#------------------------------------------------------------------------------ #$Date: 2024-12-06 19:30:55 +0200 (Fri, 06 Dec 2024) $ #$Revision: 296464 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/24/93/7249373.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_7249373 loop_ _publ_author_name 'Chen, Jiali' 'Fu, Yuying' 'Liu, Qiaoyun' 'Shen, Shoujie' 'Liu, Jinjian' _publ_section_title ; Design and synthesis of two functional coordination polymers based on the 1,1′-bis(3-carboxybenzyl)-4,4′-bipyridinium ligand ; _journal_issue 39 _journal_name_full CrystEngComm _journal_page_first 5518 _journal_page_last 5524 _journal_paper_doi 10.1039/D4CE00732H _journal_volume 26 _journal_year 2024 _chemical_formula_moiety 'C18 H13 N O7 Zn' _chemical_formula_sum 'C18 H13 N O7 Zn' _chemical_formula_weight 420.66 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_creation_date 2024-08-08 _audit_creation_method ; Olex2 1.5 (compiled 2024.02.16 svn.r378c4104 for OlexSys, GUI svn.r6928) ; _audit_update_record ; 2024-08-08 deposited with the CCDC. 2024-09-16 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 99.246(3) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.9146(4) _cell_length_b 10.0980(3) _cell_length_c 15.0368(4) _cell_measurement_reflns_used 6211 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 27.0350 _cell_measurement_theta_min 4.0290 _cell_volume 1635.76(9) _computing_cell_refinement 'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)' _computing_data_collection 'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)' _computing_data_reduction 'CrysAlisPro 1.171.41.123a (Rigaku OD, 2022)' _computing_molecular_graphics 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.5 (Dolomanov et al., 2009)' _computing_structure_refinement 'SHELXL 2018/3 (Sheldrick, 2015)' _computing_structure_solution 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 293(2) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0710 _diffrn_detector_type Eos _diffrn_measured_fraction_theta_full 0.998 _diffrn_measured_fraction_theta_max 0.935 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -73.00 -22.00 1.00 5.00 -- -18.75 126.00 96.00 51 2 \w 10.00 37.00 1.00 5.00 -- 20.16-145.00-147.00 27 3 \w 49.00 74.00 1.00 5.00 -- 20.16-126.00 19.00 25 4 \w -2.00 32.00 1.00 5.00 -- 20.16-126.00 19.00 34 5 \w -32.00 -6.00 1.00 5.00 -- -18.75 -38.00 60.00 26 6 \w -88.00 -60.00 1.00 5.00 -- -18.75 -38.00 60.00 28 7 \w -82.00 -57.00 1.00 5.00 -- -18.75 145.00 -96.00 25 8 \w -19.00 11.00 1.00 5.00 -- -18.75 -99.00-150.00 30 9 \w 6.00 87.00 1.00 5.00 -- 20.16 57.00 150.00 81 10 \w 0.00 74.00 1.00 5.00 -- 20.16-125.00 87.03 74 11 \w -25.00 58.00 1.00 5.00 -- 20.16 -99.00 -60.00 83 12 \w -25.00 59.00 1.00 5.00 -- 20.16 -99.00-150.00 84 13 \w 1.00 89.00 1.00 5.00 -- 20.16 38.00-120.00 88 14 \w 28.00 89.00 1.00 5.00 -- 20.16 38.00 -60.00 61 15 \w 17.00 87.00 1.00 5.00 -- 20.16 57.00 60.00 70 16 \w -2.00 88.00 1.00 5.00 -- 20.16 77.00 -30.00 90 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'Xcalibur, Eos, Gemini' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0029669000 _diffrn_orient_matrix_UB_12 -0.0591621000 _diffrn_orient_matrix_UB_13 0.0256600000 _diffrn_orient_matrix_UB_21 0.0057064000 _diffrn_orient_matrix_UB_22 0.0378486000 _diffrn_orient_matrix_UB_23 0.0401962000 _diffrn_orient_matrix_UB_31 -0.0655409000 _diffrn_orient_matrix_UB_32 0.0006253000 _diffrn_orient_matrix_UB_33 -0.0030582000 _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_radiation_type 'Mo K\a' _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0451 _diffrn_reflns_av_unetI/netI 0.0370 _diffrn_reflns_Laue_measured_fraction_full 0.998 _diffrn_reflns_Laue_measured_fraction_max 0.935 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_number 34381 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.935 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.965 _diffrn_reflns_theta_min 3.219 _diffrn_source 'fine-focus sealed X-ray tube' _diffrn_source_type 'Enhance (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 1.546 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.86042 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.41.123a (Rigaku Oxford Diffraction, 2022) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.708 _exptl_crystal_description block _exptl_crystal_F_000 856 _exptl_crystal_size_max 0.3 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _refine_diff_density_max 0.507 _refine_diff_density_min -0.806 _refine_diff_density_rms 0.069 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.022 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 282 _refine_ls_number_reflns 4871 _refine_ls_number_restraints 96 _refine_ls_restrained_S_all 1.056 _refine_ls_R_factor_all 0.0899 _refine_ls_R_factor_gt 0.0481 _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^)+(0.0400P)^2^+1.9713P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1009 _refine_ls_wR_factor_ref 0.1195 _reflns_Friedel_coverage 0.000 _reflns_number_gt 3118 _reflns_number_total 4871 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4ce00732h2.cif _cod_data_source_block exp_437_auto _cod_depositor_comments 'Adding full bibliography for 7249372--7249373.cif.' _cod_database_code 7249373 _shelx_shelxl_version_number 2018/3 _chemical_oxdiff_formula 'C H O N' _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 0.747 _shelx_estimated_absorpt_t_min 0.654 _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 O(H,H) groups 2. Restrained distances O7-C17 = C17-O21 1.25 with sigma of 0.02 O6-C17 = C17-O20 1.25 with sigma of 0.02 O4-C14 = C14-O5 1.25 with sigma of 0.02 O8-C14 = C14-O9 1.25 with sigma of 0.02 O7-O21 2.165 with sigma of 0.04 O6-O20 2.165 with sigma of 0.04 O4-O5 2.165 with sigma of 0.04 O8-O9 2.165 with sigma of 0.04 3. Uiso/Uaniso restraints and constraints C8 \\sim N1 \\sim C9 \\sim C11 \\sim C13 \\sim C12 \\sim C10 \\sim C7: within 2A with sigma of 0.01 and sigma for terminal atoms of 0.02 within 2A 4. Rigid body (RIGU) restrains O4, C14, O5 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 O8, C14, O9 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 O20, C17, O6 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 O21, C17, O7 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 5. Others Sof(O7)=Sof(O21)=Sof(O8)=Sof(O9)=1-FVAR(1) Sof(O6)=Sof(O4)=Sof(O5)=Sof(O20)=FVAR(1) 6.a Rotating group: O3(H3A,H3B) 6.b Secondary CH2 refined with riding coordinates: C8(H8A,H8B) 6.c Aromatic/amide H refined with riding coordinates: C18(H18), C3(H3), C4(H4), C5(H5), C6(H6), C9(H9), C11(H11), C12(H12), C10(H10) ; _shelx_res_file ; TITL exp_437_auto_a.res in P2(1)/n exp_437_auto.res created by SHELXL-2018/3 at 00:03:15 on 08-Aug-2024 REM Old TITL exp_437_auto in P2(1)/n REM SHELXT solution in P2(1)/n: R1 0.302, Rweak 0.157, Alpha 0.047 REM 0.500 for 200 systematic absences, Orientation as input REM Formula found by SHELXT: C19 N5 O3 Br CELL 0.71073 10.9146 10.098 15.0368 90 99.246 90 ZERR 4 0.0004 0.0003 0.0004 0 0.003 0 LATT 1 SYMM 0.5-X,0.5+Y,0.5-Z SFAC C H N O Zn UNIT 72 52 4 28 4 DFIX 1.25 O7 C17 C17 O21 DANG 2.165 O7 O21 DFIX 1.25 O6 C17 C17 O20 DANG 2.165 O6 O20 DFIX 1.25 O4 C14 C14 O5 DANG 2.165 O4 O5 DFIX 1.25 O8 C14 C14 O9 DANG 2.165 O8 O9 RIGU 0.001 0.001 O4 C14 O5 RIGU 0.001 0.001 O8 C14 O9 RIGU 0.001 0.001 O20 C17 O6 RIGU 0.001 0.001 O21 C17 O7 SIMU 0.01 0.02 2 C8 N1 C9 C11 C13 C12 C10 C7 L.S. 20 PLAN 2 SIZE 0.3 0.2 0.2 BOND list 4 fmap 2 acta REM REM REM WGHT 0.040000 1.971300 FVAR 0.42244 0.64711 ZN1 5 0.723436 0.434959 0.658963 11.00000 0.06142 0.03021 = 0.04170 -0.00428 -0.02861 -0.00415 O3 4 0.568882 0.546416 0.667051 11.00000 0.07190 0.04323 = 0.05540 0.00285 -0.01256 -0.00151 AFIX 7 H3A 2 0.512367 0.536808 0.618744 11.00000 -1.50000 H3B 2 0.586111 0.631356 0.666235 11.00000 -1.50000 AFIX 0 PART 1 O6 4 0.893402 0.781827 0.852150 21.00000 0.03963 0.02869 = 0.03965 0.00683 -0.00937 0.00615 PART 0 O2 4 0.803638 0.523758 0.566621 11.00000 0.05706 0.07058 = 0.05800 0.00296 -0.01896 0.00181 C16 1 0.928298 0.588631 0.941593 11.00000 0.02720 0.02512 = 0.02282 0.00491 -0.00506 0.00120 O1 4 0.636751 0.472104 0.468460 11.00000 0.05530 0.10821 = 0.06810 0.03096 -0.02006 -0.02399 PART 1 O4 4 0.843738 0.487940 0.763389 21.00000 0.05770 0.03588 = 0.02714 0.00217 -0.01941 -0.00903 PART 0 C17 1 0.850575 0.690477 0.885919 11.00000 0.04134 0.03057 = 0.02539 0.00305 -0.01071 0.00713 C18 1 0.991705 0.630861 1.024872 11.00000 0.03978 0.02250 = 0.02798 -0.00009 -0.00980 0.00172 AFIX 43 H18 2 0.986474 0.719185 1.041380 11.00000 -1.20000 AFIX 0 C15 1 0.937477 0.456381 0.916337 11.00000 0.03218 0.02726 = 0.02206 0.00194 -0.00851 -0.00106 C14 1 0.871656 0.405934 0.826324 11.00000 0.04705 0.02964 = 0.02834 -0.00176 -0.01439 0.00098 C2 1 0.779718 0.626617 0.423816 11.00000 0.04015 0.04902 = 0.05683 -0.00841 0.00071 0.00163 N1 3 0.587249 0.747962 0.159117 11.00000 0.07338 0.09854 = 0.06170 0.04210 0.01356 -0.01028 C3 1 0.692923 0.692840 0.362623 11.00000 0.03852 0.05177 = 0.06229 0.00359 0.00493 0.00194 AFIX 43 H3 2 0.608863 0.677878 0.362691 11.00000 -1.20000 AFIX 0 PART 2 O7 4 0.775832 0.759201 0.906292 -21.00000 0.06239 0.04671 = 0.03781 0.01322 0.00332 0.02605 PART 0 C1 1 0.735003 0.533954 0.489812 11.00000 0.04595 0.06122 = 0.05500 0.00319 -0.00760 0.00790 PART 1 O5 4 0.838267 0.287227 0.819358 21.00000 0.12176 0.03250 = 0.06337 0.00464 -0.05527 -0.01781 PART 0 C7 1 0.729302 0.781863 0.300674 11.00000 0.05278 0.05334 = 0.07857 0.01056 0.01132 -0.00513 C4 1 0.905531 0.648183 0.421217 11.00000 0.03985 0.06638 = 0.08584 -0.01406 -0.00421 0.00556 AFIX 43 H4 2 0.965467 0.604950 0.461947 11.00000 -1.20000 AFIX 0 C5 1 0.941143 0.733726 0.358174 11.00000 0.03990 0.08736 = 0.09978 -0.01934 0.01797 -0.01855 AFIX 43 H5 2 1.025007 0.745765 0.355711 11.00000 -1.20000 AFIX 0 C6 1 0.853727 0.801034 0.299187 11.00000 0.06016 0.07117 = 0.09607 0.00587 0.01909 -0.01795 AFIX 43 H6 2 0.878797 0.859858 0.258042 11.00000 -1.20000 AFIX 0 C13 1 0.518299 0.551171 0.033517 11.00000 0.06106 0.14629 = 0.04636 0.04064 0.01328 -0.01249 C9 1 0.474267 0.696816 0.149708 11.00000 0.06130 0.15629 = 0.06055 0.02260 0.01016 -0.01267 AFIX 43 H9 2 0.418454 0.727593 0.185614 11.00000 -1.20000 AFIX 0 C8 1 0.632265 0.845298 0.231260 11.00000 0.07829 0.06906 = 0.09829 0.04173 0.00899 -0.00711 AFIX 23 H8A 2 0.563362 0.875278 0.259545 11.00000 -1.20000 H8B 2 0.667369 0.921628 0.205334 11.00000 -1.20000 AFIX 0 C11 1 0.438535 0.599309 0.087877 11.00000 0.06118 0.18113 = 0.05870 0.00846 0.01100 -0.02320 AFIX 43 H11 2 0.358666 0.564843 0.082474 11.00000 -1.20000 AFIX 0 C12 1 0.634982 0.607362 0.046372 11.00000 0.07949 0.16260 = 0.10360 0.00200 0.04654 -0.02948 AFIX 43 H12 2 0.693278 0.577911 0.012065 11.00000 -1.20000 AFIX 0 C10 1 0.666189 0.703632 0.107334 11.00000 0.08408 0.14476 = 0.11860 0.00171 0.04015 -0.04002 AFIX 43 H10 2 0.745257 0.740320 0.113497 11.00000 -1.20000 AFIX 0 PART 2 O21 4 0.911139 0.730235 0.817403 -21.00000 0.04955 0.07059 = 0.05088 0.03412 0.00444 0.01486 O8 4 0.780918 0.471999 0.791963 -21.00000 0.05611 0.04915 = 0.03869 -0.01315 -0.03028 0.01026 PART 1 O20 4 0.732221 0.677578 0.888974 21.00000 0.03623 0.07259 = 0.07181 0.03638 -0.00420 0.00950 PART 2 O9 4 0.918921 0.311559 0.794403 -21.00000 0.08765 0.04644 = 0.03135 -0.01053 -0.01315 0.02128 HKLF 4 REM exp_437_auto_a.res in P2(1)/n REM wR2 = 0.1195, GooF = S = 1.022, Restrained GooF = 1.056 for all data REM R1 = 0.0481 for 3118 Fo > 4sig(Fo) and 0.0899 for all 4871 data REM 282 parameters refined using 96 restraints END WGHT 0.0398 1.9722 REM Highest difference peak 0.507, deepest hole -0.806, 1-sigma level 0.069 Q1 1 0.6756 0.4359 0.7002 11.00000 0.05 0.51 Q2 1 0.8249 0.4360 0.0264 11.00000 0.05 0.43 ; _shelx_res_checksum 77929 _shelx_hkl_file ; 0 0 3 1.23 0.88 0 0 -3 0.85 0.60 0 0 -3 1.87 1.06 0 0 3 0.70 0.96 0 0 3 0.62 0.58 0 0 -3 0.23 0.49 0 0 4 2998.85 40.87 0 0 -4 2990.13 40.73 0 0 4 3038.57 45.48 0 0 4 3073.69 45.31 0 0 -4 3009.50 45.14 0 0 4 3039.07 45.24 0 0 -4 3015.62 40.78 0 0 -5 0.63 0.82 0 0 5 -0.52 1.11 0 0 5 -0.84 1.03 0 0 -5 0.33 1.25 0 0 5 0.57 1.54 0 0 -5 0.19 0.70 0 0 -6 1608.68 26.72 0 0 6 1641.44 32.48 0 0 6 1633.96 32.19 0 0 -6 1691.87 27.00 0 0 -6 1648.45 32.23 0 0 -7 0.46 1.74 0 0 7 0.75 1.99 0 0 -7 0.56 0.92 0 0 -7 0.68 0.96 0 0 8 334.60 14.61 0 0 -8 343.68 14.36 0 0 -8 336.00 10.65 0 0 -8 344.52 10.80 0 0 -9 -2.56 2.38 0 0 9 0.67 2.32 0 0 -9 1.13 1.02 0 0 -9 -0.11 1.07 0 0 -10 585.76 16.12 0 0 10 568.64 21.89 0 0 -10 577.66 21.53 0 0 -10 579.62 21.38 0 0 11 1.38 3.26 0 0 -11 2.10 2.87 0 0 -11 0.01 2.54 0 0 -11 0.51 1.19 0 0 -12 405.55 19.50 0 0 -12 411.91 14.38 0 0 12 429.41 20.51 0 0 -12 414.28 19.90 0 0 13 -2.50 3.88 0 0 -13 -0.42 1.41 0 0 -13 2.79 2.82 0 0 14 -5.27 3.57 0 0 -14 1.15 1.95 0 0 -14 -0.04 3.03 0 0 15 -2.74 3.80 0 0 -15 2.95 2.00 0 0 -15 5.26 4.12 0 0 -16 150.58 13.95 0 0 16 142.85 14.13 0 0 16 142.99 13.93 0 0 -17 -0.62 4.07 0 0 17 -2.78 3.47 0 0 -18 3.43 4.09 0 0 18 3.82 4.77 0 0 -19 -3.14 3.91 0 0 19 1.59 5.15 0 0 20 3.75 4.64 0 0 -21 11.52 7.10 0 1 2 886.22 15.88 0 -1 2 826.46 14.68 0 -1 2 866.59 15.46 0 1 3 970.58 14.46 0 -1 -3 964.30 14.46 0 -1 3 987.73 18.12 0 1 -3 978.51 17.96 0 -1 -3 1013.47 19.07 0 1 3 999.44 19.00 0 -1 3 982.57 18.55 0 -1 3 986.50 18.68 0 1 4 25.56 2.94 0 1 4 29.99 3.26 0 -1 4 37.20 3.42 0 -1 -4 31.01 1.95 0 1 -4 35.40 2.85 0 1 4 34.41 1.98 0 1 -4 31.52 3.02 0 -1 -4 34.50 3.31 0 -1 4 31.90 3.19 0 -1 4 31.34 2.97 0 -1 4 31.64 3.05 0 1 4 34.36 2.03 0 -1 5 126.36 6.97 0 1 5 131.62 7.23 0 1 5 131.49 4.46 0 1 -5 129.98 5.98 0 -1 -5 133.78 4.57 0 -1 5 127.80 6.77 0 1 -5 132.33 6.83 0 -1 -5 130.95 7.11 0 1 5 135.72 7.29 0 -1 -5 122.67 6.80 0 -1 5 132.29 7.08 0 -1 5 130.52 6.68 0 1 5 136.48 4.50 0 -1 6 491.53 8.27 0 1 6 500.93 10.72 0 1 -6 494.09 13.21 0 -1 -6 498.76 10.81 0 -1 6 494.47 15.26 0 -1 -6 478.79 15.57 0 1 -6 513.17 15.36 0 -1 6 498.90 15.69 0 1 6 485.39 15.73 0 -1 6 531.60 16.12 0 1 -6 499.43 13.23 0 1 6 492.42 10.64 0 -1 6 492.11 14.61 0 1 -7 1193.91 16.61 0 -1 7 1222.09 28.29 0 1 7 1153.87 27.91 0 1 -7 1181.54 23.86 0 -1 -7 1169.81 20.74 0 1 7 1173.11 20.64 0 -1 7 1167.74 26.23 0 -1 -7 1136.87 27.68 0 1 -7 1189.86 27.26 0 1 -7 1234.04 24.26 0 1 -8 1.28 1.45 0 1 -8 1.26 1.20 0 -1 -8 2.64 1.17 0 1 8 1.74 2.52 0 -1 8 6.88 3.06 0 1 -8 0.10 1.86 0 -1 -8 1.33 2.21 0 -1 9 828.20 25.05 0 1 9 773.01 24.83 0 -1 -9 799.01 24.68 0 1 -9 758.75 23.46 0 1 -9 846.13 20.66 0 -1 -9 787.29 17.32 0 1 -9 778.99 19.98 0 1 -10 4.47 2.08 0 -1 -10 2.92 1.44 0 1 10 11.20 3.97 0 -1 10 2.80 3.17 0 1 -10 1.89 2.38 0 -1 -10 2.11 1.96 0 -1 -10 7.15 2.81 0 1 -11 0.18 1.76 0 -1 -11 0.38 1.24 0 -1 11 -1.62 3.23 0 1 11 0.78 2.69 0 1 11 2.17 3.36 0 -1 -11 3.26 2.93 0 1 -11 4.96 2.77 0 -1 -11 -2.31 2.68 0 1 -12 21.90 3.64 0 1 12 27.31 5.69 0 -1 12 37.48 5.88 0 1 12 25.83 5.48 0 -1 -12 35.32 6.05 0 1 -12 35.09 6.02 0 -1 -12 36.07 6.34 0 -1 -12 33.06 3.66 0 1 13 250.27 16.21 0 1 -13 267.42 12.69 0 -1 -13 241.20 10.32 0 1 13 264.68 16.88 0 -1 13 249.65 16.35 0 1 -13 273.83 16.44 0 -1 -13 265.25 16.55 0 -1 -13 244.53 15.99 0 1 -14 -0.24 1.99 0 -1 -14 2.02 1.81 0 -1 -14 -1.02 3.76 0 -1 14 9.72 5.07 0 1 14 -0.73 3.92 0 1 14 3.33 3.84 0 1 -14 -3.55 3.28 0 -1 -14 2.79 3.02 0 -1 -15 19.90 5.99 0 -1 15 28.32 6.94 0 1 15 29.25 7.08 0 1 -15 16.18 3.51 0 -1 -15 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19.04 3.09 -3 3 8 26.67 3.60 -3 3 7 108.71 7.62 -3 -3 7 99.92 7.02 -3 -3 7 96.09 6.34 -3 3 7 105.64 6.91 3 3 -7 101.18 7.59 3 3 -7 108.85 8.82 3 -3 -7 98.31 7.64 -3 -3 6 2.56 1.34 -3 3 6 2.99 1.65 3 3 -6 4.46 2.29 -3 -3 6 4.30 2.00 3 -3 -6 3.26 1.99 3 3 -6 0.64 1.83 3 -3 -6 7.16 2.02 -3 3 6 1.70 1.75 -3 -3 6 3.79 1.79 -3 3 6 3.09 0.77 3 3 -6 4.50 1.80 3 3 -6 5.68 1.95 3 -3 -6 0.12 2.12 -3 3 6 4.29 1.70 3 3 -5 346.12 13.56 -3 -3 5 366.60 13.68 3 -3 -5 363.51 11.75 -3 3 5 346.26 11.77 -3 -3 5 345.90 12.24 -3 3 5 346.12 13.04 3 -3 -5 356.54 12.88 3 -3 -5 343.15 12.71 -3 3 5 350.97 12.80 3 3 -5 351.31 11.37 -3 -3 5 346.61 11.19 -3 3 5 351.01 8.52 3 3 -5 345.33 12.84 -3 3 5 340.22 12.44 -3 -3 5 344.83 12.34 3 -3 -5 330.72 14.17 -3 -3 4 16.10 2.80 -3 3 4 14.89 2.83 3 3 -4 18.10 3.41 3 -3 -4 15.59 1.47 -3 -3 4 15.44 3.07 -3 -3 4 17.03 2.52 -3 3 4 14.91 2.62 3 -3 -4 19.83 2.96 3 -3 -4 16.84 2.83 -3 3 4 17.72 2.86 -3 -3 4 14.96 2.16 3 3 -4 21.04 2.47 3 3 -4 20.91 3.22 -3 3 4 16.17 2.01 3 -3 -4 12.91 3.05 -3 3 4 13.84 1.91 3 -3 -4 15.58 2.55 -3 -3 4 20.73 3.31 -3 3 4 16.63 2.58 -3 -3 3 1948.96 36.21 -3 3 3 2011.10 36.86 3 -3 -3 1983.85 29.98 -3 -3 3 1978.26 38.21 3 3 -3 1981.68 37.83 3 -3 -3 1955.70 33.64 -3 -3 3 1985.56 35.67 -3 3 3 1997.97 34.00 -3 -3 3 2001.00 32.25 -3 3 3 2040.15 33.79 3 -3 -3 1984.43 33.02 -3 -3 3 2027.06 33.53 3 -3 -3 1972.97 35.67 -3 -3 3 1986.69 30.24 -3 3 3 1994.14 32.18 3 3 -3 2133.49 36.47 -3 -3 3 1928.65 35.82 -3 3 3 2020.54 32.25 3 -3 -3 2049.11 38.95 -3 -3 2 41.21 4.22 3 3 -2 46.32 4.66 3 -3 -2 49.50 3.48 3 3 -2 48.02 4.25 -3 3 2 45.23 3.79 3 -3 -2 51.20 4.05 -3 3 2 43.68 4.45 -3 3 2 44.68 3.27 3 -3 -2 43.66 3.12 3 -3 -2 45.27 4.21 -3 -3 2 52.86 4.05 -3 -3 2 42.67 2.71 -3 3 2 48.99 3.99 -3 -3 2 47.67 4.43 -3 -3 2 44.14 3.99 -3 3 2 39.66 3.45 3 -3 -2 41.29 4.57 -3 3 1 43.47 4.37 -3 3 1 47.95 2.77 3 3 -1 47.15 4.04 -3 -3 1 48.49 4.11 3 -3 -1 47.34 4.73 -3 3 1 47.80 4.13 3 -3 -1 47.90 3.99 -3 -3 1 44.41 4.34 -3 3 1 40.62 3.88 -3 -3 1 48.13 4.39 3 3 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6 10 103.84 12.37 5 -6 10 100.84 11.98 -5 -6 -10 109.31 9.67 -5 6 -10 88.06 10.83 5 6 10 106.92 11.73 -5 -6 -10 90.77 8.72 -5 6 -10 100.60 9.73 -5 -6 -10 109.79 12.18 5 -6 11 93.09 12.27 -5 6 -11 86.55 9.00 -5 6 -11 87.16 11.19 5 6 11 91.10 11.84 -5 -6 -11 103.26 9.65 5 6 11 86.11 10.95 -5 -6 -11 90.14 11.55 -5 -6 -12 -3.67 5.16 -5 -6 -12 1.49 2.54 -5 6 -12 -3.67 4.28 5 -6 12 8.43 5.07 5 6 12 3.40 4.59 5 6 12 -1.41 4.61 -5 6 -13 2.90 3.96 5 -6 13 5.46 4.37 -5 -6 -13 2.34 4.41 5 6 13 2.28 3.47 5 6 13 3.99 4.29 -5 6 -14 42.95 8.83 5 -6 14 36.06 8.66 -5 -6 -14 34.13 7.70 5 6 14 48.00 9.50 5 6 14 15.00 5.38 -5 6 -15 17.38 5.82 5 -6 15 35.34 9.00 -5 -6 -15 14.59 5.77 5 6 15 27.50 7.98 5 6 15 22.63 6.99 -5 6 -16 32.61 7.76 5 -7 -18 -9.89 5.38 5 7 -17 3.29 4.93 5 -7 -17 5.48 5.34 5 7 -17 -1.29 4.28 5 7 -16 -0.95 4.26 -5 -7 16 15.29 7.34 -5 7 16 10.20 5.24 5 -7 -16 -1.59 5.09 5 -7 -15 -4.10 5.72 -5 7 15 1.41 3.88 5 7 -15 -1.64 4.10 -5 -7 15 7.09 4.66 -5 -7 15 3.82 4.82 5 -7 -14 -0.84 3.97 5 7 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8.52 2.88 5 -7 -7 14.67 5.08 -5 7 7 5.03 2.13 -5 -7 7 4.98 3.46 5 -7 -7 6.28 3.30 -5 7 7 7.59 2.56 -5 7 7 8.34 3.60 5 7 -7 8.82 4.43 -5 -7 6 12.31 3.77 -5 -7 6 7.31 2.60 5 -7 -6 6.38 4.41 -5 7 6 10.16 2.80 -5 -7 6 14.37 4.90 5 -7 -6 9.00 4.53 -5 7 6 6.44 2.90 5 7 -6 13.70 4.43 -5 -7 5 -1.08 2.51 -5 -7 5 1.43 2.75 -5 -7 5 -0.07 1.64 5 -7 -5 -2.59 3.23 -5 7 5 1.20 2.10 5 -7 -5 -1.78 2.94 5 7 -5 3.66 3.71 -5 7 5 1.09 2.70 -5 7 4 174.99 13.56 -5 -7 4 193.75 13.73 -5 -7 4 185.76 9.38 -5 7 4 187.56 11.35 -5 -7 4 160.82 11.53 5 -7 -4 174.92 13.69 -5 -7 4 177.83 11.24 5 7 -4 189.42 14.17 5 -7 -4 162.62 12.90 -5 -7 3 64.65 6.46 -5 -7 3 51.57 7.15 5 -7 -3 64.24 8.20 -5 -7 3 62.01 5.31 -5 -7 3 57.18 6.96 -5 7 3 67.80 7.08 5 -7 -3 53.16 8.08 5 7 -3 57.72 7.96 -5 7 3 58.09 8.02 -5 -7 2 78.91 6.07 -5 7 2 79.53 8.96 -5 -7 2 66.74 7.52 -5 7 2 83.01 8.12 5 7 -2 86.93 9.68 -5 -7 2 90.29 7.33 -5 -7 2 92.59 9.66 5 -7 -2 85.08 9.27 5 -7 -1 127.61 11.28 -5 7 1 129.48 10.51 5 -7 -1 124.08 7.19 -5 -7 1 137.16 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-2 -4 8.92 5.99 14 -2 -4 7.82 4.45 -14 2 3 -1.77 3.95 14 2 -3 3.81 4.41 -14 -2 3 12.01 6.70 14 -2 -3 0.62 3.74 -14 -2 3 7.80 5.05 14 2 -2 10.01 5.64 14 -2 -2 -3.63 3.93 14 -2 -2 -9.00 6.43 -14 2 2 0.72 5.30 -14 -2 2 3.71 5.16 -14 2 1 4.57 4.20 14 -2 -1 2.22 3.86 14 2 -1 0.19 3.38 -14 2 1 7.31 6.53 -14 -2 1 4.73 4.81 -14 2 0 7.25 5.00 -14 -2 0 3.41 3.83 14 -2 0 1.48 3.91 14 2 0 3.53 4.02 -14 2 0 20.53 7.40 -14 -2 0 14.17 7.62 -14 2 -1 6.81 6.33 -14 -2 -1 -6.59 6.21 14 -2 1 -1.05 4.33 14 2 1 5.15 4.48 -14 2 -1 1.52 5.71 -14 -2 -1 0.56 5.32 14 2 2 0.52 4.30 -14 2 -2 -6.42 6.20 -14 -2 -2 -3.98 5.04 -14 -2 -2 12.69 6.98 14 2 3 -0.40 4.58 -14 -2 -3 10.65 6.61 -14 -2 -3 -2.25 5.18 14 3 -10 -3.75 4.50 14 3 -9 -3.32 4.93 14 -3 -9 -10.57 5.76 14 3 -8 -8.57 5.04 14 -3 -8 9.01 5.29 14 -3 -7 -0.62 3.43 -14 -3 7 8.36 5.53 -14 -3 7 -1.01 4.23 14 3 -7 -3.11 3.73 -14 -3 7 -3.07 5.91 -14 3 7 6.34 5.28 14 -3 -6 3.08 4.47 14 -3 -6 5.20 4.42 -14 -3 6 -2.10 5.19 -14 -3 6 3.19 4.94 -14 3 6 0.81 4.89 -14 3 6 5.47 5.48 -14 -3 6 6.17 5.77 14 3 -6 -0.60 3.70 14 3 -6 3.45 4.05 14 -3 -5 3.83 3.69 14 -3 -5 9.37 4.89 -14 -3 5 -2.53 4.50 -14 -3 5 -0.98 4.50 -14 3 5 -2.03 5.72 -14 -3 5 -4.04 5.34 14 3 -5 -4.89 4.42 14 3 -5 0.16 3.99 -14 -3 4 0.62 5.55 -14 -3 4 5.30 5.65 -14 3 4 8.84 7.08 -14 -3 4 -5.24 6.07 14 3 -4 4.63 4.27 14 -3 -4 -5.26 3.93 14 -3 -4 8.53 5.79 -14 -3 3 10.55 6.19 14 3 -3 0.40 3.20 -14 3 3 9.74 5.61 -14 -3 3 -4.56 6.01 14 -3 -3 3.19 4.24 -14 3 3 -2.22 4.54 -14 -3 3 -2.21 5.08 -14 3 2 3.23 5.04 -14 3 2 2.46 5.23 14 3 -2 1.99 4.15 -14 -3 2 0.62 4.84 -14 -3 2 0.76 4.35 14 -3 -2 12.29 6.69 -14 3 1 2.70 4.95 -14 -3 1 4.03 4.84 -14 3 1 -0.93 4.81 14 3 -1 -4.01 4.23 -14 -3 1 -0.68 4.12 -14 -3 1 1.13 4.37 14 -3 -1 5.54 4.81 -14 3 0 14.87 6.95 -14 -3 0 15.31 7.06 -14 3 0 16.41 6.73 14 3 0 -1.27 5.39 -14 -3 0 7.69 5.63 -14 -3 0 22.51 9.32 14 -3 0 11.35 5.55 -14 3 -1 2.73 3.57 -14 -3 -1 1.79 5.05 14 3 1 1.15 5.36 -14 3 -1 -4.79 7.32 14 -3 1 9.98 5.78 -14 -3 -1 6.51 5.07 -14 3 -2 -6.23 7.24 14 3 2 0.86 3.68 -14 -3 -2 6.52 6.34 14 -4 -8 -3.07 6.23 14 4 -8 -2.28 5.01 14 -4 -7 7.45 4.94 14 4 -7 -1.76 5.12 14 4 -7 11.49 5.07 14 -4 -6 -6.27 4.82 -14 -4 6 5.98 6.76 14 4 -6 -3.84 5.14 14 4 -6 1.87 4.65 -14 -4 5 -0.23 4.56 14 -4 -5 8.68 5.55 14 4 -5 8.60 4.56 14 -4 -5 2.41 3.85 14 -4 -4 -1.71 4.10 14 -4 -4 -5.98 4.97 -14 -4 4 -2.75 4.64 14 4 -4 -5.12 4.83 -14 4 4 3.29 3.90 -14 -4 3 6.85 5.21 14 4 -3 -8.48 4.97 14 -4 -3 5.89 5.08 -14 4 3 5.70 4.96 14 4 -2 -0.14 4.35 -14 4 2 -3.76 3.88 14 -4 -2 3.12 3.56 14 -4 -1 10.14 6.16 -14 4 1 18.12 7.71 14 4 -1 10.78 6.78 14 -4 0 14.32 6.13 14 4 0 5.28 5.59 -14 4 0 -3.18 4.42 -14 4 -1 -2.91 3.60 14 -5 -7 6.94 6.33 14 5 -7 3.85 3.76 14 -5 -6 1.64 4.39 14 5 -6 -9.82 5.08 -14 -5 5 2.84 4.84 14 5 -5 2.67 4.65 14 -5 -5 -2.58 4.07 14 -5 -4 5.05 4.40 14 -5 -4 -0.28 3.60 -14 -5 4 -0.11 3.92 -14 5 4 -3.37 5.10 14 -5 -3 3.18 4.29 14 -5 -3 10.59 5.24 -14 -5 3 2.15 4.64 -14 5 3 10.62 5.77 14 5 -3 -0.21 3.93 -14 5 2 0.51 3.98 14 -5 -2 6.99 5.70 14 5 -2 17.71 7.07 14 -5 -1 0.74 4.28 -14 5 1 4.77 5.78 -14 5 0 2.99 4.30 14 -6 -5 -2.56 4.72 -14 -6 4 -0.23 5.27 14 -6 -4 -2.40 3.41 -14 6 3 0.64 5.83 -14 -6 3 2.99 6.00 14 -6 -3 -0.08 3.43 -14 6 2 4.20 5.18 -14 6 1 -6.85 6.83 15 0 -9 -1.94 5.58 15 0 -8 -0.30 3.35 15 0 -7 -8.71 7.36 15 0 -6 -1.75 5.64 15 0 -5 10.92 5.68 15 0 -4 -0.78 4.12 15 0 -3 -0.02 5.75 15 0 -2 -4.65 3.66 15 0 -1 7.27 4.94 15 0 0 6.69 4.41 15 0 1 0.07 3.50 15 -1 -8 1.88 3.99 15 -1 -7 4.59 6.05 15 -1 -7 -4.24 4.04 15 -1 -6 -0.69 4.59 15 -1 -5 -3.91 4.30 15 -1 -4 -6.79 6.14 15 -1 -3 1.20 3.84 15 1 -3 4.78 4.27 15 1 -2 -18.83 6.27 15 1 -1 6.16 6.05 15 -1 -1 2.38 4.07 15 1 0 -0.02 4.47 15 -1 0 10.65 5.76 15 -1 1 3.55 4.36 15 2 -9 -6.98 5.11 15 -2 -8 5.32 4.95 15 2 -8 -1.33 3.10 15 -2 -7 2.02 3.78 15 -2 -6 -4.65 4.26 15 -2 -5 -1.04 3.88 15 -2 -4 1.53 4.58 15 2 -4 2.78 4.01 15 -2 -3 6.49 4.63 15 2 -3 -0.70 3.20 15 2 -2 0.66 5.20 15 2 -1 3.12 3.84 15 -3 -7 -19.78 6.64 15 3 -7 0.66 3.77 15 -3 -6 1.66 3.71 15 3 -6 -4.40 4.31 15 -3 -5 -4.14 4.36 15 3 -5 -4.30 4.65 15 3 -5 2.14 3.06 15 3 -4 -0.82 3.19 15 -3 -4 0.62 4.53 15 3 -3 5.40 5.25 15 3 -2 2.69 4.58 15 -4 -6 -1.63 3.50 15 4 -5 -21.36 6.97 15 4 -5 4.26 4.34 -15 4 3 1.78 3.59 0 0 0 0.00 0.00 TITL exp_437_auto in P2(1)/n REM P2(1)/n (#14 in standard setting) CELL 0.71073 10.914641 10.098042 15.036766 90.0000 99.2457 90.0000 ZERR 31.00 0.000367 0.000276 0.000433 0.0000 0.0028 0.0000 LATT 1 SYMM -x+1/2, y+1/2,-z+1/2 SFAC C H N O UNIT 31.00 31.00 31.00 31.00 TREF HKLF 4 END _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 90885 _olex2_submission_special_instructions 'No special instructions were received' _oxdiff_exptl_absorpt_empirical_details ; Empirical correction (ABSPACK) includes: - Absorption correction using spherical harmonics - Frame scaling ; _oxdiff_exptl_absorpt_empirical_full_max 1.096 _oxdiff_exptl_absorpt_empirical_full_min 0.869 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Zn1 Zn 0.72344(3) 0.43496(3) 0.65896(2) 0.04850(14) Uani 1 1 d . . . . . O3 O 0.5689(2) 0.5464(2) 0.66705(16) 0.0593(6) Uani 1 1 d . . . . . H3A H 0.512367 0.536808 0.618744 0.089 Uiso 1 1 d R U . . . H3B H 0.586111 0.631356 0.666235 0.089 Uiso 1 1 d R U . . . O6 O 0.8934(4) 0.7818(3) 0.8522(3) 0.0377(9) Uani 0.647(8) 1 d D . P A 1 O2 O 0.8036(2) 0.5238(3) 0.56662(16) 0.0650(7) Uani 1 1 d . . . . . C16 C 0.9283(2) 0.5886(2) 0.94159(15) 0.0260(5) Uani 1 1 d . . . . . O1 O 0.6368(2) 0.4721(3) 0.46846(18) 0.0805(9) Uani 1 1 d . . . . . O4 O 0.8437(5) 0.4879(3) 0.7634(2) 0.0431(11) Uani 0.647(8) 1 d D . P A 1 C17 C 0.8506(2) 0.6905(3) 0.88592(16) 0.0342(5) Uani 1 1 d D . . . . C18 C 0.9917(2) 0.6309(2) 1.02487(16) 0.0318(5) Uani 1 1 d . . . . . H18 H 0.986474 0.719185 1.041380 0.038 Uiso 1 1 calc R U . . . C15 C 0.9375(2) 0.4564(2) 0.91634(15) 0.0286(5) Uani 1 1 d . . . . . C14 C 0.8717(3) 0.4059(3) 0.82632(17) 0.0373(6) Uani 1 1 d D . . . . C2 C 0.7797(3) 0.6266(3) 0.4238(2) 0.0494(7) Uani 1 1 d . . . . . N1 N 0.5872(3) 0.7480(4) 0.1591(2) 0.0776(10) Uani 1 1 d . U . . . C3 C 0.6929(3) 0.6928(3) 0.3626(2) 0.0512(8) Uani 1 1 d . . . . . H3 H 0.608863 0.677878 0.362691 0.061 Uiso 1 1 calc R U . . . O7 O 0.7758(8) 0.7592(9) 0.9063(4) 0.049(2) Uani 0.353(8) 1 d D . P A 2 C1 C 0.7350(3) 0.5340(4) 0.4898(2) 0.0558(8) Uani 1 1 d . . . . . O5 O 0.8383(7) 0.2872(4) 0.8194(4) 0.080(2) Uani 0.647(8) 1 d D . P A 1 C7 C 0.7293(3) 0.7819(4) 0.3007(3) 0.0615(9) Uani 1 1 d . U . . . C4 C 0.9055(3) 0.6482(4) 0.4212(3) 0.0656(10) Uani 1 1 d . . . . . H4 H 0.965467 0.604950 0.461947 0.079 Uiso 1 1 calc R U . . . C5 C 0.9411(3) 0.7337(5) 0.3582(3) 0.0749(12) Uani 1 1 d . . . . . H5 H 1.025007 0.745765 0.355711 0.090 Uiso 1 1 calc R U . . . C6 C 0.8537(4) 0.8010(4) 0.2992(3) 0.0751(11) Uani 1 1 d . . . . . H6 H 0.878797 0.859858 0.258042 0.090 Uiso 1 1 calc R U . . . C13 C 0.5183(4) 0.5512(5) 0.0335(2) 0.0841(14) Uani 1 1 d . U . . . C9 C 0.4743(4) 0.6968(6) 0.1497(3) 0.0927(15) Uani 1 1 d . U . . . H9 H 0.418454 0.727593 0.185614 0.111 Uiso 1 1 calc R U . . . C8 C 0.6323(4) 0.8453(4) 0.2313(3) 0.0824(12) Uani 1 1 d . U . . . H8A H 0.563362 0.875278 0.259545 0.099 Uiso 1 1 calc R U . . . H8B H 0.667369 0.921628 0.205334 0.099 Uiso 1 1 calc R U . . . C11 C 0.4385(4) 0.5993(7) 0.0879(3) 0.1002(16) Uani 1 1 d . U . . . H11 H 0.358666 0.564843 0.082474 0.120 Uiso 1 1 calc R U . . . C12 C 0.6350(5) 0.6074(7) 0.0464(4) 0.1117(17) Uani 1 1 d . U . . . H12 H 0.693278 0.577911 0.012065 0.134 Uiso 1 1 calc R U . . . C10 C 0.6662(5) 0.7036(7) 0.1073(4) 0.1132(18) Uani 1 1 d . U . . . H10 H 0.745257 0.740320 0.113497 0.136 Uiso 1 1 calc R U . . . O21 O 0.9111(7) 0.7302(11) 0.8174(6) 0.057(2) Uani 0.353(8) 1 d D . P A 2 O8 O 0.7809(9) 0.4720(8) 0.7920(6) 0.052(2) Uani 0.353(8) 1 d D . P A 2 O20 O 0.7322(3) 0.6776(6) 0.8890(3) 0.0616(14) Uani 0.647(8) 1 d D . P A 1 O9 O 0.9189(10) 0.3116(8) 0.7944(4) 0.058(3) Uani 0.353(8) 1 d D . P A 2 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 Zn1 0.0614(2) 0.03021(17) 0.0417(2) -0.00428(14) -0.02861(15) -0.00415(15) O3 0.0719(15) 0.0432(13) 0.0554(14) 0.0028(10) -0.0126(11) -0.0015(11) O6 0.0396(17) 0.0287(15) 0.040(2) 0.0068(13) -0.0094(13) 0.0062(12) O2 0.0571(14) 0.0706(16) 0.0580(14) 0.0030(12) -0.0190(11) 0.0018(12) C16 0.0272(11) 0.0251(11) 0.0228(11) 0.0049(8) -0.0051(8) 0.0012(9) O1 0.0553(15) 0.108(2) 0.0681(17) 0.0310(16) -0.0201(12) -0.0240(15) O4 0.058(3) 0.0359(15) 0.0271(16) 0.0022(11) -0.0194(15) -0.0090(15) C17 0.0413(11) 0.0306(11) 0.0254(11) 0.0031(9) -0.0107(9) 0.0071(9) C18 0.0398(13) 0.0225(11) 0.0280(12) -0.0001(9) -0.0098(10) 0.0017(10) C15 0.0322(12) 0.0273(12) 0.0221(11) 0.0019(9) -0.0085(9) -0.0011(9) C14 0.0471(14) 0.0296(10) 0.0283(12) -0.0018(8) -0.0144(10) 0.0010(9) C2 0.0401(16) 0.0490(18) 0.0568(19) -0.0084(15) 0.0007(13) 0.0016(13) N1 0.073(2) 0.099(2) 0.0617(19) 0.0421(18) 0.0136(16) -0.0103(19) C3 0.0385(15) 0.0518(19) 0.062(2) 0.0036(16) 0.0049(14) 0.0019(14) O7 0.062(4) 0.047(4) 0.038(3) 0.013(3) 0.003(2) 0.026(3) C1 0.0460(17) 0.061(2) 0.0550(19) 0.0032(16) -0.0076(14) 0.0079(15) O5 0.122(5) 0.0325(14) 0.063(3) 0.0046(15) -0.055(3) -0.0178(18) C7 0.0528(19) 0.053(2) 0.079(2) 0.0106(18) 0.0113(17) -0.0051(16) C4 0.0398(17) 0.066(2) 0.086(3) -0.014(2) -0.0042(17) 0.0056(16) C5 0.0399(18) 0.087(3) 0.100(3) -0.019(3) 0.018(2) -0.019(2) C6 0.060(2) 0.071(3) 0.096(3) 0.006(2) 0.019(2) -0.018(2) C13 0.061(2) 0.146(4) 0.046(2) 0.041(2) 0.0133(18) -0.012(2) C9 0.061(2) 0.156(4) 0.061(2) 0.023(3) 0.0102(19) -0.013(3) C8 0.078(3) 0.069(3) 0.098(3) 0.042(2) 0.009(2) -0.007(2) C11 0.061(2) 0.181(5) 0.059(2) 0.008(3) 0.011(2) -0.023(3) C12 0.079(3) 0.163(5) 0.104(4) 0.002(3) 0.047(3) -0.029(3) C10 0.084(3) 0.145(5) 0.119(4) 0.002(4) 0.040(3) -0.040(3) O21 0.050(3) 0.071(6) 0.051(4) 0.034(4) 0.004(3) 0.015(3) O8 0.056(4) 0.049(3) 0.039(4) -0.013(3) -0.030(3) 0.010(3) O20 0.0362(13) 0.073(4) 0.072(3) 0.036(2) -0.0042(15) 0.0095(16) O9 0.088(6) 0.046(3) 0.031(3) -0.011(3) -0.013(3) 0.021(4) 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' 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' Zn Zn 0.2839 1.4301 '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 O6 Zn1 O3 84.80(12) 2_646 . ? O6 Zn1 O7 48.2(2) 2_646 2_646 ? O2 Zn1 O3 104.77(10) . . ? O2 Zn1 O6 130.08(15) . 2_646 ? O2 Zn1 O7 91.18(19) . 2_646 ? O2 Zn1 O8 120.5(4) . . ? O4 Zn1 O3 104.81(17) . . ? O4 Zn1 O6 128.18(19) . 2_646 ? O4 Zn1 O2 97.15(16) . . ? O4 Zn1 O7 125.0(3) . 2_646 ? O7 Zn1 O3 125.2(3) 2_646 . ? O7 Zn1 O8 127.8(3) 2_646 . ? O8 Zn1 O3 88.1(2) . . ? C17 O6 Zn1 110.4(3) . 2_656 ? C1 O2 Zn1 114.3(2) . . ? C18 C16 C17 116.4(2) . . ? C15 C16 C17 124.2(2) . . ? C15 C16 C18 119.3(2) . . ? C14 O4 Zn1 118.4(3) . . ? O6 C17 C16 123.1(3) . . ? O6 C17 O20 123.6(3) . . ? O7 C17 C16 128.8(4) . . ? O7 C17 O21 118.2(5) . . ? O21 C17 C16 108.8(4) . . ? O20 C17 C16 112.7(3) . . ? C15 C18 C16 121.4(2) 3_767 . ? C16 C15 C14 121.3(2) . . ? C18 C15 C16 119.3(2) 3_767 . ? C18 C15 C14 119.3(2) 3_767 . ? O4 C14 C15 118.3(3) . . ? O5 C14 O4 122.4(3) . . ? O5 C14 C15 119.1(3) . . ? O8 C14 C15 115.1(4) . . ? O9 C14 C15 116.4(4) . . ? O9 C14 O8 128.2(5) . . ? C3 C2 C1 118.7(3) . . ? C3 C2 C4 118.5(3) . . ? C4 C2 C1 122.8(3) . . ? C9 N1 C8 121.9(4) . . ? C9 N1 C10 119.1(5) . . ? C10 N1 C8 118.7(4) . . ? C2 C3 C7 121.1(3) . . ? C17 O7 Zn1 109.9(6) . 2_656 ? O2 C1 C2 116.3(3) . . ? O1 C1 O2 123.5(3) . . ? O1 C1 C2 120.2(3) . . ? C3 C7 C8 119.5(3) . . ? C6 C7 C3 119.2(4) . . ? C6 C7 C8 121.0(4) . . ? C5 C4 C2 120.1(4) . . ? C6 C5 C4 120.6(3) . . ? C5 C6 C7 120.3(4) . . ? C11 C13 C13 122.3(5) . 3_665 ? C11 C13 C12 115.5(5) . . ? C12 C13 C13 122.3(5) . 3_665 ? N1 C9 C11 120.9(5) . . ? N1 C8 C7 109.7(4) . . ? C9 C11 C13 121.3(4) . . ? C10 C12 C13 121.4(5) . . ? N1 C10 C12 121.8(5) . . ? C14 O8 Zn1 114.3(5) . . ? loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Zn1 O3 2.048(2) . ? Zn1 O6 1.994(4) 2_646 ? Zn1 O2 1.972(3) . ? Zn1 O4 1.953(3) . ? Zn1 O7 2.029(8) 2_646 ? Zn1 O8 2.032(7) . ? O6 C17 1.185(4) . ? O2 C1 1.276(4) . ? C16 C17 1.500(3) . ? C16 C18 1.397(3) . ? C16 C15 1.396(3) . ? O1 C1 1.238(4) . ? O4 C14 1.258(4) . ? C17 O7 1.149(6) . ? C17 O21 1.371(7) . ? C17 O20 1.306(4) . ? C18 C15 1.391(3) 3_767 ? C15 C14 1.515(3) . ? C14 O5 1.252(4) . ? C14 O8 1.236(6) . ? C14 O9 1.218(6) . ? C2 C3 1.382(4) . ? C2 C1 1.501(5) . ? C2 C4 1.397(5) . ? N1 C9 1.323(5) . ? N1 C8 1.488(6) . ? N1 C10 1.328(6) . ? C3 C7 1.397(5) . ? C7 C6 1.376(5) . ? C7 C8 1.505(5) . ? C4 C5 1.384(6) . ? C5 C6 1.374(6) . ? C13 C13 1.454(10) 3_665 ? C13 C11 1.375(7) . ? C13 C12 1.379(6) . ? C9 C11 1.367(7) . ? C12 C10 1.342(8) . ?