#------------------------------------------------------------------------------ #$Date: 2021-07-23 05:43:59 +0300 (Fri, 23 Jul 2021) $ #$Revision: 267714 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/70/78/7707874.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_7707874 loop_ _publ_author_name 'Ingham, Aidan' 'Kostelnik, Tom Kostelnik' 'McNeil, Brooke' 'Patrick, Brian O.' 'Choudhary, Neha' 'Jaraquemada-Pel\'aez, Mar\'ia de Guadalupe' 'Orvig, Chris' _publ_section_title ; Getting a Lead on Pb2+ - Amide Chelators for 203/212Pb Radiopharmaceuticals ; _journal_name_full 'Dalton Transactions' _journal_paper_doi 10.1039/D1DT01653A _journal_year 2021 _chemical_formula_moiety 'C24 H34 N8 O6 Pb, 2(N O3), 2.085(H2 O), 0.582(O)' _chemical_formula_sum 'C24 H38.58 N10 O14.67 Pb' _chemical_formula_weight 909.10 _space_group_crystal_system monoclinic _space_group_IT_number 15 _space_group_name_Hall '-C 2yc' _space_group_name_H-M_alt 'C 1 2/c 1' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary dual _audit_block_doi 10.5517/ccdc.csd.cc27z4bq _audit_creation_date 2021-02-23 _audit_creation_method ; Olex2 1.3 (compiled 2020.11.12 svn.r5f609507 for OlexSys, GUI svn.r6272) ; _audit_update_record ; 2021-05-19 deposited with the CCDC. 2021-07-21 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 123.133(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 14.0872(7) _cell_length_b 22.5964(10) _cell_length_c 12.3531(9) _cell_measurement_reflns_used 9967 _cell_measurement_temperature 115(2) _cell_measurement_theta_max 30.59 _cell_measurement_theta_min 2.67 _cell_volume 3292.9(3) _computing_cell_refinement 'SAINT V8.40B (Bruker, 2016)' _computing_data_reduction 'SAINT V8.40B (Bruker, 2016)' _computing_molecular_graphics 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 1.3 (Dolomanov et al., 2009)' _computing_structure_refinement 'XL (Sheldrick, 2008)' _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' _diffrn_ambient_temperature 115(2) _diffrn_detector 'Bruker APEX2 area detector' _diffrn_detector_area_resol_mean 7.9 _diffrn_detector_type 'CCD area detector' _diffrn_measured_fraction_theta_full 1.000 _diffrn_measured_fraction_theta_max 0.991 _diffrn_measurement_device 'Bruker-Nonius Kappa diffractometer' _diffrn_measurement_device_type 'Bruker APEX II area detector' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0615 _diffrn_reflns_av_unetI/netI 0.0551 _diffrn_reflns_Laue_measured_fraction_full 1.000 _diffrn_reflns_Laue_measured_fraction_max 0.991 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_k_max 32 _diffrn_reflns_limit_k_min -31 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_number 19580 _diffrn_reflns_point_group_measured_fraction_full 1.000 _diffrn_reflns_point_group_measured_fraction_max 0.991 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.705 _diffrn_reflns_theta_min 1.802 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_current 0.99 _diffrn_source_power 0.0495 _diffrn_source_type 'Incoatec I\ms' _diffrn_source_voltage 50.0 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 5.208 _exptl_absorpt_correction_T_max 0.695 _exptl_absorpt_correction_T_min 0.358 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; SADABS-2016/2 (Bruker, 2016/2) was used for absorption correction. wR2(int) was 0.1339 before and 0.0768 after correction. The ratio of minimum to maximum transmission is 0.5157. The \l/2 correction factor is not present. ; _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.834 _exptl_crystal_description irregular _exptl_crystal_F_000 1808 _exptl_crystal_recrystallization_method 'The material was recrystallised from water by slow evaporation' _exptl_crystal_size_max 0.187 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.07 _refine_diff_density_max 1.568 _refine_diff_density_min -2.072 _refine_diff_density_rms 0.138 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_hydrogen_treatment mixed _refine_ls_matrix_type full _refine_ls_number_parameters 333 _refine_ls_number_reflns 5069 _refine_ls_number_restraints 139 _refine_ls_restrained_S_all 1.014 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0319 _refine_ls_shift/su_max 0.004 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0334P)^2^] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0710 _refine_ls_wR_factor_ref 0.0742 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4486 _reflns_number_total 5069 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file d1dt01653a2.cif _cod_data_source_block co583 _cod_database_code 7707874 _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. ; _shelx_estimated_absorpt_t_max 0.712 _shelx_estimated_absorpt_t_min 0.443 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups At 1.5 times of: All N(H,H) groups, All O(H,H) groups 2. Restrained distances N5-O4 = N5-O6 1.25 with sigma of 0.02 N5-O5 1.24 with sigma of 0.02 N5A-O6A = N5A-O4A 1.25 with sigma of 0.02 N5A-O5A 1.24 with sigma of 0.02 N5B-O4B = N5B-O5B 1.25 with sigma of 0.02 N5B-O6B 1.24 with sigma of 0.02 N5-O4 \\sim N5-O5 \\sim N5-O6 with sigma of 0.02 O6A-O5A \\sim O5A-O4A \\sim O4A-O6A with sigma of 0.04 O4-O5 \\sim O5-O6 \\sim O6-O4 with sigma of 0.04 N5A-O6A \\sim N5A-O5A \\sim N5A-O4A with sigma of 0.02 O4B-O6B \\sim O6B-O5B \\sim O5B-O4B with sigma of 0.04 N5B-O4B \\sim N5B-O6B \\sim N5B-O5B with sigma of 0.02 3. Restrained planarity O4, O6, O5, N5 with sigma of 0.1 O6A, O4A, O5A, N5A with sigma of 0.1 N5B, O4B, O6B, O5B with sigma of 0.1 4. Uiso/Uaniso restraints and constraints O4 \\sim O6 \\sim O5 \\sim N5: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A O6A \\sim O4A \\sim O5A \\sim N5A: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A N5B \\sim O4B \\sim O6B \\sim O5B: within 2A with sigma of 0.04 and sigma for terminal atoms of 0.08 within 2A Uanis(O6) = Uanis(O6B) 5. Rigid body (RIGU) restrains O4, O6, O5, N5 with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 O6A, O4A, O5A, N5A with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 N5B, O4B, O6B, O5B with sigma for 1-2 distances of 0.004 and sigma for 1-3 distances of 0.004 6. Others 1*[Sof(O4)+Sof(O6)+Sof(O5)+Sof(N5)]+1*[Sof(N5B)+Sof(O4B)+Sof(O6B)+Sof(O5B)]+1* [Sof(O6A)+Sof(O4A)+Sof(O5A)+Sof(N5A)]=1 with esd of 0.005 Sof(O4)=Sof(O6)=Sof(O5)=Sof(N5)=FVAR(1) Sof(N5B)=Sof(O4B)=Sof(O6B)=Sof(O5B)=FVAR(2) Sof(O6A)=Sof(O4A)=Sof(O5A)=Sof(N5A)=FVAR(3) Sof(O7)=Sof(H7A)=Sof(H7B)=FVAR(4) Sof(O9)=Sof(H9A)=Sof(H9B)=FVAR(5) 7.a Free rotating group: O7(H7A,H7B), O9(H9A,H9B) 7.b Secondary CH2 refined with riding coordinates: C2(H2A,H2B), C3(H3A,H3B), C10(H10A,H10B), C11(H11A,H11B), C12(H12A,H12B) 7.c Aromatic/amide H refined with riding coordinates: C5(H5), C6(H6), C7(H7) ; _shelx_res_file ; TITL co583_a.res in C2/c co583.res created by SHELXL-2018/3 at 13:23:07 on 23-Feb-2021 REM Old TITL co583 in Cc REM SHELXT solution in C2/c: R1 0.067, Rweak 0.008, Alpha 0.026 REM 0.170 for 91 systematic absences, Orientation as input REM Formula found by SHELXT: C30 N8 O5A Pb CELL 0.71073 14.0872 22.5964 12.3531 90 123.133 90 ZERR 4 0.0007 0.001 0.0009 0 0.002 0 LATT 7 SYMM -X,+Y,0.5-Z SFAC C H N O Pb UNIT 96 154.32 40 58.67 4 EQIV $1 1-X,1-Y,2-Z EQIV $2 -X,+Y,1.5-Z EQIV $3 -X,+Y,0.5-Z EQIV $4 0.5-X,0.5-Y,1-Z EQIV $5 -0.5-X,0.5-Y,1-Z DFIX 1.25 N5 O4 N5 O6 FLAT O4 O6 O5 N5 RIGU O4 > N5 DFIX 1.24 N5 O5 SIMU O4 > N5 SADI N5 O4 N5 O5 N5 O6 DFIX 1.25 N5A O6A N5A O4A SADI 0.04 O6A O5A O5A O4A O4A O6A SADI 0.04 O4 O5 O5 O6 O6 O4 DFIX 1.24 N5A O5A FLAT O6A O4A O5A N5A SIMU O6A > N5A RIGU O6A > N5A SADI N5A O6A N5A O5A N5A O4A FLAT N5B O4B O6B O5B DFIX 1.25 N5B O4B N5B O5B SIMU N5B O4B O6B O5B RIGU N5B O4B O6B O5B DFIX 1.24 N5B O6B SADI 0.04 O4B O6B O6B O5B O5B O4B SADI N5B O4B N5B O6B N5B O5B EADP O6 O6B SUMP 1 0.005 1 2 1 3 1 4 L.S. 20 PLAN 20 SIZE 0.07 0.15 0.187 TEMP -158(2) CONF HTAB N1 O1_$1 HTAB N1 O6_$2 HTAB N4 O7_$3 HTAB N4 O9_$4 HTAB O7 O7_$5 DAMP BOND list 4 MORE -1 BOND $H fmap 2 acta REM REM REM WGHT 0.033400 FVAR 0.19235 0.45116 0.28313 0.26581 0.66147 0.38115 PB1 5 0.500000 0.367529 0.750000 10.50000 0.02226 0.01674 = 0.02387 0.00000 0.01306 0.00000 O1 4 0.439473 0.457189 0.849201 11.00000 0.02236 0.02377 = 0.03436 -0.00599 0.01593 -0.00219 O2 4 0.508924 0.325838 0.550891 11.00000 0.03433 0.02968 = 0.03039 0.00317 0.02097 0.00311 O3 4 0.381281 0.267054 0.690004 11.00000 0.03801 0.01816 = 0.03203 -0.00135 0.02139 -0.00490 N1 3 0.382502 0.457082 0.986851 11.00000 0.02613 0.03509 = 0.03560 -0.01433 0.01848 -0.00789 H1A 2 0.432917 0.479635 1.038301 11.00000 -1.50000 H1B 2 0.340074 0.447897 0.999427 11.00000 -1.50000 N2 3 0.275332 0.380043 0.680226 11.00000 0.02035 0.02531 = 0.02772 -0.00466 0.01275 -0.00442 N3 3 0.325705 0.387287 0.496398 11.00000 0.02175 0.02547 = 0.02601 -0.00081 0.01230 -0.00486 N4 3 0.448806 0.318181 0.342071 11.00000 0.05145 0.07297 = 0.04048 0.00671 0.03481 0.00980 H4A 2 0.507756 0.292014 0.366603 11.00000 -1.50000 H4B 2 0.391337 0.326260 0.260955 11.00000 -1.50000 C1 1 0.373575 0.440282 0.879561 11.00000 0.01892 0.02146 = 0.03382 -0.00249 0.01451 0.00316 C2 1 0.278153 0.397079 0.796641 11.00000 0.01988 0.03171 = 0.03246 -0.00838 0.01554 -0.00555 AFIX 23 H2A 2 0.288218 0.361221 0.847948 11.00000 -1.20000 H2B 2 0.204886 0.415454 0.770914 11.00000 -1.20000 AFIX 0 C3 1 0.220719 0.427042 0.582767 11.00000 0.02136 0.03342 = 0.03183 0.00000 0.01311 0.00111 AFIX 23 H3A 2 0.252720 0.465767 0.624421 11.00000 -1.20000 H3B 2 0.138618 0.427563 0.548171 11.00000 -1.20000 AFIX 0 C4 1 0.236634 0.418890 0.472996 11.00000 0.01949 0.02583 = 0.02981 -0.00046 0.01009 -0.00424 C5 1 0.162890 0.445565 0.352860 11.00000 0.02456 0.03184 = 0.03319 0.00087 0.00844 -0.00269 AFIX 43 H5 2 0.099293 0.467704 0.337421 11.00000 -1.20000 AFIX 0 C6 1 0.184600 0.438993 0.257843 11.00000 0.03451 0.03460 = 0.02960 0.00731 0.01037 -0.00629 AFIX 43 H6 2 0.136832 0.457583 0.176328 11.00000 -1.20000 AFIX 0 C7 1 0.275414 0.405535 0.280371 11.00000 0.03412 0.03999 = 0.02821 0.00545 0.01494 -0.00816 AFIX 43 H7 2 0.291073 0.400445 0.215273 11.00000 -1.20000 AFIX 0 C8 1 0.343292 0.379503 0.400965 11.00000 0.02596 0.02929 = 0.02423 0.00014 0.01222 -0.00899 C9 1 0.440672 0.339213 0.436524 11.00000 0.03559 0.03359 = 0.03244 0.00033 0.02480 -0.00624 C10 1 0.214633 0.323075 0.627474 11.00000 0.02629 0.03189 = 0.03383 -0.00883 0.01677 -0.01092 AFIX 23 H10A 2 0.191086 0.319489 0.536154 11.00000 -1.20000 H10B 2 0.145188 0.323298 0.629182 11.00000 -1.20000 AFIX 0 C11 1 0.284963 0.270397 0.701032 11.00000 0.04209 0.02784 = 0.03833 -0.00852 0.02695 -0.01410 AFIX 23 H11A 2 0.310853 0.273945 0.793125 11.00000 -1.20000 H11B 2 0.239030 0.233904 0.665885 11.00000 -1.20000 AFIX 0 C12 1 0.450450 0.217388 0.758006 11.00000 0.05490 0.01514 = 0.03353 0.00009 0.02564 -0.00350 AFIX 23 H12A 2 0.406325 0.180366 0.722690 11.00000 -1.20000 H12B 2 0.478049 0.220072 0.850734 11.00000 -1.20000 AFIX 0 PART 2 O6A 4 -0.277347 0.315928 0.451546 41.00000 0.05608 0.13757 = 0.06646 -0.06800 0.04556 -0.03063 O4A 4 -0.089270 0.317690 0.577839 41.00000 0.04773 0.05110 = 0.11353 -0.01172 0.01218 -0.00476 O5A 4 -0.186992 0.397140 0.503465 41.00000 0.06653 0.06753 = 0.02195 -0.00327 0.02159 0.01352 N5A 3 -0.183818 0.342145 0.509490 41.00000 0.04367 0.06160 = 0.04162 -0.01320 0.02682 -0.00175 PART 1 O4 4 -0.027883 0.372510 0.568454 21.00000 0.06637 0.03709 = 0.24357 0.02739 0.09247 0.02406 O6 4 -0.178083 0.417066 0.528827 21.00000 0.03327 0.09515 = 0.01769 -0.00422 0.01301 0.01923 O5 4 -0.026478 0.465950 0.578066 21.00000 0.09905 0.04793 = 0.11475 -0.01789 0.07461 -0.00940 N5 3 -0.077295 0.418757 0.561292 21.00000 0.04595 0.04093 = 0.07374 -0.00084 0.03248 0.01297 PART 3 AFIX 6 O7 4 -0.282706 0.302354 0.436934 51.00000 0.07085 0.06271 = 0.06125 -0.01062 0.03118 0.01156 H7A 2 -0.244490 0.283446 0.507707 51.00000 -1.50000 H7B 2 -0.262817 0.338215 0.457645 51.00000 -1.50000 AFIX 6 PART -1 O9 4 -0.063786 0.281104 0.672513 61.00000 0.09964 0.07747 = 0.20305 0.07873 0.11280 0.04267 H9A 2 -0.126728 0.263635 0.623634 61.00000 -1.50000 H9B 2 -0.071369 0.314100 0.635492 61.00000 -1.50000 AFIX 0 PART 4 O8 4 -0.171060 0.260149 0.568406 0.16228 0.06443 0.04487 = 0.04938 0.02438 0.04785 0.03702 PART 7 O10 4 0.000000 0.438104 0.750000 0.12883 0.08513 PART 3 N5B 3 -0.082306 0.405809 0.573450 31.00000 0.03714 0.05912 = 0.07282 -0.00614 0.01482 0.01633 O4B 4 -0.075472 0.350697 0.570993 31.00000 0.03417 0.06263 = 0.08520 -0.02909 0.00597 0.00385 O6B 4 -0.177966 0.429272 0.504193 31.00000 0.03327 0.09515 = 0.01769 -0.00422 0.01301 0.01923 O5B 4 0.002897 0.437704 0.643047 31.00000 0.02729 0.07241 = 0.11184 -0.00214 0.01886 0.00988 HKLF 4 REM co583_a.res in C2/c REM wR2 = 0.074216, GooF = S = 1.02263, Restrained GooF = 1.01355 for all data REM R1 = 0.031886 for 4486 Fo > 4sig(Fo) and 0.038843 for all 5069 data REM 333 parameters refined using 139 restraints END WGHT 0.0334 0.0000 REM Highest difference peak 1.568, deepest hole -2.072, 1-sigma level 0.138 Q1 1 0.0000 0.3974 0.7500 10.50000 0.05 1.57 Q2 1 0.4364 0.3738 0.7060 11.00000 0.05 1.55 Q3 1 0.5029 0.3757 0.8131 11.00000 0.05 1.52 Q4 1 0.4605 0.3682 0.6355 11.00000 0.05 0.96 Q5 1 0.4226 0.3427 0.7359 11.00000 0.05 0.86 Q6 1 0.3923 0.3533 0.4141 11.00000 0.05 0.69 Q7 1 0.5000 0.4093 0.7500 10.50000 0.05 0.66 Q8 1 -0.2307 0.3678 0.4611 11.00000 0.05 0.64 Q9 1 0.3924 0.3752 0.6408 11.00000 0.05 0.55 Q10 1 0.4199 0.3935 0.7372 11.00000 0.05 0.54 Q11 1 0.2237 0.4270 0.5193 11.00000 0.05 0.54 Q12 1 -0.0006 0.3877 0.6762 11.00000 0.05 0.53 Q13 1 0.4731 0.3290 0.7413 11.00000 0.05 0.52 Q14 1 0.5114 0.3669 0.6175 11.00000 0.05 0.52 Q15 1 0.4783 0.4038 0.8604 11.00000 0.05 0.51 Q16 1 0.4425 0.3227 0.4831 11.00000 0.05 0.51 Q17 1 0.4486 0.4104 0.7621 11.00000 0.05 0.50 Q18 1 0.3214 0.3540 0.5001 11.00000 0.05 0.49 Q19 1 0.2792 0.3901 0.7423 11.00000 0.05 0.48 Q20 1 0.4721 0.3295 0.5970 11.00000 0.05 0.48 ; _shelx_res_checksum 13115 _shelx_hkl_file ; 2 0 -2 2283.27 133.59 2 0 -2 1879.21 134.09 2 0 -2 2159.58 134.69 -2 0 2 1837.92 133.39 -4 0 4 1407.56 104.89 4 0 -4 1434.66 106.49 4 0 -4 1826.02 106.09 4 0 -4 1724.13 104.79 6 0 -6 2178.78 137.09 6 0 -6 1984.00 140.09 8 0 -8 899.61 63.19 8 0 -8 1035.90 68.49 10 0 -10 176.58 20.20 12 0 -12 846.62 66.29 14 0 -14 420.96 45.40 16 0 -16 236.98 38.40 1 1 -1 2974.70 212.48 1 1 -1 3378.96 214.28 1 1 -1 3445.56 213.48 -1 -1 1 3446.86 213.78 -1 -1 1 3205.18 213.68 -1 -1 1 3023.90 212.68 3 1 -3 247.38 14.90 3 -1 -3 175.18 15.90 3 -1 -3 209.28 15.30 -3 -1 3 241.18 14.80 -3 -1 3 216.48 15.50 5 1 -5 1799.92 100.79 5 1 -5 1536.05 103.29 5 -1 -5 1311.17 102.59 5 -1 -5 1610.74 100.49 -5 -1 5 1374.56 101.19 7 1 -7 273.47 18.00 7 1 -7 221.48 21.80 7 -1 -7 223.38 21.70 7 -1 -7 280.87 17.80 9 1 -9 176.78 19.20 9 1 -9 167.18 12.50 9 -1 -9 172.08 19.00 11 1 -11 513.95 44.60 11 -1 -11 586.44 45.60 13 1 -13 264.07 34.70 13 -1 -13 314.07 34.30 15 1 -15 187.18 35.00 15 -1 -15 172.58 34.00 0 2 0 12.20 1.90 0 -2 0 10.20 1.20 0 -2 0 14.60 1.30 0 -2 0 9.10 1.50 0 -2 0 13.50 1.80 2 2 -2 554.74 39.40 2 2 -2 639.14 40.40 2 2 -2 624.24 40.50 -2 -2 2 574.44 40.20 -2 -2 2 573.44 39.40 2 -2 -2 606.44 39.40 -2 -2 2 609.94 40.40 4 2 -4 371.16 29.20 4 2 -4 397.96 27.30 4 2 -4 473.45 29.20 -4 -2 4 395.56 27.20 -4 -2 4 344.67 28.00 4 -2 -4 466.35 28.10 6 2 -6 13.10 5.40 6 2 -6 7.90 2.10 6 -2 -6 11.00 4.90 6 -2 -6 9.30 2.00 -6 -2 6 5.70 2.40 8 2 -8 21.40 7.50 8 2 -8 15.60 2.90 8 -2 -8 12.50 2.50 8 -2 -8 14.90 7.00 10 2 -10 16.20 9.00 10 -2 -10 15.80 8.90 12 2 -12 3.30 10.90 12 -2 -12 5.50 11.10 14 2 -14 22.70 16.00 14 -2 -14 16.80 15.70 16 2 -16 16.50 19.00 16 -2 -16 -0.60 19.50 -1 3 1 1444.56 105.69 1 3 -1 1439.46 105.29 1 3 -1 1657.33 106.69 1 3 -1 1701.93 106.29 1 3 -1 1729.03 105.89 -1 -3 1 1646.54 106.19 -1 -3 1 1723.83 106.69 -1 -3 1 1521.75 105.29 3 3 -3 1548.65 91.19 3 3 -3 1215.88 89.29 3 3 -3 1406.56 90.99 -3 -3 3 1327.67 90.59 -3 -3 3 1326.77 89.39 3 -3 -3 1349.77 89.59 5 3 -5 1430.46 96.19 5 3 -5 1581.84 99.19 -5 -3 5 1416.66 97.69 -5 -3 5 1424.96 96.19 7 3 -7 1174.48 76.19 7 3 -7 1294.67 80.89 7 -3 -7 1097.29 75.89 7 -3 -7 1056.79 79.19 9 3 -9 566.44 42.60 9 3 -9 497.15 36.50 9 -3 -9 587.14 42.30 11 3 -11 557.04 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2 8 4 905.31 63.69 2 -8 4 1074.19 68.49 -2 -8 -4 921.11 70.69 0 8 -6 783.52 56.29 0 8 6 791.62 51.99 0 8 6 861.51 57.79 0 -8 6 659.93 55.99 0 -8 -6 745.73 60.39 -2 8 8 952.00 66.69 2 8 -8 1050.19 72.79 -2 8 8 1011.30 71.99 2 -8 -8 939.71 77.19 2 -8 -8 928.11 71.29 -2 -8 8 1190.08 74.19 4 8 -10 621.24 50.09 -4 8 10 622.54 46.90 4 -8 -10 630.54 48.60 -4 -8 10 705.23 50.09 4 -8 -10 531.75 55.09 -6 8 12 665.23 48.70 6 8 -12 635.84 54.79 -6 -8 12 672.33 52.29 6 -8 -12 666.73 53.29 8 8 -14 284.27 35.60 8 -8 -14 291.97 35.10 -8 -8 14 267.77 28.10 10 8 -16 142.39 29.80 17 9 -11 215.78 19.30 17 9 -11 252.97 30.50 17 -9 -11 188.38 24.10 17 -9 -11 206.18 28.90 15 9 -9 329.47 31.30 15 9 -9 271.27 22.70 15 -9 -9 318.47 24.30 15 -9 -9 219.78 27.40 13 9 -7 458.15 37.50 13 9 -7 413.06 32.10 -11 9 5 979.80 73.99 11 9 -5 1187.08 78.39 11 9 -5 1076.19 73.19 -9 9 3 1301.27 90.59 9 9 -3 1297.77 90.39 9 9 -3 1269.27 85.99 -9 -9 3 1203.88 91.79 7 9 -1 691.33 49.60 7 9 -1 700.73 45.40 -7 9 1 652.33 43.80 -7 9 1 653.43 43.90 -7 -9 1 670.63 50.89 7 -9 -1 547.55 46.20 5 9 1 2036.40 136.89 -5 9 -1 1870.51 135.69 5 9 1 1984.00 132.49 -5 9 -1 1960.80 135.19 -5 -9 -1 2049.99 138.39 5 -9 1 2058.19 135.59 -3 9 -3 1908.01 127.49 3 9 3 1795.62 123.69 3 9 3 1927.61 128.49 3 -9 3 1926.51 127.79 -3 -9 -3 1752.62 129.39 1 9 5 566.24 40.40 -1 9 -5 613.24 44.90 1 9 5 593.54 45.60 1 -9 5 568.94 45.00 -1 -9 -5 615.94 48.10 -1 9 7 878.21 62.99 1 9 -7 859.91 62.39 -1 9 7 779.62 57.09 1 -9 -7 874.41 66.29 -1 -9 7 919.91 63.49 3 9 -9 952.60 67.69 -3 9 9 884.51 65.59 3 -9 -9 879.41 65.89 3 -9 -9 875.61 71.19 -3 -9 9 948.31 67.39 -5 9 11 491.95 37.40 5 9 -11 503.15 42.20 5 -9 -11 457.45 45.50 -5 -9 11 430.36 39.10 5 -9 -11 478.55 40.10 7 9 -13 397.26 40.70 7 -9 -13 385.66 38.90 -7 -9 13 391.06 35.50 9 9 -15 276.87 37.40 -9 -9 15 219.88 26.30 18 10 -12 34.60 15.10 16 10 -10 43.00 7.90 16 10 -10 57.69 15.70 16 -10 -10 38.40 9.40 16 -10 -10 35.80 13.50 14 10 -8 122.69 19.80 14 10 -8 132.19 18.80 14 10 -8 130.69 13.80 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36.50 11.30 6 -10 -12 70.39 15.00 8 10 -14 121.99 25.00 8 -10 -14 119.49 28.80 -8 -10 14 124.09 19.60 10 10 -16 11.60 20.00 17 11 -11 46.60 8.10 17 11 -11 39.70 16.20 15 11 -9 5.70 8.70 15 11 -9 10.80 5.80 15 11 -9 4.30 10.80 15 -11 -9 20.70 10.30 13 11 -7 45.60 11.80 13 11 -7 45.20 7.90 11 11 -5 22.90 5.90 11 11 -5 34.60 9.90 -9 11 3 213.48 23.10 9 11 -3 225.98 18.30 9 11 -3 239.98 23.40 9 -11 -3 203.28 19.90 7 11 -1 12.10 4.30 -7 11 1 28.40 4.90 7 11 -1 19.00 7.30 7 -11 -1 22.80 7.30 -7 -11 1 24.60 9.90 5 11 1 524.35 36.00 -5 11 -1 482.25 39.70 5 11 1 561.54 41.40 5 -11 1 436.16 39.20 -5 -11 -1 544.75 42.30 -3 11 -3 192.68 22.30 3 11 3 243.48 23.20 -3 11 -3 257.97 22.60 3 11 3 241.78 18.10 3 -11 3 209.78 22.20 -3 -11 -3 238.58 24.80 -1 11 -5 102.89 14.40 1 11 5 72.59 8.80 1 11 5 103.89 14.90 -1 -11 -5 88.19 15.80 1 -11 5 95.29 14.50 1 11 -7 7.90 7.90 -1 11 7 3.70 3.00 -1 11 7 8.30 8.30 1 -11 -7 14.40 9.90 -1 -11 7 1.10 6.40 -3 11 9 161.98 19.10 3 11 -9 198.98 21.30 3 -11 -9 171.48 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359.86 30.80 0 12 6 356.26 24.30 0 12 -6 337.07 29.20 0 -12 6 280.17 28.40 0 -12 -6 310.27 30.70 -2 12 8 1088.29 75.09 2 12 -8 1051.89 74.79 -2 12 8 950.20 68.59 -2 -12 8 1104.39 75.89 2 -12 -8 954.70 75.09 -4 12 10 413.46 34.10 4 12 -10 436.96 38.80 -4 -12 10 423.66 37.50 4 -12 -10 408.66 35.30 4 -12 -10 448.06 37.90 6 12 -12 267.37 31.90 -6 -12 12 226.08 26.50 6 -12 -12 262.07 28.70 8 12 -14 145.99 28.90 -8 -12 14 86.39 17.10 10 12 -16 129.49 29.10 17 13 -11 217.08 20.90 17 13 -11 291.57 32.70 15 13 -9 304.97 31.00 15 13 -9 221.08 21.30 15 13 -9 256.77 29.30 13 13 -7 404.56 34.20 13 13 -7 342.87 34.40 13 13 -7 331.77 27.80 11 13 -5 847.12 60.79 11 13 -5 904.41 67.59 -9 13 3 825.22 66.29 9 13 -3 879.71 62.19 9 13 -3 970.10 68.69 9 -13 -3 923.81 65.79 -7 13 1 704.73 51.89 7 13 -1 787.72 58.09 7 13 -1 772.62 52.19 -7 -13 1 719.53 58.19 7 -13 -1 765.42 56.49 5 13 1 1580.74 104.19 5 13 1 1452.05 98.09 -5 13 -1 1420.76 102.49 -5 -13 -1 1460.65 103.69 5 -13 1 1372.16 102.59 3 13 3 1767.52 113.19 -3 13 -3 1714.43 116.69 3 13 3 1788.42 119.19 -3 13 -3 1619.54 119.29 -3 -13 -3 1759.72 118.89 3 -13 3 1470.65 117.59 -1 13 -5 827.42 57.49 -1 13 -5 677.63 59.89 1 13 5 701.13 58.19 1 13 5 708.13 52.49 -1 -13 -5 811.42 58.99 1 -13 5 898.41 59.49 -1 13 7 1269.57 87.69 -1 13 7 1342.67 94.19 1 13 -7 1400.06 93.29 1 -13 -7 1322.97 93.69 -1 -13 7 1212.98 93.79 3 13 -9 464.05 38.90 -3 13 9 436.96 36.50 3 -13 -9 388.16 37.10 -3 -13 9 455.35 38.30 5 13 -11 332.87 34.00 -5 13 11 312.77 27.00 5 -13 -11 322.37 34.50 -5 -13 11 310.97 31.20 7 13 -13 281.67 35.20 -7 -13 13 268.87 30.00 9 13 -15 207.88 34.60 -9 -13 15 159.88 23.90 16 14 -10 31.40 14.10 16 14 -10 24.30 6.90 14 14 -8 163.58 23.50 14 14 -8 158.38 23.00 14 14 -8 179.38 16.80 12 14 -6 94.99 16.80 12 14 -6 105.39 12.70 12 14 -6 125.39 19.20 10 14 -4 125.99 13.70 10 14 -4 140.59 19.70 10 -14 -4 133.49 16.60 8 14 -2 356.36 27.70 8 14 -2 377.56 33.40 8 -14 -2 361.36 32.10 6 14 0 295.77 24.20 6 14 0 310.67 29.40 -6 14 0 333.07 27.40 -6 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163.88 25.60 5 3 10 108.59 22.20 5 -3 10 95.69 20.90 -5 -3 -10 144.69 41.90 3 3 12 62.89 18.20 3 -3 12 57.89 19.60 -3 -3 -12 107.89 44.10 1 3 14 80.29 23.20 -1 -3 -14 163.18 51.99 1 -3 14 88.09 23.30 18 4 -3 3.70 9.90 18 -4 -3 7.80 9.30 -18 -4 3 44.20 23.60 -16 4 1 21.90 21.10 16 4 -1 7.40 8.30 16 -4 -1 -2.40 7.80 -16 -4 1 -11.40 17.60 -14 4 -1 29.60 25.40 14 4 1 12.90 12.40 14 4 1 15.30 9.20 -14 -4 -1 20.80 24.10 14 -4 1 14.10 11.40 14 -4 1 4.40 8.30 -12 4 -3 -3.30 22.20 12 4 3 -12.30 10.80 12 4 3 0.30 8.00 12 -4 3 6.10 11.00 -12 -4 -3 6.30 21.70 12 -4 3 -6.80 6.80 10 4 5 -2.90 11.00 -10 4 -5 8.30 24.40 10 4 5 -8.00 6.50 -10 -4 -5 21.80 25.20 10 -4 5 6.50 11.40 10 -4 5 -6.00 5.90 8 4 7 -4.60 11.60 8 4 7 -1.90 6.60 -8 4 -7 -21.50 22.30 8 -4 7 -4.40 10.90 8 -4 7 -2.40 6.30 -8 -4 -7 -1.30 23.80 6 4 9 38.50 9.20 6 4 9 41.30 16.60 -6 -4 -9 39.60 30.20 6 -4 9 17.60 13.90 6 -4 9 19.50 7.40 4 4 11 -4.70 12.00 -4 -4 -11 9.10 34.30 4 -4 11 -0.90 13.60 2 4 13 -1.30 14.60 -2 -4 -13 27.90 34.80 2 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-4 170.38 38.00 12 -8 4 150.28 24.40 12 -8 4 167.28 19.90 10 8 6 153.18 26.80 -10 8 -6 179.98 43.00 10 8 6 130.09 18.30 10 -8 6 100.99 20.20 10 -8 6 98.39 14.80 -10 -8 -6 110.49 33.40 -8 8 -8 154.08 42.60 8 8 8 164.88 19.30 8 8 8 130.69 26.10 8 -8 8 138.39 25.70 -8 -8 -8 171.08 42.30 8 -8 8 173.28 18.80 6 8 10 70.99 20.10 6 -8 10 129.09 24.30 -6 -8 -10 181.78 46.20 4 8 12 54.59 19.50 4 -8 12 69.19 22.30 -4 -8 -12 142.39 46.30 -15 9 -1 232.48 45.20 15 9 1 155.68 28.00 15 9 1 161.08 22.20 15 -9 1 115.89 18.20 -15 -9 -1 150.38 36.70 -13 9 -3 199.98 44.00 13 9 3 182.98 28.80 13 9 3 179.58 23.40 -13 -9 -3 213.08 40.50 13 -9 3 142.59 23.20 13 -9 3 191.68 21.10 11 9 5 182.78 21.50 11 9 5 163.18 28.40 -11 9 -5 164.68 43.60 11 -9 5 182.88 20.00 -11 -9 -5 169.28 38.40 11 -9 5 139.49 25.10 9 9 7 192.88 22.80 9 9 7 162.78 29.60 -9 9 -7 180.18 45.40 9 -9 7 228.88 30.30 9 -9 7 265.37 22.90 -9 -9 -7 228.38 44.80 7 9 9 102.89 24.20 -7 -9 -9 174.18 44.20 7 -9 9 105.29 23.70 7 -9 9 161.78 17.90 5 9 11 79.29 21.90 5 -9 11 91.29 22.20 -5 -9 -11 106.29 43.00 16 10 0 93.39 22.60 16 10 0 108.79 18.00 -16 -10 0 139.79 36.50 16 -10 0 90.39 15.40 14 10 2 6.70 9.70 -14 10 -2 3.30 21.40 14 10 2 10.10 15.00 -14 -10 -2 -26.80 20.30 14 -10 2 2.70 8.70 -12 10 -4 81.69 32.40 12 10 4 52.89 12.80 12 10 4 27.10 17.20 12 -10 4 53.49 16.10 -12 -10 -4 75.29 28.90 -10 10 -6 26.20 30.40 10 10 6 9.20 14.00 10 10 6 33.30 10.60 10 -10 6 37.60 14.90 -10 -10 -6 4.20 23.00 8 10 8 84.99 23.10 8 10 8 123.19 17.00 -8 -10 -8 133.59 37.90 8 -10 8 93.69 21.20 6 10 10 -13.10 12.60 6 -10 10 21.80 16.30 -6 -10 -10 20.00 30.60 15 11 1 7.00 14.10 15 11 1 11.40 10.40 -15 11 -1 47.10 35.50 15 -11 1 15.60 8.90 -15 -11 -1 6.60 22.30 13 11 3 44.70 12.90 13 11 3 40.90 17.40 -13 11 -3 36.40 28.10 -13 -11 -3 19.50 24.50 13 -11 3 39.80 21.20 11 11 5 14.40 15.20 11 11 5 -0.80 8.40 -11 11 -5 39.40 28.10 11 -11 5 10.00 12.90 -11 -11 -5 32.80 24.80 9 11 7 15.70 9.00 9 11 7 0.00 13.80 -9 -11 -7 9.90 26.50 9 -11 7 7.40 13.10 7 11 9 3.80 14.70 -7 -11 -9 0.50 24.50 7 -11 9 7.30 14.10 5 11 11 26.50 16.80 5 -11 11 10.10 15.90 -5 -11 -11 -3.90 28.30 14 12 2 128.99 25.90 -14 12 -2 106.29 34.50 14 12 2 124.09 18.50 -14 -12 -2 93.49 31.80 -12 12 -4 95.89 38.50 12 12 4 101.09 15.80 12 12 4 111.69 24.20 12 -12 4 92.99 19.90 -12 -12 -4 110.39 34.40 -10 12 -6 114.79 38.80 10 12 6 117.19 24.70 10 12 6 111.19 16.40 10 -12 6 87.59 20.70 -10 -12 -6 141.29 36.80 8 12 8 182.98 20.50 8 12 8 154.68 29.10 8 -12 8 143.19 27.50 -8 -12 -8 159.28 40.50 6 12 10 51.29 19.10 -6 -12 -10 56.69 31.80 6 -12 10 55.99 20.30 -13 13 -3 190.88 45.30 13 13 3 114.39 18.20 13 13 3 135.99 27.40 -13 -13 -3 149.29 36.80 11 13 5 164.88 28.80 11 13 5 159.98 20.10 -11 13 -5 152.28 43.00 -11 -13 -5 93.09 32.70 11 -13 5 117.49 23.10 9 13 7 150.58 29.10 9 13 7 215.38 22.20 9 -13 7 157.58 28.40 -9 -13 -7 220.28 43.20 7 13 9 72.59 22.20 7 -13 9 117.99 24.30 -7 -13 -9 52.49 30.80 12 14 4 68.09 22.20 -12 14 -4 65.19 30.60 12 14 4 68.49 13.80 12 -14 4 94.09 20.00 -12 -14 -4 104.69 31.60 10 14 6 21.10 9.90 -10 14 -6 4.60 28.60 10 14 6 28.40 16.90 -10 -14 -6 33.60 27.20 10 -14 6 23.30 15.20 8 14 8 61.59 11.90 8 14 8 71.99 21.80 8 -14 8 55.09 19.20 -8 -14 -8 67.99 31.20 11 15 5 1.90 8.90 -11 15 -5 24.90 28.60 11 15 5 1.00 14.00 -11 -15 -5 3.90 22.10 11 -15 5 10.90 14.50 9 15 7 -0.90 8.00 9 15 7 -22.00 13.00 -9 15 -7 4.60 12.30 9 -15 7 -0.70 13.80 16 0 1 5.30 8.80 -16 0 -1 13.50 26.30 14 0 3 7.90 13.10 -14 0 -3 20.50 25.00 14 0 3 -6.90 7.40 12 0 5 3.00 8.10 -12 0 -5 12.30 27.00 12 0 5 -4.50 12.20 -10 0 -7 -17.30 24.00 10 0 7 -4.40 6.60 10 0 7 7.90 13.40 8 0 9 7.80 13.20 -8 0 -9 -11.70 26.30 8 0 9 -6.80 6.80 6 0 11 -10.00 13.10 -6 0 -11 13.70 31.40 -15 1 -2 19.10 28.00 15 1 2 24.70 10.80 15 1 2 21.30 15.00 15 -1 2 9.60 13.70 15 -1 2 36.50 11.50 -15 -1 -2 44.50 27.70 -13 1 -4 52.69 29.70 13 1 4 57.59 12.90 13 1 4 65.49 18.50 13 -1 4 51.49 12.00 13 -1 4 62.69 18.70 -13 -1 -4 137.99 38.20 -11 1 -6 130.89 39.90 11 1 6 115.99 17.10 11 1 6 94.39 21.80 11 -1 6 92.69 14.60 -11 -1 -6 77.69 35.70 11 -1 6 118.29 22.70 -9 1 -8 96.09 38.20 9 1 8 78.39 14.00 9 1 8 59.09 19.20 9 -1 8 50.59 11.70 -9 -1 -8 55.19 32.90 9 -1 8 46.90 16.10 -7 1 -10 31.80 33.60 7 1 10 28.10 15.80 -7 -1 -10 16.20 33.60 7 -1 10 31.30 16.40 16 2 1 164.88 22.80 -16 2 -1 159.08 40.20 16 -2 1 193.18 22.70 -16 -2 -1 138.39 40.10 14 2 3 81.89 15.30 -14 2 -3 93.49 34.90 14 2 3 144.99 26.20 14 -2 3 101.59 21.30 -14 -2 -3 106.59 35.60 14 -2 3 144.39 19.00 12 2 5 160.28 27.70 -12 2 -5 245.08 51.19 12 2 5 233.88 23.90 12 -2 5 211.98 22.90 -12 -2 -5 173.78 42.70 12 -2 5 161.78 27.60 10 2 7 180.78 20.30 -10 2 -7 170.98 45.10 10 2 7 104.19 22.30 -10 -2 -7 145.89 43.80 10 -2 7 110.39 22.50 10 -2 7 142.79 19.00 8 2 9 120.99 23.50 -8 2 -9 60.59 36.40 8 2 9 99.39 17.80 8 -2 9 69.49 19.80 8 -2 9 110.09 15.10 -8 -2 -9 105.89 41.30 -6 2 -11 160.38 49.50 6 2 11 90.89 22.60 6 -2 11 156.78 28.00 -6 -2 -11 130.99 46.10 -15 3 -2 89.19 35.50 15 3 2 94.99 22.00 15 3 2 110.29 17.90 15 -3 2 143.79 19.30 -15 -3 -2 80.59 32.80 13 3 4 148.69 25.90 13 3 4 115.29 16.90 -13 3 -4 124.99 39.20 -13 -3 -4 92.49 37.00 13 -3 4 117.89 17.50 13 -3 4 101.59 21.10 -11 3 -6 200.88 46.50 11 3 6 95.79 21.30 11 3 6 136.49 19.40 -11 -3 -6 116.39 37.90 11 -3 6 63.09 18.10 11 -3 6 92.49 14.10 -9 3 -8 75.49 34.90 9 3 8 32.50 16.30 9 3 8 40.80 11.40 9 -3 8 38.00 15.10 -9 -3 -8 63.69 32.30 9 -3 8 35.00 10.10 7 3 10 99.89 22.30 -7 3 -10 177.88 49.20 -7 -3 -10 94.29 41.10 7 -3 10 63.29 19.00 16 4 1 27.50 16.40 -16 4 -1 9.60 23.90 16 4 1 2.80 9.60 -16 -4 -1 2.20 24.50 16 -4 1 14.60 10.10 14 4 3 5.20 9.60 14 4 3 13.60 14.40 -14 4 -3 15.20 24.90 14 -4 3 12.10 9.20 -14 -4 -3 -15.50 21.70 14 -4 3 19.30 13.80 12 4 5 1.80 9.00 12 4 5 -1.90 13.90 -12 4 -5 20.30 28.40 12 -4 5 3.90 8.40 12 -4 5 14.70 13.20 -12 -4 -5 -4.20 25.90 10 4 7 12.50 13.30 10 4 7 4.40 8.60 -10 4 -7 43.50 34.90 10 -4 7 10.20 12.70 10 -4 7 4.60 7.40 -10 -4 -7 -25.20 23.10 -8 4 -9 -13.90 26.60 8 4 9 8.70 13.30 8 -4 9 -0.90 13.20 8 -4 9 3.20 6.90 -8 -4 -9 -33.90 25.40 -6 4 -11 -3.60 31.70 6 4 11 27.60 16.00 6 -4 11 5.70 14.90 -6 -4 -11 12.50 31.70 15 5 2 52.09 17.90 15 5 2 46.40 13.50 -15 5 -2 38.60 27.90 15 -5 2 47.90 12.50 -15 -5 -2 9.90 25.60 13 5 4 11.40 11.10 13 5 4 24.30 15.50 -13 5 -4 42.60 29.90 13 -5 4 21.50 13.60 13 -5 4 27.60 9.60 -13 -5 -4 -0.10 25.20 -11 5 -6 41.80 32.70 11 5 6 23.00 15.90 11 5 6 7.50 9.20 11 -5 6 34.30 9.50 11 -5 6 28.10 14.00 -11 -5 -6 18.00 27.20 9 5 8 39.30 17.50 -9 5 -8 34.80 32.10 9 5 8 42.20 10.80 9 -5 8 37.80 15.70 9 -5 8 39.60 10.30 -9 -5 -8 47.10 32.30 -7 5 -10 56.79 35.90 7 5 10 24.40 16.90 7 -5 10 17.00 15.10 -7 -5 -10 24.80 31.90 14 6 3 142.99 27.10 -14 6 -3 181.68 44.00 14 6 3 151.88 22.90 -14 -6 -3 143.19 39.80 14 -6 3 156.38 20.10 14 -6 3 134.59 22.80 12 6 5 90.49 21.80 -12 6 -5 118.49 39.70 12 6 5 104.89 16.90 12 -6 5 104.89 15.50 12 -6 5 75.69 18.60 -12 -6 -5 73.99 33.40 -10 6 -7 124.49 42.80 10 6 7 163.18 21.10 10 6 7 115.19 24.70 -10 -6 -7 138.09 40.20 10 -6 7 137.19 25.20 10 -6 7 185.58 19.80 -8 6 -9 69.39 37.30 8 6 9 69.39 20.70 8 -6 9 96.89 22.50 -8 -6 -9 143.39 41.60 8 -6 9 101.29 14.40 6 6 11 113.79 23.70 6 -6 11 117.09 26.00 15 7 2 210.08 26.30 -15 7 -2 287.47 51.89 15 7 2 177.38 31.80 15 -7 2 216.88 24.20 -15 -7 -2 188.48 43.90 13 7 4 106.69 16.80 -13 7 -4 179.98 41.80 13 7 4 112.79 23.70 -13 -7 -4 95.49 33.00 13 -7 4 122.69 18.40 13 -7 4 95.99 20.50 -11 7 -6 178.98 46.40 11 7 6 115.99 17.60 11 7 6 102.99 24.20 11 -7 6 203.28 20.40 11 -7 6 115.99 22.00 -11 -7 -6 119.09 37.00 -9 7 -8 151.78 44.30 9 7 8 108.59 23.80 9 7 8 108.69 15.80 9 -7 8 52.59 18.30 -9 -7 -8 81.29 35.60 9 -7 8 123.99 17.20 -7 7 -10 96.69 40.60 7 7 10 74.29 21.90 -7 -7 -10 84.89 37.20 7 -7 10 102.79 23.10 14 8 3 15.40 12.20 -14 8 -3 24.20 27.60 14 8 3 21.50 15.80 14 -8 3 20.30 10.60 -14 -8 -3 10.30 24.50 -12 8 -5 36.90 31.70 12 8 5 70.79 14.70 12 8 5 43.60 16.90 12 -8 5 24.80 14.10 12 -8 5 23.40 9.90 -12 -8 -5 38.70 26.30 10 8 7 53.69 18.90 10 8 7 35.00 10.60 -10 8 -7 47.30 32.60 -10 -8 -7 24.20 28.00 10 -8 7 48.50 17.00 10 -8 7 36.10 9.90 -8 8 -9 -6.70 30.00 8 8 9 14.50 15.70 -8 -8 -9 33.50 31.50 8 -8 9 15.30 8.30 8 -8 9 5.40 15.30 13 9 4 7.60 10.00 -13 9 -4 10.20 24.80 13 9 4 20.50 15.40 13 -9 4 -5.90 11.30 -13 -9 -4 -1.20 22.70 13 -9 4 19.40 9.40 11 9 6 11.90 10.10 -11 9 -6 3.90 28.60 11 9 6 11.30 15.10 11 -9 6 12.10 13.70 -11 -9 -6 30.80 27.10 11 -9 6 11.50 8.70 9 9 8 1.70 14.80 9 9 8 -0.50 8.10 -9 9 -8 2.10 28.30 9 -9 8 -2.20 12.80 9 -9 8 1.70 8.00 -9 -9 -8 15.50 26.70 12 10 5 87.29 23.10 -12 10 -5 129.59 40.90 12 10 5 95.69 15.70 12 -10 5 71.39 19.30 -12 -10 -5 112.49 35.20 12 -10 5 85.39 14.60 10 10 7 133.09 20.10 10 10 7 130.49 26.80 -10 10 -7 212.98 49.50 -10 -10 -7 141.39 39.60 10 -10 7 136.19 18.70 10 -10 7 133.69 25.70 8 10 9 25.70 18.00 8 -10 9 67.09 19.80 11 11 6 164.08 21.70 11 11 6 135.79 27.10 -11 11 -6 169.28 45.10 11 -11 6 109.09 23.20 -11 -11 -6 156.68 39.40 11 -11 6 174.98 20.10 9 -11 8 170.28 28.50 14 0 4 73.89 20.10 12 0 6 152.68 26.90 -12 0 -6 114.69 39.80 12 0 6 152.68 21.50 -10 0 -8 239.98 49.70 10 0 8 149.59 20.30 10 0 8 137.79 25.80 13 1 5 61.99 19.40 -13 1 -5 118.09 38.90 13 1 5 57.79 12.90 13 -1 5 57.49 13.00 13 -1 5 64.69 19.00 -13 -1 -5 45.90 32.50 11 1 7 89.49 15.30 -11 1 -7 62.29 35.70 11 1 7 101.39 22.70 11 -1 7 84.69 20.80 -11 -1 -7 72.49 34.00 11 -1 7 89.29 14.70 -12 2 -6 14.20 32.60 12 2 6 -18.00 12.40 12 2 6 7.30 8.80 12 -2 6 -3.70 13.40 12 -2 6 0.60 8.10 -12 -2 -6 -6.30 24.20 10 2 8 -12.90 13.20 10 2 8 -4.30 8.30 10 -2 8 -6.60 7.80 10 -2 8 12.90 14.30 13 3 5 4.30 13.90 13 -3 5 23.40 15.10 11 3 7 35.00 18.80 -11 3 -7 10.00 29.50 11 3 7 52.89 12.90 -11 -3 -7 44.90 31.40 11 -3 7 61.69 18.30 11 -3 7 107.09 15.30 12 4 6 94.79 22.10 12 -4 6 59.29 17.50 10 4 8 122.49 26.10 10 -4 8 185.38 28.10 0 0 0 0.00 0.00 _computing_structure_solution 'SHELXT 2018/2 (Sheldrick, 2018)' ; _shelx_hkl_checksum 4530 _olex2_diffrn_ambient_temperature_device Kryoflex _olex2_exptl_crystal_mounting_method 'The crystal was mounted on a mylar loop in oil' _olex2_submission_original_sample_id AI-[Pb(ampam)]2+ _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -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 Pb1 Pb 0.500000 0.36753(2) 0.750000 0.02072(6) Uani 1 2 d S T P . . O1 O 0.43947(18) 0.45719(9) 0.8492(2) 0.0266(5) Uani 1 1 d . . . . . O2 O 0.5089(2) 0.32584(10) 0.5509(2) 0.0298(5) Uani 1 1 d . . . . . O3 O 0.3813(2) 0.26705(9) 0.6900(2) 0.0282(5) Uani 1 1 d . . . . . N1 N 0.3825(3) 0.45708(14) 0.9869(3) 0.0314(7) Uani 1 1 d . . . . . H1A H 0.433(4) 0.480(2) 1.038(4) 0.047 Uiso 1 1 d . U . . . H1B H 0.340(4) 0.448(2) 0.999(5) 0.047 Uiso 1 1 d . U . . . N2 N 0.2753(2) 0.38004(12) 0.6802(3) 0.0247(5) Uani 1 1 d . . . . . N3 N 0.3257(2) 0.38729(12) 0.4964(3) 0.0248(5) Uani 1 1 d . . . . . N4 N 0.4488(3) 0.31818(19) 0.3421(4) 0.0499(9) Uani 1 1 d . . . . . H4A H 0.508(5) 0.292(2) 0.367(5) 0.075 Uiso 1 1 d . U . . . H4B H 0.391(5) 0.326(2) 0.261(6) 0.075 Uiso 1 1 d . U . . . C1 C 0.3736(2) 0.44028(13) 0.8796(3) 0.0247(6) Uani 1 1 d . . . . . C2 C 0.2782(2) 0.39708(15) 0.7966(3) 0.0274(6) Uani 1 1 d . . . . . H2A H 0.288218 0.361221 0.847948 0.033 Uiso 1 1 calc R U . . . H2B H 0.204886 0.415454 0.770914 0.033 Uiso 1 1 calc R U . . . C3 C 0.2207(3) 0.42704(15) 0.5828(3) 0.0296(7) Uani 1 1 d . . . . . H3A H 0.252720 0.465767 0.624421 0.036 Uiso 1 1 calc R U . . . H3B H 0.138618 0.427563 0.548171 0.036 Uiso 1 1 calc R U . . . C4 C 0.2366(3) 0.41889(14) 0.4730(3) 0.0268(7) Uani 1 1 d . . . . . C5 C 0.1629(3) 0.44557(16) 0.3529(4) 0.0337(8) Uani 1 1 d . . . . . H5 H 0.099293 0.467704 0.337421 0.040 Uiso 1 1 calc R U . . . C6 C 0.1846(3) 0.43899(16) 0.2578(4) 0.0366(8) Uani 1 1 d . . . . . H6 H 0.136832 0.457583 0.176328 0.044 Uiso 1 1 calc R U . . . C7 C 0.2754(3) 0.40553(17) 0.2804(3) 0.0352(8) Uani 1 1 d . . . . . H7 H 0.291073 0.400445 0.215273 0.042 Uiso 1 1 calc R U . . . C8 C 0.3433(3) 0.37950(14) 0.4010(3) 0.0273(7) Uani 1 1 d . . . . . C9 C 0.4407(3) 0.33921(16) 0.4365(3) 0.0307(7) Uani 1 1 d . . . . . C10 C 0.2146(3) 0.32307(15) 0.6275(3) 0.0305(7) Uani 1 1 d . . . . . H10A H 0.191086 0.319489 0.536154 0.037 Uiso 1 1 calc R U . . . H10B H 0.145188 0.323298 0.629182 0.037 Uiso 1 1 calc R U . . . C11 C 0.2850(3) 0.27040(15) 0.7010(4) 0.0335(7) Uani 1 1 d . . . . . H11A H 0.310853 0.273945 0.793125 0.040 Uiso 1 1 calc R U . . . H11B H 0.239030 0.233904 0.665885 0.040 Uiso 1 1 calc R U . . . C12 C 0.4504(3) 0.21739(14) 0.7580(4) 0.0338(8) Uani 1 1 d . . . . . H12A H 0.406325 0.180366 0.722690 0.041 Uiso 1 1 calc R U . . . H12B H 0.478049 0.220072 0.850734 0.041 Uiso 1 1 calc R U . . . O6A O -0.2773(17) 0.3159(13) 0.452(3) 0.080(9) Uani 0.266(7) 1 d D U P A 2 O4A O -0.0893(12) 0.3177(7) 0.578(2) 0.087(7) Uani 0.266(7) 1 d D U P A 2 O5A O -0.1870(17) 0.3971(6) 0.5035(18) 0.053(4) Uani 0.266(7) 1 d D U P A 2 N5A N -0.1838(10) 0.3421(5) 0.5095(12) 0.047(3) Uani 0.266(7) 1 d D U P A 2 O4 O -0.0279(12) 0.3725(5) 0.5685(18) 0.112(6) Uani 0.451(16) 1 d D U P B 1 O6 O -0.1781(11) 0.4171(9) 0.5288(18) 0.049(3) Uani 0.451(16) 1 d D U P B 1 O5 O -0.0265(12) 0.4659(5) 0.5781(16) 0.079(4) Uani 0.451(16) 1 d D U P B 1 N5 N -0.0773(9) 0.4188(4) 0.5613(14) 0.054(3) Uani 0.451(16) 1 d D U P B 1 O7 O -0.2827(8) 0.3024(4) 0.4369(12) 0.067(3) Uani 0.661(13) 1 d G . P C 3 H7A H -0.244490 0.283446 0.507707 0.101 Uiso 0.661(13) 1 d G U P C 3 H7B H -0.262817 0.338215 0.457645 0.101 Uiso 0.661(13) 1 d G U P C 3 O9 O -0.0638(12) 0.2811(6) 0.6725(18) 0.111(7) Uani 0.381(12) 1 d G . P D -1 H9A H -0.126728 0.263635 0.623634 0.167 Uiso 0.381(12) 1 d G U P D -1 H9B H -0.071369 0.314100 0.635492 0.167 Uiso 0.381(12) 1 d G U P D -1 O8 O -0.1711(18) 0.2601(8) 0.5684(19) 0.044(8) Uani 0.162(12) 1 d . . . E 4 O10 O 0.000000 0.4381(12) 0.750000 0.085(11) Uiso 0.26(2) 2 d S . . F 7 N5B N -0.0823(13) 0.4058(8) 0.573(2) 0.064(7) Uani 0.283(17) 1 d D U P G 3 O4B O -0.0755(14) 0.3507(9) 0.5710(19) 0.075(7) Uani 0.283(17) 1 d D U P G 3 O6B O -0.1780(16) 0.4293(13) 0.504(3) 0.049(3) Uani 0.283(17) 1 d D U P G 3 O5B O 0.0029(10) 0.4377(9) 0.643(2) 0.080(7) Uani 0.283(17) 1 d D U P G 3 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 0.02226(8) 0.01674(8) 0.02387(9) 0.000 0.01306(6) 0.000 O1 0.0224(10) 0.0238(11) 0.0344(12) -0.0060(9) 0.0159(9) -0.0022(8) O2 0.0343(12) 0.0297(12) 0.0304(13) 0.0032(9) 0.0210(10) 0.0031(9) O3 0.0380(12) 0.0182(10) 0.0320(12) -0.0014(9) 0.0214(10) -0.0049(9) N1 0.0261(14) 0.0351(16) 0.0356(16) -0.0143(12) 0.0185(12) -0.0079(11) N2 0.0204(11) 0.0253(13) 0.0277(14) -0.0047(10) 0.0128(10) -0.0044(9) N3 0.0218(11) 0.0255(13) 0.0260(13) -0.0008(10) 0.0123(10) -0.0049(10) N4 0.051(2) 0.073(3) 0.040(2) 0.0067(19) 0.0348(18) 0.0098(19) C1 0.0189(13) 0.0215(14) 0.0338(17) -0.0025(12) 0.0145(12) 0.0032(10) C2 0.0199(13) 0.0317(17) 0.0325(17) -0.0084(14) 0.0155(12) -0.0056(12) C3 0.0214(13) 0.0334(17) 0.0318(17) 0.0000(13) 0.0131(13) 0.0011(12) C4 0.0195(13) 0.0258(15) 0.0298(17) -0.0005(12) 0.0101(12) -0.0042(11) C5 0.0246(15) 0.0318(18) 0.0332(18) 0.0009(14) 0.0084(13) -0.0027(13) C6 0.0345(17) 0.0346(19) 0.0296(18) 0.0073(14) 0.0104(14) -0.0063(14) C7 0.0341(17) 0.040(2) 0.0282(17) 0.0055(14) 0.0149(14) -0.0082(14) C8 0.0260(14) 0.0293(16) 0.0242(15) 0.0001(12) 0.0122(12) -0.0090(12) C9 0.0356(17) 0.0336(18) 0.0324(18) 0.0003(14) 0.0248(15) -0.0062(14) C10 0.0263(15) 0.0319(17) 0.0338(18) -0.0088(13) 0.0168(13) -0.0109(13) C11 0.0421(19) 0.0278(17) 0.0383(19) -0.0085(14) 0.0269(16) -0.0141(14) C12 0.055(2) 0.0151(14) 0.0335(18) 0.0001(12) 0.0256(17) -0.0035(13) O6A 0.056(8) 0.14(2) 0.066(12) -0.068(14) 0.046(8) -0.031(11) O4A 0.048(7) 0.051(9) 0.114(15) -0.012(9) 0.012(8) -0.005(6) O5A 0.067(9) 0.068(7) 0.022(7) -0.003(7) 0.022(6) 0.014(7) N5A 0.044(6) 0.062(7) 0.042(7) -0.013(6) 0.027(5) -0.002(5) O4 0.066(7) 0.037(5) 0.244(17) 0.027(6) 0.092(10) 0.024(5) O6 0.033(2) 0.095(8) 0.018(7) -0.004(5) 0.013(3) 0.019(3) O5 0.099(8) 0.048(5) 0.115(10) -0.018(6) 0.075(8) -0.009(5) N5 0.046(5) 0.041(4) 0.074(8) -0.001(5) 0.032(5) 0.013(4) O7 0.071(5) 0.063(5) 0.061(6) -0.011(4) 0.031(4) 0.012(3) O9 0.100(10) 0.077(9) 0.203(19) 0.079(10) 0.113(12) 0.043(7) O8 0.064(15) 0.045(11) 0.049(12) 0.024(9) 0.048(11) 0.037(10) N5B 0.037(6) 0.059(8) 0.073(13) -0.006(8) 0.015(7) 0.016(6) O4B 0.034(7) 0.063(8) 0.085(12) -0.029(8) 0.006(7) 0.004(7) O6B 0.033(2) 0.095(8) 0.018(7) -0.004(5) 0.013(3) 0.019(3) O5B 0.027(5) 0.072(11) 0.112(14) -0.002(10) 0.019(6) 0.010(6) 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 _geom_angle_publ_flag O1 Pb1 O1 84.37(10) . 2_656 ? O1 Pb1 N3 70.95(7) . 2_656 ? O1 Pb1 N3 94.98(8) 2_656 2_656 ? O1 Pb1 N3 70.95(7) 2_656 . ? O1 Pb1 N3 94.98(8) . . ? O2 Pb1 O1 147.99(7) . . ? O2 Pb1 O1 70.68(7) . 2_656 ? O2 Pb1 O1 70.68(7) 2_656 . ? O2 Pb1 O1 147.99(7) 2_656 2_656 ? O2 Pb1 O2 139.16(10) . 2_656 ? O2 Pb1 N3 129.36(8) . 2_656 ? O2 Pb1 N3 129.36(8) 2_656 . ? O2 Pb1 N3 58.57(8) 2_656 2_656 ? O2 Pb1 N3 58.57(8) . . ? O3 Pb1 O1 116.90(7) 2_656 2_656 ? O3 Pb1 O1 143.73(7) 2_656 . ? O3 Pb1 O1 116.90(7) . . ? O3 Pb1 O1 143.73(7) . 2_656 ? O3 Pb1 O2 77.57(7) 2_656 2_656 ? O3 Pb1 O2 67.83(7) 2_656 . ? O3 Pb1 O2 77.57(7) . . ? O3 Pb1 O2 67.83(7) . 2_656 ? O3 Pb1 O3 63.73(10) 2_656 . ? O3 Pb1 N3 119.02(8) . 2_656 ? O3 Pb1 N3 119.02(8) 2_656 . ? O3 Pb1 N3 77.84(8) 2_656 2_656 ? O3 Pb1 N3 77.84(8) . . ? N3 Pb1 N3 161.40(12) . 2_656 ? C1 O1 Pb1 112.13(18) . . ? C9 O2 Pb1 124.2(2) . . ? C11 O3 Pb1 114.14(18) . . ? C12 O3 Pb1 112.57(19) . . ? C12 O3 C11 111.3(3) . . ? H1A N1 H1B 118(5) . . ? C1 N1 H1A 122(3) . . ? C1 N1 H1B 120(4) . . ? C2 N2 C3 109.6(3) . . ? C2 N2 C10 111.0(3) . . ? C3 N2 C10 110.4(3) . . ? C4 N3 Pb1 118.8(2) . . ? C4 N3 C8 119.0(3) . . ? C8 N3 Pb1 119.9(2) . . ? H4A N4 H4B 127(5) . . ? C9 N4 H4A 116(3) . . ? C9 N4 H4B 117(4) . . ? O1 C1 N1 122.8(3) . . ? O1 C1 C2 121.9(3) . . ? N1 C1 C2 115.3(3) . . ? N2 C2 C1 111.7(3) . . ? N2 C2 H2A 109.3 . . ? N2 C2 H2B 109.3 . . ? C1 C2 H2A 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 107.9 . . ? N2 C3 H3A 109.1 . . ? N2 C3 H3B 109.1 . . ? N2 C3 C4 112.4(3) . . ? H3A C3 H3B 107.8 . . ? C4 C3 H3A 109.1 . . ? C4 C3 H3B 109.1 . . ? N3 C4 C3 117.3(3) . . ? N3 C4 C5 121.8(3) . . ? C5 C4 C3 120.9(3) . . ? C4 C5 H5 120.8 . . ? C6 C5 C4 118.5(3) . . ? C6 C5 H5 120.8 . . ? C5 C6 H6 119.9 . . ? C5 C6 C7 120.2(3) . . ? C7 C6 H6 119.9 . . ? C6 C7 H7 121.0 . . ? C6 C7 C8 118.0(4) . . ? C8 C7 H7 121.0 . . ? N3 C8 C7 122.6(3) . . ? N3 C8 C9 113.6(3) . . ? C7 C8 C9 123.8(3) . . ? O2 C9 N4 122.2(4) . . ? O2 C9 C8 120.0(3) . . ? N4 C9 C8 117.8(3) . . ? N2 C10 H10A 109.0 . . ? N2 C10 H10B 109.0 . . ? N2 C10 C11 113.1(3) . . ? H10A C10 H10B 107.8 . . ? C11 C10 H10A 109.0 . . ? C11 C10 H10B 109.0 . . ? O3 C11 C10 109.3(3) . . ? O3 C11 H11A 109.8 . . ? O3 C11 H11B 109.8 . . ? C10 C11 H11A 109.8 . . ? C10 C11 H11B 109.8 . . ? H11A C11 H11B 108.3 . . ? O3 C12 C12 107.8(2) . 2_656 ? O3 C12 H12A 110.1 . . ? O3 C12 H12B 110.1 . . ? C12 C12 H12A 110.1 2_656 . ? C12 C12 H12B 110.1 2_656 . ? H12A C12 H12B 108.5 . . ? O4A N5A O6A 125.2(17) . . ? O5A N5A O6A 116.5(17) . . ? O5A N5A O4A 118.2(14) . . ? O4 N5 O6 119.8(12) . . ? O4 N5 O5 117.8(10) . . ? O5 N5 O6 122.2(12) . . ? H7A O7 H7B 104.5 . . ? H9A O9 H9B 104.5 . . ? O4B N5B O6B 118.2(17) . . ? O4B N5B O5B 122.1(15) . . ? O6B N5B O5B 119.6(17) . . ? 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 O1 2.734(2) . ? Pb1 O1 2.734(2) 2_656 ? Pb1 O2 2.700(2) . ? Pb1 O2 2.700(2) 2_656 ? Pb1 O3 2.673(2) . ? Pb1 O3 2.673(2) 2_656 ? Pb1 N3 2.763(3) . ? Pb1 N3 2.763(3) 2_656 ? O1 C1 1.237(4) . ? O2 C9 1.236(4) . ? O3 C11 1.438(4) . ? O3 C12 1.421(4) . ? N1 H1A 0.82(5) . ? N1 H1B 0.73(5) . ? N1 C1 1.317(4) . ? N2 C2 1.468(4) . ? N2 C3 1.469(4) . ? N2 C10 1.485(4) . ? N3 C4 1.331(4) . ? N3 C8 1.342(5) . ? N4 H4A 0.93(6) . ? N4 H4B 0.90(6) . ? N4 C9 1.322(5) . ? C1 C2 1.518(4) . ? C2 H2A 0.9900 . ? C2 H2B 0.9900 . ? C3 H3A 0.9900 . ? C3 H3B 0.9900 . ? C3 C4 1.502(5) . ? C4 C5 1.400(5) . ? C5 H5 0.9500 . ? C5 C6 1.373(6) . ? C6 H6 0.9500 . ? C6 C7 1.377(6) . ? C7 H7 0.9500 . ? C7 C8 1.387(5) . ? C8 C9 1.498(5) . ? C10 H10A 0.9900 . ? C10 H10B 0.9900 . ? C10 C11 1.497(5) . ? C11 H11A 0.9900 . ? C11 H11B 0.9900 . ? C12 C12 1.513(8) 2_656 ? C12 H12A 0.9900 . ? C12 H12B 0.9900 . ? O6A N5A 1.252(13) . ? O4A N5A 1.250(12) . ? O5A N5A 1.244(12) . ? O4 N5 1.232(9) . ? O6 N5 1.247(11) . ? O5 N5 1.237(10) . ? O7 H7A 0.8498 . ? O7 H7B 0.8498 . ? O9 H9A 0.8493 . ? O9 H9B 0.8503 . ? N5B O4B 1.251(12) . ? N5B O6B 1.252(13) . ? N5B O5B 1.253(12) . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A _geom_hbond_publ_flag N1 H1A O1 0.82(5) 2.11(5) 2.931(4) 173(4) 5_667 yes N1 H1B O6 0.73(5) 2.22(5) 2.922(15) 162(5) 2_556 yes N4 H4A O9 0.93(6) 2.00(6) 2.830(14) 148(5) 7_556 yes N4 H4B O7 0.90(6) 2.13(6) 2.944(12) 151(5) 2 yes O7 H7A O7 0.85 2.02 2.70(2) 136.6 7_456 yes 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 _geom_torsion_publ_flag Pb1 O1 C1 N1 138.0(3) . . . . ? Pb1 O1 C1 C2 -40.2(3) . . . . ? Pb1 O2 C9 N4 179.3(3) . . . . ? Pb1 O2 C9 C8 -2.0(4) . . . . ? Pb1 O3 C11 C10 51.5(3) . . . . ? Pb1 O3 C12 C12 -50.1(4) . . . 2_656 ? Pb1 N3 C4 C3 -16.9(4) . . . . ? Pb1 N3 C4 C5 160.6(2) . . . . ? Pb1 N3 C8 C7 -159.0(2) . . . . ? Pb1 N3 C8 C9 22.4(3) . . . . ? O1 C1 C2 N2 -0.8(4) . . . . ? N1 C1 C2 N2 -179.2(3) . . . . ? N2 C3 C4 N3 -24.1(4) . . . . ? N2 C3 C4 C5 158.4(3) . . . . ? N2 C10 C11 O3 -63.4(4) . . . . ? N3 C4 C5 C6 -0.6(5) . . . . ? N3 C8 C9 O2 -13.8(4) . . . . ? N3 C8 C9 N4 164.9(3) . . . . ? C2 N2 C3 C4 167.8(2) . . . . ? C2 N2 C10 C11 -77.8(3) . . . . ? C3 N2 C2 C1 -79.4(3) . . . . ? C3 N2 C10 C11 160.4(3) . . . . ? C3 C4 C5 C6 176.9(3) . . . . ? C4 N3 C8 C7 3.3(5) . . . . ? C4 N3 C8 C9 -175.4(3) . . . . ? C4 C5 C6 C7 1.7(5) . . . . ? C5 C6 C7 C8 -0.4(5) . . . . ? C6 C7 C8 N3 -2.1(5) . . . . ? C6 C7 C8 C9 176.4(3) . . . . ? C7 C8 C9 O2 167.6(3) . . . . ? C7 C8 C9 N4 -13.7(5) . . . . ? C8 N3 C4 C3 -179.4(3) . . . . ? C8 N3 C4 C5 -1.9(5) . . . . ? C10 N2 C2 C1 158.4(3) . . . . ? C10 N2 C3 C4 -69.6(3) . . . . ? C11 O3 C12 C12 -179.7(3) . . . 2_656 ? C12 O3 C11 C10 -179.7(3) . . . . ?