# Electronic Supplementary Material (ESI) for ChemComm. # This journal is © The Royal Society of Chemistry 2017 ####################################################################### # # This file contains crystal structure data downloaded from the # Cambridge Structural Database (CSD) hosted by the Cambridge # Crystallographic Data Centre (CCDC). # # Full information about CCDC data access policies and citation # guidelines are available at http://www.ccdc.cam.ac.uk/access/V1 # # Audit and citation data items may have been added by the CCDC. # Please retain this information to preserve the provenance of # this file and to allow appropriate attribution of the data. # ####################################################################### data_AgMethionine _database_code_depnum_ccdc_archive 'CCDC 1547635' _audit_update_record ; 2017-05-03 deposited with the CCDC. 2017-05-11 downloaded from the CCDC. ; _audit_creation_method SHELXL-2014/7 _shelx_SHELXL_version_number 2014/7 _chemical_name_systematic 'poly(disilver-dimethionine-dinitrate) dihydrate' _chemical_name_common ? _chemical_formula_moiety 'C20 H44 Ag2 N4 O8 S4, 2(N O3), 2(H2 O)' _chemical_formula_sum 'C20 H48 Ag2 N6 O16 S4' _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: deuterium oxide' _chemical_melting_point ? _exptl_crystal_description needle _exptl_crystal_colour colourless _diffrn_ambient_temperature 200(2) _chemical_formula_weight 972.62 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' Ag Ag -0.8971 1.1015 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_H-M_alt 'P 21' _space_group_name_Hall 'P 2yb' _chemical_absolute_configuration syn loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z' _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _cell_length_a 5.0810(3) _cell_length_b 24.7309(12) _cell_length_c 14.5097(10) _cell_angle_alpha 90 _cell_angle_beta 99.007(5) _cell_angle_gamma 90 _cell_volume 1800.77(19) _cell_formula_units_Z 2 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 16289 _cell_measurement_theta_min 1.64 _cell_measurement_theta_max 25.58 _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.794 _exptl_crystal_F_000 992 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.480 _exptl_crystal_size_mid 0.180 _exptl_crystal_size_min 0.030 _exptl_absorpt_coefficient_mu 1.393 _shelx_estimated_absorpt_T_min 0.554 _shelx_estimated_absorpt_T_max 0.959 _exptl_absorpt_correction_type integration _exptl_absorpt_correction_T_min 0.7492 _exptl_absorpt_correction_T_max 0.9681 _exptl_absorpt_process_details ; Stoe & Cie (2002). X-SHAPE. Stoe & Cie, Darmstadt, Germany ; _exptl_special_details ; ? ; _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_source_type 'Stoe IPDS2' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'STOE IPDS 2' _diffrn_measurement_method 'rotation method' _diffrn_detector_area_resol_mean 6.67 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6406 _diffrn_reflns_av_unetI/netI 0.0814 _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_k_min -29 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 1.421 _diffrn_reflns_theta_max 25.189 _diffrn_reflns_theta_full 25.189 _diffrn_measured_fraction_theta_max 0.992 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.992 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.989 _diffrn_reflns_point_group_measured_fraction_full 0.989 _reflns_number_total 6406 _reflns_number_gt 4756 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.944 _reflns_Friedel_fraction_max 0.986 _reflns_Friedel_fraction_full 0.986 _reflns_special_details ; _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _computing_data_collection 'X-Area (Stoe & Cie, 2009)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2009)' _computing_data_reduction 'X-RED32(Stoe & Cie, 2009)' _computing_structure_solution 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_structure_refinement 'SHELXL-2014/7 (Sheldrick, 2014)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details 'Refined as a 2-component perfect twin., Twin' _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1193P)^2^+20.4046P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens mixed _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Flack x determined using 1627 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons, Flack and Wagner, Acta Cryst. B69 (2013) 249-259). ; _refine_ls_abs_structure_Flack 0.02(3) _refine_ls_number_reflns 6406 _refine_ls_number_parameters 423 _refine_ls_number_restraints 59 _refine_ls_R_factor_all 0.1164 _refine_ls_R_factor_gt 0.0864 _refine_ls_wR_factor_ref 0.2525 _refine_ls_wR_factor_gt 0.2272 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.016 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.849(4) 0.5296(10) 0.9057(17) 0.045(5) Uani 1 1 d . . . . . C2 C 0.753(4) 0.4751(9) 0.9437(16) 0.041(5) Uani 1 1 d . . . . . H2 H 0.8994 0.4606 0.9914 0.049 Uiso 1 1 calc R U . . . C3 C 0.691(4) 0.4327(9) 0.8637(16) 0.042(2) Uani 1 1 d . . . . . H3A H 0.5877 0.4026 0.8852 0.050 Uiso 1 1 calc R U . . . H3B H 0.5798 0.4498 0.8095 0.050 Uiso 1 1 calc R U . . . C4 C 0.929(5) 0.4111(13) 0.8343(19) 0.061(7) Uani 1 1 d . . . . . H4A H 1.0553 0.4005 0.8905 0.073 Uiso 1 1 calc R U . . . H4B H 1.0146 0.4401 0.8024 0.073 Uiso 1 1 calc R U . . . C5 C 0.716(9) 0.3037(15) 0.824(3) 0.094(12) Uani 1 1 d . . . . . H5A H 0.8250 0.2997 0.8860 0.141 Uiso 1 1 calc R U . . . H5B H 0.6999 0.2686 0.7926 0.141 Uiso 1 1 calc R U . . . H5C H 0.5382 0.3167 0.8318 0.141 Uiso 1 1 calc R U . . . C6 C 0.123(4) 0.4726(10) 0.5944(16) 0.041(5) Uani 1 1 d . . . . . C7 C 0.012(4) 0.5301(9) 0.5672(16) 0.039(5) Uani 1 1 d . U . . . H7 H 0.1207 0.5457 0.5218 0.047 Uiso 1 1 calc R U . . . C8 C 0.010(4) 0.5700(10) 0.6440(16) 0.042(2) Uani 1 1 d . U . . . H8A H -0.0942 0.5551 0.6905 0.050 Uiso 1 1 calc R U . . . H8B H -0.0793 0.6036 0.6183 0.050 Uiso 1 1 calc R U . . . C9 C 0.298(4) 0.5837(9) 0.6933(16) 0.040(5) Uani 1 1 d . U . . . H9A H 0.4151 0.5880 0.6452 0.048 Uiso 1 1 calc R U . . . H9B H 0.3669 0.5530 0.7338 0.048 Uiso 1 1 calc R U . . . C10 C 0.240(10) 0.6935(13) 0.674(3) 0.091(12) Uani 1 1 d . . . . . H10A H 0.4042 0.7119 0.6639 0.136 Uiso 1 1 calc R U . . . H10B H 0.1154 0.7201 0.6927 0.136 Uiso 1 1 calc R U . . . H10C H 0.1591 0.6756 0.6164 0.136 Uiso 1 1 calc R U . . . C11 C 1.016(4) 0.5416(9) 1.1585(15) 0.036(5) Uani 1 1 d . . . . . C12 C 1.138(4) 0.5975(8) 1.1963(15) 0.032(4) Uani 1 1 d . U . . . H12 H 1.0240 0.6122 1.2409 0.038 Uiso 1 1 calc R U . . . C13 C 1.154(4) 0.6408(11) 1.1207(16) 0.042(2) Uani 1 1 d . U . . . H13A H 1.2693 0.6709 1.1481 0.050 Uiso 1 1 calc R U . . . H13B H 1.2368 0.6248 1.0697 0.050 Uiso 1 1 calc R U . . . C14 C 0.893(4) 0.6620(10) 1.0827(16) 0.044(5) Uani 1 1 d . U . . . H14A H 0.8183 0.6822 1.1315 0.053 Uiso 1 1 calc R U . . . H14B H 0.7703 0.6318 1.0614 0.053 Uiso 1 1 calc R U . . . C15 C 0.589(5) 0.7323(12) 0.9575(19) 0.055(7) Uani 1 1 d . . . . . H15A H 0.4654 0.7022 0.9404 0.083 Uiso 1 1 calc R U . . . H15B H 0.5769 0.7578 0.9053 0.083 Uiso 1 1 calc R U . . . H15C H 0.5411 0.7509 1.0123 0.083 Uiso 1 1 calc R U . . . C16 C 0.118(4) 0.4694(10) 0.3488(15) 0.041(5) Uani 1 1 d . . . . . C17 C 0.217(4) 0.4176(9) 0.3080(18) 0.043(5) Uani 1 1 d . . . . . H17 H 0.0642 0.4004 0.2663 0.052 Uiso 1 1 calc R U . . . C18 C 0.323(4) 0.3773(10) 0.3870(16) 0.042(2) Uani 1 1 d . . . . . H18A H 0.4207 0.3478 0.3610 0.050 Uiso 1 1 calc R U . . . H18B H 0.4505 0.3963 0.4350 0.050 Uiso 1 1 calc R U . . . C19 C 0.103(4) 0.3539(9) 0.4315(15) 0.039(5) Uani 1 1 d . . . . . H19A H -0.0041 0.3296 0.3860 0.047 Uiso 1 1 calc R U . . . H19B H -0.0140 0.3836 0.4459 0.047 Uiso 1 1 calc R U . . . C20 C 0.434(6) 0.2667(11) 0.503(2) 0.060(7) Uani 1 1 d . . . . . H20A H 0.3584 0.2513 0.4425 0.090 Uiso 1 1 calc R U . . . H20B H 0.4599 0.2380 0.5502 0.090 Uiso 1 1 calc R U . . . H20C H 0.6064 0.2835 0.4985 0.090 Uiso 1 1 calc R U . . . Ag1 Ag 0.4999(4) 0.38136(7) 0.63749(14) 0.0565(6) Uani 1 1 d . . . . . Ag2 Ag 0.9372(5) 0.63887(8) 0.85407(16) 0.0690(7) Uani 1 1 d . . . . . N1 N 0.516(3) 0.4852(8) 0.9902(13) 0.039(4) Uani 1 1 d . . . . . H1A H 0.5486 0.5142 1.0290 0.059 Uiso 1 1 calc R U . . . H1B H 0.4841 0.4556 1.0239 0.059 Uiso 1 1 calc R U . . . H1C H 0.3719 0.4921 0.9463 0.059 Uiso 1 1 calc R U . . . N2 N -0.264(3) 0.5237(8) 0.5183(12) 0.037(4) Uani 1 1 d . . . . . H2A H -0.3602 0.5044 0.5548 0.056 Uiso 1 1 calc R U . . . H2B H -0.2626 0.5059 0.4635 0.056 Uiso 1 1 calc R U . . . H2C H -0.3394 0.5569 0.5067 0.056 Uiso 1 1 calc R U . . . N3 N 1.409(3) 0.5877(7) 1.2493(15) 0.046(5) Uani 1 1 d . . . . . H3C H 1.5023 0.5660 1.2152 0.068 Uiso 1 1 calc R U . . . H3D H 1.3958 0.5714 1.3045 0.068 Uiso 1 1 calc R U . . . H3E H 1.4963 0.6198 1.2604 0.068 Uiso 1 1 calc R U . . . N4 N 0.435(3) 0.4294(8) 0.2518(13) 0.042(4) Uani 1 1 d . . . . . H4C H 0.3651 0.4470 0.1985 0.063 Uiso 1 1 calc R U . . . H4D H 0.5102 0.3978 0.2372 0.063 Uiso 1 1 calc R U . . . H4E H 0.5607 0.4506 0.2859 0.063 Uiso 1 1 calc R U . . . N5 N -0.062(4) 0.6869(9) 0.3500(15) 0.049(4) Uani 1 1 d . U . . . N6 N -0.121(4) 0.3207(9) 0.1702(17) 0.051(5) Uani 1 1 d . . . . . O1 O 0.699(3) 0.5682(7) 0.9090(14) 0.054(4) Uani 1 1 d . . . . . O2 O 1.068(3) 0.5274(7) 0.8790(13) 0.051(4) Uani 1 1 d . . . . . O3 O -0.035(3) 0.4374(7) 0.6004(14) 0.054(4) Uani 1 1 d . . . . . O4 O 0.375(3) 0.4721(6) 0.6172(12) 0.044(4) Uani 1 1 d . . . . . O5 O 1.167(3) 0.5100(6) 1.1351(11) 0.040(4) Uani 1 1 d . . . . . O6 O 0.767(3) 0.5424(7) 1.1471(11) 0.048(4) Uani 1 1 d . . . . . O7 O 0.290(3) 0.5072(7) 0.3675(12) 0.047(4) Uani 1 1 d . . . . . O8 O -0.116(3) 0.4707(7) 0.3597(11) 0.045(4) Uani 1 1 d . . . . . O9 O -0.021(4) 0.6643(9) 0.4299(17) 0.077(6) Uani 1 1 d . U . . . O10 O 0.135(4) 0.7035(9) 0.3219(15) 0.068(5) Uani 1 1 d . U . . . O11 O -0.283(4) 0.6852(9) 0.3062(19) 0.078(6) Uani 1 1 d . U . . . O12 O -0.130(4) 0.3439(10) 0.0932(17) 0.076(6) Uani 1 1 d . . . . . O13 O -0.307(3) 0.3257(7) 0.2142(13) 0.050(4) Uani 1 1 d . . . . . O14 O 0.072(4) 0.2893(9) 0.1997(15) 0.073(6) Uani 1 1 d . . . . . O15 O -0.493(3) 0.6257(7) 0.4826(15) 0.067(5) Uani 1 1 d D . . . . H15D H -0.6324 0.6449 0.4601 0.100 Uiso 1 1 d D U . . . H15E H -0.3597 0.6442 0.4677 0.100 Uiso 1 1 d D U . . . O16 O 0.347(3) 0.3814(7) 0.0433(12) 0.054(4) Uani 1 1 d D . . . . H16A H 0.2309 0.3608 0.0643 0.082 Uiso 1 1 d D U . . . H16B H 0.4969 0.3642 0.0576 0.082 Uiso 1 1 d D U . . . S1 S 0.8725(13) 0.3521(3) 0.7554(5) 0.0553(16) Uani 1 1 d . . . . . S2 S 0.3167(12) 0.6448(3) 0.7634(4) 0.0497(14) Uani 1 1 d . . . . . S3 S 0.9237(10) 0.7068(2) 0.9844(4) 0.0415(12) Uani 1 1 d . . . . . S4 S 0.2123(11) 0.3166(3) 0.5363(4) 0.0465(13) Uani 1 1 d . . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.037(12) 0.039(13) 0.056(14) 0.005(11) -0.002(10) -0.009(10) C2 0.041(11) 0.031(11) 0.049(13) -0.005(10) 0.001(10) -0.010(9) C3 0.039(5) 0.038(5) 0.050(6) 0.013(5) 0.010(4) -0.001(4) C4 0.039(13) 0.09(2) 0.054(15) 0.009(14) -0.005(11) -0.006(12) C5 0.14(3) 0.07(2) 0.07(2) 0.012(18) 0.01(2) 0.03(2) C6 0.022(10) 0.051(14) 0.052(13) -0.016(11) 0.010(9) 0.009(9) C7 0.026(9) 0.047(12) 0.047(11) -0.005(9) 0.013(8) -0.011(8) C8 0.039(5) 0.038(5) 0.050(6) 0.013(5) 0.010(4) -0.001(4) C9 0.040(10) 0.037(11) 0.041(11) -0.007(9) 0.001(9) 0.010(9) C10 0.15(4) 0.052(19) 0.07(2) 0.014(16) 0.03(2) 0.02(2) C11 0.032(11) 0.041(12) 0.038(11) -0.002(9) 0.010(9) -0.009(9) C12 0.038(10) 0.021(9) 0.041(10) 0.000(7) 0.018(8) 0.001(8) C13 0.039(5) 0.038(5) 0.050(6) 0.013(5) 0.010(4) -0.001(4) C14 0.039(10) 0.049(13) 0.047(12) 0.006(9) 0.015(9) -0.001(9) C15 0.048(13) 0.068(17) 0.054(15) 0.005(13) 0.021(11) 0.019(12) C16 0.030(11) 0.057(15) 0.036(11) -0.014(10) 0.006(8) -0.006(10) C17 0.029(10) 0.033(12) 0.068(15) 0.006(11) 0.003(10) -0.007(9) C18 0.039(5) 0.038(5) 0.050(6) 0.013(5) 0.010(4) -0.001(4) C19 0.040(11) 0.037(11) 0.037(11) 0.002(9) -0.003(9) 0.003(9) C20 0.076(18) 0.051(16) 0.052(15) -0.016(12) 0.010(13) 0.010(13) Ag1 0.0643(11) 0.0443(11) 0.0577(11) -0.0030(10) -0.0007(9) 0.0091(10) Ag2 0.1102(18) 0.0385(11) 0.0691(14) -0.0026(10) 0.0481(13) -0.0090(12) N1 0.034(9) 0.047(11) 0.036(9) -0.003(8) 0.003(7) 0.004(8) N2 0.033(9) 0.037(10) 0.040(10) -0.003(8) 0.000(7) -0.003(7) N3 0.036(9) 0.027(9) 0.075(14) -0.016(9) 0.015(9) -0.002(7) N4 0.032(9) 0.048(11) 0.046(11) -0.012(9) 0.006(8) 0.009(8) N5 0.037(8) 0.053(12) 0.060(11) -0.014(9) 0.010(8) -0.001(8) N6 0.027(9) 0.052(13) 0.074(15) -0.013(11) 0.006(9) 0.002(9) O1 0.045(9) 0.038(9) 0.084(13) 0.002(9) 0.023(9) -0.002(8) O2 0.039(9) 0.047(10) 0.069(11) -0.001(9) 0.020(8) -0.007(7) O3 0.031(8) 0.044(10) 0.089(13) -0.002(9) 0.019(8) -0.003(7) O4 0.042(8) 0.025(8) 0.067(11) 0.004(7) 0.011(7) 0.009(6) O5 0.037(7) 0.034(8) 0.049(9) -0.016(7) 0.004(7) 0.004(7) O6 0.035(8) 0.062(11) 0.051(9) -0.017(8) 0.023(7) -0.012(7) O7 0.044(9) 0.049(10) 0.051(10) -0.003(8) 0.014(7) -0.005(7) O8 0.025(7) 0.055(10) 0.057(10) -0.006(8) 0.007(6) 0.002(6) O9 0.076(12) 0.060(12) 0.100(14) 0.027(11) 0.033(10) 0.016(10) O10 0.054(9) 0.074(13) 0.076(12) 0.002(10) 0.013(9) -0.025(9) O11 0.031(7) 0.077(14) 0.128(17) -0.013(13) 0.017(8) -0.001(9) O12 0.068(12) 0.077(14) 0.082(15) 0.026(12) 0.012(10) 0.002(10) O13 0.047(9) 0.044(10) 0.061(10) -0.004(8) 0.015(8) 0.009(7) O14 0.070(13) 0.085(15) 0.070(13) 0.000(11) 0.028(10) 0.024(11) O15 0.057(10) 0.052(12) 0.095(15) 0.012(10) 0.022(10) 0.009(8) O16 0.052(8) 0.038(9) 0.073(11) 0.019(9) 0.005(8) -0.005(8) S1 0.056(4) 0.060(4) 0.050(4) -0.002(3) 0.008(3) 0.022(3) S2 0.056(3) 0.044(3) 0.050(3) -0.003(3) 0.010(3) -0.009(3) S3 0.033(3) 0.037(3) 0.056(3) 0.000(3) 0.010(2) -0.001(2) S4 0.041(3) 0.044(3) 0.055(3) -0.002(3) 0.009(2) -0.003(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 O1 1.23(3) . ? C1 O2 1.24(3) . ? C1 C2 1.56(3) . ? C2 N1 1.49(3) . ? C2 C3 1.56(3) . ? C2 H2 1.0000 . ? C3 C4 1.44(4) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 S1 1.85(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 S1 1.82(4) . ? C5 H5A 0.9800 . ? C5 H5B 0.9800 . ? C5 H5C 0.9800 . ? C6 O3 1.20(3) . ? C6 O4 1.27(3) . ? C6 C7 1.56(3) . ? C7 N2 1.48(3) . ? C7 C8 1.49(3) . ? C7 H7 1.0000 . ? C8 C9 1.56(3) . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 S2 1.82(2) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 S2 1.77(3) . ? C10 H10A 0.9800 . ? C10 H10B 0.9800 . ? C10 H10C 0.9800 . ? C11 O5 1.18(3) . ? C11 O6 1.25(3) . ? C11 C12 1.58(3) . ? C12 N3 1.49(3) . ? C12 C13 1.54(3) . ? C12 H12 1.0000 . ? C13 C14 1.45(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 S3 1.83(2) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 S3 1.80(2) . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 O8 1.23(3) . ? C16 O7 1.28(3) . ? C16 C17 1.53(3) . ? C17 N4 1.50(3) . ? C17 C18 1.55(3) . ? C17 H17 1.0000 . ? C18 C19 1.49(3) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C19 S4 1.79(2) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 S4 1.79(3) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? Ag1 O4 2.339(14) . ? Ag1 S1 2.454(7) . ? Ag1 S4 2.487(6) . ? Ag2 O1 2.336(16) . ? Ag2 S2 2.503(6) 1_655 ? Ag2 S3 2.538(6) . ? N1 H1A 0.9100 . ? N1 H1B 0.9100 . ? N1 H1C 0.9100 . ? N2 H2A 0.9100 . ? N2 H2B 0.9100 . ? N2 H2C 0.9100 . ? N3 H3C 0.9100 . ? N3 H3D 0.9100 . ? N3 H3E 0.9100 . ? N4 H4C 0.9100 . ? N4 H4D 0.9100 . ? N4 H4E 0.9100 . ? N5 O11 1.20(3) . ? N5 O10 1.21(3) . ? N5 O9 1.27(3) . ? N6 O13 1.23(3) . ? N6 O12 1.25(3) . ? N6 O14 1.27(3) . ? O15 H15D 0.87 . ? O15 H15E 0.87 . ? O16 H16A 0.87 . ? O16 H16B 0.87 . ? S2 Ag2 2.503(6) 1_455 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 C1 O2 130(2) . . ? O1 C1 C2 115(2) . . ? O2 C1 C2 115(2) . . ? N1 C2 C3 111.7(17) . . ? N1 C2 C1 109.4(19) . . ? C3 C2 C1 110.8(19) . . ? N1 C2 H2 108.3 . . ? C3 C2 H2 108.3 . . ? C1 C2 H2 108.3 . . ? C4 C3 C2 113(2) . . ? C4 C3 H3A 109.0 . . ? C2 C3 H3A 109.0 . . ? C4 C3 H3B 109.0 . . ? C2 C3 H3B 109.0 . . ? H3A C3 H3B 107.8 . . ? C3 C4 S1 114.7(18) . . ? C3 C4 H4A 108.6 . . ? S1 C4 H4A 108.6 . . ? C3 C4 H4B 108.6 . . ? S1 C4 H4B 108.6 . . ? H4A C4 H4B 107.6 . . ? S1 C5 H5A 109.5 . . ? S1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? S1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? O3 C6 O4 129(2) . . ? O3 C6 C7 117.7(17) . . ? O4 C6 C7 113(2) . . ? N2 C7 C8 108.1(17) . . ? N2 C7 C6 107.6(17) . . ? C8 C7 C6 117.4(19) . . ? N2 C7 H7 107.8 . . ? C8 C7 H7 107.8 . . ? C6 C7 H7 107.8 . . ? C7 C8 C9 111.6(18) . . ? C7 C8 H8A 109.3 . . ? C9 C8 H8A 109.3 . . ? C7 C8 H8B 109.3 . . ? C9 C8 H8B 109.3 . . ? H8A C8 H8B 108.0 . . ? C8 C9 S2 113.5(16) . . ? C8 C9 H9A 108.9 . . ? S2 C9 H9A 108.9 . . ? C8 C9 H9B 108.9 . . ? S2 C9 H9B 108.9 . . ? H9A C9 H9B 107.7 . . ? S2 C10 H10A 109.5 . . ? S2 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? S2 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? O5 C11 O6 131(2) . . ? O5 C11 C12 116.2(17) . . ? O6 C11 C12 111.5(19) . . ? N3 C12 C13 109.2(16) . . ? N3 C12 C11 108.5(16) . . ? C13 C12 C11 115.0(18) . . ? N3 C12 H12 108.0 . . ? C13 C12 H12 108.0 . . ? C11 C12 H12 108.0 . . ? C14 C13 C12 111.7(17) . . ? C14 C13 H13A 109.3 . . ? C12 C13 H13A 109.3 . . ? C14 C13 H13B 109.3 . . ? C12 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? C13 C14 S3 109.1(15) . . ? C13 C14 H14A 109.9 . . ? S3 C14 H14A 109.9 . . ? C13 C14 H14B 109.9 . . ? S3 C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? S3 C15 H15A 109.5 . . ? S3 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? S3 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O8 C16 O7 127(2) . . ? O8 C16 C17 117.1(19) . . ? O7 C16 C17 116.2(18) . . ? N4 C17 C16 111.1(17) . . ? N4 C17 C18 108.9(17) . . ? C16 C17 C18 110(2) . . ? N4 C17 H17 108.8 . . ? C16 C17 H17 108.8 . . ? C18 C17 H17 108.8 . . ? C19 C18 C17 111.7(17) . . ? C19 C18 H18A 109.3 . . ? C17 C18 H18A 109.3 . . ? C19 C18 H18B 109.3 . . ? C17 C18 H18B 109.3 . . ? H18A C18 H18B 107.9 . . ? C18 C19 S4 114.5(15) . . ? C18 C19 H19A 108.6 . . ? S4 C19 H19A 108.6 . . ? C18 C19 H19B 108.6 . . ? S4 C19 H19B 108.6 . . ? H19A C19 H19B 107.6 . . ? S4 C20 H20A 109.5 . . ? S4 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? S4 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? O4 Ag1 S1 122.4(4) . . ? O4 Ag1 S4 114.9(4) . . ? S1 Ag1 S4 122.6(2) . . ? O1 Ag2 S2 134.9(5) . 1_655 ? O1 Ag2 S3 99.5(5) . . ? S2 Ag2 S3 117.8(2) 1_655 . ? C2 N1 H1A 109.5 . . ? C2 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C2 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? C7 N2 H2A 109.5 . . ? C7 N2 H2B 109.5 . . ? H2A N2 H2B 109.5 . . ? C7 N2 H2C 109.5 . . ? H2A N2 H2C 109.5 . . ? H2B N2 H2C 109.5 . . ? C12 N3 H3C 109.5 . . ? C12 N3 H3D 109.5 . . ? H3C N3 H3D 109.5 . . ? C12 N3 H3E 109.5 . . ? H3C N3 H3E 109.5 . . ? H3D N3 H3E 109.5 . . ? C17 N4 H4C 109.5 . . ? C17 N4 H4D 109.5 . . ? H4C N4 H4D 109.5 . . ? C17 N4 H4E 109.5 . . ? H4C N4 H4E 109.5 . . ? H4D N4 H4E 109.5 . . ? O11 N5 O10 126(3) . . ? O11 N5 O9 118(2) . . ? O10 N5 O9 116(2) . . ? O13 N6 O12 120(2) . . ? O13 N6 O14 120(2) . . ? O12 N6 O14 120(2) . . ? C1 O1 Ag2 102.2(14) . . ? C6 O4 Ag1 106.6(15) . . ? H15D O15 H15E 104.0 . . ? H16A O16 H16B 104.0 . . ? C5 S1 C4 102.5(16) . . ? C5 S1 Ag1 102.8(14) . . ? C4 S1 Ag1 103.1(9) . . ? C10 S2 C9 99.8(14) . . ? C10 S2 Ag2 109.1(15) . 1_455 ? C9 S2 Ag2 105.6(8) . 1_455 ? C15 S3 C14 100.8(11) . . ? C15 S3 Ag2 101.9(10) . . ? C14 S3 Ag2 101.3(8) . . ? C20 S4 C19 104.5(13) . . ? C20 S4 Ag1 105.4(10) . . ? C19 S4 Ag1 104.2(8) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 C1 C2 N1 -9(3) . . . . ? O2 C1 C2 N1 169.1(19) . . . . ? O1 C1 C2 C3 114(2) . . . . ? O2 C1 C2 C3 -67(3) . . . . ? N1 C2 C3 C4 -164(2) . . . . ? C1 C2 C3 C4 74(3) . . . . ? C2 C3 C4 S1 169.4(16) . . . . ? O3 C6 C7 N2 -23(3) . . . . ? O4 C6 C7 N2 164.9(18) . . . . ? O3 C6 C7 C8 100(2) . . . . ? O4 C6 C7 C8 -73(2) . . . . ? N2 C7 C8 C9 -174.3(18) . . . . ? C6 C7 C8 C9 64(2) . . . . ? C7 C8 C9 S2 163.5(16) . . . . ? O5 C11 C12 N3 -36(3) . . . . ? O6 C11 C12 N3 153.7(18) . . . . ? O5 C11 C12 C13 87(2) . . . . ? O6 C11 C12 C13 -84(2) . . . . ? N3 C12 C13 C14 -165.6(19) . . . . ? C11 C12 C13 C14 72(3) . . . . ? C12 C13 C14 S3 -173.3(16) . . . . ? O8 C16 C17 N4 149(2) . . . . ? O7 C16 C17 N4 -30(3) . . . . ? O8 C16 C17 C18 -90(2) . . . . ? O7 C16 C17 C18 91(2) . . . . ? N4 C17 C18 C19 -166.7(19) . . . . ? C16 C17 C18 C19 71(2) . . . . ? C17 C18 C19 S4 -169.4(16) . . . . ? O2 C1 O1 Ag2 -1(3) . . . . ? C2 C1 O1 Ag2 176.9(16) . . . . ? O3 C6 O4 Ag1 15(3) . . . . ? C7 C6 O4 Ag1 -173.3(14) . . . . ? C3 C4 S1 C5 -58(2) . . . . ? C3 C4 S1 Ag1 48(2) . . . . ? C8 C9 S2 C10 -68(2) . . . . ? C8 C9 S2 Ag2 45.0(18) . . . 1_455 ? C13 C14 S3 C15 -174.7(19) . . . . ? C13 C14 S3 Ag2 80.7(18) . . . . ? C18 C19 S4 C20 -55(2) . . . . ? C18 C19 S4 Ag1 54.9(19) . . . . ? 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 O6 0.91 2.01 2.81(2) 145.1 . N1 H1B O16 0.91 2.00 2.85(3) 155.8 1_556 N1 H1C O2 0.91 1.90 2.78(2) 161.0 1_455 N2 H2A O4 0.91 1.91 2.81(2) 167.7 1_455 N2 H2B O7 0.91 2.47 2.92(2) 110.7 1_455 N2 H2B O8 0.91 1.98 2.85(2) 158.7 . N2 H2C O15 0.91 1.88 2.79(3) 179.5 . N3 H3C O6 0.91 1.88 2.76(2) 160.4 1_655 N3 H3D O7 0.91 1.95 2.76(3) 147.1 1_656 N3 H3E O11 0.91 2.02 2.92(3) 170.1 1_756 N4 H4C O5 0.91 2.00 2.82(3) 149.9 1_454 N4 H4D O13 0.91 2.06 2.97(2) 175.8 1_655 N4 H4E O8 0.91 1.88 2.75(2) 159.7 1_655 O15 H15D O9 0.87 2.01 2.84(3) 157.4 1_455 O15 H15D O10 0.87 2.60 3.37(3) 146.6 1_455 O15 H15E O9 0.87 1.95 2.79(3) 163.0 . O16 H16A O12 0.87 1.99 2.79(3) 154 . O16 H16B N6 0.87 2.57 3.38(2) 155 1_655 O16 H16B O12 0.87 1.95 2.80(3) 165.5 1_655 O16 H16B O13 0.87 2.521 3.12(2) 127.5 1_655 _refine_diff_density_max 1.651 _refine_diff_density_min -1.109 _refine_diff_density_rms 0.192 _shelx_res_file ; shelx.res created by SHELXL-2014/7 TITL Ag Methionine in D2O in P2(1) CELL 0.71073 5.0810 24.7309 14.5097 90.000 99.007 90.000 ZERR 2.00 0.0003 0.0012 0.0010 0.000 0.005 0.000 LATT -1 SYMM - X, 1/2 + Y, - Z SFAC C H AG N O S UNIT 40 96 4 12 32 8 MERG 0 DELU 0.010 0.010 C12 C13 C14 SIMU 0.040 0.080 1.700 C12 C13 C14 DELU 0.010 0.010 C7 C8 C9 SIMU 0.040 0.080 1.700 C7 C8 C9 DELU 0.010 0.010 N5 O9 O10 O11 SIMU 0.040 0.080 1.700 N5 O9 O10 O11 EADP C3 C8 C13 C18 DFIX 0.910 0.020 O15 H15D DFIX 0.910 0.020 O15 H15E DFIX 0.910 0.020 H16B O16 DFIX 0.910 0.020 H16A O16 EQIV $1 x+1, y, z+1 EQIV $2 -x+1, y-1/2, -z+1 EQIV $3 x+1, y, z EQIV $4 -x, y+1/2, -z+1 EQIV $5 -x+1, y+1/2, -z+1 EQIV $6 x, y, z+1 EQIV $7 x-1, y, z EQIV $8 x+2, y, z+1 EQIV $9 x-1, y, z-1 HTAB N1 O6 HTAB N1 O16_$6 HTAB N1 O2_$7 HTAB N2 O4_$7 HTAB N2 O7_$7 HTAB N2 O8 HTAB N2 O15 HTAB N3 O6_$3 HTAB N3 O7_$1 HTAB N3 O11_$8 HTAB N4 O5_$9 HTAB N4 O13_$3 HTAB N4 O8_$3 HTAB O15 O9_$7 HTAB O15 O10_$7 HTAB O15 O9 HTAB O16 O12 HTAB O16 N6_$3 HTAB O16 O12_$3 HTAB O16 O13_$3 FMAP 2 PLAN 5 SIZE 0.030 0.180 0.480 ACTA BOND $H CONF LIST 4 L.S. 90 TEMP -73.00 WGHT 0.119300 20.404600 FVAR 10.00476 C1 1 0.848660 0.529624 0.905726 11.00000 0.03724 0.03943 = 0.05645 0.00467 -0.00162 -0.00903 C2 1 0.752792 0.475086 0.943745 11.00000 0.04133 0.03075 = 0.04897 -0.00473 0.00124 -0.01003 AFIX 13 H2 2 0.899372 0.460580 0.991385 11.00000 -1.20000 AFIX 0 C3 1 0.691409 0.432674 0.863718 11.00000 0.03884 0.03751 = 0.05025 0.01252 0.00962 -0.00116 AFIX 23 H3A 2 0.587729 0.402574 0.885192 11.00000 -1.20000 H3B 2 0.579801 0.449842 0.809547 11.00000 -1.20000 AFIX 0 C4 1 0.929132 0.411077 0.834321 11.00000 0.03900 0.08566 = 0.05446 0.00866 -0.00491 -0.00552 AFIX 23 H4A 2 1.055333 0.400475 0.890470 11.00000 -1.20000 H4B 2 1.014621 0.440067 0.802407 11.00000 -1.20000 AFIX 0 C5 1 0.715790 0.303688 0.824403 11.00000 0.13770 0.06956 = 0.07400 0.01215 0.01158 0.03324 AFIX 137 H5A 2 0.825042 0.299699 0.885960 11.00000 -1.50000 H5B 2 0.699861 0.268610 0.792596 11.00000 -1.50000 H5C 2 0.538164 0.316731 0.831796 11.00000 -1.50000 AFIX 0 C6 1 0.122898 0.472644 0.594384 11.00000 0.02171 0.05076 = 0.05243 -0.01572 0.01045 0.00866 C7 1 0.012260 0.530078 0.567162 11.00000 0.02620 0.04662 = 0.04683 -0.00456 0.01257 -0.01074 AFIX 13 H7 2 0.120748 0.545723 0.521818 11.00000 -1.20000 AFIX 0 C8 1 0.009682 0.570024 0.643994 11.00000 0.03884 0.03751 = 0.05025 0.01252 0.00962 -0.00116 AFIX 23 H8A 2 -0.094153 0.555123 0.690461 11.00000 -1.20000 H8B 2 -0.079314 0.603590 0.618264 11.00000 -1.20000 AFIX 0 C9 1 0.298177 0.583742 0.693279 11.00000 0.03953 0.03722 = 0.04094 -0.00655 0.00106 0.00972 AFIX 23 H9A 2 0.415061 0.587958 0.645194 11.00000 -1.20000 H9B 2 0.366938 0.553024 0.733772 11.00000 -1.20000 AFIX 0 C10 1 0.240332 0.693498 0.674158 11.00000 0.15289 0.05202 = 0.07229 0.01450 0.03164 0.01685 AFIX 137 H10A 2 0.404167 0.711859 0.663864 11.00000 -1.50000 H10B 2 0.115397 0.720065 0.692689 11.00000 -1.50000 H10C 2 0.159075 0.675587 0.616412 11.00000 -1.50000 AFIX 0 C11 1 1.015834 0.541602 1.158505 11.00000 0.03154 0.04059 = 0.03804 -0.00207 0.00962 -0.00901 C12 1 1.137649 0.597531 1.196338 11.00000 0.03752 0.02064 = 0.04084 -0.00008 0.01755 0.00106 AFIX 13 H12 2 1.023970 0.612218 1.240874 11.00000 -1.20000 AFIX 0 C13 1 1.154161 0.640831 1.120707 11.00000 0.03884 0.03751 = 0.05025 0.01252 0.00962 -0.00116 AFIX 23 H13A 2 1.269347 0.670891 1.148075 11.00000 -1.20000 H13B 2 1.236795 0.624774 1.069654 11.00000 -1.20000 AFIX 0 C14 1 0.892707 0.661959 1.082723 11.00000 0.03904 0.04875 = 0.04739 0.00630 0.01476 -0.00138 AFIX 23 H14A 2 0.818280 0.682233 1.131545 11.00000 -1.20000 H14B 2 0.770264 0.631761 1.061424 11.00000 -1.20000 AFIX 0 C15 1 0.588602 0.732317 0.957545 11.00000 0.04816 0.06753 = 0.05387 0.00546 0.02126 0.01865 AFIX 137 H15A 2 0.465375 0.702190 0.940367 11.00000 -1.50000 H15B 2 0.576936 0.757796 0.905335 11.00000 -1.50000 H15C 2 0.541096 0.750858 1.012326 11.00000 -1.50000 AFIX 0 C16 1 0.118268 0.469376 0.348757 11.00000 0.02952 0.05678 = 0.03569 -0.01381 0.00601 -0.00647 C17 1 0.216642 0.417585 0.308013 11.00000 0.02864 0.03251 = 0.06765 0.00563 0.00277 -0.00707 AFIX 13 H17 2 0.064232 0.400369 0.266338 11.00000 -1.20000 AFIX 0 C18 1 0.323416 0.377320 0.387033 11.00000 0.03884 0.03751 = 0.05025 0.01252 0.00962 -0.00116 AFIX 23 H18A 2 0.420721 0.347752 0.361017 11.00000 -1.20000 H18B 2 0.450467 0.396263 0.435011 11.00000 -1.20000 AFIX 0 C19 1 0.103457 0.353863 0.431474 11.00000 0.04025 0.03734 = 0.03704 0.00154 -0.00261 0.00320 AFIX 23 H19A 2 -0.004089 0.329644 0.385983 11.00000 -1.20000 H19B 2 -0.014033 0.383602 0.445887 11.00000 -1.20000 AFIX 0 C20 1 0.434322 0.266731 0.503116 11.00000 0.07598 0.05101 = 0.05222 -0.01639 0.00963 0.00969 AFIX 137 H20A 2 0.358426 0.251320 0.442538 11.00000 -1.50000 H20B 2 0.459865 0.237989 0.550166 11.00000 -1.50000 H20C 2 0.606413 0.283541 0.498470 11.00000 -1.50000 AFIX 0 AG1 3 0.499912 0.381362 0.637489 11.00000 0.06434 0.04430 = 0.05771 -0.00302 -0.00073 0.00907 AG2 3 0.937195 0.638873 0.854066 11.00000 0.11023 0.03847 = 0.06913 -0.00258 0.04815 -0.00898 N1 4 0.516373 0.485245 0.990237 11.00000 0.03388 0.04723 = 0.03607 -0.00255 0.00317 0.00433 AFIX 137 H1A 2 0.548578 0.514229 1.029000 11.00000 -1.50000 H1B 2 0.484053 0.455593 1.023878 11.00000 -1.50000 H1C 2 0.371929 0.492125 0.946262 11.00000 -1.50000 AFIX 0 N2 4 -0.264042 0.523699 0.518331 11.00000 0.03292 0.03707 = 0.03988 -0.00288 -0.00029 -0.00281 AFIX 137 H2A 2 -0.360184 0.504362 0.554789 11.00000 -1.50000 H2B 2 -0.262565 0.505938 0.463488 11.00000 -1.50000 H2C 2 -0.339420 0.556872 0.506664 11.00000 -1.50000 AFIX 0 N3 4 1.409498 0.587719 1.249277 11.00000 0.03616 0.02725 = 0.07524 -0.01621 0.01517 -0.00210 AFIX 137 H3C 2 1.502293 0.565983 1.215238 11.00000 -1.50000 H3D 2 1.395769 0.571376 1.304514 11.00000 -1.50000 H3E 2 1.496294 0.619811 1.260376 11.00000 -1.50000 AFIX 0 N4 4 0.434681 0.429424 0.251846 11.00000 0.03155 0.04781 = 0.04597 -0.01210 0.00603 0.00932 AFIX 137 H4C 2 0.365123 0.447029 0.198493 11.00000 -1.50000 H4D 2 0.510212 0.397846 0.237168 11.00000 -1.50000 H4E 2 0.560694 0.450563 0.285879 11.00000 -1.50000 AFIX 0 N5 4 -0.061741 0.686861 0.349983 11.00000 0.03687 0.05264 = 0.05959 -0.01365 0.00972 -0.00068 N6 4 -0.120656 0.320654 0.170181 11.00000 0.02693 0.05214 = 0.07425 -0.01253 0.00565 0.00156 O1 5 0.699077 0.568195 0.908963 11.00000 0.04519 0.03756 = 0.08401 0.00241 0.02303 -0.00238 O2 5 1.067958 0.527389 0.878991 11.00000 0.03933 0.04718 = 0.06890 -0.00062 0.02004 -0.00668 O3 5 -0.034532 0.437363 0.600395 11.00000 0.03067 0.04392 = 0.08919 -0.00209 0.01926 -0.00307 O4 5 0.374675 0.472110 0.617204 11.00000 0.04217 0.02491 = 0.06685 0.00368 0.01087 0.00943 O5 5 1.167260 0.509975 1.135076 11.00000 0.03741 0.03352 = 0.04942 -0.01647 0.00422 0.00397 O6 5 0.766699 0.542371 1.147071 11.00000 0.03544 0.06197 = 0.05137 -0.01704 0.02315 -0.01245 O7 5 0.289982 0.507202 0.367455 11.00000 0.04443 0.04858 = 0.05098 -0.00264 0.01380 -0.00502 O8 5 -0.116033 0.470663 0.359744 11.00000 0.02465 0.05452 = 0.05677 -0.00618 0.00659 0.00242 O9 5 -0.021411 0.664288 0.429914 11.00000 0.07628 0.05980 = 0.10031 0.02676 0.03322 0.01576 O10 5 0.134855 0.703468 0.321877 11.00000 0.05394 0.07383 = 0.07591 0.00211 0.01262 -0.02547 O11 5 -0.283418 0.685221 0.306242 11.00000 0.03128 0.07687 = 0.12787 -0.01282 0.01697 -0.00130 O12 5 -0.129846 0.343935 0.093206 11.00000 0.06831 0.07725 = 0.08228 0.02604 0.01190 0.00218 O13 5 -0.307006 0.325722 0.214219 11.00000 0.04734 0.04438 = 0.06060 -0.00353 0.01492 0.00862 O14 5 0.072061 0.289293 0.199682 11.00000 0.07003 0.08527 = 0.06954 0.00045 0.02763 0.02400 O15 5 -0.492548 0.625715 0.482640 11.00000 0.05661 0.05165 = 0.09506 0.01228 0.02210 0.00931 H15D 2 9.367640 10.644870 10.460120 11.00000 -1.50000 H15E 2 9.640330 10.644220 10.467720 11.00000 -1.50000 O16 5 0.347317 0.381373 0.043306 11.00000 0.05161 0.03762 = 0.07272 0.01898 0.00542 -0.00531 H16A 2 10.230860 10.360810 10.064310 11.00000 -1.50000 H16B 2 10.496860 10.364182 10.057590 11.00000 -1.50000 S1 6 0.872513 0.352067 0.755353 11.00000 0.05586 0.05957 = 0.05049 -0.00176 0.00793 0.02183 S2 6 0.316678 0.644801 0.763397 11.00000 0.05609 0.04388 = 0.04963 -0.00340 0.01011 -0.00942 S3 6 0.923666 0.706793 0.984376 11.00000 0.03348 0.03655 = 0.05569 -0.00048 0.01042 -0.00087 S4 6 0.212344 0.316585 0.536252 11.00000 0.04140 0.04359 = 0.05500 -0.00174 0.00893 -0.00293 HKLF 5 REM shelxt_a.res in P2(1) REM R1 = 0.0864 for 4756 Fo > 4sig(Fo) and 0.1164 for all 6406 data REM 423 parameters refined using 59 restraints END WGHT 0.1193 20.3988 REM Highest difference peak 1.651, deepest hole -1.109, 1-sigma level 0.192 Q1 1 0.7228 0.6380 0.8538 11.00000 0.05 1.65 Q2 1 0.2879 0.3787 0.6480 11.00000 0.05 1.47 Q3 1 -0.1043 0.3961 0.3588 11.00000 0.05 1.34 Q4 1 0.7402 0.3815 0.6360 11.00000 0.05 1.17 Q5 1 0.6964 0.3914 0.7284 11.00000 0.05 1.03 ; _shelx_res_checksum 13790 _shelx_hkl_file ; 1 -29 0 9640 5365 1 0 -28 0 94693 39291 1 1 -28 0 76157 27966 1 1 -27 0 5922 5198 1 2 -27 0 10100 4312 1 0 -26 0 -2018 6470 1 1 -26 0 85161 10605 1 2 -26 0 6186 4826 1 1 -25 0 16796 4484 1 2 -25 0 11934 5496 1 3 -25 0 4732 4778 1 0 -24 0 239028 26487 1 1 -24 0 58528 8082 1 2 -24 0 56267 13078 1 3 -24 0 7301 4077 1 1 -23 0 8971 4829 1 2 -23 0 7585 4596 1 3 -23 0 5959 4014 1 0 -22 0 98653 6788 1 1 -22 0 111706 11210 1 2 -22 0 20261 5187 1 3 -22 0 22182 8343 1 4 -22 0 4292 8862 1 1 -21 0 66292 6125 1 2 -21 0 99301 27561 1 3 -21 0 36972 4249 1 4 -21 0 10498 4643 1 0 -20 0 374364 7848 1 1 -20 0 133808 8352 1 2 -20 0 144921 22479 1 3 -20 0 1283 4005 1 4 -20 0 53896 10343 1 1 -19 0 11511 6660 1 2 -19 0 61386 8164 1 3 -19 0 3742 3768 1 4 -19 0 11031 4534 1 0 -18 0 660844 27562 1 1 -18 0 414652 23349 1 2 -18 0 41650 5030 1 3 -18 0 26520 4060 1 4 -18 0 45231 5736 1 1 -17 0 62336 6346 1 2 -17 0 113119 7501 1 3 -17 0 11393 4090 1 4 -17 0 777 4534 1 0 -16 0 1062358 18513 1 1 -16 0 318907 10301 1 2 -16 0 77321 8564 1 3 -16 0 6616 3813 1 4 -16 0 107734 4262 1 5 -16 0 16872 5424 1 1 -15 0 100156 5607 1 2 -15 0 67548 5761 1 3 -15 0 109488 4355 1 4 -15 0 58471 4212 1 5 -15 0 4588 4211 1 0 -14 0 120000 8113 1 1 -14 0 666442 23437 1 2 -14 0 24868 5068 1 3 -14 0 79530 3907 1 4 -14 0 51568 4145 1 5 -14 0 11520 6350 1 1 -13 0 85619 6435 1 2 -13 0 144238 25265 1 3 -13 0 125041 8773 1 4 -13 0 32562 6239 1 5 -13 0 31120 4948 1 0 -12 0 1540952 90659 1 1 -12 0 81087 5982 1 2 -12 0 444244 6258 1 3 -12 0 25423 4268 1 4 -12 0 28939 5744 1 5 -12 0 27329 6910 1 1 -11 0 193632 13482 1 2 -11 0 211814 9354 1 3 -11 0 7263 4690 1 4 -11 0 38019 3587 1 5 -11 0 2939 3190 1 0 -10 0 68873 10064 1 1 -10 0 1484376 13474 1 2 -10 0 114661 5681 1 3 -10 0 113693 5854 1 4 -10 0 12639 6133 1 5 -10 0 35772 4740 1 1 -9 0 376370 9110 1 2 -9 0 75122 38331 1 3 -9 0 67046 4156 1 4 -9 0 15999 5527 1 5 -9 0 20399 4781 1 0 -8 0 624169 37097 1 1 -8 0 812685 96840 1 2 -8 0 646837 12427 1 3 -8 0 176281 4352 1 4 -8 0 127851 3693 1 5 -8 0 60559 5677 1 1 -7 0 9911 7833 1 2 -7 0 348670 25977 1 3 -7 0 90606 3978 1 4 -7 0 36497 3864 1 5 -7 0 6203 3321 1 0 -6 0 2476786 27103 1 1 -6 0 1677024 18513 1 2 -6 0 199554 8222 1 3 -6 0 80276 4266 1 4 -6 0 63641 3403 1 5 -6 0 33991 3100 1 1 -5 0 181650 21037 1 2 -5 0 246002 7914 1 3 -5 0 77157 4273 1 4 -5 0 44484 4260 1 5 -5 0 25105 3808 1 0 -4 0 4378275 43442 1 1 -4 0 138225 32178 1 2 -4 0 923331 8257 1 3 -4 0 42796 4240 1 4 -4 0 28690 3535 1 5 -4 0 73856 10436 1 1 -3 0 34100 9104 1 2 -3 0 463091 35299 1 3 -3 0 436082 4970 1 4 -3 0 82236 4270 1 5 -3 0 10024 4865 1 0 -2 0 307168 21959 1 1 -2 0 2302887 17405 1 2 -2 0 74996 37979 1 3 -2 0 449537 4934 1 4 -2 0 31645 5487 1 5 -2 0 635 4456 1 1 -1 0 84516 36512 1 2 -1 0 298735 7064 1 3 -1 0 78854 5690 1 4 -1 0 36378 4331 1 5 -1 0 63378 3406 1 1 0 0 1013649 51932 1 2 0 0 602560 7765 1 3 0 0 43629 7175 1 4 0 0 5685 5178 1 5 0 0 144883 6204 1 6 0 0 -8175 8316 1 1 1 0 123781 43606 1 2 1 0 314560 24143 1 3 1 0 84690 5261 1 4 1 0 47752 4672 1 5 1 0 73813 4060 1 0 2 0 310470 23897 1 1 2 0 2284607 19763 1 2 2 0 24163 10558 1 3 2 0 454398 5791 1 4 2 0 20576 5374 1 5 2 0 1413 5211 1 1 3 0 65699 35562 1 2 3 0 437595 6848 1 3 3 0 457863 5948 1 4 3 0 91521 5350 1 5 3 0 8807 6044 1 0 4 0 4560961 249176 1 1 4 0 159298 61574 1 2 4 0 959219 19228 1 3 4 0 23210 6093 1 4 4 0 30502 4207 1 5 4 0 70715 4744 1 1 5 0 145578 28528 1 2 5 0 228106 9183 1 3 5 0 82243 5481 1 4 5 0 60842 14456 1 5 5 0 27630 4675 1 0 6 0 2407073 105489 1 1 6 0 1810958 44707 1 2 6 0 172202 9709 1 3 6 0 76982 5182 1 4 6 0 64614 5515 1 5 6 0 28238 3798 1 1 7 0 8856 7908 1 2 7 0 398262 64735 1 3 7 0 82687 9487 1 4 7 0 39922 5749 1 5 7 0 3095 4594 1 0 8 0 679667 29479 1 1 8 0 791422 71181 1 2 8 0 526851 24010 1 3 8 0 156794 15671 1 4 8 0 136862 4375 1 5 8 0 48473 8590 1 1 9 0 355711 22128 1 2 9 0 89165 37595 1 3 9 0 88858 12717 1 4 9 0 5558 4235 1 5 9 0 13107 9897 1 0 10 0 62546 10960 1 1 10 0 1470429 58783 1 2 10 0 98204 6993 1 3 10 0 128754 15680 1 4 10 0 22377 4865 1 5 10 0 42061 5196 1 1 11 0 184678 15819 1 2 11 0 253923 20246 1 3 11 0 -1104 4974 1 4 11 0 34970 4882 1 5 11 0 4521 8337 1 0 12 0 1629106 15518 1 1 12 0 85530 7575 1 2 12 0 436772 6317 1 3 12 0 19630 5063 1 4 12 0 28779 4736 1 5 12 0 30068 5151 1 1 13 0 66749 7140 1 2 13 0 117155 23298 1 3 13 0 138675 5745 1 4 13 0 28432 4714 1 5 13 0 27512 5437 1 0 14 0 118150 8897 1 1 14 0 625537 42495 1 2 14 0 46971 6992 1 3 14 0 92137 6535 1 4 14 0 54230 10623 1 5 14 0 11143 4840 1 1 15 0 89444 8043 1 2 15 0 72844 5863 1 3 15 0 97946 18684 1 4 15 0 44780 5330 1 5 15 0 14329 4836 1 0 16 0 1063924 11513 1 1 16 0 314506 17975 1 2 16 0 73643 5867 1 3 16 0 12459 4604 1 4 16 0 92991 6175 1 5 16 0 15024 8198 1 1 17 0 34158 4770 1 2 17 0 142347 28733 1 3 17 0 25396 8072 1 4 17 0 5531 5713 1 0 18 0 670839 74380 1 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