#------------------------------------------------------------------------------ #$Date: 2024-06-21 03:11:53 +0300 (Fri, 21 Jun 2024) $ #$Revision: 292492 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/57/19/1571954.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_1571954 loop_ _publ_author_name 'Testa, Marianna' 'De Santis, Antonio' 'Tinti, Gemma Maria' 'Paoloni, Alessandro' 'Papalino, Giuseppe' 'Felici, Giulietto' 'Chubinidze, Zaza' 'Matteocci, Fabio' 'Auf der Maur, Matthias' 'Rizzato, Silvia' 'Lo Presti, Leonardo' 'Viola, Ilenia' 'Morganti, Silvio' 'Rovelli, Chiara' _publ_section_title ; Direct detection of minimum ionizing charged particles in perovskite single crystal detector with single particle sensitivity ; _journal_name_full Nanoscale _journal_paper_doi 10.1039/D4NR01556H _journal_year 2024 _chemical_formula_moiety 'C H6 Br3 N Pb' _chemical_formula_sum 'C H6 Br3 N Pb' _chemical_formula_weight 478.92 _chemical_name_systematic 'Methylamonium bromide lead perovskite' _space_group_crystal_system cubic _space_group_IT_number 221 _space_group_name_Hall '-P 4 2 3' _space_group_name_H-M_alt 'P m -3 m' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary iterative _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2017/1 _audit_update_record ; 2024-04-03 deposited with the CCDC. 2024-06-03 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 1 _cell_length_a 5.9175(3) _cell_length_b 5.9175(3) _cell_length_c 5.9175(3) _cell_measurement_reflns_used 2692 _cell_measurement_temperature 293(2) _cell_measurement_theta_max 29.92 _cell_measurement_theta_min 3.44 _cell_volume 207.212(18) _computing_cell_refinement 'SAINT+ (Bruker AXS, Madison (USA) 1994-1996)' _computing_data_collection 'SAINT+ (Bruker AXS, Madison (USA) 1994-1996)' _computing_data_reduction 'SAINT+ (Bruker AXS, Madison (USA) 1994-1996)' _computing_molecular_graphics 'DIAMOND v3.2k (Brandenburg,Bonn,DE, 1997-2014)' _computing_structure_refinement 'SHELXL-2017/1 (Sheldrick, 2017)' _computing_structure_solution 'SHELXS-2013/1 (Sheldrick, 2013)' _diffrn_ambient_temperature 293(2) _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 1.000 _diffrn_measurement_device_type 'Bruker AXS smart APEX II' _diffrn_measurement_method \w-scan _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0245 _diffrn_reflns_av_unetI/netI 0.0063 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 1.000 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_k_max 8 _diffrn_reflns_limit_k_min -8 _diffrn_reflns_limit_l_max 8 _diffrn_reflns_limit_l_min -8 _diffrn_reflns_number 3164 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 1.000 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.162 _diffrn_reflns_theta_min 3.442 _diffrn_source 'Sealed X-ray tube' _exptl_absorpt_coefficient_mu 34.716 _exptl_absorpt_correction_T_max 0.4326 _exptl_absorpt_correction_T_min 0.1385 _exptl_absorpt_correction_type empirical _exptl_absorpt_process_details 'Sadabs (Bruker, 2007/4)' _exptl_crystal_colour orange _exptl_crystal_description rod _exptl_crystal_F_000 206 _exptl_crystal_recrystallization_method 'inverse temperature crystallization from dimethylformamide (DMF)' _exptl_crystal_size_max 0.450 _exptl_crystal_size_mid 0.100 _exptl_crystal_size_min 0.075 _refine_diff_density_max 0.694 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.096 _refine_ls_extinction_coef 0.0327(18) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_extinction_method 'SHELXL-2017/1 (Sheldrick 2017)' _refine_ls_goodness_of_fit_ref 1.271 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 17 _refine_ls_number_reflns 90 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.271 _refine_ls_R_factor_all 0.0106 _refine_ls_R_factor_gt 0.0106 _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^)+(0.0247P)^2^+0.0125P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0305 _refine_ls_wR_factor_ref 0.0305 _reflns_Friedel_coverage 0.000 _reflns_number_gt 91 _reflns_number_total 91 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d4nr01556h2.cif _cod_data_source_block PEROVRT _cod_original_cell_volume 207.21(3) _cod_database_code 1571954 _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_res_file ; TITL MAPbBr3 RT shelx.res created by SHELXL-2017/1 at 16:47:30 on 27-Feb-2021 CELL 0.71073 5.9175 5.9175 5.9175 90.000 90.000 90.000 ZERR 1 0.0003 0.0003 0.0003 0.000 0.000 0.000 LATT 1 SYMM -X,-Y,+Z SYMM -X,+Y,-Z SYMM +X,-Y,-Z SYMM +Z,+X,+Y SYMM +Z,-X,-Y SYMM -Z,-X,+Y SYMM -Z,+X,-Y SYMM +Y,+Z,+X SYMM -Y,+Z,-X SYMM +Y,-Z,-X SYMM -Y,-Z,+X SYMM +Y,+X,-Z SYMM -Y,-X,-Z SYMM +Y,-X,+Z SYMM -Y,+X,+Z SYMM +X,+Z,-Y SYMM -X,+Z,+Y SYMM -X,-Z,-Y SYMM +X,-Z,+Y SYMM +Z,+Y,-X SYMM +Z,-Y,+X SYMM -Z,+Y,+X SYMM -Z,-Y,-X SFAC Br C N Pb H He UNIT 3 1 1 1 6 0 L.S. 250 PLAN 20 DAMP 1000 BOND $H LIST 3 FMAP 2 MERG 2 MORE -1 ACTA BOND$H CONF EADP N1 C2 WGHT 0.024700 0.012500 EXTI 0.032654 FVAR 0.26094 PB1 4 0.500000 0.500000 0.500000 10.02083 0.02580 0.02580 = 0.02580 0.00000 0.00000 0.00000 BR2 1 0.500000 0.500000 0.000000 10.06250 0.13579 0.13579 = 0.02198 0.00000 0.00000 0.00000 PART -1 DFIX 0.75 0.01 N1 CENT C2 CENT AFIX 6 N1 3 -0.066022 0.112001 0.029506 10.02083 0.05232 0.05244 = 0.01337 -0.00766 -0.00555 0.01027 H1A 5 -0.101755 0.185651 -0.096604 10.02083 -1.50000 H1B 5 0.023687 0.198059 0.114166 10.02083 -1.50000 H1C 5 -0.191313 0.079793 0.106001 10.02083 -1.50000 C2 2 0.051567 -0.097941 -0.028291 10.02083 0.05232 0.05244 = 0.01337 -0.00766 -0.00555 0.01027 H2A 5 0.093666 -0.175560 0.107752 10.02083 -1.50000 H2B 5 0.184713 -0.063406 -0.114231 10.02083 -1.50000 H2C 5 -0.046672 -0.192563 -0.116344 10.02083 -1.50000 AFIX 0 PART -2 10.0 CENT 6 10.000000 10.000000 10.000000 10.00000 10.02000 PART 0 HKLF 4 REM MAPbBr3 RT REM R1 = 0.0106 for 91 Fo > 4sig(Fo) and 0.0106 for all 91 data REM 17 parameters refined using 0 restraints END WGHT 0.0246 0.0156 REM Highest difference peak 0.694, deepest hole -0.489, 1-sigma level 0.096 Q1 1 0.3481 0.5000 0.5000 10.12500 0.05 0.69 Q2 1 0.3688 0.5000 0.0000 10.25000 0.05 0.61 Q3 1 0.0000 0.5000 0.0000 10.06250 0.05 0.23 Q4 1 0.0000 0.2601 0.0000 10.12500 0.05 0.23 Q5 1 -0.2712 0.2712 -0.2712 10.16667 0.05 0.18 Q6 1 0.3325 0.5000 0.2329 10.50000 0.05 0.18 Q7 1 0.0000 0.4050 0.0000 10.12500 0.05 0.16 Q8 1 0.0000 0.3907 0.2310 10.50000 0.05 0.16 Q9 1 0.2675 0.5000 0.0000 10.25000 0.05 0.15 Q10 1 0.5000 0.5000 0.1331 10.12500 0.05 0.15 Q11 1 0.2452 0.5000 0.2452 10.25000 0.05 0.14 Q12 1 0.0000 0.5000 0.0830 10.25000 0.05 0.12 Q13 1 0.0000 0.5000 0.1840 10.25000 0.05 0.07 Q14 1 0.0000 0.1557 0.1557 10.25000 0.05 0.07 Q15 1 0.3523 0.3523 0.3523 10.16667 0.05 0.06 ; _shelx_res_checksum 47399 _shelx_hkl_file ; -1 0 0 433.02 14.05 -1 0 0 389.70 9.93 0 -1 0 407.46 13.88 0 -1 0 410.04 12.19 0 0 -1 380.77 13.75 0 0 1 403.04 13.90 0 0 1 420.33 9.88 0 0 1 418.06 11.41 0 1 0 431.29 14.06 0 1 0 423.58 10.24 1 0 0 421.10 13.93 -1 -1 0 146.79 4.72 -1 -1 0 157.32 3.87 -1 0 1 155.57 5.52 -1 0 1 160.16 4.41 -1 1 0 165.00 5.34 0 -1 -1 151.03 5.47 0 -1 -1 161.59 4.63 0 -1 -1 158.59 3.81 0 -1 1 166.42 5.50 0 -1 1 164.56 3.84 0 1 1 155.55 5.47 1 -1 0 168.56 5.33 1 -1 0 160.41 4.61 1 -1 0 155.18 3.83 1 0 -1 162.85 5.54 1 0 -1 162.99 4.65 1 0 1 147.44 5.47 1 0 1 155.58 3.80 1 0 1 164.68 4.45 1 1 0 149.83 5.79 1 1 0 160.32 4.38 1 1 0 153.81 3.91 -1 -1 -1 20.87 1.17 -1 -1 -1 20.77 0.75 -1 -1 -1 20.69 0.52 -1 -1 1 20.22 0.60 -1 1 -1 20.94 0.80 -1 1 -1 21.66 0.64 -1 1 -1 20.66 0.68 -1 1 -1 20.37 0.59 -1 1 1 20.53 0.94 -1 1 1 20.19 0.58 -1 1 1 20.53 0.68 -1 1 1 21.15 0.54 1 -1 -1 20.41 0.95 1 -1 -1 20.36 0.68 1 -1 1 20.54 0.79 1 -1 1 21.36 0.58 1 1 -1 20.63 1.25 1 1 -1 20.33 0.59 1 1 1 21.43 1.21 1 1 1 20.02 0.62 -2 0 0 943.37 27.96 -2 0 0 995.88 23.00 0 -2 0 978.87 32.07 0 -2 0 963.94 28.08 0 -2 0 1000.00 23.10 0 0 -2 916.41 32.03 0 0 -2 899.88 27.88 0 0 2 964.38 22.86 0 0 2 983.69 26.40 0 2 0 951.33 32.11 0 2 0 943.32 23.64 2 0 0 954.35 31.99 -2 0 1 424.93 13.88 -2 0 1 406.68 9.66 -1 -2 0 403.97 9.75 -1 2 0 415.14 13.56 -1 2 0 383.45 11.27 -1 2 0 399.73 9.94 0 -1 -2 399.46 13.66 0 -1 -2 401.00 11.96 0 -1 2 387.38 13.58 0 -1 2 416.14 9.76 0 -1 2 419.54 11.20 0 1 -2 377.06 10.04 0 1 2 394.59 9.71 0 1 2 395.93 11.12 1 -2 0 383.68 13.46 1 -2 0 399.47 11.76 1 -2 0 424.58 9.66 1 2 0 405.21 14.03 1 2 0 393.38 11.10 1 2 0 395.62 10.02 2 0 -1 428.66 13.86 2 0 -1 412.79 11.82 2 0 -1 397.35 9.94 2 0 1 383.08 13.99 -2 -1 0 412.86 11.83 -2 -1 0 403.53 9.67 -2 -1 0 387.56 11.12 -2 1 0 424.46 13.74 -2 1 0 378.15 11.25 -1 0 -2 393.54 13.61 -1 0 -2 402.64 11.82 -1 0 2 400.31 13.67 -1 0 2 405.45 9.72 -1 0 2 403.33 11.24 0 -2 -1 401.51 13.70 0 -2 -1 407.22 11.88 0 -2 1 419.76 9.81 0 2 -1 403.73 13.84 0 2 -1 389.27 13.69 0 2 -1 408.10 10.01 0 2 1 428.80 13.68 0 2 1 393.79 11.19 0 2 1 393.86 9.94 1 0 -2 413.43 13.71 1 0 -2 408.22 11.82 1 0 -2 404.64 9.92 1 0 2 421.21 13.63 1 0 2 409.04 9.65 1 0 2 415.88 11.19 2 -1 0 417.81 13.53 2 -1 0 407.44 11.72 2 -1 0 387.83 9.64 2 1 0 387.53 14.30 2 1 0 409.70 9.99 -2 -1 -1 147.28 5.91 -2 -1 -1 143.97 4.66 -2 -1 -1 155.87 3.71 -2 -1 1 164.27 6.16 -2 -1 1 154.52 3.73 -2 -1 1 151.46 4.37 -2 1 -1 150.06 5.38 -2 1 -1 161.23 4.53 -2 1 -1 149.43 4.41 -2 1 1 152.95 5.47 -2 1 1 153.14 3.78 -2 1 1 149.95 4.45 -1 -2 -1 142.66 5.78 -1 -2 -1 155.37 4.66 -1 -2 -1 159.21 3.71 -1 -2 1 158.24 3.74 -1 -1 -2 153.30 5.58 -1 -1 -2 153.99 4.57 -1 -1 2 146.01 5.57 -1 -1 2 155.04 3.73 -1 -1 2 154.79 4.27 -1 1 -2 150.22 5.31 -1 1 -2 155.12 4.50 -1 1 -2 150.43 3.86 -1 1 2 160.04 5.52 -1 1 2 153.73 3.75 -1 1 2 155.54 4.31 -1 2 -1 155.90 5.16 -1 2 -1 151.35 4.42 -1 2 -1 152.98 3.86 -1 2 1 161.49 5.40 -1 2 1 153.79 4.37 -1 2 1 158.11 3.83 1 -2 -1 159.83 5.45 1 -2 -1 160.29 4.54 1 -2 -1 151.41 3.77 1 -2 1 162.29 3.79 1 -1 -2 158.46 5.53 1 -1 -2 158.32 4.56 1 -1 2 154.69 5.34 1 -1 2 164.78 3.73 1 -1 2 160.56 4.30 1 1 -2 153.50 5.63 1 1 -2 156.60 4.59 1 1 -2 155.61 3.85 1 1 2 156.50 5.63 1 1 2 156.43 4.29 1 2 -1 145.88 5.85 1 2 -1 155.37 3.88 1 2 1 155.37 5.82 1 2 1 156.29 4.27 1 2 1 154.97 3.84 2 -1 -1 156.65 5.46 2 -1 -1 154.34 4.54 2 -1 1 151.66 5.40 2 -1 1 150.41 3.76 2 1 -1 149.24 6.01 2 1 -1 152.42 3.83 2 1 1 159.84 6.22 2 1 1 163.34 4.28 -2 -2 0 641.03 19.72 -2 -2 0 674.95 16.20 -2 0 2 671.02 22.77 -2 0 2 676.05 16.34 -2 0 2 645.81 18.66 -2 2 0 675.27 18.72 0 -2 -2 669.09 22.76 0 -2 -2 681.89 19.76 0 -2 -2 665.57 16.26 0 -2 2 635.05 22.70 0 -2 2 690.04 16.31 0 -2 2 693.54 18.67 0 2 -2 662.38 22.60 0 2 -2 685.48 19.77 0 2 -2 654.30 16.64 0 2 2 692.65 22.72 0 2 2 662.39 18.79 0 2 2 669.16 16.88 2 -2 0 707.58 22.73 2 -2 0 699.70 19.53 2 -2 0 677.09 16.53 2 0 -2 701.39 19.68 2 0 2 672.52 22.72 2 0 2 683.22 16.26 2 0 2 723.44 18.91 2 2 0 657.94 23.39 2 2 0 680.50 18.49 2 2 0 669.86 16.64 -2 -2 -1 342.77 12.35 -2 -2 -1 342.17 10.09 -2 -2 -1 344.48 8.18 -2 -2 1 338.98 8.15 -2 -1 -2 320.64 11.93 -2 -1 -2 343.24 9.99 -2 -1 2 328.01 11.99 -2 -1 2 343.77 8.21 -2 -1 2 333.02 9.37 -2 1 -2 338.09 11.57 -2 1 -2 347.15 9.88 -2 1 2 350.59 11.75 -2 1 2 346.95 8.21 -2 1 2 333.46 9.44 -2 2 -1 343.58 8.40 -2 2 1 356.63 11.57 -2 2 1 334.58 9.59 -2 2 1 346.20 8.34 -1 -2 -2 342.13 11.96 -1 -2 -2 336.90 9.96 -1 -2 -2 359.62 8.15 -1 -2 2 315.81 11.98 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449.18 10.95 2 -2 2 459.59 15.13 2 -2 2 464.62 10.96 2 2 -2 452.20 16.41 2 2 -2 423.64 11.23 2 2 2 465.00 16.13 2 2 2 453.56 12.66 2 2 2 462.46 11.39 -3 0 0 200.71 6.20 -3 0 0 210.64 5.07 0 -3 0 211.26 7.71 0 -3 0 210.03 6.22 0 -3 0 213.11 5.07 0 0 -3 198.57 7.39 0 0 -3 211.27 6.14 0 0 3 201.22 7.39 0 0 3 213.86 5.01 0 0 3 215.59 5.79 0 3 0 200.50 5.95 0 3 0 213.55 5.21 3 0 0 216.83 7.61 3 0 0 216.76 7.91 -3 0 -1 69.98 1.78 -3 0 -1 75.47 2.11 -3 0 1 66.47 3.11 -3 0 1 68.81 1.78 -3 0 1 64.36 2.34 -1 -3 0 73.22 3.54 -1 -3 0 71.37 2.37 -1 -3 0 73.71 1.76 -1 3 0 74.23 2.58 -1 3 0 72.10 2.27 -1 3 0 72.34 1.83 0 -1 -3 69.22 2.85 0 -1 -3 72.66 2.18 0 -1 3 70.66 2.82 0 -1 3 71.61 1.73 0 -1 3 73.39 2.01 0 1 -3 70.94 2.78 0 1 -3 71.23 2.15 0 1 -3 68.78 1.82 0 1 3 70.21 2.87 0 1 3 71.27 1.73 0 1 3 71.18 2.01 1 -3 0 67.06 2.81 1 -3 0 67.01 2.16 1 -3 0 70.96 1.81 1 3 0 73.61 3.09 1 3 0 65.13 2.05 1 3 0 69.40 1.84 3 0 -1 67.92 3.04 3 0 -1 65.19 2.22 0 3 1 72.18 2.06 0 3 1 75.45 1.83 1 0 -3 70.23 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4 2 -2 199.51 5.83 4 2 2 191.35 5.24 2 -2 -4 193.12 5.65 2 -2 4 192.74 4.58 2 -2 4 189.23 5.33 2 2 -4 183.96 5.72 -2 2 -4 191.23 5.51 -2 2 4 188.93 4.63 -2 2 4 185.56 5.32 -2 4 -2 185.98 5.56 -2 -2 4 186.48 5.22 -2 2 -4 194.25 6.70 -2 -2 4 186.80 4.58 -3 0 4 112.80 2.88 -3 0 4 114.19 3.32 -4 3 0 115.31 3.45 -4 -3 0 115.36 3.93 -4 -3 0 113.75 2.82 3 4 0 114.38 3.00 4 0 -3 112.14 3.62 4 0 3 112.79 3.34 -4 0 -3 107.88 3.54 0 3 -4 114.81 3.46 0 3 -4 110.00 3.02 0 3 4 115.67 3.30 0 3 4 116.62 2.88 3 -4 0 116.79 2.97 -4 0 -3 106.81 4.68 -3 -4 0 114.01 2.82 -3 4 0 121.45 3.48 -3 4 0 115.07 2.93 0 -3 -4 116.25 3.57 0 -3 -4 116.81 2.86 0 -3 4 103.76 4.56 0 -4 -3 116.36 3.58 0 -4 -3 120.45 2.86 0 -4 3 118.10 2.91 0 -4 3 115.84 3.24 0 4 -3 112.24 4.42 0 4 -3 109.22 4.59 0 4 -3 114.21 3.45 0 4 -3 115.31 3.04 0 4 3 114.27 3.31 3 0 -4 114.62 3.62 3 0 4 114.83 4.64 3 0 4 114.47 3.31 4 -3 0 118.94 2.97 4 3 0 114.69 3.00 -4 0 3 112.85 3.47 -3 -4 0 110.96 3.85 0 -3 4 115.52 2.86 0 -3 4 116.86 3.25 0 3 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88.86 2.83 2 -3 -4 89.59 2.32 4 2 3 92.05 2.61 -4 3 2 92.65 3.70 -4 3 2 90.21 3.00 -3 -2 -4 89.44 2.92 4 -2 -3 92.90 2.84 -3 2 4 87.53 2.35 -3 2 4 87.65 2.72 -2 -4 -3 88.40 2.99 -2 3 -4 92.16 2.45 -2 4 3 89.25 4.23 -2 4 3 89.21 2.77 3 4 2 90.02 2.39 2 -4 3 92.41 2.39 2 -4 3 88.18 2.81 2 4 -3 87.13 3.08 2 4 -3 87.81 2.47 3 -4 -2 82.88 3.62 3 -4 -2 90.38 2.75 3 -4 -2 89.68 2.36 3 -2 4 92.23 2.42 3 -2 4 89.20 2.72 3 2 -4 90.23 3.07 -4 -2 3 89.20 2.29 -2 -3 4 89.18 2.28 2 3 4 90.49 2.35 -4 -3 -2 91.04 3.08 4 -3 2 89.35 2.40 4 3 -2 86.23 3.00 4 3 -2 87.79 2.45 -3 4 -2 90.68 2.39 -3 -4 2 89.26 2.28 -4 -3 -3 49.19 1.88 -4 -3 3 49.13 1.36 -4 3 3 53.12 1.88 -3 -4 -3 51.03 1.90 -3 -4 3 50.38 1.37 -3 -3 -4 49.40 1.85 -3 -3 4 49.42 1.36 -3 3 4 49.76 1.70 -3 4 -3 51.73 1.48 -3 4 3 53.36 1.83 3 -4 -3 51.81 1.68 3 -4 -3 49.80 1.42 3 -4 3 50.53 1.48 3 -4 3 47.84 1.92 3 -3 -4 51.83 1.74 3 -3 -4 49.60 1.41 3 -3 4 47.91 1.45 3 -3 4 51.73 1.75 3 3 -4 49.22 2.04 3 3 4 50.19 1.54 3 3 4 49.31 1.42 3 4 -3 48.19 1.53 3 4 3 50.24 1.51 3 4 3 50.26 1.43 4 -3 -3 50.30 1.67 4 -3 -3 50.41 1.44 4 -3 3 45.91 1.46 4 -3 3 48.96 1.95 4 3 -3 51.34 2.08 4 3 -3 45.12 1.51 4 3 3 51.28 1.51 4 3 3 48.19 1.44 -4 -4 0 105.31 3.84 -4 -4 0 109.04 2.70 -4 0 -4 113.85 3.66 -4 0 4 108.07 2.79 -4 0 4 104.07 3.27 -4 4 0 110.87 3.29 0 -4 -4 109.88 3.45 0 -4 4 106.03 2.77 0 -4 4 110.03 3.11 0 4 -4 107.58 2.93 0 4 4 108.14 3.18 0 4 4 111.36 2.78 4 -4 0 110.73 2.86 4 0 -4 113.30 3.54 4 0 4 103.87 4.56 4 0 4 101.90 3.19 4 4 0 111.64 2.92 -4 -4 -1 98.22 3.27 -4 -4 -1 89.52 2.27 -4 -4 1 88.68 3.40 -4 -4 1 90.55 2.31 -4 -1 -4 88.91 2.98 -4 -1 4 89.83 2.37 -4 -1 4 87.65 2.76 -4 1 4 91.03 2.40 -4 1 4 91.12 2.86 -4 4 -1 95.43 2.88 -4 4 -1 94.84 2.42 -4 4 1 91.67 2.96 -1 -4 -4 91.85 3.01 -1 -4 4 85.37 4.35 -1 -4 4 93.13 2.36 -1 4 -4 92.24 2.52 -1 4 4 91.24 2.75 1 -4 -4 87.16 2.91 1 -4 -4 90.39 2.34 1 -4 4 94.02 2.42 1 4 -4 90.62 2.54 1 4 4 94.55 2.70 1 4 4 89.39 2.37 4 -4 -1 90.07 2.43 4 -4 1 89.03 2.46 4 -1 -4 93.42 3.00 4 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44.91 1.48 4 -3 -4 50.00 1.72 4 -3 -4 49.63 1.45 4 -3 4 47.39 1.49 4 -3 4 48.92 1.85 4 3 4 49.47 1.53 4 3 4 48.57 1.44 4 4 -3 46.37 1.54 4 4 3 49.24 1.45 -4 -4 -4 38.63 1.61 -4 -4 4 36.17 1.09 -4 4 4 37.84 1.53 4 -4 -4 37.27 1.36 4 -4 -4 37.25 1.16 4 -4 4 33.88 1.20 4 -4 4 33.64 1.60 4 4 4 36.10 1.17 -5 0 0 56.04 1.82 -5 0 0 51.19 1.44 0 -5 0 51.90 2.83 0 -5 0 54.89 1.84 0 -5 0 50.20 1.43 0 0 -5 51.92 1.76 0 0 5 52.38 1.59 0 5 0 54.83 2.41 0 5 0 48.72 1.71 0 5 0 50.24 1.48 5 0 0 53.14 2.60 5 0 0 54.42 2.98 -5 0 -1 31.62 1.19 -5 0 1 28.64 0.93 -5 0 1 27.86 1.10 -1 -5 0 29.64 0.89 -1 5 0 30.84 1.17 -1 5 0 30.63 0.95 0 -1 -5 30.81 1.16 0 -1 5 31.31 0.84 0 -1 5 29.78 0.99 0 1 -5 29.14 1.11 0 1 5 31.09 1.01 1 -5 0 31.14 0.96 1 5 0 29.67 1.79 1 5 0 30.46 0.98 5 0 -1 31.18 2.15 5 0 -1 30.63 1.14 5 0 1 32.01 1.88 5 0 1 29.52 2.74 5 -1 0 34.84 2.21 5 -1 0 29.90 1.07 5 -1 0 29.66 0.93 5 1 0 31.55 0.93 0 -5 -1 30.71 0.92 0 -5 1 29.12 1.25 0 -5 1 30.39 0.93 0 5 -1 33.74 1.91 0 5 -1 30.22 0.98 0 5 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16.64 0.60 -5 1 -1 19.57 0.92 -5 1 -1 17.57 0.72 0 5 2 50.02 1.63 0 5 2 48.67 1.38 0 5 -2 49.76 1.46 0 -5 -2 49.70 1.33 0 -5 2 48.91 1.38 5 -2 0 46.99 1.39 5 2 0 49.56 1.40 -2 -5 0 52.31 1.91 -2 -5 0 48.91 1.32 0 2 -5 47.83 1.44 2 -5 0 48.97 1.45 2 5 0 48.90 1.45 5 0 -2 51.01 1.75 5 0 2 44.30 2.53 5 0 2 46.22 1.61 -2 0 5 49.11 1.53 0 -5 -2 49.05 1.79 -2 5 0 48.59 1.66 -2 5 0 50.10 1.39 0 -2 -5 48.32 1.70 0 -2 5 48.47 1.28 0 -2 5 48.09 1.49 0 2 -5 47.66 1.62 -5 -2 0 48.05 1.87 -5 -2 0 47.88 1.31 -5 2 0 53.01 1.71 -2 0 -5 47.86 1.63 -2 0 5 48.06 1.32 -5 0 2 48.10 1.37 2 0 -5 48.55 1.74 2 0 5 48.28 1.53 -5 0 -2 47.14 1.70 -1 5 -2 34.04 1.08 -2 5 1 35.19 1.43 -1 -2 -5 34.12 1.30 1 -5 -2 31.63 2.10 -2 -1 5 33.96 1.10 -2 1 -5 34.46 1.92 -2 1 -5 34.37 1.25 -2 -1 5 31.46 0.95 5 -1 2 33.27 1.02 5 -1 2 31.55 1.28 -5 -1 -2 33.26 1.35 5 2 1 34.12 1.08 -5 -2 1 34.97 1.44 -5 -2 1 33.71 0.97 -5 2 -1 34.50 1.35 -5 1 2 34.02 1.05 -5 1 2 33.95 1.40 -1 -5 2 32.81 1.00 -1 5 -2 32.49 1.20 1 5 2 35.37 1.05 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3 7 -2 10.47 0.68 -2 7 -3 12.16 0.68 -2 -3 -7 10.66 0.83 3 2 7 11.57 0.67 -2 3 7 11.79 0.74 7 3 2 12.01 0.64 -7 -3 2 12.75 0.63 -3 7 2 10.21 0.86 2 -3 -7 11.39 0.84 3 -2 7 10.03 0.68 -2 7 3 11.40 0.97 -2 -3 7 11.23 0.56 3 7 2 12.26 0.72 -3 7 -2 12.93 0.68 2 -7 3 10.28 0.66 -7 3 2 10.94 0.71 2 3 7 11.65 0.67 3 -7 -2 12.41 0.70 -2 -7 -3 11.92 0.96 -7 -2 3 11.83 0.64 7 -2 -3 12.32 0.63 3 2 -7 10.27 0.94 -7 -3 -2 12.44 1.04 -3 2 7 11.59 0.74 7 2 3 11.47 0.59 2 7 -3 11.43 0.69 -3 -2 -7 10.84 0.77 -3 3 7 10.75 0.76 3 3 7 10.02 0.57 3 7 -3 10.38 0.71 3 7 3 12.17 0.72 7 -3 -3 12.04 0.67 -3 -3 7 9.32 0.56 3 -3 -7 11.35 0.87 7 3 3 10.83 0.61 -7 -3 -3 9.70 0.95 7 3 -3 12.11 0.92 -3 7 -3 9.69 0.63 -3 7 3 9.72 0.92 3 3 -7 9.30 0.91 3 3 7 10.45 0.66 3 -7 -3 10.65 0.66 3 -7 3 9.65 0.67 -7 -3 3 10.93 0.64 -7 3 3 9.15 0.76 -3 -7 -3 12.14 1.07 -3 -3 -7 9.19 0.83 3 -3 7 10.36 0.77 0 7 -4 12.20 0.75 7 0 -4 10.64 0.80 4 0 7 10.81 0.69 7 -4 0 12.81 0.69 7 4 0 12.70 0.71 0 -7 -4 11.86 0.92 0 -7 4 10.64 0.64 -7 -4 0 13.46 1.17 -7 0 4 13.12 0.73 0 -4 -7 11.41 0.87 0 4 -7 10.13 0.80 0 4 7 10.99 0.70 4 -7 0 13.38 0.78 4 7 0 11.85 0.77 -4 0 7 10.71 0.64 7 0 4 11.51 0.78 4 0 -7 11.65 0.99 7 1 -4 12.08 0.89 -1 7 -4 11.57 0.71 7 -1 4 10.06 0.77 4 -7 1 11.01 0.72 -1 -7 4 9.63 0.61 4 -1 -7 10.81 0.91 -4 -7 -1 13.77 1.15 -4 7 1 10.73 0.70 7 -4 -1 12.71 0.68 4 7 -1 12.19 0.79 -4 -1 7 10.68 0.61 -1 -4 -7 11.49 0.90 -7 1 4 11.93 0.71 -1 4 7 11.33 0.74 4 7 1 12.69 0.79 1 4 7 11.78 0.71 4 -7 -1 11.63 0.76 -4 1 7 12.47 0.81 -1 -7 -4 10.70 0.92 1 7 -4 11.11 0.73 4 1 -7 10.07 0.99 -1 7 4 10.85 0.90 1 -7 4 9.78 0.64 -7 -1 4 11.16 0.68 -1 -4 7 10.31 0.57 4 -1 7 9.75 0.69 -4 -7 1 10.26 0.56 -4 7 -1 11.90 0.76 -4 7 -1 12.27 0.64 1 -4 -7 11.91 0.87 -4 1 7 11.06 0.67 7 -1 -4 12.21 0.82 7 1 4 10.15 0.68 -7 -4 -1 10.37 1.06 7 -4 1 10.90 0.68 4 2 7 10.59 0.68 7 2 -4 10.09 0.87 7 -2 4 9.83 0.86 4 7 -2 11.08 0.76 -7 4 -2 12.44 0.94 4 -2 -7 11.38 0.93 4 -7 2 10.85 0.75 -2 -7 4 9.82 0.63 -7 2 4 9.43 0.82 -4 -7 -2 11.54 1.04 7 -4 -2 10.66 0.64 -7 -4 2 11.39 0.62 2 7 4 10.99 0.64 -4 7 2 10.25 0.81 -2 -4 -7 10.15 0.89 -4 -2 7 10.43 0.62 -2 4 7 11.88 0.80 7 4 2 10.78 0.66 2 -4 7 9.40 0.71 -2 7 -4 10.34 0.70 2 -4 -7 9.59 0.78 -7 -4 -2 8.85 0.97 4 7 2 10.98 0.73 -7 4 2 9.98 0.70 -4 -2 -7 10.72 0.87 -2 -4 7 10.85 0.58 -4 2 7 11.31 0.82 -2 -7 -4 11.72 1.00 -7 -2 4 9.84 0.64 2 4 7 10.11 0.67 -2 7 4 10.89 0.93 2 -7 4 9.28 0.62 2 7 -4 9.11 0.68 -4 7 -2 11.90 0.66 7 -2 -4 10.43 0.58 4 -2 7 9.70 0.73 4 2 -7 9.11 1.00 7 2 4 10.83 0.59 -4 -7 2 9.85 0.57 7 -4 2 10.12 0.69 4 -7 -2 11.06 0.69 0 -8 0 35.18 1.18 0 0 -8 34.02 1.48 0 0 8 34.74 1.31 0 8 0 34.96 1.23 8 0 0 36.68 1.15 -1 -8 0 30.35 1.05 -1 8 0 30.50 1.09 0 -1 -8 30.04 1.40 0 -1 8 30.40 1.19 0 1 -8 30.24 1.34 0 1 8 30.53 1.19 1 -8 0 31.19 1.11 1 8 0 30.91 1.14 0 8 1 31.53 1.12 1 0 -8 29.91 1.41 1 0 8 30.06 1.19 8 1 0 31.58 1.27 0 -8 -1 30.92 1.05 0 -8 1 30.44 1.09 0 8 -1 30.62 1.13 -1 0 8 29.97 1.19 -1 0 -8 29.11 1.33 -8 1 0 33.64 1.34 -1 -1 8 26.57 1.10 8 -1 -1 29.69 1.00 1 1 8 26.93 1.10 1 8 -1 27.43 1.07 1 8 1 28.00 1.06 8 -1 1 29.96 1.16 8 1 -1 27.86 1.17 1 -1 -8 27.01 1.32 1 -1 8 26.60 1.11 1 1 -8 25.99 1.29 -8 -1 1 27.24 1.00 -1 -8 -1 27.47 0.96 -1 -8 1 26.28 0.96 -1 -1 -8 26.52 1.27 1 -8 -1 26.77 0.99 -1 1 8 26.06 1.10 -1 8 -1 28.11 1.04 -1 8 1 27.28 1.00 1 -8 1 27.53 1.06 8 0 2 24.53 1.05 -2 8 0 25.66 0.94 0 -2 -8 23.42 1.25 0 -2 8 23.79 1.04 0 2 8 24.23 1.06 2 -8 0 25.51 1.01 2 8 0 23.92 1.01 8 0 -2 26.99 1.16 -8 0 2 24.73 0.98 -2 -8 0 24.21 0.89 0 8 2 25.02 0.94 2 0 -8 24.06 1.32 2 0 8 24.79 1.06 8 -2 0 27.05 0.94 8 2 0 25.23 1.13 0 8 -2 24.85 1.02 -2 0 -8 22.70 1.19 -2 0 8 24.14 1.06 0 -8 2 23.47 0.97 2 -8 1 24.36 0.99 2 8 -1 22.90 1.00 -1 8 -2 22.20 0.96 2 1 8 21.68 0.99 8 -1 2 24.47 1.08 8 1 -2 24.12 1.12 8 2 1 23.91 0.91 -1 -2 -8 22.71 1.19 1 -2 8 22.87 1.03 1 2 -8 22.58 1.18 -8 -2 1 22.07 1.04 8 -2 -1 24.49 0.91 1 8 2 23.86 0.95 2 -1 -8 20.71 1.20 1 -8 -2 24.05 0.93 -1 -8 2 21.23 0.87 -1 2 8 21.82 1.02 1 2 8 22.40 1.00 -8 -2 -1 24.31 1.26 -8 2 1 23.09 1.02 -2 -1 -8 21.94 1.12 -2 1 8 22.15 1.03 2 -8 -1 23.01 0.97 2 8 1 23.62 1.01 -2 8 -1 23.10 0.93 1 -8 2 22.63 0.93 1 8 -2 23.09 0.99 -8 -1 2 23.78 0.94 -2 -8 1 22.35 0.87 2 -1 8 21.78 1.01 8 -1 -2 23.63 0.88 1 -2 -8 21.69 1.22 8 2 -1 22.63 1.10 8 1 2 22.52 0.87 0 0 0 0.00 0.00 ; _shelx_hkl_checksum 2759 loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' '-x, y, -z' 'x, -y, -z' 'z, x, y' 'z, -x, -y' '-z, -x, y' '-z, x, -y' 'y, z, x' '-y, z, -x' 'y, -z, -x' '-y, -z, x' 'y, x, -z' '-y, -x, -z' 'y, -x, z' '-y, x, z' 'x, z, -y' '-x, z, y' '-x, -z, -y' 'x, -z, y' 'z, y, -x' 'z, -y, x' '-z, y, x' '-z, -y, -x' '-x, -y, -z' 'x, y, -z' 'x, -y, z' '-x, y, z' '-z, -x, -y' '-z, x, y' 'z, x, -y' 'z, -x, y' '-y, -z, -x' 'y, -z, x' '-y, z, x' 'y, z, -x' '-y, -x, z' 'y, x, z' '-y, x, -z' 'y, -x, -z' '-x, -z, y' 'x, -z, -y' 'x, z, y' '-x, z, -y' '-z, -y, x' '-z, y, -x' 'z, -y, -x' 'z, y, x' 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 0.500000 0.500000 0.500000 0.02580(6) Uani 1 48 d S T P . . Br2 Br 0.500000 0.500000 0.000000 0.0979(4) Uani 1 16 d S T P . . N1 N -0.066(18) 0.112(16) 0.030(17) 0.039(8) Uani 0.0208 1 d G . P A -1 H1A H -0.101755 0.185651 -0.096604 0.059 Uiso 0.0208 1 d G U P A -1 H1B H 0.023687 0.198059 0.114166 0.059 Uiso 0.0208 1 d G U P A -1 H1C H -0.191313 0.079793 0.106001 0.059 Uiso 0.0208 1 d G U P A -1 C2 C 0.05(2) -0.098(16) -0.03(2) 0.039(8) Uani 0.0208 1 d G . P A -1 H2A H 0.093666 -0.175560 0.107752 0.059 Uiso 0.0208 1 d G U P A -1 H2B H 0.184713 -0.063406 -0.114231 0.059 Uiso 0.0208 1 d G U P A -1 H2C H -0.046672 -0.192563 -0.116344 0.059 Uiso 0.0208 1 d G U P A -1 CENT He 0.000000 0.000000 0.000000 0.020 Uiso 0 1 d S U P B -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 Pb1 0.02580(6) 0.02580(6) 0.02580(6) 0.000 0.000 0.000 Br2 0.1358(5) 0.1358(5) 0.0220(2) 0.000 0.000 0.000 N1 0.052(16) 0.052(11) 0.013(11) -0.008(10) -0.006(6) 0.010(8) C2 0.052(16) 0.052(11) 0.013(11) -0.008(10) -0.006(6) 0.010(8) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' C C 0.0033 0.0016 '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' Pb Pb -3.3944 10.1111 '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' He He 0.0000 0.0000 '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 Br2 Pb1 Br2 90.0 9_565 . ? Br2 Pb1 Br2 90.0 9_565 1_556 ? Br2 Pb1 Br2 180.0 . 1_556 ? Br2 Pb1 Br2 90.0 9_565 5 ? Br2 Pb1 Br2 90.0 . 5 ? Br2 Pb1 Br2 90.0 1_556 5 ? Br2 Pb1 Br2 90.0 9_565 5_655 ? Br2 Pb1 Br2 90.0 . 5_655 ? Br2 Pb1 Br2 90.0 1_556 5_655 ? Br2 Pb1 Br2 180.0 5 5_655 ? Br2 Pb1 Br2 180.0 9_565 9 ? Br2 Pb1 Br2 90.0 . 9 ? Br2 Pb1 Br2 90.0 1_556 9 ? Br2 Pb1 Br2 90.0 5 9 ? Br2 Pb1 Br2 90.0 5_655 9 ? Pb1 Br2 Pb1 180.0 1_554 . ? C2 N1 H1A 109.4 . . ? C2 N1 H1B 109.5 . . ? H1A N1 H1B 109.5 . . ? C2 N1 H1C 109.5 . . ? H1A N1 H1C 109.5 . . ? H1B N1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? 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 Pb1 Br2 2.95875(15) 9_565 ? Pb1 Br2 2.95875(15) . ? Pb1 Br2 2.95875(15) 1_556 ? Pb1 Br2 2.95875(15) 5 ? Pb1 Br2 2.95875(15) 5_655 ? Pb1 Br2 2.95875(15) 9 ? N1 C2 1.4644 . ? N1 H1A 0.8897 . ? N1 H1B 0.8900 . ? N1 H1C 0.8893 . ? C2 H2A 0.9597 . ? C2 H2B 0.9598 . ? C2 H2C 0.9607 . ?