#------------------------------------------------------------------------------ #$Date: 2026-09-25 10:19:01 +0100 (Fri, 25 Sep 2026) $ #$Revision: 306908 $ #$URL: svn://www.crystallography.net/cod/cif/4/51/95/4519546.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_4519546 loop_ _publ_author_name 'Lu, Junhao' 'Fan, Yingtong' 'Zhou, Bingyue' 'Ye, Zecong' 'Mei, Sen' 'Zhou, Dan' 'Chen, Lanhua' 'Chen, Lixi' 'Liu, Hanzhou' 'Zhu, Huifang' 'Dai, Xing' 'Wang, Yanlong' 'Diwu, Juan' 'Wang, Shuao' _publ_section_title ; A General Energy-Puzzle Strategy to Fabricate Efficient Metal--Organic Framework Scintillators for X-ray Detection ; _journal_issue 9 _journal_name_full 'ACS Materials Letters' _journal_page_first 3951 _journal_page_last 3957 _journal_paper_doi 10.1021/acsmaterialslett.4c00924 _journal_volume 6 _journal_year 2024 _chemical_formula_moiety 'C12 H12 N O5 Pb' _chemical_formula_sum 'C12 H12 N O5 Pb' _chemical_formula_weight 457.42 _space_group_crystal_system orthorhombic _space_group_IT_number 62 _space_group_name_Hall '-P 2ac 2n' _space_group_name_H-M_alt 'P n m a' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _audit_contact_author_name ; ; _audit_creation_date 2024-06-14 _audit_creation_method ; Olex2 1.5 (compiled 2021.11.18 svn.ra9532c28 for OlexSys, GUI svn.r6427) ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 7.6459(2) _cell_length_b 18.1731(4) _cell_length_c 10.1540(2) _cell_measurement_reflns_used 9828 _cell_measurement_temperature 296.15 _cell_measurement_theta_max 27.395 _cell_measurement_theta_min 2.297 _cell_volume 1410.90(6) _computing_cell_refinement 'SAINT V8.40B (?, 2016)' _computing_data_reduction 'SAINT V8.40B (?, 2016)' _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 2014/5 (Sheldrick, 2014)' _diffrn_ambient_temperature 296.15 _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.999 _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0730 _diffrn_reflns_av_unetI/netI 0.0233 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.999 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 49360 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.507 _diffrn_reflns_theta_min 2.241 _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 11.972 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.2525 _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1495 before and 0.0848 after correction. The Ratio of minimum to maximum transmission is 0.3387. The \l/2 correction factor is Not present. ; _exptl_crystal_density_diffrn 2.153 _exptl_crystal_description block _exptl_crystal_F_000 852 _refine_diff_density_max 0.752 _refine_diff_density_min -1.056 _refine_diff_density_rms 0.117 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.040 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 115 _refine_ls_number_reflns 1667 _refine_ls_number_restraints 18 _refine_ls_restrained_S_all 1.047 _refine_ls_R_factor_all 0.0215 _refine_ls_R_factor_gt 0.0197 _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^)+(0.0321P)^2^+1.0748P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0503 _refine_ls_wR_factor_ref 0.0512 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1564 _reflns_number_total 1667 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file tz4c00924_si_004.cif _cod_data_source_block 1 _cod_database_code 4519546 _shelx_shelxl_version_number 2018/3 _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. ; _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups At 1.5 times of: All C(H,H,H) groups 2. Uiso/Uaniso restraints and constraints Uanis(C7) \\sim Ueq, Uanis(C8) \\sim Ueq, Uanis(C5) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04 Uanis(C5) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004 Uanis(C8) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004 3. Others Fixed Sof: C6(0.5) H6(0.5) N1(0.5) C8(0.5) H8A(0.5) H8B(0.5) H8C(0.5) C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5) C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5) 4.a Aromatic/amide H refined with riding coordinates: C3(H3), C6(H6) 4.b Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C) ; _shelx_res_file ; TITL 1_a.res in Pnma 1.res created by SHELXL-2018/3 at 21:10:42 on 14-Jun-2024 REM Old TITL 1 in Pnma REM SHELXT solution in Pnma REM R1 0.082, Rweak 0.003, Alpha 0.020, Orientation as input REM Formula found by SHELXT: C10 N O2 Pb CELL 0.71073 7.6459 18.1731 10.154 90 90 90 ZERR 4 0.0002 0.0004 0.0002 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM -X,0.5+Y,-Z SYMM 0.5+X,0.5-Y,0.5-Z SFAC C H N O Pb UNIT 48 48 4 20 4 ISOR 0.02 0.04 C7 C8 C5 ISOR 0.002 0.004 C5 ISOR 0.002 0.004 C8 L.S. 20 0 0 PLAN 1 TEMP 23 CONF BOND $H list 4 fmap 2 53 MORE -1 ACTA REM REM REM WGHT 0.032100 1.074800 FVAR 0.33561 PB01 5 0.394349 0.750000 0.692174 10.50000 0.02882 0.03017 = 0.03651 0.00000 -0.00282 0.00000 O2 4 0.131293 0.656712 0.700130 11.00000 0.05846 0.05296 = 0.08081 -0.03839 0.00548 -0.00514 O3 4 0.663629 0.750000 0.547046 10.50000 0.07558 0.06918 = 0.05930 0.00000 0.02424 0.00000 O1 4 0.308463 0.655107 0.533182 11.00000 0.09137 0.09862 = 0.07117 -0.04007 0.01639 -0.04732 C2 1 0.091185 0.561298 0.544194 11.00000 0.04686 0.03898 = 0.05609 -0.01749 -0.00992 0.00202 C1 1 0.182529 0.629139 0.594871 11.00000 0.04689 0.03995 = 0.05581 -0.01747 -0.01076 -0.00027 C4 1 0.170485 0.514032 0.456472 11.00000 0.05467 0.05959 = 0.08532 -0.03937 0.00698 -0.01021 C3 1 -0.074186 0.547047 0.587391 11.00000 0.05434 0.05109 = 0.08650 -0.04028 0.01071 -0.00561 AFIX 43 H3 2 -0.125023 0.578884 0.648026 11.00000 -1.20000 AFIX 0 PART -1 C6 1 0.698074 0.793609 0.467383 10.50000 0.06086 0.06784 = 0.05022 0.00532 0.01154 0.00284 AFIX 43 H6 2 0.639391 0.838245 0.474754 10.50000 -1.20000 AFIX 0 N1 3 0.807388 0.788787 0.369125 10.50000 0.05119 0.10435 = 0.04384 0.00713 0.00122 0.00009 C8 1 0.842206 0.853639 0.282383 10.50000 0.09762 0.09996 = 0.08734 0.00993 0.00233 -0.00925 AFIX 137 H8A 2 0.807754 0.842255 0.193780 10.50000 -1.50000 H8B 2 0.964736 0.865123 0.284270 10.50000 -1.50000 H8C 2 0.776484 0.895178 0.313405 10.50000 -1.50000 AFIX 0 C5 1 0.351086 0.530129 0.391938 10.50000 0.11053 0.11157 = 0.12303 -0.01544 0.00318 -0.00159 AFIX 137 H5A 2 0.347687 0.516359 0.300698 10.50000 -1.50000 H5B 2 0.440153 0.502283 0.436174 10.50000 -1.50000 H5C 2 0.376830 0.581676 0.399131 10.50000 -1.50000 AFIX 0 C7 1 0.904910 0.722458 0.348858 10.50000 0.13805 0.12646 = 0.15194 0.02581 0.06098 0.04007 AFIX 137 H7A 2 0.888730 0.690270 0.422827 10.50000 -1.50000 H7B 2 1.026801 0.734110 0.339936 10.50000 -1.50000 H7C 2 0.864566 0.698537 0.270228 10.50000 -1.50000 AFIX 0 HKLF 4 REM 1_a.res in Pnma REM wR2 = 0.0512, GooF = S = 1.040, Restrained GooF = 1.047 for all data REM R1 = 0.0197 for 1564 Fo > 4sig(Fo) and 0.0215 for all 1667 data REM 115 parameters refined using 18 restraints END WGHT 0.0258 1.3874 REM Highest difference peak 0.752, deepest hole -1.056, 1-sigma level 0.117 Q1 1 0.3758 0.5031 0.4679 11.00000 0.05 0.75 ; _shelx_res_checksum 61335 _shelx_hkl_file ; 1 0 0 0.50 0.40 -1 0 0 1.60 1.10 -1 0 0 0.80 1.00 -1 0 0 1.10 0.50 -1 0 0 1.10 0.50 -1 0 0 3.40 0.70 -1 0 0 0.60 0.30 1 0 0 2.90 1.10 1 0 0 1.80 0.90 1 0 0 0.50 0.40 1 0 0 0.50 0.30 2 0 0 82.19 7.60 -2 0 0 85.79 7.30 2 0 0 80.39 8.90 2 0 0 68.69 7.40 2 0 0 71.09 7.10 -2 0 0 92.69 9.10 -2 0 0 108.59 9.60 -2 0 0 87.49 7.60 -2 0 0 100.09 7.90 -2 0 0 77.09 7.70 2 0 0 100.69 9.00 -3 0 0 0.60 1.30 3 0 0 3.00 1.00 3 0 0 0.90 1.20 3 0 0 2.40 1.40 3 0 0 1.60 1.60 -3 0 0 2.10 2.90 -3 0 0 0.30 3.20 -3 0 0 -0.40 0.90 3 0 0 -1.60 3.10 3 0 0 2.50 2.50 -4 0 0 7457.85 558.74 -4 0 0 6484.95 557.04 4 0 0 6974.80 557.94 4 0 0 6468.75 556.74 -5 0 0 0.70 2.90 -5 0 0 10.30 6.90 5 0 0 0.40 1.80 -5 0 0 18.80 6.80 5 0 0 -1.60 1.80 5 0 0 -0.10 1.00 -5 0 0 0.80 2.10 5 0 0 10.70 6.00 -5 0 0 -0.50 1.60 -5 0 0 0.80 2.10 -6 0 0 828.52 64.89 -6 0 0 709.53 65.19 6 0 0 831.72 65.79 6 0 0 724.63 65.59 6 0 0 799.52 63.39 6 0 0 765.12 64.99 6 0 0 836.12 68.69 -6 0 0 775.82 69.09 6 0 0 678.63 69.49 -7 0 0 11.50 14.30 -7 0 0 -0.40 2.70 -7 0 0 -0.10 3.90 7 0 0 -2.50 2.40 7 0 0 -4.50 3.10 -7 0 0 1.40 4.70 -7 0 0 -0.10 3.00 7 0 0 -4.20 2.90 7 0 0 -0.10 8.60 8 0 0 244.58 22.60 8 0 0 237.48 23.20 -8 0 0 204.38 23.40 8 0 0 223.58 32.50 -8 0 0 227.78 21.40 -8 0 0 174.08 21.00 -8 0 0 215.28 21.80 8 0 0 255.47 29.10 -8 0 0 250.67 37.90 9 0 0 -1.60 5.50 9 0 0 -1.20 4.70 -9 0 0 -10.80 3.30 -9 0 0 -0.10 5.50 -9 0 0 35.50 27.20 -9 0 0 -5.90 4.30 9 0 0 -20.00 14.50 -9 0 0 4.90 4.30 0 0 -1 0.70 1.40 0 0 -1 2.70 1.20 0 0 -1 0.50 0.40 0 0 1 0.90 0.60 0 0 1 2.30 1.00 0 0 1 3.50 1.50 0 0 -1 0.50 0.40 0 0 -1 2.00 0.70 1 0 -1 23.20 2.80 1 0 1 20.40 2.40 -1 0 1 15.40 2.70 -1 0 -1 19.20 2.10 -1 0 -1 19.90 2.40 1 0 1 20.60 2.40 -1 0 1 22.70 4.30 -1 0 1 36.50 5.00 -1 0 -1 20.30 2.50 -1 0 -1 18.30 1.80 -1 0 1 19.20 2.60 -1 0 1 13.20 2.50 1 0 -1 20.10 2.90 -1 0 -1 23.20 1.90 1 0 -1 31.90 4.90 1 0 -1 22.00 4.10 -1 0 1 15.40 2.20 1 0 1 19.60 1.90 1 0 1 23.00 2.10 1 0 1 17.30 2.30 1 0 -1 21.50 2.80 -1 0 -1 21.90 1.90 1 0 -1 15.70 2.20 -1 0 -1 21.70 2.00 -1 0 -1 18.90 2.40 2 0 -1 2788.02 225.88 2 0 1 2501.75 223.78 -2 0 1 2804.52 226.88 -2 0 1 2959.20 225.98 -2 0 -1 2911.01 224.18 2 0 1 2601.24 223.78 -2 0 -1 2733.93 223.88 -3 0 -1 125.59 13.60 -3 0 1 170.68 16.40 -3 0 1 152.18 13.20 -3 0 1 111.89 12.60 -3 0 1 154.78 12.20 -3 0 -1 138.49 11.50 -3 0 -1 139.39 13.30 -3 0 -1 149.88 12.20 -3 0 -1 140.29 12.10 -3 0 -1 141.99 12.50 3 0 1 128.49 11.80 -3 0 1 142.99 15.10 3 0 -1 116.99 12.30 -3 0 1 130.19 12.40 3 0 1 128.49 11.70 3 0 1 128.99 12.10 3 0 -1 121.39 12.50 -3 0 -1 150.58 12.00 3 0 -1 135.99 12.80 3 0 -1 123.59 11.70 3 0 1 126.99 13.30 3 0 -1 130.19 15.50 3 0 1 130.29 12.90 -4 0 -1 1519.75 118.79 -4 0 1 1499.75 120.69 4 0 1 1499.55 117.79 4 0 -1 1272.87 118.49 4 0 -1 1436.26 116.39 4 0 1 1418.76 117.79 -4 0 1 1398.46 119.19 -4 0 -1 1384.96 116.29 -4 0 -1 1398.76 117.59 4 0 -1 1303.87 119.59 5 0 1 160.08 15.80 5 0 1 147.99 15.30 -5 0 1 179.68 16.60 5 0 -1 172.18 15.10 5 0 1 164.68 20.80 5 0 1 180.18 18.10 -5 0 -1 165.68 20.70 -5 0 -1 208.68 19.30 5 0 1 162.08 16.20 -5 0 1 194.38 24.90 -5 0 -1 196.78 16.10 5 0 -1 176.98 16.80 -5 0 1 195.48 16.10 5 0 -1 190.88 20.10 5 0 -1 150.08 16.10 -5 0 -1 155.38 16.10 -5 0 -1 182.58 15.40 -5 0 1 151.88 20.90 -5 0 1 157.18 17.00 -5 0 1 220.08 18.70 5 0 -1 162.78 16.70 -6 0 1 1013.10 83.09 -6 0 1 944.41 90.49 6 0 -1 948.51 82.19 -6 0 -1 1103.79 86.69 -6 0 1 838.52 84.39 -6 0 -1 1038.80 89.09 -6 0 -1 988.50 82.59 6 0 -1 986.50 83.99 6 0 -1 879.31 83.29 6 0 1 945.71 82.59 6 0 1 972.50 83.59 -6 0 -1 1031.70 83.09 -6 0 -1 1127.79 84.89 6 0 -1 1033.10 89.89 6 0 1 1072.49 85.69 6 0 -1 1052.49 84.29 -6 0 1 1034.60 88.19 6 0 1 912.51 86.49 6 0 1 1108.39 83.39 6 0 -1 1008.20 87.39 7 0 -1 3.30 4.40 7 0 1 5.80 3.60 7 0 -1 1.10 1.80 -7 0 1 1.20 3.30 -7 0 1 15.70 15.30 -7 0 1 -14.80 10.10 -7 0 -1 13.50 14.00 -7 0 -1 0.90 2.80 7 0 1 0.90 4.30 -7 0 -1 2.20 3.90 7 0 -1 1.00 4.30 -7 0 1 7.00 5.10 -7 0 1 7.00 3.80 -7 0 -1 0.40 2.90 -7 0 -1 5.40 4.80 7 0 1 -5.40 7.50 7 0 1 0.90 2.40 -7 0 1 3.00 5.60 -7 0 -1 -1.00 2.80 -8 0 -1 594.34 61.59 -8 0 -1 524.95 67.09 -8 0 -1 655.63 59.69 8 0 1 735.73 65.09 -8 0 -1 699.73 56.79 8 0 1 609.24 57.69 8 0 -1 776.82 59.09 -8 0 1 767.72 57.69 8 0 -1 627.94 54.29 -8 0 -1 588.64 58.19 -8 0 1 803.02 66.09 8 0 -1 620.24 59.49 -8 0 -1 664.73 56.59 8 0 1 704.43 61.09 -8 0 -1 559.24 56.59 8 0 -1 714.23 68.99 -8 0 1 665.73 59.89 -8 0 1 732.33 71.89 -8 0 1 576.74 57.29 8 0 -1 757.72 63.89 8 0 1 729.63 57.49 -9 0 1 81.89 12.60 9 0 -1 97.19 22.50 9 0 -1 84.29 13.60 -9 0 -1 89.69 13.80 -9 0 1 95.39 13.10 -9 0 1 95.49 17.10 -9 0 -1 94.49 12.30 -9 0 -1 145.59 34.50 9 0 1 73.69 27.80 9 0 1 79.19 13.30 9 0 1 90.89 12.30 -9 0 1 65.69 30.60 9 0 -1 103.69 14.40 -9 0 -1 77.09 11.20 -9 0 -1 83.49 14.50 0 0 2 1077.79 89.89 0 0 -2 1059.19 90.29 0 0 -2 1111.59 90.49 1 0 -2 3501.35 284.87 -1 0 2 3412.06 284.57 1 0 2 3428.06 282.67 -1 0 -2 3403.96 282.87 -1 0 2 3565.54 284.67 1 0 -2 3564.24 285.07 -2 0 2 880.71 73.09 -2 0 2 940.81 73.29 -2 0 2 861.71 70.69 2 0 -2 818.12 72.59 2 0 -2 819.72 70.29 2 0 -2 814.42 70.39 2 0 -2 751.12 70.49 2 0 2 848.12 69.79 -2 0 2 765.42 70.49 2 0 2 861.81 69.89 2 0 -2 867.51 73.19 -2 0 -2 876.41 69.99 -2 0 -2 935.21 70.09 3 0 2 1857.51 162.98 -3 0 2 1997.50 166.38 -3 0 -2 2143.19 163.58 -3 0 2 2147.39 167.18 3 0 -2 2054.59 167.18 -3 0 -2 2140.19 163.28 3 0 2 1817.32 163.48 3 0 -2 1819.82 165.88 4 0 2 1811.12 158.78 4 0 2 1993.60 158.58 -4 0 -2 1973.30 158.78 4 0 -2 1901.61 163.18 4 0 -2 1904.61 158.88 -4 0 2 1940.51 162.18 -4 0 -2 1989.50 159.68 -5 0 2 127.09 18.40 5 0 2 82.09 9.00 5 0 -2 82.39 11.50 5 0 2 90.89 11.50 5 0 -2 93.89 9.50 5 0 2 89.69 12.70 -5 0 -2 95.19 9.10 5 0 -2 99.19 10.90 5 0 -2 93.69 11.50 5 0 2 93.79 9.50 -5 0 -2 94.39 9.30 -5 0 -2 109.99 10.00 -5 0 -2 92.49 15.80 5 0 2 102.99 10.30 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21.70 1 -22 4 158.18 18.90 -1 22 4 157.08 42.10 -2 -22 4 -0.40 6.60 2 -22 4 -2.60 5.10 0 23 0 3.00 6.70 0 -23 0 7.90 5.50 0 23 0 5.40 8.70 0 -23 0 -2.00 7.00 0 23 0 8.60 28.50 0 23 0 -1.20 6.10 0 -23 0 4.50 27.50 1 23 0 0.20 8.30 1 -23 0 1.50 2.60 -1 -23 0 -7.50 5.30 -1 -23 0 -2.10 5.20 1 23 0 6.50 29.60 -1 23 0 -6.20 6.10 -1 23 0 4.80 8.00 -1 -23 0 19.80 29.40 1 -23 0 -1.60 4.40 1 23 0 3.90 6.30 1 -23 0 -1.30 6.20 1 23 0 -6.80 6.50 2 -23 0 378.36 32.70 2 23 0 374.06 35.90 -2 23 0 319.47 40.00 2 23 0 463.95 52.59 2 23 0 388.06 37.90 -2 -23 0 376.26 35.00 2 23 0 252.57 50.79 2 -23 0 362.86 35.80 -2 23 0 349.07 36.30 -2 -23 0 401.96 37.50 -2 -23 0 338.77 56.29 0 -23 1 356.46 34.20 0 -23 1 412.86 37.30 0 23 1 443.16 39.00 0 -23 1 356.96 33.90 0 -23 -1 300.87 51.69 0 23 1 408.66 40.70 0 23 -1 286.47 53.69 0 23 -1 411.16 38.20 0 23 1 383.66 53.59 0 -23 -1 388.86 37.50 0 -23 -1 361.56 32.30 0 -23 -1 405.26 35.30 0 23 1 413.46 37.10 0 -23 1 288.07 59.29 0 23 -1 362.86 37.20 0 23 -1 364.26 54.59 1 23 1 14.60 9.10 1 23 1 5.90 7.10 1 23 1 -17.30 28.40 1 -23 -1 14.80 6.10 -1 23 -1 12.60 7.80 -1 23 -1 11.50 9.60 -1 23 -1 9.00 7.60 -1 -23 1 18.40 8.00 1 -23 -1 7.40 7.50 -1 -23 1 30.00 33.60 -1 -23 1 9.50 5.90 -1 23 1 27.00 11.60 1 23 -1 18.20 7.80 1 -23 1 17.50 8.10 1 -23 1 22.30 4.90 1 -23 1 24.10 9.10 -1 23 1 4.20 6.90 1 23 -1 -13.20 32.70 1 23 -1 23.70 9.10 -1 -23 -1 14.90 10.60 -1 23 1 13.70 8.20 1 23 -1 11.90 9.70 -1 -23 -1 24.70 9.60 -1 -23 -1 -17.00 30.90 -2 23 -1 16.00 7.80 -2 -23 1 42.40 41.80 -2 -23 1 11.70 8.40 -2 -23 1 14.20 6.60 -2 23 -1 16.90 8.10 -2 23 -1 25.00 12.30 2 23 1 20.00 8.40 2 -23 -1 11.20 5.30 2 23 1 13.60 9.30 2 23 1 32.30 32.70 2 23 1 15.40 8.90 2 23 -1 8.40 7.70 2 23 -1 8.50 9.80 -2 23 1 20.10 8.30 2 -23 1 19.10 4.10 2 -23 1 18.40 4.60 -2 -23 -1 19.70 12.00 -2 23 1 28.50 12.80 2 -23 1 10.40 7.30 -2 -23 -1 68.39 37.40 -2 23 1 14.10 8.30 2 23 -1 7.50 7.10 0 -23 -2 -1.20 5.40 0 23 2 -1.50 7.10 0 23 2 -1.10 7.30 0 23 2 1.50 6.00 0 -23 2 2.60 6.60 0 -23 2 -0.50 4.80 0 -23 2 0.10 4.70 0 23 2 -11.10 32.50 0 23 -2 -3.60 6.40 0 23 -2 0.10 9.00 0 23 -2 -2.60 6.10 0 -23 -2 5.70 7.00 -1 23 -2 103.59 15.90 1 23 2 117.29 18.00 1 23 2 130.89 19.80 1 23 2 91.79 15.10 -1 -23 2 124.49 16.90 1 -23 -2 99.79 16.30 -1 23 -2 101.19 20.10 -1 23 -2 94.59 16.10 -1 -23 2 94.79 13.10 1 23 2 77.19 35.10 1 -23 -2 93.79 13.50 -1 23 2 113.39 17.80 -1 23 2 118.19 20.80 -1 23 2 96.79 15.20 1 -23 2 128.39 13.30 -1 -23 -2 62.89 35.10 1 23 -2 76.09 15.10 1 23 -2 144.49 21.60 1 23 -2 77.69 14.30 1 -23 2 99.19 11.80 -1 -23 -2 124.29 17.80 -1 -23 -2 104.99 14.50 1 -23 2 94.49 14.70 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 12968 _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, 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 Pb01 Pb 0.39435(2) 0.750000 0.69217(2) 0.03184(8) Uani 1 2 d S T P A . O2 O 0.1313(4) 0.6567(2) 0.7001(3) 0.0641(9) Uani 1 1 d . . . . . O3 O 0.6636(6) 0.750000 0.5470(4) 0.0680(11) Uani 1 2 d S T P . . O1 O 0.3085(5) 0.6551(2) 0.5332(3) 0.0871(11) Uani 1 1 d . . . . . C2 C 0.0912(4) 0.5613(2) 0.5442(4) 0.0473(8) Uani 1 1 d . . . . . C1 C 0.1825(5) 0.62914(18) 0.5949(4) 0.0475(8) Uani 1 1 d . . . . . C4 C 0.1705(6) 0.5140(2) 0.4565(5) 0.0665(12) Uani 1 1 d . . . . . C3 C -0.0742(5) 0.5470(2) 0.5874(5) 0.0640(12) Uani 1 1 d . . . . . H3 H -0.125023 0.578884 0.648026 0.077 Uiso 1 1 calc R U . . . C6 C 0.6981(11) 0.7936(5) 0.4674(8) 0.0596(19) Uani 0.5 1 d . . P A -1 H6 H 0.639391 0.838245 0.474754 0.072 Uiso 0.5 1 calc R U P A -1 N1 N 0.8074(10) 0.7888(6) 0.3691(7) 0.066(2) Uani 0.5 1 d . . P A -1 C8 C 0.8422(19) 0.8536(9) 0.2824(13) 0.095(4) Uani 0.5 1 d . U P A -1 H8A H 0.807754 0.842255 0.193780 0.142 Uiso 0.5 1 calc R U P A -1 H8B H 0.964736 0.865123 0.284270 0.142 Uiso 0.5 1 calc R U P A -1 H8C H 0.776484 0.895178 0.313405 0.142 Uiso 0.5 1 calc R U P A -1 C5 C 0.3511(17) 0.5301(9) 0.3919(17) 0.115(4) Uani 0.5 1 d . U P B -1 H5A H 0.347687 0.516359 0.300698 0.173 Uiso 0.5 1 calc R U P B -1 H5B H 0.440153 0.502283 0.436174 0.173 Uiso 0.5 1 calc R U P B -1 H5C H 0.376830 0.581676 0.399131 0.173 Uiso 0.5 1 calc R U P B -1 C7 C 0.905(2) 0.7225(11) 0.349(2) 0.139(8) Uani 0.5 1 d . U P A -1 H7A H 0.888730 0.690270 0.422827 0.208 Uiso 0.5 1 calc R U P A -1 H7B H 1.026801 0.734110 0.339936 0.208 Uiso 0.5 1 calc R U P A -1 H7C H 0.864566 0.698537 0.270228 0.208 Uiso 0.5 1 calc R U P A -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_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb01 0.02882(11) 0.03017(10) 0.03651(11) 0.000 -0.00282(5) 0.000 O2 0.0585(18) 0.0530(19) 0.081(2) -0.0384(15) 0.0055(12) -0.0051(13) O3 0.076(3) 0.069(3) 0.059(2) 0.000 0.024(2) 0.000 O1 0.091(2) 0.099(3) 0.0712(19) -0.0401(19) 0.0164(18) -0.047(2) C2 0.0469(19) 0.0390(17) 0.056(2) -0.0175(16) -0.0099(14) 0.0020(13) C1 0.0469(18) 0.0399(16) 0.0558(19) -0.0175(15) -0.0108(16) -0.0003(15) C4 0.055(2) 0.060(2) 0.085(3) -0.039(2) 0.007(2) -0.010(2) C3 0.054(2) 0.051(2) 0.086(3) -0.040(2) 0.011(2) -0.0056(17) C6 0.061(5) 0.068(5) 0.050(4) 0.005(4) 0.012(4) 0.003(4) N1 0.051(4) 0.104(6) 0.044(4) 0.007(4) 0.001(3) 0.000(4) C8 0.098(5) 0.100(5) 0.087(4) 0.010(4) 0.002(4) -0.009(4) C5 0.111(5) 0.112(6) 0.123(6) -0.015(4) 0.003(4) -0.002(4) C7 0.138(15) 0.126(17) 0.152(12) 0.026(12) 0.061(11) 0.040(11) 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' Pb Pb -3.3944 10.1111 '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 O2 Pb01 O2 80.21(16) . 7_575 O2 Pb01 O2 95.48(12) 7_575 4_566 O2 Pb01 O2 154.29(4) . 4_566 O2 Pb01 O2 95.48(12) . 6_657 O2 Pb01 O2 77.40(16) 4_566 6_657 O2 Pb01 O2 154.29(4) 7_575 6_657 O3 Pb01 O2 129.74(9) . . O3 Pb01 O2 129.74(9) . 7_575 O3 Pb01 O2 72.03(11) . 6_657 O3 Pb01 O2 72.03(11) . 4_566 O1 Pb01 O2 105.58(14) 7_575 . O1 Pb01 O2 90.27(13) . 6_657 O1 Pb01 O2 50.39(10) . . O1 Pb01 O2 105.58(13) . 7_575 O1 Pb01 O2 50.39(10) 7_575 7_575 O1 Pb01 O2 90.27(13) 7_575 4_566 O1 Pb01 O2 152.16(11) . 4_566 O1 Pb01 O2 152.16(11) 7_575 6_657 O1 Pb01 O3 80.48(11) . . O1 Pb01 O3 80.48(11) 7_575 . O1 Pb01 O1 89.4(2) 7_575 . Pb01 O2 Pb01 96.91(11) . 6_557 C1 O2 Pb01 144.0(3) . 6_557 C1 O2 Pb01 89.6(2) . . C6 O3 Pb01 126.1(5) . . C1 O1 Pb01 98.2(2) . . C4 C2 C1 121.8(3) . . C3 C2 C1 118.4(3) . . C3 C2 C4 119.8(3) . . O2 C1 C2 118.5(4) . . O1 C1 O2 121.6(3) . . O1 C1 C2 119.9(3) . . C2 C4 C3 117.8(4) . 5_566 C2 C4 C5 123.1(7) . . C3 C4 C5 118.7(7) 5_566 . C2 C3 C4 122.3(4) . 5_566 C2 C3 H3 118.8 . . C4 C3 H3 118.8 5_566 . O3 C6 H6 115.4 . . O3 C6 N1 129.2(9) . . N1 C6 H6 115.4 . . C6 N1 C8 120.8(10) . . C6 N1 C7 120.0(10) . . C7 N1 C8 119.1(9) . . N1 C8 H8A 109.5 . . N1 C8 H8B 109.5 . . N1 C8 H8C 109.5 . . H8A C8 H8B 109.5 . . H8A C8 H8C 109.5 . . H8B C8 H8C 109.5 . . C4 C5 H5A 109.5 . . C4 C5 H5B 109.5 . . C4 C5 H5C 109.5 . . H5A C5 H5B 109.5 . . H5A C5 H5C 109.5 . . H5B C5 H5C 109.5 . . N1 C7 H7A 109.5 . . N1 C7 H7B 109.5 . . N1 C7 H7C 109.5 . . H7A C7 H7B 109.5 . . H7A C7 H7C 109.5 . . H7B C7 H7C 109.5 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Pb01 O2 2.632(3) . Pb01 O2 2.711(3) 4_566 Pb01 O2 2.632(3) 7_575 Pb01 O2 2.711(3) 6_657 Pb01 O3 2.532(4) . Pb01 O1 2.452(3) 7_575 Pb01 O1 2.452(3) . O2 C1 1.244(4) . O3 C6 1.163(8) . O1 C1 1.242(5) . C2 C1 1.508(4) . C2 C4 1.378(5) . C2 C3 1.363(5) . C4 C3 1.404(5) 5_566 C4 C5 1.556(14) . C3 H3 0.9300 . C6 H6 0.9300 . C6 N1 1.304(11) . N1 C8 1.495(17) . N1 C7 1.432(18) . C8 H8A 0.9600 . C8 H8B 0.9600 . C8 H8C 0.9600 . C5 H5A 0.9600 . C5 H5B 0.9600 . C5 H5C 0.9600 . C7 H7A 0.9600 . C7 H7B 0.9600 . C7 H7C 0.9600 . 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 Pb01 O2 C1 O1 -4.4(4) . . . . Pb01 O2 C1 O1 96.8(5) 6_557 . . . Pb01 O2 C1 C2 173.9(3) . . . . Pb01 O2 C1 C2 -84.9(5) 6_557 . . . Pb01 O3 C6 N1 -161.5(7) . . . . Pb01 O1 C1 O2 4.7(5) . . . . Pb01 O1 C1 C2 -173.6(3) . . . . O3 C6 N1 C8 -175.7(10) . . . . O3 C6 N1 C7 -0.1(18) . . . . C1 C2 C4 C3 -178.8(4) . . . 5_566 C1 C2 C4 C5 -6.2(10) . . . . C1 C2 C3 C4 178.7(4) . . . 5_566 C4 C2 C1 O2 -158.3(4) . . . . C4 C2 C1 O1 20.1(6) . . . . C4 C2 C3 C4 -1.4(9) . . . 5_566 C3 C2 C1 O2 21.7(6) . . . . C3 C2 C1 O1 -160.0(4) . . . . C3 C2 C4 C3 1.3(8) . . . 5_566 C3 C2 C4 C5 173.9(8) . . . .