# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2003 data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C30 H35 Cl Cu N2 O, C Cl2' _chemical_formula_sum 'C31 H35 Cl3 Cu N2 O' _chemical_formula_weight 621.50 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cu' 'Cu' 0.3201 1.2651 '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' 'O' 'O' 0.0106 0.0060 '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' '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' _symmetry_cell_setting 'triclinic' _symmetry_space_group_name_H-M 'P-1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8538(9) _cell_length_b 13.1058(14) _cell_length_c 13.7598(16) _cell_angle_alpha 88.321(4) _cell_angle_beta 74.910(3) _cell_angle_gamma 77.254(4) _cell_volume 1502.92(3) _cell_formula_units_Z 2 _cell_measurement_temperature -117(2) _cell_measurement_reflns_used 1214 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 23.28 _exptl_crystal_description 'needle' _exptl_crystal_colour green _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.02 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.373 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 646 _exptl_absorpt_coefficient_mu 1.020 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.72 _exptl_absorpt_correction_T_max 0.98 _exptl_absorpt_process_details 'SADABS (Bruker)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 164(2) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6970 _diffrn_reflns_av_R_equivalents 0.0528 _diffrn_reflns_av_sigmaI/netI 0.1852 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 10 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 23.28 _reflns_number_total 4245 _reflns_number_gt 2077 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0770P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4245 _refine_ls_number_parameters 393 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1341 _refine_ls_R_factor_gt 0.0631 _refine_ls_wR_factor_ref 0.1542 _refine_ls_wR_factor_gt 0.1374 _refine_ls_goodness_of_fit_ref 0.841 _refine_ls_restrained_S_all 0.849 _refine_ls_shift/su_max 0.000 _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 0.18591(10) 0.49983(7) 0.70393(7) 0.0302(3) Uani 1 1 d . . . Cl1 Cl 0.2600(2) 0.58982(15) 0.81628(13) 0.0324(5) Uani 1 1 d . . . Cl2 Cl 0.9432(5) 0.1413(4) 0.9044(5) 0.123(2) Uani 0.889(14) 1 d PU A 1 Cl3 Cl 0.982(3) 0.110(4) 0.978(5) 0.134(16) Uani 0.111(14) 1 d PU A 2 Cl4 Cl 0.6587(3) 0.1040(2) 1.0520(2) 0.0876(9) Uani 1 1 d . A 1 O1 O 0.3307(5) 0.3746(3) 0.7042(3) 0.0301(13) Uani 1 1 d . . . N1 N -0.0314(6) 0.5946(4) 0.6998(4) 0.0276(15) Uani 1 1 d . . . N2 N 0.2262(6) 0.4953(4) 0.5600(4) 0.0231(14) Uani 1 1 d . . . C1 C -0.1633(9) 0.6331(6) 0.7722(5) 0.0291(19) Uani 1 1 d . . . C2 C -0.2755(9) 0.7188(6) 0.7487(6) 0.033(2) Uani 1 1 d . . . H1 H -0.3631 0.7511 0.7999 0.039 Uiso 1 1 calc R . . C3 C -0.2598(9) 0.7554(6) 0.6545(6) 0.034(2) Uani 1 1 d . . . H2 H -0.3354 0.8121 0.6418 0.041 Uiso 1 1 calc R . . C4 C -0.1292(9) 0.7076(6) 0.5760(6) 0.0312(19) Uani 1 1 d . . . C5 C -0.0144(9) 0.6271(6) 0.6031(5) 0.0254(18) Uani 1 1 d . . . C6 C 0.1235(8) 0.5767(6) 0.5275(5) 0.0233(18) Uani 1 1 d . . . C7 C 0.1450(9) 0.6038(6) 0.4282(5) 0.0274(19) Uani 1 1 d . . . C8 C 0.0262(9) 0.6869(6) 0.4027(6) 0.035(2) Uani 1 1 d . . . H3 H 0.0395 0.7072 0.3363 0.042 Uiso 1 1 calc R . . C9 C -0.1023(9) 0.7349(6) 0.4732(6) 0.038(2) Uani 1 1 d . . . H4 H -0.1769 0.7882 0.4545 0.045 Uiso 1 1 calc R . . C10 C 0.2840(9) 0.5486(6) 0.3597(5) 0.031(2) Uani 1 1 d . . . H5 H 0.3082 0.5678 0.2928 0.037 Uiso 1 1 calc R . . C11 C 0.3840(8) 0.4671(6) 0.3907(5) 0.0257(18) Uani 1 1 d . . . H6 H 0.4741 0.4300 0.3441 0.031 Uiso 1 1 calc R . . C12 C 0.3529(8) 0.4381(6) 0.4922(5) 0.0238(18) Uani 1 1 d . . . C13 C 0.4505(8) 0.3442(6) 0.5239(5) 0.0257(18) Uani 1 1 d . . . C14 C 0.5634(8) 0.2745(6) 0.4501(5) 0.0280(19) Uani 1 1 d . . . H7 H 0.5784 0.2938 0.3832 0.034 Uiso 1 1 calc R . . C15 C 0.6527(9) 0.1805(6) 0.4696(6) 0.033(2) Uani 1 1 d . B . C16 C 0.6284(9) 0.1563(6) 0.5710(6) 0.036(2) Uani 1 1 d . . . H8 H 0.6864 0.0925 0.5865 0.043 Uiso 1 1 calc R . . C17 C 0.5242(8) 0.2199(6) 0.6517(5) 0.0274(19) Uani 1 1 d . . . C18 C 0.4313(8) 0.3157(6) 0.6280(5) 0.0268(19) Uani 1 1 d . . . C19 C 0.5050(9) 0.1857(6) 0.7599(5) 0.035(2) Uani 1 1 d . . . C20 C 0.6141(10) 0.0792(6) 0.7681(6) 0.052(2) Uani 1 1 d . . . H9 H 0.5918 0.0275 0.7291 0.078 Uiso 1 1 calc R . . H10 H 0.5947 0.0597 0.8373 0.078 Uiso 1 1 calc R . . H11 H 0.7242 0.0836 0.7430 0.078 Uiso 1 1 calc R . . C21 C 0.5469(9) 0.2664(6) 0.8230(5) 0.040(2) Uani 1 1 d . . . H12 H 0.6572 0.2697 0.7963 0.059 Uiso 1 1 calc R . . H13 H 0.5300 0.2454 0.8917 0.059 Uiso 1 1 calc R . . H14 H 0.4795 0.3340 0.8200 0.059 Uiso 1 1 calc R . . C22 C 0.3305(9) 0.1776(6) 0.8081(5) 0.049(2) Uani 1 1 d . . . H15 H 0.2605 0.2453 0.8103 0.073 Uiso 1 1 calc R . . H16 H 0.3211 0.1527 0.8753 0.073 Uiso 1 1 calc R . . H17 H 0.3011 0.1296 0.7687 0.073 Uiso 1 1 calc R . . C23 C 0.7677(8) 0.1043(6) 0.3854(6) 0.037(2) Uani 1 1 d D . . C24 C -0.1931(8) 0.5895(6) 0.8767(5) 0.032(2) Uani 1 1 d . . . C25 C -0.0911(8) 0.4798(6) 0.8814(5) 0.039(2) Uani 1 1 d . . . H18 H -0.1047 0.4344 0.8324 0.059 Uiso 1 1 calc R . . H19 H -0.1244 0.4531 0.9474 0.059 Uiso 1 1 calc R . . H20 H 0.0197 0.4830 0.8675 0.059 Uiso 1 1 calc R . . C26 C -0.1663(8) 0.6650(6) 0.9500(5) 0.041(2) Uani 1 1 d . . . H21 H -0.0569 0.6719 0.9300 0.061 Uiso 1 1 calc R . . H22 H -0.1891 0.6383 1.0167 0.061 Uiso 1 1 calc R . . H23 H -0.2363 0.7323 0.9493 0.061 Uiso 1 1 calc R . . C27 C -0.3726(8) 0.5821(7) 0.9136(5) 0.048(2) Uani 1 1 d . . . H24 H -0.4399 0.6512 0.9212 0.072 Uiso 1 1 calc R . . H25 H -0.3901 0.5484 0.9772 0.072 Uiso 1 1 calc R . . H26 H -0.3981 0.5422 0.8651 0.072 Uiso 1 1 calc R . . C28 C 0.8005(13) 0.1830(9) 1.0188(8) 0.099(4) Uani 1 1 d . . . C29 C 0.708(2) 0.1189(13) 0.2824(10) 0.046(6) Uani 0.531(18) 1 d PD B 3 H27 H 0.7061 0.1892 0.2603 0.069 Uiso 0.531(18) 1 calc PR B 3 H28 H 0.6027 0.1054 0.2951 0.069 Uiso 0.531(18) 1 calc PR B 3 H29 H 0.7811 0.0707 0.2312 0.069 Uiso 0.531(18) 1 calc PR B 3 C30 C 0.9252(15) 0.1366(14) 0.3581(14) 0.052(6) Uani 0.531(18) 1 d PD B 3 H30 H 0.9979 0.0926 0.3035 0.077 Uiso 0.531(18) 1 calc PR B 3 H31 H 0.9694 0.1298 0.4153 0.077 Uiso 0.531(18) 1 calc PR B 3 H32 H 0.9094 0.2081 0.3380 0.077 Uiso 0.531(18) 1 calc PR B 3 C31 C 0.771(2) -0.0069(11) 0.4102(14) 0.036(5) Uani 0.531(18) 1 d PD B 3 H33 H 0.8465 -0.0511 0.3567 0.053 Uiso 0.531(18) 1 calc PR B 3 H34 H 0.6664 -0.0202 0.4184 0.053 Uiso 0.531(18) 1 calc PR B 3 H35 H 0.8031 -0.0212 0.4717 0.053 Uiso 0.531(18) 1 calc PR B 3 C32 C 0.9295(18) 0.0556(18) 0.4254(15) 0.063(9) Uani 0.469(18) 1 d PD B 4 H36 H 1.0108 0.0149 0.3720 0.095 Uiso 0.469(18) 1 calc PR B 4 H37 H 0.9025 0.0119 0.4816 0.095 Uiso 0.469(18) 1 calc PR B 4 H38 H 0.9690 0.1119 0.4459 0.095 Uiso 0.469(18) 1 calc PR B 4 C33 C 0.830(3) 0.1582(16) 0.2921(13) 0.096(13) Uani 0.469(18) 1 d PD B 4 H39 H 0.9001 0.1074 0.2422 0.144 Uiso 0.469(18) 1 calc PR B 4 H40 H 0.8887 0.2068 0.3067 0.144 Uiso 0.469(18) 1 calc PR B 4 H41 H 0.7423 0.1952 0.2672 0.144 Uiso 0.469(18) 1 calc PR B 4 C34 C 0.695(3) 0.0133(16) 0.388(2) 0.066(9) Uani 0.469(18) 1 d PD B 4 H42 H 0.5919 0.0351 0.3738 0.099 Uiso 0.469(18) 1 calc PR B 4 H43 H 0.6818 -0.0165 0.4533 0.099 Uiso 0.469(18) 1 calc PR B 4 H44 H 0.7631 -0.0382 0.3380 0.099 Uiso 0.469(18) 1 calc PR B 4 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 0.0171(5) 0.0424(7) 0.0333(6) -0.0090(5) -0.0106(4) -0.0051(4) Cl1 0.0179(10) 0.0494(14) 0.0336(11) -0.0143(10) -0.0089(9) -0.0101(10) Cl2 0.047(2) 0.199(5) 0.114(4) -0.014(3) -0.008(2) -0.022(3) Cl3 0.028(15) 0.20(3) 0.17(3) -0.01(3) -0.021(19) -0.025(18) Cl4 0.0684(19) 0.093(2) 0.106(2) 0.0107(17) -0.0239(17) -0.0262(17) O1 0.030(3) 0.032(3) 0.029(3) -0.008(2) -0.012(2) -0.002(3) N1 0.016(3) 0.034(4) 0.034(4) -0.014(3) -0.010(3) -0.002(3) N2 0.019(3) 0.022(4) 0.034(4) -0.002(3) -0.012(3) -0.010(3) C1 0.027(5) 0.039(5) 0.029(5) -0.009(4) -0.012(4) -0.018(4) C2 0.026(5) 0.033(5) 0.042(5) -0.007(4) -0.012(4) -0.008(4) C3 0.026(5) 0.031(5) 0.049(5) -0.003(4) -0.017(4) -0.007(4) C4 0.032(5) 0.033(5) 0.039(5) 0.001(4) -0.021(4) -0.015(4) C5 0.032(5) 0.034(5) 0.022(4) -0.002(4) -0.017(4) -0.020(4) C6 0.025(4) 0.025(5) 0.025(4) -0.008(4) -0.006(4) -0.015(4) C7 0.034(5) 0.029(5) 0.026(5) -0.001(4) -0.011(4) -0.015(4) C8 0.034(5) 0.035(5) 0.043(5) -0.001(4) -0.019(4) -0.012(4) C9 0.034(5) 0.039(5) 0.044(5) -0.002(4) -0.020(4) -0.004(4) C10 0.028(5) 0.047(6) 0.024(4) -0.007(4) -0.005(4) -0.023(4) C11 0.014(4) 0.034(5) 0.030(5) -0.008(4) -0.006(4) -0.006(4) C12 0.017(4) 0.031(5) 0.028(4) -0.005(4) -0.005(4) -0.014(4) C13 0.015(4) 0.033(5) 0.034(5) -0.005(4) -0.007(4) -0.015(4) C14 0.028(5) 0.030(5) 0.029(4) 0.001(4) -0.009(4) -0.010(4) C15 0.031(5) 0.026(5) 0.043(5) -0.005(4) -0.008(4) -0.011(4) C16 0.028(5) 0.033(5) 0.052(6) 0.001(5) -0.014(4) -0.012(4) C17 0.024(4) 0.025(5) 0.036(5) -0.004(4) -0.005(4) -0.012(4) C18 0.025(4) 0.027(5) 0.036(5) -0.008(4) -0.012(4) -0.017(4) C19 0.035(5) 0.026(5) 0.041(5) 0.003(4) -0.006(4) -0.006(4) C20 0.059(6) 0.046(6) 0.047(5) 0.001(4) -0.013(5) 0.000(5) C21 0.047(5) 0.045(5) 0.035(5) 0.005(4) -0.018(4) -0.017(4) C22 0.048(6) 0.060(6) 0.044(5) 0.001(4) -0.007(4) -0.029(5) C23 0.028(5) 0.034(6) 0.051(6) -0.014(5) -0.012(4) -0.009(4) C24 0.015(4) 0.044(6) 0.037(5) -0.007(4) -0.004(4) -0.012(4) C25 0.027(5) 0.058(6) 0.035(5) 0.006(4) -0.007(4) -0.015(4) C26 0.020(4) 0.054(6) 0.048(5) -0.016(4) -0.011(4) -0.003(4) C27 0.015(4) 0.082(7) 0.046(5) -0.011(5) -0.005(4) -0.009(4) C28 0.089(9) 0.124(10) 0.088(8) -0.020(7) 0.003(7) -0.062(8) C29 0.036(11) 0.050(12) 0.046(11) -0.024(9) -0.006(9) 0.001(9) C30 0.024(10) 0.057(14) 0.066(15) 0.000(12) 0.001(9) -0.007(10) C31 0.024(11) 0.042(13) 0.040(11) 0.002(9) -0.014(9) 0.001(10) C32 0.032(12) 0.09(2) 0.066(15) -0.033(14) -0.018(11) -0.001(12) C33 0.11(3) 0.08(2) 0.045(15) -0.002(14) 0.014(17) 0.05(2) C34 0.044(17) 0.053(17) 0.10(2) -0.036(14) -0.036(14) 0.016(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.847(4) . ? Cu1 N2 1.919(5) . ? Cu1 N1 2.060(5) . ? Cu1 Cl1 2.2774(19) . ? Cl2 Cl3 1.18(6) . ? Cl2 C28 1.756(11) . ? Cl3 C28 1.64(3) . ? Cl4 C28 1.762(11) . ? O1 C18 1.322(8) . ? N1 C1 1.333(8) . ? N1 C5 1.366(8) . ? N2 C12 1.348(8) . ? N2 C6 1.386(8) . ? C1 C2 1.416(9) . ? C1 C24 1.512(9) . ? C2 C3 1.353(9) . ? C3 C4 1.402(10) . ? C4 C5 1.409(9) . ? C4 C9 1.420(9) . ? C5 C6 1.426(9) . ? C6 C7 1.376(9) . ? C7 C10 1.403(9) . ? C7 C8 1.442(10) . ? C8 C9 1.333(9) . ? C10 C11 1.363(9) . ? C11 C12 1.409(9) . ? C12 C13 1.465(9) . ? C13 C14 1.410(9) . ? C13 C18 1.445(9) . ? C14 C15 1.370(9) . ? C15 C16 1.394(9) . ? C15 C23 1.543(10) . ? C16 C17 1.399(9) . ? C17 C18 1.422(9) . ? C17 C19 1.520(9) . ? C19 C20 1.532(9) . ? C19 C22 1.540(10) . ? C19 C21 1.550(9) . ? C23 C34 1.472(15) . ? C23 C31 1.482(14) . ? C23 C33 1.484(15) . ? C23 C30 1.498(13) . ? C23 C29 1.627(13) . ? C23 C32 1.658(14) . ? C24 C26 1.529(9) . ? C24 C25 1.530(9) . ? C24 C27 1.561(9) . ? C2 H1 0.9300 . ? C3 H2 0.9300 . ? C8 H3 0.9300 . ? C9 H4 0.9300 . ? C10 H5 0.9300 . ? C11 H6 0.9300 . ? C14 H7 0.9300 . ? C16 H8 0.9300 . ? C20 H9 0.9600 . ? C20 H10 0.9600 . ? C20 H11 0.9600 . ? C21 H12 0.9600 . ? C21 H13 0.9600 . ? C21 H14 0.9600 . ? C22 H15 0.9600 . ? C22 H16 0.9600 . ? C22 H17 0.9600 . ? C25 H18 0.9600 . ? C25 H19 0.9600 . ? C25 H20 0.9600 . ? C26 H21 0.9600 . ? C26 H22 0.9600 . ? C26 H23 0.9600 . ? C27 H24 0.9600 . ? C27 H25 0.9600 . ? C27 H26 0.9600 . ? C29 H27 0.9600 . ? C29 H28 0.9600 . ? C29 H29 0.9600 . ? C30 H30 0.9600 . ? C30 H31 0.9600 . ? C30 H32 0.9600 . ? C31 H33 0.9600 . ? C31 H34 0.9600 . ? C31 H35 0.9600 . ? C32 H36 0.9600 . ? C32 H37 0.9600 . ? C32 H38 0.9600 . ? C33 H39 0.9600 . ? C33 H40 0.9600 . ? C33 H41 0.9600 . ? C34 H42 0.9600 . ? C34 H43 0.9600 . ? C34 H44 0.9600 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Cu1 N2 92.7(2) . . ? O1 Cu1 N1 155.9(2) . . ? N2 Cu1 N1 84.4(2) . . ? O1 Cu1 Cl1 97.52(15) . . ? N2 Cu1 Cl1 134.80(17) . . ? N1 Cu1 Cl1 101.49(15) . . ? C18 O1 Cu1 129.8(5) . . ? C1 N1 C5 121.2(6) . . ? C1 N1 Cu1 132.0(5) . . ? C5 N1 Cu1 106.3(4) . . ? C12 N2 C6 119.4(6) . . ? C12 N2 Cu1 128.2(5) . . ? C6 N2 Cu1 111.2(4) . . ? N1 C1 C2 117.6(7) . . ? N1 C1 C24 122.0(7) . . ? C2 C1 C24 120.4(7) . . ? C3 C2 C1 122.3(7) . . ? C2 C3 C4 119.8(7) . . ? C3 C4 C5 116.3(7) . . ? C3 C4 C9 125.6(8) . . ? C5 C4 C9 118.1(7) . . ? N1 C5 C4 122.2(6) . . ? N1 C5 C6 118.5(7) . . ? C4 C5 C6 119.3(7) . . ? C7 C6 N2 123.2(6) . . ? C7 C6 C5 121.2(7) . . ? N2 C6 C5 115.4(6) . . ? C6 C7 C10 116.6(7) . . ? C6 C7 C8 118.2(7) . . ? C10 C7 C8 125.1(7) . . ? C9 C8 C7 120.8(7) . . ? C8 C9 C4 122.3(8) . . ? C11 C10 C7 120.4(7) . . ? C10 C11 C12 121.1(7) . . ? N2 C12 C11 119.0(7) . . ? N2 C12 C13 119.7(6) . . ? C11 C12 C13 121.2(6) . . ? C14 C13 C18 117.5(7) . . ? C14 C13 C12 119.2(6) . . ? C18 C13 C12 123.2(6) . . ? C15 C14 C13 124.8(7) . . ? C14 C15 C16 115.3(7) . . ? C14 C15 C23 122.7(7) . . ? C16 C15 C23 121.9(7) . . ? C15 C16 C17 125.6(7) . . ? C16 C17 C18 117.2(7) . . ? C16 C17 C19 121.5(7) . . ? C18 C17 C19 121.2(6) . . ? O1 C18 C17 117.1(6) . . ? O1 C18 C13 123.4(7) . . ? C17 C18 C13 119.5(6) . . ? C17 C19 C20 112.5(6) . . ? C17 C19 C22 110.3(6) . . ? C20 C19 C22 107.8(7) . . ? C17 C19 C21 110.3(6) . . ? C20 C19 C21 107.5(6) . . ? C22 C19 C21 108.3(6) . . ? C34 C23 C33 124.0(15) . . ? C31 C23 C33 133.8(12) . . ? C34 C23 C30 142.8(12) . . ? C31 C23 C30 116.9(10) . . ? C34 C23 C15 105.6(11) . . ? C31 C23 C15 112.6(9) . . ? C33 C23 C15 112.8(9) . . ? C30 C23 C15 107.5(8) . . ? C31 C23 C29 104.5(10) . . ? C30 C23 C29 104.1(10) . . ? C15 C23 C29 110.8(7) . . ? C34 C23 C32 102.6(11) . . ? C33 C23 C32 103.7(12) . . ? C15 C23 C32 106.3(8) . . ? C29 C23 C32 141.0(9) . . ? C1 C24 C26 109.7(6) . . ? C1 C24 C25 113.4(6) . . ? C26 C24 C25 110.6(6) . . ? C1 C24 C27 109.0(6) . . ? C26 C24 C27 106.7(6) . . ? C25 C24 C27 107.2(6) . . ? Cl3 C28 Cl4 110.4(16) . . ? Cl2 C28 Cl4 112.2(6) . . ? C3 C2 H1 118.8 . . ? C1 C2 H1 118.8 . . ? C2 C3 H2 120.1 . . ? C4 C3 H2 120.1 . . ? C9 C8 H3 119.6 . . ? C7 C8 H3 119.6 . . ? C8 C9 H4 118.9 . . ? C4 C9 H4 118.9 . . ? C11 C10 H5 119.8 . . ? C7 C10 H5 119.8 . . ? C10 C11 H6 119.5 . . ? C12 C11 H6 119.5 . . ? C15 C14 H7 117.6 . . ? C13 C14 H7 117.6 . . ? C15 C16 H8 117.2 . . ? C17 C16 H8 117.2 . . ? C19 C20 H9 109.5 . . ? C19 C20 H10 109.5 . . ? H9 C20 H10 109.5 . . ? C19 C20 H11 109.5 . . ? H9 C20 H11 109.5 . . ? H10 C20 H11 109.5 . . ? C19 C21 H12 109.5 . . ? C19 C21 H13 109.5 . . ? H12 C21 H13 109.5 . . ? C19 C21 H14 109.5 . . ? H12 C21 H14 109.5 . . ? H13 C21 H14 109.5 . . ? C19 C22 H15 109.5 . . ? C19 C22 H16 109.5 . . ? H15 C22 H16 109.5 . . ? C19 C22 H17 109.5 . . ? H15 C22 H17 109.5 . . ? H16 C22 H17 109.5 . . ? C24 C25 H18 109.5 . . ? C24 C25 H19 109.5 . . ? H18 C25 H19 109.5 . . ? C24 C25 H20 109.5 . . ? H18 C25 H20 109.5 . . ? H19 C25 H20 109.5 . . ? C24 C26 H21 109.5 . . ? C24 C26 H22 109.5 . . ? H21 C26 H22 109.5 . . ? C24 C26 H23 109.5 . . ? H21 C26 H23 109.5 . . ? H22 C26 H23 109.5 . . ? C24 C27 H24 109.5 . . ? C24 C27 H25 109.5 . . ? H24 C27 H25 109.5 . . ? C24 C27 H26 109.5 . . ? H24 C27 H26 109.5 . . ? H25 C27 H26 109.5 . . ? C23 C29 H27 109.5 . . ? C23 C29 H28 109.5 . . ? H27 C29 H28 109.5 . . ? C23 C29 H29 109.5 . . ? H27 C29 H29 109.5 . . ? H28 C29 H29 109.5 . . ? C23 C30 H30 109.5 . . ? C23 C30 H31 109.5 . . ? H30 C30 H31 109.5 . . ? C23 C30 H32 109.5 . . ? H30 C30 H32 109.5 . . ? H31 C30 H32 109.5 . . ? C23 C31 H33 109.5 . . ? C23 C31 H34 109.5 . . ? H33 C31 H34 109.5 . . ? C23 C31 H35 109.5 . . ? H33 C31 H35 109.5 . . ? H34 C31 H35 109.5 . . ? C23 C32 H36 109.5 . . ? C23 C32 H37 109.5 . . ? C23 C32 H38 109.5 . . ? C23 C33 H39 109.5 . . ? C23 C33 H40 109.5 . . ? C23 C33 H41 109.5 . . ? C23 C34 H42 109.5 . . ? C23 C34 H43 109.5 . . ? C23 C34 H44 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 N2 Cu1 O1 C18 6.1(6) . . . . ? N1 Cu1 O1 C18 88.1(8) . . . . ? Cl1 Cu1 O1 C18 -129.8(5) . . . . ? O1 Cu1 N1 C1 87.6(8) . . . . ? N2 Cu1 N1 C1 171.5(6) . . . . ? Cl1 Cu1 N1 C1 -53.9(6) . . . . ? O1 Cu1 N1 C5 -100.4(6) . . . . ? N2 Cu1 N1 C5 -16.6(4) . . . . ? Cl1 Cu1 N1 C5 118.0(4) . . . . ? O1 Cu1 N2 C12 -18.6(6) . . . . ? N1 Cu1 N2 C12 -174.6(6) . . . . ? Cl1 Cu1 N2 C12 84.8(6) . . . . ? O1 Cu1 N2 C6 174.4(4) . . . . ? N1 Cu1 N2 C6 18.3(4) . . . . ? Cl1 Cu1 N2 C6 -82.3(5) . . . . ? C5 N1 C1 C2 -8.4(9) . . . . ? Cu1 N1 C1 C2 162.6(5) . . . . ? C5 N1 C1 C24 172.7(6) . . . . ? Cu1 N1 C1 C24 -16.3(10) . . . . ? N1 C1 C2 C3 6.1(10) . . . . ? C24 C1 C2 C3 -175.0(6) . . . . ? C1 C2 C3 C4 0.4(11) . . . . ? C2 C3 C4 C5 -4.4(10) . . . . ? C2 C3 C4 C9 177.0(7) . . . . ? C1 N1 C5 C4 4.5(10) . . . . ? Cu1 N1 C5 C4 -168.6(5) . . . . ? C1 N1 C5 C6 -174.9(6) . . . . ? Cu1 N1 C5 C6 12.1(7) . . . . ? C3 C4 C5 N1 2.2(10) . . . . ? C9 C4 C5 N1 -179.1(6) . . . . ? C3 C4 C5 C6 -178.5(6) . . . . ? C9 C4 C5 C6 0.3(10) . . . . ? C12 N2 C6 C7 -0.8(9) . . . . ? Cu1 N2 C6 C7 167.5(5) . . . . ? C12 N2 C6 C5 174.9(6) . . . . ? Cu1 N2 C6 C5 -16.8(7) . . . . ? N1 C5 C6 C7 178.0(6) . . . . ? C4 C5 C6 C7 -1.3(10) . . . . ? N1 C5 C6 N2 2.2(9) . . . . ? C4 C5 C6 N2 -177.1(6) . . . . ? N2 C6 C7 C10 -3.9(10) . . . . ? C5 C6 C7 C10 -179.4(6) . . . . ? N2 C6 C7 C8 177.2(6) . . . . ? C5 C6 C7 C8 1.8(10) . . . . ? C6 C7 C8 C9 -1.2(10) . . . . ? C10 C7 C8 C9 -179.9(7) . . . . ? C7 C8 C9 C4 0.1(11) . . . . ? C3 C4 C9 C8 179.0(7) . . . . ? C5 C4 C9 C8 0.3(11) . . . . ? C6 C7 C10 C11 5.1(10) . . . . ? C8 C7 C10 C11 -176.1(7) . . . . ? C7 C10 C11 C12 -1.8(10) . . . . ? C6 N2 C12 C11 4.3(9) . . . . ? Cu1 N2 C12 C11 -161.8(5) . . . . ? C6 N2 C12 C13 -172.6(6) . . . . ? Cu1 N2 C12 C13 21.3(9) . . . . ? C10 C11 C12 N2 -3.0(10) . . . . ? C10 C11 C12 C13 173.8(6) . . . . ? N2 C12 C13 C14 168.3(6) . . . . ? C11 C12 C13 C14 -8.4(10) . . . . ? N2 C12 C13 C18 -8.1(10) . . . . ? C11 C12 C13 C18 175.1(6) . . . . ? C18 C13 C14 C15 2.0(10) . . . . ? C12 C13 C14 C15 -174.7(7) . . . . ? C13 C14 C15 C16 -1.4(11) . . . . ? C13 C14 C15 C23 176.5(7) . . . . ? C14 C15 C16 C17 -0.8(11) . . . . ? C23 C15 C16 C17 -178.6(7) . . . . ? C15 C16 C17 C18 2.2(11) . . . . ? C15 C16 C17 C19 179.3(7) . . . . ? Cu1 O1 C18 C17 -177.3(5) . . . . ? Cu1 O1 C18 C13 2.9(9) . . . . ? C16 C17 C18 O1 178.7(6) . . . . ? C19 C17 C18 O1 1.6(10) . . . . ? C16 C17 C18 C13 -1.4(9) . . . . ? C19 C17 C18 C13 -178.6(6) . . . . ? C14 C13 C18 O1 179.4(6) . . . . ? C12 C13 C18 O1 -4.1(10) . . . . ? C14 C13 C18 C17 -0.5(9) . . . . ? C12 C13 C18 C17 176.0(6) . . . . ? C16 C17 C19 C20 1.8(10) . . . . ? C18 C17 C19 C20 178.8(7) . . . . ? C16 C17 C19 C22 -118.6(7) . . . . ? C18 C17 C19 C22 58.4(9) . . . . ? C16 C17 C19 C21 121.8(7) . . . . ? C18 C17 C19 C21 -61.2(8) . . . . ? C14 C15 C23 C34 -111.3(13) . . . . ? C16 C15 C23 C34 66.4(14) . . . . ? C14 C15 C23 C31 -144.0(10) . . . . ? C16 C15 C23 C31 33.7(12) . . . . ? C14 C15 C23 C33 27.2(16) . . . . ? C16 C15 C23 C33 -155.2(15) . . . . ? C14 C15 C23 C30 85.7(12) . . . . ? C16 C15 C23 C30 -96.6(12) . . . . ? C14 C15 C23 C29 -27.4(12) . . . . ? C16 C15 C23 C29 150.3(10) . . . . ? C14 C15 C23 C32 140.2(11) . . . . ? C16 C15 C23 C32 -42.2(13) . . . . ? N1 C1 C24 C26 105.5(7) . . . . ? C2 C1 C24 C26 -73.4(8) . . . . ? N1 C1 C24 C25 -18.7(9) . . . . ? C2 C1 C24 C25 162.5(6) . . . . ? N1 C1 C24 C27 -138.0(7) . . . . ? C2 C1 C24 C27 43.1(9) . . . . ? Cl2 Cl3 C28 Cl4 101(2) . . . . ? Cl3 Cl2 C28 Cl4 -96(2) . . . . ? _diffrn_measured_fraction_theta_max 0.978 _diffrn_reflns_theta_full 23.28 _diffrn_measured_fraction_theta_full 0.978 _refine_diff_density_max 0.584 _refine_diff_density_min -0.951 _refine_diff_density_rms 0.102 data_shelxl _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C31 H35 Cu F3 N2 O4 S' _chemical_formula_sum 'C31 H35 Cu F3 N2 O4 S' _chemical_formula_weight 652.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'Cu' 'Cu' 0.3201 1.2651 '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' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting 'orthorhombic' _symmetry_space_group_name_H-M 'P b c a' _symmetry_space_group_name_Hall '-P 2ac 2ab' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' '-x+1/2, -y, z+1/2' '-x, -y, -z' '-x-1/2, y-1/2, z' 'x, -y-1/2, z-1/2' 'x-1/2, y, -z-1/2' _cell_length_a 14.5486(2) _cell_length_b 14.5834(4) _cell_length_c 28.1825(8) _cell_angle_alpha 90.0000 _cell_angle_beta 90.0000 _cell_angle_gamma 90.0000 _cell_volume 5979.4(2) _cell_formula_units_Z 8 _cell_measurement_temperature 156(2) _cell_measurement_reflns_used 4824 _cell_measurement_theta_min 1.98 _cell_measurement_theta_max 23.26 _exptl_crystal_description 'rectangular plate' _exptl_crystal_colour 'olive-green' _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.05 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.449 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2712 _exptl_absorpt_coefficient_mu 0.858 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_correction_T_min 0.813 _exptl_absorpt_correction_T_max 0.960 _exptl_absorpt_process_details 'SADABS (Bruker)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 156(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 22863 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_sigmaI/netI 0.0667 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.01 _diffrn_reflns_theta_max 23.26 _reflns_number_total 4290 _reflns_number_gt 2805 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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^)+(0.0295P)^2^+0.0000P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4290 _refine_ls_number_parameters 388 _refine_ls_number_restraints 1 _refine_ls_R_factor_all 0.0589 _refine_ls_R_factor_gt 0.0304 _refine_ls_wR_factor_ref 0.0639 _refine_ls_wR_factor_gt 0.0600 _refine_ls_goodness_of_fit_ref 0.875 _refine_ls_restrained_S_all 0.875 _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 0.08404(2) 0.08817(2) 0.630163(12) 0.02328(11) Uani 1 1 d . . . S2 S -0.03736(5) -0.06090(6) 0.66913(3) 0.0270(2) Uani 1 1 d . . . F1 F 0.11032(11) -0.14531(12) 0.70062(7) 0.0432(5) Uani 1 1 d . . . F2 F 0.00568(12) -0.12272(12) 0.75321(6) 0.0441(5) Uani 1 1 d . . . F3 F -0.01228(12) -0.22773(12) 0.70071(6) 0.0454(5) Uani 1 1 d . . . O1 O -0.01184(12) 0.15880(13) 0.60848(7) 0.0250(5) Uani 1 1 d . . . O2 O 0.00594(12) 0.02627(13) 0.68311(6) 0.0257(5) Uani 1 1 d . . . O3 O -0.13170(12) -0.06881(14) 0.68251(7) 0.0362(6) Uani 1 1 d . . . O4 O -0.01252(13) -0.08893(14) 0.62206(6) 0.0339(5) Uani 1 1 d . . . N1 N 0.20010(15) 0.02869(15) 0.65120(8) 0.0199(6) Uani 1 1 d . . . N2 N 0.12702(15) 0.05905(15) 0.56749(8) 0.0182(6) Uani 1 1 d . . . C1 C 0.24362(19) 0.02590(19) 0.69274(10) 0.0216(7) Uani 1 1 d . . . C2 C 0.31177(19) -0.0421(2) 0.70048(11) 0.0255(8) Uani 1 1 d . . . H2 H 0.3407 -0.0463 0.7306 0.031 Uiso 1 1 calc R . . C3 C 0.33614(19) -0.1012(2) 0.66547(11) 0.0248(8) Uani 1 1 d . . . H3 H 0.3812 -0.1468 0.6715 0.030 Uiso 1 1 calc R . . C4 C 0.29526(18) -0.09541(19) 0.62029(10) 0.0208(7) Uani 1 1 d . . . C5 C 0.31928(19) -0.14954(19) 0.58001(11) 0.0257(8) Uani 1 1 d . . . H5 H 0.3642 -0.1964 0.5833 0.031 Uiso 1 1 calc R . . C6 C 0.27937(19) -0.13570(19) 0.53694(11) 0.0252(8) Uani 1 1 d . . . H6 H 0.2960 -0.1736 0.5109 0.030 Uiso 1 1 calc R . . C7 C 0.21212(18) -0.06426(19) 0.53033(10) 0.0199(7) Uani 1 1 d . . . C8 C 0.17002(18) -0.03996(19) 0.48724(10) 0.0217(7) Uani 1 1 d . . . H8 H 0.1825 -0.0746 0.4594 0.026 Uiso 1 1 calc R . . C9 C 0.11141(18) 0.03299(19) 0.48503(10) 0.0201(7) Uani 1 1 d . . . H9 H 0.0847 0.0493 0.4555 0.024 Uiso 1 1 calc R . . C10 C 0.08957(18) 0.08488(19) 0.52612(9) 0.0174(7) Uani 1 1 d . . . C11 C 0.18718(18) -0.01246(18) 0.56977(10) 0.0175(7) Uani 1 1 d . . . C12 C 0.22748(18) -0.02843(19) 0.61508(10) 0.0188(7) Uani 1 1 d . . . C13 C 0.22411(19) 0.0973(2) 0.73090(10) 0.0246(7) Uani 1 1 d . . . C14 C 0.31726(19) 0.1380(2) 0.74674(11) 0.0357(9) Uani 1 1 d . . . H14A H 0.3065 0.1898 0.7682 0.054 Uiso 1 1 calc R . . H14B H 0.3514 0.1591 0.7188 0.054 Uiso 1 1 calc R . . H14C H 0.3530 0.0908 0.7633 0.054 Uiso 1 1 calc R . . C15 C 0.1657(2) 0.1767(2) 0.71231(11) 0.0373(9) Uani 1 1 d . . . H15A H 0.1031 0.1550 0.7061 0.056 Uiso 1 1 calc R . . H15B H 0.1927 0.2003 0.6829 0.056 Uiso 1 1 calc R . . H15C H 0.1639 0.2258 0.7361 0.056 Uiso 1 1 calc R . . C16 C 0.1765(2) 0.0528(2) 0.77374(10) 0.0344(9) Uani 1 1 d . . . H16A H 0.1164 0.0290 0.7641 0.052 Uiso 1 1 calc R . . H16B H 0.1684 0.0986 0.7988 0.052 Uiso 1 1 calc R . . H16C H 0.2145 0.0022 0.7856 0.052 Uiso 1 1 calc R . . C17 C 0.02959(18) 0.16597(19) 0.52526(10) 0.0165(7) Uani 1 1 d . . . C18 C 0.02223(18) 0.21384(19) 0.48219(10) 0.0188(7) Uani 1 1 d . . . H18 H 0.0562 0.1928 0.4555 0.023 Uiso 1 1 calc R . . C19 C -0.03282(19) 0.29062(19) 0.47733(10) 0.0188(7) Uani 1 1 d . . . C20 C -0.08536(19) 0.31471(19) 0.51684(10) 0.0219(7) Uani 1 1 d . . . H20 H -0.1267 0.3647 0.5135 0.026 Uiso 1 1 calc R . . C21 C -0.08187(19) 0.27137(18) 0.56057(9) 0.0185(7) Uani 1 1 d . . . C22 C -0.01898(18) 0.19675(19) 0.56587(10) 0.0186(7) Uani 1 1 d . . . C23 C -0.03920(19) 0.34488(19) 0.43085(10) 0.0216(7) Uani 1 1 d U . . C24 C -0.0488(2) 0.4476(2) 0.44032(11) 0.0381(9) Uani 1 1 d . . . H24A H -0.0483 0.4809 0.4101 0.057 Uiso 1 1 calc R . . H24B H 0.0027 0.4684 0.4600 0.057 Uiso 1 1 calc R . . H24C H -0.1068 0.4594 0.4569 0.057 Uiso 1 1 calc R . . C25 C -0.1239(2) 0.3118(2) 0.40301(11) 0.0416(9) Uani 1 1 d U . . H25A H -0.1296 0.3473 0.3736 0.062 Uiso 1 1 calc R . . H25B H -0.1792 0.3205 0.4224 0.062 Uiso 1 1 calc R . . H25C H -0.1169 0.2467 0.3953 0.062 Uiso 1 1 calc R . . C26 C 0.0460(2) 0.3323(2) 0.40029(11) 0.0363(9) Uani 1 1 d . . . H26A H 0.0524 0.2675 0.3918 0.055 Uiso 1 1 calc R . . H26B H 0.1003 0.3523 0.4180 0.055 Uiso 1 1 calc R . . H26C H 0.0400 0.3692 0.3714 0.055 Uiso 1 1 calc R . . C27 C -0.14361(19) 0.3023(2) 0.60193(10) 0.0230(8) Uani 1 1 d . . . C28 C -0.20473(19) 0.2223(2) 0.61847(10) 0.0332(9) Uani 1 1 d . . . H28A H -0.2447 0.2432 0.6443 0.050 Uiso 1 1 calc R . . H28B H -0.1659 0.1720 0.6298 0.050 Uiso 1 1 calc R . . H28C H -0.2425 0.2010 0.5919 0.050 Uiso 1 1 calc R . . C29 C -0.2079(2) 0.3806(2) 0.58782(11) 0.0397(9) Uani 1 1 d . . . H29A H -0.2457 0.3981 0.6151 0.060 Uiso 1 1 calc R . . H29B H -0.2478 0.3605 0.5618 0.060 Uiso 1 1 calc R . . H29C H -0.1714 0.4334 0.5775 0.060 Uiso 1 1 calc R . . C30 C -0.0853(2) 0.3361(2) 0.64390(10) 0.0323(8) Uani 1 1 d . . . H30A H -0.0484 0.3889 0.6339 0.048 Uiso 1 1 calc R . . H30B H -0.0446 0.2867 0.6545 0.048 Uiso 1 1 calc R . . H30C H -0.1258 0.3543 0.6700 0.048 Uiso 1 1 calc R . . C31 C 0.0199(2) -0.1434(2) 0.70761(11) 0.0300(8) 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 0.0245(2) 0.0265(2) 0.0188(2) 0.00176(19) 0.00046(18) 0.00765(19) S2 0.0274(5) 0.0347(5) 0.0188(4) 0.0014(4) 0.0006(4) 0.0028(4) F1 0.0303(11) 0.0418(12) 0.0575(14) 0.0159(10) 0.0048(10) 0.0074(9) F2 0.0524(12) 0.0561(13) 0.0239(11) 0.0083(10) -0.0023(9) 0.0044(10) F3 0.0553(13) 0.0332(12) 0.0476(13) 0.0096(10) -0.0013(10) -0.0073(10) O1 0.0272(12) 0.0310(13) 0.0169(12) 0.0056(10) 0.0035(10) 0.0131(10) O2 0.0282(12) 0.0256(12) 0.0232(12) 0.0020(10) 0.0012(10) 0.0040(10) O3 0.0210(12) 0.0538(16) 0.0338(14) -0.0014(12) 0.0010(10) -0.0021(11) O4 0.0473(13) 0.0372(13) 0.0173(13) -0.0011(10) 0.0040(10) 0.0016(12) N1 0.0212(14) 0.0168(14) 0.0218(15) 0.0036(12) -0.0003(12) 0.0006(12) N2 0.0177(13) 0.0189(15) 0.0180(15) 0.0013(11) -0.0001(11) 0.0015(12) C1 0.0210(17) 0.0227(19) 0.0210(19) 0.0064(15) 0.0000(15) -0.0043(15) C2 0.0218(18) 0.029(2) 0.0261(19) 0.0077(16) -0.0042(15) 0.0000(16) C3 0.0187(17) 0.0177(19) 0.038(2) 0.0091(16) -0.0011(16) 0.0025(14) C4 0.0174(16) 0.0162(17) 0.029(2) 0.0051(16) 0.0014(14) -0.0011(15) C5 0.0200(17) 0.0151(18) 0.042(2) 0.0013(16) 0.0040(17) 0.0053(14) C6 0.0275(19) 0.0162(18) 0.032(2) -0.0037(15) 0.0074(16) 0.0006(15) C7 0.0167(16) 0.0181(19) 0.0251(19) 0.0000(15) 0.0036(14) -0.0032(14) C8 0.0211(18) 0.0212(19) 0.0228(19) -0.0067(15) 0.0031(15) -0.0028(15) C9 0.0203(18) 0.0224(19) 0.0175(18) 0.0022(15) 0.0006(14) -0.0040(14) C10 0.0151(15) 0.0183(17) 0.0187(17) -0.0001(15) 0.0036(14) -0.0064(15) C11 0.0125(15) 0.0170(18) 0.0229(19) 0.0010(14) 0.0026(14) -0.0001(14) C12 0.0160(16) 0.0169(18) 0.0235(19) 0.0014(15) 0.0035(14) -0.0030(14) C13 0.0294(18) 0.0229(18) 0.0215(18) 0.0012(15) -0.0033(15) 0.0032(16) C14 0.043(2) 0.033(2) 0.031(2) -0.0016(17) -0.0037(17) -0.0083(17) C15 0.054(2) 0.028(2) 0.030(2) -0.0070(16) -0.0096(18) 0.0090(18) C16 0.037(2) 0.038(2) 0.028(2) -0.0035(16) 0.0028(17) -0.0013(17) C17 0.0153(16) 0.0173(18) 0.0168(18) -0.0008(14) -0.0017(14) -0.0001(14) C18 0.0176(17) 0.0246(19) 0.0140(17) -0.0037(14) 0.0017(14) 0.0002(15) C19 0.0192(17) 0.0214(19) 0.0157(18) -0.0019(14) -0.0009(14) -0.0011(15) C20 0.0185(16) 0.0214(18) 0.0258(19) -0.0004(15) -0.0045(16) 0.0049(15) C21 0.0178(16) 0.0221(17) 0.0156(17) -0.0029(14) -0.0006(15) 0.0012(15) C22 0.0149(16) 0.0215(18) 0.0193(19) -0.0001(14) -0.0019(14) -0.0034(14) C23 0.0225(17) 0.0207(19) 0.0215(18) 0.0018(14) -0.0004(15) 0.0035(14) C24 0.055(2) 0.031(2) 0.029(2) 0.0096(16) 0.0065(18) 0.0067(17) C25 0.042(2) 0.055(2) 0.027(2) 0.0137(19) -0.0061(17) -0.0049(19) C26 0.042(2) 0.038(2) 0.030(2) 0.0119(17) 0.0089(17) 0.0088(17) C27 0.0229(18) 0.028(2) 0.0177(18) -0.0020(15) 0.0000(15) 0.0077(15) C28 0.0237(18) 0.048(2) 0.028(2) -0.0023(17) 0.0072(15) 0.0007(17) C29 0.045(2) 0.050(2) 0.025(2) 0.0045(17) 0.0099(17) 0.0291(18) C30 0.0335(19) 0.038(2) 0.025(2) -0.0079(15) 0.0032(16) 0.0045(18) C31 0.038(2) 0.029(2) 0.023(2) 0.0039(16) 0.0022(17) -0.0037(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O1 1.8384(18) . ? Cu1 N2 1.921(2) . ? Cu1 N1 1.989(2) . ? Cu1 O2 2.0816(19) . ? S2 O3 1.4280(19) . ? S2 O4 1.4345(19) . ? S2 O2 1.4724(19) . ? S2 C31 1.821(3) . ? F1 C31 1.331(3) . ? F2 C31 1.336(3) . ? F3 C31 1.330(3) . ? O1 C22 1.326(3) . ? N1 C1 1.331(3) . ? N1 C12 1.374(3) . ? N2 C10 1.341(3) . ? N2 C11 1.363(3) . ? C1 C2 1.419(4) . ? C1 C13 1.524(4) . ? C2 C3 1.357(4) . ? C2 H2 0.9500 . ? C3 C4 1.408(4) . ? C3 H3 0.9500 . ? C4 C12 1.396(4) . ? C4 C5 1.426(4) . ? C5 C6 1.360(4) . ? C5 H5 0.9500 . ? C6 C7 1.441(4) . ? C6 H6 0.9500 . ? C7 C11 1.392(4) . ? C7 C8 1.405(4) . ? C8 C9 1.365(4) . ? C8 H8 0.9500 . ? C9 C10 1.419(4) . ? C9 H9 0.9500 . ? C10 C17 1.470(4) . ? C11 C12 1.424(4) . ? C13 C15 1.528(4) . ? C13 C16 1.536(4) . ? C13 C14 1.545(4) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 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 C18 1.404(4) . ? C17 C22 1.418(4) . ? C18 C19 1.384(3) . ? C18 H18 0.9500 . ? C19 C20 1.396(4) . ? C19 C23 1.533(4) . ? C20 C21 1.386(4) . ? C20 H20 0.9500 . ? C21 C22 1.430(4) . ? C21 C27 1.539(4) . ? C23 C26 1.520(4) . ? C23 C24 1.528(4) . ? C23 C25 1.538(4) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 H25A 0.9800 . ? C25 H25B 0.9800 . ? C25 H25C 0.9800 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 C29 1.528(4) . ? C27 C30 1.537(4) . ? C27 C28 1.539(4) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 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 O1 Cu1 N2 93.74(9) . . ? O1 Cu1 N1 170.98(9) . . ? N2 Cu1 N1 84.34(9) . . ? O1 Cu1 O2 93.84(8) . . ? N2 Cu1 O2 137.80(9) . . ? N1 Cu1 O2 93.47(8) . . ? O3 S2 O4 117.60(13) . . ? O3 S2 O2 114.23(12) . . ? O4 S2 O2 112.69(12) . . ? O3 S2 C31 103.24(14) . . ? O4 S2 C31 104.31(14) . . ? O2 S2 C31 102.44(13) . . ? C22 O1 Cu1 126.45(17) . . ? S2 O2 Cu1 114.59(11) . . ? C1 N1 C12 119.7(2) . . ? C1 N1 Cu1 132.8(2) . . ? C12 N1 Cu1 106.83(18) . . ? C10 N2 C11 121.1(2) . . ? C10 N2 Cu1 127.24(18) . . ? C11 N2 Cu1 109.55(18) . . ? N1 C1 C2 119.3(3) . . ? N1 C1 C13 120.7(3) . . ? C2 C1 C13 120.0(3) . . ? C3 C2 C1 120.9(3) . . ? C3 C2 H2 119.5 . . ? C1 C2 H2 119.5 . . ? C2 C3 C4 120.6(3) . . ? C2 C3 H3 119.7 . . ? C4 C3 H3 119.7 . . ? C12 C4 C3 115.8(3) . . ? C12 C4 C5 118.5(3) . . ? C3 C4 C5 125.7(3) . . ? C6 C5 C4 121.6(3) . . ? C6 C5 H5 119.2 . . ? C4 C5 H5 119.2 . . ? C5 C6 C7 120.8(3) . . ? C5 C6 H6 119.6 . . ? C7 C6 H6 119.6 . . ? C11 C7 C8 116.1(3) . . ? C11 C7 C6 117.8(3) . . ? C8 C7 C6 126.1(3) . . ? C9 C8 C7 120.5(3) . . ? C9 C8 H8 119.7 . . ? C7 C8 H8 119.7 . . ? C8 C9 C10 121.2(3) . . ? C8 C9 H9 119.4 . . ? C10 C9 H9 119.4 . . ? N2 C10 C9 118.0(3) . . ? N2 C10 C17 118.8(2) . . ? C9 C10 C17 123.3(2) . . ? N2 C11 C7 123.0(3) . . ? N2 C11 C12 115.6(2) . . ? C7 C11 C12 121.3(3) . . ? N1 C12 C4 123.4(3) . . ? N1 C12 C11 116.5(2) . . ? C4 C12 C11 120.0(3) . . ? C1 C13 C15 112.3(2) . . ? C1 C13 C16 110.4(2) . . ? C15 C13 C16 109.9(2) . . ? C1 C13 C14 107.6(2) . . ? C15 C13 C14 107.2(2) . . ? C16 C13 C14 109.3(2) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C22 120.1(3) . . ? C18 C17 C10 117.3(2) . . ? C22 C17 C10 122.5(2) . . ? C19 C18 C17 122.1(3) . . ? C19 C18 H18 118.9 . . ? C17 C18 H18 118.9 . . ? C18 C19 C20 116.2(3) . . ? C18 C19 C23 122.5(2) . . ? C20 C19 C23 121.2(2) . . ? C21 C20 C19 125.1(3) . . ? C21 C20 H20 117.5 . . ? C19 C20 H20 117.5 . . ? C20 C21 C22 117.6(3) . . ? C20 C21 C27 121.2(3) . . ? C22 C21 C27 121.2(2) . . ? O1 C22 C17 124.0(2) . . ? O1 C22 C21 117.5(2) . . ? C17 C22 C21 118.4(3) . . ? C26 C23 C24 106.9(2) . . ? C26 C23 C19 111.9(2) . . ? C24 C23 C19 111.2(2) . . ? C26 C23 C25 109.0(2) . . ? C24 C23 C25 108.9(2) . . ? C19 C23 C25 108.8(2) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C30 107.3(2) . . ? C29 C27 C28 106.9(2) . . ? C30 C27 C28 109.2(2) . . ? C29 C27 C21 112.3(2) . . ? C30 C27 C21 110.8(2) . . ? C28 C27 C21 110.2(2) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? F3 C31 F1 107.9(3) . . ? F3 C31 F2 107.2(2) . . ? F1 C31 F2 107.5(3) . . ? F3 C31 S2 111.3(2) . . ? F1 C31 S2 112.2(2) . . ? F2 C31 S2 110.7(2) . . ? 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 N2 Cu1 O1 C22 -20.2(2) . . . . ? O2 Cu1 O1 C22 -158.6(2) . . . . ? O3 S2 O2 Cu1 -134.21(12) . . . . ? O4 S2 O2 Cu1 3.41(16) . . . . ? C31 S2 O2 Cu1 114.91(14) . . . . ? O1 Cu1 O2 S2 92.67(12) . . . . ? N2 Cu1 O2 S2 -7.20(19) . . . . ? N1 Cu1 O2 S2 -92.60(13) . . . . ? N2 Cu1 N1 C1 167.7(3) . . . . ? O2 Cu1 N1 C1 -54.5(3) . . . . ? N2 Cu1 N1 C12 -22.38(17) . . . . ? O2 Cu1 N1 C12 115.33(17) . . . . ? O1 Cu1 N2 C10 -1.8(2) . . . . ? N1 Cu1 N2 C10 -173.0(2) . . . . ? O2 Cu1 N2 C10 98.1(2) . . . . ? O1 Cu1 N2 C11 -165.35(17) . . . . ? N1 Cu1 N2 C11 23.49(18) . . . . ? O2 Cu1 N2 C11 -65.4(2) . . . . ? C12 N1 C1 C2 -6.0(4) . . . . ? Cu1 N1 C1 C2 162.8(2) . . . . ? C12 N1 C1 C13 171.2(2) . . . . ? Cu1 N1 C1 C13 -20.0(4) . . . . ? N1 C1 C2 C3 3.2(4) . . . . ? C13 C1 C2 C3 -174.0(3) . . . . ? C1 C2 C3 C4 1.0(4) . . . . ? C2 C3 C4 C12 -2.2(4) . . . . ? C2 C3 C4 C5 175.8(3) . . . . ? C12 C4 C5 C6 1.6(4) . . . . ? C3 C4 C5 C6 -176.3(3) . . . . ? C4 C5 C6 C7 1.1(4) . . . . ? C5 C6 C7 C11 -2.3(4) . . . . ? C5 C6 C7 C8 176.2(3) . . . . ? C11 C7 C8 C9 2.6(4) . . . . ? C6 C7 C8 C9 -175.9(3) . . . . ? C7 C8 C9 C10 -1.5(4) . . . . ? C11 N2 C10 C9 2.7(4) . . . . ? Cu1 N2 C10 C9 -159.13(19) . . . . ? C11 N2 C10 C17 -176.3(2) . . . . ? Cu1 N2 C10 C17 21.9(3) . . . . ? C8 C9 C10 N2 -1.2(4) . . . . ? C8 C9 C10 C17 177.7(3) . . . . ? C10 N2 C11 C7 -1.5(4) . . . . ? Cu1 N2 C11 C7 163.2(2) . . . . ? C10 N2 C11 C12 175.3(2) . . . . ? Cu1 N2 C11 C12 -20.0(3) . . . . ? C8 C7 C11 N2 -1.2(4) . . . . ? C6 C7 C11 N2 177.4(2) . . . . ? C8 C7 C11 C12 -177.8(2) . . . . ? C6 C7 C11 C12 0.8(4) . . . . ? C1 N1 C12 C4 4.9(4) . . . . ? Cu1 N1 C12 C4 -166.6(2) . . . . ? C1 N1 C12 C11 -171.0(2) . . . . ? Cu1 N1 C12 C11 17.5(3) . . . . ? C3 C4 C12 N1 -0.7(4) . . . . ? C5 C4 C12 N1 -178.8(2) . . . . ? C3 C4 C12 C11 175.1(2) . . . . ? C5 C4 C12 C11 -3.0(4) . . . . ? N2 C11 C12 N1 1.1(4) . . . . ? C7 C11 C12 N1 177.9(2) . . . . ? N2 C11 C12 C4 -175.0(2) . . . . ? C7 C11 C12 C4 1.8(4) . . . . ? N1 C1 C13 C15 -10.3(4) . . . . ? C2 C1 C13 C15 166.9(3) . . . . ? N1 C1 C13 C16 112.7(3) . . . . ? C2 C1 C13 C16 -70.1(3) . . . . ? N1 C1 C13 C14 -128.0(3) . . . . ? C2 C1 C13 C14 49.1(3) . . . . ? N2 C10 C17 C18 154.2(2) . . . . ? C9 C10 C17 C18 -24.7(4) . . . . ? N2 C10 C17 C22 -25.2(4) . . . . ? C9 C10 C17 C22 156.0(3) . . . . ? C22 C17 C18 C19 -1.1(4) . . . . ? C10 C17 C18 C19 179.5(2) . . . . ? C17 C18 C19 C20 -3.9(4) . . . . ? C17 C18 C19 C23 178.2(2) . . . . ? C18 C19 C20 C21 4.2(4) . . . . ? C23 C19 C20 C21 -177.9(3) . . . . ? C19 C20 C21 C22 0.7(4) . . . . ? C19 C20 C21 C27 -179.2(3) . . . . ? Cu1 O1 C22 C17 21.6(4) . . . . ? Cu1 O1 C22 C21 -160.45(18) . . . . ? C18 C17 C22 O1 -176.0(2) . . . . ? C10 C17 C22 O1 3.3(4) . . . . ? C18 C17 C22 C21 6.1(4) . . . . ? C10 C17 C22 C21 -174.6(2) . . . . ? C20 C21 C22 O1 176.2(2) . . . . ? C27 C21 C22 O1 -3.9(4) . . . . ? C20 C21 C22 C17 -5.8(4) . . . . ? C27 C21 C22 C17 174.1(2) . . . . ? C18 C19 C23 C26 -24.3(4) . . . . ? C20 C19 C23 C26 158.0(3) . . . . ? C18 C19 C23 C24 -143.8(3) . . . . ? C20 C19 C23 C24 38.5(4) . . . . ? C18 C19 C23 C25 96.3(3) . . . . ? C20 C19 C23 C25 -81.5(3) . . . . ? C20 C21 C27 C29 2.1(4) . . . . ? C22 C21 C27 C29 -177.8(2) . . . . ? C20 C21 C27 C30 -117.9(3) . . . . ? C22 C21 C27 C30 62.2(3) . . . . ? C20 C21 C27 C28 121.1(3) . . . . ? C22 C21 C27 C28 -58.7(3) . . . . ? O3 S2 C31 F3 59.7(2) . . . . ? O4 S2 C31 F3 -63.7(2) . . . . ? O2 S2 C31 F3 178.6(2) . . . . ? O3 S2 C31 F1 -179.3(2) . . . . ? O4 S2 C31 F1 57.2(3) . . . . ? O2 S2 C31 F1 -60.4(2) . . . . ? O3 S2 C31 F2 -59.3(2) . . . . ? O4 S2 C31 F2 177.3(2) . . . . ? O2 S2 C31 F2 59.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 23.26 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 0.286 _refine_diff_density_min -0.356 _refine_diff_density_rms 0.050