#------------------------------------------------------------------------------ #$Date: 2020-09-03 04:46:59 +0300 (Thu, 03 Sep 2020) $ #$Revision: 255817 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/53/7705342.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_7705342 loop_ _publ_author_name 'Jarrah, Najmeh' 'Troyano, Javier' 'Carn\'e-S\'anchez, Arnau' 'Imaz, Inhar' 'Tangestaninejad, Shahram' 'Moghadam, Majid' 'Maspoch, Daniel' _publ_section_title ; Dynamic porous coordination polymers built-up from flexible 4,4′ dithiodibenzoate and rigid N-based ligands ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D0DT02411B _journal_year 2020 _chemical_formula_moiety '0.33(C114 H78 Cu6 N6 O24 S12), 0.33(C3 H7 N O)' _chemical_formula_sum 'C39 H28.33 Cu2 N2.33 O8.33 S4' _chemical_formula_weight 918.29 _space_group_crystal_system triclinic _space_group_IT_number 2 _space_group_name_Hall '-P 1' _space_group_name_H-M_alt 'P -1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _audit_creation_date 2020-08-24 _audit_creation_method ; Olex2 1.2 (compiled 2018.05.29 svn.r3508 for OlexSys, GUI svn.r5506) ; _audit_update_record ; 2020-08-25 deposited with the CCDC. 2020-09-02 downloaded from the CCDC. ; _cell_angle_alpha 115.86(5) _cell_angle_beta 103.91(5) _cell_angle_gamma 93.65(5) _cell_formula_units_Z 3 _cell_length_a 10.390(6) _cell_length_b 21.680(6) _cell_length_c 21.910(6) _cell_measurement_reflns_used 1241 _cell_measurement_temperature 100 _cell_measurement_theta_max 30 _cell_measurement_theta_min 1 _cell_volume 4230(4) _computing_cell_refinement 'xds (Kabsch et al., 2010)' _computing_data_collection 'Mxcube (Gabadinho et al. 2010)' _computing_data_reduction 'xds (Kabsch et al., 2010)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'olex2.solve (Bourhis et al., 2015)' _diffrn_ambient_temperature 100 _diffrn_measured_fraction_theta_full 0.902 _diffrn_measured_fraction_theta_max 0.753 _diffrn_measurement_device_type 'Pilatus DECTRIS 6M' _diffrn_measurement_method 'w/ scan' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.82643 _diffrn_reflns_av_R_equivalents 0.1310 _diffrn_reflns_av_unetI/netI 0.1583 _diffrn_reflns_Laue_measured_fraction_full 0.902 _diffrn_reflns_Laue_measured_fraction_max 0.753 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_number 38580 _diffrn_reflns_point_group_measured_fraction_full 0.902 _diffrn_reflns_point_group_measured_fraction_max 0.753 _diffrn_reflns_theta_full 29.726 _diffrn_reflns_theta_max 33.813 _diffrn_reflns_theta_min 1.237 _exptl_absorpt_coefficient_mu 1.422 _exptl_absorpt_correction_type none _exptl_crystal_colour 'clear dark green' _exptl_crystal_colour_lustre clear _exptl_crystal_colour_modifier dark _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 1.081 _exptl_crystal_description block _exptl_crystal_F_000 1402 _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.21 _refine_diff_density_max 0.729 _refine_diff_density_min -1.110 _refine_diff_density_rms 0.114 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.941 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 751 _refine_ls_number_reflns 16297 _refine_ls_number_restraints 46 _refine_ls_restrained_S_all 0.941 _refine_ls_R_factor_all 0.1630 _refine_ls_R_factor_gt 0.0974 _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^)+(0.1638P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2670 _refine_ls_wR_factor_ref 0.3117 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7028 _reflns_number_total 16297 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02411b2.cif _cod_data_source_block import02 _cod_original_cell_volume 4230(3) _cod_database_code 7705342 _shelx_shelxl_version_number 2018/1 _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 0.754 _shelx_estimated_absorpt_t_min 0.727 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Restrained distances C84-C83 1.395 with sigma of 0.02 C37-C36 1.395 with sigma of 0.02 O1S-C2S 1.215 with sigma of 0.02 C36-C37 1.395 with sigma of 0.02 3. Rigid bond restraints C82, C83, C84 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C73, C74, C75 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 N71, C72, C73, C74, C75, C76 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 N81, C82, C83, C84, C85, C86 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 4. Uiso/Uaniso restraints and constraints Uanis(C74) \\sim Ueq, Uanis(C75) \\sim Ueq, Uanis(C73) \\sim Ueq: with sigma of 0.1 and sigma for terminal atoms of 0.2 5. Others Fixed Sof: O1S(0.5) N3S(0.5) C2S(0.5) H2S(0.5) C5S(0.5) H5SA(0.5) H5SB(0.5) H5SC(0.5) C6S(0.5) H6SA(0.5) H6SB(0.5) H6SC(0.5) 6.a Me refined with riding coordinates: C6S(H6SA,H6SB,H6SC) 6.b Aromatic/amide H refined with riding coordinates: C2S(H2S), C5(H5), C6(H6), C8(H8), C9(H9), C13(H13), C14(H14), C16(H16), C17(H17), C25(H25), C26(H26), C28(H28), C29(H29), C33(H33), C34(H34), C36(H36), C37(H37), C45(H45), C46(H46), C48(H48), C49(H49), C53(H53), C54(H54), C56(H56), C57(H57), C62(H62), C63(H63), C64(H64), C65(H65), C66(H66), C72(H72), C73(H73), C74(H74), C75(H75), C76(H76), C82(H82), C83(H83), C84(H84), C85(H85), C86(H86) 6.c Idealised Me refined as rotating group: C5S(H5SA,H5SB,H5SC) ; _shelx_res_file ; TITL import02.res created by SHELXL-2018/1 at 16:44:08 on 24-Aug-2020 CELL 0.82643 10.39 21.68 21.91 115.86 103.91 93.65 ZERR 3 0.006 0.006 0.006 0.05 0.05 0.05 LATT 1 SFAC C H Cu N O S DISP C 0.0052 0.0023 16.0976 DISP Cu 0.2557 1.6823 7813.756 DISP H -0 0 0.63 DISP N 0.0094 0.0046 28.7478 DISP O 0.0162 0.0086 48.7782 DISP S 0.1566 0.1676 825.3281 UNIT 117 85 6 7 25 12 DFIX 1.395 C84 C83 DFIX 1.395 C37 C36 DFIX 1.215 O1S C2S DFIX 1.395 C36 C37 DELU C82 C83 C84 DELU C73 C74 C75 DELU N71 C72 > C76 DELU N81 C82 > C86 ISOR C74 C75 C73 L.S. 20 PLAN 52 SIZE 0.24 0.21 0.23 TEMP -173.15 ABIN fmap 2 acta MERG 2 OMIT -3 -3 3 REM REM REM WGHT 0.163800 FVAR 0.77112 CU1 3 0.005460 0.314938 1.162286 11.00000 0.05598 0.06374 = 0.06668 0.03319 0.02654 0.01013 CU2 3 0.124803 0.014197 0.498829 11.00000 0.05258 0.05859 = 0.06805 0.02474 0.02796 0.00187 CU3 3 -0.771430 -0.355505 -0.160725 11.00000 0.05709 0.06082 = 0.06743 0.03090 0.02661 0.00961 S10 6 0.101907 0.427829 0.811568 11.00000 0.08928 0.05725 = 0.06277 0.02319 0.03338 0.00438 S11 6 -0.073962 0.446490 0.834051 11.00000 0.09040 0.06327 = 0.06349 0.03325 0.03140 0.02168 S30 6 -0.279810 0.089702 0.152488 11.00000 0.13487 0.07847 = 0.06638 0.03273 0.01780 -0.02271 S31 6 -0.480959 0.085507 0.129576 11.00000 0.14181 0.06145 = 0.07570 0.02910 0.01670 0.00243 S50 6 -0.832920 -0.201246 -0.472531 11.00000 0.11931 0.06661 = 0.07746 0.03384 0.04450 0.00471 S51 6 0.302422 0.746397 1.482078 11.00000 0.09207 0.07235 = 0.07820 0.02728 0.03514 -0.00940 O1 5 0.113614 0.108585 0.566740 11.00000 0.06403 0.06257 = 0.09189 0.03003 0.03911 0.00550 O1S 5 0.373100 0.400335 0.654984 10.50000 0.12088 O2 5 0.097238 -0.085343 0.431588 11.00000 0.06215 0.07301 = 0.07326 0.02220 0.03231 0.00141 O19 5 -0.007728 0.335473 1.081852 11.00000 0.06311 0.07059 = 0.05909 0.02354 0.02968 0.01185 O20 5 -0.815985 -0.389394 -0.096404 11.00000 0.06513 0.06237 = 0.06816 0.02748 0.02945 0.01698 O21 5 0.182527 -0.005407 0.578987 11.00000 0.06119 0.07629 = 0.08307 0.03421 0.03654 0.00307 O22 5 0.025892 0.029155 0.419190 11.00000 0.06149 0.09817 = 0.09216 0.04723 0.03310 -0.00181 O39 5 -0.697651 -0.262209 -0.078469 11.00000 0.06088 0.06783 = 0.06879 0.02909 0.02312 0.01504 O40 5 -0.893136 -0.221839 -0.095000 11.00000 0.06411 0.06969 = 0.07064 0.03204 0.02623 0.00995 O41 5 -0.763139 -0.312202 -0.223992 11.00000 0.06291 0.07727 = 0.07592 0.04097 0.02898 0.01041 O42 5 -0.982005 -0.300516 -0.242941 11.00000 0.05067 0.08955 = 0.08310 0.04800 0.02947 0.01170 O59 5 -0.116137 0.438356 1.245467 11.00000 0.06703 0.07831 = 0.07062 0.03437 0.03153 0.01395 O60 5 0.083776 0.413218 1.230785 11.00000 0.05137 0.07627 = 0.07145 0.02997 0.03212 0.00613 N3S 4 0.376099 0.283018 0.584547 10.50000 0.09146 N61 4 0.195825 0.280228 1.160258 11.00000 0.06459 0.06084 = 0.07242 0.02460 0.02649 0.01555 N71 4 0.319104 0.044936 0.489156 11.00000 0.06355 0.07241 = 0.11684 0.05082 0.04731 0.01288 N81 4 -0.582783 -0.394574 -0.156900 11.00000 0.06616 0.07730 = 0.10592 0.05627 0.04172 0.02350 C2S 1 0.332586 0.346355 0.595962 10.50000 0.11030 AFIX 43 H2S 2 0.270214 0.348251 0.557511 10.50000 -1.20000 AFIX 0 C3 1 0.017755 0.126174 0.588669 11.00000 0.05531 0.05827 = 0.07541 0.01751 0.02774 -0.00296 C4 1 0.029975 0.200055 0.643187 11.00000 0.05058 0.05528 = 0.07163 0.03410 0.01792 0.00738 C5 1 0.151674 0.245929 0.665138 11.00000 0.07271 0.06306 = 0.09555 0.02333 0.03762 0.00320 AFIX 43 H5 2 0.222028 0.230366 0.644852 11.00000 -1.20000 AFIX 0 C5S 1 0.317324 0.226127 0.518548 10.50000 0.08773 AFIX 137 H5SA 2 0.371240 0.189524 0.512115 10.50000 -1.50000 H5SB 2 0.313458 0.240366 0.481498 10.50000 -1.50000 H5SC 2 0.225583 0.208137 0.515218 10.50000 -1.50000 AFIX 0 C6 1 0.168711 0.314112 0.716606 11.00000 0.06884 0.05105 = 0.11245 0.02265 0.04596 -0.00402 AFIX 43 H6 2 0.252399 0.344659 0.731547 11.00000 -1.20000 AFIX 0 C6S 1 0.483438 0.277391 0.647021 10.50000 0.11150 AFIX 33 H6SA 2 0.512750 0.323262 0.689212 10.50000 -1.50000 H6SB 2 0.441505 0.243720 0.658571 10.50000 -1.50000 H6SC 2 0.561787 0.261745 0.631536 10.50000 -1.50000 AFIX 0 C7 1 0.068797 0.340109 0.747586 11.00000 0.06659 0.05492 = 0.07144 0.03297 0.02552 0.00913 C8 1 -0.057844 0.291174 0.722370 11.00000 0.05765 0.07330 = 0.07372 0.02967 0.02598 0.00580 AFIX 43 H8 2 -0.130419 0.305564 0.741155 11.00000 -1.20000 AFIX 0 C9 1 -0.070402 0.223761 0.670872 11.00000 0.05074 0.07549 = 0.07262 0.03039 0.02240 0.00236 AFIX 43 H9 2 -0.153832 0.192367 0.653977 11.00000 -1.20000 AFIX 0 C12 1 -0.075529 0.420107 0.900469 11.00000 0.06900 0.03657 = 0.05321 0.01853 0.01967 0.00559 C13 1 0.008218 0.380168 0.917623 11.00000 0.06304 0.07592 = 0.06141 0.03353 0.02747 0.01803 AFIX 43 H13 2 0.071915 0.364132 0.892372 11.00000 -1.20000 AFIX 0 C14 1 0.003247 0.362657 0.969696 11.00000 0.07409 0.04775 = 0.07007 0.03318 0.02905 0.01446 AFIX 43 H14 2 0.061323 0.333660 0.979048 11.00000 -1.20000 AFIX 0 C15 1 -0.086773 0.386923 1.009890 11.00000 0.06434 0.04667 = 0.06726 0.01515 0.02966 0.00088 C16 1 -0.174146 0.427981 0.991641 11.00000 0.06143 0.07458 = 0.07614 0.04163 0.02852 0.02139 AFIX 43 H16 2 -0.238760 0.443466 1.016397 11.00000 -1.20000 AFIX 0 C17 1 -0.168547 0.446083 0.939507 11.00000 0.06640 0.06995 = 0.05374 0.02190 0.02008 0.01916 AFIX 43 H17 2 -0.225440 0.475292 0.929660 11.00000 -1.20000 AFIX 0 C18 1 -0.095379 0.369811 1.066991 11.00000 0.05399 0.06553 = 0.06980 0.02936 0.02681 0.00905 C23 1 -0.096545 0.026187 0.398567 11.00000 0.06984 0.05859 = 0.08087 0.02497 0.04536 0.01004 C24 1 -0.147646 0.038593 0.336539 11.00000 0.07188 0.05954 = 0.06268 0.02811 0.03092 0.01662 C25 1 -0.056440 0.065368 0.311641 11.00000 0.07922 0.09459 = 0.09078 0.04420 0.03210 -0.00537 AFIX 43 H25 2 0.038031 0.073382 0.333476 11.00000 -1.20000 AFIX 0 C26 1 -0.101885 0.079676 0.257274 11.00000 0.13969 0.08651 = 0.07989 0.04654 0.04456 0.01170 AFIX 43 H26 2 -0.039176 0.096774 0.240424 11.00000 -1.20000 AFIX 0 C27 1 -0.242448 0.069493 0.224868 11.00000 0.09161 0.06585 = 0.06655 0.01917 0.02125 -0.00160 C28 1 -0.331443 0.044938 0.248905 11.00000 0.09969 0.07530 = 0.07016 0.03156 0.02512 -0.00098 AFIX 43 H28 2 -0.426030 0.038304 0.228277 11.00000 -1.20000 AFIX 0 C29 1 -0.281297 0.029650 0.304454 11.00000 0.08100 0.06972 = 0.06452 0.03304 0.03444 0.00716 AFIX 43 H29 2 -0.344115 0.011967 0.320833 11.00000 -1.20000 AFIX 0 C32 1 -0.556036 -0.005065 0.072705 11.00000 0.11102 0.06691 = 0.06127 0.03009 0.03233 0.01439 C33 1 -0.491608 -0.057935 0.059174 11.00000 0.08515 0.08042 = 0.07742 0.03614 0.02788 -0.00603 AFIX 43 H33 2 -0.396867 -0.048509 0.081042 11.00000 -1.20000 AFIX 0 C34 1 -0.555962 -0.125331 0.015097 11.00000 0.06517 0.05760 = 0.07627 0.03209 0.02351 0.00967 AFIX 43 H34 2 -0.505967 -0.161915 0.005229 11.00000 -1.20000 AFIX 0 C35 1 -0.694534 -0.140373 -0.015301 11.00000 0.08063 0.07629 = 0.05982 0.03075 0.03533 0.01233 C36 1 -0.763993 -0.086902 -0.002659 11.00000 0.09665 0.04396 = 0.07572 0.02759 0.01393 0.02222 AFIX 43 H36 2 -0.859159 -0.096184 -0.023211 11.00000 -1.20000 AFIX 0 C37 1 -0.691985 -0.017483 0.041522 11.00000 0.10119 0.06255 = 0.08574 0.02487 0.02399 0.03127 AFIX 43 H37 2 -0.738187 0.020448 0.049479 11.00000 -1.20000 AFIX 0 C38 1 -0.767834 -0.213974 -0.067898 11.00000 0.07943 0.05957 = 0.05714 0.03666 0.02375 0.01530 C43 1 -0.868274 -0.296911 -0.254427 11.00000 0.06231 0.06907 = 0.06006 0.02638 0.02191 0.01152 C44 1 -0.856862 -0.274497 -0.308295 11.00000 0.07034 0.07392 = 0.06051 0.03945 0.02633 0.01330 C45 1 -0.729167 -0.251226 -0.310714 11.00000 0.06618 0.09660 = 0.07660 0.04360 0.02929 0.00713 AFIX 43 H45 2 -0.648455 -0.249868 -0.278220 11.00000 -1.20000 AFIX 0 C46 1 -0.724569 -0.230274 -0.362058 11.00000 0.09016 0.06987 = 0.09561 0.04529 0.04666 0.00767 AFIX 43 H46 2 -0.639107 -0.214963 -0.364510 11.00000 -1.20000 AFIX 0 C47 1 -0.838380 -0.231059 -0.408676 11.00000 0.06770 0.05584 = 0.05976 0.02583 0.01646 0.00843 C48 1 -0.960915 -0.252952 -0.405936 11.00000 0.06737 0.10003 = 0.09479 0.05868 0.02411 0.01063 AFIX 43 H48 2 -1.040457 -0.254813 -0.439474 11.00000 -1.20000 AFIX 0 C49 1 -0.971832 -0.272779 -0.354579 11.00000 0.06430 0.11027 = 0.08863 0.05604 0.02668 0.01123 AFIX 43 H49 2 -1.058407 -0.285141 -0.351344 11.00000 -1.20000 AFIX 0 C52 1 0.211400 0.660163 1.421070 11.00000 0.07063 0.06272 = 0.06214 0.02679 0.02290 0.00378 C53 1 0.282867 0.612593 1.387534 11.00000 0.09094 0.08314 = 0.07584 0.03395 0.03604 0.01630 AFIX 43 H53 2 0.377913 0.625990 1.399150 11.00000 -1.20000 AFIX 0 C54 1 0.219438 0.544834 1.336649 11.00000 0.06399 0.08235 = 0.06199 0.01924 0.02509 0.00022 AFIX 43 H54 2 0.271494 0.512539 1.314048 11.00000 -1.20000 AFIX 0 C55 1 0.081650 0.524057 1.318669 11.00000 0.06868 0.07040 = 0.05689 0.03608 0.02440 0.02005 C56 1 0.006334 0.573371 1.353459 11.00000 0.06995 0.07033 = 0.06334 0.03241 0.02593 0.00429 AFIX 43 H56 2 -0.088928 0.560545 1.341540 11.00000 -1.20000 AFIX 0 C57 1 0.072283 0.640043 1.404688 11.00000 0.09998 0.05620 = 0.06782 0.02472 0.03466 0.01979 AFIX 43 H57 2 0.022276 0.672534 1.429019 11.00000 -1.20000 AFIX 0 C58 1 0.010108 0.451750 1.259905 11.00000 0.07219 0.05533 = 0.06012 0.02714 0.02600 0.00797 C62 1 0.302406 0.314925 1.211861 11.00000 0.09328 0.07769 = 0.09320 0.03713 0.02154 0.01802 AFIX 43 H62 2 0.294684 0.353658 1.252809 11.00000 -1.20000 AFIX 0 C63 1 0.437611 0.297773 1.211053 11.00000 0.06731 0.10556 = 0.14088 0.07507 0.03418 0.01999 AFIX 43 H63 2 0.516439 0.321677 1.250565 11.00000 -1.20000 AFIX 0 C64 1 0.438080 0.244187 1.147925 11.00000 0.07670 0.08303 = 0.14016 0.01419 0.05199 0.00977 AFIX 43 H64 2 0.522539 0.233710 1.141132 11.00000 -1.20000 AFIX 0 C65 1 0.323678 0.205265 1.094524 11.00000 0.08313 0.09874 = 0.13948 0.04722 0.05318 0.02955 AFIX 43 H65 2 0.325872 0.164680 1.053615 11.00000 -1.20000 AFIX 0 C66 1 0.204213 0.226937 1.101982 11.00000 0.08399 0.09002 = 0.09636 0.04982 0.03839 0.01282 AFIX 43 H66 2 0.123983 0.202511 1.063504 11.00000 -1.20000 AFIX 0 C72 1 0.428693 0.075432 0.543650 11.00000 0.07427 0.07949 = 0.15343 0.05656 0.03754 0.01032 AFIX 43 H72 2 0.423176 0.082672 0.588874 11.00000 -1.20000 AFIX 0 C73 1 0.550819 0.097414 0.538769 11.00000 0.06097 0.08105 = 0.26495 0.03516 0.06634 0.00478 AFIX 43 H73 2 0.625056 0.123334 0.580418 11.00000 -1.20000 AFIX 0 C74 1 0.563635 0.082774 0.478043 11.00000 0.08318 0.11413 = 0.33759 0.13330 0.13932 0.06310 AFIX 43 H74 2 0.649964 0.093316 0.473547 11.00000 -1.20000 AFIX 0 C75 1 0.452636 0.051683 0.418837 11.00000 0.14308 0.18789 = 0.25570 0.13204 0.15574 0.06663 AFIX 43 H75 2 0.459146 0.043674 0.373556 11.00000 -1.20000 AFIX 0 C76 1 0.333951 0.032844 0.426953 11.00000 0.11322 0.15751 = 0.14226 0.07475 0.09245 0.03907 AFIX 43 H76 2 0.257480 0.009790 0.385960 11.00000 -1.20000 AFIX 0 C82 1 -0.475901 -0.358310 -0.103218 11.00000 0.08250 0.11897 = 0.16979 0.05767 0.02678 0.02615 AFIX 43 H82 2 -0.482010 -0.315433 -0.066093 11.00000 -1.20000 AFIX 0 C83 1 -0.351395 -0.380720 -0.098495 11.00000 0.06195 0.24067 = 0.22049 0.11434 0.03094 0.03878 AFIX 43 H83 2 -0.279833 -0.355191 -0.055504 11.00000 -1.20000 AFIX 0 C84 1 -0.328626 -0.434874 -0.150118 11.00000 0.08806 0.14548 = 0.28640 0.15512 0.11751 0.05172 AFIX 43 H84 2 -0.241740 -0.445266 -0.151912 11.00000 -1.20000 AFIX 0 C85 1 -0.449692 -0.475057 -0.201987 11.00000 0.13264 0.10564 = 0.22791 0.11354 0.12224 0.06535 AFIX 43 H85 2 -0.447474 -0.519596 -0.238003 11.00000 -1.20000 AFIX 0 C86 1 -0.571610 -0.454211 -0.204159 11.00000 0.10259 0.07639 = 0.19238 0.05120 0.08159 0.01886 AFIX 43 H86 2 -0.649924 -0.484374 -0.241362 11.00000 -1.20000 AFIX 0 HKLF 4 REM REM R1 = 0.0974 for 7028 Fo > 4sig(Fo) and 0.1630 for all 16297 data REM 751 parameters refined using 46 restraints END WGHT 0.1625 0.0000 REM Highest difference peak 0.729, deepest hole -1.110, 1-sigma level 0.114 Q1 1 -0.7372 -0.2235 -0.4692 11.00000 0.05 0.73 Q2 1 0.3211 0.2847 0.4917 11.00000 0.05 0.69 Q3 1 0.7359 0.0757 0.5079 11.00000 0.05 0.68 Q4 1 0.0927 -0.0193 0.4293 11.00000 0.05 0.66 Q5 1 -0.0097 0.0985 0.5051 11.00000 0.05 0.65 Q6 1 0.1430 0.2377 1.1671 11.00000 0.05 0.63 Q7 1 -0.0207 0.3104 1.1055 11.00000 0.05 0.62 Q8 1 0.1291 0.0380 0.5542 11.00000 0.05 0.59 Q9 1 -0.1244 0.4092 1.1717 11.00000 0.05 0.57 Q10 1 0.4539 0.0334 0.4845 11.00000 0.05 0.53 Q11 1 -0.7808 -0.3492 -0.1052 11.00000 0.05 0.51 Q12 1 -0.0023 0.3330 1.2161 11.00000 0.05 0.50 Q13 1 -0.6734 -0.3637 -0.1492 11.00000 0.05 0.49 Q14 1 0.3239 0.3506 0.5547 11.00000 0.05 0.49 Q15 1 -0.8735 -0.3386 -0.1666 11.00000 0.05 0.49 Q16 1 0.3124 0.4053 0.6114 11.00000 0.05 0.49 Q17 1 -0.8621 -0.1813 -0.5135 11.00000 0.05 0.49 Q18 1 -0.7783 -0.3682 -0.2198 11.00000 0.05 0.49 Q19 1 -0.5219 0.1109 0.1888 11.00000 0.05 0.48 Q20 1 0.3513 0.2277 0.5501 11.00000 0.05 0.48 Q21 1 -0.6178 -0.4327 -0.1495 11.00000 0.05 0.46 Q22 1 -0.4621 -0.5483 -0.2233 11.00000 0.05 0.46 Q23 1 -0.0138 0.4369 0.7902 11.00000 0.05 0.45 Q24 1 -0.7201 -0.4784 -0.1563 11.00000 0.05 0.44 Q25 1 0.3648 0.1378 1.1073 11.00000 0.05 0.44 Q26 1 0.4516 0.2095 0.5036 11.00000 0.05 0.43 Q27 1 0.0922 0.2960 1.1105 11.00000 0.05 0.43 Q28 1 -0.4735 -0.5096 -0.1655 11.00000 0.05 0.42 Q29 1 0.3982 0.3128 0.6138 11.00000 0.05 0.42 Q30 1 0.3324 -0.0291 0.4818 11.00000 0.05 0.42 Q31 1 -0.1116 0.2830 1.1652 11.00000 0.05 0.41 Q32 1 -0.6382 -0.3775 -0.1684 11.00000 0.05 0.41 Q33 1 0.3617 0.3363 0.6179 11.00000 0.05 0.40 Q34 1 0.1937 0.2701 0.7387 11.00000 0.05 0.40 Q35 1 0.0707 0.3775 0.8452 11.00000 0.05 0.39 Q36 1 -0.4676 -0.3744 -0.1627 11.00000 0.05 0.38 Q37 1 0.1107 -0.0518 0.5042 11.00000 0.05 0.38 Q38 1 0.3359 0.1083 0.4791 11.00000 0.05 0.37 Q39 1 -0.6674 -0.4504 -0.2320 11.00000 0.05 0.37 Q40 1 -0.8654 -0.1307 -0.4769 11.00000 0.05 0.37 Q41 1 -0.4192 -0.4106 -0.0765 11.00000 0.05 0.36 Q42 1 0.3813 0.7179 1.5170 11.00000 0.05 0.36 Q43 1 -0.3470 -0.4283 -0.1252 11.00000 0.05 0.36 Q44 1 0.3971 0.7171 1.4804 11.00000 0.05 0.36 Q45 1 0.2214 0.1979 0.4711 11.00000 0.05 0.36 Q46 1 -0.5609 0.1097 0.0974 11.00000 0.05 0.35 Q47 1 0.5391 0.3215 0.7212 11.00000 0.05 0.35 Q48 1 -0.8325 -0.1548 -0.4182 11.00000 0.05 0.34 Q49 1 -0.5587 -0.5189 -0.2101 11.00000 0.05 0.34 Q50 1 -1.0754 -0.2797 -0.2190 11.00000 0.05 0.34 Q51 1 -0.0647 0.4495 0.8855 11.00000 0.05 0.34 Q52 1 0.2863 0.1809 0.4537 11.00000 0.05 0.34 ; _shelx_res_checksum 823 _shelx_fab_file ; -13 0 5 0.3537 0.0517 -13 0 6 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2.1078 0.2001 10 -8 3 -1.7419 -0.0819 10 -8 4 2.7940 0.0189 10 -8 5 5.0111 -0.0636 10 -8 6 1.6482 0.0216 10 -8 7 -0.3772 -0.0377 10 -8 8 -2.2702 -0.0297 10 -8 9 -4.2593 -0.0315 10 -8 10 2.0274 0.0250 10 -8 11 2.9486 -0.0455 10 -8 12 -0.8454 0.0141 10 -8 13 -5.5420 0.0160 10 -8 14 1.2733 -0.0524 10 -7 0 -2.3822 -0.5609 10 -7 1 2.0225 0.1679 10 -7 2 -2.4152 -0.2785 10 -7 3 0.0302 -0.0751 10 -7 4 1.0075 0.0378 10 -7 5 1.2873 0.0555 10 -7 6 -0.7422 -0.0947 10 -7 7 -1.1206 -0.0004 10 -7 8 -3.9683 0.0110 10 -7 9 -0.7964 -0.0287 10 -7 10 -0.3313 -0.0066 10 -7 11 3.7390 0.0218 10 -7 12 0.1349 -0.0077 10 -7 13 5.2389 -0.0014 10 -7 14 0.2786 -0.0378 10 -6 0 0.3912 0.1989 10 -6 1 -1.8733 0.0164 10 -6 2 1.7117 -0.0569 10 -6 3 1.5463 -0.0420 10 -6 4 0.9753 -0.0081 10 -6 5 -0.3632 -0.0536 10 -6 6 2.7592 -0.0276 10 -6 7 -3.0331 0.0401 10 -6 8 -1.8937 -0.0361 10 -6 9 -1.1192 -0.0240 10 -6 10 0.0694 0.0504 10 -6 11 -4.4208 0.0170 10 -6 12 0.6919 0.0153 10 -6 13 -0.5199 0.0869 10 -5 0 -3.0550 -0.4060 10 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-4.0449 0.0138 11 -6 8 -2.8498 -0.1018 11 -6 9 -0.0940 0.0542 11 -6 10 -1.5838 -0.0351 11 -6 11 1.4811 -0.1220 11 -5 0 0.7687 0.4258 11 -5 1 2.2904 0.0190 11 -5 2 0.4671 0.0490 11 -5 3 1.6629 -0.0298 11 -5 4 0.3349 0.0328 11 -5 5 2.6978 -0.0506 11 -5 6 -1.1492 0.0867 11 -5 7 -1.0114 0.0235 11 -5 8 0.9559 0.0281 11 -5 9 1.1533 0.0536 11 -5 10 -2.0136 0.0450 11 -4 0 -2.9342 0.0598 11 -4 1 0.8666 0.0533 11 -4 2 3.7123 -0.1411 11 -4 3 -1.7625 0.0120 11 -4 4 3.0193 0.1240 11 -4 5 0.7938 -0.0233 11 -4 6 -0.5302 0.0058 11 -4 7 -3.1388 0.0699 11 -4 8 2.0411 0.0200 11 -4 9 0.5404 0.0215 11 -3 0 -5.5791 0.4724 11 -3 1 1.6707 0.1961 11 -3 2 -3.3373 -0.3196 11 -3 3 1.2693 0.0045 11 -3 4 1.1238 0.0118 11 -3 5 1.5954 0.0360 11 -3 6 -2.0196 -0.0073 11 -3 7 0.0453 0.0575 11 -3 8 -3.8884 -0.0333 11 -2 0 2.1406 0.5164 11 -2 1 -7.5432 -0.0046 11 -2 2 -0.8468 0.0662 11 -2 3 3.1242 -0.0458 11 -2 4 2.1071 0.0566 11 -2 5 0.9795 -0.0519 11 -2 6 2.1215 0.0171 11 -2 7 -3.8494 0.0160 11 -2 8 -0.5371 0.0336 11 -1 0 -1.0245 0.1080 11 -1 1 -3.2257 0.1032 11 -1 2 -0.3800 -0.2158 11 -1 3 -1.7797 0.0408 11 -1 4 2.4113 0.0961 11 -1 5 5.6173 0.0206 11 -1 6 -2.8287 0.0081 11 -1 7 0.4223 0.0463 11 0 0 -3.2804 0.7116 11 0 1 0.1769 0.1514 11 0 2 -1.4814 -0.2609 11 0 3 -2.8830 0.0004 11 0 4 1.9473 -0.0035 11 0 5 0.7933 0.0536 11 0 6 2.7945 0.0209 11 1 0 -0.7090 0.5182 11 1 1 2.0081 0.0119 11 1 2 -1.2506 0.0864 11 1 3 -4.3981 -0.0103 11 1 4 -4.3940 0.0598 11 1 5 1.7725 -0.0313 11 2 0 -2.2077 0.1930 11 2 1 2.7474 0.1163 11 2 2 0.9161 -0.3089 11 2 3 -5.9110 0.0442 11 2 4 -0.5278 0.0767 11 2 5 -4.8863 0.0395 11 3 0 0.8477 0.8488 11 3 1 3.7655 0.0857 11 3 2 2.2431 -0.1761 11 3 3 3.3796 -0.0136 11 3 4 -2.2478 -0.0531 11 4 0 -1.3744 0.3991 11 4 1 -3.9417 0.1149 11 4 2 0.1890 0.0719 11 4 3 -1.9158 0.0883 11 5 0 1.2975 0.3259 11 5 1 -0.1832 0.1290 11 5 2 -1.7533 -0.3718 11 6 0 1.1942 0.7377 11 6 1 2.2905 0.0924 12 -13 0 -4.8095 0.2606 12 -12 0 0.6305 -0.0476 12 -12 1 -3.9622 -0.0381 12 -12 2 3.7742 0.0288 12 -12 3 4.6092 0.0012 12 -11 0 -2.2865 0.2098 12 -11 1 -7.6089 0.1800 12 -11 2 -3.8417 -0.1594 12 -11 3 2.4486 0.0586 12 -11 4 2.4445 0.0443 12 -11 5 0.5969 0.0107 12 -10 0 4.4171 0.4302 12 -10 1 -2.6324 -0.0236 12 -10 2 -0.7722 0.0311 12 -10 3 -1.1245 0.0574 12 -10 4 3.3508 -0.0246 12 -10 5 2.2163 -0.0816 12 -10 6 -0.0743 0.1059 12 -9 0 -3.8957 0.0501 12 -9 1 4.1619 0.0270 12 -9 2 -1.1200 -0.0085 12 -9 3 0.9652 0.0237 12 -9 4 -1.2753 0.0054 12 -9 5 -2.0288 0.0315 12 -9 6 2.2027 0.0749 12 -9 7 -1.7209 0.0310 12 -8 0 -1.9840 0.3907 12 -8 1 -3.0632 0.1541 12 -8 2 3.1838 -0.1919 12 -8 3 2.7529 0.0326 12 -8 4 -1.5943 0.0174 12 -8 5 -2.0783 0.0147 12 -8 6 -3.6022 -0.0490 12 -8 7 -3.0451 0.0992 12 -8 8 -0.7282 -0.0128 12 -7 0 -3.2453 0.4296 12 -7 1 -0.0010 -0.0573 12 -7 2 1.8495 0.0785 12 -7 3 4.9883 0.0179 12 -7 4 4.6590 -0.0308 12 -7 5 -0.4166 -0.0662 12 -7 6 -3.1727 0.1263 12 -7 7 -4.0533 -0.1044 12 -7 8 -3.5186 -0.0249 12 -6 1 -0.2325 0.0858 12 -6 2 -0.9152 -0.0612 12 -6 3 2.9609 0.0274 12 -6 4 3.4931 0.0749 12 -6 5 2.6255 0.1135 12 -6 6 -0.0101 0.0329 12 -6 7 -1.0794 0.0442 12 -5 0 1.1040 0.5524 12 -5 1 -2.6559 0.1247 12 -5 3 -0.6085 0.0410 12 -5 4 1.7979 -0.0574 12 -5 5 0.6352 -0.0232 12 -5 6 -1.8639 -0.0000 12 -5 7 0.2863 0.0687 12 -4 0 -0.8167 0.4222 12 -4 1 1.8923 -0.0872 12 -4 2 -4.7613 0.1435 12 -4 3 0.1758 0.0420 12 -4 4 0.2614 -0.0472 12 -4 5 -0.9202 -0.0213 12 -4 6 -3.5077 0.0969 12 -3 0 4.9211 0.2120 12 -3 1 -3.7144 0.0859 12 -3 2 -0.9881 -0.1951 12 -3 3 -1.0687 0.0419 12 -3 4 -0.2070 0.0491 12 -2 0 -1.6190 0.7071 12 -2 1 5.8066 0.1217 12 -2 2 1.1393 -0.0863 12 -2 3 -0.5187 0.0845 12 -2 4 4.2145 -0.0388 12 -1 0 -3.1542 0.3311 12 -1 1 0.1496 0.0023 12 -1 2 -3.4405 0.1125 12 -1 3 1.4258 0.0770 12 0 0 -0.8527 0.2442 12 0 1 0.2988 0.0492 12 0 2 -0.0055 -0.3045 12 1 1 -1.1746 0.0821 12 2 0 2.6845 0.2173 13 -10 0 -2.1958 0.2298 13 -9 0 -0.1260 0.2502 13 -9 1 -1.4314 -0.0038 13 -9 2 1.2563 0.1068 13 -8 0 0.5760 -0.0062 13 -8 1 0.3012 -0.0523 13 -8 2 1.2658 -0.0047 13 -8 3 1.5075 -0.0149 13 -7 0 -2.4143 0.3810 13 -7 1 -3.4060 0.0935 13 -7 2 -2.3415 -0.0224 13 -7 3 2.7229 -0.0413 13 -7 4 2.9427 0.1673 13 -6 0 3.8895 0.1813 13 -6 1 -2.9112 -0.0344 13 -6 2 -3.0656 0.0887 13 -6 3 0.6899 0.1041 13 -5 0 3.4322 0.0337 13 -5 1 2.4887 0.0055 13 -5 2 0.3290 -0.0033 13 -4 0 -1.5102 0.4037 13 -4 1 1.2351 0.0126 13 -3 0 -0.8318 0.0457 0 0 0 0.0 0.0 ; _shelx_fab_checksum 63095 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, -z' 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 0.00546(10) 0.31494(5) 1.16229(5) 0.0595(3) Uani 1 1 d . . . . . Cu2 Cu 0.12480(9) 0.01420(5) 0.49883(6) 0.0601(3) Uani 1 1 d . . . . . Cu3 Cu -0.77143(10) -0.35551(5) -0.16073(6) 0.0599(3) Uani 1 1 d . . . . . S10 S 0.1019(2) 0.42783(11) 0.81157(12) 0.0700(6) Uani 1 1 d . . . . . S11 S -0.0740(2) 0.44649(12) 0.83405(12) 0.0690(6) Uani 1 1 d . . . . . S30 S -0.2798(3) 0.08970(14) 0.15249(14) 0.0982(10) Uani 1 1 d . . . . . S31 S -0.4810(3) 0.08551(14) 0.12958(15) 0.0980(9) Uani 1 1 d . . . . . S50 S -0.8329(3) -0.20125(13) -0.47253(14) 0.0854(8) Uani 1 1 d . . . . . S51 S 0.3024(3) 0.74640(13) 1.48208(14) 0.0832(8) Uani 1 1 d . . . . . O1 O 0.1136(6) 0.1086(3) 0.5667(3) 0.0724(17) Uani 1 1 d . . . . . O1S O 0.3731(17) 0.4003(9) 0.6550(10) 0.121(5) Uiso 0.5 1 d D . P . . O2 O 0.0972(6) -0.0853(3) 0.4316(3) 0.0722(16) Uani 1 1 d . . . . . O19 O -0.0077(6) 0.3355(3) 1.0819(3) 0.0646(15) Uani 1 1 d . . . . . O20 O -0.8160(5) -0.3894(3) -0.0964(3) 0.0642(14) Uani 1 1 d . . . . . O21 O 0.1825(5) -0.0054(3) 0.5790(3) 0.0722(16) Uani 1 1 d . . . . . O22 O 0.0259(6) 0.0292(3) 0.4192(3) 0.0817(18) Uani 1 1 d . . . . . O39 O -0.6977(5) -0.2622(3) -0.0785(3) 0.0660(15) Uani 1 1 d . . . . . O40 O -0.8931(6) -0.2218(3) -0.0950(3) 0.0674(15) Uani 1 1 d . . . . . O41 O -0.7631(6) -0.3122(3) -0.2240(3) 0.0686(15) Uani 1 1 d . . . . . O42 O -0.9820(5) -0.3005(3) -0.2429(3) 0.0697(16) Uani 1 1 d . . . . . O59 O -0.1161(6) 0.4384(3) 1.2455(3) 0.0700(16) Uani 1 1 d . . . . . O60 O 0.0838(5) 0.4132(3) 1.2308(3) 0.0657(15) Uani 1 1 d . . . . . N3S N 0.3761(17) 0.2830(9) 0.5845(10) 0.091(5) Uiso 0.5 1 d . . P . . N61 N 0.1958(7) 0.2802(4) 1.1603(4) 0.0671(19) Uani 1 1 d . . . . . N71 N 0.3191(7) 0.0449(4) 0.4892(5) 0.078(2) Uani 1 1 d . U . . . N81 N -0.5828(8) -0.3946(4) -0.1569(5) 0.074(2) Uani 1 1 d . U . . . C2S C 0.333(2) 0.3464(12) 0.5960(12) 0.110(7) Uiso 0.5 1 d D . P . . H2S H 0.270214 0.348251 0.557511 0.132 Uiso 0.5 1 calc R . P . . C3 C 0.0178(8) 0.1262(4) 0.5887(5) 0.067(2) Uani 1 1 d . . . . . C4 C 0.0300(7) 0.2001(4) 0.6432(5) 0.058(2) Uani 1 1 d . . . . . C5 C 0.1517(9) 0.2459(5) 0.6651(5) 0.080(3) Uani 1 1 d . . . . . H5 H 0.222028 0.230366 0.644852 0.096 Uiso 1 1 calc R . . . . C5S C 0.317(2) 0.2261(10) 0.5185(11) 0.088(6) Uiso 0.5 1 d . . P . . H5SA H 0.371240 0.189524 0.512115 0.132 Uiso 0.5 1 calc GR . P . . H5SB H 0.313458 0.240366 0.481498 0.132 Uiso 0.5 1 calc GR . P . . H5SC H 0.225583 0.208137 0.515218 0.132 Uiso 0.5 1 calc GR . P . . C6 C 0.1687(9) 0.3141(4) 0.7166(5) 0.080(3) Uani 1 1 d . . . . . H6 H 0.252399 0.344659 0.731547 0.097 Uiso 1 1 calc R . . . . C6S C 0.483(2) 0.2774(13) 0.6470(13) 0.112(8) Uiso 0.5 1 d . . P . . H6SA H 0.512750 0.323262 0.689212 0.167 Uiso 0.5 1 calc R . P . . H6SB H 0.441505 0.243720 0.658571 0.167 Uiso 0.5 1 calc R . P . . H6SC H 0.561787 0.261745 0.631536 0.167 Uiso 0.5 1 calc R . P . . C7 C 0.0688(8) 0.3401(4) 0.7476(5) 0.062(2) Uani 1 1 d . . . . . C8 C -0.0578(8) 0.2912(5) 0.7224(5) 0.069(2) Uani 1 1 d . . . . . H8 H -0.130419 0.305564 0.741155 0.083 Uiso 1 1 calc R . . . . C9 C -0.0704(8) 0.2238(5) 0.6709(5) 0.068(2) Uani 1 1 d . . . . . H9 H -0.153832 0.192367 0.653977 0.081 Uiso 1 1 calc R . . . . C12 C -0.0755(8) 0.4201(4) 0.9005(4) 0.0538(19) Uani 1 1 d . . . . . C13 C 0.0082(8) 0.3802(5) 0.9176(4) 0.064(2) Uani 1 1 d . . . . . H13 H 0.071915 0.364132 0.892372 0.077 Uiso 1 1 calc R . . . . C14 C 0.0032(8) 0.3627(4) 0.9697(4) 0.060(2) Uani 1 1 d . . . . . H14 H 0.061323 0.333660 0.979048 0.072 Uiso 1 1 calc R . . . . C15 C -0.0868(8) 0.3869(4) 1.0099(5) 0.062(2) Uani 1 1 d . . . . . C16 C -0.1741(8) 0.4280(5) 0.9916(5) 0.066(2) Uani 1 1 d . . . . . H16 H -0.238760 0.443466 1.016397 0.079 Uiso 1 1 calc R . . . . C17 C -0.1685(8) 0.4461(5) 0.9395(4) 0.065(2) Uani 1 1 d . . . . . H17 H -0.225440 0.475292 0.929660 0.078 Uiso 1 1 calc R . . . . C18 C -0.0954(8) 0.3698(4) 1.0670(5) 0.062(2) Uani 1 1 d . . . . . C23 C -0.0965(9) 0.0262(4) 0.3986(5) 0.068(2) Uani 1 1 d . . . . . C24 C -0.1476(9) 0.0386(4) 0.3365(5) 0.063(2) Uani 1 1 d . . . . . C25 C -0.0564(10) 0.0654(5) 0.3116(6) 0.088(3) Uani 1 1 d . . . . . H25 H 0.038031 0.073382 0.333476 0.105 Uiso 1 1 calc R . . . . C26 C -0.1019(13) 0.0797(6) 0.2573(6) 0.097(3) Uani 1 1 d . . . . . H26 H -0.039176 0.096774 0.240424 0.117 Uiso 1 1 calc R . . . . C27 C -0.2424(11) 0.0695(5) 0.2249(5) 0.080(3) Uani 1 1 d . . . . . C28 C -0.3314(11) 0.0449(5) 0.2489(5) 0.084(3) Uani 1 1 d . . . . . H28 H -0.426030 0.038304 0.228277 0.100 Uiso 1 1 calc R . . . . C29 C -0.2813(9) 0.0297(4) 0.3045(5) 0.069(2) Uani 1 1 d . . . . . H29 H -0.344115 0.011967 0.320833 0.083 Uiso 1 1 calc R . . . . C32 C -0.5560(12) -0.0051(5) 0.0727(5) 0.078(3) Uani 1 1 d . . . . . C33 C -0.4916(11) -0.0579(5) 0.0592(5) 0.082(3) Uani 1 1 d . . . . . H33 H -0.396867 -0.048509 0.081042 0.098 Uiso 1 1 calc R . . . . C34 C -0.5560(9) -0.1253(4) 0.0151(5) 0.066(2) Uani 1 1 d . . . . . H34 H -0.505967 -0.161915 0.005229 0.079 Uiso 1 1 calc R . . . . C35 C -0.6945(9) -0.1404(5) -0.0153(5) 0.070(2) Uani 1 1 d . . . . . C36 C -0.7640(10) -0.0869(4) -0.0027(5) 0.074(2) Uani 1 1 d D . . . . H36 H -0.859159 -0.096184 -0.023211 0.089 Uiso 1 1 calc R . . . . C37 C -0.6920(11) -0.0175(5) 0.0415(5) 0.087(3) Uani 1 1 d D . . . . H37 H -0.738187 0.020448 0.049479 0.104 Uiso 1 1 calc R . . . . C38 C -0.7678(10) -0.2140(4) -0.0679(4) 0.061(2) Uani 1 1 d . . . . . C43 C -0.8683(9) -0.2969(5) -0.2544(5) 0.065(2) Uani 1 1 d . . . . . C44 C -0.8569(9) -0.2745(5) -0.3083(5) 0.064(2) Uani 1 1 d . . . . . C45 C -0.7292(9) -0.2512(5) -0.3107(5) 0.077(3) Uani 1 1 d . . . . . H45 H -0.648455 -0.249868 -0.278220 0.093 Uiso 1 1 calc R . . . . C46 C -0.7246(11) -0.2303(5) -0.3621(5) 0.079(3) Uani 1 1 d . . . . . H46 H -0.639107 -0.214963 -0.364510 0.095 Uiso 1 1 calc R . . . . C47 C -0.8384(9) -0.2311(4) -0.4087(5) 0.062(2) Uani 1 1 d . . . . . C48 C -0.9609(10) -0.2530(5) -0.4059(6) 0.083(3) Uani 1 1 d . . . . . H48 H -1.040457 -0.254813 -0.439474 0.099 Uiso 1 1 calc R . . . . C49 C -0.9718(10) -0.2728(6) -0.3546(5) 0.084(3) Uani 1 1 d . . . . . H49 H -1.058407 -0.285141 -0.351344 0.100 Uiso 1 1 calc R . . . . C52 C 0.2114(9) 0.6602(4) 1.4211(5) 0.066(2) Uani 1 1 d . . . . . C53 C 0.2829(11) 0.6126(5) 1.3875(5) 0.082(3) Uani 1 1 d . . . . . H53 H 0.377913 0.625990 1.399150 0.099 Uiso 1 1 calc R . . . . C54 C 0.2194(9) 0.5448(5) 1.3366(5) 0.074(3) Uani 1 1 d . . . . . H54 H 0.271494 0.512539 1.314048 0.089 Uiso 1 1 calc R . . . . C55 C 0.0817(8) 0.5241(5) 1.3187(4) 0.061(2) Uani 1 1 d . . . . . C56 C 0.0063(9) 0.5734(4) 1.3535(5) 0.067(2) Uani 1 1 d . . . . . H56 H -0.088928 0.560545 1.341540 0.080 Uiso 1 1 calc R . . . . C57 C 0.0723(10) 0.6400(5) 1.4047(5) 0.074(3) Uani 1 1 d . . . . . H57 H 0.022276 0.672534 1.429019 0.089 Uiso 1 1 calc R . . . . C58 C 0.0101(9) 0.4517(4) 1.2599(4) 0.061(2) Uani 1 1 d . . . . . C62 C 0.3024(11) 0.3149(6) 1.2119(6) 0.090(3) Uani 1 1 d . . . . . H62 H 0.294684 0.353658 1.252809 0.108 Uiso 1 1 calc R . . . . C63 C 0.4376(10) 0.2978(6) 1.2111(7) 0.097(3) Uani 1 1 d . . . . . H63 H 0.516439 0.321677 1.250565 0.116 Uiso 1 1 calc R . . . . C64 C 0.4381(12) 0.2442(6) 1.1479(8) 0.111(4) Uani 1 1 d . . . . . H64 H 0.522539 0.233710 1.141132 0.133 Uiso 1 1 calc R . . . . C65 C 0.3237(12) 0.2053(6) 1.0945(7) 0.106(4) Uani 1 1 d . . . . . H65 H 0.325872 0.164680 1.053615 0.127 Uiso 1 1 calc R . . . . C66 C 0.2042(10) 0.2269(6) 1.1020(6) 0.086(3) Uani 1 1 d . . . . . H66 H 0.123983 0.202511 1.063504 0.103 Uiso 1 1 calc R . . . . C72 C 0.4287(11) 0.0754(5) 0.5437(8) 0.101(3) Uani 1 1 d . U . . . H72 H 0.423176 0.082672 0.588874 0.121 Uiso 1 1 calc R . . . . C73 C 0.5508(11) 0.0974(6) 0.5388(10) 0.150(5) Uani 1 1 d . U . . . H73 H 0.625056 0.123334 0.580418 0.180 Uiso 1 1 calc R . . . . C74 C 0.5636(13) 0.0828(8) 0.4780(12) 0.150(6) Uani 1 1 d . U . . . H74 H 0.649964 0.093316 0.473547 0.180 Uiso 1 1 calc R . . . . C75 C 0.4526(17) 0.0517(9) 0.4188(11) 0.164(6) Uani 1 1 d . U . . . H75 H 0.459146 0.043674 0.373556 0.197 Uiso 1 1 calc R . . . . C76 C 0.3340(13) 0.0328(7) 0.4270(8) 0.124(4) Uani 1 1 d . U . . . H76 H 0.257480 0.009790 0.385960 0.149 Uiso 1 1 calc R . . . . C82 C -0.4759(13) -0.3583(8) -0.1032(9) 0.129(5) Uani 1 1 d . U . . . H82 H -0.482010 -0.315433 -0.066093 0.155 Uiso 1 1 calc R . . . . C83 C -0.3514(13) -0.3807(9) -0.0985(10) 0.173(7) Uani 1 1 d D U . . . H83 H -0.279833 -0.355191 -0.055504 0.208 Uiso 1 1 calc R . . . . C84 C -0.3286(13) -0.4349(7) -0.1501(9) 0.139(6) Uani 1 1 d D U . . . H84 H -0.241740 -0.445266 -0.151912 0.167 Uiso 1 1 calc R . . . . C85 C -0.4497(14) -0.4751(7) -0.2020(9) 0.126(4) Uani 1 1 d . U . . . H85 H -0.447474 -0.519596 -0.238003 0.151 Uiso 1 1 calc R . . . . C86 C -0.5716(12) -0.4542(6) -0.2042(8) 0.121(4) Uani 1 1 d . U . . . H86 H -0.649924 -0.484374 -0.241362 0.145 Uiso 1 1 calc R . . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.0560(6) 0.0637(6) 0.0667(7) 0.0332(5) 0.0265(5) 0.0101(5) Cu2 0.0526(6) 0.0586(6) 0.0681(7) 0.0247(5) 0.0280(5) 0.0019(4) Cu3 0.0571(6) 0.0608(6) 0.0674(7) 0.0309(5) 0.0266(5) 0.0096(5) S10 0.0893(15) 0.0572(13) 0.0628(14) 0.0232(11) 0.0334(12) 0.0044(11) S11 0.0904(16) 0.0633(14) 0.0635(14) 0.0332(12) 0.0314(12) 0.0217(12) S30 0.135(2) 0.0785(18) 0.0664(17) 0.0327(14) 0.0178(16) -0.0227(16) S31 0.142(3) 0.0614(16) 0.0757(18) 0.0291(14) 0.0167(17) 0.0024(16) S50 0.119(2) 0.0666(15) 0.0775(17) 0.0338(13) 0.0445(16) 0.0047(14) S51 0.0921(17) 0.0723(15) 0.0782(17) 0.0273(13) 0.0351(14) -0.0094(13) O1 0.064(4) 0.063(4) 0.092(5) 0.030(3) 0.039(3) 0.006(3) O2 0.062(3) 0.073(4) 0.073(4) 0.022(3) 0.032(3) 0.001(3) O19 0.063(3) 0.071(4) 0.059(4) 0.024(3) 0.030(3) 0.012(3) O20 0.065(3) 0.062(3) 0.068(4) 0.027(3) 0.029(3) 0.017(3) O21 0.061(3) 0.076(4) 0.083(4) 0.034(3) 0.037(3) 0.003(3) O22 0.061(4) 0.098(5) 0.092(5) 0.047(4) 0.033(3) -0.002(3) O39 0.061(3) 0.068(4) 0.069(4) 0.029(3) 0.023(3) 0.015(3) O40 0.064(4) 0.070(4) 0.071(4) 0.032(3) 0.026(3) 0.010(3) O41 0.063(4) 0.077(4) 0.076(4) 0.041(3) 0.029(3) 0.010(3) O42 0.051(3) 0.090(4) 0.083(4) 0.048(4) 0.029(3) 0.012(3) O59 0.067(4) 0.078(4) 0.071(4) 0.034(3) 0.032(3) 0.014(3) O60 0.051(3) 0.076(4) 0.071(4) 0.030(3) 0.032(3) 0.006(3) N61 0.065(4) 0.061(4) 0.072(5) 0.025(4) 0.026(4) 0.016(4) N71 0.064(4) 0.072(5) 0.117(6) 0.051(5) 0.047(4) 0.013(4) N81 0.066(4) 0.077(5) 0.106(6) 0.056(5) 0.042(4) 0.024(4) C3 0.055(5) 0.058(5) 0.075(6) 0.018(5) 0.028(4) -0.003(4) C4 0.051(4) 0.055(5) 0.072(6) 0.034(4) 0.018(4) 0.007(4) C5 0.073(6) 0.063(6) 0.096(7) 0.023(5) 0.038(5) 0.003(5) C6 0.069(6) 0.051(5) 0.112(8) 0.023(5) 0.046(6) -0.004(4) C7 0.067(5) 0.055(5) 0.071(6) 0.033(4) 0.026(4) 0.009(4) C8 0.058(5) 0.073(6) 0.074(6) 0.030(5) 0.026(4) 0.006(4) C9 0.051(5) 0.075(6) 0.073(6) 0.030(5) 0.022(4) 0.002(4) C12 0.069(5) 0.037(4) 0.053(5) 0.019(4) 0.020(4) 0.006(4) C13 0.063(5) 0.076(6) 0.061(5) 0.034(5) 0.027(4) 0.018(4) C14 0.074(5) 0.048(4) 0.070(6) 0.033(4) 0.029(4) 0.014(4) C15 0.064(5) 0.047(4) 0.067(6) 0.015(4) 0.030(4) 0.001(4) C16 0.061(5) 0.075(6) 0.076(6) 0.042(5) 0.029(4) 0.021(4) C17 0.066(5) 0.070(6) 0.054(5) 0.022(4) 0.020(4) 0.019(4) C18 0.054(5) 0.066(5) 0.070(6) 0.029(5) 0.027(4) 0.009(4) C23 0.070(6) 0.059(5) 0.081(6) 0.025(5) 0.045(5) 0.010(4) C24 0.072(6) 0.060(5) 0.063(5) 0.028(4) 0.031(5) 0.017(4) C25 0.079(6) 0.095(8) 0.091(8) 0.044(6) 0.032(6) -0.005(5) C26 0.140(11) 0.087(8) 0.080(8) 0.047(7) 0.045(7) 0.012(7) C27 0.092(7) 0.066(6) 0.067(6) 0.019(5) 0.021(5) -0.002(5) C28 0.100(7) 0.075(7) 0.070(7) 0.032(5) 0.025(6) -0.001(5) C29 0.081(6) 0.070(6) 0.065(6) 0.033(5) 0.034(5) 0.007(5) C32 0.111(8) 0.067(6) 0.061(6) 0.030(5) 0.032(6) 0.014(6) C33 0.085(7) 0.080(7) 0.077(7) 0.036(6) 0.028(5) -0.006(6) C34 0.065(5) 0.058(5) 0.076(6) 0.032(5) 0.024(5) 0.010(4) C35 0.081(6) 0.076(6) 0.060(6) 0.031(5) 0.035(5) 0.012(5) C36 0.097(7) 0.044(5) 0.076(6) 0.028(5) 0.014(5) 0.022(5) C37 0.101(8) 0.063(6) 0.086(7) 0.025(6) 0.024(6) 0.031(6) C38 0.079(6) 0.060(5) 0.057(5) 0.037(5) 0.024(5) 0.015(5) C43 0.062(5) 0.069(6) 0.060(5) 0.026(5) 0.022(4) 0.012(4) C44 0.070(5) 0.074(6) 0.061(5) 0.039(5) 0.026(4) 0.013(4) C45 0.066(5) 0.097(7) 0.077(6) 0.044(6) 0.029(5) 0.007(5) C46 0.090(7) 0.070(6) 0.096(8) 0.045(6) 0.047(6) 0.008(5) C47 0.068(5) 0.056(5) 0.060(5) 0.026(4) 0.016(4) 0.008(4) C48 0.067(6) 0.100(8) 0.095(8) 0.059(7) 0.024(5) 0.011(5) C49 0.064(6) 0.110(8) 0.089(7) 0.056(7) 0.027(5) 0.011(5) C52 0.071(5) 0.063(5) 0.062(6) 0.027(5) 0.023(4) 0.004(4) C53 0.091(7) 0.083(7) 0.076(7) 0.034(6) 0.036(6) 0.016(6) C54 0.064(5) 0.082(7) 0.062(6) 0.019(5) 0.025(4) 0.000(5) C55 0.069(5) 0.070(6) 0.057(5) 0.036(5) 0.024(4) 0.020(4) C56 0.070(5) 0.070(6) 0.063(6) 0.032(5) 0.026(4) 0.004(4) C57 0.100(7) 0.056(5) 0.068(6) 0.025(5) 0.035(5) 0.020(5) C58 0.072(6) 0.055(5) 0.060(5) 0.027(4) 0.026(4) 0.008(4) C62 0.093(8) 0.078(7) 0.093(8) 0.037(6) 0.022(7) 0.018(6) C63 0.067(6) 0.106(9) 0.141(11) 0.075(9) 0.034(7) 0.020(6) C64 0.077(7) 0.083(8) 0.140(11) 0.014(8) 0.052(8) 0.010(6) C65 0.083(8) 0.099(9) 0.139(11) 0.047(8) 0.053(8) 0.030(7) C66 0.084(7) 0.090(7) 0.096(8) 0.050(7) 0.038(6) 0.013(6) C72 0.074(6) 0.079(7) 0.153(9) 0.057(7) 0.038(6) 0.010(5) C73 0.061(6) 0.081(8) 0.265(14) 0.035(10) 0.066(8) 0.005(5) C74 0.083(6) 0.114(10) 0.338(19) 0.133(13) 0.139(9) 0.063(7) C75 0.143(10) 0.188(16) 0.256(14) 0.132(14) 0.156(10) 0.067(11) C76 0.113(7) 0.158(12) 0.142(8) 0.075(9) 0.092(7) 0.039(7) C82 0.083(7) 0.119(10) 0.170(12) 0.058(8) 0.027(7) 0.026(6) C83 0.062(7) 0.241(18) 0.220(16) 0.114(11) 0.031(8) 0.039(8) C84 0.088(6) 0.145(11) 0.286(18) 0.155(12) 0.118(9) 0.052(7) C85 0.133(9) 0.106(8) 0.228(13) 0.114(8) 0.122(9) 0.065(7) C86 0.103(7) 0.076(7) 0.192(12) 0.051(7) 0.082(8) 0.019(6) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0052 0.0023 '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 0.2557 1.6823 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0094 0.0046 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0162 0.0086 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1566 0.1676 '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 O19 Cu1 Cu3 84.34(17) . 2_456 ? O19 Cu1 O42 168.1(2) . 2_456 ? O19 Cu1 N61 94.3(3) . . ? O40 Cu1 Cu3 84.14(18) 2_456 2_456 ? O40 Cu1 O19 89.0(2) 2_456 . ? O40 Cu1 O42 89.7(2) 2_456 2_456 ? O40 Cu1 N61 94.8(3) 2_456 . ? O42 Cu1 Cu3 83.75(16) 2_456 2_456 ? O42 Cu1 N61 97.6(3) 2_456 . ? O60 Cu1 Cu3 84.81(17) . 2_456 ? O60 Cu1 O19 91.1(2) . . ? O60 Cu1 O40 168.9(2) . 2_456 ? O60 Cu1 O42 87.9(2) . 2_456 ? O60 Cu1 N61 96.2(3) . . ? N61 Cu1 Cu3 178.4(2) . 2_456 ? O1 Cu2 Cu2 81.89(17) . 2_556 ? O1 Cu2 O22 90.2(3) . . ? O1 Cu2 N71 95.6(3) . . ? O2 Cu2 Cu2 85.96(17) . 2_556 ? O2 Cu2 O1 167.8(2) . . ? O2 Cu2 O22 88.3(3) . . ? O2 Cu2 N71 96.5(3) . . ? O21 Cu2 Cu2 86.46(16) . 2_556 ? O21 Cu2 O1 88.0(3) . . ? O21 Cu2 O2 90.8(3) . . ? O21 Cu2 O22 167.2(2) . . ? O21 Cu2 N71 100.7(3) . . ? O22 Cu2 Cu2 80.74(17) . 2_556 ? O22 Cu2 N71 92.1(3) . . ? N71 Cu2 Cu2 172.3(2) . 2_556 ? O20 Cu3 Cu1 83.26(16) . 2_456 ? O20 Cu3 O41 167.3(2) . . ? O20 Cu3 N81 92.8(2) . . ? O39 Cu3 Cu1 84.23(18) . 2_456 ? O39 Cu3 O20 89.0(2) . . ? O39 Cu3 O41 88.4(2) . . ? O39 Cu3 N81 97.3(3) . . ? O41 Cu3 Cu1 84.11(17) . 2_456 ? O41 Cu3 N81 99.9(3) . . ? O59 Cu3 Cu1 82.16(18) 2_456 2_456 ? O59 Cu3 O20 92.5(2) 2_456 . ? O59 Cu3 O39 166.1(2) 2_456 . ? O59 Cu3 O41 87.2(2) 2_456 . ? O59 Cu3 N81 96.5(3) 2_456 . ? N81 Cu3 Cu1 175.73(18) . 2_456 ? C7 S10 S11 105.8(3) . . ? C12 S11 S10 105.4(3) . . ? C27 S30 S31 103.1(4) . . ? C32 S31 S30 105.5(4) . . ? C47 S50 S51 102.0(3) . 1_443 ? C52 S51 S50 105.6(3) . 1_667 ? C3 O1 Cu2 126.8(5) . . ? C3 O2 Cu2 120.4(5) 2_556 . ? C18 O19 Cu1 120.9(5) . . ? C18 O20 Cu3 122.6(6) 2_456 . ? C23 O21 Cu2 120.6(6) 2_556 . ? C23 O22 Cu2 127.2(6) . . ? C38 O39 Cu3 120.0(6) . . ? C38 O40 Cu1 121.5(6) . 2_456 ? C43 O41 Cu3 121.3(5) . . ? C43 O42 Cu1 122.1(6) . 2_456 ? C58 O59 Cu3 122.3(5) . 2_456 ? C58 O60 Cu1 119.1(5) . . ? C2S N3S C6S 120.8(18) . . ? C5S N3S C2S 116.9(18) . . ? C5S N3S C6S 122.2(17) . . ? C62 N61 Cu1 120.4(7) . . ? C62 N61 C66 119.7(9) . . ? C66 N61 Cu1 119.6(7) . . ? C72 N71 Cu2 122.8(7) . . ? C72 N71 C76 115.8(10) . . ? C76 N71 Cu2 121.4(8) . . ? C82 N81 Cu3 119.6(8) . . ? C86 N81 Cu3 123.5(8) . . ? C86 N81 C82 116.9(11) . . ? O1S C2S N3S 122(2) . . ? O1 C3 O2 124.9(8) . 2_556 ? O1 C3 C4 119.3(7) . . ? O2 C3 C4 115.8(7) 2_556 . ? C5 C4 C3 117.3(7) . . ? C9 C4 C3 123.2(7) . . ? C9 C4 C5 119.4(8) . . ? C6 C5 C4 119.3(8) . . ? C5 C6 C7 122.9(8) . . ? C6 C7 S10 118.6(6) . . ? C6 C7 C8 116.3(8) . . ? C8 C7 S10 125.1(6) . . ? C9 C8 C7 118.8(7) . . ? C4 C9 C8 123.2(8) . . ? C13 C12 S11 125.0(6) . . ? C13 C12 C17 119.3(7) . . ? C17 C12 S11 115.7(6) . . ? C14 C13 C12 122.1(8) . . ? C13 C14 C15 120.9(8) . . ? C14 C15 C16 116.8(8) . . ? C14 C15 C18 123.0(8) . . ? C16 C15 C18 120.2(7) . . ? C17 C16 C15 122.3(8) . . ? C16 C17 C12 118.5(8) . . ? O19 C18 C15 115.5(7) . . ? O20 C18 O19 125.9(8) 2_456 . ? O20 C18 C15 118.6(8) 2_456 . ? O21 C23 C24 117.7(8) 2_556 . ? O22 C23 O21 124.5(9) . 2_556 ? O22 C23 C24 117.2(7) . . ? C25 C24 C23 120.1(9) . . ? C29 C24 C23 122.6(7) . . ? C29 C24 C25 117.2(9) . . ? C26 C25 C24 120.6(10) . . ? C25 C26 C27 120.6(10) . . ? C26 C27 S30 113.1(7) . . ? C28 C27 S30 127.4(9) . . ? C28 C27 C26 119.5(10) . . ? C27 C28 C29 118.5(10) . . ? C24 C29 C28 123.6(8) . . ? C33 C32 S31 126.0(9) . . ? C33 C32 C37 119.7(10) . . ? C37 C32 S31 114.3(8) . . ? C32 C33 C34 122.4(10) . . ? C33 C34 C35 119.7(9) . . ? C34 C35 C38 121.0(8) . . ? C36 C35 C34 119.3(9) . . ? C36 C35 C38 119.4(9) . . ? C35 C36 C37 118.9(9) . . ? C32 C37 C36 119.9(9) . . ? O39 C38 C35 116.9(8) . . ? O40 C38 O39 126.8(8) . . ? O40 C38 C35 116.2(8) . . ? O41 C43 C44 117.3(7) . . ? O42 C43 O41 125.1(8) . . ? O42 C43 C44 117.6(8) . . ? C45 C44 C43 120.7(8) . . ? C49 C44 C43 120.2(8) . . ? C49 C44 C45 119.0(8) . . ? C46 C45 C44 118.2(9) . . ? C47 C46 C45 122.1(8) . . ? C46 C47 S50 122.2(6) . . ? C48 C47 S50 118.2(7) . . ? C48 C47 C46 119.6(8) . . ? C47 C48 C49 120.9(9) . . ? C44 C49 C48 120.1(8) . . ? C53 C52 S51 117.2(7) . . ? C53 C52 C57 119.2(9) . . ? C57 C52 S51 123.6(7) . . ? C52 C53 C54 121.3(9) . . ? C55 C54 C53 120.6(9) . . ? C54 C55 C56 118.5(8) . . ? C54 C55 C58 121.0(8) . . ? C56 C55 C58 120.3(8) . . ? C57 C56 C55 119.7(8) . . ? C56 C57 C52 120.7(8) . . ? O59 C58 C55 116.6(7) . . ? O60 C58 O59 127.7(8) . . ? O60 C58 C55 115.7(8) . . ? N61 C62 C63 123.1(11) . . ? C64 C63 C62 113.4(11) . . ? C65 C64 C63 123.1(10) . . ? C64 C65 C66 117.3(11) . . ? N61 C66 C65 123.1(11) . . ? N71 C72 C73 123.5(14) . . ? C74 C73 C72 119.3(16) . . ? C73 C74 C75 120.0(11) . . ? C76 C75 C74 118.0(16) . . ? N71 C76 C75 123.1(16) . . ? N81 C82 C83 121.9(14) . . ? C84 C83 C82 123.7(15) . . ? C83 C84 C85 110.5(12) . . ? C86 C85 C84 123.9(13) . . ? N81 C86 C85 121.6(13) . . ? 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 Cu3 2.635(2) 2_456 ? Cu1 O19 1.975(6) . ? Cu1 O40 1.971(6) 2_456 ? Cu1 O42 1.990(5) 2_456 ? Cu1 O60 1.964(6) . ? Cu1 N61 2.164(7) . ? Cu2 Cu2 2.645(2) 2_556 ? Cu2 O1 1.968(6) . ? Cu2 O2 1.963(6) . ? Cu2 O21 1.950(6) . ? Cu2 O22 1.970(7) . ? Cu2 N71 2.173(7) . ? Cu3 O20 1.978(5) . ? Cu3 O39 1.971(6) . ? Cu3 O41 1.998(6) . ? Cu3 O59 1.954(6) 2_456 ? Cu3 N81 2.182(7) . ? S10 S11 2.024(3) . ? S10 C7 1.749(9) . ? S11 C12 1.784(8) . ? S30 S31 2.015(5) . ? S30 C27 1.786(11) . ? S31 C32 1.794(10) . ? S50 S51 2.036(4) 1_443 ? S50 C47 1.789(8) . ? S51 C52 1.779(9) . ? O1 C3 1.219(9) . ? O1S C2S 1.255(16) . ? O2 C3 1.294(9) 2_556 ? O19 C18 1.282(10) . ? O20 C18 1.241(9) 2_456 ? O21 C23 1.263(9) 2_556 ? O22 C23 1.231(10) . ? O39 C38 1.283(10) . ? O40 C38 1.260(10) . ? O41 C43 1.279(10) . ? O42 C43 1.270(9) . ? O59 C58 1.256(10) . ? O60 C58 1.242(9) . ? N3S C2S 1.41(3) . ? N3S C5S 1.38(2) . ? N3S C6S 1.60(3) . ? N61 C62 1.273(12) . ? N61 C66 1.324(12) . ? N71 C72 1.312(14) . ? N71 C76 1.321(13) . ? N81 C82 1.300(15) . ? N81 C86 1.291(13) . ? C3 C4 1.497(11) . ? C4 C5 1.396(11) . ? C4 C9 1.349(11) . ? C5 C6 1.380(12) . ? C6 C7 1.391(11) . ? C7 C8 1.457(11) . ? C8 C9 1.376(11) . ? C12 C13 1.368(11) . ? C12 C17 1.425(10) . ? C13 C14 1.361(11) . ? C14 C15 1.408(10) . ? C15 C16 1.420(12) . ? C15 C18 1.471(12) . ? C16 C17 1.372(11) . ? C23 C24 1.480(12) . ? C24 C25 1.410(11) . ? C24 C29 1.356(12) . ? C25 C26 1.345(14) . ? C26 C27 1.418(15) . ? C27 C28 1.353(12) . ? C28 C29 1.390(12) . ? C32 C33 1.322(13) . ? C32 C37 1.364(14) . ? C33 C34 1.360(12) . ? C34 C35 1.383(12) . ? C35 C36 1.365(12) . ? C35 C38 1.508(12) . ? C36 C37 1.414(10) . ? C43 C44 1.484(11) . ? C44 C45 1.411(11) . ? C44 C49 1.383(12) . ? C45 C46 1.394(12) . ? C46 C47 1.358(13) . ? C47 C48 1.354(12) . ? C48 C49 1.393(12) . ? C52 C53 1.361(12) . ? C52 C57 1.394(12) . ? C53 C54 1.389(13) . ? C54 C55 1.378(12) . ? C55 C56 1.421(11) . ? C55 C58 1.516(12) . ? C56 C57 1.381(12) . ? C62 C63 1.478(14) . ? C63 C64 1.366(15) . ? C64 C65 1.355(16) . ? C65 C66 1.376(14) . ? C72 C73 1.372(15) . ? C73 C74 1.27(2) . ? C74 C75 1.37(2) . ? C75 C76 1.350(16) . ? C82 C83 1.407(18) . ? C83 C84 1.311(15) . ? C84 C85 1.39(2) . ? C85 C86 1.369(16) . ? loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.797 -0.895 -0.743 1705.9 369.4 '12 DMF'