#------------------------------------------------------------------------------ #$Date: 2018-12-08 02:00:07 +0200 (Sat, 08 Dec 2018) $ #$Revision: 212481 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/23/19/7231962.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_7231962 loop_ _publ_author_name 'Kobayashi, Jun' 'Misawa, Toshiyuki' 'Umeda, Chihiro' 'Isono, Toru' 'Ono, Seiji' 'Naruke, Haruo' 'Okamura, Yosuke' 'Koguchi, Shinichi' 'Higuchi, Masashi' 'Nagase, Yu' 'Ito, Takeru' _publ_section_title ; Controlled introduction of metal cations into polymerizable ionic liquid-polyoxomolybdate hybrid crystals ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/C8CE01658E _journal_year 2018 _chemical_formula_moiety 'C32 H56 Ag2 Mo8 N6 O32' _chemical_formula_sum 'C32 H56 Ag2 Mo8 N6 O32' _chemical_formula_weight 2020.07 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_update_record ; 2018-09-28 deposited with the CCDC. 2018-12-07 downloaded from the CCDC. ; _cell_angle_alpha 87.894(12) _cell_angle_beta 72.005(9) _cell_angle_gamma 75.7836(10) _cell_formula_units_Z 1 _cell_length_a 9.5969(7) _cell_length_b 10.9992(12) _cell_length_c 14.5293(12) _cell_measurement_reflns_used 3732 _cell_measurement_temperature 93 _cell_measurement_theta_max 27.50 _cell_measurement_theta_min 3.10 _cell_volume 1412.7(2) _computing_cell_refinement 'CrystalClear-SM Expert 2.1 b45' _computing_data_collection 'CrystalClear-SM Expert 2.1 b45 (Rigaku, 2015)' _computing_data_reduction 'CrystalClear-SM Expert 2.1 b45' _computing_molecular_graphics 'CrystalStructure 4.3' _computing_publication_material 'CrystalStructure 4.3 (Rigaku, 2018)' _computing_structure_refinement 'SHELXL Version 2014/7 (Sheldrick, 2008)' _computing_structure_solution 'Superflip (Palatinus, et al., 2007)' _diffrn_ambient_temperature 93 _diffrn_detector_area_resol_mean 5.814 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.993 _diffrn_measurement_device_type 'Rigaku XtaLAB P200' _diffrn_measurement_method \w _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71075 _diffrn_reflns_av_R_equivalents 0.0470 _diffrn_reflns_av_unetI/netI 0.0401 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.993 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_number 25493 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.993 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.533 _diffrn_reflns_theta_min 3.096 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 2.478 _exptl_absorpt_correction_T_max 0.928 _exptl_absorpt_correction_T_min 0.788 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'REQAB (Rigaku, 1998)' _exptl_crystal_colour colorless _exptl_crystal_density_diffrn 2.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_description fiber _exptl_crystal_F_000 976.00 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.030 _exptl_crystal_size_min 0.030 _refine_diff_density_max 1.07 _refine_diff_density_min -1.26 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.937 _refine_ls_hydrogen_treatment constr _refine_ls_number_parameters 365 _refine_ls_number_reflns 6479 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0370 _refine_ls_R_factor_gt 0.0246 _refine_ls_shift/su_max 0.001 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w = 1/[\s^2^(Fo^2^)+(0.0316P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0546 _refine_ls_wR_factor_ref 0.0577 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5141 _reflns_number_total 6479 _reflns_threshold_expression F^2^>2.0\s(F^2^) _cod_data_source_file c8ce01658e1.cif _cod_data_source_block 20150908_Koba_b _cod_database_code 7231962 _shelx_res_file ; shelxl.res created by SHELXL-2014/7 TITL 20150908_Koba_b CELL 0.71075 9.59690 10.99920 14.52930 87.89400 72.00500 75.78360 ZERR 1 0.00070 0.00120 0.00120 0.01200 0.00900 0.00100 LATT 1 SFAC C H AG MO N O UNIT 32 56 2 8 6 32 L.S. 10 FMAP 2 PLAN 50 WPDB -2 HTAB BOND $H CONF LIST 4 TEMP -180.0 ACTA SIZE 0.300 0.030 0.030 WGHT 0.031600 FVAR 0.08092 AG1 3 1.001964 0.037865 -0.103538 11.00000 0.00827 0.02155 = 0.01683 0.00508 -0.00399 -0.00168 MO1 4 0.627870 0.232687 -0.133679 11.00000 0.00595 0.01144 = 0.01022 0.00278 -0.00389 -0.00259 MO2 4 0.660657 -0.110644 -0.007210 11.00000 0.00358 0.00872 = 0.00895 0.00132 -0.00283 -0.00007 MO3 4 0.628205 -0.140056 0.224341 11.00000 0.00615 0.01091 = 0.00986 0.00197 -0.00448 -0.00061 MO4 4 0.618544 0.164713 0.088519 11.00000 0.00542 0.00932 = 0.01019 0.00108 -0.00421 -0.00114 O1 6 0.558863 0.247588 0.196383 11.00000 0.01211 0.01365 = 0.01230 -0.00077 -0.00535 -0.00294 O2 6 0.584572 0.292480 -0.002152 11.00000 0.01055 0.01159 = 0.01386 0.00276 -0.00658 -0.00377 O3 6 0.569825 -0.042430 0.324155 11.00000 0.01368 0.01833 = 0.01520 -0.00028 -0.00714 -0.00184 O4 6 0.821369 -0.163311 0.181652 11.00000 0.00960 0.01472 = 0.01775 0.00406 -0.00768 -0.00127 O5 6 0.820775 0.177781 -0.166727 11.00000 0.01140 0.01801 = 0.01557 0.00227 -0.00718 -0.00355 O6 6 0.605726 0.062769 -0.039239 11.00000 0.00536 0.01078 = 0.01109 0.00125 -0.00404 -0.00191 O7 6 0.602136 -0.002652 0.127187 11.00000 0.00733 0.01014 = 0.01140 0.00193 -0.00387 -0.00096 O8 6 0.620118 -0.297858 0.278713 11.00000 0.01285 0.01583 = 0.01282 0.00470 -0.00577 -0.00451 O9 6 0.814603 0.132632 0.051469 11.00000 0.00914 0.01412 = 0.01642 0.00160 -0.00608 -0.00178 O10 6 0.612942 0.121287 -0.235848 11.00000 0.00710 0.01497 = 0.01126 0.00106 -0.00304 -0.00034 O11 6 0.852170 -0.137846 -0.034372 11.00000 0.00696 0.01480 = 0.01542 0.00229 -0.00431 -0.00033 O12 6 0.632524 -0.184020 -0.103455 11.00000 0.00689 0.01019 = 0.01302 0.00036 -0.00346 0.00035 O13 6 0.600247 0.374126 -0.185686 11.00000 0.01504 0.01711 = 0.01768 0.00587 -0.00831 -0.00709 O14 6 0.609965 -0.225941 0.091654 11.00000 0.00702 0.01047 = 0.01213 0.00123 -0.00485 -0.00106 O15 6 -0.122271 0.369480 0.463994 11.00000 0.02046 0.07292 = 0.03854 0.00451 -0.00509 -0.00384 O16 6 0.120217 0.327235 0.370196 11.00000 0.01812 0.05007 = 0.02080 0.01451 -0.00785 -0.00814 N1 5 0.161434 0.495895 0.145829 11.00000 0.01130 0.01147 = 0.01748 0.00092 -0.00718 -0.00055 N2 5 0.188118 0.544025 -0.002535 11.00000 0.01022 0.01263 = 0.01987 0.00211 -0.00653 -0.00316 N3 5 1.097272 -0.091333 -0.246838 11.00000 0.02159 0.04429 = 0.02574 -0.00288 -0.00936 -0.00394 C1 1 0.253235 0.472644 0.056153 11.00000 0.01048 0.01199 = 0.01834 0.00079 -0.00568 -0.00193 AFIX 43 H1 2 0.349541 0.414730 0.036769 11.00000 -1.20000 AFIX 0 C2 1 0.051541 0.618234 0.052363 11.00000 0.01339 0.01327 = 0.01997 -0.00096 -0.00846 0.00202 AFIX 43 H2 2 -0.017083 0.679261 0.029084 11.00000 -1.20000 AFIX 0 C3 1 0.033533 0.587869 0.145621 11.00000 0.01344 0.01261 = 0.02267 -0.00159 -0.00733 0.00341 AFIX 43 H3 2 -0.050371 0.622742 0.200325 11.00000 -1.20000 AFIX 0 C4 1 0.253743 0.544172 -0.108123 11.00000 0.01695 0.01810 = 0.01686 0.00166 -0.00485 -0.00498 AFIX 33 H4A 2 0.184125 0.604662 -0.134703 11.00000 -1.20000 H4B 2 0.350230 0.567835 -0.123984 11.00000 -1.20000 H4C 2 0.270699 0.460117 -0.136194 11.00000 -1.20000 AFIX 0 C5 1 0.193493 0.439986 0.232838 11.00000 0.01442 0.01568 = 0.01551 0.00267 -0.00705 -0.00210 AFIX 23 H5A 2 0.194412 0.506921 0.276218 11.00000 -1.20000 H5B 2 0.294725 0.380866 0.213899 11.00000 -1.20000 AFIX 0 C6 1 0.076590 0.371294 0.286091 11.00000 0.02337 0.04277 = 0.02745 0.01903 -0.01568 -0.01610 AFIX 23 H6A 2 -0.025965 0.428337 0.305080 11.00000 -1.20000 H6B 2 0.078235 0.300169 0.245617 11.00000 -1.20000 AFIX 0 C7 1 0.010995 0.333194 0.454901 11.00000 0.02112 0.02847 = 0.02299 0.00244 -0.00344 -0.01003 C8 1 0.077423 0.285713 0.534431 11.00000 0.03430 0.03233 = 0.02124 0.00369 -0.00983 -0.01912 C9 1 -0.017058 0.272414 0.620479 11.00000 0.05430 0.04124 = 0.02193 -0.00015 -0.00469 -0.02775 AFIX 93 H9A 2 -0.122835 0.292659 0.630244 11.00000 -1.20000 H9B 2 0.021021 0.242639 0.672369 11.00000 -1.20000 AFIX 0 C10 1 0.246859 0.256023 0.510887 11.00000 0.04045 0.06823 = 0.03349 0.02307 -0.02571 -0.02983 AFIX 137 H10A 2 0.293910 0.193846 0.456663 11.00000 -1.20000 H10B 2 0.275255 0.222111 0.567669 11.00000 -1.20000 H10C 2 0.281587 0.332805 0.493019 11.00000 -1.20000 AFIX 0 C11 1 0.507459 -0.331929 0.359233 11.00000 0.01766 0.01986 = 0.01014 0.00296 -0.00235 -0.00442 AFIX 23 H11A 2 0.406494 -0.300084 0.350797 11.00000 -1.20000 H11B 2 0.506399 -0.292966 0.419872 11.00000 -1.20000 AFIX 0 C12 1 0.540225 -0.471978 0.366370 11.00000 0.03046 0.02099 = 0.02007 0.00792 -0.00784 -0.00892 AFIX 137 H12A 2 0.640918 -0.503497 0.373587 11.00000 -1.20000 H12B 2 0.536790 -0.510149 0.307468 11.00000 -1.20000 H12C 2 0.464357 -0.493724 0.422716 11.00000 -1.20000 AFIX 0 C13 1 0.726044 0.006321 -0.278894 11.00000 0.01022 0.01674 = 0.02032 -0.00404 -0.00484 0.00136 AFIX 23 H13A 2 0.677361 -0.064658 -0.270811 11.00000 -1.20000 H13B 2 0.803957 -0.012792 -0.245405 11.00000 -1.20000 AFIX 0 C14 1 0.799617 0.021598 -0.385498 11.00000 0.03117 0.02252 = 0.02441 -0.00494 0.00996 -0.00200 AFIX 137 H14A 2 0.881976 -0.052744 -0.412228 11.00000 -1.20000 H14B 2 0.840181 0.096210 -0.393609 11.00000 -1.20000 H14C 2 0.724349 0.031222 -0.419706 11.00000 -1.20000 AFIX 0 C15 1 1.199372 -0.134004 -0.311118 11.00000 0.01918 0.02642 = 0.02088 -0.00190 -0.00829 -0.00478 C16 1 1.330494 -0.189881 -0.392347 11.00000 0.02341 0.02890 = 0.01728 -0.00471 -0.00069 -0.00511 AFIX 137 H16A 2 1.412135 -0.236504 -0.368129 11.00000 -1.20000 H16B 2 1.364321 -0.123574 -0.433594 11.00000 -1.20000 H16C 2 1.303491 -0.247262 -0.430122 11.00000 -1.20000 AFIX 0 HKLF 4 REM 20150908_Koba_b REM R1 = 0.0246 for 5141 Fo > 4sig(Fo) and 0.0370 for all 6479 data REM 365 parameters refined using 0 restraints END WGHT 0.0316 0.0000 REM Instructions for potential hydrogen bonds HTAB C1 O2 EQIV $1 x-1, y+1, z HTAB C2 O11_$1 HTAB C3 O4_$1 EQIV $2 -x+1, -y+1, -z HTAB C4 O1_$2 EQIV $3 -x+1, -y, -z HTAB C4 O8_$3 HTAB C5 O1 HTAB C5 O12_$3 HTAB C11 O10_$3 HTAB C11 O13_$3 HTAB C13 O5 EQIV $4 -x+2, -y, -z HTAB C16 O1_$4 HTAB C16 O15_$3 REM Highest difference peak 1.070, deepest hole -1.261, 1-sigma level 0.153 Q1 1 0.7677 -0.0521 -0.2358 11.00000 0.05 1.07 Q2 1 0.6195 0.3204 -0.1503 11.00000 0.05 0.66 Q3 1 0.5906 0.0724 0.1274 11.00000 0.05 0.66 Q4 1 0.6237 -0.0223 0.0194 11.00000 0.05 0.63 Q5 1 0.6634 -0.0182 -0.0394 11.00000 0.05 0.63 Q6 1 0.6131 -0.2203 0.2509 11.00000 0.05 0.60 Q7 1 0.6040 -0.0571 0.2678 11.00000 0.05 0.60 Q8 1 0.9976 0.1198 -0.1021 11.00000 0.05 0.59 Q9 1 0.6070 0.1421 -0.1919 11.00000 0.05 0.58 Q10 1 0.2410 0.3532 0.0619 11.00000 0.05 0.57 Q11 1 1.0102 -0.0606 -0.0764 11.00000 0.05 0.56 Q12 1 0.6355 -0.1778 0.0685 11.00000 0.05 0.55 Q13 1 1.0336 -0.0458 -0.1487 11.00000 0.05 0.54 Q14 1 0.6587 -0.2147 0.1945 11.00000 0.05 0.53 Q15 1 0.5808 0.2519 0.1339 11.00000 0.05 0.51 Q16 1 0.6359 0.1658 -0.1364 11.00000 0.05 0.51 Q17 1 0.6932 -0.2370 0.0020 11.00000 0.05 0.49 Q18 1 0.6408 0.1183 -0.0320 11.00000 0.05 0.49 Q19 1 0.6073 -0.0301 0.1487 11.00000 0.05 0.48 Q20 1 0.6141 -0.0233 0.1023 11.00000 0.05 0.47 Q21 1 0.6078 -0.2220 0.3053 11.00000 0.05 0.46 Q22 1 0.0417 0.6892 0.0188 11.00000 0.05 0.45 Q23 1 0.5856 0.1082 0.1944 11.00000 0.05 0.44 Q24 1 0.6354 0.0972 0.0492 11.00000 0.05 0.44 Q25 1 0.2369 0.6410 -0.1560 11.00000 0.05 0.44 Q26 1 0.9663 -0.1777 0.1298 11.00000 0.05 0.43 Q27 1 0.1842 0.4380 -0.0478 11.00000 0.05 0.43 Q28 1 0.5883 0.0701 0.0167 11.00000 0.05 0.43 Q29 1 0.0549 0.6383 0.0914 11.00000 0.05 0.43 Q30 1 -0.0997 0.4580 0.4774 11.00000 0.05 0.43 Q31 1 0.3776 0.5140 -0.1303 11.00000 0.05 0.42 Q32 1 0.7792 0.0930 0.0763 11.00000 0.05 0.42 Q33 1 -0.0253 0.4062 0.5459 11.00000 0.05 0.42 Q34 1 0.4138 -0.5416 0.2672 11.00000 0.05 0.41 Q35 1 1.0616 -0.0436 -0.2178 11.00000 0.05 0.41 Q36 1 0.1958 0.4198 -0.0264 11.00000 0.05 0.41 Q37 1 0.5192 -0.3987 0.3651 11.00000 0.05 0.41 Q38 1 0.3633 0.4038 -0.0020 11.00000 0.05 0.41 Q39 1 0.6875 -0.0028 -0.1913 11.00000 0.05 0.40 Q40 1 0.6515 -0.2058 0.1192 11.00000 0.05 0.40 Q41 1 0.9373 0.2569 -0.1845 11.00000 0.05 0.40 Q42 1 0.6769 -0.1867 -0.0712 11.00000 0.05 0.40 Q43 1 -0.0706 0.7626 0.0312 11.00000 0.05 0.40 Q44 1 0.8154 -0.1947 -0.0104 11.00000 0.05 0.39 Q45 1 0.2133 0.1169 0.5709 11.00000 0.05 0.39 Q46 1 0.6936 0.3199 -0.1511 11.00000 0.05 0.39 Q47 1 0.5984 -0.2047 0.1434 11.00000 0.05 0.39 Q48 1 1.1640 -0.1980 -0.1876 11.00000 0.05 0.38 Q49 1 0.1657 0.7549 -0.1416 11.00000 0.05 0.38 Q50 1 0.6156 -0.0058 -0.1293 11.00000 0.05 0.38 ; _shelx_res_checksum 16490 loop_ _space_group_symop_id _space_group_symop_operation_xyz 1 +X,+Y,+Z 2 -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 Ag1 Ag 1.00196(3) 0.03786(2) -0.10354(2) 0.01601(6) Uani 1 1 d . . Mo1 Mo 0.62787(3) 0.23269(2) -0.13368(2) 0.00886(6) Uani 1 1 d . . Mo2 Mo 0.66066(3) -0.11064(2) -0.00721(2) 0.00717(6) Uani 1 1 d . . Mo3 Mo 0.62821(3) -0.14006(2) 0.22434(2) 0.00882(6) Uani 1 1 d . . Mo4 Mo 0.61854(3) 0.16471(2) 0.08852(2) 0.00803(6) Uani 1 1 d . . O1 O 0.5589(3) 0.2476(2) 0.19638(17) 0.0123(4) Uani 1 1 d . . O2 O 0.5846(3) 0.2925(2) -0.00215(17) 0.0112(4) Uani 1 1 d . . O3 O 0.5698(3) -0.0424(2) 0.32416(18) 0.0155(5) Uani 1 1 d . . O4 O 0.8214(3) -0.1633(2) 0.18165(18) 0.0136(5) Uani 1 1 d . . O5 O 0.8208(3) 0.1778(2) -0.16673(18) 0.0143(5) Uani 1 1 d . . O6 O 0.6057(2) 0.0628(2) -0.03924(16) 0.0088(4) Uani 1 1 d . . O7 O 0.6021(2) -0.0027(2) 0.12719(16) 0.0097(4) Uani 1 1 d . . O8 O 0.6201(3) -0.2979(2) 0.27871(17) 0.0133(5) Uani 1 1 d . . O9 O 0.8146(3) 0.1326(2) 0.05147(18) 0.0130(5) Uani 1 1 d . . O10 O 0.6129(3) 0.1213(2) -0.23585(17) 0.0115(4) Uani 1 1 d . . O11 O 0.8522(3) -0.1378(2) -0.03437(17) 0.0127(4) Uani 1 1 d . . O12 O 0.6325(2) -0.1840(2) -0.10345(17) 0.0104(4) Uani 1 1 d . . O13 O 0.6002(3) 0.3741(2) -0.18569(18) 0.0154(5) Uani 1 1 d . . O14 O 0.6100(2) -0.2259(2) 0.09165(16) 0.0097(4) Uani 1 1 d . . O15 O -0.1223(4) 0.3695(4) 0.4640(3) 0.0464(9) Uani 1 1 d . . O16 O 0.1202(3) 0.3272(3) 0.3702(2) 0.0296(7) Uani 1 1 d . . N1 N 0.1614(3) 0.4959(3) 0.1458(2) 0.0132(5) Uani 1 1 d . . N2 N 0.1881(3) 0.5440(3) -0.0025(2) 0.0138(6) Uani 1 1 d . . N3 N 1.0973(4) -0.0913(4) -0.2468(3) 0.0307(8) Uani 1 1 d . . C1 C 0.2532(4) 0.4726(3) 0.0562(3) 0.0135(6) Uani 1 1 d . . H1 H 0.3495 0.4147 0.0368 0.016 Uiso 1 1 calc R U C2 C 0.0515(4) 0.6182(3) 0.0524(3) 0.0157(7) Uani 1 1 d . . H2 H -0.0171 0.6793 0.0291 0.019 Uiso 1 1 calc R U C3 C 0.0335(4) 0.5879(3) 0.1456(3) 0.0170(7) Uani 1 1 d . . H3 H -0.0504 0.6227 0.2003 0.020 Uiso 1 1 calc R U C4 C 0.2537(4) 0.5442(3) -0.1081(3) 0.0173(7) Uani 1 1 d . . H4A H 0.1841 0.6047 -0.1347 0.021 Uiso 1 1 calc R U H4B H 0.3502 0.5678 -0.1240 0.021 Uiso 1 1 calc R U H4C H 0.2707 0.4601 -0.1362 0.021 Uiso 1 1 calc R U C5 C 0.1935(4) 0.4400(3) 0.2328(3) 0.0150(6) Uani 1 1 d . . H5A H 0.1944 0.5069 0.2762 0.018 Uiso 1 1 calc R U H5B H 0.2947 0.3809 0.2139 0.018 Uiso 1 1 calc R U C6 C 0.0766(5) 0.3713(4) 0.2861(3) 0.0284(9) Uani 1 1 d . . H6A H -0.0260 0.4283 0.3051 0.034 Uiso 1 1 calc R U H6B H 0.0782 0.3002 0.2456 0.034 Uiso 1 1 calc R U C7 C 0.0110(5) 0.3332(4) 0.4549(3) 0.0243(8) Uani 1 1 d . . C8 C 0.0774(5) 0.2857(4) 0.5344(3) 0.0271(8) Uani 1 1 d . . C9 C -0.0171(7) 0.2724(5) 0.6205(3) 0.0379(11) Uani 1 1 d . . H9A H -0.1228 0.2927 0.6302 0.045 Uiso 1 1 calc R U H9B H 0.0210 0.2426 0.6724 0.045 Uiso 1 1 calc R U C10 C 0.2469(6) 0.2560(6) 0.5109(4) 0.0416(12) Uani 1 1 d . . H10A H 0.2939 0.1938 0.4567 0.050 Uiso 1 1 calc R U H10B H 0.2753 0.2221 0.5677 0.050 Uiso 1 1 calc R U H10C H 0.2816 0.3328 0.4930 0.050 Uiso 1 1 calc R U C11 C 0.5075(4) -0.3319(3) 0.3592(2) 0.0164(7) Uani 1 1 d . . H11A H 0.4065 -0.3001 0.3508 0.020 Uiso 1 1 calc R U H11B H 0.5064 -0.2930 0.4199 0.020 Uiso 1 1 calc R U C12 C 0.5402(5) -0.4720(3) 0.3664(3) 0.0235(8) Uani 1 1 d . . H12A H 0.6409 -0.5035 0.3736 0.028 Uiso 1 1 calc R U H12B H 0.5368 -0.5101 0.3075 0.028 Uiso 1 1 calc R U H12C H 0.4644 -0.4937 0.4227 0.028 Uiso 1 1 calc R U C13 C 0.7260(4) 0.0063(3) -0.2789(3) 0.0165(7) Uani 1 1 d . . H13A H 0.6774 -0.0647 -0.2708 0.020 Uiso 1 1 calc R U H13B H 0.8040 -0.0128 -0.2454 0.020 Uiso 1 1 calc R U C14 C 0.7996(5) 0.0216(4) -0.3855(3) 0.0311(10) Uani 1 1 d . . H14A H 0.8820 -0.0527 -0.4122 0.037 Uiso 1 1 calc R U H14B H 0.8402 0.0962 -0.3936 0.037 Uiso 1 1 calc R U H14C H 0.7243 0.0312 -0.4197 0.037 Uiso 1 1 calc R U C15 C 1.1994(4) -0.1340(4) -0.3111(3) 0.0217(8) Uani 1 1 d . . C16 C 1.3305(5) -0.1899(4) -0.3923(3) 0.0246(8) Uani 1 1 d . . H16A H 1.4121 -0.2365 -0.3681 0.030 Uiso 1 1 calc R U H16B H 1.3643 -0.1236 -0.4336 0.030 Uiso 1 1 calc R U H16C H 1.3035 -0.2473 -0.4301 0.030 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 0.00827(11) 0.02155(13) 0.01683(13) 0.00508(9) -0.00399(9) -0.00168(9) Mo1 0.00595(12) 0.01144(12) 0.01022(13) 0.00278(9) -0.00389(10) -0.00259(9) Mo2 0.00358(11) 0.00872(11) 0.00895(12) 0.00132(9) -0.00283(9) -0.00007(8) Mo3 0.00615(12) 0.01091(12) 0.00986(13) 0.00197(9) -0.00448(10) -0.00061(9) Mo4 0.00542(12) 0.00932(12) 0.01019(13) 0.00108(9) -0.00421(9) -0.00114(9) O1 0.0121(11) 0.0136(10) 0.0123(11) -0.0008(8) -0.0054(9) -0.0029(8) O2 0.0106(10) 0.0116(10) 0.0139(11) 0.0028(8) -0.0066(9) -0.0038(8) O3 0.0137(11) 0.0183(11) 0.0152(12) -0.0003(9) -0.0071(10) -0.0018(9) O4 0.0096(11) 0.0147(11) 0.0177(12) 0.0041(9) -0.0077(9) -0.0013(9) O5 0.0114(11) 0.0180(11) 0.0156(12) 0.0023(9) -0.0072(9) -0.0036(9) O6 0.0054(10) 0.0108(10) 0.0111(10) 0.0013(8) -0.0040(8) -0.0019(8) O7 0.0073(10) 0.0101(10) 0.0114(11) 0.0019(8) -0.0039(8) -0.0010(8) O8 0.0129(11) 0.0158(11) 0.0128(11) 0.0047(9) -0.0058(9) -0.0045(9) O9 0.0091(10) 0.0141(10) 0.0164(12) 0.0016(9) -0.0061(9) -0.0018(8) O10 0.0071(10) 0.0150(10) 0.0113(11) 0.0011(8) -0.0030(9) -0.0003(8) O11 0.0070(10) 0.0148(10) 0.0154(11) 0.0023(8) -0.0043(9) -0.0003(8) O12 0.0069(10) 0.0102(10) 0.0130(11) 0.0004(8) -0.0035(9) 0.0004(8) O13 0.0150(11) 0.0171(11) 0.0177(12) 0.0059(9) -0.0083(10) -0.0071(9) O14 0.0070(10) 0.0105(10) 0.0121(11) 0.0012(8) -0.0049(8) -0.0011(8) O15 0.0205(16) 0.073(3) 0.039(2) 0.0045(18) -0.0051(14) -0.0038(16) O16 0.0181(13) 0.0501(18) 0.0208(14) 0.0145(13) -0.0079(11) -0.0081(12) N1 0.0113(13) 0.0115(12) 0.0175(14) 0.0009(10) -0.0072(11) -0.0006(10) N2 0.0102(13) 0.0126(12) 0.0199(15) 0.0021(11) -0.0065(11) -0.0032(10) N3 0.0216(17) 0.044(2) 0.0257(19) -0.0029(16) -0.0094(15) -0.0039(15) C1 0.0105(14) 0.0120(14) 0.0183(17) 0.0008(12) -0.0057(13) -0.0019(11) C2 0.0134(15) 0.0133(14) 0.0200(17) -0.0010(12) -0.0085(13) 0.0020(12) C3 0.0134(16) 0.0126(14) 0.0227(18) -0.0016(12) -0.0073(14) 0.0034(12) C4 0.0170(16) 0.0181(16) 0.0169(17) 0.0017(13) -0.0048(14) -0.0050(13) C5 0.0144(15) 0.0157(15) 0.0155(16) 0.0027(12) -0.0070(13) -0.0021(12) C6 0.023(2) 0.043(2) 0.027(2) 0.0190(18) -0.0157(17) -0.0161(17) C7 0.0211(19) 0.0285(19) 0.023(2) 0.0024(15) -0.0034(16) -0.0100(15) C8 0.034(2) 0.032(2) 0.021(2) 0.0037(16) -0.0098(17) -0.0191(17) C9 0.054(3) 0.041(2) 0.022(2) -0.0002(18) -0.005(2) -0.028(2) C10 0.040(3) 0.068(3) 0.033(3) 0.023(2) -0.026(2) -0.030(2) C11 0.0177(16) 0.0199(16) 0.0101(16) 0.0030(12) -0.0023(13) -0.0044(13) C12 0.030(2) 0.0210(17) 0.0201(19) 0.0079(14) -0.0078(16) -0.0089(15) C13 0.0102(15) 0.0167(15) 0.0203(18) -0.0040(13) -0.0048(13) 0.0014(12) C14 0.031(2) 0.0225(18) 0.024(2) -0.0049(15) 0.0100(17) -0.0020(16) C15 0.0192(18) 0.0264(18) 0.0209(19) -0.0019(14) -0.0083(16) -0.0048(15) C16 0.0234(19) 0.0289(19) 0.0173(18) -0.0047(15) -0.0007(15) -0.0051(15) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; H H 0.0000 0.0000 ; International Tables for Crystallography (Vol. C, Table 6.1.1.4) ; Ag Ag -0.8971 1.1015 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; Mo Mo -1.6832 0.6857 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; N N 0.0061 0.0033 ; International Tables for Crystallography (Vol. C, Tables 4.2.6.8 and 6.1.1.4) ; O O 0.0106 0.0060 ; International Tables for Crystallography (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 N3 Ag1 O5 91.25(10) . . N3 Ag1 O4 87.87(12) . 2_755 O5 Ag1 O4 87.19(8) . 2_755 N3 Ag1 O9 156.08(11) . . O5 Ag1 O9 81.03(8) . . O4 Ag1 O9 114.10(8) 2_755 . N3 Ag1 O9 81.76(10) . 2_755 O5 Ag1 O9 171.64(8) . 2_755 O4 Ag1 O9 97.07(8) 2_755 2_755 O9 Ag1 O9 103.58(6) . 2_755 N3 Ag1 Ag1 128.18(10) . 2_755 O5 Ag1 Ag1 132.77(6) . 2_755 O4 Ag1 Ag1 115.36(6) 2_755 2_755 O9 Ag1 Ag1 52.21(5) . 2_755 O9 Ag1 Ag1 51.37(6) 2_755 2_755 O13 Mo1 O5 104.36(12) . . O13 Mo1 O2 98.42(11) . . O5 Mo1 O2 100.84(10) . . O13 Mo1 O10 100.35(11) . . O5 Mo1 O10 92.01(10) . . O2 Mo1 O10 153.83(10) . . O13 Mo1 O14 94.91(10) . 2_655 O5 Mo1 O14 158.20(10) . 2_655 O2 Mo1 O14 86.08(9) . 2_655 O10 Mo1 O14 74.31(9) . 2_655 O13 Mo1 O6 165.84(10) . . O5 Mo1 O6 88.88(10) . . O2 Mo1 O6 73.74(9) . . O10 Mo1 O6 83.92(9) . . O14 Mo1 O6 73.10(8) 2_655 . O11 Mo2 O12 105.06(11) . . O11 Mo2 O14 103.14(10) . . O12 Mo2 O14 99.59(10) . . O11 Mo2 O6 101.89(10) . . O12 Mo2 O6 99.92(10) . . O14 Mo2 O6 142.82(9) . . O11 Mo2 O7 96.86(10) . . O12 Mo2 O7 158.07(9) . . O14 Mo2 O7 75.55(9) . . O6 Mo2 O7 74.55(9) . . O11 Mo2 O6 175.89(10) . 2_655 O12 Mo2 O6 78.98(9) . 2_655 O14 Mo2 O6 76.67(8) . 2_655 O6 Mo2 O6 76.43(10) . 2_655 O7 Mo2 O6 79.09(8) . 2_655 O3 Mo3 O4 105.67(12) . . O3 Mo3 O8 102.40(11) . . O4 Mo3 O8 98.42(10) . . O3 Mo3 O7 96.60(10) . . O4 Mo3 O7 90.86(10) . . O8 Mo3 O7 155.66(10) . . O3 Mo3 O10 88.88(10) . 2_655 O4 Mo3 O10 163.79(10) . 2_655 O8 Mo3 O10 85.06(9) . 2_655 O7 Mo3 O10 80.20(9) . 2_655 O3 Mo3 O14 156.25(9) . . O4 Mo3 O14 95.00(10) . . O8 Mo3 O14 85.66(9) . . O7 Mo3 O14 71.08(8) . . O10 Mo3 O14 69.37(8) 2_655 . O1 Mo4 O9 105.75(11) . . O1 Mo4 O2 103.27(10) . . O9 Mo4 O2 97.63(11) . . O1 Mo4 O7 103.08(11) . . O9 Mo4 O7 96.91(10) . . O2 Mo4 O7 145.02(10) . . O1 Mo4 O6 158.98(10) . . O9 Mo4 O6 95.22(10) . . O2 Mo4 O6 74.63(9) . . O7 Mo4 O6 72.50(9) . . O1 Mo4 O12 87.69(10) . 2_655 O9 Mo4 O12 166.55(10) . 2_655 O2 Mo4 O12 78.21(9) . 2_655 O7 Mo4 O12 80.30(9) . 2_655 O6 Mo4 O12 71.36(8) . 2_655 Mo4 O2 Mo1 115.63(11) . . Mo3 O4 Ag1 136.27(12) . 2_755 Mo1 O5 Ag1 137.01(13) . . Mo2 O6 Mo4 102.12(9) . . Mo2 O6 Mo1 155.21(12) . . Mo4 O6 Mo1 91.88(8) . . Mo2 O6 Mo2 103.57(10) . 2_655 Mo4 O6 Mo2 95.78(8) . 2_655 Mo1 O6 Mo2 95.13(7) . 2_655 Mo4 O7 Mo3 146.97(12) . . Mo4 O7 Mo2 105.11(10) . . Mo3 O7 Mo2 102.47(9) . . C11 O8 Mo3 130.1(2) . . Mo4 O9 Ag1 130.01(12) . . Mo4 O9 Ag1 128.69(12) . 2_755 Ag1 O9 Ag1 76.42(6) . 2_755 C13 O10 Mo1 124.43(19) . . C13 O10 Mo3 119.7(2) . 2_655 Mo1 O10 Mo3 110.24(10) . 2_655 Mo2 O12 Mo4 113.86(11) . 2_655 Mo2 O14 Mo1 113.43(10) . 2_655 Mo2 O14 Mo3 104.38(10) . . Mo1 O14 Mo3 103.31(9) 2_655 . C7 O16 C6 118.1(3) . . C1 N1 C3 109.0(3) . . C1 N1 C5 125.7(3) . . C3 N1 C5 125.2(3) . . C1 N2 C2 108.8(3) . . C1 N2 C4 125.1(3) . . C2 N2 C4 126.1(3) . . C15 N3 Ag1 146.8(3) . . N1 C1 N2 108.5(3) . . N1 C1 H1 125.7 . . N2 C1 H1 125.7 . . C3 C2 N2 107.1(3) . . C3 C2 H2 126.5 . . N2 C2 H2 126.5 . . C2 C3 N1 106.6(3) . . C2 C3 H3 126.7 . . N1 C3 H3 126.7 . . N2 C4 H4A 109.5 . . N2 C4 H4B 109.5 . . H4A C4 H4B 109.5 . . N2 C4 H4C 109.5 . . H4A C4 H4C 109.5 . . H4B C4 H4C 109.5 . . N1 C5 C6 111.0(3) . . N1 C5 H5A 109.4 . . C6 C5 H5A 109.4 . . N1 C5 H5B 109.4 . . C6 C5 H5B 109.4 . . H5A C5 H5B 108.0 . . O16 C6 C5 104.1(3) . . O16 C6 H6A 110.9 . . C5 C6 H6A 110.9 . . O16 C6 H6B 110.9 . . C5 C6 H6B 110.9 . . H6A C6 H6B 109.0 . . O15 C7 O16 123.6(4) . . O15 C7 C8 125.7(4) . . O16 C7 C8 110.7(3) . . C9 C8 C7 117.8(4) . . C9 C8 C10 124.4(4) . . C7 C8 C10 117.8(4) . . C8 C9 H9A 120.0 . . C8 C9 H9B 120.0 . . H9A C9 H9B 120.0 . . C8 C10 H10A 109.5 . . C8 C10 H10B 109.5 . . H10A C10 H10B 109.5 . . C8 C10 H10C 109.5 . . H10A C10 H10C 109.5 . . H10B C10 H10C 109.5 . . O8 C11 C12 110.4(3) . . O8 C11 H11A 109.6 . . C12 C11 H11A 109.6 . . O8 C11 H11B 109.6 . . C12 C11 H11B 109.6 . . H11A C11 H11B 108.1 . . C11 C12 H12A 109.5 . . C11 C12 H12B 109.5 . . H12A C12 H12B 109.5 . . C11 C12 H12C 109.5 . . H12A C12 H12C 109.5 . . H12B C12 H12C 109.5 . . O10 C13 C14 110.1(3) . . O10 C13 H13A 109.6 . . C14 C13 H13A 109.6 . . O10 C13 H13B 109.6 . . C14 C13 H13B 109.6 . . H13A C13 H13B 108.1 . . C13 C14 H14A 109.5 . . C13 C14 H14B 109.5 . . H14A C14 H14B 109.5 . . C13 C14 H14C 109.5 . . H14A C14 H14C 109.5 . . H14B C14 H14C 109.5 . . N3 C15 C16 179.2(5) . . C15 C16 H16A 109.5 . . C15 C16 H16B 109.5 . . H16A C16 H16B 109.5 . . C15 C16 H16C 109.5 . . H16A C16 H16C 109.5 . . H16B C16 H16C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Ag1 N3 2.365(4) . Ag1 O5 2.409(2) . Ag1 O4 2.431(3) 2_755 Ag1 O9 2.478(2) . Ag1 O9 2.507(2) 2_755 Ag1 Ag1 3.0836(6) 2_755 Mo1 O13 1.702(2) . Mo1 O5 1.716(2) . Mo1 O2 1.930(2) . Mo1 O10 2.019(2) . Mo1 O14 2.192(2) 2_655 Mo1 O6 2.291(2) . Mo2 O11 1.707(2) . Mo2 O12 1.762(2) . Mo2 O14 1.909(2) . Mo2 O6 1.930(2) . Mo2 O7 2.169(2) . Mo2 O6 2.359(2) 2_655 Mo3 O3 1.699(2) . Mo3 O4 1.719(2) . Mo3 O8 1.890(2) . Mo3 O7 2.053(2) . Mo3 O10 2.226(2) 2_655 Mo3 O14 2.250(2) . Mo4 O1 1.706(2) . Mo4 O9 1.737(2) . Mo4 O2 1.929(2) . Mo4 O7 1.934(2) . Mo4 O6 2.254(2) . Mo4 O12 2.308(2) 2_655 O4 Ag1 2.431(3) 2_755 O6 Mo2 2.359(2) 2_655 O8 C11 1.436(4) . O9 Ag1 2.507(2) 2_755 O10 C13 1.460(4) . O10 Mo3 2.226(2) 2_655 O12 Mo4 2.308(2) 2_655 O14 Mo1 2.192(2) 2_655 O15 C7 1.209(5) . O16 C7 1.339(5) . O16 C6 1.441(5) . N1 C1 1.321(5) . N1 C3 1.386(4) . N1 C5 1.470(4) . N2 C1 1.332(4) . N2 C2 1.377(4) . N2 C4 1.467(5) . N3 C15 1.137(5) . C1 H1 0.9500 . C2 C3 1.352(5) . C2 H2 0.9500 . C3 H3 0.9500 . C4 H4A 0.9800 . C4 H4B 0.9800 . C4 H4C 0.9800 . C5 C6 1.505(5) . C5 H5A 0.9900 . C5 H5B 0.9900 . C6 H6A 0.9900 . C6 H6B 0.9900 . C7 C8 1.504(6) . C8 C9 1.326(6) . C8 C10 1.507(7) . C9 H9A 0.9500 . C9 H9B 0.9500 . C10 H10A 0.9800 . C10 H10B 0.9800 . C10 H10C 0.9800 . C11 C12 1.501(5) . C11 H11A 0.9900 . C11 H11B 0.9900 . C12 H12A 0.9800 . C12 H12B 0.9800 . C12 H12C 0.9800 . C13 C14 1.513(5) . C13 H13A 0.9900 . C13 H13B 0.9900 . C14 H14A 0.9800 . C14 H14B 0.9800 . C14 H14C 0.9800 . C15 C16 1.453(5) . C16 H16A 0.9800 . C16 H16B 0.9800 . C16 H16C 0.9800 . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_4 O3 Mo3 O4 Ag1 -70.1(2) . 2_755 O8 Mo3 O4 Ag1 -175.62(17) . 2_755 O7 Mo3 O4 Ag1 26.96(18) . 2_755 O10 Mo3 O4 Ag1 83.0(4) 2_655 2_755 O14 Mo3 O4 Ag1 98.04(17) . 2_755 O13 Mo1 O5 Ag1 153.63(17) . . O2 Mo1 O5 Ag1 51.93(19) . . O10 Mo1 O5 Ag1 -105.15(18) . . O14 Mo1 O5 Ag1 -55.0(4) 2_655 . O6 Mo1 O5 Ag1 -21.28(18) . . O3 Mo3 O8 C11 42.5(3) . . O4 Mo3 O8 C11 150.7(3) . . O7 Mo3 O8 C11 -97.9(3) . . O10 Mo3 O8 C11 -45.2(3) 2_655 . O14 Mo3 O8 C11 -114.9(3) . . O1 Mo4 O9 Ag1 -172.49(14) . . O2 Mo4 O9 Ag1 -66.33(15) . . O7 Mo4 O9 Ag1 81.78(15) . . O6 Mo4 O9 Ag1 8.82(15) . . O12 Mo4 O9 Ag1 4.7(5) 2_655 . O1 Mo4 O9 Ag1 81.28(16) . 2_755 O2 Mo4 O9 Ag1 -172.55(14) . 2_755 O7 Mo4 O9 Ag1 -24.45(16) . 2_755 O6 Mo4 O9 Ag1 -97.41(14) . 2_755 O12 Mo4 O9 Ag1 -101.6(4) 2_655 2_755 O11 Mo2 O12 Mo4 179.90(11) . 2_655 O14 Mo2 O12 Mo4 73.39(12) . 2_655 O6 Mo2 O12 Mo4 -74.81(12) . 2_655 O7 Mo2 O12 Mo4 -1.7(3) . 2_655 O6 Mo2 O12 Mo4 -0.88(10) 2_655 2_655 C3 N1 C1 N2 -1.4(4) . . C5 N1 C1 N2 -177.6(3) . . C2 N2 C1 N1 1.8(4) . . C4 N2 C1 N1 -179.2(3) . . C1 N2 C2 C3 -1.5(4) . . C4 N2 C2 C3 179.5(3) . . N2 C2 C3 N1 0.6(4) . . C1 N1 C3 C2 0.5(4) . . C5 N1 C3 C2 176.6(3) . . C1 N1 C5 C6 -121.6(4) . . C3 N1 C5 C6 62.8(5) . . C7 O16 C6 C5 139.7(4) . . N1 C5 C6 O16 -177.7(3) . . C6 O16 C7 O15 2.6(7) . . C6 O16 C7 C8 -178.9(4) . . O15 C7 C8 C9 5.9(7) . . O16 C7 C8 C9 -172.5(4) . . O15 C7 C8 C10 -174.3(5) . . O16 C7 C8 C10 7.2(6) . . Mo3 O8 C11 C12 172.0(2) . . Mo1 O10 C13 C14 -114.6(3) . . Mo3 O10 C13 C14 94.4(3) 2_655 .