# Electronic Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_aa #TrackingRef '01-2acetone.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C161 H142 Cl28 Cu3 N12 O54' _chemical_formula_weight 4292.09 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting Trigonal _symmetry_space_group_name_H-M P-3c1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-y, x-y, z' '-x+y, -x, z' 'y, x, -z+1/2' 'x-y, -y, -z+1/2' '-x, -x+y, -z+1/2' '-x, -y, -z' 'y, -x+y, -z' 'x-y, x, -z' '-y, -x, z-1/2' '-x+y, y, z-1/2' 'x, x-y, z-1/2' _cell_length_a 22.6009(4) _cell_length_b 22.6009(4) _cell_length_c 22.3136(6) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 120.00 _cell_volume 9870.8(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 1458 _cell_measurement_theta_min 2.75 _cell_measurement_theta_max 16.86 _exptl_crystal_description BLOCK _exptl_crystal_colour purple _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.444 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4374 _exptl_absorpt_coefficient_mu 0.779 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7561 _exptl_absorpt_correction_T_max 0.8473 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker Breeze CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 49309 _diffrn_reflns_av_R_equivalents 0.1777 _diffrn_reflns_av_sigmaI/netI 0.1267 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -26 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.80 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6472 _reflns_number_gt 2794 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1677P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6472 _refine_ls_number_parameters 413 _refine_ls_number_restraints 21 _refine_ls_R_factor_all 0.2036 _refine_ls_R_factor_gt 0.0917 _refine_ls_wR_factor_ref 0.3174 _refine_ls_wR_factor_gt 0.2457 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 4.271 _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 0.5051(2) 0.0000 0.2500 0.0373(16) Uani 1 2 d S . . Cl1 Cl 0.4138(8) 0.2019(6) 0.7176(5) 0.094(4) Uani 1 1 d . . . Cl2 Cl 0.6667 0.3333 0.0978(12) 0.098(7) Uani 1 3 d S . . Cl3 Cl 0.617(3) 0.302(3) 0.217(3) 0.17(3) Uani 0.33 1 d P . . Cl4 Cl 0.6429(10) 0.1108(8) -0.0401(7) 0.145(7) Uani 1 1 d . . . Cl5 Cl 0.5736(7) 0.0007(5) 0.0425(5) 0.091(4) Uani 1 1 d . . . Cl6 Cl 0.796(4) 0.891(3) 0.296(4) 0.31(4) Uani 0.50 1 d PD . . Cl7 Cl 0.882(3) 1.032(3) 0.313(6) 0.52(11) Uani 0.50 1 d PD . . O1 O 0.7187(12) 0.2440(11) 0.4301(11) 0.056(6) Uani 1 1 d . . . O2 O 0.7084(10) 0.1422(10) 0.4079(9) 0.041(5) Uani 1 1 d . . . O3 O 0.6790(12) 0.0545(12) 0.5751(10) 0.056(6) Uani 1 1 d . . . O4 O 0.7020(11) 0.1528(11) 0.5301(10) 0.049(6) Uani 1 1 d . . . O5 O 0.6111(13) 0.0000 0.2500 0.046(8) Uani 1 2 d S . . O6 O 0.3904(14) 0.0000 0.2500 0.051(8) Uani 1 2 d S . . O7 O 0.417(2) 0.2597(16) 0.7004(19) 0.149(17) Uani 1 1 d D A . O8 O 0.3954(18) 0.1506(15) 0.6769(15) 0.103(11) Uani 1 1 d . A . O9 O 0.437(4) 0.195(2) 0.770(2) 0.24(4) Uani 1 1 d . A . O10 O 0.331(5) 0.163(5) 0.743(5) 0.17(4) Uani 0.50 1 d PU A 1 O10' O 0.497(4) 0.245(6) 0.702(5) 0.22(5) Uani 0.50 1 d PDU A 2 N1 N 0.5447(12) 0.0875(12) 0.2975(11) 0.038(6) Uani 1 1 d . . . N2 N 0.5269(13) 0.0575(12) 0.6752(11) 0.040(6) Uani 1 1 d . . . C1 C 0.5202(17) 0.1310(16) 0.2917(15) 0.048(8) Uani 1 1 d . . . H1 H 0.4831 0.1191 0.2651 0.058 Uiso 1 1 calc R . . C2 C 0.5468(18) 0.1918(18) 0.3226(16) 0.056(10) Uani 1 1 d . . . H2 H 0.5278 0.2207 0.3178 0.068 Uiso 1 1 calc R . . C3 C 0.6005(16) 0.2098(17) 0.3602(16) 0.051(9) Uani 1 1 d . . . H3 H 0.6188 0.2512 0.3824 0.061 Uiso 1 1 calc R . . C4 C 0.6286(15) 0.1678(15) 0.3662(14) 0.041(8) Uani 1 1 d . . . C5 C 0.5986(15) 0.1064(15) 0.3352(13) 0.039(7) Uani 1 1 d . . . H5 H 0.6163 0.0764 0.3405 0.047 Uiso 1 1 calc R . . C6 C 0.6896(16) 0.1907(16) 0.4050(14) 0.040(8) Uani 1 1 d . . . C7 C 0.7651(16) 0.1561(15) 0.4424(14) 0.039(7) Uani 1 1 d . . . C8 C 0.8218(16) 0.1636(15) 0.4159(16) 0.046(8) Uani 1 1 d . . . H8 H 0.8243 0.1629 0.3734 0.055 Uiso 1 1 calc R . . C9 C 0.8780(16) 0.1724(16) 0.4509(18) 0.050(9) Uani 1 1 d . . . C10 C 0.9385(18) 0.1793(19) 0.425(2) 0.073(12) Uani 1 1 d . . . H10 H 0.9413 0.1771 0.3824 0.087 Uiso 1 1 calc R . . C11 C 0.992(2) 0.189(2) 0.458(3) 0.097(16) Uani 1 1 d . . . H11 H 1.0316 0.1926 0.4403 0.117 Uiso 1 1 calc R . . C12 C 0.988(2) 0.193(2) 0.522(3) 0.105(19) Uani 1 1 d . . . H12 H 1.0259 0.2018 0.5454 0.126 Uiso 1 1 calc R . . C13 C 0.930(2) 0.1860(19) 0.550(2) 0.076(13) Uani 1 1 d . . . H13 H 0.9279 0.1872 0.5925 0.091 Uiso 1 1 calc R . . C14 C 0.8749(17) 0.1766(17) 0.5136(18) 0.054(9) Uani 1 1 d . . . C15 C 0.8150(18) 0.1695(16) 0.5403(17) 0.056(10) Uani 1 1 d . . . H15 H 0.8123 0.1722 0.5826 0.067 Uiso 1 1 calc R . . C16 C 0.7611(16) 0.1586(15) 0.5054(15) 0.043(8) Uani 1 1 d . . . C17 C 0.6662(17) 0.0994(18) 0.5674(15) 0.049(9) Uani 1 1 d . . . C18 C 0.5751(16) 0.0567(16) 0.6411(13) 0.041(8) Uani 1 1 d . . . H18 H 0.5856 0.0214 0.6478 0.049 Uiso 1 1 calc R . . C19 C 0.6096(16) 0.1028(16) 0.5979(15) 0.044(8) Uani 1 1 d . . . C20 C 0.5945(17) 0.1540(17) 0.5865(16) 0.053(9) Uani 1 1 d . . . H20 H 0.6190 0.1880 0.5571 0.063 Uiso 1 1 calc R . . C21 C 0.5417(18) 0.1540(16) 0.6201(16) 0.054(9) Uani 1 1 d . . . H21 H 0.5278 0.1866 0.6124 0.064 Uiso 1 1 calc R . . C22 C 0.5111(17) 0.1061(16) 0.6640(15) 0.049(8) Uani 1 1 d . . . H22 H 0.4769 0.1073 0.6878 0.059 Uiso 1 1 calc R . . C23 C 0.664(2) 0.0000 0.2500 0.043(11) Uani 1 2 d S . . C24 C 0.6922(19) -0.0141(19) 0.1963(18) 0.066(11) Uani 1 1 d . . . H24A H 0.6614 -0.0228 0.1624 0.079 Uiso 1 1 calc R . . H24B H 0.6969 -0.0544 0.2033 0.079 Uiso 1 1 calc R . . H24C H 0.7371 0.0253 0.1874 0.079 Uiso 1 1 calc R . . C25 C 0.336(3) 0.0000 0.2500 0.062(14) Uani 1 2 d S . . C26 C 0.313(2) 0.024(2) 0.303(2) 0.090(15) Uani 1 1 d . . . H26A H 0.3473 0.0383 0.3347 0.109 Uiso 1 1 calc R . . H26B H 0.2693 -0.0129 0.3169 0.109 Uiso 1 1 calc R . . H26C H 0.3082 0.0632 0.2906 0.109 Uiso 1 1 calc R . . C27 C 0.6667 0.3333 0.174(8) 0.27(8) Uani 1 3 d SD . . H27A H 0.6647 0.3121 0.1632 0.325 Uiso 0.33 1 d PRD . . H27B H 0.6667 0.3333 0.2006 0.325 Uiso 1 3 d SRD . . C28 C 0.651(2) 0.062(2) 0.015(2) 0.094(16) Uani 1 1 d . . . H28A H 0.6754 0.0389 -0.0026 0.112 Uiso 1 1 calc R . . H28B H 0.6798 0.0916 0.0476 0.112 Uiso 1 1 calc R . . C29 C 0.866(6) 0.954(4) 0.324(8) 0.27(8) Uani 0.50 1 d PD . . H29A H 0.9049 0.9501 0.3070 0.325 Uiso 0.50 1 calc PR . . H29B H 0.8658 0.9465 0.3675 0.325 Uiso 0.50 1 calc PR . . 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 0.040(2) 0.036(3) 0.035(3) -0.001(2) -0.0006(12) 0.0182(15) Cl1 0.162(13) 0.075(8) 0.072(7) -0.017(7) -0.030(8) 0.080(9) Cl2 0.088(9) 0.088(9) 0.119(19) 0.000 0.000 0.044(4) Cl3 0.19(6) 0.12(5) 0.17(5) 0.06(4) 0.10(5) 0.06(4) Cl4 0.22(2) 0.104(11) 0.123(12) 0.056(9) 0.063(12) 0.093(12) Cl5 0.121(10) 0.063(7) 0.084(8) 0.014(6) 0.032(7) 0.041(7) Cl6 0.31(9) 0.23(6) 0.35(10) -0.07(7) 0.00(8) 0.12(6) Cl7 0.16(6) 0.49(15) 0.9(3) -0.39(18) -0.04(10) 0.13(8) O1 0.055(14) 0.036(13) 0.067(17) -0.006(12) -0.012(12) 0.016(12) O2 0.040(12) 0.041(12) 0.041(12) -0.002(10) -0.004(10) 0.020(10) O3 0.060(15) 0.053(15) 0.058(15) 0.009(12) 0.010(13) 0.029(13) O4 0.051(14) 0.048(13) 0.047(14) 0.009(11) 0.013(12) 0.023(11) O5 0.036(13) 0.043(18) 0.06(2) 0.003(15) 0.001(8) 0.022(9) O6 0.041(13) 0.06(2) 0.06(2) 0.000(17) 0.000(8) 0.028(10) O7 0.23(5) 0.06(2) 0.16(4) 0.00(2) -0.05(3) 0.07(3) O8 0.13(3) 0.07(2) 0.11(3) -0.04(2) -0.05(2) 0.06(2) O9 0.37(8) 0.09(3) 0.12(4) 0.01(3) -0.15(5) 0.02(4) O10 0.20(7) 0.17(6) 0.20(7) 0.02(5) 0.04(5) 0.15(6) O10' 0.17(7) 0.22(8) 0.25(8) -0.10(6) 0.06(6) 0.08(6) N1 0.040(15) 0.039(14) 0.036(14) 0.003(12) 0.005(13) 0.020(13) N2 0.042(15) 0.037(14) 0.037(14) 0.001(12) 0.004(13) 0.018(12) C1 0.05(2) 0.05(2) 0.05(2) 0.001(17) -0.001(17) 0.026(17) C2 0.06(2) 0.07(2) 0.06(2) -0.01(2) -0.02(2) 0.05(2) C3 0.05(2) 0.045(19) 0.05(2) -0.001(17) -0.003(19) 0.024(18) C4 0.042(18) 0.042(18) 0.039(18) -0.002(15) 0.006(15) 0.021(15) C5 0.043(18) 0.041(18) 0.034(17) 0.005(15) 0.006(15) 0.022(15) C6 0.045(19) 0.040(19) 0.035(18) 0.008(15) 0.006(15) 0.020(16) C7 0.040(18) 0.039(18) 0.038(18) 0.006(15) -0.002(15) 0.019(15) C8 0.05(2) 0.035(18) 0.050(19) 0.003(15) 0.003(16) 0.016(16) C9 0.034(18) 0.035(18) 0.08(3) 0.007(18) 0.001(19) 0.013(14) C10 0.04(2) 0.07(3) 0.10(3) 0.02(2) 0.02(2) 0.02(2) C11 0.05(3) 0.11(4) 0.14(5) 0.01(4) 0.00(3) 0.04(3) C12 0.04(3) 0.07(3) 0.17(6) 0.02(4) -0.04(3) 0.01(2) C13 0.04(2) 0.06(3) 0.10(3) 0.01(2) -0.02(2) 0.01(2) C14 0.039(19) 0.04(2) 0.07(3) 0.004(18) -0.006(19) 0.013(16) C15 0.06(2) 0.05(2) 0.05(2) -0.001(18) -0.010(18) 0.016(18) C16 0.041(19) 0.037(18) 0.04(2) 0.000(15) 0.001(16) 0.013(15) C17 0.05(2) 0.05(2) 0.04(2) -0.005(17) -0.001(17) 0.020(18) C18 0.05(2) 0.041(18) 0.035(17) -0.005(15) -0.002(16) 0.026(16) C19 0.047(19) 0.043(19) 0.041(19) 0.006(16) 0.007(16) 0.022(16) C20 0.06(2) 0.039(19) 0.05(2) 0.007(17) 0.003(18) 0.014(17) C21 0.06(2) 0.036(18) 0.07(2) 0.012(18) 0.01(2) 0.024(17) C22 0.05(2) 0.05(2) 0.05(2) 0.003(17) 0.006(17) 0.026(18) C23 0.04(2) 0.04(3) 0.05(3) 0.00(2) -0.001(11) 0.019(13) C24 0.06(2) 0.06(2) 0.08(3) 0.00(2) 0.01(2) 0.03(2) C25 0.07(3) 0.07(4) 0.05(3) 0.01(3) 0.006(14) 0.034(18) C26 0.11(4) 0.12(4) 0.08(3) 0.01(3) 0.02(3) 0.09(3) C27 0.34(13) 0.34(13) 0.14(11) 0.000 0.000 0.17(7) C28 0.05(2) 0.10(3) 0.14(4) -0.05(3) -0.01(3) 0.04(2) C29 0.34(13) 0.34(13) 0.14(11) 0.000 0.000 0.17(7) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 N2 2.01(2) 11_655 ? Cu1 N2 2.01(2) 7_656 ? Cu1 N1 2.02(2) . ? Cu1 N1 2.02(2) 5 ? Cu1 O5 2.39(3) . ? Cl1 O9 1.33(4) . ? Cl1 O7 1.33(3) . ? Cl1 O8 1.36(3) . ? Cl1 O10' 1.67(9) . ? Cl1 O10 1.72(10) . ? Cl2 C27 1.71(17) . ? Cl2 H27A 1.5293 . ? Cl3 C27 1.37(11) . ? Cl3 Cl3 1.69(11) 3_665 ? Cl3 Cl3 1.69(11) 2_655 ? Cl3 H27A 1.5484 . ? Cl3 H27B 1.0440 . ? Cl4 C28 1.72(5) . ? Cl5 C28 1.72(4) . ? Cl6 C29 1.630(6) . ? Cl7 C29 1.630(9) . ? O1 C6 1.18(3) . ? O2 C6 1.36(3) . ? O2 C7 1.39(3) . ? O3 C17 1.20(4) . ? O4 C17 1.35(4) . ? O4 C16 1.39(4) . ? O5 C23 1.20(5) . ? O6 C25 1.22(6) . ? N1 C1 1.36(4) . ? N1 C5 1.36(4) . ? N2 C18 1.34(4) . ? N2 C22 1.34(4) . ? N2 Cu1 2.01(2) 7_656 ? C1 C2 1.38(4) . ? C1 H1 0.9500 . ? C2 C3 1.36(4) . ? C2 H2 0.9500 . ? C3 C4 1.39(4) . ? C3 H3 0.9500 . ? C4 C5 1.39(4) . ? C4 C6 1.48(4) . ? C5 H5 0.9500 . ? C7 C8 1.34(4) . ? C7 C16 1.41(4) . ? C8 C9 1.42(5) . ? C8 H8 0.9500 . ? C9 C14 1.40(5) . ? C9 C10 1.42(5) . ? C10 C11 1.34(6) . ? C10 H10 0.9500 . ? C11 C12 1.43(8) . ? C11 H11 0.9500 . ? C12 C13 1.37(7) . ? C12 H12 0.9500 . ? C13 C14 1.42(5) . ? C13 H13 0.9500 . ? C14 C15 1.41(5) . ? C15 C16 1.36(4) . ? C15 H15 0.9500 . ? C17 C19 1.48(4) . ? C18 C19 1.35(4) . ? C18 H18 0.9500 . ? C19 C20 1.38(4) . ? C20 C21 1.41(5) . ? C20 H20 0.9500 . ? C21 C22 1.36(4) . ? C21 H21 0.9500 . ? C22 H22 0.9500 . ? C23 C24 1.46(4) 5 ? C23 C24 1.46(4) . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.49(5) 5 ? C25 C26 1.49(5) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 Cl3 1.37(11) 3_665 ? C27 Cl3 1.37(11) 2_655 ? C27 H27A 0.5214 . ? C27 H27B 0.5877 . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? 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 N2 Cu1 N2 175.8(15) 11_655 7_656 ? N2 Cu1 N1 87.7(9) 11_655 . ? N2 Cu1 N1 92.1(9) 7_656 . ? N2 Cu1 N1 92.1(9) 11_655 5 ? N2 Cu1 N1 87.7(9) 7_656 5 ? N1 Cu1 N1 174.6(14) . 5 ? N2 Cu1 O5 92.1(7) 11_655 . ? N2 Cu1 O5 92.1(7) 7_656 . ? N1 Cu1 O5 92.7(7) . . ? N1 Cu1 O5 92.7(7) 5 . ? O9 Cl1 O7 123(3) . . ? O9 Cl1 O8 117(3) . . ? O7 Cl1 O8 119(2) . . ? O9 Cl1 O10' 81(5) . . ? O7 Cl1 O10' 83(3) . . ? O8 Cl1 O10' 98(4) . . ? O9 Cl1 O10 93(5) . . ? O7 Cl1 O10 96(4) . . ? O8 Cl1 O10 89(4) . . ? O10' Cl1 O10 172(5) . . ? C27 Cl2 H27A 17.5 . . ? C27 Cl3 Cl3 52(5) . 3_665 ? C27 Cl3 Cl3 52(5) . 2_655 ? Cl3 Cl3 Cl3 60.000(16) 3_665 2_655 ? C27 Cl3 H27A 19.3 . . ? Cl3 Cl3 H27A 70.1 3_665 . ? Cl3 Cl3 H27A 51.1 2_655 . ? C27 Cl3 H27B 23.7 . . ? Cl3 Cl3 H27B 35.9 3_665 . ? Cl3 Cl3 H27B 35.9 2_655 . ? H27A Cl3 H27B 37.1 . . ? C6 O2 C7 118(2) . . ? C17 O4 C16 117(3) . . ? C23 O5 Cu1 180.000(3) . . ? C1 N1 C5 117(3) . . ? C1 N1 Cu1 121(2) . . ? C5 N1 Cu1 121(2) . . ? C18 N2 C22 117(3) . . ? C18 N2 Cu1 120(2) . 7_656 ? C22 N2 Cu1 122(2) . 7_656 ? N1 C1 C2 123(3) . . ? N1 C1 H1 118.5 . . ? C2 C1 H1 118.5 . . ? C3 C2 C1 119(3) . . ? C3 C2 H2 120.4 . . ? C1 C2 H2 120.4 . . ? C2 C3 C4 120(3) . . ? C2 C3 H3 120.0 . . ? C4 C3 H3 120.0 . . ? C3 C4 C5 118(3) . . ? C3 C4 C6 119(3) . . ? C5 C4 C6 123(3) . . ? N1 C5 C4 122(3) . . ? N1 C5 H5 118.8 . . ? C4 C5 H5 118.8 . . ? O1 C6 O2 124(3) . . ? O1 C6 C4 125(3) . . ? O2 C6 C4 111(3) . . ? C8 C7 O2 120(3) . . ? C8 C7 C16 121(3) . . ? O2 C7 C16 119(3) . . ? C7 C8 C9 120(3) . . ? C7 C8 H8 119.8 . . ? C9 C8 H8 119.8 . . ? C14 C9 C8 119(3) . . ? C14 C9 C10 119(3) . . ? C8 C9 C10 122(4) . . ? C11 C10 C9 122(5) . . ? C11 C10 H10 119.2 . . ? C9 C10 H10 119.2 . . ? C10 C11 C12 119(5) . . ? C10 C11 H11 120.7 . . ? C12 C11 H11 120.7 . . ? C13 C12 C11 123(4) . . ? C13 C12 H12 118.6 . . ? C11 C12 H12 118.6 . . ? C12 C13 C14 117(5) . . ? C12 C13 H13 121.3 . . ? C14 C13 H13 121.3 . . ? C9 C14 C15 119(3) . . ? C9 C14 C13 121(4) . . ? C15 C14 C13 120(4) . . ? C16 C15 C14 120(3) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C15 C16 O4 122(3) . . ? C15 C16 C7 120(3) . . ? O4 C16 C7 118(3) . . ? O3 C17 O4 124(3) . . ? O3 C17 C19 124(3) . . ? O4 C17 C19 113(3) . . ? N2 C18 C19 124(3) . . ? N2 C18 H18 118.0 . . ? C19 C18 H18 118.0 . . ? C18 C19 C20 119(3) . . ? C18 C19 C17 118(3) . . ? C20 C19 C17 123(3) . . ? C19 C20 C21 118(3) . . ? C19 C20 H20 121.1 . . ? C21 C20 H20 121.1 . . ? C22 C21 C20 118(3) . . ? C22 C21 H21 120.8 . . ? C20 C21 H21 120.8 . . ? N2 C22 C21 123(3) . . ? N2 C22 H22 118.4 . . ? C21 C22 H22 118.4 . . ? O5 C23 C24 123(2) . 5 ? O5 C23 C24 123(2) . . ? C24 C23 C24 114(4) 5 . ? 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 . . ? O6 C25 C26 122(3) . 5 ? O6 C25 C26 122(3) . . ? C26 C25 C26 116(5) 5 . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Cl3 C27 Cl3 76(9) 3_665 . ? Cl3 C27 Cl3 76(9) 3_665 2_655 ? Cl3 C27 Cl3 76(9) . 2_655 ? Cl3 C27 Cl2 134(6) 3_665 . ? Cl3 C27 Cl2 134(6) . . ? Cl3 C27 Cl2 134(6) 2_655 . ? Cl3 C27 H27A 159.4 3_665 . ? Cl3 C27 H27A 100.4 . . ? Cl3 C27 H27A 83.0 2_655 . ? Cl2 C27 H27A 61.7 . . ? Cl3 C27 H27B 45.6 3_665 . ? Cl3 C27 H27B 45.6 . . ? Cl3 C27 H27B 45.6 2_655 . ? Cl2 C27 H27B 180.0 . . ? H27A C27 H27B 118.3 . . ? Cl5 C28 Cl4 112(2) . . ? Cl5 C28 H28A 109.2 . . ? Cl4 C28 H28A 109.2 . . ? Cl5 C28 H28B 109.2 . . ? Cl4 C28 H28B 109.2 . . ? H28A C28 H28B 107.9 . . ? Cl6 C29 Cl7 118.4(11) . . ? Cl6 C29 H29A 107.7 . . ? Cl7 C29 H29A 107.7 . . ? Cl6 C29 H29B 107.7 . . ? Cl7 C29 H29B 107.7 . . ? H29A C29 H29B 107.1 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.140 _refine_diff_density_min -0.756 _refine_diff_density_rms 0.120 _database_code_depnum_ccdc_archive 'CCDC 928711' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_dd #TrackingRef '02-2CH3CN.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C152 H138 Cl22 Cu3 N18 O58' _chemical_formula_weight 4115.32 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' O O 0.0106 0.0060 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 38.9150(7) _cell_length_b 22.2085(3) _cell_length_c 21.7493(3) _cell_angle_alpha 90.00 _cell_angle_beta 98.683(2) _cell_angle_gamma 90.00 _cell_volume 18581.3(5) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8197 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 20.32 _exptl_crystal_description block _exptl_crystal_colour blue _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.26 _exptl_crystal_size_min 0.23 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.471 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8404 _exptl_absorpt_coefficient_mu 0.743 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7809 _exptl_absorpt_correction_T_max 0.8476 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker Breeze CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 146146 _diffrn_reflns_av_R_equivalents 0.0892 _diffrn_reflns_av_sigmaI/netI 0.0727 _diffrn_reflns_limit_h_min -48 _diffrn_reflns_limit_h_max 48 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 26.00 _reflns_number_total 18265 _reflns_number_gt 9794 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.1886P)^2^+143.1234P] 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 18265 _refine_ls_number_parameters 1143 _refine_ls_number_restraints 23 _refine_ls_R_factor_all 0.1889 _refine_ls_R_factor_gt 0.1148 _refine_ls_wR_factor_ref 0.3728 _refine_ls_wR_factor_gt 0.3114 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.040 _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 0.24820(3) 0.28717(4) 0.74918(4) 0.0467(3) Uani 1 1 d . . . Cu2 Cu 0.0000 0.48034(6) 0.2500 0.0465(4) Uani 1 2 d S . . Cl1 Cl 0.09392(9) 0.3246(2) 0.72273(15) 0.1071(12) Uani 1 1 d . . . Cl2 Cl 0.21087(8) 0.02834(10) 0.72879(11) 0.0723(7) Uani 1 1 d . . . Cl3 Cl 0.10384(14) 0.7162(3) 0.72713(17) 0.160(2) Uani 1 1 d D . . Cl4 Cl 0.31738(16) 0.3030(2) -0.0412(2) 0.1588(19) Uani 1 1 d . . . Cl5 Cl 0.29183(14) 0.2146(2) 0.0378(2) 0.1517(18) Uani 1 1 d . . . Cl6 Cl 0.3087(4) 0.3277(6) 0.4392(7) 0.376(9) Uani 1 1 d . . . Cl7 Cl 0.2635(5) 0.3076(15) 0.5040(16) 0.93(4) Uani 1 1 d . . . Cl8 Cl 0.05431(13) 0.4128(3) 0.4826(2) 0.1535(17) Uani 1 1 d . . . Cl9 Cl -0.00152(10) 0.4311(3) 0.5506(2) 0.162(2) Uani 1 1 d . . . Cl10 Cl 0.1673(2) 0.5120(5) 0.6499(8) 0.372(9) Uani 1 1 d . . . Cl11 Cl 0.1515(4) 0.5591(15) 0.7486(9) 0.64(3) Uani 1 1 d . . . O1 O 0.18363(19) 0.1385(3) 0.8924(3) 0.0715(18) Uani 1 1 d . . . O2 O 0.22202(15) 0.0675(2) 0.9344(2) 0.0517(13) Uani 1 1 d . . . O3 O 0.26153(16) 0.0013(3) 1.0455(3) 0.0625(16) Uani 1 1 d . . . O4 O 0.21800(15) 0.0637(2) 1.0588(2) 0.0499(13) Uani 1 1 d . . . O5 O 0.34582(17) 0.2961(3) 0.5949(3) 0.0664(17) Uani 1 1 d . . . O6 O 0.36039(15) 0.2009(2) 0.5746(3) 0.0542(14) Uani 1 1 d . . . O7 O 0.3548(2) 0.1044(3) 0.4890(3) 0.083(2) Uani 1 1 d . . . O8 O 0.35044(16) 0.1968(3) 0.4469(3) 0.0618(15) Uani 1 1 d . . . O9 O 0.02915(17) 0.3300(3) 0.0680(3) 0.0697(17) Uani 1 1 d . . . O10 O 0.07996(16) 0.3592(3) 0.0389(3) 0.0638(16) Uani 1 1 d . . . O11 O 0.12555(15) 0.4076(3) -0.0471(3) 0.0692(17) Uani 1 1 d . . . O12 O 0.07273(15) 0.3727(3) -0.0870(3) 0.0547(14) Uani 1 1 d . . . O13 O 0.0883(2) 0.3631(4) 0.7711(3) 0.108(3) Uani 1 1 d . . . O14 O 0.1004(5) 0.2711(6) 0.7466(7) 0.221(9) Uani 1 1 d . . . O15 O 0.1211(2) 0.3422(6) 0.6920(4) 0.134(4) Uani 1 1 d . . . O16 O 0.0630(2) 0.3315(5) 0.6753(4) 0.123(3) Uani 1 1 d . . . O17 O 0.1983(4) 0.0683(5) 0.6796(5) 0.153(4) Uani 1 1 d . . . O18 O 0.2346(4) -0.0069(5) 0.7051(5) 0.153(5) Uani 1 1 d . . . O19 O 0.1875(3) -0.0068(5) 0.7546(8) 0.168(6) Uani 1 1 d . . . O20 O 0.2265(4) 0.0669(5) 0.7753(5) 0.149(4) Uani 1 1 d . . . O21 O 0.0904(5) 0.6675(6) 0.7002(8) 0.327(16) Uani 1 1 d D . . O22 O 0.1001(6) 0.7619(6) 0.6874(7) 0.52(3) Uani 1 1 d D . . O23 O 0.1373(2) 0.7087(11) 0.7486(11) 0.60(5) Uani 1 1 d D . . O24 O 0.0874(5) 0.7302(11) 0.7752(7) 0.54(3) Uani 1 1 d D . . O25 O -0.0230(5) 0.8606(7) 0.2891(8) 0.233(8) Uani 1 1 d . . . H25B H -0.0034 0.8730 0.2832 0.280 Uiso 1 1 d R . . H25C H -0.0377 0.8884 0.2812 0.280 Uiso 1 1 d R . . O26 O 0.0898(9) 0.0281(18) 0.7370(18) 0.51(3) Uani 1 1 d . . . H26A H 0.0744 0.0495 0.7495 0.614 Uiso 1 1 d R . . H26B H 0.0819 0.0133 0.7022 0.614 Uiso 1 1 d R . . O27 O 0.0053(13) 0.000(3) 0.557(3) 0.65(6) Uani 1 1 d . . . H27B H 0.0045 -0.0296 0.5802 0.782 Uiso 1 1 d R . . H27C H -0.0146 0.0160 0.5491 0.782 Uiso 1 1 d R . . O28 O 0.0488(10) 0.044(3) 0.133(3) 0.79(7) Uani 1 1 d . . . H28A H 0.0480 0.0326 0.0959 0.954 Uiso 1 1 d R . . H28B H 0.0365 0.0204 0.1512 0.954 Uiso 1 1 d R . . O29 O -0.0253(11) 0.086(2) 0.227(2) 0.57(3) Uani 1 1 d U . . H29A H -0.0432 0.0647 0.2220 0.690 Uiso 1 1 d R . . H29B H -0.0127 0.0765 0.2002 0.690 Uiso 1 1 d R . . N1 N 0.26233(19) 0.2264(3) 0.8185(3) 0.0478(16) Uani 1 1 d . . . N2 N 0.27603(18) 0.1587(3) 1.1945(3) 0.0483(16) Uani 1 1 d . . . N3 N 0.26939(16) 0.2313(3) 0.6908(3) 0.0409(14) Uani 1 1 d . . . N4 N 0.26687(17) 0.1550(3) 0.3227(3) 0.0456(15) Uani 1 1 d . . . N5 N 0.3034(2) 0.3363(3) 0.7777(3) 0.0537(17) Uani 1 1 d . . . N6 N 0.1894(2) 0.2253(3) 0.7202(3) 0.0571(19) Uani 1 1 d . . . N7 N 0.03062(17) 0.4782(3) 0.1832(3) 0.0476(15) Uani 1 1 d . . . N8 N 0.04463(17) 0.5223(3) -0.1858(3) 0.0465(15) Uani 1 1 d . . . N9 N 0.0000 0.5896(5) 0.2500 0.054(2) Uani 1 2 d S . . N10 N 0.0000 0.3646(5) 0.2500 0.071(3) Uani 1 2 d SD . . C1 C 0.2373(2) 0.1988(3) 0.8442(3) 0.0485(19) Uani 1 1 d . . . H1A H 0.2141 0.2136 0.8352 0.058 Uiso 1 1 calc R . . C2 C 0.2440(2) 0.1493(3) 0.8836(3) 0.0487(19) Uani 1 1 d . . . C3 C 0.2773(2) 0.1299(4) 0.8991(4) 0.054(2) Uani 1 1 d . . . H3A H 0.2826 0.0968 0.9267 0.065 Uiso 1 1 calc R . . C4 C 0.3033(3) 0.1591(4) 0.8738(4) 0.062(2) Uani 1 1 d . . . H4A H 0.3268 0.1466 0.8840 0.074 Uiso 1 1 calc R . . C5 C 0.2947(2) 0.2065(4) 0.8339(4) 0.057(2) Uani 1 1 d . . . H5A H 0.3128 0.2259 0.8164 0.069 Uiso 1 1 calc R . . C6 C 0.2131(3) 0.1198(4) 0.9032(4) 0.052(2) Uani 1 1 d . . . C7 C 0.1951(2) 0.0347(3) 0.9539(4) 0.054(2) Uani 1 1 d . . . C8 C 0.1719(3) 0.0043(4) 0.9125(5) 0.073(3) Uani 1 1 d . . . H8A H 0.1736 0.0045 0.8693 0.088 Uiso 1 1 calc R . . C9 C 0.1443(3) -0.0288(4) 0.9361(6) 0.077(3) Uani 1 1 d . . . C10 C 0.1175(3) -0.0588(5) 0.8953(8) 0.108(5) Uani 1 1 d . . . H10A H 0.1168 -0.0568 0.8515 0.129 Uiso 1 1 calc R . . C11 C 0.0931(4) -0.0898(6) 0.9197(11) 0.124(6) Uani 1 1 d . . . H11A H 0.0760 -0.1112 0.8924 0.148 Uiso 1 1 calc R . . C12 C 0.0919(5) -0.0918(7) 0.9801(12) 0.136(7) Uani 1 1 d . . . H12A H 0.0735 -0.1127 0.9950 0.163 Uiso 1 1 calc R . . C13 C 0.1166(3) -0.0645(6) 1.0209(9) 0.113(5) Uani 1 1 d . . . H13A H 0.1157 -0.0676 1.0642 0.135 Uiso 1 1 calc R . . C14 C 0.1438(3) -0.0315(4) 1.0005(6) 0.079(3) Uani 1 1 d . . . C15 C 0.1693(2) -0.0020(4) 1.0399(5) 0.065(2) Uani 1 1 d . . . H15A H 0.1696 -0.0046 1.0835 0.078 Uiso 1 1 calc R . . C16 C 0.1939(2) 0.0305(3) 1.0178(4) 0.054(2) Uani 1 1 d . . . C17 C 0.2508(2) 0.0444(3) 1.0695(4) 0.0479(19) Uani 1 1 d . . . C18 C 0.2574(2) 0.1258(3) 1.1500(4) 0.0449(18) Uani 1 1 d . . . H18A H 0.2330 0.1312 1.1420 0.054 Uiso 1 1 calc R . . C19 C 0.2725(2) 0.0845(3) 1.1157(4) 0.0477(19) Uani 1 1 d . . . C20 C 0.3081(3) 0.0780(5) 1.1264(5) 0.082(3) Uani 1 1 d . . . H20A H 0.3192 0.0496 1.1033 0.099 Uiso 1 1 calc R . . C21 C 0.3271(3) 0.1130(6) 1.1706(6) 0.095(4) Uani 1 1 d . . . H21A H 0.3518 0.1102 1.1779 0.115 Uiso 1 1 calc R . . C22 C 0.3102(2) 0.1521(5) 1.2042(5) 0.072(3) Uani 1 1 d . . . H22A H 0.3235 0.1755 1.2358 0.087 Uiso 1 1 calc R . . C23 C 0.2605(2) 0.1730(3) 0.6844(4) 0.0508(19) Uani 1 1 d . . . H23A H 0.2425 0.1579 0.7052 0.061 Uiso 1 1 calc R . . C24 C 0.2768(2) 0.1341(4) 0.6483(4) 0.053(2) Uani 1 1 d . . . H24A H 0.2697 0.0933 0.6437 0.063 Uiso 1 1 calc R . . C25 C 0.3031(2) 0.1546(4) 0.6194(4) 0.055(2) Uani 1 1 d . . . H25A H 0.3149 0.1283 0.5953 0.065 Uiso 1 1 calc R . . C26 C 0.3123(2) 0.2150(3) 0.6260(3) 0.0457(18) Uani 1 1 d . . . C27 C 0.2946(2) 0.2517(3) 0.6615(3) 0.0483(19) Uani 1 1 d . . . H27A H 0.3005 0.2932 0.6650 0.058 Uiso 1 1 calc R . . C28 C 0.3410(2) 0.2434(4) 0.5983(4) 0.0493(19) Uani 1 1 d . . . C29 C 0.3871(2) 0.2213(4) 0.5434(4) 0.053(2) Uani 1 1 d . . . C30 C 0.4171(2) 0.2452(4) 0.5752(5) 0.065(2) Uani 1 1 d . . . H30A H 0.4201 0.2488 0.6192 0.078 Uiso 1 1 calc R . . C31 C 0.4434(3) 0.2642(4) 0.5422(6) 0.077(3) Uani 1 1 d . . . C32 C 0.4744(3) 0.2915(6) 0.5700(7) 0.097(4) Uani 1 1 d . . . H32A H 0.4788 0.2946 0.6141 0.116 Uiso 1 1 calc R . . C33 C 0.4982(3) 0.3135(7) 0.5370(10) 0.129(6) Uani 1 1 d . . . H33A H 0.5186 0.3327 0.5575 0.154 Uiso 1 1 calc R . . C34 C 0.4925(4) 0.3077(8) 0.4721(9) 0.124(5) Uani 1 1 d . . . H34A H 0.5092 0.3227 0.4484 0.149 Uiso 1 1 calc R . . C35 C 0.4640(3) 0.2813(6) 0.4440(7) 0.101(4) Uani 1 1 d . . . H35A H 0.4610 0.2766 0.4001 0.122 Uiso 1 1 calc R . . C36 C 0.4385(3) 0.2606(5) 0.4757(5) 0.071(3) Uani 1 1 d . . . C37 C 0.4072(3) 0.2353(5) 0.4461(5) 0.073(3) Uani 1 1 d . . . H37A H 0.4035 0.2311 0.4021 0.088 Uiso 1 1 calc R . . C38 C 0.3824(2) 0.2169(4) 0.4787(4) 0.058(2) Uani 1 1 d . . . C39 C 0.3400(3) 0.1397(4) 0.4550(4) 0.060(2) Uani 1 1 d . . . C40 C 0.2947(2) 0.1667(3) 0.3644(4) 0.0463(18) Uani 1 1 d . . . H40A H 0.3071 0.2030 0.3609 0.056 Uiso 1 1 calc R . . C41 C 0.3061(2) 0.1280(3) 0.4122(4) 0.055(2) Uani 1 1 d . . . C42 C 0.2882(3) 0.0755(4) 0.4181(5) 0.079(3) Uani 1 1 d . . . H42A H 0.2958 0.0483 0.4510 0.094 Uiso 1 1 calc R . . C43 C 0.2593(3) 0.0628(4) 0.3765(6) 0.085(3) Uani 1 1 d . . . H43A H 0.2463 0.0272 0.3802 0.102 Uiso 1 1 calc R . . C44 C 0.2494(3) 0.1036(4) 0.3282(5) 0.067(3) Uani 1 1 d . . . H44A H 0.2297 0.0948 0.2983 0.081 Uiso 1 1 calc R . . C45 C 0.3289(3) 0.3579(4) 0.7908(5) 0.068(3) Uani 1 1 d . . . C46 C 0.3625(4) 0.3862(7) 0.8110(12) 0.199(12) Uani 1 1 d . . . H46A H 0.3613 0.4289 0.7994 0.239 Uiso 1 1 calc R . . H46B H 0.3803 0.3662 0.7908 0.239 Uiso 1 1 calc R . . H46C H 0.3685 0.3825 0.8562 0.239 Uiso 1 1 calc R . . C47 C 0.1680(4) 0.1952(6) 0.7149(7) 0.105(4) Uani 1 1 d . . . C48 C 0.1368(4) 0.1513(9) 0.7096(19) 0.34(3) Uani 1 1 d . . . H48A H 0.1450 0.1114 0.7242 0.404 Uiso 1 1 calc R . . H48B H 0.1258 0.1487 0.6661 0.404 Uiso 1 1 calc R . . H48C H 0.1199 0.1661 0.7351 0.404 Uiso 1 1 calc R . . C49 C 0.0550(2) 0.5196(4) 0.1807(4) 0.054(2) Uani 1 1 d . . . H49A H 0.0556 0.5536 0.2074 0.064 Uiso 1 1 calc R . . C50 C 0.0793(2) 0.5155(5) 0.1413(4) 0.063(2) Uani 1 1 d . . . H50A H 0.0959 0.5466 0.1398 0.075 Uiso 1 1 calc R . . C51 C 0.0792(2) 0.4656(4) 0.1039(4) 0.060(2) Uani 1 1 d . . . H51A H 0.0961 0.4613 0.0770 0.072 Uiso 1 1 calc R . . C52 C 0.0545(2) 0.4222(4) 0.1060(4) 0.052(2) Uani 1 1 d . . . C53 C 0.0305(2) 0.4305(4) 0.1462(4) 0.0509(19) Uani 1 1 d . . . H53A H 0.0131 0.4007 0.1474 0.061 Uiso 1 1 calc R . . C54 C 0.0519(2) 0.3659(5) 0.0696(4) 0.057(2) Uani 1 1 d . . . C55 C 0.0817(2) 0.3085(4) 0.0034(4) 0.062(2) Uani 1 1 d . . . C56 C 0.0843(3) 0.2513(5) 0.0279(5) 0.069(3) Uani 1 1 d . . . H56A H 0.0851 0.2453 0.0713 0.083 Uiso 1 1 calc R . . C57 C 0.0856(3) 0.2017(5) -0.0117(6) 0.082(3) Uani 1 1 d . . . C58 C 0.0880(3) 0.1403(6) 0.0131(8) 0.106(4) Uani 1 1 d . . . H58A H 0.0890 0.1325 0.0562 0.127 Uiso 1 1 calc R . . C59 C 0.0887(4) 0.0941(6) -0.0296(11) 0.131(6) Uani 1 1 d . . . H59A H 0.0909 0.0540 -0.0145 0.157 Uiso 1 1 calc R . . C60 C 0.0862(5) 0.1038(7) -0.0938(10) 0.136(6) Uani 1 1 d . . . H60A H 0.0859 0.0703 -0.1212 0.163 Uiso 1 1 calc R . . C61 C 0.0845(4) 0.1587(6) -0.1165(8) 0.116(5) Uani 1 1 d . . . H61A H 0.0831 0.1647 -0.1601 0.139 Uiso 1 1 calc R . . C62 C 0.0847(3) 0.2098(5) -0.0760(6) 0.077(3) Uani 1 1 d . . . C63 C 0.0816(3) 0.2686(5) -0.0990(5) 0.070(3) Uani 1 1 d . . . H63A H 0.0810 0.2751 -0.1423 0.084 Uiso 1 1 calc R . . C64 C 0.0796(2) 0.3157(4) -0.0619(4) 0.055(2) Uani 1 1 d . . . C65 C 0.0978(2) 0.4157(4) -0.0778(4) 0.053(2) Uani 1 1 d . . . C66 C 0.0545(2) 0.4749(4) -0.1513(4) 0.0490(19) Uani 1 1 d . . . H66A H 0.0393 0.4411 -0.1539 0.059 Uiso 1 1 calc R . . C67 C 0.0862(2) 0.4713(4) -0.1110(4) 0.0480(19) Uani 1 1 d . . . C68 C 0.1074(2) 0.5217(4) -0.1050(5) 0.067(3) Uani 1 1 d . . . H68A H 0.1286 0.5221 -0.0769 0.080 Uiso 1 1 calc R . . C69 C 0.0967(3) 0.5718(4) -0.1411(5) 0.075(3) Uani 1 1 d . . . H69A H 0.1109 0.6068 -0.1386 0.090 Uiso 1 1 calc R . . C70 C 0.0661(2) 0.5707(4) -0.1801(4) 0.061(2) Uani 1 1 d . . . H70A H 0.0593 0.6054 -0.2045 0.073 Uiso 1 1 calc R . . C71 C 0.0000 0.6402(6) 0.2500 0.075(4) Uani 1 2 d S . . C72 C 0.0000 0.7058(7) 0.2500 0.162(13) Uani 1 2 d S . . H72A H -0.0220 0.7206 0.2271 0.195 Uiso 0.50 1 calc PR . . H72B H 0.0193 0.7206 0.2300 0.195 Uiso 0.50 1 calc PR . . H72C H 0.0027 0.7206 0.2929 0.195 Uiso 0.50 1 calc PR . . C73 C 0.0000 0.3149(5) 0.2500 0.096(5) Uani 1 2 d SD . . C74 C 0.0000 0.2459(5) 0.2500 0.30(3) Uani 1 2 d SD . . H74A H -0.0220 0.2312 0.2271 0.364 Uiso 0.50 1 calc PR . . H74B H 0.0027 0.2312 0.2929 0.364 Uiso 0.50 1 calc PR . . H74C H 0.0193 0.2312 0.2300 0.364 Uiso 0.50 1 calc PR . . C75 C 0.3278(3) 0.2486(6) 0.0190(6) 0.099(4) Uani 1 1 d . . . H75A H 0.3434 0.2177 0.0052 0.119 Uiso 1 1 calc R . . H75B H 0.3405 0.2685 0.0564 0.119 Uiso 1 1 calc R . . C76 C 0.2873(6) 0.3662(6) 0.4978(10) 0.161(8) Uani 1 1 d . . . H76A H 0.3033 0.3760 0.5364 0.193 Uiso 1 1 calc R . . H76B H 0.2738 0.4021 0.4816 0.193 Uiso 1 1 calc R . . C77 C 0.0310(3) 0.3837(6) 0.5326(6) 0.093(4) Uani 1 1 d . . . H77A H 0.0466 0.3734 0.5714 0.111 Uiso 1 1 calc R . . H77B H 0.0202 0.3458 0.5150 0.111 Uiso 1 1 calc R . . C78 C 0.1964(14) 0.517(3) 0.7372(14) 0.47(5) Uani 1 1 d . . . H78A H 0.2009 0.4780 0.7593 0.562 Uiso 1 1 calc R . . H78B H 0.2173 0.5427 0.7407 0.562 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 0.0678(7) 0.0360(5) 0.0392(5) 0.0017(4) 0.0171(4) 0.0109(4) Cu2 0.0477(8) 0.0518(8) 0.0422(7) 0.000 0.0135(6) 0.000 Cl1 0.098(2) 0.151(3) 0.0742(19) -0.030(2) 0.0186(17) 0.043(2) Cl2 0.115(2) 0.0405(11) 0.0588(13) -0.0069(10) 0.0051(13) 0.0055(13) Cl3 0.187(4) 0.217(5) 0.0654(19) 0.015(3) -0.015(2) -0.141(4) Cl4 0.211(5) 0.110(3) 0.142(4) 0.008(3) -0.016(4) 0.007(3) Cl5 0.179(4) 0.158(4) 0.130(3) -0.043(3) 0.059(3) -0.039(3) Cl6 0.359(15) 0.306(13) 0.388(16) 0.001(13) -0.185(14) 0.056(12) Cl7 0.36(2) 1.16(7) 1.13(6) 0.93(6) -0.33(3) -0.31(3) Cl8 0.150(4) 0.190(5) 0.132(3) 0.003(3) 0.057(3) 0.001(3) Cl9 0.092(3) 0.260(6) 0.139(3) -0.090(4) 0.032(2) -0.025(3) Cl10 0.157(6) 0.262(9) 0.73(3) -0.183(13) 0.171(11) -0.067(6) Cl11 0.303(16) 1.21(7) 0.42(2) -0.39(3) 0.113(16) -0.32(3) O1 0.076(5) 0.050(3) 0.093(5) 0.013(3) 0.026(4) 0.012(3) O2 0.069(4) 0.041(3) 0.046(3) 0.005(2) 0.008(3) 0.002(3) O3 0.070(4) 0.049(3) 0.070(4) -0.019(3) 0.012(3) 0.007(3) O4 0.061(4) 0.042(3) 0.047(3) -0.001(2) 0.008(3) 0.010(3) O5 0.077(4) 0.044(3) 0.085(4) 0.010(3) 0.035(4) 0.010(3) O6 0.058(3) 0.052(3) 0.054(3) -0.004(3) 0.016(3) 0.005(3) O7 0.104(5) 0.051(4) 0.080(5) -0.002(3) -0.034(4) 0.010(4) O8 0.069(4) 0.055(4) 0.060(4) -0.002(3) 0.006(3) -0.008(3) O9 0.054(4) 0.083(5) 0.074(4) -0.010(4) 0.017(3) 0.004(4) O10 0.066(4) 0.076(4) 0.054(3) -0.003(3) 0.025(3) 0.008(3) O11 0.041(3) 0.094(5) 0.071(4) 0.003(4) 0.003(3) 0.001(3) O12 0.058(4) 0.058(3) 0.048(3) 0.002(3) 0.007(3) 0.004(3) O13 0.107(6) 0.154(8) 0.061(4) -0.020(5) 0.005(4) 0.069(6) O14 0.38(2) 0.130(9) 0.191(13) 0.024(9) 0.176(15) 0.121(13) O15 0.084(6) 0.243(13) 0.079(5) -0.023(7) 0.020(5) 0.051(7) O16 0.107(7) 0.167(9) 0.089(6) -0.036(6) 0.000(5) 0.035(6) O17 0.218(12) 0.120(8) 0.104(7) 0.017(6) -0.028(8) 0.012(8) O18 0.244(14) 0.113(7) 0.113(8) -0.015(6) 0.067(8) 0.062(8) O19 0.102(7) 0.110(8) 0.299(17) -0.059(10) 0.056(9) -0.030(6) O20 0.240(13) 0.111(7) 0.103(7) -0.063(6) 0.047(8) -0.057(8) O21 0.42(3) 0.26(2) 0.25(2) 0.022(18) -0.10(2) -0.22(2) O22 1.04(9) 0.35(3) 0.141(15) 0.069(18) 0.01(3) -0.40(5) O23 0.26(3) 1.30(15) 0.23(3) -0.02(5) -0.02(2) -0.39(6) O24 0.63(6) 0.87(9) 0.160(19) -0.19(4) 0.17(3) -0.23(6) O25 0.33(2) 0.155(12) 0.234(17) 0.013(12) 0.106(17) 0.056(14) O26 0.47(5) 0.58(6) 0.47(5) 0.15(5) 0.04(4) 0.34(5) O27 0.41(5) 0.55(6) 0.92(15) -0.23(10) -0.14(9) 0.20(5) O28 0.38(5) 1.12(13) 0.83(10) 0.80(11) -0.10(5) -0.18(6) O29 0.56(3) 0.55(3) 0.56(3) 0.022(13) -0.059(13) 0.010(13) N1 0.068(5) 0.044(4) 0.034(3) -0.002(3) 0.016(3) 0.005(3) N2 0.059(4) 0.040(3) 0.049(4) -0.001(3) 0.019(3) 0.004(3) N3 0.053(4) 0.036(3) 0.034(3) 0.000(3) 0.011(3) 0.006(3) N4 0.059(4) 0.029(3) 0.050(4) -0.002(3) 0.014(3) 0.000(3) N5 0.065(5) 0.049(4) 0.048(4) -0.004(3) 0.010(4) 0.006(4) N6 0.066(5) 0.050(4) 0.056(4) -0.001(3) 0.013(4) -0.007(4) N7 0.050(4) 0.050(4) 0.043(4) 0.007(3) 0.011(3) 0.004(3) N8 0.049(4) 0.045(4) 0.046(4) -0.003(3) 0.010(3) -0.002(3) N9 0.038(5) 0.060(7) 0.063(6) 0.000 0.005(4) 0.000 N10 0.087(8) 0.065(7) 0.064(7) 0.000 0.020(6) 0.000 C1 0.072(6) 0.038(4) 0.037(4) 0.000(3) 0.015(4) 0.011(4) C2 0.073(6) 0.035(4) 0.038(4) -0.004(3) 0.008(4) 0.001(4) C3 0.067(6) 0.048(5) 0.046(5) 0.004(4) 0.007(4) 0.011(4) C4 0.069(6) 0.056(5) 0.061(5) 0.012(4) 0.012(5) 0.012(5) C5 0.069(6) 0.053(5) 0.052(5) 0.008(4) 0.015(4) 0.012(4) C6 0.073(6) 0.042(4) 0.041(4) 0.000(3) 0.010(4) 0.000(4) C7 0.067(6) 0.035(4) 0.057(5) 0.004(4) 0.000(4) 0.000(4) C8 0.093(8) 0.049(5) 0.069(6) -0.001(5) -0.017(6) 0.003(5) C9 0.070(7) 0.032(4) 0.122(10) 0.011(5) -0.011(6) 0.001(4) C10 0.103(10) 0.059(6) 0.145(12) 0.003(7) -0.037(9) -0.008(7) C11 0.079(9) 0.073(9) 0.205(19) 0.008(11) -0.021(11) -0.032(7) C12 0.099(12) 0.074(9) 0.24(2) 0.052(13) 0.030(14) -0.016(8) C13 0.065(7) 0.071(7) 0.199(16) 0.062(9) 0.011(9) -0.003(6) C14 0.066(6) 0.047(5) 0.121(10) 0.042(6) 0.004(6) 0.006(5) C15 0.063(6) 0.056(5) 0.076(6) 0.024(5) 0.009(5) 0.005(5) C16 0.061(5) 0.038(4) 0.063(5) 0.008(4) 0.010(4) 0.008(4) C17 0.061(5) 0.036(4) 0.050(4) 0.002(3) 0.019(4) 0.000(4) C18 0.053(5) 0.037(4) 0.047(4) 0.003(3) 0.014(4) -0.001(3) C19 0.058(5) 0.041(4) 0.048(4) -0.003(3) 0.021(4) 0.009(4) C20 0.064(6) 0.089(7) 0.099(8) -0.055(6) 0.027(6) 0.001(5) C21 0.060(6) 0.101(9) 0.128(10) -0.060(8) 0.023(6) 0.002(6) C22 0.052(6) 0.090(7) 0.080(7) -0.031(6) 0.024(5) 0.000(5) C23 0.065(5) 0.038(4) 0.050(5) 0.000(3) 0.009(4) 0.001(4) C24 0.064(5) 0.038(4) 0.057(5) -0.007(4) 0.016(4) 0.001(4) C25 0.072(6) 0.044(4) 0.048(5) -0.006(4) 0.009(4) 0.014(4) C26 0.059(5) 0.044(4) 0.035(4) 0.003(3) 0.008(3) 0.008(4) C27 0.074(6) 0.037(4) 0.034(4) 0.000(3) 0.010(4) 0.007(4) C28 0.051(5) 0.054(5) 0.041(4) -0.002(4) 0.002(4) 0.007(4) C29 0.049(5) 0.055(5) 0.056(5) -0.014(4) 0.008(4) 0.010(4) C30 0.063(6) 0.065(6) 0.069(6) -0.021(5) 0.016(5) 0.002(5) C31 0.055(6) 0.056(5) 0.122(9) -0.037(6) 0.018(6) -0.005(5) C32 0.061(7) 0.105(9) 0.123(10) -0.037(8) 0.007(7) 0.009(7) C33 0.060(8) 0.126(12) 0.201(19) -0.043(13) 0.023(10) -0.022(8) C34 0.093(11) 0.130(12) 0.163(16) -0.031(12) 0.068(11) -0.010(9) C35 0.080(8) 0.096(9) 0.140(12) -0.029(8) 0.054(8) -0.023(7) C36 0.062(6) 0.067(6) 0.090(7) -0.032(6) 0.029(5) -0.011(5) C37 0.092(8) 0.068(6) 0.065(6) -0.017(5) 0.030(6) 0.002(6) C38 0.060(5) 0.052(5) 0.060(5) -0.011(4) 0.010(4) -0.001(4) C39 0.071(6) 0.050(5) 0.055(5) -0.005(4) -0.001(4) 0.006(5) C40 0.053(5) 0.037(4) 0.049(4) -0.006(3) 0.009(4) -0.003(4) C41 0.072(6) 0.036(4) 0.054(5) 0.008(4) 0.001(4) 0.001(4) C42 0.088(7) 0.060(6) 0.080(7) 0.028(5) -0.014(6) -0.013(5) C43 0.086(7) 0.051(5) 0.108(9) 0.028(6) -0.016(7) -0.020(5) C44 0.079(6) 0.043(5) 0.072(6) 0.014(4) -0.015(5) -0.013(5) C45 0.057(6) 0.046(5) 0.095(8) 0.000(5) -0.009(5) 0.014(5) C46 0.109(12) 0.093(11) 0.35(3) -0.028(15) -0.102(16) -0.003(9) C47 0.096(10) 0.074(8) 0.148(13) -0.028(8) 0.031(9) 0.024(8) C48 0.076(11) 0.150(18) 0.78(8) -0.22(3) 0.04(2) -0.010(12) C49 0.047(5) 0.066(5) 0.047(5) 0.000(4) 0.009(4) 0.004(4) C50 0.049(5) 0.074(6) 0.068(6) 0.012(5) 0.018(4) -0.002(4) C51 0.049(5) 0.084(7) 0.050(5) 0.002(5) 0.016(4) 0.012(5) C52 0.045(5) 0.068(5) 0.045(4) 0.008(4) 0.008(4) 0.009(4) C53 0.055(5) 0.059(5) 0.040(4) 0.003(4) 0.011(4) 0.006(4) C54 0.058(6) 0.074(6) 0.040(4) 0.002(4) 0.009(4) 0.019(5) C55 0.060(5) 0.065(6) 0.065(6) -0.003(5) 0.023(5) 0.014(5) C56 0.072(6) 0.075(7) 0.064(6) 0.014(5) 0.024(5) 0.016(5) C57 0.061(6) 0.075(7) 0.112(9) 0.014(7) 0.019(6) 0.030(5) C58 0.085(8) 0.075(8) 0.162(13) 0.031(8) 0.033(8) 0.038(7) C59 0.110(11) 0.054(7) 0.23(2) 0.014(11) 0.027(12) 0.040(7) C60 0.172(16) 0.086(11) 0.163(17) -0.015(11) 0.065(14) 0.027(10) C61 0.146(13) 0.069(8) 0.144(13) -0.011(8) 0.060(10) 0.033(8) C62 0.073(7) 0.069(6) 0.094(8) -0.003(6) 0.032(6) 0.029(5) C63 0.072(6) 0.069(6) 0.073(6) -0.002(5) 0.026(5) 0.021(5) C64 0.050(5) 0.063(5) 0.054(5) 0.002(4) 0.011(4) 0.009(4) C65 0.049(5) 0.074(6) 0.040(4) -0.010(4) 0.018(4) 0.000(4) C66 0.050(5) 0.059(5) 0.040(4) -0.006(4) 0.012(4) -0.008(4) C67 0.042(4) 0.055(5) 0.048(4) -0.011(4) 0.012(4) -0.003(4) C68 0.056(5) 0.072(6) 0.071(6) -0.018(5) 0.001(5) -0.011(5) C69 0.069(7) 0.054(6) 0.100(8) -0.018(6) 0.009(6) -0.019(5) C70 0.061(6) 0.057(5) 0.065(6) -0.007(4) 0.015(5) -0.007(4) C71 0.039(7) 0.049(8) 0.137(14) 0.000 0.011(8) 0.000 C72 0.087(13) 0.055(10) 0.35(4) 0.000 0.061(19) 0.000 C73 0.112(14) 0.109(14) 0.064(10) 0.000 -0.002(9) 0.000 C74 0.43(7) 0.067(16) 0.35(6) 0.000 -0.16(5) 0.000 C75 0.072(7) 0.101(9) 0.123(10) -0.039(8) 0.005(7) 0.004(7) C76 0.21(2) 0.059(8) 0.190(19) 0.018(10) -0.058(16) -0.013(10) C77 0.085(8) 0.099(9) 0.083(8) -0.002(7) -0.023(6) -0.008(7) C78 0.56(8) 0.67(9) 0.16(3) -0.03(4) 0.01(4) -0.52(8) _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 2.037(6) . ? Cu1 N1 2.037(6) . ? Cu1 N4 2.040(6) 7_556 ? Cu1 N2 2.046(6) 7_557 ? Cu1 N5 2.406(9) . ? Cu2 N7 2.014(6) 2 ? Cu2 N7 2.014(6) . ? Cu2 N8 2.059(7) 5_565 ? Cu2 N8 2.059(7) 6_566 ? Cu2 N9 2.427(11) . ? Cl1 O14 1.308(13) . ? Cl1 O15 1.390(11) . ? Cl1 O13 1.397(8) . ? Cl1 O16 1.470(9) . ? Cl2 O18 1.369(10) . ? Cl2 O19 1.382(12) . ? Cl2 O20 1.392(9) . ? Cl2 O17 1.420(10) . ? Cl3 O21 1.301(10) . ? Cl3 O23 1.326(4) . ? Cl3 O22 1.328(4) . ? Cl3 O24 1.340(11) . ? Cl4 C75 1.783(15) . ? Cl5 C75 1.694(13) . ? Cl6 C76 1.83(3) . ? Cl6 Cl7 2.46(3) . ? Cl7 C76 1.62(2) . ? Cl8 C77 1.650(13) . ? Cl9 C77 1.736(14) . ? Cl10 C78 2.06(4) . ? Cl11 C78 2.03(7) . ? O1 C6 1.209(10) . ? O2 C6 1.365(10) . ? O2 C7 1.393(10) . ? O3 C17 1.195(9) . ? O4 C17 1.332(10) . ? O4 C16 1.403(10) . ? O5 C28 1.189(10) . ? O6 C28 1.356(9) . ? O6 C29 1.400(10) . ? O7 C39 1.167(10) . ? O8 C39 1.351(11) . ? O8 C38 1.400(11) . ? O9 C54 1.188(11) . ? O10 C54 1.372(10) . ? O10 C55 1.373(11) . ? O11 C65 1.195(10) . ? O12 C65 1.358(10) . ? O12 C64 1.389(10) . ? N1 C5 1.331(11) . ? N1 C1 1.343(10) . ? N2 C22 1.323(11) . ? N2 C18 1.334(10) . ? N2 Cu1 2.045(6) 7_557 ? N3 C27 1.328(10) . ? N3 C23 1.342(10) . ? N4 C40 1.330(10) . ? N4 C44 1.342(10) . ? N4 Cu1 2.040(6) 7_556 ? N5 C45 1.100(11) . ? N6 C47 1.061(15) . ? N7 C49 1.327(10) . ? N7 C53 1.329(10) . ? N8 C66 1.316(10) . ? N8 C70 1.356(11) . ? N8 Cu2 2.059(7) 5_565 ? N9 C71 1.124(15) . ? N10 C73 1.102(4) . ? C1 C2 1.395(10) . ? C2 C3 1.359(12) . ? C2 C6 1.487(12) . ? C3 C4 1.384(12) . ? C4 C5 1.373(12) . ? C7 C8 1.357(13) . ? C7 C16 1.399(12) . ? C8 C9 1.458(16) . ? C9 C14 1.405(17) . ? C9 C10 1.428(16) . ? C10 C11 1.34(2) . ? C11 C12 1.32(2) . ? C12 C13 1.35(2) . ? C13 C14 1.412(15) . ? C14 C15 1.378(15) . ? C15 C16 1.344(12) . ? C17 C19 1.505(12) . ? C18 C19 1.369(10) . ? C19 C20 1.377(13) . ? C20 C21 1.365(14) . ? C21 C22 1.366(13) . ? C23 C24 1.385(11) . ? C24 C25 1.356(12) . ? C25 C26 1.390(11) . ? C26 C27 1.378(10) . ? C26 C28 1.486(11) . ? C29 C30 1.372(12) . ? C29 C38 1.395(12) . ? C30 C31 1.400(14) . ? C31 C32 1.404(15) . ? C31 C36 1.431(16) . ? C32 C33 1.35(2) . ? C33 C34 1.40(2) . ? C34 C35 1.32(2) . ? C35 C36 1.372(15) . ? C36 C37 1.405(14) . ? C37 C38 1.346(13) . ? C39 C41 1.517(13) . ? C40 C41 1.369(11) . ? C41 C42 1.376(12) . ? C42 C43 1.360(14) . ? C43 C44 1.396(13) . ? C45 C46 1.458(18) . ? C47 C48 1.55(2) . ? C49 C50 1.373(12) . ? C50 C51 1.374(13) . ? C51 C52 1.365(12) . ? C52 C53 1.385(11) . ? C52 C54 1.476(13) . ? C55 C56 1.375(13) . ? C55 C64 1.418(13) . ? C56 C57 1.402(15) . ? C57 C62 1.406(16) . ? C57 C58 1.464(16) . ? C58 C59 1.39(2) . ? C59 C60 1.40(2) . ? C60 C61 1.31(2) . ? C61 C62 1.436(16) . ? C62 C63 1.396(14) . ? C63 C64 1.332(13) . ? C65 C67 1.465(12) . ? C66 C67 1.404(11) . ? C67 C68 1.386(12) . ? C68 C69 1.389(14) . ? C69 C70 1.356(14) . ? C71 C72 1.46(2) . ? C73 C74 1.534(4) . ? 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 88.2(2) . . ? N3 Cu1 N4 90.2(2) . 7_556 ? N1 Cu1 N4 177.5(3) . 7_556 ? N3 Cu1 N2 176.5(3) . 7_557 ? N1 Cu1 N2 92.4(2) . 7_557 ? N4 Cu1 N2 89.1(2) 7_556 7_557 ? N3 Cu1 N5 90.4(2) . . ? N1 Cu1 N5 88.8(3) . . ? N4 Cu1 N5 93.1(3) 7_556 . ? N2 Cu1 N5 93.1(3) 7_557 . ? N7 Cu2 N7 177.3(4) 2 . ? N7 Cu2 N8 87.6(3) 2 5_565 ? N7 Cu2 N8 92.3(3) . 5_565 ? N7 Cu2 N8 92.3(3) 2 6_566 ? N7 Cu2 N8 87.6(3) . 6_566 ? N8 Cu2 N8 176.8(4) 5_565 6_566 ? N7 Cu2 N9 91.37(19) 2 . ? N7 Cu2 N9 91.36(19) . . ? N8 Cu2 N9 91.62(18) 5_565 . ? N8 Cu2 N9 91.62(18) 6_566 . ? O14 Cl1 O15 109.3(8) . . ? O14 Cl1 O13 107.4(7) . . ? O15 Cl1 O13 114.0(7) . . ? O14 Cl1 O16 117.4(11) . . ? O15 Cl1 O16 103.7(6) . . ? O13 Cl1 O16 105.2(5) . . ? O18 Cl2 O19 110.7(7) . . ? O18 Cl2 O20 112.4(8) . . ? O19 Cl2 O20 107.1(8) . . ? O18 Cl2 O17 104.4(7) . . ? O19 Cl2 O17 119.1(9) . . ? O20 Cl2 O17 103.1(7) . . ? O21 Cl3 O23 111.2(8) . . ? O21 Cl3 O22 110.3(7) . . ? O23 Cl3 O22 109.2(5) . . ? O21 Cl3 O24 109.7(4) . . ? O23 Cl3 O24 108.2(7) . . ? O22 Cl3 O24 108.2(7) . . ? C76 Cl6 Cl7 41.1(11) . . ? C76 Cl7 Cl6 48.3(12) . . ? C6 O2 C7 116.8(7) . . ? C17 O4 C16 118.0(6) . . ? C28 O6 C29 117.1(6) . . ? C39 O8 C38 119.8(7) . . ? C54 O10 C55 118.2(8) . . ? C65 O12 C64 119.6(7) . . ? C5 N1 C1 117.7(7) . . ? C5 N1 Cu1 123.1(6) . . ? C1 N1 Cu1 118.6(6) . . ? C22 N2 C18 118.5(7) . . ? C22 N2 Cu1 120.8(6) . 7_557 ? C18 N2 Cu1 120.5(5) . 7_557 ? C27 N3 C23 118.6(6) . . ? C27 N3 Cu1 119.2(5) . . ? C23 N3 Cu1 122.0(5) . . ? C40 N4 C44 118.4(7) . . ? C40 N4 Cu1 120.7(5) . 7_556 ? C44 N4 Cu1 120.9(6) . 7_556 ? C45 N5 Cu1 179.0(7) . . ? C49 N7 C53 117.7(7) . . ? C49 N7 Cu2 121.1(6) . . ? C53 N7 Cu2 120.5(5) . . ? C66 N8 C70 117.4(7) . . ? C66 N8 Cu2 120.5(5) . 5_565 ? C70 N8 Cu2 121.9(6) . 5_565 ? C71 N9 Cu2 180.000(2) . . ? N1 C1 C2 122.3(8) . . ? C3 C2 C1 119.1(8) . . ? C3 C2 C6 124.8(7) . . ? C1 C2 C6 116.0(8) . . ? C2 C3 C4 118.6(8) . . ? C5 C4 C3 119.3(9) . . ? N1 C5 C4 122.9(9) . . ? O1 C6 O2 123.5(8) . . ? O1 C6 C2 125.3(8) . . ? O2 C6 C2 111.2(8) . . ? C8 C7 O2 120.9(9) . . ? C8 C7 C16 120.5(9) . . ? O2 C7 C16 118.4(7) . . ? C7 C8 C9 118.0(10) . . ? C14 C9 C10 118.7(12) . . ? C14 C9 C8 119.7(10) . . ? C10 C9 C8 121.6(13) . . ? C11 C10 C9 119.0(16) . . ? C12 C11 C10 123.0(16) . . ? C11 C12 C13 120.5(16) . . ? C12 C13 C14 121.3(17) . . ? C15 C14 C9 118.8(9) . . ? C15 C14 C13 123.8(13) . . ? C9 C14 C13 117.4(13) . . ? C16 C15 C14 121.3(10) . . ? C15 C16 C7 121.5(9) . . ? C15 C16 O4 119.9(8) . . ? C7 C16 O4 118.5(7) . . ? O3 C17 O4 124.9(8) . . ? O3 C17 C19 124.6(8) . . ? O4 C17 C19 110.6(6) . . ? N2 C18 C19 122.1(8) . . ? C18 C19 C20 118.8(8) . . ? C18 C19 C17 121.2(7) . . ? C20 C19 C17 120.0(7) . . ? C21 C20 C19 118.9(8) . . ? C20 C21 C22 119.0(10) . . ? N2 C22 C21 122.6(10) . . ? N3 C23 C24 121.7(8) . . ? C25 C24 C23 119.8(8) . . ? C24 C25 C26 118.5(7) . . ? C27 C26 C25 119.0(8) . . ? C27 C26 C28 116.6(7) . . ? C25 C26 C28 124.4(7) . . ? N3 C27 C26 122.4(7) . . ? O5 C28 O6 124.0(8) . . ? O5 C28 C26 125.2(7) . . ? O6 C28 C26 110.7(7) . . ? C30 C29 C38 120.5(9) . . ? C30 C29 O6 121.3(8) . . ? C38 C29 O6 118.2(7) . . ? C29 C30 C31 119.4(9) . . ? C30 C31 C32 123.8(12) . . ? C30 C31 C36 120.2(9) . . ? C32 C31 C36 115.8(11) . . ? C33 C32 C31 122.9(14) . . ? C32 C33 C34 119.1(14) . . ? C35 C34 C33 120.1(14) . . ? C34 C35 C36 122.5(15) . . ? C35 C36 C37 123.1(11) . . ? C35 C36 C31 119.5(10) . . ? C37 C36 C31 117.4(9) . . ? C38 C37 C36 121.4(10) . . ? C37 C38 C29 120.9(9) . . ? C37 C38 O8 119.4(9) . . ? C29 C38 O8 119.5(8) . . ? O7 C39 O8 125.7(9) . . ? O7 C39 C41 125.1(8) . . ? O8 C39 C41 109.2(7) . . ? N4 C40 C41 122.2(7) . . ? C40 C41 C42 119.4(8) . . ? C40 C41 C39 120.8(8) . . ? C42 C41 C39 119.6(8) . . ? C43 C42 C41 119.6(9) . . ? C42 C43 C44 118.1(9) . . ? N4 C44 C43 122.2(9) . . ? N5 C45 C46 177.5(16) . . ? N6 C47 C48 178(2) . . ? N7 C49 C50 122.8(9) . . ? C49 C50 C51 118.8(9) . . ? C52 C51 C50 119.3(8) . . ? C51 C52 C53 118.1(8) . . ? C51 C52 C54 124.9(8) . . ? C53 C52 C54 116.9(8) . . ? N7 C53 C52 123.2(8) . . ? O9 C54 O10 124.0(9) . . ? O9 C54 C52 125.1(8) . . ? O10 C54 C52 110.9(8) . . ? O10 C55 C56 123.2(9) . . ? O10 C55 C64 118.0(8) . . ? C56 C55 C64 118.8(9) . . ? C55 C56 C57 119.6(9) . . ? C56 C57 C62 120.9(10) . . ? C56 C57 C58 120.8(12) . . ? C62 C57 C58 118.4(12) . . ? C59 C58 C57 116.8(15) . . ? C58 C59 C60 123.3(14) . . ? C61 C60 C59 120.5(16) . . ? C60 C61 C62 120.5(16) . . ? C63 C62 C57 117.6(10) . . ? C63 C62 C61 121.8(12) . . ? C57 C62 C61 120.5(11) . . ? C64 C63 C62 121.8(10) . . ? C63 C64 O12 120.2(8) . . ? C63 C64 C55 121.2(9) . . ? O12 C64 C55 118.4(8) . . ? O11 C65 O12 123.0(9) . . ? O11 C65 C67 125.9(8) . . ? O12 C65 C67 111.1(7) . . ? N8 C66 C67 123.7(8) . . ? C68 C67 C66 117.9(8) . . ? C68 C67 C65 120.0(8) . . ? C66 C67 C65 122.1(7) . . ? C67 C68 C69 118.1(9) . . ? C70 C69 C68 120.0(9) . . ? C69 C70 N8 122.8(9) . . ? N9 C71 C72 180.000(5) . . ? N10 C73 C74 180.000(3) . . ? Cl5 C75 Cl4 112.0(7) . . ? Cl7 C76 Cl6 90.5(19) . . ? Cl8 C77 Cl9 113.8(8) . . ? Cl11 C78 Cl10 77(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.946 _refine_diff_density_min -1.231 _refine_diff_density_rms 0.140 _database_code_depnum_ccdc_archive 'CCDC 928712' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_rr #TrackingRef '03-ace-CH3CN.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C153 H157 B6 Cl12 Cu3 F24 N15 O44' _chemical_formula_weight 4046.82 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 38.6764(4) _cell_length_b 22.1804(2) _cell_length_c 21.8948(4) _cell_angle_alpha 90.00 _cell_angle_beta 96.2840(10) _cell_angle_gamma 90.00 _cell_volume 18669.8(4) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8084 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 19.95 _exptl_crystal_description BLOCK _exptl_crystal_colour purple _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.42 _exptl_crystal_size_min 0.32 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.440 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 8276 _exptl_absorpt_coefficient_mu 0.611 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7705 _exptl_absorpt_correction_T_max 0.8284 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Bruker Breeze CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 141709 _diffrn_reflns_av_R_equivalents 0.1253 _diffrn_reflns_av_sigmaI/netI 0.0840 _diffrn_reflns_limit_h_min -47 _diffrn_reflns_limit_h_max 47 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.06 _diffrn_reflns_theta_max 26.00 _reflns_number_total 18363 _reflns_number_gt 9623 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker APEX2' _computing_data_reduction 'Bruker APEX2' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.2000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18363 _refine_ls_number_parameters 1156 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.1970 _refine_ls_R_factor_gt 0.1195 _refine_ls_wR_factor_ref 0.3911 _refine_ls_wR_factor_gt 0.3300 _refine_ls_goodness_of_fit_ref 1.283 _refine_ls_restrained_S_all 1.288 _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 0.25561(2) 0.28578(4) 0.25382(4) 0.0379(3) Uani 1 1 d . . . Cu2 Cu 0.0000 -0.01596(6) 0.7500 0.0442(4) Uani 1 2 d S . . F1 F 0.08975(16) 0.1313(3) 0.7706(3) 0.094(2) Uani 1 1 d . . . F2 F 0.06562(18) 0.1689(4) 0.6822(3) 0.123(3) Uani 1 1 d . . . F3 F 0.12118(16) 0.1531(4) 0.6926(3) 0.116(3) Uani 1 1 d . . . F4 F 0.1029(4) 0.2227(4) 0.7506(6) 0.243(8) Uani 1 1 d . . . F5 F 0.2953(2) 0.9224(3) 0.7960(6) 0.223(7) Uani 1 1 d D . . F6 F 0.2813(4) 1.0167(4) 0.7941(4) 0.265(9) Uani 1 1 d D . . F7 F 0.2934(3) 0.9728(6) 0.7111(3) 0.328(13) Uani 1 1 d D . . F8 F 0.3343(2) 0.9896(5) 0.7846(7) 0.293(9) Uani 1 1 d DU . . F9 F 0.0807(3) 0.8236(4) 0.7085(5) 0.215(6) Uani 1 1 d D . . F10 F 0.1074(5) 0.7790(6) 0.7876(5) 0.306(11) Uani 1 1 d D . . F11 F 0.0821(3) 0.7261(4) 0.7125(8) 0.350(15) Uani 1 1 d D . . F12 F 0.1289(3) 0.7757(6) 0.7008(9) 0.330(13) Uani 1 1 d D . . B1 B 0.0953(3) 0.1705(7) 0.7261(6) 0.082(4) Uani 1 1 d . . . B2 B 0.3010(2) 0.9754(3) 0.7713(3) 0.134(7) Uani 1 1 d DU . . B3 B 0.0998(2) 0.7763(4) 0.7272(5) 0.220(19) Uani 1 1 d D . . Cl1 Cl -0.05134(16) 0.0946(3) 1.0209(3) 0.170(2) Uani 1 1 d . . . Cl2 Cl 0.00319(12) 0.0661(3) 0.9517(2) 0.162(2) Uani 1 1 d . . . Cl3 Cl 0.28710(19) 0.20813(18) -0.0343(2) 0.171(2) Uani 1 1 d . . . Cl4 Cl 0.3106(3) 0.2980(3) 0.0452(3) 0.274(5) Uani 1 1 d . . . Cl5 Cl 0.1897(3) 0.3278(5) 0.5650(5) 0.277(4) Uani 1 1 d D . . Cl6 Cl 0.2305(5) 0.3441(8) 0.4886(6) 0.513(14) Uani 1 1 d D . . O1 O 0.26338(15) 0.5001(3) 0.0506(3) 0.0606(16) Uani 1 1 d . . . O2 O 0.21994(13) 0.4351(2) 0.0646(2) 0.0414(12) Uani 1 1 d . . . O3 O 0.18351(17) 0.3625(3) -0.1013(3) 0.0636(17) Uani 1 1 d . . . O4 O 0.22266(13) 0.4305(2) -0.0605(2) 0.0441(12) Uani 1 1 d . . . O5 O 0.15564(16) 0.2974(3) 0.4105(3) 0.0589(16) Uani 1 1 d . . . O6 O 0.13979(13) 0.2027(2) 0.4309(2) 0.0473(13) Uani 1 1 d . . . O7 O 0.1428(2) 0.1005(3) 0.5179(3) 0.090(2) Uani 1 1 d . . . O8 O 0.14883(15) 0.1944(2) 0.5573(3) 0.0519(14) Uani 1 1 d . . . O9 O 0.19827(14) 0.3373(2) 0.2301(3) 0.0495(13) Uani 1 1 d . . . O10 O 0.12514(16) 0.0827(3) 0.9530(3) 0.0625(16) Uani 1 1 d . . . O11 O 0.07467(14) 0.1242(2) 0.9123(2) 0.0503(14) Uani 1 1 d . . . O12 O 0.02981(16) 0.1679(3) 1.0679(3) 0.0609(16) Uani 1 1 d . . . O13 O 0.08091(15) 0.1373(2) 1.0375(3) 0.0555(15) Uani 1 1 d . . . O14 O 0.0000 -0.1322(4) 0.7500 0.061(2) Uani 1 2 d S . . O15 O 0.1614(3) 0.9753(6) 0.6401(9) 0.217(8) Uani 1 1 d . . . H15B H 0.1595 0.9708 0.6018 0.260 Uiso 1 1 d R . . H15C H 0.1453 0.9975 0.6499 0.260 Uiso 1 1 d R . . O16 O 0.1471(5) 0.9223(12) 0.7372(10) 0.409(19) Uani 1 1 d D . . H16A H 0.1391 0.9008 0.7074 0.491 Uiso 1 1 d R . . H16B H 0.1352 0.9173 0.7666 0.491 Uiso 1 1 d R . . O17 O 0.2002(6) 0.9857(10) 0.7440(12) 0.329(8) Uani 1 1 d D . . H17A H 0.2204 0.9735 0.7398 0.395 Uiso 1 1 d R . . H17B H 0.1885 0.9565 0.7627 0.395 Uiso 1 1 d R . . O18 O 0.0239(6) 0.6327(11) 1.2253(12) 0.329(8) Uani 1 1 d U . . H18B H 0.0411 0.6438 1.2309 0.395 Uiso 1 1 d R . . H18C H 0.0154 0.6180 1.1911 0.395 Uiso 1 1 d R . . O19 O 0.0461(5) 0.4035(13) 1.2669(18) 0.45(2) Uani 1 1 d . . . H19B H 0.0274 0.3928 1.2799 0.539 Uiso 1 1 d R . . H19C H 0.0446 0.3960 1.2207 0.539 Uiso 1 1 d R . . O20 O 0.0000 0.5000 1.0000 0.79(8) Uani 1 2 d S . . H20B H -0.0137 0.4795 0.9757 0.946 Uiso 0.50 1 d PR . . H20C H 0.0073 0.5008 0.9618 0.946 Uiso 0.50 1 d PR . . O21 O 0.0829(11) 0.5163(18) 1.230(2) 0.61(4) Uani 1 1 d . . . H21A H 0.0666 0.5366 1.2421 0.733 Uiso 1 1 d R . . H21B H 0.0799 0.5130 1.1918 0.733 Uiso 1 1 d R . . O22 O 0.0586(8) 0.4466(14) 1.1459(16) 0.397(15) Uani 1 1 d U . . H22B H 0.0414 0.4638 1.1587 0.476 Uiso 1 1 d R . . H22C H 0.0549 0.4435 1.1017 0.476 Uiso 1 1 d R . . O23 O 0.0602(11) 0.592(2) 1.170(2) 0.58(3) Uani 1 1 d . . . H23B H 0.0460 0.5694 1.1848 0.697 Uiso 1 1 d R . . H23C H 0.0581 0.5891 1.1317 0.697 Uiso 1 1 d R . . N1 N 0.27869(16) 0.3417(3) 0.1974(3) 0.0415(15) Uani 1 1 d . . . N2 N 0.25942(16) 0.2732(3) -0.1839(3) 0.0410(15) Uani 1 1 d . . . N3 N 0.23260(16) 0.2309(3) 0.3115(3) 0.0378(14) Uani 1 1 d . . . N4 N 0.23093(16) 0.1543(3) 0.6769(3) 0.0405(14) Uani 1 1 d . . . N5 N 0.31040(16) 0.2269(3) 0.2759(3) 0.0456(16) Uani 1 1 d D . . N6 N 0.04415(17) -0.0218(3) 0.8111(3) 0.0450(16) Uani 1 1 d . . . N7 N 0.03117(18) 0.0183(3) 1.1823(3) 0.0468(16) Uani 1 1 d . . . N8 N 0.0000 0.0908(4) 0.7500 0.044(2) Uani 1 2 d S . . C1 C 0.2595(2) 0.3748(3) 0.1544(3) 0.0397(17) Uani 1 1 d . . . H1A H 0.2352 0.3680 0.1476 0.048 Uiso 1 1 calc R . . C2 C 0.2742(2) 0.4179(3) 0.1203(4) 0.0446(18) Uani 1 1 d . . . C3 C 0.3098(2) 0.4266(5) 0.1277(5) 0.073(3) Uani 1 1 d . . . H3A H 0.3205 0.4559 0.1044 0.088 Uiso 1 1 calc R . . C4 C 0.3294(2) 0.3904(5) 0.1709(5) 0.082(3) Uani 1 1 d . . . H4A H 0.3541 0.3935 0.1762 0.098 Uiso 1 1 calc R . . C5 C 0.3130(2) 0.3509(4) 0.2052(4) 0.061(2) Uani 1 1 d . . . H5A H 0.3265 0.3287 0.2362 0.073 Uiso 1 1 calc R . . C6 C 0.2527(2) 0.4565(3) 0.0750(3) 0.0427(18) Uani 1 1 d . . . C7 C 0.1959(2) 0.4681(3) 0.0263(3) 0.0407(17) Uani 1 1 d . . . C8 C 0.1717(2) 0.5005(3) 0.0518(4) 0.0445(19) Uani 1 1 d . . . H8A H 0.1727 0.5038 0.0952 0.053 Uiso 1 1 calc R . . C9 C 0.1447(2) 0.5295(3) 0.0135(4) 0.047(2) Uani 1 1 d . . . C10 C 0.1175(2) 0.5612(4) 0.0378(4) 0.060(2) Uani 1 1 d . . . H10A H 0.1171 0.5642 0.0810 0.071 Uiso 1 1 calc R . . C11 C 0.0924(3) 0.5868(4) 0.0000(5) 0.067(3) Uani 1 1 d . . . H11A H 0.0743 0.6076 0.0171 0.081 Uiso 1 1 calc R . . C12 C 0.0918(2) 0.5844(4) -0.0632(5) 0.062(2) Uani 1 1 d . . . H12A H 0.0735 0.6032 -0.0888 0.075 Uiso 1 1 calc R . . C13 C 0.1177(2) 0.5547(4) -0.0885(4) 0.055(2) Uani 1 1 d . . . H13A H 0.1174 0.5534 -0.1320 0.066 Uiso 1 1 calc R . . C14 C 0.1444(2) 0.5264(3) -0.0520(4) 0.047(2) Uani 1 1 d . . . C15 C 0.1714(2) 0.4937(3) -0.0761(4) 0.0443(19) Uani 1 1 d . . . H15A H 0.1724 0.4923 -0.1193 0.053 Uiso 1 1 calc R . . C16 C 0.1961(2) 0.4641(3) -0.0377(4) 0.0414(18) Uani 1 1 d . . . C17 C 0.2125(2) 0.3802(3) -0.0928(3) 0.0420(18) Uani 1 1 d . . . C18 C 0.2927(2) 0.2913(3) -0.1724(3) 0.0460(19) Uani 1 1 d . . . H18A H 0.3100 0.2721 -0.1931 0.055 Uiso 1 1 calc R . . C19 C 0.3025(2) 0.3375(4) -0.1311(4) 0.053(2) Uani 1 1 d . . . H19A H 0.3263 0.3478 -0.1217 0.064 Uiso 1 1 calc R . . C20 C 0.2770(2) 0.3683(3) -0.1039(4) 0.0463(19) Uani 1 1 d . . . H20A H 0.2829 0.4013 -0.0771 0.056 Uiso 1 1 calc R . . C21 C 0.2429(2) 0.3501(3) -0.1165(3) 0.0401(17) Uani 1 1 d . . . C22 C 0.2351(2) 0.3021(3) -0.1560(3) 0.0398(17) Uani 1 1 d . . . H22A H 0.2116 0.2891 -0.1637 0.048 Uiso 1 1 calc R . . C23 C 0.20761(19) 0.2518(3) 0.3424(3) 0.0385(17) Uani 1 1 d . . . H23A H 0.2027 0.2937 0.3407 0.046 Uiso 1 1 calc R . . C24 C 0.18837(19) 0.2151(3) 0.3769(3) 0.0392(16) Uani 1 1 d . . . C25 C 0.1967(2) 0.1544(3) 0.3817(4) 0.049(2) Uani 1 1 d . . . H25A H 0.1842 0.1281 0.4056 0.058 Uiso 1 1 calc R . . C26 C 0.2230(2) 0.1332(4) 0.3519(4) 0.053(2) Uani 1 1 d . . . H26A H 0.2293 0.0919 0.3549 0.064 Uiso 1 1 calc R . . C27 C 0.2406(2) 0.1718(3) 0.3170(4) 0.0468(19) Uani 1 1 d . . . H27A H 0.2589 0.1563 0.2962 0.056 Uiso 1 1 calc R . . C28 C 0.1602(2) 0.2446(3) 0.4068(3) 0.0416(17) Uani 1 1 d . . . C29 C 0.1130(2) 0.2239(3) 0.4634(3) 0.0418(18) Uani 1 1 d . . . C30 C 0.0839(2) 0.2499(3) 0.4355(4) 0.0462(19) Uani 1 1 d . . . H30A H 0.0813 0.2549 0.3921 0.055 Uiso 1 1 calc R . . C31 C 0.0574(2) 0.2695(4) 0.4700(4) 0.049(2) Uani 1 1 d . . . C32 C 0.0269(2) 0.2985(4) 0.4433(5) 0.060(2) Uani 1 1 d . . . H32A H 0.0233 0.3045 0.4001 0.072 Uiso 1 1 calc R . . C33 C 0.0023(2) 0.3183(5) 0.4802(6) 0.073(3) Uani 1 1 d . . . H33A H -0.0178 0.3389 0.4621 0.088 Uiso 1 1 calc R . . C34 C 0.0064(3) 0.3090(5) 0.5405(6) 0.081(3) Uani 1 1 d . . . H34A H -0.0114 0.3222 0.5641 0.097 Uiso 1 1 calc R . . C35 C 0.0346(3) 0.2814(4) 0.5698(5) 0.069(3) Uani 1 1 d . . . H35A H 0.0366 0.2756 0.6130 0.083 Uiso 1 1 calc R . . C36 C 0.0617(2) 0.2610(4) 0.5346(4) 0.055(2) Uani 1 1 d . . . C37 C 0.0922(2) 0.2332(4) 0.5622(4) 0.056(2) Uani 1 1 d . . . H37A H 0.0951 0.2267 0.6053 0.067 Uiso 1 1 calc R . . C38 C 0.1173(2) 0.2156(3) 0.5275(4) 0.0445(18) Uani 1 1 d . . . C39 C 0.1586(2) 0.1366(4) 0.5504(4) 0.055(2) Uani 1 1 d . . . C40 C 0.2034(2) 0.1657(3) 0.6365(3) 0.0428(18) Uani 1 1 d . . . H40A H 0.1919 0.2035 0.6383 0.051 Uiso 1 1 calc R . . C41 C 0.1907(2) 0.1244(4) 0.5917(4) 0.051(2) Uani 1 1 d . . . C42 C 0.2079(3) 0.0688(4) 0.5880(5) 0.081(3) Uani 1 1 d . . . H42A H 0.1998 0.0399 0.5578 0.098 Uiso 1 1 calc R . . C43 C 0.2366(3) 0.0573(4) 0.6293(5) 0.078(3) Uani 1 1 d . . . H43A H 0.2489 0.0204 0.6276 0.093 Uiso 1 1 calc R . . C44 C 0.2473(2) 0.1004(4) 0.6734(4) 0.057(2) Uani 1 1 d . . . H44A H 0.2669 0.0918 0.7022 0.068 Uiso 1 1 calc R . . C45 C 0.3334(2) 0.1961(4) 0.2832(5) 0.063(2) Uani 1 1 d D . . C46 C 0.3612(3) 0.1588(6) 0.2842(13) 0.239(16) Uani 1 1 d D . . H46A H 0.3630 0.1344 0.3218 0.287 Uiso 1 1 calc R . . H46B H 0.3825 0.1827 0.2833 0.287 Uiso 1 1 calc R . . H46C H 0.3583 0.1321 0.2483 0.287 Uiso 1 1 calc R . . C47 C 0.1526(3) 0.3647(5) 0.1564(5) 0.083(3) Uani 1 1 d . . . H47A H 0.1682 0.3496 0.1276 0.099 Uiso 1 1 calc R . . H47B H 0.1473 0.4072 0.1477 0.099 Uiso 1 1 calc R . . H47C H 0.1310 0.3412 0.1518 0.099 Uiso 1 1 calc R . . C48 C 0.1692(2) 0.3588(3) 0.2186(4) 0.0477(19) Uani 1 1 d . . . C49 C 0.1492(3) 0.3795(5) 0.2701(5) 0.078(3) Uani 1 1 d . . . H49A H 0.1632 0.3730 0.3096 0.093 Uiso 1 1 calc R . . H49B H 0.1275 0.3565 0.2691 0.093 Uiso 1 1 calc R . . H49C H 0.1438 0.4225 0.2650 0.093 Uiso 1 1 calc R . . C50 C 0.0651(2) -0.0713(4) 0.8149(4) 0.053(2) Uani 1 1 d . . . H50A H 0.0585 -0.1044 0.7886 0.064 Uiso 1 1 calc R . . C51 C 0.0945(3) -0.0762(4) 0.8536(5) 0.062(2) Uani 1 1 d . . . H51A H 0.1077 -0.1123 0.8548 0.075 Uiso 1 1 calc R . . C52 C 0.1055(3) -0.0282(4) 0.8920(5) 0.063(2) Uani 1 1 d . . . H52A H 0.1257 -0.0313 0.9207 0.076 Uiso 1 1 calc R . . C53 C 0.0856(2) 0.0251(3) 0.8865(4) 0.046(2) Uani 1 1 d . . . C54 C 0.0550(2) 0.0246(3) 0.8470(3) 0.0438(19) Uani 1 1 d . . . H54A H 0.0408 0.0596 0.8455 0.053 Uiso 1 1 calc R . . C55 C 0.0982(2) 0.0785(4) 0.9220(4) 0.047(2) Uani 1 1 d . . . C56 C 0.0817(2) 0.1814(3) 0.9383(4) 0.0445(18) Uani 1 1 d . . . C57 C 0.0846(2) 0.2279(4) 0.9001(4) 0.055(2) Uani 1 1 d . . . H57A H 0.0844 0.2211 0.8572 0.066 Uiso 1 1 calc R . . C58 C 0.0879(2) 0.2873(4) 0.9237(4) 0.055(2) Uani 1 1 d . . . C59 C 0.0897(3) 0.3387(4) 0.8856(5) 0.070(3) Uani 1 1 d . . . H59A H 0.0901 0.3328 0.8427 0.084 Uiso 1 1 calc R . . C60 C 0.0908(4) 0.3949(5) 0.9075(6) 0.098(4) Uani 1 1 d . . . H60A H 0.0915 0.4284 0.8807 0.118 Uiso 1 1 calc R . . C61 C 0.0907(3) 0.4036(5) 0.9710(6) 0.081(3) Uani 1 1 d . . . H61A H 0.0909 0.4434 0.9870 0.098 Uiso 1 1 calc R . . C62 C 0.0904(2) 0.3561(4) 1.0097(5) 0.064(2) Uani 1 1 d . . . H62A H 0.0915 0.3633 1.0527 0.077 Uiso 1 1 calc R . . C63 C 0.0883(2) 0.2955(4) 0.9878(4) 0.050(2) Uani 1 1 d . . . C64 C 0.0867(2) 0.2460(4) 1.0265(4) 0.051(2) Uani 1 1 d . . . H64A H 0.0880 0.2513 1.0697 0.061 Uiso 1 1 calc R . . C65 C 0.0830(2) 0.1892(4) 1.0013(4) 0.0470(19) Uani 1 1 d . . . C66 C 0.0531(2) 0.1318(4) 1.0684(3) 0.050(2) Uani 1 1 d . . . C67 C 0.0303(2) 0.0673(3) 1.1453(3) 0.0438(18) Uani 1 1 d . . . H67A H 0.0129 0.0972 1.1480 0.053 Uiso 1 1 calc R . . C68 C 0.0545(2) 0.0742(3) 1.1036(4) 0.049(2) Uani 1 1 d . . . C69 C 0.0798(2) 0.0306(4) 1.0993(4) 0.056(2) Uani 1 1 d . . . H69A H 0.0968 0.0353 1.0716 0.068 Uiso 1 1 calc R . . C70 C 0.0795(3) -0.0187(4) 1.1354(4) 0.063(3) Uani 1 1 d . . . H70A H 0.0962 -0.0497 1.1325 0.076 Uiso 1 1 calc R . . C71 C 0.0548(2) -0.0243(3) 1.1767(4) 0.051(2) Uani 1 1 d . . . H71A H 0.0549 -0.0594 1.2016 0.061 Uiso 1 1 calc R . . C72 C 0.0000 0.1427(7) 0.7500 0.067(4) Uani 1 2 d S . . C73 C 0.0000 0.2031(10) 0.7500 0.36(4) Uani 1 2 d S . . H73A H -0.0210 0.2178 0.7255 0.432 Uiso 0.50 1 calc PR . . H73B H 0.0206 0.2178 0.7322 0.432 Uiso 0.50 1 calc PR . . H73C H 0.0004 0.2178 0.7923 0.432 Uiso 0.50 1 calc PR . . C74 C 0.0000 -0.1863(6) 0.7500 0.062(3) Uani 1 2 d S . . C75 C -0.0081(4) -0.2239(5) 0.6924(5) 0.094(4) Uani 1 1 d . . . H75A H -0.0066 -0.2668 0.7031 0.113 Uiso 1 1 calc R . . H75B H 0.0086 -0.2145 0.6632 0.113 Uiso 1 1 calc R . . H75C H -0.0317 -0.2147 0.6736 0.113 Uiso 1 1 calc R . . C76 C -0.0246(4) 0.1127(10) 0.9655(9) 0.170(8) Uani 1 1 d . . . H76A H -0.0395 0.1209 0.9267 0.203 Uiso 1 1 calc R . . H76B H -0.0125 0.1508 0.9780 0.203 Uiso 1 1 calc R . . C77 C 0.3232(3) 0.2388(13) 0.0012(13) 0.260(18) Uani 1 1 d . . . H77A H 0.3383 0.2537 -0.0294 0.312 Uiso 1 1 calc R . . H77B H 0.3364 0.2086 0.0276 0.312 Uiso 1 1 calc R . . C78 C 0.2208(6) 0.2842(7) 0.5345(10) 0.238(12) Uani 1 1 d DU . . H78A H 0.2404 0.2722 0.5651 0.286 Uiso 1 1 calc R . . H78B H 0.2111 0.2488 0.5111 0.286 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 0.0486(6) 0.0340(5) 0.0320(5) 0.0009(4) 0.0094(4) 0.0013(4) Cu2 0.0583(9) 0.0419(7) 0.0347(7) 0.000 0.0159(6) 0.000 F1 0.099(5) 0.125(5) 0.056(3) 0.018(3) 0.006(3) -0.043(4) F2 0.082(5) 0.183(8) 0.103(5) 0.066(5) 0.005(4) -0.005(5) F3 0.067(4) 0.217(8) 0.064(4) 0.031(5) 0.006(3) -0.017(5) F4 0.47(2) 0.085(6) 0.217(12) -0.047(7) 0.216(14) -0.118(9) F5 0.128(8) 0.080(5) 0.47(2) 0.097(9) 0.069(11) -0.001(5) F6 0.49(2) 0.216(11) 0.090(6) 0.001(7) 0.052(10) 0.239(15) F7 0.335(19) 0.57(3) 0.069(6) -0.029(11) -0.004(9) 0.32(2) F8 0.272(15) 0.281(15) 0.333(17) -0.022(13) 0.068(13) -0.062(12) F9 0.241(14) 0.188(11) 0.204(12) 0.006(9) -0.029(10) 0.098(10) F10 0.46(3) 0.268(18) 0.159(13) 0.035(12) -0.090(16) -0.012(18) F11 0.157(12) 0.200(14) 0.66(4) -0.18(2) -0.099(18) 0.044(10) F12 0.159(11) 0.245(15) 0.63(4) -0.096(19) 0.228(19) -0.011(10) B1 0.071(8) 0.110(11) 0.067(8) 0.022(8) 0.018(7) -0.019(8) B2 0.159(14) 0.116(12) 0.127(13) -0.076(11) 0.022(11) 0.016(11) B3 0.15(2) 0.19(3) 0.28(4) 0.16(3) -0.13(3) -0.05(2) Cl1 0.177(5) 0.185(5) 0.157(5) 0.018(4) 0.056(4) -0.001(4) Cl2 0.120(3) 0.242(6) 0.128(4) -0.062(4) 0.036(3) -0.020(4) Cl3 0.304(8) 0.102(3) 0.105(3) 0.000(2) 0.014(4) -0.040(4) Cl4 0.520(17) 0.151(5) 0.149(6) -0.017(4) 0.022(8) -0.021(7) Cl5 0.263(9) 0.256(9) 0.296(11) -0.007(8) -0.043(8) -0.012(7) Cl6 0.61(3) 0.61(3) 0.256(12) 0.154(15) -0.202(15) -0.37(2) O1 0.056(4) 0.052(3) 0.073(4) 0.025(3) 0.004(3) -0.006(3) O2 0.051(3) 0.037(3) 0.036(3) 0.005(2) 0.003(2) 0.002(2) O3 0.057(4) 0.051(3) 0.085(5) -0.016(3) 0.020(3) -0.008(3) O4 0.049(3) 0.043(3) 0.042(3) 0.001(2) 0.012(2) 0.008(2) O5 0.061(4) 0.052(4) 0.069(4) -0.002(3) 0.028(3) 0.001(3) O6 0.044(3) 0.049(3) 0.050(3) 0.004(3) 0.013(3) 0.002(2) O7 0.120(6) 0.054(4) 0.083(5) -0.015(4) -0.046(5) 0.013(4) O8 0.058(4) 0.046(3) 0.050(3) -0.003(3) -0.003(3) 0.006(3) O9 0.047(3) 0.050(3) 0.053(3) 0.004(3) 0.010(3) 0.005(3) O10 0.046(4) 0.071(4) 0.071(4) -0.009(3) 0.006(3) 0.003(3) O11 0.057(4) 0.045(3) 0.049(3) -0.005(3) 0.008(3) -0.003(3) O12 0.064(4) 0.064(4) 0.058(4) 0.014(3) 0.023(3) 0.006(3) O13 0.065(4) 0.054(3) 0.051(3) 0.010(3) 0.023(3) 0.003(3) O14 0.087(6) 0.042(5) 0.056(5) 0.000 0.023(5) 0.000 O15 0.088(8) 0.163(11) 0.41(3) 0.051(13) 0.058(11) 0.024(7) O16 0.33(3) 0.64(5) 0.30(3) 0.12(3) 0.23(3) 0.11(3) O17 0.372(14) 0.300(12) 0.320(14) -0.007(11) 0.064(12) 0.040(11) O18 0.372(14) 0.300(12) 0.320(14) -0.007(11) 0.064(12) 0.040(11) O19 0.126(15) 0.48(4) 0.74(7) 0.23(4) 0.02(2) 0.051(18) O20 0.14(2) 0.126(18) 2.0(2) 0.02(5) -0.33(6) -0.060(16) O21 0.49(6) 0.40(5) 0.90(11) 0.21(6) -0.09(7) 0.02(4) O22 0.393(19) 0.402(19) 0.39(2) -0.065(14) 0.034(14) 0.047(14) O23 0.57(7) 0.71(9) 0.47(6) 0.17(6) 0.08(5) 0.19(6) N1 0.042(4) 0.042(3) 0.041(4) 0.006(3) 0.007(3) 0.002(3) N2 0.047(4) 0.044(3) 0.032(3) 0.001(3) 0.006(3) 0.003(3) N3 0.045(4) 0.033(3) 0.036(3) 0.002(3) 0.007(3) 0.007(3) N4 0.047(4) 0.038(3) 0.035(3) 0.004(3) 0.001(3) -0.001(3) N5 0.042(4) 0.043(4) 0.053(4) -0.001(3) 0.010(3) 0.007(3) N6 0.064(4) 0.037(3) 0.037(3) 0.001(3) 0.016(3) 0.003(3) N7 0.062(4) 0.045(4) 0.035(3) -0.003(3) 0.012(3) -0.003(3) N8 0.055(6) 0.027(5) 0.052(6) 0.000 0.020(4) 0.000 C1 0.046(4) 0.036(4) 0.039(4) -0.003(3) 0.010(3) 0.001(3) C2 0.049(5) 0.044(4) 0.043(4) 0.006(4) 0.012(4) -0.001(4) C3 0.056(6) 0.082(7) 0.083(7) 0.046(6) 0.017(5) -0.001(5) C4 0.040(5) 0.097(8) 0.110(9) 0.053(7) 0.012(5) 0.004(5) C5 0.049(5) 0.068(6) 0.066(6) 0.032(5) 0.007(4) 0.000(4) C6 0.049(5) 0.042(4) 0.039(4) 0.006(3) 0.013(4) 0.006(4) C7 0.052(5) 0.031(4) 0.039(4) -0.001(3) 0.002(4) -0.001(3) C8 0.061(5) 0.037(4) 0.036(4) -0.001(3) 0.009(4) -0.001(4) C9 0.051(5) 0.037(4) 0.055(5) -0.007(4) 0.011(4) -0.001(4) C10 0.067(6) 0.051(5) 0.061(6) -0.015(4) 0.009(5) 0.012(5) C11 0.067(6) 0.049(5) 0.087(8) -0.010(5) 0.014(6) 0.015(5) C12 0.057(6) 0.046(5) 0.082(7) 0.006(5) -0.001(5) 0.013(4) C13 0.059(6) 0.048(5) 0.058(5) 0.008(4) 0.005(4) 0.002(4) C14 0.056(5) 0.028(4) 0.058(5) 0.005(3) 0.007(4) 0.001(3) C15 0.065(5) 0.035(4) 0.036(4) 0.005(3) 0.014(4) -0.003(4) C16 0.051(5) 0.031(4) 0.043(4) 0.003(3) 0.012(4) 0.005(3) C17 0.055(5) 0.031(4) 0.043(4) -0.001(3) 0.016(4) 0.001(4) C18 0.053(5) 0.048(5) 0.038(4) 0.000(4) 0.010(4) 0.006(4) C19 0.045(5) 0.052(5) 0.064(5) -0.009(4) 0.009(4) -0.001(4) C20 0.053(5) 0.043(4) 0.042(4) -0.003(4) 0.002(4) -0.002(4) C21 0.051(5) 0.035(4) 0.035(4) 0.005(3) 0.009(3) 0.004(3) C22 0.051(5) 0.041(4) 0.028(4) 0.001(3) 0.011(3) -0.001(3) C23 0.053(5) 0.029(4) 0.033(4) -0.002(3) 0.005(3) 0.005(3) C24 0.040(4) 0.040(4) 0.037(4) 0.000(3) 0.003(3) 0.002(3) C25 0.052(5) 0.034(4) 0.061(5) 0.009(4) 0.016(4) -0.002(4) C26 0.057(5) 0.038(4) 0.066(6) 0.008(4) 0.014(4) 0.001(4) C27 0.043(5) 0.043(4) 0.055(5) 0.008(4) 0.014(4) 0.008(4) C28 0.056(5) 0.034(4) 0.035(4) 0.005(3) 0.009(3) 0.002(4) C29 0.043(5) 0.041(4) 0.043(4) 0.002(3) 0.010(3) -0.002(3) C30 0.048(5) 0.051(5) 0.040(4) 0.005(4) 0.006(4) -0.006(4) C31 0.037(5) 0.051(5) 0.060(5) 0.001(4) 0.006(4) -0.004(4) C32 0.054(6) 0.051(5) 0.074(6) -0.001(5) 0.000(5) -0.002(4) C33 0.044(6) 0.075(7) 0.104(9) -0.005(6) 0.018(6) 0.001(5) C34 0.061(7) 0.088(8) 0.100(9) -0.004(7) 0.040(6) 0.004(6) C35 0.060(6) 0.071(6) 0.082(7) -0.001(5) 0.036(5) 0.010(5) C36 0.056(5) 0.055(5) 0.057(5) 0.004(4) 0.021(4) -0.002(4) C37 0.068(6) 0.058(5) 0.044(5) 0.008(4) 0.019(4) 0.010(4) C38 0.046(5) 0.042(4) 0.046(4) 0.003(4) 0.005(4) 0.002(4) C39 0.068(6) 0.043(5) 0.051(5) -0.008(4) -0.011(4) 0.001(4) C40 0.055(5) 0.037(4) 0.038(4) 0.003(3) 0.011(4) 0.003(4) C41 0.066(6) 0.042(4) 0.043(5) -0.003(4) -0.003(4) 0.007(4) C42 0.112(9) 0.058(6) 0.067(7) -0.024(5) -0.020(6) 0.018(6) C43 0.087(8) 0.057(6) 0.084(8) -0.016(5) -0.017(6) 0.030(5) C44 0.060(6) 0.049(5) 0.059(5) -0.011(4) -0.005(4) 0.008(4) C45 0.061(6) 0.056(5) 0.075(7) 0.008(5) 0.018(5) -0.007(5) C46 0.078(11) 0.092(11) 0.56(5) 0.097(18) 0.107(19) 0.040(8) C47 0.080(8) 0.087(8) 0.079(7) 0.019(6) 0.001(6) 0.003(6) C48 0.049(5) 0.041(4) 0.054(5) 0.009(4) 0.008(4) -0.001(4) C49 0.082(7) 0.075(7) 0.082(7) -0.008(6) 0.036(6) 0.012(6) C50 0.061(6) 0.039(4) 0.062(5) -0.003(4) 0.019(5) 0.005(4) C51 0.069(6) 0.039(5) 0.081(7) 0.004(5) 0.017(5) 0.011(4) C52 0.063(6) 0.061(6) 0.068(6) 0.009(5) 0.017(5) 0.013(5) C53 0.057(5) 0.037(4) 0.047(4) 0.010(3) 0.020(4) 0.001(4) C54 0.053(5) 0.043(4) 0.036(4) 0.004(3) 0.007(4) 0.008(4) C55 0.051(5) 0.054(5) 0.041(4) 0.004(4) 0.021(4) -0.001(4) C56 0.052(5) 0.040(4) 0.044(4) 0.001(4) 0.013(4) -0.004(4) C57 0.062(6) 0.057(5) 0.048(5) -0.002(4) 0.010(4) -0.008(4) C58 0.053(5) 0.053(5) 0.060(5) 0.010(4) 0.011(4) -0.011(4) C59 0.096(8) 0.050(5) 0.067(6) 0.012(5) 0.020(6) -0.016(5) C60 0.146(12) 0.061(7) 0.087(9) 0.013(6) 0.012(8) -0.035(7) C61 0.096(8) 0.049(6) 0.100(9) 0.001(6) 0.013(7) -0.020(5) C62 0.060(6) 0.064(6) 0.070(6) -0.018(5) 0.015(5) -0.017(5) C63 0.044(5) 0.052(5) 0.055(5) -0.001(4) 0.002(4) -0.015(4) C64 0.052(5) 0.057(5) 0.044(5) 0.003(4) 0.010(4) 0.000(4) C65 0.047(5) 0.052(5) 0.044(4) 0.009(4) 0.016(4) -0.003(4) C66 0.063(6) 0.055(5) 0.034(4) -0.001(4) 0.015(4) -0.009(4) C67 0.062(5) 0.037(4) 0.033(4) 0.003(3) 0.013(4) 0.000(4) C68 0.061(5) 0.043(4) 0.045(4) -0.001(4) 0.016(4) 0.001(4) C69 0.063(6) 0.060(5) 0.052(5) 0.007(4) 0.029(4) 0.004(4) C70 0.071(6) 0.059(5) 0.065(6) 0.009(5) 0.031(5) 0.008(5) C71 0.066(6) 0.041(4) 0.050(5) 0.002(4) 0.022(4) 0.003(4) C72 0.056(8) 0.065(9) 0.085(10) 0.000 0.032(7) 0.000 C73 0.17(3) 0.072(15) 0.89(12) 0.000 0.31(5) 0.000 C74 0.081(10) 0.061(8) 0.047(7) 0.000 0.021(7) 0.000 C75 0.146(11) 0.079(7) 0.057(6) -0.024(6) 0.009(7) -0.035(7) C76 0.081(11) 0.24(2) 0.181(18) -0.101(17) -0.017(11) -0.015(12) C77 0.034(7) 0.39(3) 0.36(3) 0.31(3) 0.028(12) 0.020(13) C78 0.211(18) 0.29(2) 0.208(18) -0.055(16) -0.007(15) -0.028(16) _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 2.026(6) . ? Cu1 N3 2.029(6) . ? Cu1 N4 2.041(6) 7_556 ? Cu1 N2 2.049(6) 7 ? Cu2 N7 2.012(6) 5_557 ? Cu2 N7 2.012(6) 6 ? Cu2 N6 2.055(7) . ? Cu2 N6 2.055(7) 2_556 ? Cu2 N8 2.368(8) . ? F1 B1 1.340(13) . ? F2 B1 1.416(15) . ? F3 B1 1.359(15) . ? F4 B1 1.295(17) . ? F5 B2 1.322(3) . ? F6 B2 1.322(3) . ? F7 B2 1.321(3) . ? F8 B2 1.328(3) . ? F9 B3 1.323(3) . ? F10 B3 1.325(3) . ? F11 B3 1.326(3) . ? F12 B3 1.323(3) . ? Cl1 C76 1.73(2) . ? Cl2 C76 1.546(17) . ? Cl3 C77 1.67(2) . ? Cl4 C77 1.73(3) . ? Cl5 C78 1.735(5) . ? Cl5 Cl6 2.45(2) . ? Cl6 C78 1.732(5) . ? O1 C6 1.199(9) . ? O2 C6 1.349(9) . ? O2 C7 1.392(9) . ? O3 C17 1.183(9) . ? O4 C17 1.356(9) . ? O4 C16 1.406(8) . ? O5 C28 1.189(8) . ? O6 C28 1.363(9) . ? O6 C29 1.401(8) . ? O7 C39 1.194(10) . ? O8 C39 1.351(10) . ? O8 C38 1.399(10) . ? O9 C48 1.221(9) . ? O10 C55 1.183(10) . ? O11 C55 1.363(10) . ? O11 C56 1.404(9) . ? O12 C66 1.205(10) . ? O13 C66 1.336(9) . ? O13 C65 1.406(9) . ? O14 C74 1.199(14) . ? N1 C5 1.334(10) . ? N1 C1 1.348(9) . ? N2 C22 1.339(9) . ? N2 C18 1.344(10) . ? N2 Cu1 2.048(6) 7 ? N3 C23 1.322(9) . ? N3 C27 1.349(9) . ? N4 C40 1.333(10) . ? N4 C44 1.359(10) . ? N4 Cu1 2.041(6) 7_556 ? N5 C45 1.121(4) . ? N6 C54 1.333(10) . ? N6 C50 1.362(10) . ? N7 C71 1.331(10) . ? N7 C67 1.352(9) . ? N7 Cu2 2.012(6) 5_557 ? N8 C72 1.150(15) . ? C1 C2 1.374(10) . ? C2 C3 1.384(12) . ? C2 C6 1.492(11) . ? C3 C4 1.399(13) . ? C4 C5 1.356(12) . ? C7 C8 1.348(10) . ? C7 C16 1.403(10) . ? C8 C9 1.419(11) . ? C9 C10 1.418(11) . ? C9 C14 1.435(12) . ? C10 C11 1.331(13) . ? C11 C12 1.382(14) . ? C12 C13 1.366(12) . ? C13 C14 1.385(12) . ? C14 C15 1.420(11) . ? C15 C16 1.368(11) . ? C17 C21 1.495(10) . ? C18 C19 1.391(11) . ? C19 C20 1.387(11) . ? C20 C21 1.378(11) . ? C21 C22 1.386(10) . ? C23 C24 1.383(10) . ? C24 C25 1.387(10) . ? C24 C28 1.481(10) . ? C25 C26 1.352(11) . ? C26 C27 1.373(10) . ? C29 C30 1.350(11) . ? C29 C38 1.407(11) . ? C30 C31 1.408(11) . ? C31 C32 1.414(12) . ? C31 C36 1.418(12) . ? C32 C33 1.385(13) . ? C33 C34 1.330(16) . ? C34 C35 1.351(15) . ? C35 C36 1.440(11) . ? C36 C37 1.405(12) . ? C37 C38 1.355(11) . ? C39 C41 1.479(12) . ? C40 C41 1.390(11) . ? C41 C42 1.406(12) . ? C42 C43 1.377(14) . ? C43 C44 1.389(13) . ? C45 C46 1.355(4) . ? C47 C48 1.448(13) . ? C48 C49 1.507(12) . ? C50 C51 1.346(13) . ? C51 C52 1.393(13) . ? C52 C53 1.408(11) . ? C53 C54 1.387(12) . ? C53 C55 1.472(12) . ? C56 C57 1.341(11) . ? C56 C65 1.385(11) . ? C57 C58 1.416(12) . ? C58 C63 1.413(12) . ? C58 C59 1.418(12) . ? C59 C60 1.335(14) . ? C60 C61 1.403(16) . ? C61 C62 1.354(14) . ? C62 C63 1.428(12) . ? C63 C64 1.392(11) . ? C64 C65 1.376(11) . ? C66 C68 1.491(11) . ? C67 C68 1.386(10) . ? C68 C69 1.384(11) . ? C69 C70 1.351(12) . ? C70 C71 1.389(11) . ? C72 C73 1.34(2) . ? C74 C75 1.517(12) . ? C74 C75 1.517(12) 2_556 ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Cu1 N3 179.0(3) . . ? N1 Cu1 N4 87.7(2) . 7_556 ? N3 Cu1 N4 91.3(2) . 7_556 ? N1 Cu1 N2 92.5(2) . 7 ? N3 Cu1 N2 88.5(2) . 7 ? N4 Cu1 N2 178.2(3) 7_556 7 ? N7 Cu2 N7 177.0(4) 5_557 6 ? N7 Cu2 N6 92.3(3) 5_557 . ? N7 Cu2 N6 87.5(3) 6 . ? N7 Cu2 N6 87.5(3) 5_557 2_556 ? N7 Cu2 N6 92.3(3) 6 2_556 ? N6 Cu2 N6 172.8(3) . 2_556 ? N7 Cu2 N8 91.49(18) 5_557 . ? N7 Cu2 N8 91.49(18) 6 . ? N6 Cu2 N8 93.59(17) . . ? N6 Cu2 N8 93.59(17) 2_556 . ? F4 B1 F1 109.1(11) . . ? F4 B1 F3 109.4(11) . . ? F1 B1 F3 113.2(12) . . ? F4 B1 F2 115.7(15) . . ? F1 B1 F2 107.1(9) . . ? F3 B1 F2 102.5(10) . . ? F7 B2 F5 110.0(4) . . ? F7 B2 F6 109.4(3) . . ? F5 B2 F6 109.5(4) . . ? F7 B2 F8 109.5(4) . . ? F5 B2 F8 108.7(3) . . ? F6 B2 F8 109.8(4) . . ? F12 B3 F9 110.3(4) . . ? F12 B3 F10 109.2(3) . . ? F9 B3 F10 109.2(3) . . ? F12 B3 F11 109.0(3) . . ? F9 B3 F11 109.6(4) . . ? F10 B3 F11 109.5(4) . . ? C78 Cl5 Cl6 45.0(5) . . ? C78 Cl6 Cl5 45.1(5) . . ? C6 O2 C7 118.0(5) . . ? C17 O4 C16 116.1(6) . . ? C28 O6 C29 117.4(6) . . ? C39 O8 C38 120.5(6) . . ? C55 O11 C56 120.8(7) . . ? C66 O13 C65 117.4(6) . . ? C5 N1 C1 118.0(6) . . ? C5 N1 Cu1 120.9(5) . . ? C1 N1 Cu1 120.9(5) . . ? C22 N2 C18 118.5(6) . . ? C22 N2 Cu1 119.3(5) . 7 ? C18 N2 Cu1 121.2(5) . 7 ? C23 N3 C27 117.9(6) . . ? C23 N3 Cu1 120.1(5) . . ? C27 N3 Cu1 121.8(5) . . ? C40 N4 C44 118.3(7) . . ? C40 N4 Cu1 119.3(5) . 7_556 ? C44 N4 Cu1 122.2(5) . 7_556 ? C54 N6 C50 116.1(7) . . ? C54 N6 Cu2 121.4(5) . . ? C50 N6 Cu2 122.4(6) . . ? C71 N7 C67 119.3(6) . . ? C71 N7 Cu2 121.5(5) . 5_557 ? C67 N7 Cu2 118.9(5) . 5_557 ? C72 N8 Cu2 180.000(2) . . ? N1 C1 C2 122.1(7) . . ? C1 C2 C3 119.8(8) . . ? C1 C2 C6 122.0(7) . . ? C3 C2 C6 118.2(7) . . ? C2 C3 C4 117.3(8) . . ? C5 C4 C3 119.5(9) . . ? N1 C5 C4 123.2(8) . . ? O1 C6 O2 124.9(7) . . ? O1 C6 C2 124.4(8) . . ? O2 C6 C2 110.7(6) . . ? C8 C7 O2 118.7(7) . . ? C8 C7 C16 121.8(7) . . ? O2 C7 C16 119.4(6) . . ? C7 C8 C9 119.7(7) . . ? C10 C9 C8 122.1(8) . . ? C10 C9 C14 118.3(8) . . ? C8 C9 C14 119.6(7) . . ? C11 C10 C9 120.0(9) . . ? C10 C11 C12 122.5(9) . . ? C13 C12 C11 119.5(9) . . ? C12 C13 C14 121.2(9) . . ? C13 C14 C15 123.3(8) . . ? C13 C14 C9 118.6(7) . . ? C15 C14 C9 118.1(7) . . ? C16 C15 C14 120.5(7) . . ? C15 C16 C7 120.3(7) . . ? C15 C16 O4 121.5(7) . . ? C7 C16 O4 118.2(7) . . ? O3 C17 O4 124.9(7) . . ? O3 C17 C21 124.4(7) . . ? O4 C17 C21 110.7(7) . . ? N2 C18 C19 122.0(7) . . ? C20 C19 C18 119.1(8) . . ? C21 C20 C19 118.6(7) . . ? C20 C21 C22 119.3(7) . . ? C20 C21 C17 124.9(7) . . ? C22 C21 C17 115.8(7) . . ? N2 C22 C21 122.5(7) . . ? N3 C23 C24 122.7(6) . . ? C23 C24 C25 118.6(7) . . ? C23 C24 C28 116.6(6) . . ? C25 C24 C28 124.8(7) . . ? C26 C25 C24 118.7(7) . . ? C25 C26 C27 119.8(7) . . ? N3 C27 C26 122.1(7) . . ? O5 C28 O6 123.2(7) . . ? O5 C28 C24 126.0(7) . . ? O6 C28 C24 110.9(6) . . ? C30 C29 O6 122.7(7) . . ? C30 C29 C38 120.6(7) . . ? O6 C29 C38 116.7(7) . . ? C29 C30 C31 120.6(7) . . ? C30 C31 C32 122.8(8) . . ? C30 C31 C36 118.8(8) . . ? C32 C31 C36 118.4(8) . . ? C33 C32 C31 119.9(10) . . ? C34 C33 C32 121.0(10) . . ? C33 C34 C35 123.0(10) . . ? C34 C35 C36 119.1(10) . . ? C37 C36 C31 119.2(7) . . ? C37 C36 C35 122.1(9) . . ? C31 C36 C35 118.6(9) . . ? C38 C37 C36 120.3(8) . . ? C37 C38 O8 118.6(7) . . ? C37 C38 C29 120.4(8) . . ? O8 C38 C29 120.8(7) . . ? O7 C39 O8 125.0(8) . . ? O7 C39 C41 125.6(8) . . ? O8 C39 C41 109.3(7) . . ? N4 C40 C41 122.5(7) . . ? C40 C41 C42 119.1(8) . . ? C40 C41 C39 121.2(7) . . ? C42 C41 C39 119.6(8) . . ? C43 C42 C41 118.5(9) . . ? C42 C43 C44 119.1(9) . . ? N4 C44 C43 122.6(8) . . ? N5 C45 C46 172.8(15) . . ? O9 C48 C47 122.3(8) . . ? O9 C48 C49 120.1(8) . . ? C47 C48 C49 117.7(9) . . ? C51 C50 N6 123.9(8) . . ? C50 C51 C52 120.0(8) . . ? C51 C52 C53 117.5(9) . . ? C54 C53 C52 117.8(8) . . ? C54 C53 C55 123.2(7) . . ? C52 C53 C55 119.0(8) . . ? N6 C54 C53 124.5(7) . . ? O10 C55 O11 124.2(8) . . ? O10 C55 C53 125.8(8) . . ? O11 C55 C53 109.9(8) . . ? C57 C56 C65 121.9(7) . . ? C57 C56 O11 117.9(7) . . ? C65 C56 O11 120.0(7) . . ? C56 C57 C58 119.9(8) . . ? C63 C58 C57 118.2(7) . . ? C63 C58 C59 119.1(8) . . ? C57 C58 C59 122.7(9) . . ? C60 C59 C58 122.6(10) . . ? C59 C60 C61 118.8(10) . . ? C62 C61 C60 120.9(10) . . ? C61 C62 C63 121.8(9) . . ? C64 C63 C58 120.5(7) . . ? C64 C63 C62 122.9(8) . . ? C58 C63 C62 116.7(8) . . ? C65 C64 C63 119.1(8) . . ? C64 C65 C56 120.3(7) . . ? C64 C65 O13 122.2(7) . . ? C56 C65 O13 117.5(7) . . ? O12 C66 O13 125.3(7) . . ? O12 C66 C68 124.0(7) . . ? O13 C66 C68 110.8(7) . . ? N7 C67 C68 120.5(7) . . ? C69 C68 C67 120.1(7) . . ? C69 C68 C66 123.3(7) . . ? C67 C68 C66 116.5(7) . . ? C70 C69 C68 118.3(7) . . ? C69 C70 C71 120.2(8) . . ? N7 C71 C70 121.6(8) . . ? N8 C72 C73 180.000(6) . . ? O14 C74 C75 123.4(6) . . ? O14 C74 C75 123.4(6) . 2_556 ? C75 C74 C75 113.3(13) . 2_556 ? Cl2 C76 Cl1 117.7(15) . . ? Cl3 C77 Cl4 107.2(10) . . ? Cl6 C78 Cl5 90.0(10) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.315 _refine_diff_density_min -1.475 _refine_diff_density_rms 0.149 _database_code_depnum_ccdc_archive 'CCDC 928713'