#------------------------------------------------------------------------------ #$Date: 2026-09-25 10:19:25 +0100 (Fri, 25 Sep 2026) $ #$Revision: 306910 $ #$URL: svn://www.crystallography.net/cod/cif/4/51/95/4519548.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_4519548 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 direct _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 7.6774(2) _cell_length_b 18.1243(6) _cell_length_c 10.1579(3) _cell_measurement_reflns_used 9854 _cell_measurement_temperature 296.15 _cell_measurement_theta_max 27.511 _cell_measurement_theta_min 3.326 _cell_volume 1413.45(7) _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 'XS (Sheldrick, 2008)' _diffrn_ambient_temperature 296.15 _diffrn_measured_fraction_theta_full 0.998 _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 0.0866 _diffrn_reflns_av_unetI/netI 0.0365 _diffrn_reflns_Laue_measured_fraction_full 0.998 _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 26153 _diffrn_reflns_point_group_measured_fraction_full 0.998 _diffrn_reflns_point_group_measured_fraction_max 0.999 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 27.510 _diffrn_reflns_theta_min 3.326 _diffrn_source_current 0.0 _diffrn_source_power 0.0 _diffrn_source_voltage 0.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 11.950 _exptl_absorpt_correction_T_max 0.7456 _exptl_absorpt_correction_T_min 0.2662 _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1698 before and 0.1026 after correction. The Ratio of minimum to maximum transmission is 0.3570. The \l/2 correction factor is Not present. ; _exptl_crystal_density_diffrn 2.150 _exptl_crystal_description block _exptl_crystal_F_000 852 _refine_diff_density_max 1.466 _refine_diff_density_min -0.954 _refine_diff_density_rms 0.153 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 115 _refine_ls_number_reflns 1669 _refine_ls_number_restraints 103 _refine_ls_restrained_S_all 1.052 _refine_ls_R_factor_all 0.0334 _refine_ls_R_factor_gt 0.0311 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1000P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1145 _refine_ls_wR_factor_ref 0.1174 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 1538 _reflns_number_total 1669 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file tz4c00924_si_008.cif _cod_data_source_block 5 _cod_database_code 4519548 _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: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A O2: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A Uanis(C8) \\sim Ueq, Uanis(C7) \\sim Ueq: with sigma of 0.02 and sigma for terminal atoms of 0.04 Uanis(C7) \\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 Uanis(C5) \\sim Ueq: with sigma of 0.002 and sigma for terminal atoms of 0.004 Uanis(O2) \\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: C6(0.5) H6(0.5) C5(0.5) H5A(0.5) H5B(0.5) H5C(0.5) N1(0.5) C7(0.5) H7A(0.5) H7B(0.5) H7C(0.5) C8(0.5) H8A(0.5) H8B(0.5) H8C(0.5) 5.a Aromatic/amide H refined with riding coordinates: C3(H3), C6(H6) 5.b Idealised Me refined as rotating group: C5(H5A,H5B,H5C), C7(H7A,H7B,H7C), C8(H8A,H8B,H8C) ; _shelx_res_file ; TITL 5 in Pnma #62 5.res created by SHELXL-2018/3 at 10:24:17 on 11-Jun-2024 REM reset to Pnma #62 CELL 0.71073 7.6774 18.1243 10.1579 90 90 90 ZERR 4 0.0002 0.0006 0.0003 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 RIGU ISOR 0.02 0.04 C8 C7 ISOR 0.002 0.004 C7 SIMU C5 ISOR 0.002 0.004 C8 SIMU O2 ISOR 0.002 0.004 C5 ISOR 0.002 0.004 O2 L.S. 30 0 0 PLAN 30 TEMP 23 CONF MORE -1 BOND $H fmap 2 53 ACTA REM REM REM WGHT 0.100000 FVAR 0.11091 PB1 5 0.105147 0.750000 0.806551 10.50000 0.03494 0.03520 = 0.04906 0.00000 -0.00474 0.00000 O1 4 0.370928 0.842251 0.799647 11.00000 0.07522 0.05759 = 0.08822 -0.03623 0.00649 -0.00623 O3 4 -0.160434 0.750000 0.951102 10.50000 0.08659 0.07560 = 0.06186 0.00000 0.01706 0.00000 O2 4 0.192990 0.843702 0.965877 11.00000 0.08727 0.08595 = 0.08275 -0.01288 0.00296 -0.01625 C2 1 0.407472 0.937998 0.956152 11.00000 0.05586 0.04171 = 0.06496 -0.01663 -0.01061 0.00390 C3 1 0.573400 0.952668 0.912830 11.00000 0.06827 0.05959 = 0.09119 -0.04125 0.01182 -0.00355 AFIX 43 H3 2 0.623234 0.921297 0.850939 11.00000 -1.20000 AFIX 0 C4 1 0.328388 0.986400 1.041425 11.00000 0.06441 0.06910 = 0.10398 -0.04718 0.00980 -0.01109 C1 1 0.317234 0.871044 0.903210 11.00000 0.05611 0.04364 = 0.06178 -0.01874 -0.00710 0.00218 PART -1 C6 1 -0.200669 0.708903 1.030281 10.50000 0.11554 0.07977 = 0.04645 -0.00651 0.01287 -0.02544 AFIX 43 H6 2 -0.146923 0.663257 1.020335 10.50000 -1.20000 AFIX 0 C5 1 0.144497 0.971999 1.100132 10.50000 0.09669 0.10292 = 0.10656 -0.00682 0.00592 -0.00144 AFIX 137 H5A 2 0.077539 0.942808 1.039652 10.50000 -1.50000 H5B 2 0.086672 1.018229 1.114892 10.50000 -1.50000 H5C 2 0.155726 0.946069 1.182102 10.50000 -1.50000 AFIX 0 N1 3 -0.305486 0.711112 1.132409 10.50000 0.07074 0.14113 = 0.06286 0.02848 0.00453 0.01144 C7 1 -0.341811 0.649718 1.210746 10.50000 0.10117 0.10430 = 0.09824 0.00786 0.00407 -0.00349 AFIX 137 H7A 2 -0.281235 0.607491 1.176704 10.50000 -1.50000 H7B 2 -0.464883 0.640358 1.210064 10.50000 -1.50000 H7C 2 -0.304294 0.659089 1.299335 10.50000 -1.50000 AFIX 0 C8 1 -0.404347 0.775519 1.148468 10.50000 0.12251 0.12091 = 0.12352 -0.00011 0.00706 0.00310 AFIX 137 H8A 2 -0.375589 0.809998 1.080098 10.50000 -1.50000 H8B 2 -0.379141 0.797070 1.232671 10.50000 -1.50000 H8C 2 -0.526011 0.763592 1.143633 10.50000 -1.50000 AFIX 0 HKLF 4 REM 5 in Pnma #62 REM wR2 = 0.1174, GooF = S = 1.033, Restrained GooF = 1.052 for all data REM R1 = 0.0311 for 1538 Fo > 4sig(Fo) and 0.0334 for all 1669 data REM 115 parameters refined using 103 restraints END WGHT 0.0468 3.3615 REM Highest difference peak 1.466, deepest hole -0.954, 1-sigma level 0.153 Q1 1 0.0493 0.7500 0.8761 10.50000 0.05 1.47 Q2 1 0.1860 0.7500 0.8186 10.50000 0.05 1.45 Q3 1 0.1497 0.7500 0.7358 10.50000 0.05 1.28 Q4 1 0.1403 0.8693 0.9417 11.00000 0.05 1.18 Q5 1 -0.0287 0.7500 0.8008 10.50000 0.05 0.88 Q6 1 -0.2999 0.7500 0.9291 10.50000 0.05 0.87 Q7 1 0.0333 0.7500 0.7586 10.50000 0.05 0.80 Q8 1 0.1230 0.9989 1.0315 11.00000 0.05 0.67 Q9 1 0.1299 0.7928 0.7434 11.00000 0.05 0.62 Q10 1 0.3947 0.8132 0.8681 11.00000 0.05 0.56 Q11 1 0.2703 0.7803 0.8037 11.00000 0.05 0.55 Q12 1 0.2646 0.8185 0.9820 11.00000 0.05 0.53 Q13 1 0.3640 0.9847 1.0758 11.00000 0.05 0.50 Q14 1 0.0998 0.7008 0.8351 11.00000 0.05 0.46 Q15 1 0.3009 0.8549 0.8067 11.00000 0.05 0.41 Q16 1 -0.3724 0.8166 1.2374 11.00000 0.05 0.40 Q17 1 -0.2888 0.6206 1.2085 11.00000 0.05 0.37 Q18 1 0.1202 0.7500 0.9886 10.50000 0.05 0.36 Q19 1 0.1968 0.8183 0.8091 11.00000 0.05 0.34 Q20 1 0.5351 0.9802 0.8805 11.00000 0.05 0.34 Q21 1 0.4152 0.9533 0.9347 11.00000 0.05 0.33 Q22 1 0.4196 0.8626 0.6854 11.00000 0.05 0.33 Q23 1 -0.1069 0.7500 1.0261 10.50000 0.05 0.33 Q24 1 -0.1758 0.7018 1.1546 11.00000 0.05 0.33 Q25 1 -0.0937 0.7500 1.1377 10.50000 0.05 0.32 Q26 1 -0.6358 0.8022 1.2456 11.00000 0.05 0.31 Q27 1 0.1310 0.7500 1.0629 10.50000 0.05 0.30 Q28 1 0.1903 0.9517 1.1570 11.00000 0.05 0.30 Q29 1 0.2462 0.9006 1.1959 11.00000 0.05 0.30 Q30 1 0.3995 0.8588 0.7416 11.00000 0.05 0.29 ; _shelx_res_checksum 44372 _shelx_hkl_file ; 1 0 0 0.00 0.13 1 0 0 0.09 0.02 1 0 0 0.20 0.10 -1 0 0 0.22 0.19 -2 0 0 9.93 1.21 -2 0 0 7.49 0.80 2 0 0 9.75 1.67 2 0 0 7.72 0.68 2 0 0 8.10 0.86 -3 0 0 0.48 0.46 3 0 0 0.13 0.44 3 0 0 0.54 0.29 -3 0 0 -0.10 0.18 4 0 0 767.82 67.79 -4 0 0 813.26 67.63 5 0 0 0.25 0.84 5 0 0 -0.05 0.10 -5 0 0 -0.21 0.29 5 0 0 0.12 0.51 -5 0 0 -0.32 0.70 -6 0 0 81.64 7.84 6 0 0 73.59 6.37 -6 0 0 64.50 6.64 6 0 0 88.78 8.53 6 0 0 81.85 7.09 -7 0 0 -0.10 0.48 -7 0 0 -0.31 0.96 7 0 0 -1.29 1.44 7 0 0 0.04 0.86 -7 0 0 0.22 0.11 -8 0 0 17.59 1.41 8 0 0 13.90 3.87 -8 0 0 13.39 1.91 9 0 0 1.51 2.55 0 0 -1 0.28 0.10 0 0 1 0.19 0.03 0 0 1 0.11 0.13 0 0 -1 0.54 0.27 -1 0 -1 2.13 0.17 1 0 1 1.58 0.26 1 0 1 1.83 0.17 1 0 1 2.16 0.52 1 0 -1 2.11 0.56 1 0 -1 1.77 0.18 1 0 -1 1.55 0.30 -1 0 1 2.47 0.55 -2 0 1 339.02 27.58 2 0 1 352.90 27.56 2 0 -1 267.89 27.58 -3 0 1 9.00 1.11 -3 0 -1 9.92 1.08 -3 0 -1 10.72 0.90 3 0 -1 9.93 1.23 -3 0 1 11.78 1.64 3 0 -1 6.67 1.69 3 0 1 11.86 0.90 3 0 1 10.86 1.62 4 0 -1 144.83 11.98 4 0 1 157.56 12.81 4 0 -1 120.24 12.75 -4 0 -1 130.69 11.72 -4 0 1 160.64 12.69 -4 0 1 118.12 11.74 -5 0 1 15.13 1.79 5 0 -1 20.35 3.73 5 0 1 18.90 2.93 5 0 1 18.71 1.50 5 0 -1 19.41 2.15 -5 0 -1 15.77 1.77 6 0 -1 95.27 8.29 6 0 1 97.19 9.47 -6 0 -1 81.79 7.82 6 0 1 90.61 7.53 6 0 -1 92.65 9.68 -6 0 1 78.57 7.84 -6 0 1 93.42 8.93 -6 0 1 92.34 7.52 -7 0 -1 0.14 0.50 7 0 -1 -0.16 1.35 -7 0 1 -0.10 1.71 -7 0 -1 0.13 0.48 7 0 -1 -0.32 1.17 -7 0 1 -0.18 0.44 7 0 1 0.03 1.34 -7 0 1 0.07 0.11 7 0 1 -0.16 0.15 7 0 1 -2.06 1.22 -8 0 1 61.61 6.32 8 0 -1 60.99 5.69 -8 0 1 56.76 4.39 8 0 1 51.48 4.43 -8 0 -1 57.34 4.89 8 0 1 58.50 12.02 8 0 1 56.16 7.35 8 0 -1 41.94 6.76 -8 0 1 44.74 4.81 -8 0 -1 45.07 4.81 -8 0 -1 47.11 4.38 -9 0 -1 5.86 0.59 -9 0 -1 5.02 1.12 -9 0 1 6.27 1.30 -9 0 1 6.08 0.58 9 0 1 3.81 3.68 9 0 1 8.96 1.40 0 0 -2 141.20 11.90 0 0 2 130.25 11.84 -1 0 -2 379.59 33.55 -1 0 2 408.54 33.65 1 0 2 406.53 33.59 1 0 -2 376.63 33.64 -2 0 2 89.33 7.72 2 0 -2 68.45 7.70 2 0 -2 76.19 7.23 2 0 2 89.57 7.68 -2 0 -2 87.67 7.17 -2 0 2 82.91 7.22 -2 0 -2 82.71 7.57 2 0 2 86.66 7.17 3 0 2 196.78 17.35 -3 0 2 184.02 16.72 3 0 2 204.99 17.44 -3 0 -2 198.74 16.65 -3 0 2 195.46 17.33 4 0 2 184.20 16.81 -4 0 -2 191.75 15.86 -4 0 2 216.05 16.82 4 0 -2 152.94 16.93 4 0 2 192.75 16.86 4 0 -2 172.77 16.06 -4 0 2 186.65 15.93 5 0 -2 6.69 1.33 -5 0 2 8.39 1.86 -5 0 -2 7.01 1.14 5 0 2 5.65 1.82 5 0 2 7.12 0.63 -5 0 -2 6.53 0.62 5 0 2 7.62 0.67 -5 0 -2 5.95 0.95 5 0 2 7.98 2.31 -5 0 2 6.53 1.02 6 0 2 51.90 6.83 -6 0 -2 58.49 5.33 6 0 -2 57.06 5.74 -6 0 -2 53.39 5.29 -6 0 -2 60.58 4.97 6 0 2 62.95 6.92 -6 0 2 57.43 5.37 6 0 2 60.43 4.98 6 0 -2 51.92 6.95 -6 0 2 56.84 6.24 -6 0 2 64.19 4.97 -7 0 2 48.59 4.79 -7 0 2 58.53 4.36 -7 0 2 55.25 5.98 -7 0 -2 46.89 4.74 7 0 2 45.12 6.69 7 0 2 52.92 6.73 -7 0 -2 51.87 4.37 7 0 -2 50.98 5.38 7 0 2 49.17 4.38 -8 0 2 21.51 2.57 -8 0 2 24.75 2.03 -8 0 -2 24.51 2.62 8 0 2 25.27 4.95 -8 0 -2 21.09 2.59 8 0 -2 23.42 5.36 8 0 -2 24.47 3.37 -8 0 2 25.97 3.73 8 0 2 23.61 2.07 8 0 2 25.38 5.81 9 0 2 4.50 0.55 9 0 -2 2.96 1.58 -9 0 2 3.63 1.04 -9 0 -2 3.10 0.92 -9 0 2 4.50 0.44 9 0 2 1.91 3.35 -9 0 -2 4.54 0.46 0 0 -3 0.04 0.04 0 0 -3 -0.05 0.35 0 0 -3 0.25 0.05 0 0 -3 0.11 0.04 0 0 3 0.16 0.05 0 0 3 0.10 0.24 0 0 -3 0.53 0.28 0 0 3 0.38 0.37 -1 0 3 229.01 19.42 1 0 3 251.42 19.48 -1 0 -3 216.41 19.39 1 0 -3 192.22 19.40 -2 0 -3 110.72 8.95 -2 0 3 105.19 9.54 -2 0 -3 99.93 9.45 2 0 3 108.89 8.95 2 0 -3 91.38 9.61 2 0 -3 94.97 8.99 2 0 3 110.61 9.57 -3 0 -3 9.25 1.03 3 0 3 9.02 0.72 3 0 3 7.92 0.72 3 0 -3 7.62 0.75 -3 0 3 7.16 1.55 3 0 -3 6.38 1.85 3 0 -3 6.98 1.08 -3 0 3 8.43 1.08 3 0 3 11.20 1.95 -3 0 -3 8.07 0.71 4 0 3 14.94 1.26 -4 0 -3 15.28 1.59 4 0 -3 8.30 2.37 4 0 3 17.26 2.62 4 0 -3 11.02 1.68 -4 0 -3 12.40 1.50 -4 0 3 16.11 1.68 -4 0 -3 16.29 1.25 4 0 3 11.78 3.15 -4 0 3 16.15 2.27 5 0 -3 209.84 21.29 -5 0 -3 228.37 19.64 -5 0 3 241.48 20.63 -5 0 3 252.32 19.76 5 0 3 221.99 22.11 5 0 -3 202.69 19.87 5 0 3 244.79 21.12 -6 0 -3 27.20 2.37 6 0 3 26.33 2.38 -6 0 3 27.11 3.64 6 0 3 29.24 5.21 6 0 -3 22.82 3.10 6 0 3 30.30 2.41 -6 0 3 30.50 2.37 6 0 3 31.18 4.44 -6 0 -3 26.08 2.76 -6 0 -3 27.10 2.80 -6 0 3 27.22 2.86 6 0 -3 28.66 5.53 -7 0 3 2.45 0.30 -7 0 3 2.82 1.37 7 0 -3 2.53 1.14 -7 0 -3 2.83 0.33 -7 0 -3 2.24 0.78 7 0 3 2.12 1.96 -7 0 -3 2.86 0.85 7 0 3 3.63 0.58 7 0 3 2.66 2.16 -7 0 3 1.92 0.81 7 0 3 2.32 0.36 -8 0 3 11.33 1.04 8 0 3 8.27 3.19 -8 0 -3 12.75 1.05 -8 0 3 11.57 1.73 8 0 -3 14.37 2.49 -8 0 -3 10.06 1.62 8 0 3 6.37 2.94 8 0 -3 9.83 3.68 -8 0 -3 12.23 2.05 8 0 3 11.80 1.09 -9 0 -3 22.03 2.81 9 0 3 26.10 2.29 9 0 3 29.08 8.73 9 0 -3 27.60 3.69 -9 0 3 26.72 2.23 -9 0 3 27.74 2.93 0 0 -4 30.39 3.65 0 0 -4 33.87 2.82 0 0 4 36.45 3.70 0 0 -4 35.36 3.12 0 0 4 30.43 2.82 0 0 4 38.69 3.13 0 0 -4 30.27 2.82 0 0 4 33.03 2.82 1 0 -4 298.34 26.97 1 0 -4 296.95 26.24 -1 0 -4 312.97 26.90 -1 0 4 326.13 26.89 -2 0 -4 2.36 0.21 2 0 4 1.50 0.81 -2 0 4 1.84 0.87 -2 0 4 2.05 0.19 2 0 -4 1.70 0.52 2 0 -4 2.78 1.08 2 0 4 1.51 0.20 -2 0 4 1.67 0.22 -2 0 4 2.04 0.20 2 0 4 1.57 0.50 -2 0 -4 2.59 1.02 2 0 4 2.05 0.21 -2 0 -4 2.43 0.55 -2 0 -4 1.66 0.19 3 0 -4 354.45 36.64 3 0 4 490.36 36.68 -3 0 4 460.65 36.53 -3 0 -4 430.71 36.39 3 0 -4 370.18 35.68 4 0 4 12.55 1.14 4 0 4 12.94 1.13 4 0 4 12.62 2.72 -4 0 -4 14.04 1.51 -4 0 4 13.56 2.48 -4 0 -4 12.48 1.51 4 0 4 19.65 3.38 -4 0 -4 13.42 1.13 4 0 -4 9.73 2.70 -4 0 4 12.51 1.58 5 0 4 16.81 3.32 -5 0 4 12.08 2.50 5 0 4 14.69 1.33 -5 0 -4 15.85 1.31 5 0 -4 16.37 3.93 5 0 4 14.24 1.31 -5 0 4 16.72 1.89 -5 0 -4 15.84 1.77 -5 0 -4 13.93 1.76 5 0 4 16.87 3.60 -6 0 -4 0.21 0.13 -6 0 4 -0.19 0.57 -6 0 -4 0.45 0.57 -6 0 4 -0.20 0.83 6 0 4 0.30 0.15 6 0 -4 0.51 0.70 6 0 4 0.20 0.23 -6 0 4 0.35 0.12 6 0 4 0.46 1.45 6 0 4 -0.16 1.33 6 0 -4 -0.46 1.31 -7 0 -4 107.16 8.49 7 0 4 106.23 11.43 -7 0 -4 93.68 9.21 -7 0 4 105.99 8.48 -7 0 4 109.92 9.05 7 0 -4 89.88 9.34 -7 0 4 100.21 10.01 -7 0 -4 98.21 8.93 7 0 4 92.91 8.50 8 0 4 3.52 0.56 -8 0 4 2.38 0.31 8 0 -4 2.68 1.19 8 0 4 0.76 2.13 8 0 4 3.33 0.42 -8 0 4 2.08 0.88 -8 0 -4 2.82 0.38 8 0 4 0.42 2.07 -8 0 -4 1.85 0.84 -9 0 -4 2.04 0.90 9 0 4 4.20 0.81 9 0 -4 2.46 1.45 -9 0 4 2.55 0.33 9 0 4 4.72 3.62 -9 0 -4 3.25 0.41 -9 0 4 1.92 0.95 0 0 -5 0.11 0.07 0 0 -5 0.02 0.07 0 0 -5 -0.15 0.37 0 0 5 0.06 0.45 0 0 5 -0.03 0.54 0 0 -5 0.18 0.82 0 0 5 -0.02 0.07 -1 0 -5 294.20 27.63 1 0 -5 295.48 27.76 1 0 5 326.94 27.67 1 0 -5 310.65 26.89 -1 0 5 347.51 27.72 2 0 5 6.52 0.57 -2 0 -5 6.85 0.57 2 0 -5 5.54 0.57 2 0 -5 6.43 1.04 2 0 5 5.51 0.56 2 0 -5 3.71 1.34 -2 0 -5 6.78 1.03 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5.76 2 -21 -5 -0.41 0.49 -2 -21 5 0.14 0.33 -2 21 -5 -1.34 2.67 2 -21 -5 0.13 0.17 -2 -21 5 0.62 0.32 -2 21 5 -2.20 2.40 -2 -21 -5 -0.13 0.21 2 -21 5 -1.14 2.45 2 -21 5 0.41 0.28 2 -21 5 0.13 0.25 0 22 0 46.93 4.33 0 -22 0 50.40 4.36 0 -22 0 50.43 6.88 0 22 0 51.01 7.04 0 -22 0 56.09 4.37 -1 22 0 -0.36 1.72 1 -22 0 -0.14 0.16 1 22 0 1.28 2.91 -1 -22 0 -0.05 2.68 1 -22 0 1.51 1.79 -1 -22 0 -0.13 0.33 -1 22 0 -0.04 0.15 1 22 0 -0.31 0.15 1 -22 0 0.50 0.20 2 22 0 12.45 5.75 -2 -22 0 0.58 2.23 -2 22 0 0.85 1.29 2 -22 0 2.60 0.36 2 -22 0 1.81 0.28 2 22 0 1.90 0.30 -2 -22 0 1.84 0.33 -3 22 0 -1.22 0.83 3 -22 0 0.10 0.12 -3 -22 0 0.10 0.25 3 -22 0 0.41 0.21 3 -22 0 -0.02 0.10 3 -22 0 -0.33 0.33 0 -22 -1 -2.71 1.51 0 22 1 2.65 2.51 0 -22 -1 0.07 0.18 0 -22 1 0.02 0.21 0 22 -1 -2.91 1.78 0 22 -1 -0.11 0.17 0 -22 1 -2.75 1.92 0 -22 1 -0.26 0.22 -1 -22 1 3.18 2.65 -1 22 -1 4.66 2.08 1 -22 -1 2.99 0.38 1 22 1 3.20 0.35 -1 22 -1 2.66 0.38 1 -22 1 0.47 2.14 1 -22 1 3.31 0.43 1 22 -1 3.99 2.85 1 -22 1 3.68 0.43 -1 -22 -1 3.91 2.38 1 22 -1 2.79 0.39 -1 22 1 3.26 2.33 -2 -22 1 34.10 6.21 -2 22 -1 29.73 2.45 2 22 1 28.04 6.88 2 -22 -1 25.09 2.72 -2 -22 1 28.63 2.49 2 -22 -1 27.46 2.41 -2 22 -1 26.38 3.89 2 -22 1 26.37 2.42 2 -22 1 26.47 4.38 -2 -22 -1 31.50 2.48 -2 22 1 28.48 3.74 2 -22 1 29.47 2.44 2 -22 1 30.53 2.47 2 -22 1 25.99 2.42 -2 -22 -1 24.53 5.57 -3 22 -1 -0.84 1.00 -3 -22 1 0.35 0.26 3 -22 1 0.80 0.15 -3 -22 -1 0.77 0.28 3 -22 1 0.66 0.14 3 -22 1 1.22 0.27 0 22 2 24.77 5.21 0 -22 2 30.82 5.92 0 22 -2 20.12 4.57 0 -22 2 24.42 2.16 0 -22 2 24.69 2.20 -1 -22 2 6.47 3.49 1 -22 -2 5.43 1.12 -1 -22 2 6.48 0.69 1 -22 -2 6.08 0.62 -1 22 -2 6.03 2.40 1 22 2 10.16 4.09 -1 -22 2 6.28 0.70 1 -22 2 6.05 2.68 1 -22 2 7.07 0.72 -1 22 2 6.94 2.34 1 -22 2 5.86 0.73 -1 -22 -2 6.26 0.65 1 22 -2 5.63 2.79 -2 -22 2 0.99 0.29 2 22 2 3.21 3.90 2 -22 -2 0.96 0.18 -2 22 -2 -1.49 1.20 2 -22 -2 1.12 0.52 -2 -22 2 1.36 2.58 2 -22 2 1.58 0.25 -2 -22 -2 -1.32 2.12 2 -22 2 1.23 0.20 2 -22 2 1.55 0.30 2 22 -2 -2.44 3.10 -2 -22 -2 1.06 0.26 2 -22 2 2.29 1.91 -3 -22 2 12.61 1.21 -3 22 -2 13.79 2.62 3 -22 2 11.03 1.10 -3 -22 -2 13.11 1.19 3 -22 2 14.47 1.19 3 -22 2 9.16 2.57 0 -22 3 -0.17 0.22 0 22 -3 -1.99 2.20 0 -22 3 0.13 2.35 0 22 3 0.24 2.69 0 -22 3 0.26 0.24 0 -22 -3 -0.01 0.16 0 -22 -3 -0.14 0.68 -1 -22 3 17.56 1.51 -1 -22 3 16.20 1.51 -1 -22 3 10.21 3.91 1 -22 -3 14.76 1.43 1 -22 -3 12.85 1.90 1 22 3 14.57 4.55 -1 22 -3 11.66 3.30 -1 22 3 21.28 3.88 1 -22 3 17.79 1.50 1 -22 3 19.07 1.50 1 22 -3 11.68 4.40 -1 -22 -3 14.13 2.21 -1 -22 -3 16.28 1.46 1 -22 3 17.86 1.46 1 -22 3 10.33 3.68 -2 -22 3 6.74 0.78 -2 -22 3 7.88 0.78 -2 22 -3 3.65 2.08 2 -22 3 6.57 0.68 2 -22 3 7.44 0.76 2 -22 3 7.34 0.73 -2 22 3 5.91 2.01 2 -22 3 4.88 2.96 -2 -22 -3 7.54 0.73 0 -22 -4 1.49 0.78 0 -22 4 2.32 0.37 0 -22 -4 1.74 0.27 0 -22 4 2.18 0.38 0 22 4 -0.70 3.12 -1 -22 4 13.54 1.23 1 -22 -4 11.95 1.14 1 -22 -4 9.78 1.63 -1 -22 4 13.74 1.25 1 -22 4 6.53 3.47 1 -22 4 13.30 1.23 1 -22 4 14.05 1.23 -1 22 4 13.80 3.65 -1 -22 -4 13.08 1.17 0 23 0 -0.13 2.63 0 -23 0 -0.35 2.20 0 -23 0 0.00 0.20 1 -23 0 1.02 2.19 1 -23 0 0.59 0.21 1 -23 0 0.08 0.18 -1 23 0 0.12 1.87 -1 -23 0 1.78 3.49 -2 23 0 31.77 5.93 2 -23 0 29.41 2.51 2 -23 0 26.61 2.48 -2 -23 0 31.07 2.55 0 -23 -1 34.37 2.88 0 23 -1 34.63 6.64 0 -23 1 35.92 2.90 0 -23 1 31.89 2.90 0 23 1 28.03 5.71 0 -23 1 24.14 5.26 0 -23 -1 29.96 5.41 -1 23 -1 -0.90 2.86 1 -23 -1 1.21 0.22 -1 -23 1 1.50 0.30 -1 23 1 0.51 1.98 1 -23 1 -0.90 2.07 1 -23 1 1.07 0.25 -1 -23 -1 1.38 0.28 2 -23 1 1.45 0.22 0 -23 -2 0.39 0.19 0 -23 2 0.79 4.11 0 -23 2 -0.21 0.22 0 -23 2 0.48 0.25 0 23 2 -2.49 2.82 0 -23 -2 0.31 0.68 1 -23 -2 5.94 1.35 1 -23 -2 7.06 0.76 -1 23 -2 2.97 2.44 -1 -23 2 8.64 0.85 -1 -23 2 9.19 0.86 1 -23 2 9.84 0.85 1 -23 2 10.97 3.27 -1 -23 -2 8.41 0.82 -1 23 2 9.47 2.78 1 -23 2 8.47 0.82 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 81093 _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 0.10515(3) 0.750000 0.80655(2) 0.03973(18) Uani 1 2 d S T P A . O1 O 0.3709(9) 0.8423(5) 0.7996(5) 0.0737(19) Uani 1 1 d . . . . . O3 O -0.1604(11) 0.750000 0.9511(7) 0.0747(17) Uani 1 2 d S T P . . O2 O 0.1930(7) 0.8437(3) 0.9659(6) 0.0853(14) Uani 1 1 d . U . . . C2 C 0.4075(7) 0.9380(4) 0.9562(7) 0.0542(14) Uani 1 1 d . . . . . C3 C 0.5734(10) 0.9527(5) 0.9128(8) 0.073(2) Uani 1 1 d . . . . . H3 H 0.623234 0.921297 0.850939 0.088 Uiso 1 1 calc R U . . . C4 C 0.3284(9) 0.9864(4) 1.0414(8) 0.079(2) Uani 1 1 d . . . . . C1 C 0.3172(8) 0.8710(3) 0.9032(6) 0.0538(12) Uani 1 1 d . . . . . C6 C -0.201(2) 0.7089(8) 1.0303(13) 0.081(4) Uani 0.5 1 d . . P A -1 H6 H -0.146923 0.663257 1.020335 0.097 Uiso 0.5 1 calc R U P A -1 C5 C 0.144(3) 0.9720(15) 1.100(2) 0.102(5) Uani 0.5 1 d . U P B -1 H5A H 0.077539 0.942808 1.039652 0.153 Uiso 0.5 1 calc R U P B -1 H5B H 0.086672 1.018229 1.114892 0.153 Uiso 0.5 1 calc R U P B -1 H5C H 0.155726 0.946069 1.182102 0.153 Uiso 0.5 1 calc R U P B -1 N1 N -0.3055(16) 0.7111(10) 1.1324(13) 0.092(4) Uani 0.5 1 d . . P A -1 C7 C -0.342(4) 0.6497(18) 1.211(2) 0.101(5) Uani 0.5 1 d . U P A -1 H7A H -0.281235 0.607491 1.176704 0.152 Uiso 0.5 1 calc R U P A -1 H7B H -0.464883 0.640358 1.210064 0.152 Uiso 0.5 1 calc R U P A -1 H7C H -0.304294 0.659089 1.299335 0.152 Uiso 0.5 1 calc R U P A -1 C8 C -0.404(3) 0.7755(17) 1.148(3) 0.122(7) Uani 0.5 1 d . U P A -1 H8A H -0.375589 0.809998 1.080098 0.183 Uiso 0.5 1 calc R U P A -1 H8B H -0.379141 0.797070 1.232671 0.183 Uiso 0.5 1 calc R U P A -1 H8C H -0.526011 0.763592 1.143633 0.183 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 0.0349(2) 0.0352(2) 0.0491(2) 0.000 -0.00474(7) 0.000 O1 0.075(4) 0.058(4) 0.088(4) -0.036(3) 0.0065(19) -0.006(3) O3 0.087(4) 0.076(5) 0.062(4) 0.000 0.017(3) 0.000 O2 0.087(2) 0.086(2) 0.0828(19) -0.0129(17) 0.0030(16) -0.0162(16) C2 0.056(3) 0.042(3) 0.065(3) -0.017(3) -0.011(2) 0.004(2) C3 0.068(3) 0.060(4) 0.091(5) -0.041(4) 0.012(3) -0.004(3) C4 0.064(4) 0.069(4) 0.104(5) -0.047(4) 0.010(3) -0.011(3) C1 0.056(3) 0.044(3) 0.062(3) -0.019(2) -0.007(2) 0.002(2) C6 0.116(12) 0.080(8) 0.046(5) -0.007(5) 0.013(6) -0.025(7) C5 0.097(5) 0.103(6) 0.107(6) -0.007(4) 0.006(4) -0.001(4) N1 0.071(8) 0.141(10) 0.063(6) 0.028(7) 0.005(5) 0.011(6) C7 0.101(6) 0.104(6) 0.098(6) 0.008(4) 0.004(4) -0.003(4) C8 0.123(8) 0.121(7) 0.124(7) 0.000(4) 0.007(4) 0.003(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 O1 Pb1 O1 78.6(4) 8_575 . O1 Pb1 O1 77.1(3) 3_466 6_557 O1 Pb1 O1 96.5(3) . 6_557 O1 Pb1 O1 96.5(3) 8_575 3_466 O1 Pb1 O1 154.52(9) 8_575 6_557 O1 Pb1 O1 154.52(9) . 3_466 O3 Pb1 O1 130.01(16) . . O3 Pb1 O1 130.02(16) . 8_575 O3 Pb1 O1 72.00(18) . 3_466 O3 Pb1 O1 72.00(18) . 6_557 O2 Pb1 O1 91.0(2) 8_575 3_466 O2 Pb1 O1 91.0(2) . 6_557 O2 Pb1 O1 104.2(2) . 8_575 O2 Pb1 O1 152.34(18) . 3_466 O2 Pb1 O1 104.2(2) 8_575 . O2 Pb1 O1 50.44(17) . . O2 Pb1 O1 152.34(18) 8_575 6_557 O2 Pb1 O1 50.45(17) 8_575 8_575 O2 Pb1 O3 80.60(19) . . O2 Pb1 O3 80.60(19) 8_575 . O2 Pb1 O2 88.2(3) 8_575 . Pb1 O1 Pb1 97.7(2) . 6_657 C1 O1 Pb1 145.4(6) . 6_657 C1 O1 Pb1 89.3(4) . . C6 O3 Pb1 129.3(10) . . C1 O2 Pb1 98.6(4) . . C3 C2 C4 119.2(6) . . C3 C2 C1 118.1(6) . . C4 C2 C1 122.6(6) . . C2 C3 H3 118.7 . . C2 C3 C4 122.7(6) . 5_677 C4 C3 H3 118.7 5_677 . C2 C4 C3 118.0(7) . 5_677 C2 C4 C5 122.4(11) . . C3 C4 C5 119.3(12) 5_677 . O1 C1 O2 121.2(6) . . O1 C1 C2 119.4(6) . . O2 C1 C2 119.5(5) . . O3 C6 H6 112.6 . . O3 C6 N1 134.7(16) . . N1 C6 H6 112.6 . . 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 . . C6 N1 C7 123.2(19) . . C6 N1 C8 116.7(19) . . C7 N1 C8 119.3(18) . . 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 . . 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 . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Pb1 O1 2.639(7) 8_575 Pb1 O1 2.682(7) 3_466 Pb1 O1 2.639(7) . Pb1 O1 2.682(7) 6_557 Pb1 O3 2.513(8) . Pb1 O2 2.441(5) 8_575 Pb1 O2 2.441(5) . O1 C1 1.245(7) . O3 C6 1.139(14) . O2 C1 1.249(8) . C2 C3 1.374(9) . C2 C4 1.374(9) . C2 C1 1.497(8) . C3 H3 0.9300 . C3 C4 1.416(9) 5_677 C4 C5 1.55(2) . C6 H6 0.9300 . C6 N1 1.314(19) . C5 H5A 0.9600 . C5 H5B 0.9600 . C5 H5C 0.9600 . N1 C7 1.40(3) . N1 C8 1.40(3) . C7 H7A 0.9600 . C7 H7B 0.9600 . C7 H7C 0.9600 . C8 H8A 0.9600 . C8 H8B 0.9600 . C8 H8C 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 O1 C1 O2 7.4(7) . . . . Pb1 O1 C1 O2 -95.2(10) 6_657 . . . Pb1 O1 C1 C2 82.5(11) 6_657 . . . Pb1 O1 C1 C2 -174.9(5) . . . . Pb1 O3 C6 N1 158.9(15) . . . . Pb1 O2 C1 O1 -8.1(7) . . . . Pb1 O2 C1 C2 174.2(5) . . . . O3 C6 N1 C7 175(2) . . . . O3 C6 N1 C8 6(3) . . . . C3 C2 C4 C3 -3.8(14) . . . 5_677 C3 C2 C4 C5 -177.1(13) . . . . C3 C2 C1 O1 -18.9(10) . . . . C3 C2 C1 O2 158.9(7) . . . . C4 C2 C3 C4 4.0(15) . . . 5_677 C4 C2 C1 O1 158.4(8) . . . . C4 C2 C1 O2 -23.9(11) . . . . C1 C2 C3 C4 -178.7(8) . . . 5_677 C1 C2 C4 C3 179.0(8) . . . 5_677 C1 C2 C4 C5 5.7(16) . . . .