# Electronic Supplementary Material (ESI) for Dalton Transactions # 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_global #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_chiara150911 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C27 Ag3 F27 N6, 2(C7 H8)' _chemical_formula_sum 'C41 H16 Ag3 F27 N6' _chemical_formula_weight 1429.21 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.5640(5) _cell_length_b 12.8440(4) _cell_length_c 16.4240(7) _cell_angle_alpha 74.837(3) _cell_angle_beta 75.239(4) _cell_angle_gamma 60.808(4) _cell_volume 2207.60(15) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 8027 _cell_measurement_theta_min 3.3502 _cell_measurement_theta_max 29.397 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 2.15 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1376 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.474 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.895 _exptl_absorpt_correction_T_max 0.987 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector_area_resol_mean 16.1978 _diffrn_orient_matrix_ub_11 -0.0422453 _diffrn_orient_matrix_ub_12 0.0036396 _diffrn_orient_matrix_ub_13 -0.0234699 _diffrn_orient_matrix_ub_21 0.0136186 _diffrn_orient_matrix_ub_22 -0.0611753 _diffrn_orient_matrix_ub_23 0.0170236 _diffrn_orient_matrix_ub_31 -0.0480586 _diffrn_orient_matrix_ub_32 0.0188408 _diffrn_orient_matrix_ub_33 0.034757 _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_reflns_av_R_equivalents 0.0549 _diffrn_reflns_av_unetI/netI 0.0772 _diffrn_reflns_number 26584 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 3.36 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _reflns_number_total 8997 _reflns_number_gt 6552 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.35.11 (release 16-05-2011 CrysAlis171 .NET) (compiled May 16 2011,17:55:39) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # 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. ; _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^)+(0.0308P)^2^+32.3602P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 8997 _refine_ls_number_parameters 696 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.1017 _refine_ls_R_factor_gt 0.0685 _refine_ls_wR_factor_ref 0.1608 _refine_ls_wR_factor_gt 0.1474 _refine_ls_goodness_of_fit_ref 1.093 _refine_ls_restrained_S_all 1.093 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.126 _refine_diff_density_min -0.886 _refine_diff_density_rms 0.174 #----------------------------------------------------------------------------# # 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' 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' 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 C1 C 0.1223(8) 0.6498(8) 0.2075(6) 0.032(2) Uani 1 1 d . . . C2 C 0.2282(8) 0.5693(8) 0.2588(6) 0.0244(19) Uani 1 1 d . . . C3 C 0.3441(8) 0.4920(7) 0.2083(5) 0.0219(18) Uani 1 1 d . . . C4 C 0.4330(8) 0.5232(7) 0.1505(5) 0.0200(17) Uani 1 1 d . . . C5 C 0.5190(7) 0.4161(7) 0.1199(5) 0.0179(17) Uani 1 1 d . . . C6 C 0.6229(7) 0.4110(7) 0.0605(5) 0.0197(17) Uani 1 1 d . . . C7 C 0.6366(8) 0.5130(7) 0.0321(5) 0.0219(18) Uani 1 1 d . . . C8 C 0.5512(8) 0.6203(7) 0.0620(6) 0.0246(19) Uani 1 1 d . . . C9 C 0.4497(8) 0.6284(7) 0.1206(6) 0.0241(19) Uani 1 1 d . . . C11 C 0.7538(9) -0.3914(8) 0.2890(6) 0.031(2) Uani 1 1 d . . . C12 C 0.7042(8) -0.3361(7) 0.2037(6) 0.026(2) Uani 1 1 d . . . C13 C 0.7250(8) -0.2292(7) 0.1560(6) 0.0222(18) Uani 1 1 d . . . C14 C 0.8181(7) -0.2197(7) 0.0906(5) 0.0204(18) Uani 1 1 d . . . C15 C 0.7857(8) -0.0960(7) 0.0749(5) 0.0210(18) Uani 1 1 d . . . C16 C 0.8547(8) -0.0474(8) 0.0117(6) 0.0235(19) Uani 1 1 d . . . C17 C 0.9541(8) -0.1223(8) -0.0352(6) 0.0253(19) Uani 1 1 d . . . C18 C 0.9891(8) -0.2464(8) -0.0199(6) 0.026(2) Uani 1 1 d . . . C19 C 0.9222(8) -0.2941(7) 0.0411(6) 0.0240(19) Uani 1 1 d . . . C21 C 0.1466(10) 0.2821(10) 0.5350(8) 0.047(3) Uani 1 1 d . . . C22 C 0.0983(9) 0.2473(9) 0.4760(6) 0.029(2) Uani 1 1 d . . . C23 C 0.1797(7) 0.1309(7) 0.4451(5) 0.0191(17) Uani 1 1 d . . . C24 C 0.1830(8) 0.0162(8) 0.4781(5) 0.0213(18) Uani 1 1 d . . . C25 C 0.2800(8) -0.0581(8) 0.4228(5) 0.0240(19) Uani 1 1 d . . . C26 C 0.3123(9) -0.1823(9) 0.4303(6) 0.033(2) Uani 1 1 d . . . C28 C 0.1428(11) -0.1461(11) 0.5573(7) 0.045(3) Uani 1 1 d . . . C29 C 0.1169(8) -0.0303(9) 0.5458(6) 0.030(2) Uani 1 1 d . . . C51 C 0.3343(9) 0.9909(8) 0.1345(6) 0.027(2) Uani 1 1 d . . . H51 H 0.3967 0.9175 0.1162 0.033 Uiso 1 1 calc R . . C52 C 0.3440(9) 1.0980(8) 0.1036(6) 0.028(2) Uani 1 1 d . . . H52 H 0.4141 1.0976 0.0641 0.034 Uiso 1 1 calc R . . C53 C 0.2527(8) 1.2052(8) 0.1298(6) 0.027(2) Uani 1 1 d . . . H53 H 0.2604 1.2778 0.1082 0.033 Uiso 1 1 calc R . . C54 C 0.1493(8) 1.2071(8) 0.1878(6) 0.027(2) Uani 1 1 d . . . C55 C 0.1401(8) 1.1011(8) 0.2194(6) 0.0244(19) Uani 1 1 d . . . H55 H 0.0707 1.1014 0.2597 0.029 Uiso 1 1 calc R . . C56 C 0.2315(8) 0.9933(8) 0.1928(6) 0.0253(19) Uani 1 1 d . . . H56 H 0.2236 0.9208 0.2147 0.03 Uiso 1 1 calc R . . C57 C 0.0484(10) 1.3244(8) 0.2136(7) 0.038(2) Uani 1 1 d . . . H57A H -0.0266 1.3152 0.2393 0.057 Uiso 1 1 calc R . . H57B H 0.0319 1.3877 0.1632 0.057 Uiso 1 1 calc R . . H57C H 0.074 1.3469 0.2552 0.057 Uiso 1 1 calc R . . F27 F 0.2748(6) -0.3432(5) 0.5104(4) 0.0500(16) Uani 1 1 d . . . C66 C 0.7400(11) 0.2002(12) 0.2583(7) 0.060(4) Uani 1 1 d D . . H66 H 0.8044 0.2043 0.2145 0.071 Uiso 1 1 calc R . . C62 C 0.6325(14) 0.0876(15) 0.3475(10) 0.101(7) Uani 1 1 d D . . H62 H 0.6228 0.0157 0.3639 0.121 Uiso 1 1 calc R . . C63 C 0.5525(13) 0.1877(14) 0.3845(9) 0.076(5) Uani 1 1 d D . . H63 H 0.4881 0.1831 0.4282 0.091 Uiso 1 1 calc R . . C64 C 0.5610(11) 0.2952(12) 0.3613(9) 0.071(4) Uani 1 1 d D . . N1 N 0.3782(6) 0.3753(6) 0.2101(4) 0.0202(15) Uani 1 1 d . . . N2 N 0.4844(6) 0.3271(6) 0.1558(4) 0.0205(15) Uani 1 1 d . . . N3 N 0.6805(6) -0.0363(6) 0.1268(5) 0.0208(15) Uani 1 1 d . . . N4 N 0.6453(7) -0.1190(6) 0.1763(5) 0.0237(16) Uani 1 1 d . . . N5 N 0.3325(7) 0.0045(7) 0.3642(5) 0.0259(17) Uani 1 1 d . . . N6 N 0.2698(7) 0.1219(6) 0.3792(5) 0.0223(15) Uani 1 1 d . . . Ag1 Ag 0.58300(6) 0.14426(5) 0.14488(4) 0.02301(17) Uani 1 1 d . . . Ag2 Ag 0.31866(7) 0.25055(6) 0.29273(4) 0.02737(18) Uani 1 1 d . . . Ag3 Ag 0.47740(6) -0.05336(6) 0.26321(4) 0.02665(18) Uani 1 1 d . . . F1 F 0.1518(5) 0.7206(5) 0.1422(4) 0.0409(14) Uani 1 1 d . . . F2 F 0.0218(5) 0.7189(5) 0.2553(4) 0.0434(15) Uani 1 1 d . . . F3 F 0.0940(5) 0.5800(5) 0.1779(4) 0.0373(13) Uani 1 1 d . . . F4 F 0.2457(5) 0.6437(5) 0.2928(3) 0.0355(13) Uani 1 1 d . . . F5 F 0.1878(5) 0.5012(5) 0.3248(3) 0.0342(13) Uani 1 1 d . . . F6 F 0.7038(4) 0.3080(4) 0.0307(3) 0.0245(11) Uani 1 1 d . . . F7 F 0.7328(4) 0.5144(4) -0.0272(3) 0.0265(11) Uani 1 1 d . . . F8 F 0.5696(5) 0.7197(4) 0.0314(3) 0.0264(11) Uani 1 1 d . . . F9 F 0.3696(5) 0.7324(4) 0.1473(3) 0.0294(12) Uani 1 1 d . . . F11 F 0.8732(5) -0.4230(5) 0.2774(4) 0.0372(13) Uani 1 1 d . . . F12 F 0.6954(5) -0.3108(5) 0.3421(3) 0.0356(13) Uani 1 1 d . . . F13 F 0.7369(6) -0.4880(5) 0.3251(4) 0.0445(15) Uani 1 1 d . . . F14 F 0.7594(5) -0.4252(4) 0.1561(3) 0.0316(12) Uani 1 1 d . . . F15 F 0.5820(5) -0.3064(5) 0.2214(3) 0.0293(12) Uani 1 1 d . . . F16 F 0.8181(5) 0.0731(4) -0.0050(4) 0.0341(13) Uani 1 1 d . . . F17 F 1.0229(5) -0.0808(5) -0.0982(3) 0.0335(13) Uani 1 1 d . . . F18 F 1.0883(5) -0.3164(5) -0.0706(4) 0.0354(13) Uani 1 1 d . . . F19 F 0.9596(5) -0.4145(4) 0.0525(4) 0.0326(13) Uani 1 1 d . . . F21 F 0.0702(6) 0.3869(6) 0.5620(4) 0.0533(17) Uani 1 1 d . . . F22 F 0.2519(6) 0.2859(6) 0.4978(5) 0.0573(19) Uani 1 1 d . . . F23 F 0.1731(7) 0.1944(6) 0.6062(4) 0.0590(19) Uani 1 1 d . . . F24 F -0.0126(5) 0.2556(6) 0.5185(4) 0.0499(17) Uani 1 1 d . . . F25 F 0.0739(6) 0.3439(5) 0.4113(4) 0.0512(17) Uani 1 1 d . . . F26 F 0.4022(6) -0.2475(5) 0.3771(4) 0.0514(17) Uani 1 1 d . . . F28 F 0.0924(6) -0.2053(5) 0.6182(4) 0.0469(16) Uani 1 1 d . . . F29 F 0.0266(6) 0.0324(6) 0.6036(4) 0.0454(15) Uani 1 1 d . . . C61 C 0.7276(14) 0.0942(13) 0.2856(9) 0.068(4) Uani 1 1 d D . . H61 H 0.7862 0.0244 0.2611 0.082 Uiso 1 1 calc R . . C165 C 0.6561(12) 0.2988(11) 0.2966(8) 0.069(4) Uani 1 1 d D . . H165 H 0.6632 0.372 0.2783 0.082 Uiso 1 1 calc R . . C67 C 0.4715(17) 0.4022(18) 0.4063(13) 0.119(8) Uani 1 1 d . . . H67A H 0.3868 0.4199 0.4048 0.178 Uiso 1 1 calc R . . H67B H 0.4849 0.4729 0.3773 0.178 Uiso 1 1 calc R . . H67C H 0.4851 0.383 0.4657 0.178 Uiso 1 1 calc R . . C27 C 0.2472(10) -0.2249(9) 0.4976(8) 0.043(3) 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 C1 0.026(5) 0.029(5) 0.035(6) -0.006(4) 0.003(4) -0.011(4) C2 0.030(5) 0.022(4) 0.022(5) -0.008(4) 0.002(4) -0.013(4) C3 0.023(4) 0.018(4) 0.022(5) -0.005(3) 0.002(4) -0.009(3) C4 0.024(4) 0.020(4) 0.021(4) -0.001(3) -0.006(3) -0.014(4) C5 0.018(4) 0.019(4) 0.019(4) 0.000(3) -0.007(3) -0.010(3) C6 0.017(4) 0.018(4) 0.022(4) -0.004(3) -0.006(3) -0.004(3) C7 0.022(4) 0.023(4) 0.020(4) -0.001(3) -0.005(3) -0.009(4) C8 0.026(5) 0.020(4) 0.031(5) -0.001(4) -0.008(4) -0.012(4) C9 0.024(4) 0.017(4) 0.027(5) -0.004(3) -0.005(4) -0.005(4) C11 0.032(5) 0.029(5) 0.036(6) 0.003(4) -0.011(4) -0.019(4) C12 0.021(4) 0.018(4) 0.037(5) -0.009(4) 0.000(4) -0.008(4) C13 0.026(4) 0.013(4) 0.026(5) 0.002(3) -0.014(4) -0.005(3) C14 0.018(4) 0.019(4) 0.025(5) -0.005(3) -0.007(3) -0.007(3) C15 0.020(4) 0.019(4) 0.024(5) -0.002(3) -0.003(3) -0.010(3) C16 0.023(4) 0.022(4) 0.026(5) -0.004(4) -0.007(4) -0.009(4) C17 0.022(4) 0.030(5) 0.024(5) -0.006(4) -0.004(4) -0.010(4) C18 0.016(4) 0.028(5) 0.027(5) -0.011(4) -0.005(4) -0.002(4) C19 0.032(5) 0.020(4) 0.023(5) -0.004(3) -0.014(4) -0.009(4) C21 0.038(6) 0.042(6) 0.052(7) -0.016(5) 0.013(5) -0.017(5) C22 0.031(5) 0.037(5) 0.018(5) -0.003(4) 0.006(4) -0.021(4) C23 0.022(4) 0.026(4) 0.016(4) -0.004(3) -0.005(3) -0.015(4) C24 0.020(4) 0.028(5) 0.017(4) 0.002(3) -0.004(3) -0.014(4) C25 0.031(5) 0.030(5) 0.012(4) 0.001(3) -0.003(4) -0.017(4) C26 0.025(5) 0.034(5) 0.034(6) -0.001(4) 0.000(4) -0.013(4) C28 0.065(8) 0.064(7) 0.031(6) 0.023(5) -0.024(5) -0.057(7) C29 0.023(5) 0.048(6) 0.024(5) -0.012(4) 0.001(4) -0.018(4) C51 0.034(5) 0.019(4) 0.027(5) -0.002(4) -0.008(4) -0.009(4) C52 0.030(5) 0.025(5) 0.033(5) -0.002(4) -0.005(4) -0.016(4) C53 0.036(5) 0.022(4) 0.030(5) 0.003(4) -0.008(4) -0.020(4) C54 0.031(5) 0.027(5) 0.025(5) -0.002(4) -0.012(4) -0.012(4) C55 0.026(5) 0.026(5) 0.022(5) -0.005(4) 0.001(4) -0.014(4) C56 0.028(5) 0.026(5) 0.025(5) -0.001(4) -0.004(4) -0.017(4) C57 0.045(6) 0.025(5) 0.044(6) -0.008(4) -0.011(5) -0.012(5) F27 0.052(4) 0.035(3) 0.062(4) -0.002(3) -0.005(3) -0.024(3) C66 0.043(7) 0.097(11) 0.029(6) 0.000(7) -0.015(5) -0.024(7) C62 0.122(16) 0.074(12) 0.127(17) 0.016(11) -0.103(15) -0.036(12) C63 0.063(9) 0.116(14) 0.068(10) 0.029(10) -0.040(8) -0.063(10) C64 0.039(7) 0.089(11) 0.068(10) -0.028(8) -0.022(7) -0.002(7) N1 0.025(4) 0.016(3) 0.024(4) -0.002(3) -0.007(3) -0.011(3) N2 0.025(4) 0.023(4) 0.021(4) -0.003(3) -0.006(3) -0.015(3) N3 0.014(3) 0.018(3) 0.027(4) -0.007(3) 0.002(3) -0.005(3) N4 0.028(4) 0.011(3) 0.027(4) -0.003(3) -0.005(3) -0.004(3) N5 0.030(4) 0.033(4) 0.019(4) -0.004(3) 0.004(3) -0.021(4) N6 0.027(4) 0.023(4) 0.022(4) -0.002(3) -0.004(3) -0.017(3) Ag1 0.0236(3) 0.0147(3) 0.0277(4) -0.0024(3) -0.0026(3) -0.0075(3) Ag2 0.0336(4) 0.0261(4) 0.0249(4) 0.0014(3) -0.0020(3) -0.0191(3) Ag3 0.0265(4) 0.0247(4) 0.0265(4) -0.0032(3) 0.0014(3) -0.0129(3) F1 0.034(3) 0.033(3) 0.042(4) 0.003(3) -0.001(3) -0.012(3) F2 0.029(3) 0.034(3) 0.049(4) -0.013(3) 0.009(3) -0.005(3) F3 0.031(3) 0.039(3) 0.044(4) -0.012(3) -0.006(3) -0.015(3) F4 0.043(3) 0.034(3) 0.033(3) -0.018(2) 0.003(3) -0.019(3) F5 0.036(3) 0.029(3) 0.030(3) -0.004(2) 0.008(2) -0.015(2) F6 0.021(2) 0.017(2) 0.031(3) -0.008(2) 0.002(2) -0.006(2) F7 0.022(3) 0.024(3) 0.030(3) -0.001(2) 0.003(2) -0.013(2) F8 0.035(3) 0.018(2) 0.029(3) -0.001(2) -0.002(2) -0.017(2) F9 0.029(3) 0.016(2) 0.043(3) -0.010(2) -0.002(2) -0.009(2) F11 0.032(3) 0.032(3) 0.047(4) 0.002(3) -0.020(3) -0.012(2) F12 0.044(3) 0.030(3) 0.031(3) -0.006(2) -0.006(3) -0.013(3) F13 0.059(4) 0.034(3) 0.044(4) 0.013(3) -0.016(3) -0.030(3) F14 0.037(3) 0.017(2) 0.041(3) -0.008(2) -0.008(3) -0.010(2) F15 0.026(3) 0.031(3) 0.039(3) -0.004(2) -0.007(2) -0.018(2) F16 0.036(3) 0.021(3) 0.039(3) -0.002(2) 0.003(2) -0.014(2) F17 0.025(3) 0.037(3) 0.035(3) -0.004(2) 0.003(2) -0.015(2) F18 0.025(3) 0.034(3) 0.036(3) -0.011(2) -0.001(2) -0.004(2) F19 0.033(3) 0.016(2) 0.043(3) -0.014(2) -0.004(2) -0.004(2) F21 0.055(4) 0.046(4) 0.057(4) -0.027(3) 0.004(3) -0.018(3) F22 0.043(4) 0.069(5) 0.071(5) -0.032(4) 0.011(3) -0.033(4) F23 0.075(5) 0.050(4) 0.038(4) -0.007(3) -0.009(3) -0.017(4) F24 0.030(3) 0.044(4) 0.074(5) -0.016(3) 0.009(3) -0.020(3) F25 0.063(4) 0.032(3) 0.048(4) -0.012(3) 0.009(3) -0.020(3) F26 0.045(4) 0.027(3) 0.072(5) -0.016(3) 0.014(3) -0.015(3) F28 0.046(4) 0.045(4) 0.046(4) -0.002(3) -0.002(3) -0.023(3) F29 0.043(4) 0.052(4) 0.041(4) -0.009(3) -0.001(3) -0.024(3) C61 0.066(9) 0.100(12) 0.047(8) -0.005(8) -0.031(7) -0.038(9) C165 0.089(11) 0.053(8) 0.088(11) 0.007(7) -0.062(9) -0.036(8) C67 0.089(13) 0.116(16) 0.119(16) -0.059(13) -0.036(12) 0.007(12) C27 0.039(6) 0.024(5) 0.063(8) -0.006(5) 0.001(5) -0.017(5) #----------------------------------------------------------------------------# # 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 C1 F1 1.316(10) . ? C1 F2 1.329(10) . ? C1 F3 1.340(11) . ? C1 C2 1.524(13) . ? C2 F4 1.349(10) . ? C2 F5 1.362(10) . ? C2 C3 1.482(11) . ? C3 N1 1.337(10) . ? C3 C4 1.416(11) . ? C4 C5 1.396(11) . ? C4 C9 1.410(11) . ? C5 N2 1.358(10) . ? C5 C6 1.401(11) . ? C6 F6 1.341(9) . ? C6 C7 1.349(11) . ? C7 F7 1.350(9) . ? C7 C8 1.391(12) . ? C8 F8 1.351(9) . ? C8 C9 1.365(12) . ? C9 F9 1.327(9) . ? C11 F13 1.321(10) . ? C11 F11 1.325(10) . ? C11 F12 1.333(11) . ? C11 C12 1.532(13) . ? C12 F14 1.349(10) . ? C12 F15 1.359(10) . ? C12 C13 1.499(11) . ? C13 N4 1.346(10) . ? C13 C14 1.402(12) . ? C14 C19 1.389(12) . ? C14 C15 1.402(11) . ? C15 N3 1.356(10) . ? C15 C16 1.397(12) . ? C16 C17 1.342(12) . ? C16 F16 1.353(9) . ? C17 F17 1.345(10) . ? C17 C18 1.399(12) . ? C18 F18 1.352(9) . ? C18 C19 1.356(13) . ? C19 F19 1.354(9) . ? C21 F22 1.327(12) . ? C21 F21 1.328(12) . ? C21 F23 1.374(13) . ? C21 C22 1.516(16) . ? C22 F24 1.357(10) . ? C22 F25 1.366(11) . ? C22 C23 1.476(12) . ? C23 N6 1.334(10) . ? C23 C24 1.413(11) . ? C24 C29 1.397(12) . ? C24 C25 1.406(12) . ? C25 N5 1.340(10) . ? C25 C26 1.419(13) . ? C26 F26 1.303(11) . ? C26 C27 1.360(14) . ? C28 F28 1.315(11) . ? C28 C29 1.329(15) . ? C28 C27 1.510(16) . ? C29 F29 1.340(11) . ? C51 C56 1.390(12) . ? C51 C52 1.390(12) . ? C51 H51 0.95 . ? C52 C53 1.384(13) . ? C52 H52 0.95 . ? C53 C54 1.395(13) . ? C53 H53 0.95 . ? C54 C55 1.375(12) . ? C54 C57 1.502(13) . ? C55 C56 1.391(12) . ? C55 H55 0.95 . ? C56 H56 0.95 . ? C57 H57A 0.98 . ? C57 H57B 0.98 . ? C57 H57C 0.98 . ? F27 C27 1.352(11) . ? C66 C165 1.373(9) . ? C66 C61 1.389(9) . ? C66 H66 0.95 . ? C62 C63 1.367(9) . ? C62 C61 1.380(9) . ? C62 H62 0.95 . ? C63 C64 1.382(9) . ? C63 H63 0.95 . ? C64 C165 1.394(9) . ? C64 C67 1.52(2) . ? N1 N2 1.354(10) . ? N1 Ag2 2.118(7) . ? N2 Ag1 2.086(7) . ? N3 N4 1.345(9) . ? N3 Ag1 2.091(7) . ? N4 Ag3 2.135(7) . ? N5 N6 1.375(10) . ? N5 Ag3 2.099(7) . ? N6 Ag2 2.108(7) . ? Ag1 Ag3 3.3721(9) . ? C61 H61 0.95 . ? C165 H165 0.95 . ? C67 H67A 0.98 . ? C67 H67B 0.98 . ? C67 H67C 0.98 . ? 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 F1 C1 F2 108.2(7) . . ? F1 C1 F3 108.4(8) . . ? F2 C1 F3 107.7(8) . . ? F1 C1 C2 111.7(8) . . ? F2 C1 C2 111.6(8) . . ? F3 C1 C2 109.0(7) . . ? F4 C2 F5 107.1(7) . . ? F4 C2 C3 110.8(7) . . ? F5 C2 C3 111.1(7) . . ? F4 C2 C1 106.4(7) . . ? F5 C2 C1 106.9(7) . . ? C3 C2 C1 114.2(7) . . ? N1 C3 C4 108.5(7) . . ? N1 C3 C2 122.1(7) . . ? C4 C3 C2 129.3(7) . . ? C5 C4 C9 119.7(8) . . ? C5 C4 C3 104.1(7) . . ? C9 C4 C3 136.2(8) . . ? N2 C5 C4 110.1(7) . . ? N2 C5 C6 129.0(8) . . ? C4 C5 C6 120.9(7) . . ? F6 C6 C7 121.3(7) . . ? F6 C6 C5 120.3(7) . . ? C7 C6 C5 118.4(8) . . ? C6 C7 F7 121.0(7) . . ? C6 C7 C8 121.2(8) . . ? F7 C7 C8 117.8(7) . . ? F8 C8 C9 119.2(8) . . ? F8 C8 C7 118.7(8) . . ? C9 C8 C7 122.1(8) . . ? F9 C9 C8 120.6(8) . . ? F9 C9 C4 121.8(8) . . ? C8 C9 C4 117.7(8) . . ? F13 C11 F11 108.6(7) . . ? F13 C11 F12 108.4(8) . . ? F11 C11 F12 108.5(8) . . ? F13 C11 C12 111.2(8) . . ? F11 C11 C12 110.3(8) . . ? F12 C11 C12 109.8(7) . . ? F14 C12 F15 107.5(7) . . ? F14 C12 C13 110.2(7) . . ? F15 C12 C13 111.0(7) . . ? F14 C12 C11 106.5(7) . . ? F15 C12 C11 106.4(7) . . ? C13 C12 C11 114.9(7) . . ? N4 C13 C14 109.3(7) . . ? N4 C13 C12 119.1(8) . . ? C14 C13 C12 131.6(8) . . ? C19 C14 C15 118.0(8) . . ? C19 C14 C13 138.6(8) . . ? C15 C14 C13 103.4(7) . . ? N3 C15 C16 127.9(7) . . ? N3 C15 C14 110.3(7) . . ? C16 C15 C14 121.8(8) . . ? C17 C16 F16 120.9(8) . . ? C17 C16 C15 118.4(8) . . ? F16 C16 C15 120.6(8) . . ? C16 C17 F17 121.2(8) . . ? C16 C17 C18 120.9(8) . . ? F17 C17 C18 117.9(8) . . ? F18 C18 C19 120.9(8) . . ? F18 C18 C17 118.0(8) . . ? C19 C18 C17 121.1(8) . . ? F19 C19 C18 118.6(8) . . ? F19 C19 C14 121.4(8) . . ? C18 C19 C14 119.9(8) . . ? F22 C21 F21 107.9(9) . . ? F22 C21 F23 106.3(10) . . ? F21 C21 F23 107.2(9) . . ? F22 C21 C22 110.5(9) . . ? F21 C21 C22 115.3(10) . . ? F23 C21 C22 109.2(9) . . ? F24 C22 F25 106.4(8) . . ? F24 C22 C23 113.3(8) . . ? F25 C22 C23 112.6(7) . . ? F24 C22 C21 104.7(8) . . ? F25 C22 C21 101.5(8) . . ? C23 C22 C21 117.2(8) . . ? N6 C23 C24 109.8(7) . . ? N6 C23 C22 120.7(7) . . ? C24 C23 C22 129.4(8) . . ? C29 C24 C25 121.3(8) . . ? C29 C24 C23 135.8(8) . . ? C25 C24 C23 102.9(7) . . ? N5 C25 C24 111.1(8) . . ? N5 C25 C26 126.8(8) . . ? C24 C25 C26 122.1(8) . . ? F26 C26 C27 124.9(9) . . ? F26 C26 C25 120.0(8) . . ? C27 C26 C25 115.0(9) . . ? F28 C28 C29 128.2(11) . . ? F28 C28 C27 113.5(9) . . ? C29 C28 C27 118.2(9) . . ? C28 C29 F29 114.6(9) . . ? C28 C29 C24 120.0(9) . . ? F29 C29 C24 125.4(9) . . ? C56 C51 C52 118.8(8) . . ? C56 C51 H51 120.6 . . ? C52 C51 H51 120.6 . . ? C53 C52 C51 120.6(9) . . ? C53 C52 H52 119.7 . . ? C51 C52 H52 119.7 . . ? C52 C53 C54 120.3(8) . . ? C52 C53 H53 119.9 . . ? C54 C53 H53 119.9 . . ? C55 C54 C53 119.3(8) . . ? C55 C54 C57 120.7(9) . . ? C53 C54 C57 120.0(8) . . ? C54 C55 C56 120.6(8) . . ? C54 C55 H55 119.7 . . ? C56 C55 H55 119.7 . . ? C51 C56 C55 120.5(8) . . ? C51 C56 H56 119.8 . . ? C55 C56 H56 119.8 . . ? C54 C57 H57A 109.5 . . ? C54 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C54 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C165 C66 C61 118.0(12) . . ? C165 C66 H66 121 . . ? C61 C66 H66 121 . . ? C63 C62 C61 118.0(15) . . ? C63 C62 H62 121 . . ? C61 C62 H62 121 . . ? C62 C63 C64 123.1(14) . . ? C62 C63 H63 118.4 . . ? C64 C63 H63 118.4 . . ? C63 C64 C165 116.8(12) . . ? C63 C64 C67 120.7(15) . . ? C165 C64 C67 122.4(15) . . ? C3 N1 N2 110.3(7) . . ? C3 N1 Ag2 133.0(6) . . ? N2 N1 Ag2 115.8(5) . . ? N1 N2 C5 107.1(6) . . ? N1 N2 Ag1 124.5(5) . . ? C5 N2 Ag1 128.0(6) . . ? N4 N3 C15 107.2(6) . . ? N4 N3 Ag1 120.4(5) . . ? C15 N3 Ag1 132.2(5) . . ? N3 N4 C13 109.7(7) . . ? N3 N4 Ag3 116.8(5) . . ? C13 N4 Ag3 133.4(6) . . ? C25 N5 N6 107.0(7) . . ? C25 N5 Ag3 129.4(6) . . ? N6 N5 Ag3 123.6(5) . . ? C23 N6 N5 109.2(6) . . ? C23 N6 Ag2 132.9(6) . . ? N5 N6 Ag2 117.6(5) . . ? N2 Ag1 N3 176.8(3) . . ? N2 Ag1 Ag3 120.34(19) . . ? N3 Ag1 Ag3 61.23(18) . . ? N6 Ag2 N1 176.1(3) . . ? N5 Ag3 N4 169.9(3) . . ? N5 Ag3 Ag1 118.2(2) . . ? N4 Ag3 Ag1 61.35(18) . . ? C62 C61 C66 121.7(15) . . ? C62 C61 H61 119.1 . . ? C66 C61 H61 119.1 . . ? C66 C165 C64 122.3(12) . . ? C66 C165 H165 118.9 . . ? C64 C165 H165 118.9 . . ? C64 C67 H67A 109.5 . . ? C64 C67 H67B 109.5 . . ? H67A C67 H67B 109.5 . . ? C64 C67 H67C 109.5 . . ? H67A C67 H67C 109.5 . . ? H67B C67 H67C 109.5 . . ? F27 C27 C26 118.5(9) . . ? F27 C27 C28 118.1(9) . . ? C26 C27 C28 123.3(9) . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF _database_code_depnum_ccdc_archive 'CCDC 929490' ####################################################################### # # 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_global #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_Mickael170511 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C27 Ag3 F27 N6, C4 H10 O' _chemical_formula_sum 'C31 H10 Ag3 F27 N6 O' _chemical_formula_weight 1319.06 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.6128(9) _cell_length_b 12.9362(5) _cell_length_c 13.6226(7) _cell_angle_alpha 78.199(3) _cell_angle_beta 73.173(3) _cell_angle_gamma 63.132(4) _cell_volume 1890.77(18) _cell_formula_units_Z 2 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 13900 _cell_measurement_theta_min 3.375 _cell_measurement_theta_max 29.1977 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.03 _exptl_crystal_density_diffrn 2.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1260 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.712 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_absorpt_correction_T_min 0.6954 _exptl_absorpt_correction_T_max 0.8779 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini ultra' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 16.1978 _diffrn_orient_matrix_ub_11 0.0264744 _diffrn_orient_matrix_ub_12 -0.0542672 _diffrn_orient_matrix_ub_13 0.0281049 _diffrn_orient_matrix_ub_21 -0.0255412 _diffrn_orient_matrix_ub_22 -0.02448 _diffrn_orient_matrix_ub_23 -0.023743 _diffrn_orient_matrix_ub_31 0.0532386 _diffrn_orient_matrix_ub_32 -0.0161927 _diffrn_orient_matrix_ub_33 -0.0403436 _diffrn_reflns_av_R_equivalents 0.0432 _diffrn_reflns_av_unetI/netI 0.0445 _diffrn_reflns_number 31328 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.38 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 7710 _reflns_number_gt 5955 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_cell_refinement ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_data_reduction ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.34.44 (release 25-10-2010 CrysAlis171 .NET) (compiled Oct 25 2010,18:11:34) ; _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # 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. ; _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^)+(0.0293P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7710 _refine_ls_number_parameters 615 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0497 _refine_ls_R_factor_gt 0.031 _refine_ls_wR_factor_ref 0.0687 _refine_ls_wR_factor_gt 0.0621 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 0.999 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.803 _refine_diff_density_min -0.5 _refine_diff_density_rms 0.09 #----------------------------------------------------------------------------# # 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' O O 0.0106 0.006 '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' 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' 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 C1 C 0.8677(3) 0.3029(3) 0.2502(2) 0.0271(8) Uani 1 1 d . . . C2 C 0.9335(3) 0.3584(3) 0.2666(3) 0.0319(8) Uani 1 1 d . . . C3 C 0.9024(3) 0.4016(3) 0.3577(3) 0.0334(8) Uani 1 1 d . . . C4 C 0.8036(4) 0.3930(3) 0.4350(2) 0.0367(9) Uani 1 1 d . . . C5 C 0.7382(3) 0.3403(3) 0.4209(2) 0.0317(8) Uani 1 1 d . . . C6 C 0.7694(3) 0.2925(3) 0.3272(2) 0.0277(8) Uani 1 1 d . . . C7 C 0.7312(3) 0.2298(3) 0.2828(2) 0.0295(8) Uani 1 1 d . . . C8 C 0.6260(3) 0.1976(3) 0.3227(3) 0.0371(9) Uani 1 1 d . . . C9 C 0.5046(4) 0.2944(4) 0.3093(3) 0.0486(11) Uani 1 1 d . . . C11 C 1.1772(3) 0.3203(3) -0.1654(2) 0.0278(8) Uani 1 1 d . . . C12 C 1.2040(3) 0.3878(3) -0.1166(3) 0.0316(8) Uani 1 1 d . . . C13 C 1.2947(3) 0.4219(3) -0.1663(3) 0.0332(8) Uani 1 1 d . . . C14 C 1.3604(3) 0.3907(3) -0.2671(3) 0.0330(8) Uani 1 1 d . . . C15 C 1.3353(3) 0.3265(3) -0.3168(3) 0.0336(8) Uani 1 1 d . . . C16 C 1.2419(3) 0.2900(3) -0.2671(2) 0.0285(8) Uani 1 1 d . . . C17 C 1.1898(3) 0.2231(3) -0.2876(2) 0.0290(8) Uani 1 1 d . . . C18 C 1.2154(3) 0.1691(3) -0.3838(3) 0.0382(9) Uani 1 1 d . . . C19 C 1.1532(4) 0.2543(4) -0.4672(3) 0.0466(10) Uani 1 1 d . . . C21 C 0.7510(3) -0.0375(3) -0.0357(2) 0.0277(8) Uani 1 1 d . . . C22 C 0.6688(3) -0.0657(3) 0.0472(2) 0.0314(8) Uani 1 1 d . . . C23 C 0.6085(3) -0.1209(3) 0.0283(3) 0.0324(8) Uani 1 1 d . . . C24 C 0.6261(3) -0.1490(3) -0.0705(3) 0.0357(9) Uani 1 1 d . . . C25 C 0.7029(3) -0.1208(3) -0.1522(3) 0.0346(9) Uani 1 1 d . . . C26 C 0.7670(3) -0.0631(3) -0.1368(2) 0.0279(8) Uani 1 1 d . . . C27 C 0.8510(3) -0.0176(3) -0.1958(2) 0.0265(7) Uani 1 1 d . . . C28 C 0.8983(3) -0.0103(3) -0.3096(2) 0.0321(8) Uani 1 1 d . . . C29 C 0.8149(4) 0.0943(4) -0.3667(3) 0.0456(10) Uani 1 1 d . . . C51 C 0.6750(5) 0.3633(5) -0.0626(4) 0.0820(17) Uani 1 1 d . . . H51A H 0.6799 0.3268 0.0082 0.098 Uiso 1 1 calc R . . H51B H 0.6313 0.4486 -0.0596 0.098 Uiso 1 1 calc R . . C52 C 0.6110(5) 0.3235(5) -0.1037(6) 0.106(2) Uani 1 1 d . . . H52A H 0.5997 0.3652 -0.1711 0.158 Uiso 1 1 calc R . . H52B H 0.5312 0.3375 -0.0572 0.158 Uiso 1 1 calc R . . H52C H 0.6576 0.2399 -0.1112 0.158 Uiso 1 1 calc R . . C53 C 0.8013(4) 0.4174(4) -0.2168(4) 0.0706(14) Uani 1 1 d . . . H53A H 0.8791 0.3825 -0.2677 0.085 Uiso 1 1 calc R . . H53B H 0.7337 0.4353 -0.2496 0.085 Uiso 1 1 calc R . . C54 C 0.7912(5) 0.5229(5) -0.1888(5) 0.102(2) Uani 1 1 d . . . H54A H 0.7114 0.561 -0.143 0.153 Uiso 1 1 calc R . . H54B H 0.7997 0.5749 -0.251 0.153 Uiso 1 1 calc R . . H54C H 0.8557 0.505 -0.1533 0.153 Uiso 1 1 calc R . . O1 O 0.7973(2) 0.3336(2) -0.1272(2) 0.0608(8) Uani 1 1 d . . . Ag1 Ag 0.81581(2) 0.10216(2) 0.080958(19) 0.03188(8) Uani 1 1 d . . . Ag2 Ag 0.98435(2) 0.26637(2) 0.016343(19) 0.03193(8) Uani 1 1 d . . . Ag3 Ag 0.98627(2) 0.12791(2) -0.170724(19) 0.03176(8) Uani 1 1 d . . . N1 N 0.8852(2) 0.2512(2) 0.1660(2) 0.0296(7) Uani 1 1 d . . . N2 N 0.8004(2) 0.2067(3) 0.1877(2) 0.0308(7) Uani 1 1 d . . . N3 N 1.0949(2) 0.2738(2) -0.1301(2) 0.0289(6) Uani 1 1 d . . . N4 N 1.1036(2) 0.2144(2) -0.2058(2) 0.0290(7) Uani 1 1 d . . . N5 N 0.8209(2) 0.0168(2) -0.03538(19) 0.0276(6) Uani 1 1 d . . . N6 N 0.8803(2) 0.0294(2) -0.1350(2) 0.0268(6) Uani 1 1 d . . . F2 F 1.02689(18) 0.3659(2) 0.19141(15) 0.0450(6) Uani 1 1 d . . . F3 F 0.9625(2) 0.45508(19) 0.37650(16) 0.0483(6) Uani 1 1 d . . . F4 F 0.7763(2) 0.4386(2) 0.52409(15) 0.0496(6) Uani 1 1 d . . . F5 F 0.64534(18) 0.33353(19) 0.49644(14) 0.0434(5) Uani 1 1 d . . . F7 F 0.6156(2) 0.16026(19) 0.42335(14) 0.0477(6) Uani 1 1 d . . . F8 F 0.6428(2) 0.1088(2) 0.27292(16) 0.0530(6) Uani 1 1 d . . . F9 F 0.4151(2) 0.2606(3) 0.3418(2) 0.0736(8) Uani 1 1 d . . . F10 F 0.5100(2) 0.3324(3) 0.20988(19) 0.0715(8) Uani 1 1 d . . . F11 F 0.4759(2) 0.3837(2) 0.3603(2) 0.0622(7) Uani 1 1 d . . . F12 F 1.14117(19) 0.4175(2) -0.02108(15) 0.0450(6) Uani 1 1 d . . . F13 F 1.32134(19) 0.48751(19) -0.12239(16) 0.0456(6) Uani 1 1 d . . . F14 F 1.44863(19) 0.4267(2) -0.31160(16) 0.0484(6) Uani 1 1 d . . . F15 F 1.39923(19) 0.2993(2) -0.41206(15) 0.0493(6) Uani 1 1 d . . . F17 F 1.33656(19) 0.1209(2) -0.42502(16) 0.0505(6) Uani 1 1 d . . . F18 F 1.1762(2) 0.0835(2) -0.36377(16) 0.0527(6) Uani 1 1 d . . . F19 F 1.1863(2) 0.3411(2) -0.49277(16) 0.0564(6) Uani 1 1 d . . . F20 F 1.1817(3) 0.2027(2) -0.55142(17) 0.0707(8) Uani 1 1 d . . . F21 F 1.0330(2) 0.2966(3) -0.43283(18) 0.0718(8) Uani 1 1 d . . . F22 F 0.65070(18) -0.03767(18) 0.14195(14) 0.0391(5) Uani 1 1 d . . . F23 F 0.52836(18) -0.14883(19) 0.10537(15) 0.0443(5) Uani 1 1 d . . . F24 F 0.5613(2) -0.2028(2) -0.08353(17) 0.0529(6) Uani 1 1 d . . . F25 F 0.7147(2) -0.1465(2) -0.24611(16) 0.0520(6) Uani 1 1 d . . . F27 F 0.91719(19) -0.10689(18) -0.34840(15) 0.0420(5) Uani 1 1 d . . . F28 F 1.00699(19) -0.00396(19) -0.33268(15) 0.0435(5) Uani 1 1 d . . . F29 F 0.7053(2) 0.0957(2) -0.34510(18) 0.0669(7) Uani 1 1 d . . . F30 F 0.8049(3) 0.1915(2) -0.33948(18) 0.0681(7) Uani 1 1 d . . . F31 F 0.8579(2) 0.0924(2) -0.46783(16) 0.0643(7) 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 C1 0.0297(19) 0.0290(19) 0.0222(17) -0.0011(14) -0.0092(14) -0.0104(16) C2 0.0300(19) 0.036(2) 0.0256(18) -0.0036(16) -0.0016(15) -0.0130(17) C3 0.039(2) 0.035(2) 0.033(2) -0.0053(16) -0.0132(17) -0.0164(18) C4 0.054(2) 0.037(2) 0.0203(18) -0.0050(16) -0.0104(17) -0.018(2) C5 0.032(2) 0.038(2) 0.0192(17) -0.0030(15) 0.0001(15) -0.0125(17) C6 0.0276(18) 0.032(2) 0.0213(17) -0.0008(14) -0.0050(14) -0.0112(16) C7 0.0311(19) 0.036(2) 0.0210(17) -0.0036(15) -0.0014(15) -0.0162(17) C8 0.047(2) 0.048(2) 0.0215(18) -0.0079(17) 0.0037(16) -0.029(2) C9 0.038(2) 0.067(3) 0.045(2) -0.007(2) -0.0019(19) -0.029(2) C11 0.0276(19) 0.031(2) 0.0258(17) -0.0017(15) -0.0060(15) -0.0135(16) C12 0.032(2) 0.035(2) 0.0255(18) -0.0057(15) -0.0037(15) -0.0121(17) C13 0.034(2) 0.034(2) 0.036(2) -0.0012(16) -0.0146(17) -0.0150(18) C14 0.0285(19) 0.037(2) 0.036(2) 0.0046(17) -0.0066(16) -0.0190(18) C15 0.033(2) 0.040(2) 0.0277(19) 0.0005(16) -0.0026(16) -0.0195(18) C16 0.0281(18) 0.033(2) 0.0251(17) 0.0010(15) -0.0069(15) -0.0143(16) C17 0.0269(18) 0.036(2) 0.0241(17) -0.0041(15) -0.0011(14) -0.0151(17) C18 0.038(2) 0.044(2) 0.036(2) -0.0134(18) 0.0056(17) -0.025(2) C19 0.051(3) 0.063(3) 0.030(2) -0.013(2) -0.0025(19) -0.028(2) C21 0.0298(19) 0.0240(18) 0.0286(18) -0.0023(14) -0.0053(15) -0.0115(16) C22 0.037(2) 0.031(2) 0.0248(18) 0.0008(15) -0.0097(16) -0.0134(17) C23 0.031(2) 0.031(2) 0.035(2) 0.0024(16) -0.0049(16) -0.0165(17) C24 0.041(2) 0.031(2) 0.044(2) -0.0008(17) -0.0123(18) -0.0217(18) C25 0.038(2) 0.036(2) 0.034(2) -0.0052(17) -0.0094(17) -0.0164(18) C26 0.0306(19) 0.0288(19) 0.0255(17) -0.0043(15) -0.0058(15) -0.0131(16) C27 0.0287(18) 0.0237(18) 0.0258(17) -0.0031(14) -0.0053(15) -0.0101(15) C28 0.036(2) 0.037(2) 0.0253(18) -0.0059(16) 0.0010(16) -0.0202(18) C29 0.061(3) 0.044(3) 0.026(2) -0.0024(18) -0.0060(19) -0.019(2) C51 0.078(4) 0.073(4) 0.087(4) 0.019(3) -0.028(3) -0.030(3) C52 0.089(4) 0.082(4) 0.161(6) 0.017(4) -0.062(5) -0.040(4) C53 0.047(3) 0.066(4) 0.082(4) -0.015(3) -0.003(3) -0.012(3) C54 0.078(4) 0.091(5) 0.159(6) 0.003(4) -0.045(4) -0.048(4) O1 0.0337(16) 0.0450(18) 0.084(2) 0.0119(16) -0.0067(15) -0.0110(14) Ag1 0.03623(16) 0.03952(17) 0.02388(14) -0.00739(12) -0.00466(11) -0.01863(14) Ag2 0.03120(15) 0.04224(18) 0.02158(13) -0.00524(11) 0.00173(11) -0.01831(13) Ag3 0.03385(16) 0.03881(17) 0.02881(14) -0.00207(12) -0.00424(12) -0.02254(13) N1 0.0298(16) 0.0374(18) 0.0228(14) -0.0062(13) -0.0010(12) -0.0166(14) N2 0.0307(16) 0.0392(18) 0.0245(15) -0.0066(13) -0.0017(12) -0.0173(14) N3 0.0265(15) 0.0378(18) 0.0234(14) -0.0057(13) -0.0026(12) -0.0150(14) N4 0.0260(15) 0.0381(18) 0.0242(14) -0.0053(13) -0.0019(12) -0.0156(14) N5 0.0322(16) 0.0318(17) 0.0208(14) -0.0034(12) -0.0045(12) -0.0156(14) N6 0.0300(16) 0.0269(16) 0.0244(14) -0.0028(12) -0.0046(12) -0.0133(13) F2 0.0419(13) 0.0676(16) 0.0376(12) -0.0125(11) 0.0030(10) -0.0370(12) F3 0.0596(15) 0.0577(15) 0.0439(13) -0.0116(11) -0.0132(11) -0.0347(13) F4 0.0644(15) 0.0591(15) 0.0311(11) -0.0189(11) -0.0040(11) -0.0286(13) F5 0.0456(13) 0.0575(15) 0.0239(10) -0.0101(10) 0.0067(9) -0.0249(12) F7 0.0617(15) 0.0566(15) 0.0258(11) -0.0014(10) 0.0053(10) -0.0356(13) F8 0.0652(16) 0.0645(16) 0.0438(13) -0.0209(12) 0.0089(12) -0.0456(14) F9 0.0443(15) 0.103(2) 0.0834(19) -0.0090(16) 0.0019(13) -0.0492(16) F10 0.0510(16) 0.110(2) 0.0503(15) 0.0120(15) -0.0184(12) -0.0349(16) F11 0.0436(14) 0.0593(17) 0.0752(17) -0.0139(14) -0.0005(13) -0.0189(13) F12 0.0478(13) 0.0625(15) 0.0324(11) -0.0160(10) -0.0005(10) -0.0298(12) F13 0.0494(13) 0.0504(14) 0.0511(13) -0.0110(11) -0.0132(11) -0.0291(12) F14 0.0446(13) 0.0622(15) 0.0518(13) -0.0028(11) -0.0029(11) -0.0394(12) F15 0.0500(14) 0.0724(17) 0.0313(12) -0.0113(11) 0.0105(10) -0.0395(13) F17 0.0381(13) 0.0573(15) 0.0501(14) -0.0241(12) 0.0147(11) -0.0216(12) F18 0.0642(15) 0.0569(15) 0.0479(13) -0.0217(11) 0.0106(12) -0.0416(13) F19 0.0823(18) 0.0578(16) 0.0353(12) -0.0008(11) -0.0125(12) -0.0363(15) F20 0.104(2) 0.104(2) 0.0304(12) -0.0269(13) -0.0012(13) -0.0652(19) F21 0.0490(16) 0.119(2) 0.0444(14) -0.0063(15) -0.0145(12) -0.0302(16) F22 0.0457(13) 0.0502(14) 0.0232(10) -0.0011(9) -0.0036(9) -0.0251(11) F23 0.0436(13) 0.0502(14) 0.0443(12) 0.0038(10) -0.0031(10) -0.0315(12) F24 0.0630(15) 0.0626(16) 0.0577(14) -0.0119(12) -0.0086(12) -0.0476(14) F25 0.0690(16) 0.0704(17) 0.0383(12) -0.0162(11) -0.0074(11) -0.0459(14) F27 0.0548(14) 0.0405(13) 0.0348(11) -0.0135(10) -0.0050(10) -0.0223(11) F28 0.0433(13) 0.0614(15) 0.0307(11) -0.0134(10) 0.0049(10) -0.0301(12) F29 0.0507(16) 0.085(2) 0.0523(15) 0.0105(14) -0.0203(13) -0.0190(15) F30 0.109(2) 0.0366(14) 0.0497(15) 0.0010(12) -0.0189(14) -0.0237(15) F31 0.0840(19) 0.0681(17) 0.0243(12) 0.0022(11) -0.0096(12) -0.0218(15) #----------------------------------------------------------------------------# # 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 C1 N1 1.358(4) . ? C1 C2 1.401(5) . ? C1 C6 1.413(4) . ? C2 F2 1.346(4) . ? C2 C3 1.347(5) . ? C3 F3 1.332(4) . ? C3 C4 1.411(5) . ? C4 F4 1.344(4) . ? C4 C5 1.356(5) . ? C5 F5 1.340(4) . ? C5 C6 1.407(5) . ? C6 C7 1.406(5) . ? C7 N2 1.341(4) . ? C7 C8 1.490(5) . ? C8 F7 1.346(4) . ? C8 F8 1.357(4) . ? C8 C9 1.511(6) . ? C9 F9 1.319(4) . ? C9 F11 1.325(5) . ? C9 F10 1.336(4) . ? C11 N3 1.352(4) . ? C11 C12 1.398(5) . ? C11 C16 1.421(4) . ? C12 F12 1.341(4) . ? C12 C13 1.359(5) . ? C13 F13 1.332(4) . ? C13 C14 1.414(5) . ? C14 F14 1.336(4) . ? C14 C15 1.356(5) . ? C15 F15 1.335(4) . ? C15 C16 1.407(4) . ? C16 C17 1.407(5) . ? C17 N4 1.339(4) . ? C17 C18 1.495(5) . ? C18 F17 1.350(4) . ? C18 F18 1.355(4) . ? C18 C19 1.530(6) . ? C19 F19 1.317(4) . ? C19 F20 1.323(4) . ? C19 F21 1.327(4) . ? C21 N5 1.356(4) . ? C21 C22 1.406(4) . ? C21 C26 1.419(4) . ? C22 F22 1.341(4) . ? C22 C23 1.353(5) . ? C23 F23 1.347(4) . ? C23 C24 1.396(5) . ? C24 F24 1.354(4) . ? C24 C25 1.357(5) . ? C25 F25 1.337(4) . ? C25 C26 1.400(5) . ? C26 C27 1.412(4) . ? C27 N6 1.334(4) . ? C27 C28 1.491(4) . ? C28 F27 1.350(4) . ? C28 F28 1.352(4) . ? C28 C29 1.517(5) . ? C29 F29 1.320(5) . ? C29 F30 1.325(5) . ? C29 F31 1.327(4) . ? C51 C52 1.409(7) . ? C51 O1 1.456(5) . ? C51 H51A 0.99 . ? C51 H51B 0.99 . ? C52 H52A 0.98 . ? C52 H52B 0.98 . ? C52 H52C 0.98 . ? C53 C54 1.433(7) . ? C53 O1 1.462(5) . ? C53 H53A 0.99 . ? C53 H53B 0.99 . ? C54 H54A 0.98 . ? C54 H54B 0.98 . ? C54 H54C 0.98 . ? Ag1 N5 2.080(3) . ? Ag1 N2 2.094(3) . ? Ag1 Ag3 3.1857(4) 2_755 ? Ag2 N1 2.084(3) . ? Ag2 N3 2.090(3) . ? Ag3 N4 2.131(3) . ? Ag3 N6 2.135(3) . ? Ag3 Ag1 3.1857(4) 2_755 ? N1 N2 1.367(4) . ? N3 N4 1.358(4) . ? N5 N6 1.364(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 N1 C1 C2 128.7(3) . . ? N1 C1 C6 110.1(3) . . ? C2 C1 C6 121.2(3) . . ? F2 C2 C3 121.7(3) . . ? F2 C2 C1 119.3(3) . . ? C3 C2 C1 119.1(3) . . ? F3 C3 C2 121.0(3) . . ? F3 C3 C4 118.5(3) . . ? C2 C3 C4 120.4(3) . . ? F4 C4 C5 120.6(3) . . ? F4 C4 C3 117.8(3) . . ? C5 C4 C3 121.6(3) . . ? F5 C5 C4 119.7(3) . . ? F5 C5 C6 120.8(3) . . ? C4 C5 C6 119.4(3) . . ? C7 C6 C5 138.1(3) . . ? C7 C6 C1 103.7(3) . . ? C5 C6 C1 118.2(3) . . ? N2 C7 C6 109.6(3) . . ? N2 C7 C8 120.4(3) . . ? C6 C7 C8 129.9(3) . . ? F7 C8 F8 106.8(3) . . ? F7 C8 C7 110.9(3) . . ? F8 C8 C7 110.4(3) . . ? F7 C8 C9 107.9(3) . . ? F8 C8 C9 106.0(3) . . ? C7 C8 C9 114.5(3) . . ? F9 C9 F11 107.9(3) . . ? F9 C9 F10 107.9(3) . . ? F11 C9 F10 107.7(4) . . ? F9 C9 C8 112.3(4) . . ? F11 C9 C8 110.9(3) . . ? F10 C9 C8 110.0(3) . . ? N3 C11 C12 129.7(3) . . ? N3 C11 C16 109.8(3) . . ? C12 C11 C16 120.4(3) . . ? F12 C12 C13 120.6(3) . . ? F12 C12 C11 120.0(3) . . ? C13 C12 C11 119.4(3) . . ? F13 C13 C12 120.8(3) . . ? F13 C13 C14 118.8(3) . . ? C12 C13 C14 120.4(3) . . ? F14 C14 C15 121.1(3) . . ? F14 C14 C13 117.4(3) . . ? C15 C14 C13 121.5(3) . . ? F15 C15 C14 119.6(3) . . ? F15 C15 C16 121.1(3) . . ? C14 C15 C16 119.4(3) . . ? C17 C16 C15 137.9(3) . . ? C17 C16 C11 103.1(3) . . ? C15 C16 C11 118.9(3) . . ? N4 C17 C16 110.0(3) . . ? N4 C17 C18 120.6(3) . . ? C16 C17 C18 129.4(3) . . ? F17 C18 F18 107.5(3) . . ? F17 C18 C17 110.5(3) . . ? F18 C18 C17 110.8(3) . . ? F17 C18 C19 107.5(3) . . ? F18 C18 C19 106.2(3) . . ? C17 C18 C19 114.0(3) . . ? F19 C19 F20 107.8(3) . . ? F19 C19 F21 109.0(4) . . ? F20 C19 F21 107.9(3) . . ? F19 C19 C18 110.9(3) . . ? F20 C19 C18 111.4(3) . . ? F21 C19 C18 109.6(3) . . ? N5 C21 C22 128.7(3) . . ? N5 C21 C26 110.6(3) . . ? C22 C21 C26 120.6(3) . . ? F22 C22 C23 121.3(3) . . ? F22 C22 C21 120.4(3) . . ? C23 C22 C21 118.3(3) . . ? F23 C23 C22 120.2(3) . . ? F23 C23 C24 118.3(3) . . ? C22 C23 C24 121.4(3) . . ? F24 C24 C25 120.4(3) . . ? F24 C24 C23 118.0(3) . . ? C25 C24 C23 121.6(3) . . ? F25 C25 C24 119.7(3) . . ? F25 C25 C26 121.1(3) . . ? C24 C25 C26 119.1(3) . . ? C25 C26 C27 138.4(3) . . ? C25 C26 C21 118.9(3) . . ? C27 C26 C21 102.7(3) . . ? N6 C27 C26 109.9(3) . . ? N6 C27 C28 121.1(3) . . ? C26 C27 C28 128.9(3) . . ? F27 C28 F28 107.0(3) . . ? F27 C28 C27 110.5(3) . . ? F28 C28 C27 110.1(3) . . ? F27 C28 C29 107.9(3) . . ? F28 C28 C29 107.0(3) . . ? C27 C28 C29 114.0(3) . . ? F29 C29 F30 108.7(4) . . ? F29 C29 F31 108.2(3) . . ? F30 C29 F31 108.2(3) . . ? F29 C29 C28 110.3(3) . . ? F30 C29 C28 110.1(3) . . ? F31 C29 C28 111.3(3) . . ? C52 C51 O1 109.5(5) . . ? C52 C51 H51A 109.8 . . ? O1 C51 H51A 109.8 . . ? C52 C51 H51B 109.8 . . ? O1 C51 H51B 109.8 . . ? H51A C51 H51B 108.2 . . ? 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 . . ? C54 C53 O1 111.6(5) . . ? C54 C53 H53A 109.3 . . ? O1 C53 H53A 109.3 . . ? C54 C53 H53B 109.3 . . ? O1 C53 H53B 109.3 . . ? H53A C53 H53B 108 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C51 O1 C53 112.8(3) . . ? N5 Ag1 N2 173.12(11) . . ? N5 Ag1 Ag3 92.23(8) . 2_755 ? N2 Ag1 Ag3 94.37(8) . 2_755 ? N1 Ag2 N3 175.98(11) . . ? N4 Ag3 N6 175.77(10) . . ? N4 Ag3 Ag1 91.67(8) . 2_755 ? N6 Ag3 Ag1 84.30(7) . 2_755 ? C1 N1 N2 107.0(2) . . ? C1 N1 Ag2 129.8(2) . . ? N2 N1 Ag2 121.4(2) . . ? C7 N2 N1 109.6(3) . . ? C7 N2 Ag1 132.8(2) . . ? N1 N2 Ag1 117.03(19) . . ? C11 N3 N4 107.8(2) . . ? C11 N3 Ag2 130.6(2) . . ? N4 N3 Ag2 121.19(19) . . ? C17 N4 N3 109.3(3) . . ? C17 N4 Ag3 134.4(2) . . ? N3 N4 Ag3 116.26(18) . . ? C21 N5 N6 106.7(3) . . ? C21 N5 Ag1 129.1(2) . . ? N6 N5 Ag1 122.8(2) . . ? C27 N6 N5 110.0(3) . . ? C27 N6 Ag3 131.0(2) . . ? N5 N6 Ag3 118.7(2) . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF _database_code_depnum_ccdc_archive 'CCDC 929491' ####################################################################### # # 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_global #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_chiara210611 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C54 Cu5 F54 N12, C6 H16 N, C4 H10 O' _chemical_formula_sum 'C64 H26 Cu5 F54 N13 O' _chemical_formula_weight 2336.68 _chemical_compound_source 'synthesis as described' _chemical_absolute_configuration rm #----------------------------------------------------------------------------# # 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' _symmetry_Int_Tables_number 33 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 22.0065(12) _cell_length_b 13.1308(9) _cell_length_c 27.0131(19) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 7805.8(9) _cell_formula_units_Z 4 _cell_measurement_temperature 180(2) _cell_measurement_reflns_used 9801 _cell_measurement_theta_min 2.35 _cell_measurement_theta_max 23.9 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description cube _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.11 _exptl_crystal_density_diffrn 1.988 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4560 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.523 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.897 _exptl_absorpt_correction_T_max 0.991 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 180(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa APEX II' _diffrn_measurement_method \w-\f _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.0419 _diffrn_reflns_av_unetI/netI 0.0418 _diffrn_reflns_number 83406 _diffrn_reflns_limit_h_min -25 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -33 _diffrn_reflns_limit_l_max 33 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 26.37 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 15886 _reflns_number_gt 12135 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # 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. ; _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^)+(0.0790P)^2^+8.4485P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 15886 _refine_ls_number_parameters 1159 _refine_ls_number_restraints 30 _refine_ls_R_factor_all 0.0723 _refine_ls_R_factor_gt 0.0479 _refine_ls_wR_factor_ref 0.139 _refine_ls_wR_factor_gt 0.1226 _refine_ls_goodness_of_fit_ref 1.017 _refine_ls_restrained_S_all 1.022 _refine_ls_shift/su_max 0.01 _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 -0.013(11) _refine_diff_density_max 1.198 _refine_diff_density_min -0.667 _refine_diff_density_rms 0.099 #----------------------------------------------------------------------------# # 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' Cu Cu 0.3201 1.2651 '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 C1 C 0.4480(3) 0.8040(6) 0.8076(3) 0.0516(18) Uani 1 1 d . . . C2 C 0.4620(3) 0.9136(5) 0.7908(3) 0.0451(16) Uani 1 1 d . . . C3 C 0.5166(3) 0.9609(5) 0.8136(2) 0.0382(15) Uani 1 1 d . . . C4 C 0.5796(3) 0.9543(5) 0.8001(3) 0.0408(15) Uani 1 1 d . . . C5 C 0.6081(3) 1.0160(5) 0.8350(2) 0.0368(15) Uani 1 1 d . . . C6 C 0.6713(3) 1.0300(5) 0.8347(3) 0.0448(16) Uani 1 1 d . . . C7 C 0.7039(4) 0.9766(6) 0.8006(3) 0.058(2) Uani 1 1 d . . . C8 C 0.6753(4) 0.9138(6) 0.7651(3) 0.063(2) Uani 1 1 d . . . C9 C 0.6142(4) 0.9035(6) 0.7643(3) 0.0505(18) Uani 1 1 d . . . C11 C 0.4637(4) 1.3102(6) 0.7952(2) 0.0558(19) Uani 1 1 d . . . C12 C 0.4105(4) 1.2880(5) 0.8309(3) 0.0519(18) Uani 1 1 d . . . C13 C 0.4249(3) 1.2945(4) 0.8842(2) 0.0373(14) Uani 1 1 d . . . C14 C 0.4295(3) 1.3828(5) 0.9151(2) 0.0347(13) Uani 1 1 d . . . C15 C 0.4393(2) 1.3402(4) 0.9619(2) 0.0331(13) Uani 1 1 d . . . C16 C 0.4456(3) 1.4046(5) 1.0039(3) 0.0361(14) Uani 1 1 d . . . C17 C 0.4429(3) 1.5053(5) 0.9979(2) 0.0379(15) Uani 1 1 d . . . C18 C 0.4326(3) 1.5487(5) 0.9503(3) 0.0427(16) Uani 1 1 d . . . C19 C 0.4258(3) 1.4888(5) 0.9098(3) 0.0434(16) Uani 1 1 d . . . C21 C 0.5759(4) 0.7963(6) 1.1207(3) 0.0546(19) Uani 1 1 d . . . C22 C 0.5662(4) 0.9037(6) 1.1395(3) 0.0534(19) Uani 1 1 d . . . C23 C 0.5130(3) 0.9595(5) 1.1185(3) 0.0407(16) Uani 1 1 d . . . C24 C 0.4523(4) 0.9556(5) 1.1332(3) 0.0458(18) Uani 1 1 d . . . C25 C 0.4213(3) 1.0197(5) 1.0974(3) 0.0408(15) Uani 1 1 d . . . C26 C 0.3598(4) 1.0335(5) 1.0989(3) 0.0495(18) Uani 1 1 d . . . C27 C 0.3258(4) 0.9838(6) 1.1341(4) 0.066(2) Uani 1 1 d . . . C28 C 0.3557(4) 0.9228(6) 1.1695(3) 0.063(2) Uani 1 1 d . . . C29 C 0.4162(4) 0.9070(6) 1.1701(3) 0.057(2) Uani 1 1 d . . . C31 C 0.7652(3) 1.0953(5) 0.9910(3) 0.0494(18) Uani 1 1 d . . . C32 C 0.7396(3) 1.0007(5) 1.0152(3) 0.0477(17) Uani 1 1 d . . . C33 C 0.6915(3) 0.9462(4) 0.9860(3) 0.0376(14) Uani 1 1 d . . . C34 C 0.6980(3) 0.8778(5) 0.9460(2) 0.0372(14) Uani 1 1 d . . . C35 C 0.6375(3) 0.8556(4) 0.9333(2) 0.0352(15) Uani 1 1 d . . . C36 C 0.6247(3) 0.7890(5) 0.8929(3) 0.0405(15) Uani 1 1 d . . . C37 C 0.6714(4) 0.7480(5) 0.8676(3) 0.0490(18) Uani 1 1 d . . . C38 C 0.7314(3) 0.7726(5) 0.8797(3) 0.0493(18) Uani 1 1 d . . . C39 C 0.7448(3) 0.8333(5) 0.9177(3) 0.0498(19) Uani 1 1 d . . . C42 C 0.6220(4) 1.2806(6) 1.1030(3) 0.066(2) Uani 1 1 d D . . C43 C 0.6041(3) 1.2912(5) 1.0500(2) 0.0439(16) Uani 1 1 d . . . C44 C 0.6004(3) 1.3769(5) 1.0201(2) 0.0376(14) Uani 1 1 d . . . C45 C 0.5906(2) 1.3372(4) 0.9716(2) 0.0306(12) Uani 1 1 d . . . C46 C 0.5847(3) 1.3996(5) 0.9304(3) 0.0365(14) Uani 1 1 d . . . C47 C 0.5867(3) 1.5023(5) 0.9368(3) 0.0428(16) Uani 1 1 d . . . C48 C 0.5936(3) 1.5462(5) 0.9845(3) 0.0436(16) Uani 1 1 d . . . C49 C 0.6019(3) 1.4863(5) 1.0253(3) 0.0431(16) Uani 1 1 d . . . C51 C 0.2642(3) 1.1117(5) 0.9401(3) 0.052(2) Uani 1 1 d . . . C52 C 0.2899(3) 1.0140(5) 0.9153(3) 0.0434(16) Uani 1 1 d . . . C53 C 0.3365(3) 0.9562(5) 0.9461(3) 0.0400(16) Uani 1 1 d . . . C54 C 0.3282(3) 0.8894(5) 0.9852(3) 0.0386(15) Uani 1 1 d . . . C55 C 0.3875(3) 0.8632(4) 0.9983(3) 0.0378(15) Uani 1 1 d . . . C56 C 0.4003(3) 0.7983(5) 1.0378(3) 0.0395(15) Uani 1 1 d . . . C57 C 0.3527(3) 0.7593(5) 1.0647(3) 0.0451(16) Uani 1 1 d . . . C58 C 0.2927(3) 0.7843(6) 1.0522(3) 0.054(2) Uani 1 1 d . . . C59 C 0.2799(3) 0.8479(5) 1.0133(3) 0.0433(15) Uani 1 1 d . . . N1 N 0.5673(2) 1.0576(4) 0.8668(2) 0.0366(12) Uani 1 1 d . . . N2 N 0.5112(2) 1.0213(4) 0.8528(2) 0.0381(13) Uani 1 1 d . . . N3 N 0.4338(2) 1.2112(4) 0.91102(19) 0.0378(12) Uani 1 1 d . . . N4 N 0.4422(2) 1.2373(4) 0.95934(19) 0.0327(11) Uani 1 1 d . . . N5 N 0.4637(2) 1.0557(4) 1.0650(2) 0.0364(12) Uani 1 1 d . . . N6 N 0.5182(2) 1.0170(4) 1.07844(19) 0.0365(12) Uani 1 1 d . . . N7 N 0.6330(2) 0.9637(4) 0.9954(2) 0.0313(11) Uani 1 1 d . . . N8 N 0.5987(2) 0.9060(4) 0.9635(2) 0.0345(11) Uani 1 1 d . . . N9 N 0.5890(2) 1.2338(4) 0.97385(19) 0.0333(11) Uani 1 1 d . . . N10 N 0.5970(2) 1.2057(4) 1.02252(19) 0.0372(12) Uani 1 1 d . . . N11 N 0.4277(2) 0.9120(4) 0.9680(2) 0.0363(11) Uani 1 1 d . . . N12 N 0.3949(2) 0.9697(4) 0.9355(2) 0.0375(12) Uani 1 1 d . . . F1 F 0.4928(2) 0.7419(3) 0.79628(17) 0.0620(11) Uani 1 1 d . . . F2 F 0.3977(2) 0.7692(4) 0.78627(19) 0.0738(14) Uani 1 1 d . . . F3 F 0.4399(2) 0.8028(4) 0.85651(18) 0.0655(12) Uani 1 1 d . . . F4 F 0.4679(2) 0.9082(3) 0.74059(16) 0.0617(11) Uani 1 1 d . . . F5 F 0.41137(18) 0.9683(3) 0.80093(17) 0.0600(12) Uani 1 1 d . . . F6 F 0.69868(19) 1.0911(3) 0.86744(17) 0.0584(11) Uani 1 1 d . . . F7 F 0.7647(2) 0.9873(5) 0.7977(2) 0.0908(17) Uani 1 1 d . . . F8 F 0.7102(3) 0.8670(5) 0.7314(2) 0.0962(19) Uani 1 1 d . . . F9 F 0.5881(2) 0.8431(4) 0.73026(19) 0.0714(14) Uani 1 1 d . . . F11 F 0.4467(3) 1.3014(5) 0.74862(15) 0.0906(17) Uani 1 1 d . . . F12 F 0.4859(2) 1.3976(4) 0.80312(16) 0.0654(11) Uani 1 1 d . . . F13 F 0.5065(2) 1.2399(4) 0.80280(18) 0.0765(14) Uani 1 1 d . . . F14 F 0.38943(19) 1.1924(3) 0.81842(16) 0.0569(10) Uani 1 1 d . . . F15 F 0.3659(2) 1.3555(3) 0.81794(17) 0.0635(12) Uani 1 1 d . . . F16 F 0.45566(18) 1.3621(3) 1.04924(15) 0.0487(10) Uani 1 1 d . . . F17 F 0.44918(19) 1.5681(3) 1.03658(18) 0.0565(11) Uani 1 1 d . . . F18 F 0.4310(2) 1.6508(3) 0.94679(18) 0.0567(11) Uani 1 1 d . . . F19 F 0.4158(2) 1.5324(3) 0.86571(16) 0.0595(11) Uani 1 1 d . . . F21 F 0.6258(3) 0.7548(4) 1.1403(2) 0.0815(15) Uani 1 1 d . . . F22 F 0.58180(19) 0.7946(3) 1.07179(16) 0.0574(11) Uani 1 1 d . . . F23 F 0.5284(2) 0.7386(3) 1.13357(17) 0.0621(11) Uani 1 1 d . . . F24 F 0.6180(2) 0.9556(3) 1.12800(18) 0.0627(12) Uani 1 1 d . . . F25 F 0.5633(2) 0.9005(4) 1.18962(16) 0.0680(12) Uani 1 1 d . . . F26 F 0.3319(2) 1.0923(3) 1.06347(18) 0.0622(11) Uani 1 1 d . . . F27 F 0.2649(2) 0.9941(4) 1.1350(2) 0.0879(18) Uani 1 1 d . . . F28 F 0.3196(3) 0.8752(4) 1.2038(2) 0.0961(19) Uani 1 1 d . . . F29 F 0.4411(3) 0.8456(4) 1.20365(18) 0.0762(15) Uani 1 1 d . . . F31 F 0.80643(18) 1.1410(3) 1.0197(2) 0.0662(13) Uani 1 1 d . . . F32 F 0.79029(19) 1.0751(3) 0.94744(18) 0.0624(12) Uani 1 1 d . . . F33 F 0.72070(18) 1.1641(3) 0.9833(2) 0.0650(13) Uani 1 1 d . . . F34 F 0.71727(18) 1.0288(3) 1.06046(16) 0.0574(11) Uani 1 1 d . . . F35 F 0.78810(17) 0.9391(3) 1.02336(18) 0.0589(12) Uani 1 1 d . . . F36 F 0.56651(18) 0.7707(3) 0.88193(15) 0.0459(10) Uani 1 1 d . . . F37 F 0.6603(2) 0.6875(3) 0.82874(16) 0.0617(11) Uani 1 1 d . . . F38 F 0.7760(2) 0.7291(3) 0.8526(2) 0.0734(14) Uani 1 1 d . . . F39 F 0.80398(18) 0.8537(3) 0.9292(2) 0.0668(13) Uani 1 1 d . . . F41 F 0.5509(3) 1.3880(6) 1.1296(3) 0.1211(13) Uani 1 1 d DU . . F42 F 0.5273(4) 1.2281(6) 1.1292(3) 0.1211(13) Uani 1 1 d DU . . F44 F 0.6708(3) 1.3469(5) 1.1154(2) 0.104(2) Uani 1 1 d . . . F45 F 0.6441(6) 1.1870(5) 1.1140(2) 0.178(5) Uani 1 1 d . . . F46 F 0.57604(19) 1.3612(3) 0.88562(14) 0.0489(10) Uani 1 1 d . . . F47 F 0.5801(2) 1.5661(3) 0.89920(18) 0.0574(11) Uani 1 1 d . . . F48 F 0.59399(19) 1.6470(3) 0.98892(18) 0.0570(11) Uani 1 1 d . . . F49 F 0.6099(3) 1.5280(3) 1.06992(17) 0.0691(13) Uani 1 1 d . . . F51 F 0.22433(19) 1.1562(3) 0.91044(18) 0.0617(12) Uani 1 1 d . . . F52 F 0.30892(17) 1.1759(3) 0.94953(19) 0.0629(13) Uani 1 1 d . . . F53 F 0.23714(19) 1.0894(3) 0.98260(17) 0.0581(11) Uani 1 1 d . . . F54 F 0.24028(17) 0.9539(3) 0.90638(18) 0.0604(12) Uani 1 1 d . . . F55 F 0.31287(17) 1.0435(3) 0.87199(16) 0.0549(11) Uani 1 1 d . . . F56 F 0.45770(17) 0.7755(3) 1.04973(15) 0.0483(10) Uani 1 1 d . . . F57 F 0.3609(2) 0.6982(3) 1.10336(16) 0.0603(11) Uani 1 1 d . . . F58 F 0.2474(2) 0.7461(4) 1.0796(2) 0.0776(15) Uani 1 1 d . . . F59 F 0.22218(17) 0.8711(3) 1.0029(2) 0.0657(13) Uani 1 1 d . . . Cu1 Cu 0.57662(3) 1.14102(5) 0.92230(3) 0.03465(17) Uani 1 1 d . . . Cu2 Cu 0.45431(3) 1.14279(5) 1.01039(3) 0.03574(17) Uani 1 1 d . . . Cu3 Cu 0.44307(3) 1.06438(6) 0.89490(3) 0.03848(18) Uani 1 1 d . . . Cu4 Cu 0.51347(4) 0.91100(4) 0.96558(3) 0.03453(15) Uani 1 1 d . . . Cu5 Cu 0.58710(3) 1.05894(6) 1.03649(3) 0.03865(18) Uani 1 1 d . . . O2 O 0.3658(3) 0.4580(5) 0.1875(3) 0.0908(19) Uiso 1 1 d . . . N20 N 0.2249(4) 1.0551(6) 0.7378(3) 0.082(2) Uiso 1 1 d . . . H20 H 0.1941 1.0194 0.7217 0.099 Uiso 1 1 calc R . . C105 C 0.3503(7) 0.4186(10) 0.1391(5) 0.118(2) Uiso 1 1 d . . . H10A H 0.3757 0.4528 0.1139 0.142 Uiso 1 1 calc R . . H10B H 0.3073 0.4349 0.1319 0.142 Uiso 1 1 calc R . . C104 C 0.2402(7) 1.1416(10) 0.7039(5) 0.1239(18) Uiso 1 1 d . . . H10C H 0.2021 1.1766 0.6944 0.149 Uiso 1 1 calc R . . H10D H 0.2587 1.1137 0.6734 0.149 Uiso 1 1 calc R . . C102 C 0.1947(7) 1.0952(11) 0.7881(5) 0.1239(18) Uiso 1 1 d . . . H10E H 0.1758 1.037 0.8055 0.149 Uiso 1 1 calc R . . H10F H 0.2271 1.1227 0.8098 0.149 Uiso 1 1 calc R . . C106 C 0.3595(6) 0.3047(9) 0.1353(5) 0.118(2) Uiso 1 1 d . . . H10G H 0.4006 0.2873 0.1463 0.177 Uiso 1 1 calc R . . H10H H 0.354 0.2831 0.1009 0.177 Uiso 1 1 calc R . . H10I H 0.3297 0.2699 0.1564 0.177 Uiso 1 1 calc R . . C107 C 0.4290(6) 0.4495(10) 0.2057(5) 0.118(2) Uiso 1 1 d . . . H10J H 0.4473 0.3833 0.1965 0.142 Uiso 1 1 calc R . . H10K H 0.431 0.4581 0.2421 0.142 Uiso 1 1 calc R . . C108 C 0.4599(6) 0.5371(10) 0.1790(5) 0.118(2) Uiso 1 1 d . . . H10L H 0.4558 0.5278 0.1432 0.177 Uiso 1 1 calc R . . H10M H 0.503 0.5385 0.1879 0.177 Uiso 1 1 calc R . . H10N H 0.4407 0.6014 0.1888 0.177 Uiso 1 1 calc R . . C103 C 0.2689(7) 0.9727(10) 0.7571(5) 0.1239(18) Uiso 1 1 d D . . H10O H 0.3074 1.0054 0.7674 0.149 Uiso 1 1 calc R . . H10P H 0.2509 0.9395 0.7865 0.149 Uiso 1 1 calc R . . C111 C 0.2841(6) 1.2208(10) 0.7266(5) 0.1239(18) Uiso 1 1 d . . . H11A H 0.2732 1.2328 0.7613 0.186 Uiso 1 1 calc R . . H11B H 0.2812 1.2848 0.7081 0.186 Uiso 1 1 calc R . . H11C H 0.3258 1.195 0.7248 0.186 Uiso 1 1 calc R . . C109 C 0.1500(7) 1.1720(11) 0.7807(5) 0.1239(18) Uiso 1 1 d . . . H10Q H 0.1654 1.2227 0.7573 0.186 Uiso 1 1 calc R . . H10R H 0.141 1.2052 0.8124 0.186 Uiso 1 1 calc R . . H10S H 0.1129 1.1411 0.7675 0.186 Uiso 1 1 calc R . . C110 C 0.2819(7) 0.8958(10) 0.7196(5) 0.1239(18) Uiso 1 1 d D . . H11D H 0.2445 0.8794 0.7016 0.186 Uiso 1 1 calc R . . H11E H 0.2975 0.8342 0.7357 0.186 Uiso 1 1 calc R . . H11F H 0.3123 0.922 0.6965 0.186 Uiso 1 1 calc R . . C41 C 0.5730(4) 1.2969(8) 1.1368(4) 0.112(4) Uani 1 1 d DU . . F43 F 0.5904(3) 1.2938(6) 1.1859(3) 0.1211(13) Uani 1 1 d DU . . 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 C1 0.056(5) 0.043(4) 0.056(5) -0.012(4) -0.012(3) -0.004(3) C2 0.052(4) 0.036(4) 0.047(4) -0.005(3) -0.014(3) 0.008(3) C3 0.046(4) 0.033(3) 0.036(4) -0.004(3) 0.001(3) 0.003(3) C4 0.047(4) 0.033(3) 0.043(4) 0.001(3) 0.005(3) 0.005(3) C5 0.044(4) 0.029(3) 0.038(4) 0.012(3) 0.004(3) 0.008(3) C6 0.043(4) 0.045(4) 0.047(4) 0.004(3) 0.006(3) -0.003(3) C7 0.044(4) 0.059(5) 0.072(6) 0.005(4) 0.021(4) -0.001(4) C8 0.067(5) 0.059(5) 0.062(5) 0.003(4) 0.034(4) 0.008(4) C9 0.059(5) 0.046(4) 0.046(4) -0.004(3) 0.008(4) 0.005(3) C11 0.062(4) 0.071(5) 0.034(4) 0.009(3) -0.008(3) -0.004(4) C12 0.074(5) 0.042(4) 0.040(4) 0.005(3) -0.010(3) 0.010(3) C13 0.041(3) 0.028(3) 0.043(4) -0.003(3) -0.002(3) 0.002(2) C14 0.027(3) 0.037(3) 0.041(4) -0.003(3) 0.006(2) 0.006(2) C15 0.021(3) 0.037(3) 0.041(3) 0.000(3) 0.010(2) 0.003(2) C16 0.031(3) 0.035(3) 0.042(4) -0.002(3) 0.005(3) -0.002(2) C17 0.034(3) 0.034(3) 0.047(4) -0.009(3) 0.004(3) 0.001(2) C18 0.038(3) 0.029(3) 0.061(5) 0.001(3) 0.005(3) 0.003(3) C19 0.041(4) 0.039(4) 0.051(4) 0.005(3) 0.002(3) 0.002(3) C21 0.059(5) 0.055(5) 0.050(5) 0.008(4) -0.015(4) 0.013(4) C22 0.070(5) 0.047(4) 0.044(4) 0.013(3) -0.015(4) -0.011(4) C23 0.058(4) 0.024(3) 0.040(4) -0.001(3) 0.005(3) -0.004(3) C24 0.071(5) 0.035(4) 0.032(4) 0.000(3) 0.012(3) -0.005(3) C25 0.053(4) 0.027(3) 0.043(4) -0.008(3) 0.013(3) -0.001(3) C26 0.055(5) 0.039(4) 0.055(5) -0.010(3) 0.015(4) 0.001(3) C27 0.064(5) 0.048(4) 0.087(6) -0.024(4) 0.038(5) -0.008(4) C28 0.074(6) 0.049(4) 0.067(6) 0.013(4) 0.028(5) -0.003(4) C29 0.079(6) 0.050(4) 0.042(4) 0.003(3) 0.022(4) -0.006(4) C31 0.027(3) 0.052(4) 0.069(5) 0.014(4) -0.008(3) -0.002(3) C32 0.037(4) 0.044(4) 0.062(5) 0.006(3) -0.013(3) -0.002(3) C33 0.033(3) 0.031(3) 0.049(4) 0.009(3) -0.006(3) -0.001(2) C34 0.028(3) 0.036(3) 0.048(4) 0.010(3) 0.003(3) 0.002(2) C35 0.028(3) 0.026(3) 0.051(4) 0.012(3) 0.009(3) 0.003(2) C36 0.039(4) 0.033(3) 0.049(4) 0.010(3) -0.003(3) 0.000(3) C37 0.056(5) 0.034(4) 0.057(4) 0.008(3) 0.011(4) 0.002(3) C38 0.044(4) 0.042(4) 0.062(5) -0.002(3) 0.020(3) 0.002(3) C39 0.031(3) 0.039(4) 0.079(5) 0.013(4) 0.021(3) 0.004(3) C42 0.106(7) 0.046(4) 0.047(4) 0.000(4) -0.015(4) -0.007(4) C43 0.048(4) 0.042(4) 0.041(4) 0.002(3) -0.002(3) -0.009(3) C44 0.034(3) 0.033(3) 0.045(4) -0.002(3) 0.001(3) -0.002(2) C45 0.025(3) 0.028(3) 0.039(3) -0.002(3) 0.003(2) -0.004(2) C46 0.030(3) 0.037(3) 0.042(4) 0.001(3) 0.004(2) -0.005(2) C47 0.038(4) 0.040(4) 0.051(4) 0.009(3) 0.006(3) -0.001(3) C48 0.034(3) 0.026(3) 0.071(5) -0.001(3) 0.007(3) -0.002(2) C49 0.044(4) 0.036(3) 0.049(4) -0.012(3) 0.002(3) -0.011(3) C51 0.024(3) 0.034(3) 0.097(6) 0.001(4) -0.001(3) 0.001(3) C52 0.024(3) 0.047(4) 0.059(4) -0.009(3) -0.003(3) 0.001(3) C53 0.025(3) 0.039(3) 0.056(4) -0.011(3) 0.004(3) 0.003(3) C54 0.034(3) 0.024(3) 0.058(4) -0.009(3) 0.000(3) 0.001(2) C55 0.033(3) 0.027(3) 0.053(4) -0.018(3) 0.001(3) -0.002(2) C56 0.037(3) 0.025(3) 0.057(4) -0.002(3) -0.006(3) 0.003(2) C57 0.054(4) 0.035(3) 0.046(4) -0.007(3) 0.008(3) 0.002(3) C58 0.041(4) 0.041(4) 0.078(6) -0.008(4) 0.017(4) -0.007(3) C59 0.030(3) 0.036(3) 0.064(4) -0.009(3) 0.004(3) -0.006(2) N1 0.043(3) 0.029(3) 0.038(3) 0.001(2) 0.000(2) 0.003(2) N2 0.042(3) 0.037(3) 0.036(3) -0.004(2) 0.001(2) 0.001(2) N3 0.038(3) 0.036(3) 0.040(3) -0.003(2) -0.001(2) 0.002(2) N4 0.027(2) 0.032(3) 0.039(3) -0.002(2) 0.002(2) 0.0015(18) N5 0.038(3) 0.031(3) 0.039(3) -0.003(2) 0.000(2) 0.001(2) N6 0.042(3) 0.030(3) 0.038(3) 0.001(2) -0.002(2) -0.004(2) N7 0.028(3) 0.026(2) 0.039(3) 0.005(2) -0.003(2) 0.0021(19) N8 0.034(3) 0.023(2) 0.046(3) 0.005(2) -0.005(2) 0.0009(19) N9 0.029(2) 0.029(3) 0.042(3) -0.002(2) 0.005(2) 0.0013(18) N10 0.041(3) 0.032(3) 0.039(3) 0.003(2) -0.004(2) -0.006(2) N11 0.029(3) 0.029(2) 0.051(3) -0.006(2) 0.004(2) 0.000(2) N12 0.025(2) 0.032(3) 0.056(3) -0.003(2) -0.007(2) 0.002(2) F1 0.070(3) 0.040(2) 0.076(3) -0.010(2) -0.006(2) 0.002(2) F2 0.072(3) 0.066(3) 0.083(4) -0.014(3) -0.031(3) -0.013(2) F3 0.075(3) 0.065(3) 0.057(3) 0.005(2) -0.003(2) -0.012(2) F4 0.086(3) 0.052(3) 0.047(3) -0.004(2) -0.017(2) 0.002(2) F5 0.049(2) 0.058(3) 0.073(3) -0.018(2) -0.016(2) 0.016(2) F6 0.046(2) 0.061(3) 0.068(3) -0.007(2) 0.004(2) -0.0103(19) F7 0.052(3) 0.109(4) 0.111(4) -0.013(4) 0.033(3) 0.002(3) F8 0.082(4) 0.114(4) 0.093(4) -0.030(3) 0.044(3) 0.008(3) F9 0.088(4) 0.062(3) 0.064(3) -0.030(3) 0.009(2) 0.003(2) F11 0.141(5) 0.107(4) 0.023(2) -0.004(2) 0.000(3) -0.004(4) F12 0.088(3) 0.062(3) 0.047(2) 0.005(2) 0.010(2) -0.009(2) F13 0.084(3) 0.081(3) 0.064(3) 0.001(2) 0.025(2) 0.029(3) F14 0.060(2) 0.053(2) 0.058(3) -0.007(2) -0.018(2) -0.0047(19) F15 0.064(3) 0.067(3) 0.059(3) 0.008(2) -0.018(2) 0.006(2) F16 0.057(3) 0.048(2) 0.042(2) -0.0005(18) 0.0062(17) -0.0023(17) F17 0.068(3) 0.041(2) 0.061(3) -0.014(2) 0.006(2) -0.0022(18) F18 0.062(3) 0.0263(19) 0.081(3) -0.0041(19) -0.002(2) 0.0034(17) F19 0.079(3) 0.045(2) 0.054(3) 0.010(2) -0.012(2) 0.007(2) F21 0.086(4) 0.069(3) 0.090(4) 0.002(3) -0.031(3) 0.027(3) F22 0.063(3) 0.062(3) 0.047(3) -0.005(2) -0.0020(19) 0.011(2) F23 0.080(3) 0.044(2) 0.062(3) 0.012(2) -0.006(2) -0.002(2) F24 0.061(3) 0.053(3) 0.074(3) 0.014(2) -0.024(2) -0.002(2) F25 0.100(4) 0.064(3) 0.040(2) 0.000(2) -0.013(2) 0.009(3) F26 0.050(3) 0.055(2) 0.082(3) -0.007(2) 0.006(2) 0.011(2) F27 0.057(3) 0.083(4) 0.123(5) -0.011(3) 0.044(3) 0.003(3) F28 0.107(4) 0.083(3) 0.097(4) 0.014(3) 0.062(4) -0.011(3) F29 0.109(4) 0.072(3) 0.047(3) 0.020(2) 0.023(3) 0.003(3) F31 0.036(2) 0.058(3) 0.105(4) 0.005(2) -0.011(2) -0.0169(18) F32 0.039(2) 0.063(3) 0.085(3) 0.016(2) 0.010(2) -0.0067(18) F33 0.036(2) 0.044(2) 0.115(4) 0.021(2) -0.004(2) -0.0023(17) F34 0.043(2) 0.073(3) 0.056(3) 0.000(2) -0.0052(19) -0.0082(19) F35 0.035(2) 0.050(2) 0.092(3) 0.013(2) -0.019(2) 0.0039(16) F36 0.045(2) 0.035(2) 0.057(3) 0.0013(18) -0.0061(17) -0.0002(16) F37 0.070(3) 0.054(2) 0.062(3) -0.008(2) 0.012(2) 0.003(2) F38 0.061(3) 0.060(3) 0.100(4) -0.005(3) 0.039(3) 0.004(2) F39 0.029(2) 0.068(3) 0.103(4) 0.004(3) 0.015(2) 0.0034(18) F41 0.1221(14) 0.1212(14) 0.1198(14) 0.0003(6) 0.0000(6) -0.0012(6) F42 0.1221(14) 0.1212(14) 0.1198(14) 0.0003(6) 0.0000(6) -0.0012(6) F44 0.104(4) 0.142(5) 0.067(3) -0.024(3) -0.040(3) 0.015(4) F45 0.402(16) 0.066(4) 0.065(4) 0.004(3) -0.060(6) 0.052(6) F46 0.064(3) 0.047(2) 0.036(2) 0.0021(18) 0.0032(17) 0.0000(18) F47 0.072(3) 0.037(2) 0.064(3) 0.021(2) 0.001(2) -0.0038(18) F48 0.059(3) 0.031(2) 0.081(3) -0.004(2) 0.000(2) -0.0044(16) F49 0.112(4) 0.038(2) 0.057(3) -0.017(2) -0.006(3) -0.011(2) F51 0.046(2) 0.056(2) 0.083(3) -0.003(2) -0.011(2) 0.0191(19) F52 0.033(2) 0.041(2) 0.114(4) -0.016(2) 0.000(2) 0.0005(17) F53 0.045(2) 0.060(3) 0.070(3) -0.014(2) 0.008(2) 0.0080(19) F54 0.033(2) 0.052(2) 0.097(4) -0.018(2) -0.018(2) -0.0002(17) F55 0.042(2) 0.062(3) 0.061(3) -0.009(2) -0.0091(19) 0.0162(19) F56 0.043(2) 0.040(2) 0.062(3) -0.0008(18) -0.0102(17) 0.0021(16) F57 0.069(3) 0.055(3) 0.057(3) 0.007(2) 0.006(2) -0.001(2) F58 0.064(3) 0.062(3) 0.107(4) 0.008(3) 0.040(3) -0.011(2) F59 0.029(2) 0.063(3) 0.105(4) -0.002(3) 0.012(2) 0.0000(18) Cu1 0.0360(4) 0.0293(4) 0.0387(4) -0.0033(3) 0.0016(3) 0.0000(3) Cu2 0.0364(4) 0.0302(4) 0.0406(4) 0.0007(3) 0.0015(3) 0.0008(3) Cu3 0.0347(4) 0.0351(4) 0.0457(4) -0.0048(4) -0.0003(3) 0.0038(3) Cu4 0.0245(3) 0.0294(3) 0.0496(4) -0.0006(4) 0.0004(3) 0.0007(3) Cu5 0.0381(4) 0.0331(4) 0.0447(4) 0.0042(4) -0.0012(3) -0.0012(3) C41 0.112(4) 0.112(4) 0.111(4) -0.0001(10) -0.0007(10) -0.0007(10) F43 0.1221(14) 0.1212(14) 0.1198(14) 0.0003(6) 0.0000(6) -0.0012(6) #----------------------------------------------------------------------------# # 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 C1 F1 1.316(9) . ? C1 F2 1.328(8) . ? C1 F3 1.332(9) . ? C1 C2 1.541(11) . ? C2 F5 1.354(8) . ? C2 F4 1.364(9) . ? C2 C3 1.485(10) . ? C3 N2 1.329(8) . ? C3 C4 1.436(9) . ? C4 C5 1.393(10) . ? C4 C9 1.401(10) . ? C5 N1 1.356(8) . ? C5 C6 1.403(9) . ? C6 F6 1.339(8) . ? C6 C7 1.362(10) . ? C7 F7 1.347(9) . ? C7 C8 1.412(13) . ? C8 F8 1.339(9) . ? C8 C9 1.351(11) . ? C9 F9 1.344(9) . ? C11 F12 1.265(9) . ? C11 F11 1.319(8) . ? C11 F13 1.335(9) . ? C11 C12 1.544(11) . ? C12 F15 1.368(8) . ? C12 F14 1.380(8) . ? C12 C13 1.477(9) . ? C13 N3 1.325(8) . ? C13 C14 1.432(9) . ? C14 C15 1.399(9) . ? C14 C19 1.401(9) . ? C15 N4 1.354(8) . ? C15 C16 1.422(9) . ? C16 C17 1.334(9) . ? C16 F16 1.364(8) . ? C17 F17 1.339(7) . ? C17 C18 1.425(10) . ? C18 F18 1.344(7) . ? C18 C19 1.355(10) . ? C19 F19 1.339(8) . ? C21 F22 1.327(9) . ? C21 F21 1.336(9) . ? C21 F23 1.337(10) . ? C21 C22 1.514(11) . ? C22 F25 1.356(9) . ? C22 F24 1.364(9) . ? C22 C23 1.492(11) . ? C23 N6 1.325(8) . ? C23 C24 1.394(10) . ? C24 C29 1.426(10) . ? C24 C25 1.453(10) . ? C25 N5 1.365(8) . ? C25 C26 1.365(10) . ? C26 F26 1.375(9) . ? C26 C27 1.376(11) . ? C27 F27 1.349(9) . ? C27 C28 1.409(13) . ? C28 C29 1.347(12) . ? C28 F28 1.371(9) . ? C29 F29 1.330(10) . ? C31 F32 1.326(9) . ? C31 F31 1.336(8) . ? C31 F33 1.349(8) . ? C31 C32 1.514(10) . ? C32 F35 1.358(7) . ? C32 F34 1.367(9) . ? C32 C33 1.501(9) . ? C33 N7 1.332(8) . ? C33 C34 1.413(9) . ? C34 C35 1.405(9) . ? C34 C39 1.410(9) . ? C35 N8 1.354(8) . ? C35 C36 1.427(10) . ? C36 F36 1.337(7) . ? C36 C37 1.345(10) . ? C37 F37 1.339(9) . ? C37 C38 1.398(11) . ? C38 C39 1.334(11) . ? C38 F38 1.352(8) . ? C39 F39 1.364(8) . ? C42 F45 1.355(10) . ? C42 F44 1.423(10) . ? C42 C41 1.427(9) . ? C42 C43 1.491(10) . ? C43 N10 1.355(8) . ? C43 C44 1.388(9) . ? C44 C45 1.428(9) . ? C44 C49 1.443(9) . ? C45 N9 1.360(8) . ? C45 C46 1.388(9) . ? C46 F46 1.324(8) . ? C46 C47 1.360(9) . ? C47 F47 1.325(8) . ? C47 C48 1.419(10) . ? C48 F48 1.328(7) . ? C48 C49 1.367(10) . ? C49 F49 1.335(8) . ? C51 F52 1.320(8) . ? C51 F51 1.324(8) . ? C51 F53 1.327(9) . ? C51 C52 1.553(10) . ? C52 F55 1.332(8) . ? C52 F54 1.368(7) . ? C52 C53 1.523(9) . ? C53 N12 1.329(8) . ? C53 C54 1.387(10) . ? C54 C55 1.395(9) . ? C54 C59 1.415(10) . ? C55 N11 1.366(8) . ? C55 C56 1.393(10) . ? C56 F56 1.338(7) . ? C56 C57 1.373(10) . ? C57 F57 1.330(8) . ? C57 C58 1.403(10) . ? C58 F58 1.339(8) . ? C58 C59 1.372(11) . ? C59 F59 1.335(7) . ? N1 N2 1.376(7) . ? N1 Cu1 1.868(5) . ? N2 Cu3 1.965(5) . ? N3 N4 1.362(7) . ? N3 Cu3 1.988(5) . ? N4 Cu2 1.874(5) . ? N5 N6 1.354(7) . ? N5 Cu2 1.877(5) . ? N6 Cu5 1.971(5) . ? N7 N8 1.374(7) . ? N7 Cu5 1.953(5) . ? N8 Cu4 1.877(5) . ? N9 N10 1.377(7) . ? N9 Cu1 1.870(5) . ? N10 Cu5 1.976(5) . ? N11 N12 1.365(8) . ? N11 Cu4 1.889(5) . ? N12 Cu3 1.967(6) . ? F41 C41 1.306(8) . ? F42 C41 1.366(8) . ? O2 C105 1.445(14) . ? O2 C107 1.478(15) . ? N20 C104 1.496(15) . ? N20 C103 1.544(15) . ? N20 C102 1.602(16) . ? N20 H20 0.93 . ? C105 C106 1.513(17) . ? C105 H10A 0.99 . ? C105 H10B 0.99 . ? C104 C111 1.547(17) . ? C104 H10C 0.99 . ? C104 H10D 0.99 . ? C102 C109 1.422(18) . ? C102 H10E 0.99 . ? C102 H10F 0.99 . ? C106 H10G 0.98 . ? C106 H10H 0.98 . ? C106 H10I 0.98 . ? C107 C108 1.517(17) . ? C107 H10J 0.99 . ? C107 H10K 0.99 . ? C108 H10L 0.98 . ? C108 H10M 0.98 . ? C108 H10N 0.98 . ? C103 C110 1.458(9) . ? C103 H10O 0.99 . ? C103 H10P 0.99 . ? C111 H11A 0.98 . ? C111 H11B 0.98 . ? C111 H11C 0.98 . ? C109 H10Q 0.98 . ? C109 H10R 0.98 . ? C109 H10S 0.98 . ? C110 H11D 0.98 . ? C110 H11E 0.98 . ? C110 H11F 0.98 . ? C41 F43 1.381(8) . ? 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 F1 C1 F2 108.0(6) . . ? F1 C1 F3 108.9(6) . . ? F2 C1 F3 108.4(7) . . ? F1 C1 C2 111.0(6) . . ? F2 C1 C2 111.1(6) . . ? F3 C1 C2 109.3(6) . . ? F5 C2 F4 107.9(5) . . ? F5 C2 C3 111.1(6) . . ? F4 C2 C3 110.9(6) . . ? F5 C2 C1 105.7(6) . . ? F4 C2 C1 105.3(6) . . ? C3 C2 C1 115.5(6) . . ? N2 C3 C4 108.9(6) . . ? N2 C3 C2 120.6(6) . . ? C4 C3 C2 130.5(6) . . ? C5 C4 C9 120.0(7) . . ? C5 C4 C3 103.2(6) . . ? C9 C4 C3 136.8(7) . . ? N1 C5 C4 111.4(6) . . ? N1 C5 C6 127.5(6) . . ? C4 C5 C6 121.2(6) . . ? F6 C6 C7 121.2(7) . . ? F6 C6 C5 121.3(6) . . ? C7 C6 C5 117.4(7) . . ? F7 C7 C6 120.6(8) . . ? F7 C7 C8 117.7(7) . . ? C6 C7 C8 121.6(7) . . ? F8 C8 C9 120.9(8) . . ? F8 C8 C7 118.3(8) . . ? C9 C8 C7 120.8(7) . . ? F9 C9 C8 119.7(7) . . ? F9 C9 C4 121.4(7) . . ? C8 C9 C4 118.9(7) . . ? F12 C11 F11 110.5(6) . . ? F12 C11 F13 109.2(7) . . ? F11 C11 F13 106.6(7) . . ? F12 C11 C12 111.0(7) . . ? F11 C11 C12 111.4(7) . . ? F13 C11 C12 108.0(6) . . ? F15 C12 F14 106.6(6) . . ? F15 C12 C13 111.5(6) . . ? F14 C12 C13 111.3(6) . . ? F15 C12 C11 105.2(6) . . ? F14 C12 C11 105.9(6) . . ? C13 C12 C11 115.8(6) . . ? N3 C13 C14 109.9(5) . . ? N3 C13 C12 121.1(6) . . ? C14 C13 C12 129.0(6) . . ? C15 C14 C19 119.9(6) . . ? C15 C14 C13 102.2(5) . . ? C19 C14 C13 137.9(6) . . ? N4 C15 C14 111.2(6) . . ? N4 C15 C16 129.0(6) . . ? C14 C15 C16 119.9(6) . . ? C17 C16 F16 121.4(6) . . ? C17 C16 C15 119.2(6) . . ? F16 C16 C15 119.3(5) . . ? C16 C17 F17 120.8(6) . . ? C16 C17 C18 120.9(6) . . ? F17 C17 C18 118.4(5) . . ? F18 C18 C19 121.3(6) . . ? F18 C18 C17 117.8(6) . . ? C19 C18 C17 120.9(6) . . ? F19 C19 C18 119.2(6) . . ? F19 C19 C14 121.6(6) . . ? C18 C19 C14 119.2(6) . . ? F22 C21 F21 107.8(7) . . ? F22 C21 F23 109.0(6) . . ? F21 C21 F23 108.0(7) . . ? F22 C21 C22 111.3(6) . . ? F21 C21 C22 111.3(7) . . ? F23 C21 C22 109.3(7) . . ? F25 C22 F24 106.4(6) . . ? F25 C22 C23 110.9(7) . . ? F24 C22 C23 108.9(6) . . ? F25 C22 C21 108.2(6) . . ? F24 C22 C21 105.7(7) . . ? C23 C22 C21 116.1(6) . . ? N6 C23 C24 109.7(6) . . ? N6 C23 C22 121.5(6) . . ? C24 C23 C22 128.7(7) . . ? C23 C24 C29 138.6(8) . . ? C23 C24 C25 103.8(6) . . ? C29 C24 C25 117.5(7) . . ? N5 C25 C26 130.5(7) . . ? N5 C25 C24 107.9(6) . . ? C26 C25 C24 121.6(6) . . ? C25 C26 F26 119.9(6) . . ? C25 C26 C27 119.7(8) . . ? F26 C26 C27 120.3(8) . . ? F27 C27 C26 120.3(9) . . ? F27 C27 C28 120.7(8) . . ? C26 C27 C28 119.0(8) . . ? C29 C28 F28 119.5(8) . . ? C29 C28 C27 123.9(7) . . ? F28 C28 C27 116.5(8) . . ? F29 C29 C28 120.6(7) . . ? F29 C29 C24 121.2(8) . . ? C28 C29 C24 118.2(8) . . ? F32 C31 F31 108.9(6) . . ? F32 C31 F33 107.4(6) . . ? F31 C31 F33 106.4(6) . . ? F32 C31 C32 112.0(7) . . ? F31 C31 C32 111.8(6) . . ? F33 C31 C32 110.2(6) . . ? F35 C32 F34 107.4(6) . . ? F35 C32 C33 110.8(6) . . ? F34 C32 C33 110.2(6) . . ? F35 C32 C31 105.4(6) . . ? F34 C32 C31 107.4(6) . . ? C33 C32 C31 115.3(6) . . ? N7 C33 C34 110.7(5) . . ? N7 C33 C32 119.9(6) . . ? C34 C33 C32 129.4(6) . . ? C35 C34 C39 118.4(7) . . ? C35 C34 C33 102.8(5) . . ? C39 C34 C33 138.7(7) . . ? N8 C35 C34 110.5(6) . . ? N8 C35 C36 129.5(6) . . ? C34 C35 C36 119.9(6) . . ? F36 C36 C37 123.1(7) . . ? F36 C36 C35 117.9(6) . . ? C37 C36 C35 119.0(6) . . ? F37 C37 C36 119.8(7) . . ? F37 C37 C38 119.4(7) . . ? C36 C37 C38 120.6(7) . . ? C39 C38 F38 120.5(7) . . ? C39 C38 C37 121.9(6) . . ? F38 C38 C37 117.6(7) . . ? C38 C39 F39 120.3(6) . . ? C38 C39 C34 120.1(7) . . ? F39 C39 C34 119.5(7) . . ? F45 C42 F44 103.4(8) . . ? F45 C42 C41 105.5(8) . . ? F44 C42 C41 109.1(7) . . ? F45 C42 C43 113.0(7) . . ? F44 C42 C43 111.6(7) . . ? C41 C42 C43 113.6(8) . . ? N10 C43 C44 110.2(5) . . ? N10 C43 C42 118.6(6) . . ? C44 C43 C42 130.5(6) . . ? C43 C44 C45 104.3(5) . . ? C43 C44 C49 138.5(6) . . ? C45 C44 C49 117.1(6) . . ? N9 C45 C46 128.6(6) . . ? N9 C45 C44 109.1(5) . . ? C46 C45 C44 122.3(6) . . ? F46 C46 C47 120.0(6) . . ? F46 C46 C45 121.4(6) . . ? C47 C46 C45 118.7(6) . . ? F47 C47 C46 121.6(6) . . ? F47 C47 C48 116.8(6) . . ? C46 C47 C48 121.5(6) . . ? F48 C48 C49 120.0(7) . . ? F48 C48 C47 119.1(6) . . ? C49 C48 C47 120.8(6) . . ? F49 C49 C48 120.6(6) . . ? F49 C49 C44 120.0(6) . . ? C48 C49 C44 119.4(6) . . ? F52 C51 F51 109.2(6) . . ? F52 C51 F53 107.9(7) . . ? F51 C51 F53 108.8(5) . . ? F52 C51 C52 109.9(5) . . ? F51 C51 C52 110.2(6) . . ? F53 C51 C52 110.8(6) . . ? F55 C52 F54 108.5(6) . . ? F55 C52 C53 111.6(5) . . ? F54 C52 C53 110.3(6) . . ? F55 C52 C51 106.0(6) . . ? F54 C52 C51 105.2(5) . . ? C53 C52 C51 114.9(6) . . ? N12 C53 C54 112.1(6) . . ? N12 C53 C52 117.9(6) . . ? C54 C53 C52 130.0(6) . . ? C53 C54 C55 103.1(6) . . ? C53 C54 C59 138.7(6) . . ? C55 C54 C59 118.2(7) . . ? N11 C55 C56 128.0(6) . . ? N11 C55 C54 109.7(6) . . ? C56 C55 C54 122.3(6) . . ? F56 C56 C57 120.6(6) . . ? F56 C56 C55 120.8(6) . . ? C57 C56 C55 118.6(6) . . ? F57 C57 C56 122.5(7) . . ? F57 C57 C58 117.2(6) . . ? C56 C57 C58 120.3(7) . . ? F58 C58 C59 119.9(7) . . ? F58 C58 C57 118.7(8) . . ? C59 C58 C57 121.4(6) . . ? F59 C59 C58 119.7(6) . . ? F59 C59 C54 120.9(7) . . ? C58 C59 C54 119.3(6) . . ? C5 N1 N2 106.3(5) . . ? C5 N1 Cu1 132.1(5) . . ? N2 N1 Cu1 121.5(4) . . ? C3 N2 N1 110.3(5) . . ? C3 N2 Cu3 134.5(5) . . ? N1 N2 Cu3 115.2(4) . . ? C13 N3 N4 109.6(5) . . ? C13 N3 Cu3 134.1(4) . . ? N4 N3 Cu3 116.1(4) . . ? C15 N4 N3 107.0(5) . . ? C15 N4 Cu2 129.1(5) . . ? N3 N4 Cu2 123.9(4) . . ? N6 N5 C25 107.6(5) . . ? N6 N5 Cu2 122.5(4) . . ? C25 N5 Cu2 129.8(5) . . ? C23 N6 N5 110.9(5) . . ? C23 N6 Cu5 134.1(5) . . ? N5 N6 Cu5 115.0(4) . . ? C33 N7 N8 108.4(5) . . ? C33 N7 Cu5 136.0(4) . . ? N8 N7 Cu5 115.1(4) . . ? C35 N8 N7 107.5(5) . . ? C35 N8 Cu4 131.7(5) . . ? N7 N8 Cu4 120.8(4) . . ? C45 N9 N10 107.9(5) . . ? C45 N9 Cu1 128.3(4) . . ? N10 N9 Cu1 123.7(4) . . ? C43 N10 N9 108.4(5) . . ? C43 N10 Cu5 135.7(4) . . ? N9 N10 Cu5 115.4(4) . . ? N12 N11 C55 107.7(5) . . ? N12 N11 Cu4 120.6(4) . . ? C55 N11 Cu4 131.6(5) . . ? C53 N12 N11 107.4(5) . . ? C53 N12 Cu3 136.5(5) . . ? N11 N12 Cu3 115.1(4) . . ? N1 Cu1 N9 174.6(2) . . ? N4 Cu2 N5 175.4(2) . . ? N2 Cu3 N12 123.5(2) . . ? N2 Cu3 N3 119.0(2) . . ? N12 Cu3 N3 115.8(2) . . ? N8 Cu4 N11 178.38(18) . . ? N7 Cu5 N6 123.1(2) . . ? N7 Cu5 N10 117.3(2) . . ? N6 Cu5 N10 117.8(2) . . ? C105 O2 C107 119.7(10) . . ? C104 N20 C103 126.7(10) . . ? C104 N20 C102 111.3(9) . . ? C103 N20 C102 101.7(8) . . ? C104 N20 H20 105.1 . . ? C103 N20 H20 105.1 . . ? C102 N20 H20 105.1 . . ? O2 C105 C106 112.5(11) . . ? O2 C105 H10A 109.1 . . ? C106 C105 H10A 109.1 . . ? O2 C105 H10B 109.1 . . ? C106 C105 H10B 109.1 . . ? H10A C105 H10B 107.8 . . ? N20 C104 C111 114.1(11) . . ? N20 C104 H10C 108.7 . . ? C111 C104 H10C 108.7 . . ? N20 C104 H10D 108.7 . . ? C111 C104 H10D 108.7 . . ? H10C C104 H10D 107.6 . . ? C109 C102 N20 113.6(12) . . ? C109 C102 H10E 108.9 . . ? N20 C102 H10E 108.9 . . ? C109 C102 H10F 108.9 . . ? N20 C102 H10F 108.9 . . ? H10E C102 H10F 107.7 . . ? C105 C106 H10G 109.5 . . ? C105 C106 H10H 109.5 . . ? H10G C106 H10H 109.5 . . ? C105 C106 H10I 109.5 . . ? H10G C106 H10I 109.5 . . ? H10H C106 H10I 109.5 . . ? O2 C107 C108 101.9(10) . . ? O2 C107 H10J 111.4 . . ? C108 C107 H10J 111.4 . . ? O2 C107 H10K 111.4 . . ? C108 C107 H10K 111.4 . . ? H10J C107 H10K 109.3 . . ? C107 C108 H10L 109.5 . . ? C107 C108 H10M 109.5 . . ? H10L C108 H10M 109.5 . . ? C107 C108 H10N 109.5 . . ? H10L C108 H10N 109.5 . . ? H10M C108 H10N 109.5 . . ? C110 C103 N20 112.0(11) . . ? C110 C103 H10O 109.2 . . ? N20 C103 H10O 109.2 . . ? C110 C103 H10P 109.2 . . ? N20 C103 H10P 109.2 . . ? H10O C103 H10P 107.9 . . ? C104 C111 H11A 109.5 . . ? C104 C111 H11B 109.5 . . ? H11A C111 H11B 109.5 . . ? C104 C111 H11C 109.5 . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? C102 C109 H10Q 109.5 . . ? C102 C109 H10R 109.5 . . ? H10Q C109 H10R 109.5 . . ? C102 C109 H10S 109.5 . . ? H10Q C109 H10S 109.5 . . ? H10R C109 H10S 109.5 . . ? C103 C110 H11D 109.5 . . ? C103 C110 H11E 109.5 . . ? H11D C110 H11E 109.5 . . ? C103 C110 H11F 109.5 . . ? H11D C110 H11F 109.5 . . ? H11E C110 H11F 109.5 . . ? F41 C41 F42 108.0(9) . . ? F41 C41 F43 105.8(8) . . ? F42 C41 F43 109.1(8) . . ? F41 C41 C42 108.9(8) . . ? F42 C41 C42 111.2(9) . . ? F43 C41 C42 113.6(8) . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF _database_code_depnum_ccdc_archive 'CCDC 929492' ####################################################################### # # 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_global #------------------ SECTION 2. COMPOUND(S) DETAILS -------------------------# data_chiara250711 #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C8 H12 Cu N4, B F4' _chemical_formula_sum 'C8 H12 B Cu F4 N4' _chemical_formula_weight 314.58 _chemical_compound_source 'synthesis as described' _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' _symmetry_Int_Tables_number 33 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 23.705(5) _cell_length_b 8.276(5) _cell_length_c 20.188(5) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3961(3) _cell_formula_units_Z 12 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9984 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 35.6 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1896 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.688 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.876 _exptl_absorpt_correction_T_max 0.985 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_ambient_temperature 100(2) _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker Kappa APEX II' _diffrn_measurement_method \w-\f _diffrn_standards_number 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_av_R_equivalents 0.0213 _diffrn_reflns_av_unetI/netI 0.0239 _diffrn_reflns_number 95171 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 39 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 36.37 _diffrn_reflns_theta_full 25 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.943 _reflns_number_total 15924 _reflns_number_gt 14368 _reflns_threshold_expression >2\s(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SIR92 (Giacovazzo et al, 1993)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # 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. ; _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^)+(0.0307P)^2^+0.3447P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 15924 _refine_ls_number_parameters 498 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0293 _refine_ls_R_factor_gt 0.0238 _refine_ls_wR_factor_ref 0.0575 _refine_ls_wR_factor_gt 0.056 _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.004 _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 0.035(4) _refine_diff_density_max 0.472 _refine_diff_density_min -0.306 _refine_diff_density_rms 0.056 #----------------------------------------------------------------------------# # 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' Cu Cu 0.3201 1.2651 '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' 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 C1 C 0.38787(5) 0.07477(15) -0.09019(7) 0.0180(2) Uani 1 1 d . . . C2 C 0.36057(6) -0.00523(19) -0.14579(8) 0.0278(3) Uani 1 1 d . . . H2A H 0.3402 0.0749 -0.1723 0.042 Uiso 1 1 calc R . . H2B H 0.334 -0.0863 -0.1291 0.042 Uiso 1 1 calc R . . H2C H 0.3892 -0.0581 -0.1733 0.042 Uiso 1 1 calc R . . C3 C 0.57769(4) 0.08213(14) 0.02828(7) 0.01707(19) Uani 1 1 d . . . C4 C 0.63328(5) 0.00695(17) 0.03150(8) 0.0235(3) Uani 1 1 d . . . H4A H 0.6586 0.06 -0.0001 0.035 Uiso 1 1 calc R . . H4B H 0.6301 -0.108 0.0204 0.035 Uiso 1 1 calc R . . H4C H 0.6485 0.0183 0.0764 0.035 Uiso 1 1 calc R . . C5 C 0.39473(5) 0.06466(16) 0.14964(6) 0.0178(2) Uani 1 1 d . . . C6 C 0.36223(7) -0.02212(19) 0.19911(8) 0.0268(3) Uani 1 1 d . . . H6A H 0.3269 0.0357 0.2077 0.04 Uiso 1 1 calc R . . H6B H 0.3841 -0.0297 0.2402 0.04 Uiso 1 1 calc R . . H6C H 0.3538 -0.131 0.1829 0.04 Uiso 1 1 calc R . . C7 C 0.45434(5) 0.60020(14) 0.02650(8) 0.0178(2) Uani 1 1 d . . . C8 C 0.45596(5) 0.77593(15) 0.02574(10) 0.0214(2) Uani 1 1 d . . . H8A H 0.4181 0.818 0.0166 0.032 Uiso 1 1 calc R . . H8B H 0.482 0.8125 -0.0088 0.032 Uiso 1 1 calc R . . H8C H 0.4688 0.8156 0.0689 0.032 Uiso 1 1 calc R . . C9 C 0.60004(5) 0.56187(15) 0.31025(6) 0.0177(2) Uani 1 1 d . . . C10 C 0.62296(6) 0.48520(19) 0.36891(8) 0.0277(3) Uani 1 1 d . . . H10A H 0.6193 0.5585 0.4068 0.042 Uiso 1 1 calc R . . H10B H 0.6629 0.4601 0.3617 0.042 Uiso 1 1 calc R . . H10C H 0.6022 0.3852 0.3779 0.042 Uiso 1 1 calc R . . C11 C 0.60029(5) 0.56683(15) 0.06094(6) 0.0172(2) Uani 1 1 d . . . C12 C 0.63400(6) 0.50182(18) 0.00699(7) 0.0240(3) Uani 1 1 d . . . H12A H 0.6683 0.5665 0.0019 0.036 Uiso 1 1 calc R . . H12B H 0.6121 0.5054 -0.0342 0.036 Uiso 1 1 calc R . . H12C H 0.6442 0.3897 0.0169 0.036 Uiso 1 1 calc R . . C13 C 0.41812(5) 0.56353(15) 0.20414(6) 0.0179(2) Uani 1 1 d . . . C14 C 0.36340(6) 0.48798(18) 0.21613(8) 0.0255(3) Uani 1 1 d . . . H14A H 0.3492 0.5214 0.2596 0.038 Uiso 1 1 calc R . . H14B H 0.3676 0.3702 0.2151 0.038 Uiso 1 1 calc R . . H14C H 0.3367 0.5217 0.1817 0.038 Uiso 1 1 calc R . . C15 C 0.54042(5) 1.08414(16) 0.19247(7) 0.0182(2) Uani 1 1 d . . . C16 C 0.54023(5) 1.25941(16) 0.19620(8) 0.0220(3) Uani 1 1 d . . . H16A H 0.5272 1.2933 0.2401 0.033 Uiso 1 1 calc R . . H16B H 0.5148 1.303 0.1623 0.033 Uiso 1 1 calc R . . H16C H 0.5785 1.3002 0.1887 0.033 Uiso 1 1 calc R . . C17 C 0.72928(5) 0.70498(15) 0.23345(7) 0.0188(2) Uani 1 1 d . . . C18 C 0.70243(6) 0.6771(2) 0.17007(7) 0.0273(3) Uani 1 1 d . . . H18A H 0.6666 0.7363 0.1683 0.041 Uiso 1 1 d . . . H18B H 0.6952 0.5614 0.1645 0.041 Uiso 1 1 d . . . H18C H 0.7272 0.7151 0.1345 0.041 Uiso 1 1 d . . . C19 C 0.72783(5) 0.69964(14) 0.49476(7) 0.0177(2) Uani 1 1 d . . . C20 C 0.70084(6) 0.66667(18) 0.55774(7) 0.0229(2) Uani 1 1 d . . . H20A H 0.7232 0.5874 0.5824 0.034 Uiso 1 1 calc R . . H20B H 0.6629 0.6234 0.55 0.034 Uiso 1 1 calc R . . H20C H 0.6981 0.7669 0.5834 0.034 Uiso 1 1 calc R . . C21 C 0.78870(5) 1.17883(14) 0.36440(9) 0.01635(19) Uani 1 1 d . . . C22 C 0.78911(5) 1.35488(15) 0.36345(9) 0.0216(2) Uani 1 1 d . . . H22A H 0.8281 1.3935 0.3613 0.032 Uiso 1 1 calc R . . H22B H 0.7712 1.396 0.4038 0.032 Uiso 1 1 calc R . . H22C H 0.7683 1.3935 0.3246 0.032 Uiso 1 1 calc R . . C23 C 0.91588(5) 0.70860(14) 0.36000(7) 0.0175(2) Uani 1 1 d . . . C24 C 0.97650(5) 0.68399(18) 0.35569(7) 0.0248(3) Uani 1 1 d . . . H24A H 0.988 0.6833 0.3091 0.037 Uiso 1 1 calc R . . H24B H 0.9864 0.5804 0.3762 0.037 Uiso 1 1 calc R . . H24C H 0.996 0.7717 0.3789 0.037 Uiso 1 1 calc R . . N1 N 0.41049(4) 0.13671(14) -0.04729(6) 0.0186(2) Uani 1 1 d . . . N2 N 0.53418(4) 0.14058(13) 0.02594(6) 0.01899(18) Uani 1 1 d . . . N3 N 0.41943(4) 0.13220(14) 0.10995(6) 0.0195(2) Uani 1 1 d . . . N4 N 0.45335(4) 0.46234(13) 0.02739(7) 0.02012(19) Uani 1 1 d . . . N5 N 0.58111(4) 0.62238(14) 0.26446(6) 0.0187(2) Uani 1 1 d . . . N6 N 0.57497(4) 0.61972(14) 0.10381(5) 0.0183(2) Uani 1 1 d . . . N7 N 0.46064(4) 0.62320(13) 0.19510(5) 0.0201(2) Uani 1 1 d . . . N8 N 0.54013(5) 0.94634(14) 0.18906(7) 0.0210(2) Uani 1 1 d . . . N9 N 0.75050(4) 0.72742(14) 0.28338(6) 0.0201(2) Uani 1 1 d . . . N10 N 0.74950(4) 0.72526(14) 0.44561(6) 0.0197(2) Uani 1 1 d . . . N11 N 0.78843(4) 1.04165(13) 0.36512(7) 0.01854(18) Uani 1 1 d . . . N12 N 0.86844(4) 0.72982(12) 0.36350(6) 0.01898(18) Uani 1 1 d . . . F1 F 0.32539(4) 0.73587(17) -0.02893(5) 0.0447(3) Uani 1 1 d . . . F2 F 0.32263(4) 0.71772(12) 0.08319(5) 0.0327(2) Uani 1 1 d . . . F3 F 0.24169(3) 0.70330(11) 0.02292(5) 0.02973(19) Uani 1 1 d . . . F4 F 0.28881(5) 0.93913(12) 0.03292(7) 0.0478(3) Uani 1 1 d . . . F5 F 0.32114(4) 0.71645(12) 0.63981(5) 0.0313(2) Uani 1 1 d . . . F6 F 0.24248(4) 0.72808(17) 0.70395(5) 0.0460(3) Uani 1 1 d . . . F7 F 0.32753(4) 0.71921(15) 0.75200(5) 0.0402(3) Uani 1 1 d . . . F8 F 0.30088(7) 0.94285(13) 0.69581(7) 0.0634(4) Uani 1 1 d . . . F9 F 1.06991(4) 0.69821(15) 0.80542(6) 0.0436(3) Uani 1 1 d . . . F10 F 1.06978(4) 0.69985(13) 0.91732(6) 0.0379(2) Uani 1 1 d . . . F11 F 1.04765(5) 0.92688(14) 0.86063(8) 0.0568(3) Uani 1 1 d . . . F12 F 0.98731(3) 0.71442(12) 0.86132(6) 0.0356(2) Uani 1 1 d . . . Cu1 Cu 0.455340(6) 0.22481(2) 0.028552(9) 0.01694(3) Uani 1 1 d . . . Cu2 Cu 0.539211(6) 0.70732(2) 0.185187(8) 0.01699(3) Uani 1 1 d . . . Cu3 Cu 0.788535(6) 0.800521(18) 0.365201(9) 0.01624(3) Uani 1 1 d . . . B1 B 0.29482(6) 0.7748(2) 0.02709(10) 0.0198(2) Uani 1 1 d . . . B2 B 0.29794(7) 0.7785(2) 0.69813(8) 0.0195(3) Uani 1 1 d . . . B3 B 1.04359(6) 0.7627(2) 0.86162(11) 0.0213(3) 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 C1 0.0146(5) 0.0154(5) 0.0239(6) 0.0018(4) -0.0004(4) 0.0008(4) C2 0.0246(6) 0.0256(7) 0.0333(9) -0.0068(5) -0.0086(6) -0.0017(5) C3 0.0178(4) 0.0178(5) 0.0156(5) 0.0000(4) 0.0011(4) -0.0030(3) C4 0.0154(5) 0.0232(6) 0.0318(8) -0.0020(5) -0.0008(5) 0.0029(4) C5 0.0166(5) 0.0182(6) 0.0186(6) 0.0005(4) -0.0008(4) 0.0036(4) C6 0.0319(7) 0.0259(7) 0.0226(7) 0.0035(5) 0.0074(5) -0.0017(5) C7 0.0170(4) 0.0186(5) 0.0177(5) 0.0001(5) -0.0024(4) -0.0005(4) C8 0.0250(5) 0.0142(5) 0.0249(6) 0.0016(5) -0.0025(5) -0.0008(4) C9 0.0195(5) 0.0162(5) 0.0175(6) -0.0026(4) 0.0004(4) 0.0025(4) C10 0.0386(7) 0.0288(7) 0.0157(6) 0.0018(6) -0.0044(6) 0.0116(6) C11 0.0182(5) 0.0168(5) 0.0165(6) 0.0005(4) -0.0010(4) -0.0022(4) C12 0.0284(6) 0.0242(6) 0.0196(7) -0.0029(5) 0.0073(5) 0.0017(5) C13 0.0210(5) 0.0178(5) 0.0148(5) -0.0010(4) 0.0007(4) 0.0026(4) C14 0.0223(6) 0.0277(7) 0.0264(7) -0.0010(5) 0.0045(5) -0.0044(5) C15 0.0188(5) 0.0204(6) 0.0155(6) -0.0008(5) -0.0002(4) 0.0001(4) C16 0.0244(6) 0.0172(6) 0.0244(8) -0.0014(5) 0.0012(5) -0.0009(4) C17 0.0176(5) 0.0209(6) 0.0180(6) 0.0009(4) 0.0001(4) -0.0017(4) C18 0.0265(6) 0.0387(8) 0.0166(7) -0.0001(5) -0.0045(5) -0.0091(6) C19 0.0162(5) 0.0160(5) 0.0209(6) -0.0020(4) -0.0011(4) 0.0023(4) C20 0.0233(5) 0.0261(6) 0.0194(6) 0.0007(5) 0.0056(5) 0.0011(5) C21 0.0170(4) 0.0173(5) 0.0147(5) -0.0009(5) 0.0004(4) -0.0003(4) C22 0.0280(5) 0.0130(5) 0.0238(6) 0.0003(6) 0.0015(5) 0.0000(4) C23 0.0203(5) 0.0175(5) 0.0145(5) 0.0015(4) 0.0000(4) -0.0007(4) C24 0.0150(5) 0.0330(7) 0.0264(8) 0.0058(5) 0.0010(4) 0.0015(5) N1 0.0164(4) 0.0184(5) 0.0210(5) 0.0011(4) 0.0005(4) -0.0003(4) N2 0.0185(4) 0.0198(4) 0.0187(5) 0.0007(4) 0.0008(4) -0.0009(3) N3 0.0189(4) 0.0206(5) 0.0191(5) 0.0009(4) 0.0009(4) 0.0028(4) N4 0.0207(4) 0.0179(5) 0.0217(5) 0.0003(5) -0.0019(4) 0.0000(4) N5 0.0198(4) 0.0182(5) 0.0182(5) -0.0007(4) 0.0004(4) 0.0017(4) N6 0.0164(4) 0.0212(5) 0.0173(5) 0.0001(4) -0.0010(3) -0.0002(4) N7 0.0197(4) 0.0226(5) 0.0181(6) -0.0004(4) 0.0009(3) 0.0026(4) N8 0.0235(5) 0.0191(5) 0.0203(5) 0.0021(5) -0.0008(4) 0.0012(4) N9 0.0209(5) 0.0183(5) 0.0210(5) -0.0018(4) -0.0023(4) 0.0007(4) N10 0.0206(5) 0.0168(5) 0.0218(5) 0.0001(4) 0.0015(4) 0.0010(4) N11 0.0199(4) 0.0181(5) 0.0176(5) -0.0001(5) 0.0002(4) -0.0001(4) N12 0.0195(4) 0.0183(5) 0.0191(5) -0.0003(4) -0.0011(4) 0.0004(3) F1 0.0273(5) 0.0831(9) 0.0237(5) -0.0167(5) 0.0072(4) 0.0009(5) F2 0.0353(5) 0.0362(5) 0.0266(5) 0.0023(4) -0.0107(4) -0.0015(4) F3 0.0232(3) 0.0412(5) 0.0248(4) -0.0025(4) -0.0016(3) -0.0097(3) F4 0.0583(6) 0.0202(4) 0.0647(8) 0.0012(5) -0.0067(6) -0.0014(4) F5 0.0380(5) 0.0332(5) 0.0228(5) -0.0032(4) 0.0065(4) 0.0026(4) F6 0.0235(4) 0.0868(8) 0.0276(5) 0.0093(5) 0.0002(4) -0.0103(5) F7 0.0354(5) 0.0615(7) 0.0239(5) 0.0047(5) -0.0079(4) 0.0123(5) F8 0.1141(11) 0.0164(4) 0.0595(9) 0.0001(5) 0.0241(7) -0.0014(6) F9 0.0340(5) 0.0649(8) 0.0319(6) -0.0061(5) 0.0087(4) 0.0052(5) F10 0.0318(5) 0.0502(7) 0.0316(5) 0.0123(4) -0.0078(4) 0.0009(4) F11 0.0741(8) 0.0226(5) 0.0738(9) 0.0046(5) -0.0112(8) -0.0013(5) F12 0.0206(3) 0.0524(6) 0.0340(5) 0.0011(5) -0.0009(4) -0.0026(3) Cu1 0.01687(6) 0.01543(6) 0.01852(8) 0.00022(7) 0.00052(6) -0.00012(5) Cu2 0.01798(6) 0.01714(8) 0.01586(7) 0.00036(6) 0.00066(5) 0.00207(5) Cu3 0.01698(6) 0.01562(7) 0.01611(7) -0.00073(6) -0.00108(5) 0.00014(5) B1 0.0197(5) 0.0214(6) 0.0182(6) -0.0017(6) 0.0020(6) 0.0003(5) B2 0.0216(6) 0.0189(6) 0.0181(7) -0.0001(5) 0.0003(5) 0.0000(5) B3 0.0220(6) 0.0202(8) 0.0218(7) -0.0001(5) -0.0006(6) -0.0007(5) #----------------------------------------------------------------------------# # 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 C1 N1 1.1403(17) . ? C1 C2 1.4549(19) . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 N2 1.1401(14) . ? C3 C4 1.4588(16) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 N3 1.1390(17) . ? C5 C6 1.4516(19) . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 N4 1.1413(17) . ? C7 C8 1.4549(19) . ? C8 H8A 0.98 . ? C8 H8B 0.98 . ? C8 H8C 0.98 . ? C9 N5 1.1429(17) . ? C9 C10 1.4493(19) . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 N6 1.1406(16) . ? C11 C12 1.4540(19) . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 N7 1.1372(16) . ? C13 C14 1.4602(18) . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 N8 1.1425(19) . ? C15 C16 1.453(2) . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 N9 1.1418(17) . ? C17 C18 1.4475(19) . ? C18 H18A 0.9807 . ? C18 H18B 0.9793 . ? C18 H18C 0.98 . ? C19 N10 1.1372(18) . ? C19 C20 1.4493(19) . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 N11 1.1354(17) . ? C21 C22 1.4571(19) . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 N12 1.1405(15) . ? C23 C24 1.4538(16) . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? N1 Cu1 2.0016(12) . ? N2 Cu1 1.9954(10) . ? N3 Cu1 2.0031(12) . ? N4 Cu1 1.9664(16) . ? N5 Cu2 2.0105(12) . ? N6 Cu2 1.9857(12) . ? N7 Cu2 1.9984(11) . ? N8 Cu2 1.9798(17) . ? N9 Cu3 1.9767(12) . ? N10 Cu3 1.9696(12) . ? N11 Cu3 1.9956(16) . ? N12 Cu3 1.9828(10) . ? F1 B1 1.381(2) . ? F2 B1 1.393(2) . ? F3 B1 1.3942(16) . ? F4 B1 1.372(2) . ? F5 B2 1.3972(19) . ? F6 B2 1.3843(19) . ? F7 B2 1.3840(19) . ? F8 B2 1.363(2) . ? F9 B3 1.400(2) . ? F10 B3 1.386(2) . ? F11 B3 1.362(2) . ? F12 B3 1.3926(17) . ? 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 N1 C1 C2 178.36(14) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 C4 179.78(16) . . ? C3 C4 H4A 109.5 . . ? C3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C3 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 C6 178.68(15) . . ? C5 C6 H6A 109.5 . . ? C5 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C5 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N4 C7 C8 179.55(18) . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? N5 C9 C10 178.88(13) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? N6 C11 C12 178.36(14) . . ? 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 . . ? N7 C13 C14 179.53(15) . . ? 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 . . ? N8 C15 C16 179.30(16) . . ? 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 . . ? N9 C17 C18 179.80(17) . . ? C17 C18 H18A 109.4 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.4 . . ? H18B C18 H18C 109.5 . . ? N10 C19 C20 179.35(14) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? N11 C21 C22 179.9(2) . . ? 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 . . ? N12 C23 C24 179.19(14) . . ? 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 . . ? C1 N1 Cu1 173.99(11) . . ? C3 N2 Cu1 173.92(11) . . ? C5 N3 Cu1 169.53(11) . . ? C7 N4 Cu1 177.44(10) . . ? C9 N5 Cu2 172.25(11) . . ? C11 N6 Cu2 172.99(10) . . ? C13 N7 Cu2 173.44(11) . . ? C15 N8 Cu2 178.77(14) . . ? C17 N9 Cu3 171.30(11) . . ? C19 N10 Cu3 171.99(11) . . ? C21 N11 Cu3 179.21(14) . . ? C23 N12 Cu3 171.33(10) . . ? N4 Cu1 N2 111.80(4) . . ? N4 Cu1 N1 110.02(5) . . ? N2 Cu1 N1 110.49(5) . . ? N4 Cu1 N3 112.46(5) . . ? N2 Cu1 N3 106.62(5) . . ? N1 Cu1 N3 105.22(5) . . ? N8 Cu2 N6 113.13(5) . . ? N8 Cu2 N7 110.76(5) . . ? N6 Cu2 N7 110.70(5) . . ? N8 Cu2 N5 108.21(5) . . ? N6 Cu2 N5 108.66(5) . . ? N7 Cu2 N5 105.00(5) . . ? N10 Cu3 N9 112.19(5) . . ? N10 Cu3 N12 111.70(5) . . ? N9 Cu3 N12 109.32(5) . . ? N10 Cu3 N11 108.44(5) . . ? N9 Cu3 N11 107.74(5) . . ? N12 Cu3 N11 107.24(4) . . ? F4 B1 F1 110.86(15) . . ? F4 B1 F2 108.39(15) . . ? F1 B1 F2 109.76(12) . . ? F4 B1 F3 109.41(12) . . ? F1 B1 F3 108.99(14) . . ? F2 B1 F3 109.42(14) . . ? F8 B2 F7 110.78(15) . . ? F8 B2 F6 110.62(14) . . ? F7 B2 F6 107.92(13) . . ? F8 B2 F5 108.53(14) . . ? F7 B2 F5 109.41(13) . . ? F6 B2 F5 109.56(13) . . ? F11 B3 F10 110.76(15) . . ? F11 B3 F12 110.72(13) . . ? F10 B3 F12 108.96(15) . . ? F11 B3 F9 109.68(16) . . ? F10 B3 F9 108.35(13) . . ? F12 B3 F9 108.30(14) . . ? # The following lines are used to test the character set of files sent by # network email or other means. They are not part of the CIF data set # abcdefghijklmnopqrstuvwxyzABCDEFGHIJKLMNOPQRSTUVWXYZ0123456789 # !@#$%^&*()_+{}:"~<>?|\-=[];'`,./ # END of CIF _database_code_depnum_ccdc_archive 'CCDC 929493'