#------------------------------------------------------------------------------ #$Date: 2020-10-06 12:01:12 +0300 (Tue, 06 Oct 2020) $ #$Revision: 257559 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/51/7705178.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_7705178 loop_ _publ_author_name 'Li, Yinghua' 'Fan, Weibin' 'Zhang, Zilong' 'Xie, Xingkun' 'Xiang, Shiqun' 'Huang, Deguang' _publ_section_title ; Copper(II)-hydroxide facilitated C-C bond formation: the carboxamido pyridine system versus the methylimino pyridine system. ; _journal_issue 35 _journal_name_full 'Dalton transactions (Cambridge, England : 2003)' _journal_page_first 12189 _journal_page_last 12196 _journal_paper_doi 10.1039/d0dt02288h _journal_volume 49 _journal_year 2020 _chemical_formula_moiety 'C46 H42 Cu2 N6 O4, 2(C8 H20 N), C2 H3 N' _chemical_formula_sum 'C64 H85 Cu2 N9 O4' _chemical_formula_weight 1171.48 _chemical_name_common '[Cu2(NNN-pincer)2] (Et4N)2 MeCN' _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _audit_creation_method SHELXL-2018/3 _audit_update_record ; 2020-07-20 deposited with the CCDC. 2020-08-17 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 105.8272(11) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.36064(14) _cell_length_b 16.83191(16) _cell_length_c 25.6876(3) _cell_measurement_reflns_used 21440 _cell_measurement_temperature 100(2) _cell_measurement_theta_max 73.3520 _cell_measurement_theta_min 4.4110 _cell_volume 5973.73(11) _computing_cell_refinement 'CrysAlisPro, Agilent Technologies' _computing_data_collection 'CrysAlisPro, Agilent Technologies' _computing_data_reduction 'CrysAlisPro, Agilent Technologies' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-2018/3 (Sheldrick, 2018)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _diffrn_ambient_temperature 100(2) _diffrn_detector_area_resol_mean 10.5594 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54184 _diffrn_reflns_av_R_equivalents 0.0436 _diffrn_reflns_av_unetI/netI 0.0325 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_number 47190 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 67.684 _diffrn_reflns_theta_max 70.987 _diffrn_reflns_theta_min 3.577 _diffrn_source 'SuperNova (Cu) X-ray Source' _exptl_absorpt_coefficient_mu 1.307 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.82306 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies,Version 1.171.36.28 Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour black-red _exptl_crystal_density_diffrn 1.303 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 2488 _exptl_crystal_size_max 0.150 _exptl_crystal_size_mid 0.130 _exptl_crystal_size_min 0.030 _refine_diff_density_max 0.856 _refine_diff_density_min -0.628 _refine_diff_density_rms 0.074 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 713 _refine_ls_number_reflns 11522 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.065 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0452 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0692P)^2^+5.8501P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1247 _refine_ls_wR_factor_ref 0.1294 _reflns_Friedel_coverage 0.000 _reflns_number_gt 10192 _reflns_number_total 11522 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d0dt02288h2.cif _cod_data_source_block Complex3 _cod_depositor_comments 'Adding full bibliography for 7705173--7705180.cif.' _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7705178 _shelx_shelxl_version_number 2018/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.828 _shelx_estimated_absorpt_t_max 0.962 _shelx_res_file ; TITL DH237-1 in P21/n #14 full.res created by SHELXL-2018/3 at 11:40:39 on 20-Jul-2020 CELL 1.54184 14.36064 16.83191 25.6876 90 105.8272 90 ZERR 4 0.00014 0.00016 0.00028 0 0.0011 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H Cu N O UNIT 256 340 8 36 16 TEMP -173 SIZE 0.15 0.13 0.03 REM black-red prism OMIT 0 142 L.S. 10 PLAN 2 BOND $H CONF fmap 2 acta WGHT 0.069200 5.850101 FVAR 2.71955 CU1 3 0.522043 0.767919 0.065423 11.00000 0.01618 0.01366 = 0.01074 -0.00253 0.00223 -0.00257 CU2 3 0.348687 0.764057 0.095744 11.00000 0.01199 0.01362 = 0.01401 0.00241 0.00339 0.00101 O1 5 0.590048 0.944794 0.172201 11.00000 0.02118 0.02164 = 0.02351 -0.01047 -0.00157 0.00065 O2 5 0.130995 0.901199 0.001249 11.00000 0.01318 0.03076 = 0.02469 0.00940 0.00087 0.00630 O3 5 0.395922 0.600556 -0.041822 11.00000 0.01974 0.01664 = 0.01779 -0.00557 0.00307 -0.00311 O4 5 0.385326 0.619604 0.228294 11.00000 0.02757 0.02251 = 0.01613 0.00548 0.00709 0.00274 N1 4 0.584136 0.827902 0.125404 11.00000 0.01344 0.01423 = 0.01263 -0.00036 0.00108 -0.00054 N2 4 0.378232 0.880133 0.078759 11.00000 0.01461 0.01424 = 0.01144 -0.00078 0.00458 0.00120 N3 4 0.212766 0.792926 0.048099 11.00000 0.01019 0.02007 = 0.01421 -0.00006 0.00258 -0.00030 N4 4 0.470249 0.712726 0.001642 11.00000 0.02085 0.01645 = 0.01152 -0.00144 0.00426 -0.00429 N5 4 0.404712 0.649715 0.093524 11.00000 0.01033 0.01344 = 0.01457 -0.00060 0.00278 -0.00093 N6 4 0.336507 0.725925 0.169676 11.00000 0.01221 0.01688 = 0.01274 0.00065 0.00467 -0.00026 N7 4 -0.085084 0.876109 -0.121635 11.00000 0.01417 0.02661 = 0.01945 0.00263 0.00478 0.00163 N8 4 0.217997 0.503389 -0.181448 11.00000 0.01556 0.01879 = 0.01813 0.00442 0.00277 0.00185 N9 4 -0.021180 0.563467 -0.127333 11.00000 0.03376 0.06093 = 0.04012 -0.00752 0.01347 -0.00402 C1 1 0.550058 0.898009 0.135249 11.00000 0.01405 0.01585 = 0.01374 -0.00056 0.00323 -0.00178 C2 1 0.457854 0.926249 0.094708 11.00000 0.01643 0.01321 = 0.01430 -0.00206 0.00344 -0.00037 C3 1 0.462130 1.003206 0.075666 11.00000 0.02303 0.01678 = 0.02664 0.00059 0.00175 -0.00366 AFIX 43 H3A 2 0.519302 1.033993 0.088276 11.00000 -1.20000 AFIX 0 C4 1 0.382573 1.034352 0.038311 11.00000 0.02811 0.01539 = 0.02978 0.00565 0.00199 -0.00028 AFIX 43 H4A 2 0.384808 1.085887 0.023619 11.00000 -1.20000 AFIX 0 C5 1 0.299269 0.988634 0.022724 11.00000 0.02119 0.01813 = 0.02110 0.00335 0.00264 0.00502 AFIX 43 H5A 2 0.242948 1.008937 -0.002390 11.00000 -1.20000 AFIX 0 C6 1 0.298849 0.912975 0.044111 11.00000 0.01458 0.01595 = 0.01350 0.00032 0.00476 0.00293 C7 1 0.205160 0.865820 0.029141 11.00000 0.01334 0.02213 = 0.01269 0.00048 0.00354 0.00221 C8 1 0.127230 0.748768 0.044784 11.00000 0.01064 0.02355 = 0.01424 0.00209 0.00237 -0.00011 C9 1 0.111752 0.676381 0.016548 11.00000 0.01457 0.02739 = 0.01884 -0.00288 0.00427 -0.00263 C10 1 0.032413 0.629430 0.018063 11.00000 0.02150 0.02977 = 0.02669 -0.00891 0.00718 -0.00983 AFIX 43 H10A 2 0.022174 0.580373 -0.000937 11.00000 -1.20000 AFIX 0 C11 1 -0.031894 0.653152 0.046871 11.00000 0.01778 0.03705 = 0.02855 -0.00107 0.00852 -0.01067 AFIX 43 H11A 2 -0.085362 0.620504 0.047832 11.00000 -1.20000 AFIX 0 C12 1 -0.016995 0.724919 0.074115 11.00000 0.01606 0.03367 = 0.02475 0.00111 0.01015 -0.00121 AFIX 43 H12A 2 -0.061140 0.741361 0.093612 11.00000 -1.20000 AFIX 0 C13 1 0.061294 0.773761 0.073664 11.00000 0.01345 0.02582 = 0.01858 0.00189 0.00564 0.00195 C14 1 0.075400 0.851119 0.103848 11.00000 0.01912 0.02853 = 0.02534 -0.00403 0.01120 0.00092 AFIX 33 H14A 2 0.133380 0.877686 0.099274 11.00000 -1.50000 H14B 2 0.018824 0.885176 0.089608 11.00000 -1.50000 H14C 2 0.083209 0.841015 0.142375 11.00000 -1.50000 AFIX 0 C15 1 0.178760 0.649605 -0.015951 11.00000 0.02209 0.03563 = 0.02879 -0.01311 0.01166 -0.00673 AFIX 33 H15A 2 0.230279 0.688989 -0.012754 11.00000 -1.50000 H15B 2 0.207368 0.598278 -0.002232 11.00000 -1.50000 H15C 2 0.142275 0.644112 -0.054032 11.00000 -1.50000 AFIX 0 C16 1 0.678355 0.807714 0.158767 11.00000 0.01338 0.01418 = 0.01249 -0.00268 0.00288 -0.00051 C17 1 0.760066 0.834040 0.143589 11.00000 0.01921 0.01891 = 0.01770 -0.00495 0.00829 -0.00465 C18 1 0.851934 0.815127 0.176429 11.00000 0.01454 0.02674 = 0.02862 -0.00845 0.01072 -0.00233 AFIX 43 H18A 2 0.907613 0.832183 0.166318 11.00000 -1.20000 AFIX 0 C19 1 0.863032 0.771847 0.223540 11.00000 0.01228 0.02713 = 0.02609 -0.00559 0.00101 0.00544 AFIX 43 H19A 2 0.925944 0.760730 0.246158 11.00000 -1.20000 AFIX 0 C20 1 0.782073 0.744811 0.237579 11.00000 0.01881 0.01931 = 0.01670 -0.00075 0.00111 0.00554 AFIX 43 H20A 2 0.789977 0.714502 0.269691 11.00000 -1.20000 AFIX 0 C21 1 0.688877 0.761462 0.205191 11.00000 0.01563 0.01628 = 0.01366 -0.00195 0.00421 0.00179 C22 1 0.601662 0.730343 0.220243 11.00000 0.01945 0.02587 = 0.01949 0.00550 0.00649 -0.00153 AFIX 33 H22A 2 0.622609 0.699373 0.253714 11.00000 -1.50000 H22B 2 0.561584 0.774995 0.225740 11.00000 -1.50000 H22C 2 0.563899 0.696362 0.191094 11.00000 -1.50000 AFIX 0 C23 1 0.748148 0.882076 0.092949 11.00000 0.02883 0.03303 = 0.02276 0.00209 0.01077 -0.00992 AFIX 33 H23A 2 0.679085 0.889476 0.075199 11.00000 -1.50000 H23B 2 0.779052 0.934023 0.102200 11.00000 -1.50000 H23C 2 0.778529 0.854087 0.068390 11.00000 -1.50000 AFIX 0 C24 1 0.427333 0.642222 -0.000682 11.00000 0.01053 0.01482 = 0.01588 -0.00172 0.00438 0.00105 C25 1 0.423896 0.605980 0.053272 11.00000 0.01049 0.01390 = 0.01778 -0.00048 0.00442 -0.00132 C26 1 0.442861 0.524880 0.058541 11.00000 0.01854 0.01571 = 0.02622 -0.00243 0.01089 0.00054 AFIX 43 H26A 2 0.453256 0.495604 0.029006 11.00000 -1.20000 AFIX 0 C27 1 0.446568 0.486882 0.106869 11.00000 0.01970 0.01331 = 0.02944 0.00449 0.00878 0.00266 AFIX 43 H27A 2 0.461363 0.431873 0.111398 11.00000 -1.20000 AFIX 0 C28 1 0.428199 0.531009 0.148359 11.00000 0.01542 0.01734 = 0.02102 0.00418 0.00506 0.00058 AFIX 43 H28A 2 0.430766 0.506788 0.182126 11.00000 -1.20000 AFIX 0 C29 1 0.405877 0.611400 0.140125 11.00000 0.01001 0.01580 = 0.01589 0.00112 0.00238 -0.00138 C30 1 0.375211 0.655264 0.184308 11.00000 0.01280 0.01741 = 0.01596 0.00045 0.00352 -0.00282 C31 1 0.282054 0.760354 0.202236 11.00000 0.01326 0.02128 = 0.01337 0.00243 0.00483 0.00192 C32 1 0.305278 0.836047 0.225162 11.00000 0.02011 0.02308 = 0.01393 0.00070 0.00318 0.00395 C33 1 0.245645 0.870618 0.253794 11.00000 0.03321 0.02971 = 0.02004 -0.00339 0.00823 0.00901 AFIX 43 H33A 2 0.261055 0.921880 0.269211 11.00000 -1.20000 AFIX 0 C34 1 0.164513 0.831497 0.260092 11.00000 0.03291 0.04625 = 0.02751 0.00167 0.01952 0.01345 AFIX 43 H34A 2 0.125169 0.855315 0.280100 11.00000 -1.20000 AFIX 0 C35 1 0.141444 0.757308 0.236896 11.00000 0.02034 0.04306 = 0.03050 0.00687 0.01506 0.00455 AFIX 43 H35A 2 0.085462 0.730758 0.240947 11.00000 -1.20000 AFIX 0 C36 1 0.198178 0.720674 0.207811 11.00000 0.01752 0.02787 = 0.02072 0.00563 0.00892 0.00049 C37 1 0.168619 0.641932 0.181295 11.00000 0.01794 0.03277 = 0.03079 0.00377 0.00854 -0.00748 AFIX 33 H37A 2 0.216323 0.624801 0.162663 11.00000 -1.50000 H37B 2 0.165187 0.602598 0.208839 11.00000 -1.50000 H37C 2 0.105005 0.646874 0.155033 11.00000 -1.50000 AFIX 0 C38 1 0.393640 0.879410 0.219775 11.00000 0.02689 0.02034 = 0.02109 -0.00372 0.00448 -0.00369 AFIX 33 H38A 2 0.426972 0.847081 0.198679 11.00000 -1.50000 H38B 2 0.374316 0.930186 0.201321 11.00000 -1.50000 H38C 2 0.437260 0.889244 0.255812 11.00000 -1.50000 AFIX 0 C39 1 0.483848 0.742887 -0.048097 11.00000 0.02627 0.01634 = 0.01154 -0.00515 0.00535 -0.00805 C40 1 0.571195 0.727075 -0.060456 11.00000 0.03016 0.01907 = 0.01830 -0.00449 0.00976 -0.00706 C41 1 0.585563 0.756930 -0.108463 11.00000 0.03861 0.03248 = 0.02351 -0.00684 0.01687 -0.01234 AFIX 43 H41A 2 0.643784 0.745065 -0.117661 11.00000 -1.20000 AFIX 0 C42 1 0.515887 0.803515 -0.142639 11.00000 0.05551 0.03114 = 0.01366 -0.00056 0.01132 -0.01874 AFIX 43 H42A 2 0.526231 0.823534 -0.175190 11.00000 -1.20000 AFIX 0 C43 1 0.431660 0.820848 -0.129503 11.00000 0.04322 0.02147 = 0.01393 0.00029 -0.00206 -0.01073 AFIX 43 H43A 2 0.384547 0.853545 -0.153014 11.00000 -1.20000 AFIX 0 C44 1 0.413700 0.791346 -0.082164 11.00000 0.03061 0.01816 = 0.01268 -0.00429 -0.00005 -0.00818 C45 1 0.322359 0.814043 -0.068027 11.00000 0.03416 0.03174 = 0.02342 -0.00321 0.00043 0.00094 AFIX 33 H45A 2 0.321180 0.788488 -0.033934 11.00000 -1.50000 H45B 2 0.320130 0.871861 -0.064035 11.00000 -1.50000 H45C 2 0.266201 0.796584 -0.096894 11.00000 -1.50000 AFIX 0 C46 1 0.650070 0.681405 -0.021433 11.00000 0.02949 0.02828 = 0.03019 -0.00120 0.01377 0.00108 AFIX 33 H46A 2 0.627728 0.665085 0.009754 11.00000 -1.50000 H46B 2 0.666412 0.634202 -0.039474 11.00000 -1.50000 H46C 2 0.707496 0.715151 -0.009137 11.00000 -1.50000 AFIX 0 C47 1 -0.090947 0.909081 -0.066704 11.00000 0.02279 0.03691 = 0.02172 -0.00362 0.00605 0.00403 AFIX 23 H47A 2 -0.024525 0.920120 -0.044059 11.00000 -1.20000 H47B 2 -0.126497 0.960136 -0.072853 11.00000 -1.20000 AFIX 0 C48 1 -0.140252 0.853924 -0.035962 11.00000 0.03286 0.04781 = 0.02727 0.00684 0.01273 0.01003 AFIX 33 H48A 2 -0.141326 0.878695 -0.001605 11.00000 -1.50000 H48B 2 -0.206726 0.843721 -0.057607 11.00000 -1.50000 H48C 2 -0.104620 0.803652 -0.028775 11.00000 -1.50000 AFIX 0 C49 1 -0.021065 0.803532 -0.110471 11.00000 0.02702 0.02674 = 0.02735 0.00149 0.00632 0.00458 AFIX 23 H49A 2 -0.052800 0.762268 -0.093795 11.00000 -1.20000 H49B 2 0.040785 0.817688 -0.083933 11.00000 -1.20000 AFIX 0 C50 1 0.000576 0.769092 -0.160170 11.00000 0.05147 0.03545 = 0.03364 -0.00431 0.01396 0.00903 AFIX 33 H50A 2 0.042276 0.722364 -0.149950 11.00000 -1.50000 H50B 2 -0.060099 0.753533 -0.186349 11.00000 -1.50000 H50C 2 0.033600 0.809022 -0.176476 11.00000 -1.50000 AFIX 0 C51 1 -0.041945 0.940791 -0.149448 11.00000 0.02590 0.02575 = 0.02862 -0.00123 0.00873 -0.00167 AFIX 23 H51A 2 -0.048903 0.924143 -0.187283 11.00000 -1.20000 H51B 2 -0.080702 0.989747 -0.150692 11.00000 -1.20000 AFIX 0 C52 1 0.062935 0.960899 -0.123842 11.00000 0.03023 0.04265 = 0.03558 0.00282 0.00827 -0.00924 AFIX 33 H52A 2 0.083215 1.002912 -0.144805 11.00000 -1.50000 H52B 2 0.070917 0.979327 -0.086691 11.00000 -1.50000 H52C 2 0.102813 0.913523 -0.123394 11.00000 -1.50000 AFIX 0 C53 1 -0.184004 0.856183 -0.158207 11.00000 0.01756 0.03472 = 0.02427 -0.00698 0.00452 -0.00499 AFIX 23 H53A 2 -0.176912 0.841875 -0.194313 11.00000 -1.20000 H53B 2 -0.208807 0.808749 -0.143514 11.00000 -1.20000 AFIX 0 C54 1 -0.258162 0.921443 -0.165131 11.00000 0.01866 0.04717 = 0.03187 0.00508 0.00496 0.00637 AFIX 33 H54A 2 -0.319659 0.903294 -0.189339 11.00000 -1.50000 H54B 2 -0.267520 0.935146 -0.129821 11.00000 -1.50000 H54C 2 -0.235553 0.968348 -0.180736 11.00000 -1.50000 AFIX 0 C55 1 0.318418 0.496401 -0.188285 11.00000 0.02136 0.04171 = 0.03623 0.01749 0.01388 0.00953 AFIX 23 H55A 2 0.340731 0.440877 -0.180686 11.00000 -1.20000 H55B 2 0.362415 0.530751 -0.161113 11.00000 -1.20000 AFIX 0 C56 1 0.326550 0.519152 -0.244152 11.00000 0.03450 0.05833 = 0.04507 0.02655 0.02541 0.01354 AFIX 33 H56A 2 0.393800 0.513048 -0.245350 11.00000 -1.50000 H56B 2 0.284687 0.484527 -0.271361 11.00000 -1.50000 H56C 2 0.306406 0.574547 -0.251756 11.00000 -1.50000 AFIX 0 C57 1 0.150690 0.449630 -0.222377 11.00000 0.03209 0.01641 = 0.01890 0.00108 0.00376 -0.00006 AFIX 23 H57A 2 0.141011 0.472941 -0.258852 11.00000 -1.20000 H57B 2 0.182706 0.397500 -0.222185 11.00000 -1.20000 AFIX 0 C58 1 0.052633 0.436108 -0.212757 11.00000 0.02534 0.02788 = 0.03489 -0.00373 -0.00203 -0.00527 AFIX 33 H58A 2 0.014155 0.400938 -0.240897 11.00000 -1.50000 H58B 2 0.060982 0.411511 -0.177198 11.00000 -1.50000 H58C 2 0.019201 0.487109 -0.213941 11.00000 -1.50000 AFIX 0 C59 1 0.179499 0.587772 -0.191287 11.00000 0.02124 0.01670 = 0.02200 0.00173 0.00236 0.00019 AFIX 23 H59A 2 0.168756 0.600505 -0.230105 11.00000 -1.20000 H59B 2 0.115969 0.590296 -0.183225 11.00000 -1.20000 AFIX 0 C60 1 0.245145 0.650474 -0.158024 11.00000 0.03982 0.02201 = 0.02291 0.00097 0.00039 -0.00810 AFIX 33 H60A 2 0.215306 0.702920 -0.166684 11.00000 -1.50000 H60B 2 0.254866 0.639426 -0.119451 11.00000 -1.50000 H60C 2 0.307744 0.649653 -0.166411 11.00000 -1.50000 AFIX 0 C61 1 0.221531 0.479998 -0.123610 11.00000 0.02123 0.02584 = 0.01753 0.00587 0.00461 -0.00014 AFIX 23 H61A 2 0.268245 0.515031 -0.098402 11.00000 -1.20000 H61B 2 0.156994 0.489386 -0.117875 11.00000 -1.20000 AFIX 0 C62 1 0.250062 0.394399 -0.109601 11.00000 0.03378 0.03155 = 0.02651 0.01389 0.00835 0.00601 AFIX 33 H62A 2 0.250689 0.384008 -0.071969 11.00000 -1.50000 H62B 2 0.203268 0.359052 -0.133636 11.00000 -1.50000 H62C 2 0.314694 0.384737 -0.114133 11.00000 -1.50000 AFIX 0 C63 1 -0.090004 0.552539 -0.114496 11.00000 0.02980 0.04523 = 0.02856 -0.00772 0.00606 0.00064 C64 1 -0.177453 0.539109 -0.097546 11.00000 0.03283 0.06963 = 0.04855 -0.00731 0.01776 -0.00556 AFIX 137 H64A 2 -0.180625 0.483188 -0.087547 11.00000 -1.50000 H64B 2 -0.234253 0.552244 -0.127375 11.00000 -1.50000 H64C 2 -0.176396 0.572847 -0.066297 11.00000 -1.50000 AFIX 0 HKLF 4 REM DH237-1 in P21/n #14 REM wR2 = 0.1294, GooF = S = 1.065, Restrained GooF = 1.065 for all data REM R1 = 0.0452 for 10192 Fo > 4sig(Fo) and 0.0509 for all 11522 data REM 713 parameters refined using 0 restraints END WGHT 0.0692 5.8505 REM Highest difference peak 0.856, deepest hole -0.628, 1-sigma level 0.074 Q1 1 -0.0607 0.9582 0.0083 11.00000 0.05 0.86 Q2 1 -0.0434 0.7999 -0.1542 11.00000 0.05 0.81 ; _shelx_res_checksum 56528 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' 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 0.52204(2) 0.76792(2) 0.06542(2) 0.01381(9) Uani 1 1 d . . . . . Cu2 Cu 0.34869(2) 0.76406(2) 0.09574(2) 0.01324(9) Uani 1 1 d . . . . . O1 O 0.59005(11) 0.94479(10) 0.17220(7) 0.0236(3) Uani 1 1 d . . . . . O2 O 0.13099(11) 0.90120(10) 0.00125(7) 0.0237(3) Uani 1 1 d . . . . . O3 O 0.39592(11) 0.60056(9) -0.04182(6) 0.0185(3) Uani 1 1 d . . . . . O4 O 0.38533(12) 0.61960(10) 0.22829(6) 0.0218(3) Uani 1 1 d . . . . . N1 N 0.58414(12) 0.82790(10) 0.12540(7) 0.0139(3) Uani 1 1 d . . . . . N2 N 0.37823(12) 0.88013(10) 0.07876(7) 0.0132(3) Uani 1 1 d . . . . . N3 N 0.21277(12) 0.79293(11) 0.04810(7) 0.0150(3) Uani 1 1 d . . . . . N4 N 0.47025(13) 0.71273(11) 0.00164(7) 0.0163(3) Uani 1 1 d . . . . . N5 N 0.40471(11) 0.64972(10) 0.09352(7) 0.0129(3) Uani 1 1 d . . . . . N6 N 0.33651(12) 0.72593(10) 0.16968(7) 0.0137(3) Uani 1 1 d . . . . . N7 N -0.08508(13) 0.87611(12) -0.12163(8) 0.0200(4) Uani 1 1 d . . . . . N8 N 0.21800(13) 0.50339(11) -0.18145(8) 0.0179(4) Uani 1 1 d . . . . . N9 N -0.02118(18) 0.56347(18) -0.12733(11) 0.0443(6) Uani 1 1 d . . . . . C1 C 0.55006(14) 0.89801(12) 0.13525(8) 0.0147(4) Uani 1 1 d . . . . . C2 C 0.45785(15) 0.92625(12) 0.09471(8) 0.0148(4) Uani 1 1 d . . . . . C3 C 0.46213(17) 1.00321(14) 0.07567(10) 0.0231(5) Uani 1 1 d . . . . . H3A H 0.519302 1.033993 0.088276 0.028 Uiso 1 1 calc R U . . . C4 C 0.38257(18) 1.03435(14) 0.03831(10) 0.0256(5) Uani 1 1 d . . . . . H4A H 0.384808 1.085887 0.023619 0.031 Uiso 1 1 calc R U . . . C5 C 0.29927(16) 0.98863(13) 0.02272(9) 0.0208(4) Uani 1 1 d . . . . . H5A H 0.242948 1.008937 -0.002390 0.025 Uiso 1 1 calc R U . . . C6 C 0.29885(14) 0.91298(12) 0.04411(8) 0.0145(4) Uani 1 1 d . . . . . C7 C 0.20516(14) 0.86582(13) 0.02914(8) 0.0161(4) Uani 1 1 d . . . . . C8 C 0.12723(15) 0.74877(14) 0.04478(9) 0.0163(4) Uani 1 1 d . . . . . C9 C 0.11175(15) 0.67638(14) 0.01655(9) 0.0203(4) Uani 1 1 d . . . . . C10 C 0.03241(17) 0.62943(15) 0.01806(10) 0.0259(5) Uani 1 1 d . . . . . H10A H 0.022174 0.580373 -0.000937 0.031 Uiso 1 1 calc R U . . . C11 C -0.03189(17) 0.65315(16) 0.04687(10) 0.0274(5) Uani 1 1 d . . . . . H11A H -0.085362 0.620504 0.047832 0.033 Uiso 1 1 calc R U . . . C12 C -0.01699(17) 0.72492(15) 0.07412(10) 0.0239(5) Uani 1 1 d . . . . . H12A H -0.061140 0.741361 0.093612 0.029 Uiso 1 1 calc R U . . . C13 C 0.06129(15) 0.77376(14) 0.07366(9) 0.0190(4) Uani 1 1 d . . . . . C14 C 0.07540(16) 0.85112(14) 0.10385(10) 0.0233(5) Uani 1 1 d . . . . . H14A H 0.133380 0.877686 0.099274 0.035 Uiso 1 1 calc R U . . . H14B H 0.018824 0.885176 0.089608 0.035 Uiso 1 1 calc R U . . . H14C H 0.083209 0.841015 0.142375 0.035 Uiso 1 1 calc R U . . . C15 C 0.17876(17) 0.64961(16) -0.01595(11) 0.0279(5) Uani 1 1 d . . . . . H15A H 0.230279 0.688989 -0.012754 0.042 Uiso 1 1 calc R U . . . H15B H 0.207368 0.598278 -0.002232 0.042 Uiso 1 1 calc R U . . . H15C H 0.142275 0.644112 -0.054032 0.042 Uiso 1 1 calc R U . . . C16 C 0.67836(14) 0.80771(12) 0.15877(8) 0.0135(4) Uani 1 1 d . . . . . C17 C 0.76007(16) 0.83404(13) 0.14359(9) 0.0180(4) Uani 1 1 d . . . . . C18 C 0.85193(16) 0.81513(14) 0.17643(10) 0.0224(5) Uani 1 1 d . . . . . H18A H 0.907613 0.832183 0.166318 0.027 Uiso 1 1 calc R U . . . C19 C 0.86303(16) 0.77185(14) 0.22354(10) 0.0227(5) Uani 1 1 d . . . . . H19A H 0.925944 0.760730 0.246158 0.027 Uiso 1 1 calc R U . . . C20 C 0.78207(16) 0.74481(13) 0.23758(9) 0.0190(4) Uani 1 1 d . . . . . H20A H 0.789977 0.714502 0.269691 0.023 Uiso 1 1 calc R U . . . C21 C 0.68888(15) 0.76146(12) 0.20519(9) 0.0151(4) Uani 1 1 d . . . . . C22 C 0.60166(16) 0.73034(14) 0.22024(9) 0.0214(5) Uani 1 1 d . . . . . H22A H 0.622609 0.699373 0.253714 0.032 Uiso 1 1 calc R U . . . H22B H 0.561584 0.774995 0.225740 0.032 Uiso 1 1 calc R U . . . H22C H 0.563899 0.696362 0.191094 0.032 Uiso 1 1 calc R U . . . C23 C 0.74815(18) 0.88208(16) 0.09295(10) 0.0275(5) Uani 1 1 d . . . . . H23A H 0.679085 0.889476 0.075199 0.041 Uiso 1 1 calc R U . . . H23B H 0.779052 0.934023 0.102200 0.041 Uiso 1 1 calc R U . . . H23C H 0.778529 0.854087 0.068390 0.041 Uiso 1 1 calc R U . . . C24 C 0.42733(14) 0.64222(12) -0.00068(8) 0.0136(4) Uani 1 1 d . . . . . C25 C 0.42390(14) 0.60598(12) 0.05327(9) 0.0139(4) Uani 1 1 d . . . . . C26 C 0.44286(15) 0.52488(13) 0.05854(10) 0.0192(4) Uani 1 1 d . . . . . H26A H 0.453256 0.495604 0.029006 0.023 Uiso 1 1 calc R U . . . C27 C 0.44657(16) 0.48688(13) 0.10687(10) 0.0204(4) Uani 1 1 d . . . . . H27A H 0.461363 0.431873 0.111398 0.024 Uiso 1 1 calc R U . . . C28 C 0.42820(15) 0.53101(13) 0.14836(9) 0.0179(4) Uani 1 1 d . . . . . H28A H 0.430766 0.506788 0.182126 0.021 Uiso 1 1 calc R U . . . C29 C 0.40588(14) 0.61140(12) 0.14013(8) 0.0141(4) Uani 1 1 d . . . . . C30 C 0.37521(14) 0.65526(13) 0.18431(9) 0.0155(4) Uani 1 1 d . . . . . C31 C 0.28205(15) 0.76035(13) 0.20224(9) 0.0157(4) Uani 1 1 d . . . . . C32 C 0.30528(16) 0.83605(14) 0.22516(9) 0.0193(4) Uani 1 1 d . . . . . C33 C 0.24565(19) 0.87062(16) 0.25379(10) 0.0275(5) Uani 1 1 d . . . . . H33A H 0.261055 0.921880 0.269211 0.033 Uiso 1 1 calc R U . . . C34 C 0.1645(2) 0.83150(18) 0.26009(11) 0.0333(6) Uani 1 1 d . . . . . H34A H 0.125169 0.855315 0.280100 0.040 Uiso 1 1 calc R U . . . C35 C 0.14144(18) 0.75731(17) 0.23690(11) 0.0297(6) Uani 1 1 d . . . . . H35A H 0.085462 0.730758 0.240947 0.036 Uiso 1 1 calc R U . . . C36 C 0.19818(16) 0.72067(14) 0.20781(9) 0.0213(5) Uani 1 1 d . . . . . C37 C 0.16862(17) 0.64193(15) 0.18130(11) 0.0268(5) Uani 1 1 d . . . . . H37A H 0.216323 0.624801 0.162663 0.040 Uiso 1 1 calc R U . . . H37B H 0.165187 0.602598 0.208839 0.040 Uiso 1 1 calc R U . . . H37C H 0.105005 0.646874 0.155033 0.040 Uiso 1 1 calc R U . . . C38 C 0.39364(17) 0.87941(14) 0.21977(10) 0.0232(5) Uani 1 1 d . . . . . H38A H 0.426972 0.847081 0.198679 0.035 Uiso 1 1 calc R U . . . H38B H 0.374316 0.930186 0.201321 0.035 Uiso 1 1 calc R U . . . H38C H 0.437260 0.889244 0.255812 0.035 Uiso 1 1 calc R U . . . C39 C 0.48385(17) 0.74289(13) -0.04810(9) 0.0180(4) Uani 1 1 d . . . . . C40 C 0.57120(18) 0.72707(13) -0.06046(10) 0.0219(5) Uani 1 1 d . . . . . C41 C 0.5856(2) 0.75693(16) -0.10846(11) 0.0299(6) Uani 1 1 d . . . . . H41A H 0.643784 0.745065 -0.117661 0.036 Uiso 1 1 calc R U . . . C42 C 0.5159(2) 0.80351(16) -0.14264(10) 0.0331(6) Uani 1 1 d . . . . . H42A H 0.526231 0.823534 -0.175190 0.040 Uiso 1 1 calc R U . . . C43 C 0.4317(2) 0.82085(15) -0.12950(9) 0.0281(5) Uani 1 1 d . . . . . H43A H 0.384547 0.853545 -0.153014 0.034 Uiso 1 1 calc R U . . . C44 C 0.41370(17) 0.79135(14) -0.08216(9) 0.0217(5) Uani 1 1 d . . . . . C45 C 0.32236(19) 0.81404(16) -0.06803(11) 0.0312(5) Uani 1 1 d . . . . . H45A H 0.321180 0.788488 -0.033934 0.047 Uiso 1 1 calc R U . . . H45B H 0.320130 0.871861 -0.064035 0.047 Uiso 1 1 calc R U . . . H45C H 0.266201 0.796584 -0.096894 0.047 Uiso 1 1 calc R U . . . C46 C 0.65007(18) 0.68140(15) -0.02143(11) 0.0282(5) Uani 1 1 d . . . . . H46A H 0.627728 0.665085 0.009754 0.042 Uiso 1 1 calc R U . . . H46B H 0.666412 0.634202 -0.039474 0.042 Uiso 1 1 calc R U . . . H46C H 0.707496 0.715151 -0.009137 0.042 Uiso 1 1 calc R U . . . C47 C -0.09095(18) 0.90908(16) -0.06670(10) 0.0271(5) Uani 1 1 d . . . . . H47A H -0.024525 0.920120 -0.044059 0.033 Uiso 1 1 calc R U . . . H47B H -0.126497 0.960136 -0.072853 0.033 Uiso 1 1 calc R U . . . C48 C -0.1403(2) 0.85392(19) -0.03596(11) 0.0351(6) Uani 1 1 d . . . . . H48A H -0.141326 0.878695 -0.001605 0.053 Uiso 1 1 calc R U . . . H48B H -0.206726 0.843721 -0.057607 0.053 Uiso 1 1 calc R U . . . H48C H -0.104620 0.803652 -0.028775 0.053 Uiso 1 1 calc R U . . . C49 C -0.02106(18) 0.80353(15) -0.11047(10) 0.0272(5) Uani 1 1 d . . . . . H49A H -0.052800 0.762268 -0.093795 0.033 Uiso 1 1 calc R U . . . H49B H 0.040785 0.817688 -0.083933 0.033 Uiso 1 1 calc R U . . . C50 C 0.0006(2) 0.76909(18) -0.16017(13) 0.0397(7) Uani 1 1 d . . . . . H50A H 0.042276 0.722364 -0.149950 0.060 Uiso 1 1 calc R U . . . H50B H -0.060099 0.753533 -0.186349 0.060 Uiso 1 1 calc R U . . . H50C H 0.033600 0.809022 -0.176476 0.060 Uiso 1 1 calc R U . . . C51 C -0.04194(18) 0.94079(15) -0.14945(10) 0.0265(5) Uani 1 1 d . . . . . H51A H -0.048903 0.924143 -0.187283 0.032 Uiso 1 1 calc R U . . . H51B H -0.080702 0.989747 -0.150692 0.032 Uiso 1 1 calc R U . . . C52 C 0.0629(2) 0.96090(18) -0.12384(12) 0.0363(6) Uani 1 1 d . . . . . H52A H 0.083215 1.002912 -0.144805 0.054 Uiso 1 1 calc R U . . . H52B H 0.070917 0.979327 -0.086691 0.054 Uiso 1 1 calc R U . . . H52C H 0.102813 0.913523 -0.123394 0.054 Uiso 1 1 calc R U . . . C53 C -0.18400(16) 0.85618(16) -0.15821(10) 0.0258(5) Uani 1 1 d . . . . . H53A H -0.176912 0.841875 -0.194313 0.031 Uiso 1 1 calc R U . . . H53B H -0.208807 0.808749 -0.143514 0.031 Uiso 1 1 calc R U . . . C54 C -0.25816(18) 0.92144(18) -0.16513(11) 0.0329(6) Uani 1 1 d . . . . . H54A H -0.319659 0.903294 -0.189339 0.049 Uiso 1 1 calc R U . . . H54B H -0.267520 0.935146 -0.129821 0.049 Uiso 1 1 calc R U . . . H54C H -0.235553 0.968348 -0.180736 0.049 Uiso 1 1 calc R U . . . C55 C 0.31842(18) 0.49640(17) -0.18829(11) 0.0319(6) Uani 1 1 d . . . . . H55A H 0.340731 0.440877 -0.180686 0.038 Uiso 1 1 calc R U . . . H55B H 0.362415 0.530751 -0.161113 0.038 Uiso 1 1 calc R U . . . C56 C 0.3266(2) 0.5192(2) -0.24415(13) 0.0431(8) Uani 1 1 d . . . . . H56A H 0.393800 0.513048 -0.245350 0.065 Uiso 1 1 calc R U . . . H56B H 0.284687 0.484527 -0.271361 0.065 Uiso 1 1 calc R U . . . H56C H 0.306406 0.574547 -0.251756 0.065 Uiso 1 1 calc R U . . . C57 C 0.15069(18) 0.44963(14) -0.22238(9) 0.0231(5) Uani 1 1 d . . . . . H57A H 0.141011 0.472941 -0.258852 0.028 Uiso 1 1 calc R U . . . H57B H 0.182706 0.397500 -0.222185 0.028 Uiso 1 1 calc R U . . . C58 C 0.05263(18) 0.43611(16) -0.21276(11) 0.0314(6) Uani 1 1 d . . . . . H58A H 0.014155 0.400938 -0.240897 0.047 Uiso 1 1 calc R U . . . H58B H 0.060982 0.411511 -0.177198 0.047 Uiso 1 1 calc R U . . . H58C H 0.019201 0.487109 -0.213941 0.047 Uiso 1 1 calc R U . . . C59 C 0.17950(16) 0.58777(13) -0.19129(9) 0.0207(4) Uani 1 1 d . . . . . H59A H 0.168756 0.600505 -0.230105 0.025 Uiso 1 1 calc R U . . . H59B H 0.115969 0.590296 -0.183225 0.025 Uiso 1 1 calc R U . . . C60 C 0.2451(2) 0.65047(15) -0.15802(10) 0.0299(5) Uani 1 1 d . . . . . H60A H 0.215306 0.702920 -0.166684 0.045 Uiso 1 1 calc R U . . . H60B H 0.254866 0.639426 -0.119451 0.045 Uiso 1 1 calc R U . . . H60C H 0.307744 0.649653 -0.166411 0.045 Uiso 1 1 calc R U . . . C61 C 0.22153(16) 0.48000(14) -0.12361(9) 0.0217(5) Uani 1 1 d . . . . . H61A H 0.268245 0.515031 -0.098402 0.026 Uiso 1 1 calc R U . . . H61B H 0.156994 0.489386 -0.117875 0.026 Uiso 1 1 calc R U . . . C62 C 0.25006(19) 0.39440(16) -0.10960(11) 0.0306(5) Uani 1 1 d . . . . . H62A H 0.250689 0.384008 -0.071969 0.046 Uiso 1 1 calc R U . . . H62B H 0.203268 0.359052 -0.133636 0.046 Uiso 1 1 calc R U . . . H62C H 0.314694 0.384737 -0.114133 0.046 Uiso 1 1 calc R U . . . C63 C -0.0900(2) 0.55254(18) -0.11450(11) 0.0349(6) Uani 1 1 d . . . . . C64 C -0.1775(2) 0.5391(2) -0.09755(15) 0.0490(8) Uani 1 1 d . . . . . H64A H -0.180625 0.483188 -0.087547 0.074 Uiso 1 1 calc R U . . . H64B H -0.234253 0.552244 -0.127375 0.074 Uiso 1 1 calc R U . . . H64C H -0.176396 0.572847 -0.066297 0.074 Uiso 1 1 calc R U . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Cu1 0.01618(16) 0.01366(16) 0.01074(16) -0.00253(11) 0.00223(12) -0.00257(11) Cu2 0.01199(15) 0.01362(16) 0.01401(16) 0.00241(11) 0.00339(12) 0.00101(10) O1 0.0212(8) 0.0216(8) 0.0235(8) -0.0105(7) -0.0016(6) 0.0006(6) O2 0.0132(7) 0.0308(9) 0.0247(8) 0.0094(7) 0.0009(6) 0.0063(6) O3 0.0197(7) 0.0166(7) 0.0178(7) -0.0056(6) 0.0031(6) -0.0031(6) O4 0.0276(8) 0.0225(8) 0.0161(7) 0.0055(6) 0.0071(6) 0.0027(6) N1 0.0134(8) 0.0142(8) 0.0126(8) -0.0004(6) 0.0011(6) -0.0005(6) N2 0.0146(8) 0.0142(8) 0.0114(8) -0.0008(6) 0.0046(6) 0.0012(6) N3 0.0102(8) 0.0201(9) 0.0142(8) -0.0001(7) 0.0026(6) -0.0003(7) N4 0.0209(9) 0.0164(8) 0.0115(8) -0.0014(7) 0.0043(7) -0.0043(7) N5 0.0103(7) 0.0134(8) 0.0146(8) -0.0006(6) 0.0028(6) -0.0009(6) N6 0.0122(8) 0.0169(8) 0.0127(8) 0.0007(7) 0.0047(7) -0.0003(6) N7 0.0142(8) 0.0266(10) 0.0194(9) 0.0026(8) 0.0048(7) 0.0016(7) N8 0.0156(8) 0.0188(9) 0.0181(9) 0.0044(7) 0.0028(7) 0.0018(7) N9 0.0338(13) 0.0609(17) 0.0401(14) -0.0075(13) 0.0135(11) -0.0040(12) C1 0.0140(9) 0.0158(10) 0.0137(9) -0.0006(8) 0.0032(8) -0.0018(7) C2 0.0164(9) 0.0132(9) 0.0143(9) -0.0021(8) 0.0034(8) -0.0004(8) C3 0.0230(11) 0.0168(11) 0.0266(12) 0.0006(9) 0.0017(9) -0.0037(8) C4 0.0281(12) 0.0154(11) 0.0298(12) 0.0056(9) 0.0020(10) -0.0003(9) C5 0.0212(10) 0.0181(10) 0.0211(11) 0.0033(9) 0.0026(9) 0.0050(8) C6 0.0146(9) 0.0159(10) 0.0135(9) 0.0003(8) 0.0048(8) 0.0029(7) C7 0.0133(9) 0.0221(10) 0.0127(9) 0.0005(8) 0.0035(8) 0.0022(8) C8 0.0106(9) 0.0235(10) 0.0142(10) 0.0021(8) 0.0024(8) -0.0001(8) C9 0.0146(10) 0.0274(12) 0.0188(10) -0.0029(9) 0.0043(8) -0.0026(8) C10 0.0215(11) 0.0298(12) 0.0267(12) -0.0089(10) 0.0072(9) -0.0098(9) C11 0.0178(11) 0.0371(14) 0.0286(12) -0.0011(11) 0.0085(9) -0.0107(9) C12 0.0161(10) 0.0337(13) 0.0247(12) 0.0011(10) 0.0102(9) -0.0012(9) C13 0.0135(10) 0.0258(11) 0.0186(10) 0.0019(9) 0.0056(8) 0.0020(8) C14 0.0191(10) 0.0285(12) 0.0253(12) -0.0040(10) 0.0112(9) 0.0009(9) C15 0.0221(11) 0.0356(14) 0.0288(12) -0.0131(11) 0.0117(10) -0.0067(10) C16 0.0134(9) 0.0142(9) 0.0125(9) -0.0027(7) 0.0029(8) -0.0005(7) C17 0.0192(10) 0.0189(10) 0.0177(10) -0.0049(8) 0.0083(8) -0.0047(8) C18 0.0145(10) 0.0267(12) 0.0286(12) -0.0084(9) 0.0107(9) -0.0023(8) C19 0.0123(10) 0.0271(12) 0.0261(12) -0.0056(9) 0.0010(9) 0.0054(8) C20 0.0188(10) 0.0193(10) 0.0167(10) -0.0008(8) 0.0011(8) 0.0055(8) C21 0.0156(10) 0.0163(10) 0.0137(10) -0.0020(8) 0.0042(8) 0.0018(7) C22 0.0194(11) 0.0259(12) 0.0195(11) 0.0055(9) 0.0065(9) -0.0015(8) C23 0.0288(12) 0.0330(13) 0.0228(12) 0.0021(10) 0.0108(10) -0.0099(10) C24 0.0105(9) 0.0148(9) 0.0159(10) -0.0017(8) 0.0044(7) 0.0011(7) C25 0.0105(9) 0.0139(9) 0.0178(10) -0.0005(8) 0.0044(7) -0.0013(7) C26 0.0185(10) 0.0157(10) 0.0262(11) -0.0024(9) 0.0109(9) 0.0005(8) C27 0.0197(10) 0.0133(10) 0.0294(12) 0.0045(9) 0.0088(9) 0.0027(8) C28 0.0154(9) 0.0173(10) 0.0210(10) 0.0042(8) 0.0051(8) 0.0006(8) C29 0.0100(8) 0.0158(10) 0.0159(10) 0.0011(8) 0.0024(7) -0.0014(7) C30 0.0128(9) 0.0174(10) 0.0160(10) 0.0004(8) 0.0035(8) -0.0028(7) C31 0.0133(9) 0.0213(11) 0.0134(10) 0.0024(8) 0.0048(8) 0.0019(8) C32 0.0201(10) 0.0231(11) 0.0139(10) 0.0007(8) 0.0032(8) 0.0039(8) C33 0.0332(13) 0.0297(13) 0.0200(11) -0.0034(10) 0.0082(10) 0.0090(10) C34 0.0329(13) 0.0463(16) 0.0275(13) 0.0017(12) 0.0195(11) 0.0134(12) C35 0.0203(11) 0.0431(15) 0.0305(13) 0.0069(11) 0.0151(10) 0.0046(10) C36 0.0175(10) 0.0279(12) 0.0207(11) 0.0056(9) 0.0089(9) 0.0005(9) C37 0.0179(10) 0.0328(13) 0.0308(13) 0.0038(10) 0.0085(9) -0.0075(9) C38 0.0269(11) 0.0203(11) 0.0211(11) -0.0037(9) 0.0045(9) -0.0037(9) C39 0.0263(11) 0.0163(10) 0.0115(10) -0.0052(8) 0.0054(8) -0.0081(8) C40 0.0302(12) 0.0191(11) 0.0183(11) -0.0045(9) 0.0098(9) -0.0071(9) C41 0.0386(14) 0.0325(13) 0.0235(12) -0.0068(10) 0.0169(11) -0.0123(11) C42 0.0555(17) 0.0311(13) 0.0137(11) -0.0006(10) 0.0113(11) -0.0187(12) C43 0.0432(14) 0.0215(11) 0.0139(10) 0.0003(9) -0.0021(10) -0.0107(10) C44 0.0306(12) 0.0182(10) 0.0127(10) -0.0043(8) -0.0001(9) -0.0082(9) C45 0.0342(13) 0.0317(13) 0.0234(12) -0.0032(10) 0.0004(10) 0.0009(10) C46 0.0295(12) 0.0283(12) 0.0302(13) -0.0012(10) 0.0138(10) 0.0011(10) C47 0.0228(11) 0.0369(14) 0.0217(12) -0.0036(10) 0.0060(9) 0.0040(10) C48 0.0329(14) 0.0478(16) 0.0273(13) 0.0068(12) 0.0127(11) 0.0100(12) C49 0.0270(12) 0.0267(12) 0.0273(13) 0.0015(10) 0.0063(10) 0.0046(10) C50 0.0515(18) 0.0355(15) 0.0336(15) -0.0043(12) 0.0140(13) 0.0090(12) C51 0.0259(12) 0.0257(12) 0.0286(12) -0.0012(10) 0.0087(10) -0.0017(9) C52 0.0302(13) 0.0426(16) 0.0356(15) 0.0028(12) 0.0083(11) -0.0092(12) C53 0.0176(11) 0.0347(13) 0.0243(12) -0.0070(10) 0.0045(9) -0.0050(9) C54 0.0187(11) 0.0472(16) 0.0319(13) 0.0051(12) 0.0050(10) 0.0064(11) C55 0.0214(12) 0.0417(15) 0.0362(14) 0.0175(12) 0.0139(11) 0.0095(10) C56 0.0345(14) 0.0583(19) 0.0451(17) 0.0265(15) 0.0254(13) 0.0135(13) C57 0.0321(12) 0.0164(10) 0.0189(11) 0.0011(8) 0.0038(9) -0.0001(9) C58 0.0253(12) 0.0279(13) 0.0349(14) -0.0037(11) -0.0020(10) -0.0053(10) C59 0.0212(10) 0.0167(10) 0.0220(11) 0.0017(9) 0.0024(9) 0.0002(8) C60 0.0398(14) 0.0220(12) 0.0229(12) 0.0010(10) 0.0004(10) -0.0081(10) C61 0.0212(10) 0.0258(12) 0.0175(11) 0.0059(9) 0.0046(8) -0.0001(9) C62 0.0338(13) 0.0316(13) 0.0265(13) 0.0139(11) 0.0084(11) 0.0060(10) C63 0.0298(14) 0.0452(16) 0.0286(13) -0.0077(12) 0.0061(11) 0.0006(11) C64 0.0328(15) 0.070(2) 0.0486(18) -0.0073(17) 0.0178(14) -0.0056(15) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 '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 N4 Cu1 N1 173.38(8) . . ? N4 Cu1 Cu2 93.51(6) . . ? N1 Cu1 Cu2 92.52(5) . . ? N6 Cu2 N3 108.47(7) . . ? N6 Cu2 N2 124.25(7) . . ? N3 Cu2 N2 82.39(7) . . ? N6 Cu2 N5 82.43(7) . . ? N3 Cu2 N5 120.66(7) . . ? N2 Cu2 N5 139.42(7) . . ? N6 Cu2 Cu1 124.69(5) . . ? N3 Cu2 Cu1 126.78(5) . . ? N2 Cu2 Cu1 70.81(5) . . ? N5 Cu2 Cu1 68.70(5) . . ? C1 N1 C16 115.74(17) . . ? C1 N1 Cu1 121.56(14) . . ? C16 N1 Cu1 122.01(13) . . ? C2 N2 C6 117.07(18) . . ? C2 N2 Cu2 133.14(14) . . ? C6 N2 Cu2 109.79(13) . . ? C7 N3 C8 118.96(18) . . ? C7 N3 Cu2 114.22(14) . . ? C8 N3 Cu2 125.24(14) . . ? C24 N4 C39 116.66(17) . . ? C24 N4 Cu1 123.76(15) . . ? C39 N4 Cu1 119.33(14) . . ? C29 N5 C25 117.29(17) . . ? C29 N5 Cu2 109.00(13) . . ? C25 N5 Cu2 132.76(14) . . ? C30 N6 C31 117.20(17) . . ? C30 N6 Cu2 114.07(14) . . ? C31 N6 Cu2 128.14(14) . . ? C49 N7 C53 111.05(19) . . ? C49 N7 C51 111.29(18) . . ? C53 N7 C51 107.49(18) . . ? C49 N7 C47 107.49(18) . . ? C53 N7 C47 111.87(17) . . ? C51 N7 C47 107.64(19) . . ? C55 N8 C57 108.80(19) . . ? C55 N8 C59 111.74(18) . . ? C57 N8 C59 107.93(16) . . ? C55 N8 C61 108.39(17) . . ? C57 N8 C61 111.51(17) . . ? C59 N8 C61 108.50(17) . . ? O1 C1 N1 126.1(2) . . ? O1 C1 C2 117.28(18) . . ? N1 C1 C2 116.40(18) . . ? N2 C2 C3 122.9(2) . . ? N2 C2 C1 122.37(18) . . ? C3 C2 C1 114.71(19) . . ? C4 C3 C2 119.4(2) . . ? C4 C3 H3A 120.3 . . ? C2 C3 H3A 120.3 . . ? C3 C4 C5 118.4(2) . . ? C3 C4 H4A 120.8 . . ? C5 C4 H4A 120.8 . . ? C4 C5 C6 119.4(2) . . ? C4 C5 H5A 120.3 . . ? C6 C5 H5A 120.3 . . ? N2 C6 C5 122.66(19) . . ? N2 C6 C7 118.73(18) . . ? C5 C6 C7 118.60(19) . . ? O2 C7 N3 128.6(2) . . ? O2 C7 C6 116.77(19) . . ? N3 C7 C6 114.58(18) . . ? C9 C8 C13 119.6(2) . . ? C9 C8 N3 119.88(19) . . ? C13 C8 N3 120.3(2) . . ? C10 C9 C8 119.5(2) . . ? C10 C9 C15 119.8(2) . . ? C8 C9 C15 120.8(2) . . ? C11 C10 C9 121.2(2) . . ? C11 C10 H10A 119.4 . . ? C9 C10 H10A 119.4 . . ? C12 C11 C10 119.1(2) . . ? C12 C11 H11A 120.4 . . ? C10 C11 H11A 120.4 . . ? C11 C12 C13 121.6(2) . . ? C11 C12 H12A 119.2 . . ? C13 C12 H12A 119.2 . . ? C12 C13 C8 119.0(2) . . ? C12 C13 C14 120.2(2) . . ? C8 C13 C14 120.9(2) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C9 C15 H15A 109.5 . . ? C9 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C9 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C21 C16 C17 120.55(19) . . ? C21 C16 N1 120.52(18) . . ? C17 C16 N1 118.92(19) . . ? C18 C17 C16 118.9(2) . . ? C18 C17 C23 120.8(2) . . ? C16 C17 C23 120.2(2) . . ? C19 C18 C17 120.9(2) . . ? C19 C18 H18A 119.6 . . ? C17 C18 H18A 119.6 . . ? C18 C19 C20 119.7(2) . . ? C18 C19 H19A 120.1 . . ? C20 C19 H19A 120.1 . . ? C19 C20 C21 121.0(2) . . ? C19 C20 H20A 119.5 . . ? C21 C20 H20A 119.5 . . ? C16 C21 C20 118.86(19) . . ? C16 C21 C22 120.68(19) . . ? C20 C21 C22 120.5(2) . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C17 C23 H23A 109.5 . . ? C17 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C17 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? O3 C24 N4 126.59(19) . . ? O3 C24 C25 116.81(18) . . ? N4 C24 C25 116.39(18) . . ? N5 C25 C26 122.21(19) . . ? N5 C25 C24 122.56(18) . . ? C26 C25 C24 115.23(18) . . ? C27 C26 C25 119.9(2) . . ? C27 C26 H26A 120.0 . . ? C25 C26 H26A 120.0 . . ? C28 C27 C26 118.3(2) . . ? C28 C27 H27A 120.8 . . ? C26 C27 H27A 120.8 . . ? C27 C28 C29 119.3(2) . . ? C27 C28 H28A 120.4 . . ? C29 C28 H28A 120.4 . . ? N5 C29 C28 122.88(19) . . ? N5 C29 C30 119.54(18) . . ? C28 C29 C30 117.45(19) . . ? O4 C30 N6 128.6(2) . . ? O4 C30 C29 117.13(19) . . ? N6 C30 C29 114.22(18) . . ? C32 C31 N6 120.84(19) . . ? C32 C31 C36 119.7(2) . . ? N6 C31 C36 119.2(2) . . ? C33 C32 C31 119.2(2) . . ? C33 C32 C38 120.0(2) . . ? C31 C32 C38 120.78(19) . . ? C34 C33 C32 121.2(2) . . ? C34 C33 H33A 119.4 . . ? C32 C33 H33A 119.4 . . ? C35 C34 C33 119.2(2) . . ? C35 C34 H34A 120.4 . . ? C33 C34 H34A 120.4 . . ? C34 C35 C36 121.6(2) . . ? C34 C35 H35A 119.2 . . ? C36 C35 H35A 119.2 . . ? C35 C36 C31 118.9(2) . . ? C35 C36 C37 120.1(2) . . ? C31 C36 C37 120.9(2) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C32 C38 H38A 109.5 . . ? C32 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C32 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C40 C39 C44 120.3(2) . . ? C40 C39 N4 118.8(2) . . ? C44 C39 N4 120.8(2) . . ? C41 C40 C39 119.2(2) . . ? C41 C40 C46 120.4(2) . . ? C39 C40 C46 120.3(2) . . ? C42 C41 C40 120.6(2) . . ? C42 C41 H41A 119.7 . . ? C40 C41 H41A 119.7 . . ? C43 C42 C41 119.9(2) . . ? C43 C42 H42A 120.0 . . ? C41 C42 H42A 120.0 . . ? C42 C43 C44 121.4(2) . . ? C42 C43 H43A 119.3 . . ? C44 C43 H43A 119.3 . . ? C43 C44 C39 118.5(2) . . ? C43 C44 C45 119.9(2) . . ? C39 C44 C45 121.5(2) . . ? C44 C45 H45A 109.5 . . ? C44 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? C44 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? C40 C46 H46A 109.5 . . ? C40 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? C40 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C48 C47 N7 114.0(2) . . ? C48 C47 H47A 108.7 . . ? N7 C47 H47A 108.7 . . ? C48 C47 H47B 108.7 . . ? N7 C47 H47B 108.7 . . ? H47A C47 H47B 107.6 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? N7 C49 C50 113.9(2) . . ? N7 C49 H49A 108.8 . . ? C50 C49 H49A 108.8 . . ? N7 C49 H49B 108.8 . . ? C50 C49 H49B 108.8 . . ? H49A C49 H49B 107.7 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C52 C51 N7 116.2(2) . . ? C52 C51 H51A 108.2 . . ? N7 C51 H51A 108.2 . . ? C52 C51 H51B 108.2 . . ? N7 C51 H51B 108.2 . . ? H51A C51 H51B 107.4 . . ? C51 C52 H52A 109.5 . . ? C51 C52 H52B 109.5 . . ? H52A C52 H52B 109.5 . . ? C51 C52 H52C 109.5 . . ? H52A C52 H52C 109.5 . . ? H52B C52 H52C 109.5 . . ? C54 C53 N7 115.2(2) . . ? C54 C53 H53A 108.5 . . ? N7 C53 H53A 108.5 . . ? C54 C53 H53B 108.5 . . ? N7 C53 H53B 108.5 . . ? H53A C53 H53B 107.5 . . ? C53 C54 H54A 109.5 . . ? C53 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C53 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? N8 C55 C56 114.4(2) . . ? N8 C55 H55A 108.7 . . ? C56 C55 H55A 108.7 . . ? N8 C55 H55B 108.7 . . ? C56 C55 H55B 108.7 . . ? H55A C55 H55B 107.6 . . ? C55 C56 H56A 109.5 . . ? C55 C56 H56B 109.5 . . ? H56A C56 H56B 109.5 . . ? C55 C56 H56C 109.5 . . ? H56A C56 H56C 109.5 . . ? H56B C56 H56C 109.5 . . ? C58 C57 N8 115.0(2) . . ? C58 C57 H57A 108.5 . . ? N8 C57 H57A 108.5 . . ? C58 C57 H57B 108.5 . . ? N8 C57 H57B 108.5 . . ? H57A C57 H57B 107.5 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C60 C59 N8 114.53(19) . . ? C60 C59 H59A 108.6 . . ? N8 C59 H59A 108.6 . . ? C60 C59 H59B 108.6 . . ? N8 C59 H59B 108.6 . . ? H59A C59 H59B 107.6 . . ? C59 C60 H60A 109.5 . . ? C59 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C59 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C62 C61 N8 114.3(2) . . ? C62 C61 H61A 108.7 . . ? N8 C61 H61A 108.7 . . ? C62 C61 H61B 108.7 . . ? N8 C61 H61B 108.7 . . ? H61A C61 H61B 107.6 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? N9 C63 C64 179.3(4) . . ? C63 C64 H64A 109.5 . . ? C63 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? C63 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? 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 N4 1.8536(18) . ? Cu1 N1 1.8545(17) . ? Cu1 Cu2 2.8047(4) . ? Cu2 N6 2.0568(17) . ? Cu2 N3 2.0593(17) . ? Cu2 N2 2.0709(17) . ? Cu2 N5 2.0928(17) . ? O1 C1 1.246(3) . ? O2 C7 1.259(3) . ? O3 C24 1.246(3) . ? O4 C30 1.252(3) . ? N1 C1 1.328(3) . ? N1 C16 1.431(3) . ? N2 C2 1.350(3) . ? N2 C6 1.358(3) . ? N3 C7 1.314(3) . ? N3 C8 1.418(3) . ? N4 C24 1.331(3) . ? N4 C39 1.437(3) . ? N5 C29 1.356(3) . ? N5 C25 1.357(3) . ? N6 C30 1.323(3) . ? N6 C31 1.415(3) . ? N7 C49 1.509(3) . ? N7 C53 1.512(3) . ? N7 C51 1.523(3) . ? N7 C47 1.540(3) . ? N8 C55 1.504(3) . ? N8 C57 1.518(3) . ? N8 C59 1.520(3) . ? N8 C61 1.524(3) . ? N9 C63 1.139(4) . ? C1 C2 1.520(3) . ? C2 C3 1.392(3) . ? C3 C4 1.379(3) . ? C3 H3A 0.9500 . ? C4 C5 1.386(3) . ? C4 H4A 0.9500 . ? C5 C6 1.388(3) . ? C5 H5A 0.9500 . ? C6 C7 1.518(3) . ? C8 C9 1.404(3) . ? C8 C13 1.417(3) . ? C9 C10 1.396(3) . ? C9 C15 1.505(3) . ? C10 C11 1.390(3) . ? C10 H10A 0.9500 . ? C11 C12 1.383(4) . ? C11 H11A 0.9500 . ? C12 C13 1.395(3) . ? C12 H12A 0.9500 . ? C13 C14 1.501(3) . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C21 1.397(3) . ? C16 C17 1.405(3) . ? C17 C18 1.395(3) . ? C17 C23 1.501(3) . ? C18 C19 1.384(4) . ? C18 H18A 0.9500 . ? C19 C20 1.385(3) . ? C19 H19A 0.9500 . ? C20 C21 1.398(3) . ? C20 H20A 0.9500 . ? C21 C22 1.502(3) . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 C25 1.527(3) . ? C25 C26 1.391(3) . ? C26 C27 1.385(3) . ? C26 H26A 0.9500 . ? C27 C28 1.382(3) . ? C27 H27A 0.9500 . ? C28 C29 1.393(3) . ? C28 H28A 0.9500 . ? C29 C30 1.517(3) . ? C31 C32 1.405(3) . ? C31 C36 1.418(3) . ? C32 C33 1.399(3) . ? C32 C38 1.503(3) . ? C33 C34 1.386(4) . ? C33 H33A 0.9500 . ? C34 C35 1.384(4) . ? C34 H34A 0.9500 . ? C35 C36 1.391(3) . ? C35 H35A 0.9500 . ? C36 C37 1.498(4) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 C40 1.401(3) . ? C39 C44 1.402(3) . ? C40 C41 1.398(3) . ? C40 C46 1.503(4) . ? C41 C42 1.381(4) . ? C41 H41A 0.9500 . ? C42 C43 1.373(4) . ? C42 H42A 0.9500 . ? C43 C44 1.401(3) . ? C43 H43A 0.9500 . ? C44 C45 1.503(4) . ? C45 H45A 0.9800 . ? C45 H45B 0.9800 . ? C45 H45C 0.9800 . ? C46 H46A 0.9800 . ? C46 H46B 0.9800 . ? C46 H46C 0.9800 . ? C47 C48 1.514(4) . ? C47 H47A 0.9900 . ? C47 H47B 0.9900 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C49 C50 1.510(4) . ? C49 H49A 0.9900 . ? C49 H49B 0.9900 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C52 1.508(4) . ? C51 H51A 0.9900 . ? C51 H51B 0.9900 . ? C52 H52A 0.9800 . ? C52 H52B 0.9800 . ? C52 H52C 0.9800 . ? C53 C54 1.506(4) . ? C53 H53A 0.9900 . ? C53 H53B 0.9900 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.520(4) . ? C55 H55A 0.9900 . ? C55 H55B 0.9900 . ? C56 H56A 0.9800 . ? C56 H56B 0.9800 . ? C56 H56C 0.9800 . ? C57 C58 1.512(4) . ? C57 H57A 0.9900 . ? C57 H57B 0.9900 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 C60 1.514(3) . ? C59 H59A 0.9900 . ? C59 H59B 0.9900 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C62 1.514(3) . ? C61 H61A 0.9900 . ? C61 H61B 0.9900 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C64 1.455(4) . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? 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 Cu2 Cu1 N1 C1 -57.58(16) . . . . ? Cu2 Cu1 N1 C16 132.36(15) . . . . ? Cu2 Cu1 N4 C24 -54.87(17) . . . . ? Cu2 Cu1 N4 C39 131.04(16) . . . . ? C16 N1 C1 O1 -4.1(3) . . . . ? Cu1 N1 C1 O1 -174.75(17) . . . . ? C16 N1 C1 C2 170.53(17) . . . . ? Cu1 N1 C1 C2 -0.1(2) . . . . ? C6 N2 C2 C3 -2.5(3) . . . . ? Cu2 N2 C2 C3 176.99(17) . . . . ? C6 N2 C2 C1 177.28(18) . . . . ? Cu2 N2 C2 C1 -3.3(3) . . . . ? O1 C1 C2 N2 -134.4(2) . . . . ? N1 C1 C2 N2 50.5(3) . . . . ? O1 C1 C2 C3 45.4(3) . . . . ? N1 C1 C2 C3 -129.7(2) . . . . ? N2 C2 C3 C4 -0.8(4) . . . . ? C1 C2 C3 C4 179.4(2) . . . . ? C2 C3 C4 C5 2.7(4) . . . . ? C3 C4 C5 C6 -1.2(4) . . . . ? C2 N2 C6 C5 4.0(3) . . . . ? Cu2 N2 C6 C5 -175.59(17) . . . . ? C2 N2 C6 C7 -174.57(17) . . . . ? Cu2 N2 C6 C7 5.9(2) . . . . ? C4 C5 C6 N2 -2.2(3) . . . . ? C4 C5 C6 C7 176.4(2) . . . . ? C8 N3 C7 O2 -10.0(3) . . . . ? Cu2 N3 C7 O2 -176.46(18) . . . . ? C8 N3 C7 C6 168.89(18) . . . . ? Cu2 N3 C7 C6 2.5(2) . . . . ? N2 C6 C7 O2 173.22(18) . . . . ? C5 C6 C7 O2 -5.4(3) . . . . ? N2 C6 C7 N3 -5.9(3) . . . . ? C5 C6 C7 N3 175.53(19) . . . . ? C7 N3 C8 C9 121.1(2) . . . . ? Cu2 N3 C8 C9 -74.1(2) . . . . ? C7 N3 C8 C13 -64.3(3) . . . . ? Cu2 N3 C8 C13 100.5(2) . . . . ? C13 C8 C9 C10 -1.0(3) . . . . ? N3 C8 C9 C10 173.6(2) . . . . ? C13 C8 C9 C15 178.0(2) . . . . ? N3 C8 C9 C15 -7.4(3) . . . . ? C8 C9 C10 C11 0.3(4) . . . . ? C15 C9 C10 C11 -178.8(2) . . . . ? C9 C10 C11 C12 0.5(4) . . . . ? C10 C11 C12 C13 -0.4(4) . . . . ? C11 C12 C13 C8 -0.4(4) . . . . ? C11 C12 C13 C14 -179.8(2) . . . . ? C9 C8 C13 C12 1.1(3) . . . . ? N3 C8 C13 C12 -173.5(2) . . . . ? C9 C8 C13 C14 -179.5(2) . . . . ? N3 C8 C13 C14 5.9(3) . . . . ? C1 N1 C16 C21 95.3(2) . . . . ? Cu1 N1 C16 C21 -94.1(2) . . . . ? C1 N1 C16 C17 -85.8(2) . . . . ? Cu1 N1 C16 C17 84.9(2) . . . . ? C21 C16 C17 C18 -1.8(3) . . . . ? N1 C16 C17 C18 179.29(19) . . . . ? C21 C16 C17 C23 178.5(2) . . . . ? N1 C16 C17 C23 -0.4(3) . . . . ? C16 C17 C18 C19 -0.6(3) . . . . ? C23 C17 C18 C19 179.0(2) . . . . ? C17 C18 C19 C20 2.0(3) . . . . ? C18 C19 C20 C21 -0.9(3) . . . . ? C17 C16 C21 C20 2.8(3) . . . . ? N1 C16 C21 C20 -178.25(18) . . . . ? C17 C16 C21 C22 -177.4(2) . . . . ? N1 C16 C21 C22 1.5(3) . . . . ? C19 C20 C21 C16 -1.5(3) . . . . ? C19 C20 C21 C22 178.7(2) . . . . ? C39 N4 C24 O3 -1.7(3) . . . . ? Cu1 N4 C24 O3 -175.89(16) . . . . ? C39 N4 C24 C25 172.94(18) . . . . ? Cu1 N4 C24 C25 -1.3(3) . . . . ? C29 N5 C25 C26 0.9(3) . . . . ? Cu2 N5 C25 C26 -166.59(15) . . . . ? C29 N5 C25 C24 -178.46(17) . . . . ? Cu2 N5 C25 C24 14.1(3) . . . . ? O3 C24 C25 N5 -143.80(19) . . . . ? N4 C24 C25 N5 41.1(3) . . . . ? O3 C24 C25 C26 36.8(3) . . . . ? N4 C24 C25 C26 -138.3(2) . . . . ? N5 C25 C26 C27 -2.7(3) . . . . ? C24 C25 C26 C27 176.64(19) . . . . ? C25 C26 C27 C28 1.9(3) . . . . ? C26 C27 C28 C29 0.6(3) . . . . ? C25 N5 C29 C28 1.8(3) . . . . ? Cu2 N5 C29 C28 172.05(16) . . . . ? C25 N5 C29 C30 -173.91(17) . . . . ? Cu2 N5 C29 C30 -3.6(2) . . . . ? C27 C28 C29 N5 -2.5(3) . . . . ? C27 C28 C29 C30 173.26(19) . . . . ? C31 N6 C30 O4 -13.9(3) . . . . ? Cu2 N6 C30 O4 174.14(18) . . . . ? C31 N6 C30 C29 162.60(17) . . . . ? Cu2 N6 C30 C29 -9.4(2) . . . . ? N5 C29 C30 O4 -174.08(18) . . . . ? C28 C29 C30 O4 10.0(3) . . . . ? N5 C29 C30 N6 9.0(3) . . . . ? C28 C29 C30 N6 -166.93(18) . . . . ? C30 N6 C31 C32 124.1(2) . . . . ? Cu2 N6 C31 C32 -65.2(3) . . . . ? C30 N6 C31 C36 -61.3(3) . . . . ? Cu2 N6 C31 C36 109.3(2) . . . . ? N6 C31 C32 C33 175.3(2) . . . . ? C36 C31 C32 C33 0.8(3) . . . . ? N6 C31 C32 C38 -5.4(3) . . . . ? C36 C31 C32 C38 -179.9(2) . . . . ? C31 C32 C33 C34 0.2(4) . . . . ? C38 C32 C33 C34 -179.0(2) . . . . ? C32 C33 C34 C35 -1.0(4) . . . . ? C33 C34 C35 C36 0.6(4) . . . . ? C34 C35 C36 C31 0.5(4) . . . . ? C34 C35 C36 C37 -177.4(2) . . . . ? C32 C31 C36 C35 -1.2(3) . . . . ? N6 C31 C36 C35 -175.8(2) . . . . ? C32 C31 C36 C37 176.7(2) . . . . ? N6 C31 C36 C37 2.0(3) . . . . ? C24 N4 C39 C40 -92.7(2) . . . . ? Cu1 N4 C39 C40 81.8(2) . . . . ? C24 N4 C39 C44 91.2(2) . . . . ? Cu1 N4 C39 C44 -94.3(2) . . . . ? C44 C39 C40 C41 -3.1(3) . . . . ? N4 C39 C40 C41 -179.3(2) . . . . ? C44 C39 C40 C46 174.4(2) . . . . ? N4 C39 C40 C46 -1.8(3) . . . . ? C39 C40 C41 C42 2.0(4) . . . . ? C46 C40 C41 C42 -175.5(2) . . . . ? C40 C41 C42 C43 0.0(4) . . . . ? C41 C42 C43 C44 -0.9(4) . . . . ? C42 C43 C44 C39 -0.3(3) . . . . ? C42 C43 C44 C45 177.7(2) . . . . ? C40 C39 C44 C43 2.3(3) . . . . ? N4 C39 C44 C43 178.38(19) . . . . ? C40 C39 C44 C45 -175.7(2) . . . . ? N4 C39 C44 C45 0.4(3) . . . . ? C49 N7 C47 C48 -64.8(2) . . . . ? C53 N7 C47 C48 57.3(3) . . . . ? C51 N7 C47 C48 175.2(2) . . . . ? C53 N7 C49 C50 63.5(3) . . . . ? C51 N7 C49 C50 -56.2(3) . . . . ? C47 N7 C49 C50 -173.9(2) . . . . ? C49 N7 C51 C52 -49.3(3) . . . . ? C53 N7 C51 C52 -171.1(2) . . . . ? C47 N7 C51 C52 68.3(3) . . . . ? C49 N7 C53 C54 171.2(2) . . . . ? C51 N7 C53 C54 -66.8(3) . . . . ? C47 N7 C53 C54 51.1(3) . . . . ? C57 N8 C55 C56 59.4(3) . . . . ? C59 N8 C55 C56 -59.6(3) . . . . ? C61 N8 C55 C56 -179.2(2) . . . . ? C55 N8 C57 C58 167.2(2) . . . . ? C59 N8 C57 C58 -71.4(2) . . . . ? C61 N8 C57 C58 47.7(3) . . . . ? C55 N8 C59 C60 -53.5(3) . . . . ? C57 N8 C59 C60 -173.09(19) . . . . ? C61 N8 C59 C60 65.9(2) . . . . ? C55 N8 C61 C62 -63.7(3) . . . . ? C57 N8 C61 C62 56.0(2) . . . . ? C59 N8 C61 C62 174.74(19) . . . . ?