#------------------------------------------------------------------------------ #$Date: 2021-06-08 06:44:06 +0300 (Tue, 08 Jun 2021) $ #$Revision: 266250 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/06/07/7060709.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_7060709 loop_ _publ_author_name 'Liu, Meiying' 'Liang, Jingjing' 'Liu, Zhiliang' _publ_section_title ; Modulating the Ferroelectric Performance by Altering Halogen Anions in Crystals of Tetranuclear Copper-Clusters ; _journal_name_full 'New Journal of Chemistry' _journal_paper_doi 10.1039/D1NJ01894A _journal_year 2021 _chemical_absolute_configuration ad _chemical_formula_moiety 'C68.712 H75.424 Cu4 N4 O14, 2(Br)' _chemical_formula_sum 'C68.71 H75.43 Br2 Cu4 N4 O14' _chemical_formula_weight 1595.25 _space_group_crystal_system monoclinic _space_group_IT_number 4 _space_group_name_Hall 'P 2yb' _space_group_name_H-M_alt 'P 1 21 1' _atom_sites_solution_hydrogens mixed _audit_creation_date 2021-05-15 _audit_creation_method ; Olex2 1.3 (compiled 2020.07.31 svn.rc2a77460 for OlexSys, GUI svn.r6145) ; _audit_update_record ; 2021-05-17 deposited with the CCDC. 2021-06-04 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 93.987(2) _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 10.2904(5) _cell_length_b 21.3262(9) _cell_length_c 15.8441(7) _cell_measurement_reflns_used 9630 _cell_measurement_temperature 273(2) _cell_measurement_theta_max 26.22 _cell_measurement_theta_min 2.98 _cell_volume 3468.7(3) _computing_cell_refinement 'Bruker SAINT' _computing_data_collection 'Bruker APEX2' _computing_data_reduction 'Bruker SAINT' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 273.01 _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0335 _diffrn_reflns_av_unetI/netI 0.0314 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_number 86122 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.500 _diffrn_reflns_theta_min 2.749 _diffrn_source_current 30.0 _diffrn_source_power 1.5 _diffrn_source_voltage 50.0 _exptl_absorpt_coefficient_mu 2.427 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.6234 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2014/5 (Bruker,2014/5) was used for absorption correction. wR2(int) was 0.0736 before and 0.0642 after correction. The Ratio of minimum to maximum transmission is 0.8363. The \l/2 correction factor is Not present. ; _exptl_crystal_colour green _exptl_crystal_colour_primary green _exptl_crystal_density_diffrn 1.527 _exptl_crystal_description block _exptl_crystal_F_000 1627 _exptl_crystal_size_max 0.09 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _refine_diff_density_max 0.371 _refine_diff_density_min -0.240 _refine_diff_density_rms 0.046 _refine_ls_abs_structure_details ; Flack x determined using 5043 quotients [(I+)-(I-)]/[(I+)+(I-)] (Parsons and Flack (2004), Acta Cryst. A60, s61). ; _refine_ls_abs_structure_Flack 0.010(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.072 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 881 _refine_ls_number_reflns 12882 _refine_ls_number_restraints 16 _refine_ls_restrained_S_all 1.076 _refine_ls_R_factor_all 0.0408 _refine_ls_R_factor_gt 0.0307 _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^)+(0.0311P)^2^+1.2355P] where P=(Fo^2^+2Fc^2^)/3 ; _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0681 _refine_ls_wR_factor_ref 0.0723 _reflns_Friedel_coverage 0.942 _reflns_Friedel_fraction_full 0.997 _reflns_Friedel_fraction_max 0.997 _reflns_number_gt 11288 _reflns_number_total 12882 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1nj01894a2.cif _cod_data_source_block mo_171017e_0m _cod_database_code 7060709 _shelxl_version_number 2013-2 _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 0.868 _shelx_estimated_absorpt_t_min 0.811 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H) groups, All O(H,H) groups 2. Restrained distances O9-H9 0.85 with sigma of 0.01 O3-H3A 0.85 with sigma of 0.01 O13B-H13B 0.85 with sigma of 0.01 O13A-H13C = O13A-H13A 0.85 with sigma of 0.02 H13A-O5 1 with sigma of 0.1 C17-H9 1.922206 with sigma of 0.02 Cu1-H9 2.731233 with sigma of 0.02 C68-H3A 1.933862 with sigma of 0.02 Cu4-H3A 2.683168 with sigma of 0.02 Cu4-H13B 2.655452 with sigma of 0.02 C69-H13B 1.847995 with sigma of 0.02 H13C-H13A 1.34 with sigma of 0.04 Cu4-H13C \\sim Cu4-H13A with sigma of 0.02 3. Rigid bond restraints O13B, C69 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.0005 4. Others Sof(Br3)=Sof(Br4)=Sof(O13A)=Sof(H13A)=Sof(H13C)=1-FVAR(1) Sof(Br2)=Sof(Br1)=Sof(O13B)=Sof(H13B)=Sof(C69)=Sof(H69A)=Sof(H69B)=Sof(H69C)= FVAR(1) 5.a Riding coordinates: O13A(H13A,H13C) 5.b Rotating group: O14(H14A,H14B) 5.c Ternary CH refined with riding coordinates: C33(H33), C16(H16), C50(H50), C67(H67) 5.d Secondary CH2 refined with riding coordinates: C32(H32A,H32B), C15(H15A,H15B), C51(H51A,H51B), C17(H17A,H17B), C34(H34A, H34B), C66(H66A,H66B), C49(H49A,H49B), C68(H68A,H68B) 5.e Aromatic/amide H refined with riding coordinates: C3(H3), C8(H8), C25(H25), C5(H5), C4(H4), C39(H39), C22(H22), C44(H44), C55(H55), C56(H56), C42(H42), C21(H21), C54(H54), C47(H47), C45(H45), C26(H26), C43(H43), C20(H20), C37(H37), C12(H12), C9(H9A), C38(H38), C13(H13), C46(H46), C64(H64), C60(H60), C61(H61), C30(H30), C11(H11), C62(H62), C10(H10), C29(H29), C63(H63), C59(H59), C27(H27), C28(H28) 5.f Idealised Me refined as rotating group: C1(H1A,H1B,H1C), C18(H18A,H18B,H18C), C52(H52A,H52B,H52C), C35(H35A,H35B, H35C), C69(H69A,H69B,H69C) ; _shelx_res_file ; TITL mo_171017e_0m in P21 #4 REM reset to P21 #4 CELL 0.71073 10.2904 21.3262 15.8441 90 93.9869 90 ZERR 2 0.0005 0.0009 0.0007 0 0.0021 0 LATT -1 SYMM -X,0.5+Y,-Z SFAC C H Br Cu N O DISP Br -0.2901 2.4595 DISP C 0.0033 0.0016 DISP Cu 0.3201 1.2651 DISP H 0 0 DISP N 0.0061 0.0033 DISP O 0.0106 0.006 UNIT 137.42 150.85 4 8 8 28 DFIX 0.85 0.01 O9 H9 DFIX 0.85 0.01 O3 H3a DANG 1.922206 0.02 C17 H9 DANG 2.731233 0.02 Cu1 H9 DANG 1.933862 0.02 C68 H3a DANG 2.683168 0.02 Cu4 H3a DELU 0.001 0.0005 O13B C69 DANG 2.655452 0.02 Cu4 H13B DANG 1.847995 0.02 C69 H13B DFIX 0.85 0.01 O13B H13B DANG 1.34 H13c H13a SADI Cu4 H13c Cu4 H13a DFIX 0.85 O13A H13c O13A H13a DFIX 1 0.1 H13a O5 L.S. 10 PLAN 10 SIZE 0.09 0.08 0.06 TEMP -0.14 CONF HTAB O14 O11 HTAB O13B O5 HTAB O13A O5 MORE -1 BOND $H fmap 2 acta OMIT -3 51 REM REM REM > REM REM > REM > REM REM WGHT 0.031100 1.235500 FVAR 0.44236 0.71176 CU3 4 0.146446 0.011159 0.792098 11.00000 0.05123 0.02977 = 0.03654 -0.00412 -0.01074 0.00326 CU1 4 -0.038227 0.002060 0.601641 11.00000 0.04553 0.03366 = 0.03428 -0.00302 -0.00721 -0.00286 CU2 4 -0.171363 0.017062 0.774255 11.00000 0.05028 0.03692 = 0.03783 -0.00533 -0.00334 0.00666 CU4 4 0.008378 -0.123009 0.799767 11.00000 0.05846 0.03080 = 0.04004 0.00272 -0.00098 0.00212 O2 6 0.131326 -0.074521 0.739335 11.00000 0.05199 0.02970 = 0.04507 -0.00679 0.00343 -0.00022 O11 6 -0.267897 0.082283 0.714415 11.00000 0.05416 0.04297 = 0.05279 -0.00689 -0.01041 0.01377 C33 1 -0.090687 0.031518 0.947843 11.00000 0.05730 0.05971 = 0.03278 -0.00917 0.00020 0.01285 AFIX 13 H33 2 -0.004786 0.050066 0.941482 11.00000 -1.20000 AFIX 0 N2 5 0.168554 0.097548 0.829496 11.00000 0.05287 0.03129 = 0.04551 -0.00522 -0.01312 0.00062 O8 6 -0.167860 -0.034409 0.668809 11.00000 0.05264 0.03694 = 0.03958 -0.01049 0.00295 -0.00847 N1 5 0.048612 -0.199138 0.738412 11.00000 0.06321 0.02699 = 0.04565 -0.00374 -0.01359 0.00294 O7 6 -0.345952 -0.060743 0.772048 11.00000 0.05639 0.05821 = 0.06296 -0.00775 0.01690 -0.00599 O1 6 0.307928 0.003737 0.693029 11.00000 0.05523 0.04924 = 0.06260 -0.00475 0.00452 -0.01179 O10 6 -0.401801 0.153598 0.608193 11.00000 0.07442 0.05755 = 0.06661 0.00829 -0.01689 0.01399 C24 1 -0.333216 0.127351 0.747278 11.00000 0.03963 0.03950 = 0.05867 -0.00314 -0.00956 -0.00395 C19 1 -0.411897 0.167346 0.691331 11.00000 0.05299 0.04080 = 0.06622 0.00199 -0.00389 -0.00099 C3 1 -0.397824 -0.159074 0.699037 11.00000 0.04796 0.05985 = 0.06575 0.01071 -0.00175 -0.00770 AFIX 43 H3 2 -0.459540 -0.169783 0.736731 11.00000 -1.20000 AFIX 0 C2 1 -0.330112 -0.103841 0.709923 11.00000 0.04956 0.04511 = 0.04468 -0.00027 -0.00625 0.00530 C7 1 -0.235431 -0.086883 0.654730 11.00000 0.04062 0.03720 = 0.04106 -0.00151 -0.00915 0.00167 C8 1 -0.137334 -0.109713 0.517321 11.00000 0.05519 0.03739 = 0.04037 -0.01087 -0.01016 0.00580 AFIX 43 H8 2 -0.135827 -0.137759 0.472452 11.00000 -1.20000 AFIX 0 N4 5 -0.069632 -0.059519 0.512772 11.00000 0.04900 0.03643 = 0.03621 -0.00495 -0.00610 0.00499 C16 1 -0.012343 -0.043660 0.433033 11.00000 0.04961 0.04996 = 0.03850 -0.00806 -0.00129 0.00092 AFIX 13 H16 2 0.006208 -0.082513 0.403107 11.00000 -1.20000 AFIX 0 C58 1 0.207362 -0.093620 0.680905 11.00000 0.04218 0.03722 = 0.03308 -0.00260 -0.01073 0.00676 C57 1 0.200359 -0.154579 0.645623 11.00000 0.05835 0.03456 = 0.03836 -0.00324 -0.00735 0.00915 O9 6 0.099331 0.032446 0.526168 11.00000 0.05529 0.05187 = 0.04480 0.00067 -0.00678 -0.00892 H9 2 0.117023 0.069556 0.509394 11.00000 -1.50000 C32 1 -0.122544 0.041929 1.040076 11.00000 0.06751 0.10116 = 0.04359 -0.01474 0.00212 0.02017 AFIX 23 H32A 2 -0.139773 0.086063 1.049024 11.00000 -1.20000 H32B 2 -0.200435 0.018593 1.051210 11.00000 -1.20000 AFIX 0 C53 1 0.301779 -0.052285 0.651671 11.00000 0.04118 0.04656 = 0.04227 -0.00063 -0.00582 0.00692 C15 1 -0.107529 -0.004364 0.377418 11.00000 0.05109 0.05183 = 0.04098 -0.00123 -0.00658 -0.00075 AFIX 23 H15A 2 -0.126303 0.033995 0.407138 11.00000 -1.20000 H15B 2 -0.066811 0.007123 0.326219 11.00000 -1.20000 AFIX 0 N3 5 -0.180954 0.059716 0.882649 11.00000 0.05267 0.04447 = 0.04319 -0.00713 -0.00352 0.00866 C25 1 -0.254355 0.105976 0.896647 11.00000 0.06936 0.04682 = 0.04862 -0.01544 0.00514 0.00641 AFIX 43 H25 2 -0.256438 0.119096 0.952515 11.00000 -1.20000 AFIX 0 C5 1 -0.287110 -0.183597 0.576831 11.00000 0.07139 0.03995 = 0.06005 -0.00607 -0.00845 -0.01183 AFIX 43 H5 2 -0.273051 -0.210531 0.532210 11.00000 -1.20000 AFIX 0 O5 6 0.249382 -0.021330 0.886876 11.00000 0.06822 0.04109 = 0.04487 -0.00220 -0.01709 0.00901 C41 1 0.323795 0.010999 0.940856 11.00000 0.04861 0.05815 = 0.03432 -0.00538 -0.00663 0.00957 C1 1 -0.433383 -0.076067 0.835473 11.00000 0.07474 0.08794 = 0.07198 -0.00289 0.02002 0.00360 AFIX 137 H1A 2 -0.518370 -0.084426 0.808995 11.00000 -1.50000 H1B 2 -0.438299 -0.041493 0.873922 11.00000 -1.50000 H1C 2 -0.402075 -0.112551 0.866009 11.00000 -1.50000 AFIX 0 C40 1 0.328285 0.076769 0.945372 11.00000 0.05467 0.05862 = 0.03895 -0.00915 -0.00755 0.00217 C4 1 -0.375518 -0.198955 0.632852 11.00000 0.07027 0.04442 = 0.07533 -0.00473 -0.01075 -0.01958 AFIX 43 H4 2 -0.421338 -0.236455 0.626747 11.00000 -1.20000 AFIX 0 O6 6 0.025324 0.046321 0.702974 11.00000 0.05214 0.02960 = 0.03711 -0.00099 -0.01194 -0.00177 O12 6 -0.056414 -0.043207 0.838268 11.00000 0.06722 0.03866 = 0.03200 0.00080 0.00225 0.00874 C51 1 0.054164 0.110919 0.694492 11.00000 0.06539 0.02846 = 0.04955 0.00376 -0.01436 -0.00350 AFIX 23 H51A 2 -0.018709 0.131886 0.664325 11.00000 -1.20000 H51B 2 0.129900 0.115747 0.661885 11.00000 -1.20000 AFIX 0 O14 6 -0.182396 0.077074 0.549974 11.00000 0.07687 0.06709 = 0.05728 -0.00595 -0.01390 0.01955 AFIX 7 H14A 2 -0.142026 0.112925 0.534458 11.00000 -1.50000 H14B 2 -0.233511 0.091761 0.590303 11.00000 -1.50000 AFIX 0 C17 1 0.114110 -0.010031 0.455891 11.00000 0.04690 0.06283 = 0.04946 -0.00173 -0.00053 0.00527 AFIX 23 H17A 2 0.181808 -0.040408 0.471295 11.00000 -1.20000 H17B 2 0.140067 0.013418 0.407373 11.00000 -1.20000 AFIX 0 C50 1 0.080352 0.140468 0.779783 11.00000 0.04910 0.03085 = 0.05027 -0.00552 -0.00963 -0.00008 AFIX 13 H50 2 -0.002397 0.140751 0.806887 11.00000 -1.20000 AFIX 0 O3 6 -0.127059 -0.178172 0.845191 11.00000 0.07861 0.05352 = 0.06352 0.01139 0.01478 -0.00640 H3A 2 -0.149679 -0.182796 0.896192 11.00000 -1.50000 C23 1 -0.333976 0.139724 0.834634 11.00000 0.05855 0.03855 = 0.06403 -0.00348 0.00104 0.00687 C39 1 0.413202 0.106162 1.007317 11.00000 0.08294 0.07475 = 0.05623 -0.01052 -0.02236 -0.01121 AFIX 43 H39 2 0.414593 0.149663 1.011398 11.00000 -1.20000 AFIX 0 C22 1 -0.412881 0.188705 0.863452 11.00000 0.08475 0.04973 = 0.07267 -0.00747 0.00959 0.01362 AFIX 43 H22 2 -0.412674 0.196853 0.921125 11.00000 -1.20000 AFIX 0 C44 1 -0.191972 0.296707 0.734029 11.00000 0.07987 0.06642 = 0.13022 0.00262 0.00420 0.01182 AFIX 43 H44 2 -0.263038 0.308042 0.763872 11.00000 -1.20000 AFIX 0 C55 1 0.368552 -0.127903 0.551586 11.00000 0.06037 0.07930 = 0.05581 -0.00806 0.00739 0.02375 AFIX 43 H55 2 0.419318 -0.138531 0.507415 11.00000 -1.20000 AFIX 0 C56 1 0.281902 -0.170274 0.580521 11.00000 0.06797 0.05554 = 0.05545 -0.01307 -0.00527 0.01872 AFIX 43 H56 2 0.276614 -0.210177 0.556853 11.00000 -1.20000 AFIX 0 C42 1 0.246721 0.116306 0.891277 11.00000 0.06334 0.04137 = 0.04592 -0.00957 -0.01038 -0.00414 AFIX 43 H42 2 0.250565 0.159207 0.901680 11.00000 -1.20000 AFIX 0 C31 1 -0.011256 0.020981 1.100616 11.00000 0.08797 0.09165 = 0.03381 -0.01282 0.00891 0.04204 C48 1 0.016529 0.247365 0.732065 11.00000 0.06602 0.02711 = 0.07178 -0.00401 -0.01833 -0.00603 C21 1 -0.488735 0.223908 0.808231 11.00000 0.07761 0.04936 = 0.10311 -0.00624 0.01047 0.02301 AFIX 43 H21 2 -0.541384 0.255280 0.828182 11.00000 -1.20000 AFIX 0 C34 1 -0.080864 -0.037980 0.925642 11.00000 0.07622 0.05414 = 0.03650 0.00132 0.00931 0.01310 AFIX 23 H34A 2 -0.010635 -0.057386 0.960362 11.00000 -1.20000 H34B 2 -0.161482 -0.059214 0.936248 11.00000 -1.20000 AFIX 0 C54 1 0.379934 -0.069331 0.588482 11.00000 0.03995 0.07121 = 0.05797 0.00773 -0.00136 0.00275 AFIX 43 H54 2 0.441067 -0.041102 0.570437 11.00000 -1.20000 AFIX 0 C47 1 0.015807 0.262578 0.648606 11.00000 0.06769 0.04798 = 0.08830 0.00793 -0.01211 -0.00979 AFIX 43 H47 2 0.086455 0.251572 0.618171 11.00000 -1.20000 AFIX 0 C45 1 -0.191420 0.310844 0.652156 11.00000 0.06963 0.05609 = 0.12208 0.01639 -0.03168 0.00042 AFIX 43 H45 2 -0.261641 0.332086 0.625366 11.00000 -1.20000 AFIX 0 C6 1 -0.215411 -0.126465 0.585709 11.00000 0.04835 0.03548 = 0.04869 -0.00264 -0.00081 -0.00059 C26 1 0.094521 0.058293 1.115185 11.00000 0.07663 0.13378 = 0.08029 -0.04176 -0.02156 0.03639 AFIX 43 H26 2 0.098706 0.097102 1.088742 11.00000 -1.20000 AFIX 0 C67 1 -0.011884 -0.256159 0.770449 11.00000 0.06993 0.03029 = 0.06502 0.00187 -0.01103 -0.00404 AFIX 13 H67 2 -0.026877 -0.286106 0.723875 11.00000 -1.20000 AFIX 0 C43 1 -0.086562 0.264871 0.775977 11.00000 0.08449 0.05262 = 0.08996 -0.00451 -0.00249 0.01031 AFIX 43 H43 2 -0.087333 0.255845 0.833366 11.00000 -1.20000 AFIX 0 C65 1 0.214496 -0.301780 0.813124 11.00000 0.08823 0.04219 = 0.07790 0.01942 -0.01358 0.00814 C14 1 -0.233326 -0.037846 0.353658 11.00000 0.06135 0.06562 = 0.04036 0.01081 -0.01625 -0.00440 C20 1 -0.487522 0.212964 0.721921 11.00000 0.06436 0.04016 = 0.09877 0.00463 -0.01044 0.01232 AFIX 43 H20 2 -0.539474 0.237339 0.684419 11.00000 -1.20000 AFIX 0 C66 1 0.082361 -0.285922 0.840164 11.00000 0.08464 0.04057 = 0.07744 0.01945 -0.00252 -0.00493 AFIX 23 H66A 2 0.092233 -0.257069 0.887503 11.00000 -1.20000 H66B 2 0.042683 -0.323894 0.860165 11.00000 -1.20000 AFIX 0 C18 1 -0.473007 0.190908 0.546618 11.00000 0.11649 0.08275 = 0.08442 0.02292 -0.02486 0.02106 AFIX 137 H18A 2 -0.444384 0.181736 0.491564 11.00000 -1.50000 H18B 2 -0.458482 0.234479 0.559240 11.00000 -1.50000 H18C 2 -0.564220 0.181695 0.547484 11.00000 -1.50000 AFIX 0 O4 6 0.391951 -0.086134 0.993734 11.00000 0.10273 0.06889 = 0.05623 0.00504 -0.02660 0.02527 C37 1 0.488188 0.006948 1.058810 11.00000 0.07835 0.10506 = 0.04575 -0.00476 -0.02274 0.02403 AFIX 43 H37 2 0.541656 -0.016286 1.096822 11.00000 -1.20000 AFIX 0 C36 1 0.405665 -0.023044 1.001292 11.00000 0.06219 0.07321 = 0.04018 -0.00289 -0.00610 0.02335 C52 1 0.399554 0.048517 0.668473 11.00000 0.07366 0.05926 = 0.12461 -0.00237 0.01788 -0.02146 AFIX 137 H52A 2 0.379814 0.059878 0.610365 11.00000 -1.50000 H52B 2 0.485531 0.030916 0.674960 11.00000 -1.50000 H52C 2 0.395460 0.085129 0.703440 11.00000 -1.50000 AFIX 0 C49 1 0.125053 0.208907 0.774590 11.00000 0.06502 0.03467 = 0.07058 -0.00405 -0.01962 -0.00295 AFIX 23 H49A 2 0.147356 0.225008 0.831001 11.00000 -1.20000 H49B 2 0.201789 0.211480 0.742500 11.00000 -1.20000 AFIX 0 C12 1 -0.348533 -0.118765 0.274084 11.00000 0.12677 0.10034 = 0.09919 0.00228 -0.04461 -0.04862 AFIX 43 H12 2 -0.348045 -0.151486 0.235306 11.00000 -1.20000 AFIX 0 C9 1 -0.345485 -0.022352 0.390103 11.00000 0.06467 0.10978 = 0.06263 0.01315 -0.00373 -0.00712 AFIX 43 H9A 2 -0.345251 0.009725 0.429877 11.00000 -1.20000 AFIX 0 C38 1 0.493012 0.071225 1.061077 11.00000 0.08698 0.10457 = 0.05638 -0.01214 -0.03560 -0.00873 AFIX 43 H38 2 0.551359 0.091168 1.099708 11.00000 -1.20000 AFIX 0 C13 1 -0.236381 -0.086815 0.296423 11.00000 0.09477 0.07957 = 0.06238 -0.00250 -0.02149 -0.02407 AFIX 43 H13 2 -0.159932 -0.098327 0.272456 11.00000 -1.20000 AFIX 0 C35 1 0.465010 -0.124415 1.054726 11.00000 0.18905 0.09783 = 0.10311 0.01606 -0.06550 0.05718 AFIX 137 H35A 2 0.441071 -0.167580 1.046228 11.00000 -1.50000 H35B 2 0.446348 -0.111763 1.110761 11.00000 -1.50000 H35C 2 0.556424 -0.119479 1.047941 11.00000 -1.50000 AFIX 0 C46 1 -0.089160 0.294404 0.607994 11.00000 0.08812 0.05798 = 0.09167 0.01886 -0.03331 -0.01417 AFIX 43 H46 2 -0.088713 0.304242 0.550831 11.00000 -1.20000 AFIX 0 C68 1 -0.139631 -0.238356 0.802624 11.00000 0.05912 0.04378 = 0.09033 0.01122 -0.00496 -0.01273 AFIX 23 H68A 2 -0.205447 -0.235730 0.755866 11.00000 -1.20000 H68B 2 -0.166542 -0.270019 0.841754 11.00000 -1.20000 AFIX 0 C64 1 0.231945 -0.349055 0.755402 11.00000 0.11232 0.07256 = 0.10734 -0.00246 -0.02121 0.02194 AFIX 43 H64 2 0.161451 -0.373142 0.734666 11.00000 -1.20000 AFIX 0 C60 1 0.320798 -0.269132 0.843273 11.00000 0.08996 0.05490 = 0.11692 0.02312 -0.01356 -0.00003 AFIX 43 H60 2 0.311541 -0.237194 0.882370 11.00000 -1.20000 AFIX 0 C61 1 0.443510 -0.282762 0.816517 11.00000 0.09185 0.07940 = 0.17535 0.05458 -0.01130 -0.00411 AFIX 43 H61 2 0.514980 -0.260436 0.839696 11.00000 -1.20000 AFIX 0 C30 1 -0.016660 -0.034268 1.140254 11.00000 0.16199 0.12973 = 0.05404 0.01436 0.02251 0.05930 AFIX 43 H30 2 -0.090218 -0.059311 1.130789 11.00000 -1.20000 AFIX 0 C11 1 -0.460089 -0.102635 0.308545 11.00000 0.10683 0.14490 = 0.11119 0.04130 -0.04945 -0.06314 AFIX 43 H11 2 -0.536713 -0.123899 0.292377 11.00000 -1.20000 AFIX 0 C62 1 0.462326 -0.326821 0.758663 11.00000 0.12162 0.11676 = 0.15709 0.06507 0.02312 0.03882 AFIX 43 H62 2 0.544469 -0.334301 0.739757 11.00000 -1.20000 AFIX 0 C10 1 -0.462034 -0.055298 0.367106 11.00000 0.07498 0.14327 = 0.11143 0.03728 -0.00746 -0.01645 AFIX 43 H10 2 -0.538942 -0.044991 0.391380 11.00000 -1.20000 AFIX 0 C29 1 0.084783 -0.054850 1.194931 11.00000 0.24287 0.20575 = 0.06840 0.03765 0.01106 0.14588 AFIX 43 H29 2 0.080740 -0.093868 1.220830 11.00000 -1.20000 AFIX 0 C63 1 0.356031 -0.360464 0.728371 11.00000 0.15536 0.11311 = 0.10919 0.00338 0.01500 0.06506 AFIX 43 H63 2 0.366667 -0.391824 0.688652 11.00000 -1.20000 AFIX 0 C59 1 0.120548 -0.202715 0.676693 11.00000 0.06619 0.03403 = 0.04593 -0.00753 -0.01895 0.01090 AFIX 43 H59 2 0.121198 -0.241016 0.648662 11.00000 -1.20000 AFIX 0 PART 1 BR2 3 0.047303 0.166025 0.451710 21.00000 0.13703 0.06219 = 0.07469 0.02416 0.00271 -0.00061 BR1 3 -0.237838 -0.210320 1.015837 21.00000 0.12434 0.11102 = 0.09341 0.05360 0.03321 0.01344 PART 0 C27 1 0.197284 0.037551 1.170585 11.00000 0.09008 0.29997 = 0.09264 -0.07360 -0.02909 0.07673 AFIX 43 H27 2 0.270976 0.062580 1.179463 11.00000 -1.20000 AFIX 0 C28 1 0.192514 -0.016708 1.210708 11.00000 0.17750 0.36637 = 0.06086 -0.03078 -0.02611 0.19699 AFIX 43 H28 2 0.260454 -0.029017 1.248893 11.00000 -1.20000 AFIX 0 PART 2 BR3 3 0.135680 0.158100 0.449606 -21.00000 0.24975 0.07854 = 0.12389 0.03257 -0.00514 -0.05083 BR4 3 -0.161108 -0.202017 1.028024 -21.00000 0.20405 0.19933 = 0.08259 0.07535 -0.00893 -0.05635 PART 1 O13B 6 0.151061 -0.142717 0.913416 21.00000 0.10180 0.04534 = 0.08188 -0.01058 -0.03829 0.02238 H13B 2 0.198788 -0.110395 0.919153 21.00000 -1.50000 C69 1 0.140557 -0.159128 1.004836 21.00000 0.11573 0.11411 = 0.08207 -0.01279 -0.01871 0.03015 AFIX 137 H69A 2 0.052676 -0.171304 1.013537 21.00000 -1.50000 H69B 2 0.163842 -0.123344 1.039408 21.00000 -1.50000 H69C 2 0.198438 -0.193229 1.020019 21.00000 -1.50000 AFIX 0 PART 2 O13A 6 0.152613 -0.132824 0.919832 -21.00000 0.08785 0.05591 = 0.03634 0.01848 -0.00581 -0.00718 AFIX 3 H13A 2 0.208883 -0.098624 0.905202 -21.00000 -1.50000 H13C 2 0.207283 -0.162344 0.896182 -21.00000 -1.50000 AFIX 0 HKLF 4 REM mo_171017e_0m in P21 #4 REM R1 = 0.0307 for 11288 Fo > 4sig(Fo) and 0.0408 for all 12882 data REM 881 parameters refined using 16 restraints END WGHT 0.0311 1.2355 REM Highest difference peak 0.371, deepest hole -0.240, 1-sigma level 0.046 Q1 1 -0.1430 0.1788 0.4731 11.00000 0.05 0.37 Q2 1 -0.1851 -0.2402 0.9944 11.00000 0.05 0.34 Q3 1 0.6392 0.0028 0.5852 11.00000 0.05 0.32 Q4 1 0.2788 -0.0005 0.6222 11.00000 0.05 0.28 Q5 1 -0.3084 -0.1173 0.7857 11.00000 0.05 0.28 Q6 1 0.0500 -0.1596 0.7802 11.00000 0.05 0.27 Q7 1 -0.0627 -0.2464 1.0180 11.00000 0.05 0.24 Q8 1 -0.6741 -0.1277 0.8146 11.00000 0.05 0.23 Q9 1 -0.0850 -0.0063 0.7397 11.00000 0.05 0.22 Q10 1 -0.5317 0.0091 0.8172 11.00000 0.05 0.22 ; _shelx_res_checksum 73116 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -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 Cu3 Cu 0.14645(5) 0.01116(3) 0.79210(3) 0.03982(14) Uani 1 1 d . . . . . Cu1 Cu -0.03823(5) 0.00206(2) 0.60164(3) 0.03829(14) Uani 1 1 d D . . . . Cu2 Cu -0.17136(6) 0.01706(3) 0.77425(3) 0.04197(14) Uani 1 1 d . . . . . Cu4 Cu 0.00838(6) -0.12301(3) 0.79977(4) 0.04330(15) Uani 1 1 d D . . . . O2 O 0.1313(3) -0.07452(14) 0.7393(2) 0.0423(8) Uani 1 1 d . . . . . O11 O -0.2679(4) 0.08228(16) 0.7144(2) 0.0506(9) Uani 1 1 d . . . . . C33 C -0.0907(5) 0.0315(3) 0.9478(3) 0.0501(13) Uani 1 1 d . . . . . H33 H -0.0048 0.0501 0.9415 0.060 Uiso 1 1 calc R U . . . N2 N 0.1686(4) 0.09755(18) 0.8295(3) 0.0440(10) Uani 1 1 d . . . . . O8 O -0.1679(3) -0.03441(15) 0.6688(2) 0.0431(8) Uani 1 1 d . . . . . N1 N 0.0486(4) -0.19914(18) 0.7384(3) 0.0461(10) Uani 1 1 d . . . . . O7 O -0.3460(4) -0.06074(18) 0.7720(2) 0.0586(10) Uani 1 1 d . . . . . O1 O 0.3079(3) 0.00374(18) 0.6930(2) 0.0557(9) Uani 1 1 d . . . . . O10 O -0.4018(4) 0.15360(19) 0.6082(3) 0.0672(11) Uani 1 1 d . . . . . C24 C -0.3332(5) 0.1274(2) 0.7473(3) 0.0465(12) Uani 1 1 d . . . . . C19 C -0.4119(6) 0.1673(2) 0.6913(4) 0.0537(14) Uani 1 1 d . . . . . C3 C -0.3978(6) -0.1591(3) 0.6990(4) 0.0581(15) Uani 1 1 d . . . . . H3 H -0.4595 -0.1698 0.7367 0.070 Uiso 1 1 calc R U . . . C2 C -0.3301(5) -0.1038(2) 0.7099(3) 0.0469(12) Uani 1 1 d . . . . . C7 C -0.2354(5) -0.0869(2) 0.6547(3) 0.0402(11) Uani 1 1 d . . . . . C8 C -0.1373(5) -0.1097(2) 0.5173(3) 0.0449(12) Uani 1 1 d . . . . . H8 H -0.1358 -0.1378 0.4725 0.054 Uiso 1 1 calc R U . . . N4 N -0.0696(4) -0.05952(18) 0.5128(2) 0.0410(9) Uani 1 1 d . . . . . C16 C -0.0123(5) -0.0437(2) 0.4330(3) 0.0462(12) Uani 1 1 d . . . . . H16 H 0.0062 -0.0825 0.4031 0.055 Uiso 1 1 calc R U . . . C58 C 0.2074(5) -0.0936(2) 0.6809(3) 0.0381(11) Uani 1 1 d . . . . . C57 C 0.2004(5) -0.1546(2) 0.6456(3) 0.0443(12) Uani 1 1 d . . . . . O9 O 0.0993(3) 0.03245(16) 0.5262(2) 0.0511(9) Uani 1 1 d D . . . . H9 H 0.117(5) 0.0696(8) 0.509(3) 0.077 Uiso 1 1 d D U . . . C32 C -0.1225(6) 0.0419(4) 1.0401(3) 0.0708(18) Uani 1 1 d . . . . . H32A H -0.1398 0.0861 1.0490 0.085 Uiso 1 1 calc R U . . . H32B H -0.2004 0.0186 1.0512 0.085 Uiso 1 1 calc R U . . . C53 C 0.3018(5) -0.0523(2) 0.6517(3) 0.0437(12) Uani 1 1 d . . . . . C15 C -0.1075(5) -0.0044(2) 0.3774(3) 0.0484(12) Uani 1 1 d . . . . . H15A H -0.1263 0.0340 0.4071 0.058 Uiso 1 1 calc R U . . . H15B H -0.0668 0.0071 0.3262 0.058 Uiso 1 1 calc R U . . . N3 N -0.1810(4) 0.0597(2) 0.8826(3) 0.0471(10) Uani 1 1 d . . . . . C25 C -0.2544(6) 0.1060(3) 0.8966(3) 0.0549(14) Uani 1 1 d . . . . . H25 H -0.2564 0.1191 0.9525 0.066 Uiso 1 1 calc R U . . . C5 C -0.2871(6) -0.1836(2) 0.5768(4) 0.0577(14) Uani 1 1 d . . . . . H5 H -0.2731 -0.2105 0.5322 0.069 Uiso 1 1 calc R U . . . O5 O 0.2494(4) -0.02133(16) 0.8869(2) 0.0524(9) Uani 1 1 d D . . . . C41 C 0.3238(4) 0.0110(3) 0.9409(3) 0.0475(11) Uani 1 1 d . . . . . C1 C -0.4334(7) -0.0761(4) 0.8355(4) 0.0775(19) Uani 1 1 d . . . . . H1A H -0.5184 -0.0844 0.8090 0.116 Uiso 1 1 calc R U . . . H1B H -0.4383 -0.0415 0.8739 0.116 Uiso 1 1 calc R U . . . H1C H -0.4021 -0.1126 0.8660 0.116 Uiso 1 1 calc R U . . . C40 C 0.3283(5) 0.0768(3) 0.9454(3) 0.0512(13) Uani 1 1 d . . . . . C4 C -0.3755(6) -0.1990(3) 0.6329(4) 0.0641(16) Uani 1 1 d . . . . . H4 H -0.4213 -0.2365 0.6267 0.077 Uiso 1 1 calc R U . . . O6 O 0.0253(3) 0.04632(14) 0.70297(19) 0.0403(7) Uani 1 1 d . . . . . O12 O -0.0564(4) -0.04321(15) 0.8383(2) 0.0460(8) Uani 1 1 d . . . . . C51 C 0.0542(6) 0.1109(2) 0.6945(3) 0.0487(13) Uani 1 1 d . . . . . H51A H -0.0187 0.1319 0.6643 0.058 Uiso 1 1 calc R U . . . H51B H 0.1299 0.1157 0.6619 0.058 Uiso 1 1 calc R U . . . O14 O -0.1824(4) 0.0771(2) 0.5500(3) 0.0679(11) Uani 1 1 d . . . . . H14A H -0.1420 0.1129 0.5345 0.102 Uiso 1 1 d R U . . . H14B H -0.2335 0.0918 0.5903 0.102 Uiso 1 1 d R U . . . C17 C 0.1141(5) -0.0100(3) 0.4559(3) 0.0532(13) Uani 1 1 d D . . . . H17A H 0.1818 -0.0404 0.4713 0.064 Uiso 1 1 calc R U . . . H17B H 0.1401 0.0134 0.4074 0.064 Uiso 1 1 calc R U . . . C50 C 0.0804(5) 0.1405(2) 0.7798(3) 0.0440(11) Uani 1 1 d . . . . . H50 H -0.0024 0.1408 0.8069 0.053 Uiso 1 1 calc R U . . . O3 O -0.1271(4) -0.17817(19) 0.8452(3) 0.0648(11) Uani 1 1 d D . . . . H3A H -0.150(6) -0.1828(19) 0.8962(16) 0.097 Uiso 1 1 d D U . . . C23 C -0.3340(5) 0.1397(2) 0.8346(4) 0.0539(13) Uani 1 1 d . . . . . C39 C 0.4132(7) 0.1062(3) 1.0073(4) 0.0726(18) Uani 1 1 d . . . . . H39 H 0.4146 0.1497 1.0114 0.087 Uiso 1 1 calc R U . . . C22 C -0.4129(7) 0.1887(3) 0.8635(4) 0.0689(17) Uani 1 1 d . . . . . H22 H -0.4127 0.1969 0.9211 0.083 Uiso 1 1 calc R U . . . C44 C -0.1920(8) 0.2967(4) 0.7340(6) 0.092(2) Uani 1 1 d . . . . . H44 H -0.2630 0.3080 0.7639 0.111 Uiso 1 1 calc R U . . . C55 C 0.3686(6) -0.1279(3) 0.5516(4) 0.0650(16) Uani 1 1 d . . . . . H55 H 0.4193 -0.1385 0.5074 0.078 Uiso 1 1 calc R U . . . C56 C 0.2819(6) -0.1703(3) 0.5805(4) 0.0601(15) Uani 1 1 d . . . . . H56 H 0.2766 -0.2102 0.5569 0.072 Uiso 1 1 calc R U . . . C42 C 0.2467(5) 0.1163(2) 0.8913(3) 0.0509(13) Uani 1 1 d . . . . . H42 H 0.2506 0.1592 0.9017 0.061 Uiso 1 1 calc R U . . . C31 C -0.0113(7) 0.0210(4) 1.1006(3) 0.0709(19) Uani 1 1 d . . . . . C48 C 0.0165(6) 0.2474(2) 0.7321(4) 0.0560(15) Uani 1 1 d . . . . . C21 C -0.4887(7) 0.2239(3) 0.8082(5) 0.0765(19) Uani 1 1 d . . . . . H21 H -0.5414 0.2553 0.8282 0.092 Uiso 1 1 calc R U . . . C34 C -0.0809(6) -0.0380(3) 0.9256(3) 0.0554(14) Uani 1 1 d . . . . . H34A H -0.0106 -0.0574 0.9604 0.066 Uiso 1 1 calc R U . . . H34B H -0.1615 -0.0592 0.9362 0.066 Uiso 1 1 calc R U . . . C54 C 0.3799(5) -0.0693(3) 0.5885(4) 0.0566(14) Uani 1 1 d . . . . . H54 H 0.4411 -0.0411 0.5704 0.068 Uiso 1 1 calc R U . . . C47 C 0.0158(6) 0.2626(3) 0.6486(4) 0.0688(17) Uani 1 1 d . . . . . H47 H 0.0865 0.2516 0.6182 0.083 Uiso 1 1 calc R U . . . C45 C -0.1914(8) 0.3108(3) 0.6522(6) 0.084(2) Uani 1 1 d . . . . . H45 H -0.2616 0.3321 0.6254 0.101 Uiso 1 1 calc R U . . . C6 C -0.2154(5) -0.1265(2) 0.5857(3) 0.0444(11) Uani 1 1 d . . . . . C26 C 0.0945(8) 0.0583(5) 1.1152(5) 0.098(3) Uani 1 1 d . . . . . H26 H 0.0987 0.0971 1.0887 0.118 Uiso 1 1 calc R U . . . C67 C -0.0119(6) -0.2562(2) 0.7704(4) 0.0558(14) Uani 1 1 d . . . . . H67 H -0.0269 -0.2861 0.7239 0.067 Uiso 1 1 calc R U . . . C43 C -0.0866(7) 0.2649(3) 0.7760(5) 0.0761(19) Uani 1 1 d . . . . . H43 H -0.0873 0.2558 0.8334 0.091 Uiso 1 1 calc R U . . . C65 C 0.2145(7) -0.3018(3) 0.8131(4) 0.0703(18) Uani 1 1 d . . . . . C14 C -0.2333(6) -0.0378(3) 0.3537(3) 0.0567(14) Uani 1 1 d . . . . . C20 C -0.4875(6) 0.2130(3) 0.7219(5) 0.0685(18) Uani 1 1 d . . . . . H20 H -0.5395 0.2373 0.6844 0.082 Uiso 1 1 calc R U . . . C66 C 0.0824(6) -0.2859(3) 0.8402(4) 0.0679(17) Uani 1 1 d . . . . . H66A H 0.0922 -0.2571 0.8875 0.082 Uiso 1 1 calc R U . . . H66B H 0.0427 -0.3239 0.8602 0.082 Uiso 1 1 calc R U . . . C18 C -0.4730(8) 0.1909(4) 0.5466(5) 0.096(2) Uani 1 1 d . . . . . H18A H -0.4444 0.1817 0.4916 0.144 Uiso 1 1 calc R U . . . H18B H -0.4585 0.2345 0.5592 0.144 Uiso 1 1 calc R U . . . H18C H -0.5642 0.1817 0.5475 0.144 Uiso 1 1 calc R U . . . O4 O 0.3920(5) -0.0861(2) 0.9937(3) 0.0774(13) Uani 1 1 d . . . . . C37 C 0.4882(6) 0.0069(4) 1.0588(3) 0.0776(19) Uani 1 1 d . . . . . H37 H 0.5417 -0.0163 1.0968 0.093 Uiso 1 1 calc R U . . . C36 C 0.4057(6) -0.0230(3) 1.0013(3) 0.0590(15) Uani 1 1 d . . . . . C52 C 0.3996(7) 0.0485(3) 0.6685(5) 0.085(2) Uani 1 1 d . . . . . H52A H 0.3798 0.0599 0.6104 0.128 Uiso 1 1 calc R U . . . H52B H 0.4855 0.0309 0.6750 0.128 Uiso 1 1 calc R U . . . H52C H 0.3955 0.0851 0.7034 0.128 Uiso 1 1 calc R U . . . C49 C 0.1251(6) 0.2089(2) 0.7746(4) 0.0579(15) Uani 1 1 d . . . . . H49A H 0.1474 0.2250 0.8310 0.069 Uiso 1 1 calc R U . . . H49B H 0.2018 0.2115 0.7425 0.069 Uiso 1 1 calc R U . . . C12 C -0.3485(11) -0.1188(5) 0.2741(6) 0.111(3) Uani 1 1 d . . . . . H12 H -0.3480 -0.1515 0.2353 0.133 Uiso 1 1 calc R U . . . C9 C -0.3455(7) -0.0224(4) 0.3901(4) 0.079(2) Uani 1 1 d . . . . . H9A H -0.3453 0.0097 0.4299 0.095 Uiso 1 1 calc R U . . . C38 C 0.4930(7) 0.0712(4) 1.0611(4) 0.085(2) Uani 1 1 d . . . . . H38 H 0.5514 0.0912 1.0997 0.101 Uiso 1 1 calc R U . . . C13 C -0.2364(8) -0.0868(3) 0.2964(4) 0.080(2) Uani 1 1 d . . . . . H13 H -0.1599 -0.0983 0.2725 0.096 Uiso 1 1 calc R U . . . C35 C 0.4650(11) -0.1244(5) 1.0547(6) 0.134(4) Uani 1 1 d . . . . . H35A H 0.4411 -0.1676 1.0462 0.200 Uiso 1 1 calc R U . . . H35B H 0.4463 -0.1118 1.1108 0.200 Uiso 1 1 calc R U . . . H35C H 0.5564 -0.1195 1.0479 0.200 Uiso 1 1 calc R U . . . C46 C -0.0892(8) 0.2944(3) 0.6080(5) 0.081(2) Uani 1 1 d . . . . . H46 H -0.0887 0.3042 0.5508 0.097 Uiso 1 1 calc R U . . . C68 C -0.1396(6) -0.2384(3) 0.8026(4) 0.0649(17) Uani 1 1 d D . . . . H68A H -0.2054 -0.2357 0.7559 0.078 Uiso 1 1 calc R U . . . H68B H -0.1665 -0.2700 0.8418 0.078 Uiso 1 1 calc R U . . . C64 C 0.2319(9) -0.3491(4) 0.7554(6) 0.099(3) Uani 1 1 d . . . . . H64 H 0.1615 -0.3731 0.7347 0.119 Uiso 1 1 calc R U . . . C60 C 0.3208(8) -0.2691(3) 0.8433(6) 0.088(2) Uani 1 1 d . . . . . H60 H 0.3115 -0.2372 0.8824 0.106 Uiso 1 1 calc R U . . . C61 C 0.4435(10) -0.2828(5) 0.8165(8) 0.116(4) Uani 1 1 d . . . . . H61 H 0.5150 -0.2604 0.8397 0.140 Uiso 1 1 calc R U . . . C30 C -0.0167(11) -0.0343(5) 1.1403(5) 0.115(3) Uani 1 1 d . . . . . H30 H -0.0902 -0.0593 1.1308 0.137 Uiso 1 1 calc R U . . . C11 C -0.4601(11) -0.1026(6) 0.3085(7) 0.124(4) Uani 1 1 d . . . . . H11 H -0.5367 -0.1239 0.2924 0.148 Uiso 1 1 calc R U . . . C62 C 0.4623(12) -0.3268(7) 0.7587(9) 0.131(4) Uani 1 1 d . . . . . H62 H 0.5445 -0.3343 0.7398 0.157 Uiso 1 1 calc R U . . . C10 C -0.4620(9) -0.0553(5) 0.3671(7) 0.111(3) Uani 1 1 d . . . . . H10 H -0.5389 -0.0450 0.3914 0.133 Uiso 1 1 calc R U . . . C29 C 0.0848(18) -0.0549(8) 1.1949(7) 0.172(7) Uani 1 1 d . . . . . H29 H 0.0807 -0.0939 1.2208 0.207 Uiso 1 1 calc R U . . . C63 C 0.3560(14) -0.3605(6) 0.7284(7) 0.126(4) Uani 1 1 d . . . . . H63 H 0.3667 -0.3918 0.6887 0.151 Uiso 1 1 calc R U . . . C59 C 0.1205(5) -0.2027(2) 0.6767(3) 0.0498(13) Uani 1 1 d . . . . . H59 H 0.1212 -0.2410 0.6487 0.060 Uiso 1 1 calc R U . . . Br2 Br 0.0473(3) 0.16603(8) 0.45171(11) 0.0915(7) Uani 0.712(9) 1 d . . P A 1 Br1 Br -0.2378(4) -0.21032(12) 1.01584(18) 0.1084(10) Uani 0.712(9) 1 d . . P A 1 C27 C 0.1973(10) 0.0376(9) 1.1706(7) 0.163(7) Uani 1 1 d . . . . . H27 H 0.2710 0.0626 1.1795 0.195 Uiso 1 1 calc R U . . . C28 C 0.1925(16) -0.0167(12) 1.2107(7) 0.203(12) Uani 1 1 d . . . . . H28 H 0.2605 -0.0290 1.2489 0.244 Uiso 1 1 calc R U . . . Br3 Br 0.1357(19) 0.1581(4) 0.4496(4) 0.152(4) Uani 0.288(9) 1 d . . P A 2 Br4 Br -0.1611(16) -0.2020(4) 1.0280(4) 0.163(3) Uani 0.288(9) 1 d . . P A 2 O13B O 0.151(2) -0.1427(8) 0.9134(14) 0.078(4) Uani 0.712(9) 1 d D U P A 1 H13B H 0.199(6) -0.110(3) 0.919(3) 0.118 Uiso 0.712(9) 1 d D U P A 1 C69 C 0.1406(13) -0.1591(6) 1.0048(7) 0.105(4) Uani 0.712(9) 1 d D U P A 1 H69A H 0.0527 -0.1713 1.0135 0.158 Uiso 0.712(9) 1 calc R U P A 1 H69B H 0.1638 -0.1233 1.0394 0.158 Uiso 0.712(9) 1 calc R U P A 1 H69C H 0.1984 -0.1932 1.0200 0.158 Uiso 0.712(9) 1 calc R U P A 1 O13A O 0.153(5) -0.1328(17) 0.920(2) 0.061(10) Uani 0.288(9) 1 d D . P A 2 H13A H 0.2089 -0.0986 0.9052 0.091 Uiso 0.288(9) 1 d DR U P A 2 H13C H 0.2073 -0.1623 0.8962 0.091 Uiso 0.288(9) 1 d DR U 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 Cu3 0.0512(3) 0.0298(3) 0.0365(3) -0.0041(3) -0.0107(2) 0.0033(3) Cu1 0.0455(3) 0.0337(3) 0.0343(3) -0.0030(2) -0.0072(2) -0.0029(2) Cu2 0.0503(3) 0.0369(3) 0.0378(3) -0.0053(3) -0.0033(2) 0.0067(3) Cu4 0.0585(4) 0.0308(3) 0.0400(3) 0.0027(2) -0.0010(3) 0.0021(3) O2 0.052(2) 0.0297(16) 0.0451(19) -0.0068(14) 0.0034(16) -0.0002(14) O11 0.054(2) 0.0430(19) 0.053(2) -0.0069(17) -0.0104(17) 0.0138(16) C33 0.057(3) 0.060(3) 0.033(2) -0.009(2) 0.000(2) 0.013(2) N2 0.053(3) 0.031(2) 0.046(2) -0.0052(18) -0.0131(19) 0.0006(17) O8 0.053(2) 0.0369(18) 0.0396(18) -0.0105(14) 0.0030(15) -0.0085(15) N1 0.063(3) 0.027(2) 0.046(2) -0.0037(18) -0.014(2) 0.0029(18) O7 0.056(2) 0.058(2) 0.063(2) -0.008(2) 0.0169(19) -0.0060(18) O1 0.055(2) 0.049(2) 0.063(2) -0.005(2) 0.0045(16) -0.0118(18) O10 0.074(3) 0.058(2) 0.067(3) 0.008(2) -0.017(2) 0.014(2) C24 0.040(3) 0.039(3) 0.059(3) -0.003(2) -0.010(2) -0.004(2) C19 0.053(3) 0.041(3) 0.066(4) 0.002(3) -0.004(3) -0.001(2) C3 0.048(3) 0.060(4) 0.066(4) 0.011(3) -0.002(3) -0.008(3) C2 0.050(3) 0.045(3) 0.045(3) 0.000(2) -0.006(2) 0.005(2) C7 0.041(3) 0.037(3) 0.041(3) -0.002(2) -0.009(2) 0.002(2) C8 0.055(3) 0.037(3) 0.040(3) -0.011(2) -0.010(2) 0.006(2) N4 0.049(2) 0.036(2) 0.036(2) -0.0049(17) -0.0061(18) 0.0050(18) C16 0.050(3) 0.050(3) 0.039(3) -0.008(2) -0.001(2) 0.001(2) C58 0.042(3) 0.037(2) 0.033(2) -0.003(2) -0.011(2) 0.007(2) C57 0.058(3) 0.035(3) 0.038(3) -0.003(2) -0.007(2) 0.009(2) O9 0.055(2) 0.052(2) 0.0448(19) 0.0007(16) -0.0068(16) -0.0089(17) C32 0.068(4) 0.101(5) 0.044(3) -0.015(3) 0.002(3) 0.020(3) C53 0.041(3) 0.047(3) 0.042(3) -0.001(2) -0.006(2) 0.007(2) C15 0.051(3) 0.052(3) 0.041(2) -0.001(2) -0.007(2) -0.001(2) N3 0.053(3) 0.044(2) 0.043(2) -0.0071(19) -0.0035(19) 0.009(2) C25 0.069(4) 0.047(3) 0.049(3) -0.015(2) 0.005(3) 0.006(3) C5 0.071(4) 0.040(3) 0.060(3) -0.006(3) -0.008(3) -0.012(3) O5 0.068(2) 0.0411(19) 0.045(2) -0.0022(16) -0.0171(17) 0.0090(17) C41 0.049(3) 0.058(3) 0.034(2) -0.005(3) -0.007(2) 0.010(3) C1 0.075(4) 0.088(5) 0.072(4) -0.003(4) 0.020(4) 0.004(4) C40 0.055(3) 0.059(3) 0.039(3) -0.009(2) -0.008(2) 0.002(3) C4 0.070(4) 0.044(3) 0.075(4) -0.005(3) -0.011(3) -0.020(3) O6 0.052(2) 0.0296(16) 0.0371(16) -0.0010(13) -0.0119(14) -0.0018(14) O12 0.067(2) 0.0387(18) 0.0320(16) 0.0008(14) 0.0023(15) 0.0087(16) C51 0.065(3) 0.028(2) 0.050(3) 0.004(2) -0.014(2) -0.004(2) O14 0.077(3) 0.067(3) 0.057(2) -0.006(2) -0.014(2) 0.020(2) C17 0.047(3) 0.063(4) 0.049(3) -0.002(3) -0.001(2) 0.005(2) C50 0.049(3) 0.031(2) 0.050(3) -0.006(2) -0.010(2) 0.000(2) O3 0.079(3) 0.054(2) 0.064(3) 0.011(2) 0.015(2) -0.006(2) C23 0.059(3) 0.039(3) 0.064(3) -0.003(3) 0.001(3) 0.007(2) C39 0.083(5) 0.075(4) 0.056(4) -0.011(3) -0.022(3) -0.011(4) C22 0.085(4) 0.050(3) 0.073(4) -0.007(3) 0.010(3) 0.014(3) C44 0.080(5) 0.066(5) 0.130(7) 0.003(5) 0.004(5) 0.012(4) C55 0.060(4) 0.079(4) 0.056(3) -0.008(3) 0.007(3) 0.024(3) C56 0.068(4) 0.056(3) 0.055(3) -0.013(3) -0.005(3) 0.019(3) C42 0.063(3) 0.041(3) 0.046(3) -0.010(2) -0.010(3) -0.004(2) C31 0.088(4) 0.092(5) 0.034(3) -0.013(3) 0.009(3) 0.042(4) C48 0.066(4) 0.027(2) 0.072(4) -0.004(3) -0.018(3) -0.006(2) C21 0.078(5) 0.049(4) 0.103(6) -0.006(4) 0.010(4) 0.023(3) C34 0.076(4) 0.054(3) 0.036(3) 0.001(2) 0.009(3) 0.013(3) C54 0.040(3) 0.071(4) 0.058(3) 0.008(3) -0.001(3) 0.003(3) C47 0.068(4) 0.048(3) 0.088(5) 0.008(3) -0.012(3) -0.010(3) C45 0.070(5) 0.056(4) 0.122(7) 0.016(4) -0.032(5) 0.000(3) C6 0.048(3) 0.035(2) 0.049(3) -0.003(2) -0.001(2) -0.001(2) C26 0.077(5) 0.134(7) 0.080(5) -0.042(5) -0.022(4) 0.036(5) C67 0.070(4) 0.030(3) 0.065(3) 0.002(2) -0.011(3) -0.004(2) C43 0.084(5) 0.053(4) 0.090(5) -0.005(3) -0.002(4) 0.010(3) C65 0.088(5) 0.042(3) 0.078(4) 0.019(3) -0.014(4) 0.008(3) C14 0.061(4) 0.066(4) 0.040(3) 0.011(3) -0.016(3) -0.004(3) C20 0.064(4) 0.040(3) 0.099(5) 0.005(3) -0.010(4) 0.012(3) C66 0.085(5) 0.041(3) 0.077(4) 0.019(3) -0.003(3) -0.005(3) C18 0.116(6) 0.083(5) 0.084(5) 0.023(4) -0.025(5) 0.021(5) O4 0.103(3) 0.069(3) 0.056(2) 0.005(2) -0.027(2) 0.025(2) C37 0.078(4) 0.105(6) 0.046(3) -0.005(4) -0.023(3) 0.024(4) C36 0.062(4) 0.073(4) 0.040(3) -0.003(3) -0.006(3) 0.023(3) C52 0.074(5) 0.059(4) 0.125(6) -0.002(4) 0.018(4) -0.021(3) C49 0.065(4) 0.035(3) 0.071(4) -0.004(3) -0.020(3) -0.003(2) C12 0.127(8) 0.100(6) 0.099(6) 0.002(5) -0.045(6) -0.049(6) C9 0.065(4) 0.110(6) 0.063(4) 0.013(4) -0.004(3) -0.007(4) C38 0.087(5) 0.105(6) 0.056(4) -0.012(4) -0.036(4) -0.009(4) C13 0.095(5) 0.080(5) 0.062(4) -0.003(4) -0.021(4) -0.024(4) C35 0.189(10) 0.098(6) 0.103(6) 0.016(5) -0.066(7) 0.057(7) C46 0.088(5) 0.058(4) 0.092(5) 0.019(4) -0.033(4) -0.014(4) C68 0.059(4) 0.044(3) 0.090(5) 0.011(3) -0.005(3) -0.013(3) C64 0.112(7) 0.073(5) 0.107(6) -0.002(5) -0.021(5) 0.022(5) C60 0.090(6) 0.055(4) 0.117(6) 0.023(4) -0.014(5) 0.000(4) C61 0.092(7) 0.079(6) 0.175(11) 0.055(7) -0.011(7) -0.004(5) C30 0.162(9) 0.130(8) 0.054(4) 0.014(5) 0.023(5) 0.059(7) C11 0.107(8) 0.145(10) 0.111(7) 0.041(7) -0.049(6) -0.063(7) C62 0.122(9) 0.117(9) 0.157(11) 0.065(9) 0.023(8) 0.039(8) C10 0.075(5) 0.143(9) 0.111(7) 0.037(7) -0.007(5) -0.016(5) C29 0.243(16) 0.206(15) 0.068(7) 0.038(8) 0.011(9) 0.146(14) C63 0.155(10) 0.113(8) 0.109(7) 0.003(6) 0.015(8) 0.065(8) C59 0.066(4) 0.034(3) 0.046(3) -0.008(2) -0.019(3) 0.011(2) Br2 0.1370(18) 0.0622(7) 0.0747(8) 0.0242(5) 0.0027(9) -0.0006(9) Br1 0.1243(18) 0.1110(14) 0.0934(12) 0.0536(10) 0.0332(12) 0.0134(11) C27 0.090(7) 0.30(2) 0.093(7) -0.074(10) -0.029(6) 0.077(10) C28 0.178(14) 0.37(3) 0.061(6) -0.031(10) -0.026(8) 0.197(18) Br3 0.250(12) 0.079(3) 0.124(3) 0.033(2) -0.005(5) -0.051(5) Br4 0.204(9) 0.199(6) 0.083(2) 0.075(3) -0.009(4) -0.056(5) O13B 0.102(10) 0.045(5) 0.082(6) -0.011(5) -0.038(6) 0.022(5) C69 0.116(9) 0.114(9) 0.082(6) -0.013(6) -0.019(7) 0.030(8) O13A 0.09(2) 0.056(18) 0.036(11) 0.018(12) -0.006(11) -0.007(14) 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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 O2 Cu3 O1 72.63(13) . . y N2 Cu3 O2 172.74(16) . . y N2 Cu3 O1 101.11(16) . . y N2 Cu3 O6 84.97(14) . . y O5 Cu3 O2 91.14(14) . . y O5 Cu3 N2 93.30(15) . . y O5 Cu3 O1 96.93(15) . . y O5 Cu3 O6 173.71(15) . . y O6 Cu3 O2 91.21(13) . . y O6 Cu3 O1 89.34(13) . . y O8 Cu1 N4 92.34(15) . . y O8 Cu1 O9 174.70(14) . . y O8 Cu1 O6 86.89(14) . . y O8 Cu1 O14 91.33(16) . . y N4 Cu1 O9 82.85(16) . . y N4 Cu1 O6 164.41(14) . . y N4 Cu1 O14 98.19(15) . . y O9 Cu1 O14 91.57(16) . . y O6 Cu1 O9 97.13(14) . . y O6 Cu1 O14 97.39(14) . . y O11 Cu2 O8 91.37(14) . . y O11 Cu2 N3 92.34(16) . . y O11 Cu2 O12 173.67(16) . . y N3 Cu2 O8 174.24(16) . . y N3 Cu2 O12 85.22(15) . . y O12 Cu2 O8 91.54(14) . . y O2 Cu4 N1 91.68(17) . . y O2 Cu4 O12 86.43(14) . . y O2 Cu4 O3 171.46(16) . . y O2 Cu4 O13B 94.7(6) . . y O2 Cu4 O13A 92.9(10) . . y N1 Cu4 O3 82.35(19) . . y N1 Cu4 O13B 95.3(5) . . y N1 Cu4 O13A 100.7(10) . . y O12 Cu4 N1 167.20(15) . . y O12 Cu4 O3 98.03(17) . . y O12 Cu4 O13B 97.5(5) . . y O12 Cu4 O13A 92.0(10) . . y O3 Cu4 O13B 91.9(6) . . y O3 Cu4 O13A 94.2(9) . . y Cu4 O2 Cu3 108.29(15) . . ? C58 O2 Cu3 122.7(3) . . ? C58 O2 Cu4 128.5(3) . . ? C24 O11 Cu2 126.9(3) . . ? C32 C33 H33 107.1 . . ? N3 C33 H33 107.1 . . ? N3 C33 C32 116.3(4) . . ? N3 C33 C34 106.5(4) . . ? C34 C33 H33 107.1 . . ? C34 C33 C32 112.4(5) . . ? C50 N2 Cu3 111.7(3) . . ? C42 N2 Cu3 125.5(4) . . ? C42 N2 C50 122.8(4) . . ? Cu1 O8 Cu2 107.03(14) . . ? C7 O8 Cu1 128.4(3) . . ? C7 O8 Cu2 124.2(3) . . ? C67 N1 Cu4 114.0(4) . . ? C59 N1 Cu4 126.1(4) . . ? C59 N1 C67 119.9(4) . . ? C2 O7 C1 117.7(5) . . ? C53 O1 Cu3 111.5(3) . . ? C53 O1 C52 118.0(5) . . ? C52 O1 Cu3 130.4(4) . . ? C19 O10 C18 118.2(5) . . ? O11 C24 C19 118.4(5) . . ? O11 C24 C23 124.7(5) . . ? C23 C24 C19 116.9(5) . . ? O10 C19 C24 113.0(5) . . ? C20 C19 O10 125.8(5) . . ? C20 C19 C24 121.2(6) . . ? C2 C3 H3 119.5 . . ? C2 C3 C4 120.9(6) . . ? C4 C3 H3 119.5 . . ? O7 C2 C3 125.7(5) . . ? O7 C2 C7 113.5(4) . . ? C3 C2 C7 120.8(5) . . ? O8 C7 C2 119.4(4) . . ? O8 C7 C6 122.2(5) . . ? C2 C7 C6 118.4(4) . . ? N4 C8 H8 117.1 . . ? N4 C8 C6 125.7(4) . . ? C6 C8 H8 117.1 . . ? C8 N4 Cu1 126.1(4) . . ? C8 N4 C16 119.5(4) . . ? C16 N4 Cu1 114.3(3) . . ? N4 C16 H16 108.9 . . ? N4 C16 C15 110.1(4) . . ? N4 C16 C17 107.1(4) . . ? C15 C16 H16 108.9 . . ? C17 C16 H16 108.9 . . ? C17 C16 C15 112.8(4) . . ? O2 C58 C57 123.0(5) . . ? O2 C58 C53 119.5(4) . . ? C53 C58 C57 117.4(5) . . ? C58 C57 C59 122.7(5) . . ? C56 C57 C58 119.3(5) . . ? C56 C57 C59 117.9(5) . . ? Cu1 O9 H9 131(3) . . ? C17 O9 Cu1 111.6(3) . . ? C17 O9 H9 108(2) . . ? C33 C32 H32A 109.4 . . ? C33 C32 H32B 109.4 . . ? H32A C32 H32B 108.0 . . ? C31 C32 C33 111.0(5) . . ? C31 C32 H32A 109.4 . . ? C31 C32 H32B 109.4 . . ? O1 C53 C58 113.5(4) . . ? O1 C53 C54 124.9(5) . . ? C54 C53 C58 121.6(5) . . ? C16 C15 H15A 109.0 . . ? C16 C15 H15B 109.0 . . ? H15A C15 H15B 107.8 . . ? C14 C15 C16 113.1(4) . . ? C14 C15 H15A 109.0 . . ? C14 C15 H15B 109.0 . . ? C33 N3 Cu2 111.1(3) . . ? C25 N3 Cu2 125.6(4) . . ? C25 N3 C33 123.3(4) . . ? N3 C25 H25 116.9 . . ? N3 C25 C23 126.2(5) . . ? C23 C25 H25 116.9 . . ? C4 C5 H5 119.7 . . ? C4 C5 C6 120.5(5) . . ? C6 C5 H5 119.7 . . ? C41 O5 Cu3 126.4(3) . . ? O5 C41 C40 125.2(4) . . ? O5 C41 C36 117.6(5) . . ? C40 C41 C36 117.2(5) . . ? O7 C1 H1A 109.5 . . ? O7 C1 H1B 109.5 . . ? O7 C1 H1C 109.5 . . ? H1A C1 H1B 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? C41 C40 C39 119.6(5) . . ? C41 C40 C42 122.8(4) . . ? C39 C40 C42 117.6(5) . . ? C3 C4 H4 119.9 . . ? C5 C4 C3 120.2(5) . . ? C5 C4 H4 119.9 . . ? Cu1 O6 Cu3 124.77(16) . . ? C51 O6 Cu3 108.2(3) . . ? C51 O6 Cu1 117.1(3) . . ? Cu4 O12 Cu2 127.93(17) . . ? C34 O12 Cu2 107.9(3) . . ? C34 O12 Cu4 117.4(3) . . ? O6 C51 H51A 109.6 . . ? O6 C51 H51B 109.6 . . ? O6 C51 C50 110.4(4) . . ? H51A C51 H51B 108.1 . . ? C50 C51 H51A 109.6 . . ? C50 C51 H51B 109.6 . . ? Cu1 O14 H14A 112.7 . . ? Cu1 O14 H14B 112.3 . . ? H14A O14 H14B 101.4 . . ? C16 C17 H17A 109.6 . . ? C16 C17 H17B 109.6 . . ? O9 C17 C16 110.3(4) . . ? O9 C17 H17A 109.6 . . ? O9 C17 H17B 109.6 . . ? H17A C17 H17B 108.1 . . ? N2 C50 C51 106.6(4) . . ? N2 C50 H50 106.9 . . ? N2 C50 C49 116.3(4) . . ? C51 C50 H50 106.9 . . ? C51 C50 C49 112.8(4) . . ? C49 C50 H50 106.9 . . ? Cu4 O3 H3A 130(3) . . ? C68 O3 Cu4 113.3(4) . . ? C68 O3 H3A 108(2) . . ? C24 C23 C25 122.6(5) . . ? C24 C23 C22 119.8(5) . . ? C22 C23 C25 117.6(5) . . ? C40 C39 H39 119.7 . . ? C38 C39 C40 120.5(6) . . ? C38 C39 H39 119.7 . . ? C23 C22 H22 119.5 . . ? C21 C22 C23 121.1(6) . . ? C21 C22 H22 119.5 . . ? C45 C44 H44 119.5 . . ? C45 C44 C43 120.9(8) . . ? C43 C44 H44 119.5 . . ? C56 C55 H55 120.2 . . ? C56 C55 C54 119.5(6) . . ? C54 C55 H55 120.2 . . ? C57 C56 H56 119.3 . . ? C55 C56 C57 121.4(5) . . ? C55 C56 H56 119.3 . . ? N2 C42 C40 125.6(5) . . ? N2 C42 H42 117.2 . . ? C40 C42 H42 117.2 . . ? C26 C31 C32 120.0(7) . . ? C30 C31 C32 120.3(8) . . ? C30 C31 C26 119.7(8) . . ? C47 C48 C49 121.2(6) . . ? C43 C48 C47 118.7(6) . . ? C43 C48 C49 120.1(6) . . ? C22 C21 H21 120.1 . . ? C22 C21 C20 119.8(6) . . ? C20 C21 H21 120.1 . . ? C33 C34 H34A 110.0 . . ? C33 C34 H34B 110.0 . . ? O12 C34 C33 108.5(4) . . ? O12 C34 H34A 110.0 . . ? O12 C34 H34B 110.0 . . ? H34A C34 H34B 108.4 . . ? C53 C54 C55 120.7(6) . . ? C53 C54 H54 119.7 . . ? C55 C54 H54 119.7 . . ? C48 C47 H47 119.5 . . ? C48 C47 C46 121.1(7) . . ? C46 C47 H47 119.5 . . ? C44 C45 H45 119.9 . . ? C44 C45 C46 120.1(7) . . ? C46 C45 H45 119.9 . . ? C7 C6 C8 123.8(4) . . ? C7 C6 C5 119.1(5) . . ? C5 C6 C8 116.8(5) . . ? C31 C26 H26 120.5 . . ? C31 C26 C27 119.0(11) . . ? C27 C26 H26 120.5 . . ? N1 C67 H67 109.1 . . ? N1 C67 C66 108.9(4) . . ? N1 C67 C68 108.1(4) . . ? C66 C67 H67 109.1 . . ? C68 C67 H67 109.1 . . ? C68 C67 C66 112.5(5) . . ? C44 C43 H43 120.2 . . ? C48 C43 C44 119.6(7) . . ? C48 C43 H43 120.2 . . ? C64 C65 C66 121.2(7) . . ? C60 C65 C66 120.8(7) . . ? C60 C65 C64 118.0(8) . . ? C9 C14 C15 121.1(6) . . ? C9 C14 C13 118.6(6) . . ? C13 C14 C15 120.2(6) . . ? C19 C20 C21 121.2(6) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C67 C66 H66A 108.5 . . ? C67 C66 H66B 108.5 . . ? C65 C66 C67 115.1(5) . . ? C65 C66 H66A 108.5 . . ? C65 C66 H66B 108.5 . . ? H66A C66 H66B 107.5 . . ? O10 C18 H18A 109.5 . . ? O10 C18 H18B 109.5 . . ? O10 C18 H18C 109.5 . . ? H18A C18 H18B 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C36 O4 C35 117.2(6) . . ? C36 C37 H37 119.8 . . ? C36 C37 C38 120.4(6) . . ? C38 C37 H37 119.8 . . ? O4 C36 C41 113.1(5) . . ? O4 C36 C37 125.5(6) . . ? C37 C36 C41 121.4(6) . . ? O1 C52 H52A 109.5 . . ? O1 C52 H52B 109.5 . . ? O1 C52 H52C 109.5 . . ? H52A C52 H52B 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C50 C49 H49A 109.9 . . ? C50 C49 H49B 109.9 . . ? C48 C49 C50 109.0(4) . . ? C48 C49 H49A 109.9 . . ? C48 C49 H49B 109.9 . . ? H49A C49 H49B 108.3 . . ? C13 C12 H12 120.2 . . ? C11 C12 H12 120.2 . . ? C11 C12 C13 119.7(10) . . ? C14 C9 H9A 120.1 . . ? C14 C9 C10 119.8(8) . . ? C10 C9 H9A 120.1 . . ? C39 C38 C37 120.7(6) . . ? C39 C38 H38 119.6 . . ? C37 C38 H38 119.6 . . ? C14 C13 H13 119.1 . . ? C12 C13 C14 121.8(9) . . ? C12 C13 H13 119.1 . . ? O4 C35 H35A 109.5 . . ? O4 C35 H35B 109.5 . . ? O4 C35 H35C 109.5 . . ? H35A C35 H35B 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C47 C46 H46 120.2 . . ? C45 C46 C47 119.6(7) . . ? C45 C46 H46 120.2 . . ? O3 C68 C67 109.4(5) . . ? O3 C68 H68A 109.8 . . ? O3 C68 H68B 109.8 . . ? C67 C68 H68A 109.8 . . ? C67 C68 H68B 109.8 . . ? H68A C68 H68B 108.2 . . ? C65 C64 H64 120.2 . . ? C65 C64 C63 119.6(9) . . ? C63 C64 H64 120.2 . . ? C65 C60 H60 119.6 . . ? C65 C60 C61 120.9(9) . . ? C61 C60 H60 119.6 . . ? C60 C61 H61 118.9 . . ? C62 C61 C60 122.3(10) . . ? C62 C61 H61 118.9 . . ? C31 C30 H30 119.3 . . ? C31 C30 C29 121.3(13) . . ? C29 C30 H30 119.3 . . ? C12 C11 H11 119.5 . . ? C12 C11 C10 120.9(9) . . ? C10 C11 H11 119.5 . . ? C61 C62 H62 121.3 . . ? C61 C62 C63 117.3(11) . . ? C63 C62 H62 121.3 . . ? C9 C10 H10 120.4 . . ? C11 C10 C9 119.2(9) . . ? C11 C10 H10 120.4 . . ? C30 C29 H29 120.4 . . ? C30 C29 C28 119.2(15) . . ? C28 C29 H29 120.4 . . ? C64 C63 H63 119.1 . . ? C62 C63 C64 121.8(11) . . ? C62 C63 H63 119.1 . . ? N1 C59 C57 127.2(5) . . ? N1 C59 H59 116.4 . . ? C57 C59 H59 116.4 . . ? C26 C27 H27 119.1 . . ? C28 C27 C26 121.8(15) . . ? C28 C27 H27 119.1 . . ? C29 C28 H28 120.5 . . ? C27 C28 C29 118.9(11) . . ? C27 C28 H28 120.5 . . ? Cu4 O13B H13B 106(3) . . ? C69 O13B Cu4 135.9(15) . . ? C69 O13B H13B 100(3) . . ? O13B C69 H69A 109.5 . . ? O13B C69 H69B 109.5 . . ? O13B C69 H69C 109.5 . . ? H69A C69 H69B 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? Cu4 O13A H13A 95.4 . . ? Cu4 O13A H13C 95.7 . . ? H13A O13A H13C 91.4 . . ? 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 Cu3 O2 2.011(3) . y Cu3 N2 1.944(4) . y Cu3 O1 2.369(3) . y Cu3 O5 1.907(3) . y Cu3 O6 1.966(3) . y Cu1 O8 1.927(3) . y Cu1 N4 1.936(4) . y Cu1 O9 2.022(4) . y Cu1 O6 1.937(3) . y Cu1 O14 2.294(4) . y Cu2 O11 1.921(3) . y Cu2 O8 2.001(3) . y Cu2 N3 1.952(4) . y Cu2 O12 1.978(3) . y Cu4 O2 1.938(3) . y Cu4 N1 1.951(4) . y Cu4 O12 1.942(3) . y Cu4 O3 1.996(4) . y Cu4 O13B 2.28(2) . y Cu4 O13A 2.34(5) . y O2 C58 1.318(6) . ? O11 C24 1.302(6) . ? C33 H33 0.9800 . ? C33 C32 1.536(7) . ? C33 N3 1.469(6) . ? C33 C34 1.528(8) . ? N2 C50 1.477(6) . ? N2 C42 1.287(6) . ? O8 C7 1.328(6) . ? N1 C67 1.472(7) . ? N1 C59 1.269(7) . ? O7 C2 1.365(6) . ? O7 C1 1.432(7) . ? O1 C53 1.362(6) . ? O1 C52 1.415(7) . ? O10 C19 1.360(7) . ? O10 C18 1.422(7) . ? C24 C19 1.438(7) . ? C24 C23 1.410(8) . ? C19 C20 1.356(8) . ? C3 H3 0.9300 . ? C3 C2 1.373(8) . ? C3 C4 1.382(9) . ? C2 C7 1.401(7) . ? C7 C6 1.408(7) . ? C8 H8 0.9300 . ? C8 N4 1.282(6) . ? C8 C6 1.438(7) . ? N4 C16 1.470(7) . ? C16 H16 0.9800 . ? C16 C15 1.523(7) . ? C16 C17 1.508(7) . ? C58 C57 1.415(7) . ? C58 C53 1.414(7) . ? C57 C56 1.414(8) . ? C57 C59 1.424(8) . ? O9 H9 0.858(13) . ? O9 C17 1.452(6) . ? C32 H32A 0.9700 . ? C32 H32B 0.9700 . ? C32 C31 1.509(8) . ? C53 C54 1.376(8) . ? C15 H15A 0.9700 . ? C15 H15B 0.9700 . ? C15 C14 1.503(7) . ? N3 C25 1.271(7) . ? C25 H25 0.9300 . ? C25 C23 1.429(8) . ? C5 H5 0.9300 . ? C5 C4 1.355(9) . ? C5 C6 1.426(7) . ? O5 C41 1.305(6) . ? C41 C40 1.405(8) . ? C41 C36 1.429(7) . ? C1 H1A 0.9600 . ? C1 H1B 0.9600 . ? C1 H1C 0.9600 . ? C40 C39 1.414(7) . ? C40 C42 1.432(7) . ? C4 H4 0.9300 . ? O6 C51 1.418(6) . ? O12 C34 1.429(6) . ? C51 H51A 0.9700 . ? C51 H51B 0.9700 . ? C51 C50 1.498(7) . ? O14 H14A 0.9120 . ? O14 H14B 0.9109 . ? C17 H17A 0.9700 . ? C17 H17B 0.9700 . ? C50 H50 0.9800 . ? C50 C49 1.534(7) . ? O3 H3A 0.862(14) . ? O3 C68 1.451(7) . ? C23 C22 1.418(8) . ? C39 H39 0.9300 . ? C39 C38 1.363(9) . ? C22 H22 0.9300 . ? C22 C21 1.358(9) . ? C44 H44 0.9300 . ? C44 C45 1.332(11) . ? C44 C43 1.407(10) . ? C55 H55 0.9300 . ? C55 C56 1.371(9) . ? C55 C54 1.381(9) . ? C56 H56 0.9300 . ? C42 H42 0.9300 . ? C31 C26 1.355(11) . ? C31 C30 1.338(11) . ? C48 C47 1.361(9) . ? C48 C43 1.361(9) . ? C48 C49 1.506(8) . ? C21 H21 0.9300 . ? C21 C20 1.388(10) . ? C34 H34A 0.9700 . ? C34 H34B 0.9700 . ? C54 H54 0.9300 . ? C47 H47 0.9300 . ? C47 C46 1.395(9) . ? C45 H45 0.9300 . ? C45 C46 1.350(11) . ? C26 H26 0.9300 . ? C26 C27 1.398(13) . ? C67 H67 0.9800 . ? C67 C66 1.554(8) . ? C67 C68 1.492(8) . ? C43 H43 0.9300 . ? C65 C66 1.493(10) . ? C65 C64 1.381(10) . ? C65 C60 1.355(10) . ? C14 C9 1.367(9) . ? C14 C13 1.382(9) . ? C20 H20 0.9300 . ? C66 H66A 0.9700 . ? C66 H66B 0.9700 . ? C18 H18A 0.9600 . ? C18 H18B 0.9600 . ? C18 H18C 0.9600 . ? O4 C36 1.357(8) . ? O4 C35 1.437(8) . ? C37 H37 0.9300 . ? C37 C36 1.361(9) . ? C37 C38 1.372(11) . ? C52 H52A 0.9600 . ? C52 H52B 0.9600 . ? C52 H52C 0.9600 . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C12 H12 0.9300 . ? C12 C13 1.366(10) . ? C12 C11 1.350(15) . ? C9 H9A 0.9300 . ? C9 C10 1.416(12) . ? C38 H38 0.9300 . ? C13 H13 0.9300 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C46 H46 0.9300 . ? C68 H68A 0.9700 . ? C68 H68B 0.9700 . ? C64 H64 0.9300 . ? C64 C63 1.396(14) . ? C60 H60 0.9300 . ? C60 C61 1.390(13) . ? C61 H61 0.9300 . ? C61 C62 1.336(16) . ? C30 H30 0.9300 . ? C30 C29 1.381(15) . ? C11 H11 0.9300 . ? C11 C10 1.372(14) . ? C62 H62 0.9300 . ? C62 C63 1.367(16) . ? C10 H10 0.9300 . ? C29 H29 0.9300 . ? C29 C28 1.38(3) . ? C63 H63 0.9300 . ? C59 H59 0.9300 . ? C27 H27 0.9300 . ? C27 C28 1.32(2) . ? C28 H28 0.9300 . ? O13B H13B 0.848(15) . ? O13B C69 1.50(2) . ? C69 H69A 0.9600 . ? C69 H69B 0.9600 . ? C69 H69C 0.9600 . ? O13A H13A 0.9694 . ? O13A H13C 0.9394 . ? 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 O14 H14B O11 0.91 2.03 2.810(6) 142.4 . O13B H13B O5 0.848(15) 2.04(3) 2.822(19) 152(4) . O13A H13A O5 0.97 1.73 2.64(4) 155.8 . 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 Cu3 O2 C58 C57 177.7(3) . . . . ? Cu3 O2 C58 C53 -1.7(5) . . . . ? Cu3 N2 C50 C51 -27.6(5) . . . . ? Cu3 N2 C50 C49 -154.3(4) . . . . ? Cu3 N2 C42 C40 -2.2(8) . . . . ? Cu3 O1 C53 C58 -3.7(5) . . . . ? Cu3 O1 C53 C54 177.6(4) . . . . ? Cu3 O5 C41 C40 8.9(7) . . . . ? Cu3 O5 C41 C36 -172.3(4) . . . . ? Cu3 O6 C51 C50 -42.0(5) . . . . ? Cu1 O8 C7 C2 -177.2(3) . . . . ? Cu1 O8 C7 C6 2.8(6) . . . . ? Cu1 N4 C16 C15 -88.3(4) . . . . ? Cu1 N4 C16 C17 34.7(5) . . . . ? Cu1 O9 C17 C16 28.5(5) . . . . ? Cu1 O6 C51 C50 170.6(3) . . . . ? Cu2 O11 C24 C19 -172.7(4) . . . . ? Cu2 O11 C24 C23 6.5(7) . . . . ? Cu2 O8 C7 C2 9.8(6) . . . . ? Cu2 O8 C7 C6 -170.3(3) . . . . ? Cu2 N3 C25 C23 -6.8(9) . . . . ? Cu2 O12 C34 C33 -43.3(5) . . . . ? Cu4 O2 C58 C57 7.0(6) . . . . ? Cu4 O2 C58 C53 -172.5(3) . . . . ? Cu4 N1 C67 C66 -89.8(5) . . . . ? Cu4 N1 C67 C68 32.7(5) . . . . ? Cu4 N1 C59 C57 8.7(7) . . . . ? Cu4 O12 C34 C33 163.2(4) . . . . ? Cu4 O3 C68 C67 28.9(6) . . . . ? O2 C58 C57 C56 177.3(4) . . . . ? O2 C58 C57 C59 -7.1(7) . . . . ? O2 C58 C53 O1 3.8(6) . . . . ? O2 C58 C53 C54 -177.5(4) . . . . ? O11 C24 C19 O10 -2.9(7) . . . . ? O11 C24 C19 C20 176.5(5) . . . . ? O11 C24 C23 C25 4.5(8) . . . . ? O11 C24 C23 C22 -177.6(5) . . . . ? C33 C32 C31 C26 79.0(7) . . . . ? C33 C32 C31 C30 -101.2(7) . . . . ? C33 N3 C25 C23 173.0(5) . . . . ? N2 C50 C49 C48 -172.4(5) . . . . ? O8 C7 C6 C8 -10.4(7) . . . . ? O8 C7 C6 C5 177.0(4) . . . . ? N1 C67 C66 C65 -57.1(7) . . . . ? N1 C67 C68 O3 -38.7(6) . . . . ? O7 C2 C7 O8 3.0(6) . . . . ? O7 C2 C7 C6 -177.0(4) . . . . ? O1 C53 C54 C55 178.4(5) . . . . ? O10 C19 C20 C21 -178.7(6) . . . . ? C24 C19 C20 C21 1.9(9) . . . . ? C24 C23 C22 C21 0.4(9) . . . . ? C19 C24 C23 C25 -176.2(5) . . . . ? C19 C24 C23 C22 1.7(8) . . . . ? C3 C2 C7 O8 -177.3(5) . . . . ? C3 C2 C7 C6 2.7(7) . . . . ? C2 C3 C4 C5 -0.8(9) . . . . ? C2 C7 C6 C8 169.5(5) . . . . ? C2 C7 C6 C5 -3.1(7) . . . . ? C8 N4 C16 C15 89.5(5) . . . . ? C8 N4 C16 C17 -147.6(4) . . . . ? N4 C8 C6 C7 5.0(8) . . . . ? N4 C8 C6 C5 177.8(5) . . . . ? N4 C16 C15 C14 -61.0(6) . . . . ? N4 C16 C17 O9 -40.0(5) . . . . ? C16 C15 C14 C9 105.8(6) . . . . ? C16 C15 C14 C13 -71.8(6) . . . . ? C58 C57 C56 C55 0.7(8) . . . . ? C58 C57 C59 N1 -1.2(8) . . . . ? C58 C53 C54 C55 -0.2(8) . . . . ? C57 C58 C53 O1 -175.7(4) . . . . ? C57 C58 C53 C54 3.0(7) . . . . ? C32 C33 N3 Cu2 -157.4(4) . . . . ? C32 C33 N3 C25 22.8(8) . . . . ? C32 C33 C34 O12 177.7(4) . . . . ? C32 C31 C26 C27 -179.1(6) . . . . ? C32 C31 C30 C29 179.0(7) . . . . ? C53 C58 C57 C56 -3.3(6) . . . . ? C53 C58 C57 C59 172.4(4) . . . . ? C15 C16 C17 O9 81.3(5) . . . . ? C15 C14 C9 C10 -179.2(6) . . . . ? C15 C14 C13 C12 179.2(6) . . . . ? N3 C33 C32 C31 -169.9(6) . . . . ? N3 C33 C34 O12 49.2(6) . . . . ? N3 C25 C23 C24 -4.3(9) . . . . ? N3 C25 C23 C22 177.8(6) . . . . ? C25 C23 C22 C21 178.4(6) . . . . ? O5 C41 C40 C39 179.7(5) . . . . ? O5 C41 C40 C42 1.9(9) . . . . ? O5 C41 C36 O4 -0.8(7) . . . . ? O5 C41 C36 C37 178.7(5) . . . . ? C41 C40 C39 C38 1.7(10) . . . . ? C41 C40 C42 N2 -5.4(9) . . . . ? C1 O7 C2 C3 5.0(8) . . . . ? C1 O7 C2 C7 -175.3(5) . . . . ? C40 C41 C36 O4 178.1(5) . . . . ? C40 C41 C36 C37 -2.4(8) . . . . ? C40 C39 C38 C37 -3.1(12) . . . . ? C4 C3 C2 O7 178.9(5) . . . . ? C4 C3 C2 C7 -0.8(8) . . . . ? C4 C5 C6 C7 1.5(8) . . . . ? C4 C5 C6 C8 -171.6(5) . . . . ? O6 C51 C50 N2 45.7(6) . . . . ? O6 C51 C50 C49 174.5(4) . . . . ? C51 C50 C49 C48 64.0(7) . . . . ? C17 C16 C15 C14 179.4(5) . . . . ? C50 N2 C42 C40 175.7(5) . . . . ? C23 C24 C19 O10 177.8(5) . . . . ? C23 C24 C19 C20 -2.8(8) . . . . ? C23 C22 C21 C20 -1.4(11) . . . . ? C39 C40 C42 N2 176.7(6) . . . . ? C22 C21 C20 C19 0.2(11) . . . . ? C44 C45 C46 C47 0.0(11) . . . . ? C56 C57 C59 N1 174.5(5) . . . . ? C56 C55 C54 C53 -2.5(8) . . . . ? C42 N2 C50 C51 154.3(5) . . . . ? C42 N2 C50 C49 27.5(8) . . . . ? C42 C40 C39 C38 179.7(6) . . . . ? C31 C26 C27 C28 -1.8(14) . . . . ? C31 C30 C29 C28 1.8(16) . . . . ? C48 C47 C46 C45 0.5(9) . . . . ? C34 C33 C32 C31 67.0(8) . . . . ? C34 C33 N3 Cu2 -31.3(5) . . . . ? C34 C33 N3 C25 148.9(6) . . . . ? C54 C55 C56 C57 2.2(9) . . . . ? C47 C48 C43 C44 1.5(9) . . . . ? C47 C48 C49 C50 -99.1(6) . . . . ? C45 C44 C43 C48 -1.1(11) . . . . ? C6 C8 N4 Cu1 7.6(7) . . . . ? C6 C8 N4 C16 -169.8(4) . . . . ? C6 C5 C4 C3 0.5(9) . . . . ? C26 C31 C30 C29 -1.2(11) . . . . ? C26 C27 C28 C29 2.4(19) . . . . ? C67 N1 C59 C57 -170.5(5) . . . . ? C43 C44 C45 C46 0.3(12) . . . . ? C43 C48 C47 C46 -1.2(9) . . . . ? C43 C48 C49 C50 77.5(7) . . . . ? C65 C64 C63 C62 1.3(14) . . . . ? C65 C60 C61 C62 2.0(13) . . . . ? C14 C9 C10 C11 0.3(12) . . . . ? C66 C67 C68 O3 81.6(6) . . . . ? C66 C65 C64 C63 176.8(7) . . . . ? C66 C65 C60 C61 -178.3(6) . . . . ? C18 O10 C19 C24 -178.6(6) . . . . ? C18 O10 C19 C20 2.0(9) . . . . ? C36 C41 C40 C39 0.9(8) . . . . ? C36 C41 C40 C42 -176.9(5) . . . . ? C36 C37 C38 C39 1.6(12) . . . . ? C52 O1 C53 C58 180.0(5) . . . . ? C52 O1 C53 C54 1.3(7) . . . . ? C49 C48 C47 C46 175.5(5) . . . . ? C49 C48 C43 C44 -175.2(6) . . . . ? C12 C11 C10 C9 1.2(14) . . . . ? C9 C14 C13 C12 1.6(10) . . . . ? C38 C37 C36 C41 1.2(10) . . . . ? C38 C37 C36 O4 -179.4(7) . . . . ? C13 C14 C9 C10 -1.6(10) . . . . ? C13 C12 C11 C10 -1.3(15) . . . . ? C35 O4 C36 C41 -176.7(7) . . . . ? C35 O4 C36 C37 3.9(10) . . . . ? C68 C67 C66 C65 -177.0(5) . . . . ? C64 C65 C66 C67 -68.1(8) . . . . ? C64 C65 C60 C61 0.3(10) . . . . ? C60 C65 C66 C67 110.5(7) . . . . ? C60 C65 C64 C63 -1.8(11) . . . . ? C60 C61 C62 C63 -2.5(15) . . . . ? C61 C62 C63 C64 0.9(16) . . . . ? C30 C31 C26 C27 1.1(10) . . . . ? C30 C29 C28 C27 -2(2) . . . . ? C11 C12 C13 C14 -0.2(13) . . . . ? C59 N1 C67 C66 89.5(6) . . . . ? C59 N1 C67 C68 -148.0(5) . . . . ? C59 C57 C56 C55 -175.1(5) . . . . ?