#------------------------------------------------------------------------------ #$Date: 2021-10-21 11:08:57 +0300 (Thu, 21 Oct 2021) $ #$Revision: 270055 $ #$URL: file:///home/coder/svn-repositories/cod/cif/1/56/50/1565034.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_1565034 loop_ _publ_author_name 'Correia, Bruna B.' 'Brown, Thomas R.' 'Reibenspies, Joseph H.' 'Lee, Hee-Seung' 'Hancock, Robert D.' _publ_section_title ; Exciplex formation as an approach to selective Copper(II) fluorescent sensors ; _journal_name_full 'Inorganica Chimica Acta' _journal_page_first 119544 _journal_paper_doi 10.1016/j.ica.2020.119544 _journal_volume 506 _journal_year 2020 _chemical_formula_moiety 'C36 H44 N4 Pb, 2(Cl O4)' _chemical_formula_sum 'C36 H44 Cl2 N4 O8 Pb' _chemical_formula_weight 938.84 _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2ybc' _space_group_name_H-M_alt 'P 1 21/c 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary dual _cell_angle_alpha 90 _cell_angle_beta 91.106(2) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 10.1622(4) _cell_length_b 18.9273(7) _cell_length_c 19.6809(7) _cell_measurement_reflns_used 9891 _cell_measurement_temperature 100 _cell_measurement_theta_max 65.30 _cell_measurement_theta_min 3.24 _cell_volume 3784.8(2) _computing_cell_refinement 'SAINT V8.38A (?, 2016)' _computing_data_collection APEX3 _computing_data_reduction 'SAINT V8.38A (?, 2016)' _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 'ShelXT (Sheldrick, 2015)' _diffrn_ambient_temperature 100 _diffrn_detector 'Bruker CMOS area detector' _diffrn_detector_area_resol_mean 10.5 _diffrn_detector_type 'CMOS area detector' _diffrn_measured_fraction_theta_full 0.990 _diffrn_measured_fraction_theta_max 0.990 _diffrn_measurement_device 'three-circle diffractometer' _diffrn_measurement_device_type 'Bruker Micro-Source CMOS' _diffrn_measurement_method '\f and \w scans' _diffrn_radiation_monochromator 'mirror optics' _diffrn_radiation_probe x-ray _diffrn_radiation_type CuK\a _diffrn_radiation_wavelength 1.54178 _diffrn_reflns_av_R_equivalents 0.0695 _diffrn_reflns_av_unetI/netI 0.0485 _diffrn_reflns_Laue_measured_fraction_full 0.990 _diffrn_reflns_Laue_measured_fraction_max 0.990 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_number 35484 _diffrn_reflns_point_group_measured_fraction_full 0.990 _diffrn_reflns_point_group_measured_fraction_max 0.990 _diffrn_reflns_theta_full 65.418 _diffrn_reflns_theta_max 65.418 _diffrn_reflns_theta_min 3.240 _diffrn_source 'microfocus sealed X-ray tube' _diffrn_source_current 50 _diffrn_source_target Mo _diffrn_source_type 'Incoatec I\ms' _diffrn_source_voltage .1 _diffrn_standards_number 0 _exptl_absorpt_coefficient_mu 10.428 _exptl_absorpt_correction_T_max 0.3165 _exptl_absorpt_correction_T_min 0.1928 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details 'SADABS-2016/2 (Bruker,2016/2) was used for absorption correction. wR2(int) was 0.1221 before and 0.0802 after correction. The Ratio of minimum to maximum transmission is 0.6092. The \l/2 correction factor is Not present.' _exptl_crystal_colour colourless _exptl_crystal_colour_primary colourless _exptl_crystal_density_diffrn 1.648 _exptl_crystal_description plate _exptl_crystal_F_000 1872 _exptl_crystal_size_max 0.11 _exptl_crystal_size_mid 0.088 _exptl_crystal_size_min 0.039 _refine_diff_density_max 2.160 _refine_diff_density_min -1.457 _refine_diff_density_rms 0.134 _refine_ls_extinction_coef . _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.038 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 460 _refine_ls_number_reflns 6439 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.038 _refine_ls_R_factor_all 0.0597 _refine_ls_R_factor_gt 0.0465 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.0210P)^2^+35.0000P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.0957 _refine_ls_wR_factor_ref 0.1013 _reflns_Friedel_coverage 0.000 _reflns_Friedel_fraction_full . _reflns_Friedel_fraction_max . _reflns_number_gt 5460 _reflns_number_total 6439 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file ICA-2020-506-119544.cif _cod_data_source_block rh147 _cod_database_code 1565034 _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 0.687 _shelx_estimated_absorpt_t_min 0.393 _olex2_refinement_description ; 1. Fixed Uiso At 1.2 times of: All C(H) groups, All C(H,H) groups 2.a Secondary CH2 refined with riding coordinates: C1(H1A,H1B), C2(H2A,H2B), C3(H3A,H3B), C4(H4A,H4B), C5(H5A,H5B), C6(H6A,H6B), C7(H7A,H7B), C8(H8A,H8B), C9(H9A,H9B), C16(H16A,H16B), C23(H23A,H23B), C30(H30A,H30B) 2.b Aromatic/amide H refined with riding coordinates: C11(H11), C12(H12), C13(H13), C14(H14), C15(H15), C18(H18), C19(H19), C20(H20), C21(H21), C22(H22), C25(H25), C26(H26), C27(H27), C28(H28), C29(H29), C32(H32), C33(H33), C34(H34), C35(H35), C36(H36) ; _shelx_res_file ; TITL rh_a.res in P2(1)/c rh147.res created by SHELXL-2016/6 at 09:29:45 on 09-Jun-2017 REM Old TITL rh in P2(1)/c REM SHELXT solution in P2(1)/c REM R1 0.099, Rweak 0.010, Alpha 0.098, Orientation as input REM Formula found by SHELXT: C38 Cl2 N5 O4 Pb CELL 1.54178 10.1622 18.9273 19.6809 90 91.106 90 ZERR 4 0.0004 0.0007 0.0007 0 0.002 0 LATT 1 SYMM -X,0.5+Y,0.5-Z SFAC C H Cl N O Pb UNIT 144 176 8 16 32 4 L.S. 4 PLAN 5 SIZE 0.039 0.088 0.11 TEMP -173.15 BOND $H fmap 2 acta OMIT 2 8 15 OMIT -2 3 17 OMIT 6 2 18 OMIT -2 1 20 OMIT -2 2 18 OMIT -3 1 18 OMIT 5 2 16 OMIT 0 1 16 OMIT 0 1 20 OMIT -1 0 12 OMIT -2 1 16 OMIT -2 0 18 OMIT -5 4 17 OMIT 3 3 17 REM REM REM WGHT 0.021000 35.000000 FVAR 0.21455 PB1 6 0.277528 0.714525 0.378081 11.00000 0.02269 0.02907 = 0.02236 0.00062 0.00028 0.00114 N1 4 0.308485 0.629750 0.279054 11.00000 0.02436 0.02561 = 0.02561 0.00387 0.00354 -0.00022 N2 4 0.081216 0.634523 0.371241 11.00000 0.02062 0.03255 = 0.02825 0.00081 0.00141 0.00454 N3 4 0.262631 0.651484 0.490809 11.00000 0.02478 0.03512 = 0.02636 -0.00045 -0.00106 0.00426 N4 4 0.490787 0.647343 0.399004 11.00000 0.01915 0.03584 = 0.02961 0.00047 0.00168 0.00084 C1 1 0.491550 0.584431 0.353497 11.00000 0.02491 0.03144 = 0.03217 0.00239 0.00184 0.00439 AFIX 23 H1A 2 0.433839 0.547510 0.372466 11.00000 -1.20000 H1B 2 0.581984 0.565103 0.352115 11.00000 -1.20000 AFIX 0 C2 1 0.445010 0.601760 0.281765 11.00000 0.02535 0.03822 = 0.03292 -0.00043 0.00810 -0.00065 AFIX 23 H2A 2 0.505035 0.637180 0.262123 11.00000 -1.20000 H2B 2 0.449379 0.558538 0.253569 11.00000 -1.20000 AFIX 0 C3 1 0.211046 0.571141 0.284401 11.00000 0.03224 0.02568 = 0.02827 -0.00196 0.00455 -0.00141 AFIX 23 H3A 2 0.243145 0.536554 0.318623 11.00000 -1.20000 H3B 2 0.203294 0.546540 0.240113 11.00000 -1.20000 AFIX 0 C4 1 0.077879 0.597520 0.304300 11.00000 0.02541 0.03543 = 0.02792 -0.00459 -0.00266 -0.00126 AFIX 23 H4A 2 0.044109 0.630390 0.268933 11.00000 -1.20000 H4B 2 0.016356 0.557067 0.306531 11.00000 -1.20000 AFIX 0 C5 1 0.093180 0.582512 0.427557 11.00000 0.02131 0.03136 = 0.03038 0.00620 0.00485 0.00014 AFIX 23 H5A 2 0.160041 0.546646 0.416011 11.00000 -1.20000 H5B 2 0.007955 0.557965 0.432813 11.00000 -1.20000 AFIX 0 C6 1 0.131783 0.617229 0.493519 11.00000 0.03367 0.03741 = 0.02242 0.00435 0.00933 0.00192 AFIX 23 H6A 2 0.064946 0.653166 0.504907 11.00000 -1.20000 H6B 2 0.133051 0.581305 0.530087 11.00000 -1.20000 AFIX 0 C7 1 0.367061 0.596551 0.496261 11.00000 0.03276 0.03704 = 0.02638 0.00372 -0.00077 0.00815 AFIX 23 H7A 2 0.340105 0.554713 0.469200 11.00000 -1.20000 H7B 2 0.377381 0.581620 0.544278 11.00000 -1.20000 AFIX 0 C8 1 0.498062 0.623723 0.471094 11.00000 0.02801 0.03789 = 0.03161 -0.00158 -0.00834 0.00459 AFIX 23 H8A 2 0.527252 0.663783 0.500002 11.00000 -1.20000 H8B 2 0.564693 0.585780 0.475706 11.00000 -1.20000 AFIX 0 C9 1 0.284941 0.666221 0.211817 11.00000 0.03242 0.04088 = 0.01991 0.00454 0.00113 0.00200 AFIX 23 H9A 2 0.188943 0.669393 0.202803 11.00000 -1.20000 H9B 2 0.323352 0.637199 0.175347 11.00000 -1.20000 AFIX 0 C10 1 0.343196 0.739429 0.209168 11.00000 0.03449 0.04026 = 0.01641 0.00516 0.00008 0.00089 C11 1 0.468100 0.751366 0.184775 11.00000 0.03381 0.04624 = 0.03518 0.01105 -0.00487 -0.00099 AFIX 43 H11 2 0.519913 0.712810 0.169812 11.00000 -1.20000 AFIX 0 C12 1 0.517895 0.819867 0.182148 11.00000 0.03623 0.06219 = 0.03637 0.02355 -0.00265 -0.01179 AFIX 43 H12 2 0.603572 0.827779 0.165233 11.00000 -1.20000 AFIX 0 C13 1 0.444242 0.876013 0.203785 11.00000 0.05924 0.03980 = 0.03983 0.01383 -0.01723 -0.01227 AFIX 43 H13 2 0.479223 0.922532 0.202581 11.00000 -1.20000 AFIX 0 C14 1 0.319287 0.864467 0.227255 11.00000 0.06654 0.04148 = 0.02249 0.00030 -0.00563 0.00371 AFIX 43 H14 2 0.267428 0.903184 0.241799 11.00000 -1.20000 AFIX 0 C15 1 0.269406 0.796939 0.229676 11.00000 0.03709 0.03770 = 0.02716 0.00179 -0.00442 0.00219 AFIX 43 H15 2 0.182874 0.789603 0.245684 11.00000 -1.20000 AFIX 0 C16 1 -0.048034 0.674556 0.377862 11.00000 0.01799 0.04127 = 0.02943 0.00133 0.00548 0.00087 AFIX 23 H16A 2 -0.120448 0.644572 0.359782 11.00000 -1.20000 H16B 2 -0.064193 0.682739 0.426678 11.00000 -1.20000 AFIX 0 C17 1 -0.052050 0.743954 0.341800 11.00000 0.02147 0.03273 = 0.04551 0.00004 0.00080 0.00528 C18 1 -0.100113 0.749754 0.275404 11.00000 0.02559 0.04341 = 0.03973 -0.00086 -0.00481 0.00524 AFIX 43 H18 2 -0.133536 0.709157 0.252533 11.00000 -1.20000 AFIX 0 C19 1 -0.099522 0.814516 0.242372 11.00000 0.04369 0.04872 = 0.04576 0.01133 -0.00939 0.00830 AFIX 43 H19 2 -0.133964 0.818188 0.197292 11.00000 -1.20000 AFIX 0 C20 1 -0.049046 0.873763 0.274734 11.00000 0.04849 0.03725 = 0.05637 0.01446 0.00146 0.01368 AFIX 43 H20 2 -0.047239 0.917864 0.251722 11.00000 -1.20000 AFIX 0 C21 1 -0.001005 0.868364 0.341114 11.00000 0.03495 0.03660 = 0.06242 -0.00465 0.00112 0.00545 AFIX 43 H21 2 0.032874 0.908915 0.363885 11.00000 -1.20000 AFIX 0 C22 1 -0.002666 0.804021 0.373793 11.00000 0.02769 0.04296 = 0.03073 0.00264 -0.00199 0.00593 AFIX 43 H22 2 0.030632 0.800669 0.419115 11.00000 -1.20000 AFIX 0 C23 1 0.281265 0.701459 0.548876 11.00000 0.03580 0.04571 = 0.02444 -0.00336 -0.00320 0.00492 AFIX 23 H23A 2 0.375727 0.713943 0.552663 11.00000 -1.20000 H23B 2 0.257506 0.676812 0.591278 11.00000 -1.20000 AFIX 0 C24 1 0.201717 0.769271 0.543620 11.00000 0.04367 0.04330 = 0.02473 -0.00843 -0.00511 0.00064 C25 1 0.255814 0.827881 0.513225 11.00000 0.03979 0.05062 = 0.03405 -0.01199 0.00059 -0.00125 AFIX 43 H25 2 0.340800 0.824809 0.494165 11.00000 -1.20000 AFIX 0 C26 1 0.187487 0.891148 0.510217 11.00000 0.06631 0.03999 = 0.05296 -0.00469 -0.00520 -0.00389 AFIX 43 H26 2 0.224125 0.931159 0.488409 11.00000 -1.20000 AFIX 0 C27 1 0.063734 0.895187 0.539788 11.00000 0.06049 0.05250 = 0.05512 -0.01539 -0.00504 0.01105 AFIX 43 H27 2 0.016742 0.938579 0.538985 11.00000 -1.20000 AFIX 0 C28 1 0.009595 0.836895 0.569989 11.00000 0.03672 0.07062 = 0.04335 -0.01491 0.00343 0.01207 AFIX 43 H28 2 -0.074807 0.839929 0.589713 11.00000 -1.20000 AFIX 0 C29 1 0.077794 0.774065 0.571641 11.00000 0.03758 0.05322 = 0.02516 -0.00818 0.00601 0.00243 AFIX 43 H29 2 0.039724 0.733679 0.592122 11.00000 -1.20000 AFIX 0 C30 1 0.608096 0.693239 0.385678 11.00000 0.01875 0.04840 = 0.04563 0.00666 0.00249 -0.00156 AFIX 23 H30A 2 0.621997 0.695059 0.336059 11.00000 -1.20000 H30B 2 0.686993 0.671192 0.407001 11.00000 -1.20000 AFIX 0 C31 1 0.595618 0.767564 0.411968 11.00000 0.01955 0.03379 = 0.03678 0.00029 -0.00287 -0.00137 C32 1 0.540330 0.818768 0.368237 11.00000 0.03831 0.03500 = 0.04030 0.00806 -0.00364 -0.00167 AFIX 43 H32 2 0.511545 0.805835 0.323741 11.00000 -1.20000 AFIX 0 C33 1 0.527795 0.887761 0.389813 11.00000 0.04112 0.04222 = 0.05540 0.00131 -0.00383 0.00251 AFIX 43 H33 2 0.486303 0.921615 0.360918 11.00000 -1.20000 AFIX 0 C34 1 0.574795 0.907773 0.452637 11.00000 0.05376 0.03223 = 0.06886 -0.00750 -0.00319 -0.00589 AFIX 43 H34 2 0.567766 0.955525 0.466984 11.00000 -1.20000 AFIX 0 C35 1 0.632561 0.857853 0.494988 11.00000 0.04854 0.05639 = 0.05271 -0.00837 -0.01180 -0.01235 AFIX 43 H35 2 0.665317 0.871602 0.538549 11.00000 -1.20000 AFIX 0 C36 1 0.643239 0.787986 0.474637 11.00000 0.04113 0.04254 = 0.05031 0.00746 -0.01426 -0.00455 AFIX 43 H36 2 0.683543 0.754253 0.504100 11.00000 -1.20000 AFIX 0 CL1 3 0.242293 1.060632 0.308259 11.00000 0.03725 0.03935 = 0.04611 -0.00232 0.00596 0.00442 O1 5 0.268175 1.131884 0.326195 11.00000 0.05545 0.04385 = 0.06479 -0.00513 -0.00226 -0.00878 O2 5 0.112634 1.041743 0.326447 11.00000 0.06253 0.06241 = 0.07225 -0.01024 0.02662 -0.02087 O3 5 0.248238 1.054543 0.235334 11.00000 0.05679 0.12088 = 0.04861 -0.01905 0.01365 -0.00615 O4 5 0.338260 1.018346 0.337285 11.00000 0.12062 0.07845 = 0.11735 0.00952 -0.04492 0.04348 CL2 3 0.197193 0.404683 0.427860 11.00000 0.02865 0.03495 = 0.02974 0.00489 0.00166 -0.00035 O5 5 0.182728 0.430967 0.495900 11.00000 0.03484 0.06618 = 0.02769 0.00372 0.00829 0.00402 O6 5 0.216253 0.330048 0.428745 11.00000 0.04512 0.03399 = 0.06732 0.01045 -0.00979 -0.00474 O7 5 0.309889 0.438424 0.399098 11.00000 0.03326 0.03475 = 0.03627 0.00355 0.00988 0.00144 O8 5 0.081895 0.421651 0.387742 11.00000 0.03615 0.04436 = 0.04008 0.00091 -0.00776 0.00774 HKLF 4 REM rh_a.res in P2(1)/c REM R1 = 0.0465 for 5460 Fo > 4sig(Fo) and 0.0597 for all 6439 data REM 460 parameters refined using 0 restraints END WGHT 0.0215 27.1747 REM Highest difference peak 2.160, deepest hole -1.457, 1-sigma level 0.134 Q1 1 0.2374 0.7720 0.3575 11.00000 0.05 2.16 Q2 1 0.2706 0.6641 0.3748 11.00000 0.05 1.91 Q3 1 0.1953 0.7169 0.3868 11.00000 0.05 1.61 Q4 1 0.3075 0.7167 0.3304 11.00000 0.05 1.52 Q5 1 0.1648 0.7849 0.3986 11.00000 0.05 1.24 ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -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 0.27753(3) 0.71452(2) 0.37808(2) 0.02471(10) Uani 1 1 d . . . . . N1 N 0.3085(5) 0.6298(3) 0.2791(3) 0.0252(13) Uani 1 1 d . . . . . N2 N 0.0812(5) 0.6345(3) 0.3712(3) 0.0271(13) Uani 1 1 d . . . . . N3 N 0.2626(6) 0.6515(3) 0.4908(3) 0.0288(13) Uani 1 1 d . . . . . N4 N 0.4908(5) 0.6473(3) 0.3990(3) 0.0282(13) Uani 1 1 d . . . . . C1 C 0.4916(7) 0.5844(4) 0.3535(4) 0.0295(16) Uani 1 1 d . . . . . H1A H 0.433839 0.547510 0.372466 0.035 Uiso 1 1 calc R . . . . H1B H 0.581984 0.565103 0.352115 0.035 Uiso 1 1 calc R . . . . C2 C 0.4450(7) 0.6018(4) 0.2818(4) 0.0321(17) Uani 1 1 d . . . . . H2A H 0.505035 0.637180 0.262123 0.038 Uiso 1 1 calc R . . . . H2B H 0.449379 0.558538 0.253569 0.038 Uiso 1 1 calc R . . . . C3 C 0.2110(7) 0.5711(4) 0.2844(4) 0.0287(16) Uani 1 1 d . . . . . H3A H 0.243145 0.536554 0.318623 0.034 Uiso 1 1 calc R . . . . H3B H 0.203294 0.546540 0.240113 0.034 Uiso 1 1 calc R . . . . C4 C 0.0779(7) 0.5975(4) 0.3043(3) 0.0296(16) Uani 1 1 d . . . . . H4A H 0.044109 0.630390 0.268933 0.036 Uiso 1 1 calc R . . . . H4B H 0.016356 0.557067 0.306531 0.036 Uiso 1 1 calc R . . . . C5 C 0.0932(7) 0.5825(4) 0.4276(3) 0.0276(16) Uani 1 1 d . . . . . H5A H 0.160041 0.546646 0.416011 0.033 Uiso 1 1 calc R . . . . H5B H 0.007955 0.557965 0.432813 0.033 Uiso 1 1 calc R . . . . C6 C 0.1318(7) 0.6172(4) 0.4935(3) 0.0311(17) Uani 1 1 d . . . . . H6A H 0.064946 0.653166 0.504907 0.037 Uiso 1 1 calc R . . . . H6B H 0.133051 0.581305 0.530087 0.037 Uiso 1 1 calc R . . . . C7 C 0.3671(7) 0.5966(4) 0.4963(4) 0.0321(17) Uani 1 1 d . . . . . H7A H 0.340105 0.554713 0.469200 0.038 Uiso 1 1 calc R . . . . H7B H 0.377381 0.581620 0.544278 0.038 Uiso 1 1 calc R . . . . C8 C 0.4981(7) 0.6237(4) 0.4711(4) 0.0326(17) Uani 1 1 d . . . . . H8A H 0.527252 0.663783 0.500002 0.039 Uiso 1 1 calc R . . . . H8B H 0.564693 0.585780 0.475706 0.039 Uiso 1 1 calc R . . . . C9 C 0.2849(7) 0.6662(4) 0.2118(3) 0.0311(17) Uani 1 1 d . . . . . H9A H 0.188943 0.669393 0.202803 0.037 Uiso 1 1 calc R . . . . H9B H 0.323352 0.637199 0.175347 0.037 Uiso 1 1 calc R . . . . C10 C 0.3432(7) 0.7394(4) 0.2092(3) 0.0304(17) Uani 1 1 d . . . . . C11 C 0.4681(8) 0.7514(5) 0.1848(4) 0.0385(19) Uani 1 1 d . . . . . H11 H 0.519913 0.712810 0.169812 0.046 Uiso 1 1 calc R . . . . C12 C 0.5179(8) 0.8199(5) 0.1821(4) 0.045(2) Uani 1 1 d . . . . . H12 H 0.603572 0.827779 0.165233 0.054 Uiso 1 1 calc R . . . . C13 C 0.4442(9) 0.8760(5) 0.2038(4) 0.047(2) Uani 1 1 d . . . . . H13 H 0.479223 0.922532 0.202581 0.056 Uiso 1 1 calc R . . . . C14 C 0.3193(9) 0.8645(5) 0.2273(4) 0.044(2) Uani 1 1 d . . . . . H14 H 0.267428 0.903184 0.241799 0.052 Uiso 1 1 calc R . . . . C15 C 0.2694(8) 0.7969(4) 0.2297(4) 0.0340(18) Uani 1 1 d . . . . . H15 H 0.182874 0.789603 0.245684 0.041 Uiso 1 1 calc R . . . . C16 C -0.0480(7) 0.6746(4) 0.3779(4) 0.0295(16) Uani 1 1 d . . . . . H16A H -0.120448 0.644572 0.359782 0.035 Uiso 1 1 calc R . . . . H16B H -0.064193 0.682739 0.426678 0.035 Uiso 1 1 calc R . . . . C17 C -0.0520(7) 0.7440(4) 0.3418(4) 0.0332(17) Uani 1 1 d . . . . . C18 C -0.1001(7) 0.7498(4) 0.2754(4) 0.0363(18) Uani 1 1 d . . . . . H18 H -0.133536 0.709157 0.252533 0.044 Uiso 1 1 calc R . . . . C19 C -0.0995(8) 0.8145(5) 0.2424(5) 0.046(2) Uani 1 1 d . . . . . H19 H -0.133964 0.818188 0.197292 0.055 Uiso 1 1 calc R . . . . C20 C -0.0490(9) 0.8738(5) 0.2747(5) 0.047(2) Uani 1 1 d . . . . . H20 H -0.047239 0.917864 0.251722 0.057 Uiso 1 1 calc R . . . . C21 C -0.0010(8) 0.8684(5) 0.3411(5) 0.045(2) Uani 1 1 d . . . . . H21 H 0.032874 0.908915 0.363885 0.054 Uiso 1 1 calc R . . . . C22 C -0.0027(7) 0.8040(4) 0.3738(4) 0.0338(18) Uani 1 1 d . . . . . H22 H 0.030632 0.800669 0.419115 0.041 Uiso 1 1 calc R . . . . C23 C 0.2813(8) 0.7015(4) 0.5489(4) 0.0354(18) Uani 1 1 d . . . . . H23A H 0.375727 0.713943 0.552663 0.042 Uiso 1 1 calc R . . . . H23B H 0.257506 0.676812 0.591278 0.042 Uiso 1 1 calc R . . . . C24 C 0.2017(8) 0.7693(4) 0.5436(4) 0.0373(19) Uani 1 1 d . . . . . C25 C 0.2558(8) 0.8279(5) 0.5132(4) 0.041(2) Uani 1 1 d . . . . . H25 H 0.340800 0.824809 0.494165 0.050 Uiso 1 1 calc R . . . . C26 C 0.1875(10) 0.8911(5) 0.5102(5) 0.053(2) Uani 1 1 d . . . . . H26 H 0.224125 0.931159 0.488409 0.064 Uiso 1 1 calc R . . . . C27 C 0.0637(10) 0.8952(5) 0.5398(5) 0.056(3) Uani 1 1 d . . . . . H27 H 0.016742 0.938579 0.538985 0.067 Uiso 1 1 calc R . . . . C28 C 0.0096(9) 0.8369(5) 0.5700(4) 0.050(2) Uani 1 1 d . . . . . H28 H -0.074807 0.839929 0.589713 0.060 Uiso 1 1 calc R . . . . C29 C 0.0778(8) 0.7741(5) 0.5716(4) 0.0386(19) Uani 1 1 d . . . . . H29 H 0.039724 0.733679 0.592122 0.046 Uiso 1 1 calc R . . . . C30 C 0.6081(7) 0.6932(4) 0.3857(4) 0.0376(19) Uani 1 1 d . . . . . H30A H 0.621997 0.695059 0.336059 0.045 Uiso 1 1 calc R . . . . H30B H 0.686993 0.671192 0.407001 0.045 Uiso 1 1 calc R . . . . C31 C 0.5956(7) 0.7676(4) 0.4120(4) 0.0301(17) Uani 1 1 d . . . . . C32 C 0.5403(8) 0.8188(4) 0.3682(4) 0.0379(19) Uani 1 1 d . . . . . H32 H 0.511545 0.805835 0.323741 0.046 Uiso 1 1 calc R . . . . C33 C 0.5278(8) 0.8878(5) 0.3898(5) 0.046(2) Uani 1 1 d . . . . . H33 H 0.486303 0.921615 0.360918 0.056 Uiso 1 1 calc R . . . . C34 C 0.5748(9) 0.9078(5) 0.4526(5) 0.052(2) Uani 1 1 d . . . . . H34 H 0.567766 0.955525 0.466984 0.062 Uiso 1 1 calc R . . . . C35 C 0.6326(9) 0.8579(5) 0.4950(5) 0.053(2) Uani 1 1 d . . . . . H35 H 0.665317 0.871602 0.538549 0.063 Uiso 1 1 calc R . . . . C36 C 0.6432(8) 0.7880(5) 0.4746(4) 0.045(2) Uani 1 1 d . . . . . H36 H 0.683543 0.754253 0.504100 0.054 Uiso 1 1 calc R . . . . Cl1 Cl 0.24229(19) 1.06063(11) 0.30826(10) 0.0408(4) Uani 1 1 d . . . . . O1 O 0.2682(6) 1.1319(3) 0.3262(3) 0.0547(16) Uani 1 1 d . . . . . O2 O 0.1126(7) 1.0417(4) 0.3264(3) 0.0654(19) Uani 1 1 d . . . . . O3 O 0.2482(7) 1.0545(4) 0.2353(3) 0.075(2) Uani 1 1 d . . . . . O4 O 0.3383(10) 1.0183(5) 0.3373(5) 0.106(3) Uani 1 1 d . . . . . Cl2 Cl 0.19719(17) 0.40468(9) 0.42786(8) 0.0311(4) Uani 1 1 d . . . . . O5 O 0.1827(5) 0.4310(3) 0.4959(3) 0.0428(14) Uani 1 1 d . . . . . O6 O 0.2163(6) 0.3300(3) 0.4287(3) 0.0490(15) Uani 1 1 d . . . . . O7 O 0.3099(5) 0.4384(3) 0.3991(2) 0.0346(12) Uani 1 1 d . . . . . O8 O 0.0819(5) 0.4217(3) 0.3877(3) 0.0403(13) Uani 1 1 d . . . . . 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 0.02269(14) 0.02907(16) 0.02236(14) 0.00062(12) 0.00028(9) 0.00114(13) N1 0.024(3) 0.026(3) 0.026(3) 0.004(2) 0.004(2) 0.000(2) N2 0.021(3) 0.033(3) 0.028(3) 0.001(3) 0.001(2) 0.005(3) N3 0.025(3) 0.035(4) 0.026(3) 0.000(3) -0.001(2) 0.004(3) N4 0.019(3) 0.036(4) 0.030(3) 0.000(3) 0.002(2) 0.001(3) C1 0.025(4) 0.031(4) 0.032(4) 0.002(3) 0.002(3) 0.004(3) C2 0.025(4) 0.038(4) 0.033(4) 0.000(3) 0.008(3) -0.001(3) C3 0.032(4) 0.026(4) 0.028(4) -0.002(3) 0.005(3) -0.001(3) C4 0.025(4) 0.035(4) 0.028(4) -0.005(3) -0.003(3) -0.001(3) C5 0.021(4) 0.031(4) 0.030(4) 0.006(3) 0.005(3) 0.000(3) C6 0.034(4) 0.037(4) 0.022(4) 0.004(3) 0.009(3) 0.002(3) C7 0.033(4) 0.037(4) 0.026(4) 0.004(3) -0.001(3) 0.008(3) C8 0.028(4) 0.038(5) 0.032(4) -0.002(3) -0.008(3) 0.005(3) C9 0.032(4) 0.041(5) 0.020(3) 0.005(3) 0.001(3) 0.002(3) C10 0.034(4) 0.040(5) 0.016(3) 0.005(3) 0.000(3) 0.001(3) C11 0.034(5) 0.046(5) 0.035(4) 0.011(4) -0.005(3) -0.001(4) C12 0.036(5) 0.062(6) 0.036(5) 0.024(4) -0.003(4) -0.012(4) C13 0.059(6) 0.040(5) 0.040(5) 0.014(4) -0.017(4) -0.012(4) C14 0.067(6) 0.041(5) 0.022(4) 0.000(4) -0.006(4) 0.004(4) C15 0.037(4) 0.038(5) 0.027(4) 0.002(3) -0.004(3) 0.002(3) C16 0.018(3) 0.041(5) 0.029(4) 0.001(3) 0.005(3) 0.001(3) C17 0.021(4) 0.033(4) 0.046(5) 0.000(4) 0.001(3) 0.005(3) C18 0.026(4) 0.043(5) 0.040(4) -0.001(4) -0.005(3) 0.005(3) C19 0.044(5) 0.049(5) 0.046(5) 0.011(4) -0.009(4) 0.008(4) C20 0.048(5) 0.037(5) 0.056(6) 0.014(4) 0.001(4) 0.014(4) C21 0.035(5) 0.037(5) 0.062(6) -0.005(4) 0.001(4) 0.005(4) C22 0.028(4) 0.043(5) 0.031(4) 0.003(3) -0.002(3) 0.006(3) C23 0.036(4) 0.046(5) 0.024(4) -0.003(3) -0.003(3) 0.005(4) C24 0.044(5) 0.043(5) 0.025(4) -0.008(3) -0.005(3) 0.001(4) C25 0.040(5) 0.051(6) 0.034(4) -0.012(4) 0.001(4) -0.001(4) C26 0.066(7) 0.040(5) 0.053(6) -0.005(4) -0.005(5) -0.004(5) C27 0.060(6) 0.052(6) 0.055(6) -0.015(5) -0.005(5) 0.011(5) C28 0.037(5) 0.071(7) 0.043(5) -0.015(5) 0.003(4) 0.012(5) C29 0.038(4) 0.053(6) 0.025(4) -0.008(4) 0.006(3) 0.002(4) C30 0.019(4) 0.048(5) 0.046(5) 0.007(4) 0.002(3) -0.002(3) C31 0.020(4) 0.034(4) 0.037(4) 0.000(3) -0.003(3) -0.001(3) C32 0.038(5) 0.035(5) 0.040(5) 0.008(4) -0.004(4) -0.002(4) C33 0.041(5) 0.042(5) 0.055(5) 0.001(4) -0.004(4) 0.003(4) C34 0.054(6) 0.032(5) 0.069(6) -0.007(4) -0.003(5) -0.006(4) C35 0.049(5) 0.056(6) 0.053(5) -0.008(5) -0.012(4) -0.012(5) C36 0.041(5) 0.043(5) 0.050(5) 0.007(4) -0.014(4) -0.005(4) Cl1 0.0372(10) 0.0394(11) 0.0461(11) -0.0023(9) 0.0060(9) 0.0044(8) O1 0.055(4) 0.044(4) 0.065(4) -0.005(3) -0.002(3) -0.009(3) O2 0.063(4) 0.062(5) 0.072(4) -0.010(4) 0.027(4) -0.021(3) O3 0.057(4) 0.121(7) 0.049(4) -0.019(4) 0.014(3) -0.006(4) O4 0.121(7) 0.078(6) 0.117(7) 0.010(5) -0.045(6) 0.043(5) Cl2 0.0286(9) 0.0350(10) 0.0297(9) 0.0049(7) 0.0017(7) -0.0004(7) O5 0.035(3) 0.066(4) 0.028(3) 0.004(3) 0.008(2) 0.004(3) O6 0.045(3) 0.034(3) 0.067(4) 0.010(3) -0.010(3) -0.005(3) O7 0.033(3) 0.035(3) 0.036(3) 0.004(2) 0.010(2) 0.001(2) O8 0.036(3) 0.044(3) 0.040(3) 0.001(3) -0.008(2) 0.008(3) loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 0.3639 0.7018 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0311 0.0180 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -4.0753 8.5060 '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 N2 Pb1 N1 71.84(18) . . N2 Pb1 N3 72.58(18) . . N2 Pb1 N4 112.47(19) . . N3 Pb1 N1 112.62(19) . . N3 Pb1 N4 71.73(18) . . N4 Pb1 N1 72.01(18) . . C2 N1 Pb1 109.0(4) . . C2 N1 C3 110.7(5) . . C2 N1 C9 109.1(5) . . C3 N1 Pb1 108.8(4) . . C3 N1 C9 107.9(5) . . C9 N1 Pb1 111.3(4) . . C4 N2 Pb1 109.6(4) . . C4 N2 C16 107.7(5) . . C5 N2 Pb1 107.9(4) . . C5 N2 C4 110.4(5) . . C5 N2 C16 108.9(5) . . C16 N2 Pb1 112.4(4) . . C6 N3 Pb1 107.9(4) . . C6 N3 C7 109.3(6) . . C6 N3 C23 110.5(6) . . C7 N3 Pb1 109.8(4) . . C7 N3 C23 107.9(5) . . C23 N3 Pb1 111.4(4) . . C1 N4 Pb1 108.5(4) . . C1 N4 C30 110.1(6) . . C8 N4 Pb1 109.4(4) . . C8 N4 C1 109.4(6) . . C8 N4 C30 108.4(5) . . C30 N4 Pb1 111.1(4) . . N4 C1 H1A 109.1 . . N4 C1 H1B 109.1 . . N4 C1 C2 112.4(6) . . H1A C1 H1B 107.8 . . C2 C1 H1A 109.1 . . C2 C1 H1B 109.1 . . N1 C2 C1 112.6(6) . . N1 C2 H2A 109.1 . . N1 C2 H2B 109.1 . . C1 C2 H2A 109.1 . . C1 C2 H2B 109.1 . . H2A C2 H2B 107.8 . . N1 C3 H3A 109.2 . . N1 C3 H3B 109.2 . . N1 C3 C4 112.0(6) . . H3A C3 H3B 107.9 . . C4 C3 H3A 109.2 . . C4 C3 H3B 109.2 . . N2 C4 C3 112.4(5) . . N2 C4 H4A 109.1 . . N2 C4 H4B 109.1 . . C3 C4 H4A 109.1 . . C3 C4 H4B 109.1 . . H4A C4 H4B 107.9 . . N2 C5 H5A 109.3 . . N2 C5 H5B 109.3 . . N2 C5 C6 111.8(6) . . H5A C5 H5B 107.9 . . C6 C5 H5A 109.3 . . C6 C5 H5B 109.3 . . N3 C6 C5 112.4(6) . . N3 C6 H6A 109.1 . . N3 C6 H6B 109.1 . . C5 C6 H6A 109.1 . . C5 C6 H6B 109.1 . . H6A C6 H6B 107.9 . . N3 C7 H7A 109.3 . . N3 C7 H7B 109.3 . . N3 C7 C8 111.6(6) . . H7A C7 H7B 108.0 . . C8 C7 H7A 109.3 . . C8 C7 H7B 109.3 . . N4 C8 C7 112.6(5) . . N4 C8 H8A 109.1 . . N4 C8 H8B 109.1 . . C7 C8 H8A 109.1 . . C7 C8 H8B 109.1 . . H8A C8 H8B 107.8 . . N1 C9 H9A 108.9 . . N1 C9 H9B 108.9 . . N1 C9 C10 113.3(6) . . H9A C9 H9B 107.7 . . C10 C9 H9A 108.9 . . C10 C9 H9B 108.9 . . C11 C10 C9 121.7(7) . . C11 C10 C15 118.5(8) . . C15 C10 C9 119.8(7) . . C10 C11 H11 120.0 . . C10 C11 C12 120.1(8) . . C12 C11 H11 120.0 . . C11 C12 H12 119.7 . . C13 C12 C11 120.6(8) . . C13 C12 H12 119.7 . . C12 C13 H13 120.2 . . C12 C13 C14 119.6(8) . . C14 C13 H13 120.2 . . C13 C14 H14 119.9 . . C15 C14 C13 120.1(8) . . C15 C14 H14 119.9 . . C10 C15 H15 119.4 . . C14 C15 C10 121.2(8) . . C14 C15 H15 119.4 . . N2 C16 H16A 108.7 . . N2 C16 H16B 108.7 . . H16A C16 H16B 107.6 . . C17 C16 N2 114.4(6) . . C17 C16 H16A 108.7 . . C17 C16 H16B 108.7 . . C18 C17 C16 121.5(7) . . C22 C17 C16 119.9(7) . . C22 C17 C18 118.6(7) . . C17 C18 H18 119.8 . . C19 C18 C17 120.4(8) . . C19 C18 H18 119.8 . . C18 C19 H19 119.8 . . C20 C19 C18 120.4(8) . . C20 C19 H19 119.8 . . C19 C20 H20 120.2 . . C19 C20 C21 119.6(8) . . C21 C20 H20 120.2 . . C20 C21 H21 120.1 . . C22 C21 C20 119.8(8) . . C22 C21 H21 120.1 . . C17 C22 H22 119.3 . . C21 C22 C17 121.3(7) . . C21 C22 H22 119.3 . . N3 C23 H23A 108.5 . . N3 C23 H23B 108.5 . . N3 C23 C24 115.1(6) . . H23A C23 H23B 107.5 . . C24 C23 H23A 108.5 . . C24 C23 H23B 108.5 . . C25 C24 C23 119.5(8) . . C25 C24 C29 119.5(8) . . C29 C24 C23 120.9(8) . . C24 C25 H25 119.7 . . C24 C25 C26 120.7(9) . . C26 C25 H25 119.7 . . C25 C26 H26 120.5 . . C25 C26 C27 118.9(9) . . C27 C26 H26 120.5 . . C26 C27 H27 119.8 . . C28 C27 C26 120.5(9) . . C28 C27 H27 119.8 . . C27 C28 H28 120.0 . . C27 C28 C29 119.9(9) . . C29 C28 H28 120.0 . . C24 C29 H29 119.7 . . C28 C29 C24 120.5(8) . . C28 C29 H29 119.7 . . N4 C30 H30A 108.7 . . N4 C30 H30B 108.7 . . N4 C30 C31 114.1(6) . . H30A C30 H30B 107.6 . . C31 C30 H30A 108.7 . . C31 C30 H30B 108.7 . . C32 C31 C30 118.0(7) . . C36 C31 C30 122.8(7) . . C36 C31 C32 119.1(7) . . C31 C32 H32 119.9 . . C33 C32 C31 120.1(8) . . C33 C32 H32 119.9 . . C32 C33 H33 119.8 . . C34 C33 C32 120.4(8) . . C34 C33 H33 119.8 . . C33 C34 H34 120.3 . . C33 C34 C35 119.4(8) . . C35 C34 H34 120.3 . . C34 C35 H35 119.6 . . C34 C35 C36 120.8(8) . . C36 C35 H35 119.6 . . C31 C36 C35 120.0(8) . . C31 C36 H36 120.0 . . C35 C36 H36 120.0 . . O1 Cl1 O2 110.2(4) . . O1 Cl1 O3 108.2(4) . . O2 Cl1 O3 106.7(4) . . O4 Cl1 O1 108.9(5) . . O4 Cl1 O2 113.8(6) . . O4 Cl1 O3 108.9(5) . . O6 Cl2 O5 110.3(4) . . O6 Cl2 O7 109.6(3) . . O6 Cl2 O8 109.7(3) . . O7 Cl2 O5 108.0(3) . . O8 Cl2 O5 109.7(3) . . O8 Cl2 O7 109.4(3) . . loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 Pb1 N1 2.549(6) . Pb1 N2 2.506(6) . Pb1 N3 2.526(6) . Pb1 N4 2.539(6) . N1 C2 1.485(9) . N1 C3 1.492(9) . N1 C9 1.508(8) . N2 C4 1.492(9) . N2 C5 1.486(9) . N2 C16 1.524(9) . N3 C6 1.481(9) . N3 C7 1.488(9) . N3 C23 1.493(9) . N4 C1 1.490(9) . N4 C8 1.488(9) . N4 C30 1.502(9) . C1 H1A 0.9900 . C1 H1B 0.9900 . C1 C2 1.516(10) . C2 H2A 0.9900 . C2 H2B 0.9900 . C3 H3A 0.9900 . C3 H3B 0.9900 . C3 C4 1.501(10) . C4 H4A 0.9900 . C4 H4B 0.9900 . C5 H5A 0.9900 . C5 H5B 0.9900 . C5 C6 1.500(10) . C6 H6A 0.9900 . C6 H6B 0.9900 . C7 H7A 0.9900 . C7 H7B 0.9900 . C7 C8 1.519(10) . C8 H8A 0.9900 . C8 H8B 0.9900 . C9 H9A 0.9900 . C9 H9B 0.9900 . C9 C10 1.508(11) . C10 C11 1.384(11) . C10 C15 1.386(10) . C11 H11 0.9500 . C11 C12 1.393(12) . C12 H12 0.9500 . C12 C13 1.372(13) . C13 H13 0.9500 . C13 C14 1.377(12) . C14 H14 0.9500 . C14 C15 1.376(11) . C15 H15 0.9500 . C16 H16A 0.9900 . C16 H16B 0.9900 . C16 C17 1.493(10) . C17 C18 1.391(10) . C17 C22 1.389(11) . C18 H18 0.9500 . C18 C19 1.388(11) . C19 H19 0.9500 . C19 C20 1.383(12) . C20 H20 0.9500 . C20 C21 1.390(12) . C21 H21 0.9500 . C21 C22 1.377(11) . C22 H22 0.9500 . C23 H23A 0.9900 . C23 H23B 0.9900 . C23 C24 1.519(11) . C24 C25 1.380(12) . C24 C29 1.387(11) . C25 H25 0.9500 . C25 C26 1.385(12) . C26 H26 0.9500 . C26 C27 1.398(14) . C27 H27 0.9500 . C27 C28 1.373(14) . C28 H28 0.9500 . C28 C29 1.376(12) . C29 H29 0.9500 . C30 H30A 0.9900 . C30 H30B 0.9900 . C30 C31 1.505(11) . C31 C32 1.406(10) . C31 C36 1.372(11) . C32 H32 0.9500 . C32 C33 1.380(12) . C33 H33 0.9500 . C33 C34 1.370(12) . C34 H34 0.9500 . C34 C35 1.383(13) . C35 H35 0.9500 . C35 C36 1.387(12) . C36 H36 0.9500 . Cl1 O1 1.417(6) . Cl1 O2 1.418(7) . Cl1 O3 1.442(7) . Cl1 O4 1.377(7) . Cl2 O5 1.439(5) . Cl2 O6 1.426(6) . Cl2 O7 1.437(5) . Cl2 O8 1.437(5) .