#------------------------------------------------------------------------------ #$Date: 2026-09-25 10:18:57 +0100 (Fri, 25 Sep 2026) $ #$Revision: 306907 $ #$URL: svn://www.crystallography.net/cod/cif/4/51/95/4519545.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_4519545 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 iterative _audit_contact_author_name ; ; _audit_creation_date 2024-06-11 _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 7.6476(2) _cell_length_b 18.2198(3) _cell_length_c 10.1548(2) _cell_measurement_reflns_used 9993 _cell_measurement_temperature 296.15 _cell_measurement_theta_max 27.523 _cell_measurement_theta_min 3.335 _cell_volume 1414.95(5) _computing_cell_refinement 'SAINT V8.38A (Bruker, 2018)' _computing_data_reduction 'SAINT V8.38A (Bruker, 2018)' _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 'olex2.solve 1.5 (Bourhis et al., 2015)' _diffrn_ambient_temperature 296.15 _diffrn_measured_fraction_theta_full 0.986 _diffrn_measured_fraction_theta_max 0.988 _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 0.0655 _diffrn_reflns_av_unetI/netI 0.0272 _diffrn_reflns_Laue_measured_fraction_full 0.986 _diffrn_reflns_Laue_measured_fraction_max 0.988 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_number 24350 _diffrn_reflns_point_group_measured_fraction_full 0.986 _diffrn_reflns_point_group_measured_fraction_max 0.988 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.523 _diffrn_reflns_theta_min 3.335 _diffrn_source_current 1.4 _diffrn_source_power 0.07 _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 11.938 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.3841 _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1482 before and 0.0725 after correction. The Ratio of minimum to maximum transmission is 0.5152. The \l/2 correction factor is Not present. ; _exptl_crystal_density_diffrn 2.147 _exptl_crystal_description block _exptl_crystal_F_000 852 _refine_diff_density_max 0.825 _refine_diff_density_min -1.000 _refine_diff_density_rms 0.137 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.120 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 115 _refine_ls_number_reflns 1653 _refine_ls_number_restraints 109 _refine_ls_restrained_S_all 1.162 _refine_ls_R_factor_all 0.0247 _refine_ls_R_factor_gt 0.0235 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0223P)^2^+3.2292P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0565 _refine_ls_wR_factor_ref 0.0570 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1580 _reflns_number_total 1653 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file 2024_Lu_3951.cif _cod_data_source_block 0 _cod_database_code 4519545 _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 C5 \\sim C3: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A C5: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A Uanis(O1) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04 Uanis(C8) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04 Uanis(C8) \\sim Ueq, Uanis(C7) \\sim Ueq, Uanis(O1) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004 Uanis(C5) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004 3. Rigid body (RIGU) restrains All non-hydrogen atoms with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 4. Others Fixed Sof: N1(0.5) C6(0.5) H6(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) 5.a Aromatic/amide H refined with riding coordinates: C4(H4), C6(H6) 5.b Idealised Me refined as rotating group: C8(H8A,H8B,H8C), C5(H5A,H5B,H5C), C7(H7A,H7B,H7C) ; _shelx_res_file ; TITL 0 in Pnma #62 0.res created by SHELXL-2018/3 at 09:36:00 on 11-Jun-2024 REM reset to Pnma #62 CELL 0.71073 7.6476 18.2198 10.1548 90 90 90 ZERR 4 0.0002 0.0003 0.0002 0 0 0 LATT 1 SYMM 0.5-X,-Y,0.5+Z SYMM 0.5+X,0.5-Y,0.5-Z SYMM -X,0.5+Y,-Z SFAC C H N O Pb UNIT 48 48 4 20 4 ISOR 0.02 0.04 O1 ISOR 0.02 0.04 C8 C7 ISOR 0.002 0.004 C8 C7 O1 RIGU ISOR 0.002 0.004 C5 SIMU C5 C3 SIMU C5 L.S. 20 PLAN 1 TEMP 23 CONF MORE -1 fmap 2 53 BOND $H ACTA REM REM REM WGHT 0.022300 3.229200 FVAR 0.36152 PB1 5 0.107944 0.250000 0.192202 10.50000 0.02568 0.02826 = 0.03287 0.00000 0.00223 0.00000 O2 4 0.370643 0.343809 0.201358 11.00000 0.05356 0.05433 = 0.08412 0.04093 -0.00781 -0.00547 O3 4 -0.164164 0.250000 0.047477 10.50000 0.07462 0.06578 = 0.05318 0.00000 -0.02467 0.00000 O1 4 0.193788 0.344478 0.031720 11.00000 0.07633 0.07431 = 0.06894 0.01538 -0.00423 -0.01823 C2 1 0.409768 0.438436 0.044287 11.00000 0.04127 0.03730 = 0.05259 0.01750 0.00892 0.00088 C1 1 0.319274 0.370868 0.094597 11.00000 0.04317 0.03814 = 0.05453 0.01535 0.00834 -0.00169 C3 1 0.330380 0.485647 -0.043692 11.00000 0.04921 0.05621 = 0.08066 0.03880 -0.00681 -0.00687 C4 1 0.424866 0.546530 -0.087890 11.00000 0.04856 0.05062 = 0.07647 0.03675 -0.00794 -0.00364 AFIX 43 H4 2 0.373556 0.577862 -0.148995 11.00000 -1.20000 AFIX 0 PART -1 N1 3 -0.304850 0.290213 -0.131942 10.50000 0.03835 0.10294 = 0.04991 0.00654 0.00056 0.00110 C6 1 -0.197914 0.294009 -0.031034 10.50000 0.05196 0.06310 = 0.05186 0.00526 -0.00662 0.00446 AFIX 43 H6 2 -0.140635 0.338687 -0.021002 10.50000 -1.20000 AFIX 0 C8 1 -0.342822 0.352662 -0.214964 10.50000 0.09052 0.09406 = 0.08458 0.00804 -0.00340 0.00687 AFIX 137 H8A 2 -0.464666 0.364748 -0.208124 10.50000 -1.50000 H8B 2 -0.315242 0.340860 -0.304727 10.50000 -1.50000 H8C 2 -0.273774 0.393849 -0.187176 10.50000 -1.50000 AFIX 0 C5 1 0.145630 0.471165 -0.103248 10.50000 0.08742 0.09392 = 0.10098 0.01218 -0.00977 -0.00566 AFIX 137 H5A 2 0.157781 0.451287 -0.190319 10.50000 -1.50000 H5B 2 0.081650 0.516440 -0.107371 10.50000 -1.50000 H5C 2 0.083720 0.436854 -0.048718 10.50000 -1.50000 AFIX 0 C7 1 -0.401807 0.222186 -0.145804 10.50000 0.10544 0.10415 = 0.10883 -0.00078 -0.00718 -0.01071 AFIX 137 H7A 2 -0.372380 0.199446 -0.228153 10.50000 -1.50000 H7B 2 -0.524922 0.232403 -0.143662 10.50000 -1.50000 H7C 2 -0.372262 0.189707 -0.074768 10.50000 -1.50000 AFIX 0 HKLF 4 REM 0 in Pnma #62 REM wR2 = 0.0570, GooF = S = 1.120, Restrained GooF = 1.162 for all data REM R1 = 0.0235 for 1580 Fo > 4sig(Fo) and 0.0247 for all 1653 data REM 115 parameters refined using 109 restraints END WGHT 0.0222 3.2317 REM Highest difference peak 0.825, deepest hole -1.000, 1-sigma level 0.137 Q1 1 0.1206 0.4961 -0.0343 11.00000 0.05 0.83 ; _shelx_res_checksum 5728 _shelx_hkl_file ; 1 0 0 1.60 0.50 1 0 0 2.60 2.30 -1 0 0 1.60 2.00 -1 0 0 2.30 0.60 -1 0 0 2.00 0.80 2 0 0 165.68 10.50 2 0 0 150.78 16.50 -2 0 0 150.98 11.00 -2 0 0 164.58 16.60 -2 0 0 154.08 10.40 2 0 0 135.39 10.90 -3 0 0 3.70 1.90 3 0 0 1.20 6.30 -3 0 0 2.40 1.60 -3 0 0 0.10 5.40 3 0 0 6.60 2.30 3 0 0 2.30 1.50 -4 0 0 8537.65 571.44 4 0 0 9999.00 575.64 5 0 0 4.20 2.70 5 0 0 2.00 2.40 5 0 0 1.40 9.80 -5 0 0 2.80 3.30 -5 0 0 0.60 2.50 5 0 0 1.50 3.10 -5 0 0 1.00 9.40 6 0 0 667.83 46.80 -6 0 0 735.33 49.00 6 0 0 750.02 47.20 -6 0 0 660.93 65.89 6 0 0 654.53 48.70 -6 0 0 771.12 47.30 7 0 0 -17.50 11.50 7 0 0 0.70 3.10 -7 0 0 8.00 6.40 7 0 0 -3.20 3.20 -7 0 0 0.00 3.60 -8 0 0 389.36 30.70 -8 0 0 387.66 56.49 -8 0 0 408.26 33.00 8 0 0 399.66 58.09 8 0 0 414.96 30.60 9 0 0 8.10 12.50 -9 0 0 1.80 6.20 -9 0 0 20.00 22.60 0 0 1 6.60 2.50 0 0 -1 0.70 1.90 1 0 -1 21.50 2.20 1 0 1 25.40 5.60 -1 0 1 18.10 2.20 -1 0 1 19.00 2.10 1 0 1 11.80 1.30 1 0 1 10.90 1.60 -1 0 -1 30.10 5.70 1 0 -1 18.30 6.00 1 0 -1 17.40 2.10 -1 0 1 15.20 2.00 -1 0 1 15.90 6.10 2 0 1 3287.87 193.58 -2 0 1 2760.42 194.48 2 0 -1 3543.95 197.88 -2 0 -1 2746.33 191.98 3 0 -1 186.48 14.80 3 0 -1 191.58 14.20 -3 0 -1 203.68 13.70 3 0 1 224.08 23.40 3 0 1 204.58 13.70 -3 0 1 211.28 14.90 -3 0 1 194.28 23.50 -3 0 -1 180.28 21.40 -3 0 1 186.08 13.90 3 0 1 177.88 14.90 3 0 -1 225.38 25.80 4 0 1 1347.37 90.89 4 0 1 1511.05 105.09 4 0 -1 1440.26 91.49 -4 0 1 1348.77 104.49 4 0 -1 1628.74 90.49 4 0 -1 1719.53 110.69 4 0 -1 1455.45 90.49 -4 0 1 1395.36 90.99 -4 0 -1 1293.17 101.79 -5 0 -1 172.18 14.20 -5 0 -1 179.68 27.20 -5 0 -1 196.38 16.00 -5 0 1 194.08 15.90 5 0 -1 157.38 15.50 5 0 -1 236.88 40.50 5 0 1 201.88 29.60 5 0 1 171.98 14.10 -5 0 1 186.18 14.70 5 0 -1 174.28 14.50 5 0 -1 204.78 15.20 -5 0 1 181.28 33.20 5 0 1 185.88 15.90 6 0 -1 1363.86 88.39 6 0 1 1224.88 87.39 -6 0 1 1224.08 106.39 -6 0 -1 1259.07 105.39 6 0 1 1469.25 85.39 -6 0 -1 1310.07 87.39 6 0 1 1413.86 85.89 -6 0 -1 1391.86 85.89 6 0 -1 1508.95 115.39 6 0 -1 1476.45 86.89 6 0 -1 1339.27 86.19 -6 0 1 1431.36 87.89 -6 0 1 1253.37 85.79 7 0 1 5.80 14.70 -7 0 -1 -10.60 16.40 7 0 1 5.40 3.80 -7 0 1 3.40 4.40 7 0 -1 -0.70 15.70 7 0 1 9.70 4.30 -7 0 -1 12.50 5.00 7 0 -1 4.50 3.70 -7 0 1 -0.80 5.80 8 0 -1 768.02 54.39 8 0 -1 767.72 84.99 -8 0 1 771.82 82.29 -8 0 -1 765.72 53.69 -8 0 1 713.53 52.99 -8 0 -1 808.62 81.19 -8 0 1 766.52 51.79 8 0 1 744.73 81.49 8 0 1 701.13 50.29 -9 0 1 132.69 16.20 -9 0 -1 106.49 26.00 9 0 1 115.19 38.50 -9 0 -1 160.58 50.39 -9 0 1 159.38 47.10 9 0 -1 155.78 50.79 0 0 -2 1224.48 80.59 0 0 2 1239.48 80.39 1 0 -2 4042.70 239.28 -1 0 2 3603.44 238.68 2 0 -2 987.80 70.29 -2 0 2 848.12 68.49 2 0 -2 891.71 57.49 2 0 2 1005.70 65.29 2 0 -2 889.51 57.49 -2 0 -2 912.61 64.49 3 0 2 2287.17 149.59 -3 0 -2 2202.18 148.99 -3 0 2 2155.88 153.68 3 0 -2 2438.86 156.78 4 0 -2 2422.26 154.28 4 0 2 2691.63 169.58 -4 0 2 2518.35 172.88 4 0 -2 2775.22 176.88 -4 0 -2 2219.48 165.58 5 0 2 183.08 28.90 5 0 2 178.08 14.70 -5 0 2 202.68 15.70 5 0 -2 224.88 16.90 5 0 2 166.58 15.90 -5 0 2 197.08 16.60 -5 0 2 212.98 38.50 -5 0 -2 183.08 28.10 5 0 -2 242.78 42.30 5 0 -2 187.88 15.60 -5 0 -2 196.58 16.20 -6 0 2 552.84 62.89 6 0 2 579.24 43.70 -6 0 2 660.53 43.80 -6 0 -2 629.44 43.50 6 0 -2 608.44 44.30 6 0 2 721.13 42.40 6 0 -2 688.73 69.69 6 0 -2 695.53 43.70 -6 0 2 600.54 42.50 -6 0 -2 586.74 60.09 6 0 -2 566.14 42.90 6 0 2 620.64 74.69 7 0 2 828.52 53.89 -7 0 2 862.91 55.79 7 0 2 850.71 55.09 7 0 -2 784.32 55.79 7 0 2 782.82 79.29 -7 0 -2 761.42 56.89 -7 0 -2 846.32 79.69 7 0 -2 896.11 56.69 7 0 -2 946.31 89.19 8 0 2 521.25 65.79 -8 0 -2 565.14 66.59 -8 0 2 498.65 68.29 8 0 2 560.84 36.20 8 0 -2 591.74 72.09 -8 0 2 567.54 40.80 -8 0 -2 498.65 40.50 8 0 2 537.45 37.50 -8 0 2 505.45 39.00 -9 0 2 32.90 15.50 -9 0 2 96.39 36.40 -9 0 2 29.30 8.40 -9 0 -2 30.60 11.30 9 0 2 29.80 7.20 9 0 -2 30.20 23.10 9 0 2 42.40 7.60 0 0 3 -0.50 0.70 0 0 3 0.30 4.10 0 0 -3 0.20 1.10 0 0 -3 1.00 1.10 0 0 -3 1.20 4.50 0 0 3 0.40 1.10 1 0 -3 2224.38 139.69 -1 0 3 1883.41 137.59 1 0 3 2306.07 137.29 -1 0 -3 2066.19 136.99 2 0 -3 1107.29 70.49 2 0 3 1256.87 79.99 -2 0 -3 1059.59 78.49 2 0 -3 1223.08 70.69 -2 0 3 1017.80 82.99 2 0 -3 1020.90 88.09 -3 0 -3 169.88 22.10 3 0 3 179.18 22.90 3 0 3 188.28 13.50 3 0 -3 148.69 13.80 3 0 -3 194.58 33.70 -3 0 3 164.08 13.40 -3 0 3 183.18 13.80 3 0 3 176.18 11.70 -3 0 3 170.68 13.60 3 0 -3 156.58 13.80 3 0 -3 164.68 14.10 -3 0 3 176.88 32.10 -3 0 -3 201.28 13.40 -4 0 3 166.18 33.80 -4 0 3 156.38 12.80 4 0 -3 154.28 13.60 4 0 3 173.38 24.90 4 0 -3 145.09 13.20 -4 0 -3 163.78 13.00 4 0 3 146.09 10.60 4 0 3 148.59 12.90 4 0 -3 161.48 33.80 -4 0 3 159.48 13.30 -4 0 -3 150.68 27.60 4 0 -3 131.39 13.10 5 0 -3 2897.41 187.68 5 0 3 3283.57 208.18 -5 0 -3 2878.31 204.08 5 0 3 2926.71 186.18 5 0 -3 3333.47 188.78 -5 0 3 2982.10 212.08 5 0 3 3103.89 188.08 5 0 -3 2931.31 188.58 5 0 -3 3176.38 216.28 6 0 -3 318.87 25.00 6 0 3 307.97 25.70 6 0 -3 339.37 47.90 -6 0 3 295.97 44.50 6 0 3 338.27 21.90 -6 0 3 309.57 24.10 6 0 -3 299.07 24.50 6 0 -3 335.67 26.20 -6 0 3 338.87 25.20 6 0 3 332.37 45.50 -6 0 -3 331.87 25.00 -6 0 -3 264.27 39.20 6 0 3 290.47 25.00 7 0 -3 12.90 18.70 -7 0 3 11.80 22.30 7 0 3 2.60 3.50 -7 0 3 0.80 6.80 -7 0 3 4.40 5.00 -7 0 -3 17.60 18.20 7 0 -3 0.60 4.20 -7 0 -3 2.80 6.40 7 0 3 12.00 17.40 -8 0 3 228.68 51.49 8 0 3 178.98 43.60 8 0 -3 258.27 54.39 8 0 3 179.78 14.40 -8 0 -3 171.18 19.40 8 0 3 164.08 15.10 -8 0 3 146.09 17.10 -8 0 -3 152.68 42.60 -8 0 3 171.28 18.70 9 0 3 633.54 73.99 -9 0 3 553.74 43.70 -9 0 3 572.14 42.70 9 0 -3 647.54 79.09 9 0 3 596.04 40.30 9 0 3 555.54 38.60 -9 0 -3 560.14 44.70 -9 0 3 592.04 77.29 0 0 4 291.37 19.90 0 0 -4 259.67 28.90 0 0 4 277.67 19.80 0 0 -4 343.47 20.40 0 0 -4 299.37 20.10 0 0 4 340.97 30.30 1 0 4 4005.30 227.98 -1 0 -4 3286.37 226.78 1 0 -4 3423.56 228.48 -2 0 -4 30.50 3.30 -2 0 4 30.00 15.20 2 0 4 24.20 3.80 2 0 4 26.10 3.90 2 0 4 23.70 3.20 2 0 -4 27.80 4.30 2 0 -4 23.50 4.70 -2 0 4 26.90 4.80 -2 0 4 36.40 4.40 -2 0 4 26.50 4.60 -2 0 -4 26.80 11.20 2 0 -4 29.30 13.40 2 0 -4 26.90 5.20 2 0 4 27.60 11.10 -3 0 -4 4885.91 338.57 3 0 -4 5334.37 347.67 -3 0 4 5322.47 348.37 3 0 4 6000.60 341.67 4 0 4 83.29 7.10 -4 0 4 85.39 26.50 -4 0 4 73.29 9.00 4 0 -4 96.29 27.30 4 0 4 82.49 8.10 -4 0 -4 103.19 9.40 4 0 -4 82.09 9.70 4 0 -4 74.99 9.50 -4 0 4 103.09 9.80 4 0 -4 106.19 10.70 4 0 4 85.99 22.20 -4 0 -4 89.89 22.20 -4 0 4 83.39 9.20 4 0 4 86.19 9.20 -5 0 4 351.06 27.50 -5 0 4 390.26 28.10 5 0 4 384.56 26.50 -5 0 -4 402.96 27.70 -5 0 4 345.97 48.40 -5 0 -4 341.87 42.10 5 0 4 379.06 43.80 5 0 -4 383.96 28.90 5 0 4 349.77 27.80 5 0 4 403.46 25.10 5 0 -4 370.16 49.99 5 0 -4 420.66 29.30 6 0 4 1.30 13.80 -6 0 4 0.30 17.20 6 0 -4 6.60 16.40 -6 0 -4 6.20 19.40 6 0 4 3.60 3.00 -6 0 4 6.40 4.80 6 0 -4 10.20 5.30 6 0 -4 16.30 5.70 6 0 -4 5.60 4.90 -6 0 -4 2.60 4.70 -6 0 4 1.50 3.80 -7 0 4 1742.03 108.39 -7 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21 -4 93.09 16.90 3 -21 4 96.49 22.80 -3 -21 -4 71.69 11.20 3 -21 4 64.99 12.20 0 -21 -5 14.00 5.90 0 -21 -5 12.20 4.40 0 -21 5 12.70 9.70 0 21 -5 23.70 17.50 0 -21 5 17.10 5.20 0 -21 5 22.60 8.00 -1 -21 5 270.47 23.30 1 -21 -5 273.87 23.30 -1 -21 5 306.07 26.80 -1 21 -5 280.27 41.50 -1 -21 5 255.77 23.00 1 -21 -5 291.07 20.00 -1 -21 -5 258.57 21.00 1 -21 5 255.77 19.60 1 -21 5 260.07 26.50 1 -21 5 264.17 25.40 -2 21 -5 -9.00 26.50 -2 -21 5 2.70 7.70 2 -21 -5 2.90 6.30 -2 -21 -5 3.20 4.30 -2 -21 -5 6.80 4.10 2 -21 5 2.60 4.30 2 -21 5 -3.50 5.70 2 21 -5 3.20 15.90 0 -21 6 3.70 6.50 0 -21 6 -0.80 4.30 0 -21 6 -1.30 6.90 0 -21 -6 7.80 5.80 0 21 -6 11.20 31.10 0 -22 0 839.12 58.39 0 -22 0 843.32 56.39 -1 -22 0 10.20 5.40 1 -22 0 3.90 6.30 -1 -22 0 9.00 7.00 1 -22 0 3.90 5.50 -2 -22 0 23.30 8.70 2 -22 0 15.70 7.60 -2 -22 0 27.80 6.60 2 -22 0 27.40 8.70 -3 -22 0 3.10 4.40 3 -22 0 9.60 11.50 -3 -22 0 6.40 7.40 0 -22 1 8.00 6.00 0 -22 -1 2.50 5.30 0 -22 1 7.50 6.70 0 -22 -1 -0.20 5.70 1 -22 -1 44.80 9.30 -1 -22 1 56.79 11.40 -1 -22 1 68.79 10.10 1 -22 -1 42.60 9.80 1 -22 1 55.29 10.10 1 -22 1 30.10 9.80 -1 -22 -1 49.50 10.50 -1 -22 -1 47.30 8.40 2 -22 -1 502.25 36.50 -2 -22 1 482.05 34.20 -2 -22 1 499.55 38.40 2 -22 -1 451.45 36.40 2 -22 1 470.55 37.80 -2 -22 -1 505.15 37.80 2 -22 1 499.35 39.30 -2 -22 -1 467.75 33.60 -3 22 -1 52.89 14.50 -3 -22 1 25.80 6.70 -3 -22 1 19.50 9.50 -3 -22 -1 16.60 8.70 3 -22 1 26.20 8.60 3 -22 1 21.40 4.50 -3 -22 -1 27.20 6.00 0 -22 -2 355.16 27.00 0 -22 2 351.86 29.80 0 -22 -2 349.77 28.20 0 -22 2 348.57 27.30 -1 -22 2 105.59 12.90 1 -22 -2 101.99 13.50 -1 -22 2 129.69 16.60 1 -22 -2 103.89 13.50 -1 -22 -2 82.09 15.10 1 -22 2 119.59 14.50 1 -22 2 117.79 16.20 -1 -22 -2 99.89 12.10 -2 -22 2 20.50 8.90 2 -22 -2 6.90 6.60 -2 -22 2 26.80 7.20 -2 -22 -2 20.40 7.50 -2 -22 -2 25.20 6.20 2 -22 2 11.60 7.20 2 -22 2 10.90 7.70 -3 -22 2 187.88 17.70 -3 22 -2 207.78 39.50 -3 -22 2 227.48 22.80 3 -22 2 204.68 16.30 3 -22 2 195.88 20.90 -3 -22 -2 247.28 22.80 3 -22 2 188.98 15.10 -3 -22 -2 214.68 16.30 0 -22 -3 3.50 5.40 0 -22 -3 -0.10 5.20 0 -22 3 3.10 5.70 -1 -22 3 309.67 23.70 1 -22 -3 250.37 22.90 1 -22 -3 269.47 20.80 -1 -22 3 244.28 26.40 1 -22 -3 272.47 23.00 -1 -22 -3 279.37 23.60 1 -22 3 299.37 24.20 -1 -22 -3 298.27 24.10 1 -22 3 277.47 35.00 -2 -22 3 97.09 17.80 -2 -22 3 99.49 12.70 -2 22 -3 184.68 24.00 2 -22 -3 114.49 14.40 2 -22 -3 97.39 12.90 -2 -22 -3 113.89 14.60 2 -22 3 101.09 9.00 -2 -22 -3 108.89 11.20 2 -22 3 105.89 14.90 2 -22 3 107.89 10.10 0 -22 -4 23.50 6.90 0 -22 -4 33.20 7.30 0 -22 4 18.90 7.60 0 -22 4 19.80 14.80 0 -22 4 24.80 5.60 0 22 -4 27.70 12.10 0 -22 4 19.70 3.70 -1 -22 4 234.78 27.30 -1 -22 4 231.88 24.20 1 -22 -4 256.67 20.00 -1 22 -4 267.67 29.40 1 -22 -4 225.08 21.10 1 -22 4 249.48 17.70 -1 -22 -4 232.88 19.40 1 -22 4 243.18 22.00 1 -22 4 198.08 16.20 -1 -22 -4 251.97 20.60 -2 22 -4 27.40 23.10 2 -22 -4 1.10 4.70 -2 -22 4 3.20 7.20 2 -22 -4 7.30 8.20 -2 -22 4 -6.50 4.70 2 -22 4 0.30 6.30 2 -22 4 5.20 3.30 2 -22 4 1.20 7.30 -2 -22 -4 -6.30 3.40 -2 -22 -4 -0.30 4.90 0 -23 0 1.90 5.50 0 -23 0 0.60 6.40 1 -23 0 1.60 6.50 -1 -23 0 4.20 6.70 -1 -23 0 4.50 5.60 1 -23 0 1.10 5.80 2 -23 0 527.75 44.70 -2 -23 0 497.95 38.30 -2 -23 0 465.65 33.90 2 -23 0 444.76 37.00 0 -23 1 490.55 36.40 0 -23 1 528.25 39.10 0 -23 -1 496.95 38.00 0 -23 -1 485.15 36.10 1 -23 -1 18.00 7.80 -1 -23 1 15.30 8.30 1 -23 -1 23.10 7.70 -1 -23 1 23.10 7.30 -1 -23 -1 20.80 6.70 -1 -23 -1 26.70 9.10 1 -23 1 14.70 8.70 1 -23 1 21.00 8.60 2 -23 -1 20.00 8.10 2 -23 -1 29.80 8.60 -2 -23 1 20.50 10.40 -2 -23 1 17.40 6.50 2 -23 1 10.30 7.90 -2 -23 -1 15.20 7.90 2 -23 1 18.90 8.40 -2 -23 -1 10.20 5.60 0 -23 2 7.30 7.70 0 -23 -2 -2.70 5.50 0 -23 -2 2.20 5.40 1 -23 -2 162.58 16.90 -1 -23 2 135.29 15.20 -1 -23 2 170.88 19.00 1 -23 -2 141.19 16.00 1 -23 2 129.69 16.20 1 -23 2 115.09 25.20 -1 -23 -2 139.09 14.50 -1 -23 -2 157.08 17.50 0 -23 -3 135.59 15.20 0 -23 3 121.99 15.10 0 -23 -3 108.19 13.80 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' _computing_structure_solution 'SHELXT 2014/5 (Sheldrick, 2014)' ; _shelx_hkl_checksum 46102 _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+1/2, -y+1/2, -z+1/2' '-x, y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' '-x-1/2, y-1/2, z-1/2' 'x, -y-1/2, z' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.10794(3) 0.250000 0.19220(2) 0.02893(9) Uani 1 2 d S T P . . O2 O 0.3706(5) 0.3438(3) 0.2014(4) 0.0640(12) Uani 1 1 d . . . . . O3 O -0.1642(8) 0.250000 0.0475(5) 0.0645(14) Uani 1 2 d S T P . . O1 O 0.1938(6) 0.3445(2) 0.0317(4) 0.0732(11) Uani 1 1 d . U . . . C2 C 0.4098(6) 0.4384(3) 0.0443(5) 0.0437(10) Uani 1 1 d . . . . . C1 C 0.3193(6) 0.3709(2) 0.0946(5) 0.0453(10) Uani 1 1 d . . . . . C3 C 0.3304(7) 0.4856(3) -0.0437(6) 0.0620(15) Uani 1 1 d . U . . . C4 C 0.4249(7) 0.5465(3) -0.0879(6) 0.0585(14) Uani 1 1 d . . . . . H4 H 0.373556 0.577862 -0.148995 0.070 Uiso 1 1 calc R U . . . N1 N -0.3048(12) 0.2902(6) -0.1319(9) 0.064(2) Uani 0.5 1 d . . P A -1 C6 C -0.1979(14) 0.2940(6) -0.0310(10) 0.056(2) Uani 0.5 1 d . . P A -1 H6 H -0.140635 0.338687 -0.021002 0.067 Uiso 0.5 1 calc R U P A -1 C8 C -0.343(2) 0.3527(12) -0.2150(16) 0.090(4) Uani 0.5 1 d . U P A -1 H8A H -0.464666 0.364748 -0.208124 0.135 Uiso 0.5 1 calc R U P A -1 H8B H -0.315242 0.340860 -0.304727 0.135 Uiso 0.5 1 calc R U P A -1 H8C H -0.273774 0.393849 -0.187176 0.135 Uiso 0.5 1 calc R U P A -1 C5 C 0.146(2) 0.4712(10) -0.1032(18) 0.094(4) Uani 0.5 1 d . U P B -1 H5A H 0.157781 0.451287 -0.190319 0.141 Uiso 0.5 1 calc R U P B -1 H5B H 0.081650 0.516440 -0.107371 0.141 Uiso 0.5 1 calc R U P B -1 H5C H 0.083720 0.436854 -0.048718 0.141 Uiso 0.5 1 calc R U P B -1 C7 C -0.402(2) 0.2222(11) -0.146(2) 0.106(5) Uani 0.5 1 d . U P A -1 H7A H -0.372380 0.199446 -0.228153 0.159 Uiso 0.5 1 calc R U P A -1 H7B H -0.524922 0.232403 -0.143662 0.159 Uiso 0.5 1 calc R U P A -1 H7C H -0.372262 0.189707 -0.074768 0.159 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 Pb1 0.02568(13) 0.02826(12) 0.03287(13) 0.000 0.00223(7) 0.000 O2 0.054(2) 0.054(2) 0.084(3) 0.041(2) -0.0078(17) -0.0055(16) O3 0.075(4) 0.066(3) 0.053(3) 0.000 -0.025(3) 0.000 O1 0.0763(18) 0.0743(18) 0.0689(17) 0.0154(15) -0.0042(15) -0.0182(15) C2 0.041(2) 0.037(2) 0.053(3) 0.0175(19) 0.0089(18) 0.0009(17) C1 0.043(2) 0.038(2) 0.055(3) 0.0154(19) 0.008(2) -0.0017(19) C3 0.049(3) 0.056(3) 0.081(4) 0.039(3) -0.007(3) -0.007(2) C4 0.049(3) 0.051(3) 0.076(4) 0.037(3) -0.008(2) -0.004(2) N1 0.038(5) 0.103(6) 0.050(4) 0.007(4) 0.001(3) 0.001(4) C6 0.052(6) 0.063(6) 0.052(5) 0.005(4) -0.007(4) 0.004(4) C8 0.091(5) 0.094(5) 0.085(5) 0.008(4) -0.003(4) 0.007(4) C5 0.087(5) 0.094(5) 0.101(5) 0.012(4) -0.010(4) -0.006(4) C7 0.105(6) 0.104(6) 0.109(6) -0.001(4) -0.007(4) -0.011(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' 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 Pb1 O2 80.72(19) 8_565 . O2 Pb1 O2 154.39(4) . 3_455 O2 Pb1 O2 94.99(16) 8_565 3_455 O2 Pb1 O2 154.39(4) 8_565 6_556 O2 Pb1 O2 78.0(2) 3_455 6_556 O2 Pb1 O2 94.99(16) . 6_556 O3 Pb1 O2 129.95(11) . 8_565 O3 Pb1 O2 129.95(11) . . O3 Pb1 O2 71.57(14) . 6_556 O3 Pb1 O2 71.57(14) . 3_455 O1 Pb1 O2 105.87(16) . 8_565 O1 Pb1 O2 151.89(13) 8_565 6_556 O1 Pb1 O2 50.73(13) 8_565 8_565 O1 Pb1 O2 105.87(16) 8_565 . O1 Pb1 O2 50.73(13) . . O1 Pb1 O2 151.89(13) . 3_455 O1 Pb1 O2 90.09(16) 8_565 3_455 O1 Pb1 O2 90.09(16) . 6_556 O1 Pb1 O3 80.55(14) 8_565 . O1 Pb1 O3 80.55(14) . . O1 Pb1 O1 88.8(2) . 8_565 Pb1 O2 Pb1 96.61(13) . 6_656 C1 O2 Pb1 143.2(4) . 6_656 C1 O2 Pb1 89.2(3) . . C6 O3 Pb1 125.3(6) . . C1 O1 Pb1 97.8(3) . . C3 C2 C1 121.9(4) . . C4 C2 C1 118.7(4) 5_665 . C4 C2 C3 119.4(4) 5_665 . O2 C1 C2 118.2(5) . . O1 C1 O2 122.1(4) . . O1 C1 C2 119.7(4) . . C2 C3 C4 118.3(5) . . C2 C3 C5 123.0(8) . . C4 C3 C5 118.6(8) . . C2 C4 C3 122.2(5) 5_665 . C2 C4 H4 118.9 5_665 . C3 C4 H4 118.9 . . C6 N1 C8 122.6(13) . . C6 N1 C7 116.0(13) . . C8 N1 C7 120.9(12) . . O3 C6 N1 129.7(11) . . O3 C6 H6 115.2 . . N1 C6 H6 115.2 . . 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 . . C3 C5 H5A 109.5 . . C3 C5 H5B 109.5 . . C3 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 Pb1 O2 2.639(4) 8_565 Pb1 O2 2.717(4) 3_455 Pb1 O2 2.639(4) . Pb1 O2 2.717(4) 6_556 Pb1 O3 2.548(5) . Pb1 O1 2.460(4) . Pb1 O1 2.460(4) 8_565 O2 C1 1.254(6) . O3 C6 1.160(11) . O1 C1 1.249(6) . C2 C1 1.502(6) . C2 C3 1.381(7) . C2 C4 1.368(7) 5_665 C3 C4 1.398(7) . C3 C5 1.559(16) . C4 H4 0.9300 . N1 C6 1.313(14) . N1 C8 1.45(2) . N1 C7 1.45(2) . C6 H6 0.9300 . 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 Pb1 O2 C1 O1 -4.4(5) . . . . Pb1 O2 C1 O1 95.6(7) 6_656 . . . Pb1 O2 C1 C2 173.8(4) . . . . Pb1 O2 C1 C2 -86.2(7) 6_656 . . . Pb1 O3 C6 N1 160.0(9) . . . . Pb1 O1 C1 O2 4.8(6) . . . . Pb1 O1 C1 C2 -173.4(4) . . . . C2 C3 C4 C2 -1.7(11) . . . 5_665 C1 C2 C3 C4 -178.7(5) . . . . C1 C2 C3 C5 -3.1(12) . . . . C3 C2 C1 O2 -157.7(6) . . . . C3 C2 C1 O1 20.5(8) . . . . C4 C2 C1 O2 21.9(7) 5_665 . . . C4 C2 C1 O1 -159.8(6) 5_665 . . . C4 C2 C3 C4 1.7(10) 5_665 . . . C4 C2 C3 C5 177.3(10) 5_665 . . . C8 N1 C6 O3 174.9(13) . . . . C5 C3 C4 C2 -177.5(9) . . . 5_665 C7 N1 C6 O3 3(2) . . . .