# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # ####################################################################### data_3 _database_code_depnum_ccdc_archive 'CCDC 917666' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C51 H42 Cu N4 P2, C2 H6 O, N O3, C2 H3 N' _chemical_formula_sum 'C55 H51 Cu N6 O4 P2' _chemical_formula_weight 985.50 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' 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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.9116(6) _cell_length_b 21.1567(9) _cell_length_c 16.8197(6) _cell_angle_alpha 90.00 _cell_angle_beta 110.7150(10) _cell_angle_gamma 90.00 _cell_volume 4963.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9956 _cell_measurement_theta_min 2.42 _cell_measurement_theta_max 24.15 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.319 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2056 _exptl_absorpt_coefficient_mu 0.557 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7681 _exptl_absorpt_correction_T_max 0.8079 _exptl_absorpt_process_details ; APEX2 Software Suite; Bruker 2005. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker-Nonius X8kappa APEX II CCD area detector ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 43638 _diffrn_reflns_av_R_equivalents 0.0372 _diffrn_reflns_av_sigmaI/netI 0.0317 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.25 _reflns_number_total 8913 _reflns_number_gt 6604 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker, 2007)' _computing_cell_refinement 'APEX2 Software Suite (Bruker, 2007)' _computing_data_reduction 'APEX2 Software Suite (Bruker, 2007)' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL and publCIF (Westrip, 2010)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1332P)^2^+4.8868P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8913 _refine_ls_number_parameters 643 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.0922 _refine_ls_R_factor_gt 0.0671 _refine_ls_wR_factor_ref 0.2188 _refine_ls_wR_factor_gt 0.2002 _refine_ls_goodness_of_fit_ref 1.088 _refine_ls_restrained_S_all 1.207 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.28953(4) 0.02785(3) 0.14774(3) 0.0355(2) Uani 1 1 d U . . P1 P 0.19458(8) 0.11114(6) 0.09170(7) 0.0387(3) Uani 1 1 d U . . P2 P 0.36388(8) 0.01115(6) 0.29061(7) 0.0363(3) Uani 1 1 d U . . N1 N 0.2769(3) -0.09469(18) 0.0540(2) 0.0385(7) Uani 1 1 d U . . N2 N 0.2346(3) -0.06142(17) 0.1013(2) 0.0380(8) Uani 1 1 d U . . N3 N 0.4137(3) -0.03326(18) 0.0605(2) 0.0399(8) Uani 1 1 d U . . N4 N 0.4109(3) 0.02048(18) 0.1061(3) 0.0412(8) Uani 1 1 d U . . C1 C 0.1936(3) -0.1033(2) 0.1346(3) 0.0393(9) Uani 1 1 d U . . H1 H 0.1589 -0.0931 0.1706 0.047 Uiso 1 1 calc R . . C2 C 0.2072(3) -0.1650(2) 0.1110(3) 0.0384(8) Uani 1 1 d U . . C3 C 0.1785(4) -0.2263(2) 0.1264(3) 0.0519(11) Uani 1 1 d U . . H3 H 0.1410 -0.2322 0.1611 0.062 Uiso 1 1 calc R . . C4 C 0.2062(4) -0.2757(3) 0.0903(4) 0.0597(12) Uani 1 1 d U . . H4 H 0.1878 -0.3172 0.1001 0.072 Uiso 1 1 calc R . . C5 C 0.2619(4) -0.2678(3) 0.0380(4) 0.0590(12) Uani 1 1 d U . . H5 H 0.2793 -0.3042 0.0136 0.071 Uiso 1 1 calc R . . C6 C 0.2916(4) -0.2097(2) 0.0216(3) 0.0505(10) Uani 1 1 d U . . H6 H 0.3294 -0.2044 -0.0131 0.061 Uiso 1 1 calc R . . C7 C 0.2625(3) -0.1583(2) 0.0594(3) 0.0389(8) Uani 1 1 d U . . C8 C 0.5013(3) 0.0341(2) 0.1509(3) 0.0444(9) Uani 1 1 d U . . H8 H 0.5208 0.0699 0.1870 0.053 Uiso 1 1 calc R . . C9 C 0.5649(4) -0.0104(3) 0.1388(3) 0.0485(10) Uani 1 1 d U . . C10 C 0.6651(4) -0.0201(3) 0.1729(4) 0.0633(12) Uani 1 1 d U . . H10 H 0.7067 0.0087 0.2123 0.076 Uiso 1 1 calc R . . C11 C 0.6991(5) -0.0730(4) 0.1464(4) 0.0754(14) Uani 1 1 d U . . H11 H 0.7661 -0.0808 0.1688 0.090 Uiso 1 1 calc R . . C12 C 0.6413(5) -0.1153(4) 0.0892(4) 0.0751(14) Uani 1 1 d U . . H12 H 0.6697 -0.1514 0.0741 0.090 Uiso 1 1 calc R . . C13 C 0.5424(4) -0.1071(3) 0.0523(4) 0.0614(12) Uani 1 1 d U . . H13 H 0.5025 -0.1355 0.0113 0.074 Uiso 1 1 calc R . . C14 C 0.5067(3) -0.0542(3) 0.0801(3) 0.0452(9) Uani 1 1 d U . . C15 C 0.3254(3) -0.0608(2) 0.0059(3) 0.0430(9) Uani 1 1 d U . . H15A H 0.3388 -0.0903 -0.0342 0.052 Uiso 1 1 calc R . . H15B H 0.2828 -0.0271 -0.0278 0.052 Uiso 1 1 calc R . . C16 C 0.1293(3) 0.1055(2) -0.0228(3) 0.0390(9) Uani 1 1 d U . . C17 C 0.1181(4) 0.1564(2) -0.0781(3) 0.0470(10) Uani 1 1 d U . . H17 H 0.1425 0.1969 -0.0567 0.056 Uiso 1 1 calc R . . C18 C 0.0705(4) 0.1474(3) -0.1651(3) 0.0504(11) Uani 1 1 d U . . H18 H 0.0641 0.1819 -0.2028 0.060 Uiso 1 1 calc R . . C19 C 0.0330(4) 0.0898(3) -0.1972(3) 0.0484(10) Uani 1 1 d U . . H19 H 0.0000 0.0846 -0.2565 0.058 Uiso 1 1 calc R . . C20 C 0.0434(4) 0.0397(2) -0.1430(3) 0.0468(10) Uani 1 1 d U . . H20 H 0.0177 -0.0004 -0.1649 0.056 Uiso 1 1 calc R . . C21 C 0.0913(3) 0.0471(2) -0.0563(3) 0.0429(10) Uani 1 1 d U . . H21 H 0.0982 0.0120 -0.0194 0.051 Uiso 1 1 calc R . . C22 C 0.1008(3) 0.1264(3) 0.1354(3) 0.0488(10) Uani 1 1 d U . . C23 C 0.1287(4) 0.1352(4) 0.2210(4) 0.0862(16) Uani 1 1 d U . . H23 H 0.1950 0.1342 0.2546 0.103 Uiso 1 1 calc R . . C24 C 0.0620(5) 0.1456(4) 0.2601(4) 0.0927(17) Uani 1 1 d U . . H24 H 0.0829 0.1517 0.3199 0.111 Uiso 1 1 calc R . . C25 C -0.0338(4) 0.1472(3) 0.2126(4) 0.0708(14) Uani 1 1 d U . . H25 H -0.0799 0.1547 0.2388 0.085 Uiso 1 1 calc R . . C26 C -0.0615(4) 0.1379(3) 0.1283(3) 0.0572(12) Uani 1 1 d U . . H26 H -0.1279 0.1383 0.0950 0.069 Uiso 1 1 calc R . . C27 C 0.0042(3) 0.1279(3) 0.0890(3) 0.0487(10) Uani 1 1 d U . . H27 H -0.0175 0.1219 0.0292 0.058 Uiso 1 1 calc R . . C28 C 0.2577(4) 0.1866(2) 0.1053(3) 0.0465(10) Uani 1 1 d U . . C29 C 0.3522(4) 0.1868(2) 0.1076(3) 0.0502(10) Uani 1 1 d U . . H29 H 0.3815 0.1482 0.1016 0.060 Uiso 1 1 calc R . . C30 C 0.4037(5) 0.2424(3) 0.1184(4) 0.0627(12) Uani 1 1 d U . . H30 H 0.4680 0.2417 0.1198 0.075 Uiso 1 1 calc R . . C31 C 0.3624(5) 0.2981(3) 0.1271(4) 0.0691(14) Uani 1 1 d U . . H31 H 0.3978 0.3363 0.1340 0.083 Uiso 1 1 calc R . . C32 C 0.2688(5) 0.2993(3) 0.1261(5) 0.0767(15) Uani 1 1 d U . . H32 H 0.2404 0.3383 0.1324 0.092 Uiso 1 1 calc R . . C33 C 0.2167(4) 0.2433(3) 0.1157(4) 0.0651(13) Uani 1 1 d U . . H33 H 0.1530 0.2440 0.1157 0.078 Uiso 1 1 calc R . . C34 C 0.2952(4) 0.0220(3) 0.3606(3) 0.0532(11) Uani 1 1 d U . . C35 C 0.3307(4) 0.0542(2) 0.4371(3) 0.0469(10) Uani 1 1 d U . . H35 H 0.3937 0.0713 0.4552 0.056 Uiso 1 1 calc R . . C36 C 0.2757(4) 0.0617(3) 0.4871(3) 0.0563(11) Uani 1 1 d U . . H36 H 0.3013 0.0834 0.5398 0.068 Uiso 1 1 calc R . . C37 C 0.1854(5) 0.0385(4) 0.4618(5) 0.0776(14) Uani 1 1 d U . . H37 H 0.1468 0.0453 0.4955 0.093 Uiso 1 1 calc R . . C38 C 0.1501(6) 0.0052(5) 0.3873(5) 0.0945(16) Uani 1 1 d U . . H38 H 0.0882 -0.0134 0.3707 0.113 Uiso 1 1 calc R . . C39 C 0.2047(5) -0.0014(4) 0.3363(5) 0.0850(15) Uani 1 1 d U . . H39 H 0.1784 -0.0227 0.2833 0.102 Uiso 1 1 calc R . . C40 C 0.4176(3) -0.0669(2) 0.3222(3) 0.0399(9) Uani 1 1 d U . . C41 C 0.4475(4) -0.1011(2) 0.2650(3) 0.0477(10) Uani 1 1 d U . . H41 H 0.4354 -0.0847 0.2096 0.057 Uiso 1 1 calc R . . C42 C 0.4940(4) -0.1581(3) 0.2875(4) 0.0565(12) Uani 1 1 d U . . H42 H 0.5158 -0.1801 0.2485 0.068 Uiso 1 1 calc R . . C43 C 0.5092(4) -0.1832(3) 0.3676(4) 0.0593(12) Uani 1 1 d U . . H43 H 0.5408 -0.2227 0.3836 0.071 Uiso 1 1 calc R . . C44 C 0.4781(4) -0.1508(2) 0.4232(3) 0.0563(12) Uani 1 1 d U . . H44 H 0.4880 -0.1681 0.4777 0.068 Uiso 1 1 calc R . . C45 C 0.4326(4) -0.0933(2) 0.4015(3) 0.0484(10) Uani 1 1 d U . . H45 H 0.4114 -0.0715 0.4411 0.058 Uiso 1 1 calc R . . C46 C 0.4654(3) 0.0648(2) 0.3329(3) 0.0399(9) Uani 1 1 d U . . C47 C 0.4493(4) 0.1289(2) 0.3159(3) 0.0467(10) Uani 1 1 d U . . H47 H 0.3858 0.1438 0.2881 0.056 Uiso 1 1 calc R . . C48 C 0.5253(4) 0.1714(3) 0.3391(4) 0.0553(12) Uani 1 1 d U . . H48 H 0.5133 0.2151 0.3270 0.066 Uiso 1 1 calc R . . C49 C 0.6172(4) 0.1507(3) 0.3791(4) 0.0591(12) Uani 1 1 d U . . H49 H 0.6689 0.1799 0.3948 0.071 Uiso 1 1 calc R . . C50 C 0.6344(4) 0.0872(3) 0.3965(4) 0.0577(12) Uani 1 1 d U . . H50 H 0.6982 0.0728 0.4244 0.069 Uiso 1 1 calc R . . C51 C 0.5591(4) 0.0440(2) 0.3736(3) 0.0479(11) Uani 1 1 d U . . H51 H 0.5716 0.0004 0.3858 0.058 Uiso 1 1 calc R . . O1 O 0.7183(7) 0.1280(5) 0.1871(6) 0.163(3) Uani 1 1 d U . . O2 O 0.6162(7) 0.1865(6) 0.1262(6) 0.180(3) Uani 1 1 d U . . O3 O 0.7218(9) 0.2174(5) 0.2410(7) 0.201(4) Uani 1 1 d U . . N5 N 0.6854(11) 0.1763(8) 0.1843(9) 0.153(3) Uani 1 1 d U . . O4A O 0.8382(11) 0.1429(9) 0.3545(10) 0.156(5) Uani 0.50 1 d PDU A 1 H4A H 0.7787 0.1277 0.3267 0.187 Uiso 0.50 1 d PR A 1 C52A C 0.8812(13) 0.1936(12) 0.4045(14) 0.145(5) Uani 0.50 1 d PDU A 1 H52A H 0.8583 0.2319 0.3693 0.174 Uiso 0.50 1 calc PR A 1 H52B H 0.8548 0.1956 0.4508 0.174 Uiso 0.50 1 calc PR A 1 C53A C 0.9742(11) 0.1993(11) 0.4404(11) 0.123(5) Uani 0.50 1 d PDU A 1 H53A H 0.9955 0.1791 0.4964 0.185 Uiso 0.50 1 calc PR A 1 H53B H 0.9913 0.2442 0.4468 0.185 Uiso 0.50 1 calc PR A 1 H53C H 1.0055 0.1789 0.4047 0.185 Uiso 0.50 1 calc PR A 1 O4B O 0.8658(13) 0.0566(9) 0.3422(10) 0.169(5) Uani 0.50 1 d PDU B 2 H4B H 0.8692 0.0210 0.3205 0.203 Uiso 0.50 1 d PR B 2 C52B C 0.9284(18) 0.0517(11) 0.4281(14) 0.162(6) Uani 0.50 1 d PDU B 2 H52C H 0.9945 0.0413 0.4320 0.194 Uiso 0.50 1 calc PR B 2 H52D H 0.9058 0.0193 0.4592 0.194 Uiso 0.50 1 calc PR B 2 C53B C 0.923(2) 0.1201(12) 0.4631(15) 0.172(7) Uani 0.50 1 d PDU B 2 H53D H 0.9550 0.1501 0.4380 0.258 Uiso 0.50 1 calc PR B 2 H53E H 0.9538 0.1203 0.5251 0.258 Uiso 0.50 1 calc PR B 2 H53F H 0.8552 0.1324 0.4480 0.258 Uiso 0.50 1 calc PR B 2 N6 N 0.0518(7) 0.0680(5) 0.6078(6) 0.151(3) Uani 1 1 d DU . . C54 C 0.1055(10) 0.1226(7) 0.6167(9) 0.171(3) Uani 1 1 d DU . . C55 C 0.2023(9) 0.1583(6) 0.6552(8) 0.153(3) Uani 1 1 d DU . . H55A H 0.1939 0.1949 0.6876 0.229 Uiso 1 1 calc R . . H55B H 0.2234 0.1727 0.6093 0.229 Uiso 1 1 calc R . . H55C H 0.2506 0.1299 0.6929 0.229 Uiso 1 1 calc R . . 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 Cu1 0.0300(3) 0.0341(3) 0.0372(3) -0.0006(2) 0.0055(2) 0.0032(2) P1 0.0326(6) 0.0359(6) 0.0389(6) -0.0033(5) 0.0021(5) 0.0077(5) P2 0.0326(6) 0.0372(6) 0.0347(6) -0.0008(5) 0.0063(5) -0.0041(5) N1 0.0395(17) 0.0364(16) 0.0400(17) -0.0038(14) 0.0145(14) -0.0032(14) N2 0.0370(18) 0.0341(16) 0.0419(18) -0.0042(14) 0.0127(14) -0.0026(14) N3 0.0384(16) 0.0413(18) 0.0441(18) 0.0034(14) 0.0196(14) -0.0014(14) N4 0.0375(17) 0.0385(19) 0.0475(19) 0.0034(15) 0.0148(15) -0.0023(14) C1 0.035(2) 0.0394(19) 0.044(2) -0.0024(17) 0.0139(16) -0.0046(17) C2 0.0338(19) 0.0378(18) 0.0401(19) -0.0002(16) 0.0089(15) -0.0056(16) C3 0.056(3) 0.043(2) 0.056(2) 0.0015(19) 0.019(2) -0.012(2) C4 0.070(3) 0.039(2) 0.065(3) -0.001(2) 0.017(2) -0.011(2) C5 0.065(3) 0.041(2) 0.067(3) -0.010(2) 0.018(2) -0.002(2) C6 0.052(2) 0.043(2) 0.056(2) -0.0100(19) 0.0176(19) -0.0028(19) C7 0.0371(19) 0.0361(17) 0.0398(19) -0.0036(15) 0.0089(15) -0.0039(16) C8 0.0382(19) 0.048(2) 0.048(2) 0.0057(17) 0.0167(17) -0.0068(17) C9 0.0383(18) 0.063(2) 0.049(2) 0.0139(18) 0.0218(17) 0.0015(17) C10 0.042(2) 0.091(3) 0.062(3) 0.015(2) 0.025(2) 0.005(2) C11 0.048(3) 0.105(4) 0.079(3) 0.016(3) 0.031(2) 0.023(2) C12 0.062(3) 0.096(3) 0.081(3) 0.009(3) 0.041(2) 0.026(2) C13 0.060(2) 0.073(3) 0.064(3) 0.007(2) 0.037(2) 0.014(2) C14 0.0420(18) 0.055(2) 0.047(2) 0.0126(17) 0.0268(16) 0.0052(17) C15 0.045(2) 0.043(2) 0.042(2) 0.0002(17) 0.0164(16) -0.0037(18) C16 0.033(2) 0.037(2) 0.0412(18) -0.0025(15) 0.0049(16) 0.0107(16) C17 0.049(2) 0.038(2) 0.047(2) 0.0019(17) 0.0086(19) 0.0122(19) C18 0.051(2) 0.048(2) 0.047(2) 0.0053(19) 0.0112(19) 0.015(2) C19 0.043(2) 0.053(2) 0.043(2) -0.0012(17) 0.0067(18) 0.0115(19) C20 0.039(2) 0.046(2) 0.046(2) -0.0061(17) 0.0034(18) 0.0030(19) C21 0.035(2) 0.042(2) 0.042(2) -0.0016(17) 0.0025(17) 0.0020(18) C22 0.0340(19) 0.059(3) 0.045(2) -0.010(2) 0.0036(17) 0.0117(18) C23 0.044(2) 0.150(4) 0.052(2) -0.026(3) 0.0027(19) 0.028(3) C24 0.059(3) 0.156(4) 0.055(3) -0.025(3) 0.010(2) 0.027(3) C25 0.046(2) 0.105(4) 0.059(2) -0.011(3) 0.016(2) 0.018(3) C26 0.036(2) 0.074(3) 0.057(2) -0.007(2) 0.0092(19) 0.003(2) C27 0.0348(19) 0.059(3) 0.045(2) -0.006(2) 0.0054(17) 0.001(2) C28 0.043(2) 0.0389(19) 0.048(2) -0.0030(18) 0.0044(18) 0.0052(17) C29 0.052(2) 0.040(2) 0.059(2) 0.004(2) 0.020(2) 0.0039(18) C30 0.060(3) 0.049(2) 0.077(3) 0.005(2) 0.021(2) -0.003(2) C31 0.066(3) 0.044(2) 0.082(3) -0.006(2) 0.008(3) -0.006(2) C32 0.065(3) 0.045(2) 0.099(3) -0.019(3) 0.002(3) 0.004(2) C33 0.047(2) 0.046(2) 0.085(3) -0.018(2) 0.003(2) 0.0042(19) C34 0.054(2) 0.058(3) 0.052(2) -0.014(2) 0.025(2) -0.014(2) C35 0.057(2) 0.040(2) 0.042(2) -0.0010(18) 0.0150(18) 0.004(2) C36 0.072(3) 0.050(3) 0.049(2) -0.005(2) 0.024(2) 0.008(2) C37 0.084(3) 0.088(3) 0.078(3) -0.021(3) 0.049(3) -0.012(3) C38 0.079(3) 0.125(4) 0.096(3) -0.044(3) 0.052(3) -0.036(3) C39 0.069(3) 0.115(4) 0.082(3) -0.048(3) 0.041(2) -0.036(3) C40 0.039(2) 0.0346(19) 0.040(2) 0.0013(15) 0.0074(17) -0.0073(16) C41 0.051(2) 0.043(2) 0.046(2) 0.0052(18) 0.0137(19) 0.0011(19) C42 0.058(3) 0.045(2) 0.061(2) 0.005(2) 0.015(2) 0.009(2) C43 0.061(3) 0.041(2) 0.062(3) 0.0097(19) 0.004(2) 0.000(2) C44 0.068(3) 0.041(2) 0.047(2) 0.0077(18) 0.004(2) -0.014(2) C45 0.056(2) 0.040(2) 0.041(2) 0.0010(17) 0.0074(19) -0.0130(19) C46 0.0392(19) 0.0368(19) 0.038(2) 0.0028(17) 0.0071(16) -0.0058(16) C47 0.047(2) 0.036(2) 0.051(2) 0.0031(18) 0.0096(19) -0.0007(17) C48 0.059(2) 0.036(2) 0.066(3) 0.003(2) 0.015(2) -0.0077(18) C49 0.052(2) 0.049(2) 0.068(3) 0.001(2) 0.012(2) -0.017(2) C50 0.043(2) 0.052(2) 0.067(3) 0.006(2) 0.004(2) -0.0100(19) C51 0.040(2) 0.042(2) 0.052(2) 0.0092(19) 0.0040(19) -0.0061(17) O1 0.151(6) 0.183(6) 0.146(6) -0.020(5) 0.041(5) -0.034(5) O2 0.135(5) 0.296(9) 0.146(6) 0.011(6) 0.095(4) 0.029(5) O3 0.271(8) 0.169(6) 0.176(7) -0.015(5) 0.094(6) -0.076(6) N5 0.157(5) 0.181(5) 0.135(5) -0.003(4) 0.070(4) -0.024(4) O4A 0.126(8) 0.203(11) 0.145(9) -0.060(8) 0.055(7) -0.033(8) C52A 0.120(8) 0.196(10) 0.136(9) -0.066(8) 0.065(8) -0.020(8) C53A 0.110(8) 0.182(11) 0.117(9) -0.063(8) 0.087(7) -0.034(8) O4B 0.152(10) 0.183(11) 0.159(9) 0.024(8) 0.037(8) -0.048(9) C52B 0.152(10) 0.187(11) 0.147(10) 0.005(9) 0.055(8) -0.043(10) C53B 0.168(12) 0.191(12) 0.164(11) 0.006(9) 0.069(10) -0.027(11) N6 0.152(5) 0.198(5) 0.140(5) 0.002(4) 0.097(4) -0.027(4) C54 0.170(4) 0.184(5) 0.166(4) 0.000(4) 0.067(4) -0.022(3) C55 0.159(4) 0.164(5) 0.149(4) 0.007(4) 0.072(4) -0.015(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Cu1 N2 2.096(4) . ? Cu1 N4 2.165(4) . ? Cu1 P1 2.2481(12) . ? Cu1 P2 2.2899(12) . ? P1 C22 1.825(5) . ? P1 C28 1.826(5) . ? P1 C16 1.828(5) . ? P2 C46 1.824(5) . ? P2 C34 1.827(5) . ? P2 C40 1.829(5) . ? N1 C7 1.370(6) . ? N1 N2 1.372(5) . ? N1 C15 1.450(6) . ? N2 C1 1.309(6) . ? N3 C14 1.380(6) . ? N3 N4 1.381(5) . ? N3 C15 1.437(6) . ? N4 C8 1.322(6) . ? C1 C2 1.400(6) . ? C1 H1 0.9500 . ? C2 C7 1.400(6) . ? C2 C3 1.416(7) . ? C3 C4 1.346(8) . ? C3 H3 0.9500 . ? C4 C5 1.417(8) . ? C4 H4 0.9500 . ? C5 C6 1.369(8) . ? C5 H5 0.9500 . ? C6 C7 1.404(7) . ? C6 H6 0.9500 . ? C8 C9 1.402(7) . ? C8 H8 0.9500 . ? C9 C14 1.408(8) . ? C9 C10 1.414(8) . ? C10 C11 1.366(9) . ? C10 H10 0.9500 . ? C11 C12 1.372(10) . ? C11 H11 0.9500 . ? C12 C13 1.394(9) . ? C12 H12 0.9500 . ? C13 C14 1.388(8) . ? C13 H13 0.9500 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C21 1.392(7) . ? C16 C17 1.394(7) . ? C17 C18 1.396(7) . ? C17 H17 0.9500 . ? C18 C19 1.370(8) . ? C18 H18 0.9500 . ? C19 C20 1.371(7) . ? C19 H19 0.9500 . ? C20 C21 1.386(7) . ? C20 H20 0.9500 . ? C21 H21 0.9500 . ? C22 C23 1.362(8) . ? C22 C27 1.374(7) . ? C23 C24 1.391(9) . ? C23 H23 0.9500 . ? C24 C25 1.368(9) . ? C24 H24 0.9500 . ? C25 C26 1.343(8) . ? C25 H25 0.9500 . ? C26 C27 1.379(7) . ? C26 H26 0.9500 . ? C27 H27 0.9500 . ? C28 C33 1.385(7) . ? C28 C29 1.396(7) . ? C29 C30 1.380(8) . ? C29 H29 0.9500 . ? C30 C31 1.362(9) . ? C30 H30 0.9500 . ? C31 C32 1.390(9) . ? C31 H31 0.9500 . ? C32 C33 1.394(9) . ? C32 H32 0.9500 . ? C33 H33 0.9500 . ? C34 C39 1.358(8) . ? C34 C35 1.386(7) . ? C35 C36 1.377(7) . ? C35 H35 0.9500 . ? C36 C37 1.352(9) . ? C36 H36 0.9500 . ? C37 C38 1.371(10) . ? C37 H37 0.9500 . ? C38 C39 1.384(9) . ? C38 H38 0.9500 . ? C39 H39 0.9500 . ? C40 C45 1.389(7) . ? C40 C41 1.396(7) . ? C41 C42 1.377(7) . ? C41 H41 0.9500 . ? C42 C43 1.392(8) . ? C42 H42 0.9500 . ? C43 C44 1.366(8) . ? C43 H43 0.9500 . ? C44 C45 1.378(7) . ? C44 H44 0.9500 . ? C45 H45 0.9500 . ? C46 C47 1.389(7) . ? C46 C51 1.392(7) . ? C47 C48 1.389(7) . ? C47 H47 0.9500 . ? C48 C49 1.368(8) . ? C48 H48 0.9500 . ? C49 C50 1.379(8) . ? C49 H49 0.9500 . ? C50 C51 1.392(7) . ? C50 H50 0.9500 . ? C51 H51 0.9500 . ? O1 N5 1.128(15) . ? O2 N5 1.163(14) . ? O3 N5 1.262(15) . ? O4A C52A 1.373(17) . ? O4A H4A 0.9031 . ? C52A C53A 1.308(17) . ? C52A H52A 0.9900 . ? C52A H52B 0.9900 . ? C53A H53A 0.9800 . ? C53A H53B 0.9800 . ? C53A H53C 0.9800 . ? O4B C52B 1.419(18) . ? O4B H4B 0.8455 . ? C52B C53B 1.577(19) . ? C52B H52C 0.9900 . ? C52B H52D 0.9900 . ? C53B H53D 0.9800 . ? C53B H53E 0.9800 . ? C53B H53F 0.9800 . ? N6 C54 1.383(13) . ? C54 C55 1.553(14) . ? C55 H55A 0.9800 . ? C55 H55B 0.9800 . ? C55 H55C 0.9800 . ? 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 Cu1 N4 94.35(14) . . ? N2 Cu1 P1 116.42(11) . . ? N4 Cu1 P1 113.30(11) . . ? N2 Cu1 P2 103.41(11) . . ? N4 Cu1 P2 100.27(11) . . ? P1 Cu1 P2 124.08(5) . . ? C22 P1 C28 103.2(2) . . ? C22 P1 C16 103.8(2) . . ? C28 P1 C16 104.4(2) . . ? C22 P1 Cu1 115.39(18) . . ? C28 P1 Cu1 114.34(16) . . ? C16 P1 Cu1 114.32(15) . . ? C46 P2 C34 104.3(2) . . ? C46 P2 C40 103.3(2) . . ? C34 P2 C40 102.4(2) . . ? C46 P2 Cu1 109.88(15) . . ? C34 P2 Cu1 118.9(2) . . ? C40 P2 Cu1 116.35(15) . . ? C7 N1 N2 110.5(4) . . ? C7 N1 C15 130.0(4) . . ? N2 N1 C15 119.5(4) . . ? C1 N2 N1 106.3(4) . . ? C1 N2 Cu1 129.1(3) . . ? N1 N2 Cu1 118.6(3) . . ? C14 N3 N4 111.0(4) . . ? C14 N3 C15 129.7(4) . . ? N4 N3 C15 119.2(4) . . ? C8 N4 N3 105.7(4) . . ? C8 N4 Cu1 126.9(3) . . ? N3 N4 Cu1 115.6(3) . . ? N2 C1 C2 111.9(4) . . ? N2 C1 H1 124.0 . . ? C2 C1 H1 124.0 . . ? C7 C2 C1 104.9(4) . . ? C7 C2 C3 119.2(4) . . ? C1 C2 C3 135.9(5) . . ? C4 C3 C2 118.0(5) . . ? C4 C3 H3 121.0 . . ? C2 C3 H3 121.0 . . ? C3 C4 C5 121.9(5) . . ? C3 C4 H4 119.1 . . ? C5 C4 H4 119.1 . . ? C6 C5 C4 122.3(5) . . ? C6 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? C5 C6 C7 115.5(5) . . ? C5 C6 H6 122.3 . . ? C7 C6 H6 122.3 . . ? N1 C7 C2 106.3(4) . . ? N1 C7 C6 130.5(4) . . ? C2 C7 C6 123.1(4) . . ? N4 C8 C9 112.1(5) . . ? N4 C8 H8 123.9 . . ? C9 C8 H8 123.9 . . ? C8 C9 C14 105.2(4) . . ? C8 C9 C10 135.3(6) . . ? C14 C9 C10 119.4(5) . . ? C11 C10 C9 116.5(6) . . ? C11 C10 H10 121.8 . . ? C9 C10 H10 121.8 . . ? C10 C11 C12 123.4(6) . . ? C10 C11 H11 118.3 . . ? C12 C11 H11 118.3 . . ? C11 C12 C13 122.2(6) . . ? C11 C12 H12 118.9 . . ? C13 C12 H12 118.9 . . ? C14 C13 C12 115.0(6) . . ? C14 C13 H13 122.5 . . ? C12 C13 H13 122.5 . . ? N3 C14 C13 130.7(5) . . ? N3 C14 C9 105.9(4) . . ? C13 C14 C9 123.4(5) . . ? N3 C15 N1 111.7(4) . . ? N3 C15 H15A 109.3 . . ? N1 C15 H15A 109.3 . . ? N3 C15 H15B 109.3 . . ? N1 C15 H15B 109.3 . . ? H15A C15 H15B 107.9 . . ? C21 C16 C17 118.6(4) . . ? C21 C16 P1 118.3(4) . . ? C17 C16 P1 123.0(4) . . ? C16 C17 C18 119.4(5) . . ? C16 C17 H17 120.3 . . ? C18 C17 H17 120.3 . . ? C19 C18 C17 121.3(5) . . ? C19 C18 H18 119.3 . . ? C17 C18 H18 119.3 . . ? C18 C19 C20 119.4(5) . . ? C18 C19 H19 120.3 . . ? C20 C19 H19 120.3 . . ? C19 C20 C21 120.4(5) . . ? C19 C20 H20 119.8 . . ? C21 C20 H20 119.8 . . ? C20 C21 C16 120.8(5) . . ? C20 C21 H21 119.6 . . ? C16 C21 H21 119.6 . . ? C23 C22 C27 117.7(5) . . ? C23 C22 P1 117.3(4) . . ? C27 C22 P1 125.0(4) . . ? C22 C23 C24 121.3(6) . . ? C22 C23 H23 119.4 . . ? C24 C23 H23 119.4 . . ? C25 C24 C23 120.1(6) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C26 C25 C24 118.6(6) . . ? C26 C25 H25 120.7 . . ? C24 C25 H25 120.7 . . ? C25 C26 C27 121.6(5) . . ? C25 C26 H26 119.2 . . ? C27 C26 H26 119.2 . . ? C22 C27 C26 120.7(5) . . ? C22 C27 H27 119.7 . . ? C26 C27 H27 119.7 . . ? C33 C28 C29 118.7(5) . . ? C33 C28 P1 122.8(4) . . ? C29 C28 P1 118.5(4) . . ? C30 C29 C28 121.1(5) . . ? C30 C29 H29 119.5 . . ? C28 C29 H29 119.5 . . ? C31 C30 C29 119.9(6) . . ? C31 C30 H30 120.0 . . ? C29 C30 H30 120.0 . . ? C30 C31 C32 120.4(6) . . ? C30 C31 H31 119.8 . . ? C32 C31 H31 119.8 . . ? C31 C32 C33 119.9(6) . . ? C31 C32 H32 120.0 . . ? C33 C32 H32 120.0 . . ? C28 C33 C32 120.0(6) . . ? C28 C33 H33 120.0 . . ? C32 C33 H33 120.0 . . ? C39 C34 C35 118.1(5) . . ? C39 C34 P2 118.9(4) . . ? C35 C34 P2 122.9(4) . . ? C36 C35 C34 120.7(5) . . ? C36 C35 H35 119.7 . . ? C34 C35 H35 119.7 . . ? C37 C36 C35 120.6(5) . . ? C37 C36 H36 119.7 . . ? C35 C36 H36 119.7 . . ? C36 C37 C38 119.5(6) . . ? C36 C37 H37 120.3 . . ? C38 C37 H37 120.3 . . ? C37 C38 C39 120.0(7) . . ? C37 C38 H38 120.0 . . ? C39 C38 H38 120.0 . . ? C34 C39 C38 121.1(6) . . ? C34 C39 H39 119.4 . . ? C38 C39 H39 119.4 . . ? C45 C40 C41 118.1(5) . . ? C45 C40 P2 123.1(4) . . ? C41 C40 P2 118.7(3) . . ? C42 C41 C40 121.2(5) . . ? C42 C41 H41 119.4 . . ? C40 C41 H41 119.4 . . ? C41 C42 C43 119.6(5) . . ? C41 C42 H42 120.2 . . ? C43 C42 H42 120.2 . . ? C44 C43 C42 119.5(5) . . ? C44 C43 H43 120.3 . . ? C42 C43 H43 120.3 . . ? C43 C44 C45 121.2(5) . . ? C43 C44 H44 119.4 . . ? C45 C44 H44 119.4 . . ? C44 C45 C40 120.4(5) . . ? C44 C45 H45 119.8 . . ? C40 C45 H45 119.8 . . ? C47 C46 C51 118.7(4) . . ? C47 C46 P2 117.9(4) . . ? C51 C46 P2 123.0(4) . . ? C46 C47 C48 120.6(5) . . ? C46 C47 H47 119.7 . . ? C48 C47 H47 119.7 . . ? C49 C48 C47 120.4(5) . . ? C49 C48 H48 119.8 . . ? C47 C48 H48 119.8 . . ? C48 C49 C50 119.8(5) . . ? C48 C49 H49 120.1 . . ? C50 C49 H49 120.1 . . ? C49 C50 C51 120.6(5) . . ? C49 C50 H50 119.7 . . ? C51 C50 H50 119.7 . . ? C46 C51 C50 120.0(5) . . ? C46 C51 H51 120.0 . . ? C50 C51 H51 120.0 . . ? O1 N5 O2 116.5(17) . . ? O1 N5 O3 121.9(17) . . ? O2 N5 O3 121.6(18) . . ? C52A O4A H4A 139.1 . . ? C53A C52A O4A 123.0(18) . . ? C53A C52A H52A 106.6 . . ? O4A C52A H52A 106.6 . . ? C53A C52A H52B 106.6 . . ? O4A C52A H52B 106.6 . . ? H52A C52A H52B 106.5 . . ? C52B O4B H4B 104.9 . . ? O4B C52B C53B 102.1(16) . . ? O4B C52B H52C 111.4 . . ? C53B C52B H52C 111.4 . . ? O4B C52B H52D 111.4 . . ? C53B C52B H52D 111.4 . . ? H52C C52B H52D 109.2 . . ? C52B C53B H53D 109.5 . . ? C52B C53B H53E 109.5 . . ? H53D C53B H53E 109.5 . . ? C52B C53B H53F 109.5 . . ? H53D C53B H53F 109.5 . . ? H53E C53B H53F 109.5 . . ? N6 C54 C55 150.2(14) . . ? C54 C55 H55A 109.5 . . ? C54 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C54 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? 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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N2 Cu1 P1 C22 80.4(2) . . . . ? N4 Cu1 P1 C22 -171.8(2) . . . . ? P2 Cu1 P1 C22 -50.07(19) . . . . ? N2 Cu1 P1 C28 -160.1(2) . . . . ? N4 Cu1 P1 C28 -52.2(2) . . . . ? P2 Cu1 P1 C28 69.5(2) . . . . ? N2 Cu1 P1 C16 -39.8(2) . . . . ? N4 Cu1 P1 C16 68.0(2) . . . . ? P2 Cu1 P1 C16 -170.29(17) . . . . ? N2 Cu1 P2 C46 149.5(2) . . . . ? N4 Cu1 P2 C46 52.5(2) . . . . ? P1 Cu1 P2 C46 -74.95(18) . . . . ? N2 Cu1 P2 C34 -90.5(2) . . . . ? N4 Cu1 P2 C34 172.5(2) . . . . ? P1 Cu1 P2 C34 45.0(2) . . . . ? N2 Cu1 P2 C40 32.6(2) . . . . ? N4 Cu1 P2 C40 -64.4(2) . . . . ? P1 Cu1 P2 C40 168.12(17) . . . . ? C7 N1 N2 C1 -0.8(5) . . . . ? C15 N1 N2 C1 177.5(4) . . . . ? C7 N1 N2 Cu1 154.4(3) . . . . ? C15 N1 N2 Cu1 -27.2(5) . . . . ? N4 Cu1 N2 C1 142.2(4) . . . . ? P1 Cu1 N2 C1 -99.1(4) . . . . ? P2 Cu1 N2 C1 40.6(4) . . . . ? N4 Cu1 N2 N1 -6.6(3) . . . . ? P1 Cu1 N2 N1 112.1(3) . . . . ? P2 Cu1 N2 N1 -108.3(3) . . . . ? C14 N3 N4 C8 2.4(5) . . . . ? C15 N3 N4 C8 179.0(4) . . . . ? C14 N3 N4 Cu1 -143.3(3) . . . . ? C15 N3 N4 Cu1 33.3(5) . . . . ? N2 Cu1 N4 C8 -133.4(4) . . . . ? P1 Cu1 N4 C8 105.3(4) . . . . ? P2 Cu1 N4 C8 -28.9(4) . . . . ? N2 Cu1 N4 N3 3.9(3) . . . . ? P1 Cu1 N4 N3 -117.3(3) . . . . ? P2 Cu1 N4 N3 108.4(3) . . . . ? N1 N2 C1 C2 0.1(5) . . . . ? Cu1 N2 C1 C2 -151.7(3) . . . . ? N2 C1 C2 C7 0.6(5) . . . . ? N2 C1 C2 C3 -178.6(5) . . . . ? C7 C2 C3 C4 0.0(7) . . . . ? C1 C2 C3 C4 179.2(5) . . . . ? C2 C3 C4 C5 -0.2(8) . . . . ? C3 C4 C5 C6 0.5(9) . . . . ? C4 C5 C6 C7 -0.5(8) . . . . ? N2 N1 C7 C2 1.2(5) . . . . ? C15 N1 C7 C2 -176.9(4) . . . . ? N2 N1 C7 C6 179.4(5) . . . . ? C15 N1 C7 C6 1.3(8) . . . . ? C1 C2 C7 N1 -1.1(5) . . . . ? C3 C2 C7 N1 178.3(4) . . . . ? C1 C2 C7 C6 -179.5(4) . . . . ? C3 C2 C7 C6 -0.1(7) . . . . ? C5 C6 C7 N1 -177.7(5) . . . . ? C5 C6 C7 C2 0.3(7) . . . . ? N3 N4 C8 C9 -2.1(5) . . . . ? Cu1 N4 C8 C9 138.5(4) . . . . ? N4 C8 C9 C14 1.0(6) . . . . ? N4 C8 C9 C10 -176.4(6) . . . . ? C8 C9 C10 C11 176.5(6) . . . . ? C14 C9 C10 C11 -0.7(8) . . . . ? C9 C10 C11 C12 0.6(10) . . . . ? C10 C11 C12 C13 0.8(11) . . . . ? C11 C12 C13 C14 -2.1(9) . . . . ? N4 N3 C14 C13 177.3(5) . . . . ? C15 N3 C14 C13 1.1(8) . . . . ? N4 N3 C14 C9 -1.8(5) . . . . ? C15 N3 C14 C9 -178.0(4) . . . . ? C12 C13 C14 N3 -176.9(5) . . . . ? C12 C13 C14 C9 2.1(8) . . . . ? C8 C9 C14 N3 0.5(5) . . . . ? C10 C9 C14 N3 178.4(4) . . . . ? C8 C9 C14 C13 -178.6(5) . . . . ? C10 C9 C14 C13 -0.7(8) . . . . ? C14 N3 C15 N1 100.4(5) . . . . ? N4 N3 C15 N1 -75.5(5) . . . . ? C7 N1 C15 N3 -110.4(5) . . . . ? N2 N1 C15 N3 71.6(5) . . . . ? C22 P1 C16 C21 -86.5(4) . . . . ? C28 P1 C16 C21 165.7(4) . . . . ? Cu1 P1 C16 C21 40.0(4) . . . . ? C22 P1 C16 C17 95.2(4) . . . . ? C28 P1 C16 C17 -12.6(5) . . . . ? Cu1 P1 C16 C17 -138.3(4) . . . . ? C21 C16 C17 C18 -0.9(7) . . . . ? P1 C16 C17 C18 177.4(4) . . . . ? C16 C17 C18 C19 1.3(8) . . . . ? C17 C18 C19 C20 -1.0(8) . . . . ? C18 C19 C20 C21 0.2(8) . . . . ? C19 C20 C21 C16 0.1(8) . . . . ? C17 C16 C21 C20 0.2(7) . . . . ? P1 C16 C21 C20 -178.2(4) . . . . ? C28 P1 C22 C23 -69.1(6) . . . . ? C16 P1 C22 C23 -177.8(6) . . . . ? Cu1 P1 C22 C23 56.4(6) . . . . ? C28 P1 C22 C27 112.9(5) . . . . ? C16 P1 C22 C27 4.3(6) . . . . ? Cu1 P1 C22 C27 -121.6(5) . . . . ? C27 C22 C23 C24 -0.3(12) . . . . ? P1 C22 C23 C24 -178.5(7) . . . . ? C22 C23 C24 C25 0.0(14) . . . . ? C23 C24 C25 C26 0.6(13) . . . . ? C24 C25 C26 C27 -0.9(11) . . . . ? C23 C22 C27 C26 0.0(9) . . . . ? P1 C22 C27 C26 178.0(5) . . . . ? C25 C26 C27 C22 0.6(10) . . . . ? C22 P1 C28 C33 -21.0(5) . . . . ? C16 P1 C28 C33 87.2(5) . . . . ? Cu1 P1 C28 C33 -147.1(4) . . . . ? C22 P1 C28 C29 157.3(4) . . . . ? C16 P1 C28 C29 -94.5(4) . . . . ? Cu1 P1 C28 C29 31.2(5) . . . . ? C33 C28 C29 C30 -1.1(8) . . . . ? P1 C28 C29 C30 -179.5(4) . . . . ? C28 C29 C30 C31 0.0(9) . . . . ? C29 C30 C31 C32 0.7(10) . . . . ? C30 C31 C32 C33 -0.3(11) . . . . ? C29 C28 C33 C32 1.5(9) . . . . ? P1 C28 C33 C32 179.8(5) . . . . ? C31 C32 C33 C28 -0.8(10) . . . . ? C46 P2 C34 C39 166.5(6) . . . . ? C40 P2 C34 C39 -86.0(6) . . . . ? Cu1 P2 C34 C39 43.7(7) . . . . ? C46 P2 C34 C35 -12.3(6) . . . . ? C40 P2 C34 C35 95.1(5) . . . . ? Cu1 P2 C34 C35 -135.1(4) . . . . ? C39 C34 C35 C36 0.5(9) . . . . ? P2 C34 C35 C36 179.3(4) . . . . ? C34 C35 C36 C37 -1.0(9) . . . . ? C35 C36 C37 C38 2.6(11) . . . . ? C36 C37 C38 C39 -3.7(14) . . . . ? C35 C34 C39 C38 -1.6(13) . . . . ? P2 C34 C39 C38 179.5(7) . . . . ? C37 C38 C39 C34 3.3(15) . . . . ? C46 P2 C40 C45 84.4(4) . . . . ? C34 P2 C40 C45 -23.8(5) . . . . ? Cu1 P2 C40 C45 -155.1(4) . . . . ? C46 P2 C40 C41 -93.8(4) . . . . ? C34 P2 C40 C41 158.0(4) . . . . ? Cu1 P2 C40 C41 26.7(4) . . . . ? C45 C40 C41 C42 -2.7(7) . . . . ? P2 C40 C41 C42 175.6(4) . . . . ? C40 C41 C42 C43 2.0(8) . . . . ? C41 C42 C43 C44 -0.5(8) . . . . ? C42 C43 C44 C45 -0.5(8) . . . . ? C43 C44 C45 C40 -0.2(8) . . . . ? C41 C40 C45 C44 1.7(7) . . . . ? P2 C40 C45 C44 -176.5(4) . . . . ? C34 P2 C46 C47 -76.4(4) . . . . ? C40 P2 C46 C47 176.9(4) . . . . ? Cu1 P2 C46 C47 52.1(4) . . . . ? C34 P2 C46 C51 110.3(5) . . . . ? C40 P2 C46 C51 3.6(5) . . . . ? Cu1 P2 C46 C51 -121.2(4) . . . . ? C51 C46 C47 C48 0.0(8) . . . . ? P2 C46 C47 C48 -173.6(4) . . . . ? C46 C47 C48 C49 0.0(8) . . . . ? C47 C48 C49 C50 0.0(9) . . . . ? C48 C49 C50 C51 0.1(9) . . . . ? C47 C46 C51 C50 0.1(8) . . . . ? P2 C46 C51 C50 173.4(4) . . . . ? C49 C50 C51 C46 -0.1(9) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O4A H4A O1 0.90 2.20 2.768(18) 120.7 . O4A H4A N5 0.90 2.52 3.04(2) 117.3 . O4B H4B N6 0.85 2.32 2.90(2) 126.4 3_656 _diffrn_measured_fraction_theta_max 0.990 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.990 _refine_diff_density_max 0.859 _refine_diff_density_min -1.685 _refine_diff_density_rms 0.089 data_8 _database_code_depnum_ccdc_archive 'CCDC 917667' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C32 H24 Cu F3 N8 O2, C2 F3 O2, C2 H6 O' _chemical_formula_sum 'C36 H30 Cu F6 N8 O5' _chemical_formula_weight 832.22 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' 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' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.7362(2) _cell_length_b 12.7941(3) _cell_length_c 13.0346(3) _cell_angle_alpha 79.9940(10) _cell_angle_beta 85.8750(10) _cell_angle_gamma 74.6510(9) _cell_volume 1857.99(8) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9433 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 31.33 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.488 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 850 _exptl_absorpt_coefficient_mu 0.672 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7300 _exptl_absorpt_correction_T_max 0.7749 _exptl_absorpt_process_details ; APEX2 Software Suite; Bruker 2005. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker-Nonius X8kappa APEX II CCD area detector ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 45021 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_sigmaI/netI 0.0120 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.11 _diffrn_reflns_theta_max 25.25 _reflns_number_total 6528 _reflns_number_gt 6051 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker, 2007)' _computing_cell_refinement 'APEX2 Software Suite (Bruker, 2007)' _computing_data_reduction 'APEX2 Software Suite (Bruker, 2007)' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL and publCIF (Westrip, 2010)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0235P)^2^+2.4575P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6528 _refine_ls_number_parameters 507 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0615 _refine_ls_R_factor_gt 0.0575 _refine_ls_wR_factor_ref 0.1762 _refine_ls_wR_factor_gt 0.1718 _refine_ls_goodness_of_fit_ref 1.066 _refine_ls_restrained_S_all 1.066 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.51320(3) 0.29139(3) 0.18192(3) 0.02030(16) Uani 1 1 d . . . F1 F 0.2668(3) 0.2432(4) -0.0565(3) 0.1040(15) Uani 1 1 d . . . F2 F 0.4215(4) 0.1149(3) -0.0708(3) 0.1072(15) Uani 1 1 d . . . F3 F 0.3965(3) 0.2608(3) -0.1760(2) 0.0845(10) Uani 1 1 d . . . N1 N 0.5505(2) 0.4010(2) 0.2592(2) 0.0239(5) Uani 1 1 d . . . N2 N 0.4783(2) 0.5043(2) 0.2555(2) 0.0255(6) Uani 1 1 d . . . N3 N 0.3416(2) 0.3624(2) 0.2028(2) 0.0244(5) Uani 1 1 d . . . N4 N 0.3018(2) 0.4701(2) 0.2121(2) 0.0261(6) Uani 1 1 d . . . N5 N 0.5381(2) 0.1504(2) 0.3107(2) 0.0247(5) Uani 1 1 d . . . N6 N 0.6366(2) 0.0658(2) 0.3023(2) 0.0261(6) Uani 1 1 d . . . N7 N 0.6838(2) 0.2389(2) 0.1385(2) 0.0243(5) Uani 1 1 d . . . N8 N 0.7444(2) 0.1305(2) 0.1541(2) 0.0252(6) Uani 1 1 d . . . O1 O 0.46705(19) 0.20922(17) 0.08309(17) 0.0254(5) Uani 1 1 d . . . O2 O 0.4550(2) 0.3627(2) -0.0319(2) 0.0377(6) Uani 1 1 d . . . C1 C 0.5049(3) 0.5593(3) 0.3248(3) 0.0315(7) Uani 1 1 d . . . H1 H 0.4659 0.6322 0.3347 0.038 Uiso 1 1 calc R . . C2 C 0.6005(3) 0.4894(3) 0.3795(3) 0.0308(7) Uani 1 1 d . . . C3 C 0.6666(4) 0.4957(3) 0.4644(3) 0.0416(9) Uani 1 1 d . . . H3 H 0.6511 0.5610 0.4940 0.050 Uiso 1 1 calc R . . C4 C 0.7523(3) 0.4059(4) 0.5021(3) 0.0432(9) Uani 1 1 d . . . H4 H 0.7971 0.4088 0.5589 0.052 Uiso 1 1 calc R . . C5 C 0.7766(3) 0.3080(3) 0.4587(3) 0.0358(8) Uani 1 1 d . . . H5 H 0.8369 0.2466 0.4878 0.043 Uiso 1 1 calc R . . C6 C 0.7161(3) 0.2991(3) 0.3763(3) 0.0283(7) Uani 1 1 d . . . H6 H 0.7343 0.2335 0.3470 0.034 Uiso 1 1 calc R . . C7 C 0.6260(3) 0.3907(2) 0.3367(2) 0.0239(6) Uani 1 1 d . . . C8 C 0.1876(3) 0.4990(3) 0.2411(3) 0.0311(7) Uani 1 1 d . . . H8 H 0.1429 0.5701 0.2516 0.037 Uiso 1 1 calc R . . C9 C 0.1470(3) 0.4046(3) 0.2532(3) 0.0301(7) Uani 1 1 d . . . C10 C 0.0370(3) 0.3798(4) 0.2812(3) 0.0443(9) Uani 1 1 d . . . H10 H -0.0303 0.4345 0.2988 0.053 Uiso 1 1 calc R . . C11 C 0.0312(3) 0.2754(4) 0.2818(3) 0.0447(9) Uani 1 1 d . . . H11 H -0.0421 0.2575 0.2993 0.054 Uiso 1 1 calc R . . C12 C 0.1308(3) 0.1916(3) 0.2573(3) 0.0392(8) Uani 1 1 d . . . H12 H 0.1224 0.1194 0.2595 0.047 Uiso 1 1 calc R . . C13 C 0.2385(3) 0.2123(3) 0.2307(3) 0.0310(7) Uani 1 1 d . . . H13 H 0.3053 0.1561 0.2148 0.037 Uiso 1 1 calc R . . C14 C 0.2458(3) 0.3208(3) 0.2278(2) 0.0251(6) Uani 1 1 d . . . C15 C 0.3817(3) 0.5399(3) 0.1834(3) 0.0294(7) Uani 1 1 d . . . H15A H 0.3394 0.6173 0.1866 0.035 Uiso 1 1 calc R . . H15B H 0.4129 0.5347 0.1114 0.035 Uiso 1 1 calc R . . C16 C 0.6831(3) 0.0135(3) 0.3937(3) 0.0302(7) Uani 1 1 d . . . H16 H 0.7514 -0.0464 0.4044 0.036 Uiso 1 1 calc R . . C17 C 0.6115(3) 0.0644(3) 0.4702(3) 0.0290(7) Uani 1 1 d . . . C18 C 0.6124(3) 0.0499(3) 0.5806(3) 0.0375(8) Uani 1 1 d . . . H18 H 0.6716 -0.0057 0.6188 0.045 Uiso 1 1 calc R . . C19 C 0.5252(4) 0.1188(3) 0.6299(3) 0.0404(9) Uani 1 1 d . . . H19 H 0.5244 0.1110 0.7037 0.049 Uiso 1 1 calc R . . C20 C 0.4360(3) 0.2015(3) 0.5741(3) 0.0363(8) Uani 1 1 d . . . H20 H 0.3765 0.2472 0.6116 0.044 Uiso 1 1 calc R . . C21 C 0.4327(3) 0.2178(3) 0.4672(3) 0.0307(7) Uani 1 1 d . . . H21 H 0.3723 0.2733 0.4304 0.037 Uiso 1 1 calc R . . C22 C 0.5228(3) 0.1486(3) 0.4147(2) 0.0259(6) Uani 1 1 d . . . C23 C 0.8569(3) 0.1141(3) 0.1203(3) 0.0319(7) Uani 1 1 d . . . H23 H 0.9143 0.0455 0.1242 0.038 Uiso 1 1 calc R . . C24 C 0.8739(3) 0.2167(3) 0.0782(3) 0.0292(7) Uani 1 1 d . . . C25 C 0.9702(3) 0.2547(3) 0.0277(3) 0.0391(8) Uani 1 1 d . . . H25 H 1.0442 0.2049 0.0165 0.047 Uiso 1 1 calc R . . C26 C 0.9531(3) 0.3641(3) -0.0040(3) 0.0408(9) Uani 1 1 d . . . H26 H 1.0160 0.3912 -0.0384 0.049 Uiso 1 1 calc R . . C27 C 0.8430(3) 0.4392(3) 0.0130(3) 0.0368(8) Uani 1 1 d . . . H27 H 0.8349 0.5154 -0.0100 0.044 Uiso 1 1 calc R . . C28 C 0.7484(3) 0.4059(3) 0.0614(3) 0.0294(7) Uani 1 1 d . . . H28 H 0.6756 0.4571 0.0732 0.035 Uiso 1 1 calc R . . C29 C 0.7639(3) 0.2921(3) 0.0927(2) 0.0245(6) Uani 1 1 d . . . C30 C 0.6825(3) 0.0473(3) 0.1990(3) 0.0279(7) Uani 1 1 d . . . H30A H 0.6167 0.0509 0.1540 0.034 Uiso 1 1 calc R . . H30B H 0.7375 -0.0267 0.2031 0.034 Uiso 1 1 calc R . . C31 C 0.4420(3) 0.2710(3) -0.0037(2) 0.0265(7) Uani 1 1 d . . . C32 C 0.3813(4) 0.2219(4) -0.0778(3) 0.0453(9) Uani 1 1 d . . . F4 F 0.7160(3) 0.0527(3) 0.8011(3) 0.0844(10) Uani 1 1 d . . . F5 F 0.6883(3) 0.1668(3) 0.9095(3) 0.0793(9) Uani 1 1 d . . . F6 F 0.8260(3) 0.0196(3) 0.9291(2) 0.0784(9) Uani 1 1 d . . . O3 O 0.8130(3) 0.2574(3) 0.7559(3) 0.0673(9) Uani 1 1 d . . . O4 O 0.9529(4) 0.1011(3) 0.7793(5) 0.120(2) Uani 1 1 d . . . C33 C 0.8538(5) 0.1603(4) 0.7914(4) 0.0596(12) Uani 1 1 d . . . C34 C 0.7700(4) 0.1009(4) 0.8574(3) 0.0508(10) Uani 1 1 d . . . O5 O 0.1411(4) 0.1796(3) 0.7161(4) 0.0910(14) Uani 1 1 d . . . H5A H 0.0774 0.1612 0.7169 0.137 Uiso 1 1 calc R . . C35 C 0.1186(5) 0.2954(5) 0.6903(5) 0.0705(14) Uani 1 1 d . . . H35A H 0.1903 0.3179 0.7024 0.085 Uiso 1 1 calc R . . H35B H 0.0543 0.3299 0.7367 0.085 Uiso 1 1 calc R . . C36 C 0.0847(6) 0.3352(6) 0.5817(6) 0.090(2) Uani 1 1 d . . . H36A H 0.1490 0.3031 0.5353 0.135 Uiso 1 1 calc R . . H36B H 0.0692 0.4154 0.5676 0.135 Uiso 1 1 calc R . . H36C H 0.0132 0.3139 0.5695 0.135 Uiso 1 1 calc R . . 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 Cu1 0.0187(2) 0.0178(2) 0.0225(2) -0.00380(15) -0.00024(15) -0.00112(16) F1 0.0531(18) 0.206(5) 0.084(2) -0.063(3) 0.0008(16) -0.063(2) F2 0.179(4) 0.064(2) 0.099(3) -0.0302(19) -0.058(3) -0.043(2) F3 0.109(3) 0.128(3) 0.0295(13) -0.0161(15) -0.0055(14) -0.051(2) N1 0.0237(13) 0.0172(12) 0.0284(13) -0.0047(10) -0.0023(10) -0.0002(10) N2 0.0242(13) 0.0184(13) 0.0314(14) -0.0029(10) -0.0018(10) -0.0016(11) N3 0.0218(13) 0.0204(13) 0.0283(13) -0.0031(10) -0.0007(10) -0.0016(11) N4 0.0232(13) 0.0212(13) 0.0298(14) -0.0029(10) -0.0028(10) 0.0009(11) N5 0.0272(13) 0.0195(13) 0.0242(13) -0.0026(10) 0.0017(10) -0.0017(11) N6 0.0297(14) 0.0168(12) 0.0281(13) -0.0019(10) 0.0011(11) -0.0013(11) N7 0.0250(13) 0.0191(12) 0.0258(13) -0.0025(10) -0.0008(10) -0.0010(11) N8 0.0259(13) 0.0190(13) 0.0263(13) -0.0044(10) 0.0019(10) 0.0019(11) O1 0.0276(11) 0.0207(11) 0.0264(11) -0.0036(9) -0.0011(9) -0.0034(9) O2 0.0427(15) 0.0280(13) 0.0384(13) 0.0029(10) 0.0001(11) -0.0076(11) C1 0.0332(17) 0.0203(15) 0.0405(18) -0.0095(13) -0.0011(14) -0.0027(14) C2 0.0311(17) 0.0273(17) 0.0354(17) -0.0089(14) 0.0010(14) -0.0080(14) C3 0.042(2) 0.042(2) 0.046(2) -0.0211(17) -0.0061(17) -0.0098(18) C4 0.038(2) 0.055(2) 0.040(2) -0.0183(18) -0.0094(16) -0.0096(18) C5 0.0282(17) 0.039(2) 0.0378(19) -0.0041(15) -0.0048(14) -0.0050(15) C6 0.0221(15) 0.0266(16) 0.0356(17) -0.0057(13) -0.0021(13) -0.0041(13) C7 0.0230(15) 0.0210(15) 0.0277(15) -0.0034(12) 0.0021(12) -0.0070(12) C8 0.0224(16) 0.0323(18) 0.0332(17) -0.0088(14) -0.0039(13) 0.0052(14) C9 0.0224(16) 0.0372(19) 0.0278(16) -0.0077(14) -0.0024(12) -0.0005(14) C10 0.0247(17) 0.061(3) 0.047(2) -0.0204(19) 0.0048(15) -0.0055(17) C11 0.0279(18) 0.060(3) 0.052(2) -0.0175(19) 0.0058(16) -0.0185(18) C12 0.0339(19) 0.045(2) 0.042(2) -0.0082(16) 0.0022(15) -0.0156(17) C13 0.0285(17) 0.0315(18) 0.0331(17) -0.0045(14) -0.0007(13) -0.0084(14) C14 0.0199(14) 0.0320(17) 0.0212(14) -0.0021(12) -0.0020(11) -0.0041(13) C15 0.0280(16) 0.0208(15) 0.0351(17) 0.0014(13) -0.0048(13) -0.0016(13) C16 0.0339(18) 0.0218(16) 0.0311(17) 0.0013(13) -0.0029(13) -0.0036(14) C17 0.0336(17) 0.0230(16) 0.0285(16) 0.0001(12) -0.0028(13) -0.0062(14) C18 0.044(2) 0.037(2) 0.0293(17) 0.0024(14) -0.0060(15) -0.0100(17) C19 0.051(2) 0.048(2) 0.0241(17) -0.0045(15) -0.0011(15) -0.0173(19) C20 0.043(2) 0.0353(19) 0.0322(18) -0.0120(15) 0.0059(15) -0.0099(16) C21 0.0340(18) 0.0263(16) 0.0304(17) -0.0042(13) 0.0011(13) -0.0062(14) C22 0.0305(16) 0.0215(15) 0.0264(15) -0.0025(12) -0.0009(12) -0.0088(13) C23 0.0256(16) 0.0302(17) 0.0336(17) -0.0062(14) -0.0014(13) 0.0044(14) C24 0.0227(16) 0.0331(18) 0.0287(16) -0.0045(13) -0.0025(12) -0.0016(14) C25 0.0237(17) 0.051(2) 0.0402(19) -0.0059(17) 0.0016(14) -0.0068(16) C26 0.0312(19) 0.055(2) 0.0399(19) -0.0029(17) 0.0015(15) -0.0212(18) C27 0.041(2) 0.0376(19) 0.0360(18) 0.0012(15) -0.0053(15) -0.0205(17) C28 0.0278(16) 0.0289(17) 0.0300(16) -0.0034(13) -0.0040(13) -0.0048(14) C29 0.0226(15) 0.0290(16) 0.0218(14) -0.0041(12) -0.0029(11) -0.0061(13) C30 0.0335(17) 0.0176(15) 0.0295(16) -0.0053(12) 0.0022(13) -0.0009(13) C31 0.0247(15) 0.0265(17) 0.0259(15) -0.0048(13) 0.0014(12) -0.0029(13) C32 0.051(2) 0.059(3) 0.0311(19) -0.0108(17) -0.0049(16) -0.019(2) F4 0.091(2) 0.084(2) 0.091(2) -0.0372(19) -0.0316(19) -0.0219(19) F5 0.0677(19) 0.077(2) 0.092(2) -0.0364(18) 0.0152(17) -0.0069(16) F6 0.104(3) 0.0639(19) 0.0595(18) 0.0000(14) -0.0203(17) -0.0103(18) O3 0.071(2) 0.0334(16) 0.083(2) -0.0066(16) -0.0023(18) 0.0103(16) O4 0.079(3) 0.049(2) 0.187(6) 0.016(3) 0.049(3) 0.026(2) C33 0.059(3) 0.035(2) 0.073(3) -0.013(2) 0.003(2) 0.009(2) C34 0.059(3) 0.044(2) 0.048(2) -0.0210(19) -0.0098(19) 0.000(2) O5 0.067(2) 0.066(2) 0.107(3) 0.000(2) 0.013(2) 0.028(2) C35 0.051(3) 0.063(3) 0.084(4) -0.013(3) 0.007(3) 0.009(2) C36 0.074(4) 0.095(5) 0.100(5) 0.010(4) -0.032(4) -0.029(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Cu1 O1 1.983(2) . ? Cu1 N3 1.999(3) . ? Cu1 N7 2.010(3) . ? Cu1 N1 2.014(3) . ? Cu1 N5 2.212(3) . ? F1 C32 1.317(5) . ? F2 C32 1.314(6) . ? F3 C32 1.308(5) . ? N1 C7 1.357(4) . ? N1 N2 1.363(4) . ? N2 C1 1.336(4) . ? N2 C15 1.451(4) . ? N3 N4 1.356(4) . ? N3 C14 1.363(4) . ? N4 C8 1.338(4) . ? N4 C15 1.447(4) . ? N5 C22 1.351(4) . ? N5 N6 1.372(4) . ? N6 C16 1.337(4) . ? N6 C30 1.448(4) . ? N7 C29 1.349(4) . ? N7 N8 1.368(4) . ? N8 C23 1.335(4) . ? N8 C30 1.462(4) . ? O1 C31 1.267(4) . ? O2 C31 1.213(4) . ? C1 C2 1.389(5) . ? C1 H1 0.9500 . ? C2 C7 1.420(4) . ? C2 C3 1.421(5) . ? C3 C4 1.354(6) . ? C3 H3 0.9500 . ? C4 C5 1.416(5) . ? C4 H4 0.9500 . ? C5 C6 1.366(5) . ? C5 H5 0.9500 . ? C6 C7 1.404(5) . ? C6 H6 0.9500 . ? C8 C9 1.392(5) . ? C8 H8 0.9500 . ? C9 C10 1.418(5) . ? C9 C14 1.418(5) . ? C10 C11 1.354(6) . ? C10 H10 0.9500 . ? C11 C12 1.421(6) . ? C11 H11 0.9500 . ? C12 C13 1.368(5) . ? C12 H12 0.9500 . ? C13 C14 1.407(5) . ? C13 H13 0.9500 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.393(5) . ? C16 H16 0.9500 . ? C17 C18 1.418(5) . ? C17 C22 1.419(5) . ? C18 C19 1.365(6) . ? C18 H18 0.9500 . ? C19 C20 1.415(6) . ? C19 H19 0.9500 . ? C20 C21 1.374(5) . ? C20 H20 0.9500 . ? C21 C22 1.408(5) . ? C21 H21 0.9500 . ? C23 C24 1.392(5) . ? C23 H23 0.9500 . ? C24 C29 1.415(5) . ? C24 C25 1.422(5) . ? C25 C26 1.353(6) . ? C25 H25 0.9500 . ? C26 C27 1.420(6) . ? C26 H26 0.9500 . ? C27 C28 1.367(5) . ? C27 H27 0.9500 . ? C28 C29 1.408(5) . ? C28 H28 0.9500 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.542(5) . ? F4 C34 1.324(5) . ? F5 C34 1.329(5) . ? F6 C34 1.333(5) . ? O3 C33 1.226(6) . ? O4 C33 1.225(6) . ? C33 C34 1.527(7) . ? O5 C35 1.417(7) . ? O5 H5A 0.8400 . ? C35 C36 1.465(9) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? 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 O1 Cu1 N3 87.99(10) . . ? O1 Cu1 N7 90.29(10) . . ? N3 Cu1 N7 170.17(11) . . ? O1 Cu1 N1 168.42(10) . . ? N3 Cu1 N1 88.41(11) . . ? N7 Cu1 N1 91.39(10) . . ? O1 Cu1 N5 93.17(9) . . ? N3 Cu1 N5 100.37(10) . . ? N7 Cu1 N5 89.38(10) . . ? N1 Cu1 N5 98.30(10) . . ? C7 N1 N2 104.6(2) . . ? C7 N1 Cu1 132.7(2) . . ? N2 N1 Cu1 121.4(2) . . ? C1 N2 N1 113.2(3) . . ? C1 N2 C15 128.0(3) . . ? N1 N2 C15 118.7(3) . . ? N4 N3 C14 104.6(2) . . ? N4 N3 Cu1 122.0(2) . . ? C14 N3 Cu1 132.5(2) . . ? C8 N4 N3 113.4(3) . . ? C8 N4 C15 128.2(3) . . ? N3 N4 C15 118.3(3) . . ? C22 N5 N6 103.3(2) . . ? C22 N5 Cu1 130.1(2) . . ? N6 N5 Cu1 115.91(18) . . ? C16 N6 N5 114.0(3) . . ? C16 N6 C30 127.6(3) . . ? N5 N6 C30 118.3(3) . . ? C29 N7 N8 104.5(2) . . ? C29 N7 Cu1 132.6(2) . . ? N8 N7 Cu1 122.9(2) . . ? C23 N8 N7 113.0(3) . . ? C23 N8 C30 127.4(3) . . ? N7 N8 C30 119.5(2) . . ? C31 O1 Cu1 109.93(19) . . ? N2 C1 C2 106.8(3) . . ? N2 C1 H1 126.6 . . ? C2 C1 H1 126.6 . . ? C1 C2 C7 105.3(3) . . ? C1 C2 C3 135.0(3) . . ? C7 C2 C3 119.6(3) . . ? C4 C3 C2 118.3(3) . . ? C4 C3 H3 120.9 . . ? C2 C3 H3 120.9 . . ? C3 C4 C5 121.5(3) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C6 C5 C4 122.0(3) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C5 C6 C7 117.5(3) . . ? C5 C6 H6 121.3 . . ? C7 C6 H6 121.3 . . ? N1 C7 C6 128.8(3) . . ? N1 C7 C2 110.1(3) . . ? C6 C7 C2 121.1(3) . . ? N4 C8 C9 106.7(3) . . ? N4 C8 H8 126.6 . . ? C9 C8 H8 126.6 . . ? C8 C9 C10 135.0(3) . . ? C8 C9 C14 105.3(3) . . ? C10 C9 C14 119.7(3) . . ? C11 C10 C9 117.6(4) . . ? C11 C10 H10 121.2 . . ? C9 C10 H10 121.2 . . ? C10 C11 C12 122.4(3) . . ? C10 C11 H11 118.8 . . ? C12 C11 H11 118.8 . . ? C13 C12 C11 121.7(4) . . ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? C12 C13 C14 116.8(3) . . ? C12 C13 H13 121.6 . . ? C14 C13 H13 121.6 . . ? N3 C14 C13 128.1(3) . . ? N3 C14 C9 110.0(3) . . ? C13 C14 C9 121.9(3) . . ? N4 C15 N2 108.6(3) . . ? N4 C15 H15A 110.0 . . ? N2 C15 H15A 110.0 . . ? N4 C15 H15B 110.0 . . ? N2 C15 H15B 110.0 . . ? H15A C15 H15B 108.3 . . ? N6 C16 C17 106.3(3) . . ? N6 C16 H16 126.8 . . ? C17 C16 H16 126.8 . . ? C16 C17 C18 134.8(3) . . ? C16 C17 C22 104.9(3) . . ? C18 C17 C22 120.3(3) . . ? C19 C18 C17 117.6(3) . . ? C19 C18 H18 121.2 . . ? C17 C18 H18 121.2 . . ? C18 C19 C20 121.8(3) . . ? C18 C19 H19 119.1 . . ? C20 C19 H19 119.1 . . ? C21 C20 C19 122.0(3) . . ? C21 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? C20 C21 C22 117.1(3) . . ? C20 C21 H21 121.4 . . ? C22 C21 H21 121.4 . . ? N5 C22 C21 127.4(3) . . ? N5 C22 C17 111.4(3) . . ? C21 C22 C17 121.2(3) . . ? N8 C23 C24 106.8(3) . . ? N8 C23 H23 126.6 . . ? C24 C23 H23 126.6 . . ? C23 C24 C29 105.1(3) . . ? C23 C24 C25 134.7(3) . . ? C29 C24 C25 120.1(3) . . ? C26 C25 C24 117.8(3) . . ? C26 C25 H25 121.1 . . ? C24 C25 H25 121.1 . . ? C25 C26 C27 121.5(3) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C28 C27 C26 122.4(3) . . ? C28 C27 H27 118.8 . . ? C26 C27 H27 118.8 . . ? C27 C28 C29 116.8(3) . . ? C27 C28 H28 121.6 . . ? C29 C28 H28 121.6 . . ? N7 C29 C28 128.2(3) . . ? N7 C29 C24 110.6(3) . . ? C28 C29 C24 121.3(3) . . ? N6 C30 N8 109.8(2) . . ? N6 C30 H30A 109.7 . . ? N8 C30 H30A 109.7 . . ? N6 C30 H30B 109.7 . . ? N8 C30 H30B 109.7 . . ? H30A C30 H30B 108.2 . . ? O2 C31 O1 128.3(3) . . ? O2 C31 C32 118.2(3) . . ? O1 C31 C32 113.4(3) . . ? F3 C32 F2 105.0(4) . . ? F3 C32 F1 108.0(4) . . ? F2 C32 F1 107.5(4) . . ? F3 C32 C31 112.9(3) . . ? F2 C32 C31 113.2(3) . . ? F1 C32 C31 110.0(3) . . ? O4 C33 O3 129.4(5) . . ? O4 C33 C34 113.6(4) . . ? O3 C33 C34 117.0(4) . . ? F4 C34 F5 108.4(4) . . ? F4 C34 F6 104.4(4) . . ? F5 C34 F6 105.7(4) . . ? F4 C34 C33 112.3(4) . . ? F5 C34 C33 112.8(4) . . ? F6 C34 C33 112.6(4) . . ? C35 O5 H5A 109.5 . . ? O5 C35 C36 112.3(6) . . ? O5 C35 H35A 109.1 . . ? C36 C35 H35A 109.1 . . ? O5 C35 H35B 109.1 . . ? C36 C35 H35B 109.1 . . ? H35A C35 H35B 107.9 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? 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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O1 Cu1 N1 C7 -154.5(4) . . . . ? N3 Cu1 N1 C7 133.6(3) . . . . ? N7 Cu1 N1 C7 -56.3(3) . . . . ? N5 Cu1 N1 C7 33.3(3) . . . . ? O1 Cu1 N1 N2 40.9(6) . . . . ? N3 Cu1 N1 N2 -31.1(2) . . . . ? N7 Cu1 N1 N2 139.1(2) . . . . ? N5 Cu1 N1 N2 -131.3(2) . . . . ? C7 N1 N2 C1 0.7(3) . . . . ? Cu1 N1 N2 C1 169.1(2) . . . . ? C7 N1 N2 C15 -176.6(3) . . . . ? Cu1 N1 N2 C15 -8.2(4) . . . . ? O1 Cu1 N3 N4 -140.6(2) . . . . ? N1 Cu1 N3 N4 28.4(2) . . . . ? N5 Cu1 N3 N4 126.6(2) . . . . ? O1 Cu1 N3 C14 52.1(3) . . . . ? N1 Cu1 N3 C14 -139.0(3) . . . . ? N5 Cu1 N3 C14 -40.8(3) . . . . ? C14 N3 N4 C8 0.0(3) . . . . ? Cu1 N3 N4 C8 -170.4(2) . . . . ? C14 N3 N4 C15 -175.8(3) . . . . ? Cu1 N3 N4 C15 13.8(4) . . . . ? O1 Cu1 N5 C22 -149.0(3) . . . . ? N3 Cu1 N5 C22 -60.4(3) . . . . ? N7 Cu1 N5 C22 120.8(3) . . . . ? N1 Cu1 N5 C22 29.5(3) . . . . ? O1 Cu1 N5 N6 73.1(2) . . . . ? N3 Cu1 N5 N6 161.6(2) . . . . ? N7 Cu1 N5 N6 -17.2(2) . . . . ? N1 Cu1 N5 N6 -108.5(2) . . . . ? C22 N5 N6 C16 -0.8(3) . . . . ? Cu1 N5 N6 C16 147.5(2) . . . . ? C22 N5 N6 C30 -177.0(3) . . . . ? Cu1 N5 N6 C30 -28.8(3) . . . . ? O1 Cu1 N7 C29 117.6(3) . . . . ? N1 Cu1 N7 C29 -50.9(3) . . . . ? N5 Cu1 N7 C29 -149.2(3) . . . . ? O1 Cu1 N7 N8 -63.4(2) . . . . ? N1 Cu1 N7 N8 128.0(2) . . . . ? N5 Cu1 N7 N8 29.7(2) . . . . ? C29 N7 N8 C23 -0.2(3) . . . . ? Cu1 N7 N8 C23 -179.4(2) . . . . ? C29 N7 N8 C30 -177.4(3) . . . . ? Cu1 N7 N8 C30 3.4(4) . . . . ? N3 Cu1 O1 C31 77.9(2) . . . . ? N7 Cu1 O1 C31 -92.4(2) . . . . ? N1 Cu1 O1 C31 5.9(6) . . . . ? N5 Cu1 O1 C31 178.2(2) . . . . ? N1 N2 C1 C2 -0.3(4) . . . . ? C15 N2 C1 C2 176.7(3) . . . . ? N2 C1 C2 C7 -0.2(4) . . . . ? N2 C1 C2 C3 -176.9(4) . . . . ? C1 C2 C3 C4 176.0(4) . . . . ? C7 C2 C3 C4 -0.3(6) . . . . ? C2 C3 C4 C5 0.1(6) . . . . ? C3 C4 C5 C6 0.7(6) . . . . ? C4 C5 C6 C7 -1.3(5) . . . . ? N2 N1 C7 C6 177.4(3) . . . . ? Cu1 N1 C7 C6 10.9(5) . . . . ? N2 N1 C7 C2 -0.8(3) . . . . ? Cu1 N1 C7 C2 -167.3(2) . . . . ? C5 C6 C7 N1 -176.8(3) . . . . ? C5 C6 C7 C2 1.2(5) . . . . ? C1 C2 C7 N1 0.7(4) . . . . ? C3 C2 C7 N1 177.9(3) . . . . ? C1 C2 C7 C6 -177.7(3) . . . . ? C3 C2 C7 C6 -0.4(5) . . . . ? N3 N4 C8 C9 0.4(4) . . . . ? C15 N4 C8 C9 175.7(3) . . . . ? N4 C8 C9 C10 -179.4(4) . . . . ? N4 C8 C9 C14 -0.6(4) . . . . ? C8 C9 C10 C11 178.3(4) . . . . ? C14 C9 C10 C11 -0.3(5) . . . . ? C9 C10 C11 C12 1.0(6) . . . . ? C10 C11 C12 C13 -0.6(6) . . . . ? C11 C12 C13 C14 -0.5(5) . . . . ? N4 N3 C14 C13 -180.0(3) . . . . ? Cu1 N3 C14 C13 -11.0(5) . . . . ? N4 N3 C14 C9 -0.4(3) . . . . ? Cu1 N3 C14 C9 168.6(2) . . . . ? C12 C13 C14 N3 -179.3(3) . . . . ? C12 C13 C14 C9 1.2(5) . . . . ? C8 C9 C14 N3 0.6(4) . . . . ? C10 C9 C14 N3 179.6(3) . . . . ? C8 C9 C14 C13 -179.8(3) . . . . ? C10 C9 C14 C13 -0.8(5) . . . . ? C8 N4 C15 N2 119.2(3) . . . . ? N3 N4 C15 N2 -65.7(4) . . . . ? C1 N2 C15 N4 -114.5(3) . . . . ? N1 N2 C15 N4 62.4(4) . . . . ? N5 N6 C16 C17 0.7(4) . . . . ? C30 N6 C16 C17 176.5(3) . . . . ? N6 C16 C17 C18 -179.2(4) . . . . ? N6 C16 C17 C22 -0.3(4) . . . . ? C16 C17 C18 C19 179.2(4) . . . . ? C22 C17 C18 C19 0.5(5) . . . . ? C17 C18 C19 C20 0.5(6) . . . . ? C18 C19 C20 C21 -0.6(6) . . . . ? C19 C20 C21 C22 -0.3(5) . . . . ? N6 N5 C22 C21 -179.1(3) . . . . ? Cu1 N5 C22 C21 39.1(5) . . . . ? N6 N5 C22 C17 0.5(3) . . . . ? Cu1 N5 C22 C17 -141.3(2) . . . . ? C20 C21 C22 N5 -179.1(3) . . . . ? C20 C21 C22 C17 1.3(5) . . . . ? C16 C17 C22 N5 -0.1(4) . . . . ? C18 C17 C22 N5 178.9(3) . . . . ? C16 C17 C22 C21 179.5(3) . . . . ? C18 C17 C22 C21 -1.4(5) . . . . ? N7 N8 C23 C24 -0.7(4) . . . . ? C30 N8 C23 C24 176.3(3) . . . . ? N8 C23 C24 C29 1.2(4) . . . . ? N8 C23 C24 C25 -177.7(4) . . . . ? C23 C24 C25 C26 179.7(4) . . . . ? C29 C24 C25 C26 0.9(5) . . . . ? C24 C25 C26 C27 0.5(6) . . . . ? C25 C26 C27 C28 -0.5(6) . . . . ? C26 C27 C28 C29 -0.9(5) . . . . ? N8 N7 C29 C28 -178.9(3) . . . . ? Cu1 N7 C29 C28 0.2(5) . . . . ? N8 N7 C29 C24 1.0(3) . . . . ? Cu1 N7 C29 C24 -180.0(2) . . . . ? C27 C28 C29 N7 -177.8(3) . . . . ? C27 C28 C29 C24 2.4(5) . . . . ? C23 C24 C29 N7 -1.4(4) . . . . ? C25 C24 C29 N7 177.7(3) . . . . ? C23 C24 C29 C28 178.5(3) . . . . ? C25 C24 C29 C28 -2.4(5) . . . . ? C16 N6 C30 N8 -100.2(4) . . . . ? N5 N6 C30 N8 75.5(3) . . . . ? C23 N8 C30 N6 122.0(3) . . . . ? N7 N8 C30 N6 -61.2(4) . . . . ? Cu1 O1 C31 O2 8.1(4) . . . . ? Cu1 O1 C31 C32 -168.3(2) . . . . ? O2 C31 C32 F3 28.1(5) . . . . ? O1 C31 C32 F3 -155.1(4) . . . . ? O2 C31 C32 F2 147.2(4) . . . . ? O1 C31 C32 F2 -35.9(5) . . . . ? O2 C31 C32 F1 -92.6(4) . . . . ? O1 C31 C32 F1 84.3(4) . . . . ? O4 C33 C34 F4 -86.3(6) . . . . ? O3 C33 C34 F4 91.6(5) . . . . ? O4 C33 C34 F5 150.8(6) . . . . ? O3 C33 C34 F5 -31.4(6) . . . . ? O4 C33 C34 F6 31.2(7) . . . . ? O3 C33 C34 F6 -150.9(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O5 H5A O4 0.84 1.90 2.682(7) 155.2 1_455 _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.613 _refine_diff_density_min -0.425 _refine_diff_density_rms 0.118 data_9 _database_code_depnum_ccdc_archive 'CCDC 917668' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H24 Cl4 Cu2 N8' _chemical_formula_sum 'C30 H24 Cl4 Cu2 N8' _chemical_formula_weight 765.45 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_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' _cell_length_a 18.3110(7) _cell_length_b 15.5229(6) _cell_length_c 13.5546(9) _cell_angle_alpha 90.00 _cell_angle_beta 128.0440(10) _cell_angle_gamma 90.00 _cell_volume 3034.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 5992 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 27.25 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.676 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1544 _exptl_absorpt_coefficient_mu 1.791 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8005 _exptl_absorpt_correction_T_max 0.8554 _exptl_absorpt_process_details ; APEX2 Software Suite; Bruker 2005. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker-Nonius X8kappa APEX II CCD area detector ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 22059 _diffrn_reflns_av_R_equivalents 0.0462 _diffrn_reflns_av_sigmaI/netI 0.0297 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 25.24 _reflns_number_total 2756 _reflns_number_gt 2256 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker, 2007)' _computing_cell_refinement 'APEX2 Software Suite (Bruker, 2007)' _computing_data_reduction 'APEX2 Software Suite (Bruker, 2007)' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL and publCIF (Westrip, 2010)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0585P)^2^+1.6912P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2756 _refine_ls_number_parameters 199 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0541 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.1117 _refine_ls_wR_factor_gt 0.1065 _refine_ls_goodness_of_fit_ref 1.052 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.24295(3) 0.18048(3) 0.38187(4) 0.02334(17) Uani 1 1 d . . . Cl1 Cl 0.35273(7) 0.27171(6) 0.53083(10) 0.0321(3) Uani 1 1 d . . . Cl2 Cl 0.19527(9) 0.27161(6) 0.22396(10) 0.0417(3) Uani 1 1 d . . . N1 N 0.1572(2) 0.01122(18) 0.2573(3) 0.0207(7) Uani 1 1 d . . . N2 N 0.1412(2) 0.09737(18) 0.2610(3) 0.0208(7) Uani 1 1 d . . . N3 N 0.3017(2) -0.00374(19) 0.4574(3) 0.0256(7) Uani 1 1 d . . . N4 N 0.3138(2) 0.07951(19) 0.5000(3) 0.0269(7) Uani 1 1 d . . . C1 C 0.0507(2) 0.1082(2) 0.1865(3) 0.0208(8) Uani 1 1 d . . . H1 H 0.0203 0.1618 0.1711 0.025 Uiso 1 1 calc R . . C2 C 0.0048(3) 0.0286(2) 0.1326(3) 0.0203(8) Uani 1 1 d . . . C3 C -0.0891(3) 0.0022(2) 0.0489(4) 0.0246(8) Uani 1 1 d . . . H3 H -0.1385 0.0423 0.0156 0.029 Uiso 1 1 calc R . . C4 C -0.1058(3) -0.0836(2) 0.0182(4) 0.0273(9) Uani 1 1 d . . . H4 H -0.1681 -0.1034 -0.0353 0.033 Uiso 1 1 calc R . . C5 C -0.0335(3) -0.1431(2) 0.0633(4) 0.0279(9) Uani 1 1 d . . . H5 H -0.0485 -0.2015 0.0371 0.033 Uiso 1 1 calc R . . C6 C 0.0584(3) -0.1194(2) 0.1443(4) 0.0236(8) Uani 1 1 d . . . H6 H 0.1072 -0.1595 0.1747 0.028 Uiso 1 1 calc R . . C7 C 0.0755(3) -0.0318(2) 0.1794(3) 0.0195(8) Uani 1 1 d . . . C8 C 0.3561(3) 0.0751(3) 0.6212(4) 0.0295(9) Uani 1 1 d . . . H8 H 0.3733 0.1236 0.6743 0.035 Uiso 1 1 calc R . . C9 C 0.3722(3) -0.0117(3) 0.6612(4) 0.0274(9) Uani 1 1 d . . . C10 C 0.4123(3) -0.0540(3) 0.7759(4) 0.0358(10) Uani 1 1 d . . . H10 H 0.4390 -0.0226 0.8511 0.043 Uiso 1 1 calc R . . C11 C 0.4114(3) -0.1423(3) 0.7751(5) 0.0409(11) Uani 1 1 d . . . H11 H 0.4370 -0.1722 0.8511 0.049 Uiso 1 1 calc R . . C12 C 0.3737(3) -0.1899(3) 0.6651(4) 0.0385(11) Uani 1 1 d . . . H12 H 0.3749 -0.2510 0.6693 0.046 Uiso 1 1 calc R . . C13 C 0.3353(3) -0.1511(3) 0.5525(4) 0.0313(9) Uani 1 1 d . . . H13 H 0.3103 -0.1834 0.4785 0.038 Uiso 1 1 calc R . . C14 C 0.3348(3) -0.0603(2) 0.5526(4) 0.0249(8) Uani 1 1 d . . . C15 C 0.2513(3) -0.0172(2) 0.3252(3) 0.0240(8) Uani 1 1 d . . . H15A H 0.2815 0.0151 0.2963 0.029 Uiso 1 1 calc R . . H15B H 0.2522 -0.0791 0.3087 0.029 Uiso 1 1 calc R . . 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 Cu1 0.0227(3) 0.0113(2) 0.0319(3) -0.00267(18) 0.0148(2) -0.00452(18) Cl1 0.0270(5) 0.0205(5) 0.0432(6) -0.0093(4) 0.0188(5) -0.0104(4) Cl2 0.0609(8) 0.0222(5) 0.0400(6) -0.0008(4) 0.0301(6) -0.0158(5) N1 0.0184(15) 0.0080(13) 0.0296(16) -0.0002(12) 0.0117(14) 0.0012(12) N2 0.0228(17) 0.0097(14) 0.0289(17) -0.0005(12) 0.0154(14) 0.0002(12) N3 0.0246(17) 0.0132(15) 0.0311(18) 0.0005(13) 0.0132(15) 0.0022(13) N4 0.0237(17) 0.0139(15) 0.0329(19) -0.0050(13) 0.0124(15) -0.0034(13) C1 0.0208(19) 0.0150(17) 0.0248(19) 0.0004(14) 0.0130(16) 0.0002(14) C2 0.0238(19) 0.0167(17) 0.0234(18) 0.0003(14) 0.0160(16) 0.0005(15) C3 0.023(2) 0.0222(19) 0.030(2) 0.0005(16) 0.0177(17) -0.0010(16) C4 0.025(2) 0.027(2) 0.032(2) -0.0055(17) 0.0188(18) -0.0108(17) C5 0.037(2) 0.0132(17) 0.034(2) -0.0033(16) 0.0222(19) -0.0077(17) C6 0.028(2) 0.0120(17) 0.030(2) -0.0002(15) 0.0179(18) -0.0027(15) C7 0.0244(19) 0.0134(17) 0.0224(18) 0.0026(14) 0.0152(16) -0.0012(15) C8 0.024(2) 0.025(2) 0.030(2) -0.0027(17) 0.0122(18) 0.0007(17) C9 0.0210(19) 0.027(2) 0.029(2) 0.0015(17) 0.0133(17) 0.0076(16) C10 0.034(2) 0.039(2) 0.035(2) 0.0056(19) 0.021(2) 0.011(2) C11 0.042(3) 0.039(3) 0.046(3) 0.018(2) 0.029(2) 0.015(2) C12 0.048(3) 0.025(2) 0.050(3) 0.013(2) 0.033(2) 0.0099(19) C13 0.031(2) 0.023(2) 0.044(2) 0.0021(18) 0.025(2) 0.0039(17) C14 0.0194(19) 0.0207(19) 0.036(2) 0.0049(16) 0.0175(18) 0.0028(15) C15 0.026(2) 0.0148(17) 0.030(2) -0.0017(15) 0.0163(17) 0.0019(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Cu1 N2 2.014(3) . ? Cu1 N4 2.036(3) . ? Cu1 Cl2 2.2453(11) . ? Cu1 Cl1 2.2629(10) . ? Cu1 Cl1 2.7522(11) 7_556 ? Cl1 Cu1 2.7522(11) 7_556 ? N1 C7 1.361(5) . ? N1 N2 1.376(4) . ? N1 C15 1.433(5) . ? N2 C1 1.316(5) . ? N3 C14 1.356(5) . ? N3 N4 1.377(4) . ? N3 C15 1.438(5) . ? N4 C8 1.317(5) . ? C1 C2 1.417(5) . ? C1 H1 0.9500 . ? C2 C7 1.395(5) . ? C2 C3 1.417(5) . ? C3 C4 1.373(5) . ? C3 H3 0.9500 . ? C4 C5 1.409(6) . ? C4 H4 0.9500 . ? C5 C6 1.376(5) . ? C5 H5 0.9500 . ? C6 C7 1.411(5) . ? C6 H6 0.9500 . ? C8 C9 1.415(6) . ? C8 H8 0.9500 . ? C9 C14 1.401(6) . ? C9 C10 1.407(6) . ? C10 C11 1.370(6) . ? C10 H10 0.9500 . ? C11 C12 1.405(7) . ? C11 H11 0.9500 . ? C12 C13 1.365(6) . ? C12 H12 0.9500 . ? C13 C14 1.410(5) . ? C13 H13 0.9500 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? 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 Cu1 N4 88.19(12) . . ? N2 Cu1 Cl2 90.39(9) . . ? N4 Cu1 Cl2 156.91(11) . . ? N2 Cu1 Cl1 173.90(9) . . ? N4 Cu1 Cl1 89.71(9) . . ? Cl2 Cu1 Cl1 93.79(4) . . ? N2 Cu1 Cl1 90.44(9) . 7_556 ? N4 Cu1 Cl1 97.79(10) . 7_556 ? Cl2 Cu1 Cl1 105.27(4) . 7_556 ? Cl1 Cu1 Cl1 84.17(4) . 7_556 ? Cu1 Cl1 Cu1 95.83(4) . 7_556 ? C7 N1 N2 110.4(3) . . ? C7 N1 C15 131.2(3) . . ? N2 N1 C15 118.3(3) . . ? C1 N2 N1 106.9(3) . . ? C1 N2 Cu1 129.7(2) . . ? N1 N2 Cu1 122.8(2) . . ? C14 N3 N4 110.3(3) . . ? C14 N3 C15 131.3(3) . . ? N4 N3 C15 118.2(3) . . ? C8 N4 N3 107.1(3) . . ? C8 N4 Cu1 128.4(3) . . ? N3 N4 Cu1 122.2(2) . . ? N2 C1 C2 110.5(3) . . ? N2 C1 H1 124.7 . . ? C2 C1 H1 124.7 . . ? C7 C2 C3 119.9(3) . . ? C7 C2 C1 105.2(3) . . ? C3 C2 C1 134.9(3) . . ? C4 C3 C2 117.2(4) . . ? C4 C3 H3 121.4 . . ? C2 C3 H3 121.4 . . ? C3 C4 C5 122.0(4) . . ? C3 C4 H4 119.0 . . ? C5 C4 H4 119.0 . . ? C6 C5 C4 122.1(3) . . ? C6 C5 H5 119.0 . . ? C4 C5 H5 119.0 . . ? C5 C6 C7 115.8(3) . . ? C5 C6 H6 122.1 . . ? C7 C6 H6 122.1 . . ? N1 C7 C2 106.9(3) . . ? N1 C7 C6 130.1(3) . . ? C2 C7 C6 123.0(3) . . ? N4 C8 C9 110.5(4) . . ? N4 C8 H8 124.7 . . ? C9 C8 H8 124.7 . . ? C14 C9 C10 119.6(4) . . ? C14 C9 C8 105.0(3) . . ? C10 C9 C8 135.4(4) . . ? C11 C10 C9 117.6(4) . . ? C11 C10 H10 121.2 . . ? C9 C10 H10 121.2 . . ? C10 C11 C12 122.0(4) . . ? C10 C11 H11 119.0 . . ? C12 C11 H11 119.0 . . ? C13 C12 C11 122.1(4) . . ? C13 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? C12 C13 C14 116.1(4) . . ? C12 C13 H13 122.0 . . ? C14 C13 H13 122.0 . . ? N3 C14 C9 107.1(3) . . ? N3 C14 C13 130.2(4) . . ? C9 C14 C13 122.7(4) . . ? N1 C15 N3 110.5(3) . . ? N1 C15 H15A 109.5 . . ? N3 C15 H15A 109.5 . . ? N1 C15 H15B 109.5 . . ? N3 C15 H15B 109.5 . . ? H15A C15 H15B 108.1 . . ? 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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Cu1 Cl1 Cu1 -97.86(10) . . . 7_556 ? Cl2 Cu1 Cl1 Cu1 104.99(4) . . . 7_556 ? Cl1 Cu1 Cl1 Cu1 0.0 7_556 . . 7_556 ? C7 N1 N2 C1 0.1(4) . . . . ? C15 N1 N2 C1 176.4(3) . . . . ? C7 N1 N2 Cu1 171.9(2) . . . . ? C15 N1 N2 Cu1 -11.9(4) . . . . ? N4 Cu1 N2 C1 142.8(3) . . . . ? Cl2 Cu1 N2 C1 -60.3(3) . . . . ? Cl1 Cu1 N2 C1 45.0(3) 7_556 . . . ? N4 Cu1 N2 N1 -27.0(3) . . . . ? Cl2 Cu1 N2 N1 130.0(3) . . . . ? Cl1 Cu1 N2 N1 -124.8(3) 7_556 . . . ? C14 N3 N4 C8 1.4(4) . . . . ? C15 N3 N4 C8 176.0(3) . . . . ? C14 N3 N4 Cu1 -162.5(3) . . . . ? C15 N3 N4 Cu1 12.1(5) . . . . ? N2 Cu1 N4 C8 -133.5(4) . . . . ? Cl2 Cu1 N4 C8 139.8(3) . . . . ? Cl1 Cu1 N4 C8 40.8(3) . . . . ? Cl1 Cu1 N4 C8 -43.3(4) 7_556 . . . ? N2 Cu1 N4 N3 26.8(3) . . . . ? Cl2 Cu1 N4 N3 -59.9(4) . . . . ? Cl1 Cu1 N4 N3 -158.9(3) . . . . ? Cl1 Cu1 N4 N3 117.0(3) 7_556 . . . ? N1 N2 C1 C2 0.5(4) . . . . ? Cu1 N2 C1 C2 -170.5(2) . . . . ? N2 C1 C2 C7 -0.8(4) . . . . ? N2 C1 C2 C3 179.4(4) . . . . ? C7 C2 C3 C4 0.3(5) . . . . ? C1 C2 C3 C4 180.0(4) . . . . ? C2 C3 C4 C5 -2.3(6) . . . . ? C3 C4 C5 C6 2.2(6) . . . . ? C4 C5 C6 C7 0.1(6) . . . . ? N2 N1 C7 C2 -0.6(4) . . . . ? C15 N1 C7 C2 -176.2(4) . . . . ? N2 N1 C7 C6 177.8(4) . . . . ? C15 N1 C7 C6 2.2(7) . . . . ? C3 C2 C7 N1 -179.4(3) . . . . ? C1 C2 C7 N1 0.8(4) . . . . ? C3 C2 C7 C6 2.1(5) . . . . ? C1 C2 C7 C6 -177.7(3) . . . . ? C5 C6 C7 N1 179.6(4) . . . . ? C5 C6 C7 C2 -2.2(5) . . . . ? N3 N4 C8 C9 -0.4(5) . . . . ? Cu1 N4 C8 C9 162.2(3) . . . . ? N4 C8 C9 C14 -0.6(5) . . . . ? N4 C8 C9 C10 -179.0(4) . . . . ? C14 C9 C10 C11 -1.0(6) . . . . ? C8 C9 C10 C11 177.2(5) . . . . ? C9 C10 C11 C12 1.1(7) . . . . ? C10 C11 C12 C13 -0.4(7) . . . . ? C11 C12 C13 C14 -0.6(6) . . . . ? N4 N3 C14 C9 -1.8(4) . . . . ? C15 N3 C14 C9 -175.5(4) . . . . ? N4 N3 C14 C13 178.3(4) . . . . ? C15 N3 C14 C13 4.6(7) . . . . ? C10 C9 C14 N3 -179.8(4) . . . . ? C8 C9 C14 N3 1.5(4) . . . . ? C10 C9 C14 C13 0.1(6) . . . . ? C8 C9 C14 C13 -178.6(4) . . . . ? C12 C13 C14 N3 -179.4(4) . . . . ? C12 C13 C14 C9 0.7(6) . . . . ? C7 N1 C15 N3 -120.9(4) . . . . ? N2 N1 C15 N3 63.8(4) . . . . ? C14 N3 C15 N1 109.5(4) . . . . ? N4 N3 C15 N1 -63.8(4) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.666 _refine_diff_density_min -0.439 _refine_diff_density_rms 0.094 data_10 _database_code_depnum_ccdc_archive 'CCDC 917669' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C18 H19 Cl2 Cu N5 O' _chemical_formula_sum 'C18 H19 Cl2 Cu N5 O' _chemical_formula_weight 455.82 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' Cl Cl 0.1484 0.1585 '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' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 9.4972(4) _cell_length_b 18.6410(7) _cell_length_c 21.2437(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3760.9(2) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9936 _cell_measurement_theta_min 2.59 _cell_measurement_theta_max 30.38 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.52 _exptl_crystal_size_min 0.25 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.610 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1864 _exptl_absorpt_coefficient_mu 1.465 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5052 _exptl_absorpt_correction_T_max 0.7109 _exptl_absorpt_process_details ; APEX2 Software Suite; Bruker 2005. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker-Nonius X8kappa APEX II CCD area detector ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 27232 _diffrn_reflns_av_R_equivalents 0.0295 _diffrn_reflns_av_sigmaI/netI 0.0166 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.25 _reflns_number_total 3397 _reflns_number_gt 3012 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker, 2007)' _computing_cell_refinement 'APEX2 Software Suite (Bruker, 2007)' _computing_data_reduction 'APEX2 Software Suite (Bruker, 2007)' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL and publCIF (Westrip, 2010)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0393P)^2^+2.4860P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3397 _refine_ls_number_parameters 246 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0315 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0710 _refine_ls_wR_factor_gt 0.0688 _refine_ls_goodness_of_fit_ref 1.063 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 1.05972(3) 0.237896(13) 0.384698(11) 0.01842(9) Uani 1 1 d . . . Cl1 Cl 1.29723(6) 0.22807(3) 0.38371(3) 0.03290(15) Uani 1 1 d . . . Cl2 Cl 0.99089(5) 0.35154(3) 0.43492(2) 0.02311(13) Uani 1 1 d . . . O1 O 1.06302(16) 0.27903(8) 0.29866(6) 0.0255(3) Uani 1 1 d . . . N1 N 0.77171(17) 0.17384(9) 0.40207(7) 0.0185(3) Uani 1 1 d . . . N2 N 0.86275(18) 0.20108(9) 0.35816(7) 0.0189(3) Uani 1 1 d . . . N3 N 0.92332(16) 0.15510(8) 0.48892(7) 0.0172(3) Uani 1 1 d . . . N4 N 1.04906(17) 0.17153(9) 0.46095(7) 0.0184(4) Uani 1 1 d . . . N5 N 1.17733(18) 0.34866(9) 0.22808(7) 0.0202(4) Uani 1 1 d . . . C25 C 0.8195(2) 0.17807(11) 0.30237(9) 0.0208(4) Uani 1 1 d . . . H25 H 0.8631 0.1896 0.2634 0.025 Uiso 1 1 calc R . . C26 C 0.6997(2) 0.13409(11) 0.30891(9) 0.0207(4) Uani 1 1 d . . . C27 C 0.6139(2) 0.09456(11) 0.26724(10) 0.0278(5) Uani 1 1 d . . . H27 H 0.6282 0.0968 0.2230 0.033 Uiso 1 1 calc R . . C28 C 0.5097(2) 0.05300(12) 0.29250(11) 0.0335(5) Uani 1 1 d . . . H28 H 0.4516 0.0254 0.2653 0.040 Uiso 1 1 calc R . . C29 C 0.4864(2) 0.05021(12) 0.35822(11) 0.0326(5) Uani 1 1 d . . . H29 H 0.4142 0.0198 0.3740 0.039 Uiso 1 1 calc R . . C30 C 0.5643(2) 0.08996(12) 0.40015(11) 0.0253(5) Uani 1 1 d . . . H30 H 0.5460 0.0893 0.4441 0.030 Uiso 1 1 calc R . . C31 C 0.6722(2) 0.13144(11) 0.37416(9) 0.0194(4) Uani 1 1 d . . . C32 C 1.1459(2) 0.13015(10) 0.48639(9) 0.0186(4) Uani 1 1 d . . . H32 H 1.2430 0.1308 0.4756 0.022 Uiso 1 1 calc R . . C33 C 1.0848(2) 0.08451(10) 0.53210(8) 0.0174(4) Uani 1 1 d . . . C34 C 1.1355(2) 0.02981(10) 0.57203(9) 0.0200(4) Uani 1 1 d . . . H34 H 1.2324 0.0172 0.5724 0.024 Uiso 1 1 calc R . . C35 C 1.0409(2) -0.00458(11) 0.61018(9) 0.0213(4) Uani 1 1 d . . . H35 H 1.0727 -0.0417 0.6373 0.026 Uiso 1 1 calc R . . C36 C 0.8965(2) 0.01425(11) 0.60991(9) 0.0226(4) Uani 1 1 d . . . H36 H 0.8339 -0.0109 0.6369 0.027 Uiso 1 1 calc R . . C37 C 0.8435(2) 0.06767(11) 0.57188(9) 0.0197(4) Uani 1 1 d . . . H37 H 0.7468 0.0806 0.5724 0.024 Uiso 1 1 calc R . . C38 C 0.9410(2) 0.10182(10) 0.53237(8) 0.0165(4) Uani 1 1 d . . . C39 C 0.7967(2) 0.19078(11) 0.46781(8) 0.0177(4) Uani 1 1 d . . . H39A H 0.8071 0.2433 0.4730 0.021 Uiso 1 1 calc R . . H39B H 0.7156 0.1749 0.4935 0.021 Uiso 1 1 calc R . . C40 C 1.1541(2) 0.32511(11) 0.28559(9) 0.0217(4) Uani 1 1 d . . . H40 H 1.2094 0.3441 0.3189 0.026 Uiso 1 1 calc R . . C41 C 1.2853(2) 0.40281(12) 0.21625(10) 0.0288(5) Uani 1 1 d . . . H41A H 1.3377 0.4121 0.2552 0.043 Uiso 1 1 calc R . . H41B H 1.2406 0.4473 0.2019 0.043 Uiso 1 1 calc R . . H41C H 1.3502 0.3854 0.1838 0.043 Uiso 1 1 calc R . . C42 C 1.0969(2) 0.32163(12) 0.17448(9) 0.0262(5) Uani 1 1 d . . . H42A H 1.0509 0.2765 0.1861 0.039 Uiso 1 1 calc R . . H42B H 1.1606 0.3133 0.1389 0.039 Uiso 1 1 calc R . . H42C H 1.0254 0.3570 0.1625 0.039 Uiso 1 1 calc R . . 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 Cu1 0.02182(15) 0.02030(15) 0.01314(14) 0.00330(9) 0.00114(9) -0.00187(10) Cl1 0.0229(3) 0.0413(3) 0.0345(3) 0.0159(2) 0.0071(2) 0.0029(2) Cl2 0.0259(3) 0.0210(2) 0.0224(2) -0.00110(18) -0.00134(19) 0.0004(2) O1 0.0304(8) 0.0302(8) 0.0159(7) 0.0047(6) -0.0001(6) -0.0084(7) N1 0.0200(8) 0.0221(9) 0.0135(7) 0.0023(6) -0.0003(6) -0.0022(7) N2 0.0222(8) 0.0215(8) 0.0131(8) 0.0032(6) 0.0012(7) -0.0019(7) N3 0.0186(8) 0.0180(8) 0.0150(8) 0.0026(6) 0.0000(6) -0.0002(7) N4 0.0208(8) 0.0199(9) 0.0146(8) 0.0009(6) 0.0016(6) -0.0024(7) N5 0.0261(9) 0.0205(8) 0.0139(8) 0.0043(7) 0.0001(7) -0.0021(7) C25 0.0268(10) 0.0212(10) 0.0144(9) 0.0002(8) -0.0002(8) 0.0038(9) C26 0.0248(10) 0.0200(10) 0.0174(9) -0.0014(8) -0.0037(8) 0.0065(9) C27 0.0317(12) 0.0269(11) 0.0248(11) -0.0071(9) -0.0088(9) 0.0064(10) C28 0.0308(12) 0.0277(12) 0.0420(13) -0.0088(10) -0.0150(10) 0.0006(11) C29 0.0232(11) 0.0282(12) 0.0463(14) 0.0009(10) -0.0048(10) -0.0014(10) C30 0.0215(11) 0.0259(11) 0.0287(11) 0.0034(9) -0.0015(9) 0.0024(9) C31 0.0203(10) 0.0161(9) 0.0218(10) 0.0007(8) -0.0043(8) 0.0050(8) C32 0.0194(9) 0.0208(10) 0.0157(9) -0.0009(8) -0.0017(8) -0.0002(8) C33 0.0228(10) 0.0167(9) 0.0128(9) -0.0035(7) -0.0021(7) -0.0001(8) C34 0.0244(10) 0.0195(10) 0.0160(9) -0.0024(8) -0.0024(8) 0.0046(9) C35 0.0328(11) 0.0163(10) 0.0148(10) 0.0013(7) -0.0038(8) 0.0022(9) C36 0.0305(11) 0.0215(10) 0.0157(10) 0.0025(8) 0.0012(8) -0.0023(9) C37 0.0236(10) 0.0220(10) 0.0135(9) 0.0007(8) 0.0000(8) -0.0004(9) C38 0.0238(10) 0.0152(9) 0.0104(8) -0.0020(7) -0.0017(7) 0.0003(8) C39 0.0200(10) 0.0194(10) 0.0138(9) 0.0014(7) -0.0009(7) 0.0015(8) C40 0.0263(11) 0.0235(10) 0.0153(9) 0.0023(8) -0.0012(8) -0.0010(9) C41 0.0300(12) 0.0313(12) 0.0252(11) 0.0092(9) 0.0000(9) -0.0056(10) C42 0.0384(12) 0.0254(11) 0.0149(9) 0.0013(8) -0.0039(9) -0.0010(10) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Cu1 O1 1.9824(14) . ? Cu1 N4 2.0407(16) . ? Cu1 N2 2.0708(17) . ? Cu1 Cl1 2.2633(6) . ? Cu1 Cl2 2.4603(5) . ? O1 C40 1.250(2) . ? N1 C31 1.367(3) . ? N1 N2 1.369(2) . ? N1 C39 1.451(2) . ? N2 C25 1.326(2) . ? N3 C38 1.366(2) . ? N3 N4 1.368(2) . ? N3 C39 1.445(2) . ? N4 C32 1.316(3) . ? N5 C40 1.317(2) . ? N5 C42 1.461(3) . ? N5 C41 1.461(3) . ? C25 C26 1.409(3) . ? C25 H25 0.9500 . ? C26 C27 1.411(3) . ? C26 C31 1.411(3) . ? C27 C28 1.367(3) . ? C27 H27 0.9500 . ? C28 C29 1.415(3) . ? C28 H28 0.9500 . ? C29 C30 1.375(3) . ? C29 H29 0.9500 . ? C30 C31 1.397(3) . ? C30 H30 0.9500 . ? C32 C33 1.416(3) . ? C32 H32 0.9500 . ? C33 C38 1.403(3) . ? C33 C34 1.411(3) . ? C34 C35 1.369(3) . ? C34 H34 0.9500 . ? C35 C36 1.415(3) . ? C35 H35 0.9500 . ? C36 C37 1.378(3) . ? C36 H36 0.9500 . ? C37 C38 1.402(3) . ? C37 H37 0.9500 . ? C39 H39A 0.9900 . ? C39 H39B 0.9900 . ? C40 H40 0.9500 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? 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 O1 Cu1 N4 165.27(6) . . ? O1 Cu1 N2 83.77(6) . . ? N4 Cu1 N2 88.30(6) . . ? O1 Cu1 Cl1 90.40(5) . . ? N4 Cu1 Cl1 90.44(5) . . ? N2 Cu1 Cl1 150.58(5) . . ? O1 Cu1 Cl2 94.07(5) . . ? N4 Cu1 Cl2 99.47(5) . . ? N2 Cu1 Cl2 99.41(5) . . ? Cl1 Cu1 Cl2 109.79(2) . . ? C40 O1 Cu1 118.78(13) . . ? C31 N1 N2 110.81(15) . . ? C31 N1 C39 131.02(16) . . ? N2 N1 C39 118.11(16) . . ? C25 N2 N1 107.05(16) . . ? C25 N2 Cu1 129.09(14) . . ? N1 N2 Cu1 120.52(12) . . ? C38 N3 N4 110.43(15) . . ? C38 N3 C39 130.26(16) . . ? N4 N3 C39 119.21(15) . . ? C32 N4 N3 107.46(15) . . ? C32 N4 Cu1 130.28(13) . . ? N3 N4 Cu1 121.58(12) . . ? C40 N5 C42 121.37(17) . . ? C40 N5 C41 120.51(17) . . ? C42 N5 C41 118.12(16) . . ? N2 C25 C26 110.50(17) . . ? N2 C25 H25 124.7 . . ? C26 C25 H25 124.7 . . ? C25 C26 C27 135.1(2) . . ? C25 C26 C31 105.46(17) . . ? C27 C26 C31 119.42(19) . . ? C28 C27 C26 117.9(2) . . ? C28 C27 H27 121.1 . . ? C26 C27 H27 121.1 . . ? C27 C28 C29 121.4(2) . . ? C27 C28 H28 119.3 . . ? C29 C28 H28 119.3 . . ? C30 C29 C28 122.4(2) . . ? C30 C29 H29 118.8 . . ? C28 C29 H29 118.8 . . ? C29 C30 C31 115.9(2) . . ? C29 C30 H30 122.0 . . ? C31 C30 H30 122.0 . . ? N1 C31 C30 130.94(19) . . ? N1 C31 C26 106.13(17) . . ? C30 C31 C26 122.90(19) . . ? N4 C32 C33 110.33(17) . . ? N4 C32 H32 124.8 . . ? C33 C32 H32 124.8 . . ? C38 C33 C34 119.74(18) . . ? C38 C33 C32 105.29(17) . . ? C34 C33 C32 134.96(19) . . ? C35 C34 C33 118.04(19) . . ? C35 C34 H34 121.0 . . ? C33 C34 H34 121.0 . . ? C34 C35 C36 121.14(18) . . ? C34 C35 H35 119.4 . . ? C36 C35 H35 119.4 . . ? C37 C36 C35 122.39(19) . . ? C37 C36 H36 118.8 . . ? C35 C36 H36 118.8 . . ? C36 C37 C38 115.97(19) . . ? C36 C37 H37 122.0 . . ? C38 C37 H37 122.0 . . ? N3 C38 C37 130.81(18) . . ? N3 C38 C33 106.49(17) . . ? C37 C38 C33 122.70(18) . . ? N3 C39 N1 109.56(15) . . ? N3 C39 H39A 109.8 . . ? N1 C39 H39A 109.8 . . ? N3 C39 H39B 109.8 . . ? N1 C39 H39B 109.8 . . ? H39A C39 H39B 108.2 . . ? O1 C40 N5 123.44(19) . . ? O1 C40 H40 118.3 . . ? N5 C40 H40 118.3 . . ? N5 C41 H41A 109.5 . . ? N5 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? N5 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? N5 C42 H42A 109.5 . . ? N5 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? N5 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? 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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Cu1 O1 C40 -136.4(2) . . . . ? N2 Cu1 O1 C40 165.73(16) . . . . ? Cl1 Cu1 O1 C40 -43.17(15) . . . . ? Cl2 Cu1 O1 C40 66.70(15) . . . . ? C31 N1 N2 C25 1.8(2) . . . . ? C39 N1 N2 C25 179.48(17) . . . . ? C31 N1 N2 Cu1 -159.36(13) . . . . ? C39 N1 N2 Cu1 18.3(2) . . . . ? O1 Cu1 N2 C25 35.78(17) . . . . ? N4 Cu1 N2 C25 -131.78(18) . . . . ? Cl1 Cu1 N2 C25 -43.9(2) . . . . ? Cl2 Cu1 N2 C25 128.90(17) . . . . ? O1 Cu1 N2 N1 -167.63(15) . . . . ? N4 Cu1 N2 N1 24.80(14) . . . . ? Cl1 Cu1 N2 N1 112.69(14) . . . . ? Cl2 Cu1 N2 N1 -74.52(14) . . . . ? C38 N3 N4 C32 -0.6(2) . . . . ? C39 N3 N4 C32 -177.39(16) . . . . ? C38 N3 N4 Cu1 170.81(12) . . . . ? C39 N3 N4 Cu1 -5.9(2) . . . . ? O1 Cu1 N4 C32 80.8(3) . . . . ? N2 Cu1 N4 C32 138.12(17) . . . . ? Cl1 Cu1 N4 C32 -12.48(17) . . . . ? Cl2 Cu1 N4 C32 -122.63(17) . . . . ? O1 Cu1 N4 N3 -88.5(3) . . . . ? N2 Cu1 N4 N3 -31.16(14) . . . . ? Cl1 Cu1 N4 N3 178.25(14) . . . . ? Cl2 Cu1 N4 N3 68.10(14) . . . . ? N1 N2 C25 C26 -0.9(2) . . . . ? Cu1 N2 C25 C26 158.08(13) . . . . ? N2 C25 C26 C27 -178.0(2) . . . . ? N2 C25 C26 C31 -0.2(2) . . . . ? C25 C26 C27 C28 175.3(2) . . . . ? C31 C26 C27 C28 -2.2(3) . . . . ? C26 C27 C28 C29 0.9(3) . . . . ? C27 C28 C29 C30 1.5(4) . . . . ? C28 C29 C30 C31 -2.4(3) . . . . ? N2 N1 C31 C30 176.1(2) . . . . ? C39 N1 C31 C30 -1.2(4) . . . . ? N2 N1 C31 C26 -1.9(2) . . . . ? C39 N1 C31 C26 -179.21(19) . . . . ? C29 C30 C31 N1 -176.7(2) . . . . ? C29 C30 C31 C26 1.0(3) . . . . ? C25 C26 C31 N1 1.3(2) . . . . ? C27 C26 C31 N1 179.46(18) . . . . ? C25 C26 C31 C30 -176.92(19) . . . . ? C27 C26 C31 C30 1.3(3) . . . . ? N3 N4 C32 C33 0.4(2) . . . . ? Cu1 N4 C32 C33 -170.04(13) . . . . ? N4 C32 C33 C38 0.0(2) . . . . ? N4 C32 C33 C34 178.4(2) . . . . ? C38 C33 C34 C35 -0.2(3) . . . . ? C32 C33 C34 C35 -178.5(2) . . . . ? C33 C34 C35 C36 -0.3(3) . . . . ? C34 C35 C36 C37 -0.2(3) . . . . ? C35 C36 C37 C38 1.0(3) . . . . ? N4 N3 C38 C37 -179.66(19) . . . . ? C39 N3 C38 C37 -3.4(3) . . . . ? N4 N3 C38 C33 0.6(2) . . . . ? C39 N3 C38 C33 176.90(17) . . . . ? C36 C37 C38 N3 178.78(19) . . . . ? C36 C37 C38 C33 -1.5(3) . . . . ? C34 C33 C38 N3 -179.09(16) . . . . ? C32 C33 C38 N3 -0.3(2) . . . . ? C34 C33 C38 C37 1.1(3) . . . . ? C32 C33 C38 C37 179.89(17) . . . . ? C38 N3 C39 N1 -114.3(2) . . . . ? N4 N3 C39 N1 61.7(2) . . . . ? C31 N1 C39 N3 108.3(2) . . . . ? N2 N1 C39 N3 -68.8(2) . . . . ? Cu1 O1 C40 N5 170.67(16) . . . . ? C42 N5 C40 O1 -0.3(3) . . . . ? C41 N5 C40 O1 179.82(19) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.748 _refine_diff_density_min -0.375 _refine_diff_density_rms 0.059 data_11 _database_code_depnum_ccdc_archive 'CCDC 917670' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H24 Ag N8, N O3' _chemical_formula_sum 'C30 H24 Ag N9 O3' _chemical_formula_weight 666.45 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' 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.1130(3) _cell_length_b 12.0540(3) _cell_length_c 20.2158(5) _cell_angle_alpha 90.00 _cell_angle_beta 95.6670(10) _cell_angle_gamma 90.00 _cell_volume 2694.79(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7408 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 29.51 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.16 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.643 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.801 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8826 _exptl_absorpt_correction_T_max 0.8962 _exptl_absorpt_process_details ; APEX2 Software Suite; Bruker 2005. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker-Nonius X8kappa APEX II CCD area detector ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23453 _diffrn_reflns_av_R_equivalents 0.0317 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 25.25 _reflns_number_total 4695 _reflns_number_gt 3968 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker, 2007)' _computing_cell_refinement 'APEX2 Software Suite (Bruker, 2007)' _computing_data_reduction 'APEX2 Software Suite (Bruker, 2007)' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL and publCIF (Westrip, 2010)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0303P)^2^+1.6519P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4695 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0358 _refine_ls_R_factor_gt 0.0273 _refine_ls_wR_factor_ref 0.0663 _refine_ls_wR_factor_gt 0.0634 _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.903776(17) 0.182135(17) 0.081147(9) 0.03084(8) Uani 1 1 d . . . N1 N 0.75570(16) 0.12658(15) -0.05766(9) 0.0207(4) Uani 1 1 d . . . N2 N 0.86822(16) 0.11045(15) -0.02465(9) 0.0222(4) Uani 1 1 d . . . N3 N 0.66429(17) 0.27823(16) -0.00403(9) 0.0226(4) Uani 1 1 d . . . N4 N 0.74061(18) 0.31269(17) 0.04924(10) 0.0271(5) Uani 1 1 d . . . N5 N 1.17182(17) 0.22723(16) 0.15769(9) 0.0225(4) Uani 1 1 d . . . N6 N 1.11987(17) 0.21099(16) 0.09407(9) 0.0251(4) Uani 1 1 d . . . N7 N 1.01884(17) 0.20038(15) 0.23327(9) 0.0214(4) Uani 1 1 d . . . N8 N 0.91740(17) 0.16654(16) 0.19461(10) 0.0256(4) Uani 1 1 d . . . C1 C 0.9414(2) 0.08703(18) -0.07032(11) 0.0220(5) Uani 1 1 d . . . H1 H 1.0251 0.0713 -0.0611 0.026 Uiso 1 1 calc R . . C2 C 0.8787(2) 0.08842(18) -0.13480(11) 0.0211(5) Uani 1 1 d . . . C3 C 0.9106(2) 0.06976(19) -0.19954(12) 0.0278(6) Uani 1 1 d . . . H3 H 0.9908 0.0496 -0.2071 0.033 Uiso 1 1 calc R . . C4 C 0.8227(3) 0.0815(2) -0.25114(13) 0.0334(6) Uani 1 1 d . . . H4 H 0.8423 0.0699 -0.2953 0.040 Uiso 1 1 calc R . . C5 C 0.7033(3) 0.1105(2) -0.24022(13) 0.0343(6) Uani 1 1 d . . . H5 H 0.6449 0.1194 -0.2775 0.041 Uiso 1 1 calc R . . C6 C 0.6686(2) 0.12636(19) -0.17761(12) 0.0279(6) Uani 1 1 d . . . H6 H 0.5875 0.1437 -0.1705 0.033 Uiso 1 1 calc R . . C7 C 0.7589(2) 0.11569(17) -0.12493(11) 0.0208(5) Uani 1 1 d . . . C8 C 0.7411(2) 0.4217(2) 0.04691(12) 0.0292(6) Uani 1 1 d . . . H8 H 0.7857 0.4676 0.0788 0.035 Uiso 1 1 calc R . . C9 C 0.6670(2) 0.4626(2) -0.00881(12) 0.0249(5) Uani 1 1 d . . . C10 C 0.6356(2) 0.5676(2) -0.03571(13) 0.0315(6) Uani 1 1 d . . . H10 H 0.6652 0.6335 -0.0141 0.038 Uiso 1 1 calc R . . C11 C 0.5615(2) 0.5724(2) -0.09366(13) 0.0339(6) Uani 1 1 d . . . H11 H 0.5409 0.6425 -0.1131 0.041 Uiso 1 1 calc R . . C12 C 0.5151(2) 0.4752(2) -0.12508(13) 0.0351(6) Uani 1 1 d . . . H12 H 0.4637 0.4815 -0.1653 0.042 Uiso 1 1 calc R . . C13 C 0.5415(2) 0.3713(2) -0.09966(12) 0.0302(6) Uani 1 1 d . . . H13 H 0.5081 0.3060 -0.1205 0.036 Uiso 1 1 calc R . . C14 C 0.6202(2) 0.36733(19) -0.04141(11) 0.0221(5) Uani 1 1 d . . . C15 C 0.6579(2) 0.16172(18) -0.02076(12) 0.0232(5) Uani 1 1 d . . . H15A H 0.6598 0.1177 0.0207 0.028 Uiso 1 1 calc R . . H15B H 0.5801 0.1466 -0.0474 0.028 Uiso 1 1 calc R . . C16 C 1.2042(2) 0.16628(19) 0.06090(12) 0.0234(5) Uani 1 1 d . . . H16 H 1.1927 0.1456 0.0154 0.028 Uiso 1 1 calc R . . C17 C 1.3136(2) 0.15326(18) 0.10184(11) 0.0210(5) Uani 1 1 d . . . C18 C 1.4306(2) 0.11519(19) 0.09239(12) 0.0249(5) Uani 1 1 d . . . H18 H 1.4487 0.0875 0.0505 0.030 Uiso 1 1 calc R . . C19 C 1.5173(2) 0.1194(2) 0.14534(13) 0.0290(6) Uani 1 1 d . . . H19 H 1.5970 0.0949 0.1399 0.035 Uiso 1 1 calc R . . C20 C 1.4909(2) 0.1593(2) 0.20787(13) 0.0299(6) Uani 1 1 d . . . H20 H 1.5534 0.1606 0.2435 0.036 Uiso 1 1 calc R . . C21 C 1.3780(2) 0.19635(19) 0.21883(12) 0.0254(5) Uani 1 1 d . . . H21 H 1.3606 0.2228 0.2611 0.030 Uiso 1 1 calc R . . C22 C 1.2897(2) 0.19310(17) 0.16443(11) 0.0201(5) Uani 1 1 d . . . C23 C 0.8501(2) 0.1129(2) 0.23411(12) 0.0272(5) Uani 1 1 d . . . H23 H 0.7747 0.0791 0.2199 0.033 Uiso 1 1 calc R . . C24 C 0.9042(2) 0.11193(19) 0.30047(12) 0.0243(5) Uani 1 1 d . . . C25 C 0.8717(2) 0.0713(2) 0.36156(13) 0.0317(6) Uani 1 1 d . . . H25 H 0.7982 0.0319 0.3641 0.038 Uiso 1 1 calc R . . C26 C 0.9493(2) 0.0904(2) 0.41704(13) 0.0344(6) Uani 1 1 d . . . H26 H 0.9289 0.0644 0.4589 0.041 Uiso 1 1 calc R . . C27 C 1.0585(2) 0.1474(2) 0.41370(13) 0.0318(6) Uani 1 1 d . . . H27 H 1.1097 0.1591 0.4535 0.038 Uiso 1 1 calc R . . C28 C 1.0940(2) 0.18711(19) 0.35497(12) 0.0260(5) Uani 1 1 d . . . H28 H 1.1690 0.2242 0.3530 0.031 Uiso 1 1 calc R . . C29 C 1.0139(2) 0.16996(18) 0.29830(11) 0.0211(5) Uani 1 1 d . . . C30 C 1.1014(2) 0.27725(19) 0.20602(11) 0.0228(5) Uani 1 1 d . . . H30A H 1.0544 0.3398 0.1849 0.027 Uiso 1 1 calc R . . H30B H 1.1570 0.3078 0.2428 0.027 Uiso 1 1 calc R . . O1 O 0.3101(2) 0.3809(2) 0.32780(11) 0.0697(8) Uani 1 1 d . . . O2 O 0.2311(2) 0.46491(18) 0.40479(13) 0.0676(7) Uani 1 1 d . . . O3 O 0.3737(2) 0.3555(4) 0.42756(15) 0.1175(14) Uani 1 1 d . . . N9 N 0.30481(17) 0.40036(16) 0.38686(10) 0.0251(4) 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 0.02542(12) 0.04558(13) 0.01989(11) -0.00057(9) -0.00587(8) 0.00385(8) N1 0.0162(10) 0.0255(10) 0.0195(10) 0.0004(8) -0.0023(8) 0.0001(7) N2 0.0179(10) 0.0274(11) 0.0204(10) 0.0033(8) -0.0026(8) -0.0007(8) N3 0.0209(10) 0.0267(10) 0.0194(11) -0.0010(8) -0.0015(8) 0.0024(8) N4 0.0243(11) 0.0359(12) 0.0201(11) -0.0003(9) -0.0020(9) -0.0004(9) N5 0.0188(10) 0.0309(11) 0.0176(10) -0.0034(8) 0.0013(8) 0.0012(8) N6 0.0215(11) 0.0350(12) 0.0183(11) -0.0004(9) -0.0014(9) -0.0020(8) N7 0.0190(10) 0.0262(11) 0.0188(10) -0.0028(8) 0.0008(8) -0.0007(8) N8 0.0174(10) 0.0363(12) 0.0221(11) -0.0043(9) -0.0035(8) -0.0004(8) C1 0.0180(12) 0.0235(12) 0.0244(13) 0.0029(10) 0.0016(10) -0.0003(9) C2 0.0240(12) 0.0165(11) 0.0229(13) 0.0020(9) 0.0027(10) -0.0030(9) C3 0.0361(15) 0.0212(12) 0.0275(14) 0.0007(10) 0.0100(12) -0.0028(10) C4 0.0514(17) 0.0280(13) 0.0207(14) -0.0032(11) 0.0038(12) -0.0044(12) C5 0.0476(17) 0.0268(14) 0.0252(14) -0.0037(11) -0.0121(12) -0.0053(11) C6 0.0283(14) 0.0255(13) 0.0280(14) -0.0023(11) -0.0064(11) -0.0001(10) C7 0.0245(13) 0.0161(11) 0.0212(13) 0.0015(9) -0.0009(10) -0.0041(9) C8 0.0262(14) 0.0335(15) 0.0272(14) -0.0042(11) -0.0009(11) -0.0016(10) C9 0.0206(12) 0.0305(13) 0.0240(13) -0.0014(10) 0.0034(10) 0.0015(10) C10 0.0306(14) 0.0293(14) 0.0353(15) -0.0008(11) 0.0074(12) 0.0001(10) C11 0.0373(15) 0.0321(14) 0.0326(15) 0.0090(12) 0.0051(12) 0.0115(11) C12 0.0369(15) 0.0409(16) 0.0260(14) 0.0002(12) -0.0046(12) 0.0141(12) C13 0.0282(14) 0.0361(14) 0.0252(14) -0.0037(11) -0.0030(11) 0.0080(11) C14 0.0162(12) 0.0284(12) 0.0220(13) -0.0003(10) 0.0034(10) 0.0036(9) C15 0.0169(12) 0.0281(13) 0.0248(13) 0.0035(10) 0.0037(10) 0.0001(9) C16 0.0244(13) 0.0294(13) 0.0164(12) -0.0019(10) 0.0019(10) -0.0035(10) C17 0.0228(12) 0.0208(12) 0.0197(12) 0.0003(9) 0.0030(10) -0.0025(9) C18 0.0262(13) 0.0236(12) 0.0260(13) -0.0021(10) 0.0077(10) 0.0004(9) C19 0.0217(13) 0.0317(14) 0.0339(15) 0.0008(11) 0.0040(11) 0.0058(10) C20 0.0232(13) 0.0344(14) 0.0307(15) 0.0034(11) -0.0050(11) 0.0026(10) C21 0.0259(13) 0.0297(13) 0.0202(13) -0.0020(10) 0.0001(10) 0.0008(10) C22 0.0190(12) 0.0194(11) 0.0222(12) 0.0004(9) 0.0031(10) -0.0003(9) C23 0.0161(12) 0.0384(14) 0.0269(14) -0.0048(11) 0.0012(10) -0.0012(10) C24 0.0180(12) 0.0287(13) 0.0262(13) -0.0034(10) 0.0029(10) 0.0026(9) C25 0.0276(14) 0.0380(15) 0.0308(15) 0.0026(12) 0.0098(11) 0.0017(11) C26 0.0383(16) 0.0429(15) 0.0229(14) 0.0052(12) 0.0077(12) 0.0078(12) C27 0.0350(15) 0.0372(14) 0.0216(13) -0.0027(11) -0.0053(11) 0.0093(11) C28 0.0250(13) 0.0262(13) 0.0258(14) -0.0045(10) -0.0017(11) 0.0027(10) C29 0.0200(12) 0.0227(12) 0.0207(12) -0.0038(10) 0.0026(10) 0.0059(9) C30 0.0207(12) 0.0260(12) 0.0217(13) -0.0039(10) 0.0027(10) 0.0004(9) O1 0.101(2) 0.0736(17) 0.0385(13) -0.0292(12) 0.0290(13) -0.0425(14) O2 0.0721(16) 0.0468(13) 0.0934(19) 0.0156(12) 0.0551(15) 0.0251(12) O3 0.0458(17) 0.225(4) 0.081(2) 0.077(2) 0.0039(15) 0.048(2) N9 0.0209(11) 0.0294(11) 0.0249(12) -0.0022(9) 0.0022(9) -0.0031(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N8 2.292(2) . ? Ag1 N2 2.3045(19) . ? Ag1 N6 2.4150(19) . ? Ag1 N4 2.439(2) . ? N1 C7 1.370(3) . ? N1 N2 1.372(3) . ? N1 C15 1.441(3) . ? N2 C1 1.320(3) . ? N3 N4 1.368(3) . ? N3 C14 1.375(3) . ? N3 C15 1.445(3) . ? N4 C8 1.315(3) . ? N5 C22 1.367(3) . ? N5 N6 1.371(3) . ? N5 C30 1.443(3) . ? N6 C16 1.320(3) . ? N7 N8 1.369(3) . ? N7 C29 1.371(3) . ? N7 C30 1.450(3) . ? N8 C23 1.317(3) . ? C1 C2 1.416(3) . ? C1 H1 0.9500 . ? C2 C7 1.404(3) . ? C2 C3 1.407(3) . ? C3 C4 1.364(4) . ? C3 H3 0.9500 . ? C4 C5 1.411(4) . ? C4 H4 0.9500 . ? C5 C6 1.372(4) . ? C5 H5 0.9500 . ? C6 C7 1.395(3) . ? C6 H6 0.9500 . ? C8 C9 1.416(3) . ? C8 H8 0.9500 . ? C9 C14 1.398(3) . ? C9 C10 1.408(3) . ? C10 C11 1.365(4) . ? C10 H10 0.9500 . ? C11 C12 1.406(4) . ? C11 H11 0.9500 . ? C12 C13 1.374(4) . ? C12 H12 0.9500 . ? C13 C14 1.397(3) . ? C13 H13 0.9500 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.410(3) . ? C16 H16 0.9500 . ? C17 C22 1.403(3) . ? C17 C18 1.410(3) . ? C18 C19 1.369(3) . ? C18 H18 0.9500 . ? C19 C20 1.410(3) . ? C19 H19 0.9500 . ? C20 C21 1.370(3) . ? C20 H20 0.9500 . ? C21 C22 1.400(3) . ? C21 H21 0.9500 . ? C23 C24 1.415(3) . ? C23 H23 0.9500 . ? C24 C25 1.409(3) . ? C24 C29 1.409(3) . ? C25 C26 1.366(4) . ? C25 H25 0.9500 . ? C26 C27 1.401(4) . ? C26 H26 0.9500 . ? C27 C28 1.374(3) . ? C27 H27 0.9500 . ? C28 C29 1.395(3) . ? C28 H28 0.9500 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? O1 N9 1.224(3) . ? O2 N9 1.211(3) . ? O3 N9 1.196(3) . ? 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 N8 Ag1 N2 152.45(7) . . ? N8 Ag1 N6 86.38(7) . . ? N2 Ag1 N6 103.41(6) . . ? N8 Ag1 N4 106.95(7) . . ? N2 Ag1 N4 86.66(7) . . ? N6 Ag1 N4 129.87(7) . . ? C7 N1 N2 110.93(18) . . ? C7 N1 C15 129.6(2) . . ? N2 N1 C15 119.18(18) . . ? C1 N2 N1 106.56(18) . . ? C1 N2 Ag1 131.95(15) . . ? N1 N2 Ag1 117.57(13) . . ? N4 N3 C14 110.80(19) . . ? N4 N3 C15 119.45(19) . . ? C14 N3 C15 128.6(2) . . ? C8 N4 N3 106.22(19) . . ? C8 N4 Ag1 130.46(16) . . ? N3 N4 Ag1 113.53(14) . . ? C22 N5 N6 111.18(18) . . ? C22 N5 C30 129.56(19) . . ? N6 N5 C30 119.25(18) . . ? C16 N6 N5 106.30(18) . . ? C16 N6 Ag1 129.38(16) . . ? N5 N6 Ag1 116.38(13) . . ? N8 N7 C29 111.02(18) . . ? N8 N7 C30 119.32(19) . . ? C29 N7 C30 128.5(2) . . ? C23 N8 N7 106.58(19) . . ? C23 N8 Ag1 131.45(16) . . ? N7 N8 Ag1 121.08(14) . . ? N2 C1 C2 111.1(2) . . ? N2 C1 H1 124.4 . . ? C2 C1 H1 124.4 . . ? C7 C2 C3 119.9(2) . . ? C7 C2 C1 105.00(19) . . ? C3 C2 C1 135.1(2) . . ? C4 C3 C2 117.9(2) . . ? C4 C3 H3 121.1 . . ? C2 C3 H3 121.1 . . ? C3 C4 C5 121.3(2) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C6 C5 C4 122.2(2) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C5 C6 C7 116.4(2) . . ? C5 C6 H6 121.8 . . ? C7 C6 H6 121.8 . . ? N1 C7 C6 131.4(2) . . ? N1 C7 C2 106.4(2) . . ? C6 C7 C2 122.3(2) . . ? N4 C8 C9 111.8(2) . . ? N4 C8 H8 124.1 . . ? C9 C8 H8 124.1 . . ? C14 C9 C10 119.3(2) . . ? C14 C9 C8 104.4(2) . . ? C10 C9 C8 136.2(2) . . ? C11 C10 C9 118.4(2) . . ? C11 C10 H10 120.8 . . ? C9 C10 H10 120.8 . . ? C10 C11 C12 121.0(2) . . ? C10 C11 H11 119.5 . . ? C12 C11 H11 119.5 . . ? C13 C12 C11 122.4(2) . . ? C13 C12 H12 118.8 . . ? C11 C12 H12 118.8 . . ? C12 C13 C14 116.0(2) . . ? C12 C13 H13 122.0 . . ? C14 C13 H13 122.0 . . ? N3 C14 C13 130.5(2) . . ? N3 C14 C9 106.7(2) . . ? C13 C14 C9 122.8(2) . . ? N1 C15 N3 112.65(18) . . ? N1 C15 H15A 109.1 . . ? N3 C15 H15A 109.1 . . ? N1 C15 H15B 109.1 . . ? N3 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? N6 C16 C17 111.2(2) . . ? N6 C16 H16 124.4 . . ? C17 C16 H16 124.4 . . ? C22 C17 C18 119.5(2) . . ? C22 C17 C16 105.20(19) . . ? C18 C17 C16 135.2(2) . . ? C19 C18 C17 118.0(2) . . ? C19 C18 H18 121.0 . . ? C17 C18 H18 121.0 . . ? C18 C19 C20 121.4(2) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C21 C20 C19 122.1(2) . . ? C21 C20 H20 119.0 . . ? C19 C20 H20 119.0 . . ? C20 C21 C22 116.5(2) . . ? C20 C21 H21 121.8 . . ? C22 C21 H21 121.8 . . ? N5 C22 C21 131.3(2) . . ? N5 C22 C17 106.1(2) . . ? C21 C22 C17 122.5(2) . . ? N8 C23 C24 111.4(2) . . ? N8 C23 H23 124.3 . . ? C24 C23 H23 124.3 . . ? C25 C24 C29 119.9(2) . . ? C25 C24 C23 135.4(2) . . ? C29 C24 C23 104.7(2) . . ? C26 C25 C24 117.7(2) . . ? C26 C25 H25 121.1 . . ? C24 C25 H25 121.1 . . ? C25 C26 C27 121.5(2) . . ? C25 C26 H26 119.2 . . ? C27 C26 H26 119.2 . . ? C28 C27 C26 122.4(2) . . ? C28 C27 H27 118.8 . . ? C26 C27 H27 118.8 . . ? C27 C28 C29 116.3(2) . . ? C27 C28 H28 121.8 . . ? C29 C28 H28 121.8 . . ? N7 C29 C28 131.7(2) . . ? N7 C29 C24 106.2(2) . . ? C28 C29 C24 122.1(2) . . ? N5 C30 N7 113.33(18) . . ? N5 C30 H30A 108.9 . . ? N7 C30 H30A 108.9 . . ? N5 C30 H30B 108.9 . . ? N7 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? O3 N9 O2 119.4(3) . . ? O3 N9 O1 119.7(3) . . ? O2 N9 O1 121.0(3) . . ? 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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 N1 N2 C1 -1.4(2) . . . . ? C15 N1 N2 C1 -175.45(19) . . . . ? C7 N1 N2 Ag1 158.97(14) . . . . ? C15 N1 N2 Ag1 -15.1(2) . . . . ? N8 Ag1 N2 C1 -107.9(2) . . . . ? N6 Ag1 N2 C1 0.6(2) . . . . ? N4 Ag1 N2 C1 130.8(2) . . . . ? N8 Ag1 N2 N1 97.73(19) . . . . ? N6 Ag1 N2 N1 -153.81(14) . . . . ? N4 Ag1 N2 N1 -23.56(15) . . . . ? C14 N3 N4 C8 2.3(2) . . . . ? C15 N3 N4 C8 171.07(19) . . . . ? C14 N3 N4 Ag1 -147.47(14) . . . . ? C15 N3 N4 Ag1 21.3(2) . . . . ? N8 Ag1 N4 C8 84.4(2) . . . . ? N2 Ag1 N4 C8 -120.0(2) . . . . ? N6 Ag1 N4 C8 -15.3(2) . . . . ? N8 Ag1 N4 N3 -135.11(14) . . . . ? N2 Ag1 N4 N3 20.48(15) . . . . ? N6 Ag1 N4 N3 125.19(14) . . . . ? C22 N5 N6 C16 0.3(2) . . . . ? C30 N5 N6 C16 179.04(19) . . . . ? C22 N5 N6 Ag1 152.32(14) . . . . ? C30 N5 N6 Ag1 -29.0(2) . . . . ? N8 Ag1 N6 C16 133.9(2) . . . . ? N2 Ag1 N6 C16 -20.0(2) . . . . ? N4 Ag1 N6 C16 -117.0(2) . . . . ? N8 Ag1 N6 N5 -10.39(15) . . . . ? N2 Ag1 N6 N5 -164.32(15) . . . . ? N4 Ag1 N6 N5 98.73(16) . . . . ? C29 N7 N8 C23 -1.5(2) . . . . ? C30 N7 N8 C23 -170.05(19) . . . . ? C29 N7 N8 Ag1 -171.93(14) . . . . ? C30 N7 N8 Ag1 19.5(2) . . . . ? N2 Ag1 N8 C23 -40.4(3) . . . . ? N6 Ag1 N8 C23 -152.8(2) . . . . ? N4 Ag1 N8 C23 76.5(2) . . . . ? N2 Ag1 N8 N7 127.28(17) . . . . ? N6 Ag1 N8 N7 14.87(16) . . . . ? N4 Ag1 N8 N7 -115.83(16) . . . . ? N1 N2 C1 C2 0.7(2) . . . . ? Ag1 N2 C1 C2 -155.78(15) . . . . ? N2 C1 C2 C7 0.3(2) . . . . ? N2 C1 C2 C3 -179.7(2) . . . . ? C7 C2 C3 C4 1.4(3) . . . . ? C1 C2 C3 C4 -178.5(2) . . . . ? C2 C3 C4 C5 -0.5(4) . . . . ? C3 C4 C5 C6 -1.3(4) . . . . ? C4 C5 C6 C7 2.0(4) . . . . ? N2 N1 C7 C6 -178.9(2) . . . . ? C15 N1 C7 C6 -5.7(4) . . . . ? N2 N1 C7 C2 1.6(2) . . . . ? C15 N1 C7 C2 174.8(2) . . . . ? C5 C6 C7 N1 179.5(2) . . . . ? C5 C6 C7 C2 -1.0(3) . . . . ? C3 C2 C7 N1 178.90(19) . . . . ? C1 C2 C7 N1 -1.1(2) . . . . ? C3 C2 C7 C6 -0.6(3) . . . . ? C1 C2 C7 C6 179.3(2) . . . . ? N3 N4 C8 C9 -1.2(3) . . . . ? Ag1 N4 C8 C9 141.37(17) . . . . ? N4 C8 C9 C14 -0.2(3) . . . . ? N4 C8 C9 C10 -179.1(3) . . . . ? C14 C9 C10 C11 -1.0(3) . . . . ? C8 C9 C10 C11 177.8(3) . . . . ? C9 C10 C11 C12 1.5(4) . . . . ? C10 C11 C12 C13 -0.1(4) . . . . ? C11 C12 C13 C14 -1.7(4) . . . . ? N4 N3 C14 C13 179.4(2) . . . . ? C15 N3 C14 C13 11.9(4) . . . . ? N4 N3 C14 C9 -2.4(2) . . . . ? C15 N3 C14 C9 -169.9(2) . . . . ? C12 C13 C14 N3 -179.8(2) . . . . ? C12 C13 C14 C9 2.2(4) . . . . ? C10 C9 C14 N3 -179.3(2) . . . . ? C8 C9 C14 N3 1.5(2) . . . . ? C10 C9 C14 C13 -0.9(3) . . . . ? C8 C9 C14 C13 179.9(2) . . . . ? C7 N1 C15 N3 -96.0(3) . . . . ? N2 N1 C15 N3 76.7(2) . . . . ? N4 N3 C15 N1 -80.5(2) . . . . ? C14 N3 C15 N1 86.1(3) . . . . ? N5 N6 C16 C17 -0.6(3) . . . . ? Ag1 N6 C16 C17 -147.61(16) . . . . ? N6 C16 C17 C22 0.6(3) . . . . ? N6 C16 C17 C18 -177.2(2) . . . . ? C22 C17 C18 C19 -0.4(3) . . . . ? C16 C17 C18 C19 177.2(2) . . . . ? C17 C18 C19 C20 0.7(4) . . . . ? C18 C19 C20 C21 -0.3(4) . . . . ? C19 C20 C21 C22 -0.3(3) . . . . ? N6 N5 C22 C21 178.0(2) . . . . ? C30 N5 C22 C21 -0.5(4) . . . . ? N6 N5 C22 C17 0.0(2) . . . . ? C30 N5 C22 C17 -178.5(2) . . . . ? C20 C21 C22 N5 -177.0(2) . . . . ? C20 C21 C22 C17 0.6(3) . . . . ? C18 C17 C22 N5 177.87(19) . . . . ? C16 C17 C22 N5 -0.4(2) . . . . ? C18 C17 C22 C21 -0.3(3) . . . . ? C16 C17 C22 C21 -178.5(2) . . . . ? N7 N8 C23 C24 1.3(3) . . . . ? Ag1 N8 C23 C24 170.32(15) . . . . ? N8 C23 C24 C25 177.5(3) . . . . ? N8 C23 C24 C29 -0.6(3) . . . . ? C29 C24 C25 C26 0.0(3) . . . . ? C23 C24 C25 C26 -177.9(3) . . . . ? C24 C25 C26 C27 -0.6(4) . . . . ? C25 C26 C27 C28 -0.2(4) . . . . ? C26 C27 C28 C29 1.5(4) . . . . ? N8 N7 C29 C28 -179.1(2) . . . . ? C30 N7 C29 C28 -11.9(4) . . . . ? N8 N7 C29 C24 1.1(2) . . . . ? C30 N7 C29 C24 168.3(2) . . . . ? C27 C28 C29 N7 178.2(2) . . . . ? C27 C28 C29 C24 -2.1(3) . . . . ? C25 C24 C29 N7 -178.8(2) . . . . ? C23 C24 C29 N7 -0.3(2) . . . . ? C25 C24 C29 C28 1.4(3) . . . . ? C23 C24 C29 C28 179.9(2) . . . . ? C22 N5 C30 N7 -102.5(3) . . . . ? N6 N5 C30 N7 79.1(3) . . . . ? N8 N7 C30 N5 -73.0(2) . . . . ? C29 N7 C30 N5 120.7(2) . . . . ? _diffrn_measured_fraction_theta_max 0.985 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.985 _refine_diff_density_max 0.544 _refine_diff_density_min -0.462 _refine_diff_density_rms 0.057 data_12 _database_code_depnum_ccdc_archive 'CCDC 917671' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H24 Ag N9 O3' _chemical_formula_sum 'C30 H24 Ag N9 O3' _chemical_formula_weight 666.45 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' 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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 13.0088(7) _cell_length_b 15.4845(8) _cell_length_c 14.3809(8) _cell_angle_alpha 90.00 _cell_angle_beta 106.056(2) _cell_angle_gamma 90.00 _cell_volume 2783.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9901 _cell_measurement_theta_min 2.63 _cell_measurement_theta_max 30.41 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.48 _exptl_crystal_size_min 0.45 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1352 _exptl_absorpt_coefficient_mu 0.775 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6979 _exptl_absorpt_correction_T_max 0.7218 _exptl_absorpt_process_details ; APEX2 Software Suite; Bruker 2005. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker-Nonius X8kappa APEX II CCD area detector ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 34239 _diffrn_reflns_av_R_equivalents 0.0392 _diffrn_reflns_av_sigmaI/netI 0.0381 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -19 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.98 _diffrn_reflns_theta_max 30.62 _reflns_number_total 8364 _reflns_number_gt 6188 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker, 2007)' _computing_cell_refinement 'APEX2 Software Suite (Bruker, 2007)' _computing_data_reduction 'APEX2 Software Suite (Bruker, 2007)' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL and publCIF (Westrip, 2010)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0505P)^2^+1.1150P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8364 _refine_ls_number_parameters 388 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0538 _refine_ls_R_factor_gt 0.0377 _refine_ls_wR_factor_ref 0.1016 _refine_ls_wR_factor_gt 0.0928 _refine_ls_goodness_of_fit_ref 1.049 _refine_ls_restrained_S_all 1.049 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.444034(14) 0.133757(11) 0.047643(12) 0.03412(7) Uani 1 1 d . . . O1 O 0.47528(16) 0.28224(10) 0.12426(12) 0.0410(4) Uani 1 1 d . . . O2 O 0.54593(15) 0.40448(12) 0.10660(14) 0.0469(4) Uani 1 1 d . . . O3 O 0.42014(19) 0.35313(14) -0.00998(14) 0.0572(6) Uani 1 1 d . . . N1 N 0.57145(14) 0.14846(12) -0.02841(13) 0.0269(4) Uani 1 1 d . . . N2 N 0.55163(13) 0.13960(10) -0.12622(13) 0.0239(3) Uani 1 1 d . . . N3 N 0.32085(15) 0.15051(14) -0.11132(14) 0.0357(4) Uani 1 1 d . . . N4 N 0.35972(14) 0.14447(11) -0.18943(13) 0.0260(4) Uani 1 1 d . . . N5 N 0.36254(13) 0.07991(11) 0.14933(12) 0.0248(3) Uani 1 1 d . . . N6 N 0.38952(13) 0.09166(11) 0.24736(12) 0.0237(3) Uani 1 1 d . . . N7 N 0.64005(15) 0.09550(12) 0.25591(13) 0.0301(4) Uani 1 1 d . . . N8 N 0.58037(13) 0.09705(11) 0.31998(12) 0.0228(3) Uani 1 1 d . . . N9 N 0.48081(16) 0.34696(12) 0.07279(14) 0.0285(4) Uani 1 1 d . . . C1 C 0.62696(16) 0.17650(14) -0.16157(16) 0.0272(4) Uani 1 1 d . . . H1 H 0.6288 0.1770 -0.2271 0.033 Uiso 1 1 calc R . . C2 C 0.70095(16) 0.21340(13) -0.08352(16) 0.0271(4) Uani 1 1 d . . . C3 C 0.79746(17) 0.26043(15) -0.0714(2) 0.0374(5) Uani 1 1 d . . . H3 H 0.8238 0.2739 -0.1250 0.045 Uiso 1 1 calc R . . C4 C 0.85077(19) 0.28543(16) 0.0200(2) 0.0441(6) Uani 1 1 d . . . H4 H 0.9159 0.3164 0.0299 0.053 Uiso 1 1 calc R . . C5 C 0.81226(19) 0.26676(16) 0.1012(2) 0.0417(6) Uani 1 1 d . . . H5 H 0.8523 0.2859 0.1634 0.050 Uiso 1 1 calc R . . C6 C 0.71942(17) 0.22215(15) 0.09260(17) 0.0340(5) Uani 1 1 d . . . H6 H 0.6939 0.2101 0.1471 0.041 Uiso 1 1 calc R . . C7 C 0.66301(15) 0.19480(13) -0.00212(15) 0.0249(4) Uani 1 1 d . . . C8 C 0.30196(17) 0.18821(14) -0.26744(16) 0.0312(4) Uani 1 1 d . . . H8 H 0.3156 0.1919 -0.3289 0.037 Uiso 1 1 calc R . . C9 C 0.21814(17) 0.22705(14) -0.23984(17) 0.0322(5) Uani 1 1 d . . . C10 C 0.1313(2) 0.28061(17) -0.2860(2) 0.0492(7) Uani 1 1 d . . . H10 H 0.1202 0.2973 -0.3516 0.059 Uiso 1 1 calc R . . C11 C 0.0643(2) 0.30768(19) -0.2352(3) 0.0567(8) Uani 1 1 d . . . H11 H 0.0051 0.3434 -0.2655 0.068 Uiso 1 1 calc R . . C12 C 0.0815(2) 0.2833(2) -0.1366(3) 0.0634(9) Uani 1 1 d . . . H12 H 0.0334 0.3039 -0.1025 0.076 Uiso 1 1 calc R . . C13 C 0.1638(2) 0.2317(2) -0.0894(2) 0.0564(8) Uani 1 1 d . . . H13 H 0.1737 0.2159 -0.0236 0.068 Uiso 1 1 calc R . . C14 C 0.23436(17) 0.20234(16) -0.14217(17) 0.0347(5) Uani 1 1 d . . . C15 C 0.45617(16) 0.09423(14) -0.18091(16) 0.0284(4) Uani 1 1 d . . . H15A H 0.4627 0.0811 -0.2464 0.034 Uiso 1 1 calc R . . H15B H 0.4505 0.0387 -0.1485 0.034 Uiso 1 1 calc R . . C16 C 0.32234(17) 0.05229(13) 0.28971(16) 0.0288(4) Uani 1 1 d . . . H16 H 0.3265 0.0524 0.3567 0.035 Uiso 1 1 calc R . . C17 C 0.24536(16) 0.01123(13) 0.21618(17) 0.0285(4) Uani 1 1 d . . . C18 C 0.15313(18) -0.03934(15) 0.2117(2) 0.0399(6) Uani 1 1 d . . . H18 H 0.1334 -0.0531 0.2689 0.048 Uiso 1 1 calc R . . C19 C 0.09384(19) -0.06757(16) 0.1240(2) 0.0462(6) Uani 1 1 d . . . H19 H 0.0318 -0.1013 0.1199 0.055 Uiso 1 1 calc R . . C20 C 0.12298(18) -0.04751(15) 0.0376(2) 0.0412(6) Uani 1 1 d . . . H20 H 0.0795 -0.0684 -0.0226 0.049 Uiso 1 1 calc R . . C21 C 0.21141(18) 0.00076(14) 0.03868(18) 0.0340(5) Uani 1 1 d . . . H21 H 0.2302 0.0136 -0.0191 0.041 Uiso 1 1 calc R . . C22 C 0.27351(15) 0.03073(12) 0.12988(15) 0.0253(4) Uani 1 1 d . . . C23 C 0.62279(16) 0.05293(13) 0.40249(15) 0.0266(4) Uani 1 1 d . . . H23 H 0.5929 0.0463 0.4554 0.032 Uiso 1 1 calc R . . C24 C 0.71894(17) 0.01901(14) 0.39468(17) 0.0314(5) Uani 1 1 d . . . C25 C 0.8019(2) -0.03117(17) 0.4552(2) 0.0455(6) Uani 1 1 d . . . H25 H 0.7978 -0.0509 0.5166 0.055 Uiso 1 1 calc R . . C26 C 0.8872(2) -0.0499(2) 0.4224(3) 0.0577(8) Uani 1 1 d . . . H26 H 0.9441 -0.0831 0.4621 0.069 Uiso 1 1 calc R . . C27 C 0.8945(2) -0.0220(2) 0.3311(3) 0.0620(9) Uani 1 1 d . . . H27 H 0.9562 -0.0369 0.3114 0.074 Uiso 1 1 calc R . . C28 C 0.8157(2) 0.02620(18) 0.2696(2) 0.0489(7) Uani 1 1 d . . . H28 H 0.8214 0.0443 0.2081 0.059 Uiso 1 1 calc R . . C29 C 0.72521(17) 0.04763(14) 0.30214(17) 0.0315(5) Uani 1 1 d . . . C30 C 0.48065(16) 0.14485(13) 0.29508(16) 0.0262(4) Uani 1 1 d . . . H30A H 0.4862 0.1934 0.2519 0.031 Uiso 1 1 calc R . . H30B H 0.4688 0.1696 0.3548 0.031 Uiso 1 1 calc R . . 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 0.03741(11) 0.03764(11) 0.03094(10) -0.00090(7) 0.01550(7) -0.01145(7) O1 0.0693(12) 0.0277(8) 0.0306(8) 0.0036(7) 0.0216(8) -0.0077(8) O2 0.0539(11) 0.0351(9) 0.0532(11) -0.0024(8) 0.0174(9) -0.0148(8) O3 0.0630(14) 0.0708(14) 0.0299(9) 0.0074(9) -0.0001(9) 0.0037(10) N1 0.0239(8) 0.0319(9) 0.0252(9) -0.0021(7) 0.0076(7) -0.0040(7) N2 0.0218(8) 0.0252(8) 0.0252(8) -0.0025(7) 0.0075(6) 0.0005(6) N3 0.0286(9) 0.0507(12) 0.0280(10) -0.0071(8) 0.0081(8) -0.0006(8) N4 0.0227(8) 0.0264(8) 0.0273(9) -0.0060(7) 0.0042(7) -0.0040(6) N5 0.0227(8) 0.0267(8) 0.0233(8) 0.0019(7) 0.0033(6) -0.0031(6) N6 0.0237(8) 0.0224(8) 0.0244(8) 0.0033(6) 0.0054(6) 0.0008(6) N7 0.0338(9) 0.0295(9) 0.0306(9) -0.0027(8) 0.0148(8) -0.0089(7) N8 0.0245(8) 0.0220(8) 0.0216(8) -0.0008(6) 0.0061(6) -0.0019(6) N9 0.0338(9) 0.0282(9) 0.0266(9) 0.0026(7) 0.0137(7) 0.0020(7) C1 0.0250(10) 0.0285(10) 0.0302(10) 0.0057(8) 0.0111(8) 0.0058(8) C2 0.0205(9) 0.0229(9) 0.0386(11) 0.0078(8) 0.0096(8) 0.0055(7) C3 0.0243(10) 0.0318(11) 0.0560(15) 0.0142(11) 0.0112(10) -0.0011(9) C4 0.0252(11) 0.0361(13) 0.0678(18) 0.0063(12) 0.0073(11) -0.0070(9) C5 0.0288(11) 0.0389(13) 0.0498(15) -0.0092(11) -0.0020(10) -0.0050(10) C6 0.0281(11) 0.0366(12) 0.0341(12) -0.0026(9) 0.0035(9) -0.0027(9) C7 0.0204(9) 0.0228(9) 0.0307(10) 0.0007(8) 0.0056(7) 0.0000(7) C8 0.0263(10) 0.0321(11) 0.0330(11) -0.0002(9) 0.0046(8) -0.0039(8) C9 0.0230(10) 0.0272(10) 0.0442(13) -0.0023(9) 0.0053(9) -0.0064(8) C10 0.0310(13) 0.0403(14) 0.0716(19) 0.0081(13) 0.0063(12) -0.0004(10) C11 0.0276(13) 0.0429(15) 0.094(2) -0.0086(16) 0.0083(14) 0.0012(11) C12 0.0270(13) 0.072(2) 0.093(3) -0.0386(19) 0.0183(14) -0.0020(13) C13 0.0331(13) 0.088(2) 0.0508(16) -0.0221(16) 0.0152(12) -0.0004(14) C14 0.0226(10) 0.0399(12) 0.0401(12) -0.0133(10) 0.0060(9) -0.0053(9) C15 0.0273(10) 0.0253(10) 0.0318(11) -0.0059(8) 0.0069(8) -0.0004(8) C16 0.0307(10) 0.0265(10) 0.0315(11) 0.0062(8) 0.0122(9) 0.0036(8) C17 0.0223(9) 0.0235(9) 0.0414(12) 0.0070(9) 0.0117(8) 0.0037(7) C18 0.0272(11) 0.0340(12) 0.0625(16) 0.0097(11) 0.0192(11) -0.0023(9) C19 0.0237(11) 0.0329(12) 0.080(2) 0.0039(13) 0.0116(12) -0.0051(9) C20 0.0235(11) 0.0330(12) 0.0579(16) -0.0009(11) -0.0040(10) -0.0020(9) C21 0.0278(11) 0.0300(11) 0.0384(12) 0.0012(9) -0.0003(9) -0.0014(8) C22 0.0204(9) 0.0206(9) 0.0338(11) 0.0039(8) 0.0054(8) 0.0020(7) C23 0.0279(10) 0.0274(10) 0.0233(10) 0.0005(8) 0.0050(8) 0.0013(8) C24 0.0262(10) 0.0275(10) 0.0366(12) -0.0055(9) 0.0024(9) -0.0018(8) C25 0.0325(12) 0.0428(14) 0.0522(15) -0.0054(12) -0.0032(11) 0.0097(10) C26 0.0314(13) 0.0559(17) 0.078(2) -0.0110(16) 0.0025(13) 0.0121(12) C27 0.0286(13) 0.0565(18) 0.107(3) -0.0253(18) 0.0284(15) -0.0023(12) C28 0.0380(14) 0.0483(15) 0.0699(19) -0.0196(14) 0.0309(13) -0.0137(11) C29 0.0262(10) 0.0277(10) 0.0424(12) -0.0120(9) 0.0122(9) -0.0088(8) C30 0.0269(10) 0.0223(9) 0.0273(10) 0.0015(8) 0.0038(8) -0.0004(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N5 2.1944(16) . ? Ag1 N1 2.2357(17) . ? Ag1 N3 2.416(2) . ? Ag1 O1 2.5334(16) . ? O1 N9 1.260(2) . ? O2 N9 1.233(3) . ? O3 N9 1.237(3) . ? N1 C7 1.352(3) . ? N1 N2 1.365(2) . ? N2 C1 1.349(3) . ? N2 C15 1.454(3) . ? N3 C14 1.353(3) . ? N3 N4 1.357(3) . ? N4 C8 1.348(3) . ? N4 C15 1.452(3) . ? N5 C22 1.349(2) . ? N5 N6 1.368(2) . ? N6 C16 1.342(3) . ? N6 C30 1.451(3) . ? N7 C29 1.346(3) . ? N7 N8 1.359(2) . ? N8 C23 1.348(3) . ? N8 C30 1.450(3) . ? C1 C2 1.384(3) . ? C1 H1 0.9500 . ? C2 C3 1.420(3) . ? C2 C7 1.420(3) . ? C3 C4 1.362(4) . ? C3 H3 0.9500 . ? C4 C5 1.421(4) . ? C4 H4 0.9500 . ? C5 C6 1.367(3) . ? C5 H5 0.9500 . ? C6 C7 1.421(3) . ? C6 H6 0.9500 . ? C8 C9 1.396(3) . ? C8 H8 0.9500 . ? C9 C10 1.411(3) . ? C9 C14 1.414(3) . ? C10 C11 1.350(4) . ? C10 H10 0.9500 . ? C11 C12 1.424(5) . ? C11 H11 0.9500 . ? C12 C13 1.358(5) . ? C12 H12 0.9500 . ? C13 C14 1.418(3) . ? C13 H13 0.9500 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.393(3) . ? C16 H16 0.9500 . ? C17 C18 1.419(3) . ? C17 C22 1.420(3) . ? C18 C19 1.356(4) . ? C18 H18 0.9500 . ? C19 C20 1.430(4) . ? C19 H19 0.9500 . ? C20 C21 1.369(3) . ? C20 H20 0.9500 . ? C21 C22 1.415(3) . ? C21 H21 0.9500 . ? C23 C24 1.389(3) . ? C23 H23 0.9500 . ? C24 C25 1.417(3) . ? C24 C29 1.426(3) . ? C25 C26 1.353(4) . ? C25 H25 0.9500 . ? C26 C27 1.410(5) . ? C26 H26 0.9500 . ? C27 C28 1.374(5) . ? C27 H27 0.9500 . ? C28 C29 1.421(3) . ? C28 H28 0.9500 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? 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 N5 Ag1 N1 157.66(7) . . ? N5 Ag1 N3 110.80(6) . . ? N1 Ag1 N3 85.05(7) . . ? N5 Ag1 O1 95.97(6) . . ? N1 Ag1 O1 93.95(6) . . ? N3 Ag1 O1 107.38(6) . . ? N9 O1 Ag1 119.65(13) . . ? C7 N1 N2 104.02(16) . . ? C7 N1 Ag1 129.22(14) . . ? N2 N1 Ag1 122.66(13) . . ? C1 N2 N1 113.32(17) . . ? C1 N2 C15 126.97(18) . . ? N1 N2 C15 119.71(16) . . ? C14 N3 N4 103.65(19) . . ? C14 N3 Ag1 130.38(15) . . ? N4 N3 Ag1 118.33(14) . . ? C8 N4 N3 113.89(18) . . ? C8 N4 C15 127.53(19) . . ? N3 N4 C15 118.58(18) . . ? C22 N5 N6 104.46(16) . . ? C22 N5 Ag1 128.43(14) . . ? N6 N5 Ag1 127.08(12) . . ? C16 N6 N5 113.18(17) . . ? C16 N6 C30 126.36(18) . . ? N5 N6 C30 120.42(16) . . ? C29 N7 N8 102.79(17) . . ? C23 N8 N7 114.60(17) . . ? C23 N8 C30 126.62(17) . . ? N7 N8 C30 118.78(17) . . ? O2 N9 O3 120.6(2) . . ? O2 N9 O1 119.2(2) . . ? O3 N9 O1 120.2(2) . . ? N2 C1 C2 106.49(18) . . ? N2 C1 H1 126.8 . . ? C2 C1 H1 126.8 . . ? C1 C2 C3 134.8(2) . . ? C1 C2 C7 105.22(17) . . ? C3 C2 C7 120.0(2) . . ? C4 C3 C2 117.5(2) . . ? C4 C3 H3 121.3 . . ? C2 C3 H3 121.3 . . ? C3 C4 C5 122.3(2) . . ? C3 C4 H4 118.9 . . ? C5 C4 H4 118.9 . . ? C6 C5 C4 122.1(2) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C5 C6 C7 116.5(2) . . ? C5 C6 H6 121.8 . . ? C7 C6 H6 121.8 . . ? N1 C7 C2 110.94(18) . . ? N1 C7 C6 127.42(19) . . ? C2 C7 C6 121.63(19) . . ? N4 C8 C9 106.2(2) . . ? N4 C8 H8 126.9 . . ? C9 C8 H8 126.9 . . ? C8 C9 C10 134.9(2) . . ? C8 C9 C14 104.6(2) . . ? C10 C9 C14 120.4(2) . . ? C11 C10 C9 118.7(3) . . ? C11 C10 H10 120.6 . . ? C9 C10 H10 120.6 . . ? C10 C11 C12 120.7(3) . . ? C10 C11 H11 119.7 . . ? C12 C11 H11 119.7 . . ? C13 C12 C11 122.6(3) . . ? C13 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? C12 C13 C14 117.3(3) . . ? C12 C13 H13 121.4 . . ? C14 C13 H13 121.4 . . ? N3 C14 C9 111.6(2) . . ? N3 C14 C13 128.1(2) . . ? C9 C14 C13 120.3(2) . . ? N4 C15 N2 112.05(16) . . ? N4 C15 H15A 109.2 . . ? N2 C15 H15A 109.2 . . ? N4 C15 H15B 109.2 . . ? N2 C15 H15B 109.2 . . ? H15A C15 H15B 107.9 . . ? N6 C16 C17 106.54(19) . . ? N6 C16 H16 126.7 . . ? C17 C16 H16 126.7 . . ? C16 C17 C18 135.0(2) . . ? C16 C17 C22 105.15(18) . . ? C18 C17 C22 119.8(2) . . ? C19 C18 C17 118.4(2) . . ? C19 C18 H18 120.8 . . ? C17 C18 H18 120.8 . . ? C18 C19 C20 121.3(2) . . ? C18 C19 H19 119.4 . . ? C20 C19 H19 119.4 . . ? C21 C20 C19 122.2(2) . . ? C21 C20 H20 118.9 . . ? C19 C20 H20 118.9 . . ? C20 C21 C22 116.9(2) . . ? C20 C21 H21 121.6 . . ? C22 C21 H21 121.6 . . ? N5 C22 C21 127.9(2) . . ? N5 C22 C17 110.66(18) . . ? C21 C22 C17 121.42(19) . . ? N8 C23 C24 106.19(19) . . ? N8 C23 H23 126.9 . . ? C24 C23 H23 126.9 . . ? C23 C24 C25 135.0(2) . . ? C23 C24 C29 104.07(19) . . ? C25 C24 C29 120.9(2) . . ? C26 C25 C24 117.5(3) . . ? C26 C25 H25 121.2 . . ? C24 C25 H25 121.2 . . ? C25 C26 C27 122.1(3) . . ? C25 C26 H26 118.9 . . ? C27 C26 H26 118.9 . . ? C28 C27 C26 122.4(2) . . ? C28 C27 H27 118.8 . . ? C26 C27 H27 118.8 . . ? C27 C28 C29 117.0(3) . . ? C27 C28 H28 121.5 . . ? C29 C28 H28 121.5 . . ? N7 C29 C28 127.5(2) . . ? N7 C29 C24 112.35(18) . . ? C28 C29 C24 120.1(2) . . ? N8 C30 N6 112.66(16) . . ? N8 C30 H30A 109.1 . . ? N6 C30 H30A 109.1 . . ? N8 C30 H30B 109.1 . . ? N6 C30 H30B 109.1 . . ? H30A C30 H30B 107.8 . . ? 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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N5 Ag1 O1 N9 -151.43(17) . . . . ? N1 Ag1 O1 N9 48.62(17) . . . . ? N3 Ag1 O1 N9 -37.42(18) . . . . ? N5 Ag1 N1 C7 -86.3(2) . . . . ? N3 Ag1 N1 C7 137.04(19) . . . . ? O1 Ag1 N1 C7 29.91(18) . . . . ? N5 Ag1 N1 N2 120.22(18) . . . . ? N3 Ag1 N1 N2 -16.41(15) . . . . ? O1 Ag1 N1 N2 -123.54(15) . . . . ? C7 N1 N2 C1 1.2(2) . . . . ? Ag1 N1 N2 C1 160.27(14) . . . . ? C7 N1 N2 C15 -178.45(17) . . . . ? Ag1 N1 N2 C15 -19.4(2) . . . . ? N5 Ag1 N3 C14 65.3(2) . . . . ? N1 Ag1 N3 C14 -130.9(2) . . . . ? O1 Ag1 N3 C14 -38.3(2) . . . . ? N5 Ag1 N3 N4 -150.54(15) . . . . ? N1 Ag1 N3 N4 13.24(16) . . . . ? O1 Ag1 N3 N4 105.84(16) . . . . ? C14 N3 N4 C8 -0.9(2) . . . . ? Ag1 N3 N4 C8 -153.61(14) . . . . ? C14 N3 N4 C15 178.49(17) . . . . ? Ag1 N3 N4 C15 25.8(2) . . . . ? N1 Ag1 N5 C22 -107.8(2) . . . . ? N3 Ag1 N5 C22 25.11(19) . . . . ? O1 Ag1 N5 C22 136.28(17) . . . . ? N1 Ag1 N5 N6 74.6(2) . . . . ? N3 Ag1 N5 N6 -152.44(15) . . . . ? O1 Ag1 N5 N6 -41.27(16) . . . . ? C22 N5 N6 C16 0.2(2) . . . . ? Ag1 N5 N6 C16 178.20(14) . . . . ? C22 N5 N6 C30 -177.77(16) . . . . ? Ag1 N5 N6 C30 0.2(2) . . . . ? C29 N7 N8 C23 -0.3(2) . . . . ? C29 N7 N8 C30 179.17(17) . . . . ? Ag1 O1 N9 O2 -141.79(17) . . . . ? Ag1 O1 N9 O3 39.5(3) . . . . ? N1 N2 C1 C2 -0.9(2) . . . . ? C15 N2 C1 C2 178.72(18) . . . . ? N2 C1 C2 C3 179.6(2) . . . . ? N2 C1 C2 C7 0.2(2) . . . . ? C1 C2 C3 C4 -178.7(2) . . . . ? C7 C2 C3 C4 0.5(3) . . . . ? C2 C3 C4 C5 -0.7(4) . . . . ? C3 C4 C5 C6 0.3(4) . . . . ? C4 C5 C6 C7 0.2(4) . . . . ? N2 N1 C7 C2 -1.0(2) . . . . ? Ag1 N1 C7 C2 -158.18(14) . . . . ? N2 N1 C7 C6 -179.9(2) . . . . ? Ag1 N1 C7 C6 23.0(3) . . . . ? C1 C2 C7 N1 0.5(2) . . . . ? C3 C2 C7 N1 -178.95(18) . . . . ? C1 C2 C7 C6 179.45(19) . . . . ? C3 C2 C7 C6 0.0(3) . . . . ? C5 C6 C7 N1 178.4(2) . . . . ? C5 C6 C7 C2 -0.4(3) . . . . ? N3 N4 C8 C9 0.3(2) . . . . ? C15 N4 C8 C9 -179.06(18) . . . . ? N4 C8 C9 C10 179.8(2) . . . . ? N4 C8 C9 C14 0.4(2) . . . . ? C8 C9 C10 C11 -179.3(3) . . . . ? C14 C9 C10 C11 0.0(4) . . . . ? C9 C10 C11 C12 0.5(4) . . . . ? C10 C11 C12 C13 -0.7(5) . . . . ? C11 C12 C13 C14 0.3(5) . . . . ? N4 N3 C14 C9 1.2(2) . . . . ? Ag1 N3 C14 C9 149.17(16) . . . . ? N4 N3 C14 C13 -178.9(2) . . . . ? Ag1 N3 C14 C13 -31.0(4) . . . . ? C8 C9 C14 N3 -1.1(2) . . . . ? C10 C9 C14 N3 179.4(2) . . . . ? C8 C9 C14 C13 179.1(2) . . . . ? C10 C9 C14 C13 -0.4(3) . . . . ? C12 C13 C14 N3 -179.6(3) . . . . ? C12 C13 C14 C9 0.3(4) . . . . ? C8 N4 C15 N2 103.8(2) . . . . ? N3 N4 C15 N2 -75.6(2) . . . . ? C1 N2 C15 N4 -107.0(2) . . . . ? N1 N2 C15 N4 72.6(2) . . . . ? N5 N6 C16 C17 0.1(2) . . . . ? C30 N6 C16 C17 177.95(18) . . . . ? N6 C16 C17 C18 -179.0(2) . . . . ? N6 C16 C17 C22 -0.4(2) . . . . ? C16 C17 C18 C19 178.2(2) . . . . ? C22 C17 C18 C19 -0.2(3) . . . . ? C17 C18 C19 C20 0.2(4) . . . . ? C18 C19 C20 C21 0.0(4) . . . . ? C19 C20 C21 C22 -0.2(3) . . . . ? N6 N5 C22 C21 178.9(2) . . . . ? Ag1 N5 C22 C21 0.9(3) . . . . ? N6 N5 C22 C17 -0.4(2) . . . . ? Ag1 N5 C22 C17 -178.42(13) . . . . ? C20 C21 C22 N5 -179.0(2) . . . . ? C20 C21 C22 C17 0.2(3) . . . . ? C16 C17 C22 N5 0.5(2) . . . . ? C18 C17 C22 N5 179.38(19) . . . . ? C16 C17 C22 C21 -178.87(19) . . . . ? C18 C17 C22 C21 0.0(3) . . . . ? N7 N8 C23 C24 0.3(2) . . . . ? C30 N8 C23 C24 -179.10(18) . . . . ? N8 C23 C24 C25 178.6(2) . . . . ? N8 C23 C24 C29 -0.2(2) . . . . ? C23 C24 C25 C26 -178.0(3) . . . . ? C29 C24 C25 C26 0.7(4) . . . . ? C24 C25 C26 C27 -0.6(4) . . . . ? C25 C26 C27 C28 0.1(5) . . . . ? C26 C27 C28 C29 0.4(4) . . . . ? N8 N7 C29 C28 -178.5(2) . . . . ? N8 N7 C29 C24 0.2(2) . . . . ? C27 C28 C29 N7 178.3(2) . . . . ? C27 C28 C29 C24 -0.3(3) . . . . ? C23 C24 C29 N7 0.0(2) . . . . ? C25 C24 C29 N7 -179.0(2) . . . . ? C23 C24 C29 C28 178.8(2) . . . . ? C25 C24 C29 C28 -0.2(3) . . . . ? C23 N8 C30 N6 -88.5(2) . . . . ? N7 N8 C30 N6 92.1(2) . . . . ? C16 N6 C30 N8 96.0(2) . . . . ? N5 N6 C30 N8 -86.3(2) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.62 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.420 _refine_diff_density_min -0.986 _refine_diff_density_rms 0.085 data_13 _database_code_depnum_ccdc_archive 'CCDC 917672' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C34 H24 Ag2 F6 N8 O4' _chemical_formula_sum 'C34 H24 Ag2 F6 N8 O4' _chemical_formula_weight 938.35 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' 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' F F 0.0171 0.0103 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.3882(15) _cell_length_b 14.560(3) _cell_length_c 15.502(3) _cell_angle_alpha 71.291(4) _cell_angle_beta 89.483(5) _cell_angle_gamma 80.025(4) _cell_volume 1763.9(5) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 6334 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 28.16 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.19 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 928 _exptl_absorpt_coefficient_mu 1.193 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7893 _exptl_absorpt_correction_T_max 0.8079 _exptl_absorpt_process_details ; APEX2 Software Suite; Bruker 2005. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker-Nonius X8kappa APEX II CCD area detector ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 27870 _diffrn_reflns_av_R_equivalents 0.0294 _diffrn_reflns_av_sigmaI/netI 0.0242 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.27 _reflns_number_total 6395 _reflns_number_gt 5323 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker, 2007)' _computing_cell_refinement 'APEX2 Software Suite (Bruker, 2007)' _computing_data_reduction 'APEX2 Software Suite (Bruker, 2007)' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL and publCIF (Westrip, 2010)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1079P)^2^+0.8528P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6395 _refine_ls_number_parameters 604 _refine_ls_number_restraints 189 _refine_ls_R_factor_all 0.0718 _refine_ls_R_factor_gt 0.0504 _refine_ls_wR_factor_ref 0.1964 _refine_ls_wR_factor_gt 0.1590 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.010 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.001 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.40734(7) 0.15061(5) 0.11513(5) 0.0330(2) Uani 1 1 d U . . Ag2 Ag 0.56631(9) 0.28354(5) 0.18792(5) 0.0429(2) Uani 1 1 d U . . O1 O 0.7000(7) 0.1500(5) 0.0738(5) 0.0396(11) Uani 1 1 d U . . O2 O 0.7657(7) 0.1462(5) 0.2156(5) 0.0413(12) Uani 1 1 d U A . N1 N 0.4294(9) -0.0761(6) 0.2341(6) 0.0412(12) Uani 1 1 d U B . N2 N 0.4387(9) -0.0268(5) 0.1444(6) 0.0390(12) Uani 1 1 d U . . N3 N 0.3893(9) 0.0326(6) 0.3251(6) 0.0436(12) Uani 1 1 d U B . N4 N 0.3502(9) 0.1248(6) 0.2628(6) 0.0410(12) Uani 1 1 d U . . N5 N 0.3774(8) 0.3052(5) -0.0890(5) 0.0295(10) Uani 1 1 d U B . N6 N 0.3205(8) 0.2273(5) -0.0310(5) 0.0290(10) Uani 1 1 d U . . N7 N 0.3727(8) 0.4224(5) -0.0079(5) 0.0323(11) Uani 1 1 d U . . N8 N 0.3755(8) 0.3936(5) 0.0843(5) 0.0343(11) Uani 1 1 d U . . F1A F 1.0691(14) 0.0904(10) 0.1230(15) 0.037(2) Uani 0.33 1 d PDU A 1 F2A F 0.9278(17) -0.0067(12) 0.0943(12) 0.041(2) Uani 0.33 1 d PDU A 1 F3A F 0.984(2) -0.0181(12) 0.2321(10) 0.045(2) Uani 0.33 1 d PDU A 1 F1B F 1.0401(17) 0.0924(11) 0.0819(12) 0.036(2) Uani 0.33 1 d PDU A 2 F2B F 0.9159(17) -0.0311(10) 0.1310(14) 0.037(2) Uani 0.33 1 d PDU A 2 F3B F 1.0344(18) 0.0209(14) 0.2258(11) 0.039(2) Uani 0.33 1 d PDU A 2 F1C F 0.987(2) 0.0547(14) 0.0617(10) 0.048(2) Uani 0.33 1 d PDU A 3 F2C F 0.9217(18) -0.0400(9) 0.1851(15) 0.045(2) Uani 0.33 1 d PDU A 3 F3C F 1.0679(16) 0.0674(13) 0.1837(15) 0.043(2) Uani 0.33 1 d PDU A 3 C1 C 0.3689(10) -0.0729(6) 0.0979(7) 0.0379(13) Uani 1 1 d U . . H1 H 0.3587 -0.0532 0.0333 0.045 Uiso 1 1 calc R . . C2 C 0.3116(10) -0.1557(7) 0.1581(7) 0.0393(13) Uani 1 1 d U . . C3 C 0.2357(11) -0.2301(7) 0.1488(8) 0.0446(15) Uani 1 1 d U . . H3 H 0.2058 -0.2311 0.0902 0.054 Uiso 1 1 calc R . . C4 C 0.2052(12) -0.3014(8) 0.2258(8) 0.0535(17) Uani 1 1 d U . . H4 H 0.1570 -0.3539 0.2205 0.064 Uiso 1 1 calc R B . C5 C 0.2439(13) -0.2988(8) 0.3137(9) 0.0554(17) Uani 1 1 d U . . H5 H 0.2186 -0.3489 0.3659 0.067 Uiso 1 1 calc R . . C6 C 0.3169(12) -0.2261(8) 0.3256(8) 0.0510(16) Uani 1 1 d U . . H6 H 0.3418 -0.2235 0.3844 0.061 Uiso 1 1 calc R B . C7 C 0.3525(11) -0.1551(7) 0.2443(7) 0.0421(13) Uani 1 1 d U B . C8 C 0.2496(12) 0.1788(8) 0.3016(7) 0.0460(15) Uani 1 1 d U . . H8 H 0.2019 0.2460 0.2731 0.055 Uiso 1 1 calc R . . C9 C 0.2232(12) 0.1214(9) 0.3923(7) 0.0501(15) Uani 1 1 d U . . C10 C 0.1297(15) 0.1393(10) 0.4641(8) 0.0604(18) Uani 1 1 d U . . H10 H 0.0634 0.2015 0.4570 0.072 Uiso 1 1 calc R . . C11 C 0.1399(16) 0.0631(11) 0.5433(8) 0.0640(19) Uani 1 1 d U . . H11 H 0.0811 0.0740 0.5928 0.077 Uiso 1 1 calc R B . C12 C 0.2320(15) -0.0307(11) 0.5564(8) 0.0639(19) Uani 1 1 d U . . H12 H 0.2331 -0.0812 0.6134 0.077 Uiso 1 1 calc R . . C13 C 0.3219(14) -0.0505(10) 0.4863(7) 0.0576(17) Uani 1 1 d U . . H13 H 0.3853 -0.1135 0.4935 0.069 Uiso 1 1 calc R B . C14 C 0.3131(12) 0.0276(8) 0.4053(7) 0.0480(14) Uani 1 1 d U B . C15 C 0.4994(11) -0.0429(7) 0.3007(7) 0.0444(14) Uani 1 1 d U . . H15A H 0.5976 -0.0165 0.2763 0.053 Uiso 1 1 calc R B . H15B H 0.5333 -0.1000 0.3564 0.053 Uiso 1 1 calc R . . C16 C 0.2416(9) 0.1915(6) -0.0817(6) 0.0312(12) Uani 1 1 d U . . H16 H 0.1890 0.1364 -0.0584 0.037 Uiso 1 1 calc R . . C17 C 0.2444(10) 0.2443(7) -0.1744(6) 0.0359(12) Uani 1 1 d U . . C18 C 0.1829(12) 0.2378(8) -0.2557(7) 0.0469(15) Uani 1 1 d U . . H18 H 0.1233 0.1878 -0.2552 0.056 Uiso 1 1 calc R . . C19 C 0.2121(14) 0.3068(9) -0.3367(8) 0.0553(17) Uani 1 1 d U . . H19 H 0.1724 0.3038 -0.3927 0.066 Uiso 1 1 calc R B . C20 C 0.2998(14) 0.3819(9) -0.3377(8) 0.0550(17) Uani 1 1 d U . . H20 H 0.3160 0.4288 -0.3945 0.066 Uiso 1 1 calc R . . C21 C 0.3614(12) 0.3886(8) -0.2596(7) 0.0462(15) Uani 1 1 d U . . H21 H 0.4220 0.4384 -0.2609 0.055 Uiso 1 1 calc R B . C22 C 0.3323(10) 0.3188(6) -0.1761(6) 0.0343(12) Uani 1 1 d U B . C23 C 0.2638(10) 0.4599(6) 0.1070(7) 0.0361(13) Uani 1 1 d U . . H23 H 0.2396 0.4577 0.1675 0.043 Uiso 1 1 calc R B . C24 C 0.1884(10) 0.5331(6) 0.0269(7) 0.0351(12) Uani 1 1 d U B . C25 C 0.0682(10) 0.6197(6) 0.0080(7) 0.0388(14) Uani 1 1 d U . . H25 H 0.0180 0.6392 0.0561 0.047 Uiso 1 1 calc R B . C26 C 0.0271(11) 0.6737(7) -0.0801(8) 0.0452(16) Uani 1 1 d U . . H26 H -0.0543 0.7311 -0.0936 0.054 Uiso 1 1 calc R . . C27 C 0.1019(11) 0.6469(7) -0.1521(8) 0.0450(16) Uani 1 1 d U . . H27 H 0.0707 0.6878 -0.2129 0.054 Uiso 1 1 calc R B . C28 C 0.2194(10) 0.5632(6) -0.1378(7) 0.0410(15) Uani 1 1 d U B . H28 H 0.2689 0.5447 -0.1866 0.049 Uiso 1 1 calc R . . C29 C 0.2600(9) 0.5077(6) -0.0461(7) 0.0333(12) Uani 1 1 d U B . C30 C 0.4715(9) 0.3619(6) -0.0554(6) 0.0313(12) Uani 1 1 d U B . H30A H 0.5213 0.4053 -0.1072 0.038 Uiso 1 1 calc R . . H30B H 0.5600 0.3165 -0.0131 0.038 Uiso 1 1 calc R . . C31 C 0.7860(10) 0.1230(6) 0.1446(6) 0.0347(12) Uani 1 1 d U A . C32 C 0.9420(9) 0.0498(6) 0.1467(5) 0.0372(12) Uani 1 1 d DU . . O3A O 0.446(3) 0.4373(13) 0.2800(12) 0.069(3) Uani 0.50 1 d PDU B 1 O4A O 0.580(3) 0.2807(16) 0.3261(13) 0.074(2) Uani 0.50 1 d PDU B 1 C33A C 0.497(8) 0.354(2) 0.3350(19) 0.0739(18) Uani 0.50 1 d PDU B 1 C34A C 0.420(3) 0.3718(15) 0.4265(16) 0.0740(19) Uani 0.50 1 d PDU B 1 F4A F 0.438(3) 0.2810(14) 0.4926(15) 0.077(3) Uani 0.50 1 d PDU B 1 F5A F 0.275(2) 0.4235(14) 0.4138(13) 0.091(3) Uani 0.50 1 d PDU B 1 F6A F 0.516(2) 0.4170(13) 0.4643(11) 0.082(2) Uani 0.50 1 d PDU B 1 O3B O 0.544(3) 0.2698(15) 0.3567(13) 0.074(2) Uani 0.50 1 d PDU B 2 O4B O 0.465(3) 0.4043(14) 0.2682(12) 0.072(2) Uani 0.50 1 d PDU B 2 C33B C 0.491(8) 0.354(2) 0.3466(16) 0.0735(18) Uani 0.50 1 d PDU B 2 C34B C 0.488(2) 0.3673(15) 0.4384(18) 0.0731(18) Uani 0.50 1 d PDU B 2 F4B F 0.398(3) 0.3012(15) 0.4930(15) 0.080(3) Uani 0.50 1 d PDU B 2 F5B F 0.637(2) 0.3718(14) 0.4693(12) 0.088(3) Uani 0.50 1 d PDU B 2 F6B F 0.400(2) 0.4575(12) 0.4300(12) 0.080(2) Uani 0.50 1 d PDU B 2 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 0.0266(3) 0.0345(4) 0.0380(4) -0.0122(3) 0.0024(2) -0.0048(2) Ag2 0.0425(4) 0.0425(4) 0.0470(5) -0.0255(3) 0.0004(3) 0.0045(3) O1 0.026(2) 0.048(3) 0.047(3) -0.020(2) 0.0023(18) -0.002(2) O2 0.033(2) 0.043(3) 0.044(3) -0.013(2) 0.002(2) 0.000(2) N1 0.034(3) 0.038(2) 0.050(3) -0.015(2) 0.000(2) 0.000(2) N2 0.030(3) 0.034(2) 0.051(3) -0.015(2) 0.000(2) 0.003(2) N3 0.038(3) 0.053(3) 0.040(2) -0.016(2) -0.001(2) -0.007(2) N4 0.033(3) 0.052(3) 0.039(2) -0.019(2) 0.000(2) -0.003(2) N5 0.023(2) 0.026(2) 0.041(2) -0.0130(18) 0.007(2) -0.0053(18) N6 0.022(2) 0.025(2) 0.040(2) -0.0113(19) 0.002(2) -0.0023(19) N7 0.024(2) 0.027(2) 0.051(2) -0.0189(19) 0.006(2) -0.0046(18) N8 0.025(2) 0.031(2) 0.053(2) -0.023(2) 0.007(2) -0.0054(19) F1A 0.030(3) 0.041(3) 0.042(4) -0.014(3) 0.005(3) -0.007(3) F2A 0.041(4) 0.038(3) 0.048(4) -0.019(3) 0.003(3) -0.004(3) F3A 0.044(4) 0.042(4) 0.045(3) -0.012(3) 0.004(3) -0.001(3) F1B 0.031(3) 0.038(3) 0.043(3) -0.017(3) 0.008(3) -0.006(3) F2B 0.038(4) 0.033(3) 0.039(4) -0.012(3) 0.004(3) -0.005(3) F3B 0.032(3) 0.040(4) 0.043(3) -0.012(3) 0.002(3) -0.007(3) F1C 0.043(4) 0.051(4) 0.047(3) -0.016(3) 0.008(3) 0.001(3) F2C 0.042(3) 0.038(3) 0.053(4) -0.012(3) 0.003(3) -0.006(3) F3C 0.034(3) 0.044(3) 0.049(4) -0.013(3) 0.001(3) -0.006(3) C1 0.028(3) 0.036(3) 0.052(3) -0.021(2) 0.004(3) 0.003(2) C2 0.025(3) 0.040(3) 0.055(3) -0.023(2) 0.005(2) 0.001(2) C3 0.030(3) 0.046(3) 0.062(3) -0.024(3) 0.007(3) -0.006(3) C4 0.040(3) 0.052(3) 0.069(4) -0.019(3) 0.009(3) -0.012(3) C5 0.045(3) 0.054(3) 0.065(4) -0.013(3) 0.010(3) -0.014(3) C6 0.041(3) 0.051(3) 0.058(3) -0.013(3) 0.006(3) -0.008(3) C7 0.030(3) 0.042(3) 0.054(3) -0.018(2) 0.005(2) -0.002(2) C8 0.041(3) 0.060(3) 0.041(3) -0.023(3) 0.003(3) -0.007(3) C9 0.045(3) 0.071(3) 0.040(3) -0.025(3) 0.004(2) -0.014(3) C10 0.059(4) 0.087(4) 0.043(3) -0.029(3) 0.007(3) -0.016(3) C11 0.064(4) 0.094(4) 0.042(3) -0.026(3) 0.006(3) -0.026(3) C12 0.064(4) 0.090(4) 0.040(3) -0.017(3) 0.001(3) -0.028(3) C13 0.055(4) 0.079(4) 0.040(3) -0.015(3) -0.003(3) -0.023(3) C14 0.044(3) 0.066(3) 0.038(3) -0.020(2) -0.002(2) -0.017(3) C15 0.036(3) 0.046(3) 0.047(3) -0.012(3) -0.002(3) -0.003(2) C16 0.024(3) 0.029(3) 0.042(2) -0.013(2) 0.004(2) -0.006(2) C17 0.029(3) 0.039(3) 0.042(2) -0.016(2) 0.004(2) -0.006(2) C18 0.044(3) 0.055(3) 0.043(3) -0.018(3) 0.004(3) -0.009(3) C19 0.057(4) 0.065(4) 0.041(3) -0.016(3) 0.005(3) -0.008(3) C20 0.058(4) 0.060(4) 0.041(3) -0.009(3) 0.012(3) -0.009(3) C21 0.046(3) 0.047(3) 0.042(3) -0.009(3) 0.015(3) -0.009(3) C22 0.030(3) 0.033(3) 0.040(2) -0.013(2) 0.012(2) -0.005(2) C23 0.026(3) 0.033(3) 0.057(3) -0.024(2) 0.006(2) -0.007(2) C24 0.024(2) 0.028(2) 0.061(3) -0.023(2) 0.005(2) -0.0077(19) C25 0.026(3) 0.029(3) 0.067(3) -0.024(3) 0.004(3) -0.008(2) C26 0.031(3) 0.031(3) 0.071(4) -0.015(3) 0.003(3) -0.003(2) C27 0.034(3) 0.033(3) 0.064(3) -0.011(3) 0.002(3) -0.004(2) C28 0.029(3) 0.033(3) 0.060(3) -0.013(3) 0.003(3) -0.006(2) C29 0.022(2) 0.027(2) 0.056(3) -0.019(2) 0.005(2) -0.0079(19) C30 0.023(3) 0.027(3) 0.047(3) -0.016(2) 0.008(2) -0.005(2) C31 0.026(2) 0.037(2) 0.045(3) -0.017(2) 0.004(2) -0.0073(19) C32 0.029(2) 0.037(2) 0.046(2) -0.015(2) 0.0051(19) -0.0057(19) O3A 0.100(6) 0.064(5) 0.057(4) -0.045(4) 0.008(5) -0.008(5) O4A 0.103(4) 0.073(4) 0.052(3) -0.037(3) 0.004(3) -0.004(3) C33A 0.101(4) 0.072(3) 0.057(3) -0.037(2) 0.007(3) -0.007(3) C34A 0.097(4) 0.072(3) 0.061(3) -0.037(3) 0.009(3) -0.007(3) F4A 0.088(4) 0.080(4) 0.065(4) -0.026(3) 0.008(4) -0.010(3) F5A 0.091(4) 0.091(4) 0.085(4) -0.030(4) 0.012(3) -0.002(3) F6A 0.099(4) 0.084(4) 0.073(4) -0.041(3) 0.006(3) -0.014(3) O3B 0.103(4) 0.074(4) 0.052(3) -0.037(3) 0.008(3) -0.005(4) O4B 0.101(5) 0.070(4) 0.056(3) -0.043(3) 0.009(4) -0.004(4) C33B 0.100(4) 0.072(3) 0.057(3) -0.037(2) 0.008(3) -0.006(3) C34B 0.097(3) 0.073(3) 0.060(3) -0.038(3) 0.007(3) -0.010(3) F4B 0.090(4) 0.081(4) 0.067(4) -0.026(3) 0.012(3) -0.006(3) F5B 0.098(4) 0.089(4) 0.080(4) -0.031(4) -0.005(3) -0.017(3) F6B 0.096(4) 0.077(3) 0.073(4) -0.038(3) 0.012(3) -0.005(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N6 2.243(7) . ? Ag1 N4 2.259(8) . ? Ag1 N2 2.441(7) . ? Ag1 O1 2.531(6) . ? Ag1 Ag2 3.0199(10) . ? Ag2 O4A 2.132(18) . ? Ag2 N8 2.284(8) . ? Ag2 O2 2.298(6) . ? Ag2 O4B 2.496(17) . ? Ag2 O3B 2.567(17) . ? O1 C31 1.233(11) . ? O2 C31 1.253(11) . ? N1 N2 1.355(12) . ? N1 C7 1.379(12) . ? N1 C15 1.440(13) . ? N2 C1 1.329(12) . ? N3 N4 1.365(12) . ? N3 C14 1.379(13) . ? N3 C15 1.454(13) . ? N4 C8 1.325(12) . ? N5 C22 1.347(12) . ? N5 N6 1.360(9) . ? N5 C30 1.444(10) . ? N6 C16 1.312(11) . ? N7 N8 1.353(11) . ? N7 C29 1.385(11) . ? N7 C30 1.469(10) . ? N8 C23 1.353(11) . ? F1A C32 1.301(14) . ? F2A C32 1.347(14) . ? F3A C32 1.379(14) . ? F1B C32 1.354(14) . ? F2B C32 1.329(14) . ? F3B C32 1.361(14) . ? F1C C32 1.350(14) . ? F2C C32 1.291(14) . ? F3C C32 1.307(14) . ? C1 C2 1.424(13) . ? C1 H1 0.9500 . ? C2 C7 1.385(14) . ? C2 C3 1.393(13) . ? C3 C4 1.364(16) . ? C3 H3 0.9500 . ? C4 C5 1.417(17) . ? C4 H4 0.9500 . ? C5 C6 1.371(16) . ? C5 H5 0.9500 . ? C6 C7 1.419(15) . ? C6 H6 0.9500 . ? C8 C9 1.424(15) . ? C8 H8 0.9500 . ? C9 C14 1.395(16) . ? C9 C10 1.422(15) . ? C10 C11 1.357(18) . ? C10 H10 0.9500 . ? C11 C12 1.401(19) . ? C11 H11 0.9500 . ? C12 C13 1.394(17) . ? C12 H12 0.9500 . ? C13 C14 1.391(16) . ? C13 H13 0.9500 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.397(13) . ? C16 H16 0.9500 . ? C17 C18 1.403(14) . ? C17 C22 1.406(12) . ? C18 C19 1.385(16) . ? C18 H18 0.9500 . ? C19 C20 1.415(17) . ? C19 H19 0.9500 . ? C20 C21 1.360(16) . ? C20 H20 0.9500 . ? C21 C22 1.415(13) . ? C21 H21 0.9500 . ? C23 C24 1.417(13) . ? C23 H23 0.9500 . ? C24 C29 1.399(13) . ? C24 C25 1.422(12) . ? C25 C26 1.351(15) . ? C25 H25 0.9500 . ? C26 C27 1.404(15) . ? C26 H26 0.9500 . ? C27 C28 1.387(13) . ? C27 H27 0.9500 . ? C28 C29 1.402(14) . ? C28 H28 0.9500 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C31 C32 1.532(11) . ? O3A C33A 1.242(18) . ? O4A C33A 1.216(18) . ? C33A C34A 1.63(4) . ? C34A F5A 1.294(17) . ? C34A F6A 1.365(17) . ? C34A F4A 1.373(18) . ? O3B C33B 1.187(18) . ? O4B C33B 1.200(18) . ? C33B C34B 1.50(4) . ? C34B F5B 1.358(17) . ? C34B F6B 1.358(17) . ? C34B F4B 1.393(18) . ? 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 N6 Ag1 N4 146.2(3) . . ? N6 Ag1 N2 108.0(3) . . ? N4 Ag1 N2 88.6(3) . . ? N6 Ag1 O1 91.4(2) . . ? N4 Ag1 O1 117.9(2) . . ? N2 Ag1 O1 91.7(2) . . ? N6 Ag1 Ag2 110.65(16) . . ? N4 Ag1 Ag2 70.5(2) . . ? N2 Ag1 Ag2 135.85(18) . . ? O1 Ag1 Ag2 67.12(15) . . ? O4A Ag2 N8 121.6(6) . . ? O4A Ag2 O2 92.4(6) . . ? N8 Ag2 O2 145.6(2) . . ? O4A Ag2 O4B 45.8(7) . . ? N8 Ag2 O4B 78.0(5) . . ? O2 Ag2 O4B 136.2(5) . . ? O4A Ag2 O3B 8.4(10) . . ? N8 Ag2 O3B 118.6(5) . . ? O2 Ag2 O3B 94.4(5) . . ? O4B Ag2 O3B 46.5(6) . . ? O4A Ag2 Ag1 126.8(6) . . ? N8 Ag2 Ag1 77.75(17) . . ? O2 Ag2 Ag1 77.59(17) . . ? O4B Ag2 Ag1 133.7(6) . . ? O3B Ag2 Ag1 119.2(5) . . ? C31 O1 Ag1 108.7(5) . . ? C31 O2 Ag2 109.8(6) . . ? N2 N1 C7 109.8(8) . . ? N2 N1 C15 119.1(8) . . ? C7 N1 C15 131.1(9) . . ? C1 N2 N1 107.2(8) . . ? C1 N2 Ag1 127.6(6) . . ? N1 N2 Ag1 111.5(5) . . ? N4 N3 C14 110.9(8) . . ? N4 N3 C15 119.1(8) . . ? C14 N3 C15 129.9(9) . . ? C8 N4 N3 107.1(8) . . ? C8 N4 Ag1 130.9(7) . . ? N3 N4 Ag1 120.1(6) . . ? C22 N5 N6 110.8(7) . . ? C22 N5 C30 128.1(7) . . ? N6 N5 C30 121.1(7) . . ? C16 N6 N5 106.4(7) . . ? C16 N6 Ag1 126.2(6) . . ? N5 N6 Ag1 125.2(5) . . ? N8 N7 C29 111.3(7) . . ? N8 N7 C30 120.9(7) . . ? C29 N7 C30 127.6(8) . . ? C23 N8 N7 106.9(7) . . ? C23 N8 Ag2 122.2(6) . . ? N7 N8 Ag2 129.2(5) . . ? N2 C1 C2 110.8(9) . . ? N2 C1 H1 124.6 . . ? C2 C1 H1 124.6 . . ? C7 C2 C3 119.8(9) . . ? C7 C2 C1 104.2(8) . . ? C3 C2 C1 136.0(10) . . ? C4 C3 C2 118.4(10) . . ? C4 C3 H3 120.8 . . ? C2 C3 H3 120.8 . . ? C3 C4 C5 121.3(10) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C6 C5 C4 121.9(11) . . ? C6 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? C5 C6 C7 115.5(11) . . ? C5 C6 H6 122.3 . . ? C7 C6 H6 122.3 . . ? N1 C7 C2 108.0(9) . . ? N1 C7 C6 129.0(10) . . ? C2 C7 C6 123.0(9) . . ? N4 C8 C9 110.1(10) . . ? N4 C8 H8 124.9 . . ? C9 C8 H8 124.9 . . ? C14 C9 C10 119.3(11) . . ? C14 C9 C8 105.7(9) . . ? C10 C9 C8 135.0(11) . . ? C11 C10 C9 116.6(12) . . ? C11 C10 H10 121.7 . . ? C9 C10 H10 121.7 . . ? C10 C11 C12 124.0(12) . . ? C10 C11 H11 118.0 . . ? C12 C11 H11 118.0 . . ? C13 C12 C11 120.4(12) . . ? C13 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? C14 C13 C12 115.9(12) . . ? C14 C13 H13 122.1 . . ? C12 C13 H13 122.1 . . ? N3 C14 C13 130.0(11) . . ? N3 C14 C9 106.1(9) . . ? C13 C14 C9 123.8(10) . . ? N1 C15 N3 113.4(8) . . ? N1 C15 H15A 108.9 . . ? N3 C15 H15A 108.9 . . ? N1 C15 H15B 108.9 . . ? N3 C15 H15B 108.9 . . ? H15A C15 H15B 107.7 . . ? N6 C16 C17 111.7(7) . . ? N6 C16 H16 124.2 . . ? C17 C16 H16 124.2 . . ? C16 C17 C18 135.3(9) . . ? C16 C17 C22 104.0(8) . . ? C18 C17 C22 120.6(9) . . ? C19 C18 C17 117.7(10) . . ? C19 C18 H18 121.2 . . ? C17 C18 H18 121.2 . . ? C18 C19 C20 121.3(11) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C21 C20 C19 121.7(10) . . ? C21 C20 H20 119.2 . . ? C19 C20 H20 119.2 . . ? C20 C21 C22 117.7(10) . . ? C20 C21 H21 121.1 . . ? C22 C21 H21 121.1 . . ? N5 C22 C17 107.0(8) . . ? N5 C22 C21 132.0(9) . . ? C17 C22 C21 121.0(9) . . ? N8 C23 C24 109.8(8) . . ? N8 C23 H23 125.1 . . ? C24 C23 H23 125.1 . . ? C29 C24 C23 105.9(7) . . ? C29 C24 C25 118.8(9) . . ? C23 C24 C25 135.3(9) . . ? C26 C25 C24 118.4(9) . . ? C26 C25 H25 120.8 . . ? C24 C25 H25 120.8 . . ? C25 C26 C27 121.6(9) . . ? C25 C26 H26 119.2 . . ? C27 C26 H26 119.2 . . ? C28 C27 C26 122.5(10) . . ? C28 C27 H27 118.7 . . ? C26 C27 H27 118.7 . . ? C27 C28 C29 115.1(9) . . ? C27 C28 H28 122.4 . . ? C29 C28 H28 122.4 . . ? N7 C29 C24 106.2(8) . . ? N7 C29 C28 130.3(8) . . ? C24 C29 C28 123.5(8) . . ? N5 C30 N7 112.3(6) . . ? N5 C30 H30A 109.2 . . ? N7 C30 H30A 109.2 . . ? N5 C30 H30B 109.2 . . ? N7 C30 H30B 109.2 . . ? H30A C30 H30B 107.9 . . ? O1 C31 O2 129.9(8) . . ? O1 C31 C32 115.4(8) . . ? O2 C31 C32 114.6(8) . . ? F2C C32 F1A 133.6(11) . . ? F2C C32 F3C 111.1(13) . . ? F1A C32 F2B 124.9(11) . . ? F3C C32 F2B 131.0(11) . . ? F2C C32 F2A 60.8(12) . . ? F1A C32 F2A 108.1(12) . . ? F3C C32 F2A 132.3(11) . . ? F2C C32 F1C 105.2(13) . . ? F1A C32 F1C 66.4(12) . . ? F3C C32 F1C 103.8(13) . . ? F2B C32 F1C 71.5(12) . . ? F2A C32 F1C 47.0(11) . . ? F2C C32 F1B 133.7(12) . . ? F3C C32 F1B 69.2(12) . . ? F2B C32 F1B 107.0(12) . . ? F2A C32 F1B 84.5(12) . . ? F2C C32 F3B 77.1(12) . . ? F1A C32 F3B 76.3(12) . . ? F2B C32 F3B 107.7(12) . . ? F2A C32 F3B 125.5(11) . . ? F1C C32 F3B 129.7(11) . . ? F1B C32 F3B 104.1(12) . . ? F2C C32 F3A 46.5(11) . . ? F1A C32 F3A 105.0(13) . . ? F3C C32 F3A 68.8(12) . . ? F2B C32 F3A 80.5(12) . . ? F2A C32 F3A 103.4(12) . . ? F1C C32 F3A 134.2(10) . . ? F1B C32 F3A 128.8(11) . . ? F2C C32 C31 111.2(9) . . ? F1A C32 C31 114.2(8) . . ? F3C C32 C31 113.6(9) . . ? F2B C32 C31 113.2(8) . . ? F2A C32 C31 112.5(8) . . ? F1C C32 C31 111.4(9) . . ? F1B C32 C31 110.0(8) . . ? F3B C32 C31 114.2(8) . . ? F3A C32 C31 112.8(8) . . ? C33A O4A Ag2 111(2) . . ? O4A C33A O3A 132(3) . . ? O4A C33A C34A 129(2) . . ? O3A C33A C34A 98.4(19) . . ? F5A C34A F6A 107.8(19) . . ? F5A C34A F4A 116(2) . . ? F6A C34A F4A 100.3(19) . . ? F5A C34A C33A 115(2) . . ? F6A C34A C33A 111(3) . . ? F4A C34A C33A 106.7(18) . . ? C33B O3B Ag2 98.1(17) . . ? C33B O4B Ag2 101.4(16) . . ? O3B C33B O4B 114(3) . . ? O3B C33B C34B 108.0(19) . . ? O4B C33B C34B 138(2) . . ? F5B C34B F6B 103.4(18) . . ? F5B C34B F4B 120(2) . . ? F6B C34B F4B 104.4(18) . . ? F5B C34B C33B 113(3) . . ? F6B C34B C33B 108.4(19) . . ? F4B C34B C33B 107(3) . . ? 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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N6 Ag1 Ag2 O4A 151.9(7) . . . . ? N4 Ag1 Ag2 O4A 7.8(7) . . . . ? N2 Ag1 Ag2 O4A -58.5(8) . . . . ? O1 Ag1 Ag2 O4A -125.7(7) . . . . ? N6 Ag1 Ag2 N8 31.3(3) . . . . ? N4 Ag1 Ag2 N8 -112.7(3) . . . . ? N2 Ag1 Ag2 N8 -179.0(3) . . . . ? O1 Ag1 Ag2 N8 113.8(2) . . . . ? N6 Ag1 Ag2 O2 -124.5(2) . . . . ? N4 Ag1 Ag2 O2 91.5(3) . . . . ? N2 Ag1 Ag2 O2 25.1(3) . . . . ? O1 Ag1 Ag2 O2 -42.0(2) . . . . ? N6 Ag1 Ag2 O4B 91.2(6) . . . . ? N4 Ag1 Ag2 O4B -52.8(6) . . . . ? N2 Ag1 Ag2 O4B -119.1(7) . . . . ? O1 Ag1 Ag2 O4B 173.7(6) . . . . ? N6 Ag1 Ag2 O3B 147.4(6) . . . . ? N4 Ag1 Ag2 O3B 3.4(6) . . . . ? N2 Ag1 Ag2 O3B -62.9(6) . . . . ? O1 Ag1 Ag2 O3B -130.1(6) . . . . ? N6 Ag1 O1 C31 170.6(6) . . . . ? N4 Ag1 O1 C31 8.1(7) . . . . ? N2 Ag1 O1 C31 -81.3(6) . . . . ? Ag2 Ag1 O1 C31 58.8(5) . . . . ? O4A Ag2 O2 C31 177.2(9) . . . . ? N8 Ag2 O2 C31 5.0(8) . . . . ? O4B Ag2 O2 C31 -167.5(9) . . . . ? O3B Ag2 O2 C31 169.0(8) . . . . ? Ag1 Ag2 O2 C31 50.1(5) . . . . ? C7 N1 N2 C1 0.2(9) . . . . ? C15 N1 N2 C1 178.7(7) . . . . ? C7 N1 N2 Ag1 144.2(6) . . . . ? C15 N1 N2 Ag1 -37.3(9) . . . . ? N6 Ag1 N2 C1 -21.6(8) . . . . ? N4 Ag1 N2 C1 128.5(8) . . . . ? O1 Ag1 N2 C1 -113.6(8) . . . . ? Ag2 Ag1 N2 C1 -171.7(6) . . . . ? N6 Ag1 N2 N1 -156.4(5) . . . . ? N4 Ag1 N2 N1 -6.3(6) . . . . ? O1 Ag1 N2 N1 111.5(5) . . . . ? Ag2 Ag1 N2 N1 53.4(6) . . . . ? C14 N3 N4 C8 -0.4(10) . . . . ? C15 N3 N4 C8 -179.9(8) . . . . ? C14 N3 N4 Ag1 -166.4(6) . . . . ? C15 N3 N4 Ag1 14.0(10) . . . . ? N6 Ag1 N4 C8 -23.6(11) . . . . ? N2 Ag1 N4 C8 -145.0(9) . . . . ? O1 Ag1 N4 C8 123.8(8) . . . . ? Ag2 Ag1 N4 C8 74.7(8) . . . . ? N6 Ag1 N4 N3 138.7(6) . . . . ? N2 Ag1 N4 N3 17.2(6) . . . . ? O1 Ag1 N4 N3 -74.0(7) . . . . ? Ag2 Ag1 N4 N3 -123.1(6) . . . . ? C22 N5 N6 C16 0.7(8) . . . . ? C30 N5 N6 C16 -179.7(7) . . . . ? C22 N5 N6 Ag1 164.5(5) . . . . ? C30 N5 N6 Ag1 -15.9(9) . . . . ? N4 Ag1 N6 C16 -92.0(8) . . . . ? N2 Ag1 N6 C16 24.2(7) . . . . ? O1 Ag1 N6 C16 116.4(6) . . . . ? Ag2 Ag1 N6 C16 -177.6(6) . . . . ? N4 Ag1 N6 N5 107.3(7) . . . . ? N2 Ag1 N6 N5 -136.5(6) . . . . ? O1 Ag1 N6 N5 -44.2(6) . . . . ? Ag2 Ag1 N6 N5 21.8(6) . . . . ? C29 N7 N8 C23 0.2(8) . . . . ? C30 N7 N8 C23 -175.3(7) . . . . ? C29 N7 N8 Ag2 -164.5(5) . . . . ? C30 N7 N8 Ag2 20.0(10) . . . . ? O4A Ag2 N8 C23 -0.7(10) . . . . ? O2 Ag2 N8 C23 170.3(5) . . . . ? O4B Ag2 N8 C23 -15.1(8) . . . . ? O3B Ag2 N8 C23 8.4(9) . . . . ? Ag1 Ag2 N8 C23 125.2(6) . . . . ? O4A Ag2 N8 N7 162.0(9) . . . . ? O2 Ag2 N8 N7 -27.1(9) . . . . ? O4B Ag2 N8 N7 147.6(8) . . . . ? O3B Ag2 N8 N7 171.1(8) . . . . ? Ag1 Ag2 N8 N7 -72.1(6) . . . . ? N1 N2 C1 C2 -0.2(9) . . . . ? Ag1 N2 C1 C2 -136.5(7) . . . . ? N2 C1 C2 C7 0.2(9) . . . . ? N2 C1 C2 C3 -177.8(10) . . . . ? C7 C2 C3 C4 -0.7(13) . . . . ? C1 C2 C3 C4 177.0(10) . . . . ? C2 C3 C4 C5 2.3(15) . . . . ? C3 C4 C5 C6 -1.5(17) . . . . ? C4 C5 C6 C7 -0.8(15) . . . . ? N2 N1 C7 C2 -0.1(10) . . . . ? C15 N1 C7 C2 -178.4(8) . . . . ? N2 N1 C7 C6 180.0(9) . . . . ? C15 N1 C7 C6 1.6(16) . . . . ? C3 C2 C7 N1 178.3(8) . . . . ? C1 C2 C7 N1 -0.1(9) . . . . ? C3 C2 C7 C6 -1.7(14) . . . . ? C1 C2 C7 C6 179.9(9) . . . . ? C5 C6 C7 N1 -177.6(9) . . . . ? C5 C6 C7 C2 2.4(14) . . . . ? N3 N4 C8 C9 1.0(11) . . . . ? Ag1 N4 C8 C9 164.9(7) . . . . ? N4 C8 C9 C14 -1.2(11) . . . . ? N4 C8 C9 C10 -179.8(12) . . . . ? C14 C9 C10 C11 2.6(16) . . . . ? C8 C9 C10 C11 -178.9(12) . . . . ? C9 C10 C11 C12 -2.0(18) . . . . ? C10 C11 C12 C13 0.7(19) . . . . ? C11 C12 C13 C14 0.0(16) . . . . ? N4 N3 C14 C13 -178.3(10) . . . . ? C15 N3 C14 C13 1.2(17) . . . . ? N4 N3 C14 C9 -0.4(10) . . . . ? C15 N3 C14 C9 179.2(9) . . . . ? C12 C13 C14 N3 178.4(10) . . . . ? C12 C13 C14 C9 0.8(15) . . . . ? C10 C9 C14 N3 179.7(9) . . . . ? C8 C9 C14 N3 0.9(11) . . . . ? C10 C9 C14 C13 -2.2(16) . . . . ? C8 C9 C14 C13 179.0(9) . . . . ? N2 N1 C15 N3 87.1(10) . . . . ? C7 N1 C15 N3 -94.7(12) . . . . ? N4 N3 C15 N1 -70.6(11) . . . . ? C14 N3 C15 N1 109.9(11) . . . . ? N5 N6 C16 C17 0.1(9) . . . . ? Ag1 N6 C16 C17 -163.5(5) . . . . ? N6 C16 C17 C18 179.4(10) . . . . ? N6 C16 C17 C22 -0.9(9) . . . . ? C16 C17 C18 C19 179.7(10) . . . . ? C22 C17 C18 C19 0.0(14) . . . . ? C17 C18 C19 C20 -0.4(16) . . . . ? C18 C19 C20 C21 1.1(17) . . . . ? C19 C20 C21 C22 -1.2(16) . . . . ? N6 N5 C22 C17 -1.3(9) . . . . ? C30 N5 C22 C17 179.2(7) . . . . ? N6 N5 C22 C21 -179.8(9) . . . . ? C30 N5 C22 C21 0.7(14) . . . . ? C16 C17 C22 N5 1.3(9) . . . . ? C18 C17 C22 N5 -178.9(8) . . . . ? C16 C17 C22 C21 180.0(8) . . . . ? C18 C17 C22 C21 -0.2(13) . . . . ? C20 C21 C22 N5 179.2(9) . . . . ? C20 C21 C22 C17 0.8(14) . . . . ? N7 N8 C23 C24 -0.2(9) . . . . ? Ag2 N8 C23 C24 165.8(5) . . . . ? N8 C23 C24 C29 0.1(9) . . . . ? N8 C23 C24 C25 -178.6(8) . . . . ? C29 C24 C25 C26 0.5(12) . . . . ? C23 C24 C25 C26 179.1(9) . . . . ? C24 C25 C26 C27 -1.0(13) . . . . ? C25 C26 C27 C28 1.3(14) . . . . ? C26 C27 C28 C29 -0.8(13) . . . . ? N8 N7 C29 C24 -0.1(8) . . . . ? C30 N7 C29 C24 175.0(7) . . . . ? N8 N7 C29 C28 178.9(8) . . . . ? C30 N7 C29 C28 -6.0(13) . . . . ? C23 C24 C29 N7 0.0(8) . . . . ? C25 C24 C29 N7 179.0(7) . . . . ? C23 C24 C29 C28 -179.1(8) . . . . ? C25 C24 C29 C28 -0.1(12) . . . . ? C27 C28 C29 N7 -178.6(8) . . . . ? C27 C28 C29 C24 0.3(12) . . . . ? C22 N5 C30 N7 108.5(9) . . . . ? N6 N5 C30 N7 -71.0(9) . . . . ? N8 N7 C30 N5 101.2(9) . . . . ? C29 N7 C30 N5 -73.5(10) . . . . ? Ag1 O1 C31 O2 -43.1(11) . . . . ? Ag1 O1 C31 C32 137.0(6) . . . . ? Ag2 O2 C31 O1 -14.5(12) . . . . ? Ag2 O2 C31 C32 165.4(5) . . . . ? O1 C31 C32 F2C -94.9(14) . . . . ? O2 C31 C32 F2C 85.2(14) . . . . ? O1 C31 C32 F1A 95.0(14) . . . . ? O2 C31 C32 F1A -84.9(14) . . . . ? O1 C31 C32 F3C 138.9(13) . . . . ? O2 C31 C32 F3C -41.0(15) . . . . ? O1 C31 C32 F2B -56.1(14) . . . . ? O2 C31 C32 F2B 124.0(12) . . . . ? O1 C31 C32 F2A -28.8(14) . . . . ? O2 C31 C32 F2A 151.3(12) . . . . ? O1 C31 C32 F1C 22.1(14) . . . . ? O2 C31 C32 F1C -157.8(12) . . . . ? O1 C31 C32 F1B 63.5(13) . . . . ? O2 C31 C32 F1B -116.4(12) . . . . ? O1 C31 C32 F3B -179.8(12) . . . . ? O2 C31 C32 F3B 0.3(14) . . . . ? O1 C31 C32 F3A -145.2(12) . . . . ? O2 C31 C32 F3A 34.8(14) . . . . ? N8 Ag2 O4A C33A -13(4) . . . . ? O2 Ag2 O4A C33A 172(4) . . . . ? O4B Ag2 O4A C33A 7(4) . . . . ? O3B Ag2 O4A C33A -84(7) . . . . ? Ag1 Ag2 O4A C33A -111(4) . . . . ? Ag2 O4A C33A O3A -23(9) . . . . ? Ag2 O4A C33A C34A 158(5) . . . . ? O4A C33A C34A F5A -141(6) . . . . ? O3A C33A C34A F5A 40(5) . . . . ? O4A C33A C34A F6A 97(7) . . . . ? O3A C33A C34A F6A -83(4) . . . . ? O4A C33A C34A F4A -11(7) . . . . ? O3A C33A C34A F4A 169(3) . . . . ? O4A Ag2 O3B C33B 79(7) . . . . ? N8 Ag2 O3B C33B -35(4) . . . . ? O2 Ag2 O3B C33B 156(4) . . . . ? O4B Ag2 O3B C33B -2(4) . . . . ? Ag1 Ag2 O3B C33B -126(4) . . . . ? O4A Ag2 O4B C33B -10(4) . . . . ? N8 Ag2 O4B C33B 153(4) . . . . ? O2 Ag2 O4B C33B -31(4) . . . . ? O3B Ag2 O4B C33B 2(4) . . . . ? Ag1 Ag2 O4B C33B 93(4) . . . . ? Ag2 O3B C33B O4B 3(6) . . . . ? Ag2 O3B C33B C34B -172(4) . . . . ? Ag2 O4B C33B O3B -4(6) . . . . ? Ag2 O4B C33B C34B 171(7) . . . . ? O3B C33B C34B F5B 78(5) . . . . ? O4B C33B C34B F5B -97(8) . . . . ? O3B C33B C34B F6B -168(4) . . . . ? O4B C33B C34B F6B 17(9) . . . . ? O3B C33B C34B F4B -56(5) . . . . ? O4B C33B C34B F4B 129(8) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.27 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.076 _refine_diff_density_min -1.159 _refine_diff_density_rms 0.205 data_14 _database_code_depnum_ccdc_archive 'CCDC 917673' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H12 Ag F3 N4 O2' _chemical_formula_sum 'C17 H12 Ag F3 N4 O2' _chemical_formula_weight 469.18 _chemical_absolute_configuration ad 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' 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' F F 0.0171 0.0103 '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' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M 'P 41 21 2' _symmetry_space_group_name_Hall 'P 4abw 2nw' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-y+1/2, x+1/2, z+1/4' 'y+1/2, -x+1/2, z+3/4' '-x+1/2, y+1/2, -z+1/4' 'x+1/2, -y+1/2, -z+3/4' 'y, x, -z' '-y, -x, -z+1/2' _cell_length_a 12.1082(3) _cell_length_b 12.1082(3) _cell_length_c 24.2726(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3558.57(16) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9976 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 28.60 _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.751 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1856 _exptl_absorpt_coefficient_mu 1.183 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7034 _exptl_absorpt_correction_T_max 0.7893 _exptl_absorpt_process_details ; APEX2 Software Suite; Bruker 2005. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker-Nonius X8kappa APEX II CCD area detector ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 43786 _diffrn_reflns_av_R_equivalents 0.0357 _diffrn_reflns_av_sigmaI/netI 0.0202 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.88 _diffrn_reflns_theta_max 30.51 _reflns_number_total 5443 _reflns_number_gt 4978 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker, 2007)' _computing_cell_refinement 'APEX2 Software Suite (Bruker, 2007)' _computing_data_reduction 'APEX2 Software Suite (Bruker, 2007)' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL and publCIF (Westrip, 2010)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0591P)^2^+2.0827P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.04(3) _refine_ls_number_reflns 5443 _refine_ls_number_parameters 271 _refine_ls_number_restraints 45 _refine_ls_R_factor_all 0.0407 _refine_ls_R_factor_gt 0.0354 _refine_ls_wR_factor_ref 0.0993 _refine_ls_wR_factor_gt 0.0946 _refine_ls_goodness_of_fit_ref 1.070 _refine_ls_restrained_S_all 1.110 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.27589(2) 0.89812(2) 0.746723(10) 0.03443(8) Uani 1 1 d . . . F1A F 0.1251(6) 1.1930(6) 0.8634(3) 0.0671(16) Uani 0.50 1 d PDU A 1 F2A F -0.0115(5) 1.1071(5) 0.8471(2) 0.0519(12) Uani 0.50 1 d PDU A 1 F3A F 0.0088(5) 1.2256(5) 0.7856(2) 0.0532(13) Uani 0.50 1 d PDU A 1 F1B F 0.0594(9) 1.1505(9) 0.8653(4) 0.109(3) Uani 0.50 1 d PDU A 2 F2B F -0.0474(7) 1.0914(7) 0.8209(4) 0.090(2) Uani 0.50 1 d PDU A 2 F3B F 0.0462(5) 1.2492(5) 0.7987(2) 0.0493(13) Uani 0.50 1 d PDU A 2 O1 O 0.1481(3) 0.9801(2) 0.80400(11) 0.0435(6) Uani 1 1 d . . . O2 O 0.1815(3) 1.1161(2) 0.74333(11) 0.0465(6) Uani 1 1 d . . . N1 N 0.3783(2) 0.7705(2) 0.79282(10) 0.0266(5) Uani 1 1 d . . . N2 N 0.3580(2) 0.7237(2) 0.84269(9) 0.0251(4) Uani 1 1 d . . . N3 N 0.3314(2) 0.9001(2) 0.65841(10) 0.0255(4) Uani 1 1 d . . . N4 N 0.1800(2) 0.6785(2) 0.88076(10) 0.0250(5) Uani 1 1 d . . . C1 C 0.4307(3) 0.6447(3) 0.85675(14) 0.0305(6) Uani 1 1 d . . . H1 H 0.4314 0.6027 0.8898 0.037 Uiso 1 1 calc R . . C2 C 0.5050(2) 0.6370(3) 0.81290(13) 0.0274(6) Uani 1 1 d . . . C3 C 0.5983(3) 0.5701(3) 0.80186(14) 0.0346(6) Uani 1 1 d . . . H3 H 0.6226 0.5156 0.8273 0.041 Uiso 1 1 calc R . . C4 C 0.6523(3) 0.5871(3) 0.75278(16) 0.0381(7) Uani 1 1 d . . . H4 H 0.7142 0.5422 0.7440 0.046 Uiso 1 1 calc R . . C5 C 0.6185(3) 0.6694(3) 0.71498(14) 0.0374(7) Uani 1 1 d . . . H5 H 0.6596 0.6800 0.6821 0.045 Uiso 1 1 calc R . . C6 C 0.5283(3) 0.7337(3) 0.72477(13) 0.0349(7) Uani 1 1 d . . . H6 H 0.5051 0.7879 0.6990 0.042 Uiso 1 1 calc R . . C7 C 0.4703(2) 0.7168(3) 0.77463(11) 0.0261(5) Uani 1 1 d . . . C8 C 0.2658(3) 0.7608(2) 0.87623(12) 0.0287(6) Uani 1 1 d . . . H8A H 0.2931 0.7795 0.9135 0.034 Uiso 1 1 calc R . . H8B H 0.2344 0.8288 0.8598 0.034 Uiso 1 1 calc R . . C9 C 0.3921(3) 0.8316(3) 0.57721(12) 0.0320(6) Uani 1 1 d . . . H9 H 0.3985 0.7846 0.5460 0.038 Uiso 1 1 calc R . . C10 C 0.4544(3) 0.9259(3) 0.58789(13) 0.0308(6) Uani 1 1 d . . . C11 C 0.5373(4) 0.9844(3) 0.55953(18) 0.0464(10) Uani 1 1 d . . . H11 H 0.5649 0.9594 0.5251 0.056 Uiso 1 1 calc R . . C12 C 0.5762(3) 1.0787(3) 0.5836(2) 0.0501(11) Uani 1 1 d . . . H12 H 0.6322 1.1197 0.5653 0.060 Uiso 1 1 calc R . . C13 C 0.5364(3) 1.1169(3) 0.63440(19) 0.0433(9) Uani 1 1 d . . . H13 H 0.5670 1.1824 0.6496 0.052 Uiso 1 1 calc R . . C14 C 0.4554(3) 1.0635(3) 0.66268(15) 0.0342(7) Uani 1 1 d . . . H14 H 0.4287 1.0908 0.6969 0.041 Uiso 1 1 calc R . . C15 C 0.4129(2) 0.9661(3) 0.63910(11) 0.0258(5) Uani 1 1 d . . . C16 C 0.1359(3) 1.0737(3) 0.78375(15) 0.0393(8) Uani 1 1 d . A . C17 C 0.0581(6) 1.1493(5) 0.8164(2) 0.085(2) Uani 1 1 d 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 0.04391(14) 0.03042(11) 0.02897(11) 0.00343(9) 0.00800(10) 0.00336(10) F1A 0.0685(18) 0.0669(18) 0.0658(18) -0.0049(10) 0.0011(10) 0.0021(10) F2A 0.0505(14) 0.0527(14) 0.0524(14) 0.0012(10) 0.0069(10) 0.0012(10) F3A 0.0532(15) 0.0524(16) 0.0540(15) 0.0026(10) 0.0019(10) 0.0031(10) F1B 0.110(3) 0.109(3) 0.107(3) -0.0007(10) 0.0013(10) 0.0017(11) F2B 0.088(2) 0.090(2) 0.091(2) 0.0012(10) 0.0037(10) 0.0011(10) F3B 0.0507(15) 0.0475(15) 0.0498(15) 0.0002(10) 0.0025(10) 0.0025(10) O1 0.0523(16) 0.0381(13) 0.0401(13) 0.0059(11) 0.0064(12) 0.0098(12) O2 0.0537(15) 0.0486(15) 0.0374(13) 0.0058(12) 0.0155(12) 0.0061(12) N1 0.0270(11) 0.0285(11) 0.0242(10) 0.0003(9) 0.0027(8) 0.0000(10) N2 0.0248(10) 0.0265(11) 0.0240(10) 0.0014(9) 0.0012(9) -0.0031(10) N3 0.0282(11) 0.0252(11) 0.0231(10) 0.0019(9) 0.0020(9) 0.0030(10) N4 0.0228(10) 0.0288(11) 0.0235(10) 0.0007(9) 0.0025(8) 0.0016(10) C1 0.0279(13) 0.0334(14) 0.0301(14) 0.0045(12) -0.0025(11) -0.0026(13) C2 0.0232(12) 0.0297(13) 0.0294(13) 0.0009(11) -0.0012(10) -0.0059(11) C3 0.0282(14) 0.0331(15) 0.0423(16) 0.0026(13) -0.0026(13) 0.0037(13) C4 0.0257(13) 0.0428(17) 0.0458(17) -0.0040(17) 0.0029(14) 0.0041(13) C5 0.0312(16) 0.0499(19) 0.0311(14) -0.0015(14) 0.0052(12) 0.0022(15) C6 0.0300(14) 0.0448(18) 0.0299(13) 0.0034(13) 0.0028(11) -0.0001(15) C7 0.0220(12) 0.0293(14) 0.0271(12) -0.0007(11) -0.0005(10) -0.0061(11) C8 0.0317(13) 0.0284(13) 0.0260(12) -0.0022(10) 0.0050(11) -0.0031(13) C9 0.0468(18) 0.0251(13) 0.0240(12) 0.0002(10) 0.0112(13) 0.0017(14) C10 0.0331(16) 0.0263(14) 0.0329(14) 0.0030(11) 0.0090(12) 0.0011(12) C11 0.050(2) 0.0351(17) 0.054(2) 0.0065(16) 0.0256(19) 0.0009(17) C12 0.0366(19) 0.0358(19) 0.078(3) 0.0114(19) 0.0155(19) -0.0039(16) C13 0.0362(17) 0.0302(16) 0.064(2) 0.0050(16) -0.0052(16) -0.0049(14) C14 0.0369(17) 0.0268(14) 0.0388(16) 0.0000(12) -0.0069(14) 0.0021(13) C15 0.0257(13) 0.0253(13) 0.0265(12) 0.0040(10) -0.0008(11) 0.0034(11) C16 0.0417(18) 0.0431(18) 0.0331(15) 0.0056(14) 0.0081(13) 0.0103(16) C17 0.118(5) 0.070(3) 0.067(3) 0.037(3) 0.061(4) 0.047(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N3 2.247(2) . ? Ag1 N1 2.275(3) . ? Ag1 O1 2.305(3) . ? Ag1 Ag1 2.9840(5) 8_666 ? F1A C17 1.496(9) . ? F2A C17 1.235(7) . ? F3A C17 1.331(7) . ? F1B C17 1.187(10) . ? F2B C17 1.462(10) . ? F3B C17 1.292(7) . ? O1 C16 1.244(5) . ? O2 C16 1.237(4) . ? N1 N2 1.360(3) . ? N1 C7 1.362(4) . ? N2 C1 1.344(4) . ? N2 C8 1.453(4) . ? N3 C15 1.353(4) . ? N3 N4 1.364(4) 8_666 ? N4 C9 1.339(4) 8_666 ? N4 N3 1.364(4) 8_666 ? N4 C8 1.444(4) . ? C1 C2 1.397(4) . ? C1 H1 0.9500 . ? C2 C7 1.405(4) . ? C2 C3 1.415(4) . ? C3 C4 1.374(5) . ? C3 H3 0.9500 . ? C4 C5 1.415(5) . ? C4 H4 0.9500 . ? C5 C6 1.363(5) . ? C5 H5 0.9500 . ? C6 C7 1.414(4) . ? C6 H6 0.9500 . ? C8 H8A 0.9900 . ? C8 H8B 0.9900 . ? C9 N4 1.339(4) 8_666 ? C9 C10 1.393(5) . ? C9 H9 0.9500 . ? C10 C11 1.407(5) . ? C10 C15 1.426(4) . ? C11 C12 1.367(6) . ? C11 H11 0.9500 . ? C12 C13 1.403(7) . ? C12 H12 0.9500 . ? C13 C14 1.361(5) . ? C13 H13 0.9500 . ? C14 C15 1.408(5) . ? C14 H14 0.9500 . ? C16 C17 1.534(6) . ? 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 N3 Ag1 N1 108.26(9) . . ? N3 Ag1 O1 140.52(9) . . ? N1 Ag1 O1 111.21(9) . . ? N3 Ag1 Ag1 105.65(7) . 8_666 ? N1 Ag1 Ag1 83.07(6) . 8_666 ? O1 Ag1 Ag1 78.34(8) . 8_666 ? C16 O1 Ag1 103.5(2) . . ? N2 N1 C7 103.7(2) . . ? N2 N1 Ag1 128.48(19) . . ? C7 N1 Ag1 127.59(19) . . ? C1 N2 N1 113.8(3) . . ? C1 N2 C8 125.6(3) . . ? N1 N2 C8 120.6(2) . . ? C15 N3 N4 104.1(2) . 8_666 ? C15 N3 Ag1 123.7(2) . . ? N4 N3 Ag1 129.1(2) 8_666 . ? C9 N4 N3 113.6(3) 8_666 8_666 ? C9 N4 C8 125.1(3) 8_666 . ? N3 N4 C8 121.3(2) 8_666 . ? N2 C1 C2 106.1(3) . . ? N2 C1 H1 127.0 . . ? C2 C1 H1 127.0 . . ? C1 C2 C7 105.3(3) . . ? C1 C2 C3 134.2(3) . . ? C7 C2 C3 120.5(3) . . ? C4 C3 C2 117.3(3) . . ? C4 C3 H3 121.4 . . ? C2 C3 H3 121.4 . . ? C3 C4 C5 122.0(3) . . ? C3 C4 H4 119.0 . . ? C5 C4 H4 119.0 . . ? C6 C5 C4 121.4(3) . . ? C6 C5 H5 119.3 . . ? C4 C5 H5 119.3 . . ? C5 C6 C7 117.7(3) . . ? C5 C6 H6 121.1 . . ? C7 C6 H6 121.1 . . ? N1 C7 C2 111.0(3) . . ? N1 C7 C6 127.9(3) . . ? C2 C7 C6 121.1(3) . . ? N4 C8 N2 112.4(2) . . ? N4 C8 H8A 109.1 . . ? N2 C8 H8A 109.1 . . ? N4 C8 H8B 109.1 . . ? N2 C8 H8B 109.1 . . ? H8A C8 H8B 107.9 . . ? N4 C9 C10 106.9(3) 8_666 . ? N4 C9 H9 126.5 8_666 . ? C10 C9 H9 126.5 . . ? C9 C10 C11 135.0(3) . . ? C9 C10 C15 104.5(3) . . ? C11 C10 C15 120.4(3) . . ? C12 C11 C10 117.2(4) . . ? C12 C11 H11 121.4 . . ? C10 C11 H11 121.4 . . ? C11 C12 C13 122.2(4) . . ? C11 C12 H12 118.9 . . ? C13 C12 H12 118.9 . . ? C14 C13 C12 122.3(4) . . ? C14 C13 H13 118.9 . . ? C12 C13 H13 118.9 . . ? C13 C14 C15 117.2(3) . . ? C13 C14 H14 121.4 . . ? C15 C14 H14 121.4 . . ? N3 C15 C14 128.3(3) . . ? N3 C15 C10 110.9(3) . . ? C14 C15 C10 120.7(3) . . ? O2 C16 O1 129.7(4) . . ? O2 C16 C17 115.9(4) . . ? O1 C16 C17 114.3(3) . . ? F1B C17 F2A 53.9(6) . . ? F1B C17 F3B 108.8(7) . . ? F2A C17 F3B 120.7(6) . . ? F1B C17 F3A 124.0(7) . . ? F2A C17 F3A 108.6(6) . . ? F1B C17 F2B 86.7(7) . . ? F3B C17 F2B 112.1(6) . . ? F3A C17 F2B 89.0(6) . . ? F2A C17 F1A 93.2(5) . . ? F3B C17 F1A 89.0(6) . . ? F3A C17 F1A 115.3(6) . . ? F2B C17 F1A 125.9(5) . . ? F1B C17 C16 121.1(7) . . ? F2A C17 C16 118.9(5) . . ? F3B C17 C16 117.1(4) . . ? F3A C17 C16 113.5(4) . . ? F2B C17 C16 106.8(6) . . ? F1A C17 C16 105.8(5) . . ? 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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Ag1 O1 C16 -30.7(3) . . . . ? N1 Ag1 O1 C16 151.0(3) . . . . ? Ag1 Ag1 O1 C16 -131.2(3) 8_666 . . . ? N3 Ag1 N1 N2 -163.7(2) . . . . ? O1 Ag1 N1 N2 15.2(3) . . . . ? Ag1 Ag1 N1 N2 -59.4(2) 8_666 . . . ? N3 Ag1 N1 C7 10.6(3) . . . . ? O1 Ag1 N1 C7 -170.5(2) . . . . ? Ag1 Ag1 N1 C7 114.9(2) 8_666 . . . ? C7 N1 N2 C1 0.0(3) . . . . ? Ag1 N1 N2 C1 175.4(2) . . . . ? C7 N1 N2 C8 178.9(3) . . . . ? Ag1 N1 N2 C8 -5.8(4) . . . . ? N1 Ag1 N3 C15 -90.0(2) . . . . ? O1 Ag1 N3 C15 91.7(3) . . . . ? Ag1 Ag1 N3 C15 -177.7(2) 8_666 . . . ? N1 Ag1 N3 N4 66.8(3) . . . 8_666 ? O1 Ag1 N3 N4 -111.5(3) . . . 8_666 ? Ag1 Ag1 N3 N4 -20.9(3) 8_666 . . 8_666 ? N1 N2 C1 C2 -0.6(4) . . . . ? C8 N2 C1 C2 -179.4(3) . . . . ? N2 C1 C2 C7 0.9(3) . . . . ? N2 C1 C2 C3 -179.0(3) . . . . ? C1 C2 C3 C4 -179.9(4) . . . . ? C7 C2 C3 C4 0.2(5) . . . . ? C2 C3 C4 C5 1.3(5) . . . . ? C3 C4 C5 C6 -2.1(6) . . . . ? C4 C5 C6 C7 1.1(6) . . . . ? N2 N1 C7 C2 0.6(3) . . . . ? Ag1 N1 C7 C2 -174.8(2) . . . . ? N2 N1 C7 C6 -179.4(3) . . . . ? Ag1 N1 C7 C6 5.3(5) . . . . ? C1 C2 C7 N1 -1.0(3) . . . . ? C3 C2 C7 N1 179.0(3) . . . . ? C1 C2 C7 C6 179.0(3) . . . . ? C3 C2 C7 C6 -1.1(5) . . . . ? C5 C6 C7 N1 -179.6(3) . . . . ? C5 C6 C7 C2 0.4(5) . . . . ? C9 N4 C8 N2 96.9(3) 8_666 . . . ? N3 N4 C8 N2 -84.9(3) 8_666 . . . ? C1 N2 C8 N4 -69.7(4) . . . . ? N1 N2 C8 N4 111.6(3) . . . . ? N4 C9 C10 C11 -176.9(4) 8_666 . . . ? N4 C9 C10 C15 -0.1(4) 8_666 . . . ? C9 C10 C11 C12 177.4(4) . . . . ? C15 C10 C11 C12 1.0(6) . . . . ? C10 C11 C12 C13 0.0(7) . . . . ? C11 C12 C13 C14 -0.8(7) . . . . ? C12 C13 C14 C15 0.6(6) . . . . ? N4 N3 C15 C14 178.4(3) 8_666 . . . ? Ag1 N3 C15 C14 -19.9(4) . . . . ? N4 N3 C15 C10 -0.6(3) 8_666 . . . ? Ag1 N3 C15 C10 161.1(2) . . . . ? C13 C14 C15 N3 -178.5(3) . . . . ? C13 C14 C15 C10 0.4(5) . . . . ? C9 C10 C15 N3 0.5(4) . . . . ? C11 C10 C15 N3 177.8(3) . . . . ? C9 C10 C15 C14 -178.6(3) . . . . ? C11 C10 C15 C14 -1.3(5) . . . . ? Ag1 O1 C16 O2 -1.2(6) . . . . ? Ag1 O1 C16 C17 -176.8(4) . . . . ? O2 C16 C17 F1B -136.3(9) . . . . ? O1 C16 C17 F1B 39.9(11) . . . . ? O2 C16 C17 F2A 160.6(6) . . . . ? O1 C16 C17 F2A -23.2(9) . . . . ? O2 C16 C17 F3B 0.7(9) . . . . ? O1 C16 C17 F3B 177.0(6) . . . . ? O2 C16 C17 F3A 30.9(8) . . . . ? O1 C16 C17 F3A -152.8(6) . . . . ? O2 C16 C17 F2B 127.3(5) . . . . ? O1 C16 C17 F2B -56.5(7) . . . . ? O2 C16 C17 F1A -96.5(5) . . . . ? O1 C16 C17 F1A 79.7(6) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.51 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.046 _refine_diff_density_min -0.496 _refine_diff_density_rms 0.094 data_15 _database_code_depnum_ccdc_archive 'CCDC 917674' # start Validation Reply Form ================================================ _vrf_PLAT601_15 ; PROBLEM: Structure Contains Solvent Accessible VOIDS of . 263 A**3 RESPONSE: A search for solvent-accessible voids in the crystal structure using PLATON showed a potential solvent volume of 1081 Ang^3^ and subsequent application of SQUEEZE procedures showed four relevant voids each with a solvent-accessible volume of 269 Ang^3^. However, this procedure showed no electrons in the voids. This indicates that the crystal lost nearly all of its solvent of crystallization by the time it was used for data collection, without collapse of the structure. ; # end Validation Reply Form ================================================== _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H24 Ag N8, C H3 O3 S' _chemical_formula_sum 'C31 H27 Ag N8 O3 S' _chemical_formula_weight 699.54 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' 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' S S 0.1246 0.1234 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_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' _cell_length_a 43.4103(9) _cell_length_b 12.3013(3) _cell_length_c 19.7415(4) _cell_angle_alpha 90.00 _cell_angle_beta 112.0110(10) _cell_angle_gamma 90.00 _cell_volume 9773.6(4) _cell_formula_units_Z 12 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9930 _cell_measurement_theta_min 2.38 _cell_measurement_theta_max 30.14 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.426 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4272 _exptl_absorpt_coefficient_mu 0.727 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8743 _exptl_absorpt_correction_T_max 0.8864 _exptl_absorpt_process_details ; APEX2 Software Suite; Bruker 2005. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker-Nonius X8kappa APEX II CCD area detector ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 46746 _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_sigmaI/netI 0.0290 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 52 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.07 _diffrn_reflns_theta_max 25.25 _reflns_number_total 8815 _reflns_number_gt 6585 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker, 2007)' _computing_cell_refinement 'APEX2 Software Suite (Bruker, 2007)' _computing_data_reduction 'APEX2 Software Suite (Bruker, 2007)' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL and publCIF (Westrip, 2010)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1627P)^2^+48.3179P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8815 _refine_ls_number_parameters 619 _refine_ls_number_restraints 127 _refine_ls_R_factor_all 0.0989 _refine_ls_R_factor_gt 0.0643 _refine_ls_wR_factor_ref 0.2100 _refine_ls_wR_factor_gt 0.1459 _refine_ls_goodness_of_fit_ref 1.106 _refine_ls_restrained_S_all 1.119 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.772572(14) 0.43832(5) 0.43938(3) 0.0487(2) Uani 1 1 d . . . N1 N 0.73794(11) 0.4774(4) 0.2673(2) 0.0306(10) Uani 1 1 d . . . N2 N 0.76703(13) 0.4452(4) 0.3215(3) 0.0369(12) Uani 1 1 d . . . N3 N 0.69594(12) 0.4825(4) 0.3183(2) 0.0308(10) Uani 1 1 d . . . N4 N 0.70956(13) 0.4594(4) 0.3917(3) 0.0346(11) Uani 1 1 d . . . N5 N 0.81305(12) 0.3803(4) 0.6048(2) 0.0322(11) Uani 1 1 d . . . N6 N 0.78290(12) 0.3625(4) 0.5499(3) 0.0320(10) Uani 1 1 d . . . N7 N 0.83840(14) 0.5359(4) 0.5718(3) 0.0352(11) Uani 1 1 d . . . N8 N 0.81764(15) 0.5727(4) 0.5057(3) 0.0436(13) Uani 1 1 d . . . C1 C 0.78497(16) 0.3972(6) 0.2899(4) 0.0409(15) Uani 1 1 d . . . H1 H 0.8063 0.3667 0.3152 0.049 Uiso 1 1 d R . . C2 C 0.76850(15) 0.3967(5) 0.2136(3) 0.0346(13) Uani 1 1 d . . . C3 C 0.77578(18) 0.3572(6) 0.1537(4) 0.0452(16) Uani 1 1 d . . . H3 H 0.7961 0.3204 0.1615 0.054 Uiso 1 1 d R . . C4 C 0.7525(2) 0.3738(6) 0.0846(4) 0.056(2) Uani 1 1 d . . . H4 H 0.7571 0.3491 0.0438 0.067 Uiso 1 1 d R . . C5 C 0.7225(2) 0.4278(6) 0.0739(4) 0.0477(17) Uani 1 1 d . . . H5 H 0.7072 0.4379 0.0253 0.057 Uiso 1 1 d R . . C6 C 0.71457(16) 0.4662(5) 0.1302(3) 0.0386(14) Uani 1 1 d . . . H6 H 0.6940 0.5014 0.1220 0.046 Uiso 1 1 d R . . C7 C 0.73801(15) 0.4497(5) 0.2005(3) 0.0309(12) Uani 1 1 d . . . C8 C 0.68694(15) 0.4020(5) 0.4066(3) 0.0333(13) Uani 1 1 d . . . H8 H 0.6898 0.3744 0.4535 0.040 Uiso 1 1 d R . . C9 C 0.65813(14) 0.3867(5) 0.3428(3) 0.0304(12) Uani 1 1 d . . . C10 C 0.62695(15) 0.3357(5) 0.3264(3) 0.0372(14) Uani 1 1 d . . . H10 H 0.6218 0.3005 0.3637 0.045 Uiso 1 1 d R . . C11 C 0.60474(15) 0.3394(6) 0.2573(4) 0.0414(15) Uani 1 1 d . . . H11 H 0.5838 0.3047 0.2457 0.050 Uiso 1 1 d R . . C12 C 0.61199(16) 0.3920(6) 0.2015(3) 0.0435(15) Uani 1 1 d . . . H12 H 0.5956 0.3934 0.1534 0.052 Uiso 1 1 d R . . C13 C 0.64194(15) 0.4423(5) 0.2149(3) 0.0335(13) Uani 1 1 d . . . H13 H 0.6468 0.4773 0.1773 0.040 Uiso 1 1 d R . . C14 C 0.66491(14) 0.4388(4) 0.2867(3) 0.0296(12) Uani 1 1 d . . . C15 C 0.71480(15) 0.5435(5) 0.2851(3) 0.0334(13) Uani 1 1 d . . . H15A H 0.6994 0.5787 0.2401 0.040 Uiso 1 1 d R . . H15B H 0.7271 0.6017 0.3192 0.040 Uiso 1 1 d R . . C16 C 0.76229(16) 0.3331(5) 0.5830(3) 0.0355(13) Uani 1 1 d . . . H16 H 0.7395 0.3155 0.5580 0.043 Uiso 1 1 d R . . C17 C 0.77872(16) 0.3309(5) 0.6586(3) 0.0356(13) Uani 1 1 d . . . C18 C 0.7692(2) 0.3061(5) 0.7180(4) 0.0456(16) Uani 1 1 d . . . H18 H 0.7471 0.2842 0.7100 0.055 Uiso 1 1 d R . . C19 C 0.7927(2) 0.3157(6) 0.7862(4) 0.057(2) Uani 1 1 d . . . H19 H 0.7871 0.2976 0.8270 0.069 Uiso 1 1 d R . . C20 C 0.8249(2) 0.3493(6) 0.7985(4) 0.054(2) Uani 1 1 d . . . H20 H 0.8401 0.3575 0.8476 0.065 Uiso 1 1 d R . . C21 C 0.83581(19) 0.3741(5) 0.7422(3) 0.0456(16) Uani 1 1 d . . . H21 H 0.8580 0.3958 0.7511 0.055 Uiso 1 1 d R . . C22 C 0.81159(16) 0.3637(4) 0.6716(3) 0.0343(13) Uani 1 1 d . . . C23 C 0.81776(18) 0.6799(6) 0.5108(4) 0.0466(16) Uani 1 1 d . . . H23 H 0.8052 0.7272 0.4723 0.056 Uiso 1 1 d R . . C24 C 0.83878(15) 0.7152(5) 0.5822(4) 0.0387(14) Uani 1 1 d . . . C25 C 0.84888(18) 0.8160(6) 0.6166(4) 0.0495(17) Uani 1 1 d . . . H25 H 0.8413 0.8824 0.5912 0.059 Uiso 1 1 d R . . C26 C 0.87007(19) 0.8150(7) 0.6879(5) 0.058(2) Uani 1 1 d . . . H26 H 0.8766 0.8821 0.7130 0.069 Uiso 1 1 d R . . C27 C 0.8823(2) 0.7175(7) 0.7255(4) 0.0562(19) Uani 1 1 d . . . H27 H 0.8970 0.7205 0.7752 0.067 Uiso 1 1 d R . . C28 C 0.87355(19) 0.6175(6) 0.6918(4) 0.0494(17) Uani 1 1 d . . . H28 H 0.8824 0.5517 0.7167 0.059 Uiso 1 1 d R . . C29 C 0.85190(14) 0.6188(5) 0.6202(3) 0.0322(12) Uani 1 1 d . . . C30 C 0.84033(17) 0.4204(5) 0.5864(4) 0.0384(14) Uani 1 1 d . . . H30A H 0.8404 0.3811 0.5427 0.046 Uiso 1 1 d R . . H30B H 0.8615 0.4042 0.6272 0.046 Uiso 1 1 d R . . Ag2 Ag 0.5000 0.45777(9) 0.2500 0.0660(3) Uani 1 2 d S . . N9 N 0.53771(12) 0.4015(4) 0.4158(3) 0.0321(11) Uani 1 1 d . . . N10 N 0.50781(13) 0.3869(5) 0.3613(3) 0.0406(12) Uani 1 1 d . . . N11 N 0.56662(13) 0.5432(4) 0.3789(3) 0.0355(12) Uani 1 1 d . . . N12 N 0.45464(13) 0.5801(5) 0.1877(3) 0.0404(13) Uani 1 1 d . . . C31 C 0.48644(16) 0.3624(6) 0.3925(4) 0.0467(16) Uani 1 1 d . . . H31 H 0.4635 0.3479 0.3669 0.056 Uiso 1 1 d R . . C32 C 0.50227(15) 0.3605(6) 0.4690(3) 0.0393(14) Uani 1 1 d . . . C33 C 0.49247(18) 0.3390(7) 0.5280(4) 0.0520(18) Uani 1 1 d . . . H33 H 0.4702 0.3187 0.5195 0.062 Uiso 1 1 d R . . C34 C 0.51575(19) 0.3485(6) 0.5974(4) 0.0511(18) Uani 1 1 d . . . H34 H 0.5094 0.3355 0.6378 0.061 Uiso 1 1 d R . . C35 C 0.54927(17) 0.3769(6) 0.6108(4) 0.0464(16) Uani 1 1 d . . . H35 H 0.5648 0.3834 0.6596 0.056 Uiso 1 1 d R . . C36 C 0.55965(15) 0.3946(5) 0.5532(3) 0.0358(13) Uani 1 1 d . . . H36 H 0.5821 0.4122 0.5616 0.043 Uiso 1 1 d R . . C37 C 0.53575(14) 0.3870(5) 0.4829(3) 0.0316(12) Uani 1 1 d . . . C38 C 0.45342(17) 0.6871(6) 0.1842(4) 0.0450(16) Uani 1 1 d . . . H38 H 0.4656 0.7338 0.2234 0.054 Uiso 1 1 d R . . C39 C 0.56833(16) 0.7237(6) 0.3856(4) 0.0418(15) Uani 1 1 d . . . C40 C 0.5787(2) 0.8232(6) 0.4191(5) 0.0556(19) Uani 1 1 d . . . H40 H 0.5710 0.8894 0.3935 0.067 Uiso 1 1 d R . . C41 C 0.6002(3) 0.8247(8) 0.4903(5) 0.076(3) Uani 1 1 d . . . H41 H 0.6079 0.8919 0.5143 0.091 Uiso 1 1 d R . . C42 C 0.6115(2) 0.7291(8) 0.5279(4) 0.076(3) Uani 1 1 d . . . H42 H 0.6263 0.7330 0.5775 0.092 Uiso 1 1 d R . . C43 C 0.60260(19) 0.6291(7) 0.4982(4) 0.054(2) Uani 1 1 d . . . H43 H 0.6107 0.5641 0.5249 0.065 Uiso 1 1 d R . . C44 C 0.58048(15) 0.6276(6) 0.4248(3) 0.0396(14) Uani 1 1 d . . . C45 C 0.56617(14) 0.4285(5) 0.3966(3) 0.0348(13) Uani 1 1 d . . . H45A H 0.5869 0.4107 0.4382 0.042 Uiso 1 1 d R . . H45B H 0.5655 0.3839 0.3543 0.042 Uiso 1 1 d R . . S1 S 0.84820(4) 0.20911(15) 0.43060(9) 0.0458(4) Uani 1 1 d U . . O1 O 0.8345(2) 0.1835(6) 0.3512(4) 0.091(2) Uani 1 1 d U . . O2 O 0.82083(13) 0.2497(5) 0.4449(4) 0.0664(15) Uani 1 1 d U . . O3 O 0.86327(17) 0.1099(7) 0.4645(5) 0.110(3) Uani 1 1 d U . . C46 C 0.8749(3) 0.3110(10) 0.4354(8) 0.105(4) Uani 1 1 d U . . H46A H 0.8713 0.3381 0.3864 0.157 Uiso 1 1 d R . . H46B H 0.8977 0.2836 0.4584 0.157 Uiso 1 1 d R . . H46C H 0.8714 0.3702 0.4650 0.157 Uiso 1 1 d R . . S2 S 0.55204(9) 0.1223(3) 0.3254(2) 0.0691(11) Uani 0.50 1 d PDU A -1 O6 O 0.58558(14) 0.1304(12) 0.3764(6) 0.093(2) Uani 0.50 1 d PDU A -1 O5 O 0.5505(4) 0.0170(7) 0.2935(8) 0.099(3) Uani 0.50 1 d PDU A -1 O4 O 0.5337(3) 0.1027(14) 0.3711(7) 0.097(2) Uani 0.50 1 d PDU A -1 C47 C 0.5214(3) 0.2158(12) 0.2765(9) 0.074(3) Uani 0.50 1 d PDU A -1 H47A H 0.5201 0.2870 0.2975 0.110 Uiso 0.50 1 d PR A -1 H47B H 0.4982 0.1909 0.2498 0.110 Uiso 0.50 1 d PR A -1 H47C H 0.5347 0.2218 0.2460 0.110 Uiso 0.50 1 d PR A -1 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 0.0604(4) 0.0536(4) 0.0207(3) 0.0024(2) 0.0021(2) -0.0094(2) N1 0.029(2) 0.039(3) 0.021(2) 0.003(2) 0.0062(19) -0.003(2) N2 0.033(3) 0.048(3) 0.027(3) 0.010(2) 0.008(2) 0.004(2) N3 0.032(3) 0.038(3) 0.023(2) -0.001(2) 0.0099(19) 0.000(2) N4 0.040(3) 0.041(3) 0.021(2) 0.001(2) 0.010(2) 0.006(2) N5 0.040(3) 0.032(3) 0.021(2) -0.0002(19) 0.007(2) 0.004(2) N6 0.036(3) 0.029(2) 0.027(2) -0.0023(19) 0.008(2) 0.003(2) N7 0.046(3) 0.027(3) 0.031(3) 0.000(2) 0.013(2) 0.000(2) N8 0.053(3) 0.038(3) 0.029(3) -0.002(2) 0.003(2) -0.003(2) C1 0.036(3) 0.046(4) 0.041(4) 0.012(3) 0.016(3) 0.005(3) C2 0.035(3) 0.034(3) 0.037(3) 0.003(3) 0.016(3) -0.004(3) C3 0.056(4) 0.044(4) 0.049(4) -0.001(3) 0.034(3) -0.005(3) C4 0.083(6) 0.051(4) 0.049(4) -0.011(3) 0.044(4) -0.020(4) C5 0.072(5) 0.040(4) 0.027(3) 0.001(3) 0.013(3) -0.015(3) C6 0.042(3) 0.036(3) 0.031(3) 0.008(3) 0.006(3) -0.007(3) C7 0.034(3) 0.031(3) 0.027(3) 0.003(2) 0.011(2) -0.008(2) C8 0.039(3) 0.037(3) 0.024(3) 0.004(2) 0.013(2) 0.011(3) C9 0.039(3) 0.026(3) 0.027(3) 0.002(2) 0.013(2) 0.010(2) C10 0.038(3) 0.040(3) 0.039(3) 0.005(3) 0.020(3) 0.010(3) C11 0.027(3) 0.049(4) 0.045(4) 0.000(3) 0.010(3) 0.004(3) C12 0.034(3) 0.063(4) 0.028(3) 0.000(3) 0.006(3) 0.002(3) C13 0.037(3) 0.039(3) 0.023(3) 0.002(2) 0.010(2) 0.002(3) C14 0.036(3) 0.030(3) 0.024(3) 0.000(2) 0.011(2) 0.002(2) C15 0.037(3) 0.031(3) 0.033(3) 0.002(2) 0.013(3) 0.002(2) C16 0.039(3) 0.028(3) 0.040(3) 0.000(2) 0.015(3) 0.005(2) C17 0.055(4) 0.022(3) 0.033(3) 0.001(2) 0.019(3) 0.006(3) C18 0.079(5) 0.027(3) 0.041(4) 0.002(3) 0.034(4) 0.003(3) C19 0.107(7) 0.034(4) 0.040(4) 0.010(3) 0.037(4) 0.013(4) C20 0.089(6) 0.045(4) 0.023(3) 0.006(3) 0.014(3) 0.018(4) C21 0.058(4) 0.036(3) 0.030(3) -0.001(3) 0.003(3) 0.009(3) C22 0.054(4) 0.021(3) 0.028(3) 0.003(2) 0.016(3) 0.005(3) C23 0.053(4) 0.038(4) 0.037(4) 0.007(3) 0.004(3) 0.004(3) C24 0.033(3) 0.033(3) 0.046(4) -0.002(3) 0.011(3) 0.001(3) C25 0.044(4) 0.038(4) 0.059(5) -0.012(3) 0.011(3) 0.003(3) C26 0.048(4) 0.058(5) 0.062(5) -0.028(4) 0.015(4) -0.010(4) C27 0.061(5) 0.056(5) 0.041(4) -0.016(3) 0.008(3) -0.013(4) C28 0.056(4) 0.049(4) 0.036(4) -0.001(3) 0.008(3) -0.013(3) C29 0.028(3) 0.038(3) 0.029(3) -0.005(2) 0.010(2) 0.001(2) C30 0.046(4) 0.032(3) 0.039(3) -0.001(3) 0.019(3) 0.005(3) Ag2 0.0620(6) 0.1005(8) 0.0209(4) 0.000 -0.0009(4) 0.000 N9 0.027(2) 0.046(3) 0.021(2) 0.005(2) 0.0069(19) 0.006(2) N10 0.030(3) 0.059(4) 0.026(3) 0.000(2) 0.002(2) -0.001(2) N11 0.035(3) 0.049(3) 0.022(2) 0.006(2) 0.010(2) 0.007(2) N12 0.034(3) 0.058(4) 0.025(3) -0.007(2) 0.006(2) 0.001(2) C31 0.026(3) 0.068(5) 0.039(4) 0.002(3) 0.004(3) 0.002(3) C32 0.034(3) 0.049(4) 0.037(3) 0.000(3) 0.014(3) 0.000(3) C33 0.041(4) 0.070(5) 0.052(4) 0.004(4) 0.026(3) 0.001(3) C34 0.061(4) 0.063(5) 0.038(4) 0.005(3) 0.028(3) 0.004(4) C35 0.045(4) 0.059(4) 0.032(3) 0.000(3) 0.009(3) 0.007(3) C36 0.032(3) 0.047(4) 0.027(3) 0.005(3) 0.009(2) 0.006(3) C37 0.036(3) 0.033(3) 0.028(3) 0.002(2) 0.014(2) 0.006(2) C38 0.042(4) 0.059(5) 0.034(3) -0.013(3) 0.014(3) 0.000(3) C39 0.037(3) 0.059(4) 0.034(3) 0.007(3) 0.020(3) 0.000(3) C40 0.066(5) 0.044(4) 0.068(5) 0.003(4) 0.038(4) -0.006(4) C41 0.103(7) 0.078(6) 0.057(5) -0.022(5) 0.041(5) -0.046(6) C42 0.092(7) 0.096(7) 0.033(4) -0.006(4) 0.014(4) -0.058(6) C43 0.055(4) 0.072(5) 0.030(3) 0.002(3) 0.010(3) -0.029(4) C44 0.036(3) 0.056(4) 0.030(3) 0.006(3) 0.016(3) -0.005(3) C45 0.027(3) 0.047(4) 0.032(3) 0.003(3) 0.013(2) 0.005(3) S1 0.0519(10) 0.0523(10) 0.0391(9) 0.0072(7) 0.0240(8) 0.0188(8) O1 0.123(6) 0.087(5) 0.073(4) -0.029(4) 0.050(4) -0.026(4) O2 0.044(3) 0.061(3) 0.092(4) -0.019(3) 0.024(3) 0.001(2) O3 0.056(4) 0.092(5) 0.164(7) 0.040(5) 0.022(4) 0.018(4) C46 0.065(6) 0.091(7) 0.157(10) -0.034(7) 0.040(6) -0.017(5) S2 0.0643(17) 0.0703(18) 0.0743(18) 0.0035(14) 0.0277(14) 0.0018(14) O6 0.089(3) 0.094(3) 0.093(3) 0.0027(19) 0.0296(18) -0.0015(19) O5 0.102(3) 0.095(3) 0.099(3) -0.0029(19) 0.0356(19) 0.0038(19) O4 0.100(3) 0.099(3) 0.096(3) 0.0046(18) 0.040(2) -0.0001(19) C47 0.078(3) 0.070(3) 0.070(3) -0.003(2) 0.0241(19) -0.0091(19) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 2.250(5) . ? Ag1 N6 2.258(5) . ? Ag1 N8 2.521(6) . ? Ag1 N4 2.551(5) . ? N1 C7 1.363(7) . ? N1 N2 1.372(7) . ? N1 C15 1.435(8) . ? N2 C1 1.307(9) . ? N3 C14 1.365(8) . ? N3 N4 1.374(7) . ? N3 C15 1.437(8) . ? N4 C8 1.329(8) . ? N5 C22 1.359(7) . ? N5 N6 1.369(7) . ? N5 C30 1.449(8) . ? N6 C16 1.340(8) . ? N7 N8 1.355(7) . ? N7 C29 1.370(8) . ? N7 C30 1.446(8) . ? N8 C23 1.322(9) . ? C1 C2 1.404(9) . ? C1 H1 0.9500 . ? C2 C7 1.410(9) . ? C2 C3 1.419(9) . ? C3 C4 1.375(11) . ? C3 H3 0.9500 . ? C4 C5 1.405(12) . ? C4 H4 0.9500 . ? C5 C6 1.366(10) . ? C5 H5 0.9500 . ? C6 C7 1.394(8) . ? C6 H6 0.9500 . ? C8 C9 1.416(8) . ? C8 H8 0.9500 . ? C9 C14 1.403(8) . ? C9 C10 1.415(9) . ? C10 C11 1.345(9) . ? C10 H10 0.9500 . ? C11 C12 1.411(10) . ? C11 H11 0.9500 . ? C12 C13 1.373(9) . ? C12 H12 0.9500 . ? C13 C14 1.394(8) . ? C13 H13 0.9500 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.394(9) . ? C16 H16 0.9500 . ? C17 C22 1.411(9) . ? C17 C18 1.414(9) . ? C18 C19 1.354(11) . ? C18 H18 0.9500 . ? C19 C20 1.390(12) . ? C19 H19 0.9500 . ? C20 C21 1.396(11) . ? C20 H20 0.9500 . ? C21 C22 1.402(9) . ? C21 H21 0.9500 . ? C23 C24 1.429(9) . ? C23 H23 0.9500 . ? C24 C25 1.402(9) . ? C24 C29 1.405(9) . ? C25 C26 1.364(12) . ? C25 H25 0.9500 . ? C26 C27 1.405(12) . ? C26 H26 0.9500 . ? C27 C28 1.382(10) . ? C27 H27 0.9500 . ? C28 C29 1.373(10) . ? C28 H28 0.9500 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? Ag2 N10 2.268(5) 2_655 ? Ag2 N10 2.268(5) . ? Ag2 N12 2.416(6) 2_655 ? Ag2 N12 2.416(6) . ? N9 N10 1.352(7) . ? N9 C37 1.371(7) . ? N9 C45 1.460(7) . ? N10 C31 1.326(9) . ? N11 C44 1.362(9) . ? N11 N12 1.369(7) 2_655 ? N11 C45 1.455(8) . ? N12 C38 1.318(9) . ? N12 N11 1.369(7) 2_655 ? C31 C32 1.406(9) . ? C31 H31 0.9500 . ? C32 C33 1.406(9) . ? C32 C37 1.412(9) . ? C33 C34 1.369(11) . ? C33 H33 0.9499 . ? C34 C35 1.422(10) . ? C34 H34 0.9500 . ? C35 C36 1.389(9) . ? C35 H35 0.9500 . ? C36 C37 1.390(8) . ? C36 H36 0.9500 . ? C38 C39 1.420(10) 2_655 ? C38 H38 0.9500 . ? C39 C40 1.384(11) . ? C39 C44 1.402(10) . ? C39 C38 1.420(10) 2_655 ? C40 C41 1.365(12) . ? C40 H40 0.9500 . ? C41 C42 1.378(15) . ? C41 H41 0.9500 . ? C42 C43 1.356(12) . ? C42 H42 0.9500 . ? C43 C44 1.407(9) . ? C43 H43 0.9500 . ? C45 H45A 0.9900 . ? C45 H45B 0.9900 . ? S1 O2 1.412(5) . ? S1 O3 1.427(8) . ? S1 O1 1.487(7) . ? S1 C46 1.685(11) . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? S2 O6 1.4300(2) . ? S2 O5 1.4300(2) . ? S2 O4 1.4300(2) . ? S2 C47 1.7501(2) . ? C47 H47A 0.9800 . ? C47 H47B 0.9921 . ? C47 H47C 0.9800 . ? 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 N6 157.03(18) . . ? N2 Ag1 N8 105.90(19) . . ? N6 Ag1 N8 86.24(18) . . ? N2 Ag1 N4 86.01(17) . . ? N6 Ag1 N4 101.28(17) . . ? N8 Ag1 N4 129.88(18) . . ? C7 N1 N2 110.3(5) . . ? C7 N1 C15 129.4(5) . . ? N2 N1 C15 119.8(5) . . ? C1 N2 N1 107.3(5) . . ? C1 N2 Ag1 128.6(4) . . ? N1 N2 Ag1 121.9(4) . . ? C14 N3 N4 111.2(5) . . ? C14 N3 C15 129.1(5) . . ? N4 N3 C15 119.7(5) . . ? C8 N4 N3 106.4(5) . . ? C8 N4 Ag1 130.1(4) . . ? N3 N4 Ag1 112.8(3) . . ? C22 N5 N6 111.5(5) . . ? C22 N5 C30 129.4(5) . . ? N6 N5 C30 119.0(5) . . ? C16 N6 N5 105.8(5) . . ? C16 N6 Ag1 131.0(4) . . ? N5 N6 Ag1 118.9(4) . . ? N8 N7 C29 112.3(5) . . ? N8 N7 C30 119.2(5) . . ? C29 N7 C30 128.0(5) . . ? C23 N8 N7 106.1(5) . . ? C23 N8 Ag1 132.3(5) . . ? N7 N8 Ag1 112.8(4) . . ? N2 C1 C2 111.0(6) . . ? N2 C1 H1 124.5 . . ? C2 C1 H1 124.5 . . ? C1 C2 C7 105.1(5) . . ? C1 C2 C3 135.4(6) . . ? C7 C2 C3 119.5(6) . . ? C4 C3 C2 117.8(7) . . ? C4 C3 H3 121.5 . . ? C2 C3 H3 120.8 . . ? C3 C4 C5 121.0(6) . . ? C3 C4 H4 119.0 . . ? C5 C4 H4 120.0 . . ? C6 C5 C4 122.9(7) . . ? C6 C5 H5 118.8 . . ? C4 C5 H5 118.2 . . ? C5 C6 C7 116.5(6) . . ? C5 C6 H6 121.8 . . ? C7 C6 H6 121.7 . . ? N1 C7 C6 131.4(6) . . ? N1 C7 C2 106.2(5) . . ? C6 C7 C2 122.4(6) . . ? N4 C8 C9 110.7(5) . . ? N4 C8 H8 124.7 . . ? C9 C8 H8 124.6 . . ? C14 C9 C10 119.2(5) . . ? C14 C9 C8 105.4(5) . . ? C10 C9 C8 135.4(5) . . ? C11 C10 C9 118.5(6) . . ? C11 C10 H10 121.1 . . ? C9 C10 H10 120.4 . . ? C10 C11 C12 121.6(6) . . ? C10 C11 H11 119.0 . . ? C12 C11 H11 119.4 . . ? C13 C12 C11 121.8(6) . . ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.0 . . ? C12 C13 C14 116.6(6) . . ? C12 C13 H13 121.8 . . ? C14 C13 H13 121.6 . . ? N3 C14 C13 131.3(5) . . ? N3 C14 C9 106.3(5) . . ? C13 C14 C9 122.3(5) . . ? N1 C15 N3 112.7(5) . . ? N1 C15 H15A 109.1 . . ? N3 C15 H15A 109.2 . . ? N1 C15 H15B 109.1 . . ? N3 C15 H15B 108.8 . . ? H15A C15 H15B 107.8 . . ? N6 C16 C17 111.2(6) . . ? N6 C16 H16 124.3 . . ? C17 C16 H16 124.5 . . ? C16 C17 C22 105.4(5) . . ? C16 C17 C18 134.6(7) . . ? C22 C17 C18 120.0(6) . . ? C19 C18 C17 117.4(7) . . ? C19 C18 H18 121.7 . . ? C17 C18 H18 120.8 . . ? C18 C19 C20 122.2(7) . . ? C18 C19 H19 119.1 . . ? C20 C19 H19 118.7 . . ? C19 C20 C21 123.0(7) . . ? C19 C20 H20 118.5 . . ? C21 C20 H20 118.5 . . ? C20 C21 C22 114.9(7) . . ? C20 C21 H21 122.5 . . ? C22 C21 H21 122.7 . . ? N5 C22 C21 131.3(6) . . ? N5 C22 C17 106.2(5) . . ? C21 C22 C17 122.5(6) . . ? N8 C23 C24 111.1(6) . . ? N8 C23 H23 124.4 . . ? C24 C23 H23 124.4 . . ? C25 C24 C29 119.8(6) . . ? C25 C24 C23 135.6(6) . . ? C29 C24 C23 104.6(5) . . ? C26 C25 C24 117.4(7) . . ? C26 C25 H25 121.2 . . ? C24 C25 H25 121.4 . . ? C25 C26 C27 121.9(7) . . ? C25 C26 H26 119.1 . . ? C27 C26 H26 119.1 . . ? C28 C27 C26 121.6(7) . . ? C28 C27 H27 119.3 . . ? C26 C27 H27 119.1 . . ? C29 C28 C27 116.3(7) . . ? C29 C28 H28 122.0 . . ? C27 C28 H28 121.7 . . ? N7 C29 C28 131.2(6) . . ? N7 C29 C24 105.9(5) . . ? C28 C29 C24 123.0(6) . . ? N7 C30 N5 113.1(5) . . ? N7 C30 H30A 109.0 . . ? N5 C30 H30A 108.8 . . ? N7 C30 H30B 109.1 . . ? N5 C30 H30B 108.9 . . ? H30A C30 H30B 107.8 . . ? N10 Ag2 N10 134.8(3) 2_655 . ? N10 Ag2 N12 122.02(19) 2_655 2_655 ? N10 Ag2 N12 87.06(18) . 2_655 ? N10 Ag2 N12 87.06(18) 2_655 . ? N10 Ag2 N12 122.02(19) . . ? N12 Ag2 N12 103.0(3) 2_655 . ? N10 N9 C37 111.3(5) . . ? N10 N9 C45 118.5(5) . . ? C37 N9 C45 130.2(5) . . ? C31 N10 N9 106.9(5) . . ? C31 N10 Ag2 131.3(4) . . ? N9 N10 Ag2 118.0(4) . . ? C44 N11 N12 110.9(5) . 2_655 ? C44 N11 C45 128.5(5) . . ? N12 N11 C45 119.2(5) 2_655 . ? C38 N12 N11 106.4(5) . 2_655 ? C38 N12 Ag2 131.1(5) . . ? N11 N12 Ag2 114.2(4) 2_655 . ? N10 C31 C32 110.9(6) . . ? N10 C31 H31 124.9 . . ? C32 C31 H31 124.1 . . ? C33 C32 C31 135.6(6) . . ? C33 C32 C37 119.4(6) . . ? C31 C32 C37 104.9(5) . . ? C34 C33 C32 118.3(6) . . ? C34 C33 H33 121.2 . . ? C32 C33 H33 120.5 . . ? C33 C34 C35 121.8(6) . . ? C33 C34 H34 119.3 . . ? C35 C34 H34 118.9 . . ? C36 C35 C34 120.6(6) . . ? C36 C35 H35 119.4 . . ? C34 C35 H35 120.0 . . ? C35 C36 C37 117.2(6) . . ? C35 C36 H36 121.3 . . ? C37 C36 H36 121.5 . . ? N9 C37 C36 131.5(5) . . ? N9 C37 C32 105.9(5) . . ? C36 C37 C32 122.6(5) . . ? N12 C38 C39 111.5(6) . 2_655 ? N12 C38 H38 124.2 . . ? C39 C38 H38 124.3 2_655 . ? C40 C39 C44 119.6(6) . . ? C40 C39 C38 136.3(7) . 2_655 ? C44 C39 C38 104.1(6) . 2_655 ? C41 C40 C39 118.5(8) . . ? C41 C40 H40 120.3 . . ? C39 C40 H40 121.2 . . ? C40 C41 C42 120.7(8) . . ? C40 C41 H41 120.1 . . ? C42 C41 H41 119.1 . . ? C43 C42 C41 123.7(8) . . ? C43 C42 H42 117.7 . . ? C41 C42 H42 118.6 . . ? C42 C43 C44 115.5(8) . . ? C42 C43 H43 122.6 . . ? C44 C43 H43 122.0 . . ? N11 C44 C39 107.2(5) . . ? N11 C44 C43 131.0(7) . . ? C39 C44 C43 121.9(7) . . ? N11 C45 N9 111.9(5) . . ? N11 C45 H45A 108.9 . . ? N9 C45 H45A 109.3 . . ? N11 C45 H45B 109.5 . . ? N9 C45 H45B 109.4 . . ? H45A C45 H45B 107.8 . . ? O2 S1 O3 118.7(5) . . ? O2 S1 O1 104.5(4) . . ? O3 S1 O1 104.2(5) . . ? O2 S1 C46 109.8(5) . . ? O3 S1 C46 115.1(5) . . ? O1 S1 C46 102.3(6) . . ? S1 C46 H46A 110.2 . . ? S1 C46 H46B 108.9 . . ? H46A C46 H46B 109.5 . . ? S1 C46 H46C 109.3 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? O6 S2 O5 104.0(8) . . ? O6 S2 O4 103.2(9) . . ? O5 S2 O4 100.3(10) . . ? O6 S2 C47 134.9(9) . . ? O5 S2 C47 116.8(9) . . ? O4 S2 C47 88.3(10) . . ? S2 C47 H47A 120.3 . . ? S2 C47 H47B 120.0 . . ? H47A C47 H47B 107.1 . . ? S2 C47 H47C 83.6 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 114.1 . . ? 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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 N1 N2 C1 -0.7(7) . . . . ? C15 N1 N2 C1 -173.0(5) . . . . ? C7 N1 N2 Ag1 -165.2(4) . . . . ? C15 N1 N2 Ag1 22.6(7) . . . . ? N6 Ag1 N2 C1 -38.4(8) . . . . ? N8 Ag1 N2 C1 81.4(6) . . . . ? N4 Ag1 N2 C1 -148.1(6) . . . . ? N6 Ag1 N2 N1 122.5(5) . . . . ? N8 Ag1 N2 N1 -117.7(4) . . . . ? N4 Ag1 N2 N1 12.7(4) . . . . ? C14 N3 N4 C8 -0.7(6) . . . . ? C15 N3 N4 C8 -179.3(5) . . . . ? C14 N3 N4 Ag1 147.7(4) . . . . ? C15 N3 N4 Ag1 -30.9(6) . . . . ? N2 Ag1 N4 C8 130.1(5) . . . . ? N6 Ag1 N4 C8 -27.9(5) . . . . ? N8 Ag1 N4 C8 -122.4(5) . . . . ? N2 Ag1 N4 N3 -8.8(4) . . . . ? N6 Ag1 N4 N3 -166.8(4) . . . . ? N8 Ag1 N4 N3 98.7(4) . . . . ? C22 N5 N6 C16 -0.7(6) . . . . ? C30 N5 N6 C16 -176.1(5) . . . . ? C22 N5 N6 Ag1 158.5(4) . . . . ? C30 N5 N6 Ag1 -16.9(6) . . . . ? N2 Ag1 N6 C16 -105.5(6) . . . . ? N8 Ag1 N6 C16 131.2(5) . . . . ? N4 Ag1 N6 C16 1.3(5) . . . . ? N2 Ag1 N6 N5 101.4(6) . . . . ? N8 Ag1 N6 N5 -21.9(4) . . . . ? N4 Ag1 N6 N5 -151.8(4) . . . . ? C29 N7 N8 C23 0.4(8) . . . . ? C30 N7 N8 C23 172.3(6) . . . . ? C29 N7 N8 Ag1 -151.5(4) . . . . ? C30 N7 N8 Ag1 20.4(7) . . . . ? N2 Ag1 N8 C23 78.0(7) . . . . ? N6 Ag1 N8 C23 -121.8(7) . . . . ? N4 Ag1 N8 C23 -20.2(8) . . . . ? N2 Ag1 N8 N7 -139.7(4) . . . . ? N6 Ag1 N8 N7 20.4(4) . . . . ? N4 Ag1 N8 N7 122.0(4) . . . . ? N1 N2 C1 C2 0.5(7) . . . . ? Ag1 N2 C1 C2 163.6(4) . . . . ? N2 C1 C2 C7 -0.1(7) . . . . ? N2 C1 C2 C3 180.0(7) . . . . ? C1 C2 C3 C4 -179.5(7) . . . . ? C7 C2 C3 C4 0.6(9) . . . . ? C2 C3 C4 C5 -0.2(10) . . . . ? C3 C4 C5 C6 -0.3(11) . . . . ? C4 C5 C6 C7 0.3(10) . . . . ? N2 N1 C7 C6 -179.1(6) . . . . ? C15 N1 C7 C6 -7.8(10) . . . . ? N2 N1 C7 C2 0.6(6) . . . . ? C15 N1 C7 C2 171.9(6) . . . . ? C5 C6 C7 N1 179.9(6) . . . . ? C5 C6 C7 C2 0.2(9) . . . . ? C1 C2 C7 N1 -0.3(6) . . . . ? C3 C2 C7 N1 179.6(5) . . . . ? C1 C2 C7 C6 179.5(6) . . . . ? C3 C2 C7 C6 -0.7(9) . . . . ? N3 N4 C8 C9 0.0(6) . . . . ? Ag1 N4 C8 C9 -140.8(4) . . . . ? N4 C8 C9 C14 0.6(7) . . . . ? N4 C8 C9 C10 -178.6(6) . . . . ? C14 C9 C10 C11 -0.3(8) . . . . ? C8 C9 C10 C11 178.8(6) . . . . ? C9 C10 C11 C12 0.4(10) . . . . ? C10 C11 C12 C13 -0.3(11) . . . . ? C11 C12 C13 C14 0.0(10) . . . . ? N4 N3 C14 C13 179.1(6) . . . . ? C15 N3 C14 C13 -2.4(10) . . . . ? N4 N3 C14 C9 1.1(6) . . . . ? C15 N3 C14 C9 179.5(5) . . . . ? C12 C13 C14 N3 -177.8(6) . . . . ? C12 C13 C14 C9 0.1(9) . . . . ? C10 C9 C14 N3 178.4(5) . . . . ? C8 C9 C14 N3 -1.0(6) . . . . ? C10 C9 C14 C13 0.1(8) . . . . ? C8 C9 C14 C13 -179.3(5) . . . . ? C7 N1 C15 N3 112.6(6) . . . . ? N2 N1 C15 N3 -76.8(7) . . . . ? C14 N3 C15 N1 -96.6(7) . . . . ? N4 N3 C15 N1 81.8(6) . . . . ? N5 N6 C16 C17 -0.4(6) . . . . ? Ag1 N6 C16 C17 -156.1(4) . . . . ? N6 C16 C17 C22 1.2(7) . . . . ? N6 C16 C17 C18 -179.9(6) . . . . ? C16 C17 C18 C19 -178.5(7) . . . . ? C22 C17 C18 C19 0.2(9) . . . . ? C17 C18 C19 C20 0.6(10) . . . . ? C18 C19 C20 C21 -1.1(11) . . . . ? C19 C20 C21 C22 0.7(10) . . . . ? N6 N5 C22 C21 -178.6(6) . . . . ? C30 N5 C22 C21 -3.8(10) . . . . ? N6 N5 C22 C17 1.4(6) . . . . ? C30 N5 C22 C17 176.2(5) . . . . ? C20 C21 C22 N5 -179.8(6) . . . . ? C20 C21 C22 C17 0.1(9) . . . . ? C16 C17 C22 N5 -1.6(6) . . . . ? C18 C17 C22 N5 179.4(5) . . . . ? C16 C17 C22 C21 178.5(5) . . . . ? C18 C17 C22 C21 -0.6(9) . . . . ? N7 N8 C23 C24 -0.7(8) . . . . ? Ag1 N8 C23 C24 143.3(5) . . . . ? N8 C23 C24 C25 177.4(8) . . . . ? N8 C23 C24 C29 0.7(8) . . . . ? C29 C24 C25 C26 -3.4(10) . . . . ? C23 C24 C25 C26 -179.7(8) . . . . ? C24 C25 C26 C27 2.0(12) . . . . ? C25 C26 C27 C28 0.2(13) . . . . ? C26 C27 C28 C29 -1.0(12) . . . . ? N8 N7 C29 C28 179.5(7) . . . . ? C30 N7 C29 C28 8.5(11) . . . . ? N8 N7 C29 C24 0.0(7) . . . . ? C30 N7 C29 C24 -171.0(6) . . . . ? C27 C28 C29 N7 -179.9(7) . . . . ? C27 C28 C29 C24 -0.5(11) . . . . ? C25 C24 C29 N7 -177.7(6) . . . . ? C23 C24 C29 N7 -0.4(7) . . . . ? C25 C24 C29 C28 2.7(10) . . . . ? C23 C24 C29 C28 -179.9(7) . . . . ? N8 N7 C30 N5 -79.4(7) . . . . ? C29 N7 C30 N5 91.0(7) . . . . ? C22 N5 C30 N7 -95.7(7) . . . . ? N6 N5 C30 N7 78.7(7) . . . . ? C37 N9 N10 C31 -0.4(7) . . . . ? C45 N9 N10 C31 179.4(6) . . . . ? C37 N9 N10 Ag2 160.4(4) . . . . ? C45 N9 N10 Ag2 -19.8(7) . . . . ? N10 Ag2 N10 C31 -92.2(7) 2_655 . . . ? N12 Ag2 N10 C31 133.6(7) 2_655 . . . ? N12 Ag2 N10 C31 30.1(7) . . . . ? N10 Ag2 N10 N9 112.6(5) 2_655 . . . ? N12 Ag2 N10 N9 -21.5(5) 2_655 . . . ? N12 Ag2 N10 N9 -125.0(4) . . . . ? N10 Ag2 N12 C38 -120.2(6) 2_655 . . . ? N10 Ag2 N12 C38 96.7(6) . . . . ? N12 Ag2 N12 C38 2.0(5) 2_655 . . . ? N10 Ag2 N12 N11 23.1(4) 2_655 . . 2_655 ? N10 Ag2 N12 N11 -120.0(4) . . . 2_655 ? N12 Ag2 N12 N11 145.3(5) 2_655 . . 2_655 ? N9 N10 C31 C32 0.0(8) . . . . ? Ag2 N10 C31 C32 -157.2(5) . . . . ? N10 C31 C32 C33 -179.1(8) . . . . ? N10 C31 C32 C37 0.4(8) . . . . ? C31 C32 C33 C34 -178.3(8) . . . . ? C37 C32 C33 C34 2.3(11) . . . . ? C32 C33 C34 C35 -1.3(12) . . . . ? C33 C34 C35 C36 -1.0(12) . . . . ? C34 C35 C36 C37 2.2(10) . . . . ? N10 N9 C37 C36 -179.3(6) . . . . ? C45 N9 C37 C36 0.9(11) . . . . ? N10 N9 C37 C32 0.6(7) . . . . ? C45 N9 C37 C32 -179.2(6) . . . . ? C35 C36 C37 N9 178.7(6) . . . . ? C35 C36 C37 C32 -1.2(10) . . . . ? C33 C32 C37 N9 179.0(6) . . . . ? C31 C32 C37 N9 -0.5(7) . . . . ? C33 C32 C37 C36 -1.1(10) . . . . ? C31 C32 C37 C36 179.4(6) . . . . ? N11 N12 C38 C39 -1.1(7) 2_655 . . 2_655 ? Ag2 N12 C38 C39 144.3(5) . . . 2_655 ? C44 C39 C40 C41 -1.1(10) . . . . ? C38 C39 C40 C41 178.7(8) 2_655 . . . ? C39 C40 C41 C42 0.2(13) . . . . ? C40 C41 C42 C43 0.5(15) . . . . ? C41 C42 C43 C44 -0.3(13) . . . . ? N12 N11 C44 C39 -1.6(7) 2_655 . . . ? C45 N11 C44 C39 -167.2(6) . . . . ? N12 N11 C44 C43 177.7(7) 2_655 . . . ? C45 N11 C44 C43 12.1(11) . . . . ? C40 C39 C44 N11 -179.3(6) . . . . ? C38 C39 C44 N11 0.9(7) 2_655 . . . ? C40 C39 C44 C43 1.3(10) . . . . ? C38 C39 C44 C43 -178.5(6) 2_655 . . . ? C42 C43 C44 N11 -179.8(7) . . . . ? C42 C43 C44 C39 -0.5(11) . . . . ? C44 N11 C45 N9 88.0(7) . . . . ? N12 N11 C45 N9 -76.5(7) 2_655 . . . ? N10 N9 C45 N11 79.8(7) . . . . ? C37 N9 C45 N11 -100.5(7) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 1.488 _refine_diff_density_min -1.672 _refine_diff_density_rms 0.139 data_16 _database_code_depnum_ccdc_archive 'CCDC 917675' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C16 H15 Ag N4 O3 S' _chemical_formula_sum 'C16 H15 Ag N4 O3 S' _chemical_formula_weight 451.25 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' 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' S S 0.1246 0.1234 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 6.8541(4) _cell_length_b 10.2636(6) _cell_length_c 12.8115(7) _cell_angle_alpha 90.296(2) _cell_angle_beta 100.4080(10) _cell_angle_gamma 95.7830(10) _cell_volume 881.67(9) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9993 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 30.49 _exptl_crystal_description needle _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.700 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 452 _exptl_absorpt_coefficient_mu 1.284 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8308 _exptl_absorpt_correction_T_max 0.9042 _exptl_absorpt_process_details ; APEX2 Software Suite; Bruker 2005. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker-Nonius X8kappa APEX II CCD area detector ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 20960 _diffrn_reflns_av_R_equivalents 0.0296 _diffrn_reflns_av_sigmaI/netI 0.0178 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.54 _diffrn_reflns_theta_max 25.25 _reflns_number_total 3145 _reflns_number_gt 2895 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker, 2007)' _computing_cell_refinement 'APEX2 Software Suite (Bruker, 2007)' _computing_data_reduction 'APEX2 Software Suite (Bruker, 2007)' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL and publCIF (Westrip, 2010)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0519P)^2^+0.4063P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3145 _refine_ls_number_parameters 227 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0300 _refine_ls_R_factor_gt 0.0265 _refine_ls_wR_factor_ref 0.0765 _refine_ls_wR_factor_gt 0.0740 _refine_ls_goodness_of_fit_ref 1.069 _refine_ls_restrained_S_all 1.069 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.57325(3) 0.076123(19) 0.691027(16) 0.03241(10) Uani 1 1 d . . . S1 S 0.48678(9) 0.19740(6) 0.45212(5) 0.02477(15) Uani 1 1 d . . . O1 O 0.6398(3) 0.2307(2) 0.54579(16) 0.0423(5) Uani 1 1 d . . . O2 O 0.5689(3) 0.15549(19) 0.36168(15) 0.0364(4) Uani 1 1 d . . . O3 O 0.3250(3) 0.10545(19) 0.47461(15) 0.0357(4) Uani 1 1 d . . . N1 N 0.8505(3) 0.0058(2) 0.77554(16) 0.0241(4) Uani 1 1 d . . . N2 N 1.0079(3) -0.01886(19) 0.73135(15) 0.0218(4) Uani 1 1 d . . . N3 N 0.3452(3) 0.1973(2) 0.72670(16) 0.0230(4) Uani 1 1 d . . . N4 N 0.1505(3) 0.1868(2) 0.67866(15) 0.0219(4) Uani 1 1 d . . . C1 C 1.1164(4) -0.1093(2) 0.7829(2) 0.0258(5) Uani 1 1 d . . . H1 H 1.2330 -0.1398 0.7653 0.031 Uiso 1 1 calc R . . C2 C 1.0231(4) -0.1488(2) 0.8668(2) 0.0268(5) Uani 1 1 d . . . C3 C 1.0595(5) -0.2395(3) 0.9507(2) 0.0378(6) Uani 1 1 d . . . H3 H 1.1689 -0.2907 0.9576 0.045 Uiso 1 1 calc R . . C4 C 0.9304(5) -0.2496(3) 1.0207(2) 0.0427(7) Uani 1 1 d . . . H4 H 0.9520 -0.3085 1.0775 0.051 Uiso 1 1 calc R . . C5 C 0.7664(5) -0.1754(3) 1.0112(2) 0.0431(8) Uani 1 1 d . . . H5 H 0.6809 -0.1865 1.0618 0.052 Uiso 1 1 calc R . . C6 C 0.7253(4) -0.0877(3) 0.9318(2) 0.0359(6) Uani 1 1 d . . . H6 H 0.6138 -0.0385 0.9262 0.043 Uiso 1 1 calc R . . C7 C 0.8588(4) -0.0744(2) 0.85834(18) 0.0243(5) Uani 1 1 d . . . C8 C 0.0668(4) 0.2991(2) 0.6789(2) 0.0275(5) Uani 1 1 d . . . H8 H -0.0671 0.3123 0.6499 0.033 Uiso 1 1 calc R . . C9 C 0.2151(4) 0.3931(2) 0.7303(2) 0.0274(5) Uani 1 1 d . . . C10 C 0.2272(5) 0.5282(3) 0.7581(3) 0.0431(7) Uani 1 1 d . . . H10 H 0.1155 0.5766 0.7390 0.052 Uiso 1 1 calc R . . C11 C 0.4020(5) 0.5858(3) 0.8125(3) 0.0463(8) Uani 1 1 d . . . H11 H 0.4115 0.6756 0.8329 0.056 Uiso 1 1 calc R . . C12 C 0.5718(5) 0.5164(3) 0.8400(3) 0.0430(7) Uani 1 1 d . . . H12 H 0.6918 0.5613 0.8780 0.052 Uiso 1 1 calc R . . C13 C 0.5680(4) 0.3866(3) 0.8135(2) 0.0334(6) Uani 1 1 d . . . H13 H 0.6828 0.3407 0.8315 0.040 Uiso 1 1 calc R . . C14 C 0.3853(4) 0.3242(2) 0.75819(18) 0.0242(5) Uani 1 1 d . . . C15 C 1.0534(4) 0.0580(2) 0.64212(19) 0.0238(5) Uani 1 1 d . . . H15A H 1.1419 0.0121 0.6048 0.029 Uiso 1 1 calc R . . H15B H 0.9286 0.0676 0.5914 0.029 Uiso 1 1 calc R . . C16 C 0.3788(6) 0.3432(3) 0.4154(3) 0.0502(8) Uani 1 1 d . . . H16A H 0.2759 0.3262 0.3516 0.075 Uiso 1 1 calc R . . H16B H 0.4820 0.4102 0.4007 0.075 Uiso 1 1 calc R . . H16C H 0.3184 0.3741 0.4734 0.075 Uiso 1 1 calc R . . 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 0.02113(14) 0.03498(14) 0.04172(15) 0.00021(9) 0.00459(9) 0.00784(9) S1 0.0209(3) 0.0279(3) 0.0241(3) -0.0014(2) 0.0019(2) 0.0000(2) O1 0.0305(11) 0.0548(13) 0.0347(11) -0.0001(9) -0.0052(9) -0.0089(9) O2 0.0389(11) 0.0357(10) 0.0380(10) -0.0019(8) 0.0180(9) 0.0012(8) O3 0.0295(10) 0.0427(11) 0.0336(10) -0.0057(8) 0.0088(8) -0.0076(8) N1 0.0169(10) 0.0322(11) 0.0227(10) -0.0042(8) 0.0034(8) 0.0013(8) N2 0.0172(10) 0.0259(10) 0.0214(10) -0.0030(8) 0.0030(8) -0.0013(8) N3 0.0155(10) 0.0286(11) 0.0233(10) -0.0028(8) 0.0001(8) 0.0013(8) N4 0.0163(10) 0.0280(11) 0.0199(9) -0.0022(8) 0.0008(8) -0.0001(8) C1 0.0190(12) 0.0285(13) 0.0288(13) -0.0028(10) 0.0012(10) 0.0031(9) C2 0.0262(13) 0.0257(12) 0.0255(12) -0.0030(10) -0.0011(10) -0.0017(10) C3 0.0420(17) 0.0343(14) 0.0319(14) 0.0035(11) -0.0045(12) -0.0015(12) C4 0.054(2) 0.0433(17) 0.0246(14) 0.0049(12) -0.0013(13) -0.0103(14) C5 0.0503(19) 0.0530(18) 0.0237(14) -0.0037(12) 0.0123(13) -0.0160(14) C6 0.0334(15) 0.0490(17) 0.0248(13) -0.0075(12) 0.0096(11) -0.0065(12) C7 0.0210(12) 0.0311(13) 0.0183(11) -0.0063(9) 0.0012(9) -0.0050(9) C8 0.0172(12) 0.0324(13) 0.0319(13) 0.0030(10) 0.0007(10) 0.0049(10) C9 0.0260(13) 0.0285(13) 0.0274(13) 0.0020(10) 0.0038(10) 0.0025(10) C10 0.0448(18) 0.0294(14) 0.0558(19) 0.0009(13) 0.0086(15) 0.0079(12) C11 0.052(2) 0.0259(14) 0.058(2) -0.0082(13) 0.0062(16) -0.0034(13) C12 0.0410(18) 0.0378(16) 0.0429(17) -0.0076(13) -0.0022(13) -0.0132(13) C13 0.0247(14) 0.0403(15) 0.0308(14) -0.0034(11) -0.0031(11) -0.0024(11) C14 0.0228(13) 0.0292(13) 0.0200(11) 0.0001(10) 0.0036(9) 0.0001(9) C15 0.0195(12) 0.0308(13) 0.0197(11) -0.0023(9) 0.0021(9) -0.0017(9) C16 0.061(2) 0.0418(17) 0.0514(19) 0.0049(14) 0.0104(16) 0.0233(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N3 2.201(2) . ? Ag1 N1 2.201(2) . ? Ag1 O2 2.5170(19) 2_656 ? Ag1 O1 2.526(2) . ? S1 O3 1.4530(19) . ? S1 O2 1.4574(19) . ? S1 O1 1.458(2) . ? S1 C16 1.764(3) . ? O2 Ag1 2.5170(19) 2_656 ? N1 C7 1.343(3) . ? N1 N2 1.350(3) . ? N2 C1 1.348(3) . ? N2 C15 1.454(3) . ? N3 C14 1.348(3) . ? N3 N4 1.358(3) . ? N4 C8 1.338(3) . ? N4 C15 1.454(3) 1_455 ? C1 C2 1.390(4) . ? C1 H1 0.9500 . ? C2 C7 1.412(4) . ? C2 C3 1.430(4) . ? C3 C4 1.365(4) . ? C3 H3 0.9500 . ? C4 C5 1.408(5) . ? C4 H4 0.9500 . ? C5 C6 1.371(4) . ? C5 H5 0.9500 . ? C6 C7 1.425(3) . ? C6 H6 0.9500 . ? C8 C9 1.397(4) . ? C8 H8 0.9500 . ? C9 C14 1.417(4) . ? C9 C10 1.421(4) . ? C10 C11 1.350(5) . ? C10 H10 0.9500 . ? C11 C12 1.416(5) . ? C11 H11 0.9500 . ? C12 C13 1.371(4) . ? C12 H12 0.9500 . ? C13 C14 1.412(4) . ? C13 H13 0.9500 . ? C15 N4 1.454(3) 1_655 ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? 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 N3 Ag1 N1 137.67(7) . . ? N3 Ag1 O2 112.22(7) . 2_656 ? N1 Ag1 O2 90.52(7) . 2_656 ? N3 Ag1 O1 89.51(7) . . ? N1 Ag1 O1 111.41(7) . . ? O2 Ag1 O1 117.99(6) 2_656 . ? O3 S1 O2 112.59(11) . . ? O3 S1 O1 112.51(12) . . ? O2 S1 O1 112.66(12) . . ? O3 S1 C16 105.61(16) . . ? O2 S1 C16 106.52(15) . . ? O1 S1 C16 106.28(16) . . ? S1 O1 Ag1 108.18(10) . . ? S1 O2 Ag1 109.06(10) . 2_656 ? C7 N1 N2 104.1(2) . . ? C7 N1 Ag1 123.84(16) . . ? N2 N1 Ag1 125.59(15) . . ? C1 N2 N1 113.6(2) . . ? C1 N2 C15 126.9(2) . . ? N1 N2 C15 119.3(2) . . ? C14 N3 N4 104.07(19) . . ? C14 N3 Ag1 123.36(16) . . ? N4 N3 Ag1 126.10(15) . . ? C8 N4 N3 113.6(2) . . ? C8 N4 C15 127.6(2) . 1_455 ? N3 N4 C15 118.54(19) . 1_455 ? N2 C1 C2 106.1(2) . . ? N2 C1 H1 126.9 . . ? C2 C1 H1 126.9 . . ? C1 C2 C7 104.7(2) . . ? C1 C2 C3 135.1(3) . . ? C7 C2 C3 120.2(2) . . ? C4 C3 C2 117.3(3) . . ? C4 C3 H3 121.4 . . ? C2 C3 H3 121.4 . . ? C3 C4 C5 122.1(3) . . ? C3 C4 H4 118.9 . . ? C5 C4 H4 118.9 . . ? C6 C5 C4 122.6(3) . . ? C6 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? C5 C6 C7 116.4(3) . . ? C5 C6 H6 121.8 . . ? C7 C6 H6 121.8 . . ? N1 C7 C2 111.5(2) . . ? N1 C7 C6 127.1(2) . . ? C2 C7 C6 121.4(2) . . ? N4 C8 C9 106.6(2) . . ? N4 C8 H8 126.7 . . ? C9 C8 H8 126.7 . . ? C8 C9 C14 104.4(2) . . ? C8 C9 C10 135.9(3) . . ? C14 C9 C10 119.7(2) . . ? C11 C10 C9 118.0(3) . . ? C11 C10 H10 121.0 . . ? C9 C10 H10 121.0 . . ? C10 C11 C12 122.1(3) . . ? C10 C11 H11 119.0 . . ? C12 C11 H11 119.0 . . ? C13 C12 C11 122.0(3) . . ? C13 C12 H12 119.0 . . ? C11 C12 H12 119.0 . . ? C12 C13 C14 116.7(3) . . ? C12 C13 H13 121.6 . . ? C14 C13 H13 121.6 . . ? N3 C14 C13 127.1(2) . . ? N3 C14 C9 111.3(2) . . ? C13 C14 C9 121.6(2) . . ? N4 C15 N2 110.42(18) 1_655 . ? N4 C15 H15A 109.6 1_655 . ? N2 C15 H15A 109.6 . . ? N4 C15 H15B 109.6 1_655 . ? N2 C15 H15B 109.6 . . ? H15A C15 H15B 108.1 . . ? S1 C16 H16A 109.5 . . ? S1 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? S1 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? 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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag O3 S1 O1 Ag1 10.73(16) . . . . ? O2 S1 O1 Ag1 -117.85(11) . . . . ? C16 S1 O1 Ag1 125.85(15) . . . . ? N3 Ag1 O1 S1 -80.73(13) . . . . ? N1 Ag1 O1 S1 137.02(12) . . . . ? O2 Ag1 O1 S1 34.34(15) 2_656 . . . ? O3 S1 O2 Ag1 -9.71(15) . . . 2_656 ? O1 S1 O2 Ag1 118.83(12) . . . 2_656 ? C16 S1 O2 Ag1 -125.02(15) . . . 2_656 ? N3 Ag1 N1 C7 63.3(2) . . . . ? O2 Ag1 N1 C7 -61.51(19) 2_656 . . . ? O1 Ag1 N1 C7 177.98(17) . . . . ? N3 Ag1 N1 N2 -149.49(16) . . . . ? O2 Ag1 N1 N2 85.65(18) 2_656 . . . ? O1 Ag1 N1 N2 -34.9(2) . . . . ? C7 N1 N2 C1 -0.8(3) . . . . ? Ag1 N1 N2 C1 -153.15(17) . . . . ? C7 N1 N2 C15 -176.00(19) . . . . ? Ag1 N1 N2 C15 31.7(3) . . . . ? N1 Ag1 N3 C14 61.4(2) . . . . ? O2 Ag1 N3 C14 179.02(17) 2_656 . . . ? O1 Ag1 N3 C14 -60.75(18) . . . . ? N1 Ag1 N3 N4 -151.38(16) . . . . ? O2 Ag1 N3 N4 -33.8(2) 2_656 . . . ? O1 Ag1 N3 N4 86.44(18) . . . . ? C14 N3 N4 C8 -0.4(3) . . . . ? Ag1 N3 N4 C8 -152.58(17) . . . . ? C14 N3 N4 C15 -175.23(19) . . . 1_455 ? Ag1 N3 N4 C15 32.6(3) . . . 1_455 ? N1 N2 C1 C2 0.7(3) . . . . ? C15 N2 C1 C2 175.5(2) . . . . ? N2 C1 C2 C7 -0.3(3) . . . . ? N2 C1 C2 C3 -179.8(3) . . . . ? C1 C2 C3 C4 179.2(3) . . . . ? C7 C2 C3 C4 -0.3(4) . . . . ? C2 C3 C4 C5 0.6(4) . . . . ? C3 C4 C5 C6 -0.3(5) . . . . ? C4 C5 C6 C7 -0.3(4) . . . . ? N2 N1 C7 C2 0.6(2) . . . . ? Ag1 N1 C7 C2 153.55(17) . . . . ? N2 N1 C7 C6 -179.7(2) . . . . ? Ag1 N1 C7 C6 -26.7(3) . . . . ? C1 C2 C7 N1 -0.2(3) . . . . ? C3 C2 C7 N1 179.4(2) . . . . ? C1 C2 C7 C6 -179.9(2) . . . . ? C3 C2 C7 C6 -0.3(4) . . . . ? C5 C6 C7 N1 -179.1(2) . . . . ? C5 C6 C7 C2 0.6(4) . . . . ? N3 N4 C8 C9 0.3(3) . . . . ? C15 N4 C8 C9 174.6(2) 1_455 . . . ? N4 C8 C9 C14 -0.1(3) . . . . ? N4 C8 C9 C10 -179.3(3) . . . . ? C8 C9 C10 C11 177.9(3) . . . . ? C14 C9 C10 C11 -1.2(4) . . . . ? C9 C10 C11 C12 1.3(5) . . . . ? C10 C11 C12 C13 -0.3(5) . . . . ? C11 C12 C13 C14 -0.7(5) . . . . ? N4 N3 C14 C13 179.3(2) . . . . ? Ag1 N3 C14 C13 -27.5(3) . . . . ? N4 N3 C14 C9 0.3(3) . . . . ? Ag1 N3 C14 C9 153.50(17) . . . . ? C12 C13 C14 N3 -178.1(2) . . . . ? C12 C13 C14 C9 0.8(4) . . . . ? C8 C9 C14 N3 -0.2(3) . . . . ? C10 C9 C14 N3 179.2(2) . . . . ? C8 C9 C14 C13 -179.2(2) . . . . ? C10 C9 C14 C13 0.2(4) . . . . ? C1 N2 C15 N4 -97.5(3) . . . 1_655 ? N1 N2 C15 N4 76.9(3) . . . 1_655 ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.839 _refine_diff_density_min -0.611 _refine_diff_density_rms 0.089 data_17 _database_code_depnum_ccdc_archive 'CCDC 917676' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H24 Ag F3 N8 O3 S, C30 H24 Ag N8, C F3 O3 S' _chemical_formula_sum 'C62 H48 Ag2 F6 N16 O6 S2' _chemical_formula_weight 1507.02 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' 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' F F 0.0171 0.0103 '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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.0012(8) _cell_length_b 12.6108(8) _cell_length_c 21.0839(14) _cell_angle_alpha 81.438(2) _cell_angle_beta 85.256(2) _cell_angle_gamma 74.156(1) _cell_volume 3032.5(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9925 _cell_measurement_theta_min 2.44 _cell_measurement_theta_max 24.32 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.36 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.650 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 0.801 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6702 _exptl_absorpt_correction_T_max 0.7514 _exptl_absorpt_process_details ; APEX2 Software Suite; Bruker 2005. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker-Nonius X8kappa APEX II CCD area detector ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 58204 _diffrn_reflns_av_R_equivalents 0.0545 _diffrn_reflns_av_sigmaI/netI 0.0716 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.69 _diffrn_reflns_theta_max 30.53 _reflns_number_total 18544 _reflns_number_gt 10660 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker, 2007)' _computing_cell_refinement 'APEX2 Software Suite (Bruker, 2007)' _computing_data_reduction 'APEX2 Software Suite (Bruker, 2007)' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL and publCIF (Westrip, 2010)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type fullcycle _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0942P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18544 _refine_ls_number_parameters 847 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1136 _refine_ls_R_factor_gt 0.0634 _refine_ls_wR_factor_ref 0.1759 _refine_ls_wR_factor_gt 0.1480 _refine_ls_goodness_of_fit_ref 1.018 _refine_ls_restrained_S_all 1.018 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.55236(2) 0.76517(2) 0.061898(13) 0.03781(8) Uani 1 1 d . . . N1 N 0.7233(2) 0.7411(2) -0.06368(13) 0.0288(6) Uani 1 1 d . . . N2 N 0.6103(2) 0.7700(2) -0.04150(13) 0.0298(6) Uani 1 1 d . . . N3 N 0.8481(2) 0.5566(2) -0.03966(13) 0.0292(6) Uani 1 1 d . . . N4 N 0.9516(2) 0.5209(2) -0.07224(14) 0.0324(6) Uani 1 1 d . . . N5 N 0.3207(2) 0.9039(2) 0.12883(13) 0.0296(6) Uani 1 1 d . . . N6 N 0.3898(3) 0.9195(2) 0.07515(14) 0.0328(6) Uani 1 1 d . . . N7 N 0.3810(2) 0.7118(2) 0.17443(13) 0.0284(6) Uani 1 1 d . . . N8 N 0.4742(2) 0.6580(2) 0.13875(13) 0.0317(6) Uani 1 1 d . . . C1 C 0.5494(3) 0.8329(3) -0.08993(16) 0.0326(7) Uani 1 1 d . . . H1 H 0.4679 0.8646 -0.0878 0.039 Uiso 1 1 calc R . . C2 C 0.6224(3) 0.8460(3) -0.14499(16) 0.0308(7) Uani 1 1 d . . . C3 C 0.6075(4) 0.9046(3) -0.20747(18) 0.0395(9) Uani 1 1 d . . . H3 H 0.5331 0.9473 -0.2209 0.047 Uiso 1 1 calc R . . C4 C 0.7034(4) 0.8982(3) -0.24823(18) 0.0442(10) Uani 1 1 d . . . H4 H 0.6951 0.9375 -0.2904 0.053 Uiso 1 1 calc R . . C5 C 0.8141(4) 0.8343(3) -0.22885(18) 0.0440(9) Uani 1 1 d . . . H5 H 0.8784 0.8311 -0.2586 0.053 Uiso 1 1 calc R . . C6 C 0.8321(3) 0.7762(3) -0.16793(17) 0.0345(8) Uani 1 1 d . . . H6 H 0.9067 0.7329 -0.1550 0.041 Uiso 1 1 calc R . . C7 C 0.7335(3) 0.7852(3) -0.12660(15) 0.0292(7) Uani 1 1 d . . . C8 C 0.9599(3) 0.4172(3) -0.07976(17) 0.0340(8) Uani 1 1 d . . . H8 H 1.0235 0.3718 -0.1015 0.041 Uiso 1 1 calc R . . C9 C 0.8628(3) 0.3812(3) -0.05156(16) 0.0304(7) Uani 1 1 d . . . C10 C 0.8261(3) 0.2834(3) -0.04545(17) 0.0356(8) Uani 1 1 d . . . H10 H 0.8725 0.2193 -0.0626 0.043 Uiso 1 1 calc R . . C11 C 0.7218(3) 0.2830(3) -0.01406(18) 0.0379(8) Uani 1 1 d . . . H11 H 0.6962 0.2172 -0.0093 0.045 Uiso 1 1 calc R . . C12 C 0.6517(3) 0.3766(3) 0.01124(17) 0.0372(8) Uani 1 1 d . . . H12 H 0.5800 0.3726 0.0328 0.045 Uiso 1 1 calc R . . C13 C 0.6841(3) 0.4747(3) 0.00555(17) 0.0338(8) Uani 1 1 d . . . H13 H 0.6361 0.5387 0.0221 0.041 Uiso 1 1 calc R . . C14 C 0.7912(3) 0.4750(3) -0.02574(15) 0.0280(7) Uani 1 1 d . . . C15 C 0.8124(3) 0.6688(3) -0.02367(16) 0.0296(7) Uani 1 1 d . . . H15A H 0.7835 0.6670 0.0217 0.036 Uiso 1 1 calc R . . H15B H 0.8806 0.6996 -0.0280 0.036 Uiso 1 1 calc R . . C16 C 0.3208(3) 0.9859(3) 0.03117(17) 0.0353(8) Uani 1 1 d . . . H16 H 0.3464 1.0102 -0.0109 0.042 Uiso 1 1 calc R . . C17 C 0.2051(3) 1.0156(3) 0.05491(17) 0.0342(8) Uani 1 1 d . . . C18 C 0.0989(4) 1.0796(3) 0.0308(2) 0.0442(10) Uani 1 1 d . . . H18 H 0.0948 1.1174 -0.0118 0.053 Uiso 1 1 calc R . . C19 C 0.0015(4) 1.0863(3) 0.0695(2) 0.0469(10) Uani 1 1 d . . . H19 H -0.0714 1.1279 0.0533 0.056 Uiso 1 1 calc R . . C20 C 0.0067(3) 1.0329(3) 0.1334(2) 0.0430(9) Uani 1 1 d . . . H20 H -0.0629 1.0414 0.1595 0.052 Uiso 1 1 calc R . . C21 C 0.1079(3) 0.9695(3) 0.15896(18) 0.0340(8) Uani 1 1 d . . . H21 H 0.1108 0.9335 0.2019 0.041 Uiso 1 1 calc R . . C22 C 0.2066(3) 0.9604(3) 0.11850(17) 0.0302(7) Uani 1 1 d . . . C23 C 0.4617(3) 0.5577(3) 0.13605(16) 0.0339(8) Uani 1 1 d . . . H23 H 0.5154 0.5021 0.1150 0.041 Uiso 1 1 calc R . . C24 C 0.3575(3) 0.5445(3) 0.16884(16) 0.0314(7) Uani 1 1 d . . . C25 C 0.3015(4) 0.4585(3) 0.18008(17) 0.0405(9) Uani 1 1 d . . . H25 H 0.3350 0.3890 0.1648 0.049 Uiso 1 1 calc R . . C26 C 0.1969(4) 0.4785(3) 0.21382(18) 0.0433(9) Uani 1 1 d . . . H26 H 0.1570 0.4220 0.2217 0.052 Uiso 1 1 calc R . . C27 C 0.1473(3) 0.5806(3) 0.23701(18) 0.0390(8) Uani 1 1 d . . . H27 H 0.0743 0.5913 0.2599 0.047 Uiso 1 1 calc R . . C28 C 0.2007(3) 0.6656(3) 0.22778(16) 0.0318(7) Uani 1 1 d . . . H28 H 0.1673 0.7340 0.2442 0.038 Uiso 1 1 calc R . . C29 C 0.3073(3) 0.6455(3) 0.19275(15) 0.0296(7) Uani 1 1 d . . . C30 C 0.3676(3) 0.8270(3) 0.18352(15) 0.0281(7) Uani 1 1 d . . . H30A H 0.3156 0.8442 0.2217 0.034 Uiso 1 1 calc R . . H30B H 0.4440 0.8366 0.1917 0.034 Uiso 1 1 calc R . . S1 S 0.70878(8) 0.86350(8) 0.15797(4) 0.0373(2) Uani 1 1 d . . . F1 F 0.8647(2) 0.69435(19) 0.21121(13) 0.0585(7) Uani 1 1 d . . . F2 F 0.93537(17) 0.81222(18) 0.14870(11) 0.0472(5) Uani 1 1 d . . . F3 F 0.8632(2) 0.8500(2) 0.24150(11) 0.0587(7) Uani 1 1 d . . . O1 O 0.7200(2) 0.8088(3) 0.10139(12) 0.0504(7) Uani 1 1 d . . . O2 O 0.6303(2) 0.8306(3) 0.20780(13) 0.0530(8) Uani 1 1 d . . . O3 O 0.7005(3) 0.9802(2) 0.14524(16) 0.0660(9) Uani 1 1 d . . . C31 C 0.8510(3) 0.8022(3) 0.19129(18) 0.0364(8) Uani 1 1 d . . . Ag2 Ag 0.56175(3) 0.65409(3) 0.592753(16) 0.05566(9) Uani 1 1 d . . . N9 N 0.6159(2) 0.8776(2) 0.51736(14) 0.0343(7) Uani 1 1 d . . . N10 N 0.5457(2) 0.8087(3) 0.51500(15) 0.0392(7) Uani 1 1 d . . . N11 N 0.7594(3) 0.7819(3) 0.59395(14) 0.0358(7) Uani 1 1 d . . . N12 N 0.7408(3) 0.6784(3) 0.60923(15) 0.0427(8) Uani 1 1 d . . . N13 N 0.4189(3) 0.4712(2) 0.62553(14) 0.0350(7) Uani 1 1 d . . . N14 N 0.4410(3) 0.5507(3) 0.57810(14) 0.0397(7) Uani 1 1 d . . . N15 N 0.4394(3) 0.5460(2) 0.71973(14) 0.0352(7) Uani 1 1 d . . . N16 N 0.4941(3) 0.6296(3) 0.70605(15) 0.0460(8) Uani 1 1 d . . . C32 C 0.5211(3) 0.8174(3) 0.45415(18) 0.0416(9) Uani 1 1 d . . . H32 H 0.4736 0.7786 0.4387 0.050 Uiso 1 1 calc R . . C33 C 0.5747(3) 0.8919(3) 0.41535(17) 0.0341(8) Uani 1 1 d . . . C34 C 0.5812(3) 0.9294(3) 0.34909(18) 0.0415(9) Uani 1 1 d . . . H34 H 0.5409 0.9048 0.3197 0.050 Uiso 1 1 calc R . . C35 C 0.6465(4) 1.0013(4) 0.32837(19) 0.0483(10) Uani 1 1 d . . . H35 H 0.6530 1.0261 0.2838 0.058 Uiso 1 1 calc R . . C36 C 0.7043(4) 1.0396(4) 0.3715(2) 0.0515(11) Uani 1 1 d . . . H36 H 0.7476 1.0914 0.3553 0.062 Uiso 1 1 calc R . . C37 C 0.7007(3) 1.0048(3) 0.43654(19) 0.0439(9) Uani 1 1 d . . . H37 H 0.7398 1.0311 0.4657 0.053 Uiso 1 1 calc R . . C38 C 0.6366(3) 0.9290(3) 0.45671(17) 0.0331(8) Uani 1 1 d . . . C39 C 0.8395(4) 0.6099(3) 0.62687(18) 0.0455(9) Uani 1 1 d . . . H39 H 0.8511 0.5322 0.6393 0.055 Uiso 1 1 calc R . . C40 C 0.9267(3) 0.6662(3) 0.62511(18) 0.0414(9) Uani 1 1 d . . . C41 C 1.0451(4) 0.6365(4) 0.6407(2) 0.0579(12) Uani 1 1 d . . . H41 H 1.0841 0.5619 0.6559 0.069 Uiso 1 1 calc R . . C42 C 1.1003(4) 0.7176(4) 0.6332(3) 0.0701(15) Uani 1 1 d . . . H42 H 1.1797 0.6989 0.6429 0.084 Uiso 1 1 calc R . . C43 C 1.0447(4) 0.8285(4) 0.6115(3) 0.0670(14) Uani 1 1 d . . . H43 H 1.0872 0.8828 0.6076 0.080 Uiso 1 1 calc R . . C44 C 0.9297(3) 0.8613(4) 0.5955(2) 0.0472(10) Uani 1 1 d . . . H44 H 0.8920 0.9363 0.5803 0.057 Uiso 1 1 calc R . . C45 C 0.8726(3) 0.7773(3) 0.60318(16) 0.0358(8) Uani 1 1 d . . . C46 C 0.6635(3) 0.8779(3) 0.57748(16) 0.0367(8) Uani 1 1 d . . . H46A H 0.6017 0.8802 0.6118 0.044 Uiso 1 1 calc R . . H46B H 0.6901 0.9460 0.5755 0.044 Uiso 1 1 calc R . . C47 C 0.3677(3) 0.5626(3) 0.53273(18) 0.0414(9) Uani 1 1 d . . . H47 H 0.3640 0.6128 0.4941 0.050 Uiso 1 1 calc R . . C48 C 0.2955(3) 0.4903(3) 0.54959(18) 0.0383(8) Uani 1 1 d . . . C49 C 0.2054(4) 0.4668(3) 0.5201(2) 0.0498(10) Uani 1 1 d . . . H49 H 0.1803 0.5051 0.4793 0.060 Uiso 1 1 calc R . . C50 C 0.1547(4) 0.3870(4) 0.5518(2) 0.0534(11) Uani 1 1 d . . . H50 H 0.0947 0.3691 0.5324 0.064 Uiso 1 1 calc R . . C51 C 0.1905(4) 0.3316(3) 0.6125(2) 0.0506(10) Uani 1 1 d . . . H51 H 0.1533 0.2774 0.6332 0.061 Uiso 1 1 calc R . . C52 C 0.2773(3) 0.3532(3) 0.64287(19) 0.0398(8) Uani 1 1 d . . . H52 H 0.3008 0.3156 0.6840 0.048 Uiso 1 1 calc R . . C53 C 0.3296(3) 0.4337(3) 0.60988(16) 0.0339(8) Uani 1 1 d . . . C54 C 0.4397(4) 0.7074(3) 0.74039(19) 0.0482(10) Uani 1 1 d . . . H54 H 0.4605 0.7748 0.7405 0.058 Uiso 1 1 calc R . . C55 C 0.3458(3) 0.6791(3) 0.77755(18) 0.0419(9) Uani 1 1 d . . . C56 C 0.2611(4) 0.7273(4) 0.8223(2) 0.0556(12) Uani 1 1 d . . . H56 H 0.2587 0.7978 0.8340 0.067 Uiso 1 1 calc R . . C57 C 0.1826(4) 0.6719(4) 0.8489(2) 0.0594(12) Uani 1 1 d . . . H57 H 0.1243 0.7043 0.8788 0.071 Uiso 1 1 calc R . . C58 C 0.1870(4) 0.5674(4) 0.8324(2) 0.0577(12) Uani 1 1 d . . . H58 H 0.1311 0.5304 0.8518 0.069 Uiso 1 1 calc R . . C59 C 0.2688(3) 0.5159(4) 0.78942(18) 0.0442(9) Uani 1 1 d . . . H59 H 0.2714 0.4446 0.7789 0.053 Uiso 1 1 calc R . . C60 C 0.3470(3) 0.5744(3) 0.76241(16) 0.0337(8) Uani 1 1 d . . . C61 C 0.4749(3) 0.4520(3) 0.68523(17) 0.0363(8) Uani 1 1 d . . . H61A H 0.4568 0.3870 0.7121 0.044 Uiso 1 1 calc R . . H61B H 0.5599 0.4342 0.6767 0.044 Uiso 1 1 calc R . . S2 S 0.76462(8) 0.18183(8) 0.62157(5) 0.0376(2) Uani 1 1 d . . . F4 F 0.8912(3) 0.2673(3) 0.53290(15) 0.1016(12) Uani 1 1 d . . . F5 F 0.9260(3) 0.2814(3) 0.62803(17) 0.0983(11) Uani 1 1 d . . . F6 F 0.9859(2) 0.1247(3) 0.59107(17) 0.0882(10) Uani 1 1 d . . . O4 O 0.6829(3) 0.2888(3) 0.61810(16) 0.0631(9) Uani 1 1 d . . . O5 O 0.7911(3) 0.1267(3) 0.68457(13) 0.0546(8) Uani 1 1 d . . . O6 O 0.7484(3) 0.1123(3) 0.57728(15) 0.0605(8) Uani 1 1 d . . . C62 C 0.8994(4) 0.2151(4) 0.5917(2) 0.0541(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 0.03227(15) 0.04161(15) 0.04089(15) -0.00660(12) 0.00794(11) -0.01418(12) N1 0.0256(14) 0.0285(14) 0.0346(15) -0.0054(12) 0.0035(11) -0.0115(11) N2 0.0245(14) 0.0250(13) 0.0406(16) -0.0058(12) 0.0040(12) -0.0085(11) N3 0.0244(14) 0.0275(14) 0.0358(15) -0.0045(12) 0.0012(11) -0.0077(11) N4 0.0240(14) 0.0316(15) 0.0407(16) -0.0049(13) 0.0038(12) -0.0076(12) N5 0.0293(15) 0.0231(13) 0.0369(15) -0.0019(12) 0.0021(12) -0.0099(11) N6 0.0364(16) 0.0257(14) 0.0392(16) -0.0070(13) 0.0069(13) -0.0144(12) N7 0.0265(14) 0.0257(13) 0.0345(15) -0.0026(12) 0.0007(11) -0.0105(11) N8 0.0274(15) 0.0286(14) 0.0384(16) -0.0037(12) 0.0020(12) -0.0080(12) C1 0.0272(17) 0.0298(17) 0.0414(19) -0.0093(15) -0.0013(15) -0.0062(14) C2 0.040(2) 0.0245(15) 0.0340(18) -0.0100(14) -0.0020(15) -0.0146(14) C3 0.052(2) 0.0264(17) 0.042(2) -0.0033(16) -0.0075(18) -0.0132(16) C4 0.072(3) 0.037(2) 0.0303(19) -0.0031(16) -0.0022(19) -0.026(2) C5 0.061(3) 0.046(2) 0.036(2) -0.0134(18) 0.0142(18) -0.033(2) C6 0.0361(19) 0.0324(18) 0.0394(19) -0.0081(15) 0.0057(15) -0.0170(15) C7 0.0347(18) 0.0245(15) 0.0325(17) -0.0053(14) 0.0044(14) -0.0157(14) C8 0.0262(17) 0.0323(18) 0.043(2) -0.0095(16) 0.0025(15) -0.0053(14) C9 0.0309(18) 0.0273(16) 0.0327(17) -0.0056(14) -0.0047(14) -0.0051(14) C10 0.035(2) 0.0291(17) 0.042(2) -0.0066(15) -0.0076(16) -0.0057(15) C11 0.042(2) 0.0265(17) 0.050(2) -0.0022(16) -0.0107(17) -0.0149(15) C12 0.0310(19) 0.0371(19) 0.046(2) 0.0001(17) -0.0023(16) -0.0159(15) C13 0.0271(17) 0.0309(17) 0.044(2) -0.0076(16) 0.0028(15) -0.0095(14) C14 0.0264(16) 0.0253(15) 0.0327(17) -0.0022(14) -0.0027(13) -0.0081(13) C15 0.0263(17) 0.0284(16) 0.0375(18) -0.0072(14) 0.0015(14) -0.0120(13) C16 0.051(2) 0.0221(15) 0.0343(18) -0.0020(14) 0.0013(16) -0.0137(15) C17 0.046(2) 0.0188(15) 0.041(2) -0.0070(14) -0.0079(16) -0.0113(14) C18 0.057(3) 0.0268(18) 0.050(2) -0.0077(17) -0.020(2) -0.0068(17) C19 0.041(2) 0.0294(19) 0.070(3) -0.0060(19) -0.018(2) -0.0045(16) C20 0.0289(19) 0.0299(18) 0.071(3) -0.0076(19) -0.0027(18) -0.0089(15) C21 0.0317(18) 0.0253(16) 0.047(2) -0.0004(15) -0.0001(15) -0.0136(14) C22 0.0297(17) 0.0204(15) 0.0433(19) -0.0051(14) -0.0049(15) -0.0100(13) C23 0.043(2) 0.0261(16) 0.0313(18) -0.0037(14) -0.0046(15) -0.0051(15) C24 0.0366(19) 0.0258(16) 0.0329(18) -0.0003(14) -0.0065(15) -0.0105(14) C25 0.058(3) 0.0296(18) 0.041(2) -0.0025(16) -0.0083(18) -0.0215(17) C26 0.052(2) 0.040(2) 0.047(2) 0.0032(18) -0.0081(18) -0.0303(19) C27 0.035(2) 0.041(2) 0.044(2) 0.0043(17) -0.0030(16) -0.0202(16) C28 0.0290(18) 0.0293(16) 0.0391(19) -0.0015(15) -0.0005(14) -0.0131(14) C29 0.0312(18) 0.0268(16) 0.0322(17) 0.0017(14) -0.0044(14) -0.0120(14) C30 0.0283(17) 0.0257(15) 0.0331(17) -0.0054(14) 0.0026(13) -0.0124(13) S1 0.0263(4) 0.0473(5) 0.0402(5) -0.0124(4) -0.0001(4) -0.0097(4) F1 0.0455(14) 0.0413(13) 0.0848(18) 0.0088(12) 0.0027(12) -0.0154(11) F2 0.0296(11) 0.0495(13) 0.0676(14) -0.0118(11) 0.0138(10) -0.0215(10) F3 0.0444(14) 0.0850(19) 0.0550(14) -0.0273(14) -0.0083(11) -0.0199(13) O1 0.0411(16) 0.077(2) 0.0432(15) -0.0192(15) 0.0033(12) -0.0272(15) O2 0.0298(14) 0.092(2) 0.0454(15) -0.0226(16) 0.0073(12) -0.0248(15) O3 0.064(2) 0.0395(16) 0.087(2) -0.0068(16) -0.0182(18) 0.0026(15) C31 0.0283(18) 0.0375(19) 0.046(2) -0.0094(17) 0.0073(15) -0.0140(15) Ag2 0.0494(2) 0.0675(2) 0.0577(2) 0.00475(17) 0.00507(16) -0.03728(17) N9 0.0274(15) 0.0400(16) 0.0393(16) -0.0050(14) -0.0028(12) -0.0148(13) N10 0.0245(15) 0.0428(17) 0.0517(19) -0.0022(15) -0.0024(13) -0.0130(13) N11 0.0323(16) 0.0406(17) 0.0361(16) -0.0007(13) 0.0000(13) -0.0149(13) N12 0.0422(19) 0.0479(19) 0.0406(17) 0.0053(15) -0.0052(14) -0.0214(16) N13 0.0357(17) 0.0362(16) 0.0349(16) -0.0031(13) 0.0013(13) -0.0146(13) N14 0.0404(18) 0.0456(18) 0.0344(16) -0.0001(14) 0.0031(13) -0.0176(15) N15 0.0342(16) 0.0354(16) 0.0388(16) -0.0037(13) 0.0019(13) -0.0155(13) N16 0.053(2) 0.052(2) 0.0422(18) -0.0012(16) 0.0018(15) -0.0329(17) C32 0.033(2) 0.043(2) 0.053(2) -0.0049(18) -0.0087(17) -0.0158(17) C33 0.0271(18) 0.0332(18) 0.042(2) -0.0103(16) -0.0026(15) -0.0050(14) C34 0.042(2) 0.0361(19) 0.045(2) -0.0111(17) -0.0090(17) -0.0018(17) C35 0.047(2) 0.057(3) 0.036(2) -0.0028(19) -0.0006(18) -0.010(2) C36 0.047(2) 0.062(3) 0.051(2) 0.008(2) -0.0023(19) -0.031(2) C37 0.037(2) 0.051(2) 0.048(2) -0.0032(19) -0.0077(17) -0.0191(18) C38 0.0233(17) 0.0349(18) 0.0406(19) -0.0057(16) -0.0007(14) -0.0064(14) C39 0.051(2) 0.045(2) 0.040(2) 0.0015(18) -0.0072(18) -0.0148(19) C40 0.036(2) 0.047(2) 0.038(2) -0.0081(18) -0.0046(16) -0.0045(17) C41 0.040(2) 0.057(3) 0.069(3) -0.011(2) -0.015(2) 0.005(2) C42 0.029(2) 0.070(3) 0.111(4) -0.015(3) -0.020(2) -0.006(2) C43 0.036(2) 0.067(3) 0.106(4) -0.014(3) -0.008(2) -0.023(2) C44 0.031(2) 0.049(2) 0.063(3) -0.007(2) -0.0015(18) -0.0122(18) C45 0.0288(18) 0.045(2) 0.0333(18) -0.0074(16) 0.0011(14) -0.0092(16) C46 0.0272(18) 0.047(2) 0.0369(19) -0.0083(17) 0.0040(15) -0.0112(16) C47 0.045(2) 0.045(2) 0.0340(19) 0.0009(17) 0.0013(16) -0.0152(18) C48 0.039(2) 0.0383(19) 0.040(2) -0.0077(17) -0.0004(16) -0.0130(16) C49 0.058(3) 0.048(2) 0.046(2) -0.0035(19) -0.015(2) -0.017(2) C50 0.054(3) 0.053(3) 0.065(3) -0.013(2) -0.013(2) -0.028(2) C51 0.058(3) 0.041(2) 0.061(3) -0.009(2) 0.002(2) -0.027(2) C52 0.043(2) 0.0300(18) 0.047(2) -0.0047(16) 0.0017(17) -0.0123(16) C53 0.0327(19) 0.0312(17) 0.0362(19) -0.0085(15) 0.0021(15) -0.0048(15) C54 0.057(3) 0.042(2) 0.052(2) -0.003(2) -0.006(2) -0.025(2) C55 0.044(2) 0.038(2) 0.043(2) -0.0054(17) -0.0086(17) -0.0086(17) C56 0.058(3) 0.048(2) 0.058(3) -0.023(2) -0.009(2) 0.001(2) C57 0.040(2) 0.075(3) 0.061(3) -0.028(3) 0.009(2) -0.005(2) C58 0.035(2) 0.086(4) 0.055(3) -0.014(3) 0.0136(19) -0.024(2) C59 0.035(2) 0.053(2) 0.048(2) -0.0097(19) 0.0041(17) -0.0169(18) C60 0.0277(18) 0.0374(19) 0.0358(18) -0.0038(16) -0.0026(14) -0.0088(15) C61 0.0301(18) 0.0383(19) 0.0392(19) -0.0044(16) -0.0022(15) -0.0072(15) S2 0.0305(5) 0.0404(5) 0.0445(5) -0.0115(4) 0.0004(4) -0.0114(4) F4 0.140(3) 0.086(2) 0.071(2) 0.0086(18) 0.042(2) -0.042(2) F5 0.095(2) 0.120(3) 0.117(3) -0.045(2) 0.030(2) -0.086(2) F6 0.0386(15) 0.090(2) 0.130(3) -0.009(2) 0.0181(16) -0.0158(15) O4 0.0537(19) 0.0519(18) 0.077(2) -0.0197(17) -0.0058(16) 0.0039(15) O5 0.065(2) 0.0607(19) 0.0427(16) 0.0009(14) 0.0060(14) -0.0308(16) O6 0.0484(18) 0.0601(19) 0.080(2) -0.0370(17) -0.0127(16) -0.0094(15) C62 0.055(3) 0.058(3) 0.051(3) -0.005(2) 0.011(2) -0.022(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 2.230(3) . ? Ag1 N8 2.263(3) . ? Ag1 N6 2.381(3) . ? Ag1 O1 2.462(3) . ? N1 N2 1.366(4) . ? N1 C7 1.369(4) . ? N1 C15 1.440(4) . ? N2 C1 1.331(4) . ? N3 N4 1.365(4) . ? N3 C14 1.369(4) . ? N3 C15 1.444(4) . ? N4 C8 1.316(4) . ? N5 N6 1.369(4) . ? N5 C22 1.379(4) . ? N5 C30 1.436(4) . ? N6 C16 1.328(4) . ? N7 N8 1.369(4) . ? N7 C29 1.371(4) . ? N7 C30 1.457(4) . ? N8 C23 1.324(4) . ? C1 C2 1.413(5) . ? C1 H1 0.9500 . ? C2 C7 1.399(5) . ? C2 C3 1.411(5) . ? C3 C4 1.369(5) . ? C3 H3 0.9500 . ? C4 C5 1.410(6) . ? C4 H4 0.9500 . ? C5 C6 1.383(5) . ? C5 H5 0.9500 . ? C6 C7 1.399(5) . ? C6 H6 0.9500 . ? C8 C9 1.419(5) . ? C8 H8 0.9500 . ? C9 C10 1.404(5) . ? C9 C14 1.411(4) . ? C10 C11 1.368(5) . ? C10 H10 0.9500 . ? C11 C12 1.399(5) . ? C11 H11 0.9500 . ? C12 C13 1.381(5) . ? C12 H12 0.9500 . ? C13 C14 1.395(5) . ? C13 H13 0.9500 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.406(5) . ? C16 H16 0.9500 . ? C17 C18 1.399(5) . ? C17 C22 1.415(5) . ? C18 C19 1.360(6) . ? C18 H18 0.9500 . ? C19 C20 1.411(6) . ? C19 H19 0.9500 . ? C20 C21 1.362(5) . ? C20 H20 0.9500 . ? C21 C22 1.390(5) . ? C21 H21 0.9500 . ? C23 C24 1.417(5) . ? C23 H23 0.9500 . ? C24 C29 1.400(5) . ? C24 C25 1.407(5) . ? C25 C26 1.371(6) . ? C25 H25 0.9500 . ? C26 C27 1.404(5) . ? C26 H26 0.9500 . ? C27 C28 1.375(5) . ? C27 H27 0.9500 . ? C28 C29 1.404(5) . ? C28 H28 0.9500 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? S1 O3 1.433(3) . ? S1 O2 1.443(3) . ? S1 O1 1.444(3) . ? S1 C31 1.822(4) . ? F1 C31 1.332(4) . ? F2 C31 1.317(4) . ? F3 C31 1.330(4) . ? Ag2 N14 2.263(3) . ? Ag2 N12 2.312(3) . ? Ag2 N10 2.328(3) . ? Ag2 N16 2.461(3) . ? N9 N10 1.374(4) . ? N9 C38 1.380(4) . ? N9 C46 1.433(4) . ? N10 C32 1.322(5) . ? N11 N12 1.370(4) . ? N11 C45 1.373(4) . ? N11 C46 1.446(4) . ? N12 C39 1.307(5) . ? N13 C53 1.365(5) . ? N13 N14 1.370(4) . ? N13 C61 1.433(4) . ? N14 C47 1.318(5) . ? N15 C60 1.371(4) . ? N15 N16 1.372(4) . ? N15 C61 1.431(5) . ? N16 C54 1.303(5) . ? C32 C33 1.407(5) . ? C32 H32 0.9500 . ? C33 C38 1.397(5) . ? C33 C34 1.409(5) . ? C34 C35 1.357(6) . ? C34 H34 0.9500 . ? C35 C36 1.400(6) . ? C35 H35 0.9500 . ? C36 C37 1.377(5) . ? C36 H36 0.9500 . ? C37 C38 1.383(5) . ? C37 H37 0.9500 . ? C39 C40 1.411(6) . ? C39 H39 0.9500 . ? C40 C45 1.400(5) . ? C40 C41 1.420(6) . ? C41 C42 1.346(7) . ? C41 H41 0.9500 . ? C42 C43 1.400(7) . ? C42 H42 0.9500 . ? C43 C44 1.383(6) . ? C43 H43 0.9500 . ? C44 C45 1.395(6) . ? C44 H44 0.9500 . ? C46 H46A 0.9900 . ? C46 H46B 0.9900 . ? C47 C48 1.412(5) . ? C47 H47 0.9500 . ? C48 C53 1.396(5) . ? C48 C49 1.408(6) . ? C49 C50 1.378(6) . ? C49 H49 0.9500 . ? C50 C51 1.402(6) . ? C50 H50 0.9500 . ? C51 C52 1.374(6) . ? C51 H51 0.9500 . ? C52 C53 1.405(5) . ? C52 H52 0.9500 . ? C54 C55 1.415(6) . ? C54 H54 0.9500 . ? C55 C60 1.400(5) . ? C55 C56 1.404(6) . ? C56 C57 1.358(7) . ? C56 H56 0.9500 . ? C57 C58 1.398(7) . ? C57 H57 0.9500 . ? C58 C59 1.373(5) . ? C58 H58 0.9500 . ? C59 C60 1.384(5) . ? C59 H59 0.9500 . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? S2 O5 1.422(3) . ? S2 O4 1.430(3) . ? S2 O6 1.431(3) . ? S2 C62 1.819(5) . ? F4 C62 1.313(5) . ? F5 C62 1.328(5) . ? F6 C62 1.316(5) . ? 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 N8 139.27(10) . . ? N2 Ag1 N6 109.50(10) . . ? N8 Ag1 N6 89.93(10) . . ? N2 Ag1 O1 97.65(9) . . ? N8 Ag1 O1 110.98(10) . . ? N6 Ag1 O1 106.55(10) . . ? N2 N1 C7 110.6(3) . . ? N2 N1 C15 121.1(3) . . ? C7 N1 C15 128.3(3) . . ? C1 N2 N1 106.7(3) . . ? C1 N2 Ag1 125.2(2) . . ? N1 N2 Ag1 124.7(2) . . ? N4 N3 C14 111.9(3) . . ? N4 N3 C15 119.8(3) . . ? C14 N3 C15 128.4(3) . . ? C8 N4 N3 105.8(3) . . ? N6 N5 C22 110.9(3) . . ? N6 N5 C30 120.4(3) . . ? C22 N5 C30 128.3(3) . . ? C16 N6 N5 106.6(3) . . ? C16 N6 Ag1 129.2(2) . . ? N5 N6 Ag1 114.14(19) . . ? N8 N7 C29 110.6(3) . . ? N8 N7 C30 119.7(3) . . ? C29 N7 C30 129.5(3) . . ? C23 N8 N7 106.9(3) . . ? C23 N8 Ag1 127.6(2) . . ? N7 N8 Ag1 116.78(19) . . ? N2 C1 C2 110.8(3) . . ? N2 C1 H1 124.6 . . ? C2 C1 H1 124.6 . . ? C7 C2 C3 119.3(3) . . ? C7 C2 C1 105.0(3) . . ? C3 C2 C1 135.7(3) . . ? C4 C3 C2 118.2(4) . . ? C4 C3 H3 120.9 . . ? C2 C3 H3 120.9 . . ? C3 C4 C5 121.3(3) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? C6 C5 C4 122.2(4) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C5 C6 C7 115.7(3) . . ? C5 C6 H6 122.1 . . ? C7 C6 H6 122.1 . . ? N1 C7 C2 107.0(3) . . ? N1 C7 C6 129.8(3) . . ? C2 C7 C6 123.3(3) . . ? N4 C8 C9 112.1(3) . . ? N4 C8 H8 124.0 . . ? C9 C8 H8 124.0 . . ? C10 C9 C14 119.3(3) . . ? C10 C9 C8 136.5(3) . . ? C14 C9 C8 104.2(3) . . ? C11 C10 C9 118.1(3) . . ? C11 C10 H10 120.9 . . ? C9 C10 H10 120.9 . . ? C10 C11 C12 122.0(3) . . ? C10 C11 H11 119.0 . . ? C12 C11 H11 119.0 . . ? C13 C12 C11 121.6(3) . . ? C13 C12 H12 119.2 . . ? C11 C12 H12 119.2 . . ? C12 C13 C14 116.6(3) . . ? C12 C13 H13 121.7 . . ? C14 C13 H13 121.7 . . ? N3 C14 C13 131.5(3) . . ? N3 C14 C9 106.0(3) . . ? C13 C14 C9 122.4(3) . . ? N1 C15 N3 113.0(3) . . ? N1 C15 H15A 109.0 . . ? N3 C15 H15A 109.0 . . ? N1 C15 H15B 109.0 . . ? N3 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? N6 C16 C17 111.4(3) . . ? N6 C16 H16 124.3 . . ? C17 C16 H16 124.3 . . ? C18 C17 C16 136.2(4) . . ? C18 C17 C22 118.7(4) . . ? C16 C17 C22 105.1(3) . . ? C19 C18 C17 118.5(4) . . ? C19 C18 H18 120.7 . . ? C17 C18 H18 120.7 . . ? C18 C19 C20 121.3(4) . . ? C18 C19 H19 119.4 . . ? C20 C19 H19 119.4 . . ? C21 C20 C19 122.3(4) . . ? C21 C20 H20 118.9 . . ? C19 C20 H20 118.9 . . ? C20 C21 C22 116.1(3) . . ? C20 C21 H21 121.9 . . ? C22 C21 H21 121.9 . . ? N5 C22 C21 131.0(3) . . ? N5 C22 C17 106.0(3) . . ? C21 C22 C17 123.0(3) . . ? N8 C23 C24 110.8(3) . . ? N8 C23 H23 124.6 . . ? C24 C23 H23 124.6 . . ? C29 C24 C25 120.1(3) . . ? C29 C24 C23 105.0(3) . . ? C25 C24 C23 134.9(3) . . ? C26 C25 C24 117.6(4) . . ? C26 C25 H25 121.2 . . ? C24 C25 H25 121.2 . . ? C25 C26 C27 121.5(3) . . ? C25 C26 H26 119.2 . . ? C27 C26 H26 119.2 . . ? C28 C27 C26 122.3(4) . . ? C28 C27 H27 118.9 . . ? C26 C27 H27 118.9 . . ? C27 C28 C29 116.2(3) . . ? C27 C28 H28 121.9 . . ? C29 C28 H28 121.9 . . ? N7 C29 C24 106.8(3) . . ? N7 C29 C28 131.0(3) . . ? C24 C29 C28 122.2(3) . . ? N5 C30 N7 112.4(3) . . ? N5 C30 H30A 109.1 . . ? N7 C30 H30A 109.1 . . ? N5 C30 H30B 109.1 . . ? N7 C30 H30B 109.1 . . ? H30A C30 H30B 107.9 . . ? O3 S1 O2 116.0(2) . . ? O3 S1 O1 114.6(2) . . ? O2 S1 O1 114.41(18) . . ? O3 S1 C31 104.36(18) . . ? O2 S1 C31 103.52(17) . . ? O1 S1 C31 101.43(17) . . ? S1 O1 Ag1 121.06(15) . . ? F2 C31 F3 107.9(3) . . ? F2 C31 F1 107.9(3) . . ? F3 C31 F1 107.6(3) . . ? F2 C31 S1 111.9(3) . . ? F3 C31 S1 111.2(2) . . ? F1 C31 S1 110.2(3) . . ? N14 Ag2 N12 153.56(12) . . ? N14 Ag2 N10 112.66(11) . . ? N12 Ag2 N10 84.97(11) . . ? N14 Ag2 N16 84.46(11) . . ? N12 Ag2 N16 97.71(11) . . ? N10 Ag2 N16 133.41(11) . . ? N10 N9 C38 110.7(3) . . ? N10 N9 C46 118.4(3) . . ? C38 N9 C46 130.6(3) . . ? C32 N10 N9 106.5(3) . . ? C32 N10 Ag2 127.5(3) . . ? N9 N10 Ag2 118.8(2) . . ? N12 N11 C45 110.3(3) . . ? N12 N11 C46 120.2(3) . . ? C45 N11 C46 129.1(3) . . ? C39 N12 N11 107.0(3) . . ? C39 N12 Ag2 133.4(3) . . ? N11 N12 Ag2 119.4(2) . . ? C53 N13 N14 110.4(3) . . ? C53 N13 C61 129.4(3) . . ? N14 N13 C61 119.3(3) . . ? C47 N14 N13 107.1(3) . . ? C47 N14 Ag2 130.7(3) . . ? N13 N14 Ag2 121.3(2) . . ? C60 N15 N16 110.7(3) . . ? C60 N15 C61 129.6(3) . . ? N16 N15 C61 119.4(3) . . ? C54 N16 N15 106.6(3) . . ? C54 N16 Ag2 127.1(3) . . ? N15 N16 Ag2 112.7(2) . . ? N10 C32 C33 111.0(3) . . ? N10 C32 H32 124.5 . . ? C33 C32 H32 124.5 . . ? C38 C33 C32 105.9(3) . . ? C38 C33 C34 118.8(4) . . ? C32 C33 C34 135.2(4) . . ? C35 C34 C33 118.3(4) . . ? C35 C34 H34 120.8 . . ? C33 C34 H34 120.8 . . ? C34 C35 C36 121.2(4) . . ? C34 C35 H35 119.4 . . ? C36 C35 H35 119.4 . . ? C37 C36 C35 122.3(4) . . ? C37 C36 H36 118.8 . . ? C35 C36 H36 118.8 . . ? C36 C37 C38 115.8(4) . . ? C36 C37 H37 122.1 . . ? C38 C37 H37 122.1 . . ? N9 C38 C37 130.6(3) . . ? N9 C38 C33 105.9(3) . . ? C37 C38 C33 123.4(3) . . ? N12 C39 C40 111.2(4) . . ? N12 C39 H39 124.4 . . ? C40 C39 H39 124.4 . . ? C45 C40 C39 105.0(3) . . ? C45 C40 C41 119.1(4) . . ? C39 C40 C41 135.9(4) . . ? C42 C41 C40 117.9(4) . . ? C42 C41 H41 121.1 . . ? C40 C41 H41 121.1 . . ? C41 C42 C43 122.3(4) . . ? C41 C42 H42 118.8 . . ? C43 C42 H42 118.8 . . ? C44 C43 C42 121.9(4) . . ? C44 C43 H43 119.1 . . ? C42 C43 H43 119.1 . . ? C43 C44 C45 115.8(4) . . ? C43 C44 H44 122.1 . . ? C45 C44 H44 122.1 . . ? N11 C45 C44 130.6(3) . . ? N11 C45 C40 106.3(3) . . ? C44 C45 C40 123.0(3) . . ? N9 C46 N11 113.2(3) . . ? N9 C46 H46A 108.9 . . ? N11 C46 H46A 108.9 . . ? N9 C46 H46B 108.9 . . ? N11 C46 H46B 108.9 . . ? H46A C46 H46B 107.8 . . ? N14 C47 C48 110.4(3) . . ? N14 C47 H47 124.8 . . ? C48 C47 H47 124.8 . . ? C53 C48 C49 119.5(4) . . ? C53 C48 C47 105.4(3) . . ? C49 C48 C47 135.0(4) . . ? C50 C49 C48 118.3(4) . . ? C50 C49 H49 120.8 . . ? C48 C49 H49 120.8 . . ? C49 C50 C51 120.9(4) . . ? C49 C50 H50 119.5 . . ? C51 C50 H50 119.5 . . ? C52 C51 C50 122.3(4) . . ? C52 C51 H51 118.9 . . ? C50 C51 H51 118.9 . . ? C51 C52 C53 116.5(4) . . ? C51 C52 H52 121.7 . . ? C53 C52 H52 121.7 . . ? N13 C53 C48 106.6(3) . . ? N13 C53 C52 131.0(3) . . ? C48 C53 C52 122.4(3) . . ? N16 C54 C55 111.7(4) . . ? N16 C54 H54 124.2 . . ? C55 C54 H54 124.2 . . ? C60 C55 C56 118.5(4) . . ? C60 C55 C54 104.7(3) . . ? C56 C55 C54 136.8(4) . . ? C57 C56 C55 119.2(4) . . ? C57 C56 H56 120.4 . . ? C55 C56 H56 120.4 . . ? C56 C57 C58 120.4(4) . . ? C56 C57 H57 119.8 . . ? C58 C57 H57 119.8 . . ? C59 C58 C57 122.7(4) . . ? C59 C58 H58 118.6 . . ? C57 C58 H58 118.6 . . ? C58 C59 C60 115.9(4) . . ? C58 C59 H59 122.1 . . ? C60 C59 H59 122.1 . . ? N15 C60 C59 130.4(3) . . ? N15 C60 C55 106.3(3) . . ? C59 C60 C55 123.3(3) . . ? N15 C61 N13 112.3(3) . . ? N15 C61 H61A 109.1 . . ? N13 C61 H61A 109.1 . . ? N15 C61 H61B 109.1 . . ? N13 C61 H61B 109.1 . . ? H61A C61 H61B 107.9 . . ? O5 S2 O4 115.6(2) . . ? O5 S2 O6 114.8(2) . . ? O4 S2 O6 114.89(19) . . ? O5 S2 C62 102.8(2) . . ? O4 S2 C62 102.9(2) . . ? O6 S2 C62 103.2(2) . . ? F4 C62 F6 107.3(4) . . ? F4 C62 F5 107.1(4) . . ? F6 C62 F5 108.7(4) . . ? F4 C62 S2 111.6(4) . . ? F6 C62 S2 111.4(3) . . ? F5 C62 S2 110.5(3) . . ? 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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 N1 N2 C1 -0.5(3) . . . . ? C15 N1 N2 C1 -177.5(3) . . . . ? C7 N1 N2 Ag1 -160.6(2) . . . . ? C15 N1 N2 Ag1 22.4(4) . . . . ? N8 Ag1 N2 C1 100.1(3) . . . . ? N6 Ag1 N2 C1 -14.1(3) . . . . ? O1 Ag1 N2 C1 -124.7(3) . . . . ? N8 Ag1 N2 N1 -103.4(3) . . . . ? N6 Ag1 N2 N1 142.4(2) . . . . ? O1 Ag1 N2 N1 31.8(2) . . . . ? C14 N3 N4 C8 0.7(4) . . . . ? C15 N3 N4 C8 -179.9(3) . . . . ? C22 N5 N6 C16 0.5(4) . . . . ? C30 N5 N6 C16 174.1(3) . . . . ? C22 N5 N6 Ag1 -148.3(2) . . . . ? C30 N5 N6 Ag1 25.3(3) . . . . ? N2 Ag1 N6 C16 15.9(3) . . . . ? N8 Ag1 N6 C16 -127.6(3) . . . . ? O1 Ag1 N6 C16 120.5(3) . . . . ? N2 Ag1 N6 N5 156.1(2) . . . . ? N8 Ag1 N6 N5 12.7(2) . . . . ? O1 Ag1 N6 N5 -99.2(2) . . . . ? C29 N7 N8 C23 -1.8(4) . . . . ? C30 N7 N8 C23 -177.2(3) . . . . ? C29 N7 N8 Ag1 148.3(2) . . . . ? C30 N7 N8 Ag1 -27.1(3) . . . . ? N2 Ag1 N8 C23 10.9(4) . . . . ? N6 Ag1 N8 C23 131.5(3) . . . . ? O1 Ag1 N8 C23 -120.7(3) . . . . ? N2 Ag1 N8 N7 -132.1(2) . . . . ? N6 Ag1 N8 N7 -11.4(2) . . . . ? O1 Ag1 N8 N7 96.3(2) . . . . ? N1 N2 C1 C2 0.1(4) . . . . ? Ag1 N2 C1 C2 160.1(2) . . . . ? N2 C1 C2 C7 0.4(4) . . . . ? N2 C1 C2 C3 -177.5(4) . . . . ? C7 C2 C3 C4 0.9(5) . . . . ? C1 C2 C3 C4 178.5(4) . . . . ? C2 C3 C4 C5 0.4(5) . . . . ? C3 C4 C5 C6 -0.8(6) . . . . ? C4 C5 C6 C7 -0.3(5) . . . . ? N2 N1 C7 C2 0.8(4) . . . . ? C15 N1 C7 C2 177.5(3) . . . . ? N2 N1 C7 C6 -179.6(3) . . . . ? C15 N1 C7 C6 -2.8(6) . . . . ? C3 C2 C7 N1 177.6(3) . . . . ? C1 C2 C7 N1 -0.7(3) . . . . ? C3 C2 C7 C6 -2.1(5) . . . . ? C1 C2 C7 C6 179.6(3) . . . . ? C5 C6 C7 N1 -177.9(3) . . . . ? C5 C6 C7 C2 1.7(5) . . . . ? N3 N4 C8 C9 -0.8(4) . . . . ? N4 C8 C9 C10 179.5(4) . . . . ? N4 C8 C9 C14 0.5(4) . . . . ? C14 C9 C10 C11 -0.4(5) . . . . ? C8 C9 C10 C11 -179.2(4) . . . . ? C9 C10 C11 C12 0.5(5) . . . . ? C10 C11 C12 C13 0.2(6) . . . . ? C11 C12 C13 C14 -1.0(5) . . . . ? N4 N3 C14 C13 -179.0(3) . . . . ? C15 N3 C14 C13 1.7(6) . . . . ? N4 N3 C14 C9 -0.4(4) . . . . ? C15 N3 C14 C9 -179.7(3) . . . . ? C12 C13 C14 N3 179.5(3) . . . . ? C12 C13 C14 C9 1.1(5) . . . . ? C10 C9 C14 N3 -179.2(3) . . . . ? C8 C9 C14 N3 0.0(3) . . . . ? C10 C9 C14 C13 -0.4(5) . . . . ? C8 C9 C14 C13 178.7(3) . . . . ? N2 N1 C15 N3 103.1(3) . . . . ? C7 N1 C15 N3 -73.3(4) . . . . ? N4 N3 C15 N1 104.8(3) . . . . ? C14 N3 C15 N1 -76.0(4) . . . . ? N5 N6 C16 C17 0.1(4) . . . . ? Ag1 N6 C16 C17 142.6(2) . . . . ? N6 C16 C17 C18 -178.7(4) . . . . ? N6 C16 C17 C22 -0.6(4) . . . . ? C16 C17 C18 C19 178.2(4) . . . . ? C22 C17 C18 C19 0.3(5) . . . . ? C17 C18 C19 C20 1.6(6) . . . . ? C18 C19 C20 C21 -1.9(6) . . . . ? C19 C20 C21 C22 0.2(5) . . . . ? N6 N5 C22 C21 -179.3(3) . . . . ? C30 N5 C22 C21 7.8(6) . . . . ? N6 N5 C22 C17 -0.9(4) . . . . ? C30 N5 C22 C17 -173.8(3) . . . . ? C20 C21 C22 N5 180.0(3) . . . . ? C20 C21 C22 C17 1.8(5) . . . . ? C18 C17 C22 N5 179.4(3) . . . . ? C16 C17 C22 N5 0.9(4) . . . . ? C18 C17 C22 C21 -2.1(5) . . . . ? C16 C17 C22 C21 179.4(3) . . . . ? N7 N8 C23 C24 1.5(4) . . . . ? Ag1 N8 C23 C24 -144.3(2) . . . . ? N8 C23 C24 C29 -0.7(4) . . . . ? N8 C23 C24 C25 178.9(4) . . . . ? C29 C24 C25 C26 1.1(5) . . . . ? C23 C24 C25 C26 -178.4(4) . . . . ? C24 C25 C26 C27 -0.6(6) . . . . ? C25 C26 C27 C28 -0.5(6) . . . . ? C26 C27 C28 C29 1.0(5) . . . . ? N8 N7 C29 C24 1.4(4) . . . . ? C30 N7 C29 C24 176.2(3) . . . . ? N8 N7 C29 C28 -178.1(3) . . . . ? C30 N7 C29 C28 -3.3(6) . . . . ? C25 C24 C29 N7 179.9(3) . . . . ? C23 C24 C29 N7 -0.4(4) . . . . ? C25 C24 C29 C28 -0.6(5) . . . . ? C23 C24 C29 C28 179.1(3) . . . . ? C27 C28 C29 N7 178.9(3) . . . . ? C27 C28 C29 C24 -0.5(5) . . . . ? N6 N5 C30 N7 -77.6(4) . . . . ? C22 N5 C30 N7 94.7(4) . . . . ? N8 N7 C30 N5 79.4(4) . . . . ? C29 N7 C30 N5 -95.0(4) . . . . ? O3 S1 O1 Ag1 -101.1(2) . . . . ? O2 S1 O1 Ag1 36.4(3) . . . . ? C31 S1 O1 Ag1 147.11(18) . . . . ? N2 Ag1 O1 S1 152.40(19) . . . . ? N8 Ag1 O1 S1 -57.1(2) . . . . ? N6 Ag1 O1 S1 39.4(2) . . . . ? O3 S1 C31 F2 -66.1(3) . . . . ? O2 S1 C31 F2 172.1(3) . . . . ? O1 S1 C31 F2 53.2(3) . . . . ? O3 S1 C31 F3 54.6(3) . . . . ? O2 S1 C31 F3 -67.2(3) . . . . ? O1 S1 C31 F3 174.0(3) . . . . ? O3 S1 C31 F1 173.8(3) . . . . ? O2 S1 C31 F1 52.0(3) . . . . ? O1 S1 C31 F1 -66.8(3) . . . . ? C38 N9 N10 C32 -0.9(4) . . . . ? C46 N9 N10 C32 -175.2(3) . . . . ? C38 N9 N10 Ag2 151.7(2) . . . . ? C46 N9 N10 Ag2 -22.6(4) . . . . ? N14 Ag2 N10 C32 -32.5(3) . . . . ? N12 Ag2 N10 C32 127.1(3) . . . . ? N16 Ag2 N10 C32 -137.0(3) . . . . ? N14 Ag2 N10 N9 -178.7(2) . . . . ? N12 Ag2 N10 N9 -19.1(3) . . . . ? N16 Ag2 N10 N9 76.8(3) . . . . ? C45 N11 N12 C39 -0.8(4) . . . . ? C46 N11 N12 C39 -175.0(3) . . . . ? C45 N11 N12 Ag2 -176.0(2) . . . . ? C46 N11 N12 Ag2 9.8(4) . . . . ? N14 Ag2 N12 C39 -14.7(5) . . . . ? N10 Ag2 N12 C39 -148.4(4) . . . . ? N16 Ag2 N12 C39 78.4(4) . . . . ? N14 Ag2 N12 N11 159.0(2) . . . . ? N10 Ag2 N12 N11 25.3(3) . . . . ? N16 Ag2 N12 N11 -107.9(3) . . . . ? C53 N13 N14 C47 -0.6(4) . . . . ? C61 N13 N14 C47 -171.3(3) . . . . ? C53 N13 N14 Ag2 169.7(2) . . . . ? C61 N13 N14 Ag2 -1.0(4) . . . . ? N12 Ag2 N14 C47 -126.7(4) . . . . ? N10 Ag2 N14 C47 2.1(4) . . . . ? N16 Ag2 N14 C47 137.1(4) . . . . ? N12 Ag2 N14 N13 65.6(4) . . . . ? N10 Ag2 N14 N13 -165.7(2) . . . . ? N16 Ag2 N14 N13 -30.6(3) . . . . ? C60 N15 N16 C54 1.5(4) . . . . ? C61 N15 N16 C54 175.3(3) . . . . ? C60 N15 N16 Ag2 -142.1(2) . . . . ? C61 N15 N16 Ag2 31.7(4) . . . . ? N14 Ag2 N16 C54 -119.1(4) . . . . ? N12 Ag2 N16 C54 87.4(4) . . . . ? N10 Ag2 N16 C54 -3.0(4) . . . . ? N14 Ag2 N16 N15 15.5(2) . . . . ? N12 Ag2 N16 N15 -137.9(2) . . . . ? N10 Ag2 N16 N15 131.7(2) . . . . ? N9 N10 C32 C33 0.2(4) . . . . ? Ag2 N10 C32 C33 -149.3(2) . . . . ? N10 C32 C33 C38 0.6(4) . . . . ? N10 C32 C33 C34 177.7(4) . . . . ? C38 C33 C34 C35 -0.9(5) . . . . ? C32 C33 C34 C35 -177.7(4) . . . . ? C33 C34 C35 C36 -1.2(6) . . . . ? C34 C35 C36 C37 1.6(7) . . . . ? C35 C36 C37 C38 0.3(6) . . . . ? N10 N9 C38 C37 179.4(4) . . . . ? C46 N9 C38 C37 -7.2(6) . . . . ? N10 N9 C38 C33 1.3(4) . . . . ? C46 N9 C38 C33 174.6(3) . . . . ? C36 C37 C38 N9 179.6(4) . . . . ? C36 C37 C38 C33 -2.5(6) . . . . ? C32 C33 C38 N9 -1.1(4) . . . . ? C34 C33 C38 N9 -178.8(3) . . . . ? C32 C33 C38 C37 -179.4(3) . . . . ? C34 C33 C38 C37 2.9(5) . . . . ? N11 N12 C39 C40 1.2(4) . . . . ? Ag2 N12 C39 C40 175.5(3) . . . . ? N12 C39 C40 C45 -1.2(4) . . . . ? N12 C39 C40 C41 177.4(4) . . . . ? C45 C40 C41 C42 -0.3(7) . . . . ? C39 C40 C41 C42 -178.7(5) . . . . ? C40 C41 C42 C43 0.7(8) . . . . ? C41 C42 C43 C44 -1.0(9) . . . . ? C42 C43 C44 C45 0.8(7) . . . . ? N12 N11 C45 C44 -178.2(4) . . . . ? C46 N11 C45 C44 -4.7(6) . . . . ? N12 N11 C45 C40 0.0(4) . . . . ? C46 N11 C45 C40 173.6(3) . . . . ? C43 C44 C45 N11 177.6(4) . . . . ? C43 C44 C45 C40 -0.4(6) . . . . ? C39 C40 C45 N11 0.6(4) . . . . ? C41 C40 C45 N11 -178.2(3) . . . . ? C39 C40 C45 C44 179.1(4) . . . . ? C41 C40 C45 C44 0.2(6) . . . . ? N10 N9 C46 N11 76.4(4) . . . . ? C38 N9 C46 N11 -96.6(4) . . . . ? N12 N11 C46 N9 -68.6(4) . . . . ? C45 N11 C46 N9 118.4(4) . . . . ? N13 N14 C47 C48 -0.1(4) . . . . ? Ag2 N14 C47 C48 -169.2(2) . . . . ? N14 C47 C48 C53 0.8(4) . . . . ? N14 C47 C48 C49 -179.0(4) . . . . ? C53 C48 C49 C50 -0.8(6) . . . . ? C47 C48 C49 C50 178.9(4) . . . . ? C48 C49 C50 C51 1.0(7) . . . . ? C49 C50 C51 C52 -0.5(7) . . . . ? C50 C51 C52 C53 -0.3(6) . . . . ? N14 N13 C53 C48 1.1(4) . . . . ? C61 N13 C53 C48 170.6(3) . . . . ? N14 N13 C53 C52 179.6(3) . . . . ? C61 N13 C53 C52 -10.9(6) . . . . ? C49 C48 C53 N13 178.7(3) . . . . ? C47 C48 C53 N13 -1.1(4) . . . . ? C49 C48 C53 C52 0.0(6) . . . . ? C47 C48 C53 C52 -179.8(3) . . . . ? C51 C52 C53 N13 -177.8(4) . . . . ? C51 C52 C53 C48 0.6(5) . . . . ? N15 N16 C54 C55 -0.8(4) . . . . ? Ag2 N16 C54 C55 136.0(3) . . . . ? N16 C54 C55 C60 -0.3(5) . . . . ? N16 C54 C55 C56 178.8(4) . . . . ? C60 C55 C56 C57 -0.8(6) . . . . ? C54 C55 C56 C57 -179.8(5) . . . . ? C55 C56 C57 C58 0.9(7) . . . . ? C56 C57 C58 C59 -0.1(7) . . . . ? C57 C58 C59 C60 -0.6(6) . . . . ? N16 N15 C60 C59 -179.7(4) . . . . ? C61 N15 C60 C59 7.4(6) . . . . ? N16 N15 C60 C55 -1.7(4) . . . . ? C61 N15 C60 C55 -174.7(3) . . . . ? C58 C59 C60 N15 178.3(4) . . . . ? C58 C59 C60 C55 0.7(6) . . . . ? C56 C55 C60 N15 -178.1(3) . . . . ? C54 C55 C60 N15 1.2(4) . . . . ? C56 C55 C60 C59 0.0(6) . . . . ? C54 C55 C60 C59 179.3(4) . . . . ? C60 N15 C61 N13 87.3(4) . . . . ? N16 N15 C61 N13 -85.2(4) . . . . ? C53 N13 C61 N15 -103.6(4) . . . . ? N14 N13 C61 N15 65.1(4) . . . . ? O5 S2 C62 F4 180.0(3) . . . . ? O4 S2 C62 F4 -59.6(4) . . . . ? O6 S2 C62 F4 60.2(4) . . . . ? O5 S2 C62 F6 60.0(4) . . . . ? O4 S2 C62 F6 -179.6(3) . . . . ? O6 S2 C62 F6 -59.7(4) . . . . ? O5 S2 C62 F5 -61.0(4) . . . . ? O4 S2 C62 F5 59.5(4) . . . . ? O6 S2 C62 F5 179.3(3) . . . . ? _diffrn_measured_fraction_theta_max 0.988 _diffrn_reflns_theta_full 30.53 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 1.897 _refine_diff_density_min -1.553 _refine_diff_density_rms 0.117 data_19 _database_code_depnum_ccdc_archive 'CCDC 917677' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H24 Ag N8, Cl O4' _chemical_formula_sum 'C30 H24 Ag Cl N8 O4' _chemical_formula_weight 703.89 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' 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.3429(3) _cell_length_b 12.3026(4) _cell_length_c 20.4226(6) _cell_angle_alpha 90.00 _cell_angle_beta 95.3780(10) _cell_angle_gamma 90.00 _cell_volume 2837.37(15) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9935 _cell_measurement_theta_min 2.45 _cell_measurement_theta_max 30.33 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.46 _exptl_crystal_size_mid 0.36 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.648 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1424 _exptl_absorpt_coefficient_mu 0.858 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6937 _exptl_absorpt_correction_T_max 0.8404 _exptl_absorpt_process_details ; APEX2 Software Suite; Bruker 2005. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker-Nonius X8kappa APEX II CCD area detector ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 37798 _diffrn_reflns_av_R_equivalents 0.0274 _diffrn_reflns_av_sigmaI/netI 0.0207 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 30.53 _reflns_number_total 8441 _reflns_number_gt 5901 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker, 2007)' _computing_cell_refinement 'APEX2 Software Suite (Bruker, 2007)' _computing_data_reduction 'APEX2 Software Suite (Bruker, 2007)' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL and publCIF (Westrip, 2010)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0547P)^2^+2.9405P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8441 _refine_ls_number_parameters 397 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0534 _refine_ls_R_factor_gt 0.0413 _refine_ls_wR_factor_ref 0.1177 _refine_ls_wR_factor_gt 0.1092 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.040 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.88506(2) 0.69183(2) 0.082161(11) 0.04960(10) Uani 1 1 d . . . N1 N 0.74816(17) 0.63477(16) -0.05671(10) 0.0305(4) Uani 1 1 d . . . N2 N 0.85631(19) 0.61680(18) -0.02159(11) 0.0354(5) Uani 1 1 d . . . N3 N 0.66031(19) 0.78814(16) -0.00691(11) 0.0311(4) Uani 1 1 d . . . N4 N 0.7325(2) 0.82138(18) 0.04662(11) 0.0371(5) Uani 1 1 d . . . C1 C 0.9294(2) 0.5879(2) -0.06430(13) 0.0347(6) Uani 1 1 d . . . H1 H 1.0103 0.5702 -0.0532 0.042 Uiso 1 1 calc R . . C2 C 0.8732(2) 0.58611(19) -0.12910(13) 0.0308(5) Uani 1 1 d . . . C3 C 0.9076(2) 0.5605(2) -0.19162(14) 0.0377(6) Uani 1 1 d . . . H3 H 0.9859 0.5369 -0.1969 0.045 Uiso 1 1 calc R . . C4 C 0.8253(3) 0.5704(2) -0.24446(15) 0.0439(7) Uani 1 1 d . . . H4 H 0.8469 0.5536 -0.2871 0.053 Uiso 1 1 calc R . . C5 C 0.7090(3) 0.6052(2) -0.23703(15) 0.0454(7) Uani 1 1 d . . . H5 H 0.6548 0.6129 -0.2751 0.055 Uiso 1 1 calc R . . C6 C 0.6714(2) 0.6284(2) -0.17649(14) 0.0376(6) Uani 1 1 d . . . H6 H 0.5923 0.6501 -0.1717 0.045 Uiso 1 1 calc R . . C7 C 0.7560(2) 0.61840(17) -0.12214(12) 0.0290(5) Uani 1 1 d . . . C8 C 0.7334(2) 0.9282(2) 0.04499(13) 0.0375(6) Uani 1 1 d . . . H8 H 0.7762 0.9726 0.0770 0.045 Uiso 1 1 calc R . . C9 C 0.6627(2) 0.96890(19) -0.01050(13) 0.0310(5) Uani 1 1 d . . . C10 C 0.6335(2) 1.0721(2) -0.03688(14) 0.0386(6) Uani 1 1 d . . . H10 H 0.6622 1.1364 -0.0151 0.046 Uiso 1 1 calc R . . C11 C 0.5629(3) 1.0771(2) -0.09464(15) 0.0431(7) Uani 1 1 d . . . H11 H 0.5432 1.1461 -0.1136 0.052 Uiso 1 1 calc R . . C12 C 0.5183(3) 0.9822(2) -0.12692(14) 0.0414(6) Uani 1 1 d . . . H12 H 0.4692 0.9891 -0.1670 0.050 Uiso 1 1 calc R . . C13 C 0.5436(2) 0.8800(2) -0.10213(13) 0.0334(5) Uani 1 1 d . . . H13 H 0.5125 0.8163 -0.1236 0.040 Uiso 1 1 calc R . . C14 C 0.61762(19) 0.87526(18) -0.04357(12) 0.0272(5) Uani 1 1 d . . . C15 C 0.6508(2) 0.67393(19) -0.02283(14) 0.0337(5) Uani 1 1 d . . . H15A H 0.6474 0.6319 0.0183 0.040 Uiso 1 1 calc R . . H15B H 0.5759 0.6612 -0.0507 0.040 Uiso 1 1 calc R . . N5 N 0.9901(2) 0.70015(17) 0.23340(11) 0.0344(5) Uani 1 1 d . . . N6 N 0.8929(2) 0.66678(19) 0.19392(11) 0.0377(5) Uani 1 1 d . . . N7 N 1.1432(2) 0.73292(18) 0.16146(11) 0.0355(5) Uani 1 1 d . . . N8 N 1.0947(2) 0.7180(2) 0.09771(12) 0.0397(5) Uani 1 1 d . . . C16 C 0.8293(2) 0.6065(2) 0.23066(14) 0.0389(6) Uani 1 1 d . . . H16 H 0.7570 0.5720 0.2153 0.047 Uiso 1 1 calc R . . C17 C 0.8828(2) 0.5998(2) 0.29645(13) 0.0355(6) Uani 1 1 d . . . C18 C 0.8549(3) 0.5498(3) 0.35473(16) 0.0478(7) Uani 1 1 d . . . H18 H 0.7856 0.5067 0.3558 0.057 Uiso 1 1 calc R . . C19 C 0.9312(3) 0.5655(3) 0.41030(16) 0.0557(8) Uani 1 1 d . . . H19 H 0.9139 0.5332 0.4505 0.067 Uiso 1 1 calc R . . C20 C 1.0340(3) 0.6282(3) 0.40883(15) 0.0514(8) Uani 1 1 d . . . H20 H 1.0842 0.6374 0.4483 0.062 Uiso 1 1 calc R . . C21 C 1.0645(3) 0.6763(2) 0.35281(14) 0.0414(6) Uani 1 1 d . . . H21 H 1.1351 0.7176 0.3523 0.050 Uiso 1 1 calc R . . C22 C 0.9865(2) 0.6620(2) 0.29594(13) 0.0320(5) Uani 1 1 d . . . C23 C 1.1791(2) 0.6771(2) 0.06528(14) 0.0370(6) Uani 1 1 d . . . H23 H 1.1696 0.6583 0.0200 0.044 Uiso 1 1 calc R . . C24 C 1.2864(2) 0.66437(19) 0.10658(12) 0.0308(5) Uani 1 1 d . . . C25 C 1.4009(2) 0.6278(2) 0.09766(14) 0.0350(5) Uani 1 1 d . . . H25 H 1.4203 0.6014 0.0563 0.042 Uiso 1 1 calc R . . C26 C 1.4840(2) 0.6316(2) 0.15123(15) 0.0405(6) Uani 1 1 d . . . H26 H 1.5625 0.6079 0.1465 0.049 Uiso 1 1 calc R . . C27 C 1.4560(3) 0.6695(2) 0.21259(15) 0.0429(7) Uani 1 1 d . . . H27 H 1.5163 0.6713 0.2482 0.051 Uiso 1 1 calc R . . C28 C 1.3446(3) 0.7039(2) 0.22288(14) 0.0400(6) Uani 1 1 d . . . H28 H 1.3257 0.7283 0.2648 0.048 Uiso 1 1 calc R . . C29 C 1.2596(2) 0.70142(18) 0.16826(13) 0.0314(5) Uani 1 1 d . . . C30 C 1.0707(3) 0.7778(2) 0.20871(15) 0.0405(6) Uani 1 1 d . . . H30A H 1.0244 0.8391 0.1882 0.049 Uiso 1 1 calc R . . H30B H 1.1228 0.8071 0.2462 0.049 Uiso 1 1 calc R . . Cl1 Cl 0.69020(5) 0.38960(5) 0.10176(3) 0.03393(14) Uani 1 1 d . . . O1 O 0.8020(3) 0.4362(3) 0.0996(2) 0.1152(15) Uani 1 1 d U . . O2 O 0.6565(4) 0.3880(3) 0.16498(16) 0.1123(14) Uani 1 1 d U . . O3 O 0.6087(3) 0.4580(2) 0.06228(15) 0.0831(9) Uani 1 1 d U . . O4 O 0.6902(3) 0.28377(18) 0.07310(14) 0.0667(7) Uani 1 1 d 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 0.04187(13) 0.07714(18) 0.02811(14) 0.00567(10) -0.00562(10) 0.01402(10) N1 0.0268(9) 0.0336(10) 0.0305(11) 0.0049(8) 0.0004(8) 0.0030(7) N2 0.0309(10) 0.0422(11) 0.0319(12) 0.0094(9) -0.0037(9) 0.0061(8) N3 0.0312(10) 0.0332(10) 0.0286(11) 0.0036(8) 0.0002(9) 0.0028(8) N4 0.0348(11) 0.0480(12) 0.0273(11) 0.0011(9) -0.0030(9) 0.0033(9) C1 0.0290(11) 0.0415(13) 0.0332(14) 0.0068(10) 0.0016(11) 0.0045(10) C2 0.0314(11) 0.0289(10) 0.0321(13) 0.0044(9) 0.0029(10) -0.0035(8) C3 0.0409(13) 0.0365(12) 0.0366(15) -0.0011(10) 0.0085(12) -0.0069(10) C4 0.0575(17) 0.0438(14) 0.0310(15) -0.0058(11) 0.0071(13) -0.0129(13) C5 0.0524(16) 0.0438(14) 0.0369(16) -0.0055(11) -0.0124(13) -0.0077(12) C6 0.0356(12) 0.0344(12) 0.0407(15) -0.0032(10) -0.0072(12) -0.0020(10) C7 0.0306(11) 0.0242(9) 0.0319(13) 0.0027(8) 0.0006(10) -0.0038(8) C8 0.0345(12) 0.0491(14) 0.0285(13) -0.0055(10) 0.0009(11) -0.0007(11) C9 0.0294(11) 0.0355(11) 0.0289(13) -0.0045(9) 0.0064(10) -0.0009(9) C10 0.0436(14) 0.0316(12) 0.0419(16) -0.0040(10) 0.0117(12) -0.0005(10) C11 0.0523(16) 0.0320(12) 0.0458(17) 0.0059(11) 0.0081(14) 0.0077(11) C12 0.0455(14) 0.0417(13) 0.0353(15) 0.0047(11) -0.0045(12) 0.0119(11) C13 0.0339(12) 0.0344(11) 0.0310(13) -0.0014(9) -0.0030(10) 0.0033(9) C14 0.0244(10) 0.0316(10) 0.0262(12) 0.0014(8) 0.0046(9) 0.0011(8) C15 0.0300(11) 0.0317(11) 0.0398(15) 0.0071(10) 0.0058(11) -0.0003(9) N5 0.0356(11) 0.0394(11) 0.0279(12) -0.0034(8) 0.0022(9) 0.0017(8) N6 0.0349(11) 0.0495(12) 0.0282(12) -0.0034(9) 0.0014(10) 0.0053(9) N7 0.0362(11) 0.0431(11) 0.0276(12) -0.0031(9) 0.0045(9) 0.0015(9) N8 0.0363(11) 0.0531(13) 0.0291(12) 0.0036(9) 0.0001(10) 0.0020(10) C16 0.0287(11) 0.0555(16) 0.0327(14) -0.0058(11) 0.0035(11) 0.0024(11) C17 0.0311(11) 0.0447(13) 0.0310(14) -0.0023(10) 0.0051(11) 0.0070(10) C18 0.0397(14) 0.0658(19) 0.0396(17) 0.0059(14) 0.0132(13) 0.0065(13) C19 0.0540(18) 0.083(2) 0.0316(16) 0.0133(15) 0.0090(15) 0.0150(17) C20 0.0488(16) 0.073(2) 0.0313(16) -0.0030(13) -0.0029(14) 0.0161(15) C21 0.0393(14) 0.0521(15) 0.0319(15) -0.0087(11) -0.0014(12) 0.0046(11) C22 0.0344(12) 0.0357(11) 0.0263(13) -0.0055(9) 0.0043(10) 0.0076(9) C23 0.0340(12) 0.0508(15) 0.0261(14) -0.0008(10) 0.0020(11) -0.0028(10) C24 0.0345(12) 0.0302(10) 0.0270(13) 0.0006(9) -0.0003(10) -0.0040(9) C25 0.0368(12) 0.0342(12) 0.0339(14) -0.0011(10) 0.0024(11) -0.0013(9) C26 0.0352(12) 0.0402(13) 0.0446(16) 0.0018(11) -0.0035(12) 0.0029(10) C27 0.0443(15) 0.0460(14) 0.0358(15) 0.0037(11) -0.0098(13) -0.0029(11) C28 0.0499(16) 0.0424(14) 0.0267(14) -0.0031(10) -0.0018(12) -0.0059(11) C29 0.0366(12) 0.0299(11) 0.0275(13) 0.0004(8) 0.0017(11) -0.0041(9) C30 0.0481(15) 0.0350(12) 0.0394(16) -0.0038(10) 0.0102(13) 0.0017(11) Cl1 0.0278(3) 0.0351(3) 0.0387(4) -0.0008(2) 0.0024(2) -0.0017(2) O1 0.0543(16) 0.121(3) 0.174(4) -0.072(3) 0.030(2) -0.0396(17) O2 0.202(4) 0.081(2) 0.063(2) 0.0277(16) 0.059(2) 0.021(2) O3 0.113(2) 0.0641(16) 0.0671(18) 0.0067(13) -0.0190(17) 0.0283(16) O4 0.0827(18) 0.0401(11) 0.0733(18) -0.0123(11) -0.0146(14) 0.0009(11) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N6 2.297(2) . ? Ag1 N2 2.306(2) . ? Ag1 N8 2.391(2) . ? Ag1 N4 2.414(2) . ? N1 C7 1.362(3) . ? N1 N2 1.380(3) . ? N1 C15 1.440(3) . ? N2 C1 1.308(4) . ? N3 N4 1.366(3) . ? N3 C14 1.370(3) . ? N3 C15 1.444(3) . ? N4 C8 1.315(4) . ? C1 C2 1.415(3) . ? C1 H1 0.9500 . ? C2 C3 1.406(4) . ? C2 C7 1.407(3) . ? C3 C4 1.365(4) . ? C3 H3 0.9500 . ? C4 C5 1.408(5) . ? C4 H4 0.9500 . ? C5 C6 1.375(4) . ? C5 H5 0.9500 . ? C6 C7 1.403(3) . ? C6 H6 0.9500 . ? C8 C9 1.417(3) . ? C8 H8 0.9500 . ? C9 C10 1.406(4) . ? C9 C14 1.407(3) . ? C10 C11 1.364(4) . ? C10 H10 0.9500 . ? C11 C12 1.411(4) . ? C11 H11 0.9500 . ? C12 C13 1.376(3) . ? C12 H12 0.9500 . ? C13 C14 1.397(3) . ? C13 H13 0.9500 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? N5 C22 1.365(4) . ? N5 N6 1.366(3) . ? N5 C30 1.445(4) . ? N6 C16 1.317(4) . ? N7 C29 1.370(3) . ? N7 N8 1.377(3) . ? N7 C30 1.435(4) . ? N8 C23 1.314(4) . ? C16 C17 1.424(4) . ? C16 H16 0.9500 . ? C17 C18 1.402(4) . ? C17 C22 1.405(4) . ? C18 C19 1.375(4) . ? C18 H18 0.9500 . ? C19 C20 1.400(5) . ? C19 H19 0.9500 . ? C20 C21 1.361(5) . ? C20 H20 0.9500 . ? C21 C22 1.403(3) . ? C21 H21 0.9500 . ? C23 C24 1.423(3) . ? C23 H23 0.9500 . ? C24 C29 1.400(4) . ? C24 C25 1.403(4) . ? C25 C26 1.377(4) . ? C25 H25 0.9500 . ? C26 C27 1.401(4) . ? C26 H26 0.9500 . ? C27 C28 1.368(4) . ? C27 H27 0.9500 . ? C28 C29 1.405(3) . ? C28 H28 0.9500 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? Cl1 O2 1.380(3) . ? Cl1 O1 1.396(3) . ? Cl1 O4 1.428(2) . ? Cl1 O3 1.440(3) . ? 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 N6 Ag1 N2 148.04(8) . . ? N6 Ag1 N8 86.59(8) . . ? N2 Ag1 N8 103.25(8) . . ? N6 Ag1 N4 110.34(8) . . ? N2 Ag1 N4 87.27(7) . . ? N8 Ag1 N4 128.83(8) . . ? C7 N1 N2 110.5(2) . . ? C7 N1 C15 130.1(2) . . ? N2 N1 C15 119.2(2) . . ? C1 N2 N1 106.6(2) . . ? C1 N2 Ag1 132.67(17) . . ? N1 N2 Ag1 117.12(17) . . ? N4 N3 C14 110.97(19) . . ? N4 N3 C15 119.88(19) . . ? C14 N3 C15 128.6(2) . . ? C8 N4 N3 106.6(2) . . ? C8 N4 Ag1 131.33(18) . . ? N3 N4 Ag1 113.71(15) . . ? N2 C1 C2 111.7(2) . . ? N2 C1 H1 124.2 . . ? C2 C1 H1 124.2 . . ? C3 C2 C7 120.1(2) . . ? C3 C2 C1 135.5(2) . . ? C7 C2 C1 104.4(2) . . ? C4 C3 C2 118.0(3) . . ? C4 C3 H3 121.0 . . ? C2 C3 H3 121.0 . . ? C3 C4 C5 121.4(3) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C6 C5 C4 122.2(3) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C5 C6 C7 116.5(3) . . ? C5 C6 H6 121.8 . . ? C7 C6 H6 121.8 . . ? N1 C7 C6 131.3(2) . . ? N1 C7 C2 106.8(2) . . ? C6 C7 C2 121.8(2) . . ? N4 C8 C9 111.6(2) . . ? N4 C8 H8 124.2 . . ? C9 C8 H8 124.2 . . ? C10 C9 C14 119.6(2) . . ? C10 C9 C8 136.1(2) . . ? C14 C9 C8 104.3(2) . . ? C11 C10 C9 118.1(2) . . ? C11 C10 H10 121.0 . . ? C9 C10 H10 121.0 . . ? C10 C11 C12 121.5(2) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C13 C12 C11 122.1(2) . . ? C13 C12 H12 119.0 . . ? C11 C12 H12 119.0 . . ? C12 C13 C14 116.2(2) . . ? C12 C13 H13 121.9 . . ? C14 C13 H13 121.9 . . ? N3 C14 C13 130.9(2) . . ? N3 C14 C9 106.5(2) . . ? C13 C14 C9 122.6(2) . . ? N1 C15 N3 112.9(2) . . ? N1 C15 H15A 109.0 . . ? N3 C15 H15A 109.0 . . ? N1 C15 H15B 109.0 . . ? N3 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C22 N5 N6 110.8(2) . . ? C22 N5 C30 129.0(2) . . ? N6 N5 C30 119.6(2) . . ? C16 N6 N5 106.7(2) . . ? C16 N6 Ag1 132.01(18) . . ? N5 N6 Ag1 120.02(18) . . ? C29 N7 N8 110.7(2) . . ? C29 N7 C30 130.3(2) . . ? N8 N7 C30 118.9(2) . . ? C23 N8 N7 106.4(2) . . ? C23 N8 Ag1 130.04(18) . . ? N7 N8 Ag1 116.57(18) . . ? N6 C16 C17 111.2(2) . . ? N6 C16 H16 124.4 . . ? C17 C16 H16 124.4 . . ? C18 C17 C22 120.1(2) . . ? C18 C17 C16 135.8(3) . . ? C22 C17 C16 104.1(2) . . ? C19 C18 C17 117.7(3) . . ? C19 C18 H18 121.2 . . ? C17 C18 H18 121.2 . . ? C18 C19 C20 121.4(3) . . ? C18 C19 H19 119.3 . . ? C20 C19 H19 119.3 . . ? C21 C20 C19 122.4(3) . . ? C21 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? C20 C21 C22 116.8(3) . . ? C20 C21 H21 121.6 . . ? C22 C21 H21 121.6 . . ? N5 C22 C21 131.3(3) . . ? N5 C22 C17 107.0(2) . . ? C21 C22 C17 121.7(3) . . ? N8 C23 C24 111.5(2) . . ? N8 C23 H23 124.3 . . ? C24 C23 H23 124.3 . . ? C29 C24 C25 120.2(2) . . ? C29 C24 C23 104.6(2) . . ? C25 C24 C23 135.2(3) . . ? C26 C25 C24 117.4(3) . . ? C26 C25 H25 121.3 . . ? C24 C25 H25 121.3 . . ? C25 C26 C27 121.8(3) . . ? C25 C26 H26 119.1 . . ? C27 C26 H26 119.1 . . ? C28 C27 C26 122.0(2) . . ? C28 C27 H27 119.0 . . ? C26 C27 H27 119.0 . . ? C27 C28 C29 116.5(3) . . ? C27 C28 H28 121.7 . . ? C29 C28 H28 121.7 . . ? N7 C29 C24 106.8(2) . . ? N7 C29 C28 131.1(3) . . ? C24 C29 C28 122.1(3) . . ? N7 C30 N5 113.7(2) . . ? N7 C30 H30A 108.8 . . ? N5 C30 H30A 108.8 . . ? N7 C30 H30B 108.8 . . ? N5 C30 H30B 108.8 . . ? H30A C30 H30B 107.7 . . ? O2 Cl1 O1 111.5(3) . . ? O2 Cl1 O4 112.4(2) . . ? O1 Cl1 O4 109.08(19) . . ? O2 Cl1 O3 108.2(2) . . ? O1 Cl1 O3 106.2(2) . . ? O4 Cl1 O3 109.16(16) . . ? 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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 N1 N2 C1 -1.1(3) . . . . ? C15 N1 N2 C1 -176.5(2) . . . . ? C7 N1 N2 Ag1 160.14(15) . . . . ? C15 N1 N2 Ag1 -15.3(3) . . . . ? N6 Ag1 N2 C1 -102.3(3) . . . . ? N8 Ag1 N2 C1 2.9(2) . . . . ? N4 Ag1 N2 C1 132.2(2) . . . . ? N6 Ag1 N2 N1 102.42(19) . . . . ? N8 Ag1 N2 N1 -152.39(17) . . . . ? N4 Ag1 N2 N1 -23.07(17) . . . . ? C14 N3 N4 C8 1.5(3) . . . . ? C15 N3 N4 C8 173.5(2) . . . . ? C14 N3 N4 Ag1 -150.48(17) . . . . ? C15 N3 N4 Ag1 21.5(3) . . . . ? N6 Ag1 N4 C8 84.3(3) . . . . ? N2 Ag1 N4 C8 -123.1(3) . . . . ? N8 Ag1 N4 C8 -18.2(3) . . . . ? N6 Ag1 N4 N3 -132.52(18) . . . . ? N2 Ag1 N4 N3 20.12(18) . . . . ? N8 Ag1 N4 N3 124.96(17) . . . . ? N1 N2 C1 C2 0.4(3) . . . . ? Ag1 N2 C1 C2 -156.76(17) . . . . ? N2 C1 C2 C3 -178.9(3) . . . . ? N2 C1 C2 C7 0.5(3) . . . . ? C7 C2 C3 C4 1.5(4) . . . . ? C1 C2 C3 C4 -179.1(3) . . . . ? C2 C3 C4 C5 -0.1(4) . . . . ? C3 C4 C5 C6 -1.6(4) . . . . ? C4 C5 C6 C7 1.6(4) . . . . ? N2 N1 C7 C6 -178.8(2) . . . . ? C15 N1 C7 C6 -4.0(4) . . . . ? N2 N1 C7 C2 1.4(2) . . . . ? C15 N1 C7 C2 176.2(2) . . . . ? C5 C6 C7 N1 -179.9(2) . . . . ? C5 C6 C7 C2 -0.1(3) . . . . ? C3 C2 C7 N1 178.4(2) . . . . ? C1 C2 C7 N1 -1.1(2) . . . . ? C3 C2 C7 C6 -1.5(3) . . . . ? C1 C2 C7 C6 179.0(2) . . . . ? N3 N4 C8 C9 -0.8(3) . . . . ? Ag1 N4 C8 C9 144.3(2) . . . . ? N4 C8 C9 C10 -178.8(3) . . . . ? N4 C8 C9 C14 -0.2(3) . . . . ? C14 C9 C10 C11 -0.8(4) . . . . ? C8 C9 C10 C11 177.7(3) . . . . ? C9 C10 C11 C12 1.0(4) . . . . ? C10 C11 C12 C13 -0.1(5) . . . . ? C11 C12 C13 C14 -0.9(4) . . . . ? N4 N3 C14 C13 178.7(3) . . . . ? C15 N3 C14 C13 7.7(5) . . . . ? N4 N3 C14 C9 -1.6(3) . . . . ? C15 N3 C14 C9 -172.7(3) . . . . ? C12 C13 C14 N3 -179.3(3) . . . . ? C12 C13 C14 C9 1.2(4) . . . . ? C10 C9 C14 N3 180.0(2) . . . . ? C8 C9 C14 N3 1.1(3) . . . . ? C10 C9 C14 C13 -0.3(4) . . . . ? C8 C9 C14 C13 -179.3(2) . . . . ? C7 N1 C15 N3 -98.4(3) . . . . ? N2 N1 C15 N3 75.9(3) . . . . ? N4 N3 C15 N1 -80.0(3) . . . . ? C14 N3 C15 N1 90.3(3) . . . . ? C22 N5 N6 C16 -1.1(3) . . . . ? C30 N5 N6 C16 -173.3(2) . . . . ? C22 N5 N6 Ag1 -169.79(16) . . . . ? C30 N5 N6 Ag1 18.0(3) . . . . ? N2 Ag1 N6 C16 -38.6(3) . . . . ? N8 Ag1 N6 C16 -148.3(3) . . . . ? N4 Ag1 N6 C16 81.3(3) . . . . ? N2 Ag1 N6 N5 126.84(19) . . . . ? N8 Ag1 N6 N5 17.07(18) . . . . ? N4 Ag1 N6 N5 -113.30(18) . . . . ? C29 N7 N8 C23 0.5(3) . . . . ? C30 N7 N8 C23 179.7(2) . . . . ? C29 N7 N8 Ag1 154.29(17) . . . . ? C30 N7 N8 Ag1 -26.5(3) . . . . ? N6 Ag1 N8 C23 133.4(2) . . . . ? N2 Ag1 N8 C23 -15.8(3) . . . . ? N4 Ag1 N8 C23 -113.1(2) . . . . ? N6 Ag1 N8 N7 -12.97(19) . . . . ? N2 Ag1 N8 N7 -162.19(18) . . . . ? N4 Ag1 N8 N7 100.54(19) . . . . ? N5 N6 C16 C17 0.8(3) . . . . ? Ag1 N6 C16 C17 167.66(18) . . . . ? N6 C16 C17 C18 179.1(3) . . . . ? N6 C16 C17 C22 -0.3(3) . . . . ? C22 C17 C18 C19 0.9(4) . . . . ? C16 C17 C18 C19 -178.5(3) . . . . ? C17 C18 C19 C20 -0.7(5) . . . . ? C18 C19 C20 C21 -0.4(5) . . . . ? C19 C20 C21 C22 1.1(5) . . . . ? N6 N5 C22 C21 -178.9(3) . . . . ? C30 N5 C22 C21 -7.6(4) . . . . ? N6 N5 C22 C17 0.9(3) . . . . ? C30 N5 C22 C17 172.2(2) . . . . ? C20 C21 C22 N5 178.9(3) . . . . ? C20 C21 C22 C17 -0.9(4) . . . . ? C18 C17 C22 N5 -179.9(2) . . . . ? C16 C17 C22 N5 -0.4(3) . . . . ? C18 C17 C22 C21 -0.1(4) . . . . ? C16 C17 C22 C21 179.4(2) . . . . ? N7 N8 C23 C24 -0.4(3) . . . . ? Ag1 N8 C23 C24 -149.38(18) . . . . ? N8 C23 C24 C29 0.2(3) . . . . ? N8 C23 C24 C25 -178.5(3) . . . . ? C29 C24 C25 C26 -0.9(4) . . . . ? C23 C24 C25 C26 177.7(3) . . . . ? C24 C25 C26 C27 0.5(4) . . . . ? C25 C26 C27 C28 0.5(4) . . . . ? C26 C27 C28 C29 -1.2(4) . . . . ? N8 N7 C29 C24 -0.4(3) . . . . ? C30 N7 C29 C24 -179.4(3) . . . . ? N8 N7 C29 C28 178.3(3) . . . . ? C30 N7 C29 C28 -0.7(5) . . . . ? C25 C24 C29 N7 179.1(2) . . . . ? C23 C24 C29 N7 0.1(3) . . . . ? C25 C24 C29 C28 0.2(4) . . . . ? C23 C24 C29 C28 -178.7(2) . . . . ? C27 C28 C29 N7 -177.7(3) . . . . ? C27 C28 C29 C24 0.8(4) . . . . ? C29 N7 C30 N5 -102.7(3) . . . . ? N8 N7 C30 N5 78.3(3) . . . . ? C22 N5 C30 N7 116.2(3) . . . . ? N6 N5 C30 N7 -73.2(3) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 30.53 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 0.839 _refine_diff_density_min -0.747 _refine_diff_density_rms 0.072 data_21 _database_code_depnum_ccdc_archive 'CCDC 917678' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H24 Ag N8, B F4' _chemical_formula_sum 'C30 H24 Ag B F4 N8' _chemical_formula_weight 691.25 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' B B 0.0013 0.0007 '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' F F 0.0171 0.0103 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.3230(7) _cell_length_b 12.1730(8) _cell_length_c 20.4002(13) _cell_angle_alpha 90.00 _cell_angle_beta 95.9300(10) _cell_angle_gamma 90.00 _cell_volume 2796.8(3) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9868 _cell_measurement_theta_min 2.46 _cell_measurement_theta_max 30.47 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.30 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.642 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1392 _exptl_absorpt_coefficient_mu 0.785 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6949 _exptl_absorpt_correction_T_max 0.7986 _exptl_absorpt_process_details ; APEX2 Software Suite; Bruker 2005. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker-Nonius X8kappa APEX II CCD area detector ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 40511 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0176 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.81 _diffrn_reflns_theta_max 25.25 _reflns_number_total 5068 _reflns_number_gt 4501 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker, 2007)' _computing_cell_refinement 'APEX2 Software Suite (Bruker, 2007)' _computing_data_reduction 'APEX2 Software Suite (Bruker, 2007)' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL and publCIF (Westrip, 2010)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0443P)^2^+2.7335P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5068 _refine_ls_number_parameters 425 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.0376 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0874 _refine_ls_wR_factor_gt 0.0842 _refine_ls_goodness_of_fit_ref 1.057 _refine_ls_restrained_S_all 1.214 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ag1 Ag 0.39015(2) 0.81066(2) 0.080634(11) 0.04453(11) Uani 1 1 d . . . N1 N 0.1599(2) 0.71678(18) -0.00672(11) 0.0284(5) Uani 1 1 d . . . N2 N 0.2347(2) 0.6828(2) 0.04648(12) 0.0345(5) Uani 1 1 d . . . N3 N 0.24936(19) 0.86959(18) -0.05776(11) 0.0284(5) Uani 1 1 d . . . N4 N 0.3582(2) 0.88772(19) -0.02320(11) 0.0320(5) Uani 1 1 d . . . N5 N 0.4961(2) 0.80466(18) 0.23279(11) 0.0304(5) Uani 1 1 d . . . N6 N 0.3988(2) 0.8384(2) 0.19248(11) 0.0351(5) Uani 1 1 d . . . N7 N 0.6489(2) 0.7703(2) 0.16090(11) 0.0325(5) Uani 1 1 d . . . N8 N 0.5989(2) 0.7833(2) 0.09699(12) 0.0359(5) Uani 1 1 d . . . C1 C 0.2350(3) 0.5748(2) 0.04484(14) 0.0347(6) Uani 1 1 d . . . H1 H 0.2784 0.5296 0.0768 0.042 Uiso 1 1 calc R . . C2 C 0.1623(2) 0.5341(2) -0.01082(13) 0.0294(6) Uani 1 1 d . . . C3 C 0.1322(3) 0.4294(2) -0.03696(15) 0.0362(6) Uani 1 1 d . . . H3 H 0.1616 0.3644 -0.0153 0.043 Uiso 1 1 calc R . . C4 C 0.0591(3) 0.4248(2) -0.09472(15) 0.0396(7) Uani 1 1 d . . . H4 H 0.0390 0.3553 -0.1139 0.048 Uiso 1 1 calc R . . C5 C 0.0131(3) 0.5210(3) -0.12627(15) 0.0393(7) Uani 1 1 d . . . H5 H -0.0379 0.5144 -0.1661 0.047 Uiso 1 1 calc R . . C6 C 0.0395(2) 0.6242(2) -0.10128(14) 0.0322(6) Uani 1 1 d . . . H6 H 0.0072 0.6887 -0.1224 0.039 Uiso 1 1 calc R . . C7 C 0.1162(2) 0.6288(2) -0.04328(13) 0.0262(5) Uani 1 1 d . . . C8 C 0.4314(2) 0.9132(2) -0.06694(14) 0.0320(6) Uani 1 1 d . . . H8 H 0.5131 0.9301 -0.0564 0.038 Uiso 1 1 calc R . . C9 C 0.3726(2) 0.9122(2) -0.13179(13) 0.0285(6) Uani 1 1 d . . . C10 C 0.4064(3) 0.9335(2) -0.19507(14) 0.0355(6) Uani 1 1 d . . . H10 H 0.4850 0.9557 -0.2010 0.043 Uiso 1 1 calc R . . C11 C 0.3221(3) 0.9212(3) -0.24763(15) 0.0418(7) Uani 1 1 d . . . H11 H 0.3428 0.9347 -0.2909 0.050 Uiso 1 1 calc R . . C12 C 0.2061(3) 0.8891(3) -0.23898(15) 0.0420(7) Uani 1 1 d . . . H12 H 0.1507 0.8799 -0.2768 0.050 Uiso 1 1 calc R . . C13 C 0.1690(3) 0.8703(2) -0.17778(14) 0.0352(6) Uani 1 1 d . . . H13 H 0.0895 0.8506 -0.1724 0.042 Uiso 1 1 calc R . . C14 C 0.2555(2) 0.8821(2) -0.12386(13) 0.0271(5) Uani 1 1 d . . . C15 C 0.1519(2) 0.8324(2) -0.02291(14) 0.0308(6) Uani 1 1 d . . . H15A H 0.0762 0.8463 -0.0505 0.037 Uiso 1 1 calc R . . H15B H 0.1509 0.8754 0.0182 0.037 Uiso 1 1 calc R . . C16 C 0.3328(3) 0.8973(3) 0.22900(14) 0.0372(7) Uani 1 1 d . . . H16 H 0.2600 0.9315 0.2131 0.045 Uiso 1 1 calc R . . C17 C 0.3852(2) 0.9027(2) 0.29525(14) 0.0333(6) Uani 1 1 d . . . C18 C 0.3546(3) 0.9506(3) 0.35412(16) 0.0450(8) Uani 1 1 d . . . H18 H 0.2841 0.9927 0.3548 0.054 Uiso 1 1 calc R . . C19 C 0.4297(3) 0.9343(3) 0.41026(16) 0.0507(9) Uani 1 1 d . . . H19 H 0.4109 0.9659 0.4505 0.061 Uiso 1 1 calc R . . C20 C 0.5335(3) 0.8724(3) 0.40982(15) 0.0462(8) Uani 1 1 d . . . H20 H 0.5824 0.8622 0.4501 0.055 Uiso 1 1 calc R . . C21 C 0.5674(3) 0.8256(3) 0.35329(14) 0.0382(7) Uani 1 1 d . . . H21 H 0.6390 0.7849 0.3532 0.046 Uiso 1 1 calc R . . C22 C 0.4899(2) 0.8415(2) 0.29582(13) 0.0299(6) Uani 1 1 d . . . C23 C 0.6830(3) 0.8237(2) 0.06396(14) 0.0332(6) Uani 1 1 d . . . H23 H 0.6727 0.8413 0.0184 0.040 Uiso 1 1 calc R . . C24 C 0.7906(2) 0.8374(2) 0.10493(13) 0.0281(5) Uani 1 1 d . . . C25 C 0.9054(3) 0.8742(2) 0.09584(14) 0.0337(6) Uani 1 1 d . . . H25 H 0.9238 0.8996 0.0541 0.040 Uiso 1 1 calc R . . C26 C 0.9899(3) 0.8724(2) 0.14894(15) 0.0385(7) Uani 1 1 d . . . H26 H 1.0682 0.8966 0.1438 0.046 Uiso 1 1 calc R . . C27 C 0.9629(3) 0.8353(3) 0.21093(15) 0.0391(7) Uani 1 1 d . . . H27 H 1.0240 0.8342 0.2465 0.047 Uiso 1 1 calc R . . C28 C 0.8514(3) 0.8008(2) 0.22189(14) 0.0355(6) Uani 1 1 d . . . H28 H 0.8336 0.7772 0.2642 0.043 Uiso 1 1 calc R . . C29 C 0.7652(2) 0.8020(2) 0.16757(13) 0.0282(6) Uani 1 1 d . . . C30 C 0.5772(3) 0.7256(2) 0.20894(14) 0.0344(6) Uani 1 1 d . . . H30A H 0.6302 0.6973 0.2468 0.041 Uiso 1 1 calc R . . H30B H 0.5308 0.6629 0.1890 0.041 Uiso 1 1 calc R . . F1A F 0.7011(2) 0.5634(3) 0.40332(18) 0.0806(11) Uani 0.761(4) 1 d PDU A 1 F3A F 0.8311(4) 0.6236(3) 0.33585(12) 0.0798(11) Uani 0.761(4) 1 d PDU A 1 F2A F 0.8925(3) 0.5514(2) 0.43436(14) 0.0656(9) Uani 0.761(4) 1 d PDU A 1 F4A F 0.8023(2) 0.71548(15) 0.42885(11) 0.0631(6) Uani 0.761(4) 1 d PDU A 1 F1B F 0.7953(11) 0.5289(4) 0.4325(5) 0.082(3) Uani 0.239(4) 1 d PDU A 2 F2B F 0.9167(6) 0.6187(7) 0.3713(5) 0.077(3) Uani 0.239(4) 1 d PDU A 2 F3B F 0.7239(7) 0.6188(7) 0.3418(4) 0.071(3) Uani 0.239(4) 1 d PDU A 2 F4B F 0.8023(2) 0.71548(15) 0.42885(11) 0.0631(6) Uani 0.239(4) 1 d PDU A 2 B1 B 0.8071(2) 0.6163(2) 0.39772(13) 0.0333(7) Uani 1 1 d 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 0.04074(16) 0.0648(2) 0.02632(14) -0.00446(10) -0.00506(10) -0.01019(11) N1 0.0313(12) 0.0269(12) 0.0265(11) -0.0009(9) 0.0002(9) -0.0020(9) N2 0.0346(13) 0.0420(15) 0.0261(12) 0.0001(10) -0.0011(10) -0.0030(10) N3 0.0301(11) 0.0277(12) 0.0270(11) -0.0035(9) 0.0011(9) -0.0027(9) N4 0.0332(12) 0.0335(13) 0.0288(12) -0.0067(10) 0.0006(9) -0.0061(10) N5 0.0351(12) 0.0319(12) 0.0243(11) 0.0027(9) 0.0038(9) -0.0012(9) N6 0.0355(13) 0.0430(14) 0.0266(12) 0.0023(10) 0.0021(10) -0.0049(11) N7 0.0377(13) 0.0357(13) 0.0242(11) 0.0020(10) 0.0041(9) -0.0019(10) N8 0.0351(13) 0.0463(15) 0.0259(12) -0.0022(10) 0.0013(10) 0.0010(11) C1 0.0357(15) 0.0398(17) 0.0282(14) 0.0067(12) 0.0005(11) 0.0014(12) C2 0.0309(13) 0.0303(14) 0.0276(13) 0.0025(11) 0.0065(11) 0.0003(11) C3 0.0445(16) 0.0266(14) 0.0388(16) 0.0034(12) 0.0105(13) 0.0021(12) C4 0.0516(18) 0.0283(15) 0.0397(16) -0.0054(12) 0.0081(13) -0.0095(13) C5 0.0472(17) 0.0377(16) 0.0316(15) -0.0017(13) -0.0027(13) -0.0116(13) C6 0.0358(14) 0.0303(15) 0.0294(14) 0.0037(11) -0.0017(11) -0.0041(11) C7 0.0277(13) 0.0252(13) 0.0266(13) -0.0008(10) 0.0069(10) -0.0022(10) C8 0.0303(14) 0.0325(15) 0.0326(14) -0.0046(11) 0.0005(11) -0.0034(11) C9 0.0341(14) 0.0205(12) 0.0310(14) -0.0025(10) 0.0041(11) 0.0035(10) C10 0.0451(16) 0.0272(14) 0.0356(15) 0.0011(12) 0.0106(13) 0.0060(12) C11 0.060(2) 0.0361(16) 0.0295(15) 0.0054(12) 0.0067(13) 0.0106(14) C12 0.0561(19) 0.0342(16) 0.0323(15) 0.0048(12) -0.0115(13) 0.0066(14) C13 0.0393(15) 0.0274(14) 0.0366(15) 0.0040(12) -0.0070(12) 0.0010(12) C14 0.0346(14) 0.0174(12) 0.0289(13) -0.0025(10) 0.0019(11) 0.0036(10) C15 0.0321(14) 0.0270(14) 0.0340(14) -0.0052(11) 0.0062(11) 0.0006(11) C16 0.0311(14) 0.0456(17) 0.0348(15) 0.0032(13) 0.0031(12) -0.0025(12) C17 0.0331(14) 0.0370(15) 0.0307(14) 0.0009(12) 0.0077(11) -0.0087(12) C18 0.0414(17) 0.055(2) 0.0407(17) -0.0081(15) 0.0137(14) -0.0056(14) C19 0.053(2) 0.069(2) 0.0322(16) -0.0125(16) 0.0124(14) -0.0149(17) C20 0.0492(19) 0.060(2) 0.0283(15) 0.0005(14) 0.0000(13) -0.0151(16) C21 0.0406(16) 0.0422(17) 0.0313(15) 0.0055(12) 0.0003(12) -0.0075(13) C22 0.0337(14) 0.0297(14) 0.0268(13) 0.0031(11) 0.0061(11) -0.0079(11) C23 0.0369(15) 0.0396(16) 0.0233(13) 0.0011(11) 0.0049(11) 0.0045(12) C24 0.0352(14) 0.0229(13) 0.0261(13) -0.0005(10) 0.0029(11) 0.0040(11) C25 0.0385(15) 0.0286(14) 0.0349(15) 0.0035(12) 0.0076(12) 0.0007(12) C26 0.0365(15) 0.0342(16) 0.0443(17) -0.0032(13) 0.0018(13) -0.0027(12) C27 0.0411(17) 0.0388(16) 0.0351(16) -0.0055(13) -0.0073(13) 0.0012(13) C28 0.0461(17) 0.0358(16) 0.0240(14) 0.0009(11) 0.0009(12) 0.0040(12) C29 0.0355(15) 0.0221(13) 0.0271(13) -0.0011(10) 0.0039(11) 0.0039(10) C30 0.0427(16) 0.0290(14) 0.0328(15) 0.0034(12) 0.0098(12) -0.0015(12) F1A 0.0543(17) 0.092(2) 0.099(2) -0.0279(19) 0.0234(16) -0.0333(16) F3A 0.134(3) 0.0699(19) 0.0403(15) 0.0172(14) 0.0333(17) 0.005(2) F2A 0.0716(19) 0.0587(17) 0.0628(17) -0.0008(13) -0.0113(14) 0.0249(14) F4A 0.0830(15) 0.0433(11) 0.0610(13) -0.0115(10) -0.0013(11) 0.0056(10) F1B 0.093(5) 0.073(4) 0.081(4) 0.021(4) 0.011(4) 0.000(4) F2B 0.066(4) 0.077(4) 0.090(5) -0.016(4) 0.020(4) -0.002(4) F3B 0.075(4) 0.056(4) 0.075(4) -0.020(3) -0.021(4) 0.009(3) F4B 0.0830(15) 0.0433(11) 0.0610(13) -0.0115(10) -0.0013(11) 0.0056(10) B1 0.0308(16) 0.0310(16) 0.0383(17) 0.0006(14) 0.0039(13) -0.0008(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N6 2.299(2) . ? Ag1 N4 2.311(2) . ? Ag1 N8 2.376(2) . ? Ag1 N2 2.398(2) . ? N1 C7 1.368(3) . ? N1 N2 1.370(3) . ? N1 C15 1.446(3) . ? N2 C1 1.316(4) . ? N3 C14 1.366(3) . ? N3 N4 1.373(3) . ? N3 C15 1.446(3) . ? N4 C8 1.316(4) . ? N5 N6 1.368(3) . ? N5 C22 1.370(4) . ? N5 C30 1.448(4) . ? N6 C16 1.320(4) . ? N7 C29 1.366(4) . ? N7 N8 1.376(3) . ? N7 C30 1.442(4) . ? N8 C23 1.318(4) . ? C1 C2 1.421(4) . ? C1 H1 0.9500 . ? C2 C7 1.402(4) . ? C2 C3 1.410(4) . ? C3 C4 1.369(4) . ? C3 H3 0.9500 . ? C4 C5 1.410(4) . ? C4 H4 0.9500 . ? C5 C6 1.377(4) . ? C5 H5 0.9500 . ? C6 C7 1.395(4) . ? C6 H6 0.9500 . ? C8 C9 1.418(4) . ? C8 H8 0.9500 . ? C9 C14 1.400(4) . ? C9 C10 1.408(4) . ? C10 C11 1.368(4) . ? C10 H10 0.9500 . ? C11 C12 1.399(5) . ? C11 H11 0.9500 . ? C12 C13 1.376(4) . ? C12 H12 0.9500 . ? C13 C14 1.403(4) . ? C13 H13 0.9500 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C16 C17 1.421(4) . ? C16 H16 0.9500 . ? C17 C22 1.399(4) . ? C17 C18 1.410(4) . ? C18 C19 1.369(5) . ? C18 H18 0.9500 . ? C19 C20 1.397(5) . ? C19 H19 0.9500 . ? C20 C21 1.376(5) . ? C20 H20 0.9500 . ? C21 C22 1.403(4) . ? C21 H21 0.9500 . ? C23 C24 1.414(4) . ? C23 H23 0.9500 . ? C24 C25 1.405(4) . ? C24 C29 1.406(4) . ? C25 C26 1.370(4) . ? C25 H25 0.9500 . ? C26 C27 1.406(4) . ? C26 H26 0.9500 . ? C27 C28 1.371(5) . ? C27 H27 0.9500 . ? C28 C29 1.399(4) . ? C28 H28 0.9500 . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? F1A B1 1.377(3) . ? F3A B1 1.321(3) . ? F2A B1 1.404(3) . ? F4A B1 1.368(3) . ? F1B B1 1.294(4) . ? F2B B1 1.403(4) . ? F3B B1 1.403(5) . ? 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 N6 Ag1 N4 146.81(9) . . ? N6 Ag1 N8 86.65(8) . . ? N4 Ag1 N8 104.18(8) . . ? N6 Ag1 N2 109.77(8) . . ? N4 Ag1 N2 87.50(8) . . ? N8 Ag1 N2 129.75(9) . . ? C7 N1 N2 110.8(2) . . ? C7 N1 C15 128.8(2) . . ? N2 N1 C15 119.6(2) . . ? C1 N2 N1 106.5(2) . . ? C1 N2 Ag1 130.7(2) . . ? N1 N2 Ag1 114.19(16) . . ? C14 N3 N4 110.7(2) . . ? C14 N3 C15 129.8(2) . . ? N4 N3 C15 119.2(2) . . ? C8 N4 N3 106.5(2) . . ? C8 N4 Ag1 131.85(19) . . ? N3 N4 Ag1 116.91(16) . . ? N6 N5 C22 110.5(2) . . ? N6 N5 C30 119.8(2) . . ? C22 N5 C30 128.9(2) . . ? C16 N6 N5 107.0(2) . . ? C16 N6 Ag1 132.2(2) . . ? N5 N6 Ag1 120.10(17) . . ? C29 N7 N8 111.1(2) . . ? C29 N7 C30 130.1(2) . . ? N8 N7 C30 118.8(2) . . ? C23 N8 N7 106.2(2) . . ? C23 N8 Ag1 129.6(2) . . ? N7 N8 Ag1 117.10(17) . . ? N2 C1 C2 111.4(3) . . ? N2 C1 H1 124.3 . . ? C2 C1 H1 124.3 . . ? C7 C2 C3 120.0(3) . . ? C7 C2 C1 104.4(2) . . ? C3 C2 C1 135.6(3) . . ? C4 C3 C2 117.6(3) . . ? C4 C3 H3 121.2 . . ? C2 C3 H3 121.2 . . ? C3 C4 C5 121.4(3) . . ? C3 C4 H4 119.3 . . ? C5 C4 H4 119.3 . . ? C6 C5 C4 122.2(3) . . ? C6 C5 H5 118.9 . . ? C4 C5 H5 118.9 . . ? C5 C6 C7 116.3(3) . . ? C5 C6 H6 121.9 . . ? C7 C6 H6 121.9 . . ? N1 C7 C6 130.7(2) . . ? N1 C7 C2 106.9(2) . . ? C6 C7 C2 122.5(2) . . ? N4 C8 C9 111.2(2) . . ? N4 C8 H8 124.4 . . ? C9 C8 H8 124.4 . . ? C14 C9 C10 120.3(3) . . ? C14 C9 C8 104.7(2) . . ? C10 C9 C8 135.0(3) . . ? C11 C10 C9 117.7(3) . . ? C11 C10 H10 121.1 . . ? C9 C10 H10 121.1 . . ? C10 C11 C12 121.3(3) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C13 C12 C11 122.6(3) . . ? C13 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? C12 C13 C14 116.2(3) . . ? C12 C13 H13 121.9 . . ? C14 C13 H13 121.9 . . ? N3 C14 C9 106.8(2) . . ? N3 C14 C13 131.3(3) . . ? C9 C14 C13 121.9(3) . . ? N3 C15 N1 112.6(2) . . ? N3 C15 H15A 109.1 . . ? N1 C15 H15A 109.1 . . ? N3 C15 H15B 109.1 . . ? N1 C15 H15B 109.1 . . ? H15A C15 H15B 107.8 . . ? N6 C16 C17 110.9(3) . . ? N6 C16 H16 124.6 . . ? C17 C16 H16 124.6 . . ? C22 C17 C18 119.7(3) . . ? C22 C17 C16 104.7(2) . . ? C18 C17 C16 135.5(3) . . ? C19 C18 C17 117.8(3) . . ? C19 C18 H18 121.1 . . ? C17 C18 H18 121.1 . . ? C18 C19 C20 121.5(3) . . ? C18 C19 H19 119.2 . . ? C20 C19 H19 119.2 . . ? C21 C20 C19 122.5(3) . . ? C21 C20 H20 118.8 . . ? C19 C20 H20 118.8 . . ? C20 C21 C22 116.0(3) . . ? C20 C21 H21 122.0 . . ? C22 C21 H21 122.0 . . ? N5 C22 C17 107.0(2) . . ? N5 C22 C21 130.6(3) . . ? C17 C22 C21 122.5(3) . . ? N8 C23 C24 111.5(2) . . ? N8 C23 H23 124.3 . . ? C24 C23 H23 124.3 . . ? C25 C24 C29 119.8(3) . . ? C25 C24 C23 135.4(3) . . ? C29 C24 C23 104.8(2) . . ? C26 C25 C24 118.1(3) . . ? C26 C25 H25 121.0 . . ? C24 C25 H25 121.0 . . ? C25 C26 C27 121.1(3) . . ? C25 C26 H26 119.4 . . ? C27 C26 H26 119.4 . . ? C28 C27 C26 122.4(3) . . ? C28 C27 H27 118.8 . . ? C26 C27 H27 118.8 . . ? C27 C28 C29 116.5(3) . . ? C27 C28 H28 121.7 . . ? C29 C28 H28 121.7 . . ? N7 C29 C28 131.5(3) . . ? N7 C29 C24 106.4(2) . . ? C28 C29 C24 122.1(3) . . ? N7 C30 N5 113.5(2) . . ? N7 C30 H30A 108.9 . . ? N5 C30 H30A 108.9 . . ? N7 C30 H30B 108.9 . . ? N5 C30 H30B 108.9 . . ? H30A C30 H30B 107.7 . . ? F1B B1 F3A 128.5(5) . . ? F1B B1 F4A 117.4(4) . . ? F3A B1 F4A 114.0(2) . . ? F1B B1 F1A 55.2(5) . . ? F3A B1 F1A 112.2(3) . . ? F4A B1 F1A 107.3(2) . . ? F1B B1 F2B 111.9(5) . . ? F3A B1 F2B 49.8(4) . . ? F4A B1 F2B 103.9(3) . . ? F1A B1 F2B 148.7(4) . . ? F1B B1 F3B 111.4(7) . . ? F3A B1 F3B 53.8(4) . . ? F4A B1 F3B 107.7(3) . . ? F1A B1 F3B 63.9(5) . . ? F2B B1 F3B 103.5(4) . . ? F1B B1 F2A 49.4(5) . . ? F3A B1 F2A 110.4(3) . . ? F4A B1 F2A 108.0(2) . . ? F1A B1 F2A 104.5(3) . . ? F2B B1 F2A 68.2(4) . . ? F3B B1 F2A 144.4(4) . . ? 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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 N1 N2 C1 -2.1(3) . . . . ? C15 N1 N2 C1 -172.5(2) . . . . ? C7 N1 N2 Ag1 149.38(17) . . . . ? C15 N1 N2 Ag1 -21.0(3) . . . . ? N6 Ag1 N2 C1 -86.1(3) . . . . ? N4 Ag1 N2 C1 122.9(3) . . . . ? N8 Ag1 N2 C1 16.5(3) . . . . ? N6 Ag1 N2 N1 130.98(18) . . . . ? N4 Ag1 N2 N1 -20.00(18) . . . . ? N8 Ag1 N2 N1 -126.41(18) . . . . ? C14 N3 N4 C8 1.1(3) . . . . ? C15 N3 N4 C8 175.8(2) . . . . ? C14 N3 N4 Ag1 -157.55(17) . . . . ? C15 N3 N4 Ag1 17.1(3) . . . . ? N6 Ag1 N4 C8 106.3(3) . . . . ? N8 Ag1 N4 C8 0.3(3) . . . . ? N2 Ag1 N4 C8 -130.2(3) . . . . ? N6 Ag1 N4 N3 -101.6(2) . . . . ? N8 Ag1 N4 N3 152.36(18) . . . . ? N2 Ag1 N4 N3 21.88(18) . . . . ? C22 N5 N6 C16 1.0(3) . . . . ? C30 N5 N6 C16 171.5(2) . . . . ? C22 N5 N6 Ag1 172.20(17) . . . . ? C30 N5 N6 Ag1 -17.4(3) . . . . ? N4 Ag1 N6 C16 40.3(3) . . . . ? N8 Ag1 N6 C16 151.3(3) . . . . ? N2 Ag1 N6 C16 -77.4(3) . . . . ? N4 Ag1 N6 N5 -128.2(2) . . . . ? N8 Ag1 N6 N5 -17.2(2) . . . . ? N2 Ag1 N6 N5 114.05(19) . . . . ? C29 N7 N8 C23 -0.4(3) . . . . ? C30 N7 N8 C23 -179.3(3) . . . . ? C29 N7 N8 Ag1 -153.79(18) . . . . ? C30 N7 N8 Ag1 27.3(3) . . . . ? N6 Ag1 N8 C23 -133.7(3) . . . . ? N4 Ag1 N8 C23 14.5(3) . . . . ? N2 Ag1 N8 C23 113.2(3) . . . . ? N6 Ag1 N8 N7 12.4(2) . . . . ? N4 Ag1 N8 N7 160.57(19) . . . . ? N2 Ag1 N8 N7 -100.7(2) . . . . ? N1 N2 C1 C2 1.5(3) . . . . ? Ag1 N2 C1 C2 -143.5(2) . . . . ? N2 C1 C2 C7 -0.3(3) . . . . ? N2 C1 C2 C3 178.8(3) . . . . ? C7 C2 C3 C4 1.0(4) . . . . ? C1 C2 C3 C4 -178.1(3) . . . . ? C2 C3 C4 C5 -1.5(4) . . . . ? C3 C4 C5 C6 0.5(5) . . . . ? C4 C5 C6 C7 1.0(4) . . . . ? N2 N1 C7 C6 -179.0(3) . . . . ? C15 N1 C7 C6 -9.7(4) . . . . ? N2 N1 C7 C2 1.9(3) . . . . ? C15 N1 C7 C2 171.2(3) . . . . ? C5 C6 C7 N1 179.5(3) . . . . ? C5 C6 C7 C2 -1.5(4) . . . . ? C3 C2 C7 N1 179.7(2) . . . . ? C1 C2 C7 N1 -1.0(3) . . . . ? C3 C2 C7 C6 0.6(4) . . . . ? C1 C2 C7 C6 179.9(2) . . . . ? N3 N4 C8 C9 -0.2(3) . . . . ? Ag1 N4 C8 C9 153.94(19) . . . . ? N4 C8 C9 C14 -0.7(3) . . . . ? N4 C8 C9 C10 179.2(3) . . . . ? C14 C9 C10 C11 -1.5(4) . . . . ? C8 C9 C10 C11 178.6(3) . . . . ? C9 C10 C11 C12 0.4(4) . . . . ? C10 C11 C12 C13 1.4(5) . . . . ? C11 C12 C13 C14 -1.8(4) . . . . ? N4 N3 C14 C9 -1.5(3) . . . . ? C15 N3 C14 C9 -175.5(2) . . . . ? N4 N3 C14 C13 178.8(3) . . . . ? C15 N3 C14 C13 4.9(5) . . . . ? C10 C9 C14 N3 -178.6(2) . . . . ? C8 C9 C14 N3 1.3(3) . . . . ? C10 C9 C14 C13 1.1(4) . . . . ? C8 C9 C14 C13 -179.0(2) . . . . ? C12 C13 C14 N3 -179.8(3) . . . . ? C12 C13 C14 C9 0.6(4) . . . . ? C14 N3 C15 N1 96.4(3) . . . . ? N4 N3 C15 N1 -77.1(3) . . . . ? C7 N1 C15 N3 -89.0(3) . . . . ? N2 N1 C15 N3 79.5(3) . . . . ? N5 N6 C16 C17 -0.7(3) . . . . ? Ag1 N6 C16 C17 -170.34(19) . . . . ? N6 C16 C17 C22 0.1(3) . . . . ? N6 C16 C17 C18 -178.6(3) . . . . ? C22 C17 C18 C19 -0.3(5) . . . . ? C16 C17 C18 C19 178.2(3) . . . . ? C17 C18 C19 C20 -0.1(5) . . . . ? C18 C19 C20 C21 1.0(5) . . . . ? C19 C20 C21 C22 -1.4(5) . . . . ? N6 N5 C22 C17 -1.0(3) . . . . ? C30 N5 C22 C17 -170.3(3) . . . . ? N6 N5 C22 C21 178.6(3) . . . . ? C30 N5 C22 C21 9.3(5) . . . . ? C18 C17 C22 N5 179.5(3) . . . . ? C16 C17 C22 N5 0.5(3) . . . . ? C18 C17 C22 C21 -0.2(4) . . . . ? C16 C17 C22 C21 -179.1(3) . . . . ? C20 C21 C22 N5 -178.5(3) . . . . ? C20 C21 C22 C17 1.0(4) . . . . ? N7 N8 C23 C24 0.5(3) . . . . ? Ag1 N8 C23 C24 149.3(2) . . . . ? N8 C23 C24 C25 178.8(3) . . . . ? N8 C23 C24 C29 -0.4(3) . . . . ? C29 C24 C25 C26 1.1(4) . . . . ? C23 C24 C25 C26 -177.9(3) . . . . ? C24 C25 C26 C27 -0.3(4) . . . . ? C25 C26 C27 C28 -0.9(5) . . . . ? C26 C27 C28 C29 1.2(4) . . . . ? N8 N7 C29 C28 -178.0(3) . . . . ? C30 N7 C29 C28 0.7(5) . . . . ? N8 N7 C29 C24 0.2(3) . . . . ? C30 N7 C29 C24 178.9(3) . . . . ? C27 C28 C29 N7 177.6(3) . . . . ? C27 C28 C29 C24 -0.4(4) . . . . ? C25 C24 C29 N7 -179.2(2) . . . . ? C23 C24 C29 N7 0.1(3) . . . . ? C25 C24 C29 C28 -0.8(4) . . . . ? C23 C24 C29 C28 178.5(2) . . . . ? C29 N7 C30 N5 103.1(3) . . . . ? N8 N7 C30 N5 -78.2(3) . . . . ? N6 N5 C30 N7 72.1(3) . . . . ? C22 N5 C30 N7 -119.4(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.661 _refine_diff_density_min -0.746 _refine_diff_density_rms 0.061 data_23 _database_code_depnum_ccdc_archive 'CCDC 917679' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H12 Au Cl2 N4, Au Cl4' _chemical_formula_sum 'C15 H12 Au2 Cl6 N4' _chemical_formula_weight 854.92 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' Cl Cl 0.1484 0.1585 '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' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5418(6) _cell_length_b 10.6453(7) _cell_length_c 10.6524(6) _cell_angle_alpha 67.967(1) _cell_angle_beta 71.490(2) _cell_angle_gamma 78.281(2) _cell_volume 1045.98(11) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8488 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 30.57 _exptl_crystal_description plate _exptl_crystal_colour gold _exptl_crystal_size_max 0.08 _exptl_crystal_size_mid 0.06 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.714 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 780 _exptl_absorpt_coefficient_mu 14.785 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3842 _exptl_absorpt_correction_T_max 0.5252 _exptl_absorpt_process_details ; APEX2 Software Suite; Bruker 2005. ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker-Nonius X8kappa APEX II CCD area detector ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 23614 _diffrn_reflns_av_R_equivalents 0.0321 _diffrn_reflns_av_sigmaI/netI 0.0335 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.05 _diffrn_reflns_theta_max 30.59 _reflns_number_total 6273 _reflns_number_gt 5233 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker, 2005)' _computing_cell_refinement 'APEX2 Software Suite' _computing_data_reduction 'APEX2 Software Suite' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997a)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 1997b)' _computing_publication_material SHELXTL _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0189P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6273 _refine_ls_number_parameters 244 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0319 _refine_ls_R_factor_gt 0.0221 _refine_ls_wR_factor_ref 0.0447 _refine_ls_wR_factor_gt 0.0418 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.185920(12) 0.638789(13) 0.398089(12) 0.01805(4) Uani 1 1 d . . . Cl1 Cl -0.01467(9) 0.65826(11) 0.55201(9) 0.0329(2) Uani 1 1 d . . . Cl2 Cl 0.28387(9) 0.54173(9) 0.57557(9) 0.02721(19) Uani 1 1 d . . . N1 N 0.1687(3) 0.8057(3) 0.1094(3) 0.0191(6) Uani 1 1 d . . . N2 N 0.0982(3) 0.7248(3) 0.2369(3) 0.0201(6) Uani 1 1 d . . . N3 N 0.3885(3) 0.7096(3) 0.1232(3) 0.0167(6) Uani 1 1 d . . . N4 N 0.3648(3) 0.6189(3) 0.2574(3) 0.0166(6) Uani 1 1 d . . . C1 C -0.0149(3) 0.7029(3) 0.2218(4) 0.0207(7) Uani 1 1 d . . . H1 H -0.0817 0.6494 0.2942 0.025 Uiso 1 1 calc R . . C2 C -0.0202(3) 0.7709(3) 0.0825(4) 0.0202(7) Uani 1 1 d . . . C3 C -0.1130(4) 0.7836(4) 0.0065(4) 0.0259(8) Uani 1 1 d . . . H3 H -0.1941 0.7407 0.0509 0.031 Uiso 1 1 calc R . . C4 C -0.0822(4) 0.8596(4) -0.1327(4) 0.0320(9) Uani 1 1 d . . . H4 H -0.1423 0.8683 -0.1863 0.038 Uiso 1 1 calc R . . C5 C 0.0371(4) 0.9259(4) -0.1991(4) 0.0279(8) Uani 1 1 d . . . H5 H 0.0542 0.9785 -0.2961 0.034 Uiso 1 1 calc R . . C6 C 0.1287(3) 0.9172(3) -0.1291(3) 0.0212(7) Uani 1 1 d . . . H6 H 0.2079 0.9633 -0.1740 0.025 Uiso 1 1 calc R . . C7 C 0.0989(3) 0.8364(3) 0.0126(3) 0.0172(6) Uani 1 1 d . . . C8 C 0.4638(3) 0.5198(3) 0.2635(3) 0.0209(7) Uani 1 1 d . . . H8 H 0.4697 0.4427 0.3443 0.025 Uiso 1 1 calc R . . C9 C 0.5589(3) 0.5463(3) 0.1318(3) 0.0191(7) Uani 1 1 d . . . C10 C 0.6832(4) 0.4805(4) 0.0764(4) 0.0256(8) Uani 1 1 d . . . H10 H 0.7204 0.3982 0.1334 0.031 Uiso 1 1 calc R . . C11 C 0.7476(4) 0.5390(4) -0.0612(4) 0.0273(8) Uani 1 1 d . . . H11 H 0.8304 0.4956 -0.1008 0.033 Uiso 1 1 calc R . . C12 C 0.6948(4) 0.6621(4) -0.1463(4) 0.0262(8) Uani 1 1 d . . . H12 H 0.7432 0.6989 -0.2419 0.031 Uiso 1 1 calc R . . C13 C 0.5758(3) 0.7312(4) -0.0963(3) 0.0227(7) Uani 1 1 d . . . H13 H 0.5415 0.8152 -0.1536 0.027 Uiso 1 1 calc R . . C14 C 0.5087(3) 0.6694(3) 0.0447(3) 0.0183(7) Uani 1 1 d . . . C15 C 0.3021(3) 0.8349(3) 0.0942(3) 0.0191(7) Uani 1 1 d . . . H15A H 0.3390 0.8958 -0.0026 0.023 Uiso 1 1 calc R . . H15B H 0.2977 0.8819 0.1602 0.023 Uiso 1 1 calc R . . Au2 Au 0.518968(13) 0.137832(12) 0.581012(13) 0.01839(4) Uani 1 1 d . . . Cl3 Cl 0.30841(9) 0.20582(10) 0.55138(10) 0.0315(2) Uani 1 1 d . . . Cl4 Cl 0.59835(10) 0.17053(9) 0.34834(9) 0.0287(2) Uani 1 1 d . . . Cl5 Cl 0.73222(9) 0.06741(10) 0.60698(10) 0.02929(19) Uani 1 1 d . . . Cl6 Cl 0.43713(10) 0.11235(10) 0.81406(9) 0.0302(2) 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 Au1 0.01678(6) 0.02118(7) 0.01370(6) -0.00372(5) -0.00218(5) -0.00360(5) Cl1 0.0218(4) 0.0477(6) 0.0205(4) -0.0095(4) 0.0032(4) -0.0023(4) Cl2 0.0305(5) 0.0310(5) 0.0197(4) -0.0039(3) -0.0106(4) -0.0047(4) N1 0.0142(13) 0.0261(15) 0.0140(13) -0.0026(11) -0.0040(11) -0.0032(11) N2 0.0150(13) 0.0239(15) 0.0156(13) -0.0026(11) -0.0004(11) -0.0031(11) N3 0.0148(13) 0.0190(14) 0.0126(12) -0.0023(10) -0.0024(11) -0.0014(11) N4 0.0156(13) 0.0198(14) 0.0115(12) -0.0018(10) -0.0030(10) -0.0028(11) C1 0.0139(15) 0.0230(17) 0.0232(17) -0.0068(14) -0.0040(13) -0.0009(13) C2 0.0156(16) 0.0219(17) 0.0218(17) -0.0059(13) -0.0047(13) -0.0019(13) C3 0.0218(18) 0.0260(19) 0.033(2) -0.0097(16) -0.0103(16) -0.0033(15) C4 0.036(2) 0.035(2) 0.034(2) -0.0109(17) -0.0210(18) -0.0022(17) C5 0.034(2) 0.0255(19) 0.0233(18) -0.0052(15) -0.0121(16) 0.0008(16) C6 0.0197(17) 0.0238(17) 0.0185(16) -0.0071(13) -0.0043(14) 0.0001(14) C7 0.0166(15) 0.0180(15) 0.0173(15) -0.0060(12) -0.0064(13) 0.0008(12) C8 0.0192(17) 0.0185(16) 0.0204(17) -0.0017(13) -0.0043(14) -0.0029(13) C9 0.0185(16) 0.0182(16) 0.0203(16) -0.0065(13) -0.0044(13) -0.0025(13) C10 0.0255(18) 0.0199(17) 0.032(2) -0.0115(15) -0.0061(16) -0.0008(14) C11 0.0196(17) 0.030(2) 0.034(2) -0.0187(16) -0.0008(16) -0.0020(15) C12 0.0215(18) 0.036(2) 0.0227(18) -0.0139(15) 0.0003(15) -0.0075(16) C13 0.0198(17) 0.0299(19) 0.0196(17) -0.0078(14) -0.0057(14) -0.0051(14) C14 0.0175(16) 0.0205(16) 0.0195(16) -0.0074(13) -0.0070(13) -0.0025(13) C15 0.0151(16) 0.0182(16) 0.0204(16) -0.0011(13) -0.0059(13) -0.0021(12) Au2 0.02121(7) 0.01630(6) 0.01723(6) -0.00440(5) -0.00510(5) -0.00329(5) Cl3 0.0240(4) 0.0310(5) 0.0389(5) -0.0105(4) -0.0110(4) 0.0004(4) Cl4 0.0361(5) 0.0288(5) 0.0187(4) -0.0067(3) -0.0070(4) -0.0009(4) Cl5 0.0257(4) 0.0348(5) 0.0293(5) -0.0113(4) -0.0120(4) 0.0019(4) Cl6 0.0326(5) 0.0384(5) 0.0198(4) -0.0101(4) 0.0014(4) -0.0167(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Au1 N4 2.032(3) . ? Au1 N2 2.032(3) . ? Au1 Cl2 2.2470(8) . ? Au1 Cl1 2.2535(9) . ? N1 C7 1.357(4) . ? N1 N2 1.371(4) . ? N1 C15 1.448(4) . ? N2 C1 1.328(4) . ? N3 C14 1.365(4) . ? N3 N4 1.369(3) . ? N3 C15 1.443(4) . ? N4 C8 1.323(4) . ? C1 C2 1.400(5) . ? C1 H1 0.9500 . ? C2 C7 1.411(4) . ? C2 C3 1.413(5) . ? C3 C4 1.363(5) . ? C3 H3 0.9500 . ? C4 C5 1.415(5) . ? C4 H4 0.9500 . ? C5 C6 1.366(5) . ? C5 H5 0.9500 . ? C6 C7 1.397(4) . ? C6 H6 0.9500 . ? C8 C9 1.406(5) . ? C8 H8 0.9500 . ? C9 C14 1.406(4) . ? C9 C10 1.415(5) . ? C10 C11 1.361(5) . ? C10 H10 0.9500 . ? C11 C12 1.408(5) . ? C11 H11 0.9500 . ? C12 C13 1.376(5) . ? C12 H12 0.9500 . ? C13 C14 1.401(5) . ? C13 H13 0.9500 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? Au2 Cl4 2.2624(9) . ? Au2 Cl3 2.2741(9) . ? Au2 Cl6 2.2828(9) . ? Au2 Cl5 2.2906(9) . ? 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 N4 Au1 N2 89.20(11) . . ? N4 Au1 Cl2 90.44(7) . . ? N2 Au1 Cl2 179.39(9) . . ? N4 Au1 Cl1 178.66(8) . . ? N2 Au1 Cl1 90.01(8) . . ? Cl2 Au1 Cl1 90.35(4) . . ? C7 N1 N2 109.7(3) . . ? C7 N1 C15 130.7(3) . . ? N2 N1 C15 119.3(3) . . ? C1 N2 N1 108.3(3) . . ? C1 N2 Au1 131.2(2) . . ? N1 N2 Au1 119.7(2) . . ? C14 N3 N4 109.1(3) . . ? C14 N3 C15 131.1(3) . . ? N4 N3 C15 118.9(3) . . ? C8 N4 N3 108.6(3) . . ? C8 N4 Au1 131.4(2) . . ? N3 N4 Au1 119.3(2) . . ? N2 C1 C2 109.3(3) . . ? N2 C1 H1 125.4 . . ? C2 C1 H1 125.4 . . ? C1 C2 C7 106.1(3) . . ? C1 C2 C3 134.6(3) . . ? C7 C2 C3 119.3(3) . . ? C4 C3 C2 117.7(3) . . ? C4 C3 H3 121.1 . . ? C2 C3 H3 121.1 . . ? C3 C4 C5 121.5(3) . . ? C3 C4 H4 119.2 . . ? C5 C4 H4 119.2 . . ? C6 C5 C4 122.5(3) . . ? C6 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? C5 C6 C7 115.9(3) . . ? C5 C6 H6 122.0 . . ? C7 C6 H6 122.0 . . ? N1 C7 C6 130.4(3) . . ? N1 C7 C2 106.6(3) . . ? C6 C7 C2 122.9(3) . . ? N4 C8 C9 109.5(3) . . ? N4 C8 H8 125.2 . . ? C9 C8 H8 125.2 . . ? C8 C9 C14 105.5(3) . . ? C8 C9 C10 135.2(3) . . ? C14 C9 C10 119.3(3) . . ? C11 C10 C9 117.8(3) . . ? C11 C10 H10 121.1 . . ? C9 C10 H10 121.1 . . ? C10 C11 C12 121.8(3) . . ? C10 C11 H11 119.1 . . ? C12 C11 H11 119.1 . . ? C13 C12 C11 122.5(3) . . ? C13 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? C12 C13 C14 115.5(3) . . ? C12 C13 H13 122.2 . . ? C14 C13 H13 122.2 . . ? N3 C14 C13 129.7(3) . . ? N3 C14 C9 107.2(3) . . ? C13 C14 C9 123.1(3) . . ? N3 C15 N1 109.6(3) . . ? N3 C15 H15A 109.8 . . ? N1 C15 H15A 109.8 . . ? N3 C15 H15B 109.8 . . ? N1 C15 H15B 109.8 . . ? H15A C15 H15B 108.2 . . ? Cl4 Au2 Cl3 88.98(4) . . ? Cl4 Au2 Cl6 178.12(3) . . ? Cl3 Au2 Cl6 90.29(4) . . ? Cl4 Au2 Cl5 89.96(3) . . ? Cl3 Au2 Cl5 178.75(4) . . ? Cl6 Au2 Cl5 90.79(3) . . ? 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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 N1 N2 C1 0.5(4) . . . . ? C15 N1 N2 C1 -174.5(3) . . . . ? C7 N1 N2 Au1 171.5(2) . . . . ? C15 N1 N2 Au1 -3.6(4) . . . . ? N4 Au1 N2 C1 133.9(3) . . . . ? Cl1 Au1 N2 C1 -45.0(3) . . . . ? N4 Au1 N2 N1 -34.7(3) . . . . ? Cl1 Au1 N2 N1 146.4(2) . . . . ? C14 N3 N4 C8 -2.8(4) . . . . ? C15 N3 N4 C8 -173.0(3) . . . . ? C14 N3 N4 Au1 -174.5(2) . . . . ? C15 N3 N4 Au1 15.4(4) . . . . ? N2 Au1 N4 C8 -140.7(3) . . . . ? Cl2 Au1 N4 C8 38.8(3) . . . . ? N2 Au1 N4 N3 28.8(2) . . . . ? Cl2 Au1 N4 N3 -151.7(2) . . . . ? N1 N2 C1 C2 -0.4(4) . . . . ? Au1 N2 C1 C2 -169.9(2) . . . . ? N2 C1 C2 C7 0.1(4) . . . . ? N2 C1 C2 C3 179.5(4) . . . . ? C1 C2 C3 C4 -179.3(4) . . . . ? C7 C2 C3 C4 0.1(5) . . . . ? C2 C3 C4 C5 -1.1(6) . . . . ? C3 C4 C5 C6 0.5(6) . . . . ? C4 C5 C6 C7 1.1(5) . . . . ? N2 N1 C7 C6 178.5(3) . . . . ? C15 N1 C7 C6 -7.2(6) . . . . ? N2 N1 C7 C2 -0.4(4) . . . . ? C15 N1 C7 C2 173.9(3) . . . . ? C5 C6 C7 N1 179.0(3) . . . . ? C5 C6 C7 C2 -2.2(5) . . . . ? C1 C2 C7 N1 0.2(4) . . . . ? C3 C2 C7 N1 -179.3(3) . . . . ? C1 C2 C7 C6 -178.8(3) . . . . ? C3 C2 C7 C6 1.7(5) . . . . ? N3 N4 C8 C9 2.0(4) . . . . ? Au1 N4 C8 C9 172.3(2) . . . . ? N4 C8 C9 C14 -0.5(4) . . . . ? N4 C8 C9 C10 178.6(4) . . . . ? C8 C9 C10 C11 179.6(4) . . . . ? C14 C9 C10 C11 -1.3(5) . . . . ? C9 C10 C11 C12 1.1(6) . . . . ? C10 C11 C12 C13 0.3(6) . . . . ? C11 C12 C13 C14 -1.3(5) . . . . ? N4 N3 C14 C13 -178.4(3) . . . . ? C15 N3 C14 C13 -9.8(6) . . . . ? N4 N3 C14 C9 2.4(4) . . . . ? C15 N3 C14 C9 171.0(3) . . . . ? C12 C13 C14 N3 -178.0(3) . . . . ? C12 C13 C14 C9 1.1(5) . . . . ? C8 C9 C14 N3 -1.2(4) . . . . ? C10 C9 C14 N3 179.5(3) . . . . ? C8 C9 C14 C13 179.6(3) . . . . ? C10 C9 C14 C13 0.2(5) . . . . ? C14 N3 C15 N1 124.6(3) . . . . ? N4 N3 C15 N1 -67.8(4) . . . . ? C7 N1 C15 N3 -113.3(4) . . . . ? N2 N1 C15 N3 60.6(4) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.59 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.088 _refine_diff_density_min -0.729 _refine_diff_density_rms 0.162 data_24 _database_code_depnum_ccdc_archive 'CCDC 917680' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C15 H12 Au Cl2 N4, Au Cl4, 2(C2 H3 N)' _chemical_formula_sum 'C19 H18 Au2 Cl6 N6' _chemical_formula_weight 937.03 _chemical_absolute_configuration . 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' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Au Au -2.0133 8.8022 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' _symmetry_space_group_name_Hall 'P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 7.9242(7) _cell_length_b 15.9274(12) _cell_length_c 20.1872(16) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2547.9(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9948 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 26.63 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.13 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 2.443 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1736 _exptl_absorpt_coefficient_mu 12.154 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1980 _exptl_absorpt_correction_T_max 0.3761 _exptl_absorpt_process_details ; program SADABS, Bruker (2001). ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker-Nonius X8kappa APEX II CCD area detector ; _diffrn_measurement_method 'phi and omega scans with narrow frames' _diffrn_detector_area_resol_mean 8.26 _diffrn_standards_decay_% 0 _diffrn_reflns_number 39194 _diffrn_reflns_av_R_equivalents 0.0447 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.24 _reflns_number_total 4556 _reflns_number_gt 4332 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'APEX2 Software Suite (Bruker, 2007)' _computing_cell_refinement 'APEX2 Software Suite (Bruker, 2007)' _computing_data_reduction 'APEX2 Software Suite (Bruker, 2007)' _computing_structure_solution 'SIR2002 (Burla et al., 2003)' _computing_structure_refinement 'SHELXL97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL (Sheldrick, 2008)' _computing_publication_material 'SHELXTL and publCIF (Westrip, 2010)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0346P)^2^+6.1542P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.453(8) _refine_ls_number_reflns 4556 _refine_ls_number_parameters 301 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0263 _refine_ls_R_factor_gt 0.0239 _refine_ls_wR_factor_ref 0.0577 _refine_ls_wR_factor_gt 0.0568 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Au1 Au 0.72319(3) 0.481244(16) 0.265830(12) 0.01435(7) Uani 1 1 d . . . Cl1 Cl 0.5468(2) 0.37986(12) 0.30305(10) 0.0241(4) Uani 1 1 d . . . Cl2 Cl 0.5419(2) 0.58052(12) 0.30401(10) 0.0248(4) Uani 1 1 d . . . N1 N 0.8911(7) 0.3933(3) 0.2340(4) 0.0183(13) Uani 1 1 d . . . N2 N 1.0581(7) 0.4104(3) 0.2429(3) 0.0146(13) Uani 1 1 d . . . N3 N 0.8838(7) 0.5709(4) 0.2356(3) 0.0203(13) Uani 1 1 d . . . N4 N 1.0533(7) 0.5581(3) 0.2411(3) 0.0177(13) Uani 1 1 d . . . C1 C 1.1543(11) 0.3523(4) 0.2133(4) 0.0196(16) Uani 1 1 d . . . H1 H 1.2741 0.3512 0.2118 0.023 Uiso 1 1 calc R . . C2 C 1.0450(10) 0.2938(5) 0.1852(4) 0.0186(16) Uani 1 1 d . . . C3 C 1.0715(12) 0.2195(5) 0.1480(4) 0.0268(18) Uani 1 1 d . . . H3 H 1.1820 0.1989 0.1394 0.032 Uiso 1 1 calc R . . C4 C 0.9348(12) 0.1794(5) 0.1253(4) 0.0269(19) Uani 1 1 d . . . H4 H 0.9488 0.1282 0.1018 0.032 Uiso 1 1 calc R . . C5 C 0.7696(12) 0.2112(5) 0.1353(4) 0.0272(18) Uani 1 1 d . . . H5 H 0.6770 0.1821 0.1161 0.033 Uiso 1 1 calc R . . C6 C 0.7383(10) 0.2819(4) 0.1715(4) 0.0224(17) Uani 1 1 d . . . H6 H 0.6270 0.3022 0.1784 0.027 Uiso 1 1 calc R . . C7 C 0.8806(9) 0.3231(4) 0.1981(4) 0.0183(16) Uani 1 1 d . . . C8 C 1.1406(9) 0.6178(4) 0.2111(3) 0.0159(15) Uani 1 1 d . . . H8 H 1.2601 0.6224 0.2104 0.019 Uiso 1 1 calc R . . C9 C 1.0285(10) 0.6725(5) 0.1808(4) 0.0200(17) Uani 1 1 d . . . C10 C 1.0479(11) 0.7468(5) 0.1443(4) 0.0223(17) Uani 1 1 d . . . H10 H 1.1561 0.7705 0.1365 0.027 Uiso 1 1 calc R . . C11 C 0.9038(12) 0.7839(5) 0.1203(4) 0.0263(19) Uani 1 1 d . . . H11 H 0.9127 0.8340 0.0950 0.032 Uiso 1 1 calc R . . C12 C 0.7429(11) 0.7491(5) 0.1323(4) 0.0253(18) Uani 1 1 d . . . H12 H 0.6469 0.7758 0.1135 0.030 Uiso 1 1 calc R . . C13 C 0.7195(11) 0.6782(5) 0.1701(4) 0.0232(17) Uani 1 1 d . . . H13 H 0.6102 0.6561 0.1786 0.028 Uiso 1 1 calc R . . C14 C 0.8646(10) 0.6407(4) 0.1952(4) 0.0171(16) Uani 1 1 d . . . C15 C 1.1119(8) 0.4858(4) 0.2777(3) 0.0191(14) Uani 1 1 d . . . H15A H 1.0642 0.4863 0.3230 0.023 Uiso 1 1 calc R . . H15B H 1.2365 0.4869 0.2812 0.023 Uiso 1 1 calc R . . Au2 Au 0.33471(3) 0.494375(17) 0.043885(12) 0.02006(8) Uani 1 1 d . . . Cl3 Cl 0.4657(2) 0.48507(14) 0.14451(9) 0.0316(4) Uani 1 1 d . . . Cl4 Cl 0.3488(3) 0.63700(11) 0.04924(11) 0.0356(5) Uani 1 1 d . . . Cl5 Cl 0.2022(2) 0.50361(13) -0.05602(8) 0.0311(4) Uani 1 1 d . . . Cl6 Cl 0.3257(3) 0.35141(11) 0.04039(11) 0.0357(5) Uani 1 1 d . . . N5 N 0.9390(10) 0.4786(5) 0.0973(4) 0.0437(19) Uani 1 1 d . . . C16 C 0.8975(11) 0.4303(6) 0.0584(5) 0.037(2) Uani 1 1 d . . . C17 C 0.8472(15) 0.3686(6) 0.0089(5) 0.044(2) Uani 1 1 d . . . H17A H 0.8926 0.3848 -0.0344 0.066 Uiso 1 1 calc R . . H17B H 0.7237 0.3661 0.0065 0.066 Uiso 1 1 calc R . . H17C H 0.8913 0.3133 0.0213 0.066 Uiso 1 1 calc R . . N6 N 0.8479(9) 0.4733(5) 0.4132(4) 0.0439(19) Uani 1 1 d . . . C18 C 0.7777(11) 0.4279(5) 0.4464(4) 0.0269(17) Uani 1 1 d . . . C19 C 0.6839(14) 0.3694(6) 0.4875(4) 0.043(3) Uani 1 1 d . . . H19A H 0.5671 0.3661 0.4719 0.065 Uiso 1 1 calc R . . H19B H 0.6853 0.3890 0.5336 0.065 Uiso 1 1 calc R . . H19C H 0.7362 0.3138 0.4849 0.065 Uiso 1 1 calc R . . 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 Au1 0.00948(11) 0.01825(13) 0.01534(12) 0.00075(10) 0.00055(9) -0.00154(9) Cl1 0.0160(9) 0.0306(11) 0.0256(10) 0.0057(8) 0.0018(8) -0.0082(7) Cl2 0.0172(9) 0.0296(11) 0.0275(10) -0.0066(8) 0.0044(8) 0.0032(7) N1 0.014(3) 0.017(3) 0.023(3) -0.001(3) 0.007(3) -0.007(2) N2 0.011(3) 0.018(3) 0.014(3) 0.000(2) -0.002(3) -0.002(2) N3 0.016(3) 0.026(3) 0.018(3) 0.001(3) -0.005(3) 0.002(2) N4 0.014(3) 0.018(3) 0.020(3) 0.004(3) 0.002(3) 0.002(2) C1 0.019(4) 0.018(4) 0.022(4) 0.001(3) 0.008(3) 0.006(3) C2 0.021(4) 0.021(4) 0.014(4) 0.008(3) -0.002(3) 0.002(3) C3 0.032(5) 0.023(4) 0.026(4) 0.001(3) -0.004(4) 0.002(4) C4 0.046(6) 0.014(4) 0.021(4) 0.007(3) 0.001(4) -0.002(4) C5 0.033(5) 0.023(4) 0.025(4) 0.004(3) -0.008(4) -0.011(4) C6 0.017(4) 0.020(4) 0.030(4) 0.005(3) 0.007(4) -0.005(3) C7 0.020(4) 0.016(4) 0.019(4) 0.003(3) 0.000(3) 0.000(3) C8 0.006(3) 0.022(4) 0.020(4) -0.004(3) 0.001(3) -0.006(3) C9 0.025(5) 0.016(4) 0.019(4) -0.005(3) 0.002(3) -0.004(3) C10 0.023(4) 0.026(4) 0.019(4) -0.005(3) 0.006(3) -0.006(3) C11 0.046(6) 0.017(4) 0.015(4) -0.003(3) 0.000(4) 0.001(4) C12 0.024(5) 0.025(4) 0.027(4) -0.001(3) 0.005(4) 0.007(3) C13 0.024(4) 0.022(4) 0.023(4) -0.005(3) -0.003(4) 0.000(3) C14 0.021(4) 0.015(4) 0.015(4) -0.006(3) 0.003(3) -0.002(3) C15 0.013(3) 0.021(4) 0.022(4) -0.001(3) 0.000(3) -0.007(3) Au2 0.01849(13) 0.02493(15) 0.01676(13) -0.00022(11) 0.00142(10) -0.00008(11) Cl3 0.0325(10) 0.0374(11) 0.0250(9) 0.0027(9) -0.0079(7) -0.0031(10) Cl4 0.0515(13) 0.0232(9) 0.0320(12) -0.0002(8) 0.0056(11) 0.0006(9) Cl5 0.0297(9) 0.0450(11) 0.0185(8) -0.0004(8) -0.0020(7) 0.0006(9) Cl6 0.0532(14) 0.0236(10) 0.0303(11) -0.0019(8) 0.0047(11) -0.0023(9) N5 0.057(5) 0.041(5) 0.033(4) 0.010(4) 0.004(4) 0.005(4) C16 0.034(5) 0.045(6) 0.031(5) 0.014(5) 0.011(4) 0.005(4) C17 0.056(7) 0.041(6) 0.036(6) 0.011(4) -0.015(5) -0.015(5) N6 0.036(4) 0.061(5) 0.035(4) -0.002(4) -0.001(3) 0.004(4) C18 0.026(4) 0.032(4) 0.023(4) 0.000(3) -0.001(4) 0.005(4) C19 0.060(7) 0.038(5) 0.032(5) 0.002(4) 0.010(5) 0.008(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 Au1 N3 2.009(6) . ? Au1 N1 2.035(6) . ? Au1 Cl1 2.2642(18) . ? Au1 Cl2 2.2710(18) . ? N1 C7 1.336(10) . ? N1 N2 1.363(8) . ? N2 C1 1.340(9) . ? N2 C15 1.454(8) . ? N3 N4 1.363(8) . ? N3 C14 1.386(10) . ? N4 C8 1.322(9) . ? N4 C15 1.446(9) . ? C1 C2 1.393(11) . ? C1 H1 0.9500 . ? C2 C7 1.407(11) . ? C2 C3 1.419(11) . ? C3 C4 1.338(12) . ? C3 H3 0.9500 . ? C4 C5 1.418(13) . ? C4 H4 0.9500 . ? C5 C6 1.365(11) . ? C5 H5 0.9500 . ? C6 C7 1.411(11) . ? C6 H6 0.9500 . ? C8 C9 1.387(11) . ? C8 H8 0.9500 . ? C9 C10 1.402(11) . ? C9 C14 1.424(11) . ? C10 C11 1.374(12) . ? C10 H10 0.9500 . ? C11 C12 1.411(13) . ? C11 H11 0.9500 . ? C12 C13 1.376(11) . ? C12 H12 0.9500 . ? C13 C14 1.392(11) . ? C13 H13 0.9500 . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? Au2 Cl4 2.2769(19) . ? Au2 Cl5 2.2785(17) . ? Au2 Cl6 2.2793(18) . ? Au2 Cl3 2.2859(18) . ? N5 C16 1.146(11) . ? C16 C17 1.458(14) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? N6 C18 1.132(10) . ? C18 C19 1.453(12) . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? 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 N3 Au1 N1 88.8(2) . . ? N3 Au1 Cl1 178.16(19) . . ? N1 Au1 Cl1 91.01(16) . . ? N3 Au1 Cl2 90.51(18) . . ? N1 Au1 Cl2 178.1(2) . . ? Cl1 Au1 Cl2 89.62(7) . . ? C7 N1 N2 107.4(6) . . ? C7 N1 Au1 135.0(5) . . ? N2 N1 Au1 117.1(4) . . ? C1 N2 N1 110.9(6) . . ? C1 N2 C15 128.2(6) . . ? N1 N2 C15 120.9(5) . . ? N4 N3 C14 106.1(6) . . ? N4 N3 Au1 119.5(4) . . ? C14 N3 Au1 132.8(5) . . ? C8 N4 N3 111.7(6) . . ? C8 N4 C15 129.7(6) . . ? N3 N4 C15 118.5(5) . . ? N2 C1 C2 106.8(7) . . ? N2 C1 H1 126.6 . . ? C2 C1 H1 126.6 . . ? C1 C2 C7 106.2(7) . . ? C1 C2 C3 133.0(8) . . ? C7 C2 C3 120.8(8) . . ? C4 C3 C2 117.3(8) . . ? C4 C3 H3 121.3 . . ? C2 C3 H3 121.3 . . ? C3 C4 C5 121.9(8) . . ? C3 C4 H4 119.0 . . ? C5 C4 H4 119.0 . . ? C6 C5 C4 122.6(8) . . ? C6 C5 H5 118.7 . . ? C4 C5 H5 118.7 . . ? C5 C6 C7 116.2(7) . . ? C5 C6 H6 121.9 . . ? C7 C6 H6 121.9 . . ? N1 C7 C2 108.7(7) . . ? N1 C7 C6 130.2(7) . . ? C2 C7 C6 121.0(7) . . ? N4 C8 C9 108.6(6) . . ? N4 C8 H8 125.7 . . ? C9 C8 H8 125.7 . . ? C8 C9 C10 133.8(8) . . ? C8 C9 C14 105.7(7) . . ? C10 C9 C14 120.5(7) . . ? C11 C10 C9 117.2(8) . . ? C11 C10 H10 121.4 . . ? C9 C10 H10 121.4 . . ? C10 C11 C12 121.5(7) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C13 C12 C11 122.6(8) . . ? C13 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? C12 C13 C14 116.3(8) . . ? C12 C13 H13 121.8 . . ? C14 C13 H13 121.8 . . ? N3 C14 C13 130.5(7) . . ? N3 C14 C9 107.8(7) . . ? C13 C14 C9 121.7(7) . . ? N4 C15 N2 108.5(5) . . ? N4 C15 H15A 110.0 . . ? N2 C15 H15A 110.0 . . ? N4 C15 H15B 110.0 . . ? N2 C15 H15B 110.0 . . ? H15A C15 H15B 108.4 . . ? Cl4 Au2 Cl5 90.02(8) . . ? Cl4 Au2 Cl6 178.60(8) . . ? Cl5 Au2 Cl6 91.30(8) . . ? Cl4 Au2 Cl3 90.01(8) . . ? Cl5 Au2 Cl3 179.55(7) . . ? Cl6 Au2 Cl3 88.67(8) . . ? N5 C16 C17 179.2(11) . . ? 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 . . ? N6 C18 C19 178.4(9) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? 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_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Au1 N1 C7 -133.3(8) . . . . ? Cl1 Au1 N1 C7 48.6(7) . . . . ? N3 Au1 N1 N2 37.3(5) . . . . ? Cl1 Au1 N1 N2 -140.9(5) . . . . ? C7 N1 N2 C1 0.0(8) . . . . ? Au1 N1 N2 C1 -173.1(5) . . . . ? C7 N1 N2 C15 177.1(6) . . . . ? Au1 N1 N2 C15 4.1(9) . . . . ? N1 Au1 N3 N4 -35.2(5) . . . . ? Cl2 Au1 N3 N4 143.0(6) . . . . ? N1 Au1 N3 C14 128.1(8) . . . . ? Cl2 Au1 N3 C14 -53.7(7) . . . . ? C14 N3 N4 C8 4.2(8) . . . . ? Au1 N3 N4 C8 171.5(5) . . . . ? C14 N3 N4 C15 -176.4(6) . . . . ? Au1 N3 N4 C15 -9.1(9) . . . . ? N1 N2 C1 C2 -1.3(8) . . . . ? C15 N2 C1 C2 -178.2(6) . . . . ? N2 C1 C2 C7 2.1(8) . . . . ? N2 C1 C2 C3 179.8(8) . . . . ? C1 C2 C3 C4 -176.7(8) . . . . ? C7 C2 C3 C4 0.7(12) . . . . ? C2 C3 C4 C5 2.7(12) . . . . ? C3 C4 C5 C6 -3.5(13) . . . . ? C4 C5 C6 C7 0.8(12) . . . . ? N2 N1 C7 C2 1.4(8) . . . . ? Au1 N1 C7 C2 172.6(6) . . . . ? N2 N1 C7 C6 -175.1(8) . . . . ? Au1 N1 C7 C6 -3.9(13) . . . . ? C1 C2 C7 N1 -2.2(9) . . . . ? C3 C2 C7 N1 179.8(7) . . . . ? C1 C2 C7 C6 174.7(7) . . . . ? C3 C2 C7 C6 -3.3(11) . . . . ? C5 C6 C7 N1 178.6(8) . . . . ? C5 C6 C7 C2 2.5(11) . . . . ? N3 N4 C8 C9 -2.8(9) . . . . ? C15 N4 C8 C9 178.0(7) . . . . ? N4 C8 C9 C10 177.8(8) . . . . ? N4 C8 C9 C14 0.1(8) . . . . ? C8 C9 C10 C11 178.8(8) . . . . ? C14 C9 C10 C11 -3.8(11) . . . . ? C9 C10 C11 C12 0.6(11) . . . . ? C10 C11 C12 C13 2.1(12) . . . . ? C11 C12 C13 C14 -1.4(12) . . . . ? N4 N3 C14 C13 175.7(7) . . . . ? Au1 N3 C14 C13 10.8(12) . . . . ? N4 N3 C14 C9 -4.0(8) . . . . ? Au1 N3 C14 C9 -168.9(5) . . . . ? C12 C13 C14 N3 178.4(7) . . . . ? C12 C13 C14 C9 -1.9(11) . . . . ? C8 C9 C14 N3 2.4(8) . . . . ? C10 C9 C14 N3 -175.7(7) . . . . ? C8 C9 C14 C13 -177.3(7) . . . . ? C10 C9 C14 C13 4.6(12) . . . . ? C8 N4 C15 N2 -116.2(8) . . . . ? N3 N4 C15 N2 64.6(8) . . . . ? C1 N2 C15 N4 114.6(8) . . . . ? N1 N2 C15 N4 -62.0(8) . . . . ? _diffrn_measured_fraction_theta_max 0.987 _diffrn_reflns_theta_full 25.24 _diffrn_measured_fraction_theta_full 0.987 _refine_diff_density_max 3.788 _refine_diff_density_min -1.013 _refine_diff_density_rms 0.148 ###END