#------------------------------------------------------------------------------ #$Date: 2026-06-16 01:35:41 +0100 (Tue, 16 Jun 2026) $ #$Revision: 306571 $ #$URL: svn://www.crystallography.net/cod/cif/7/06/44/7064445.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_7064445 loop_ _publ_author_name 'Gorbachuk, Elena' 'Mikhaylov, Maxim' 'Tagiltsev, Kirill' 'Yudin, Vasily' 'Sukhikh, Taisiya' 'Sukhov, Aleksandr' 'Faizullin, Bulat' 'Shmelev, Artemiy' 'Nikiforov, Viktor' 'Sokolov, Maxim' 'Yakhvarov, Dmitry' _publ_section_title ; A highly intensive red luminescent benzotriazolate complex of {Mo6I8} with {Ag(tBuXPhos)} ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/D5NJ04454E _journal_year 2026 _chemical_formula_moiety 'C32 H48 Ag F3 N O3 P S' _chemical_formula_sum 'C32 H48 Ag F3 N O3 P S' _chemical_formula_weight 722.61 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_creation_date 2024-11-20 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _audit_update_record ; 2025-09-28 deposited with the CCDC. 2026-05-11 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 100.459(4) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 9.0695(11) _cell_length_b 22.929(2) _cell_length_c 16.5120(17) _cell_measurement_reflns_used 9891 _cell_measurement_temperature 150(2) _cell_measurement_theta_max 28.79 _cell_measurement_theta_min 2.45 _cell_volume 3376.7(6) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX3' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2014/7 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 150(2) _diffrn_detector PIXEL _diffrn_detector_area_resol_mean 7.41 _diffrn_detector_type 'Bruker PHOTON III area detector' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker D8 Venture diffractometer' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'Incoatec HELIOS multilayer mirrors' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0694 _diffrn_reflns_av_unetI/netI 0.0621 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 44550 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 29.130 _diffrn_reflns_theta_min 1.537 _diffrn_source 'Incoatec IuS3.0 microfocus X-ray tube' _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_voltage 50.0 _exptl_absorpt_coefficient_mu 0.755 _exptl_absorpt_correction_T_max 0.7461 _exptl_absorpt_correction_T_min 0.6410 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1521 before and 0.0651 after correction. The Ratio of minimum to maximum transmission is 0.8591. The \l/2 correction factor is Not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.421 _exptl_crystal_description needle _exptl_crystal_F_000 1504 _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.04 _refine_diff_density_max 0.710 _refine_diff_density_min -0.831 _refine_diff_density_rms 0.112 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.055 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 392 _refine_ls_number_reflns 9023 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.055 _refine_ls_R_factor_all 0.0702 _refine_ls_R_factor_gt 0.0521 _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^)+(0.0445P)^2^+6.2585P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1178 _refine_ls_wR_factor_ref 0.1269 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7017 _reflns_number_total 9023 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d5nj04454e2.cif _cod_data_source_block gev17_a _cod_original_cell_volume 3376.6(6) _cod_database_code 7064445 _shelx_shelxl_version_number 2014/7 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.970 _shelx_estimated_absorpt_t_min 0.828 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2.a Ternary CH refined with riding coordinates: C13(H13), C16(H16), C19(H19) 2.b Aromatic/amide H refined with riding coordinates: C2(H2), C3(H3), C4(H4), C5(H5), C9(H9), C11(H11) 2.c Idealised Me refined as rotating group: C14(H14A,H14B,H14C), C15(H15A,H15B,H15C), C17(H17A,H17B,H17C), C18(H18A,H18B, H18C), C20(H20A,H20B,H20C), C21(H21A,H21B,H21C), C23(H23A,H23B,H23C), C24(H24A, H24B,H24C), C25(H25A,H25B,H25C), C27(H27A,H27B,H27C), C28(H28A,H28B,H28C), C29(H29A,H29B,H29C), C31(H31A,H31B,H31C) ; _shelx_res_file ; gev17_a.res created by SHELXL-2014/7 TITL gev17_a_a.res in P2(1)/c REM Old TITL GEV17_a in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.123, Rweak 0.011, Alpha 0.060, Orientation as input REM Formula found by SHELXT: C39 P2 Ag CELL 0.71073 9.0695 22.9286 16.512 90 100.459 90 ZERR 4 0.0011 0.002 0.0017 0 0.004 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Ag F N O P S UNIT 128 192 4 12 4 12 4 4 L.S. 4 0 0 PLAN 11 SIZE 0.26 0.06 0.04 TEMP -123(2) list 4 MORE -1 BOND $H fmap 2 53 acta SHEL 17 0.73 OMIT -6 12 3 OMIT 1 0 0 OMIT 1 15 0 OMIT 1 17 6 OMIT 2 16 6 OMIT 3 14 5 REM REM REM WGHT 0.044500 6.258500 FVAR 0.40902 AG1 3 0.395381 0.330254 0.247774 11.00000 0.02479 0.01970 = 0.02713 0.00287 0.00446 0.00709 S1 8 0.221597 0.191057 0.297857 11.00000 0.02250 0.01847 = 0.03011 0.00233 0.00763 -0.00223 P1 7 0.229706 0.395923 0.163697 11.00000 0.01841 0.01517 = 0.01841 0.00011 0.00441 0.00280 F1 4 0.421361 0.149668 0.216059 11.00000 0.05914 0.06048 = 0.05773 -0.01569 0.04277 -0.01274 F2 4 0.305664 0.084027 0.273605 11.00000 0.04908 0.02402 = 0.08507 -0.01772 0.03061 -0.00621 F3 4 0.477090 0.136248 0.346959 11.00000 0.02886 0.05065 = 0.06259 -0.00243 0.00419 0.00976 O1 6 0.305928 0.244474 0.310443 11.00000 0.03721 0.02059 = 0.04817 0.00242 0.01163 -0.00872 O2 6 0.112812 0.187906 0.223073 11.00000 0.03784 0.04610 = 0.03947 0.00671 -0.00445 -0.00485 O3 6 0.169952 0.170139 0.369878 11.00000 0.03329 0.03148 = 0.03647 0.00075 0.01813 -0.00101 N1 5 0.607260 0.278397 0.267944 11.00000 0.02223 0.02883 = 0.03630 0.00017 0.00617 0.00152 C1 1 0.175452 0.457967 0.222052 11.00000 0.01416 0.01234 = 0.02311 0.00103 0.00545 0.00183 C2 1 0.092818 0.503435 0.179093 11.00000 0.01879 0.01906 = 0.02414 0.00135 0.00299 0.00170 AFIX 43 H2 2 0.068728 0.501189 0.120735 11.00000 -1.20000 AFIX 0 C3 1 0.044534 0.551574 0.217785 11.00000 0.02043 0.01840 = 0.02898 0.00266 0.00336 0.00750 AFIX 43 H3 2 -0.012899 0.581279 0.186635 11.00000 -1.20000 AFIX 0 C4 1 0.081650 0.555560 0.302842 11.00000 0.02107 0.01756 = 0.02882 -0.00442 0.00711 0.00399 AFIX 43 H4 2 0.049676 0.588115 0.330770 11.00000 -1.20000 AFIX 0 C5 1 0.165719 0.511692 0.346749 11.00000 0.01604 0.02213 = 0.02568 -0.00221 0.00360 0.00352 AFIX 43 H5 2 0.191496 0.515265 0.404922 11.00000 -1.20000 AFIX 0 C6 1 0.214415 0.462310 0.309222 11.00000 0.01193 0.01543 = 0.02354 0.00129 0.00355 -0.00018 C7 1 0.304717 0.418398 0.365460 11.00000 0.01351 0.01592 = 0.01735 -0.00049 0.00482 0.00158 C8 1 0.462886 0.418263 0.376133 11.00000 0.01297 0.01758 = 0.01944 0.00020 0.00432 -0.00138 C9 1 0.543984 0.379180 0.431548 11.00000 0.01236 0.02155 = 0.02233 0.00317 0.00626 0.00080 AFIX 43 H9 2 0.650101 0.378481 0.437243 11.00000 -1.20000 AFIX 0 C10 1 0.475623 0.341123 0.478884 11.00000 0.01746 0.01643 = 0.01885 0.00126 0.00599 0.00224 C11 1 0.320299 0.343462 0.470022 11.00000 0.01627 0.01815 = 0.02151 0.00347 0.00643 -0.00023 AFIX 43 H11 2 0.271639 0.318496 0.502820 11.00000 -1.20000 AFIX 0 C12 1 0.233571 0.381240 0.414584 11.00000 0.01225 0.01716 = 0.02004 -0.00187 0.00471 -0.00179 C13 1 0.065155 0.383039 0.414270 11.00000 0.01395 0.02114 = 0.02365 0.00190 0.00667 0.00041 AFIX 13 H13 2 0.016219 0.406005 0.365207 11.00000 -1.20000 AFIX 0 C14 1 -0.005747 0.322196 0.409006 11.00000 0.01869 0.02655 = 0.03415 0.00181 0.00819 -0.00379 AFIX 137 H14A 2 0.028108 0.299855 0.365205 11.00000 -1.50000 H14B 2 -0.115201 0.325829 0.396748 11.00000 -1.50000 H14C 2 0.024496 0.301983 0.461699 11.00000 -1.50000 AFIX 0 C15 1 0.034796 0.414025 0.492097 11.00000 0.01764 0.03356 = 0.03423 -0.00566 0.00951 0.00077 AFIX 137 H15A 2 0.087133 0.393471 0.541004 11.00000 -1.50000 H15B 2 -0.073213 0.414062 0.492235 11.00000 -1.50000 H15C 2 0.071101 0.454307 0.492694 11.00000 -1.50000 AFIX 0 C16 1 0.564403 0.298045 0.537894 11.00000 0.01910 0.02270 = 0.02430 0.01017 0.00498 0.00403 AFIX 13 H16 2 0.496062 0.281997 0.573607 11.00000 -1.20000 AFIX 0 C17 1 0.697977 0.325928 0.593929 11.00000 0.03002 0.03524 = 0.02828 0.00838 -0.00343 0.00143 AFIX 137 H17A 2 0.768181 0.341168 0.560472 11.00000 -1.50000 H17B 2 0.748683 0.296618 0.632390 11.00000 -1.50000 H17C 2 0.662908 0.357918 0.624936 11.00000 -1.50000 AFIX 0 C18 1 0.617516 0.246717 0.490093 11.00000 0.03297 0.02211 = 0.03848 0.00404 0.00404 0.01058 AFIX 137 H18A 2 0.531765 0.230377 0.452178 11.00000 -1.50000 H18B 2 0.662021 0.216530 0.528991 11.00000 -1.50000 H18C 2 0.692516 0.260627 0.458734 11.00000 -1.50000 AFIX 0 C19 1 0.545905 0.465764 0.338196 11.00000 0.01401 0.01921 = 0.02233 0.00664 0.00304 -0.00085 AFIX 13 H19 2 0.475491 0.482391 0.290088 11.00000 -1.20000 AFIX 0 C20 1 0.685434 0.443378 0.307079 11.00000 0.01535 0.03262 = 0.04136 0.01315 0.00949 0.00200 AFIX 137 H20A 2 0.760421 0.430306 0.353958 11.00000 -1.50000 H20B 2 0.727557 0.474880 0.278243 11.00000 -1.50000 H20C 2 0.657242 0.410682 0.269205 11.00000 -1.50000 AFIX 0 C21 1 0.589105 0.514595 0.400916 11.00000 0.04259 0.02577 = 0.03156 -0.00033 0.00868 -0.01302 AFIX 137 H21A 2 0.645694 0.544584 0.377334 11.00000 -1.50000 H21B 2 0.651190 0.498631 0.450770 11.00000 -1.50000 H21C 2 0.498150 0.531906 0.414893 11.00000 -1.50000 AFIX 0 C22 1 0.321936 0.426395 0.077715 11.00000 0.02481 0.02860 = 0.01834 0.00251 0.00683 0.00068 C23 1 0.216068 0.446311 -0.000639 11.00000 0.03572 0.03089 = 0.02229 0.00362 0.00566 -0.00087 AFIX 137 H23A 2 0.148973 0.476708 0.013345 11.00000 -1.50000 H23B 2 0.156545 0.413043 -0.025410 11.00000 -1.50000 H23C 2 0.275054 0.461904 -0.039908 11.00000 -1.50000 AFIX 0 C24 1 0.423296 0.377898 0.053529 11.00000 0.03805 0.04733 = 0.02688 0.00091 0.01537 0.01201 AFIX 137 H24A 2 0.361880 0.343998 0.033051 11.00000 -1.50000 H24B 2 0.497363 0.366572 0.101837 11.00000 -1.50000 H24C 2 0.475110 0.392281 0.010318 11.00000 -1.50000 AFIX 0 C25 1 0.420381 0.477549 0.112265 11.00000 0.03091 0.04558 = 0.02788 0.00010 0.01077 -0.01185 AFIX 137 H25A 2 0.479092 0.490653 0.071367 11.00000 -1.50000 H25B 2 0.488379 0.465335 0.162472 11.00000 -1.50000 H25C 2 0.357103 0.509620 0.125219 11.00000 -1.50000 AFIX 0 C26 1 0.047718 0.357643 0.121831 11.00000 0.02517 0.02036 = 0.02430 -0.00302 0.00328 -0.00193 C27 1 0.082489 0.305003 0.070740 11.00000 0.04394 0.02358 = 0.03047 -0.00783 0.01126 -0.00608 AFIX 137 H27A 2 0.161341 0.281297 0.103599 11.00000 -1.50000 H27B 2 0.116524 0.318789 0.021047 11.00000 -1.50000 H27C 2 -0.008237 0.281376 0.055011 11.00000 -1.50000 AFIX 0 C28 1 -0.009387 0.335241 0.198380 11.00000 0.02463 0.03013 = 0.03153 -0.00295 0.00913 -0.00634 AFIX 137 H28A 2 0.067531 0.310631 0.231121 11.00000 -1.50000 H28B 2 -0.100972 0.312367 0.181097 11.00000 -1.50000 H28C 2 -0.031092 0.368458 0.231679 11.00000 -1.50000 AFIX 0 C29 1 -0.079226 0.394194 0.071725 11.00000 0.02313 0.03238 = 0.03959 0.00376 -0.00290 -0.00653 AFIX 137 H29A 2 -0.167986 0.369616 0.055181 11.00000 -1.50000 H29B 2 -0.046565 0.409639 0.022528 11.00000 -1.50000 H29C 2 -0.103996 0.426613 0.105546 11.00000 -1.50000 AFIX 0 C30 1 0.692364 0.242221 0.287935 11.00000 0.02072 0.02590 = 0.03195 -0.00353 0.00592 -0.00147 C31 1 0.797831 0.195388 0.313237 11.00000 0.02340 0.03108 = 0.03927 -0.00080 0.00340 0.00840 AFIX 137 H31A 2 0.881532 0.198435 0.283364 11.00000 -1.50000 H31B 2 0.747374 0.157785 0.300906 11.00000 -1.50000 H31C 2 0.835953 0.198253 0.372560 11.00000 -1.50000 AFIX 0 C32 1 0.363339 0.137764 0.282451 11.00000 0.03208 0.02913 = 0.04124 -0.00830 0.01632 -0.00538 HKLF 4 REM gev17_a_a.res in P2(1)/c REM R1 = 0.0521 for 7017 Fo > 4sig(Fo) and 0.0702 for all 9023 data REM 392 parameters refined using 0 restraints END WGHT 0.0445 6.2644 REM Highest difference peak 0.710, deepest hole -0.831, 1-sigma level 0.112 Q1 1 0.4414 0.3992 0.2396 11.00000 0.05 0.71 Q2 1 0.4540 0.3344 0.3792 11.00000 0.05 0.61 Q3 1 0.4423 0.3268 0.3315 11.00000 0.05 0.58 Q4 1 0.3376 0.3353 0.1192 11.00000 0.05 0.58 Q5 1 0.3476 0.2765 0.2413 11.00000 0.05 0.54 Q6 1 0.3763 0.2725 0.2740 11.00000 0.05 0.53 Q7 1 0.3718 0.2662 0.2547 11.00000 0.05 0.49 Q8 1 0.1629 0.4809 0.1882 11.00000 0.05 0.47 Q9 1 0.3563 0.3532 0.1794 11.00000 0.05 0.47 Q10 1 -0.2072 0.3363 0.1965 11.00000 0.05 0.46 Q11 1 0.3479 0.3392 0.1640 11.00000 0.05 0.46 ; _shelx_res_checksum 76943 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 0.39538(3) 0.33025(2) 0.24777(2) 0.02391(8) Uani 1 1 d . . . . . S1 S 0.22160(10) 0.19106(4) 0.29786(5) 0.02333(18) Uani 1 1 d . . . . . P1 P 0.22971(10) 0.39592(3) 0.16370(5) 0.01720(16) Uani 1 1 d . . . . . F1 F 0.4214(3) 0.14967(13) 0.21606(17) 0.0551(8) Uani 1 1 d . . . . . F2 F 0.3057(3) 0.08403(10) 0.27360(18) 0.0504(7) Uani 1 1 d . . . . . F3 F 0.4771(3) 0.13625(12) 0.34696(17) 0.0479(6) Uani 1 1 d . . . . . O1 O 0.3059(3) 0.24447(11) 0.31044(18) 0.0348(6) Uani 1 1 d . . . . . O2 O 0.1128(4) 0.18791(14) 0.22307(18) 0.0426(7) Uani 1 1 d . . . . . O3 O 0.1700(3) 0.17014(11) 0.36988(17) 0.0323(6) Uani 1 1 d . . . . . N1 N 0.6073(3) 0.27840(14) 0.26794(19) 0.0290(7) Uani 1 1 d . . . . . C1 C 0.1755(3) 0.45797(12) 0.22205(19) 0.0163(6) Uani 1 1 d . . . . . C2 C 0.0928(4) 0.50343(14) 0.1791(2) 0.0208(6) Uani 1 1 d . . . . . H2 H 0.0687 0.5012 0.1207 0.025 Uiso 1 1 calc R U . . . C3 C 0.0445(4) 0.55157(14) 0.2178(2) 0.0227(7) Uani 1 1 d . . . . . H3 H -0.0129 0.5813 0.1866 0.027 Uiso 1 1 calc R U . . . C4 C 0.0817(4) 0.55556(14) 0.3028(2) 0.0222(7) Uani 1 1 d . . . . . H4 H 0.0497 0.5881 0.3308 0.027 Uiso 1 1 calc R U . . . C5 C 0.1657(4) 0.51169(14) 0.3467(2) 0.0213(6) Uani 1 1 d . . . . . H5 H 0.1915 0.5153 0.4049 0.026 Uiso 1 1 calc R U . . . C6 C 0.2144(3) 0.46231(13) 0.30922(19) 0.0169(6) Uani 1 1 d . . . . . C7 C 0.3047(3) 0.41840(13) 0.36546(18) 0.0153(6) Uani 1 1 d . . . . . C8 C 0.4629(3) 0.41826(13) 0.37613(18) 0.0165(6) Uani 1 1 d . . . . . C9 C 0.5440(4) 0.37918(13) 0.43155(19) 0.0184(6) Uani 1 1 d . . . . . H9 H 0.6501 0.3785 0.4372 0.022 Uiso 1 1 calc R U . . . C10 C 0.4756(4) 0.34112(13) 0.47888(18) 0.0172(6) Uani 1 1 d . . . . . C11 C 0.3203(4) 0.34346(13) 0.47002(19) 0.0183(6) Uani 1 1 d . . . . . H11 H 0.2716 0.3185 0.5028 0.022 Uiso 1 1 calc R U . . . C12 C 0.2336(3) 0.38124(13) 0.41458(18) 0.0163(6) Uani 1 1 d . . . . . C13 C 0.0652(4) 0.38304(14) 0.41427(19) 0.0192(6) Uani 1 1 d . . . . . H13 H 0.0162 0.4060 0.3652 0.023 Uiso 1 1 calc R U . . . C14 C -0.0057(4) 0.32220(15) 0.4090(2) 0.0260(7) Uani 1 1 d . . . . . H14A H 0.0281 0.2999 0.3652 0.039 Uiso 1 1 calc R U . . . H14B H -0.1152 0.3258 0.3967 0.039 Uiso 1 1 calc R U . . . H14C H 0.0245 0.3020 0.4617 0.039 Uiso 1 1 calc R U . . . C15 C 0.0348(4) 0.41403(16) 0.4921(2) 0.0279(7) Uani 1 1 d . . . . . H15A H 0.0871 0.3935 0.5410 0.042 Uiso 1 1 calc R U . . . H15B H -0.0732 0.4141 0.4922 0.042 Uiso 1 1 calc R U . . . H15C H 0.0711 0.4543 0.4927 0.042 Uiso 1 1 calc R U . . . C16 C 0.5644(4) 0.29804(14) 0.5379(2) 0.0219(7) Uani 1 1 d . . . . . H16 H 0.4961 0.2820 0.5736 0.026 Uiso 1 1 calc R U . . . C17 C 0.6980(5) 0.32593(17) 0.5939(2) 0.0323(8) Uani 1 1 d . . . . . H17A H 0.7682 0.3412 0.5605 0.048 Uiso 1 1 calc R U . . . H17B H 0.7487 0.2966 0.6324 0.048 Uiso 1 1 calc R U . . . H17C H 0.6629 0.3579 0.6249 0.048 Uiso 1 1 calc R U . . . C18 C 0.6175(5) 0.24672(15) 0.4901(2) 0.0315(8) Uani 1 1 d . . . . . H18A H 0.5318 0.2304 0.4522 0.047 Uiso 1 1 calc R U . . . H18B H 0.6620 0.2165 0.5290 0.047 Uiso 1 1 calc R U . . . H18C H 0.6925 0.2606 0.4587 0.047 Uiso 1 1 calc R U . . . C19 C 0.5459(4) 0.46576(13) 0.33820(19) 0.0185(6) Uani 1 1 d . . . . . H19 H 0.4755 0.4824 0.2901 0.022 Uiso 1 1 calc R U . . . C20 C 0.6854(4) 0.44338(16) 0.3071(2) 0.0292(8) Uani 1 1 d . . . . . H20A H 0.7604 0.4303 0.3540 0.044 Uiso 1 1 calc R U . . . H20B H 0.7276 0.4749 0.2782 0.044 Uiso 1 1 calc R U . . . H20C H 0.6572 0.4107 0.2692 0.044 Uiso 1 1 calc R U . . . C21 C 0.5891(5) 0.51460(16) 0.4009(2) 0.0331(9) Uani 1 1 d . . . . . H21A H 0.6457 0.5446 0.3773 0.050 Uiso 1 1 calc R U . . . H21B H 0.6512 0.4986 0.4508 0.050 Uiso 1 1 calc R U . . . H21C H 0.4982 0.5319 0.4149 0.050 Uiso 1 1 calc R U . . . C22 C 0.3219(4) 0.42640(15) 0.07771(19) 0.0236(7) Uani 1 1 d . . . . . C23 C 0.2161(5) 0.44631(16) -0.0006(2) 0.0296(8) Uani 1 1 d . . . . . H23A H 0.1490 0.4767 0.0133 0.044 Uiso 1 1 calc R U . . . H23B H 0.1565 0.4130 -0.0254 0.044 Uiso 1 1 calc R U . . . H23C H 0.2751 0.4619 -0.0399 0.044 Uiso 1 1 calc R U . . . C24 C 0.4233(5) 0.37790(19) 0.0535(2) 0.0362(9) Uani 1 1 d . . . . . H24A H 0.3619 0.3440 0.0331 0.054 Uiso 1 1 calc R U . . . H24B H 0.4974 0.3666 0.1018 0.054 Uiso 1 1 calc R U . . . H24C H 0.4751 0.3923 0.0103 0.054 Uiso 1 1 calc R U . . . C25 C 0.4204(5) 0.47755(18) 0.1123(2) 0.0341(9) Uani 1 1 d . . . . . H25A H 0.4791 0.4907 0.0714 0.051 Uiso 1 1 calc R U . . . H25B H 0.4884 0.4653 0.1625 0.051 Uiso 1 1 calc R U . . . H25C H 0.3571 0.5096 0.1252 0.051 Uiso 1 1 calc R U . . . C26 C 0.0477(4) 0.35764(14) 0.1218(2) 0.0234(7) Uani 1 1 d . . . . . C27 C 0.0825(5) 0.30500(16) 0.0707(2) 0.0321(8) Uani 1 1 d . . . . . H27A H 0.1613 0.2813 0.1036 0.048 Uiso 1 1 calc R U . . . H27B H 0.1165 0.3188 0.0210 0.048 Uiso 1 1 calc R U . . . H27C H -0.0082 0.2814 0.0550 0.048 Uiso 1 1 calc R U . . . C28 C -0.0094(4) 0.33524(16) 0.1984(2) 0.0283(7) Uani 1 1 d . . . . . H28A H 0.0675 0.3106 0.2311 0.042 Uiso 1 1 calc R U . . . H28B H -0.1010 0.3124 0.1811 0.042 Uiso 1 1 calc R U . . . H28C H -0.0311 0.3685 0.2317 0.042 Uiso 1 1 calc R U . . . C29 C -0.0792(4) 0.39419(17) 0.0717(2) 0.0328(8) Uani 1 1 d . . . . . H29A H -0.1680 0.3696 0.0552 0.049 Uiso 1 1 calc R U . . . H29B H -0.0466 0.4096 0.0225 0.049 Uiso 1 1 calc R U . . . H29C H -0.1040 0.4266 0.1055 0.049 Uiso 1 1 calc R U . . . C30 C 0.6924(4) 0.24222(15) 0.2879(2) 0.0260(7) Uani 1 1 d . . . . . C31 C 0.7978(4) 0.19539(17) 0.3132(2) 0.0315(8) Uani 1 1 d . . . . . H31A H 0.8815 0.1984 0.2834 0.047 Uiso 1 1 calc R U . . . H31B H 0.7474 0.1578 0.3009 0.047 Uiso 1 1 calc R U . . . H31C H 0.8360 0.1983 0.3726 0.047 Uiso 1 1 calc R U . . . C32 C 0.3633(5) 0.13776(17) 0.2825(2) 0.0329(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 Ag1 0.02479(14) 0.01970(13) 0.02713(13) 0.00287(10) 0.00446(10) 0.00709(10) S1 0.0225(4) 0.0185(4) 0.0301(4) 0.0023(3) 0.0076(3) -0.0022(3) P1 0.0184(4) 0.0152(4) 0.0184(4) 0.0001(3) 0.0044(3) 0.0028(3) F1 0.0591(19) 0.0605(17) 0.0577(16) -0.0157(14) 0.0428(15) -0.0127(14) F2 0.0491(16) 0.0240(12) 0.085(2) -0.0177(12) 0.0306(15) -0.0062(11) F3 0.0289(13) 0.0506(16) 0.0626(17) -0.0024(13) 0.0042(12) 0.0098(11) O1 0.0372(16) 0.0206(12) 0.0482(16) 0.0024(11) 0.0116(13) -0.0087(11) O2 0.0378(18) 0.0461(18) 0.0395(15) 0.0067(13) -0.0045(13) -0.0049(14) O3 0.0333(15) 0.0315(14) 0.0365(14) 0.0007(11) 0.0181(12) -0.0010(11) N1 0.0222(16) 0.0288(16) 0.0363(16) 0.0002(13) 0.0062(13) 0.0015(13) C1 0.0142(14) 0.0123(13) 0.0231(14) 0.0010(11) 0.0055(12) 0.0018(11) C2 0.0188(16) 0.0191(15) 0.0241(15) 0.0014(12) 0.0030(13) 0.0017(12) C3 0.0204(17) 0.0184(15) 0.0290(16) 0.0027(13) 0.0034(13) 0.0075(13) C4 0.0211(17) 0.0176(15) 0.0288(16) -0.0044(12) 0.0071(13) 0.0040(12) C5 0.0160(16) 0.0221(16) 0.0257(15) -0.0022(12) 0.0036(12) 0.0035(12) C6 0.0119(14) 0.0154(14) 0.0235(15) 0.0013(11) 0.0035(11) -0.0002(11) C7 0.0135(14) 0.0159(14) 0.0173(13) -0.0005(11) 0.0048(11) 0.0016(11) C8 0.0130(14) 0.0176(14) 0.0194(14) 0.0002(11) 0.0043(11) -0.0014(11) C9 0.0124(14) 0.0215(15) 0.0223(14) 0.0032(12) 0.0063(12) 0.0008(11) C10 0.0175(15) 0.0164(14) 0.0188(14) 0.0013(11) 0.0060(12) 0.0022(11) C11 0.0163(15) 0.0182(15) 0.0215(14) 0.0035(11) 0.0064(12) -0.0002(11) C12 0.0123(14) 0.0172(14) 0.0200(14) -0.0019(11) 0.0047(11) -0.0018(11) C13 0.0139(15) 0.0211(15) 0.0237(15) 0.0019(12) 0.0067(12) 0.0004(12) C14 0.0187(17) 0.0266(18) 0.0342(18) 0.0018(14) 0.0082(14) -0.0038(13) C15 0.0176(17) 0.0336(19) 0.0342(18) -0.0057(15) 0.0095(14) 0.0008(14) C16 0.0191(16) 0.0227(16) 0.0243(15) 0.0102(13) 0.0050(13) 0.0040(12) C17 0.030(2) 0.035(2) 0.0283(18) 0.0084(15) -0.0034(15) 0.0014(16) C18 0.033(2) 0.0221(17) 0.038(2) 0.0040(15) 0.0040(16) 0.0106(15) C19 0.0140(15) 0.0192(15) 0.0223(14) 0.0066(12) 0.0030(12) -0.0009(11) C20 0.0154(17) 0.0326(19) 0.041(2) 0.0132(16) 0.0095(15) 0.0020(14) C21 0.043(2) 0.0258(18) 0.0316(18) -0.0003(15) 0.0087(17) -0.0130(16) C22 0.0248(18) 0.0286(17) 0.0183(14) 0.0025(13) 0.0068(13) 0.0007(14) C23 0.036(2) 0.0309(19) 0.0223(16) 0.0036(14) 0.0057(15) -0.0009(16) C24 0.038(2) 0.047(2) 0.0269(18) 0.0009(16) 0.0154(17) 0.0120(19) C25 0.031(2) 0.046(2) 0.0279(18) 0.0001(16) 0.0108(16) -0.0118(17) C26 0.0252(18) 0.0204(16) 0.0243(16) -0.0030(13) 0.0033(13) -0.0019(13) C27 0.044(2) 0.0236(17) 0.0305(18) -0.0078(14) 0.0113(17) -0.0061(16) C28 0.0246(18) 0.0301(18) 0.0315(18) -0.0029(14) 0.0091(14) -0.0063(14) C29 0.0231(19) 0.032(2) 0.040(2) 0.0038(16) -0.0029(16) -0.0065(15) C30 0.0207(17) 0.0259(17) 0.0319(18) -0.0035(14) 0.0059(14) -0.0015(14) C31 0.0234(19) 0.0311(19) 0.039(2) -0.0008(16) 0.0034(16) 0.0084(15) C32 0.032(2) 0.0291(19) 0.041(2) -0.0083(16) 0.0163(17) -0.0054(16) 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 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 -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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 P1 Ag1 O1 122.34(7) . . ? N1 Ag1 P1 148.96(8) . . ? N1 Ag1 O1 81.39(11) . . ? O1 S1 C32 102.75(18) . . ? O2 S1 O1 115.55(18) . . ? O2 S1 O3 114.74(18) . . ? O2 S1 C32 103.77(19) . . ? O3 S1 O1 114.14(17) . . ? O3 S1 C32 103.62(17) . . ? C1 P1 Ag1 112.60(10) . . ? C1 P1 C22 107.62(15) . . ? C1 P1 C26 104.65(15) . . ? C22 P1 Ag1 110.45(11) . . ? C26 P1 Ag1 109.65(11) . . ? C26 P1 C22 111.75(15) . . ? S1 O1 Ag1 146.87(18) . . ? C30 N1 Ag1 161.7(3) . . ? C2 C1 P1 118.8(2) . . ? C2 C1 C6 118.2(3) . . ? C6 C1 P1 123.0(2) . . ? C1 C2 H2 118.5 . . ? C3 C2 C1 123.0(3) . . ? C3 C2 H2 118.5 . . ? C2 C3 H3 120.6 . . ? C2 C3 C4 118.7(3) . . ? C4 C3 H3 120.6 . . ? C3 C4 H4 120.3 . . ? C5 C4 C3 119.5(3) . . ? C5 C4 H4 120.3 . . ? C4 C5 H5 118.5 . . ? C4 C5 C6 122.9(3) . . ? C6 C5 H5 118.5 . . ? C1 C6 C7 125.8(3) . . ? C5 C6 C1 117.7(3) . . ? C5 C6 C7 116.6(3) . . ? C8 C7 C6 120.3(3) . . ? C12 C7 C6 120.2(3) . . ? C12 C7 C8 119.1(3) . . ? C7 C8 C19 120.9(3) . . ? C9 C8 C7 119.1(3) . . ? C9 C8 C19 119.3(3) . . ? C8 C9 H9 118.7 . . ? C10 C9 C8 122.5(3) . . ? C10 C9 H9 118.7 . . ? C9 C10 C11 117.6(3) . . ? C9 C10 C16 122.2(3) . . ? C11 C10 C16 120.2(3) . . ? C10 C11 H11 118.9 . . ? C10 C11 C12 122.2(3) . . ? C12 C11 H11 118.9 . . ? C7 C12 C13 122.9(3) . . ? C11 C12 C7 119.3(3) . . ? C11 C12 C13 117.6(3) . . ? C12 C13 H13 108.3 . . ? C12 C13 C14 112.6(3) . . ? C12 C13 C15 109.9(3) . . ? C14 C13 H13 108.3 . . ? C14 C13 C15 109.4(3) . . ? C15 C13 H13 108.3 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14B 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C10 C16 H16 107.8 . . ? C10 C16 C17 112.9(3) . . ? C10 C16 C18 110.4(3) . . ? C17 C16 H16 107.8 . . ? C17 C16 C18 110.1(3) . . ? C18 C16 H16 107.8 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17B 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C8 C19 H19 107.9 . . ? C8 C19 C20 113.4(3) . . ? C8 C19 C21 109.3(3) . . ? C20 C19 H19 107.9 . . ? C21 C19 H19 107.9 . . ? C21 C19 C20 110.2(3) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20B 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21B 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 P1 116.4(3) . . ? C23 C22 C24 107.9(3) . . ? C24 C22 P1 107.0(2) . . ? C25 C22 P1 108.1(2) . . ? C25 C22 C23 108.8(3) . . ? C25 C22 C24 108.5(3) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24B 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25B 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C27 C26 P1 108.3(3) . . ? C27 C26 C28 108.8(3) . . ? C27 C26 C29 109.9(3) . . ? C28 C26 P1 104.9(2) . . ? C29 C26 P1 117.6(2) . . ? C29 C26 C28 107.0(3) . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27B 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C26 C29 H29A 109.5 . . ? C26 C29 H29B 109.5 . . ? C26 C29 H29C 109.5 . . ? H29A C29 H29B 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N1 C30 C31 178.8(4) . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31B 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? F1 C32 S1 111.9(3) . . ? F1 C32 F2 107.8(3) . . ? F1 C32 F3 107.3(3) . . ? F2 C32 S1 111.2(3) . . ? F2 C32 F3 107.0(3) . . ? F3 C32 S1 111.5(3) . . ? 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 P1 2.3864(8) . ? Ag1 O1 2.429(3) . ? Ag1 N1 2.233(3) . ? S1 O1 1.439(3) . ? S1 O2 1.436(3) . ? S1 O3 1.437(3) . ? S1 C32 1.825(4) . ? P1 C1 1.835(3) . ? P1 C22 1.906(3) . ? P1 C26 1.886(4) . ? F1 C32 1.328(5) . ? F2 C32 1.336(4) . ? F3 C32 1.342(5) . ? N1 C30 1.140(5) . ? C1 C2 1.400(4) . ? C1 C6 1.422(4) . ? C2 H2 0.9500 . ? C2 C3 1.386(4) . ? C3 H3 0.9500 . ? C3 C4 1.387(5) . ? C4 H4 0.9500 . ? C4 C5 1.385(4) . ? C5 H5 0.9500 . ? C5 C6 1.400(4) . ? C6 C7 1.507(4) . ? C7 C8 1.413(4) . ? C7 C12 1.411(4) . ? C8 C9 1.392(4) . ? C8 C19 1.522(4) . ? C9 H9 0.9500 . ? C9 C10 1.390(4) . ? C10 C11 1.391(4) . ? C10 C16 1.513(4) . ? C11 H11 0.9500 . ? C11 C12 1.395(4) . ? C12 C13 1.527(4) . ? C13 H13 1.0000 . ? C13 C14 1.532(4) . ? C13 C15 1.536(5) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16 1.0000 . ? C16 C17 1.525(5) . ? C16 C18 1.542(5) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19 1.0000 . ? C19 C20 1.538(5) . ? C19 C21 1.527(5) . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C23 1.534(5) . ? C22 C24 1.541(5) . ? C22 C25 1.521(5) . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 C27 1.538(5) . ? C26 C28 1.539(5) . ? C26 C29 1.538(5) . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 C31 1.448(5) . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ?