data_publication_text _publ_contact_author_name 'Kenneth D. Karlin' _publ_contact_author_address ;Department of Chemistry Johns Hopkins University Baltimore, MD 21218 USA ; _publ_contact_author_email karlin@jhu.edu _publ_contact_author_phone '(410) 516-8027' loop_ _publ_author_name _publ_author_address 'Hematian, S.' ;Department of Chemistry Johns Hopkins University Baltimore, MD 21218 USA ; 'Siegler, M. A.' ;Department of Chemistry Johns Hopkins University Baltimore, MD 21218 USA ; 'Karlin, K. D.' ;Department of Chemistry Johns Hopkins University Baltimore, MD 21218 USA ; data_[(tmpa)CuII(NO2)][B(C6F5)4] _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C24 B F20, C18 H18 Cu N5 O2' _chemical_formula_sum 'C42 H18 B Cu F20 N5 O2' _chemical_formula_weight 1078.96 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'B' 'B' 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' _cell_length_a 13.3059(2) _cell_length_b 22.9396(5) _cell_length_c 26.0492(7) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 7951.1(3) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _cell_measurement_reflns_used 9233 _cell_measurement_theta_min 1.72 _cell_measurement_theta_max 26.31 _exptl_crystal_description block _exptl_crystal_colour green _exptl_crystal_size_max 0.67 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.803 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4280 _exptl_absorpt_coefficient_mu 0.692 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.711 _exptl_absorpt_correction_T_max 0.894 _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) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 110(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator 'graphite' _diffrn_measurement_device_type 'Goniometer KM4/Xcalibur, detector: Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 15.989 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25595 _diffrn_reflns_av_R_equivalents 0.0356 _diffrn_reflns_av_sigmaI/netI 0.0370 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -28 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 26.25 _reflns_number_total 8030 _reflns_number_gt 6640 _reflns_threshold_expression 'I>2\s(I)' _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 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL v6.10 (Sheldrick, 2008)' _computing_publication_material 'SHELXTL v6.10 (Sheldrick, 2008)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0373P)^2^+5.2153P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8030 _refine_ls_number_parameters 659 _refine_ls_number_restraints 63 _refine_ls_R_factor_all 0.0428 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0833 _refine_ls_wR_factor_gt 0.0784 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.031 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.303974(16) 0.088465(10) 0.225262(9) 0.01608(7) Uani 1 1 d . . . C1 C 0.35486(15) -0.00859(8) 0.30200(8) 0.0216(4) Uani 1 1 d . . . H1 H 0.2948 0.0019 0.3194 0.026 Uiso 1 1 calc R A . C2 C 0.41336(16) -0.05250(9) 0.32204(9) 0.0268(5) Uani 1 1 d . A . H2 H 0.3942 -0.0719 0.3527 0.032 Uiso 1 1 calc R . . C3 C 0.50073(16) -0.06771(9) 0.29646(9) 0.0293(5) Uani 1 1 d . . . H3 H 0.5430 -0.0975 0.3098 0.035 Uiso 1 1 calc R A . C4 C 0.52615(15) -0.03935(9) 0.25139(8) 0.0239(4) Uani 1 1 d . A . H4 H 0.5849 -0.0500 0.2329 0.029 Uiso 1 1 calc R . . C5 C 0.46411(14) 0.00484(8) 0.23389(7) 0.0170(4) Uani 1 1 d . . . C6 C 0.48916(13) 0.04129(8) 0.18751(7) 0.0170(4) Uani 1 1 d . A . H6A H 0.5366 0.0726 0.1974 0.020 Uiso 1 1 calc R . . H6B H 0.5222 0.0166 0.1613 0.020 Uiso 1 1 calc R . . C7 C 0.34183(14) 0.02461(9) 0.13357(8) 0.0203(4) Uani 1 1 d . . . H7A H 0.3484 -0.0147 0.1488 0.024 Uiso 1 1 calc R A . H7B H 0.3715 0.0236 0.0987 0.024 Uiso 1 1 calc R . . C8 C 0.23204(14) 0.04092(8) 0.13008(8) 0.0193(4) Uani 1 1 d . A . C9 C 0.17104(15) 0.02373(9) 0.08982(8) 0.0234(4) Uani 1 1 d . . . H9 H 0.1972 0.0010 0.0624 0.028 Uiso 1 1 calc R A . C10 C 0.07104(15) 0.04036(9) 0.09029(9) 0.0282(5) Uani 1 1 d . A . H10 H 0.0278 0.0291 0.0630 0.034 Uiso 1 1 calc R . . C11 C 0.03437(15) 0.07326(9) 0.13040(9) 0.0267(5) Uani 1 1 d . . . H11 H -0.0337 0.0857 0.1308 0.032 Uiso 1 1 calc R A . C12 C 0.09903(14) 0.08779(8) 0.17010(8) 0.0221(4) Uani 1 1 d . A . H12 H 0.0737 0.1095 0.1983 0.027 Uiso 1 1 calc R . . C13 C 0.41910(14) 0.12169(8) 0.13712(7) 0.0193(4) Uani 1 1 d . . . H13A H 0.3631 0.1307 0.1134 0.023 Uiso 1 1 calc R A . H13B H 0.4809 0.1163 0.1165 0.023 Uiso 1 1 calc R . . C14 C 0.43331(14) 0.17148(8) 0.17403(8) 0.0190(4) Uani 1 1 d . A . C15 C 0.49125(15) 0.21973(9) 0.16156(9) 0.0250(4) Uani 1 1 d . . . H15 H 0.5260 0.2216 0.1297 0.030 Uiso 1 1 calc R A . C16 C 0.49740(15) 0.26490(9) 0.19624(9) 0.0295(5) Uani 1 1 d . A . H16 H 0.5357 0.2987 0.1884 0.035 Uiso 1 1 calc R . . C17 C 0.44733(15) 0.26072(9) 0.24264(9) 0.0274(5) Uani 1 1 d . . . H17 H 0.4506 0.2915 0.2670 0.033 Uiso 1 1 calc R A . C18 C 0.39240(14) 0.21082(9) 0.25282(9) 0.0233(4) Uani 1 1 d . A . H18 H 0.3590 0.2076 0.2849 0.028 Uiso 1 1 calc R . . N1 N 0.37929(11) 0.02001(7) 0.25886(6) 0.0168(3) Uani 1 1 d . A . N2 N 0.39660(11) 0.06753(7) 0.16565(6) 0.0157(3) Uani 1 1 d . A . N3 N 0.19655(11) 0.07206(7) 0.16998(6) 0.0184(3) Uani 1 1 d . A . N4 N 0.38452(11) 0.16692(7) 0.21911(6) 0.0181(3) Uani 1 1 d . A . N5 N 0.2184(2) 0.1146(3) 0.32353(13) 0.0264(8) Uani 0.875(5) 1 d PDU A 1 O1 O 0.20060(10) 0.10011(6) 0.27627(6) 0.0234(3) Uani 0.875(5) 1 d PDU A 1 O2 O 0.30735(14) 0.12294(8) 0.33341(7) 0.0291(6) Uani 0.875(5) 1 d PDU A 1 N5' N 0.2419(19) 0.116(2) 0.3191(8) 0.024(3) Uani 0.125(5) 1 d PDU A 2 O1' O 0.20060(10) 0.10011(6) 0.27627(6) 0.0234(3) Uani 0.125(5) 1 d PDU A 2 O2' O 0.1760(10) 0.1243(5) 0.3514(5) 0.027(4) Uani 0.125(5) 1 d PDU A 2 B1 B 0.09959(15) 0.30296(9) 0.05891(8) 0.0141(4) Uani 1 1 d . . . C19 C 0.12051(13) 0.24152(8) 0.02794(7) 0.0142(4) Uani 1 1 d . . . C20 C 0.19455(13) 0.20072(8) 0.03830(7) 0.0154(4) Uani 1 1 d . . . C21 C 0.20440(14) 0.14845(8) 0.01227(8) 0.0183(4) Uani 1 1 d . . . C22 C 0.13837(14) 0.13516(8) -0.02659(7) 0.0181(4) Uani 1 1 d . . . C23 C 0.06632(14) 0.17525(8) -0.04059(7) 0.0177(4) Uani 1 1 d . . . C24 C 0.06085(13) 0.22726(8) -0.01416(7) 0.0156(4) Uani 1 1 d . . . C25 C 0.13998(14) 0.35367(8) 0.01906(7) 0.0156(4) Uani 1 1 d . . . C26 C 0.24282(14) 0.35786(8) 0.00950(8) 0.0181(4) Uani 1 1 d . . . C27 C 0.28640(15) 0.39848(8) -0.02245(8) 0.0217(4) Uani 1 1 d . . . C28 C 0.22664(16) 0.43734(8) -0.04828(8) 0.0226(4) Uani 1 1 d . . . C29 C 0.12412(16) 0.43483(9) -0.04119(8) 0.0229(4) Uani 1 1 d . . . C30 C 0.08353(14) 0.39351(8) -0.00853(8) 0.0184(4) Uani 1 1 d . . . C32 C -0.05227(13) 0.36212(8) 0.09829(7) 0.0166(4) Uani 1 1 d . . . C33 C -0.14681(14) 0.37148(8) 0.11837(7) 0.0180(4) Uani 1 1 d . . . C34 C -0.21552(13) 0.32679(9) 0.11742(7) 0.0177(4) Uani 1 1 d . . . C35 C -0.18812(13) 0.27385(8) 0.09772(7) 0.0181(4) Uani 1 1 d . . . C36 C -0.09170(14) 0.26608(8) 0.07857(7) 0.0162(4) Uani 1 1 d . . . C37 C 0.15488(13) 0.30626(8) 0.11575(7) 0.0160(4) Uani 1 1 d . . . C38 C 0.20291(13) 0.35475(9) 0.13635(8) 0.0197(4) Uani 1 1 d . . . C39 C 0.23105(15) 0.35897(10) 0.18739(9) 0.0273(5) Uani 1 1 d . . . C40 C 0.21682(16) 0.31301(11) 0.21990(8) 0.0315(5) Uani 1 1 d . . . C41 C 0.17316(16) 0.26309(10) 0.20141(8) 0.0267(5) Uani 1 1 d . . . C42 C 0.14074(14) 0.26179(9) 0.15110(8) 0.0203(4) Uani 1 1 d . . . C503 C -0.01963(13) 0.30998(8) 0.07661(7) 0.0141(4) Uani 1 1 d . . . F1 F 0.26194(8) 0.20918(5) 0.07659(4) 0.0204(2) Uani 1 1 d . . . F2 F 0.27853(8) 0.11088(5) 0.02433(5) 0.0238(3) Uani 1 1 d . . . F3 F 0.14592(9) 0.08385(5) -0.05142(5) 0.0272(3) Uani 1 1 d . . . F4 F 0.00399(8) 0.16340(5) -0.07989(4) 0.0248(3) Uani 1 1 d . . . F5 F -0.01065(8) 0.26527(5) -0.02984(4) 0.0200(2) Uani 1 1 d . . . F6 F 0.30595(8) 0.32096(5) 0.03377(5) 0.0235(3) Uani 1 1 d . . . F7 F 0.38720(9) 0.40149(5) -0.02784(5) 0.0309(3) Uani 1 1 d . . . F8 F 0.26714(10) 0.47691(5) -0.08014(5) 0.0330(3) Uani 1 1 d . . . F9 F 0.06402(10) 0.47266(5) -0.06630(5) 0.0322(3) Uani 1 1 d . . . F10 F -0.01809(8) 0.39425(5) -0.00504(5) 0.0240(3) Uani 1 1 d . . . F11 F 0.01218(8) 0.40797(5) 0.10136(5) 0.0212(2) Uani 1 1 d . . . F12 F -0.17183(9) 0.42341(5) 0.13907(5) 0.0258(3) Uani 1 1 d . . . F13 F -0.30940(8) 0.33472(5) 0.13561(4) 0.0232(3) Uani 1 1 d . . . F14 F -0.25501(8) 0.22984(5) 0.09674(5) 0.0259(3) Uani 1 1 d . . . F15 F -0.07171(8) 0.21172(5) 0.06210(4) 0.0215(2) Uani 1 1 d . . . F16 F 0.22307(8) 0.40227(5) 0.10749(5) 0.0242(3) Uani 1 1 d . . . F17 F 0.27193(10) 0.40917(6) 0.20513(6) 0.0395(3) Uani 1 1 d . . . F18 F 0.24519(11) 0.31679(8) 0.26941(5) 0.0468(4) Uani 1 1 d . . . F19 F 0.16005(10) 0.21671(6) 0.23227(5) 0.0370(3) Uani 1 1 d . . . F20 F 0.09094(9) 0.21305(5) 0.13682(4) 0.0247(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 Cu1 0.01212(11) 0.01766(12) 0.01846(13) 0.00154(9) 0.00156(9) 0.00036(9) C1 0.0218(10) 0.0183(10) 0.0245(11) 0.0030(8) 0.0045(8) -0.0034(8) C2 0.0317(11) 0.0199(10) 0.0289(12) 0.0108(9) 0.0027(9) -0.0029(9) C3 0.0287(11) 0.0217(10) 0.0373(13) 0.0107(9) -0.0007(10) 0.0034(9) C4 0.0205(9) 0.0213(10) 0.0297(12) 0.0035(9) 0.0032(9) 0.0042(8) C5 0.0151(9) 0.0162(9) 0.0195(10) -0.0002(7) -0.0009(7) -0.0029(7) C6 0.0109(8) 0.0208(10) 0.0192(10) 0.0017(8) 0.0001(7) 0.0012(7) C7 0.0177(9) 0.0204(10) 0.0229(10) -0.0046(8) -0.0024(8) -0.0007(8) C8 0.0181(9) 0.0163(9) 0.0236(10) 0.0034(8) -0.0014(8) -0.0020(7) C9 0.0234(10) 0.0226(10) 0.0241(11) 0.0018(8) -0.0065(8) -0.0027(8) C10 0.0234(10) 0.0272(11) 0.0339(13) 0.0057(9) -0.0111(9) -0.0045(9) C11 0.0163(9) 0.0256(11) 0.0381(13) 0.0103(10) -0.0060(9) -0.0015(8) C12 0.0159(9) 0.0193(10) 0.0311(12) 0.0062(8) -0.0006(8) 0.0005(7) C13 0.0196(9) 0.0213(10) 0.0169(10) 0.0046(8) -0.0002(8) 0.0005(8) C14 0.0152(8) 0.0193(10) 0.0224(10) 0.0052(8) -0.0016(8) 0.0010(7) C15 0.0240(10) 0.0218(10) 0.0292(12) 0.0079(9) 0.0020(9) -0.0025(8) C16 0.0237(10) 0.0206(11) 0.0441(14) 0.0053(10) 0.0002(10) -0.0058(8) C17 0.0221(10) 0.0215(11) 0.0385(13) -0.0068(9) -0.0016(9) -0.0027(8) C18 0.0180(9) 0.0246(10) 0.0272(11) -0.0045(9) 0.0022(8) 0.0002(8) N1 0.0168(7) 0.0149(8) 0.0187(8) 0.0019(6) 0.0008(6) -0.0020(6) N2 0.0128(7) 0.0162(8) 0.0181(8) 0.0020(6) -0.0013(6) -0.0004(6) N3 0.0153(7) 0.0170(8) 0.0229(9) 0.0041(7) -0.0015(7) -0.0007(6) N4 0.0138(7) 0.0188(8) 0.0216(9) 0.0005(7) 0.0008(7) -0.0001(6) N5 0.0193(18) 0.0263(12) 0.0337(16) -0.0006(13) -0.0001(14) 0.0015(17) O1 0.0172(7) 0.0292(8) 0.0239(8) 0.0022(6) 0.0040(6) 0.0011(6) O2 0.0258(11) 0.0316(10) 0.0298(11) -0.0012(8) -0.0028(8) 0.0011(7) N5' 0.018(5) 0.023(5) 0.030(5) 0.004(5) 0.008(5) 0.002(6) O1' 0.0172(7) 0.0292(8) 0.0239(8) 0.0022(6) 0.0040(6) 0.0011(6) O2' 0.031(6) 0.022(6) 0.029(7) -0.009(5) 0.016(6) 0.005(5) B1 0.0145(9) 0.0101(9) 0.0175(11) 0.0002(8) -0.0012(8) 0.0010(7) C19 0.0139(8) 0.0124(9) 0.0162(9) 0.0015(7) 0.0034(7) -0.0012(7) C20 0.0158(9) 0.0163(9) 0.0141(9) 0.0016(7) 0.0010(7) -0.0011(7) C21 0.0182(9) 0.0158(9) 0.0209(10) 0.0043(8) 0.0056(8) 0.0046(7) C22 0.0245(10) 0.0133(9) 0.0165(10) -0.0032(7) 0.0062(8) -0.0014(7) C23 0.0171(9) 0.0208(10) 0.0151(9) -0.0026(8) 0.0009(7) -0.0027(7) C24 0.0123(8) 0.0159(9) 0.0185(10) 0.0004(7) 0.0014(7) 0.0019(7) C25 0.0191(9) 0.0120(9) 0.0155(9) -0.0022(7) -0.0009(7) -0.0013(7) C26 0.0195(9) 0.0123(9) 0.0225(10) -0.0017(7) 0.0009(8) 0.0003(7) C27 0.0228(10) 0.0173(10) 0.0250(11) -0.0054(8) 0.0072(8) -0.0047(7) C28 0.0369(11) 0.0154(10) 0.0156(10) 0.0001(8) 0.0034(9) -0.0092(8) C29 0.0343(11) 0.0154(9) 0.0191(10) 0.0029(8) -0.0076(9) -0.0015(8) C30 0.0183(9) 0.0173(9) 0.0196(10) -0.0008(8) -0.0032(8) -0.0010(7) C32 0.0163(9) 0.0152(9) 0.0183(10) 0.0017(7) -0.0025(7) -0.0014(7) C33 0.0203(9) 0.0178(9) 0.0158(10) -0.0030(8) -0.0016(8) 0.0061(7) C34 0.0127(8) 0.0275(10) 0.0128(9) 0.0025(8) 0.0010(7) 0.0035(7) C35 0.0169(9) 0.0198(9) 0.0176(10) 0.0034(8) 0.0004(8) -0.0046(7) C36 0.0189(9) 0.0130(9) 0.0167(9) 0.0000(7) -0.0006(8) 0.0025(7) C37 0.0129(8) 0.0172(9) 0.0181(10) -0.0030(7) -0.0002(7) 0.0038(7) C38 0.0144(9) 0.0219(10) 0.0228(10) -0.0048(8) -0.0008(8) 0.0048(7) C39 0.0189(9) 0.0343(12) 0.0287(12) -0.0161(10) -0.0053(9) 0.0049(9) C40 0.0268(11) 0.0509(15) 0.0167(11) -0.0088(10) -0.0051(9) 0.0174(10) C41 0.0265(10) 0.0349(12) 0.0187(11) 0.0043(9) 0.0025(9) 0.0156(9) C42 0.0189(9) 0.0219(10) 0.0202(10) -0.0017(8) 0.0011(8) 0.0057(7) C503 0.0156(8) 0.0135(9) 0.0133(9) 0.0016(7) -0.0016(7) 0.0020(7) F1 0.0183(5) 0.0204(6) 0.0225(6) -0.0009(5) -0.0051(5) 0.0046(4) F2 0.0252(6) 0.0188(6) 0.0273(7) 0.0008(5) 0.0025(5) 0.0107(5) F3 0.0377(7) 0.0160(6) 0.0280(7) -0.0088(5) 0.0033(6) 0.0022(5) F4 0.0238(6) 0.0289(6) 0.0217(6) -0.0094(5) -0.0042(5) -0.0016(5) F5 0.0181(5) 0.0210(6) 0.0210(6) -0.0010(5) -0.0042(4) 0.0040(4) F6 0.0154(5) 0.0212(6) 0.0339(7) 0.0047(5) 0.0027(5) 0.0027(4) F7 0.0223(6) 0.0255(6) 0.0449(8) -0.0004(6) 0.0153(6) -0.0057(5) F8 0.0497(8) 0.0215(6) 0.0276(7) 0.0060(5) 0.0075(6) -0.0147(6) F9 0.0421(7) 0.0229(6) 0.0317(7) 0.0127(5) -0.0136(6) -0.0034(5) F10 0.0168(5) 0.0235(6) 0.0317(7) 0.0074(5) -0.0068(5) 0.0000(5) F11 0.0181(5) 0.0139(5) 0.0316(7) -0.0060(5) -0.0011(5) -0.0009(4) F12 0.0246(6) 0.0226(6) 0.0304(7) -0.0101(5) 0.0012(5) 0.0081(5) F13 0.0141(5) 0.0346(7) 0.0210(6) 0.0005(5) 0.0042(4) 0.0045(5) F14 0.0186(5) 0.0246(6) 0.0345(7) 0.0014(5) 0.0050(5) -0.0083(5) F15 0.0208(5) 0.0132(5) 0.0305(7) -0.0035(5) 0.0045(5) -0.0029(4) F16 0.0238(6) 0.0188(6) 0.0300(7) -0.0061(5) -0.0004(5) -0.0052(5) F17 0.0311(7) 0.0468(8) 0.0405(8) -0.0265(7) -0.0104(6) 0.0001(6) F18 0.0481(9) 0.0767(11) 0.0155(6) -0.0149(7) -0.0109(6) 0.0256(8) F19 0.0457(8) 0.0468(8) 0.0184(6) 0.0128(6) 0.0055(6) 0.0215(7) F20 0.0307(6) 0.0181(6) 0.0251(6) 0.0061(5) 0.0029(5) -0.0003(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.9309(14) . ? Cu1 N2 2.0399(16) . ? Cu1 N1 2.0582(16) . ? Cu1 N3 2.0635(16) . ? Cu1 N4 2.1007(16) . ? C1 N1 1.341(3) . ? C1 C2 1.376(3) . ? C1 H1 0.9500 . ? C2 C3 1.385(3) . ? C2 H2 0.9500 . ? C3 C4 1.384(3) . ? C3 H3 0.9500 . ? C4 C5 1.384(3) . ? C4 H4 0.9500 . ? C5 N1 1.348(2) . ? C5 C6 1.507(3) . ? C6 N2 1.484(2) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N2 1.483(2) . ? C7 C8 1.511(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N3 1.347(3) . ? C8 C9 1.384(3) . ? C9 C10 1.384(3) . ? C9 H9 0.9500 . ? C10 C11 1.378(3) . ? C10 H10 0.9500 . ? C11 C12 1.386(3) . ? C11 H11 0.9500 . ? C12 N3 1.347(2) . ? C12 H12 0.9500 . ? C13 N2 1.479(2) . ? C13 C14 1.505(3) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C14 N4 1.346(2) . ? C14 C15 1.387(3) . ? C15 C16 1.377(3) . ? C15 H15 0.9500 . ? C16 C17 1.384(3) . ? C16 H16 0.9500 . ? C17 C18 1.384(3) . ? C17 H17 0.9500 . ? C18 N4 1.340(3) . ? C18 H18 0.9500 . ? N5 O2 1.226(3) . ? N5 O1 1.297(3) . ? N5' O2' 1.229(18) . ? B1 C19 1.648(3) . ? B1 C25 1.649(3) . ? B1 C37 1.655(3) . ? B1 C503 1.660(3) . ? C19 C20 1.385(2) . ? C19 C24 1.393(3) . ? C20 F1 1.355(2) . ? C20 C21 1.384(3) . ? C21 F2 1.347(2) . ? C21 C22 1.375(3) . ? C22 F3 1.347(2) . ? C22 C23 1.378(3) . ? C23 F4 1.345(2) . ? C23 C24 1.379(3) . ? C24 F5 1.354(2) . ? C25 C30 1.384(3) . ? C25 C26 1.394(3) . ? C26 F6 1.350(2) . ? C26 C27 1.377(3) . ? C27 F7 1.350(2) . ? C27 C28 1.371(3) . ? C28 F8 1.343(2) . ? C28 C29 1.378(3) . ? C29 F9 1.349(2) . ? C29 C30 1.383(3) . ? C30 F10 1.355(2) . ? C32 F11 1.359(2) . ? C32 C33 1.379(3) . ? C32 C503 1.392(3) . ? C33 F12 1.349(2) . ? C33 C34 1.374(3) . ? C34 F13 1.348(2) . ? C34 C35 1.368(3) . ? C35 F14 1.346(2) . ? C35 C36 1.388(3) . ? C36 F15 1.345(2) . ? C36 C503 1.392(3) . ? C37 C42 1.387(3) . ? C37 C38 1.391(3) . ? C38 F16 1.351(2) . ? C38 C39 1.385(3) . ? C39 F17 1.355(2) . ? C39 C40 1.366(3) . ? C40 F18 1.346(2) . ? C40 C41 1.371(3) . ? C41 F19 1.345(3) . ? C41 C42 1.380(3) . ? C42 F20 1.352(2) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N2 170.67(6) . . ? O1 Cu1 N1 99.20(6) . . ? N2 Cu1 N1 81.37(6) . . ? O1 Cu1 N3 90.69(6) . . ? N2 Cu1 N3 81.05(6) . . ? N1 Cu1 N3 119.66(6) . . ? O1 Cu1 N4 107.30(6) . . ? N2 Cu1 N4 80.52(6) . . ? N1 Cu1 N4 115.96(6) . . ? N3 Cu1 N4 117.15(6) . . ? N1 C1 C2 122.60(18) . . ? N1 C1 H1 118.7 . . ? C2 C1 H1 118.7 . . ? C1 C2 C3 118.49(19) . . ? C1 C2 H2 120.8 . . ? C3 C2 H2 120.8 . . ? C4 C3 C2 119.66(19) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 118.54(19) . . ? C3 C4 H4 120.7 . . ? C5 C4 H4 120.7 . . ? N1 C5 C4 121.95(18) . . ? N1 C5 C6 115.40(16) . . ? C4 C5 C6 122.58(17) . . ? N2 C6 C5 110.43(14) . . ? N2 C6 H6A 109.6 . . ? C5 C6 H6A 109.6 . . ? N2 C6 H6B 109.6 . . ? C5 C6 H6B 109.6 . . ? H6A C6 H6B 108.1 . . ? N2 C7 C8 110.16(15) . . ? N2 C7 H7A 109.6 . . ? C8 C7 H7A 109.6 . . ? N2 C7 H7B 109.6 . . ? C8 C7 H7B 109.6 . . ? H7A C7 H7B 108.1 . . ? N3 C8 C9 122.05(18) . . ? N3 C8 C7 115.09(17) . . ? C9 C8 C7 122.83(18) . . ? C8 C9 C10 118.6(2) . . ? C8 C9 H9 120.7 . . ? C10 C9 H9 120.7 . . ? C11 C10 C9 119.9(2) . . ? C11 C10 H10 120.1 . . ? C9 C10 H10 120.1 . . ? C10 C11 C12 118.52(19) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? N3 C12 C11 122.2(2) . . ? N3 C12 H12 118.9 . . ? C11 C12 H12 118.9 . . ? N2 C13 C14 110.01(15) . . ? N2 C13 H13A 109.7 . . ? C14 C13 H13A 109.7 . . ? N2 C13 H13B 109.7 . . ? C14 C13 H13B 109.7 . . ? H13A C13 H13B 108.2 . . ? N4 C14 C15 122.30(19) . . ? N4 C14 C13 115.97(16) . . ? C15 C14 C13 121.71(18) . . ? C16 C15 C14 118.7(2) . . ? C16 C15 H15 120.7 . . ? C14 C15 H15 120.7 . . ? C15 C16 C17 119.50(19) . . ? C15 C16 H16 120.3 . . ? C17 C16 H16 120.3 . . ? C16 C17 C18 118.6(2) . . ? C16 C17 H17 120.7 . . ? C18 C17 H17 120.7 . . ? N4 C18 C17 122.5(2) . . ? N4 C18 H18 118.7 . . ? C17 C18 H18 118.7 . . ? C1 N1 C5 118.75(17) . . ? C1 N1 Cu1 127.69(13) . . ? C5 N1 Cu1 113.53(12) . . ? C13 N2 C7 111.99(15) . . ? C13 N2 C6 111.44(14) . . ? C7 N2 C6 110.78(14) . . ? C13 N2 Cu1 107.89(11) . . ? C7 N2 Cu1 106.76(11) . . ? C6 N2 Cu1 107.74(11) . . ? C8 N3 C12 118.79(17) . . ? C8 N3 Cu1 113.11(12) . . ? C12 N3 Cu1 128.10(14) . . ? C18 N4 C14 118.39(17) . . ? C18 N4 Cu1 129.32(14) . . ? C14 N4 Cu1 112.29(12) . . ? O2 N5 O1 114.5(3) . . ? N5 O1 Cu1 123.96(16) . . ? C19 B1 C25 103.89(15) . . ? C19 B1 C37 113.70(14) . . ? C25 B1 C37 112.71(15) . . ? C19 B1 C503 112.36(14) . . ? C25 B1 C503 114.70(15) . . ? C37 B1 C503 99.90(14) . . ? C20 C19 C24 113.59(16) . . ? C20 C19 B1 127.05(16) . . ? C24 C19 B1 119.35(15) . . ? F1 C20 C21 114.97(16) . . ? F1 C20 C19 121.14(16) . . ? C21 C20 C19 123.87(17) . . ? F2 C21 C22 119.86(17) . . ? F2 C21 C20 120.63(17) . . ? C22 C21 C20 119.50(17) . . ? F3 C22 C21 119.98(17) . . ? F3 C22 C23 120.55(17) . . ? C21 C22 C23 119.45(17) . . ? F4 C23 C22 119.70(17) . . ? F4 C23 C24 121.47(17) . . ? C22 C23 C24 118.82(17) . . ? F5 C24 C23 116.33(16) . . ? F5 C24 C19 119.15(16) . . ? C23 C24 C19 124.47(17) . . ? C30 C25 C26 113.22(17) . . ? C30 C25 B1 128.00(16) . . ? C26 C25 B1 118.75(16) . . ? F6 C26 C27 116.44(16) . . ? F6 C26 C25 118.94(16) . . ? C27 C26 C25 124.60(18) . . ? F7 C27 C28 119.46(18) . . ? F7 C27 C26 121.03(18) . . ? C28 C27 C26 119.49(18) . . ? F8 C28 C27 120.68(19) . . ? F8 C28 C29 120.56(19) . . ? C27 C28 C29 118.76(18) . . ? F9 C29 C28 119.66(18) . . ? F9 C29 C30 120.50(18) . . ? C28 C29 C30 119.84(18) . . ? F10 C30 C29 114.97(17) . . ? F10 C30 C25 120.98(17) . . ? C29 C30 C25 124.04(18) . . ? F11 C32 C33 115.64(16) . . ? F11 C32 C503 119.46(16) . . ? C33 C32 C503 124.89(17) . . ? F12 C33 C34 120.12(16) . . ? F12 C33 C32 120.93(17) . . ? C34 C33 C32 118.95(17) . . ? F13 C34 C35 119.91(17) . . ? F13 C34 C33 120.63(17) . . ? C35 C34 C33 119.47(17) . . ? F14 C35 C34 119.79(16) . . ? F14 C35 C36 120.52(17) . . ? C34 C35 C36 119.69(17) . . ? F15 C36 C35 114.62(16) . . ? F15 C36 C503 121.52(16) . . ? C35 C36 C503 123.86(17) . . ? C42 C37 C38 113.22(18) . . ? C42 C37 B1 120.00(16) . . ? C38 C37 B1 125.88(17) . . ? F16 C38 C39 115.10(18) . . ? F16 C38 C37 121.45(17) . . ? C39 C38 C37 123.4(2) . . ? F17 C39 C40 120.0(2) . . ? F17 C39 C38 119.7(2) . . ? C40 C39 C38 120.3(2) . . ? F18 C40 C39 120.4(2) . . ? F18 C40 C41 120.6(2) . . ? C39 C40 C41 119.05(19) . . ? F19 C41 C40 120.37(19) . . ? F19 C41 C42 120.7(2) . . ? C40 C41 C42 119.0(2) . . ? F20 C42 C41 115.62(18) . . ? F20 C42 C37 119.47(17) . . ? C41 C42 C37 124.90(19) . . ? C36 C503 C32 113.07(16) . . ? C36 C503 B1 126.78(16) . . ? C32 C503 B1 119.61(16) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 -0.1(3) . . . . ? C1 C2 C3 C4 -1.0(3) . . . . ? C2 C3 C4 C5 1.7(3) . . . . ? C3 C4 C5 N1 -1.3(3) . . . . ? C3 C4 C5 C6 175.33(19) . . . . ? N1 C5 C6 N2 -25.5(2) . . . . ? C4 C5 C6 N2 157.57(18) . . . . ? N2 C7 C8 N3 -26.5(2) . . . . ? N2 C7 C8 C9 155.53(18) . . . . ? N3 C8 C9 C10 1.5(3) . . . . ? C7 C8 C9 C10 179.35(19) . . . . ? C8 C9 C10 C11 -0.1(3) . . . . ? C9 C10 C11 C12 -1.4(3) . . . . ? C10 C11 C12 N3 1.7(3) . . . . ? N2 C13 C14 N4 -27.2(2) . . . . ? N2 C13 C14 C15 154.39(17) . . . . ? N4 C14 C15 C16 -1.2(3) . . . . ? C13 C14 C15 C16 177.12(18) . . . . ? C14 C15 C16 C17 1.0(3) . . . . ? C15 C16 C17 C18 0.1(3) . . . . ? C16 C17 C18 N4 -1.2(3) . . . . ? C2 C1 N1 C5 0.5(3) . . . . ? C2 C1 N1 Cu1 -177.39(15) . . . . ? C4 C5 N1 C1 0.2(3) . . . . ? C6 C5 N1 C1 -176.68(17) . . . . ? C4 C5 N1 Cu1 178.44(15) . . . . ? C6 C5 N1 Cu1 1.5(2) . . . . ? O1 Cu1 N1 C1 4.01(17) . . . . ? N2 Cu1 N1 C1 -166.56(17) . . . . ? N3 Cu1 N1 C1 -92.08(17) . . . . ? N4 Cu1 N1 C1 118.46(16) . . . . ? O1 Cu1 N1 C5 -174.01(13) . . . . ? N2 Cu1 N1 C5 15.42(13) . . . . ? N3 Cu1 N1 C5 89.89(13) . . . . ? N4 Cu1 N1 C5 -59.57(14) . . . . ? C14 C13 N2 C7 156.26(15) . . . . ? C14 C13 N2 C6 -79.02(19) . . . . ? C14 C13 N2 Cu1 39.07(17) . . . . ? C8 C7 N2 C13 -78.62(19) . . . . ? C8 C7 N2 C6 156.29(16) . . . . ? C8 C7 N2 Cu1 39.24(18) . . . . ? C5 C6 N2 C13 154.41(16) . . . . ? C5 C6 N2 C7 -80.19(19) . . . . ? C5 C6 N2 Cu1 36.24(17) . . . . ? N1 Cu1 N2 C13 -148.52(12) . . . . ? N3 Cu1 N2 C13 89.43(12) . . . . ? N4 Cu1 N2 C13 -30.22(11) . . . . ? N1 Cu1 N2 C7 90.94(12) . . . . ? N3 Cu1 N2 C7 -31.11(12) . . . . ? N4 Cu1 N2 C7 -150.75(12) . . . . ? N1 Cu1 N2 C6 -28.09(11) . . . . ? N3 Cu1 N2 C6 -150.14(12) . . . . ? N4 Cu1 N2 C6 90.21(12) . . . . ? C9 C8 N3 C12 -1.2(3) . . . . ? C7 C8 N3 C12 -179.25(17) . . . . ? C9 C8 N3 Cu1 177.81(15) . . . . ? C7 C8 N3 Cu1 -0.2(2) . . . . ? C11 C12 N3 C8 -0.4(3) . . . . ? C11 C12 N3 Cu1 -179.29(14) . . . . ? O1 Cu1 N3 C8 -157.47(13) . . . . ? N2 Cu1 N3 C8 18.18(13) . . . . ? N1 Cu1 N3 C8 -56.47(15) . . . . ? N4 Cu1 N3 C8 92.63(14) . . . . ? O1 Cu1 N3 C12 21.48(16) . . . . ? N2 Cu1 N3 C12 -162.87(17) . . . . ? N1 Cu1 N3 C12 122.47(16) . . . . ? N4 Cu1 N3 C12 -88.42(17) . . . . ? C17 C18 N4 C14 1.0(3) . . . . ? C17 C18 N4 Cu1 -178.66(15) . . . . ? C15 C14 N4 C18 0.2(3) . . . . ? C13 C14 N4 C18 -178.20(17) . . . . ? C15 C14 N4 Cu1 179.92(15) . . . . ? C13 C14 N4 Cu1 1.5(2) . . . . ? O1 Cu1 N4 C18 21.45(18) . . . . ? N2 Cu1 N4 C18 -163.79(18) . . . . ? N1 Cu1 N4 C18 -88.30(17) . . . . ? N3 Cu1 N4 C18 121.46(17) . . . . ? O1 Cu1 N4 C14 -158.23(12) . . . . ? N2 Cu1 N4 C14 16.54(12) . . . . ? N1 Cu1 N4 C14 92.03(13) . . . . ? N3 Cu1 N4 C14 -58.22(14) . . . . ? O2 N5 O1 Cu1 2.9(6) . . . . ? N1 Cu1 O1 N5 61.9(3) . . . . ? N3 Cu1 O1 N5 -177.9(3) . . . . ? N4 Cu1 O1 N5 -59.1(3) . . . . ? C25 B1 C19 C20 106.7(2) . . . . ? C37 B1 C19 C20 -16.2(3) . . . . ? C503 B1 C19 C20 -128.73(18) . . . . ? C25 B1 C19 C24 -71.97(19) . . . . ? C37 B1 C19 C24 165.15(16) . . . . ? C503 B1 C19 C24 52.6(2) . . . . ? C24 C19 C20 F1 177.06(16) . . . . ? B1 C19 C20 F1 -1.7(3) . . . . ? C24 C19 C20 C21 -4.8(3) . . . . ? B1 C19 C20 C21 176.46(18) . . . . ? F1 C20 C21 F2 -2.0(2) . . . . ? C19 C20 C21 F2 179.80(16) . . . . ? F1 C20 C21 C22 178.70(16) . . . . ? C19 C20 C21 C22 0.5(3) . . . . ? F2 C21 C22 F3 2.1(3) . . . . ? C20 C21 C22 F3 -178.54(16) . . . . ? F2 C21 C22 C23 -176.37(17) . . . . ? C20 C21 C22 C23 3.0(3) . . . . ? F3 C22 C23 F4 -1.0(3) . . . . ? C21 C22 C23 F4 177.46(16) . . . . ? F3 C22 C23 C24 179.87(16) . . . . ? C21 C22 C23 C24 -1.7(3) . . . . ? F4 C23 C24 F5 0.3(3) . . . . ? C22 C23 C24 F5 179.36(16) . . . . ? F4 C23 C24 C19 177.65(17) . . . . ? C22 C23 C24 C19 -3.3(3) . . . . ? C20 C19 C24 F5 -176.44(15) . . . . ? B1 C19 C24 F5 2.4(2) . . . . ? C20 C19 C24 C23 6.2(3) . . . . ? B1 C19 C24 C23 -174.90(17) . . . . ? C19 B1 C25 C30 109.4(2) . . . . ? C37 B1 C25 C30 -127.05(19) . . . . ? C503 B1 C25 C30 -13.6(3) . . . . ? C19 B1 C25 C26 -68.7(2) . . . . ? C37 B1 C25 C26 54.9(2) . . . . ? C503 B1 C25 C26 168.32(16) . . . . ? C30 C25 C26 F6 -179.42(16) . . . . ? B1 C25 C26 F6 -1.1(3) . . . . ? C30 C25 C26 C27 2.3(3) . . . . ? B1 C25 C26 C27 -179.31(18) . . . . ? F6 C26 C27 F7 -1.5(3) . . . . ? C25 C26 C27 F7 176.82(18) . . . . ? F6 C26 C27 C28 -179.96(17) . . . . ? C25 C26 C27 C28 -1.7(3) . . . . ? F7 C27 C28 F8 2.3(3) . . . . ? C26 C27 C28 F8 -179.18(17) . . . . ? F7 C27 C28 C29 -178.08(18) . . . . ? C26 C27 C28 C29 0.4(3) . . . . ? F8 C28 C29 F9 -0.3(3) . . . . ? C27 C28 C29 F9 -179.95(18) . . . . ? F8 C28 C29 C30 179.51(18) . . . . ? C27 C28 C29 C30 -0.1(3) . . . . ? F9 C29 C30 F10 0.9(3) . . . . ? C28 C29 C30 F10 -178.94(18) . . . . ? F9 C29 C30 C25 -179.19(18) . . . . ? C28 C29 C30 C25 1.0(3) . . . . ? C26 C25 C30 F10 177.93(17) . . . . ? B1 C25 C30 F10 -0.2(3) . . . . ? C26 C25 C30 C29 -2.0(3) . . . . ? B1 C25 C30 C29 179.86(18) . . . . ? F11 C32 C33 F12 0.5(3) . . . . ? C503 C32 C33 F12 179.45(17) . . . . ? F11 C32 C33 C34 -178.92(16) . . . . ? C503 C32 C33 C34 0.0(3) . . . . ? F12 C33 C34 F13 2.1(3) . . . . ? C32 C33 C34 F13 -178.46(17) . . . . ? F12 C33 C34 C35 -178.03(17) . . . . ? C32 C33 C34 C35 1.4(3) . . . . ? F13 C34 C35 F14 -0.2(3) . . . . ? C33 C34 C35 F14 179.90(17) . . . . ? F13 C34 C35 C36 179.35(17) . . . . ? C33 C34 C35 C36 -0.5(3) . . . . ? F14 C35 C36 F15 -3.0(3) . . . . ? C34 C35 C36 F15 177.43(16) . . . . ? F14 C35 C36 C503 177.66(17) . . . . ? C34 C35 C36 C503 -1.9(3) . . . . ? C19 B1 C37 C42 -52.6(2) . . . . ? C25 B1 C37 C42 -170.46(16) . . . . ? C503 B1 C37 C42 67.3(2) . . . . ? C19 B1 C37 C38 139.01(18) . . . . ? C25 B1 C37 C38 21.1(2) . . . . ? C503 B1 C37 C38 -101.10(19) . . . . ? C42 C37 C38 F16 179.93(16) . . . . ? B1 C37 C38 F16 -11.0(3) . . . . ? C42 C37 C38 C39 -1.9(3) . . . . ? B1 C37 C38 C39 167.24(18) . . . . ? F16 C38 C39 F17 2.4(3) . . . . ? C37 C38 C39 F17 -175.91(17) . . . . ? F16 C38 C39 C40 -178.25(18) . . . . ? C37 C38 C39 C40 3.4(3) . . . . ? F17 C39 C40 F18 -1.4(3) . . . . ? C38 C39 C40 F18 179.24(18) . . . . ? F17 C39 C40 C41 178.49(18) . . . . ? C38 C39 C40 C41 -0.9(3) . . . . ? F18 C40 C41 F19 -1.4(3) . . . . ? C39 C40 C41 F19 178.66(18) . . . . ? F18 C40 C41 C42 176.96(18) . . . . ? C39 C40 C41 C42 -2.9(3) . . . . ? F19 C41 C42 F20 3.8(3) . . . . ? C40 C41 C42 F20 -174.64(17) . . . . ? F19 C41 C42 C37 -176.91(17) . . . . ? C40 C41 C42 C37 4.7(3) . . . . ? C38 C37 C42 F20 177.09(15) . . . . ? B1 C37 C42 F20 7.3(3) . . . . ? C38 C37 C42 C41 -2.2(3) . . . . ? B1 C37 C42 C41 -172.04(17) . . . . ? F15 C36 C503 C32 -176.20(16) . . . . ? C35 C36 C503 C32 3.1(3) . . . . ? F15 C36 C503 B1 -4.7(3) . . . . ? C35 C36 C503 B1 174.53(18) . . . . ? F11 C32 C503 C36 176.73(16) . . . . ? C33 C32 C503 C36 -2.1(3) . . . . ? F11 C32 C503 B1 4.6(3) . . . . ? C33 C32 C503 B1 -174.27(18) . . . . ? C19 B1 C503 C36 15.9(3) . . . . ? C25 B1 C503 C36 134.27(19) . . . . ? C37 B1 C503 C36 -105.0(2) . . . . ? C19 B1 C503 C32 -173.14(16) . . . . ? C25 B1 C503 C32 -54.8(2) . . . . ? C37 B1 C503 C32 66.0(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.25 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.393 _refine_diff_density_min -0.579 _refine_diff_density_rms 0.063 _iucr_refine_instructions_details ; TITL x0881a - SHELXL CELL 0.71073 13.3059 22.9396 26.0492 90.000 90.000 90.000 ZERR 8 0.0002 0.0005 0.0007 0.0000 0.0000 0.0000 LATT 1 SYMM 0.50000 - X , - Y , 0.50000 + Z SYMM 0.50000 + X , 0.50000 - Y , - Z SYMM - X , 0.50000 + Y , 0.50000 - Z SFAC C H B CU F N O UNIT 336 144 8 8 160 40 16 TEMP -163 ACTA HTAB BOND BOND $H CONF WPDB L.S. 6 FMAP 2 PLAN 10 OMIT -2 52.5 OMIT 0 2 1 OMIT 1 0 2 WGHT 0.037300 5.215300 FVAR 1.85306 0.87506 PART 0 REM Cu complex CU1 4 0.303974 0.088465 0.225262 11.00000 0.01212 0.01766 = 0.01846 0.00154 0.00156 0.00036 C1 1 0.354859 -0.008589 0.302003 11.00000 0.02185 0.01829 = 0.02452 0.00303 0.00455 -0.00345 AFIX 43 H1 2 0.294784 0.001890 0.319416 11.00000 -1.20000 AFIX 0 C2 1 0.413363 -0.052503 0.322037 11.00000 0.03169 0.01994 = 0.02889 0.01076 0.00266 -0.00288 AFIX 43 H2 2 0.394243 -0.071948 0.352719 11.00000 -1.20000 AFIX 0 C3 1 0.500735 -0.067709 0.296463 11.00000 0.02873 0.02174 = 0.03730 0.01069 -0.00067 0.00342 AFIX 43 H3 2 0.543023 -0.097453 0.309780 11.00000 -1.20000 AFIX 0 C4 1 0.526151 -0.039346 0.251387 11.00000 0.02054 0.02135 = 0.02968 0.00352 0.00318 0.00422 AFIX 43 H4 2 0.584870 -0.049969 0.232870 11.00000 -1.20000 AFIX 0 C5 1 0.464110 0.004844 0.233888 11.00000 0.01511 0.01622 = 0.01953 -0.00022 -0.00089 -0.00288 C6 1 0.489163 0.041291 0.187509 11.00000 0.01093 0.02083 = 0.01924 0.00172 0.00011 0.00116 AFIX 23 H6A 2 0.536606 0.072583 0.197394 11.00000 -1.20000 H6B 2 0.522178 0.016639 0.161266 11.00000 -1.20000 AFIX 0 C7 1 0.341826 0.024605 0.133574 11.00000 0.01773 0.02041 = 0.02287 -0.00458 -0.00242 -0.00074 AFIX 23 H7A 2 0.348431 -0.014744 0.148812 11.00000 -1.20000 H7B 2 0.371481 0.023620 0.098729 11.00000 -1.20000 AFIX 0 C8 1 0.232040 0.040921 0.130083 11.00000 0.01811 0.01632 = 0.02359 0.00335 -0.00136 -0.00199 C9 1 0.171042 0.023726 0.089820 11.00000 0.02339 0.02260 = 0.02406 0.00179 -0.00655 -0.00275 AFIX 43 H9 2 0.197234 0.000986 0.062434 11.00000 -1.20000 AFIX 0 C10 1 0.071045 0.040357 0.090288 11.00000 0.02342 0.02722 = 0.03394 0.00569 -0.01111 -0.00451 AFIX 43 H10 2 0.027784 0.029116 0.063017 11.00000 -1.20000 AFIX 0 C11 1 0.034369 0.073262 0.130403 11.00000 0.01632 0.02563 = 0.03814 0.01032 -0.00599 -0.00148 AFIX 43 H11 2 -0.033722 0.085707 0.130830 11.00000 -1.20000 AFIX 0 C12 1 0.099026 0.087785 0.170096 11.00000 0.01590 0.01930 = 0.03108 0.00615 -0.00059 0.00052 AFIX 43 H12 2 0.073737 0.109544 0.198309 11.00000 -1.20000 AFIX 0 C13 1 0.419104 0.121694 0.137119 11.00000 0.01960 0.02125 = 0.01690 0.00456 -0.00021 0.00050 AFIX 23 H13A 2 0.363135 0.130654 0.113354 11.00000 -1.20000 H13B 2 0.480929 0.116332 0.116509 11.00000 -1.20000 AFIX 0 C14 1 0.433306 0.171482 0.174030 11.00000 0.01523 0.01933 = 0.02238 0.00520 -0.00165 0.00098 C15 1 0.491251 0.219733 0.161563 11.00000 0.02404 0.02182 = 0.02918 0.00787 0.00198 -0.00250 AFIX 43 H15 2 0.525987 0.221573 0.129742 11.00000 -1.20000 AFIX 0 C16 1 0.497398 0.264902 0.196241 11.00000 0.02372 0.02061 = 0.04413 0.00531 0.00016 -0.00579 AFIX 43 H16 2 0.535728 0.298676 0.188362 11.00000 -1.20000 AFIX 0 C17 1 0.447328 0.260721 0.242644 11.00000 0.02215 0.02154 = 0.03850 -0.00682 -0.00159 -0.00271 AFIX 43 H17 2 0.450594 0.291470 0.267016 11.00000 -1.20000 AFIX 0 C18 1 0.392395 0.210823 0.252816 11.00000 0.01796 0.02465 = 0.02724 -0.00454 0.00220 0.00021 AFIX 43 H18 2 0.358988 0.207560 0.284919 11.00000 -1.20000 AFIX 0 N1 6 0.379292 0.020009 0.258861 11.00000 0.01680 0.01488 = 0.01868 0.00188 0.00077 -0.00203 N2 6 0.396601 0.067527 0.165649 11.00000 0.01283 0.01622 = 0.01811 0.00197 -0.00126 -0.00039 N3 6 0.196551 0.072062 0.169984 11.00000 0.01526 0.01702 = 0.02288 0.00405 -0.00152 -0.00066 N4 6 0.384518 0.166917 0.219106 11.00000 0.01385 0.01879 = 0.02158 0.00051 0.00084 -0.00007 EADP O1 O1' EXYZ O1 O1' SIMU 0.01 N5 > O2' PART 1 N5 6 0.218389 0.114610 0.323533 21.00000 0.01928 0.02630 = 0.03371 -0.00062 -0.00011 0.00153 O1 7 0.200604 0.100112 0.276266 21.00000 0.01721 0.02919 = 0.02393 0.00225 0.00398 0.00106 O2 7 0.307345 0.122941 0.333409 21.00000 0.02576 0.03162 = 0.02979 -0.00118 -0.00279 0.00105 PART 2 SAME N5 > O2 N5' 6 0.241870 0.116183 0.319122 -21.00000 0.01831 0.02279 = 0.02960 0.00371 0.00840 0.00190 O1' 7 0.200604 0.100112 0.276266 -21.00000 0.01721 0.02919 = 0.02393 0.00225 0.00398 0.00106 O2' 7 0.175985 0.124253 0.351417 -21.00000 0.03070 0.02183 = 0.02867 -0.00913 0.01558 0.00485 REM BARF counterion PART 0 B1 3 0.099588 0.302961 0.058912 11.00000 0.01453 0.01013 = 0.01755 0.00016 -0.00117 0.00105 C19 1 0.120509 0.241515 0.027937 11.00000 0.01392 0.01244 = 0.01623 0.00150 0.00340 -0.00115 C20 1 0.194546 0.200717 0.038302 11.00000 0.01578 0.01633 = 0.01406 0.00159 0.00102 -0.00106 C21 1 0.204401 0.148449 0.012272 11.00000 0.01820 0.01575 = 0.02092 0.00433 0.00555 0.00460 C22 1 0.138368 0.135161 -0.026592 11.00000 0.02454 0.01326 = 0.01646 -0.00318 0.00623 -0.00136 C23 1 0.066317 0.175253 -0.040587 11.00000 0.01709 0.02082 = 0.01509 -0.00265 0.00090 -0.00275 C24 1 0.060847 0.227260 -0.014160 11.00000 0.01232 0.01595 = 0.01851 0.00040 0.00138 0.00190 C25 1 0.139978 0.353669 0.019063 11.00000 0.01913 0.01199 = 0.01554 -0.00224 -0.00095 -0.00125 C26 1 0.242819 0.357859 0.009498 11.00000 0.01950 0.01226 = 0.02248 -0.00168 0.00090 0.00035 C27 1 0.286400 0.398483 -0.022451 11.00000 0.02280 0.01731 = 0.02497 -0.00542 0.00719 -0.00465 C28 1 0.226645 0.437341 -0.048282 11.00000 0.03694 0.01543 = 0.01557 0.00014 0.00341 -0.00918 C29 1 0.124118 0.434830 -0.041189 11.00000 0.03432 0.01536 = 0.01906 0.00293 -0.00756 -0.00150 C30 1 0.083527 0.393507 -0.008530 11.00000 0.01833 0.01731 = 0.01961 -0.00084 -0.00323 -0.00103 C32 1 -0.052267 0.362123 0.098293 11.00000 0.01632 0.01518 = 0.01831 0.00172 -0.00255 -0.00144 C33 1 -0.146810 0.371481 0.118366 11.00000 0.02026 0.01778 = 0.01584 -0.00305 -0.00159 0.00613 C34 1 -0.215516 0.326789 0.117419 11.00000 0.01272 0.02753 = 0.01275 0.00250 0.00098 0.00353 C35 1 -0.188120 0.273853 0.097724 11.00000 0.01686 0.01980 = 0.01764 0.00342 0.00043 -0.00461 C36 1 -0.091705 0.266078 0.078574 11.00000 0.01894 0.01305 = 0.01673 -0.00001 -0.00057 0.00254 C37 1 0.154881 0.306257 0.115749 11.00000 0.01291 0.01718 = 0.01805 -0.00299 -0.00017 0.00379 C38 1 0.202913 0.354749 0.136354 11.00000 0.01442 0.02189 = 0.02275 -0.00477 -0.00084 0.00485 C39 1 0.231048 0.358970 0.187393 11.00000 0.01891 0.03429 = 0.02868 -0.01612 -0.00528 0.00490 C40 1 0.216822 0.313006 0.219900 11.00000 0.02683 0.05093 = 0.01666 -0.00879 -0.00506 0.01738 C41 1 0.173163 0.263091 0.201408 11.00000 0.02649 0.03490 = 0.01867 0.00428 0.00246 0.01563 C42 1 0.140740 0.261791 0.151104 11.00000 0.01889 0.02189 = 0.02019 -0.00172 0.00106 0.00570 C503 1 -0.019633 0.309976 0.076611 11.00000 0.01559 0.01346 = 0.01334 0.00161 -0.00159 0.00198 F1 5 0.261939 0.209181 0.076590 11.00000 0.01826 0.02040 = 0.02246 -0.00086 -0.00509 0.00462 F2 5 0.278533 0.110875 0.024334 11.00000 0.02516 0.01883 = 0.02735 0.00076 0.00247 0.01075 F3 5 0.145923 0.083851 -0.051418 11.00000 0.03766 0.01596 = 0.02799 -0.00885 0.00329 0.00217 F4 5 0.003986 0.163398 -0.079890 11.00000 0.02380 0.02889 = 0.02175 -0.00942 -0.00420 -0.00162 F5 5 -0.010646 0.265268 -0.029845 11.00000 0.01808 0.02098 = 0.02098 -0.00105 -0.00419 0.00395 F6 5 0.305954 0.320960 0.033773 11.00000 0.01539 0.02118 = 0.03386 0.00465 0.00270 0.00273 F7 5 0.387199 0.401489 -0.027843 11.00000 0.02231 0.02551 = 0.04495 -0.00042 0.01528 -0.00570 F8 5 0.267141 0.476914 -0.080143 11.00000 0.04967 0.02154 = 0.02765 0.00596 0.00746 -0.01466 F9 5 0.064023 0.472665 -0.066298 11.00000 0.04213 0.02285 = 0.03170 0.01266 -0.01355 -0.00340 F10 5 -0.018086 0.394245 -0.005036 11.00000 0.01685 0.02346 = 0.03168 0.00742 -0.00681 -0.00003 F11 5 0.012178 0.407972 0.101358 11.00000 0.01806 0.01389 = 0.03157 -0.00602 -0.00112 -0.00091 F12 5 -0.171832 0.423412 0.139071 11.00000 0.02455 0.02256 = 0.03039 -0.01007 0.00118 0.00810 F13 5 -0.309400 0.334724 0.135609 11.00000 0.01407 0.03459 = 0.02099 0.00053 0.00418 0.00446 F14 5 -0.255006 0.229837 0.096740 11.00000 0.01856 0.02457 = 0.03450 0.00137 0.00495 -0.00827 F15 5 -0.071706 0.211717 0.062104 11.00000 0.02083 0.01316 = 0.03049 -0.00353 0.00448 -0.00292 F16 5 0.223072 0.402274 0.107490 11.00000 0.02381 0.01882 = 0.02996 -0.00610 -0.00043 -0.00521 F17 5 0.271931 0.409173 0.205133 11.00000 0.03113 0.04681 = 0.04054 -0.02647 -0.01036 0.00013 F18 5 0.245186 0.316789 0.269405 11.00000 0.04813 0.07671 = 0.01554 -0.01487 -0.01086 0.02556 F19 5 0.160048 0.216705 0.232267 11.00000 0.04567 0.04677 = 0.01843 0.01278 0.00553 0.02146 F20 5 0.090938 0.213053 0.136821 11.00000 0.03075 0.01815 = 0.02508 0.00612 0.00291 -0.00029 HKLF 4 REM x0881a - SHELXL REM R1 = 0.0317 for 6640 Fo > 4sig(Fo) and 0.0428 for all 8030 data REM 659 parameters refined using 63 restraints END WGHT 0.0373 5.2153 REM Highest difference peak 0.393, deepest hole -0.579, 1-sigma level 0.063 Q1 1 0.3028 0.1262 0.2474 11.00000 0.05 0.39 Q2 1 0.3040 0.0501 0.2533 11.00000 0.05 0.35 Q3 1 0.4625 0.1923 0.1689 11.00000 0.05 0.33 Q4 1 0.1169 0.3286 0.0367 11.00000 0.05 0.32 Q5 1 0.3142 0.1361 0.2124 11.00000 0.05 0.32 Q6 1 0.4294 0.1504 0.1561 11.00000 0.05 0.32 Q7 1 0.0390 0.3075 0.0658 11.00000 0.05 0.31 Q8 1 0.2279 0.3512 0.1609 11.00000 0.05 0.31 Q9 1 0.1157 0.1614 -0.0388 11.00000 0.05 0.29 Q10 1 0.0954 0.1562 -0.0304 11.00000 0.05 0.28 ;