# Supplementary Material (ESI) for Chemical Communications # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _publ_contact_author_name 'Kenneth Karlin' _publ_contact_author_email KARLIN@JHU.EDU _publ_section_title ; Thioether S-Ligation in a Side-on ?-?2:?2-Peroxo Dicopper(II) Complex ; loop_ _publ_author_name 'Kenneth Karlin' 'Yunho Lee.' 'Dong-Heon Lee.' 'Ga Young Park.' 'Amy A. Narducci Sarjeant' ; E.I.Solomon ; 'Julia S. Woertink' data_x0325 _database_code_depnum_ccdc_archive 'CCDC 738906' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C17 H30 Cl2 Cu N2 S' _chemical_formula_sum 'C17 H30 Cl2 Cu N2 S' _chemical_formula_weight 428.93 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.4850(6) _cell_length_b 9.3727(3) _cell_length_c 16.0378(6) _cell_angle_alpha 90.00 _cell_angle_beta 115.278(5) _cell_angle_gamma 90.00 _cell_volume 1968.86(15) _cell_formula_units_Z 4 _cell_measurement_temperature 110(2) _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.447 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 900 _exptl_special_details ; ? ; _diffrn_radiation_wavelength 0.71073 _diffrn_standards_number ? _diffrn_standards_interval_count 2 _diffrn_standards_interval_time 50 _diffrn_standards_decay_% ? _diffrn_reflns_number 12886 _diffrn_reflns_av_R_equivalents 0.0309 _diffrn_reflns_av_sigmaI/netI 0.0346 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.85 _diffrn_reflns_theta_max 27.88 _diffrn_reflns_resolution_max 0.76 _reflns_number_total 4653 _reflns_number_gt 3594 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Oxford Diffraction CrysAlis CCD' _computing_cell_refinement 'Oxford Diffraction CrysAlis RED' _computing_data_reduction 'Oxford Diffraction CrysAlis RED' _computing_structure_solution 'Sheldrick, G.M. (2000). SHELXTL v6.10.' _computing_structure_refinement 'Sheldrick, G.M. (2000). SHELXTL v6.10.' _computing_molecular_graphics 'Sheldrick, G.M. (2000). SHELXTL v6.10.' _computing_publication_material 'Sheldrick, G.M. (2000). SHELXTL v6.10.' _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^)+(0.0326P)^2^+1.6682P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4653 _refine_ls_number_parameters 212 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0519 _refine_ls_R_factor_gt 0.0323 _refine_ls_wR_factor_ref 0.0794 _refine_ls_wR_factor_gt 0.0676 _refine_ls_goodness_of_fit_ref 1.080 _refine_ls_restrained_S_all 1.080 _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 0.269120(19) 0.29356(3) 0.078606(18) 0.01541(8) Uani 1 1 d . . . Cl1 Cl 0.21579(4) 0.21341(6) -0.07996(4) 0.02116(12) Uani 1 1 d . . . Cl2 Cl 0.23511(4) 0.52181(6) 0.11145(4) 0.01969(12) Uani 1 1 d . . . S1 S 0.41989(4) 0.38808(6) 0.07398(4) 0.01805(12) Uani 1 1 d . . . N1 N 0.13866(13) 0.2158(2) 0.08540(13) 0.0175(4) Uani 1 1 d . . . N2 N 0.36265(13) 0.1123(2) 0.14081(13) 0.0159(4) Uani 1 1 d . . . C1 C 0.04908(17) 0.2865(3) 0.01160(18) 0.0262(5) Uani 1 1 d . . . H1A H -0.0138 0.2514 0.0133 0.039 Uiso 1 1 calc R . . H1B H 0.0479 0.2648 -0.0486 0.039 Uiso 1 1 calc R . . H1C H 0.0541 0.3900 0.0215 0.039 Uiso 1 1 calc R . . C2 C 0.13577(18) 0.2503(3) 0.17488(16) 0.0225(5) Uani 1 1 d . . . H2A H 0.0736 0.2104 0.1756 0.034 Uiso 1 1 calc R . . H2B H 0.1361 0.3541 0.1824 0.034 Uiso 1 1 calc R . . H2C H 0.1957 0.2091 0.2255 0.034 Uiso 1 1 calc R . . C3 C 0.12557(17) 0.0597(3) 0.06961(16) 0.0218(5) Uani 1 1 d . . . H3A H 0.1162 0.0398 0.0059 0.026 Uiso 1 1 calc R . . H3B H 0.0621 0.0307 0.0740 0.026 Uiso 1 1 calc R . . C4 C 0.21236(17) -0.0328(3) 0.13507(17) 0.0216(5) Uani 1 1 d . . . H4A H 0.2302 -0.0020 0.1992 0.026 Uiso 1 1 calc R . . H4B H 0.1886 -0.1329 0.1290 0.026 Uiso 1 1 calc R . . C5 C 0.30740(18) -0.0267(2) 0.11785(17) 0.0211(5) Uani 1 1 d . . . H5A H 0.3549 -0.1026 0.1546 0.025 Uiso 1 1 calc R . . H5B H 0.2878 -0.0478 0.0520 0.025 Uiso 1 1 calc R . . C6 C 0.41408(18) 0.1312(3) 0.24263(15) 0.0213(5) Uani 1 1 d . . . H6A H 0.4668 0.0579 0.2697 0.032 Uiso 1 1 calc R . . H6B H 0.3637 0.1223 0.2680 0.032 Uiso 1 1 calc R . . H6C H 0.4457 0.2259 0.2572 0.032 Uiso 1 1 calc R . . C7 C 0.43984(17) 0.1026(2) 0.10299(17) 0.0195(5) Uani 1 1 d . . . H7A H 0.4041 0.0840 0.0359 0.023 Uiso 1 1 calc R . . H7B H 0.4849 0.0200 0.1317 0.023 Uiso 1 1 calc R . . C8 C 0.50546(17) 0.2344(2) 0.11819(17) 0.0200(5) Uani 1 1 d . . . H8A H 0.5482 0.2472 0.1858 0.024 Uiso 1 1 calc R . . C9 C 0.57531(19) 0.2201(3) 0.06941(19) 0.0269(6) Uani 1 1 d . . . H9A H 0.6209 0.1383 0.0947 0.040 Uiso 1 1 calc R . . H9B H 0.6160 0.3072 0.0789 0.040 Uiso 1 1 calc R . . H9C H 0.5339 0.2056 0.0033 0.040 Uiso 1 1 calc R . . C10 C 0.47922(17) 0.5182(3) 0.16564(17) 0.0218(5) Uani 1 1 d . . . H10A H 0.4393 0.6079 0.1481 0.026 Uiso 1 1 calc R . . H10B H 0.4763 0.4820 0.2224 0.026 Uiso 1 1 calc R . . C11 C 0.59042(17) 0.5514(3) 0.18654(17) 0.0225(5) Uani 1 1 d . . . H11A H 0.6336 0.4668 0.2143 0.027 Uiso 1 1 calc R . . H11B H 0.5960 0.5754 0.1287 0.027 Uiso 1 1 calc R . . C12 C 0.62650(16) 0.6760(2) 0.25279(16) 0.0182(5) Uani 1 1 d . . . C13 C 0.64181(17) 0.8100(3) 0.22404(17) 0.0208(5) Uani 1 1 d . . . H13A H 0.6343 0.8227 0.1627 0.025 Uiso 1 1 calc R . . C14 C 0.66805(17) 0.9260(3) 0.28402(17) 0.0219(5) Uani 1 1 d . . . H14A H 0.6782 1.0172 0.2634 0.026 Uiso 1 1 calc R . . C15 C 0.67934(17) 0.9087(3) 0.37343(17) 0.0222(5) Uani 1 1 d . . . H15A H 0.6953 0.9883 0.4139 0.027 Uiso 1 1 calc R . . C16 C 0.66717(17) 0.7742(3) 0.40386(17) 0.0214(5) Uani 1 1 d . . . H16A H 0.6769 0.7612 0.4658 0.026 Uiso 1 1 calc R . . C17 C 0.64073(16) 0.6586(3) 0.34367(16) 0.0193(5) Uani 1 1 d . . . H17A H 0.6323 0.5670 0.3648 0.023 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01520(13) 0.01614(14) 0.01613(14) -0.00103(11) 0.00787(11) -0.00007(11) Cl1 0.0290(3) 0.0198(3) 0.0159(3) -0.0021(2) 0.0108(2) -0.0017(2) Cl2 0.0223(3) 0.0187(3) 0.0208(3) -0.0005(2) 0.0117(2) 0.0034(2) S1 0.0186(3) 0.0166(3) 0.0217(3) -0.0031(2) 0.0112(2) -0.0019(2) N1 0.0141(8) 0.0220(10) 0.0157(9) -0.0028(8) 0.0057(7) -0.0008(8) N2 0.0164(9) 0.0165(9) 0.0171(9) -0.0010(7) 0.0094(8) -0.0010(7) C1 0.0156(11) 0.0341(15) 0.0253(13) 0.0016(11) 0.0053(10) 0.0023(10) C2 0.0220(11) 0.0283(13) 0.0206(12) -0.0038(10) 0.0124(10) -0.0016(10) C3 0.0191(11) 0.0289(13) 0.0160(11) -0.0053(10) 0.0063(9) -0.0076(10) C4 0.0258(12) 0.0185(12) 0.0210(12) 0.0006(9) 0.0105(10) -0.0059(9) C5 0.0243(12) 0.0181(12) 0.0208(12) -0.0004(9) 0.0094(10) -0.0002(9) C6 0.0208(11) 0.0242(12) 0.0173(11) -0.0004(9) 0.0067(9) -0.0021(10) C7 0.0177(11) 0.0190(12) 0.0235(12) -0.0031(9) 0.0102(9) 0.0024(9) C8 0.0167(10) 0.0195(12) 0.0260(13) -0.0039(9) 0.0112(9) 0.0010(9) C9 0.0237(12) 0.0266(14) 0.0381(15) -0.0062(11) 0.0204(11) -0.0021(10) C10 0.0192(11) 0.0190(12) 0.0295(13) -0.0095(10) 0.0125(10) -0.0042(9) C11 0.0200(11) 0.0227(13) 0.0266(13) -0.0069(10) 0.0117(10) -0.0038(10) C12 0.0128(10) 0.0221(12) 0.0221(12) -0.0024(9) 0.0096(9) -0.0002(9) C13 0.0184(11) 0.0247(12) 0.0210(12) 0.0030(10) 0.0101(9) -0.0007(9) C14 0.0172(11) 0.0175(11) 0.0282(13) 0.0010(10) 0.0071(10) -0.0008(9) C15 0.0164(11) 0.0216(12) 0.0268(13) -0.0054(10) 0.0075(10) 0.0002(9) C16 0.0173(11) 0.0284(13) 0.0193(12) -0.0006(10) 0.0086(9) 0.0001(10) C17 0.0170(11) 0.0189(11) 0.0239(12) -0.0006(9) 0.0106(9) -0.0020(9) _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 2.0714(18) . ? Cu1 N2 2.1362(19) . ? Cu1 Cl2 2.3061(6) . ? Cu1 S1 2.3870(6) . ? Cu1 Cl1 2.4394(6) . ? S1 C10 1.819(2) . ? S1 C8 1.834(2) . ? N1 C3 1.482(3) . ? N1 C1 1.488(3) . ? N1 C2 1.489(3) . ? N2 C7 1.485(3) . ? N2 C6 1.488(3) . ? N2 C5 1.490(3) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.519(3) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.516(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.514(3) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C9 1.526(3) . ? C8 H8A 1.0000 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.530(3) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C12 1.514(3) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C13 1.388(3) . ? C12 C17 1.392(3) . ? C13 C14 1.393(3) . ? C13 H13A 0.9500 . ? C14 C15 1.382(3) . ? C14 H14A 0.9500 . ? C15 C16 1.390(3) . ? C15 H15A 0.9500 . ? C16 C17 1.392(3) . ? C16 H16A 0.9500 . ? C17 H17A 0.9500 . ? 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 N2 96.10(7) . . ? N1 Cu1 Cl2 91.49(5) . . ? N2 Cu1 Cl2 141.80(5) . . ? N1 Cu1 S1 178.39(6) . . ? N2 Cu1 S1 84.46(5) . . ? Cl2 Cu1 S1 87.15(2) . . ? N1 Cu1 Cl1 93.24(5) . . ? N2 Cu1 Cl1 95.58(5) . . ? Cl2 Cu1 Cl1 121.36(2) . . ? S1 Cu1 Cl1 88.20(2) . . ? C10 S1 C8 101.90(11) . . ? C10 S1 Cu1 110.28(8) . . ? C8 S1 Cu1 99.95(8) . . ? C3 N1 C1 107.43(17) . . ? C3 N1 C2 108.95(18) . . ? C1 N1 C2 107.22(18) . . ? C3 N1 Cu1 113.03(14) . . ? C1 N1 Cu1 107.85(14) . . ? C2 N1 Cu1 112.08(14) . . ? C7 N2 C6 110.12(17) . . ? C7 N2 C5 105.32(17) . . ? C6 N2 C5 109.87(18) . . ? C7 N2 Cu1 107.20(13) . . ? C6 N2 Cu1 109.76(14) . . ? C5 N2 Cu1 114.40(13) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N1 C3 C4 115.94(18) . . ? N1 C3 H3A 108.3 . . ? C4 C3 H3A 108.3 . . ? N1 C3 H3B 108.3 . . ? C4 C3 H3B 108.3 . . ? H3A C3 H3B 107.4 . . ? C5 C4 C3 113.6(2) . . ? C5 C4 H4A 108.8 . . ? C3 C4 H4A 108.8 . . ? C5 C4 H4B 108.8 . . ? C3 C4 H4B 108.8 . . ? H4A C4 H4B 107.7 . . ? N2 C5 C4 114.95(19) . . ? N2 C5 H5A 108.5 . . ? C4 C5 H5A 108.5 . . ? N2 C5 H5B 108.5 . . ? C4 C5 H5B 108.5 . . ? H5A C5 H5B 107.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N2 C7 C8 114.51(18) . . ? N2 C7 H7A 108.6 . . ? C8 C7 H7A 108.6 . . ? N2 C7 H7B 108.6 . . ? C8 C7 H7B 108.6 . . ? H7A C7 H7B 107.6 . . ? C7 C8 C9 110.73(19) . . ? C7 C8 S1 107.73(15) . . ? C9 C8 S1 110.93(18) . . ? C7 C8 H8A 109.1 . . ? C9 C8 H8A 109.1 . . ? S1 C8 H8A 109.1 . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 S1 113.76(16) . . ? C11 C10 H10A 108.8 . . ? S1 C10 H10A 108.8 . . ? C11 C10 H10B 108.8 . . ? S1 C10 H10B 108.8 . . ? H10A C10 H10B 107.7 . . ? C12 C11 C10 109.02(19) . . ? C12 C11 H11A 109.9 . . ? C10 C11 H11A 109.9 . . ? C12 C11 H11B 109.9 . . ? C10 C11 H11B 109.9 . . ? H11A C11 H11B 108.3 . . ? C13 C12 C17 118.7(2) . . ? C13 C12 C11 121.4(2) . . ? C17 C12 C11 119.8(2) . . ? C12 C13 C14 120.8(2) . . ? C12 C13 H13A 119.6 . . ? C14 C13 H13A 119.6 . . ? C15 C14 C13 120.1(2) . . ? C15 C14 H14A 120.0 . . ? C13 C14 H14A 120.0 . . ? C14 C15 C16 119.6(2) . . ? C14 C15 H15A 120.2 . . ? C16 C15 H15A 120.2 . . ? C15 C16 C17 120.1(2) . . ? C15 C16 H16A 120.0 . . ? C17 C16 H16A 120.0 . . ? C16 C17 C12 120.6(2) . . ? C16 C17 H17A 119.7 . . ? C12 C17 H17A 119.7 . . ? 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 Cu1 S1 C10 8(2) . . . . ? N2 Cu1 S1 C10 -102.55(10) . . . . ? Cl2 Cu1 S1 C10 40.14(9) . . . . ? Cl1 Cu1 S1 C10 161.66(9) . . . . ? N1 Cu1 S1 C8 115(2) . . . . ? N2 Cu1 S1 C8 4.19(9) . . . . ? Cl2 Cu1 S1 C8 146.88(8) . . . . ? Cl1 Cu1 S1 C8 -91.60(8) . . . . ? N2 Cu1 N1 C3 -36.34(15) . . . . ? Cl2 Cu1 N1 C3 -178.85(14) . . . . ? S1 Cu1 N1 C3 -147(2) . . . . ? Cl1 Cu1 N1 C3 59.63(14) . . . . ? N2 Cu1 N1 C1 -154.95(15) . . . . ? Cl2 Cu1 N1 C1 62.55(15) . . . . ? S1 Cu1 N1 C1 95(2) . . . . ? Cl1 Cu1 N1 C1 -58.98(15) . . . . ? N2 Cu1 N1 C2 87.26(15) . . . . ? Cl2 Cu1 N1 C2 -55.25(15) . . . . ? S1 Cu1 N1 C2 -23(2) . . . . ? Cl1 Cu1 N1 C2 -176.77(14) . . . . ? N1 Cu1 N2 C7 151.08(14) . . . . ? Cl2 Cu1 N2 C7 -108.66(13) . . . . ? S1 Cu1 N2 C7 -30.43(13) . . . . ? Cl1 Cu1 N2 C7 57.21(13) . . . . ? N1 Cu1 N2 C6 -89.32(14) . . . . ? Cl2 Cu1 N2 C6 10.94(18) . . . . ? S1 Cu1 N2 C6 89.17(13) . . . . ? Cl1 Cu1 N2 C6 176.81(13) . . . . ? N1 Cu1 N2 C5 34.71(15) . . . . ? Cl2 Cu1 N2 C5 134.97(13) . . . . ? S1 Cu1 N2 C5 -146.80(15) . . . . ? Cl1 Cu1 N2 C5 -59.16(15) . . . . ? C1 N1 C3 C4 176.9(2) . . . . ? C2 N1 C3 C4 -67.3(2) . . . . ? Cu1 N1 C3 C4 58.0(2) . . . . ? N1 C3 C4 C5 -73.0(3) . . . . ? C7 N2 C5 C4 -169.93(19) . . . . ? C6 N2 C5 C4 71.5(2) . . . . ? Cu1 N2 C5 C4 -52.5(2) . . . . ? C3 C4 C5 N2 69.0(3) . . . . ? C6 N2 C7 C8 -61.9(2) . . . . ? C5 N2 C7 C8 179.71(19) . . . . ? Cu1 N2 C7 C8 57.5(2) . . . . ? N2 C7 C8 C9 -174.69(19) . . . . ? N2 C7 C8 S1 -53.2(2) . . . . ? C10 S1 C8 C7 135.28(17) . . . . ? Cu1 S1 C8 C7 21.91(17) . . . . ? C10 S1 C8 C9 -103.39(18) . . . . ? Cu1 S1 C8 C9 143.25(15) . . . . ? C8 S1 C10 C11 57.4(2) . . . . ? Cu1 S1 C10 C11 162.81(16) . . . . ? S1 C10 C11 C12 171.44(17) . . . . ? C10 C11 C12 C13 -107.6(2) . . . . ? C10 C11 C12 C17 69.7(3) . . . . ? C17 C12 C13 C14 -1.8(3) . . . . ? C11 C12 C13 C14 175.4(2) . . . . ? C12 C13 C14 C15 0.1(3) . . . . ? C13 C14 C15 C16 1.8(3) . . . . ? C14 C15 C16 C17 -1.9(3) . . . . ? C15 C16 C17 C12 0.2(3) . . . . ? C13 C12 C17 C16 1.7(3) . . . . ? C11 C12 C17 C16 -175.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 27.88 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 0.524 _refine_diff_density_min -0.373 _refine_diff_density_rms 0.079 _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' _symmetry_space_group_name_Hall '-P 2yn' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist 18.00 0.00 -18.00 0.0308 -17.00 0.00 19.00 0.0512 -19.00 0.00 16.00 0.0426 8.00 5.00 13.00 0.1424 -11.00 0.00 -12.00 0.0676 5.00 -11.00 6.00 0.3121 14.00 -1.00 8.00 0.0973 -1.00 -1.00 21.00 0.0994 -10.00 11.00 11.00 0.2818 _audit_creation_date ; 'Tue Dec 19 14:17:38 2006' ; _audit_creation_method_reference ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_collection_reference ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_cell_refinment_reference ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _computing_data_reduction_reference ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) ; _cell_measurement_reflns_used 7885 _cell_measurement_theta_min 3.8383 _cell_measurement_theta_max 27.9996 _cell_measurement_resolution_max 0.76 _exptl_crystal_size_max 0.7668 _exptl_crystal_size_mid 0.1797 _exptl_crystal_size_min 0.0788 _exptl_absorpt_coefficient_mu 1.472 _exptl_absorpt_correction_T_min 0.519 _exptl_absorpt_correction_T_max 0.899 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.31.7 (release 18-10-2006 CrysAlis171 .NET) (compiled Oct 18 2006,16:28:17) 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) ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 15.9890 _diffrn_orient_matrix_UB_11 0.0322687683 _diffrn_orient_matrix_UB_12 0.0348316513 _diffrn_orient_matrix_UB_13 0.0413398054 _diffrn_orient_matrix_UB_21 0.0185375016 _diffrn_orient_matrix_UB_22 0.0447538567 _diffrn_orient_matrix_UB_23 -0.0249994427 _diffrn_orient_matrix_UB_31 -0.0391993542 _diffrn_orient_matrix_UB_32 0.0498213471 _diffrn_orient_matrix_UB_33 -0.0065187853 _diffrn_measurement_details 'see scan set' loop_ _diffrn_scan_number _diffrn_scan_type _diffrn_scan_start _diffrn_scan_end _diffrn_scan_width _diffrn_scan_exptime _diffrn_scan_omega _diffrn_scan_theta _diffrn_scan_kappa _diffrn_scan_phi _diffrn_scan_omega1 _diffrn_scan_theta1 _diffrn_scan_frames 1 omega -3.00 48.00 1.00 25.00 - 24.43 65.00 119.00 0.00 0.00 51 2 omega 43.00 97.00 1.00 25.00 - 24.43 75.00 120.00 0.00 0.00 54 3 omega -2.00 44.00 1.00 25.00 - 24.43 -126.00 323.00 0.00 0.00 46 4 omega 41.00 85.00 1.00 25.00 - 24.43 -126.00 323.00 0.00 0.00 44 5 omega -52.00 -3.00 1.00 25.00 - -25.05 45.00 240.00 0.00 0.00 49 6 omega -5.00 45.00 1.00 25.00 - -25.05 65.00 119.00 0.00 0.00 50 7 phi -56.00 -1.00 1.00 25.00 -40.00 -25.05 0.00 - 0.00 0.00 55 8 omega -4.00 24.00 1.00 25.00 - -25.05 45.00 120.00 0.00 0.00 28 _diffrn_measurement_method ' omega phi scans' _JHU_your_name_here 'Dr. Amy A Sarjeant' _JHU_your_lab_here 'NCB 240' _JHU_your_phone_number_here x6-8569 _JHU_your_email_here xray@jhu.edu _JHU_Institutional_Source 'Karlin Lab' _JHU_Submitting_Scientist 'Yunho Lee' _JHU_Scientist_Phone x6-6161 _JHU_Scientist_EMail yunho@jhu.edu _JHU_identifying_number x0325 _JHU_xray_labbook II-47 _JHU_crystalization_labbook L04-ANSCu2 _diffrn_source_power 2 _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_measurement_device Kappa _diffrn_measurement_device_type Xcalibur3 _diffrn_ambient_temperature 110 _JHU_diffraction_detector_distance 50 _JHU_quality_factor 1 data_x0363 _database_code_depnum_ccdc_archive 'CCDC 738907' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C19 H33 Cu N3 S, C24 B F20' _chemical_formula_sum 'C43 H33 B Cu F20 N3 S' _chemical_formula_weight 1078.13 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 20.3371(4) _cell_length_b 16.4920(3) _cell_length_c 26.8598(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 9008.8(3) _cell_formula_units_Z 8 _cell_measurement_temperature 110(2) _exptl_crystal_description prism _exptl_crystal_colour colorless _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.590 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4336 _exptl_special_details ; 1.0mm collimator used for data collection ; _diffrn_radiation_wavelength 0.71073 _diffrn_standards_number ? _diffrn_standards_interval_count 2 _diffrn_standards_interval_time 50 _diffrn_standards_decay_% ? _diffrn_reflns_number 55908 _diffrn_reflns_av_R_equivalents 0.0825 _diffrn_reflns_av_sigmaI/netI 0.0674 _diffrn_reflns_limit_h_min -26 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.84 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_resolution_max 0.77 _reflns_number_total 10274 _reflns_number_gt 6304 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Oxford Diffraction CrysAlis CCD' _computing_cell_refinement 'Oxford Diffraction CrysAlis RED' _computing_data_reduction 'Oxford Diffraction CrysAlis RED' _computing_structure_solution 'Sheldrick, G.M. (2000). SHELXTL v6.10.' _computing_structure_refinement 'Sheldrick, G.M. (2000). SHELXTL v6.10.' _computing_molecular_graphics 'Sheldrick, G.M. (2000). SHELXTL v6.10.' _computing_publication_material 'Sheldrick, G.M. (2000). SHELXTL v6.10.' _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. This structure exhibits whole-molecule disorder for the cationic portion. The two conformations occupy roughly the same space and are disordered in a 59/41 ratio. The minor component was restrained to have similar bond distances to the major component by the SAME instruction. DELU and SIMU restraints were used for the cations only as well. ; _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^)+(0.0000P)^2^+26.3525P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10274 _refine_ls_number_parameters 848 _refine_ls_number_restraints 762 _refine_ls_R_factor_all 0.1570 _refine_ls_R_factor_gt 0.0910 _refine_ls_wR_factor_ref 0.1412 _refine_ls_wR_factor_gt 0.1169 _refine_ls_goodness_of_fit_ref 1.253 _refine_ls_restrained_S_all 1.217 _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 0.32638(12) 1.1194(2) 0.14901(12) 0.0332(5) Uani 0.59 1 d PDU A 1 S1 S 0.39303(10) 1.06131(12) 0.09018(8) 0.0373(5) Uani 0.59 1 d PDU A 1 N1 N 0.2314(4) 1.0772(5) 0.1458(3) 0.039(2) Uani 0.59 1 d PDU A 1 N2 N 0.3289(4) 1.2288(5) 0.1074(3) 0.0281(19) Uani 0.59 1 d PDU A 1 N3 N 0.3617(8) 1.1304(12) 0.2156(4) 0.035(3) Uani 0.59 1 d PDU A 1 C1 C 0.2086(7) 1.0516(8) 0.1955(5) 0.075(4) Uani 0.59 1 d PDU A 1 H1A H 0.1625 1.0346 0.1935 0.112 Uiso 0.59 1 calc PR A 1 H1B H 0.2127 1.0970 0.2188 0.112 Uiso 0.59 1 calc PR A 1 H1C H 0.2356 1.0061 0.2072 0.112 Uiso 0.59 1 calc PR A 1 C2 C 0.2297(5) 1.0056(5) 0.1116(4) 0.061(3) Uani 0.59 1 d PDU A 1 H2A H 0.1848 0.9840 0.1101 0.092 Uiso 0.59 1 calc PR A 1 H2B H 0.2595 0.9636 0.1241 0.092 Uiso 0.59 1 calc PR A 1 H2C H 0.2436 1.0223 0.0782 0.092 Uiso 0.59 1 calc PR A 1 C3 C 0.1869(4) 1.1389(5) 0.1259(3) 0.0368(17) Uani 0.59 1 d PDU A 1 H3A H 0.1744 1.1756 0.1535 0.044 Uiso 0.59 1 calc PR A 1 H3B H 0.1463 1.1115 0.1145 0.044 Uiso 0.59 1 calc PR A 1 C4 C 0.2123(6) 1.1895(8) 0.0841(5) 0.036(3) Uani 0.59 1 d PDU A 1 H4A H 0.1741 1.2149 0.0674 0.044 Uiso 0.59 1 calc PR A 1 H4B H 0.2333 1.1528 0.0597 0.044 Uiso 0.59 1 calc PR A 1 C5 C 0.2614(4) 1.2564(4) 0.0967(3) 0.0375(17) Uani 0.59 1 d PDU A 1 H5A H 0.2630 1.2948 0.0684 0.045 Uiso 0.59 1 calc PR A 1 H5B H 0.2448 1.2866 0.1259 0.045 Uiso 0.59 1 calc PR A 1 C6 C 0.3647(7) 1.2934(8) 0.1358(5) 0.046(4) Uani 0.59 1 d PDU A 1 H6A H 0.3648 1.3437 0.1163 0.069 Uiso 0.59 1 calc PR A 1 H6B H 0.4100 1.2761 0.1419 0.069 Uiso 0.59 1 calc PR A 1 H6C H 0.3425 1.3028 0.1677 0.069 Uiso 0.59 1 calc PR A 1 C7 C 0.3645(4) 1.2128(5) 0.0610(3) 0.0334(17) Uani 0.59 1 d PDU A 1 H7A H 0.3785 1.2651 0.0463 0.040 Uiso 0.59 1 calc PR A 1 H7B H 0.3343 1.1863 0.0371 0.040 Uiso 0.59 1 calc PR A 1 C8 C 0.4247(5) 1.1591(6) 0.0682(4) 0.035(2) Uani 0.59 1 d PDU A 1 H8A H 0.4529 1.1833 0.0949 0.043 Uiso 0.59 1 calc PR A 1 C9 C 0.4629(4) 1.0237(5) 0.1246(3) 0.046(2) Uani 0.59 1 d PDU A 1 H9A H 0.4992 1.0109 0.1013 0.055 Uiso 0.59 1 calc PR A 1 H9B H 0.4785 1.0659 0.1480 0.055 Uiso 0.59 1 calc PR A 1 C10 C 0.4434(4) 0.9475(5) 0.1535(3) 0.043(2) Uani 0.59 1 d PDU A 1 H10A H 0.4046 0.9591 0.1745 0.052 Uiso 0.59 1 calc PR A 1 H10B H 0.4315 0.9038 0.1298 0.052 Uiso 0.59 1 calc PR A 1 C11 C 0.5002(5) 0.9198(7) 0.1860(4) 0.037(2) Uani 0.59 1 d PDU A 1 C12 C 0.5001(6) 0.9391(9) 0.2360(5) 0.048(3) Uani 0.59 1 d PDU A 1 H12A H 0.4630 0.9647 0.2507 0.058 Uiso 0.59 1 calc PR A 1 C13 C 0.5555(5) 0.9204(7) 0.2648(4) 0.054(3) Uani 0.59 1 d PDU A 1 H13A H 0.5545 0.9300 0.2997 0.065 Uiso 0.59 1 calc PR A 1 C14 C 0.6107(5) 0.8887(7) 0.2437(4) 0.046(3) Uani 0.59 1 d PDU A 1 H14A H 0.6487 0.8782 0.2632 0.055 Uiso 0.59 1 calc PR A 1 C15 C 0.6101(8) 0.872(2) 0.1935(6) 0.044(4) Uani 0.59 1 d PDU A 1 H15A H 0.6486 0.8511 0.1782 0.053 Uiso 0.59 1 calc PR A 1 C16 C 0.5556(6) 0.8854(15) 0.1653(6) 0.039(3) Uani 0.59 1 d PDU A 1 H16A H 0.5557 0.8709 0.1310 0.047 Uiso 0.59 1 calc PR A 1 C17 C 0.3802(15) 1.144(2) 0.2545(6) 0.037(5) Uani 0.59 1 d PDU A 1 C18 C 0.4139(10) 1.1575(13) 0.3018(5) 0.048(5) Uani 0.59 1 d PDU A 1 H18A H 0.3818 1.1738 0.3272 0.073 Uiso 0.59 1 calc PR A 1 H18B H 0.4467 1.2006 0.2977 0.073 Uiso 0.59 1 calc PR A 1 H18C H 0.4358 1.1074 0.3124 0.073 Uiso 0.59 1 calc PR A 1 C19 C 0.4652(8) 1.1501(11) 0.0216(6) 0.056(5) Uani 0.59 1 d PDU A 1 H19A H 0.4824 1.2032 0.0117 0.084 Uiso 0.59 1 calc PR A 1 H19B H 0.4376 1.1283 -0.0052 0.084 Uiso 0.59 1 calc PR A 1 H19C H 0.5019 1.1130 0.0279 0.084 Uiso 0.59 1 calc PR A 1 Cu1' Cu 0.34569(17) 1.1082(3) 0.15500(17) 0.0318(7) Uani 0.41 1 d PDU B 2 S1' S 0.43743(15) 1.06568(17) 0.11537(11) 0.0301(6) Uani 0.41 1 d PDU B 2 N1' N 0.2519(5) 1.0637(7) 0.1539(5) 0.038(3) Uani 0.41 1 d PDU B 2 N2' N 0.3420(6) 1.2106(7) 0.1061(5) 0.036(3) Uani 0.41 1 d PDU B 2 N3' N 0.3664(12) 1.1424(18) 0.2238(5) 0.035(4) Uani 0.41 1 d PDU B 2 C1' C 0.2146(9) 1.0899(9) 0.1990(5) 0.044(4) Uani 0.41 1 d PDU B 2 H1'A H 0.1692 1.0702 0.1968 0.067 Uiso 0.41 1 calc PR B 2 H1'B H 0.2145 1.1493 0.2010 0.067 Uiso 0.41 1 calc PR B 2 H1'C H 0.2355 1.0675 0.2288 0.067 Uiso 0.41 1 calc PR B 2 C2' C 0.2497(7) 0.9744(6) 0.1547(6) 0.057(3) Uani 0.41 1 d PDU B 2 H2'A H 0.2038 0.9563 0.1540 0.085 Uiso 0.41 1 calc PR B 2 H2'B H 0.2709 0.9545 0.1851 0.085 Uiso 0.41 1 calc PR B 2 H2'C H 0.2728 0.9529 0.1255 0.085 Uiso 0.41 1 calc PR B 2 C3' C 0.2159(6) 1.0896(7) 0.1098(5) 0.043(3) Uani 0.41 1 d PDU B 2 H3'A H 0.1689 1.0753 0.1141 0.052 Uiso 0.41 1 calc PR B 2 H3'B H 0.2325 1.0589 0.0807 0.052 Uiso 0.41 1 calc PR B 2 C4' C 0.2205(8) 1.1780(12) 0.0984(9) 0.050(5) Uani 0.41 1 d PDU B 2 H4'A H 0.2144 1.2082 0.1300 0.060 Uiso 0.41 1 calc PR B 2 H4'B H 0.1833 1.1925 0.0764 0.060 Uiso 0.41 1 calc PR B 2 C5' C 0.2833(5) 1.2077(8) 0.0742(4) 0.048(3) Uani 0.41 1 d PDU B 2 H5'A H 0.2930 1.1722 0.0454 0.058 Uiso 0.41 1 calc PR B 2 H5'B H 0.2753 1.2629 0.0611 0.058 Uiso 0.41 1 calc PR B 2 C6' C 0.3417(8) 1.2865(9) 0.1364(8) 0.037(4) Uani 0.41 1 d PDU B 2 H6'A H 0.3376 1.3335 0.1142 0.056 Uiso 0.41 1 calc PR B 2 H6'B H 0.3828 1.2905 0.1553 0.056 Uiso 0.41 1 calc PR B 2 H6'C H 0.3044 1.2855 0.1595 0.056 Uiso 0.41 1 calc PR B 2 C7' C 0.4014(6) 1.2083(7) 0.0756(4) 0.035(3) Uani 0.41 1 d PDU B 2 H7'A H 0.4377 1.2334 0.0947 0.042 Uiso 0.41 1 calc PR B 2 H7'B H 0.3939 1.2420 0.0457 0.042 Uiso 0.41 1 calc PR B 2 C8' C 0.4233(7) 1.1245(8) 0.0589(5) 0.036(3) Uani 0.41 1 d PDU B 2 H8'A H 0.3865 1.0988 0.0399 0.044 Uiso 0.41 1 calc PR B 2 C9' C 0.4310(6) 0.9645(6) 0.0901(4) 0.038(3) Uani 0.41 1 d PDU B 2 H9'A H 0.3912 0.9604 0.0690 0.045 Uiso 0.41 1 calc PR B 2 H9'B H 0.4698 0.9527 0.0692 0.045 Uiso 0.41 1 calc PR B 2 C10' C 0.4268(6) 0.9028(7) 0.1325(4) 0.039(3) Uani 0.41 1 d PDU B 2 H10C H 0.3862 0.9127 0.1519 0.047 Uiso 0.41 1 calc PR B 2 H10D H 0.4240 0.8476 0.1182 0.047 Uiso 0.41 1 calc PR B 2 C11' C 0.4850(7) 0.9070(10) 0.1669(5) 0.034(3) Uani 0.41 1 d PDU B 2 C12' C 0.4792(8) 0.9381(11) 0.2140(6) 0.047(3) Uani 0.41 1 d PDU B 2 H12B H 0.4377 0.9583 0.2244 0.056 Uiso 0.41 1 calc PR B 2 C13' C 0.5319(8) 0.9414(13) 0.2472(6) 0.050(4) Uani 0.41 1 d PDU B 2 H13B H 0.5264 0.9630 0.2797 0.060 Uiso 0.41 1 calc PR B 2 C14' C 0.5917(8) 0.9128(11) 0.2319(6) 0.048(4) Uani 0.41 1 d PDU B 2 H14B H 0.6290 0.9159 0.2531 0.057 Uiso 0.41 1 calc PR B 2 C15' C 0.5966(12) 0.879(3) 0.1849(8) 0.040(4) Uani 0.41 1 d PDU B 2 H15B H 0.6380 0.8589 0.1744 0.048 Uiso 0.41 1 calc PR B 2 C16' C 0.5448(10) 0.874(2) 0.1529(8) 0.041(5) Uani 0.41 1 d PDU B 2 H16B H 0.5498 0.8489 0.1215 0.049 Uiso 0.41 1 calc PR B 2 C17' C 0.391(2) 1.147(3) 0.2615(9) 0.022(4) Uani 0.41 1 d PDU B 2 C18' C 0.4152(14) 1.1615(17) 0.3120(7) 0.036(5) Uani 0.41 1 d PDU B 2 H18D H 0.4539 1.1275 0.3180 0.054 Uiso 0.41 1 calc PR B 2 H18E H 0.3807 1.1477 0.3360 0.054 Uiso 0.41 1 calc PR B 2 H18F H 0.4272 1.2187 0.3158 0.054 Uiso 0.41 1 calc PR B 2 C19' C 0.4828(11) 1.1292(16) 0.0252(8) 0.044(5) Uani 0.41 1 d PDU B 2 H19D H 0.4742 1.1677 -0.0018 0.066 Uiso 0.41 1 calc PR B 2 H19E H 0.4917 1.0755 0.0112 0.066 Uiso 0.41 1 calc PR B 2 H19F H 0.5209 1.1474 0.0445 0.066 Uiso 0.41 1 calc PR B 2 B1 B 0.3256(2) 0.8782(3) 0.39193(17) 0.0237(10) Uani 1 1 d . . . F1 F 0.44874(12) 0.96153(15) 0.34910(10) 0.0385(6) Uani 1 1 d . . . F2 F 0.51867(13) 1.07368(16) 0.39423(12) 0.0519(8) Uani 1 1 d . . . F3 F 0.48918(15) 1.12114(16) 0.48872(12) 0.0571(9) Uani 1 1 d . . . F4 F 0.38868(15) 1.04815(15) 0.53813(10) 0.0493(8) Uani 1 1 d . . . F5 F 0.31708(13) 0.93391(14) 0.49341(9) 0.0334(6) Uani 1 1 d . . . F6 F 0.31670(12) 1.01197(14) 0.32286(9) 0.0323(6) Uani 1 1 d . . . F7 F 0.22140(13) 1.12190(15) 0.31432(10) 0.0409(7) Uani 1 1 d . . . F8 F 0.11286(13) 1.11413(15) 0.37361(10) 0.0416(7) Uani 1 1 d . . . F9 F 0.10383(13) 0.99469(15) 0.44301(10) 0.0397(6) Uani 1 1 d . . . F10 F 0.19567(12) 0.88414(14) 0.45203(9) 0.0316(6) Uani 1 1 d . . . F11 F 0.21555(11) 0.77223(14) 0.37402(9) 0.0306(6) Uani 1 1 d . . . F12 F 0.18078(12) 0.63978(14) 0.42291(10) 0.0380(6) Uani 1 1 d . . . F13 F 0.25751(14) 0.58230(14) 0.49901(10) 0.0416(7) Uani 1 1 d . . . F14 F 0.36879(14) 0.66387(15) 0.52427(10) 0.0439(7) Uani 1 1 d . . . F15 F 0.40174(12) 0.79996(14) 0.47897(9) 0.0345(6) Uani 1 1 d . . . F16 F 0.44807(12) 0.79337(15) 0.37984(9) 0.0347(6) Uani 1 1 d . . . F17 F 0.49482(13) 0.71939(17) 0.29972(10) 0.0480(7) Uani 1 1 d . . . F18 F 0.42617(14) 0.72270(19) 0.21264(11) 0.0564(8) Uani 1 1 d . . . F19 F 0.30881(14) 0.80237(18) 0.20874(10) 0.0525(8) Uani 1 1 d . . . F20 F 0.25983(12) 0.87313(15) 0.28804(9) 0.0338(6) Uani 1 1 d . . . C101 C 0.3790(2) 0.9398(2) 0.41935(16) 0.0246(9) Uani 1 1 d . . . C102 C 0.4308(2) 0.9791(3) 0.39664(17) 0.0307(10) Uani 1 1 d . . . C103 C 0.4685(2) 1.0382(3) 0.41903(19) 0.0366(12) Uani 1 1 d . . . C104 C 0.4541(2) 1.0621(3) 0.4669(2) 0.0393(12) Uani 1 1 d . . . C105 C 0.4035(2) 1.0254(3) 0.49140(18) 0.0358(11) Uani 1 1 d . . . C106 C 0.3679(2) 0.9663(2) 0.46747(16) 0.0286(10) Uani 1 1 d . . . C107 C 0.26115(19) 0.9392(2) 0.38639(15) 0.0219(9) Uani 1 1 d . . . C108 C 0.2631(2) 1.0033(2) 0.35248(15) 0.0239(9) Uani 1 1 d . . . C109 C 0.2149(2) 1.0607(2) 0.34749(16) 0.0275(9) Uani 1 1 d . . . C110 C 0.1599(2) 1.0575(2) 0.37720(17) 0.0299(10) Uani 1 1 d . . . C111 C 0.1559(2) 0.9975(3) 0.41239(16) 0.0284(10) Uani 1 1 d . . . C112 C 0.2051(2) 0.9402(2) 0.41594(15) 0.0254(9) Uani 1 1 d . . . C113 C 0.3093(2) 0.7956(2) 0.42462(15) 0.0222(9) Uani 1 1 d . . . C114 C 0.2548(2) 0.7492(2) 0.41231(15) 0.0245(9) Uani 1 1 d . . . C115 C 0.2362(2) 0.6794(2) 0.43651(17) 0.0290(10) Uani 1 1 d . . . C116 C 0.2739(2) 0.6503(2) 0.47467(17) 0.0319(11) Uani 1 1 d . . . C117 C 0.3302(2) 0.6915(2) 0.48703(15) 0.0294(10) Uani 1 1 d . . . C118 C 0.3461(2) 0.7629(2) 0.46299(15) 0.0274(10) Uani 1 1 d . . . C119 C 0.3524(2) 0.8398(2) 0.33893(15) 0.0255(9) Uani 1 1 d . . . C120 C 0.4115(2) 0.7977(3) 0.33812(16) 0.0291(10) Uani 1 1 d . . . C121 C 0.4365(2) 0.7583(3) 0.29732(18) 0.0346(11) Uani 1 1 d . . . C122 C 0.4025(2) 0.7596(3) 0.25310(18) 0.0390(12) Uani 1 1 d . . . C123 C 0.3435(2) 0.7998(3) 0.25166(17) 0.0355(11) Uani 1 1 d . . . C124 C 0.3195(2) 0.8372(2) 0.29370(16) 0.0269(9) 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 0.0370(13) 0.0312(10) 0.0315(10) 0.0057(7) -0.0047(9) -0.0043(9) S1 0.0356(12) 0.0316(10) 0.0447(12) 0.0028(9) -0.0028(10) 0.0011(9) N1 0.031(4) 0.039(4) 0.047(5) 0.005(4) 0.001(4) -0.010(4) N2 0.033(4) 0.029(4) 0.021(4) 0.003(3) 0.001(3) -0.003(3) N3 0.035(5) 0.031(7) 0.038(4) 0.005(5) 0.001(4) -0.006(5) C1 0.061(7) 0.094(11) 0.069(7) 0.043(7) 0.005(6) -0.021(8) C2 0.059(6) 0.031(4) 0.095(7) -0.008(5) -0.040(6) -0.004(4) C3 0.031(4) 0.042(4) 0.037(5) -0.003(4) 0.003(3) -0.009(3) C4 0.038(5) 0.036(5) 0.035(7) 0.004(4) -0.005(4) 0.006(4) C5 0.052(4) 0.025(4) 0.035(4) 0.002(3) 0.006(4) 0.006(3) C6 0.068(10) 0.036(5) 0.035(6) -0.005(4) -0.007(7) -0.012(6) C7 0.042(5) 0.031(4) 0.028(4) 0.004(3) -0.003(4) -0.003(4) C8 0.039(5) 0.031(5) 0.036(5) 0.006(4) 0.000(4) 0.003(5) C9 0.043(5) 0.037(5) 0.059(6) 0.026(4) -0.010(4) 0.014(4) C10 0.040(5) 0.036(4) 0.053(5) 0.010(4) -0.005(4) 0.005(4) C11 0.036(5) 0.036(6) 0.038(6) 0.011(5) 0.001(4) 0.007(4) C12 0.043(7) 0.064(7) 0.037(6) 0.003(7) 0.004(5) 0.016(8) C13 0.046(6) 0.076(7) 0.041(6) 0.012(5) 0.007(4) 0.013(5) C14 0.033(5) 0.055(7) 0.048(6) 0.004(5) -0.001(4) 0.005(5) C15 0.028(6) 0.047(8) 0.056(7) 0.006(9) 0.007(5) 0.005(6) C16 0.042(6) 0.035(6) 0.040(7) -0.004(6) 0.004(5) 0.003(6) C17 0.041(14) 0.040(8) 0.030(7) 0.016(7) 0.002(6) -0.010(9) C18 0.058(9) 0.046(8) 0.041(8) 0.012(7) -0.002(7) -0.033(7) C19 0.061(11) 0.048(8) 0.059(8) -0.002(6) 0.017(8) -0.004(7) Cu1' 0.0417(19) 0.0311(15) 0.0227(12) 0.0012(10) -0.0049(13) -0.0066(14) S1' 0.0344(16) 0.0266(14) 0.0292(15) 0.0016(12) -0.0101(13) -0.0011(13) N1' 0.041(6) 0.029(5) 0.043(6) -0.004(5) -0.009(5) 0.004(5) N2' 0.040(6) 0.040(6) 0.030(6) -0.001(5) -0.004(4) 0.011(5) N3' 0.061(10) 0.023(8) 0.022(5) -0.009(6) -0.002(6) -0.016(7) C1' 0.046(8) 0.053(9) 0.035(6) 0.017(7) 0.005(6) -0.002(8) C2' 0.048(8) 0.038(5) 0.084(10) -0.005(6) -0.005(8) -0.019(5) C3' 0.038(6) 0.053(6) 0.039(6) -0.018(5) -0.009(5) -0.002(6) C4' 0.041(7) 0.056(7) 0.054(12) 0.009(7) -0.011(7) 0.023(7) C5' 0.044(6) 0.065(7) 0.035(6) 0.018(5) -0.013(5) 0.020(6) C6' 0.032(9) 0.022(6) 0.058(10) 0.006(6) 0.010(7) 0.018(6) C7' 0.041(6) 0.033(6) 0.031(7) 0.004(5) 0.006(5) 0.001(6) C8' 0.039(7) 0.035(6) 0.035(7) 0.004(6) 0.000(5) 0.013(7) C9' 0.049(7) 0.032(5) 0.032(6) -0.001(4) -0.012(5) 0.001(5) C10' 0.040(6) 0.027(5) 0.050(7) -0.002(5) -0.002(5) 0.001(5) C11' 0.039(7) 0.027(6) 0.038(7) 0.012(6) -0.004(5) 0.001(6) C12' 0.050(8) 0.048(8) 0.042(8) -0.003(8) 0.002(6) 0.011(7) C13' 0.063(11) 0.066(10) 0.022(7) 0.002(7) 0.005(6) 0.021(11) C14' 0.050(8) 0.061(10) 0.033(7) 0.008(7) -0.005(7) 0.010(7) C15' 0.040(9) 0.042(11) 0.037(8) 0.002(9) 0.002(7) 0.001(11) C16' 0.042(7) 0.040(12) 0.041(9) 0.009(8) -0.003(6) 0.012(9) C17' 0.013(8) 0.018(8) 0.035(8) 0.007(7) -0.014(6) -0.005(6) C18' 0.056(12) 0.036(10) 0.015(6) -0.002(6) -0.008(6) 0.029(8) C19' 0.036(9) 0.071(14) 0.025(7) 0.004(8) 0.002(6) 0.007(8) B1 0.023(2) 0.020(2) 0.028(2) 0.000(2) -0.001(2) 0.003(2) F1 0.0309(14) 0.0381(14) 0.0464(16) 0.0065(13) 0.0034(13) -0.0109(12) F2 0.0364(16) 0.0440(16) 0.076(2) 0.0147(16) -0.0118(15) -0.0166(14) F3 0.057(2) 0.0319(14) 0.082(2) -0.0043(16) -0.0382(17) -0.0110(14) F4 0.072(2) 0.0316(14) 0.0442(18) -0.0122(13) -0.0221(15) 0.0013(15) F5 0.0483(16) 0.0244(12) 0.0276(14) -0.0029(11) -0.0035(12) -0.0014(12) F6 0.0357(15) 0.0276(12) 0.0335(14) 0.0069(11) 0.0024(12) -0.0034(11) F7 0.0541(17) 0.0287(13) 0.0397(15) 0.0119(12) -0.0047(13) 0.0055(13) F8 0.0408(16) 0.0310(13) 0.0530(17) 0.0039(13) -0.0050(13) 0.0113(12) F9 0.0367(15) 0.0372(14) 0.0451(16) -0.0012(13) 0.0101(13) 0.0070(13) F10 0.0389(15) 0.0271(12) 0.0288(13) 0.0042(11) 0.0047(11) 0.0022(11) F11 0.0309(14) 0.0281(13) 0.0330(14) -0.0010(11) -0.0068(11) -0.0025(11) F12 0.0400(15) 0.0296(13) 0.0445(16) -0.0029(12) 0.0075(13) -0.0143(12) F13 0.0646(19) 0.0225(12) 0.0379(15) 0.0071(11) 0.0080(14) -0.0073(13) F14 0.0630(19) 0.0312(14) 0.0375(16) 0.0108(12) -0.0115(14) 0.0054(14) F15 0.0370(15) 0.0243(12) 0.0423(16) 0.0028(12) -0.0141(12) -0.0021(11) F16 0.0301(14) 0.0407(15) 0.0333(15) 0.0005(12) -0.0050(11) 0.0058(12) F17 0.0341(16) 0.0594(18) 0.0505(18) -0.0082(15) 0.0026(13) 0.0163(14) F18 0.0500(18) 0.075(2) 0.0444(18) -0.0250(16) 0.0051(14) 0.0145(16) F19 0.0551(19) 0.071(2) 0.0311(16) -0.0177(15) -0.0093(14) 0.0107(16) F20 0.0328(14) 0.0407(14) 0.0278(13) -0.0056(12) -0.0041(11) 0.0056(12) C101 0.026(2) 0.0151(18) 0.033(2) 0.0018(18) -0.0087(19) -0.0010(17) C102 0.031(2) 0.030(2) 0.031(3) 0.004(2) -0.005(2) -0.002(2) C103 0.024(2) 0.028(2) 0.057(3) 0.012(2) -0.010(2) -0.007(2) C104 0.040(3) 0.022(2) 0.056(3) 0.004(2) -0.029(3) -0.010(2) C105 0.047(3) 0.023(2) 0.038(3) -0.005(2) -0.022(2) 0.006(2) C106 0.036(3) 0.018(2) 0.032(2) 0.0010(18) -0.012(2) 0.0038(19) C107 0.023(2) 0.0192(19) 0.024(2) -0.0009(17) -0.0093(17) -0.0015(17) C108 0.027(2) 0.025(2) 0.020(2) -0.0016(18) -0.0018(18) -0.0033(18) C109 0.039(3) 0.0184(19) 0.026(2) 0.0020(18) -0.011(2) -0.0015(19) C110 0.027(2) 0.022(2) 0.040(3) -0.006(2) -0.006(2) 0.0080(19) C111 0.028(2) 0.027(2) 0.030(2) -0.0052(19) -0.0028(19) -0.0008(19) C112 0.029(2) 0.022(2) 0.025(2) -0.0021(18) -0.0029(18) -0.0055(18) C113 0.026(2) 0.0198(19) 0.021(2) -0.0021(17) 0.0040(17) 0.0025(17) C114 0.028(2) 0.0218(19) 0.024(2) -0.0032(18) 0.0007(18) 0.0010(18) C115 0.031(2) 0.019(2) 0.038(3) -0.0025(19) 0.005(2) -0.0059(19) C116 0.046(3) 0.0158(19) 0.033(3) -0.0046(19) 0.008(2) -0.002(2) C117 0.043(3) 0.020(2) 0.025(2) 0.0016(18) 0.002(2) 0.005(2) C118 0.034(2) 0.022(2) 0.027(2) -0.0065(18) -0.0015(19) -0.0004(19) C119 0.026(2) 0.022(2) 0.028(2) 0.0047(18) 0.0021(18) -0.0064(18) C120 0.030(2) 0.028(2) 0.029(2) -0.0016(19) -0.0030(19) -0.0023(19) C121 0.026(2) 0.035(3) 0.043(3) 0.003(2) 0.003(2) 0.006(2) C122 0.043(3) 0.042(3) 0.032(3) -0.012(2) 0.009(2) -0.002(2) C123 0.040(3) 0.038(3) 0.029(2) -0.006(2) -0.007(2) 0.000(2) C124 0.024(2) 0.026(2) 0.031(2) -0.0005(19) 0.0016(19) -0.0005(18) _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 N3 1.935(8) . ? Cu1 N1 2.056(7) . ? Cu1 N2 2.122(7) . ? Cu1 S1 2.292(4) . ? S1 C9 1.804(8) . ? S1 C8 1.835(9) . ? N1 C3 1.462(10) . ? N1 C1 1.475(11) . ? N1 C2 1.495(11) . ? N2 C7 1.466(10) . ? N2 C5 1.476(9) . ? N2 C6 1.499(10) . ? N3 C17 1.134(11) . ? C1 H1A 0.9800 . ? C1 H1B 0.9800 . ? C1 H1C 0.9800 . ? C2 H2A 0.9800 . ? C2 H2B 0.9800 . ? C2 H2C 0.9800 . ? C3 C4 1.490(12) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C4 C5 1.525(12) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C6 H6A 0.9800 . ? C6 H6B 0.9800 . ? C6 H6C 0.9800 . ? C7 C8 1.523(11) . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C8 C19 1.506(12) . ? C8 H8A 1.0000 . ? C9 C10 1.530(10) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? C10 C11 1.518(11) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C11 C16 1.378(11) . ? C11 C12 1.381(13) . ? C12 C13 1.401(13) . ? C12 H12A 0.9500 . ? C13 C14 1.362(12) . ? C13 H13A 0.9500 . ? C14 C15 1.376(12) . ? C14 H14A 0.9500 . ? C15 C16 1.362(12) . ? C15 H15A 0.9500 . ? C16 H16A 0.9500 . ? C17 C18 1.462(12) . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? Cu1' N3' 1.976(11) . ? Cu1' N1' 2.044(10) . ? Cu1' N2' 2.139(11) . ? Cu1' S1' 2.260(5) . ? S1' C9' 1.806(9) . ? S1' C8' 1.824(12) . ? N1' C3' 1.457(13) . ? N1' C2' 1.474(12) . ? N1' C1' 1.495(13) . ? N2' C7' 1.459(13) . ? N2' C5' 1.471(13) . ? N2' C6' 1.493(13) . ? N3' C17' 1.133(13) . ? C1' H1'A 0.9800 . ? C1' H1'B 0.9800 . ? C1' H1'C 0.9800 . ? C2' H2'A 0.9800 . ? C2' H2'B 0.9800 . ? C2' H2'C 0.9800 . ? C3' C4' 1.493(16) . ? C3' H3'A 0.9900 . ? C3' H3'B 0.9900 . ? C4' C5' 1.515(16) . ? C4' H4'A 0.9900 . ? C4' H4'B 0.9900 . ? C5' H5'A 0.9900 . ? C5' H5'B 0.9900 . ? C6' H6'A 0.9800 . ? C6' H6'B 0.9800 . ? C6' H6'C 0.9800 . ? C7' C8' 1.520(13) . ? C7' H7'A 0.9900 . ? C7' H7'B 0.9900 . ? C8' C19' 1.511(14) . ? C8' H8'A 1.0000 . ? C9' C10' 1.529(12) . ? C9' H9'A 0.9900 . ? C9' H9'B 0.9900 . ? C10' C11' 1.502(14) . ? C10' H10C 0.9900 . ? C10' H10D 0.9900 . ? C11' C12' 1.370(15) . ? C11' C16' 1.382(13) . ? C12' C13' 1.396(16) . ? C12' H12B 0.9500 . ? C13' C14' 1.367(16) . ? C13' H13B 0.9500 . ? C14' C15' 1.381(14) . ? C14' H14B 0.9500 . ? C15' C16' 1.360(15) . ? C15' H15B 0.9500 . ? C16' H16B 0.9500 . ? C17' C18' 1.461(14) . ? C18' H18D 0.9800 . ? C18' H18E 0.9800 . ? C18' H18F 0.9800 . ? C19' H19D 0.9800 . ? C19' H19E 0.9800 . ? C19' H19F 0.9800 . ? B1 C119 1.651(6) . ? B1 C113 1.655(6) . ? B1 C107 1.658(6) . ? B1 C101 1.659(6) . ? F1 C102 1.359(5) . ? F2 C103 1.351(5) . ? F3 C104 1.342(5) . ? F4 C105 1.344(5) . ? F5 C106 1.356(5) . ? F6 C108 1.356(4) . ? F7 C109 1.353(5) . ? F8 C110 1.340(5) . ? F9 C111 1.342(5) . ? F10 C112 1.353(4) . ? F11 C114 1.356(4) . ? F12 C115 1.353(5) . ? F13 C116 1.340(5) . ? F14 C117 1.351(5) . ? F15 C118 1.356(5) . ? F16 C120 1.346(5) . ? F17 C121 1.350(5) . ? F18 C122 1.336(5) . ? F19 C123 1.352(5) . ? F20 C124 1.359(5) . ? C101 C102 1.380(6) . ? C101 C106 1.383(6) . ? C102 C103 1.379(6) . ? C103 C104 1.376(7) . ? C104 C105 1.365(7) . ? C105 C106 1.373(6) . ? C107 C112 1.389(6) . ? C107 C108 1.396(5) . ? C108 C109 1.370(6) . ? C109 C110 1.375(6) . ? C110 C111 1.371(6) . ? C111 C112 1.380(6) . ? C113 C118 1.383(6) . ? C113 C114 1.387(5) . ? C114 C115 1.374(6) . ? C115 C116 1.368(6) . ? C116 C117 1.372(6) . ? C117 C118 1.382(6) . ? C119 C124 1.387(6) . ? C119 C120 1.390(6) . ? C120 C121 1.372(6) . ? C121 C122 1.375(7) . ? C122 C123 1.371(6) . ? C123 C124 1.376(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N3 Cu1 N1 114.8(5) . . ? N3 Cu1 N2 113.4(6) . . ? N1 Cu1 N2 106.8(3) . . ? N3 Cu1 S1 117.2(5) . . ? N1 Cu1 S1 112.6(3) . . ? N2 Cu1 S1 88.7(3) . . ? C9 S1 C8 101.0(4) . . ? C9 S1 Cu1 104.8(3) . . ? C8 S1 Cu1 93.6(3) . . ? C3 N1 C1 109.6(9) . . ? C3 N1 C2 108.1(8) . . ? C1 N1 C2 108.8(9) . . ? C3 N1 Cu1 111.2(5) . . ? C1 N1 Cu1 110.7(8) . . ? C2 N1 Cu1 108.4(6) . . ? C7 N2 C5 110.4(7) . . ? C7 N2 C6 108.7(8) . . ? C5 N2 C6 109.4(8) . . ? C7 N2 Cu1 107.9(5) . . ? C5 N2 Cu1 110.1(5) . . ? C6 N2 Cu1 110.4(7) . . ? C17 N3 Cu1 174(2) . . ? N1 C3 C4 116.7(8) . . ? N1 C3 H3A 108.1 . . ? C4 C3 H3A 108.1 . . ? N1 C3 H3B 108.1 . . ? C4 C3 H3B 108.1 . . ? H3A C3 H3B 107.3 . . ? C3 C4 C5 117.8(10) . . ? C3 C4 H4A 107.9 . . ? C5 C4 H4A 107.9 . . ? C3 C4 H4B 107.9 . . ? C5 C4 H4B 107.9 . . ? H4A C4 H4B 107.2 . . ? N2 C5 C4 115.4(8) . . ? N2 C5 H5A 108.4 . . ? C4 C5 H5A 108.4 . . ? N2 C5 H5B 108.4 . . ? C4 C5 H5B 108.4 . . ? H5A C5 H5B 107.5 . . ? N2 C7 C8 113.1(7) . . ? N2 C7 H7A 109.0 . . ? C8 C7 H7A 109.0 . . ? N2 C7 H7B 109.0 . . ? C8 C7 H7B 109.0 . . ? H7A C7 H7B 107.8 . . ? C19 C8 C7 113.0(9) . . ? C19 C8 S1 111.9(9) . . ? C7 C8 S1 105.6(6) . . ? C19 C8 H8A 108.7 . . ? C7 C8 H8A 108.7 . . ? S1 C8 H8A 108.7 . . ? C10 C9 S1 109.8(6) . . ? C10 C9 H9A 109.7 . . ? S1 C9 H9A 109.7 . . ? C10 C9 H9B 109.7 . . ? S1 C9 H9B 109.7 . . ? H9A C9 H9B 108.2 . . ? C11 C10 C9 110.0(7) . . ? C11 C10 H10A 109.7 . . ? C9 C10 H10A 109.7 . . ? C11 C10 H10B 109.7 . . ? C9 C10 H10B 109.7 . . ? H10A C10 H10B 108.2 . . ? C16 C11 C12 119.2(10) . . ? C16 C11 C10 120.9(10) . . ? C12 C11 C10 119.3(9) . . ? C11 C12 C13 119.1(9) . . ? C11 C12 H12A 120.5 . . ? C13 C12 H12A 120.5 . . ? C14 C13 C12 121.2(10) . . ? C14 C13 H13A 119.4 . . ? C12 C13 H13A 119.4 . . ? C13 C14 C15 118.5(10) . . ? C13 C14 H14A 120.8 . . ? C15 C14 H14A 120.8 . . ? C16 C15 C14 121.4(10) . . ? C16 C15 H15A 119.3 . . ? C14 C15 H15A 119.3 . . ? C15 C16 C11 120.5(10) . . ? C15 C16 H16A 119.8 . . ? C11 C16 H16A 119.8 . . ? N3 C17 C18 171(3) . . ? N3' Cu1' N1' 108.4(8) . . ? N3' Cu1' N2' 110.8(9) . . ? N1' Cu1' N2' 104.0(5) . . ? N3' Cu1' S1' 110.7(8) . . ? N1' Cu1' S1' 130.7(4) . . ? N2' Cu1' S1' 89.1(4) . . ? C9' S1' C8' 99.7(6) . . ? C9' S1' Cu1' 113.8(4) . . ? C8' S1' Cu1' 95.6(4) . . ? C3' N1' C2' 106.8(11) . . ? C3' N1' C1' 108.6(11) . . ? C2' N1' C1' 105.2(10) . . ? C3' N1' Cu1' 112.1(8) . . ? C2' N1' Cu1' 112.8(8) . . ? C1' N1' Cu1' 111.0(10) . . ? C7' N2' C5' 110.1(11) . . ? C7' N2' C6' 109.3(12) . . ? C5' N2' C6' 109.8(11) . . ? C7' N2' Cu1' 107.2(8) . . ? C5' N2' Cu1' 111.1(8) . . ? C6' N2' Cu1' 109.2(10) . . ? C17' N3' Cu1' 162(3) . . ? N1' C1' H1'A 109.5 . . ? N1' C1' H1'B 109.5 . . ? H1'A C1' H1'B 109.5 . . ? N1' C1' H1'C 109.5 . . ? H1'A C1' H1'C 109.5 . . ? H1'B C1' H1'C 109.5 . . ? N1' C2' H2'A 109.5 . . ? N1' C2' H2'B 109.5 . . ? H2'A C2' H2'B 109.5 . . ? N1' C2' H2'C 109.5 . . ? H2'A C2' H2'C 109.5 . . ? H2'B C2' H2'C 109.5 . . ? N1' C3' C4' 114.9(11) . . ? N1' C3' H3'A 108.5 . . ? C4' C3' H3'A 108.5 . . ? N1' C3' H3'B 108.5 . . ? C4' C3' H3'B 108.5 . . ? H3'A C3' H3'B 107.5 . . ? C3' C4' C5' 117.1(17) . . ? C3' C4' H4'A 108.0 . . ? C5' C4' H4'A 108.0 . . ? C3' C4' H4'B 108.0 . . ? C5' C4' H4'B 108.0 . . ? H4'A C4' H4'B 107.3 . . ? N2' C5' C4' 116.4(11) . . ? N2' C5' H5'A 108.2 . . ? C4' C5' H5'A 108.2 . . ? N2' C5' H5'B 108.2 . . ? C4' C5' H5'B 108.2 . . ? H5'A C5' H5'B 107.3 . . ? N2' C6' H6'A 109.5 . . ? N2' C6' H6'B 109.5 . . ? H6'A C6' H6'B 109.5 . . ? N2' C6' H6'C 109.5 . . ? H6'A C6' H6'C 109.5 . . ? H6'B C6' H6'C 109.5 . . ? N2' C7' C8' 115.7(10) . . ? N2' C7' H7'A 108.4 . . ? C8' C7' H7'A 108.4 . . ? N2' C7' H7'B 108.4 . . ? C8' C7' H7'B 108.4 . . ? H7'A C7' H7'B 107.4 . . ? C19' C8' C7' 111.5(14) . . ? C19' C8' S1' 113.5(12) . . ? C7' C8' S1' 106.4(9) . . ? C19' C8' H8'A 108.4 . . ? C7' C8' H8'A 108.4 . . ? S1' C8' H8'A 108.4 . . ? C10' C9' S1' 109.9(7) . . ? C10' C9' H9'A 109.7 . . ? S1' C9' H9'A 109.7 . . ? C10' C9' H9'B 109.7 . . ? S1' C9' H9'B 109.7 . . ? H9'A C9' H9'B 108.2 . . ? C11' C10' C9' 112.5(10) . . ? C11' C10' H10C 109.1 . . ? C9' C10' H10C 109.1 . . ? C11' C10' H10D 109.1 . . ? C9' C10' H10D 109.1 . . ? H10C C10' H10D 107.8 . . ? C12' C11' C16' 118.2(13) . . ? C12' C11' C10' 121.1(11) . . ? C16' C11' C10' 120.6(13) . . ? C11' C12' C13' 122.5(13) . . ? C11' C12' H12B 118.7 . . ? C13' C12' H12B 118.7 . . ? C14' C13' C12' 118.5(14) . . ? C14' C13' H13B 120.7 . . ? C12' C13' H13B 120.7 . . ? C13' C14' C15' 118.5(14) . . ? C13' C14' H14B 120.8 . . ? C15' C14' H14B 120.8 . . ? C16' C15' C14' 123.0(14) . . ? C16' C15' H15B 118.5 . . ? C14' C15' H15B 118.5 . . ? C15' C16' C11' 119.2(15) . . ? C15' C16' H16B 120.4 . . ? C11' C16' H16B 120.4 . . ? N3' C17' C18' 172(4) . . ? C17' C18' H18D 109.5 . . ? C17' C18' H18E 109.5 . . ? H18D C18' H18E 109.5 . . ? C17' C18' H18F 109.5 . . ? H18D C18' H18F 109.5 . . ? H18E C18' H18F 109.5 . . ? C8' C19' H19D 109.5 . . ? C8' C19' H19E 109.5 . . ? H19D C19' H19E 109.5 . . ? C8' C19' H19F 109.5 . . ? H19D C19' H19F 109.5 . . ? H19E C19' H19F 109.5 . . ? C119 B1 C113 102.0(3) . . ? C119 B1 C107 114.6(3) . . ? C113 B1 C107 112.9(3) . . ? C119 B1 C101 113.7(3) . . ? C113 B1 C101 113.6(3) . . ? C107 B1 C101 100.7(3) . . ? C102 C101 C106 112.9(4) . . ? C102 C101 B1 126.3(4) . . ? C106 C101 B1 120.1(4) . . ? F1 C102 C103 114.3(4) . . ? F1 C102 C101 121.3(4) . . ? C103 C102 C101 124.4(4) . . ? F2 C103 C104 119.9(4) . . ? F2 C103 C102 120.7(5) . . ? C104 C103 C102 119.4(4) . . ? F3 C104 C105 120.8(5) . . ? F3 C104 C103 120.2(5) . . ? C105 C104 C103 119.0(4) . . ? F4 C105 C104 119.7(4) . . ? F4 C105 C106 121.2(5) . . ? C104 C105 C106 119.1(5) . . ? F5 C106 C105 116.1(4) . . ? F5 C106 C101 118.7(4) . . ? C105 C106 C101 125.2(4) . . ? C112 C107 C108 112.8(4) . . ? C112 C107 B1 127.2(4) . . ? C108 C107 B1 119.7(4) . . ? F6 C108 C109 116.5(4) . . ? F6 C108 C107 119.0(3) . . ? C109 C108 C107 124.5(4) . . ? F7 C109 C108 120.6(4) . . ? F7 C109 C110 119.4(4) . . ? C108 C109 C110 120.0(4) . . ? F8 C110 C111 120.7(4) . . ? F8 C110 C109 120.8(4) . . ? C111 C110 C109 118.4(4) . . ? F9 C111 C110 119.6(4) . . ? F9 C111 C112 120.4(4) . . ? C110 C111 C112 120.0(4) . . ? F10 C112 C111 114.5(4) . . ? F10 C112 C107 121.2(4) . . ? C111 C112 C107 124.3(4) . . ? C118 C113 C114 113.3(4) . . ? C118 C113 B1 127.4(4) . . ? C114 C113 B1 119.2(4) . . ? F11 C114 C115 115.6(4) . . ? F11 C114 C113 119.7(3) . . ? C115 C114 C113 124.7(4) . . ? F12 C115 C116 120.0(4) . . ? F12 C115 C114 120.4(4) . . ? C116 C115 C114 119.7(4) . . ? F13 C116 C115 121.3(4) . . ? F13 C116 C117 120.3(4) . . ? C115 C116 C117 118.4(4) . . ? F14 C117 C116 119.8(4) . . ? F14 C117 C118 119.8(4) . . ? C116 C117 C118 120.3(4) . . ? F15 C118 C117 115.6(4) . . ? F15 C118 C113 120.8(4) . . ? C117 C118 C113 123.6(4) . . ? C124 C119 C120 112.8(4) . . ? C124 C119 B1 127.5(4) . . ? C120 C119 B1 119.4(4) . . ? F16 C120 C121 115.8(4) . . ? F16 C120 C119 119.4(4) . . ? C121 C120 C119 124.7(4) . . ? F17 C121 C120 120.8(4) . . ? F17 C121 C122 119.4(4) . . ? C120 C121 C122 119.7(4) . . ? F18 C122 C123 120.9(4) . . ? F18 C122 C121 120.9(4) . . ? C123 C122 C121 118.2(4) . . ? F19 C123 C122 119.7(4) . . ? F19 C123 C124 120.0(4) . . ? C122 C123 C124 120.3(4) . . ? F20 C124 C123 114.9(4) . . ? F20 C124 C119 121.0(4) . . ? C123 C124 C119 124.2(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N3 Cu1 S1 C9 8.7(7) . . . . ? N1 Cu1 S1 C9 -127.8(4) . . . . ? N2 Cu1 S1 C9 124.5(4) . . . . ? N3 Cu1 S1 C8 -93.6(8) . . . . ? N1 Cu1 S1 C8 129.9(5) . . . . ? N2 Cu1 S1 C8 22.2(4) . . . . ? N3 Cu1 N1 C3 114.4(9) . . . . ? N2 Cu1 N1 C3 -12.2(7) . . . . ? S1 Cu1 N1 C3 -108.0(6) . . . . ? N3 Cu1 N1 C1 -7.7(11) . . . . ? N2 Cu1 N1 C1 -134.3(8) . . . . ? S1 Cu1 N1 C1 129.9(8) . . . . ? N3 Cu1 N1 C2 -126.9(9) . . . . ? N2 Cu1 N1 C2 106.5(7) . . . . ? S1 Cu1 N1 C2 10.7(7) . . . . ? N3 Cu1 N2 C7 124.7(7) . . . . ? N1 Cu1 N2 C7 -107.8(6) . . . . ? S1 Cu1 N2 C7 5.5(6) . . . . ? N3 Cu1 N2 C5 -114.8(8) . . . . ? N1 Cu1 N2 C5 12.7(7) . . . . ? S1 Cu1 N2 C5 126.0(6) . . . . ? N3 Cu1 N2 C6 6.1(9) . . . . ? N1 Cu1 N2 C6 133.5(8) . . . . ? S1 Cu1 N2 C6 -113.2(7) . . . . ? N1 Cu1 N3 C17 -90(19) . . . . ? N2 Cu1 N3 C17 33(20) . . . . ? S1 Cu1 N3 C17 134(19) . . . . ? C1 N1 C3 C4 161.9(10) . . . . ? C2 N1 C3 C4 -79.7(10) . . . . ? Cu1 N1 C3 C4 39.2(11) . . . . ? N1 C3 C4 C5 -76.0(14) . . . . ? C7 N2 C5 C4 80.2(10) . . . . ? C6 N2 C5 C4 -160.2(10) . . . . ? Cu1 N2 C5 C4 -38.7(10) . . . . ? C3 C4 C5 N2 75.7(14) . . . . ? C5 N2 C7 C8 -161.1(7) . . . . ? C6 N2 C7 C8 78.9(10) . . . . ? Cu1 N2 C7 C8 -40.8(9) . . . . ? N2 C7 C8 C19 -173.8(11) . . . . ? N2 C7 C8 S1 63.5(9) . . . . ? C9 S1 C8 C19 83.1(11) . . . . ? Cu1 S1 C8 C19 -171.0(10) . . . . ? C9 S1 C8 C7 -153.5(6) . . . . ? Cu1 S1 C8 C7 -47.7(6) . . . . ? C8 S1 C9 C10 171.0(7) . . . . ? Cu1 S1 C9 C10 74.3(7) . . . . ? S1 C9 C10 C11 -175.1(7) . . . . ? C9 C10 C11 C16 -71.7(17) . . . . ? C9 C10 C11 C12 99.6(13) . . . . ? C16 C11 C12 C13 -2(2) . . . . ? C10 C11 C12 C13 -173.9(11) . . . . ? C11 C12 C13 C14 4(2) . . . . ? C12 C13 C14 C15 -3(2) . . . . ? C13 C14 C15 C16 -1(4) . . . . ? C14 C15 C16 C11 3(5) . . . . ? C12 C11 C16 C15 -1(3) . . . . ? C10 C11 C16 C15 170(2) . . . . ? Cu1 N3 C17 C18 -124(21) . . . . ? N3' Cu1' S1' C9' 124.7(10) . . . . ? N1' Cu1' S1' C9' -15.5(6) . . . . ? N2' Cu1' S1' C9' -123.3(5) . . . . ? N3' Cu1' S1' C8' -132.2(11) . . . . ? N1' Cu1' S1' C8' 87.6(7) . . . . ? N2' Cu1' S1' C8' -20.2(6) . . . . ? N3' Cu1' N1' C3' 139.1(12) . . . . ? N2' Cu1' N1' C3' 21.1(10) . . . . ? S1' Cu1' N1' C3' -80.0(9) . . . . ? N3' Cu1' N1' C2' -100.2(14) . . . . ? N2' Cu1' N1' C2' 141.8(10) . . . . ? S1' Cu1' N1' C2' 40.7(12) . . . . ? N3' Cu1' N1' C1' 17.5(13) . . . . ? N2' Cu1' N1' C1' -100.5(10) . . . . ? S1' Cu1' N1' C1' 158.4(8) . . . . ? N3' Cu1' N2' C7' 106.3(12) . . . . ? N1' Cu1' N2' C7' -137.4(9) . . . . ? S1' Cu1' N2' C7' -5.5(9) . . . . ? N3' Cu1' N2' C5' -133.4(11) . . . . ? N1' Cu1' N2' C5' -17.1(10) . . . . ? S1' Cu1' N2' C5' 114.8(9) . . . . ? N3' Cu1' N2' C6' -12.0(13) . . . . ? N1' Cu1' N2' C6' 104.3(10) . . . . ? S1' Cu1' N2' C6' -123.8(9) . . . . ? N1' Cu1' N3' C17' 121(11) . . . . ? N2' Cu1' N3' C17' -125(11) . . . . ? S1' Cu1' N3' C17' -28(11) . . . . ? C2' N1' C3' C4' -171.9(14) . . . . ? C1' N1' C3' C4' 75.2(16) . . . . ? Cu1' N1' C3' C4' -47.8(16) . . . . ? N1' C3' C4' C5' 78(2) . . . . ? C7' N2' C5' C4' 157.5(14) . . . . ? C6' N2' C5' C4' -82.0(17) . . . . ? Cu1' N2' C5' C4' 39.0(16) . . . . ? C3' C4' C5' N2' -73(2) . . . . ? C5' N2' C7' C8' -82.4(14) . . . . ? C6' N2' C7' C8' 156.8(13) . . . . ? Cu1' N2' C7' C8' 38.6(14) . . . . ? N2' C7' C8' C19' 176.8(15) . . . . ? N2' C7' C8' S1' -58.9(15) . . . . ? C9' S1' C8' C19' -78.1(16) . . . . ? Cu1' S1' C8' C19' 166.6(15) . . . . ? C9' S1' C8' C7' 158.9(10) . . . . ? Cu1' S1' C8' C7' 43.5(10) . . . . ? C8' S1' C9' C10' -168.2(9) . . . . ? Cu1' S1' C9' C10' -67.7(8) . . . . ? S1' C9' C10' C11' -58.0(12) . . . . ? C9' C10' C11' C12' 108.0(16) . . . . ? C9' C10' C11' C16' -76(2) . . . . ? C16' C11' C12' C13' 3(3) . . . . ? C10' C11' C12' C13' 178.6(18) . . . . ? C11' C12' C13' C14' 0(3) . . . . ? C12' C13' C14' C15' -2(4) . . . . ? C13' C14' C15' C16' 1(6) . . . . ? C14' C15' C16' C11' 3(6) . . . . ? C12' C11' C16' C15' -4(5) . . . . ? C10' C11' C16' C15' 180(3) . . . . ? Cu1' N3' C17' C18' -174(26) . . . . ? C119 B1 C101 C102 20.7(6) . . . . ? C113 B1 C101 C102 136.7(4) . . . . ? C107 B1 C101 C102 -102.3(4) . . . . ? C119 B1 C101 C106 -169.8(3) . . . . ? C113 B1 C101 C106 -53.8(5) . . . . ? C107 B1 C101 C106 67.1(4) . . . . ? C106 C101 C102 F1 -179.5(4) . . . . ? B1 C101 C102 F1 -9.4(6) . . . . ? C106 C101 C102 C103 0.5(6) . . . . ? B1 C101 C102 C103 170.7(4) . . . . ? F1 C102 C103 F2 -0.2(6) . . . . ? C101 C102 C103 F2 179.8(4) . . . . ? F1 C102 C103 C104 178.8(4) . . . . ? C101 C102 C103 C104 -1.2(7) . . . . ? F2 C103 C104 F3 0.9(6) . . . . ? C102 C103 C104 F3 -178.1(4) . . . . ? F2 C103 C104 C105 -179.8(4) . . . . ? C102 C103 C104 C105 1.2(7) . . . . ? F3 C104 C105 F4 -0.5(6) . . . . ? C103 C104 C105 F4 -179.8(4) . . . . ? F3 C104 C105 C106 178.7(4) . . . . ? C103 C104 C105 C106 -0.6(7) . . . . ? F4 C105 C106 F5 0.9(6) . . . . ? C104 C105 C106 F5 -178.3(4) . . . . ? F4 C105 C106 C101 179.2(4) . . . . ? C104 C105 C106 C101 0.0(7) . . . . ? C102 C101 C106 F5 178.3(3) . . . . ? B1 C101 C106 F5 7.5(5) . . . . ? C102 C101 C106 C105 0.1(6) . . . . ? B1 C101 C106 C105 -170.7(4) . . . . ? C119 B1 C107 C112 135.5(4) . . . . ? C113 B1 C107 C112 19.4(6) . . . . ? C101 B1 C107 C112 -102.1(4) . . . . ? C119 B1 C107 C108 -51.9(5) . . . . ? C113 B1 C107 C108 -168.1(3) . . . . ? C101 B1 C107 C108 70.5(4) . . . . ? C112 C107 C108 F6 176.9(3) . . . . ? B1 C107 C108 F6 3.3(5) . . . . ? C112 C107 C108 C109 -1.4(6) . . . . ? B1 C107 C108 C109 -175.0(4) . . . . ? F6 C108 C109 F7 0.3(6) . . . . ? C107 C108 C109 F7 178.6(4) . . . . ? F6 C108 C109 C110 -178.1(4) . . . . ? C107 C108 C109 C110 0.2(6) . . . . ? F7 C109 C110 F8 0.1(6) . . . . ? C108 C109 C110 F8 178.5(4) . . . . ? F7 C109 C110 C111 -176.5(4) . . . . ? C108 C109 C110 C111 1.9(6) . . . . ? F8 C110 C111 F9 1.1(6) . . . . ? C109 C110 C111 F9 177.7(4) . . . . ? F8 C110 C111 C112 -179.3(4) . . . . ? C109 C110 C111 C112 -2.7(6) . . . . ? F9 C111 C112 F10 -0.4(5) . . . . ? C110 C111 C112 F10 -179.9(4) . . . . ? F9 C111 C112 C107 -178.9(4) . . . . ? C110 C111 C112 C107 1.5(6) . . . . ? C108 C107 C112 F10 -177.9(3) . . . . ? B1 C107 C112 F10 -4.9(6) . . . . ? C108 C107 C112 C111 0.5(6) . . . . ? B1 C107 C112 C111 173.6(4) . . . . ? C119 B1 C113 C118 104.1(4) . . . . ? C107 B1 C113 C118 -132.5(4) . . . . ? C101 B1 C113 C118 -18.7(6) . . . . ? C119 B1 C113 C114 -72.6(4) . . . . ? C107 B1 C113 C114 50.8(5) . . . . ? C101 B1 C113 C114 164.7(3) . . . . ? C118 C113 C114 F11 -177.5(3) . . . . ? B1 C113 C114 F11 -0.3(5) . . . . ? C118 C113 C114 C115 2.8(6) . . . . ? B1 C113 C114 C115 179.9(4) . . . . ? F11 C114 C115 F12 -2.2(6) . . . . ? C113 C114 C115 F12 177.6(4) . . . . ? F11 C114 C115 C116 178.1(4) . . . . ? C113 C114 C115 C116 -2.1(7) . . . . ? F12 C115 C116 F13 0.5(6) . . . . ? C114 C115 C116 F13 -179.8(4) . . . . ? F12 C115 C116 C117 179.2(4) . . . . ? C114 C115 C116 C117 -1.1(6) . . . . ? F13 C116 C117 F14 -0.8(6) . . . . ? C115 C116 C117 F14 -179.5(4) . . . . ? F13 C116 C117 C118 -178.0(4) . . . . ? C115 C116 C117 C118 3.3(6) . . . . ? F14 C117 C118 F15 1.0(6) . . . . ? C116 C117 C118 F15 178.2(4) . . . . ? F14 C117 C118 C113 -179.9(4) . . . . ? C116 C117 C118 C113 -2.7(7) . . . . ? C114 C113 C118 F15 178.7(3) . . . . ? B1 C113 C118 F15 1.9(6) . . . . ? C114 C113 C118 C117 -0.4(6) . . . . ? B1 C113 C118 C117 -177.2(4) . . . . ? C113 B1 C119 C124 106.1(4) . . . . ? C107 B1 C119 C124 -16.1(6) . . . . ? C101 B1 C119 C124 -131.2(4) . . . . ? C113 B1 C119 C120 -67.1(4) . . . . ? C107 B1 C119 C120 170.6(4) . . . . ? C101 B1 C119 C120 55.5(5) . . . . ? C124 C119 C120 F16 -178.4(4) . . . . ? B1 C119 C120 F16 -4.2(6) . . . . ? C124 C119 C120 C121 0.9(6) . . . . ? B1 C119 C120 C121 175.1(4) . . . . ? F16 C120 C121 F17 -1.3(6) . . . . ? C119 C120 C121 F17 179.4(4) . . . . ? F16 C120 C121 C122 -179.9(4) . . . . ? C119 C120 C121 C122 0.7(7) . . . . ? F17 C121 C122 F18 0.3(7) . . . . ? C120 C121 C122 F18 179.0(4) . . . . ? F17 C121 C122 C123 -179.7(4) . . . . ? C120 C121 C122 C123 -1.1(7) . . . . ? F18 C122 C123 F19 -0.2(7) . . . . ? C121 C122 C123 F19 179.9(4) . . . . ? F18 C122 C123 C124 179.6(4) . . . . ? C121 C122 C123 C124 -0.3(7) . . . . ? F19 C123 C124 F20 1.5(6) . . . . ? C122 C123 C124 F20 -178.3(4) . . . . ? F19 C123 C124 C119 -178.0(4) . . . . ? C122 C123 C124 C119 2.2(7) . . . . ? C120 C119 C124 F20 178.2(3) . . . . ? B1 C119 C124 F20 4.5(6) . . . . ? C120 C119 C124 C123 -2.4(6) . . . . ? B1 C119 C124 C123 -176.0(4) . . . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.673 _refine_diff_density_min -0.517 _refine_diff_density_rms 0.089 _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'Pbca ' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _exptl_crystal_face_index_h _exptl_crystal_face_index_k _exptl_crystal_face_index_l _exptl_crystal_face_perp_dist -29.00 -1.00 3.00 0.0535 -28.00 0.00 -8.00 0.0643 -3.00 -22.00 -9.00 0.3956 29.00 0.00 -4.00 0.0545 -5.00 -1.00 -37.00 0.1129 5.00 -1.00 37.00 0.1307 -19.00 0.00 29.00 0.0724 28.00 0.00 8.00 0.0672 -20.00 0.00 -27.00 0.0586 2.00 -23.00 0.00 0.4101 2.00 23.00 9.00 0.3347 _audit_creation_date ; 'Thu May 24 09:23:11 2007' ; _audit_creation_method_reference ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_data_collection_reference ; CrysAlis CCD, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_cell_refinment_reference ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _computing_data_reduction_reference ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) ; _cell_measurement_reflns_used 16953 _cell_measurement_theta_min 3.8307 _cell_measurement_theta_max 27.5000 _cell_measurement_resolution_max 0.77 _exptl_crystal_size_max 0.7807 _exptl_crystal_size_mid 0.2529 _exptl_crystal_size_min 0.1232 _exptl_absorpt_coefficient_mu 0.652 _exptl_absorpt_correction_T_min 0.690 _exptl_absorpt_correction_T_max 0.941 _exptl_absorpt_correction_type analytical _exptl_absorpt_process_details ; CrysAlis RED, Oxford Diffraction Ltd., Version 1.171.32.4 (release 27-04-2006 CrysAlis171 .NET) (compiled Apr 27 2007,17:53:11) 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) ; _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_detector_area_resol_mean 15.9890 _diffrn_orient_matrix_UB_11 -0.0059855743 _diffrn_orient_matrix_UB_12 -0.0078978144 _diffrn_orient_matrix_UB_13 -0.0254552119 _diffrn_orient_matrix_UB_21 0.0151394536 _diffrn_orient_matrix_UB_22 -0.0320955875 _diffrn_orient_matrix_UB_23 0.0043631141 _diffrn_orient_matrix_UB_31 -0.0397651304 _diffrn_orient_matrix_UB_32 -0.0110891954 _diffrn_orient_matrix_UB_33 0.0055053357 _diffrn_measurement_details 'see scan set' loop_ _diffrn_scan_number _diffrn_scan_type _diffrn_scan_start _diffrn_scan_end _diffrn_scan_width _diffrn_scan_exptime _diffrn_scan_omega _diffrn_scan_theta _diffrn_scan_kappa _diffrn_scan_phi _diffrn_scan_omega1 _diffrn_scan_theta1 _diffrn_scan_frames 1 omega -29.00 15.00 1.00 60.00 - 22.84 111.00 -123.00 0.00 0.00 44 2 omega -4.00 48.00 1.00 60.00 - 22.84 45.00 120.00 0.00 0.00 52 3 omega 41.00 95.00 1.00 60.00 - 22.84 75.00 0.00 0.00 0.00 54 4 omega -22.00 25.00 1.00 60.00 - 22.84 99.00 156.00 0.00 0.00 47 5 omega -32.00 15.00 1.00 60.00 - -23.46 111.00 37.00 0.00 0.00 47 6 omega -23.00 25.00 1.00 60.00 - -23.46 99.00 128.00 0.00 0.00 48 7 omega -5.00 49.00 1.00 60.00 - -23.46 75.00 120.00 0.00 0.00 54 8 omega -48.00 4.00 1.00 60.00 - -23.46 -45.00 240.00 0.00 0.00 52 _diffrn_measurement_method ' omega scans' _JHU_your_name_here 'Dr. Amy A Sarjeant' _JHU_your_lab_here 'NCB 240' _JHU_your_phone_number_here x6-8569 _JHU_your_email_here xray@jhu.edu _JHU_Institutional_Source 'Karlin Lab' _JHU_Submitting_Scientist 'GaYoung Park' _JHU_Scientist_Phone x6-6161 _JHU_Scientist_EMail gpark8@jhu.edu _JHU_identifying_number x0363 _JHU_xray_labbook II-68 _JHU_crystalization_labbook ANS-BARF _JHU_crystalization_solvent 'Heptane, Ether, Pentane' _diffrn_source_power 2 _diffrn_source_voltage 50 _diffrn_source_current 40 _diffrn_measurement_device Kappa _diffrn_measurement_device_type Xcalibur3 _diffrn_ambient_temperature 110 _JHU_diffraction_detector_distance 50 _JHU_quality_factor 3