#------------------------------------------------------------------------------ #$Date: 2020-03-04 09:48:00 +0200 (Wed, 04 Mar 2020) $ #$Revision: 248753 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/74/1557456.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_1557456 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 'C46 H88 Ag2 Li4 N6 O2' _chemical_formula_sum 'C46 H88 Ag2 Li4 N6 O2' _chemical_formula_weight 1000.72 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2016/6 _audit_update_record ; 2019-05-30 deposited with the CCDC. 2020-01-03 downloaded from the CCDC. ; _cell_angle_alpha 86.881(2) _cell_angle_beta 79.282(2) _cell_angle_gamma 83.876(2) _cell_formula_units_Z 1 _cell_length_a 8.3861(3) _cell_length_b 11.5994(4) _cell_length_c 14.0500(5) _cell_measurement_reflns_used 9905 _cell_measurement_temperature 180(2) _cell_measurement_theta_max 66.6 _cell_measurement_theta_min 3.203 _cell_volume 1334.35(8) _computing_cell_refinement 'SAINT (Bruker, 2016)' _computing_data_collection 'APEX3 (Bruker, 2016)' _computing_data_reduction SAINT _computing_molecular_graphics 'Mercury (Macrae et al., 2008)' _computing_publication_material 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_refinement 'SHELXL-2016/6 (Sheldrick, 2016)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 180(2) _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _diffrn_measurement_device_type 'Bruker D8-QUEST PHOTON-100' _diffrn_measurement_method 'Thin slice \w and \f scans' _diffrn_radiation_source 'Incoatec I\mS Cu microsource' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0325 _diffrn_reflns_av_unetI/netI 0.0336 _diffrn_reflns_Laue_measured_fraction_full 0.988 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 14620 _diffrn_reflns_point_group_measured_fraction_full 0.988 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 66.637 _diffrn_reflns_theta_max 66.637 _diffrn_reflns_theta_min 3.203 _exptl_absorpt_coefficient_mu 6.165 _exptl_absorpt_correction_T_max 0.7528 _exptl_absorpt_correction_T_min 0.5959 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; multi-scan from symmetry-related measurements 'SADABS (Bruker, 2016)' ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.245 _exptl_crystal_description block _exptl_crystal_F_000 528 _exptl_crystal_size_max 0.103 _exptl_crystal_size_mid 0.080 _exptl_crystal_size_min 0.050 _refine_diff_density_max 0.486 _refine_diff_density_min -0.377 _refine_diff_density_rms 0.068 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 307 _refine_ls_number_reflns 4655 _refine_ls_number_restraints 256 _refine_ls_restrained_S_all 1.084 _refine_ls_R_factor_all 0.0330 _refine_ls_R_factor_gt 0.0272 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0286P)^2^+0.8500P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0633 _refine_ls_wR_factor_ref 0.0673 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4220 _reflns_number_total 4655 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc06060j2.cif _cod_data_source_block aw1709 _cod_database_code 1557456 _shelx_shelxl_version_number 2016/6 _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_min 0.569 _shelx_estimated_absorpt_t_max 0.748 _shelx_res_file ; TITL aw1709 in P-1 aw1709.res created by SHELXL-2016/6 at 11:23:53 on 02-Jun-2017 CELL 1.54184 8.3861 11.5994 14.0500 86.881 79.282 83.876 ZERR 1.000 0.0003 0.0004 0.0005 0.002 0.002 0.002 LATT 1 SFAC C H LI N O AG UNIT 46 88 4 6 2 2 TEMP -93.150 SIZE 0.05 0.08 0.103 L.S. 16 BOND $H HTAB WPDB -1 ACTA LIST 6 EXYZ C21 C21' EXYZ C22 C22' EADP C21 C21' EADP C22 C22' DELU O1 > C22' SIMU O1 > C22' ISOR 0.01 O1 > C22' FMAP 2 PLAN 10 WGHT 0.028600 0.850000 FVAR 0.59398 0.44990 AG1 6 0.726612 0.394344 0.225297 11.00000 0.02776 0.02466 = 0.02197 -0.00204 -0.00282 -0.00094 N1 4 0.766605 0.546706 0.292554 11.00000 0.02460 0.02324 = 0.02205 0.00295 -0.00213 -0.00362 C1 1 0.704197 0.654583 0.244145 11.00000 0.04517 0.02598 = 0.03650 0.00473 -0.01570 -0.00524 C2 1 0.775589 0.668005 0.135015 11.00000 0.08977 0.05489 = 0.03631 0.01659 -0.02148 -0.01575 AFIX 137 H2A 2 0.764639 0.597416 0.102466 11.00000 -1.50000 H2B 2 0.891152 0.680587 0.126718 11.00000 -1.50000 H2C 2 0.716268 0.734528 0.106625 11.00000 -1.50000 AFIX 0 C3 1 0.520980 0.650895 0.252683 11.00000 0.05130 0.03509 = 0.07790 -0.00975 -0.03268 0.00800 AFIX 137 H3A 2 0.470041 0.646151 0.321276 11.00000 -1.50000 H3B 2 0.500339 0.582769 0.220207 11.00000 -1.50000 H3C 2 0.474725 0.721392 0.222058 11.00000 -1.50000 AFIX 0 C4 1 0.731262 0.761490 0.296875 11.00000 0.05697 0.02424 = 0.05551 0.00693 -0.02039 -0.00899 AFIX 23 H4A 2 0.699423 0.832401 0.259620 11.00000 -1.20000 H4B 2 0.659603 0.762996 0.361397 11.00000 -1.20000 AFIX 0 C5 1 0.906088 0.763025 0.309733 11.00000 0.06139 0.03899 = 0.05444 0.00497 -0.01499 -0.02614 AFIX 23 H5A 2 0.977952 0.769067 0.245604 11.00000 -1.20000 H5B 2 0.916020 0.831068 0.347052 11.00000 -1.20000 AFIX 0 C6 1 0.957183 0.652664 0.363069 11.00000 0.04143 0.04431 = 0.05053 -0.00381 -0.01825 -0.01129 AFIX 23 H6A 2 0.892499 0.651867 0.429619 11.00000 -1.20000 H6B 2 1.073435 0.651836 0.368245 11.00000 -1.20000 AFIX 0 C7 1 0.934012 0.542498 0.312757 11.00000 0.02870 0.03845 = 0.03589 -0.00296 -0.00885 -0.00531 C8 1 1.071953 0.522637 0.224028 11.00000 0.03441 0.07915 = 0.06969 -0.02057 0.00204 -0.00428 AFIX 137 H8A 2 1.177320 0.510500 0.245562 11.00000 -1.50000 H8B 2 1.070701 0.590711 0.179594 11.00000 -1.50000 H8C 2 1.055402 0.454090 0.190604 11.00000 -1.50000 AFIX 0 C9 1 0.953531 0.438693 0.383571 11.00000 0.06254 0.04060 = 0.06367 -0.00417 -0.03988 0.00351 AFIX 137 H9A 2 1.062812 0.432685 0.399919 11.00000 -1.50000 H9B 2 0.938747 0.367375 0.353298 11.00000 -1.50000 H9C 2 0.871501 0.449724 0.442721 11.00000 -1.50000 AFIX 0 LI1 3 0.614799 0.515069 0.412495 11.00000 0.06325 0.03659 = 0.02823 -0.00815 0.01132 -0.01998 LI2 3 0.513256 0.215585 0.286179 11.00000 0.05506 0.03976 = 0.03169 -0.00911 0.01010 -0.01515 N2 4 0.675003 0.238089 0.166758 11.00000 0.02639 0.02346 = 0.02166 -0.00364 -0.00245 0.00304 C10 1 0.596023 0.265112 0.080660 11.00000 0.03907 0.02952 = 0.02780 -0.00433 -0.01135 -0.00070 C11 1 0.686655 0.344416 0.002410 11.00000 0.07589 0.04777 = 0.02950 0.00781 -0.01690 -0.00783 AFIX 137 H11A 2 0.708476 0.414205 0.032162 11.00000 -1.50000 H11B 2 0.619267 0.366637 -0.046877 11.00000 -1.50000 H11C 2 0.790030 0.302987 -0.027963 11.00000 -1.50000 AFIX 0 C12 1 0.428443 0.328129 0.117739 11.00000 0.04264 0.04344 = 0.05601 -0.01165 -0.02378 0.01166 AFIX 137 H12A 2 0.364549 0.277486 0.164659 11.00000 -1.50000 H12B 2 0.371700 0.348293 0.063212 11.00000 -1.50000 H12C 2 0.441505 0.399061 0.149147 11.00000 -1.50000 AFIX 0 C13 1 0.569410 0.152860 0.034447 11.00000 0.04797 0.04502 = 0.03684 -0.01087 -0.01526 -0.00256 AFIX 23 H13A 2 0.484981 0.112871 0.078862 11.00000 -1.20000 H13B 2 0.528462 0.173212 -0.026622 11.00000 -1.20000 AFIX 0 C14 1 0.787841 0.042572 0.105944 11.00000 0.03858 0.02826 = 0.05633 -0.01340 -0.00391 0.00404 AFIX 23 H14A 2 0.890752 -0.008908 0.091770 11.00000 -1.20000 H14B 2 0.708041 -0.000272 0.151396 11.00000 -1.20000 AFIX 0 C15 1 0.723681 0.070777 0.012989 11.00000 0.05487 0.04229 = 0.04536 -0.02110 -0.00373 -0.00239 AFIX 23 H15A 2 0.700010 -0.001263 -0.014059 11.00000 -1.20000 H15B 2 0.806422 0.107478 -0.035341 11.00000 -1.20000 AFIX 0 C16 1 0.819497 0.150685 0.155000 11.00000 0.03433 0.02521 = 0.03707 -0.00555 -0.00635 0.00463 C17 1 0.978692 0.195818 0.101444 11.00000 0.03232 0.04444 = 0.07176 -0.01551 -0.00045 0.00142 AFIX 137 H17A 2 0.971735 0.212001 0.033070 11.00000 -1.50000 H17B 2 1.070172 0.137073 0.106303 11.00000 -1.50000 H17C 2 0.995827 0.267201 0.130760 11.00000 -1.50000 AFIX 0 C18 1 0.845426 0.112906 0.258283 11.00000 0.06406 0.03922 = 0.05720 -0.00039 -0.02801 0.01261 AFIX 137 H18A 2 0.746733 0.081888 0.294505 11.00000 -1.50000 H18B 2 0.868393 0.179939 0.291241 11.00000 -1.50000 H18C 2 0.937650 0.052857 0.254811 11.00000 -1.50000 AFIX 0 PART 1 SAME O1 C22 < C19 O1 5 0.401618 0.081712 0.336951 21.00000 0.06468 0.04796 = 0.04326 -0.00417 0.00026 -0.03100 C19 1 0.346598 0.062505 0.439258 21.00000 0.12599 0.09457 = 0.06625 0.00411 -0.01137 -0.04516 AFIX 23 H19A 2 0.434847 0.071661 0.475446 21.00000 -1.20000 H19B 2 0.251863 0.118440 0.463271 21.00000 -1.20000 AFIX 0 C20 1 0.301581 -0.053560 0.451240 21.00000 0.06629 0.08770 = 0.09241 0.04007 -0.01250 -0.02721 AFIX 23 H20A 2 0.394486 -0.108282 0.464486 21.00000 -1.20000 H20B 2 0.208886 -0.059661 0.505743 21.00000 -1.20000 AFIX 0 C21 1 0.259205 -0.077089 0.367792 21.00000 0.10431 0.06752 = 0.11408 -0.00475 0.01521 -0.03810 AFIX 23 H21A 2 0.139168 -0.064347 0.373880 21.00000 -1.20000 H21B 2 0.293620 -0.159482 0.353038 21.00000 -1.20000 AFIX 0 C22 1 0.336591 -0.002082 0.288413 21.00000 0.06257 0.05787 = 0.07472 -0.01626 -0.00270 -0.01920 AFIX 23 H22A 2 0.424146 -0.047014 0.244232 21.00000 -1.20000 H22B 2 0.255492 0.035532 0.250652 21.00000 -1.20000 AFIX 0 PART 2 SAME O1 > C22 SAME O1' C22' < C19' O1' 5 0.352675 0.103044 0.329170 -21.00000 0.06630 0.04732 = 0.05089 -0.01242 0.00770 -0.01654 C19' 1 0.234944 0.111145 0.416844 -21.00000 0.07054 0.06578 = 0.06965 -0.01908 0.02353 -0.02750 AFIX 23 H19C 2 0.138977 0.164794 0.406882 -21.00000 -1.20000 H19D 2 0.282755 0.140862 0.468883 -21.00000 -1.20000 AFIX 0 C20' 1 0.187123 -0.004060 0.443258 -21.00000 0.08907 0.07045 = 0.10418 0.00650 0.03515 -0.01329 AFIX 23 H20C 2 0.223928 -0.032396 0.504106 -21.00000 -1.20000 H20D 2 0.066923 -0.002833 0.453592 -21.00000 -1.20000 AFIX 0 C21' 1 0.259205 -0.077089 0.367792 -21.00000 0.10431 0.06752 = 0.11408 -0.00475 0.01521 -0.03810 AFIX 23 H21C 2 0.175714 -0.118530 0.346192 -21.00000 -1.20000 H21D 2 0.341693 -0.135132 0.389367 -21.00000 -1.20000 AFIX 0 C22' 1 0.336591 -0.002082 0.288413 -21.00000 0.06257 0.05787 = 0.07472 -0.01626 -0.00270 -0.01920 AFIX 23 H22C 2 0.444938 -0.039029 0.258533 -21.00000 -1.20000 H22D 2 0.268135 0.011675 0.237825 -21.00000 -1.20000 AFIX 0 PART 0 N3 4 0.450906 0.389832 0.468260 11.00000 0.08544 0.05586 = 0.04272 -0.02129 0.02987 -0.04173 C23 1 0.470534 0.327645 0.406153 11.00000 0.07413 0.05624 = 0.04161 -0.01814 0.02536 -0.03773 HKLF 4 REM aw1709 in P-1 REM R1 = 0.0272 for 4220 Fo > 4sig(Fo) and 0.0330 for all 4655 data REM 307 parameters refined using 256 restraints END WGHT 0.0286 0.8500 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.486, deepest hole -0.377, 1-sigma level 0.068 Q1 1 0.4472 0.0191 0.4307 11.00000 0.05 0.49 Q2 1 0.2599 0.0188 0.4772 11.00000 0.05 0.44 Q3 1 0.6723 0.4121 0.2925 11.00000 0.05 0.41 Q4 1 0.6446 0.4556 0.2081 11.00000 0.05 0.35 Q5 1 0.7730 0.4455 0.1754 11.00000 0.05 0.34 Q6 1 0.7737 0.3891 0.1607 11.00000 0.05 0.33 Q7 1 0.7862 0.4542 0.2401 11.00000 0.05 0.33 Q8 1 0.8166 0.3566 0.2570 11.00000 0.05 0.31 Q9 1 0.5198 0.2972 0.1050 11.00000 0.05 0.31 Q10 1 0.6779 0.3171 0.2077 11.00000 0.05 0.29 ; _shelx_res_checksum 84486 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 0.72661(2) 0.39434(2) 0.22530(2) 0.02509(7) Uani 1 1 d . . . . . N1 N 0.7666(3) 0.54671(18) 0.29255(15) 0.0236(5) Uani 1 1 d . . . . . C1 C 0.7042(4) 0.6546(2) 0.2441(2) 0.0349(7) Uani 1 1 d . . . . . C2 C 0.7756(5) 0.6680(3) 0.1350(2) 0.0591(10) Uani 1 1 d . . . . . H2A H 0.764639 0.597416 0.102466 0.089 Uiso 1 1 calc R U . . . H2B H 0.891152 0.680587 0.126718 0.089 Uiso 1 1 calc R U . . . H2C H 0.716268 0.734528 0.106625 0.089 Uiso 1 1 calc R U . . . C3 C 0.5210(4) 0.6509(3) 0.2527(3) 0.0527(9) Uani 1 1 d . . . . . H3A H 0.470041 0.646151 0.321276 0.079 Uiso 1 1 calc R U . . . H3B H 0.500339 0.582769 0.220207 0.079 Uiso 1 1 calc R U . . . H3C H 0.474725 0.721392 0.222058 0.079 Uiso 1 1 calc R U . . . C4 C 0.7313(4) 0.7615(3) 0.2969(3) 0.0442(8) Uani 1 1 d . . . . . H4A H 0.699423 0.832401 0.259620 0.053 Uiso 1 1 calc R U . . . H4B H 0.659603 0.762996 0.361397 0.053 Uiso 1 1 calc R U . . . C5 C 0.9061(5) 0.7630(3) 0.3097(3) 0.0497(9) Uani 1 1 d . . . . . H5A H 0.977952 0.769067 0.245604 0.060 Uiso 1 1 calc R U . . . H5B H 0.916020 0.831068 0.347052 0.060 Uiso 1 1 calc R U . . . C6 C 0.9572(4) 0.6527(3) 0.3631(2) 0.0435(8) Uani 1 1 d . . . . . H6A H 0.892499 0.651867 0.429619 0.052 Uiso 1 1 calc R U . . . H6B H 1.073435 0.651836 0.368245 0.052 Uiso 1 1 calc R U . . . C7 C 0.9340(4) 0.5425(3) 0.3128(2) 0.0338(7) Uani 1 1 d . . . . . C8 C 1.0720(4) 0.5226(4) 0.2240(3) 0.0620(11) Uani 1 1 d . . . . . H8A H 1.177320 0.510500 0.245562 0.093 Uiso 1 1 calc R U . . . H8B H 1.070701 0.590711 0.179594 0.093 Uiso 1 1 calc R U . . . H8C H 1.055402 0.454090 0.190604 0.093 Uiso 1 1 calc R U . . . C9 C 0.9535(5) 0.4387(3) 0.3836(3) 0.0525(9) Uani 1 1 d . . . . . H9A H 1.062812 0.432685 0.399919 0.079 Uiso 1 1 calc R U . . . H9B H 0.938747 0.367375 0.353298 0.079 Uiso 1 1 calc R U . . . H9C H 0.871501 0.449724 0.442721 0.079 Uiso 1 1 calc R U . . . Li1 Li 0.6148(7) 0.5151(4) 0.4125(4) 0.0439(14) Uani 1 1 d . . . . . Li2 Li 0.5133(7) 0.2156(5) 0.2862(4) 0.0434(13) Uani 1 1 d . . . . . N2 N 0.6750(3) 0.23809(18) 0.16676(15) 0.0244(5) Uani 1 1 d . . . . . C10 C 0.5960(4) 0.2651(2) 0.0807(2) 0.0315(6) Uani 1 1 d . . . . . C11 C 0.6867(5) 0.3444(3) 0.0024(2) 0.0503(9) Uani 1 1 d . . . . . H11A H 0.708476 0.414205 0.032162 0.075 Uiso 1 1 calc R U . . . H11B H 0.619267 0.366637 -0.046877 0.075 Uiso 1 1 calc R U . . . H11C H 0.790030 0.302987 -0.027963 0.075 Uiso 1 1 calc R U . . . C12 C 0.4284(4) 0.3281(3) 0.1177(3) 0.0462(8) Uani 1 1 d . . . . . H12A H 0.364549 0.277486 0.164659 0.069 Uiso 1 1 calc R U . . . H12B H 0.371700 0.348293 0.063212 0.069 Uiso 1 1 calc R U . . . H12C H 0.441505 0.399061 0.149147 0.069 Uiso 1 1 calc R U . . . C13 C 0.5694(4) 0.1529(3) 0.0344(2) 0.0421(8) Uani 1 1 d . . . . . H13A H 0.484981 0.112871 0.078862 0.051 Uiso 1 1 calc R U . . . H13B H 0.528462 0.173212 -0.026622 0.051 Uiso 1 1 calc R U . . . C14 C 0.7878(4) 0.0426(3) 0.1059(2) 0.0418(8) Uani 1 1 d . . . . . H14A H 0.890752 -0.008908 0.091770 0.050 Uiso 1 1 calc R U . . . H14B H 0.708041 -0.000272 0.151396 0.050 Uiso 1 1 calc R U . . . C15 C 0.7237(4) 0.0708(3) 0.0130(2) 0.0476(8) Uani 1 1 d . . . . . H15A H 0.700010 -0.001263 -0.014059 0.057 Uiso 1 1 calc R U . . . H15B H 0.806422 0.107478 -0.035341 0.057 Uiso 1 1 calc R U . . . C16 C 0.8195(4) 0.1507(2) 0.1550(2) 0.0326(6) Uani 1 1 d . . . . . C17 C 0.9787(4) 0.1958(3) 0.1014(3) 0.0505(9) Uani 1 1 d . . . . . H17A H 0.971735 0.212001 0.033070 0.076 Uiso 1 1 calc R U . . . H17B H 1.070172 0.137073 0.106303 0.076 Uiso 1 1 calc R U . . . H17C H 0.995827 0.267201 0.130760 0.076 Uiso 1 1 calc R U . . . C18 C 0.8454(5) 0.1129(3) 0.2583(3) 0.0526(9) Uani 1 1 d . . . . . H18A H 0.746733 0.081888 0.294505 0.079 Uiso 1 1 calc R U . . . H18B H 0.868393 0.179939 0.291241 0.079 Uiso 1 1 calc R U . . . H18C H 0.937650 0.052857 0.254811 0.079 Uiso 1 1 calc R U . . . O1 O 0.4016(14) 0.0817(9) 0.3370(7) 0.051(3) Uani 0.450(10) 1 d D U P A 1 C19 C 0.347(2) 0.0625(11) 0.4393(7) 0.094(4) Uani 0.450(10) 1 d D U P A 1 H19A H 0.434847 0.071661 0.475446 0.113 Uiso 0.450(10) 1 calc R U P A 1 H19B H 0.251863 0.118440 0.463271 0.113 Uiso 0.450(10) 1 calc R U P A 1 C20 C 0.3016(16) -0.0536(10) 0.4512(7) 0.083(3) Uani 0.450(10) 1 d D U P A 1 H20A H 0.394486 -0.108282 0.464486 0.099 Uiso 0.450(10) 1 calc R U P A 1 H20B H 0.208886 -0.059661 0.505743 0.099 Uiso 0.450(10) 1 calc R U P A 1 C21 C 0.2592(7) -0.0771(4) 0.3678(4) 0.0976(16) Uani 0.450(10) 1 d D U P A 1 H21A H 0.139168 -0.064347 0.373880 0.117 Uiso 0.450(10) 1 calc R U P A 1 H21B H 0.293620 -0.159482 0.353038 0.117 Uiso 0.450(10) 1 calc R U P A 1 C22 C 0.3366(5) -0.0021(3) 0.2884(3) 0.0648(11) Uani 0.450(10) 1 d D U P A 1 H22A H 0.424146 -0.047014 0.244232 0.078 Uiso 0.450(10) 1 calc R U P A 1 H22B H 0.255492 0.035532 0.250652 0.078 Uiso 0.450(10) 1 calc R U P A 1 O1' O 0.3527(12) 0.1030(8) 0.3292(7) 0.056(2) Uani 0.550(10) 1 d D U P A 2 C19' C 0.2349(12) 0.1111(7) 0.4168(6) 0.071(3) Uani 0.550(10) 1 d D U P A 2 H19C H 0.138977 0.164794 0.406882 0.085 Uiso 0.550(10) 1 calc R U P A 2 H19D H 0.282755 0.140862 0.468883 0.085 Uiso 0.550(10) 1 calc R U P A 2 C20' C 0.1871(15) -0.0041(7) 0.4433(7) 0.095(3) Uani 0.550(10) 1 d D U P A 2 H20C H 0.223928 -0.032396 0.504106 0.114 Uiso 0.550(10) 1 calc R U P A 2 H20D H 0.066923 -0.002833 0.453592 0.114 Uiso 0.550(10) 1 calc R U P A 2 C21' C 0.2592(7) -0.0771(4) 0.3678(4) 0.0976(16) Uani 0.550(10) 1 d D U P A 2 H21C H 0.175714 -0.118530 0.346192 0.117 Uiso 0.550(10) 1 calc R U P A 2 H21D H 0.341693 -0.135132 0.389367 0.117 Uiso 0.550(10) 1 calc R U P A 2 C22' C 0.3366(5) -0.0021(3) 0.2884(3) 0.0648(11) Uani 0.550(10) 1 d D U P A 2 H22C H 0.444938 -0.039029 0.258533 0.078 Uiso 0.550(10) 1 calc R U P A 2 H22D H 0.268135 0.011675 0.237825 0.078 Uiso 0.550(10) 1 calc R U P A 2 N3 N 0.4509(4) 0.3898(3) 0.4683(2) 0.0634(10) Uani 1 1 d . . . . . C23 C 0.4705(5) 0.3276(3) 0.4062(2) 0.0591(11) 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 Ag1 0.02776(12) 0.02466(11) 0.02197(11) -0.00204(7) -0.00282(7) -0.00094(7) N1 0.0246(12) 0.0232(11) 0.0221(11) 0.0030(9) -0.0021(9) -0.0036(9) C1 0.0452(19) 0.0260(14) 0.0365(16) 0.0047(12) -0.0157(14) -0.0052(12) C2 0.090(3) 0.055(2) 0.0363(19) 0.0166(16) -0.0215(19) -0.016(2) C3 0.051(2) 0.0351(18) 0.078(3) -0.0098(17) -0.0327(19) 0.0080(15) C4 0.057(2) 0.0242(15) 0.056(2) 0.0069(14) -0.0204(17) -0.0090(14) C5 0.061(2) 0.0390(18) 0.054(2) 0.0050(15) -0.0150(18) -0.0261(16) C6 0.041(2) 0.0443(18) 0.051(2) -0.0038(15) -0.0182(16) -0.0113(14) C7 0.0287(16) 0.0384(16) 0.0359(16) -0.0030(13) -0.0088(13) -0.0053(12) C8 0.034(2) 0.079(3) 0.070(3) -0.021(2) 0.0020(18) -0.0043(18) C9 0.063(2) 0.0406(19) 0.064(2) -0.0042(16) -0.040(2) 0.0035(16) Li1 0.063(4) 0.037(3) 0.028(3) -0.008(2) 0.011(2) -0.020(3) Li2 0.055(4) 0.040(3) 0.032(3) -0.009(2) 0.010(2) -0.015(2) N2 0.0264(12) 0.0235(11) 0.0217(11) -0.0036(9) -0.0025(9) 0.0030(9) C10 0.0391(17) 0.0295(15) 0.0278(14) -0.0043(11) -0.0113(13) -0.0007(12) C11 0.076(3) 0.048(2) 0.0295(17) 0.0078(14) -0.0169(17) -0.0078(18) C12 0.043(2) 0.0434(19) 0.056(2) -0.0117(16) -0.0238(16) 0.0117(15) C13 0.048(2) 0.0450(19) 0.0368(17) -0.0109(14) -0.0153(15) -0.0026(15) C14 0.0386(19) 0.0283(15) 0.056(2) -0.0134(14) -0.0039(15) 0.0040(13) C15 0.055(2) 0.0423(19) 0.0454(19) -0.0211(15) -0.0037(16) -0.0024(16) C16 0.0343(17) 0.0252(14) 0.0371(16) -0.0055(12) -0.0063(13) 0.0046(12) C17 0.0323(19) 0.0444(19) 0.072(2) -0.0155(17) -0.0004(16) 0.0014(14) C18 0.064(2) 0.0392(19) 0.057(2) -0.0004(16) -0.0280(18) 0.0126(16) O1 0.065(6) 0.048(4) 0.043(4) -0.004(3) 0.000(4) -0.031(4) C19 0.126(8) 0.095(6) 0.066(5) 0.004(5) -0.011(5) -0.045(6) C20 0.066(6) 0.088(6) 0.092(5) 0.040(5) -0.013(5) -0.027(5) C21 0.104(4) 0.068(3) 0.114(3) -0.005(2) 0.015(3) -0.038(3) C22 0.063(2) 0.058(2) 0.075(2) -0.0163(19) -0.003(2) -0.0192(18) O1' 0.066(5) 0.047(3) 0.051(4) -0.012(3) 0.008(3) -0.017(3) C19' 0.071(5) 0.066(4) 0.070(5) -0.019(4) 0.024(4) -0.028(4) C20' 0.089(6) 0.070(5) 0.104(5) 0.006(4) 0.035(5) -0.013(4) C21' 0.104(4) 0.068(3) 0.114(3) -0.005(2) 0.015(3) -0.038(3) C22' 0.063(2) 0.058(2) 0.075(2) -0.0163(19) -0.003(2) -0.0192(18) N3 0.085(2) 0.0559(18) 0.0427(17) -0.0213(15) 0.0299(16) -0.0417(17) C23 0.074(3) 0.056(2) 0.042(2) -0.0181(17) 0.0254(18) -0.038(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' 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' Ag Ag 0.1306 4.2820 '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 N1 Ag1 N2 176.01(8) . . ? N1 Ag1 Li2 132.61(11) . . ? N2 Ag1 Li2 43.41(11) . . ? N1 Ag1 Li1 40.71(11) . . ? N2 Ag1 Li1 135.30(11) . . ? Li2 Ag1 Li1 91.94(14) . . ? C7 N1 C1 116.6(2) . . ? C7 N1 Li1 109.7(2) . . ? C1 N1 Li1 109.4(3) . . ? C7 N1 Ag1 112.45(16) . . ? C1 N1 Ag1 112.34(16) . . ? Li1 N1 Ag1 93.96(17) . . ? N1 C1 C3 106.9(2) . . ? N1 C1 C4 110.4(2) . . ? C3 C1 C4 107.8(3) . . ? N1 C1 C2 114.7(3) . . ? C3 C1 C2 106.9(3) . . ? C4 C1 C2 109.8(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C5 C4 C1 112.9(3) . . ? C5 C4 H4A 109.0 . . ? C1 C4 H4A 109.0 . . ? C5 C4 H4B 109.0 . . ? C1 C4 H4B 109.0 . . ? H4A C4 H4B 107.8 . . ? C6 C5 C4 109.1(3) . . ? C6 C5 H5A 109.9 . . ? C4 C5 H5A 109.9 . . ? C6 C5 H5B 109.9 . . ? C4 C5 H5B 109.9 . . ? H5A C5 H5B 108.3 . . ? C5 C6 C7 112.9(3) . . ? C5 C6 H6A 109.0 . . ? C7 C6 H6A 109.0 . . ? C5 C6 H6B 109.0 . . ? C7 C6 H6B 109.0 . . ? H6A C6 H6B 107.8 . . ? N1 C7 C9 106.3(2) . . ? N1 C7 C6 110.9(2) . . ? C9 C7 C6 107.9(2) . . ? N1 C7 C8 115.3(3) . . ? C9 C7 C8 106.7(3) . . ? C6 C7 C8 109.3(3) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? N1 Li1 N3 129.2(3) . 2_666 ? N1 Li1 N3 138.0(3) . . ? N3 Li1 N3 92.7(2) 2_666 . ? N1 Li1 C23 112.7(2) . . ? N3 Li1 C23 118.0(2) 2_666 . ? N3 Li1 C23 25.27(11) . . ? N1 Li1 Li1 176.2(4) . 2_666 ? N3 Li1 Li1 47.97(16) 2_666 2_666 ? N3 Li1 Li1 44.75(16) . 2_666 ? C23 Li1 Li1 70.0(2) . 2_666 ? N1 Li1 Ag1 45.34(12) . . ? N3 Li1 Ag1 174.3(2) 2_666 . ? N3 Li1 Ag1 92.69(18) . . ? C23 Li1 Ag1 67.42(13) . . ? Li1 Li1 Ag1 137.4(3) 2_666 . ? O1 Li2 N2 130.9(4) . . ? O1' Li2 N2 134.1(4) . . ? O1 Li2 C23 103.8(4) . . ? O1' Li2 C23 102.0(3) . . ? N2 Li2 C23 123.9(3) . . ? O1 Li2 Ag1 169.8(5) . . ? O1' Li2 Ag1 175.4(4) . . ? N2 Li2 Ag1 48.31(13) . . ? C23 Li2 Ag1 75.60(17) . . ? C16 N2 C10 116.8(2) . . ? C16 N2 Li2 114.4(2) . . ? C10 N2 Li2 111.9(2) . . ? C16 N2 Ag1 111.16(16) . . ? C10 N2 Ag1 110.74(15) . . ? Li2 N2 Ag1 88.29(17) . . ? N2 C10 C12 106.5(2) . . ? N2 C10 C11 114.8(2) . . ? C12 C10 C11 107.5(3) . . ? N2 C10 C13 110.8(2) . . ? C12 C10 C13 107.6(2) . . ? C11 C10 C13 109.3(2) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C10 112.7(3) . . ? C15 C13 H13A 109.1 . . ? C10 C13 H13A 109.1 . . ? C15 C13 H13B 109.1 . . ? C10 C13 H13B 109.1 . . ? H13A C13 H13B 107.8 . . ? C15 C14 C16 113.0(3) . . ? C15 C14 H14A 109.0 . . ? C16 C14 H14A 109.0 . . ? C15 C14 H14B 109.0 . . ? C16 C14 H14B 109.0 . . ? H14A C14 H14B 107.8 . . ? C14 C15 C13 108.8(3) . . ? C14 C15 H15A 109.9 . . ? C13 C15 H15A 109.9 . . ? C14 C15 H15B 109.9 . . ? C13 C15 H15B 109.9 . . ? H15A C15 H15B 108.3 . . ? N2 C16 C14 111.4(2) . . ? N2 C16 C17 114.9(2) . . ? C14 C16 C17 109.6(2) . . ? N2 C16 C18 106.0(2) . . ? C14 C16 C18 107.4(2) . . ? C17 C16 C18 107.0(3) . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C22 O1 C19 107.2(7) . . ? C22 O1 Li2 130.4(7) . . ? C19 O1 Li2 121.7(7) . . ? C20 C19 O1 106.1(8) . . ? C20 C19 H19A 110.5 . . ? O1 C19 H19A 110.5 . . ? C20 C19 H19B 110.5 . . ? O1 C19 H19B 110.5 . . ? H19A C19 H19B 108.7 . . ? C21 C20 C19 105.8(7) . . ? C21 C20 H20A 110.6 . . ? C19 C20 H20A 110.6 . . ? C21 C20 H20B 110.6 . . ? C19 C20 H20B 110.6 . . ? H20A C20 H20B 108.7 . . ? C20 C21 C22 110.2(5) . . ? C20 C21 H21A 109.6 . . ? C22 C21 H21A 109.6 . . ? C20 C21 H21B 109.6 . . ? C22 C21 H21B 109.6 . . ? H21A C21 H21B 108.1 . . ? O1 C22 C21 103.8(5) . . ? O1 C22 H22A 111.0 . . ? C21 C22 H22A 111.0 . . ? O1 C22 H22B 111.0 . . ? C21 C22 H22B 111.0 . . ? H22A C22 H22B 109.0 . . ? C22' O1' C19' 106.5(6) . . ? C22' O1' Li2 129.3(6) . . ? C19' O1' Li2 124.0(6) . . ? O1' C19' C20' 107.4(6) . . ? O1' C19' H19C 110.2 . . ? C20' C19' H19C 110.2 . . ? O1' C19' H19D 110.2 . . ? C20' C19' H19D 110.2 . . ? H19C C19' H19D 108.5 . . ? C21' C20' C19' 108.1(6) . . ? C21' C20' H20C 110.1 . . ? C19' C20' H20C 110.1 . . ? C21' C20' H20D 110.1 . . ? C19' C20' H20D 110.1 . . ? H20C C20' H20D 108.4 . . ? C20' C21' C22' 106.4(5) . . ? C20' C21' H21C 110.4 . . ? C22' C21' H21C 110.4 . . ? C20' C21' H21D 110.4 . . ? C22' C21' H21D 110.4 . . ? H21C C21' H21D 108.6 . . ? O1' C22' C21' 106.9(5) . . ? O1' C22' H22C 110.3 . . ? C21' C22' H22C 110.3 . . ? O1' C22' H22D 110.3 . . ? C21' C22' H22D 110.3 . . ? H22C C22' H22D 108.6 . . ? C23 N3 Li1 170.6(3) . 2_666 ? C23 N3 Li1 102.0(3) . . ? Li1 N3 Li1 87.3(2) 2_666 . ? N3 C23 Li2 177.8(3) . . ? N3 C23 Li1 52.7(2) . . ? Li2 C23 Li1 125.0(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 Ag1 N1 2.134(2) . ? Ag1 N2 2.147(2) . ? Ag1 Li2 2.874(5) . ? Ag1 Li1 2.994(5) . ? N1 C7 1.479(4) . ? N1 C1 1.484(3) . ? N1 Li1 1.957(5) . ? C1 C3 1.524(5) . ? C1 C4 1.536(4) . ? C1 C2 1.545(4) . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 H3A 0.9800 . ? C3 H3B 0.9800 . ? C3 H3C 0.9800 . ? C4 C5 1.512(5) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 C6 1.511(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 C7 1.540(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 C9 1.534(4) . ? C7 C8 1.544(4) . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? Li1 N3 2.014(6) 2_666 ? Li1 N3 2.125(6) . ? Li1 C23 2.612(6) . ? Li1 Li1 2.857(10) 2_666 ? Li2 O1 1.933(11) . ? Li2 O1' 1.967(10) . ? Li2 N2 1.976(5) . ? Li2 C23 2.139(6) . ? N2 C16 1.485(3) . ? N2 C10 1.488(3) . ? C10 C12 1.527(4) . ? C10 C11 1.537(4) . ? C10 C13 1.541(4) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C15 1.515(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.510(5) . ? C14 C16 1.533(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.535(4) . ? C16 C18 1.540(4) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? O1 C22 1.425(10) . ? O1 C19 1.438(11) . ? C19 C20 1.430(11) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 C21 1.336(10) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C21 C22 1.472(6) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? O1' C22' 1.405(9) . ? O1' C19' 1.429(9) . ? C19' C20' 1.445(9) . ? C19' H19C 0.9900 . ? C19' H19D 0.9900 . ? C20' C21' 1.399(9) . ? C20' H20C 0.9900 . ? C20' H20D 0.9900 . ? C21' C22' 1.472(6) . ? C21' H21C 0.9900 . ? C21' H21D 0.9900 . ? C22' H22C 0.9900 . ? C22' H22D 0.9900 . ? N3 C23 1.140(4) . ?