Electronic Supplementary Material for CrystEngComm This Journal is © The Royal SOciety of Chemistry 2005 data_global _journal_name_full CrystEngComm _journal_coden_Cambridge 1350 _publ_contact_author_name 'ProfD Christoph Janiak' _publ_contact_author_address ; Albert-Ludwigs-Universitat Freiburg Institut fur Anorganische Chemie Albertstr. 21 Freiburg D-79104 GERMANY ; _publ_contact_author_email JANIAK@UNI-FREIBURG.DE _publ_section_title ; Chiral S-1,1'-bi-2-naphthol (S-BINOL) as a synthon for supramolecular hydrogen-bonded {(S-BINOLATn{)(S-BINOL)n}-strands with naphthyl-paneled channels or cavities for [Cd(NH3)4]2+ (n = 2) or [Ag(NH3)2]+ (n = 1) (Part 2) ; loop_ _publ_author_name 'Christoph Janiak' 'Katharina Fromm' 'Christian Nather' 'Barbara Paul' data_barbnm _database_code_depnum_ccdc_archive 'CCDC 263506' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Diammine-silver(I)((S)-1,1'-bi-2-naphtholate(-))((S)-1,1'-bi-2-naphthol)- dihydrate-methanol ; _chemical_name_common ; Diammine-silver(i)((S)-1,1'-bi-2-naphtholate(-))((S)-1,1'-bi- 2-naphthol)-dihydrate-methanol ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C41 H41 Ag N2 O7' _chemical_formula_weight 781.63 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 P212121 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 10.815(2) _cell_length_b 9.4999(19) _cell_length_c 35.478(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3645.0(13) _cell_formula_units_Z 4 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plates _exptl_crystal_colour colorless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.424 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1616 _exptl_absorpt_coefficient_mu 0.606 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8297 _exptl_absorpt_correction_T_max 0.9762 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(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 'Bruker AXS CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 24262 _diffrn_reflns_av_R_equivalents 0.0340 _diffrn_reflns_av_sigmaI/netI 0.0604 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 5 _diffrn_reflns_limit_l_min -46 _diffrn_reflns_limit_l_max 49 _diffrn_reflns_theta_min 1.15 _diffrn_reflns_theta_max 30.00 _reflns_number_total 10082 _reflns_number_gt 6649 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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^)+(0.0267P)^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 0.018(16) _refine_ls_number_reflns 10082 _refine_ls_number_parameters 486 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.0669 _refine_ls_R_factor_gt 0.0368 _refine_ls_wR_factor_ref 0.0707 _refine_ls_wR_factor_gt 0.0640 _refine_ls_goodness_of_fit_ref 0.935 _refine_ls_restrained_S_all 0.937 _refine_ls_shift/su_max 0.002 _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 Ag Ag 0.20745(2) 0.51895(2) 0.186832(7) 0.04811(7) Uani 1 1 d . . . N1 N 0.2796(2) 0.3164(2) 0.20156(6) 0.0430(6) Uani 1 1 d . . . H1A H 0.3627 0.3204 0.2023 0.064 Uiso 1 1 calc R . . H1B H 0.2558 0.2527 0.1842 0.064 Uiso 1 1 calc R . . H1C H 0.2505 0.2909 0.2243 0.064 Uiso 1 1 calc R . . N2 N 0.1585(2) 0.7235(2) 0.16648(7) 0.0423(6) Uani 1 1 d . . . H2A H 0.2276 0.7740 0.1624 0.064 Uiso 1 1 calc R . . H2B H 0.1112 0.7675 0.1837 0.064 Uiso 1 1 calc R . . H2C H 0.1161 0.7149 0.1448 0.064 Uiso 1 1 calc R . . O1 O 0.13880(18) 0.0818(2) 0.15848(5) 0.0385(5) Uani 1 1 d . . . H1D H 0.097(3) 0.043(3) 0.1703(9) 0.058 Uiso 1 1 d . . . O2 O 0.33951(19) -0.1272(2) 0.10456(7) 0.0479(6) Uani 1 1 d D . . H2D H 0.273(3) -0.130(4) 0.0974(11) 0.072 Uiso 1 1 d D . . O3 O 0.11366(18) 0.1285(2) 0.24884(5) 0.0355(5) Uani 1 1 d . . . H3A H 0.086(3) 0.062(3) 0.2369(8) 0.053 Uiso 1 1 d . . . O4 O -0.00714(15) 0.43971(17) 0.29433(5) 0.0307(4) Uani 1 1 d . . . O5 O -0.0660(5) -0.2237(4) -0.02721(11) 0.1364(16) Uani 1 1 d D . . H5A H -0.095(6) -0.263(7) -0.0530(14) 0.205 Uiso 1 1 d D . . H5B H -0.028(6) -0.132(6) -0.036(2) 0.205 Uiso 1 1 d D . . O6 O 0.1206(2) -0.2239(3) 0.07912(8) 0.0619(7) Uani 1 1 d . . . H6A H 0.125(4) -0.260(4) 0.0567(12) 0.093 Uiso 1 1 d . . . H6B H 0.045(4) -0.187(4) 0.0767(12) 0.093 Uiso 1 1 d . . . C1 C 0.1817(2) 0.1147(2) 0.09410(7) 0.0261(5) Uani 1 1 d . . . C2 C 0.0971(2) 0.0914(3) 0.12236(7) 0.0287(6) Uani 1 1 d . . . C3 C -0.0310(2) 0.0790(3) 0.11449(8) 0.0346(6) Uani 1 1 d . . . H3B H -0.0875 0.0626 0.1341 0.042 Uiso 1 1 calc R . . C4 C -0.0717(3) 0.0908(3) 0.07835(8) 0.0387(7) Uani 1 1 d . . . H4A H -0.1568 0.0832 0.0734 0.046 Uiso 1 1 calc R . . C5 C -0.0289(3) 0.1251(3) 0.01055(9) 0.0484(8) Uani 1 1 d . . . H5C H -0.1138 0.1183 0.0052 0.058 Uiso 1 1 calc R . . C6 C 0.0517(4) 0.1452(4) -0.01814(9) 0.0556(9) Uani 1 1 d . . . H6C H 0.0226 0.1526 -0.0430 0.067 Uiso 1 1 calc R . . C7 C 0.1787(3) 0.1548(3) -0.01059(8) 0.0491(8) Uani 1 1 d . . . H7C H 0.2348 0.1680 -0.0305 0.059 Uiso 1 1 calc R . . C8 C 0.2215(3) 0.1449(3) 0.02567(7) 0.0395(7) Uani 1 1 d . . . H8A H 0.3069 0.1515 0.0303 0.047 Uiso 1 1 calc R . . C9 C 0.1402(2) 0.1252(3) 0.05600(7) 0.0288(6) Uani 1 1 d . . . C10 C 0.0110(3) 0.1143(3) 0.04800(8) 0.0339(6) Uani 1 1 d . . . C11 C 0.3163(2) 0.1253(3) 0.10354(7) 0.0279(6) Uani 1 1 d . . . C12 C 0.3854(2) 0.0058(3) 0.10876(7) 0.0352(6) Uani 1 1 d . . . C13 C 0.5110(2) 0.0142(4) 0.11957(8) 0.0486(7) Uani 1 1 d . . . H13A H 0.5570 -0.0688 0.1229 0.058 Uiso 1 1 calc R . . C14 C 0.5655(3) 0.1402(4) 0.12518(9) 0.0504(8) Uani 1 1 d . . . H14A H 0.6487 0.1435 0.1327 0.061 Uiso 1 1 calc R . . C15 C 0.5539(3) 0.4019(4) 0.12519(9) 0.0569(9) Uani 1 1 d . . . H15A H 0.6366 0.4084 0.1332 0.068 Uiso 1 1 calc R . . C16 C 0.4887(3) 0.5208(4) 0.11887(9) 0.0606(9) Uani 1 1 d . . . H16A H 0.5273 0.6087 0.1219 0.073 Uiso 1 1 calc R . . C17 C 0.3648(3) 0.5152(3) 0.10787(8) 0.0527(8) Uani 1 1 d . . . H17A H 0.3201 0.5987 0.1039 0.063 Uiso 1 1 calc R . . C18 C 0.3087(3) 0.3867(3) 0.10294(7) 0.0374(6) Uani 1 1 d . . . H18A H 0.2254 0.3834 0.0955 0.045 Uiso 1 1 calc R . . C19 C 0.3735(2) 0.2598(3) 0.10883(7) 0.0317(6) Uani 1 1 d . . . C20 C 0.4999(3) 0.2672(3) 0.11992(8) 0.0411(7) Uani 1 1 d . . . C21 C 0.1486(2) 0.1993(2) 0.31178(8) 0.0249(5) Uani 1 1 d . . . C22 C 0.1085(2) 0.0994(3) 0.28625(7) 0.0278(6) Uani 1 1 d . . . C23 C 0.0648(2) -0.0340(3) 0.29833(8) 0.0327(6) Uani 1 1 d . . . H23A H 0.0375 -0.1003 0.2805 0.039 Uiso 1 1 calc R . . C24 C 0.0624(3) -0.0662(3) 0.33610(8) 0.0388(7) Uani 1 1 d . . . H24A H 0.0314 -0.1540 0.3439 0.047 Uiso 1 1 calc R . . C25 C 0.1085(3) -0.0024(3) 0.40246(7) 0.0446(7) Uani 1 1 d . . . H25A H 0.0777 -0.0894 0.4109 0.054 Uiso 1 1 calc R . . C26 C 0.1551(3) 0.0905(4) 0.42775(8) 0.0546(9) Uani 1 1 d . . . H26A H 0.1580 0.0664 0.4534 0.066 Uiso 1 1 calc R . . C27 C 0.1992(3) 0.2223(3) 0.41597(8) 0.0466(7) Uani 1 1 d . . . H27A H 0.2315 0.2860 0.4337 0.056 Uiso 1 1 calc R . . C28 C 0.1950(3) 0.2578(3) 0.37879(7) 0.0349(6) Uani 1 1 d . . . H28A H 0.2232 0.3472 0.3714 0.042 Uiso 1 1 calc R . . C29 C 0.1493(2) 0.1637(3) 0.35082(7) 0.0286(6) Uani 1 1 d . . . C30 C 0.1055(2) 0.0296(3) 0.36337(7) 0.0331(6) Uani 1 1 d . . . C31 C 0.1959(2) 0.3392(2) 0.29878(6) 0.0236(5) Uani 1 1 d . . . C32 C 0.1159(2) 0.4504(2) 0.29140(7) 0.0264(5) Uani 1 1 d . . . C33 C 0.1679(2) 0.5835(3) 0.28100(8) 0.0343(6) Uani 1 1 d . . . H33A H 0.1146 0.6597 0.2764 0.041 Uiso 1 1 calc R . . C34 C 0.2917(3) 0.6031(3) 0.27756(7) 0.0375(6) Uani 1 1 d . . . H34A H 0.3223 0.6924 0.2710 0.045 Uiso 1 1 calc R . . C35 C 0.5046(2) 0.5068(3) 0.27959(8) 0.0431(7) Uani 1 1 d . . . H35A H 0.5370 0.5943 0.2721 0.052 Uiso 1 1 calc R . . C36 C 0.5828(3) 0.3980(4) 0.28621(9) 0.0522(9) Uani 1 1 d . . . H36A H 0.6684 0.4102 0.2832 0.063 Uiso 1 1 calc R . . C37 C 0.5358(3) 0.2677(3) 0.29753(8) 0.0452(7) Uani 1 1 d . . . H37A H 0.5903 0.1930 0.3025 0.054 Uiso 1 1 calc R . . C38 C 0.4114(2) 0.2480(3) 0.30138(7) 0.0341(6) Uani 1 1 d . . . H38A H 0.3816 0.1589 0.3085 0.041 Uiso 1 1 calc R . . C39 C 0.3263(2) 0.3583(3) 0.29487(7) 0.0276(6) Uani 1 1 d . . . C40 C 0.3753(2) 0.4911(3) 0.28366(7) 0.0336(6) Uani 1 1 d . . . O7 O 0.1326(3) -0.3417(3) 0.00850(9) 0.0900(9) Uani 1 1 d D . . H7A H 0.063(4) -0.303(5) -0.0052(14) 0.135 Uiso 1 1 d D . . C41 C 0.1180(4) -0.4886(5) 0.00384(13) 0.1012(14) Uani 1 1 d . . . H41A H 0.1167 -0.5111 -0.0228 0.152 Uiso 1 1 calc R . . H41B H 0.0408 -0.5182 0.0153 0.152 Uiso 1 1 calc R . . H41C H 0.1863 -0.5373 0.0158 0.152 Uiso 1 1 calc R . . 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 Ag 0.04404(12) 0.03704(10) 0.06326(14) 0.00435(11) -0.00065(12) -0.00259(10) N1 0.0508(15) 0.0403(12) 0.0378(12) 0.0010(10) -0.0015(12) -0.0014(12) N2 0.0349(13) 0.0368(13) 0.0553(15) 0.0013(12) 0.0012(11) 0.0016(10) O1 0.0371(12) 0.0500(12) 0.0283(11) 0.0037(9) -0.0008(8) -0.0117(9) O2 0.0397(13) 0.0323(11) 0.0718(16) 0.0045(11) -0.0049(11) 0.0029(10) O3 0.0447(11) 0.0335(11) 0.0283(10) -0.0024(8) -0.0039(9) -0.0120(9) O4 0.0257(9) 0.0316(10) 0.0346(10) 0.0035(8) -0.0001(8) 0.0055(7) O5 0.191(5) 0.103(3) 0.115(3) 0.002(2) -0.054(3) 0.019(3) O6 0.0572(15) 0.0497(14) 0.0787(17) -0.0114(13) -0.0152(15) 0.0004(12) C1 0.0277(15) 0.0207(11) 0.0298(13) -0.0028(10) -0.0005(11) -0.0002(10) C2 0.0303(15) 0.0262(13) 0.0295(14) -0.0038(11) -0.0007(11) -0.0026(11) C3 0.0270(14) 0.0345(14) 0.0423(16) -0.0014(13) 0.0042(12) -0.0036(12) C4 0.0296(15) 0.0387(16) 0.0476(17) 0.0003(14) -0.0065(13) -0.0007(12) C5 0.0493(19) 0.0520(19) 0.0440(18) 0.0024(16) -0.0164(15) 0.0033(16) C6 0.072(2) 0.064(2) 0.0307(17) 0.0040(16) -0.0171(17) -0.0008(19) C7 0.064(2) 0.0508(18) 0.0326(16) 0.0012(14) 0.0071(15) 0.0031(16) C8 0.0446(18) 0.0416(15) 0.0325(15) -0.0009(12) 0.0023(14) 0.0021(15) C9 0.0334(15) 0.0267(13) 0.0263(13) -0.0013(11) -0.0020(11) 0.0008(11) C10 0.0390(16) 0.0312(14) 0.0316(15) -0.0006(12) -0.0070(12) 0.0017(12) C11 0.0274(15) 0.0300(13) 0.0262(13) 0.0028(10) 0.0005(11) -0.0022(11) C12 0.0335(13) 0.0363(16) 0.0356(14) 0.0037(13) -0.0004(11) -0.0013(13) C13 0.0323(14) 0.059(2) 0.0549(18) 0.0154(18) -0.0028(13) 0.0113(16) C14 0.0245(15) 0.076(2) 0.0504(19) 0.0126(17) -0.0062(14) -0.0111(16) C15 0.051(2) 0.077(3) 0.0428(19) -0.0038(18) 0.0018(16) -0.0340(19) C16 0.082(3) 0.0498(19) 0.0496(19) -0.0081(18) 0.0133(18) -0.036(2) C17 0.069(2) 0.0361(16) 0.0530(18) -0.0095(16) 0.0183(16) -0.0159(17) C18 0.0434(17) 0.0334(14) 0.0354(15) -0.0019(12) 0.0063(14) -0.0075(14) C19 0.0333(15) 0.0377(15) 0.0241(13) 0.0009(12) 0.0043(11) -0.0098(12) C20 0.0381(17) 0.0564(19) 0.0288(15) 0.0011(14) 0.0008(13) -0.0170(15) C21 0.0216(12) 0.0228(11) 0.0304(13) 0.0008(12) -0.0013(11) 0.0031(9) C22 0.0236(13) 0.0279(13) 0.0319(15) 0.0047(11) 0.0007(11) 0.0031(11) C23 0.0352(14) 0.0227(12) 0.0403(14) -0.0012(12) -0.0019(11) -0.0023(11) C24 0.0392(16) 0.0228(13) 0.0543(19) 0.0098(13) 0.0092(14) 0.0013(11) C25 0.0590(17) 0.0385(17) 0.0363(15) 0.0112(15) 0.0065(13) 0.0065(16) C26 0.073(2) 0.059(2) 0.0315(16) 0.0121(16) -0.0009(15) 0.0231(17) C27 0.0509(18) 0.0541(18) 0.0349(15) -0.0035(13) -0.0066(15) 0.0121(18) C28 0.0361(15) 0.0341(13) 0.0344(14) -0.0011(11) -0.0012(13) 0.0046(13) C29 0.0266(13) 0.0279(13) 0.0312(14) 0.0020(11) -0.0017(11) 0.0071(11) C30 0.0340(13) 0.0301(13) 0.0353(14) 0.0076(13) 0.0029(11) 0.0113(13) C31 0.0264(13) 0.0233(11) 0.0211(11) -0.0014(9) -0.0033(11) -0.0024(11) C32 0.0310(14) 0.0229(13) 0.0254(13) -0.0010(10) -0.0021(11) 0.0026(10) C33 0.0392(17) 0.0248(13) 0.0388(15) 0.0026(12) -0.0036(12) 0.0044(11) C34 0.0428(16) 0.0253(12) 0.0443(15) 0.0030(11) 0.0037(15) -0.0073(15) C35 0.0368(15) 0.0442(17) 0.0481(16) 0.0023(16) 0.0007(12) -0.0148(15) C36 0.0267(16) 0.067(2) 0.063(2) 0.0036(18) 0.0046(15) -0.0111(15) C37 0.0291(15) 0.0536(18) 0.0529(19) -0.0013(15) -0.0012(14) 0.0096(14) C38 0.0297(15) 0.0344(14) 0.0383(16) -0.0003(12) -0.0014(11) 0.0008(12) C39 0.0296(14) 0.0294(13) 0.0238(13) -0.0022(11) -0.0036(10) -0.0009(10) C40 0.0315(13) 0.0355(15) 0.0337(13) -0.0018(13) -0.0017(11) -0.0051(13) O7 0.096(2) 0.076(2) 0.098(2) 0.0014(17) -0.0176(18) -0.0019(17) C41 0.109(3) 0.071(3) 0.124(4) -0.006(3) 0.018(3) 0.033(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 Ag N2 2.139(2) . ? Ag N1 2.141(2) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N1 H1C 0.9000 . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N2 H2C 0.9000 . ? O1 C2 1.361(3) . ? O1 H1D 0.72(3) . ? O2 C12 1.365(3) . ? O2 H2D 0.76(3) . ? O3 C22 1.357(3) . ? O3 H3A 0.82(3) . ? O4 C32 1.339(3) . ? O5 H5A 1.04(4) . ? O5 H5B 1.02(4) . ? O6 H6A 0.87(4) . ? O6 H6B 0.89(4) . ? C1 C2 1.375(3) . ? C1 C9 1.428(3) . ? C1 C11 1.497(4) . ? C2 C3 1.418(4) . ? C3 C4 1.361(4) . ? C3 H3B 0.9400 . ? C4 C10 1.418(4) . ? C4 H4A 0.9400 . ? C5 C6 1.354(5) . ? C5 C10 1.401(4) . ? C5 H5C 0.9400 . ? C6 C7 1.403(5) . ? C6 H6C 0.9400 . ? C7 C8 1.370(4) . ? C7 H7C 0.9400 . ? C8 C9 1.402(4) . ? C8 H8A 0.9400 . ? C9 C10 1.429(4) . ? C11 C12 1.372(4) . ? C11 C19 1.432(3) . ? C12 C13 1.413(4) . ? C13 C14 1.349(4) . ? C13 H13A 0.9400 . ? C14 C20 1.412(4) . ? C14 H14A 0.9400 . ? C15 C16 1.350(5) . ? C15 C20 1.419(4) . ? C15 H15A 0.9400 . ? C16 C17 1.397(5) . ? C16 H16A 0.9400 . ? C17 C18 1.374(4) . ? C17 H17A 0.9400 . ? C18 C19 1.410(4) . ? C18 H18A 0.9400 . ? C19 C20 1.424(4) . ? C21 C22 1.381(3) . ? C21 C29 1.426(4) . ? C21 C31 1.497(3) . ? C22 C23 1.419(3) . ? C23 C24 1.375(4) . ? C23 H23A 0.9400 . ? C24 C30 1.408(4) . ? C24 H24A 0.9400 . ? C25 C26 1.356(4) . ? C25 C30 1.420(3) . ? C25 H25A 0.9400 . ? C26 C27 1.404(4) . ? C26 H26A 0.9400 . ? C27 C28 1.362(4) . ? C27 H27A 0.9400 . ? C28 C29 1.425(4) . ? C28 H28A 0.9400 . ? C29 C30 1.430(4) . ? C31 C32 1.390(3) . ? C31 C39 1.430(4) . ? C32 C33 1.432(3) . ? C33 C34 1.358(4) . ? C33 H33A 0.9400 . ? C34 C40 1.413(4) . ? C34 H34A 0.9400 . ? C35 C36 1.356(4) . ? C35 C40 1.413(3) . ? C35 H35A 0.9400 . ? C36 C37 1.397(4) . ? C36 H36A 0.9400 . ? C37 C38 1.366(4) . ? C37 H37A 0.9400 . ? C38 C39 1.413(3) . ? C38 H38A 0.9400 . ? C39 C40 1.425(4) . ? O7 C41 1.415(5) . ? O7 H7A 0.97(4) . ? C41 H41A 0.9700 . ? C41 H41B 0.9700 . ? C41 H41C 0.9700 . ? 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 N2 Ag N1 171.40(9) . . ? Ag N1 H1A 109.5 . . ? Ag N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? Ag N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? Ag N2 H2A 109.5 . . ? Ag N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? Ag N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C2 O1 H1D 112(3) . . ? C12 O2 H2D 114(3) . . ? C22 O3 H3A 109(2) . . ? H5A O5 H5B 99(5) . . ? H6A O6 H6B 97(4) . . ? C2 C1 C9 119.5(2) . . ? C2 C1 C11 119.6(2) . . ? C9 C1 C11 120.8(2) . . ? O1 C2 C1 118.5(2) . . ? O1 C2 C3 120.2(2) . . ? C1 C2 C3 121.3(2) . . ? C4 C3 C2 119.7(3) . . ? C4 C3 H3B 120.2 . . ? C2 C3 H3B 120.2 . . ? C3 C4 C10 121.6(3) . . ? C3 C4 H4A 119.2 . . ? C10 C4 H4A 119.2 . . ? C6 C5 C10 121.7(3) . . ? C6 C5 H5C 119.2 . . ? C10 C5 H5C 119.2 . . ? C5 C6 C7 119.7(3) . . ? C5 C6 H6C 120.1 . . ? C7 C6 H6C 120.1 . . ? C8 C7 C6 120.4(3) . . ? C8 C7 H7C 119.8 . . ? C6 C7 H7C 119.8 . . ? C7 C8 C9 121.2(3) . . ? C7 C8 H8A 119.4 . . ? C9 C8 H8A 119.4 . . ? C8 C9 C1 122.6(2) . . ? C8 C9 C10 118.0(2) . . ? C1 C9 C10 119.3(2) . . ? C5 C10 C4 122.5(3) . . ? C5 C10 C9 119.0(3) . . ? C4 C10 C9 118.5(2) . . ? C12 C11 C19 119.0(2) . . ? C12 C11 C1 120.3(2) . . ? C19 C11 C1 120.7(2) . . ? O2 C12 C11 123.6(2) . . ? O2 C12 C13 115.5(3) . . ? C11 C12 C13 120.9(3) . . ? C14 C13 C12 120.7(3) . . ? C14 C13 H13A 119.7 . . ? C12 C13 H13A 119.7 . . ? C13 C14 C20 121.3(3) . . ? C13 C14 H14A 119.4 . . ? C20 C14 H14A 119.4 . . ? C16 C15 C20 121.1(3) . . ? C16 C15 H15A 119.4 . . ? C20 C15 H15A 119.4 . . ? C15 C16 C17 121.0(3) . . ? C15 C16 H16A 119.5 . . ? C17 C16 H16A 119.5 . . ? C18 C17 C16 119.5(3) . . ? C18 C17 H17A 120.2 . . ? C16 C17 H17A 120.2 . . ? C17 C18 C19 121.4(3) . . ? C17 C18 H18A 119.3 . . ? C19 C18 H18A 119.3 . . ? C18 C19 C20 118.4(3) . . ? C18 C19 C11 121.9(2) . . ? C20 C19 C11 119.7(3) . . ? C14 C20 C15 123.1(3) . . ? C14 C20 C19 118.5(3) . . ? C15 C20 C19 118.5(3) . . ? C22 C21 C29 118.4(2) . . ? C22 C21 C31 121.0(2) . . ? C29 C21 C31 120.5(2) . . ? O3 C22 C21 119.3(2) . . ? O3 C22 C23 119.4(2) . . ? C21 C22 C23 121.3(2) . . ? C24 C23 C22 120.0(2) . . ? C24 C23 H23A 120.0 . . ? C22 C23 H23A 120.0 . . ? C23 C24 C30 121.3(2) . . ? C23 C24 H24A 119.4 . . ? C30 C24 H24A 119.4 . . ? C26 C25 C30 121.0(3) . . ? C26 C25 H25A 119.5 . . ? C30 C25 H25A 119.5 . . ? C25 C26 C27 120.7(3) . . ? C25 C26 H26A 119.7 . . ? C27 C26 H26A 119.7 . . ? C28 C27 C26 119.9(3) . . ? C28 C27 H27A 120.1 . . ? C26 C27 H27A 120.1 . . ? C27 C28 C29 122.0(3) . . ? C27 C28 H28A 119.0 . . ? C29 C28 H28A 119.0 . . ? C28 C29 C21 122.0(2) . . ? C28 C29 C30 117.2(2) . . ? C21 C29 C30 120.8(2) . . ? C24 C30 C25 122.7(3) . . ? C24 C30 C29 118.1(2) . . ? C25 C30 C29 119.2(3) . . ? C32 C31 C39 119.9(2) . . ? C32 C31 C21 121.4(2) . . ? C39 C31 C21 118.7(2) . . ? O4 C32 C31 123.1(2) . . ? O4 C32 C33 118.5(2) . . ? C31 C32 C33 118.4(2) . . ? C34 C33 C32 122.1(2) . . ? C34 C33 H33A 119.0 . . ? C32 C33 H33A 119.0 . . ? C33 C34 C40 121.0(2) . . ? C33 C34 H34A 119.5 . . ? C40 C34 H34A 119.5 . . ? C36 C35 C40 121.3(3) . . ? C36 C35 H35A 119.4 . . ? C40 C35 H35A 119.4 . . ? C35 C36 C37 119.9(3) . . ? C35 C36 H36A 120.1 . . ? C37 C36 H36A 120.1 . . ? C38 C37 C36 120.6(3) . . ? C38 C37 H37A 119.7 . . ? C36 C37 H37A 119.7 . . ? C37 C38 C39 121.5(3) . . ? C37 C38 H38A 119.2 . . ? C39 C38 H38A 119.2 . . ? C38 C39 C40 117.4(2) . . ? C38 C39 C31 122.2(2) . . ? C40 C39 C31 120.4(2) . . ? C34 C40 C35 122.5(3) . . ? C34 C40 C39 118.1(2) . . ? C35 C40 C39 119.3(2) . . ? C41 O7 H7A 103(3) . . ? O7 C41 H41A 109.5 . . ? O7 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? O7 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? 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 N1 H1B O1 0.90 2.25 3.102(3) 157.2 . N1 H1C O3 0.90 2.31 3.036(3) 137.9 . N2 H2A O2 0.90 2.56 3.267(3) 135.8 1_565 N2 H2B O4 0.90 2.13 2.972(3) 154.7 3 N2 H2C O6 0.90 2.40 3.166(4) 143.0 1_565 O1 H1D O4 0.72(3) 1.87(3) 2.579(2) 172(4) 3_545 O2 H2D O6 0.76(3) 1.98(3) 2.695(3) 155(4) . O3 H3A O4 0.82(3) 1.82(3) 2.625(2) 169(3) 3_545 O5 H5A O2 1.04(4) 2.22(4) 3.253(5) 173(6) 4_445 O6 H6A O7 0.87(4) 1.88(4) 2.747(4) 179(5) . O7 H7A O5 0.97(4) 1.77(4) 2.734(5) 176(5) . _diffrn_measured_fraction_theta_max 0.972 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.972 _refine_diff_density_max 0.356 _refine_diff_density_min -0.901 _refine_diff_density_rms 0.062 data_barbkm _database_code_depnum_ccdc_archive 'CCDC 264202' _audit_creation_method SHELXL-97 _chemical_name_systematic ; [tetraammine-\k^2^O,O'-((S)-1,1'-bi-2-naphtholate(2-))cadmium(II)]- bis((S)-1,1'-bi-2-naphthol)hydrate-bis(methanol) ; _chemical_name_common ; (tetraammine-kappa$2!O,O'-((S)-1,1'-bi-2-naphtholate(2- ))cadmium(ii))-bis((S)-1,1'-bi-2-naphthol)hydrate-bis(methanol) ; _chemical_melting_point ? _chemical_formula_moiety '[Cd(C20 H12 O2)(NH3)4], 2(C20 H14 O2), H2O, 2(CH3OH)' _chemical_formula_sum 'C62 H62 Cd N4 O9' _chemical_formula_weight 1119.56 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' Cd Cd -0.8075 1.2024 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M C2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z' _cell_length_a 24.024(6) _cell_length_b 10.689(2) _cell_length_c 10.982(2) _cell_angle_alpha 90.00 _cell_angle_beta 108.657(4) _cell_angle_gamma 90.00 _cell_volume 2671.9(10) _cell_formula_units_Z 2 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description isometric _exptl_crystal_colour colorless _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.392 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1164 _exptl_absorpt_coefficient_mu 0.472 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.8952 _exptl_absorpt_correction_T_max 0.9369 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(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 'Bruker AXS CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 10963 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0467 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 1.79 _diffrn_reflns_theta_max 26.30 _reflns_number_total 5303 _reflns_number_gt 4835 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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. Hydrogen atoms on the aromatic rings and methanol molecule were placed at calculated positions with an appropriate riding model (AFIX 43 for CH and AFIX 133 for CH3) and an isotropic temperature factor of Ueq(H) = 1.2 Ueq(CH) and 1.5 Ueg(CH3). The hydrogen atoms of the ammin ligands were calculated as an idealized NH3 group with tetrahedral angles in a rotating group refinement (AFIX 137) with Ueq(H) = 1.5 Ueq(N). Hydrogen atoms on the BINOL-OH groups, methanol-OH and the water protons were found and refined with Ueq(H) = 1.5 Ueq(O). ; _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^)+(0.0138P)^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 0.017(12) _refine_ls_number_reflns 5303 _refine_ls_number_parameters 358 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0308 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0467 _refine_ls_wR_factor_gt 0.0454 _refine_ls_goodness_of_fit_ref 0.930 _refine_ls_restrained_S_all 0.930 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cd Cd 0.5000 0.57317(2) 1.0000 0.03970(7) Uani 1 2 d S . . N1 N 0.43366(8) 0.5775(4) 0.78751(17) 0.0680(6) Uani 1 1 d . . . H1B H 0.4476 0.6288 0.7391 0.102 Uiso 1 1 calc R . . H1C H 0.3985 0.6054 0.7885 0.102 Uiso 1 1 calc R . . H1D H 0.4297 0.4998 0.7542 0.102 Uiso 1 1 calc R . . N2 N 0.56058(11) 0.4127(2) 0.9619(3) 0.0596(8) Uani 1 1 d . . . H2C H 0.5969 0.4430 0.9741 0.089 Uiso 1 1 calc R . . H2D H 0.5453 0.3852 0.8805 0.089 Uiso 1 1 calc R . . H2B H 0.5625 0.3489 1.0166 0.089 Uiso 1 1 calc R . . O1 O 0.39903(7) 0.60208(14) 0.17493(15) 0.0445(5) Uani 1 1 d . . . H1A H 0.4182(11) 0.665(2) 0.140(2) 0.067 Uiso 1 1 d . . . O2 O 0.43815(8) 0.40694(15) 0.51773(18) 0.0481(5) Uani 1 1 d . . . H2A H 0.4457(14) 0.472(3) 0.506(3) 0.072 Uiso 1 1 d . . . O3 O 0.54389(8) 0.74144(19) 0.92675(17) 0.0317(5) Uani 1 1 d . . . O4 O 0.48718(10) 0.7924(2) 0.6772(2) 0.0758(6) Uani 1 1 d D . . H4A H 0.5039(14) 0.794(3) 0.774(3) 0.114 Uiso 1 1 d D . . O5 O 0.5000 0.6215(2) 0.5000 0.0532(8) Uani 1 2 d S . . H5A H 0.4972(14) 0.672(2) 0.439(3) 0.080 Uiso 1 1 d . . . C1 C 0.35438(8) 0.5526(2) 0.32877(18) 0.0279(6) Uani 1 1 d . . . C2 C 0.37333(10) 0.6421(2) 0.2614(2) 0.0320(5) Uani 1 1 d . . . C3 C 0.36650(13) 0.7695(2) 0.2813(3) 0.0379(7) Uani 1 1 d . . . H3 H 0.3782 0.8291 0.2314 0.045 Uiso 1 1 calc R . . C4 C 0.34292(10) 0.8080(2) 0.3726(2) 0.0402(6) Uani 1 1 d . . . H4B H 0.3400 0.8940 0.3871 0.048 Uiso 1 1 calc R . . C5 C 0.29931(11) 0.7581(2) 0.5424(2) 0.0453(6) Uani 1 1 d . . . H5B H 0.2971 0.8436 0.5601 0.054 Uiso 1 1 calc R . . C6 C 0.27966(12) 0.6730(3) 0.6106(3) 0.0520(8) Uani 1 1 d . . . H6 H 0.2640 0.6997 0.6744 0.062 Uiso 1 1 calc R . . C7 C 0.28279(11) 0.5460(3) 0.5857(2) 0.0449(8) Uani 1 1 d . . . H7 H 0.2682 0.4873 0.6316 0.054 Uiso 1 1 calc R . . C8 C 0.30691(9) 0.5052(2) 0.4950(2) 0.0369(6) Uani 1 1 d . . . H8 H 0.3094 0.4189 0.4810 0.044 Uiso 1 1 calc R . . C9 C 0.32802(8) 0.5914(3) 0.42256(18) 0.0288(6) Uani 1 1 d . . . C10 C 0.32307(10) 0.7218(2) 0.4451(2) 0.0350(5) Uani 1 1 d . . . C11 C 0.36486(11) 0.4170(2) 0.3098(3) 0.0303(6) Uani 1 1 d . . . C12 C 0.40572(10) 0.3520(2) 0.4057(2) 0.0375(6) Uani 1 1 d . . . C13 C 0.41559(12) 0.2230(2) 0.3909(3) 0.0496(7) Uani 1 1 d . . . H13 H 0.4423 0.1787 0.4585 0.060 Uiso 1 1 calc R . . C14 C 0.38704(12) 0.1636(2) 0.2808(3) 0.0552(8) Uani 1 1 d . . . H14 H 0.3940 0.0779 0.2732 0.066 Uiso 1 1 calc R . . C15 C 0.31994(13) 0.1683(3) 0.0557(3) 0.0589(8) Uani 1 1 d . . . H15 H 0.3281 0.0839 0.0445 0.071 Uiso 1 1 calc R . . C16 C 0.28271(14) 0.2319(3) -0.0436(3) 0.0647(9) Uani 1 1 d . . . H16 H 0.2654 0.1917 -0.1228 0.078 Uiso 1 1 calc R . . C17 C 0.26992(11) 0.3579(3) -0.0285(3) 0.0542(7) Uani 1 1 d . . . H17 H 0.2439 0.4017 -0.0978 0.065 Uiso 1 1 calc R . . C18 C 0.29483(10) 0.4174(2) 0.0857(2) 0.0407(6) Uani 1 1 d . . . H18 H 0.2854 0.5015 0.0946 0.049 Uiso 1 1 calc R . . C19 C 0.33477(10) 0.3543(2) 0.1915(2) 0.0337(5) Uani 1 1 d . . . C20 C 0.34685(11) 0.2263(2) 0.1760(3) 0.0442(6) Uani 1 1 d . . . C21 C 0.53253(8) 0.92862(18) 1.03322(19) 0.0253(5) Uani 1 1 d . . . C22 C 0.56740(9) 0.83406(19) 1.0089(2) 0.0275(5) Uani 1 1 d . . . C23 C 0.62912(9) 0.8364(2) 1.0711(2) 0.0334(5) Uani 1 1 d . . . H23 H 0.6526 0.7728 1.0542 0.040 Uiso 1 1 calc R . . C24 C 0.65475(10) 0.9300(2) 1.1552(2) 0.0365(6) Uani 1 1 d . . . H24 H 0.6958 0.9303 1.1940 0.044 Uiso 1 1 calc R . . C25 C 0.64673(11) 1.1197(2) 1.2749(2) 0.0465(7) Uani 1 1 d . . . H25 H 0.6877 1.1206 1.3144 0.056 Uiso 1 1 calc R . . C26 C 0.61368(12) 1.2092(3) 1.3061(3) 0.0544(7) Uani 1 1 d . . . H26 H 0.6315 1.2716 1.3663 0.065 Uiso 1 1 calc R . . C27 C 0.55243(12) 1.2079(2) 1.2474(2) 0.0507(7) Uani 1 1 d . . . H27 H 0.5293 1.2694 1.2694 0.061 Uiso 1 1 calc R . . C28 C 0.52620(11) 1.11922(19) 1.1597(2) 0.0387(6) Uani 1 1 d . . . H28 H 0.4851 1.1205 1.1219 0.046 Uiso 1 1 calc R . . C29 C 0.55911(9) 1.02451(18) 1.1236(2) 0.0283(5) Uani 1 1 d . . . C30 C 0.62112(10) 1.02531(19) 1.1846(2) 0.0323(5) Uani 1 1 d . . . C31 C 0.4670(2) 0.8987(4) 0.6173(4) 0.1337(18) Uani 1 1 d . . . H31A H 0.4310 0.9218 0.6335 0.201 Uiso 1 1 calc R . . H31B H 0.4592 0.8881 0.5256 0.201 Uiso 1 1 calc R . . H31C H 0.4961 0.9641 0.6488 0.201 Uiso 1 1 calc R . . 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 Cd 0.04094(14) 0.03023(12) 0.05411(16) 0.000 0.02388(12) 0.000 N1 0.0703(14) 0.0598(13) 0.0657(14) -0.011(2) 0.0100(11) -0.018(2) N2 0.0638(18) 0.0374(15) 0.097(2) 0.0018(15) 0.0536(17) 0.0024(13) O1 0.0652(11) 0.0309(13) 0.0544(10) -0.0005(8) 0.0429(9) -0.0051(8) O2 0.0529(11) 0.0376(11) 0.0479(12) 0.0106(9) 0.0078(9) 0.0009(9) O3 0.0362(10) 0.0295(10) 0.0329(10) -0.0043(8) 0.0163(9) -0.0019(7) O4 0.1066(18) 0.0711(15) 0.0411(13) 0.0027(11) 0.0113(12) 0.0145(13) O5 0.0670(18) 0.0436(17) 0.0411(17) 0.000 0.0064(15) 0.000 C1 0.0269(10) 0.0258(17) 0.0311(11) 0.0011(10) 0.0093(9) -0.0017(10) C2 0.0329(13) 0.0292(13) 0.0350(14) 0.0013(10) 0.0126(11) 0.0004(10) C3 0.0440(17) 0.0236(15) 0.0490(19) 0.0044(12) 0.0189(14) -0.0004(12) C4 0.0463(15) 0.0265(13) 0.0490(16) -0.0017(11) 0.0167(13) 0.0035(11) C5 0.0492(17) 0.0408(14) 0.0499(17) -0.0097(13) 0.0213(14) 0.0042(12) C6 0.0507(17) 0.066(2) 0.0461(17) -0.0112(16) 0.0254(14) 0.0018(16) C7 0.0442(13) 0.055(3) 0.0417(15) 0.0002(13) 0.0226(11) -0.0038(13) C8 0.0320(13) 0.0416(14) 0.0385(14) 0.0022(11) 0.0133(12) -0.0035(11) C9 0.0263(10) 0.0295(17) 0.0288(11) -0.0001(11) 0.0061(9) 0.0002(11) C10 0.0346(13) 0.0340(13) 0.0350(14) -0.0059(11) 0.0091(11) 0.0011(11) C11 0.0304(13) 0.0271(15) 0.0393(15) 0.0004(12) 0.0196(12) -0.0019(11) C12 0.0422(14) 0.0306(13) 0.0437(16) 0.0047(11) 0.0194(12) -0.0024(11) C13 0.0526(17) 0.0308(14) 0.068(2) 0.0115(13) 0.0229(15) 0.0077(13) C14 0.0635(19) 0.0260(13) 0.087(2) -0.0036(15) 0.0388(17) 0.0029(13) C15 0.070(2) 0.0399(16) 0.076(2) -0.0285(16) 0.0354(18) -0.0158(15) C16 0.070(2) 0.068(2) 0.063(2) -0.0336(18) 0.0307(18) -0.0267(17) C17 0.0457(16) 0.067(2) 0.0470(17) -0.0115(15) 0.0111(13) -0.0133(15) C18 0.0345(14) 0.0447(15) 0.0453(16) -0.0100(12) 0.0162(12) -0.0081(11) C19 0.0331(13) 0.0315(13) 0.0439(15) -0.0058(11) 0.0226(12) -0.0084(11) C20 0.0471(16) 0.0308(14) 0.0659(19) -0.0073(13) 0.0338(15) -0.0087(12) C21 0.0269(11) 0.0237(11) 0.0269(12) 0.0025(9) 0.0111(9) -0.0008(9) C22 0.0323(12) 0.0267(12) 0.0269(12) 0.0019(10) 0.0141(10) -0.0042(10) C23 0.0302(13) 0.0348(13) 0.0383(14) 0.0045(11) 0.0152(11) 0.0048(10) C24 0.0266(12) 0.0465(14) 0.0350(14) 0.0048(11) 0.0078(11) -0.0020(11) C25 0.0410(15) 0.0546(18) 0.0430(15) -0.0097(12) 0.0122(13) -0.0132(12) C26 0.0581(18) 0.0550(18) 0.0478(17) -0.0241(14) 0.0138(15) -0.0162(15) C27 0.0579(18) 0.0449(16) 0.0500(17) -0.0190(13) 0.0182(15) 0.0009(14) C28 0.0422(14) 0.0359(14) 0.0378(14) -0.0071(10) 0.0124(12) 0.0014(10) C29 0.0316(12) 0.0280(11) 0.0259(12) 0.0016(9) 0.0102(10) -0.0035(9) C30 0.0331(13) 0.0375(13) 0.0278(13) -0.0007(10) 0.0118(11) -0.0073(10) C31 0.156(4) 0.125(4) 0.101(4) -0.035(3) 0.015(3) 0.038(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 Cd O3 2.3530(19) 2_657 ? Cd O3 2.353(2) . ? Cd N1 2.3681(18) . ? Cd N1 2.3681(18) 2_657 ? Cd N2 2.372(2) . ? Cd N2 2.372(2) 2_657 ? N1 H1B 0.9000 . ? N1 H1C 0.9000 . ? N1 H1D 0.9000 . ? N2 H2C 0.9000 . ? N2 H2D 0.9000 . ? N2 H2B 0.9000 . ? O1 C2 1.357(3) . ? O1 H1A 0.96(3) . ? O2 C12 1.361(3) . ? O2 H2A 0.74(3) . ? O3 C22 1.337(3) . ? O4 C31 1.325(4) . ? O4 H4A 1.01(3) . ? O5 H5A 0.85(2) . ? C1 C2 1.373(3) . ? C1 C9 1.432(3) . ? C1 C11 1.497(3) . ? C2 C3 1.397(3) . ? C3 C4 1.364(3) . ? C3 H3 0.9400 . ? C4 C10 1.397(3) . ? C4 H4B 0.9400 . ? C5 C6 1.355(3) . ? C5 C10 1.417(3) . ? C5 H5B 0.9400 . ? C6 C7 1.392(4) . ? C6 H6 0.9400 . ? C7 C8 1.374(3) . ? C7 H7 0.9400 . ? C8 C9 1.413(3) . ? C8 H8 0.9400 . ? C9 C10 1.428(3) . ? C11 C12 1.376(3) . ? C11 C19 1.434(3) . ? C12 C13 1.417(3) . ? C13 C14 1.344(4) . ? C13 H13 0.9400 . ? C14 C20 1.412(4) . ? C14 H14 0.9400 . ? C15 C16 1.352(4) . ? C15 C20 1.415(4) . ? C15 H15 0.9400 . ? C16 C17 1.403(4) . ? C16 H16 0.9400 . ? C17 C18 1.362(3) . ? C17 H17 0.9400 . ? C18 C19 1.418(3) . ? C18 H18 0.9400 . ? C19 C20 1.420(3) . ? C21 C22 1.392(3) . ? C21 C29 1.427(3) . ? C21 C21 1.499(4) 2_657 ? C22 C23 1.420(3) . ? C23 C24 1.367(3) . ? C23 H23 0.9400 . ? C24 C30 1.401(3) . ? C24 H24 0.9400 . ? C25 C26 1.356(3) . ? C25 C30 1.411(3) . ? C25 H25 0.9400 . ? C26 C27 1.405(4) . ? C26 H26 0.9400 . ? C27 C28 1.355(3) . ? C27 H27 0.9400 . ? C28 C29 1.417(3) . ? C28 H28 0.9400 . ? C29 C30 1.425(3) . ? C31 H31A 0.9700 . ? C31 H31B 0.9700 . ? C31 H31C 0.9700 . ? 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 O3 Cd O3 80.29(9) 2_657 . ? O3 Cd N1 95.05(9) 2_657 . ? O3 Cd N1 83.24(9) . . ? O3 Cd N1 83.24(9) 2_657 2_657 ? O3 Cd N1 95.05(9) . 2_657 ? N1 Cd N1 177.78(19) . 2_657 ? O3 Cd N2 168.68(9) 2_657 . ? O3 Cd N2 97.20(6) . . ? N1 Cd N2 95.61(11) . . ? N1 Cd N2 86.00(11) 2_657 . ? O3 Cd N2 97.20(6) 2_657 2_657 ? O3 Cd N2 168.68(9) . 2_657 ? N1 Cd N2 86.00(11) . 2_657 ? N1 Cd N2 95.61(11) 2_657 2_657 ? N2 Cd N2 87.34(12) . 2_657 ? Cd N1 H1B 109.5 . . ? Cd N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? Cd N1 H1D 109.5 . . ? H1B N1 H1D 109.5 . . ? H1C N1 H1D 109.5 . . ? Cd N2 H2C 109.5 . . ? Cd N2 H2D 109.5 . . ? H2C N2 H2D 109.5 . . ? Cd N2 H2B 109.5 . . ? H2C N2 H2B 109.5 . . ? H2D N2 H2B 109.5 . . ? C2 O1 H1A 116.6(15) . . ? C12 O2 H2A 111(2) . . ? C22 O3 Cd 118.32(14) . . ? C31 O4 H4A 118(2) . . ? C2 C1 C9 119.0(2) . . ? C2 C1 C11 120.0(2) . . ? C9 C1 C11 120.9(2) . . ? O1 C2 C1 117.5(2) . . ? O1 C2 C3 121.3(2) . . ? C1 C2 C3 121.3(2) . . ? C4 C3 C2 120.4(2) . . ? C4 C3 H3 119.8 . . ? C2 C3 H3 119.8 . . ? C3 C4 C10 121.2(2) . . ? C3 C4 H4B 119.4 . . ? C10 C4 H4B 119.4 . . ? C6 C5 C10 121.9(2) . . ? C6 C5 H5B 119.0 . . ? C10 C5 H5B 119.0 . . ? C5 C6 C7 119.7(2) . . ? C5 C6 H6 120.1 . . ? C7 C6 H6 120.1 . . ? C8 C7 C6 120.9(2) . . ? C8 C7 H7 119.5 . . ? C6 C7 H7 119.5 . . ? C7 C8 C9 120.8(2) . . ? C7 C8 H8 119.6 . . ? C9 C8 H8 119.6 . . ? C8 C9 C10 118.3(2) . . ? C8 C9 C1 122.5(2) . . ? C10 C9 C1 119.2(2) . . ? C4 C10 C5 122.8(2) . . ? C4 C10 C9 118.9(2) . . ? C5 C10 C9 118.3(2) . . ? C12 C11 C19 119.1(2) . . ? C12 C11 C1 119.5(2) . . ? C19 C11 C1 121.3(2) . . ? O2 C12 C11 122.4(2) . . ? O2 C12 C13 117.1(2) . . ? C11 C12 C13 120.5(2) . . ? C14 C13 C12 120.5(3) . . ? C14 C13 H13 119.8 . . ? C12 C13 H13 119.8 . . ? C13 C14 C20 121.9(2) . . ? C13 C14 H14 119.1 . . ? C20 C14 H14 119.1 . . ? C16 C15 C20 121.3(3) . . ? C16 C15 H15 119.3 . . ? C20 C15 H15 119.3 . . ? C15 C16 C17 120.1(3) . . ? C15 C16 H16 120.0 . . ? C17 C16 H16 120.0 . . ? C18 C17 C16 120.6(3) . . ? C18 C17 H17 119.7 . . ? C16 C17 H17 119.7 . . ? C17 C18 C19 121.0(2) . . ? C17 C18 H18 119.5 . . ? C19 C18 H18 119.5 . . ? C18 C19 C20 118.1(2) . . ? C18 C19 C11 122.2(2) . . ? C20 C19 C11 119.7(2) . . ? C14 C20 C15 122.8(2) . . ? C14 C20 C19 118.2(2) . . ? C15 C20 C19 118.9(3) . . ? C22 C21 C29 119.47(18) . . ? C22 C21 C21 120.30(16) . 2_657 ? C29 C21 C21 120.22(16) . 2_657 ? O3 C22 C21 121.13(19) . . ? O3 C22 C23 119.2(2) . . ? C21 C22 C23 119.64(19) . . ? C24 C23 C22 120.9(2) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C23 C24 C30 121.3(2) . . ? C23 C24 H24 119.3 . . ? C30 C24 H24 119.3 . . ? C26 C25 C30 121.6(2) . . ? C26 C25 H25 119.2 . . ? C30 C25 H25 119.2 . . ? C25 C26 C27 119.3(2) . . ? C25 C26 H26 120.4 . . ? C27 C26 H26 120.4 . . ? C28 C27 C26 120.9(2) . . ? C28 C27 H27 119.5 . . ? C26 C27 H27 119.5 . . ? C27 C28 C29 121.6(2) . . ? C27 C28 H28 119.2 . . ? C29 C28 H28 119.2 . . ? C28 C29 C30 117.20(19) . . ? C28 C29 C21 122.8(2) . . ? C30 C29 C21 119.94(19) . . ? C24 C30 C25 121.9(2) . . ? C24 C30 C29 118.7(2) . . ? C25 C30 C29 119.4(2) . . ? O4 C31 H31A 109.5 . . ? O4 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O4 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? 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 N1 H1B O4 0.90 2.20 3.065(4) 161.3 . N2 H2C O1 0.90 2.38 2.869(3) 114.0 2_656 O1 H1A O3 0.96(3) 1.57(3) 2.515(2) 167(2) 2_656 O2 H2A O5 0.74(3) 2.08(3) 2.773(3) 157(3) . O4 H4A O3 1.01(3) 1.74(3) 2.698(3) 157(3) . O5 H5A O4 0.85(2) 1.93(3) 2.757(3) 165(3) 2_656 _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.30 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.431 _refine_diff_density_min -0.507 _refine_diff_density_rms 0.040 data_barbgm _database_code_depnum_ccdc_archive 'CCDC 264203' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Diammine-silver(I)((S)-1,1'-bi-2-naphtholate(-))((S)-1,1'-bi-2-naphthol)- ethanol ; _chemical_name_common ; Diammine-silver(i)((S)-1,1'-bi-2-naphtholate(-))((S)-1,1'-bi- 2-naphthol)-ethanol ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H39 Ag N2 O5' _chemical_formula_weight 759.62 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 triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.373(3) _cell_length_b 10.796(3) _cell_length_c 18.074(5) _cell_angle_alpha 78.215(5) _cell_angle_beta 81.104(5) _cell_angle_gamma 89.636(5) _cell_volume 1768.3(8) _cell_formula_units_Z 2 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description isometric _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.619 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7682 _exptl_absorpt_correction_T_max 0.9877 _exptl_absorpt_process_details SADABS _exptl_special_details ; Compound was formed in enantiomeric excess from rac-BINOL by spontaneous resolution upon crystallization. ; _diffrn_ambient_temperature 243(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 'Bruker AXS CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15031 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.1550 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 26.90 _reflns_number_total 13383 _reflns_number_gt 6348 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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. Hydrogen atoms on the aromatic rings and ethanol molecules were placed at calculated positions with an appropriate riding model (AFIX 43 for CH, AFIX 23 for CH2, and AFIX 33 for CH3) and an isotropic temperature factor of Ueq(H) = 1.2 Ueq(CH, CH2) and 1.5 Ueg(CH3). The hydrogen atoms of the ammin ligands were calculated as an idealized NH3 group with tetrahedral angles in a rotating group refinement (AFIX 137) with Ueq(H) = 1.5 Ueq(N). Hydrogen atoms on the BINOL-OH groups with O1, O3, and O5 were found and refined with Ueq(H) = 1.5 Ueq(O). Hydrogen atoms on the BINOL-OH groups with O6, O7, and O8 were calculated as an idealized OH-group in a rotating group refinement (AFIX 147) with Ueq(H) = 1.5 Ueq(O). Hydrogen atoms on the ethanol-OH group were calcuated with AFIX 147 and then fixed in the calculated positions (by AFIX 1) to stabilize the model. ; _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^)+(0.0508P)^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 0.31(3) _refine_ls_number_reflns 13383 _refine_ls_number_parameters 918 _refine_ls_number_restraints 4 _refine_ls_R_factor_all 0.1471 _refine_ls_R_factor_gt 0.0594 _refine_ls_wR_factor_ref 0.1335 _refine_ls_wR_factor_gt 0.1082 _refine_ls_goodness_of_fit_ref 0.883 _refine_ls_restrained_S_all 0.883 _refine_ls_shift/su_max 0.004 _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 Ag1 Ag 0.32366(6) 0.35682(6) 0.30503(5) 0.0527(3) Uani 1 1 d . . . Ag2 Ag -0.09418(6) 0.86858(6) 0.03938(4) 0.0528(3) Uani 1 1 d . . . N1 N 0.5374(7) 0.2938(7) 0.2723(4) 0.0440(19) Uani 1 1 d . . . H1A H 0.5928 0.3033 0.3074 0.066 Uiso 1 1 calc R . . H1B H 0.5760 0.3401 0.2264 0.066 Uiso 1 1 calc R . . H1C H 0.5332 0.2117 0.2695 0.066 Uiso 1 1 calc R . . N2 N 0.1033(7) 0.3947(6) 0.3468(4) 0.0445(19) Uani 1 1 d . . . H2A H 0.0536 0.3210 0.3655 0.067 Uiso 1 1 calc R . . H2B H 0.0628 0.4400 0.3082 0.067 Uiso 1 1 calc R . . H2C H 0.1015 0.4388 0.3841 0.067 Uiso 1 1 calc R . . N3 N -0.2901(7) 0.8298(6) -0.0023(4) 0.049(2) Uani 1 1 d . . . H3A H -0.3421 0.9004 -0.0093 0.073 Uiso 1 1 calc R . . H3B H -0.3424 0.7682 0.0321 0.073 Uiso 1 1 calc R . . H3C H -0.2672 0.8046 -0.0471 0.073 Uiso 1 1 calc R . . N4 N 0.0977(7) 0.9297(7) 0.0727(4) 0.047(2) Uani 1 1 d . . . H4A H 0.1720 0.9323 0.0343 0.070 Uiso 1 1 calc R . . H4B H 0.1168 0.8752 0.1145 0.070 Uiso 1 1 calc R . . H4C H 0.0854 1.0073 0.0832 0.070 Uiso 1 1 calc R . . O1 O 0.7529(6) 0.4970(6) 0.1777(3) 0.0389(16) Uani 1 1 d . . . H1D H 0.787(10) 0.520(9) 0.217(5) 0.058 Uiso 1 1 d . . . O2 O 0.4740(5) 0.6512(5) 0.0813(3) 0.0331(13) Uani 1 1 d . . . O3 O 1.2562(7) 0.7299(6) 0.1694(4) 0.0410(18) Uani 1 1 d . . . H3D H 1.315(11) 0.704(10) 0.150(6) 0.061 Uiso 1 1 d . . . O4 O 0.9150(5) 0.5749(5) 0.2664(3) 0.0312(13) Uani 1 1 d . . . O5 O 0.3567(6) 0.8126(5) -0.0149(3) 0.0391(15) Uani 1 1 d D . . H5B H 0.389(10) 0.749(6) 0.014(5) 0.059 Uiso 1 1 d D . . O6 O 0.5638(8) 1.0390(8) -0.1128(5) 0.045(2) Uani 1 1 d . . . H6A H 0.5699 0.9834 -0.1387 0.067 Uiso 1 1 calc R . . O7 O 0.9097(7) 0.1702(7) 0.4667(6) 0.054(2) Uani 1 1 d . . . H7A H 0.9014 0.2335 0.4863 0.081 Uiso 1 1 calc R . . O8 O 0.7431(6) 0.4111(5) 0.3605(3) 0.0393(15) Uani 1 1 d . . . H8B H 0.8152 0.4562 0.3392 0.059 Uiso 1 1 calc R . . O9 O 0.6943(8) -0.1372(7) 0.8089(6) 0.091(3) Uani 1 1 d . . . H9A H 0.6793 -0.2123 0.8105 0.137 Uiso 1 1 d . . . O10 O 0.9917(9) 0.3486(7) 0.5434(5) 0.085(3) Uani 1 1 d . . . H10A H 0.9740 0.4251 0.5399 0.128 Uiso 1 1 d . . . C1 C 0.7308(8) 0.5094(7) 0.0494(4) 0.0256(18) Uani 1 1 d . . . C2 C 0.8086(9) 0.5303(8) 0.1033(5) 0.032(2) Uani 1 1 d . . . C3 C 0.9504(10) 0.5861(8) 0.0820(5) 0.035(3) Uani 1 1 d . . . H3E H 1.0021 0.6030 0.1196 0.042 Uiso 1 1 calc R . . C4 C 1.0103(8) 0.6148(8) 0.0065(5) 0.037(2) Uani 1 1 d . . . H4D H 1.1050 0.6491 -0.0069 0.045 Uiso 1 1 calc R . . C5 C 0.9925(11) 0.6252(10) -0.1286(6) 0.046(3) Uani 1 1 d . . . H5A H 1.0837 0.6662 -0.1429 0.055 Uiso 1 1 calc R . . C6 C 0.9228(11) 0.5982(11) -0.1837(6) 0.057(3) Uani 1 1 d . . . H6B H 0.9669 0.6176 -0.2352 0.069 Uiso 1 1 calc R . . C7 C 0.7843(10) 0.5410(9) -0.1637(5) 0.047(2) Uani 1 1 d . . . H7B H 0.7351 0.5220 -0.2018 0.056 Uiso 1 1 calc R . . C8 C 0.7217(9) 0.5133(8) -0.0890(5) 0.039(2) Uani 1 1 d . . . H8A H 0.6291 0.4748 -0.0761 0.046 Uiso 1 1 calc R . . C9 C 0.7916(8) 0.5406(7) -0.0301(4) 0.0296(19) Uani 1 1 d . . . C10 C 0.9342(11) 0.5946(10) -0.0528(6) 0.032(3) Uani 1 1 d . . . C11 C 0.5788(8) 0.4510(7) 0.0733(4) 0.0250(18) Uani 1 1 d . . . C12 C 0.4622(9) 0.5288(8) 0.0874(5) 0.027(2) Uani 1 1 d . . . C13 C 0.3207(10) 0.4698(9) 0.1081(5) 0.039(3) Uani 1 1 d . . . H13A H 0.2397 0.5198 0.1166 0.047 Uiso 1 1 calc R . . C14 C 0.3018(10) 0.3408(9) 0.1155(5) 0.041(2) Uani 1 1 d . . . H14A H 0.2077 0.3054 0.1292 0.049 Uiso 1 1 calc R . . C15 C 0.4015(12) 0.1295(10) 0.1118(7) 0.042(3) Uani 1 1 d . . . H15A H 0.3089 0.0914 0.1272 0.051 Uiso 1 1 calc R . . C16 C 0.5166(12) 0.0558(9) 0.0983(6) 0.061(3) Uani 1 1 d . . . H16A H 0.5039 -0.0323 0.1047 0.073 Uiso 1 1 calc R . . C17 C 0.6537(11) 0.1125(8) 0.0747(6) 0.057(3) Uani 1 1 d . . . H17A H 0.7334 0.0624 0.0638 0.068 Uiso 1 1 calc R . . C18 C 0.6738(9) 0.2387(7) 0.0672(5) 0.035(2) Uani 1 1 d . . . H18A H 0.7680 0.2737 0.0526 0.042 Uiso 1 1 calc R . . C19 C 0.5588(9) 0.3191(7) 0.0806(4) 0.0257(18) Uani 1 1 d . . . C20 C 0.4172(10) 0.2608(10) 0.1035(5) 0.036(3) Uani 1 1 d . . . C21 C 1.1524(8) 0.7148(7) 0.2972(4) 0.0250(18) Uani 1 1 d . . . C22 C 1.2675(9) 0.6938(8) 0.2450(5) 0.026(2) Uani 1 1 d . . . C23 C 1.3934(10) 0.6383(8) 0.2665(5) 0.034(2) Uani 1 1 d . . . H23A H 1.4688 0.6240 0.2287 0.041 Uiso 1 1 calc R . . C24 C 1.4080(9) 0.6050(8) 0.3405(5) 0.037(2) Uani 1 1 d . . . H24A H 1.4935 0.5673 0.3540 0.044 Uiso 1 1 calc R . . C25 C 1.3077(12) 0.5937(9) 0.4777(6) 0.043(3) Uani 1 1 d . . . H25A H 1.3906 0.5541 0.4935 0.051 Uiso 1 1 calc R . . C26 C 1.2000(12) 0.6197(9) 0.5297(6) 0.054(3) Uani 1 1 d . . . H26A H 1.2092 0.5981 0.5818 0.065 Uiso 1 1 calc R . . C27 C 1.0748(11) 0.6778(9) 0.5091(5) 0.049(3) Uani 1 1 d . . . H27A H 1.0017 0.6973 0.5465 0.058 Uiso 1 1 calc R . . C28 C 1.0602(9) 0.7057(8) 0.4341(5) 0.039(2) Uani 1 1 d . . . H28A H 0.9743 0.7423 0.4204 0.046 Uiso 1 1 calc R . . C29 C 1.1675(8) 0.6821(7) 0.3765(4) 0.0277(19) Uani 1 1 d . . . C30 C 1.2965(11) 0.6261(10) 0.3984(6) 0.033(3) Uani 1 1 d . . . C31 C 1.0184(8) 0.7732(7) 0.2730(4) 0.0257(18) Uani 1 1 d . . . C32 C 0.9059(10) 0.6983(9) 0.2596(5) 0.036(2) Uani 1 1 d . . . C33 C 0.7801(10) 0.7594(8) 0.2391(5) 0.033(2) Uani 1 1 d . . . H33A H 0.7042 0.7108 0.2300 0.040 Uiso 1 1 calc R . . C34 C 0.7654(9) 0.8844(9) 0.2320(5) 0.045(2) Uani 1 1 d . . . H34A H 0.6787 0.9201 0.2190 0.054 Uiso 1 1 calc R . . C35 C 0.8641(12) 1.0948(10) 0.2335(6) 0.041(3) Uani 1 1 d . . . H35A H 0.7806 1.1334 0.2179 0.049 Uiso 1 1 calc R . . C36 C 0.9724(11) 1.1694(9) 0.2460(6) 0.056(3) Uani 1 1 d . . . H36A H 0.9634 1.2576 0.2394 0.067 Uiso 1 1 calc R . . C37 C 1.0958(10) 1.1110(8) 0.2688(5) 0.048(2) Uani 1 1 d . . . H37A H 1.1701 1.1607 0.2784 0.057 Uiso 1 1 calc R . . C38 C 1.1114(9) 0.9856(8) 0.2774(5) 0.039(2) Uani 1 1 d . . . H38A H 1.1967 0.9499 0.2925 0.047 Uiso 1 1 calc R . . C39 C 1.0028(8) 0.9049(7) 0.2643(4) 0.0254(18) Uani 1 1 d . . . C40 C 0.8740(10) 0.9646(9) 0.2432(5) 0.033(2) Uani 1 1 d . . . C41 C 0.3311(8) 0.8919(8) -0.1425(4) 0.0283(19) Uani 1 1 d . . . C42 C 0.3589(8) 0.7928(8) -0.0853(5) 0.0297(19) Uani 1 1 d . . . C43 C 0.3865(9) 0.6718(8) -0.1026(5) 0.037(2) Uani 1 1 d . . . H43A H 0.4054 0.6044 -0.0637 0.044 Uiso 1 1 calc R . . C44 C 0.3864(8) 0.6516(8) -0.1728(5) 0.040(2) Uani 1 1 d . . . H44A H 0.4071 0.5709 -0.1831 0.047 Uiso 1 1 calc R . . C45 C 0.3529(10) 0.7344(9) -0.3075(5) 0.049(3) Uani 1 1 d . . . H45A H 0.3704 0.6538 -0.3186 0.059 Uiso 1 1 calc R . . C46 C 0.3268(14) 0.8294(11) -0.3640(6) 0.076(4) Uani 1 1 d . . . H46A H 0.3238 0.8146 -0.4132 0.091 Uiso 1 1 calc R . . C47 C 0.3042(11) 0.9501(11) -0.3488(6) 0.057(3) Uani 1 1 d . . . H47A H 0.2891 1.0177 -0.3886 0.068 Uiso 1 1 calc R . . C48 C 0.3039(9) 0.9711(9) -0.2770(5) 0.040(2) Uani 1 1 d . . . H48A H 0.2854 1.0527 -0.2677 0.048 Uiso 1 1 calc R . . C49 C 0.3305(9) 0.8738(9) -0.2164(5) 0.033(2) Uani 1 1 d . . . C50 C 0.3552(9) 0.7506(9) -0.2321(5) 0.040(2) Uani 1 1 d . . . C51 C 0.3120(11) 1.0202(9) -0.1234(6) 0.032(2) Uani 1 1 d . . . C52 C 0.4296(12) 1.0870(11) -0.1091(6) 0.038(3) Uani 1 1 d . . . C53 C 0.4089(13) 1.1995(11) -0.0833(6) 0.047(3) Uani 1 1 d . . . H53A H 0.4876 1.2379 -0.0693 0.057 Uiso 1 1 calc R . . C54 C 0.2793(11) 1.2556(8) -0.0778(5) 0.047(2) Uani 1 1 d . . . H54A H 0.2701 1.3334 -0.0620 0.056 Uiso 1 1 calc R . . C55 C 0.0186(12) 1.2548(10) -0.0905(7) 0.063(3) Uani 1 1 d . . . H55A H 0.0066 1.3327 -0.0750 0.076 Uiso 1 1 calc R . . C56 C -0.0944(14) 1.1945(13) -0.1084(7) 0.073(4) Uani 1 1 d . . . H56A H -0.1848 1.2330 -0.1067 0.087 Uiso 1 1 calc R . . C57 C -0.0794(12) 1.0769(12) -0.1292(7) 0.055(3) Uani 1 1 d . . . H57A H -0.1603 1.0384 -0.1410 0.066 Uiso 1 1 calc R . . C58 C 0.0479(9) 1.0162(9) -0.1330(5) 0.043(2) Uani 1 1 d . . . H58A H 0.0542 0.9358 -0.1455 0.051 Uiso 1 1 calc R . . C59 C 0.1761(9) 1.0783(8) -0.1171(5) 0.035(2) Uani 1 1 d . . . C60 C 0.1557(10) 1.1968(9) -0.0957(5) 0.043(2) Uani 1 1 d . . . C61 C 0.6548(10) 0.1952(10) 0.4695(6) 0.031(3) Uani 1 1 d . . . C62 C 0.7775(13) 0.1313(12) 0.4574(7) 0.046(3) Uani 1 1 d . . . C63 C 0.7760(13) 0.0099(10) 0.4360(7) 0.053(3) Uani 1 1 d . . . H63A H 0.8615 -0.0354 0.4296 0.063 Uiso 1 1 calc R . . C64 C 0.6498(11) -0.0376(9) 0.4254(6) 0.059(3) Uani 1 1 d . . . H64A H 0.6497 -0.1144 0.4086 0.071 Uiso 1 1 calc R . . C65 C 0.3836(12) -0.0275(11) 0.4294(6) 0.056(3) Uani 1 1 d . . . H65A H 0.3807 -0.1058 0.4145 0.067 Uiso 1 1 calc R . . C66 C 0.2615(14) 0.0340(12) 0.4416(7) 0.060(4) Uani 1 1 d . . . H66A H 0.1743 -0.0009 0.4345 0.072 Uiso 1 1 calc R . . C67 C 0.2614(12) 0.1497(12) 0.4650(7) 0.053(3) Uani 1 1 d . . . H67A H 0.1736 0.1901 0.4754 0.064 Uiso 1 1 calc R . . C68 C 0.3888(10) 0.2053(9) 0.4730(5) 0.045(2) Uani 1 1 d . . . H68A H 0.3883 0.2849 0.4866 0.054 Uiso 1 1 calc R . . C69 C 0.5209(9) 0.1414(7) 0.4606(4) 0.0305(19) Uani 1 1 d . . . C70 C 0.5193(10) 0.0230(9) 0.4385(5) 0.048(2) Uani 1 1 d . . . C71 C 0.6611(7) 0.3214(7) 0.4908(5) 0.0251(18) Uani 1 1 d . . . C72 C 0.7097(7) 0.4252(7) 0.4330(4) 0.0244(18) Uani 1 1 d . . . C73 C 0.7245(9) 0.5461(7) 0.4517(5) 0.034(2) Uani 1 1 d . . . H73A H 0.7570 0.6163 0.4126 0.041 Uiso 1 1 calc R . . C74 C 0.6929(8) 0.5605(8) 0.5234(5) 0.038(2) Uani 1 1 d . . . H74A H 0.7057 0.6409 0.5343 0.045 Uiso 1 1 calc R . . C75 C 0.6079(10) 0.4739(10) 0.6609(5) 0.055(3) Uani 1 1 d . . . H75A H 0.6213 0.5532 0.6730 0.066 Uiso 1 1 calc R . . C76 C 0.5563(12) 0.3711(12) 0.7181(6) 0.076(4) Uani 1 1 d . . . H76A H 0.5300 0.3812 0.7688 0.091 Uiso 1 1 calc R . . C77 C 0.5436(11) 0.2531(10) 0.7001(6) 0.061(3) Uani 1 1 d . . . H77A H 0.5147 0.1827 0.7397 0.073 Uiso 1 1 calc R . . C78 C 0.5716(10) 0.2370(9) 0.6278(5) 0.048(3) Uani 1 1 d . . . H78A H 0.5555 0.1568 0.6175 0.058 Uiso 1 1 calc R . . C79 C 0.6252(8) 0.3386(8) 0.5661(5) 0.033(2) Uani 1 1 d . . . C80 C 0.6403(9) 0.4586(8) 0.5842(5) 0.037(2) Uani 1 1 d . . . C81 C 0.787(3) -0.0813(17) 0.7281(10) 0.197(11) Uani 1 1 d . . . H81A H 0.7719 0.0101 0.7176 0.236 Uiso 1 1 calc R . . H81B H 0.8886 -0.0926 0.7344 0.236 Uiso 1 1 calc R . . C82 C 0.772(3) -0.122(2) 0.6630(13) 0.228(13) Uani 1 1 d . . . H82A H 0.8349 -0.0717 0.6199 0.342 Uiso 1 1 calc R . . H82B H 0.6721 -0.1122 0.6543 0.342 Uiso 1 1 calc R . . H82C H 0.7965 -0.2101 0.6686 0.342 Uiso 1 1 calc R . . C83 C 1.004(3) 0.294(3) 0.6246(15) 0.227(15) Uani 1 1 d . . . H83A H 0.9021 0.2851 0.6484 0.273 Uiso 1 1 calc R . . H83B H 1.0335 0.2080 0.6220 0.273 Uiso 1 1 calc R . . C84 C 1.055(4) 0.312(3) 0.6704(17) 0.32(2) Uani 1 1 d . . . H84A H 1.0966 0.2342 0.6943 0.477 Uiso 1 1 calc R . . H84B H 0.9838 0.3404 0.7079 0.477 Uiso 1 1 calc R . . H84C H 1.1302 0.3763 0.6506 0.477 Uiso 1 1 calc R . . 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 0.0371(5) 0.0456(6) 0.0757(7) -0.0121(5) -0.0097(5) -0.0055(4) Ag2 0.0367(5) 0.0463(6) 0.0764(7) -0.0111(5) -0.0135(5) -0.0006(4) N1 0.052(5) 0.040(5) 0.040(5) -0.006(4) -0.011(4) -0.006(4) N2 0.034(4) 0.029(4) 0.068(5) -0.004(4) -0.008(4) 0.001(3) N3 0.029(4) 0.036(5) 0.076(6) 0.001(4) -0.010(4) -0.003(3) N4 0.038(5) 0.052(5) 0.050(5) 0.000(4) -0.018(4) -0.004(4) O1 0.038(4) 0.047(4) 0.027(4) 0.001(3) -0.003(3) -0.021(3) O2 0.032(3) 0.022(3) 0.043(4) -0.006(3) -0.003(3) 0.001(2) O3 0.036(4) 0.049(4) 0.037(4) -0.006(3) -0.007(3) 0.013(3) O4 0.031(3) 0.027(3) 0.036(3) -0.005(3) -0.009(3) -0.010(2) O5 0.044(4) 0.032(4) 0.042(4) -0.005(3) -0.014(3) 0.012(3) O6 0.033(5) 0.049(5) 0.053(5) -0.007(4) -0.014(4) -0.004(4) O7 0.025(4) 0.046(5) 0.093(6) -0.020(4) -0.006(4) -0.002(3) O8 0.042(4) 0.038(4) 0.034(4) -0.002(3) 0.000(3) -0.023(3) O9 0.063(5) 0.058(5) 0.146(8) -0.029(5) 0.011(5) -0.004(4) O10 0.085(6) 0.065(6) 0.115(7) -0.025(5) -0.035(6) -0.005(5) C1 0.027(4) 0.024(5) 0.025(5) -0.001(4) -0.004(4) -0.002(3) C2 0.030(5) 0.029(6) 0.031(6) 0.005(4) -0.003(4) -0.001(4) C3 0.024(5) 0.042(6) 0.039(6) -0.008(5) -0.005(4) -0.009(4) C4 0.018(4) 0.049(6) 0.040(6) -0.006(5) 0.009(4) -0.015(4) C5 0.032(6) 0.058(7) 0.041(7) -0.006(5) 0.008(5) -0.004(5) C6 0.051(7) 0.086(9) 0.026(6) 0.000(6) 0.006(5) -0.018(6) C7 0.058(7) 0.055(7) 0.029(6) -0.006(5) -0.011(5) 0.007(5) C8 0.039(5) 0.041(6) 0.037(6) -0.009(4) -0.008(4) -0.002(4) C9 0.036(5) 0.026(5) 0.024(5) -0.002(4) 0.000(4) 0.000(4) C10 0.030(6) 0.036(7) 0.028(6) -0.004(5) -0.001(5) -0.013(5) C11 0.032(5) 0.023(4) 0.023(4) -0.006(4) -0.011(4) 0.005(4) C12 0.028(5) 0.024(5) 0.028(5) -0.003(4) -0.007(4) 0.006(4) C13 0.020(5) 0.042(7) 0.056(7) -0.019(5) 0.002(4) -0.004(4) C14 0.031(5) 0.044(6) 0.044(6) 0.002(5) -0.007(4) -0.017(5) C15 0.036(6) 0.028(6) 0.059(8) 0.001(6) -0.009(5) -0.012(5) C16 0.070(8) 0.035(6) 0.081(8) -0.025(6) -0.006(6) -0.020(6) C17 0.066(7) 0.025(6) 0.080(8) -0.014(5) -0.012(6) 0.013(5) C18 0.037(5) 0.023(5) 0.048(6) -0.007(4) -0.015(4) 0.002(4) C19 0.031(5) 0.023(5) 0.021(5) 0.001(4) -0.006(4) -0.006(4) C20 0.034(6) 0.034(6) 0.036(6) 0.000(4) -0.006(5) -0.016(5) C21 0.019(4) 0.022(4) 0.035(5) -0.008(4) -0.005(4) -0.006(3) C22 0.025(5) 0.028(5) 0.026(5) -0.010(4) -0.001(4) -0.008(4) C23 0.028(5) 0.038(6) 0.039(6) -0.009(5) -0.010(4) 0.003(4) C24 0.036(5) 0.032(5) 0.047(6) -0.004(5) -0.026(5) 0.002(4) C25 0.054(7) 0.039(6) 0.035(6) 0.003(5) -0.021(5) -0.019(5) C26 0.069(8) 0.048(7) 0.040(7) 0.001(5) -0.005(6) -0.024(6) C27 0.055(7) 0.063(7) 0.028(6) -0.011(5) -0.002(5) -0.016(5) C28 0.037(5) 0.045(6) 0.034(6) -0.010(4) -0.004(4) -0.009(4) C29 0.038(5) 0.025(5) 0.025(5) -0.014(4) -0.006(4) -0.013(4) C30 0.040(7) 0.019(6) 0.045(7) -0.010(5) -0.017(5) 0.004(5) C31 0.028(4) 0.023(4) 0.027(5) -0.010(4) 0.000(4) -0.003(3) C32 0.038(6) 0.034(6) 0.035(6) -0.012(5) 0.000(4) -0.018(5) C33 0.027(5) 0.034(6) 0.044(6) -0.011(5) -0.017(4) 0.004(4) C34 0.025(5) 0.043(7) 0.063(7) 0.002(5) -0.014(5) 0.006(5) C35 0.051(7) 0.032(7) 0.044(7) -0.014(5) -0.015(5) 0.015(5) C36 0.074(8) 0.032(6) 0.066(7) -0.015(5) -0.019(6) 0.011(5) C37 0.058(6) 0.019(5) 0.069(7) -0.011(5) -0.015(5) -0.008(4) C38 0.048(6) 0.032(5) 0.040(6) -0.011(4) -0.011(4) -0.001(4) C39 0.023(4) 0.023(5) 0.026(5) -0.001(4) 0.003(4) 0.000(3) C40 0.050(7) 0.025(6) 0.026(5) -0.006(4) -0.006(5) 0.002(5) C41 0.021(4) 0.037(5) 0.026(5) -0.004(4) -0.004(4) -0.001(4) C42 0.029(5) 0.040(5) 0.020(5) -0.008(4) -0.002(4) -0.007(4) C43 0.034(5) 0.029(5) 0.044(6) -0.004(4) 0.001(4) 0.003(4) C44 0.036(5) 0.032(5) 0.053(6) -0.015(5) -0.009(4) 0.004(4) C45 0.064(7) 0.041(6) 0.044(7) -0.013(5) -0.008(5) -0.009(5) C46 0.128(11) 0.059(9) 0.046(7) -0.009(7) -0.033(7) -0.008(7) C47 0.069(7) 0.059(8) 0.038(7) 0.011(6) -0.022(5) -0.018(6) C48 0.056(6) 0.040(6) 0.028(5) -0.007(5) -0.018(5) -0.006(5) C49 0.033(5) 0.038(6) 0.026(5) 0.001(4) -0.009(4) -0.015(4) C50 0.039(5) 0.042(6) 0.039(6) -0.012(5) -0.004(4) -0.007(4) C51 0.033(6) 0.028(6) 0.032(6) 0.000(4) -0.007(4) 0.007(4) C52 0.038(7) 0.033(7) 0.036(7) 0.015(5) -0.013(5) 0.002(5) C53 0.057(7) 0.038(7) 0.049(7) -0.009(5) -0.017(6) -0.013(6) C54 0.071(7) 0.027(5) 0.043(6) -0.002(4) -0.018(5) -0.003(5) C55 0.056(8) 0.038(7) 0.085(9) -0.004(6) 0.013(6) 0.005(6) C56 0.057(9) 0.068(10) 0.082(10) 0.001(8) 0.000(7) 0.027(7) C57 0.039(7) 0.058(9) 0.057(8) 0.008(6) 0.001(6) 0.001(6) C58 0.027(5) 0.035(6) 0.058(7) 0.005(5) -0.002(5) -0.007(4) C59 0.035(5) 0.030(5) 0.032(5) 0.005(4) 0.003(4) 0.000(4) C60 0.042(6) 0.048(6) 0.030(5) 0.006(4) -0.001(4) 0.006(5) C61 0.024(6) 0.023(6) 0.050(7) -0.010(5) -0.010(5) -0.006(4) C62 0.043(7) 0.049(8) 0.050(8) -0.020(6) -0.008(6) 0.002(6) C63 0.059(8) 0.022(6) 0.075(9) -0.009(6) -0.009(6) 0.010(5) C64 0.064(8) 0.047(7) 0.063(7) -0.008(5) 0.000(6) -0.018(6) C65 0.061(8) 0.055(7) 0.045(7) 0.011(6) -0.014(6) -0.034(6) C66 0.063(9) 0.068(10) 0.047(7) 0.000(6) -0.021(6) -0.027(7) C67 0.045(8) 0.052(8) 0.059(8) 0.004(6) -0.017(6) -0.010(6) C68 0.033(6) 0.050(6) 0.044(6) 0.006(5) -0.003(4) -0.017(5) C69 0.037(5) 0.025(5) 0.029(5) 0.001(4) -0.012(4) -0.008(4) C70 0.048(6) 0.054(7) 0.039(6) -0.004(5) -0.008(5) -0.013(5) C71 0.020(4) 0.022(4) 0.034(5) -0.003(4) -0.008(4) 0.004(3) C72 0.019(4) 0.033(5) 0.023(5) -0.006(4) -0.006(3) -0.002(3) C73 0.041(5) 0.023(5) 0.037(6) 0.001(4) -0.011(4) -0.008(4) C74 0.032(5) 0.034(5) 0.049(6) -0.009(5) -0.012(4) -0.013(4) C75 0.062(7) 0.062(7) 0.045(7) -0.026(6) 0.000(5) -0.018(5) C76 0.104(10) 0.098(10) 0.022(6) -0.028(6) 0.026(6) -0.044(7) C77 0.080(8) 0.059(8) 0.044(7) -0.012(6) -0.008(6) -0.027(6) C78 0.062(7) 0.046(6) 0.033(6) 0.001(5) -0.004(5) -0.023(5) C79 0.024(5) 0.042(6) 0.031(5) -0.007(4) 0.000(4) -0.006(4) C80 0.046(5) 0.038(6) 0.033(5) -0.015(4) -0.012(4) -0.009(4) C81 0.40(4) 0.092(14) 0.093(14) -0.001(12) -0.038(19) -0.017(17) C82 0.37(4) 0.19(2) 0.17(2) -0.09(2) -0.10(2) 0.09(2) C83 0.30(3) 0.21(3) 0.21(3) -0.01(2) -0.19(3) -0.02(2) C84 0.49(6) 0.25(3) 0.20(3) 0.08(3) -0.19(3) -0.19(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ag1 N1 2.146(7) . ? Ag1 N2 2.153(6) . ? Ag2 N4 2.132(6) . ? Ag2 N3 2.164(6) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N1 H1C 0.9000 . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N2 H2C 0.9000 . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N3 H3C 0.9000 . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? N4 H4C 0.9000 . ? O1 C2 1.342(10) . ? O1 H1D 0.90(9) . ? O2 C12 1.307(9) . ? O3 C22 1.363(10) . ? O3 H3D 0.70(10) . ? O4 C32 1.317(10) . ? O5 C42 1.330(9) . ? O5 H5B 0.86(5) . ? O6 C52 1.355(12) . ? O6 H6A 0.8300 . ? O7 C62 1.358(12) . ? O7 H7A 0.8300 . ? O8 C72 1.338(8) . ? O8 H8B 0.8300 . ? O9 C81 1.58(2) . ? O9 H9A 0.8181 . ? O10 C83 1.49(2) . ? O10 H10A 0.8339 . ? C1 C2 1.357(11) . ? C1 C9 1.434(10) . ? C1 C11 1.524(10) . ? C2 C3 1.427(11) . ? C3 C4 1.365(11) . ? C3 H3E 0.9400 . ? C4 C10 1.428(12) . ? C4 H4D 0.9400 . ? C5 C6 1.350(13) . ? C5 C10 1.369(13) . ? C5 H5A 0.9400 . ? C6 C7 1.404(13) . ? C6 H6B 0.9400 . ? C7 C8 1.360(11) . ? C7 H7B 0.9400 . ? C8 C9 1.413(10) . ? C8 H8A 0.9400 . ? C9 C10 1.427(12) . ? C11 C12 1.398(11) . ? C11 C19 1.413(10) . ? C12 C13 1.437(11) . ? C13 C14 1.381(12) . ? C13 H13A 0.9400 . ? C14 C20 1.398(13) . ? C14 H14A 0.9400 . ? C15 C16 1.358(14) . ? C15 C20 1.401(14) . ? C15 H15A 0.9400 . ? C16 C17 1.394(13) . ? C16 H16A 0.9400 . ? C17 C18 1.353(11) . ? C17 H17A 0.9400 . ? C18 C19 1.402(11) . ? C18 H18A 0.9400 . ? C19 C20 1.437(11) . ? C21 C22 1.369(11) . ? C21 C29 1.433(10) . ? C21 C31 1.487(10) . ? C22 C23 1.393(11) . ? C23 C24 1.340(11) . ? C23 H23A 0.9400 . ? C24 C30 1.413(13) . ? C24 H24A 0.9400 . ? C25 C26 1.338(14) . ? C25 C30 1.426(14) . ? C25 H25A 0.9400 . ? C26 C27 1.393(13) . ? C26 H26A 0.9400 . ? C27 C28 1.355(11) . ? C27 H27A 0.9400 . ? C28 C29 1.394(11) . ? C28 H28A 0.9400 . ? C29 C30 1.423(12) . ? C31 C39 1.407(10) . ? C31 C32 1.412(11) . ? C32 C33 1.410(12) . ? C33 C34 1.337(12) . ? C33 H33A 0.9400 . ? C34 C40 1.405(12) . ? C34 H34A 0.9400 . ? C35 C36 1.372(14) . ? C35 C40 1.385(14) . ? C35 H35A 0.9400 . ? C36 C37 1.392(12) . ? C36 H36A 0.9400 . ? C37 C38 1.340(11) . ? C37 H37A 0.9400 . ? C38 C39 1.422(11) . ? C38 H38A 0.9400 . ? C39 C40 1.433(12) . ? C41 C42 1.382(10) . ? C41 C49 1.391(11) . ? C41 C51 1.497(13) . ? C42 C43 1.417(11) . ? C43 C44 1.332(11) . ? C43 H43A 0.9400 . ? C44 C50 1.414(11) . ? C44 H44A 0.9400 . ? C45 C46 1.341(13) . ? C45 C50 1.412(11) . ? C45 H45A 0.9400 . ? C46 C47 1.394(15) . ? C46 H46A 0.9400 . ? C47 C48 1.363(14) . ? C47 H47A 0.9400 . ? C48 C49 1.405(12) . ? C48 H48A 0.9400 . ? C49 C50 1.426(12) . ? C51 C52 1.406(14) . ? C51 C59 1.415(12) . ? C52 C53 1.389(16) . ? C53 C54 1.354(14) . ? C53 H53A 0.9400 . ? C54 C60 1.435(12) . ? C54 H54A 0.9400 . ? C55 C56 1.361(16) . ? C55 C60 1.424(13) . ? C55 H55A 0.9400 . ? C56 C57 1.397(17) . ? C56 H56A 0.9400 . ? C57 C58 1.357(13) . ? C57 H57A 0.9400 . ? C58 C59 1.474(11) . ? C58 H58A 0.9400 . ? C59 C60 1.414(12) . ? C61 C62 1.349(15) . ? C61 C69 1.431(12) . ? C61 C71 1.493(12) . ? C62 C63 1.440(16) . ? C63 C64 1.348(14) . ? C63 H63A 0.9400 . ? C64 C70 1.394(13) . ? C64 H64A 0.9400 . ? C65 C66 1.330(15) . ? C65 C70 1.433(12) . ? C65 H65A 0.9400 . ? C66 C67 1.399(16) . ? C66 H66A 0.9400 . ? C67 C68 1.380(12) . ? C67 H67A 0.9400 . ? C68 C69 1.423(12) . ? C68 H68A 0.9400 . ? C69 C70 1.416(12) . ? C71 C72 1.391(10) . ? C71 C79 1.400(11) . ? C72 C73 1.426(10) . ? C73 C74 1.325(11) . ? C73 H73A 0.9400 . ? C74 C80 1.416(11) . ? C74 H74A 0.9400 . ? C75 C76 1.384(14) . ? C75 C80 1.417(11) . ? C75 H75A 0.9400 . ? C76 C77 1.388(14) . ? C76 H76A 0.9400 . ? C77 C78 1.339(12) . ? C77 H77A 0.9400 . ? C78 C79 1.427(11) . ? C78 H78A 0.9400 . ? C79 C80 1.412(11) . ? C81 C82 1.36(2) . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C82 H82A 0.9700 . ? C82 H82B 0.9700 . ? C82 H82C 0.9700 . ? C83 C84 1.06(2) . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C84 H84A 0.9700 . ? C84 H84B 0.9700 . ? C84 H84C 0.9700 . ? 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 N2 172.3(3) . . ? N4 Ag2 N3 173.0(3) . . ? Ag1 N1 H1A 109.5 . . ? Ag1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? Ag1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? Ag1 N2 H2A 109.5 . . ? Ag1 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? Ag1 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? Ag2 N3 H3A 109.5 . . ? Ag2 N3 H3B 109.5 . . ? H3A N3 H3B 109.5 . . ? Ag2 N3 H3C 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? Ag2 N4 H4A 109.5 . . ? Ag2 N4 H4B 109.5 . . ? H4A N4 H4B 109.5 . . ? Ag2 N4 H4C 109.5 . . ? H4A N4 H4C 109.5 . . ? H4B N4 H4C 109.5 . . ? C2 O1 H1D 127(6) . . ? C22 O3 H3D 105(9) . . ? C42 O5 H5B 111(6) . . ? C52 O6 H6A 109.5 . . ? C62 O7 H7A 109.5 . . ? C72 O8 H8B 109.5 . . ? C81 O9 H9A 106.9 . . ? C83 O10 H10A 107.8 . . ? C2 C1 C9 120.2(7) . . ? C2 C1 C11 120.1(7) . . ? C9 C1 C11 119.7(7) . . ? O1 C2 C1 120.0(8) . . ? O1 C2 C3 119.1(8) . . ? C1 C2 C3 120.9(8) . . ? C4 C3 C2 119.4(8) . . ? C4 C3 H3E 120.3 . . ? C2 C3 H3E 120.3 . . ? C3 C4 C10 122.3(8) . . ? C3 C4 H4D 118.9 . . ? C10 C4 H4D 118.9 . . ? C6 C5 C10 121.9(10) . . ? C6 C5 H5A 119.0 . . ? C10 C5 H5A 119.0 . . ? C5 C6 C7 119.8(9) . . ? C5 C6 H6B 120.1 . . ? C7 C6 H6B 120.1 . . ? C8 C7 C6 119.5(9) . . ? C8 C7 H7B 120.2 . . ? C6 C7 H7B 120.2 . . ? C7 C8 C9 122.1(8) . . ? C7 C8 H8A 119.0 . . ? C9 C8 H8A 119.0 . . ? C8 C9 C10 116.4(7) . . ? C8 C9 C1 123.5(7) . . ? C10 C9 C1 119.9(8) . . ? C5 C10 C9 120.1(9) . . ? C5 C10 C4 122.7(9) . . ? C9 C10 C4 117.2(8) . . ? C12 C11 C19 121.4(7) . . ? C12 C11 C1 119.4(7) . . ? C19 C11 C1 119.2(7) . . ? O2 C12 C11 124.2(7) . . ? O2 C12 C13 118.5(7) . . ? C11 C12 C13 117.3(8) . . ? C14 C13 C12 121.0(9) . . ? C14 C13 H13A 119.5 . . ? C12 C13 H13A 119.5 . . ? C13 C14 C20 122.6(8) . . ? C13 C14 H14A 118.7 . . ? C20 C14 H14A 118.7 . . ? C16 C15 C20 121.8(10) . . ? C16 C15 H15A 119.1 . . ? C20 C15 H15A 119.1 . . ? C15 C16 C17 119.1(9) . . ? C15 C16 H16A 120.5 . . ? C17 C16 H16A 120.5 . . ? C18 C17 C16 121.0(9) . . ? C18 C17 H17A 119.5 . . ? C16 C17 H17A 119.5 . . ? C17 C18 C19 122.2(8) . . ? C17 C18 H18A 118.9 . . ? C19 C18 H18A 118.9 . . ? C18 C19 C11 122.6(7) . . ? C18 C19 C20 116.7(8) . . ? C11 C19 C20 120.7(8) . . ? C14 C20 C15 123.8(9) . . ? C14 C20 C19 116.9(9) . . ? C15 C20 C19 119.2(9) . . ? C22 C21 C29 117.3(7) . . ? C22 C21 C31 121.7(7) . . ? C29 C21 C31 121.0(7) . . ? O3 C22 C21 117.6(8) . . ? O3 C22 C23 119.8(8) . . ? C21 C22 C23 122.6(8) . . ? C24 C23 C22 120.7(9) . . ? C24 C23 H23A 119.7 . . ? C22 C23 H23A 119.7 . . ? C23 C24 C30 120.8(8) . . ? C23 C24 H24A 119.6 . . ? C30 C24 H24A 119.6 . . ? C26 C25 C30 119.9(11) . . ? C26 C25 H25A 120.0 . . ? C30 C25 H25A 120.0 . . ? C25 C26 C27 122.1(10) . . ? C25 C26 H26A 118.9 . . ? C27 C26 H26A 118.9 . . ? C28 C27 C26 118.8(9) . . ? C28 C27 H27A 120.6 . . ? C26 C27 H27A 120.6 . . ? C27 C28 C29 122.6(9) . . ? C27 C28 H28A 118.7 . . ? C29 C28 H28A 118.7 . . ? C28 C29 C30 117.8(8) . . ? C28 C29 C21 122.1(8) . . ? C30 C29 C21 120.0(8) . . ? C24 C30 C29 118.5(9) . . ? C24 C30 C25 122.8(9) . . ? C29 C30 C25 118.7(10) . . ? C39 C31 C32 119.5(7) . . ? C39 C31 C21 119.5(6) . . ? C32 C31 C21 121.0(7) . . ? O4 C32 C33 119.8(8) . . ? O4 C32 C31 122.1(8) . . ? C33 C32 C31 118.0(9) . . ? C34 C33 C32 122.0(9) . . ? C34 C33 H33A 119.0 . . ? C32 C33 H33A 119.0 . . ? C33 C34 C40 122.9(8) . . ? C33 C34 H34A 118.6 . . ? C40 C34 H34A 118.6 . . ? C36 C35 C40 122.2(10) . . ? C36 C35 H35A 118.9 . . ? C40 C35 H35A 118.9 . . ? C35 C36 C37 118.3(9) . . ? C35 C36 H36A 120.9 . . ? C37 C36 H36A 120.9 . . ? C38 C37 C36 121.7(9) . . ? C38 C37 H37A 119.2 . . ? C36 C37 H37A 119.2 . . ? C37 C38 C39 122.0(8) . . ? C37 C38 H38A 119.0 . . ? C39 C38 H38A 119.0 . . ? C31 C39 C38 122.4(7) . . ? C31 C39 C40 121.3(7) . . ? C38 C39 C40 116.2(7) . . ? C35 C40 C34 124.2(10) . . ? C35 C40 C39 119.6(9) . . ? C34 C40 C39 116.2(8) . . ? C42 C41 C49 120.6(8) . . ? C42 C41 C51 117.8(8) . . ? C49 C41 C51 121.4(8) . . ? O5 C42 C41 119.2(7) . . ? O5 C42 C43 121.5(8) . . ? C41 C42 C43 119.3(8) . . ? C44 C43 C42 121.4(8) . . ? C44 C43 H43A 119.3 . . ? C42 C43 H43A 119.3 . . ? C43 C44 C50 120.5(8) . . ? C43 C44 H44A 119.8 . . ? C50 C44 H44A 119.8 . . ? C46 C45 C50 122.7(9) . . ? C46 C45 H45A 118.6 . . ? C50 C45 H45A 118.6 . . ? C45 C46 C47 119.3(10) . . ? C45 C46 H46A 120.4 . . ? C47 C46 H46A 120.4 . . ? C48 C47 C46 120.6(10) . . ? C48 C47 H47A 119.7 . . ? C46 C47 H47A 119.7 . . ? C47 C48 C49 121.6(9) . . ? C47 C48 H48A 119.2 . . ? C49 C48 H48A 119.2 . . ? C41 C49 C48 123.1(9) . . ? C41 C49 C50 119.1(8) . . ? C48 C49 C50 117.7(8) . . ? C45 C50 C44 122.9(9) . . ? C45 C50 C49 118.0(8) . . ? C44 C50 C49 119.0(8) . . ? C52 C51 C59 117.1(10) . . ? C52 C51 C41 120.7(9) . . ? C59 C51 C41 122.2(9) . . ? O6 C52 C53 117.5(11) . . ? O6 C52 C51 121.6(11) . . ? C53 C52 C51 120.6(11) . . ? C54 C53 C52 122.1(11) . . ? C54 C53 H53A 118.9 . . ? C52 C53 H53A 118.9 . . ? C53 C54 C60 120.3(9) . . ? C53 C54 H54A 119.8 . . ? C60 C54 H54A 119.8 . . ? C56 C55 C60 118.3(11) . . ? C56 C55 H55A 120.8 . . ? C60 C55 H55A 120.8 . . ? C55 C56 C57 121.6(12) . . ? C55 C56 H56A 119.2 . . ? C57 C56 H56A 119.2 . . ? C58 C57 C56 122.3(12) . . ? C58 C57 H57A 118.8 . . ? C56 C57 H57A 118.8 . . ? C57 C58 C59 119.0(10) . . ? C57 C58 H58A 120.5 . . ? C59 C58 H58A 120.5 . . ? C60 C59 C51 122.6(8) . . ? C60 C59 C58 116.8(8) . . ? C51 C59 C58 120.6(9) . . ? C59 C60 C55 122.0(9) . . ? C59 C60 C54 116.9(8) . . ? C55 C60 C54 121.1(10) . . ? C62 C61 C69 119.2(10) . . ? C62 C61 C71 119.6(9) . . ? C69 C61 C71 121.1(8) . . ? C61 C62 O7 124.7(11) . . ? C61 C62 C63 121.3(11) . . ? O7 C62 C63 114.0(11) . . ? C64 C63 C62 118.8(11) . . ? C64 C63 H63A 120.6 . . ? C62 C63 H63A 120.6 . . ? C63 C64 C70 122.5(10) . . ? C63 C64 H64A 118.8 . . ? C70 C64 H64A 118.8 . . ? C66 C65 C70 121.4(12) . . ? C66 C65 H65A 119.3 . . ? C70 C65 H65A 119.3 . . ? C65 C66 C67 120.9(11) . . ? C65 C66 H66A 119.6 . . ? C67 C66 H66A 119.6 . . ? C68 C67 C66 120.7(12) . . ? C68 C67 H67A 119.7 . . ? C66 C67 H67A 119.7 . . ? C67 C68 C69 119.6(10) . . ? C67 C68 H68A 120.2 . . ? C69 C68 H68A 120.2 . . ? C70 C69 C68 119.2(8) . . ? C70 C69 C61 119.6(9) . . ? C68 C69 C61 121.2(8) . . ? C64 C70 C69 118.5(8) . . ? C64 C70 C65 123.3(10) . . ? C69 C70 C65 118.2(10) . . ? C72 C71 C79 119.0(7) . . ? C72 C71 C61 117.9(8) . . ? C79 C71 C61 123.1(8) . . ? O8 C72 C71 120.0(7) . . ? O8 C72 C73 120.4(7) . . ? C71 C72 C73 119.6(7) . . ? C74 C73 C72 120.7(8) . . ? C74 C73 H73A 119.6 . . ? C72 C73 H73A 119.6 . . ? C73 C74 C80 122.0(8) . . ? C73 C74 H74A 119.0 . . ? C80 C74 H74A 119.0 . . ? C76 C75 C80 119.6(9) . . ? C76 C75 H75A 120.2 . . ? C80 C75 H75A 120.2 . . ? C75 C76 C77 119.6(9) . . ? C75 C76 H76A 120.2 . . ? C77 C76 H76A 120.2 . . ? C78 C77 C76 121.7(10) . . ? C78 C77 H77A 119.2 . . ? C76 C77 H77A 119.2 . . ? C77 C78 C79 121.6(9) . . ? C77 C78 H78A 119.2 . . ? C79 C78 H78A 119.2 . . ? C71 C79 C80 121.1(7) . . ? C71 C79 C78 122.0(8) . . ? C80 C79 C78 116.9(8) . . ? C79 C80 C74 117.5(8) . . ? C79 C80 C75 120.5(8) . . ? C74 C80 C75 121.9(8) . . ? C82 C81 O9 123(2) . . ? C82 C81 H81A 106.5 . . ? O9 C81 H81A 106.5 . . ? C82 C81 H81B 106.5 . . ? O9 C81 H81B 106.5 . . ? H81A C81 H81B 106.5 . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C84 C83 O10 141(3) . . ? C84 C83 H83A 101.7 . . ? O10 C83 H83A 101.7 . . ? C84 C83 H83B 101.7 . . ? O10 C83 H83B 101.7 . . ? H83A C83 H83B 104.7 . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? 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 N1 H1A O8 0.90 2.27 3.109(9) 154.7 . N1 H1B O1 0.90 2.32 3.045(9) 137.8 . N2 H2A O7 0.90 2.42 3.250(11) 153.0 1_455 N2 H2B O4 0.90 2.11 2.934(8) 151.4 1_455 N3 H3A O6 0.90 2.42 3.151(11) 138.3 1_455 N3 H3B O2 0.90 2.11 2.954(8) 156.0 1_455 N4 H4A O5 0.90 2.33 3.096(9) 143.1 . N4 H4B O3 0.90 2.21 3.023(9) 149.8 1_455 O1 H1D O4 0.90(9) 1.77(9) 2.626(7) 157(9) . O3 H3D O2 0.70(10) 1.95(10) 2.636(7) 170(12) 1_655 O5 H5B O2 0.86(5) 1.73(5) 2.568(7) 165(9) . O6 H6A O9 0.83 2.02 2.766(11) 148.6 1_564 O7 H7A O10 0.83 2.03 2.767(11) 147.3 . O8 H8B O4 0.83 1.79 2.564(7) 155.2 . _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 26.90 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.817 _refine_diff_density_min -0.952 _refine_diff_density_rms 0.097 data_barbjm _database_code_depnum_ccdc_archive 'CCDC 264204' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Diammine-silver(I)((S)-1,1'-bi-2-naphtholate(-))((S)-1,1'-bi-2-naphthol)- ethanol ; _chemical_name_common ; Diammine-silver(i)((S)-1,1'-bi-2-naphtholate(-))((S)-1,1'-bi- 2-naphthol)-ethanol ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H39 Ag N2 O5' _chemical_formula_weight 759.62 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 triclinic _symmetry_space_group_name_H-M P1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' _cell_length_a 9.3931(16) _cell_length_b 10.8023(18) _cell_length_c 18.105(3) _cell_angle_alpha 78.274(3) _cell_angle_beta 81.002(3) _cell_angle_gamma 89.577(3) _cell_volume 1776.0(5) _cell_formula_units_Z 2 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description isometric _exptl_crystal_colour colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.420 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 0.616 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.9242 _exptl_absorpt_correction_T_max 0.9758 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(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 'Bruker AXS CCD diffractometer' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15491 _diffrn_reflns_av_R_equivalents 0.0252 _diffrn_reflns_av_sigmaI/netI 0.1096 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.16 _diffrn_reflns_theta_max 27.10 _reflns_number_total 13739 _reflns_number_gt 7694 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _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. Hydrogen atoms on the aromatic rings and ethanol molecules were placed at calculated positions with an appropriate riding model (AFIX 43 for CH, AFIX 23 for CH2, and AFIX 33 for CH3) and an isotropic temperature factor of Ueq(H) = 1.2 Ueq(CH, CH2) and 1.5 Ueg(CH3). The hydrogen atoms of the ammin ligands were calculated as an idealized NH3 group with tetrahedral angles in a rotating group refinement (AFIX 137) with Ueq(H) = 1.5 Ueq(N). Hydrogen atoms on the BINOL-OH groups with O1, O3, O5, and O8 were found and refined with Ueq(H) = 1.5 Ueq(O). Hydrogen atoms on the BINOL-OH groups with O6 and O7 were calculated as an idealized OH-group in a rotating group refinement (AFIX 147) with Ueq(H) = 1.5 Ueq(O). Hydrogen atoms on the ethanol-OH group were calcuated with AFIX 147 and then fixed in the calculated positions (by AFIX 1) to stabilize the model. ; _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^)+(0.0158P)^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 0.040(18) _refine_ls_number_reflns 13739 _refine_ls_number_parameters 919 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1041 _refine_ls_R_factor_gt 0.0498 _refine_ls_wR_factor_ref 0.0794 _refine_ls_wR_factor_gt 0.0667 _refine_ls_goodness_of_fit_ref 0.924 _refine_ls_restrained_S_all 0.924 _refine_ls_shift/su_max 0.003 _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 Ag1 Ag 0.32319(4) 0.35693(4) 0.30509(3) 0.05297(18) Uani 1 1 d . . . Ag2 Ag -0.09372(4) 0.86851(4) 0.03923(3) 0.05317(18) Uani 1 1 d . . . N1 N 0.5366(4) 0.2957(4) 0.2722(3) 0.0477(14) Uani 1 1 d . . . H1A H 0.5943 0.3141 0.3040 0.072 Uiso 1 1 calc R . . H1B H 0.5707 0.3355 0.2241 0.072 Uiso 1 1 calc R . . H1C H 0.5346 0.2116 0.2748 0.072 Uiso 1 1 calc R . . N2 N 0.1048(4) 0.3925(4) 0.3468(3) 0.0460(14) Uani 1 1 d . . . H2A H 0.0527 0.3196 0.3584 0.069 Uiso 1 1 calc R . . H2B H 0.0682 0.4476 0.3106 0.069 Uiso 1 1 calc R . . H2C H 0.1012 0.4254 0.3889 0.069 Uiso 1 1 calc R . . N3 N -0.2889(4) 0.8313(4) -0.0016(3) 0.0450(14) Uani 1 1 d . . . H3A H -0.3383 0.9031 -0.0104 0.068 Uiso 1 1 calc R . . H3B H -0.3432 0.7726 0.0338 0.068 Uiso 1 1 calc R . . H3C H -0.2668 0.8026 -0.0452 0.068 Uiso 1 1 calc R . . N4 N 0.0970(5) 0.9297(4) 0.0726(3) 0.0504(14) Uani 1 1 d . . . H4A H 0.1695 0.9395 0.0328 0.076 Uiso 1 1 calc R . . H4B H 0.1207 0.8714 0.1116 0.076 Uiso 1 1 calc R . . H4C H 0.0816 1.0038 0.0875 0.076 Uiso 1 1 calc R . . O1 O 0.7524(4) 0.4968(4) 0.1782(2) 0.0383(11) Uani 1 1 d . . . H1D H 0.811(6) 0.526(6) 0.205(3) 0.057 Uiso 1 1 d . . . O2 O 0.4750(3) 0.6512(3) 0.0809(2) 0.0314(9) Uani 1 1 d . . . O3 O 1.2562(4) 0.7288(4) 0.1690(2) 0.0397(12) Uani 1 1 d . . . H3D H 1.316(7) 0.707(6) 0.142(4) 0.060 Uiso 1 1 d . . . O4 O 0.9149(3) 0.5732(3) 0.26693(19) 0.0315(9) Uani 1 1 d . . . O5 O 0.3573(4) 0.8126(4) -0.0140(2) 0.0383(10) Uani 1 1 d D . . H5B H 0.395(6) 0.751(5) 0.014(4) 0.057 Uiso 1 1 d D . . O6 O 0.5630(5) 1.0401(5) -0.1130(3) 0.0414(14) Uani 1 1 d . . . H6A H 0.5660 0.9758 -0.1317 0.062 Uiso 1 1 calc R . . O7 O 0.9091(5) 0.1711(5) 0.4674(4) 0.0567(16) Uani 1 1 d . . . H7A H 0.9002 0.2383 0.4831 0.085 Uiso 1 1 calc R . . O8 O 0.7415(4) 0.4107(4) 0.3613(2) 0.0415(11) Uani 1 1 d D . . H8B H 0.799(6) 0.464(6) 0.335(4) 0.062 Uiso 1 1 d D . . O9 O 0.6938(6) -0.1361(5) 0.8073(4) 0.0880(18) Uani 1 1 d . . . H9A H 0.6793 -0.2123 0.8105 0.132 Uiso 1 1 d . . . O10 O 0.9928(6) 0.3492(5) 0.5433(4) 0.0905(18) Uani 1 1 d . . . H10A H 0.9740 0.4251 0.5399 0.136 Uiso 1 1 d . . . C1 C 0.7296(5) 0.5084(4) 0.0493(3) 0.0252(13) Uani 1 1 d . . . C2 C 0.8097(6) 0.5307(5) 0.1036(3) 0.0276(15) Uani 1 1 d . . . C3 C 0.9487(6) 0.5847(6) 0.0814(4) 0.0346(17) Uani 1 1 d . . . H3E H 1.0010 0.5998 0.1191 0.041 Uiso 1 1 calc R . . C4 C 1.0102(6) 0.6161(5) 0.0062(4) 0.0373(15) Uani 1 1 d . . . H4D H 1.1036 0.6526 -0.0070 0.045 Uiso 1 1 calc R . . C5 C 0.9940(7) 0.6242(7) -0.1295(4) 0.046(2) Uani 1 1 d . . . H5A H 1.0860 0.6632 -0.1442 0.055 Uiso 1 1 calc R . . C6 C 0.9217(8) 0.5980(7) -0.1835(4) 0.055(2) Uani 1 1 d . . . H6B H 0.9648 0.6174 -0.2350 0.066 Uiso 1 1 calc R . . C7 C 0.7837(7) 0.5423(6) -0.1636(4) 0.0488(17) Uani 1 1 d . . . H7B H 0.7341 0.5246 -0.2017 0.059 Uiso 1 1 calc R . . C8 C 0.7201(6) 0.5132(5) -0.0877(3) 0.0360(14) Uani 1 1 d . . . H8A H 0.6270 0.4762 -0.0745 0.043 Uiso 1 1 calc R . . C9 C 0.7935(5) 0.5384(5) -0.0297(3) 0.0285(13) Uani 1 1 d . . . C10 C 0.9346(7) 0.5943(7) -0.0521(4) 0.0313(18) Uani 1 1 d . . . C11 C 0.5793(5) 0.4515(5) 0.0733(3) 0.0255(12) Uani 1 1 d . . . C12 C 0.4636(6) 0.5274(5) 0.0875(3) 0.0265(15) Uani 1 1 d . . . C13 C 0.3228(7) 0.4685(6) 0.1078(3) 0.0350(17) Uani 1 1 d . . . H13A H 0.2425 0.5193 0.1159 0.042 Uiso 1 1 calc R . . C14 C 0.3009(6) 0.3408(6) 0.1160(3) 0.0398(16) Uani 1 1 d . . . H14A H 0.2069 0.3057 0.1300 0.048 Uiso 1 1 calc R . . C15 C 0.4013(8) 0.1284(7) 0.1119(4) 0.044(2) Uani 1 1 d . . . H15A H 0.3088 0.0903 0.1269 0.053 Uiso 1 1 calc R . . C16 C 0.5162(8) 0.0563(6) 0.0986(4) 0.057(2) Uani 1 1 d . . . H16A H 0.5039 -0.0317 0.1048 0.068 Uiso 1 1 calc R . . C17 C 0.6532(7) 0.1122(6) 0.0757(4) 0.0518(18) Uani 1 1 d . . . H17A H 0.7324 0.0608 0.0663 0.062 Uiso 1 1 calc R . . C18 C 0.6759(6) 0.2388(5) 0.0665(3) 0.0390(15) Uani 1 1 d . . . H18A H 0.7697 0.2737 0.0505 0.047 Uiso 1 1 calc R . . C19 C 0.5598(6) 0.3183(5) 0.0809(3) 0.0267(13) Uani 1 1 d . . . C20 C 0.4184(7) 0.2619(6) 0.1035(4) 0.0324(16) Uani 1 1 d . . . C21 C 1.1531(5) 0.7137(4) 0.2974(3) 0.0241(12) Uani 1 1 d . . . C22 C 1.2661(7) 0.6930(5) 0.2446(4) 0.0292(16) Uani 1 1 d . . . C23 C 1.3929(6) 0.6388(6) 0.2671(4) 0.0361(17) Uani 1 1 d . . . H23A H 1.4694 0.6249 0.2298 0.043 Uiso 1 1 calc R . . C24 C 1.4066(6) 0.6061(5) 0.3425(4) 0.0382(15) Uani 1 1 d . . . H24A H 1.4917 0.5690 0.3567 0.046 Uiso 1 1 calc R . . C25 C 1.3048(8) 0.5934(7) 0.4778(4) 0.046(2) Uani 1 1 d . . . H25A H 1.3869 0.5522 0.4933 0.056 Uiso 1 1 calc R . . C26 C 1.1978(8) 0.6193(7) 0.5313(4) 0.055(2) Uani 1 1 d . . . H26A H 1.2073 0.5989 0.5832 0.066 Uiso 1 1 calc R . . C27 C 1.0739(7) 0.6763(6) 0.5092(4) 0.0513(18) Uani 1 1 d . . . H27A H 0.9998 0.6941 0.5465 0.062 Uiso 1 1 calc R . . C28 C 1.0583(6) 0.7064(5) 0.4347(3) 0.0371(15) Uani 1 1 d . . . H28A H 0.9728 0.7442 0.4215 0.044 Uiso 1 1 calc R . . C29 C 1.1673(6) 0.6828(5) 0.3758(3) 0.0287(13) Uani 1 1 d . . . C30 C 1.2957(8) 0.6273(7) 0.3982(4) 0.0355(19) Uani 1 1 d . . . C31 C 1.0186(5) 0.7726(5) 0.2726(3) 0.0260(12) Uani 1 1 d . . . C32 C 0.9085(6) 0.6983(6) 0.2603(4) 0.0317(16) Uani 1 1 d . . . C33 C 0.7819(7) 0.7591(6) 0.2385(4) 0.0398(18) Uani 1 1 d . . . H33A H 0.7077 0.7098 0.2286 0.048 Uiso 1 1 calc R . . C34 C 0.7646(6) 0.8850(6) 0.2313(4) 0.0453(17) Uani 1 1 d . . . H34A H 0.6780 0.9208 0.2185 0.054 Uiso 1 1 calc R . . C35 C 0.8635(8) 1.0954(7) 0.2328(5) 0.047(2) Uani 1 1 d . . . H35A H 0.7807 1.1340 0.2165 0.057 Uiso 1 1 calc R . . C36 C 0.9707(8) 1.1692(6) 0.2459(4) 0.0542(19) Uani 1 1 d . . . H36A H 0.9605 1.2572 0.2397 0.065 Uiso 1 1 calc R . . C37 C 1.0957(7) 1.1129(5) 0.2687(3) 0.0494(17) Uani 1 1 d . . . H37A H 1.1690 1.1627 0.2789 0.059 Uiso 1 1 calc R . . C38 C 1.1109(6) 0.9851(5) 0.2760(3) 0.0391(15) Uani 1 1 d . . . H38A H 1.1973 0.9492 0.2891 0.047 Uiso 1 1 calc R . . C39 C 1.0030(6) 0.9059(5) 0.2647(3) 0.0286(13) Uani 1 1 d . . . C40 C 0.8740(6) 0.9628(6) 0.2429(4) 0.0338(17) Uani 1 1 d . . . C41 C 0.3338(5) 0.8934(5) -0.1421(3) 0.0288(13) Uani 1 1 d . . . C42 C 0.3586(5) 0.7929(5) -0.0853(3) 0.0298(13) Uani 1 1 d . . . C43 C 0.3862(6) 0.6716(5) -0.1017(3) 0.0339(14) Uani 1 1 d . . . H43A H 0.4056 0.6044 -0.0629 0.041 Uiso 1 1 calc R . . C44 C 0.3846(6) 0.6519(5) -0.1731(3) 0.0405(15) Uani 1 1 d . . . H44A H 0.4024 0.5706 -0.1830 0.049 Uiso 1 1 calc R . . C45 C 0.3520(7) 0.7333(6) -0.3081(4) 0.0560(19) Uani 1 1 d . . . H45A H 0.3672 0.6525 -0.3192 0.067 Uiso 1 1 calc R . . C46 C 0.3263(9) 0.8289(7) -0.3636(4) 0.073(2) Uani 1 1 d . . . H46A H 0.3221 0.8143 -0.4127 0.087 Uiso 1 1 calc R . . C47 C 0.3060(7) 0.9492(7) -0.3492(4) 0.060(2) Uani 1 1 d . . . H47A H 0.2922 1.0167 -0.3891 0.072 Uiso 1 1 calc R . . C48 C 0.3057(6) 0.9710(6) -0.2775(4) 0.0429(17) Uani 1 1 d . . . H48A H 0.2884 1.0529 -0.2685 0.051 Uiso 1 1 calc R . . C49 C 0.3308(6) 0.8734(6) -0.2167(3) 0.0359(16) Uani 1 1 d . . . C50 C 0.3569(6) 0.7503(6) -0.2330(3) 0.0401(15) Uani 1 1 d . . . C51 C 0.3129(7) 1.0208(6) -0.1229(4) 0.0296(17) Uani 1 1 d . . . C52 C 0.4262(8) 1.0851(7) -0.1078(4) 0.0364(19) Uani 1 1 d . . . C53 C 0.4095(8) 1.1998(7) -0.0847(4) 0.045(2) Uani 1 1 d . . . H53A H 0.4892 1.2400 -0.0732 0.054 Uiso 1 1 calc R . . C54 C 0.2783(7) 1.2544(5) -0.0784(3) 0.0455(17) Uani 1 1 d . . . H54A H 0.2682 1.3319 -0.0623 0.055 Uiso 1 1 calc R . . C55 C 0.0209(8) 1.2523(7) -0.0908(4) 0.061(2) Uani 1 1 d . . . H55A H 0.0093 1.3305 -0.0757 0.074 Uiso 1 1 calc R . . C56 C -0.0942(9) 1.1942(8) -0.1076(5) 0.064(3) Uani 1 1 d . . . H56A H -0.1846 1.2325 -0.1048 0.077 Uiso 1 1 calc R . . C57 C -0.0778(8) 1.0782(7) -0.1289(4) 0.051(2) Uani 1 1 d . . . H57A H -0.1575 1.0386 -0.1408 0.062 Uiso 1 1 calc R . . C58 C 0.0515(6) 1.0203(6) -0.1328(3) 0.0429(17) Uani 1 1 d . . . H58A H 0.0590 0.9406 -0.1462 0.051 Uiso 1 1 calc R . . C59 C 0.1754(6) 1.0782(5) -0.1170(3) 0.0325(14) Uani 1 1 d . . . C60 C 0.1579(7) 1.1965(6) -0.0958(3) 0.0418(16) Uani 1 1 d . . . C61 C 0.6523(7) 0.1969(6) 0.4694(4) 0.0302(17) Uani 1 1 d . . . C62 C 0.7755(8) 0.1290(7) 0.4583(4) 0.038(2) Uani 1 1 d . . . C63 C 0.7765(8) 0.0111(7) 0.4349(5) 0.053(2) Uani 1 1 d . . . H63A H 0.8629 -0.0320 0.4262 0.063 Uiso 1 1 calc R . . C64 C 0.6517(8) -0.0367(6) 0.4255(4) 0.0547(19) Uani 1 1 d . . . H64A H 0.6519 -0.1141 0.4094 0.066 Uiso 1 1 calc R . . C65 C 0.3855(8) -0.0267(7) 0.4295(4) 0.055(2) Uani 1 1 d . . . H65A H 0.3839 -0.1045 0.4139 0.066 Uiso 1 1 calc R . . C66 C 0.2615(9) 0.0328(8) 0.4424(5) 0.061(3) Uani 1 1 d . . . H66A H 0.1747 -0.0040 0.4365 0.073 Uiso 1 1 calc R . . C67 C 0.2603(8) 0.1519(9) 0.4651(4) 0.055(2) Uani 1 1 d . . . H67A H 0.1732 0.1936 0.4744 0.067 Uiso 1 1 calc R . . C68 C 0.3881(6) 0.2047(6) 0.4731(3) 0.0409(16) Uani 1 1 d . . . H68A H 0.3880 0.2839 0.4871 0.049 Uiso 1 1 calc R . . C69 C 0.5191(6) 0.1423(5) 0.4609(3) 0.0343(14) Uani 1 1 d . . . C70 C 0.5197(7) 0.0236(6) 0.4386(3) 0.0425(16) Uani 1 1 d . . . C71 C 0.6617(5) 0.3233(5) 0.4904(3) 0.0271(13) Uani 1 1 d . . . C72 C 0.7086(5) 0.4263(5) 0.4339(3) 0.0310(14) Uani 1 1 d . . . C73 C 0.7238(6) 0.5466(5) 0.4516(4) 0.0370(15) Uani 1 1 d . . . H73A H 0.7571 0.6164 0.4125 0.044 Uiso 1 1 calc R . . C74 C 0.6906(6) 0.5616(6) 0.5246(4) 0.0416(16) Uani 1 1 d . . . H74A H 0.7003 0.6423 0.5354 0.050 Uiso 1 1 calc R . . C75 C 0.6071(7) 0.4720(7) 0.6618(4) 0.059(2) Uani 1 1 d . . . H75A H 0.6173 0.5517 0.6740 0.070 Uiso 1 1 calc R . . C76 C 0.5594(8) 0.3706(8) 0.7181(4) 0.079(3) Uani 1 1 d . . . H76A H 0.5367 0.3807 0.7690 0.095 Uiso 1 1 calc R . . C77 C 0.5443(7) 0.2529(7) 0.7010(4) 0.064(2) Uani 1 1 d . . . H77A H 0.5125 0.1833 0.7404 0.077 Uiso 1 1 calc R . . C78 C 0.5750(7) 0.2369(6) 0.6277(4) 0.0515(18) Uani 1 1 d . . . H78A H 0.5613 0.1565 0.6171 0.062 Uiso 1 1 calc R . . C79 C 0.6267(6) 0.3376(6) 0.5675(3) 0.0338(15) Uani 1 1 d . . . C80 C 0.6413(6) 0.4583(6) 0.5851(3) 0.0390(15) Uani 1 1 d . . . C81 C 0.782(2) -0.0795(12) 0.7300(8) 0.208(7) Uani 1 1 d . . . H81A H 0.7600 0.0105 0.7193 0.249 Uiso 1 1 calc R . . H81B H 0.8835 -0.0842 0.7373 0.249 Uiso 1 1 calc R . . C82 C 0.7758(19) -0.1211(13) 0.6651(8) 0.258(9) Uani 1 1 d . . . H82A H 0.8401 -0.0695 0.6232 0.387 Uiso 1 1 calc R . . H82B H 0.6779 -0.1151 0.6541 0.387 Uiso 1 1 calc R . . H82C H 0.8049 -0.2085 0.6714 0.387 Uiso 1 1 calc R . . C83 C 1.008(2) 0.2902(19) 0.6262(10) 0.231(9) Uani 1 1 d . . . H83A H 0.9073 0.2743 0.6504 0.277 Uiso 1 1 calc R . . H83B H 1.0449 0.2065 0.6216 0.277 Uiso 1 1 calc R . . C84 C 1.059(3) 0.310(2) 0.6730(11) 0.327(15) Uani 1 1 d . . . H84A H 1.1014 0.2338 0.6977 0.491 Uiso 1 1 calc R . . H84B H 0.9868 0.3390 0.7098 0.491 Uiso 1 1 calc R . . H84C H 1.1334 0.3753 0.6530 0.491 Uiso 1 1 calc R . . 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 0.0397(4) 0.0486(4) 0.0720(5) -0.0144(3) -0.0101(3) -0.0007(3) Ag2 0.0392(4) 0.0504(4) 0.0730(5) -0.0156(4) -0.0147(3) 0.0051(3) N1 0.040(3) 0.056(3) 0.044(3) 0.000(3) -0.008(3) -0.002(3) N2 0.042(3) 0.034(3) 0.061(4) -0.004(3) -0.012(3) -0.004(2) N3 0.033(3) 0.034(3) 0.063(4) 0.003(3) -0.012(3) 0.002(2) N4 0.043(3) 0.057(3) 0.051(4) -0.008(3) -0.011(3) 0.001(3) O1 0.033(2) 0.052(3) 0.029(3) -0.008(2) -0.0030(19) -0.015(2) O2 0.030(2) 0.026(2) 0.037(2) -0.0044(19) -0.0050(18) 0.0051(17) O3 0.034(3) 0.049(3) 0.035(3) -0.009(2) -0.002(2) 0.016(2) O4 0.034(2) 0.026(2) 0.036(2) -0.0080(19) -0.0063(18) -0.0034(17) O5 0.048(3) 0.036(3) 0.031(3) -0.005(2) -0.009(2) 0.012(2) O6 0.035(3) 0.044(3) 0.049(3) -0.012(3) -0.013(2) 0.002(2) O7 0.037(3) 0.055(4) 0.084(4) -0.030(3) -0.005(3) 0.002(3) O8 0.050(3) 0.044(3) 0.027(3) -0.003(2) 0.001(2) -0.015(2) O9 0.080(4) 0.068(4) 0.118(5) -0.044(4) 0.013(4) -0.005(3) O10 0.092(4) 0.075(4) 0.120(5) -0.041(4) -0.037(4) 0.005(3) C1 0.025(3) 0.018(3) 0.032(4) -0.004(3) -0.004(3) 0.002(2) C2 0.026(3) 0.028(4) 0.024(4) 0.001(3) 0.001(3) 0.002(3) C3 0.025(4) 0.042(4) 0.040(5) -0.014(3) -0.008(3) -0.001(3) C4 0.026(3) 0.031(3) 0.050(4) -0.004(3) 0.003(3) -0.011(3) C5 0.037(4) 0.050(4) 0.042(5) -0.001(4) 0.007(4) 0.008(4) C6 0.055(5) 0.071(5) 0.031(4) -0.008(4) 0.013(4) -0.003(4) C7 0.050(4) 0.062(5) 0.037(4) -0.013(4) -0.013(3) 0.003(4) C8 0.033(3) 0.039(4) 0.035(4) -0.006(3) -0.002(3) 0.002(3) C9 0.028(3) 0.025(3) 0.032(4) -0.006(3) -0.003(3) 0.002(2) C10 0.028(4) 0.034(5) 0.030(5) -0.005(4) -0.003(3) 0.004(3) C11 0.022(3) 0.032(3) 0.024(3) -0.009(3) -0.004(2) 0.001(2) C12 0.017(3) 0.039(4) 0.025(4) -0.007(3) -0.007(3) 0.001(3) C13 0.027(4) 0.037(4) 0.043(4) -0.015(3) -0.004(3) 0.007(3) C14 0.034(4) 0.045(4) 0.037(4) -0.003(3) -0.005(3) -0.004(3) C15 0.051(5) 0.035(4) 0.043(5) -0.004(4) -0.004(4) -0.017(4) C16 0.073(5) 0.032(4) 0.065(5) -0.013(4) -0.002(4) -0.007(4) C17 0.055(4) 0.038(4) 0.064(5) -0.016(4) -0.006(4) 0.010(3) C18 0.039(4) 0.033(4) 0.047(4) -0.007(3) -0.014(3) 0.002(3) C19 0.026(3) 0.024(3) 0.032(4) -0.006(3) -0.007(3) 0.004(2) C20 0.035(4) 0.031(4) 0.031(4) -0.005(3) -0.006(3) -0.004(3) C21 0.026(3) 0.019(3) 0.029(3) -0.003(3) -0.011(3) -0.002(2) C22 0.036(4) 0.032(4) 0.025(4) -0.011(3) -0.011(3) -0.003(3) C23 0.025(4) 0.045(4) 0.037(4) -0.006(3) -0.004(3) 0.004(3) C24 0.030(3) 0.039(4) 0.049(4) -0.008(3) -0.020(3) 0.009(3) C25 0.053(5) 0.041(4) 0.051(5) -0.007(4) -0.028(4) -0.003(4) C26 0.063(5) 0.072(5) 0.031(5) -0.014(4) -0.008(4) -0.011(4) C27 0.057(5) 0.067(5) 0.029(4) -0.014(4) 0.000(3) -0.013(4) C28 0.042(4) 0.041(4) 0.030(4) -0.007(3) -0.010(3) -0.005(3) C29 0.036(3) 0.024(3) 0.029(4) -0.008(3) -0.009(3) -0.004(3) C30 0.038(5) 0.034(5) 0.038(5) -0.009(4) -0.013(4) -0.002(4) C31 0.025(3) 0.030(3) 0.024(3) -0.009(3) -0.004(2) -0.001(2) C32 0.030(3) 0.034(4) 0.033(4) -0.010(3) -0.007(3) 0.003(3) C33 0.031(4) 0.046(5) 0.044(5) -0.013(4) -0.005(3) -0.008(3) C34 0.028(4) 0.055(5) 0.057(5) -0.010(4) -0.017(3) 0.011(3) C35 0.047(5) 0.042(5) 0.053(5) -0.009(4) -0.009(4) 0.022(4) C36 0.073(5) 0.031(4) 0.064(5) -0.018(4) -0.016(4) 0.008(4) C37 0.060(4) 0.032(4) 0.060(5) -0.019(3) -0.009(4) -0.009(3) C38 0.039(4) 0.032(4) 0.047(4) -0.010(3) -0.006(3) 0.002(3) C39 0.031(3) 0.026(3) 0.030(4) -0.009(3) -0.003(3) 0.005(3) C40 0.028(4) 0.037(4) 0.035(4) -0.007(3) -0.003(3) 0.007(3) C41 0.019(3) 0.039(4) 0.026(3) -0.001(3) -0.003(3) 0.000(3) C42 0.025(3) 0.040(4) 0.023(4) -0.008(3) 0.000(3) 0.003(3) C43 0.036(4) 0.031(4) 0.037(4) -0.011(3) -0.007(3) 0.004(3) C44 0.045(4) 0.031(4) 0.046(4) -0.014(3) -0.002(3) 0.005(3) C45 0.075(5) 0.044(4) 0.048(5) -0.009(4) -0.010(4) 0.001(4) C46 0.119(7) 0.061(6) 0.045(5) -0.013(4) -0.029(5) -0.009(5) C47 0.088(6) 0.061(5) 0.035(5) -0.009(4) -0.024(4) -0.012(4) C48 0.056(4) 0.040(4) 0.039(4) -0.013(3) -0.018(3) 0.000(3) C49 0.033(4) 0.037(4) 0.034(4) 0.001(3) -0.006(3) -0.004(3) C50 0.038(4) 0.045(4) 0.037(4) -0.010(3) -0.003(3) -0.002(3) C51 0.022(4) 0.028(4) 0.034(4) -0.001(3) 0.002(3) -0.001(3) C52 0.033(4) 0.038(5) 0.034(5) -0.001(4) -0.002(3) 0.000(3) C53 0.061(5) 0.034(4) 0.047(5) -0.011(4) -0.021(4) -0.007(4) C54 0.065(5) 0.027(4) 0.047(4) -0.013(3) -0.011(4) 0.007(3) C55 0.067(6) 0.052(5) 0.059(6) -0.006(4) 0.003(4) 0.012(4) C56 0.043(5) 0.067(6) 0.078(7) -0.006(5) -0.007(5) 0.019(4) C57 0.032(5) 0.052(5) 0.060(6) 0.007(4) 0.001(4) 0.005(4) C58 0.024(3) 0.048(4) 0.050(5) 0.004(3) -0.007(3) 0.005(3) C59 0.036(4) 0.030(3) 0.027(3) 0.001(3) 0.001(3) 0.004(3) C60 0.045(4) 0.039(4) 0.036(4) -0.001(3) 0.000(3) 0.010(3) C61 0.029(4) 0.027(4) 0.036(4) -0.005(3) -0.009(3) -0.001(3) C62 0.035(4) 0.038(5) 0.042(5) -0.009(4) -0.005(3) -0.005(3) C63 0.053(5) 0.035(4) 0.070(6) -0.017(4) -0.002(4) 0.005(4) C64 0.078(5) 0.033(4) 0.055(5) -0.018(3) -0.005(4) -0.009(4) C65 0.073(6) 0.048(5) 0.047(5) -0.007(4) -0.023(4) -0.025(4) C66 0.059(6) 0.070(6) 0.057(5) -0.003(5) -0.032(5) -0.021(5) C67 0.030(5) 0.085(7) 0.047(5) 0.010(5) -0.022(4) -0.002(4) C68 0.037(4) 0.044(4) 0.039(4) 0.004(3) -0.013(3) -0.006(3) C69 0.039(4) 0.039(4) 0.023(3) -0.004(3) -0.004(3) -0.007(3) C70 0.047(4) 0.048(4) 0.033(4) -0.006(3) -0.012(3) -0.008(3) C71 0.024(3) 0.031(3) 0.027(3) -0.008(3) -0.004(3) 0.001(2) C72 0.023(3) 0.036(4) 0.035(4) -0.007(3) -0.008(3) 0.001(3) C73 0.036(4) 0.032(4) 0.042(4) -0.002(3) -0.010(3) -0.011(3) C74 0.042(4) 0.040(4) 0.045(4) -0.008(3) -0.009(3) -0.008(3) C75 0.078(5) 0.058(5) 0.044(5) -0.027(4) -0.001(4) -0.016(4) C76 0.111(7) 0.090(6) 0.030(5) -0.028(5) 0.030(4) -0.031(5) C77 0.091(6) 0.063(5) 0.040(5) -0.018(4) -0.005(4) -0.015(4) C78 0.063(5) 0.048(4) 0.043(5) -0.011(4) -0.006(4) -0.011(4) C79 0.025(3) 0.043(4) 0.030(4) -0.003(3) 0.000(3) -0.004(3) C80 0.041(4) 0.045(4) 0.035(4) -0.020(3) -0.006(3) -0.001(3) C81 0.38(2) 0.133(11) 0.113(12) -0.050(10) -0.028(14) 0.005(13) C82 0.47(3) 0.188(16) 0.134(14) -0.058(12) -0.086(16) 0.120(17) C83 0.34(2) 0.230(19) 0.156(19) -0.047(16) -0.134(18) -0.003(16) C84 0.59(5) 0.22(2) 0.16(2) 0.037(17) -0.14(2) -0.14(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 Ag1 N2 2.133(4) . ? Ag1 N1 2.140(4) . ? Ag2 N4 2.129(4) . ? Ag2 N3 2.150(4) . ? N1 H1A 0.9000 . ? N1 H1B 0.9000 . ? N1 H1C 0.9000 . ? N2 H2A 0.9000 . ? N2 H2B 0.9000 . ? N2 H2C 0.9000 . ? N3 H3A 0.9000 . ? N3 H3B 0.9000 . ? N3 H3C 0.9000 . ? N4 H4A 0.9000 . ? N4 H4B 0.9000 . ? N4 H4C 0.9000 . ? O1 C2 1.351(6) . ? O1 H1D 0.88(6) . ? O2 C12 1.322(6) . ? O3 C22 1.362(7) . ? O3 H3D 0.75(6) . ? O4 C32 1.333(6) . ? O5 C42 1.349(6) . ? O5 H5B 0.86(4) . ? O6 C52 1.366(7) . ? O6 H6A 0.8300 . ? O7 C62 1.383(7) . ? O7 H7A 0.8300 . ? O8 C72 1.347(6) . ? O8 H8B 0.81(4) . ? O9 C81 1.523(14) . ? O9 H9A 0.8245 . ? O10 C83 1.534(15) . ? O10 H10A 0.8297 . ? C1 C2 1.386(7) . ? C1 C9 1.434(7) . ? C1 C11 1.508(6) . ? C2 C3 1.399(7) . ? C3 C4 1.369(8) . ? C3 H3E 0.9400 . ? C4 C10 1.419(8) . ? C4 H4D 0.9400 . ? C5 C6 1.348(9) . ? C5 C10 1.397(9) . ? C5 H5A 0.9400 . ? C6 C7 1.397(8) . ? C6 H6B 0.9400 . ? C7 C8 1.383(7) . ? C7 H7B 0.9400 . ? C8 C9 1.413(7) . ? C8 H8A 0.9400 . ? C9 C10 1.425(8) . ? C11 C12 1.380(7) . ? C11 C19 1.428(7) . ? C12 C13 1.433(7) . ? C13 C14 1.371(8) . ? C13 H13A 0.9400 . ? C14 C20 1.408(8) . ? C14 H14A 0.9400 . ? C15 C16 1.345(9) . ? C15 C20 1.427(9) . ? C15 H15A 0.9400 . ? C16 C17 1.391(8) . ? C16 H16A 0.9400 . ? C17 C18 1.359(7) . ? C17 H17A 0.9400 . ? C18 C19 1.408(7) . ? C18 H18A 0.9400 . ? C19 C20 1.430(7) . ? C21 C22 1.363(8) . ? C21 C29 1.418(7) . ? C21 C31 1.501(6) . ? C22 C23 1.404(7) . ? C23 C24 1.365(8) . ? C23 H23A 0.9400 . ? C24 C30 1.384(9) . ? C24 H24A 0.9400 . ? C25 C26 1.351(9) . ? C25 C30 1.430(10) . ? C25 H25A 0.9400 . ? C26 C27 1.389(8) . ? C26 H26A 0.9400 . ? C27 C28 1.353(7) . ? C27 H27A 0.9400 . ? C28 C29 1.419(7) . ? C28 H28A 0.9400 . ? C29 C30 1.422(8) . ? C31 C32 1.386(7) . ? C31 C39 1.426(7) . ? C32 C33 1.426(8) . ? C33 C34 1.351(8) . ? C33 H33A 0.9400 . ? C34 C40 1.399(8) . ? C34 H34A 0.9400 . ? C35 C36 1.368(9) . ? C35 C40 1.412(10) . ? C35 H35A 0.9400 . ? C36 C37 1.399(8) . ? C36 H36A 0.9400 . ? C37 C38 1.368(7) . ? C37 H37A 0.9400 . ? C38 C39 1.396(7) . ? C38 H38A 0.9400 . ? C39 C40 1.429(7) . ? C41 C42 1.381(7) . ? C41 C49 1.414(8) . ? C41 C51 1.492(8) . ? C42 C43 1.415(7) . ? C43 C44 1.355(7) . ? C43 H43A 0.9400 . ? C44 C50 1.410(7) . ? C44 H44A 0.9400 . ? C45 C46 1.336(8) . ? C45 C50 1.416(8) . ? C45 H45A 0.9400 . ? C46 C47 1.384(10) . ? C46 H46A 0.9400 . ? C47 C48 1.365(9) . ? C47 H47A 0.9400 . ? C48 C49 1.409(8) . ? C48 H48A 0.9400 . ? C49 C50 1.431(8) . ? C51 C52 1.366(9) . ? C51 C59 1.427(8) . ? C52 C53 1.387(10) . ? C53 C54 1.361(8) . ? C53 H53A 0.9400 . ? C54 C60 1.404(8) . ? C54 H54A 0.9400 . ? C55 C56 1.359(9) . ? C55 C60 1.415(8) . ? C55 H55A 0.9400 . ? C56 C57 1.385(10) . ? C56 H56A 0.9400 . ? C57 C58 1.360(8) . ? C57 H57A 0.9400 . ? C58 C59 1.420(7) . ? C58 H58A 0.9400 . ? C59 C60 1.408(7) . ? C61 C62 1.375(9) . ? C61 C69 1.430(8) . ? C61 C71 1.497(8) . ? C62 C63 1.421(10) . ? C63 C64 1.333(8) . ? C63 H63A 0.9400 . ? C64 C70 1.406(8) . ? C64 H64A 0.9400 . ? C65 C66 1.338(10) . ? C65 C70 1.422(8) . ? C65 H65A 0.9400 . ? C66 C67 1.427(11) . ? C66 H66A 0.9400 . ? C67 C68 1.373(8) . ? C67 H67A 0.9400 . ? C68 C69 1.408(7) . ? C68 H68A 0.9400 . ? C69 C70 1.420(8) . ? C71 C72 1.372(7) . ? C71 C79 1.422(7) . ? C72 C73 1.414(7) . ? C73 C74 1.351(7) . ? C73 H73A 0.9400 . ? C74 C80 1.419(7) . ? C74 H74A 0.9400 . ? C75 C76 1.360(9) . ? C75 C80 1.413(8) . ? C75 H75A 0.9400 . ? C76 C77 1.382(9) . ? C76 H76A 0.9400 . ? C77 C78 1.359(8) . ? C77 H77A 0.9400 . ? C78 C79 1.403(7) . ? C78 H78A 0.9400 . ? C79 C80 1.416(7) . ? C81 C82 1.350(14) . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C82 H82A 0.9700 . ? C82 H82B 0.9700 . ? C82 H82C 0.9700 . ? C83 C84 1.093(16) . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C84 H84A 0.9700 . ? C84 H84B 0.9700 . ? C84 H84C 0.9700 . ? 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 N2 Ag1 N1 172.21(18) . . ? N4 Ag2 N3 172.73(18) . . ? Ag1 N1 H1A 109.5 . . ? Ag1 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? Ag1 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? Ag1 N2 H2A 109.5 . . ? Ag1 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? Ag1 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? Ag2 N3 H3A 109.5 . . ? Ag2 N3 H3B 109.5 . . ? H3A N3 H3B 109.5 . . ? Ag2 N3 H3C 109.5 . . ? H3A N3 H3C 109.5 . . ? H3B N3 H3C 109.5 . . ? Ag2 N4 H4A 109.5 . . ? Ag2 N4 H4B 109.5 . . ? H4A N4 H4B 109.5 . . ? Ag2 N4 H4C 109.5 . . ? H4A N4 H4C 109.5 . . ? H4B N4 H4C 109.5 . . ? C2 O1 H1D 108(4) . . ? C22 O3 H3D 115(5) . . ? C42 O5 H5B 111(5) . . ? C52 O6 H6A 109.5 . . ? C62 O7 H7A 109.5 . . ? C72 O8 H8B 113(5) . . ? C81 O9 H9A 109.7 . . ? C83 O10 H10A 109.5 . . ? C2 C1 C9 118.7(5) . . ? C2 C1 C11 120.3(5) . . ? C9 C1 C11 120.9(5) . . ? O1 C2 C1 118.8(5) . . ? O1 C2 C3 120.7(5) . . ? C1 C2 C3 120.5(5) . . ? C4 C3 C2 121.5(6) . . ? C4 C3 H3E 119.2 . . ? C2 C3 H3E 119.2 . . ? C3 C4 C10 120.8(6) . . ? C3 C4 H4D 119.6 . . ? C10 C4 H4D 119.6 . . ? C6 C5 C10 121.2(7) . . ? C6 C5 H5A 119.4 . . ? C10 C5 H5A 119.4 . . ? C5 C6 C7 120.8(7) . . ? C5 C6 H6B 119.6 . . ? C7 C6 H6B 119.6 . . ? C8 C7 C6 119.8(6) . . ? C8 C7 H7B 120.1 . . ? C6 C7 H7B 120.1 . . ? C7 C8 C9 120.8(5) . . ? C7 C8 H8A 119.6 . . ? C9 C8 H8A 119.6 . . ? C8 C9 C10 117.7(5) . . ? C8 C9 C1 121.6(5) . . ? C10 C9 C1 120.6(5) . . ? C5 C10 C4 122.5(6) . . ? C5 C10 C9 119.7(6) . . ? C4 C10 C9 117.8(6) . . ? C12 C11 C19 121.1(5) . . ? C12 C11 C1 120.3(5) . . ? C19 C11 C1 118.6(4) . . ? O2 C12 C11 123.7(5) . . ? O2 C12 C13 118.5(5) . . ? C11 C12 C13 117.7(5) . . ? C14 C13 C12 122.4(6) . . ? C14 C13 H13A 118.8 . . ? C12 C13 H13A 118.8 . . ? C13 C14 C20 120.4(6) . . ? C13 C14 H14A 119.8 . . ? C20 C14 H14A 119.8 . . ? C16 C15 C20 120.7(7) . . ? C16 C15 H15A 119.6 . . ? C20 C15 H15A 119.6 . . ? C15 C16 C17 119.9(6) . . ? C15 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? C18 C17 C16 121.9(6) . . ? C18 C17 H17A 119.0 . . ? C16 C17 H17A 119.0 . . ? C17 C18 C19 120.5(5) . . ? C17 C18 H18A 119.8 . . ? C19 C18 H18A 119.8 . . ? C18 C19 C11 122.3(5) . . ? C18 C19 C20 117.9(5) . . ? C11 C19 C20 119.8(5) . . ? C14 C20 C15 122.5(6) . . ? C14 C20 C19 118.5(6) . . ? C15 C20 C19 119.0(6) . . ? C22 C21 C29 118.7(5) . . ? C22 C21 C31 120.5(5) . . ? C29 C21 C31 120.8(5) . . ? O3 C22 C21 119.0(5) . . ? O3 C22 C23 120.1(5) . . ? C21 C22 C23 120.9(6) . . ? C24 C23 C22 120.8(6) . . ? C24 C23 H23A 119.6 . . ? C22 C23 H23A 119.6 . . ? C23 C24 C30 120.4(6) . . ? C23 C24 H24A 119.8 . . ? C30 C24 H24A 119.8 . . ? C26 C25 C30 121.4(7) . . ? C26 C25 H25A 119.3 . . ? C30 C25 H25A 119.3 . . ? C25 C26 C27 119.8(7) . . ? C25 C26 H26A 120.1 . . ? C27 C26 H26A 120.1 . . ? C28 C27 C26 121.0(6) . . ? C28 C27 H27A 119.5 . . ? C26 C27 H27A 119.5 . . ? C27 C28 C29 121.9(6) . . ? C27 C28 H28A 119.0 . . ? C29 C28 H28A 119.0 . . ? C21 C29 C28 122.8(5) . . ? C21 C29 C30 120.0(6) . . ? C28 C29 C30 117.2(6) . . ? C24 C30 C29 119.2(6) . . ? C24 C30 C25 122.2(7) . . ? C29 C30 C25 118.6(7) . . ? C32 C31 C39 120.3(5) . . ? C32 C31 C21 120.6(5) . . ? C39 C31 C21 119.1(4) . . ? O4 C32 C31 123.7(5) . . ? O4 C32 C33 118.1(5) . . ? C31 C32 C33 118.1(6) . . ? C34 C33 C32 122.5(6) . . ? C34 C33 H33A 118.8 . . ? C32 C33 H33A 118.8 . . ? C33 C34 C40 120.8(6) . . ? C33 C34 H34A 119.6 . . ? C40 C34 H34A 119.6 . . ? C36 C35 C40 121.8(7) . . ? C36 C35 H35A 119.1 . . ? C40 C35 H35A 119.1 . . ? C35 C36 C37 119.6(6) . . ? C35 C36 H36A 120.2 . . ? C37 C36 H36A 120.2 . . ? C38 C37 C36 119.8(6) . . ? C38 C37 H37A 120.1 . . ? C36 C37 H37A 120.1 . . ? C37 C38 C39 122.5(6) . . ? C37 C38 H38A 118.7 . . ? C39 C38 H38A 118.7 . . ? C38 C39 C31 122.5(5) . . ? C38 C39 C40 117.8(5) . . ? C31 C39 C40 119.6(5) . . ? C34 C40 C35 122.8(6) . . ? C34 C40 C39 118.7(6) . . ? C35 C40 C39 118.4(6) . . ? C42 C41 C49 119.5(5) . . ? C42 C41 C51 118.6(5) . . ? C49 C41 C51 121.9(5) . . ? O5 C42 C41 118.9(5) . . ? O5 C42 C43 120.4(5) . . ? C41 C42 C43 120.7(5) . . ? C44 C43 C42 120.1(5) . . ? C44 C43 H43A 119.9 . . ? C42 C43 H43A 119.9 . . ? C43 C44 C50 121.7(5) . . ? C43 C44 H44A 119.2 . . ? C50 C44 H44A 119.2 . . ? C46 C45 C50 121.9(6) . . ? C46 C45 H45A 119.1 . . ? C50 C45 H45A 119.1 . . ? C45 C46 C47 120.3(7) . . ? C45 C46 H46A 119.9 . . ? C47 C46 H46A 119.9 . . ? C48 C47 C46 120.6(7) . . ? C48 C47 H47A 119.7 . . ? C46 C47 H47A 119.7 . . ? C47 C48 C49 121.5(7) . . ? C47 C48 H48A 119.3 . . ? C49 C48 H48A 119.3 . . ? C48 C49 C41 122.8(6) . . ? C48 C49 C50 117.4(6) . . ? C41 C49 C50 119.8(5) . . ? C44 C50 C45 123.4(6) . . ? C44 C50 C49 118.2(6) . . ? C45 C50 C49 118.4(6) . . ? C52 C51 C59 117.6(7) . . ? C52 C51 C41 120.3(6) . . ? C59 C51 C41 122.1(6) . . ? C51 C52 O6 122.6(7) . . ? C51 C52 C53 122.1(7) . . ? O6 C52 C53 115.3(7) . . ? C54 C53 C52 120.4(7) . . ? C54 C53 H53A 119.8 . . ? C52 C53 H53A 119.8 . . ? C53 C54 C60 120.8(6) . . ? C53 C54 H54A 119.6 . . ? C60 C54 H54A 119.6 . . ? C56 C55 C60 120.7(8) . . ? C56 C55 H55A 119.6 . . ? C60 C55 H55A 119.6 . . ? C55 C56 C57 119.7(8) . . ? C55 C56 H56A 120.2 . . ? C57 C56 H56A 120.2 . . ? C58 C57 C56 121.3(8) . . ? C58 C57 H57A 119.3 . . ? C56 C57 H57A 119.3 . . ? C57 C58 C59 121.1(7) . . ? C57 C58 H58A 119.5 . . ? C59 C58 H58A 119.5 . . ? C60 C59 C58 117.2(5) . . ? C60 C59 C51 120.8(6) . . ? C58 C59 C51 122.0(6) . . ? C54 C60 C59 118.2(5) . . ? C54 C60 C55 121.8(6) . . ? C59 C60 C55 120.0(6) . . ? C62 C61 C69 118.0(7) . . ? C62 C61 C71 119.4(6) . . ? C69 C61 C71 122.6(6) . . ? C61 C62 O7 122.8(7) . . ? C61 C62 C63 122.7(7) . . ? O7 C62 C63 114.5(7) . . ? C64 C63 C62 118.2(7) . . ? C64 C63 H63A 120.9 . . ? C62 C63 H63A 120.9 . . ? C63 C64 C70 122.9(6) . . ? C63 C64 H64A 118.5 . . ? C70 C64 H64A 118.5 . . ? C66 C65 C70 122.3(7) . . ? C66 C65 H65A 118.9 . . ? C70 C65 H65A 118.9 . . ? C65 C66 C67 120.3(7) . . ? C65 C66 H66A 119.8 . . ? C67 C66 H66A 119.8 . . ? C68 C67 C66 119.1(7) . . ? C68 C67 H67A 120.4 . . ? C66 C67 H67A 120.4 . . ? C67 C68 C69 121.2(7) . . ? C67 C68 H68A 119.4 . . ? C69 C68 H68A 119.4 . . ? C68 C69 C70 119.4(5) . . ? C68 C69 C61 121.3(6) . . ? C70 C69 C61 119.2(6) . . ? C64 C70 C69 118.8(5) . . ? C64 C70 C65 123.6(7) . . ? C69 C70 C65 117.6(6) . . ? C72 C71 C79 119.8(5) . . ? C72 C71 C61 118.8(5) . . ? C79 C71 C61 121.4(5) . . ? O8 C72 C71 118.9(5) . . ? O8 C72 C73 120.4(5) . . ? C71 C72 C73 120.7(5) . . ? C74 C73 C72 120.1(6) . . ? C74 C73 H73A 120.0 . . ? C72 C73 H73A 120.0 . . ? C73 C74 C80 121.5(6) . . ? C73 C74 H74A 119.2 . . ? C80 C74 H74A 119.2 . . ? C76 C75 C80 120.4(6) . . ? C76 C75 H75A 119.8 . . ? C80 C75 H75A 119.8 . . ? C75 C76 C77 120.4(7) . . ? C75 C76 H76A 119.8 . . ? C77 C76 H76A 119.8 . . ? C78 C77 C76 120.7(7) . . ? C78 C77 H77A 119.7 . . ? C76 C77 H77A 119.7 . . ? C77 C78 C79 121.5(6) . . ? C77 C78 H78A 119.3 . . ? C79 C78 H78A 119.3 . . ? C78 C79 C80 117.7(5) . . ? C78 C79 C71 122.7(6) . . ? C80 C79 C71 119.5(5) . . ? C75 C80 C79 119.4(6) . . ? C75 C80 C74 122.3(6) . . ? C79 C80 C74 118.3(5) . . ? C82 C81 O9 124.4(14) . . ? C82 C81 H81A 106.2 . . ? O9 C81 H81A 106.2 . . ? C82 C81 H81B 106.2 . . ? O9 C81 H81B 106.2 . . ? H81A C81 H81B 106.4 . . ? C81 C82 H82A 109.5 . . ? C81 C82 H82B 109.5 . . ? H82A C82 H82B 109.5 . . ? C81 C82 H82C 109.5 . . ? H82A C82 H82C 109.5 . . ? H82B C82 H82C 109.5 . . ? C84 C83 O10 140(2) . . ? C84 C83 H83A 102.0 . . ? O10 C83 H83A 102.0 . . ? C84 C83 H83B 102.0 . . ? O10 C83 H83B 102.0 . . ? H83A C83 H83B 104.8 . . ? C83 C84 H84A 109.5 . . ? C83 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C83 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? 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 N1 H1A O8 0.90 2.23 3.110(6) 164.5 . N1 H1B O1 0.90 2.38 3.034(6) 129.9 . N2 H2A O7 0.90 2.49 3.249(7) 142.3 1_455 N2 H2B O4 0.90 2.10 2.947(5) 155.5 1_455 N3 H3A O6 0.90 2.43 3.175(7) 140.3 1_455 N3 H3B O2 0.90 2.12 2.963(5) 156.0 1_455 N4 H4A O5 0.90 2.38 3.098(6) 136.4 . N4 H4B O3 0.90 2.19 3.036(6) 155.8 1_455 O1 H1D O4 0.88(6) 1.75(6) 2.630(5) 173(6) . O3 H3D O2 0.75(6) 1.89(6) 2.640(5) 176(7) 1_655 O5 H5B O2 0.86(4) 1.72(4) 2.562(5) 167(7) . O6 H6A O9 0.83 2.06 2.782(7) 145.8 1_564 O7 H7A O10 0.83 2.06 2.765(7) 143.1 . O8 H8B O4 0.81(4) 1.76(4) 2.571(5) 173(8) . _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.10 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.726 _refine_diff_density_min -0.924 _refine_diff_density_rms 0.079