#------------------------------------------------------------------------------ #$Date: 2017-04-21 05:23:32 +0300 (Fri, 21 Apr 2017) $ #$Revision: 195646 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/04/27/7042741.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_7042741 loop_ _publ_author_name 'Liberato, Andrea' 'Aguinaco, Almudena' 'Clares, Maria Paz' 'Delgado-Pinar, Estefania' 'Blasco, Salvador' 'Pitarch-Jarque, Javier' 'Basallote, Manuel G.' 'Garc\'ia-Espa\~na, Enrique' 'Verdejo, Bego\~na' _publ_section_title ; Pb2+ Complexes of Small-Cavity Azamacrocyclic Ligands. Thermodynamic and Kinetic Studies ; _journal_name_full 'Dalton Trans.' _journal_paper_doi 10.1039/C7DT00680B _journal_year 2017 _chemical_formula_moiety '2(C27 H34 Cl0.5 N5.5 O2 Pb), 2(Cl), 3(O)' _chemical_formula_sum 'C54 H68 Cl3 N11 O7 Pb2' _chemical_formula_weight 1503.92 _space_group_crystal_system orthorhombic _space_group_IT_number 60 _space_group_name_Hall '-P 2n 2ab' _space_group_name_H-M_alt 'P b c n' _symmetry_space_group_name_Hall '-P 2n 2ab' _symmetry_space_group_name_H-M 'P b c n' _atom_sites_solution_hydrogens mixed _atom_sites_solution_primary direct _audit_creation_date 2017-01-18 _audit_creation_method ; Olex2 1.2 (compiled 2017.01.04 svn.r3372 for OlexSys, GUI svn.r5289) ; _audit_update_record ; 2017-01-22 deposited with the CCDC. 2017-04-20 downloaded from the CCDC. ; _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 13.1619(4) _cell_length_b 13.0751(4) _cell_length_c 33.1703(10) _cell_measurement_reflns_used 1350 _cell_measurement_temperature 120.00(10) _cell_measurement_theta_max 28.3720 _cell_measurement_theta_min 3.7510 _cell_volume 5708.4(3) _computing_cell_refinement 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_collection 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_data_reduction 'CrysAlisPro 1.171.38.43f (Rigaku OD, 2015)' _computing_molecular_graphics 'Olex2 (Dolomanov et al., 2009)' _computing_publication_material 'Olex2 (Dolomanov et al., 2009)' _computing_structure_refinement 'ShelXL (Sheldrick, 2015)' _computing_structure_solution 'SIR2004 (Burla et al., 2007)' _diffrn_ambient_environment N~2~ _diffrn_ambient_temperature 120.00(10) _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 16.0267 _diffrn_detector_type Sapphire3 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _diffrn_measurement_details ; List of Runs (angles in degrees, time in seconds): # Type Start End Width t~exp~ \w \q \k \f Frames #-------------------------------------------------------------------------- 1 \w -36.00 1.00 1.00 46.00 -- -20.96 -19.00 -90.00 37 ; _diffrn_measurement_device 'four-circle diffractometer' _diffrn_measurement_device_type 'SuperNova, Single source at offset, Sapphire3' _diffrn_measurement_method '\w scans' _diffrn_orient_matrix_type 'CrysAlisPro convention (1999,Acta A55,543-557)' _diffrn_orient_matrix_UB_11 0.0206898000 _diffrn_orient_matrix_UB_12 -0.0056338000 _diffrn_orient_matrix_UB_13 0.0123664000 _diffrn_orient_matrix_UB_21 -0.0049056000 _diffrn_orient_matrix_UB_22 -0.0004117000 _diffrn_orient_matrix_UB_23 0.0527593000 _diffrn_orient_matrix_UB_31 -0.0021361000 _diffrn_orient_matrix_UB_32 -0.0535504000 _diffrn_orient_matrix_UB_33 -0.0017330000 _diffrn_radiation_monochromator mirror _diffrn_radiation_probe x-ray _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0405 _diffrn_reflns_av_unetI/netI 0.0513 _diffrn_reflns_Laue_measured_fraction_full 0.996 _diffrn_reflns_Laue_measured_fraction_max 0.996 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_limit_l_min -39 _diffrn_reflns_number 13519 _diffrn_reflns_point_group_measured_fraction_full 0.996 _diffrn_reflns_point_group_measured_fraction_max 0.996 _diffrn_reflns_theta_full 25.000 _diffrn_reflns_theta_max 25.000 _diffrn_reflns_theta_min 3.295 _diffrn_source 'micro-focus sealed X-ray tube' _diffrn_source_type 'SuperNova (Mo) X-ray Source' _exptl_absorpt_coefficient_mu 6.092 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_T_min 0.93098 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; CrysAlisPro 1.171.38.43f (Rigaku Oxford Diffraction, 2015) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_crystal_colour COLORLESS _exptl_crystal_density_diffrn 1.750 _exptl_crystal_description BLOCK _exptl_crystal_F_000 2960 _exptl_crystal_preparation ', Luminescent' _exptl_crystal_recrystallization_method 'Re-crystallisation from solvent: water' _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.1 _refine_diff_density_max 1.533 _refine_diff_density_min -1.827 _refine_diff_density_rms 0.166 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.368 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 445 _refine_ls_number_reflns 5006 _refine_ls_number_restraints 104 _refine_ls_restrained_S_all 1.362 _refine_ls_R_factor_all 0.0765 _refine_ls_R_factor_gt 0.0651 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+104.1935P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1313 _refine_ls_wR_factor_ref 0.1350 _reflns_Friedel_coverage 0.000 _reflns_number_gt 4305 _reflns_number_total 5006 _reflns_threshold_expression 'I > 2\s(I)' _iucr_refine_instructions_details ; TITL begopb_a.res in Pbcn begopb.res created by SHELXL-2016/6 at 14:08:08 on 18-Jan-2017 REM Old TITL bego pb in Pnma REM SHELXT solution in Pbcn REM R1 0.120, Rweak 0.011, Alpha 0.082, Orientation a'=b, b'=c, c'=a REM Formula found by SHELXT: C39 N10 O2N Pb CELL 0.71073 13.1619 13.0751 33.1703 90 90 90 ZERR 4 0.0004 0.0004 0.001 0 0 0 LATT 1 SYMM 0.5-X,0.5-Y,0.5+Z SYMM -X,+Y,0.5-Z SYMM 0.5+X,0.5-Y,-Z SFAC C H Cl N O Pb UNIT 216 272 12 44 28 8 DFIX 1.87 0.01 H1d O2 DFIX 2.27 0.01 H1c Cl1 DFIX 1.89 0.01 H1c O2N DELU O1 Pb1 DELU C8 C9B DELU C22 C23 DELU C21 C22 DELU O1N C18 C19 DELU 0.001 0.001 Pb1 O1N SIMU 0.02 0.04 1.7 C9B C8 ISOR 0.01 0.1 N4A N4B C10B C10A C9B C9A ISOR 0.008 0.08 C10B ISOR 0.01 0.1 C11A C11B ISOR 0.01 0.1 C23 C24 C16 C17 C8 ISOR 0.01 0.02 O1N ISOR 0.01 0.01 C12B C9B L.S. 10 PLAN 20 BIND N4A Pb1 BIND O1 Pb1 BIND O1N Pb1 FREE O1N O2N BOND $H LIST 6 fmap 2 acta 50 OMIT -3 50 OMIT 2 0 10 OMIT 2 2 2 OMIT 3 2 11 OMIT 1 3 5 OMIT 3 4 11 OMIT 6 1 20 REM REM REM WGHT 0.000000 104.193497 FVAR 0.17626 PB1 6 0.337342 0.447997 0.621001 11.00000 0.01806 0.01812 = 0.02436 -0.00071 -0.00108 0.00289 PART 2 CL1 3 0.225516 0.506816 0.548895 10.50000 0.03597 0.03524 = 0.05178 -0.00214 -0.01437 0.00567 PART 0 PART 1 CL2B 3 0.079957 0.179497 0.690630 10.50000 0.03793 0.03318 = 0.03112 0.00558 -0.00727 -0.00626 PART 0 N1 4 0.454783 0.399970 0.563839 11.00000 0.02298 0.00968 = 0.02064 0.00582 -0.00197 0.00112 PART 2 CL2A 3 0.119828 0.195205 0.655220 10.50000 0.04499 0.04105 = 0.08825 -0.00407 0.01196 -0.01621 PART 0 N2 4 0.528351 0.506030 0.628992 11.00000 0.02764 0.04233 = 0.05016 -0.02377 0.00782 -0.00930 AFIX 13 H2 2 0.529019 0.569314 0.644821 11.00000 -1.20000 AFIX 0 N5 4 0.309578 0.272451 0.592405 11.00000 0.02653 0.01936 = 0.02624 -0.00595 -0.00115 -0.00931 PART 1 AFIX 13 H5A 2 0.235811 0.263573 0.594371 10.50000 -1.20000 AFIX 13 PART 0 PART 2 H5B 2 0.240946 0.247887 0.598528 10.50000 -1.20000 AFIX 0 PART 0 C2 1 0.425440 0.327315 0.538586 11.00000 0.02588 0.01366 = 0.03566 0.00491 -0.00729 0.00119 C18 1 0.293991 0.715025 0.825000 11.00000 0.02792 0.02341 = 0.03639 0.00432 -0.00383 0.01258 AFIX 23 H18A 2 0.366483 0.704691 0.821661 11.00000 -1.20000 H18B 2 0.275550 0.781017 0.813822 11.00000 -1.20000 AFIX 0 C3 1 0.481604 0.306578 0.504641 11.00000 0.03803 0.01856 = 0.02288 -0.00176 0.00148 0.00659 AFIX 43 H3 2 0.460664 0.255767 0.486868 11.00000 -1.20000 AFIX 0 N3 4 0.436700 0.317976 0.664549 11.00000 0.02090 0.03752 = 0.01764 -0.00257 0.00103 0.01256 C13 1 0.318602 0.367201 0.720708 11.00000 0.02029 0.02137 = 0.02530 0.00130 0.00599 0.00082 PART 2 AFIX 23 H13C 2 0.278161 0.307692 0.713822 10.50000 -1.20000 H13D 2 0.315482 0.377089 0.749664 10.50000 -1.20000 AFIX 23 PART 0 PART 1 H13A 2 0.294665 0.346848 0.747177 10.50000 -1.20000 H13B 2 0.363755 0.425286 0.723858 10.50000 -1.20000 AFIX 0 PART 0 C6 1 0.541085 0.452515 0.557657 11.00000 0.01856 0.02218 = 0.03085 0.00438 -0.00324 0.00899 C1 1 0.327633 0.272766 0.549010 11.00000 0.03199 0.01991 = 0.03256 -0.00569 -0.00007 0.00311 AFIX 23 H1A 2 0.271367 0.306373 0.535548 11.00000 -1.20000 H1B 2 0.330913 0.202838 0.539332 11.00000 -1.20000 AFIX 0 C14 1 0.176436 0.485206 0.710041 11.00000 0.03055 0.03744 = 0.07415 -0.00925 -0.00403 0.00317 PART 2 AFIX 23 H14C 2 0.131360 0.427391 0.706058 10.50000 -1.20000 H14D 2 0.154079 0.540604 0.692732 10.50000 -1.20000 AFIX 23 PART 0 PART 1 H14A 2 0.106149 0.476066 0.702021 10.50000 -1.20000 H14B 2 0.201716 0.543269 0.694852 10.50000 -1.20000 AFIX 0 PART 0 C16 1 0.232595 0.601862 0.764962 11.00000 0.02871 0.01646 = 0.02907 0.00206 0.00291 0.01107 AFIX 43 H16 2 0.270115 0.638318 0.746043 11.00000 -1.20000 AFIX 0 C7 1 0.568400 0.529829 0.588715 11.00000 0.02612 0.01484 = 0.05391 0.00707 0.00022 -0.00580 AFIX 23 H7A 2 0.641827 0.534817 0.590269 11.00000 -1.20000 H7B 2 0.542587 0.595995 0.580349 11.00000 -1.20000 AFIX 0 C8 1 0.586459 0.431023 0.650568 11.00000 0.03518 0.07268 = 0.04240 0.01459 -0.00558 -0.01060 PART 2 AFIX 23 H8BC 2 0.654029 0.429072 0.638919 10.50000 -1.20000 H8BD 2 0.593577 0.454314 0.678188 10.50000 -1.20000 AFIX 23 PART 0 PART 1 H8AA 2 0.632080 0.467900 0.668348 10.50000 -1.20000 H8AB 2 0.628604 0.395956 0.630961 10.50000 -1.20000 AFIX 0 PART 0 C5 1 0.600102 0.434744 0.523715 11.00000 0.02336 0.03398 = 0.04220 0.01350 0.00750 0.00654 AFIX 43 H5 2 0.659315 0.471842 0.519219 11.00000 -1.20000 AFIX 0 C17 1 0.234340 0.630011 0.805332 11.00000 0.02801 0.02301 = 0.03275 0.00544 0.00138 0.01417 C23 1 0.153152 0.606201 0.910459 11.00000 0.04021 0.06481 = 0.04977 0.02314 0.00842 0.02211 AFIX 43 H23 2 0.106055 0.553966 0.914052 11.00000 -1.20000 AFIX 0 C15 1 0.173966 0.518364 0.753149 11.00000 0.02068 0.02718 = 0.04724 -0.00031 -0.00370 0.01417 PART 1 O2 5 0.083975 0.232989 0.599564 10.50000 0.03051 0.05437 = 0.04426 -0.02650 0.01215 -0.01629 PART 0 PART 2 N4B 4 0.280041 0.456628 0.700127 10.50000 0.01592 0.01943 = 0.01487 -0.00041 0.00158 0.00470 AFIX 13 H4B 2 0.320836 0.512768 0.711133 10.50000 -1.20000 AFIX 0 PART 0 C26 1 0.116054 0.498751 0.821079 11.00000 0.02781 0.02985 = 0.07148 0.02049 0.02392 0.01398 AFIX 43 H26 2 0.075703 0.464577 0.839741 11.00000 -1.20000 AFIX 0 C24 1 0.193331 0.626279 0.872627 11.00000 0.02905 0.03908 = 0.02880 0.01471 0.00154 0.01829 C25 1 0.175257 0.578983 0.833318 11.00000 0.02783 0.03271 = 0.03704 0.01236 0.00598 0.02080 C4 1 0.569071 0.361250 0.496983 11.00000 0.04608 0.02401 = 0.02514 0.00757 0.01048 0.01420 AFIX 43 H4 2 0.606756 0.348318 0.473821 11.00000 -1.20000 AFIX 0 C27 1 0.115759 0.468435 0.781631 11.00000 0.01605 0.01947 = 0.09045 -0.00813 -0.00352 0.00377 AFIX 43 H27 2 0.075686 0.413271 0.773859 11.00000 -1.20000 AFIX 0 C19 1 0.263939 0.707575 0.868620 11.00000 0.02815 0.04323 = 0.02726 0.00699 0.00355 0.02192 PART 1 N4A 4 0.231693 0.395069 0.694731 10.50000 0.02699 0.02159 = 0.02567 0.00548 -0.00117 0.01258 AFIX 13 H4A 2 0.185911 0.336865 0.690671 10.50000 -1.20000 AFIX 0 PART 0 C22 1 0.184877 0.666176 0.943240 11.00000 0.05319 0.11889 = 0.02940 0.01253 0.00969 0.05734 AFIX 43 H22 2 0.160024 0.651398 0.968831 11.00000 -1.20000 AFIX 0 C20 1 0.291395 0.764861 0.901104 11.00000 0.03934 0.07581 = 0.03094 -0.01456 -0.01246 0.03635 AFIX 43 H20 2 0.337880 0.817910 0.898170 11.00000 -1.20000 AFIX 0 PART 2 O3 5 0.004477 0.075556 0.727846 10.50000 0.04130 0.01953 = 0.09391 -0.02015 -0.01794 0.01576 C12B 1 0.430019 0.351419 0.707190 10.50000 0.01647 0.02147 = 0.01749 0.00162 -0.00487 0.00641 AFIX 23 H12A 2 0.467067 0.415010 0.710464 10.50000 -1.20000 H12B 2 0.461707 0.300403 0.724298 10.50000 -1.20000 AFIX 0 PART 0 C21 1 0.249630 0.743709 0.938693 11.00000 0.05494 0.11327 = 0.03376 -0.02372 -0.01126 0.05483 AFIX 43 H21 2 0.266968 0.783877 0.960785 11.00000 -1.20000 AFIX 0 PART 1 C12A 1 0.375758 0.277120 0.700291 10.50000 0.04019 0.02762 = 0.01728 0.00339 0.00861 0.01551 AFIX 23 H12C 2 0.421088 0.244948 0.719547 10.50000 -1.20000 H12D 2 0.327405 0.226248 0.691076 10.50000 -1.20000 AFIX 0 PART 0 PART 2 C9B 1 0.552521 0.340684 0.651364 10.50000 0.02870 0.03756 = 0.01674 0.00648 -0.00596 0.01597 AFIX 23 H9BA 2 0.596002 0.301786 0.669319 10.50000 -1.20000 H9BB 2 0.561616 0.312336 0.624583 10.50000 -1.20000 AFIX 0 PART 0 PART 1 C9A 1 0.532184 0.345506 0.676931 10.50000 0.03183 0.02959 = 0.03353 -0.00733 -0.00309 0.00319 AFIX 23 H9AA 2 0.574736 0.284935 0.676949 10.50000 -1.20000 H9AB 2 0.527900 0.369750 0.704516 10.50000 -1.20000 AFIX 0 C10A 1 0.441261 0.217996 0.636976 10.50000 0.03216 0.02906 = 0.02556 0.00085 0.00060 0.00562 AFIX 23 H10A 2 0.494665 0.226954 0.617136 10.50000 -1.20000 H10B 2 0.459911 0.160282 0.653794 10.50000 -1.20000 AFIX 0 PART 0 PART 2 C10B 1 0.407538 0.224311 0.656435 10.50000 0.01846 0.01470 = 0.01536 0.01181 0.00169 0.00230 AFIX 23 H10C 2 0.343184 0.212286 0.669875 10.50000 -1.20000 H10D 2 0.456710 0.177507 0.668015 10.50000 -1.20000 AFIX 6 PART 0 PART 1 O1 5 0.108511 0.421737 0.617612 10.50000 0.03239 0.04431 = 0.09837 -0.00215 -0.00729 0.00047 H1C 2 0.113927 0.434163 0.592582 10.50000 -1.50000 H1D 2 0.077835 0.365150 0.620980 10.50000 -1.50000 AFIX 0 C11A 1 0.347190 0.193145 0.615911 10.50000 0.02459 0.03888 = 0.02284 0.00039 -0.00143 -0.00291 AFIX 23 H11A 2 0.358974 0.134180 0.598792 10.50000 -1.20000 H11B 2 0.296122 0.174261 0.635638 10.50000 -1.20000 AFIX 0 PART 0 PART 2 C11B 1 0.395126 0.198292 0.612751 10.50000 0.02675 0.02166 = 0.03105 -0.00116 -0.00182 0.00858 AFIX 23 H11C 2 0.374522 0.127392 0.610057 10.50000 -1.20000 H11D 2 0.459450 0.206957 0.598894 10.50000 -1.20000 AFIX 0 PART 0 PART 1 O3N 5 0.137093 0.557000 0.493717 10.50000 0.07631 0.04298 = 0.06759 -0.01359 0.01089 0.00830 PART 0 PART 2 O4 5 0.005711 0.417387 0.567899 10.50000 0.07471 0.05683 = 0.08435 -0.00494 -0.00253 -0.00471 PART 0 PART 1 N1AA 4 0.147345 0.499286 0.524686 10.50000 0.07852 0.05256 = 0.02636 -0.01630 0.00338 -0.02529 O2N 5 0.086740 0.431856 0.536629 10.50000 0.08871 0.06941 = 0.08696 -0.02276 -0.00476 -0.04109 O1N 5 0.202028 0.492188 0.546963 10.50000 0.03638 0.03932 = 0.03386 -0.00036 -0.01448 0.00409 HKLF 4 REM begopb_a.res in Pbcn REM R1 = 0.0651 for 4305 Fo > 4sig(Fo) and 0.0765 for all 5006 data REM 445 parameters refined using 104 restraints END WGHT 0.0000 104.2036 REM Highest difference peak 1.533, deepest hole -1.827, 1-sigma level 0.166 Q1 1 0.1244 0.1874 0.6182 11.00000 0.05 1.53 Q2 1 0.3336 0.4007 0.5998 11.00000 0.05 1.25 Q3 1 0.3368 0.4967 0.5981 11.00000 0.05 0.96 Q4 1 0.0128 0.5557 0.8606 11.00000 0.05 0.95 Q5 1 0.3366 0.3750 0.6410 11.00000 0.05 0.87 Q6 1 0.4016 0.4217 0.6207 11.00000 0.05 0.85 Q7 1 0.0345 0.2609 0.6588 11.00000 0.05 0.70 Q8 1 0.1131 0.4527 0.5769 11.00000 0.05 0.68 Q9 1 0.0675 0.5571 0.5337 11.00000 0.05 0.68 Q10 1 0.0089 0.5009 0.8685 11.00000 0.05 0.67 Q11 1 0.3195 0.5044 0.6515 11.00000 0.05 0.65 Q12 1 0.5944 0.3820 0.6458 11.00000 0.05 0.63 Q13 1 0.0597 0.5654 0.4790 11.00000 0.05 0.63 Q14 1 0.1197 0.4225 0.6816 11.00000 0.05 0.61 Q15 1 0.3357 0.2479 0.6265 11.00000 0.05 0.61 Q16 1 0.4580 0.4860 0.6952 11.00000 0.05 0.61 Q17 1 0.0597 0.4218 0.6201 11.00000 0.05 0.60 Q18 1 0.1458 0.1381 0.6801 11.00000 0.05 0.59 Q19 1 0.1989 0.2085 0.6178 11.00000 0.05 0.59 Q20 1 0.1682 0.6513 0.9179 11.00000 0.05 0.56 REM The information below was added by Olex2. REM REM R1 = 0.0651 for 4305 Fo > 4sig(Fo) and 0.0765 for all 18595 data REM n/a parameters refined using n/a restraints REM Highest difference peak 1.53, deepest hole -1.83 REM Mean Shift 0, Max Shift -0.003. REM +++ Tabular Listing of Refinement Information +++ REM R1_all = 0.0765 REM R1_gt = 0.0651 REM wR_ref = 0.1350 REM GOOF = 1.368 REM Shift_max = -0.003 REM Shift_mean = 0 REM Reflections_all = 18595 REM Reflections_gt = 4305 REM Parameters = n/a REM Hole = -1.83 REM Peak = 1.53 REM Flack = n/a ; _cod_data_source_file c7dt00680b2.cif _cod_data_source_block begopb _cod_database_code 7042741 _shelx_shelxl_version_number 2016/6 _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. ; _cell_oxdiff_angle_alpha 90.028(7) _cell_oxdiff_angle_beta 90.037(9) _cell_oxdiff_angle_gamma 89.992(3) _cell_oxdiff_length_a 33.1908(15) _cell_oxdiff_length_b 13.1724(3) _cell_oxdiff_length_c 13.083(3) _cell_oxdiff_measurement_reflns_used 1350 _cell_oxdiff_volume 5720(2) _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups, All C(H,H,H,H) groups, All N(H) groups, All N(H,H) groups At 1.5 times of: All O(H,H) groups 2. Restrained distances H1d-O2 1.87 with sigma of 0.01 H1c-Cl1 2.27 with sigma of 0.01 H1c-O4 1.89 with sigma of 0.01 3. Rigid bond restraints O1, Pb01 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C8, C9B with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C22, C23 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 C21, C22 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 O13, C18, C19 with sigma for 1-2 distances of 0.01 and sigma for 1-3 distances of 0.01 Pb01, O13 with sigma for 1-2 distances of 0.001 and sigma for 1-3 distances of 0.001 4. Uiso/Uaniso restraints and constraints C9B \\sim C8: within 1.7A with sigma of 0.02 and sigma for terminal atoms of 0.04 Uanis(N4A) \\sim Ueq, Uanis(N4B) \\sim Ueq, Uanis(C10B) \\sim Ueq, Uanis(C10A) \\sim Ueq, Uanis(C9B) \\sim Ueq, Uanis(C9A) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1 Uanis(C10B) \\sim Ueq: with sigma of 0.008 and sigma for terminal atoms of 0.08 Uanis(C11A) \\sim Ueq, Uanis(C11B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1 Uanis(C23) \\sim Ueq, Uanis(C24) \\sim Ueq, Uanis(C16) \\sim Ueq, Uanis(C17) \\sim Ueq, Uanis(C8) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.1 Uanis(O13) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.02 Uanis(C12B) \\sim Ueq, Uanis(C9B) \\sim Ueq: with sigma of 0.01 and sigma for terminal atoms of 0.01 5. Others Fixed Sof: Cl1(0.5) Cl2B(0.5) Cl2A(0.5) H5a(0.5) H5b(0.5) H13c(0.5) H13d(0.5) H13a(0.5) H13b(0.5) H14c(0.5) H14d(0.5) H14a(0.5) H14b(0.5) H8bc(0.5) H8bd(0.5) H8aa(0.5) H8ab(0.5) O2(0.5) N4B(0.5) H4B(0.5) N4A(0.5) H4A(0.5) O3(0.5) C12B(0.5) H12a(0.5) H12b(0.5) C12A(0.5) H12c(0.5) H12d(0.5) C9B(0.5) H9Ba(0.5) H9Bb(0.5) C9A(0.5) H9Aa(0.5) H9Ab(0.5) C10A(0.5) H10a(0.5) H10b(0.5) C10B(0.5) H10c(0.5) H10d(0.5) O1(0.5) H1c(0.5) H1d(0.5) C11A(0.5) H11a(0.5) H11b(0.5) C11B(0.5) H11c(0.5) H11d(0.5) O2AA(0.5) O0AA(0.5) N1AA(0.5) O4(0.5) O13(0.5) 6.a Free rotating group: O1(H1c,H1d) 6.b Ternary CH refined with riding coordinates: N2(H2), N5(H5a), N5(H5b), N4B(H4B), N4A(H4A) 6.c Secondary CH2 refined with riding coordinates: C18(H18a,H18b), C13(H13c,H13d), C13(H13a,H13b), C1(H1a,H1b), C14(H14c,H14d), C14(H14a,H14b), C7(H7a,H7b), C8(H8bc,H8bd), C8(H8aa,H8ab), C12B(H12a,H12b), C12A(H12c,H12d), C9B(H9Ba,H9Bb), C9A(H9Aa,H9Ab), C10A(H10a,H10b), C10B(H10c, H10d), C11A(H11a,H11b), C11B(H11c,H11d) 6.d Aromatic/amide H refined with riding coordinates: C3(H3), C16(H16), C5(H5), C23(H23), C26(H26), C4(H4), C27(H27), C22(H22), C20(H20), C21(H21) ; _olex2_submission_special_instructions 'No special instructions were received' loop_ _space_group_symop_operation_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, 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 0.33734(3) 0.44800(3) 0.62100(2) 0.02018(14) Uani 1 1 d . U . . . Cl1 Cl 0.2255(10) 0.5068(13) 0.5489(6) 0.041(3) Uani 0.5 1 d D . P A 2 Cl2B Cl 0.0800(5) 0.1795(5) 0.6906(2) 0.0341(15) Uani 0.5 1 d . . P B 1 N1 N 0.4548(7) 0.4000(7) 0.5638(3) 0.018(2) Uani 1 1 d . . . . . Cl2A Cl 0.1198(6) 0.1952(6) 0.6552(3) 0.058(2) Uani 0.5 1 d . . P C 2 N2 N 0.5284(7) 0.5060(9) 0.6290(4) 0.040(3) Uani 1 1 d . . . . . H2 H 0.529019 0.569314 0.644821 0.048 Uiso 1 1 calc R . . . . N5 N 0.3096(7) 0.2725(7) 0.5924(3) 0.024(2) Uani 1 1 d . . . . . H5A H 0.235811 0.263573 0.594371 0.029 Uiso 0.5 1 calc R . P D 1 H5B H 0.240946 0.247887 0.598528 0.029 Uiso 0.5 1 calc R . P E 2 C2 C 0.4254(9) 0.3273(9) 0.5386(4) 0.025(3) Uani 1 1 d . . . . . C18 C 0.2940(9) 0.7150(10) 0.8250(4) 0.029(3) Uani 1 1 d . U . . . H18A H 0.366483 0.704691 0.821661 0.035 Uiso 1 1 calc R . . . . H18B H 0.275550 0.781017 0.813822 0.035 Uiso 1 1 calc R . . . . C3 C 0.4816(9) 0.3066(9) 0.5046(4) 0.026(3) Uani 1 1 d . . . . . H3 H 0.460664 0.255767 0.486868 0.032 Uiso 1 1 calc R . . . . N3 N 0.4367(7) 0.3180(8) 0.6645(3) 0.025(2) Uani 1 1 d . . . . . C13 C 0.3186(8) 0.3672(9) 0.7207(3) 0.022(3) Uani 1 1 d . . . . . H13C H 0.278161 0.307692 0.713822 0.027 Uiso 0.5 1 calc R . P A 2 H13D H 0.315482 0.377089 0.749664 0.027 Uiso 0.5 1 calc R . P A 2 H13A H 0.294665 0.346848 0.747177 0.027 Uiso 0.5 1 calc R . P A 1 H13B H 0.363755 0.425286 0.723858 0.027 Uiso 0.5 1 calc R . P A 1 C6 C 0.5411(8) 0.4525(9) 0.5577(4) 0.024(3) Uani 1 1 d . . . . . C1 C 0.3276(9) 0.2728(9) 0.5490(4) 0.028(3) Uani 1 1 d . . . . . H1A H 0.271367 0.306373 0.535548 0.034 Uiso 1 1 calc R . . . . H1B H 0.330913 0.202838 0.539332 0.034 Uiso 1 1 calc R . . . . C14 C 0.1764(11) 0.4852(12) 0.7100(5) 0.047(4) Uani 1 1 d . . . . . H14C H 0.131360 0.427391 0.706058 0.057 Uiso 0.5 1 calc R . P A 2 H14D H 0.154079 0.540604 0.692732 0.057 Uiso 0.5 1 calc R . P A 2 H14A H 0.106149 0.476066 0.702021 0.057 Uiso 0.5 1 calc R . P A 1 H14B H 0.201716 0.543269 0.694852 0.057 Uiso 0.5 1 calc R . P A 1 C16 C 0.2326(9) 0.6019(9) 0.7650(4) 0.025(3) Uani 1 1 d . U . . . H16 H 0.270115 0.638318 0.746043 0.030 Uiso 1 1 calc R . . . . C7 C 0.5684(9) 0.5298(9) 0.5887(4) 0.032(3) Uani 1 1 d . . . . . H7A H 0.641827 0.534817 0.590269 0.038 Uiso 1 1 calc R . . . . H7B H 0.542587 0.595995 0.580349 0.038 Uiso 1 1 calc R . . . . C8 C 0.5865(11) 0.4310(13) 0.6506(5) 0.050(4) Uani 1 1 d . U . . . H8BC H 0.654029 0.429072 0.638919 0.060 Uiso 0.5 1 calc R . P F 2 H8BD H 0.593577 0.454314 0.678188 0.060 Uiso 0.5 1 calc R . P F 2 H8AA H 0.632080 0.467900 0.668348 0.060 Uiso 0.5 1 calc R . P G 1 H8AB H 0.628604 0.395956 0.630961 0.060 Uiso 0.5 1 calc R . P G 1 C5 C 0.6001(9) 0.4347(10) 0.5237(4) 0.033(3) Uani 1 1 d . . . . . H5 H 0.659315 0.471842 0.519219 0.040 Uiso 1 1 calc R . . . . C17 C 0.2343(9) 0.6300(9) 0.8053(4) 0.028(3) Uani 1 1 d . U . . . C23 C 0.1532(11) 0.6062(13) 0.9105(5) 0.052(4) Uani 1 1 d . U . . . H23 H 0.106055 0.553966 0.914052 0.062 Uiso 1 1 calc R . . . . C15 C 0.1740(9) 0.5184(10) 0.7531(4) 0.032(3) Uani 1 1 d . . . . . O2 O 0.0840(13) 0.2330(16) 0.5996(6) 0.043(5) Uani 0.5 1 d D . P H 1 N4B N 0.2800(13) 0.4566(15) 0.7001(5) 0.017(4) Uani 0.5 1 d . U P A 2 H4B H 0.320836 0.512768 0.711133 0.020 Uiso 0.5 1 calc R . P A 2 C26 C 0.1161(10) 0.4988(11) 0.8211(5) 0.043(4) Uani 1 1 d . . . . . H26 H 0.075703 0.464577 0.839741 0.052 Uiso 1 1 calc R . . . . C24 C 0.1933(9) 0.6263(10) 0.8726(4) 0.032(3) Uani 1 1 d . U . . . C25 C 0.1753(9) 0.5790(10) 0.8333(4) 0.033(3) Uani 1 1 d . . . . . C4 C 0.5691(10) 0.3613(10) 0.4970(4) 0.032(3) Uani 1 1 d . . . . . H4 H 0.606756 0.348318 0.473821 0.038 Uiso 1 1 calc R . . . . C27 C 0.1158(9) 0.4684(10) 0.7816(5) 0.042(4) Uani 1 1 d . . . . . H27 H 0.075686 0.413271 0.773859 0.050 Uiso 1 1 calc R . . . . C19 C 0.2639(9) 0.7076(11) 0.8686(4) 0.033(3) Uani 1 1 d . U . . . N4A N 0.2317(15) 0.3951(16) 0.6947(6) 0.025(5) Uani 0.5 1 d . U P A 1 H4A H 0.185911 0.336865 0.690671 0.030 Uiso 0.5 1 calc R . P A 1 C22 C 0.1849(13) 0.6662(17) 0.9432(5) 0.067(5) Uani 1 1 d . U . . . H22 H 0.160024 0.651398 0.968831 0.081 Uiso 1 1 calc R . . . . C20 C 0.2914(11) 0.7649(14) 0.9011(4) 0.049(4) Uani 1 1 d . . . . . H20 H 0.337880 0.817910 0.898170 0.058 Uiso 1 1 calc R . . . . O3 O 0.0045(15) 0.0756(13) 0.7278(7) 0.052(6) Uani 0.5 1 d . . P I 2 C12B C 0.4300(16) 0.3514(18) 0.7072(6) 0.018(5) Uani 0.5 1 d . U P A 2 H12A H 0.467067 0.415010 0.710464 0.022 Uiso 0.5 1 calc R . P A 2 H12B H 0.461707 0.300403 0.724298 0.022 Uiso 0.5 1 calc R . P A 2 C21 C 0.2496(14) 0.7437(17) 0.9387(5) 0.067(5) Uani 1 1 d . U . . . H21 H 0.266968 0.783877 0.960785 0.081 Uiso 1 1 calc R . . . . C12A C 0.376(2) 0.277(2) 0.7003(7) 0.028(6) Uani 0.5 1 d . . P A 1 H12C H 0.421088 0.244948 0.719547 0.034 Uiso 0.5 1 calc R . P A 1 H12D H 0.327405 0.226248 0.691076 0.034 Uiso 0.5 1 calc R . P A 1 C9B C 0.5525(18) 0.341(2) 0.6514(8) 0.028(5) Uani 0.5 1 d . U P A 2 H9BA H 0.596002 0.301786 0.669319 0.033 Uiso 0.5 1 calc R . P A 2 H9BB H 0.561616 0.312336 0.624583 0.033 Uiso 0.5 1 calc R . P A 2 C9A C 0.5322(19) 0.346(2) 0.6769(9) 0.032(6) Uani 0.5 1 d . U P A 1 H9AA H 0.574736 0.284935 0.676949 0.038 Uiso 0.5 1 calc R . P A 1 H9AB H 0.527900 0.369750 0.704516 0.038 Uiso 0.5 1 calc R . P A 1 C10A C 0.441(2) 0.218(2) 0.6370(9) 0.029(6) Uani 0.5 1 d . U P A 1 H10A H 0.494665 0.226954 0.617136 0.035 Uiso 0.5 1 calc R . P A 1 H10B H 0.459911 0.160282 0.653794 0.035 Uiso 0.5 1 calc R . P A 1 C10B C 0.4075(18) 0.2243(17) 0.6564(7) 0.016(5) Uani 0.5 1 d . U P A 2 H10C H 0.343184 0.212286 0.669875 0.019 Uiso 0.5 1 calc R . P A 2 H10D H 0.456710 0.177507 0.668015 0.019 Uiso 0.5 1 calc R . P A 2 O1 O 0.1085(15) 0.4217(16) 0.6176(7) 0.058(6) Uani 0.5 1 d . U P A 1 H1C H 0.113927 0.434163 0.592582 0.088 Uiso 0.5 1 d DG . P A 1 H1D H 0.077835 0.365150 0.620980 0.088 Uiso 0.5 1 d DG . P A 1 C11A C 0.347(2) 0.193(2) 0.6159(8) 0.029(6) Uani 0.5 1 d . U P A 1 H11A H 0.358974 0.134180 0.598792 0.035 Uiso 0.5 1 calc R . P A 1 H11B H 0.296122 0.174261 0.635638 0.035 Uiso 0.5 1 calc R . P A 1 C11B C 0.395(2) 0.198(2) 0.6128(9) 0.026(6) Uani 0.5 1 d . U P A 2 H11C H 0.374522 0.127392 0.610057 0.032 Uiso 0.5 1 calc R . P A 2 H11D H 0.459450 0.206957 0.598894 0.032 Uiso 0.5 1 calc R . P A 2 O3N O 0.1371(18) 0.5570(17) 0.4937(7) 0.062(6) Uani 0.5 1 d . . P A 1 O4 O 0.006(2) 0.4174(18) 0.5679(8) 0.072(7) Uani 0.5 1 d . . P J 2 N1AA N 0.147(2) 0.499(2) 0.5247(7) 0.052(7) Uani 0.5 1 d . . P A 1 O2N O 0.087(2) 0.432(2) 0.5366(8) 0.082(8) Uani 0.5 1 d D . P A 1 O1N O 0.202(3) 0.492(4) 0.5470(17) 0.037(8) Uani 0.5 1 d . 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 0.0181(2) 0.0181(2) 0.0244(2) -0.0007(2) -0.00108(19) 0.00289(19) Cl1 0.036(6) 0.035(6) 0.052(6) -0.002(5) -0.014(5) 0.006(5) Cl2B 0.038(3) 0.033(4) 0.031(3) 0.006(3) -0.007(3) -0.006(3) N1 0.023(5) 0.010(4) 0.021(5) 0.006(4) -0.002(4) 0.001(4) Cl2A 0.045(4) 0.041(4) 0.088(7) -0.004(5) 0.012(4) -0.016(4) N2 0.028(6) 0.042(7) 0.050(7) -0.024(6) 0.008(5) -0.009(5) N5 0.027(5) 0.019(5) 0.026(5) -0.006(5) -0.001(4) -0.009(4) C2 0.026(6) 0.014(6) 0.036(7) 0.005(6) -0.007(5) 0.001(5) C18 0.028(6) 0.023(7) 0.036(6) 0.004(6) -0.004(6) 0.013(6) C3 0.038(7) 0.019(6) 0.023(6) -0.002(5) 0.001(6) 0.007(6) N3 0.021(5) 0.038(6) 0.018(5) -0.003(5) 0.001(4) 0.013(5) C13 0.020(6) 0.021(6) 0.025(6) 0.001(5) 0.006(5) 0.001(5) C6 0.019(5) 0.022(6) 0.031(6) 0.004(6) -0.003(5) 0.009(5) C1 0.032(7) 0.020(6) 0.033(7) -0.006(6) 0.000(6) 0.003(6) C14 0.031(8) 0.037(8) 0.074(11) -0.009(8) -0.004(7) 0.003(7) C16 0.029(6) 0.016(5) 0.029(6) 0.002(5) 0.003(5) 0.011(5) C7 0.026(6) 0.015(6) 0.054(8) 0.007(6) 0.000(6) -0.006(5) C8 0.035(6) 0.073(7) 0.042(6) 0.015(6) -0.006(5) -0.011(6) C5 0.023(6) 0.034(8) 0.042(8) 0.014(7) 0.007(6) 0.007(6) C17 0.028(5) 0.023(6) 0.033(6) 0.005(5) 0.001(5) 0.014(5) C23 0.040(7) 0.065(8) 0.050(7) 0.023(6) 0.008(6) 0.022(6) C15 0.021(6) 0.027(7) 0.047(8) 0.000(6) -0.004(6) 0.014(6) O2 0.031(10) 0.054(13) 0.044(12) -0.026(11) 0.012(9) -0.016(10) N4B 0.016(7) 0.019(8) 0.015(7) 0.000(7) 0.002(6) 0.005(7) C26 0.028(7) 0.030(8) 0.071(11) 0.020(8) 0.024(7) 0.014(6) C24 0.029(6) 0.039(6) 0.029(6) 0.015(5) 0.002(5) 0.018(5) C25 0.028(7) 0.033(8) 0.037(7) 0.012(6) 0.006(6) 0.021(6) C4 0.046(8) 0.024(7) 0.025(7) 0.008(6) 0.010(6) 0.014(6) C27 0.016(6) 0.019(7) 0.090(12) -0.008(8) -0.004(7) 0.004(5) C19 0.028(7) 0.043(8) 0.027(6) 0.007(7) 0.004(5) 0.022(6) N4A 0.027(8) 0.022(8) 0.026(8) 0.005(7) -0.001(7) 0.013(7) C22 0.053(10) 0.119(15) 0.029(7) 0.013(8) 0.010(7) 0.057(9) C20 0.039(8) 0.076(12) 0.031(8) -0.015(8) -0.012(6) 0.036(8) O3 0.041(11) 0.020(10) 0.094(16) -0.020(9) -0.018(13) 0.016(9) C12B 0.016(8) 0.021(9) 0.017(8) 0.002(7) -0.005(7) 0.006(7) C21 0.055(10) 0.113(15) 0.034(8) -0.024(11) -0.011(8) 0.055(9) C12A 0.040(14) 0.028(14) 0.017(12) 0.003(11) 0.009(11) 0.016(12) C9B 0.029(8) 0.038(8) 0.017(8) 0.006(8) -0.006(7) 0.016(7) C9A 0.032(9) 0.030(9) 0.034(9) -0.007(8) -0.003(8) 0.003(8) C10A 0.032(9) 0.029(10) 0.026(9) 0.001(8) 0.001(8) 0.006(8) C10B 0.018(8) 0.015(8) 0.015(8) 0.012(7) 0.002(6) 0.002(6) O1 0.032(8) 0.044(13) 0.098(18) -0.002(13) -0.007(12) 0.000(9) C11A 0.025(9) 0.039(10) 0.023(9) 0.000(8) -0.001(8) -0.003(9) C11B 0.027(10) 0.022(9) 0.031(10) -0.001(8) -0.002(9) 0.009(8) O3N 0.076(16) 0.043(13) 0.068(16) -0.014(13) 0.011(13) 0.008(13) O4 0.075(16) 0.057(16) 0.084(19) -0.005(14) -0.003(15) -0.005(14) N1AA 0.08(2) 0.053(18) 0.026(13) -0.016(14) 0.003(15) -0.025(17) O2N 0.089(19) 0.069(19) 0.09(2) -0.023(16) -0.005(16) -0.041(16) O1N 0.036(12) 0.039(13) 0.034(9) 0.000(9) -0.014(8) 0.004(9) 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' Cl Cl 0.1484 0.1585 '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 N1 Pb1 Cl1 76.0(4) N1 Pb1 N2 64.1(3) N1 Pb1 N3 86.9(3) N1 Pb1 N4B 154.2(4) N1 Pb1 N4A 150.2(4) N1 Pb1 O1 123.5(5) N1 Pb1 O1N 78.6(10) N2 Pb1 Cl1 119.2(4) N2 Pb1 N4B 98.9(5) N2 Pb1 N4A 116.2(5) N2 Pb1 O1 169.1(5) N2 Pb1 O1N 125.1(9) N5 Pb1 Cl1 81.8(4) N5 Pb1 N1 65.0(3) N5 Pb1 N2 116.1(3) N5 Pb1 N3 71.6(3) N5 Pb1 N4B 111.1(5) N5 Pb1 N4A 91.8(5) N5 Pb1 O1 74.8(5) N5 Pb1 O1N 77.7(9) N3 Pb1 Cl1 152.6(4) N3 Pb1 N2 69.6(4) N3 Pb1 N4B 68.3(4) N3 Pb1 N4A 67.3(4) N3 Pb1 O1 116.6(5) N3 Pb1 O1N 149.2(9) N4B Pb1 Cl1 129.7(5) N4A Pb1 O1 61.8(6) N4A Pb1 O1N 116.1(10) O1 Pb1 O1N 54.5(10) C2 N1 Pb1 118.3(7) C2 N1 C6 121.1(10) C6 N1 Pb1 120.3(8) Pb1 N2 H2 107.8 C7 N2 Pb1 108.1(8) C7 N2 H2 107.8 C8 N2 Pb1 111.2(8) C8 N2 H2 107.8 C8 N2 C7 114.0(11) Pb1 N5 H5A 103.1 Pb1 N5 H5B 110.8 C1 N5 Pb1 110.3(7) C1 N5 H5A 103.1 C1 N5 H5B 110.8 C1 N5 C11B 107.3(13) C11A N5 Pb1 114.8(13) C11A N5 H5A 103.1 C11A N5 C1 119.9(15) C11B N5 Pb1 106.7(12) C11B N5 H5B 110.8 N1 C2 C3 120.2(11) N1 C2 C1 116.2(11) C3 C2 C1 123.5(11) H18A C18 H18B 109.1 C17 C18 H18A 111.1 C17 C18 H18B 111.1 C19 C18 H18A 111.1 C19 C18 H18B 111.1 C19 C18 C17 103.4(11) C2 C3 H3 120.1 C2 C3 C4 119.9(12) C4 C3 H3 120.1 C12B N3 Pb1 108.0(10) C12B N3 C9B 105.1(14) C12A N3 Pb1 113.4(10) C12A N3 C10A 100.3(16) C9B N3 Pb1 101.9(10) C9A N3 Pb1 117.3(13) C9A N3 C12A 109.9(17) C9A N3 C10A 110.6(16) C10A N3 Pb1 103.7(11) C10B N3 Pb1 110.6(11) C10B N3 C12B 117.0(16) C10B N3 C9B 113.1(16) H13C C13 H13D 108.5 H13A C13 H13B 108.4 N4B C13 H13C 110.2 N4B C13 H13D 110.2 N4B C13 C12B 107.7(13) N4A C13 H13A 110.1 N4A C13 H13B 110.1 N4A C13 C12A 107.9(15) C12B C13 H13C 110.2 C12B C13 H13D 110.2 C12A C13 H13A 110.1 C12A C13 H13B 110.1 N1 C6 C7 116.5(10) N1 C6 C5 120.8(12) C5 C6 C7 122.7(11) N5 C1 C2 111.4(10) N5 C1 H1A 109.3 N5 C1 H1B 109.3 C2 C1 H1A 109.3 C2 C1 H1B 109.3 H1A C1 H1B 108.0 H14C C14 H14D 108.4 H14A C14 H14B 106.3 C15 C14 H14C 110.1 C15 C14 H14D 110.1 C15 C14 H14A 106.1 C15 C14 H14B 106.1 N4B C14 H14C 110.1 N4B C14 H14D 110.1 N4B C14 C15 108.2(13) N4A C14 H14A 106.1 N4A C14 H14B 106.1 N4A C14 C15 124.9(14) C17 C16 H16 120.4 C17 C16 C15 119.2(12) C15 C16 H16 120.4 N2 C7 C6 113.5(10) N2 C7 H7A 108.9 N2 C7 H7B 108.9 C6 C7 H7A 108.9 C6 C7 H7B 108.9 H7A C7 H7B 107.7 N2 C8 H8BC 107.9 N2 C8 H8BD 107.9 N2 C8 H8AA 107.1 N2 C8 H8AB 107.1 N2 C8 C9A 121.0(14) H8BC C8 H8BD 107.2 H8AA C8 H8AB 106.8 C9B C8 N2 117.5(16) C9B C8 H8BC 107.9 C9B C8 H8BD 107.9 C9A C8 H8AA 107.1 C9A C8 H8AB 107.1 C6 C5 H5 120.8 C4 C5 C6 118.4(12) C4 C5 H5 120.8 C16 C17 C18 128.4(12) C25 C17 C18 111.0(11) C25 C17 C16 120.7(12) C24 C23 H23 120.6 C24 C23 C22 118.8(17) C22 C23 H23 120.6 C16 C15 C14 119.0(12) C27 C15 C14 122.0(13) C27 C15 C16 119.0(13) Pb1 N4B H4B 103.7 C13 N4B Pb1 108.9(10) C13 N4B C14 115.5(15) C13 N4B H4B 103.7 C14 N4B Pb1 119.2(11) C14 N4B H4B 103.7 C25 C26 H26 119.7 C27 C26 H26 119.7 C27 C26 C25 120.5(13) C23 C24 C25 131.7(14) C23 C24 C19 118.5(14) C19 C24 C25 109.9(11) C17 C25 C24 107.6(12) C26 C25 C17 119.4(13) C26 C25 C24 132.9(13) C3 C4 H4 120.2 C5 C4 C3 119.6(12) C5 C4 H4 120.2 C15 C27 H27 119.5 C26 C27 C15 121.1(13) C26 C27 H27 119.5 C24 C19 C18 108.1(12) C20 C19 C18 131.0(14) C20 C19 C24 120.8(13) Pb1 N4A H4A 111.4 C13 N4A Pb1 100.3(10) C13 N4A H4A 111.4 C14 N4A Pb1 109.7(12) C14 N4A C13 112.2(16) C14 N4A H4A 111.4 C23 C22 H22 119.1 C21 C22 C23 121.8(16) C21 C22 H22 119.1 C19 C20 H20 120.2 C19 C20 C21 119.7(18) C21 C20 H20 120.2 N3 C12B C13 111.8(14) N3 C12B H12A 109.2 N3 C12B H12B 109.2 C13 C12B H12A 109.2 C13 C12B H12B 109.2 H12A C12B H12B 107.9 C22 C21 C20 120.4(17) C22 C21 H21 119.8 C20 C21 H21 119.8 N3 C12A C13 109.1(16) N3 C12A H12C 109.9 N3 C12A H12D 109.9 C13 C12A H12C 109.9 C13 C12A H12D 109.9 H12C C12A H12D 108.3 N3 C9B H9BA 107.1 N3 C9B H9BB 107.1 C8 C9B N3 121(2) C8 C9B H9BA 107.1 C8 C9B H9BB 107.1 H9BA C9B H9BB 106.8 N3 C9A C8 115.6(19) N3 C9A H9AA 108.4 N3 C9A H9AB 108.4 C8 C9A H9AA 108.4 C8 C9A H9AB 108.4 H9AA C9A H9AB 107.4 N3 C10A H10A 108.5 N3 C10A H10B 108.5 H10A C10A H10B 107.5 C11A C10A N3 115(2) C11A C10A H10A 108.5 C11A C10A H10B 108.5 N3 C10B H10C 108.2 N3 C10B H10D 108.2 N3 C10B C11B 116(2) H10C C10B H10D 107.4 C11B C10B H10C 108.2 C11B C10B H10D 108.2 Pb1 O1 H1C 86.1 Pb1 O1 H1D 124.4 H1C O1 H1D 109.6 N5 C11A C10A 114(2) N5 C11A H11A 108.8 N5 C11A H11B 108.8 C10A C11A H11A 108.8 C10A C11A H11B 108.8 H11A C11A H11B 107.7 N5 C11B H11C 109.7 N5 C11B H11D 109.7 C10B C11B N5 109.9(19) C10B C11B H11C 109.7 C10B C11B H11D 109.7 H11C C11B H11D 108.2 O2N N1AA O3N 127(3) O1N N1AA O3N 134(4) O1N N1AA O2N 99(4) N1AA O1N Pb1 170(4) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Pb1 Cl1 2.912(16) . Pb1 N1 2.526(9) . Pb1 N2 2.639(10) . Pb1 N5 2.510(9) . Pb1 N3 2.586(10) . Pb1 N4B 2.733(17) . Pb1 N4A 2.90(2) . Pb1 O1 3.03(2) . Pb1 O1N 3.09(5) . N1 C2 1.324(15) . N1 C6 1.343(14) . N2 H2 0.9800 . N2 C7 1.470(17) . N2 C8 1.435(18) . N5 H5A 0.9800 . N5 H5B 0.9800 . N5 C1 1.459(15) . N5 C11A 1.39(3) . N5 C11B 1.63(3) . C2 C3 1.374(17) . C2 C1 1.512(17) . C18 H18A 0.9700 . C18 H18B 0.9700 . C18 C17 1.509(18) . C18 C19 1.503(17) . C3 H3 0.9300 . C3 C4 1.379(18) . N3 C12B 1.48(2) . N3 C12A 1.53(2) . N3 C9B 1.61(3) . N3 C9A 1.37(3) . N3 C10A 1.60(3) . N3 C10B 1.31(2) . C13 H13C 0.9700 . C13 H13D 0.9700 . C13 H13A 0.9700 . C13 H13B 0.9700 . C13 N4B 1.45(2) . C13 N4A 1.48(2) . C13 C12B 1.55(2) . C13 C12A 1.55(3) . C6 C7 1.487(17) . C6 C5 1.387(17) . C1 H1A 0.9700 . C1 H1B 0.9700 . C14 H14C 0.9700 . C14 H14D 0.9700 . C14 H14A 0.9700 . C14 H14B 0.9700 . C14 C15 1.49(2) . C14 N4B 1.45(2) . C14 N4A 1.48(2) . C16 H16 0.9300 . C16 C17 1.389(17) . C16 C15 1.393(17) . C7 H7A 0.9700 . C7 H7B 0.9700 . C8 H8BC 0.9700 . C8 H8BD 0.9700 . C8 H8AA 0.9700 . C8 H8AB 0.9700 . C8 C9B 1.26(3) . C8 C9A 1.59(3) . C5 H5 0.9300 . C5 C4 1.370(19) . C17 C25 1.383(17) . C23 H23 0.9300 . C23 C24 1.387(18) . C23 C22 1.40(2) . C15 C27 1.38(2) . N4B H4B 0.9800 . C26 H26 0.9300 . C26 C25 1.37(2) . C26 C27 1.37(2) . C24 C25 1.463(19) . C24 C19 1.418(19) . C4 H4 0.9300 . C27 H27 0.9300 . C19 C20 1.361(19) . N4A H4A 0.9800 . C22 H22 0.9300 . C22 C21 1.33(3) . C20 H20 0.9300 . C20 C21 1.39(2) . O3 O3 1.47(4) 3_556 C12B H12A 0.9700 . C12B H12B 0.9700 . C21 H21 0.9300 . C12A H12C 0.9700 . C12A H12D 0.9700 . C9B H9BA 0.9700 . C9B H9BB 0.9700 . C9A H9AA 0.9700 . C9A H9AB 0.9700 . C10A H10A 0.9700 . C10A H10B 0.9700 . C10A C11A 1.46(4) . C10B H10C 0.9700 . C10B H10D 0.9700 . C10B C11B 1.50(4) . O1 H1C 0.8490 . O1 H1D 0.8503 . C11A H11A 0.9700 . C11A H11B 0.9700 . C11B H11C 0.9700 . C11B H11D 0.9700 . O3N N1AA 1.28(3) . N1AA O2N 1.25(3) . N1AA O1N 1.04(4) .