#------------------------------------------------------------------------------ #$Date: 2021-04-23 04:43:43 +0300 (Fri, 23 Apr 2021) $ #$Revision: 264435 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/71/7707172.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_7707172 loop_ _publ_author_name 'Li, Jia-Ming' 'Xu, Tian-Yang' 'Zhao, Ya-Li' 'Hu, Xing-Liang' 'He, Kun-Huan' _publ_section_title ; Two 6/10-connected Cu12S6 cluster-based organic frameworks: crystal structure and proton conduction ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT00782C _journal_year 2021 _chemical_formula_moiety 'C12 H30 Cu12 O21 S12' _chemical_formula_sum 'C12 H30 Cu12 O21 S12' _chemical_formula_weight 1657.56 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens mixed _audit_creation_date 2021-04-20 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _audit_update_record ; 2021-04-20 deposited with the CCDC. 2021-04-22 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 96.951(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 11.8921(4) _cell_length_b 17.7132(6) _cell_length_c 18.9516(7) _cell_measurement_reflns_used 9832 _cell_measurement_temperature 298.15 _cell_measurement_theta_max 32.6230 _cell_measurement_theta_min 2.4830 _cell_volume 3962.8(2) _computing_cell_refinement 'CrysAlisPro 1.171.39.34a (Rigaku OD, 2017)' _computing_data_collection 'CrysAlisPro 1.171.39.34a (Rigaku OD, 2017)' _computing_data_reduction 'CrysAlisPro 1.171.39.34a (Rigaku OD, 2017)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 298.15 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -14.00 12.00 1.00 10.00 -- 30.00 54.00 -60.00 26 2 \w 51.00 92.00 1.00 10.00 -- 30.00 54.00 -60.00 41 3 \w 16.00 42.00 1.00 10.00 -- 30.00 54.00-150.00 26 4 \w -63.00 119.00 1.00 10.00 -- 30.00 54.00 120.00 182 ; _diffrn_measurement_device 'two-circle diffractometer' _diffrn_measurement_device_type 'XtaLAB Mini (ROW)' _diffrn_measurement_method '\w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0249 _diffrn_reflns_av_unetI/netI 0.0296 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_number 16906 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.097 _diffrn_reflns_theta_max 25.097 _diffrn_reflns_theta_min 2.452 _exptl_absorpt_coefficient_mu 7.004 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.43478 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.39.34a (Rigaku Oxford Diffraction, 2017) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour red _exptl_crystal_colour_primary red _exptl_crystal_density_diffrn 2.778 _exptl_crystal_description block _exptl_crystal_F_000 3240 _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.15 _refine_diff_density_max 0.844 _refine_diff_density_min -1.387 _refine_diff_density_rms 0.139 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 558 _refine_ls_number_reflns 7036 _refine_ls_number_restraints 14 _refine_ls_restrained_S_all 1.065 _refine_ls_R_factor_all 0.0421 _refine_ls_R_factor_gt 0.0317 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0369P)^2^+4.3695P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0746 _refine_ls_wR_factor_ref 0.0787 _reflns_Friedel_coverage 0.000 _reflns_number_gt 5847 _reflns_number_total 7036 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt00782c2.cif _cod_data_source_block 190108c _cod_database_code 7707172 _shelx_shelxl_version_number 2018/3 _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. ; _shelx_estimated_absorpt_t_max 0.420 _shelx_estimated_absorpt_t_min 0.273 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H,H) groups At 1.5 times of: All O(H,H) groups 2. Restrained distances S3-O4 = S3-O5 = S3-O6 1.45 with sigma of 0.02 S3A-O4A = S3A-O5A = S3A-O6A 1.45 with sigma of 0.02 C3-C4 = C3A-C4A 1.53 with sigma of 0.02 C3-S3 = C3-S3A 1.78 with sigma of 0.02 C4-S4 = C4A-S4 1.83 with sigma of 0.02 O7-Cu4 \\sim O7-Cu4A with sigma of 0.02 S5-Cu4 \\sim S5-Cu4A with sigma of 0.02 S4-Cu4 \\sim S4-Cu4A with sigma of 0.02 3. Uiso/Uaniso restraints and constraints Uanis(C4) = Uanis(C4A) = Uanis(C3) = Uanis(C3A) Uanis(Cu4) = Uanis(Cu4A) 4. Others Sof(S3A)=Sof(O4A)=Sof(O5A)=Sof(O6A)=Sof(C3A)=Sof(H3AA)=Sof(H3AB)=Sof(C4A)= Sof(H4AA)=Sof(H4AB)=1-FVAR(1) Sof(C3)=Sof(H3A)=Sof(H3B)=Sof(C4)=Sof(H4A)=Sof(H4B)=Sof(S3)=Sof(O4)=Sof(O5)= Sof(O6)=FVAR(1) Sof(Cu4A)=1-FVAR(2) Sof(Cu4)=FVAR(2) 5.a Rotating group: O7(H7A,H7B), O15(H15A,H15B), O14(H14A,H14B) 5.b Secondary CH2 refined with riding coordinates: C6(H6A,H6B), C7(H7C,H7D), C12(H12A,H12B), C5(H5A,H5B), C8(H8A,H8B), C11(H11A, H11B), C1(H1A,H1B), C2(H2A,H2B), C10(H10A,H10B), C3(H3A,H3B), C9(H9A,H9B), C4(H4A,H4B), C3A(H3AA,H3AB), C4A(H4AA,H4AB) ; _shelx_res_file ; TITL 190108c_a.res in P2(1)/c 190108c.res created by SHELXL-2018/3 at 08:52:55 on 20-Apr-2021 REM Old TITL 190108C in P21/c #14 REM SHELXT solution in P2(1)/c REM R1 0.152, Rweak 0.003, Alpha 0.026, Orientation as input REM Formula found by SHELXT: C16 N2 O16 S13 Cu11 CELL 0.71073 11.892128 17.713178 18.951606 90 96.9509 90 ZERR 4 0.000403 0.000608 0.000671 0 0.0033 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cu O S UNIT 48 120 48 84 48 EQIV $1 -1+X,0.5-Y,-0.5+Z EQIV $2 1-X,-Y,1-Z EQIV $3 -1+X,+Y,+Z EQIV $4 +X,-1+Y,+Z EQIV $5 1-X,-0.5+Y,1.5-Z EQIV $6 -X,-0.5+Y,1.5-Z EQIV $7 1+X,+Y,+Z EQIV $8 1-X,0.5+Y,1.5-Z EQIV $9 +X,0.5-Y,0.5+Z EQIV $10 -X,1-Y,1-Z EQIV $11 1-X,1-Y,2-Z DFIX 1.45 S3 O4 S3 O5 S3 O6 DFIX 1.45 S3A O4A S3A O5A S3A O6A DFIX 1.53 C3 C4 C3A C4A DFIX 1.78 C3 S3 C3 S3A DFIX 1.83 C4 S4 C4A S4 EADP C4 C4A C3 C3A SADI O7 Cu4 O7 Cu4A SADI S5 Cu4 S5 Cu4A SADI S4 Cu4 S4 Cu4A EADP Cu4 Cu4A L.S. 20 PLAN 10 SIZE 0.25 0.2 0.15 TEMP 25 CONF HTAB O7 O21_$1 HTAB O7 O19_$1 HTAB O7 O17_$1 HTAB O15 O2_$8 HTAB O15 O3_$8 HTAB O15 O3_$9 HTAB C6 O19_$8 HTAB C6 O4_$10 HTAB C7 O18_$11 HTAB C7 O15_$11 HTAB C12 O2_$2 HTAB C12 O17 HTAB C5 O21_$1 HTAB C5 O14_$3 HTAB C8 O3_$8 HTAB C8 O14 HTAB C11 O12_$4 HTAB C1 O20_$2 HTAB C10 O13_$5 HTAB C10 O1_$9 HTAB C3 O20_$8 HTAB C3 O8_$6 HTAB C9 O9_$5 HTAB C4 O11_$6 HTAB O14 O10_$7 HTAB O14 O8_$7 BOND $H LIST 6 MORE -1 fmap 2 acta OMIT 0 50.2 OMIT 0 0 2 OMIT -1 1 1 OMIT 1 1 1 OMIT 0 2 1 OMIT 0 2 0 OMIT -2 0 2 OMIT -3 3 6 OMIT 1 5 2 OMIT 1 0 2 REM REM REM WGHT 0.036900 4.369500 FVAR 0.11555 0.63307 0.82088 CU12 3 0.647238 0.132913 1.137632 11.00000 0.01488 0.02764 = 0.02410 0.00408 0.00370 -0.00505 CU3 3 0.129477 0.035821 0.630880 11.00000 0.01475 0.02264 = 0.02833 0.00173 0.00362 -0.00532 CU2 3 -0.120619 0.129019 0.378051 11.00000 0.01986 0.02812 = 0.02423 -0.00627 0.00400 0.00464 CU7 3 0.237241 0.788368 0.745355 11.00000 0.02467 0.02680 = 0.01999 -0.00096 0.00524 -0.00178 CU6 3 0.024834 0.861430 0.759229 11.00000 0.02085 0.02287 = 0.02614 0.00606 -0.00219 0.00049 CU1 3 0.553197 0.141851 0.270398 11.00000 0.02193 0.02465 = 0.02397 -0.00425 -0.00106 -0.00252 CU5 3 -0.061957 0.521441 0.729311 11.00000 0.02715 0.02328 = 0.02709 0.01055 -0.00054 -0.00122 CU11 3 0.398027 0.030727 0.876768 11.00000 0.02062 0.02512 = 0.03407 -0.00765 0.00203 0.00514 CU8 3 0.530163 0.513486 0.775744 11.00000 0.02737 0.02279 = 0.03220 -0.01177 -0.00276 0.00330 CU9 3 0.736168 0.594628 0.747972 11.00000 0.02977 0.03322 = 0.02251 0.00276 0.00981 0.00376 CU10 3 0.670239 0.446392 0.897941 11.00000 0.03760 0.01878 = 0.03715 -0.00106 0.00914 0.00219 PART 1 CU4 3 -0.153502 0.447792 0.608931 31.00000 0.07726 0.02237 = 0.03157 0.00392 0.02481 0.00582 PART 0 S11 5 0.484753 -0.059514 0.822926 11.00000 0.00950 0.01573 = 0.01546 0.00151 0.00165 0.00003 S4 5 -0.168467 0.334531 0.655917 11.00000 0.01339 0.01456 = 0.01573 -0.00448 0.00291 0.00176 S2 5 -0.012687 0.048040 0.327599 11.00000 0.00875 0.01296 = 0.01743 -0.00026 0.00174 -0.00134 S9 5 0.697763 0.332127 0.855086 11.00000 0.01706 0.01379 = 0.01467 0.00311 0.00220 -0.00172 S6 5 0.011246 0.691407 0.692525 11.00000 0.01937 0.01197 = 0.02196 -0.00322 0.00335 -0.00457 S7 5 0.457386 0.686687 0.801682 11.00000 0.01694 0.01372 = 0.02363 0.00418 0.00404 0.00580 S12 5 0.856280 -0.064274 0.862184 11.00000 0.01043 0.03420 = 0.02070 -0.00714 0.00459 -0.00195 S5 5 -0.211414 0.556922 0.645712 11.00000 0.01539 0.01653 = 0.01921 0.00452 0.00298 -0.00263 S10 5 0.563926 0.141844 0.970931 11.00000 0.03139 0.01948 = 0.01828 -0.00161 0.00616 -0.01072 S1 5 0.356562 0.084756 0.365755 11.00000 0.01101 0.02714 = 0.01967 0.00163 0.00244 -0.00276 S8 5 0.683197 0.558699 0.850615 11.00000 0.01419 0.01631 = 0.01894 -0.00223 0.00291 0.00538 O18 4 0.572845 0.179199 1.039671 11.00000 0.03980 0.02156 = 0.01494 0.00104 -0.00023 -0.00443 O20 4 0.869001 -0.129821 0.817429 11.00000 0.01783 0.02873 = 0.03029 -0.00545 0.00809 0.00224 O2 4 0.379643 0.012004 0.332783 11.00000 0.02130 0.02455 = 0.04174 -0.00277 0.01283 0.00104 O12 4 0.521406 0.754327 0.785197 11.00000 0.02486 0.01719 = 0.03856 0.01117 0.00420 0.00079 O10 4 -0.052779 0.760259 0.706669 11.00000 0.02375 0.01771 = 0.03737 -0.01003 0.00227 -0.00031 O11 4 0.339129 0.703733 0.807376 11.00000 0.01921 0.04059 = 0.05683 0.02496 0.01018 0.01151 O3 4 0.388498 0.083160 0.442329 11.00000 0.03141 0.07378 = 0.02258 -0.00211 -0.00295 0.00240 O16 4 0.451882 0.108343 0.951514 11.00000 0.03489 0.03961 = 0.03738 -0.01068 -0.00187 -0.01004 O9 4 0.129724 0.707160 0.684920 11.00000 0.01731 0.03781 = 0.04829 -0.01904 0.00673 -0.00850 O13 4 0.470447 0.625758 0.751881 11.00000 0.05356 0.02237 = 0.02376 -0.00197 -0.00597 0.01054 O1 4 0.405348 0.148299 0.330466 11.00000 0.02543 0.02338 = 0.04992 0.00235 0.01809 -0.00608 O21 4 0.869406 -0.082277 0.937698 11.00000 0.02296 0.07864 = 0.02083 -0.00113 0.00088 0.00749 O19 4 0.931203 -0.001989 0.846411 11.00000 0.02710 0.04045 = 0.05885 -0.02102 0.02455 -0.01665 O8 4 -0.001537 0.633711 0.745370 11.00000 0.05951 0.02063 = 0.02107 0.00163 -0.00377 -0.01296 O7 4 -0.115127 0.439507 0.507489 11.00000 0.08534 0.07053 = 0.02781 0.00176 0.01389 -0.01585 AFIX 7 H7A 2 -0.088602 0.484129 0.488003 11.00000 -1.50000 H7B 2 -0.175668 0.424881 0.473604 11.00000 -1.50000 AFIX 0 O17 4 0.652758 0.089210 0.965168 11.00000 0.03998 0.04850 = 0.08224 -0.02013 0.01539 0.00855 O15 4 0.643445 0.439662 1.000517 11.00000 0.15499 0.05250 = 0.05919 -0.01440 0.06847 -0.02820 AFIX 7 H15A 2 0.571719 0.425352 1.005139 11.00000 -1.50000 H15B 2 0.655855 0.483828 1.024952 11.00000 -1.50000 AFIX 0 C6 1 -0.046616 0.658617 0.607100 11.00000 0.02492 0.01698 = 0.01771 -0.00080 0.00648 -0.00603 AFIX 23 H6A 2 -0.032211 0.696407 0.572255 11.00000 -1.20000 H6B 2 -0.006349 0.613182 0.596473 11.00000 -1.20000 AFIX 0 C7 1 0.514484 0.657122 0.888410 11.00000 0.02547 0.01731 = 0.01959 0.00188 0.01048 0.00821 AFIX 23 H7C 2 0.497733 0.695526 0.922102 11.00000 -1.20000 H7D 2 0.476016 0.611245 0.899873 11.00000 -1.20000 AFIX 0 C12 1 0.715801 -0.029975 0.840575 11.00000 0.01395 0.01984 = 0.02455 -0.00338 0.00472 -0.00166 AFIX 23 H12A 2 0.708349 0.018126 0.864031 11.00000 -1.20000 H12B 2 0.701260 -0.021717 0.789691 11.00000 -1.20000 AFIX 0 C5 1 -0.173298 0.641230 0.597797 11.00000 0.02026 0.01920 = 0.01694 0.00562 -0.00089 -0.00047 AFIX 23 H5A 2 -0.198521 0.634571 0.547568 11.00000 -1.20000 H5B 2 -0.213444 0.684273 0.614136 11.00000 -1.20000 AFIX 0 C8 1 0.641803 0.642387 0.898669 11.00000 0.02205 0.01535 = 0.01858 -0.00358 -0.00087 0.00214 AFIX 23 H8A 2 0.666560 0.635911 0.948977 11.00000 -1.20000 H8B 2 0.680474 0.686206 0.882577 11.00000 -1.20000 AFIX 0 C11 1 0.628777 -0.084745 0.863041 11.00000 0.01176 0.02325 = 0.02522 0.00599 -0.00149 0.00318 AFIX 23 H11A 2 0.631848 -0.084276 0.914419 11.00000 -1.20000 H11B 2 0.646651 -0.135433 0.848546 11.00000 -1.20000 AFIX 0 C1 1 0.208113 0.100985 0.350469 11.00000 0.01430 0.02156 = 0.03373 -0.00048 0.00374 -0.00129 AFIX 23 H1A 2 0.189884 0.143396 0.379408 11.00000 -1.20000 H1B 2 0.188370 0.115097 0.301068 11.00000 -1.20000 AFIX 0 C2 1 0.135539 0.034132 0.366630 11.00000 0.01455 0.03065 = 0.04251 0.01558 0.00098 -0.00266 AFIX 23 H2A 2 0.138609 0.028083 0.417697 11.00000 -1.20000 H2B 2 0.165139 -0.011523 0.347454 11.00000 -1.20000 AFIX 0 C10 1 0.570025 0.216414 0.907526 11.00000 0.04438 0.04707 = 0.02336 0.00758 -0.00182 -0.01008 AFIX 23 H10A 2 0.561106 0.195358 0.859928 11.00000 -1.20000 H10B 2 0.508016 0.251273 0.910960 11.00000 -1.20000 AFIX 0 PART 1 C3 1 -0.033760 0.227555 0.597234 21.00000 0.02205 0.02469 = 0.02392 -0.01782 0.00198 0.00206 AFIX 23 H3A 2 -0.014795 0.209398 0.645494 21.00000 -1.20000 H3B 2 0.021050 0.265916 0.588412 21.00000 -1.20000 AFIX 0 PART 0 C9 1 0.677832 0.257430 0.919657 11.00000 0.04213 0.03260 = 0.02453 0.01491 -0.00173 -0.01158 AFIX 23 H9A 2 0.739089 0.221301 0.919457 11.00000 -1.20000 H9B 2 0.684083 0.279857 0.966663 11.00000 -1.20000 AFIX 0 PART 1 C4 1 -0.150197 0.261405 0.589259 21.00000 0.02205 0.02469 = 0.02392 -0.01782 0.00198 0.00206 AFIX 23 H4A 2 -0.205144 0.221594 0.593074 21.00000 -1.20000 H4B 2 -0.165759 0.283346 0.542195 21.00000 -1.20000 AFIX 0 PART 0 O14 4 0.735659 0.711874 0.748126 11.00000 0.03795 0.02730 = 0.09319 -0.00166 0.03791 -0.00017 AFIX 7 H14A 2 0.803780 0.729314 0.746507 11.00000 -1.50000 H14B 2 0.711047 0.729294 0.786445 11.00000 -1.50000 AFIX 0 PART 1 S3 5 -0.026750 0.151749 0.536812 21.00000 0.02293 0.01092 = 0.01518 0.00113 0.00299 0.00515 O4 4 -0.033858 0.185836 0.465925 21.00000 0.04004 0.02048 = 0.01414 0.00196 -0.00521 -0.00491 O5 4 0.083829 0.115575 0.556002 21.00000 0.02400 0.02653 = 0.03040 0.00762 0.00425 0.01272 O6 4 -0.121471 0.102743 0.544667 21.00000 0.03262 0.02108 = 0.04780 0.00056 0.01051 -0.00544 PART 2 S3A 5 0.013081 0.172676 0.530179 -21.00000 0.02686 0.02005 = 0.01682 -0.00320 0.00165 0.00974 O4A 4 -0.077931 0.176124 0.471022 -21.00000 0.03651 0.03779 = 0.02708 -0.01611 -0.01561 0.01713 O5A 4 0.009847 0.102672 0.569891 -21.00000 0.03974 0.02227 = 0.04811 0.00501 -0.00229 0.01073 O6A 4 0.123244 0.186406 0.507548 -21.00000 0.02909 0.03816 = 0.04506 -0.00363 0.02133 0.00700 C3A 1 -0.014781 0.246910 0.590138 -21.00000 0.02205 0.02469 = 0.02392 -0.01782 0.00198 0.00206 AFIX 23 H3AA 2 0.035979 0.241395 0.633910 -21.00000 -1.20000 H3AB 2 0.001419 0.295070 0.569193 -21.00000 -1.20000 AFIX 0 C4A 1 -0.136235 0.247463 0.607560 -21.00000 0.02205 0.02469 = 0.02392 -0.01782 0.00198 0.00206 AFIX 23 H4AA 2 -0.148552 0.203740 0.636471 -21.00000 -1.20000 H4AB 2 -0.187543 0.243875 0.563826 -21.00000 -1.20000 AFIX 0 CU4A 3 -0.194684 0.442176 0.583178 -31.00000 0.07726 0.02237 = 0.03157 0.00392 0.02481 0.00582 HKLF 4 REM 190108c_a.res in P2(1)/c REM wR2 = 0.0787, GooF = S = 1.047, Restrained GooF = 1.065 for all data REM R1 = 0.0317 for 5847 Fo > 4sig(Fo) and 0.0421 for all 7036 data REM 558 parameters refined using 14 restraints END WGHT 0.0369 4.3706 REM Highest difference peak 0.844, deepest hole -1.387, 1-sigma level 0.139 Q1 1 0.6694 0.1897 0.9162 11.00000 0.05 0.84 Q2 1 0.4838 0.1336 0.9226 11.00000 0.05 0.65 Q3 1 0.6487 0.0537 0.9999 11.00000 0.05 0.64 Q4 1 0.5635 0.5389 0.7418 11.00000 0.05 0.59 Q5 1 -0.0909 0.4531 0.6040 11.00000 0.05 0.57 Q6 1 0.7422 0.4437 0.9376 11.00000 0.05 0.57 Q7 1 0.5921 0.4405 0.8974 11.00000 0.05 0.56 Q8 1 0.6084 0.2793 0.9186 11.00000 0.05 0.53 Q9 1 0.6142 0.1648 1.0655 11.00000 0.05 0.51 Q10 1 0.5822 0.4433 0.9846 11.00000 0.05 0.51 ; _shelx_res_checksum 20610 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' 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 Cu12 Cu 0.64724(4) 0.13291(3) 1.13763(3) 0.02210(13) Uani 1 1 d . . . . . Cu3 Cu 0.12948(4) 0.03582(3) 0.63088(3) 0.02183(12) Uani 1 1 d . . . . . Cu2 Cu -0.12062(4) 0.12902(3) 0.37805(3) 0.02396(13) Uani 1 1 d . . . . . Cu7 Cu 0.23724(4) 0.78837(3) 0.74535(2) 0.02361(13) Uani 1 1 d . . . . . Cu6 Cu 0.02483(4) 0.86143(3) 0.75923(3) 0.02370(13) Uani 1 1 d . . . . . Cu1 Cu 0.55320(4) 0.14185(3) 0.27040(3) 0.02383(13) Uani 1 1 d . . . . . Cu5 Cu -0.06196(5) 0.52144(3) 0.72931(3) 0.02616(13) Uani 1 1 d . . . . . Cu11 Cu 0.39803(4) 0.03073(3) 0.87677(3) 0.02671(13) Uani 1 1 d . . . . . Cu8 Cu 0.53016(5) 0.51349(3) 0.77574(3) 0.02798(14) Uani 1 1 d . . . . . Cu9 Cu 0.73617(5) 0.59463(3) 0.74797(3) 0.02795(14) Uani 1 1 d . . . . . Cu10 Cu 0.67024(5) 0.44639(3) 0.89794(3) 0.03080(14) Uani 1 1 d . . . . . Cu4 Cu -0.15350(17) 0.44779(5) 0.60893(10) 0.0422(4) Uani 0.821(5) 1 d D . P A 1 S11 S 0.48475(8) -0.05951(5) 0.82293(5) 0.0136(2) Uani 1 1 d . . . . . S4 S -0.16847(8) 0.33453(5) 0.65592(5) 0.0145(2) Uani 1 1 d D . . . . S2 S -0.01269(8) 0.04804(5) 0.32760(5) 0.0130(2) Uani 1 1 d . . . . . S9 S 0.69776(8) 0.33213(5) 0.85509(5) 0.0151(2) Uani 1 1 d . . . . . S6 S 0.01125(8) 0.69141(5) 0.69253(5) 0.0177(2) Uani 1 1 d . . . . . S7 S 0.45739(8) 0.68669(5) 0.80168(5) 0.0180(2) Uani 1 1 d . . . . . S12 S 0.85628(8) -0.06427(6) 0.86218(5) 0.0216(2) Uani 1 1 d . . . . . S5 S -0.21141(8) 0.55692(5) 0.64571(5) 0.0170(2) Uani 1 1 d D . . . . S10 S 0.56393(9) 0.14184(6) 0.97093(5) 0.0228(2) Uani 1 1 d . . . . . S1 S 0.35656(8) 0.08476(6) 0.36576(5) 0.0192(2) Uani 1 1 d . . . . . S8 S 0.68320(8) 0.55870(5) 0.85062(5) 0.0164(2) Uani 1 1 d . . . . . O18 O 0.5728(3) 0.17920(16) 1.03967(14) 0.0257(7) Uani 1 1 d . . . . . O20 O 0.8690(2) -0.12982(16) 0.81743(15) 0.0252(7) Uani 1 1 d . . . . . O2 O 0.3796(2) 0.01200(16) 0.33278(16) 0.0285(7) Uani 1 1 d . . . . . O12 O 0.5214(2) 0.75433(15) 0.78520(16) 0.0268(7) Uani 1 1 d . . . . . O10 O -0.0528(2) 0.76026(15) 0.70667(16) 0.0264(7) Uani 1 1 d . . . . . O11 O 0.3391(3) 0.70373(18) 0.80738(18) 0.0384(8) Uani 1 1 d . . . . . O3 O 0.3885(3) 0.0832(2) 0.44233(16) 0.0431(9) Uani 1 1 d . . . . . O16 O 0.4519(3) 0.10834(18) 0.95151(17) 0.0378(8) Uani 1 1 d . . . . . O9 O 0.1297(2) 0.70716(18) 0.68492(17) 0.0342(8) Uani 1 1 d . . . . . O13 O 0.4704(3) 0.62576(16) 0.75188(15) 0.0341(8) Uani 1 1 d . . . . . O1 O 0.4053(3) 0.14830(16) 0.33047(17) 0.0318(7) Uani 1 1 d . . . . . O21 O 0.8694(3) -0.0823(2) 0.93770(15) 0.0410(9) Uani 1 1 d . . . . . O19 O 0.9312(3) -0.00199(19) 0.84641(18) 0.0406(9) Uani 1 1 d . . . . . O8 O -0.0015(3) 0.63371(16) 0.74537(15) 0.0344(8) Uani 1 1 d . . . . . O7 O -0.1151(4) 0.4395(2) 0.50749(18) 0.0606(12) Uani 1 1 d D . . . . H7A H -0.088602 0.484129 0.488003 0.091 Uiso 1 1 d R U . A . H7B H -0.175668 0.424881 0.473604 0.091 Uiso 1 1 d R U . . . O17 O 0.6528(3) 0.0892(2) 0.9652(2) 0.0563(11) Uani 1 1 d . . . . . O15 O 0.6434(5) 0.4397(2) 1.0005(2) 0.0843(17) Uani 1 1 d . . . . . H15A H 0.571719 0.425352 1.005139 0.127 Uiso 1 1 d R U . . . H15B H 0.655855 0.483828 1.024952 0.127 Uiso 1 1 d R U . . . C6 C -0.0466(3) 0.6586(2) 0.6071(2) 0.0196(9) Uani 1 1 d . . . . . H6A H -0.032211 0.696407 0.572255 0.023 Uiso 1 1 calc R U . . . H6B H -0.006349 0.613182 0.596473 0.023 Uiso 1 1 calc R U . . . C7 C 0.5145(3) 0.6571(2) 0.8884(2) 0.0202(9) Uani 1 1 d . . . . . H7C H 0.497733 0.695526 0.922102 0.024 Uiso 1 1 calc R U . . . H7D H 0.476016 0.611245 0.899873 0.024 Uiso 1 1 calc R U . . . C12 C 0.7158(3) -0.0300(2) 0.8406(2) 0.0193(9) Uani 1 1 d . . . . . H12A H 0.708349 0.018126 0.864031 0.023 Uiso 1 1 calc R U . . . H12B H 0.701260 -0.021717 0.789691 0.023 Uiso 1 1 calc R U . . . C5 C -0.1733(3) 0.6412(2) 0.5978(2) 0.0191(9) Uani 1 1 d . . . . . H5A H -0.198521 0.634571 0.547568 0.023 Uiso 1 1 calc R U . . . H5B H -0.213444 0.684273 0.614136 0.023 Uiso 1 1 calc R U . . . C8 C 0.6418(3) 0.6424(2) 0.8987(2) 0.0189(9) Uani 1 1 d . . . . . H8A H 0.666560 0.635911 0.948977 0.023 Uiso 1 1 calc R U . . . H8B H 0.680474 0.686206 0.882577 0.023 Uiso 1 1 calc R U . . . C11 C 0.6288(3) -0.0847(2) 0.8630(2) 0.0204(9) Uani 1 1 d . . . . . H11A H 0.631848 -0.084276 0.914419 0.024 Uiso 1 1 calc R U . . . H11B H 0.646651 -0.135433 0.848546 0.024 Uiso 1 1 calc R U . . . C1 C 0.2081(3) 0.1010(2) 0.3505(2) 0.0231(9) Uani 1 1 d . . . . . H1A H 0.189884 0.143396 0.379408 0.028 Uiso 1 1 calc R U . . . H1B H 0.188370 0.115097 0.301068 0.028 Uiso 1 1 calc R U . . . C2 C 0.1355(4) 0.0341(2) 0.3666(3) 0.0294(10) Uani 1 1 d . . . . . H2A H 0.138609 0.028083 0.417697 0.035 Uiso 1 1 calc R U . . . H2B H 0.165139 -0.011523 0.347454 0.035 Uiso 1 1 calc R U . . . C10 C 0.5700(4) 0.2164(3) 0.9075(2) 0.0388(12) Uani 1 1 d . . . . . H10A H 0.561106 0.195358 0.859928 0.047 Uiso 1 1 calc R U . . . H10B H 0.508016 0.251273 0.910960 0.047 Uiso 1 1 calc R U . . . C3 C -0.0338(8) 0.2276(5) 0.5972(6) 0.0236(16) Uani 0.633(6) 1 d D . P A 1 H3A H -0.014795 0.209398 0.645494 0.028 Uiso 0.633(6) 1 calc R U P A 1 H3B H 0.021050 0.265916 0.588412 0.028 Uiso 0.633(6) 1 calc R U P A 1 C9 C 0.6778(4) 0.2574(3) 0.9197(2) 0.0336(11) Uani 1 1 d . . . . . H9A H 0.739089 0.221301 0.919457 0.040 Uiso 1 1 calc R U . . . H9B H 0.684083 0.279857 0.966663 0.040 Uiso 1 1 calc R U . . . C4 C -0.1502(8) 0.2614(6) 0.5893(4) 0.0236(16) Uani 0.633(6) 1 d D . P A 1 H4A H -0.205144 0.221594 0.593074 0.028 Uiso 0.633(6) 1 calc R U P A 1 H4B H -0.165759 0.283346 0.542195 0.028 Uiso 0.633(6) 1 calc R U P A 1 O14 O 0.7357(3) 0.7119(2) 0.7481(2) 0.0504(11) Uani 1 1 d . . . . . H14A H 0.803780 0.729314 0.746507 0.076 Uiso 1 1 d R U . . . H14B H 0.711047 0.729294 0.786445 0.076 Uiso 1 1 d R U . . . S3 S -0.0268(3) 0.15175(16) 0.53681(14) 0.0163(6) Uani 0.633(6) 1 d D . P A 1 O4 O -0.0339(7) 0.1858(7) 0.4659(5) 0.026(2) Uani 0.633(6) 1 d D . P A 1 O5 O 0.0838(5) 0.1156(3) 0.5560(3) 0.0269(13) Uani 0.633(6) 1 d D . P A 1 O6 O -0.1215(4) 0.1027(3) 0.5447(3) 0.0334(14) Uani 0.633(6) 1 d D . P A 1 S3A S 0.0131(5) 0.1727(3) 0.5302(3) 0.0213(11) Uani 0.367(6) 1 d D . P A 2 O4A O -0.0779(12) 0.1761(13) 0.4710(9) 0.035(5) Uani 0.367(6) 1 d D . P A 2 O5A O 0.0098(10) 0.1027(5) 0.5699(5) 0.037(3) Uani 0.367(6) 1 d D . P A 2 O6A O 0.1232(7) 0.1864(5) 0.5075(5) 0.036(3) Uani 0.367(6) 1 d D . P A 2 C3A C -0.0148(14) 0.2469(10) 0.5901(12) 0.0236(16) Uani 0.367(6) 1 d D . P A 2 H3AA H 0.035979 0.241395 0.633910 0.028 Uiso 0.367(6) 1 calc R U P A 2 H3AB H 0.001419 0.295070 0.569193 0.028 Uiso 0.367(6) 1 calc R U P A 2 C4A C -0.1362(13) 0.2475(10) 0.6076(8) 0.0236(16) Uani 0.367(6) 1 d D . P A 2 H4AA H -0.148552 0.203740 0.636471 0.028 Uiso 0.367(6) 1 calc R U P A 2 H4AB H -0.187543 0.243875 0.563826 0.028 Uiso 0.367(6) 1 calc R U P A 2 Cu4A Cu -0.1947(7) 0.4422(3) 0.5832(4) 0.0422(4) Uani 0.179(5) 1 d D . P A 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 Cu12 0.0149(3) 0.0276(3) 0.0241(3) 0.0041(2) 0.0037(2) -0.0051(2) Cu3 0.0148(3) 0.0226(3) 0.0283(3) 0.0017(2) 0.0036(2) -0.0053(2) Cu2 0.0199(3) 0.0281(3) 0.0242(3) -0.0063(2) 0.0040(2) 0.0046(2) Cu7 0.0247(3) 0.0268(3) 0.0200(3) -0.0010(2) 0.0052(2) -0.0018(2) Cu6 0.0208(3) 0.0229(3) 0.0261(3) 0.0061(2) -0.0022(2) 0.0005(2) Cu1 0.0219(3) 0.0247(3) 0.0240(3) -0.0042(2) -0.0011(2) -0.0025(2) Cu5 0.0272(3) 0.0233(3) 0.0271(3) 0.0106(2) -0.0005(2) -0.0012(2) Cu11 0.0206(3) 0.0251(3) 0.0341(3) -0.0077(2) 0.0020(2) 0.0051(2) Cu8 0.0274(3) 0.0228(3) 0.0322(3) -0.0118(2) -0.0028(2) 0.0033(2) Cu9 0.0298(3) 0.0332(3) 0.0225(3) 0.0028(2) 0.0098(2) 0.0038(2) Cu10 0.0376(3) 0.0188(3) 0.0372(3) -0.0011(2) 0.0091(3) 0.0022(2) Cu4 0.0773(10) 0.0224(4) 0.0316(8) 0.0039(4) 0.0248(7) 0.0058(4) S11 0.0095(5) 0.0157(5) 0.0155(4) 0.0015(4) 0.0017(4) 0.0000(4) S4 0.0134(5) 0.0146(5) 0.0157(4) -0.0045(4) 0.0029(4) 0.0018(4) S2 0.0088(4) 0.0130(4) 0.0174(5) -0.0003(4) 0.0017(4) -0.0013(4) S9 0.0171(5) 0.0138(4) 0.0147(4) 0.0031(4) 0.0022(4) -0.0017(4) S6 0.0194(5) 0.0120(5) 0.0220(5) -0.0032(4) 0.0034(4) -0.0046(4) S7 0.0169(5) 0.0137(5) 0.0236(5) 0.0042(4) 0.0040(4) 0.0058(4) S12 0.0104(5) 0.0342(6) 0.0207(5) -0.0071(5) 0.0046(4) -0.0020(4) S5 0.0154(5) 0.0165(5) 0.0192(5) 0.0045(4) 0.0030(4) -0.0026(4) S10 0.0314(6) 0.0195(5) 0.0183(5) -0.0016(4) 0.0062(4) -0.0107(4) S1 0.0110(5) 0.0271(5) 0.0197(5) 0.0016(4) 0.0024(4) -0.0028(4) S8 0.0142(5) 0.0163(5) 0.0189(5) -0.0022(4) 0.0029(4) 0.0054(4) O18 0.0398(19) 0.0216(15) 0.0149(13) 0.0010(12) -0.0002(13) -0.0044(13) O20 0.0178(15) 0.0287(16) 0.0303(16) -0.0054(14) 0.0081(13) 0.0022(13) O2 0.0213(16) 0.0246(16) 0.0417(18) -0.0028(14) 0.0128(14) 0.0010(13) O12 0.0249(16) 0.0172(15) 0.0386(17) 0.0112(14) 0.0042(14) 0.0008(12) O10 0.0237(16) 0.0177(14) 0.0374(17) -0.0100(13) 0.0023(14) -0.0003(12) O11 0.0192(17) 0.0406(19) 0.057(2) 0.0250(17) 0.0102(15) 0.0115(14) O3 0.0314(19) 0.074(3) 0.0226(16) -0.0021(17) -0.0029(14) 0.0024(18) O16 0.035(2) 0.0396(19) 0.0374(18) -0.0107(16) -0.0019(15) -0.0100(16) O9 0.0173(16) 0.0378(18) 0.0483(19) -0.0190(16) 0.0067(14) -0.0085(14) O13 0.054(2) 0.0224(16) 0.0238(16) -0.0020(13) -0.0060(15) 0.0105(15) O1 0.0254(17) 0.0234(16) 0.0499(19) 0.0024(15) 0.0181(15) -0.0061(13) O21 0.0230(17) 0.079(3) 0.0208(16) -0.0011(17) 0.0009(14) 0.0075(17) O19 0.0271(18) 0.040(2) 0.059(2) -0.0210(18) 0.0245(17) -0.0166(15) O8 0.060(2) 0.0206(15) 0.0211(15) 0.0016(13) -0.0038(15) -0.0130(15) O7 0.085(3) 0.071(3) 0.0278(19) 0.0018(19) 0.014(2) -0.016(2) O17 0.040(2) 0.049(2) 0.082(3) -0.020(2) 0.015(2) 0.0085(18) O15 0.155(5) 0.052(3) 0.059(3) -0.014(2) 0.068(3) -0.028(3) C6 0.025(2) 0.017(2) 0.0177(19) -0.0008(17) 0.0065(17) -0.0060(17) C7 0.025(2) 0.017(2) 0.0196(19) 0.0019(17) 0.0105(17) 0.0082(17) C12 0.014(2) 0.020(2) 0.025(2) -0.0034(18) 0.0047(17) -0.0017(16) C5 0.020(2) 0.019(2) 0.0169(19) 0.0056(17) -0.0009(17) -0.0005(17) C8 0.022(2) 0.0153(19) 0.0186(19) -0.0036(17) -0.0009(17) 0.0021(17) C11 0.012(2) 0.023(2) 0.025(2) 0.0060(18) -0.0015(17) 0.0032(17) C1 0.014(2) 0.022(2) 0.034(2) -0.0005(19) 0.0037(18) -0.0013(17) C2 0.015(2) 0.031(2) 0.043(3) 0.016(2) 0.0010(19) -0.0027(18) C10 0.044(3) 0.047(3) 0.023(2) 0.008(2) -0.002(2) -0.010(2) C3 0.022(3) 0.025(4) 0.024(3) -0.018(3) 0.002(2) 0.0021(17) C9 0.042(3) 0.033(3) 0.025(2) 0.015(2) -0.002(2) -0.012(2) C4 0.022(3) 0.025(4) 0.024(3) -0.018(3) 0.002(2) 0.0021(17) O14 0.038(2) 0.0273(19) 0.093(3) -0.0017(18) 0.038(2) -0.0002(15) S3 0.0229(15) 0.0109(12) 0.0152(10) 0.0011(9) 0.0030(10) 0.0051(10) O4 0.040(5) 0.020(3) 0.014(3) 0.002(2) -0.005(4) -0.005(5) O5 0.024(3) 0.027(3) 0.030(3) 0.008(2) 0.004(2) 0.013(2) O6 0.033(3) 0.021(3) 0.048(3) 0.001(2) 0.011(2) -0.005(2) S3A 0.027(3) 0.020(3) 0.0168(18) -0.0032(17) 0.0017(19) 0.0097(19) O4A 0.037(10) 0.038(10) 0.027(7) -0.016(6) -0.016(7) 0.017(8) O5A 0.040(7) 0.022(5) 0.048(6) 0.005(5) -0.002(5) 0.011(5) O6A 0.029(5) 0.038(5) 0.045(5) -0.004(4) 0.021(4) 0.007(4) C3A 0.022(3) 0.025(4) 0.024(3) -0.018(3) 0.002(2) 0.0021(17) C4A 0.022(3) 0.025(4) 0.024(3) -0.018(3) 0.002(2) 0.0021(17) Cu4A 0.0773(10) 0.0224(4) 0.0316(8) 0.0039(4) 0.0248(7) 0.0058(4) 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' 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' 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 Cu7 Cu12 Cu1 59.415(17) 3_667 1_556 ? Cu7 Cu12 Cu11 128.41(2) 3_667 3_657 ? Cu7 Cu12 Cu4 93.45(4) 3_667 4_666 ? Cu1 Cu12 Cu11 92.81(2) 1_556 3_657 ? Cu4 Cu12 Cu1 127.51(4) 4_666 1_556 ? Cu4 Cu12 Cu11 68.89(3) 4_666 3_657 ? S11 Cu12 Cu7 108.57(3) 3_657 3_667 ? S11 Cu12 Cu1 51.46(3) 3_657 1_556 ? S11 Cu12 Cu11 48.15(3) 3_657 3_657 ? S11 Cu12 Cu4 113.72(4) 3_657 4_666 ? S11 Cu12 S4 143.81(4) 3_657 4_666 ? S11 Cu12 Cu4A 113.80(11) 3_657 4_666 ? S4 Cu12 Cu7 51.85(3) 4_666 3_667 ? S4 Cu12 Cu1 108.98(3) 4_666 1_556 ? S4 Cu12 Cu11 115.37(3) 4_666 3_657 ? S4 Cu12 Cu4 49.27(4) 4_666 4_666 ? S4 Cu12 Cu4A 57.20(16) 4_666 4_666 ? O18 Cu12 Cu7 127.33(8) . 3_667 ? O18 Cu12 Cu1 125.34(9) . 1_556 ? O18 Cu12 Cu11 104.25(8) . 3_657 ? O18 Cu12 Cu4 107.01(10) . 4_666 ? O18 Cu12 S11 106.38(9) . 3_657 ? O18 Cu12 S4 109.30(9) . 4_666 ? O18 Cu12 Cu4A 95.4(2) . 4_666 ? Cu2 Cu3 Cu10 58.695(17) 3_556 2_646 ? Cu5 Cu3 Cu2 87.29(2) 2_546 3_556 ? Cu5 Cu3 Cu10 116.30(2) 2_546 2_646 ? Cu9 Cu3 Cu2 115.26(2) 2_646 3_556 ? Cu9 Cu3 Cu5 58.528(18) 2_646 2_546 ? Cu9 Cu3 Cu10 87.64(2) 2_646 2_646 ? S2 Cu3 Cu2 48.64(3) 3_556 3_556 ? S2 Cu3 Cu5 50.40(3) 3_556 2_546 ? S2 Cu3 Cu9 105.78(3) 3_556 2_646 ? S2 Cu3 Cu10 104.85(3) 3_556 2_646 ? S2 Cu3 S8 135.15(4) 3_556 2_646 ? S8 Cu3 Cu2 102.52(3) 2_646 3_556 ? S8 Cu3 Cu5 104.73(3) 2_646 2_546 ? S8 Cu3 Cu9 49.95(3) 2_646 2_646 ? S8 Cu3 Cu10 47.37(3) 2_646 2_646 ? O5 Cu3 Cu2 130.51(15) . 3_556 ? O5 Cu3 Cu5 128.76(15) . 2_546 ? O5 Cu3 Cu9 112.82(15) . 2_646 ? O5 Cu3 Cu10 113.32(15) . 2_646 ? O5 Cu3 S2 125.62(17) . 3_556 ? O5 Cu3 S8 99.19(17) . 2_646 ? Cu3 Cu2 Cu7 115.96(2) 3_556 3_566 ? Cu3 Cu2 Cu6 91.21(2) 3_556 3_566 ? Cu7 Cu2 Cu6 58.117(17) 3_566 3_566 ? Cu10 Cu2 Cu3 61.342(18) 4_465 3_556 ? Cu10 Cu2 Cu7 90.18(2) 4_465 3_566 ? Cu10 Cu2 Cu6 124.66(2) 4_465 3_566 ? S2 Cu2 Cu3 49.32(3) . 3_556 ? S2 Cu2 Cu7 102.69(3) . 3_566 ? S2 Cu2 Cu6 49.86(3) . 3_566 ? S2 Cu2 Cu10 108.04(3) . 4_465 ? S2 Cu2 S9 134.75(4) . 4_465 ? S9 Cu2 Cu3 105.43(3) 4_465 3_556 ? S9 Cu2 Cu7 49.53(3) 4_465 3_566 ? S9 Cu2 Cu6 105.85(3) 4_465 3_566 ? S9 Cu2 Cu10 49.26(3) 4_465 4_465 ? O4 Cu2 Cu3 122.2(3) . 3_556 ? O4 Cu2 Cu7 121.8(3) . 3_566 ? O4 Cu2 Cu6 117.6(2) . 3_566 ? O4 Cu2 Cu10 117.7(2) . 4_465 ? O4 Cu2 S2 113.4(3) . . ? O4 Cu2 S9 111.9(3) . 4_465 ? O4A Cu2 S2 124.2(5) . . ? Cu12 Cu7 Cu2 120.83(2) 3_667 3_566 ? Cu12 Cu7 Cu6 93.15(2) 3_667 . ? Cu6 Cu7 Cu2 61.127(17) . 3_566 ? Cu1 Cu7 Cu12 61.143(18) 3_666 3_667 ? Cu1 Cu7 Cu2 92.01(2) 3_666 3_566 ? Cu1 Cu7 Cu6 127.38(2) 3_666 . ? S4 Cu7 Cu12 50.90(3) 2_556 3_667 ? S4 Cu7 Cu2 106.90(3) 2_556 3_566 ? S4 Cu7 Cu6 50.10(3) 2_556 . ? S4 Cu7 Cu1 109.73(3) 2_556 3_666 ? S9 Cu7 Cu12 107.81(3) 2_656 3_667 ? S9 Cu7 Cu2 49.03(3) 2_656 3_566 ? S9 Cu7 Cu6 108.30(3) 2_656 . ? S9 Cu7 Cu1 50.97(3) 2_656 3_666 ? S9 Cu7 S4 139.06(4) 2_656 2_556 ? O11 Cu7 Cu12 74.39(10) . 3_667 ? O11 Cu7 Cu2 160.62(10) . 3_566 ? O11 Cu7 Cu6 134.15(9) . . ? O11 Cu7 Cu1 85.30(9) . 3_666 ? O11 Cu7 S4 92.02(10) . 2_556 ? O11 Cu7 S9 117.54(9) . 2_656 ? O9 Cu7 Cu12 160.72(9) . 3_667 ? O9 Cu7 Cu2 73.70(9) . 3_566 ? O9 Cu7 Cu6 83.00(8) . . ? O9 Cu7 Cu1 135.04(9) . 3_666 ? O9 Cu7 S4 115.19(9) . 2_556 ? O9 Cu7 S9 91.29(9) . 2_656 ? O9 Cu7 O11 94.74(14) . . ? Cu7 Cu6 Cu2 60.758(18) . 3_566 ? Cu5 Cu6 Cu2 86.46(2) 2_556 3_566 ? Cu5 Cu6 Cu7 108.78(2) 2_556 . ? S4 Cu6 Cu2 107.44(3) 2_556 3_566 ? S4 Cu6 Cu7 51.07(3) 2_556 . ? S4 Cu6 Cu5 93.35(3) 2_556 2_556 ? S4 Cu6 S2 129.65(4) 2_556 3_566 ? S4 Cu6 O20 105.10(8) 2_556 1_465 ? S2 Cu6 Cu2 47.76(3) 3_566 3_566 ? S2 Cu6 Cu7 103.24(3) 3_566 . ? S2 Cu6 Cu5 50.14(3) 3_566 2_556 ? O20 Cu6 Cu2 147.46(7) 1_465 3_566 ? O20 Cu6 Cu7 148.29(8) 1_465 . ? O20 Cu6 Cu5 91.31(7) 1_465 2_556 ? O20 Cu6 S2 108.46(8) 1_465 3_566 ? O10 Cu6 Cu2 80.44(8) . 3_566 ? O10 Cu6 Cu7 85.24(8) . . ? O10 Cu6 Cu5 152.97(8) . 2_556 ? O10 Cu6 S4 113.07(8) . 2_556 ? O10 Cu6 S2 105.00(8) . 3_566 ? O10 Cu6 O20 87.32(11) . 1_465 ? Cu7 Cu1 Cu12 59.443(17) 3_666 1_554 ? Cu8 Cu1 Cu12 91.60(2) 4_565 1_554 ? Cu8 Cu1 Cu7 122.03(2) 4_565 3_666 ? S11 Cu1 Cu12 49.64(3) 3_656 1_554 ? S11 Cu1 Cu7 106.85(3) 3_656 3_666 ? S11 Cu1 Cu8 52.07(3) 3_656 4_565 ? S9 Cu1 Cu12 106.87(3) 4_565 1_554 ? S9 Cu1 Cu7 51.68(3) 4_565 3_666 ? S9 Cu1 Cu8 104.34(3) 4_565 4_565 ? S9 Cu1 S11 137.82(4) 4_565 3_656 ? O12 Cu1 Cu12 78.95(8) 3_666 1_554 ? O12 Cu1 Cu7 84.02(8) 3_666 3_666 ? O12 Cu1 Cu8 142.67(8) 3_666 4_565 ? O12 Cu1 S11 97.41(8) 3_666 3_656 ? O12 Cu1 S9 112.98(8) 3_666 4_565 ? O1 Cu1 Cu12 150.51(9) . 1_554 ? O1 Cu1 Cu7 142.88(8) . 3_666 ? O1 Cu1 Cu8 86.79(8) . 4_565 ? O1 Cu1 S11 109.59(8) . 3_656 ? O1 Cu1 S9 102.04(9) . 4_565 ? O1 Cu1 O12 84.59(11) . 3_666 ? Cu3 Cu5 Cu6 94.32(2) 2_556 2_546 ? Cu9 Cu5 Cu3 60.033(18) 1_455 2_556 ? Cu9 Cu5 Cu6 125.17(2) 1_455 2_546 ? Cu4 Cu5 Cu3 133.16(3) . 2_556 ? Cu4 Cu5 Cu6 68.58(3) . 2_546 ? Cu4 Cu5 Cu9 93.76(4) . 1_455 ? S2 Cu5 Cu3 50.10(3) 4_566 2_556 ? S2 Cu5 Cu6 51.36(3) 4_566 2_546 ? S2 Cu5 Cu9 106.93(3) 4_566 1_455 ? S2 Cu5 Cu4 117.82(4) 4_566 . ? S2 Cu5 S5 144.55(4) 4_566 . ? S2 Cu5 O19 107.01(8) 4_566 2_656 ? S5 Cu5 Cu3 109.23(3) . 2_556 ? S5 Cu5 Cu6 114.64(3) . 2_546 ? S5 Cu5 Cu9 50.24(3) . 1_455 ? S5 Cu5 Cu4 50.60(4) . . ? O19 Cu5 Cu3 152.36(9) 2_656 2_556 ? O19 Cu5 Cu6 75.97(8) 2_656 2_546 ? O19 Cu5 Cu9 145.94(8) 2_656 1_455 ? O19 Cu5 Cu4 67.73(10) 2_656 . ? O19 Cu5 S5 98.28(9) 2_656 . ? O8 Cu5 Cu3 84.97(9) . 2_556 ? O8 Cu5 Cu6 150.09(10) . 2_546 ? O8 Cu5 Cu9 80.10(10) . 1_455 ? O8 Cu5 Cu4 131.25(8) . . ? O8 Cu5 S2 110.11(8) . 4_566 ? O8 Cu5 S5 93.56(9) . . ? O8 Cu5 O19 90.92(13) . 2_656 ? Cu12 Cu11 Cu4A 51.56(10) 3_657 2_546 ? Cu9 Cu11 Cu12 103.31(2) 2_646 3_657 ? Cu9 Cu11 Cu4A 91.65(17) 2_646 2_546 ? S11 Cu11 Cu12 48.69(3) . 3_657 ? S11 Cu11 Cu9 98.40(3) . 2_646 ? S11 Cu11 S5 124.27(4) . 2_546 ? S11 Cu11 Cu4A 99.82(10) . 2_546 ? S5 Cu11 Cu12 91.16(3) 2_546 3_657 ? S5 Cu11 Cu9 48.55(3) 2_546 2_646 ? S5 Cu11 Cu4A 50.39(15) 2_546 2_546 ? O16 Cu11 Cu12 140.40(10) . 3_657 ? O16 Cu11 Cu9 113.58(10) . 2_646 ? O16 Cu11 S11 133.41(10) . . ? O16 Cu11 S5 102.32(10) . 2_546 ? O16 Cu11 Cu4A 111.61(15) . 2_546 ? Cu1 Cu8 Cu9 113.00(2) 4_566 . ? Cu1 Cu8 Cu10 64.990(19) 4_566 . ? Cu10 Cu8 Cu9 86.19(2) . . ? S11 Cu8 Cu1 53.13(3) 2_656 4_566 ? S11 Cu8 Cu9 96.60(3) 2_656 . ? S11 Cu8 Cu10 113.63(3) 2_656 . ? S11 Cu8 S8 133.04(4) 2_656 . ? S8 Cu8 Cu1 107.03(3) . 4_566 ? S8 Cu8 Cu9 47.91(3) . . ? S8 Cu8 Cu10 47.66(3) . . ? O2 Cu8 Cu1 84.60(8) 4_566 4_566 ? O2 Cu8 Cu9 156.01(8) 4_566 . ? O2 Cu8 Cu10 87.03(8) 4_566 . ? O2 Cu8 S11 107.19(8) 4_566 2_656 ? O2 Cu8 S8 112.85(9) 4_566 . ? O13 Cu8 Cu1 161.28(8) . 4_566 ? O13 Cu8 Cu9 76.74(10) . . ? O13 Cu8 Cu10 133.20(8) . . ? O13 Cu8 S11 111.43(8) . 2_656 ? O13 Cu8 S8 91.39(9) . . ? O13 Cu8 O2 91.44(12) . 4_566 ? Cu3 Cu9 Cu11 135.57(3) 2_656 2_656 ? Cu3 Cu9 Cu8 94.33(2) 2_656 . ? Cu5 Cu9 Cu3 61.438(18) 1_655 2_656 ? Cu5 Cu9 Cu11 96.42(2) 1_655 2_656 ? Cu5 Cu9 Cu8 122.95(3) 1_655 . ? Cu11 Cu9 Cu8 64.504(19) 2_656 . ? S5 Cu9 Cu3 114.11(3) 1_655 2_656 ? S5 Cu9 Cu5 53.82(3) 1_655 1_655 ? S5 Cu9 Cu11 49.95(3) 1_655 2_656 ? S5 Cu9 Cu8 109.79(3) 1_655 . ? S8 Cu9 Cu3 51.20(3) . 2_656 ? S8 Cu9 Cu5 108.62(3) . 1_655 ? S8 Cu9 Cu11 114.55(3) . 2_656 ? S8 Cu9 Cu8 50.92(3) . . ? S8 Cu9 S5 145.67(5) . 1_655 ? O14 Cu9 Cu3 111.60(11) . 2_656 ? O14 Cu9 Cu5 117.89(9) . 1_655 ? O14 Cu9 Cu11 112.82(11) . 2_656 ? O14 Cu9 Cu8 119.05(9) . . ? O14 Cu9 S5 107.74(10) . 1_655 ? O14 Cu9 S8 106.59(10) . . ? Cu2 Cu10 Cu3 59.964(18) 4_666 2_656 ? Cu2 Cu10 Cu8 119.99(2) 4_666 . ? Cu8 Cu10 Cu3 91.73(2) . 2_656 ? S9 Cu10 Cu3 105.21(3) . 2_656 ? S9 Cu10 Cu2 50.43(3) . 4_666 ? S9 Cu10 Cu8 100.09(3) . . ? S8 Cu10 Cu3 48.93(3) . 2_656 ? S8 Cu10 Cu2 105.17(3) . 4_666 ? S8 Cu10 Cu8 51.10(3) . . ? S8 Cu10 S9 131.00(4) . . ? O15 Cu10 Cu3 115.75(15) . 2_656 ? O15 Cu10 Cu2 109.78(17) . 4_666 ? O15 Cu10 Cu8 130.20(17) . . ? O15 Cu10 S9 110.32(13) . . ? O15 Cu10 S8 118.41(13) . . ? Cu5 Cu4 Cu12 109.46(4) . 4_465 ? S4 Cu4 Cu12 50.53(4) . 4_465 ? S4 Cu4 Cu5 98.05(7) . . ? S5 Cu4 Cu12 94.61(5) . 4_465 ? S5 Cu4 Cu5 54.81(5) . . ? S5 Cu4 S4 128.90(6) . . ? O7 Cu4 Cu12 115.29(16) . 4_465 ? O7 Cu4 Cu5 135.24(15) . . ? O7 Cu4 S4 110.69(13) . . ? O7 Cu4 S5 118.61(13) . . ? Cu12 S11 Cu1 78.90(3) 3_657 3_656 ? Cu12 S11 Cu8 128.37(4) 3_657 2_646 ? Cu11 S11 Cu12 83.16(4) . 3_657 ? Cu11 S11 Cu1 138.94(5) . 3_656 ? Cu11 S11 Cu8 88.51(4) . 2_646 ? Cu8 S11 Cu1 74.80(3) 2_646 3_656 ? C11 S11 Cu12 112.10(13) . 3_657 ? C11 S11 Cu1 104.48(14) . 3_656 ? C11 S11 Cu11 116.48(14) . . ? C11 S11 Cu8 117.10(13) . 2_646 ? Cu12 S4 Cu7 77.25(4) 4_465 2_546 ? Cu12 S4 Cu4A 69.18(19) 4_465 . ? Cu7 S4 Cu4A 137.38(14) 2_546 . ? Cu6 S4 Cu12 134.11(5) 2_546 4_465 ? Cu6 S4 Cu7 78.84(3) 2_546 2_546 ? Cu6 S4 Cu4A 106.4(2) 2_546 . ? Cu4 S4 Cu12 80.21(6) . 4_465 ? Cu4 S4 Cu7 135.20(5) . 2_546 ? Cu4 S4 Cu6 90.26(7) . 2_546 ? C4 S4 Cu12 105.6(3) . 4_465 ? C4 S4 Cu7 113.2(4) . 2_546 ? C4 S4 Cu6 119.8(3) . 2_546 ? C4 S4 Cu4 109.9(3) . . ? C4A S4 Cu4A 113.9(6) . . ? Cu3 S2 Cu6 136.80(4) 3_556 3_566 ? Cu3 S2 Cu5 79.50(3) 3_556 4_565 ? Cu2 S2 Cu3 82.05(4) . 3_556 ? Cu2 S2 Cu6 82.38(4) . 3_566 ? Cu2 S2 Cu5 127.19(4) . 4_565 ? Cu5 S2 Cu6 78.50(3) 4_565 3_566 ? C2 S2 Cu3 111.95(14) . 3_556 ? C2 S2 Cu2 119.25(16) . . ? C2 S2 Cu6 110.85(14) . 3_566 ? C2 S2 Cu5 113.55(16) . 4_565 ? Cu2 S9 Cu7 81.45(4) 4_666 2_646 ? Cu1 S9 Cu2 134.79(5) 4_566 4_666 ? Cu1 S9 Cu7 77.35(3) 4_566 2_646 ? Cu10 S9 Cu2 80.30(4) . 4_666 ? Cu10 S9 Cu7 134.16(5) . 2_646 ? Cu10 S9 Cu1 86.59(4) . 4_566 ? C9 S9 Cu2 106.77(15) . 4_666 ? C9 S9 Cu7 113.34(17) . 2_646 ? C9 S9 Cu1 118.23(16) . 4_566 ? C9 S9 Cu10 112.11(17) . . ? O10 S6 C6 106.46(18) . . ? O9 S6 O10 112.59(18) . . ? O9 S6 C6 104.13(19) . . ? O8 S6 O10 110.87(19) . . ? O8 S6 O9 112.7(2) . . ? O8 S6 C6 109.69(17) . . ? O12 S7 C7 106.62(19) . . ? O11 S7 O12 112.08(18) . . ? O11 S7 C7 104.88(19) . . ? O13 S7 O12 111.55(19) . . ? O13 S7 O11 112.5(2) . . ? O13 S7 C7 108.80(18) . . ? O20 S12 O19 111.80(18) . . ? O20 S12 C12 107.41(18) . . ? O21 S12 O20 113.0(2) . . ? O21 S12 O19 111.6(2) . . ? O21 S12 C12 106.69(19) . . ? O19 S12 C12 105.8(2) . . ? Cu5 S5 Cu4A 90.3(2) . . ? Cu11 S5 Cu5 136.70(5) 2_556 . ? Cu11 S5 Cu4A 82.5(2) 2_556 . ? Cu9 S5 Cu5 75.94(4) 1_455 . ? Cu9 S5 Cu11 81.51(4) 1_455 2_556 ? Cu9 S5 Cu4A 138.28(13) 1_455 . ? Cu4 S5 Cu5 74.59(7) . . ? Cu4 S5 Cu11 95.64(7) . 2_556 ? Cu4 S5 Cu9 132.66(6) . 1_455 ? C5 S5 Cu5 110.13(13) . . ? C5 S5 Cu11 111.74(13) . 2_556 ? C5 S5 Cu9 107.53(14) . 1_455 ? C5 S5 Cu4 117.03(14) . . ? C5 S5 Cu4A 114.18(18) . . ? O18 S10 O16 112.04(19) . . ? O18 S10 C10 105.1(2) . . ? O16 S10 C10 103.9(2) . . ? O17 S10 O18 113.1(2) . . ? O17 S10 O16 112.1(2) . . ? O17 S10 C10 109.9(3) . . ? O2 S1 C1 107.75(18) . . ? O3 S1 O2 111.5(2) . . ? O3 S1 O1 113.6(2) . . ? O3 S1 C1 107.5(2) . . ? O1 S1 O2 111.98(18) . . ? O1 S1 C1 103.99(19) . . ? Cu3 S8 Cu8 136.43(5) 2_656 . ? Cu9 S8 Cu3 78.85(4) . 2_656 ? Cu9 S8 Cu8 81.17(4) . . ? Cu10 S8 Cu3 83.70(4) . 2_656 ? Cu10 S8 Cu8 81.25(4) . . ? Cu10 S8 Cu9 131.47(5) . . ? C8 S8 Cu3 112.81(13) . 2_656 ? C8 S8 Cu8 110.21(13) . . ? C8 S8 Cu9 109.02(14) . . ? C8 S8 Cu10 119.49(14) . . ? S10 O18 Cu12 125.85(18) . . ? S12 O20 Cu6 119.02(16) . 1_645 ? S1 O2 Cu8 125.49(17) . 4_565 ? S7 O12 Cu1 125.45(17) . 3_666 ? S6 O10 Cu6 123.85(17) . . ? S7 O11 Cu7 125.58(19) . . ? S10 O16 Cu11 130.8(2) . . ? S6 O9 Cu7 126.26(18) . . ? S7 O13 Cu8 127.65(17) . . ? S1 O1 Cu1 125.40(18) . . ? S12 O19 Cu5 137.81(19) . 2_646 ? S6 O8 Cu5 128.48(17) . . ? Cu4 O7 H7A 115.7 . . ? Cu4 O7 H7B 115.1 . . ? H7A O7 H7B 103.2 . . ? Cu4A O7 H7A 121.3 . . ? Cu4A O7 H7B 96.8 . . ? Cu10 O15 H15A 111.8 . . ? Cu10 O15 H15B 113.9 . . ? H15A O15 H15B 106.7 . . ? S6 C6 H6A 108.3 . . ? S6 C6 H6B 108.3 . . ? H6A C6 H6B 107.4 . . ? C5 C6 S6 116.0(3) . . ? C5 C6 H6A 108.3 . . ? C5 C6 H6B 108.3 . . ? S7 C7 H7C 108.4 . . ? S7 C7 H7D 108.4 . . ? H7C C7 H7D 107.5 . . ? C8 C7 S7 115.5(3) . . ? C8 C7 H7C 108.4 . . ? C8 C7 H7D 108.4 . . ? S12 C12 H12A 109.3 . . ? S12 C12 H12B 109.3 . . ? H12A C12 H12B 107.9 . . ? C11 C12 S12 111.8(3) . . ? C11 C12 H12A 109.3 . . ? C11 C12 H12B 109.3 . . ? S5 C5 H5A 108.8 . . ? S5 C5 H5B 108.8 . . ? C6 C5 S5 114.0(3) . . ? C6 C5 H5A 108.8 . . ? C6 C5 H5B 108.8 . . ? H5A C5 H5B 107.6 . . ? S8 C8 H8A 108.9 . . ? S8 C8 H8B 108.9 . . ? C7 C8 S8 113.3(3) . . ? C7 C8 H8A 108.9 . . ? C7 C8 H8B 108.9 . . ? H8A C8 H8B 107.7 . . ? S11 C11 H11A 109.4 . . ? S11 C11 H11B 109.4 . . ? C12 C11 S11 111.1(3) . . ? C12 C11 H11A 109.4 . . ? C12 C11 H11B 109.4 . . ? H11A C11 H11B 108.0 . . ? S1 C1 H1A 108.6 . . ? S1 C1 H1B 108.6 . . ? H1A C1 H1B 107.6 . . ? C2 C1 S1 114.7(3) . . ? C2 C1 H1A 108.6 . . ? C2 C1 H1B 108.6 . . ? S2 C2 H2A 109.5 . . ? S2 C2 H2B 109.5 . . ? C1 C2 S2 110.7(3) . . ? C1 C2 H2A 109.5 . . ? C1 C2 H2B 109.5 . . ? H2A C2 H2B 108.1 . . ? S10 C10 H10A 109.3 . . ? S10 C10 H10B 109.3 . . ? H10A C10 H10B 108.0 . . ? C9 C10 S10 111.4(3) . . ? C9 C10 H10A 109.3 . . ? C9 C10 H10B 109.3 . . ? H3A C3 H3B 108.1 . . ? C4 C3 H3A 109.5 . . ? C4 C3 H3B 109.5 . . ? C4 C3 S3 110.7(6) . . ? S3 C3 H3A 109.5 . . ? S3 C3 H3B 109.5 . . ? S9 C9 H9A 108.4 . . ? S9 C9 H9B 108.4 . . ? C10 C9 S9 115.7(3) . . ? C10 C9 H9A 108.4 . . ? C10 C9 H9B 108.4 . . ? H9A C9 H9B 107.4 . . ? S4 C4 H4A 108.9 . . ? S4 C4 H4B 108.9 . . ? C3 C4 S4 113.4(5) . . ? C3 C4 H4A 108.9 . . ? C3 C4 H4B 108.9 . . ? H4A C4 H4B 107.7 . . ? Cu9 O14 H14A 110.6 . . ? Cu9 O14 H14B 110.9 . . ? H14A O14 H14B 108.1 . . ? O4 S3 C3 106.1(7) . . ? O4 S3 O5 110.9(5) . . ? O5 S3 C3 106.3(5) . . ? O6 S3 C3 106.9(4) . . ? O6 S3 O4 112.5(5) . . ? O6 S3 O5 113.5(4) . . ? S3 O4 Cu2 119.8(6) . . ? S3 O5 Cu3 129.3(4) . . ? O4A S3A C3A 106.2(12) . . ? O5A S3A O4A 111.7(11) . . ? O5A S3A C3A 106.2(9) . . ? O6A S3A O4A 112.2(9) . . ? O6A S3A O5A 112.2(7) . . ? O6A S3A C3A 107.9(6) . . ? S3A O4A Cu2 139.3(13) . . ? S3A O5A Cu3 135.3(8) . . ? S3A C3A H3AA 108.9 . . ? S3A C3A H3AB 108.9 . . ? H3AA C3A H3AB 107.7 . . ? C4A C3A S3A 113.3(9) . . ? C4A C3A H3AA 108.9 . . ? C4A C3A H3AB 108.9 . . ? S4 C4A H4AA 109.3 . . ? S4 C4A H4AB 109.3 . . ? C3A C4A S4 111.8(13) . . ? C3A C4A H4AA 109.3 . . ? C3A C4A H4AB 109.3 . . ? H4AA C4A H4AB 107.9 . . ? Cu12 Cu4A Cu11 62.26(13) 4_465 2_556 ? S4 Cu4A Cu12 53.62(11) . 4_465 ? S4 Cu4A Cu11 108.88(18) . 2_556 ? S4 Cu4A S5 114.5(3) . . ? S5 Cu4A Cu12 97.52(18) . 4_465 ? S5 Cu4A Cu11 47.10(10) . 2_556 ? O7 Cu4A Cu12 140.2(4) . 4_465 ? O7 Cu4A Cu11 135.7(3) . 2_556 ? O7 Cu4A S4 113.5(3) . . ? O7 Cu4A S5 120.1(3) . . ? 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 Cu12 Cu7 2.8306(7) 3_667 ? Cu12 Cu1 2.8789(7) 1_556 ? Cu12 Cu11 2.9548(7) 3_657 ? Cu12 Cu4 2.8751(16) 4_666 ? Cu12 S11 2.2354(11) 3_657 ? Cu12 S4 2.2521(10) 4_666 ? Cu12 O18 2.122(3) . ? Cu12 Cu4A 2.615(6) 4_666 ? Cu3 Cu2 2.9259(7) 3_556 ? Cu3 Cu5 2.8714(8) 2_546 ? Cu3 Cu9 2.8322(7) 2_646 ? Cu3 Cu10 2.9657(8) 2_646 ? Cu3 S2 2.2404(10) 3_556 ? Cu3 S8 2.2497(11) 2_646 ? Cu3 O5 2.029(5) . ? Cu3 O5A 2.089(9) . ? Cu2 Cu7 2.9579(7) 3_566 ? Cu2 Cu6 2.9686(8) 3_566 ? Cu2 Cu10 2.8877(8) 4_465 ? Cu2 S2 2.2173(10) . ? Cu2 S9 2.2584(11) 4_465 ? Cu2 O4 2.106(10) . ? Cu2 O4A 1.960(18) . ? Cu7 Cu6 2.8784(7) . ? Cu7 Cu1 2.8298(7) 3_666 ? Cu7 S4 2.2823(11) 2_556 ? Cu7 S9 2.2755(11) 2_656 ? Cu7 O11 2.180(3) . ? Cu7 O9 2.159(3) . ? Cu6 Cu5 2.8726(7) 2_556 ? Cu6 S4 2.2507(10) 2_556 ? Cu6 S2 2.2896(10) 3_566 ? Cu6 O20 2.274(3) 1_465 ? Cu6 O10 2.198(3) . ? Cu1 Cu8 2.7682(7) 4_565 ? Cu1 S11 2.2947(10) 3_656 ? Cu1 S9 2.2531(10) 4_565 ? Cu1 O12 2.248(3) 3_666 ? Cu1 O1 2.210(3) . ? Cu5 Cu9 2.7883(8) 1_455 ? Cu5 Cu4 2.737(2) . ? Cu5 S2 2.2502(10) 4_566 ? Cu5 S5 2.3200(11) . ? Cu5 O19 2.278(3) 2_656 ? Cu5 O8 2.124(3) . ? Cu11 Cu9 2.9160(8) 2_646 ? Cu11 S11 2.2169(10) . ? Cu11 S5 2.2567(11) 2_546 ? Cu11 O16 2.022(3) . ? Cu11 Cu4A 3.054(6) 2_546 ? Cu8 Cu9 2.9422(8) . ? Cu8 Cu10 2.9354(8) . ? Cu8 S11 2.2627(10) 2_656 ? Cu8 S8 2.3112(11) . ? Cu8 O2 2.246(3) 4_566 ? Cu8 O13 2.141(3) . ? Cu9 S5 2.2098(11) 1_655 ? Cu9 S8 2.2096(11) . ? Cu9 O14 2.077(4) . ? Cu10 S9 2.2198(11) . ? Cu10 S8 2.1952(11) . ? Cu10 O15 2.011(4) . ? Cu4 S4 2.2108(13) . ? Cu4 S5 2.1939(13) . ? Cu4 O7 2.034(4) . ? S11 C11 1.843(4) . ? S4 C4 1.840(7) . ? S4 C4A 1.858(13) . ? S4 Cu4A 2.351(5) . ? S2 C2 1.844(4) . ? S9 C9 1.837(4) . ? S6 O10 1.479(3) . ? S6 O9 1.460(3) . ? S6 O8 1.452(3) . ? S6 C6 1.778(4) . ? S7 O12 1.473(3) . ? S7 O11 1.455(3) . ? S7 O13 1.454(3) . ? S7 C7 1.780(4) . ? S12 O20 1.457(3) . ? S12 O21 1.456(3) . ? S12 O19 1.471(3) . ? S12 C12 1.778(4) . ? S5 C5 1.833(4) . ? S5 Cu4A 2.373(6) . ? S10 O18 1.454(3) . ? S10 O16 1.464(3) . ? S10 O17 1.423(4) . ? S10 C10 1.793(5) . ? S1 O2 1.472(3) . ? S1 O3 1.455(3) . ? S1 O1 1.464(3) . ? S1 C1 1.777(4) . ? S8 C8 1.838(4) . ? O7 H7A 0.9428 . ? O7 H7B 0.9413 . ? O7 Cu4A 1.812(6) . ? O15 H15A 0.9042 . ? O15 H15B 0.9120 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 C5 1.527(6) . ? C7 H7C 0.9700 . ? C7 H7D 0.9700 . ? C7 C8 1.525(6) . ? C12 H12A 0.9700 . ? C12 H12B 0.9700 . ? C12 C11 1.517(5) . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C8 H8A 0.9700 . ? C8 H8B 0.9700 . ? C11 H11A 0.9700 . ? C11 H11B 0.9700 . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 C2 1.518(6) . ? C2 H2A 0.9700 . ? C2 H2B 0.9700 . ? C10 H10A 0.9700 . ? C10 H10B 0.9700 . ? C10 C9 1.467(6) . ? C3 H3A 0.9700 . ? C3 H3B 0.9700 . ? C3 C4 1.500(11) . ? C3 S3 1.773(8) . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? O14 H14A 0.8710 . ? O14 H14B 0.8716 . ? S3 O4 1.466(9) . ? S3 O5 1.468(6) . ? S3 O6 1.444(6) . ? S3A O4A 1.462(14) . ? S3A O5A 1.453(10) . ? S3A O6A 1.448(9) . ? S3A C3A 1.795(15) . ? C3A H3AA 0.9700 . ? C3A H3AB 0.9700 . ? C3A C4A 1.520(16) . ? C4A H4AA 0.9700 . ? C4A H4AB 0.9700 . ? 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 O7 H7A O21 0.94 2.02 2.850(5) 146.4 4_465 yes O7 H7A O19 0.94 2.74 3.355(5) 123.6 4_465 yes O7 H7B O17 0.94 2.04 2.826(6) 139.6 4_465 yes O15 H15A O3 0.90 2.36 3.124(7) 142.6 4_566 yes O15 H15B O2 0.91 2.82 3.451(5) 127.1 2_656 yes O15 H15B O3 0.91 1.96 2.807(6) 153.9 2_656 yes C6 H6A O4 0.97 2.37 3.278(11) 155.0 3_566 yes C6 H6B O19 0.97 2.43 3.234(5) 140.2 2_656 yes C7 H7C O18 0.97 2.51 3.418(5) 155.8 3_667 yes C7 H7D O15 0.97 2.65 3.443(6) 138.7 3_667 yes C12 H12A O17 0.97 2.45 3.320(5) 149.1 . yes C12 H12B O2 0.97 2.41 3.359(5) 166.2 3_656 yes C5 H5A O21 0.97 2.50 3.306(5) 140.3 4_465 yes C5 H5B O14 0.97 2.72 3.406(5) 127.7 1_455 yes C8 H8A O3 0.97 2.42 3.252(5) 143.1 2_656 yes C8 H8B O14 0.97 2.74 3.416(5) 126.9 . yes C11 H11B O12 0.97 2.65 3.388(5) 132.8 1_545 yes C1 H1B O20 0.97 2.28 3.243(5) 171.1 3_656 yes C10 H10A O13 0.97 2.44 3.404(6) 171.7 2_646 yes C10 H10B O1 0.97 2.56 3.319(6) 135.7 4_566 yes C3 H3A O8 0.97 2.45 3.396(13) 164.2 2_546 yes C3 H3B O20 0.97 2.78 3.474(8) 128.9 2_656 yes C9 H9A O9 0.97 2.68 3.325(6) 124.8 2_646 yes C4 H4A O11 0.97 2.63 3.316(12) 127.8 2_546 yes O14 H14A O10 0.87 2.02 2.857(4) 159.9 1_655 yes O14 H14A O8 0.87 2.87 3.424(5) 123.1 1_655 yes 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 Cu12 S11 C11 C12 -175.0(2) 3_657 . . . ? Cu12 S4 C4 C3 -175.0(9) 4_465 . . . ? Cu12 S4 C4A C3A 152.1(15) 4_465 . . . ? Cu3 S2 C2 C1 -167.7(3) 3_556 . . . ? Cu3 S8 C8 C7 -178.2(2) 2_656 . . . ? Cu2 S2 C2 C1 -74.5(3) . . . . ? Cu2 S9 C9 C10 -171.3(4) 4_666 . . . ? Cu7 S4 C4 C3 -92.4(10) 2_546 . . . ? Cu7 S4 C4A C3A -126.4(17) 2_546 . . . ? Cu7 S9 C9 C10 -83.6(4) 2_646 . . . ? Cu6 S4 C4 C3 -2.3(11) 2_546 . . . ? Cu6 S4 C4A C3A -43.7(19) 2_546 . . . ? Cu6 S2 C2 C1 18.4(4) 3_566 . . . ? Cu1 S11 C11 C12 101.3(3) 3_656 . . . ? Cu1 S9 C9 C10 4.2(5) 4_566 . . . ? Cu5 S2 C2 C1 104.6(3) 4_565 . . . ? Cu5 S5 C5 C6 15.2(3) . . . . ? Cu11 S11 C11 C12 -81.6(3) . . . . ? Cu11 S5 C5 C6 -176.1(2) 2_556 . . . ? Cu8 S11 C11 C12 21.2(3) 2_646 . . . ? Cu8 S8 C8 C7 8.8(3) . . . . ? Cu9 S5 C5 C6 96.2(3) 1_455 . . . ? Cu9 S8 C8 C7 96.2(3) . . . . ? Cu10 S9 C9 C10 102.5(4) . . . . ? Cu10 S8 C8 C7 -82.4(3) . . . . ? Cu4 S4 C4 C3 100.0(9) . . . . ? Cu4 S5 C5 C6 -67.3(3) . . . . ? S6 C6 C5 S5 -70.7(4) . . . . ? S7 C7 C8 S8 -69.1(3) . . . . ? S12 C12 C11 S11 -167.1(2) . . . . ? S10 C10 C9 S9 176.8(3) . . . . ? S1 C1 C2 S2 -165.2(2) . . . . ? O18 S10 O16 Cu11 -164.1(2) . . . . ? O18 S10 C10 C9 61.5(4) . . . . ? O20 S12 O19 Cu5 0.5(4) . . . 2_646 ? O20 S12 C12 C11 67.8(3) . . . . ? O2 S1 O1 Cu1 -25.6(3) . . . . ? O2 S1 C1 C2 47.4(4) . . . . ? O12 S7 O11 Cu7 34.0(3) . . . . ? O12 S7 O13 Cu8 123.7(2) . . . . ? O12 S7 C7 C8 -55.7(3) . . . . ? O10 S6 O9 Cu7 37.8(3) . . . . ? O10 S6 O8 Cu5 123.5(2) . . . . ? O10 S6 C6 C5 -57.8(3) . . . . ? O11 S7 O12 Cu1 -25.2(3) . . . 3_666 ? O11 S7 O13 Cu8 -109.3(3) . . . . ? O11 S7 C7 C8 -174.7(3) . . . . ? O3 S1 O2 Cu8 -100.4(2) . . . 4_565 ? O3 S1 O1 Cu1 101.8(2) . . . . ? O3 S1 C1 C2 -72.8(4) . . . . ? O16 S10 O18 Cu12 98.7(3) . . . . ? O16 S10 C10 C9 179.3(4) . . . . ? O9 S6 O10 Cu6 -27.2(3) . . . . ? O9 S6 O8 Cu5 -109.3(3) . . . . ? O9 S6 C6 C5 -177.0(3) . . . . ? O13 S7 O12 Cu1 102.0(2) . . . 3_666 ? O13 S7 O11 Cu7 -92.6(3) . . . . ? O13 S7 C7 C8 64.7(3) . . . . ? O1 S1 O2 Cu8 28.2(3) . . . 4_565 ? O1 S1 C1 C2 166.4(3) . . . . ? O21 S12 O20 Cu6 -110.0(2) . . . 1_645 ? O21 S12 O19 Cu5 128.2(3) . . . 2_646 ? O21 S12 C12 C11 -53.7(3) . . . . ? O19 S12 O20 Cu6 17.0(3) . . . 1_645 ? O19 S12 C12 C11 -172.7(3) . . . . ? O8 S6 O10 Cu6 100.1(2) . . . . ? O8 S6 O9 Cu7 -88.4(3) . . . . ? O8 S6 C6 C5 62.2(3) . . . . ? O17 S10 O18 Cu12 -29.2(3) . . . . ? O17 S10 O16 Cu11 -35.6(4) . . . . ? O17 S10 C10 C9 -60.5(4) . . . . ? C6 S6 O10 Cu6 -140.7(2) . . . . ? C6 S6 O9 Cu7 152.8(2) . . . . ? C6 S6 O8 Cu5 6.2(3) . . . . ? C7 S7 O12 Cu1 -139.4(2) . . . 3_666 ? C7 S7 O11 Cu7 149.3(2) . . . . ? C7 S7 O13 Cu8 6.4(3) . . . . ? C12 S12 O20 Cu6 132.58(19) . . . 1_645 ? C12 S12 O19 Cu5 -116.2(3) . . . 2_646 ? C1 S1 O2 Cu8 142.0(2) . . . 4_565 ? C1 S1 O1 Cu1 -141.7(2) . . . . ? C10 S10 O18 Cu12 -149.1(2) . . . . ? C10 S10 O16 Cu11 83.0(3) . . . . ? C3 S3 O4 Cu2 -144.4(6) . . . . ? C3 S3 O5 Cu3 84.4(5) . . . . ? C4 C3 S3 O4 70.2(9) . . . . ? C4 C3 S3 O5 -171.7(9) . . . . ? C4 C3 S3 O6 -50.1(11) . . . . ? S3 C3 C4 S4 174.5(4) . . . . ? O4 S3 O5 Cu3 -160.7(6) . . . . ? O5 S3 O4 Cu2 100.5(6) . . . . ? O6 S3 O4 Cu2 -27.8(9) . . . . ? O6 S3 O5 Cu3 -32.8(5) . . . . ? S3A C3A C4A S4 -169.6(8) . . . . ? O4A S3A O5A Cu3 152.0(10) . . . . ? O4A S3A C3A C4A 49(2) . . . . ? O5A S3A O4A Cu2 -71(2) . . . . ? O5A S3A C3A C4A -70(2) . . . . ? O6A S3A O4A Cu2 56(2) . . . . ? O6A S3A O5A Cu3 24.9(11) . . . . ? O6A S3A C3A C4A 169.5(17) . . . . ? C3A S3A O4A Cu2 173.8(17) . . . . ? C3A S3A O5A Cu3 -92.7(11) . . . . ? Cu4A S4 C4A C3A 75.7(16) . . . . ? Cu4A S5 C5 C6 -84.7(4) . . . . ?