#------------------------------------------------------------------------------ #$Date: 2024-07-09 01:18:42 +0300 (Tue, 09 Jul 2024) $ #$Revision: 293306 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/20/1572095.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_1572095 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_formula_moiety '4(I), C102 H104 Cu2 N4 O12, 4[C3H7NO], 2[H2O]' _chemical_formula_sum 'C114 H136 Cu2 I4 N8 O18' _chemical_formula_weight 2540.98 _space_group_crystal_system orthorhombic _space_group_IT_number 48 _space_group_name_Hall '-P 2ab 2bc' _space_group_name_H-M_alt 'P n n n :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 4 _cell_length_a 13.7025(3) _cell_length_b 22.6702(5) _cell_length_c 41.6085(10) _cell_measurement_reflns_used 6346 _cell_measurement_temperature 193.00 _cell_measurement_theta_max 62.25 _cell_measurement_theta_min 3.40 _cell_volume 12925.2(5) _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 (Sheldrick, 2015)' _diffrn_ambient_temperature 193.00 _diffrn_detector CPAD _diffrn_detector_area_resol_mean 7.41 _diffrn_detector_type 'Bruker PHOTON III' _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Bruker D8 VENTURE dual wavelength Mo/Cu' _diffrn_measurement_method '\w and \f scans' _diffrn_radiation_monochromator 'Helios Multi-layer Optic' _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.1172 _diffrn_reflns_av_unetI/netI 0.0900 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_k_max 26 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_l_max 46 _diffrn_reflns_limit_l_min -50 _diffrn_reflns_number 88773 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.998 _diffrn_reflns_theta_full 67.679 _diffrn_reflns_theta_max 68.544 _diffrn_reflns_theta_min 2.219 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_current 1.0 _diffrn_source_power 0.05 _diffrn_source_type 'Incoatec I\ms DIAMOND' _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 8.385 _exptl_absorpt_correction_T_max 0.7531 _exptl_absorpt_correction_T_min 0.2906 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1442 before and 0.0777 after correction. The Ratio of minimum to maximum transmission is 0.3859. The \l/2 correction factor is Not present. ; _exptl_crystal_colour brown _exptl_crystal_colour_primary brown _exptl_crystal_density_diffrn 1.306 _exptl_crystal_description block _exptl_crystal_F_000 5160 _exptl_crystal_size_max 0.12 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.09 _refine_diff_density_max 1.290 _refine_diff_density_min -0.721 _refine_diff_density_rms 0.113 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 690 _refine_ls_number_reflns 11909 _refine_ls_number_restraints 274 _refine_ls_restrained_S_all 1.177 _refine_ls_R_factor_all 0.1716 _refine_ls_R_factor_gt 0.1319 _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^)+(0.0700P)^2^+60.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.3146 _refine_ls_wR_factor_ref 0.3384 _reflns_Friedel_coverage 0.000 _reflns_number_gt 7024 _reflns_number_total 11909 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4sc03022b2.cif _cod_data_source_block cu_231121lu_lgpz184505_1_0m _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_original_sg_symbol_H-M 'P n n n' _cod_database_code 1572095 _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 0.519 _shelx_estimated_absorpt_t_min 0.433 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All C(H,H,H) groups, All O(H,H) groups 2. Restrained distances C2A-C3 = C1A-C2A = N1-C1A = N1-C5A = C4A-C5A = C4A-C3 1.39 with sigma of 0.01 Cu1-O6B \\sim Cu1-O6 \\sim Cu1-O6A \\sim Cu1-O5A \\sim Cu1-O5 with sigma of 0.02 3. Restrained planarity N1, C1A, C2A, C3, C4A, C5A with sigma of 0.005 4. Uiso/Uaniso restraints and constraints N1 \\sim C1 \\sim C1A \\sim C2 \\sim C2A \\sim C3 \\sim C4 \\sim C4A \\sim C5 \\sim C5A: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A O5 \\sim O5A \\sim O6 \\sim O6A \\sim O6B: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A N2 \\sim C47 \\sim C48 \\sim C49 \\sim C50 \\sim C51: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A Uanis(O5) \\sim Ueq, Uanis(O5A) \\sim Ueq, Uanis(O6B) \\sim Ueq, Uanis(O6) \\sim Ueq, Uanis(O6A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(I1) \\sim Ueq, Uanis(I2) \\sim Ueq, Uanis(I3) \\sim Ueq, Uanis(I4) \\sim Ueq, Uanis(I5) \\sim Ueq, Uanis(I6) \\sim Ueq, Uanis(I7) \\sim Ueq, Uanis(I8) \\sim Ueq, Uanis(I9) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(O5) \\sim Ueq: with sigma of 0.005 and sigma for terminal atoms of 0.01 5. Others 1*[Sof(O6)+Sof(H6A)+Sof(H6B)]+1*[Sof(O6B)+Sof(H6BA)+Sof(H6BB)]+1*[Sof(O6A)+ Sof(H6AA)+Sof(H6AB)]=1 with esd of 0 1*[Sof(I1)+Sof(O5)+Sof(H5A)+Sof(H5B)+Sof(O5A)+Sof(H5AA)+Sof(H5AB)]+1* [Sof(I7)]+1*[Sof(I6)]+1*[Sof(I5)]=1 with esd of 0 1*[Sof(I8)]+1*[Sof(I4)]+1*[Sof(I2)]+1*[Sof(I3)]+1*[Sof(I9)]=1 with esd of 0 Sof(C1A)=Sof(H1A)=Sof(C2A)=Sof(H2A)=Sof(C4A)=Sof(H4A)=Sof(C5A)=Sof(H5AC)=1- FVAR(1) Sof(C1)=Sof(H1)=Sof(C2)=Sof(H2)=Sof(C4)=Sof(H4)=Sof(C5)=Sof(H5)=FVAR(1) Sof(O6)=Sof(H6A)=Sof(H6B)=FVAR(2) Sof(O6B)=Sof(H6BA)=Sof(H6BB)=FVAR(3) Sof(O6A)=Sof(H6AA)=Sof(H6AB)=FVAR(4) Sof(O5A)=Sof(H5AA)=Sof(H5AB)=1-FVAR(5) Sof(I1)=Sof(O5)=Sof(H5A)=Sof(H5B)=FVAR(5) 6.a Riding coordinates: O5(H5A,H5B), O5A(H5AA,H5AB), O6(H6A,H6B), O6A(H6AA,H6AB), O6B(H6BA,H6BB) 6.b Secondary CH2 refined with riding coordinates: C18(H18A,H18B), C25(H25A,H25B), C27(H27A,H27B), C29(H29A,H29B), C36(H36A, H36B), C38(H38A,H38B), C40(H40A,H40B) 6.c Aromatic/amide H refined with riding coordinates: C1(H1), C1A(H1A), C2(H2), C2A(H2A), C4(H4), C4A(H4A), C5(H5), C5A(H5AC), C7(H7), C8(H8), C10(H10), C11(H11), C13(H13), C16(H16), C20(H20), C23(H23), C32(H32), C35(H35), C42(H42), C43(H43), C45(H45), C46(H46), C50(H50), C51(H51), C47(H47), C48(H48) 6.d Fitted hexagon refined as free rotating group: C49(C50,C51,N2,C47,C48) 6.e Idealised Me refined as rotating group: C26(H26A,H26B,H26C), C28(H28A,H28B,H28C), C37(H37A,H37B,H37C), C39(H39A,H39B, H39C) ; _smtbx_masks_special_details ; A solvent mask was calculated and 710 electrons were found in a volume of 2406\%A^3^ in 1 void per unit cell. This is consistent with the presence of 4[C3H7NO], 2[H2O] per formula unit which account for 720 electrons per unit cell. ; _smtbx_masks_void_probe_radius 1.2 _smtbx_masks_void_truncation_radius 1.2 _shelx_res_file ; TITL cu_231121lu_lgpz184505_1_0m_a.res in Pnnn cu_231121lu_lgpz184505_1_0m.res created by SHELXL-2019/3 at 20:53:01 on 18-Jun-2024 REM Old TITL cu_231121LU_LGPZ184505_1_0m in Pnnn REM SHELXT solution in Pnnn: R1 0.444, Rweak 0.068, Alpha 0.084 REM 0.913 for 659 systematic absences, Orientation as input REM Formula found by SHELXT: C194 N38 O33 Cu4 CELL 1.54178 13.7025 22.6702 41.6085 90 90 90 ZERR 4 0.0003 0.0005 0.001 0 0 0 LATT 1 SYMM 0.5-X,0.5-Y,+Z SYMM 0.5-X,+Y,0.5-Z SYMM +X,0.5-Y,0.5-Z SFAC C H Cu I N O UNIT 456 544 8 16 32 72 SADI Cu1 O6B Cu1 O6 Cu1 O6A Cu1 O5A Cu1 O5 ISOR 0.01 0.02 O5 O5A O6B O6 O6A ISOR 0.01 0.02 I1 > I9 SIMU 0.01 0.02 2 N1 > C5A SIMU 0.01 0.02 2 O5 > O6B FLAT 0.005 N1 C1A C2A C3 C4A C5A SIMU 0.01 0.02 2 N2 C47 C48 C49 > C51 DFIX 1.39 0.01 C2A C3 C1A C2A N1 C1A N1 C5A C4A C5A C4A C3 ISOR 0.005 0.01 O5 SUMP 1 0 1 3 1 4 1 5 SUMP 1 0 1 6 1 7 1 8 1 9 SUMP 1 0 1 10 1 11 1 12 1 13 1 14 L.S. 20 0 335 PLAN 40 SIZE 0.09 0.1 0.12 TEMP -80.15 CONF list 4 MORE -1 ABIN BOND $H fmap 2 acta OMIT 0 0 2 OMIT 0 3 1 OMIT 1 0 5 OMIT 1 2 2 OMIT 1 3 0 OMIT 1 3 2 OMIT 2 0 0 OMIT 2 2 2 OMIT 3 1 1 OMIT 3 2 2 OMIT 4 2 7 REM REM REM WGHT 0.070000 60.000000 FVAR 0.20327 0.81190 0.35739 0.31838 0.32424 0.33122 0.24760 FVAR 0.27104 0.15019 0.42342 0.17102 0.11457 0.17725 0.11374 PART 1 I1 4 0.356309 0.595912 0.663617 61.00000 0.12350 0.12905 = 0.09812 0.02762 -0.01941 -0.00855 I2 4 0.717632 0.266418 0.758639 121.00000 0.15946 0.16692 = 0.18442 0.04423 -0.00259 0.00751 PART 3 I3 4 0.725581 0.199155 0.656216 131.00000 0.08954 0.29000 = 0.32578 -0.04972 -0.01809 0.06485 PART 4 I4 4 0.754295 0.306438 0.597466 111.00000 0.05316 0.17145 = 0.36748 -0.05287 0.03420 0.00176 PART 5 I5 4 0.751528 0.308328 0.522948 91.00000 0.23238 0.03462 = 0.29492 -0.00404 0.03389 -0.04671 PART 4 I6 4 0.696416 0.300004 0.508720 81.00000 0.17247 0.08090 = 0.16889 -0.02317 -0.02747 0.05878 PART 3 I7 4 0.723849 0.289987 0.414770 71.00000 0.05148 0.08732 = 0.26357 -0.05970 0.05207 -0.01999 PART 2 I8 4 0.709818 0.306269 0.376010 101.00000 0.06236 0.10422 = 0.20711 0.01174 -0.00151 -0.00560 PART 4 I9 4 0.731172 0.216358 0.684578 141.00000 0.10375 0.20781 = 0.28446 -0.01166 -0.02890 0.06826 PART 0 CU1 3 0.500061 0.489305 0.769001 11.00000 0.22622 0.19058 = 0.08975 -0.07988 -0.02977 -0.01521 O1 6 0.618099 0.472113 0.581332 11.00000 0.06785 0.07556 = 0.08010 -0.01084 -0.01632 -0.02021 O2 6 0.455640 0.386243 0.468991 11.00000 0.06045 0.06363 = 0.05907 -0.00415 0.00275 -0.00917 O3 6 0.498391 0.081053 0.575845 11.00000 0.07150 0.07143 = 0.06111 -0.00074 0.00456 0.01530 O4 6 0.706363 0.026704 0.466224 11.00000 0.05427 0.07092 = 0.07469 -0.01506 0.00723 0.00522 PART 1 O5 6 0.646216 0.443930 0.776462 61.00000 0.18475 0.13795 = 0.13771 -0.05774 -0.02700 0.00467 AFIX 3 H5A 2 0.673906 0.435170 0.794662 61.00000 -1.50000 H5B 2 0.686686 0.431120 0.761962 61.00000 -1.50000 AFIX 0 PART 2 O5A 6 0.498138 0.407206 0.794959 -61.00000 0.38199 0.16339 = 0.10321 -0.04525 -0.06584 0.08840 AFIX 3 H5AA 2 0.499138 0.401886 0.815649 -61.00000 -1.50000 H5AB 2 0.504688 0.371976 0.786939 -61.00000 -1.50000 AFIX 0 PART 1 O6 6 0.545914 0.565457 0.740117 31.00000 0.19128 0.12399 = 0.07433 -0.03877 -0.05638 0.01091 AFIX 3 H6A 2 0.564305 0.599927 0.747017 31.00000 -1.50000 H6B 2 0.547525 0.568457 0.719287 31.00000 -1.50000 AFIX 0 PART 3 O6A 6 0.433188 0.570804 0.749569 51.00000 0.19707 0.14750 = 0.08178 -0.02085 -0.05883 0.01532 AFIX 3 H6AA 2 0.407448 0.599784 0.760349 51.00000 -1.50000 H6AB 2 0.424618 0.580463 0.729519 51.00000 -1.50000 AFIX 0 PART 2 O6B 6 0.620860 0.537164 0.743766 41.00000 0.17729 0.12709 = 0.06903 -0.03592 -0.03193 -0.01751 AFIX 3 H6BA 2 0.668760 0.557064 0.752206 41.00000 -1.50000 H6BB 2 0.629250 0.540654 0.723126 41.00000 -1.50000 AFIX 0 PART 0 N1 5 0.479173 0.440899 0.728888 11.00000 0.15755 0.13905 = 0.09197 -0.04534 -0.02452 0.00669 PART 1 C1 1 0.519822 0.389343 0.724559 21.00000 0.15400 0.13490 = 0.08645 -0.04278 -0.03720 0.01578 AFIX 43 H1 2 0.562755 0.374453 0.740546 21.00000 -1.20000 AFIX 0 PART 2 C1A 1 0.560504 0.423385 0.711377 -21.00000 0.15207 0.13201 = 0.08377 -0.04055 -0.03256 0.01151 AFIX 43 H1A 2 0.626249 0.432466 0.716672 -21.00000 -1.20000 AFIX 0 PART 1 C2 1 0.502211 0.355869 0.697433 21.00000 0.15097 0.12855 = 0.07806 -0.03953 -0.03679 0.01327 AFIX 43 H2 2 0.535175 0.319280 0.694977 21.00000 -1.20000 AFIX 0 PART 2 C2A 1 0.530853 0.390536 0.684921 -21.00000 0.14673 0.12777 = 0.07876 -0.03957 -0.03240 0.01100 AFIX 43 H2A 2 0.583053 0.377060 0.671811 -21.00000 -1.20000 AFIX 0 PART 0 C3 1 0.438960 0.373721 0.674067 11.00000 0.13125 0.11574 = 0.06520 -0.03842 -0.02354 0.00419 PART 1 C4 1 0.400827 0.428925 0.678174 21.00000 0.13120 0.11561 = 0.07317 -0.04480 -0.01987 0.00852 AFIX 43 H4 2 0.359035 0.445012 0.662204 21.00000 -1.20000 AFIX 0 PART 2 C4A 1 0.360320 0.392530 0.692569 -21.00000 0.13768 0.12143 = 0.07677 -0.04458 -0.01799 0.00917 AFIX 43 H4A 2 0.294630 0.383394 0.687227 -21.00000 -1.20000 AFIX 0 PART 1 C5 1 0.422655 0.461987 0.705627 21.00000 0.14217 0.12382 = 0.08269 -0.04447 -0.01724 0.01118 AFIX 43 H5 2 0.396352 0.500573 0.707697 21.00000 -1.20000 AFIX 0 PART 2 C5A 1 0.385122 0.425745 0.719500 -21.00000 0.14232 0.12709 = 0.08322 -0.04519 -0.01903 0.00843 AFIX 43 H5AC 2 0.333050 0.439274 0.732649 -21.00000 -1.20000 AFIX 0 PART 0 C6 1 0.422143 0.340938 0.644441 11.00000 0.08171 0.08487 = 0.05710 -0.01348 -0.00542 -0.01011 C7 1 0.494267 0.304588 0.631475 11.00000 0.09102 0.07292 = 0.06253 -0.01053 -0.01771 0.00559 AFIX 43 H7 2 0.552718 0.297889 0.643199 11.00000 -1.20000 AFIX 0 C8 1 0.481789 0.278043 0.601646 11.00000 0.07278 0.05738 = 0.06370 -0.00159 -0.01386 0.00478 AFIX 43 H8 2 0.533035 0.254990 0.592773 11.00000 -1.20000 AFIX 0 C9 1 0.394260 0.284911 0.584466 11.00000 0.05020 0.05184 = 0.05119 -0.00555 -0.00094 -0.00604 C10 1 0.319970 0.317027 0.598817 11.00000 0.05341 0.07191 = 0.06228 -0.02119 -0.00054 -0.00697 AFIX 43 H10 2 0.258737 0.319872 0.588221 11.00000 -1.20000 AFIX 0 C11 1 0.332237 0.345134 0.628156 11.00000 0.06672 0.09573 = 0.06543 -0.02847 0.00708 -0.00401 AFIX 43 H11 2 0.280129 0.367166 0.637252 11.00000 -1.20000 AFIX 0 C12 1 0.386796 0.258835 0.551752 11.00000 0.04043 0.04675 = 0.04892 -0.00100 -0.00094 -0.00352 C13 1 0.398155 0.198690 0.548422 11.00000 0.04513 0.04627 = 0.04880 0.00062 -0.00025 -0.00525 AFIX 43 H13 2 0.407230 0.175447 0.567183 11.00000 -1.20000 AFIX 0 C14 1 0.396833 0.170603 0.518518 11.00000 0.03812 0.03905 = 0.06064 -0.00530 0.00279 -0.00172 C15 1 0.388480 0.204830 0.491167 11.00000 0.04418 0.04051 = 0.05178 -0.00802 -0.00119 -0.00064 C16 1 0.375211 0.265802 0.494775 11.00000 0.04268 0.04632 = 0.05130 0.00005 -0.00095 -0.00496 AFIX 43 H16 2 0.368082 0.289364 0.476040 11.00000 -1.20000 AFIX 0 C17 1 0.372094 0.292918 0.524379 11.00000 0.04044 0.04392 = 0.05204 -0.00706 -0.00354 -0.00729 C18 1 0.357981 0.359171 0.525347 11.00000 0.04317 0.04566 = 0.06221 -0.00754 -0.00363 0.00153 AFIX 23 H18A 2 0.318662 0.371129 0.506479 11.00000 -1.20000 H18B 2 0.320246 0.369363 0.544863 11.00000 -1.20000 AFIX 0 C19 1 0.451213 0.394058 0.525407 11.00000 0.04117 0.04040 = 0.06672 -0.00212 -0.00440 0.00257 C20 1 0.490380 0.416062 0.553885 11.00000 0.05701 0.04852 = 0.06414 0.00016 -0.00227 -0.00252 AFIX 43 H20 2 0.458858 0.407605 0.573692 11.00000 -1.20000 AFIX 0 C21 1 0.575848 0.450619 0.553873 11.00000 0.04957 0.04464 = 0.08101 -0.00314 -0.00942 -0.00489 C22 1 0.621351 0.464512 0.524690 11.00000 0.04982 0.03581 = 0.08466 0.00320 -0.00516 0.00214 C23 1 0.582947 0.442467 0.496648 11.00000 0.04521 0.04655 = 0.07590 0.00339 0.00149 -0.00147 AFIX 43 H23 2 0.614209 0.451072 0.476816 11.00000 -1.20000 AFIX 0 C24 1 0.499367 0.407869 0.496730 11.00000 0.05110 0.04066 = 0.06014 -0.00356 -0.00153 0.00691 C25 1 0.506811 0.394582 0.439695 11.00000 0.07168 0.07135 = 0.05921 0.00027 0.00648 0.00101 AFIX 23 H25A 2 0.572577 0.376664 0.441019 11.00000 -1.20000 H25B 2 0.514171 0.437187 0.435069 11.00000 -1.20000 AFIX 0 C26 1 0.447833 0.365196 0.413749 11.00000 0.08258 0.10730 = 0.07162 -0.00034 0.00282 0.00239 AFIX 137 H26A 2 0.484984 0.365282 0.393623 11.00000 -1.50000 H26B 2 0.386515 0.386726 0.410689 11.00000 -1.50000 H26C 2 0.433573 0.324435 0.420031 11.00000 -1.50000 AFIX 0 C27 1 0.574855 0.459331 0.611453 11.00000 0.11624 0.12148 = 0.06552 0.00571 -0.01182 -0.04328 AFIX 23 H27A 2 0.570767 0.416133 0.614671 11.00000 -1.20000 H27B 2 0.508074 0.475900 0.612439 11.00000 -1.20000 AFIX 0 C28 1 0.637925 0.486708 0.636943 11.00000 0.17808 0.17381 = 0.08593 -0.00263 -0.03364 -0.09562 AFIX 137 H28A 2 0.657422 0.526402 0.630176 11.00000 -1.50000 H28B 2 0.696250 0.462399 0.640163 11.00000 -1.50000 H28C 2 0.601245 0.489184 0.657118 11.00000 -1.50000 AFIX 0 C29 1 0.406576 0.103305 0.517735 11.00000 0.04691 0.04121 = 0.06691 -0.00395 0.00376 0.00109 AFIX 23 H29A 2 0.369172 0.086733 0.535980 11.00000 -1.20000 H29B 2 0.376186 0.088604 0.497691 11.00000 -1.20000 AFIX 0 C30 1 0.509928 0.080100 0.519452 11.00000 0.04585 0.03552 = 0.06676 -0.00502 0.00064 -0.00324 C31 1 0.553505 0.068142 0.548931 11.00000 0.05773 0.04225 = 0.06258 -0.00162 0.00418 0.00112 C32 1 0.644530 0.040550 0.550254 11.00000 0.06031 0.04093 = 0.06826 -0.00011 -0.00511 -0.00062 AFIX 43 H32 2 0.672028 0.030989 0.570555 11.00000 -1.20000 AFIX 0 C33 1 0.695295 0.026916 0.522529 11.00000 0.04423 0.03819 = 0.08238 -0.00567 0.00191 -0.00364 C34 1 0.653917 0.041575 0.493124 11.00000 0.05342 0.03839 = 0.07625 -0.01179 0.01088 -0.00401 C35 1 0.560813 0.067881 0.491616 11.00000 0.04788 0.04084 = 0.07034 -0.01095 -0.00051 -0.00214 AFIX 43 H35 2 0.532964 0.077244 0.471339 11.00000 -1.20000 AFIX 0 C36 1 0.669347 0.037917 0.435648 11.00000 0.07148 0.07036 = 0.07466 -0.00700 0.01327 0.00547 AFIX 23 H36A 2 0.661217 0.080912 0.432459 11.00000 -1.20000 H36B 2 0.604836 0.018818 0.433101 11.00000 -1.20000 AFIX 0 C37 1 0.740292 0.013535 0.411294 11.00000 0.08010 0.14549 = 0.08640 -0.01936 0.01850 0.01348 AFIX 137 H37A 2 0.716974 0.022502 0.389571 11.00000 -1.50000 H37B 2 0.745435 -0.029304 0.413959 11.00000 -1.50000 H37C 2 0.804537 0.031573 0.414538 11.00000 -1.50000 AFIX 0 C38 1 0.539623 0.071967 0.606605 11.00000 0.10781 0.11938 = 0.06551 0.00033 -0.00484 0.03205 AFIX 23 H38A 2 0.600550 0.094973 0.609140 11.00000 -1.20000 H38B 2 0.554165 0.029692 0.610159 11.00000 -1.20000 AFIX 0 C39 1 0.462671 0.093146 0.629487 11.00000 0.17484 0.22179 = 0.08867 -0.00983 0.01342 0.06294 AFIX 137 H39A 2 0.398950 0.092470 0.618798 11.00000 -1.50000 H39B 2 0.477772 0.133527 0.636266 11.00000 -1.50000 H39C 2 0.461002 0.067281 0.648351 11.00000 -1.50000 AFIX 0 C40 1 0.790020 -0.004319 0.524431 11.00000 0.04549 0.04446 = 0.09760 -0.00287 -0.00438 0.00309 AFIX 23 H40A 2 0.795213 -0.031462 0.505870 11.00000 -1.20000 H40B 2 0.790686 -0.028618 0.544199 11.00000 -1.20000 AFIX 0 C41 1 0.397955 0.180198 0.458142 11.00000 0.05393 0.04801 = 0.04921 -0.00390 0.00447 -0.00291 C42 1 0.329858 0.143027 0.444965 11.00000 0.06037 0.06491 = 0.05199 -0.01290 0.00809 -0.01152 AFIX 43 H42 2 0.271918 0.134545 0.456621 11.00000 -1.20000 AFIX 0 C43 1 0.343942 0.117100 0.414477 11.00000 0.07355 0.07153 = 0.06361 -0.01803 0.00176 -0.01907 AFIX 43 H43 2 0.296361 0.090636 0.406239 11.00000 -1.20000 AFIX 0 C44 1 0.425708 0.129654 0.396527 11.00000 0.07719 0.06203 = 0.05165 -0.01214 0.01148 -0.00666 C45 1 0.494322 0.169125 0.409798 11.00000 0.06613 0.07982 = 0.05773 -0.00582 0.01410 -0.01634 AFIX 43 H45 2 0.551222 0.178788 0.397862 11.00000 -1.20000 AFIX 0 C46 1 0.480654 0.194047 0.439757 11.00000 0.05660 0.06690 = 0.05911 -0.01106 0.01000 -0.01198 AFIX 43 H46 2 0.527736 0.220837 0.447994 11.00000 -1.20000 AFIX 66 C49 1 0.443893 0.099289 0.365677 11.00000 0.08967 0.11980 = 0.06027 -0.02965 0.01401 -0.00952 C50 1 0.538988 0.087217 0.356087 11.00000 0.10724 0.15389 = 0.08666 -0.04687 0.01673 0.00546 AFIX 43 H50 2 0.592330 0.100084 0.368876 11.00000 -1.20000 AFIX 65 C51 1 0.556038 0.056320 0.327784 11.00000 0.12305 0.17217 = 0.09823 -0.06317 0.01648 0.01299 AFIX 43 H51 2 0.621032 0.048070 0.321229 11.00000 -1.20000 AFIX 65 N2 5 0.477991 0.037494 0.309071 11.00000 0.13147 0.16797 = 0.09086 -0.06067 0.01607 0.00327 C47 1 0.382895 0.049565 0.318661 11.00000 0.12554 0.15874 = 0.08551 -0.05219 0.01242 -0.01724 AFIX 43 H47 2 0.329553 0.036698 0.305871 11.00000 -1.20000 AFIX 65 C48 1 0.365844 0.080462 0.346964 11.00000 0.11038 0.14247 = 0.06959 -0.04194 0.01152 -0.01974 AFIX 43 H48 2 0.300850 0.088712 0.353519 11.00000 -1.20000 AFIX 0 HKLF 4 REM cu_231121lu_lgpz184505_1_0m_a.res in Pnnn REM wR2 = 0.3384, GooF = S = 1.142, Restrained GooF = 1.177 for all data REM R1 = 0.1319 for 7024 Fo > 4sig(Fo) and 0.1716 for all 11909 data REM 690 parameters refined using 274 restraints END WGHT 0.2000 0.0000 REM Highest difference peak 1.290, deepest hole -0.721, 1-sigma level 0.113 Q1 1 0.8243 0.2885 0.5216 11.00000 0.05 1.29 Q2 1 0.3851 0.4003 0.8059 11.00000 0.05 1.24 Q3 1 0.7215 0.2955 0.5283 11.00000 0.05 0.94 Q4 1 0.7500 0.2500 0.4280 10.50000 0.05 0.89 Q5 1 0.7140 0.2988 0.3998 11.00000 0.05 0.85 Q6 1 0.7042 0.4552 0.7657 11.00000 0.05 0.82 Q7 1 0.6524 0.2689 0.5162 11.00000 0.05 0.79 Q8 1 0.7732 0.3076 0.5466 11.00000 0.05 0.79 Q9 1 0.7223 0.2819 0.3555 11.00000 0.05 0.78 Q10 1 0.6992 0.3897 0.8000 11.00000 0.05 0.77 Q11 1 0.5979 0.2633 0.7625 11.00000 0.05 0.77 Q12 1 0.3290 0.6280 0.6567 11.00000 0.05 0.75 Q13 1 0.7000 0.3443 0.3698 11.00000 0.05 0.73 Q14 1 0.7500 0.4702 0.7500 10.50000 0.05 0.73 Q15 1 0.7427 0.2971 0.4997 11.00000 0.05 0.73 Q16 1 0.7777 0.3060 0.5047 11.00000 0.05 0.71 Q17 1 0.3614 0.5850 0.6573 11.00000 0.05 0.71 Q18 1 0.7500 0.2500 0.5863 10.50000 0.05 0.68 Q19 1 0.7297 0.2985 0.4276 11.00000 0.05 0.67 Q20 1 0.5581 0.4258 0.7890 11.00000 0.05 0.65 Q21 1 0.6842 0.3155 0.5031 11.00000 0.05 0.65 Q22 1 0.5006 0.5533 0.7456 11.00000 0.05 0.64 Q23 1 0.3989 0.6079 0.6677 11.00000 0.05 0.61 Q24 1 0.3178 0.5962 0.6753 11.00000 0.05 0.59 Q25 1 0.6650 0.5130 0.7440 11.00000 0.05 0.56 Q26 1 0.3687 0.5446 0.7608 11.00000 0.05 0.55 Q27 1 0.7249 0.2778 0.7846 11.00000 0.05 0.54 Q28 1 0.6338 0.5785 0.7312 11.00000 0.05 0.49 Q29 1 0.7662 0.2886 0.6193 11.00000 0.05 0.48 Q30 1 0.7526 0.3057 0.5820 11.00000 0.05 0.41 Q31 1 0.7500 0.2500 0.7500 10.25000 0.05 0.39 Q32 1 0.6352 0.1886 0.7012 11.00000 0.05 0.38 Q33 1 0.4437 0.6202 0.7562 11.00000 0.05 0.38 Q34 1 0.6283 0.1194 0.6177 11.00000 0.05 0.35 Q35 1 0.4775 0.1247 0.3375 11.00000 0.05 0.35 Q36 1 0.7224 0.2120 0.6687 11.00000 0.05 0.32 Q37 1 0.7500 0.3016 0.7500 10.50000 0.05 0.30 Q38 1 0.4772 0.4816 0.7172 11.00000 0.05 0.30 Q39 1 0.5241 0.1011 0.3132 11.00000 0.05 0.30 Q40 1 0.4776 0.5022 0.7321 11.00000 0.05 0.28 ; _shelx_res_checksum 28425 _shelx_hkl_file ; -1 0 0 1.19221 0.72789 6 1 0 0 1.54330 0.63689 6 -2 0 0 585.020 91.2263 6 3 0 0 2.46760 4.15127 1 -3 0 0 7.12963 2.97595 6 4 0 0 6807.84 1060.47 1 5 0 0 4.63932 6.04861 1 -5 0 0 3.12078 3.77137 6 -6 0 0 87.8753 14.4120 6 6 0 0 60.9926 15.4455 1 6 0 0 90.1524 14.0485 4 -7 0 0 16.5971 6.12954 6 7 0 0 8.45809 4.94668 4 7 0 0 22.4326 11.3897 1 8 0 0 1479.02 214.572 4 -8 0 0 1265.75 214.923 6 8 0 0 1359.71 216.154 1 9 0 0 6.60817 9.47921 1 -9 0 0 8.16476 3.95436 3 9 0 0 6.49301 5.56677 4 -9 0 0 6.05934 5.30556 7 -9 0 0 0.25482 7.32003 6 -10 0 0 312.719 45.6184 6 -10 0 0 280.851 42.9982 7 10 0 0 264.061 47.4327 1 10 0 0 253.761 44.9293 4 -10 0 0 260.193 42.9471 3 11 0 0 24.6495 14.3110 1 -11 0 0 2.74252 4.34593 7 -11 0 0 -0.7424 4.25920 3 11 0 0 10.1625 6.60314 4 -11 0 0 8.73553 10.3060 6 -12 0 0 42.3153 8.47011 7 -12 0 0 46.9953 8.65207 3 -13 0 0 -4.0817 5.80693 7 -13 0 0 1.76286 4.39129 3 -14 0 0 53.8565 9.66909 3 -15 0 0 2.97231 3.70818 3 -16 0 0 -0.4780 3.00632 3 0 -1 0 3.01194 0.61188 4 -2 -1 0 0.02420 2.10433 6 -2 -1 0 0.28180 2.98416 1 2 -1 0 3.21858 2.91321 1 -4 1 0 -0.2461 2.91343 6 -4 -1 0 -0.0933 3.56078 6 4 -1 0 0.15097 4.67734 1 4 1 0 2.34549 5.41322 1 -5 1 0 3731.14 584.833 6 5 -1 0 3819.98 585.547 1 5 1 0 3717.85 585.504 1 6 -1 0 5.04072 7.26659 1 -6 -1 0 6.26288 5.10981 6 6 1 0 2.16791 11.4428 1 -6 1 0 3.14794 4.58492 6 6 -1 0 11.2659 4.62069 4 -7 1 0 15.0215 5.99423 6 -7 -1 0 19.6357 6.85169 6 7 -1 0 6.34062 7.81102 1 7 -1 0 28.1318 5.97316 4 7 1 0 21.0163 8.67382 1 -8 -1 0 3.36299 6.76023 6 8 -1 0 -3.5862 7.95484 1 8 1 0 21.3412 10.8994 1 8 1 0 10.5382 5.01167 4 -8 1 0 8.97785 6.31890 6 8 -1 0 11.4877 5.48093 4 -9 1 0 13.1748 4.32215 7 -9 -1 0 14.3985 5.22442 7 9 -1 0 2.03132 10.4064 1 -9 1 0 22.0688 7.86766 6 -9 -1 0 17.8183 4.67804 3 -9 1 0 12.7565 4.45553 3 -9 -1 0 19.3541 8.25636 6 9 1 0 15.4159 14.5144 1 9 -1 0 15.1343 6.35960 4 9 1 0 12.1941 5.88696 4 -10 -1 0 0.50332 3.69516 7 10 -1 0 6.58960 6.44888 4 -10 1 0 2.74197 3.88488 7 -10 -1 0 -11.407 8.17075 6 -10 -1 0 2.32495 3.78641 3 10 1 0 -10.259 14.8322 1 10 -1 0 -17.412 14.3623 1 10 1 0 -4.1479 5.64487 4 -10 1 0 3.22964 3.87905 3 11 1 0 12.8308 15.0695 1 11 -1 0 32.3340 13.8873 1 -11 1 0 28.0949 7.27775 7 11 -1 0 38.9049 9.37780 4 -11 1 0 42.2137 7.39829 3 11 1 0 32.9895 8.73250 4 -11 -1 0 34.6486 7.35657 7 -11 -1 0 33.9161 13.0808 6 -11 -1 0 38.4331 7.23511 3 -11 1 0 27.3789 11.3431 6 -12 -1 0 6.38027 4.69690 3 12 -1 0 -7.9685 12.2955 1 -12 -1 0 4.96144 4.33255 7 12 -1 0 -2.0047 6.50781 4 -12 1 0 2.69035 4.43188 3 -12 1 0 8.43105 4.61797 7 -13 -1 0 178.428 26.5577 3 -13 -1 0 192.100 26.7438 7 13 -1 0 81.5658 30.8753 1 -13 1 0 149.752 27.0547 7 -13 1 0 156.376 26.5687 3 -14 1 0 -0.1510 4.08733 3 -14 1 0 -0.8564 3.73829 7 -14 -1 0 -4.2434 4.01689 3 -15 1 0 56.7290 9.64924 3 -15 -1 0 52.3875 9.55707 3 -16 -1 0 -1.4236 2.54524 3 -16 1 0 -2.5639 2.80369 3 1 2 0 0.10750 0.81972 6 1 -2 0 1.85591 1.46481 1 1 -2 0 1.52411 1.12710 4 -1 -2 0 -0.2830 1.71469 1 1 2 0 0.57986 0.80159 6 3 -2 0 10.1609 4.80709 1 -3 -2 0 6.38116 3.55077 6 -3 -2 0 10.5137 4.96899 1 4 -2 0 1889.77 285.736 4 -4 -2 0 1691.22 285.842 6 4 -2 0 1932.02 286.440 1 5 -2 0 9.02765 6.72156 1 -5 -2 0 4.19903 4.65225 6 -5 2 0 3.33838 3.58100 6 5 2 0 10.0328 6.17438 1 5 -2 0 5.01340 4.12924 4 -6 -2 0 3107.71 497.953 6 6 -2 0 3345.67 497.915 4 -6 2 0 3048.71 497.759 6 6 -2 0 3292.04 498.739 1 7 -2 0 9.29749 5.06683 4 7 2 0 1.58829 7.62526 1 -7 -2 0 -0.8954 5.68318 6 7 -2 0 -9.8648 7.93616 1 -7 2 0 -2.6861 4.75810 6 7 2 0 0.54011 4.10763 4 8 -2 0 319.645 57.3842 1 8 2 0 345.201 57.6327 1 8 -2 0 413.693 55.4950 4 -8 -2 0 322.273 56.0213 6 -8 2 0 294.219 55.5713 6 8 2 0 363.088 55.0406 4 -9 -2 0 5.32977 3.59286 3 -9 -2 0 -5.6044 7.68958 6 9 2 0 -2.4973 14.3420 1 9 -2 0 -0.4074 10.0579 1 -9 -2 0 -3.0959 3.35359 7 -9 2 0 9.33615 7.26561 6 9 -2 0 13.0052 6.30795 4 -9 2 0 3.79446 3.60989 3 9 2 0 10.9526 5.44804 4 -9 2 0 8.76241 3.72942 7 10 2 0 50.8498 9.56658 4 -10 -2 0 41.9500 8.26079 3 -10 2 0 39.8201 8.31564 3 -10 -2 0 54.1119 8.25893 7 10 -2 0 53.6638 10.3656 4 -10 2 0 41.3815 8.34084 7 -10 2 0 39.0740 11.6866 6 10 -2 0 15.8146 12.8069 1 10 2 0 35.4694 15.1239 1 -10 -2 0 67.7751 13.7561 6 11 -2 0 1.03001 9.48368 1 -11 2 0 -1.6634 8.84698 6 -11 -2 0 11.0644 4.48031 3 11 -2 0 10.6669 7.25516 4 -11 2 0 6.39516 4.39519 3 -11 2 0 11.0429 4.80936 7 -12 2 0 26.0030 5.96400 3 -12 2 0 7.30149 10.5272 6 -12 -2 0 12.6430 5.22438 7 12 -2 0 25.0613 8.25639 4 -12 2 0 27.7511 6.08292 7 -12 -2 0 29.2215 5.89021 3 12 -2 0 12.1660 11.9340 1 -13 -2 0 7.05865 5.61243 3 -13 2 0 1.35916 4.63578 3 13 -2 0 -11.768 17.4306 1 -13 2 0 10.2928 6.79951 7 -14 2 0 23.4580 6.87458 7 -14 -2 0 37.9269 7.05250 3 -14 2 0 41.2873 7.02807 3 -15 2 0 -2.6051 3.72545 3 -15 -2 0 0.32498 4.30894 3 -16 2 0 10.2221 3.11295 3 -16 -2 0 2.77689 2.79161 3 0 -3 0 1.07138 1.32563 1 0 -3 0 0.21867 1.05575 4 1 -3 0 760.664 127.211 4 1 -3 0 827.873 127.334 1 -1 -3 0 850.397 127.442 1 1 3 0 864.496 127.161 6 -1 -3 0 784.512 127.143 4 -2 -3 0 7.34865 4.46670 1 2 -3 0 5.60270 3.68225 1 -2 -3 0 8.43656 2.88461 6 2 -3 0 7.82014 3.03403 4 -2 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4.68123 5 -1 -5 -48 2.75010 5.13380 5 -1 5 -48 5.83625 5.03272 5 1 -5 -48 6.66875 5.33301 5 2 5 -48 7.72164 4.72238 5 -2 -5 -48 1.14781 4.67250 5 2 -5 -48 -7.8460 4.62469 5 3 5 -48 3.89995 4.14514 5 -3 -5 -48 2.29979 4.34764 5 3 -5 -48 -2.0877 4.55496 5 0 6 -48 17.3219 4.89576 5 0 -6 -48 4.25978 5.29877 5 -1 -6 -48 -4.3947 5.08859 5 1 6 -48 2.05490 4.38430 5 1 -6 -48 1.60490 4.63206 5 2 6 -48 -2.2260 4.22040 5 -2 -6 -48 3.46384 4.72114 5 2 -6 -48 -1.4880 4.52879 5 3 6 -48 0.71861 4.15965 5 -3 -6 -48 -0.7362 4.03681 5 3 -6 -48 -6.1022 3.93123 5 0 -7 -48 2.39400 4.53659 5 -1 -7 -48 3.05242 4.63115 5 1 7 -48 4.43113 5.54864 5 1 -7 -48 6.28767 4.54817 5 -2 -7 -48 -4.1698 3.97950 5 2 7 -48 -1.7035 3.68752 5 2 -7 -48 8.72366 4.59950 5 0 0 -49 -2.2271 4.70113 5 1 0 -49 1.62200 4.90325 5 -1 0 -49 0.33089 4.94851 5 -2 0 -49 3.80327 5.19605 5 2 0 -49 4.47899 4.74268 5 3 0 -49 -0.6868 4.21052 5 0 -1 -49 -2.5940 4.70448 5 0 1 -49 0.85335 4.62028 5 1 1 -49 8.85731 4.84150 5 -1 -1 -49 2.37861 4.65426 5 1 -1 -49 6.38944 5.34216 5 -1 1 -49 3.27849 4.66881 5 -2 -1 -49 -0.3481 4.54286 5 2 1 -49 -1.0430 4.69169 5 2 -1 -49 -5.9178 4.65420 5 -2 1 -49 3.13756 4.47520 5 -3 -1 -49 5.22575 4.29559 7 3 1 -49 -7.6462 4.04116 5 3 -1 -49 -2.9127 4.22237 5 0 -2 -49 2.57335 5.02027 5 0 2 -49 -6.6713 4.33550 5 1 2 -49 5.83758 4.86711 5 -1 -2 -49 -4.7718 4.50395 5 -1 2 -49 3.33967 4.65617 5 1 -2 -49 -0.7167 4.92497 5 2 2 -49 -6.7667 4.19416 5 -2 -2 -49 -1.8300 4.41221 5 2 -2 -49 -1.5221 4.53002 5 3 2 -49 -1.2393 3.99491 5 -3 -2 -49 2.63151 5.02984 5 3 -2 -49 0.29966 4.22383 5 0 -3 -49 4.40338 4.91844 5 0 3 -49 -1.9016 4.50899 5 1 3 -49 -1.7180 4.33709 5 -1 -3 -49 -2.4414 4.36529 5 1 -3 -49 0.82966 4.71309 5 -1 3 -49 3.59960 4.33690 5 -2 -3 -49 4.37247 4.28849 5 2 3 -49 -1.7311 4.26874 5 2 -3 -49 0.13839 4.38571 5 -3 -3 -49 -1.2560 4.12481 5 3 3 -49 -4.2107 3.84097 5 3 -3 -49 2.93307 4.19967 5 0 4 -49 1.74005 4.64213 5 0 -4 -49 -5.5500 4.63548 5 1 4 -49 -5.8512 4.05302 5 -1 -4 -49 -4.5687 4.26010 5 1 -4 -49 0.71355 4.29413 5 -2 -4 -49 -1.3188 4.14380 5 2 4 -49 0.11893 4.10733 5 2 -4 -49 4.05832 4.52714 5 0 -5 -49 5.00581 4.64077 5 1 5 -49 8.09265 4.48111 5 -1 -5 -49 1.38769 4.63413 5 1 -5 -49 5.29188 4.64184 5 0 0 -50 7.03811 4.95691 5 -1 0 -50 0.00481 4.14653 5 1 0 -50 4.57603 4.51762 5 0 -1 -50 5.72995 4.29022 5 0 1 -50 -3.2958 6.10712 5 1 1 -50 -1.5785 4.07215 5 -1 -1 -50 4.09595 6.17223 5 1 -1 -50 2.80736 4.17255 5 -1 1 -50 6.97267 4.47446 5 0 -2 -50 4.84329 4.27059 5 0 2 -50 1.09525 4.16826 5 0 0 0 0.00 0.00 0 _exptl_absorpt_process_details ) SADABS 2016/2: Krause, L., Herbst-Irmer, R., Sheldrick G.M. & Stalke D., J. Appl. Cryst. 48 (2015) 3-10 ) _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_max 0.7531 _exptl_absorpt_correction_T_min 0.2906 _exptl_special_details ) The following wavelength and cell were deduced by SADABS from the direction cosines etc. They are given here for emergency use only: CELL 1.54184 13.719 22.675 41.653 89.910 89.983 90.043 ) ; _shelx_hkl_checksum 4869 _shelx_fab_file ; 0 0 2 -531.8673 -4.8885 0 0 4 208.0329 6.8076 0 0 6 -14.9713 -3.0353 0 0 8 -46.4476 -2.7658 0 0 10 44.0789 5.9465 0 0 12 -28.7533 -6.1395 0 0 14 30.1196 3.3473 0 0 16 -25.3143 0.9546 0 0 18 8.9811 -3.2907 0 0 20 3.9874 2.0830 0 0 22 -10.4072 1.1303 0 0 24 8.3612 -2.2580 0 0 26 -5.3374 -0.5074 0 0 28 3.7911 3.2843 0 0 30 0.4623 -2.7799 0 0 32 -2.4917 0.5008 0 0 34 1.8525 0.9377 0 0 36 -0.0867 -0.7390 0 0 38 -2.6365 -0.2053 0 0 40 1.9638 0.7123 0 0 42 1.7044 -0.4785 0 0 44 -4.1646 -0.1268 0 0 46 2.0169 0.5602 0 0 48 3.2108 -0.5388 0 0 50 -4.2244 0.2687 0 1 1 -140.6560 -4.7694 0 1 3 2.7210 6.1950 0 1 5 54.9456 -3.2144 0 1 7 -9.5387 -1.8318 0 1 9 -37.9653 1.7317 0 1 11 55.0090 1.3623 0 1 13 -31.3521 -1.8466 0 1 15 -8.1941 0.1339 0 1 17 26.6806 0.6046 0 1 19 -26.5869 0.8235 0 1 21 17.6490 -1.4432 0 1 23 -10.4414 -0.4698 0 1 25 8.3079 1.1940 0 1 27 -3.8121 0.4255 0 1 29 0.8420 -1.0294 0 1 31 -0.4618 0.1044 0 1 33 -0.6051 0.4478 0 1 35 0.7411 -0.2468 0 1 37 -1.8530 -0.0472 0 1 39 3.3264 0.0387 0 1 41 -3.2930 0.0423 0 1 43 2.6675 0.0192 0 1 45 -1.1954 -0.0062 0 1 47 0.4531 -0.0934 0 1 49 0.0551 0.0816 0 2 0 -334.9773 2.0485 0 2 2 214.3333 2.1579 0 2 4 -25.4275 -3.7935 0 2 6 -41.0340 -1.7572 0 2 8 24.1460 5.5316 0 2 10 8.0860 -2.7051 0 2 12 -23.6887 0.0053 0 2 14 13.5237 -1.3208 0 2 16 -7.6790 3.6714 0 2 18 13.2218 -2.7631 0 2 20 -17.9938 -0.4778 0 2 22 17.9985 0.6406 0 2 24 -10.4182 1.3887 0 2 26 4.1695 -0.8099 0 2 28 -1.9752 -0.7227 0 2 30 -1.5155 0.2631 0 2 32 2.8519 0.6209 0 2 34 -2.1183 -0.4137 0 2 36 0.3407 -0.2493 0 2 38 2.1003 0.4348 0 2 40 -0.9880 -0.1280 0 2 42 -2.2438 0.0029 0 2 44 4.4377 -0.1057 0 2 46 -3.9722 0.0583 0 2 48 0.5369 0.0109 0 2 50 1.3516 0.0944 0 3 1 65.8138 7.8044 0 3 3 25.4734 -5.8255 0 3 5 -56.4594 -0.1215 0 3 7 25.3351 4.1102 0 3 9 -3.5433 0.5255 0 3 11 -1.2803 -7.0882 0 3 13 -10.4397 7.2146 0 3 15 23.7268 -1.7222 0 3 17 -21.7208 -2.7710 0 3 19 11.7238 1.0970 0 3 21 -0.1598 2.6999 0 3 23 -3.9157 -2.4676 0 3 25 1.5008 0.4907 0 3 27 -3.3762 0.2325 0 3 29 5.1730 -0.8413 0 3 31 -3.9916 0.9540 0 3 33 1.7747 0.1045 0 3 35 1.6733 -0.9167 0 3 37 -3.0664 0.5449 0 3 39 3.5712 0.4298 0 3 41 -3.7145 -0.8270 0 3 43 1.6819 0.3359 0 3 45 -1.1910 0.1823 0 3 47 2.3286 -0.2808 0 3 49 -2.2045 0.2435 0 4 0 90.7506 -2.6212 0 4 2 -34.4378 2.4949 0 4 4 -34.2849 -3.3982 0 4 6 27.1328 5.3821 0 4 8 -0.5113 -4.2494 0 4 10 -3.8649 0.9111 0 4 12 -10.8583 0.4599 0 4 14 28.2014 0.6979 0 4 16 -26.7793 -3.4655 0 4 18 14.3800 4.3570 0 4 20 -3.1141 -1.1247 0 4 22 -2.7960 -1.6743 0 4 24 -0.1391 1.3699 0 4 26 1.9270 -0.3640 0 4 28 -0.4573 -0.6215 0 4 30 0.7115 1.2518 0 4 32 0.3824 -0.4624 0 4 34 -1.5735 -0.7196 0 4 36 2.3855 0.9563 0 4 38 -2.5609 -0.3278 0 4 40 -0.4582 -0.3831 0 4 42 2.1416 0.4351 0 4 44 -2.2134 -0.0506 0 4 46 4.3090 -0.1756 0 4 48 -4.9416 0.2461 0 5 1 22.1914 -6.4047 0 5 3 -64.3247 2.3722 0 5 5 61.1545 -0.2828 0 5 7 -20.8294 1.8817 0 5 9 -7.5108 -3.4277 0 5 11 18.4822 2.5641 0 5 13 -17.3554 -2.6702 0 5 15 14.8174 3.4393 0 5 17 -12.7026 -1.3704 0 5 19 8.7949 -0.7147 0 5 21 -8.9045 0.0640 0 5 23 6.2948 0.8337 0 5 25 -0.6538 -0.6910 0 5 27 -0.2738 -0.0089 0 5 29 0.7667 0.6757 0 5 31 -1.1892 -0.3689 0 5 33 1.0626 -0.2693 0 5 35 -2.2793 0.2746 0 5 37 2.5471 -0.1049 0 5 39 -4.4936 0.0442 0 5 41 5.9903 -0.0024 0 5 43 -2.3874 -0.0112 0 5 45 0.6485 0.0565 0 5 47 -3.0964 0.0291 0 5 49 3.3884 -0.2423 0 6 0 45.6253 1.2113 0 6 2 -70.7132 -4.2820 0 6 4 90.3964 5.5562 0 6 6 -60.0965 -0.2100 0 6 8 22.0565 -3.0037 0 6 10 -9.5695 -1.9657 0 6 12 15.5073 6.1067 0 6 14 -15.8800 -2.3321 0 6 16 4.3776 -1.6452 0 6 18 2.0957 -0.0804 0 6 20 -4.2304 2.3925 0 6 22 6.7699 -1.7275 0 6 24 -6.1616 0.3755 0 6 26 6.9798 -0.2718 0 6 28 -6.8289 0.6832 0 6 30 4.0505 -0.2399 0 6 32 -3.6550 -0.2490 0 6 34 2.6552 -0.3726 0 6 36 -1.3187 0.8162 0 6 38 -0.0824 -0.1820 0 6 40 3.4624 -0.4747 0 6 42 -2.2351 0.4262 0 6 44 -1.5972 0.0374 0 6 46 -0.3975 -0.2860 0 6 48 3.6867 0.0758 0 7 1 40.4971 3.3528 0 7 3 5.7071 2.2925 0 7 5 -35.0527 0.8991 0 7 7 33.1253 -8.3491 0 7 9 -24.5349 4.9251 0 7 11 19.6149 4.4006 0 7 13 -10.5748 -3.9416 0 7 15 -6.2845 -4.1053 0 7 17 13.5940 6.2401 0 7 19 -9.5799 -1.5162 0 7 21 8.8376 -1.3913 0 7 23 -7.4455 0.3020 0 7 25 4.0156 0.6084 0 7 27 -2.1818 -0.0323 0 7 29 -0.5468 0.3314 0 7 31 0.4033 -1.3232 0 7 33 1.0762 0.5633 0 7 35 -1.2229 1.0402 0 7 37 3.3033 -1.0391 0 7 39 -2.2156 -0.0379 0 7 41 -1.0574 0.5144 0 7 43 -0.2804 -0.1375 0 7 45 0.4417 -0.3573 0 7 47 2.7977 0.3546 0 8 0 18.1683 4.8680 0 8 2 0.1965 3.1176 0 8 4 -21.1639 -9.7683 0 8 6 9.3791 1.4841 0 8 8 14.1259 4.7797 0 8 10 -16.4060 1.6301 0 8 12 0.7262 -6.9536 0 8 14 5.9604 2.3694 0 8 16 -5.5143 2.7319 0 8 18 13.8823 -0.8131 0 8 20 -19.6857 -2.4115 0 8 22 16.1881 0.9401 0 8 24 -9.3961 1.4228 0 8 26 0.5016 -0.2380 0 8 28 3.7450 -1.1445 0 8 30 -3.9216 -0.4072 0 8 32 4.6462 1.6065 0 8 34 -1.9667 -0.3236 0 8 36 0.0807 -0.8073 0 8 38 -0.3803 0.3557 0 8 40 -2.0970 0.3449 0 8 42 1.6443 -0.3687 0 8 44 1.5943 -0.0109 0 8 46 -0.3608 0.2124 0 8 48 -1.6314 -0.1420 0 9 1 -16.7666 -7.1450 0 9 3 -9.0684 -4.5010 0 9 5 24.4407 3.1952 0 9 7 -16.5587 6.7882 0 9 9 6.2176 -5.5517 0 9 11 -6.3537 -2.1750 0 9 13 0.8782 2.4888 0 9 15 15.0711 2.2880 0 9 17 -19.6142 -2.6628 0 9 19 13.4557 -1.3280 0 9 21 -10.1374 1.9153 0 9 23 5.5274 1.7313 0 9 25 -0.7444 -2.2766 0 9 27 -2.1439 -0.9635 0 9 29 4.7261 1.6374 0 9 31 -2.5635 0.4905 0 9 33 0.4443 -1.0764 0 9 35 -0.0691 0.1576 0 9 37 -4.5463 0.1789 0 9 39 6.2952 0.0143 0 9 41 -3.0610 -0.1268 0 9 43 2.3930 0.1174 0 9 45 -1.7620 -0.1193 0 9 47 -0.5564 0.1675 0 10 0 -12.2404 -11.2775 0 10 2 2.3627 0.8524 0 10 4 8.3398 9.8090 0 10 6 4.0812 -3.2892 0 10 8 -27.2026 -3.2948 0 10 10 30.9358 0.2700 0 10 12 -17.8307 2.3652 0 10 14 12.1323 -0.5195 0 10 16 -9.2191 -0.9917 0 10 18 -0.8039 -1.1142 0 10 20 6.8358 3.3200 0 10 22 -7.8975 -0.6812 0 10 24 6.4772 -2.4695 0 10 26 -0.7442 0.3240 0 10 28 -1.9618 2.5228 0 10 30 2.5979 -1.3650 0 10 32 -3.3999 -0.4525 0 10 34 -0.4179 0.3731 0 10 36 2.0041 0.1120 0 10 38 0.2089 -0.2140 0 10 40 1.2739 0.2105 0 10 42 -2.1874 -0.1627 0 10 44 0.4150 0.0606 0 10 46 -0.6035 0.1136 0 11 1 15.0991 5.1817 0 11 3 -2.1881 4.4222 0 11 5 -6.7965 -2.4971 0 11 7 4.6985 -4.8501 0 11 9 -5.2381 2.9233 0 11 11 13.7364 1.3344 0 11 13 -12.4042 -0.6941 0 11 15 0.7254 -1.9216 0 11 17 2.9384 2.4749 0 11 19 -2.1576 0.4830 0 11 21 3.4556 -1.8718 0 11 23 -2.5346 -1.3505 0 11 25 3.4954 2.7335 0 11 27 -4.4214 -0.1654 0 11 29 2.2179 -0.9081 0 11 31 -2.5560 -0.0530 0 11 33 1.0412 0.2459 0 11 35 2.4150 -0.0204 0 11 37 -0.3222 0.0748 0 11 39 -1.1993 -0.0364 0 11 41 -0.6547 -0.1062 0 11 43 0.0094 0.2465 0 11 45 1.0148 -0.2178 0 12 0 2.3591 5.3673 0 12 2 -0.1680 0.8944 0 12 4 1.2648 -5.3372 0 12 6 -15.0099 -0.0752 0 12 8 30.5882 1.4128 0 12 10 -28.7149 1.9541 0 12 12 15.6792 -2.2616 0 12 14 -8.1699 0.6342 0 12 16 2.1802 1.4437 0 12 18 3.9018 -1.3659 0 12 20 -4.6513 -1.8767 0 12 22 6.1100 2.1652 0 12 24 -6.6279 0.6206 0 12 26 2.9211 -0.8160 0 12 28 -2.8567 -0.1962 0 12 30 3.0867 -0.1316 0 12 32 -0.5635 0.0707 0 12 34 1.0604 0.3932 0 12 36 -0.2956 -0.1179 0 12 38 -2.1646 -0.3578 0 12 40 0.2910 0.4738 0 12 42 1.8406 -0.1749 0 12 44 -1.5916 -0.2058 0 13 1 -8.2972 -0.2653 0 13 3 3.4163 -2.3805 0 13 5 0.2355 -1.9423 0 13 7 -1.1627 4.5129 0 13 9 5.7094 -0.2790 0 13 11 -10.7395 -1.6313 0 13 13 5.1036 0.9796 0 13 15 3.6715 0.0276 0 13 17 -4.4075 -2.1978 0 13 19 4.2033 1.1877 0 13 21 -4.4566 1.6608 0 13 23 2.5057 -0.8444 0 13 25 -3.2238 -0.6682 0 13 27 1.4119 0.3406 0 13 29 4.0682 -0.4159 0 13 31 -4.2561 0.3725 0 13 33 3.2778 0.3871 0 13 35 -4.0511 -0.4220 0 13 37 1.7171 -0.1438 0 13 39 -0.0806 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11 0.4740 0.2428 15 8 12 -0.2429 -0.0389 15 8 13 -0.8981 -0.0694 15 8 14 -0.5972 -0.5572 15 8 15 1.4150 0.0772 15 9 0 -1.3835 1.0874 15 9 1 0.6269 -0.6123 15 9 2 2.0223 0.1206 15 9 3 -1.4517 0.0932 15 9 4 -2.5806 -0.9431 15 9 5 0.4729 0.0872 15 9 6 2.1207 0.3933 15 9 7 1.5172 0.0394 15 9 8 -1.9168 0.1078 15 9 9 -1.6106 0.1509 15 9 10 2.3428 0.0691 15 9 11 0.7818 -0.1273 15 9 12 -2.6281 -0.0364 15 9 13 -1.1977 -0.3666 15 10 1 1.4724 -0.2649 15 10 2 0.8835 0.3273 15 10 3 -0.6528 -0.6372 15 10 4 -1.1276 0.0621 15 10 5 -0.7866 0.5608 15 10 6 1.9286 -0.0561 15 10 7 1.7762 0.1040 15 10 8 -2.3142 0.2279 15 10 9 -1.7297 -0.1975 15 10 10 1.2793 -0.4554 15 11 0 1.7006 -0.8977 15 11 1 -0.2966 0.5435 15 11 2 -2.1151 0.0851 15 11 3 0.6573 -0.0907 15 11 4 2.6723 0.6278 15 11 5 0.1408 -0.1650 15 11 6 -2.2572 -0.4743 16 0 0 3.8375 0.1192 16 0 2 -1.4282 -0.2671 16 0 4 0.1003 0.0372 16 0 6 -2.9808 0.4755 16 0 8 4.4614 -0.2496 16 0 10 -3.0178 -0.1801 16 0 12 0.5995 0.1296 16 1 1 0.7699 -0.3836 16 1 2 0.9042 1.0048 16 1 3 -3.8242 0.1391 16 1 4 -1.4415 -0.2244 16 1 5 2.9649 0.2950 16 1 6 1.2219 -0.6159 16 1 7 -0.0769 -0.2958 16 1 8 -0.4650 0.3752 16 1 9 -1.0457 0.0059 16 1 10 0.0865 0.0499 16 1 11 0.8592 0.0320 16 1 12 -0.4218 -0.3738 16 2 0 -4.4987 -0.4608 16 2 1 0.5239 1.1948 16 2 2 2.0406 0.1196 16 2 3 -1.3577 -0.5904 16 2 4 -0.2590 0.3247 16 2 5 1.3736 -0.6739 16 2 6 2.3761 -0.5670 16 2 7 -0.3480 0.8178 16 2 8 -3.6548 0.2901 16 2 9 -0.5890 -0.0211 16 2 10 2.9517 0.0277 16 2 11 0.1434 -0.4869 16 2 12 -1.6057 -0.2742 16 3 1 -0.0454 0.2075 16 3 2 -0.8334 -1.2514 16 3 3 2.6413 0.1931 16 3 4 1.5669 0.2637 16 3 5 -2.1918 -0.2711 16 3 6 -1.3869 0.5599 16 3 7 0.4706 -0.0071 16 3 8 0.0147 -0.3664 16 3 9 -0.1733 -0.0720 16 3 10 0.9928 0.0294 16 3 11 0.3273 0.2016 16 4 0 4.7359 0.2664 16 4 1 -0.1784 -1.5731 16 4 2 -2.7331 0.0938 16 4 3 0.6845 0.9591 16 4 4 1.2161 -0.3521 16 4 5 -1.0918 0.1617 16 4 6 -2.6368 0.0648 16 4 7 0.5859 -0.3326 16 4 8 3.1373 0.1255 16 4 9 0.4710 -0.0757 16 4 10 -2.2497 0.1376 16 5 1 3.1089 0.2403 16 5 2 0.8371 0.8355 16 5 3 -4.0261 -0.4485 16 5 4 -1.8270 -0.2631 16 5 5 2.2747 -0.0931 16 5 6 2.3832 -0.0599 16 5 7 -0.1827 0.6902 16 5 8 -1.3638 0.1353 16 6 0 -3.4020 -0.0778 16 6 1 -0.2346 0.6026 16 6 2 1.8517 -0.2907 16 6 3 0.5048 -0.1753 16 6 4 -0.6913 0.3097 16 6 5 -0.1757 -0.1427 16 6 6 1.8659 0.4670 0 0 0 0.0 0.0 ; _shelx_fab_checksum 68369 _olex2_submission_special_instructions 'No special instructions were received' _site XU loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x+1/2, y, -z+1/2' 'x, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x-1/2, -y, z-1/2' '-x, 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 I1 I 0.3563(2) 0.59591(12) 0.66362(6) 0.1169(11) Uani 0.331(2) 1 d . U P A 1 I2 I 0.7176(7) 0.2664(5) 0.7586(3) 0.170(6) Uani 0.115(2) 1 d . U P B 1 I3 I 0.7256(6) 0.1992(5) 0.6562(4) 0.235(5) Uani 0.177(3) 1 d . U P C 3 I4 I 0.7543(4) 0.3064(3) 0.5975(2) 0.197(4) Uani 0.171(2) 1 d . U P D 4 I5 I 0.7515(9) 0.3083(3) 0.5229(3) 0.187(5) Uani 0.150(3) 1 d . U P E 5 I6 I 0.6964(4) 0.3000(2) 0.50872(11) 0.1408(19) Uani 0.271(3) 1 d . U P F 4 I7 I 0.72385(19) 0.28999(14) 0.41477(13) 0.134(2) Uani 0.248(2) 1 d . U P G 3 I8 I 0.70982(12) 0.30627(9) 0.37601(7) 0.1246(10) Uani 0.423(2) 1 d . U P H 2 I9 I 0.7312(9) 0.2164(7) 0.6846(5) 0.199(6) Uani 0.114(3) 1 d . U P I 4 Cu1 Cu 0.5001(2) 0.48930(11) 0.76900(4) 0.1689(11) Uani 1 1 d D . . . . O1 O 0.6181(4) 0.4721(2) 0.58133(14) 0.0745(15) Uani 1 1 d . . . . . O2 O 0.4556(4) 0.3862(2) 0.46899(11) 0.0611(12) Uani 1 1 d . . . . . O3 O 0.4984(4) 0.0811(2) 0.57585(12) 0.0680(14) Uani 1 1 d . . . . . O4 O 0.7064(4) 0.0267(2) 0.46622(13) 0.0666(13) Uani 1 1 d . . . . . O5 O 0.6462(15) 0.4439(11) 0.7765(7) 0.153(9) Uani 0.331(2) 1 d D U P A 1 H5A H 0.673906 0.435170 0.794662 0.230 Uiso 0.331(2) 1 d R U P A 1 H5B H 0.686686 0.431120 0.761962 0.230 Uiso 0.331(2) 1 d R U P A 1 O5A O 0.4981(17) 0.4072(6) 0.7950(3) 0.216(8) Uani 0.669(2) 1 d D U P A 2 H5AA H 0.499138 0.401886 0.815649 0.324 Uiso 0.669(2) 1 d R U P A 2 H5AB H 0.504688 0.371976 0.786939 0.324 Uiso 0.669(2) 1 d R U P A 2 O6 O 0.546(2) 0.5655(8) 0.7401(4) 0.130(6) Uani 0.357(3) 1 d D U P A 1 H6A H 0.564305 0.599927 0.747017 0.195 Uiso 0.357(3) 1 d R U P A 1 H6B H 0.547525 0.568457 0.719287 0.195 Uiso 0.357(3) 1 d R U P A 1 O6A O 0.433(2) 0.5708(9) 0.7496(6) 0.142(7) Uani 0.324(3) 1 d D U P A 3 H6AA H 0.407448 0.599784 0.760349 0.213 Uiso 0.324(3) 1 d R U P A 3 H6AB H 0.424618 0.580463 0.729519 0.213 Uiso 0.324(3) 1 d R U P A 3 O6B O 0.6209(17) 0.5372(11) 0.7438(5) 0.124(7) Uani 0.318(3) 1 d D U P A 2 H6BA H 0.668760 0.557064 0.752206 0.187 Uiso 0.318(3) 1 d R U P A 2 H6BB H 0.629250 0.540654 0.723126 0.187 Uiso 0.318(3) 1 d R U P A 2 N1 N 0.4792(9) 0.4409(5) 0.7289(2) 0.130(3) Uani 1 1 d D U . . . C1 C 0.5198(13) 0.3893(8) 0.7246(3) 0.125(3) Uani 0.812(11) 1 d . U P J 1 H1 H 0.562755 0.374453 0.740546 0.150 Uiso 0.812(11) 1 calc R U P J 1 C1A C 0.5605(17) 0.4234(10) 0.7114(6) 0.123(4) Uani 0.188(11) 1 d D U P J 2 H1A H 0.626249 0.432466 0.716672 0.147 Uiso 0.188(11) 1 calc R U P J 2 C2 C 0.5022(12) 0.3559(7) 0.6974(3) 0.119(3) Uani 0.812(11) 1 d . U P J 1 H2 H 0.535175 0.319280 0.694977 0.143 Uiso 0.812(11) 1 calc R U P J 1 C2A C 0.5309(17) 0.3905(10) 0.6849(8) 0.118(4) Uani 0.188(11) 1 d D U P J 2 H2A H 0.583053 0.377060 0.671811 0.141 Uiso 0.188(11) 1 calc R U P J 2 C3 C 0.4390(9) 0.3737(5) 0.6741(2) 0.104(3) Uani 1 1 d D U . . . C4 C 0.4008(11) 0.4289(6) 0.6782(3) 0.107(3) Uani 0.812(11) 1 d . U P J 1 H4 H 0.359035 0.445012 0.662204 0.128 Uiso 0.812(11) 1 calc R U P J 1 C4A C 0.360(2) 0.3925(13) 0.6926(7) 0.112(4) Uani 0.188(11) 1 d D U P J 2 H4A H 0.294630 0.383394 0.687227 0.134 Uiso 0.188(11) 1 calc R U P J 2 C5 C 0.4227(12) 0.4620(7) 0.7056(3) 0.116(3) Uani 0.812(11) 1 d . U P J 1 H5 H 0.396352 0.500573 0.707697 0.139 Uiso 0.812(11) 1 calc R U P J 1 C5A C 0.3851(17) 0.4257(13) 0.7195(9) 0.118(4) Uani 0.188(11) 1 d D U P J 2 H5AC H 0.333050 0.439274 0.732649 0.141 Uiso 0.188(11) 1 calc R U P J 2 C6 C 0.4221(7) 0.3409(4) 0.64444(19) 0.075(2) Uani 1 1 d . . . . . C7 C 0.4943(7) 0.3046(4) 0.63148(19) 0.075(2) Uani 1 1 d . . . . . H7 H 0.552718 0.297889 0.643199 0.091 Uiso 1 1 calc R U . . . C8 C 0.4818(6) 0.2780(3) 0.60165(18) 0.0646(19) Uani 1 1 d . . . . . H8 H 0.533035 0.254990 0.592773 0.078 Uiso 1 1 calc R U . . . C9 C 0.3943(5) 0.2849(3) 0.58447(16) 0.0511(15) Uani 1 1 d . . . . . C10 C 0.3200(5) 0.3170(3) 0.59882(18) 0.0625(19) Uani 1 1 d . . . . . H10 H 0.258737 0.319872 0.588221 0.075 Uiso 1 1 calc R U . . . C11 C 0.3322(6) 0.3451(4) 0.62816(19) 0.076(2) Uani 1 1 d . . . . . H11 H 0.280129 0.367166 0.637252 0.091 Uiso 1 1 calc R U . . . C12 C 0.3868(4) 0.2588(3) 0.55175(15) 0.0454(14) Uani 1 1 d . . . . . C13 C 0.3982(5) 0.1987(3) 0.54842(15) 0.0467(14) Uani 1 1 d . . . . . H13 H 0.407230 0.175447 0.567183 0.056 Uiso 1 1 calc R U . . . C14 C 0.3968(4) 0.1706(3) 0.51852(16) 0.0459(14) Uani 1 1 d . . . . . C15 C 0.3885(5) 0.2048(3) 0.49117(15) 0.0455(14) Uani 1 1 d . . . . . C16 C 0.3752(4) 0.2658(3) 0.49478(16) 0.0468(14) Uani 1 1 d . . . . . H16 H 0.368082 0.289364 0.476040 0.056 Uiso 1 1 calc R U . . . C17 C 0.3721(4) 0.2929(3) 0.52438(15) 0.0455(14) Uani 1 1 d . . . . . C18 C 0.3580(5) 0.3592(3) 0.52535(17) 0.0503(15) Uani 1 1 d . . . . . H18A H 0.318662 0.371129 0.506479 0.060 Uiso 1 1 calc R U . . . H18B H 0.320246 0.369363 0.544863 0.060 Uiso 1 1 calc R U . . . C19 C 0.4512(5) 0.3941(3) 0.52541(17) 0.0494(15) Uani 1 1 d . . . . . C20 C 0.4904(5) 0.4161(3) 0.55389(18) 0.0566(17) Uani 1 1 d . . . . . H20 H 0.458858 0.407605 0.573692 0.068 Uiso 1 1 calc R U . . . C21 C 0.5758(5) 0.4506(3) 0.55387(19) 0.0584(18) Uani 1 1 d . . . . . C22 C 0.6214(5) 0.4645(3) 0.52469(19) 0.0568(17) Uani 1 1 d . . . . . C23 C 0.5829(5) 0.4425(3) 0.49665(19) 0.0559(17) Uani 1 1 d . . . . . H23 H 0.614209 0.451072 0.476816 0.067 Uiso 1 1 calc R U . . . C24 C 0.4994(5) 0.4079(3) 0.49673(16) 0.0506(15) Uani 1 1 d . . . . . C25 C 0.5068(6) 0.3946(4) 0.43969(17) 0.067(2) Uani 1 1 d . . . . . H25A H 0.572577 0.376664 0.441019 0.081 Uiso 1 1 calc R U . . . H25B H 0.514171 0.437187 0.435069 0.081 Uiso 1 1 calc R U . . . C26 C 0.4478(7) 0.3652(5) 0.4137(2) 0.087(3) Uani 1 1 d . . . . . H26A H 0.484984 0.365282 0.393623 0.131 Uiso 1 1 calc R U . . . H26B H 0.386515 0.386726 0.410689 0.131 Uiso 1 1 calc R U . . . H26C H 0.433573 0.324435 0.420031 0.131 Uiso 1 1 calc R U . . . C27 C 0.5749(9) 0.4593(5) 0.6115(2) 0.101(3) Uani 1 1 d . . . . . H27A H 0.570767 0.416133 0.614671 0.121 Uiso 1 1 calc R U . . . H27B H 0.508074 0.475900 0.612439 0.121 Uiso 1 1 calc R U . . . C28 C 0.6379(11) 0.4867(7) 0.6369(3) 0.146(6) Uani 1 1 d . . . . . H28A H 0.657422 0.526402 0.630176 0.219 Uiso 1 1 calc R U . . . H28B H 0.696250 0.462399 0.640163 0.219 Uiso 1 1 calc R U . . . H28C H 0.601245 0.489184 0.657118 0.219 Uiso 1 1 calc R U . . . C29 C 0.4066(5) 0.1033(3) 0.51774(17) 0.0517(16) Uani 1 1 d . . . . . H29A H 0.369172 0.086733 0.535980 0.062 Uiso 1 1 calc R U . . . H29B H 0.376186 0.088604 0.497691 0.062 Uiso 1 1 calc R U . . . C30 C 0.5099(5) 0.0801(3) 0.51945(17) 0.0494(15) Uani 1 1 d . . . . . C31 C 0.5535(5) 0.0681(3) 0.54893(17) 0.0542(16) Uani 1 1 d . . . . . C32 C 0.6445(5) 0.0406(3) 0.55025(18) 0.0565(17) Uani 1 1 d . . . . . H32 H 0.672028 0.030989 0.570555 0.068 Uiso 1 1 calc R U . . . C33 C 0.6953(5) 0.0269(3) 0.52253(19) 0.0549(17) Uani 1 1 d . . . . . C34 C 0.6539(5) 0.0416(3) 0.49312(19) 0.0560(17) Uani 1 1 d . . . . . C35 C 0.5608(5) 0.0679(3) 0.49162(18) 0.0530(16) Uani 1 1 d . . . . . H35 H 0.532964 0.077244 0.471339 0.064 Uiso 1 1 calc R U . . . C36 C 0.6693(6) 0.0379(4) 0.4356(2) 0.072(2) Uani 1 1 d . . . . . H36A H 0.661217 0.080912 0.432459 0.087 Uiso 1 1 calc R U . . . H36B H 0.604836 0.018818 0.433101 0.087 Uiso 1 1 calc R U . . . C37 C 0.7403(8) 0.0135(6) 0.4113(2) 0.104(3) Uani 1 1 d . . . . . H37A H 0.716974 0.022502 0.389571 0.156 Uiso 1 1 calc R U . . . H37B H 0.745435 -0.029304 0.413959 0.156 Uiso 1 1 calc R U . . . H37C H 0.804537 0.031573 0.414538 0.156 Uiso 1 1 calc R U . . . C38 C 0.5396(8) 0.0720(5) 0.6066(2) 0.098(3) Uani 1 1 d . . . . . H38A H 0.600550 0.094973 0.609140 0.117 Uiso 1 1 calc R U . . . H38B H 0.554165 0.029692 0.610159 0.117 Uiso 1 1 calc R U . . . C39 C 0.4627(12) 0.0931(8) 0.6295(3) 0.162(6) Uani 1 1 d . . . . . H39A H 0.398950 0.092470 0.618798 0.243 Uiso 1 1 calc R U . . . H39B H 0.477772 0.133527 0.636266 0.243 Uiso 1 1 calc R U . . . H39C H 0.461002 0.067281 0.648351 0.243 Uiso 1 1 calc R U . . . C40 C 0.7900(5) -0.0043(3) 0.5244(2) 0.0625(19) Uani 1 1 d . . . . . H40A H 0.795213 -0.031462 0.505870 0.075 Uiso 1 1 calc R U . . . H40B H 0.790686 -0.028618 0.544199 0.075 Uiso 1 1 calc R U . . . C41 C 0.3980(5) 0.1802(3) 0.45814(16) 0.0504(15) Uani 1 1 d . . . . . C42 C 0.3299(5) 0.1430(3) 0.44497(16) 0.0591(18) Uani 1 1 d . . . . . H42 H 0.271918 0.134545 0.456621 0.071 Uiso 1 1 calc R U . . . C43 C 0.3439(6) 0.1171(4) 0.41448(19) 0.070(2) Uani 1 1 d . . . . . H43 H 0.296361 0.090636 0.406239 0.083 Uiso 1 1 calc R U . . . C44 C 0.4257(6) 0.1297(3) 0.39653(17) 0.0636(19) Uani 1 1 d . . . . . C45 C 0.4943(6) 0.1691(4) 0.40980(18) 0.068(2) Uani 1 1 d . . . . . H45 H 0.551222 0.178788 0.397862 0.081 Uiso 1 1 calc R U . . . C46 C 0.4807(5) 0.1940(3) 0.43976(17) 0.0609(18) Uani 1 1 d . . . . . H46 H 0.527736 0.220837 0.447994 0.073 Uiso 1 1 calc R U . . . C49 C 0.4439(5) 0.0993(3) 0.36568(12) 0.090(2) Uani 1 1 d G U . . . C50 C 0.5390(4) 0.0872(4) 0.35609(15) 0.116(3) Uani 1 1 d G U . . . H50 H 0.592330 0.100084 0.368876 0.139 Uiso 1 1 calc R U . . . C51 C 0.5560(4) 0.0563(4) 0.32778(17) 0.131(3) Uani 1 1 d G U . . . H51 H 0.621032 0.048070 0.321229 0.157 Uiso 1 1 calc R U . . . N2 N 0.4780(5) 0.0375(4) 0.30907(14) 0.130(3) Uani 1 1 d G U . . . C47 C 0.3829(5) 0.0496(4) 0.31866(15) 0.123(3) Uani 1 1 d G U . . . H47 H 0.329553 0.036698 0.305871 0.148 Uiso 1 1 calc R U . . . C48 C 0.3658(4) 0.0805(4) 0.34696(15) 0.107(3) Uani 1 1 d G U . . . H48 H 0.300850 0.088712 0.353519 0.129 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 I1 0.123(2) 0.129(2) 0.0981(17) 0.0276(14) -0.0194(13) -0.0086(15) I2 0.159(8) 0.167(10) 0.184(10) 0.044(7) -0.003(6) 0.008(6) I3 0.090(4) 0.290(10) 0.326(13) -0.050(9) -0.018(6) 0.065(5) I4 0.053(2) 0.171(6) 0.367(11) -0.053(6) 0.034(4) 0.002(3) I5 0.232(10) 0.035(2) 0.295(12) -0.004(4) 0.034(8) -0.047(4) I6 0.172(4) 0.081(2) 0.169(3) -0.023(2) -0.027(3) 0.059(3) I7 0.0515(14) 0.0873(19) 0.264(6) -0.060(3) 0.052(2) -0.0200(13) I8 0.0624(9) 0.1042(13) 0.207(3) 0.0117(14) -0.0015(12) -0.0056(8) I9 0.104(7) 0.208(11) 0.284(15) -0.012(10) -0.029(9) 0.068(8) Cu1 0.226(3) 0.191(2) 0.0898(12) -0.0799(14) -0.0298(14) -0.0152(19) O1 0.068(3) 0.076(3) 0.080(4) -0.011(3) -0.016(3) -0.020(3) O2 0.060(3) 0.064(3) 0.059(3) -0.004(2) 0.003(2) -0.009(2) O3 0.072(3) 0.071(3) 0.061(3) -0.001(2) 0.005(3) 0.015(3) O4 0.054(3) 0.071(3) 0.075(3) -0.015(3) 0.007(3) 0.005(2) O5 0.185(13) 0.138(12) 0.138(12) -0.058(9) -0.027(9) 0.005(9) O5A 0.382(18) 0.163(11) 0.103(9) -0.045(8) -0.066(11) 0.088(13) O6 0.191(13) 0.124(11) 0.074(9) -0.039(8) -0.056(10) 0.011(11) O6A 0.197(15) 0.148(13) 0.082(10) -0.021(10) -0.059(12) 0.015(13) O6B 0.177(15) 0.127(13) 0.069(10) -0.036(10) -0.032(11) -0.018(12) N1 0.158(6) 0.139(6) 0.092(5) -0.045(5) -0.025(5) 0.007(5) C1 0.154(7) 0.135(7) 0.086(6) -0.043(5) -0.037(5) 0.016(6) C1A 0.152(8) 0.132(8) 0.084(7) -0.041(6) -0.033(6) 0.012(7) C2 0.151(7) 0.129(7) 0.078(5) -0.040(5) -0.037(5) 0.013(6) C2A 0.147(8) 0.128(8) 0.079(7) -0.040(6) -0.032(6) 0.011(7) C3 0.131(6) 0.116(6) 0.065(4) -0.038(4) -0.024(4) 0.004(5) C4 0.131(7) 0.116(6) 0.073(5) -0.045(5) -0.020(5) 0.009(6) C4A 0.138(8) 0.121(7) 0.077(6) -0.045(6) -0.018(6) 0.009(7) C5 0.142(7) 0.124(7) 0.083(6) -0.044(5) -0.017(5) 0.011(6) C5A 0.142(8) 0.127(7) 0.083(7) -0.045(6) -0.019(6) 0.008(7) C6 0.082(6) 0.085(6) 0.057(5) -0.013(4) -0.005(4) -0.010(5) C7 0.091(6) 0.073(5) 0.063(5) -0.011(4) -0.018(4) 0.006(5) C8 0.073(5) 0.057(4) 0.064(5) -0.002(3) -0.014(4) 0.005(4) C9 0.050(4) 0.052(4) 0.051(4) -0.006(3) -0.001(3) -0.006(3) C10 0.053(4) 0.072(5) 0.062(4) -0.021(4) -0.001(3) -0.007(4) C11 0.067(5) 0.096(6) 0.065(5) -0.028(4) 0.007(4) -0.004(5) C12 0.040(3) 0.047(3) 0.049(3) -0.001(3) -0.001(3) -0.004(3) C13 0.045(3) 0.046(3) 0.049(4) 0.001(3) 0.000(3) -0.005(3) C14 0.038(3) 0.039(3) 0.061(4) -0.005(3) 0.003(3) -0.002(3) C15 0.044(3) 0.041(3) 0.052(4) -0.008(3) -0.001(3) -0.001(3) C16 0.043(3) 0.046(3) 0.051(4) 0.000(3) -0.001(3) -0.005(3) C17 0.040(3) 0.044(3) 0.052(4) -0.007(3) -0.004(3) -0.007(3) C18 0.043(3) 0.046(3) 0.062(4) -0.008(3) -0.004(3) 0.002(3) C19 0.041(3) 0.040(3) 0.067(4) -0.002(3) -0.004(3) 0.003(3) C20 0.057(4) 0.049(4) 0.064(4) 0.000(3) -0.002(3) -0.003(3) C21 0.050(4) 0.045(4) 0.081(5) -0.003(3) -0.009(4) -0.005(3) C22 0.050(4) 0.036(3) 0.085(5) 0.003(3) -0.005(4) 0.002(3) C23 0.045(4) 0.047(4) 0.076(5) 0.003(3) 0.001(3) -0.001(3) C24 0.051(4) 0.041(3) 0.060(4) -0.004(3) -0.002(3) 0.007(3) C25 0.072(5) 0.071(5) 0.059(4) 0.000(4) 0.006(4) 0.001(4) C26 0.083(6) 0.107(7) 0.072(6) 0.000(5) 0.003(5) 0.002(5) C27 0.116(8) 0.121(8) 0.066(6) 0.006(5) -0.012(6) -0.043(7) C28 0.178(13) 0.174(13) 0.086(8) -0.003(8) -0.034(8) -0.096(11) C29 0.047(4) 0.041(3) 0.067(4) -0.004(3) 0.004(3) 0.001(3) C30 0.046(3) 0.036(3) 0.067(4) -0.005(3) 0.001(3) -0.003(3) C31 0.058(4) 0.042(3) 0.063(4) -0.002(3) 0.004(3) 0.001(3) C32 0.060(4) 0.041(3) 0.068(5) 0.000(3) -0.005(4) -0.001(3) C33 0.044(4) 0.038(3) 0.082(5) -0.006(3) 0.002(4) -0.004(3) C34 0.053(4) 0.038(3) 0.076(5) -0.012(3) 0.011(4) -0.004(3) C35 0.048(4) 0.041(3) 0.070(4) -0.011(3) -0.001(3) -0.002(3) C36 0.071(5) 0.070(5) 0.075(5) -0.007(4) 0.013(4) 0.005(4) C37 0.080(6) 0.145(10) 0.086(7) -0.019(6) 0.018(5) 0.013(7) C38 0.108(8) 0.119(8) 0.066(6) 0.000(5) -0.005(5) 0.032(7) C39 0.175(15) 0.222(17) 0.089(8) -0.010(9) 0.013(9) 0.063(13) C40 0.045(4) 0.044(4) 0.098(6) -0.003(4) -0.004(4) 0.003(3) C41 0.054(4) 0.048(4) 0.049(4) -0.004(3) 0.004(3) -0.003(3) C42 0.060(4) 0.065(4) 0.052(4) -0.013(3) 0.008(3) -0.012(4) C43 0.074(5) 0.072(5) 0.064(5) -0.018(4) 0.002(4) -0.019(4) C44 0.077(5) 0.062(4) 0.052(4) -0.012(3) 0.011(4) -0.007(4) C45 0.066(5) 0.080(5) 0.058(4) -0.006(4) 0.014(4) -0.016(4) C46 0.057(4) 0.067(4) 0.059(4) -0.011(3) 0.010(3) -0.012(4) C49 0.090(5) 0.120(6) 0.060(4) -0.030(4) 0.014(4) -0.010(5) C50 0.107(6) 0.154(7) 0.087(5) -0.047(5) 0.017(5) 0.005(6) C51 0.123(7) 0.172(7) 0.098(6) -0.063(5) 0.016(5) 0.013(6) N2 0.131(6) 0.168(7) 0.091(5) -0.061(5) 0.016(5) 0.003(6) C47 0.126(6) 0.159(7) 0.086(5) -0.052(5) 0.012(5) -0.017(6) C48 0.110(6) 0.142(7) 0.070(5) -0.042(5) 0.012(5) -0.020(5) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cu Cu -1.9646 0.5888 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.3257 6.8362 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag I2 I2 I2 64.1(13) 4_556 3_656 ? I2 I2 I2 62.5(13) 4_556 2_655 ? I2 I2 I2 53.5(12) 3_656 2_655 ? O5A Cu1 O6B 131.5(10) . . ? O6 Cu1 O5 100.3(11) . . ? N1 Cu1 O5 89.5(7) . . ? N1 Cu1 O5A 86.7(5) . . ? N1 Cu1 O6 90.9(6) . . ? N1 Cu1 O6A 95.3(7) . . ? N1 Cu1 O6B 88.9(6) . . ? N2 Cu1 O5 90(2) 8_666 . ? N2 Cu1 O5A 93(3) 8_666 . ? N2 Cu1 O6 89(3) 8_666 . ? N2 Cu1 O6A 85(3) 8_666 . ? N2 Cu1 O6B 91(3) 8_666 . ? N2 Cu1 N1 180(2) 8_666 . ? C21 O1 C27 119.2(6) . . ? C24 O2 C25 117.0(6) . . ? C31 O3 C38 119.0(6) . . ? C34 O4 C36 120.6(6) . . ? Cu1 O5 H5A 127.3 . . ? Cu1 O5 H5B 128.2 . . ? H5A O5 H5B 104.5 . . ? Cu1 O5A H5AA 128.1 . . ? Cu1 O5A H5AB 126.9 . . ? H5AA O5A H5AB 104.5 . . ? Cu1 O6 H6A 127.5 . . ? Cu1 O6 H6B 127.9 . . ? H6A O6 H6B 104.6 . . ? Cu1 O6A H6AA 127.5 . . ? Cu1 O6A H6AB 128.0 . . ? H6AA O6A H6AB 104.4 . . ? Cu1 O6B H6BA 128.2 . . ? Cu1 O6B H6BB 127.2 . . ? H6BA O6B H6BB 104.6 . . ? C1 N1 Cu1 122.7(9) . . ? C1 N1 C5 118.0(11) . . ? C1A N1 Cu1 118.4(13) . . ? C1A N1 C5A 122(2) . . ? C5 N1 Cu1 119.3(9) . . ? C5A N1 Cu1 119.9(18) . . ? N1 C1 H1 119.0 . . ? N1 C1 C2 122.0(14) . . ? C2 C1 H1 119.0 . . ? N1 C1A H1A 125.2 . . ? N1 C1A C2A 110(3) . . ? C2A C1A H1A 125.2 . . ? C1 C2 H2 119.0 . . ? C3 C2 C1 122.0(14) . . ? C3 C2 H2 119.0 . . ? C1A C2A H2A 114.0 . . ? C1A C2A C3 132(3) . . ? C3 C2A H2A 114.0 . . ? C2 C3 C4 115.2(10) . . ? C2 C3 C6 123.5(11) . . ? C2A C3 C4A 116(2) . . ? C2A C3 C6 123.9(17) . . ? C4 C3 C6 120.8(10) . . ? C4A C3 C6 120.1(18) . . ? C3 C4 H4 119.6 . . ? C3 C4 C5 120.7(13) . . ? C5 C4 H4 119.6 . . ? C3 C4A H4A 122.5 . . ? C3 C4A C5A 115(3) . . ? C5A C4A H4A 122.5 . . ? N1 C5 C4 121.8(14) . . ? N1 C5 H5 119.1 . . ? C4 C5 H5 119.1 . . ? N1 C5A C4A 126(4) . . ? N1 C5A H5AC 117.1 . . ? C4A C5A H5AC 117.1 . . ? C7 C6 C3 121.1(9) . . ? C7 C6 C11 118.2(7) . . ? C11 C6 C3 120.7(9) . . ? C6 C7 H7 119.5 . . ? C8 C7 C6 120.9(8) . . ? C8 C7 H7 119.5 . . ? C7 C8 H8 119.6 . . ? C7 C8 C9 120.8(8) . . ? C9 C8 H8 119.6 . . ? C8 C9 C12 118.7(6) . . ? C10 C9 C8 117.8(6) . . ? C10 C9 C12 123.5(6) . . ? C9 C10 H10 119.0 . . ? C9 C10 C11 122.1(7) . . ? C11 C10 H10 119.0 . . ? C6 C11 H11 120.1 . . ? C10 C11 C6 119.9(8) . . ? C10 C11 H11 120.1 . . ? C13 C12 C9 118.5(6) . . ? C13 C12 C17 118.9(6) . . ? C17 C12 C9 122.6(6) . . ? C12 C13 H13 118.7 . . ? C12 C13 C14 122.6(6) . . ? C14 C13 H13 118.7 . . ? C13 C14 C29 118.1(6) . . ? C15 C14 C13 118.6(6) . . ? C15 C14 C29 123.3(6) . . ? C14 C15 C16 118.4(6) . . ? C14 C15 C41 122.8(6) . . ? C16 C15 C41 118.7(6) . . ? C15 C16 H16 118.7 . . ? C17 C16 C15 122.7(6) . . ? C17 C16 H16 118.7 . . ? C12 C17 C18 123.2(6) . . ? C16 C17 C12 118.7(6) . . ? C16 C17 C18 118.1(6) . . ? C17 C18 H18A 108.7 . . ? C17 C18 H18B 108.7 . . ? H18A C18 H18B 107.6 . . ? C19 C18 C17 114.4(5) . . ? C19 C18 H18A 108.7 . . ? C19 C18 H18B 108.7 . . ? C20 C19 C18 121.2(6) . . ? C20 C19 C24 117.6(6) . . ? C24 C19 C18 121.2(6) . . ? C19 C20 H20 119.4 . . ? C19 C20 C21 121.3(7) . . ? C21 C20 H20 119.4 . . ? O1 C21 C20 123.3(7) . . ? O1 C21 C22 117.0(6) . . ? C22 C21 C20 119.7(7) . . ? C21 C22 C40 119.8(7) . 2_655 ? C23 C22 C21 118.9(6) . . ? C23 C22 C40 121.2(7) . 2_655 ? C22 C23 H23 119.4 . . ? C22 C23 C24 121.3(7) . . ? C24 C23 H23 119.4 . . ? O2 C24 C19 115.2(6) . . ? C23 C24 O2 123.6(6) . . ? C23 C24 C19 121.2(6) . . ? O2 C25 H25A 110.3 . . ? O2 C25 H25B 110.3 . . ? O2 C25 C26 107.0(7) . . ? H25A C25 H25B 108.6 . . ? C26 C25 H25A 110.3 . . ? C26 C25 H25B 110.3 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26B 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? O1 C27 H27A 110.2 . . ? O1 C27 H27B 110.2 . . ? O1 C27 C28 107.4(9) . . ? H27A C27 H27B 108.5 . . ? C28 C27 H27A 110.2 . . ? C28 C27 H27B 110.2 . . ? 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 . . ? C14 C29 H29A 108.5 . . ? C14 C29 H29B 108.5 . . ? H29A C29 H29B 107.5 . . ? C30 C29 C14 115.3(5) . . ? C30 C29 H29A 108.5 . . ? C30 C29 H29B 108.5 . . ? C31 C30 C29 120.8(6) . . ? C35 C30 C29 120.2(6) . . ? C35 C30 C31 119.0(6) . . ? O3 C31 C30 116.0(6) . . ? O3 C31 C32 123.4(7) . . ? C30 C31 C32 120.4(7) . . ? C31 C32 H32 119.4 . . ? C33 C32 C31 121.1(7) . . ? C33 C32 H32 119.4 . . ? C32 C33 C34 118.4(6) . . ? C32 C33 C40 120.2(7) . . ? C34 C33 C40 121.3(7) . . ? O4 C34 C33 116.5(6) . . ? O4 C34 C35 122.8(7) . . ? C33 C34 C35 120.7(7) . . ? C30 C35 C34 120.3(7) . . ? C30 C35 H35 119.8 . . ? C34 C35 H35 119.8 . . ? O4 C36 H36A 110.1 . . ? O4 C36 H36B 110.1 . . ? O4 C36 C37 108.2(7) . . ? H36A C36 H36B 108.4 . . ? C37 C36 H36A 110.1 . . ? C37 C36 H36B 110.1 . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37B 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? O3 C38 H38A 110.9 . . ? O3 C38 H38B 110.9 . . ? O3 C38 C39 104.3(9) . . ? 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 . . ? C22 C40 H40A 108.6 2_655 . ? C22 C40 H40B 108.6 2_655 . ? C33 C40 C22 114.8(6) . 2_655 ? C33 C40 H40A 108.6 . . ? C33 C40 H40B 108.6 . . ? H40A C40 H40B 107.6 . . ? C42 C41 C15 122.7(6) . . ? C42 C41 C46 118.0(6) . . ? C46 C41 C15 119.3(6) . . ? C41 C42 H42 119.3 . . ? C41 C42 C43 121.5(7) . . ? C43 C42 H42 119.3 . . ? C42 C43 H43 119.6 . . ? C44 C43 C42 120.9(7) . . ? C44 C43 H43 119.6 . . ? C43 C44 C45 117.5(7) . . ? C43 C44 C49 120.8(7) . . ? C45 C44 C49 121.5(7) . . ? C44 C45 H45 119.3 . . ? C46 C45 C44 121.5(7) . . ? C46 C45 H45 119.3 . . ? C41 C46 H46 119.7 . . ? C45 C46 C41 120.7(7) . . ? C45 C46 H46 119.7 . . ? C50 C49 C44 119.9(5) . . ? C50 C49 C48 120.0 . . ? C48 C49 C44 120.0(5) . . ? C49 C50 H50 120.0 . . ? C51 C50 C49 120.0 . . ? C51 C50 H50 120.0 . . ? C50 C51 H51 120.0 . . ? C50 C51 N2 120.0 . . ? N2 C51 H51 120.0 . . ? C51 N2 Cu1 121.0(4) . 8_655 ? C51 N2 C47 120.0 . . ? C47 N2 Cu1 118.9(4) . 8_655 ? N2 C47 H47 120.0 . . ? C48 C47 N2 120.0 . . ? C48 C47 H47 120.0 . . ? C49 C48 H48 120.0 . . ? C47 C48 C49 120.0 . . ? C47 C48 H48 120.0 . . ? 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 I2 I2 1.03(2) 4_556 ? I2 I2 1.14(2) 3_656 ? I2 I2 1.16(2) 2_655 ? I3 I3 2.40(3) 2_655 ? I4 I4 2.562(15) 2_655 ? I5 I5 2.645(11) 2_655 ? I6 I6 2.701(7) 2_655 ? I7 I7 1.950(7) 2_655 ? I8 I8 2.779(4) 2_655 ? I9 I9 1.61(3) 2_655 ? Cu1 O5 2.273(17) . ? Cu1 O5A 2.152(13) . ? Cu1 O6 2.195(15) . ? Cu1 O6A 2.215(16) . ? Cu1 O6B 2.240(16) . ? Cu1 N1 2.018(9) . ? Cu1 N2 2.016(18) 8_666 ? O1 C21 1.370(8) . ? O1 C27 1.416(10) . ? O2 C24 1.390(8) . ? O2 C25 1.419(9) . ? O3 C31 1.382(8) . ? O3 C38 1.414(10) . ? O4 C34 1.372(8) . ? O4 C36 1.393(10) . ? O5 H5A 0.8700 . ? O5 H5B 0.8694 . ? O5A H5AA 0.8694 . ? O5A H5AB 0.8702 . ? O6 H6A 0.8698 . ? O6 H6B 0.8697 . ? O6A H6AA 0.8702 . ? O6A H6AB 0.8705 . ? O6B H6BA 0.8704 . ? O6B H6BB 0.8701 . ? N1 C1 1.307(17) . ? N1 C1A 1.389(10) . ? N1 C5 1.329(17) . ? N1 C5A 1.390(10) . ? C1 H1 0.9500 . ? C1 C2 1.381(16) . ? C1A H1A 0.9500 . ? C1A C2A 1.390(10) . ? C2 H2 0.9500 . ? C2 C3 1.364(17) . ? C2A H2A 0.9500 . ? C2A C3 1.391(10) . ? C3 C4 1.367(17) . ? C3 C4A 1.391(10) . ? C3 C6 1.458(11) . ? C4 H4 0.9500 . ? C4 C5 1.399(15) . ? C4A H4A 0.9500 . ? C4A C5A 1.392(10) . ? C5 H5 0.9500 . ? C5A H5AC 0.9500 . ? C6 C7 1.395(12) . ? C6 C11 1.409(12) . ? C7 H7 0.9500 . ? C7 C8 1.390(10) . ? C8 H8 0.9500 . ? C8 C9 1.405(10) . ? C9 C10 1.387(10) . ? C9 C12 1.488(9) . ? C10 H10 0.9500 . ? C10 C11 1.387(10) . ? C11 H11 0.9500 . ? C12 C13 1.379(9) . ? C12 C17 1.391(9) . ? C13 H13 0.9500 . ? C13 C14 1.398(9) . ? C14 C15 1.382(9) . ? C14 C29 1.532(8) . ? C15 C16 1.402(9) . ? C15 C41 1.489(9) . ? C16 H16 0.9500 . ? C16 C17 1.377(9) . ? C17 C18 1.515(9) . ? C18 H18A 0.9900 . ? C18 H18B 0.9900 . ? C18 C19 1.503(9) . ? C19 C20 1.393(9) . ? C19 C24 1.399(9) . ? C20 H20 0.9500 . ? C20 C21 1.409(10) . ? C21 C22 1.401(10) . ? C22 C23 1.374(10) . ? C22 C40 1.513(9) 2_655 ? C23 H23 0.9500 . ? C23 C24 1.388(9) . ? C25 H25A 0.9900 . ? C25 H25B 0.9900 . ? C25 C26 1.504(12) . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9900 . ? C27 H27B 0.9900 . ? C27 C28 1.502(13) . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 H29A 0.9900 . ? C29 H29B 0.9900 . ? C29 C30 1.512(9) . ? C30 C31 1.391(10) . ? C30 C35 1.380(9) . ? C31 C32 1.396(10) . ? C32 H32 0.9500 . ? C32 C33 1.382(10) . ? C33 C34 1.389(10) . ? C33 C40 1.481(9) . ? C34 C35 1.410(10) . ? C35 H35 0.9500 . ? C36 H36A 0.9900 . ? C36 H36B 0.9900 . ? C36 C37 1.509(11) . ? C37 H37A 0.9800 . ? C37 H37B 0.9800 . ? C37 H37C 0.9800 . ? C38 H38A 0.9900 . ? C38 H38B 0.9900 . ? C38 C39 1.500(15) . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 H40A 0.9900 . ? C40 H40B 0.9900 . ? C41 C42 1.372(9) . ? C41 C46 1.403(9) . ? C42 H42 0.9500 . ? C42 C43 1.411(10) . ? C43 H43 0.9500 . ? C43 C44 1.376(11) . ? C44 C45 1.411(11) . ? C44 C49 1.478(8) . ? C45 H45 0.9500 . ? C45 C46 1.381(10) . ? C46 H46 0.9500 . ? C49 C50 1.3900 . ? C49 C48 1.3900 . ? C50 H50 0.9500 . ? C50 C51 1.3900 . ? C51 H51 0.9500 . ? C51 N2 1.3900 . ? N2 C47 1.3900 . ? C47 H47 0.9500 . ? C47 C48 1.3900 . ? C48 H48 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 N1 C1 C2 177.8(13) . . . . ? Cu1 N1 C1A C2A 179.8(7) . . . . ? Cu1 N1 C5 C4 -176.1(12) . . . . ? Cu1 N1 C5A C4A -179.8(8) . . . . ? Cu1 N2 C47 C48 177.2(6) 8_655 . . . ? O1 C21 C22 C23 178.2(6) . . . . ? O1 C21 C22 C40 -3.1(9) . . . 2_655 ? O3 C31 C32 C33 177.9(6) . . . . ? O4 C34 C35 C30 177.8(6) . . . . ? N1 C1 C2 C3 -2(3) . . . . ? N1 C1A C2A C3 0.00(16) . . . . ? C1 N1 C5 C4 4(2) . . . . ? C1 C2 C3 C4 5(2) . . . . ? C1 C2 C3 C6 177.0(14) . . . . ? C1A N1 C5A C4A 0.0(3) . . . . ? C1A C2A C3 C4A 0.0(3) . . . . ? C1A C2A C3 C6 177.0(10) . . . . ? C2 C3 C4 C5 -3(2) . . . . ? C2 C3 C6 C7 -27.3(18) . . . . ? C2 C3 C6 C11 152.6(13) . . . . ? C2A C3 C4A C5A 0.0(4) . . . . ? C2A C3 C6 C7 25.6(17) . . . . ? C2A C3 C6 C11 -154.5(13) . . . . ? C3 C4 C5 N1 -1(2) . . . . ? C3 C4A C5A N1 0.0(4) . . . . ? C3 C6 C7 C8 -173.5(9) . . . . ? C3 C6 C11 C10 175.4(9) . . . . ? C4 C3 C6 C7 144.0(12) . . . . ? C4 C3 C6 C11 -36.0(17) . . . . ? C4A C3 C6 C7 -157.5(14) . . . . ? C4A C3 C6 C11 22.4(17) . . . . ? C5 N1 C1 C2 -3(3) . . . . ? C5A N1 C1A C2A 0.00(14) . . . . ? C6 C3 C4 C5 -175.5(13) . . . . ? C6 C3 C4A C5A -177.1(10) . . . . ? C6 C7 C8 C9 -3.0(13) . . . . ? C7 C6 C11 C10 -4.7(13) . . . . ? C7 C8 C9 C10 -2.4(11) . . . . ? C7 C8 C9 C12 176.1(7) . . . . ? C8 C9 C10 C11 4.3(12) . . . . ? C8 C9 C12 C13 60.1(9) . . . . ? C8 C9 C12 C17 -117.7(7) . . . . ? C9 C10 C11 C6 -0.7(13) . . . . ? C9 C12 C13 C14 -177.0(6) . . . . ? C9 C12 C17 C16 174.0(6) . . . . ? C9 C12 C17 C18 -2.7(9) . . . . ? C10 C9 C12 C13 -121.4(8) . . . . ? C10 C9 C12 C17 60.8(9) . . . . ? C11 C6 C7 C8 6.6(13) . . . . ? C12 C9 C10 C11 -174.2(7) . . . . ? C12 C13 C14 C15 3.2(9) . . . . ? C12 C13 C14 C29 -177.9(6) . . . . ? C12 C17 C18 C19 85.6(8) . . . . ? C13 C12 C17 C16 -3.8(9) . . . . ? C13 C12 C17 C18 179.5(6) . . . . ? C13 C14 C15 C16 -4.2(9) . . . . ? C13 C14 C15 C41 172.7(6) . . . . ? C13 C14 C29 C30 -83.0(8) . . . . ? C14 C15 C16 C17 1.3(9) . . . . ? C14 C15 C41 C42 69.1(9) . . . . ? C14 C15 C41 C46 -109.3(8) . . . . ? C14 C29 C30 C31 89.6(8) . . . . ? C14 C29 C30 C35 -93.4(7) . . . . ? C15 C14 C29 C30 95.9(8) . . . . ? C15 C16 C17 C12 2.8(9) . . . . ? C15 C16 C17 C18 179.7(6) . . . . ? C15 C41 C42 C43 -175.6(7) . . . . ? C15 C41 C46 C45 176.2(7) . . . . ? C16 C15 C41 C42 -114.1(8) . . . . ? C16 C15 C41 C46 67.5(9) . . . . ? C16 C17 C18 C19 -91.1(7) . . . . ? C17 C12 C13 C14 0.9(10) . . . . ? C17 C18 C19 C20 -98.5(7) . . . . ? C17 C18 C19 C24 84.5(8) . . . . ? C18 C19 C20 C21 -177.6(6) . . . . ? C18 C19 C24 O2 -1.1(8) . . . . ? C18 C19 C24 C23 176.9(6) . . . . ? C19 C20 C21 O1 -178.6(6) . . . . ? C19 C20 C21 C22 1.6(10) . . . . ? C20 C19 C24 O2 -178.2(6) . . . . ? C20 C19 C24 C23 -0.3(9) . . . . ? C20 C21 C22 C23 -2.0(10) . . . . ? C20 C21 C22 C40 176.7(6) . . . 2_655 ? C21 O1 C27 C28 178.3(9) . . . . ? C21 C22 C23 C24 1.2(10) . . . . ? C22 C23 C24 O2 177.6(6) . . . . ? C22 C23 C24 C19 -0.1(10) . . . . ? C24 O2 C25 C26 177.3(6) . . . . ? C24 C19 C20 C21 -0.5(10) . . . . ? C25 O2 C24 C19 -174.4(6) . . . . ? C25 O2 C24 C23 7.7(9) . . . . ? C27 O1 C21 C20 0.1(11) . . . . ? C27 O1 C21 C22 180.0(8) . . . . ? C29 C14 C15 C16 177.0(6) . . . . ? C29 C14 C15 C41 -6.2(10) . . . . ? C29 C30 C31 O3 -2.6(9) . . . . ? C29 C30 C31 C32 172.7(6) . . . . ? C29 C30 C35 C34 -174.6(6) . . . . ? C30 C31 C32 C33 2.9(10) . . . . ? C31 O3 C38 C39 177.2(9) . . . . ? C31 C30 C35 C34 2.4(9) . . . . ? C31 C32 C33 C34 0.3(10) . . . . ? C31 C32 C33 C40 -177.7(6) . . . . ? C32 C33 C34 O4 -179.4(6) . . . . ? C32 C33 C34 C35 -2.2(9) . . . . ? C32 C33 C40 C22 -93.9(8) . . . 2_655 ? C33 C34 C35 C30 0.8(9) . . . . ? C34 O4 C36 C37 -176.7(7) . . . . ? C34 C33 C40 C22 88.1(8) . . . 2_655 ? C35 C30 C31 O3 -179.6(6) . . . . ? C35 C30 C31 C32 -4.3(9) . . . . ? C36 O4 C34 C33 177.9(6) . . . . ? C36 O4 C34 C35 0.8(10) . . . . ? C38 O3 C31 C30 -177.7(8) . . . . ? C38 O3 C31 C32 7.1(11) . . . . ? C40 C22 C23 C24 -177.4(6) 2_655 . . . ? C40 C33 C34 O4 -1.3(9) . . . . ? C40 C33 C34 C35 175.9(6) . . . . ? C41 C15 C16 C17 -175.7(6) . . . . ? C41 C42 C43 C44 -1.8(13) . . . . ? C42 C41 C46 C45 -2.3(11) . . . . ? C42 C43 C44 C45 0.1(13) . . . . ? C42 C43 C44 C49 175.6(8) . . . . ? C43 C44 C45 C46 0.4(13) . . . . ? C43 C44 C49 C50 -146.8(7) . . . . ? C43 C44 C49 C48 30.3(10) . . . . ? C44 C45 C46 C41 0.7(13) . . . . ? C44 C49 C50 C51 177.1(7) . . . . ? C44 C49 C48 C47 -177.1(7) . . . . ? C45 C44 C49 C50 28.5(10) . . . . ? C45 C44 C49 C48 -154.4(7) . . . . ? C46 C41 C42 C43 2.9(11) . . . . ? C49 C44 C45 C46 -175.0(8) . . . . ? C49 C50 C51 N2 0.0 . . . . ? C50 C49 C48 C47 0.0 . . . . ? C50 C51 N2 Cu1 -177.1(6) . . . 8_655 ? C50 C51 N2 C47 0.0 . . . . ? C51 N2 C47 C48 0.0 . . . . ? N2 C47 C48 C49 0.0 . . . . ? C48 C49 C50 C51 0.0 . . . . ? 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 -0.157 0.552 0.250 1203.4 354.9 '8 DMF,4 H2O' 2 -0.107 0.740 0.750 1203.4 359.1 '8 DMF,4 H2O'