data_2_sub2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C52 H66 Cu2 N6 O4 S2, 2(C24 B F20), 2(C5 H12)' _chemical_formula_sum 'C110 H90 B2 Cu2 F40 N6 O4 S2' _chemical_formula_weight 2532.70 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 0.0090 0.0039 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0727 0.0534 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.3331 0.5567 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.5520(5) _cell_length_b 14.6344(5) _cell_length_c 15.0327(6) _cell_angle_alpha 67.739(3) _cell_angle_beta 88.928(3) _cell_angle_gamma 65.891(3) _cell_volume 2669.02(17) _cell_formula_units_Z 1 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 17137 _cell_measurement_theta_min 3.60 _cell_measurement_theta_max 71.89 _exptl_crystal_description needle _exptl_crystal_colour colorless _exptl_crystal_size_max 0.49 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.576 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1284 _exptl_absorpt_coefficient_mu 1.989 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.572 _exptl_absorpt_correction_T_max 0.880 _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) 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 100(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator 'mirror' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean 10.3875 _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 31449 _diffrn_reflns_av_R_equivalents 0.0211 _diffrn_reflns_av_sigmaI/netI 0.0197 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.37 _diffrn_reflns_theta_max 71.90 _reflns_number_total 10473 _reflns_number_gt 9658 _reflns_threshold_expression 'I>2\s(I)' _computing_data_collection ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_cell_refinement ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _computing_data_reduction ; CrysAlisPro, Agilent Technologies, Version 1.171.36.24 (release 03-12-2012 CrysAlis171 .NET) (compiled Dec 3 2012,18:21:49) ; _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^)+(0.0397P)^2^+1.4385P] 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 10473 _refine_ls_number_parameters 852 _refine_ls_number_restraints 317 _refine_ls_R_factor_all 0.0324 _refine_ls_R_factor_gt 0.0297 _refine_ls_wR_factor_ref 0.0784 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 1.037838(15) 0.607888(16) 0.569939(14) 0.01555(6) Uani 1 1 d . . . C1 C 0.81533(11) 0.75260(12) 0.55803(11) 0.0191(3) Uani 1 1 d . . . H1 H 0.8162 0.6913 0.6119 0.023 Uiso 1 1 calc R . . C2 C 0.72440(11) 0.84720(13) 0.52127(11) 0.0199(3) Uani 1 1 d . . . C3 C 0.72524(11) 0.93563(12) 0.44131(11) 0.0203(3) Uani 1 1 d . . . C4 C 0.81534(12) 0.92989(12) 0.40369(11) 0.0192(3) Uani 1 1 d . . . C5 C 0.90204(11) 0.82994(12) 0.44600(10) 0.0174(3) Uani 1 1 d . . . C6 C 1.00490(11) 0.81558(11) 0.41486(11) 0.0181(3) Uani 1 1 d . . . H6A H 0.9947 0.8662 0.3459 0.022 Uiso 1 1 calc R . . H6B H 1.0415 0.8347 0.4547 0.022 Uiso 1 1 calc R . . C7 C 1.17695(11) 0.67236(12) 0.44691(10) 0.0170(3) Uani 1 1 d . . . H7A H 1.1938 0.7266 0.3951 0.020 Uiso 1 1 calc R . . H7B H 1.2181 0.5996 0.4463 0.020 Uiso 1 1 calc R . . C8 C 1.20444(11) 0.66985(11) 0.54460(10) 0.0160(3) Uani 1 1 d . . . C9 C 1.28006(11) 0.69988(12) 0.56128(10) 0.0176(3) Uani 1 1 d . . . C10 C 1.30169(11) 0.69027(11) 0.65564(11) 0.0177(3) Uani 1 1 d . . . C11 C 1.25028(12) 0.65275(13) 0.72910(11) 0.0214(3) Uani 1 1 d . . . C12 C 1.17619(12) 0.62638(13) 0.70409(11) 0.0208(3) Uani 1 1 d . . . H12 H 1.1398 0.6010 0.7532 0.025 Uiso 1 1 calc R . . C13 C 0.63058(12) 0.85541(14) 0.56767(12) 0.0255(3) Uani 1 1 d . . . H13A H 0.6424 0.7831 0.6169 0.038 Uiso 1 1 calc R . . H13B H 0.5728 0.8815 0.5177 0.038 Uiso 1 1 calc R . . H13C H 0.6154 0.9069 0.5986 0.038 Uiso 1 1 calc R . . C14 C 0.59382(13) 1.06727(14) 0.30677(13) 0.0305(4) Uani 1 1 d . . . H14A H 0.5306 1.1347 0.2891 0.046 Uiso 0.50 1 calc PR . . H14B H 0.5791 1.0110 0.2987 0.046 Uiso 0.50 1 calc PR . . H14C H 0.6427 1.0819 0.2645 0.046 Uiso 0.50 1 calc PR . . H14D H 0.6377 1.0170 0.2791 0.046 Uiso 0.50 1 calc PR . . H14E H 0.5891 1.1408 0.2695 0.046 Uiso 0.50 1 calc PR . . H14F H 0.5256 1.0698 0.3037 0.046 Uiso 0.50 1 calc PR . . C15 C 0.82042(12) 1.02933(12) 0.32644(12) 0.0246(3) Uani 1 1 d . . . H15A H 0.8200 1.0241 0.2634 0.037 Uiso 1 1 calc R . . H15B H 0.8832 1.0330 0.3432 0.037 Uiso 1 1 calc R . . H15C H 0.7613 1.0956 0.3225 0.037 Uiso 1 1 calc R . . C16 C 1.33658(13) 0.74104(15) 0.48237(12) 0.0271(3) Uani 1 1 d . . . H16A H 1.3725 0.7751 0.5034 0.041 Uiso 1 1 calc R . . H16B H 1.2879 0.7953 0.4227 0.041 Uiso 1 1 calc R . . H16C H 1.3860 0.6795 0.4697 0.041 Uiso 1 1 calc R . . C17 C 1.47478(12) 0.64283(14) 0.70029(14) 0.0285(4) Uani 1 1 d . . . H17A H 1.4839 0.5828 0.7630 0.043 Uiso 1 1 calc R . . H17B H 1.5203 0.6756 0.7049 0.043 Uiso 1 1 calc R . . H17C H 1.4911 0.6143 0.6497 0.043 Uiso 1 1 calc R . . C18 C 1.27221(16) 0.64297(18) 0.83059(12) 0.0355(4) Uani 1 1 d . . . H18A H 1.2255 0.6192 0.8704 0.053 Uiso 1 1 calc R . . H18B H 1.2626 0.7143 0.8280 0.053 Uiso 1 1 calc R . . H18C H 1.3428 0.5890 0.8594 0.053 Uiso 1 1 calc R . . C19 C 1.04512(11) 0.68982(12) 0.33648(10) 0.0165(3) Uani 1 1 d . . . H19A H 1.0923 0.7063 0.2916 0.020 Uiso 1 1 calc R . . H19B H 0.9748 0.7448 0.3040 0.020 Uiso 1 1 calc R . . C20 C 1.05466(11) 0.57651(12) 0.35416(10) 0.0168(3) Uani 1 1 d . A . H20A H 1.1132 0.5204 0.4063 0.020 Uiso 1 1 calc R . . H20B H 1.0686 0.5638 0.2941 0.020 Uiso 1 1 calc R . . S1 S 0.93945(2) 0.56110(3) 0.38914(2) 0.01521(7) Uani 1 1 d D . . C21 C 0.8553(9) 0.6507(8) 0.2754(6) 0.0198(7) Uani 0.665(16) 1 d PDU A 1 C22 C 0.8731(5) 0.6292(5) 0.1921(4) 0.0289(11) Uani 0.665(16) 1 d PDU A 1 H22 H 0.9287 0.5640 0.1955 0.035 Uiso 0.665(16) 1 calc PR A 1 C23 C 0.8089(6) 0.7036(4) 0.1045(4) 0.0389(12) Uani 0.665(16) 1 d PDU A 1 H23 H 0.8206 0.6887 0.0480 0.047 Uiso 0.665(16) 1 calc PR A 1 C24 C 0.7282(5) 0.7992(4) 0.0984(5) 0.0345(12) Uani 0.665(16) 1 d PDU A 1 H24 H 0.6846 0.8494 0.0380 0.041 Uiso 0.665(16) 1 calc PR A 1 C25 C 0.7107(6) 0.8217(6) 0.1795(5) 0.0293(15) Uani 0.665(16) 1 d PDU A 1 H25 H 0.6551 0.8874 0.1753 0.035 Uiso 0.665(16) 1 calc PR A 1 C26 C 0.7747(8) 0.7478(8) 0.2683(6) 0.0220(13) Uani 0.665(16) 1 d PDU A 1 H26 H 0.7632 0.7640 0.3242 0.026 Uiso 0.665(16) 1 calc PR A 1 C21' C 0.8497(19) 0.6580(17) 0.2819(12) 0.0198(7) Uani 0.335(16) 1 d PDU A 2 C22' C 0.8442(9) 0.6307(10) 0.2049(9) 0.032(2) Uani 0.335(16) 1 d PDU A 2 H22' H 0.8900 0.5609 0.2074 0.038 Uiso 0.335(16) 1 calc PR A 2 C23' C 0.7700(10) 0.7073(7) 0.1224(8) 0.0375(19) Uani 0.335(16) 1 d PDU A 2 H23' H 0.7674 0.6920 0.0667 0.045 Uiso 0.335(16) 1 calc PR A 2 C24' C 0.7008(10) 0.8053(8) 0.1234(10) 0.033(2) Uani 0.335(16) 1 d PDU A 2 H24' H 0.6508 0.8581 0.0676 0.040 Uiso 0.335(16) 1 calc PR A 2 C25' C 0.7036(12) 0.8272(12) 0.2043(10) 0.023(2) Uani 0.335(16) 1 d PDU A 2 H25' H 0.6540 0.8942 0.2042 0.028 Uiso 0.335(16) 1 calc PR A 2 C26' C 0.7772(16) 0.7536(15) 0.2860(11) 0.018(2) Uani 0.335(16) 1 d PDU A 2 H26' H 0.7780 0.7679 0.3425 0.022 Uiso 0.335(16) 1 calc PR A 2 N1 N 0.90236(9) 0.74278(10) 0.52172(9) 0.0177(2) Uani 1 1 d . . . N2 N 1.06777(9) 0.70114(9) 0.42626(8) 0.0152(2) Uani 1 1 d . . . N3 N 1.15271(9) 0.63452(10) 0.61442(9) 0.0168(2) Uani 1 1 d . . . O1 O 0.63624(9) 1.02961(10) 0.40605(9) 0.0307(3) Uani 1 1 d . . . O2 O 1.37088(8) 0.72447(9) 0.67567(8) 0.0212(2) Uani 1 1 d . . . B1 B 0.35574(12) 0.77360(12) 0.12200(11) 0.0135(3) Uani 1 1 d . . . C27 C 0.43356(10) 0.76294(11) 0.04097(10) 0.0148(3) Uani 1 1 d . . . C28 C 0.46196(11) 0.84738(11) -0.00539(10) 0.0158(3) Uani 1 1 d . . . C29 C 0.52770(11) 0.84758(12) -0.07280(10) 0.0184(3) Uani 1 1 d . . . C30 C 0.57276(11) 0.75699(13) -0.09460(11) 0.0200(3) Uani 1 1 d . . . C31 C 0.55027(11) 0.66942(12) -0.04918(11) 0.0196(3) Uani 1 1 d . . . C32 C 0.48230(11) 0.67388(12) 0.01680(10) 0.0172(3) Uani 1 1 d . . . C33 C 0.31723(10) 0.67506(11) 0.15815(10) 0.0140(3) Uani 1 1 d . . . C34 C 0.26461(11) 0.66524(11) 0.08826(10) 0.0157(3) Uani 1 1 d . . . C35 C 0.22510(11) 0.58973(13) 0.10812(11) 0.0186(3) Uani 1 1 d . . . C36 C 0.23862(11) 0.51672(12) 0.20280(11) 0.0189(3) Uani 1 1 d . . . C37 C 0.28780(11) 0.52351(11) 0.27554(10) 0.0171(3) Uani 1 1 d . . . C38 C 0.32473(10) 0.60201(11) 0.25267(10) 0.0151(3) Uani 1 1 d . . . C39 C 0.42446(10) 0.77038(11) 0.21034(10) 0.0138(3) Uani 1 1 d . . . C40 C 0.51402(11) 0.67626(11) 0.26047(10) 0.0160(3) Uani 1 1 d . . . C41 C 0.57855(11) 0.66362(12) 0.33477(11) 0.0197(3) Uani 1 1 d . . . C42 C 0.55579(12) 0.74919(13) 0.36242(11) 0.0201(3) Uani 1 1 d . . . C43 C 0.47038(11) 0.84565(12) 0.31387(11) 0.0182(3) Uani 1 1 d . . . C44 C 0.40786(11) 0.85493(11) 0.23924(10) 0.0151(3) Uani 1 1 d . . . C45 C 0.24676(11) 0.88589(11) 0.07777(10) 0.0143(3) Uani 1 1 d . . . C46 C 0.17795(11) 0.91071(11) 0.14025(10) 0.0154(3) Uani 1 1 d . . . C47 C 0.08396(11) 1.00046(12) 0.11281(11) 0.0188(3) Uani 1 1 d . . . C48 C 0.05291(11) 1.07227(12) 0.01580(12) 0.0212(3) Uani 1 1 d . . . C49 C 0.11587(12) 1.05004(12) -0.05005(11) 0.0211(3) Uani 1 1 d . . . C50 C 0.20916(11) 0.95882(12) -0.01918(10) 0.0172(3) Uani 1 1 d . . . F1 F 0.42243(7) 0.93756(7) 0.01442(6) 0.01936(17) Uani 1 1 d . . . F2 F 0.54825(7) 0.93441(8) -0.11684(7) 0.02516(19) Uani 1 1 d . . . F3 F 0.63742(7) 0.75434(8) -0.15980(7) 0.0292(2) Uani 1 1 d . . . F4 F 0.59444(7) 0.58040(8) -0.06930(7) 0.0278(2) Uani 1 1 d . . . F5 F 0.46652(7) 0.58295(7) 0.05787(7) 0.02225(18) Uani 1 1 d . . . F6 F 0.25124(7) 0.73239(7) -0.00633(6) 0.01976(18) Uani 1 1 d . . . F7 F 0.17537(7) 0.58499(8) 0.03661(7) 0.0261(2) Uani 1 1 d . . . F8 F 0.20323(7) 0.44022(8) 0.22395(7) 0.0265(2) Uani 1 1 d . . . F9 F 0.30077(7) 0.45296(7) 0.36896(6) 0.02288(19) Uani 1 1 d . . . F10 F 0.37002(6) 0.60251(7) 0.33026(6) 0.01864(17) Uani 1 1 d . . . F11 F 0.54086(7) 0.58886(7) 0.23734(6) 0.02068(18) Uani 1 1 d . . . F12 F 0.66262(7) 0.56943(8) 0.38071(7) 0.0291(2) Uani 1 1 d . . . F13 F 0.61708(8) 0.73866(8) 0.43508(7) 0.0302(2) Uani 1 1 d . . . F14 F 0.44749(7) 0.92994(8) 0.34000(7) 0.0261(2) Uani 1 1 d . . . F15 F 0.32722(6) 0.95373(7) 0.19554(6) 0.01932(17) Uani 1 1 d . . . F16 F 0.20354(6) 0.84376(7) 0.23664(6) 0.01840(17) Uani 1 1 d . . . F17 F 0.02272(7) 1.01775(8) 0.17864(7) 0.02508(19) Uani 1 1 d . . . F18 F -0.03746(7) 1.16041(8) -0.01353(8) 0.0316(2) Uani 1 1 d . . . F19 F 0.08490(7) 1.11682(8) -0.14541(7) 0.0309(2) Uani 1 1 d . . . F20 F 0.26254(7) 0.94371(7) -0.09116(6) 0.02212(18) Uani 1 1 d . . . C1S C 0.0944(4) 0.0239(4) 0.4037(4) 0.0493(11) Uani 0.668(4) 1 d PDU B 1 H1S1 H 0.0587 0.0743 0.4342 0.074 Uiso 0.668(4) 1 calc PR B 1 H1S2 H 0.1438 -0.0459 0.4534 0.074 Uiso 0.668(4) 1 calc PR B 1 H1S3 H 0.0449 0.0112 0.3726 0.074 Uiso 0.668(4) 1 calc PR B 1 C2S C 0.1505(3) 0.0740(3) 0.3267(3) 0.0459(8) Uani 0.668(4) 1 d PDU B 1 H2S1 H 0.2088 0.0742 0.3595 0.055 Uiso 0.668(4) 1 calc PR B 1 H2S2 H 0.1779 0.0284 0.2892 0.055 Uiso 0.668(4) 1 calc PR B 1 C3S C 0.0812(3) 0.1885(3) 0.2585(3) 0.0469(9) Uani 0.668(4) 1 d PDU B 1 H3S1 H 0.0510 0.2326 0.2968 0.056 Uiso 0.668(4) 1 calc PR B 1 H3S2 H 0.0248 0.1874 0.2238 0.056 Uiso 0.668(4) 1 calc PR B 1 C4S C 0.1349(3) 0.2435(4) 0.1840(3) 0.0621(10) Uani 0.668(4) 1 d PDU B 1 H4S1 H 0.1920 0.2437 0.2188 0.074 Uiso 0.668(4) 1 calc PR B 1 H4S2 H 0.1643 0.2001 0.1451 0.074 Uiso 0.668(4) 1 calc PR B 1 C5S C 0.0657(4) 0.3589(4) 0.1166(4) 0.0721(13) Uani 0.668(4) 1 d PDU B 1 H5S1 H 0.0120 0.3590 0.0782 0.108 Uiso 0.668(4) 1 calc PR B 1 H5S2 H 0.1052 0.3914 0.0727 0.108 Uiso 0.668(4) 1 calc PR B 1 H5S3 H 0.0347 0.4020 0.1547 0.108 Uiso 0.668(4) 1 calc PR B 1 C1' C 0.1325(11) 0.0125(11) 0.3868(11) 0.086(4) Uani 0.332(4) 1 d PDU B 2 H1'1 H 0.1512 -0.0326 0.3492 0.129 Uiso 0.332(4) 1 calc PR B 2 H1'2 H 0.0964 -0.0149 0.4385 0.129 Uiso 0.332(4) 1 calc PR B 2 H1'3 H 0.1942 0.0089 0.4159 0.129 Uiso 0.332(4) 1 calc PR B 2 C2' C 0.0635(6) 0.1304(7) 0.3201(6) 0.0550(17) Uani 0.332(4) 1 d PDU B 2 H2'1 H 0.0448 0.1773 0.3569 0.066 Uiso 0.332(4) 1 calc PR B 2 H2'2 H 0.0003 0.1356 0.2908 0.066 Uiso 0.332(4) 1 calc PR B 2 C3' C 0.1249(8) 0.1673(8) 0.2397(7) 0.0631(19) Uani 0.332(4) 1 d PDU B 2 H3'1 H 0.1458 0.1191 0.2042 0.076 Uiso 0.332(4) 1 calc PR B 2 H3'2 H 0.1867 0.1655 0.2684 0.076 Uiso 0.332(4) 1 calc PR B 2 C4' C 0.0489(8) 0.2892(9) 0.1690(8) 0.094(3) Uani 0.332(4) 1 d PDU B 2 H4'1 H -0.0173 0.2909 0.1520 0.113 Uiso 0.332(4) 1 calc PR B 2 H4'2 H 0.0369 0.3374 0.2040 0.113 Uiso 0.332(4) 1 calc PR B 2 C5' C 0.0875(13) 0.3335(14) 0.0775(11) 0.128(5) Uani 0.332(4) 1 d PDU B 2 H5'1 H 0.1388 0.3559 0.0910 0.191 Uiso 0.332(4) 1 calc PR B 2 H5'2 H 0.0307 0.3970 0.0289 0.191 Uiso 0.332(4) 1 calc PR B 2 H5'3 H 0.1185 0.2768 0.0523 0.191 Uiso 0.332(4) 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01455(11) 0.01352(10) 0.01347(10) -0.00162(8) 0.00214(8) -0.00493(8) C1 0.0196(7) 0.0182(7) 0.0188(7) -0.0067(6) 0.0046(6) -0.0084(6) C2 0.0177(7) 0.0222(7) 0.0216(7) -0.0117(6) 0.0050(6) -0.0078(6) C3 0.0181(7) 0.0172(7) 0.0204(7) -0.0082(6) 0.0017(6) -0.0023(6) C4 0.0207(7) 0.0159(7) 0.0171(7) -0.0059(6) 0.0024(6) -0.0050(6) C5 0.0185(7) 0.0162(7) 0.0156(7) -0.0059(5) 0.0031(5) -0.0063(6) C6 0.0171(7) 0.0139(6) 0.0182(7) -0.0027(5) 0.0026(5) -0.0054(5) C7 0.0156(7) 0.0207(7) 0.0126(6) -0.0048(5) 0.0028(5) -0.0076(6) C8 0.0156(6) 0.0153(6) 0.0138(6) -0.0045(5) 0.0026(5) -0.0049(5) C9 0.0172(7) 0.0176(7) 0.0160(7) -0.0060(5) 0.0031(5) -0.0064(6) C10 0.0169(7) 0.0152(6) 0.0198(7) -0.0083(5) 0.0018(5) -0.0047(5) C11 0.0236(7) 0.0243(7) 0.0158(7) -0.0091(6) 0.0033(6) -0.0091(6) C12 0.0226(7) 0.0253(7) 0.0147(7) -0.0076(6) 0.0060(6) -0.0110(6) C13 0.0203(7) 0.0272(8) 0.0292(8) -0.0140(7) 0.0102(6) -0.0083(6) C14 0.0210(8) 0.0266(8) 0.0334(9) -0.0080(7) -0.0040(7) -0.0042(7) C15 0.0238(8) 0.0158(7) 0.0251(8) -0.0034(6) 0.0047(6) -0.0047(6) C16 0.0294(8) 0.0385(9) 0.0215(8) -0.0110(7) 0.0078(6) -0.0234(8) C17 0.0184(8) 0.0277(8) 0.0403(10) -0.0165(7) 0.0005(7) -0.0082(7) C18 0.0436(11) 0.0573(12) 0.0198(8) -0.0199(8) 0.0098(7) -0.0311(10) C19 0.0164(6) 0.0185(7) 0.0109(6) -0.0019(5) 0.0008(5) -0.0078(5) C20 0.0144(6) 0.0187(7) 0.0151(6) -0.0055(5) 0.0041(5) -0.0067(5) S1 0.01392(15) 0.01399(15) 0.01287(15) -0.00196(12) 0.00055(12) -0.00475(12) C21 0.0208(14) 0.0145(14) 0.0193(12) -0.0013(8) -0.0048(12) -0.0082(9) C22 0.037(2) 0.0240(14) 0.0187(16) -0.0071(12) -0.0057(16) -0.0074(17) C23 0.050(3) 0.0348(16) 0.0245(17) -0.0081(13) -0.0104(17) -0.0140(18) C24 0.037(2) 0.0284(17) 0.025(2) 0.0047(15) -0.0165(17) -0.0161(17) C25 0.0233(18) 0.0202(17) 0.029(3) 0.002(2) -0.008(2) -0.0060(13) C26 0.0186(16) 0.0212(16) 0.023(3) -0.0047(17) 0.0004(19) -0.0097(13) C21' 0.0208(14) 0.0145(14) 0.0193(12) -0.0013(8) -0.0048(12) -0.0082(9) C22' 0.036(4) 0.018(2) 0.028(3) -0.004(2) -0.004(3) -0.005(3) C23' 0.046(4) 0.033(3) 0.026(3) -0.006(2) -0.017(3) -0.014(3) C24' 0.035(4) 0.020(3) 0.031(4) 0.002(3) -0.012(3) -0.009(3) C25' 0.020(3) 0.019(3) 0.027(5) -0.005(3) -0.005(3) -0.008(2) C26' 0.015(3) 0.016(3) 0.019(4) -0.004(3) -0.005(3) -0.005(2) N1 0.0174(6) 0.0156(6) 0.0168(6) -0.0048(5) 0.0033(5) -0.0057(5) N2 0.0139(6) 0.0156(6) 0.0131(5) -0.0040(4) 0.0017(4) -0.0052(5) N3 0.0165(6) 0.0169(6) 0.0135(6) -0.0042(5) 0.0031(4) -0.0059(5) O1 0.0220(6) 0.0235(6) 0.0266(6) -0.0056(5) 0.0042(5) 0.0041(5) O2 0.0190(5) 0.0203(5) 0.0259(5) -0.0121(4) 0.0013(4) -0.0075(4) B1 0.0156(7) 0.0128(7) 0.0116(7) -0.0046(6) 0.0026(6) -0.0061(6) C27 0.0141(6) 0.0170(6) 0.0129(6) -0.0057(5) 0.0017(5) -0.0065(5) C28 0.0171(7) 0.0157(6) 0.0150(6) -0.0067(5) 0.0016(5) -0.0069(5) C29 0.0183(7) 0.0209(7) 0.0162(7) -0.0039(6) 0.0027(5) -0.0119(6) C30 0.0156(7) 0.0285(8) 0.0160(7) -0.0091(6) 0.0068(5) -0.0098(6) C31 0.0186(7) 0.0210(7) 0.0211(7) -0.0128(6) 0.0054(6) -0.0066(6) C32 0.0184(7) 0.0173(7) 0.0177(7) -0.0071(5) 0.0042(5) -0.0096(6) C33 0.0136(6) 0.0135(6) 0.0148(6) -0.0069(5) 0.0046(5) -0.0048(5) C34 0.0167(6) 0.0177(7) 0.0129(6) -0.0066(5) 0.0052(5) -0.0073(5) C35 0.0193(7) 0.0245(7) 0.0203(7) -0.0149(6) 0.0076(6) -0.0121(6) C36 0.0194(7) 0.0183(7) 0.0267(8) -0.0128(6) 0.0116(6) -0.0123(6) C37 0.0168(7) 0.0156(6) 0.0156(7) -0.0047(5) 0.0069(5) -0.0058(5) C38 0.0130(6) 0.0162(6) 0.0154(6) -0.0076(5) 0.0033(5) -0.0047(5) C39 0.0149(6) 0.0144(6) 0.0124(6) -0.0045(5) 0.0040(5) -0.0076(5) C40 0.0173(7) 0.0146(6) 0.0165(7) -0.0067(5) 0.0036(5) -0.0071(5) C41 0.0161(7) 0.0181(7) 0.0188(7) -0.0036(6) -0.0011(5) -0.0053(6) C42 0.0204(7) 0.0273(8) 0.0149(7) -0.0079(6) 0.0005(6) -0.0130(6) C43 0.0222(7) 0.0213(7) 0.0180(7) -0.0113(6) 0.0065(6) -0.0129(6) C44 0.0149(6) 0.0143(6) 0.0144(6) -0.0047(5) 0.0031(5) -0.0059(5) C45 0.0160(6) 0.0141(6) 0.0133(6) -0.0046(5) 0.0018(5) -0.0078(5) C46 0.0181(7) 0.0146(6) 0.0118(6) -0.0030(5) 0.0000(5) -0.0077(5) C47 0.0161(7) 0.0198(7) 0.0217(7) -0.0095(6) 0.0046(6) -0.0080(6) C48 0.0138(7) 0.0153(7) 0.0266(8) -0.0037(6) -0.0028(6) -0.0032(6) C49 0.0214(7) 0.0203(7) 0.0151(7) 0.0010(6) -0.0035(6) -0.0104(6) C50 0.0193(7) 0.0195(7) 0.0134(6) -0.0053(5) 0.0025(5) -0.0102(6) F1 0.0242(4) 0.0163(4) 0.0209(4) -0.0087(3) 0.0065(3) -0.0108(3) F2 0.0299(5) 0.0270(5) 0.0232(4) -0.0066(4) 0.0099(4) -0.0200(4) F3 0.0256(5) 0.0389(5) 0.0266(5) -0.0155(4) 0.0167(4) -0.0160(4) F4 0.0291(5) 0.0272(5) 0.0341(5) -0.0214(4) 0.0160(4) -0.0109(4) F5 0.0269(5) 0.0176(4) 0.0284(5) -0.0127(4) 0.0126(4) -0.0126(4) F6 0.0254(4) 0.0251(4) 0.0124(4) -0.0072(3) 0.0034(3) -0.0148(4) F7 0.0321(5) 0.0385(5) 0.0242(5) -0.0189(4) 0.0090(4) -0.0250(4) F8 0.0352(5) 0.0269(5) 0.0327(5) -0.0163(4) 0.0166(4) -0.0242(4) F9 0.0266(5) 0.0193(4) 0.0185(4) -0.0020(3) 0.0073(3) -0.0113(4) F10 0.0211(4) 0.0214(4) 0.0128(4) -0.0049(3) 0.0017(3) -0.0105(3) F11 0.0201(4) 0.0140(4) 0.0255(4) -0.0094(3) 0.0005(3) -0.0036(3) F12 0.0211(5) 0.0218(5) 0.0304(5) -0.0051(4) -0.0092(4) -0.0010(4) F13 0.0292(5) 0.0380(5) 0.0242(5) -0.0136(4) -0.0068(4) -0.0141(4) F14 0.0314(5) 0.0266(5) 0.0295(5) -0.0194(4) 0.0040(4) -0.0138(4) F15 0.0186(4) 0.0135(4) 0.0235(4) -0.0081(3) 0.0001(3) -0.0041(3) F16 0.0201(4) 0.0196(4) 0.0109(4) -0.0036(3) 0.0037(3) -0.0067(3) F17 0.0184(4) 0.0274(5) 0.0282(5) -0.0141(4) 0.0086(4) -0.0064(4) F18 0.0167(4) 0.0220(5) 0.0380(6) -0.0038(4) -0.0035(4) 0.0009(4) F19 0.0273(5) 0.0291(5) 0.0171(4) 0.0069(4) -0.0070(4) -0.0089(4) F20 0.0230(4) 0.0281(5) 0.0116(4) -0.0047(3) 0.0035(3) -0.0108(4) C1S 0.050(3) 0.058(2) 0.060(2) -0.0371(19) 0.0138(19) -0.030(2) C2S 0.0403(17) 0.058(2) 0.061(2) -0.0424(17) 0.0141(15) -0.0244(15) C3S 0.0426(19) 0.056(2) 0.062(2) -0.0356(17) 0.0088(17) -0.0294(17) C4S 0.054(2) 0.074(2) 0.073(2) -0.035(2) 0.0218(18) -0.0379(19) C5S 0.076(3) 0.074(3) 0.090(4) -0.046(3) 0.031(3) -0.044(3) C1' 0.095(9) 0.086(7) 0.093(8) -0.048(6) -0.006(7) -0.042(7) C2' 0.055(3) 0.066(3) 0.070(4) -0.050(3) 0.015(3) -0.030(3) C3' 0.056(4) 0.080(4) 0.073(4) -0.041(3) 0.025(3) -0.039(3) C4' 0.062(4) 0.090(4) 0.102(5) -0.006(4) 0.014(4) -0.038(4) C5' 0.092(8) 0.134(9) 0.117(9) -0.026(8) 0.014(7) -0.036(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N1 2.0246(12) . ? Cu1 N3 2.0408(13) . ? Cu1 S1 2.1889(4) 2_766 ? Cu1 N2 2.2213(12) . ? C1 N1 1.3444(19) . ? C1 C2 1.387(2) . ? C1 H1 0.9500 . ? C2 C3 1.398(2) . ? C2 C13 1.503(2) . ? C3 O1 1.3668(18) . ? C3 C4 1.401(2) . ? C4 C5 1.398(2) . ? C4 C15 1.509(2) . ? C5 N1 1.3483(19) . ? C5 C6 1.515(2) . ? C6 N2 1.4859(18) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C7 N2 1.4733(18) . ? C7 C8 1.5122(19) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 N3 1.3464(18) . ? C8 C9 1.398(2) . ? C9 C10 1.400(2) . ? C9 C16 1.508(2) . ? C10 O2 1.3754(18) . ? C10 C11 1.388(2) . ? C11 C12 1.385(2) . ? C11 C18 1.505(2) . ? C12 N3 1.3455(19) . ? C12 H12 0.9500 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 O1 1.430(2) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C14 H14D 0.9800 . ? C14 H14E 0.9800 . ? C14 H14F 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 O2 1.4355(19) . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 N2 1.4793(18) . ? C19 C20 1.523(2) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C20 S1 1.8233(14) . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? S1 C21' 1.774(11) . ? S1 C21 1.791(6) . ? S1 Cu1 2.1888(4) 2_766 ? C21 C26 1.390(7) . ? C21 C22 1.399(7) . ? C22 C23 1.386(5) . ? C22 H22 0.9500 . ? C23 C24 1.382(6) . ? C23 H23 0.9500 . ? C24 C25 1.372(6) . ? C24 H24 0.9500 . ? C25 C26 1.396(6) . ? C25 H25 0.9500 . ? C26 H26 0.9500 . ? C21' C22' 1.374(13) . ? C21' C26' 1.390(12) . ? C22' C23' 1.403(10) . ? C22' H22' 0.9500 . ? C23' C24' 1.381(11) . ? C23' H23' 0.9500 . ? C24' C25' 1.375(11) . ? C24' H24' 0.9500 . ? C25' C26' 1.385(12) . ? C25' H25' 0.9500 . ? C26' H26' 0.9500 . ? B1 C39 1.652(2) . ? B1 C27 1.655(2) . ? B1 C45 1.655(2) . ? B1 C33 1.656(2) . ? C27 C32 1.388(2) . ? C27 C28 1.392(2) . ? C28 F1 1.3537(16) . ? C28 C29 1.380(2) . ? C29 F2 1.3447(17) . ? C29 C30 1.380(2) . ? C30 F3 1.3462(17) . ? C30 C31 1.374(2) . ? C31 F4 1.3450(17) . ? C31 C32 1.388(2) . ? C32 F5 1.3515(16) . ? C33 C38 1.3906(19) . ? C33 C34 1.395(2) . ? C34 F6 1.3494(16) . ? C34 C35 1.380(2) . ? C35 F7 1.3456(17) . ? C35 C36 1.376(2) . ? C36 F8 1.3472(16) . ? C36 C37 1.374(2) . ? C37 F9 1.3514(16) . ? C37 C38 1.387(2) . ? C38 F10 1.3543(16) . ? C39 C44 1.392(2) . ? C39 C40 1.3954(19) . ? C40 F11 1.3540(16) . ? C40 C41 1.380(2) . ? C41 F12 1.3441(17) . ? C41 C42 1.379(2) . ? C42 F13 1.3450(17) . ? C42 C43 1.375(2) . ? C43 F14 1.3466(17) . ? C43 C44 1.388(2) . ? C44 F15 1.3499(16) . ? C45 C50 1.3917(19) . ? C45 C46 1.394(2) . ? C46 F16 1.3582(16) . ? C46 C47 1.382(2) . ? C47 F17 1.3455(17) . ? C47 C48 1.382(2) . ? C48 F18 1.3389(17) . ? C48 C49 1.375(2) . ? C49 F19 1.3476(17) . ? C49 C50 1.384(2) . ? C50 F20 1.3538(17) . ? C1S C2S 1.535(5) . ? C1S H1S1 0.9800 . ? C1S H1S2 0.9800 . ? C1S H1S3 0.9800 . ? C2S C3S 1.494(5) . ? C2S H2S1 0.9900 . ? C2S H2S2 0.9900 . ? C3S C4S 1.520(5) . ? C3S H3S1 0.9900 . ? C3S H3S2 0.9900 . ? C4S C5S 1.499(7) . ? C4S H4S1 0.9900 . ? C4S H4S2 0.9900 . ? C5S H5S1 0.9800 . ? C5S H5S2 0.9800 . ? C5S H5S3 0.9800 . ? C1' C2' 1.518(13) . ? C1' H1'1 0.9800 . ? C1' H1'2 0.9800 . ? C1' H1'3 0.9800 . ? C2' C3' 1.551(10) . ? C2' H2'1 0.9900 . ? C2' H2'2 0.9900 . ? C3' C4' 1.591(12) . ? C3' H3'1 0.9900 . ? C3' H3'2 0.9900 . ? C4' C5' 1.491(13) . ? C4' H4'1 0.9900 . ? C4' H4'2 0.9900 . ? C5' H5'1 0.9800 . ? C5' H5'2 0.9800 . ? C5' H5'3 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N3 113.25(5) . . ? N1 Cu1 S1 126.07(4) . 2_766 ? N3 Cu1 S1 118.75(4) . 2_766 ? N1 Cu1 N2 80.57(5) . . ? N3 Cu1 N2 80.07(5) . . ? S1 Cu1 N2 120.70(3) 2_766 . ? N1 C1 C2 123.72(14) . . ? N1 C1 H1 118.1 . . ? C2 C1 H1 118.1 . . ? C1 C2 C3 116.84(14) . . ? C1 C2 C13 121.46(14) . . ? C3 C2 C13 121.66(14) . . ? O1 C3 C2 116.96(14) . . ? O1 C3 C4 121.82(14) . . ? C2 C3 C4 121.08(14) . . ? C5 C4 C3 116.89(13) . . ? C5 C4 C15 121.46(14) . . ? C3 C4 C15 121.48(13) . . ? N1 C5 C4 122.93(13) . . ? N1 C5 C6 115.23(12) . . ? C4 C5 C6 121.65(13) . . ? N2 C6 C5 111.32(11) . . ? N2 C6 H6A 109.4 . . ? C5 C6 H6A 109.4 . . ? N2 C6 H6B 109.4 . . ? C5 C6 H6B 109.4 . . ? H6A C6 H6B 108.0 . . ? N2 C7 C8 111.64(11) . . ? N2 C7 H7A 109.3 . . ? C8 C7 H7A 109.3 . . ? N2 C7 H7B 109.3 . . ? C8 C7 H7B 109.3 . . ? H7A C7 H7B 108.0 . . ? N3 C8 C9 122.66(13) . . ? N3 C8 C7 115.32(12) . . ? C9 C8 C7 122.00(13) . . ? C8 C9 C10 116.94(13) . . ? C8 C9 C16 122.40(13) . . ? C10 C9 C16 120.66(13) . . ? O2 C10 C11 118.50(13) . . ? O2 C10 C9 119.96(13) . . ? C11 C10 C9 121.42(14) . . ? C12 C11 C10 116.68(13) . . ? C12 C11 C18 121.37(14) . . ? C10 C11 C18 121.93(15) . . ? N3 C12 C11 123.93(14) . . ? N3 C12 H12 118.0 . . ? C11 C12 H12 118.0 . . ? C2 C13 H13A 109.5 . . ? C2 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C2 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? O1 C14 H14A 109.5 . . ? O1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? O1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? O1 C14 H14D 109.5 . . ? H14A C14 H14D 141.1 . . ? H14B C14 H14D 56.3 . . ? H14C C14 H14D 56.3 . . ? O1 C14 H14E 109.5 . . ? H14A C14 H14E 56.3 . . ? H14B C14 H14E 141.1 . . ? H14C C14 H14E 56.3 . . ? H14D C14 H14E 109.5 . . ? O1 C14 H14F 109.5 . . ? H14A C14 H14F 56.3 . . ? H14B C14 H14F 56.3 . . ? H14C C14 H14F 141.1 . . ? H14D C14 H14F 109.5 . . ? H14E C14 H14F 109.5 . . ? C4 C15 H15A 109.5 . . ? C4 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C4 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C9 C16 H16A 109.5 . . ? C9 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C9 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? O2 C17 H17A 109.5 . . ? O2 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? O2 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C11 C18 H18A 109.5 . . ? C11 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C11 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? N2 C19 C20 113.83(11) . . ? N2 C19 H19A 108.8 . . ? C20 C19 H19A 108.8 . . ? N2 C19 H19B 108.8 . . ? C20 C19 H19B 108.8 . . ? H19A C19 H19B 107.7 . . ? C19 C20 S1 112.08(10) . . ? C19 C20 H20A 109.2 . . ? S1 C20 H20A 109.2 . . ? C19 C20 H20B 109.2 . . ? S1 C20 H20B 109.2 . . ? H20A C20 H20B 107.9 . . ? C21' S1 C20 101.2(12) . . ? C21 S1 C20 99.2(6) . . ? C21' S1 Cu1 114.4(10) . 2_766 ? C21 S1 Cu1 111.0(5) . 2_766 ? C20 S1 Cu1 110.98(5) . 2_766 ? C26 C21 C22 119.2(5) . . ? C26 C21 S1 119.1(5) . . ? C22 C21 S1 121.5(5) . . ? C23 C22 C21 119.6(4) . . ? C23 C22 H22 120.2 . . ? C21 C22 H22 120.2 . . ? C24 C23 C22 120.7(4) . . ? C24 C23 H23 119.6 . . ? C22 C23 H23 119.6 . . ? C25 C24 C23 120.2(4) . . ? C25 C24 H24 119.9 . . ? C23 C24 H24 119.9 . . ? C24 C25 C26 119.8(5) . . ? C24 C25 H25 120.1 . . ? C26 C25 H25 120.1 . . ? C21 C26 C25 120.4(5) . . ? C21 C26 H26 119.8 . . ? C25 C26 H26 119.8 . . ? C22' C21' C26' 122.2(10) . . ? C22' C21' S1 120.1(11) . . ? C26' C21' S1 116.9(11) . . ? C21' C22' C23' 119.0(9) . . ? C21' C22' H22' 120.5 . . ? C23' C22' H22' 120.5 . . ? C24' C23' C22' 119.0(9) . . ? C24' C23' H23' 120.5 . . ? C22' C23' H23' 120.5 . . ? C25' C24' C23' 120.7(9) . . ? C25' C24' H24' 119.7 . . ? C23' C24' H24' 119.7 . . ? C24' C25' C26' 121.3(11) . . ? C24' C25' H25' 119.3 . . ? C26' C25' H25' 119.3 . . ? C25' C26' C21' 117.3(11) . . ? C25' C26' H26' 121.3 . . ? C21' C26' H26' 121.3 . . ? C1 N1 C5 118.45(13) . . ? C1 N1 Cu1 126.36(10) . . ? C5 N1 Cu1 115.19(10) . . ? C7 N2 C19 110.69(11) . . ? C7 N2 C6 110.14(11) . . ? C19 N2 C6 109.38(11) . . ? C7 N2 Cu1 102.37(8) . . ? C19 N2 Cu1 122.64(9) . . ? C6 N2 Cu1 100.86(8) . . ? C12 N3 C8 118.34(13) . . ? C12 N3 Cu1 126.01(10) . . ? C8 N3 Cu1 115.51(10) . . ? C3 O1 C14 116.23(13) . . ? C10 O2 C17 113.99(11) . . ? C39 B1 C27 103.00(11) . . ? C39 B1 C45 112.76(11) . . ? C27 B1 C45 113.18(11) . . ? C39 B1 C33 113.43(11) . . ? C27 B1 C33 112.41(11) . . ? C45 B1 C33 102.46(11) . . ? C32 C27 C28 113.29(13) . . ? C32 C27 B1 127.54(12) . . ? C28 C27 B1 118.99(12) . . ? F1 C28 C29 116.14(12) . . ? F1 C28 C27 119.18(12) . . ? C29 C28 C27 124.68(13) . . ? F2 C29 C28 120.84(13) . . ? F2 C29 C30 120.01(13) . . ? C28 C29 C30 119.16(13) . . ? F3 C30 C31 120.23(14) . . ? F3 C30 C29 120.71(14) . . ? C31 C30 C29 119.06(13) . . ? F4 C31 C30 119.52(13) . . ? F4 C31 C32 120.84(13) . . ? C30 C31 C32 119.65(14) . . ? F5 C32 C31 114.70(13) . . ? F5 C32 C27 121.20(13) . . ? C31 C32 C27 124.10(13) . . ? C38 C33 C34 113.36(12) . . ? C38 C33 B1 128.16(12) . . ? C34 C33 B1 118.35(12) . . ? F6 C34 C35 116.16(12) . . ? F6 C34 C33 119.13(12) . . ? C35 C34 C33 124.70(13) . . ? F7 C35 C36 119.57(13) . . ? F7 C35 C34 121.30(13) . . ? C36 C35 C34 119.12(13) . . ? F8 C36 C37 120.47(13) . . ? F8 C36 C35 120.38(14) . . ? C37 C36 C35 119.15(13) . . ? F9 C37 C36 119.77(13) . . ? F9 C37 C38 120.33(13) . . ? C36 C37 C38 119.89(13) . . ? F10 C38 C37 114.76(12) . . ? F10 C38 C33 121.54(12) . . ? C37 C38 C33 123.70(13) . . ? C44 C39 C40 113.15(13) . . ? C44 C39 B1 127.62(12) . . ? C40 C39 B1 119.10(12) . . ? F11 C40 C41 116.03(12) . . ? F11 C40 C39 119.19(12) . . ? C41 C40 C39 124.77(13) . . ? F12 C41 C42 119.63(13) . . ? F12 C41 C40 121.17(13) . . ? C42 C41 C40 119.19(14) . . ? F13 C42 C43 120.61(14) . . ? F13 C42 C41 120.34(14) . . ? C43 C42 C41 119.04(13) . . ? F14 C43 C42 119.61(13) . . ? F14 C43 C44 120.57(13) . . ? C42 C43 C44 119.81(13) . . ? F15 C44 C43 114.80(12) . . ? F15 C44 C39 121.26(12) . . ? C43 C44 C39 123.94(13) . . ? C50 C45 C46 112.88(13) . . ? C50 C45 B1 127.61(12) . . ? C46 C45 B1 119.35(12) . . ? F16 C46 C47 115.66(12) . . ? F16 C46 C45 119.02(12) . . ? C47 C46 C45 125.32(13) . . ? F17 C47 C46 121.02(13) . . ? F17 C47 C48 120.13(13) . . ? C46 C47 C48 118.84(14) . . ? F18 C48 C49 120.80(14) . . ? F18 C48 C47 120.59(14) . . ? C49 C48 C47 118.60(14) . . ? F19 C49 C48 119.32(14) . . ? F19 C49 C50 120.20(14) . . ? C48 C49 C50 120.47(14) . . ? F20 C50 C49 114.91(13) . . ? F20 C50 C45 121.29(13) . . ? C49 C50 C45 123.79(14) . . ? C3S C2S C1S 111.3(3) . . ? C3S C2S H2S1 109.4 . . ? C1S C2S H2S1 109.4 . . ? C3S C2S H2S2 109.4 . . ? C1S C2S H2S2 109.4 . . ? H2S1 C2S H2S2 108.0 . . ? C2S C3S C4S 113.2(4) . . ? C2S C3S H3S1 108.9 . . ? C4S C3S H3S1 108.9 . . ? C2S C3S H3S2 108.9 . . ? C4S C3S H3S2 108.9 . . ? H3S1 C3S H3S2 107.8 . . ? C5S C4S C3S 113.1(4) . . ? C5S C4S H4S1 108.9 . . ? C3S C4S H4S1 108.9 . . ? C5S C4S H4S2 108.9 . . ? C3S C4S H4S2 108.9 . . ? H4S1 C4S H4S2 107.8 . . ? C2' C1' H1'1 109.5 . . ? C2' C1' H1'2 109.5 . . ? H1'1 C1' H1'2 109.5 . . ? C2' C1' H1'3 109.5 . . ? H1'1 C1' H1'3 109.5 . . ? H1'2 C1' H1'3 109.5 . . ? C1' C2' C3' 106.5(8) . . ? C1' C2' H2'1 110.4 . . ? C3' C2' H2'1 110.4 . . ? C1' C2' H2'2 110.4 . . ? C3' C2' H2'2 110.4 . . ? H2'1 C2' H2'2 108.6 . . ? C2' C3' C4' 105.0(8) . . ? C2' C3' H3'1 110.7 . . ? C4' C3' H3'1 110.7 . . ? C2' C3' H3'2 110.7 . . ? C4' C3' H3'2 110.7 . . ? H3'1 C3' H3'2 108.8 . . ? C5' C4' C3' 113.4(10) . . ? C5' C4' H4'1 108.9 . . ? C3' C4' H4'1 108.9 . . ? C5' C4' H4'2 108.9 . . ? C3' C4' H4'2 108.9 . . ? H4'1 C4' H4'2 107.7 . . ? C4' C5' H5'1 109.5 . . ? C4' C5' H5'2 109.5 . . ? H5'1 C5' H5'2 109.5 . . ? C4' C5' H5'3 109.5 . . ? H5'1 C5' H5'3 109.5 . . ? H5'2 C5' H5'3 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 C1 C2 C3 0.7(2) . . . . ? N1 C1 C2 C13 -177.09(14) . . . . ? C1 C2 C3 O1 -178.84(14) . . . . ? C13 C2 C3 O1 -1.0(2) . . . . ? C1 C2 C3 C4 -3.0(2) . . . . ? C13 C2 C3 C4 174.75(14) . . . . ? O1 C3 C4 C5 179.36(14) . . . . ? C2 C3 C4 C5 3.8(2) . . . . ? O1 C3 C4 C15 3.9(2) . . . . ? C2 C3 C4 C15 -171.71(15) . . . . ? C3 C4 C5 N1 -2.2(2) . . . . ? C15 C4 C5 N1 173.23(14) . . . . ? C3 C4 C5 C6 -176.93(14) . . . . ? C15 C4 C5 C6 -1.5(2) . . . . ? N1 C5 C6 N2 35.12(17) . . . . ? C4 C5 C6 N2 -149.81(13) . . . . ? N2 C7 C8 N3 34.55(17) . . . . ? N2 C7 C8 C9 -146.85(13) . . . . ? N3 C8 C9 C10 0.9(2) . . . . ? C7 C8 C9 C10 -177.60(13) . . . . ? N3 C8 C9 C16 -179.03(14) . . . . ? C7 C8 C9 C16 2.5(2) . . . . ? C8 C9 C10 O2 -176.17(12) . . . . ? C16 C9 C10 O2 3.8(2) . . . . ? C8 C9 C10 C11 -0.1(2) . . . . ? C16 C9 C10 C11 179.87(14) . . . . ? O2 C10 C11 C12 175.60(13) . . . . ? C9 C10 C11 C12 -0.6(2) . . . . ? O2 C10 C11 C18 -3.3(2) . . . . ? C9 C10 C11 C18 -179.47(15) . . . . ? C10 C11 C12 N3 0.4(2) . . . . ? C18 C11 C12 N3 179.34(16) . . . . ? N2 C19 C20 S1 83.37(13) . . . . ? C19 C20 S1 C21' 64.7(7) . . . . ? C19 C20 S1 C21 69.8(3) . . . . ? C19 C20 S1 Cu1 -173.48(8) . . . 2_766 ? C21' S1 C21 C26 1(18) . . . . ? C20 S1 C21 C26 -111.7(12) . . . . ? Cu1 S1 C21 C26 131.5(11) 2_766 . . . ? C21' S1 C21 C22 176(20) . . . . ? C20 S1 C21 C22 63.5(12) . . . . ? Cu1 S1 C21 C22 -53.3(13) 2_766 . . . ? C26 C21 C22 C23 -1.5(16) . . . . ? S1 C21 C22 C23 -176.7(9) . . . . ? C21 C22 C23 C24 0.5(9) . . . . ? C22 C23 C24 C25 0.2(8) . . . . ? C23 C24 C25 C26 0.0(11) . . . . ? C22 C21 C26 C25 1.7(19) . . . . ? S1 C21 C26 C25 177.0(10) . . . . ? C24 C25 C26 C21 -1.0(16) . . . . ? C21 S1 C21' C22' 14(17) . . . . ? C20 S1 C21' C22' 82(3) . . . . ? Cu1 S1 C21' C22' -37(3) 2_766 . . . ? C21 S1 C21' C26' -176(21) . . . . ? C20 S1 C21' C26' -107(2) . . . . ? Cu1 S1 C21' C26' 133(2) 2_766 . . . ? C26' C21' C22' C23' 8(4) . . . . ? S1 C21' C22' C23' 177.6(16) . . . . ? C21' C22' C23' C24' -4(2) . . . . ? C22' C23' C24' C25' -0.8(17) . . . . ? C23' C24' C25' C26' 2(2) . . . . ? C24' C25' C26' C21' 2(3) . . . . ? C22' C21' C26' C25' -6(4) . . . . ? S1 C21' C26' C25' -177(2) . . . . ? C2 C1 N1 C5 0.8(2) . . . . ? C2 C1 N1 Cu1 -179.48(11) . . . . ? C4 C5 N1 C1 0.0(2) . . . . ? C6 C5 N1 C1 175.01(13) . . . . ? C4 C5 N1 Cu1 -179.74(11) . . . . ? C6 C5 N1 Cu1 -4.74(16) . . . . ? N3 Cu1 N1 C1 -120.79(12) . . . . ? S1 Cu1 N1 C1 43.09(14) 2_766 . . . ? N2 Cu1 N1 C1 164.37(13) . . . . ? N3 Cu1 N1 C5 58.94(12) . . . . ? S1 Cu1 N1 C5 -137.18(9) 2_766 . . . ? N2 Cu1 N1 C5 -15.89(10) . . . . ? C8 C7 N2 C19 -173.03(11) . . . . ? C8 C7 N2 C6 65.89(14) . . . . ? C8 C7 N2 Cu1 -40.73(12) . . . . ? C20 C19 N2 C7 90.21(14) . . . . ? C20 C19 N2 C6 -148.26(12) . . . . ? C20 C19 N2 Cu1 -30.70(15) . . . . ? C5 C6 N2 C7 -150.13(12) . . . . ? C5 C6 N2 C19 88.01(14) . . . . ? C5 C6 N2 Cu1 -42.51(12) . . . . ? N1 Cu1 N2 C7 145.13(9) . . . . ? N3 Cu1 N2 C7 29.32(9) . . . . ? S1 Cu1 N2 C7 -88.32(8) 2_766 . . . ? N1 Cu1 N2 C19 -90.13(11) . . . . ? N3 Cu1 N2 C19 154.07(11) . . . . ? S1 Cu1 N2 C19 36.43(11) 2_766 . . . ? N1 Cu1 N2 C6 31.49(8) . . . . ? N3 Cu1 N2 C6 -84.32(9) . . . . ? S1 Cu1 N2 C6 158.04(7) 2_766 . . . ? C11 C12 N3 C8 0.4(2) . . . . ? C11 C12 N3 Cu1 -175.24(12) . . . . ? C9 C8 N3 C12 -1.0(2) . . . . ? C7 C8 N3 C12 177.54(13) . . . . ? C9 C8 N3 Cu1 175.01(11) . . . . ? C7 C8 N3 Cu1 -6.40(16) . . . . ? N1 Cu1 N3 C12 87.05(13) . . . . ? S1 Cu1 N3 C12 -78.12(13) 2_766 . . . ? N2 Cu1 N3 C12 162.20(13) . . . . ? N1 Cu1 N3 C8 -88.65(11) . . . . ? S1 Cu1 N3 C8 106.18(10) 2_766 . . . ? N2 Cu1 N3 C8 -13.50(10) . . . . ? C2 C3 O1 C14 -120.30(16) . . . . ? C4 C3 O1 C14 63.9(2) . . . . ? C11 C10 O2 C17 97.35(16) . . . . ? C9 C10 O2 C17 -86.43(17) . . . . ? C39 B1 C27 C32 109.16(15) . . . . ? C45 B1 C27 C32 -128.78(15) . . . . ? C33 B1 C27 C32 -13.3(2) . . . . ? C39 B1 C27 C28 -65.64(15) . . . . ? C45 B1 C27 C28 56.41(17) . . . . ? C33 B1 C27 C28 171.91(12) . . . . ? C32 C27 C28 F1 -177.84(12) . . . . ? B1 C27 C28 F1 -2.32(19) . . . . ? C32 C27 C28 C29 3.2(2) . . . . ? B1 C27 C28 C29 178.71(13) . . . . ? F1 C28 C29 F2 -1.4(2) . . . . ? C27 C28 C29 F2 177.57(13) . . . . ? F1 C28 C29 C30 178.38(13) . . . . ? C27 C28 C29 C30 -2.6(2) . . . . ? F2 C29 C30 F3 0.0(2) . . . . ? C28 C29 C30 F3 -179.84(13) . . . . ? F2 C29 C30 C31 -179.64(13) . . . . ? C28 C29 C30 C31 0.5(2) . . . . ? F3 C30 C31 F4 0.9(2) . . . . ? C29 C30 C31 F4 -179.44(13) . . . . ? F3 C30 C31 C32 -179.03(13) . . . . ? C29 C30 C31 C32 0.6(2) . . . . ? F4 C31 C32 F5 0.7(2) . . . . ? C30 C31 C32 F5 -179.37(13) . . . . ? F4 C31 C32 C27 -179.78(13) . . . . ? C30 C31 C32 C27 0.2(2) . . . . ? C28 C27 C32 F5 177.58(12) . . . . ? B1 C27 C32 F5 2.5(2) . . . . ? C28 C27 C32 C31 -2.0(2) . . . . ? B1 C27 C32 C31 -177.01(14) . . . . ? C39 B1 C33 C38 8.8(2) . . . . ? C27 B1 C33 C38 125.15(14) . . . . ? C45 B1 C33 C38 -113.04(15) . . . . ? C39 B1 C33 C34 -175.64(12) . . . . ? C27 B1 C33 C34 -59.29(16) . . . . ? C45 B1 C33 C34 62.52(15) . . . . ? C38 C33 C34 F6 179.35(12) . . . . ? B1 C33 C34 F6 3.15(19) . . . . ? C38 C33 C34 C35 -1.5(2) . . . . ? B1 C33 C34 C35 -177.70(13) . . . . ? F6 C34 C35 F7 -0.6(2) . . . . ? C33 C34 C35 F7 -179.81(13) . . . . ? F6 C34 C35 C36 178.18(12) . . . . ? C33 C34 C35 C36 -1.0(2) . . . . ? F7 C35 C36 F8 0.6(2) . . . . ? C34 C35 C36 F8 -178.22(13) . . . . ? F7 C35 C36 C37 -178.79(13) . . . . ? C34 C35 C36 C37 2.4(2) . . . . ? F8 C36 C37 F9 0.0(2) . . . . ? C35 C36 C37 F9 179.39(13) . . . . ? F8 C36 C37 C38 179.39(12) . . . . ? C35 C36 C37 C38 -1.2(2) . . . . ? F9 C37 C38 F10 -1.84(19) . . . . ? C36 C37 C38 F10 178.77(12) . . . . ? F9 C37 C38 C33 177.88(12) . . . . ? C36 C37 C38 C33 -1.5(2) . . . . ? C34 C33 C38 F10 -177.55(12) . . . . ? B1 C33 C38 F10 -1.8(2) . . . . ? C34 C33 C38 C37 2.7(2) . . . . ? B1 C33 C38 C37 178.49(13) . . . . ? C27 B1 C39 C44 112.27(15) . . . . ? C45 B1 C39 C44 -10.06(19) . . . . ? C33 B1 C39 C44 -125.96(14) . . . . ? C27 B1 C39 C40 -63.33(15) . . . . ? C45 B1 C39 C40 174.34(12) . . . . ? C33 B1 C39 C40 58.44(16) . . . . ? C44 C39 C40 F11 -178.06(12) . . . . ? B1 C39 C40 F11 -1.84(19) . . . . ? C44 C39 C40 C41 3.1(2) . . . . ? B1 C39 C40 C41 179.29(13) . . . . ? F11 C40 C41 F12 -0.1(2) . . . . ? C39 C40 C41 F12 178.79(13) . . . . ? F11 C40 C41 C42 -179.79(13) . . . . ? C39 C40 C41 C42 -0.9(2) . . . . ? F12 C41 C42 F13 -0.2(2) . . . . ? C40 C41 C42 F13 179.54(13) . . . . ? F12 C41 C42 C43 179.04(13) . . . . ? C40 C41 C42 C43 -1.3(2) . . . . ? F13 C42 C43 F14 -0.6(2) . . . . ? C41 C42 C43 F14 -179.80(13) . . . . ? F13 C42 C43 C44 -179.83(13) . . . . ? C41 C42 C43 C44 1.0(2) . . . . ? F14 C43 C44 F15 1.88(19) . . . . ? C42 C43 C44 F15 -178.90(13) . . . . ? F14 C43 C44 C39 -177.70(13) . . . . ? C42 C43 C44 C39 1.5(2) . . . . ? C40 C39 C44 F15 177.08(12) . . . . ? B1 C39 C44 F15 1.3(2) . . . . ? C40 C39 C44 C43 -3.4(2) . . . . ? B1 C39 C44 C43 -179.19(13) . . . . ? C39 B1 C45 C50 127.45(14) . . . . ? C27 B1 C45 C50 11.0(2) . . . . ? C33 B1 C45 C50 -110.26(15) . . . . ? C39 B1 C45 C46 -57.60(16) . . . . ? C27 B1 C45 C46 -174.02(12) . . . . ? C33 B1 C45 C46 64.70(15) . . . . ? C50 C45 C46 F16 177.70(12) . . . . ? B1 C45 C46 F16 2.04(19) . . . . ? C50 C45 C46 C47 -3.3(2) . . . . ? B1 C45 C46 C47 -178.92(13) . . . . ? F16 C46 C47 F17 -0.8(2) . . . . ? C45 C46 C47 F17 -179.84(13) . . . . ? F16 C46 C47 C48 179.93(13) . . . . ? C45 C46 C47 C48 0.9(2) . . . . ? F17 C47 C48 F18 1.0(2) . . . . ? C46 C47 C48 F18 -179.71(13) . . . . ? F17 C47 C48 C49 -177.76(13) . . . . ? C46 C47 C48 C49 1.6(2) . . . . ? F18 C48 C49 F19 -1.4(2) . . . . ? C47 C48 C49 F19 177.33(13) . . . . ? F18 C48 C49 C50 179.98(13) . . . . ? C47 C48 C49 C50 -1.3(2) . . . . ? F19 C49 C50 F20 -0.8(2) . . . . ? C48 C49 C50 F20 177.79(13) . . . . ? F19 C49 C50 C45 179.96(13) . . . . ? C48 C49 C50 C45 -1.4(2) . . . . ? C46 C45 C50 F20 -175.66(12) . . . . ? B1 C45 C50 F20 -0.4(2) . . . . ? C46 C45 C50 C49 3.5(2) . . . . ? B1 C45 C50 C49 178.73(14) . . . . ? C1S C2S C3S C4S 177.1(4) . . . . ? C2S C3S C4S C5S -179.2(4) . . . . ? C1' C2' C3' C4' 177.8(10) . . . . ? C2' C3' C4' C5' -170.5(12) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 71.90 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.502 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.049 _iucr_refine_instructions_details ; TITL xs0033a in P-1 CELL 1.54178 14.5520 14.6344 15.0327 67.739 88.928 65.891 ZERR 1 0.0005 0.0005 0.0006 0.003 0.003 0.003 LATT 1 SFAC C H B N O F S CU UNIT 110 90 2 6 4 40 2 2 TEMP -173 ACTA HTAB BOND BOND $H CONF WPDB L.S. 6 FMAP 2 PLAN 10 OMIT -2 143.8 WGHT 0.039700 1.438500 FVAR 4.18695 0.66481 0.66842 PART 0 rem Cu complex CU1 8 1.037838 0.607888 0.569939 11.00000 0.01455 0.01352 = 0.01347 -0.00162 0.00214 -0.00493 C1 1 0.815329 0.752599 0.558026 11.00000 0.01958 0.01821 = 0.01884 -0.00673 0.00458 -0.00837 AFIX 43 H1 2 0.816154 0.691272 0.611909 11.00000 -1.20000 AFIX 0 C2 1 0.724397 0.847198 0.521274 11.00000 0.01775 0.02216 = 0.02156 -0.01166 0.00500 -0.00778 C3 1 0.725241 0.935635 0.441305 11.00000 0.01813 0.01720 = 0.02041 -0.00816 0.00173 -0.00225 C4 1 0.815337 0.929893 0.403688 11.00000 0.02069 0.01593 = 0.01708 -0.00590 0.00239 -0.00504 C5 1 0.902038 0.829937 0.446000 11.00000 0.01846 0.01624 = 0.01557 -0.00587 0.00308 -0.00626 C6 1 1.004904 0.815580 0.414859 11.00000 0.01706 0.01387 = 0.01818 -0.00268 0.00260 -0.00535 AFIX 23 H6A 2 0.994735 0.866189 0.345876 11.00000 -1.20000 H6B 2 1.041471 0.834656 0.454717 11.00000 -1.20000 AFIX 0 C7 1 1.176950 0.672359 0.446914 11.00000 0.01561 0.02068 = 0.01255 -0.00482 0.00281 -0.00761 AFIX 23 H7A 2 1.193768 0.726640 0.395129 11.00000 -1.20000 H7B 2 1.218092 0.599554 0.446280 11.00000 -1.20000 AFIX 0 C8 1 1.204438 0.669851 0.544599 11.00000 0.01557 0.01526 = 0.01376 -0.00447 0.00256 -0.00490 C9 1 1.280056 0.699879 0.561284 11.00000 0.01716 0.01757 = 0.01597 -0.00598 0.00311 -0.00643 C10 1 1.301694 0.690273 0.655641 11.00000 0.01689 0.01520 = 0.01980 -0.00830 0.00183 -0.00474 C11 1 1.250282 0.652751 0.729096 11.00000 0.02358 0.02430 = 0.01583 -0.00912 0.00331 -0.00906 C12 1 1.176189 0.626378 0.704093 11.00000 0.02258 0.02527 = 0.01471 -0.00760 0.00603 -0.01102 AFIX 43 H12 2 1.139752 0.601013 0.753203 11.00000 -1.20000 AFIX 0 C13 1 0.630578 0.855407 0.567666 11.00000 0.02028 0.02716 = 0.02918 -0.01395 0.01017 -0.00826 AFIX 137 H13A 2 0.642361 0.783082 0.616898 11.00000 -1.50000 H13B 2 0.572791 0.881545 0.517722 11.00000 -1.50000 H13C 2 0.615402 0.906947 0.598630 11.00000 -1.50000 AFIX 0 C14 1 0.593822 1.067275 0.306766 11.00000 0.02102 0.02656 = 0.03343 -0.00803 -0.00396 -0.00416 AFIX 123 H14A 2 0.530560 1.134711 0.289129 10.50000 -1.50000 H14B 2 0.579143 1.010970 0.298651 10.50000 -1.50000 H14C 2 0.642700 1.081949 0.264489 10.50000 -1.50000 H14D 2 0.637708 1.017042 0.279051 10.50000 -1.50000 H14E 2 0.589126 1.140784 0.269528 10.50000 -1.50000 H14F 2 0.525568 1.069804 0.303690 10.50000 -1.50000 AFIX 0 C15 1 0.820421 1.029327 0.326436 11.00000 0.02381 0.01584 = 0.02506 -0.00341 0.00470 -0.00466 AFIX 137 H15A 2 0.820031 1.024065 0.263378 11.00000 -1.50000 H15B 2 0.883231 1.032951 0.343232 11.00000 -1.50000 H15C 2 0.761301 1.095555 0.322515 11.00000 -1.50000 AFIX 0 C16 1 1.336577 0.741035 0.482367 11.00000 0.02935 0.03851 = 0.02147 -0.01097 0.00784 -0.02340 AFIX 137 H16A 2 1.372536 0.775061 0.503421 11.00000 -1.50000 H16B 2 1.287933 0.795273 0.422731 11.00000 -1.50000 H16C 2 1.385999 0.679520 0.469658 11.00000 -1.50000 AFIX 0 C17 1 1.474778 0.642825 0.700291 11.00000 0.01839 0.02772 = 0.04034 -0.01650 0.00051 -0.00820 AFIX 137 H17A 2 1.483853 0.582789 0.763002 11.00000 -1.50000 H17B 2 1.520276 0.675625 0.704937 11.00000 -1.50000 H17C 2 1.491135 0.614324 0.649739 11.00000 -1.50000 AFIX 0 C18 1 1.272205 0.642966 0.830593 11.00000 0.04358 0.05725 = 0.01980 -0.01992 0.00980 -0.03108 AFIX 137 H18A 2 1.225540 0.619206 0.870416 11.00000 -1.50000 H18B 2 1.262592 0.714282 0.827997 11.00000 -1.50000 H18C 2 1.342757 0.589040 0.859448 11.00000 -1.50000 AFIX 0 C19 1 1.045119 0.689816 0.336484 11.00000 0.01641 0.01854 = 0.01086 -0.00195 0.00083 -0.00782 AFIX 23 H19A 2 1.092299 0.706315 0.291569 11.00000 -1.20000 H19B 2 0.974844 0.744761 0.304022 11.00000 -1.20000 AFIX 0 C20 1 1.054664 0.576509 0.354158 11.00000 0.01444 0.01871 = 0.01511 -0.00547 0.00412 -0.00667 AFIX 23 H20A 2 1.113189 0.520410 0.406311 11.00000 -1.20000 H20B 2 1.068583 0.563816 0.294101 11.00000 -1.20000 AFIX 0 S1 7 0.939452 0.561101 0.389137 11.00000 0.01392 0.01399 = 0.01287 -0.00196 0.00055 -0.00475 FLAT C21 > C26 EADP C21 C21' SADI 0.02 S1 C21 S1 C21' SIMU 0.01 C21 > C26' PART 1 C21 1 0.855266 0.650689 0.275448 21.00000 0.02083 0.01453 = 0.01926 -0.00129 -0.00477 -0.00815 C22 1 0.873051 0.629186 0.192103 21.00000 0.03662 0.02401 = 0.01869 -0.00705 -0.00568 -0.00741 AFIX 43 H22 2 0.928738 0.563979 0.195532 21.00000 -1.20000 AFIX 0 C23 1 0.808934 0.703589 0.104480 21.00000 0.04960 0.03481 = 0.02455 -0.00810 -0.01044 -0.01402 AFIX 43 H23 2 0.820615 0.688745 0.047951 21.00000 -1.20000 AFIX 0 C24 1 0.728161 0.799178 0.098437 21.00000 0.03706 0.02845 = 0.02538 0.00471 -0.01648 -0.01608 AFIX 43 H24 2 0.684640 0.849421 0.037981 21.00000 -1.20000 AFIX 0 C25 1 0.710667 0.821696 0.179529 21.00000 0.02326 0.02024 = 0.02913 0.00201 -0.00837 -0.00596 AFIX 43 H25 2 0.655106 0.887405 0.175256 21.00000 -1.20000 AFIX 0 C26 1 0.774722 0.747804 0.268312 21.00000 0.01861 0.02118 = 0.02311 -0.00475 0.00043 -0.00968 AFIX 43 H26 2 0.763211 0.763970 0.324188 21.00000 -1.20000 AFIX 0 PART 2 SAME C21 > C26 C21' 1 0.849721 0.657969 0.281940 -21.00000 0.02083 0.01453 = 0.01926 -0.00129 -0.00477 -0.00815 C22' 1 0.844214 0.630662 0.204885 -21.00000 0.03583 0.01824 = 0.02815 -0.00389 -0.00360 -0.00463 AFIX 43 H22' 2 0.889972 0.560928 0.207433 -21.00000 -1.20000 AFIX 0 C23' 1 0.770030 0.707271 0.122405 -21.00000 0.04628 0.03251 = 0.02574 -0.00631 -0.01705 -0.01382 AFIX 43 H23' 2 0.767442 0.691964 0.066719 -21.00000 -1.20000 AFIX 0 C24' 1 0.700809 0.805292 0.123384 -21.00000 0.03511 0.01967 = 0.03138 0.00157 -0.01216 -0.00890 AFIX 43 H24' 2 0.650799 0.858121 0.067603 -21.00000 -1.20000 AFIX 0 C25' 1 0.703554 0.827187 0.204310 -21.00000 0.02001 0.01861 = 0.02711 -0.00453 -0.00486 -0.00810 AFIX 43 H25' 2 0.653965 0.894163 0.204207 -21.00000 -1.20000 AFIX 0 C26' 1 0.777158 0.753566 0.285969 -21.00000 0.01498 0.01613 = 0.01866 -0.00431 -0.00453 -0.00490 AFIX 43 H26' 2 0.777988 0.767870 0.342469 -21.00000 -1.20000 AFIX 0 PART 0 N1 4 0.902361 0.742778 0.521716 11.00000 0.01739 0.01560 = 0.01680 -0.00482 0.00334 -0.00570 N2 4 1.067770 0.701138 0.426264 11.00000 0.01389 0.01556 = 0.01306 -0.00405 0.00174 -0.00516 N3 4 1.152711 0.634522 0.614417 11.00000 0.01647 0.01686 = 0.01351 -0.00416 0.00315 -0.00589 O1 5 0.636238 1.029614 0.406050 11.00000 0.02204 0.02352 = 0.02659 -0.00559 0.00423 0.00415 O2 5 1.370877 0.724470 0.675675 11.00000 0.01897 0.02032 = 0.02589 -0.01205 0.00127 -0.00745 rem counterion B1 3 0.355745 0.773602 0.122004 11.00000 0.01563 0.01282 = 0.01165 -0.00459 0.00264 -0.00611 C27 1 0.433556 0.762940 0.040969 11.00000 0.01414 0.01695 = 0.01286 -0.00573 0.00168 -0.00650 C28 1 0.461963 0.847377 -0.005395 11.00000 0.01708 0.01568 = 0.01497 -0.00666 0.00164 -0.00685 C29 1 0.527697 0.847578 -0.072802 11.00000 0.01825 0.02086 = 0.01620 -0.00393 0.00271 -0.01193 C30 1 0.572763 0.756991 -0.094595 11.00000 0.01563 0.02852 = 0.01602 -0.00907 0.00679 -0.00978 C31 1 0.550267 0.669418 -0.049176 11.00000 0.01855 0.02103 = 0.02113 -0.01277 0.00542 -0.00658 C32 1 0.482297 0.673878 0.016804 11.00000 0.01837 0.01730 = 0.01768 -0.00706 0.00416 -0.00959 C33 1 0.317234 0.675064 0.158149 11.00000 0.01359 0.01350 = 0.01483 -0.00688 0.00455 -0.00476 C34 1 0.264614 0.665241 0.088260 11.00000 0.01666 0.01767 = 0.01292 -0.00660 0.00524 -0.00729 C35 1 0.225097 0.589729 0.108115 11.00000 0.01929 0.02450 = 0.02034 -0.01491 0.00761 -0.01214 C36 1 0.238615 0.516717 0.202798 11.00000 0.01941 0.01832 = 0.02671 -0.01276 0.01157 -0.01232 C37 1 0.287798 0.523510 0.275535 11.00000 0.01680 0.01558 = 0.01562 -0.00467 0.00688 -0.00579 C38 1 0.324728 0.602006 0.252675 11.00000 0.01301 0.01620 = 0.01538 -0.00756 0.00331 -0.00469 C39 1 0.424464 0.770380 0.210344 11.00000 0.01491 0.01442 = 0.01240 -0.00448 0.00396 -0.00756 C40 1 0.514018 0.676263 0.260467 11.00000 0.01730 0.01456 = 0.01654 -0.00672 0.00356 -0.00706 C41 1 0.578550 0.663624 0.334766 11.00000 0.01609 0.01813 = 0.01878 -0.00357 -0.00109 -0.00534 C42 1 0.555788 0.749187 0.362418 11.00000 0.02044 0.02730 = 0.01492 -0.00793 0.00047 -0.01295 C43 1 0.470377 0.845649 0.313869 11.00000 0.02224 0.02130 = 0.01798 -0.01134 0.00653 -0.01294 C44 1 0.407861 0.854931 0.239235 11.00000 0.01491 0.01430 = 0.01437 -0.00470 0.00312 -0.00595 C45 1 0.246755 0.885886 0.077771 11.00000 0.01603 0.01409 = 0.01330 -0.00456 0.00181 -0.00779 C46 1 0.177955 0.910710 0.140248 11.00000 0.01806 0.01462 = 0.01181 -0.00300 0.00001 -0.00770 C47 1 0.083962 1.000458 0.112806 11.00000 0.01612 0.01977 = 0.02167 -0.00953 0.00457 -0.00799 C48 1 0.052910 1.072269 0.015803 11.00000 0.01384 0.01528 = 0.02664 -0.00370 -0.00278 -0.00325 C49 1 0.115870 1.050044 -0.050051 11.00000 0.02143 0.02032 = 0.01509 0.00103 -0.00349 -0.01043 C50 1 0.209161 0.958821 -0.019177 11.00000 0.01933 0.01947 = 0.01339 -0.00529 0.00252 -0.01025 F1 6 0.422432 0.937557 0.014420 11.00000 0.02416 0.01626 = 0.02085 -0.00869 0.00654 -0.01078 F2 6 0.548252 0.934411 -0.116839 11.00000 0.02986 0.02700 = 0.02317 -0.00663 0.00988 -0.02002 F3 6 0.637424 0.754337 -0.159804 11.00000 0.02561 0.03893 = 0.02663 -0.01546 0.01674 -0.01597 F4 6 0.594437 0.580401 -0.069296 11.00000 0.02911 0.02721 = 0.03406 -0.02139 0.01601 -0.01090 F5 6 0.466519 0.582949 0.057868 11.00000 0.02686 0.01763 = 0.02843 -0.01273 0.01263 -0.01259 F6 6 0.251244 0.732394 -0.006326 11.00000 0.02541 0.02512 = 0.01243 -0.00719 0.00342 -0.01476 F7 6 0.175367 0.584991 0.036610 11.00000 0.03213 0.03852 = 0.02417 -0.01894 0.00896 -0.02503 F8 6 0.203228 0.440216 0.223952 11.00000 0.03516 0.02693 = 0.03266 -0.01634 0.01663 -0.02418 F9 6 0.300767 0.452957 0.368960 11.00000 0.02658 0.01925 = 0.01849 -0.00204 0.00734 -0.01128 F10 6 0.370025 0.602513 0.330261 11.00000 0.02114 0.02138 = 0.01280 -0.00489 0.00167 -0.01051 F11 6 0.540857 0.588856 0.237336 11.00000 0.02007 0.01396 = 0.02546 -0.00944 0.00054 -0.00360 F12 6 0.662624 0.569433 0.380707 11.00000 0.02113 0.02176 = 0.03040 -0.00513 -0.00921 -0.00100 F13 6 0.617079 0.738657 0.435079 11.00000 0.02925 0.03804 = 0.02421 -0.01361 -0.00681 -0.01413 F14 6 0.447487 0.929936 0.340000 11.00000 0.03140 0.02664 = 0.02953 -0.01941 0.00396 -0.01381 F15 6 0.327217 0.953731 0.195541 11.00000 0.01856 0.01352 = 0.02347 -0.00813 0.00011 -0.00405 F16 6 0.203538 0.843764 0.236638 11.00000 0.02008 0.01956 = 0.01092 -0.00364 0.00365 -0.00671 F17 6 0.022716 1.017750 0.178640 11.00000 0.01835 0.02739 = 0.02822 -0.01414 0.00863 -0.00636 F18 6 -0.037458 1.160409 -0.013534 11.00000 0.01665 0.02204 = 0.03798 -0.00379 -0.00347 0.00093 F19 6 0.084895 1.116823 -0.145406 11.00000 0.02727 0.02911 = 0.01713 0.00685 -0.00697 -0.00888 F20 6 0.262542 0.943714 -0.091162 11.00000 0.02301 0.02811 = 0.01156 -0.00468 0.00354 -0.01083 SIMU 0.01 C1S > C5' rem solvent molecule PART 1 C1S 1 0.094374 0.023872 0.403688 31.00000 0.05047 0.05791 = 0.05962 -0.03710 0.01380 -0.03018 AFIX 137 H1S1 2 0.058660 0.074340 0.434212 31.00000 -1.50000 H1S2 2 0.143762 -0.045893 0.453441 31.00000 -1.50000 H1S3 2 0.044856 0.011173 0.372574 31.00000 -1.50000 AFIX 0 C2S 1 0.150519 0.073990 0.326678 31.00000 0.04026 0.05761 = 0.06105 -0.04240 0.01406 -0.02437 AFIX 23 H2S1 2 0.208787 0.074154 0.359466 31.00000 -1.20000 H2S2 2 0.177870 0.028426 0.289191 31.00000 -1.20000 AFIX 0 C3S 1 0.081190 0.188524 0.258516 31.00000 0.04260 0.05649 = 0.06172 -0.03563 0.00883 -0.02942 AFIX 23 H3S1 2 0.050965 0.232562 0.296805 31.00000 -1.20000 H3S2 2 0.024793 0.187376 0.223800 31.00000 -1.20000 AFIX 0 C4S 1 0.134935 0.243506 0.184049 31.00000 0.05410 0.07433 = 0.07349 -0.03540 0.02181 -0.03793 AFIX 23 H4S1 2 0.191964 0.243683 0.218767 31.00000 -1.20000 H4S2 2 0.164290 0.200059 0.145112 31.00000 -1.20000 AFIX 0 C5S 1 0.065701 0.358945 0.116591 31.00000 0.07645 0.07383 = 0.09018 -0.04582 0.03121 -0.04424 AFIX 137 H5S1 2 0.011986 0.358954 0.078223 31.00000 -1.50000 H5S2 2 0.105154 0.391351 0.072745 31.00000 -1.50000 H5S3 2 0.034702 0.401999 0.154705 31.00000 -1.50000 AFIX 0 PART 2 SAME C1S > C5S C1' 1 0.132462 0.012515 0.386843 -31.00000 0.09482 0.08558 = 0.09343 -0.04817 -0.00642 -0.04211 AFIX 137 H1'1 2 0.151246 -0.032587 0.349199 -31.00000 -1.50000 H1'2 2 0.096397 -0.014903 0.438512 -31.00000 -1.50000 H1'3 2 0.194246 0.008877 0.415934 -31.00000 -1.50000 AFIX 0 C2' 1 0.063547 0.130449 0.320074 -31.00000 0.05514 0.06575 = 0.07036 -0.05009 0.01528 -0.03007 AFIX 23 H2'1 2 0.044833 0.177334 0.356866 -31.00000 -1.20000 H2'2 2 0.000284 0.135615 0.290791 -31.00000 -1.20000 AFIX 0 C3' 1 0.124932 0.167302 0.239740 -31.00000 0.05566 0.08007 = 0.07284 -0.04057 0.02478 -0.03913 AFIX 23 H3'1 2 0.145820 0.119104 0.204180 -31.00000 -1.20000 H3'2 2 0.186709 0.165457 0.268379 -31.00000 -1.20000 AFIX 0 C4' 1 0.048948 0.289201 0.168987 -31.00000 0.06165 0.09048 = 0.10199 -0.00575 0.01436 -0.03799 AFIX 23 H4'1 2 -0.017308 0.290897 0.152023 -31.00000 -1.20000 H4'2 2 0.036879 0.337361 0.203958 -31.00000 -1.20000 AFIX 0 C5' 1 0.087543 0.333529 0.077455 -31.00000 0.09247 0.13435 = 0.11732 -0.02620 0.01354 -0.03629 AFIX 137 H5'1 2 0.138770 0.355948 0.090951 -31.00000 -1.50000 H5'2 2 0.030747 0.396994 0.028893 -31.00000 -1.50000 H5'3 2 0.118486 0.276789 0.052345 -31.00000 -1.50000 HKLF 4 REM xs0033a in P-1 REM R1 = 0.0297 for 9658 Fo > 4sig(Fo) and 0.0324 for all 10473 data REM 852 parameters refined using 317 restraints END WGHT 0.0396 1.4338 REM Highest difference peak 0.502, deepest hole -0.421, 1-sigma level 0.049 Q1 1 0.0348 0.3124 0.2281 11.00000 0.05 0.50 Q2 1 0.0162 0.3177 0.1061 11.00000 0.05 0.36 Q3 1 0.8959 0.6082 0.3293 11.00000 0.05 0.31 Q4 1 0.2953 0.8373 0.0932 11.00000 0.05 0.30 Q5 1 0.3412 0.7124 0.1472 11.00000 0.05 0.29 Q6 1 0.0978 0.2328 0.1401 11.00000 0.05 0.29 Q7 1 0.3983 0.7645 0.0769 11.00000 0.05 0.28 Q8 1 0.5226 0.6705 -0.0103 11.00000 0.05 0.28 Q9 1 0.2283 0.9190 0.0304 11.00000 0.05 0.28 Q10 1 0.1523 0.1173 0.2625 11.00000 0.05 0.27 ;