# Electronic Supplementary Material (ESI) for CrystEngComm # This journal is © The Royal Society of Chemistry 2012 ####################################################################### # # 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_jp359x _database_code_depnum_ccdc_archive 'CCDC 637852' #TrackingRef 'web_deposit_cif_file_0_BrianSkelton_1351829001.jp359x.cif' _audit_creation_date 2012-08-25T13:49:18-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C8 H12 Ag N4, F6 P' _chemical_formula_sum 'C8 H12 Ag F6 N4 P' _chemical_formula_weight 417.06 #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.5321(4) _cell_length_b 20.7094(10) _cell_length_c 25.7690(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4553.2(4) _cell_formula_units_Z 12 _cell_measurement_temperature 150(2) #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description cuboid _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.35 _exptl_crystal_size_min 0.30 _exptl_crystal_density_diffrn 1.825 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2448 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.491 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min 0.595 _exptl_absorpt_correction_T_max 0.844 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.084 _diffrn_reflns_av_unetI/netI 0.1279 _diffrn_reflns_number 95255 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -35 _diffrn_reflns_limit_k_max 35 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_l_max 44 _diffrn_reflns_theta_min 1.26 _diffrn_reflns_theta_max 37.56 _diffrn_reflns_theta_full 37.56 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 24028 _reflns_number_gt 9573 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Siemens SMART (Siemens, 1995)' _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_structure_solution SIR92 _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ORTEPII _computing_publication_material WinGX #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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. The three hexafluorophosphate anions are each disordered over two sites. The geometries of the disordered atoms were restrained to ideal values with the displacement parameters restrained to reasonable values. ; _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^)+(0.0219P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 24028 _refine_ls_number_parameters 682 _refine_ls_number_restraints 208 _refine_ls_R_factor_all 0.1507 _refine_ls_R_factor_gt 0.0378 _refine_ls_wR_factor_ref 0.0706 _refine_ls_wR_factor_gt 0.0565 _refine_ls_goodness_of_fit_ref 0.762 _refine_ls_restrained_S_all 0.797 _refine_ls_shift/su_max 0.046 _refine_ls_shift/su_mean 0.001 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.006(15) _refine_diff_density_max 1.578 _refine_diff_density_min -0.402 _refine_diff_density_rms 0.08 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' Ag Ag -0.8971 1.1015 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.19946(4) 0.324503(13) 0.212613(11) 0.03493(6) Uani 1 1 d . . . Ag2 Ag 0.28457(3) 0.670109(15) 0.211186(13) 0.03723(8) Uani 1 1 d . . . Ag3 Ag 0.18711(3) 0.498876(14) 0.458541(9) 0.03692(6) Uani 1 1 d . . . N111 N 0.1167(3) 0.41396(13) 0.16686(10) 0.0371(7) Uani 1 1 d . . . C111 C 0.0574(4) 0.45698(16) 0.14828(13) 0.0361(8) Uani 1 1 d . . . C112 C -0.0213(5) 0.51297(19) 0.12511(16) 0.0593(13) Uani 1 1 d . . . H11A H 0.0154 0.5525 0.1421 0.089 Uiso 1 1 calc R . . H11B H -0.1348 0.5089 0.1298 0.089 Uiso 1 1 calc R . . H11C H 0.0029 0.5149 0.088 0.089 Uiso 1 1 calc R . . N121 N 0.1211(3) 0.33267(13) 0.29718(10) 0.0387(7) Uani 1 1 d . . . C121 C 0.0693(4) 0.33841(15) 0.33681(13) 0.0324(7) Uani 1 1 d . . . C122 C 0.0037(6) 0.3460(2) 0.38872(14) 0.0408(10) Uani 1 1 d . . . H12A H 0.0879 0.3432 0.4145 0.061 Uiso 1 1 calc R . . H12B H -0.073 0.3116 0.3951 0.061 Uiso 1 1 calc R . . H12C H -0.048 0.3881 0.3914 0.061 Uiso 1 1 calc R . . N131 N 0.4651(3) 0.32752(16) 0.21273(11) 0.0425(8) Uani 1 1 d . . . C131 C 0.5979(4) 0.32773(17) 0.21244(12) 0.0304(7) Uani 1 1 d . . . C132 C 0.7670(3) 0.3280(2) 0.2132(2) 0.0391(11) Uani 1 1 d . . . H13A H 0.8043 0.3011 0.242 0.059 Uiso 1 1 calc R . . H13B H 0.8048 0.3723 0.2178 0.059 Uiso 1 1 calc R . . H13C H 0.8068 0.3106 0.1804 0.059 Uiso 1 1 calc R . . N141 N 0.1116(3) 0.23480(12) 0.17041(10) 0.0357(7) Uani 1 1 d . . . C141 C 0.0643(4) 0.19579(16) 0.14462(13) 0.0309(8) Uani 1 1 d . . . C142 C 0.0061(6) 0.14492(19) 0.10978(16) 0.0454(11) Uani 1 1 d . . . H14A H 0.0816 0.138 0.0817 0.068 Uiso 1 1 calc R . . H14B H -0.0949 0.1581 0.0951 0.068 Uiso 1 1 calc R . . H14C H -0.0073 0.1047 0.1294 0.068 Uiso 1 1 calc R . . N211 N 0.3689(3) 0.58188(13) 0.16448(10) 0.0370(7) Uani 1 1 d . . . C211 C 0.4253(4) 0.54179(16) 0.14276(13) 0.0346(8) Uani 1 1 d . . . C212 C 0.4989(5) 0.4881(2) 0.11435(16) 0.0697(14) Uani 1 1 d . . . H21A H 0.5838 0.4698 0.1353 0.105 Uiso 1 1 calc R . . H21B H 0.5414 0.504 0.0814 0.105 Uiso 1 1 calc R . . H21C H 0.4204 0.4546 0.1074 0.105 Uiso 1 1 calc R . . N221 N 0.3642(3) 0.66504(13) 0.29604(10) 0.0389(7) Uani 1 1 d . . . C221 C 0.4204(4) 0.66246(14) 0.33504(12) 0.0307(7) Uani 1 1 d . . . C222 C 0.4942(6) 0.6582(2) 0.38567(15) 0.0463(12) Uani 1 1 d . . . H22A H 0.5031 0.6128 0.3959 0.069 Uiso 1 1 calc R . . H22B H 0.4305 0.6814 0.4112 0.069 Uiso 1 1 calc R . . H22C H 0.599 0.6775 0.3841 0.069 Uiso 1 1 calc R . . N231 N 0.0206(4) 0.66803(16) 0.20867(11) 0.0452(8) Uani 1 1 d . . . C231 C -0.1121(4) 0.66926(17) 0.21090(12) 0.0322(8) Uani 1 1 d . . . C232 C -0.2807(4) 0.6718(2) 0.21256(17) 0.0362(10) Uani 1 1 d . . . H23A H -0.3155 0.7165 0.2077 0.054 Uiso 1 1 calc R . . H23B H -0.3175 0.6559 0.2462 0.054 Uiso 1 1 calc R . . H23C H -0.324 0.6448 0.1848 0.054 Uiso 1 1 calc R . . N241 N 0.3739(3) 0.76145(13) 0.17126(10) 0.0376(7) Uani 1 1 d . . . C241 C 0.4269(4) 0.79989(17) 0.14570(13) 0.0334(8) Uani 1 1 d . . . C242 C 0.4962(7) 0.8489(2) 0.11207(17) 0.0507(12) Uani 1 1 d . . . H24A H 0.447 0.8469 0.0778 0.076 Uiso 1 1 calc R . . H24B H 0.6089 0.8409 0.1087 0.076 Uiso 1 1 calc R . . H24C H 0.4791 0.8917 0.1272 0.076 Uiso 1 1 calc R . . N311 N 0.2669(4) 0.5892(2) 0.50107(18) 0.0489(11) Uani 1 1 d . . . C311 C 0.2642(4) 0.6326(2) 0.5277(2) 0.0342(11) Uani 1 1 d . . . C312 C 0.2600(4) 0.6884(2) 0.56163(19) 0.0418(11) Uani 1 1 d . . . H31A H 0.1788 0.7184 0.5497 0.063 Uiso 1 1 calc R . . H31B H 0.3621 0.71 0.561 0.063 Uiso 1 1 calc R . . H31C H 0.2363 0.6744 0.5971 0.063 Uiso 1 1 calc R . . N321 N -0.0767(3) 0.4978(2) 0.45986(12) 0.0463(7) Uani 1 1 d . . . C321 C -0.2082(4) 0.4996(2) 0.46363(13) 0.0343(7) Uani 1 1 d . . . C322 C -0.3777(4) 0.5030(3) 0.46895(13) 0.0460(9) Uani 1 1 d . . . H32A H -0.4157 0.4642 0.4868 0.069 Uiso 1 1 calc R . . H32B H -0.4258 0.5057 0.4345 0.069 Uiso 1 1 calc R . . H32C H -0.406 0.5414 0.4892 0.069 Uiso 1 1 calc R . . N331 N 0.2597(3) 0.4992(2) 0.37420(10) 0.0420(7) Uani 1 1 d . . . C331 C 0.2569(3) 0.4989(3) 0.33023(12) 0.0371(7) Uani 1 1 d . . . C332 C 0.2511(4) 0.4985(3) 0.27407(11) 0.0516(11) Uani 1 1 d . . . H33A H 0.3396 0.4734 0.2605 0.077 Uiso 1 1 calc R . . H33B H 0.2574 0.5429 0.2611 0.077 Uiso 1 1 calc R . . H33C H 0.1526 0.4788 0.2626 0.077 Uiso 1 1 calc R . . N341 N 0.2717(4) 0.4116(2) 0.50254(18) 0.0494(10) Uani 1 1 d . . . C341 C 0.2764(4) 0.3680(2) 0.52838(19) 0.0348(10) Uani 1 1 d . . . C342 C 0.2824(5) 0.3129(2) 0.56222(18) 0.0447(10) Uani 1 1 d . . . H34A H 0.315 0.2748 0.5424 0.067 Uiso 1 1 calc R . . H34B H 0.1785 0.3053 0.5772 0.067 Uiso 1 1 calc R . . H34C H 0.358 0.3209 0.5901 0.067 Uiso 1 1 calc R . . P1 P -0.25390(11) 0.50036(9) 0.29339(4) 0.03738(19) Uani 1 1 d D . . F11 F -0.3636(5) 0.43930(12) 0.29231(15) 0.1038(14) Uani 1 1 d . A . F12 F -0.1422(5) 0.56044(13) 0.29310(15) 0.1026(14) Uani 1 1 d . A . F13 F -0.1272(8) 0.4484(3) 0.2979(3) 0.0712(19) Uani 0.5 1 d PDU A 1 F15 F -0.3989(7) 0.5507(3) 0.2870(4) 0.0642(17) Uani 0.5 1 d PDU A 1 F14 F -0.2845(12) 0.5032(5) 0.35303(19) 0.104(3) Uani 0.5 1 d PDU A 1 F16 F -0.2403(10) 0.5000(5) 0.23294(17) 0.0743(17) Uani 0.5 1 d PDU A 1 F13' F -0.1355(10) 0.4792(4) 0.3386(3) 0.125(3) Uani 0.5 1 d PDU A 2 F14' F -0.3661(10) 0.5298(5) 0.3320(5) 0.144(4) Uani 0.5 1 d PDU A 2 F15' F -0.3561(13) 0.5213(5) 0.2479(4) 0.144(4) Uani 0.5 1 d PDU A 2 F16' F -0.1322(10) 0.4702(5) 0.2541(4) 0.142(4) Uani 0.5 1 d PDU A 2 P2 P -0.26676(10) 0.32876(6) 0.05046(6) 0.0343(3) Uani 1 1 d D . . F21 F -0.3796(3) 0.32632(14) 0.09987(10) 0.0674(8) Uani 1 1 d U B . F22 F -0.1566(4) 0.33242(13) 0.00111(10) 0.0697(8) Uani 1 1 d U B . F23 F -0.1744(8) 0.2704(3) 0.0697(3) 0.116(3) Uani 0.637(7) 1 d PDU B 1 F24 F -0.3879(6) 0.2797(3) 0.02217(19) 0.0744(19) Uani 0.637(7) 1 d PDU B 1 F25 F -0.3780(7) 0.3859(3) 0.0296(2) 0.096(2) Uani 0.637(7) 1 d PDU B 1 F26 F -0.1556(8) 0.3769(3) 0.0781(2) 0.090(2) Uani 0.637(7) 1 d PDU B 1 F23' F -0.2606(14) 0.2541(4) 0.0461(4) 0.076(4) Uani 0.363(7) 1 d PDU B 2 F24' F -0.3955(9) 0.3313(6) 0.0125(3) 0.065(3) Uani 0.363(7) 1 d PDU B 2 F25' F -0.2519(12) 0.4035(4) 0.0563(5) 0.074(4) Uani 0.363(7) 1 d PDU B 2 F26' F -0.1162(8) 0.3237(6) 0.0913(3) 0.069(3) Uani 0.363(7) 1 d PDU B 2 P3 P -0.26851(11) 0.67164(6) 0.05067(6) 0.0345(3) Uani 1 1 d D . . F31 F -0.4019(6) 0.6833(3) 0.0936(2) 0.0731(18) Uani 0.615(6) 1 d PDU C 1 F32 F -0.1396(6) 0.6573(3) 0.01026(18) 0.0789(19) Uani 0.615(6) 1 d PDU C 1 F33 F -0.3928(6) 0.6724(3) 0.0064(2) 0.0645(18) Uani 0.615(6) 1 d PDU C 1 F34 F -0.2424(8) 0.7444(2) 0.0485(3) 0.090(3) Uani 0.615(6) 1 d PDU C 1 F35 F -0.1430(5) 0.6664(3) 0.09727(17) 0.0604(16) Uani 0.615(6) 1 d PDU C 1 F36 F -0.2995(10) 0.5952(2) 0.0584(2) 0.092(2) Uani 0.615(6) 1 d PDU C 1 F31' F -0.1985(16) 0.7076(5) 0.0992(3) 0.109(3) Uani 0.385(6) 1 d PDU C 2 F32' F -0.3327(19) 0.6477(6) -0.0008(5) 0.119(5) Uani 0.385(6) 1 d PDU C 2 F33' F -0.3947(9) 0.6424(5) 0.0835(4) 0.079(3) Uani 0.385(6) 1 d PDU C 2 F34' F -0.1598(13) 0.6162(5) 0.0572(4) 0.104(4) Uani 0.385(6) 1 d PDU C 2 F35' F -0.1354(8) 0.7120(5) 0.0180(3) 0.073(3) Uani 0.385(6) 1 d PDU C 2 F36' F -0.3761(11) 0.7345(4) 0.0403(4) 0.088(3) Uani 0.385(6) 1 d PDU C 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 0.03348(14) 0.03698(15) 0.03434(15) -0.00300(12) -0.00057(15) 0.00117(15) Ag2 0.03636(16) 0.03918(17) 0.03616(17) 0.00036(13) 0.00019(14) 0.00132(13) Ag3 0.04110(14) 0.03587(11) 0.03378(11) 0.00024(15) -0.00103(14) 0.00049(13) N111 0.0443(18) 0.0302(15) 0.0368(16) -0.0016(13) -0.0033(13) -0.0003(13) C111 0.033(2) 0.035(2) 0.041(2) -0.0042(16) -0.0064(15) -0.0042(15) C112 0.052(3) 0.042(3) 0.085(3) 0.021(2) -0.015(2) 0.001(2) N121 0.0456(17) 0.0377(17) 0.0328(16) 0.0000(13) 0.0041(12) 0.0018(13) C121 0.0320(18) 0.0275(18) 0.0376(19) -0.0005(15) -0.0027(14) -0.0057(13) C122 0.046(3) 0.046(2) 0.030(2) -0.0007(19) 0.0072(19) 0.000(2) N131 0.0285(16) 0.057(2) 0.0418(18) 0.0028(19) -0.0011(13) 0.0052(14) C131 0.0295(18) 0.0340(19) 0.0278(17) 0.0036(19) 0.0006(15) -0.0038(16) C132 0.0257(18) 0.050(3) 0.042(3) -0.002(3) 0.0008(15) -0.0088(17) N141 0.0472(19) 0.0296(15) 0.0304(15) -0.0018(12) -0.0030(12) -0.0046(13) C141 0.032(2) 0.0298(19) 0.0314(19) 0.0035(15) 0.0009(14) 0.0011(14) C142 0.048(3) 0.036(2) 0.052(3) -0.009(2) -0.006(2) -0.005(2) N211 0.0433(18) 0.0333(16) 0.0345(16) 0.0020(13) 0.0048(13) -0.0008(12) C211 0.033(2) 0.034(2) 0.036(2) -0.0052(16) 0.0066(15) -0.0056(15) C212 0.065(3) 0.045(3) 0.099(3) -0.025(3) 0.027(3) 0.004(2) N221 0.0452(17) 0.0378(17) 0.0338(17) 0.0028(13) -0.0004(12) 0.0009(12) C221 0.0322(18) 0.0271(18) 0.0329(18) 0.0017(15) 0.0030(14) -0.0007(13) C222 0.045(3) 0.054(3) 0.039(3) 0.000(2) -0.008(2) -0.005(2) N231 0.0406(18) 0.048(2) 0.047(2) -0.0073(18) 0.0040(15) 0.0013(15) C231 0.0316(18) 0.036(2) 0.0289(18) -0.0025(19) -0.0028(16) -0.0004(16) C232 0.0292(17) 0.042(2) 0.037(2) 0.002(2) -0.011(2) -0.005(2) N241 0.0487(19) 0.0315(16) 0.0325(16) 0.0035(13) -0.0004(13) -0.0003(13) C241 0.028(2) 0.040(2) 0.0316(19) -0.0069(16) -0.0037(14) 0.0042(15) C242 0.058(3) 0.042(2) 0.051(3) 0.011(2) 0.007(2) -0.010(2) N311 0.049(2) 0.043(2) 0.055(3) -0.012(2) 0.0002(15) -0.0054(14) C311 0.034(2) 0.036(2) 0.032(3) 0.0039(19) -0.0054(13) -0.0006(14) C312 0.057(3) 0.036(2) 0.032(3) -0.0045(19) -0.0048(14) -0.0039(14) N321 0.0365(17) 0.0450(16) 0.0573(16) 0.003(2) 0.0016(17) -0.0004(18) C321 0.036(2) 0.0284(14) 0.0385(15) -0.001(2) -0.0065(19) -0.006(3) C322 0.035(2) 0.049(2) 0.054(2) -0.003(3) 0.0005(17) -0.008(3) N331 0.0474(18) 0.0448(15) 0.0338(14) 0.001(3) 0.0040(11) 0.0014(13) C331 0.044(2) 0.0339(16) 0.0334(16) 0.002(3) 0.0015(13) -0.0058(13) C332 0.071(3) 0.054(2) 0.0291(17) -0.002(3) -0.0019(15) -0.0214(19) N341 0.042(2) 0.049(2) 0.057(3) 0.017(2) -0.0014(16) 0.0009(15) C341 0.0264(18) 0.039(2) 0.039(3) 0.0011(19) 0.0035(16) 0.0003(16) C342 0.058(2) 0.039(2) 0.037(3) 0.0069(19) 0.0112(19) -0.0024(19) P1 0.0453(5) 0.0309(4) 0.0359(4) -0.0002(8) 0.0030(4) 0.0021(3) F11 0.120(4) 0.0587(17) 0.133(3) -0.0046(19) 0.043(3) -0.042(2) F12 0.106(3) 0.0624(18) 0.139(3) 0.007(2) -0.034(3) -0.032(2) F13 0.061(4) 0.052(3) 0.101(5) 0.021(3) -0.020(4) 0.028(3) F15 0.051(3) 0.043(3) 0.099(5) 0.006(3) 0.012(4) 0.008(2) F14 0.167(7) 0.114(5) 0.032(2) 0.014(4) 0.010(4) 0.007(6) F16 0.106(5) 0.089(4) 0.029(2) 0.001(4) 0.015(3) 0.009(4) F13' 0.132(6) 0.129(7) 0.115(5) 0.051(4) -0.054(5) 0.019(5) F14' 0.122(6) 0.147(7) 0.164(7) -0.101(6) 0.036(6) 0.030(5) F15' 0.144(7) 0.152(8) 0.137(6) 0.050(5) -0.100(5) -0.040(5) F16' 0.095(6) 0.175(8) 0.157(7) -0.074(6) 0.073(5) -0.037(5) P2 0.0376(6) 0.0337(6) 0.0317(7) -0.0020(6) 0.0024(4) -0.0006(4) F21 0.0607(16) 0.103(2) 0.0384(13) -0.0095(15) 0.0109(11) -0.0175(16) F22 0.082(2) 0.0673(17) 0.0597(16) -0.0155(14) 0.0409(15) -0.0184(16) F23 0.086(4) 0.091(4) 0.172(6) 0.068(4) -0.005(4) 0.045(3) F24 0.072(3) 0.087(4) 0.064(3) -0.032(3) 0.021(2) -0.047(3) F25 0.106(4) 0.075(4) 0.106(4) 0.034(3) 0.012(3) 0.051(3) F26 0.088(4) 0.109(5) 0.073(3) -0.030(3) 0.000(3) -0.059(3) F23' 0.130(8) 0.041(4) 0.057(5) -0.012(4) 0.005(4) -0.004(4) F24' 0.052(4) 0.113(7) 0.028(3) 0.008(4) -0.018(3) 0.006(5) F25' 0.102(7) 0.038(4) 0.083(6) -0.026(4) 0.044(4) 0.006(3) F26' 0.034(3) 0.127(7) 0.046(4) -0.012(5) -0.007(3) 0.024(4) P3 0.0356(5) 0.0393(7) 0.0285(6) -0.0008(6) -0.0002(4) 0.0033(4) F31 0.058(3) 0.114(4) 0.048(3) -0.014(3) 0.011(2) 0.028(3) F32 0.064(3) 0.123(5) 0.050(3) -0.009(3) 0.030(2) 0.008(3) F33 0.053(3) 0.093(4) 0.047(3) 0.022(3) -0.019(2) -0.017(3) F34 0.144(6) 0.040(3) 0.086(4) -0.002(3) -0.042(3) -0.021(3) F35 0.035(2) 0.114(4) 0.031(2) 0.012(3) -0.0062(15) 0.011(2) F36 0.147(5) 0.043(3) 0.086(4) 0.016(2) -0.001(4) -0.012(3) F31' 0.150(7) 0.115(6) 0.062(5) -0.024(5) -0.021(5) -0.054(6) F32' 0.151(8) 0.121(7) 0.085(6) -0.035(5) -0.057(6) -0.012(6) F33' 0.049(4) 0.086(6) 0.100(6) 0.044(5) 0.021(4) -0.017(4) F34' 0.098(6) 0.092(5) 0.124(6) 0.052(5) 0.008(5) 0.062(5) F35' 0.053(4) 0.095(6) 0.070(5) 0.044(4) -0.001(3) -0.016(4) F36' 0.083(5) 0.072(5) 0.111(6) 0.017(5) 0.029(5) 0.048(4) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N131 2.268(3) . ? Ag1 N141 2.280(3) . ? Ag1 N121 2.286(3) . ? Ag1 N111 2.307(3) . ? Ag2 N231 2.253(3) . ? Ag2 N241 2.284(3) . ? Ag2 N221 2.292(3) . ? Ag2 N211 2.303(3) . ? Ag3 N341 2.252(4) . ? Ag3 N321 2.251(3) . ? Ag3 N331 2.260(2) . ? Ag3 N311 2.272(4) . ? N111 C111 1.131(4) . ? C111 C112 1.467(5) . ? C112 H11A 0.98 . ? C112 H11B 0.98 . ? C112 H11C 0.98 . ? N121 C121 1.119(4) . ? C121 C122 1.459(5) . ? C122 H12A 0.98 . ? C122 H12B 0.98 . ? C122 H12C 0.98 . ? N131 C131 1.133(4) . ? C131 C132 1.443(4) . ? C132 H13A 0.98 . ? C132 H13B 0.98 . ? C132 H13C 0.98 . ? N141 C141 1.121(4) . ? C141 C142 1.471(5) . ? C142 H14A 0.98 . ? C142 H14B 0.98 . ? C142 H14C 0.98 . ? N211 C211 1.111(4) . ? C211 C212 1.472(5) . ? C212 H21A 0.98 . ? C212 H21B 0.98 . ? C212 H21C 0.98 . ? N221 C221 1.115(4) . ? C221 C222 1.451(5) . ? C222 H22A 0.98 . ? C222 H22B 0.98 . ? C222 H22C 0.98 . ? N231 C231 1.134(4) . ? C231 C232 1.440(4) . ? C232 H23A 0.98 . ? C232 H23B 0.98 . ? C232 H23C 0.98 . ? N241 C241 1.128(4) . ? C241 C242 1.459(5) . ? C242 H24A 0.98 . ? C242 H24B 0.98 . ? C242 H24C 0.98 . ? N311 C311 1.130(6) . ? C311 C312 1.450(6) . ? C312 H31A 0.98 . ? C312 H31B 0.98 . ? C312 H31C 0.98 . ? N321 C321 1.127(3) . ? C321 C322 1.455(4) . ? C322 H32A 0.98 . ? C322 H32B 0.98 . ? C322 H32C 0.98 . ? N331 C331 1.133(4) . ? C331 C332 1.448(4) . ? C332 H33A 0.98 . ? C332 H33B 0.98 . ? C332 H33C 0.98 . ? N341 C341 1.123(5) . ? C341 C342 1.437(6) . ? C342 H34A 0.98 . ? C342 H34B 0.98 . ? C342 H34C 0.98 . ? P1 F15' 1.524(6) . ? P1 F14' 1.509(7) . ? P1 F13 1.529(6) . ? P1 F14 1.560(5) . ? P1 F16' 1.580(6) . ? P1 F16 1.562(5) . ? P1 F12 1.568(3) . ? P1 F11 1.573(3) . ? P1 F13' 1.604(6) . ? P1 F15 1.627(6) . ? P2 F24' 1.471(7) . ? P2 F23 1.526(4) . ? P2 F23' 1.551(8) . ? P2 F26 1.549(4) . ? P2 F25' 1.560(8) . ? P2 F22 1.583(3) . ? P2 F21 1.597(3) . ? P2 F25 1.610(4) . ? P2 F24 1.622(4) . ? P2 F26' 1.665(7) . ? P3 F34' 1.485(7) . ? P3 F33' 1.497(7) . ? P3 F32' 1.517(10) . ? P3 F34 1.524(5) . ? P3 F32 1.543(4) . ? P3 F33 1.558(5) . ? P3 F31' 1.573(8) . ? P3 F31 1.605(5) . ? P3 F35 1.612(4) . ? P3 F36' 1.615(7) . ? P3 F36 1.617(5) . ? P3 F35' 1.642(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 N131 Ag1 N141 110.60(11) . . ? N131 Ag1 N121 106.80(10) . . ? N141 Ag1 N121 114.77(9) . . ? N131 Ag1 N111 106.53(11) . . ? N141 Ag1 N111 108.06(9) . . ? N121 Ag1 N111 109.78(9) . . ? N231 Ag2 N241 109.65(11) . . ? N231 Ag2 N221 108.83(10) . . ? N241 Ag2 N221 111.64(9) . . ? N231 Ag2 N211 106.38(11) . . ? N241 Ag2 N211 108.50(9) . . ? N221 Ag2 N211 111.69(9) . . ? N341 Ag3 N321 107.73(14) . . ? N341 Ag3 N331 113.48(16) . . ? N321 Ag3 N331 106.78(10) . . ? N341 Ag3 N311 108.77(10) . . ? N321 Ag3 N311 107.50(14) . . ? N331 Ag3 N311 112.30(16) . . ? C111 N111 Ag1 170.4(3) . . ? N111 C111 C112 178.9(4) . . ? C111 C112 H11A 109.5 . . ? C111 C112 H11B 109.5 . . ? H11A C112 H11B 109.5 . . ? C111 C112 H11C 109.5 . . ? H11A C112 H11C 109.5 . . ? H11B C112 H11C 109.5 . . ? C121 N121 Ag1 173.4(3) . . ? N121 C121 C122 179.3(4) . . ? C121 C122 H12A 109.5 . . ? C121 C122 H12B 109.5 . . ? H12A C122 H12B 109.5 . . ? C121 C122 H12C 109.5 . . ? H12A C122 H12C 109.5 . . ? H12B C122 H12C 109.5 . . ? C131 N131 Ag1 178.6(3) . . ? N131 C131 C132 178.8(4) . . ? C131 C132 H13A 109.5 . . ? C131 C132 H13B 109.5 . . ? H13A C132 H13B 109.5 . . ? C131 C132 H13C 109.5 . . ? H13A C132 H13C 109.5 . . ? H13B C132 H13C 109.5 . . ? C141 N141 Ag1 171.3(3) . . ? N141 C141 C142 178.4(4) . . ? C141 C142 H14A 109.5 . . ? C141 C142 H14B 109.5 . . ? H14A C142 H14B 109.5 . . ? C141 C142 H14C 109.5 . . ? H14A C142 H14C 109.5 . . ? H14B C142 H14C 109.5 . . ? C211 N211 Ag2 172.5(3) . . ? N211 C211 C212 179.3(4) . . ? C211 C212 H21A 109.5 . . ? C211 C212 H21B 109.5 . . ? H21A C212 H21B 109.5 . . ? C211 C212 H21C 109.5 . . ? H21A C212 H21C 109.5 . . ? H21B C212 H21C 109.5 . . ? C221 N221 Ag2 171.7(3) . . ? N221 C221 C222 179.2(4) . . ? C221 C222 H22A 109.5 . . ? C221 C222 H22B 109.5 . . ? H22A C222 H22B 109.5 . . ? C221 C222 H22C 109.5 . . ? H22A C222 H22C 109.5 . . ? H22B C222 H22C 109.5 . . ? C231 N231 Ag2 174.9(3) . . ? N231 C231 C232 178.5(4) . . ? C231 C232 H23A 109.5 . . ? C231 C232 H23B 109.5 . . ? H23A C232 H23B 109.5 . . ? C231 C232 H23C 109.5 . . ? H23A C232 H23C 109.5 . . ? H23B C232 H23C 109.5 . . ? C241 N241 Ag2 168.9(3) . . ? N241 C241 C242 179.2(4) . . ? C241 C242 H24A 109.5 . . ? C241 C242 H24B 109.5 . . ? H24A C242 H24B 109.5 . . ? C241 C242 H24C 109.5 . . ? H24A C242 H24C 109.5 . . ? H24B C242 H24C 109.5 . . ? C311 N311 Ag3 160.2(3) . . ? N311 C311 C312 179.7(5) . . ? C311 C312 H31A 109.5 . . ? C311 C312 H31B 109.5 . . ? H31A C312 H31B 109.5 . . ? C311 C312 H31C 109.5 . . ? H31A C312 H31C 109.5 . . ? H31B C312 H31C 109.5 . . ? C321 N321 Ag3 175.2(4) . . ? N321 C321 C322 179.1(6) . . ? C321 C322 H32A 109.5 . . ? C321 C322 H32B 109.5 . . ? H32A C322 H32B 109.5 . . ? C321 C322 H32C 109.5 . . ? H32A C322 H32C 109.5 . . ? H32B C322 H32C 109.5 . . ? C331 N331 Ag3 162.8(2) . . ? N331 C331 C332 179.3(3) . . ? C331 C332 H33A 109.5 . . ? C331 C332 H33B 109.5 . . ? H33A C332 H33B 109.5 . . ? C331 C332 H33C 109.5 . . ? H33A C332 H33C 109.5 . . ? H33B C332 H33C 109.5 . . ? C341 N341 Ag3 162.8(3) . . ? N341 C341 C342 179.0(5) . . ? C341 C342 H34A 109.5 . . ? C341 C342 H34B 109.5 . . ? H34A C342 H34B 109.5 . . ? C341 C342 H34C 109.5 . . ? H34A C342 H34C 109.5 . . ? H34B C342 H34C 109.5 . . ? F15' P1 F14' 91.6(6) . . ? F13 P1 F14 94.0(4) . . ? F15' P1 F16' 89.7(5) . . ? F14' P1 F16' 178.3(5) . . ? F13 P1 F16 91.1(4) . . ? F14 P1 F16 174.3(5) . . ? F15' P1 F12 96.8(3) . . ? F14' P1 F12 93.9(4) . . ? F13 P1 F12 97.4(3) . . ? F14 P1 F12 94.4(4) . . ? F16' P1 F12 84.9(3) . . ? F16 P1 F12 87.3(4) . . ? F15' P1 F11 82.8(3) . . ? F14' P1 F11 87.7(4) . . ? F13 P1 F11 81.7(4) . . ? F14 P1 F11 87.0(4) . . ? F16' P1 F11 93.5(3) . . ? F16 P1 F11 91.3(4) . . ? F12 P1 F11 178.4(2) . . ? F15' P1 F13' 175.9(5) . . ? F14' P1 F13' 91.8(5) . . ? F16' P1 F13' 86.8(5) . . ? F12 P1 F13' 80.7(3) . . ? F11 P1 F13' 99.6(3) . . ? F13 P1 F15 175.1(4) . . ? F14 P1 F15 87.0(4) . . ? F16 P1 F15 87.6(4) . . ? F12 P1 F15 87.3(3) . . ? F11 P1 F15 93.5(3) . . ? F24' P2 F23' 90.7(6) . . ? F23 P2 F26 92.5(4) . . ? F24' P2 F25' 95.1(6) . . ? F23' P2 F25' 173.3(5) . . ? F24' P2 F22 84.7(3) . . ? F23 P2 F22 89.6(3) . . ? F23' P2 F22 88.2(4) . . ? F26 P2 F22 88.6(2) . . ? F25' P2 F22 88.9(4) . . ? F24' P2 F21 94.6(3) . . ? F23 P2 F21 91.5(3) . . ? F23' P2 F21 92.7(4) . . ? F26 P2 F21 91.3(2) . . ? F25' P2 F21 90.2(4) . . ? F22 P2 F21 178.88(19) . . ? F23 P2 F25 174.7(4) . . ? F26 P2 F25 92.4(4) . . ? F22 P2 F25 92.7(2) . . ? F21 P2 F25 86.2(2) . . ? F23 P2 F24 88.8(4) . . ? F26 P2 F24 178.2(3) . . ? F22 P2 F24 92.71(19) . . ? F21 P2 F24 87.39(18) . . ? F25 P2 F24 86.3(3) . . ? F24' P2 F26' 177.2(5) . . ? F23' P2 F26' 87.6(5) . . ? F25' P2 F26' 86.5(6) . . ? F22 P2 F26' 93.0(3) . . ? F21 P2 F26' 87.6(3) . . ? F34' P3 F33' 94.2(5) . . ? F34' P3 F32' 94.1(7) . . ? F33' P3 F32' 95.8(7) . . ? F34 P3 F32 93.5(4) . . ? F32 P3 F33 89.6(3) . . ? F34' P3 F31' 92.2(6) . . ? F33' P3 F31' 90.9(6) . . ? F32' P3 F31' 170.4(7) . . ? F34 P3 F31 88.9(4) . . ? F32 P3 F31 177.5(3) . . ? F33 P3 F31 91.2(3) . . ? F34 P3 F35 89.8(3) . . ? F32 P3 F35 90.9(3) . . ? F33 P3 F35 176.5(3) . . ? F31 P3 F35 88.2(3) . . ? F34' P3 F36' 175.2(5) . . ? F33' P3 F36' 90.6(5) . . ? F32' P3 F36' 85.0(6) . . ? F31' P3 F36' 88.1(6) . . ? F34 P3 F36 175.0(4) . . ? F32 P3 F36 90.6(4) . . ? F33 P3 F36 89.3(4) . . ? F31 P3 F36 87.0(3) . . ? F35 P3 F36 87.2(3) . . ? F34' P3 F35' 91.1(5) . . ? F33' P3 F35' 173.2(6) . . ? F32' P3 F35' 88.1(6) . . ? F31' P3 F35' 84.6(5) . . ? F36' P3 F35' 84.2(5) . . ? #===END data_p2moc _database_code_depnum_ccdc_archive 'CCDC 637853' _audit_creation_date 2007-02-21T13:04:34-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C8 H12 Ag Cl N4 O4' _chemical_formula_moiety 'C8 H12 Ag N4, Cl O4' _chemical_formula_weight 371.54 _chemical_absolute_configuration ad #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P n a 21' _symmetry_space_group_name_Hall P_2c_-2n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' '-x+1/2, y+1/2, z+1/2' 'x+1/2, -y+1/2, z' _cell_length_a 24.2440(10) _cell_length_b 8.5678(5) _cell_length_c 20.6540(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 4290.2(4) _cell_formula_units_Z 12 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8192 _cell_measurement_theta_min 2.43 _cell_measurement_theta_max 34.8 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.32 _exptl_crystal_density_diffrn 1.726 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2208 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.607 _diffrn_measurement_device_type ; Bruker SMART CCD diffractometer ; _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS; Sheldrick, 1996 ; _exptl_absorpt_correction_T_min .617 _exptl_absorpt_correction_T_max .862 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_reflns_av_R_equivalents 0.036 _diffrn_reflns_av_unetI/netI 0.0222 _diffrn_reflns_number 78407 _diffrn_reflns_limit_h_min -39 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 35.05 _diffrn_reflns_theta_full 35.05 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 18896 _reflns_number_gt 16029 _reflns_threshold_expression I>2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_cell_refinement 'Siemens SAINT (Siemens, 1995)' _computing_data_reduction xtal_ADDREF_SORTRF _computing_structure_solution xtal _computing_molecular_graphics xtal _computing_publication_material WinGX _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^)+(0.0322P)^2^+0.7729P] 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_number_reflns 18896 _refine_ls_number_parameters 499 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0432 _refine_ls_R_factor_gt 0.0325 _refine_ls_wR_factor_ref 0.0685 _refine_ls_wR_factor_gt 0.0656 _refine_ls_goodness_of_fit_ref 1.031 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.017 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.273(13) _refine_diff_density_max 0.442 _refine_diff_density_min -0.816 _refine_diff_density_rms 0.075 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.785009(7) 0.80699(2) 1.000005(10) 0.03414(4) Uani 1 1 d . . . N111 N 0.78534(8) 1.0671(2) 0.99794(13) 0.0338(4) Uani 1 1 d . . . C111 C 0.78638(8) 1.1999(3) 0.99711(14) 0.0266(4) Uani 1 1 d . . . C112 C 0.78726(10) 1.3694(3) 0.99625(16) 0.0359(5) Uani 1 1 d . . . H11A H 0.763 1.4075 0.9617 0.054 Uiso 1 1 calc R . . H11B H 0.825 1.4057 0.9884 0.054 Uiso 1 1 calc R . . H11C H 0.7743 1.4093 1.0381 0.054 Uiso 1 1 calc R . . N121 N 0.74435(10) 0.7024(3) 1.08706(11) 0.0438(5) Uani 1 1 d . . . C121 C 0.72264(10) 0.6778(3) 1.13437(13) 0.0329(5) Uani 1 1 d . . . C122 C 0.69557(11) 0.6469(4) 1.19485(13) 0.0423(6) Uani 1 1 d . . . H12A H 0.7199 0.5848 1.2226 0.063 Uiso 1 1 calc R . . H12B H 0.6614 0.5889 1.1868 0.063 Uiso 1 1 calc R . . H12C H 0.6869 0.7458 1.2164 0.063 Uiso 1 1 calc R . . N131 N 0.74463(10) 0.7103(3) 0.90953(12) 0.0436(5) Uani 1 1 d . . . C131 C 0.72481(10) 0.6910(3) 0.86128(12) 0.0325(5) Uani 1 1 d . . . C132 C 0.69891(12) 0.6675(4) 0.79900(12) 0.0453(7) Uani 1 1 d . . . H13A H 0.6604 0.7015 0.8011 0.068 Uiso 1 1 calc R . . H13B H 0.7003 0.5565 0.7876 0.068 Uiso 1 1 calc R . . H13C H 0.7185 0.7284 0.7661 0.068 Uiso 1 1 calc R . . N141 N 0.87358(8) 0.7159(2) 0.99615(13) 0.0409(4) Uani 1 1 d . . . C141 C 0.91983(8) 0.6996(2) 0.99228(12) 0.0315(4) Uani 1 1 d . . . C142 C 0.97888(10) 0.6787(3) 0.98564(15) 0.0459(6) Uani 1 1 d . . . H14A H 0.9877 0.6523 0.9406 0.069 Uiso 1 1 calc R . . H14B H 0.9911 0.594 1.0141 0.069 Uiso 1 1 calc R . . H14C H 0.9978 0.7755 0.9977 0.069 Uiso 1 1 calc R . . Ag2 Ag 0.456751(8) 0.24774(2) 0.661112(11) 0.03513(4) Uani 1 1 d . . . N211 N 0.54365(8) 0.1480(2) 0.65802(12) 0.0361(4) Uani 1 1 d . . . C211 C 0.58406(8) 0.0822(2) 0.66127(11) 0.0285(4) Uani 1 1 d . . . C212 C 0.63588(10) -0.0029(3) 0.66470(15) 0.0374(6) Uani 1 1 d . . . H21A H 0.6635 0.0494 0.6377 0.056 Uiso 1 1 calc R . . H21B H 0.6303 -0.1097 0.6491 0.056 Uiso 1 1 calc R . . H21C H 0.6488 -0.0056 0.7097 0.056 Uiso 1 1 calc R . . N221 N 0.45157(9) 0.5076(2) 0.65876(13) 0.0394(5) Uani 1 1 d . . . C221 C 0.45328(9) 0.6396(2) 0.65835(14) 0.0288(4) Uani 1 1 d . . . C222 C 0.45671(11) 0.8081(2) 0.65827(16) 0.0362(5) Uani 1 1 d . . . H22A H 0.465 0.8451 0.7021 0.054 Uiso 1 1 calc R . . H22B H 0.4214 0.852 0.644 0.054 Uiso 1 1 calc R . . H22C H 0.486 0.8415 0.6287 0.054 Uiso 1 1 calc R . . N231 N 0.40486(8) 0.1505(3) 0.57770(11) 0.0352(4) Uani 1 1 d . . . C231 C 0.38519(9) 0.0834(3) 0.53669(11) 0.0291(4) Uani 1 1 d . . . C232 C 0.36106(11) -0.0034(3) 0.48337(15) 0.0442(7) Uani 1 1 d . . . H23A H 0.3881 -0.0783 0.4667 0.066 Uiso 1 1 calc R . . H23B H 0.3505 0.0691 0.4488 0.066 Uiso 1 1 calc R . . H23C H 0.3283 -0.0595 0.4986 0.066 Uiso 1 1 calc R . . N241 N 0.41802(9) 0.1428(3) 0.75277(10) 0.0388(5) Uani 1 1 d . . . C241 C 0.39309(9) 0.0736(3) 0.78964(11) 0.0298(4) Uani 1 1 d . . . C242 C 0.36160(13) -0.0174(3) 0.83478(14) 0.0413(6) Uani 1 1 d . . . H24A H 0.355 -0.1215 0.8166 0.062 Uiso 1 1 calc R . . H24B H 0.3262 0.0342 0.843 0.062 Uiso 1 1 calc R . . H24C H 0.3821 -0.0272 0.8755 0.062 Uiso 1 1 calc R . . Ag3 Ag 0.538690(8) 0.71885(2) 0.814273(9) 0.03364(4) Uani 1 1 d . . . N311 N 0.58545(9) 0.6256(2) 0.90386(10) 0.0337(4) Uani 1 1 d . . . C311 C 0.60215(9) 0.5602(3) 0.94715(11) 0.0272(4) Uani 1 1 d . . . C312 C 0.62300(12) 0.4758(3) 1.00248(13) 0.0412(6) Uani 1 1 d . . . H31A H 0.5967 0.3939 1.0146 0.062 Uiso 1 1 calc R . . H31B H 0.6279 0.5479 1.0389 0.062 Uiso 1 1 calc R . . H31C H 0.6586 0.4282 0.9915 0.062 Uiso 1 1 calc R . . N321 N 0.54092(11) 0.9809(3) 0.82250(13) 0.0443(6) Uani 1 1 d . . . C321 C 0.54028(10) 1.1121(3) 0.82571(12) 0.0317(5) Uani 1 1 d . . . C322 C 0.53864(12) 1.2809(3) 0.82919(13) 0.0376(6) Uani 1 1 d . . . H32A H 0.5764 1.3221 0.8287 0.056 Uiso 1 1 calc R . . H32B H 0.5202 1.3129 0.8693 0.056 Uiso 1 1 calc R . . H32C H 0.5182 1.322 0.7919 0.056 Uiso 1 1 calc R . . N331 N 0.57699(8) 0.6164(3) 0.72420(10) 0.0342(4) Uani 1 1 d . . . C331 C 0.60298(9) 0.5604(3) 0.68463(11) 0.0277(4) Uani 1 1 d . . . C332 C 0.63748(12) 0.4906(3) 0.63497(13) 0.0383(6) Uani 1 1 d . . . H33A H 0.6678 0.5619 0.6243 0.057 Uiso 1 1 calc R . . H33B H 0.6153 0.4711 0.5961 0.057 Uiso 1 1 calc R . . H33C H 0.6526 0.3918 0.651 0.057 Uiso 1 1 calc R . . N341 N 0.45063(9) 0.6291(3) 0.82784(10) 0.0418(5) Uani 1 1 d . . . C341 C 0.41015(10) 0.5690(3) 0.83875(11) 0.0311(4) Uani 1 1 d . . . C342 C 0.35843(13) 0.4922(3) 0.85356(16) 0.0454(7) Uani 1 1 d . . . H34A H 0.3563 0.3932 0.8299 0.068 Uiso 1 1 calc R . . H34B H 0.3277 0.5596 0.8407 0.068 Uiso 1 1 calc R . . H34C H 0.3563 0.4717 0.9002 0.068 Uiso 1 1 calc R . . Cl1 Cl 0.95543(2) 0.23310(7) 0.99483(3) 0.03416(13) Uani 1 1 d . . . O11 O 0.92857(12) 0.2970(4) 0.93922(13) 0.0679(8) Uani 1 1 d . . . O12 O 1.01186(8) 0.2805(3) 0.99481(14) 0.0635(6) Uani 1 1 d . . . O13 O 0.92911(11) 0.2924(3) 1.05186(12) 0.0597(6) Uani 1 1 d . . . O14 O 0.95175(13) 0.0691(3) 0.99290(18) 0.0839(8) Uani 1 1 d . . . Cl2 Cl 0.70131(3) 0.21916(7) 0.82951(3) 0.02959(10) Uani 1 1 d . . . O21 O 0.70416(14) 0.0540(3) 0.82855(14) 0.0738(9) Uani 1 1 d . . . O22 O 0.75602(10) 0.2836(3) 0.83515(11) 0.0569(6) Uani 1 1 d . . . O23 O 0.66952(11) 0.2712(3) 0.88410(11) 0.0544(6) Uani 1 1 d . . . O24 O 0.67688(11) 0.2729(3) 0.77058(11) 0.0524(6) Uani 1 1 d . . . Cl3 Cl 0.79489(2) 0.71112(6) 0.65821(3) 0.02935(10) Uani 1 1 d . . . O31 O 0.78717(11) 0.5473(3) 0.66102(18) 0.0753(8) Uani 1 1 d . . . O32 O 0.74248(8) 0.7868(2) 0.65379(10) 0.0456(4) Uani 1 1 d . . . O33 O 0.82696(10) 0.7529(3) 0.60288(11) 0.0618(7) Uani 1 1 d . . . O34 O 0.82306(11) 0.7599(3) 0.71590(11) 0.0546(6) 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 0.03814(8) 0.02703(8) 0.03725(9) -0.00031(7) -0.00613(7) -0.00092(6) N111 0.0414(9) 0.0255(9) 0.0345(9) 0.0001(9) -0.0018(9) 0.0005(7) C111 0.0286(8) 0.0273(9) 0.0240(9) -0.0019(9) -0.0003(8) -0.0020(7) C112 0.0506(12) 0.0219(9) 0.0350(12) 0.0031(11) 0.0034(11) 0.0012(9) N121 0.0539(14) 0.0336(11) 0.0439(12) 0.0033(9) 0.0107(10) 0.0032(10) C121 0.0304(11) 0.0292(11) 0.0391(12) -0.0061(9) -0.0012(9) 0.0048(9) C122 0.0345(12) 0.0565(16) 0.0360(12) -0.0069(11) 0.0047(10) 0.0028(12) N131 0.0528(14) 0.0350(11) 0.0430(11) -0.0062(9) -0.0175(10) 0.0005(10) C131 0.0298(11) 0.0337(12) 0.0339(11) -0.0002(9) -0.0028(9) -0.0002(9) C132 0.0429(14) 0.0645(19) 0.0285(12) 0.0018(11) -0.0050(10) -0.0128(13) N141 0.0348(9) 0.0346(10) 0.0532(13) -0.0055(10) -0.0042(10) 0.0015(7) C141 0.0325(9) 0.0318(10) 0.0301(10) 0.0004(9) -0.0021(9) -0.0037(8) C142 0.0302(11) 0.0609(17) 0.0465(15) 0.0078(14) 0.0034(11) -0.0017(11) Ag2 0.03837(8) 0.02832(7) 0.03869(9) 0.00019(7) 0.00118(9) 0.00214(7) N211 0.0313(8) 0.0383(9) 0.0385(10) 0.0032(9) 0.0026(8) 0.0037(8) C211 0.0268(9) 0.0289(9) 0.0297(10) 0.0001(8) 0.0021(8) -0.0032(7) C212 0.0278(11) 0.0345(12) 0.0500(16) -0.0060(11) -0.0056(11) 0.0040(8) N221 0.0435(11) 0.0264(8) 0.0484(12) 0.0001(10) -0.0066(10) 0.0010(8) C221 0.0269(9) 0.0270(9) 0.0324(10) -0.0003(10) -0.0043(9) 0.0015(7) C222 0.0406(11) 0.0227(9) 0.0451(13) 0.0037(12) -0.0007(11) -0.0002(9) N231 0.0323(10) 0.0340(10) 0.0391(11) 0.0017(8) -0.0010(8) -0.0024(8) C231 0.0222(9) 0.0286(10) 0.0366(11) 0.0038(8) -0.0002(8) 0.0005(7) C232 0.0426(13) 0.0407(15) 0.0491(17) -0.0059(12) -0.0110(12) -0.0054(11) N241 0.0392(11) 0.0441(12) 0.0332(10) 0.0035(9) 0.0024(8) 0.0030(9) C241 0.0306(10) 0.0303(10) 0.0286(10) -0.0001(8) -0.0040(8) 0.0066(8) C242 0.0478(16) 0.0373(13) 0.0389(13) 0.0057(10) 0.0103(12) 0.0012(11) Ag3 0.03697(9) 0.03243(7) 0.03152(8) 0.00145(8) 0.00213(7) 0.00600(7) N311 0.0372(10) 0.0344(10) 0.0296(9) 0.0023(8) -0.0016(7) 0.0058(8) C311 0.0273(9) 0.0277(10) 0.0265(10) -0.0023(8) 0.0014(8) 0.0033(8) C312 0.0582(15) 0.0376(12) 0.0278(11) 0.0044(10) -0.0052(12) 0.0127(11) N321 0.0567(14) 0.0296(10) 0.0464(14) 0.0057(10) -0.0014(11) 0.0046(9) C321 0.0332(11) 0.0293(9) 0.0327(13) -0.0004(9) -0.0014(9) 0.0018(9) C322 0.0441(14) 0.0258(10) 0.0428(16) -0.0048(10) -0.0008(10) -0.0006(9) N331 0.0326(9) 0.0432(11) 0.0269(9) -0.0037(8) -0.0010(7) 0.0001(8) C331 0.0281(10) 0.0281(10) 0.0270(10) -0.0001(8) -0.0017(8) -0.0039(8) C332 0.0460(15) 0.0358(13) 0.0332(12) -0.0053(10) 0.0080(10) 0.0015(11) N341 0.0331(11) 0.0502(12) 0.0420(13) 0.0004(9) 0.0038(8) 0.0011(9) C341 0.0323(11) 0.0328(11) 0.0282(10) -0.0043(8) 0.0001(8) 0.0042(8) C342 0.0436(15) 0.0426(15) 0.0499(16) -0.0088(12) 0.0104(13) -0.0082(12) Cl1 0.0359(2) 0.0326(3) 0.0339(3) -0.0023(3) 0.0001(3) 0.00187(18) O11 0.0576(15) 0.098(2) 0.0482(13) 0.0158(13) -0.0120(11) 0.0078(14) O12 0.0366(9) 0.0953(17) 0.0586(14) 0.0020(15) 0.0020(11) -0.0062(10) O13 0.0547(14) 0.0768(17) 0.0477(13) -0.0191(12) 0.0140(11) -0.0015(12) O14 0.116(2) 0.0361(13) 0.099(2) -0.0077(15) -0.004(2) 0.0026(12) Cl2 0.0353(3) 0.0251(2) 0.0284(2) -0.0015(2) 0.00222(19) 0.0014(2) O21 0.112(2) 0.0279(10) 0.082(2) -0.0029(12) 0.0005(15) 0.0057(12) O22 0.0394(12) 0.0755(16) 0.0556(13) -0.0104(11) 0.0011(9) -0.0128(11) O23 0.0582(14) 0.0683(15) 0.0366(10) -0.0060(10) 0.0167(10) 0.0139(11) O24 0.0653(15) 0.0579(14) 0.0341(10) 0.0053(9) -0.0111(10) 0.0014(11) Cl3 0.0294(2) 0.0309(2) 0.0277(2) 0.0044(3) 0.0037(2) 0.00044(18) O31 0.0777(18) 0.0314(10) 0.117(2) 0.0073(15) 0.0019(17) 0.0006(10) O32 0.0373(9) 0.0602(12) 0.0394(9) 0.0051(10) -0.0031(8) 0.0158(8) O33 0.0430(12) 0.107(2) 0.0354(10) 0.0184(11) 0.0120(9) -0.0079(12) O34 0.0595(14) 0.0669(16) 0.0374(10) 0.0018(10) -0.0155(10) 0.0020(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 N111 2.2290(19) . ? Ag1 N121 2.238(2) . ? Ag1 N131 2.266(2) . ? Ag1 N141 2.2862(19) . ? N111 C111 1.138(3) . ? C111 C112 1.453(3) . ? C112 H11A 0.98 . ? C112 H11B 0.98 . ? C112 H11C 0.98 . ? N121 C121 1.130(3) . ? C121 C122 1.436(4) . ? C122 H12A 0.98 . ? C122 H12B 0.98 . ? C122 H12C 0.98 . ? N131 C131 1.119(3) . ? C131 C132 1.445(4) . ? C132 H13A 0.98 . ? C132 H13B 0.98 . ? C132 H13C 0.98 . ? N141 C141 1.133(3) . ? C141 C142 1.449(3) . ? C142 H14A 0.98 . ? C142 H14B 0.98 . ? C142 H14C 0.98 . ? Ag2 N221 2.230(2) . ? Ag2 N211 2.2746(19) . ? Ag2 N231 2.290(2) . ? Ag2 N241 2.297(2) . ? N211 C211 1.132(3) . ? C211 C212 1.454(3) . ? C212 H21A 0.98 . ? C212 H21B 0.98 . ? C212 H21C 0.98 . ? N221 C221 1.132(3) . ? C221 C222 1.446(3) . ? C222 H22A 0.98 . ? C222 H22B 0.98 . ? C222 H22C 0.98 . ? N231 C231 1.130(3) . ? C231 C232 1.452(4) . ? C232 H23A 0.98 . ? C232 H23B 0.98 . ? C232 H23C 0.98 . ? N241 C241 1.138(3) . ? C241 C242 1.436(4) . ? C242 H24A 0.98 . ? C242 H24B 0.98 . ? C242 H24C 0.98 . ? Ag3 N321 2.252(2) . ? Ag3 N331 2.257(2) . ? Ag3 N341 2.287(2) . ? Ag3 N311 2.312(2) . ? N311 C311 1.130(3) . ? C311 C312 1.444(3) . ? C312 H31A 0.98 . ? C312 H31B 0.98 . ? C312 H31C 0.98 . ? N321 C321 1.126(3) . ? C321 C322 1.449(3) . ? C322 H32A 0.98 . ? C322 H32B 0.98 . ? C322 H32C 0.98 . ? N331 C331 1.138(3) . ? C331 C332 1.452(3) . ? C332 H33A 0.98 . ? C332 H33B 0.98 . ? C332 H33C 0.98 . ? N341 C341 1.131(3) . ? C341 C342 1.449(4) . ? C342 H34A 0.98 . ? C342 H34B 0.98 . ? C342 H34C 0.98 . ? Cl1 O14 1.409(2) . ? Cl1 O12 1.427(2) . ? Cl1 O11 1.429(2) . ? Cl1 O13 1.433(2) . ? Cl2 O21 1.416(2) . ? Cl2 O24 1.430(2) . ? Cl2 O23 1.437(2) . ? Cl2 O22 1.441(2) . ? Cl3 O31 1.417(2) . ? Cl3 O33 1.428(2) . ? Cl3 O32 1.4295(18) . ? Cl3 O34 1.436(2) . ? 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 N111 Ag1 N121 114.66(9) . . ? N111 Ag1 N131 110.55(9) . . ? N121 Ag1 N131 109.02(8) . . ? N111 Ag1 N141 109.71(7) . . ? N121 Ag1 N141 107.77(9) . . ? N131 Ag1 N141 104.61(9) . . ? C111 N111 Ag1 178.9(2) . . ? N111 C111 C112 179.5(3) . . ? C111 C112 H11A 109.5 . . ? C111 C112 H11B 109.5 . . ? H11A C112 H11B 109.5 . . ? C111 C112 H11C 109.5 . . ? H11A C112 H11C 109.5 . . ? H11B C112 H11C 109.5 . . ? C121 N121 Ag1 167.2(2) . . ? N121 C121 C122 179.4(3) . . ? C121 C122 H12A 109.5 . . ? C121 C122 H12B 109.5 . . ? H12A C122 H12B 109.5 . . ? C121 C122 H12C 109.5 . . ? H12A C122 H12C 109.5 . . ? H12B C122 H12C 109.5 . . ? C131 N131 Ag1 167.0(2) . . ? N131 C131 C132 179.4(3) . . ? C131 C132 H13A 109.5 . . ? C131 C132 H13B 109.5 . . ? H13A C132 H13B 109.5 . . ? C131 C132 H13C 109.5 . . ? H13A C132 H13C 109.5 . . ? H13B C132 H13C 109.5 . . ? C141 N141 Ag1 166.98(18) . . ? N141 C141 C142 178.6(3) . . ? C141 C142 H14A 109.5 . . ? C141 C142 H14B 109.5 . . ? H14A C142 H14B 109.5 . . ? C141 C142 H14C 109.5 . . ? H14A C142 H14C 109.5 . . ? H14B C142 H14C 109.5 . . ? N221 Ag2 N211 115.26(8) . . ? N221 Ag2 N231 108.41(8) . . ? N211 Ag2 N231 110.54(8) . . ? N221 Ag2 N241 112.70(9) . . ? N211 Ag2 N241 104.75(8) . . ? N231 Ag2 N241 104.65(8) . . ? C211 N211 Ag2 170.73(19) . . ? N211 C211 C212 179.4(3) . . ? C211 C212 H21A 109.5 . . ? C211 C212 H21B 109.5 . . ? H21A C212 H21B 109.5 . . ? C211 C212 H21C 109.5 . . ? H21A C212 H21C 109.5 . . ? H21B C212 H21C 109.5 . . ? C221 N221 Ag2 174.6(2) . . ? N221 C221 C222 178.8(3) . . ? C221 C222 H22A 109.5 . . ? C221 C222 H22B 109.5 . . ? H22A C222 H22B 109.5 . . ? C221 C222 H22C 109.5 . . ? H22A C222 H22C 109.5 . . ? H22B C222 H22C 109.5 . . ? C231 N231 Ag2 168.9(2) . . ? N231 C231 C232 178.8(3) . . ? C231 C232 H23A 109.5 . . ? C231 C232 H23B 109.5 . . ? H23A C232 H23B 109.5 . . ? C231 C232 H23C 109.5 . . ? H23A C232 H23C 109.5 . . ? H23B C232 H23C 109.5 . . ? C241 N241 Ag2 166.5(2) . . ? N241 C241 C242 178.3(3) . . ? C241 C242 H24A 109.5 . . ? C241 C242 H24B 109.5 . . ? H24A C242 H24B 109.5 . . ? C241 C242 H24C 109.5 . . ? H24A C242 H24C 109.5 . . ? H24B C242 H24C 109.5 . . ? N321 Ag3 N331 116.10(9) . . ? N321 Ag3 N341 110.39(9) . . ? N331 Ag3 N341 110.76(8) . . ? N321 Ag3 N311 105.79(8) . . ? N331 Ag3 N311 108.89(7) . . ? N341 Ag3 N311 104.09(8) . . ? C311 N311 Ag3 168.5(2) . . ? N311 C311 C312 179.5(3) . . ? C311 C312 H31A 109.5 . . ? C311 C312 H31B 109.5 . . ? H31A C312 H31B 109.5 . . ? C311 C312 H31C 109.5 . . ? H31A C312 H31C 109.5 . . ? H31B C312 H31C 109.5 . . ? C321 N321 Ag3 177.6(2) . . ? N321 C321 C322 179.1(3) . . ? C321 C322 H32A 109.5 . . ? C321 C322 H32B 109.5 . . ? H32A C322 H32B 109.5 . . ? C321 C322 H32C 109.5 . . ? H32A C322 H32C 109.5 . . ? H32B C322 H32C 109.5 . . ? C331 N331 Ag3 169.65(19) . . ? N331 C331 C332 178.4(3) . . ? C331 C332 H33A 109.5 . . ? C331 C332 H33B 109.5 . . ? H33A C332 H33B 109.5 . . ? C331 C332 H33C 109.5 . . ? H33A C332 H33C 109.5 . . ? H33B C332 H33C 109.5 . . ? C341 N341 Ag3 171.1(2) . . ? N341 C341 C342 179.3(3) . . ? C341 C342 H34A 109.5 . . ? C341 C342 H34B 109.5 . . ? H34A C342 H34B 109.5 . . ? C341 C342 H34C 109.5 . . ? H34A C342 H34C 109.5 . . ? H34B C342 H34C 109.5 . . ? O14 Cl1 O12 110.16(17) . . ? O14 Cl1 O11 109.29(19) . . ? O12 Cl1 O11 109.12(17) . . ? O14 Cl1 O13 110.40(18) . . ? O12 Cl1 O13 109.05(16) . . ? O11 Cl1 O13 108.79(15) . . ? O21 Cl2 O24 109.25(16) . . ? O21 Cl2 O23 110.32(17) . . ? O24 Cl2 O23 110.24(15) . . ? O21 Cl2 O22 109.79(18) . . ? O24 Cl2 O22 109.07(15) . . ? O23 Cl2 O22 108.15(15) . . ? O31 Cl3 O33 110.67(19) . . ? O31 Cl3 O32 109.55(14) . . ? O33 Cl3 O32 108.60(14) . . ? O31 Cl3 O34 108.50(18) . . ? O33 Cl3 O34 109.41(14) . . ? O32 Cl3 O34 110.10(14) . . ? #===END data_lfl12jp _database_code_depnum_ccdc_archive 'CCDC 883470' #TrackingRef 'web_deposit_cif_file_0_BrianSkelton_1337769688.lfl12jp.cif' _audit_creation_date 2012-04-18T12:03:56-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_sum 'C10 H15 Cu F6 N5 P' _chemical_formula_moiety 'C8 H12 Cu N4, F6 P, C2 H3 N' _chemical_formula_weight 413.78 _chemical_absolute_configuration unk #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _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+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 8.57130(10) _cell_length_b 21.9018(3) _cell_length_c 27.8052(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 5219.78(13) _cell_formula_units_Z 12 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 16514 _cell_measurement_theta_min 2.9368 _cell_measurement_theta_max 32.8039 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.06 _exptl_crystal_density_diffrn 1.58 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2496 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.407 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _exptl_absorpt_correction_T_min 0.76243 _exptl_absorpt_correction_T_max 1 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0265 _diffrn_reflns_av_unetI/netI 0.0356 _diffrn_reflns_number 47834 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 33 _diffrn_reflns_limit_l_min -42 _diffrn_reflns_limit_l_max 42 _diffrn_reflns_theta_min 2.94 _diffrn_reflns_theta_max 32.88 _diffrn_reflns_theta_full 31.5 _diffrn_measured_fraction_theta_full 0.992 _diffrn_measured_fraction_theta_max 0.938 _reflns_number_total 17660 _reflns_number_gt 14497 _reflns_threshold_expression I>2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.21 (release 20-01-2012 CrysAlis171 .NET) (compiled Jan 23 2012,18:06:46) ; _computing_molecular_graphics 'OrtepII (Johnson, C. K. (1976)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' #----------------------------------------------------------------------------# # STRUCTURE SOLUTION #----------------------------------------------------------------------------# _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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^ > 2\s(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. All hexafluorophosphate anions were modelled as being rotationally disordered about one F-P-F vector. The site occupancy factors refined to 0.690(10), 0.803(9) and 0.760(9) and their respective complements. Electron density of the methyl hydrogen atoms were observed in later difference maps with the hydrogen atoms added and refined by use of a riding model with isotropic displacement parameters based on those of the parent atoms. ; _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^)+(0.0354P)^2^+1.2519P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 17660 _refine_ls_number_parameters 749 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.053 _refine_ls_R_factor_gt 0.0366 _refine_ls_wR_factor_ref 0.0841 _refine_ls_wR_factor_gt 0.0771 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0 _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.404(6) _refine_diff_density_max 0.491 _refine_diff_density_min -0.367 _refine_diff_density_rms 0.06 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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' 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' 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 0.99295(3) 0.905701(11) 0.774216(9) 0.02810(6) Uani 1 1 d . . . N11 N 0.9045(2) 0.97890(8) 0.74012(7) 0.0312(4) Uani 1 1 d . . . N12 N 0.9015(2) 0.90760(8) 0.84010(6) 0.0283(4) Uani 1 1 d . . . N13 N 1.2220(2) 0.90590(8) 0.77387(7) 0.0305(4) Uani 1 1 d . . . N14 N 0.8972(2) 0.83177(8) 0.74280(7) 0.0292(4) Uani 1 1 d . . . C11 C 0.8369(3) 1.01643(9) 0.72102(9) 0.0299(4) Uani 1 1 d . . . C12 C 0.7497(3) 1.06394(11) 0.69649(12) 0.0492(8) Uani 1 1 d . . . H12A H 0.8223 1.0917 0.6803 0.074 Uiso 1 1 calc R . . H12B H 0.6876 1.0868 0.72 0.074 Uiso 1 1 calc R . . H12C H 0.6801 1.0454 0.6726 0.074 Uiso 1 1 calc R . . C13 C 0.8318(2) 0.90985(9) 0.87474(7) 0.0250(4) Uani 1 1 d . . . C14 C 0.7408(3) 0.91229(13) 0.91849(9) 0.0380(5) Uani 1 1 d . . . H14A H 0.6749 0.9489 0.9182 0.057 Uiso 1 1 calc R . . H14B H 0.8109 0.9138 0.9463 0.057 Uiso 1 1 calc R . . H14C H 0.6747 0.8759 0.9207 0.057 Uiso 1 1 calc R . . C15 C 1.3543(3) 0.90565(10) 0.77698(8) 0.0277(4) Uani 1 1 d . . . C16 C 1.5225(3) 0.90473(11) 0.78205(9) 0.0365(5) Uani 1 1 d . . . H16A H 1.5582 0.9441 0.7947 0.055 Uiso 1 1 calc R . . H16B H 1.5705 0.8974 0.7506 0.055 Uiso 1 1 calc R . . H16C H 1.5526 0.8721 0.8043 0.055 Uiso 1 1 calc R . . C17 C 0.8219(2) 0.79615(9) 0.72454(8) 0.0260(4) Uani 1 1 d . . . C18 C 0.7239(3) 0.75122(11) 0.70060(9) 0.0363(5) Uani 1 1 d . . . H18A H 0.6411 0.7722 0.6827 0.054 Uiso 1 1 calc R . . H18B H 0.6772 0.7241 0.7247 0.054 Uiso 1 1 calc R . . H18C H 0.7874 0.7271 0.6783 0.054 Uiso 1 1 calc R . . Cu2 Cu 1.02273(3) 0.743165(11) 0.571690(9) 0.02808(6) Uani 1 1 d . . . N21 N 1.1194(2) 0.67280(8) 0.53646(7) 0.0299(4) Uani 1 1 d . . . N22 N 1.1061(2) 0.81911(8) 0.53955(7) 0.0295(4) Uani 1 1 d . . . N23 N 1.1081(2) 0.74267(8) 0.63861(6) 0.0296(4) Uani 1 1 d . . . N24 N 0.7928(2) 0.74061(8) 0.56918(7) 0.0311(4) Uani 1 1 d . . . C21 C 1.1843(3) 0.63285(9) 0.51992(8) 0.0268(4) Uani 1 1 d . . . C22 C 1.2686(3) 0.58152(12) 0.49959(10) 0.0400(6) Uani 1 1 d . . . H22A H 1.3459 0.5669 0.5229 0.06 Uiso 1 1 calc R . . H22B H 1.3217 0.5945 0.4701 0.06 Uiso 1 1 calc R . . H22C H 1.1951 0.5486 0.4921 0.06 Uiso 1 1 calc R . . C23 C 1.1626(3) 0.85858(9) 0.52034(8) 0.0278(4) Uani 1 1 d . . . C24 C 1.2358(3) 0.90915(12) 0.49435(10) 0.0406(6) Uani 1 1 d . . . H24A H 1.3486 0.9087 0.5002 0.061 Uiso 1 1 calc R . . H24B H 1.1919 0.9479 0.5056 0.061 Uiso 1 1 calc R . . H24C H 1.216 0.9047 0.4598 0.061 Uiso 1 1 calc R . . C25 C 1.1690(2) 0.74141(9) 0.67483(8) 0.0273(4) Uani 1 1 d . . . C26 C 1.2464(3) 0.74066(13) 0.72108(9) 0.0403(6) Uani 1 1 d . . . H26A H 1.2552 0.7825 0.7333 0.061 Uiso 1 1 calc R . . H26B H 1.3509 0.723 0.7175 0.061 Uiso 1 1 calc R . . H26C H 1.1856 0.716 0.7437 0.061 Uiso 1 1 calc R . . C27 C 0.6600(2) 0.74136(9) 0.56881(7) 0.0268(4) Uani 1 1 d . . . C28 C 0.4903(3) 0.74224(9) 0.56858(8) 0.0329(4) Uani 1 1 d . . . H28A H 0.4507 0.702 0.5779 0.049 Uiso 1 1 calc R . . H28B H 0.453 0.7524 0.5362 0.049 Uiso 1 1 calc R . . H28C H 0.4529 0.773 0.5915 0.049 Uiso 1 1 calc R . . Cu3 Cu 1.01435(3) 0.578082(11) 0.947417(9) 0.03079(6) Uani 1 1 d . . . N31 N 0.9741(2) 0.65160(8) 0.90667(7) 0.0358(4) Uani 1 1 d . . . N32 N 1.2488(2) 0.57859(8) 0.95408(7) 0.0310(4) Uani 1 1 d . . . N33 N 0.9678(3) 0.50196(8) 0.91040(7) 0.0354(4) Uani 1 1 d . . . N34 N 0.9083(2) 0.58176(9) 1.01092(7) 0.0337(4) Uani 1 1 d . . . C31 C 0.9717(3) 0.69397(10) 0.88303(8) 0.0315(4) Uani 1 1 d . . . C32 C 0.9708(3) 0.74817(10) 0.85262(8) 0.0386(5) Uani 1 1 d . . . H32A H 1.0447 0.7782 0.8654 0.058 Uiso 1 1 calc R . . H32B H 0.8658 0.7658 0.8522 0.058 Uiso 1 1 calc R . . H32C H 1.0014 0.7369 0.8198 0.058 Uiso 1 1 calc R . . C33 C 1.3802(3) 0.57636(9) 0.95070(8) 0.0288(4) Uani 1 1 d . . . C34 C 1.5489(3) 0.57287(12) 0.94644(10) 0.0420(6) Uani 1 1 d . . . H34A H 1.5938 0.5605 0.9774 0.063 Uiso 1 1 calc R . . H34B H 1.5902 0.613 0.9373 0.063 Uiso 1 1 calc R . . H34C H 1.5766 0.5428 0.9218 0.063 Uiso 1 1 calc R . . C35 C 0.9591(3) 0.45936(10) 0.88736(8) 0.0315(5) Uani 1 1 d . . . C36 C 0.9496(3) 0.40442(10) 0.85815(9) 0.0395(6) Uani 1 1 d . . . H36A H 1.0549 0.389 0.8519 0.059 Uiso 1 1 calc R . . H36B H 0.8982 0.414 0.8276 0.059 Uiso 1 1 calc R . . H36C H 0.8891 0.3733 0.8753 0.059 Uiso 1 1 calc R . . C37 C 0.8537(2) 0.58521(10) 1.04802(8) 0.0295(4) Uani 1 1 d . . . C38 C 0.7875(3) 0.58952(12) 1.09595(9) 0.0368(5) Uani 1 1 d . . . H38A H 0.8177 0.5535 1.1147 0.055 Uiso 1 1 calc R . . H38B H 0.6735 0.5915 1.0937 0.055 Uiso 1 1 calc R . . H38C H 0.8266 0.6264 1.1118 0.055 Uiso 1 1 calc R . . N41 N 0.5320(3) 0.67654(10) 1.03861(9) 0.0511(6) Uani 1 1 d . . . C41 C 0.5979(3) 0.71481(12) 1.02006(9) 0.0393(5) Uani 1 1 d . . . C42 C 0.6792(4) 0.76441(16) 0.99606(12) 0.0663(10) Uani 1 1 d . . . H42A H 0.743 0.7479 0.9699 0.099 Uiso 1 1 calc R . . H42B H 0.7465 0.7855 1.0192 0.099 Uiso 1 1 calc R . . H42C H 0.6029 0.7933 0.9829 0.099 Uiso 1 1 calc R . . N51 N 0.9376(3) 0.64551(11) 0.75936(9) 0.0511(6) Uani 1 1 d . . . C51 C 0.8446(3) 0.61446(11) 0.77468(10) 0.0414(6) Uani 1 1 d . . . C52 C 0.7250(4) 0.57478(16) 0.79471(14) 0.0670(9) Uani 1 1 d . . . H52A H 0.7625 0.5571 0.825 0.101 Uiso 1 1 calc R . . H52B H 0.7018 0.5419 0.7719 0.101 Uiso 1 1 calc R . . H52C H 0.6302 0.5986 0.8008 0.101 Uiso 1 1 calc R . . N61 N 1.0115(3) 1.01697(9) 0.93326(8) 0.0471(5) Uani 1 1 d . . . C61 C 1.0123(3) 1.04194(10) 0.89729(9) 0.0378(5) Uani 1 1 d . . . C62 C 1.0129(3) 1.07362(12) 0.85160(10) 0.0506(6) Uani 1 1 d . . . H62A H 0.9061 1.0856 0.8433 0.076 Uiso 1 1 calc R . . H62B H 1.0543 1.0466 0.8266 0.076 Uiso 1 1 calc R . . H62C H 1.0786 1.1101 0.854 0.076 Uiso 1 1 calc R . . P1 P 0.48513(7) 0.57986(2) 0.65050(2) 0.02873(11) Uani 1 1 d . . . F11 F 0.3546(2) 0.62089(9) 0.62708(10) 0.0857(8) Uani 1 1 d . A . F12 F 0.6157(2) 0.53742(8) 0.67314(8) 0.0650(6) Uani 1 1 d . A . F13A F 0.4810(7) 0.6169(2) 0.69790(13) 0.107(2) Uani 0.690(10) 1 d P A 1 F14A F 0.6194(3) 0.62407(13) 0.62989(14) 0.0531(14) Uani 0.690(10) 1 d P A 1 F15A F 0.4979(5) 0.54247(18) 0.60138(12) 0.0850(15) Uani 0.690(10) 1 d P A 1 F16A F 0.3558(3) 0.53469(17) 0.66842(19) 0.067(2) Uani 0.690(10) 1 d P A 1 F13B F 0.3854(11) 0.5742(5) 0.6987(3) 0.092(5) Uani 0.310(10) 1 d P A 2 F14B F 0.5673(12) 0.6387(3) 0.6666(4) 0.092(5) Uani 0.310(10) 1 d PU A 2 F15B F 0.5780(12) 0.5831(6) 0.6034(3) 0.108(6) Uani 0.310(10) 1 d P A 2 F16B F 0.3999(14) 0.5202(3) 0.6332(5) 0.101(6) Uani 0.310(10) 1 d P A 2 P2 P 0.47916(8) 0.73700(2) 0.85623(2) 0.03079(11) Uani 1 1 d . . . F21 F 0.3511(2) 0.78011(8) 0.83206(8) 0.0635(5) Uani 1 1 d . B . F22 F 0.6093(3) 0.69653(9) 0.88083(10) 0.0825(7) Uani 1 1 d . B . F23A F 0.3856(4) 0.7403(2) 0.90527(11) 0.0919(15) Uani 0.803(9) 1 d P B 1 F24A F 0.5736(3) 0.79616(10) 0.87214(13) 0.0640(11) Uani 0.803(9) 1 d P B 1 F25A F 0.5715(4) 0.7364(2) 0.80755(10) 0.0893(14) Uani 0.803(9) 1 d P B 1 F26A F 0.3831(5) 0.67959(13) 0.8413(2) 0.0979(17) Uani 0.803(9) 1 d P B 1 F23B F 0.466(2) 0.7752(6) 0.9029(5) 0.084(7) Uani 0.197(9) 1 d PU B 2 F24B F 0.6087(11) 0.7801(6) 0.8344(7) 0.080(7) Uani 0.197(9) 1 d PU B 2 F25B F 0.490(3) 0.6963(6) 0.8091(4) 0.094(6) Uani 0.197(9) 1 d P B 2 F26B F 0.3532(13) 0.6925(6) 0.8748(6) 0.068(5) Uani 0.197(9) 1 d P B 2 P3 P 0.53132(7) 0.91104(2) 0.63189(2) 0.02850(11) Uani 1 1 d . . . F31 F 0.6290(2) 0.96556(7) 0.60874(7) 0.0513(4) Uani 1 1 d . C . F32 F 0.4361(2) 0.85600(7) 0.65529(7) 0.0541(4) Uani 1 1 d . C . F33A F 0.4299(5) 0.9567(2) 0.6607(2) 0.0744(17) Uani 0.760(9) 1 d P C 1 F34A F 0.4189(5) 0.9101(2) 0.58881(12) 0.0836(15) Uani 0.760(9) 1 d P C 1 F35A F 0.6447(5) 0.86321(11) 0.60470(17) 0.0692(13) Uani 0.760(9) 1 d P C 1 F36A F 0.6574(4) 0.9093(2) 0.67523(13) 0.0731(12) Uani 0.760(9) 1 d P C 1 F33B F 0.3731(9) 0.9430(5) 0.6073(5) 0.064(4) Uani 0.240(9) 1 d P C 2 F34B F 0.5517(17) 0.8753(4) 0.5843(3) 0.063(4) Uani 0.240(9) 1 d PU C 2 F35B F 0.6670(11) 0.8821(5) 0.6529(5) 0.063(4) Uani 0.240(9) 1 d PU C 2 F36B F 0.495(3) 0.9527(7) 0.6767(5) 0.094(7) Uani 0.240(9) 1 d P C 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 Cu1 0.02751(13) 0.03256(11) 0.02422(11) -0.00050(9) 0.00110(11) 0.00136(11) N11 0.0331(10) 0.0291(8) 0.0314(10) -0.0013(8) 0.0007(8) 0.0019(7) N12 0.0288(8) 0.0307(8) 0.0253(9) -0.0009(7) 0.0009(7) -0.0015(7) N13 0.0288(9) 0.0338(9) 0.0288(9) -0.0013(8) 0.0008(8) 0.0005(7) N14 0.0325(10) 0.0303(8) 0.0248(9) 0.0002(7) 0.0009(8) 0.0041(7) C11 0.0281(10) 0.0276(9) 0.0339(12) -0.0027(9) -0.0012(10) -0.0015(8) C12 0.0438(15) 0.0317(12) 0.072(2) 0.0042(13) -0.0208(15) 0.0065(10) C13 0.0231(9) 0.0264(9) 0.0254(10) -0.0004(8) -0.0038(8) -0.0005(7) C14 0.0358(12) 0.0468(13) 0.0313(12) -0.0002(11) 0.0084(10) -0.0028(10) C15 0.0323(10) 0.0292(9) 0.0216(9) -0.0009(8) 0.0016(8) 0.0005(8) C16 0.0258(10) 0.0424(11) 0.0413(12) 0.0012(10) -0.0003(10) 0.0002(10) C17 0.0278(10) 0.0261(9) 0.0241(10) 0.0028(8) 0.0005(9) 0.0038(8) C18 0.0397(12) 0.0345(11) 0.0348(12) -0.0028(10) -0.0091(10) -0.0009(10) Cu2 0.02884(12) 0.02860(11) 0.02679(12) -0.00032(10) -0.00029(11) -0.00104(10) N21 0.0340(10) 0.0277(8) 0.0279(10) -0.0022(7) -0.0004(8) -0.0025(7) N22 0.0353(10) 0.0282(8) 0.0250(9) -0.0010(7) 0.0029(8) -0.0032(7) N23 0.0311(9) 0.0308(9) 0.0270(9) -0.0005(8) -0.0003(7) 0.0013(7) N24 0.0305(9) 0.0326(9) 0.0302(9) -0.0013(8) -0.0003(8) -0.0022(7) C21 0.0261(10) 0.0295(10) 0.0250(10) -0.0014(8) -0.0015(8) -0.0052(8) C22 0.0368(12) 0.0377(12) 0.0456(16) -0.0086(11) 0.0043(11) 0.0060(10) C23 0.0290(10) 0.0313(10) 0.0231(10) -0.0032(8) 0.0021(9) 0.0008(8) C24 0.0427(13) 0.0404(13) 0.0387(14) 0.0109(11) 0.0062(11) -0.0093(11) C25 0.0256(9) 0.0259(9) 0.0304(10) -0.0007(9) 0.0017(8) 0.0004(8) C26 0.0374(12) 0.0534(14) 0.0302(12) 0.0013(12) -0.0061(10) -0.0008(11) C27 0.0318(10) 0.0259(9) 0.0229(9) -0.0027(8) 0.0006(8) -0.0032(8) C28 0.0276(10) 0.0352(9) 0.0360(10) -0.0026(9) 0.0018(10) -0.0007(9) Cu3 0.03201(14) 0.03087(11) 0.02949(12) -0.00087(10) -0.00097(12) 0.00174(11) N31 0.0365(10) 0.0344(8) 0.0365(10) 0.0021(8) -0.0025(9) 0.0051(9) N32 0.0335(10) 0.0298(8) 0.0298(10) -0.0004(8) -0.0018(8) 0.0021(7) N33 0.0401(11) 0.0331(8) 0.0331(10) -0.0025(8) -0.0010(9) -0.0022(8) N34 0.0290(9) 0.0419(10) 0.0303(10) -0.0004(9) -0.0038(8) -0.0010(8) C31 0.0305(11) 0.0353(10) 0.0287(10) -0.0052(8) -0.0035(9) 0.0025(9) C32 0.0439(14) 0.0349(10) 0.0371(12) 0.0055(9) -0.0031(11) -0.0004(11) C33 0.0350(11) 0.0248(9) 0.0268(10) -0.0034(9) -0.0023(9) 0.0018(8) C34 0.0289(11) 0.0421(12) 0.0550(16) -0.0074(12) -0.0023(11) -0.0005(10) C35 0.0370(12) 0.0327(10) 0.0250(10) 0.0033(8) 0.0046(9) -0.0039(9) C36 0.0562(16) 0.0318(10) 0.0305(11) -0.0047(9) 0.0092(11) -0.0063(11) C37 0.0227(9) 0.0331(10) 0.0327(11) -0.0021(9) -0.0041(9) -0.0029(8) C38 0.0360(12) 0.0401(12) 0.0343(12) -0.0034(11) 0.0021(10) -0.0044(10) N41 0.0558(14) 0.0428(11) 0.0547(14) 0.0004(10) -0.0046(13) -0.0024(11) C41 0.0406(13) 0.0448(13) 0.0326(13) -0.0074(11) -0.0030(11) -0.0007(11) C42 0.076(2) 0.072(2) 0.0507(18) -0.0010(16) 0.0073(17) -0.0339(19) N51 0.0501(14) 0.0455(12) 0.0576(15) 0.0041(11) -0.0042(12) -0.0011(11) C51 0.0429(14) 0.0383(12) 0.0429(14) -0.0007(11) -0.0059(12) 0.0057(11) C52 0.061(2) 0.0619(19) 0.078(2) 0.0049(19) 0.0115(18) -0.0100(17) N61 0.0484(13) 0.0441(10) 0.0487(13) -0.0144(10) -0.0012(12) -0.0039(10) C61 0.0293(11) 0.0342(10) 0.0500(14) -0.0144(10) -0.0006(12) -0.0014(10) C62 0.0373(14) 0.0568(15) 0.0576(16) 0.0037(13) -0.0004(14) -0.0001(13) P1 0.0265(3) 0.0262(2) 0.0335(3) 0.0022(2) 0.0004(2) -0.0001(2) F11 0.0368(9) 0.0762(13) 0.144(2) 0.0635(14) -0.0061(12) 0.0070(9) F12 0.0395(9) 0.0596(10) 0.0961(16) 0.0323(11) -0.0134(10) 0.0024(8) F13A 0.159(5) 0.092(3) 0.070(2) -0.039(2) 0.037(3) 0.001(4) F14A 0.0333(13) 0.0481(18) 0.078(3) 0.0281(19) -0.0018(14) -0.0101(11) F15A 0.106(3) 0.089(3) 0.060(2) -0.0308(19) -0.002(2) -0.024(3) F16A 0.0267(12) 0.059(2) 0.116(5) 0.049(3) 0.0071(17) -0.0037(12) F13B 0.099(7) 0.130(11) 0.048(4) 0.030(6) 0.045(5) 0.030(8) F14B 0.097(7) 0.043(3) 0.138(12) -0.004(4) -0.039(8) -0.036(4) F15B 0.103(8) 0.162(14) 0.059(5) 0.008(8) 0.053(5) 0.018(10) F16B 0.108(9) 0.058(4) 0.137(12) -0.028(5) -0.049(10) -0.031(5) P2 0.0313(3) 0.0282(2) 0.0329(3) -0.0022(2) -0.0020(2) -0.0030(2) F21 0.0488(10) 0.0641(11) 0.0775(13) 0.0101(10) -0.0221(10) 0.0059(8) F22 0.0633(12) 0.0614(12) 0.123(2) 0.0343(13) -0.0231(14) 0.0138(10) F23A 0.083(2) 0.140(4) 0.0532(17) 0.004(2) 0.0312(15) -0.010(2) F24A 0.0727(19) 0.0449(12) 0.075(3) -0.0044(12) -0.0265(18) -0.0211(11) F25A 0.087(2) 0.134(4) 0.0477(15) -0.018(2) 0.0277(14) 0.002(2) F26A 0.099(3) 0.0522(15) 0.142(5) -0.031(2) -0.018(3) -0.0356(16) F23B 0.110(13) 0.072(8) 0.069(8) -0.035(7) -0.025(9) 0.043(8) F24B 0.030(4) 0.088(9) 0.121(15) 0.063(10) -0.018(6) -0.013(5) F25B 0.147(17) 0.074(9) 0.060(7) -0.021(6) 0.027(9) 0.026(10) F26B 0.049(6) 0.051(7) 0.102(12) 0.037(8) 0.003(7) -0.019(5) P3 0.0326(3) 0.0254(2) 0.0274(2) 0.0010(2) -0.0012(2) -0.0005(2) F31 0.0599(11) 0.0335(7) 0.0604(11) 0.0106(7) 0.0094(9) -0.0074(7) F32 0.0580(11) 0.0384(7) 0.0661(11) 0.0095(8) 0.0189(9) -0.0101(7) F33A 0.066(2) 0.0415(14) 0.115(5) -0.025(2) 0.040(2) 0.0091(16) F34A 0.085(3) 0.110(3) 0.0564(19) 0.012(2) -0.0466(18) -0.026(3) F35A 0.065(2) 0.0358(12) 0.106(3) -0.0179(14) 0.041(2) -0.0011(12) F36A 0.0579(17) 0.111(3) 0.0504(18) 0.0127(19) -0.0260(15) -0.014(2) F33B 0.024(3) 0.066(6) 0.103(10) 0.051(6) -0.013(4) -0.004(3) F34B 0.088(8) 0.055(4) 0.046(5) -0.023(4) 0.038(5) -0.017(5) F35B 0.039(4) 0.066(5) 0.083(8) 0.033(5) -0.024(5) 0.010(4) F36B 0.165(19) 0.067(7) 0.050(7) -0.022(5) 0.054(10) -0.053(10) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 N13 1.9633(19) . ? Cu1 N12 1.9931(18) . ? Cu1 N11 2.0111(19) . ? Cu1 N14 2.0144(19) . ? N11 C11 1.137(3) . ? N12 C13 1.134(3) . ? N13 C15 1.137(3) . ? N14 C17 1.133(3) . ? C11 C12 1.451(3) . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 C14 1.446(3) . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 C16 1.449(3) . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 C18 1.455(3) . ? C18 H18A 0.98 . ? C18 H18B 0.98 . ? C18 H18C 0.98 . ? Cu2 N24 1.9730(19) . ? Cu2 N23 1.9995(18) . ? Cu2 N21 2.0052(19) . ? Cu2 N22 2.0190(18) . ? N21 C21 1.134(3) . ? N22 C23 1.126(3) . ? N23 C25 1.135(3) . ? N24 C27 1.138(3) . ? C21 C22 1.451(3) . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 C24 1.464(3) . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 C26 1.447(3) . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 C28 1.454(3) . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? Cu3 N34 1.988(2) . ? Cu3 N31 1.9988(18) . ? Cu3 N33 1.9995(19) . ? Cu3 N32 2.018(2) . ? N31 C31 1.137(3) . ? N32 C33 1.132(3) . ? N33 C35 1.134(3) . ? N34 C37 1.135(3) . ? C31 C32 1.457(3) . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? C33 C34 1.453(3) . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 C36 1.454(3) . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C37 C38 1.451(3) . ? C38 H38A 0.98 . ? C38 H38B 0.98 . ? C38 H38C 0.98 . ? N41 C41 1.135(3) . ? C41 C42 1.453(4) . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? N51 C51 1.131(4) . ? C51 C52 1.455(4) . ? C52 H52A 0.98 . ? C52 H52B 0.98 . ? C52 H52C 0.98 . ? N61 C61 1.140(3) . ? C61 C62 1.447(4) . ? C62 H62A 0.98 . ? C62 H62B 0.98 . ? C62 H62C 0.98 . ? P1 F15B 1.534(7) . ? P1 F14B 1.536(6) . ? P1 F13A 1.548(3) . ? P1 F16A 1.567(3) . ? P1 F16B 1.572(6) . ? P1 F11 1.5756(18) . ? P1 F12 1.5853(17) . ? P1 F13B 1.594(6) . ? P1 F15A 1.597(3) . ? P1 F14A 1.610(2) . ? P2 F26B 1.543(9) . ? P2 F23B 1.548(10) . ? P2 F26A 1.559(3) . ? P2 F25A 1.568(3) . ? P2 F24B 1.579(10) . ? P2 F22 1.5801(19) . ? P2 F23A 1.584(3) . ? P2 F25B 1.587(10) . ? P2 F24A 1.590(2) . ? P2 F21 1.5964(18) . ? P3 F35B 1.448(8) . ? P3 F34A 1.537(3) . ? P3 F34B 1.548(7) . ? P3 F33A 1.549(4) . ? P3 F36B 1.576(14) . ? P3 F31 1.5940(15) . ? P3 F32 1.5947(16) . ? P3 F35A 1.617(3) . ? P3 F36A 1.619(3) . ? P3 F33B 1.672(7) . ? 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 N13 Cu1 N12 113.44(8) . . ? N13 Cu1 N11 111.90(8) . . ? N12 Cu1 N11 105.56(8) . . ? N13 Cu1 N14 114.02(8) . . ? N12 Cu1 N14 104.78(8) . . ? N11 Cu1 N14 106.43(8) . . ? C11 N11 Cu1 171.27(19) . . ? C13 N12 Cu1 171.29(18) . . ? C15 N13 Cu1 175.35(19) . . ? C17 N14 Cu1 168.55(18) . . ? N11 C11 C12 179.5(3) . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? N12 C13 C14 179.0(2) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? N13 C15 C16 178.7(3) . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? N14 C17 C18 179.0(2) . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N24 Cu2 N23 113.48(8) . . ? N24 Cu2 N21 111.94(8) . . ? N23 Cu2 N21 107.41(8) . . ? N24 Cu2 N22 111.18(8) . . ? N23 Cu2 N22 106.67(8) . . ? N21 Cu2 N22 105.71(7) . . ? C21 N21 Cu2 173.48(19) . . ? C23 N22 Cu2 174.26(19) . . ? C25 N23 Cu2 173.98(18) . . ? C27 N24 Cu2 177.12(19) . . ? N21 C21 C22 179.0(3) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N22 C23 C24 178.7(2) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N23 C25 C26 179.3(2) . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? N24 C27 C28 179.7(3) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? N34 Cu3 N31 113.08(8) . . ? N34 Cu3 N33 113.56(8) . . ? N31 Cu3 N33 110.21(8) . . ? N34 Cu3 N32 111.94(8) . . ? N31 Cu3 N32 102.67(8) . . ? N33 Cu3 N32 104.51(8) . . ? C31 N31 Cu3 171.1(2) . . ? C33 N32 Cu3 169.6(2) . . ? C35 N33 Cu3 171.8(2) . . ? C37 N34 Cu3 176.78(19) . . ? N31 C31 C32 179.2(3) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? N32 C33 C34 179.4(3) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? N33 C35 C36 179.3(3) . . ? 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 . . ? N34 C37 C38 178.7(2) . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? N41 C41 C42 178.8(3) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? N51 C51 C52 179.6(4) . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? N61 C61 C62 179.8(3) . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? F15B P1 F14B 88.4(7) . . ? F13A P1 F16A 92.5(3) . . ? F15B P1 F16B 91.1(7) . . ? F14B P1 F16B 179.0(5) . . ? F15B P1 F11 89.4(4) . . ? F14B P1 F11 88.1(3) . . ? F13A P1 F11 92.1(2) . . ? F16A P1 F11 89.39(13) . . ? F16B P1 F11 91.0(3) . . ? F15B P1 F12 90.0(4) . . ? F14B P1 F12 93.0(3) . . ? F13A P1 F12 89.17(19) . . ? F16A P1 F12 90.18(11) . . ? F16B P1 F12 87.8(3) . . ? F11 P1 F12 178.67(14) . . ? F15B P1 F13B 177.8(7) . . ? F14B P1 F13B 93.8(7) . . ? F16B P1 F13B 86.7(6) . . ? F11 P1 F13B 90.6(3) . . ? F12 P1 F13B 90.0(3) . . ? F13A P1 F15A 177.3(3) . . ? F16A P1 F15A 89.8(2) . . ? F11 P1 F15A 89.28(18) . . ? F12 P1 F15A 89.46(17) . . ? F13A P1 F14A 90.2(2) . . ? F16A P1 F14A 177.2(3) . . ? F11 P1 F14A 91.00(11) . . ? F12 P1 F14A 89.38(12) . . ? F15A P1 F14A 87.4(2) . . ? F26B P2 F23B 90.6(9) . . ? F26A P2 F25A 91.8(2) . . ? F26B P2 F24B 176.5(9) . . ? F23B P2 F24B 92.9(10) . . ? F26B P2 F22 89.7(4) . . ? F23B P2 F22 89.6(4) . . ? F26A P2 F22 92.03(17) . . ? F25A P2 F22 90.74(17) . . ? F24B P2 F22 90.3(4) . . ? F26A P2 F23A 89.9(2) . . ? F25A P2 F23A 177.8(2) . . ? F22 P2 F23A 90.62(17) . . ? F26B P2 F25B 87.8(9) . . ? F23B P2 F25B 178.4(10) . . ? F24B P2 F25B 88.7(9) . . ? F22 P2 F25B 90.1(5) . . ? F26A P2 F24A 178.6(2) . . ? F25A P2 F24A 89.4(2) . . ? F22 P2 F24A 88.71(13) . . ? F23A P2 F24A 88.90(19) . . ? F26B P2 F21 91.9(4) . . ? F23B P2 F21 89.0(4) . . ? F26A P2 F21 90.10(17) . . ? F25A P2 F21 89.33(16) . . ? F24B P2 F21 88.2(3) . . ? F22 P2 F21 177.86(12) . . ? F23A P2 F21 89.25(16) . . ? F25B P2 F21 91.4(5) . . ? F24A P2 F21 89.15(12) . . ? F35B P3 F34B 91.9(6) . . ? F34A P3 F33A 93.5(2) . . ? F35B P3 F36B 95.4(8) . . ? F34B P3 F36B 172.5(9) . . ? F35B P3 F31 94.0(4) . . ? F34A P3 F31 91.43(15) . . ? F34B P3 F31 88.5(3) . . ? F33A P3 F31 91.1(2) . . ? F36B P3 F31 89.4(6) . . ? F35B P3 F32 85.2(4) . . ? F34A P3 F32 89.22(15) . . ? F34B P3 F32 91.4(3) . . ? F33A P3 F32 89.4(2) . . ? F36B P3 F32 90.8(6) . . ? F31 P3 F32 179.12(11) . . ? F34A P3 F35A 90.2(2) . . ? F33A P3 F35A 176.3(2) . . ? F31 P3 F35A 88.90(11) . . ? F32 P3 F35A 90.50(11) . . ? F34A P3 F36A 176.2(2) . . ? F33A P3 F36A 90.3(2) . . ? F31 P3 F36A 88.17(14) . . ? F32 P3 F36A 91.14(15) . . ? F35A P3 F36A 86.1(2) . . ? F35B P3 F33B 178.8(6) . . ? F34B P3 F33B 87.3(6) . . ? F36B P3 F33B 85.4(8) . . ? F31 P3 F33B 87.0(3) . . ? F32 P3 F33B 93.9(3) . . ? #===END