#------------------------------------------------------------------------------ #$Date: 2023-06-29 17:52:52 +0200 (Thu, 29 Jun 2023) $ #$Revision: 284696 $ #$URL: svn://www.crystallography.net/cod/cif/2/02/27/2022798.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/. The original data for this entry # were provided by IUCr Journals, http://journals.iucr.org/. # # The file may be used within the scientific community so long as # proper attribution is given to the journal article from which the # data were obtained. # data_2022798 loop_ _publ_author_name 'Suzuki, Soma' 'Akiyama, Yukihito' 'Nakane, Daisuke' 'Akitsu, Takashiro' _publ_section_title ; Crystal structure and Hirshfeld surface analysis of (1H-imidazole-\kN 3)[N-(2-oxidobenzylidene)tyrosinato-\k3 O,N,O′]copper(II) ; _journal_coeditor_code EX2071 _journal_issue 7 _journal_name_full 'Acta Crystallographica Section E Crystallographic Communications' _journal_paper_doi 10.1107/S2056989023004735 _journal_volume 79 _journal_year 2023 _chemical_absolute_configuration syn _chemical_formula_iupac '[Cu (C16 H13 N O4) (C3 H4 N2)]' _chemical_formula_moiety '[Cu (C16 H13 N O4) (C3 H4 N2)]' _chemical_formula_sum 'C19 H17 Cu N3 O4' _chemical_formula_weight 414.89 _chemical_name_systematic (1H-Imidazole-\kN^3^)[N-(2-oxidobenzylidene)tyrosinato-\k^3^O,N,O']copper(II) _space_group_crystal_system orthorhombic _space_group_IT_number 19 _space_group_name_Hall 'P 2ac 2ab' _space_group_name_H-M_alt 'P 21 21 21' _atom_sites_solution_hydrogens mixed _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 5.5005(2) _cell_length_b 12.1363(5) _cell_length_c 26.1470(10) _cell_measurement_reflns_used 9965 _cell_measurement_temperature 173.(2) _cell_measurement_theta_max 26.3890 _cell_measurement_theta_min 2.8773 _cell_volume 1745.46(12) _computing_cell_refinement ; SAINT V8.40B (Bruker, 2019) ; _computing_data_collection ; APEX2 (Bruker, 2019) ; _computing_data_reduction ; SAINT V8.40B (Bruker, 2019) ; _computing_molecular_graphics ; ShelXle (H\"ubschle et al., 2011) ; _computing_structure_refinement ; SHELXL2018/3 (Sheldrick, 2015b) ; _computing_structure_solution ; SHELXT2018/2 (Sheldrick, 2015a) ; _diffrn_ambient_temperature 173.(2) _diffrn_detector_area_resol_mean 7.3910 _diffrn_measured_fraction_theta_full 0.994 _diffrn_measured_fraction_theta_max 0.994 _diffrn_measurement_device_type 'Bruker D8 QUEST' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0471 _diffrn_reflns_av_unetI/netI 0.0432 _diffrn_reflns_limit_h_max 6 _diffrn_reflns_limit_h_min -6 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_limit_l_min -32 _diffrn_reflns_number 19853 _diffrn_reflns_theta_full 25.00 _diffrn_reflns_theta_max 26.41 _diffrn_reflns_theta_min 1.85 _exptl_absorpt_coefficient_mu 1.283 _exptl_absorpt_correction_T_max 0.78 _exptl_absorpt_correction_T_min 0.55 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; (SADABS; Krause et al., 2015) ; _exptl_crystal_colour black _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_method 'not measured' _exptl_crystal_description prism _exptl_crystal_F_000 852 _exptl_crystal_size_max 0.500 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.200 _refine_diff_density_max 0.334 _refine_diff_density_min -0.210 _refine_ls_abs_structure_details ; Refined as an inversion twin ; _refine_ls_abs_structure_Flack 0.017(12) _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.056 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 251 _refine_ls_number_reflns 3571 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.056 _refine_ls_R_factor_all 0.0255 _refine_ls_R_factor_gt 0.0250 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0276P)^2^+0.2834P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0613 _refine_ls_wR_factor_ref 0.0617 _reflns_number_gt 3501 _reflns_number_total 3571 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file 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18.00 0 2 -30 439.36 34.00 0 2 -30 463.85 37.70 0 -2 30 419.66 31.40 -1 2 -30 188.38 18.20 -1 2 -30 177.88 22.50 -2 2 -30 108.99 13.30 2 1 -30 118.09 11.90 2 1 -30 132.39 15.70 2 1 -30 132.79 13.70 -2 -1 30 108.59 12.70 1 1 -30 41.70 7.20 1 1 -30 27.30 7.90 1 1 -30 22.80 4.70 -1 -1 30 17.50 5.10 0 1 -30 146.69 16.70 0 1 -30 134.89 13.50 0 -1 30 125.19 11.80 -1 1 -30 12.80 6.80 1 -1 30 24.10 4.00 -2 1 -30 96.59 11.80 2 -1 30 103.49 8.70 2 -1 30 110.79 9.70 2 0 -30 102.29 11.70 2 0 -30 88.59 9.90 2 0 -30 76.59 13.30 -2 0 30 83.49 10.50 1 0 -30 611.44 40.90 1 0 -30 546.75 44.40 1 0 -30 540.95 39.70 -1 0 30 506.65 40.20 0 0 -30 62.79 11.60 0 0 -30 59.59 8.40 0 0 30 40.50 6.60 -1 0 -30 579.24 45.00 -1 0 -30 565.64 41.10 1 0 30 516.65 38.50 -2 0 -30 72.29 9.10 2 0 30 84.29 7.60 2 -1 -30 113.59 12.80 2 -1 -30 101.99 15.60 -2 1 30 120.89 12.80 1 -1 -30 21.10 5.20 1 -1 -30 11.80 6.10 -1 1 30 31.50 6.20 0 -1 -30 152.18 13.50 0 -1 -30 143.99 17.00 0 1 30 139.49 13.20 -1 -1 -30 35.60 6.00 -1 -1 -30 21.80 7.50 1 1 30 9.50 3.40 2 1 30 109.29 10.00 2 -2 -30 137.29 13.70 2 -2 -30 105.09 16.80 -2 2 30 113.19 13.30 1 -2 -30 184.68 15.10 1 -2 -30 172.48 19.30 -1 2 30 140.79 15.00 0 -2 -30 429.56 37.70 0 -2 -30 483.55 33.10 0 2 30 422.66 33.10 -1 -2 -30 151.38 18.00 -1 -2 -30 133.19 12.60 1 2 30 171.18 13.70 2 2 30 121.99 11.30 2 -3 -30 102.89 12.10 -2 3 30 110.19 12.40 1 -3 -30 50.09 7.60 -1 3 30 59.19 8.70 0 -3 -30 612.44 53.19 0 -3 -30 648.34 43.70 0 3 30 576.34 44.20 1 3 30 49.80 7.30 2 3 30 103.59 10.50 2 -4 -30 229.48 23.00 2 -4 -30 193.78 19.10 -2 4 30 228.58 20.00 1 -4 -30 52.39 7.40 1 -4 -30 47.50 9.10 -1 4 30 39.90 7.70 0 -4 -30 55.59 6.20 0 -4 -30 44.20 7.20 0 4 30 49.30 7.80 1 4 30 52.99 7.90 2 4 30 229.18 19.00 1 -5 -30 151.08 13.90 1 -5 -30 132.09 14.80 -1 5 30 139.89 14.30 0 -5 -30 35.60 4.70 0 -5 -30 34.80 5.40 0 5 30 25.60 6.20 1 5 30 145.89 14.20 0 6 30 1.90 3.50 1 4 -31 84.69 8.30 1 4 -31 90.49 12.00 -1 -4 31 105.69 9.90 0 4 -31 10.60 5.50 -1 4 -31 91.89 14.10 1 3 -31 131.49 11.20 1 3 -31 141.19 16.20 -1 -3 31 122.69 12.30 0 3 -31 41.10 8.30 0 -3 31 44.60 5.50 -1 3 -31 130.39 15.10 2 2 -31 49.10 10.60 1 2 -31 106.69 16.60 1 2 -31 141.29 11.60 1 2 -31 137.79 13.90 -1 -2 31 113.19 12.30 0 2 -31 212.28 19.20 0 -2 31 201.38 16.50 -1 2 -31 130.19 14.60 2 1 -31 152.78 18.90 2 1 -31 199.98 17.70 2 1 -31 159.88 15.30 -2 -1 31 196.18 17.30 1 1 -31 73.49 8.10 1 1 -31 84.69 9.80 1 1 -31 74.59 13.50 -1 -1 31 62.59 9.10 0 1 -31 -0.50 3.30 0 -1 31 4.10 2.80 -1 1 -31 60.99 9.80 1 -1 31 63.89 6.60 -2 1 -31 203.58 17.70 2 -1 31 157.88 12.80 2 0 -31 9.00 5.00 -2 0 31 6.00 3.90 1 0 -31 79.39 9.50 1 0 -31 59.69 13.50 -1 0 31 68.39 9.40 0 0 -31 4.90 3.50 -1 0 -31 83.09 10.00 1 0 31 73.89 8.00 -2 0 -31 7.00 3.00 2 0 31 8.10 2.70 2 -1 -31 208.88 18.00 -2 1 31 159.08 16.90 1 -1 -31 74.99 9.20 -1 1 31 71.79 9.90 0 -1 -31 3.80 5.50 0 1 31 5.20 3.20 -1 -1 -31 81.49 9.30 2 1 31 203.38 16.20 1 -2 -31 135.39 12.50 -1 2 31 115.49 12.50 0 -2 -31 224.58 17.20 0 2 31 178.68 16.90 -1 -2 -31 130.49 11.60 1 2 31 125.69 11.90 1 -3 -31 146.69 12.60 -1 3 31 104.39 12.60 0 -3 -31 41.70 6.10 0 3 31 31.80 6.40 1 3 31 113.39 11.30 1 -4 -31 81.09 12.70 1 -4 -31 106.29 10.10 -1 4 31 82.29 10.60 0 -4 -31 3.60 2.60 0 -4 -31 12.00 3.40 0 4 31 5.40 3.50 1 4 31 108.79 11.40 0 3 -32 4.10 4.50 0 -3 32 2.40 2.20 1 2 -32 84.89 11.00 -1 -2 32 88.79 9.90 0 2 -32 252.07 22.40 0 -2 32 250.77 19.60 -1 2 -32 104.69 12.80 1 1 -32 238.48 19.00 -1 -1 32 174.08 17.30 0 1 -32 1.50 3.60 0 -1 32 1.00 2.40 -1 1 -32 193.88 18.60 1 -1 32 201.58 15.50 1 0 -32 181.88 16.10 -1 0 32 160.68 15.50 0 0 -32 360.56 27.80 0 0 32 336.07 26.40 -1 0 -32 185.38 16.40 1 0 32 156.88 13.80 1 -1 -32 212.68 18.10 -1 1 32 204.18 18.40 0 -1 -32 -2.60 2.60 0 1 32 1.00 2.70 -1 -1 -32 222.48 17.40 1 1 32 167.38 15.60 1 -2 -32 114.19 10.80 -1 2 32 67.99 10.50 0 -2 -32 282.67 21.00 0 2 32 230.48 20.70 -1 -2 -32 88.19 8.90 1 2 32 99.09 9.80 0 -3 -32 1.80 2.70 0 3 32 1.40 3.00 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 46212 _shelx_res_file ; TITL Tyr_Imi_2_0m_a.res in P2(1)2(1)2(1) Tyr_Imi_2_0m_a.res created by SHELXL-2018/3 at 10:32:21 on 07-Jan-2023 REM Old TITL Tyr_Imi_2_0m in P2(1)2(1)2(1) REM SHELXT solution in P2(1)2(1)2(1): R1 0.079, Rweak 0.027, Alpha 0.005 REM 2.414 for 26 systematic absences, Orientation as input REM Flack x = 0.033 ( 0.006 ) from 1426 Parsons' quotients REM Formula found by SHELXT: C20 Cu N O5 CELL 0.71073 5.5005 12.1363 26.1470 90.000 90.000 90.000 ZERR 4.000 0.0002 0.0005 0.0010 0.000 0.000 0.000 LATT -1 SYMM 1/2-X, -Y, 1/2+Z SYMM -X, 1/2+Y, 1/2-Z SYMM 1/2+X, 1/2-Y, -Z SFAC C H CU N O UNIT 76 68 4 12 16 TEMP -100 ACTA 50 SIZE 0.5 0.3 0.2 HTAB L.S. 10 BOND LIST 4 FMAP 2 PLAN 20 TWIN WGHT 0.027600 0.283400 BASF 0.01683 FVAR 0.68869 CU1 3 0.674677 0.469815 0.560468 11.00000 0.03258 0.02037 = 0.01908 0.00198 0.00109 0.00257 O1 5 0.893869 0.350047 0.556145 11.00000 0.04179 0.02974 = 0.02872 0.00891 0.01079 0.00864 N1 4 0.932900 0.664273 0.445519 11.00000 0.07500 0.02709 = 0.02390 0.00517 0.00612 -0.00989 H11 2 0.951028 0.717379 0.431723 11.00000 0.03064 C1 1 0.542091 0.316520 0.639343 11.00000 0.03386 0.02232 = 0.02274 -0.00082 0.00330 0.00044 AFIX 43 H1 2 0.429138 0.291841 0.664328 11.00000 -1.20000 AFIX 0 O2 5 0.429411 0.585261 0.564090 11.00000 0.03963 0.02562 = 0.02071 0.00277 -0.00042 0.00610 N2 4 0.834622 0.540822 0.502266 11.00000 0.04108 0.02364 = 0.02173 0.00126 -0.00062 -0.00162 C2 1 0.739726 0.244566 0.627158 11.00000 0.03609 0.02013 = 0.02359 -0.00018 -0.00012 0.00159 N3 4 0.504249 0.412123 0.619266 11.00000 0.02949 0.02177 = 0.02275 0.00006 0.00128 0.00343 O3 5 0.114358 0.646493 0.607356 11.00000 0.05374 0.04266 = 0.03457 0.00592 0.00555 0.02452 C3 1 0.767655 0.149647 0.657884 11.00000 0.04335 0.02427 = 0.03040 0.00462 0.00349 0.00228 AFIX 43 H3 2 0.654313 0.136020 0.684559 11.00000 -1.20000 AFIX 0 O4 5 0.308851 0.220655 0.856802 11.00000 0.03610 0.03640 = 0.02969 0.00984 0.00020 0.00089 AFIX 148 H4A 2 0.190871 0.191346 0.858343 11.00000 -1.50000 AFIX 0 C4 1 0.954384 0.076751 0.650124 11.00000 0.04886 0.02183 = 0.03590 0.00590 -0.00228 0.00418 AFIX 43 H4 2 0.973698 0.014587 0.671828 11.00000 -1.20000 AFIX 0 C5 1 1.115054 0.095228 0.609989 11.00000 0.03780 0.02424 = 0.04287 -0.00029 -0.00132 0.00902 AFIX 43 H5 2 1.244308 0.044786 0.604282 11.00000 -1.20000 AFIX 0 C6 1 1.090413 0.185384 0.578298 11.00000 0.03767 0.02956 = 0.03400 0.00188 0.00677 0.00358 AFIX 43 H6 2 1.200419 0.194846 0.550635 11.00000 -1.20000 AFIX 0 C7 1 0.905029 0.263749 0.586195 11.00000 0.03376 0.02079 = 0.02684 -0.00073 -0.00109 0.00191 C8 1 1.047307 0.509141 0.477971 11.00000 0.03320 0.03570 = 0.02613 0.00163 -0.00102 -0.00304 AFIX 43 H8 2 1.136848 0.443916 0.484952 11.00000 -1.20000 AFIX 0 C9 1 1.106472 0.585640 0.442917 11.00000 0.04349 0.04228 = 0.02610 -0.00062 0.00314 -0.01054 AFIX 43 H9 2 1.243185 0.584623 0.420719 11.00000 -1.20000 AFIX 0 C10 1 0.771864 0.635769 0.481337 11.00000 0.05932 0.02521 = 0.02716 0.00051 0.00494 0.00278 AFIX 43 H10 2 0.632492 0.677619 0.490455 11.00000 -1.20000 AFIX 0 C11 1 0.275107 0.578005 0.600064 11.00000 0.03594 0.02517 = 0.02294 -0.00335 -0.00435 0.00496 C12 1 0.297274 0.478986 0.636430 11.00000 0.03155 0.02309 = 0.02393 -0.00172 0.00294 0.00352 AFIX 13 H12 2 0.145376 0.433906 0.634481 11.00000 -1.20000 AFIX 0 C13 1 0.328360 0.523287 0.691539 11.00000 0.04439 0.02231 = 0.02361 -0.00082 0.00538 0.00165 AFIX 23 H13A 2 0.485063 0.563191 0.693498 11.00000 -1.20000 H13B 2 0.197503 0.577417 0.698212 11.00000 -1.20000 AFIX 0 C14 1 0.323331 0.437907 0.733468 11.00000 0.02964 0.02302 = 0.02163 -0.00271 0.00441 0.00249 C15 1 0.513477 0.430858 0.768357 11.00000 0.02567 0.03264 = 0.02883 -0.00224 0.00449 -0.00340 AFIX 43 H15 2 0.651326 0.477154 0.764186 11.00000 -1.20000 AFIX 0 C16 1 0.506477 0.358059 0.808947 11.00000 0.02589 0.03948 = 0.02612 0.00112 -0.00082 0.00042 AFIX 43 H16 2 0.638341 0.354933 0.832366 11.00000 -1.20000 AFIX 0 C17 1 0.307715 0.289727 0.815525 11.00000 0.02968 0.02356 = 0.02202 0.00022 0.00265 0.00347 C18 1 0.118381 0.292828 0.780486 11.00000 0.02786 0.02550 = 0.02955 0.00011 0.00164 -0.00429 AFIX 43 H18 2 -0.016298 0.244436 0.784071 11.00000 -1.20000 AFIX 0 C19 1 0.127102 0.367315 0.740050 11.00000 0.02789 0.03069 = 0.02390 -0.00069 -0.00347 -0.00097 AFIX 43 H19 2 -0.004041 0.369920 0.716438 11.00000 -1.20000 REM ##### AFIX 0 HKLF 4 REM Tyr_Imi_2_0m_a.res in P2(1)2(1)2(1) REM wR2 = 0.061718, GooF = S = 1.05622, Restrained GooF = 1.05622 for all data REM R1 = 0.024958 for 3501 Fo > 4sig(Fo) and 0.025511 for all 3571 data REM 251 parameters refined using 0 restraints END WGHT 0.0276 0.2834 REM Instructions for potential hydrogen bonds EQIV $1 x+1/2, -y+3/2, -z+1 HTAB N1 O2_$1 EQIV $2 -x+3/2, -y+1, z-1/2 HTAB N1 O4_$2 EQIV $3 -x, y-1/2, -z+3/2 HTAB O4 O3_$3 EQIV $4 -x+1, y+1/2, -z+3/2 HTAB C13 O4_$4 REM Highest difference peak 0.334, deepest hole -0.210, 1-sigma level 0.055 Q1 1 0.5119 0.4719 0.5620 11.00000 0.05 0.33 Q2 1 0.3276 0.4755 0.7125 11.00000 0.05 0.28 Q3 1 0.2601 0.2791 0.7886 11.00000 0.05 0.27 Q4 1 0.3242 0.5752 0.5753 11.00000 0.05 0.27 Q5 1 0.8464 0.4733 0.5617 11.00000 0.05 0.26 Q6 1 0.9066 0.3202 0.5706 11.00000 0.05 0.23 Q7 1 0.4365 0.3011 0.8015 11.00000 0.05 0.23 Q8 1 0.9151 0.3362 0.5459 11.00000 0.05 0.22 Q9 1 0.4976 0.3861 0.7863 11.00000 0.05 0.22 Q10 1 0.5334 0.3791 0.6367 11.00000 0.05 0.22 Q11 1 0.7689 0.2437 0.6047 11.00000 0.05 0.21 Q12 1 0.7661 0.2105 0.6395 11.00000 0.05 0.21 Q13 1 0.4959 0.5623 0.5622 11.00000 0.05 0.20 Q14 1 0.4029 0.5942 0.5445 11.00000 0.05 0.20 Q15 1 1.0477 0.2371 0.5914 11.00000 0.05 0.20 Q16 1 0.2828 0.5225 0.6130 11.00000 0.05 0.20 Q17 1 0.3456 0.5795 0.5421 11.00000 0.05 0.19 Q18 1 0.9905 0.6161 0.4437 11.00000 0.05 0.19 Q19 1 0.2995 0.4954 0.6652 11.00000 0.05 0.19 Q20 1 0.2021 0.4169 0.7410 11.00000 0.05 0.19 ; _shelx_res_checksum 6688 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' loop_ _atom_site_type_symbol _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_calc_flag _atom_site_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Cu Cu1 0.67468(5) 0.46981(2) 0.56047(2) 0.02401(11) Uani d 1 . . O O1 0.8939(3) 0.35005(15) 0.55615(7) 0.0334(4) Uani d 1 . . N N1 0.9329(6) 0.6643(2) 0.44552(9) 0.0420(6) Uani d 1 . . H H11 0.951(6) 0.717(3) 0.4317(12) 0.031(8) Uiso d 1 . . C C1 0.5421(5) 0.3165(2) 0.63934(9) 0.0263(5) Uani d 1 . . H H1 0.429138 0.291841 0.664328 0.032 Uiso calc 1 . . O O2 0.4294(3) 0.58526(14) 0.56409(7) 0.0287(4) Uani d 1 . . N N2 0.8346(4) 0.54082(17) 0.50227(7) 0.0288(4) Uani d 1 . . C C2 0.7397(5) 0.2446(2) 0.62716(9) 0.0266(5) Uani d 1 . . N N3 0.5042(4) 0.41212(17) 0.61927(8) 0.0247(4) Uani d 1 . . O O3 0.1144(4) 0.64649(19) 0.60736(8) 0.0437(5) Uani d 1 . . C C3 0.7677(6) 0.1496(2) 0.65788(10) 0.0327(6) Uani d 1 . . H H3 0.654313 0.13602 0.684559 0.039 Uiso calc 1 . . O O4 0.3089(4) 0.22066(16) 0.85680(7) 0.0341(4) Uani d 1 . . H H4A 0.191(7) 0.191(3) 0.8583(9) 0.051 Uiso calc 1 . . C C4 0.9544(6) 0.0768(2) 0.65012(11) 0.0355(6) Uani d 1 . . H H4 0.973698 0.014587 0.671828 0.043 Uiso calc 1 . . C C5 1.1151(5) 0.0952(2) 0.60999(11) 0.0350(6) Uani d 1 . . H H5 1.244308 0.044786 0.604282 0.042 Uiso calc 1 . . C C6 1.0904(5) 0.1854(2) 0.57830(11) 0.0337(6) Uani d 1 . . H H6 1.200419 0.194846 0.550635 0.04 Uiso calc 1 . . C C7 0.9050(5) 0.2637(2) 0.58620(9) 0.0271(5) Uani d 1 . . C C8 1.0473(5) 0.5091(2) 0.47797(9) 0.0317(6) Uani d 1 . . H H8 1.136848 0.443916 0.484952 0.038 Uiso calc 1 . . C C9 1.1065(5) 0.5856(2) 0.44292(10) 0.0373(6) Uani d 1 . . H H9 1.243185 0.584623 0.420719 0.045 Uiso calc 1 . . C C10 0.7719(6) 0.6358(2) 0.48134(10) 0.0372(7) Uani d 1 . . H H10 0.632492 0.677619 0.490455 0.045 Uiso calc 1 . . C C11 0.2751(5) 0.5780(2) 0.60006(9) 0.0280(5) Uani d 1 . . C C12 0.2973(5) 0.4790(2) 0.63643(8) 0.0262(5) Uani d 1 . . H H12 0.145376 0.433906 0.634481 0.031 Uiso calc 1 . . C C13 0.3284(5) 0.5233(2) 0.69154(8) 0.0301(5) Uani d 1 . . H H13A 0.485063 0.563191 0.693498 0.036 Uiso calc 1 . . H H13B 0.197503 0.577417 0.698212 0.036 Uiso calc 1 . . C C14 0.3233(5) 0.43791(19) 0.73347(8) 0.0248(5) Uani d 1 . . C C15 0.5135(5) 0.4309(2) 0.76836(10) 0.0290(6) Uani d 1 . . H H15 0.651326 0.477154 0.764186 0.035 Uiso calc 1 . . C C16 0.5065(5) 0.3581(2) 0.80895(10) 0.0305(5) Uani d 1 . . H H16 0.638341 0.354933 0.832366 0.037 Uiso calc 1 . . C C17 0.3077(5) 0.28973(19) 0.81552(8) 0.0251(5) Uani d 1 . . C C18 0.1184(5) 0.2928(2) 0.78049(9) 0.0276(5) Uani d 1 . . H H18 -0.016298 0.244436 0.784071 0.033 Uiso calc 1 . . C C19 0.1271(5) 0.3673(2) 0.74005(9) 0.0275(5) Uani d 1 . . H H19 -0.004041 0.36992 0.716438 0.033 Uiso calc 1 . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Cu1 0.03258(17) 0.02037(15) 0.01908(14) 0.00257(12) 0.00109(11) 0.00198(11) O1 0.0418(10) 0.0297(9) 0.0287(9) 0.0086(8) 0.0108(8) 0.0089(8) N1 0.0750(19) 0.0271(12) 0.0239(11) -0.0099(12) 0.0061(12) 0.0052(10) C1 0.0339(14) 0.0223(12) 0.0227(11) 0.0004(11) 0.0033(10) -0.0008(9) O2 0.0396(9) 0.0256(8) 0.0207(8) 0.0061(7) -0.0004(8) 0.0028(7) N2 0.0411(12) 0.0236(10) 0.0217(9) -0.0016(11) -0.0006(9) 0.0013(8) C2 0.0361(14) 0.0201(11) 0.0236(11) 0.0016(10) -0.0001(9) -0.0002(9) N3 0.0295(11) 0.0218(10) 0.0228(9) 0.0034(9) 0.0013(8) 0.0001(8) O3 0.0537(14) 0.0427(11) 0.0346(10) 0.0245(11) 0.0055(9) 0.0059(9) C3 0.0434(16) 0.0243(12) 0.0304(13) 0.0023(12) 0.0035(11) 0.0046(10) O4 0.0361(10) 0.0364(10) 0.0297(9) 0.0009(9) 0.0002(9) 0.0098(8) C4 0.0489(17) 0.0218(12) 0.0359(14) 0.0042(12) -0.0023(13) 0.0059(11) C5 0.0378(15) 0.0242(13) 0.0429(15) 0.0090(12) -0.0013(12) -0.0003(11) C6 0.0377(15) 0.0296(14) 0.0340(13) 0.0036(12) 0.0068(11) 0.0019(11) C7 0.0338(13) 0.0208(12) 0.0268(12) 0.0019(10) -0.0011(10) -0.0007(10) C8 0.0332(14) 0.0357(14) 0.0261(12) -0.0030(11) -0.0010(10) 0.0016(10) C9 0.0435(15) 0.0423(15) 0.0261(12) -0.0105(13) 0.0031(12) -0.0006(12) C10 0.0593(19) 0.0252(12) 0.0272(12) 0.0028(13) 0.0049(12) 0.0005(10) C11 0.0359(14) 0.0252(12) 0.0229(11) 0.0050(11) -0.0043(10) -0.0033(9) C12 0.0316(12) 0.0231(11) 0.0239(11) 0.0035(12) 0.0029(9) -0.0017(9) C13 0.0444(14) 0.0223(11) 0.0236(11) 0.0016(13) 0.0054(11) -0.0008(10) C14 0.0296(13) 0.0230(11) 0.0216(10) 0.0025(10) 0.0044(10) -0.0027(8) C15 0.0257(13) 0.0326(13) 0.0288(12) -0.0034(11) 0.0045(10) -0.0022(10) C16 0.0259(12) 0.0395(14) 0.0261(12) 0.0004(12) -0.0008(10) 0.0011(11) C17 0.0297(12) 0.0236(11) 0.0220(10) 0.0035(11) 0.0027(10) 0.0002(9) C18 0.0279(13) 0.0255(12) 0.0296(12) -0.0043(10) 0.0016(10) 0.0001(10) C19 0.0279(14) 0.0307(13) 0.0239(11) -0.0010(11) -0.0035(9) -0.0007(10) 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_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle _geom_angle_publ_flag O1 Cu1 N3 . . 94.49(8) ? O1 Cu1 O2 . . 175.72(8) ? N3 Cu1 O2 . . 83.45(8) ? O1 Cu1 N2 . . 90.31(8) ? N3 Cu1 N2 . . 174.98(9) ? O2 Cu1 N2 . . 91.86(8) ? C7 O1 Cu1 . . 127.44(16) ? C10 N1 C9 . . 108.7(2) ? N3 C1 C2 . . 125.5(2) ? C11 O2 Cu1 . . 116.69(16) ? C10 N2 C8 . . 105.8(2) ? C10 N2 Cu1 . . 126.0(2) ? C8 N2 Cu1 . . 127.85(18) ? C3 C2 C7 . . 119.4(2) ? C3 C2 C1 . . 117.0(2) ? C7 C2 C1 . . 123.6(2) ? C1 N3 C12 . . 119.8(2) ? C1 N3 Cu1 . . 124.84(18) ? C12 N3 Cu1 . . 114.78(15) ? C4 C3 C2 . . 121.6(3) ? C3 C4 C5 . . 118.9(2) ? C6 C5 C4 . . 121.3(3) ? C5 C6 C7 . . 121.2(2) ? O1 C7 C6 . . 119.0(2) ? O1 C7 C2 . . 123.5(2) ? C6 C7 C2 . . 117.5(2) ? C9 C8 N2 . . 109.0(3) ? C8 C9 N1 . . 106.4(3) ? N2 C10 N1 . . 110.1(3) ? O3 C11 O2 . . 123.3(2) ? O3 C11 C12 . . 119.3(2) ? O2 C11 C12 . . 117.3(2) ? N3 C12 C11 . . 107.73(19) ? N3 C12 C13 . . 113.0(2) ? C11 C12 C13 . . 108.25(19) ? C14 C13 C12 . . 115.8(2) ? C19 C14 C15 . . 117.7(2) ? C19 C14 C13 . . 121.9(2) ? C15 C14 C13 . . 120.3(2) ? C16 C15 C14 . . 121.5(3) ? C15 C16 C17 . . 120.1(3) ? O4 C17 C16 . . 117.5(2) ? O4 C17 C18 . . 122.8(2) ? C16 C17 C18 . . 119.7(2) ? C17 C18 C19 . . 119.6(2) ? C14 C19 C18 . . 121.4(2) ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_site_symmetry_2 _geom_bond_distance _geom_bond_publ_flag Cu1 O1 . 1.8919(18) yes Cu1 N3 . 1.932(2) yes Cu1 O2 . 1.9473(17) yes Cu1 N2 . 1.958(2) yes O1 C7 . 1.311(3) ? N1 C10 . 1.335(4) ? N1 C9 . 1.352(4) ? C1 N3 . 1.290(3) ? C1 C2 . 1.430(4) ? O2 C11 . 1.270(3) ? N2 C10 . 1.322(4) yes N2 C8 . 1.386(4) ? C2 C3 . 1.413(3) ? C2 C7 . 1.424(4) ? N3 C12 . 1.468(3) ? O3 C11 . 1.228(3) ? C3 C4 . 1.371(4) ? O4 C17 . 1.367(3) ? C4 C5 . 1.390(4) ? C5 C6 . 1.379(4) ? C6 C7 . 1.410(4) ? C8 C9 . 1.345(4) ? C11 C12 . 1.537(3) ? C12 C13 . 1.547(3) ? C13 C14 . 1.509(3) ? C14 C19 . 1.389(4) ? C14 C15 . 1.390(4) ? C15 C16 . 1.381(4) ? C16 C17 . 1.383(4) ? C17 C18 . 1.388(4) ? C18 C19 . 1.392(4) ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_site_symmetry_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_publ_flag N1 H11 O2 4_566 0.75(4) 2.40(4) 3.050(3) 147.(3) yes N1 H11 O4 2_664 0.75(4) 2.48(3) 3.058(3) 136.(3) yes O4 H4A O3 3_546 0.74 1.98 2.666(3) 154.0 yes C13 H13A O4 3_656 0.99 2.58 3.364(3) 135.9 yes _cod_database_fobs_code 2022798