 113.2(7) . . ? C29 C7 C6 116.5(7) . . ? C9 C7 C6 110.3(6) . . ? C29 C7 H7 105.3 . . ? C9 C7 H7 105.3 . . ? C6 C7 H7 105.3 . . ? C27 C26 O8 118.4(11) . . ? C27 C26 C25 120.5(9) . . ? O8 C26 C25 121.0(9) . . ? C9 C10 O3 119.2(8) . . ? C9 C10 C11 121.6(7) . . ? O3 C10 C11 119.1(7) . . ? C19 C18 C17 121.4(6) . . ? C19 C18 C3N 118.9(7) . . ? C17 C18 C3N 119.7(7) . . ? O6 C19 C18 115.3(7) . . ? O6 C19 C20 124.7(7) . . ? C18 C19 C20 119.9(6) . . ? O4 C12 C13 118.4(7) . . ? O4 C12 C11 122.1(7) . . ? C13 C12 C11 119.5(7) . . ? C16 C14 C13 110.1(5) . . ? C16 C14 C35 114.3(6) . . ? C13 C14 C35 110.3(6) . . ? C16 C14 H14 107.3 . . ? C13 C14 H14 107.3 . . ? C35 C14 H14 107.3 . . ? N4 C4N C25 175.8(14) . . ? C24 C25 C26 120.0(8) . . ? C24 C25 C4N 119.5(10) . . ? C26 C25 C4N 119.6(9) . . ? C1N N1 Ag1 174.4(8) . . ? C37 C36 C35 115.5(8) . . ? C37 C36 H36A 108.4 . . ? C35 C36 H36A 108.4 . . ? C37 C36 H36B 108.4 . . ? C35 C36 H36B 108.4 . . ? H36A C36 H36B 107.5 . . ? C26 O8 H8O 114.8 . . ? C24 O7 H7O 141.8 . . ? O2 C5 C4 116.9(7) . . ? O2 C5 C6 123.5(7) . . ? C4 C5 C6 119.7(7) . . ? O7 C24 C25 119.9(7) . . ? O7 C24 C23 119.3(8) . . ? C25 C24 C23 120.8(9) . . ? O1 C3 C4 116.2(7) . . ? O1 C3 C2 124.5(7) . . ? C4 C3 C2 119.3(7) . . ? C43 C42 C41 113.4(8) . . ? C43 C42 H42A 108.9 . . ? C41 C42 H42A 108.9 . . ? C43 C42 H42B 108.9 . . ? C41 C42 H42B 108.9 . . ? H42A C42 H42B 107.7 . . ? N1 C1N C4 175.9(10) . . ? C36 C35 C14 113.1(7) . . ? C36 C35 H35A 109.0 . . ? C14 C35 H35A 109.0 . . ? C36 C35 H35B 109.0 . . ? C14 C35 H35B 109.0 . . ? H35A C35 H35B 107.8 . . ? N2 C2N C11 175.6(11) . . ? C4N N4 Ag1 173.3(10) . 4_745 ? C48 C47 C28 118.8(9) . . ? C48 C47 H47A 107.6 . . ? C28 C47 H47A 107.6 . . ? C48 C47 H47B 107.6 . . ? C28 C47 H47B 107.6 . . ? H47A C47 H47B 107.0 . . ? C39 C40 H40A 109.5 . . ? C39 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C39 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C45 C44 C43 115.9(9) . . ? C45 C44 H44A 108.3 . . ? C43 C44 H44A 108.3 . . ? C45 C44 H44B 108.3 . . ? C43 C44 H44B 108.3 . . ? H44A C44 H44B 107.4 . . ? C44 C45 C46 114.1(11) . . ? C44 C45 H45A 108.7 . . ? C46 C45 H45A 108.7 . . ? C44 C45 H45B 108.7 . . ? C46 C45 H45B 108.7 . . ? H45A C45 H45B 107.6 . . ? C2N N2 Ag1 151.6(9) . 4_755 ? C42 C43 C44 112.3(8) . . ? C42 C43 H43A 109.1 . . ? C44 C43 H43A 109.1 . . ? C42 C43 H43B 109.1 . . ? C44 C43 H43B 109.1 . . ? H43A C43 H43B 107.9 . . ? C36 C37 C38 121.4(11) . . ? C36 C37 H37A 107.0 . . ? C38 C37 H37A 107.0 . . ? C36 C37 H37B 107.0 . . ? C38 C37 H37B 107.0 . . ? H37A C37 H37B 106.7 . . ? C39 C38 C37 117.4(12) . . ? C39 C38 H38A 108.0 . . ? C37 C38 H38A 108.0 . . ? C39 C38 H38B 108.0 . . ? C37 C38 H38B 108.0 . . ? H38A C38 H38B 107.2 . . ? C45 C46 H46A 109.5 . . ? C45 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C45 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C47 C48 C49 113.6(12) . . ? C47 C48 H48A 108.8 . . ? C49 C48 H48A 108.8 . . ? C47 C48 H48B 108.8 . . ? C49 C48 H48B 108.8 . . ? H48A C48 H48B 107.7 . . ? C48 C49 C50 107.2(12) . . ? C48 C49 H49A 110.3 . . ? C50 C49 H49A 110.3 . . ? C48 C49 H49B 110.3 . . ? C50 C49 H49B 110.3 . . ? H49A C49 H49B 108.5 . . ? C51 C50 C49 106.8(12) . . ? C51 C50 H50A 110.4 . . ? C49 C50 H50A 110.4 . . ? C51 C50 H50B 110.4 . . ? C49 C50 H50B 110.4 . . ? H50A C50 H50B 108.6 . . ? C30 C29 C7 120.1(9) . . ? C30 C29 H29A 107.3 . . ? C7 C29 H29A 107.3 . . ? C30 C29 H29B 107.3 . . ? C7 C29 H29B 107.3 . . ? H29A C29 H29B 106.9 . . ? C31' C30' H30A 108.7 . . ? C31' C30' H30B 108.7 . . ? H30A C30' H30B 107.6 . . ? C30' C31' C32' 112.2(15) . . ? C30' C31' H31A 109.2 . . ? C32' C31' H31A 109.2 . . ? C30' C31' H31B 109.2 . . ? C32' C31' H31B 109.2 . . ? H31A C31' H31B 107.9 . . ? C29 C30 C31 124.4(17) . . ? C29 C30 H30C 106.2 . . ? C31 C30 H30C 106.2 . . ? C29 C30 H30D 106.2 . . ? C31 C30 H30D 106.2 . . ? H30C C30 H30D 106.4 . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C34 C33 C32 107.8(16) . . ? C34 C33 H33A 110.2 . . ? C32 C33 H33A 110.2 . . ? C34 C33 H33B 110.2 . . ? C32 C33 H33B 110.2 . . ? H33A C33 H33B 108.5 . . ? C33 C32 C31 100.8(14) . . ? C33 C32 H32A 111.6 . . ? C31 C32 H32A 111.6 . . ? C33 C32 H32B 111.6 . . ? C31 C32 H32B 111.6 . . ? H32A C32 H32B 109.4 . . ? C33' C32' C31' 107.6(19) . . ? C33' C32' H32C 110.2 . . ? C31' C32' H32C 110.2 . . ? C33' C32' H32D 110.2 . . ? C31' C32' H32D 110.2 . . ? H32C C32' H32D 108.5 . . ? C34' C33' C32' 121(3) . . ? C34' C33' H33C 107.1 . . ? C32' C33' H33C 107.1 . . ? C34' C33' H33D 107.1 . . ? C32' C33' H33D 107.1 . . ? H33C C33' H33D 106.8 . . ? C1 C6 C5 117.5(7) . . ? C1 C6 C7 121.7(7) . . ? C5 C6 C7 120.5(7) . . ? C38 C39 C40 107.8(13) . . ? C38 C39 H39A 110.2 . . ? C40 C39 H39A 110.1 . . ? C38 C39 H39B 110.2 . . ? C40 C39 H39B 110.1 . . ? H39A C39 H39B 108.5 . . ? C52 C51 C50 110.8(12) . . ? C52 C51 H51A 109.5 . . ? C50 C51 H51A 109.5 . . ? C52 C51 H51B 109.5 . . ? C50 C51 H51B 109.5 . . ? H51A C51 H51B 108.1 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C30 C31 C32 97.4(11) . . ? C30 C31 H31C 112.3 . . ? C32 C31 H31C 112.3 . . ? C30 C31 H31D 112.3 . . ? C32 C31 H31D 112.3 . . ? H31C C31 H31D 109.9 . . ? C33' C34' H34D 109.5 . . ? C33' C34' H34E 109.5 . . ? H34D C34' H34E 109.5 . . ? C33' C34' H34F 109.5 . . ? H34D C34' H34F 109.5 . . ? H34E C34' H34F 109.5 . . ? C33" C34" H34G 109.5 . . ? C33" C34" H34H 109.4 . . ? H34G C34" H34H 109.5 . . ? C33" C34" H34I 109.5 . . ? H34G C34" H34I 109.5 . . ? H34H C34" H34I 109.5 . . ? C34" C33" H33E 110.9 . . ? C34" C33" H33F 110.9 . . ? H33E C33" H33F 108.9 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 C15 C20 C19 -2.0(8) . . . . ? C16 C15 C20 C21 178.6(7) . . . . ? C20 C15 C16 C17 0.5(8) . . . . ? C20 C15 C16 C14 -177.7(7) . . . . ? O5 C17 C16 C15 178.5(6) . . . . ? C18 C17 C16 C15 0.5(9) . . . . ? O5 C17 C16 C14 -3.2(10) . . . . ? C18 C17 C16 C14 178.8(6) . . . . ? C1 C2 C28 C47 27.8(13) . . . . ? C3 C2 C28 C47 -148.8(8) . . . . ? C1 C2 C28 C27 -95.3(11) . . . . ? C3 C2 C28 C27 88.1(9) . . . . ? C19 C20 C21 C23 -84.5(8) . . . . ? C15 C20 C21 C23 94.9(7) . . . . ? C19 C20 C21 C41 145.6(7) . . . . ? C15 C20 C21 C41 -35.0(10) . . . . ? C2 C28 C27 C22 75.3(10) . . . . ? C47 C28 C27 C22 -47.4(10) . . . . ? C2 C28 C27 C26 -103.3(9) . . . . ? C47 C28 C27 C26 134.0(8) . . . . ? C3 C2 C1 C6 1.6(12) . . . . ? C28 C2 C1 C6 -175.0(9) . . . . ? C20 C21 C23 C24 97.4(8) . . . . ? C41 C21 C23 C24 -132.3(8) . . . . ? C20 C21 C23 C22 -82.8(9) . . . . ? C41 C21 C23 C22 47.4(9) . . . . ? C9 C8 C13 C12 -1.4(10) . . . . ? C9 C8 C13 C14 179.1(6) . . . . ? C13 C8 C9 C10 1.4(10) . . . . ? C13 C8 C9 C7 -176.7(6) . . . . ? C26 C27 C22 C23 -2.4(13) . . . . ? C28 C27 C22 C23 179.0(8) . . . . ? C24 C23 C22 C27 4.2(12) . . . . ? C21 C23 C22 C27 -175.5(8) . . . . ? C23 C21 C41 C42 174.3(7) . . . . ? C20 C21 C41 C42 -58.1(10) . . . . ? C10 C9 C7 C29 -128.5(8) . . . . ? C8 C9 C7 C29 49.4(9) . . . . ? C10 C9 C7 C6 99.0(8) . . . . ? C8 C9 C7 C6 -83.1(8) . . . . ? C22 C27 C26 O8 -176.0(8) . . . . ? C28 C27 C26 O8 2.7(12) . . . . ? C22 C27 C26 C25 -0.1(12) . . . . ? C28 C27 C26 C25 178.5(8) . . . . ? C8 C9 C10 O3 176.4(7) . . . . ? C7 C9 C10 O3 -5.7(11) . . . . ? C8 C9 C10 C11 -0.1(10) . . . . ? C7 C9 C10 C11 177.8(7) . . . . ? C12 C11 C10 C9 -1.2(11) . . . . ? C2N C11 C10 C9 -179.9(8) . . . . ? C12 C11 C10 O3 -177.7(7) . . . . ? C2N C11 C10 O3 3.6(11) . . . . ? O5 C17 C18 C19 -178.2(7) . . . . ? C16 C17 C18 C19 0.0(10) . . . . ? O5 C17 C18 C3N 1.7(10) . . . . ? C16 C17 C18 C3N 179.8(6) . . . . ? N3 C3N C18 C19 159(14) . . . . ? N3 C3N C18 C17 -21(14) . . . . ? C17 C18 C19 O6 -177.1(7) . . . . ? C3N C18 C19 O6 3.1(9) . . . . ? C17 C18 C19 C20 -1.5(10) . . . . ? C3N C18 C19 C20 178.7(6) . . . . ? C15 C20 C19 O6 177.5(6) . . . . ? C21 C20 C19 O6 -3.1(11) . . . . ? C15 C20 C19 C18 2.4(9) . . . . ? C21 C20 C19 C18 -178.2(6) . . . . ? C8 C13 C12 O4 -177.7(7) . . . . ? C14 C13 C12 O4 1.8(10) . . . . ? C8 C13 C12 C11 0.1(10) . . . . ? C14 C13 C12 C11 179.6(6) . . . . ? C10 C11 C12 O4 178.9(7) . . . . ? C2N C11 C12 O4 -2.5(12) . . . . ? C10 C11 C12 C13 1.2(11) . . . . ? C2N C11 C12 C13 179.8(8) . . . . ? C15 C16 C14 C13 -94.7(8) . . . . ? C17 C16 C14 C13 87.2(8) . . . . ? C15 C16 C14 C35 30.2(10) . . . . ? C17 C16 C14 C35 -147.9(7) . . . . ? C8 C13 C14 C16 79.8(8) . . . . ? C12 C13 C14 C16 -99.7(8) . . . . ? C8 C13 C14 C35 -47.3(8) . . . . ? C12 C13 C14 C35 133.2(7) . . . . ? C27 C26 C25 C24 0.7(13) . . . . ? O8 C26 C25 C24 176.4(8) . . . . ? C27 C26 C25 C4N -168.9(9) . . . . ? O8 C26 C25 C4N 6.9(13) . . . . ? N4 C4N C25 C24 145(14) . . . . ? N4 C4N C25 C26 -46(15) . . . . ? N4 Ag1 N1 C1N 79(9) 4_755 . . . ? N2 Ag1 N1 C1N -122(9) 4_745 . . . ? C3 C4 C5 O2 178.6(8) . . . . ? C1N C4 C5 O2 0.4(11) . . . . ? C3 C4 C5 C6 -2.0(11) . . . . ? C1N C4 C5 C6 179.8(7) . . . . ? C26 C25 C24 O7 -179.7(8) . . . . ? C4N C25 C24 O7 -10.1(12) . . . . ? C26 C25 C24 C23 1.3(12) . . . . ? C4N C25 C24 C23 170.8(8) . . . . ? C22 C23 C24 O7 177.5(7) . . . . ? C21 C23 C24 O7 -2.8(11) . . . . ? C22 C23 C24 C25 -3.5(11) . . . . ? C21 C23 C24 C25 176.3(7) . . . . ? C5 C4 C3 O1 179.6(8) . . . . ? C1N C4 C3 O1 -2.2(11) . . . . ? C5 C4 C3 C2 -0.5(11) . . . . ? C1N C4 C3 C2 177.8(7) . . . . ? C1 C2 C3 O1 -179.3(8) . . . . ? C28 C2 C3 O1 -2.3(13) . . . . ? C1 C2 C3 C4 0.8(12) . . . . ? C28 C2 C3 C4 177.8(8) . . . . ? C21 C41 C42 C43 -58.9(11) . . . . ? Ag1 N1 C1N C4 -32(20) . . . . ? C5 C4 C1N N1 -30(13) . . . . ? C3 C4 C1N N1 151(13) . . . . ? C37 C36 C35 C14 174.0(9) . . . . ? C16 C14 C35 C36 62.0(9) . . . . ? C13 C14 C35 C36 -173.3(6) . . . . ? C10 C11 C2N N2 -62(16) . . . . ? C12 C11 C2N N2 120(15) . . . . ? C25 C4N N4 Ag1 -32(20) . . . 4_745 ? C2 C28 C47 C48 -177.2(9) . . . . ? C27 C28 C47 C48 -56.0(11) . . . . ? C43 C44 C45 C46 172.7(10) . . . . ? C11 C2N N2 Ag1 120(15) . . . 4_755 ? C41 C42 C43 C44 -171.1(8) . . . . ? C45 C44 C43 C42 179.4(10) . . . . ? C35 C36 C37 C38 178.1(10) . . . . ? C36 C37 C38 C39 -69.6(19) . . . . ? C28 C47 C48 C49 -167.7(10) . . . . ? C47 C48 C49 C50 -178.4(10) . . . . ? C48 C49 C50 C51 168.4(13) . . . . ? C9 C7 C29 C30 -178.9(9) . . . . ? C6 C7 C29 C30 -49.5(12) . . . . ? C7 C29 C30 C31 -168.7(12) . . . . ? C34 C33 C32 C31 -178.9(18) . . . . ? C30' C31' C32' C33' -173(2) . . . . ? C31' C32' C33' C34' 164(4) . . . . ? C2 C1 C6 C5 -4.0(11) . . . . ? C2 C1 C6 C7 -179.3(8) . . . . ? O2 C5 C6 C1 -176.6(8) . . . . ? C4 C5 C6 C1 4.0(11) . . . . ? O2 C5 C6 C7 -1.3(11) . . . . ? C4 C5 C6 C7 179.3(7) . . . . ? C29 C7 C6 C1 -34.2(11) . . . . ? C9 C7 C6 C1 96.6(9) . . . . ? C29 C7 C6 C5 150.7(8) . . . . ? C9 C7 C6 C5 -78.5(9) . . . . ? C37 C38 C39 C40 -79.8(16) . . . . ? C49 C50 C51 C52 -179.6(13) . . . . ? C29 C30 C31 C32 -94.8(18) . . . . ? C33 C32 C31 C30 173.8(18) . . . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.156 _refine_diff_density_min -0.482 _refine_diff_density_rms 0.132