#------------------------------------------------------------------------------ #$Date: 2022-08-07 01:27:25 +0300 (Sun, 07 Aug 2022) $ #$Revision: 277149 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/52/7245276.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_7245276 loop_ _publ_author_name 'Kim, Gyeongwoo' 'Kim, Gyeongmin' 'Kim, Dongwon' 'Jung, Ok-Sang' _publ_section_title ; Subtle metal(II) effects of 2D coordination networks on SCSC guest exchange ; _journal_name_full CrystEngComm _journal_paper_doi 10.1039/D2CE00837H _journal_year 2022 _chemical_formula_sum 'C52 H53 Cu N5 O20' _chemical_formula_weight 1131.53 _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 _atom_sites_solution_primary dual _audit_creation_method SHELXL-2019/2 _audit_update_record ; 2022-06-15 deposited with the CCDC. 2022-08-05 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 114.74(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 20.698(4) _cell_length_b 12.339(3) _cell_length_c 22.916(5) _cell_measurement_reflns_used 79760 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 33.417 _cell_measurement_theta_min 0.435 _cell_volume 5315(2) _computing_cell_refinement 'HKL3000sm (Otwinowski & Minor, 1997)' _computing_data_collection 'PAL BL2D-SMDC Program (Shin et. al, 2016)' _computing_data_reduction 'HKL3000sm (Otwinowski & Minor, 1997)' _computing_structure_refinement 'SHELXL-2019/2 (Sheldrick, 2019)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 0.981 _diffrn_measured_fraction_theta_max 0.795 _diffrn_measurement_device_type 'Rayonix MX225HS CCD area detector' _diffrn_measurement_method 'omega scan' _diffrn_radiation_type synchrotron _diffrn_radiation_wavelength 0.760 _diffrn_reflns_av_R_equivalents 0.0761 _diffrn_reflns_av_unetI/netI 0.0901 _diffrn_reflns_Laue_measured_fraction_full 0.981 _diffrn_reflns_Laue_measured_fraction_max 0.795 _diffrn_reflns_limit_h_max 28 _diffrn_reflns_limit_h_min -28 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_l_max 30 _diffrn_reflns_limit_l_min -30 _diffrn_reflns_number 45296 _diffrn_reflns_point_group_measured_fraction_full 0.981 _diffrn_reflns_point_group_measured_fraction_max 0.795 _diffrn_reflns_theta_full 27.129 _diffrn_reflns_theta_max 33.311 _diffrn_reflns_theta_min 1.192 _diffrn_source 'PLSII 2D bending magnet' _exptl_absorpt_coefficient_mu 0.588 _exptl_absorpt_correction_T_max 1.000 _exptl_absorpt_correction_T_min 0.958 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'HKL3000sm Scalepack(Otwinowski et.al,2003)' _exptl_crystal_colour blue _exptl_crystal_density_diffrn 1.414 _exptl_crystal_description block _exptl_crystal_F_000 2356 _exptl_crystal_size_max 0.04 _exptl_crystal_size_mid 0.03 _exptl_crystal_size_min 0.02 _refine_diff_density_max 0.760 _refine_diff_density_min -0.540 _refine_diff_density_rms 0.092 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.921 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 851 _refine_ls_number_reflns 13355 _refine_ls_number_restraints 924 _refine_ls_restrained_S_all 0.938 _refine_ls_R_factor_all 0.1466 _refine_ls_R_factor_gt 0.0789 _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^)+(0.1729P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2355 _refine_ls_wR_factor_ref 0.2694 _reflns_Friedel_coverage 0.000 _reflns_number_gt 6332 _reflns_number_total 13355 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d2ce00837h2.cif _cod_data_source_block CuNO3_dioxane_exchange _cod_original_cell_volume 5316(2) _cod_original_sg_symbol_H-M 'P 21/n' _cod_database_code 7245276 _shelx_shelxl_version_number 2019/2 _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_res_file ; TITL KGW2_a.res in P2(1)/n CuNO3_dioxane_exchange.res created by SHELXL-2019/2 at 21:50:37 on 15-Jun-2022 REM Old TITL KGW2 in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.213, Rweak 0.016, Alpha 0.049 REM 0.236 for 449 systematic absences, Orientation as input REM Formula found by SHELXT: C48 N7 O11 Cu CELL 0.76000 20.6980 12.3390 22.9160 90.000 114.736 90.000 ZERR 4.000 0.0041 0.0025 0.0046 0.000 0.030 0.000 LATT 1 SYMM 1/2-X, 1/2+Y, 1/2-Z SFAC C H N O CU DISP $C 0.00411 0.00197 13.03582!source kissel DISP $H -0.00002 0.00000 0.66628!source kissel DISP $N 0.00785 0.00398 22.79284!source kissel DISP $O 0.01334 0.00722 38.15216!source kissel DISP $Cu 0.29772 1.43149 6226.63986!source kissel UNIT 208 212 20 80 4 ACTA L.S. 24 BOND $H LIST 4 FMAP 2 PLAN 50 EQIV $1 1-x, 1-y, -z EQIV $2 1-x, -y, 1-z DFIX 1.2 0.01 N4' O7' DFIX 1.43 0.01 O1C C1C O1C C4C O2C C2C O2C C3C O3C C5C O3C C8C O4C C6C O4C C7C DFIX 1.43 0.01 O1D C2D_$2 O1E C1E O1E C2E_$1 O2E C3E_$1 DFIX 1.51 0.01 C1B C2B C1C C2C C3C C4C C7C C8C C1E C2E DANG 2.83 0.01 O1C O2C O3C O4C O1D O1D_$2 O1E O1E_$1 DANG 2.80 0.01 C1C C3C C2C C4C C1E C1E_$1 C2E C2E_$1 C4E C4E_$1 DANG 2.35 0.01 C1C C4C C5C C8C C6C C7C SIMU 0.01 ISOR 0.01 O1A C4A C3B C6C ISOR 0.05 O1C O2C C1C C2C C3C C4C O3C O4C C5C C7C C8C O1E O2E FREE C6C C7C WGHT 0.172900 FVAR 0.31308 0.40911 0.52589 0.23801 0.64621 CU01 5 0.277243 0.421479 0.534281 11.00000 0.03966 0.04346 = 0.05679 -0.00765 0.02240 -0.00586 O1 4 0.489777 0.285676 0.369630 11.00000 0.05965 0.05701 = 0.03935 -0.00853 0.01916 0.00945 O1A 4 0.578811 0.289863 0.823837 11.00000 0.17296 0.17066 = 0.17460 -0.00261 -0.01415 -0.04241 O1B 4 0.318538 0.195251 0.284490 11.00000 0.11580 0.12200 = 0.09148 -0.02610 0.01938 -0.02832 PART 1 21 O1C 4 0.750428 -0.081878 0.204632 21.00000 0.19989 0.25864 = 0.18730 0.06521 0.07763 0.06961 O2C 4 0.712282 -0.212753 0.284788 21.00000 0.18839 0.25549 = 0.17139 0.06266 0.10913 0.07225 C1C 1 0.808866 -0.102707 0.266537 21.00000 0.20118 0.25075 = 0.18078 0.05926 0.08984 0.07383 AFIX 23 H1CA 2 0.829046 -0.034338 0.286911 21.00000 -1.20000 H1CB 2 0.845744 -0.142892 0.260267 21.00000 -1.20000 AFIX 0 C2C 1 0.784103 -0.167491 0.310604 21.00000 0.19948 0.24083 = 0.16981 0.06771 0.09530 0.07555 AFIX 23 H2CA 2 0.817126 -0.227121 0.328276 21.00000 -1.20000 H2CB 2 0.789045 -0.120798 0.346283 21.00000 -1.20000 AFIX 0 C3C 1 0.700015 -0.257440 0.223353 21.00000 0.20521 0.26433 = 0.19354 0.06407 0.08098 0.05889 AFIX 23 H3CA 2 0.649910 -0.275411 0.201486 21.00000 -1.20000 H3CB 2 0.726373 -0.324826 0.230544 21.00000 -1.20000 AFIX 0 C4C 1 0.719636 -0.187556 0.177800 21.00000 0.20673 0.26405 = 0.19403 0.06646 0.07158 0.06824 AFIX 23 H4CA 2 0.753445 -0.227049 0.166696 21.00000 -1.20000 H4CB 2 0.677236 -0.175807 0.138497 21.00000 -1.20000 AFIX 0 PART 2 -21 O3C 4 0.777217 -0.063075 0.299825 -21.00000 0.21809 0.25691 = 0.19162 0.04537 0.08655 0.08153 O4C 4 0.744093 -0.217977 0.199723 -21.00000 0.19908 0.26445 = 0.19546 0.05696 0.08201 0.07272 C5C 1 0.820013 -0.158534 0.317679 -21.00000 0.18801 0.22817 = 0.16287 0.07498 0.10056 0.08547 AFIX 23 H5CA 2 0.807209 -0.201525 0.346686 -21.00000 -1.20000 H5CB 2 0.869680 -0.138348 0.340130 -21.00000 -1.20000 AFIX 0 C6C 1 0.809164 -0.230273 0.254900 -21.00000 0.19215 0.23174 = 0.17649 0.06272 0.09083 0.07141 AFIX 23 H6C1 2 0.847623 -0.213031 0.242787 -21.00000 -1.20000 H6C2 2 0.814107 -0.306057 0.267264 -21.00000 -1.20000 AFIX 0 C7C 1 0.719351 -0.106297 0.199880 -21.00000 0.19976 0.25860 = 0.18708 0.06160 0.07544 0.07703 AFIX 23 H7C1 2 0.676065 -0.094028 0.161448 -21.00000 -1.20000 H7C2 2 0.755109 -0.055795 0.199546 -21.00000 -1.20000 AFIX 0 C8C 1 0.705530 -0.086693 0.257625 -21.00000 0.18839 0.25434 = 0.17543 0.05493 0.08994 0.08722 AFIX 23 H8C1 2 0.673948 -0.025729 0.252241 -21.00000 -1.20000 H8C2 2 0.687505 -0.150500 0.270629 -21.00000 -1.20000 AFIX 0 PART 0 PART 3 31 O1D 4 0.427213 0.020988 0.483303 31.00000 0.14875 0.17929 = 0.21318 0.04539 0.06097 0.01791 C1D 1 0.482523 0.008433 0.558180 31.00000 0.14378 0.16288 = 0.19939 0.06526 0.07002 0.01197 AFIX 23 H1DA 2 0.504370 0.076928 0.576939 31.00000 -1.20000 H1DB 2 0.460341 -0.023698 0.583875 31.00000 -1.20000 AFIX 0 C2D 1 0.533723 -0.066543 0.549099 31.00000 0.13476 0.14412 = 0.17851 0.08260 0.08037 0.02204 AFIX 23 H2DA 2 0.567131 -0.091930 0.590945 31.00000 -1.20000 H2DB 2 0.507783 -0.129117 0.525024 31.00000 -1.20000 AFIX 0 PART 4 -31 O2D 4 0.457315 -0.064084 0.450863 -31.00000 0.14937 0.17124 = 0.21002 0.03447 0.05420 0.00668 C3D 1 0.447532 -0.044338 0.507935 -31.00000 0.14226 0.15841 = 0.19983 0.06179 0.06997 0.01074 AFIX 23 H3DA 2 0.478372 -0.091778 0.541932 -31.00000 -1.20000 H3DB 2 0.398698 -0.060082 0.500202 -31.00000 -1.20000 AFIX 0 C4D 1 0.464492 0.072703 0.528646 -31.00000 0.14385 0.16297 = 0.20733 0.05345 0.06568 0.01107 AFIX 23 H4DA 2 0.442260 0.123066 0.493342 -31.00000 -1.20000 H4DB 2 0.452264 0.091569 0.563873 -31.00000 -1.20000 AFIX 0 PART 0 PART 5 41 O1E 4 0.448589 0.476537 -0.062674 41.00000 0.18263 0.15487 = 0.29314 -0.00494 0.16243 -0.00402 C1E 1 0.450666 0.417811 -0.007506 41.00000 0.18240 0.15672 = 0.29096 -0.01210 0.16236 -0.00167 AFIX 23 H1EA 2 0.433135 0.344674 -0.019967 41.00000 -1.20000 H1EB 2 0.420428 0.453274 0.009557 41.00000 -1.20000 AFIX 0 C2E 1 0.526693 0.414238 0.043443 41.00000 0.18584 0.15882 = 0.29337 -0.01176 0.16092 0.00728 AFIX 23 H2EA 2 0.528792 0.373286 0.080327 41.00000 -1.20000 H2EB 2 0.556927 0.378662 0.026417 41.00000 -1.20000 AFIX 0 PART 6 -41 O2E 4 0.538671 0.459033 -0.032462 -41.00000 0.17945 0.14374 = 0.29409 -0.01271 0.16321 0.00659 C3E 1 0.427221 0.534672 -0.037937 -41.00000 0.17140 0.15088 = 0.28685 -0.01567 0.17384 0.00506 AFIX 23 H3EA 2 0.393248 0.593115 -0.055750 -41.00000 -1.20000 H3EB 2 0.402677 0.466075 -0.051916 -41.00000 -1.20000 AFIX 0 C4E 1 0.489348 0.545046 -0.059410 -41.00000 0.17897 0.14745 = 0.29373 -0.01512 0.16440 0.01042 AFIX 23 H4EA 2 0.470494 0.542371 -0.105911 -41.00000 -1.20000 H4EB 2 0.513221 0.614077 -0.045228 -41.00000 -1.20000 AFIX 0 PART 0 N1 3 0.353896 0.393455 0.503637 11.00000 0.03996 0.05487 = 0.05592 -0.01626 0.01799 -0.00740 C1 1 0.444257 0.316816 0.257574 11.00000 0.04621 0.04244 = 0.04128 -0.00828 0.01657 0.00139 C1A 1 0.594361 0.232327 0.786539 11.00000 0.15512 0.19730 = 0.19299 0.02168 0.00939 -0.03694 AFIX 23 H1AA 2 0.634036 0.186113 0.812172 11.00000 -1.20000 H1AB 2 0.610398 0.279534 0.761415 11.00000 -1.20000 AFIX 0 C1B 1 0.256141 0.182211 0.229986 11.00000 0.13708 0.15550 = 0.14788 0.00800 0.02443 -0.04101 AFIX 23 H1B1 2 0.267858 0.177892 0.193257 11.00000 -1.20000 H1B2 2 0.227307 0.246597 0.224596 11.00000 -1.20000 AFIX 0 O2 4 0.450805 0.454920 0.332138 11.00000 0.10069 0.04533 = 0.06393 -0.01386 0.04261 0.00644 O2A 4 0.471680 0.222936 0.709948 11.00000 0.14726 0.15314 = 0.11621 0.01609 -0.01670 -0.02535 O2B 4 0.255194 -0.007986 0.252467 11.00000 0.16791 0.16200 = 0.18845 0.01526 0.00311 -0.05440 N2 3 0.697922 0.050120 0.062395 11.00000 0.04095 0.04272 = 0.05385 -0.00337 0.02268 -0.00024 C2 1 0.482497 0.232067 0.247590 11.00000 0.03492 0.04312 = 0.03739 -0.00540 0.00491 0.00362 AFIX 43 H2 2 0.518329 0.198312 0.282407 11.00000 -1.20000 AFIX 0 C2A 1 0.536231 0.162626 0.741541 11.00000 0.14205 0.18458 = 0.16505 0.01044 0.00108 -0.02578 AFIX 23 H2AA 2 0.550477 0.132441 0.709629 11.00000 -1.20000 H2AB 2 0.528008 0.102973 0.765163 11.00000 -1.20000 AFIX 0 C2B 1 0.213055 0.087757 0.228824 11.00000 0.12500 0.14884 = 0.18203 0.00283 0.01876 -0.04837 AFIX 23 H2B1 2 0.187220 0.102564 0.254823 11.00000 -1.20000 H2B2 2 0.178464 0.075151 0.185084 11.00000 -1.20000 AFIX 0 O3 4 0.483363 0.080166 0.112976 11.00000 0.03241 0.04298 = 0.03141 -0.00536 0.00625 0.00947 N3 3 0.236433 0.752926 -0.031386 11.00000 0.03549 0.03562 = 0.04854 0.00408 0.00702 0.00147 C3 1 0.467177 0.197866 0.185650 11.00000 0.03183 0.04094 = 0.03484 -0.00489 0.00928 0.00432 C3A 1 0.457219 0.270499 0.759242 11.00000 0.17686 0.15249 = 0.15148 0.02578 -0.01294 -0.01768 AFIX 23 H3AA 2 0.451421 0.214774 0.786526 11.00000 -1.20000 H3AB 2 0.413771 0.312758 0.740931 11.00000 -1.20000 AFIX 0 C3B 1 0.314035 0.004611 0.307676 11.00000 0.13488 0.15879 = 0.16595 0.02575 0.03367 -0.04406 AFIX 23 H3B1 2 0.342933 -0.060384 0.316366 11.00000 -1.20000 H3B2 2 0.300434 0.015323 0.342958 11.00000 -1.20000 AFIX 0 O4 4 0.555622 0.058963 0.217579 11.00000 0.05560 0.07046 = 0.03735 -0.00593 0.00180 0.02947 PART 7 51 N4 3 0.357262 0.541451 0.632699 51.00000 0.05038 0.05462 = 0.07587 -0.01871 0.02093 0.00316 O7 4 0.320330 0.562099 0.575222 51.00000 0.04553 0.05005 = 0.06448 -0.00982 0.02518 -0.01375 O8 4 0.362024 0.447264 0.654034 51.00000 0.07562 0.06633 = 0.06440 -0.00277 0.01170 0.01121 O9 4 0.387452 0.618581 0.668359 51.00000 0.06519 0.08206 = 0.09584 -0.05142 0.01996 -0.02360 PART 8 -51 N4' 3 0.365908 0.525158 0.650622 -51.00000 0.05480 0.06271 = 0.07772 -0.02673 0.02849 -0.00900 O7' 4 0.338321 0.602029 0.616515 -51.00000 0.09188 0.07419 = 0.09255 -0.03292 0.04098 -0.02492 O8' 4 0.348286 0.427929 0.626204 -51.00000 0.05327 0.05889 = 0.08083 -0.02025 0.02690 -0.00147 O9' 4 0.403352 0.535579 0.705923 -51.00000 0.05661 0.07980 = 0.08965 -0.03402 0.00939 -0.00368 PART 0 C4 1 0.412062 0.245907 0.133857 11.00000 0.04029 0.03851 = 0.03754 -0.00518 0.00975 0.00504 AFIX 43 H4 2 0.402387 0.224157 0.092163 11.00000 -1.20000 AFIX 0 C4A 1 0.518084 0.341018 0.796948 11.00000 0.19232 0.16592 = 0.18203 0.00455 0.00064 -0.02226 AFIX 23 H4AA 2 0.522219 0.396863 0.768913 11.00000 -1.20000 H4AB 2 0.508459 0.376606 0.830217 11.00000 -1.20000 AFIX 0 C4B 1 0.353729 0.093812 0.303391 11.00000 0.14286 0.14767 = 0.14762 0.02211 0.01820 -0.04982 AFIX 23 H4B1 2 0.373757 0.075512 0.273216 11.00000 -1.20000 H4B2 2 0.393236 0.103474 0.345049 11.00000 -1.20000 AFIX 0 O5 4 0.314618 0.365160 0.034141 11.00000 0.05035 0.04711 = 0.04195 0.00550 0.01117 0.01381 N5 3 0.190840 0.526230 0.408454 11.00000 0.07207 0.07501 = 0.08760 0.02135 0.04499 0.02581 C5 1 0.371514 0.326384 0.144506 11.00000 0.04910 0.03981 = 0.04358 0.00452 0.01178 0.01079 O6 4 0.256655 0.408396 0.095449 11.00000 0.07312 0.10119 = 0.06445 0.02212 0.02812 0.04698 C6 1 0.388482 0.362850 0.206296 11.00000 0.05479 0.04186 = 0.04907 -0.00256 0.02064 0.01319 AFIX 43 H6 2 0.362220 0.418503 0.213249 11.00000 -1.20000 AFIX 0 C7 1 0.462292 0.361366 0.323053 11.00000 0.05381 0.04965 = 0.04814 -0.01143 0.02035 -0.00005 C8 1 0.508078 0.317497 0.433718 11.00000 0.05051 0.04529 = 0.04637 -0.01050 0.01893 -0.00448 C9 1 0.577398 0.319775 0.474577 11.00000 0.05148 0.05693 = 0.05426 -0.01078 0.02375 -0.00205 AFIX 43 H9 2 0.611699 0.303810 0.459588 11.00000 -1.20000 AFIX 0 O10 4 0.192018 0.440676 0.436712 11.00000 0.06092 0.06862 = 0.07607 0.02218 0.03229 0.00992 C10 1 0.598542 0.346124 0.539882 11.00000 0.04386 0.06848 = 0.05668 -0.01342 0.01326 -0.00308 AFIX 43 H10 2 0.646497 0.347048 0.567963 11.00000 -1.20000 AFIX 0 O11 4 0.227269 0.603714 0.437780 11.00000 0.08007 0.08983 = 0.13772 0.00740 0.05559 -0.00668 C11 1 0.548734 0.369899 0.561177 11.00000 0.04742 0.06008 = 0.05075 -0.01042 0.01309 0.00113 AFIX 43 H11 2 0.562745 0.386974 0.604292 11.00000 -1.20000 AFIX 0 O12 4 0.148709 0.530472 0.348654 11.00000 0.13372 0.12087 = 0.07206 0.03216 0.03440 0.04882 C12 1 0.476431 0.369494 0.519936 11.00000 0.04725 0.04454 = 0.05039 -0.01330 0.01930 -0.00542 C13 1 0.454172 0.340881 0.454344 11.00000 0.05118 0.04194 = 0.04160 -0.00937 0.01229 -0.00299 C14 1 0.379484 0.338366 0.415626 11.00000 0.04845 0.06370 = 0.04556 -0.01752 0.01486 -0.00823 AFIX 43 H14 2 0.362752 0.317843 0.372745 11.00000 -1.20000 AFIX 0 C15 1 0.333050 0.364982 0.439851 11.00000 0.04061 0.06331 = 0.05054 -0.01841 0.01157 -0.00625 AFIX 43 H15 2 0.284766 0.364359 0.412770 11.00000 -1.20000 AFIX 0 C16 1 0.422563 0.395948 0.540879 11.00000 0.05144 0.04961 = 0.04834 -0.01105 0.02046 -0.00367 AFIX 43 H16 2 0.436772 0.416268 0.583551 11.00000 -1.20000 AFIX 0 C17 1 0.507142 0.104583 0.176183 11.00000 0.03298 0.04539 = 0.03295 -0.00424 0.00730 0.00177 C18 1 0.515720 -0.006307 0.095423 11.00000 0.03326 0.03815 = 0.03075 -0.00236 0.00563 0.00707 C19 1 0.483409 -0.103980 0.082431 11.00000 0.03653 0.04660 = 0.04574 -0.00117 0.01214 -0.00064 AFIX 43 H19 2 0.442252 -0.115652 0.088499 11.00000 -1.20000 AFIX 0 C20 1 0.512977 -0.188761 0.059379 11.00000 0.04678 0.03863 = 0.05430 -0.01090 0.01297 -0.00473 AFIX 43 H20 2 0.492142 -0.257116 0.051947 11.00000 -1.20000 AFIX 0 C21 1 0.571792 -0.170486 0.048073 11.00000 0.04809 0.03594 = 0.05295 -0.00724 0.02139 0.00376 AFIX 43 H21 2 0.589738 -0.225497 0.031342 11.00000 -1.20000 AFIX 0 C22 1 0.605294 -0.068520 0.061701 11.00000 0.03719 0.03530 = 0.03867 -0.00145 0.01065 0.00300 C23 1 0.577378 0.015629 0.086910 11.00000 0.03357 0.03570 = 0.03218 -0.00145 0.00858 0.00509 C24 1 0.613999 0.115791 0.100526 11.00000 0.04305 0.03737 = 0.05315 -0.00828 0.01963 0.00275 AFIX 43 H24 2 0.598101 0.172318 0.117980 11.00000 -1.20000 AFIX 0 C25 1 0.671857 0.129851 0.088351 11.00000 0.05034 0.03959 = 0.05963 -0.00853 0.02276 -0.00578 AFIX 43 H25 2 0.695033 0.196421 0.097970 11.00000 -1.20000 AFIX 0 C26 1 0.665738 -0.044396 0.050687 11.00000 0.04294 0.04095 = 0.04322 -0.00301 0.01679 0.00824 AFIX 43 H26 2 0.684099 -0.098957 0.034024 11.00000 -1.20000 AFIX 0 C27 1 0.308168 0.370023 0.090854 11.00000 0.05767 0.04795 = 0.04941 0.00407 0.01468 0.01810 C28 1 0.259941 0.413507 -0.018406 11.00000 0.04252 0.03928 = 0.04641 0.00248 0.00629 0.00601 C29 1 0.215904 0.351040 -0.067189 11.00000 0.05450 0.04607 = 0.05983 -0.00421 0.00567 -0.00242 AFIX 43 H29 2 0.220592 0.276011 -0.065067 11.00000 -1.20000 AFIX 0 C30 1 0.162396 0.401121 -0.121726 11.00000 0.05628 0.05943 = 0.05981 -0.01421 -0.00568 -0.00779 AFIX 43 H30 2 0.133200 0.358103 -0.155931 11.00000 -1.20000 AFIX 0 C31 1 0.152805 0.508298 -0.125293 11.00000 0.04807 0.05599 = 0.04726 -0.00381 -0.00796 -0.00496 AFIX 43 H31 2 0.115772 0.539034 -0.160506 11.00000 -1.20000 AFIX 0 C32 1 0.199406 0.574577 -0.075108 11.00000 0.03602 0.04517 = 0.03688 0.00121 0.00256 -0.00388 C33 1 0.254591 0.528093 -0.020663 11.00000 0.03580 0.04081 = 0.04029 0.00055 0.00286 -0.00038 C34 1 0.301090 0.598925 0.026880 11.00000 0.03965 0.04674 = 0.04135 -0.00126 -0.00248 0.00521 AFIX 43 H34 2 0.338723 0.570779 0.062648 11.00000 -1.20000 AFIX 0 C35 1 0.291111 0.707614 0.020604 11.00000 0.03918 0.04371 = 0.04424 -0.00409 -0.00050 0.00070 AFIX 43 H35 2 0.322215 0.752814 0.052449 11.00000 -1.20000 AFIX 0 C36 1 0.192500 0.688929 -0.076373 11.00000 0.03688 0.04830 = 0.04129 0.00969 0.00409 0.00351 AFIX 43 H36 2 0.154920 0.720349 -0.110834 11.00000 -1.20000 REM ##### REM ##### AFIX 0 HKLF 4 REM KGW2_a.res in P2(1)/n REM wR2 = 0.2694, GooF = S = 0.921, Restrained GooF = 0.938 for all data REM R1 = 0.0789 for 6332 Fo > 4sig(Fo) and 0.1466 for all 13355 data REM 851 parameters refined using 924 restraints END WGHT 0.1719 0.0000 REM Highest difference peak 0.760, deepest hole -0.540, 1-sigma level 0.092 Q1 1 0.2593 0.4747 0.5118 11.00000 0.05 0.76 Q2 1 0.2679 0.5738 0.4903 11.00000 0.05 0.70 Q3 1 0.4529 0.5272 0.3716 11.00000 0.05 0.65 Q4 1 0.5787 0.4299 0.5396 11.00000 0.05 0.65 Q5 1 0.5902 0.5003 0.5906 11.00000 0.05 0.59 Q6 1 0.3405 0.4696 0.4790 11.00000 0.05 0.58 Q7 1 0.7310 -0.3119 0.2018 11.00000 0.05 0.58 Q8 1 0.9103 -0.1248 0.3675 11.00000 0.05 0.54 Q9 1 0.5010 0.3880 0.6097 11.00000 0.05 0.54 Q10 1 0.6208 0.4544 0.5027 11.00000 0.05 0.53 Q11 1 0.2712 0.1105 0.3186 11.00000 0.05 0.53 Q12 1 0.4961 0.3143 0.5631 11.00000 0.05 0.51 Q13 1 0.7286 -0.0226 0.2465 11.00000 0.05 0.51 Q14 1 0.3623 0.4223 0.3910 11.00000 0.05 0.48 Q15 1 0.6881 -0.1538 0.2196 11.00000 0.05 0.47 Q16 1 0.5183 0.3486 0.3719 11.00000 0.05 0.47 Q17 1 0.7024 -0.3192 0.2489 11.00000 0.05 0.45 Q18 1 0.4534 0.5760 -0.1518 11.00000 0.05 0.45 Q19 1 0.5537 0.3268 0.8376 11.00000 0.05 0.44 Q20 1 0.7002 -0.1263 0.2417 11.00000 0.05 0.42 Q21 1 0.2177 0.0842 0.2703 11.00000 0.05 0.40 Q22 1 0.5451 -0.0069 0.5801 11.00000 0.05 0.39 Q23 1 0.5138 0.2872 0.7062 11.00000 0.05 0.38 Q24 1 0.4817 0.3607 0.7989 11.00000 0.05 0.37 Q25 1 0.8209 -0.1905 0.2683 11.00000 0.05 0.36 Q26 1 0.5300 0.3395 0.5175 11.00000 0.05 0.36 Q27 1 0.3831 0.5816 -0.1011 11.00000 0.05 0.35 Q28 1 0.2297 0.5253 0.4514 11.00000 0.05 0.34 Q29 1 0.5387 0.2323 0.7023 11.00000 0.05 0.33 Q30 1 0.1895 0.1788 0.2099 11.00000 0.05 0.33 Q31 1 0.2569 0.2230 0.2895 11.00000 0.05 0.33 Q32 1 0.7777 -0.0127 0.2519 11.00000 0.05 0.32 Q33 1 0.3318 0.4429 0.5814 11.00000 0.05 0.32 Q34 1 0.4563 0.4312 -0.0763 11.00000 0.05 0.32 Q35 1 0.3620 0.5049 -0.1115 11.00000 0.05 0.32 Q36 1 0.4222 0.4634 -0.1520 11.00000 0.05 0.31 Q37 1 0.2318 0.3908 0.4807 11.00000 0.05 0.31 Q38 1 0.2939 0.5155 0.5591 11.00000 0.05 0.30 Q39 1 0.5126 0.3415 0.7302 11.00000 0.05 0.30 Q40 1 0.2826 0.2739 0.2569 11.00000 0.05 0.30 Q41 1 0.5562 0.3479 0.7590 11.00000 0.05 0.29 Q42 1 0.2045 0.5603 0.3663 11.00000 0.05 0.29 Q43 1 0.4092 0.4198 -0.1166 11.00000 0.05 0.28 Q44 1 0.2105 0.8197 -0.0307 11.00000 0.05 0.26 Q45 1 0.1947 0.2204 0.1915 11.00000 0.05 0.26 Q46 1 0.5862 0.2184 0.7262 11.00000 0.05 0.25 Q47 1 0.4461 0.4430 -0.1287 11.00000 0.05 0.25 Q48 1 0.6080 0.1818 0.7620 11.00000 0.05 0.25 Q49 1 0.4016 0.0979 0.5132 11.00000 0.05 0.25 Q50 1 0.8427 0.0095 0.3381 11.00000 0.05 0.25 ; _shelx_res_checksum 76472 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 Cu01 Cu 0.27724(3) 0.42148(4) 0.53428(3) 0.04588(19) Uani 1 1 d . U . . . O1 O 0.48978(16) 0.2857(2) 0.36963(13) 0.0525(7) Uani 1 1 d . U . . . O1A O 0.5788(5) 0.2899(8) 0.8238(4) 0.202(3) Uani 1 1 d . U . . . O1B O 0.3185(3) 0.1953(5) 0.2845(2) 0.1179(16) Uani 1 1 d . U . . . O1C O 0.7504(12) -0.0819(16) 0.2046(11) 0.216(4) Uani 0.409(7) 1 d D U P A 1 O2C O 0.7123(10) -0.2128(17) 0.2848(9) 0.194(4) Uani 0.409(7) 1 d D U P A 1 C1C C 0.8089(13) -0.103(2) 0.2665(11) 0.208(4) Uani 0.409(7) 1 d D U P A 1 H1CA H 0.829046 -0.034338 0.286911 0.249 Uiso 0.409(7) 1 calc R U P A 1 H1CB H 0.845744 -0.142892 0.260267 0.249 Uiso 0.409(7) 1 calc R U P A 1 C2C C 0.7841(13) -0.167(3) 0.3106(9) 0.197(4) Uani 0.409(7) 1 d D U P A 1 H2CA H 0.817126 -0.227121 0.328276 0.237 Uiso 0.409(7) 1 calc R U P A 1 H2CB H 0.789045 -0.120798 0.346283 0.237 Uiso 0.409(7) 1 calc R U P A 1 C3C C 0.7000(14) -0.257(2) 0.2234(11) 0.222(5) Uani 0.409(7) 1 d D U P A 1 H3CA H 0.649910 -0.275411 0.201486 0.266 Uiso 0.409(7) 1 calc R U P A 1 H3CB H 0.726373 -0.324826 0.230544 0.266 Uiso 0.409(7) 1 calc R U P A 1 C4C C 0.7196(17) -0.188(2) 0.1778(8) 0.226(5) Uani 0.409(7) 1 d D U P A 1 H4CA H 0.753445 -0.227049 0.166696 0.271 Uiso 0.409(7) 1 calc R U P A 1 H4CB H 0.677236 -0.175807 0.138497 0.271 Uiso 0.409(7) 1 calc R U P A 1 O3C O 0.7772(9) -0.0631(10) 0.2998(7) 0.222(4) Uani 0.591(7) 1 d D U P A 2 O4C O 0.7441(8) -0.2180(12) 0.1997(7) 0.220(4) Uani 0.591(7) 1 d D U P A 2 C5C C 0.8200(9) -0.1585(16) 0.3177(9) 0.184(4) Uani 0.591(7) 1 d D U P A 2 H5CA H 0.807209 -0.201525 0.346686 0.221 Uiso 0.591(7) 1 calc R U P A 2 H5CB H 0.869680 -0.138348 0.340130 0.221 Uiso 0.591(7) 1 calc R U P A 2 C6C C 0.8092(9) -0.2303(17) 0.2549(8) 0.195(4) Uani 0.591(7) 1 d D U P A 2 H6C1 H 0.847623 -0.213031 0.242787 0.235 Uiso 0.591(7) 1 calc R U P A 2 H6C2 H 0.814107 -0.306057 0.267264 0.235 Uiso 0.591(7) 1 calc R U P A 2 C7C C 0.7194(13) -0.1063(16) 0.1999(10) 0.217(4) Uani 0.591(7) 1 d D U P A 2 H7C1 H 0.676065 -0.094028 0.161448 0.260 Uiso 0.591(7) 1 calc R U P A 2 H7C2 H 0.755109 -0.055795 0.199546 0.260 Uiso 0.591(7) 1 calc R U P A 2 C8C C 0.7055(8) -0.0867(17) 0.2576(9) 0.201(4) Uani 0.591(7) 1 d D U P A 2 H8C1 H 0.673948 -0.025729 0.252241 0.242 Uiso 0.591(7) 1 calc R U P A 2 H8C2 H 0.687505 -0.150500 0.270629 0.242 Uiso 0.591(7) 1 calc R U P A 2 O1D O 0.4272(4) 0.0210(17) 0.4833(9) 0.185(5) Uani 0.526(9) 1 d D U P B 3 C1D C 0.4825(13) 0.008(2) 0.5582(13) 0.169(5) Uani 0.526(9) 1 d . U P B 3 H1DA H 0.504370 0.076928 0.576939 0.203 Uiso 0.526(9) 1 calc R U P B 3 H1DB H 0.460341 -0.023698 0.583875 0.203 Uiso 0.526(9) 1 calc R U P B 3 C2D C 0.5337(10) -0.0665(15) 0.5491(10) 0.147(5) Uani 0.526(9) 1 d . U P B 3 H2DA H 0.567131 -0.091930 0.590945 0.177 Uiso 0.526(9) 1 calc R U P B 3 H2DB H 0.507783 -0.129117 0.525024 0.177 Uiso 0.526(9) 1 calc R U P B 3 O2D O 0.4573(10) -0.0641(14) 0.4509(10) 0.184(5) Uani 0.474(9) 1 d . U P B 4 C3D C 0.4475(16) -0.044(2) 0.5079(17) 0.167(5) Uani 0.474(9) 1 d . U P B 4 H3DA H 0.478372 -0.091778 0.541932 0.201 Uiso 0.474(9) 1 calc R U P B 4 H3DB H 0.398698 -0.060082 0.500202 0.201 Uiso 0.474(9) 1 calc R U P B 4 C4D C 0.4645(16) 0.073(2) 0.5286(17) 0.174(5) Uani 0.474(9) 1 d . U P B 4 H4DA H 0.442260 0.123066 0.493342 0.209 Uiso 0.474(9) 1 calc R U P B 4 H4DB H 0.452264 0.091569 0.563873 0.209 Uiso 0.474(9) 1 calc R U P B 4 O1E O 0.4486(12) 0.477(3) -0.0627(7) 0.189(5) Uani 0.238(9) 1 d D U P C 5 C1E C 0.4507(16) 0.418(2) -0.0075(17) 0.189(6) Uani 0.238(9) 1 d D U P C 5 H1EA H 0.433135 0.344674 -0.019967 0.226 Uiso 0.238(9) 1 calc R U P C 5 H1EB H 0.420428 0.453274 0.009557 0.226 Uiso 0.238(9) 1 calc R U P C 5 C2E C 0.5267(19) 0.4142(19) 0.0434(14) 0.192(6) Uani 0.238(9) 1 d D U P C 5 H2EA H 0.528792 0.373286 0.080327 0.231 Uiso 0.238(9) 1 calc R U P C 5 H2EB H 0.556927 0.378662 0.026417 0.231 Uiso 0.238(9) 1 calc R U P C 5 O2E O 0.5387(6) 0.4590(9) -0.0325(7) 0.184(4) Uani 0.762(9) 1 d D U P C 6 C3E C 0.4272(7) 0.5347(14) -0.0379(7) 0.177(4) Uani 0.762(9) 1 d . U P C 6 H3EA H 0.393248 0.593115 -0.055750 0.212 Uiso 0.762(9) 1 calc R U P C 6 H3EB H 0.402677 0.466075 -0.051916 0.212 Uiso 0.762(9) 1 calc R U P C 6 C4E C 0.4893(8) 0.5450(13) -0.0594(5) 0.185(4) Uani 0.762(9) 1 d D U P C 6 H4EA H 0.470494 0.542371 -0.105911 0.221 Uiso 0.762(9) 1 calc R U P C 6 H4EB H 0.513221 0.614077 -0.045228 0.221 Uiso 0.762(9) 1 calc R U P C 6 N1 N 0.35390(18) 0.3935(3) 0.50364(17) 0.0510(8) Uani 1 1 d . U . . . C1 C 0.4443(2) 0.3168(3) 0.25757(18) 0.0439(9) Uani 1 1 d . U . . . C1A C 0.5944(7) 0.2323(12) 0.7865(7) 0.203(4) Uani 1 1 d . U . . . H1AA H 0.634036 0.186113 0.812172 0.244 Uiso 1 1 calc R U . . . H1AB H 0.610398 0.279534 0.761415 0.244 Uiso 1 1 calc R U . . . C1B C 0.2561(5) 0.1822(8) 0.2300(5) 0.159(3) Uani 1 1 d D U . . . H1B1 H 0.267858 0.177892 0.193257 0.190 Uiso 1 1 calc R U . . . H1B2 H 0.227307 0.246597 0.224596 0.190 Uiso 1 1 calc R U . . . O2 O 0.4508(2) 0.4549(3) 0.33214(16) 0.0672(9) Uani 1 1 d . U . . . O2A O 0.4717(4) 0.2229(6) 0.7099(3) 0.163(2) Uani 1 1 d . U . . . O2B O 0.2552(5) -0.0080(7) 0.2525(4) 0.197(3) Uani 1 1 d . U . . . N2 N 0.69792(17) 0.0501(3) 0.06239(16) 0.0449(8) Uani 1 1 d . U . . . C2 C 0.4825(2) 0.2321(3) 0.24759(18) 0.0419(9) Uani 1 1 d . U . . . H2 H 0.518329 0.198312 0.282407 0.050 Uiso 1 1 calc R U . . . C2A C 0.5362(6) 0.1626(10) 0.7415(6) 0.185(4) Uani 1 1 d . U . . . H2AA H 0.550477 0.132441 0.709629 0.222 Uiso 1 1 calc R U . . . H2AB H 0.528008 0.102973 0.765163 0.222 Uiso 1 1 calc R U . . . C2B C 0.2131(6) 0.0878(8) 0.2288(6) 0.167(3) Uani 1 1 d D U . . . H2B1 H 0.187220 0.102564 0.254823 0.201 Uiso 1 1 calc R U . . . H2B2 H 0.178464 0.075151 0.185084 0.201 Uiso 1 1 calc R U . . . O3 O 0.48336(13) 0.0802(2) 0.11298(11) 0.0380(6) Uani 1 1 d . U . . . N3 N 0.23643(16) 0.7529(3) -0.03139(15) 0.0435(7) Uani 1 1 d . U . . . C3 C 0.46718(18) 0.1979(3) 0.18565(17) 0.0374(8) Uani 1 1 d . U . . . C3A C 0.4572(6) 0.2705(10) 0.7592(5) 0.188(4) Uani 1 1 d . U . . . H3AA H 0.451421 0.214774 0.786526 0.225 Uiso 1 1 calc R U . . . H3AB H 0.413771 0.312758 0.740931 0.225 Uiso 1 1 calc R U . . . C3B C 0.3140(6) 0.0046(9) 0.3077(5) 0.163(3) Uani 1 1 d . U . . . H3B1 H 0.342933 -0.060384 0.316366 0.196 Uiso 1 1 calc R U . . . H3B2 H 0.300434 0.015323 0.342958 0.196 Uiso 1 1 calc R U . . . O4 O 0.55562(17) 0.0590(3) 0.21758(13) 0.0604(9) Uani 1 1 d . U . . . N4 N 0.3573(7) 0.5415(10) 0.6327(6) 0.062(2) Uani 0.646(7) 1 d . U P D 7 O7 O 0.3203(3) 0.5621(4) 0.5752(3) 0.0526(13) Uani 0.646(7) 1 d . U P D 7 O8 O 0.3620(5) 0.4473(7) 0.6540(4) 0.075(2) Uani 0.646(7) 1 d . U P D 7 O9 O 0.3875(3) 0.6186(6) 0.6684(3) 0.086(2) Uani 0.646(7) 1 d . U P D 7 N4' N 0.3659(15) 0.5252(18) 0.6506(11) 0.065(3) Uani 0.354(7) 1 d D U P D 8 O7' O 0.3383(8) 0.6020(11) 0.6165(7) 0.085(3) Uani 0.354(7) 1 d D U P D 8 O8' O 0.3483(7) 0.4279(12) 0.6262(7) 0.065(3) Uani 0.354(7) 1 d . U P D 8 O9' O 0.4034(6) 0.5356(11) 0.7059(6) 0.083(3) Uani 0.354(7) 1 d . U P D 8 C4 C 0.41206(19) 0.2459(3) 0.13386(18) 0.0410(8) Uani 1 1 d . U . . . H4 H 0.402387 0.224157 0.092163 0.049 Uiso 1 1 calc R U . . . C4A C 0.5181(7) 0.3410(10) 0.7969(7) 0.206(4) Uani 1 1 d . U . . . H4AA H 0.522219 0.396863 0.768913 0.248 Uiso 1 1 calc R U . . . H4AB H 0.508459 0.376606 0.830217 0.248 Uiso 1 1 calc R U . . . C4B C 0.3537(6) 0.0938(9) 0.3034(5) 0.160(3) Uani 1 1 d . U . . . H4B1 H 0.373757 0.075512 0.273216 0.193 Uiso 1 1 calc R U . . . H4B2 H 0.393236 0.103474 0.345049 0.193 Uiso 1 1 calc R U . . . O5 O 0.31462(15) 0.3652(2) 0.03414(13) 0.0492(7) Uani 1 1 d . U . . . N5 N 0.1908(3) 0.5262(4) 0.4085(3) 0.0743(12) Uani 1 1 d . U . . . C5 C 0.3715(2) 0.3264(3) 0.14451(19) 0.0467(9) Uani 1 1 d . U . . . O6 O 0.2567(2) 0.4084(3) 0.09545(17) 0.0798(11) Uani 1 1 d . U . . . C6 C 0.3885(2) 0.3628(3) 0.2063(2) 0.0489(10) Uani 1 1 d . U . . . H6 H 0.362220 0.418503 0.213249 0.059 Uiso 1 1 calc R U . . . C7 C 0.4623(2) 0.3614(4) 0.3231(2) 0.0509(10) Uani 1 1 d . U . . . C8 C 0.5081(2) 0.3175(3) 0.4337(2) 0.0478(9) Uani 1 1 d . U . . . C9 C 0.5774(2) 0.3198(4) 0.4746(2) 0.0537(10) Uani 1 1 d . U . . . H9 H 0.611699 0.303810 0.459588 0.064 Uiso 1 1 calc R U . . . O10 O 0.19202(18) 0.4407(3) 0.43671(17) 0.0673(9) Uani 1 1 d . U . . . C10 C 0.5985(2) 0.3461(4) 0.5399(2) 0.0590(11) Uani 1 1 d . U . . . H10 H 0.646497 0.347048 0.567963 0.071 Uiso 1 1 calc R U . . . O11 O 0.2273(2) 0.6037(4) 0.4378(3) 0.0992(14) Uani 1 1 d . U . . . C11 C 0.5487(2) 0.3699(4) 0.5612(2) 0.0553(10) Uani 1 1 d . U . . . H11 H 0.562745 0.386974 0.604292 0.066 Uiso 1 1 calc R U . . . O12 O 0.1487(3) 0.5305(4) 0.3487(2) 0.1118(16) Uani 1 1 d . U . . . C12 C 0.4764(2) 0.3695(3) 0.5199(2) 0.0478(9) Uani 1 1 d . U . . . C13 C 0.4542(2) 0.3409(3) 0.45434(19) 0.0473(9) Uani 1 1 d . U . . . C14 C 0.3795(2) 0.3384(4) 0.4156(2) 0.0542(11) Uani 1 1 d . U . . . H14 H 0.362752 0.317843 0.372745 0.065 Uiso 1 1 calc R U . . . C15 C 0.3330(2) 0.3650(4) 0.4399(2) 0.0540(11) Uani 1 1 d . U . . . H15 H 0.284766 0.364359 0.412770 0.065 Uiso 1 1 calc R U . . . C16 C 0.4226(2) 0.3959(3) 0.5409(2) 0.0499(10) Uani 1 1 d . U . . . H16 H 0.436772 0.416268 0.583551 0.060 Uiso 1 1 calc R U . . . C17 C 0.5071(2) 0.1046(3) 0.17618(17) 0.0393(8) Uani 1 1 d . U . . . C18 C 0.51572(19) -0.0063(3) 0.09542(16) 0.0367(8) Uani 1 1 d . U . . . C19 C 0.4834(2) -0.1040(3) 0.08243(19) 0.0447(9) Uani 1 1 d . U . . . H19 H 0.442252 -0.115652 0.088499 0.054 Uiso 1 1 calc R U . . . C20 C 0.5130(2) -0.1888(3) 0.0594(2) 0.0493(10) Uani 1 1 d . U . . . H20 H 0.492142 -0.257116 0.051947 0.059 Uiso 1 1 calc R U . . . C21 C 0.5718(2) -0.1705(3) 0.04807(19) 0.0456(9) Uani 1 1 d . U . . . H21 H 0.589738 -0.225497 0.031342 0.055 Uiso 1 1 calc R U . . . C22 C 0.6053(2) -0.0685(3) 0.06170(18) 0.0388(8) Uani 1 1 d . U . . . C23 C 0.57738(19) 0.0156(3) 0.08691(17) 0.0356(8) Uani 1 1 d . U . . . C24 C 0.6140(2) 0.1158(3) 0.1005(2) 0.0447(9) Uani 1 1 d . U . . . H24 H 0.598101 0.172318 0.117980 0.054 Uiso 1 1 calc R U . . . C25 C 0.6719(2) 0.1299(3) 0.0884(2) 0.0499(10) Uani 1 1 d . U . . . H25 H 0.695033 0.196421 0.097970 0.060 Uiso 1 1 calc R U . . . C26 C 0.6657(2) -0.0444(3) 0.05069(18) 0.0428(9) Uani 1 1 d . U . . . H26 H 0.684099 -0.098957 0.034024 0.051 Uiso 1 1 calc R U . . . C27 C 0.3082(2) 0.3700(4) 0.0909(2) 0.0543(10) Uani 1 1 d . U . . . C28 C 0.2599(2) 0.4135(3) -0.0184(2) 0.0469(9) Uani 1 1 d . U . . . C29 C 0.2159(2) 0.3510(4) -0.0672(2) 0.0596(12) Uani 1 1 d . U . . . H29 H 0.220592 0.276011 -0.065067 0.072 Uiso 1 1 calc R U . . . C30 C 0.1624(3) 0.4011(4) -0.1217(2) 0.0686(14) Uani 1 1 d . U . . . H30 H 0.133200 0.358103 -0.155931 0.082 Uiso 1 1 calc R U . . . C31 C 0.1528(2) 0.5083(4) -0.1253(2) 0.0599(12) Uani 1 1 d . U . . . H31 H 0.115772 0.539034 -0.160506 0.072 Uiso 1 1 calc R U . . . C32 C 0.1994(2) 0.5746(3) -0.07511(18) 0.0436(9) Uani 1 1 d . U . . . C33 C 0.2546(2) 0.5281(3) -0.02066(18) 0.0434(9) Uani 1 1 d . U . . . C34 C 0.3011(2) 0.5989(3) 0.0269(2) 0.0491(10) Uani 1 1 d . U . . . H34 H 0.338723 0.570779 0.062648 0.059 Uiso 1 1 calc R U . . . C35 C 0.2911(2) 0.7076(3) 0.02060(19) 0.0484(9) Uani 1 1 d . U . . . H35 H 0.322215 0.752814 0.052449 0.058 Uiso 1 1 calc R U . . . C36 C 0.1925(2) 0.6889(3) -0.07637(19) 0.0463(9) Uani 1 1 d . U . . . H36 H 0.154920 0.720349 -0.110834 0.056 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 Cu01 0.0397(3) 0.0435(3) 0.0568(3) -0.0076(2) 0.0224(2) -0.0059(2) O1 0.0596(17) 0.0570(18) 0.0394(15) -0.0085(13) 0.0192(14) 0.0095(14) O1A 0.173(5) 0.171(5) 0.175(5) -0.003(4) -0.014(4) -0.042(5) O1B 0.116(4) 0.122(4) 0.091(3) -0.026(3) 0.019(3) -0.028(3) O1C 0.200(7) 0.259(8) 0.187(6) 0.065(6) 0.078(6) 0.070(7) O2C 0.188(7) 0.255(8) 0.171(7) 0.063(7) 0.109(7) 0.072(7) C1C 0.201(7) 0.251(7) 0.181(6) 0.059(6) 0.090(6) 0.074(7) C2C 0.199(7) 0.241(7) 0.170(6) 0.068(6) 0.095(6) 0.076(7) C3C 0.205(8) 0.264(9) 0.194(8) 0.064(8) 0.081(8) 0.059(8) C4C 0.207(8) 0.264(8) 0.194(7) 0.066(7) 0.072(7) 0.068(8) O3C 0.218(7) 0.257(8) 0.192(6) 0.045(6) 0.087(6) 0.082(7) O4C 0.199(7) 0.264(8) 0.195(6) 0.057(6) 0.082(6) 0.073(7) C5C 0.188(7) 0.228(8) 0.163(6) 0.075(6) 0.101(6) 0.085(7) C6C 0.192(7) 0.232(7) 0.176(6) 0.063(6) 0.091(5) 0.071(6) C7C 0.200(7) 0.259(8) 0.187(6) 0.062(7) 0.075(6) 0.077(7) C8C 0.188(7) 0.254(8) 0.175(6) 0.055(6) 0.090(6) 0.087(7) O1D 0.149(8) 0.179(10) 0.213(11) 0.045(9) 0.061(7) 0.018(7) C1D 0.144(8) 0.163(10) 0.199(11) 0.065(9) 0.070(8) 0.012(8) C2D 0.135(9) 0.144(10) 0.179(11) 0.083(9) 0.080(8) 0.022(8) O2D 0.149(9) 0.171(10) 0.210(11) 0.034(9) 0.054(9) 0.007(8) C3D 0.142(8) 0.158(10) 0.200(11) 0.062(9) 0.070(8) 0.011(7) C4D 0.144(9) 0.163(11) 0.207(12) 0.053(9) 0.066(9) 0.011(9) O1E 0.183(9) 0.155(8) 0.293(11) -0.005(9) 0.162(10) -0.004(7) C1E 0.182(10) 0.157(9) 0.291(12) -0.012(10) 0.162(11) -0.002(8) C2E 0.186(11) 0.159(10) 0.293(12) -0.012(10) 0.161(11) 0.007(9) O2E 0.179(8) 0.144(6) 0.294(10) -0.013(7) 0.163(9) 0.007(5) C3E 0.171(9) 0.151(8) 0.287(11) -0.016(9) 0.174(9) 0.005(6) C4E 0.179(9) 0.147(8) 0.294(11) -0.015(8) 0.164(9) 0.010(6) N1 0.0400(18) 0.055(2) 0.056(2) -0.0163(16) 0.0180(17) -0.0074(15) C1 0.046(2) 0.042(2) 0.041(2) -0.0083(16) 0.0166(18) 0.0014(17) C1A 0.155(7) 0.197(8) 0.193(8) 0.022(6) 0.009(6) -0.037(6) C1B 0.137(6) 0.155(6) 0.148(6) 0.008(5) 0.024(5) -0.041(5) O2 0.101(3) 0.0453(18) 0.064(2) -0.0139(15) 0.043(2) 0.0064(18) O2A 0.147(5) 0.153(5) 0.116(4) 0.016(4) -0.017(4) -0.025(4) O2B 0.168(6) 0.162(6) 0.188(5) 0.015(5) 0.003(4) -0.054(5) N2 0.0409(17) 0.0427(19) 0.0539(19) -0.0034(15) 0.0227(16) -0.0002(14) C2 0.0349(18) 0.043(2) 0.0374(19) -0.0054(16) 0.0049(16) 0.0036(16) C2A 0.142(6) 0.185(7) 0.165(7) 0.010(6) 0.001(6) -0.026(6) C2B 0.125(6) 0.149(7) 0.182(6) 0.003(6) 0.019(5) -0.048(5) O3 0.0324(12) 0.0430(14) 0.0314(12) -0.0054(11) 0.0063(11) 0.0095(11) N3 0.0355(16) 0.0356(17) 0.0485(18) 0.0041(14) 0.0070(15) 0.0015(13) C3 0.0318(17) 0.041(2) 0.0348(18) -0.0049(15) 0.0093(15) 0.0043(15) C3A 0.177(7) 0.152(7) 0.151(7) 0.026(6) -0.013(6) -0.018(6) C3B 0.135(5) 0.159(6) 0.166(6) 0.026(5) 0.034(4) -0.044(5) O4 0.0556(18) 0.070(2) 0.0374(15) -0.0059(14) 0.0018(14) 0.0295(16) N4 0.050(4) 0.055(4) 0.076(5) -0.019(4) 0.021(4) 0.003(3) O7 0.046(2) 0.050(3) 0.064(3) -0.010(2) 0.025(2) -0.014(2) O8 0.076(5) 0.066(5) 0.064(4) -0.003(4) 0.012(4) 0.011(4) O9 0.065(4) 0.082(4) 0.096(5) -0.051(4) 0.020(3) -0.024(3) N4' 0.055(5) 0.063(5) 0.078(6) -0.027(5) 0.028(5) -0.009(5) O7' 0.092(7) 0.074(7) 0.093(7) -0.033(7) 0.041(6) -0.025(6) O8' 0.053(5) 0.059(5) 0.081(6) -0.020(5) 0.027(5) -0.001(4) O9' 0.057(5) 0.080(7) 0.090(7) -0.034(6) 0.009(5) -0.004(5) C4 0.0403(19) 0.039(2) 0.0375(19) -0.0052(16) 0.0097(16) 0.0050(16) C4A 0.192(6) 0.166(6) 0.182(6) 0.005(5) 0.001(5) -0.022(5) C4B 0.143(6) 0.148(6) 0.148(6) 0.022(5) 0.018(5) -0.050(5) O5 0.0504(16) 0.0471(16) 0.0420(15) 0.0055(12) 0.0112(13) 0.0138(13) N5 0.072(3) 0.075(3) 0.088(3) 0.021(3) 0.045(3) 0.026(2) C5 0.049(2) 0.040(2) 0.044(2) 0.0045(16) 0.0118(18) 0.0108(17) O6 0.073(2) 0.101(3) 0.064(2) 0.0221(19) 0.028(2) 0.047(2) C6 0.055(2) 0.042(2) 0.049(2) -0.0026(18) 0.021(2) 0.0132(18) C7 0.054(2) 0.050(2) 0.048(2) -0.0114(19) 0.020(2) 0.0000(19) C8 0.051(2) 0.045(2) 0.046(2) -0.0105(17) 0.0189(19) -0.0045(18) C9 0.051(2) 0.057(3) 0.054(2) -0.011(2) 0.024(2) -0.002(2) O10 0.061(2) 0.069(2) 0.076(2) 0.0222(18) 0.0323(19) 0.0099(17) C10 0.044(2) 0.068(3) 0.057(3) -0.013(2) 0.013(2) -0.003(2) O11 0.080(3) 0.090(3) 0.138(4) 0.007(3) 0.056(3) -0.007(2) C11 0.047(2) 0.060(3) 0.051(2) -0.010(2) 0.013(2) 0.001(2) O12 0.134(4) 0.121(4) 0.072(3) 0.032(3) 0.034(3) 0.049(3) C12 0.047(2) 0.045(2) 0.050(2) -0.0133(18) 0.0193(19) -0.0054(18) C13 0.051(2) 0.042(2) 0.042(2) -0.0094(17) 0.0123(18) -0.0030(18) C14 0.048(2) 0.064(3) 0.046(2) -0.0175(19) 0.0149(19) -0.008(2) C15 0.041(2) 0.063(3) 0.051(2) -0.018(2) 0.0116(19) -0.0063(19) C16 0.051(2) 0.050(2) 0.048(2) -0.0111(19) 0.020(2) -0.0037(19) C17 0.0330(18) 0.045(2) 0.0329(18) -0.0042(16) 0.0073(16) 0.0018(16) C18 0.0333(17) 0.0381(19) 0.0308(17) -0.0024(14) 0.0056(15) 0.0071(15) C19 0.0365(19) 0.047(2) 0.046(2) -0.0012(17) 0.0121(18) -0.0006(17) C20 0.047(2) 0.039(2) 0.054(2) -0.0109(18) 0.0130(19) -0.0047(17) C21 0.048(2) 0.036(2) 0.053(2) -0.0072(17) 0.0214(19) 0.0038(17) C22 0.0372(18) 0.0353(19) 0.0387(18) -0.0014(15) 0.0107(16) 0.0030(15) C23 0.0336(17) 0.0357(19) 0.0322(17) -0.0014(14) 0.0086(15) 0.0051(14) C24 0.043(2) 0.037(2) 0.053(2) -0.0083(18) 0.0196(19) 0.0028(17) C25 0.050(2) 0.040(2) 0.060(2) -0.0085(19) 0.023(2) -0.0058(18) C26 0.043(2) 0.041(2) 0.043(2) -0.0030(16) 0.0168(18) 0.0082(17) C27 0.058(2) 0.048(2) 0.049(2) 0.0041(19) 0.015(2) 0.018(2) C28 0.043(2) 0.039(2) 0.046(2) 0.0025(17) 0.0063(18) 0.0060(17) C29 0.055(3) 0.046(2) 0.060(3) -0.004(2) 0.006(2) -0.002(2) C30 0.056(3) 0.059(3) 0.060(3) -0.014(2) -0.006(2) -0.008(2) C31 0.048(2) 0.056(3) 0.047(2) -0.004(2) -0.008(2) -0.005(2) C32 0.0360(19) 0.045(2) 0.0369(19) 0.0012(16) 0.0026(16) -0.0039(16) C33 0.0358(19) 0.041(2) 0.040(2) 0.0005(16) 0.0029(16) -0.0004(16) C34 0.040(2) 0.047(2) 0.041(2) -0.0013(17) -0.0025(17) 0.0052(17) C35 0.039(2) 0.044(2) 0.044(2) -0.0041(17) -0.0005(17) 0.0007(17) C36 0.0369(19) 0.048(2) 0.041(2) 0.0097(18) 0.0041(17) 0.0035(17) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0041 0.0020 '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' N N 0.0079 0.0040 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0133 0.0072 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.2977 1.4315 '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 O7 Cu01 N1 92.92(17) . . ? O8' Cu01 N1 92.0(4) . . ? N1 Cu01 N2 178.31(14) . 4_566 ? O7 Cu01 N3 154.82(18) . 2_545 ? O8' Cu01 N3 95.9(4) . 2_545 ? N1 Cu01 N3 86.24(14) . 2_545 ? N2 Cu01 N3 93.72(13) 4_566 2_545 ? O7 Cu01 O10 113.17(18) . . ? O8' Cu01 O10 170.2(4) . . ? N1 Cu01 O10 94.44(14) . . ? N2 Cu01 O10 83.87(13) 4_566 . ? N3 Cu01 O10 91.97(13) 2_545 . ? C7 O1 C8 118.1(3) . . ? C1A O1A C4A 115.0(12) . . ? C1B O1B C4B 109.8(7) . . ? C1C O1C C4C 106.9(9) . . ? C3C O2C C2C 106.1(13) . . ? O1C C1C C2C 111.4(16) . . ? O1C C1C H1CA 109.4 . . ? C2C C1C H1CA 109.4 . . ? O1C C1C H1CB 109.4 . . ? C2C C1C H1CB 109.4 . . ? H1CA C1C H1CB 108.0 . . ? O2C C2C C1C 119.7(14) . . ? O2C C2C H2CA 107.4 . . ? C1C C2C H2CA 107.4 . . ? O2C C2C H2CB 107.4 . . ? C1C C2C H2CB 107.4 . . ? H2CA C2C H2CB 106.9 . . ? O2C C3C C4C 117.6(17) . . ? O2C C3C H3CA 107.9 . . ? C4C C3C H3CA 107.9 . . ? O2C C3C H3CB 107.9 . . ? C4C C3C H3CB 107.9 . . ? H3CA C3C H3CB 107.2 . . ? O1C C4C C3C 114.0(17) . . ? O1C C4C H4CA 108.8 . . ? C3C C4C H4CA 108.8 . . ? O1C C4C H4CB 108.8 . . ? C3C C4C H4CB 108.8 . . ? H4CA C4C H4CB 107.7 . . ? C8C O3C C5C 111.8(10) . . ? C6C O4C C7C 107.5(9) . . ? O3C C5C C6C 110.9(13) . . ? O3C C5C H5CA 109.5 . . ? C6C C5C H5CA 109.5 . . ? O3C C5C H5CB 109.5 . . ? C6C C5C H5CB 109.5 . . ? H5CA C5C H5CB 108.0 . . ? O4C C6C C5C 117.4(12) . . ? O4C C6C H6C1 108.0 . . ? C5C C6C H6C1 108.0 . . ? O4C C6C H6C2 108.0 . . ? C5C C6C H6C2 108.0 . . ? H6C1 C6C H6C2 107.2 . . ? O4C C7C C8C 110.6(15) . . ? O4C C7C H7C1 109.5 . . ? C8C C7C H7C1 109.5 . . ? O4C C7C H7C2 109.5 . . ? C8C C7C H7C2 109.5 . . ? H7C1 C7C H7C2 108.1 . . ? O3C C8C C7C 96.0(14) . . ? O3C C8C H8C1 112.6 . . ? C7C C8C H8C1 112.6 . . ? O3C C8C H8C2 112.6 . . ? C7C C8C H8C2 112.6 . . ? H8C1 C8C H8C2 110.1 . . ? C2D O1D C1D 106.6(14) 3_656 . ? C2D C1D O1D 98(2) . . ? C2D C1D H1DA 112.2 . . ? O1D C1D H1DA 112.2 . . ? C2D C1D H1DB 112.2 . . ? O1D C1D H1DB 112.2 . . ? H1DA C1D H1DB 109.8 . . ? O1D C2D C1D 114.9(16) 3_656 . ? O1D C2D H2DA 108.5 3_656 . ? C1D C2D H2DA 108.5 . . ? O1D C2D H2DB 108.5 3_656 . ? C1D C2D H2DB 108.5 . . ? H2DA C2D H2DB 107.5 . . ? O2D C3D C4D 110(2) . . ? O2D C3D H3DA 109.6 . . ? C4D C3D H3DA 109.6 . . ? O2D C3D H3DB 109.6 . . ? C4D C3D H3DB 109.6 . . ? H3DA C3D H3DB 108.1 . . ? O2D C4D C3D 96(2) 3_656 . ? O2D C4D H4DA 112.5 3_656 . ? C3D C4D H4DA 112.5 . . ? O2D C4D H4DB 112.5 3_656 . ? C3D C4D H4DB 112.5 . . ? H4DA C4D H4DB 110.0 . . ? O1E C1E C2E 109.3(10) . . ? O1E C1E H1EA 109.8 . . ? C2E C1E H1EA 109.8 . . ? O1E C1E H1EB 109.8 . . ? C2E C1E H1EB 109.8 . . ? H1EA C1E H1EB 108.3 . . ? O1E C2E C1E 109.2(10) 3_665 . ? O1E C2E H2EA 109.8 3_665 . ? C1E C2E H2EA 109.8 . . ? O1E C2E H2EB 109.8 3_665 . ? C1E C2E H2EB 109.8 . . ? H2EA C2E H2EB 108.3 . . ? O2E C3E C4E 105.1(11) 3_665 . ? O2E C3E H3EA 110.7 3_665 . ? C4E C3E H3EA 110.7 . . ? O2E C3E H3EB 110.7 3_665 . ? C4E C3E H3EB 110.7 . . ? H3EA C3E H3EB 108.8 . . ? O2E C4E C3E 109.8(9) . . ? O2E C4E H4EA 109.7 . . ? C3E C4E H4EA 109.7 . . ? O2E C4E H4EB 109.7 . . ? C3E C4E H4EB 109.7 . . ? H4EA C4E H4EB 108.2 . . ? C16 N1 C15 117.7(4) . . ? C16 N1 Cu01 124.3(3) . . ? C15 N1 Cu01 117.9(3) . . ? C6 C1 C2 120.1(4) . . ? C6 C1 C7 118.3(4) . . ? C2 C1 C7 121.6(4) . . ? O1A C1A C2A 115.9(13) . . ? O1A C1A H1AA 108.3 . . ? C2A C1A H1AA 108.3 . . ? O1A C1A H1AB 108.3 . . ? C2A C1A H1AB 108.3 . . ? H1AA C1A H1AB 107.4 . . ? O1B C1B C2B 116.3(8) . . ? O1B C1B H1B1 108.2 . . ? C2B C1B H1B1 108.2 . . ? O1B C1B H1B2 108.2 . . ? C2B C1B H1B2 108.2 . . ? H1B1 C1B H1B2 107.4 . . ? C3A O2A C2A 106.1(8) . . ? C3B O2B C2B 115.3(9) . . ? C26 N2 C25 117.9(3) . . ? C26 N2 Cu01 119.8(3) . 4_665 ? C25 N2 Cu01 122.1(3) . 4_665 ? C3 C2 C1 119.8(4) . . ? C3 C2 H2 120.1 . . ? C1 C2 H2 120.1 . . ? O2A C2A C1A 111.3(11) . . ? O2A C2A H2AA 109.4 . . ? C1A C2A H2AA 109.4 . . ? O2A C2A H2AB 109.4 . . ? C1A C2A H2AB 109.4 . . ? H2AA C2A H2AB 108.0 . . ? O2B C2B C1B 112.4(9) . . ? O2B C2B H2B1 109.1 . . ? C1B C2B H2B1 109.1 . . ? O2B C2B H2B2 109.1 . . ? C1B C2B H2B2 109.1 . . ? H2B1 C2B H2B2 107.9 . . ? C17 O3 C18 118.1(3) . . ? C36 N3 C35 119.0(3) . . ? C36 N3 Cu01 122.1(3) . 2 ? C35 N3 Cu01 118.9(3) . 2 ? C2 C3 C4 120.0(3) . . ? C2 C3 C17 118.9(3) . . ? C4 C3 C17 121.0(3) . . ? O2A C3A C4A 107.4(12) . . ? O2A C3A H3AA 110.2 . . ? C4A C3A H3AA 110.2 . . ? O2A C3A H3AB 110.2 . . ? C4A C3A H3AB 110.2 . . ? H3AA C3A H3AB 108.5 . . ? O2B C3B C4B 110.5(9) . . ? O2B C3B H3B1 109.5 . . ? C4B C3B H3B1 109.5 . . ? O2B C3B H3B2 109.5 . . ? C4B C3B H3B2 109.5 . . ? H3B1 C3B H3B2 108.1 . . ? O9 N4 O7 117.3(11) . . ? O9 N4 O8 121.4(11) . . ? O7 N4 O8 121.3(12) . . ? N4 O7 Cu01 106.0(7) . . ? O9' N4' O7' 122(2) . . ? O9' N4' O8' 119.8(17) . . ? O7' N4' O8' 118(2) . . ? N4' O8' Cu01 115.9(13) . . ? C5 C4 C3 119.8(3) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? O1A C4A C3A 114.1(12) . . ? O1A C4A H4AA 108.7 . . ? C3A C4A H4AA 108.7 . . ? O1A C4A H4AB 108.7 . . ? C3A C4A H4AB 108.7 . . ? H4AA C4A H4AB 107.6 . . ? C3B C4B O1B 118.2(10) . . ? C3B C4B H4B1 107.8 . . ? O1B C4B H4B1 107.8 . . ? C3B C4B H4B2 107.8 . . ? O1B C4B H4B2 107.8 . . ? H4B1 C4B H4B2 107.1 . . ? C27 O5 C28 115.9(3) . . ? O11 N5 O10 120.4(5) . . ? O11 N5 O12 122.7(5) . . ? O10 N5 O12 116.9(6) . . ? C6 C5 C4 120.0(4) . . ? C6 C5 C27 119.4(4) . . ? C4 C5 C27 120.5(4) . . ? C1 C6 C5 120.1(4) . . ? C1 C6 H6 119.9 . . ? C5 C6 H6 119.9 . . ? O2 C7 O1 124.7(4) . . ? O2 C7 C1 122.6(4) . . ? O1 C7 C1 112.7(4) . . ? C9 C8 O1 118.3(4) . . ? C9 C8 C13 121.6(4) . . ? O1 C8 C13 120.0(4) . . ? C8 C9 C10 120.7(4) . . ? C8 C9 H9 119.7 . . ? C10 C9 H9 119.7 . . ? N5 O10 Cu01 117.1(4) . . ? C11 C10 C9 119.4(4) . . ? C11 C10 H10 120.3 . . ? C9 C10 H10 120.3 . . ? C10 C11 C12 121.4(4) . . ? C10 C11 H11 119.3 . . ? C12 C11 H11 119.3 . . ? C11 C12 C13 119.9(4) . . ? C11 C12 C16 122.7(4) . . ? C13 C12 C16 117.4(4) . . ? C8 C13 C12 117.0(4) . . ? C8 C13 C14 126.2(4) . . ? C12 C13 C14 116.8(4) . . ? C15 C14 C13 121.2(4) . . ? C15 C14 H14 119.4 . . ? C13 C14 H14 119.4 . . ? C14 C15 N1 122.7(4) . . ? C14 C15 H15 118.7 . . ? N1 C15 H15 118.7 . . ? N1 C16 C12 124.1(4) . . ? N1 C16 H16 117.9 . . ? C12 C16 H16 117.9 . . ? O4 C17 O3 123.6(3) . . ? O4 C17 C3 125.7(3) . . ? O3 C17 C3 110.7(3) . . ? C19 C18 C23 122.7(3) . . ? C19 C18 O3 119.3(3) . . ? C23 C18 O3 117.8(3) . . ? C18 C19 C20 119.3(4) . . ? C18 C19 H19 120.4 . . ? C20 C19 H19 120.4 . . ? C21 C20 C19 120.4(4) . . ? C21 C20 H20 119.8 . . ? C19 C20 H20 119.8 . . ? C20 C21 C22 120.1(4) . . ? C20 C21 H21 120.0 . . ? C22 C21 H21 120.0 . . ? C21 C22 C26 122.8(3) . . ? C21 C22 C23 119.8(3) . . ? C26 C22 C23 117.4(3) . . ? C18 C23 C24 125.1(3) . . ? C18 C23 C22 117.7(3) . . ? C24 C23 C22 117.1(3) . . ? C25 C24 C23 120.4(4) . . ? C25 C24 H24 119.8 . . ? C23 C24 H24 119.8 . . ? C24 C25 N2 122.8(4) . . ? C24 C25 H25 118.6 . . ? N2 C25 H25 118.6 . . ? N2 C26 C22 124.3(3) . . ? N2 C26 H26 117.8 . . ? C22 C26 H26 117.8 . . ? O6 C27 O5 122.8(4) . . ? O6 C27 C5 125.4(4) . . ? O5 C27 C5 111.8(4) . . ? C29 C28 O5 119.6(4) . . ? C29 C28 C33 121.6(4) . . ? O5 C28 C33 118.7(4) . . ? C28 C29 C30 119.3(4) . . ? C28 C29 H29 120.4 . . ? C30 C29 H29 120.4 . . ? C31 C30 C29 121.8(4) . . ? C31 C30 H30 119.1 . . ? C29 C30 H30 119.1 . . ? C30 C31 C32 119.4(4) . . ? C30 C31 H31 120.3 . . ? C32 C31 H31 120.3 . . ? C31 C32 C33 120.5(4) . . ? C31 C32 C36 122.1(4) . . ? C33 C32 C36 117.3(4) . . ? C32 C33 C34 117.9(4) . . ? C32 C33 C28 117.3(4) . . ? C34 C33 C28 124.8(4) . . ? C35 C34 C33 120.4(4) . . ? C35 C34 H34 119.8 . . ? C33 C34 H34 119.8 . . ? C34 C35 N3 121.9(4) . . ? C34 C35 H35 119.0 . . ? N3 C35 H35 119.0 . . ? N3 C36 C32 123.4(4) . . ? N3 C36 H36 118.3 . . ? C32 C36 H36 118.3 . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Cu01 O7 1.996(5) . ? Cu01 O8' 2.003(14) . ? Cu01 N1 2.016(3) . ? Cu01 N2 2.029(3) 4_566 ? Cu01 N3 2.096(3) 2_545 ? Cu01 O10 2.206(4) . ? O1 C7 1.352(5) . ? O1 C8 1.410(5) . ? O1A C1A 1.252(14) . ? O1A C4A 1.308(14) . ? O1B C1B 1.380(10) . ? O1B C4B 1.422(11) . ? O1C C1C 1.451(10) . ? O1C C4C 1.469(10) . ? O2C C3C 1.432(10) . ? O2C C2C 1.461(10) . ? C1C C2C 1.534(10) . ? C1C H1CA 0.9700 . ? C1C H1CB 0.9700 . ? C2C H2CA 0.9700 . ? C2C H2CB 0.9700 . ? C3C C4C 1.534(10) . ? C3C H3CA 0.9700 . ? C3C H3CB 0.9700 . ? C4C H4CA 0.9700 . ? C4C H4CB 0.9700 . ? O3C C8C 1.422(9) . ? O3C C5C 1.427(9) . ? O4C C6C 1.418(9) . ? O4C C7C 1.471(9) . ? C5C C6C 1.62(3) . ? C5C H5CA 0.9700 . ? C5C H5CB 0.9700 . ? C6C H6C1 0.9700 . ? C6C H6C2 0.9700 . ? C7C C8C 1.486(10) . ? C7C H7C1 0.9700 . ? C7C H7C2 0.9700 . ? C8C H8C1 0.9700 . ? C8C H8C2 0.9700 . ? O1D C2D 1.422(9) 3_656 ? O1D C1D 1.62(3) . ? C1D C2D 1.49(3) . ? C1D H1DA 0.9700 . ? C1D H1DB 0.9700 . ? C2D H2DA 0.9700 . ? C2D H2DB 0.9700 . ? O2D C3D 1.43(3) . ? O2D C4D 1.49(3) 3_656 ? C3D C4D 1.51(5) . ? C3D H3DA 0.9700 . ? C3D H3DB 0.9700 . ? C4D H4DA 0.9700 . ? C4D H4DB 0.9700 . ? O1E C1E 1.442(10) . ? O1E C2E 1.443(10) 3_665 ? C1E C2E 1.518(10) . ? C1E H1EA 0.9700 . ? C1E H1EB 0.9700 . ? C2E H2EA 0.9700 . ? C2E H2EB 0.9700 . ? O2E C4E 1.422(14) . ? O2E C3E 1.468(9) 3_665 ? C3E C4E 1.563(17) . ? C3E H3EA 0.9700 . ? C3E H3EB 0.9700 . ? C4E H4EA 0.9700 . ? C4E H4EB 0.9700 . ? N1 C16 1.317(5) . ? N1 C15 1.385(5) . ? C1 C6 1.379(6) . ? C1 C2 1.387(5) . ? C1 C7 1.491(5) . ? C1A C2A 1.487(15) . ? C1A H1AA 0.9700 . ? C1A H1AB 0.9700 . ? C1B C2B 1.461(8) . ? C1B H1B1 0.9700 . ? C1B H1B2 0.9700 . ? O2 C7 1.214(5) . ? O2A C3A 1.412(13) . ? O2A C2A 1.433(12) . ? O2B C3B 1.349(11) . ? O2B C2B 1.433(12) . ? N2 C26 1.314(5) . ? N2 C25 1.372(5) . ? C2 C3 1.384(5) . ? C2 H2 0.9300 . ? C2A H2AA 0.9700 . ? C2A H2AB 0.9700 . ? C2B H2B1 0.9700 . ? C2B H2B2 0.9700 . ? O3 C17 1.354(4) . ? O3 C18 1.405(4) . ? N3 C36 1.315(5) . ? N3 C35 1.373(5) . ? C3 C4 1.389(5) . ? C3 C17 1.485(5) . ? C3A C4A 1.476(14) . ? C3A H3AA 0.9700 . ? C3A H3AB 0.9700 . ? C3B C4B 1.401(12) . ? C3B H3B1 0.9700 . ? C3B H3B2 0.9700 . ? O4 C17 1.195(5) . ? N4 O9 1.240(14) . ? N4 O7 1.242(12) . ? N4 O8 1.249(15) . ? N4' O9' 1.18(2) . ? N4' O7' 1.210(10) . ? N4' O8' 1.31(3) . ? C4 C5 1.386(5) . ? C4 H4 0.9300 . ? C4A H4AA 0.9700 . ? C4A H4AB 0.9700 . ? C4B H4B1 0.9700 . ? C4B H4B2 0.9700 . ? O5 C27 1.362(5) . ? O5 C28 1.395(5) . ? N5 O11 1.229(6) . ? N5 O10 1.233(6) . ? N5 O12 1.281(6) . ? C5 C6 1.384(6) . ? C5 C27 1.474(6) . ? O6 C27 1.211(5) . ? C6 H6 0.9300 . ? C8 C9 1.346(6) . ? C8 C13 1.412(6) . ? C9 C10 1.410(6) . ? C9 H9 0.9300 . ? C10 C11 1.345(6) . ? C10 H10 0.9300 . ? C11 C12 1.396(6) . ? C11 H11 0.9300 . ? C12 C13 1.420(6) . ? C12 C16 1.424(6) . ? C13 C14 1.425(6) . ? C14 C15 1.337(6) . ? C14 H14 0.9300 . ? C15 H15 0.9300 . ? C16 H16 0.9300 . ? C18 C19 1.350(5) . ? C18 C23 1.396(5) . ? C19 C20 1.421(6) . ? C19 H19 0.9300 . ? C20 C21 1.365(6) . ? C20 H20 0.9300 . ? C21 C22 1.407(5) . ? C21 H21 0.9300 . ? C22 C26 1.408(5) . ? C22 C23 1.423(5) . ? C23 C24 1.415(5) . ? C24 C25 1.350(6) . ? C24 H24 0.9300 . ? C25 H25 0.9300 . ? C26 H26 0.9300 . ? C28 C29 1.350(6) . ? C28 C33 1.417(5) . ? C29 C30 1.418(7) . ? C29 H29 0.9300 . ? C30 C31 1.335(7) . ? C30 H30 0.9300 . ? C31 C32 1.412(6) . ? C31 H31 0.9300 . ? C32 C33 1.413(5) . ? C32 C36 1.417(6) . ? C33 C34 1.414(6) . ? C34 C35 1.355(6) . ? C34 H34 0.9300 . ? C35 H35 0.9300 . ? C36 H36 0.9300 . ?