# Supplementary Material (ESI) for Chemical Communications # This journal is © The Royal Society of Chemistry 2009 data_global _journal_name_full Chem.Commun. _journal_coden_Cambridge 0182 _journal_volume ? _journal_page_first ? _journal_year ? _publ_contact_author_name 'Stephen Loeb' _publ_contact_author_email LOEB@UWINDSOR.CA _publ_section_title ; Eliminating the need for independent counterions in the construction of metal organic rotaxane frameworks (MORFs) ; loop_ _publ_author_name 'Stephen Loeb' 'Christopher B. Caputo' 'Lisa K. Knight' 'Elizabeth Viljoen' 'V. Nicholas Vukotic' # Attachment 'CCDC 736643 (B911889F-R2).txt' data_vnv139 _database_code_depnum_ccdc_archive 'CCDC 736643' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C56 H85 N5 O22 S2' _chemical_formula_weight 1244.41 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' S S 0.1246 0.1234 '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 10.3418(19) _cell_length_b 12.310(2) _cell_length_c 13.586(2) _cell_angle_alpha 73.597(2) _cell_angle_beta 69.539(2) _cell_angle_gamma 76.445(2) _cell_volume 1536.7(5) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.22 _exptl_crystal_size_min 0.18 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.345 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_absorpt_coefficient_mu 0.168 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.869131 _exptl_absorpt_correction_T_max 1.000000 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 14583 _diffrn_reflns_av_R_equivalents 0.0398 _diffrn_reflns_av_sigmaI/netI 0.0503 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.64 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5386 _reflns_number_gt 3889 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker SHELXTL XCIF' _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^)+(0.1141P)^2^+2.3114P] 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 5386 _refine_ls_number_parameters 412 _refine_ls_number_restraints 5 _refine_ls_R_factor_all 0.1078 _refine_ls_R_factor_gt 0.0808 _refine_ls_wR_factor_ref 0.2327 _refine_ls_wR_factor_gt 0.2101 _refine_ls_goodness_of_fit_ref 1.034 _refine_ls_restrained_S_all 1.038 _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 N1 N 0.9766(4) 0.6797(3) 0.3135(3) 0.0434(9) Uani 1 1 d . . . N2 N 0.6343(3) 0.4929(3) 0.8664(2) 0.0359(8) Uani 1 1 d . . . C1 C 0.8590(5) 0.6353(4) 0.3481(3) 0.0459(11) Uani 1 1 d . . . H1A H 0.8212 0.6296 0.2956 0.055 Uiso 1 1 calc R . . C2 C 0.7875(4) 0.5969(4) 0.4555(3) 0.0391(9) Uani 1 1 d . . . H2A H 0.7053 0.5638 0.4754 0.047 Uiso 1 1 calc R . . C3 C 0.8391(4) 0.6079(3) 0.5338(3) 0.0322(8) Uani 1 1 d . . . C4 C 0.9606(4) 0.6560(3) 0.4982(3) 0.0380(9) Uani 1 1 d . . . H4A H 0.9990 0.6656 0.5488 0.046 Uiso 1 1 calc R . . C5 C 1.0253(4) 0.6900(4) 0.3893(3) 0.0407(10) Uani 1 1 d . . . H5A H 1.1086 0.7223 0.3669 0.049 Uiso 1 1 calc R . . C6 C 0.7671(4) 0.5677(3) 0.6499(3) 0.0327(8) Uani 1 1 d . . . C7 C 0.6754(4) 0.4880(3) 0.6858(3) 0.0366(9) Uani 1 1 d . . . H7A H 0.6583 0.4581 0.6350 0.044 Uiso 1 1 calc R . . C8 C 0.6100(4) 0.4524(3) 0.7932(3) 0.0372(9) Uani 1 1 d . . . H8A H 0.5469 0.3987 0.8164 0.045 Uiso 1 1 calc R . . C9 C 0.7234(4) 0.5678(4) 0.8351(3) 0.0413(10) Uani 1 1 d . . . H9A H 0.7411 0.5942 0.8878 0.050 Uiso 1 1 calc R . . C10 C 0.7896(4) 0.6072(3) 0.7282(3) 0.0366(9) Uani 1 1 d . . . H10A H 0.8513 0.6616 0.7074 0.044 Uiso 1 1 calc R . . C11 C 0.5617(4) 0.4542(4) 0.9828(3) 0.0418(10) Uani 1 1 d . . . H11A H 0.6267 0.4422 1.0251 0.050 Uiso 1 1 calc R . . H11B H 0.5284 0.3808 0.9958 0.050 Uiso 1 1 calc R . . S1 S 0.45930(12) 0.75349(9) 0.37497(8) 0.0422(3) Uani 1 1 d . . . O1 O 0.5289(4) 0.8447(3) 0.2957(3) 0.0718(11) Uani 1 1 d . . . O2 O 0.3119(4) 0.7687(3) 0.3864(3) 0.0641(10) Uani 1 1 d . . . O3 O 0.5276(3) 0.6410(3) 0.3591(2) 0.0472(7) Uani 1 1 d . . . O4 O 0.3330(3) 0.6274(2) 0.7883(2) 0.0383(7) Uani 1 1 d . . . O5 O 0.2508(4) 0.4123(3) 0.9463(2) 0.0558(9) Uani 1 1 d . . . O6 O 0.5603(5) 0.7723(3) 0.9896(4) 0.0823(13) Uani 1 1 d . . . O7 O 0.4681(3) 0.7754(2) 0.8021(2) 0.0424(7) Uani 1 1 d . . . C12 C 0.4723(4) 0.7745(3) 0.7010(3) 0.0355(9) Uani 1 1 d . . . C13 C 0.5403(5) 0.8465(4) 0.6081(3) 0.0435(10) Uani 1 1 d . . . H13A H 0.5892 0.9004 0.6126 0.052 Uiso 1 1 calc R . . C14 C 0.5376(4) 0.8404(4) 0.5076(3) 0.0418(10) Uani 1 1 d . . . H14A H 0.5846 0.8902 0.4442 0.050 Uiso 1 1 calc R . . C15 C 0.4674(4) 0.7630(3) 0.5004(3) 0.0351(9) Uani 1 1 d . . . C16 C 0.3998(4) 0.6887(3) 0.5939(3) 0.0343(9) Uani 1 1 d . . . H16A H 0.3534 0.6335 0.5885 0.041 Uiso 1 1 calc R . . C17 C 0.4001(4) 0.6947(3) 0.6927(3) 0.0338(8) Uani 1 1 d . . . C18 C 0.2438(4) 0.5573(4) 0.7818(3) 0.0390(9) Uani 1 1 d . . . H18A H 0.3003 0.4981 0.7411 0.047 Uiso 1 1 calc R . . H18B H 0.1765 0.6051 0.7441 0.047 Uiso 1 1 calc R . . C19 C 0.1676(5) 0.5020(4) 0.8941(3) 0.0477(11) Uani 1 1 d . . . H19A H 0.1281 0.5613 0.9374 0.057 Uiso 1 1 calc R . . H19B H 0.0886 0.4712 0.8919 0.057 Uiso 1 1 calc R . . C20 C 0.2659(5) 0.3046(4) 0.9232(3) 0.0486(11) Uani 1 1 d . . . H20A H 0.3293 0.3048 0.8492 0.058 Uiso 1 1 calc R . . H20B H 0.1739 0.2905 0.9266 0.058 Uiso 1 1 calc R . . C21 C 0.6781(7) 0.7868(5) 1.0012(5) 0.0789(19) Uani 1 1 d . . . H21A H 0.6605 0.8594 1.0249 0.095 Uiso 1 1 calc R . . H21B H 0.7502 0.7953 0.9298 0.095 Uiso 1 1 calc R . . C22 C 0.4923(6) 0.8660(4) 0.9270(4) 0.0603(13) Uani 1 1 d . . . H22A H 0.5142 0.9381 0.9317 0.072 Uiso 1 1 calc R . . H22B H 0.3901 0.8674 0.9591 0.072 Uiso 1 1 calc R . . C23 C 0.5309(5) 0.8632(4) 0.8116(4) 0.0501(11) Uani 1 1 d . . . H23A H 0.4977 0.9385 0.7706 0.060 Uiso 1 1 calc R . . H23B H 0.6337 0.8471 0.7814 0.060 Uiso 1 1 calc R . . O1M O 1.1055(4) 0.6717(3) 0.0902(3) 0.0703(11) Uani 1 1 d . . . H1MD H 1.0867 0.6841 0.1518 0.105 Uiso 1 1 calc R . . C1M C 1.1054(6) 0.7759(5) 0.0148(4) 0.0659(14) Uani 1 1 d . . . H1MA H 1.1540 0.8264 0.0292 0.099 Uiso 1 1 calc R . . H1MB H 1.0089 0.8124 0.0200 0.099 Uiso 1 1 calc R . . H1MC H 1.1533 0.7622 -0.0578 0.099 Uiso 1 1 calc R . . O2M O 1.2349(5) 1.0796(5) 0.8530(4) 0.0996(15) Uani 1 1 d . . . H2MD H 1.3147 1.0944 0.8138 0.149 Uiso 1 1 calc R . . C2M C 1.1776(7) 1.0294(6) 0.7981(6) 0.0884(19) Uani 1 1 d . . . H2MC H 1.1520 1.0881 0.7394 0.133 Uiso 1 1 calc R . . H2MB H 1.0944 0.9974 0.8486 0.133 Uiso 1 1 calc R . . H2MA H 1.2471 0.9683 0.7684 0.133 Uiso 1 1 calc R . . O3M O 0.7824(16) 1.0370(7) 0.7419(10) 0.285(7) Uani 1 1 d D . . H3MD H 0.8169 0.9673 0.7500 0.427 Uiso 1 1 calc R . . C3M C 0.7811(11) 1.0789(8) 0.8291(5) 0.134(4) Uani 1 1 d D . . H3MC H 0.8254 1.1482 0.8014 0.200 Uiso 1 1 calc R . . H3MB H 0.8327 1.0204 0.8732 0.200 Uiso 1 1 calc R . . H3MA H 0.6845 1.0971 0.8732 0.200 Uiso 1 1 calc R . . O4M O 1.0701(14) 1.1728(11) 0.2932(13) 0.095(4) Uani 0.50 1 d PD A -1 H4MD H 1.1023 1.1925 0.3332 0.143 Uiso 0.50 1 calc PR A -1 C4M C 0.9292(13) 1.1503(15) 0.351(2) 0.34(3) Uani 0.50 1 d PD A -1 H4MA H 0.8929 1.1846 0.4142 0.503 Uiso 0.50 1 calc PR A -1 H4MB H 0.9289 1.0674 0.3744 0.503 Uiso 0.50 1 calc PR A -1 H4MC H 0.8701 1.1837 0.3039 0.503 Uiso 0.50 1 calc PR A -1 O1D O 0.9787(15) 0.7751(9) 0.7211(15) 0.100(5) Uani 0.50 1 d PD B -1 N1D N 1.0412(11) 0.9311(11) 0.5935(11) 0.102(4) Uani 0.50 1 d PD B -1 C1D C 0.9151(17) 0.9550(15) 0.5576(14) 0.116(3) Uani 0.50 1 d PD B -1 H1DA H 0.8430 0.9124 0.6124 0.174 Uiso 0.50 1 calc PR B -1 H1DB H 0.9395 0.9312 0.4895 0.174 Uiso 0.50 1 calc PR B -1 H1DC H 0.8797 1.0372 0.5472 0.174 Uiso 0.50 1 calc PR B -1 C2D C 1.1528(18) 1.0022(14) 0.5353(14) 0.116(3) Uani 0.50 1 d PD B -1 H2DA H 1.2238 0.9808 0.5726 0.174 Uiso 0.50 1 calc PR B -1 H2DB H 1.1133 1.0831 0.5326 0.174 Uiso 0.50 1 calc PR B -1 H2DC H 1.1957 0.9899 0.4618 0.174 Uiso 0.50 1 calc PR B -1 C3D C 1.057(2) 0.8422(16) 0.6863(15) 0.116(3) Uani 0.50 1 d PD B -1 H3DB H 1.1270 0.8382 0.7178 0.139 Uiso 0.50 1 calc PR B -1 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 N1 0.044(2) 0.053(2) 0.0301(18) -0.0114(15) -0.0066(15) -0.0048(17) N2 0.0379(18) 0.0410(19) 0.0272(16) -0.0066(14) -0.0051(14) -0.0113(15) C1 0.050(3) 0.060(3) 0.032(2) -0.015(2) -0.0140(19) -0.007(2) C2 0.036(2) 0.051(2) 0.033(2) -0.0127(18) -0.0098(17) -0.0080(19) C3 0.033(2) 0.033(2) 0.0280(19) -0.0082(16) -0.0069(16) -0.0026(16) C4 0.037(2) 0.046(2) 0.032(2) -0.0098(17) -0.0097(17) -0.0080(18) C5 0.036(2) 0.046(2) 0.036(2) -0.0062(18) -0.0053(17) -0.0099(19) C6 0.0289(19) 0.038(2) 0.031(2) -0.0085(16) -0.0092(16) -0.0035(16) C7 0.033(2) 0.046(2) 0.036(2) -0.0154(18) -0.0072(16) -0.0106(18) C8 0.034(2) 0.042(2) 0.037(2) -0.0131(18) -0.0044(17) -0.0134(18) C9 0.049(2) 0.051(2) 0.030(2) -0.0087(18) -0.0084(18) -0.023(2) C10 0.037(2) 0.045(2) 0.031(2) -0.0085(17) -0.0073(17) -0.0171(18) C11 0.046(2) 0.051(3) 0.0236(19) -0.0029(17) -0.0029(17) -0.016(2) S1 0.0547(7) 0.0448(6) 0.0317(5) -0.0054(4) -0.0161(5) -0.0154(5) O1 0.121(3) 0.067(2) 0.0373(18) 0.0034(16) -0.0244(19) -0.050(2) O2 0.056(2) 0.088(3) 0.059(2) -0.0259(19) -0.0318(17) 0.0010(18) O3 0.0534(18) 0.0540(18) 0.0430(17) -0.0172(14) -0.0181(14) -0.0116(15) O4 0.0439(16) 0.0448(16) 0.0291(14) -0.0095(12) -0.0058(12) -0.0188(13) O5 0.088(2) 0.0533(19) 0.0408(17) -0.0013(14) -0.0294(17) -0.0335(18) O6 0.113(3) 0.067(2) 0.108(3) -0.035(2) -0.079(3) -0.002(2) O7 0.0537(18) 0.0463(17) 0.0356(15) -0.0130(13) -0.0136(13) -0.0184(14) C12 0.038(2) 0.037(2) 0.034(2) -0.0124(17) -0.0108(17) -0.0043(17) C13 0.052(3) 0.040(2) 0.043(2) -0.0097(19) -0.013(2) -0.019(2) C14 0.049(2) 0.043(2) 0.033(2) -0.0050(18) -0.0059(18) -0.020(2) C15 0.039(2) 0.033(2) 0.035(2) -0.0100(16) -0.0120(17) -0.0048(17) C16 0.039(2) 0.036(2) 0.032(2) -0.0087(16) -0.0102(17) -0.0116(17) C17 0.033(2) 0.033(2) 0.034(2) -0.0086(16) -0.0073(16) -0.0062(16) C18 0.041(2) 0.049(2) 0.032(2) -0.0089(18) -0.0100(17) -0.0190(19) C19 0.050(3) 0.059(3) 0.038(2) -0.014(2) -0.002(2) -0.027(2) C20 0.062(3) 0.058(3) 0.037(2) -0.013(2) -0.017(2) -0.025(2) C21 0.121(5) 0.058(3) 0.088(4) 0.004(3) -0.068(4) -0.041(3) C22 0.075(3) 0.059(3) 0.066(3) -0.032(3) -0.036(3) 0.000(3) C23 0.063(3) 0.048(3) 0.051(3) -0.020(2) -0.020(2) -0.015(2) O1M 0.088(3) 0.074(2) 0.0376(18) -0.0170(17) -0.0122(18) 0.004(2) C1M 0.070(3) 0.070(4) 0.050(3) -0.015(3) -0.002(2) -0.020(3) O2M 0.097(4) 0.116(4) 0.096(4) -0.044(3) -0.017(3) -0.029(3) C2M 0.090(5) 0.077(4) 0.107(5) -0.016(4) -0.042(4) -0.014(4) O3M 0.441(18) 0.128(6) 0.422(17) -0.054(9) -0.345(16) 0.023(9) C3M 0.206(10) 0.171(9) 0.058(4) -0.001(5) -0.048(5) -0.111(8) O4M 0.107(10) 0.077(8) 0.128(10) -0.036(8) -0.040(8) -0.039(7) C4M 0.123(17) 0.060(11) 0.94(9) -0.19(3) -0.30(4) 0.073(11) O1D 0.094(9) 0.057(7) 0.163(11) 0.002(8) -0.068(8) -0.026(6) N1D 0.056(7) 0.095(9) 0.148(12) -0.043(8) -0.010(7) -0.009(6) C1D 0.109(8) 0.109(8) 0.121(8) -0.003(6) -0.027(6) -0.035(6) C2D 0.109(8) 0.109(8) 0.121(8) -0.003(6) -0.027(6) -0.035(6) C3D 0.109(8) 0.109(8) 0.121(8) -0.003(6) -0.027(6) -0.035(6) _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 N1 C1 1.329(6) . ? N1 C5 1.341(5) . ? N2 C9 1.334(5) . ? N2 C8 1.349(5) . ? N2 C11 1.484(5) . ? C1 C2 1.385(6) . ? C2 C3 1.395(5) . ? C3 C4 1.388(5) . ? C3 C6 1.482(5) . ? C4 C5 1.379(5) . ? C6 C7 1.393(5) . ? C6 C10 1.393(5) . ? C7 C8 1.366(5) . ? C9 C10 1.370(5) . ? C11 C11 1.524(8) 2_667 ? S1 O3 1.437(3) . ? S1 O1 1.447(3) . ? S1 O2 1.449(3) . ? S1 C15 1.773(4) . ? O4 C17 1.373(5) . ? O4 C18 1.441(4) . ? O5 C20 1.408(5) . ? O5 C19 1.415(6) . ? O6 C21 1.339(6) . ? O6 C22 1.426(6) . ? O7 C12 1.362(5) . ? O7 C23 1.439(5) . ? C12 C13 1.382(6) . ? C12 C17 1.415(5) . ? C13 C14 1.399(6) . ? C14 C15 1.367(5) . ? C15 C16 1.400(5) . ? C16 C17 1.367(5) . ? C18 C19 1.495(6) . ? C20 C21 1.454(7) 2_667 ? C21 C20 1.454(7) 2_667 ? C22 C23 1.484(6) . ? O1M C1M 1.398(6) . ? O2M C2M 1.424(7) . ? O3M C3M 1.414(5) . ? O4M C4M 1.443(5) . ? O1D C3D 1.175(5) . ? N1D C3D 1.447(5) . ? N1D C2D 1.472(15) . ? N1D C1D 1.487(16) . ? 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 C1 N1 C5 116.5(3) . . ? C9 N2 C8 120.5(3) . . ? C9 N2 C11 119.7(3) . . ? C8 N2 C11 119.9(3) . . ? N1 C1 C2 124.6(4) . . ? C1 C2 C3 118.5(4) . . ? C4 C3 C2 117.2(3) . . ? C4 C3 C6 122.0(3) . . ? C2 C3 C6 120.7(3) . . ? C5 C4 C3 119.9(4) . . ? N1 C5 C4 123.3(4) . . ? C7 C6 C10 117.0(3) . . ? C7 C6 C3 121.8(3) . . ? C10 C6 C3 121.3(3) . . ? C8 C7 C6 120.8(4) . . ? N2 C8 C7 120.4(4) . . ? N2 C9 C10 121.1(4) . . ? C9 C10 C6 120.3(4) . . ? N2 C11 C11 108.5(4) . 2_667 ? O3 S1 O1 113.5(2) . . ? O3 S1 O2 111.5(2) . . ? O1 S1 O2 113.0(2) . . ? O3 S1 C15 106.81(18) . . ? O1 S1 C15 105.86(19) . . ? O2 S1 C15 105.51(19) . . ? C17 O4 C18 116.0(3) . . ? C20 O5 C19 115.1(3) . . ? C21 O6 C22 117.4(4) . . ? C12 O7 C23 116.7(3) . . ? O7 C12 C13 124.4(4) . . ? O7 C12 C17 116.6(3) . . ? C13 C12 C17 119.0(3) . . ? C12 C13 C14 120.5(4) . . ? C15 C14 C13 120.1(4) . . ? C14 C15 C16 119.8(4) . . ? C14 C15 S1 121.7(3) . . ? C16 C15 S1 118.5(3) . . ? C17 C16 C15 120.6(3) . . ? C16 C17 O4 124.3(3) . . ? C16 C17 C12 119.9(3) . . ? O4 C17 C12 115.8(3) . . ? O4 C18 C19 108.0(3) . . ? O5 C19 C18 114.4(4) . . ? O5 C20 C21 111.4(4) . 2_667 ? O6 C21 C20 115.5(5) . 2_667 ? O6 C22 C23 114.9(4) . . ? O7 C23 C22 109.2(4) . . ? C3D N1D C2D 118.4(12) . . ? C3D N1D C1D 122.2(13) . . ? C2D N1D C1D 119.3(13) . . ? O1D C3D N1D 117.2(16) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.829 _refine_diff_density_min -0.757 _refine_diff_density_rms 0.073 # Attachment 'CCDC 736644 (B911889F-R2).txt' data_ln2 _database_code_depnum_ccdc_archive 'CCDC 736644' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C79 H85 Cu2 N5 O25 S2' _chemical_formula_weight 1695.72 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _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 10.756(3) _cell_length_b 11.397(3) _cell_length_c 17.365(5) _cell_angle_alpha 103.580(3) _cell_angle_beta 98.407(3) _cell_angle_gamma 104.257(3) _cell_volume 1957.8(9) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7125 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.15 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.438 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 884 _exptl_absorpt_coefficient_mu 0.679 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.837790 _exptl_absorpt_correction_T_max 1.000000 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 18532 _diffrn_reflns_av_R_equivalents 0.0663 _diffrn_reflns_av_sigmaI/netI 0.0914 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 1.92 _diffrn_reflns_theta_max 25.00 _reflns_number_total 6873 _reflns_number_gt 4675 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker SHELXTL XCIF' _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^)+(0.0812P)^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 6873 _refine_ls_number_parameters 533 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0982 _refine_ls_R_factor_gt 0.0593 _refine_ls_wR_factor_ref 0.1497 _refine_ls_wR_factor_gt 0.1324 _refine_ls_goodness_of_fit_ref 0.991 _refine_ls_restrained_S_all 0.991 _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 0.06040(5) 0.07581(4) 0.07277(3) 0.01814(17) Uani 1 1 d . . . O1 O -0.0284(3) -0.0579(3) 0.11626(17) 0.0288(7) Uani 1 1 d . . . O2 O -0.1318(3) -0.1855(3) -0.00742(17) 0.0277(7) Uani 1 1 d . . . O3 O 0.2020(3) -0.0024(3) 0.06048(17) 0.0279(7) Uani 1 1 d . . . O4 O 0.0999(3) -0.1269(3) -0.06377(16) 0.0271(7) Uani 1 1 d . . . N1 N 0.1578(3) 0.2214(3) 0.18649(19) 0.0211(8) Uani 1 1 d . . . N2 N 0.4577(3) 0.8240(3) 0.4572(2) 0.0228(8) Uani 1 1 d . . . C1 C 0.0897(4) 0.2776(4) 0.2338(2) 0.0266(10) Uani 1 1 d . . . H1A H -0.0011 0.2369 0.2273 0.032 Uiso 1 1 calc R . . C2 C 0.1463(4) 0.3936(4) 0.2925(2) 0.0253(10) Uani 1 1 d . . . H2A H 0.0950 0.4305 0.3254 0.030 Uiso 1 1 calc R . . C3 C 0.2770(4) 0.4537(4) 0.3020(2) 0.0212(9) Uani 1 1 d . . . C4 C 0.3507(4) 0.3925(4) 0.2564(2) 0.0258(10) Uani 1 1 d . . . H4A H 0.4428 0.4286 0.2639 0.031 Uiso 1 1 calc R . . C5 C 0.2858(4) 0.2775(4) 0.2000(2) 0.0228(10) Uani 1 1 d . . . H5A H 0.3361 0.2359 0.1688 0.027 Uiso 1 1 calc R . . C6 C 0.3394(4) 0.5837(4) 0.3573(2) 0.0223(10) Uani 1 1 d . . . C7 C 0.3126(4) 0.6205(4) 0.4335(3) 0.0265(10) Uani 1 1 d . . . H7A H 0.2524 0.5626 0.4518 0.032 Uiso 1 1 calc R . . C8 C 0.3738(4) 0.7415(4) 0.4825(3) 0.0281(11) Uani 1 1 d . . . H8A H 0.3561 0.7665 0.5350 0.034 Uiso 1 1 calc R . . C9 C 0.4823(4) 0.7915(4) 0.3826(2) 0.0265(10) Uani 1 1 d . . . H9A H 0.5409 0.8517 0.3650 0.032 Uiso 1 1 calc R . . C10 C 0.4238(4) 0.6728(4) 0.3321(3) 0.0279(10) Uani 1 1 d . . . H10A H 0.4409 0.6511 0.2792 0.034 Uiso 1 1 calc R . . C11 C 0.5295(4) 0.9524(3) 0.5125(2) 0.0250(10) Uani 1 1 d . . . H11A H 0.6235 0.9732 0.5100 0.030 Uiso 1 1 calc R . . H11B H 0.5233 0.9542 0.5691 0.030 Uiso 1 1 calc R . . C12 C -0.1105(4) -0.1565(4) 0.0685(3) 0.0231(10) Uani 1 1 d . . . C13 C -0.1902(4) -0.2438(4) 0.1068(3) 0.0266(10) Uani 1 1 d . . . C14 C -0.2700(5) -0.3628(4) 0.0593(3) 0.0374(12) Uani 1 1 d . . . H14A H -0.2700 -0.3903 0.0033 0.045 Uiso 1 1 calc R . . C15 C -0.3489(5) -0.4400(5) 0.0945(4) 0.0512(15) Uani 1 1 d . . . H15A H -0.4017 -0.5219 0.0628 0.061 Uiso 1 1 calc R . . C16 C -0.3516(6) -0.3996(6) 0.1746(4) 0.0579(17) Uani 1 1 d . . . H16A H -0.4076 -0.4532 0.1978 0.069 Uiso 1 1 calc R . . C17 C -0.2749(5) -0.2829(5) 0.2220(3) 0.0488(14) Uani 1 1 d . . . H17A H -0.2770 -0.2554 0.2777 0.059 Uiso 1 1 calc R . . C18 C -0.1944(5) -0.2059(5) 0.1874(3) 0.0373(12) Uani 1 1 d . . . H18A H -0.1408 -0.1249 0.2200 0.045 Uiso 1 1 calc R . . C19 C 0.1967(4) -0.0840(4) -0.0039(2) 0.0208(9) Uani 1 1 d . . . C20 C 0.3126(4) -0.1313(4) -0.0119(2) 0.0206(9) Uani 1 1 d . . . C21 C 0.4130(4) -0.1063(4) 0.0543(3) 0.0293(11) Uani 1 1 d . . . H21A H 0.4068 -0.0598 0.1059 0.035 Uiso 1 1 calc R . . C22 C 0.5213(4) -0.1468(4) 0.0472(3) 0.0351(12) Uani 1 1 d . . . H22A H 0.5890 -0.1295 0.0936 0.042 Uiso 1 1 calc R . . C23 C 0.5318(4) -0.2128(4) -0.0277(3) 0.0296(11) Uani 1 1 d . . . H23A H 0.6075 -0.2401 -0.0333 0.036 Uiso 1 1 calc R . . C24 C 0.4318(4) -0.2394(4) -0.0948(3) 0.0274(10) Uani 1 1 d . . . H24A H 0.4390 -0.2845 -0.1466 0.033 Uiso 1 1 calc R . . C25 C 0.3226(4) -0.2006(4) -0.0866(3) 0.0246(10) Uani 1 1 d . . . H25A H 0.2530 -0.2214 -0.1325 0.030 Uiso 1 1 calc R . . S1 S 0.23962(13) -0.44738(13) -0.35228(8) 0.0445(4) Uani 1 1 d . . . O5 O 0.3316(4) -0.5163(4) -0.3743(3) 0.0904(15) Uani 1 1 d . . . O6 O 0.2935(4) -0.3587(4) -0.2745(2) 0.0792(15) Uani 1 1 d . . . O7 O 0.1922(4) -0.3961(4) -0.4140(2) 0.0697(13) Uani 1 1 d . . . O8 O -0.1439(3) -0.8573(3) -0.46788(17) 0.0416(9) Uani 1 1 d . . . O9 O -0.3098(3) -0.9627(3) -0.62901(17) 0.0371(8) Uani 1 1 d . . . O10 O -0.5587(3) -1.0184(3) -0.72081(18) 0.0319(7) Uani 1 1 d . . . O11 O -0.7988(3) -1.1449(3) -0.67304(17) 0.0357(8) Uani 1 1 d . . . C26 C -0.1011(4) -0.7561(4) -0.3282(3) 0.0292(11) Uani 1 1 d . . . C27 C -0.0301(4) -0.6563(4) -0.2618(3) 0.0304(11) Uani 1 1 d . . . H27A H -0.0520 -0.6530 -0.2104 0.036 Uiso 1 1 calc R . . C28 C 0.0718(4) -0.5617(4) -0.2684(3) 0.0298(11) Uani 1 1 d . . . H28A H 0.1204 -0.4950 -0.2215 0.036 Uiso 1 1 calc R . . C29 C 0.1035(4) -0.5628(4) -0.3421(3) 0.0337(11) Uani 1 1 d . . . C30 C 0.0315(4) -0.6599(5) -0.4101(3) 0.0379(12) Uani 1 1 d . . . H30A H 0.0516 -0.6598 -0.4615 0.045 Uiso 1 1 calc R . . C31 C -0.0691(4) -0.7571(5) -0.4038(3) 0.0347(12) Uani 1 1 d . . . C32 C -0.0978(5) -0.8680(6) -0.5429(3) 0.0557(16) Uani 1 1 d . . . H32A H -0.0972 -0.7921 -0.5614 0.067 Uiso 1 1 calc R . . H32B H -0.0071 -0.8748 -0.5342 0.067 Uiso 1 1 calc R . . C33 C -0.1839(5) -0.9784(5) -0.6030(3) 0.0537(15) Uani 1 1 d . . . H33A H -0.1435 -0.9969 -0.6504 0.064 Uiso 1 1 calc R . . H33B H -0.1954 -1.0513 -0.5802 0.064 Uiso 1 1 calc R . . C34 C -0.3306(4) -0.9313(5) -0.7038(3) 0.0352(12) Uani 1 1 d . . . H34A H -0.3279 -1.0016 -0.7489 0.042 Uiso 1 1 calc R . . H34B H -0.2603 -0.8551 -0.7016 0.042 Uiso 1 1 calc R . . C35 C -0.4602(4) -0.9074(4) -0.7180(3) 0.0323(11) Uani 1 1 d . . . H35A H -0.4624 -0.8358 -0.6737 0.039 Uiso 1 1 calc R . . H35B H -0.4758 -0.8859 -0.7699 0.039 Uiso 1 1 calc R . . C36 C -0.6879(4) -1.0077(4) -0.7417(3) 0.0331(11) Uani 1 1 d . . . H36A H -0.6986 -0.9837 -0.7929 0.040 Uiso 1 1 calc R . . H36B H -0.7015 -0.9411 -0.6985 0.040 Uiso 1 1 calc R . . C37 C -0.7867(4) -1.1303(4) -0.7516(3) 0.0333(11) Uani 1 1 d . . . H37A H -0.8726 -1.1323 -0.7824 0.040 Uiso 1 1 calc R . . H37B H -0.7587 -1.2005 -0.7823 0.040 Uiso 1 1 calc R . . O1M O 0.2826(4) -0.7557(4) -0.4756(3) 0.0669(12) Uani 1 1 d . . . H1MD H 0.2968 -0.6849 -0.4409 0.080 Uiso 1 1 d R . . C1M C 0.2670(8) -0.7390(8) -0.5525(4) 0.094(3) Uani 1 1 d . . . H1MA H 0.2012 -0.6940 -0.5592 0.113 Uiso 1 1 calc R . . H1MB H 0.2377 -0.8214 -0.5932 0.113 Uiso 1 1 calc R . . H1MC H 0.3510 -0.6896 -0.5594 0.113 Uiso 1 1 calc R . . O1DA O -0.7367(13) -1.4258(10) -0.8587(6) 0.086(4) Uani 0.50 1 d P A -1 N1DA N -0.9226(12) -1.4811(11) -0.9549(7) 0.071(3) Uani 0.50 1 d P A -1 C1DA C -0.9388(12) -1.4112(8) -1.0135(9) 0.196(7) Uani 1 1 d . A -1 H1DA H -1.0278 -1.4466 -1.0476 0.295 Uiso 1 1 calc R A -1 H1DB H -0.8744 -1.4171 -1.0477 0.295 Uiso 1 1 calc R A -1 H1DC H -0.9251 -1.3224 -0.9849 0.295 Uiso 1 1 calc R A -1 C2DA C -0.845(3) -1.503(2) -0.8927(13) 0.043(6) Uani 0.25 1 d P A -1 H2DA H -0.8744 -1.5773 -0.8760 0.052 Uiso 0.25 1 calc PR A -1 C2DB C -0.774(3) -1.405(3) -0.912(2) 0.082(9) Uani 0.25 1 d P B -2 H2DB H -0.7216 -1.3453 -0.9340 0.098 Uiso 0.25 1 d PR B -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0217(3) 0.0130(3) 0.0150(3) -0.0012(2) 0.0002(2) 0.0037(2) O1 0.0357(18) 0.0228(17) 0.0235(17) 0.0073(14) 0.0025(14) 0.0019(14) O2 0.0372(18) 0.0194(16) 0.0225(17) 0.0015(13) 0.0062(14) 0.0056(14) O3 0.0283(16) 0.0304(17) 0.0195(16) -0.0032(14) -0.0014(13) 0.0124(14) O4 0.0215(16) 0.0301(17) 0.0213(16) -0.0054(13) -0.0038(13) 0.0097(13) N1 0.0260(19) 0.0199(19) 0.0139(18) -0.0010(15) 0.0040(15) 0.0065(16) N2 0.035(2) 0.0110(17) 0.0174(19) -0.0011(15) 0.0030(16) 0.0041(16) C1 0.023(2) 0.025(2) 0.021(2) -0.0041(19) -0.0009(19) 0.0006(19) C2 0.032(2) 0.022(2) 0.022(2) -0.0013(19) 0.007(2) 0.013(2) C3 0.032(2) 0.011(2) 0.014(2) -0.0012(17) -0.0007(18) -0.0001(18) C4 0.026(2) 0.022(2) 0.024(2) -0.0013(19) 0.0040(19) 0.0049(19) C5 0.024(2) 0.019(2) 0.022(2) 0.0001(18) 0.0055(19) 0.0055(19) C6 0.029(2) 0.018(2) 0.015(2) -0.0028(18) 0.0045(18) 0.0046(19) C7 0.032(2) 0.016(2) 0.024(2) -0.0015(19) 0.006(2) 0.0004(19) C8 0.040(3) 0.021(2) 0.015(2) -0.0052(19) 0.006(2) 0.006(2) C9 0.039(3) 0.015(2) 0.020(2) 0.0039(19) 0.005(2) 0.001(2) C10 0.041(3) 0.020(2) 0.015(2) -0.0044(19) 0.006(2) 0.004(2) C11 0.032(2) 0.012(2) 0.019(2) -0.0075(17) -0.0006(19) 0.0002(18) C12 0.024(2) 0.017(2) 0.033(3) 0.009(2) 0.008(2) 0.0117(19) C13 0.030(2) 0.023(2) 0.034(3) 0.012(2) 0.009(2) 0.014(2) C14 0.042(3) 0.028(3) 0.046(3) 0.015(2) 0.014(2) 0.010(2) C15 0.050(3) 0.030(3) 0.077(4) 0.027(3) 0.017(3) 0.004(3) C16 0.056(4) 0.054(4) 0.086(5) 0.046(4) 0.037(4) 0.017(3) C17 0.057(4) 0.054(4) 0.053(4) 0.028(3) 0.032(3) 0.024(3) C18 0.043(3) 0.036(3) 0.041(3) 0.018(2) 0.016(2) 0.018(2) C19 0.026(2) 0.017(2) 0.019(2) 0.0062(19) 0.004(2) 0.0051(19) C20 0.023(2) 0.016(2) 0.020(2) 0.0039(18) 0.0013(18) 0.0049(18) C21 0.031(3) 0.034(3) 0.019(2) -0.001(2) 0.001(2) 0.014(2) C22 0.032(3) 0.040(3) 0.029(3) 0.003(2) -0.005(2) 0.017(2) C23 0.025(2) 0.028(3) 0.039(3) 0.011(2) 0.008(2) 0.011(2) C24 0.036(3) 0.021(2) 0.029(3) 0.004(2) 0.014(2) 0.013(2) C25 0.023(2) 0.024(2) 0.023(2) 0.0028(19) -0.0009(19) 0.0075(19) S1 0.0465(8) 0.0433(8) 0.0291(7) 0.0048(6) 0.0055(6) -0.0065(6) O5 0.051(3) 0.067(3) 0.136(4) 0.008(3) 0.032(3) -0.001(2) O6 0.105(3) 0.058(3) 0.031(2) 0.0034(19) 0.001(2) -0.036(2) O7 0.073(3) 0.079(3) 0.045(2) 0.036(2) -0.002(2) -0.009(2) O8 0.0379(19) 0.050(2) 0.0171(17) -0.0053(15) -0.0002(14) -0.0039(16) O9 0.0356(19) 0.050(2) 0.0188(17) 0.0019(15) -0.0011(14) 0.0108(16) O10 0.0294(17) 0.0276(17) 0.0332(19) 0.0101(14) -0.0016(14) 0.0021(14) O11 0.0342(18) 0.045(2) 0.0177(17) 0.0058(14) 0.0002(14) -0.0016(15) C26 0.022(2) 0.037(3) 0.025(3) 0.007(2) 0.002(2) 0.006(2) C27 0.031(2) 0.039(3) 0.020(2) 0.007(2) 0.005(2) 0.010(2) C28 0.032(3) 0.033(3) 0.020(2) 0.003(2) 0.002(2) 0.010(2) C29 0.033(3) 0.039(3) 0.026(3) 0.004(2) 0.004(2) 0.011(2) C30 0.033(3) 0.047(3) 0.024(3) 0.004(2) 0.004(2) 0.003(2) C31 0.028(3) 0.047(3) 0.021(3) 0.002(2) 0.000(2) 0.006(2) C32 0.036(3) 0.077(4) 0.035(3) -0.008(3) 0.009(3) 0.005(3) C33 0.050(3) 0.058(4) 0.042(3) -0.005(3) 0.012(3) 0.013(3) C34 0.038(3) 0.037(3) 0.024(3) 0.004(2) 0.007(2) 0.005(2) C35 0.039(3) 0.025(3) 0.023(3) 0.006(2) 0.001(2) -0.004(2) C36 0.038(3) 0.037(3) 0.025(3) 0.010(2) 0.003(2) 0.014(2) C37 0.033(3) 0.045(3) 0.019(2) 0.008(2) 0.001(2) 0.009(2) O1M 0.075(3) 0.067(3) 0.069(3) 0.028(2) 0.007(2) 0.037(2) C1M 0.122(7) 0.131(7) 0.060(5) 0.034(5) 0.035(5) 0.075(6) O1DA 0.139(10) 0.076(8) 0.033(6) 0.005(5) -0.004(6) 0.038(7) N1DA 0.088(8) 0.061(7) 0.063(7) -0.001(6) 0.016(6) 0.039(7) C1DA 0.234(14) 0.097(8) 0.377(19) 0.155(11) 0.219(14) 0.088(9) C2DA 0.100(19) 0.031(12) 0.028(12) 0.024(10) 0.045(13) 0.038(13) C2DB 0.11(3) 0.044(17) 0.08(2) -0.006(17) 0.03(2) 0.023(18) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 O4 1.948(3) 2 ? Cu1 O3 1.958(3) . ? Cu1 O1 1.959(3) . ? Cu1 O2 1.972(3) 2 ? Cu1 N1 2.179(3) . ? Cu1 Cu1 2.6351(11) 2 ? O1 C12 1.261(5) . ? O2 C12 1.253(5) . ? O2 Cu1 1.972(3) 2 ? O3 C19 1.259(5) . ? O4 C19 1.263(5) . ? O4 Cu1 1.948(3) 2 ? N1 C5 1.327(5) . ? N1 C1 1.335(5) . ? N2 C8 1.336(5) . ? N2 C9 1.344(5) . ? N2 C11 1.492(5) . ? C1 C2 1.394(5) . ? C2 C3 1.370(6) . ? C3 C4 1.392(6) . ? C3 C6 1.492(5) . ? C4 C5 1.383(5) . ? C6 C10 1.385(6) . ? C6 C7 1.385(5) . ? C7 C8 1.377(5) . ? C9 C10 1.363(5) . ? C11 C11 1.501(8) 2_676 ? C12 C13 1.492(6) . ? C13 C18 1.375(6) . ? C13 C14 1.397(6) . ? C14 C15 1.379(6) . ? C15 C16 1.366(8) . ? C16 C17 1.368(8) . ? C17 C18 1.380(6) . ? C19 C20 1.487(6) . ? C20 C21 1.377(6) . ? C20 C25 1.386(5) . ? C21 C22 1.366(6) . ? C22 C23 1.377(6) . ? C23 C24 1.383(6) . ? C24 C25 1.367(6) . ? S1 O6 1.423(4) . ? S1 O7 1.426(4) . ? S1 O5 1.448(4) . ? S1 C29 1.772(5) . ? O8 C31 1.370(5) . ? O8 C32 1.450(6) . ? O9 C34 1.427(5) . ? O9 C33 1.430(6) . ? O10 C35 1.422(5) . ? O10 C36 1.425(5) . ? O11 C26 1.361(5) 2_434 ? O11 C37 1.433(5) . ? C26 O11 1.361(5) 2_434 ? C26 C27 1.381(6) . ? C26 C31 1.403(6) . ? C27 C28 1.374(6) . ? C28 C29 1.370(6) . ? C29 C30 1.384(6) . ? C30 C31 1.382(6) . ? C32 C33 1.434(7) . ? C34 C35 1.482(6) . ? C36 C37 1.488(6) . ? O1M C1M 1.384(7) . ? O1DA C2DA 1.24(3) . ? N1DA C2DA 1.38(3) . ? N1DA C1DA 1.449(14) . ? 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 O4 Cu1 O3 167.99(11) 2 . ? O4 Cu1 O1 87.87(12) 2 . ? O3 Cu1 O1 90.16(12) . . ? O4 Cu1 O2 91.00(12) 2 2 ? O3 Cu1 O2 88.54(12) . 2 ? O1 Cu1 O2 168.36(11) . 2 ? O4 Cu1 N1 93.82(12) 2 . ? O3 Cu1 N1 98.19(12) . . ? O1 Cu1 N1 99.17(12) . . ? O2 Cu1 N1 92.46(12) 2 . ? O4 Cu1 Cu1 82.19(8) 2 2 ? O3 Cu1 Cu1 85.88(8) . 2 ? O1 Cu1 Cu1 87.07(9) . 2 ? O2 Cu1 Cu1 81.31(9) 2 2 ? N1 Cu1 Cu1 172.50(9) . 2 ? C12 O1 Cu1 119.5(3) . . ? C12 O2 Cu1 125.9(3) . 2 ? C19 O3 Cu1 121.4(3) . . ? C19 O4 Cu1 126.2(3) . 2 ? C5 N1 C1 117.1(3) . . ? C5 N1 Cu1 119.3(3) . . ? C1 N1 Cu1 121.5(3) . . ? C8 N2 C9 120.7(3) . . ? C8 N2 C11 120.3(3) . . ? C9 N2 C11 118.9(3) . . ? N1 C1 C2 122.8(4) . . ? C3 C2 C1 119.1(4) . . ? C2 C3 C4 118.6(4) . . ? C2 C3 C6 121.4(4) . . ? C4 C3 C6 120.0(4) . . ? C5 C4 C3 117.9(4) . . ? N1 C5 C4 124.3(4) . . ? C10 C6 C7 118.1(4) . . ? C10 C6 C3 120.0(3) . . ? C7 C6 C3 121.9(4) . . ? C8 C7 C6 119.5(4) . . ? N2 C8 C7 120.8(4) . . ? N2 C9 C10 120.4(4) . . ? C9 C10 C6 120.4(4) . . ? N2 C11 C11 109.4(4) . 2_676 ? O2 C12 O1 125.7(4) . . ? O2 C12 C13 118.0(4) . . ? O1 C12 C13 116.3(4) . . ? C18 C13 C14 118.8(4) . . ? C18 C13 C12 121.1(4) . . ? C14 C13 C12 119.9(4) . . ? C15 C14 C13 119.5(5) . . ? C16 C15 C14 120.4(5) . . ? C15 C16 C17 121.0(5) . . ? C16 C17 C18 118.9(5) . . ? C13 C18 C17 121.5(5) . . ? O3 C19 O4 124.3(4) . . ? O3 C19 C20 118.5(3) . . ? O4 C19 C20 117.2(4) . . ? C21 C20 C25 118.4(4) . . ? C21 C20 C19 121.1(4) . . ? C25 C20 C19 120.5(4) . . ? C22 C21 C20 121.5(4) . . ? C21 C22 C23 119.6(4) . . ? C22 C23 C24 119.8(4) . . ? C25 C24 C23 120.0(4) . . ? C24 C25 C20 120.6(4) . . ? O6 S1 O7 114.8(3) . . ? O6 S1 O5 109.7(3) . . ? O7 S1 O5 113.2(3) . . ? O6 S1 C29 107.0(2) . . ? O7 S1 C29 107.0(2) . . ? O5 S1 C29 104.4(2) . . ? C31 O8 C32 115.4(4) . . ? C34 O9 C33 116.3(4) . . ? C35 O10 C36 112.2(3) . . ? C26 O11 C37 116.0(3) 2_434 . ? O11 C26 C27 125.3(4) 2_434 . ? O11 C26 C31 116.4(4) 2_434 . ? C27 C26 C31 118.3(4) . . ? C28 C27 C26 121.3(4) . . ? C29 C28 C27 120.5(4) . . ? C28 C29 C30 119.3(4) . . ? C28 C29 S1 121.9(4) . . ? C30 C29 S1 118.7(4) . . ? C31 C30 C29 120.7(4) . . ? O8 C31 C30 124.3(4) . . ? O8 C31 C26 115.8(4) . . ? C30 C31 C26 119.9(4) . . ? C33 C32 O8 108.6(4) . . ? O9 C33 C32 111.9(5) . . ? O9 C34 C35 109.3(4) . . ? O10 C35 C34 108.4(4) . . ? O10 C36 C37 109.8(4) . . ? O11 C37 C36 109.1(4) . . ? C2DA N1DA C1DA 150.3(16) . . ? O1DA C2DA N1DA 119.1(17) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.851 _refine_diff_density_min -0.370 _refine_diff_density_rms 0.089 # Attachment 'CCDC 736645 (B911889F-R2).txt' data_lk11z _database_code_depnum_ccdc_archive 'CCDC 736645' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H78 Br Cu N4 O24 S2' _chemical_formula_weight 1422.81 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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Br Br -0.2901 2.4595 '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 27.257(5) _cell_length_b 14.035(2) _cell_length_c 21.840(4) _cell_angle_alpha 90.00 _cell_angle_beta 125.981(4) _cell_angle_gamma 90.00 _cell_volume 6761(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 7645 _cell_measurement_theta_min 1.5 _cell_measurement_theta_max 28.15 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas 'not measured' _exptl_crystal_density_diffrn 1.398 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2968 _exptl_absorpt_coefficient_mu 1.054 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.749122 _exptl_absorpt_correction_T_max 1.000000 _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 ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 21266 _diffrn_reflns_av_R_equivalents 0.0741 _diffrn_reflns_av_sigmaI/netI 0.0564 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 20.82 _reflns_number_total 3526 _reflns_number_gt 2159 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SHELXTL XPREP' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL XP' _computing_publication_material 'Bruker SHELXTL XCIF' _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 3526 _refine_ls_number_parameters 407 _refine_ls_number_restraints 22 _refine_ls_R_factor_all 0.1453 _refine_ls_R_factor_gt 0.1001 _refine_ls_wR_factor_ref 0.3176 _refine_ls_wR_factor_gt 0.2816 _refine_ls_goodness_of_fit_ref 1.150 _refine_ls_restrained_S_all 1.163 _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 0.0000 0.58343(14) 0.2500 0.0781(9) Uani 1 2 d S . . Br1 Br 0.0000 0.41217(13) 0.2500 0.0935(9) Uani 1 2 d S . . N1 N 0.0672(4) 0.6372(6) 0.3456(5) 0.063(3) Uani 1 1 d . . . N2 N 0.4635(4) 0.9494(6) 0.9027(4) 0.057(2) Uani 1 1 d . . . C1 C 0.0690(6) 0.7276(10) 0.3632(7) 0.113(5) Uani 1 1 d . . . H1A H 0.0357 0.7672 0.3280 0.135 Uiso 1 1 calc R . . C2 C 0.1178(6) 0.7691(9) 0.4317(7) 0.112(5) Uani 1 1 d . . . H2A H 0.1167 0.8345 0.4420 0.134 Uiso 1 1 calc R . . C3 C 0.1675(5) 0.7126(7) 0.4838(5) 0.060(3) Uani 1 1 d . . . C4 C 0.1644(5) 0.6211(8) 0.4628(6) 0.077(4) Uani 1 1 d . . . H4A H 0.1973 0.5793 0.4950 0.093 Uiso 1 1 calc R . . C5 C 0.1144(6) 0.5877(8) 0.3955(6) 0.078(4) Uani 1 1 d . . . H5A H 0.1143 0.5221 0.3846 0.094 Uiso 1 1 calc R . . C6 C 0.2203(4) 0.7540(8) 0.5557(5) 0.056(3) Uani 1 1 d . . . C7 C 0.2227(5) 0.8520(7) 0.5705(6) 0.071(3) Uani 1 1 d . . . H7A H 0.1912 0.8930 0.5338 0.085 Uiso 1 1 calc R . . C8 C 0.2709(6) 0.8885(7) 0.6382(6) 0.076(4) Uani 1 1 d . . . H8A H 0.2722 0.9551 0.6468 0.091 Uiso 1 1 calc R . . C9 C 0.3176(4) 0.8322(7) 0.6942(5) 0.055(3) Uani 1 1 d . . . C10 C 0.3141(4) 0.7356(6) 0.6781(5) 0.059(3) Uani 1 1 d . . . H10A H 0.3454 0.6949 0.7156 0.071 Uiso 1 1 calc R . . C11 C 0.2675(5) 0.6960(7) 0.6104(6) 0.070(3) Uani 1 1 d . . . H11A H 0.2677 0.6299 0.6012 0.084 Uiso 1 1 calc R . . C12 C 0.3686(5) 0.8729(7) 0.7672(5) 0.054(3) Uani 1 1 d . . . C13 C 0.3862(5) 0.9679(7) 0.7734(5) 0.056(3) Uani 1 1 d . . . H13A H 0.3649 1.0078 0.7300 0.067 Uiso 1 1 calc R . . C14 C 0.4329(5) 1.0038(7) 0.8401(6) 0.061(3) Uani 1 1 d . . . H14A H 0.4443 1.0685 0.8430 0.074 Uiso 1 1 calc R . . C15 C 0.4478(5) 0.8567(8) 0.8970(6) 0.076(4) Uani 1 1 d . . . H15A H 0.4704 0.8173 0.9405 0.091 Uiso 1 1 calc R . . C16 C 0.4016(5) 0.8190(7) 0.8322(6) 0.068(3) Uani 1 1 d . . . H16A H 0.3912 0.7541 0.8309 0.082 Uiso 1 1 calc R . . C17 C 0.5122(5) 0.9904(7) 0.9780(5) 0.060(3) Uani 1 1 d . . . H17A H 0.5465 0.9451 1.0060 0.072 Uiso 1 1 calc R . . H17B H 0.5274 1.0504 0.9709 0.072 Uiso 1 1 calc R . . S1 S -0.1399(2) 1.0587(2) -0.1128(3) 0.139(2) Uani 1 1 d . . . O1 O -0.0989(6) 1.1108(9) -0.1198(8) 0.230(10) Uani 1 1 d D . . O2 O -0.1669(6) 1.1187(9) -0.0894(8) 0.258(11) Uani 1 1 d D . . O3 O -0.1113(4) 0.9757(6) -0.0659(5) 0.117(4) Uani 1 1 d D . . O4 O -0.3358(4) 0.9320(5) -0.4200(5) 0.079(2) Uani 1 1 d . . . O5 O -0.5695(5) 1.1938(7) -0.4668(6) 0.120(4) Uani 1 1 d . . . O6 O -0.4540(4) 1.2178(5) -0.4212(5) 0.091(3) Uani 1 1 d . . . O7 O -0.3456(3) 1.0950(4) -0.3728(4) 0.070(2) Uani 1 1 d . . . C18 C -0.2940(5) 1.0426(7) -0.3215(7) 0.057(3) Uani 1 1 d . . . C19 C -0.2488(5) 1.0710(7) -0.2515(8) 0.078(4) Uani 1 1 d . . . H19A H -0.2527 1.1298 -0.2332 0.093 Uiso 1 1 calc R . . C20 C -0.1985(6) 1.0192(8) -0.2066(8) 0.091(5) Uani 1 1 d . . . C21 C -0.1933(6) 0.9312(10) -0.2309(9) 0.111(5) Uani 1 1 d . . . H21A H -0.1583 0.8933 -0.1982 0.133 Uiso 1 1 calc R . . C22 C -0.2376(6) 0.8986(8) -0.3008(8) 0.098(5) Uani 1 1 d . . . H22A H -0.2338 0.8383 -0.3174 0.118 Uiso 1 1 calc R . . C23 C -0.2901(6) 0.9565(8) -0.3493(7) 0.071(3) Uani 1 1 d . . . C24 C -0.3271(6) 0.8457(8) -0.4494(7) 0.085(4) Uani 1 1 d . . . H24A H -0.3227 0.7905 -0.4183 0.102 Uiso 1 1 calc R . . H24B H -0.2895 0.8513 -0.4464 0.102 Uiso 1 1 calc R . . C25 C -0.6214(7) 1.1695(11) -0.4723(8) 0.105(5) Uani 1 1 d . . . H25A H -0.6312 1.2211 -0.4502 0.126 Uiso 1 1 calc R . . H25B H -0.6137 1.1107 -0.4429 0.126 Uiso 1 1 calc R . . C26 C -0.5383(6) 1.2670(9) -0.4258(8) 0.090(4) Uani 1 1 d . . . H26A H -0.5253 1.2552 -0.3735 0.108 Uiso 1 1 calc R . . H26B H -0.5657 1.3229 -0.4452 0.108 Uiso 1 1 calc R . . C27 C -0.4873(8) 1.2910(10) -0.4223(8) 0.104(5) Uani 1 1 d . . . H27A H -0.5004 1.3319 -0.4664 0.125 Uiso 1 1 calc R . . H27B H -0.4604 1.3299 -0.3763 0.125 Uiso 1 1 calc R . . C28 C -0.4025(6) 1.2410(8) -0.4182(7) 0.080(4) Uani 1 1 d . . . H28A H -0.3968 1.3109 -0.4137 0.096 Uiso 1 1 calc R . . H28B H -0.4090 1.2208 -0.4659 0.096 Uiso 1 1 calc R . . C29 C -0.3461(5) 1.1936(7) -0.3522(6) 0.067(3) Uani 1 1 d . . . H29A H -0.3095 1.2272 -0.3405 0.080 Uiso 1 1 calc R . . H29B H -0.3460 1.1958 -0.3068 0.080 Uiso 1 1 calc R . . O1W O -0.0163(7) 0.9485(12) 0.0883(8) 0.212(7) Uani 1 1 d D . . H1WA H -0.0471 0.9726 0.0834 0.254 Uiso 1 1 d R . . H1WB H -0.0035 0.9066 0.0727 0.254 Uiso 1 1 d R . . O2W O -0.2634(10) 1.1212(16) -0.0785(12) 0.375(11) Uani 1 1 d DU . . H2WA H -0.2378 1.1103 -0.0881 0.450 Uiso 1 1 d R . . H2WB H -0.3017 1.1157 -0.1039 0.450 Uiso 1 1 d R . . O3W O -0.3534(11) 1.2496(18) -0.1725(14) 0.392(12) Uani 1 1 d DU . . H3WA H -0.3462 1.1950 -0.1824 0.470 Uiso 1 1 d R . . H3WB H -0.3781 1.2945 -0.1826 0.470 Uiso 1 1 d R . . O4W O -0.2032(13) 1.0406(17) 0.0629(14) 0.364(11) Uani 1 1 d DU . . H4WA H -0.1700 1.0636 0.1003 0.437 Uiso 1 1 d R . . H4WB H -0.2090 1.0720 0.0259 0.437 Uiso 1 1 d R . . O5W O -0.0911(14) 1.060(2) 0.1934(16) 0.402(12) Uani 1 1 d DU . . H5WA H -0.0565 1.0842 0.2259 0.482 Uiso 1 1 d R . . H5WB H -0.0824 1.0013 0.1957 0.482 Uiso 1 1 d 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 0.0673(15) 0.0792(15) 0.0419(13) 0.000 0.0065(11) 0.000 Br1 0.1092(17) 0.0689(13) 0.0698(14) 0.000 0.0345(12) 0.000 N1 0.076(7) 0.039(5) 0.047(6) 0.001(5) 0.020(5) 0.009(5) N2 0.059(6) 0.034(5) 0.037(5) -0.012(4) 0.004(5) -0.002(5) C1 0.086(10) 0.083(11) 0.071(10) 0.030(8) -0.008(8) 0.024(8) C2 0.106(11) 0.062(8) 0.068(9) -0.020(7) -0.004(9) 0.019(8) C3 0.067(8) 0.051(7) 0.034(6) 0.002(5) 0.014(6) 0.013(6) C4 0.074(8) 0.054(8) 0.045(7) -0.005(6) 0.002(7) 0.013(6) C5 0.085(9) 0.044(7) 0.049(8) -0.008(6) 0.008(8) 0.013(7) C6 0.049(7) 0.061(7) 0.031(6) -0.007(5) 0.010(5) 0.002(6) C7 0.092(9) 0.044(7) 0.040(7) -0.001(5) 0.018(7) 0.015(6) C8 0.100(9) 0.038(6) 0.036(7) -0.013(6) 0.010(7) -0.003(7) C9 0.059(7) 0.055(7) 0.028(6) 0.001(5) 0.012(6) 0.010(6) C10 0.063(7) 0.032(6) 0.036(6) 0.001(5) 0.003(6) 0.020(5) C11 0.062(7) 0.042(6) 0.052(7) -0.010(6) 0.004(7) 0.007(6) C12 0.059(7) 0.041(6) 0.038(7) -0.012(5) 0.015(6) -0.004(5) C13 0.083(8) 0.032(6) 0.029(6) -0.003(5) 0.020(6) -0.005(6) C14 0.079(8) 0.043(6) 0.048(8) -0.011(6) 0.030(7) -0.019(6) C15 0.083(9) 0.041(7) 0.047(8) -0.001(5) 0.006(7) 0.002(6) C16 0.090(8) 0.032(6) 0.040(7) -0.003(6) 0.014(7) -0.011(6) C17 0.051(7) 0.043(6) 0.044(7) -0.005(5) 0.005(5) -0.003(5) S1 0.079(3) 0.039(2) 0.139(4) -0.004(2) -0.025(3) -0.003(2) O1 0.134(10) 0.117(9) 0.199(14) 0.081(9) -0.036(10) -0.063(9) O2 0.144(11) 0.130(10) 0.193(13) -0.115(10) -0.071(9) 0.076(9) O3 0.094(7) 0.052(5) 0.095(7) -0.015(5) -0.007(6) -0.003(5) O4 0.099(7) 0.041(5) 0.073(6) 0.015(4) 0.037(6) 0.007(4) O5 0.112(8) 0.107(8) 0.155(10) -0.080(7) 0.086(8) -0.046(7) O6 0.061(6) 0.045(5) 0.125(8) 0.016(5) 0.032(5) 0.010(5) O7 0.070(5) 0.032(4) 0.074(5) -0.003(4) 0.024(5) 0.002(4) C18 0.055(8) 0.029(6) 0.069(8) 0.013(6) 0.026(7) 0.006(6) C19 0.060(8) 0.026(6) 0.089(10) 0.012(6) 0.011(8) 0.003(6) C20 0.072(9) 0.026(7) 0.124(12) -0.006(7) 0.029(9) 0.005(6) C21 0.065(9) 0.078(11) 0.093(11) 0.005(8) -0.008(9) 0.013(7) C22 0.087(10) 0.052(8) 0.098(11) 0.002(8) 0.022(9) 0.028(7) C23 0.079(9) 0.048(7) 0.059(8) 0.004(7) 0.026(8) -0.007(7) C24 0.097(10) 0.059(8) 0.078(9) -0.013(7) 0.040(9) -0.005(7) C25 0.110(12) 0.103(11) 0.095(12) -0.004(9) 0.056(11) 0.006(10) C26 0.078(10) 0.049(8) 0.121(12) 0.012(8) 0.046(9) 0.015(7) C27 0.124(13) 0.073(10) 0.112(12) -0.045(8) 0.068(11) -0.013(11) C28 0.091(10) 0.040(7) 0.076(9) -0.005(6) 0.031(8) -0.004(7) C29 0.062(7) 0.045(7) 0.072(8) 0.004(6) 0.027(7) 0.009(6) O1W 0.201(15) 0.233(15) 0.125(11) 0.028(11) 0.052(11) -0.048(13) O2W 0.55(3) 0.250(17) 0.46(2) 0.050(17) 0.37(2) 0.032(19) O3W 0.54(3) 0.35(2) 0.45(3) 0.107(19) 0.38(2) -0.02(2) O4W 0.58(3) 0.239(15) 0.45(2) 0.038(18) 0.40(2) 0.06(2) O5W 0.59(3) 0.32(2) 0.48(3) 0.06(2) 0.42(3) 0.05(2) _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 1.947(8) . ? Cu1 N1 1.947(8) 2 ? Cu1 Br1 2.404(3) . ? N1 C5 1.296(13) . ? N1 C1 1.318(15) . ? N2 C14 1.344(12) . ? N2 C15 1.352(13) . ? N2 C17 1.494(12) . ? C1 C2 1.417(17) . ? C2 C3 1.395(15) . ? C3 C4 1.350(14) . ? C3 C6 1.490(13) . ? C4 C5 1.372(14) . ? C6 C11 1.393(13) . ? C6 C7 1.406(14) . ? C7 C8 1.374(14) . ? C8 C9 1.383(14) . ? C9 C10 1.388(13) . ? C9 C12 1.484(13) . ? C10 C11 1.379(13) . ? C12 C16 1.377(13) . ? C12 C13 1.396(13) . ? C13 C14 1.348(14) . ? C15 C16 1.332(14) . ? C17 C17 1.48(2) 5_677 ? S1 O2 1.397(14) . ? S1 O1 1.419(16) . ? S1 O3 1.441(9) . ? S1 C20 1.792(14) . ? O4 C23 1.339(13) . ? O4 C24 1.454(13) . ? O5 C26 1.298(14) . ? O5 C25 1.390(16) . ? O6 C27 1.362(15) . ? O6 C28 1.403(14) . ? O7 C18 1.387(12) . ? O7 C29 1.457(12) . ? C18 C19 1.341(15) . ? C18 C23 1.384(16) . ? C19 C20 1.338(15) . ? C20 C21 1.384(17) . ? C21 C22 1.353(18) . ? C22 C23 1.432(17) . ? C24 C25 1.456(17) 5_474 ? C25 C24 1.456(17) 5_474 ? C26 C27 1.389(17) . ? C28 C29 1.510(15) . ? 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 N1 134.4(5) . 2 ? N1 Cu1 Br1 112.8(3) . . ? N1 Cu1 Br1 112.8(3) 2 . ? C5 N1 C1 115.0(10) . . ? C5 N1 Cu1 122.5(7) . . ? C1 N1 Cu1 122.5(8) . . ? C14 N2 C15 118.6(8) . . ? C14 N2 C17 121.3(8) . . ? C15 N2 C17 120.1(8) . . ? N1 C1 C2 123.6(11) . . ? C3 C2 C1 119.2(11) . . ? C4 C3 C2 115.2(10) . . ? C4 C3 C6 123.9(10) . . ? C2 C3 C6 120.8(10) . . ? C3 C4 C5 120.9(11) . . ? N1 C5 C4 126.0(10) . . ? C11 C6 C7 118.7(9) . . ? C11 C6 C3 120.7(9) . . ? C7 C6 C3 120.6(9) . . ? C8 C7 C6 119.9(10) . . ? C7 C8 C9 122.6(9) . . ? C8 C9 C10 116.4(9) . . ? C8 C9 C12 121.7(9) . . ? C10 C9 C12 121.9(9) . . ? C11 C10 C9 123.2(9) . . ? C10 C11 C6 119.2(9) . . ? C16 C12 C13 116.5(9) . . ? C16 C12 C9 121.9(9) . . ? C13 C12 C9 121.6(9) . . ? C14 C13 C12 120.9(9) . . ? N2 C14 C13 121.0(9) . . ? C16 C15 N2 122.1(10) . . ? C15 C16 C12 120.9(10) . . ? C17 C17 N2 109.7(11) 5_677 . ? O2 S1 O1 110.3(10) . . ? O2 S1 O3 114.1(10) . . ? O1 S1 O3 111.2(7) . . ? O2 S1 C20 107.3(6) . . ? O1 S1 C20 105.4(9) . . ? O3 S1 C20 108.0(5) . . ? C23 O4 C24 116.2(9) . . ? C26 O5 C25 118.3(12) . . ? C27 O6 C28 117.6(10) . . ? C18 O7 C29 116.3(8) . . ? C19 C18 C23 120.3(10) . . ? C19 C18 O7 125.4(10) . . ? C23 C18 O7 114.3(10) . . ? C20 C19 C18 122.2(12) . . ? C19 C20 C21 119.7(12) . . ? C19 C20 S1 120.8(10) . . ? C21 C20 S1 119.4(10) . . ? C22 C21 C20 120.7(12) . . ? C21 C22 C23 118.9(12) . . ? O4 C23 C18 118.1(11) . . ? O4 C23 C22 123.7(11) . . ? C18 C23 C22 118.2(11) . . ? O4 C24 C25 110.3(11) . 5_474 ? O5 C25 C24 111.5(12) . 5_474 ? O5 C26 C27 117.4(13) . . ? O6 C27 C26 117.0(12) . . ? O6 C28 C29 111.9(10) . . ? O7 C29 C28 108.2(9) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 20.82 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.928 _refine_diff_density_min -0.643 _refine_diff_density_rms 0.120