_publ_requested_journal 'JACS' _publ_section_title ; Robust Affinity Standards for Cu(I) Biochemistry ; _publ_contact_author_email fahrni@chemistry.gatech.edu _publ_contact_author_name 'Christoph J. Fahrni' _publ_contact_author_phone ? _publ_contact_author_address ; School of Chemistry and Biochemistry, Petit Institute for Bioengineering and Bioscience, Georgia Institute of Technology, 901 Atlantic Drive, Atlanta, GA 30332, U.S.A. ; data_13a _audit_creation_date 2012-11-21 _audit_creation_method ; Olex2 1.2-beta (compiled Aug 15 2012 15:59:22, GUI svn.r4314) ; _publ_section_references ; Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122 Petricek,V., Dusek,M. & Palatinus,L.(2006). Jana2006. The crystallographic computing system. Institute of Physics, Praha, Czech Republic. Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. Bruker (2011). APEX2 Version 2011.2-4. Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2009). SAINT-Plus Version 7.68a. Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (2008). SADABS Version 2008-1. Bruker AXS Inc., Madison, Wisconsin, USA. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety '2(C15 H30 S6 O9 N Cu 2-), 7(Na +), 4(H2 O), 3(Cl O4 -)' _chemical_formula_sum 'C30 H68 Cl3 Cu2 N2 Na7 O34 S12' _chemical_formula_weight 1780.08 _chemical_melting_point ? 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' 'Cl' 'Cl' 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_Hall '-P 1' _symmetry_space_group_name_H-M 'P -1' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.8246(15) _cell_length_b 9.8488(15) _cell_length_c 18.657(3) _cell_angle_alpha 82.967(2) _cell_angle_beta 84.686(2) _cell_angle_gamma 64.474(2) _cell_volume 1615.2(4) _cell_formula_units_Z 1 _cell_measurement_reflns_used 9936 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 31.052 _cell_measurement_theta_min 2.202 _exptl_absorpt_coefficient_mu 1.308 _exptl_absorpt_correction_T_max 1.0000 _exptl_absorpt_correction_T_min 0.5883 _exptl_absorpt_correction_type numerical _exptl_absorpt_process_details ; SADABS-2012/1 was used for absorption correction. wR2(int) was 0.0628 before and 0.0436 after correction. The Ratio of minimum to maximum transmission is 0.5883. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.830 _exptl_crystal_density_meas . _exptl_crystal_density_method ? _exptl_crystal_description needle _exptl_crystal_F_000 912 _exptl_crystal_size_max 0.721 _exptl_crystal_size_mid 0.249 _exptl_crystal_size_min 0.092 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0316 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_number 25301 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_sigmaI/netI 0.0387 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 31.126 _diffrn_reflns_theta_min 2.202 _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean 512 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device_type 'Bruker D8 diffractometer with APEX2 detector' _diffrn_measurement_method '\f and \w scans with a narrow frame width' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 8718 _reflns_number_total 10289 _reflns_special_details ; The reflections were merged according to the crystal class for structure refinement and the calculation of statistics. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT v7.68A (Bruker, 2009)' _computing_data_collection 'APEX2 v2011.2-4 (Bruker, 2011)' _computing_data_reduction 'SAINT v7.68A (Bruker, 2009)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 1.026 _refine_diff_density_min -0.603 _refine_diff_density_rms 0.105 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.029 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 574 _refine_ls_number_reflns 10289 _refine_ls_number_restraints 572 _refine_ls_R_factor_all 0.0474 _refine_ls_R_factor_gt 0.0390 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0640P)^2^+0.8928P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1038 _refine_ls_wR_factor_ref 0.1098 _refine_special_details ; ? ; _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary iterative _atom_sites_solution_secondary ? 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.66506(3) 0.11200(3) 0.18236(2) 0.01700(6) Uani 1 1 d . . . . . Cl1B Cl 0.3334(6) -0.2371(6) 0.1917(3) 0.0244(3) Uani 0.286(4) 1 d D U P A 2 S6 S 0.88956(5) -0.19620(5) 0.39018(2) 0.01282(8) Uiso 1 1 d . . . . . S4 S 0.70864(5) 0.33564(5) 0.42428(2) 0.01376(9) Uani 1 1 d . . . . . S5 S 0.24553(5) 0.16255(5) 0.39652(2) 0.01390(9) Uani 1 1 d . . . . . S1 S 0.87474(5) 0.14421(5) 0.19409(3) 0.01803(9) Uani 1 1 d . . . . . S3 S 0.65595(6) -0.11331(5) 0.17887(3) 0.01841(9) Uani 1 1 d . . . . . S2 S 0.43167(6) 0.31165(6) 0.17988(3) 0.01937(10) Uani 1 1 d . . . . . Na3 Na 1.0000 0.0000 0.5000 0.01450(19) Uani 1 2 d S . P . . Na1 Na 0.60152(9) 0.09457(9) 0.47388(4) 0.01723(15) Uani 1 1 d . . . . . Na2 Na 0.25275(9) -0.18843(9) 0.38272(4) 0.01844(15) Uani 1 1 d D . . . . Na4 Na 0.16645(10) 0.47606(10) 0.47315(5) 0.02457(18) Uani 1 1 d D . . . . O8 O 0.72804(15) -0.09713(16) 0.39529(8) 0.0205(3) Uani 1 1 d . . . . . O5 O 0.13880(17) 0.32033(15) 0.39763(8) 0.0217(3) Uani 1 1 d . . . . . O1 O 0.78672(15) 0.21573(15) 0.48014(8) 0.0190(3) Uani 1 1 d . . . . . O7 O 0.92822(17) -0.34137(16) 0.43276(8) 0.0205(3) Uani 1 1 d . . . . . O2 O 0.56356(15) 0.33532(16) 0.41225(8) 0.0195(3) Uani 1 1 d . . . . . O6 O 0.36938(17) 0.11894(18) 0.44509(8) 0.0224(3) Uani 1 1 d . . . . . O9 O 0.98200(16) -0.12077(16) 0.40534(8) 0.0201(3) Uani 1 1 d . . . . . O4 O 0.17159(16) 0.06007(16) 0.40955(8) 0.0189(3) Uani 1 1 d . . . . . O3 O 0.69605(17) 0.48197(15) 0.43993(8) 0.0216(3) Uani 1 1 d . . . . . O1W O 0.49990(16) -0.21760(16) 0.41425(8) 0.0204(3) Uani 1 1 d D . . . . O3B O 0.2822(14) -0.1145(12) 0.1347(6) 0.0420(7) Uani 0.286(4) 1 d D U P A 2 O2W O 0.30015(18) 0.55862(17) 0.37391(10) 0.0285(3) Uani 1 1 d D . . . . O4B O 0.4836(13) -0.3409(18) 0.1699(10) 0.0530(9) Uani 0.286(4) 1 d D U P A 2 O2B O 0.3390(15) -0.1806(16) 0.2580(5) 0.0676(11) Uani 0.286(4) 1 d D U P A 2 O5B O 0.2322(9) -0.3087(10) 0.2001(5) 0.0508(8) Uani 0.286(4) 1 d D U P A 2 N1 N 0.6864(2) 0.1408(2) 0.06579(9) 0.0201(3) Uani 1 1 d . . . . . C15 C 0.9323(2) -0.2310(2) 0.29836(10) 0.0173(3) Uani 1 1 d D . . . . C12 C 0.3330(2) 0.1414(2) 0.30840(10) 0.0188(3) Uani 1 1 d D . . . . C8 C 0.7255(2) 0.3822(2) 0.27694(11) 0.0181(3) Uani 1 1 d D . . . . C9 C 0.8175(2) 0.2904(2) 0.34219(10) 0.0181(3) Uani 1 1 d D . . . . C1 C 0.9324(2) 0.1319(3) 0.09859(12) 0.0243(4) Uani 1 1 d D . . . . C5 C 0.6479(3) -0.0960(2) 0.08105(11) 0.0228(4) Uani 1 1 d D . . . . C7 C 0.8134(2) 0.3438(2) 0.20489(11) 0.0190(3) Uani 1 1 d D . . . . C2 C 0.8023(3) 0.2001(3) 0.04768(11) 0.0243(4) Uani 1 1 d D . . . . C14 C 0.8571(3) -0.3220(2) 0.27281(11) 0.0214(4) Uani 1 1 d D . . . . C10 C 0.2994(2) 0.2282(3) 0.17470(11) 0.0230(4) Uani 1 1 d D . . . . C6 C 0.7361(3) -0.0118(2) 0.04129(11) 0.0231(4) Uani 1 1 d D . . . . C3 C 0.4535(3) 0.3763(2) 0.08582(12) 0.0247(4) Uani 1 1 d D . . . . C13 C 0.8298(3) -0.2850(2) 0.19196(11) 0.0230(4) Uani 1 1 d D . . . . C11 C 0.2213(2) 0.2217(3) 0.24892(11) 0.0222(4) Uani 1 1 d D . . . . C4 C 0.5383(3) 0.2485(2) 0.03772(11) 0.0230(4) Uani 1 1 d D . . . . O12 O 0.9597(6) 0.4035(6) -0.0425(3) 0.0643(15) Uani 0.5 1 d D U P B -1 O10 O 0.8986(5) 0.6543(5) -0.0183(3) 0.0546(12) Uani 0.5 1 d D U P B -1 O13 O 1.1544(5) 0.4750(5) -0.0306(3) 0.0545(12) Uani 0.5 1 d D U P B -1 O11 O 1.0036(6) 0.4493(5) 0.0736(2) 0.0582(13) Uani 0.5 1 d D U P B -1 Cl2 Cl 1.004(2) 0.503(2) 0.0004(16) 0.0256(10) Uani 0.5 1 d . U P B -1 O3A O 0.3020(5) -0.0871(4) 0.1415(2) 0.0420(7) Uani 0.714(4) 1 d D U P A 1 O2A O 0.2856(6) -0.1970(6) 0.25625(19) 0.0676(11) Uani 0.714(4) 1 d D U P A 1 Cl1A Cl 0.3097(2) -0.2233(2) 0.18144(10) 0.0244(3) Uani 0.714(4) 1 d D U P A 1 O5A O 0.1955(4) -0.2615(4) 0.1597(2) 0.0508(8) Uani 0.714(4) 1 d D U P A 1 O4A O 0.4590(5) -0.3410(7) 0.1680(4) 0.0530(9) Uani 0.714(4) 1 d D U P A 1 H8A H 0.693(2) 0.4865(8) 0.2789(13) 0.012(5) Uiso 1 1 d D . . . . H12A H 0.4040(18) 0.182(2) 0.3061(14) 0.023(6) Uiso 1 1 d D . . . . H9A H 0.851(3) 0.1856(8) 0.3419(14) 0.024(7) Uiso 1 1 d D . . . . H14A H 0.7635(13) -0.300(3) 0.2978(11) 0.015(6) Uiso 1 1 d D . . . . H10A H 0.229(2) 0.291(3) 0.1407(11) 0.031(7) Uiso 1 1 d D . . . . H6A H 0.8401(9) -0.068(3) 0.0478(14) 0.021(6) Uiso 1 1 d D . . . . H10B H 0.343(3) 0.1314(13) 0.1580(13) 0.027(7) Uiso 1 1 d D . . . . H15A H 1.0380(7) -0.281(3) 0.2927(14) 0.023(7) Uiso 1 1 d D . . . . H4A H 0.4804(19) 0.195(2) 0.0338(13) 0.016(6) Uiso 1 1 d D . . . . H9B H 0.9049(15) 0.303(3) 0.3488(14) 0.023(6) Uiso 1 1 d D . . . . H8B H 0.6394(15) 0.363(2) 0.2776(14) 0.019(6) Uiso 1 1 d D . . . . H11A H 0.160(2) 0.3186(13) 0.2634(13) 0.022(6) Uiso 1 1 d D . . . . H14B H 0.916(3) -0.4258(10) 0.2839(16) 0.034(8) Uiso 1 1 d D . . . . H1A H 0.985(3) 0.0275(9) 0.0949(15) 0.025(7) Uiso 1 1 d D . . . . H5A H 0.5434(8) -0.047(3) 0.0748(15) 0.026(7) Uiso 1 1 d D . . . . H3A H 0.505(2) 0.437(2) 0.0869(15) 0.028(7) Uiso 1 1 d D . . . . H7A H 0.9026(15) 0.356(3) 0.2069(15) 0.023(6) Uiso 1 1 d D . . . . H7B H 0.747(2) 0.405(2) 0.1687(10) 0.024(7) Uiso 1 1 d D . . . . H2A H 0.754(3) 0.3044(9) 0.0528(14) 0.024(7) Uiso 1 1 d D . . . . H6B H 0.727(3) 0.000(3) -0.0091(4) 0.021(6) Uiso 1 1 d D . . . . H15B H 0.896(3) -0.1335(14) 0.2740(13) 0.033(8) Uiso 1 1 d D . . . . H11B H 0.161(2) 0.169(2) 0.2481(17) 0.040(8) Uiso 1 1 d D . . . . H13A H 0.910(3) -0.271(3) 0.1662(16) 0.029(7) Uiso 1 1 d . . . . . H2B H 0.841(3) 0.179(3) 0.0002(6) 0.029(7) Uiso 1 1 d D . . . . H3B H 0.3573(14) 0.436(3) 0.0678(14) 0.032(7) Uiso 1 1 d D . . . . H5B H 0.683(3) -0.1952(12) 0.0682(14) 0.032(8) Uiso 1 1 d D . . . . H1B H 0.996(2) 0.181(2) 0.0874(15) 0.029(7) Uiso 1 1 d D . . . . H12B H 0.392(3) 0.0381(10) 0.3034(15) 0.029(7) Uiso 1 1 d D . . . . H4B H 0.545(3) 0.289(3) -0.0100(5) 0.023(7) Uiso 1 1 d D . . . . H13B H 0.816(3) -0.3594(19) 0.1705(13) 0.029(7) Uiso 1 1 d D . . . . H2WA H 0.4054(11) 0.481(2) 0.3799(12) 0.035 Uiso 1 1 d D U . . . H2WB H 0.271(2) 0.535(3) 0.3292(7) 0.035 Uiso 1 1 d D U . . . H1WA H 0.5802(19) -0.3209(13) 0.425(2) 0.089(11) Uiso 1 1 d D . . . . H1WB H 0.554(2) -0.158(3) 0.3909(19) 0.089(11) Uiso 1 1 d D . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0210(1) 0.0189(1) 0.0137(1) -0.0008(1) -0.0010(1) -0.0110(1) Cl1A 0.0306(7) 0.0259(4) 0.0186(6) -0.0008(4) -0.0011(4) -0.0142(4) S1 0.0200(2) 0.0183(2) 0.0175(2) -0.0015(2) -0.0013(2) -0.0097(2) S2 0.0222(2) 0.0196(2) 0.0166(2) 0.0003(2) -0.0008(2) -0.0097(2) S3 0.0227(2) 0.0188(2) 0.0169(2) -0.0008(2) -0.0032(2) -0.0115(2) S4 0.0127(2) 0.0107(2) 0.0161(2) 0.0002(1) -0.0021(2) -0.0033(1) S5 0.0140(2) 0.0134(2) 0.0150(2) 0.0002(2) -0.0012(2) -0.0068(2) S6 0.0135(2) 0.0120(2) 0.0130(2) -0.0017(1) -0.0008(1) -0.0052(1) Na1 0.0165(3) 0.0155(3) 0.0207(4) -0.0017(3) -0.0006(3) -0.0077(3) Na2 0.0188(4) 0.0171(3) 0.0202(4) -0.0031(3) -0.0006(3) -0.0081(3) Na3 0.0125(4) 0.0131(4) 0.0161(5) -0.0029(4) -0.0021(4) -0.0030(4) Na4 0.0280(4) 0.0231(4) 0.0258(4) 0.0021(3) -0.0078(3) -0.0137(3) O1 0.0171(6) 0.0162(6) 0.0167(6) 0.0028(5) -0.0027(5) -0.0012(5) O1W 0.0161(6) 0.0153(6) 0.0269(7) -0.0022(5) -0.0004(5) -0.0039(5) O2 0.0140(6) 0.0193(6) 0.0248(7) 0.0020(5) -0.0041(5) -0.0072(5) O2A 0.083(3) 0.107(2) 0.0229(10) -0.0123(12) 0.0041(14) -0.048(2) O2W 0.0201(7) 0.0178(7) 0.0431(10) -0.0027(6) -0.0064(7) -0.0030(5) O3 0.0253(7) 0.0116(6) 0.0275(7) -0.0037(5) -0.0031(6) -0.0065(5) O3A 0.0461(16) 0.0425(15) 0.0461(14) 0.0161(12) -0.0158(11) -0.0295(11) O4 0.0178(6) 0.0177(6) 0.0246(7) -0.0028(5) 0.0026(5) -0.0112(5) O4A 0.0376(15) 0.0357(10) 0.0844(18) -0.0165(11) -0.0010(14) -0.0118(12) O5 0.0269(7) 0.0130(6) 0.0231(7) -0.0018(5) -0.0021(6) -0.0064(5) O5A 0.0451(15) 0.0576(18) 0.064(2) -0.0093(15) -0.0024(13) -0.0345(14) O6 0.0201(7) 0.0315(8) 0.0181(7) 0.0044(6) -0.0068(5) -0.0140(6) O7 0.0258(7) 0.0157(6) 0.0178(6) 0.0025(5) -0.0006(5) -0.0078(5) O8 0.0139(6) 0.0196(6) 0.0251(7) -0.0058(5) 0.0013(5) -0.0038(5) O9 0.0217(7) 0.0223(7) 0.0214(7) -0.0055(5) -0.0034(5) -0.0127(5) N1 0.0247(8) 0.0228(8) 0.0152(7) -0.0006(6) -0.0007(6) -0.0126(7) C1 0.0250(10) 0.0320(11) 0.0194(9) -0.0062(8) 0.0052(8) -0.0155(8) C2 0.0313(11) 0.0305(10) 0.0157(9) -0.0010(8) 0.0040(8) -0.0186(9) C3 0.0295(10) 0.0222(9) 0.0192(9) 0.0046(7) -0.0010(8) -0.0097(8) C4 0.0295(10) 0.0249(10) 0.0142(8) 0.0026(7) -0.0036(7) -0.0118(8) C5 0.0311(10) 0.0232(9) 0.0181(9) -0.0021(7) -0.0072(8) -0.0141(8) C6 0.0304(10) 0.0261(10) 0.0139(8) -0.0043(7) -0.0013(7) -0.0123(8) C7 0.0247(9) 0.0178(8) 0.0174(8) 0.0006(7) -0.0027(7) -0.0118(7) C8 0.0198(8) 0.0163(8) 0.0170(8) 0.0000(6) -0.0048(7) -0.0060(7) C9 0.0163(8) 0.0182(8) 0.0163(8) -0.0004(7) -0.0007(6) -0.0044(7) C10 0.0226(9) 0.0329(11) 0.0168(9) 0.0004(8) -0.0039(7) -0.0151(8) C11 0.0172(8) 0.0306(10) 0.0189(9) 0.0015(8) -0.0029(7) -0.0108(8) C12 0.0150(8) 0.0230(9) 0.0154(8) 0.0022(7) 0.0001(6) -0.0066(7) C13 0.0326(11) 0.0170(8) 0.0174(9) -0.0044(7) -0.0049(8) -0.0073(8) C14 0.0320(10) 0.0169(8) 0.0174(9) -0.0009(7) -0.0059(8) -0.0115(8) C15 0.0213(8) 0.0201(8) 0.0124(8) -0.0025(6) 0.0003(6) -0.0106(7) Cl1B 0.0306(7) 0.0259(4) 0.0186(6) -0.0008(4) -0.0011(4) -0.0142(4) O2B 0.083(3) 0.107(2) 0.0229(10) -0.0123(12) 0.0041(14) -0.048(2) O3B 0.0461(16) 0.0425(15) 0.0461(14) 0.0161(12) -0.0158(11) -0.0295(11) O4B 0.0376(15) 0.0357(10) 0.0844(18) -0.0165(11) -0.0010(14) -0.0118(12) O5B 0.0451(15) 0.0576(18) 0.064(2) -0.0093(15) -0.0024(13) -0.0345(14) Cl2 0.0277(14) 0.0243(10) 0.0254(6) 0.0025(8) -0.0020(12) -0.0126(9) O10 0.054(3) 0.0299(19) 0.057(3) 0.0062(18) 0.002(2) 0.0010(17) O11 0.083(3) 0.053(3) 0.0270(19) 0.0056(18) 0.000(2) -0.021(2) O12 0.070(3) 0.094(3) 0.066(3) -0.053(3) 0.030(2) -0.064(3) O13 0.037(2) 0.056(3) 0.085(3) -0.033(2) 0.027(2) -0.0318(19) _geom_special_details ; Bond distances, angles etc. have been calculated using the rounded fractional coordinates. All su's are estimated from the variances of the (full) variance-covariance matrix. The cell esds are taken into account in the estimation of distances, angles and torsion angles ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_1 _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 S1 2.2485(7) . . yes Cu1 S2 2.2886(7) . . yes Cu1 S3 2.2680(7) . . yes Cu1 N1 2.1610(17) . . yes Cl1A O2A 1.430(4) . . yes Cl1A O3A 1.428(4) . . yes Cl1A O4A 1.448(6) . . yes Cl1A O5A 1.432(5) . . yes Cl1B O3B 1.450(12) . . yes Cl1B O4B 1.442(17) . . yes Cl1B O2B 1.432(12) . . yes Cl1B O5B 1.435(12) . . yes Cl2 O11 1.40(3) . . yes Cl2 O12 1.55(2) . . yes Cl2 O13 1.46(2) . . yes Cl2 O10 1.42(2) . . yes S1 C7 1.8225(19) . . yes S1 C1 1.821(2) . . yes S2 C3 1.818(2) . . yes S2 C10 1.827(3) . . yes S3 C13 1.823(2) . . yes S3 C5 1.818(2) . . yes S4 O1 1.4612(15) . . yes S4 Na1 3.0060(11) . . yes S4 C9 1.772(2) . . yes S4 O2 1.4647(17) . . yes S4 O3 1.4561(15) . . yes S5 C12 1.7756(19) . . yes S5 O6 1.4645(18) . . yes S5 O5 1.4540(15) . . yes S5 O4 1.4644(17) . . yes S6 O7 1.4592(15) . . yes S6 O8 1.4627(17) . . yes S6 C15 1.7649(19) . . yes S6 O9 1.4619(17) . . yes Na1 O6 2.296(2) . . yes Na1 O2 2.3944(17) . . yes Na1 O8 2.3616(17) . . yes Na1 O1W 2.4517(17) . 2_656 yes Na1 O6 2.3606(18) . 2_656 yes Na1 O1 2.5871(19) . . yes Na2 O9 2.456(2) . 1_455 yes Na2 O2B 2.405(10) . . yes Na2 O2A 2.359(4) . . yes Na2 O4 2.3282(17) . . yes Na2 O1W 2.439(2) . . yes Na2 O1 2.5509(17) . 2_656 yes Na2 O2W 2.3530(18) . 1_545 yes Na3 O4 2.4754(17) . 2_656 yes Na3 O9 2.3062(15) . 2_756 yes Na3 O4 2.4754(17) . 1_655 yes Na3 O1 2.2708(15) . 2_756 yes Na3 O9 2.3062(15) . . yes Na3 O1 2.2708(15) . . yes Na4 O5 2.3175(18) . . yes Na4 O2W 2.432(2) . . yes Na4 O3 2.383(2) . 2_666 yes Na4 O7 2.3763(19) . 1_465 yes Na4 O7 2.4284(19) . 2_656 yes O1W H1WB 0.99(3) . . no O1W H1WA 0.993(16) . . no O2W H2WA 0.993(16) . . no O2W H2WB 0.991(17) . . no N1 C4 1.480(3) . . yes N1 C6 1.483(3) . . yes N1 C2 1.485(4) . . yes C1 C2 1.522(4) . . no C3 C4 1.523(3) . . no C5 C6 1.529(4) . . no C7 C8 1.524(3) . . no C8 C9 1.532(3) . . no C10 C11 1.528(3) . . no C11 C12 1.524(3) . . no C13 C14 1.528(3) . . no C14 C15 1.522(3) . . no C1 H1B 0.94(2) . . no C1 H1A 0.939(9) . . no C2 H2A 0.941(9) . . no C2 H2B 0.942(15) . . no C3 H3B 0.94(2) . . no C3 H3A 0.94(2) . . no C4 H4A 0.94(2) . . no C4 H4B 0.939(13) . . no C5 H5A 0.939(19) . . no C5 H5B 0.940(13) . . no C6 H6A 0.94(2) . . no C6 H6B 0.941(9) . . no C7 H7B 0.942(19) . . no C7 H7A 0.94(2) . . no C8 H8A 0.940(8) . . no C8 H8B 0.942(17) . . no C9 H9B 0.94(2) . . no C9 H9A 0.939(8) . . no C10 H10B 0.941(14) . . no C10 H10A 0.94(2) . . no C11 H11B 0.94(2) . . no C11 H11A 0.940(14) . . no C12 H12A 0.94(2) . . no C12 H12B 0.941(11) . . no C13 H13A 0.94(3) . . no C13 H13B 0.94(2) . . no C14 H14B 0.940(13) . . no C14 H14A 0.94(2) . . no C15 H15A 0.940(18) . . no C15 H15B 0.940(16) . . no 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_2 _geom_angle_site_symmetry_3 _geom_angle_publ_flag S1 Cu1 S2 121.41(2) . . . yes S1 Cu1 S3 125.49(2) . . . yes S1 Cu1 N1 91.90(6) . . . yes S2 Cu1 S3 112.99(3) . . . yes S2 Cu1 N1 89.88(5) . . . yes S3 Cu1 N1 91.32(5) . . . yes O2A Cl1A O3A 107.3(3) . . . yes O2A Cl1A O4A 110.5(4) . . . yes O2A Cl1A O5A 109.9(3) . . . yes O3A Cl1A O4A 107.7(3) . . . yes O3A Cl1A O5A 110.2(3) . . . yes O4A Cl1A O5A 111.1(3) . . . yes O2B Cl1B O5B 110.4(8) . . . yes O2B Cl1B O3B 110.2(8) . . . yes O2B Cl1B O4B 109.1(10) . . . yes O4B Cl1B O5B 111.1(8) . . . yes O3B Cl1B O4B 106.9(10) . . . yes O3B Cl1B O5B 109.0(8) . . . yes O10 Cl2 O12 105.4(16) . . . yes O10 Cl2 O11 116.4(17) . . . yes O11 Cl2 O12 107.0(13) . . . yes O11 Cl2 O13 113.3(16) . . . yes O10 Cl2 O13 111.3(16) . . . yes O12 Cl2 O13 102.0(15) . . . yes Cu1 S1 C1 94.31(8) . . . yes Cu1 S1 C7 106.67(7) . . . yes C1 S1 C7 103.05(11) . . . yes C3 S2 C10 101.93(11) . . . yes Cu1 S2 C3 94.68(8) . . . yes Cu1 S2 C10 105.07(9) . . . yes C5 S3 C13 100.32(10) . . . yes Cu1 S3 C5 94.55(7) . . . yes Cu1 S3 C13 118.14(9) . . . yes Na1 S4 O2 51.78(6) . . . yes Na1 S4 O1 59.35(7) . . . yes O1 S4 O3 112.17(9) . . . yes O1 S4 C9 107.58(9) . . . yes O3 S4 C9 107.44(9) . . . yes Na1 S4 C9 109.08(7) . . . yes O1 S4 O2 109.68(9) . . . yes Na1 S4 O3 143.29(7) . . . yes O2 S4 O3 113.62(9) . . . yes O2 S4 C9 105.97(9) . . . yes O6 S5 C12 104.99(10) . . . yes O4 S5 C12 107.81(9) . . . yes O5 S5 O6 112.94(9) . . . yes O5 S5 C12 106.69(9) . . . yes O4 S5 O6 111.42(9) . . . yes O4 S5 O5 112.46(10) . . . yes O7 S6 O9 112.93(9) . . . yes O7 S6 C15 107.84(9) . . . yes O7 S6 O8 112.59(10) . . . yes O8 S6 C15 105.88(9) . . . yes O8 S6 O9 112.16(9) . . . yes O9 S6 C15 104.78(9) . . . yes O1 Na1 O1W 81.13(6) . . 2_656 yes O1 Na1 O6 117.98(6) . . 2_656 yes O2 Na1 O6 92.71(6) . . . yes S4 Na1 O1 29.07(3) . . . yes S4 Na1 O2 28.72(4) . . . yes S4 Na1 O6 121.42(5) . . . yes S4 Na1 O8 105.22(5) . . . yes O2 Na1 O8 109.88(6) . . . yes O1W Na1 O2 89.01(6) 2_656 . . yes O1 Na1 O2 57.24(5) . . . yes O1 Na1 O6 149.18(6) . . . yes O1 Na1 O8 104.01(6) . . . yes O2 Na1 O6 169.01(6) . . 2_656 yes O6 Na1 O8 91.98(6) . . . yes O1W Na1 O6 92.66(6) 2_656 . . yes S4 Na1 O1W 88.56(4) . . 2_656 yes S4 Na1 O6 147.00(6) . . 2_656 yes O1W Na1 O6 80.28(6) 2_656 . 2_656 yes O6 Na1 O8 80.57(6) 2_656 . . yes O1W Na1 O8 160.31(6) 2_656 . . yes O6 Na1 O6 90.25(7) . . 2_656 yes O1W Na2 O2W 101.05(7) . . 1_545 yes O1W Na2 O9 154.22(6) . . 1_455 yes O2A Na2 O9 103.21(16) . . 1_455 yes O1 Na2 O1W 82.12(6) 2_656 . . yes O2A Na2 O4 109.12(14) . . . yes O2W Na2 O9 90.62(7) 1_545 . 1_455 yes O1 Na2 O9 74.46(6) 2_656 . 1_455 yes O1 Na2 O2W 92.18(6) 2_656 . 1_545 yes O2W Na2 O4 168.69(7) 1_545 . . yes O1 Na2 O4 78.75(5) 2_656 . . yes O2A Na2 O2W 79.62(14) . . 1_545 yes O1 Na2 O2A 171.51(15) 2_656 . . yes O1 Na2 O2B 169.3(4) 2_656 . . yes O2B Na2 O4 103.1(3) . . . yes O4 Na2 O9 80.52(6) . . 1_455 yes O2B Na2 O9 116.2(4) . . 1_455 yes O2B Na2 O2W 87.1(3) . . 1_545 yes O1W Na2 O4 84.52(6) . . . yes O1W Na2 O2B 87.5(4) . . . yes O1W Na2 O2A 101.48(16) . . . yes O1 Na3 O4 98.56(5) . . 1_655 yes O1 Na3 O4 81.44(5) . . 2_656 yes O1 Na3 O9 97.10(5) 2_756 . 2_756 yes O4 Na3 O9 80.53(5) 2_656 . 2_756 yes O1 Na3 O9 97.10(5) . . . yes O1 Na3 O1 180.00 . . 2_756 yes O1 Na3 O9 82.91(5) . . 2_756 yes O1 Na3 O9 82.91(5) 2_756 . . yes O1 Na3 O4 81.44(5) 2_756 . 1_655 yes O4 Na3 O9 80.53(5) 1_655 . . yes O4 Na3 O9 99.47(5) 2_656 . . yes O1 Na3 O4 98.56(5) 2_756 . 2_656 yes O9 Na3 O9 180.00 . . 2_756 yes O4 Na3 O9 99.47(5) 1_655 . 2_756 yes O4 Na3 O4 180.00 1_655 . 2_656 yes O2W Na4 O7 168.06(7) . . 2_656 yes O2W Na4 O3 91.50(7) . . 2_666 yes O2W Na4 O7 91.91(6) . . 1_465 yes O2W Na4 O5 88.74(6) . . . yes O3 Na4 O7 123.65(6) 2_666 . 1_465 yes O5 Na4 O7 85.50(6) . . 1_465 yes O3 Na4 O5 150.80(7) 2_666 . . yes O5 Na4 O7 84.29(6) . . 2_656 yes O3 Na4 O7 89.91(6) 2_666 . 2_656 yes O7 Na4 O7 97.17(7) 1_465 . 2_656 yes S4 O1 Na1 91.58(8) . . . yes Na2 O1 Na3 83.81(5) 2_656 . . yes S4 O1 Na3 142.66(9) . . . yes Na1 O1 Na3 98.23(5) . . . yes Na1 O1 Na2 87.04(5) . . 2_656 yes S4 O1 Na2 132.86(8) . . 2_656 yes Na1 O1W Na2 92.69(6) 2_656 . . yes S4 O2 Na1 99.50(8) . . . yes Cl1A O2A Na2 172.3(4) . . . yes Cl1B O2B Na2 140.2(10) . . . yes Na2 O2W Na4 109.48(7) 1_565 . . yes S4 O3 Na4 125.97(9) . . 2_666 yes S5 O4 Na3 139.90(9) . . 1_455 yes S5 O4 Na2 130.83(10) . . . yes Na2 O4 Na3 84.35(5) . . 1_455 yes S5 O5 Na4 121.33(10) . . . yes S5 O6 Na1 153.69(10) . . . yes S5 O6 Na1 112.93(10) . . 2_656 yes Na1 O6 Na1 89.75(6) . . 2_656 yes Na4 O7 Na4 82.83(6) 1_645 . 2_656 yes S6 O7 Na4 143.56(10) . . 2_656 yes S6 O7 Na4 129.68(11) . . 1_645 yes S6 O8 Na1 127.68(9) . . . yes S6 O9 Na2 131.20(9) . . 1_655 yes Na2 O9 Na3 85.26(6) 1_655 . . yes S6 O9 Na3 135.89(9) . . . yes Na1 O1W H1WA 110(2) 2_656 . . no Na2 O1W H1WA 118.9(11) . . . no Na2 O1W H1WB 125.5(17) . . . no H1WA O1W H1WB 105(2) . . . no Na1 O1W H1WB 101.3(19) 2_656 . . no Na4 O2W H2WB 106.0(12) . . . no Na4 O2W H2WA 101.5(12) . . . no Na2 O2W H2WA 117.4(10) 1_565 . . no Na2 O2W H2WB 117.4(15) 1_565 . . no H2WA O2W H2WB 103.5(19) . . . no Cu1 N1 C2 106.81(13) . . . yes Cu1 N1 C4 108.88(13) . . . yes Cu1 N1 C6 105.77(12) . . . yes C4 N1 C6 112.06(18) . . . yes C2 N1 C4 111.26(18) . . . yes C2 N1 C6 111.7(2) . . . yes S1 C1 C2 114.43(17) . . . yes N1 C2 C1 113.20(19) . . . yes S2 C3 C4 113.68(13) . . . yes N1 C4 C3 112.50(19) . . . yes S3 C5 C6 113.76(18) . . . yes N1 C6 C5 112.03(18) . . . yes S1 C7 C8 109.92(13) . . . yes C7 C8 C9 113.22(16) . . . no S4 C9 C8 111.38(14) . . . yes S2 C10 C11 109.36(15) . . . yes C10 C11 C12 112.61(19) . . . no S5 C12 C11 112.96(15) . . . yes S3 C13 C14 108.86(15) . . . yes C13 C14 C15 111.10(19) . . . no S6 C15 C14 113.41(15) . . . yes C2 C1 H1B 109.0(15) . . . no H1A C1 H1B 111(2) . . . no S1 C1 H1A 103.5(17) . . . no S1 C1 H1B 108.3(17) . . . no C2 C1 H1A 110.2(18) . . . no C1 C2 H2A 107.1(17) . . . no N1 C2 H2A 106.7(18) . . . no N1 C2 H2B 108.5(19) . . . no C1 C2 H2B 108.9(18) . . . no H2A C2 H2B 113(2) . . . no S2 C3 H3B 108.8(15) . . . no S2 C3 H3A 104.9(17) . . . no H3A C3 H3B 109.2(19) . . . no C4 C3 H3A 111.3(14) . . . no C4 C3 H3B 108.8(16) . . . no C3 C4 H4B 109.6(16) . . . no H4A C4 H4B 103(2) . . . no C3 C4 H4A 109.8(13) . . . no N1 C4 H4A 108.4(12) . . . no N1 C4 H4B 113.3(19) . . . no S3 C5 H5B 105.6(16) . . . no S3 C5 H5A 101.8(17) . . . no H5A C5 H5B 108(2) . . . no C6 C5 H5A 114.0(15) . . . no C6 C5 H5B 112.7(18) . . . no C5 C6 H6B 112.6(19) . . . no N1 C6 H6A 109.6(15) . . . no N1 C6 H6B 107.6(16) . . . no C5 C6 H6A 110.2(15) . . . no H6A C6 H6B 105(2) . . . no H7A C7 H7B 117(2) . . . no S1 C7 H7B 110.8(11) . . . no S1 C7 H7A 105.4(16) . . . no C8 C7 H7A 107.7(17) . . . no C8 C7 H7B 106.4(12) . . . no C7 C8 H8B 109.2(15) . . . no C7 C8 H8A 106.5(14) . . . no H8A C8 H8B 108.1(16) . . . no C9 C8 H8A 111.7(14) . . . no C9 C8 H8B 108.0(15) . . . no C8 C9 H9B 116.4(16) . . . no S4 C9 H9A 104.9(16) . . . no S4 C9 H9B 104.9(16) . . . no C8 C9 H9A 113.7(16) . . . no H9A C9 H9B 105(2) . . . no S2 C10 H10A 106.6(15) . . . no S2 C10 H10B 114.6(18) . . . no H10A C10 H10B 106(2) . . . no C11 C10 H10B 109.4(15) . . . no C11 C10 H10A 110.7(14) . . . no C12 C11 H11A 105.8(14) . . . no C10 C11 H11B 110.0(19) . . . no C10 C11 H11A 112.1(14) . . . no C12 C11 H11B 107.5(16) . . . no H11A C11 H11B 108.7(18) . . . no H12A C12 H12B 104(2) . . . no S5 C12 H12A 106.9(15) . . . no S5 C12 H12B 109.1(17) . . . no C11 C12 H12A 109.6(14) . . . no C11 C12 H12B 113.8(17) . . . no S3 C13 H13B 105.7(16) . . . no C14 C13 H13A 111.6(19) . . . no S3 C13 H13A 109.4(17) . . . no H13A C13 H13B 107(2) . . . no C14 C13 H13B 114.0(14) . . . no C15 C14 H14A 110.2(14) . . . no C13 C14 H14B 111.2(18) . . . no C13 C14 H14A 108.2(13) . . . no C15 C14 H14B 110.0(18) . . . no H14A C14 H14B 106(2) . . . no H15A C15 H15B 111(2) . . . no S6 C15 H15A 106.9(16) . . . no S6 C15 H15B 103.3(14) . . . no C14 C15 H15A 111.2(15) . . . no C14 C15 H15B 110.8(17) . . . no loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag S2 Cu1 S1 C1 -102.11(9) . . . . no S2 Cu1 S1 C7 2.89(8) . . . . no S3 Cu1 S1 C1 81.88(9) . . . . no S3 Cu1 S1 C7 -173.12(7) . . . . no N1 Cu1 S1 C1 -11.10(10) . . . . no N1 Cu1 S1 C7 93.90(9) . . . . no S1 Cu1 S2 C3 79.28(9) . . . . no S1 Cu1 S2 C10 -177.02(7) . . . . no S3 Cu1 S2 C3 -104.25(9) . . . . no S3 Cu1 S2 C10 -0.55(8) . . . . no N1 Cu1 S2 C3 -12.87(10) . . . . no N1 Cu1 S2 C10 90.83(9) . . . . no S1 Cu1 S3 C5 -100.34(10) . . . . no S1 Cu1 S3 C13 3.91(9) . . . . no S2 Cu1 S3 C5 83.35(9) . . . . no S2 Cu1 S3 C13 -172.39(8) . . . . no N1 Cu1 S3 C5 -7.07(11) . . . . no N1 Cu1 S3 C13 97.19(10) . . . . no S1 Cu1 N1 C2 -12.06(14) . . . . no S1 Cu1 N1 C4 -132.30(14) . . . . no S1 Cu1 N1 C6 107.11(16) . . . . no S2 Cu1 N1 C2 109.37(14) . . . . no S2 Cu1 N1 C4 -10.87(14) . . . . no S2 Cu1 N1 C6 -131.47(16) . . . . no S3 Cu1 N1 C2 -137.64(14) . . . . no S3 Cu1 N1 C4 102.13(14) . . . . no S3 Cu1 N1 C6 -18.47(16) . . . . no Cu1 S1 C1 C2 35.20(19) . . . . no C7 S1 C1 C2 -73.0(2) . . . . no Cu1 S1 C7 C8 67.51(15) . . . . no C1 S1 C7 C8 166.13(15) . . . . no Cu1 S2 C3 C4 37.3(2) . . . . no C10 S2 C3 C4 -69.2(2) . . . . no Cu1 S2 C10 C11 103.14(17) . . . . no C3 S2 C10 C11 -158.62(17) . . . . no Cu1 S3 C5 C6 33.29(16) . . . . no C13 S3 C5 C6 -86.41(17) . . . . no Cu1 S3 C13 C14 79.94(19) . . . . no C5 S3 C13 C14 -179.19(19) . . . . no O1 S4 Na1 O2 164.78(10) . . . . no O1 S4 Na1 O6 166.45(9) . . . . no O1 S4 Na1 O8 -91.53(8) . . . . no O1 S4 Na1 O1W 74.21(8) . . . 2_656 no O1 S4 Na1 O6 4.63(11) . . . 2_656 no O2 S4 Na1 O1 -164.78(10) . . . . no O2 S4 Na1 O6 1.67(9) . . . . no O2 S4 Na1 O8 103.69(9) . . . . no O2 S4 Na1 O1W -90.57(9) . . . 2_656 no O2 S4 Na1 O6 -160.15(12) . . . 2_656 no O3 S4 Na1 O1 -86.50(13) . . . . no O3 S4 Na1 O2 78.28(14) . . . . no O3 S4 Na1 O6 79.95(13) . . . . no O3 S4 Na1 O8 -178.03(12) . . . . no O3 S4 Na1 O1W -12.29(13) . . . 2_656 no O3 S4 Na1 O6 -81.87(15) . . . 2_656 no C9 S4 Na1 O1 99.58(10) . . . . no C9 S4 Na1 O2 -95.64(10) . . . . no C9 S4 Na1 O6 -93.97(9) . . . . no C9 S4 Na1 O8 8.05(9) . . . . no C9 S4 Na1 O1W 173.80(8) . . . 2_656 no C9 S4 Na1 O6 104.21(12) . . . 2_656 no Na1 S4 O1 Na3 105.79(15) . . . . no Na1 S4 O1 Na2 -87.42(12) . . . 2_656 no O2 S4 O1 Na1 12.65(9) . . . . no O2 S4 O1 Na3 118.44(15) . . . . no O2 S4 O1 Na2 -74.77(13) . . . 2_656 no O3 S4 O1 Na1 139.89(8) . . . . no O3 S4 O1 Na3 -114.32(15) . . . . no O3 S4 O1 Na2 52.47(15) . . . 2_656 no C9 S4 O1 Na1 -102.17(8) . . . . no C9 S4 O1 Na3 3.62(18) . . . . no C9 S4 O1 Na2 170.40(11) . . . 2_656 no O1 S4 O2 Na1 -13.88(9) . . . . no O3 S4 O2 Na1 -140.30(8) . . . . no C9 S4 O2 Na1 101.97(8) . . . . no Na1 S4 O3 Na4 82.81(16) . . . 2_666 no O1 S4 O3 Na4 14.80(15) . . . 2_666 no O2 S4 O3 Na4 139.90(11) . . . 2_666 no C9 S4 O3 Na4 -103.22(12) . . . 2_666 no Na1 S4 C9 C8 100.82(13) . . . . no O1 S4 C9 C8 163.68(13) . . . . no O2 S4 C9 C8 46.42(15) . . . . no O3 S4 C9 C8 -75.37(16) . . . . no O5 S5 O4 Na2 159.39(10) . . . . no O5 S5 O4 Na3 -55.11(16) . . . 1_455 no O6 S5 O4 Na2 -72.65(13) . . . . no O6 S5 O4 Na3 72.86(16) . . . 1_455 no C12 S5 O4 Na2 42.06(14) . . . . no C12 S5 O4 Na3 -172.44(13) . . . 1_455 no O4 S5 O5 Na4 125.20(11) . . . . no O6 S5 O5 Na4 -1.96(14) . . . . no C12 S5 O5 Na4 -116.81(11) . . . . no O4 S5 O6 Na1 146.6(2) . . . . no O4 S5 O6 Na1 -1.07(12) . . . 2_656 no O5 S5 O6 Na1 -85.7(2) . . . . no O5 S5 O6 Na1 126.64(9) . . . 2_656 no C12 S5 O6 Na1 30.2(2) . . . . no C12 S5 O6 Na1 -117.51(9) . . . 2_656 no O4 S5 C12 C11 77.13(16) . . . . no O5 S5 C12 C11 -43.88(18) . . . . no O6 S5 C12 C11 -163.98(15) . . . . no O8 S6 O7 Na4 -162.19(10) . . . 1_645 no O8 S6 O7 Na4 -13.92(19) . . . 2_656 no O9 S6 O7 Na4 -33.92(14) . . . 1_645 no O9 S6 O7 Na4 114.36(17) . . . 2_656 no C15 S6 O7 Na4 81.37(13) . . . 1_645 no C15 S6 O7 Na4 -130.35(16) . . . 2_656 no O7 S6 O8 Na1 95.37(12) . . . . no O9 S6 O8 Na1 -33.31(13) . . . . no C15 S6 O8 Na1 -147.03(10) . . . . no O7 S6 O9 Na3 -71.68(14) . . . . no O7 S6 O9 Na2 66.52(13) . . . 1_655 no O8 S6 O9 Na3 56.83(15) . . . . no O8 S6 O9 Na2 -164.97(10) . . . 1_655 no C15 S6 O9 Na3 171.22(12) . . . . no C15 S6 O9 Na2 -50.58(13) . . . 1_655 no O7 S6 C15 C14 54.53(17) . . . . no O8 S6 C15 C14 -66.21(16) . . . . no O9 S6 C15 C14 175.06(14) . . . . no S4 Na1 O1 Na3 -143.86(10) . . . . no S4 Na1 O1 Na2 132.83(8) . . . 2_656 no O2 Na1 O1 S4 -8.63(6) . . . . no O2 Na1 O1 Na3 -152.49(8) . . . . no O2 Na1 O1 Na2 124.21(7) . . . 2_656 no O6 Na1 O1 S4 -22.97(15) . . . . no O6 Na1 O1 Na3 -166.83(10) . . . . no O6 Na1 O1 Na2 109.87(11) . . . 2_656 no O8 Na1 O1 S4 96.22(7) . . . . no O8 Na1 O1 Na3 -47.64(7) . . . . no O8 Na1 O1 Na2 -130.95(5) . . . 2_656 no O1W Na1 O1 S4 -103.19(7) 2_656 . . . no O1W Na1 O1 Na3 112.95(6) 2_656 . . . no O1W Na1 O1 Na2 29.64(5) 2_656 . . 2_656 no O6 Na1 O1 S4 -177.15(7) 2_656 . . . no O6 Na1 O1 Na3 39.00(8) 2_656 . . . no O6 Na1 O1 Na2 -44.31(7) 2_656 . . 2_656 no O1 Na1 O2 S4 8.73(6) . . . . no O6 Na1 O2 S4 -178.57(8) . . . . no O8 Na1 O2 S4 -85.48(9) . . . . no O1W Na1 O2 S4 88.81(8) 2_656 . . . no S4 Na1 O6 S5 39.3(3) . . . . no S4 Na1 O6 Na1 -170.22(4) . . . 2_656 no O1 Na1 O6 S5 52.1(3) . . . . no O1 Na1 O6 Na1 -157.38(10) . . . 2_656 no O2 Na1 O6 S5 40.1(2) . . . . no O2 Na1 O6 Na1 -169.41(6) . . . 2_656 no O8 Na1 O6 S5 -69.9(2) . . . . no O8 Na1 O6 Na1 80.58(6) . . . 2_656 no O1W Na1 O6 S5 129.2(2) 2_656 . . . no O1W Na1 O6 Na1 -80.28(6) 2_656 . . 2_656 no O6 Na1 O6 S5 -150.5(2) 2_656 . . . no O6 Na1 O6 Na1 0.00(7) 2_656 . . 2_656 no S4 Na1 O8 S6 67.85(11) . . . . no O1 Na1 O8 S6 37.81(12) . . . . no O2 Na1 O8 S6 97.62(11) . . . . no O6 Na1 O8 S6 -168.78(11) . . . . no O6 Na1 O8 S6 -78.86(12) 2_656 . . . no S4 Na1 O1W Na2 -59.39(4) . . 2_656 2_656 no O1 Na1 O1W Na2 -31.15(5) . . 2_656 2_656 no O2 Na1 O1W Na2 -88.12(6) . . 2_656 2_656 no O6 Na1 O1W Na2 179.22(6) . . 2_656 2_656 no S4 Na1 O6 S5 -1.73(16) . . 2_656 2_656 no S4 Na1 O6 Na1 164.56(7) . . 2_656 2_656 no O1 Na1 O6 S5 0.81(12) . . 2_656 2_656 no O1 Na1 O6 Na1 167.11(5) . . 2_656 2_656 no O6 Na1 O6 S5 -166.29(9) . . 2_656 2_656 no O6 Na1 O6 Na1 0.02(9) . . 2_656 2_656 no O8 Na1 O6 S5 101.74(10) . . 2_656 2_656 no O8 Na1 O6 Na1 -91.97(6) . . 2_656 2_656 no O2A Na2 O1W Na1 156.25(14) . . . 2_656 no O4 Na2 O1W Na1 47.81(6) . . . 2_656 no O9 Na2 O1W Na1 -6.80(16) 1_455 . . 2_656 no O2W Na2 O1W Na1 -122.24(6) 1_545 . . 2_656 no O1 Na2 O1W Na1 -31.55(5) 2_656 . . 2_656 no O1W Na2 O4 S5 37.28(12) . . . . no O1W Na2 O4 Na3 -121.21(5) . . . 1_455 no O2A Na2 O4 S5 -63.0(2) . . . . no O2A Na2 O4 Na3 138.52(17) . . . 1_455 no O9 Na2 O4 S5 -163.79(12) 1_455 . . . no O1 Na2 O4 S5 120.32(12) 2_656 . . . no O1W Na2 O9 S6 -137.87(13) . . 1_455 1_455 no O2A Na2 O9 S6 59.20(18) . . 1_455 1_455 no O4 Na2 O9 S6 166.77(12) . . 1_455 1_455 no O1W Na2 O2W Na4 110.87(8) . . 1_545 1_545 no O2A Na2 O2W Na4 -149.33(17) . . 1_545 1_545 no O1W Na2 O1 S4 -59.67(13) . . 2_656 2_656 no O1W Na2 O1 Na1 29.73(5) . . 2_656 2_656 no O4 Na2 O1 S4 -145.61(13) . . 2_656 2_656 no O4 Na2 O1 Na1 -56.20(6) . . 2_656 2_656 no O9 Na3 O1 S4 -52.15(16) . . . . no O9 Na3 O1 Na1 51.46(6) . . . . no O9 Na3 O1 Na2 137.55(5) . . . 2_656 no O4 Na3 O1 S4 29.28(16) 1_655 . . . no O4 Na3 O1 Na1 132.90(5) 1_655 . . . no O4 Na3 O1 S4 -150.72(16) 2_656 . . . no O4 Na3 O1 Na1 -47.10(5) 2_656 . . . no O9 Na3 O1 S4 127.85(16) 2_756 . . . no O9 Na3 O1 Na1 -128.54(6) 2_756 . . . no O1 Na3 O9 S6 -74.59(13) . . . . no O1 Na3 O9 Na2 135.62(5) . . . 1_655 no O4 Na3 O9 S6 -172.14(13) 1_655 . . . no O4 Na3 O9 S6 7.86(13) 2_656 . . . no O1 Na3 O9 S6 105.41(13) 2_756 . . . no O5 Na4 O2W Na2 147.90(8) . . . 1_565 no O7 Na4 O2W Na2 62.44(8) 1_465 . . 1_565 no O3 Na4 O2W Na2 -61.31(8) 2_666 . . 1_565 no O2W Na4 O5 S5 94.42(11) . . . . no O7 Na4 O5 S5 -173.57(11) 1_465 . . . no O7 Na4 O5 S5 -75.88(11) 2_656 . . . no O3 Na4 O5 S5 3.6(2) 2_666 . . . no O2W Na4 O7 S6 -26.11(12) . . 1_465 1_465 no O5 Na4 O7 S6 -114.70(12) . . 1_465 1_465 no O5 Na4 O7 S6 71.21(17) . . 2_656 2_656 no O2W Na4 O3 S4 68.40(12) . . 2_666 2_666 no O5 Na4 O3 S4 158.50(12) . . 2_666 2_666 no Cu1 N1 C2 C1 37.5(2) . . . . no C4 N1 C2 C1 156.24(19) . . . . no C6 N1 C2 C1 -77.7(2) . . . . no Cu1 N1 C4 C3 37.4(2) . . . . no C2 N1 C4 C3 -80.0(2) . . . . no C6 N1 C4 C3 154.1(2) . . . . no Cu1 N1 C6 C5 44.2(2) . . . . no C2 N1 C6 C5 160.08(19) . . . . no C4 N1 C6 C5 -74.3(2) . . . . no S1 C1 C2 N1 -52.7(3) . . . . no S2 C3 C4 N1 -53.6(3) . . . . no S3 C5 C6 N1 -55.9(2) . . . . no S1 C7 C8 C9 59.3(2) . . . . no C7 C8 C9 S4 -178.41(13) . . . . no S2 C10 C11 C12 -53.9(2) . . . . no C10 C11 C12 S5 169.34(17) . . . . no S3 C13 C14 C15 -82.5(2) . . . . no C13 C14 C15 S6 151.88(16) . . . . no loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag O2W H2WA O2 0.993(16) 1.696(17) 2.664(2) 163.9(19) . yes O1W H1WA O3 0.993(16) 1.779(13) 2.758(2) 168(2) 1_545 yes O1W H1WB O8 0.99(3) 2.05(2) 2.932(2) 147(3) . yes C1 H1B O10 0.94(2) 2.46(2) 3.349(6) 158(2) 2_765 yes C5 H5B O10 0.940(13) 2.56(2) 3.256(5) 132(2) 1_545 yes C6 H6B O3A 0.941(9) 2.514(10) 3.439(4) 168(2) 2_655 yes C8 H8B O2 0.942(17) 2.57(3) 2.953(3) 104.8(18) . yes C9 H9A S1 0.939(8) 2.81(3) 3.164(2) 103.5(17) . yes C10 H10A O11 0.94(2) 2.44(2) 3.362(6) 166.8(19) 1_455 yes C10 H10A O10 0.94(2) 2.59(2) 3.453(6) 153(2) 2_665 yes C10 H10B O3A 0.941(14) 2.41(2) 3.229(5) 145(2) . yes C11 H11A O5 0.940(14) 2.50(2) 2.977(3) 111.9(15) . yes C12 H12A S2 0.94(2) 2.59(2) 3.080(2) 113.2(18) . yes data_14a _audit_creation_date 2013-07-02 _audit_creation_method ; Olex2 1.2-beta (compiled Nov 5 2012 18:25:38, GUI svn.r4372) ; _publ_section_references ; Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122 Petricek,V., Dusek,M. & Palatinus,L.(2006). Jana2006. The crystallographic computing system. Institute of Physics, Praha, Czech Republic. Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. Bruker (2011). APEX2 Version 2011.2-4. Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2009). SAINT-Plus Version 7.68a. Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (2008). SADABS Version 2008-1. Bruker AXS Inc., Madison, Wisconsin, USA. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C36 H96 Cu2 N2 Na6 O30 S12, 2(F6 P), 3(H2 O)' _chemical_formula_sum 'C36 H102 Cu2 F12 N2 Na6 O33 P2 S12' _chemical_formula_weight 2030.87 _chemical_melting_point ? 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' 'Cu' 'Cu' 0.3201 1.2651 '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' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Na' 'Na' 0.0362 0.0249 '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' _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.8551(17) _cell_length_b 11.9311(17) _cell_length_c 32.214(5) _cell_angle_alpha 91.273(2) _cell_angle_beta 98.023(2) _cell_angle_gamma 119.384(2) _cell_volume 3909.7(10) _cell_formula_units_Z 2 _cell_measurement_reflns_used 9918 _cell_measurement_temperature 173(2) _cell_measurement_theta_max 32.08 _cell_measurement_theta_min 2.18 _exptl_absorpt_coefficient_mu 1.047 _exptl_absorpt_correction_T_max 0.8602 _exptl_absorpt_correction_T_min 0.6223 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0547 before and 0.0411 after correction. The Ratio of minimum to maximum transmission is 0.7234. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.725 _exptl_crystal_density_meas . _exptl_crystal_density_method ? _exptl_crystal_description prism _exptl_crystal_F_000 2100 _exptl_crystal_size_max 0.783 _exptl_crystal_size_mid 0.451 _exptl_crystal_size_min 0.316 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_unetI/netI 0.0399 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.927 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_limit_l_min -45 _diffrn_reflns_number 50063 _diffrn_reflns_point_group_measured_fraction_full 0.997 _diffrn_reflns_point_group_measured_fraction_max 0.927 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 32.106 _diffrn_reflns_theta_min 1.284 _diffrn_ambient_temperature 173(2) _diffrn_detector_area_resol_mean 512 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.927 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\w scans with a narrow frame width' _diffrn_radiation_monochromator 'graphite' _diffrn_radiation_type 'MoK\a' _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 19582 _reflns_number_total 25380 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT v7.68A (Bruker, 2009)' _computing_data_collection 'APEX2 v2011.2-4 (Bruker, 2011)' _computing_data_reduction 'SAINT v8.27A (Bruker, 2012)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement ; SHELXL, G.M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _computing_structure_solution 'SUPERFLIP, J. Appl. Cryst. (2007) 40, 786-790' _refine_diff_density_max 1.934 _refine_diff_density_min -1.296 _refine_diff_density_rms 0.117 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment refxyz _refine_ls_matrix_type full _refine_ls_number_parameters 1277 _refine_ls_number_reflns 25380 _refine_ls_number_restraints 52 _refine_ls_R_factor_all 0.0631 _refine_ls_R_factor_gt 0.0484 _refine_ls_restrained_S_all 6.452 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0690P)^2^+3.0344P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1243 _refine_ls_wR_factor_ref 0.1340 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups 2. Restrained distances O15W-H15A = O15W-H15B 0.99 with sigma of 0.01 H15B-H15A 1.585 with sigma of 0.01 O5W-H5WA = O5W-H5WB 0.99 with sigma of 0.01 H5WA-H5WB 1.585 with sigma of 0.01 O13W-H13B = O13W-H13A 0.99 with sigma of 0.01 H13B-H13A 1.585 with sigma of 0.01 O2W-H2WB = O2W-H2WA 0.99 with sigma of 0.01 H2WB-H2WA 1.585 with sigma of 0.01 O12W-H12A = O12W-H12B 0.99 with sigma of 0.01 H12A-H12B 1.585 with sigma of 0.01 O14W-H14E = O14W-H14F 0.99 with sigma of 0.01 H14F-H14E 1.585 with sigma of 0.01 O7W-H7WB = O7W-H7WA 0.99 with sigma of 0.01 H7WB-H7WA 1.585 with sigma of 0.01 O1W-H1WA = O1W-H1WB 0.99 with sigma of 0.01 H1WB-H1WA 1.585 with sigma of 0.01 O11W-H11B = O11W-H11A 0.99 with sigma of 0.01 H11B-H11A 1.585 with sigma of 0.01 O4W-H4WA 0.99 with sigma of 0.01 O4W-H4WB 0.99 with sigma of 0.01 H4WA-H4WB 1.59 with sigma of 0.01 O7B-H4WB 1.92 with sigma of 0.01 O6-H4WA 1.77 with sigma of 0.01 O3W-H3WA 0.99 with sigma of 0.01 H3WA-Na2 2.75 with sigma of 0.01 O3W-H3WA 0.99 with sigma of 0.01 O6W-H6WB = O6W-H6WA 0.99 with sigma of 0.01 H6WA-H6WB 1.585 with sigma of 0.01 O3W-H3WB 0.99 with sigma of 0.01 H3WA-H3WB 1.585 with sigma of 0.01 Na1-H3WB 2.7 with sigma of 0.01 O2B-H6WA 1.733 with sigma of 0.02 H3WB_$4-H3WB_$3 1.99 with sigma of 0.01 O8W-H8WA 0.985 with sigma of 0.01 O8W-H8WB 0.985 with sigma of 0.01 H8WB-H8WA 1.555 with sigma of 0.01 O10W-H10B = O10W-H10A 0.99 with sigma of 0.01 H10B-H10A 1.585 with sigma of 0.01 O9W-H9WA = O9W-H9WB 0.985 with sigma of 0.01 H9WA-H9WB 1.555 with sigma of 0.01 3. Uiso/Uaniso restraints and constraints Uiso(H3WB) = Uiso(H3WA) Uiso(H9WA) = Uiso(H9WB) 4. Others Fixed Uiso: H6WA(0.02018) H6WB(0.02018) H9WA(0.02296) H9WB(0.02296) ; _atom_sites_solution_hydrogens difmap _atom_sites_solution_primary iterative _atom_sites_solution_secondary ? 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu -0.32201(2) -0.16242(2) 0.02334(2) 0.01471(6) Uani 1 1 d . . . . . Cu1B Cu 0.31959(2) 0.16033(2) 0.47736(2) 0.01434(6) Uani 1 1 d . . . . . S1 S -0.49975(5) -0.14273(5) 0.03227(2) 0.01515(9) Uani 1 1 d . . . . . S4 S -0.49637(5) -0.39052(5) 0.17614(2) 0.01463(9) Uani 1 1 d . . . . . S5 S 0.03970(5) -0.06976(5) 0.17399(2) 0.01546(9) Uani 1 1 d . . . . . S6B S -0.04251(5) 0.06823(5) 0.32590(2) 0.01663(9) Uani 1 1 d . . . . . S3B S 0.32329(5) 0.35151(5) 0.46728(2) 0.01529(9) Uani 1 1 d . . . . . S1B S 0.49912(5) 0.14616(5) 0.46593(2) 0.01486(9) Uani 1 1 d . . . . . S4B S 0.47299(5) 0.40633(5) 0.32892(2) 0.01592(9) Uani 1 1 d . . . . . S2B S 0.12087(5) -0.02684(5) 0.46656(2) 0.01471(9) Uani 1 1 d . . . . . S2 S -0.33165(5) -0.35545(5) 0.03462(2) 0.01541(9) Uani 1 1 d . . . . . S3 S -0.12057(5) 0.02145(5) 0.03465(2) 0.01518(9) Uani 1 1 d . . . . . S6 S -0.28785(5) 0.14350(5) 0.17265(2) 0.01632(9) Uani 1 1 d . . . . . S5B S 0.29525(5) -0.13434(5) 0.32877(2) 0.01737(10) Uani 1 1 d . . . . . Na3 Na -0.21851(9) -0.09476(9) 0.22723(3) 0.02332(18) Uani 1 1 d . . . . . Na5 Na 0.30654(9) -0.08671(9) 0.23072(3) 0.02051(17) Uani 1 1 d . . . . . Na4 Na 0.22466(9) 0.09966(8) 0.28279(3) 0.02078(17) Uani 1 1 d . . . . . Na1 Na 0.31339(10) 0.38029(9) 0.24210(3) 0.02472(19) Uani 1 1 d D . . . . Na6 Na -0.28882(10) -0.40393(9) 0.26062(3) 0.0271(2) Uani 1 1 d . . . . . Na2 Na 0.35977(12) 0.68473(10) 0.25236(3) 0.0335(2) Uani 1 1 d D . . . . O3B O 0.33387(15) 0.30978(15) 0.31754(5) 0.0219(3) Uani 1 1 d . . . . . O3 O -0.56886(17) -0.42847(15) 0.21159(5) 0.0223(3) Uani 1 1 d . . . . . O1 O -0.35745(15) -0.29861(16) 0.19029(5) 0.0241(3) Uani 1 1 d . . . . . O6 O -0.04686(15) -0.01895(15) 0.18187(5) 0.0202(3) Uani 1 1 d D . . . . O5 O 0.10853(15) -0.08273(16) 0.21368(5) 0.0210(3) Uani 1 1 d . . . . . O5B O 0.2518(2) -0.2300(2) 0.29255(6) 0.0372(5) Uani 1 1 d . . . . . O6B O 0.40782(16) -0.12251(17) 0.35781(5) 0.0238(3) Uani 1 1 d . . . . . O4B O 0.32002(18) -0.00994(19) 0.31515(6) 0.0327(4) Uani 1 1 d . . . . . O9B O 0.04378(15) 0.01463(15) 0.32121(5) 0.0210(3) Uani 1 1 d . . . . . O7B O -0.10080(16) 0.08512(16) 0.28509(5) 0.0226(3) Uani 1 1 d D . . . . O8B O -0.14211(15) -0.00842(16) 0.35131(5) 0.0233(3) Uani 1 1 d . . . . . O1B O 0.53003(17) 0.45215(17) 0.29118(5) 0.0267(4) Uani 1 1 d . . . . . O10W O -0.0897(2) -0.20776(19) 0.26141(6) 0.0392(5) Uani 1 1 d D . . . . O9W O -0.3057(2) -0.2234(2) 0.28991(7) 0.0449(5) Uani 1 1 d D . . A 2 O13W O -0.3204(3) -0.5457(2) 0.20200(7) 0.0497(6) Uani 1 1 d D . . . . O12W O -0.16372(18) -0.49382(17) 0.29639(6) 0.0289(4) Uani 1 1 d D . . . . O3W O 0.2075(2) 0.47961(19) 0.27263(7) 0.0406(5) Uani 1 1 d D . . . . O4W O 0.11173(17) 0.19651(16) 0.23931(5) 0.0265(3) Uani 1 1 d D . . . . O1W O 0.32221(19) 0.26735(17) 0.18179(5) 0.0296(4) Uani 1 1 d D . . . . O2B O 0.49484(18) 0.51124(16) 0.35907(5) 0.0265(3) Uani 1 1 d D . . . . O5W O 0.40059(16) 0.14760(16) 0.24446(5) 0.0239(3) Uani 1 1 d D . . . . O15W O 0.50719(16) -0.09488(16) 0.24626(5) 0.0231(3) Uani 1 1 d D . . . . O11W O 0.19473(18) -0.31351(17) 0.20307(6) 0.0303(4) Uani 1 1 d D . . . . O6W O 0.4597(2) 0.6923(2) 0.31979(6) 0.0418(5) Uani 1 1 d D . . . . O2W O 0.34739(18) -0.05372(18) 0.16152(6) 0.0287(4) Uani 1 1 d D . . . . O4 O 0.13038(15) 0.00603(16) 0.14602(5) 0.0228(3) Uani 1 1 d . . . . . O7 O -0.31225(16) 0.02397(16) 0.19114(5) 0.0223(3) Uani 1 1 d . . . . . O9 O -0.23932(18) 0.25250(16) 0.20516(5) 0.0269(4) Uani 1 1 d . . . . . O8 O -0.40107(16) 0.12677(18) 0.14322(5) 0.0260(3) Uani 1 1 d . . . . . O2 O -0.51694(15) -0.50236(14) 0.14960(5) 0.0195(3) Uani 1 1 d . . . . . N1B N 0.35656(16) 0.18247(16) 0.54433(5) 0.0147(3) Uani 1 1 d . . . . . N1 N -0.35615(16) -0.18469(16) -0.04369(5) 0.0144(3) Uani 1 1 d . . . . . C12 C -0.5639(2) -0.3111(2) 0.14470(7) 0.0168(4) Uani 1 1 d . . . . . H12C H -0.652(3) -0.367(3) 0.1403(9) 0.020 Uiso 1 1 d . U . . . H12D H -0.555(3) -0.241(3) 0.1616(9) 0.020 Uiso 1 1 d . U . . . C11 C -0.5080(2) -0.2746(2) 0.10417(6) 0.0173(4) Uani 1 1 d . . . . . H11C H -0.537(3) -0.351(3) 0.0872(9) 0.021 Uiso 1 1 d . U . . . H11D H -0.414(3) -0.238(3) 0.1109(9) 0.021 Uiso 1 1 d . U . . . C10 C -0.5494(2) -0.1838(2) 0.08320(6) 0.0173(4) Uani 1 1 d . . . . . H10C H -0.511(3) -0.101(3) 0.1008(9) 0.021 Uiso 1 1 d . U . . . H10D H -0.643(3) -0.217(3) 0.0808(9) 0.021 Uiso 1 1 d . U . . . C18B C 0.0578(2) 0.2237(2) 0.35382(7) 0.0186(4) Uani 1 1 d . . . . . H18A H 0.119(3) 0.274(3) 0.3379(9) 0.022 Uiso 1 1 d . U . . . H18B H -0.001(3) 0.258(3) 0.3569(9) 0.022 Uiso 1 1 d . U . . . C17B C 0.1262(2) 0.2171(2) 0.39687(7) 0.0193(4) Uani 1 1 d . . . . . H17A H 0.063(3) 0.179(3) 0.4145(9) 0.023 Uiso 1 1 d . U . . . H17B H 0.154(3) 0.158(3) 0.3925(9) 0.023 Uiso 1 1 d . U . . . C16B C 0.2354(2) 0.3508(2) 0.41623(7) 0.0170(4) Uani 1 1 d . . . . . H16A H 0.202(3) 0.402(3) 0.4204(9) 0.020 Uiso 1 1 d . U . . . H16B H 0.302(3) 0.387(3) 0.3982(9) 0.020 Uiso 1 1 d . U . . . C10B C 0.5450(2) 0.1919(2) 0.41473(7) 0.0165(4) Uani 1 1 d . . . . . H10E H 0.633(3) 0.223(3) 0.4169(9) 0.020 Uiso 1 1 d . U . . . H10F H 0.504(3) 0.113(3) 0.3970(9) 0.020 Uiso 1 1 d . U . . . C11B C 0.5011(2) 0.2837(2) 0.39650(7) 0.0181(4) Uani 1 1 d . . . . . H11E H 0.529(3) 0.353(3) 0.4157(9) 0.022 Uiso 1 1 d . U . . . H11F H 0.399(3) 0.237(3) 0.3901(9) 0.022 Uiso 1 1 d . U . . . C12B C 0.5507(2) 0.3268(2) 0.35531(7) 0.0190(4) Uani 1 1 d . . . . . H12E H 0.535(3) 0.260(3) 0.3335(9) 0.023 Uiso 1 1 d . U . . . H12F H 0.634(3) 0.384(3) 0.3584(9) 0.023 Uiso 1 1 d . U . . . C1B C 0.6219(2) 0.2890(2) 0.50079(7) 0.0192(4) Uani 1 1 d . . . . . H1BA H 0.703(3) 0.301(3) 0.4983(9) 0.023 Uiso 1 1 d . U . . . H1BB H 0.611(3) 0.359(3) 0.4923(9) 0.023 Uiso 1 1 d . U . . . C2B C 0.6047(2) 0.2697(2) 0.54660(7) 0.0198(4) Uani 1 1 d . . . . . H2BA H 0.684(3) 0.332(3) 0.5629(9) 0.024 Uiso 1 1 d . U . . . H2BB H 0.594(3) 0.191(3) 0.5530(9) 0.024 Uiso 1 1 d . U . . . C3B C 0.4950(2) 0.2855(2) 0.56075(7) 0.0187(4) Uani 1 1 d . . . . . H3BA H 0.509(3) 0.295(3) 0.5913(9) 0.022 Uiso 1 1 d . U . . . H3BB H 0.506(3) 0.364(3) 0.5514(9) 0.022 Uiso 1 1 d . U . . . C9B C 0.2678(2) 0.2201(2) 0.56185(7) 0.0192(4) Uani 1 1 d . . . . . H9BA H 0.291(3) 0.229(3) 0.5904(10) 0.023 Uiso 1 1 d . U . . . H9BB H 0.183(3) 0.149(3) 0.5554(9) 0.023 Uiso 1 1 d . U . . . C8B C 0.2689(2) 0.3422(2) 0.54803(7) 0.0203(4) Uani 1 1 d . . . . . H8BA H 0.357(3) 0.414(3) 0.5536(9) 0.024 Uiso 1 1 d . U . . . H8BB H 0.214(3) 0.356(3) 0.5644(9) 0.024 Uiso 1 1 d . U . . . C7B C 0.2088(2) 0.3348(2) 0.50217(7) 0.0192(4) Uani 1 1 d . . . . . H7BA H 0.192(3) 0.400(3) 0.5015(9) 0.023 Uiso 1 1 d . U . . . H7BB H 0.127(3) 0.257(3) 0.4934(9) 0.023 Uiso 1 1 d . U . . . C6B C 0.3362(2) 0.0602(2) 0.56150(7) 0.0189(4) Uani 1 1 d . . . . . H6BA H 0.352(3) 0.078(3) 0.5919(9) 0.023 Uiso 1 1 d . U . . . H6BB H 0.406(3) 0.051(3) 0.5537(9) 0.023 Uiso 1 1 d . U . . . C5B C 0.2019(2) -0.0608(2) 0.54762(7) 0.0200(4) Uani 1 1 d . . . . . H5BA H 0.199(3) -0.128(3) 0.5632(9) 0.024 Uiso 1 1 d . U . . . H5BB H 0.134(3) -0.045(3) 0.5529(9) 0.024 Uiso 1 1 d . U . . . C4B C 0.1712(2) -0.1180(2) 0.50188(7) 0.0193(4) Uani 1 1 d . . . . . H4BA H 0.103(3) -0.203(3) 0.4995(9) 0.023 Uiso 1 1 d . U . . . H4BB H 0.249(3) -0.115(3) 0.4936(9) 0.023 Uiso 1 1 d . U . . . C13B C 0.0814(2) -0.1201(2) 0.41601(7) 0.0170(4) Uani 1 1 d . . . . . H13C H 0.031(3) -0.208(3) 0.4192(9) 0.020 Uiso 1 1 d . U . . . H13D H 0.026(3) -0.101(3) 0.3970(9) 0.020 Uiso 1 1 d . U . . . C14B C 0.2011(2) -0.0938(2) 0.39677(7) 0.0178(4) Uani 1 1 d . . . . . H14A H 0.261(3) -0.102(3) 0.4164(9) 0.021 Uiso 1 1 d . U . . . H14B H 0.239(3) -0.013(3) 0.3890(9) 0.021 Uiso 1 1 d . U . . . C15B C 0.1644(2) -0.1870(2) 0.35762(7) 0.0180(4) Uani 1 1 d . . . . . H15C H 0.090(3) -0.193(3) 0.3388(9) 0.022 Uiso 1 1 d . U . . . H15D H 0.147(3) -0.270(3) 0.3638(9) 0.022 Uiso 1 1 d . U . . . C15 C -0.0645(2) -0.2273(2) 0.14773(7) 0.0174(4) Uani 1 1 d . . . . . H15E H -0.008(3) -0.264(3) 0.1454(9) 0.021 Uiso 1 1 d . U . . . H15F H -0.124(3) -0.276(3) 0.1644(9) 0.021 Uiso 1 1 d . U . . . C14 C -0.1349(2) -0.2219(2) 0.10490(7) 0.0187(4) Uani 1 1 d . . . . . H14C H -0.164(3) -0.160(3) 0.1106(9) 0.022 Uiso 1 1 d . U . . . H14D H -0.070(3) -0.187(3) 0.0856(9) 0.022 Uiso 1 1 d . U . . . C13 C -0.2465(2) -0.3550(2) 0.08625(6) 0.0163(4) Uani 1 1 d . . . . . H13E H -0.310(3) -0.385(3) 0.1036(9) 0.020 Uiso 1 1 d . U . . . H13F H -0.216(3) -0.411(3) 0.0828(9) 0.020 Uiso 1 1 d . U . . . C4 C -0.2161(2) -0.3423(2) 0.00067(7) 0.0198(4) Uani 1 1 d . . . . . H4A H -0.135(3) -0.263(3) 0.0088(9) 0.024 Uiso 1 1 d . U . . . H4B H -0.199(3) -0.407(3) 0.0031(9) 0.024 Uiso 1 1 d . U . . . C5 C -0.2729(2) -0.3482(2) -0.04556(7) 0.0206(4) Uani 1 1 d . . . . . H5A H -0.215(3) -0.362(3) -0.0616(9) 0.025 Uiso 1 1 d . U . . . H5B H -0.359(3) -0.419(3) -0.0502(9) 0.025 Uiso 1 1 d . U . . . C6 C -0.2665(2) -0.2239(2) -0.05972(7) 0.0198(4) Uani 1 1 d . . . . . H6A H -0.177(3) -0.152(3) -0.0505(9) 0.024 Uiso 1 1 d . U . . . H6B H -0.284(3) -0.230(3) -0.0898(10) 0.024 Uiso 1 1 d . U . . . C3 C -0.4943(2) -0.2855(2) -0.06155(7) 0.0194(4) Uani 1 1 d . . . . . H3A H -0.507(3) -0.370(3) -0.0524(9) 0.023 Uiso 1 1 d . U . . . H3B H -0.508(3) -0.295(3) -0.0927(9) 0.023 Uiso 1 1 d . U . . . C2 C -0.6037(2) -0.2677(2) -0.04826(7) 0.0199(4) Uani 1 1 d . . . . . H2A H -0.679(3) -0.329(3) -0.0652(9) 0.024 Uiso 1 1 d . U . . . H2B H -0.591(3) -0.186(3) -0.0542(9) 0.024 Uiso 1 1 d . U . . . C1 C -0.6225(2) -0.2861(2) -0.00239(7) 0.0192(4) Uani 1 1 d . . . . . H1A H -0.614(3) -0.362(3) 0.0061(9) 0.023 Uiso 1 1 d . U . . . H1B H -0.705(3) -0.300(3) -0.0008(9) 0.023 Uiso 1 1 d . U . . . C9 C -0.3318(2) -0.0614(2) -0.06083(7) 0.0193(4) Uani 1 1 d . . . . . H9A H -0.395(3) -0.044(3) -0.0515(9) 0.023 Uiso 1 1 d . U . . . H9B H -0.353(3) -0.082(3) -0.0911(10) 0.023 Uiso 1 1 d . U . . . C8 C -0.1967(2) 0.0579(2) -0.04660(7) 0.0199(4) Uani 1 1 d . . . . . H8A H -0.193(3) 0.126(3) -0.0632(9) 0.024 Uiso 1 1 d . U . . . H8B H -0.133(3) 0.041(3) -0.0507(9) 0.024 Uiso 1 1 d . U . . . C7 C -0.1658(2) 0.1152(2) -0.00077(7) 0.0195(4) Uani 1 1 d . . . . . H7A H -0.237(3) 0.119(3) 0.0075(9) 0.023 Uiso 1 1 d . U . . . H7B H -0.096(3) 0.197(3) 0.0029(9) 0.023 Uiso 1 1 d . U . . . C16 C -0.0802(2) 0.1142(2) 0.08531(6) 0.0168(4) Uani 1 1 d . . . . . H16C H -0.029(3) 0.086(3) 0.1035(9) 0.020 Uiso 1 1 d . U . . . H16D H -0.037(3) 0.197(3) 0.0816(9) 0.020 Uiso 1 1 d . U . . . C17 C -0.1991(2) 0.0903(2) 0.10492(7) 0.0180(4) Uani 1 1 d . . . . . H17C H -0.260(3) 0.100(3) 0.0851(9) 0.022 Uiso 1 1 d . U . . . H17D H -0.243(3) 0.006(3) 0.1127(9) 0.022 Uiso 1 1 d . U . . . C18 C -0.1580(2) 0.1852(2) 0.14394(7) 0.0172(4) Uani 1 1 d . . . . . H18C H -0.132(3) 0.268(3) 0.1367(9) 0.021 Uiso 1 1 d . U . . . H18D H -0.085(3) 0.189(3) 0.1634(9) 0.021 Uiso 1 1 d . U . . . P2 P 0.04755(5) 0.52845(5) 0.58531(2) 0.01964(11) Uani 1 1 d . . . . . F1 F 0.09257(15) 0.44086(14) 0.61306(5) 0.0283(3) Uani 1 1 d . . . . . F2 F -0.05685(16) 0.40251(16) 0.55456(5) 0.0393(4) Uani 1 1 d . . . . . F3 F 0.15147(15) 0.65288(15) 0.61705(5) 0.0358(4) Uani 1 1 d . . . . . F4 F 0.15672(16) 0.55369(16) 0.55718(5) 0.0367(4) Uani 1 1 d . . . . . F5 F -0.06114(16) 0.50142(16) 0.61429(6) 0.0352(4) Uani 1 1 d . . . . . F6 F 0.00365(17) 0.61544(17) 0.55844(6) 0.0387(4) Uani 1 1 d . . . . . P3 P 0.04189(5) 0.52448(5) 0.08327(2) 0.01882(11) Uani 1 1 d . . . . . F7 F -0.05745(18) 0.39085(16) 0.05566(6) 0.0443(4) Uani 1 1 d . . . . . F8 F -0.01365(17) 0.59809(17) 0.05390(6) 0.0402(4) Uani 1 1 d . . . . . F9 F -0.06502(16) 0.49840(16) 0.11282(6) 0.0365(4) Uani 1 1 d . . . . . F10 F 0.09912(16) 0.45278(15) 0.11371(5) 0.0356(4) Uani 1 1 d . . . . . F11 F 0.15064(17) 0.55225(17) 0.05480(6) 0.0391(4) Uani 1 1 d . . . . . F12 F 0.14176(15) 0.65969(14) 0.11177(5) 0.0307(3) Uani 1 1 d . . . . . O7W O 0.64187(17) 1.03560(18) 0.32638(5) 0.0261(3) Uani 1 1 d D . . . . O14W O 0.67009(17) 0.24025(16) 0.28032(5) 0.0258(3) Uani 1 1 d D . . . . O8W O 0.9894(2) 0.4913(2) 0.23875(8) 0.0451(5) Uani 1 1 d D . . . . H15A H 0.552(3) -0.054(3) 0.2748(4) 0.046(9) Uiso 1 1 d D . . . . H15B H 0.563(3) -0.046(3) 0.2265(7) 0.057(11) Uiso 1 1 d D . . . . H5WA H 0.378(3) 0.194(3) 0.2233(10) 0.073(13) Uiso 1 1 d D . . . . H5WB H 0.4936(13) 0.197(3) 0.2560(11) 0.076(13) Uiso 1 1 d D . . . . H13A H -0.320(3) -0.627(2) 0.1976(11) 0.062(11) Uiso 1 1 d D . . . . H13B H -0.376(4) -0.541(4) 0.1773(9) 0.090(15) Uiso 1 1 d D . . . . H2WA H 0.4327(16) 0.013(3) 0.1557(12) 0.065(13) Uiso 1 1 d D . . . . H2WB H 0.280(2) -0.036(4) 0.1466(12) 0.067(13) Uiso 1 1 d D . . . . H12A H -0.235(3) -0.5839(16) 0.2930(10) 0.072(13) Uiso 1 1 d D . . . . H12B H -0.127(3) -0.470(3) 0.3264(4) 0.062(11) Uiso 1 1 d D . . . . H14E H 0.707(4) 0.232(3) 0.2561(7) 0.067(12) Uiso 1 1 d D . . . . H14F H 0.674(3) 0.181(3) 0.3002(8) 0.052(10) Uiso 1 1 d D . . . . H7WA H 0.566(2) 0.985(4) 0.3404(12) 0.068(13) Uiso 1 1 d D . . . . H7WB H 0.715(3) 1.027(5) 0.3411(14) 0.12(2) Uiso 1 1 d D . . . . H1WA H 0.255(3) 0.186(2) 0.1656(10) 0.092(16) Uiso 1 1 d D . . . . H1WB H 0.363(3) 0.333(2) 0.1628(9) 0.071(13) Uiso 1 1 d D . . . . H10A H -0.028(3) -0.189(4) 0.2415(11) 0.093(17) Uiso 1 1 d D . . . . H10B H -0.045(4) -0.140(3) 0.2853(9) 0.091(16) Uiso 1 1 d D . . . . H11A H 0.181(3) -0.325(3) 0.1723(3) 0.060(11) Uiso 1 1 d D . . . . H11B H 0.116(2) -0.380(3) 0.2123(9) 0.074(13) Uiso 1 1 d D . . . . H4WA H 0.065(3) 0.125(2) 0.2162(8) 0.060(12) Uiso 1 1 d D . . . . H4WB H 0.047(3) 0.186(2) 0.2573(11) 0.094(17) Uiso 1 1 d D . . . . H3WA H 0.239(4) 0.494(2) 0.3033(3) 0.143(17) Uiso 1 1 d D . . . . H3WB H 0.1180(8) 0.4062(19) 0.2668(9) 0.143(17) Uiso 1 1 d D . . . . H6WA H 0.477(2) 0.6364(19) 0.3391(6) 0.020 Uiso 1 1 d D U . . . H6WB H 0.438(2) 0.747(2) 0.3374(6) 0.020 Uiso 1 1 d D U . . . H8WA H 0.959(5) 0.512(5) 0.2633(12) 0.16(3) Uiso 1 1 d D . . . . H8WB H 0.917(3) 0.406(2) 0.2264(14) 0.108(18) Uiso 1 1 d D . . . . H9WA H -0.3866(15) -0.273(2) 0.3034(7) 0.023 Uiso 1 1 d D U . . . H9WB H -0.2480(18) -0.1498(17) 0.3117(6) 0.023 Uiso 1 1 d D U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01625(11) 0.01641(11) 0.01239(11) 0.00201(9) 0.00269(9) 0.00876(9) Cu1B 0.01554(11) 0.01574(11) 0.01264(11) 0.00171(9) 0.00251(9) 0.00846(9) S1 0.0169(2) 0.0177(2) 0.0138(2) 0.00520(17) 0.00468(17) 0.01031(18) S4 0.0176(2) 0.0144(2) 0.0117(2) 0.00201(16) 0.00120(16) 0.00821(18) S5 0.0145(2) 0.0175(2) 0.0130(2) 0.00055(17) -0.00006(16) 0.00759(18) S6B 0.0174(2) 0.0209(2) 0.0130(2) 0.00091(17) 0.00207(17) 0.01076(19) S3B 0.0159(2) 0.0151(2) 0.0151(2) 0.00072(17) 0.00083(17) 0.00835(18) S1B 0.0162(2) 0.0165(2) 0.0145(2) 0.00421(17) 0.00415(16) 0.00969(18) S4B 0.0190(2) 0.0159(2) 0.0127(2) 0.00353(16) 0.00273(17) 0.00847(18) S2B 0.0150(2) 0.0163(2) 0.0135(2) 0.00000(16) 0.00379(16) 0.00799(17) S2 0.0154(2) 0.0150(2) 0.0149(2) 0.00068(17) -0.00018(17) 0.00756(18) S3 0.0150(2) 0.0166(2) 0.0143(2) 0.00043(17) 0.00394(16) 0.00787(18) S6 0.0183(2) 0.0179(2) 0.0144(2) 0.00157(17) 0.00534(17) 0.00966(19) S5B 0.0216(2) 0.0220(2) 0.0126(2) 0.00426(18) 0.00677(18) 0.0129(2) Na3 0.0216(4) 0.0211(4) 0.0237(5) -0.0025(3) -0.0009(3) 0.0094(4) Na5 0.0225(4) 0.0232(4) 0.0184(4) 0.0037(3) 0.0045(3) 0.0130(4) Na4 0.0222(4) 0.0190(4) 0.0241(5) 0.0053(3) 0.0060(3) 0.0119(3) Na1 0.0290(5) 0.0196(4) 0.0201(4) 0.0034(3) 0.0030(4) 0.0082(4) Na6 0.0329(5) 0.0229(4) 0.0256(5) 0.0043(4) 0.0099(4) 0.0128(4) Na2 0.0532(7) 0.0247(5) 0.0319(6) 0.0095(4) 0.0225(5) 0.0224(5) O3B 0.0194(7) 0.0218(7) 0.0230(8) 0.0025(6) 0.0018(6) 0.0097(6) O3 0.0349(9) 0.0211(7) 0.0140(7) 0.0065(6) 0.0092(6) 0.0149(7) O1 0.0194(7) 0.0219(8) 0.0258(8) -0.0024(6) -0.0040(6) 0.0086(6) O6 0.0204(7) 0.0217(7) 0.0199(7) -0.0022(6) -0.0006(6) 0.0127(6) O5 0.0188(7) 0.0276(8) 0.0155(7) 0.0013(6) -0.0020(5) 0.0119(6) O5B 0.0391(10) 0.0495(12) 0.0216(9) -0.0111(8) 0.0092(8) 0.0208(9) O6B 0.0232(8) 0.0360(9) 0.0201(8) 0.0092(7) 0.0055(6) 0.0201(7) O4B 0.0321(9) 0.0396(10) 0.0420(11) 0.0284(9) 0.0197(8) 0.0254(8) O9B 0.0221(7) 0.0231(7) 0.0218(8) -0.0006(6) 0.0031(6) 0.0146(6) O7B 0.0257(8) 0.0295(8) 0.0130(7) 0.0020(6) -0.0002(6) 0.0149(7) O8B 0.0203(7) 0.0292(8) 0.0193(8) 0.0050(6) 0.0059(6) 0.0107(7) O1B 0.0309(9) 0.0343(9) 0.0183(8) 0.0140(7) 0.0097(6) 0.0170(7) O10W 0.0428(11) 0.0297(10) 0.0290(10) -0.0014(8) 0.0123(9) 0.0044(8) O9W 0.0454(12) 0.0402(12) 0.0411(12) -0.0058(9) 0.0045(10) 0.0164(10) O13W 0.0743(16) 0.0647(15) 0.0328(11) -0.0134(10) -0.0138(10) 0.0584(14) O12W 0.0308(9) 0.0291(9) 0.0238(9) 0.0019(7) 0.0035(7) 0.0131(8) O3W 0.0584(13) 0.0296(10) 0.0416(12) 0.0109(8) 0.0244(10) 0.0235(10) O4W 0.0271(8) 0.0232(8) 0.0216(8) -0.0032(6) 0.0033(7) 0.0072(7) O1W 0.0361(10) 0.0233(8) 0.0203(8) 0.0022(6) 0.0027(7) 0.0085(7) O2B 0.0397(10) 0.0206(8) 0.0202(8) 0.0002(6) 0.0023(7) 0.0165(7) O5W 0.0262(8) 0.0248(8) 0.0193(8) 0.0042(6) 0.0045(6) 0.0114(7) O15W 0.0274(8) 0.0256(8) 0.0172(7) 0.0058(6) 0.0058(6) 0.0132(7) O11W 0.0350(10) 0.0265(9) 0.0251(9) 0.0009(7) 0.0105(7) 0.0108(8) O6W 0.0601(14) 0.0509(12) 0.0296(10) 0.0043(9) 0.0055(9) 0.0399(11) O2W 0.0285(9) 0.0364(10) 0.0228(8) 0.0095(7) 0.0089(7) 0.0160(8) O4 0.0200(7) 0.0236(8) 0.0189(7) 0.0038(6) 0.0036(6) 0.0063(6) O7 0.0274(8) 0.0229(7) 0.0214(8) 0.0084(6) 0.0105(6) 0.0144(7) O9 0.0320(9) 0.0247(8) 0.0221(8) -0.0051(6) 0.0105(7) 0.0114(7) O8 0.0210(8) 0.0365(9) 0.0245(8) 0.0084(7) 0.0043(6) 0.0171(7) O2 0.0256(8) 0.0167(7) 0.0159(7) -0.0002(5) 0.0027(6) 0.0105(6) N1B 0.0147(7) 0.0160(7) 0.0137(7) 0.0021(6) 0.0025(6) 0.0079(6) N1 0.0148(7) 0.0164(7) 0.0122(7) 0.0019(6) 0.0019(6) 0.0079(6) C12 0.0175(9) 0.0210(9) 0.0154(9) 0.0062(7) 0.0049(7) 0.0116(8) C11 0.0221(10) 0.0211(9) 0.0141(9) 0.0060(7) 0.0057(7) 0.0142(8) C10 0.0223(10) 0.0220(10) 0.0140(9) 0.0060(7) 0.0076(7) 0.0147(8) C18B 0.0217(10) 0.0208(9) 0.0150(9) 0.0011(7) 0.0006(7) 0.0125(8) C17B 0.0205(10) 0.0206(10) 0.0155(9) 0.0029(7) 0.0010(7) 0.0098(8) C16B 0.0196(9) 0.0168(9) 0.0162(9) 0.0027(7) 0.0015(7) 0.0107(8) C10B 0.0182(9) 0.0197(9) 0.0160(9) 0.0046(7) 0.0057(7) 0.0120(8) C11B 0.0238(10) 0.0196(9) 0.0159(9) 0.0062(7) 0.0074(8) 0.0133(8) C12B 0.0196(10) 0.0243(10) 0.0176(10) 0.0075(8) 0.0064(7) 0.0134(8) C1B 0.0164(9) 0.0218(10) 0.0166(9) 0.0031(8) 0.0025(7) 0.0075(8) C2B 0.0166(9) 0.0251(10) 0.0155(9) 0.0017(8) -0.0005(7) 0.0097(8) C3B 0.0173(9) 0.0193(9) 0.0149(9) -0.0016(7) 0.0001(7) 0.0063(8) C9B 0.0220(10) 0.0258(10) 0.0148(9) 0.0033(8) 0.0061(7) 0.0148(9) C8B 0.0264(11) 0.0220(10) 0.0166(10) -0.0023(8) 0.0020(8) 0.0159(9) C7B 0.0206(10) 0.0256(10) 0.0166(9) 0.0012(8) 0.0030(7) 0.0155(9) C6B 0.0221(10) 0.0201(9) 0.0151(9) 0.0045(7) 0.0016(7) 0.0114(8) C5B 0.0238(10) 0.0197(10) 0.0151(9) 0.0054(7) 0.0057(8) 0.0090(8) C4B 0.0238(10) 0.0169(9) 0.0174(10) 0.0032(7) 0.0050(8) 0.0100(8) C13B 0.0154(9) 0.0190(9) 0.0157(9) -0.0020(7) 0.0031(7) 0.0079(8) C14B 0.0175(9) 0.0202(9) 0.0151(9) -0.0022(7) 0.0034(7) 0.0089(8) C15B 0.0201(9) 0.0185(9) 0.0145(9) 0.0007(7) 0.0073(7) 0.0080(8) C15 0.0181(9) 0.0161(9) 0.0157(9) -0.0001(7) -0.0015(7) 0.0080(8) C14 0.0192(9) 0.0171(9) 0.0152(9) 0.0000(7) -0.0020(7) 0.0069(8) C13 0.0168(9) 0.0163(9) 0.0151(9) 0.0019(7) -0.0007(7) 0.0087(7) C4 0.0210(10) 0.0247(10) 0.0183(10) 0.0007(8) 0.0023(8) 0.0151(9) C5 0.0266(11) 0.0230(10) 0.0153(9) -0.0028(8) 0.0015(8) 0.0154(9) C6 0.0226(10) 0.0261(10) 0.0143(9) 0.0023(8) 0.0058(7) 0.0143(9) C3 0.0194(9) 0.0212(10) 0.0144(9) -0.0015(7) 0.0004(7) 0.0084(8) C2 0.0157(9) 0.0252(10) 0.0158(9) 0.0023(8) -0.0007(7) 0.0089(8) C1 0.0151(9) 0.0212(10) 0.0189(10) 0.0034(8) 0.0032(7) 0.0073(8) C9 0.0232(10) 0.0185(9) 0.0161(9) 0.0061(7) 0.0022(8) 0.0103(8) C8 0.0227(10) 0.0181(9) 0.0172(10) 0.0059(7) 0.0068(8) 0.0079(8) C7 0.0227(10) 0.0179(9) 0.0186(10) 0.0039(8) 0.0053(8) 0.0101(8) C16 0.0168(9) 0.0181(9) 0.0150(9) -0.0009(7) 0.0032(7) 0.0083(8) C17 0.0172(9) 0.0217(10) 0.0148(9) -0.0013(7) 0.0037(7) 0.0093(8) C18 0.0177(9) 0.0176(9) 0.0151(9) 0.0002(7) 0.0050(7) 0.0073(8) P2 0.0172(2) 0.0180(2) 0.0243(3) 0.0028(2) 0.0034(2) 0.0092(2) F1 0.0336(8) 0.0285(7) 0.0293(8) 0.0037(6) 0.0012(6) 0.0215(6) F2 0.0359(9) 0.0306(8) 0.0373(9) -0.0080(7) -0.0111(7) 0.0108(7) F3 0.0310(8) 0.0241(7) 0.0437(9) -0.0098(6) 0.0011(7) 0.0091(6) F4 0.0362(8) 0.0408(9) 0.0403(9) 0.0093(7) 0.0207(7) 0.0210(7) F5 0.0326(8) 0.0351(8) 0.0485(10) 0.0145(7) 0.0224(7) 0.0206(7) F6 0.0421(9) 0.0398(9) 0.0459(10) 0.0201(8) 0.0098(8) 0.0280(8) P3 0.0178(2) 0.0187(2) 0.0202(3) 0.0005(2) 0.00130(19) 0.0098(2) F7 0.0405(9) 0.0284(8) 0.0487(11) -0.0153(7) -0.0096(8) 0.0106(7) F8 0.0432(9) 0.0448(9) 0.0393(9) 0.0126(7) -0.0029(7) 0.0293(8) F9 0.0304(8) 0.0366(8) 0.0489(10) 0.0116(7) 0.0218(7) 0.0176(7) F10 0.0332(8) 0.0339(8) 0.0449(10) 0.0138(7) 0.0012(7) 0.0216(7) F11 0.0426(9) 0.0434(9) 0.0395(9) 0.0054(7) 0.0237(8) 0.0234(8) F12 0.0315(8) 0.0224(7) 0.0293(8) -0.0048(6) 0.0008(6) 0.0081(6) O7W 0.0214(8) 0.0340(9) 0.0235(8) 0.0103(7) 0.0058(6) 0.0136(7) O14W 0.0329(9) 0.0278(8) 0.0208(8) 0.0039(6) 0.0092(7) 0.0169(7) O8W 0.0348(11) 0.0371(11) 0.0540(13) -0.0054(9) 0.0193(10) 0.0083(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu1 S1 2.2869(6) . ? Cu1 S2 2.2890(6) . ? Cu1 S3 2.2867(6) . ? Cu1 N1 2.1264(17) . ? Cu1B S3B 2.2911(6) . ? Cu1B S1B 2.2941(6) . ? Cu1B S2B 2.2873(6) . ? Cu1B N1B 2.1245(17) . ? S1 C10 1.817(2) . ? S1 C1 1.819(2) . ? S4 O3 1.4706(16) . ? S4 O1 1.4556(16) . ? S4 O2 1.4639(15) . ? S5 O6 1.4701(16) . ? S5 O5 1.4715(16) . ? S5 O4 1.4622(16) . ? S6B O9B 1.4694(16) . ? S6B O7B 1.4632(16) . ? S6B O8B 1.4642(16) . ? S3B C16B 1.817(2) . ? S3B C7B 1.821(2) . ? S1B C10B 1.820(2) . ? S1B C1B 1.819(2) . ? S4B O3B 1.4593(16) . ? S4B O1B 1.4596(16) . ? S4B O2B 1.4610(17) . ? S2B C4B 1.827(2) . ? S2B C13B 1.818(2) . ? S2 C13 1.820(2) . ? S2 C4 1.820(2) . ? S3 C7 1.821(2) . ? S3 C16 1.816(2) . ? S6 O7 1.4674(16) . ? S6 O9 1.4682(17) . ? S6 O8 1.4539(17) . ? S5B O5B 1.4581(18) . ? S5B O6B 1.4619(17) . ? S5B O4B 1.4556(18) . ? Na3 O1 2.3318(18) . ? Na3 O6 2.4852(19) . ? Na3 O7B 2.4870(19) . ? Na3 O10W 2.642(3) . ? Na3 O9W 2.582(3) . ? Na3 O7 2.4187(19) . ? Na5 O5 2.3591(18) . ? Na5 O5B 2.595(2) . ? Na5 O5W 2.4500(19) . ? Na5 O15W 2.4116(19) . ? Na5 O11W 2.432(2) . ? Na5 O2W 2.3480(19) . ? Na4 O3B 2.3452(18) . ? Na4 O5 2.7526(18) . ? Na4 O4B 2.2928(19) . ? Na4 O9B 2.4127(18) . ? Na4 O4W 2.481(2) . ? Na4 O5W 2.4044(19) . ? Na1 O3B 2.6073(19) . ? Na1 O3 2.3404(18) 1_665 ? Na1 O1B 2.545(2) . ? Na1 O3W 2.388(2) . ? Na1 O4W 2.3062(19) . ? Na1 O1W 2.383(2) . ? Na6 O1 2.826(2) . ? Na6 O1B 2.3614(19) 1_445 ? Na6 O10W 2.368(2) . ? Na6 O9W 2.440(2) . ? Na6 O13W 2.368(2) . ? Na6 O12W 2.412(2) . ? Na2 O3 2.3700(18) 1_665 ? Na2 O5B 2.455(2) 1_565 ? Na2 O3W 2.396(2) . ? Na2 O15W 2.3699(19) 1_565 ? Na2 O11W 2.350(2) 1_565 ? Na2 O6W 2.302(2) . ? O3 Na1 2.3405(18) 1_445 ? O3 Na2 2.3702(18) 1_445 ? O5B Na2 2.455(2) 1_545 ? O1B Na6 2.3614(19) 1_665 ? O10W H10A 0.983(10) . ? O10W H10B 0.984(10) . ? O9W H9WA 1.015(9) . ? O9W H9WB 0.991(9) . ? O13W H13A 0.979(10) . ? O13W H13B 0.982(10) . ? O12W H12A 0.979(10) . ? O12W H12B 0.977(10) . ? O3W H3WA 0.984(7) . ? O3W H3WB 0.977(10) . ? O4W H4WA 0.994(7) . ? O4W H4WB 0.990(9) . ? O1W H1WA 0.975(10) . ? O1W H1WB 0.974(10) . ? O5W H5WA 0.973(10) . ? O5W H5WB 0.969(10) . ? O15W Na2 2.3699(19) 1_545 ? O15W H15A 0.979(10) . ? O15W H15B 0.972(10) . ? O11W Na2 2.350(2) 1_545 ? O11W H11A 0.976(10) . ? O11W H11B 0.977(10) . ? O6W H6WA 0.997(9) . ? O6W H6WB 0.999(9) . ? O2W H2WA 0.981(10) . ? O2W H2WB 0.984(10) . ? N1B C3B 1.494(3) . ? N1B C9B 1.498(3) . ? N1B C6B 1.489(3) . ? N1 C6 1.499(3) . ? N1 C3 1.494(3) . ? N1 C9 1.489(3) . ? C12 H12C 0.91(3) . ? C12 H12D 0.94(3) . ? C12 C11 1.522(3) . ? C11 H11C 0.93(3) . ? C11 H11D 0.96(3) . ? C11 C10 1.528(3) . ? C10 H10C 0.99(3) . ? C10 H10D 0.97(3) . ? C18B H18A 0.91(3) . ? C18B H18B 0.97(3) . ? C18B C17B 1.530(3) . ? C17B H17A 0.94(3) . ? C17B H17B 0.93(3) . ? C17B C16B 1.521(3) . ? C16B H16A 0.90(3) . ? C16B H16B 0.97(3) . ? C10B H10E 0.91(3) . ? C10B H10F 0.95(3) . ? C10B C11B 1.523(3) . ? C11B H11E 0.91(3) . ? C11B H11F 1.04(3) . ? C11B C12B 1.524(3) . ? C12B H12E 0.98(3) . ? C12B H12F 0.87(3) . ? C1B H1BA 0.92(3) . ? C1B H1BB 0.94(3) . ? C1B C2B 1.525(3) . ? C2B H2BA 0.94(3) . ? C2B H2BB 0.91(3) . ? C2B C3B 1.529(3) . ? C3B H3BA 0.97(3) . ? C3B H3BB 0.94(3) . ? C9B H9BA 0.91(3) . ? C9B H9BB 0.93(3) . ? C9B C8B 1.527(3) . ? C8B H8BA 0.96(3) . ? C8B H8BB 0.96(3) . ? C8B C7B 1.529(3) . ? C7B H7BA 0.89(3) . ? C7B H7BB 0.95(3) . ? C6B H6BA 0.97(3) . ? C6B H6BB 0.95(3) . ? C6B C5B 1.529(3) . ? C5B H5BA 0.94(3) . ? C5B H5BB 0.94(3) . ? C5B C4B 1.527(3) . ? C4B H4BA 0.93(3) . ? C4B H4BB 0.98(3) . ? C13B H13C 0.94(3) . ? C13B H13D 0.95(3) . ? C13B C14B 1.521(3) . ? C14B H14A 0.92(3) . ? C14B H14B 0.90(3) . ? C14B C15B 1.525(3) . ? C15B H15C 0.97(3) . ? C15B H15D 0.93(3) . ? C15 H15E 0.97(3) . ? C15 H15F 0.92(3) . ? C15 C14 1.530(3) . ? C14 H14C 0.98(3) . ? C14 H14D 0.99(3) . ? C14 C13 1.520(3) . ? C13 H13E 0.93(3) . ? C13 H13F 0.91(3) . ? C4 H4A 0.96(3) . ? C4 H4B 0.89(3) . ? C4 C5 1.531(3) . ? C5 H5A 0.98(3) . ? C5 H5B 0.94(3) . ? C5 C6 1.530(3) . ? C6 H6A 0.98(3) . ? C6 H6B 0.96(3) . ? C3 H3A 1.00(3) . ? C3 H3B 0.99(3) . ? C3 C2 1.527(3) . ? C2 H2A 0.91(3) . ? C2 H2B 0.94(3) . ? C2 C1 1.529(3) . ? C1 H1A 1.00(3) . ? C1 H1B 0.92(3) . ? C9 H9A 0.95(3) . ? C9 H9B 0.97(3) . ? C9 C8 1.527(3) . ? C8 H8A 0.97(3) . ? C8 H8B 0.90(3) . ? C8 C7 1.530(3) . ? C7 H7A 0.94(3) . ? C7 H7B 0.90(3) . ? C16 H16C 0.97(3) . ? C16 H16D 0.89(3) . ? C16 C17 1.527(3) . ? C17 H17C 0.95(3) . ? C17 H17D 0.94(3) . ? C17 C18 1.524(3) . ? C18 H18C 0.93(3) . ? C18 H18D 0.98(3) . ? P2 F1 1.6223(15) . ? P2 F2 1.5929(17) . ? P2 F3 1.5979(16) . ? P2 F4 1.5949(16) . ? P2 F5 1.6053(16) . ? P2 F6 1.5942(16) . ? P3 F7 1.5880(17) . ? P3 F8 1.5907(16) . ? P3 F9 1.6040(16) . ? P3 F10 1.6047(16) . ? P3 F11 1.5928(16) . ? P3 F12 1.6136(15) . ? O7W H7WA 0.985(10) . ? O7W H7WB 0.985(10) . ? O14W H14E 0.974(10) . ? O14W H14F 0.979(10) . ? O8W H8WA 0.985(10) . ? O8W H8WB 0.980(10) . ? 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 S1 Cu1 S2 117.77(2) . . ? S3 Cu1 S1 117.61(2) . . ? S3 Cu1 S2 118.35(2) . . ? N1 Cu1 S1 97.86(5) . . ? N1 Cu1 S2 98.52(5) . . ? N1 Cu1 S3 98.77(5) . . ? S3B Cu1B S1B 117.60(2) . . ? S2B Cu1B S3B 118.52(2) . . ? S2B Cu1B S1B 117.33(2) . . ? N1B Cu1B S3B 97.98(5) . . ? N1B Cu1B S1B 98.90(5) . . ? N1B Cu1B S2B 98.85(5) . . ? C10 S1 Cu1 113.55(7) . . ? C10 S1 C1 102.03(10) . . ? C1 S1 Cu1 96.73(7) . . ? O1 S4 O3 111.78(10) . . ? O1 S4 O2 112.01(10) . . ? O2 S4 O3 112.33(9) . . ? O6 S5 O5 111.41(9) . . ? O4 S5 O6 112.08(10) . . ? O4 S5 O5 112.20(9) . . ? O7B S6B O9B 111.85(10) . . ? O7B S6B O8B 112.09(10) . . ? O8B S6B O9B 111.58(10) . . ? C16B S3B Cu1B 113.82(7) . . ? C16B S3B C7B 102.14(10) . . ? C7B S3B Cu1B 97.11(8) . . ? C10B S1B Cu1B 113.49(7) . . ? C1B S1B Cu1B 96.83(7) . . ? C1B S1B C10B 101.80(10) . . ? O3B S4B O1B 110.51(10) . . ? O3B S4B O2B 111.86(10) . . ? O1B S4B O2B 112.95(10) . . ? C4B S2B Cu1B 96.54(7) . . ? C13B S2B Cu1B 114.24(7) . . ? C13B S2B C4B 101.23(10) . . ? C13 S2 Cu1 113.78(7) . . ? C13 S2 C4 101.96(10) . . ? C4 S2 Cu1 96.85(8) . . ? C7 S3 Cu1 96.60(7) . . ? C16 S3 Cu1 114.11(7) . . ? C16 S3 C7 101.63(10) . . ? O7 S6 O9 111.80(10) . . ? O8 S6 O7 112.41(10) . . ? O8 S6 O9 112.23(11) . . ? O5B S5B O6B 113.34(11) . . ? O4B S5B O5B 110.72(13) . . ? O4B S5B O6B 111.72(11) . . ? O1 Na3 O6 97.01(6) . . ? O1 Na3 O7B 162.11(7) . . ? O1 Na3 O10W 83.31(7) . . ? O1 Na3 O9W 81.21(7) . . ? O1 Na3 O7 99.08(7) . . ? O6 Na3 O7B 98.54(6) . . ? O6 Na3 O10W 82.30(6) . . ? O6 Na3 O9W 146.09(8) . . ? O7B Na3 O10W 90.03(6) . . ? O7B Na3 O9W 80.95(7) . . ? O9W Na3 O10W 63.82(7) . . ? O7 Na3 O6 90.29(6) . . ? O7 Na3 O7B 89.67(6) . . ? O7 Na3 O10W 172.45(7) . . ? O7 Na3 O9W 123.54(7) . . ? O5 Na5 O5B 99.66(7) . . ? O5 Na5 O5W 82.74(6) . . ? O5 Na5 O15W 178.31(7) . . ? O5 Na5 O11W 90.39(7) . . ? O5W Na5 O5B 119.94(7) . . ? O15W Na5 O5B 80.87(6) . . ? O15W Na5 O5W 98.40(6) . . ? O15W Na5 O11W 88.28(7) . . ? O11W Na5 O5B 70.44(6) . . ? O11W Na5 O5W 168.32(7) . . ? O2W Na5 O5 91.42(7) . . ? O2W Na5 O5B 151.09(7) . . ? O2W Na5 O5W 87.75(7) . . ? O2W Na5 O15W 87.38(7) . . ? O2W Na5 O11W 82.97(7) . . ? O3B Na4 O5 155.17(6) . . ? O3B Na4 O9B 95.93(6) . . ? O3B Na4 O4W 79.90(6) . . ? O3B Na4 O5W 92.29(6) . . ? O4B Na4 O3B 107.29(8) . . ? O4B Na4 O5 91.55(7) . . ? O4B Na4 O9B 94.60(7) . . ? O4B Na4 O4W 172.21(8) . . ? O4B Na4 O5W 77.58(7) . . ? O9B Na4 O5 98.57(6) . . ? O9B Na4 O4W 87.48(6) . . ? O4W Na4 O5 80.71(6) . . ? O5W Na4 O5 75.78(6) . . ? O5W Na4 O9B 170.07(7) . . ? O5W Na4 O4W 99.48(7) . . ? O3 Na1 O3B 134.09(7) 1_665 . ? O3 Na1 O1B 85.11(6) 1_665 . ? O3 Na1 O3W 88.04(7) 1_665 . ? O3 Na1 O1W 87.45(7) 1_665 . ? O1B Na1 O3B 55.47(5) . . ? O3W Na1 O3B 82.84(7) . . ? O3W Na1 O1B 106.78(8) . . ? O4W Na1 O3B 77.99(6) . . ? O4W Na1 O3 145.11(8) . 1_665 ? O4W Na1 O1B 129.77(7) . . ? O4W Na1 O3W 82.52(8) . . ? O4W Na1 O1W 83.03(7) . . ? O1W Na1 O3B 121.98(7) . . ? O1W Na1 O1B 104.77(7) . . ? O1W Na1 O3W 147.59(9) . . ? O1B Na6 O1 113.71(7) 1_445 . ? O1B Na6 O10W 152.81(8) 1_445 . ? O1B Na6 O9W 89.41(8) 1_445 . ? O1B Na6 O13W 98.20(9) 1_445 . ? O1B Na6 O12W 88.80(7) 1_445 . ? O10W Na6 O1 78.72(7) . . ? O10W Na6 O9W 70.08(8) . . ? O10W Na6 O12W 88.86(8) . . ? O9W Na6 O1 74.52(7) . . ? O13W Na6 O1 75.75(7) . . ? O13W Na6 O10W 108.50(9) . . ? O13W Na6 O9W 149.88(9) . . ? O13W Na6 O12W 84.31(7) . . ? O12W Na6 O1 151.55(7) . . ? O12W Na6 O9W 125.15(8) . . ? O3 Na2 O5B 170.86(8) 1_665 1_565 ? O3 Na2 O3W 87.17(7) 1_665 . ? O3W Na2 O5B 84.84(8) . 1_565 ? O15W Na2 O3 103.74(7) 1_565 1_665 ? O15W Na2 O5B 84.67(7) 1_565 1_565 ? O15W Na2 O3W 167.76(8) 1_565 . ? O11W Na2 O3 101.62(7) 1_565 1_665 ? O11W Na2 O5B 74.27(7) 1_565 1_565 ? O11W Na2 O3W 91.99(8) 1_565 . ? O11W Na2 O15W 91.23(7) 1_565 1_565 ? O6W Na2 O3 102.67(8) . 1_665 ? O6W Na2 O5B 80.06(8) . 1_565 ? O6W Na2 O3W 78.31(9) . . ? O6W Na2 O15W 93.66(8) . 1_565 ? O6W Na2 O11W 153.29(8) . 1_565 ? S4B O3B Na4 132.23(10) . . ? S4B O3B Na1 93.60(8) . . ? Na4 O3B Na1 84.65(6) . . ? S4 O3 Na1 136.37(10) . 1_445 ? S4 O3 Na2 130.59(9) . 1_445 ? Na1 O3 Na2 92.30(6) 1_445 1_445 ? S4 O1 Na3 141.02(10) . . ? S4 O1 Na6 103.46(9) . . ? Na3 O1 Na6 87.58(6) . . ? S5 O6 Na3 129.57(10) . . ? S5 O5 Na5 132.47(10) . . ? S5 O5 Na4 124.82(9) . . ? Na5 O5 Na4 80.98(5) . . ? S5B O5B Na5 102.04(11) . . ? S5B O5B Na2 134.95(12) . 1_545 ? Na2 O5B Na5 77.34(6) 1_545 . ? S5B O4B Na5 93.05(10) . . ? S5B O4B Na4 144.64(12) . . ? Na4 O4B Na5 80.90(6) . . ? S6B O9B Na4 126.39(10) . . ? S6B O7B Na3 121.51(10) . . ? S4B O1B Na1 96.18(9) . . ? S4B O1B Na6 149.11(11) . 1_665 ? Na6 O1B Na1 111.49(7) 1_665 . ? Na3 O10W H10A 99(3) . . ? Na3 O10W H10B 91(3) . . ? Na6 O10W Na3 91.29(8) . . ? Na6 O10W H10A 126(2) . . ? Na6 O10W H10B 125(2) . . ? H10A O10W H10B 107.9(14) . . ? Na3 O9W H9WA 144.3(15) . . ? Na3 O9W H9WB 94.9(14) . . ? Na6 O9W Na3 91.14(8) . . ? Na6 O9W H9WA 99.6(14) . . ? Na6 O9W H9WB 133.3(16) . . ? H9WA O9W H9WB 101.8(12) . . ? Na6 O13W H13A 136(2) . . ? Na6 O13W H13B 112(2) . . ? H13A O13W H13B 107.3(14) . . ? Na6 O12W H12A 97(2) . . ? Na6 O12W H12B 121(2) . . ? H12A O12W H12B 107.5(14) . . ? Na1 O3W Na2 90.51(8) . . ? Na1 O3W H3WA 107(4) . . ? Na1 O3W H3WB 98.0(8) . . ? Na2 O3W H3WA 100.3(7) . . ? Na2 O3W H3WB 146(2) . . ? H3WA O3W H3WB 108.4(13) . . ? Na4 O4W H4WA 97(2) . . ? Na4 O4W H4WB 98(3) . . ? Na1 O4W Na4 88.42(7) . . ? Na1 O4W H4WA 127.1(16) . . ? Na1 O4W H4WB 124.9(14) . . ? H4WA O4W H4WB 106.4(11) . . ? Na1 O1W H1WA 130(3) . . ? Na1 O1W H1WB 106(2) . . ? H1WA O1W H1WB 109.9(15) . . ? Na5 O5W H5WA 119(2) . . ? Na5 O5W H5WB 116(2) . . ? Na4 O5W Na5 86.71(6) . . ? Na4 O5W H5WA 97(2) . . ? Na4 O5W H5WB 126(2) . . ? H5WA O5W H5WB 110.1(14) . . ? Na5 O15W H15A 109.4(19) . . ? Na5 O15W H15B 108(2) . . ? Na2 O15W Na5 82.65(6) 1_545 . ? Na2 O15W H15A 107.0(17) 1_545 . ? Na2 O15W H15B 136.9(19) 1_545 . ? H15A O15W H15B 108.3(14) . . ? Na5 O11W H11A 112(2) . . ? Na5 O11W H11B 123(2) . . ? Na2 O11W Na5 82.62(7) 1_545 . ? Na2 O11W H11A 129(2) 1_545 . ? Na2 O11W H11B 101(2) 1_545 . ? H11A O11W H11B 108.3(14) . . ? Na2 O6W H6WA 141.0(14) . . ? Na2 O6W H6WB 104.5(13) . . ? H6WA O6W H6WB 106.2(12) . . ? Na5 O2W H2WA 122(2) . . ? Na5 O2W H2WB 107(2) . . ? H2WA O2W H2WB 107.1(14) . . ? S6 O7 Na3 147.03(10) . . ? C3B N1B Cu1B 110.65(12) . . ? C3B N1B C9B 107.56(16) . . ? C9B N1B Cu1B 111.60(13) . . ? C6B N1B Cu1B 111.35(13) . . ? C6B N1B C3B 107.88(16) . . ? C6B N1B C9B 107.62(16) . . ? C6 N1 Cu1 110.57(12) . . ? C3 N1 Cu1 111.90(12) . . ? C3 N1 C6 107.75(16) . . ? C9 N1 Cu1 111.06(13) . . ? C9 N1 C6 107.86(16) . . ? C9 N1 C3 107.54(16) . . ? S4 C12 H12C 104.0(17) . . ? S4 C12 H12D 108.5(17) . . ? H12C C12 H12D 103(2) . . ? C11 C12 S4 112.99(14) . . ? C11 C12 H12C 113.5(18) . . ? C11 C12 H12D 113.9(17) . . ? C12 C11 H11C 107.7(18) . . ? C12 C11 H11D 108.3(17) . . ? C12 C11 C10 109.86(16) . . ? H11C C11 H11D 105(2) . . ? C10 C11 H11C 112.8(18) . . ? C10 C11 H11D 113.2(17) . . ? S1 C10 H10C 105.6(16) . . ? S1 C10 H10D 109.9(17) . . ? C11 C10 S1 114.36(14) . . ? C11 C10 H10C 111.3(16) . . ? C11 C10 H10D 112.0(17) . . ? H10C C10 H10D 103(2) . . ? S6B C18B H18A 108.1(18) . . ? S6B C18B H18B 105.9(17) . . ? H18A C18B H18B 110(2) . . ? C17B C18B S6B 111.38(15) . . ? C17B C18B H18A 110.1(18) . . ? C17B C18B H18B 111.1(17) . . ? C18B C17B H17A 108.8(18) . . ? C18B C17B H17B 106.1(18) . . ? H17A C17B H17B 105(2) . . ? C16B C17B C18B 111.05(18) . . ? C16B C17B H17A 111.1(18) . . ? C16B C17B H17B 114.3(18) . . ? S3B C16B H16A 106.0(18) . . ? S3B C16B H16B 105.3(17) . . ? C17B C16B S3B 113.93(14) . . ? C17B C16B H16A 110.2(18) . . ? C17B C16B H16B 110.0(17) . . ? H16A C16B H16B 111(2) . . ? S1B C10B H10E 108.4(18) . . ? S1B C10B H10F 105.2(17) . . ? H10E C10B H10F 105(2) . . ? C11B C10B S1B 113.44(14) . . ? C11B C10B H10E 113.3(18) . . ? C11B C10B H10F 110.6(17) . . ? C10B C11B H11E 109.7(18) . . ? C10B C11B H11F 109.8(16) . . ? C10B C11B C12B 111.27(17) . . ? H11E C11B H11F 107(2) . . ? C12B C11B H11E 111.0(18) . . ? C12B C11B H11F 107.6(16) . . ? S4B C12B H12E 102.7(16) . . ? S4B C12B H12F 103.2(19) . . ? C11B C12B S4B 110.97(14) . . ? C11B C12B H12E 117.9(17) . . ? C11B C12B H12F 114.4(19) . . ? H12E C12B H12F 106(2) . . ? S1B C1B H1BA 107.9(18) . . ? S1B C1B H1BB 107.2(18) . . ? H1BA C1B H1BB 112(3) . . ? C2B C1B S1B 110.78(15) . . ? C2B C1B H1BA 107.8(19) . . ? C2B C1B H1BB 110.9(18) . . ? C1B C2B H2BA 105.9(18) . . ? C1B C2B H2BB 111.3(19) . . ? C1B C2B C3B 116.55(18) . . ? H2BA C2B H2BB 106(3) . . ? C3B C2B H2BA 107.9(18) . . ? C3B C2B H2BB 108.5(19) . . ? N1B C3B C2B 117.41(17) . . ? N1B C3B H3BA 108.9(17) . . ? N1B C3B H3BB 107.6(18) . . ? C2B C3B H3BA 108.7(17) . . ? C2B C3B H3BB 105.6(18) . . ? H3BA C3B H3BB 108(2) . . ? N1B C9B H9BA 106.1(18) . . ? N1B C9B H9BB 106.7(18) . . ? N1B C9B C8B 117.53(18) . . ? H9BA C9B H9BB 106(3) . . ? C8B C9B H9BA 109.1(18) . . ? C8B C9B H9BB 110.4(18) . . ? C9B C8B H8BA 110.0(18) . . ? C9B C8B H8BB 106.0(18) . . ? C9B C8B C7B 116.28(18) . . ? H8BA C8B H8BB 110(2) . . ? C7B C8B H8BA 109.0(18) . . ? C7B C8B H8BB 104.8(18) . . ? S3B C7B H7BA 111.4(19) . . ? S3B C7B H7BB 110.1(18) . . ? C8B C7B S3B 110.54(15) . . ? C8B C7B H7BA 104.9(19) . . ? C8B C7B H7BB 112.9(18) . . ? H7BA C7B H7BB 107(3) . . ? N1B C6B H6BA 105.6(17) . . ? N1B C6B H6BB 103.3(18) . . ? N1B C6B C5B 117.30(18) . . ? H6BA C6B H6BB 109(2) . . ? C5B C6B H6BA 109.1(17) . . ? C5B C6B H6BB 112.4(18) . . ? C6B C5B H5BA 108.4(18) . . ? C6B C5B H5BB 110.2(18) . . ? H5BA C5B H5BB 109(2) . . ? C4B C5B C6B 116.13(18) . . ? C4B C5B H5BA 103.5(18) . . ? C4B C5B H5BB 109.0(18) . . ? S2B C4B H4BA 109.3(18) . . ? S2B C4B H4BB 108.2(17) . . ? C5B C4B S2B 110.63(15) . . ? C5B C4B H4BA 108.2(18) . . ? C5B C4B H4BB 110.6(17) . . ? H4BA C4B H4BB 110(2) . . ? S2B C13B H13C 108.9(17) . . ? S2B C13B H13D 108.7(17) . . ? H13C C13B H13D 105(2) . . ? C14B C13B S2B 113.91(14) . . ? C14B C13B H13C 110.7(17) . . ? C14B C13B H13D 108.9(17) . . ? C13B C14B H14A 109.5(18) . . ? C13B C14B H14B 109.8(18) . . ? C13B C14B C15B 111.83(17) . . ? H14A C14B H14B 109(3) . . ? C15B C14B H14A 108.9(18) . . ? C15B C14B H14B 107.5(18) . . ? S5B C15B H15C 106.8(17) . . ? S5B C15B H15D 104.3(17) . . ? C14B C15B S5B 111.52(15) . . ? C14B C15B H15C 110.7(17) . . ? C14B C15B H15D 113.3(18) . . ? H15C C15B H15D 110(2) . . ? S5 C15 H15E 105.8(17) . . ? S5 C15 H15F 108.9(18) . . ? H15E C15 H15F 108(2) . . ? C14 C15 S5 110.58(14) . . ? C14 C15 H15E 112.8(17) . . ? C14 C15 H15F 110.6(18) . . ? C15 C14 H14C 104.4(17) . . ? C15 C14 H14D 108.1(17) . . ? H14C C14 H14D 110(2) . . ? C13 C14 C15 111.40(17) . . ? C13 C14 H14C 113.7(17) . . ? C13 C14 H14D 109.3(17) . . ? S2 C13 H13E 105.7(17) . . ? S2 C13 H13F 106.2(18) . . ? C14 C13 S2 113.47(14) . . ? C14 C13 H13E 109.1(17) . . ? C14 C13 H13F 110.7(17) . . ? H13E C13 H13F 112(2) . . ? S2 C4 H4A 109.9(18) . . ? S2 C4 H4B 110.4(19) . . ? H4A C4 H4B 108(3) . . ? C5 C4 S2 110.60(15) . . ? C5 C4 H4A 110.2(18) . . ? C5 C4 H4B 108.1(19) . . ? C4 C5 H5A 104.4(17) . . ? C4 C5 H5B 106.3(18) . . ? H5A C5 H5B 113(2) . . ? C6 C5 C4 116.28(18) . . ? C6 C5 H5A 104.8(17) . . ? C6 C5 H5B 112.3(18) . . ? N1 C6 C5 117.21(18) . . ? N1 C6 H6A 106.4(17) . . ? N1 C6 H6B 107.5(18) . . ? C5 C6 H6A 108.6(17) . . ? C5 C6 H6B 109.9(17) . . ? H6A C6 H6B 107(2) . . ? N1 C3 H3A 107.3(16) . . ? N1 C3 H3B 110.5(17) . . ? N1 C3 C2 117.02(17) . . ? H3A C3 H3B 106(2) . . ? C2 C3 H3A 106.9(16) . . ? C2 C3 H3B 108.2(17) . . ? C3 C2 H2A 104.9(18) . . ? C3 C2 H2B 109.8(18) . . ? C3 C2 C1 116.25(18) . . ? H2A C2 H2B 108(3) . . ? C1 C2 H2A 108.1(19) . . ? C1 C2 H2B 109.3(18) . . ? S1 C1 H1A 109.1(17) . . ? S1 C1 H1B 109.7(18) . . ? C2 C1 S1 110.57(15) . . ? C2 C1 H1A 109.7(17) . . ? C2 C1 H1B 107.2(18) . . ? H1A C1 H1B 111(2) . . ? N1 C9 H9A 104.6(18) . . ? N1 C9 H9B 105.1(17) . . ? N1 C9 C8 117.59(18) . . ? H9A C9 H9B 110(2) . . ? C8 C9 H9A 107.5(17) . . ? C8 C9 H9B 112.1(17) . . ? C9 C8 H8A 107.1(17) . . ? C9 C8 H8B 110.4(19) . . ? C9 C8 C7 116.33(18) . . ? H8A C8 H8B 110(3) . . ? C7 C8 H8A 104.7(18) . . ? C7 C8 H8B 107.6(19) . . ? S3 C7 H7A 108.7(18) . . ? S3 C7 H7B 106.9(19) . . ? C8 C7 S3 110.74(15) . . ? C8 C7 H7A 112.2(18) . . ? C8 C7 H7B 110.2(19) . . ? H7A C7 H7B 108(3) . . ? S3 C16 H16C 104.6(17) . . ? S3 C16 H16D 107.9(19) . . ? H16C C16 H16D 114(2) . . ? C17 C16 S3 114.42(14) . . ? C17 C16 H16C 108.7(16) . . ? C17 C16 H16D 107.7(18) . . ? C16 C17 H17C 109.8(18) . . ? C16 C17 H17D 111.5(18) . . ? H17C C17 H17D 107(2) . . ? C18 C17 C16 110.97(17) . . ? C18 C17 H17C 109.1(18) . . ? C18 C17 H17D 108.4(18) . . ? S6 C18 H18C 106.4(17) . . ? S6 C18 H18D 106.8(17) . . ? C17 C18 S6 112.24(14) . . ? C17 C18 H18C 111.1(18) . . ? C17 C18 H18D 112.2(17) . . ? H18C C18 H18D 108(2) . . ? F2 P2 F1 89.60(9) . . ? F2 P2 F3 178.69(10) . . ? F2 P2 F4 90.47(10) . . ? F2 P2 F5 89.64(10) . . ? F2 P2 F6 90.88(10) . . ? F3 P2 F1 89.39(9) . . ? F3 P2 F5 89.52(9) . . ? F4 P2 F1 89.34(9) . . ? F4 P2 F3 90.35(9) . . ? F4 P2 F5 178.74(10) . . ? F5 P2 F1 89.41(8) . . ? F6 P2 F1 179.45(10) . . ? F6 P2 F3 90.13(10) . . ? F6 P2 F4 90.94(9) . . ? F6 P2 F5 90.32(9) . . ? F7 P3 F8 91.01(10) . . ? F7 P3 F9 90.06(10) . . ? F7 P3 F10 90.17(10) . . ? F7 P3 F11 91.08(10) . . ? F7 P3 F12 179.30(11) . . ? F8 P3 F9 89.97(10) . . ? F8 P3 F10 178.73(10) . . ? F8 P3 F11 90.64(10) . . ? F8 P3 F12 89.19(9) . . ? F9 P3 F10 89.56(9) . . ? F9 P3 F12 89.27(9) . . ? F10 P3 F12 89.63(9) . . ? F11 P3 F9 178.69(11) . . ? F11 P3 F10 89.80(10) . . ? F11 P3 F12 89.59(9) . . ? H7WA O7W H7WB 107.0(14) . . ? H14E O14W H14F 108.4(14) . . ? H8WA O8W H8WB 104.4(14) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O15W H15A O7W 0.979(10) 1.827(10) 2.805(2) 176(3) 1_545 O15W H15B O7 0.972(10) 1.863(13) 2.818(2) 167(3) 1_655 O5W H5WA O1W 0.973(10) 1.837(10) 2.808(2) 175(3) . O5W H5WB O14W 0.969(10) 1.928(14) 2.865(2) 162(3) . O2W H2WA O8 0.981(10) 1.873(10) 2.850(2) 174(4) 1_655 O12W H12A O14W 0.979(10) 1.831(15) 2.779(2) 162(4) 1_445 O12W H12B F1 0.977(10) 1.923(13) 2.886(2) 168(3) 2_556 O14W H14E O9 0.974(10) 1.819(12) 2.762(2) 162(3) 1_655 O14W H14F O7W 0.979(10) 1.835(14) 2.788(2) 164(3) 1_545 O7W H7WA O6B 0.985(10) 1.855(12) 2.831(2) 171(4) 1_565 O7W H7WB O8B 0.985(10) 1.922(19) 2.871(2) 161(5) 1_665 O1W H1WA O4 0.975(10) 1.939(12) 2.893(2) 166(3) . O1W H1WB O2 0.974(10) 1.881(16) 2.793(2) 155(3) 1_665 O10W H10A O5 0.983(10) 1.87(2) 2.790(3) 155(4) . O10W H10B O9B 0.984(10) 1.872(15) 2.838(3) 167(4) . O11W H11A F12 0.976(10) 1.925(11) 2.897(2) 173(3) 1_545 O11W H11B O8W 0.977(10) 1.867(12) 2.830(3) 168(3) 1_445 O4W H4WA O6 0.994(7) 1.786(8) 2.764(2) 167(2) . O4W H4WB O7B 0.990(9) 1.929(9) 2.851(2) 154(2) . O6W H6WA O2B 0.997(9) 1.732(9) 2.702(3) 163(2) . O6W H6WB O6B 0.999(9) 1.887(10) 2.861(3) 164.0(19) 1_565 O8W H8WA O12W 0.985(10) 1.90(2) 2.831(3) 157(4) 1_665 O8W H8WB O9 0.980(10) 1.875(13) 2.847(3) 171(4) 1_655 O9W H9WB O8B 0.991(9) 1.851(10) 2.841(3) 178(3) . loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag Cu1 S1 C10 C11 -23.98(18) . . . . ? Cu1 S1 C1 C2 -67.95(15) . . . . ? Cu1 S2 C13 C14 -26.77(17) . . . . ? Cu1 S2 C4 C5 -66.88(15) . . . . ? Cu1 S3 C7 C8 -66.97(15) . . . . ? Cu1 S3 C16 C17 -23.15(18) . . . . ? Cu1 N1 C6 C5 57.6(2) . . . . ? Cu1 N1 C3 C2 56.4(2) . . . . ? Cu1 N1 C9 C8 56.4(2) . . . . ? Cu1B S3B C16B C17B 26.18(18) . . . . ? Cu1B S3B C7B C8B 67.45(15) . . . . ? Cu1B S1B C10B C11B 25.06(18) . . . . ? Cu1B S1B C1B C2B 66.27(15) . . . . ? Cu1B S2B C4B C5B 67.07(15) . . . . ? Cu1B S2B C13B C14B 23.84(18) . . . . ? Cu1B N1B C3B C2B -57.0(2) . . . . ? Cu1B N1B C9B C8B -56.4(2) . . . . ? Cu1B N1B C6B C5B -56.3(2) . . . . ? S4 C12 C11 C10 -168.76(15) . . . . ? S5 C15 C14 C13 -167.18(15) . . . . ? S6B C18B C17B C16B 166.70(15) . . . . ? S1B C10B C11B C12B 175.73(15) . . . . ? S1B C1B C2B C3B -78.6(2) . . . . ? S2B C13B C14B C15B 172.23(15) . . . . ? S2 C4 C5 C6 78.6(2) . . . . ? S3 C16 C17 C18 -171.88(15) . . . . ? O3B S4B O1B Na1 19.73(11) . . . . ? O3B S4B O1B Na6 173.69(19) . . . 1_665 ? O3B S4B C12B C11B -64.53(18) . . . . ? O3 S4 O1 Na3 -58.30(19) . . . . ? O3 S4 O1 Na6 44.80(10) . . . . ? O3 S4 C12 C11 -175.12(15) . . . . ? O1 S4 O3 Na1 -116.71(15) . . . 1_445 ? O1 S4 O3 Na2 75.99(15) . . . 1_445 ? O1 S4 C12 C11 65.31(18) . . . . ? O6 S5 O5 Na5 -156.10(12) . . . . ? O6 S5 O5 Na4 -43.90(13) . . . . ? O6 S5 C15 C14 63.68(17) . . . . ? O5 S5 O6 Na3 -51.55(14) . . . . ? O5 S5 C15 C14 -177.16(15) . . . . ? O5B S5B O4B Na5 -11.83(11) . . . . ? O5B S5B O4B Na4 66.7(2) . . . . ? O5B S5B C15B C14B 179.13(17) . . . . ? O6B S5B O5B Na5 -113.36(10) . . . . ? O6B S5B O5B Na2 -29.3(2) . . . 1_545 ? O6B S5B O4B Na5 115.52(9) . . . . ? O6B S5B O4B Na4 -165.94(19) . . . . ? O6B S5B C15B C14B 57.44(18) . . . . ? O4B S5B O5B Na5 13.09(12) . . . . ? O4B S5B O5B Na2 97.13(19) . . . 1_545 ? O4B S5B C15B C14B -62.01(19) . . . . ? O9B S6B O7B Na3 52.01(13) . . . . ? O9B S6B C18B C17B -58.77(17) . . . . ? O7B S6B O9B Na4 53.47(14) . . . . ? O7B S6B C18B C17B -178.75(15) . . . . ? O8B S6B O9B Na4 179.94(10) . . . . ? O8B S6B O7B Na3 -74.18(13) . . . . ? O8B S6B C18B C17B 60.82(17) . . . . ? O1B S4B O3B Na4 66.89(15) . . . . ? O1B S4B O3B Na1 -19.16(10) . . . . ? O1B S4B C12B C11B 176.58(15) . . . . ? O2B S4B O3B Na4 -166.33(12) . . . . ? O2B S4B O3B Na1 107.62(9) . . . . ? O2B S4B O1B Na1 -106.44(10) . . . . ? O2B S4B O1B Na6 47.5(2) . . . 1_665 ? O2B S4B C12B C11B 54.82(18) . . . . ? O4 S5 O6 Na3 -178.20(10) . . . . ? O4 S5 O5 Na5 -29.51(16) . . . . ? O4 S5 O5 Na4 82.69(12) . . . . ? O4 S5 C15 C14 -56.36(17) . . . . ? O7 S6 C18 C17 68.77(18) . . . . ? O9 S6 O7 Na3 -72.0(2) . . . . ? O9 S6 C18 C17 -172.06(16) . . . . ? O8 S6 O7 Na3 160.75(17) . . . . ? O8 S6 C18 C17 -52.15(18) . . . . ? O2 S4 O3 Na1 10.18(18) . . . 1_445 ? O2 S4 O3 Na2 -157.11(12) . . . 1_445 ? O2 S4 O1 Na3 174.63(14) . . . . ? O2 S4 O1 Na6 -82.27(10) . . . . ? O2 S4 C12 C11 -55.20(18) . . . . ? N1B C9B C8B C7B 69.9(3) . . . . ? N1B C6B C5B C4B 70.9(3) . . . . ? N1 C3 C2 C1 -69.7(3) . . . . ? N1 C9 C8 C7 -70.5(3) . . . . ? C12 C11 C10 S1 -175.46(15) . . . . ? C10 S1 C1 C2 176.18(15) . . . . ? C18B C17B C16B S3B -179.33(15) . . . . ? C16B S3B C7B C8B -176.25(15) . . . . ? C10B S1B C1B C2B -177.94(15) . . . . ? C10B C11B C12B S4B 168.21(15) . . . . ? C1B S1B C10B C11B -77.84(17) . . . . ? C1B C2B C3B N1B 71.3(3) . . . . ? C3B N1B C9B C8B 65.1(2) . . . . ? C3B N1B C6B C5B -177.93(18) . . . . ? C9B N1B C3B C2B -179.13(18) . . . . ? C9B N1B C6B C5B 66.3(2) . . . . ? C9B C8B C7B S3B -78.4(2) . . . . ? C7B S3B C16B C17B -77.31(17) . . . . ? C6B N1B C3B C2B 65.0(2) . . . . ? C6B N1B C9B C8B -178.85(18) . . . . ? C6B C5B C4B S2B -79.3(2) . . . . ? C4B S2B C13B C14B -78.68(17) . . . . ? C13B S2B C4B C5B -176.57(15) . . . . ? C13B C14B C15B S5B 166.69(16) . . . . ? C15 C14 C13 S2 -178.57(15) . . . . ? C13 S2 C4 C5 176.98(15) . . . . ? C4 S2 C13 C14 76.33(17) . . . . ? C4 C5 C6 N1 -71.2(3) . . . . ? C6 N1 C3 C2 178.11(18) . . . . ? C6 N1 C9 C8 -64.9(2) . . . . ? C3 N1 C6 C5 -65.0(2) . . . . ? C3 N1 C9 C8 179.16(18) . . . . ? C3 C2 C1 S1 79.0(2) . . . . ? C1 S1 C10 C11 78.94(18) . . . . ? C9 N1 C6 C5 179.18(18) . . . . ? C9 N1 C3 C2 -65.9(2) . . . . ? C9 C8 C7 S3 78.7(2) . . . . ? C7 S3 C16 C17 79.61(17) . . . . ? C16 S3 C7 C8 176.69(15) . . . . ? C16 C17 C18 S6 -169.88(15) . . . . ? _shelx_estimated_absorpt_T_max 0.733 _shelx_estimated_absorpt_T_min 0.494 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelxl_version_number 2013-4 data_12 _audit_creation_date 2013-02-27 _audit_creation_method ; Olex2 1.2-beta (compiled Dec 5 2012 16:17:34, GUI svn.r4385) ; _publ_section_references ; Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122 Petricek,V., Dusek,M. & Palatinus,L.(2006). Jana2006. The crystallographic computing system. Institute of Physics, Praha, Czech Republic. Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. Bruker (2011). APEX2 Version 2011.2-4. Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2009). SAINT-Plus Version 7.68a. Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (2008). SADABS Version 2008-1. Bruker AXS Inc., Madison, Wisconsin, USA. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'F6 P, C16 H32 Cu O4 S4, C2 H6 O' _chemical_formula_sum 'C18 H38 Cu F6 O5 P S4' _chemical_formula_weight 671.28 _chemical_melting_point ? 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' 'Cu' 'Cu' 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'F' 'F' 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.4862(5) _cell_length_b 13.6947(4) _cell_length_c 15.8096(5) _cell_angle_alpha 71.5710(10) _cell_angle_beta 77.6760(10) _cell_angle_gamma 78.8850(10) _cell_volume 2681.45(15) _cell_formula_units_Z 4 _cell_measurement_reflns_used 9668 _cell_measurement_temperature 110(2) _cell_measurement_theta_max 40.617 _cell_measurement_theta_min 2.377 _exptl_absorpt_coefficient_mu 1.256 _exptl_absorpt_correction_T_max 0.9848 _exptl_absorpt_correction_T_min 0.6912 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2012/1 (Bruker,2012) was used for absorption correction. wR2(int) was 0.0617 before and 0.0473 after correction. The Ratio of minimum to maximum transmission is 0.7019. The \l/2 correction factor is 0.0015. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.663 _exptl_crystal_density_meas . _exptl_crystal_density_method ? _exptl_crystal_description prism _exptl_crystal_F_000 1392 _exptl_crystal_size_max 0.712 _exptl_crystal_size_mid 0.356 _exptl_crystal_size_min 0.184 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents 0.0385 _diffrn_reflns_av_unetI/netI 0.0352 _diffrn_reflns_Laue_measured_fraction_full 0.995 _diffrn_reflns_Laue_measured_fraction_max 0.972 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -24 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 110771 _diffrn_reflns_point_group_measured_fraction_full 0.995 _diffrn_reflns_point_group_measured_fraction_max 0.972 _diffrn_reflns_theta_full 35.000 _diffrn_reflns_theta_max 40.718 _diffrn_reflns_theta_min 1.376 _diffrn_ambient_temperature 110(2) _diffrn_detector_area_resol_mean 512 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.972 _diffrn_measurement_device_type 'Bruker D8 diffractometer with APEX2 detector' _diffrn_measurement_method '\f and \w scans with a narrow frame width' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 28769 _reflns_number_total 33773 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT v7.68A (Bruker, 2009)' _computing_data_collection 'APEX2 v2011.2-4 (Bruker, 2011)' _computing_data_reduction 'SAINT v7.68A (Bruker, 2009)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 1.974 _refine_diff_density_min -0.883 _refine_diff_density_rms 0.105 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 683 _refine_ls_number_reflns 33773 _refine_ls_number_restraints 253 _refine_ls_R_factor_all 0.0454 _refine_ls_R_factor_gt 0.0374 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0543P)^2^+0.8792P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0959 _refine_ls_wR_factor_ref 0.1019 _refine_special_details ; ? ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: {H10A,H10B} of C10, {H14A,H14B} of C14, H1 of O1, H4 of O4, {H28A,H28B} of C28, H3 of O3, {H29A,H29B} of C29, {H30A,H30B} of C30, {H31A,H31B} of C31, {H32A,H32B} of C32, H5 of O5, H6 of O6, H7 of O7, H8 of O8, {H11A,H11B} of C11, {H27A,H27B} of C27, {H26A,H26B} of C26, {H25A,H25B} of C25, {H13A,H13B} of C13, {H23A,H23B} of C23, {H19A,H19B} of C19, {H17A,H17B} of C17, {H9A,H9B} of C9, {H4A,H4B} of C4, H2 of O2, {H20C,H20D} of C20', H9 of O9, {H22C,H22D} of C22', {H21A,H21B} of C21, {H20A,H20B} of C20, {H22A,H22B} of C22, {H21C, H21D} of C21', {H3A,H3B} of C3, {H6A,H6B} of C6, {H15A,H15B} of C15, {H7A, H7B} of C7, {H5A,H5B} of C5, {H1A,H1B} of C1, {H12A,H12B} of C12, {H16A,H16B} of C16, {H33A,H33B} of C33, H10 of O10, {H35A,H35B} of C35 At 1.5 times of: {H36A,H36B,H36C} of C36, {H34A,H34B,H34C} of C34 2. Restrained distances C21-C20' ~ C21'-C20' with sigma of 0.005 C22'-C21 ~ C22'-C21' with sigma of 0.005 S6-C20 ~ S6-C20' with sigma of 0.005 S7-C22' ~ S7-C22 with sigma of 0.005 P2B-F9B ~ P2B-F7B ~ P2B-F11B ~ P2B-F12B ~ P2B-F10B ~ P2B-F8B with sigma of 0.005 3. Uiso/Uaniso restraints and constraints Uiso(C20) = Uiso(C20') Uiso(C22) = Uiso(C22') Uanis(P1A) = Uanis(P1B) Uanis(F1A) = Uanis(F1B) Uanis(F2A) = Uanis(F2B) Uanis(F3A) = Uanis(F3B) Uanis(F4A) = Uanis(F4B) Uanis(F5A) = Uanis(F5B) Uanis(F6A) = Uanis(F6B) Uanis(P2A) = Uanis(P2B) Uanis(F9A) = Uanis(F9B) Uanis(F11A) = Uanis(F11B) Uanis(F8A) = Uanis(F8B) Uanis(F10A) = Uanis(F10B) Uanis(F7A) = Uanis(F7B) Uanis(F12A) = Uanis(F12B) 4. Same fragment restrains {P2B, F7B, F8B, F9B, F10B, F11B, F12B} as {P2A, F7A, F8A, F9A, F10A, F11A, F12A} {C20', C21', C22'} as {C20, C21, C22} {P1B, F1B, F2B, F3B, F4B, F5B, F6B} as {P1A, F1A, F2A, F3A, F4A, F5A, F6A} 5. Others Sof(P1A)=Sof(F1A)=Sof(F2A)=Sof(F3A)=Sof(F4A)=Sof(F5A)=Sof(F6A)=1-Sof(F1A)=1- Sof(F1A)=1-Sof(F1A)=1-Sof(F1A)=1-Sof(F1A)=1-Sof(F1A)=1-Sof(F1A) Sof(C20)=Sof(H20A)=Sof(H20B)=Sof(C21)=Sof(H21A)=Sof(H21B)=Sof(C22)=Sof(H22A)= Sof(H22B)=1-Sof(H20A)=1-Sof(H20A)=1-Sof(H20A)=1-Sof(H20A)=1-Sof(H20A)=1- Sof(H20A)=1-Sof(H20A)=1-Sof(H20A)=1-Sof(H20A) Sof(P2A)=Sof(F7A)=Sof(F8A)=Sof(F9A)=Sof(F10A)=Sof(F11A)=Sof(F12A)=1-Sof(F7A)= 1-Sof(F7A)=1-Sof(F7A)=1-Sof(F7A)=1-Sof(F7A)=1-Sof(F7A)=1-Sof(F7A) 6.a Secondary CH2 refined with riding coordinates: C17(H17A,H17B), C19(H19A,H19B), C23(H23A,H23B), C25(H25A,H25B), C26(H26A, H26B), C27(H27A,H27B), C28(H28A,H28B), C29(H29A,H29B), C30(H30A,H30B), C31(H31A,H31B), C32(H32A,H32B), C4(H4A,H4B), C14(H14A,H14B), C10(H10A,H10B), C11(H11A,H11B), C13(H13A,H13B), C9(H9A,H9B), C3(H3A,H3B), C6(H6A,H6B), C15(H15A,H15B), C7(H7A,H7B), C5(H5A,H5B), C1(H1A,H1B), C12(H12A,H12B), C16(H16A,H16B), C33(H33A,H33B), C35(H35A,H35B), C20(H20A,H20B), C21(H21A,H21B), C22(H22A,H22B), C20'(H20C,H20D), C21'(H21C,H21D), C22'(H22C,H22D) 6.b Idealised Me refined as rotating group: C34(H34A,H34B,H34C), C36(H36A,H36B,H36C) 6.c Idealised tetrahedral OH refined as rotating group: O5(H5), O6(H6), O7(H7), O8(H8), O2(H2), O4(H4), O1(H1), O3(H3), O10(H10), O9(H9) ; _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary ? 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group P2A P 0.24142(10) -0.24172(10) 0.99985(8) 0.01883(9) Uani 0.808(3) 1 d D U P A 1 F7A F 0.14607(10) -0.30651(13) 1.03126(12) 0.0275(3) Uani 0.808(3) 1 d D U P A 1 F8A F 0.33887(16) -0.18043(15) 0.9710(2) 0.0410(5) Uani 0.808(3) 1 d D U P A 1 F9A F 0.16811(12) -0.13797(10) 0.95897(15) 0.0504(4) Uani 0.808(3) 1 d D U P A 1 F10A F 0.26515(12) -0.26486(11) 0.90412(7) 0.0341(3) Uani 0.808(3) 1 d D U P A 1 F11A F 0.21947(15) -0.21871(19) 1.09560(11) 0.0572(6) Uani 0.808(3) 1 d D U P A 1 F12A F 0.31534(11) -0.34938(12) 1.03870(12) 0.0462(3) Uani 0.808(3) 1 d D U P A 1 P2B P 0.2475(4) -0.2429(4) 1.0060(3) 0.01883(9) Uani 0.192(3) 1 d D U P A 2 F7B F 0.1647(5) -0.3214(6) 1.0391(6) 0.0275(3) Uani 0.192(3) 1 d D U P A 2 F8B F 0.3225(8) -0.1566(8) 0.9657(10) 0.0410(5) Uani 0.192(3) 1 d D U P A 2 F9B F 0.1563(5) -0.1505(4) 1.0081(6) 0.0504(4) Uani 0.192(3) 1 d D U P A 2 F10B F 0.2371(5) -0.2342(5) 0.9059(3) 0.0341(3) Uani 0.192(3) 1 d D U P A 2 F11B F 0.2499(7) -0.2597(8) 1.1094(4) 0.0572(6) Uani 0.192(3) 1 d D U P A 2 F12B F 0.3304(5) -0.3428(5) 1.0044(5) 0.0462(3) Uani 0.192(3) 1 d D U P A 2 C17 C 0.58342(6) 0.02405(7) 0.73470(6) 0.01484(12) Uani 1 1 d . . . . . H17A H 0.6099 -0.0463 0.7700 0.018 Uiso 1 1 calc R U . . . H17B H 0.6429 0.0546 0.6932 0.018 Uiso 1 1 calc R U . . . C18 C 0.54336(6) 0.08919(6) 0.80173(5) 0.01283(11) Uani 1 1 d . . . . . C19 C 0.51288(7) 0.20517(7) 0.75415(6) 0.01537(12) Uani 1 1 d . . . . . H19A H 0.5608 0.2250 0.6966 0.018 Uiso 1 1 calc R U . . . H19B H 0.5221 0.2465 0.7925 0.018 Uiso 1 1 calc R U . . . C23 C 0.23078(7) 0.25582(7) 0.48771(6) 0.01533(12) Uani 1 1 d . . . . . H23A H 0.1886 0.2702 0.5430 0.018 Uiso 1 1 calc R U . . . H23B H 0.2141 0.3155 0.4356 0.018 Uiso 1 1 calc R U . . . C24 C 0.20172(6) 0.15770(6) 0.47710(5) 0.01311(11) Uani 1 1 d . . . . . C25 C 0.24233(7) 0.05559(6) 0.54361(6) 0.01522(12) Uani 1 1 d . . . . . H25A H 0.3158 0.0367 0.5218 0.018 Uiso 1 1 calc R U . . . H25B H 0.2054 -0.0006 0.5443 0.018 Uiso 1 1 calc R U . . . C26 C 0.25290(8) -0.07334(7) 0.71881(7) 0.01984(15) Uani 1 1 d . . . . . H26A H 0.2386 -0.0801 0.7843 0.024 Uiso 1 1 calc R U . . . H26B H 0.2032 -0.1100 0.7068 0.024 Uiso 1 1 calc R U . . . C27 C 0.36014(8) -0.13016(7) 0.69752(7) 0.01900(14) Uani 1 1 d . . . . . H27A H 0.3809 -0.1118 0.6311 0.023 Uiso 1 1 calc R U . . . H27B H 0.3569 -0.2058 0.7196 0.023 Uiso 1 1 calc R U . . . C28 C 0.44310(8) -0.10702(7) 0.73814(7) 0.02051(16) Uani 1 1 d . . . . . H28A H 0.4973 -0.1676 0.7476 0.025 Uiso 1 1 calc R U . . . H28B H 0.4129 -0.0960 0.7978 0.025 Uiso 1 1 calc R U . . . C29 C 0.24822(7) 0.14439(7) 0.38310(6) 0.01541(12) Uani 1 1 d . . . . . H29A H 0.3234 0.1428 0.3737 0.018 Uiso 1 1 calc R U . . . H29B H 0.2344 0.0771 0.3803 0.018 Uiso 1 1 calc R U . . . C30 C 0.08414(7) 0.17343(7) 0.49023(6) 0.01705(13) Uani 1 1 d . . . . . H30A H 0.0554 0.1818 0.5510 0.020 Uiso 1 1 calc R U . . . H30B H 0.0597 0.2369 0.4446 0.020 Uiso 1 1 calc R U . . . C31 C 0.45780(6) 0.04233(7) 0.87545(5) 0.01411(12) Uani 1 1 d . . . . . H31A H 0.3981 0.0426 0.8482 0.017 Uiso 1 1 calc R U . . . H31B H 0.4820 -0.0304 0.9073 0.017 Uiso 1 1 calc R U . . . C32 C 0.63603(7) 0.08954(7) 0.84530(6) 0.01601(13) Uani 1 1 d . . . . . H32A H 0.6893 0.1237 0.7975 0.019 Uiso 1 1 calc R U . . . H32B H 0.6136 0.1311 0.8888 0.019 Uiso 1 1 calc R U . . . O5 O 0.20735(6) 0.22649(6) 0.31215(5) 0.01764(11) Uani 1 1 d . . . . . H5 H 0.2554 0.2477 0.2706 0.021 Uiso 1 1 calc R U . . . O6 O 0.05146(6) 0.08521(7) 0.48075(7) 0.02640(15) Uani 1 1 d . . . . . H6 H -0.0127 0.0897 0.4939 0.032 Uiso 1 1 calc R U . . . O7 O 0.42907(6) 0.10266(6) 0.93746(5) 0.01850(11) Uani 1 1 d . . . . . H7 H 0.3934 0.0700 0.9846 0.022 Uiso 1 1 calc R U . . . O8 O 0.67959(5) -0.01182(6) 0.89099(5) 0.01784(11) Uani 1 1 d . . . . . H8 H 0.7259 -0.0352 0.8549 0.021 Uiso 1 1 calc R U . . . S5 S 0.49982(2) 0.00779(2) 0.66499(2) 0.01454(3) Uani 1 1 d . . . . . S6 S 0.38255(2) 0.24101(2) 0.72977(2) 0.01574(4) Uani 1 1 d D . . . . S7 S 0.36588(2) 0.24582(2) 0.49491(2) 0.01648(4) Uani 1 1 d D . . . . S8 S 0.22745(2) 0.06421(2) 0.65829(2) 0.01438(3) Uani 1 1 d . . . . . Cu2 Cu 0.37022(2) 0.14190(2) 0.64329(2) 0.01524(2) Uani 1 1 d . . . . . C4 C 0.02349(7) 0.62589(7) 0.76882(7) 0.01842(14) Uani 1 1 d . . . . . H4A H 0.0545 0.6187 0.7080 0.022 Uiso 1 1 calc R U . . . H4B H -0.0335 0.6839 0.7617 0.022 Uiso 1 1 calc R U . . . O2 O 0.47005(5) 0.42563(6) 0.97218(5) 0.01836(11) Uani 1 1 d . . . . . H2 H 0.5320 0.4034 0.9760 0.022 Uiso 1 1 calc R U . . . O4 O -0.10390(6) 0.35869(7) 0.58848(5) 0.02180(13) Uani 1 1 d . . . . . H4 H -0.1510 0.3317 0.5809 0.026 Uiso 1 1 calc R U . . . O1 O 0.34766(5) 0.29421(6) 1.16285(5) 0.01727(11) Uani 1 1 d . . . . . H1 H 0.3990 0.3164 1.1685 0.021 Uiso 1 1 calc R U . . . C14 C 0.41964(6) 0.34355(7) 0.97065(6) 0.01443(12) Uani 1 1 d . . . . . H14A H 0.4502 0.2764 1.0081 0.017 Uiso 1 1 calc R U . . . H14B H 0.4286 0.3396 0.9080 0.017 Uiso 1 1 calc R U . . . C10 C 0.10514(7) 0.15664(7) 1.01899(6) 0.01659(13) Uani 1 1 d . . . . . H10A H 0.1306 0.1086 1.0738 0.020 Uiso 1 1 calc R U . . . H10B H 0.0308 0.1536 1.0276 0.020 Uiso 1 1 calc R U . . . C11 C 0.15714(8) 0.11539(7) 0.93891(7) 0.01845(14) Uani 1 1 d . . . . . H11A H 0.2236 0.1425 0.9146 0.022 Uiso 1 1 calc R U . . . H11B H 0.1718 0.0388 0.9612 0.022 Uiso 1 1 calc R U . . . S3 S 0.25027(2) 0.46576(2) 0.83720(2) 0.01295(3) Uani 1 1 d . . . . . S4 S 0.12165(2) 0.28806(2) 1.01289(2) 0.01297(3) Uani 1 1 d . . . . . C13 C 0.28919(6) 0.37535(7) 1.10386(6) 0.01457(12) Uani 1 1 d . . . . . H13A H 0.3084 0.4430 1.1001 0.017 Uiso 1 1 calc R U . . . H13B H 0.2156 0.3756 1.1301 0.017 Uiso 1 1 calc R U . . . C8 C 0.30514(6) 0.36406(6) 1.00758(5) 0.01197(11) Uani 1 1 d . . . . . S2 S -0.02636(2) 0.50589(2) 0.83882(2) 0.01341(3) Uani 1 1 d . . . . . O3 O -0.01070(6) 0.56467(6) 0.58087(5) 0.01955(12) Uani 1 1 d . . . . . H3 H 0.0293 0.5860 0.5325 0.023 Uiso 1 1 calc R U . . . C9 C 0.26031(6) 0.26862(6) 1.00809(6) 0.01415(12) Uani 1 1 d . . . . . H9A H 0.2781 0.2103 1.0608 0.017 Uiso 1 1 calc R U . . . H9B H 0.2934 0.2480 0.9529 0.017 Uiso 1 1 calc R U . . . Cu1 Cu 0.10942(2) 0.38157(2) 0.86474(2) 0.01319(2) Uani 1 1 d . . . . . S1 S 0.10854(2) 0.27293(2) 0.78343(2) 0.01381(3) Uani 1 1 d . . . . . C3 C -0.10286(6) 0.48222(7) 0.76694(6) 0.01483(12) Uani 1 1 d . . . . . H3A H -0.1619 0.4494 0.8070 0.018 Uiso 1 1 calc R U . . . H3B H -0.1309 0.5508 0.7297 0.018 Uiso 1 1 calc R U . . . C2 C -0.05379(6) 0.41542(7) 0.70234(5) 0.01307(11) Uani 1 1 d . . . . . C6 C 0.21423(7) 0.60347(7) 0.78438(6) 0.01762(14) Uani 1 1 d . . . . . H6A H 0.2607 0.6425 0.7978 0.021 Uiso 1 1 calc R U . . . H6B H 0.2269 0.6153 0.7181 0.021 Uiso 1 1 calc R U . . . C15 C 0.03152(6) 0.46491(7) 0.62998(6) 0.01453(12) Uani 1 1 d . . . . . H15A H 0.0876 0.4711 0.6587 0.017 Uiso 1 1 calc R U . . . H15B H 0.0599 0.4212 0.5888 0.017 Uiso 1 1 calc R U . . . C7 C 0.25533(6) 0.46821(6) 0.95065(5) 0.01355(11) Uani 1 1 d . . . . . H7A H 0.2948 0.5240 0.9464 0.016 Uiso 1 1 calc R U . . . H7B H 0.1849 0.4847 0.9815 0.016 Uiso 1 1 calc R U . . . C5 C 0.10407(7) 0.65055(7) 0.81142(7) 0.01808(14) Uani 1 1 d . . . . . H5A H 0.1014 0.7269 0.7947 0.022 Uiso 1 1 calc R U . . . H5B H 0.0855 0.6255 0.8780 0.022 Uiso 1 1 calc R U . . . C1 C -0.01854(7) 0.30173(7) 0.75190(6) 0.01513(12) Uani 1 1 d . . . . . H1A H -0.0206 0.2583 0.7130 0.018 Uiso 1 1 calc R U . . . H1B H -0.0689 0.2801 0.8076 0.018 Uiso 1 1 calc R U . . . C12 C 0.09582(8) 0.14330(7) 0.86190(7) 0.01935(15) Uani 1 1 d . . . . . H12A H 0.0226 0.1394 0.8878 0.023 Uiso 1 1 calc R U . . . H12B H 0.1188 0.0913 0.8278 0.023 Uiso 1 1 calc R U . . . C16 C -0.14247(7) 0.41117(8) 0.65641(6) 0.01764(14) Uani 1 1 d . . . . . H16A H -0.1955 0.3739 0.7021 0.021 Uiso 1 1 calc R U . . . H16B H -0.1743 0.4826 0.6286 0.021 Uiso 1 1 calc R U . . . C33 C 0.93150(8) -0.05965(10) 0.73825(8) 0.02388(17) Uani 1 1 d . . . . . H33A H 0.9534 -0.0655 0.6760 0.029 Uiso 1 1 calc R U . . . H33B H 0.9824 -0.1044 0.7757 0.029 Uiso 1 1 calc R U . . . C34 C 0.92550(10) 0.05153(10) 0.73771(9) 0.0293(2) Uani 1 1 d . . . . . H34A H 0.8793 0.0962 0.6966 0.044 Uiso 1 1 calc R U . . . H34B H 0.9939 0.0731 0.7173 0.044 Uiso 1 1 calc R U . . . H34C H 0.8994 0.0576 0.7989 0.044 Uiso 1 1 calc R U . . . O10 O 0.50537(6) 0.38661(6) 0.17202(5) 0.02139(12) Uani 1 1 d . . . . . H10 H 0.5182 0.4353 0.1249 0.026 Uiso 1 1 calc R U . . . C35 C 0.49238(8) 0.42337(9) 0.24939(7) 0.02327(17) Uani 1 1 d . . . . . H35A H 0.5560 0.4492 0.2495 0.028 Uiso 1 1 calc R U . . . H35B H 0.4809 0.3648 0.3048 0.028 Uiso 1 1 calc R U . . . O9 O 0.83241(6) -0.09272(6) 0.77450(5) 0.02099(12) Uani 1 1 d . . . . . H9 H 0.8258 -0.1390 0.7525 0.025 Uiso 1 1 calc R U . . . C36 C 0.40391(11) 0.50900(12) 0.25133(8) 0.0331(3) Uani 1 1 d . . . . . H36A H 0.4139 0.5665 0.1959 0.050 Uiso 1 1 calc R U . . . H36B H 0.4002 0.5337 0.3039 0.050 Uiso 1 1 calc R U . . . H36C H 0.3400 0.4825 0.2555 0.050 Uiso 1 1 calc R U . . . C20 C 0.40395(14) 0.36959(11) 0.64952(11) 0.01610(19) Uiso 0.641(3) 1 d D . P B 1 H20A H 0.3944 0.4212 0.6834 0.019 Uiso 0.641(3) 1 calc R U P B 1 H20B H 0.4753 0.3659 0.6170 0.019 Uiso 0.641(3) 1 calc R U P B 1 C21 C 0.32922(11) 0.40533(11) 0.58032(9) 0.0169(3) Uiso 0.641(3) 1 d D . P B 1 H21A H 0.2649 0.3758 0.6103 0.020 Uiso 0.641(3) 1 calc R U P B 1 H21B H 0.3125 0.4818 0.5659 0.020 Uiso 0.641(3) 1 calc R U P B 1 C22 C 0.36109(14) 0.38002(13) 0.49826(12) 0.0186(2) Uiso 0.641(3) 1 d D . P B 1 H22A H 0.4306 0.3999 0.4735 0.022 Uiso 0.641(3) 1 calc R U P B 1 H22B H 0.3154 0.4253 0.4558 0.022 Uiso 0.641(3) 1 calc R U P B 1 C20' C 0.3789(2) 0.37480(18) 0.66180(18) 0.01610(19) Uiso 0.359(3) 1 d D . P B 2 H20C H 0.3065 0.4073 0.6645 0.019 Uiso 0.359(3) 1 calc R U P B 2 H20D H 0.4142 0.4115 0.6890 0.019 Uiso 0.359(3) 1 calc R U P B 2 C21' C 0.4266(2) 0.3912(2) 0.56473(17) 0.0217(5) Uiso 0.359(3) 1 d D . P B 2 H21C H 0.4942 0.3473 0.5651 0.026 Uiso 0.359(3) 1 calc R U P B 2 H21D H 0.4409 0.4641 0.5425 0.026 Uiso 0.359(3) 1 calc R U P B 2 C22' C 0.3807(2) 0.3745(2) 0.4908(2) 0.0186(2) Uiso 0.359(3) 1 d D . P B 2 H22C H 0.4237 0.4041 0.4323 0.022 Uiso 0.359(3) 1 calc R U P B 2 H22D H 0.3123 0.4166 0.4898 0.022 Uiso 0.359(3) 1 calc R U P B 2 P1A P 0.70919(12) 0.27977(13) 0.48730(10) 0.02206(11) Uani 0.3068(17) 1 d D . P C 1 F1A F 0.7916(4) 0.3586(4) 0.4427(4) 0.0435(6) Uani 0.3068(17) 1 d D . P C 1 F2A F 0.6240(3) 0.2046(3) 0.5349(3) 0.0450(5) Uani 0.3068(17) 1 d D . P C 1 F3A F 0.7588(5) 0.2136(4) 0.4186(3) 0.0376(3) Uani 0.3068(17) 1 d D . P C 1 F4A F 0.6607(3) 0.3462(4) 0.5578(2) 0.0487(5) Uani 0.3068(17) 1 d D . P C 1 F5A F 0.6350(4) 0.3519(5) 0.4187(4) 0.0441(3) Uani 0.3068(17) 1 d D . P C 1 F6A F 0.7819(3) 0.2104(4) 0.5572(3) 0.0641(6) Uani 0.3068(17) 1 d D . P C 1 P1B P 0.73318(5) 0.25107(6) 0.48692(4) 0.02206(11) Uani 0.6932(17) 1 d D U P C 2 F1B F 0.81264(16) 0.33370(17) 0.44147(17) 0.0435(6) Uani 0.6932(17) 1 d D U P C 2 F2B F 0.65298(15) 0.17078(14) 0.53161(13) 0.0450(5) Uani 0.6932(17) 1 d D U P C 2 F3B F 0.7685(2) 0.20630(18) 0.40154(12) 0.0376(3) Uani 0.6932(17) 1 d D U P C 2 F4B F 0.70105(14) 0.29776(18) 0.57245(10) 0.0487(5) Uani 0.6932(17) 1 d D U P C 2 F5B F 0.64816(18) 0.33306(18) 0.43526(15) 0.0441(3) Uani 0.6932(17) 1 d D U P C 2 F6B F 0.81870(16) 0.1714(2) 0.53769(12) 0.0641(6) Uani 0.6932(17) 1 d D U P C 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 P2A 0.01808(19) 0.02262(11) 0.01727(19) -0.00700(13) -0.00045(13) -0.00678(12) F7A 0.0226(6) 0.0332(6) 0.0289(5) -0.0060(4) -0.0049(4) -0.0129(5) F8A 0.0386(9) 0.0552(11) 0.0355(6) -0.0164(9) 0.0094(7) -0.0324(9) F9A 0.0482(7) 0.0205(4) 0.0710(11) -0.0069(6) -0.0026(7) 0.0036(4) F10A 0.0528(8) 0.0309(6) 0.0203(3) -0.0121(4) 0.0022(4) -0.0107(5) F11A 0.0587(11) 0.1007(16) 0.0330(6) -0.0406(8) 0.0190(6) -0.0533(10) F12A 0.0299(5) 0.0473(6) 0.0453(8) 0.0110(6) -0.0139(6) -0.0003(4) P2B 0.01808(19) 0.02262(11) 0.01727(19) -0.00700(13) -0.00045(13) -0.00678(12) F7B 0.0226(6) 0.0332(6) 0.0289(5) -0.0060(4) -0.0049(4) -0.0129(5) F8B 0.0386(9) 0.0552(11) 0.0355(6) -0.0164(9) 0.0094(7) -0.0324(9) F9B 0.0482(7) 0.0205(4) 0.0710(11) -0.0069(6) -0.0026(7) 0.0036(4) F10B 0.0528(8) 0.0309(6) 0.0203(3) -0.0121(4) 0.0022(4) -0.0107(5) F11B 0.0587(11) 0.1007(16) 0.0330(6) -0.0406(8) 0.0190(6) -0.0533(10) F12B 0.0299(5) 0.0473(6) 0.0453(8) 0.0110(6) -0.0139(6) -0.0003(4) C17 0.0138(3) 0.0174(3) 0.0145(3) -0.0070(2) -0.0029(2) -0.0002(2) C18 0.0128(3) 0.0144(3) 0.0114(3) -0.0042(2) -0.0017(2) -0.0016(2) C19 0.0159(3) 0.0148(3) 0.0150(3) -0.0038(2) -0.0016(2) -0.0029(2) C23 0.0174(3) 0.0129(3) 0.0159(3) -0.0040(2) -0.0045(2) -0.0007(2) C24 0.0143(3) 0.0124(3) 0.0123(3) -0.0034(2) -0.0030(2) -0.0005(2) C25 0.0194(3) 0.0127(3) 0.0134(3) -0.0031(2) -0.0050(2) -0.0003(2) C26 0.0226(4) 0.0165(3) 0.0167(3) 0.0020(3) -0.0031(3) -0.0053(3) C27 0.0239(4) 0.0130(3) 0.0207(4) -0.0022(3) -0.0082(3) -0.0032(3) C28 0.0269(4) 0.0140(3) 0.0211(4) 0.0001(3) -0.0114(3) -0.0040(3) C29 0.0172(3) 0.0162(3) 0.0122(3) -0.0044(2) -0.0033(2) 0.0007(2) C30 0.0149(3) 0.0178(3) 0.0177(3) -0.0046(3) -0.0026(3) -0.0016(2) C31 0.0141(3) 0.0150(3) 0.0120(3) -0.0029(2) -0.0015(2) -0.0015(2) C32 0.0143(3) 0.0181(3) 0.0169(3) -0.0061(3) -0.0041(2) -0.0016(2) O5 0.0184(3) 0.0198(3) 0.0123(2) -0.0010(2) -0.0035(2) -0.0020(2) O6 0.0198(3) 0.0249(3) 0.0380(4) -0.0111(3) -0.0050(3) -0.0076(3) O7 0.0212(3) 0.0198(3) 0.0128(2) -0.0060(2) 0.0019(2) -0.0017(2) O8 0.0157(2) 0.0211(3) 0.0148(2) -0.0036(2) -0.0035(2) 0.0009(2) S5 0.01718(8) 0.01378(7) 0.01348(7) -0.00472(6) -0.00417(6) -0.00084(6) S6 0.01896(8) 0.01292(7) 0.01534(8) -0.00329(6) -0.00617(7) 0.00029(6) S7 0.01880(8) 0.01661(8) 0.01325(8) -0.00039(6) -0.00403(6) -0.00561(7) S8 0.01565(8) 0.01451(8) 0.01157(7) -0.00186(6) -0.00167(6) -0.00251(6) Cu2 0.01912(5) 0.01251(4) 0.01435(4) -0.00155(3) -0.00649(3) -0.00251(3) C4 0.0190(3) 0.0141(3) 0.0210(4) -0.0019(3) -0.0072(3) -0.0005(3) O2 0.0149(2) 0.0218(3) 0.0203(3) -0.0065(2) -0.0016(2) -0.0077(2) O4 0.0231(3) 0.0306(4) 0.0167(3) -0.0100(3) -0.0039(2) -0.0092(3) O1 0.0170(2) 0.0187(3) 0.0142(2) 0.0003(2) -0.0052(2) -0.0036(2) C14 0.0123(3) 0.0156(3) 0.0160(3) -0.0052(2) -0.0017(2) -0.0028(2) C10 0.0192(3) 0.0159(3) 0.0150(3) -0.0012(2) -0.0044(3) -0.0069(3) C11 0.0218(4) 0.0135(3) 0.0208(4) -0.0038(3) -0.0088(3) 0.0001(3) S3 0.01276(7) 0.01321(7) 0.01172(7) -0.00236(6) -0.00132(6) -0.00183(6) S4 0.01176(7) 0.01437(7) 0.01219(7) -0.00261(6) -0.00170(6) -0.00269(6) C13 0.0146(3) 0.0159(3) 0.0125(3) -0.0036(2) -0.0024(2) -0.0010(2) C8 0.0119(3) 0.0118(3) 0.0121(3) -0.0028(2) -0.0025(2) -0.0018(2) S2 0.01299(7) 0.01418(7) 0.01326(7) -0.00503(6) -0.00282(6) 0.00027(6) O3 0.0206(3) 0.0173(3) 0.0154(3) 0.0004(2) -0.0019(2) 0.0005(2) C9 0.0120(3) 0.0124(3) 0.0180(3) -0.0032(2) -0.0040(2) -0.0017(2) Cu1 0.01395(4) 0.01198(4) 0.01374(4) -0.00260(3) -0.00465(3) -0.00120(3) S1 0.01437(7) 0.01302(7) 0.01384(7) -0.00388(6) -0.00344(6) -0.00011(6) C3 0.0123(3) 0.0186(3) 0.0139(3) -0.0061(2) -0.0025(2) 0.0000(2) C2 0.0122(3) 0.0159(3) 0.0114(3) -0.0041(2) -0.0028(2) -0.0011(2) C6 0.0181(3) 0.0141(3) 0.0175(3) 0.0009(3) -0.0033(3) -0.0035(2) C15 0.0142(3) 0.0159(3) 0.0123(3) -0.0035(2) -0.0013(2) -0.0011(2) C7 0.0153(3) 0.0123(3) 0.0129(3) -0.0032(2) -0.0037(2) -0.0010(2) C5 0.0190(3) 0.0132(3) 0.0226(4) -0.0052(3) -0.0059(3) -0.0004(2) C1 0.0148(3) 0.0153(3) 0.0157(3) -0.0035(2) -0.0041(2) -0.0027(2) C12 0.0280(4) 0.0133(3) 0.0183(3) -0.0032(3) -0.0092(3) -0.0028(3) C16 0.0153(3) 0.0232(4) 0.0157(3) -0.0061(3) -0.0045(3) -0.0026(3) C33 0.0188(4) 0.0312(5) 0.0234(4) -0.0123(4) 0.0008(3) -0.0047(3) C34 0.0273(5) 0.0268(5) 0.0324(5) -0.0043(4) -0.0020(4) -0.0105(4) O10 0.0223(3) 0.0233(3) 0.0184(3) -0.0052(2) -0.0020(2) -0.0058(2) C35 0.0204(4) 0.0291(5) 0.0220(4) -0.0085(4) -0.0059(3) -0.0027(3) O9 0.0201(3) 0.0261(3) 0.0204(3) -0.0111(3) -0.0011(2) -0.0065(2) C36 0.0330(6) 0.0395(6) 0.0206(4) -0.0092(4) -0.0015(4) 0.0077(5) P1A 0.0266(3) 0.0274(3) 0.01519(11) -0.00484(19) -0.00344(16) -0.0131(2) F1A 0.0496(11) 0.0685(13) 0.0269(4) -0.0250(8) 0.0127(6) -0.0438(11) F2A 0.0630(12) 0.0461(11) 0.0297(5) 0.0013(8) -0.0043(7) -0.0403(10) F3A 0.0627(8) 0.0324(5) 0.0232(8) -0.0135(5) -0.0067(7) -0.0107(5) F4A 0.0483(10) 0.0789(14) 0.0306(6) -0.0322(8) 0.0168(6) -0.0341(8) F5A 0.0373(8) 0.0442(10) 0.0405(10) -0.0020(7) -0.0048(6) -0.0001(6) F6A 0.0500(11) 0.0959(17) 0.0327(7) 0.0005(8) -0.0213(7) 0.0067(9) P1B 0.0266(3) 0.0274(3) 0.01519(11) -0.00484(19) -0.00344(16) -0.0131(2) F1B 0.0496(11) 0.0685(13) 0.0269(4) -0.0250(8) 0.0127(6) -0.0438(11) F2B 0.0630(12) 0.0461(11) 0.0297(5) 0.0013(8) -0.0043(7) -0.0403(10) F3B 0.0627(8) 0.0324(5) 0.0232(8) -0.0135(5) -0.0067(7) -0.0107(5) F4B 0.0483(10) 0.0789(14) 0.0306(6) -0.0322(8) 0.0168(6) -0.0341(8) F5B 0.0373(8) 0.0442(10) 0.0405(10) -0.0020(7) -0.0048(6) -0.0001(6) F6B 0.0500(11) 0.0959(17) 0.0327(7) 0.0005(8) -0.0213(7) 0.0067(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag P2A F7A 1.6051(12) . ? P2A F8A 1.6022(15) . ? P2A F9A 1.6014(16) . ? P2A F10A 1.5971(13) . ? P2A F11A 1.5977(14) . ? P2A F12A 1.6331(15) . ? P2B F7B 1.593(4) . ? P2B F8B 1.593(4) . ? P2B F9B 1.590(4) . ? P2B F10B 1.583(4) . ? P2B F11B 1.584(4) . ? P2B F12B 1.594(4) . ? C17 H17A 0.9900 . ? C17 H17B 0.9900 . ? C17 C18 1.5421(12) . ? C17 S5 1.8214(9) . ? C18 C19 1.5435(12) . ? C18 C31 1.5298(11) . ? C18 C32 1.5519(12) . ? C19 H19A 0.9900 . ? C19 H19B 0.9900 . ? C19 S6 1.8210(9) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C23 C24 1.5365(12) . ? C23 S7 1.8259(9) . ? C24 C25 1.5434(11) . ? C24 C29 1.5375(12) . ? C24 C30 1.5362(12) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C25 S8 1.8199(9) . ? C26 H26A 0.9900 . ? C26 H26B 0.9900 . ? C26 C27 1.5279(15) . ? C26 S8 1.8256(10) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C27 C28 1.5286(14) . ? C28 H28A 0.9900 . ? C28 H28B 0.9900 . ? C28 S5 1.8251(10) . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C29 O5 1.4330(11) . ? C30 H30A 0.9900 . ? C30 H30B 0.9900 . ? C30 O6 1.4228(12) . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C31 O7 1.4214(11) . ? C32 H32A 0.9900 . ? C32 H32B 0.9900 . ? C32 O8 1.4235(12) . ? O5 H5 0.8400 . ? O6 H6 0.8400 . ? O7 H7 0.8400 . ? O8 H8 0.8400 . ? S5 Cu2 2.2729(3) . ? S6 Cu2 2.2576(2) . ? S6 C20 1.8495(14) . ? S6 C20' 1.805(2) . ? S7 Cu2 2.3339(2) . ? S7 C22 1.8436(16) . ? S7 C22' 1.792(3) . ? S8 Cu2 2.3088(3) . ? C4 H4A 0.9900 . ? C4 H4B 0.9900 . ? C4 S2 1.8265(9) . ? C4 C5 1.5317(13) . ? O2 H2 0.8400 . ? O2 C14 1.4301(11) . ? O4 H4 0.8400 . ? O4 C16 1.4304(12) . ? O1 H1 0.8400 . ? O1 C13 1.4308(11) . ? C14 H14A 0.9900 . ? C14 H14B 0.9900 . ? C14 C8 1.5349(11) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.5278(14) . ? C10 S4 1.8259(9) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C11 C12 1.5251(13) . ? S3 Cu1 2.3024(2) . ? S3 C6 1.8205(9) . ? S3 C7 1.8204(8) . ? S4 C9 1.8258(8) . ? S4 Cu1 2.3108(2) . ? C13 H13A 0.9900 . ? C13 H13B 0.9900 . ? C13 C8 1.5438(11) . ? C8 C9 1.5395(11) . ? C8 C7 1.5403(11) . ? S2 Cu1 2.2577(2) . ? S2 C3 1.8230(9) . ? O3 H3 0.8400 . ? O3 C15 1.4183(11) . ? C9 H9A 0.9900 . ? C9 H9B 0.9900 . ? Cu1 S1 2.2558(2) . ? S1 C1 1.8222(9) . ? S1 C12 1.8315(9) . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C2 1.5449(12) . ? C2 C15 1.5297(12) . ? C2 C1 1.5383(12) . ? C2 C16 1.5443(12) . ? C6 H6A 0.9900 . ? C6 H6B 0.9900 . ? C6 C5 1.5296(14) . ? C15 H15A 0.9900 . ? C15 H15B 0.9900 . ? C7 H7A 0.9900 . ? C7 H7B 0.9900 . ? C5 H5A 0.9900 . ? C5 H5B 0.9900 . ? C1 H1A 0.9900 . ? C1 H1B 0.9900 . ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? C16 H16A 0.9900 . ? C16 H16B 0.9900 . ? C33 H33A 0.9900 . ? C33 H33B 0.9900 . ? C33 C34 1.5065(18) . ? C33 O9 1.4359(13) . ? C34 H34A 0.9800 . ? C34 H34B 0.9800 . ? C34 H34C 0.9800 . ? O10 H10 0.8400 . ? O10 C35 1.4297(13) . ? C35 H35A 0.9900 . ? C35 H35B 0.9900 . ? C35 C36 1.5058(18) . ? O9 H9 0.8400 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C20 C21 1.547(2) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C21 C22 1.406(2) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C20' H20C 0.9900 . ? C20' H20D 0.9900 . ? C20' C21' 1.495(3) . ? C21' H21C 0.9900 . ? C21' H21D 0.9900 . ? C21' C22' 1.527(4) . ? C22' H22C 0.9900 . ? C22' H22D 0.9900 . ? P1A F1A 1.595(3) . ? P1A F2A 1.594(3) . ? P1A F3A 1.589(3) . ? P1A F4A 1.612(3) . ? P1A F5A 1.600(3) . ? P1A F6A 1.588(3) . ? P1B F1B 1.6031(14) . ? P1B F2B 1.5872(13) . ? P1B F3B 1.6003(13) . ? P1B F4B 1.6171(15) . ? P1B F5B 1.6019(16) . ? P1B F6B 1.5876(18) . ? 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 F7A P2A F12A 88.69(9) . . ? F8A P2A F7A 177.88(12) . . ? F8A P2A F12A 89.32(11) . . ? F9A P2A F7A 90.37(10) . . ? F9A P2A F8A 91.65(11) . . ? F9A P2A F12A 177.83(12) . . ? F10A P2A F7A 90.76(10) . . ? F10A P2A F8A 89.91(13) . . ? F10A P2A F9A 89.56(9) . . ? F10A P2A F11A 179.15(12) . . ? F10A P2A F12A 88.49(9) . . ? F11A P2A F7A 89.92(11) . . ? F11A P2A F8A 89.39(14) . . ? F11A P2A F9A 90.94(12) . . ? F11A P2A F12A 91.02(11) . . ? F7B P2B F12B 85.8(5) . . ? F8B P2B F7B 173.9(7) . . ? F8B P2B F12B 98.5(6) . . ? F9B P2B F7B 88.5(5) . . ? F9B P2B F8B 87.1(6) . . ? F9B P2B F12B 174.1(6) . . ? F10B P2B F7B 87.2(5) . . ? F10B P2B F8B 88.6(6) . . ? F10B P2B F9B 90.2(4) . . ? F10B P2B F11B 174.3(6) . . ? F10B P2B F12B 88.0(4) . . ? F11B P2B F7B 87.0(5) . . ? F11B P2B F8B 97.1(7) . . ? F11B P2B F9B 89.8(5) . . ? F11B P2B F12B 91.5(5) . . ? H17A C17 H17B 106.8 . . ? C18 C17 H17A 107.1 . . ? C18 C17 H17B 107.1 . . ? C18 C17 S5 120.87(6) . . ? S5 C17 H17A 107.1 . . ? S5 C17 H17B 107.1 . . ? C17 C18 C19 112.73(7) . . ? C17 C18 C32 106.32(7) . . ? C19 C18 C32 103.48(7) . . ? C31 C18 C17 111.71(7) . . ? C31 C18 C19 112.49(7) . . ? C31 C18 C32 109.56(7) . . ? C18 C19 H19A 108.3 . . ? C18 C19 H19B 108.3 . . ? C18 C19 S6 115.74(6) . . ? H19A C19 H19B 107.4 . . ? S6 C19 H19A 108.3 . . ? S6 C19 H19B 108.3 . . ? H23A C23 H23B 107.7 . . ? C24 C23 H23A 108.8 . . ? C24 C23 H23B 108.8 . . ? C24 C23 S7 113.68(6) . . ? S7 C23 H23A 108.8 . . ? S7 C23 H23B 108.8 . . ? C23 C24 C25 114.19(7) . . ? C23 C24 C29 110.89(7) . . ? C29 C24 C25 104.38(7) . . ? C30 C24 C23 105.52(7) . . ? C30 C24 C25 111.09(7) . . ? C30 C24 C29 110.90(7) . . ? C24 C25 H25A 109.0 . . ? C24 C25 H25B 109.0 . . ? C24 C25 S8 113.11(6) . . ? H25A C25 H25B 107.8 . . ? S8 C25 H25A 109.0 . . ? S8 C25 H25B 109.0 . . ? H26A C26 H26B 107.2 . . ? C27 C26 H26A 107.9 . . ? C27 C26 H26B 107.9 . . ? C27 C26 S8 117.77(7) . . ? S8 C26 H26A 107.9 . . ? S8 C26 H26B 107.9 . . ? C26 C27 H27A 108.4 . . ? C26 C27 H27B 108.4 . . ? C26 C27 C28 115.40(9) . . ? H27A C27 H27B 107.5 . . ? C28 C27 H27A 108.4 . . ? C28 C27 H27B 108.4 . . ? C27 C28 H28A 109.3 . . ? C27 C28 H28B 109.3 . . ? C27 C28 S5 111.65(6) . . ? H28A C28 H28B 108.0 . . ? S5 C28 H28A 109.3 . . ? S5 C28 H28B 109.3 . . ? C24 C29 H29A 109.2 . . ? C24 C29 H29B 109.2 . . ? H29A C29 H29B 107.9 . . ? O5 C29 C24 112.21(7) . . ? O5 C29 H29A 109.2 . . ? O5 C29 H29B 109.2 . . ? C24 C30 H30A 110.0 . . ? C24 C30 H30B 110.0 . . ? H30A C30 H30B 108.3 . . ? O6 C30 C24 108.68(8) . . ? O6 C30 H30A 110.0 . . ? O6 C30 H30B 110.0 . . ? C18 C31 H31A 110.0 . . ? C18 C31 H31B 110.0 . . ? H31A C31 H31B 108.4 . . ? O7 C31 C18 108.54(7) . . ? O7 C31 H31A 110.0 . . ? O7 C31 H31B 110.0 . . ? C18 C32 H32A 108.9 . . ? C18 C32 H32B 108.9 . . ? H32A C32 H32B 107.8 . . ? O8 C32 C18 113.16(7) . . ? O8 C32 H32A 108.9 . . ? O8 C32 H32B 108.9 . . ? C29 O5 H5 109.5 . . ? C30 O6 H6 109.5 . . ? C31 O7 H7 109.5 . . ? C32 O8 H8 109.5 . . ? C17 S5 C28 101.82(4) . . ? C17 S5 Cu2 111.15(3) . . ? C28 S5 Cu2 107.13(4) . . ? C19 S6 Cu2 105.19(3) . . ? C19 S6 C20 95.41(6) . . ? C20 S6 Cu2 105.15(5) . . ? C20' S6 C19 103.93(10) . . ? C20' S6 Cu2 109.11(8) . . ? C23 S7 Cu2 101.20(3) . . ? C23 S7 C22 96.26(6) . . ? C22 S7 Cu2 105.50(6) . . ? C22' S7 C23 103.73(10) . . ? C22' S7 Cu2 107.36(10) . . ? C25 S8 C26 99.92(4) . . ? C25 S8 Cu2 99.15(3) . . ? C26 S8 Cu2 108.82(3) . . ? S5 Cu2 S7 116.703(10) . . ? S5 Cu2 S8 104.482(9) . . ? S6 Cu2 S5 106.517(9) . . ? S6 Cu2 S7 109.358(9) . . ? S6 Cu2 S8 123.669(10) . . ? S8 Cu2 S7 96.580(9) . . ? H4A C4 H4B 108.0 . . ? S2 C4 H4A 109.5 . . ? S2 C4 H4B 109.5 . . ? C5 C4 H4A 109.5 . . ? C5 C4 H4B 109.5 . . ? C5 C4 S2 110.94(6) . . ? C14 O2 H2 109.5 . . ? C16 O4 H4 109.5 . . ? C13 O1 H1 109.5 . . ? O2 C14 H14A 109.8 . . ? O2 C14 H14B 109.8 . . ? O2 C14 C8 109.46(7) . . ? H14A C14 H14B 108.2 . . ? C8 C14 H14A 109.8 . . ? C8 C14 H14B 109.8 . . ? H10A C10 H10B 107.2 . . ? C11 C10 H10A 107.9 . . ? C11 C10 H10B 107.9 . . ? C11 C10 S4 117.71(6) . . ? S4 C10 H10A 107.9 . . ? S4 C10 H10B 107.9 . . ? C10 C11 H11A 108.5 . . ? C10 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? C12 C11 C10 115.22(8) . . ? C12 C11 H11A 108.5 . . ? C12 C11 H11B 108.5 . . ? C6 S3 Cu1 108.64(3) . . ? C7 S3 Cu1 100.79(3) . . ? C7 S3 C6 100.15(4) . . ? C10 S4 C9 98.71(4) . . ? C10 S4 Cu1 103.88(3) . . ? C9 S4 Cu1 100.48(3) . . ? O1 C13 H13A 108.9 . . ? O1 C13 H13B 108.9 . . ? O1 C13 C8 113.25(7) . . ? H13A C13 H13B 107.7 . . ? C8 C13 H13A 108.9 . . ? C8 C13 H13B 108.9 . . ? C14 C8 C13 110.81(6) . . ? C14 C8 C9 104.94(6) . . ? C14 C8 C7 111.02(7) . . ? C9 C8 C13 110.92(7) . . ? C9 C8 C7 114.19(6) . . ? C7 C8 C13 105.08(6) . . ? C4 S2 Cu1 107.30(3) . . ? C3 S2 C4 102.73(4) . . ? C3 S2 Cu1 112.02(3) . . ? C15 O3 H3 109.5 . . ? S4 C9 H9A 108.6 . . ? S4 C9 H9B 108.6 . . ? C8 C9 S4 114.81(6) . . ? C8 C9 H9A 108.6 . . ? C8 C9 H9B 108.6 . . ? H9A C9 H9B 107.5 . . ? S3 Cu1 S4 97.026(8) . . ? S2 Cu1 S3 106.772(9) . . ? S2 Cu1 S4 117.871(9) . . ? S1 Cu1 S3 118.896(9) . . ? S1 Cu1 S4 110.019(9) . . ? S1 Cu1 S2 106.648(9) . . ? C1 S1 Cu1 105.67(3) . . ? C1 S1 C12 97.79(4) . . ? C12 S1 Cu1 108.10(3) . . ? S2 C3 H3A 107.3 . . ? S2 C3 H3B 107.3 . . ? H3A C3 H3B 106.9 . . ? C2 C3 S2 120.11(6) . . ? C2 C3 H3A 107.3 . . ? C2 C3 H3B 107.3 . . ? C15 C2 C3 112.20(7) . . ? C15 C2 C1 111.97(7) . . ? C15 C2 C16 109.14(7) . . ? C1 C2 C3 113.28(7) . . ? C1 C2 C16 105.23(7) . . ? C16 C2 C3 104.41(7) . . ? S3 C6 H6A 107.9 . . ? S3 C6 H6B 107.9 . . ? H6A C6 H6B 107.2 . . ? C5 C6 S3 117.50(6) . . ? C5 C6 H6A 107.9 . . ? C5 C6 H6B 107.9 . . ? O3 C15 C2 108.14(7) . . ? O3 C15 H15A 110.1 . . ? O3 C15 H15B 110.1 . . ? C2 C15 H15A 110.1 . . ? C2 C15 H15B 110.1 . . ? H15A C15 H15B 108.4 . . ? S3 C7 H7A 109.1 . . ? S3 C7 H7B 109.1 . . ? C8 C7 S3 112.41(6) . . ? C8 C7 H7A 109.1 . . ? C8 C7 H7B 109.1 . . ? H7A C7 H7B 107.9 . . ? C4 C5 H5A 108.4 . . ? C4 C5 H5B 108.4 . . ? C6 C5 C4 115.32(8) . . ? C6 C5 H5A 108.4 . . ? C6 C5 H5B 108.4 . . ? H5A C5 H5B 107.5 . . ? S1 C1 H1A 108.1 . . ? S1 C1 H1B 108.1 . . ? C2 C1 S1 116.78(6) . . ? C2 C1 H1A 108.1 . . ? C2 C1 H1B 108.1 . . ? H1A C1 H1B 107.3 . . ? C11 C12 S1 113.59(7) . . ? C11 C12 H12A 108.8 . . ? C11 C12 H12B 108.8 . . ? S1 C12 H12A 108.8 . . ? S1 C12 H12B 108.8 . . ? H12A C12 H12B 107.7 . . ? O4 C16 C2 109.51(7) . . ? O4 C16 H16A 109.8 . . ? O4 C16 H16B 109.8 . . ? C2 C16 H16A 109.8 . . ? C2 C16 H16B 109.8 . . ? H16A C16 H16B 108.2 . . ? H33A C33 H33B 108.3 . . ? C34 C33 H33A 109.9 . . ? C34 C33 H33B 109.9 . . ? O9 C33 H33A 109.9 . . ? O9 C33 H33B 109.9 . . ? O9 C33 C34 108.93(9) . . ? C33 C34 H34A 109.5 . . ? C33 C34 H34B 109.5 . . ? C33 C34 H34C 109.5 . . ? H34A C34 H34B 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C35 O10 H10 109.5 . . ? O10 C35 H35A 109.1 . . ? O10 C35 H35B 109.1 . . ? O10 C35 C36 112.60(9) . . ? H35A C35 H35B 107.8 . . ? C36 C35 H35A 109.1 . . ? C36 C35 H35B 109.1 . . ? C33 O9 H9 109.5 . . ? C35 C36 H36A 109.5 . . ? C35 C36 H36B 109.5 . . ? C35 C36 H36C 109.5 . . ? H36A C36 H36B 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? S6 C20 H20A 109.3 . . ? S6 C20 H20B 109.3 . . ? H20A C20 H20B 108.0 . . ? C21 C20 S6 111.40(10) . . ? C21 C20 H20A 109.3 . . ? C21 C20 H20B 109.3 . . ? C20 C21 H21A 107.8 . . ? C20 C21 H21B 107.8 . . ? H21A C21 H21B 107.1 . . ? C22 C21 C20 118.03(13) . . ? C22 C21 H21A 107.8 . . ? C22 C21 H21B 107.8 . . ? S7 C22 H22A 107.2 . . ? S7 C22 H22B 107.2 . . ? C21 C22 S7 120.44(12) . . ? C21 C22 H22A 107.2 . . ? C21 C22 H22B 107.2 . . ? H22A C22 H22B 106.8 . . ? S6 C20' H20C 108.4 . . ? S6 C20' H20D 108.4 . . ? H20C C20' H20D 107.5 . . ? C21' C20' S6 115.4(2) . . ? C21' C20' H20C 108.4 . . ? C21' C20' H20D 108.4 . . ? C20' C21' H21C 105.7 . . ? C20' C21' H21D 105.7 . . ? C20' C21' C22' 126.5(2) . . ? H21C C21' H21D 106.1 . . ? C22' C21' H21C 105.7 . . ? C22' C21' H21D 105.7 . . ? S7 C22' H22C 107.4 . . ? S7 C22' H22D 107.4 . . ? C21' C22' S7 119.8(2) . . ? C21' C22' H22C 107.4 . . ? C21' C22' H22D 107.4 . . ? H22C C22' H22D 106.9 . . ? F1A P1A F4A 88.4(2) . . ? F1A P1A F5A 89.4(3) . . ? F2A P1A F1A 177.2(3) . . ? F2A P1A F4A 88.8(2) . . ? F2A P1A F5A 90.2(3) . . ? F3A P1A F1A 91.2(3) . . ? F3A P1A F2A 91.7(3) . . ? F3A P1A F4A 179.0(3) . . ? F3A P1A F5A 90.8(3) . . ? F5A P1A F4A 90.2(3) . . ? F6A P1A F1A 90.3(3) . . ? F6A P1A F2A 90.0(3) . . ? F6A P1A F3A 90.8(3) . . ? F6A P1A F4A 88.2(2) . . ? F6A P1A F5A 178.4(3) . . ? F1B P1B F4B 89.13(9) . . ? F2B P1B F1B 179.04(13) . . ? F2B P1B F3B 91.19(11) . . ? F2B P1B F4B 90.56(9) . . ? F2B P1B F5B 90.27(12) . . ? F2B P1B F6B 90.73(11) . . ? F3B P1B F1B 89.13(11) . . ? F3B P1B F4B 178.10(11) . . ? F3B P1B F5B 89.28(12) . . ? F5B P1B F1B 88.83(12) . . ? F5B P1B F4B 91.45(13) . . ? F6B P1B F1B 90.17(13) . . ? F6B P1B F3B 90.95(13) . . ? F6B P1B F4B 88.30(12) . . ? F6B P1B F5B 178.97(13) . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A O2 H2 F12A 0.84 2.04 2.8693(16) 169.5 2_657 O2 H2 F12B 0.84 1.93 2.766(6) 174.4 2_657 O1 H1 O10 0.84 1.89 2.7260(11) 171.3 1_556 O3 H3 O4 0.84 1.95 2.7823(11) 171.4 2_566 loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C17 C18 C19 S6 86.49(8) . . . . ? C17 C18 C31 O7 176.56(7) . . . . ? C17 C18 C32 O8 -58.95(9) . . . . ? C18 C17 S5 C28 -88.61(8) . . . . ? C18 C17 S5 Cu2 25.19(8) . . . . ? C18 C19 S6 Cu2 -57.75(6) . . . . ? C18 C19 S6 C20 -165.08(8) . . . . ? C18 C19 S6 C20' -172.39(11) . . . . ? C19 C18 C31 O7 -55.49(9) . . . . ? C19 C18 C32 O8 -177.90(7) . . . . ? C19 S6 C20 C21 153.60(11) . . . . ? C19 S6 C20' C21' 78.7(2) . . . . ? C23 C24 C25 S8 43.15(9) . . . . ? C23 C24 C29 O5 -64.66(9) . . . . ? C23 C24 C30 O6 179.67(7) . . . . ? C23 S7 C22 C21 83.71(14) . . . . ? C23 S7 C22' C21' 126.3(2) . . . . ? C24 C23 S7 Cu2 -76.56(6) . . . . ? C24 C23 S7 C22 176.24(8) . . . . ? C24 C23 S7 C22' 172.25(12) . . . . ? C24 C25 S8 C26 166.88(6) . . . . ? C24 C25 S8 Cu2 -82.03(6) . . . . ? C25 C24 C29 O5 171.93(7) . . . . ? C25 C24 C30 O6 -56.08(10) . . . . ? C26 C27 C28 S5 -86.56(9) . . . . ? C27 C26 S8 C25 64.67(8) . . . . ? C27 C26 S8 Cu2 -38.63(8) . . . . ? C27 C28 S5 C17 174.10(7) . . . . ? C27 C28 S5 Cu2 57.34(8) . . . . ? C29 C24 C25 S8 164.39(6) . . . . ? C29 C24 C30 O6 59.52(9) . . . . ? C30 C24 C25 S8 -76.03(8) . . . . ? C30 C24 C29 O5 52.23(9) . . . . ? C31 C18 C19 S6 -40.93(9) . . . . ? C31 C18 C32 O8 61.92(9) . . . . ? C32 C18 C19 S6 -159.08(6) . . . . ? C32 C18 C31 O7 59.02(9) . . . . ? S5 C17 C18 C19 -64.86(9) . . . . ? S5 C17 C18 C31 62.97(9) . . . . ? S5 C17 C18 C32 -177.56(6) . . . . ? S6 C20 C21 C22 -91.64(15) . . . . ? S6 C20' C21' C22' 75.6(3) . . . . ? S7 C23 C24 C25 47.39(9) . . . . ? S7 C23 C24 C29 -70.17(8) . . . . ? S7 C23 C24 C30 169.67(6) . . . . ? S8 C26 C27 C28 75.66(10) . . . . ? Cu2 S6 C20 C21 46.24(12) . . . . ? Cu2 S6 C20' C21' -33.1(2) . . . . ? Cu2 S7 C22 C21 -19.77(15) . . . . ? Cu2 S7 C22' C21' 19.7(3) . . . . ? C4 S2 C3 C2 90.93(7) . . . . ? O2 C14 C8 C13 -56.95(9) . . . . ? O2 C14 C8 C9 -176.74(7) . . . . ? O2 C14 C8 C7 59.42(9) . . . . ? O1 C13 C8 C14 -48.44(9) . . . . ? O1 C13 C8 C9 67.70(9) . . . . ? O1 C13 C8 C7 -168.42(7) . . . . ? C14 C8 C9 S4 -160.78(6) . . . . ? C14 C8 C7 S3 67.83(8) . . . . ? C10 C11 C12 S1 82.85(9) . . . . ? C10 S4 C9 C8 -176.76(6) . . . . ? C11 C10 S4 C9 -62.74(7) . . . . ? C11 C10 S4 Cu1 40.40(7) . . . . ? S3 C6 C5 C4 -76.84(10) . . . . ? S4 C10 C11 C12 -85.96(9) . . . . ? C13 C8 C9 S4 79.50(8) . . . . ? C13 C8 C7 S3 -172.32(5) . . . . ? S2 C4 C5 C6 89.12(9) . . . . ? S2 C3 C2 C15 -63.54(9) . . . . ? S2 C3 C2 C1 64.45(9) . . . . ? S2 C3 C2 C16 178.39(6) . . . . ? C9 C8 C7 S3 -50.55(8) . . . . ? Cu1 S3 C6 C5 32.36(8) . . . . ? Cu1 S3 C7 C8 80.00(6) . . . . ? Cu1 S4 C9 C8 77.28(6) . . . . ? Cu1 S2 C3 C2 -23.92(7) . . . . ? Cu1 S1 C1 C2 54.67(7) . . . . ? Cu1 S1 C12 C11 -39.34(8) . . . . ? C3 C2 C15 O3 -58.10(9) . . . . ? C3 C2 C1 S1 -85.33(8) . . . . ? C3 C2 C16 O4 174.80(7) . . . . ? C6 S3 C7 C8 -168.61(6) . . . . ? C15 C2 C1 S1 42.77(9) . . . . ? C15 C2 C16 O4 54.66(10) . . . . ? C7 S3 C6 C5 -72.77(8) . . . . ? C7 C8 C9 S4 -39.00(9) . . . . ? C5 C4 S2 Cu1 -52.89(7) . . . . ? C5 C4 S2 C3 -171.12(7) . . . . ? C1 S1 C12 C11 -148.70(8) . . . . ? C1 C2 C15 O3 173.22(7) . . . . ? C1 C2 C16 O4 -65.67(9) . . . . ? C12 S1 C1 C2 166.02(7) . . . . ? C16 C2 C15 O3 57.12(9) . . . . ? C16 C2 C1 S1 161.22(6) . . . . ? C20 S6 C20' C21' 37.8(5) . . . . ? C20 C21 C22 S7 73.98(17) . . . . ? C22 S7 C22' C21' 98.2(10) . . . . ? C20' S6 C20 C21 -66.1(5) . . . . ? C20' C21' C22' S7 -67.7(4) . . . . ? C22' S7 C22 C21 -123.7(10) . . . . ? _shelx_estimated_absorpt_T_max 0.802 _shelx_estimated_absorpt_T_min 0.468 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelxl_version_number 2012-9 data_16 _audit_creation_date 2013-07-07 _audit_creation_method ; Olex2 1.2-beta (compiled Apr 23 2013 17:59:47, GUI svn.r4466) ; _publ_section_references ; Sheldrick, G.M. (2008). Acta Cryst. A64, 112-122 Petricek,V., Dusek,M. & Palatinus,L.(2006). Jana2006. The crystallographic computing system. Institute of Physics, Praha, Czech Republic. Spek, A. L. (2003). J. Appl. Cryst. 36, 7-13. Bruker (2011). APEX2 Version 2011.2-4. Bruker AXS Inc., Madison, Wisconsin, USA. Bruker (2009). SAINT-Plus Version 7.68a. Bruker AXS Inc., Madison, Wisconsin, USA. Sheldrick, G. M. (2008). SADABS Version 2008-1. Bruker AXS Inc., Madison, Wisconsin, USA. ; _chemical_name_common ? _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C16 H32 O4 S4' _chemical_formula_sum 'C16 H32 O4 S4' _chemical_formula_weight 416.65 _chemical_melting_point ? 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' 'S' 'S' 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system 'triclinic' _space_group_IT_number 2 _space_group_name_H-M_alt 'P -1' _space_group_name_Hall '-P 1' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5948(9) _cell_length_b 9.6412(9) _cell_length_c 12.1268(12) _cell_angle_alpha 100.741(2) _cell_angle_beta 107.2010(10) _cell_angle_gamma 97.413(2) _cell_volume 1032.38(17) _cell_formula_units_Z 2 _cell_measurement_reflns_used 4864 _cell_measurement_temperature 110(2) _cell_measurement_theta_max 31.051 _cell_measurement_theta_min 2.266 _exptl_absorpt_coefficient_mu 0.477 _exptl_absorpt_correction_T_max 0.7462 _exptl_absorpt_correction_T_min 0.559773 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; TWINABS-2012/1 (Bruker,2012) was used for absorption correction. For component 1: wR2(int) was 0.0922 before and 0.0496 after correction. The Ratio of minimum to maximum transmission is 0.75. The \l/2 correction factor is Not present For component 2: wR2(int) was 0.0925 before and 0.0476 after correction. The Ratio of minimum to maximum transmission not present. The \l/2 correction factor is Not present Final HKLF 4 output contains 17303 reflections, Rint = 0.1021 (11141 with I > 3sig(I), Rint = 0.0976) ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.340 _exptl_crystal_density_meas . _exptl_crystal_density_method ? _exptl_crystal_description prism _exptl_crystal_F_000 448 _exptl_crystal_size_max 0.774 _exptl_crystal_size_mid 0.212 _exptl_crystal_size_min 0.196 _exptl_special_details ; ? ; _exptl_transmission_factor_max ? _exptl_transmission_factor_min ? _diffrn_reflns_av_R_equivalents ? _diffrn_reflns_av_unetI/netI 0.0470 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_number 7622 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.997 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.216 _diffrn_reflns_theta_min 1.809 _diffrn_ambient_temperature 110(2) _diffrn_detector_area_resol_mean 512 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device_type 'Bruker D8 diffractometer with APEX2 detector' _diffrn_measurement_method '\f and \w scans with a narrow frame width' _diffrn_radiation_monochromator graphite _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_source 'fine-focus sealed tube' _diffrn_standards_number 0 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 6791 _reflns_number_total 7622 _reflns_special_details ; _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. ; _reflns_threshold_expression 'I > 2\s(I)' _computing_cell_refinement 'SAINT v7.68A (Bruker, 2009)' _computing_data_collection 'APEX2 v2011.2-4 (Bruker, 2011)' _computing_data_reduction 'SAINT v7.68A (Bruker, 2009)' _computing_molecular_graphics ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_publication_material ; O. V. Dolomanov, L. J. Bourhis, R. J. Gildea, J. A. K. Howard and H. Puschmann, OLEX2: a complete structure solution, refinement and analysis program. J. Appl. Cryst. (2009). 42, 339-341. ; _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _refine_diff_density_max 1.736 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.125 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 245 _refine_ls_number_reflns 7622 _refine_ls_number_restraints 72 _refine_ls_R_factor_all 0.1020 _refine_ls_R_factor_gt 0.0944 _refine_ls_restrained_S_all 1.087 _refine_ls_shift/su_max 0.006 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0870P)^2^+3.5031P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2297 _refine_ls_wR_factor_ref 0.2354 _refine_special_details ; Refined as a 2-component twin. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups, All O(H) groups 2. Restrained distances C5A-C4A = C5B-C4B 1.52 with sigma of 0.01 H4-H1_$1 -2.045 with sigma of 0.02 S2B-C3 \\sim S2A-C3 with sigma of 0.005 S3B-C7 \\sim S3A-C7 with sigma of 0.005 S3A-C7 \\sim S3B-C7 with sigma of 0.004 S2A-C4A \\sim S2B-C4B with sigma of 0.004 3. Uiso/Uaniso restraints and constraints Uanis(C7) \\sim Ueq, Uanis(S3B) \\sim Ueq, Uanis(S3A) \\sim Ueq, Uanis(C6B) \\sim Ueq, Uanis(C6A) \\sim Ueq, Uanis(C5B) \\sim Ueq, Uanis(C5A) \\sim Ueq, Uanis(C4B) \\sim Ueq, Uanis(C4A) \\sim Ueq, Uanis(S2B) \\sim Ueq, Uanis(S2A) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004 Uanis(S2A) = Uanis(S2B) Uanis(C4A) = Uanis(C4B) Uanis(C5A) = Uanis(C5B) Uanis(C6A) = Uanis(C6B) Uanis(S3A) = Uanis(S3B) 4. Others Fixed Sof: S2A(0.5) C4A(0.5) H4AA(0.5) H4AB(0.5) C5A(0.5) H5AA(0.5) H5AB(0.5) C6A(0.5) H6AA(0.5) H6AB(0.5) S3A(0.5) S2B(0.5) C4B(0.5) H4BA(0.5) H4BB(0.5) C5B(0.5) H5BA(0.5) H5BB(0.5) C6B(0.5) H6BA(0.5) H6BB(0.5) S3B(0.5) 5.a Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C3(H3A,H3B), C4A(H4AA,H4AB), C5A(H5AA,H5AB), C6A(H6AA,H6AB), C4B(H4BA,H4BB), C5B(H5BA,H5BB), C6B(H6BA,H6BB), C7(H7A,H7B), C9(H9A,H9B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B), C14(H14A,H14B), C15(H15A,H15B), C16(H16A,H16B) 5.b Idealised tetrahedral OH refined as rotating group: O1(H1), O2(H2), O3(H3), O4(H4) ; _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary iterative _atom_sites_solution_secondary ? 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group H13A H 1.478(6) -0.299(5) 0.224(5) 0.021(13) Uiso 1 1 d . . . . . H13B H 1.381(5) -0.243(5) 0.115(4) 0.012(11) Uiso 1 1 d . . . . . C1 C 0.6907(5) 0.1686(5) 0.1562(4) 0.0246(10) Uani 1 1 d . . . . . H1A H 0.7851 0.1766 0.1415 0.029 Uiso 1 1 calc R U . . . H1B H 0.6153 0.1749 0.0846 0.029 Uiso 1 1 calc R U . . . C2 C 0.7010(6) 0.2953(5) 0.2576(4) 0.0264(10) Uani 1 1 d . . . . . C3 C 0.8298(6) 0.3014(6) 0.3706(4) 0.0315(11) Uani 1 1 d D . . . . H3A H 0.8200 0.2094 0.3920 0.038 Uiso 1 1 calc R U . A 1 H3B H 0.8250 0.3744 0.4356 0.038 Uiso 1 1 calc R U . A 1 S2A S 1.0103(7) 0.3434(12) 0.3484(10) 0.0359(9) Uani 0.5 1 d D U P B 1 C4A C 1.1387(18) 0.3176(16) 0.4803(13) 0.050(3) Uani 0.5 1 d D U P B 1 H4AA H 1.2368 0.3700 0.4908 0.060 Uiso 0.5 1 calc R U P B 1 H4AB H 1.1105 0.3594 0.5478 0.060 Uiso 0.5 1 calc R U P B 1 C5A C 1.148(2) 0.1630(15) 0.4817(17) 0.051(3) Uani 0.5 1 d D U P B 1 H5AA H 1.0495 0.1035 0.4447 0.061 Uiso 0.5 1 calc R U P B 1 H5AB H 1.1843 0.1549 0.5634 0.061 Uiso 0.5 1 calc R U P B 1 C6A C 1.2528(16) 0.1061(16) 0.4155(14) 0.043(2) Uani 0.5 1 d . U P B 1 H6AA H 1.3539 0.1599 0.4546 0.052 Uiso 0.5 1 calc R U P B 1 H6AB H 1.2202 0.1158 0.3341 0.052 Uiso 0.5 1 calc R U P B 1 S3A S 1.2440(4) -0.0809(5) 0.4192(3) 0.0328(7) Uani 0.5 1 d D U P B 1 S2B S 1.0130(7) 0.3232(12) 0.3512(10) 0.0359(9) Uani 0.5 1 d D U P B 2 C4B C 1.1123(18) 0.2910(15) 0.4912(13) 0.050(3) Uani 0.5 1 d D U P B 2 H4BA H 1.2137 0.3448 0.5181 0.060 Uiso 0.5 1 calc R U P B 2 H4BB H 1.0660 0.3258 0.5493 0.060 Uiso 0.5 1 calc R U P B 2 C5B C 1.115(2) 0.1348(15) 0.4844(17) 0.051(3) Uani 0.5 1 d D U P B 2 H5BA H 1.0140 0.0796 0.4520 0.061 Uiso 0.5 1 calc R U P B 2 H5BB H 1.1587 0.1211 0.5636 0.061 Uiso 0.5 1 calc R U P B 2 C6B C 1.2057(16) 0.0797(16) 0.4054(14) 0.043(2) Uani 0.5 1 d . U P B 2 H6BA H 1.3075 0.1330 0.4389 0.052 Uiso 0.5 1 calc R U P B 2 H6BB H 1.1636 0.0956 0.3266 0.052 Uiso 0.5 1 calc R U P B 2 S3B S 1.2040(4) -0.1068(5) 0.3948(3) 0.0328(7) Uani 0.5 1 d D U P B 2 C7 C 1.3285(7) -0.1367(6) 0.3061(5) 0.0358(12) Uani 1 1 d D U . . . H7A H 1.3089 -0.0751 0.2508 0.043 Uiso 1 1 calc R U . B 1 H7B H 1.4354 -0.1184 0.3448 0.043 Uiso 1 1 calc R U . B 1 C8 C 1.2804(6) -0.2918(6) 0.2344(4) 0.0310(11) Uani 1 1 d . . . . . C9 C 1.1200(6) -0.3247(7) 0.1489(5) 0.0360(13) Uani 1 1 d . . . . . H9A H 1.0535 -0.3067 0.1943 0.043 Uiso 1 1 calc R U . . . H9B H 1.0936 -0.4258 0.1084 0.043 Uiso 1 1 calc R U . . . C10 C 0.8989(6) -0.2104(6) 0.0060(5) 0.0309(11) Uani 1 1 d . . . . . H10A H 0.8653 -0.1772 -0.0664 0.037 Uiso 1 1 calc R U . . . H10B H 0.8431 -0.3071 -0.0085 0.037 Uiso 1 1 calc R U . . . C11 C 0.8641(5) -0.1126(6) 0.1044(4) 0.0276(10) Uani 1 1 d . . . . . H11A H 0.8986 -0.1441 0.1776 0.033 Uiso 1 1 calc R U . . . H11B H 0.9168 -0.0149 0.1177 0.033 Uiso 1 1 calc R U . . . C12 C 0.6985(5) -0.1149(6) 0.0723(4) 0.0276(10) Uani 1 1 d . . . . . H12A H 0.6468 -0.2136 0.0559 0.033 Uiso 1 1 calc R U . . . H12B H 0.6657 -0.0816 -0.0001 0.033 Uiso 1 1 calc R U . . . C13 C 1.3893(6) -0.3158(6) 0.1657(4) 0.0283(11) Uani 1 1 d . . . . . C14 C 1.2858(7) -0.3974(6) 0.3151(4) 0.0355(12) Uani 1 1 d . . . . . H14A H 1.2116 -0.3862 0.3540 0.043 Uiso 1 1 calc R U . . . H14B H 1.2613 -0.4951 0.2670 0.043 Uiso 1 1 calc R U . . . C15 C 0.5558(6) 0.2780(6) 0.2876(4) 0.0314(11) Uani 1 1 d . . . . . H15A H 0.4722 0.2674 0.2160 0.038 Uiso 1 1 calc R U . . . H15B H 0.5441 0.1912 0.3163 0.038 Uiso 1 1 calc R U . . . C16 C 0.7259(6) 0.4356(6) 0.2175(4) 0.0328(12) Uani 1 1 d . . . . . H16A H 0.7334 0.5165 0.2813 0.039 Uiso 1 1 calc R U . . . H16B H 0.8191 0.4460 0.2010 0.039 Uiso 1 1 calc R U . . . O1 O 1.3567(4) -0.4589(4) 0.0947(3) 0.0329(8) Uani 1 1 d . . . . . H1 H 1.3486 -0.4565 0.0259 0.039 Uiso 1 1 calc R U . . . O2 O 1.4286(6) -0.3748(5) 0.4031(3) 0.0490(12) Uani 1 1 d . . . . . H2 H 1.4715 -0.4397 0.3858 0.059 Uiso 1 1 calc R U . . . O3 O 0.5545(5) 0.3991(5) 0.3759(3) 0.0432(11) Uani 1 1 d . . . . . H3 H 0.5615 0.3750 0.4384 0.052 Uiso 1 1 calc R U . . . O4 O 0.6080(5) 0.4385(5) 0.1138(3) 0.0443(11) Uani 1 1 d . . . . . H4 H 0.5539 0.4909 0.1326 0.053 Uiso 1 1 calc DR U . . . S1 S 0.64556(16) -0.00551(15) 0.18617(12) 0.0332(3) Uani 1 1 d . . . . . S4 S 1.09397(17) -0.2169(2) 0.03913(14) 0.0477(5) 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 0.026(2) 0.030(2) 0.018(2) 0.0026(18) 0.0090(18) 0.0089(19) C2 0.030(2) 0.035(3) 0.0119(19) 0.0012(18) 0.0020(18) 0.015(2) C3 0.034(3) 0.040(3) 0.016(2) 0.001(2) 0.001(2) 0.016(2) S2A 0.0301(7) 0.035(2) 0.0369(8) 0.0047(12) 0.0021(6) 0.0137(7) C4A 0.050(3) 0.051(3) 0.050(3) 0.0106(16) 0.0157(17) 0.0112(19) C5A 0.052(3) 0.051(3) 0.048(3) 0.0108(17) 0.0177(17) 0.0081(19) C6A 0.044(3) 0.042(3) 0.043(2) 0.0087(16) 0.0150(18) 0.0109(19) S3A 0.0474(16) 0.0308(14) 0.0199(12) -0.0029(10) 0.0140(12) 0.0128(13) S2B 0.0301(7) 0.035(2) 0.0369(8) 0.0047(12) 0.0021(6) 0.0137(7) C4B 0.050(3) 0.051(3) 0.050(3) 0.0106(16) 0.0157(17) 0.0112(19) C5B 0.052(3) 0.051(3) 0.048(3) 0.0108(17) 0.0177(17) 0.0081(19) C6B 0.044(3) 0.042(3) 0.043(2) 0.0087(16) 0.0150(18) 0.0109(19) S3B 0.0474(16) 0.0308(14) 0.0199(12) -0.0029(10) 0.0140(12) 0.0128(13) C7 0.046(2) 0.035(2) 0.033(2) 0.0084(16) 0.0182(17) 0.0170(17) C8 0.045(3) 0.039(3) 0.021(2) 0.014(2) 0.018(2) 0.026(2) C9 0.039(3) 0.057(4) 0.030(3) 0.024(2) 0.022(2) 0.027(3) C10 0.025(2) 0.048(3) 0.029(3) 0.014(2) 0.014(2) 0.020(2) C11 0.025(2) 0.034(3) 0.024(2) 0.006(2) 0.0067(19) 0.011(2) C12 0.022(2) 0.034(3) 0.025(2) -0.0039(19) 0.0108(19) 0.0069(19) C13 0.031(3) 0.036(3) 0.019(2) 0.002(2) 0.009(2) 0.016(2) C14 0.056(4) 0.038(3) 0.025(2) 0.014(2) 0.020(2) 0.027(3) C15 0.030(3) 0.046(3) 0.018(2) 0.002(2) 0.0076(19) 0.016(2) C16 0.039(3) 0.039(3) 0.021(2) 0.004(2) 0.007(2) 0.018(2) O1 0.033(2) 0.039(2) 0.0269(18) -0.0027(15) 0.0162(16) 0.0098(16) O2 0.079(3) 0.041(2) 0.0240(19) 0.0087(17) 0.002(2) 0.034(2) O3 0.053(3) 0.065(3) 0.0192(18) 0.0046(17) 0.0156(17) 0.036(2) O4 0.055(3) 0.059(3) 0.0243(19) 0.0124(17) 0.0084(18) 0.037(2) S1 0.0385(7) 0.0343(7) 0.0336(7) 0.0047(5) 0.0227(6) 0.0108(5) S4 0.0377(8) 0.0930(13) 0.0453(9) 0.0479(9) 0.0308(7) 0.0411(8) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 C2 1.533(6) . ? C1 S1 1.808(5) . ? C2 C3 1.536(6) . ? C2 C15 1.537(7) . ? C2 C16 1.535(8) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 S2A 1.837(7) . ? C3 S2B 1.832(7) . ? S2A C4A 1.789(8) . ? C4A H4AA 0.9700 . ? C4A H4AB 0.9700 . ? C4A C5A 1.508(11) . ? C5A H5AA 0.9700 . ? C5A H5AB 0.9700 . ? C5A C6A 1.55(2) . ? C6A H6AA 0.9700 . ? C6A H6AB 0.9700 . ? C6A S3A 1.804(17) . ? S3A C7 1.823(6) . ? S2B C4B 1.790(8) . ? C4B H4BA 0.9700 . ? C4B H4BB 0.9700 . ? C4B C5B 1.496(11) . ? C5B H5BA 0.9700 . ? C5B H5BB 0.9700 . ? C5B C6B 1.54(2) . ? C6B H6BA 0.9700 . ? C6B H6BB 0.9700 . ? C6B S3B 1.776(16) . ? S3B C7 1.844(6) . ? C7 H7A 0.9700 . ? C7 H7B 0.9700 . ? C7 C8 1.518(7) . ? C8 C9 1.534(8) . ? C8 C13 1.531(7) . ? C8 C14 1.534(7) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 S4 1.816(5) . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 C11 1.523(7) . ? C10 S4 1.807(5) . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C11 C12 1.516(7) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 S1 1.814(5) . ? C13 H13A 0.90(5) . ? C13 H13B 1.02(5) . ? C13 O1 1.425(6) . ? C14 H14A 0.9700 . ? C14 H14B 0.9700 . ? C14 O2 1.427(7) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 O3 1.434(6) . ? C16 H16A 0.9700 . ? C16 H16B 0.9700 . ? C16 O4 1.428(6) . ? O1 H1 0.8200 . ? O2 H2 0.8200 . ? O3 H3 0.8200 . ? O4 H4 0.8200 . ? 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 H1A C1 H1B 107.7 . . ? C2 C1 H1A 108.9 . . ? C2 C1 H1B 108.9 . . ? C2 C1 S1 113.6(3) . . ? S1 C1 H1A 108.9 . . ? S1 C1 H1B 108.9 . . ? C1 C2 C3 111.7(4) . . ? C1 C2 C15 109.3(4) . . ? C1 C2 C16 108.6(4) . . ? C3 C2 C15 107.9(4) . . ? C16 C2 C3 109.1(4) . . ? C16 C2 C15 110.3(4) . . ? C2 C3 H3A 109.4 . . ? C2 C3 H3B 109.4 . . ? C2 C3 S2A 111.0(5) . . ? C2 C3 S2B 113.8(5) . . ? H3A C3 H3B 108.0 . . ? S2A C3 H3A 109.4 . . ? S2A C3 H3B 109.4 . . ? C4A S2A C3 103.0(8) . . ? S2A C4A H4AA 108.5 . . ? S2A C4A H4AB 108.5 . . ? H4AA C4A H4AB 107.5 . . ? C5A C4A S2A 115.1(12) . . ? C5A C4A H4AA 108.5 . . ? C5A C4A H4AB 108.5 . . ? C4A C5A H5AA 109.1 . . ? C4A C5A H5AB 109.1 . . ? C4A C5A C6A 112.4(14) . . ? H5AA C5A H5AB 107.9 . . ? C6A C5A H5AA 109.1 . . ? C6A C5A H5AB 109.1 . . ? C5A C6A H6AA 110.4 . . ? C5A C6A H6AB 110.4 . . ? C5A C6A S3A 106.6(10) . . ? H6AA C6A H6AB 108.6 . . ? S3A C6A H6AA 110.4 . . ? S3A C6A H6AB 110.4 . . ? C6A S3A C7 99.1(6) . . ? C4B S2B C3 96.3(8) . . ? S2B C4B H4BA 109.1 . . ? S2B C4B H4BB 109.1 . . ? H4BA C4B H4BB 107.9 . . ? C5B C4B S2B 112.4(12) . . ? C5B C4B H4BA 109.1 . . ? C5B C4B H4BB 109.1 . . ? C4B C5B H5BA 109.5 . . ? C4B C5B H5BB 109.5 . . ? C4B C5B C6B 110.9(14) . . ? H5BA C5B H5BB 108.0 . . ? C6B C5B H5BA 109.5 . . ? C6B C5B H5BB 109.5 . . ? C5B C6B H6BA 109.5 . . ? C5B C6B H6BB 109.5 . . ? C5B C6B S3B 110.5(11) . . ? H6BA C6B H6BB 108.1 . . ? S3B C6B H6BA 109.5 . . ? S3B C6B H6BB 109.5 . . ? C6B S3B C7 100.3(6) . . ? S3A C7 H7A 107.8 . . ? S3A C7 H7B 107.8 . . ? H7A C7 H7B 107.1 . . ? C8 C7 S3A 118.0(4) . . ? C8 C7 S3B 107.5(4) . . ? C8 C7 H7A 107.8 . . ? C8 C7 H7B 107.8 . . ? C7 C8 C9 112.5(4) . . ? C7 C8 C13 106.5(5) . . ? C7 C8 C14 111.5(4) . . ? C9 C8 C14 106.0(5) . . ? C13 C8 C9 110.6(4) . . ? C13 C8 C14 109.7(4) . . ? C8 C9 H9A 109.1 . . ? C8 C9 H9B 109.1 . . ? C8 C9 S4 112.6(4) . . ? H9A C9 H9B 107.8 . . ? S4 C9 H9A 109.1 . . ? S4 C9 H9B 109.1 . . ? H10A C10 H10B 107.7 . . ? C11 C10 H10A 108.8 . . ? C11 C10 H10B 108.8 . . ? C11 C10 S4 113.8(4) . . ? S4 C10 H10A 108.8 . . ? S4 C10 H10B 108.8 . . ? C10 C11 H11A 109.4 . . ? C10 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? C12 C11 C10 111.1(4) . . ? C12 C11 H11A 109.4 . . ? C12 C11 H11B 109.4 . . ? C11 C12 H12A 108.7 . . ? C11 C12 H12B 108.7 . . ? C11 C12 S1 114.3(3) . . ? H12A C12 H12B 107.6 . . ? S1 C12 H12A 108.7 . . ? S1 C12 H12B 108.7 . . ? H13A C13 H13B 114(4) . . ? C8 C13 H13A 103(3) . . ? C8 C13 H13B 106(3) . . ? O1 C13 H13A 110(3) . . ? O1 C13 H13B 111(3) . . ? O1 C13 C8 112.2(4) . . ? C8 C14 H14A 109.2 . . ? C8 C14 H14B 109.2 . . ? H14A C14 H14B 107.9 . . ? O2 C14 C8 112.0(5) . . ? O2 C14 H14A 109.2 . . ? O2 C14 H14B 109.2 . . ? C2 C15 H15A 109.3 . . ? C2 C15 H15B 109.3 . . ? H15A C15 H15B 107.9 . . ? O3 C15 C2 111.8(4) . . ? O3 C15 H15A 109.3 . . ? O3 C15 H15B 109.3 . . ? C2 C16 H16A 109.2 . . ? C2 C16 H16B 109.2 . . ? H16A C16 H16B 107.9 . . ? O4 C16 C2 112.0(5) . . ? O4 C16 H16A 109.2 . . ? O4 C16 H16B 109.2 . . ? C13 O1 H1 109.5 . . ? C14 O2 H2 109.5 . . ? C15 O3 H3 109.5 . . ? C16 O4 H4 109.5 . . ? C1 S1 C12 98.9(2) . . ? C10 S4 C9 101.4(3) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 C2 C3 S2A 66.6(6) . . . . ? C1 C2 C3 S2B 60.3(7) . . . . ? C1 C2 C15 O3 -175.6(4) . . . . ? C1 C2 C16 O4 59.3(5) . . . . ? C2 C1 S1 C12 -163.9(3) . . . . ? C2 C3 S2A C4A -171.5(7) . . . . ? C2 C3 S2B C4B -170.0(6) . . . . ? C3 C2 C15 O3 62.7(5) . . . . ? C3 C2 C16 O4 -178.7(4) . . . . ? C3 S2A C4A C5A 79.1(14) . . . . ? C3 S2B C4B C5B 89.0(13) . . . . ? S2A C3 S2B C4B 124(7) . . . . ? S2A C4A C5A C6A 82.6(17) . . . . ? C4A C5A C6A S3A -177.2(11) . . . . ? C5A C6A S3A C7 165.2(10) . . . . ? C6A S3A C7 S3B -111.1(16) . . . . ? C6A S3A C7 C8 -150.3(6) . . . . ? S3A C7 C8 C9 69.7(6) . . . . ? S3A C7 C8 C13 -169.0(4) . . . . ? S3A C7 C8 C14 -49.3(6) . . . . ? S2B C3 S2A C4A -55(6) . . . . ? S2B C4B C5B C6B 66.2(16) . . . . ? C4B C5B C6B S3B -178.5(11) . . . . ? C5B C6B S3B C7 -176.4(10) . . . . ? C6B S3B C7 S3A 65.2(15) . . . . ? C6B S3B C7 C8 -150.6(6) . . . . ? S3B C7 C8 C9 61.0(5) . . . . ? S3B C7 C8 C13 -177.6(4) . . . . ? S3B C7 C8 C14 -58.0(5) . . . . ? C7 C8 C9 S4 61.5(5) . . . . ? C7 C8 C13 O1 179.7(4) . . . . ? C7 C8 C14 O2 -54.9(6) . . . . ? C8 C9 S4 C10 -153.0(4) . . . . ? C9 C8 C13 O1 -57.7(6) . . . . ? C9 C8 C14 O2 -177.6(4) . . . . ? C10 C11 C12 S1 178.3(4) . . . . ? C11 C10 S4 C9 73.3(5) . . . . ? C11 C12 S1 C1 80.3(4) . . . . ? C13 C8 C9 S4 -57.6(5) . . . . ? C13 C8 C14 O2 62.9(6) . . . . ? C14 C8 C9 S4 -176.4(3) . . . . ? C14 C8 C13 O1 58.9(6) . . . . ? C15 C2 C3 S2A -173.3(5) . . . . ? C15 C2 C3 S2B -179.6(5) . . . . ? C15 C2 C16 O4 -60.4(5) . . . . ? C16 C2 C3 S2A -53.4(6) . . . . ? C16 C2 C3 S2B -59.8(6) . . . . ? C16 C2 C15 O3 -56.3(5) . . . . ? S1 C1 C2 C3 64.7(5) . . . . ? S1 C1 C2 C15 -54.6(5) . . . . ? S1 C1 C2 C16 -175.0(3) . . . . ? S4 C10 C11 C12 -178.6(4) . . . . ? _shelx_estimated_absorpt_T_max 0.912 _shelx_estimated_absorpt_T_min 0.709 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelxl_version_number 2013-4