#------------------------------------------------------------------------------ #$Date: 2024-11-21 03:21:30 +0200 (Thu, 21 Nov 2024) $ #$Revision: 296034 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/32/1573240.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1573240 loop_ _publ_author_name 'Nakatani, Riki' 'Sakai, Jin' 'Saha, Aishik' 'Kondo, Ayumu' 'Tomioka, Rina' 'Kawawaki, Tokuhisa' 'Das, Saikat' 'Negishi, Yuichi' _publ_section_title ; Designed construction of two new atom-precise three-dimensional and two-dimensional Ag12 cluster-assembled materials ; _journal_name_full Nanoscale _journal_paper_doi 10.1039/D4NR03992K _journal_year 2024 _chemical_formula_moiety 'C15 H14 Ag2 F3 N O2 S, 1.5[C2H5OH]' _chemical_formula_sum 'C18 H23 Ag2 F3 N O3.5 S' _chemical_formula_weight 614.17 _space_group_crystal_system trigonal _space_group_IT_number 148 _space_group_name_Hall '-R 3' _space_group_name_H-M_alt 'R -3 :H' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2024-01-15 _audit_creation_method ; Olex2 1.5 (compiled 2023.08.24 svn.re1ec1418 for OlexSys, GUI svn.r6817) ; _audit_update_record ; 2024-07-24 deposited with the CCDC. 2024-11-18 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 120 _cell_formula_units_Z 18 _cell_length_a 24.5604(4) _cell_length_b 24.5604(4) _cell_length_c 21.6065(6) _cell_measurement_reflns_used 7622 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 73.5530 _cell_measurement_theta_min 2.9010 _cell_volume 11287.2(4) _computing_cell_refinement 'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)' _computing_data_collection 'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)' _computing_data_reduction 'CrysAlisPro 1.171.43.95a (Rigaku OD, 2023)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'Hybrid Pixel Array Detector' _diffrn_detector_area_resol_mean 10.0000 _diffrn_detector_type HyPix _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.956 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w 96.00 178.00 0.50 0.33 -- 105.20 30.00 0.00 164 2 \w 30.00 55.00 0.50 0.33 -- 105.20 -45.00-120.00 50 3 \w 29.00 55.00 0.50 0.33 -- 105.20 -44.00-136.00 52 4 \w 48.00 105.00 0.50 0.33 -- 105.20 -77.00 0.00 114 5 \w 31.00 56.00 0.50 0.33 -- 105.20 -45.00 90.00 50 6 \w -17.00 63.00 0.50 0.08 -- 41.30 -99.00 94.00 160 7 \w 39.00 106.00 0.50 0.33 -- 105.20 -99.00 94.00 134 8 \w 3.00 38.00 0.50 0.08 -- -41.30 19.00 -30.00 70 9 \w -59.00 -32.00 0.50 0.33 -- -104.00 61.00 -30.00 54 10 \w -24.00 35.00 0.50 0.08 -- -41.30 19.00 90.00 118 11 \w -63.00 -37.00 0.50 0.33 -- -104.00 61.00 120.00 52 12 \w -117.00 -80.00 0.50 0.33 -- -104.00 134.00 176.00 74 13 \w -68.00 -42.00 0.50 0.33 -- -104.00 134.00 176.00 52 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Synergy R, DW system, HyPix' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0577347000 _diffrn_orient_matrix_UB_12 0.0383179000 _diffrn_orient_matrix_UB_13 -0.0416824000 _diffrn_orient_matrix_UB_21 -0.0437263000 _diffrn_orient_matrix_UB_22 -0.0088705000 _diffrn_orient_matrix_UB_23 -0.0548166000 _diffrn_orient_matrix_UB_31 0.0004783000 _diffrn_orient_matrix_UB_32 0.0609275000 _diffrn_orient_matrix_UB_33 0.0182507000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0239 _diffrn_reflns_av_unetI/netI 0.0267 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.956 _diffrn_reflns_limit_h_max 22 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_k_max 30 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 12388 _diffrn_reflns_point_group_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.956 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 74.530 _diffrn_reflns_theta_min 2.915 _diffrn_source 'Rotating-anode X-ray tube' _diffrn_source_type 'Rigaku (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 13.672 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.41227 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.43.95a (Rigaku Oxford Diffraction, 2023) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.626 _exptl_crystal_description block _exptl_crystal_F_000 5454 _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.16 _refine_diff_density_max 0.822 _refine_diff_density_min -0.951 _refine_diff_density_rms 0.121 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 220 _refine_ls_number_reflns 4922 _refine_ls_number_restraints 184 _refine_ls_restrained_S_all 1.062 _refine_ls_R_factor_all 0.0417 _refine_ls_R_factor_gt 0.0379 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0553P)^2^+89.2830P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1049 _refine_ls_wR_factor_ref 0.1076 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4397 _reflns_number_total 4922 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4nr03992k2.cif _cod_data_source_block 230111_rn_scam_90k_auto _cod_original_cell_volume 11287.2(5) _cod_original_sg_symbol_H-M 'R -3' _cod_original_formula_sum 'C18 H23 Ag2 F3 N O3.50 S' _cod_database_code 1573240 _shelx_shelxl_version_number 2018/3 _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. ; _shelx_estimated_absorpt_t_max 0.218 _shelx_estimated_absorpt_t_min 0.218 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Rigid bond restraints All non-hydrogen atoms with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 3. Uiso/Uaniso restraints and constraints All non-hydrogen atoms have similar U: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A Uanis(S1) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 4.a Aromatic/amide H refined with riding coordinates: C15(H15), C8(H8), C10(H10), C7(H7), C11(H11) 4.b Idealised Me refined as rotating group: C2(H2A,H2B,H2C), C3(H3A,H3B,H3C), C4(H4A,H4B,H4C) ; _smtbx_masks_special_details ; A solvent mask was calculated and 705 electrons were found in a volume of 4622\%A^3^ in 1 void per unit cell. This is consistent with the presence of 0.551[C2H5OH] per Unit Cell which account for 702 electrons per unit cell. ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL 230111_rn_scam_90k_auto_a.res in R-3 230111_rn_scam_90k_auto.res created by SHELXL-2018/3 at 13:41:44 on 15-Jan-2024 REM Old TITL 230111_RN_SCAM_90K_auto in R-3 REM SHELXT solution in R-3: R1 0.165, Rweak 0.008, Alpha 0.034 REM 0.000 for 0 systematic absences, Orientation as input REM Formula found by SHELXT: C108 N7 O18 I12 CELL 1.54184 24.5604 24.5604 21.6065 90 90 120 ZERR 18 0.0004 0.0004 0.0006 0 0 0 LATT 3 SYMM -Y,+X-Y,+Z SYMM +Y-X,-X,+Z SFAC C H Ag F N O S UNIT 324 414 36 54 18 63 18 DELU SIMU 0.01 0.02 2 ISOR 0.005 0.01 S1 L.S. 4 0 0 PLAN 16 SIZE 0.16 0.16 0.16 CONF list 4 MORE -1 BOND $H fmap 2 53 acta ABIN REM REM REM WGHT 0.055300 89.282997 FVAR 0.07561 AG1 3 0.399641 0.658095 0.568996 11.00000 0.02394 0.02172 = 0.04192 -0.00059 0.00011 0.01037 AG2 3 0.505989 0.733691 0.664008 11.00000 0.02143 0.04116 = 0.04697 0.00971 -0.00033 0.01093 S1 7 0.320108 0.547302 0.589701 11.00000 0.02594 0.02265 = 0.03790 -0.00119 0.00009 0.01297 O2 6 0.517443 0.653940 0.587402 11.00000 0.03199 0.03099 = 0.05316 -0.00271 0.00052 0.01663 O1 6 0.470263 0.650650 0.497225 11.00000 0.03316 0.03989 = 0.04662 -0.00372 0.00355 0.01905 F1 4 0.536178 0.580569 0.477012 11.00000 0.07348 0.07844 = 0.11462 -0.03783 0.00012 0.05172 F3 4 0.609742 0.651685 0.528247 11.00000 0.04699 0.13635 = 0.10171 -0.05200 -0.01371 0.05513 C12 1 0.811554 0.889761 0.662924 11.00000 0.02958 0.03303 = 0.04701 -0.00329 -0.00062 0.01383 C9 1 0.744453 0.853757 0.664015 11.00000 0.02629 0.03358 = 0.04357 -0.00091 0.00052 0.01045 C14 1 0.934695 0.960984 0.663311 11.00000 0.02486 0.02673 = 0.04089 -0.00099 -0.00116 0.01045 N1 5 0.612918 0.786429 0.666261 11.00000 0.02353 0.03799 = 0.05186 0.00108 -0.00126 0.01147 C15 1 0.973568 0.934795 0.663650 11.00000 0.02942 0.02236 = 0.04108 -0.00016 -0.00066 0.01123 AFIX 43 H15 2 0.956014 0.891340 0.664105 11.00000 -1.20000 AFIX 0 C2 1 0.253990 0.435518 0.526290 11.00000 0.03889 0.02995 = 0.04946 -0.00593 0.00001 0.01487 AFIX 137 H2A 2 0.253041 0.415152 0.564527 11.00000 -1.50000 H2B 2 0.250543 0.408863 0.492239 11.00000 -1.50000 H2C 2 0.219490 0.443450 0.525178 11.00000 -1.50000 AFIX 0 F2 4 0.578204 0.672490 0.442671 11.00000 0.09264 0.11936 = 0.10018 0.01996 0.05365 0.06252 C13 1 0.867750 0.921656 0.663056 11.00000 0.02979 0.02867 = 0.04455 -0.00198 -0.00157 0.01365 C8 1 0.711215 0.792103 0.644145 11.00000 0.02737 0.04024 = 0.05937 -0.00497 0.00229 0.01526 AFIX 43 H8 2 0.732344 0.771934 0.630021 11.00000 -1.20000 AFIX 0 C1 1 0.315158 0.496986 0.521460 11.00000 0.03479 0.02823 = 0.03847 -0.00571 -0.00151 0.01806 C10 1 0.710043 0.881185 0.685849 11.00000 0.02592 0.04106 = 0.05937 -0.01253 -0.00267 0.01271 AFIX 43 H10 2 0.730603 0.922421 0.700160 11.00000 -1.20000 AFIX 0 C3 1 0.318397 0.532712 0.462222 11.00000 0.04651 0.03475 = 0.03787 -0.00242 0.00107 0.02122 AFIX 137 H3A 2 0.282825 0.538936 0.460480 11.00000 -1.50000 H3B 2 0.317969 0.508825 0.426870 11.00000 -1.50000 H3C 2 0.356430 0.572776 0.462178 11.00000 -1.50000 AFIX 0 C4 1 0.370792 0.485844 0.525629 11.00000 0.04018 0.03767 = 0.05532 -0.00901 0.00079 0.02336 AFIX 137 H4A 2 0.409296 0.525434 0.523927 11.00000 -1.50000 H4B 2 0.369320 0.459958 0.491647 11.00000 -1.50000 H4C 2 0.368796 0.465121 0.563938 11.00000 -1.50000 AFIX 0 C7 1 0.645604 0.760341 0.645460 11.00000 0.02914 0.03184 = 0.05924 -0.00324 -0.00421 0.01169 AFIX 43 H7 2 0.623767 0.719123 0.631165 11.00000 -1.20000 AFIX 0 C5 1 0.511220 0.649608 0.530350 11.00000 0.02600 0.02979 = 0.05695 -0.00434 0.00278 0.01288 C11 1 0.645715 0.846519 0.685867 11.00000 0.02777 0.04479 = 0.06073 -0.00734 0.00222 0.01620 AFIX 43 H11 2 0.623458 0.865454 0.700177 11.00000 -1.20000 AFIX 0 C6 1 0.560034 0.639385 0.494592 11.00000 0.03793 0.06383 = 0.07124 -0.01224 0.00738 0.02767 HKLF 4 REM 230111_rn_scam_90k_auto_a.res in R-3 REM wR2 = 0.1076, GooF = S = 1.070, Restrained GooF = 1.062 for all data REM R1 = 0.0379 for 4397 Fo > 4sig(Fo) and 0.0417 for all 4922 data REM 220 parameters refined using 184 restraints END WGHT 0.0553 89.2736 REM Highest difference peak 0.822, deepest hole -0.951, 1-sigma level 0.121 Q1 1 0.3288 0.5934 0.6469 11.00000 0.05 0.82 Q2 1 0.5075 0.7664 0.6681 11.00000 0.05 0.78 Q3 1 0.4038 0.6611 0.5217 11.00000 0.05 0.77 Q4 1 0.6201 0.7003 0.5003 11.00000 0.05 0.70 Q5 1 0.6129 0.7046 0.4892 11.00000 0.05 0.68 Q6 1 0.3333 0.6667 0.6426 10.33333 0.05 0.56 Q7 1 0.5060 0.7371 0.6230 11.00000 0.05 0.54 Q8 1 0.2602 0.5999 0.4557 11.00000 0.05 0.51 Q9 1 0.4805 0.7082 0.6591 11.00000 0.05 0.48 Q10 1 0.5074 0.7443 0.7053 11.00000 0.05 0.47 Q11 1 0.4272 0.6650 0.5671 11.00000 0.05 0.47 Q12 1 0.4023 0.6577 0.6106 11.00000 0.05 0.44 Q13 1 0.4352 0.6578 0.6196 11.00000 0.05 0.36 Q14 1 0.6320 0.6484 0.6235 11.00000 0.05 0.36 Q15 1 0.5327 0.7397 0.6589 11.00000 0.05 0.36 Q16 1 0.5568 0.6273 0.4510 11.00000 0.05 0.36 ; _shelx_res_checksum 13591 _shelx_fab_file ; 0 0 3 -94.5204 35.2529 0 0 6 132.8767 -41.2015 0 0 9 -47.4139 -112.8323 0 0 12 40.0218 -2.3781 0 0 15 -30.1139 9.1924 0 0 18 17.5838 -65.5554 0 0 21 -12.3355 -24.5120 0 0 24 -5.6403 11.6451 0 0 27 -4.4126 -13.2358 0 1 -25 -0.7530 13.6542 0 1 -22 11.5112 -22.0576 0 1 -19 -10.5138 -32.6231 0 1 -16 22.8452 28.1023 0 1 -13 -27.1761 -4.5096 0 1 -10 36.9677 -75.9699 0 1 -7 -43.0319 -0.8422 0 1 -4 84.3131 29.6006 0 1 -1 -284.0847 -47.8103 0 1 2 142.6603 -42.2985 0 1 5 -94.5090 36.4099 0 1 8 31.1213 16.0394 0 1 11 -27.5502 -48.4695 0 1 14 25.1293 2.6267 0 1 17 -21.9565 29.3248 0 1 20 9.9951 -17.7757 0 1 23 -5.2658 -13.7994 0 1 26 4.6885 12.8728 0 2 -26 -2.3824 7.1286 0 2 -23 -5.9288 11.0726 0 2 -20 7.1566 6.7269 0 2 -17 -11.4929 8.8790 0 2 -14 18.7623 20.4661 0 2 -11 -9.7995 16.3638 0 2 -8 17.7763 15.2914 0 2 -5 -21.6210 25.6808 0 2 -2 228.3607 13.7071 0 2 1 219.8268 -5.5215 0 2 4 67.0672 5.8142 0 2 7 -18.2103 4.5389 0 2 10 11.0448 -23.1853 0 2 13 -9.4876 -6.0167 0 2 16 9.8319 7.9992 0 2 19 -8.9475 -11.0752 0 2 22 2.7586 -7.2251 0 2 25 -7.0741 3.7634 0 3 -24 1.7006 4.4930 0 3 -21 3.4798 -1.8454 0 3 -18 10.7398 1.4582 0 3 -15 -13.7712 10.5766 0 3 -12 9.8444 -1.0198 0 3 -9 8.9477 -9.5888 0 3 -6 35.7091 7.9990 0 3 -3 -129.9586 3.0788 0 3 0 -140.5360 -25.4919 0 3 3 142.6375 -9.0741 0 3 6 -17.3102 3.5599 0 3 9 -11.7763 -23.8122 0 3 12 7.8875 -21.2028 0 3 15 -2.4662 0.2185 0 3 18 2.4383 -8.9257 0 3 21 -1.3012 -16.7341 0 3 24 -0.3621 -2.7898 0 4 -25 -3.8135 3.4422 0 4 -22 8.7224 8.6017 0 4 -19 -10.8323 5.4551 0 4 -16 7.7819 9.2442 0 4 -13 1.2686 15.5232 0 4 -10 9.8048 8.2144 0 4 -7 6.5973 10.0612 0 4 -4 70.9686 21.1295 0 4 -1 6.1080 14.0230 0 4 2 122.2293 8.2438 0 4 5 41.5098 19.8177 0 4 8 -5.7282 17.6077 0 4 11 11.7711 3.4025 0 4 14 -2.8652 8.5827 0 4 17 -11.7722 10.1578 0 4 20 6.9269 1.2531 0 4 23 -3.8245 2.1639 0 4 26 -3.6978 9.6075 0 5 -26 1.1648 -0.7488 0 5 -23 -3.5161 0.6072 0 5 -20 9.5051 12.1143 0 5 -17 -9.6127 12.6322 0 5 -14 2.6301 1.8223 0 5 -11 -3.3480 11.1636 0 5 -8 13.2033 24.9341 0 5 -5 -22.8267 7.7233 0 5 -2 -10.3663 2.1883 0 5 1 -55.8299 26.6185 0 5 4 105.4461 19.2500 0 5 7 -3.2606 -1.1729 0 5 10 -8.0126 12.1129 0 5 13 -7.0096 21.3341 0 5 16 4.8999 1.1670 0 5 19 -6.7341 -0.6059 0 5 22 4.4244 11.1074 0 5 25 4.0919 1.6269 0 6 -24 -2.5278 -7.1433 0 6 -21 2.9477 9.0517 0 6 -18 -3.2239 13.6784 0 6 -15 -8.2269 -9.7425 0 6 -12 15.1314 0.7850 0 6 -9 -9.1147 25.6008 0 6 -6 5.0647 0.3354 0 6 -3 9.3560 -11.2595 0 6 0 -45.8740 17.8529 0 6 3 -1.0604 12.3197 0 6 6 14.4520 -14.9837 0 6 9 8.4502 1.2536 0 6 12 5.0717 14.0693 0 6 15 -0.4191 -5.2026 0 6 18 -1.3447 -5.0718 0 6 21 -1.7305 7.2962 0 6 24 -2.2650 1.8420 0 7 -25 1.1040 -4.5903 0 7 -22 -0.8683 -0.3274 0 7 -19 -1.0745 10.3835 0 7 -16 -0.0209 1.4485 0 7 -13 1.8482 -4.5908 0 7 -10 11.1777 13.2170 0 7 -7 12.5312 11.1666 0 7 -4 8.7509 -6.8151 0 7 -1 -46.5068 5.5210 0 7 2 -26.5562 17.0068 0 7 5 20.8177 -3.3898 0 7 8 0.2792 -2.5551 0 7 11 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-2.7971 22 1 -6 -3.4986 -13.9208 22 1 -3 -5.9329 23.8350 22 1 0 -1.5709 16.8481 22 1 3 2.3181 -14.7882 22 1 6 -4.0889 9.3618 22 1 9 0.5410 25.6589 22 1 12 -0.6100 -5.5573 22 2 -13 -0.6852 1.2273 22 2 -10 -4.0592 -6.3183 22 2 -7 0.4588 9.7049 22 2 -4 -1.1656 -4.4001 22 2 -1 2.5689 -13.5042 22 2 2 -6.5427 3.5316 22 2 5 0.9836 3.7268 22 2 8 -5.7814 -13.7434 22 2 11 -0.4832 -4.3881 22 3 -11 -1.0268 3.6128 22 3 -8 6.8951 -0.3114 22 3 -5 2.0145 -1.2017 22 3 -2 -9.7208 -2.1034 22 3 1 1.4458 -1.6709 22 3 4 -3.2601 -2.7118 22 3 7 2.1963 -3.7708 22 3 10 2.6205 1.3559 22 4 -9 -1.7679 -1.5333 22 4 -6 -3.7606 -0.1618 22 4 -3 -0.1359 4.3827 22 4 0 0.1238 6.3787 22 4 3 -0.4862 3.4908 22 4 6 -1.3120 4.1892 22 4 9 -6.6281 5.9269 22 5 -7 -3.5700 -3.0610 22 5 -4 -0.2880 -0.9702 22 5 -1 2.8990 -3.7208 22 5 2 -0.6691 -4.9373 22 5 5 -1.7178 -0.7173 22 5 8 8.5572 -3.7500 22 6 -5 -3.6996 1.3556 22 6 -2 1.8888 1.1865 22 6 1 4.7447 -2.0676 22 6 4 -0.7152 0.3526 22 6 7 -8.1360 1.0305 22 7 -3 0.2038 -3.6368 22 7 0 5.3211 1.0594 22 7 3 -0.8357 3.6751 23 1 -11 0.6009 9.7882 23 1 -8 -2.8725 -11.2836 23 1 -5 -1.7487 0.1118 23 1 -2 1.8873 24.3079 23 1 1 14.5597 -1.4155 23 1 4 -1.0652 -10.4358 23 1 7 0.2898 18.2155 23 1 10 -1.7105 10.4654 23 2 -9 -4.5166 -1.3931 23 2 -6 1.7299 7.1996 23 2 -3 7.7486 -9.4120 23 2 0 -7.9268 -7.3325 23 2 3 3.1940 8.9834 23 2 6 -3.3873 -2.0045 23 2 9 2.8055 -6.1637 23 3 -10 0.2978 1.6432 23 3 -7 1.4236 -1.9253 23 3 -4 -0.4760 -2.5563 23 3 -1 11.6885 -2.0117 23 3 2 1.6863 -2.7204 23 3 5 4.3680 -3.4997 23 3 8 0.4929 -1.0566 23 4 -8 -1.2143 0.8985 23 4 -5 -2.4264 -0.6684 23 4 -2 -1.6410 4.8245 23 4 1 1.7697 2.8631 23 4 4 -2.1857 -0.4424 23 4 7 -4.8358 1.8801 23 5 -6 13.2006 1.1414 23 5 -3 0.9485 -2.3725 23 5 0 -4.3378 1.4170 23 5 3 0.4454 -5.2987 23 5 6 1.8026 -4.4095 23 6 -1 -0.0136 -2.6741 23 6 2 -6.9724 7.3307 24 1 -10 6.0873 4.5249 24 1 -7 2.4014 -10.2578 24 1 -4 -3.6664 12.1269 24 1 -1 1.2469 15.3745 24 1 2 -5.6586 -7.3135 24 1 5 -3.4236 0.0006 24 1 8 -4.9066 17.1771 24 2 -8 -3.6626 3.4026 24 2 -5 0.2753 -1.1595 24 2 -2 -1.0432 -8.7111 24 2 1 -1.2654 -2.5055 24 2 4 -2.0067 4.6124 24 2 7 3.9005 -1.8315 24 3 -6 -2.9891 -0.0109 24 3 -3 -8.4862 1.1684 24 3 0 -0.7895 2.5519 24 3 3 0.7331 -3.8090 24 3 6 4.0724 -4.3472 24 4 -4 7.5690 -1.3065 24 4 -1 -2.8907 3.1911 24 4 2 2.6718 7.1564 25 1 -6 0.2776 9.0635 25 1 -3 -4.5247 18.3667 25 1 0 7.2051 4.8982 25 1 3 6.7004 1.6420 25 1 6 2.7816 15.1169 25 2 -4 6.4988 -1.1333 25 2 -1 -8.0240 -5.9897 25 2 2 -4.9498 0.9524 25 2 5 -2.7575 0.3983 26 1 -2 3.6381 7.7638 26 1 1 2.7058 6.0968 0 0 0 0.0 0.0 ; _shelx_fab_checksum 3391 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.830 _oxdiff_exptl_absorpt_empirical_full_min 0.743 loop_ _space_group_symop_operation_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'x+2/3, y+1/3, z+1/3' '-y+2/3, x-y+1/3, z+1/3' '-x+y+2/3, -x+1/3, z+1/3' 'x+1/3, y+2/3, z+2/3' '-y+1/3, x-y+2/3, z+2/3' '-x+y+1/3, -x+2/3, z+2/3' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-x+2/3, -y+1/3, -z+1/3' 'y+2/3, -x+y+1/3, -z+1/3' 'x-y+2/3, x+1/3, -z+1/3' '-x+1/3, -y+2/3, -z+2/3' 'y+1/3, -x+y+2/3, -z+2/3' 'x-y+1/3, x+2/3, -z+2/3' 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 Ag1 Ag 0.39964(2) 0.65809(2) 0.56900(2) 0.02966(11) Uani 1 1 d . U . . . Ag2 Ag 0.50599(2) 0.73369(2) 0.66401(2) 0.03862(12) Uani 1 1 d . U . . . S1 S 0.32011(5) 0.54730(4) 0.58970(5) 0.0285(2) Uani 1 1 d . U . . . O2 O 0.51744(15) 0.65394(15) 0.58740(17) 0.0383(7) Uani 1 1 d . U . . . O1 O 0.47026(15) 0.65065(16) 0.49723(16) 0.0395(7) Uani 1 1 d . U . . . F1 F 0.5362(2) 0.5806(2) 0.4770(2) 0.0827(13) Uani 1 1 d . U . . . F3 F 0.60974(18) 0.6517(3) 0.5282(2) 0.0909(15) Uani 1 1 d . U . . . C12 C 0.8116(2) 0.8898(2) 0.6629(2) 0.0374(9) Uani 1 1 d . U . . . C9 C 0.7445(2) 0.8538(2) 0.6640(2) 0.0365(9) Uani 1 1 d . U . . . C14 C 0.93470(19) 0.9610(2) 0.6633(2) 0.0319(9) Uani 1 1 d . U . . . N1 N 0.61292(17) 0.78643(19) 0.6663(2) 0.0395(9) Uani 1 1 d . U . . . C15 C 0.9736(2) 0.93479(19) 0.6636(2) 0.0317(9) Uani 1 1 d . U . . . H15 H 0.956014 0.891340 0.664105 0.038 Uiso 1 1 calc R U . . . C2 C 0.2540(2) 0.4355(2) 0.5263(2) 0.0405(10) Uani 1 1 d . U . . . H2A H 0.253041 0.415152 0.564527 0.061 Uiso 1 1 calc R U . . . H2B H 0.250543 0.408863 0.492239 0.061 Uiso 1 1 calc R U . . . H2C H 0.219490 0.443450 0.525178 0.061 Uiso 1 1 calc R U . . . F2 F 0.5782(2) 0.6725(3) 0.4427(3) 0.0998(15) Uani 1 1 d . U . . . C13 C 0.8677(2) 0.9217(2) 0.6631(2) 0.0348(9) Uani 1 1 d . U . . . C8 C 0.7112(2) 0.7921(2) 0.6441(3) 0.0431(11) Uani 1 1 d . U . . . H8 H 0.732344 0.771934 0.630021 0.052 Uiso 1 1 calc R U . . . C1 C 0.3152(2) 0.4970(2) 0.5215(2) 0.0328(9) Uani 1 1 d . U . . . C10 C 0.7100(2) 0.8812(2) 0.6858(3) 0.0439(11) Uani 1 1 d . U . . . H10 H 0.730603 0.922421 0.700160 0.053 Uiso 1 1 calc R U . . . C3 C 0.3184(2) 0.5327(2) 0.4622(2) 0.0393(10) Uani 1 1 d . U . . . H3A H 0.282825 0.538936 0.460480 0.059 Uiso 1 1 calc R U . . . H3B H 0.317969 0.508825 0.426870 0.059 Uiso 1 1 calc R U . . . H3C H 0.356430 0.572776 0.462178 0.059 Uiso 1 1 calc R U . . . C4 C 0.3708(2) 0.4858(2) 0.5256(3) 0.0427(11) Uani 1 1 d . U . . . H4A H 0.409296 0.525434 0.523927 0.064 Uiso 1 1 calc R U . . . H4B H 0.369320 0.459958 0.491647 0.064 Uiso 1 1 calc R U . . . H4C H 0.368796 0.465121 0.563938 0.064 Uiso 1 1 calc R U . . . C7 C 0.6456(2) 0.7603(2) 0.6455(3) 0.0417(10) Uani 1 1 d . U . . . H7 H 0.623767 0.719123 0.631165 0.050 Uiso 1 1 calc R U . . . C5 C 0.5112(2) 0.6496(2) 0.5303(3) 0.0381(10) Uani 1 1 d . U . . . C11 C 0.6457(2) 0.8465(3) 0.6859(3) 0.0453(11) Uani 1 1 d . U . . . H11 H 0.623458 0.865454 0.700177 0.054 Uiso 1 1 calc R U . . . C6 C 0.5600(3) 0.6394(3) 0.4946(3) 0.0567(13) Uani 1 1 d . U . . . 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 0.02394(16) 0.02172(16) 0.04192(19) -0.00059(11) 0.00011(11) 0.01037(12) Ag2 0.02143(16) 0.0412(2) 0.0470(2) 0.00971(14) -0.00033(12) 0.01093(14) S1 0.0259(5) 0.0226(4) 0.0379(5) -0.0012(4) 0.0001(4) 0.0130(4) O2 0.0320(16) 0.0310(16) 0.053(2) -0.0027(14) 0.0005(14) 0.0166(13) O1 0.0332(16) 0.0399(17) 0.0466(18) -0.0037(14) 0.0036(13) 0.0191(14) F1 0.073(2) 0.078(3) 0.115(3) -0.038(2) 0.000(2) 0.052(2) F3 0.047(2) 0.136(4) 0.102(3) -0.052(3) -0.014(2) 0.055(2) C12 0.030(2) 0.033(2) 0.047(2) -0.0033(18) -0.0006(18) 0.0138(17) C9 0.0263(19) 0.034(2) 0.044(2) -0.0009(18) 0.0005(17) 0.0105(17) C14 0.0249(19) 0.0267(19) 0.041(2) -0.0010(17) -0.0012(16) 0.0104(16) N1 0.0235(17) 0.038(2) 0.052(2) 0.0011(17) -0.0013(15) 0.0115(15) C15 0.029(2) 0.0224(19) 0.041(2) -0.0002(16) -0.0007(17) 0.0112(16) C2 0.039(2) 0.030(2) 0.049(3) -0.0059(19) 0.000(2) 0.0149(19) F2 0.093(3) 0.119(4) 0.100(3) 0.020(3) 0.054(3) 0.063(3) C13 0.030(2) 0.029(2) 0.045(2) -0.0020(17) -0.0016(17) 0.0137(17) C8 0.027(2) 0.040(2) 0.059(3) -0.005(2) 0.002(2) 0.0153(18) C1 0.035(2) 0.0282(19) 0.038(2) -0.0057(17) -0.0015(17) 0.0181(17) C10 0.026(2) 0.041(2) 0.059(3) -0.013(2) -0.003(2) 0.0127(18) C3 0.047(3) 0.035(2) 0.038(2) -0.0024(18) 0.001(2) 0.021(2) C4 0.040(2) 0.038(2) 0.055(3) -0.009(2) 0.001(2) 0.023(2) C7 0.029(2) 0.032(2) 0.059(3) -0.003(2) -0.004(2) 0.0117(18) C5 0.026(2) 0.030(2) 0.057(3) -0.0043(19) 0.0028(18) 0.0129(17) C11 0.028(2) 0.045(2) 0.061(3) -0.007(2) 0.002(2) 0.0162(19) C6 0.038(3) 0.064(3) 0.071(3) -0.012(3) 0.007(2) 0.028(2) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.1306 4.2820 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Ag1 Ag1 Ag1 60.0 2_665 3_565 ? Ag1 Ag1 Ag2 132.757(9) 2_665 14_456 ? Ag1 Ag1 Ag2 94.712(12) 3_565 14_456 ? Ag1 Ag1 Ag2 134.928(9) 3_565 . ? Ag1 Ag1 Ag2 97.718(12) 2_665 . ? Ag2 Ag1 Ag2 71.577(7) . 14_456 ? S1 Ag1 Ag1 111.50(2) . 2_665 ? S1 Ag1 Ag1 52.26(2) 2_665 2_665 ? S1 Ag1 Ag1 52.62(2) . 3_565 ? S1 Ag1 Ag1 111.15(2) 2_665 3_565 ? S1 Ag1 Ag2 121.56(3) 2_665 14_456 ? S1 Ag1 Ag2 52.76(2) 2_665 . ? S1 Ag1 Ag2 120.30(3) . . ? S1 Ag1 Ag2 50.09(2) . 14_456 ? S1 Ag1 S1 153.44(5) . 2_665 ? O1 Ag1 Ag1 131.91(8) . 3_565 ? O1 Ag1 Ag1 130.85(8) . 2_665 ? O1 Ag1 Ag2 96.12(8) . 14_456 ? O1 Ag1 Ag2 92.80(8) . . ? O1 Ag1 S1 102.33(8) . 2_665 ? O1 Ag1 S1 103.68(9) . . ? Ag1 Ag2 Ag1 92.272(14) . 15_556 ? S1 Ag2 Ag1 87.76(3) 15_556 . ? S1 Ag2 Ag1 49.07(2) 15_556 15_556 ? S1 Ag2 Ag1 84.49(3) 2_665 15_556 ? S1 Ag2 Ag1 50.99(2) 2_665 . ? S1 Ag2 S1 118.27(5) 15_556 2_665 ? N1 Ag2 Ag1 129.23(11) . 15_556 ? N1 Ag2 Ag1 137.85(11) . . ? N1 Ag2 S1 123.06(11) . 15_556 ? N1 Ag2 S1 117.64(11) . 2_665 ? Ag1 S1 Ag1 75.12(3) . 3_565 ? Ag1 S1 Ag2 134.21(4) 3_565 14_456 ? Ag1 S1 Ag2 76.25(3) 3_565 3_565 ? Ag1 S1 Ag2 80.84(3) . 14_456 ? Ag1 S1 Ag2 133.76(4) . 3_565 ? Ag2 S1 Ag2 94.31(4) 14_456 3_565 ? C1 S1 Ag1 109.64(15) . . ? C1 S1 Ag1 110.25(14) . 3_565 ? C1 S1 Ag2 114.03(15) . 3_565 ? C1 S1 Ag2 114.38(14) . 14_456 ? C5 O1 Ag1 104.6(3) . . ? C13 C12 C9 177.7(5) . . ? C8 C9 C12 122.7(4) . . ? C8 C9 C10 117.7(4) . . ? C10 C9 C12 119.7(4) . . ? C15 C14 C15 119.8(4) . 3_675 ? C15 C14 C13 119.5(4) 3_675 . ? C15 C14 C13 120.7(4) . . ? C7 N1 Ag2 121.4(3) . . ? C7 N1 C11 117.3(4) . . ? C11 N1 Ag2 121.2(3) . . ? C14 C15 C14 120.2(4) . 2_765 ? C14 C15 H15 119.9 . . ? C14 C15 H15 119.9 2_765 . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? C12 C13 C14 178.7(5) . . ? C9 C8 H8 120.3 . . ? C9 C8 C7 119.4(5) . . ? C7 C8 H8 120.3 . . ? C2 C1 S1 107.9(3) . . ? C2 C1 C3 111.8(4) . . ? C2 C1 C4 110.5(4) . . ? C3 C1 S1 108.0(3) . . ? C4 C1 S1 107.5(3) . . ? C4 C1 C3 111.0(4) . . ? C9 C10 H10 120.4 . . ? C11 C10 C9 119.2(5) . . ? C11 C10 H10 120.4 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 C7 C8 122.9(5) . . ? N1 C7 H7 118.5 . . ? C8 C7 H7 118.5 . . ? O2 C5 O1 129.5(4) . . ? O2 C5 C6 116.0(5) . . ? O1 C5 C6 114.5(5) . . ? N1 C11 C10 123.5(5) . . ? N1 C11 H11 118.2 . . ? C10 C11 H11 118.2 . . ? F1 C6 F3 105.3(5) . . ? F1 C6 F2 104.9(6) . . ? F1 C6 C5 111.5(5) . . ? F3 C6 F2 109.7(5) . . ? F3 C6 C5 113.0(5) . . ? F2 C6 C5 111.9(5) . . ? 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 Ag1 3.0195(5) 2_665 ? Ag1 Ag1 3.0195(5) 3_565 ? Ag1 Ag2 3.2286(5) 14_456 ? Ag1 Ag2 3.1039(5) . ? Ag1 S1 2.4708(10) . ? Ag1 S1 2.4829(10) 2_665 ? Ag1 O1 2.401(3) . ? Ag2 S1 2.5087(11) 15_556 ? Ag2 S1 2.5439(10) 2_665 ? Ag2 N1 2.275(4) . ? S1 C1 1.888(4) . ? O2 C5 1.240(6) . ? O1 C5 1.245(6) . ? F1 C6 1.314(7) . ? F3 C6 1.320(7) . ? C12 C9 1.429(6) . ? C12 C13 1.199(7) . ? C9 C8 1.381(7) . ? C9 C10 1.400(7) . ? C14 C15 1.393(6) . ? C14 C15 1.400(6) 3_675 ? C14 C13 1.431(6) . ? N1 C7 1.331(7) . ? N1 C11 1.348(7) . ? C15 H15 0.9300 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C2 C1 1.510(6) . ? F2 C6 1.325(8) . ? C8 H8 0.9300 . ? C8 C7 1.396(7) . ? C1 C3 1.531(7) . ? C1 C4 1.524(6) . ? C10 H10 0.9300 . ? C10 C11 1.370(7) . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 H4A 0.9600 . ? C4 H4B 0.9600 . ? C4 H4C 0.9600 . ? C7 H7 0.9300 . ? C5 C6 1.549(7) . ? C11 H11 0.9300 . ? 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 Ag1 S1 C1 C2 -162.4(3) . . . . ? Ag1 S1 C1 C2 -81.5(3) 3_565 . . . ? Ag1 S1 C1 C3 39.5(3) 3_565 . . . ? Ag1 S1 C1 C3 -41.3(3) . . . . ? Ag1 S1 C1 C4 159.4(3) 3_565 . . . ? Ag1 S1 C1 C4 78.5(3) . . . . ? Ag1 O1 C5 O2 -2.7(6) . . . . ? Ag1 O1 C5 C6 175.2(4) . . . . ? Ag2 S1 C1 C2 109.0(3) 14_456 . . . ? Ag2 S1 C1 C2 2.0(4) 3_565 . . . ? Ag2 S1 C1 C3 123.1(3) 3_565 . . . ? Ag2 S1 C1 C3 -130.0(3) 14_456 . . . ? Ag2 S1 C1 C4 -117.1(3) 3_565 . . . ? Ag2 S1 C1 C4 -10.1(4) 14_456 . . . ? Ag2 N1 C7 C8 177.7(4) . . . . ? Ag2 N1 C11 C10 -177.3(4) . . . . ? O2 C5 C6 F1 103.1(6) . . . . ? O2 C5 C6 F3 -15.3(7) . . . . ? O2 C5 C6 F2 -139.7(5) . . . . ? O1 C5 C6 F1 -75.2(7) . . . . ? O1 C5 C6 F3 166.5(5) . . . . ? O1 C5 C6 F2 42.0(7) . . . . ? C12 C9 C8 C7 -178.7(5) . . . . ? C12 C9 C10 C11 179.1(5) . . . . ? C9 C8 C7 N1 -1.3(9) . . . . ? C9 C10 C11 N1 0.5(9) . . . . ? C15 C14 C15 C14 -1.0(9) 3_675 . . 2_765 ? C13 C14 C15 C14 179.4(3) . . . 2_765 ? C8 C9 C10 C11 -0.8(8) . . . . ? C10 C9 C8 C7 1.2(8) . . . . ? C7 N1 C11 C10 -0.6(8) . . . . ? C11 N1 C7 C8 0.9(8) . . . . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.083 -0.981 -0.255 4621.6 705.2 '27 C2H5OH'