#------------------------------------------------------------------------------ #$Date: 2024-07-09 01:18:42 +0300 (Tue, 09 Jul 2024) $ #$Revision: 293306 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/20/1572089.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_1572089 loop_ _publ_author_name 'Chen, Zhao-Nian' 'Zhang, Le-Ping' 'Wu, Huai-Li' 'Qi, Qiao-Yan' 'Yan, Meng' 'Tian, Jia' 'Yang, Guanyu' 'Li, Zhan-Ting' 'Yang, Bo' _publ_section_title ; Accurate Construction of Monolayer, Bilayer, Sandwich Bilayer, Four-layer, Multi-layer and Chiral Bilayer 2D Pillararene-Type Supramolecular Networks ; _journal_name_full 'Chemical Science' _journal_paper_doi 10.1039/D4SC03022B _journal_year 2024 _chemical_absolute_configuration ad _chemical_formula_moiety 'C106 H100 Cu2 N4 O16, 2[C3H7NO]' _chemical_formula_sum 'C112 H114 Cu2 N6 O18' _chemical_formula_weight 1959.17 _space_group_crystal_system orthorhombic _space_group_IT_number 18 _space_group_name_Hall 'P 2 2ab' _space_group_name_H-M_alt 'P 21 21 2' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2024-06-18 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _audit_update_record ; 2024-06-25 deposited with the CCDC. 2024-07-04 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 2 _cell_length_a 19.721(5) _cell_length_b 21.191(5) _cell_length_c 13.551(3) _cell_measurement_reflns_used 8991 _cell_measurement_temperature 193.00 _cell_measurement_theta_max 20.09 _cell_measurement_theta_min 2.44 _cell_volume 5663(2) _computing_cell_refinement 'SAINT V8.40B (Bruker, 2019)' _computing_data_collection 'APEX5 V2023.9-2 (Bruker, 2023)' _computing_data_reduction 'SAINT V8.40B (Bruker, 2019)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2019/3 (Sheldrick, 2015)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 193.00 _diffrn_detector CPAD _diffrn_detector_area_resol_mean 7.41 _diffrn_detector_type 'Bruker PHOTON II' _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker D8 VENTURE TXS PHOTON II' _diffrn_measurement_method '\w and \f shutterless scans' _diffrn_measurement_specimen_support 'nylon loop' _diffrn_radiation_monochromator 'Helios Multi-layer Optic' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.1624 _diffrn_reflns_av_unetI/netI 0.1199 _diffrn_reflns_Laue_measured_fraction_full 0.997 _diffrn_reflns_Laue_measured_fraction_max 0.997 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_k_max 25 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 65274 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 25.348 _diffrn_reflns_theta_min 1.922 _diffrn_source TXS _diffrn_source_current 1.6 _diffrn_source_power 0.08 _diffrn_source_type 'Rotaing Anode' _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 0.439 _exptl_absorpt_correction_T_max 0.7454 _exptl_absorpt_correction_T_min 0.4546 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1731 before and 0.0967 after correction. The Ratio of minimum to maximum transmission is 0.6099. The \l/2 correction factor is Not present. ; _exptl_crystal_colour blue _exptl_crystal_colour_primary blue _exptl_crystal_density_diffrn 1.149 _exptl_crystal_description block _exptl_crystal_F_000 2060 _exptl_crystal_size_max 0.14 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.09 _refine_diff_density_max 0.376 _refine_diff_density_min -0.421 _refine_diff_density_rms 0.069 _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.17(3) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 0.965 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 625 _refine_ls_number_reflns 10366 _refine_ls_number_restraints 172 _refine_ls_restrained_S_all 0.978 _refine_ls_R_factor_all 0.1488 _refine_ls_R_factor_gt 0.0901 _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^)+(0.1810P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.2368 _refine_ls_wR_factor_ref 0.2844 _reflns_Friedel_coverage 0.812 _reflns_Friedel_fraction_full 0.999 _reflns_Friedel_fraction_max 0.999 _reflns_number_gt 5555 _reflns_number_total 10366 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03022b2.cif _cod_data_source_block a _cod_depositor_comments ; The following automatic conversions were performed: data item '_diffrn_radiation_probe' value 'X-ray' was changed to 'x-ray' in accordance with the /home/data/users/saulius/crontab/automatic-downloads/rss-feeds/RSC/lib/dictionaries/cif_core.dic dictionary named 'cif_core.dic' version 2.4.2 last updated on 2011-04-26. Automatic conversion script Id: cif_fix_values 8170 2020-07-09 18:12:32Z antanas ; _cod_database_code 1572089 _shelx_shelxl_version_number 2019/3 _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_max 0.962 _shelx_estimated_absorpt_t_min 0.941 _olex2_refinement_description ; 1. Twinned data refinement Scales: 0.83(4) 0.17(4) 2. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups 3. Restrained distances C41-C40 1.5 with sigma of 0.01 C42-C35 1.5 with sigma of 0.01 O1A-C1A = O2A-C1A = O1-C1 = O2-C1 = O4A-C2A = O3A-C2A = O3-C2 = O4-C2 1.25 with sigma of 0.01 C40-C33 = O6-C41 2.4 with sigma of 0.01 O1A-O2A = O1-O2 = O4A-O3A = O3-O4 2.2 with sigma of 0.01 4. Uiso/Uaniso restraints and constraints O5 \\sim C38 \\sim C39 \\sim C36: within 2A with sigma of 0.007 and sigma for terminal atoms of 0.015 within 2A C40 \\sim C41: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A O1 \\sim O2 \\sim C1 \\sim O1A \\sim O2A \\sim C1A \\sim Cu1: within 2A with sigma of 0.005 and sigma for terminal atoms of 0.01 within 2A C41 \\sim C40 \\sim O6: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A O3A \\sim C2A \\sim O4A \\sim O3 \\sim C2 \\sim O4: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A C26 \\sim O7: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A Uanis(C31) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 5. Same fragment restrains {O3A, O4A, C2A} sigma for 1-2: 0.02, 1-3: 0.04 as in {O3, O4, C2} {O1A, O2A, C1A} sigma for 1-2: 0.02, 1-3: 0.04 as in {O1, O2, C1} 6. Others Sof(O3A)=Sof(O4A)=Sof(C2A)=Sof(H2A)=1-FVAR(1) Sof(O3)=Sof(O4)=Sof(C2)=Sof(H2)=FVAR(1) Sof(O1A)=Sof(O2A)=Sof(C1A)=Sof(H1A)=1-FVAR(2) Sof(O1)=Sof(O2)=Sof(C1)=Sof(H1)=FVAR(2) 7.a Riding coordinates: C41(H41A,H41B,H41C) 7.b Secondary CH2 refined with riding coordinates: C20(H20A,H20B), C27(H27A,H27B), C29(H29A,H29B), C31(H31A,H31B), C38(H38A, H38B), C40(H40A,H40B), C42(H42A,H42B) 7.c Aromatic/amide H refined with riding coordinates: C1(H1), C1A(H1A), C2(H2), C2A(H2A), C3(H3), C4(H4), C6(H6), C7(H7), C9(H9), C10(H10), C12(H12), C13(H13), C16(H16), C19(H19), C22(H22), C25(H25), C34(H34), C37(H37), C44(H44), C45(H45), C47(H47), C48(H48), C49(H49), C50(H50), C52(H52), C53(H53) 7.d Fitted hexagon refined as free rotating group: C34(C33,C32,C37,C36,C35) 7.e Idealised Me refined as rotating group: C28(H28A,H28B,H28C), C30(H30A,H30B,H30C), C39(H39A,H39B,H39C) ; _smtbx_masks_special_details ; A solvent mask was calculated and 171 electrons were found in a volume of 1599\%A^3^ in 1 void per unit cell. This is consistent with the presence of 2[C3H7NO] per formula unit which account for 160 electrons per unit cell. ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL a_a.res in P2(1)2(1)2 a.res created by SHELXL-2019/3 at 21:43:06 on 18-Jun-2024 REM Old TITL A in P222 REM SHELXT solution in P2(1)2(1)2: R1 0.365, Rweak 0.185, Alpha 0.051 REM 2.600 for 23 systematic absences, Orientation a'=b, b'=c, c'=a REM Flack x = 0.201 ( 0.012 ) from 1979 Parsons' quotients REM Formula found by SHELXT: C42 N14 O2 Cu CELL 0.71073 19.7211 21.1909 13.5512 90 90 90 ZERR 2 0.0048 0.0049 0.0034 0 0 0 LATT -1 SYMM -X,-Y,+Z SYMM 0.5-X,0.5+Y,-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H Cu N O UNIT 224 228 4 12 36 SIMU 0.007 0.015 2 O5 C38 C39 C36 SIMU 0.005 0.01 2 C40 C41 DANG 2.4 0.01 C40 C33 O6 C41 DFIX 1.5 0.01 C41 C40 SIMU 0.005 0.01 2 O1 O2 C1 O1A O2A C1A Cu1 SIMU 0.01 0.02 2 C41 C40 O6 DFIX 1.5 0.01 C42 C35 SIMU 0.01 0.02 2 O3A C2A O4A O3 C2 O4 SIMU 0.01 0.02 2 C26 O7 ISOR 0.01 0.02 C31 DFIX 1.25 0.01 O1A C1A O2A C1A O1 C1 O2 C1 O4A C2A O3A C2A O3 C2 O4 C2 DANG 2.2 0.01 O1A O2A O1 O2 O4A O3A O3 O4 L.S. 10 0 0 PLAN 23 SIZE 0.09 0.11 0.14 TEMP -80.15 CONF FREE Cu1 C1 BOND list 4 MORE -1 BOND $H ABIN fmap 2 53 acta SHEL 999 0.83 TWIN -1 0 0 0 -1 0 0 0 -1 2 OMIT 0 3 2 OMIT 2 0 1 REM REM REM WGHT 0.181000 BASF 0.17150 FVAR 0.49228 0.59364 0.60313 CU1 3 0.269237 0.598343 0.105730 11.00000 0.06392 0.13746 = 0.11954 -0.00138 -0.05321 0.00079 SAME 0.02 0.04 O1A O2A C1A PART 1 O1 5 0.231189 0.499671 0.204304 31.00000 0.09350 0.21669 = 0.19572 -0.00876 -0.05847 0.01168 O2 5 0.291445 0.508891 0.066559 31.00000 0.08127 0.20030 = 0.18087 -0.02912 -0.06490 0.01212 C1 1 0.249533 0.480178 0.120523 31.00000 0.08553 0.20678 = 0.18575 -0.02584 -0.06530 0.01243 AFIX 43 H1 2 0.230745 0.441782 0.096816 31.00000 -1.20000 AFIX 0 PART 2 O1A 5 0.216429 0.554976 0.223395 -31.00000 0.06886 0.20972 = 0.18138 -0.02959 -0.06751 0.00617 O2A 5 0.271384 0.478994 0.147641 -31.00000 0.09394 0.21215 = 0.18908 -0.02178 -0.05921 0.01466 C1A 1 0.217134 0.500414 0.184872 -31.00000 0.08047 0.21070 = 0.18765 -0.02234 -0.06421 0.01124 AFIX 43 H1A 2 0.176999 0.475628 0.183943 -31.00000 -1.20000 AFIX 0 SAME 0.02 0.04 O3A O4A C2A PART 1 O3 5 0.262155 0.706720 0.114890 21.00000 0.11939 0.21057 = 0.15613 -0.02270 -0.09940 0.04413 O4 5 0.322273 0.661479 -0.002223 21.00000 0.12874 0.16172 = 0.12285 -0.00602 -0.09737 0.00826 C2 1 0.294797 0.708756 0.036163 21.00000 0.13330 0.19025 = 0.13862 -0.01031 -0.08832 0.02583 AFIX 43 H2 2 0.299047 0.748255 0.003584 21.00000 -1.20000 AFIX 0 PART 2 O3A 5 0.220145 0.659116 0.197758 -21.00000 0.10673 0.21056 = 0.16432 -0.02580 -0.09479 0.05320 O4A 5 0.242346 0.739404 0.098853 -21.00000 0.14635 0.23053 = 0.16105 -0.00506 -0.08159 0.02818 C2A 1 0.215823 0.715055 0.173164 -21.00000 0.12085 0.21604 = 0.16477 -0.03051 -0.09095 0.03819 AFIX 43 H2A 2 0.189933 0.741999 0.214633 -21.00000 -1.20000 AFIX 0 PART 0 O5 5 0.886524 0.293021 0.396223 11.00000 0.20186 0.20625 = 0.17776 -0.03470 -0.05347 0.06449 O6 5 0.730702 0.397495 0.696815 11.00000 0.11754 0.16602 = 0.21940 -0.02341 -0.01851 0.04789 O7 5 0.863880 0.716643 0.478593 11.00000 0.14480 0.12154 = 0.17618 0.00814 -0.05593 -0.00753 O8 5 1.054650 0.755290 0.769008 11.00000 0.07219 0.10115 = 0.23060 -0.00357 -0.05239 -0.00016 N1 4 0.353608 0.598628 0.188125 11.00000 0.05343 0.10985 = 0.10468 0.00066 -0.02433 0.00837 N2 4 1.187629 0.594281 1.018326 11.00000 0.05679 0.14167 = 0.10154 -0.00830 -0.03116 0.01144 C3 1 0.354310 0.612837 0.283172 11.00000 0.05251 0.09754 = 0.09573 -0.00079 -0.02841 0.01206 AFIX 43 H3 2 0.312974 0.626596 0.312031 11.00000 -1.20000 AFIX 0 C4 1 0.409325 0.609278 0.342366 11.00000 0.04349 0.08817 = 0.09055 0.00924 -0.02399 -0.00942 AFIX 43 H4 2 0.406261 0.619861 0.410343 11.00000 -1.20000 AFIX 0 C5 1 0.471645 0.589416 0.300769 11.00000 0.04744 0.06806 = 0.09571 0.01331 -0.03246 -0.01274 C6 1 0.470479 0.576580 0.203544 11.00000 0.05841 0.10590 = 0.09719 -0.00079 -0.02467 0.00001 AFIX 43 H6 2 0.511121 0.564081 0.171384 11.00000 -1.20000 AFIX 0 C7 1 0.412322 0.581171 0.150655 11.00000 0.08479 0.14983 = 0.08203 0.00091 -0.02940 0.01081 AFIX 43 H7 2 0.414021 0.571180 0.082358 11.00000 -1.20000 AFIX 0 C8 1 0.534007 0.583405 0.362949 11.00000 0.04349 0.06673 = 0.08538 0.00346 -0.02873 -0.00659 C9 1 0.531456 0.582073 0.463199 11.00000 0.04116 0.12764 = 0.08422 0.02907 -0.02013 -0.00823 AFIX 43 H9 2 0.488456 0.583142 0.494757 11.00000 -1.20000 AFIX 0 C10 1 0.589097 0.579224 0.520707 11.00000 0.04993 0.11369 = 0.08490 0.00268 -0.02273 -0.00599 AFIX 43 H10 2 0.585396 0.580129 0.590590 11.00000 -1.20000 AFIX 0 C11 1 0.653284 0.574987 0.476134 11.00000 0.04435 0.07541 = 0.11110 -0.00354 -0.03576 0.00404 C12 1 0.656193 0.575259 0.374400 11.00000 0.04317 0.10226 = 0.10494 -0.01592 -0.02582 0.01650 AFIX 43 H12 2 0.698894 0.573296 0.342096 11.00000 -1.20000 AFIX 0 C13 1 0.597354 0.578370 0.319225 11.00000 0.05042 0.09746 = 0.08304 -0.01171 -0.02000 0.00235 AFIX 43 H13 2 0.600391 0.577020 0.249292 11.00000 -1.20000 AFIX 0 C14 1 0.715610 0.576709 0.537838 11.00000 0.04771 0.06888 = 0.13248 -0.01651 -0.04791 0.01383 C15 1 0.751846 0.520603 0.557093 11.00000 0.08361 0.06467 = 0.15426 -0.01295 -0.07373 0.00916 C16 1 0.809399 0.526371 0.613162 11.00000 0.07251 0.05331 = 0.15549 -0.00298 -0.06434 0.00458 AFIX 43 H16 2 0.834541 0.489125 0.626714 11.00000 -1.20000 AFIX 0 C17 1 0.833265 0.582299 0.651142 11.00000 0.05066 0.07814 = 0.11645 0.00216 -0.04460 0.00109 C18 1 0.797794 0.638240 0.633081 11.00000 0.04119 0.07679 = 0.11961 -0.00801 -0.03354 0.00123 C19 1 0.736938 0.631759 0.574411 11.00000 0.05592 0.06617 = 0.12211 -0.01003 -0.04160 0.01097 AFIX 43 H19 2 0.710838 0.668485 0.561233 11.00000 -1.20000 AFIX 0 C20 1 0.819500 0.701611 0.671205 11.00000 0.04491 0.06735 = 0.12639 -0.01146 -0.01787 0.00611 AFIX 23 H20A 2 0.789479 0.734229 0.642452 11.00000 -1.20000 H20B 2 0.812998 0.702359 0.743636 11.00000 -1.20000 AFIX 0 C21 1 0.891615 0.718800 0.648945 11.00000 0.06965 0.06608 = 0.12333 -0.01806 -0.01644 -0.00088 C22 1 0.938192 0.733994 0.720379 11.00000 0.05128 0.05780 = 0.16095 -0.00620 -0.03946 -0.00092 AFIX 43 H22 2 0.925092 0.737232 0.787651 11.00000 -1.20000 AFIX 0 C23 1 1.006058 0.744702 0.691526 11.00000 0.06053 0.07204 = 0.15637 0.00104 -0.03100 0.00194 C24 1 1.025137 0.747232 0.597597 11.00000 0.08182 0.04397 = 0.21450 0.00657 0.00544 -0.00519 C25 1 0.981480 0.737432 0.525351 11.00000 0.09403 0.07306 = 0.13839 0.01062 -0.00191 -0.00495 AFIX 43 H25 2 0.994878 0.739763 0.458111 11.00000 -1.20000 AFIX 0 C26 1 0.911605 0.722832 0.553322 11.00000 0.10817 0.06868 = 0.16950 0.00037 -0.05810 -0.00134 C27 1 0.876361 0.683912 0.391619 11.00000 0.22197 0.21018 = 0.19035 -0.05560 0.01064 0.01654 AFIX 23 H27A 2 0.896297 0.642386 0.408313 11.00000 -1.20000 H27B 2 0.910382 0.707546 0.352630 11.00000 -1.20000 AFIX 0 C28 1 0.816149 0.673703 0.330147 11.00000 0.23998 0.28623 = 0.24811 -0.09050 -0.09082 -0.03695 AFIX 137 H28A 2 0.829562 0.653513 0.268082 11.00000 -1.50000 H28B 2 0.794548 0.714358 0.316008 11.00000 -1.50000 H28C 2 0.784101 0.646416 0.365274 11.00000 -1.50000 AFIX 0 C29 1 1.033162 0.757297 0.870444 11.00000 0.12078 0.11032 = 0.15858 -0.01383 -0.02828 -0.02120 AFIX 23 H29A 2 1.014289 0.716070 0.891097 11.00000 -1.20000 H29B 2 0.998245 0.790265 0.880309 11.00000 -1.20000 AFIX 0 C30 1 1.095388 0.772315 0.927020 11.00000 0.17638 0.16766 = 0.28186 -0.03492 -0.14265 -0.01168 AFIX 137 H30A 2 1.120844 0.733415 0.939557 11.00000 -1.50000 H30B 2 1.082906 0.791866 0.989989 11.00000 -1.50000 H30C 2 1.123575 0.801597 0.888936 11.00000 -1.50000 AFIX 0 C31 1 0.729200 0.459867 0.508737 11.00000 0.10020 0.09410 = 0.17860 -0.01107 -0.07313 0.00618 AFIX 23 H31A 2 0.729492 0.466402 0.436401 11.00000 -1.20000 H31B 2 0.681619 0.451903 0.528420 11.00000 -1.20000 AFIX 66 C34 1 0.813539 0.317900 0.634943 11.00000 0.06246 0.10390 = 0.20235 0.01281 -0.01790 0.01669 AFIX 43 H34 2 0.814608 0.296903 0.696864 11.00000 -1.20000 AFIX 65 C33 1 0.771642 0.369949 0.621569 11.00000 0.07232 0.11513 = 0.17365 -0.01563 -0.01505 0.01408 C32 1 0.770079 0.400671 0.530970 11.00000 0.08113 0.08231 = 0.18636 0.00343 -0.07513 0.00083 C37 1 0.810412 0.379344 0.453745 11.00000 0.10589 0.13730 = 0.15723 0.04747 -0.03136 -0.02473 AFIX 43 H37 2 0.809343 0.400341 0.391825 11.00000 -1.20000 AFIX 65 C36 1 0.852308 0.327294 0.467118 11.00000 0.18606 0.18625 = 0.16764 -0.03375 -0.07015 0.04747 C35 1 0.853873 0.296572 0.557716 11.00000 0.08609 0.08359 = 0.18998 -0.00968 -0.04238 -0.00431 AFIX 0 C38 1 0.868588 0.309674 0.304657 11.00000 0.22221 0.22187 = 0.19060 -0.02589 -0.03909 0.06118 AFIX 23 H38A 2 0.888415 0.351033 0.286726 11.00000 -1.20000 H38B 2 0.818645 0.312178 0.298391 11.00000 -1.20000 AFIX 0 C39 1 0.898655 0.254507 0.236184 11.00000 0.26342 0.25629 = 0.22919 -0.02124 -0.04414 0.06038 AFIX 137 H39A 2 0.936993 0.270849 0.197921 11.00000 -1.50000 H39B 2 0.863300 0.239534 0.191081 11.00000 -1.50000 H39C 2 0.914020 0.219477 0.277766 11.00000 -1.50000 AFIX 0 C40 1 0.677235 0.349593 0.725487 11.00000 0.18167 0.19980 = 0.26743 -0.02211 -0.02089 0.04332 AFIX 23 H40A 2 0.638656 0.351711 0.678860 11.00000 -1.20000 H40B 2 0.696554 0.306506 0.722846 11.00000 -1.20000 AFIX 0 C41 1 0.653617 0.363710 0.826806 11.00000 0.22745 0.21887 = 0.29460 -0.03320 -0.01062 0.05161 AFIX 3 H41A 2 0.685617 0.345830 0.874546 11.00000 -1.50000 H41B 2 0.608487 0.345680 0.837826 11.00000 -1.50000 H41C 2 0.651637 0.409610 0.835146 11.00000 -1.50000 AFIX 0 C42 1 0.898130 0.237835 0.569038 11.00000 0.07518 0.07483 = 0.27228 -0.01382 -0.02432 0.00541 AFIX 23 H42A 2 0.897507 0.214015 0.506198 11.00000 -1.20000 H42B 2 0.878205 0.210438 0.620622 11.00000 -1.20000 AFIX 0 C43 1 0.895140 0.582473 0.715392 11.00000 0.05142 0.06229 = 0.12025 -0.01082 -0.04564 -0.00171 C44 1 0.959051 0.581251 0.674110 11.00000 0.07259 0.06887 = 0.11876 -0.00958 -0.05385 0.00226 AFIX 43 H44 2 0.963058 0.579688 0.604291 11.00000 -1.20000 AFIX 0 C45 1 1.017801 0.582218 0.730674 11.00000 0.06041 0.06023 = 0.11810 -0.00861 -0.04918 0.00661 AFIX 43 H45 2 1.061317 0.581987 0.700610 11.00000 -1.20000 AFIX 0 C46 1 1.010593 0.583569 0.835502 11.00000 0.05135 0.08576 = 0.10811 -0.00348 -0.04246 0.00345 C47 1 0.947142 0.583353 0.875974 11.00000 0.06932 0.11331 = 0.10512 0.00215 -0.03574 0.00312 AFIX 43 H47 2 0.941963 0.583407 0.945672 11.00000 -1.20000 AFIX 0 C48 1 0.889895 0.583052 0.815419 11.00000 0.04565 0.12681 = 0.12314 -0.01061 -0.03376 0.00490 AFIX 43 H48 2 0.846170 0.583258 0.844836 11.00000 -1.20000 AFIX 0 C49 1 1.191274 0.596286 0.923280 11.00000 0.05521 0.21329 = 0.10696 -0.00240 -0.03060 0.00156 AFIX 43 H49 2 1.235141 0.600358 0.895020 11.00000 -1.20000 AFIX 0 C50 1 1.137298 0.593048 0.859380 11.00000 0.06409 0.22776 = 0.11126 -0.01526 -0.03514 0.00629 AFIX 43 H50 2 1.144009 0.593522 0.789963 11.00000 -1.20000 AFIX 0 C51 1 1.071862 0.589014 0.899903 11.00000 0.04986 0.09323 = 0.10326 -0.00765 -0.03160 0.01610 C52 1 1.067665 0.585832 1.000734 11.00000 0.05430 0.19374 = 0.12005 0.00893 -0.03973 -0.00076 AFIX 43 H52 2 1.024720 0.581710 1.031834 11.00000 -1.20000 AFIX 0 C53 1 1.126232 0.588638 1.057345 11.00000 0.09600 0.21322 = 0.10577 -0.01733 -0.04987 0.01485 AFIX 43 H53 2 1.122177 0.586421 1.127114 11.00000 -1.20000 AFIX 0 HKLF 4 REM a_a.res in P2(1)2(1)2 REM wR2 = 0.2844, GooF = S = 0.965, Restrained GooF = 0.978 for all data REM R1 = 0.0901 for 5555 Fo > 4sig(Fo) and 0.1488 for all 10366 data REM 625 parameters refined using 172 restraints END WGHT 0.1821 0.0000 REM Highest difference peak 0.376, deepest hole -0.421, 1-sigma level 0.069 Q1 1 0.2600 0.4162 0.1055 11.00000 0.05 0.38 Q2 1 0.3233 0.5346 -0.0106 11.00000 0.05 0.37 Q3 1 0.6142 0.3646 0.6519 11.00000 0.05 0.36 Q4 1 0.3022 0.5919 0.0427 11.00000 0.05 0.33 Q5 1 0.8194 0.2573 0.6853 11.00000 0.05 0.33 Q6 1 0.9925 0.7000 0.4040 11.00000 0.05 0.31 Q7 1 0.7009 0.4548 0.6012 11.00000 0.05 0.31 Q8 1 0.8014 0.2633 0.7725 11.00000 0.05 0.30 Q9 1 0.3353 0.7572 -0.0042 11.00000 0.05 0.29 Q10 1 0.8433 0.3376 0.4803 11.00000 0.05 0.28 Q11 1 0.7905 0.2401 0.6644 11.00000 0.05 0.28 Q12 1 0.3022 0.6757 0.3165 11.00000 0.05 0.26 Q13 1 1.1057 0.6244 0.9016 11.00000 0.05 0.25 Q14 1 1.0000 0.5000 0.8964 10.50000 0.05 0.25 Q15 1 0.8057 0.3958 0.4897 11.00000 0.05 0.24 Q16 1 0.7864 0.4438 0.4212 11.00000 0.05 0.24 Q17 1 0.3303 0.5371 0.2406 11.00000 0.05 0.24 Q18 1 0.3773 0.6792 -0.0241 11.00000 0.05 0.23 Q19 1 0.2415 0.7788 0.1181 11.00000 0.05 0.23 Q20 1 0.9829 0.6865 0.4720 11.00000 0.05 0.23 Q21 1 0.7163 0.6556 0.4744 11.00000 0.05 0.22 Q22 1 0.9387 0.6394 0.5590 11.00000 0.05 0.22 Q23 1 0.6997 0.6450 0.4528 11.00000 0.05 0.22 ; _shelx_res_checksum 183 _shelx_hkl_file ; 3 0 0 11.10 3.80 -3 0 0 1.10 3.40 3 0 0 6.30 4.10 4 0 0 1402.56 218.08 -4 0 0 1371.06 218.08 4 0 0 1416.86 217.98 -4 0 0 1352.36 217.98 5 0 0 43.70 9.00 -5 0 0 47.00 8.10 -5 0 0 51.29 8.70 5 0 0 28.80 8.10 -6 0 0 1501.45 244.38 6 0 0 1522.75 244.58 -6 0 0 1749.32 244.58 6 0 0 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40.90 19.30 -10 -11 -4 56.59 11.00 10 11 -4 61.29 16.50 -10 -11 -4 35.00 11.60 11 11 4 96.19 15.70 -11 -11 4 69.39 20.90 -11 -11 -4 56.09 16.10 11 11 -4 119.29 21.10 11 11 -4 41.00 22.90 -11 -11 -4 83.89 15.70 -12 -11 4 31.40 20.30 12 11 4 64.39 13.10 -12 -11 4 49.99 18.50 12 11 -4 37.10 22.00 -12 -11 -4 72.19 13.60 12 11 -4 57.09 17.00 -12 -11 -4 57.69 14.10 -13 -11 4 8.60 17.50 13 11 4 13.80 8.20 -13 -11 4 15.70 14.60 -13 -11 -4 17.00 9.60 13 11 -4 -12.40 18.30 13 11 -4 0.70 12.80 -13 -11 -4 10.50 8.40 -14 -11 4 -1.70 17.80 -14 -11 4 -11.70 13.60 14 11 -4 51.09 22.10 -14 -11 -4 0.60 9.30 -14 -11 -4 15.60 8.60 14 11 -4 -4.70 12.50 15 11 4 100.39 16.60 -15 -11 4 40.00 23.10 -15 -11 4 73.59 32.10 15 11 -4 40.50 26.10 -15 -11 -4 69.39 16.40 15 11 -4 104.99 20.80 -15 -11 -4 58.79 16.60 16 11 4 1.10 8.40 -16 -11 4 -1.40 19.40 -16 -11 4 -17.30 12.90 16 11 -4 51.09 23.90 -16 -11 -4 18.30 10.90 16 11 -4 -12.60 13.60 -16 -11 -4 4.30 9.50 -17 -11 4 19.40 20.60 17 11 4 25.20 10.80 -17 -11 4 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7.60 10.10 14 -12 -4 5.10 6.90 -14 12 -4 3.10 9.70 14 -12 -4 -6.30 9.60 -13 12 4 16.80 9.00 13 -12 4 9.60 7.90 13 -12 4 9.30 10.10 -13 12 -4 21.20 10.40 13 -12 -4 13.50 7.50 13 -12 -4 11.60 9.90 12 -12 4 13.50 9.90 12 -12 4 0.20 7.80 -12 12 4 -0.40 7.60 -12 12 -4 -2.80 12.60 12 -12 -4 11.80 6.80 -12 12 -4 3.30 9.30 12 -12 -4 16.90 9.10 11 -12 4 -13.40 7.90 -11 12 4 -0.70 6.90 11 -12 4 9.60 7.40 11 -12 -4 7.30 5.80 11 -12 -4 1.40 7.60 -11 12 -4 -12.20 9.40 -11 12 -4 14.40 7.80 10 -12 4 127.39 21.30 10 -12 4 92.49 20.20 -10 12 4 110.29 19.60 -10 12 -4 102.59 20.40 10 -12 -4 125.09 20.30 -10 12 -4 104.09 21.00 10 -12 -4 105.39 19.20 9 -12 4 1.00 7.50 9 -12 4 4.00 6.80 9 -12 -4 -2.70 4.70 -9 12 -4 2.50 9.30 9 -12 -4 -2.30 6.40 -9 12 -4 4.30 6.30 8 -12 4 41.20 11.80 8 -12 4 64.59 12.60 -8 12 4 51.99 11.10 8 -12 -4 51.39 10.30 -8 12 -4 53.29 11.80 -8 12 -4 37.40 13.10 8 -12 -4 67.39 11.40 7 -12 4 116.39 25.70 -7 12 4 145.19 24.70 7 -12 4 182.18 26.20 -7 12 -4 138.19 26.30 -7 12 -4 157.58 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15 -12 -5 15.00 8.90 14 -12 5 7.20 8.50 14 -12 5 -10.00 9.50 -14 12 5 -7.60 9.50 14 -12 -5 -2.80 9.90 -14 12 -5 -6.10 10.10 14 -12 -5 -12.80 6.50 13 -12 5 5.20 8.50 13 -12 5 22.90 11.10 -13 12 5 1.20 9.30 13 -12 -5 17.80 7.80 -13 12 -5 1.70 10.10 13 -12 -5 18.80 10.80 -12 12 5 -9.00 8.20 12 -12 5 12.50 9.80 12 -12 5 5.60 7.90 12 -12 -5 11.80 9.20 -12 12 -5 7.90 10.20 12 -12 -5 -14.50 5.70 11 -12 5 9.50 9.20 11 -12 5 12.70 8.80 -11 12 5 11.40 8.70 11 -12 -5 8.60 9.60 11 -12 -5 5.70 6.30 -11 12 -5 -3.40 10.50 10 -12 5 -2.30 7.10 10 -12 5 25.00 9.50 -10 12 5 14.40 8.80 10 -12 -5 12.50 8.20 10 -12 -5 7.30 6.10 -10 12 -5 -5.70 6.50 -10 12 -5 16.40 10.70 9 -12 5 64.39 12.60 9 -12 5 75.79 13.10 -9 12 5 29.10 12.80 -9 12 -5 41.90 13.40 -9 12 -5 55.29 11.20 9 -12 -5 38.90 11.10 9 -12 -5 35.90 9.70 8 -12 5 0.30 7.60 8 -12 5 8.80 8.00 -8 12 5 4.50 8.10 -8 12 -5 10.60 6.60 8 -12 -5 6.00 4.70 -8 12 -5 -8.10 9.60 7 -12 5 30.10 11.70 -7 12 5 45.20 12.00 7 -12 5 73.39 12.80 7 -12 -5 48.50 9.60 -7 12 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125.09 27.70 -5 -12 -5 153.58 23.40 5 12 -5 138.49 31.10 -6 -12 5 51.79 23.00 -6 -12 5 50.39 21.20 6 12 5 75.29 11.80 6 12 -5 86.19 22.60 -6 -12 -5 57.49 12.50 -7 -12 5 42.50 20.00 -7 -12 5 19.40 20.70 7 12 -5 50.39 20.00 -7 -12 -5 64.29 11.30 7 12 -5 60.99 19.00 8 12 5 3.70 4.30 -8 -12 5 -8.20 18.20 -8 -12 5 -5.70 16.00 8 12 -5 -7.80 14.00 8 12 -5 -16.60 13.50 -8 -12 -5 -1.60 5.20 -8 -12 -5 0.70 11.80 9 12 5 51.89 10.00 -9 -12 5 48.40 19.10 -9 -12 5 73.19 27.90 -9 -12 -5 47.50 11.50 -9 -12 -5 32.40 10.20 9 12 -5 58.69 19.30 9 12 -5 72.49 18.70 10 12 5 13.30 6.50 -10 -12 5 11.00 18.30 -10 -12 5 25.60 16.80 10 12 -5 8.40 14.70 -10 -12 -5 12.50 7.10 -10 -12 -5 16.60 8.60 10 12 -5 -6.10 16.60 -11 -12 5 -6.90 14.50 11 12 5 2.30 6.00 -11 -12 5 4.30 17.60 11 12 -5 -22.60 16.60 -11 -12 -5 -7.40 6.10 -11 -12 -5 -5.10 7.80 11 12 -5 -10.00 13.10 -12 -12 5 2.50 15.00 12 12 5 -7.10 6.20 -12 -12 5 35.70 21.20 12 12 -5 -18.50 18.20 -12 -12 -5 -1.30 6.60 -12 -12 -5 14.00 8.70 12 12 -5 29.80 13.60 -13 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29.50 10.70 5 -12 6 9.40 10.80 5 -12 -6 35.30 6.30 -5 12 -6 32.20 20.20 -5 12 -6 30.10 9.00 4 -12 6 4.60 9.30 4 -12 6 21.50 14.50 -4 12 -6 12.40 6.30 -4 12 -6 -12.60 17.10 3 -12 6 67.69 14.90 3 -12 6 41.10 19.10 -3 12 -6 39.30 21.20 -3 12 -6 66.69 12.90 2 -12 6 15.80 9.80 2 -12 6 8.50 14.40 -2 12 -6 12.90 6.70 -2 12 -6 -7.00 16.30 1 -12 6 41.50 12.50 1 -12 6 -5.30 14.60 -1 12 -6 4.70 17.10 -1 12 -6 39.70 9.30 0 -12 6 78.79 16.10 0 -12 6 16.20 17.30 0 12 -6 60.19 12.60 0 12 -6 48.90 21.00 -1 -12 6 40.20 13.40 -1 -12 6 30.30 15.90 1 12 -6 -10.90 17.10 1 12 -6 23.70 9.20 -2 -12 6 10.50 12.20 -2 -12 6 30.80 16.70 2 12 -6 20.80 9.10 2 12 -6 -3.10 17.40 -3 -12 6 47.40 23.60 -3 -12 6 11.90 14.30 -3 -12 6 42.30 18.90 3 12 -6 41.40 15.70 3 12 -6 37.40 12.00 3 12 -6 69.99 21.10 -4 -12 6 14.10 21.90 -4 -12 6 32.00 18.20 4 12 -6 30.90 14.80 4 12 -6 25.00 20.80 -5 -12 6 36.30 18.50 -5 -12 6 55.19 23.40 5 12 -6 17.60 14.70 5 12 -6 23.20 19.20 -5 -12 -6 30.10 6.70 6 12 6 43.90 7.80 -6 -12 6 23.10 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11.40 19 -12 -7 11.90 10.60 -19 12 -7 -18.40 12.50 18 -12 7 -11.90 10.40 18 -12 -7 26.50 10.80 -18 12 -7 -1.60 12.40 18 -12 -7 5.10 15.60 -17 12 7 4.10 22.40 17 -12 7 12.50 11.30 17 -12 -7 13.40 9.70 -17 12 -7 4.40 12.80 17 -12 -7 15.60 15.00 16 -12 7 7.70 11.30 -16 12 7 6.50 13.30 16 -12 -7 40.00 15.90 16 -12 -7 42.20 11.10 -16 12 -7 11.40 12.70 15 -12 7 -1.80 9.30 -15 12 7 34.70 15.90 15 -12 7 0.40 12.10 -15 12 -7 15.70 12.20 15 -12 -7 9.10 13.00 -15 12 -7 9.20 9.90 15 -12 -7 19.80 9.20 14 -12 7 11.60 10.20 14 -12 7 26.80 10.30 -14 12 7 21.50 15.40 14 -12 -7 -2.40 8.10 -14 12 -7 6.10 11.30 -14 12 -7 -3.10 8.90 14 -12 -7 0.90 12.30 -13 12 7 25.00 14.20 13 -12 7 16.00 11.10 -13 12 -7 45.20 11.50 13 -12 -7 33.90 13.40 13 -12 -7 27.30 9.60 12 -12 7 10.50 9.90 -12 12 7 3.10 12.80 12 -12 -7 30.60 11.90 12 -12 -7 14.50 7.80 -12 12 -7 10.30 12.40 -12 12 -7 8.60 7.80 11 -12 7 20.30 10.70 -11 12 7 -3.30 13.10 11 -12 7 0.80 7.10 -11 12 -7 -5.40 4.10 11 -12 -7 10.30 10.40 -11 12 -7 23.80 12.60 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13 -4 15.40 20.10 -13 -13 -4 14.30 9.20 14 13 4 4.50 8.50 -14 -13 4 30.50 22.10 -14 -13 4 31.60 20.70 14 13 -4 49.70 22.40 -14 -13 -4 7.00 9.80 -14 -13 -4 13.10 10.90 14 13 -4 36.60 15.20 15 13 4 9.00 8.30 -15 -13 4 15.30 15.20 -15 -13 4 -2.90 21.70 -15 -13 -4 20.30 10.60 15 13 -4 19.90 14.50 15 13 -4 -55.39 19.20 -15 -13 -4 -14.10 9.30 -16 -13 4 51.99 17.00 16 13 4 16.20 9.30 -16 -13 4 30.50 20.80 -16 -13 -4 6.20 10.80 16 13 -4 34.60 16.60 16 13 -4 6.90 24.90 -16 -13 -4 6.30 11.20 -17 -13 4 10.70 15.50 17 13 4 34.90 10.30 -17 -13 4 -23.90 18.00 -17 -13 -4 -13.10 10.00 -17 -13 -4 4.20 11.20 17 13 -4 8.10 15.10 18 13 4 15.00 10.30 18 13 4 29.60 19.20 -18 -13 4 2.60 15.30 -18 -13 4 -33.30 18.30 18 13 -4 30.10 17.70 -18 -13 -4 10.60 12.20 18 13 -4 -36.30 20.90 -18 -13 -4 28.60 13.30 -19 -13 4 -4.30 14.10 19 13 4 3.20 10.10 19 13 4 21.10 19.90 -19 -13 4 -25.30 20.10 19 13 -4 -8.60 23.90 -19 -13 -4 -21.80 10.20 -19 -13 -4 -14.60 10.60 19 13 -4 2.90 16.60 20 13 4 -3.60 10.10 20 13 4 -8.20 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21.00 11.20 7 -15 7 11.30 15.00 -7 15 -7 57.29 25.80 6 -15 7 19.70 11.40 6 -15 7 12.10 19.10 -6 15 -7 7.40 22.30 5 -15 7 4.10 10.80 5 -15 7 19.80 18.60 -5 15 -7 31.10 24.10 4 -15 7 52.49 23.80 4 -15 7 103.29 19.20 -4 15 -7 56.49 26.80 3 -15 7 -7.90 11.80 3 -15 7 10.80 18.30 -3 15 -7 -3.20 19.00 2 -15 7 21.80 13.10 2 -15 7 60.19 20.90 -2 15 -7 6.50 21.80 1 -15 7 -14.80 11.30 1 -15 7 -5.50 17.00 -1 15 -7 -2.90 8.30 -1 15 -7 3.00 19.80 0 -15 7 14.30 13.90 0 -15 7 0.80 17.90 0 15 -7 16.50 21.70 0 15 -7 13.50 9.60 -1 -15 7 -9.50 17.70 -1 -15 7 -4.30 13.60 1 15 -7 12.50 12.20 1 15 -7 -15.60 19.90 -2 -15 7 4.40 20.00 -2 -15 7 43.30 15.80 2 15 -7 8.30 23.70 -3 -15 7 49.70 22.40 -3 -15 7 7.60 15.30 3 15 -7 -10.40 22.10 -4 -15 7 62.49 18.40 -4 -15 7 29.90 22.00 4 15 -7 32.80 23.50 -5 -15 7 -8.90 23.90 -5 -15 7 -8.70 14.60 -5 -15 7 41.70 22.50 5 15 -7 0.90 14.80 5 15 -7 -33.40 18.40 -6 -15 7 53.69 26.00 -6 -15 7 5.10 20.40 6 15 -7 3.40 15.70 6 15 -7 6.60 20.10 -7 -15 7 2.00 20.20 -7 -15 7 3.00 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24.10 21.50 -3 15 -9 35.30 24.60 2 -15 9 1.80 13.10 2 -15 9 1.20 20.30 -2 15 -9 33.50 25.40 1 -15 9 18.10 12.70 1 -15 9 -8.80 18.60 -1 15 -9 -41.10 22.60 0 -15 9 3.00 12.50 0 -15 9 7.50 21.10 0 15 -9 -10.40 21.00 -1 -15 9 -1.10 20.60 -1 -15 9 26.10 14.60 1 15 -9 -28.20 22.90 -2 -15 9 0.10 20.40 -2 -15 9 37.50 15.90 2 15 -9 22.90 25.10 -3 -15 9 -12.10 19.80 -3 -15 9 12.20 22.50 3 15 -9 -15.40 24.50 -4 -15 9 77.09 23.50 -4 -15 9 33.50 22.50 4 15 -9 -2.40 22.90 -5 -15 9 -12.00 19.90 -5 -15 9 44.90 15.00 5 15 -9 0.10 23.80 5 15 -9 -17.20 5.20 5 15 -9 18.90 15.90 -6 -15 9 -37.70 19.80 -6 -15 9 5.90 25.50 -6 -15 9 49.80 15.60 6 15 -9 -22.70 21.20 6 15 -9 13.40 11.60 -7 -15 9 24.80 16.20 -7 -15 9 20.70 27.10 -7 -15 9 6.00 21.00 7 15 -9 12.00 21.90 -8 -15 9 -18.70 19.50 -8 -15 9 23.50 27.30 -8 -15 9 0.40 15.80 -8 -15 -9 5.00 5.70 8 15 -9 61.69 24.90 8 15 -9 -5.00 21.20 -9 -15 9 28.10 25.90 -9 -15 9 -9.10 20.90 9 15 9 6.60 5.80 -9 -15 -9 15.00 6.50 9 15 -9 17.30 22.10 9 15 -9 26.00 20.20 -10 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10 -7.60 13.00 12 -15 10 -9.20 21.10 -12 15 10 13.40 14.60 -12 15 -10 25.30 16.70 12 -15 -10 -2.90 6.70 12 -15 -10 1.50 15.10 11 -15 10 -6.30 14.30 11 -15 10 -1.60 21.70 -11 15 -10 79.69 30.60 11 -15 -10 -6.50 13.90 11 -15 -10 12.10 6.80 -11 15 -10 36.80 17.70 10 -15 10 25.80 16.10 10 -15 10 17.20 22.90 -10 15 -10 2.90 16.00 -10 15 -10 -5.30 25.70 10 -15 -10 7.20 14.20 10 -15 -10 3.90 6.00 9 -15 10 29.40 23.70 -9 15 -10 48.20 28.10 9 -15 -10 11.50 6.20 8 -15 10 -21.00 19.50 -8 15 -10 66.69 28.10 8 -15 -10 -2.60 4.60 7 -15 10 13.30 15.50 7 -15 10 35.70 22.50 -7 15 -10 8.40 9.10 6 -15 10 13.40 11.60 6 -15 10 -3.10 20.80 -6 15 -10 2.30 8.30 -6 15 -10 -19.50 23.70 5 -15 10 27.30 11.70 5 -15 10 9.80 20.00 -5 15 -10 -8.70 24.10 -5 15 -10 -8.70 7.30 4 -15 10 6.30 10.70 4 -15 10 -31.80 18.40 -4 15 -10 -4.80 8.00 -4 15 -10 10.10 23.60 3 -15 10 -2.70 9.60 3 -15 10 19.30 21.40 -3 15 -10 -55.79 21.40 -3 15 -10 9.90 9.00 2 -15 10 -6.80 9.20 2 -15 10 14.30 21.40 -2 15 -10 1.50 24.50 -2 15 -10 0.70 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18 9 5 2.5556 -1.5071 18 9 6 -0.9881 1.4730 18 9 7 -0.5304 -0.2429 18 9 8 -0.2163 1.1677 18 10 0 2.0804 0.0148 18 10 1 -1.0124 -1.4597 18 10 2 -1.8878 2.3126 18 10 3 -1.1327 3.0030 18 10 4 -2.0299 3.6712 18 10 5 0.8370 3.8530 18 10 6 -1.0683 1.9067 18 10 7 -0.4197 -1.4115 18 10 8 -1.9839 -0.5110 18 11 0 -0.0676 -0.0232 18 11 1 0.1320 0.3367 18 11 2 -0.3154 1.9191 18 11 3 -0.8213 -0.7861 18 11 4 -1.3874 -0.2540 18 11 5 0.3035 -0.8742 18 11 6 -2.6412 1.9978 18 11 7 -0.4389 -0.3234 18 11 8 -0.2293 -0.7927 18 12 0 -0.1334 0.0058 18 12 1 -0.9320 0.1238 18 12 2 2.9413 1.1105 18 12 3 3.2514 -2.0920 18 12 4 1.8340 -1.7690 18 12 5 1.4015 -1.5341 18 12 6 -1.2070 -0.0284 18 12 7 1.1086 0.5877 18 13 0 0.0671 -0.0305 18 13 1 -0.6382 0.4503 18 13 2 -1.2744 0.2413 18 13 3 -1.7120 -1.1245 18 13 4 -3.8569 2.8376 18 13 5 -2.0709 2.0952 18 13 6 0.5941 0.7012 18 14 0 3.4085 -0.0054 18 14 1 1.4853 -0.1844 18 14 2 0.5220 0.8642 18 14 3 -0.9774 -0.4442 18 14 4 0.1715 0.5318 18 14 5 -0.1938 -2.2585 18 15 0 -0.5262 0.0087 18 15 1 0.8914 1.1026 18 15 2 0.2335 0.7714 18 15 3 -0.6818 0.4781 18 15 4 -0.6518 -0.0789 18 16 0 -1.0147 0.0060 18 16 1 -0.3132 -0.1541 18 16 2 0.0468 2.1846 19 0 1 0.3592 0.6023 19 0 2 0.5102 0.7940 19 0 3 0.3863 1.6073 19 0 4 0.0646 0.0570 19 0 5 -0.2868 -0.3843 19 0 6 -0.4746 0.7308 19 0 7 -0.3887 0.5681 19 0 8 -0.1432 -1.0542 19 0 9 0.1128 2.1430 19 1 0 -0.3058 -0.1960 19 1 1 -0.9665 0.6439 19 1 2 -1.1049 1.0243 19 1 3 0.7992 -1.1956 19 1 4 1.3489 -0.9883 19 1 5 -1.5563 2.3623 19 1 6 -2.3950 1.8742 19 1 7 2.4328 -0.7621 19 1 8 0.2817 0.7002 19 1 9 -1.5880 3.7170 19 2 0 -1.4230 -0.1448 19 2 1 0.2732 0.0380 19 2 2 0.2508 -2.0819 19 2 3 0.0866 1.0660 19 2 4 -0.8575 -0.6307 19 2 5 0.7433 -2.7949 19 2 6 -0.1114 3.6169 19 2 7 0.5474 2.4914 19 2 8 0.4473 -1.8516 19 2 9 0.2487 0.4171 19 3 0 -0.4820 -0.1804 19 3 1 -1.1502 -1.6914 19 3 2 3.1470 -0.5195 19 3 3 3.8825 0.6157 19 3 4 -0.8897 -0.1805 19 3 5 -0.4289 -0.1896 19 3 6 0.2641 0.7686 19 3 7 1.4034 -0.3083 19 3 8 1.7608 0.2559 19 3 9 2.8674 1.1870 19 4 0 -0.9846 -0.0280 19 4 1 -0.4524 -0.5882 19 4 2 0.1821 -0.1032 19 4 3 0.0665 2.9663 19 4 4 -2.3051 0.1795 19 4 5 0.8893 -1.8462 19 4 6 -0.5690 0.6509 19 4 7 0.7560 -1.6524 19 4 8 -2.7984 -0.8238 19 4 9 -1.6892 1.0867 19 5 0 -2.3699 -0.0340 19 5 1 -2.5155 0.2636 19 5 2 -0.5973 2.9856 19 5 3 0.9073 2.3166 19 5 4 0.3101 -2.6065 19 5 5 -0.6884 -4.2873 19 5 6 -0.1199 -0.6253 19 5 7 0.6360 -1.6220 19 5 8 1.5396 -0.8596 19 5 9 1.3226 0.9982 19 6 0 -3.4070 -0.0135 19 6 1 -1.2802 0.9902 19 6 2 1.9997 1.8708 19 6 3 0.4349 0.2669 19 6 4 -1.8945 -1.8724 19 6 5 -1.1204 0.3025 19 6 6 -1.8649 -0.6168 19 6 7 1.9534 0.7314 19 6 8 -1.0565 0.4425 19 6 9 0.0971 -0.9649 19 7 0 1.1744 -0.0142 19 7 1 -0.8007 -2.6566 19 7 2 -4.3932 0.8164 19 7 3 -3.8459 1.9052 19 7 4 -0.7366 -0.3242 19 7 5 -1.3165 0.0557 19 7 6 0.0195 1.7949 19 7 7 -2.1684 0.3535 19 7 8 1.2161 0.1189 19 8 0 -1.8092 0.0120 19 8 1 -0.9573 0.1986 19 8 2 0.8736 -0.4747 19 8 3 -2.5124 -2.4175 19 8 4 -1.3785 -3.6350 19 8 5 -0.0541 -0.7700 19 8 6 0.4618 -2.6365 19 8 7 0.1188 1.7504 19 8 8 -0.3747 2.0449 19 9 0 -0.5192 -0.0344 19 9 1 -0.3797 -0.7288 19 9 2 -0.0679 1.0246 19 9 3 -1.8294 0.9202 19 9 4 -0.8694 -3.0200 19 9 5 0.1659 0.2771 19 9 6 2.2292 0.6614 19 9 7 0.5042 -0.0857 19 10 0 -0.7270 -0.0640 19 10 1 -1.7740 1.6042 19 10 2 -1.7621 1.0934 19 10 3 -4.1435 2.1004 19 10 4 -0.6913 0.5616 19 10 5 -1.7246 2.3551 19 10 6 -0.9698 0.9891 19 10 7 -0.3549 1.8730 19 11 0 -0.1441 0.0005 19 11 1 -0.5131 0.3517 19 11 2 -1.0509 0.3671 19 11 3 -0.6966 0.7537 19 11 4 0.6699 -3.8158 19 11 5 1.9066 0.1189 19 11 6 0.6188 -0.3781 19 12 0 0.0426 -0.0078 19 12 1 -0.8619 -1.5942 19 12 2 -1.2059 -1.4166 19 12 3 -1.5836 1.5542 19 12 4 1.4474 2.2543 19 12 5 0.4324 2.3089 19 12 6 2.3557 -0.7421 19 13 0 -0.0373 -0.0689 19 13 1 0.1925 1.5806 19 13 2 -0.0793 0.7536 19 13 3 3.2169 1.7367 19 13 4 1.2933 -1.2497 19 13 5 -1.2098 -1.3203 19 14 0 -0.8428 -0.0247 19 14 1 -0.7804 1.0136 19 14 2 0.2277 0.8679 19 14 3 0.7345 -0.8732 19 15 0 1.4296 -0.0130 19 15 1 0.1829 -1.2343 19 15 2 -1.1569 -0.5711 20 0 0 0.5314 0.1729 20 0 1 0.4506 0.2103 20 0 2 -0.2900 0.1963 20 0 3 -0.3961 0.0197 20 0 4 -0.2032 -0.2153 20 0 5 0.6348 -0.3571 20 0 6 2.4578 -0.3701 20 0 7 -0.0127 -0.2349 20 0 8 1.2140 -0.0069 20 1 0 1.3083 0.1152 20 1 1 0.0891 0.1099 20 1 2 -1.9546 -1.2662 20 1 3 -1.6207 -0.1019 20 1 4 1.8749 2.3949 20 1 5 2.1520 3.4373 20 1 6 0.0567 -0.9008 20 1 7 -0.9115 -1.2177 20 1 8 0.1073 2.7522 20 2 0 -0.9064 -0.0053 20 2 1 -2.2078 0.7292 20 2 2 0.2778 0.3943 20 2 3 2.5786 -0.1915 20 2 4 -0.2924 -0.2906 20 2 5 0.9039 -0.7586 20 2 6 0.8955 0.3401 20 2 7 -4.2771 0.9257 20 2 8 -0.3314 1.1615 20 3 0 -0.1520 -0.1403 20 3 1 0.2544 -1.2346 20 3 2 0.5894 -3.3874 20 3 3 -1.7493 1.8966 20 3 4 -1.0284 3.3285 20 3 5 -1.5064 3.2231 20 3 6 0.2035 0.9115 20 3 7 0.5766 -0.6827 20 3 8 1.4228 0.0949 20 4 0 1.3028 -0.0127 20 4 1 0.7762 -0.9332 20 4 2 2.1584 0.0911 20 4 3 0.0611 1.8595 20 4 4 -2.2689 0.3627 20 4 5 0.2788 -0.3804 20 4 6 -0.9099 -1.1335 20 4 7 -1.9456 0.3585 20 4 8 1.5842 0.7983 20 5 0 -1.4573 -0.0025 20 5 1 0.8316 -0.8474 20 5 2 1.6903 -1.0817 20 5 3 -2.8450 -0.4168 20 5 4 -1.6977 0.2344 20 5 5 -0.5084 0.5877 20 5 6 1.8563 -0.1219 20 5 7 0.5802 -0.8374 20 5 8 1.4692 0.0090 20 6 0 0.2998 -0.0125 20 6 1 2.0370 -2.3260 20 6 2 1.3845 0.0972 20 6 3 -0.9367 2.6359 20 6 4 0.3240 0.5284 20 6 5 2.3620 -0.8514 20 6 6 1.5988 -3.2186 20 6 7 1.4783 -1.6430 20 7 0 -5.0052 -0.0476 20 7 1 -0.8417 1.8037 20 7 2 1.2954 3.1778 20 7 3 -0.5882 -0.0318 20 7 4 -0.4565 -1.1365 20 7 5 -0.9699 -2.6492 20 7 6 -1.0533 -0.1229 20 7 7 -1.0686 -0.5978 20 8 0 -3.5604 0.0520 20 8 1 -0.1365 -0.8304 20 8 2 -1.6467 -0.3415 20 8 3 -2.7149 -0.0536 20 8 4 -1.2090 -0.7030 20 8 5 0.6579 -0.8458 20 8 6 1.9851 0.1396 20 8 7 3.8873 0.3571 20 9 0 -2.0535 0.0399 20 9 1 -0.2807 0.0214 20 9 2 -3.0234 1.9429 20 9 3 -4.5879 2.5321 20 9 4 -1.8665 0.7530 20 9 5 2.1113 -0.6880 20 9 6 0.6566 0.7311 20 10 0 -3.0436 -0.0373 20 10 1 -1.0773 2.6289 20 10 2 -2.1989 1.7865 20 10 3 -2.3255 -2.5055 20 10 4 -1.7711 -2.0965 20 10 5 -0.3905 -0.9765 20 10 6 -0.6171 0.3519 20 11 0 -2.2867 -0.0021 20 11 1 -0.2388 0.8299 20 11 2 -2.4657 -0.3276 20 11 3 -3.4228 -0.8113 20 11 4 -1.1432 -2.7679 20 11 5 1.9591 -1.5138 20 12 0 -0.7152 0.0092 20 12 1 -0.2164 -0.2147 20 12 2 -0.6449 -0.1754 20 12 3 -0.9267 -2.4639 20 12 4 -0.7529 0.3887 20 13 0 -0.5170 0.0067 20 13 1 0.5826 0.8549 20 13 2 -1.1199 -1.5459 21 0 1 -0.2285 -0.7780 21 0 2 -0.3271 -0.0681 21 0 3 -0.2145 -0.7327 21 0 4 0.0546 0.3047 21 0 5 0.2764 0.3406 21 0 6 0.3524 1.2145 21 0 7 0.2825 2.2280 21 1 0 -0.6391 0.1160 21 1 1 -1.4149 1.8669 21 1 2 1.1403 -0.1222 21 1 3 2.8721 -1.8997 21 1 4 3.5326 -0.9021 21 1 5 -0.1068 1.1002 21 1 6 -3.0780 1.5715 21 1 7 2.2390 0.6375 21 2 0 -0.3671 0.1409 21 2 1 -1.6907 0.1739 21 2 2 -2.7519 -1.9403 21 2 3 -0.5187 -0.0940 21 2 4 -0.0016 2.0488 21 2 5 0.8241 1.6412 21 2 6 1.5912 2.4756 21 2 7 1.0846 0.2538 21 3 0 -0.6417 0.1320 21 3 1 -1.9554 1.3008 21 3 2 0.9586 1.1604 21 3 3 1.9378 0.1666 21 3 4 0.9613 0.4808 21 3 5 -0.6099 -0.2082 21 3 6 -4.2897 -2.0360 21 3 7 -1.1972 -1.0245 21 4 0 -1.8311 0.0389 21 4 1 -0.4777 0.9793 21 4 2 -0.6239 0.9634 21 4 3 -0.3822 1.3635 21 4 4 -0.9691 -0.8896 21 4 5 -1.7592 1.0318 21 4 6 -2.8196 2.9589 21 4 7 -0.4501 0.5834 21 5 0 1.2443 0.0558 21 5 1 1.1263 -1.3884 21 5 2 0.3464 0.4179 21 5 3 -0.9269 -0.8605 21 5 4 1.2257 0.2976 21 5 5 2.2556 1.4717 21 5 6 1.1106 0.1698 21 6 0 -1.7911 0.0217 21 6 1 0.7659 -1.3338 21 6 2 1.5722 1.7947 21 6 3 0.6510 1.5038 21 6 4 -0.5957 -1.6835 21 6 5 -1.3381 -1.1037 21 6 6 -2.0762 -0.3434 21 7 0 0.1157 0.0204 21 7 1 1.2182 -1.8753 21 7 2 1.6702 -0.1841 21 7 3 -0.9493 -0.7648 21 7 4 -0.1909 0.2469 21 7 5 -0.2297 1.0146 21 7 6 1.1290 0.1796 21 8 0 0.6066 0.0095 21 8 1 -0.3163 -2.2873 21 8 2 0.7129 1.9164 21 8 3 1.6603 -0.0282 21 8 4 1.7140 -1.8393 21 8 5 1.5478 -2.1901 21 9 0 -1.0577 0.0306 21 9 1 -1.4368 0.4544 21 9 2 0.1429 1.0799 21 9 3 -3.4850 -0.5757 21 9 4 -2.2860 -1.9064 21 9 5 -1.2547 0.2988 21 10 0 1.0823 0.0378 21 10 1 -2.7234 -0.7695 21 10 2 -3.7330 2.0990 21 10 3 -3.2964 -0.1636 21 10 4 -0.1441 0.2546 21 11 0 -1.1449 -0.0202 21 11 1 -2.6698 0.3302 21 11 2 -2.1961 1.8842 22 0 0 -0.2128 -0.1603 22 0 1 2.4497 -0.1798 22 0 2 1.6420 -0.1333 22 0 3 1.9968 0.0300 22 0 4 0.8452 0.2401 22 0 5 0.3941 0.4073 22 0 6 0.2726 0.3204 22 1 0 0.8234 -0.0933 22 1 1 -1.1892 -1.2404 22 1 2 -1.8875 -1.1629 22 1 3 1.2221 -0.0689 22 1 4 1.8823 1.1723 22 1 5 0.7597 3.8654 22 1 6 -0.1826 0.6806 22 2 0 0.0284 0.0112 22 2 1 -0.5576 -0.2925 22 2 2 -0.9500 -1.8240 22 2 3 1.3637 -2.1108 22 2 4 0.6120 -0.1880 22 2 5 0.6658 -1.1533 22 2 6 0.1174 -0.6961 22 3 0 0.8032 0.0953 22 3 1 -0.7040 0.0232 22 3 2 -1.8527 0.0398 22 3 3 0.0935 0.9031 22 3 4 0.5990 0.7294 22 3 5 -1.9736 3.2133 22 4 0 1.2959 -0.0064 22 4 1 -0.0055 0.5421 22 4 2 -0.9045 2.0633 22 4 3 -1.4226 -0.6014 22 4 4 0.1935 1.1923 22 4 5 2.4276 2.5157 22 5 0 0.9596 -0.0117 22 5 1 0.9322 0.0072 22 5 2 -0.4743 0.9253 22 5 3 -0.3756 -1.5041 22 5 4 2.4224 -2.6460 22 5 5 -0.8384 -0.5720 22 6 0 -0.3996 -0.0075 22 6 1 1.2258 -1.5759 22 6 2 0.5378 1.1836 22 6 3 -1.8231 -0.2677 22 6 4 -1.8061 1.3013 22 7 0 -0.5562 0.0125 22 7 1 0.0026 -1.1452 22 7 2 -0.2715 0.8252 22 7 3 0.3760 0.6366 22 7 4 2.2209 0.2554 22 8 0 -4.3867 -0.0640 22 8 1 0.5528 0.0686 22 8 2 0.5628 -0.0780 22 8 3 0.1503 -0.6848 22 9 0 -0.2904 -0.0376 22 9 1 0.6508 0.3037 22 9 2 0.0652 1.2264 23 0 1 0.1075 0.0142 23 0 2 0.1727 2.4620 23 0 3 0.0810 3.1274 23 0 4 -0.0125 3.1666 23 1 0 -0.4170 -0.0390 23 1 1 0.2510 1.0014 23 1 2 1.9878 -1.5893 23 1 3 -0.1990 -1.1234 23 1 4 1.2313 0.2919 23 2 0 -1.2944 -0.0614 23 2 1 -1.1707 -0.1111 23 2 2 -0.1153 -0.8252 23 2 3 0.5252 -0.0424 23 3 0 -1.6755 -0.0595 23 3 1 -1.0202 1.8534 23 3 2 0.0652 0.1419 23 3 3 -1.1067 0.1308 23 4 0 0.1749 0.0083 23 4 1 1.9575 1.0153 23 4 2 -0.5993 0.2150 23 4 3 -1.5226 0.2628 23 5 0 -0.1053 -0.0423 23 5 1 0.8769 2.5497 23 5 2 0.2926 2.2056 23 6 0 0.1063 -0.0369 23 6 1 3.3715 0.6946 0 0 0 0.0 0.0 ; _shelx_fab_checksum 89497 _olex2_submission_special_instructions 'No special instructions were received' _site XU loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' '-x+1/2, y+1/2, -z' 'x+1/2, -y+1/2, -z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu1 Cu 0.26924(6) 0.59834(8) 0.10573(10) 0.1070(6) Uani 1 1 d . . . . . O1 O 0.2312(9) 0.4997(13) 0.2043(15) 0.169(5) Uani 0.603(15) 1 d D U P A 1 O2 O 0.2914(7) 0.5089(10) 0.0666(12) 0.154(5) Uani 0.603(15) 1 d D U P A 1 C1 C 0.2495(11) 0.4802(12) 0.1205(18) 0.159(5) Uani 0.603(15) 1 d D U P A 1 H1 H 0.230745 0.441782 0.096816 0.191 Uiso 0.603(15) 1 calc R U P A 1 O1A O 0.2164(9) 0.5550(14) 0.223(2) 0.153(5) Uani 0.397(15) 1 d D U P A 2 O2A O 0.2714(12) 0.4790(15) 0.148(3) 0.165(5) Uani 0.397(15) 1 d D U P A 2 C1A C 0.2171(13) 0.5004(17) 0.185(4) 0.160(5) Uani 0.397(15) 1 d D U P A 2 H1A H 0.176999 0.475628 0.183943 0.192 Uiso 0.397(15) 1 calc R U P A 2 O3 O 0.2622(9) 0.7067(11) 0.1149(13) 0.162(6) Uani 0.594(11) 1 d D U P A 1 O4 O 0.3223(7) 0.6615(9) -0.0022(10) 0.138(6) Uani 0.594(11) 1 d D U P A 1 C2 C 0.2948(11) 0.7088(11) 0.0362(16) 0.154(6) Uani 0.594(11) 1 d D U P A 1 H2 H 0.299047 0.748255 0.003584 0.185 Uiso 0.594(11) 1 calc R U P A 1 O3A O 0.2201(11) 0.6591(14) 0.1978(17) 0.161(7) Uani 0.406(11) 1 d D U P A 2 O4A O 0.2423(17) 0.7394(15) 0.099(2) 0.179(8) Uani 0.406(11) 1 d D U P A 2 C2A C 0.2158(15) 0.7151(14) 0.173(3) 0.167(7) Uani 0.406(11) 1 d D U P A 2 H2A H 0.189933 0.741999 0.214633 0.201 Uiso 0.406(11) 1 calc R U P A 2 O5 O 0.8865(8) 0.2930(7) 0.3962(11) 0.195(4) Uani 1 1 d . U . . . O6 O 0.7307(5) 0.3975(6) 0.6968(9) 0.168(4) Uani 1 1 d D U . . . O7 O 0.8639(6) 0.7166(5) 0.4786(10) 0.148(3) Uani 1 1 d . U . . . O8 O 1.0546(4) 0.7553(4) 0.7690(11) 0.135(4) Uani 1 1 d . . . . . N1 N 0.3536(3) 0.5986(5) 0.1881(6) 0.089(2) Uani 1 1 d . . . . . N2 N 1.1876(4) 0.5943(5) 1.0183(7) 0.100(3) Uani 1 1 d . . . . . C3 C 0.3543(4) 0.6128(5) 0.2832(8) 0.082(3) Uani 1 1 d . . . . . H3 H 0.312974 0.626596 0.312031 0.098 Uiso 1 1 calc R U . . . C4 C 0.4093(4) 0.6093(4) 0.3424(7) 0.074(2) Uani 1 1 d . . . . . H4 H 0.406261 0.619861 0.410343 0.089 Uiso 1 1 calc R U . . . C5 C 0.4716(4) 0.5894(4) 0.3008(7) 0.070(2) Uani 1 1 d . . . . . C6 C 0.4705(4) 0.5766(5) 0.2035(8) 0.087(3) Uani 1 1 d . . . . . H6 H 0.511121 0.564081 0.171384 0.105 Uiso 1 1 calc R U . . . C7 C 0.4123(5) 0.5812(6) 0.1507(8) 0.106(4) Uani 1 1 d . . . . . H7 H 0.414021 0.571180 0.082358 0.127 Uiso 1 1 calc R U . . . C8 C 0.5340(3) 0.5834(4) 0.3629(6) 0.065(2) Uani 1 1 d . . . . . C9 C 0.5315(4) 0.5821(5) 0.4632(7) 0.084(3) Uani 1 1 d . . . . . H9 H 0.488456 0.583142 0.494757 0.101 Uiso 1 1 calc R U . . . C10 C 0.5891(4) 0.5792(5) 0.5207(7) 0.083(3) Uani 1 1 d . . . . . H10 H 0.585396 0.580129 0.590590 0.099 Uiso 1 1 calc R U . . . C11 C 0.6533(4) 0.5750(4) 0.4761(8) 0.077(3) Uani 1 1 d . . . . . C12 C 0.6562(4) 0.5753(5) 0.3744(8) 0.083(3) Uani 1 1 d . . . . . H12 H 0.698894 0.573296 0.342096 0.100 Uiso 1 1 calc R U . . . C13 C 0.5974(4) 0.5784(5) 0.3192(7) 0.077(3) Uani 1 1 d . . . . . H13 H 0.600391 0.577020 0.249292 0.092 Uiso 1 1 calc R U . . . C14 C 0.7156(4) 0.5767(4) 0.5378(8) 0.083(3) Uani 1 1 d . . . . . C15 C 0.7518(5) 0.5206(4) 0.5571(9) 0.101(4) Uani 1 1 d . . . . . C16 C 0.8094(4) 0.5264(4) 0.6132(9) 0.094(3) Uani 1 1 d . . . . . H16 H 0.834541 0.489125 0.626714 0.113 Uiso 1 1 calc R U . . . C17 C 0.8333(4) 0.5823(4) 0.6511(8) 0.082(3) Uani 1 1 d . . . . . C18 C 0.7978(4) 0.6382(4) 0.6331(8) 0.079(3) Uani 1 1 d . . . . . C19 C 0.7369(4) 0.6318(4) 0.5744(7) 0.081(3) Uani 1 1 d . . . . . H19 H 0.710838 0.668485 0.561233 0.098 Uiso 1 1 calc R U . . . C20 C 0.8195(4) 0.7016(4) 0.6712(8) 0.080(3) Uani 1 1 d . . . . . H20A H 0.789479 0.734229 0.642452 0.095 Uiso 1 1 calc R U . . . H20B H 0.812998 0.702359 0.743636 0.095 Uiso 1 1 calc R U . . . C21 C 0.8916(5) 0.7188(5) 0.6489(10) 0.086(3) Uani 1 1 d . . . . . C22 C 0.9382(4) 0.7340(4) 0.7204(10) 0.090(3) Uani 1 1 d . . . . . H22 H 0.925092 0.737232 0.787651 0.108 Uiso 1 1 calc R U . . . C23 C 1.0061(5) 0.7447(5) 0.6915(12) 0.096(3) Uani 1 1 d . . . . . C24 C 1.0251(6) 0.7472(5) 0.5976(16) 0.113(5) Uani 1 1 d . . . . . C25 C 0.9815(6) 0.7374(5) 0.5254(11) 0.102(3) Uani 1 1 d . . . . . H25 H 0.994878 0.739763 0.458111 0.122 Uiso 1 1 calc R U . . . C26 C 0.9116(7) 0.7228(6) 0.5533(13) 0.115(4) Uani 1 1 d . U . . . C27 C 0.8764(13) 0.6839(13) 0.3916(19) 0.207(9) Uani 1 1 d . . . . . H27A H 0.896297 0.642386 0.408313 0.249 Uiso 1 1 calc R U . . . H27B H 0.910382 0.707546 0.352630 0.249 Uiso 1 1 calc R U . . . C28 C 0.8161(14) 0.6737(14) 0.330(2) 0.258(15) Uani 1 1 d . . . . . H28A H 0.829562 0.653513 0.268082 0.387 Uiso 1 1 calc R U . . . H28B H 0.794548 0.714358 0.316008 0.387 Uiso 1 1 calc R U . . . H28C H 0.784101 0.646416 0.365274 0.387 Uiso 1 1 calc R U . . . C29 C 1.0332(8) 0.7573(7) 0.8704(13) 0.130(5) Uani 1 1 d . . . . . H29A H 1.014289 0.716070 0.891097 0.156 Uiso 1 1 calc R U . . . H29B H 0.998245 0.790265 0.880309 0.156 Uiso 1 1 calc R U . . . C30 C 1.0954(10) 0.7723(10) 0.9270(18) 0.209(11) Uani 1 1 d . . . . . H30A H 1.120844 0.733415 0.939557 0.313 Uiso 1 1 calc R U . . . H30B H 1.082906 0.791866 0.989989 0.313 Uiso 1 1 calc R U . . . H30C H 1.123575 0.801597 0.888936 0.313 Uiso 1 1 calc R U . . . C31 C 0.7292(6) 0.4599(5) 0.5087(11) 0.124(4) Uani 1 1 d . U . . . H31A H 0.729492 0.466402 0.436401 0.149 Uiso 1 1 calc R U . . . H31B H 0.681619 0.451903 0.528420 0.149 Uiso 1 1 calc R U . . . C34 C 0.8135(4) 0.3179(4) 0.6349(7) 0.123(5) Uani 1 1 d G . . . . H34 H 0.814608 0.296903 0.696864 0.147 Uiso 1 1 calc R U . . . C33 C 0.7716(3) 0.3699(4) 0.6216(8) 0.120(4) Uani 1 1 d DG . . . . C32 C 0.7701(4) 0.4007(3) 0.5310(9) 0.117(4) Uani 1 1 d G . . . . C37 C 0.8104(5) 0.3793(5) 0.4537(7) 0.133(5) Uani 1 1 d G . . . . H37 H 0.809343 0.400341 0.391825 0.160 Uiso 1 1 calc R U . . . C36 C 0.8523(5) 0.3273(5) 0.4671(7) 0.180(5) Uani 1 1 d G U . . . C35 C 0.8539(4) 0.2966(3) 0.5577(8) 0.120(5) Uani 1 1 d DG . . . . C38 C 0.8686(14) 0.3097(13) 0.3047(17) 0.212(6) Uani 1 1 d . U . . . H38A H 0.888415 0.351033 0.286726 0.254 Uiso 1 1 calc R U . . . H38B H 0.818645 0.312178 0.298391 0.254 Uiso 1 1 calc R U . . . C39 C 0.8987(15) 0.2545(14) 0.236(2) 0.250(9) Uani 1 1 d . U . . . H39A H 0.936993 0.270849 0.197921 0.374 Uiso 1 1 calc R U . . . H39B H 0.863300 0.239534 0.191081 0.374 Uiso 1 1 calc R U . . . H39C H 0.914020 0.219477 0.277766 0.374 Uiso 1 1 calc R U . . . C40 C 0.6772(9) 0.3496(11) 0.7255(15) 0.216(6) Uani 1 1 d D U . . . H40A H 0.638656 0.351711 0.678860 0.260 Uiso 1 1 calc R U . . . H40B H 0.696554 0.306506 0.722846 0.260 Uiso 1 1 calc R U . . . C41 C 0.6536(12) 0.3637(12) 0.8268(15) 0.247(8) Uani 1 1 d D U . . . H41A H 0.685617 0.345830 0.874546 0.370 Uiso 1 1 d R U . . . H41B H 0.608487 0.345680 0.837826 0.370 Uiso 1 1 d R U . . . H41C H 0.651637 0.409610 0.835146 0.370 Uiso 1 1 d R U . . . C42 C 0.8981(6) 0.2378(5) 0.5690(16) 0.141(6) Uani 1 1 d D . . . . H42A H 0.897507 0.214015 0.506198 0.169 Uiso 1 1 calc R U . . . H42B H 0.878205 0.210438 0.620622 0.169 Uiso 1 1 calc R U . . . C43 C 0.8951(4) 0.5825(4) 0.7154(8) 0.078(3) Uani 1 1 d . . . . . C44 C 0.9591(5) 0.5813(4) 0.6741(8) 0.087(3) Uani 1 1 d . . . . . H44 H 0.963058 0.579688 0.604291 0.104 Uiso 1 1 calc R U . . . C45 C 1.0178(4) 0.5822(4) 0.7307(8) 0.080(3) Uani 1 1 d . . . . . H45 H 1.061317 0.581987 0.700610 0.095 Uiso 1 1 calc R U . . . C46 C 1.0106(4) 0.5836(5) 0.8355(8) 0.082(3) Uani 1 1 d . . . . . C47 C 0.9471(5) 0.5834(5) 0.8760(8) 0.096(3) Uani 1 1 d . . . . . H47 H 0.941963 0.583407 0.945672 0.115 Uiso 1 1 calc R U . . . C48 C 0.8899(4) 0.5831(6) 0.8154(9) 0.099(3) Uani 1 1 d . . . . . H48 H 0.846170 0.583258 0.844836 0.118 Uiso 1 1 calc R U . . . C49 C 1.1913(5) 0.5963(8) 0.9233(9) 0.125(5) Uani 1 1 d . . . . . H49 H 1.235141 0.600358 0.895020 0.150 Uiso 1 1 calc R U . . . C50 C 1.1373(5) 0.5930(9) 0.8594(9) 0.134(5) Uani 1 1 d . . . . . H50 H 1.144009 0.593522 0.789963 0.161 Uiso 1 1 calc R U . . . C51 C 1.0719(4) 0.5890(5) 0.8999(8) 0.082(3) Uani 1 1 d . . . . . C52 C 1.0677(5) 0.5858(7) 1.0007(9) 0.123(5) Uani 1 1 d . . . . . H52 H 1.024720 0.581710 1.031834 0.147 Uiso 1 1 calc R U . . . C53 C 1.1262(7) 0.5886(9) 1.0573(10) 0.138(5) Uani 1 1 d . . . . . H53 H 1.122177 0.586421 1.127114 0.166 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 0.0639(7) 0.1375(12) 0.1195(10) -0.0014(10) -0.0532(7) 0.0008(7) O1 0.093(8) 0.217(12) 0.196(12) -0.009(10) -0.058(8) 0.012(8) O2 0.081(7) 0.200(11) 0.181(11) -0.029(9) -0.065(8) 0.012(7) C1 0.086(7) 0.207(11) 0.186(11) -0.026(9) -0.065(8) 0.012(8) O1A 0.069(8) 0.210(12) 0.181(12) -0.030(11) -0.068(8) 0.006(9) O2A 0.094(9) 0.212(12) 0.189(13) -0.022(10) -0.059(9) 0.015(9) C1A 0.080(7) 0.211(11) 0.188(11) -0.022(10) -0.064(8) 0.011(8) O3 0.119(10) 0.211(14) 0.156(11) -0.023(11) -0.099(9) 0.044(9) O4 0.129(10) 0.162(13) 0.123(10) -0.006(9) -0.097(8) 0.008(9) C2 0.133(11) 0.190(14) 0.139(12) -0.010(11) -0.088(10) 0.026(10) O3A 0.107(11) 0.211(16) 0.164(13) -0.026(12) -0.095(10) 0.053(11) O4A 0.146(15) 0.23(2) 0.161(15) -0.005(15) -0.082(13) 0.028(14) C2A 0.121(13) 0.216(17) 0.165(14) -0.031(13) -0.091(11) 0.038(12) O5 0.202(9) 0.206(10) 0.178(10) -0.035(8) -0.053(8) 0.064(8) O6 0.118(7) 0.166(10) 0.219(10) -0.023(9) -0.019(8) 0.048(7) O7 0.145(7) 0.122(7) 0.176(9) 0.008(7) -0.056(7) -0.008(6) O8 0.072(5) 0.101(6) 0.231(12) -0.004(7) -0.052(6) 0.000(4) N1 0.053(4) 0.110(6) 0.105(6) 0.001(6) -0.024(4) 0.008(4) N2 0.057(4) 0.142(8) 0.102(6) -0.008(6) -0.031(4) 0.011(5) C3 0.053(4) 0.098(7) 0.096(7) -0.001(6) -0.028(4) 0.012(4) C4 0.043(4) 0.088(6) 0.091(5) 0.009(5) -0.024(4) -0.009(4) C5 0.047(4) 0.068(5) 0.096(6) 0.013(5) -0.032(4) -0.013(4) C6 0.058(5) 0.106(8) 0.097(7) -0.001(6) -0.025(5) 0.000(5) C7 0.085(7) 0.150(11) 0.082(6) 0.001(7) -0.029(5) 0.011(7) C8 0.043(4) 0.067(5) 0.085(6) 0.003(4) -0.029(4) -0.007(3) C9 0.041(4) 0.128(9) 0.084(6) 0.029(6) -0.020(4) -0.008(5) C10 0.050(4) 0.114(8) 0.085(6) 0.003(6) -0.023(4) -0.006(4) C11 0.044(4) 0.075(6) 0.111(7) -0.004(5) -0.036(4) 0.004(4) C12 0.043(4) 0.102(7) 0.105(7) -0.016(6) -0.026(4) 0.016(4) C13 0.050(4) 0.097(7) 0.083(6) -0.012(5) -0.020(4) 0.002(4) C14 0.048(4) 0.069(6) 0.132(7) -0.017(5) -0.048(5) 0.014(4) C15 0.084(6) 0.065(6) 0.154(9) -0.013(6) -0.074(6) 0.009(4) C16 0.073(5) 0.053(5) 0.155(9) -0.003(6) -0.064(6) 0.005(4) C17 0.051(4) 0.078(6) 0.116(7) 0.002(6) -0.045(4) 0.001(4) C18 0.041(4) 0.077(6) 0.120(8) -0.008(5) -0.034(4) 0.001(3) C19 0.056(4) 0.066(5) 0.122(8) -0.010(5) -0.042(5) 0.011(4) C20 0.045(4) 0.067(5) 0.126(7) -0.011(5) -0.018(4) 0.006(4) C21 0.070(5) 0.066(6) 0.123(9) -0.018(6) -0.016(6) -0.001(4) C22 0.051(4) 0.058(5) 0.161(10) -0.006(6) -0.039(5) -0.001(4) C23 0.061(5) 0.072(7) 0.156(11) 0.001(7) -0.031(7) 0.002(4) C24 0.082(7) 0.044(5) 0.215(16) 0.007(8) 0.005(10) -0.005(4) C25 0.094(8) 0.073(7) 0.138(10) 0.011(7) -0.002(7) -0.005(6) C26 0.108(8) 0.069(6) 0.169(11) 0.000(7) -0.058(8) -0.001(5) C27 0.22(2) 0.21(2) 0.19(2) -0.056(19) 0.01(2) 0.017(18) C28 0.24(3) 0.29(3) 0.25(3) -0.09(2) -0.09(2) -0.04(2) C29 0.121(11) 0.110(10) 0.159(14) -0.014(10) -0.028(10) -0.021(8) C30 0.176(17) 0.168(16) 0.28(2) -0.035(16) -0.143(18) -0.012(13) C31 0.100(7) 0.094(7) 0.179(9) -0.011(7) -0.073(7) 0.006(6) C34 0.062(6) 0.104(8) 0.202(15) 0.013(9) -0.018(7) 0.017(6) C33 0.072(6) 0.115(9) 0.174(12) -0.016(9) -0.015(8) 0.014(6) C32 0.081(7) 0.082(7) 0.186(12) 0.003(9) -0.075(8) 0.001(6) C37 0.106(9) 0.137(13) 0.157(12) 0.047(11) -0.031(9) -0.025(9) C36 0.186(11) 0.186(12) 0.168(12) -0.034(10) -0.070(10) 0.047(10) C35 0.086(7) 0.084(8) 0.190(14) -0.010(9) -0.042(8) -0.004(6) C38 0.222(11) 0.222(12) 0.191(12) -0.026(11) -0.039(11) 0.061(10) C39 0.263(18) 0.256(19) 0.229(18) -0.021(17) -0.044(17) 0.060(17) C40 0.182(12) 0.200(13) 0.267(14) -0.022(13) -0.021(13) 0.043(10) C41 0.227(15) 0.219(15) 0.295(18) -0.033(16) -0.011(16) 0.052(13) C42 0.075(7) 0.075(7) 0.27(2) -0.014(10) -0.024(9) 0.005(5) C43 0.051(4) 0.062(5) 0.120(8) -0.011(5) -0.046(5) -0.002(4) C44 0.073(5) 0.069(6) 0.119(7) -0.010(5) -0.054(5) 0.002(4) C45 0.060(4) 0.060(5) 0.118(7) -0.009(5) -0.049(5) 0.007(4) C46 0.051(4) 0.086(6) 0.108(7) -0.003(6) -0.042(4) 0.003(4) C47 0.069(6) 0.113(8) 0.105(7) 0.002(7) -0.036(5) 0.003(5) C48 0.046(4) 0.127(9) 0.123(9) -0.011(7) -0.034(5) 0.005(5) C49 0.055(5) 0.213(15) 0.107(9) -0.002(10) -0.031(5) 0.002(7) C50 0.064(6) 0.228(16) 0.111(8) -0.015(10) -0.035(6) 0.006(8) C51 0.050(4) 0.093(7) 0.103(7) -0.008(6) -0.032(4) 0.016(4) C52 0.054(5) 0.194(14) 0.120(9) 0.009(10) -0.040(5) -0.001(7) C53 0.096(8) 0.213(16) 0.106(8) -0.017(10) -0.050(7) 0.015(9) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O2 Cu1 O3 164.6(8) . . ? O2 Cu1 O4 106.7(8) . . ? O1A Cu1 C1A 29.7(6) . . ? O4 Cu1 O3 57.9(4) . . ? O3A Cu1 O1A 65.1(11) . . ? O3A Cu1 C1A 93.8(11) . . ? N1 Cu1 O2 88.2(4) . . ? N1 Cu1 O1A 89.4(5) . . ? N1 Cu1 C1A 95.9(10) . . ? N1 Cu1 O3 91.0(5) . . ? N1 Cu1 O4 88.5(4) . . ? N1 Cu1 O3A 93.0(5) . . ? N2 Cu1 O2 88.8(5) 1_454 . ? N2 Cu1 O1A 91.8(6) 1_454 . ? N2 Cu1 C1A 83.7(11) 1_454 . ? N2 Cu1 O3 91.5(5) 1_454 . ? N2 Cu1 O4 90.8(4) 1_454 . ? N2 Cu1 O3A 90.4(5) 1_454 . ? N2 Cu1 N1 176.6(4) 1_454 . ? C1 O2 Cu1 99.1(15) . . ? O1 C1 H1 118.2 . . ? O2 C1 O1 123.5(18) . . ? O2 C1 H1 118.2 . . ? C1A O1A Cu1 95(3) . . ? Cu1 C1A H1A 141.2 . . ? O1A C1A Cu1 56(2) . . ? O1A C1A H1A 120.0 . . ? O2A C1A Cu1 78(2) . . ? O2A C1A O1A 120.0(18) . . ? O2A C1A H1A 120.0 . . ? C2 O3 Cu1 87.5(12) . . ? C2 O4 Cu1 90.3(12) . . ? O3 C2 O4 123.4(18) . . ? O3 C2 H2 118.3 . . ? O4 C2 H2 118.3 . . ? C2A O3A Cu1 118.3(18) . . ? O3A C2A O4A 126(2) . . ? O3A C2A H2A 117.0 . . ? O4A C2A H2A 117.0 . . ? C38 O5 C36 112.2(15) . . ? C33 O6 C40 107.7(12) . . ? C27 O7 C26 123.1(16) . . ? C29 O8 C23 120.4(10) . . ? C3 N1 Cu1 123.5(6) . . ? C7 N1 Cu1 120.9(7) . . ? C7 N1 C3 115.5(7) . . ? C49 N2 Cu1 123.0(7) . 1_656 ? C49 N2 C53 116.8(8) . . ? C53 N2 Cu1 120.1(7) . 1_656 ? N1 C3 H3 117.5 . . ? N1 C3 C4 125.0(9) . . ? C4 C3 H3 117.5 . . ? C3 C4 H4 120.8 . . ? C3 C4 C5 118.5(9) . . ? C5 C4 H4 120.8 . . ? C4 C5 C8 121.0(8) . . ? C6 C5 C4 115.8(7) . . ? C6 C5 C8 123.2(8) . . ? C5 C6 H6 119.4 . . ? C5 C6 C7 121.2(10) . . ? C7 C6 H6 119.4 . . ? N1 C7 C6 124.0(10) . . ? N1 C7 H7 118.0 . . ? C6 C7 H7 118.0 . . ? C9 C8 C5 122.3(8) . . ? C9 C8 C13 117.3(7) . . ? C13 C8 C5 120.4(8) . . ? C8 C9 H9 118.8 . . ? C8 C9 C10 122.3(8) . . ? C10 C9 H9 118.8 . . ? C9 C10 H10 119.9 . . ? C9 C10 C11 120.1(9) . . ? C11 C10 H10 119.9 . . ? C10 C11 C14 120.1(9) . . ? C12 C11 C10 117.8(7) . . ? C12 C11 C14 121.8(8) . . ? C11 C12 H12 119.8 . . ? C11 C12 C13 120.4(8) . . ? C13 C12 H12 119.8 . . ? C8 C13 H13 119.0 . . ? C12 C13 C8 121.9(9) . . ? C12 C13 H13 119.0 . . ? C15 C14 C11 120.1(8) . . ? C19 C14 C11 119.4(7) . . ? C19 C14 C15 120.5(6) . . ? C14 C15 C31 119.2(7) . . ? C16 C15 C14 116.5(8) . . ? C16 C15 C31 124.1(8) . . ? C15 C16 H16 117.7 . . ? C15 C16 C17 124.6(8) . . ? C17 C16 H16 117.7 . . ? C16 C17 C18 119.6(6) . . ? C16 C17 C43 119.9(7) . . ? C18 C17 C43 120.5(8) . . ? C17 C18 C19 115.5(7) . . ? C17 C18 C20 123.8(7) . . ? C19 C18 C20 120.7(7) . . ? C14 C19 C18 123.3(7) . . ? C14 C19 H19 118.4 . . ? C18 C19 H19 118.4 . . ? C18 C20 H20A 108.6 . . ? C18 C20 H20B 108.6 . . ? H20A C20 H20B 107.6 . . ? C21 C20 C18 114.8(8) . . ? C21 C20 H20A 108.6 . . ? C21 C20 H20B 108.6 . . ? C22 C21 C20 123.4(12) . . ? C26 C21 C20 118.9(10) . . ? C26 C21 C22 117.7(11) . . ? C21 C22 H22 120.8 . . ? C21 C22 C23 118.5(12) . . ? C23 C22 H22 120.8 . . ? C22 C23 O8 117.0(14) . . ? C24 C23 O8 120.3(12) . . ? C24 C23 C22 122.7(11) . . ? C23 C24 C25 121.3(12) . . ? C23 C24 C42 120.6(15) . 2_765 ? C25 C24 C42 118.1(17) . 2_765 ? C24 C25 H25 121.4 . . ? C24 C25 C26 117.1(14) . . ? C26 C25 H25 121.4 . . ? O7 C26 C25 118.0(15) . . ? C21 C26 O7 119.6(13) . . ? C21 C26 C25 122.3(11) . . ? O7 C27 H27A 108.7 . . ? O7 C27 H27B 108.7 . . ? O7 C27 C28 114(2) . . ? H27A C27 H27B 107.6 . . ? C28 C27 H27A 108.7 . . ? C28 C27 H27B 108.7 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28B 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? O8 C29 H29A 110.8 . . ? O8 C29 H29B 110.8 . . ? O8 C29 C30 104.9(15) . . ? H29A C29 H29B 108.8 . . ? C30 C29 H29A 110.8 . . ? C30 C29 H29B 110.8 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30B 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C15 C31 H31A 108.0 . . ? C15 C31 H31B 108.0 . . ? C15 C31 C32 117.4(8) . . ? H31A C31 H31B 107.2 . . ? C32 C31 H31A 108.0 . . ? C32 C31 H31B 108.0 . . ? C33 C34 H34 120.0 . . ? C33 C34 C35 120.0 . . ? C35 C34 H34 120.0 . . ? C34 C33 O6 124.6(9) . . ? C32 C33 O6 115.3(9) . . ? C32 C33 C34 120.0 . . ? C33 C32 C31 125.0(10) . . ? C33 C32 C37 120.0 . . ? C37 C32 C31 115.0(10) . . ? C32 C37 H37 120.0 . . ? C36 C37 C32 120.0 . . ? C36 C37 H37 120.0 . . ? O5 C36 C37 128.1(10) . . ? O5 C36 C35 110.9(10) . . ? C37 C36 C35 120.0 . . ? C34 C35 C42 121.1(11) . . ? C36 C35 C34 120.0 . . ? C36 C35 C42 118.9(11) . . ? O5 C38 H38A 110.9 . . ? O5 C38 H38B 110.9 . . ? O5 C38 C39 104(2) . . ? H38A C38 H38B 108.9 . . ? C39 C38 H38A 110.9 . . ? C39 C38 H38B 110.9 . . ? C38 C39 H39A 109.5 . . ? C38 C39 H39B 109.5 . . ? C38 C39 H39C 109.5 . . ? H39A C39 H39B 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? O6 C40 H40A 109.9 . . ? O6 C40 H40B 109.9 . . ? H40A C40 H40B 108.3 . . ? C41 C40 O6 108.8(16) . . ? C41 C40 H40A 109.9 . . ? C41 C40 H40B 109.9 . . ? C40 C41 H41A 109.4 . . ? C40 C41 H41B 110.4 . . ? C40 C41 H41C 108.7 . . ? H41A C41 H41B 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C24 C42 H42A 108.8 2_765 . ? C24 C42 H42B 108.8 2_765 . ? C35 C42 C24 113.9(8) . 2_765 ? C35 C42 H42A 108.8 . . ? C35 C42 H42B 108.8 . . ? H42A C42 H42B 107.7 . . ? C44 C43 C17 120.5(9) . . ? C48 C43 C17 121.1(9) . . ? C48 C43 C44 118.3(7) . . ? C43 C44 H44 118.7 . . ? C43 C44 C45 122.5(10) . . ? C45 C44 H44 118.7 . . ? C44 C45 H45 121.1 . . ? C44 C45 C46 117.8(9) . . ? C46 C45 H45 121.1 . . ? C45 C46 C51 120.1(8) . . ? C47 C46 C45 119.4(7) . . ? C47 C46 C51 120.4(9) . . ? C46 C47 H47 119.8 . . ? C46 C47 C48 120.3(10) . . ? C48 C47 H47 119.8 . . ? C43 C48 C47 121.6(10) . . ? C43 C48 H48 119.2 . . ? C47 C48 H48 119.2 . . ? N2 C49 H49 117.1 . . ? N2 C49 C50 125.7(11) . . ? C50 C49 H49 117.1 . . ? C49 C50 H50 121.0 . . ? C49 C50 C51 117.9(11) . . ? C51 C50 H50 121.0 . . ? C50 C51 C46 121.3(9) . . ? C52 C51 C46 122.0(9) . . ? C52 C51 C50 116.6(8) . . ? C51 C52 H52 120.0 . . ? C51 C52 C53 119.9(11) . . ? C53 C52 H52 120.0 . . ? N2 C53 C52 122.9(12) . . ? N2 C53 H53 118.6 . . ? C52 C53 H53 118.6 . . ? 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 O2 2.017(19) . ? Cu1 O1A 2.11(3) . ? Cu1 C1A 2.55(4) . ? Cu1 O3 2.30(2) . ? Cu1 O4 2.241(17) . ? Cu1 O3A 2.04(3) . ? Cu1 N1 2.004(7) . ? Cu1 N2 2.000(7) 1_454 ? O1 C1 1.261(12) . ? O2 C1 1.260(12) . ? C1 H1 0.9500 . ? O1A C1A 1.269(13) . ? O2A C1A 1.267(13) . ? C1A H1A 0.9500 . ? O3 C2 1.247(12) . ? O4 C2 1.252(12) . ? C2 H2 0.9500 . ? O3A C2A 1.234(13) . ? O4A C2A 1.247(13) . ? C2A H2A 0.9500 . ? O5 C36 1.380(16) . ? O5 C38 1.34(2) . ? O6 C33 1.426(13) . ? O6 C40 1.51(2) . ? O7 C26 1.389(15) . ? O7 C27 1.39(2) . ? O8 C23 1.439(15) . ? O8 C29 1.439(19) . ? N1 C3 1.323(12) . ? N1 C7 1.317(14) . ? N2 C49 1.291(14) . ? N2 C53 1.327(16) . ? C3 H3 0.9500 . ? C3 C4 1.351(10) . ? C4 H4 0.9500 . ? C4 C5 1.416(12) . ? C5 C6 1.345(13) . ? C5 C8 1.496(9) . ? C6 H6 0.9500 . ? C6 C7 1.356(12) . ? C7 H7 0.9500 . ? C8 C9 1.360(12) . ? C8 C13 1.387(12) . ? C9 H9 0.9500 . ? C9 C10 1.380(10) . ? C10 H10 0.9500 . ? C10 C11 1.405(13) . ? C11 C12 1.380(14) . ? C11 C14 1.487(10) . ? C12 H12 0.9500 . ? C12 C13 1.382(10) . ? C13 H13 0.9500 . ? C14 C15 1.411(12) . ? C14 C19 1.335(12) . ? C15 C16 1.371(11) . ? C15 C31 1.512(14) . ? C16 H16 0.9500 . ? C16 C17 1.375(12) . ? C17 C18 1.398(12) . ? C17 C43 1.499(9) . ? C18 C19 1.446(11) . ? C18 C20 1.501(12) . ? C19 H19 0.9500 . ? C20 H20A 0.9900 . ? C20 H20B 0.9900 . ? C20 C21 1.499(13) . ? C21 C22 1.373(14) . ? C21 C26 1.357(19) . ? C22 H22 0.9500 . ? C22 C23 1.413(16) . ? C23 C24 1.33(2) . ? C24 C25 1.32(2) . ? C24 C42 1.594(16) 2_765 ? C25 H25 0.9500 . ? C25 C26 1.462(19) . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C27 C28 1.47(3) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C29 C30 1.482(19) . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9900 . ? C31 H31B 0.9900 . ? C31 C32 1.521(12) . ? C34 H34 0.9500 . ? C34 C33 1.3900 . ? C34 C35 1.3900 . ? C33 C32 1.3900 . ? C32 C37 1.3900 . ? C37 H37 0.9500 . ? C37 C36 1.3900 . ? C36 C35 1.3900 . ? C35 C42 1.528(10) . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C38 C39 1.61(3) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C40 C41 1.480(13) . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9900 . ? C42 H42B 0.9900 . ? C43 C44 1.379(14) . ? C43 C48 1.359(15) . ? C44 H44 0.9500 . ? C44 C45 1.389(10) . ? C45 H45 0.9500 . ? C45 C46 1.428(15) . ? C46 C47 1.366(14) . ? C46 C51 1.495(10) . ? C47 H47 0.9500 . ? C47 C48 1.396(11) . ? C48 H48 0.9500 . ? C49 H49 0.9500 . ? C49 C50 1.374(13) . ? C50 H50 0.9500 . ? C50 C51 1.405(15) . ? C51 C52 1.371(16) . ? C52 H52 0.9500 . ? C52 C53 1.388(13) . ? C53 H53 0.9500 . ? 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 Cu1 O2 C1 O1 -32(3) . . . . ? Cu1 O1A C1A O2A 46(6) . . . . ? Cu1 O3 C2 O4 -9(2) . . . . ? Cu1 O4 C2 O3 10(2) . . . . ? Cu1 O3A C2A O4A -4(5) . . . . ? Cu1 N1 C3 C4 175.2(8) . . . . ? Cu1 N1 C7 C6 -175.9(9) . . . . ? Cu1 N2 C49 C50 179.3(13) 1_656 . . . ? Cu1 N2 C53 C52 179.7(13) 1_656 . . . ? O5 C36 C35 C34 -169.8(11) . . . . ? O5 C36 C35 C42 7.7(11) . . . . ? O6 C33 C32 C31 0.4(10) . . . . ? O6 C33 C32 C37 177.2(9) . . . . ? O8 C23 C24 C25 179.7(10) . . . . ? O8 C23 C24 C42 -0.2(16) . . . 2_765 ? N1 C3 C4 C5 0.5(16) . . . . ? N2 C49 C50 C51 2(3) . . . . ? C3 N1 C7 C6 0.9(18) . . . . ? C3 C4 C5 C6 1.0(13) . . . . ? C3 C4 C5 C8 -178.9(8) . . . . ? C4 C5 C6 C7 -1.6(15) . . . . ? C4 C5 C8 C9 15.6(14) . . . . ? C4 C5 C8 C13 -165.0(8) . . . . ? C5 C6 C7 N1 0.6(19) . . . . ? C5 C8 C9 C10 -177.2(9) . . . . ? C5 C8 C13 C12 177.4(9) . . . . ? C6 C5 C8 C9 -164.3(10) . . . . ? C6 C5 C8 C13 15.1(13) . . . . ? C7 N1 C3 C4 -1.5(17) . . . . ? C8 C5 C6 C7 178.3(10) . . . . ? C8 C9 C10 C11 -2.6(16) . . . . ? C9 C8 C13 C12 -3.2(14) . . . . ? C9 C10 C11 C12 1.4(15) . . . . ? C9 C10 C11 C14 175.5(9) . . . . ? C10 C11 C12 C13 -1.2(15) . . . . ? C10 C11 C14 C15 103.8(13) . . . . ? C10 C11 C14 C19 -76.4(13) . . . . ? C11 C12 C13 C8 2.2(15) . . . . ? C11 C14 C15 C16 178.9(10) . . . . ? C11 C14 C15 C31 4.1(18) . . . . ? C11 C14 C19 C18 -178.5(10) . . . . ? C12 C11 C14 C15 -82.4(14) . . . . ? C12 C11 C14 C19 97.4(12) . . . . ? C13 C8 C9 C10 3.4(16) . . . . ? C14 C11 C12 C13 -175.2(8) . . . . ? C14 C15 C16 C17 0(2) . . . . ? C14 C15 C31 C32 179.5(12) . . . . ? C15 C14 C19 C18 1.3(17) . . . . ? C15 C16 C17 C18 0.1(19) . . . . ? C15 C16 C17 C43 177.2(12) . . . . ? C15 C31 C32 C33 69.6(14) . . . . ? C15 C31 C32 C37 -107.3(12) . . . . ? C16 C15 C31 C32 5(2) . . . . ? C16 C17 C18 C19 0.3(15) . . . . ? C16 C17 C18 C20 179.9(11) . . . . ? C16 C17 C43 C44 81.7(13) . . . . ? C16 C17 C43 C48 -97.5(13) . . . . ? C17 C18 C19 C14 -1.0(16) . . . . ? C17 C18 C20 C21 51.9(15) . . . . ? C17 C43 C44 C45 179.1(8) . . . . ? C17 C43 C48 C47 -179.9(9) . . . . ? C18 C17 C43 C44 -101.2(11) . . . . ? C18 C17 C43 C48 79.6(14) . . . . ? C18 C20 C21 C22 -123.0(11) . . . . ? C18 C20 C21 C26 60.5(14) . . . . ? C19 C14 C15 C16 -0.9(18) . . . . ? C19 C14 C15 C31 -175.7(12) . . . . ? C19 C18 C20 C21 -128.5(11) . . . . ? C20 C18 C19 C14 179.3(10) . . . . ? C20 C21 C22 C23 175.2(9) . . . . ? C20 C21 C26 O7 5.8(17) . . . . ? C20 C21 C26 C25 -178.1(9) . . . . ? C21 C22 C23 O8 -174.9(9) . . . . ? C21 C22 C23 C24 7.3(16) . . . . ? C22 C21 C26 O7 -171.0(10) . . . . ? C22 C21 C26 C25 5.2(18) . . . . ? C22 C23 C24 C25 -2.6(18) . . . . ? C22 C23 C24 C42 177.6(8) . . . 2_765 ? C23 O8 C29 C30 -177.0(12) . . . . ? C23 C24 C25 C26 -0.8(17) . . . . ? C24 C25 C26 O7 175.7(11) . . . . ? C24 C25 C26 C21 -0.5(18) . . . . ? C26 O7 C27 C28 170.0(19) . . . . ? C26 C21 C22 C23 -8.2(15) . . . . ? C27 O7 C26 C21 -140.3(19) . . . . ? C27 O7 C26 C25 43(2) . . . . ? C29 O8 C23 C22 -2.5(16) . . . . ? C29 O8 C23 C24 175.3(12) . . . . ? C31 C15 C16 C17 174.7(13) . . . . ? C31 C32 C37 C36 177.1(7) . . . . ? C34 C33 C32 C31 -176.8(8) . . . . ? C34 C33 C32 C37 0.0 . . . . ? C34 C35 C42 C24 -96.4(15) . . . 2_765 ? C33 O6 C40 C41 156.4(17) . . . . ? C33 C34 C35 C36 0.0 . . . . ? C33 C34 C35 C42 -177.4(8) . . . . ? C33 C32 C37 C36 0.0 . . . . ? C32 C37 C36 O5 167.8(13) . . . . ? C32 C37 C36 C35 0.0 . . . . ? C37 C36 C35 C34 0.0 . . . . ? C37 C36 C35 C42 177.5(8) . . . . ? C36 O5 C38 C39 -166.5(18) . . . . ? C36 C35 C42 C24 86.2(16) . . . 2_765 ? C35 C34 C33 O6 -176.9(10) . . . . ? C35 C34 C33 C32 0.0 . . . . ? C38 O5 C36 C37 -9(2) . . . . ? C38 O5 C36 C35 160.2(18) . . . . ? C40 O6 C33 C34 -65.6(13) . . . . ? C40 O6 C33 C32 117.3(11) . . . . ? C42 C24 C25 C26 179.1(9) 2_765 . . . ? C43 C17 C18 C19 -176.8(10) . . . . ? C43 C17 C18 C20 2.8(16) . . . . ? C43 C44 C45 C46 1.0(13) . . . . ? C44 C43 C48 C47 0.9(16) . . . . ? C44 C45 C46 C47 0.5(14) . . . . ? C44 C45 C46 C51 -175.9(8) . . . . ? C45 C46 C47 C48 -1.2(15) . . . . ? C45 C46 C51 C50 0.2(16) . . . . ? C45 C46 C51 C52 -175.1(11) . . . . ? C46 C47 C48 C43 0.5(17) . . . . ? C46 C51 C52 C53 177.5(13) . . . . ? C47 C46 C51 C50 -176.2(12) . . . . ? C47 C46 C51 C52 8.5(16) . . . . ? C48 C43 C44 C45 -1.7(14) . . . . ? C49 N2 C53 C52 -1(2) . . . . ? C49 C50 C51 C46 -178.3(13) . . . . ? C49 C50 C51 C52 -3(2) . . . . ? C50 C51 C52 C53 2(2) . . . . ? C51 C46 C47 C48 175.2(10) . . . . ? C51 C52 C53 N2 0(3) . . . . ? C53 N2 C49 C50 0(3) . . . . ? loop_ _twin_individual_id _twin_individual_mass_fraction_refined 1 0.83(4) 2 0.17(4) loop_ _smtbx_masks_void_nr _smtbx_masks_void_average_x _smtbx_masks_void_average_y _smtbx_masks_void_average_z _smtbx_masks_void_volume _smtbx_masks_void_count_electrons _smtbx_masks_void_content 1 -0.058 -0.834 0.000 1599.3 170.6 '4 DMF'