#------------------------------------------------------------------------------ #$Date: 2020-03-04 09:48:00 +0200 (Wed, 04 Mar 2020) $ #$Revision: 248753 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/74/1557458.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_1557458 loop_ _publ_author_name 'Tezuka, Noriyuki' 'Hirano, Keiichi' 'Peel, Andrew J.' 'Wheatley, Andrew E. H.' 'Miyamoto, Kazunori' 'Uchiyama, Masanobu' _publ_section_title ; Lipshutz-type bis(amido)argentates for directed ortho argentation ; _journal_issue 7 _journal_name_full 'Chemical Science' _journal_page_first 1855 _journal_paper_doi 10.1039/C9SC06060J _journal_volume 11 _journal_year 2020 _chemical_formula_moiety 'C30 H44 Ag Li N2 O3, 2(C6 H6)' _chemical_formula_sum 'C42 H56 Ag Li N2 O3' _chemical_formula_weight 751.69 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2019-10-18 _audit_creation_method ; Olex2 1.2-ac3 (compiled 2017.08.10 svn.r3458 for OlexSys, GUI svn.r5381) ; _audit_update_record ; 2019-10-18 deposited with the CCDC. 2020-01-03 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 93.742(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.4986(2) _cell_length_b 14.8962(2) _cell_length_c 21.7554(4) _cell_measurement_reflns_used 16840 _cell_measurement_temperature 90 _cell_measurement_theta_max 77.1570 _cell_measurement_theta_min 3.5550 _cell_volume 4041.82(11) _computing_cell_refinement 'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)' _computing_data_collection 'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)' _computing_data_reduction 'CrysAlisPro 1.171.39.45g (Rigaku OD, 2018)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 90 _diffrn_detector 'Rigaku HyPix-6000 area detector' _diffrn_detector_area_resol_mean 10.0 _diffrn_detector_type 'HPC area detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.969 _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 -44.00 112.00 0.50 0.50 -- 39.95 -16.00 19.00 312 2 \w 33.00 118.00 0.50 1.80 -- 115.57 -16.00 19.00 170 3 \w 75.00 103.00 0.50 1.80 -- 115.57 -94.00 0.00 56 4 \w 49.00 77.00 0.50 1.80 -- 115.57 -45.00 -30.00 56 5 \w 42.00 99.00 0.50 1.80 -- 115.57 -94.00 -90.00 114 6 \w 66.00 108.00 0.50 1.80 -- 115.57 -94.00-150.00 84 7 \w 58.00 84.00 0.50 1.80 -- 115.57 -94.00-180.00 52 8 \w 33.00 58.00 0.50 1.80 -- 115.57 -30.00-150.00 50 9 \w 37.00 72.00 0.50 1.80 -- 115.57 -45.00-120.00 70 10 \w 106.00 177.00 0.50 1.80 -- 115.57 16.00-171.00 142 11 \w 44.00 72.00 0.50 1.80 -- 115.57 -94.00 0.00 56 12 \w 41.00 98.00 0.50 1.80 -- 115.57-125.00 0.00 114 13 \w 34.00 64.00 0.50 1.80 -- 115.57 -30.00 0.00 60 14 \w 40.00 77.00 0.50 1.80 -- 115.57 -45.00 0.00 74 15 \w 40.00 79.00 0.50 1.80 -- 115.57 -45.00 -60.00 78 16 \w 35.00 68.00 0.50 1.80 -- 115.57 -30.00 -90.00 66 17 \w 34.00 68.00 0.50 1.80 -- 115.57 -30.00-120.00 68 18 \w -71.00 -46.00 0.50 0.50 -- -39.95 -16.00 19.00 50 19 \w -64.00 -3.00 0.50 1.80 -- -84.50 30.00 -30.00 122 20 \w -106.00 -81.00 0.50 1.80 -- -84.50 16.00-171.00 50 21 \w -117.00 -78.00 0.50 0.50 -- -39.95 16.00-171.00 78 22 \w -143.00 -90.00 0.50 1.80 -- -84.50 -16.00 19.00 106 23 \w -114.00 -10.00 0.50 1.80 -- -84.50 61.00 30.00 208 24 \w -164.00 -80.00 0.50 1.80 -- -84.50 -94.00 150.00 168 25 \w -123.00 -38.00 0.50 0.50 -- -39.95-178.00 120.00 170 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Rigaku XtaLAB Synergy-S' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 -0.1025727000 _diffrn_orient_matrix_UB_12 -0.0055106000 _diffrn_orient_matrix_UB_13 0.0354156000 _diffrn_orient_matrix_UB_21 -0.0683643000 _diffrn_orient_matrix_UB_22 0.0208910000 _diffrn_orient_matrix_UB_23 -0.0598020000 _diffrn_orient_matrix_UB_31 -0.0084441000 _diffrn_orient_matrix_UB_32 -0.1011134000 _diffrn_orient_matrix_UB_33 -0.0143263000 _diffrn_radiation_monochromator 'multi-layer mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0348 _diffrn_reflns_av_unetI/netI 0.0303 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.969 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 27075 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.969 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 77.112 _diffrn_reflns_theta_min 3.599 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_type PhotonJet-S _exptl_absorpt_coefficient_mu 4.283 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.480 _exptl_absorpt_correction_type gaussian _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.45g (Rigaku Oxford Diffraction, 2018) Numerical absorption correction based on gaussian integration over a multifaceted crystal model Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour 'clear light yellow' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier light _exptl_crystal_colour_primary yellow _exptl_crystal_density_diffrn 1.235 _exptl_crystal_description block _exptl_crystal_F_000 1584 _exptl_crystal_size_max 0.231 _exptl_crystal_size_mid 0.165 _exptl_crystal_size_min 0.162 _refine_diff_density_max 0.581 _refine_diff_density_min -1.095 _refine_diff_density_rms 0.066 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.962 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 450 _refine_ls_number_reflns 8303 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 0.962 _refine_ls_R_factor_all 0.0349 _refine_ls_R_factor_gt 0.0328 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1101 _refine_ls_wR_factor_ref 0.1128 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7705 _reflns_number_total 8303 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL exp_28_a.res in P2(1)/n exp_28.res created by SHELXL-2018/1 at 13:47:17 on 18-Oct-2019 REM Old TITL exp_28_a.res in P2(1)/n REM SHELXT solution in P2(1)/n REM R1 0.077, Rweak 0.010, Alpha 0.038, Orientation as input REM Formula found by SHELXT: C41 Ag Li N3 O3 CELL 1.54184 12.4986 14.8962 21.7554 90 93.742 90 ZERR 4 0.0002 0.0002 0.0004 0 0.002 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Ag Li N O UNIT 168 224 4 4 8 12 L.S. 10 PLAN 20 TEMP -183.15 BOND $H list 4 fmap 2 acta REM REM REM WGHT 0.100000 FVAR 0.31274 AG01 3 0.585140 0.293558 0.561150 11.00000 0.02382 0.02792 = 0.02333 -0.00278 0.00362 -0.00064 O002 6 0.557250 0.522342 0.358370 11.00000 0.04285 0.02742 = 0.02709 0.00133 -0.00529 0.00057 O003 6 0.665676 0.349613 0.401501 11.00000 0.04624 0.02480 = 0.03091 0.00189 -0.00231 -0.00002 O004 6 0.703237 0.526631 0.489189 11.00000 0.04669 0.03096 = 0.02855 -0.00335 -0.00568 -0.00032 N005 5 0.488974 0.615847 0.284081 11.00000 0.03026 0.02649 = 0.02086 0.00032 -0.00115 -0.00096 N006 5 0.662613 0.199074 0.408760 11.00000 0.02685 0.02440 = 0.02217 -0.00049 0.00080 -0.00181 C20 1 0.745541 0.303280 0.540184 11.00000 0.02208 0.02301 = 0.03062 -0.00269 0.00366 -0.00226 C008 1 0.572869 0.723417 0.414614 11.00000 0.02230 0.02988 = 0.02214 0.00143 0.00407 0.00144 C009 1 0.550045 0.599694 0.336033 11.00000 0.02758 0.02720 = 0.02326 -0.00004 0.00412 0.00150 C00A 1 0.781060 0.286337 0.481252 11.00000 0.02671 0.02079 = 0.02993 -0.00136 0.00263 -0.00346 C00B 1 0.614797 0.674157 0.366446 11.00000 0.02627 0.02628 = 0.02008 0.00178 0.00030 0.00249 C00C 1 0.829049 0.318417 0.586324 11.00000 0.03012 0.02818 = 0.03009 -0.00298 -0.00047 -0.00266 AFIX 43 H00C 2 0.810252 0.331580 0.626965 11.00000 -1.20000 AFIX 0 C00D 1 0.698746 0.279580 0.428149 11.00000 0.02642 0.02615 = 0.02549 -0.00207 0.00561 -0.00191 C00E 1 0.644338 0.786799 0.442732 11.00000 0.03272 0.02735 = 0.02421 0.00045 0.00136 -0.00039 AFIX 43 H00E 2 0.620836 0.821810 0.475772 11.00000 -1.20000 AFIX 0 C00F 1 0.699082 0.115207 0.440333 11.00000 0.03351 0.02330 = 0.03136 0.00157 -0.00315 -0.00242 AFIX 13 H00F 2 0.743402 0.133169 0.478272 11.00000 -1.20000 AFIX 0 C00G 1 0.585051 0.190711 0.354449 11.00000 0.03002 0.03054 = 0.02555 0.00012 -0.00250 -0.00419 AFIX 13 H00G 2 0.570144 0.125147 0.348945 11.00000 -1.20000 AFIX 0 C00H 1 0.747736 0.800381 0.424271 11.00000 0.03038 0.03127 = 0.03001 0.00487 -0.00555 -0.00378 AFIX 43 H00H 2 0.792918 0.843767 0.444765 11.00000 -1.20000 AFIX 0 C00I 1 0.718211 0.687006 0.347324 11.00000 0.02693 0.03492 = 0.02655 0.00378 0.00311 0.00414 AFIX 43 H00I 2 0.742831 0.652004 0.314584 11.00000 -1.20000 AFIX 0 C00J 1 0.436169 0.540417 0.249029 11.00000 0.03812 0.03211 = 0.02392 -0.00110 -0.00414 -0.00416 AFIX 13 H00J 2 0.400463 0.567051 0.210795 11.00000 -1.20000 AFIX 0 C00K 1 0.520251 0.721101 0.198482 11.00000 0.04046 0.03651 = 0.02500 0.00309 0.00170 -0.00650 AFIX 137 H00A 2 0.597065 0.707457 0.203016 11.00000 -1.50000 H00B 2 0.510120 0.783467 0.184991 11.00000 -1.50000 H00D 2 0.485171 0.680798 0.167787 11.00000 -1.50000 AFIX 0 C00L 1 0.889219 0.281384 0.468759 11.00000 0.02947 0.02794 = 0.03609 -0.00289 0.00806 -0.00319 AFIX 43 H00L 2 0.909101 0.269123 0.428196 11.00000 -1.20000 AFIX 0 C00M 1 0.632086 0.222820 0.295322 11.00000 0.04372 0.05177 = 0.02430 -0.00164 0.00379 -0.00656 AFIX 137 H00K 2 0.643806 0.287823 0.297513 11.00000 -1.50000 H00M 2 0.582124 0.208862 0.260020 11.00000 -1.50000 H00N 2 0.700540 0.192401 0.290452 11.00000 -1.50000 AFIX 0 C00N 1 0.471014 0.707985 0.260263 11.00000 0.03257 0.02726 = 0.02471 0.00242 -0.00139 0.00041 AFIX 13 H00O 2 0.508676 0.749935 0.290339 11.00000 -1.20000 AFIX 0 C00O 1 0.937064 0.314908 0.574908 11.00000 0.02895 0.03097 = 0.03916 -0.00463 -0.00429 -0.00349 AFIX 43 H00P 2 0.990064 0.326437 0.607248 11.00000 -1.20000 AFIX 0 C00P 1 0.785029 0.750835 0.376094 11.00000 0.02381 0.04063 = 0.03340 0.00579 0.00106 -0.00041 AFIX 43 H00Q 2 0.855166 0.760451 0.363014 11.00000 -1.20000 AFIX 0 C00Q 1 0.817953 0.531882 0.500604 11.00000 0.04568 0.03688 = 0.04027 -0.00413 0.00347 -0.00927 AFIX 23 H00R 2 0.849422 0.573011 0.470924 11.00000 -1.20000 H00S 2 0.851093 0.471886 0.497128 11.00000 -1.20000 AFIX 0 C00R 1 0.967522 0.294632 0.516464 11.00000 0.02362 0.03114 = 0.04783 -0.00299 0.00540 -0.00454 AFIX 43 H00T 2 1.041317 0.289782 0.508931 11.00000 -1.20000 AFIX 0 C00S 1 0.477779 0.235308 0.364881 11.00000 0.02801 0.04852 = 0.03841 0.00017 -0.00009 -0.00042 AFIX 137 H00U 2 0.454102 0.217327 0.405144 11.00000 -1.50000 H00V 2 0.424298 0.216535 0.332480 11.00000 -1.50000 H00W 2 0.486068 0.300694 0.363718 11.00000 -1.50000 AFIX 0 C00T 1 0.347807 0.496351 0.283906 11.00000 0.04531 0.04407 = 0.03495 0.00261 -0.00336 -0.01539 AFIX 137 H00X 2 0.380076 0.463257 0.319372 11.00000 -1.50000 H00Y 2 0.306958 0.454807 0.256459 11.00000 -1.50000 H 2 0.299724 0.542733 0.298252 11.00000 -1.50000 AFIX 0 C00U 1 0.771473 0.061272 0.400437 11.00000 0.03909 0.02935 = 0.04972 -0.00631 -0.00079 0.00326 AFIX 137 H00Z 2 0.731081 0.043489 0.362252 11.00000 -1.50000 HA 2 0.796932 0.007496 0.422847 11.00000 -1.50000 HB 2 0.832982 0.098130 0.390542 11.00000 -1.50000 AFIX 0 C00V 1 0.650898 0.570871 0.538197 11.00000 0.05160 0.03969 = 0.03037 -0.00097 0.00185 0.00163 AFIX 23 H00 2 0.621730 0.526374 0.566479 11.00000 -1.20000 HC 2 0.591675 0.609616 0.521337 11.00000 -1.20000 AFIX 0 C00W 1 0.604651 0.060958 0.461221 11.00000 0.04513 0.03485 = 0.03786 0.00800 -0.00061 -0.01264 AFIX 137 H0AA 2 0.560342 0.099109 0.486047 11.00000 -1.50000 HD 2 0.631421 0.009755 0.485983 11.00000 -1.50000 HE 2 0.561466 0.039127 0.425065 11.00000 -1.50000 AFIX 0 C00X 1 0.518322 0.472677 0.228082 11.00000 0.05402 0.03424 = 0.03115 -0.00684 -0.00361 0.00230 AFIX 137 H1AA 2 0.573427 0.504241 0.206397 11.00000 -1.50000 HF 2 0.482263 0.428737 0.200337 11.00000 -1.50000 HG 2 0.551893 0.441669 0.264097 11.00000 -1.50000 AFIX 0 C00Y 1 0.887284 -0.077289 0.566232 11.00000 0.06373 0.04956 = 0.02859 -0.00428 -0.00518 0.01975 AFIX 43 H2AA 2 0.935528 -0.120584 0.551820 11.00000 -1.20000 AFIX 0 C00Z 1 0.844363 0.075351 0.587744 11.00000 0.05457 0.03280 = 0.03580 0.00417 -0.00603 -0.00342 AFIX 43 H3AA 2 0.862669 0.137253 0.587954 11.00000 -1.20000 AFIX 0 C010 1 0.914173 0.013351 0.566872 11.00000 0.04484 0.05827 = 0.02842 0.00346 0.00034 -0.00185 AFIX 43 H010 2 0.980973 0.032189 0.552825 11.00000 -1.20000 AFIX 0 C011 1 0.488336 1.010196 0.209178 11.00000 0.03719 0.05173 = 0.04653 -0.00237 -0.00458 0.00320 AFIX 43 H011 2 0.430402 1.043013 0.189718 11.00000 -1.20000 AFIX 0 C012 1 0.738140 0.626311 0.571046 11.00000 0.07427 0.03160 = 0.02945 -0.00190 0.00111 -0.00710 AFIX 23 H01A 2 0.746805 0.684881 0.550447 11.00000 -1.20000 H01B 2 0.723423 0.636616 0.614651 11.00000 -1.20000 AFIX 0 C013 1 0.789054 -0.104044 0.586892 11.00000 0.07574 0.03135 = 0.02991 0.00146 -0.01282 -0.00573 AFIX 43 H013 2 0.769838 -0.165755 0.586407 11.00000 -1.20000 AFIX 0 C014 1 0.580765 0.997878 0.179690 11.00000 0.05012 0.04512 = 0.03569 0.00998 0.00296 -0.00045 AFIX 43 H014 2 0.586370 1.021934 0.139586 11.00000 -1.20000 AFIX 0 C015 1 0.835080 0.567633 0.565724 11.00000 0.05472 0.04041 = 0.03467 0.00351 -0.00617 -0.01060 AFIX 23 H01C 2 0.837060 0.518367 0.596320 11.00000 -1.20000 H01D 2 0.902223 0.602833 0.571118 11.00000 -1.20000 AFIX 0 C016 1 0.351935 0.732449 0.257011 11.00000 0.03594 0.03726 = 0.04147 0.00393 0.00089 0.00601 AFIX 137 H01E 2 0.312205 0.691788 0.228405 11.00000 -1.50000 H01F 2 0.342685 0.794418 0.242497 11.00000 -1.50000 H01G 2 0.324614 0.726819 0.298046 11.00000 -1.50000 AFIX 0 C017 1 0.719757 -0.040820 0.608046 11.00000 0.04551 0.05095 = 0.03383 0.00008 -0.00207 -0.00847 AFIX 43 H017 2 0.652827 -0.058880 0.622320 11.00000 -1.20000 AFIX 0 C018 1 0.747777 0.048383 0.608423 11.00000 0.04730 0.04525 = 0.03399 -0.00287 -0.00370 0.00811 AFIX 43 H018 2 0.699997 0.091836 0.623103 11.00000 -1.20000 AFIX 0 C019 1 0.657392 0.916427 0.265425 11.00000 0.07542 0.03333 = 0.05850 -0.00343 -0.02790 0.00736 AFIX 43 H019 2 0.715904 0.884222 0.284806 11.00000 -1.20000 AFIX 0 C01A 1 0.565548 0.927963 0.295454 11.00000 0.12411 0.03844 = 0.02641 0.00194 -0.01213 -0.02867 AFIX 43 H01H 2 0.560410 0.903977 0.335615 11.00000 -1.20000 AFIX 0 C01B 1 0.665483 0.951094 0.207493 11.00000 0.04173 0.04340 = 0.06536 -0.00340 0.00350 0.00216 AFIX 43 H01I 2 0.729279 0.942811 0.186711 11.00000 -1.20000 AFIX 0 C01C 1 0.479710 0.974889 0.267050 11.00000 0.06261 0.05964 = 0.04227 -0.01898 0.02047 -0.02489 AFIX 43 H01J 2 0.415472 0.982505 0.287521 11.00000 -1.20000 AFIX 0 LI1D 4 0.637873 0.466387 0.420568 11.00000 0.04624 0.02672 = 0.03208 -0.00114 -0.00928 -0.00003 HKLF 4 REM exp_28_a.res in P2(1)/n REM R1 = 0.0328 for 7705 Fo > 4sig(Fo) and 0.0349 for all 8303 data REM 450 parameters refined using 0 restraints END WGHT 0.0521 1.7320 REM Highest difference peak 0.581, deepest hole -1.095, 1-sigma level 0.066 Q1 1 0.5159 0.7160 0.4378 11.00000 0.05 0.58 Q2 1 0.6830 0.2969 0.5561 11.00000 0.05 0.56 Q3 1 0.5000 0.2653 0.5356 11.00000 0.05 0.37 Q4 1 0.5992 0.3870 0.5631 11.00000 0.05 0.36 Q5 1 0.5930 0.1948 0.5627 11.00000 0.05 0.36 Q6 1 0.7849 0.3089 0.5626 11.00000 0.05 0.36 Q7 1 0.5967 0.7085 0.3881 11.00000 0.05 0.34 Q8 1 0.5787 0.7047 0.4745 11.00000 0.05 0.32 Q9 1 0.7418 0.2874 0.6048 11.00000 0.05 0.31 Q10 1 0.6389 0.2828 0.6067 11.00000 0.05 0.31 Q11 1 0.7736 0.2861 0.4996 11.00000 0.05 0.29 Q12 1 0.6504 0.3315 0.5929 11.00000 0.05 0.29 Q13 1 0.7015 0.2994 0.6315 11.00000 0.05 0.27 Q14 1 0.6397 0.3643 0.5502 11.00000 0.05 0.27 Q15 1 0.5218 0.2081 0.3635 11.00000 0.05 0.27 Q16 1 0.7435 0.2800 0.4595 11.00000 0.05 0.26 Q17 1 0.5429 0.6776 0.5037 11.00000 0.05 0.25 Q18 1 0.5216 0.6662 0.5110 11.00000 0.05 0.24 Q19 1 0.6516 0.9376 0.2404 11.00000 0.05 0.24 Q20 1 0.8137 0.6243 0.5544 11.00000 0.05 0.24 REM The information below was added by Olex2. REM REM R1 = 0.0328 for 7705 Fo > 4sig(Fo) and 0.0349 for all 27643 data REM n/a parameters refined using n/a restraints REM Highest difference peak 0.58, deepest hole -1.10 REM Mean Shift 0, Max Shift 0.003. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0349 REM R1_gt = 0.0328 REM wR_ref = 0.1128 REM GOOF = 0.962 REM Shift_max = 0.003 REM Shift_mean = 0 REM Reflections_all = 27643 REM Reflections_gt = 7705 REM Parameters = n/a REM Hole = -1.10 REM Peak = 0.58 REM Flack = n/a ; _cod_data_source_file c9sc06060j2.cif _cod_data_source_block exp_28 _cod_database_code 1557458 _shelx_shelxl_version_number 2018/1 _chemical_oxdiff_formula C36H50Ag1Li1N2O3 _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. ; _reflns_odcompleteness_completeness 99.99 _reflns_odcompleteness_iscentric 1 _reflns_odcompleteness_theta 68.13 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C00F(H00F), C00G(H00G), C00J(H00J), C00N(H00O) 2.b Secondary CH2 refined with riding coordinates: C00Q(H00R,H00S), C00V(H00,HC), C012(H01A,H01B), C015(H01C,H01D) 2.c Aromatic/amide H refined with riding coordinates: C00C(H00C), C00E(H00E), C00H(H00H), C00I(H00I), C00L(H00L), C00O(H00P), C00P(H00Q), C00R(H00T), C00Y(H2AA), C00Z(H3AA), C010(H010), C011(H011), C013(H013), C014(H014), C017(H017), C018(H018), C019(H019), C01A(H01H), C01B(H01I), C01C(H01J) 2.d Idealised Me refined as rotating group: C00K(H00A,H00B,H00D), C00M(H00K,H00M,H00N), C00S(H00U,H00V,H00W), C00T(H00X, H00Y,H), C00U(H00Z,HA,HB), C00W(H0AA,HD,HE), C00X(H1AA,HF,HG), C016(H01E,H01F, H01G) ; _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 2.233 _oxdiff_exptl_absorpt_empirical_full_min 0.683 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 Ag01 Ag 0.58514(2) 0.29356(2) 0.56115(2) 0.02493(8) Uani 1 1 d . . . . . O002 O 0.55725(12) 0.52234(9) 0.35837(7) 0.0328(3) Uani 1 1 d . . . . . O003 O 0.66568(13) 0.34961(10) 0.40150(7) 0.0342(3) Uani 1 1 d . . . . . O004 O 0.70324(13) 0.52663(10) 0.48919(7) 0.0358(3) Uani 1 1 d . . . . . N005 N 0.48897(13) 0.61585(11) 0.28408(7) 0.0260(3) Uani 1 1 d . . . . . N006 N 0.66261(14) 0.19907(10) 0.40876(8) 0.0245(3) Uani 1 1 d . . . . . C20 C 0.74554(17) 0.30328(12) 0.54018(10) 0.0252(4) Uani 1 1 d . . . . . C008 C 0.57287(16) 0.72342(14) 0.41461(9) 0.0247(4) Uani 1 1 d . . . . . C009 C 0.55004(15) 0.59969(13) 0.33603(9) 0.0259(4) Uani 1 1 d . . . . . C00A C 0.78106(17) 0.28634(12) 0.48125(10) 0.0258(4) Uani 1 1 d . . . . . C00B C 0.61480(15) 0.67416(13) 0.36645(8) 0.0243(3) Uani 1 1 d . . . . . C00C C 0.82905(16) 0.31842(14) 0.58632(10) 0.0296(4) Uani 1 1 d . . . . . H00C H 0.810252 0.331580 0.626965 0.035 Uiso 1 1 calc R . . . . C00D C 0.69875(16) 0.27958(13) 0.42815(9) 0.0259(4) Uani 1 1 d . . . . . C00E C 0.64434(18) 0.78680(12) 0.44273(10) 0.0281(4) Uani 1 1 d . . . . . H00E H 0.620836 0.821810 0.475772 0.034 Uiso 1 1 calc R . . . . C00F C 0.69908(17) 0.11521(13) 0.44033(10) 0.0296(4) Uani 1 1 d . . . . . H00F H 0.743402 0.133169 0.478272 0.036 Uiso 1 1 calc R . . . . C00G C 0.58505(17) 0.19071(14) 0.35445(9) 0.0289(4) Uani 1 1 d . . . . . H00G H 0.570144 0.125147 0.348945 0.035 Uiso 1 1 calc R . . . . C00H C 0.74774(18) 0.80038(13) 0.42427(11) 0.0309(4) Uani 1 1 d . . . . . H00H H 0.792918 0.843767 0.444765 0.037 Uiso 1 1 calc R . . . . C00I C 0.71821(17) 0.68701(15) 0.34732(10) 0.0294(4) Uani 1 1 d . . . . . H00I H 0.742831 0.652004 0.314584 0.035 Uiso 1 1 calc R . . . . C00J C 0.43617(17) 0.54042(14) 0.24903(9) 0.0317(4) Uani 1 1 d . . . . . H00J H 0.400463 0.567051 0.210795 0.038 Uiso 1 1 calc R . . . . C00K C 0.52025(19) 0.72110(15) 0.19848(10) 0.0340(4) Uani 1 1 d . . . . . H00A H 0.597065 0.707457 0.203016 0.051 Uiso 1 1 calc GR . . . . H00B H 0.510120 0.783467 0.184991 0.051 Uiso 1 1 calc GR . . . . H00D H 0.485171 0.680798 0.167787 0.051 Uiso 1 1 calc GR . . . . C00L C 0.88922(18) 0.28138(14) 0.46876(11) 0.0309(4) Uani 1 1 d . . . . . H00L H 0.909101 0.269123 0.428196 0.037 Uiso 1 1 calc R . . . . C00M C 0.6321(2) 0.22282(18) 0.29532(10) 0.0399(5) Uani 1 1 d . . . . . H00K H 0.643806 0.287823 0.297513 0.060 Uiso 1 1 calc GR . . . . H00M H 0.582124 0.208862 0.260020 0.060 Uiso 1 1 calc GR . . . . H00N H 0.700540 0.192401 0.290452 0.060 Uiso 1 1 calc GR . . . . C00N C 0.47101(18) 0.70798(12) 0.26026(10) 0.0283(4) Uani 1 1 d . . . . . H00O H 0.508676 0.749935 0.290339 0.034 Uiso 1 1 calc R . . . . C00O C 0.93706(17) 0.31491(15) 0.57491(10) 0.0333(4) Uani 1 1 d . . . . . H00P H 0.990064 0.326437 0.607248 0.040 Uiso 1 1 calc R . . . . C00P C 0.78503(15) 0.75084(15) 0.37609(10) 0.0326(4) Uani 1 1 d . . . . . H00Q H 0.855166 0.760451 0.363014 0.039 Uiso 1 1 calc R . . . . C00Q C 0.8180(2) 0.53188(16) 0.50060(11) 0.0409(5) Uani 1 1 d . . . . . H00R H 0.849422 0.573011 0.470924 0.049 Uiso 1 1 calc R . . . . H00S H 0.851093 0.471886 0.497128 0.049 Uiso 1 1 calc R . . . . C00R C 0.96752(18) 0.29463(13) 0.51646(12) 0.0341(5) Uani 1 1 d . . . . . H00T H 1.041317 0.289782 0.508931 0.041 Uiso 1 1 calc R . . . . C00S C 0.47778(17) 0.23531(18) 0.36488(11) 0.0384(5) Uani 1 1 d . . . . . H00U H 0.454102 0.217327 0.405144 0.058 Uiso 1 1 calc GR . . . . H00V H 0.424298 0.216535 0.332480 0.058 Uiso 1 1 calc GR . . . . H00W H 0.486068 0.300694 0.363718 0.058 Uiso 1 1 calc GR . . . . C00T C 0.3478(2) 0.49635(17) 0.28391(11) 0.0417(5) Uani 1 1 d . . . . . H00X H 0.380076 0.463257 0.319372 0.063 Uiso 1 1 calc GR . . . . H00Y H 0.306958 0.454807 0.256459 0.063 Uiso 1 1 calc GR . . . . H H 0.299724 0.542733 0.298252 0.063 Uiso 1 1 calc GR . . . . C00U C 0.77147(19) 0.06127(15) 0.40044(12) 0.0396(5) Uani 1 1 d . . . . . H00Z H 0.731081 0.043489 0.362252 0.059 Uiso 1 1 calc GR . . . . HA H 0.796932 0.007496 0.422847 0.059 Uiso 1 1 calc GR . . . . HB H 0.832982 0.098130 0.390542 0.059 Uiso 1 1 calc GR . . . . C00V C 0.6509(2) 0.57087(16) 0.53820(10) 0.0406(5) Uani 1 1 d . . . . . H00 H 0.621730 0.526374 0.566479 0.049 Uiso 1 1 calc R . . . . HC H 0.591675 0.609616 0.521337 0.049 Uiso 1 1 calc R . . . . C00W C 0.60465(19) 0.06096(15) 0.46122(11) 0.0394(5) Uani 1 1 d . . . . . H0AA H 0.560342 0.099109 0.486047 0.059 Uiso 1 1 calc GR . . . . HD H 0.631421 0.009755 0.485983 0.059 Uiso 1 1 calc GR . . . . HE H 0.561466 0.039127 0.425065 0.059 Uiso 1 1 calc GR . . . . C00X C 0.5183(2) 0.47268(15) 0.22808(10) 0.0401(5) Uani 1 1 d . . . . . H1AA H 0.573427 0.504241 0.206397 0.060 Uiso 1 1 calc GR . . . . HF H 0.482263 0.428737 0.200337 0.060 Uiso 1 1 calc GR . . . . HG H 0.551893 0.441669 0.264097 0.060 Uiso 1 1 calc GR . . . . C00Y C 0.8873(2) -0.07729(18) 0.56623(11) 0.0477(6) Uani 1 1 d . . . . . H2AA H 0.935528 -0.120584 0.551820 0.057 Uiso 1 1 calc R . . . . C00Z C 0.8444(2) 0.07535(16) 0.58774(11) 0.0414(5) Uani 1 1 d . . . . . H3AA H 0.862669 0.137253 0.587954 0.050 Uiso 1 1 calc R . . . . C010 C 0.9142(2) 0.01335(18) 0.56687(10) 0.0439(5) Uani 1 1 d . . . . . H010 H 0.980973 0.032189 0.552825 0.053 Uiso 1 1 calc R . . . . C011 C 0.4883(2) 1.01020(18) 0.20918(12) 0.0455(5) Uani 1 1 d . . . . . H011 H 0.430402 1.043013 0.189718 0.055 Uiso 1 1 calc R . . . . C012 C 0.7381(2) 0.62631(15) 0.57105(11) 0.0452(6) Uani 1 1 d . . . . . H01A H 0.746805 0.684881 0.550447 0.054 Uiso 1 1 calc R . . . . H01B H 0.723423 0.636616 0.614651 0.054 Uiso 1 1 calc R . . . . C013 C 0.7891(2) -0.10404(16) 0.58689(11) 0.0464(6) Uani 1 1 d . . . . . H013 H 0.769838 -0.165755 0.586407 0.056 Uiso 1 1 calc R . . . . C014 C 0.5808(2) 0.99788(17) 0.17969(11) 0.0436(5) Uani 1 1 d . . . . . H014 H 0.586370 1.021934 0.139586 0.052 Uiso 1 1 calc R . . . . C015 C 0.8351(2) 0.56763(17) 0.56572(11) 0.0437(5) Uani 1 1 d . . . . . H01C H 0.837060 0.518367 0.596320 0.052 Uiso 1 1 calc R . . . . H01D H 0.902223 0.602833 0.571118 0.052 Uiso 1 1 calc R . . . . C016 C 0.35193(18) 0.73245(16) 0.25701(11) 0.0383(5) Uani 1 1 d . . . . . H01E H 0.312205 0.691788 0.228405 0.057 Uiso 1 1 calc GR . . . . H01F H 0.342685 0.794418 0.242497 0.057 Uiso 1 1 calc GR . . . . H01G H 0.324614 0.726819 0.298046 0.057 Uiso 1 1 calc GR . . . . C017 C 0.7198(2) -0.04082(17) 0.60805(11) 0.0436(5) Uani 1 1 d . . . . . H017 H 0.652827 -0.058880 0.622320 0.052 Uiso 1 1 calc R . . . . C018 C 0.7478(2) 0.04838(17) 0.60842(11) 0.0425(5) Uani 1 1 d . . . . . H018 H 0.699997 0.091836 0.623103 0.051 Uiso 1 1 calc R . . . . C019 C 0.6574(3) 0.91643(17) 0.26543(14) 0.0572(8) Uani 1 1 d . . . . . H019 H 0.715904 0.884222 0.284806 0.069 Uiso 1 1 calc R . . . . C01A C 0.5655(3) 0.92796(18) 0.29545(12) 0.0637(10) Uani 1 1 d . . . . . H01H H 0.560410 0.903977 0.335615 0.076 Uiso 1 1 calc R . . . . C01B C 0.6655(2) 0.95109(17) 0.20749(14) 0.0502(6) Uani 1 1 d . . . . . H01I H 0.729279 0.942811 0.186711 0.060 Uiso 1 1 calc R . . . . C01C C 0.4797(3) 0.9749(2) 0.26705(13) 0.0541(7) Uani 1 1 d . . . . . H01J H 0.415472 0.982505 0.287521 0.065 Uiso 1 1 calc R . . . . Li1D Li 0.6379(3) 0.4664(2) 0.42057(17) 0.0355(8) 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 Ag01 0.02382(11) 0.02792(11) 0.02333(11) -0.00278(4) 0.00362(7) -0.00064(4) O002 0.0429(8) 0.0274(7) 0.0271(7) 0.0013(5) -0.0053(6) 0.0006(6) O003 0.0462(8) 0.0248(7) 0.0309(7) 0.0019(6) -0.0023(6) 0.0000(6) O004 0.0467(8) 0.0310(7) 0.0285(7) -0.0033(6) -0.0057(6) -0.0003(6) N005 0.0303(8) 0.0265(8) 0.0209(7) 0.0003(6) -0.0011(6) -0.0010(6) N006 0.0269(8) 0.0244(8) 0.0222(8) -0.0005(5) 0.0008(6) -0.0018(6) C20 0.0221(9) 0.0230(8) 0.0306(10) -0.0027(7) 0.0037(8) -0.0023(6) C008 0.0223(9) 0.0299(8) 0.0221(9) 0.0014(7) 0.0041(7) 0.0014(7) C009 0.0276(9) 0.0272(9) 0.0233(8) 0.0000(7) 0.0041(7) 0.0015(7) C00A 0.0267(10) 0.0208(9) 0.0299(10) -0.0014(6) 0.0026(8) -0.0035(6) C00B 0.0263(8) 0.0263(9) 0.0201(8) 0.0018(7) 0.0003(7) 0.0025(7) C00C 0.0301(10) 0.0282(9) 0.0301(10) -0.0030(8) -0.0005(8) -0.0027(8) C00D 0.0264(9) 0.0262(9) 0.0255(9) -0.0021(7) 0.0056(7) -0.0019(7) C00E 0.0327(10) 0.0273(9) 0.0242(9) 0.0004(6) 0.0014(8) -0.0004(7) C00F 0.0335(10) 0.0233(9) 0.0314(10) 0.0016(7) -0.0032(8) -0.0024(7) C00G 0.0300(10) 0.0305(9) 0.0256(9) 0.0001(7) -0.0025(8) -0.0042(8) C00H 0.0304(11) 0.0313(10) 0.0300(11) 0.0049(7) -0.0056(8) -0.0038(7) C00I 0.0269(10) 0.0349(9) 0.0265(10) 0.0038(8) 0.0031(8) 0.0041(8) C00J 0.0381(10) 0.0321(10) 0.0239(9) -0.0011(7) -0.0041(8) -0.0042(8) C00K 0.0405(12) 0.0365(10) 0.0250(10) 0.0031(8) 0.0017(8) -0.0065(9) C00L 0.0295(10) 0.0279(9) 0.0361(11) -0.0029(8) 0.0081(9) -0.0032(7) C00M 0.0437(13) 0.0518(12) 0.0243(10) -0.0016(9) 0.0038(9) -0.0066(10) C00N 0.0326(11) 0.0273(10) 0.0247(10) 0.0024(6) -0.0014(8) 0.0004(7) C00O 0.0289(10) 0.0310(9) 0.0392(11) -0.0046(8) -0.0043(8) -0.0035(8) C00P 0.0238(9) 0.0406(11) 0.0334(10) 0.0058(8) 0.0011(7) -0.0004(8) C00Q 0.0457(12) 0.0369(11) 0.0403(12) -0.0041(9) 0.0035(9) -0.0093(9) C00R 0.0236(10) 0.0311(11) 0.0478(14) -0.0030(8) 0.0054(9) -0.0045(7) C00S 0.0280(10) 0.0485(12) 0.0384(11) 0.0002(10) -0.0001(8) -0.0004(9) C00T 0.0453(12) 0.0441(12) 0.0349(11) 0.0026(9) -0.0034(9) -0.0154(10) C00U 0.0391(11) 0.0294(10) 0.0497(13) -0.0063(9) -0.0008(10) 0.0033(8) C00V 0.0516(13) 0.0397(11) 0.0304(10) -0.0010(9) 0.0018(9) 0.0016(10) C00W 0.0451(12) 0.0349(11) 0.0379(11) 0.0080(9) -0.0006(9) -0.0126(9) C00X 0.0540(13) 0.0342(11) 0.0312(10) -0.0068(8) -0.0036(9) 0.0023(9) C00Y 0.0637(16) 0.0496(14) 0.0286(11) -0.0043(9) -0.0052(10) 0.0198(12) C00Z 0.0546(14) 0.0328(11) 0.0358(11) 0.0042(9) -0.0060(10) -0.0034(10) C010 0.0448(12) 0.0583(14) 0.0284(11) 0.0035(9) 0.0003(9) -0.0019(11) C011 0.0372(11) 0.0517(14) 0.0465(13) -0.0024(11) -0.0046(10) 0.0032(10) C012 0.0743(17) 0.0316(11) 0.0294(10) -0.0019(8) 0.0011(10) -0.0071(10) C013 0.0757(18) 0.0313(11) 0.0299(11) 0.0015(8) -0.0128(11) -0.0057(11) C014 0.0501(13) 0.0451(12) 0.0357(11) 0.0100(9) 0.0030(10) -0.0004(10) C015 0.0547(14) 0.0404(12) 0.0347(11) 0.0035(9) -0.0062(10) -0.0106(10) C016 0.0359(11) 0.0373(11) 0.0415(12) 0.0039(9) 0.0009(9) 0.0060(9) C017 0.0455(12) 0.0509(13) 0.0338(11) 0.0001(10) -0.0021(9) -0.0085(10) C018 0.0473(12) 0.0452(13) 0.0340(11) -0.0029(9) -0.0037(9) 0.0081(10) C019 0.0754(19) 0.0333(12) 0.0585(17) -0.0034(11) -0.0279(15) 0.0074(12) C01A 0.124(3) 0.0384(13) 0.0264(11) 0.0019(10) -0.0121(15) -0.0287(16) C01B 0.0417(12) 0.0434(13) 0.0654(17) -0.0034(12) 0.0035(12) 0.0022(10) C01C 0.0626(16) 0.0596(16) 0.0423(14) -0.0190(12) 0.0205(12) -0.0249(13) Li1D 0.046(2) 0.0267(16) 0.0321(17) -0.0011(13) -0.0093(15) 0.0000(14) 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' Li Li 0.0008 0.0003 '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' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 2 -9 2 0.1473 -6 1 -10 0.0960 -4 8 -5 0.0808 -1 10 1 0.0894 6 -1 10 0.0661 0 -9 -3 0.1329 6 1 -10 0.0608 -2 9 6 0.0796 -6 -5 8 0.1282 -2 1 14 0.0726 0 -8 8 0.1269 2 0 13 0.0679 -2 1 -13 0.0992 1 8 8 0.0807 -7 1 -4 0.0935 -5 8 -1 0.0840 -8 2 3 0.0729 -6 1 10 0.0735 7 0 6 0.0611 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 C20 Ag01 C008 176.39(7) . 3_666 ? C009 O002 Li1D 136.65(17) . . ? C00D O003 Li1D 138.68(18) . . ? C00Q O004 C00V 109.95(16) . . ? C00Q O004 Li1D 122.55(19) . . ? C00V O004 Li1D 127.48(19) . . ? C009 N005 C00J 120.30(16) . . ? C009 N005 C00N 121.72(16) . . ? C00N N005 C00J 117.98(15) . . ? C00D N006 C00F 121.40(17) . . ? C00D N006 C00G 121.00(16) . . ? C00F N006 C00G 117.59(15) . . ? C00A C20 Ag01 123.42(15) . . ? C00A C20 C00C 114.34(19) . . ? C00C C20 Ag01 121.92(16) . . ? C00B C008 Ag01 121.85(14) . 3_666 ? C00B C008 C00E 114.54(18) . . ? C00E C008 Ag01 123.55(15) . 3_666 ? O002 C009 N005 120.93(17) . . ? O002 C009 C00B 119.09(16) . . ? N005 C009 C00B 119.92(16) . . ? C20 C00A C00D 118.22(19) . . ? C00L C00A C20 123.6(2) . . ? C00L C00A C00D 118.0(2) . . ? C008 C00B C009 119.80(17) . . ? C00I C00B C008 123.15(18) . . ? C00I C00B C009 116.92(17) . . ? C20 C00C H00C 118.4 . . ? C00O C00C C20 123.1(2) . . ? C00O C00C H00C 118.4 . . ? O003 C00D N006 120.42(18) . . ? O003 C00D C00A 119.38(17) . . ? N006 C00D C00A 120.19(17) . . ? C008 C00E H00E 118.5 . . ? C00H C00E C008 123.0(2) . . ? C00H C00E H00E 118.5 . . ? N006 C00F H00F 107.1 . . ? N006 C00F C00U 110.88(18) . . ? N006 C00F C00W 111.36(17) . . ? C00U C00F H00F 107.1 . . ? C00U C00F C00W 112.99(18) . . ? C00W C00F H00F 107.1 . . ? N006 C00G H00G 106.5 . . ? N006 C00G C00M 112.17(17) . . ? N006 C00G C00S 112.31(17) . . ? C00M C00G H00G 106.5 . . ? C00M C00G C00S 112.30(19) . . ? C00S C00G H00G 106.5 . . ? C00E C00H H00H 119.9 . . ? C00P C00H C00E 120.29(19) . . ? C00P C00H H00H 119.9 . . ? C00B C00I H00I 120.0 . . ? C00P C00I C00B 120.1(2) . . ? C00P C00I H00I 120.0 . . ? N005 C00J H00J 106.6 . . ? N005 C00J C00T 112.37(17) . . ? N005 C00J C00X 111.52(17) . . ? C00T C00J H00J 106.6 . . ? C00T C00J C00X 112.66(19) . . ? C00X C00J H00J 106.6 . . ? H00A C00K H00B 109.5 . . ? H00A C00K H00D 109.5 . . ? H00B C00K H00D 109.5 . . ? C00N C00K H00A 109.5 . . ? C00N C00K H00B 109.5 . . ? C00N C00K H00D 109.5 . . ? C00A C00L H00L 120.4 . . ? C00R C00L C00A 119.3(2) . . ? C00R C00L H00L 120.4 . . ? C00G C00M H00K 109.5 . . ? C00G C00M H00M 109.5 . . ? C00G C00M H00N 109.5 . . ? H00K C00M H00M 109.5 . . ? H00K C00M H00N 109.5 . . ? H00M C00M H00N 109.5 . . ? N005 C00N C00K 111.50(17) . . ? N005 C00N H00O 107.2 . . ? N005 C00N C016 111.24(17) . . ? C00K C00N H00O 107.2 . . ? C00K C00N C016 112.07(18) . . ? C016 C00N H00O 107.2 . . ? C00C C00O H00P 120.0 . . ? C00R C00O C00C 120.07(19) . . ? C00R C00O H00P 120.0 . . ? C00H C00P C00I 118.91(19) . . ? C00H C00P H00Q 120.5 . . ? C00I C00P H00Q 120.5 . . ? O004 C00Q H00R 110.8 . . ? O004 C00Q H00S 110.8 . . ? O004 C00Q C015 105.0(2) . . ? H00R C00Q H00S 108.8 . . ? C015 C00Q H00R 110.8 . . ? C015 C00Q H00S 110.8 . . ? C00L C00R H00T 120.2 . . ? C00O C00R C00L 119.6(2) . . ? C00O C00R H00T 120.2 . . ? C00G C00S H00U 109.5 . . ? C00G C00S H00V 109.5 . . ? C00G C00S H00W 109.5 . . ? H00U C00S H00V 109.5 . . ? H00U C00S H00W 109.5 . . ? H00V C00S H00W 109.5 . . ? C00J C00T H00X 109.5 . . ? C00J C00T H00Y 109.5 . . ? C00J C00T H 109.5 . . ? H00X C00T H00Y 109.5 . . ? H00X C00T H 109.5 . . ? H00Y C00T H 109.5 . . ? C00F C00U H00Z 109.5 . . ? C00F C00U HA 109.5 . . ? C00F C00U HB 109.5 . . ? H00Z C00U HA 109.5 . . ? H00Z C00U HB 109.5 . . ? HA C00U HB 109.5 . . ? O004 C00V H00 110.8 . . ? O004 C00V HC 110.8 . . ? O004 C00V C012 104.5(2) . . ? H00 C00V HC 108.9 . . ? C012 C00V H00 110.8 . . ? C012 C00V HC 110.8 . . ? C00F C00W H0AA 109.5 . . ? C00F C00W HD 109.5 . . ? C00F C00W HE 109.5 . . ? H0AA C00W HD 109.5 . . ? H0AA C00W HE 109.5 . . ? HD C00W HE 109.5 . . ? C00J C00X H1AA 109.5 . . ? C00J C00X HF 109.5 . . ? C00J C00X HG 109.5 . . ? H1AA C00X HF 109.5 . . ? H1AA C00X HG 109.5 . . ? HF C00X HG 109.5 . . ? C010 C00Y H2AA 120.3 . . ? C010 C00Y C013 119.5(2) . . ? C013 C00Y H2AA 120.3 . . ? C010 C00Z H3AA 119.9 . . ? C010 C00Z C018 120.2(2) . . ? C018 C00Z H3AA 119.9 . . ? C00Y C010 H010 120.0 . . ? C00Z C010 C00Y 120.0(2) . . ? C00Z C010 H010 120.0 . . ? C014 C011 H011 120.1 . . ? C014 C011 C01C 119.8(2) . . ? C01C C011 H011 120.1 . . ? C00V C012 H01A 111.4 . . ? C00V C012 H01B 111.4 . . ? H01A C012 H01B 109.3 . . ? C015 C012 C00V 101.90(19) . . ? C015 C012 H01A 111.4 . . ? C015 C012 H01B 111.4 . . ? C00Y C013 H013 120.1 . . ? C017 C013 C00Y 119.9(2) . . ? C017 C013 H013 120.1 . . ? C011 C014 H014 119.6 . . ? C011 C014 C01B 120.7(2) . . ? C01B C014 H014 119.6 . . ? C00Q C015 H01C 111.3 . . ? C00Q C015 H01D 111.3 . . ? C012 C015 C00Q 102.17(19) . . ? C012 C015 H01C 111.3 . . ? C012 C015 H01D 111.3 . . ? H01C C015 H01D 109.2 . . ? C00N C016 H01E 109.5 . . ? C00N C016 H01F 109.5 . . ? C00N C016 H01G 109.5 . . ? H01E C016 H01F 109.5 . . ? H01E C016 H01G 109.5 . . ? H01F C016 H01G 109.5 . . ? C013 C017 H017 120.1 . . ? C018 C017 C013 119.8(2) . . ? C018 C017 H017 120.1 . . ? C00Z C018 H018 119.7 . . ? C017 C018 C00Z 120.6(2) . . ? C017 C018 H018 119.7 . . ? C01A C019 H019 119.8 . . ? C01A C019 C01B 120.4(3) . . ? C01B C019 H019 119.8 . . ? C019 C01A H01H 120.1 . . ? C019 C01A C01C 119.9(2) . . ? C01C C01A H01H 120.1 . . ? C014 C01B H01I 120.2 . . ? C019 C01B C014 119.6(3) . . ? C019 C01B H01I 120.2 . . ? C011 C01C C01A 119.6(3) . . ? C011 C01C H01J 120.2 . . ? C01A C01C H01J 120.2 . . ? O002 Li1D O004 123.9(2) . . ? O003 Li1D O002 111.64(19) . . ? O003 Li1D O004 123.7(2) . . ? 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 Ag01 C20 2.090(2) . ? Ag01 C008 2.092(2) 3_666 ? O002 C009 1.251(2) . ? O002 Li1D 1.834(4) . ? O003 C00D 1.251(3) . ? O003 Li1D 1.827(4) . ? O004 C00Q 1.441(3) . ? O004 C00V 1.446(3) . ? O004 Li1D 1.882(4) . ? N005 C009 1.344(2) . ? N005 C00J 1.488(2) . ? N005 C00N 1.479(2) . ? N006 C00D 1.340(2) . ? N006 C00F 1.483(2) . ? N006 C00G 1.484(2) . ? C20 C00A 1.407(3) . ? C20 C00C 1.418(3) . ? C008 C00B 1.408(3) . ? C008 C00E 1.411(3) . ? C009 C00B 1.501(3) . ? C00A C00D 1.499(3) . ? C00A C00L 1.398(3) . ? C00B C00I 1.397(3) . ? C00C H00C 0.9500 . ? C00C C00O 1.390(3) . ? C00E H00E 0.9500 . ? C00E C00H 1.393(3) . ? C00F H00F 1.0000 . ? C00F C00U 1.523(3) . ? C00F C00W 1.524(3) . ? C00G H00G 1.0000 . ? C00G C00M 1.526(3) . ? C00G C00S 1.526(3) . ? C00H H00H 0.9500 . ? C00H C00P 1.387(3) . ? C00I H00I 0.9500 . ? C00I C00P 1.387(3) . ? C00J H00J 1.0000 . ? C00J C00T 1.528(3) . ? C00J C00X 1.530(3) . ? C00K H00A 0.9800 . ? C00K H00B 0.9800 . ? C00K H00D 0.9800 . ? C00K C00N 1.527(3) . ? C00L H00L 0.9500 . ? C00L C00R 1.393(3) . ? C00M H00K 0.9800 . ? C00M H00M 0.9800 . ? C00M H00N 0.9800 . ? C00N H00O 1.0000 . ? C00N C016 1.529(3) . ? C00O H00P 0.9500 . ? C00O C00R 1.384(3) . ? C00P H00Q 0.9500 . ? C00Q H00R 0.9900 . ? C00Q H00S 0.9900 . ? C00Q C015 1.516(3) . ? C00R H00T 0.9500 . ? C00S H00U 0.9800 . ? C00S H00V 0.9800 . ? C00S H00W 0.9800 . ? C00T H00X 0.9800 . ? C00T H00Y 0.9800 . ? C00T H 0.9800 . ? C00U H00Z 0.9800 . ? C00U HA 0.9800 . ? C00U HB 0.9800 . ? C00V H00 0.9900 . ? C00V HC 0.9900 . ? C00V C012 1.510(3) . ? C00W H0AA 0.9800 . ? C00W HD 0.9800 . ? C00W HE 0.9800 . ? C00X H1AA 0.9800 . ? C00X HF 0.9800 . ? C00X HG 0.9800 . ? C00Y H2AA 0.9500 . ? C00Y C010 1.391(4) . ? C00Y C013 1.393(4) . ? C00Z H3AA 0.9500 . ? C00Z C010 1.368(4) . ? C00Z C018 1.375(4) . ? C010 H010 0.9500 . ? C011 H011 0.9500 . ? C011 C014 1.370(4) . ? C011 C01C 1.375(4) . ? C012 H01A 0.9900 . ? C012 H01B 0.9900 . ? C012 C015 1.505(4) . ? C013 H013 0.9500 . ? C013 C017 1.379(4) . ? C014 H014 0.9500 . ? C014 C01B 1.374(4) . ? C015 H01C 0.9900 . ? C015 H01D 0.9900 . ? C016 H01E 0.9800 . ? C016 H01F 0.9800 . ? C016 H01G 0.9800 . ? C017 H017 0.9500 . ? C017 C018 1.374(4) . ? C018 H018 0.9500 . ? C019 H019 0.9500 . ? C019 C01A 1.368(5) . ? C019 C01B 1.372(4) . ? C01A H01H 0.9500 . ? C01A C01C 1.391(5) . ? C01B H01I 0.9500 . ? C01C H01J 0.9500 . ? loop_ _exptl_oxdiff_crystal_face_indexfrac_h _exptl_oxdiff_crystal_face_indexfrac_k _exptl_oxdiff_crystal_face_indexfrac_l _exptl_oxdiff_crystal_face_x _exptl_oxdiff_crystal_face_y _exptl_oxdiff_crystal_face_z 2.2512 -9.1678 1.9345 -0.1119 -0.4611 0.8803 -5.5830 0.7488 -9.5245 0.2312 0.9669 0.1079 -3.8572 7.6254 -5.0523 0.1747 0.7251 -0.6661 -0.8001 9.6150 0.6791 0.0531 0.2150 -0.9752 5.5773 -0.5108 9.5658 -0.2305 -0.9640 -0.1325 -0.1421 -9.3982 -3.2943 -0.0503 0.0104 0.9987 5.8965 1.4861 -10.1092 -0.9710 0.2325 -0.0552 -1.6380 8.5269 6.1865 0.3401 -0.0798 -0.9370 -5.9580 -5.0341 8.0349 0.9234 -0.1784 0.4442 -1.9721 0.9623 14.0046 0.6930 -0.6826 -0.2813 0.0386 -8.0083 7.9812 0.3228 -0.6472 0.6951 2.0209 -0.0194 12.9712 0.2522 -0.9143 -0.2009 -2.0238 1.0184 -12.9698 -0.2574 0.9352 0.0999 0.9900 7.9789 7.9953 0.1376 -0.3791 -0.9297 -6.9965 0.9808 -3.9371 0.5728 0.7342 0.0163 -5.0152 7.9749 -0.9466 0.4369 0.5661 -0.7505 -7.9840 1.9614 3.0659 0.9167 0.4034 -0.1748 -5.9717 0.9555 10.0414 0.9629 -0.1723 -0.1900 6.9974 0.0140 5.9366 -0.5076 -0.8331 -0.1456