# Electronic Supplementary Material (ESI) for Dalton Transactions # 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_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H84 Br4 Cu11 F6 O12 P7 S12' _chemical_formula_weight 2443.12 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' 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' P P 0.1023 0.0942 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 14.7246(4) _cell_length_b 15.2002(4) _cell_length_c 21.1551(6) _cell_angle_alpha 103.0220(10) _cell_angle_beta 107.1190(10) _cell_angle_gamma 91.2670(10) _cell_volume 4388.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9995 _cell_measurement_theta_min 2.20 _cell_measurement_theta_max 25.76 _exptl_crystal_description plate _exptl_crystal_colour yellow _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.849 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2412 _exptl_absorpt_coefficient_mu 4.894 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.3411 _exptl_absorpt_correction_T_max 0.5687 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 52219 _diffrn_reflns_av_R_equivalents 0.0263 _diffrn_reflns_av_sigmaI/netI 0.0268 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 25.00 _reflns_number_total 15422 _reflns_number_gt 12474 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. Restraints on bond lengths and atomic displacement paremeters were applied by using DFIX and DELU command in SHELX program. C24, C35, C36 were split and refined anisotropically. They were finally fixed to 65/35, 50/50 and 50/50 respectively. Some elements of disorder, such as C28, C29 and C30, were modelled best large ADP on single sites as multiple sites were not resolved and they were refined isotropically. Attempts to solve the disorder of PF6 anion were failed. The residual densiy located at the solvent-accessible voids cannot be modelled as solvent molecules, thus, the SQUEEZE procedure was applied to deal with the solvent molecules. The used restraints are: DFIX 1.54 0.01 C28 C30 C28' C30' C28 C29 C28' C29' DFIX 1.54 0.01 C34 C35 C34 C36 C34 C35' C34 C36' C22 C24 DFIX 1.43 0.01 O10 C28 O10 C28' DELU C7 C8 DELU C7 C9 DELU C19 C20 DELU C19 C21 DELU C22 C23 DELU C28 C29 DELU C28 C30 DELU C28' C29' DELU C29' C30' DELU O10 C28 DELU O10 C28' ; _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^)+(0.0693P)^2^+1.9353P] 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 15422 _refine_ls_number_parameters 820 _refine_ls_number_restraints 16 _refine_ls_R_factor_all 0.0470 _refine_ls_R_factor_gt 0.0373 _refine_ls_wR_factor_ref 0.1162 _refine_ls_wR_factor_gt 0.1108 _refine_ls_goodness_of_fit_ref 1.079 _refine_ls_restrained_S_all 1.081 _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 Br4 Br 0.89182(3) 0.47625(3) 0.23784(2) 0.04425(11) Uani 1 1 d . . . Br1 Br 1.06636(3) 0.56732(3) 0.41820(2) 0.04861(12) Uani 1 1 d . . . Br2 Br 0.64270(3) 0.37371(3) 0.21070(2) 0.05119(12) Uani 1 1 d . . . Br3 Br 0.96670(3) 0.49097(3) 0.08302(2) 0.05086(12) Uani 1 1 d . . . C1 C 0.5013(4) 0.5598(4) 0.2978(3) 0.0682(14) Uani 1 1 d . . . H1 H 0.5166 0.5430 0.2548 0.082 Uiso 1 1 calc R . . C2 C 0.4792(6) 0.4756(5) 0.3164(5) 0.125(3) Uani 1 1 d . . . H2A H 0.5363 0.4457 0.3285 0.188 Uiso 1 1 calc R . . H2B H 0.4324 0.4362 0.2783 0.188 Uiso 1 1 calc R . . H2C H 0.4547 0.4902 0.3544 0.188 Uiso 1 1 calc R . . C3 C 0.4240(6) 0.6187(7) 0.2890(6) 0.159(5) Uani 1 1 d . . . H3A H 0.4051 0.6326 0.3296 0.238 Uiso 1 1 calc R . . H3B H 0.3705 0.5883 0.2511 0.238 Uiso 1 1 calc R . . H3C H 0.4453 0.6738 0.2806 0.238 Uiso 1 1 calc R . . C4 C 0.6455(4) 0.8188(3) 0.3823(3) 0.0607(13) Uani 1 1 d . . . H4 H 0.5917 0.7984 0.3404 0.073 Uiso 1 1 calc R . . C5 C 0.6096(6) 0.8400(5) 0.4420(4) 0.104(2) Uani 1 1 d . . . H5A H 0.5725 0.7877 0.4427 0.157 Uiso 1 1 calc R . . H5B H 0.5704 0.8895 0.4389 0.157 Uiso 1 1 calc R . . H5C H 0.6626 0.8567 0.4831 0.157 Uiso 1 1 calc R . . C6 C 0.7049(6) 0.8940(4) 0.3759(5) 0.107(3) Uani 1 1 d . . . H6A H 0.7676 0.8994 0.4081 0.160 Uiso 1 1 calc R . . H6B H 0.6761 0.9496 0.3851 0.160 Uiso 1 1 calc R . . H6C H 0.7097 0.8819 0.3305 0.160 Uiso 1 1 calc R . . C7 C 0.5243(5) 0.6684(6) 0.0463(4) 0.097(2) Uani 1 1 d U . . H7 H 0.5156 0.6045 0.0215 0.116 Uiso 1 1 calc R . . C8 C 0.5007(7) 0.7257(10) -0.0052(6) 0.195(6) Uani 1 1 d U . . H8A H 0.5098 0.7887 0.0182 0.292 Uiso 1 1 calc R . . H8B H 0.4354 0.7104 -0.0332 0.292 Uiso 1 1 calc R . . H8C H 0.5418 0.7144 -0.0334 0.292 Uiso 1 1 calc R . . C9 C 0.4649(6) 0.6805(10) 0.0927(5) 0.178(6) Uani 1 1 d U . . H9A H 0.4742 0.6337 0.1172 0.267 Uiso 1 1 calc R . . H9B H 0.3988 0.6767 0.0665 0.267 Uiso 1 1 calc R . . H9C H 0.4830 0.7387 0.1244 0.267 Uiso 1 1 calc R . . C10 C 0.7652(7) 0.6092(7) -0.0346(4) 0.120(3) Uani 1 1 d . . . H10 H 0.8092 0.5717 -0.0103 0.144 Uiso 1 1 calc R . . C11 C 0.7073(11) 0.5542(10) -0.1023(5) 0.226(7) Uani 1 1 d . . . H11A H 0.6502 0.5270 -0.0986 0.339 Uiso 1 1 calc R . . H11B H 0.7435 0.5075 -0.1186 0.339 Uiso 1 1 calc R . . H11C H 0.6906 0.5924 -0.1337 0.339 Uiso 1 1 calc R . . C12 C 0.8190(9) 0.6868(9) -0.0417(6) 0.196(6) Uani 1 1 d . . . H12A H 0.8713 0.6663 -0.0577 0.294 Uiso 1 1 calc R . . H12B H 0.8432 0.7295 0.0018 0.294 Uiso 1 1 calc R . . H12C H 0.7777 0.7155 -0.0738 0.294 Uiso 1 1 calc R . . C13 C 0.9954(4) 0.9447(3) 0.2912(3) 0.0651(14) Uani 1 1 d . . . H13 H 1.0083 0.9581 0.3407 0.078 Uiso 1 1 calc R . . C14 C 0.8908(5) 0.9482(4) 0.2586(4) 0.092(2) Uani 1 1 d . . . H14A H 0.8771 0.9355 0.2100 0.137 Uiso 1 1 calc R . . H14B H 0.8732 1.0075 0.2749 0.137 Uiso 1 1 calc R . . H14C H 0.8552 0.9038 0.2700 0.137 Uiso 1 1 calc R . . C15 C 1.0593(6) 1.0088(4) 0.2756(4) 0.101(2) Uani 1 1 d . . . H15A H 1.1243 1.0064 0.3018 0.151 Uiso 1 1 calc R . . H15B H 1.0415 1.0693 0.2871 0.151 Uiso 1 1 calc R . . H15C H 1.0533 0.9918 0.2279 0.151 Uiso 1 1 calc R . . C16 C 1.2185(4) 0.8401(4) 0.3836(3) 0.0735(16) Uani 1 1 d . . . H16 H 1.2215 0.8404 0.3380 0.088 Uiso 1 1 calc R . . C17 C 1.2740(5) 0.7667(6) 0.4085(5) 0.122(3) Uani 1 1 d . . . H17A H 1.2649 0.7619 0.4508 0.183 Uiso 1 1 calc R . . H17B H 1.3406 0.7811 0.4155 0.183 Uiso 1 1 calc R . . H17C H 1.2521 0.7101 0.3753 0.183 Uiso 1 1 calc R . . C18 C 1.2521(5) 0.9325(5) 0.4303(4) 0.122(3) Uani 1 1 d . . . H18A H 1.2120 0.9760 0.4130 0.182 Uiso 1 1 calc R . . H18B H 1.3168 0.9485 0.4329 0.182 Uiso 1 1 calc R . . H18C H 1.2491 0.9320 0.4750 0.182 Uiso 1 1 calc R . . C19 C 1.2937(4) 0.4231(5) 0.4379(3) 0.0846(18) Uani 1 1 d U . . H19 H 1.2302 0.4155 0.4431 0.101 Uiso 1 1 calc R . . C20 C 1.3546(9) 0.3554(8) 0.4650(4) 0.168(5) Uani 1 1 d U . . H20A H 1.3179 0.2975 0.4513 0.253 Uiso 1 1 calc R . . H20B H 1.3775 0.3742 0.5139 0.253 Uiso 1 1 calc R . . H20C H 1.4078 0.3505 0.4474 0.253 Uiso 1 1 calc R . . C21 C 1.3357(7) 0.5162(7) 0.4688(6) 0.156(4) Uani 1 1 d U . . H21A H 1.4030 0.5192 0.4747 0.233 Uiso 1 1 calc R . . H21B H 1.3257 0.5364 0.5124 0.233 Uiso 1 1 calc R . . H21C H 1.3062 0.5546 0.4398 0.233 Uiso 1 1 calc R . . C22 C 1.2666(5) 0.2065(5) 0.2587(4) 0.095(2) Uani 1 1 d DU . . H22 H 1.2467 0.1951 0.2967 0.114 Uiso 1 1 calc R A 1 C23 C 1.2221(9) 0.1339(6) 0.2009(6) 0.179(5) Uani 1 1 d U B . H23A H 1.1557 0.1240 0.1967 0.268 Uiso 1 1 calc R . . H23B H 1.2525 0.0797 0.2066 0.268 Uiso 1 1 calc R . . H23C H 1.2281 0.1489 0.1606 0.268 Uiso 1 1 calc R . . C24 C 1.3754(6) 0.2154(9) 0.2819(10) 0.163(8) Uani 0.65 1 d PD B 1 H24A H 1.3983 0.1763 0.3118 0.245 Uiso 0.65 1 calc PR B 1 H24B H 1.3990 0.2771 0.3056 0.245 Uiso 0.65 1 calc PR B 1 H24C H 1.3976 0.1985 0.2428 0.245 Uiso 0.65 1 calc PR B 1 C24' C 1.3458(17) 0.2108(18) 0.2085(19) 0.163(8) Uani 0.35 1 d P B 2 H24D H 1.3347 0.1556 0.1735 0.245 Uiso 0.35 1 calc PR B 2 H24E H 1.4108 0.2178 0.2373 0.245 Uiso 0.35 1 calc PR B 2 H24F H 1.3340 0.2613 0.1879 0.245 Uiso 0.35 1 calc PR B 2 C25 C 0.8433(4) 0.2292(5) -0.0757(3) 0.0766(16) Uani 1 1 d . . . H25 H 0.7854 0.1918 -0.0806 0.092 Uiso 1 1 calc R . . C26 C 0.8981(7) 0.1794(6) -0.1209(3) 0.126(3) Uani 1 1 d . . . H26A H 0.8591 0.1670 -0.1677 0.188 Uiso 1 1 calc R . . H26B H 0.9146 0.1234 -0.1088 0.188 Uiso 1 1 calc R . . H26C H 0.9552 0.2163 -0.1148 0.188 Uiso 1 1 calc R . . C27 C 0.8193(6) 0.3170(5) -0.0904(3) 0.098(2) Uani 1 1 d . . . H27A H 0.7831 0.3459 -0.0619 0.147 Uiso 1 1 calc R . . H27B H 0.7821 0.3079 -0.1375 0.147 Uiso 1 1 calc R . . H27C H 0.8769 0.3548 -0.0817 0.147 Uiso 1 1 calc R . . C28 C 0.7702(10) 0.0538(11) 0.0276(11) 0.136(6) Uiso 0.50 1 d PDU C 1 H28 H 0.7523 0.0875 0.0667 0.164 Uiso 0.50 1 calc PR C 1 C29 C 0.8247(18) -0.0162(16) 0.0637(13) 0.173(9) Uiso 0.50 1 d PDU C 1 H29A H 0.8481 -0.0581 0.0323 0.260 Uiso 0.50 1 calc PR C 1 H29B H 0.7823 -0.0486 0.0793 0.260 Uiso 0.50 1 calc PR C 1 H29C H 0.8774 0.0149 0.1019 0.260 Uiso 0.50 1 calc PR C 1 C30 C 0.6657(17) 0.039(3) -0.0259(18) 0.30(2) Uiso 0.50 1 d PDU C 1 H30A H 0.6645 -0.0057 -0.0662 0.455 Uiso 0.50 1 calc PR C 1 H30B H 0.6492 0.0955 -0.0378 0.455 Uiso 0.50 1 calc PR C 1 H30C H 0.6207 0.0195 -0.0060 0.455 Uiso 0.50 1 calc PR C 1 C28' C 0.9111(15) 0.0484(13) 0.0189(13) 0.185(10) Uiso 0.50 1 d PDU C 2 H28' H 0.9742 0.0640 0.0156 0.222 Uiso 0.50 1 calc PR C 2 C29' C 0.899(2) 0.007(2) 0.0753(14) 0.205(12) Uiso 0.50 1 d PDU C 2 H29D H 0.9607 0.0086 0.1082 0.307 Uiso 0.50 1 calc PR C 2 H29E H 0.8720 -0.0545 0.0563 0.307 Uiso 0.50 1 calc PR C 2 H29F H 0.8582 0.0413 0.0971 0.307 Uiso 0.50 1 calc PR C 2 C30' C 0.836(2) -0.019(2) -0.0395(15) 0.239(14) Uiso 0.50 1 d PD C 2 H30D H 0.7879 -0.0400 -0.0224 0.358 Uiso 0.50 1 calc PR C 2 H30E H 0.8659 -0.0696 -0.0577 0.358 Uiso 0.50 1 calc PR C 2 H30F H 0.8063 0.0109 -0.0748 0.358 Uiso 0.50 1 calc PR C 2 C31 C 0.9741(4) 0.1855(4) 0.4460(2) 0.0626(14) Uani 1 1 d . . . H31 H 0.9520 0.2389 0.4708 0.075 Uiso 1 1 calc R . . C32 C 0.9351(6) 0.0998(5) 0.4580(3) 0.099(2) Uani 1 1 d . . . H32A H 0.9617 0.0486 0.4367 0.149 Uiso 1 1 calc R . . H32B H 0.8668 0.0924 0.4386 0.149 Uiso 1 1 calc R . . H32C H 0.9519 0.1042 0.5061 0.149 Uiso 1 1 calc R . . C33 C 1.0797(5) 0.1945(7) 0.4648(4) 0.115(3) Uani 1 1 d . . . H33A H 1.1006 0.1401 0.4425 0.172 Uiso 1 1 calc R . . H33B H 1.1065 0.2039 0.5133 0.172 Uiso 1 1 calc R . . H33C H 1.1005 0.2452 0.4508 0.172 Uiso 1 1 calc R . . C34 C 0.6716(5) 0.2010(5) 0.3272(4) 0.098(2) Uani 1 1 d D . . H34 H 0.6573 0.2216 0.2849 0.117 Uiso 1 1 calc R D 1 C35 C 0.6123(12) 0.1129(10) 0.3179(16) 0.154(7) Uani 0.50 1 d PD E 1 H35A H 0.6083 0.0731 0.2747 0.230 Uiso 0.50 1 calc PR E 1 H35B H 0.5493 0.1258 0.3192 0.230 Uiso 0.50 1 calc PR E 1 H35C H 0.6420 0.0842 0.3538 0.230 Uiso 0.50 1 calc PR E 1 C36 C 0.6490(13) 0.2702(12) 0.3842(10) 0.154(7) Uani 0.50 1 d PD E 1 H36A H 0.6223 0.2388 0.4102 0.230 Uiso 0.50 1 calc PR E 1 H36B H 0.6039 0.3088 0.3646 0.230 Uiso 0.50 1 calc PR E 1 H36C H 0.7066 0.3063 0.4135 0.230 Uiso 0.50 1 calc PR E 1 C35' C 0.6173(13) 0.1205(14) 0.2667(9) 0.159(7) Uani 0.50 1 d PD E 2 H35D H 0.6412 0.1188 0.2289 0.238 Uiso 0.50 1 calc PR E 2 H35E H 0.5504 0.1283 0.2533 0.238 Uiso 0.50 1 calc PR E 2 H35F H 0.6269 0.0646 0.2806 0.238 Uiso 0.50 1 calc PR E 2 C36' C 0.6293(13) 0.206(2) 0.3848(8) 0.159(7) Uani 0.50 1 d PD E 2 H36D H 0.6125 0.1453 0.3870 0.238 Uiso 0.50 1 calc PR E 2 H36E H 0.5733 0.2379 0.3769 0.238 Uiso 0.50 1 calc PR E 2 H36F H 0.6753 0.2367 0.4271 0.238 Uiso 0.50 1 calc PR E 2 Cu9 Cu 0.81693(5) 0.43485(4) 0.09204(4) 0.06548(18) Uani 1 1 d . C . Cu2 Cu 0.94201(5) 0.61884(5) 0.16654(3) 0.06324(17) Uani 1 1 d . C . Cu1 Cu 1.03383(5) 0.40070(5) 0.16481(3) 0.06479(18) Uani 1 1 d . B . Cu7 Cu 1.08243(5) 0.56007(4) 0.30717(3) 0.05974(17) Uani 1 1 d . B . Cu4 Cu 0.91630(4) 0.62657(4) 0.36729(4) 0.06152(17) Uani 1 1 d . C . Cu3 Cu 1.00450(5) 0.41008(4) 0.36039(4) 0.06370(17) Uani 1 1 d . . . Cu8 Cu 0.77361(5) 0.43859(4) 0.31336(3) 0.06151(17) Uani 1 1 d . . . Cu6 Cu 0.68557(6) 0.51603(4) 0.18567(3) 0.06662(18) Uani 1 1 d . C . Cu5 Cu 0.77555(5) 0.29659(5) 0.18092(3) 0.06562(18) Uani 1 1 d . B . Cu10 Cu 0.80762(4) 0.69903(4) 0.24438(3) 0.05063(14) Uani 1 1 d . C . Cu11 Cu 0.97636(4) 0.25716(4) 0.22964(3) 0.05167(14) Uani 1 1 d . B . F1 F 0.2959(5) 0.9425(6) 0.2756(5) 0.233(4) Uani 1 1 d . . . F2 F 0.4851(5) 0.8801(7) 0.2569(4) 0.233(4) Uani 1 1 d . . . F3 F 0.3712(9) 0.9500(13) 0.2084(7) 0.363(10) Uani 1 1 d . . . F4 F 0.4103(6) 0.8726(7) 0.3296(5) 0.237(4) Uani 1 1 d . . . F5 F 0.3441(8) 0.8266(7) 0.2219(8) 0.388(10) Uani 1 1 d . . . F6 F 0.4386(8) 0.9948(6) 0.3047(9) 0.355(9) Uani 1 1 d . . . O1 O 0.5849(2) 0.6125(2) 0.35009(17) 0.0597(9) Uani 1 1 d . . . O2 O 0.7074(2) 0.7435(2) 0.39196(16) 0.0525(8) Uani 1 1 d . . . O3 O 0.6220(2) 0.6897(3) 0.08814(19) 0.0685(10) Uani 1 1 d . . . O4 O 0.7027(3) 0.6414(3) 0.00148(17) 0.0722(10) Uani 1 1 d . . . O5 O 1.0220(3) 0.85244(19) 0.26798(16) 0.0549(8) Uani 1 1 d . . . O6 O 1.1184(2) 0.8188(2) 0.38037(17) 0.0598(8) Uani 1 1 d . . . O7 O 1.2874(2) 0.4007(3) 0.36455(19) 0.0822(13) Uani 1 1 d . B . O8 O 1.2356(3) 0.2940(3) 0.2490(2) 0.0750(11) Uani 1 1 d . B . O9 O 0.9093(3) 0.2457(3) -0.00528(17) 0.0711(10) Uani 1 1 d . . . O10 O 0.8504(3) 0.1173(3) 0.0359(3) 0.0972(15) Uani 1 1 d DU . . O11 O 0.9393(2) 0.1789(2) 0.37076(15) 0.0506(7) Uani 1 1 d . E . O12 O 0.7691(3) 0.1832(3) 0.3504(2) 0.0689(10) Uani 1 1 d . E . P1 P 0.68166(8) 0.64633(7) 0.34352(6) 0.0406(2) Uani 1 1 d . . . P2 P 0.70579(9) 0.63583(8) 0.07501(6) 0.0476(3) Uani 1 1 d . C . P3 P 1.03743(8) 0.78048(7) 0.31194(6) 0.0419(2) Uani 1 1 d . C . P4 P 1.20018(8) 0.36596(8) 0.30115(6) 0.0472(3) Uani 1 1 d . . . P5 P 0.88189(9) 0.22084(9) 0.05557(6) 0.0509(3) Uani 1 1 d . C . P6 P 0.85455(8) 0.22903(7) 0.33660(6) 0.0434(3) Uani 1 1 d . . . P7 P 0.38973(15) 0.91104(15) 0.26516(14) 0.1045(7) Uani 1 1 d . . . S9 S 1.00713(8) 0.24847(9) 0.13102(6) 0.0516(3) Uani 1 1 d . . . S10 S 0.76861(8) 0.28462(8) 0.07068(6) 0.0484(3) Uani 1 1 d . . . S11 S 0.84178(8) 0.19224(7) 0.23597(6) 0.0458(2) Uani 1 1 d . B . S1 S 0.78515(8) 0.57489(7) 0.38805(6) 0.0440(2) Uani 1 1 d . . . S2 S 0.66282(8) 0.65136(8) 0.24586(6) 0.0461(2) Uani 1 1 d . . . S3 S 0.68064(8) 0.50481(8) 0.07623(6) 0.0505(3) Uani 1 1 d . . . S4 S 0.82459(8) 0.70864(8) 0.14359(6) 0.0485(3) Uani 1 1 d . . . S5 S 0.92202(8) 0.76271(7) 0.34278(6) 0.0457(2) Uani 1 1 d . . . S6 S 1.07720(8) 0.67471(7) 0.25341(5) 0.0430(2) Uani 1 1 d . . . S7 S 1.16619(8) 0.46456(8) 0.25192(6) 0.0447(2) Uani 1 1 d . B . S8 S 1.09799(8) 0.30518(8) 0.32748(6) 0.0459(3) Uani 1 1 d . B . S12 S 0.87367(8) 0.36230(7) 0.38327(6) 0.0457(2) Uani 1 1 d . E . 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 Br4 0.0439(2) 0.0523(3) 0.0371(2) 0.01090(19) 0.01359(18) -0.00025(19) Br1 0.0502(2) 0.0497(3) 0.0414(2) 0.00845(19) 0.00925(19) 0.0052(2) Br2 0.0481(2) 0.0483(3) 0.0605(3) 0.0157(2) 0.0199(2) 0.0049(2) Br3 0.0627(3) 0.0545(3) 0.0404(2) 0.0128(2) 0.0220(2) 0.0099(2) C1 0.048(3) 0.081(4) 0.074(4) 0.012(3) 0.023(3) -0.010(3) C2 0.126(7) 0.094(5) 0.177(9) 0.031(6) 0.084(7) -0.021(5) C3 0.064(5) 0.142(8) 0.238(13) 0.041(8) 0.002(6) 0.031(5) C4 0.065(3) 0.052(3) 0.063(3) 0.012(2) 0.015(3) 0.024(2) C5 0.122(6) 0.095(5) 0.098(5) 0.006(4) 0.048(5) 0.054(5) C6 0.109(6) 0.056(4) 0.159(8) 0.043(4) 0.034(5) 0.020(4) C7 0.065(4) 0.124(6) 0.098(5) 0.032(4) 0.014(3) 0.022(4) C8 0.098(6) 0.341(18) 0.201(12) 0.187(13) 0.034(7) 0.081(9) C9 0.067(5) 0.350(18) 0.134(8) 0.079(10) 0.042(5) 0.033(8) C10 0.151(8) 0.163(8) 0.083(5) 0.054(5) 0.069(5) 0.065(7) C11 0.34(2) 0.238(15) 0.076(7) -0.033(8) 0.086(10) -0.017(14) C12 0.230(14) 0.219(13) 0.179(11) 0.038(10) 0.135(11) -0.044(11) C13 0.096(4) 0.034(2) 0.077(4) 0.012(2) 0.045(3) 0.012(3) C14 0.100(5) 0.060(4) 0.127(6) 0.039(4) 0.040(4) 0.026(3) C15 0.129(6) 0.050(3) 0.148(7) 0.032(4) 0.074(5) 0.004(4) C16 0.051(3) 0.084(4) 0.071(4) -0.004(3) 0.017(3) -0.022(3) C17 0.065(4) 0.122(7) 0.147(8) 0.008(6) 0.005(5) -0.001(4) C18 0.090(5) 0.098(5) 0.130(7) -0.043(5) 0.020(5) -0.037(4) C19 0.059(3) 0.126(5) 0.063(4) 0.017(3) 0.014(3) -0.002(3) C20 0.219(12) 0.199(11) 0.075(5) 0.081(7) -0.011(6) 0.045(9) C21 0.103(6) 0.144(7) 0.173(10) -0.029(7) 0.023(6) -0.010(6) C22 0.092(5) 0.095(5) 0.106(5) 0.026(4) 0.037(4) 0.047(4) C23 0.195(12) 0.099(7) 0.194(11) 0.015(6) 0.000(9) 0.065(7) C24 0.072(7) 0.101(8) 0.26(2) 0.008(12) -0.007(9) 0.051(6) C24' 0.072(7) 0.101(8) 0.26(2) 0.008(12) -0.007(9) 0.051(6) C25 0.079(4) 0.104(5) 0.044(3) 0.016(3) 0.015(3) 0.006(3) C26 0.155(8) 0.174(8) 0.055(4) 0.016(5) 0.048(5) 0.069(7) C27 0.116(6) 0.106(5) 0.065(4) 0.028(4) 0.009(4) 0.014(4) C31 0.095(4) 0.060(3) 0.035(2) 0.018(2) 0.017(3) 0.021(3) C32 0.135(6) 0.100(5) 0.068(4) 0.049(4) 0.019(4) -0.004(4) C33 0.086(5) 0.188(9) 0.064(4) 0.054(5) 0.000(4) -0.009(5) C34 0.073(4) 0.108(5) 0.136(7) 0.072(5) 0.034(4) 0.016(4) C35 0.080(8) 0.123(10) 0.27(2) 0.038(12) 0.083(11) -0.006(7) C36 0.080(8) 0.123(10) 0.27(2) 0.038(12) 0.083(11) -0.006(7) C35' 0.080(8) 0.24(2) 0.148(12) 0.018(13) 0.052(8) -0.050(11) C36' 0.080(8) 0.24(2) 0.148(12) 0.018(13) 0.052(8) -0.050(11) Cu9 0.0663(4) 0.0580(4) 0.0773(4) 0.0178(3) 0.0283(3) 0.0116(3) Cu2 0.0588(4) 0.0639(4) 0.0569(4) 0.0009(3) 0.0126(3) 0.0105(3) Cu1 0.0670(4) 0.0670(4) 0.0556(4) 0.0200(3) 0.0079(3) 0.0049(3) Cu7 0.0780(4) 0.0518(3) 0.0574(4) 0.0185(3) 0.0281(3) 0.0175(3) Cu4 0.0537(3) 0.0641(4) 0.0785(4) 0.0318(3) 0.0267(3) 0.0109(3) Cu3 0.0654(4) 0.0524(4) 0.0786(4) 0.0102(3) 0.0345(3) 0.0015(3) Cu8 0.0691(4) 0.0476(3) 0.0644(4) 0.0121(3) 0.0159(3) 0.0132(3) Cu6 0.0967(5) 0.0537(4) 0.0542(4) 0.0150(3) 0.0291(3) 0.0053(3) Cu5 0.0752(4) 0.0807(4) 0.0535(4) 0.0286(3) 0.0275(3) 0.0333(4) Cu10 0.0521(3) 0.0543(3) 0.0474(3) 0.0139(3) 0.0171(3) 0.0024(3) Cu11 0.0535(3) 0.0570(3) 0.0464(3) 0.0140(3) 0.0171(3) 0.0053(3) F1 0.129(5) 0.326(10) 0.356(11) 0.219(9) 0.136(6) 0.121(6) F2 0.155(6) 0.371(12) 0.219(8) 0.132(8) 0.072(6) 0.145(7) F3 0.339(14) 0.66(3) 0.324(12) 0.386(17) 0.227(12) 0.335(17) F4 0.163(6) 0.342(12) 0.290(10) 0.216(10) 0.084(7) 0.088(7) F5 0.249(11) 0.159(7) 0.51(2) -0.102(10) -0.111(12) -0.006(7) F6 0.253(12) 0.149(7) 0.57(2) -0.062(11) 0.097(13) -0.072(7) O1 0.0440(17) 0.085(2) 0.0504(19) 0.0139(17) 0.0173(15) -0.0015(16) O2 0.0555(18) 0.0432(17) 0.0533(18) 0.0080(14) 0.0106(15) 0.0157(14) O3 0.058(2) 0.073(2) 0.074(2) 0.0233(19) 0.0140(18) 0.0220(18) O4 0.081(3) 0.096(3) 0.0426(19) 0.0255(19) 0.0180(18) 0.003(2) O5 0.083(2) 0.0350(16) 0.060(2) 0.0136(14) 0.0385(18) 0.0120(15) O6 0.0569(19) 0.064(2) 0.0495(19) -0.0061(16) 0.0184(15) -0.0090(16) O7 0.050(2) 0.134(4) 0.063(2) 0.050(2) 0.0005(17) -0.018(2) O8 0.083(3) 0.066(2) 0.100(3) 0.033(2) 0.053(2) 0.029(2) O9 0.070(2) 0.102(3) 0.0418(19) 0.0119(19) 0.0222(17) 0.012(2) O10 0.085(3) 0.050(2) 0.127(4) 0.000(2) 0.003(3) 0.011(2) O11 0.067(2) 0.0471(17) 0.0404(16) 0.0149(14) 0.0168(15) 0.0132(15) O12 0.063(2) 0.072(2) 0.085(3) 0.031(2) 0.034(2) -0.0039(18) P1 0.0405(6) 0.0414(6) 0.0409(6) 0.0087(5) 0.0151(5) 0.0060(5) P2 0.0493(6) 0.0563(7) 0.0396(6) 0.0175(5) 0.0124(5) 0.0103(5) P3 0.0510(6) 0.0350(5) 0.0409(6) 0.0066(5) 0.0183(5) 0.0012(5) P4 0.0399(6) 0.0537(7) 0.0579(7) 0.0252(6) 0.0206(5) 0.0119(5) P5 0.0579(7) 0.0521(7) 0.0385(6) 0.0027(5) 0.0142(5) 0.0100(6) P6 0.0493(6) 0.0399(6) 0.0470(6) 0.0170(5) 0.0190(5) 0.0034(5) P7 0.0788(12) 0.0937(14) 0.147(2) 0.0528(14) 0.0251(12) 0.0166(11) S9 0.0506(6) 0.0621(7) 0.0437(6) 0.0115(5) 0.0173(5) 0.0131(5) S10 0.0485(6) 0.0528(6) 0.0417(6) 0.0091(5) 0.0122(5) 0.0076(5) S11 0.0536(6) 0.0392(6) 0.0426(6) 0.0098(5) 0.0121(5) 0.0021(5) S1 0.0483(6) 0.0433(6) 0.0465(6) 0.0161(5) 0.0192(5) 0.0107(5) S2 0.0465(6) 0.0504(6) 0.0435(6) 0.0154(5) 0.0137(5) 0.0064(5) S3 0.0539(7) 0.0502(6) 0.0434(6) 0.0091(5) 0.0107(5) 0.0055(5) S4 0.0522(6) 0.0500(6) 0.0451(6) 0.0157(5) 0.0148(5) 0.0033(5) S5 0.0508(6) 0.0451(6) 0.0442(6) 0.0085(5) 0.0210(5) 0.0042(5) S6 0.0499(6) 0.0385(5) 0.0428(6) 0.0082(5) 0.0188(5) 0.0054(5) S7 0.0469(6) 0.0478(6) 0.0456(6) 0.0178(5) 0.0185(5) 0.0068(5) S8 0.0449(6) 0.0504(6) 0.0478(6) 0.0195(5) 0.0164(5) 0.0045(5) S12 0.0560(6) 0.0407(6) 0.0457(6) 0.0122(5) 0.0218(5) 0.0100(5) _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 Br4 Cu8 2.8132(8) . ? Br4 Cu9 2.8669(8) . ? Br4 Cu7 2.8684(8) . ? Br1 Cu7 2.4076(7) . ? Br1 Cu3 2.4430(8) . ? Br1 Cu4 2.4448(8) . ? Br2 Cu8 2.4272(8) . ? Br2 Cu6 2.4518(8) . ? Br2 Cu5 2.4682(8) . ? Br3 Cu9 2.4218(8) . ? Br3 Cu2 2.4276(8) . ? Br3 Cu1 2.4447(8) . ? C1 C3 1.458(9) . ? C1 O1 1.461(6) . ? C1 C2 1.477(9) . ? C1 H1 0.9800 . ? C2 H2A 0.9600 . ? C2 H2B 0.9600 . ? C2 H2C 0.9600 . ? C3 H3A 0.9600 . ? C3 H3B 0.9600 . ? C3 H3C 0.9600 . ? C4 C6 1.478(8) . ? C4 C5 1.483(9) . ? C4 O2 1.490(5) . ? C4 H4 0.9800 . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 O3 1.435(7) . ? C7 C9 1.481(11) . ? C7 C8 1.511(11) . ? C7 H7 0.9800 . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? C9 H9A 0.9600 . ? C9 H9B 0.9600 . ? C9 H9C 0.9600 . ? C10 O4 1.392(8) . ? C10 C12 1.466(13) . ? C10 C11 1.479(13) . ? C10 H10 0.9800 . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 H12A 0.9600 . ? C12 H12B 0.9600 . ? C12 H12C 0.9600 . ? C13 O5 1.480(5) . ? C13 C15 1.493(8) . ? C13 C14 1.498(9) . ? C13 H13 0.9800 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 O6 1.479(6) . ? C16 C17 1.497(10) . ? C16 C18 1.500(8) . ? C16 H16 0.9800 . ? C17 H17A 0.9600 . ? C17 H17B 0.9600 . ? C17 H17C 0.9600 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? C19 C21 1.457(11) . ? C19 C20 1.482(11) . ? C19 O7 1.487(7) . ? C19 H19 0.9800 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C23 1.425(12) . ? C22 O8 1.453(7) . ? C22 C24 1.525(8) . ? C22 C24' 1.80(4) . ? C22 H22 0.9800 . ? C23 H23A 0.9600 . ? C23 H23B 0.9600 . ? C23 H23C 0.9600 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C24' H24D 0.9600 . ? C24' H24E 0.9600 . ? C24' H24F 0.9600 . ? C25 C27 1.465(9) . ? C25 O9 1.481(6) . ? C25 C26 1.513(9) . ? C25 H25 0.9800 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 O10 1.452(9) . ? C28 C29 1.549(10) . ? C28 C30 1.595(10) . ? C28 H28 0.9800 . ? C29 H29A 0.9600 . ? C29 H29B 0.9600 . ? C29 H29C 0.9600 . ? C30 H30A 0.9600 . ? C30 H30B 0.9600 . ? C30 H30C 0.9600 . ? C28' O10 1.444(10) . ? C28' C29' 1.515(10) . ? C28' C30' 1.543(10) . ? C28' H28' 0.9800 . ? C29' H29D 0.9600 . ? C29' H29E 0.9600 . ? C29' H29F 0.9600 . ? C30' H30D 0.9600 . ? C30' H30E 0.9600 . ? C30' H30F 0.9600 . ? C31 C33 1.482(9) . ? C31 O11 1.501(5) . ? C31 C32 1.514(8) . ? C31 H31 0.9800 . ? C32 H32A 0.9600 . ? C32 H32B 0.9600 . ? C32 H32C 0.9600 . ? C33 H33A 0.9600 . ? C33 H33B 0.9600 . ? C33 H33C 0.9600 . ? C34 O12 1.427(7) . ? C34 C36' 1.514(9) . ? C34 C35 1.525(9) . ? C34 C36 1.534(9) . ? C34 C35' 1.557(9) . ? C34 H34 0.9800 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C35' H35D 0.9600 . ? C35' H35E 0.9600 . ? C35' H35F 0.9600 . ? C36' H36D 0.9600 . ? C36' H36E 0.9600 . ? C36' H36F 0.9600 . ? Cu9 S3 2.2648(13) . ? Cu9 S10 2.2801(14) . ? Cu2 S4 2.2355(13) . ? Cu2 S6 2.2649(13) . ? Cu2 Cu10 3.0387(8) . ? Cu1 S9 2.2514(14) . ? Cu1 S7 2.2655(13) . ? Cu1 Cu11 3.0509(9) . ? Cu7 S7 2.2711(13) . ? Cu7 S6 2.2768(12) . ? Cu4 S5 2.2494(13) . ? Cu4 S1 2.2642(12) . ? Cu3 S8 2.2547(13) . ? Cu3 S12 2.2624(13) . ? Cu8 S1 2.2736(13) . ? Cu8 S12 2.2953(13) . ? Cu6 S2 2.2508(13) . ? Cu6 S3 2.2623(13) . ? Cu5 S11 2.2483(12) . ? Cu5 S10 2.2693(13) . ? Cu5 Cu11 2.9541(9) . ? Cu10 S2 2.2479(12) . ? Cu10 S5 2.2500(13) . ? Cu10 S4 2.2545(12) . ? Cu11 S9 2.2384(13) . ? Cu11 S11 2.2467(13) . ? Cu11 S8 2.2591(13) . ? F1 P7 1.532(6) . ? F2 P7 1.536(7) . ? F3 P7 1.414(7) . ? F4 P7 1.555(8) . ? F5 P7 1.417(8) . ? F6 P7 1.401(9) . ? O1 P1 1.560(3) . ? O2 P1 1.562(3) . ? O3 P2 1.553(4) . ? O4 P2 1.564(3) . ? O5 P3 1.568(3) . ? O6 P3 1.559(3) . ? O7 P4 1.537(4) . ? O8 P4 1.583(4) . ? O9 P5 1.575(4) . ? O10 P5 1.557(4) . ? O11 P6 1.556(3) . ? O12 P6 1.557(3) . ? P1 S1 2.0194(15) . ? P1 S2 2.0213(15) . ? P2 S4 2.0215(17) . ? P2 S3 2.0249(17) . ? P3 S6 2.0080(15) . ? P3 S5 2.0244(15) . ? P4 S7 2.0027(16) . ? P4 S8 2.0227(15) . ? P5 S9 2.0138(17) . ? P5 S10 2.0175(17) . ? P6 S12 2.0168(16) . ? P6 S11 2.0257(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 Cu8 Br4 Cu9 119.08(2) . . ? Cu8 Br4 Cu7 119.92(2) . . ? Cu9 Br4 Cu7 120.98(2) . . ? Cu7 Br1 Cu3 79.31(3) . . ? Cu7 Br1 Cu4 81.26(3) . . ? Cu3 Br1 Cu4 93.24(3) . . ? Cu8 Br2 Cu6 79.83(3) . . ? Cu8 Br2 Cu5 79.67(3) . . ? Cu6 Br2 Cu5 94.32(3) . . ? Cu9 Br3 Cu2 80.28(3) . . ? Cu9 Br3 Cu1 82.90(3) . . ? Cu2 Br3 Cu1 95.44(3) . . ? C3 C1 O1 107.7(6) . . ? C3 C1 C2 114.4(6) . . ? O1 C1 C2 109.9(6) . . ? C3 C1 H1 108.2 . . ? O1 C1 H1 108.2 . . ? C2 C1 H1 108.2 . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? C1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? C1 C3 H3A 109.5 . . ? C1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? C1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? C6 C4 C5 114.7(6) . . ? C6 C4 O2 107.0(4) . . ? C5 C4 O2 106.0(5) . . ? C6 C4 H4 109.6 . . ? C5 C4 H4 109.6 . . ? O2 C4 H4 109.6 . . ? C4 C5 H5A 109.5 . . ? C4 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C4 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C4 C6 H6A 109.5 . . ? C4 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? C4 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? O3 C7 C9 107.1(6) . . ? O3 C7 C8 110.3(7) . . ? C9 C7 C8 114.1(8) . . ? O3 C7 H7 108.4 . . ? C9 C7 H7 108.4 . . ? C8 C7 H7 108.4 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? O4 C10 C12 108.7(8) . . ? O4 C10 C11 107.5(9) . . ? C12 C10 C11 110.6(9) . . ? O4 C10 H10 110.0 . . ? C12 C10 H10 110.0 . . ? C11 C10 H10 110.0 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? O5 C13 C15 106.8(4) . . ? O5 C13 C14 109.5(5) . . ? C15 C13 C14 114.9(5) . . ? O5 C13 H13 108.5 . . ? C15 C13 H13 108.5 . . ? C14 C13 H13 108.5 . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? O6 C16 C17 107.0(5) . . ? O6 C16 C18 107.6(5) . . ? C17 C16 C18 113.3(6) . . ? O6 C16 H16 109.6 . . ? C17 C16 H16 109.6 . . ? C18 C16 H16 109.6 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C21 C19 C20 113.2(7) . . ? C21 C19 O7 108.9(7) . . ? C20 C19 O7 103.3(6) . . ? C21 C19 H19 110.4 . . ? C20 C19 H19 110.4 . . ? O7 C19 H19 110.4 . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C23 C22 O8 112.7(7) . . ? C23 C22 C24 115.2(9) . . ? O8 C22 C24 107.7(7) . . ? C23 C22 C24' 79.7(11) . . ? O8 C22 C24' 90.3(9) . . ? C24 C22 C24' 51.5(11) . . ? C23 C22 H22 106.9 . . ? O8 C22 H22 106.9 . . ? C24 C22 H22 106.9 . . ? C24' C22 H22 156.7 . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? C22 C24' H24D 109.5 . . ? C22 C24' H24E 109.5 . . ? H24D C24' H24E 109.5 . . ? C22 C24' H24F 109.5 . . ? H24D C24' H24F 109.5 . . ? H24E C24' H24F 109.5 . . ? C27 C25 O9 108.4(5) . . ? C27 C25 C26 111.6(6) . . ? O9 C25 C26 105.3(5) . . ? C27 C25 H25 110.5 . . ? O9 C25 H25 110.5 . . ? C26 C25 H25 110.5 . . ? 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 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? O10 C28 C29 99.4(14) . . ? O10 C28 C30 129(2) . . ? C29 C28 C30 128(2) . . ? O10 C28 H28 96.2 . . ? C29 C28 H28 96.2 . . ? C30 C28 H28 96.2 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? O10 C28' C29' 89.6(15) . . ? O10 C28' C30' 99.0(18) . . ? C29' C28' C30' 96(2) . . ? O10 C28' H28' 121.7 . . ? C29' C28' H28' 121.7 . . ? C30' C28' H28' 121.7 . . ? C28' C29' H29D 109.5 . . ? C28' C29' H29E 109.5 . . ? H29D C29' H29E 109.5 . . ? C28' C29' H29F 109.5 . . ? H29D C29' H29F 109.5 . . ? H29E C29' H29F 109.5 . . ? C28' C30' H30D 109.5 . . ? C28' C30' H30E 109.5 . . ? H30D C30' H30E 109.5 . . ? C28' C30' H30F 109.5 . . ? H30D C30' H30F 109.5 . . ? H30E C30' H30F 109.5 . . ? C33 C31 O11 105.4(4) . . ? C33 C31 C32 112.7(6) . . ? O11 C31 C32 107.6(4) . . ? C33 C31 H31 110.3 . . ? O11 C31 H31 110.3 . . ? C32 C31 H31 110.3 . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? O12 C34 C36' 108.2(10) . . ? O12 C34 C35 106.1(9) . . ? C36' C34 C35 68.6(13) . . ? O12 C34 C36 108.9(10) . . ? C36' C34 C36 39.2(11) . . ? C35 C34 C36 106.0(12) . . ? O12 C34 C35' 108.3(10) . . ? C36' C34 C35' 108.7(11) . . ? C35 C34 C35' 43.3(12) . . ? C36 C34 C35' 137.5(11) . . ? O12 C34 H34 111.9 . . ? C36' C34 H34 137.5 . . ? C35 C34 H34 111.9 . . ? C36 C34 H34 111.9 . . ? C35' C34 H34 71.5 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? C34 C35' H35D 109.5 . . ? C34 C35' H35E 109.5 . . ? H35D C35' H35E 109.5 . . ? C34 C35' H35F 109.5 . . ? H35D C35' H35F 109.5 . . ? H35E C35' H35F 109.5 . . ? C34 C36' H36D 109.5 . . ? C34 C36' H36E 109.5 . . ? H36D C36' H36E 109.5 . . ? C34 C36' H36F 109.5 . . ? H36D C36' H36F 109.5 . . ? H36E C36' H36F 109.5 . . ? S3 Cu9 S10 104.98(5) . . ? S3 Cu9 Br3 126.39(4) . . ? S10 Cu9 Br3 123.71(4) . . ? S3 Cu9 Br4 101.86(4) . . ? S10 Cu9 Br4 99.74(4) . . ? Br3 Cu9 Br4 91.47(3) . . ? S4 Cu2 S6 119.00(5) . . ? S4 Cu2 Br3 123.89(4) . . ? S6 Cu2 Br3 112.61(4) . . ? S4 Cu2 Cu10 47.67(3) . . ? S6 Cu2 Cu10 95.07(3) . . ? Br3 Cu2 Cu10 145.67(3) . . ? S9 Cu1 S7 119.10(5) . . ? S9 Cu1 Br3 119.11(4) . . ? S7 Cu1 Br3 116.64(4) . . ? S9 Cu1 Cu11 47.01(3) . . ? S7 Cu1 Cu11 97.06(4) . . ? Br3 Cu1 Cu11 141.77(3) . . ? S7 Cu7 S6 99.71(4) . . ? S7 Cu7 Br1 127.71(4) . . ? S6 Cu7 Br1 127.96(4) . . ? S7 Cu7 Br4 100.63(4) . . ? S6 Cu7 Br4 98.40(4) . . ? Br1 Cu7 Br4 93.09(2) . . ? S5 Cu4 S1 119.76(5) . . ? S5 Cu4 Br1 118.60(4) . . ? S1 Cu4 Br1 116.62(4) . . ? S8 Cu3 S12 118.17(5) . . ? S8 Cu3 Br1 122.31(4) . . ? S12 Cu3 Br1 114.35(4) . . ? S1 Cu8 S12 100.10(5) . . ? S1 Cu8 Br2 127.25(4) . . ? S12 Cu8 Br2 127.40(4) . . ? S1 Cu8 Br4 101.84(4) . . ? S12 Cu8 Br4 99.89(4) . . ? Br2 Cu8 Br4 92.16(3) . . ? S2 Cu6 S3 117.51(5) . . ? S2 Cu6 Br2 121.55(4) . . ? S3 Cu6 Br2 115.00(4) . . ? S11 Cu5 S10 120.74(5) . . ? S11 Cu5 Br2 119.35(4) . . ? S10 Cu5 Br2 112.79(4) . . ? S11 Cu5 Cu11 48.89(3) . . ? S10 Cu5 Cu11 96.84(4) . . ? Br2 Cu5 Cu11 146.52(3) . . ? S2 Cu10 S5 120.03(5) . . ? S2 Cu10 S4 118.06(5) . . ? S5 Cu10 S4 120.65(5) . . ? S2 Cu10 Cu2 133.77(4) . . ? S5 Cu10 Cu2 96.19(3) . . ? S4 Cu10 Cu2 47.14(3) . . ? S9 Cu11 S11 122.98(5) . . ? S9 Cu11 S8 118.03(5) . . ? S11 Cu11 S8 117.54(5) . . ? S9 Cu11 Cu5 96.17(4) . . ? S11 Cu11 Cu5 48.94(3) . . ? S8 Cu11 Cu5 135.17(4) . . ? S9 Cu11 Cu1 47.37(4) . . ? S11 Cu11 Cu1 138.12(4) . . ? S8 Cu11 Cu1 93.45(3) . . ? Cu5 Cu11 Cu1 89.33(2) . . ? C1 O1 P1 129.7(3) . . ? C4 O2 P1 122.7(3) . . ? C7 O3 P2 124.5(4) . . ? C10 O4 P2 128.5(4) . . ? C13 O5 P3 123.6(3) . . ? C16 O6 P3 122.9(3) . . ? C19 O7 P4 129.7(4) . . ? C22 O8 P4 125.3(4) . . ? C25 O9 P5 124.0(4) . . ? C28' O10 C28 95.1(13) . . ? C28' O10 P5 123.4(11) . . ? C28 O10 P5 141.4(9) . . ? C31 O11 P6 123.3(3) . . ? C34 O12 P6 126.0(4) . . ? O1 P1 O2 104.74(19) . . ? O1 P1 S1 108.95(15) . . ? O2 P1 S1 103.38(13) . . ? O1 P1 S2 109.05(14) . . ? O2 P1 S2 110.72(14) . . ? S1 P1 S2 119.01(7) . . ? O3 P2 O4 103.9(2) . . ? O3 P2 S4 104.82(16) . . ? O4 P2 S4 109.68(16) . . ? O3 P2 S3 109.60(16) . . ? O4 P2 S3 109.56(17) . . ? S4 P2 S3 118.27(7) . . ? O6 P3 O5 109.54(19) . . ? O6 P3 S6 111.04(14) . . ? O5 P3 S6 103.16(12) . . ? O6 P3 S5 103.06(13) . . ? O5 P3 S5 110.56(14) . . ? S6 P3 S5 119.42(7) . . ? O7 P4 O8 106.5(2) . . ? O7 P4 S7 109.42(18) . . ? O8 P4 S7 102.15(15) . . ? O7 P4 S8 109.37(15) . . ? O8 P4 S8 109.73(16) . . ? S7 P4 S8 118.88(7) . . ? O10 P5 O9 108.4(3) . . ? O10 P5 S9 109.83(18) . . ? O9 P5 S9 102.30(15) . . ? O10 P5 S10 106.47(19) . . ? O9 P5 S10 110.80(16) . . ? S9 P5 S10 118.70(7) . . ? O11 P6 O12 102.08(19) . . ? O11 P6 S12 110.78(13) . . ? O12 P6 S12 109.58(16) . . ? O11 P6 S11 104.46(13) . . ? O12 P6 S11 110.13(16) . . ? S12 P6 S11 118.49(7) . . ? F6 P7 F3 87.0(10) . . ? F6 P7 F5 175.9(11) . . ? F3 P7 F5 90.4(10) . . ? F6 P7 F1 90.8(6) . . ? F3 P7 F1 88.8(5) . . ? F5 P7 F1 92.2(7) . . ? F6 P7 F2 88.3(6) . . ? F3 P7 F2 92.5(5) . . ? F5 P7 F2 88.8(7) . . ? F1 P7 F2 178.4(5) . . ? F6 P7 F4 90.8(9) . . ? F3 P7 F4 177.4(9) . . ? F5 P7 F4 91.9(8) . . ? F1 P7 F4 90.0(4) . . ? F2 P7 F4 88.6(4) . . ? P5 S9 Cu11 107.88(6) . . ? P5 S9 Cu1 106.23(6) . . ? Cu11 S9 Cu1 85.61(5) . . ? P5 S10 Cu5 107.39(6) . . ? P5 S10 Cu9 104.25(6) . . ? Cu5 S10 Cu9 92.07(5) . . ? P6 S11 Cu11 103.73(6) . . ? P6 S11 Cu5 112.04(6) . . ? Cu11 S11 Cu5 82.17(4) . . ? P1 S1 Cu4 103.71(6) . . ? P1 S1 Cu8 107.46(6) . . ? Cu4 S1 Cu8 92.44(5) . . ? P1 S2 Cu10 104.81(6) . . ? P1 S2 Cu6 109.67(6) . . ? Cu10 S2 Cu6 86.03(5) . . ? P2 S3 Cu6 102.45(6) . . ? P2 S3 Cu9 110.96(7) . . ? Cu6 S3 Cu9 91.12(5) . . ? P2 S4 Cu2 110.27(6) . . ? P2 S4 Cu10 103.08(6) . . ? Cu2 S4 Cu10 85.19(4) . . ? P3 S5 Cu4 110.21(6) . . ? P3 S5 Cu10 102.91(6) . . ? Cu4 S5 Cu10 86.21(4) . . ? P3 S6 Cu2 104.05(6) . . ? P3 S6 Cu7 105.50(6) . . ? Cu2 S6 Cu7 97.07(5) . . ? P4 S7 Cu1 102.98(6) . . ? P4 S7 Cu7 107.56(6) . . ? Cu1 S7 Cu7 92.93(5) . . ? P4 S8 Cu3 109.06(6) . . ? P4 S8 Cu11 105.14(6) . . ? Cu3 S8 Cu11 86.76(4) . . ? P6 S12 Cu3 102.46(6) . . ? P6 S12 Cu8 108.91(6) . . ? Cu3 S12 Cu8 93.41(5) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.839 _refine_diff_density_min -0.634 _refine_diff_density_rms 0.095 _database_code_depnum_ccdc_archive 'CCDC 943813' ####################################################################### # # 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_3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H84 Br3 Cu11 O12 P6 S13' _chemical_formula_weight 2250.30 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 17.6202(4) _cell_length_b 21.3395(5) _cell_length_c 21.0229(4) _cell_angle_alpha 90.00 _cell_angle_beta 95.7150(10) _cell_angle_gamma 90.00 _cell_volume 7865.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 296(2) _cell_measurement_reflns_used 9871 _cell_measurement_theta_min 2.32 _cell_measurement_theta_max 26.35 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.900 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4472 _exptl_absorpt_coefficient_mu 4.944 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2842 _exptl_absorpt_correction_T_max 0.4870 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 296(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 61461 _diffrn_reflns_av_R_equivalents 0.0339 _diffrn_reflns_av_sigmaI/netI 0.0287 _diffrn_reflns_limit_h_min -20 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_theta_min 1.50 _diffrn_reflns_theta_max 25.00 _reflns_number_total 13829 _reflns_number_gt 10956 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. Restraints on bond lengths and atomic displacement paremeters were applied by using DFIX, DELU, and EADP command in SHELX program. C6, C11, C12 were split and refined anisotropically, and they were finally fixed to 50/50, 60/40 and 60/40, respectively. The used restraints and constraints are: DFIX 1.54 0.01 C10 C11 C10 C12 C10 C11' C10 C12' DELU 0.0015 S13 CU8 DELU 0.0015 S13 CU9 DELU C4 C5 DELU C4 C6 DELU C10 C11 DELU C10 C12 DELU C10 C11' DELU C10 C12' DELU C19 C20 DELU C19 C21 DELU C22 C23 DELU C22 C24 DELU C34 C35 DELU C34 C36 EADP C11' C12' EADP C11 C12 EADP C23 C24 EADP C35 C36 ; _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^)+(0.0538P)^2^+21.7340P] 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 13829 _refine_ls_number_parameters 794 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.0562 _refine_ls_R_factor_gt 0.0407 _refine_ls_wR_factor_ref 0.1129 _refine_ls_wR_factor_gt 0.1024 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.136 _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 Br1 Br 0.17871(3) 0.86655(3) 0.90190(3) 0.04219(15) Uani 1 1 d . B . Br2 Br 0.06917(3) 0.57631(3) 0.84526(3) 0.04169(15) Uani 1 1 d . B . Br3 Br -0.11816(3) 0.80250(3) 0.69135(3) 0.04564(15) Uani 1 1 d . . . C1 C 0.3736(4) 0.6277(3) 0.7719(3) 0.0557(17) Uani 1 1 d . . . H1 H 0.3251 0.6102 0.7828 0.067 Uiso 1 1 calc R . . C2 C 0.4345(6) 0.6023(5) 0.8153(5) 0.100(3) Uani 1 1 d . . . H2A H 0.4816 0.6226 0.8083 0.150 Uiso 1 1 calc R . . H2B H 0.4389 0.5581 0.8079 0.150 Uiso 1 1 calc R . . H2C H 0.4235 0.6093 0.8585 0.150 Uiso 1 1 calc R . . C3 C 0.3832(6) 0.6116(5) 0.7041(5) 0.105(3) Uani 1 1 d . . . H3A H 0.3511 0.6382 0.6761 0.158 Uiso 1 1 calc R . . H3B H 0.3692 0.5686 0.6962 0.158 Uiso 1 1 calc R . . H3C H 0.4355 0.6177 0.6964 0.158 Uiso 1 1 calc R . . C4 C 0.4117(4) 0.7655(4) 0.9133(4) 0.074(2) Uani 1 1 d U . . H4 H 0.3966 0.7252 0.9305 0.089 Uiso 1 1 calc R A 1 C5 C 0.4927(5) 0.7690(6) 0.9029(7) 0.137(5) Uani 1 1 d U B . H5A H 0.4999 0.7520 0.8616 0.206 Uiso 1 1 calc R . . H5B H 0.5222 0.7453 0.9354 0.206 Uiso 1 1 calc R . . H5C H 0.5090 0.8120 0.9048 0.206 Uiso 1 1 calc R . . C6 C 0.399(2) 0.8232(16) 0.9578(16) 0.114(12) Uani 0.50 1 d PU B 1 H6A H 0.4211 0.8600 0.9414 0.171 Uiso 0.50 1 calc PR B 1 H6B H 0.4217 0.8149 1.0003 0.171 Uiso 0.50 1 calc PR B 1 H6C H 0.3448 0.8299 0.9590 0.171 Uiso 0.50 1 calc PR B 1 C6' C 0.389(3) 0.7906(14) 0.9716(19) 0.143(19) Uani 0.50 1 d P B 2 H6'1 H 0.4103 0.8318 0.9784 0.215 Uiso 0.50 1 calc PR B 2 H6'2 H 0.4076 0.7639 1.0066 0.215 Uiso 0.50 1 calc PR B 2 H6'3 H 0.3346 0.7929 0.9691 0.215 Uiso 0.50 1 calc PR B 2 C7 C -0.0199(5) 0.7398(4) 1.1334(3) 0.069(2) Uani 1 1 d . . . H7 H -0.0061 0.7833 1.1444 0.083 Uiso 1 1 calc R . . C8 C -0.1014(5) 0.7374(5) 1.1062(5) 0.096(3) Uani 1 1 d . . . H8A H -0.1094 0.7664 1.0713 0.145 Uiso 1 1 calc R . . H8B H -0.1336 0.7485 1.1387 0.145 Uiso 1 1 calc R . . H8C H -0.1136 0.6958 1.0912 0.145 Uiso 1 1 calc R . . C9 C -0.0033(8) 0.6997(6) 1.1905(5) 0.140(6) Uani 1 1 d . . . H9A H -0.0135 0.6568 1.1791 0.211 Uiso 1 1 calc R . . H9B H -0.0349 0.7122 1.2229 0.211 Uiso 1 1 calc R . . H9C H 0.0494 0.7042 1.2065 0.211 Uiso 1 1 calc R . . C10 C 0.1984(4) 0.7839(4) 1.1154(4) 0.073(2) Uani 1 1 d DU . . H10 H 0.2168 0.7453 1.0969 0.088 Uiso 1 1 calc R C 1 C11 C 0.2553(10) 0.8365(9) 1.1101(9) 0.112(5) Uani 0.60 1 d PDU D 1 H11A H 0.2569 0.8473 1.0659 0.169 Uiso 0.60 1 calc PR D 1 H11B H 0.3049 0.8230 1.1278 0.169 Uiso 0.60 1 calc PR D 1 H11C H 0.2400 0.8724 1.1331 0.169 Uiso 0.60 1 calc PR D 1 C12 C 0.1857(10) 0.7735(11) 1.1858(6) 0.112(5) Uani 0.60 1 d PDU D 1 H12A H 0.1590 0.8088 1.2011 0.169 Uiso 0.60 1 calc PR D 1 H12B H 0.2340 0.7690 1.2107 0.169 Uiso 0.60 1 calc PR D 1 H12C H 0.1559 0.7362 1.1896 0.169 Uiso 0.60 1 calc PR D 1 C11' C 0.2623(12) 0.8109(16) 1.0790(10) 0.110(6) Uani 0.40 1 d PDU D 2 H11D H 0.2692 0.7848 1.0428 0.165 Uiso 0.40 1 calc PR D 2 H11E H 0.3089 0.8124 1.1068 0.165 Uiso 0.40 1 calc PR D 2 H11F H 0.2488 0.8525 1.0646 0.165 Uiso 0.40 1 calc PR D 2 C12' C 0.1995(15) 0.8206(14) 1.1777(9) 0.110(6) Uani 0.40 1 d PDU D 2 H12D H 0.2513 0.8298 1.1936 0.165 Uiso 0.40 1 calc PR D 2 H12E H 0.1761 0.7961 1.2087 0.165 Uiso 0.40 1 calc PR D 2 H12F H 0.1718 0.8591 1.1701 0.165 Uiso 0.40 1 calc PR D 2 C13 C 0.1521(5) 0.6050(4) 0.5358(4) 0.080(3) Uani 1 1 d . . . H13 H 0.1881 0.5820 0.5657 0.096 Uiso 1 1 calc R . . C14 C 0.1901(7) 0.6617(6) 0.5139(6) 0.134(5) Uani 1 1 d . . . H14A H 0.1556 0.6839 0.4837 0.201 Uiso 1 1 calc R . . H14B H 0.2346 0.6498 0.4941 0.201 Uiso 1 1 calc R . . H14C H 0.2047 0.6883 0.5499 0.201 Uiso 1 1 calc R . . C15 C 0.1229(7) 0.5624(7) 0.4830(5) 0.144(5) Uani 1 1 d . . . H15A H 0.0900 0.5854 0.4521 0.216 Uiso 1 1 calc R . . H15B H 0.0947 0.5288 0.4999 0.216 Uiso 1 1 calc R . . H15C H 0.1649 0.5455 0.4628 0.216 Uiso 1 1 calc R . . C16 C 0.0971(5) 0.4899(3) 0.6893(4) 0.070(2) Uani 1 1 d . . . H16 H 0.1106 0.5142 0.7283 0.084 Uiso 1 1 calc R . . C17 C 0.1650(7) 0.4538(5) 0.6740(6) 0.137(5) Uani 1 1 d . . . H17A H 0.1513 0.4271 0.6378 0.205 Uiso 1 1 calc R . . H17B H 0.1833 0.4286 0.7101 0.205 Uiso 1 1 calc R . . H17C H 0.2044 0.4822 0.6640 0.205 Uiso 1 1 calc R . . C18 C 0.0290(8) 0.4515(6) 0.6977(6) 0.145(5) Uani 1 1 d . . . H18A H -0.0086 0.4770 0.7153 0.218 Uiso 1 1 calc R . . H18B H 0.0431 0.4174 0.7263 0.218 Uiso 1 1 calc R . . H18C H 0.0084 0.4353 0.6571 0.218 Uiso 1 1 calc R . . C19 C -0.2793(4) 0.6591(3) 0.9037(4) 0.0574(17) Uani 1 1 d U . . H19 H -0.2502 0.6977 0.8993 0.069 Uiso 1 1 calc R . . C20 C -0.3078(7) 0.6575(6) 0.9662(5) 0.138(5) Uani 1 1 d U . . H20A H -0.3378 0.6203 0.9698 0.206 Uiso 1 1 calc R . . H20B H -0.3388 0.6938 0.9713 0.206 Uiso 1 1 calc R . . H20C H -0.2656 0.6572 0.9988 0.206 Uiso 1 1 calc R . . C21 C -0.3423(6) 0.6552(8) 0.8519(5) 0.155(6) Uani 1 1 d U . . H21A H -0.3229 0.6400 0.8137 0.233 Uiso 1 1 calc R . . H21B H -0.3640 0.6961 0.8441 0.233 Uiso 1 1 calc R . . H21C H -0.3807 0.6271 0.8643 0.233 Uiso 1 1 calc R . . C22 C -0.1020(6) 0.4978(3) 0.9313(4) 0.083(2) Uani 1 1 d U . . H22 H -0.0730 0.5221 0.9650 0.099 Uiso 1 1 calc R . . C23 C -0.1726(8) 0.4729(5) 0.9549(7) 0.152(4) Uani 1 1 d U . . H23A H -0.2042 0.5070 0.9660 0.228 Uiso 1 1 calc R . . H23B H -0.1595 0.4473 0.9920 0.228 Uiso 1 1 calc R . . H23C H -0.1999 0.4480 0.9221 0.228 Uiso 1 1 calc R . . C24 C -0.0540(8) 0.4466(5) 0.9092(7) 0.152(4) Uani 1 1 d U . . H24A H -0.0821 0.4241 0.8751 0.228 Uiso 1 1 calc R . . H24B H -0.0398 0.4186 0.9440 0.228 Uiso 1 1 calc R . . H24C H -0.0088 0.4642 0.8942 0.228 Uiso 1 1 calc R . . C25 C 0.2276(4) 0.9474(4) 0.6365(4) 0.066(2) Uani 1 1 d . . . H25 H 0.2216 0.9584 0.6810 0.080 Uiso 1 1 calc R . . C26 C 0.3088(5) 0.9268(4) 0.6307(5) 0.096(3) Uani 1 1 d . . . H26A H 0.3190 0.8888 0.6544 0.144 Uiso 1 1 calc R . . H26B H 0.3433 0.9589 0.6476 0.144 Uiso 1 1 calc R . . H26C H 0.3156 0.9197 0.5866 0.144 Uiso 1 1 calc R . . C27 C 0.2038(6) 1.0001(4) 0.5946(6) 0.118(4) Uani 1 1 d . . . H27A H 0.2101 0.9891 0.5511 0.176 Uiso 1 1 calc R . . H27B H 0.2344 1.0361 0.6068 0.176 Uiso 1 1 calc R . . H27C H 0.1511 1.0095 0.5983 0.176 Uiso 1 1 calc R . . C28 C -0.0357(4) 0.9110(3) 0.5792(3) 0.0598(18) Uani 1 1 d . . . H28 H -0.0514 0.8802 0.6098 0.072 Uiso 1 1 calc R . . C29 C -0.0603(7) 0.8896(6) 0.5134(6) 0.141(5) Uani 1 1 d . . . H29A H -0.0394 0.9169 0.4833 0.212 Uiso 1 1 calc R . . H29B H -0.1150 0.8905 0.5065 0.212 Uiso 1 1 calc R . . H29C H -0.0426 0.8476 0.5078 0.212 Uiso 1 1 calc R . . C30 C -0.0683(6) 0.9726(5) 0.5927(6) 0.119(4) Uani 1 1 d . . . H30A H -0.0547 0.9832 0.6368 0.179 Uiso 1 1 calc R . . H30B H -0.1228 0.9708 0.5844 0.179 Uiso 1 1 calc R . . H30C H -0.0486 1.0037 0.5659 0.179 Uiso 1 1 calc R . . C31 C -0.1067(4) 0.9678(3) 0.9777(3) 0.0562(17) Uani 1 1 d . . . H31 H -0.0526 0.9658 0.9710 0.067 Uiso 1 1 calc R . . C32 C -0.1138(5) 0.9593(4) 1.0478(3) 0.077(2) Uani 1 1 d . . . H32A H -0.1667 0.9608 1.0553 0.115 Uiso 1 1 calc R . . H32B H -0.0866 0.9922 1.0715 0.115 Uiso 1 1 calc R . . H32C H -0.0927 0.9195 1.0615 0.115 Uiso 1 1 calc R . . C33 C -0.1376(7) 1.0276(4) 0.9517(4) 0.094(3) Uani 1 1 d . . . H33A H -0.1301 1.0303 0.9072 0.142 Uiso 1 1 calc R . . H33B H -0.1118 1.0617 0.9744 0.142 Uiso 1 1 calc R . . H33C H -0.1912 1.0297 0.9566 0.142 Uiso 1 1 calc R . . C34 C -0.2300(5) 0.9342(5) 0.7721(4) 0.084(2) Uani 1 1 d U . . H34 H -0.2039 0.8998 0.7524 0.100 Uiso 1 1 calc R . . C35 C -0.3123(7) 0.9229(8) 0.7652(7) 0.163(4) Uani 1 1 d U . . H35A H -0.3244 0.8915 0.7953 0.244 Uiso 1 1 calc R . . H35B H -0.3279 0.9088 0.7226 0.244 Uiso 1 1 calc R . . H35C H -0.3385 0.9611 0.7733 0.244 Uiso 1 1 calc R . . C36 C -0.2090(8) 0.9957(7) 0.7436(7) 0.163(4) Uani 1 1 d U . . H36A H -0.2392 1.0286 0.7593 0.244 Uiso 1 1 calc R . . H36B H -0.2183 0.9935 0.6978 0.244 Uiso 1 1 calc R . . H36C H -0.1559 1.0041 0.7554 0.244 Uiso 1 1 calc R . . Cu1 Cu 0.03184(8) 0.67742(8) 0.90093(7) 0.0543(4) Uani 0.80 1 d P B . Cu2 Cu 0.13536(5) 0.66896(5) 0.79551(4) 0.0636(2) Uani 1 1 d . . . Cu7 Cu -0.02139(5) 0.63174(5) 0.76923(4) 0.0585(2) Uani 1 1 d . . . Cu3 Cu -0.09405(6) 0.74695(4) 0.80249(4) 0.0622(2) Uani 1 1 d . . . Cu4 Cu 0.01178(9) 0.74139(7) 0.69851(8) 0.0557(4) Uani 0.80 1 d P . . Cu9 Cu -0.01537(5) 0.85416(5) 0.76070(4) 0.0636(2) Uani 1 1 d U B . Cu5 Cu 0.03798(8) 0.83760(8) 0.89195(7) 0.0615(4) Uani 0.90 1 d P B . Cu6 Cu 0.1574(2) 0.8361(2) 0.7880(2) 0.0687(9) Uani 0.70 1 d P . . Cu8 Cu 0.16706(5) 0.75319(4) 0.90509(4) 0.0596(2) Uani 1 1 d U B . Cu11 Cu -0.08275(4) 0.75640(3) 0.93178(4) 0.04071(17) Uani 1 1 d . B . Cu10 Cu 0.16899(4) 0.73844(3) 0.69058(4) 0.04442(18) Uani 1 1 d . B . O1 O 0.3707(3) 0.6957(2) 0.7775(3) 0.0649(14) Uani 1 1 d . B . O2 O 0.3663(2) 0.7840(2) 0.8547(2) 0.0572(12) Uani 1 1 d . B . O3 O 0.0298(3) 0.7162(2) 1.0857(2) 0.0557(12) Uani 1 1 d . D . O4 O 0.1269(3) 0.8043(2) 1.0795(2) 0.0600(13) Uani 1 1 d . D . O5 O 0.0875(3) 0.6257(2) 0.56937(19) 0.0541(11) Uani 1 1 d . . . O6 O 0.0789(3) 0.53269(19) 0.6363(2) 0.0524(11) Uani 1 1 d . . . O7 O -0.2305(2) 0.60519(19) 0.89785(19) 0.0434(9) Uani 1 1 d . . . O8 O -0.1243(2) 0.53818(17) 0.87599(18) 0.0409(9) Uani 1 1 d . . . O9 O 0.1817(2) 0.89157(19) 0.61782(19) 0.0467(10) Uani 1 1 d . . . O10 O 0.0476(3) 0.9162(2) 0.5861(2) 0.0494(10) Uani 1 1 d . . . O11 O -0.1452(2) 0.91382(18) 0.94606(18) 0.0415(9) Uani 1 1 d . . . O12 O -0.2053(2) 0.9371(2) 0.8393(2) 0.0520(11) Uani 1 1 d . . . P1 P 0.31378(8) 0.73765(7) 0.81174(8) 0.0381(3) Uani 1 1 d . . . P2 P 0.07153(9) 0.75898(7) 1.03908(7) 0.0358(3) Uani 1 1 d . . . P3 P 0.07966(9) 0.60613(7) 0.64039(7) 0.0382(3) Uani 1 1 d . . . P4 P -0.14611(8) 0.60901(7) 0.87931(7) 0.0324(3) Uani 1 1 d . . . P5 P 0.09993(9) 0.87665(7) 0.63637(7) 0.0369(3) Uani 1 1 d . . . P6 P -0.14111(8) 0.89519(7) 0.87398(7) 0.0333(3) Uani 1 1 d . . . S1 S 0.26032(8) 0.79561(7) 0.74591(7) 0.0398(3) Uani 1 1 d . B . S2 S 0.25050(8) 0.68420(7) 0.86440(7) 0.0377(3) Uani 1 1 d . B . S3 S -0.00227(8) 0.81937(6) 0.99294(7) 0.0365(3) Uani 1 1 d . B . S4 S 0.12701(8) 0.69748(6) 0.98829(7) 0.0366(3) Uani 1 1 d . B . S5 S 0.17285(8) 0.63286(7) 0.69789(7) 0.0411(3) Uani 1 1 d . . . S6 S -0.02153(8) 0.63932(7) 0.66083(7) 0.0396(3) Uani 1 1 d . . . S7 S -0.07987(8) 0.65204(6) 0.95040(7) 0.0370(3) Uani 1 1 d . B . S8 S -0.14537(8) 0.64392(7) 0.79083(6) 0.0353(3) Uani 1 1 d . . . S9 S 0.08346(9) 0.78460(7) 0.61785(7) 0.0407(3) Uani 1 1 d . . . S10 S 0.08683(9) 0.90702(7) 0.72493(7) 0.0394(3) Uani 1 1 d . B . S11 S -0.17373(8) 0.80449(6) 0.86621(7) 0.0375(3) Uani 1 1 d . . . S12 S -0.03932(8) 0.91795(6) 0.84490(7) 0.0369(3) Uani 1 1 d . B . S13 S 0.04400(7) 0.74938(6) 0.81235(6) 0.0278(3) Uani 1 1 d U B . Cu1' Cu 0.0333(3) 0.6536(2) 0.9246(3) 0.0415(12) Uani 0.20 1 d P . . Cu4' Cu -0.0057(3) 0.7436(3) 0.6657(3) 0.0476(13) Uani 0.20 1 d P . . Cu5' Cu 0.0409(6) 0.8599(5) 0.9125(5) 0.031(2) Uani 0.10 1 d P . . Cu6' Cu 0.1405(5) 0.8198(4) 0.7880(6) 0.0431(13) Uani 0.30 1 d P . . 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 Br1 0.0421(3) 0.0395(3) 0.0452(3) -0.0068(3) 0.0055(3) -0.0053(2) Br2 0.0471(3) 0.0313(3) 0.0479(3) 0.0012(2) 0.0111(3) 0.0045(2) Br3 0.0448(3) 0.0482(4) 0.0431(3) 0.0027(3) -0.0003(3) 0.0030(3) C1 0.053(4) 0.052(4) 0.065(4) 0.001(3) 0.021(3) 0.009(3) C2 0.093(7) 0.081(7) 0.119(8) -0.002(6) -0.018(6) 0.031(5) C3 0.108(8) 0.126(9) 0.087(7) -0.019(6) 0.035(6) 0.022(7) C4 0.063(4) 0.077(5) 0.075(6) 0.010(4) -0.029(4) -0.009(4) C5 0.057(5) 0.154(11) 0.190(13) -0.014(10) -0.044(7) 0.011(6) C6 0.106(19) 0.15(3) 0.072(17) -0.029(18) -0.039(14) 0.03(2) C6' 0.21(4) 0.11(3) 0.10(2) -0.02(2) -0.04(2) 0.06(3) C7 0.096(6) 0.072(5) 0.043(4) 0.001(3) 0.029(4) 0.015(4) C8 0.082(6) 0.128(9) 0.086(7) -0.004(6) 0.040(5) -0.014(6) C9 0.206(13) 0.163(12) 0.065(6) 0.044(7) 0.073(8) 0.081(10) C10 0.068(5) 0.075(5) 0.068(5) -0.010(4) -0.030(4) 0.016(4) C11 0.082(8) 0.159(13) 0.086(7) 0.030(9) -0.039(7) -0.031(8) C12 0.082(8) 0.159(13) 0.086(7) 0.030(9) -0.039(7) -0.031(8) C11' 0.092(12) 0.15(2) 0.074(10) -0.009(10) -0.046(8) -0.025(12) C12' 0.092(12) 0.15(2) 0.074(10) -0.009(10) -0.046(8) -0.025(12) C13 0.085(6) 0.107(7) 0.051(4) 0.005(4) 0.028(4) 0.046(5) C14 0.138(10) 0.137(10) 0.143(10) 0.053(8) 0.102(9) 0.047(8) C15 0.154(11) 0.195(14) 0.083(7) -0.067(8) 0.016(7) 0.052(10) C16 0.106(6) 0.039(4) 0.063(5) -0.002(3) 0.005(4) 0.002(4) C17 0.165(12) 0.086(8) 0.154(11) -0.007(7) -0.012(9) 0.071(8) C18 0.190(14) 0.106(9) 0.145(11) 0.007(8) 0.040(10) -0.076(9) C19 0.045(4) 0.046(4) 0.083(5) 0.014(4) 0.019(3) 0.004(3) C20 0.156(11) 0.177(13) 0.085(7) -0.015(7) 0.041(7) 0.091(10) C21 0.082(7) 0.283(19) 0.098(8) -0.003(10) -0.009(6) 0.095(10) C22 0.145(8) 0.038(4) 0.058(5) 0.004(3) -0.022(5) 0.001(4) C23 0.174(8) 0.097(6) 0.201(9) 0.093(6) 0.101(8) 0.074(6) C24 0.174(8) 0.097(6) 0.201(9) 0.093(6) 0.101(8) 0.074(6) C25 0.076(5) 0.057(5) 0.071(5) -0.009(4) 0.028(4) -0.022(4) C26 0.065(5) 0.073(6) 0.152(10) 0.020(6) 0.017(6) -0.016(4) C27 0.101(8) 0.050(5) 0.204(13) 0.032(7) 0.030(8) -0.005(5) C28 0.061(4) 0.060(5) 0.057(4) 0.022(3) -0.004(3) -0.004(3) C29 0.151(11) 0.136(10) 0.117(9) -0.038(8) -0.081(8) 0.024(9) C30 0.079(7) 0.124(9) 0.152(11) -0.037(8) -0.006(7) 0.031(6) C31 0.071(4) 0.044(4) 0.056(4) -0.018(3) 0.018(3) -0.006(3) C32 0.114(7) 0.063(5) 0.053(4) -0.018(4) 0.010(4) -0.002(5) C33 0.166(10) 0.042(5) 0.073(6) -0.009(4) 0.006(6) 0.003(5) C34 0.090(6) 0.091(6) 0.065(5) 0.004(4) -0.020(4) 0.033(5) C35 0.125(7) 0.209(11) 0.144(8) 0.083(8) -0.040(6) -0.012(7) C36 0.125(7) 0.209(11) 0.144(8) 0.083(8) -0.040(6) -0.012(7) Cu1 0.0483(7) 0.0607(10) 0.0548(9) -0.0175(7) 0.0100(7) -0.0049(7) Cu2 0.0608(5) 0.0766(6) 0.0545(5) -0.0042(4) 0.0104(4) -0.0197(5) Cu7 0.0496(5) 0.0774(6) 0.0504(5) 0.0110(4) 0.0136(4) 0.0127(4) Cu3 0.0901(7) 0.0442(5) 0.0550(5) -0.0006(4) 0.0209(5) -0.0037(4) Cu4 0.0650(9) 0.0418(7) 0.0639(9) -0.0034(8) 0.0236(8) 0.0003(6) Cu9 0.0668(6) 0.0698(6) 0.0568(5) -0.0153(4) 0.0199(4) -0.0164(4) Cu5 0.0474(6) 0.0819(12) 0.0565(9) 0.0211(7) 0.0113(6) 0.0158(8) Cu6 0.085(3) 0.076(3) 0.0449(11) -0.0013(16) 0.0011(17) 0.0361(16) Cu8 0.0704(6) 0.0449(5) 0.0683(6) 0.0036(4) 0.0311(4) 0.0054(4) Cu11 0.0441(4) 0.0332(4) 0.0439(4) -0.0017(3) -0.0004(3) 0.0011(3) Cu10 0.0473(4) 0.0391(4) 0.0466(4) 0.0007(3) 0.0032(3) -0.0008(3) O1 0.061(3) 0.047(3) 0.094(4) 0.016(3) 0.044(3) 0.014(2) O2 0.047(3) 0.052(3) 0.069(3) 0.009(2) -0.011(2) -0.009(2) O3 0.082(3) 0.045(3) 0.044(2) 0.008(2) 0.027(2) 0.015(2) O4 0.058(3) 0.052(3) 0.064(3) -0.018(2) -0.024(2) 0.013(2) O5 0.060(3) 0.066(3) 0.037(2) 0.002(2) 0.012(2) 0.018(2) O6 0.064(3) 0.037(2) 0.053(3) -0.013(2) -0.004(2) 0.008(2) O7 0.037(2) 0.043(2) 0.051(2) 0.0024(19) 0.0109(18) -0.0045(18) O8 0.054(2) 0.027(2) 0.041(2) 0.0015(17) -0.0020(18) -0.0023(17) O9 0.052(2) 0.044(2) 0.048(2) -0.0019(19) 0.020(2) -0.0083(19) O10 0.059(3) 0.044(2) 0.045(2) 0.0148(19) 0.004(2) 0.004(2) O11 0.047(2) 0.036(2) 0.043(2) -0.0063(17) 0.0127(18) -0.0011(18) O12 0.049(2) 0.045(2) 0.060(3) 0.006(2) -0.002(2) 0.015(2) P1 0.0304(7) 0.0363(8) 0.0480(9) 0.0041(7) 0.0055(6) 0.0007(6) P2 0.0433(8) 0.0334(8) 0.0299(7) -0.0022(6) 0.0000(6) 0.0034(6) P3 0.0438(8) 0.0361(8) 0.0349(8) -0.0043(6) 0.0047(6) 0.0056(6) P4 0.0333(7) 0.0296(7) 0.0345(7) 0.0010(6) 0.0037(6) -0.0018(6) P5 0.0447(8) 0.0336(8) 0.0333(7) 0.0050(6) 0.0079(6) 0.0005(6) P6 0.0346(7) 0.0285(7) 0.0369(8) 0.0006(6) 0.0041(6) 0.0053(6) S1 0.0387(7) 0.0356(8) 0.0452(8) 0.0064(6) 0.0056(6) -0.0037(6) S2 0.0367(7) 0.0372(8) 0.0402(8) 0.0050(6) 0.0077(6) 0.0038(6) S3 0.0406(7) 0.0311(7) 0.0371(7) -0.0037(6) 0.0010(6) 0.0039(6) S4 0.0396(7) 0.0340(7) 0.0359(7) 0.0004(6) 0.0030(6) 0.0061(6) S5 0.0376(7) 0.0368(8) 0.0487(8) -0.0032(6) 0.0034(6) 0.0044(6) S6 0.0377(7) 0.0412(8) 0.0398(8) -0.0052(6) 0.0028(6) 0.0009(6) S7 0.0456(8) 0.0307(7) 0.0338(7) -0.0004(6) -0.0006(6) -0.0022(6) S8 0.0353(7) 0.0362(7) 0.0339(7) 0.0010(6) 0.0008(6) -0.0024(6) S9 0.0512(8) 0.0346(8) 0.0363(8) 0.0002(6) 0.0042(6) 0.0008(6) S10 0.0487(8) 0.0335(8) 0.0371(8) 0.0015(6) 0.0102(6) 0.0017(6) S11 0.0336(7) 0.0315(7) 0.0468(8) -0.0012(6) 0.0021(6) -0.0007(6) S12 0.0401(7) 0.0308(7) 0.0410(8) 0.0005(6) 0.0097(6) 0.0004(6) S13 0.0299(6) 0.0225(6) 0.0310(6) -0.0035(5) 0.0032(5) -0.0031(5) Cu1' 0.047(2) 0.038(3) 0.039(3) -0.0027(19) 0.002(2) 0.000(2) Cu4' 0.049(3) 0.045(3) 0.050(3) -0.001(3) 0.009(3) -0.0001(19) Cu5' 0.037(4) 0.026(5) 0.031(5) -0.018(3) 0.007(4) -0.002(3) Cu6' 0.040(2) 0.046(3) 0.044(2) 0.006(2) 0.0087(17) -0.0014(17) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Br1 Cu8 2.4293(10) . ? Br1 Cu5' 2.465(11) . ? Br1 Cu6 2.474(5) . ? Br1 Cu5 2.5439(16) . ? Br1 Cu6' 2.619(12) . ? Br2 Cu7 2.4479(10) . ? Br2 Cu1' 2.472(6) . ? Br2 Cu2 2.5701(11) . ? Br2 Cu1 2.5711(16) . ? Br3 Cu4' 2.452(6) . ? Br3 Cu9 2.4690(11) . ? Br3 Cu3 2.6166(11) . ? Br3 Cu4 2.6262(17) . ? C1 C2 1.443(11) . ? C1 O1 1.457(8) . ? C1 C3 1.492(11) . ? C4 C6' 1.43(4) . ? C4 O2 1.454(9) . ? C4 C5 1.467(13) . ? C4 C6 1.58(3) . ? C7 C9 1.480(12) . ? C7 O3 1.484(8) . ? C7 C8 1.492(12) . ? C10 O4 1.469(8) . ? C10 C11 1.516(10) . ? C10 C12' 1.525(11) . ? C10 C12 1.535(10) . ? C10 C11' 1.536(11) . ? C13 O5 1.467(8) . ? C13 C14 1.478(14) . ? C13 C15 1.487(14) . ? C16 O6 1.451(9) . ? C16 C18 1.477(13) . ? C16 C17 1.485(13) . ? C19 O7 1.449(8) . ? C19 C20 1.452(11) . ? C19 C21 1.478(12) . ? C22 O8 1.468(8) . ? C22 C23 1.484(14) . ? C22 C24 1.485(13) . ? C25 C27 1.463(12) . ? C25 O9 1.472(8) . ? C25 C26 1.513(11) . ? C28 O10 1.465(8) . ? C28 C30 1.472(12) . ? C28 C29 1.479(12) . ? C31 O11 1.462(7) . ? C31 C33 1.471(11) . ? C31 C32 1.502(10) . ? C34 O12 1.437(9) . ? C34 C35 1.462(15) . ? C34 C36 1.504(16) . ? Cu1 Cu1' 0.711(4) . ? Cu1 S7 2.379(2) . ? Cu1 S4 2.399(2) . ? Cu1 S13 2.440(2) . ? Cu1 Cu11 2.7566(17) . ? Cu1 Cu8 2.8736(17) . ? Cu1 Cu7 2.9964(18) . ? Cu1 Cu2 3.0126(17) . ? Cu2 S5 2.3477(17) . ? Cu2 S2 2.3946(17) . ? Cu2 S13 2.4031(16) . ? Cu2 Cu10 2.7706(12) . ? Cu2 Cu7 2.8740(12) . ? Cu2 Cu8 2.9314(13) . ? Cu7 S6 2.2843(17) . ? Cu7 S8 2.2899(16) . ? Cu7 Cu4 2.8636(18) . ? Cu7 Cu3 2.8897(13) . ? Cu3 S11 2.3766(16) . ? Cu3 S8 2.3806(16) . ? Cu3 S13 2.4211(16) . ? Cu3 Cu11 2.7130(11) . ? Cu3 Cu9 2.8584(13) . ? Cu3 Cu4 3.0136(17) . ? Cu4 Cu4' 0.728(5) . ? Cu4 S6 2.371(2) . ? Cu4 S9 2.397(2) . ? Cu4 S13 2.410(2) . ? Cu4 Cu10 2.7923(18) . ? Cu4 Cu9 2.8024(17) . ? Cu9 S12 2.3051(16) . ? Cu9 S10 2.3130(17) . ? Cu9 S13 2.6546(16) . ? Cu9 Cu6' 2.845(11) . ? Cu9 Cu5 2.8471(17) . ? Cu5 Cu5' 0.641(7) . ? Cu5 S3 2.337(2) . ? Cu5 S12 2.346(2) . ? Cu5 S13 2.528(2) . ? Cu5 Cu8 2.8930(17) . ? Cu5 Cu11 2.9298(17) . ? Cu5 Cu6' 2.994(11) . ? Cu6 S1 2.267(5) . ? Cu6 S10 2.294(5) . ? Cu6 S13 2.808(3) . ? Cu6 Cu10 2.943(5) . ? Cu6 Cu8 3.023(5) . ? Cu8 S4 2.2840(16) . ? Cu8 S2 2.3045(16) . ? Cu8 S13 2.7691(16) . ? Cu8 Cu6' 2.839(11) . ? Cu11 S11 2.2546(16) . ? Cu11 S3 2.2600(16) . ? Cu11 S7 2.2607(15) . ? Cu11 Cu1' 3.013(6) . ? Cu10 S1 2.2490(17) . ? Cu10 S5 2.2588(16) . ? Cu10 S9 2.2629(17) . ? Cu10 Cu6' 2.769(12) . ? O1 P1 1.572(4) . ? O2 P1 1.576(5) . ? O3 P2 1.573(4) . ? O4 P2 1.563(5) . ? O5 P3 1.570(4) . ? O6 P3 1.569(4) . ? O7 P4 1.576(4) . ? O8 P4 1.563(4) . ? O9 P5 1.562(4) . ? O10 P5 1.577(4) . ? O11 P6 1.575(4) . ? O12 P6 1.564(4) . ? P1 S2 2.004(2) . ? P1 S1 2.018(2) . ? P2 S4 2.007(2) . ? P2 S3 2.010(2) . ? P3 S6 2.004(2) . ? P3 S5 2.022(2) . ? P4 S8 2.0051(19) . ? P4 S7 2.023(2) . ? P5 S10 2.006(2) . ? P5 S9 2.018(2) . ? P6 S12 2.0112(19) . ? P6 S11 2.021(2) . ? S1 Cu6' 2.426(11) . ? S3 Cu5' 2.107(12) . ? S4 Cu1' 2.227(6) . ? S6 Cu4' 2.243(6) . ? S7 Cu1' 2.117(6) . ? S9 Cu4' 2.135(6) . ? S10 Cu6' 2.423(11) . ? S12 Cu5' 2.270(12) . ? S13 Cu6' 2.362(6) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag Cu8 Br1 Cu5' 81.6(2) . . ? Cu8 Br1 Cu6 76.12(10) . . ? Cu5' Br1 Cu6 90.9(2) . . ? Cu8 Br1 Cu5 71.10(4) . . ? Cu5' Br1 Cu5 14.60(16) . . ? Cu6 Br1 Cu5 78.68(10) . . ? Cu8 Br1 Cu6' 68.3(2) . . ? Cu5' Br1 Cu6' 84.0(3) . . ? Cu6 Br1 Cu6' 9.82(19) . . ? Cu5 Br1 Cu6' 70.87(19) . . ? Cu7 Br2 Cu1' 85.66(13) . . ? Cu7 Br2 Cu2 69.84(3) . . ? Cu1' Br2 Cu2 85.33(12) . . ? Cu7 Br2 Cu1 73.27(4) . . ? Cu1' Br2 Cu1 16.04(10) . . ? Cu2 Br2 Cu1 71.74(4) . . ? Cu4' Br3 Cu9 78.30(14) . . ? Cu4' Br3 Cu3 84.33(14) . . ? Cu9 Br3 Cu3 68.33(3) . . ? Cu4' Br3 Cu4 16.02(11) . . ? Cu9 Br3 Cu4 66.65(4) . . ? Cu3 Br3 Cu4 70.17(4) . . ? C2 C1 O1 110.6(7) . . ? C2 C1 C3 111.7(7) . . ? O1 C1 C3 108.3(7) . . ? C6' C4 O2 116.7(18) . . ? C6' C4 C5 118(2) . . ? O2 C4 C5 108.8(8) . . ? C6' C4 C6 29(2) . . ? O2 C4 C6 101.0(12) . . ? C5 C4 C6 104.6(17) . . ? C9 C7 O3 105.6(7) . . ? C9 C7 C8 113.3(9) . . ? O3 C7 C8 109.9(7) . . ? O4 C10 C11 106.4(9) . . ? O4 C10 C12' 103.1(11) . . ? C11 C10 C12' 74.4(14) . . ? O4 C10 C12 109.8(9) . . ? C11 C10 C12 109.9(11) . . ? C12' C10 C12 40.2(12) . . ? O4 C10 C11' 105.5(12) . . ? C11 C10 C11' 33.1(13) . . ? C12' C10 C11' 106.8(16) . . ? C12 C10 C11' 136.0(12) . . ? O5 C13 C14 107.4(7) . . ? O5 C13 C15 108.4(8) . . ? C14 C13 C15 113.8(9) . . ? O6 C16 C18 108.7(8) . . ? O6 C16 C17 106.4(7) . . ? C18 C16 C17 114.8(9) . . ? O7 C19 C20 108.7(7) . . ? O7 C19 C21 107.5(7) . . ? C20 C19 C21 111.3(8) . . ? O8 C22 C23 108.0(8) . . ? O8 C22 C24 107.4(7) . . ? C23 C22 C24 111.3(8) . . ? C27 C25 O9 110.1(7) . . ? C27 C25 C26 113.0(7) . . ? O9 C25 C26 104.0(6) . . ? O10 C28 C30 108.6(7) . . ? O10 C28 C29 108.3(7) . . ? C30 C28 C29 111.9(8) . . ? O11 C31 C33 112.1(6) . . ? O11 C31 C32 105.8(6) . . ? C33 C31 C32 113.9(6) . . ? O12 C34 C35 107.7(9) . . ? O12 C34 C36 107.0(9) . . ? C35 C34 C36 112.7(9) . . ? Cu1' Cu1 S7 60.2(5) . . ? Cu1' Cu1 S4 67.6(5) . . ? S7 Cu1 S4 104.58(7) . . ? Cu1' Cu1 S13 170.4(6) . . ? S7 Cu1 S13 128.06(8) . . ? S4 Cu1 S13 111.36(7) . . ? Cu1' Cu1 Br2 74.1(5) . . ? S7 Cu1 Br2 105.57(7) . . ? S4 Cu1 Br2 107.89(7) . . ? S13 Cu1 Br2 97.75(6) . . ? Cu1' Cu1 Cu11 104.4(5) . . ? S7 Cu1 Cu11 51.60(5) . . ? S4 Cu1 Cu11 100.56(6) . . ? S13 Cu1 Cu11 85.23(6) . . ? Br2 Cu1 Cu11 147.86(7) . . ? Cu1' Cu1 Cu8 114.2(6) . . ? S7 Cu1 Cu8 146.57(7) . . ? S4 Cu1 Cu8 50.36(5) . . ? S13 Cu1 Cu8 62.19(5) . . ? Br2 Cu1 Cu8 103.72(5) . . ? Cu11 Cu1 Cu8 105.86(6) . . ? Cu1' Cu1 Cu7 113.6(5) . . ? S7 Cu1 Cu7 97.67(6) . . ? S4 Cu1 Cu7 153.65(7) . . ? S13 Cu1 Cu7 62.78(5) . . ? Br2 Cu1 Cu7 51.48(3) . . ? Cu11 Cu1 Cu7 104.30(5) . . ? Cu8 Cu1 Cu7 113.17(5) . . ? Cu1' Cu1 Cu2 119.4(5) . . ? S7 Cu1 Cu2 153.65(7) . . ? S4 Cu1 Cu2 98.37(6) . . ? S13 Cu1 Cu2 50.99(4) . . ? Br2 Cu1 Cu2 54.11(4) . . ? Cu11 Cu1 Cu2 136.14(7) . . ? Cu8 Cu1 Cu2 59.68(4) . . ? Cu7 Cu1 Cu2 57.15(3) . . ? S5 Cu2 S2 106.14(6) . . ? S5 Cu2 S13 127.88(6) . . ? S2 Cu2 S13 110.71(6) . . ? S5 Cu2 Br2 106.37(5) . . ? S2 Cu2 Br2 104.47(5) . . ? S13 Cu2 Br2 98.72(4) . . ? S5 Cu2 Cu10 51.57(4) . . ? S2 Cu2 Cu10 99.98(5) . . ? S13 Cu2 Cu10 86.25(5) . . ? Br2 Cu2 Cu10 151.32(4) . . ? S5 Cu2 Cu7 95.16(5) . . ? S2 Cu2 Cu7 153.37(5) . . ? S13 Cu2 Cu7 65.21(4) . . ? Br2 Cu2 Cu7 53.08(3) . . ? Cu10 Cu2 Cu7 105.81(4) . . ? S5 Cu2 Cu8 147.14(5) . . ? S2 Cu2 Cu8 50.04(4) . . ? S13 Cu2 Cu8 61.61(4) . . ? Br2 Cu2 Cu8 102.16(4) . . ? Cu10 Cu2 Cu8 104.98(4) . . ? Cu7 Cu2 Cu8 115.14(4) . . ? S5 Cu2 Cu1 155.01(6) . . ? S2 Cu2 Cu1 94.91(5) . . ? S13 Cu2 Cu1 52.08(5) . . ? Br2 Cu2 Cu1 54.14(4) . . ? Cu10 Cu2 Cu1 138.32(5) . . ? Cu7 Cu2 Cu1 61.14(4) . . ? Cu8 Cu2 Cu1 57.80(4) . . ? S6 Cu7 S8 106.47(6) . . ? S6 Cu7 Br2 128.43(5) . . ? S8 Cu7 Br2 119.87(5) . . ? S6 Cu7 Cu4 53.43(5) . . ? S8 Cu7 Cu4 104.97(6) . . ? Br2 Cu7 Cu4 125.48(5) . . ? S6 Cu7 Cu2 94.46(5) . . ? S8 Cu7 Cu2 147.99(6) . . ? Br2 Cu7 Cu2 57.08(3) . . ? Cu4 Cu7 Cu2 68.41(5) . . ? S6 Cu7 Cu3 102.98(5) . . ? S8 Cu7 Cu3 53.21(4) . . ? Br2 Cu7 Cu3 121.92(4) . . ? Cu4 Cu7 Cu3 63.17(4) . . ? Cu2 Cu7 Cu3 99.14(4) . . ? S6 Cu7 Cu1 150.22(6) . . ? S8 Cu7 Cu1 89.82(5) . . ? Br2 Cu7 Cu1 55.26(4) . . ? Cu4 Cu7 Cu1 98.78(6) . . ? Cu2 Cu7 Cu1 61.71(4) . . ? Cu3 Cu7 Cu1 66.74(4) . . ? S11 Cu3 S8 107.19(6) . . ? S11 Cu3 S13 125.85(6) . . ? S8 Cu3 S13 113.37(6) . . ? S11 Cu3 Br3 102.51(5) . . ? S8 Cu3 Br3 107.47(5) . . ? S13 Cu3 Br3 98.00(4) . . ? S11 Cu3 Cu11 52.08(4) . . ? S8 Cu3 Cu11 99.26(5) . . ? S13 Cu3 Cu11 86.55(5) . . ? Br3 Cu3 Cu11 148.22(4) . . ? S11 Cu3 Cu9 95.25(5) . . ? S8 Cu3 Cu9 153.95(5) . . ? S13 Cu3 Cu9 59.69(4) . . ? Br3 Cu3 Cu9 53.39(3) . . ? Cu11 Cu3 Cu9 105.01(4) . . ? S11 Cu3 Cu7 151.26(5) . . ? S8 Cu3 Cu7 50.38(4) . . ? S13 Cu3 Cu7 64.75(4) . . ? Br3 Cu3 Cu7 101.88(3) . . ? Cu11 Cu3 Cu7 108.40(4) . . ? Cu9 Cu3 Cu7 111.50(4) . . ? S11 Cu3 Cu4 150.71(6) . . ? S8 Cu3 Cu4 98.34(5) . . ? S13 Cu3 Cu4 51.24(5) . . ? Br3 Cu3 Cu4 55.06(4) . . ? Cu11 Cu3 Cu4 137.79(5) . . ? Cu9 Cu3 Cu4 56.94(4) . . ? Cu7 Cu3 Cu4 57.99(4) . . ? Cu4' Cu4 S6 71.1(5) . . ? Cu4' Cu4 S9 60.5(5) . . ? S6 Cu4 S9 104.32(7) . . ? Cu4' Cu4 S13 166.3(6) . . ? S6 Cu4 S13 115.00(8) . . ? S9 Cu4 S13 125.92(8) . . ? Cu4' Cu4 Br3 68.3(5) . . ? S6 Cu4 Br3 104.57(7) . . ? S9 Cu4 Br3 106.63(7) . . ? S13 Cu4 Br3 98.02(6) . . ? Cu4' Cu4 Cu10 105.8(5) . . ? S6 Cu4 Cu10 99.98(6) . . ? S9 Cu4 Cu10 51.01(5) . . ? S13 Cu4 Cu10 85.64(6) . . ? Br3 Cu4 Cu10 150.72(6) . . ? Cu4' Cu4 Cu9 108.1(6) . . ? S6 Cu4 Cu9 153.70(8) . . ? S9 Cu4 Cu9 97.25(6) . . ? S13 Cu4 Cu9 60.68(5) . . ? Br3 Cu4 Cu9 53.99(4) . . ? Cu10 Cu4 Cu9 105.29(6) . . ? Cu4' Cu4 Cu7 117.1(6) . . ? S6 Cu4 Cu7 50.68(5) . . ? S9 Cu4 Cu7 146.17(7) . . ? S13 Cu4 Cu7 65.31(5) . . ? Br3 Cu4 Cu7 102.33(5) . . ? Cu10 Cu4 Cu7 105.52(6) . . ? Cu9 Cu4 Cu7 113.97(6) . . ? Cu4' Cu4 Cu3 116.8(5) . . ? S6 Cu4 Cu3 97.35(6) . . ? S9 Cu4 Cu3 154.90(7) . . ? S13 Cu4 Cu3 51.57(4) . . ? Br3 Cu4 Cu3 54.76(4) . . ? Cu10 Cu4 Cu3 137.17(7) . . ? Cu9 Cu4 Cu3 58.74(4) . . ? Cu7 Cu4 Cu3 58.84(4) . . ? S12 Cu9 S10 99.77(6) . . ? S12 Cu9 Br3 122.51(5) . . ? S10 Cu9 Br3 125.09(5) . . ? S12 Cu9 S13 106.15(6) . . ? S10 Cu9 S13 104.83(6) . . ? Br3 Cu9 S13 95.82(4) . . ? S12 Cu9 Cu4 156.66(6) . . ? S10 Cu9 Cu4 95.31(5) . . ? Br3 Cu9 Cu4 59.36(4) . . ? S13 Cu9 Cu4 52.33(5) . . ? S12 Cu9 Cu6' 104.1(2) . . ? S10 Cu9 Cu6' 54.88(17) . . ? Br3 Cu9 Cu6' 129.8(2) . . ? S13 Cu9 Cu6' 50.72(15) . . ? Cu4 Cu9 Cu6' 70.5(2) . . ? S12 Cu9 Cu5 52.92(5) . . ? S10 Cu9 Cu5 100.55(6) . . ? Br3 Cu9 Cu5 131.98(5) . . ? S13 Cu9 Cu5 54.58(5) . . ? Cu4 Cu9 Cu5 106.88(6) . . ? Cu6' Cu9 Cu5 63.5(2) . . ? S12 Cu9 Cu3 96.04(5) . . ? S10 Cu9 Cu3 155.14(6) . . ? Br3 Cu9 Cu3 58.29(3) . . ? S13 Cu9 Cu3 51.94(4) . . ? Cu4 Cu9 Cu3 64.32(4) . . ? Cu6' Cu9 Cu3 102.66(16) . . ? Cu5 Cu9 Cu3 74.11(5) . . ? Cu5' Cu5 S3 61.4(11) . . ? Cu5' Cu5 S12 75.3(12) . . ? S3 Cu5 S12 106.78(7) . . ? Cu5' Cu5 S13 173.1(11) . . ? S3 Cu5 S13 120.93(8) . . ? S12 Cu5 S13 109.02(7) . . ? Cu5' Cu5 Br1 75.7(11) . . ? S3 Cu5 Br1 110.32(7) . . ? S12 Cu5 Br1 112.17(7) . . ? S13 Cu5 Br1 97.50(6) . . ? Cu5' Cu5 Cu9 123.9(12) . . ? S3 Cu5 Cu9 143.17(7) . . ? S12 Cu5 Cu9 51.61(5) . . ? S13 Cu5 Cu9 58.83(5) . . ? Br1 Cu5 Cu9 105.94(5) . . ? Cu5' Cu5 Cu8 112.8(12) . . ? S3 Cu5 Cu8 96.69(6) . . ? S12 Cu5 Cu8 155.94(7) . . ? S13 Cu5 Cu8 60.99(5) . . ? Br1 Cu5 Cu8 52.60(3) . . ? Cu9 Cu5 Cu8 110.51(5) . . ? Cu5' Cu5 Cu11 104.9(11) . . ? S3 Cu5 Cu11 49.26(5) . . ? S12 Cu5 Cu11 98.35(6) . . ? S13 Cu5 Cu11 80.11(6) . . ? Br1 Cu5 Cu11 148.18(6) . . ? Cu9 Cu5 Cu11 99.86(5) . . ? Cu8 Cu5 Cu11 101.00(5) . . ? Cu5' Cu5 Cu6' 125.0(11) . . ? S3 Cu5 Cu6' 154.3(2) . . ? S12 Cu5 Cu6' 98.8(2) . . ? S13 Cu5 Cu6' 49.77(15) . . ? Br1 Cu5 Cu6' 55.74(18) . . ? Cu9 Cu5 Cu6' 58.2(2) . . ? Cu8 Cu5 Cu6' 57.6(2) . . ? Cu11 Cu5 Cu6' 129.88(16) . . ? S1 Cu6 S10 115.8(2) . . ? S1 Cu6 Br1 115.3(2) . . ? S10 Cu6 Br1 114.0(2) . . ? S1 Cu6 S13 115.55(18) . . ? S10 Cu6 S13 100.71(16) . . ? Br1 Cu6 S13 92.21(14) . . ? S1 Cu6 Cu10 49.07(11) . . ? S10 Cu6 Cu10 97.85(18) . . ? Br1 Cu6 Cu10 147.7(2) . . ? S13 Cu6 Cu10 76.12(10) . . ? S1 Cu6 Cu8 96.43(17) . . ? S10 Cu6 Cu8 147.1(2) . . ? Br1 Cu6 Cu8 51.27(9) . . ? S13 Cu6 Cu8 56.56(8) . . ? Cu10 Cu6 Cu8 98.62(13) . . ? S4 Cu8 S2 102.06(6) . . ? S4 Cu8 Br1 124.95(5) . . ? S2 Cu8 Br1 124.55(5) . . ? S4 Cu8 S13 104.12(6) . . ? S2 Cu8 S13 101.75(6) . . ? Br1 Cu8 S13 94.14(4) . . ? S4 Cu8 Cu6' 152.51(17) . . ? S2 Cu8 Cu6' 93.1(2) . . ? Br1 Cu8 Cu6' 59.0(2) . . ? S13 Cu8 Cu6' 49.79(14) . . ? S4 Cu8 Cu1 53.98(5) . . ? S2 Cu8 Cu1 100.77(6) . . ? Br1 Cu8 Cu1 129.17(5) . . ? S13 Cu8 Cu1 51.19(5) . . ? Cu6' Cu8 Cu1 100.97(15) . . ? S4 Cu8 Cu5 95.58(5) . . ? S2 Cu8 Cu5 152.49(6) . . ? Br1 Cu8 Cu5 56.30(4) . . ? S13 Cu8 Cu5 52.99(4) . . ? Cu6' Cu8 Cu5 63.0(2) . . ? Cu1 Cu8 Cu5 72.89(5) . . ? S4 Cu8 Cu2 103.50(5) . . ? S2 Cu8 Cu2 52.80(5) . . ? Br1 Cu8 Cu2 126.79(4) . . ? S13 Cu8 Cu2 49.77(4) . . ? Cu6' Cu8 Cu2 67.9(2) . . ? Cu1 Cu8 Cu2 62.52(4) . . ? Cu5 Cu8 Cu2 102.73(5) . . ? S4 Cu8 Cu6 158.70(10) . . ? S2 Cu8 Cu6 93.32(11) . . ? Br1 Cu8 Cu6 52.61(9) . . ? S13 Cu8 Cu6 57.79(8) . . ? Cu6' Cu8 Cu6 8.2(2) . . ? Cu1 Cu8 Cu6 108.97(9) . . ? Cu5 Cu8 Cu6 65.02(10) . . ? Cu2 Cu8 Cu6 74.21(9) . . ? S11 Cu11 S3 116.41(6) . . ? S11 Cu11 S7 123.82(6) . . ? S3 Cu11 S7 119.03(6) . . ? S11 Cu11 Cu3 56.26(4) . . ? S3 Cu11 Cu3 126.40(5) . . ? S7 Cu11 Cu3 95.65(5) . . ? S11 Cu11 Cu1 128.85(6) . . ? S3 Cu11 Cu1 93.70(5) . . ? S7 Cu11 Cu1 55.54(5) . . ? Cu3 Cu11 Cu1 72.62(4) . . ? S11 Cu11 Cu5 92.77(5) . . ? S3 Cu11 Cu5 51.57(5) . . ? S7 Cu11 Cu5 128.88(6) . . ? Cu3 Cu11 Cu5 74.96(4) . . ? Cu1 Cu11 Cu5 74.02(5) . . ? S11 Cu11 Cu1' 138.21(11) . . ? S3 Cu11 Cu1' 94.08(12) . . ? S7 Cu11 Cu1' 44.57(11) . . ? Cu3 Cu11 Cu1' 83.00(10) . . ? Cu1 Cu11 Cu1' 13.21(9) . . ? Cu5 Cu11 Cu1' 84.31(11) . . ? S1 Cu10 S5 119.39(6) . . ? S1 Cu10 S9 120.50(6) . . ? S5 Cu10 S9 119.58(6) . . ? S1 Cu10 Cu6' 56.68(17) . . ? S5 Cu10 Cu6' 125.5(2) . . ? S9 Cu10 Cu6' 94.0(2) . . ? S1 Cu10 Cu2 94.43(5) . . ? S5 Cu10 Cu2 54.51(5) . . ? S9 Cu10 Cu2 126.16(5) . . ? Cu6' Cu10 Cu2 71.17(18) . . ? S1 Cu10 Cu4 128.31(6) . . ? S5 Cu10 Cu4 92.39(5) . . ? S9 Cu10 Cu4 55.43(5) . . ? Cu6' Cu10 Cu4 71.79(18) . . ? Cu2 Cu10 Cu4 70.88(4) . . ? S1 Cu10 Cu6 49.60(9) . . ? S5 Cu10 Cu6 131.51(10) . . ? S9 Cu10 Cu6 94.24(11) . . ? Cu6' Cu10 Cu6 8.53(17) . . ? Cu2 Cu10 Cu6 77.87(8) . . ? Cu4 Cu10 Cu6 78.72(9) . . ? C1 O1 P1 129.3(4) . . ? C4 O2 P1 123.8(5) . . ? C7 O3 P2 124.6(4) . . ? C10 O4 P2 123.6(4) . . ? C13 O5 P3 121.6(4) . . ? C16 O6 P3 125.9(4) . . ? C19 O7 P4 124.2(4) . . ? C22 O8 P4 125.4(4) . . ? C25 O9 P5 126.5(4) . . ? C28 O10 P5 122.6(4) . . ? C31 O11 P6 125.0(4) . . ? C34 O12 P6 124.6(5) . . ? O1 P1 O2 104.8(3) . . ? O1 P1 S2 110.15(18) . . ? O2 P1 S2 111.6(2) . . ? O1 P1 S1 108.1(2) . . ? O2 P1 S1 102.46(19) . . ? S2 P1 S1 118.70(9) . . ? O4 P2 O3 109.0(3) . . ? O4 P2 S4 112.5(2) . . ? O3 P2 S4 103.56(17) . . ? O4 P2 S3 101.81(18) . . ? O3 P2 S3 110.64(19) . . ? S4 P2 S3 119.24(9) . . ? O6 P3 O5 102.4(2) . . ? O6 P3 S6 111.21(19) . . ? O5 P3 S6 105.90(18) . . ? O6 P3 S5 108.44(18) . . ? O5 P3 S5 110.5(2) . . ? S6 P3 S5 117.31(9) . . ? O8 P4 O7 101.8(2) . . ? O8 P4 S8 107.06(16) . . ? O7 P4 S8 110.01(17) . . ? O8 P4 S7 110.20(16) . . ? O7 P4 S7 109.26(17) . . ? S8 P4 S7 117.40(9) . . ? O9 P5 O10 102.5(2) . . ? O9 P5 S10 111.10(18) . . ? O10 P5 S10 109.60(18) . . ? O9 P5 S9 105.59(17) . . ? O10 P5 S9 109.20(19) . . ? S10 P5 S9 117.76(9) . . ? O12 P6 O11 101.8(2) . . ? O12 P6 S12 110.23(19) . . ? O11 P6 S12 111.04(17) . . ? O12 P6 S11 108.82(19) . . ? O11 P6 S11 106.24(16) . . ? S12 P6 S11 117.50(8) . . ? P1 S1 Cu10 106.46(8) . . ? P1 S1 Cu6 107.65(14) . . ? Cu10 S1 Cu6 81.34(12) . . ? P1 S1 Cu6' 104.1(3) . . ? Cu10 S1 Cu6' 72.5(2) . . ? Cu6 S1 Cu6' 10.5(3) . . ? P1 S2 Cu8 104.61(8) . . ? P1 S2 Cu2 103.17(8) . . ? Cu8 S2 Cu2 77.16(6) . . ? P2 S3 Cu5' 112.5(3) . . ? P2 S3 Cu11 103.44(7) . . ? Cu5' S3 Cu11 92.5(3) . . ? P2 S3 Cu5 107.75(8) . . ? Cu5' S3 Cu5 15.5(2) . . ? Cu11 S3 Cu5 79.17(6) . . ? P2 S4 Cu1' 102.92(16) . . ? P2 S4 Cu8 105.73(8) . . ? Cu1' S4 Cu8 91.49(14) . . ? P2 S4 Cu1 100.59(8) . . ? Cu1' S4 Cu1 17.15(11) . . ? Cu8 S4 Cu1 75.66(6) . . ? P3 S5 Cu10 102.93(8) . . ? P3 S5 Cu2 109.44(8) . . ? Cu10 S5 Cu2 73.92(5) . . ? P3 S6 Cu4' 104.53(17) . . ? P3 S6 Cu7 106.03(8) . . ? Cu4' S6 Cu7 92.12(15) . . ? P3 S6 Cu4 101.56(8) . . ? Cu4' S6 Cu4 17.88(13) . . ? Cu7 S6 Cu4 75.89(6) . . ? P4 S7 Cu1' 107.84(17) . . ? P4 S7 Cu11 108.53(7) . . ? Cu1' S7 Cu11 86.90(15) . . ? P4 S7 Cu1 102.83(8) . . ? Cu1' S7 Cu1 16.93(12) . . ? Cu11 S7 Cu1 72.86(6) . . ? P4 S8 Cu7 103.67(7) . . ? P4 S8 Cu3 106.57(7) . . ? Cu7 S8 Cu3 76.42(5) . . ? P5 S9 Cu4' 114.00(18) . . ? P5 S9 Cu10 102.71(8) . . ? Cu4' S9 Cu10 88.56(17) . . ? P5 S9 Cu4 108.29(8) . . ? Cu4' S9 Cu4 17.27(14) . . ? Cu10 S9 Cu4 73.56(6) . . ? P5 S10 Cu6 102.54(15) . . ? P5 S10 Cu9 108.02(8) . . ? Cu6 S10 Cu9 83.40(10) . . ? P5 S10 Cu6' 100.7(3) . . ? Cu6 S10 Cu6' 10.7(2) . . ? Cu9 S10 Cu6' 73.80(18) . . ? P6 S11 Cu11 101.96(7) . . ? P6 S11 Cu3 111.17(7) . . ? Cu11 S11 Cu3 71.66(5) . . ? P6 S12 Cu5' 101.3(3) . . ? P6 S12 Cu9 109.14(8) . . ? Cu5' S12 Cu9 90.5(2) . . ? P6 S12 Cu5 101.14(8) . . ? Cu5' S12 Cu5 15.86(17) . . ? Cu9 S12 Cu5 75.47(6) . . ? Cu6' S13 Cu2 85.1(3) . . ? Cu6' S13 Cu4 86.2(3) . . ? Cu2 S13 Cu4 84.16(6) . . ? Cu6' S13 Cu3 137.2(3) . . ? Cu2 S13 Cu3 130.85(6) . . ? Cu4 S13 Cu3 77.19(6) . . ? Cu6' S13 Cu1 133.2(3) . . ? Cu2 S13 Cu1 76.94(6) . . ? Cu4 S13 Cu1 133.13(7) . . ? Cu3 S13 Cu1 83.57(6) . . ? Cu6' S13 Cu5 75.4(3) . . ? Cu2 S13 Cu5 134.60(7) . . ? Cu4 S13 Cu5 133.53(7) . . ? Cu3 S13 Cu5 87.97(5) . . ? Cu1 S13 Cu5 87.18(6) . . ? Cu6' S13 Cu9 68.8(3) . . ? Cu2 S13 Cu9 141.60(6) . . ? Cu4 S13 Cu9 66.99(5) . . ? Cu3 S13 Cu9 68.37(4) . . ? Cu1 S13 Cu9 141.39(6) . . ? Cu5 S13 Cu9 66.59(5) . . ? Cu6' S13 Cu8 66.7(3) . . ? Cu2 S13 Cu8 68.63(4) . . ? Cu4 S13 Cu8 142.35(7) . . ? Cu3 S13 Cu8 140.40(6) . . ? Cu1 S13 Cu8 66.62(5) . . ? Cu5 S13 Cu8 66.02(5) . . ? Cu9 S13 Cu8 120.82(5) . . ? Cu6' S13 Cu6 2.4(4) . . ? Cu2 S13 Cu6 86.83(11) . . ? Cu4 S13 Cu6 88.10(12) . . ? Cu3 S13 Cu6 136.51(12) . . ? Cu1 S13 Cu6 132.26(12) . . ? Cu5 S13 Cu6 72.99(12) . . ? Cu9 S13 Cu6 68.19(11) . . ? Cu8 S13 Cu6 65.65(11) . . ? Cu1 Cu1' S7 102.8(6) . . ? Cu1 Cu1' S4 95.3(6) . . ? S7 Cu1' S4 120.9(3) . . ? Cu1 Cu1' Br2 89.9(5) . . ? S7 Cu1' Br2 118.2(2) . . ? S4 Cu1' Br2 117.5(2) . . ? Cu1 Cu1' Cu11 62.4(5) . . ? S7 Cu1' Cu11 48.53(12) . . ? S4 Cu1' Cu11 97.47(19) . . ? Br2 Cu1' Cu11 137.7(2) . . ? Cu4 Cu4' S9 102.2(6) . . ? Cu4 Cu4' S6 91.1(6) . . ? S9 Cu4' S6 118.6(3) . . ? Cu4 Cu4' Br3 95.7(6) . . ? S9 Cu4' Br3 122.8(3) . . ? S6 Cu4' Br3 114.8(2) . . ? Cu5 Cu5' S3 103.1(12) . . ? Cu5 Cu5' S12 88.8(12) . . ? S3 Cu5' S12 118.3(5) . . ? Cu5 Cu5' Br1 89.7(11) . . ? S3 Cu5' Br1 122.3(5) . . ? S12 Cu5' Br1 118.0(5) . . ? S13 Cu6' S10 110.9(4) . . ? S13 Cu6' S1 128.0(5) . . ? S10 Cu6' S1 105.6(3) . . ? S13 Cu6' Br1 99.8(4) . . ? S10 Cu6' Br1 105.0(4) . . ? S1 Cu6' Br1 105.1(3) . . ? S13 Cu6' Cu10 87.1(3) . . ? S10 Cu6' Cu10 99.6(4) . . ? S1 Cu6' Cu10 50.8(2) . . ? Br1 Cu6' Cu10 150.0(5) . . ? S13 Cu6' Cu8 63.6(2) . . ? S10 Cu6' Cu8 151.7(5) . . ? S1 Cu6' Cu8 97.8(4) . . ? Br1 Cu6' Cu8 52.7(2) . . ? Cu10 Cu6' Cu8 107.5(4) . . ? S13 Cu6' Cu9 60.5(2) . . ? S10 Cu6' Cu9 51.3(2) . . ? S1 Cu6' Cu9 147.0(5) . . ? Br1 Cu6' Cu9 104.0(4) . . ? Cu10 Cu6' Cu9 104.8(3) . . ? Cu8 Cu6' Cu9 112.1(3) . . ? S13 Cu6' Cu5 54.8(2) . . ? S10 Cu6' Cu5 94.1(4) . . ? S1 Cu6' Cu5 154.7(5) . . ? Br1 Cu6' Cu5 53.4(2) . . ? Cu10 Cu6' Cu5 141.9(2) . . ? Cu8 Cu6' Cu5 59.4(2) . . ? Cu9 Cu6' Cu5 58.3(2) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.026 _refine_diff_density_min -1.675 _refine_diff_density_rms 0.115 _database_code_depnum_ccdc_archive 'CCDC 943814' ####################################################################### # # 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_4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H84 Cu11 I3 O12 P6 S13' _chemical_formula_weight 2391.27 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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' I I -0.4742 1.8119 '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 37.600(4) _cell_length_b 17.9079(17) _cell_length_c 27.460(3) _cell_angle_alpha 90.00 _cell_angle_beta 104.703(2) _cell_angle_gamma 90.00 _cell_volume 17884(3) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 9743 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 28.33 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.39 _exptl_crystal_size_min 0.38 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.776 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 9376 _exptl_absorpt_coefficient_mu 4.044 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2815 _exptl_absorpt_correction_T_max 0.3087 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(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 APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 100435 _diffrn_reflns_av_R_equivalents 0.0299 _diffrn_reflns_av_sigmaI/netI 0.0239 _diffrn_reflns_limit_h_min -50 _diffrn_reflns_limit_h_max 50 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -36 _diffrn_reflns_limit_l_max 36 _diffrn_reflns_theta_min 1.41 _diffrn_reflns_theta_max 28.33 _reflns_number_total 22251 _reflns_number_gt 19444 _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, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _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. Restraints on bond lengths and atomic displacement paremeters were applied by using DFIX, DELU and EADP command in SHELX program. C2, C3, C5, C6, C16, C17, C18 were split and refined anisotropically. They were finally fixed to 70/30, 70/30, 50/50, 50/50, 60/40, 60/40, and 60/40, respectively. Attempts to solve the solvent molecules into split positions result in large ADPs of them, indicating the loss of solvent when mounting the crystal onto glass fiber. Since the solvent molecules cannot be modelled perfectly, the SQUEEZE procedure was eventually applied to deal with the solvent molecules. The used restraints and constraints are: DFIX 1.54 0.01 C1 C3 DELU C16 C17 C16 C18 DELU C16' C17' C16' C18' DELU C1 C2 DELU C1 C2' DELU C1 C3 DELU C4 C6 EADP C5 C6 EADP C5' C6' ; _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^)+(0.0321P)^2^+151.3250P] 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 22251 _refine_ls_number_parameters 809 _refine_ls_number_restraints 11 _refine_ls_R_factor_all 0.0403 _refine_ls_R_factor_gt 0.0351 _refine_ls_wR_factor_ref 0.0867 _refine_ls_wR_factor_gt 0.0843 _refine_ls_goodness_of_fit_ref 1.035 _refine_ls_restrained_S_all 1.036 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.47644(15) 0.8756(4) 0.3638(3) 0.0640(16) Uani 1 1 d DU . . H1 H 0.4917 0.8507 0.3947 0.077 Uiso 1 1 calc R A 1 C2 C 0.4787(2) 0.8335(5) 0.3219(3) 0.0520(19) Uani 0.70 1 d PU B 1 H2A H 0.5038 0.8362 0.3177 0.078 Uiso 0.70 1 calc PR B 1 H2B H 0.4614 0.8534 0.2918 0.078 Uiso 0.70 1 calc PR B 1 H2C H 0.4725 0.7814 0.3269 0.078 Uiso 0.70 1 calc PR B 1 C3 C 0.4888(3) 0.9588(5) 0.3639(4) 0.070(3) Uani 0.70 1 d PDU B 1 H3A H 0.4852 0.9839 0.3940 0.105 Uiso 0.70 1 calc PR B 1 H3B H 0.4742 0.9839 0.3338 0.105 Uiso 0.70 1 calc PR B 1 H3C H 0.5149 0.9608 0.3640 0.105 Uiso 0.70 1 calc PR B 1 C2' C 0.4711(6) 0.8832(13) 0.3007(8) 0.061(5) Uani 0.30 1 d PU B 2 H2'1 H 0.4678 0.9359 0.2909 0.092 Uiso 0.30 1 calc PR B 2 H2'2 H 0.4495 0.8546 0.2830 0.092 Uiso 0.30 1 calc PR B 2 H2'3 H 0.4930 0.8636 0.2919 0.092 Uiso 0.30 1 calc PR B 2 C3' C 0.5108(6) 0.8736(16) 0.3902(10) 0.083(8) Uani 0.30 1 d P B 2 H3'1 H 0.5268 0.8635 0.3677 0.124 Uiso 0.30 1 calc PR B 2 H3'2 H 0.5139 0.8339 0.4155 0.124 Uiso 0.30 1 calc PR B 2 H3'3 H 0.5174 0.9217 0.4070 0.124 Uiso 0.30 1 calc PR B 2 C4 C 0.45356(17) 0.8796(4) 0.51198(19) 0.0573(15) Uani 1 1 d U . . H4 H 0.4356 0.8393 0.5142 0.069 Uiso 1 1 calc R C 1 C5 C 0.4368(6) 0.9631(10) 0.5259(7) 0.077(4) Uani 0.50 1 d P D 1 H5A H 0.4338 0.9617 0.5602 0.116 Uiso 0.50 1 calc PR D 1 H5B H 0.4130 0.9727 0.5022 0.116 Uiso 0.50 1 calc PR D 1 H5C H 0.4541 1.0029 0.5232 0.116 Uiso 0.50 1 calc PR D 1 C6 C 0.4874(5) 0.8616(15) 0.5425(7) 0.077(4) Uani 0.50 1 d PU D 1 H6A H 0.5066 0.8752 0.5258 0.116 Uiso 0.50 1 calc PR D 1 H6B H 0.4885 0.8078 0.5493 0.116 Uiso 0.50 1 calc PR D 1 H6C H 0.4913 0.8890 0.5744 0.116 Uiso 0.50 1 calc PR D 1 C5' C 0.4386(4) 0.9342(9) 0.5367(5) 0.054(3) Uani 0.50 1 d P D 2 H5'1 H 0.4350 0.9138 0.5682 0.080 Uiso 0.50 1 calc PR D 2 H5'2 H 0.4149 0.9503 0.5152 0.080 Uiso 0.50 1 calc PR D 2 H5'3 H 0.4553 0.9770 0.5441 0.080 Uiso 0.50 1 calc PR D 2 C6' C 0.4979(3) 0.8679(13) 0.5337(6) 0.054(3) Uani 0.50 1 d P D 2 H6'1 H 0.5106 0.9149 0.5310 0.080 Uiso 0.50 1 calc PR D 2 H6'2 H 0.5064 0.8292 0.5140 0.080 Uiso 0.50 1 calc PR D 2 H6'3 H 0.5033 0.8526 0.5691 0.080 Uiso 0.50 1 calc PR D 2 C7 C 0.46638(9) 0.3965(2) 0.54245(14) 0.0218(7) Uani 1 1 d . . . H7 H 0.4835 0.4393 0.5431 0.026 Uiso 1 1 calc R . . C8 C 0.46727(11) 0.3460(3) 0.49942(15) 0.0325(9) Uani 1 1 d . . . H8A H 0.4493 0.3057 0.4975 0.049 Uiso 1 1 calc R . . H8B H 0.4919 0.3245 0.5046 0.049 Uiso 1 1 calc R . . H8C H 0.4612 0.3745 0.4680 0.049 Uiso 1 1 calc R . . C9 C 0.47542(12) 0.3587(3) 0.59295(16) 0.0379(10) Uani 1 1 d . . . H9A H 0.4730 0.3946 0.6188 0.057 Uiso 1 1 calc R . . H9B H 0.5007 0.3400 0.6007 0.057 Uiso 1 1 calc R . . H9C H 0.4585 0.3169 0.5923 0.057 Uiso 1 1 calc R . . C10 C 0.44980(11) 0.6071(2) 0.61018(14) 0.0270(8) Uani 1 1 d . . . H10 H 0.4368 0.6428 0.5836 0.032 Uiso 1 1 calc R . . C11 C 0.43464(16) 0.6133(3) 0.6554(2) 0.0531(14) Uani 1 1 d . . . H11A H 0.4085 0.6002 0.6460 0.080 Uiso 1 1 calc R . . H11B H 0.4376 0.6646 0.6681 0.080 Uiso 1 1 calc R . . H11C H 0.4479 0.5791 0.6816 0.080 Uiso 1 1 calc R . . C12 C 0.49066(14) 0.6199(3) 0.6216(2) 0.0534(14) Uani 1 1 d . . . H12A H 0.5034 0.5824 0.6458 0.080 Uiso 1 1 calc R . . H12B H 0.4964 0.6699 0.6360 0.080 Uiso 1 1 calc R . . H12C H 0.4988 0.6159 0.5905 0.080 Uiso 1 1 calc R . . C13 C 0.29386(13) 0.9843(2) 0.33745(16) 0.0346(9) Uani 1 1 d . . . H13 H 0.3104 0.9588 0.3193 0.041 Uiso 1 1 calc R . . C14 C 0.31552(15) 1.0443(3) 0.37170(18) 0.0416(11) Uani 1 1 d . . . H14A H 0.2993 1.0703 0.3890 0.062 Uiso 1 1 calc R . . H14B H 0.3254 1.0801 0.3515 0.062 Uiso 1 1 calc R . . H14C H 0.3358 1.0211 0.3967 0.062 Uiso 1 1 calc R . . C15 C 0.26114(16) 1.0141(3) 0.3001(2) 0.0536(14) Uani 1 1 d . . . H15A H 0.2467 0.9725 0.2819 0.080 Uiso 1 1 calc R . . H15B H 0.2692 1.0466 0.2762 0.080 Uiso 1 1 calc R . . H15C H 0.2459 1.0428 0.3176 0.080 Uiso 1 1 calc R . . C16 C 0.2003(3) 0.8764(5) 0.3643(4) 0.0251(19) Uani 0.60 1 d PU E 1 H16 H 0.2141 0.9001 0.3966 0.030 Uiso 0.60 1 calc PR E 1 C17 C 0.1749(2) 0.9320(4) 0.3319(3) 0.0333(15) Uani 0.60 1 d PU E 1 H17A H 0.1640 0.9099 0.2989 0.050 Uiso 0.60 1 calc PR E 1 H17B H 0.1888 0.9768 0.3278 0.050 Uiso 0.60 1 calc PR E 1 H17C H 0.1554 0.9456 0.3480 0.050 Uiso 0.60 1 calc PR E 1 C18 C 0.1815(2) 0.8074(5) 0.3745(4) 0.0415(19) Uani 0.60 1 d PU E 1 H18A H 0.1688 0.7840 0.3425 0.062 Uiso 0.60 1 calc PR E 1 H18B H 0.1636 0.8200 0.3936 0.062 Uiso 0.60 1 calc PR E 1 H18C H 0.1997 0.7725 0.3941 0.062 Uiso 0.60 1 calc PR E 1 C16' C 0.1965(4) 0.8454(9) 0.3635(6) 0.023(3) Uani 0.40 1 d PU E 2 H16' H 0.2070 0.8255 0.3983 0.028 Uiso 0.40 1 calc PR E 2 C17' C 0.1863(4) 0.9249(8) 0.3664(7) 0.048(3) Uani 0.40 1 d PU E 2 H17D H 0.1763 0.9444 0.3323 0.072 Uiso 0.40 1 calc PR E 2 H17E H 0.2082 0.9536 0.3832 0.072 Uiso 0.40 1 calc PR E 2 H17F H 0.1677 0.9292 0.3856 0.072 Uiso 0.40 1 calc PR E 2 C18' C 0.1652(3) 0.7971(7) 0.3367(5) 0.043(3) Uani 0.40 1 d PU E 2 H18D H 0.1472 0.7932 0.3569 0.065 Uiso 0.40 1 calc PR E 2 H18E H 0.1744 0.7473 0.3318 0.065 Uiso 0.40 1 calc PR E 2 H18F H 0.1535 0.8193 0.3040 0.065 Uiso 0.40 1 calc PR E 2 C19 C 0.27391(13) 0.3950(2) 0.53267(15) 0.0330(9) Uani 1 1 d . . . H19 H 0.2898 0.3742 0.5118 0.040 Uiso 1 1 calc R . . C20 C 0.29323(16) 0.3863(3) 0.58745(19) 0.0505(13) Uani 1 1 d . . . H20A H 0.3163 0.4145 0.5949 0.076 Uiso 1 1 calc R . . H20B H 0.2985 0.3334 0.5950 0.076 Uiso 1 1 calc R . . H20C H 0.2775 0.4054 0.6081 0.076 Uiso 1 1 calc R . . C21 C 0.23685(15) 0.3574(3) 0.51817(19) 0.0441(11) Uani 1 1 d . . . H21A H 0.2205 0.3805 0.5366 0.066 Uiso 1 1 calc R . . H21B H 0.2397 0.3042 0.5266 0.066 Uiso 1 1 calc R . . H21C H 0.2262 0.3630 0.4819 0.066 Uiso 1 1 calc R . . C22 C 0.19155(10) 0.5639(2) 0.45737(15) 0.0247(7) Uani 1 1 d . . . H22 H 0.2027 0.6143 0.4666 0.030 Uiso 1 1 calc R . . C23 C 0.16149(11) 0.5696(3) 0.40968(17) 0.0351(9) Uani 1 1 d . . . H23A H 0.1716 0.5897 0.3828 0.053 Uiso 1 1 calc R . . H23B H 0.1422 0.6029 0.4151 0.053 Uiso 1 1 calc R . . H23C H 0.1511 0.5200 0.4001 0.053 Uiso 1 1 calc R . . C24 C 0.17901(12) 0.5323(3) 0.50090(16) 0.0332(9) Uani 1 1 d . . . H24A H 0.1682 0.4828 0.4919 0.050 Uiso 1 1 calc R . . H24B H 0.1605 0.5654 0.5089 0.050 Uiso 1 1 calc R . . H24C H 0.2001 0.5280 0.5303 0.050 Uiso 1 1 calc R . . C25 C 0.33103(13) 0.8524(2) 0.18220(18) 0.0361(10) Uani 1 1 d . . . H25 H 0.3575 0.8640 0.1977 0.043 Uiso 1 1 calc R . . C26 C 0.30671(18) 0.9121(3) 0.1923(2) 0.0590(16) Uani 1 1 d . . . H26A H 0.2810 0.8975 0.1787 0.088 Uiso 1 1 calc R . . H26B H 0.3115 0.9585 0.1761 0.088 Uiso 1 1 calc R . . H26C H 0.3115 0.9200 0.2287 0.088 Uiso 1 1 calc R . . C27 C 0.3234(2) 0.8422(3) 0.1250(2) 0.0625(17) Uani 1 1 d . . . H27A H 0.3388 0.8017 0.1176 0.094 Uiso 1 1 calc R . . H27B H 0.3291 0.8886 0.1097 0.094 Uiso 1 1 calc R . . H27C H 0.2974 0.8297 0.1111 0.094 Uiso 1 1 calc R . . C28 C 0.40458(11) 0.6624(2) 0.19962(15) 0.0297(8) Uani 1 1 d . . . H28 H 0.4117 0.6469 0.2358 0.036 Uiso 1 1 calc R . . C29 C 0.43210(16) 0.7175(3) 0.1900(2) 0.0592(17) Uani 1 1 d . . . H29A H 0.4264 0.7292 0.1539 0.089 Uiso 1 1 calc R . . H29B H 0.4568 0.6959 0.2006 0.089 Uiso 1 1 calc R . . H29C H 0.4311 0.7633 0.2091 0.089 Uiso 1 1 calc R . . C30 C 0.40040(14) 0.5944(3) 0.1664(2) 0.0438(11) Uani 1 1 d . . . H30A H 0.3811 0.5621 0.1731 0.066 Uiso 1 1 calc R . . H30B H 0.4237 0.5670 0.1736 0.066 Uiso 1 1 calc R . . H30C H 0.3936 0.6099 0.1310 0.066 Uiso 1 1 calc R . . C31 C 0.29190(11) 0.2933(2) 0.32807(15) 0.0271(8) Uani 1 1 d . . . H31 H 0.2759 0.3353 0.3114 0.033 Uiso 1 1 calc R . . C32 C 0.27313(12) 0.2521(2) 0.36234(17) 0.0339(9) Uani 1 1 d . . . H32A H 0.2886 0.2104 0.3783 0.051 Uiso 1 1 calc R . . H32B H 0.2494 0.2329 0.3427 0.051 Uiso 1 1 calc R . . H32C H 0.2691 0.2862 0.3883 0.051 Uiso 1 1 calc R . . C33 C 0.30111(15) 0.2446(3) 0.28862(16) 0.0401(11) Uani 1 1 d . . . H33A H 0.3123 0.2750 0.2668 0.060 Uiso 1 1 calc R . . H33B H 0.2786 0.2212 0.2684 0.060 Uiso 1 1 calc R . . H33C H 0.3185 0.2057 0.3049 0.060 Uiso 1 1 calc R . . C34 C 0.40977(11) 0.3329(2) 0.32538(16) 0.0316(9) Uani 1 1 d . . . H34 H 0.4252 0.3677 0.3505 0.038 Uiso 1 1 calc R . . C35 C 0.41078(17) 0.2561(3) 0.3482(2) 0.0537(14) Uani 1 1 d . . . H35A H 0.4020 0.2588 0.3788 0.081 Uiso 1 1 calc R . . H35B H 0.4361 0.2373 0.3566 0.081 Uiso 1 1 calc R . . H35C H 0.3949 0.2224 0.3240 0.081 Uiso 1 1 calc R . . C36 C 0.42254(13) 0.3342(3) 0.27751(18) 0.0431(11) Uani 1 1 d . . . H36A H 0.4066 0.3020 0.2523 0.065 Uiso 1 1 calc R . . H36B H 0.4479 0.3159 0.2845 0.065 Uiso 1 1 calc R . . H36C H 0.4214 0.3854 0.2647 0.065 Uiso 1 1 calc R . . Cu1 Cu 0.299619(14) 0.54409(3) 0.368782(18) 0.02710(10) Uani 1 1 d . B . Cu2 Cu 0.300881(14) 0.67844(3) 0.317795(18) 0.02598(10) Uani 1 1 d . B . Cu7 Cu 0.269847(13) 0.67578(3) 0.411046(17) 0.02528(10) Uani 1 1 d . B . Cu9 Cu 0.355604(13) 0.56129(3) 0.300548(18) 0.02579(10) Uani 1 1 d . B . Cu5 Cu 0.392890(13) 0.54927(3) 0.409596(17) 0.02533(10) Uani 1 1 d . B . Cu6 Cu 0.395122(13) 0.68105(3) 0.358487(17) 0.02555(10) Uani 1 1 d . B . Cu8 Cu 0.407560(14) 0.67954(3) 0.470873(19) 0.02889(10) Uani 1 1 d . B . Cu3 Cu 0.340367(13) 0.61918(3) 0.475876(18) 0.02619(10) Uani 1 1 d . B . Cu4 Cu 0.343799(13) 0.76042(3) 0.430172(18) 0.02785(10) Uani 1 1 d . B . Cu10 Cu 0.343649(12) 0.46855(3) 0.455146(16) 0.02023(9) Uani 1 1 d . . . Cu11 Cu 0.348633(12) 0.80732(2) 0.336039(16) 0.02087(9) Uani 1 1 d . B . I1 I 0.236728(6) 0.618002(13) 0.327176(8) 0.02139(5) Uani 1 1 d . . . I3 I 0.425949(7) 0.555889(13) 0.329637(9) 0.02324(5) Uani 1 1 d . . . I2 I 0.374266(7) 0.744337(14) 0.530936(9) 0.02736(6) Uani 1 1 d . . . O1 O 0.43867(8) 0.88091(16) 0.36856(11) 0.0320(6) Uani 1 1 d . B . O2 O 0.45172(9) 0.89434(17) 0.45942(12) 0.0362(7) Uani 1 1 d . B . O3 O 0.42806(6) 0.42473(14) 0.53335(9) 0.0211(5) Uani 1 1 d . . . O4 O 0.44333(7) 0.53017(15) 0.59155(9) 0.0225(5) Uani 1 1 d . . . O5 O 0.28275(8) 0.93089(15) 0.37103(10) 0.0262(5) Uani 1 1 d . . . O6 O 0.22646(7) 0.84840(17) 0.33512(10) 0.0293(6) Uani 1 1 d . . . O7 O 0.26972(8) 0.47618(15) 0.52393(10) 0.0253(5) Uani 1 1 d . . . O8 O 0.21936(7) 0.51312(15) 0.44558(10) 0.0225(5) Uani 1 1 d . . . O9 O 0.31985(8) 0.78195(14) 0.20179(10) 0.0252(5) Uani 1 1 d . . . O10 O 0.36886(8) 0.70019(15) 0.18832(10) 0.0262(5) Uani 1 1 d . . . O11 O 0.32599(7) 0.32385(13) 0.36123(9) 0.0208(5) Uani 1 1 d . . . O12 O 0.37192(7) 0.36041(15) 0.31081(9) 0.0245(5) Uani 1 1 d . . . P1 P 0.42694(3) 0.84715(6) 0.41505(4) 0.02510(19) Uani 1 1 d . . . P2 P 0.42000(2) 0.51031(5) 0.53646(3) 0.01744(16) Uani 1 1 d . . . P3 P 0.26900(2) 0.84799(5) 0.35809(3) 0.02039(17) Uani 1 1 d . E . P4 P 0.26185(2) 0.51533(5) 0.47068(3) 0.01801(16) Uani 1 1 d . E . P5 P 0.34850(3) 0.72191(5) 0.22998(3) 0.01952(17) Uani 1 1 d . E . P6 P 0.34900(2) 0.39062(5) 0.34747(3) 0.01698(16) Uani 1 1 d . E . S1 S 0.37354(3) 0.87058(5) 0.40750(3) 0.02367(18) Uani 1 1 d . B . S2 S 0.44128(2) 0.73910(5) 0.42313(3) 0.02369(18) Uani 1 1 d . B . S3 S 0.36597(2) 0.51918(5) 0.53209(3) 0.02040(16) Uani 1 1 d . . . S4 S 0.43952(2) 0.56812(5) 0.48578(3) 0.01838(15) Uani 1 1 d . . . S5 S 0.28781(2) 0.80643(5) 0.30126(3) 0.02069(16) Uani 1 1 d . . . S6 S 0.28302(2) 0.79830(5) 0.42596(3) 0.02093(16) Uani 1 1 d . . . S7 S 0.28300(2) 0.45476(5) 0.42268(3) 0.01841(15) Uani 1 1 d . . . S8 S 0.27966(2) 0.62040(5) 0.48756(3) 0.01966(16) Uani 1 1 d . . . S9 S 0.38587(2) 0.76596(5) 0.28931(3) 0.02011(16) Uani 1 1 d . . . S10 S 0.31739(2) 0.63772(5) 0.24400(3) 0.02071(16) Uani 1 1 d . . . S11 S 0.38308(2) 0.41970(5) 0.41390(3) 0.01755(15) Uani 1 1 d . . . S12 S 0.31549(2) 0.46770(5) 0.30704(3) 0.01900(16) Uani 1 1 d . . . S13 S 0.34600(2) 0.64009(5) 0.39371(3) 0.01623(15) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 C1 0.032(3) 0.095(5) 0.066(4) 0.022(3) 0.015(3) -0.009(3) C2 0.033(4) 0.062(5) 0.063(5) -0.011(4) 0.014(3) -0.008(3) C3 0.071(6) 0.070(6) 0.077(6) -0.024(5) 0.032(5) -0.051(5) C2' 0.063(13) 0.061(13) 0.066(9) -0.011(11) 0.028(10) -0.013(11) C3' 0.059(13) 0.092(19) 0.087(17) 0.020(14) 0.000(12) -0.031(13) C4 0.064(3) 0.073(4) 0.030(2) -0.020(2) 0.004(2) -0.024(3) C5 0.081(8) 0.094(9) 0.047(7) -0.029(7) -0.003(5) 0.025(8) C6 0.081(8) 0.094(9) 0.047(7) -0.029(7) -0.003(5) 0.025(8) C5' 0.030(4) 0.085(7) 0.039(5) -0.015(5) -0.003(3) 0.016(4) C6' 0.030(4) 0.085(7) 0.039(5) -0.015(5) -0.003(3) 0.016(4) C7 0.0178(15) 0.0231(17) 0.0258(17) 0.0032(14) 0.0080(13) 0.0073(13) C8 0.0266(19) 0.041(2) 0.029(2) -0.0034(17) 0.0069(16) 0.0130(17) C9 0.035(2) 0.051(3) 0.029(2) 0.0126(19) 0.0117(17) 0.025(2) C10 0.0317(19) 0.0250(19) 0.0212(17) -0.0041(14) 0.0007(15) -0.0004(15) C11 0.063(3) 0.055(3) 0.050(3) -0.026(3) 0.030(3) -0.009(3) C12 0.041(3) 0.060(3) 0.058(3) -0.015(3) 0.011(2) -0.016(2) C13 0.052(3) 0.024(2) 0.032(2) 0.0047(16) 0.0185(19) 0.0141(18) C14 0.061(3) 0.025(2) 0.039(2) 0.0021(18) 0.014(2) 0.004(2) C15 0.061(3) 0.054(3) 0.039(3) 0.021(2) 0.002(2) 0.011(3) C16 0.025(4) 0.029(4) 0.022(3) 0.000(4) 0.006(3) 0.005(4) C17 0.029(3) 0.036(4) 0.038(4) 0.009(3) 0.015(3) 0.011(3) C18 0.032(4) 0.042(4) 0.057(5) 0.017(4) 0.024(4) 0.005(3) C16' 0.017(5) 0.033(7) 0.020(5) -0.004(6) 0.006(4) 0.007(6) C17' 0.043(7) 0.036(6) 0.075(10) -0.016(7) 0.033(7) 0.001(5) C18' 0.030(5) 0.047(7) 0.057(8) -0.013(6) 0.018(6) -0.013(5) C19 0.047(2) 0.030(2) 0.027(2) 0.0109(16) 0.0188(18) 0.0140(18) C20 0.059(3) 0.054(3) 0.036(3) 0.022(2) 0.008(2) 0.009(3) C21 0.067(3) 0.028(2) 0.039(2) 0.0003(19) 0.016(2) -0.004(2) C22 0.0222(17) 0.0200(17) 0.034(2) -0.0072(15) 0.0110(15) 0.0017(14) C23 0.0254(19) 0.040(2) 0.040(2) -0.0038(19) 0.0082(17) 0.0129(17) C24 0.030(2) 0.037(2) 0.037(2) -0.0073(18) 0.0154(17) 0.0023(17) C25 0.042(2) 0.022(2) 0.047(3) 0.0124(18) 0.017(2) 0.0046(17) C26 0.080(4) 0.034(3) 0.076(4) 0.020(3) 0.044(3) 0.017(3) C27 0.105(5) 0.043(3) 0.043(3) 0.016(2) 0.025(3) 0.002(3) C28 0.0283(19) 0.036(2) 0.0274(19) -0.0020(16) 0.0128(16) 0.0013(16) C29 0.057(3) 0.067(4) 0.066(4) -0.041(3) 0.041(3) -0.034(3) C30 0.050(3) 0.029(2) 0.061(3) -0.009(2) 0.030(2) 0.000(2) C31 0.0287(19) 0.0170(17) 0.0290(19) 0.0022(14) -0.0052(15) -0.0035(14) C32 0.030(2) 0.026(2) 0.043(2) -0.0004(17) 0.0039(18) -0.0035(16) C33 0.059(3) 0.032(2) 0.026(2) -0.0084(17) 0.004(2) -0.016(2) C34 0.029(2) 0.035(2) 0.033(2) -0.0044(17) 0.0126(16) 0.0095(17) C35 0.063(3) 0.042(3) 0.059(3) 0.010(2) 0.021(3) 0.027(3) C36 0.040(2) 0.057(3) 0.039(2) -0.013(2) 0.021(2) 0.005(2) Cu1 0.0333(2) 0.0261(2) 0.0246(2) 0.00610(18) 0.01222(19) 0.00811(19) Cu2 0.0322(2) 0.0210(2) 0.0268(2) 0.00145(18) 0.01128(19) 0.00101(18) Cu7 0.0298(2) 0.0227(2) 0.0210(2) 0.00066(17) 0.00225(18) 0.00101(18) Cu9 0.0280(2) 0.0195(2) 0.0298(2) 0.00537(18) 0.00714(19) -0.00056(17) Cu5 0.0319(2) 0.0215(2) 0.0209(2) -0.00018(17) 0.00350(18) -0.00298(18) Cu6 0.0317(2) 0.0197(2) 0.0235(2) -0.00025(17) 0.00377(18) 0.00038(18) Cu8 0.0332(2) 0.0232(2) 0.0312(2) 0.00069(19) 0.0099(2) 0.00785(19) Cu3 0.0218(2) 0.0266(2) 0.0299(2) 0.00274(19) 0.00611(18) 0.00372(18) Cu4 0.0260(2) 0.0297(2) 0.0265(2) 0.00403(19) 0.00419(18) 0.00789(19) Cu10 0.01899(19) 0.0239(2) 0.01806(19) -0.00053(16) 0.00510(15) 0.00344(16) Cu11 0.0221(2) 0.0202(2) 0.0202(2) -0.00257(16) 0.00510(16) 0.00241(16) I1 0.02087(10) 0.02255(11) 0.01899(10) 0.00199(8) 0.00182(8) 0.00009(8) I3 0.02723(11) 0.01998(11) 0.02588(11) -0.00009(9) 0.01296(9) 0.00221(9) I2 0.03282(13) 0.02548(12) 0.01983(11) -0.00537(9) -0.00059(9) 0.00987(10) O1 0.0344(15) 0.0249(14) 0.0359(15) -0.0038(12) 0.0072(12) -0.0065(12) O2 0.0376(16) 0.0308(16) 0.0345(16) -0.0137(13) -0.0013(13) -0.0020(13) O3 0.0158(11) 0.0222(12) 0.0252(12) 0.0025(10) 0.0050(9) 0.0046(9) O4 0.0240(12) 0.0248(13) 0.0168(11) 0.0002(10) 0.0020(9) 0.0039(10) O5 0.0337(14) 0.0207(13) 0.0239(13) 0.0025(10) 0.0069(11) 0.0087(11) O6 0.0229(13) 0.0455(17) 0.0191(12) -0.0001(12) 0.0043(10) 0.0130(12) O7 0.0329(14) 0.0239(13) 0.0208(12) 0.0042(10) 0.0101(11) 0.0047(11) O8 0.0169(11) 0.0252(13) 0.0262(13) -0.0050(10) 0.0069(10) 0.0028(10) O9 0.0325(14) 0.0189(12) 0.0232(13) 0.0049(10) 0.0055(11) 0.0029(10) O10 0.0344(14) 0.0260(14) 0.0209(12) -0.0014(10) 0.0122(11) -0.0002(11) O11 0.0262(12) 0.0152(11) 0.0193(12) 0.0033(9) 0.0024(10) -0.0022(9) O12 0.0283(13) 0.0272(14) 0.0188(12) -0.0041(10) 0.0075(10) 0.0052(11) P1 0.0271(5) 0.0202(4) 0.0257(5) -0.0062(4) 0.0024(4) -0.0015(4) P2 0.0168(4) 0.0201(4) 0.0151(4) 0.0016(3) 0.0034(3) 0.0039(3) P3 0.0207(4) 0.0222(4) 0.0173(4) 0.0003(3) 0.0032(3) 0.0075(3) P4 0.0182(4) 0.0205(4) 0.0163(4) 0.0014(3) 0.0062(3) 0.0026(3) P5 0.0271(4) 0.0158(4) 0.0163(4) 0.0002(3) 0.0066(3) 0.0002(3) P6 0.0210(4) 0.0152(4) 0.0151(4) -0.0008(3) 0.0052(3) 0.0012(3) S1 0.0277(4) 0.0179(4) 0.0232(4) -0.0043(3) 0.0025(3) 0.0055(3) S2 0.0211(4) 0.0230(4) 0.0254(4) -0.0031(3) 0.0030(3) 0.0042(3) S3 0.0170(4) 0.0287(4) 0.0158(4) 0.0015(3) 0.0048(3) 0.0046(3) S4 0.0174(4) 0.0199(4) 0.0179(4) 0.0018(3) 0.0046(3) 0.0022(3) S5 0.0224(4) 0.0220(4) 0.0173(4) 0.0003(3) 0.0045(3) 0.0049(3) S6 0.0240(4) 0.0211(4) 0.0166(4) -0.0006(3) 0.0030(3) 0.0064(3) S7 0.0194(4) 0.0193(4) 0.0172(4) -0.0007(3) 0.0059(3) 0.0020(3) S8 0.0192(4) 0.0224(4) 0.0175(4) -0.0018(3) 0.0049(3) 0.0018(3) S9 0.0238(4) 0.0175(4) 0.0201(4) -0.0028(3) 0.0076(3) -0.0024(3) S10 0.0278(4) 0.0165(4) 0.0170(4) 0.0002(3) 0.0041(3) -0.0033(3) S11 0.0178(4) 0.0179(4) 0.0168(4) -0.0006(3) 0.0039(3) 0.0023(3) S12 0.0235(4) 0.0164(4) 0.0160(4) 0.0018(3) 0.0032(3) 0.0003(3) S13 0.0156(3) 0.0179(4) 0.0147(3) -0.0043(3) 0.0030(3) 0.0017(3) _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 C1 C3' 1.31(2) . ? C1 C2 1.397(10) . ? C1 O1 1.461(6) . ? C1 C3 1.561(7) . ? C1 C2' 1.70(2) . ? C4 C6 1.37(2) . ? C4 C5' 1.387(16) . ? C4 O2 1.451(6) . ? C4 C6' 1.636(14) . ? C4 C5 1.701(18) . ? C7 O3 1.487(4) . ? C7 C8 1.495(5) . ? C7 C9 1.502(5) . ? C10 O4 1.468(5) . ? C10 C11 1.496(6) . ? C10 C12 1.506(6) . ? C13 O5 1.462(5) . ? C13 C15 1.486(7) . ? C13 C14 1.520(7) . ? C16 C18 1.485(11) . ? C16 C17 1.505(12) . ? C16 O6 1.505(11) . ? C16' C17' 1.482(18) . ? C16' C18' 1.493(17) . ? C16' O6 1.526(14) . ? C19 O7 1.475(5) . ? C19 C20 1.503(6) . ? C19 C21 1.507(7) . ? C22 O8 1.482(4) . ? C22 C23 1.501(6) . ? C22 C24 1.503(6) . ? C25 O9 1.475(5) . ? C25 C26 1.478(7) . ? C25 C27 1.535(7) . ? C28 O10 1.465(5) . ? C28 C29 1.501(6) . ? C28 C30 1.504(6) . ? C31 O11 1.476(4) . ? C31 C33 1.498(6) . ? C31 C32 1.505(6) . ? C34 O12 1.463(5) . ? C34 C35 1.507(7) . ? C34 C36 1.510(6) . ? Cu1 S7 2.3683(10) . ? Cu1 S12 2.3697(10) . ? Cu1 S13 2.4207(10) . ? Cu1 I1 2.6978(6) . ? Cu1 Cu2 2.7902(7) . ? Cu1 Cu10 2.8638(7) . ? Cu1 Cu7 2.9701(7) . ? Cu2 S5 2.3639(10) . ? Cu2 S10 2.3796(10) . ? Cu2 S13 2.4289(9) . ? Cu2 I1 2.7151(6) . ? Cu2 Cu11 2.8887(7) . ? Cu2 Cu9 3.0583(7) . ? Cu7 S6 2.2635(10) . ? Cu7 S8 2.2673(10) . ? Cu7 I1 2.5435(5) . ? Cu7 Cu3 2.9717(7) . ? Cu9 S10 2.2838(10) . ? Cu9 S12 2.2919(10) . ? Cu9 I3 2.5634(6) . ? Cu9 Cu6 2.8527(7) . ? Cu9 Cu5 2.9745(7) . ? Cu5 S13 2.3568(9) . ? Cu5 S11 2.3571(10) . ? Cu5 S4 2.3880(10) . ? Cu5 Cu6 2.7579(7) . ? Cu5 I3 2.7867(6) . ? Cu5 Cu8 2.8473(7) . ? Cu5 Cu10 2.8735(7) . ? Cu6 S2 2.3833(10) . ? Cu6 S9 2.3888(10) . ? Cu6 S13 2.4067(10) . ? Cu6 I3 2.7314(6) . ? Cu6 Cu11 2.8287(7) . ? Cu6 Cu8 3.0018(7) . ? Cu8 S2 2.3038(11) . ? Cu8 S4 2.3115(10) . ? Cu8 I2 2.5849(6) . ? Cu8 Cu4 2.7811(7) . ? Cu8 Cu3 2.7833(7) . ? Cu8 S13 2.8030(10) . ? Cu3 S13 2.3491(9) . ? Cu3 S8 2.3846(10) . ? Cu3 S3 2.4003(10) . ? Cu3 Cu10 2.7660(7) . ? Cu3 I2 2.8206(6) . ? Cu3 Cu4 2.8410(7) . ? Cu4 S6 2.3583(10) . ? Cu4 S13 2.3862(10) . ? Cu4 S1 2.4256(11) . ? Cu4 I2 2.7281(6) . ? Cu4 Cu11 2.7674(7) . ? Cu10 S7 2.2414(10) . ? Cu10 S3 2.2561(10) . ? Cu10 S11 2.2581(9) . ? Cu11 S5 2.2438(10) . ? Cu11 S9 2.2513(9) . ? Cu11 S1 2.2536(10) . ? O1 P1 1.573(3) . ? O2 P1 1.578(3) . ? O3 P2 1.569(3) . ? O4 P2 1.584(3) . ? O5 P3 1.582(3) . ? O6 P3 1.563(3) . ? O7 P4 1.580(3) . ? O8 P4 1.572(3) . ? O9 P5 1.579(3) . ? O10 P5 1.578(3) . ? O11 P6 1.577(3) . ? O12 P6 1.577(3) . ? P1 S2 2.0057(14) . ? P1 S1 2.0098(14) . ? P2 S3 2.0108(12) . ? P2 S4 2.0164(12) . ? P3 S6 2.0112(12) . ? P3 S5 2.0122(12) . ? P4 S8 2.0115(13) . ? P4 S7 2.0195(12) . ? P5 S10 2.0046(13) . ? P5 S9 2.0221(13) . ? P6 S12 2.0038(12) . ? P6 S11 2.0136(12) . ? 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 C3' C1 C2 100.5(15) . . ? C3' C1 O1 142.8(14) . . ? C2 C1 O1 111.9(5) . . ? C3' C1 C3 76.9(13) . . ? C2 C1 C3 115.8(6) . . ? O1 C1 C3 103.5(5) . . ? C3' C1 C2' 114.2(15) . . ? C2 C1 C2' 38.6(8) . . ? O1 C1 C2' 102.7(8) . . ? C3 C1 C2' 83.3(9) . . ? C6 C4 C5' 107.2(9) . . ? C6 C4 O2 116.9(9) . . ? C5' C4 O2 115.8(8) . . ? C6 C4 C6' 17.5(13) . . ? C5' C4 C6' 114.5(8) . . ? O2 C4 C6' 100.0(7) . . ? C6 C4 C5 114.0(10) . . ? C5' C4 C5 18.8(12) . . ? O2 C4 C5 97.8(8) . . ? C6' C4 C5 115.6(11) . . ? O3 C7 C8 106.7(3) . . ? O3 C7 C9 106.9(3) . . ? C8 C7 C9 114.3(3) . . ? O4 C10 C11 107.1(4) . . ? O4 C10 C12 106.6(4) . . ? C11 C10 C12 113.5(4) . . ? O5 C13 C15 110.5(4) . . ? O5 C13 C14 105.4(3) . . ? C15 C13 C14 113.2(4) . . ? C18 C16 C17 113.7(8) . . ? C18 C16 O6 103.3(7) . . ? C17 C16 O6 107.9(7) . . ? C17' C16' C18' 113.6(12) . . ? C17' C16' O6 103.1(11) . . ? C18' C16' O6 111.1(10) . . ? O7 C19 C20 105.6(4) . . ? O7 C19 C21 110.1(3) . . ? C20 C19 C21 113.4(4) . . ? O8 C22 C23 105.5(3) . . ? O8 C22 C24 108.9(3) . . ? C23 C22 C24 113.6(3) . . ? O9 C25 C26 107.7(4) . . ? O9 C25 C27 105.9(4) . . ? C26 C25 C27 108.3(5) . . ? O10 C28 C29 107.2(4) . . ? O10 C28 C30 107.2(3) . . ? C29 C28 C30 113.3(4) . . ? O11 C31 C33 109.8(3) . . ? O11 C31 C32 105.5(3) . . ? C33 C31 C32 113.5(3) . . ? O12 C34 C35 109.9(4) . . ? O12 C34 C36 105.0(3) . . ? C35 C34 C36 113.3(4) . . ? S7 Cu1 S12 102.21(3) . . ? S7 Cu1 S13 126.04(4) . . ? S12 Cu1 S13 108.55(3) . . ? S7 Cu1 I1 104.72(3) . . ? S12 Cu1 I1 109.46(3) . . ? S13 Cu1 I1 105.21(3) . . ? S7 Cu1 Cu2 159.52(3) . . ? S12 Cu1 Cu2 95.70(3) . . ? S13 Cu1 Cu2 55.02(2) . . ? I1 Cu1 Cu2 59.277(15) . . ? S7 Cu1 Cu10 49.63(2) . . ? S12 Cu1 Cu10 97.02(3) . . ? S13 Cu1 Cu10 82.98(3) . . ? I1 Cu1 Cu10 147.44(2) . . ? Cu2 Cu1 Cu10 137.98(2) . . ? S7 Cu1 Cu7 96.13(3) . . ? S12 Cu1 Cu7 157.86(3) . . ? S13 Cu1 Cu7 68.99(2) . . ? I1 Cu1 Cu7 53.064(14) . . ? Cu2 Cu1 Cu7 64.371(18) . . ? Cu10 Cu1 Cu7 104.33(2) . . ? S5 Cu2 S10 102.71(3) . . ? S5 Cu2 S13 120.32(3) . . ? S10 Cu2 S13 111.58(3) . . ? S5 Cu2 I1 104.97(3) . . ? S10 Cu2 I1 112.88(3) . . ? S13 Cu2 I1 104.46(3) . . ? S5 Cu2 Cu1 154.60(3) . . ? S10 Cu2 Cu1 101.79(3) . . ? S13 Cu2 Cu1 54.74(2) . . ? I1 Cu2 Cu1 58.666(15) . . ? S5 Cu2 Cu11 49.34(3) . . ? S10 Cu2 Cu11 96.17(3) . . ? S13 Cu2 Cu11 78.99(3) . . ? I1 Cu2 Cu11 146.11(2) . . ? Cu1 Cu2 Cu11 133.70(2) . . ? S5 Cu2 Cu9 138.64(3) . . ? S10 Cu2 Cu9 47.68(2) . . ? S13 Cu2 Cu9 65.68(2) . . ? I1 Cu2 Cu9 112.96(2) . . ? Cu1 Cu2 Cu9 65.419(17) . . ? Cu11 Cu2 Cu9 99.32(2) . . ? S6 Cu7 S8 106.24(4) . . ? S6 Cu7 I1 126.33(3) . . ? S8 Cu7 I1 126.03(3) . . ? S6 Cu7 Cu1 138.89(3) . . ? S8 Cu7 Cu1 91.49(3) . . ? I1 Cu7 Cu1 57.971(15) . . ? S6 Cu7 Cu3 95.81(3) . . ? S8 Cu7 Cu3 52.06(2) . . ? I1 Cu7 Cu3 124.13(2) . . ? Cu1 Cu7 Cu3 66.156(18) . . ? S10 Cu9 S12 100.27(4) . . ? S10 Cu9 I3 130.98(3) . . ? S12 Cu9 I3 126.55(3) . . ? S10 Cu9 Cu6 94.44(3) . . ? S12 Cu9 Cu6 140.02(3) . . ? I3 Cu9 Cu6 60.290(15) . . ? S10 Cu9 Cu5 141.47(3) . . ? S12 Cu9 Cu5 91.15(3) . . ? I3 Cu9 Cu5 59.877(15) . . ? Cu6 Cu9 Cu5 56.447(16) . . ? S10 Cu9 Cu2 50.39(3) . . ? S12 Cu9 Cu2 90.44(3) . . ? I3 Cu9 Cu2 131.24(2) . . ? Cu6 Cu9 Cu2 70.954(19) . . ? Cu5 Cu9 Cu2 93.297(19) . . ? S13 Cu5 S11 124.71(4) . . ? S13 Cu5 S4 114.39(3) . . ? S11 Cu5 S4 100.64(3) . . ? S13 Cu5 Cu6 55.47(3) . . ? S11 Cu5 Cu6 153.28(3) . . ? S4 Cu5 Cu6 102.38(3) . . ? S13 Cu5 I3 106.69(3) . . ? S11 Cu5 I3 100.84(3) . . ? S4 Cu5 I3 108.00(3) . . ? Cu6 Cu5 I3 59.025(15) . . ? S13 Cu5 Cu8 64.37(2) . . ? S11 Cu5 Cu8 141.84(3) . . ? S4 Cu5 Cu8 51.49(2) . . ? Cu6 Cu5 Cu8 64.738(19) . . ? I3 Cu5 Cu8 111.87(2) . . ? S13 Cu5 Cu10 83.88(3) . . ? S11 Cu5 Cu10 49.96(2) . . ? S4 Cu5 Cu10 95.78(3) . . ? Cu6 Cu5 Cu10 139.30(2) . . ? I3 Cu5 Cu10 146.09(2) . . ? Cu8 Cu5 Cu10 101.80(2) . . ? S13 Cu5 Cu9 67.94(2) . . ? S11 Cu5 Cu9 94.70(3) . . ? S4 Cu5 Cu9 157.72(3) . . ? Cu6 Cu5 Cu9 59.547(16) . . ? I3 Cu5 Cu9 52.718(15) . . ? Cu8 Cu5 Cu9 120.44(2) . . ? Cu10 Cu5 Cu9 106.47(2) . . ? S2 Cu6 S9 104.25(4) . . ? S2 Cu6 S13 108.76(4) . . ? S9 Cu6 S13 122.81(4) . . ? S2 Cu6 I3 106.95(3) . . ? S9 Cu6 I3 106.17(3) . . ? S13 Cu6 I3 106.98(3) . . ? S2 Cu6 Cu5 96.01(3) . . ? S9 Cu6 Cu5 158.79(3) . . ? S13 Cu6 Cu5 53.78(2) . . ? I3 Cu6 Cu5 61.013(16) . . ? S2 Cu6 Cu11 96.11(3) . . ? S9 Cu6 Cu11 50.26(2) . . ? S13 Cu6 Cu11 80.58(3) . . ? I3 Cu6 Cu11 151.28(2) . . ? Cu5 Cu6 Cu11 134.27(2) . . ? S2 Cu6 Cu9 157.08(3) . . ? S9 Cu6 Cu9 94.87(3) . . ? S13 Cu6 Cu9 69.56(2) . . ? I3 Cu6 Cu9 54.599(15) . . ? Cu5 Cu6 Cu9 64.005(18) . . ? Cu11 Cu6 Cu9 105.89(2) . . ? S2 Cu6 Cu8 49.02(3) . . ? S9 Cu6 Cu8 140.94(3) . . ? S13 Cu6 Cu8 61.27(2) . . ? I3 Cu6 Cu8 108.902(18) . . ? Cu5 Cu6 Cu8 59.072(17) . . ? Cu11 Cu6 Cu8 99.070(19) . . ? Cu9 Cu6 Cu8 119.33(2) . . ? S2 Cu8 S4 99.44(4) . . ? S2 Cu8 I2 125.51(3) . . ? S4 Cu8 I2 126.06(3) . . ? S2 Cu8 Cu4 94.19(3) . . ? S4 Cu8 Cu4 151.29(3) . . ? I2 Cu8 Cu4 60.984(16) . . ? S2 Cu8 Cu3 147.72(3) . . ? S4 Cu8 Cu3 95.37(3) . . ? I2 Cu8 Cu3 63.268(17) . . ? Cu4 Cu8 Cu3 61.403(19) . . ? S2 Cu8 S13 98.90(3) . . ? S4 Cu8 S13 102.05(3) . . ? I2 Cu8 S13 98.90(2) . . ? Cu4 Cu8 S13 50.59(2) . . ? Cu3 Cu8 S13 49.73(2) . . ? S2 Cu8 Cu5 95.46(3) . . ? S4 Cu8 Cu5 53.94(3) . . ? I2 Cu8 Cu5 133.81(2) . . ? Cu4 Cu8 Cu5 99.86(2) . . ? Cu3 Cu8 Cu5 70.660(19) . . ? S13 Cu8 Cu5 49.30(2) . . ? S2 Cu8 Cu6 51.35(3) . . ? S4 Cu8 Cu6 97.36(3) . . ? I2 Cu8 Cu6 132.66(2) . . ? Cu4 Cu8 Cu6 71.862(18) . . ? Cu3 Cu8 Cu6 98.50(2) . . ? S13 Cu8 Cu6 48.84(2) . . ? Cu5 Cu8 Cu6 56.189(16) . . ? S13 Cu3 S8 116.77(3) . . ? S13 Cu3 S3 128.12(3) . . ? S8 Cu3 S3 99.31(3) . . ? S13 Cu3 Cu10 86.46(3) . . ? S8 Cu3 Cu10 97.52(3) . . ? S3 Cu3 Cu10 51.19(3) . . ? S13 Cu3 Cu8 65.57(2) . . ? S8 Cu3 Cu8 156.21(3) . . ? S3 Cu3 Cu8 95.77(3) . . ? Cu10 Cu3 Cu8 106.27(2) . . ? S13 Cu3 I2 104.45(3) . . ? S8 Cu3 I2 103.79(3) . . ? S3 Cu3 I2 101.26(3) . . ? Cu10 Cu3 I2 147.94(2) . . ? Cu8 Cu3 I2 54.934(15) . . ? S13 Cu3 Cu4 53.73(2) . . ? S8 Cu3 Cu4 101.75(3) . . ? S3 Cu3 Cu4 153.19(3) . . ? Cu10 Cu3 Cu4 140.16(2) . . ? Cu8 Cu3 Cu4 59.260(17) . . ? I2 Cu3 Cu4 57.611(16) . . ? S13 Cu3 Cu7 69.79(2) . . ? S8 Cu3 Cu7 48.58(2) . . ? S3 Cu3 Cu7 142.27(3) . . ? Cu10 Cu3 Cu7 106.80(2) . . ? Cu8 Cu3 Cu7 121.40(2) . . ? I2 Cu3 Cu7 105.259(19) . . ? Cu4 Cu3 Cu7 64.238(17) . . ? S6 Cu4 S13 112.05(4) . . ? S6 Cu4 S1 104.93(4) . . ? S13 Cu4 S1 124.01(4) . . ? S6 Cu4 I2 103.43(3) . . ? S13 Cu4 I2 106.25(3) . . ? S1 Cu4 I2 104.11(3) . . ? S6 Cu4 Cu11 99.18(3) . . ? S13 Cu4 Cu11 82.22(3) . . ? S1 Cu4 Cu11 50.92(2) . . ? I2 Cu4 Cu11 150.36(2) . . ? S6 Cu4 Cu8 153.54(3) . . ? S13 Cu4 Cu8 65.18(2) . . ? S1 Cu4 Cu8 96.90(3) . . ? I2 Cu4 Cu8 55.956(15) . . ? Cu11 Cu4 Cu8 106.21(2) . . ? S6 Cu4 Cu3 97.22(3) . . ? S13 Cu4 Cu3 52.54(2) . . ? S1 Cu4 Cu3 155.93(3) . . ? I2 Cu4 Cu3 60.820(15) . . ? Cu11 Cu4 Cu3 134.74(2) . . ? Cu8 Cu4 Cu3 59.337(18) . . ? S7 Cu10 S3 121.06(3) . . ? S7 Cu10 S11 119.28(4) . . ? S3 Cu10 S11 119.33(4) . . ? S7 Cu10 Cu3 95.47(3) . . ? S3 Cu10 Cu3 56.00(3) . . ? S11 Cu10 Cu3 123.39(3) . . ? S7 Cu10 Cu1 53.61(3) . . ? S3 Cu10 Cu1 125.81(3) . . ? S11 Cu10 Cu1 94.75(3) . . ? Cu3 Cu10 Cu1 70.318(18) . . ? S7 Cu10 Cu5 125.81(3) . . ? S3 Cu10 Cu5 94.46(3) . . ? S11 Cu10 Cu5 53.05(3) . . ? Cu3 Cu10 Cu5 70.512(18) . . ? Cu1 Cu10 Cu5 72.716(18) . . ? S5 Cu11 S9 117.99(4) . . ? S5 Cu11 S1 121.85(4) . . ? S9 Cu11 S1 118.72(4) . . ? S5 Cu11 Cu4 95.39(3) . . ? S9 Cu11 Cu4 129.08(3) . . ? S1 Cu11 Cu4 56.67(3) . . ? S5 Cu11 Cu6 126.43(3) . . ? S9 Cu11 Cu6 54.68(3) . . ? S1 Cu11 Cu6 96.59(3) . . ? Cu4 Cu11 Cu6 74.770(18) . . ? S5 Cu11 Cu2 53.06(3) . . ? S9 Cu11 Cu2 95.02(3) . . ? S1 Cu11 Cu2 130.94(3) . . ? Cu4 Cu11 Cu2 74.586(18) . . ? Cu6 Cu11 Cu2 73.837(19) . . ? Cu7 I1 Cu1 68.965(16) . . ? Cu7 I1 Cu2 71.407(17) . . ? Cu1 I1 Cu2 62.057(17) . . ? Cu9 I3 Cu6 65.110(16) . . ? Cu9 I3 Cu5 67.405(16) . . ? Cu6 I3 Cu5 59.961(15) . . ? Cu8 I2 Cu4 63.060(17) . . ? Cu8 I2 Cu3 61.798(17) . . ? Cu4 I2 Cu3 61.569(16) . . ? C1 O1 P1 121.7(3) . . ? C4 O2 P1 122.7(3) . . ? C7 O3 P2 121.0(2) . . ? C10 O4 P2 123.1(2) . . ? C13 O5 P3 127.0(3) . . ? C16 O6 C16' 21.8(4) . . ? C16 O6 P3 121.8(4) . . ? C16' O6 P3 127.3(6) . . ? C19 O7 P4 125.1(2) . . ? C22 O8 P4 125.7(2) . . ? C25 O9 P5 122.7(3) . . ? C28 O10 P5 123.2(2) . . ? C31 O11 P6 125.2(2) . . ? C34 O12 P6 126.3(2) . . ? O1 P1 O2 100.87(17) . . ? O1 P1 S2 109.74(12) . . ? O2 P1 S2 109.98(13) . . ? O1 P1 S1 108.34(13) . . ? O2 P1 S1 110.26(13) . . ? S2 P1 S1 116.50(6) . . ? O3 P2 O4 101.74(14) . . ? O3 P2 S3 106.27(10) . . ? O4 P2 S3 110.21(10) . . ? O3 P2 S4 110.79(10) . . ? O4 P2 S4 109.47(11) . . ? S3 P2 S4 117.22(5) . . ? O6 P3 O5 109.18(16) . . ? O6 P3 S6 112.12(12) . . ? O5 P3 S6 102.31(11) . . ? O6 P3 S5 102.34(11) . . ? O5 P3 S5 111.24(11) . . ? S6 P3 S5 119.60(6) . . ? O8 P4 O7 108.98(15) . . ? O8 P4 S8 111.49(11) . . ? O7 P4 S8 103.21(11) . . ? O8 P4 S7 103.01(10) . . ? O7 P4 S7 110.70(11) . . ? S8 P4 S7 119.32(5) . . ? O10 P5 O9 102.04(15) . . ? O10 P5 S10 111.58(11) . . ? O9 P5 S10 104.34(11) . . ? O10 P5 S9 108.32(12) . . ? O9 P5 S9 112.18(11) . . ? S10 P5 S9 117.30(5) . . ? O11 P6 O12 108.34(15) . . ? O11 P6 S12 110.42(10) . . ? O12 P6 S12 104.56(11) . . ? O11 P6 S11 103.93(10) . . ? O12 P6 S11 109.98(11) . . ? S12 P6 S11 119.33(5) . . ? P1 S1 Cu11 99.69(5) . . ? P1 S1 Cu4 108.51(5) . . ? Cu11 S1 Cu4 72.41(3) . . ? P1 S2 Cu8 109.78(5) . . ? P1 S2 Cu6 102.35(5) . . ? Cu8 S2 Cu6 79.63(3) . . ? P2 S3 Cu10 98.87(4) . . ? P2 S3 Cu3 109.37(5) . . ? Cu10 S3 Cu3 72.81(3) . . ? P2 S4 Cu8 107.55(4) . . ? P2 S4 Cu5 102.54(4) . . ? Cu8 S4 Cu5 74.56(3) . . ? P3 S5 Cu11 100.84(5) . . ? P3 S5 Cu2 107.85(5) . . ? Cu11 S5 Cu2 77.60(3) . . ? P3 S6 Cu7 105.51(5) . . ? P3 S6 Cu4 101.27(5) . . ? Cu7 S6 Cu4 83.97(3) . . ? P4 S7 Cu10 102.15(4) . . ? P4 S7 Cu1 104.78(5) . . ? Cu10 S7 Cu1 76.76(3) . . ? P4 S8 Cu7 103.26(4) . . ? P4 S8 Cu3 103.55(4) . . ? Cu7 S8 Cu3 79.36(3) . . ? P5 S9 Cu11 100.48(5) . . ? P5 S9 Cu6 108.88(5) . . ? Cu11 S9 Cu6 75.06(3) . . ? P5 S10 Cu9 106.52(5) . . ? P5 S10 Cu2 102.95(4) . . ? Cu9 S10 Cu2 81.94(3) . . ? P6 S11 Cu10 101.93(4) . . ? P6 S11 Cu5 106.31(4) . . ? Cu10 S11 Cu5 76.98(3) . . ? P6 S12 Cu9 102.31(5) . . ? P6 S12 Cu1 103.80(4) . . ? Cu9 S12 Cu1 85.62(3) . . ? Cu3 S13 Cu5 87.58(3) . . ? Cu3 S13 Cu4 73.73(3) . . ? Cu5 S13 Cu4 130.50(4) . . ? Cu3 S13 Cu6 134.43(4) . . ? Cu5 S13 Cu6 70.75(3) . . ? Cu4 S13 Cu6 90.30(3) . . ? Cu3 S13 Cu1 85.66(3) . . ? Cu5 S13 Cu1 90.78(3) . . ? Cu4 S13 Cu1 131.36(4) . . ? Cu6 S13 Cu1 132.38(4) . . ? Cu3 S13 Cu2 130.98(4) . . ? Cu5 S13 Cu2 132.90(4) . . ? Cu4 S13 Cu2 90.79(3) . . ? Cu6 S13 Cu2 90.52(3) . . ? Cu1 S13 Cu2 70.25(3) . . ? Cu3 S13 Cu8 64.70(3) . . ? Cu5 S13 Cu8 66.33(2) . . ? Cu4 S13 Cu8 64.23(2) . . ? Cu6 S13 Cu8 69.89(3) . . ? Cu1 S13 Cu8 142.20(4) . . ? Cu2 S13 Cu8 147.18(4) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 28.33 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.688 _refine_diff_density_min -1.705 _refine_diff_density_rms 0.127 #===END _database_code_depnum_ccdc_archive 'CCDC 943815'