#------------------------------------------------------------------------------ #$Date: 2020-03-04 09:48:00 +0200 (Wed, 04 Mar 2020) $ #$Revision: 248753 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/55/74/1557457.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_1557457 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 'C36 H72 Ag2 Li2 N4' _chemical_formula_sum 'C36 H72 Ag2 Li2 N4' _chemical_formula_weight 790.59 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2019-05-30 deposited with the CCDC. 2020-01-03 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 109.5610(10) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 22.1326(5) _cell_length_b 8.3936(2) _cell_length_c 22.8868(6) _cell_measurement_reflns_used 9366 _cell_measurement_temperature 180(2) _cell_measurement_theta_max 66.50 _cell_measurement_theta_min 4.100 _cell_volume 4006.34(17) _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 _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXT 2014/4 (Sheldrick, 2014)' _diffrn_ambient_temperature 180(2) _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _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 0.0489 _diffrn_reflns_av_unetI/netI 0.0315 _diffrn_reflns_Laue_measured_fraction_full 0.999 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 18817 _diffrn_reflns_point_group_measured_fraction_full 0.999 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 66.621 _diffrn_reflns_theta_max 66.621 _diffrn_reflns_theta_min 4.100 _exptl_absorpt_coefficient_mu 8.026 _exptl_absorpt_correction_T_max 0.7528 _exptl_absorpt_correction_T_min 0.6286 _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 1.311 _exptl_crystal_description block _exptl_crystal_F_000 1664 _exptl_crystal_size_max 0.110 _exptl_crystal_size_mid 0.090 _exptl_crystal_size_min 0.050 _refine_diff_density_max 0.295 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.074 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.128 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 208 _refine_ls_number_reflns 3517 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.128 _refine_ls_R_factor_all 0.0345 _refine_ls_R_factor_gt 0.0257 _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^)+(0.0203P)^2^+2.0569P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0517 _refine_ls_wR_factor_ref 0.0537 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3045 _reflns_number_total 3517 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c9sc06060j2.cif _cod_data_source_block aw1526 _cod_original_sg_symbol_H-M 'C 2/c' _cod_database_code 1557457 _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_min 0.472 _shelx_estimated_absorpt_t_max 0.690 _shelx_res_file ; TITL aw1526.res in C2/c aw1526.res created by SHELXL-2018/3 at 09:52:39 on 28-Feb-2019 CELL 1.54184 22.1326 8.3936 22.8868 90.000 109.561 90.000 ZERR 4 0.0005 0.0002 0.0006 0.000 0.001 0.000 LATT 7 SYMM -X, Y, 1/2-Z SFAC C H Li N Ag UNIT 144 288 8 16 8 TEMP -93.150 SIZE 0.05 0.09 0.11 L.S. 16 BOND $H HTAB WPDB -1 LIST 6 FMAP 2 ACTA PLAN 20 EXYZ Ag1 Li1' EXYZ Li1 Ag1' EADP Ag1 Li1' EADP Li1 Ag1' WGHT 0.020300 2.056900 FVAR 0.21050 0.94499 PART 1 AG1 5 0.407404 0.384266 0.244125 21.00000 0.01929 0.02112 = 0.01710 0.00015 0.00657 -0.00145 LI1 3 0.526972 0.383722 0.346300 21.00000 0.01611 0.01949 = 0.01995 -0.00048 0.00751 -0.00247 PART 2 LI1' 3 0.407404 0.384266 0.244125 -21.00000 0.01929 0.02112 = 0.01710 0.00015 0.00657 -0.00145 AG1' 5 0.526972 0.383722 0.346300 -21.00000 0.01611 0.01949 = 0.01995 -0.00048 0.00751 -0.00247 PART 0 N2 4 0.436072 0.311502 0.338520 11.00000 0.02585 0.02050 = 0.02382 -0.00005 0.01346 -0.00096 C10 1 0.411743 0.417348 0.378233 11.00000 0.03500 0.02282 = 0.03021 -0.00241 0.01978 -0.00082 C11 1 0.338450 0.445831 0.354578 11.00000 0.03860 0.04117 = 0.05077 -0.00618 0.02670 0.00601 AFIX 137 H11A 2 0.324450 0.476066 0.310703 11.00000 -1.50000 H11B 2 0.328026 0.531553 0.378678 11.00000 -1.50000 H11C 2 0.316447 0.347914 0.359368 11.00000 -1.50000 AFIX 0 C12 1 0.442602 0.580895 0.379773 11.00000 0.05259 0.02813 = 0.03676 -0.00840 0.02415 -0.00626 AFIX 137 H12A 2 0.489340 0.570700 0.397289 11.00000 -1.50000 H12B 2 0.427542 0.653522 0.405487 11.00000 -1.50000 H12C 2 0.430710 0.623329 0.337532 11.00000 -1.50000 AFIX 0 C13 1 0.433422 0.354976 0.445064 11.00000 0.05543 0.03348 = 0.03143 -0.00370 0.02580 0.00059 AFIX 23 H13A 2 0.480511 0.367020 0.463540 11.00000 -1.20000 H13B 2 0.413551 0.420954 0.469577 11.00000 -1.20000 AFIX 0 C14 1 0.415937 0.181454 0.449742 11.00000 0.08031 0.03585 = 0.03683 0.00570 0.03698 0.00049 AFIX 23 H14A 2 0.368733 0.169304 0.435492 11.00000 -1.20000 H14B 2 0.433455 0.145403 0.493380 11.00000 -1.20000 AFIX 0 C15 1 0.443886 0.081239 0.409399 11.00000 0.06649 0.02402 = 0.03907 0.00621 0.02835 0.00484 AFIX 23 H15A 2 0.430609 -0.031070 0.410413 11.00000 -1.20000 H15B 2 0.491274 0.085333 0.426793 11.00000 -1.20000 AFIX 0 C16 1 0.422130 0.138646 0.341934 11.00000 0.03716 0.02046 = 0.03292 0.00106 0.01865 -0.00002 C17 1 0.351475 0.089032 0.308523 11.00000 0.04465 0.03313 = 0.05679 -0.01037 0.02838 -0.01577 AFIX 137 H17A 2 0.336523 0.134149 0.266613 11.00000 -1.50000 H17B 2 0.324707 0.128994 0.331851 11.00000 -1.50000 H17C 2 0.348528 -0.027413 0.305981 11.00000 -1.50000 AFIX 0 C18 1 0.461035 0.047338 0.308657 11.00000 0.04575 0.02697 = 0.03896 -0.00503 0.02226 0.00320 AFIX 137 H18A 2 0.506551 0.074200 0.327424 11.00000 -1.50000 H18B 2 0.446218 0.076853 0.264693 11.00000 -1.50000 H18C 2 0.455217 -0.067435 0.312572 11.00000 -1.50000 AFIX 0 N1 4 0.384719 0.453986 0.149750 11.00000 0.02084 0.02104 = 0.01918 -0.00183 0.00254 -0.00290 C1 1 0.336377 0.348642 0.105675 11.00000 0.03086 0.02989 = 0.02580 -0.00337 0.00493 -0.00857 C8 1 0.366178 0.182487 0.110738 11.00000 0.06529 0.02656 = 0.03501 -0.00572 0.00481 -0.00776 AFIX 137 H8A 2 0.404954 0.187661 0.099179 11.00000 -1.50000 H8B 2 0.335325 0.109301 0.082785 11.00000 -1.50000 H8C 2 0.377338 0.144104 0.153491 11.00000 -1.50000 AFIX 0 C9 1 0.272465 0.328307 0.118765 11.00000 0.03959 0.06114 = 0.03676 -0.00517 0.00954 -0.02648 AFIX 137 H9A 2 0.281570 0.311220 0.163251 11.00000 -1.50000 H9B 2 0.249088 0.236324 0.095648 11.00000 -1.50000 H9C 2 0.246337 0.424524 0.105671 11.00000 -1.50000 AFIX 0 C7 1 0.323554 0.405599 0.038835 11.00000 0.03515 0.04125 = 0.02498 -0.00511 0.00515 -0.01007 AFIX 23 H7A 2 0.362742 0.389216 0.027861 11.00000 -1.20000 H7B 2 0.289051 0.339575 0.010451 11.00000 -1.20000 AFIX 0 C6 1 0.304210 0.579458 0.029025 11.00000 0.03543 0.04769 = 0.02647 0.00642 0.00319 -0.00029 AFIX 23 H6A 2 0.262251 0.595173 0.034832 11.00000 -1.20000 H6B 2 0.299964 0.611857 -0.013761 11.00000 -1.20000 AFIX 0 C5 1 0.355129 0.681022 0.075485 11.00000 0.03345 0.02933 = 0.03156 0.00636 0.00742 0.00563 AFIX 23 H5A 2 0.340681 0.793365 0.071299 11.00000 -1.20000 H5B 2 0.395294 0.675828 0.065511 11.00000 -1.20000 AFIX 0 C4 1 0.369002 0.627426 0.142880 11.00000 0.02383 0.02327 = 0.02680 -0.00270 0.00917 0.00258 C2 1 0.427620 0.717649 0.183673 11.00000 0.03078 0.02532 = 0.03396 -0.00586 0.01141 -0.00437 AFIX 137 H2A 2 0.465140 0.687140 0.172596 11.00000 -1.50000 H2B 2 0.435222 0.691422 0.227281 11.00000 -1.50000 H2C 2 0.420236 0.832468 0.177406 11.00000 -1.50000 AFIX 0 C3 1 0.313270 0.681361 0.164675 11.00000 0.02927 0.04002 = 0.04496 -0.00151 0.01655 0.00577 AFIX 137 H3A 2 0.318450 0.633924 0.205192 11.00000 -1.50000 H3B 2 0.272433 0.646613 0.134531 11.00000 -1.50000 H3C 2 0.313579 0.797756 0.168126 11.00000 -1.50000 AFIX 0 HKLF 4 REM aw1526.res in C2/c REM wR2 = 0.0537, GooF = S = 1.128, Restrained GooF = 1.128 for all data REM R1 = 0.0257 for 3045 Fo > 4sig(Fo) and 0.0345 for all 3517 data REM 208 parameters refined using 0 restraints END WGHT 0.0203 2.0569 REM No hydrogen bonds found for HTAB generation REM Highest difference peak 0.295, deepest hole -0.496, 1-sigma level 0.074 Q1 1 0.4173 0.4915 0.2686 11.00000 0.05 0.29 Q2 1 0.2467 0.3251 0.2710 11.00000 0.05 0.26 Q3 1 0.2895 0.3074 -0.0161 11.00000 0.05 0.25 Q4 1 0.4804 0.8605 0.2185 11.00000 0.05 0.25 Q5 1 0.2264 0.3467 0.2003 11.00000 0.05 0.24 Q6 1 0.3063 0.6272 0.3475 11.00000 0.05 0.24 Q7 1 0.5018 -0.1602 0.4175 11.00000 0.05 0.23 Q8 1 0.2698 0.3795 0.2120 11.00000 0.05 0.22 Q9 1 0.2748 0.2292 0.1017 11.00000 0.05 0.22 Q10 1 0.5000 0.2061 0.2500 10.50000 0.05 0.22 Q11 1 0.2981 -0.0539 0.3054 11.00000 0.05 0.22 Q12 1 0.5219 0.3400 0.4766 11.00000 0.05 0.22 Q13 1 0.2469 0.1459 0.2504 11.00000 0.05 0.21 Q14 1 0.4691 -0.0022 0.4620 11.00000 0.05 0.21 Q15 1 0.2602 -0.0023 0.3225 11.00000 0.05 0.21 Q16 1 0.4695 0.1189 0.2331 11.00000 0.05 0.21 Q17 1 0.2694 0.0370 0.2026 11.00000 0.05 0.21 Q18 1 0.4755 -0.1025 0.2697 11.00000 0.05 0.20 Q19 1 0.3443 0.7565 0.2680 11.00000 0.05 0.20 Q20 1 0.3022 -0.2139 0.2760 11.00000 0.05 0.20 ; _shelx_res_checksum 21638 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -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 Ag1 Ag 0.40740(2) 0.38427(2) 0.24413(2) 0.01905(7) Uani 0.9450(8) 1 d . . P A 1 Li1 Li 0.52697(8) 0.3837(2) 0.34630(8) 0.0181(6) Uani 0.9450(8) 1 d . . P A 1 Li1' Li 0.40740(2) 0.38427(2) 0.24413(2) 0.01905(7) Uani 0.0550(8) 1 d . . P A 2 Ag1' Ag 0.52697(8) 0.3837(2) 0.34630(8) 0.0181(6) Uani 0.0550(8) 1 d . . P A 2 N2 N 0.43607(10) 0.3115(2) 0.33852(10) 0.0221(5) Uani 1 1 d . . . . . C10 C 0.41174(13) 0.4173(3) 0.37823(14) 0.0271(6) Uani 1 1 d . . . . . C11 C 0.33845(14) 0.4458(4) 0.35458(16) 0.0406(8) Uani 1 1 d . . . . . H11A H 0.324450 0.476066 0.310703 0.061 Uiso 1 1 calc R U . . . H11B H 0.328026 0.531553 0.378678 0.061 Uiso 1 1 calc R U . . . H11C H 0.316447 0.347914 0.359368 0.061 Uiso 1 1 calc R U . . . C12 C 0.44260(15) 0.5809(3) 0.37977(15) 0.0368(7) Uani 1 1 d . . . . . H12A H 0.489340 0.570700 0.397289 0.055 Uiso 1 1 calc R U . A 1 H12B H 0.427542 0.653522 0.405487 0.055 Uiso 1 1 calc R U . A 1 H12C H 0.430710 0.623329 0.337532 0.055 Uiso 1 1 calc R U . A 1 C13 C 0.43342(15) 0.3550(3) 0.44506(14) 0.0373(7) Uani 1 1 d . . . . . H13A H 0.480511 0.367020 0.463540 0.045 Uiso 1 1 calc R U . . . H13B H 0.413551 0.420954 0.469577 0.045 Uiso 1 1 calc R U . . . C14 C 0.41594(19) 0.1815(4) 0.44974(16) 0.0466(9) Uani 1 1 d . . . . . H14A H 0.368733 0.169304 0.435492 0.056 Uiso 1 1 calc R U . . . H14B H 0.433455 0.145403 0.493380 0.056 Uiso 1 1 calc R U . . . C15 C 0.44389(17) 0.0812(3) 0.40940(15) 0.0405(8) Uani 1 1 d . . . . . H15A H 0.430609 -0.031070 0.410413 0.049 Uiso 1 1 calc R U . . . H15B H 0.491274 0.085333 0.426793 0.049 Uiso 1 1 calc R U . . . C16 C 0.42213(13) 0.1386(3) 0.34193(14) 0.0284(6) Uani 1 1 d . . . . . C17 C 0.35148(15) 0.0890(4) 0.30852(17) 0.0420(8) Uani 1 1 d . . . . . H17A H 0.336523 0.134149 0.266613 0.063 Uiso 1 1 calc R U . . . H17B H 0.324707 0.128994 0.331851 0.063 Uiso 1 1 calc R U . . . H17C H 0.348528 -0.027413 0.305981 0.063 Uiso 1 1 calc R U . . . C18 C 0.46103(14) 0.0473(4) 0.30866(15) 0.0352(7) Uani 1 1 d . . . . . H18A H 0.506551 0.074200 0.327424 0.053 Uiso 1 1 calc R U . . . H18B H 0.446218 0.076853 0.264693 0.053 Uiso 1 1 calc R U . . . H18C H 0.455217 -0.067435 0.312572 0.053 Uiso 1 1 calc R U . . . N1 N 0.38472(9) 0.4540(3) 0.14975(10) 0.0214(5) Uani 1 1 d . . . . . C1 C 0.33638(13) 0.3486(3) 0.10567(13) 0.0300(6) Uani 1 1 d . . . . . C8 C 0.36618(17) 0.1825(4) 0.11074(16) 0.0453(8) Uani 1 1 d . . . . . H8A H 0.404954 0.187661 0.099179 0.068 Uiso 1 1 calc R U . . . H8B H 0.335325 0.109301 0.082785 0.068 Uiso 1 1 calc R U . . . H8C H 0.377338 0.144104 0.153491 0.068 Uiso 1 1 calc R U . . . C9 C 0.27246(15) 0.3283(4) 0.11876(16) 0.0466(9) Uani 1 1 d . . . . . H9A H 0.281570 0.311220 0.163251 0.070 Uiso 1 1 calc R U . . . H9B H 0.249088 0.236324 0.095648 0.070 Uiso 1 1 calc R U . . . H9C H 0.246337 0.424524 0.105671 0.070 Uiso 1 1 calc R U . . . C7 C 0.32355(14) 0.4056(3) 0.03884(14) 0.0350(7) Uani 1 1 d . . . . . H7A H 0.362742 0.389216 0.027861 0.042 Uiso 1 1 calc R U . . . H7B H 0.289051 0.339575 0.010451 0.042 Uiso 1 1 calc R U . . . C6 C 0.30421(14) 0.5795(4) 0.02903(15) 0.0383(8) Uani 1 1 d . . . . . H6A H 0.262251 0.595173 0.034832 0.046 Uiso 1 1 calc R U . . . H6B H 0.299964 0.611857 -0.013761 0.046 Uiso 1 1 calc R U . . . C5 C 0.35513(13) 0.6810(3) 0.07548(14) 0.0323(7) Uani 1 1 d . . . . . H5A H 0.340681 0.793365 0.071299 0.039 Uiso 1 1 calc R U . . . H5B H 0.395294 0.675828 0.065511 0.039 Uiso 1 1 calc R U . . . C4 C 0.36900(11) 0.6274(3) 0.14288(13) 0.0245(6) Uani 1 1 d . . . . . C2 C 0.42762(13) 0.7176(3) 0.18367(14) 0.0299(7) Uani 1 1 d . . . . . H2A H 0.465140 0.687140 0.172596 0.045 Uiso 1 1 calc R U . . . H2B H 0.435222 0.691422 0.227281 0.045 Uiso 1 1 calc R U . . . H2C H 0.420236 0.832468 0.177406 0.045 Uiso 1 1 calc R U . . . C3 C 0.31327(13) 0.6814(4) 0.16467(15) 0.0370(7) Uani 1 1 d . . . . . H3A H 0.318450 0.633924 0.205192 0.056 Uiso 1 1 calc R U . . . H3B H 0.272433 0.646613 0.134531 0.056 Uiso 1 1 calc R U . . . H3C H 0.313579 0.797756 0.168126 0.056 Uiso 1 1 calc R 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 0.01929(9) 0.02112(10) 0.01710(11) 0.00015(9) 0.00657(7) -0.00145(8) Li1 0.0161(9) 0.0195(10) 0.0200(11) -0.0005(8) 0.0075(7) -0.0025(7) Li1' 0.01929(9) 0.02112(10) 0.01710(11) 0.00015(9) 0.00657(7) -0.00145(8) Ag1' 0.0161(9) 0.0195(10) 0.0200(11) -0.0005(8) 0.0075(7) -0.0025(7) N2 0.0258(11) 0.0205(11) 0.0238(13) 0.0000(9) 0.0135(10) -0.0010(8) C10 0.0350(14) 0.0228(15) 0.0302(16) -0.0024(12) 0.0198(13) -0.0008(11) C11 0.0386(17) 0.0412(18) 0.051(2) -0.0062(16) 0.0267(16) 0.0060(13) C12 0.0526(18) 0.0281(17) 0.0368(19) -0.0084(13) 0.0241(15) -0.0063(13) C13 0.0554(18) 0.0335(17) 0.0314(17) -0.0037(14) 0.0258(15) 0.0006(14) C14 0.080(2) 0.0358(18) 0.037(2) 0.0057(15) 0.0370(19) 0.0005(16) C15 0.066(2) 0.0240(16) 0.039(2) 0.0062(13) 0.0284(17) 0.0048(13) C16 0.0372(14) 0.0205(14) 0.0329(17) 0.0011(12) 0.0187(13) 0.0000(11) C17 0.0446(17) 0.0331(18) 0.057(2) -0.0104(15) 0.0284(16) -0.0158(13) C18 0.0458(17) 0.0270(15) 0.039(2) -0.0050(13) 0.0223(15) 0.0032(12) N1 0.0208(10) 0.0210(11) 0.0192(12) -0.0018(9) 0.0025(9) -0.0029(8) C1 0.0309(14) 0.0299(16) 0.0258(16) -0.0034(13) 0.0049(12) -0.0086(11) C8 0.065(2) 0.0266(16) 0.035(2) -0.0057(14) 0.0048(17) -0.0078(15) C9 0.0396(17) 0.061(2) 0.037(2) -0.0052(17) 0.0095(15) -0.0265(16) C7 0.0352(15) 0.0413(18) 0.0250(16) -0.0051(14) 0.0052(13) -0.0101(13) C6 0.0354(15) 0.048(2) 0.0265(17) 0.0064(14) 0.0032(13) -0.0003(13) C5 0.0335(15) 0.0293(15) 0.0316(18) 0.0064(13) 0.0074(13) 0.0056(12) C4 0.0238(12) 0.0233(14) 0.0268(15) -0.0027(12) 0.0092(11) 0.0026(11) C2 0.0308(14) 0.0253(15) 0.0340(18) -0.0059(13) 0.0114(13) -0.0044(11) C3 0.0293(14) 0.0400(17) 0.045(2) -0.0015(15) 0.0166(14) 0.0058(12) 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' 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 N2 Ag1 N1 176.37(8) . . ? N2 Ag1 Li1 45.23(6) . . ? N1 Ag1 Li1 131.55(6) . . ? N2 Ag1 Li1 132.39(6) . 2_655 ? N1 Ag1 Li1 44.00(6) . 2_655 ? Li1 Ag1 Li1 92.05(5) . 2_655 ? N1 Li1 N2 177.72(14) 2_655 . ? N1 Li1 C12 122.89(12) 2_655 . ? N2 Li1 C12 58.09(9) . . ? N1 Li1 Ag1 130.44(10) 2_655 . ? N2 Li1 Ag1 47.42(7) . . ? C12 Li1 Ag1 72.83(8) . . ? N1 Li1 Ag1 47.24(7) 2_655 2_655 ? N2 Li1 Ag1 130.52(10) . 2_655 ? C12 Li1 Ag1 137.48(10) . 2_655 ? Ag1 Li1 Ag1 87.95(5) . 2_655 ? N2 Li1' N1 176.37(8) . . ? N2 Li1' Ag1' 45.23(6) . . ? N1 Li1' Ag1' 131.55(6) . . ? N1 Ag1' N2 177.72(14) 2_655 . ? N1 Ag1' Li1' 130.44(10) 2_655 . ? N2 Ag1' Li1' 47.42(7) . . ? C16 N2 C10 115.1(2) . . ? C16 N2 Li1 119.82(17) . . ? C10 N2 Li1 108.31(16) . . ? C16 N2 Ag1' 119.82(17) . . ? C10 N2 Ag1' 108.31(16) . . ? C16 N2 Ag1 109.64(17) . . ? C10 N2 Ag1 113.66(16) . . ? Li1 N2 Ag1 87.35(9) . . ? C16 N2 Li1' 109.64(17) . . ? C10 N2 Li1' 113.66(16) . . ? Ag1' N2 Li1' 87.35(9) . . ? N2 C10 C12 107.4(2) . . ? N2 C10 C13 110.3(2) . . ? C12 C10 C13 107.2(2) . . ? N2 C10 C11 115.3(2) . . ? C12 C10 C11 106.1(2) . . ? C13 C10 C11 110.1(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 Li1 78.21(15) . . ? C10 C12 H12A 109.5 . . ? Li1 C12 H12A 49.3 . . ? C10 C12 H12B 109.5 . . ? Li1 C12 H12B 158.1 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? Li1 C12 H12C 85.9 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C10 113.3(3) . . ? C14 C13 H13A 108.9 . . ? C10 C13 H13A 108.9 . . ? C14 C13 H13B 108.9 . . ? C10 C13 H13B 108.9 . . ? H13A C13 H13B 107.7 . . ? C13 C14 C15 108.8(3) . . ? C13 C14 H14A 109.9 . . ? C15 C14 H14A 109.9 . . ? C13 C14 H14B 109.9 . . ? C15 C14 H14B 109.9 . . ? H14A C14 H14B 108.3 . . ? C14 C15 C16 112.5(3) . . ? C14 C15 H15A 109.1 . . ? C16 C15 H15A 109.1 . . ? C14 C15 H15B 109.1 . . ? C16 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? N2 C16 C18 107.5(2) . . ? N2 C16 C15 111.0(2) . . ? C18 C16 C15 107.7(2) . . ? N2 C16 C17 115.3(2) . . ? C18 C16 C17 105.2(2) . . ? C15 C16 C17 109.7(2) . . ? 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 . . ? C1 N1 C4 114.7(2) . . ? C1 N1 Li1 108.82(17) . 2_655 ? C4 N1 Li1 118.60(16) . 2_655 ? C1 N1 Ag1 113.30(16) . . ? C4 N1 Ag1 110.02(16) . . ? Li1 N1 Ag1 88.76(9) 2_655 . ? C1 N1 Li1' 113.30(16) . . ? C4 N1 Li1' 110.02(16) . . ? N1 C1 C8 107.2(2) . . ? N1 C1 C7 109.9(2) . . ? C8 C1 C7 106.9(3) . . ? N1 C1 C9 115.4(2) . . ? C8 C1 C9 106.4(3) . . ? C7 C1 C9 110.5(2) . . ? C1 C8 H8A 109.5 . . ? C1 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C1 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C1 C9 H9A 109.5 . . ? C1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C6 C7 C1 113.3(3) . . ? C6 C7 H7A 108.9 . . ? C1 C7 H7A 108.9 . . ? C6 C7 H7B 108.9 . . ? C1 C7 H7B 108.9 . . ? H7A C7 H7B 107.7 . . ? C7 C6 C5 109.2(2) . . ? C7 C6 H6A 109.8 . . ? C5 C6 H6A 109.8 . . ? C7 C6 H6B 109.8 . . ? C5 C6 H6B 109.8 . . ? H6A C6 H6B 108.3 . . ? C6 C5 C4 112.9(2) . . ? C6 C5 H5A 109.0 . . ? C4 C5 H5A 109.0 . . ? C6 C5 H5B 109.0 . . ? C4 C5 H5B 109.0 . . ? H5A C5 H5B 107.8 . . ? N1 C4 C2 107.4(2) . . ? N1 C4 C5 110.6(2) . . ? C2 C4 C5 108.2(2) . . ? N1 C4 C3 115.8(2) . . ? C2 C4 C3 105.4(2) . . ? C5 C4 C3 109.0(2) . . ? C4 C2 H2A 109.5 . . ? C4 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C4 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C4 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? 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 N2 2.127(2) . ? Ag1 N1 2.129(2) . ? Ag1 Li1 2.8858(17) . ? Ag1 Li1 2.8992(18) 2_655 ? Li1 N1 2.014(3) 2_655 ? Li1 N2 2.051(3) . ? Li1 C12 2.788(4) . ? Li1' N2 2.127(2) . ? Li1' N1 2.129(2) . ? Li1' Ag1' 2.8858(17) . ? Ag1' N1 2.014(3) 2_655 ? Ag1' N2 2.051(3) . ? N2 C16 1.491(3) . ? N2 C10 1.494(3) . ? C10 C12 1.528(4) . ? C10 C13 1.534(4) . ? C10 C11 1.547(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 C14 1.520(4) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 C15 1.525(4) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C15 C16 1.533(4) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C18 1.532(4) . ? C16 C17 1.550(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 . ? N1 C1 1.490(3) . ? N1 C4 1.493(3) . ? C1 C8 1.530(4) . ? C1 C7 1.536(4) . ? C1 C9 1.550(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 . ? C7 C6 1.516(4) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C6 C5 1.525(4) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C5 C4 1.536(4) . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C4 C2 1.522(4) . ? C4 C3 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 . ?