# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2008 data_global _journal_coden_Cambridge 440 loop_ _publ_author_name 'Peter Junk' 'Craig Forsyth ' 'Cameron Jones' 'Andreas Stasch' _publ_contact_author_name 'Peter Junk' _publ_contact_author_address ; School of Chemistry Monash University Clayton VIC 3800 AUSTRALIA ; _publ_contact_author_email PETER.JUNK@SCI.MONASH.EDU.AU _publ_requested_journal 'New Journal of Chemistry' _publ_section_title ; Thermally stable lead(II) amidinates and guanidinates ; data_pbcygoab _database_code_depnum_ccdc_archive 'CCDC 677774' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C74 H110 N6 O2 Pb2, 2(C7 H8), C7 H8' _chemical_formula_sum 'C95 H134 N6 O2 Pb2' _chemical_formula_weight 1806.46 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' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.0458(2) _cell_length_b 24.5646(6) _cell_length_c 17.3771(4) _cell_angle_alpha 90.00 _cell_angle_beta 97.058(1) _cell_angle_gamma 90.00 _cell_volume 4255.67(17) _cell_formula_units_Z 2 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.410 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1852 _exptl_absorpt_coefficient_mu 4.002 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.48 _exptl_absorpt_correction_T_max 0.72 _exptl_absorpt_process_details 'SORATV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius KAPPA CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35104 _diffrn_reflns_av_R_equivalents 0.0864 _diffrn_reflns_av_sigmaI/netI 0.0906 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -30 _diffrn_reflns_limit_k_max 29 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.34 _diffrn_reflns_theta_max 26.00 _reflns_number_total 8328 _reflns_number_gt 6160 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo SMN (Otwinoski and Minor, 1997)' _computing_data_reduction 'Denzo SMN (Otwinoski and Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The lattice toluene molecules C38 > C44 and C45 > C51 were modelled as disordered over two two positions (C38 > C44, refined occupancies 0.51:0.49; C45 > C51 with the second component related by inversion) and were refined with restrained geometry and anisotropic thermal parameters. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0172P)^2^+11.5693P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8328 _refine_ls_number_parameters 572 _refine_ls_number_restraints 70 _refine_ls_R_factor_all 0.0915 _refine_ls_R_factor_gt 0.0547 _refine_ls_wR_factor_ref 0.0796 _refine_ls_wR_factor_gt 0.0723 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb -0.00033(2) 0.569298(8) 0.533413(13) 0.01672(7) Uani 1 1 d . . . O1 O -0.1453(3) 0.49941(14) 0.4839(2) 0.0187(9) Uani 1 1 d . . . N1 N 0.0823(4) 0.65560(17) 0.4629(3) 0.0154(10) Uani 1 1 d . . . N2 N -0.0287(4) 0.58570(16) 0.4031(3) 0.0143(10) Uani 1 1 d . . . N3 N -0.0293(4) 0.66997(17) 0.3328(3) 0.0151(10) Uani 1 1 d . . . C1 C 0.0114(5) 0.6389(2) 0.3987(3) 0.0132(12) Uani 1 1 d . . . C2 C 0.1126(5) 0.7085(2) 0.4896(3) 0.0173(13) Uani 1 1 d . . . C3 C 0.2516(5) 0.7209(2) 0.5085(3) 0.0191(13) Uani 1 1 d . . . C4 C 0.2869(6) 0.7727(2) 0.5352(3) 0.0239(14) Uani 1 1 d . . . H4 H 0.3792 0.7816 0.5467 0.029 Uiso 1 1 calc R . . C5 C 0.1920(6) 0.8116(2) 0.5456(3) 0.0255(14) Uani 1 1 d . . . H5 H 0.2187 0.8473 0.5617 0.031 Uiso 1 1 calc R . . C6 C 0.0570(6) 0.7981(2) 0.5323(3) 0.0216(13) Uani 1 1 d . . . H6 H -0.0081 0.8245 0.5418 0.026 Uiso 1 1 calc R . . C7 C 0.0148(5) 0.7468(2) 0.5054(3) 0.0173(13) Uani 1 1 d . . . C8 C 0.3570(5) 0.6780(2) 0.5002(3) 0.0236(14) Uani 1 1 d . . . H8 H 0.3097 0.6421 0.4950 0.028 Uiso 1 1 calc R . . C9 C 0.4243(6) 0.6859(3) 0.4271(4) 0.0346(17) Uani 1 1 d . . . H9A H 0.4908 0.6570 0.4238 0.052 Uiso 1 1 calc R . . H9B H 0.4689 0.7214 0.4290 0.052 Uiso 1 1 calc R . . H9C H 0.3565 0.6842 0.3815 0.052 Uiso 1 1 calc R . . C10 C 0.4590(5) 0.6749(3) 0.5729(4) 0.0328(16) Uani 1 1 d . . . H10A H 0.5254 0.6466 0.5661 0.049 Uiso 1 1 calc R . . H10B H 0.4127 0.6659 0.6178 0.049 Uiso 1 1 calc R . . H10C H 0.5043 0.7101 0.5815 0.049 Uiso 1 1 calc R . . C11 C -0.1319(5) 0.7304(2) 0.5000(3) 0.0235(14) Uani 1 1 d . . . H11 H -0.1492 0.7033 0.4569 0.028 Uiso 1 1 calc R . . C12 C -0.1593(6) 0.7022(2) 0.5743(4) 0.0306(16) Uani 1 1 d . . . H12A H -0.2540 0.6916 0.5701 0.046 Uiso 1 1 calc R . . H12B H -0.1389 0.7271 0.6181 0.046 Uiso 1 1 calc R . . H12C H -0.1028 0.6697 0.5826 0.046 Uiso 1 1 calc R . . C13 C -0.2303(5) 0.7773(3) 0.4821(4) 0.0325(16) Uani 1 1 d . . . H13A H -0.2137 0.7948 0.4335 0.049 Uiso 1 1 calc R . . H13B H -0.2180 0.8040 0.5243 0.049 Uiso 1 1 calc R . . H13C H -0.3223 0.7633 0.4769 0.049 Uiso 1 1 calc R . . C14 C -0.0549(5) 0.5468(2) 0.3434(3) 0.0168(13) Uani 1 1 d . . . C15 C -0.1674(5) 0.5122(2) 0.3458(3) 0.0165(13) Uani 1 1 d . . . C16 C -0.2014(6) 0.4762(2) 0.2842(4) 0.0248(15) Uani 1 1 d . . . H16 H -0.2789 0.4540 0.2839 0.030 Uiso 1 1 calc R . . C17 C -0.1242(6) 0.4722(2) 0.2238(4) 0.0303(15) Uani 1 1 d . . . H17 H -0.1512 0.4492 0.1808 0.036 Uiso 1 1 calc R . . C18 C -0.0072(6) 0.5024(2) 0.2269(3) 0.0256(14) Uani 1 1 d . . . H18 H 0.0479 0.4980 0.1866 0.031 Uiso 1 1 calc R . . C19 C 0.0328(5) 0.5384(2) 0.2862(3) 0.0178(13) Uani 1 1 d . . . C20 C -0.2428(5) 0.5104(2) 0.4178(3) 0.0191(13) Uani 1 1 d . . . C21 C -0.3460(5) 0.4643(2) 0.4143(4) 0.0295(15) Uani 1 1 d . . . H21A H -0.3918 0.4653 0.4609 0.044 Uiso 1 1 calc R . . H21B H -0.3003 0.4292 0.4114 0.044 Uiso 1 1 calc R . . H21C H -0.4118 0.4689 0.3682 0.044 Uiso 1 1 calc R . . C22 C -0.3177(5) 0.5633(2) 0.4312(3) 0.0241(13) Uani 1 1 d . . . H22A H -0.2550 0.5940 0.4336 0.036 Uiso 1 1 calc R . . H22B H -0.3565 0.5608 0.4801 0.036 Uiso 1 1 calc R . . H22C H -0.3895 0.5689 0.3884 0.036 Uiso 1 1 calc R . . C23 C 0.1702(5) 0.5649(2) 0.2930(3) 0.0228(13) Uani 1 1 d . . . H23 H 0.1623 0.6020 0.3155 0.027 Uiso 1 1 calc R . . C24 C 0.2251(6) 0.5713(3) 0.2147(3) 0.0311(14) Uani 1 1 d . . . H24A H 0.3131 0.5890 0.2228 0.047 Uiso 1 1 calc R . . H24B H 0.1631 0.5937 0.1799 0.047 Uiso 1 1 calc R . . H24C H 0.2339 0.5354 0.1913 0.047 Uiso 1 1 calc R . . C25 C 0.2676(6) 0.5322(3) 0.3492(4) 0.0342(16) Uani 1 1 d . . . H25A H 0.3562 0.5495 0.3541 0.051 Uiso 1 1 calc R . . H25B H 0.2741 0.4950 0.3297 0.051 Uiso 1 1 calc R . . H25C H 0.2350 0.5312 0.4001 0.051 Uiso 1 1 calc R . . C26 C 0.0524(5) 0.7186(2) 0.3161(3) 0.0194(13) Uani 1 1 d . . . H26 H 0.1182 0.7236 0.3636 0.023 Uiso 1 1 calc R . . C27 C -0.0246(6) 0.7717(2) 0.3064(4) 0.0239(14) Uani 1 1 d . . . H27A H -0.0785 0.7763 0.3500 0.029 Uiso 1 1 calc R . . H27B H -0.0869 0.7707 0.2576 0.029 Uiso 1 1 calc R . . C28 C 0.0716(6) 0.8198(2) 0.3044(4) 0.0351(17) Uani 1 1 d . . . H28A H 0.0190 0.8538 0.2956 0.042 Uiso 1 1 calc R . . H28B H 0.1274 0.8228 0.3553 0.042 Uiso 1 1 calc R . . C29 C 0.1620(6) 0.8135(2) 0.2413(4) 0.0338(16) Uani 1 1 d . . . H29A H 0.2283 0.8435 0.2452 0.041 Uiso 1 1 calc R . . H29B H 0.1076 0.8160 0.1899 0.041 Uiso 1 1 calc R . . C30 C 0.2351(6) 0.7593(2) 0.2483(4) 0.0298(15) Uani 1 1 d . . . H30A H 0.2989 0.7590 0.2965 0.036 Uiso 1 1 calc R . . H30B H 0.2872 0.7549 0.2039 0.036 Uiso 1 1 calc R . . C31 C 0.1377(6) 0.7116(2) 0.2497(4) 0.0293(15) Uani 1 1 d . . . H31A H 0.1887 0.6771 0.2565 0.035 Uiso 1 1 calc R . . H31B H 0.0787 0.7098 0.1998 0.035 Uiso 1 1 calc R . . C32 C -0.1545(5) 0.6550(2) 0.2824(3) 0.0174(13) Uani 1 1 d . . . H32 H -0.1787 0.6183 0.3012 0.021 Uiso 1 1 calc R . . C33 C -0.2777(5) 0.6908(2) 0.2909(3) 0.0255(14) Uani 1 1 d . . . H33A H -0.2877 0.6953 0.3465 0.031 Uiso 1 1 calc R . . H33B H -0.2650 0.7273 0.2688 0.031 Uiso 1 1 calc R . . C34 C -0.4037(6) 0.6647(2) 0.2490(3) 0.0291(15) Uani 1 1 d . . . H34A H -0.4209 0.6298 0.2747 0.035 Uiso 1 1 calc R . . H34B H -0.4813 0.6889 0.2527 0.035 Uiso 1 1 calc R . . C35 C -0.3904(6) 0.6541(2) 0.1643(3) 0.0293(15) Uani 1 1 d . . . H35A H -0.4711 0.6347 0.1400 0.035 Uiso 1 1 calc R . . H35B H -0.3845 0.6893 0.1371 0.035 Uiso 1 1 calc R . . C36 C -0.2671(6) 0.6204(2) 0.1558(3) 0.0273(15) Uani 1 1 d . . . H36A H -0.2575 0.6163 0.1001 0.033 Uiso 1 1 calc R . . H36B H -0.2780 0.5837 0.1776 0.033 Uiso 1 1 calc R . . C37 C -0.1405(5) 0.6469(2) 0.1974(3) 0.0210(13) Uani 1 1 d . . . H37A H -0.0620 0.6234 0.1923 0.025 Uiso 1 1 calc R . . H37B H -0.1255 0.6824 0.1732 0.025 Uiso 1 1 calc R . . C38 C -0.5901(19) 0.3868(7) 0.2048(12) 0.048(6) Uani 0.488(16) 1 d PD A 1 C38' C -0.539(2) 0.3830(9) 0.1682(13) 0.073(9) Uani 0.512(16) 1 d PD A 2 C39 C -0.556(4) 0.4386(8) 0.184(2) 0.063(11) Uani 0.488(16) 1 d PDU A 1 H39 H -0.5925 0.4689 0.2078 0.075 Uiso 0.488(16) 1 calc PR A 1 C39' C -0.543(3) 0.4360(9) 0.1942(17) 0.058(9) Uani 0.512(16) 1 d PDU A 2 H39' H -0.5759 0.4429 0.2423 0.069 Uiso 0.512(16) 1 calc PR A 2 C40 C -0.4701(17) 0.4482(7) 0.1285(11) 0.050(6) Uani 0.488(16) 1 d PD A 1 H40 H -0.4475 0.4843 0.1156 0.061 Uiso 0.488(16) 1 calc PR A 1 C40' C -0.5015(19) 0.4796(9) 0.1516(12) 0.083(8) Uani 0.512(16) 1 d PD A 2 H40' H -0.5132 0.5160 0.1680 0.100 Uiso 0.512(16) 1 calc PR A 2 C41 C -0.418(2) 0.4041(9) 0.0923(13) 0.052(7) Uani 0.488(16) 1 d PD A 1 H41 H -0.3564 0.4095 0.0556 0.063 Uiso 0.488(16) 1 calc PR A 1 C41' C -0.443(2) 0.4693(10) 0.0857(14) 0.110(10) Uani 0.512(16) 1 d PD A 2 H41' H -0.4037 0.4979 0.0595 0.132 Uiso 0.512(16) 1 calc PR A 2 C42 C -0.456(4) 0.3522(9) 0.110(2) 0.065(10) Uani 0.488(16) 1 d PD A 1 H42 H -0.4241 0.3221 0.0840 0.078 Uiso 0.488(16) 1 calc PR A 1 C42' C -0.443(3) 0.4157(10) 0.0579(15) 0.094(11) Uani 0.512(16) 1 d PD A 2 H42' H -0.4151 0.4088 0.0086 0.113 Uiso 0.512(16) 1 calc PR A 2 C43 C -0.540(2) 0.3433(8) 0.1658(12) 0.052(6) Uani 0.488(16) 1 d PD A 1 H43 H -0.5633 0.3071 0.1776 0.062 Uiso 0.488(16) 1 calc PR A 1 C43' C -0.483(3) 0.3730(11) 0.1010(19) 0.073(11) Uani 0.512(16) 1 d PD A 2 H43' H -0.4718 0.3366 0.0844 0.087 Uiso 0.512(16) 1 calc PR A 2 C44 C -0.6860(18) 0.3776(9) 0.2590(11) 0.079(7) Uani 0.488(16) 1 d P A 1 H44A H -0.6799 0.3398 0.2769 0.118 Uiso 0.488(16) 1 calc PR A 1 H44B H -0.7767 0.3849 0.2334 0.118 Uiso 0.488(16) 1 calc PR A 1 H44C H -0.6663 0.4021 0.3035 0.118 Uiso 0.488(16) 1 calc PR A 1 C44' C -0.585(3) 0.3391(11) 0.2117(15) 0.104(10) Uani 0.512(16) 1 d P A 2 H44D H -0.6707 0.3256 0.1853 0.156 Uiso 0.512(16) 1 calc PR A 2 H44E H -0.5983 0.3520 0.2636 0.156 Uiso 0.512(16) 1 calc PR A 2 H44F H -0.5190 0.3097 0.2161 0.156 Uiso 0.512(16) 1 calc PR A 2 C45 C -0.0490(16) 0.5279(6) -0.0212(9) 0.047(4) Uani 0.50 1 d PDU B -1 C46 C -0.101(3) 0.4786(10) -0.001(2) 0.051(6) Uani 0.50 1 d PDU B -1 H46 H -0.1947 0.4722 -0.0097 0.061 Uiso 0.50 1 calc PR B -1 C47 C -0.015(3) 0.4389(7) 0.0313(12) 0.086(9) Uani 0.50 1 d PD B -1 H47 H -0.0511 0.4066 0.0507 0.103 Uiso 0.50 1 calc PR B -1 C48 C 0.122(3) 0.4453(11) 0.036(2) 0.092(10) Uani 0.50 1 d PDU B -1 H48 H 0.1810 0.4158 0.0515 0.111 Uiso 0.50 1 calc PR B -1 C49 C 0.1737(19) 0.4956(9) 0.0181(11) 0.072(5) Uani 0.50 1 d PDU B -1 H49 H 0.2674 0.5023 0.0265 0.087 Uiso 0.50 1 calc PR B -1 C50 C 0.086(2) 0.5356(11) -0.012(2) 0.054(6) Uani 0.50 1 d PDU B -1 H50 H 0.1207 0.5694 -0.0270 0.065 Uiso 0.50 1 calc PR B -1 C51 C -0.134(3) 0.5687(13) -0.0596(19) 0.085(9) Uani 0.50 1 d P B -1 H51A H -0.0984 0.6048 -0.0442 0.128 Uiso 0.50 1 calc PR B -1 H51B H -0.2245 0.5649 -0.0451 0.128 Uiso 0.50 1 calc PR B -1 H51C H -0.1364 0.5645 -0.1158 0.128 Uiso 0.50 1 calc PR B -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 0.02007(12) 0.01503(10) 0.01514(11) 0.00213(12) 0.00252(8) 0.00106(12) O1 0.018(2) 0.019(2) 0.018(2) 0.0062(17) -0.0002(17) 0.0012(16) N1 0.013(2) 0.018(2) 0.016(3) 0.004(2) 0.001(2) 0.002(2) N2 0.017(2) 0.014(2) 0.013(3) 0.005(2) 0.004(2) 0.0028(19) N3 0.018(2) 0.013(2) 0.015(3) 0.002(2) 0.002(2) -0.0016(19) C1 0.007(3) 0.013(3) 0.021(3) 0.000(3) 0.009(2) 0.000(2) C2 0.021(3) 0.018(3) 0.014(3) -0.001(3) 0.004(2) -0.003(3) C3 0.021(3) 0.020(3) 0.017(3) 0.002(3) 0.003(3) -0.001(3) C4 0.024(3) 0.027(3) 0.023(4) -0.003(3) 0.007(3) -0.006(3) C5 0.033(4) 0.026(3) 0.018(3) -0.008(3) 0.003(3) -0.011(3) C6 0.028(3) 0.023(3) 0.015(3) -0.003(3) 0.006(3) 0.001(3) C7 0.018(3) 0.026(3) 0.007(3) -0.002(3) 0.002(2) -0.001(3) C8 0.017(3) 0.023(3) 0.030(4) 0.002(3) 0.002(3) -0.003(3) C9 0.034(4) 0.039(4) 0.034(4) 0.006(3) 0.017(3) 0.013(3) C10 0.017(3) 0.041(4) 0.040(4) 0.002(3) -0.002(3) -0.002(3) C11 0.021(3) 0.029(3) 0.019(3) -0.013(3) 0.000(3) -0.001(3) C12 0.024(3) 0.026(3) 0.044(4) -0.007(3) 0.013(3) -0.002(3) C13 0.019(3) 0.052(4) 0.026(4) -0.004(3) 0.001(3) 0.008(3) C14 0.024(3) 0.010(3) 0.016(3) 0.007(2) -0.003(3) 0.004(2) C15 0.016(3) 0.012(3) 0.021(3) 0.006(3) -0.003(2) 0.002(2) C16 0.022(3) 0.017(3) 0.033(4) 0.007(3) -0.009(3) -0.003(3) C17 0.047(4) 0.018(3) 0.023(4) -0.006(3) -0.008(3) 0.003(3) C18 0.031(4) 0.016(3) 0.029(4) -0.002(3) 0.002(3) 0.007(3) C19 0.024(3) 0.009(3) 0.020(3) 0.001(3) 0.002(3) 0.005(2) C20 0.017(3) 0.018(3) 0.021(3) 0.006(3) 0.000(3) 0.001(2) C21 0.019(3) 0.031(3) 0.036(4) 0.012(3) -0.004(3) -0.007(3) C22 0.016(3) 0.027(3) 0.029(3) 0.010(3) 0.003(3) -0.002(3) C23 0.023(3) 0.021(3) 0.026(3) -0.002(3) 0.011(3) 0.007(3) C24 0.033(3) 0.034(3) 0.030(4) 0.006(3) 0.017(3) 0.004(3) C25 0.023(3) 0.048(4) 0.033(4) 0.002(3) 0.007(3) 0.000(3) C26 0.024(3) 0.016(3) 0.018(3) 0.002(3) 0.003(3) -0.007(3) C27 0.029(3) 0.017(3) 0.028(4) 0.001(3) 0.011(3) 0.002(3) C28 0.042(4) 0.013(3) 0.051(5) 0.004(3) 0.009(4) -0.001(3) C29 0.032(4) 0.028(4) 0.042(4) 0.014(3) 0.007(3) -0.014(3) C30 0.034(4) 0.030(3) 0.027(4) 0.004(3) 0.013(3) -0.007(3) C31 0.037(4) 0.026(3) 0.027(4) -0.002(3) 0.014(3) -0.005(3) C32 0.019(3) 0.012(3) 0.020(3) 0.000(3) -0.001(3) 0.000(2) C33 0.024(3) 0.029(3) 0.024(4) -0.001(3) 0.003(3) 0.004(3) C34 0.022(3) 0.036(4) 0.030(4) 0.003(3) 0.004(3) 0.004(3) C35 0.026(3) 0.034(4) 0.026(4) 0.005(3) -0.006(3) -0.004(3) C36 0.036(4) 0.029(3) 0.016(3) 0.002(3) 0.001(3) 0.001(3) C37 0.021(3) 0.025(3) 0.017(3) 0.001(3) 0.000(3) 0.000(3) C38 0.029(13) 0.068(15) 0.046(15) -0.003(12) -0.008(9) 0.005(11) C38' 0.041(16) 0.077(18) 0.09(2) -0.004(17) -0.036(14) -0.010(14) C39 0.062(19) 0.033(14) 0.09(2) -0.001(14) -0.003(17) 0.037(14) C39' 0.023(11) 0.09(2) 0.055(14) -0.033(16) -0.011(10) -0.018(14) C40 0.030(12) 0.053(12) 0.066(15) 0.006(11) -0.004(10) -0.009(10) C40' 0.040(12) 0.099(19) 0.11(2) -0.031(17) 0.010(12) 0.023(13) C41 0.041(13) 0.077(17) 0.037(13) -0.010(13) 0.000(11) 0.013(12) C41' 0.058(14) 0.13(2) 0.15(3) 0.02(2) 0.045(15) -0.037(15) C42 0.06(2) 0.041(13) 0.09(2) -0.021(13) 0.011(14) 0.018(12) C42' 0.09(2) 0.09(2) 0.10(3) -0.035(19) 0.007(19) -0.005(16) C43 0.045(12) 0.055(14) 0.056(16) -0.021(13) 0.004(11) 0.007(11) C43' 0.044(17) 0.09(2) 0.10(3) -0.05(2) 0.031(17) -0.01(2) C44 0.065(13) 0.104(17) 0.067(14) 0.027(12) 0.010(11) -0.003(12) C44' 0.11(2) 0.10(2) 0.09(2) 0.033(18) -0.039(18) 0.010(18) C45 0.049(9) 0.061(10) 0.034(9) -0.019(8) 0.016(8) 0.005(8) C46 0.054(12) 0.056(13) 0.044(14) 0.000(12) 0.013(11) -0.015(11) C47 0.18(3) 0.039(11) 0.049(14) -0.017(12) 0.048(17) -0.031(16) C48 0.119(19) 0.112(19) 0.046(18) -0.025(15) 0.010(15) 0.030(18) C49 0.087(12) 0.081(13) 0.050(11) -0.021(11) 0.014(10) 0.004(11) C50 0.064(12) 0.060(13) 0.038(13) -0.018(11) 0.009(10) -0.006(11) C51 0.091(17) 0.12(2) 0.037(19) -0.057(17) -0.009(11) 0.020(16) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 2.278(3) 3_566 ? Pb1 N2 2.282(4) . ? Pb1 O1 2.345(4) . ? Pb1 N1 2.633(4) . ? Pb1 Pb1 3.5974(4) 3_566 ? O1 C20 1.441(6) . ? O1 Pb1 2.278(3) 3_566 ? N1 C1 1.313(6) . ? N1 C2 1.401(7) . ? N2 C1 1.372(6) . ? N2 C14 1.412(6) . ? N3 C1 1.396(6) . ? N3 C32 1.487(6) . ? N3 C26 1.497(6) . ? C2 C7 1.412(7) . ? C2 C3 1.428(7) . ? C3 C4 1.384(7) . ? C3 C8 1.513(7) . ? C4 C5 1.378(8) . ? C5 C6 1.387(7) . ? C6 C7 1.391(7) . ? C7 C11 1.520(7) . ? C8 C9 1.522(8) . ? C8 C10 1.528(8) . ? C11 C12 1.519(8) . ? C11 C13 1.526(8) . ? C14 C15 1.419(7) . ? C14 C19 1.422(7) . ? C15 C16 1.398(8) . ? C15 C20 1.540(7) . ? C16 C17 1.383(8) . ? C17 C18 1.385(8) . ? C18 C19 1.381(7) . ? C19 C23 1.517(7) . ? C20 C21 1.532(7) . ? C20 C22 1.534(7) . ? C23 C25 1.523(8) . ? C23 C24 1.538(7) . ? C26 C27 1.516(7) . ? C26 C31 1.529(7) . ? C27 C28 1.529(7) . ? C28 C29 1.515(8) . ? C29 C30 1.519(8) . ? C30 C31 1.529(8) . ? C32 C37 1.515(7) . ? C32 C33 1.541(7) . ? C33 C34 1.523(8) . ? C34 C35 1.515(8) . ? C35 C36 1.512(8) . ? C36 C37 1.528(7) . ? C38 C39 1.382(16) . ? C38 C43 1.394(17) . ? C38 C44 1.44(2) . ? C38' C43' 1.377(17) . ? C38' C39' 1.381(17) . ? C38' C44' 1.43(3) . ? C39 C40 1.385(17) . ? C39' C40' 1.396(17) . ? C40 C41 1.388(17) . ? C40' C41' 1.372(16) . ? C41 C42 1.378(18) . ? C41' C42' 1.402(17) . ? C42 C43 1.367(17) . ? C42' C43' 1.377(17) . ? C45 C50 1.357(17) . ? C45 C46 1.379(13) . ? C45 C51 1.43(3) . ? C46 C47 1.375(13) . ? C47 C48 1.385(14) . ? C48 C49 1.388(14) . ? C49 C50 1.381(16) . ? 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 N2 90.20(13) 3_566 . ? O1 Pb1 O1 77.82(13) 3_566 . ? N2 Pb1 O1 76.67(13) . . ? O1 Pb1 N1 106.90(12) 3_566 . ? N2 Pb1 N1 53.45(14) . . ? O1 Pb1 N1 129.48(13) . . ? O1 Pb1 Pb1 39.58(9) 3_566 3_566 ? N2 Pb1 Pb1 81.48(10) . 3_566 ? O1 Pb1 Pb1 38.24(8) . 3_566 ? N1 Pb1 Pb1 126.77(9) . 3_566 ? C20 O1 Pb1 114.7(3) . 3_566 ? C20 O1 Pb1 119.1(3) . . ? Pb1 O1 Pb1 102.18(13) 3_566 . ? C1 N1 C2 130.1(5) . . ? C1 N1 Pb1 88.5(3) . . ? C2 N1 Pb1 131.4(3) . . ? C1 N2 C14 129.3(4) . . ? C1 N2 Pb1 102.8(3) . . ? C14 N2 Pb1 126.8(3) . . ? C1 N3 C32 119.3(4) . . ? C1 N3 C26 118.9(4) . . ? C32 N3 C26 121.8(4) . . ? N1 C1 N2 112.5(5) . . ? N1 C1 N3 126.9(4) . . ? N2 C1 N3 120.5(5) . . ? N1 C2 C7 123.7(5) . . ? N1 C2 C3 116.1(5) . . ? C7 C2 C3 119.9(5) . . ? C4 C3 C2 118.4(5) . . ? C4 C3 C8 121.2(5) . . ? C2 C3 C8 120.4(5) . . ? C5 C4 C3 121.9(5) . . ? C4 C5 C6 119.4(5) . . ? C5 C6 C7 121.6(5) . . ? C6 C7 C2 118.5(5) . . ? C6 C7 C11 121.0(5) . . ? C2 C7 C11 120.2(5) . . ? C3 C8 C9 112.3(5) . . ? C3 C8 C10 111.2(5) . . ? C9 C8 C10 112.0(5) . . ? C12 C11 C7 110.1(5) . . ? C12 C11 C13 109.7(5) . . ? C7 C11 C13 114.2(5) . . ? N2 C14 C15 117.5(5) . . ? N2 C14 C19 122.4(5) . . ? C15 C14 C19 119.9(5) . . ? C16 C15 C14 118.5(5) . . ? C16 C15 C20 120.3(5) . . ? C14 C15 C20 120.9(5) . . ? C17 C16 C15 121.2(5) . . ? C16 C17 C18 119.0(6) . . ? C19 C18 C17 122.6(5) . . ? C18 C19 C14 117.8(5) . . ? C18 C19 C23 120.7(5) . . ? C14 C19 C23 121.3(5) . . ? O1 C20 C21 106.5(4) . . ? O1 C20 C22 109.6(4) . . ? C21 C20 C22 106.9(4) . . ? O1 C20 C15 107.4(4) . . ? C21 C20 C15 112.7(5) . . ? C22 C20 C15 113.4(4) . . ? C19 C23 C25 109.3(5) . . ? C19 C23 C24 113.4(5) . . ? C25 C23 C24 110.5(4) . . ? N3 C26 C27 115.0(4) . . ? N3 C26 C31 115.4(4) . . ? C27 C26 C31 109.8(5) . . ? C26 C27 C28 110.6(5) . . ? C29 C28 C27 112.0(5) . . ? C28 C29 C30 110.9(5) . . ? C29 C30 C31 111.7(5) . . ? C30 C31 C26 110.2(5) . . ? N3 C32 C37 115.7(4) . . ? N3 C32 C33 115.7(4) . . ? C37 C32 C33 109.9(5) . . ? C34 C33 C32 110.1(5) . . ? C35 C34 C33 111.7(5) . . ? C36 C35 C34 111.1(5) . . ? C35 C36 C37 111.4(5) . . ? C32 C37 C36 110.3(4) . . ? C39 C38 C43 117.3(18) . . ? C39 C38 C44 121.6(17) . . ? C43 C38 C44 120.7(18) . . ? C43' C38' C39' 118.7(18) . . ? C43' C38' C44' 121(2) . . ? C39' C38' C44' 121(2) . . ? C38 C39 C40 122.5(16) . . ? C38' C39' C40' 121.6(18) . . ? C39 C40 C41 118.9(16) . . ? C41' C40' C39' 119.2(18) . . ? C42 C41 C40 119.0(18) . . ? C40' C41' C42' 118.6(18) . . ? C43 C42 C41 121.5(19) . . ? C43' C42' C41' 121(2) . . ? C42 C43 C38 120.6(19) . . ? C42' C43' C38' 120(2) . . ? C50 C45 C46 119.6(14) . . ? C50 C45 C51 119(2) . . ? C46 C45 C51 121(2) . . ? C47 C46 C45 119.4(16) . . ? C46 C47 C48 120.8(18) . . ? C47 C48 C49 118.9(19) . . ? C50 C49 C48 118.8(19) . . ? C45 C50 C49 121.8(18) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.196 _refine_diff_density_min -0.995 _refine_diff_density_rms 0.144 # Attachment 'PBFISOABnew.CIF' data_pbfisoab _database_code_depnum_ccdc_archive 'CCDC 677775' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C50 H70 N4 Pb' _chemical_formula_sum 'C50 H70 N4 Pb' _chemical_formula_weight 934.29 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' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 14.9163(3) _cell_length_b 16.1789(3) _cell_length_c 20.8178(5) _cell_angle_alpha 90.00 _cell_angle_beta 110.0900(10) _cell_angle_gamma 90.00 _cell_volume 4718.26(17) _cell_formula_units_Z 4 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.315 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1920 _exptl_absorpt_coefficient_mu 3.611 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.41 _exptl_absorpt_correction_T_max 0.69 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius KAPPA CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 25834 _diffrn_reflns_av_R_equivalents 0.0723 _diffrn_reflns_av_sigmaI/netI 0.0893 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.45 _diffrn_reflns_theta_max 25.00 _reflns_number_total 8289 _reflns_number_gt 5824 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo SMN (Otwinoski and Minor, 1997)' _computing_data_reduction 'Denzo SMN (Otwinoski and Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Carbon atoms C12 and C13 were modelled as disordered over two positions (occupancies set at 0.75:0.25) after trial refinement). The Uij values of the disordered components were restrained to be similar. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0780P)^2^+2.9509P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8289 _refine_ls_number_parameters 502 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0959 _refine_ls_R_factor_gt 0.0576 _refine_ls_wR_factor_ref 0.1455 _refine_ls_wR_factor_gt 0.1298 _refine_ls_goodness_of_fit_ref 1.053 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.25564(2) 0.723746(17) 0.059013(14) 0.02487(13) Uani 1 1 d . . . N1 N 0.0948(5) 0.7043(3) 0.0650(3) 0.0244(15) Uani 1 1 d . . . N2 N 0.2121(5) 0.6161(3) 0.1168(3) 0.0240(15) Uani 1 1 d . . . N3 N 0.4095(4) 0.7436(4) 0.1521(3) 0.0221(14) Uani 1 1 d . . . N4 N 0.2867(4) 0.8286(4) 0.1426(3) 0.0251(15) Uani 1 1 d . . . C1 C 0.1212(6) 0.6338(5) 0.0952(4) 0.0255(18) Uani 1 1 d . . . H1 H 0.0759 0.5962 0.1013 0.031 Uiso 1 1 calc R . . C2 C -0.0043(6) 0.7247(4) 0.0328(4) 0.0271(19) Uani 1 1 d . A . C3 C -0.0541(6) 0.7607(5) 0.0709(5) 0.035(2) Uani 1 1 d . . . C4 C -0.1506(6) 0.7827(6) 0.0387(5) 0.049(3) Uani 1 1 d . . . H4 H -0.1857 0.8056 0.0648 0.059 Uiso 1 1 calc R . . C5 C -0.1938(8) 0.7712(6) -0.0302(6) 0.056(3) Uani 1 1 d . . . H5 H -0.2590 0.7857 -0.0518 0.067 Uiso 1 1 calc R . . C6 C -0.1426(7) 0.7386(6) -0.0682(5) 0.047(3) Uani 1 1 d . A . H6 H -0.1731 0.7325 -0.1161 0.056 Uiso 1 1 calc R . . C7 C -0.0488(6) 0.7147(5) -0.0389(4) 0.034(2) Uani 1 1 d . . . C8 C -0.0079(6) 0.7752(5) 0.1482(4) 0.034(2) Uani 1 1 d . . . H8 H 0.0627 0.7693 0.1600 0.041 Uiso 1 1 calc R . . C9 C -0.0267(8) 0.8612(6) 0.1683(5) 0.058(3) Uani 1 1 d . . . H9A H -0.0950 0.8677 0.1601 0.087 Uiso 1 1 calc R . . H9B H -0.0066 0.9017 0.1409 0.087 Uiso 1 1 calc R . . H9C H 0.0094 0.8700 0.2169 0.087 Uiso 1 1 calc R . . C10 C -0.0392(10) 0.7102(7) 0.1863(6) 0.078(4) Uani 1 1 d . . . H10A H -0.0007 0.7136 0.2350 0.117 Uiso 1 1 calc R . . H10B H -0.0308 0.6557 0.1687 0.117 Uiso 1 1 calc R . . H10C H -0.1066 0.7185 0.1804 0.117 Uiso 1 1 calc R . . C11 C 0.0067(7) 0.6789(6) -0.0794(4) 0.049(3) Uani 0.75 1 d P A 1 H11 H 0.0758 0.6926 -0.0571 0.058 Uiso 0.75 1 calc PR A 1 C12 C -0.0271(12) 0.7078(10) -0.1527(7) 0.069(4) Uani 0.75 1 d PU A 1 H12A H 0.0124 0.6826 -0.1766 0.104 Uiso 0.75 1 calc PR A 1 H12B H -0.0219 0.7681 -0.1540 0.104 Uiso 0.75 1 calc PR A 1 H12C H -0.0939 0.6915 -0.1753 0.104 Uiso 0.75 1 calc PR A 1 C12' C 0.052(4) 0.761(3) -0.111(2) 0.069(4) Uani 0.25 1 d PU A 2 H12D H 0.0899 0.7404 -0.1378 0.104 Uiso 0.25 1 calc PR A 2 H12E H 0.0933 0.7942 -0.0725 0.104 Uiso 0.25 1 calc PR A 2 H12F H -0.0002 0.7953 -0.1397 0.104 Uiso 0.25 1 calc PR A 2 C13 C -0.0071(12) 0.5815(8) -0.0813(8) 0.068(4) Uani 0.75 1 d PU A 1 H13A H 0.0291 0.5564 -0.1076 0.102 Uiso 0.75 1 calc PR A 1 H13B H -0.0750 0.5682 -0.1029 0.102 Uiso 0.75 1 calc PR A 1 H13C H 0.0160 0.5598 -0.0345 0.102 Uiso 0.75 1 calc PR A 1 C13' C -0.041(3) 0.623(3) -0.140(2) 0.068(4) Uani 0.25 1 d PU A 2 H13D H 0.0062 0.6050 -0.1603 0.102 Uiso 0.25 1 calc PR A 2 H13E H -0.0928 0.6524 -0.1741 0.102 Uiso 0.25 1 calc PR A 2 H13F H -0.0669 0.5739 -0.1244 0.102 Uiso 0.25 1 calc PR A 2 C14 C 0.2498(5) 0.5392(4) 0.1493(4) 0.0258(19) Uani 1 1 d . . . C15 C 0.2474(6) 0.5197(4) 0.2146(4) 0.0277(19) Uani 1 1 d . . . C16 C 0.2824(6) 0.4431(5) 0.2421(5) 0.037(2) Uani 1 1 d . . . H16 H 0.2778 0.4276 0.2849 0.044 Uiso 1 1 calc R . . C17 C 0.3232(6) 0.3893(5) 0.2094(5) 0.042(2) Uani 1 1 d . . . H17 H 0.3483 0.3381 0.2302 0.050 Uiso 1 1 calc R . . C18 C 0.3278(6) 0.4094(5) 0.1462(5) 0.039(2) Uani 1 1 d . . . H18 H 0.3568 0.3722 0.1239 0.047 Uiso 1 1 calc R . . C19 C 0.2906(6) 0.4829(5) 0.1152(4) 0.032(2) Uani 1 1 d . . . C20 C 0.2052(6) 0.5776(5) 0.2544(4) 0.036(2) Uani 1 1 d . . . H20 H 0.1848 0.6293 0.2269 0.043 Uiso 1 1 calc R . . C21 C 0.2804(7) 0.6015(6) 0.3237(5) 0.048(3) Uani 1 1 d . . . H21A H 0.3052 0.5514 0.3503 0.072 Uiso 1 1 calc R . . H21B H 0.2510 0.6371 0.3490 0.072 Uiso 1 1 calc R . . H21C H 0.3330 0.6313 0.3158 0.072 Uiso 1 1 calc R . . C22 C 0.1186(7) 0.5413(6) 0.2654(5) 0.056(3) Uani 1 1 d . . . H22A H 0.0703 0.5280 0.2211 0.084 Uiso 1 1 calc R . . H22B H 0.0924 0.5814 0.2895 0.084 Uiso 1 1 calc R . . H22C H 0.1369 0.4908 0.2929 0.084 Uiso 1 1 calc R . . C23 C 0.2935(7) 0.5048(5) 0.0439(4) 0.040(2) Uani 1 1 d . . . H23 H 0.2502 0.5529 0.0255 0.048 Uiso 1 1 calc R . . C24 C 0.3929(10) 0.5288(10) 0.0486(7) 0.101(5) Uani 1 1 d . . . H24A H 0.4210 0.5644 0.0886 0.151 Uiso 1 1 calc R . . H24B H 0.3905 0.5586 0.0071 0.151 Uiso 1 1 calc R . . H24C H 0.4319 0.4789 0.0534 0.151 Uiso 1 1 calc R . . C25 C 0.2614(13) 0.4340(9) -0.0060(6) 0.124(6) Uani 1 1 d . . . H25A H 0.3130 0.3934 0.0030 0.185 Uiso 1 1 calc R . . H25B H 0.2451 0.4549 -0.0528 0.185 Uiso 1 1 calc R . . H25C H 0.2052 0.4077 -0.0007 0.185 Uiso 1 1 calc R . . C26 C 0.3782(6) 0.8129(4) 0.1684(4) 0.0235(18) Uani 1 1 d . . . H26 H 0.4208 0.8510 0.1984 0.028 Uiso 1 1 calc R . . C27 C 0.5066(6) 0.7263(4) 0.1667(4) 0.0240(18) Uani 1 1 d . . . C28 C 0.5567(6) 0.7579(5) 0.1247(4) 0.034(2) Uani 1 1 d . . . C29 C 0.6508(7) 0.7364(6) 0.1400(6) 0.056(3) Uani 1 1 d . . . H29 H 0.6848 0.7572 0.1123 0.067 Uiso 1 1 calc R . . C30 C 0.6979(7) 0.6850(7) 0.1949(6) 0.064(3) Uani 1 1 d . . . H30 H 0.7632 0.6710 0.2049 0.077 Uiso 1 1 calc R . . C31 C 0.6488(6) 0.6555(6) 0.2336(5) 0.047(3) Uani 1 1 d . . . H31 H 0.6813 0.6201 0.2707 0.057 Uiso 1 1 calc R . . C32 C 0.5547(6) 0.6734(5) 0.2226(4) 0.0289(19) Uani 1 1 d . . . C33 C 0.5044(7) 0.8093(5) 0.0621(4) 0.040(2) Uani 1 1 d . . . H33 H 0.4428 0.8278 0.0665 0.048 Uiso 1 1 calc R . . C34 C 0.5593(8) 0.8861(6) 0.0558(6) 0.072(4) Uani 1 1 d . . . H34A H 0.5742 0.9191 0.0977 0.108 Uiso 1 1 calc R . . H34B H 0.5203 0.9190 0.0166 0.108 Uiso 1 1 calc R . . H34C H 0.6187 0.8698 0.0490 0.108 Uiso 1 1 calc R . . C35 C 0.4806(10) 0.7562(8) -0.0015(6) 0.079(4) Uani 1 1 d . . . H35A H 0.4451 0.7892 -0.0417 0.118 Uiso 1 1 calc R . . H35B H 0.4414 0.7091 0.0025 0.118 Uiso 1 1 calc R . . H35C H 0.5397 0.7359 -0.0065 0.118 Uiso 1 1 calc R . . C36 C 0.5031(6) 0.6399(5) 0.2682(4) 0.0286(19) Uani 1 1 d . . . H36 H 0.4329 0.6472 0.2440 0.034 Uiso 1 1 calc R . . C37 C 0.5317(8) 0.6902(7) 0.3332(5) 0.064(3) Uani 1 1 d . . . H37A H 0.6004 0.6842 0.3575 0.096 Uiso 1 1 calc R . . H37B H 0.4967 0.6705 0.3624 0.096 Uiso 1 1 calc R . . H37C H 0.5165 0.7485 0.3220 0.096 Uiso 1 1 calc R . . C38 C 0.5226(7) 0.5484(5) 0.2845(5) 0.051(3) Uani 1 1 d . . . H38A H 0.5910 0.5402 0.3089 0.076 Uiso 1 1 calc R . . H38B H 0.5028 0.5166 0.2419 0.076 Uiso 1 1 calc R . . H38C H 0.4866 0.5297 0.3133 0.076 Uiso 1 1 calc R . . C39 C 0.2414(5) 0.8994(4) 0.1570(4) 0.0270(19) Uani 1 1 d . . . C40 C 0.1981(6) 0.9552(5) 0.1030(5) 0.033(2) Uani 1 1 d . . . C41 C 0.1502(6) 1.0228(5) 0.1169(5) 0.044(3) Uani 1 1 d . . . H41 H 0.1194 1.0608 0.0814 0.053 Uiso 1 1 calc R . . C42 C 0.1468(6) 1.0356(5) 0.1814(6) 0.045(3) Uani 1 1 d . . . H42 H 0.1132 1.0819 0.1896 0.054 Uiso 1 1 calc R . . C43 C 0.1907(6) 0.9828(5) 0.2333(5) 0.040(2) Uani 1 1 d . . . H43 H 0.1884 0.9935 0.2776 0.048 Uiso 1 1 calc R . . C44 C 0.2384(6) 0.9141(5) 0.2232(5) 0.032(2) Uani 1 1 d . . . C45 C 0.2048(7) 0.9417(5) 0.0331(5) 0.046(3) Uani 1 1 d . . . H45 H 0.2311 0.8848 0.0333 0.055 Uiso 1 1 calc R . . C46 C 0.2708(11) 0.9986(9) 0.0169(8) 0.106(5) Uani 1 1 d U . . H46A H 0.3345 0.9934 0.0516 0.159 Uiso 1 1 calc R . . H46B H 0.2480 1.0554 0.0163 0.159 Uiso 1 1 calc R . . H46C H 0.2740 0.9848 -0.0281 0.159 Uiso 1 1 calc R . . C47 C 0.1095(11) 0.9428(11) -0.0217(8) 0.131(6) Uani 1 1 d U . . H47A H 0.0666 0.9045 -0.0099 0.196 Uiso 1 1 calc R . . H47B H 0.1159 0.9259 -0.0651 0.196 Uiso 1 1 calc R . . H47C H 0.0830 0.9988 -0.0263 0.196 Uiso 1 1 calc R . . C48 C 0.2877(7) 0.8571(5) 0.2838(4) 0.038(2) Uani 1 1 d . . . H48 H 0.3087 0.8065 0.2652 0.046 Uiso 1 1 calc R . . C49 C 0.3776(7) 0.8980(6) 0.3337(5) 0.054(3) Uani 1 1 d . . . H49A H 0.4226 0.9099 0.3100 0.081 Uiso 1 1 calc R . . H49B H 0.4076 0.8606 0.3721 0.081 Uiso 1 1 calc R . . H49C H 0.3600 0.9497 0.3510 0.081 Uiso 1 1 calc R . . C50 C 0.2195(8) 0.8291(7) 0.3206(5) 0.064(3) Uani 1 1 d . . . H50A H 0.1975 0.8774 0.3394 0.096 Uiso 1 1 calc R . . H50B H 0.2530 0.7911 0.3578 0.096 Uiso 1 1 calc R . . H50C H 0.1645 0.8008 0.2880 0.096 Uiso 1 1 calc R . . C11' C 0.0067(7) 0.6789(6) -0.0794(4) 0.049(3) Uani 0.25 1 d P A 2 H11' H 0.0618 0.6480 -0.0470 0.058 Uiso 0.25 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0255(2) 0.02958(19) 0.01743(18) 0.00000(13) 0.00462(13) -0.00265(15) N1 0.027(4) 0.022(3) 0.025(4) -0.003(3) 0.011(3) -0.003(3) N2 0.026(4) 0.019(3) 0.028(4) 0.003(3) 0.011(3) -0.003(3) N3 0.019(4) 0.028(3) 0.015(3) -0.002(3) 0.000(3) -0.001(3) N4 0.013(4) 0.029(3) 0.026(4) -0.001(3) -0.003(3) 0.002(3) C1 0.030(5) 0.027(4) 0.018(4) 0.001(3) 0.006(4) -0.004(4) C2 0.024(4) 0.024(4) 0.026(4) 0.005(3) -0.001(4) -0.002(4) C3 0.024(5) 0.036(5) 0.040(5) -0.002(4) 0.004(4) -0.003(4) C4 0.023(5) 0.069(7) 0.047(6) -0.005(5) 0.002(5) 0.007(5) C5 0.036(6) 0.056(7) 0.063(8) 0.000(5) 0.001(6) 0.008(5) C6 0.040(6) 0.059(6) 0.026(5) -0.005(4) -0.009(5) -0.003(5) C7 0.037(5) 0.033(4) 0.024(5) -0.001(4) 0.000(4) -0.008(4) C8 0.019(4) 0.049(5) 0.034(5) -0.002(4) 0.009(4) 0.008(4) C9 0.062(7) 0.050(6) 0.050(7) -0.009(5) 0.005(6) 0.006(5) C10 0.116(12) 0.069(8) 0.047(7) 0.009(6) 0.025(8) -0.008(7) C11 0.051(6) 0.065(6) 0.023(5) -0.015(5) 0.004(5) 0.000(5) C12 0.069(11) 0.112(13) 0.036(8) 0.006(7) 0.029(8) 0.022(9) C12' 0.069(11) 0.112(13) 0.036(8) 0.006(7) 0.029(8) 0.022(9) C13 0.086(11) 0.064(9) 0.049(9) -0.024(7) 0.015(9) 0.003(8) C13' 0.086(11) 0.064(9) 0.049(9) -0.024(7) 0.015(9) 0.003(8) C14 0.020(4) 0.024(4) 0.028(5) 0.004(3) 0.002(4) -0.003(4) C15 0.024(5) 0.025(4) 0.027(5) 0.001(3) 0.000(4) -0.011(4) C16 0.036(5) 0.032(5) 0.037(5) 0.004(4) 0.004(4) -0.005(4) C17 0.040(6) 0.027(5) 0.043(6) 0.007(4) -0.006(5) 0.001(4) C18 0.037(6) 0.032(5) 0.036(5) -0.002(4) -0.003(4) 0.009(4) C19 0.031(5) 0.025(4) 0.034(5) -0.001(4) 0.003(4) -0.001(4) C20 0.040(6) 0.043(5) 0.028(5) 0.011(4) 0.017(4) 0.000(4) C21 0.051(6) 0.047(5) 0.044(6) -0.012(4) 0.013(5) -0.003(5) C22 0.051(7) 0.072(7) 0.053(7) -0.010(5) 0.029(6) -0.015(6) C23 0.049(6) 0.039(5) 0.032(5) -0.003(4) 0.013(5) 0.011(5) C24 0.091(11) 0.158(14) 0.062(9) 0.028(9) 0.038(8) 0.003(10) C25 0.187(17) 0.132(12) 0.049(8) -0.030(8) 0.038(10) -0.069(12) C26 0.030(5) 0.023(4) 0.016(4) 0.000(3) 0.007(4) -0.009(4) C27 0.023(4) 0.022(4) 0.025(4) -0.006(3) 0.007(4) -0.002(4) C28 0.037(5) 0.033(4) 0.032(5) 0.002(4) 0.012(4) 0.000(4) C29 0.042(6) 0.059(7) 0.081(9) 0.007(6) 0.040(6) 0.005(5) C30 0.035(6) 0.060(7) 0.106(10) 0.025(7) 0.036(7) 0.024(5) C31 0.023(5) 0.050(6) 0.068(7) 0.021(5) 0.016(5) 0.014(4) C32 0.034(5) 0.023(4) 0.030(5) 0.002(4) 0.011(4) 0.000(4) C33 0.048(6) 0.047(5) 0.030(5) 0.002(4) 0.020(5) -0.004(5) C34 0.062(8) 0.062(7) 0.081(9) 0.030(6) 0.012(7) -0.010(6) C35 0.120(12) 0.080(8) 0.035(6) -0.005(6) 0.025(7) -0.006(8) C36 0.017(4) 0.035(4) 0.029(5) 0.004(4) 0.002(4) -0.003(4) C37 0.056(7) 0.095(8) 0.044(7) -0.020(6) 0.022(6) -0.030(6) C38 0.042(6) 0.048(5) 0.057(7) 0.015(5) 0.010(5) 0.006(5) C39 0.018(4) 0.023(4) 0.036(5) -0.006(3) 0.004(4) -0.003(3) C40 0.026(5) 0.026(4) 0.043(6) -0.004(4) 0.006(4) -0.005(4) C41 0.024(5) 0.029(5) 0.057(7) 0.005(4) -0.015(5) -0.003(4) C42 0.030(5) 0.028(5) 0.070(8) -0.018(5) 0.010(5) -0.002(4) C43 0.037(6) 0.035(5) 0.043(6) -0.011(4) 0.009(5) -0.005(4) C44 0.021(5) 0.027(4) 0.048(6) -0.003(4) 0.011(4) 0.001(4) C45 0.057(7) 0.035(5) 0.034(6) 0.008(4) 0.001(5) 0.012(5) C46 0.108(8) 0.132(9) 0.101(8) -0.030(7) 0.066(7) -0.024(7) C47 0.113(9) 0.185(10) 0.103(9) -0.001(8) 0.047(7) -0.021(8) C48 0.046(6) 0.045(5) 0.021(5) 0.000(4) 0.008(4) 0.013(4) C49 0.053(7) 0.065(7) 0.036(6) -0.001(5) 0.006(5) -0.006(5) C50 0.077(8) 0.078(7) 0.047(6) 0.006(6) 0.033(6) -0.013(7) C11' 0.051(6) 0.065(6) 0.023(5) -0.015(5) 0.004(5) 0.000(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N2 2.332(6) . ? Pb1 N4 2.359(6) . ? Pb1 N3 2.463(6) . ? Pb1 N1 2.465(7) . ? Pb1 C1 2.783(8) . ? Pb1 C26 2.784(7) . ? N1 C1 1.296(9) . ? N1 C2 1.436(10) . ? N2 C1 1.305(10) . ? N2 C14 1.435(9) . ? N3 C26 1.303(9) . ? N3 C27 1.403(10) . ? N4 C26 1.309(9) . ? N4 C39 1.413(9) . ? C2 C3 1.388(12) . ? C2 C7 1.419(11) . ? C3 C4 1.409(12) . ? C3 C8 1.536(12) . ? C4 C5 1.368(14) . ? C5 C6 1.379(14) . ? C6 C7 1.376(13) . ? C7 C11 1.487(13) . ? C8 C10 1.485(13) . ? C8 C9 1.506(11) . ? C11 C12 1.508(16) . ? C11 C13 1.588(16) . ? C14 C15 1.407(11) . ? C14 C19 1.415(11) . ? C15 C16 1.389(11) . ? C15 C20 1.523(12) . ? C16 C17 1.370(12) . ? C17 C18 1.380(12) . ? C18 C19 1.376(11) . ? C19 C23 1.541(12) . ? C20 C22 1.506(12) . ? C20 C21 1.543(12) . ? C23 C24 1.502(15) . ? C23 C25 1.509(14) . ? C27 C32 1.424(11) . ? C27 C28 1.426(12) . ? C28 C29 1.374(13) . ? C28 C33 1.516(12) . ? C29 C30 1.392(15) . ? C30 C31 1.348(13) . ? C31 C32 1.373(11) . ? C32 C36 1.513(11) . ? C33 C35 1.516(14) . ? C33 C34 1.518(13) . ? C36 C37 1.510(12) . ? C36 C38 1.525(11) . ? C39 C44 1.413(12) . ? C39 C40 1.414(11) . ? C40 C41 1.391(12) . ? C40 C45 1.508(12) . ? C41 C42 1.377(13) . ? C42 C43 1.357(13) . ? C43 C44 1.375(11) . ? C44 C48 1.531(11) . ? C45 C46 1.469(16) . ? C45 C47 1.487(17) . ? C48 C49 1.536(12) . ? C48 C50 1.538(13) . ? 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 N2 Pb1 N4 100.1(2) . . ? N2 Pb1 N3 92.4(2) . . ? N4 Pb1 N3 55.4(2) . . ? N2 Pb1 N1 55.3(2) . . ? N4 Pb1 N1 90.2(2) . . ? N3 Pb1 N1 129.6(2) . . ? N2 Pb1 C1 27.8(2) . . ? N4 Pb1 C1 98.9(2) . . ? N3 Pb1 C1 114.8(2) . . ? N1 Pb1 C1 27.8(2) . . ? N2 Pb1 C26 100.7(2) . . ? N4 Pb1 C26 28.0(2) . . ? N3 Pb1 C26 27.9(2) . . ? N1 Pb1 C26 113.7(2) . . ? C1 Pb1 C26 112.4(2) . . ? C1 N1 C2 121.4(7) . . ? C1 N1 Pb1 89.9(5) . . ? C2 N1 Pb1 144.1(5) . . ? C1 N2 C14 123.0(7) . . ? C1 N2 Pb1 95.7(5) . . ? C14 N2 Pb1 139.2(5) . . ? C26 N3 C27 123.4(6) . . ? C26 N3 Pb1 89.9(4) . . ? C27 N3 Pb1 139.4(5) . . ? C26 N4 C39 125.3(6) . . ? C26 N4 Pb1 94.4(5) . . ? C39 N4 Pb1 138.8(5) . . ? N1 C1 N2 117.8(7) . . ? N1 C1 Pb1 62.3(4) . . ? N2 C1 Pb1 56.5(4) . . ? C3 C2 C7 120.0(8) . . ? C3 C2 N1 119.8(7) . . ? C7 C2 N1 120.0(8) . . ? C2 C3 C4 119.6(8) . . ? C2 C3 C8 121.8(7) . . ? C4 C3 C8 118.5(8) . . ? C5 C4 C3 120.0(10) . . ? C4 C5 C6 119.9(9) . . ? C7 C6 C5 122.2(9) . . ? C6 C7 C2 118.1(9) . . ? C6 C7 C11 122.6(8) . . ? C2 C7 C11 119.4(8) . . ? C10 C8 C9 112.5(9) . . ? C10 C8 C3 109.9(8) . . ? C9 C8 C3 111.9(7) . . ? C7 C11 C12 113.3(9) . . ? C7 C11 C13 107.9(9) . . ? C12 C11 C13 106.7(10) . . ? C15 C14 C19 119.9(7) . . ? C15 C14 N2 121.0(7) . . ? C19 C14 N2 119.1(7) . . ? C16 C15 C14 117.9(8) . . ? C16 C15 C20 119.4(8) . . ? C14 C15 C20 122.6(7) . . ? C17 C16 C15 122.0(9) . . ? C16 C17 C18 120.0(8) . . ? C19 C18 C17 120.4(9) . . ? C18 C19 C14 119.7(8) . . ? C18 C19 C23 120.6(8) . . ? C14 C19 C23 119.7(7) . . ? C22 C20 C15 112.3(7) . . ? C22 C20 C21 110.0(7) . . ? C15 C20 C21 111.1(7) . . ? C24 C23 C25 108.4(11) . . ? C24 C23 C19 110.5(8) . . ? C25 C23 C19 112.4(8) . . ? N3 C26 N4 118.4(7) . . ? N3 C26 Pb1 62.2(4) . . ? N4 C26 Pb1 57.7(4) . . ? N3 C27 C32 119.4(7) . . ? N3 C27 C28 121.0(7) . . ? C32 C27 C28 119.6(7) . . ? C29 C28 C27 118.4(8) . . ? C29 C28 C33 121.4(9) . . ? C27 C28 C33 120.0(8) . . ? C28 C29 C30 121.9(10) . . ? C31 C30 C29 118.5(9) . . ? C30 C31 C32 124.0(9) . . ? C31 C32 C27 117.5(8) . . ? C31 C32 C36 122.1(7) . . ? C27 C32 C36 120.3(7) . . ? C35 C33 C28 109.7(8) . . ? C35 C33 C34 111.1(9) . . ? C28 C33 C34 112.9(8) . . ? C37 C36 C32 108.7(7) . . ? C37 C36 C38 110.4(8) . . ? C32 C36 C38 112.8(7) . . ? C44 C39 N4 121.4(7) . . ? C44 C39 C40 120.7(7) . . ? N4 C39 C40 117.9(7) . . ? C41 C40 C39 117.6(8) . . ? C41 C40 C45 121.6(8) . . ? C39 C40 C45 120.8(7) . . ? C42 C41 C40 121.0(8) . . ? C43 C42 C41 120.9(8) . . ? C42 C43 C44 121.4(9) . . ? C43 C44 C39 118.5(8) . . ? C43 C44 C48 119.2(8) . . ? C39 C44 C48 122.4(7) . . ? C46 C45 C47 110.8(11) . . ? C46 C45 C40 113.7(8) . . ? C47 C45 C40 112.1(10) . . ? C44 C48 C49 111.1(7) . . ? C44 C48 C50 112.1(8) . . ? C49 C48 C50 111.3(8) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 3.334 _refine_diff_density_min -1.512 _refine_diff_density_rms 0.176 # Attachment 'PBHDGCLnew.CIF' data_pbhdgcl _database_code_depnum_ccdc_archive 'CCDC 677776' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C74 H104 Cl2 N6 Pb2, 2(C7 H8)' _chemical_formula_sum 'C88 H120 Cl2 N6 Pb2' _chemical_formula_weight 1747.18 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.9449(4) _cell_length_b 13.1345(4) _cell_length_c 15.3776(7) _cell_angle_alpha 109.593(2) _cell_angle_beta 98.675(2) _cell_angle_gamma 95.682(3) _cell_volume 2032.06(13) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.07 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.428 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 888 _exptl_absorpt_coefficient_mu 4.250 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.58 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius KAPPA CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 21071 _diffrn_reflns_av_R_equivalents 0.1043 _diffrn_reflns_av_sigmaI/netI 0.1466 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.73 _diffrn_reflns_theta_max 25.00 _reflns_number_total 7131 _reflns_number_gt 4996 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo SMN (Otwinoski and Minor, 1997)' _computing_data_reduction 'Denzo SMN (Otwinoski and Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'CIFTAB (Sheldrick,1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. Refinement of ansiotropic thermal parameters of carbon atoms C1 and C2 was restrained to be similar to neighbourning atoms. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0254P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7131 _refine_ls_number_parameters 455 _refine_ls_number_restraints 12 _refine_ls_R_factor_all 0.1088 _refine_ls_R_factor_gt 0.0559 _refine_ls_wR_factor_ref 0.0871 _refine_ls_wR_factor_gt 0.0746 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.029 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.68323(3) 0.53092(3) 0.59367(2) 0.01806(11) Uani 1 1 d . . . Cl1 Cl 0.44952(15) 0.53957(17) 0.61033(12) 0.0290(5) Uani 1 1 d . . . N1 N 0.7486(4) 0.6663(4) 0.7495(4) 0.0118(11) Uani 1 1 d U . . N2 N 0.7775(4) 0.7109(4) 0.6241(4) 0.0108(13) Uani 1 1 d . . . N3 N 0.8818(5) 0.8320(5) 0.7791(4) 0.0163(14) Uani 1 1 d . . . C1 C 0.8049(6) 0.7381(6) 0.7178(5) 0.0110(11) Uani 1 1 d U . . C2 C 0.7748(5) 0.6692(6) 0.8435(5) 0.0128(12) Uani 1 1 d U . . C3 C 0.7327(5) 0.7485(6) 0.9149(5) 0.0128(12) Uani 1 1 d U . . C4 C 0.7534(6) 0.7443(6) 1.0050(5) 0.0226(19) Uani 1 1 d . . . H4 H 0.7264 0.7981 1.0538 0.027 Uiso 1 1 calc R . . C5 C 0.8118(6) 0.6649(6) 1.0258(5) 0.0236(19) Uani 1 1 d . . . H5 H 0.8253 0.6637 1.0879 0.028 Uiso 1 1 calc R . . C6 C 0.8500(6) 0.5876(6) 0.9548(5) 0.0220(19) Uani 1 1 d . . . H6 H 0.8901 0.5325 0.9689 0.026 Uiso 1 1 calc R . . C7 C 0.8327(6) 0.5864(6) 0.8634(5) 0.0162(18) Uani 1 1 d . . . C8 C 0.6582(6) 0.8334(6) 0.8955(5) 0.0189(18) Uani 1 1 d . . . H8 H 0.6919 0.8545 0.8460 0.023 Uiso 1 1 calc R . . C9 C 0.6674(7) 0.9389(7) 0.9804(5) 0.037(2) Uani 1 1 d . . . H9A H 0.6254 0.9227 1.0272 0.056 Uiso 1 1 calc R . . H9B H 0.6270 0.9925 0.9597 0.056 Uiso 1 1 calc R . . H9C H 0.7557 0.9691 1.0083 0.056 Uiso 1 1 calc R . . C10 C 0.5207(6) 0.7820(6) 0.8549(5) 0.032(2) Uani 1 1 d . . . H10A H 0.4853 0.7576 0.9008 0.048 Uiso 1 1 calc R . . H10B H 0.5150 0.7191 0.7969 0.048 Uiso 1 1 calc R . . H10C H 0.4738 0.8363 0.8409 0.048 Uiso 1 1 calc R . . C11 C 0.8681(6) 0.4929(6) 0.7856(5) 0.0176(18) Uani 1 1 d . . . H11 H 0.8861 0.5212 0.7353 0.021 Uiso 1 1 calc R . . C12 C 0.9831(6) 0.4482(6) 0.8175(5) 0.0240(19) Uani 1 1 d . . . H12A H 1.0532 0.5085 0.8486 0.036 Uiso 1 1 calc R . . H12B H 1.0054 0.3950 0.7626 0.036 Uiso 1 1 calc R . . H12C H 0.9646 0.4124 0.8616 0.036 Uiso 1 1 calc R . . C13 C 0.7555(6) 0.3999(6) 0.7421(5) 0.0244(19) Uani 1 1 d . . . H13A H 0.7730 0.3449 0.6861 0.037 Uiso 1 1 calc R . . H13B H 0.6810 0.4296 0.7243 0.037 Uiso 1 1 calc R . . H13C H 0.7408 0.3659 0.7882 0.037 Uiso 1 1 calc R . . C14 C 0.7883(6) 0.7864(6) 0.5760(5) 0.0152(17) Uani 1 1 d . . . C15 C 0.8857(6) 0.7868(6) 0.5261(5) 0.0165(17) Uani 1 1 d . . . C16 C 0.8933(6) 0.8617(6) 0.4793(5) 0.025(2) Uani 1 1 d . . . H16 H 0.9601 0.8653 0.4470 0.030 Uiso 1 1 calc R . . C17 C 0.8061(7) 0.9297(7) 0.4794(5) 0.031(2) Uani 1 1 d . . . H17 H 0.8130 0.9808 0.4482 0.037 Uiso 1 1 calc R . . C18 C 0.7088(7) 0.9232(6) 0.5250(5) 0.027(2) Uani 1 1 d . . . H18 H 0.6476 0.9694 0.5231 0.032 Uiso 1 1 calc R . . C19 C 0.6954(6) 0.8523(6) 0.5737(5) 0.0168(18) Uani 1 1 d . . . C20 C 0.9763(6) 0.7047(6) 0.5188(5) 0.0188(18) Uani 1 1 d . . . H20 H 0.9897 0.6909 0.5794 0.023 Uiso 1 1 calc R . . C21 C 0.9169(6) 0.5969(6) 0.4407(5) 0.027(2) Uani 1 1 d . . . H21A H 0.8365 0.5708 0.4529 0.041 Uiso 1 1 calc R . . H21B H 0.9726 0.5425 0.4386 0.041 Uiso 1 1 calc R . . H21C H 0.9032 0.6078 0.3802 0.041 Uiso 1 1 calc R . . C22 C 1.1044(6) 0.7441(7) 0.5029(5) 0.030(2) Uani 1 1 d . . . H22A H 1.1605 0.6912 0.5063 0.045 Uiso 1 1 calc R . . H22B H 1.1398 0.8156 0.5515 0.045 Uiso 1 1 calc R . . H22C H 1.0951 0.7507 0.4407 0.045 Uiso 1 1 calc R . . C23 C 0.5774(6) 0.8376(7) 0.6108(6) 0.031(2) Uani 1 1 d . . . H23 H 0.5912 0.7925 0.6515 0.037 Uiso 1 1 calc R . . C24 C 0.4702(6) 0.7751(7) 0.5292(6) 0.048(3) Uani 1 1 d . . . H24A H 0.4509 0.8202 0.4910 0.072 Uiso 1 1 calc R . . H24B H 0.3962 0.7578 0.5535 0.072 Uiso 1 1 calc R . . H24C H 0.4942 0.7071 0.4903 0.072 Uiso 1 1 calc R . . C25 C 0.5416(6) 0.9460(7) 0.6702(6) 0.040(2) Uani 1 1 d . . . H25A H 0.6087 0.9839 0.7252 0.060 Uiso 1 1 calc R . . H25B H 0.4637 0.9309 0.6911 0.060 Uiso 1 1 calc R . . H25C H 0.5297 0.9923 0.6321 0.060 Uiso 1 1 calc R . . C26 C 0.9930(6) 0.8863(6) 0.7626(4) 0.0135(17) Uani 1 1 d . . . C27 C 0.9938(6) 0.9915(6) 0.7603(5) 0.0175(18) Uani 1 1 d . . . C28 C 1.1030(6) 1.0440(6) 0.7492(5) 0.0199(18) Uani 1 1 d . . . H28 H 1.1050 1.1151 0.7459 0.024 Uiso 1 1 calc R . . C29 C 1.2090(6) 0.9954(6) 0.7427(5) 0.0245(19) Uani 1 1 d . . . H29 H 1.2833 1.0327 0.7352 0.029 Uiso 1 1 calc R . . C30 C 1.2061(6) 0.8907(7) 0.7475(5) 0.021(2) Uani 1 1 d . . . H30 H 1.2791 0.8572 0.7429 0.026 Uiso 1 1 calc R . . C31 C 1.0995(6) 0.8351(6) 0.7586(5) 0.0150(18) Uani 1 1 d . . . C32 C 0.8808(6) 1.0486(6) 0.7752(5) 0.0222(19) Uani 1 1 d . . . H32 H 0.8040 0.9919 0.7465 0.027 Uiso 1 1 calc R . . C33 C 0.8833(7) 1.0998(7) 0.8810(5) 0.037(2) Uani 1 1 d . . . H33A H 0.8884 1.0434 0.9093 0.055 Uiso 1 1 calc R . . H33B H 0.8067 1.1313 0.8908 0.055 Uiso 1 1 calc R . . H33C H 0.9563 1.1576 0.9105 0.055 Uiso 1 1 calc R . . C34 C 0.8709(7) 1.1351(6) 0.7308(6) 0.034(2) Uani 1 1 d . . . H34A H 0.9387 1.1970 0.7641 0.050 Uiso 1 1 calc R . . H34B H 0.7900 1.1605 0.7351 0.050 Uiso 1 1 calc R . . H34C H 0.8775 1.1039 0.6645 0.050 Uiso 1 1 calc R . . C35 C 1.1018(6) 0.7289(6) 0.7773(5) 0.0194(18) Uani 1 1 d . . . H35 H 1.0158 0.6849 0.7532 0.023 Uiso 1 1 calc R . . C36 C 1.1948(6) 0.6585(6) 0.7285(5) 0.026(2) Uani 1 1 d . . . H36A H 1.1826 0.6520 0.6623 0.039 Uiso 1 1 calc R . . H36B H 1.1798 0.5854 0.7323 0.039 Uiso 1 1 calc R . . H36C H 1.2809 0.6935 0.7601 0.039 Uiso 1 1 calc R . . C37 C 1.1342(7) 0.7559(7) 0.8844(5) 0.033(2) Uani 1 1 d . . . H37A H 1.1302 0.6877 0.8975 0.050 Uiso 1 1 calc R . . H37B H 1.0741 0.7992 0.9145 0.050 Uiso 1 1 calc R . . H37C H 1.2189 0.7978 0.9093 0.050 Uiso 1 1 calc R . . C38 C 0.5172(6) 0.4403(7) 0.8791(6) 0.033(2) Uani 1 1 d . . . H38 H 0.5507 0.5088 0.9276 0.040 Uiso 1 1 calc R . . C39 C 0.4346(7) 0.4375(8) 0.7996(7) 0.044(3) Uani 1 1 d . . . H39 H 0.4140 0.5038 0.7938 0.052 Uiso 1 1 calc R . . C40 C 0.3830(8) 0.3393(10) 0.7296(7) 0.055(3) Uani 1 1 d . . . H40 H 0.3244 0.3361 0.6761 0.066 Uiso 1 1 calc R . . C41 C 0.4186(8) 0.2458(9) 0.7392(7) 0.061(3) Uani 1 1 d . . . H41 H 0.3867 0.1774 0.6900 0.073 Uiso 1 1 calc R . . C42 C 0.4982(8) 0.2480(9) 0.8172(7) 0.050(3) Uani 1 1 d . . . H42 H 0.5177 0.1813 0.8227 0.059 Uiso 1 1 calc R . . C43 C 0.6443(7) 0.3477(8) 0.9709(6) 0.054(3) Uani 1 1 d . . . H43A H 0.6141 0.2898 0.9930 0.081 Uiso 1 1 calc R . . H43B H 0.6553 0.4190 1.0217 0.081 Uiso 1 1 calc R . . H43C H 0.7247 0.3352 0.9518 0.081 Uiso 1 1 calc R . . C44 C 0.5511(7) 0.3462(8) 0.8885(6) 0.037(2) Uani 1 1 d . . . H3 H 0.8948 0.8248 0.8335 0.044 Uiso 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 0.01941(15) 0.01225(18) 0.01830(17) 0.00286(13) -0.00049(11) -0.00106(12) Cl1 0.0201(9) 0.0436(15) 0.0182(11) 0.0076(11) 0.0014(8) -0.0019(10) N1 0.015(2) 0.007(3) 0.016(3) 0.005(2) 0.007(2) 0.004(2) N2 0.015(3) 0.006(4) 0.010(3) 0.004(3) -0.002(3) -0.003(3) N3 0.017(3) 0.016(4) 0.010(3) -0.002(3) 0.002(3) -0.004(3) C1 0.014(2) 0.006(3) 0.016(3) 0.005(2) 0.008(2) 0.005(2) C2 0.011(3) 0.010(3) 0.012(3) 0.000(3) 0.001(2) -0.004(2) C3 0.011(3) 0.010(3) 0.012(3) 0.000(3) 0.001(2) -0.004(2) C4 0.026(4) 0.017(5) 0.020(5) 0.002(4) 0.002(4) -0.003(4) C5 0.028(4) 0.027(6) 0.010(4) 0.003(4) -0.002(4) 0.001(4) C6 0.026(4) 0.020(5) 0.020(5) 0.007(4) 0.003(4) 0.004(4) C7 0.014(4) 0.010(5) 0.020(5) 0.004(4) -0.002(3) -0.007(3) C8 0.017(4) 0.018(5) 0.017(4) 0.000(4) 0.005(3) 0.001(4) C9 0.041(5) 0.034(6) 0.030(5) 0.001(5) 0.008(4) 0.015(5) C10 0.022(4) 0.029(6) 0.044(6) 0.009(5) 0.007(4) 0.007(4) C11 0.024(4) 0.016(5) 0.016(4) 0.006(4) 0.006(3) 0.009(4) C12 0.030(4) 0.017(5) 0.027(5) 0.010(4) 0.005(4) 0.005(4) C13 0.033(4) 0.015(5) 0.028(5) 0.011(4) 0.006(4) 0.003(4) C14 0.021(4) 0.010(5) 0.014(4) 0.003(4) 0.005(3) 0.002(4) C15 0.019(4) 0.011(5) 0.010(4) -0.005(4) -0.005(3) -0.005(4) C16 0.031(4) 0.027(6) 0.017(5) 0.009(4) 0.005(4) -0.003(4) C17 0.048(5) 0.017(5) 0.028(5) 0.012(5) 0.006(4) -0.001(5) C18 0.032(5) 0.016(5) 0.030(5) 0.008(5) -0.001(4) 0.004(4) C19 0.021(4) 0.009(5) 0.015(4) 0.002(4) -0.003(3) -0.005(4) C20 0.020(4) 0.020(5) 0.016(4) 0.005(4) 0.006(3) 0.000(4) C21 0.017(4) 0.031(6) 0.032(5) 0.007(5) 0.006(4) 0.007(4) C22 0.031(4) 0.033(6) 0.026(5) 0.008(5) 0.013(4) 0.001(4) C23 0.028(4) 0.035(6) 0.039(5) 0.019(5) 0.012(4) 0.014(5) C24 0.018(4) 0.037(7) 0.073(7) 0.004(6) 0.003(5) -0.004(4) C25 0.027(4) 0.032(6) 0.054(6) 0.006(5) 0.016(4) 0.000(4) C26 0.014(4) 0.014(5) 0.008(4) 0.000(4) 0.001(3) -0.009(4) C27 0.023(4) 0.015(5) 0.009(4) 0.001(4) 0.001(3) -0.007(4) C28 0.027(4) 0.013(5) 0.016(4) -0.001(4) 0.006(3) 0.004(4) C29 0.026(4) 0.018(5) 0.024(5) 0.004(4) 0.007(4) -0.012(4) C30 0.016(4) 0.034(6) 0.014(4) 0.007(4) 0.002(3) 0.012(4) C31 0.011(4) 0.016(5) 0.012(4) -0.002(4) 0.001(3) -0.005(4) C32 0.022(4) 0.026(6) 0.020(5) 0.005(4) 0.011(4) 0.008(4) C33 0.038(5) 0.024(6) 0.040(6) -0.001(5) 0.010(4) 0.006(4) C34 0.037(5) 0.013(5) 0.049(6) 0.010(5) 0.006(4) 0.004(4) C35 0.015(4) 0.011(5) 0.027(5) 0.002(4) 0.002(3) -0.004(4) C36 0.018(4) 0.013(5) 0.039(5) 0.000(4) 0.002(4) 0.003(4) C37 0.037(5) 0.024(6) 0.040(6) 0.022(5) -0.007(4) -0.002(4) C38 0.033(5) 0.032(6) 0.032(5) 0.006(5) 0.007(4) 0.009(5) C39 0.041(5) 0.046(8) 0.051(7) 0.027(6) 0.009(5) 0.010(5) C40 0.047(6) 0.069(9) 0.039(7) 0.027(7) -0.019(5) -0.019(6) C41 0.070(7) 0.048(8) 0.052(7) 0.023(7) -0.017(6) -0.028(6) C42 0.062(6) 0.044(8) 0.057(7) 0.034(7) 0.022(6) 0.000(6) C43 0.054(6) 0.062(8) 0.048(7) 0.023(6) 0.010(5) 0.010(6) C44 0.040(5) 0.045(7) 0.033(6) 0.020(6) 0.015(5) 0.008(5) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N2 2.346(5) . ? Pb1 N1 2.405(5) . ? Pb1 Cl1 2.6186(16) . ? Pb1 C1 2.803(8) . ? Pb1 Cl1 3.0365(17) 2_666 ? Cl1 Pb1 3.0365(17) 2_666 ? N1 C1 1.338(8) . ? N1 C2 1.417(7) . ? N2 C1 1.340(8) . ? N2 C14 1.429(8) . ? N3 C1 1.376(9) . ? N3 C26 1.448(8) . ? C2 C7 1.407(8) . ? C2 C3 1.409(9) . ? C3 C4 1.389(8) . ? C3 C8 1.526(8) . ? C4 C5 1.376(9) . ? C5 C6 1.369(9) . ? C6 C7 1.385(9) . ? C7 C11 1.529(9) . ? C8 C10 1.531(9) . ? C8 C9 1.534(10) . ? C11 C12 1.524(8) . ? C11 C13 1.537(9) . ? C14 C19 1.403(8) . ? C14 C15 1.405(8) . ? C15 C16 1.402(9) . ? C15 C20 1.524(9) . ? C16 C17 1.371(9) . ? C17 C18 1.371(9) . ? C18 C19 1.387(9) . ? C19 C23 1.510(9) . ? C20 C21 1.520(10) . ? C20 C22 1.530(8) . ? C23 C24 1.517(10) . ? C23 C25 1.536(10) . ? C26 C27 1.393(9) . ? C26 C31 1.401(8) . ? C27 C28 1.382(9) . ? C27 C32 1.516(9) . ? C28 C29 1.379(9) . ? C29 C30 1.399(9) . ? C30 C31 1.378(9) . ? C31 C35 1.518(9) . ? C32 C34 1.513(9) . ? C32 C33 1.533(9) . ? C35 C37 1.540(9) . ? C35 C36 1.552(9) . ? C38 C44 1.372(10) . ? C38 C39 1.393(10) . ? C39 C40 1.373(12) . ? C40 C41 1.371(12) . ? C41 C42 1.362(11) . ? C42 C44 1.383(12) . ? C43 C44 1.495(10) . ? 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 N2 Pb1 N1 56.52(17) . . ? N2 Pb1 Cl1 106.49(12) . . ? N1 Pb1 Cl1 89.28(12) . . ? N2 Pb1 C1 28.44(16) . . ? N1 Pb1 C1 28.49(16) . . ? Cl1 Pb1 C1 102.24(12) . . ? N2 Pb1 Cl1 102.15(13) . 2_666 ? N1 Pb1 Cl1 151.23(12) . 2_666 ? Cl1 Pb1 Cl1 78.14(6) . 2_666 ? C1 Pb1 Cl1 129.60(13) . 2_666 ? Pb1 Cl1 Pb1 101.86(6) . 2_666 ? C1 N1 C2 124.9(6) . . ? C1 N1 Pb1 92.5(4) . . ? C2 N1 Pb1 138.0(4) . . ? C1 N2 C14 124.8(6) . . ? C1 N2 Pb1 95.1(4) . . ? C14 N2 Pb1 139.0(4) . . ? C1 N3 C26 126.8(5) . . ? N1 C1 N2 114.3(6) . . ? N1 C1 N3 120.9(6) . . ? N2 C1 N3 124.7(6) . . ? N1 C1 Pb1 59.0(4) . . ? N2 C1 Pb1 56.5(4) . . ? N3 C1 Pb1 170.7(4) . . ? C7 C2 C3 120.0(6) . . ? C7 C2 N1 119.5(6) . . ? C3 C2 N1 120.2(6) . . ? C4 C3 C2 118.4(6) . . ? C4 C3 C8 119.1(6) . . ? C2 C3 C8 122.4(6) . . ? C5 C4 C3 122.2(7) . . ? C6 C5 C4 118.4(7) . . ? C5 C6 C7 122.7(7) . . ? C6 C7 C2 118.3(7) . . ? C6 C7 C11 120.2(6) . . ? C2 C7 C11 121.4(6) . . ? C3 C8 C10 109.8(6) . . ? C3 C8 C9 115.1(6) . . ? C10 C8 C9 109.9(5) . . ? C12 C11 C7 114.4(6) . . ? C12 C11 C13 109.8(6) . . ? C7 C11 C13 109.2(5) . . ? C19 C14 C15 121.6(6) . . ? C19 C14 N2 118.9(6) . . ? C15 C14 N2 119.3(5) . . ? C16 C15 C14 117.8(6) . . ? C16 C15 C20 121.0(6) . . ? C14 C15 C20 121.1(6) . . ? C17 C16 C15 121.2(7) . . ? C18 C17 C16 119.3(7) . . ? C17 C18 C19 123.0(7) . . ? C18 C19 C14 116.9(6) . . ? C18 C19 C23 120.5(6) . . ? C14 C19 C23 122.2(6) . . ? C21 C20 C15 109.4(5) . . ? C21 C20 C22 110.1(6) . . ? C15 C20 C22 114.0(6) . . ? C19 C23 C24 109.4(6) . . ? C19 C23 C25 113.5(7) . . ? C24 C23 C25 109.6(6) . . ? C27 C26 C31 122.5(6) . . ? C27 C26 N3 118.7(6) . . ? C31 C26 N3 118.5(6) . . ? C28 C27 C26 117.8(6) . . ? C28 C27 C32 121.2(7) . . ? C26 C27 C32 120.9(6) . . ? C29 C28 C27 121.4(7) . . ? C28 C29 C30 119.3(6) . . ? C31 C30 C29 121.3(6) . . ? C30 C31 C26 117.5(6) . . ? C30 C31 C35 121.1(6) . . ? C26 C31 C35 121.1(6) . . ? C34 C32 C27 114.2(6) . . ? C34 C32 C33 109.7(6) . . ? C27 C32 C33 109.2(5) . . ? C31 C35 C37 108.8(6) . . ? C31 C35 C36 113.5(5) . . ? C37 C35 C36 110.0(5) . . ? C44 C38 C39 121.3(9) . . ? C40 C39 C38 120.2(8) . . ? C41 C40 C39 118.0(8) . . ? C42 C41 C40 121.9(10) . . ? C41 C42 C44 120.9(9) . . ? C38 C44 C42 117.6(8) . . ? C38 C44 C43 122.2(9) . . ? C42 C44 C43 120.1(8) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 2.152 _refine_diff_density_min -1.274 _refine_diff_density_rms 0.203 # Attachment 'pbcygclnew.CIF' data_pbcygcl _database_code_depnum_ccdc_archive 'CCDC 677777' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C74 H112 Cl2 N6 Pb2, 2(C7 H8), C7 H8' _chemical_formula_sum 'C95 H136 Cl2 N6 Pb2' _chemical_formula_weight 1847.38 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' Cl Cl 0.1484 0.1585 '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' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 13.2064(3) _cell_length_b 13.3847(3) _cell_length_c 13.9367(4) _cell_angle_alpha 63.026(1) _cell_angle_beta 80.217(1) _cell_angle_gamma 79.878(1) _cell_volume 2149.88(9) _cell_formula_units_Z 1 _cell_measurement_temperature 123(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.427 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 946 _exptl_absorpt_coefficient_mu 4.021 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.40 _exptl_absorpt_correction_T_max 0.45 _exptl_absorpt_process_details 'SORTAV (Blessing, 1997)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 123(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Enraf Nonius KAPPA CCD' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19429 _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_sigmaI/netI 0.0651 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 27.50 _reflns_number_total 9765 _reflns_number_gt 8359 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'Denzo SMN (Otwinoski and Minor, 1997)' _computing_data_reduction 'Denzo SMN (Otwinoski and Minor, 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 2001)' _computing_publication_material 'CIFTAB (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. The lattice toluene molecule C44 > C47 was modelled as disordered (occupancies fixed at 0.5:0.5 after trial refinement), the geometry of each component was restrained to resonable values and Uij parameters were restrained to be similar for neighbouring atoms within each toluene molecule. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0531P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 9765 _refine_ls_number_parameters 463 _refine_ls_number_restraints 24 _refine_ls_R_factor_all 0.0543 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.0988 _refine_ls_wR_factor_gt 0.0931 _refine_ls_goodness_of_fit_ref 1.059 _refine_ls_restrained_S_all 1.063 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 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_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.835396(12) 0.972816(12) 0.551770(13) 0.02030(6) Uani 1 1 d . . . Cl1 Cl 1.00607(9) 0.85471(9) 0.52341(11) 0.0349(3) Uani 1 1 d . . . N2 N 0.7071(3) 0.8133(3) 0.8715(3) 0.0181(7) Uani 1 1 d . . . C2 C 0.7804(4) 0.7084(3) 1.0553(4) 0.0257(10) Uani 1 1 d . . . H2A H 0.7213 0.6642 1.0941 0.031 Uiso 1 1 calc R . . H2B H 0.8310 0.6640 1.0244 0.031 Uiso 1 1 calc R . . N3 N 0.8298(3) 0.9330(3) 0.7321(3) 0.0173(7) Uani 1 1 d . . . C3 C 0.4173(3) 0.8403(4) 0.8409(5) 0.0330(12) Uani 1 1 d . . . H3A H 0.3626 0.9052 0.8217 0.040 Uiso 1 1 calc R . . H3B H 0.4274 0.8142 0.7835 0.040 Uiso 1 1 calc R . . N4 N 0.7564(3) 0.8201(3) 0.6941(3) 0.0164(7) Uani 1 1 d . . . C4 C 0.8305(4) 0.7283(4) 1.1341(4) 0.0340(12) Uani 1 1 d . . . H4A H 0.8936 0.7659 1.0967 0.041 Uiso 1 1 calc R . . H4B H 0.8515 0.6549 1.1941 0.041 Uiso 1 1 calc R . . C5 C 0.7632(3) 0.8527(3) 0.7702(3) 0.0168(8) Uani 1 1 d . . . C6 C 0.5189(3) 0.8786(4) 0.8461(4) 0.0288(11) Uani 1 1 d . . . H6A H 0.5408 0.9387 0.7746 0.035 Uiso 1 1 calc R . . H6B H 0.5078 0.9100 0.8997 0.035 Uiso 1 1 calc R . . C7 C 0.6558(3) 0.7242(3) 0.6377(4) 0.0193(9) Uani 1 1 d . . . C8 C 0.7278(3) 0.7173(3) 0.7062(3) 0.0161(8) Uani 1 1 d . . . C9 C 0.7422(3) 0.8214(3) 0.9630(3) 0.0207(9) Uani 1 1 d . . . H9 H 0.8044 0.8634 0.9312 0.025 Uiso 1 1 calc R . . C10 C 0.9425(3) 0.9967(3) 0.8084(4) 0.0215(9) Uani 1 1 d . . . C11 C 0.8444(3) 1.0080(3) 0.7741(3) 0.0184(9) Uani 1 1 d . . . C12 C 0.5694(4) 0.6823(4) 0.9863(4) 0.0326(12) Uani 1 1 d . . . H12A H 0.6233 0.6169 1.0037 0.039 Uiso 1 1 calc R . . H12B H 0.5611 0.7068 1.0447 0.039 Uiso 1 1 calc R . . C13 C 0.7727(3) 0.6101(3) 0.7784(3) 0.0198(9) Uani 1 1 d . . . C14 C 0.7688(3) 1.0964(3) 0.7753(3) 0.0208(9) Uani 1 1 d . . . C15 C 0.6115(3) 0.8367(3) 0.5537(4) 0.0239(10) Uani 1 1 d . . . H15 H 0.6175 0.8960 0.5766 0.029 Uiso 1 1 calc R . . C16 C 0.6036(3) 0.7788(3) 0.8784(4) 0.0238(10) Uani 1 1 d . . . H16 H 0.6097 0.7497 0.8228 0.029 Uiso 1 1 calc R . . C17 C 0.8585(3) 0.5956(4) 0.8442(4) 0.0245(10) Uani 1 1 d . . . H17 H 0.8528 0.6651 0.8555 0.029 Uiso 1 1 calc R . . C18 C 0.7415(3) 0.5142(3) 0.7819(4) 0.0252(10) Uani 1 1 d . . . H18 H 0.7699 0.4420 0.8311 0.030 Uiso 1 1 calc R . . C19 C 0.6293(4) 0.6247(4) 0.6446(4) 0.0257(10) Uani 1 1 d . . . H19 H 0.5816 0.6289 0.5987 0.031 Uiso 1 1 calc R . . C20 C 0.9577(4) 1.0652(4) 0.8549(4) 0.0274(10) Uani 1 1 d . . . H20 H 1.0224 1.0565 0.8806 0.033 Uiso 1 1 calc R . . C21 C 0.6747(3) 1.1299(3) 0.7125(4) 0.0259(10) Uani 1 1 d . . . H21 H 0.6615 1.0628 0.7046 0.031 Uiso 1 1 calc R . . C22 C 0.7171(4) 0.9119(4) 1.0899(4) 0.0326(12) Uani 1 1 d . . . H22A H 0.7751 0.9576 1.0508 0.039 Uiso 1 1 calc R . . H22B H 0.6659 0.9549 1.1218 0.039 Uiso 1 1 calc R . . C23 C 0.7017(4) 1.2227(4) 0.5991(4) 0.0334(11) Uani 1 1 d . . . H23A H 0.7127 1.2902 0.6048 0.050 Uiso 1 1 calc R . . H23B H 0.6448 1.2409 0.5549 0.050 Uiso 1 1 calc R . . H23C H 0.7650 1.1962 0.5652 0.050 Uiso 1 1 calc R . . C24 C 1.0294(3) 0.9138(4) 0.7908(4) 0.0251(10) Uani 1 1 d . . . H24 H 1.0162 0.9062 0.7259 0.030 Uiso 1 1 calc R . . C25 C 0.6706(4) 0.5205(4) 0.7164(4) 0.0310(11) Uani 1 1 d . . . H25 H 0.6505 0.4537 0.7208 0.037 Uiso 1 1 calc R . . C26 C 0.6664(4) 0.8924(4) 1.0096(4) 0.0259(10) Uani 1 1 d . . . H26A H 0.6042 0.8532 1.0467 0.031 Uiso 1 1 calc R . . H26B H 0.6446 0.9659 0.9501 0.031 Uiso 1 1 calc R . . C27 C 0.6757(4) 0.8646(4) 0.4443(4) 0.0367(12) Uani 1 1 d . . . H27A H 0.7485 0.8623 0.4523 0.055 Uiso 1 1 calc R . . H27B H 0.6508 0.9402 0.3918 0.055 Uiso 1 1 calc R . . H27C H 0.6690 0.8092 0.4186 0.055 Uiso 1 1 calc R . . C28 C 0.8813(4) 1.1445(4) 0.8640(4) 0.0332(12) Uani 1 1 d . . . H28 H 0.8916 1.1873 0.8997 0.040 Uiso 1 1 calc R . . C29 C 0.3828(4) 0.7464(4) 0.9474(5) 0.0386(13) Uani 1 1 d . . . H29A H 0.3193 0.7212 0.9406 0.046 Uiso 1 1 calc R . . H29B H 0.3664 0.7743 1.0036 0.046 Uiso 1 1 calc R . . C30 C 0.7884(4) 1.1627(4) 0.8213(4) 0.0289(11) Uani 1 1 d . . . H30 H 0.7376 1.2216 0.8237 0.035 Uiso 1 1 calc R . . C31 C 0.5745(4) 1.1714(4) 0.7647(5) 0.0404(14) Uani 1 1 d . . . H31A H 0.5572 1.1126 0.8375 0.061 Uiso 1 1 calc R . . H31B H 0.5180 1.1883 0.7204 0.061 Uiso 1 1 calc R . . H31C H 0.5845 1.2398 0.7696 0.061 Uiso 1 1 calc R . . C32 C 0.4980(4) 0.8414(4) 0.5416(5) 0.0392(13) Uani 1 1 d . . . H32A H 0.4902 0.7853 0.5172 0.059 Uiso 1 1 calc R . . H32B H 0.4738 0.9168 0.4883 0.059 Uiso 1 1 calc R . . H32C H 0.4569 0.8250 0.6116 0.059 Uiso 1 1 calc R . . C33 C 0.7574(5) 0.8014(4) 1.1802(4) 0.0390(13) Uani 1 1 d . . . H33A H 0.6984 0.7598 1.2255 0.047 Uiso 1 1 calc R . . H33B H 0.7944 0.8175 1.2269 0.047 Uiso 1 1 calc R . . C34 C 1.0320(4) 0.7963(4) 0.8851(4) 0.0367(12) Uani 1 1 d . . . H34A H 1.0373 0.8014 0.9520 0.055 Uiso 1 1 calc R . . H34B H 1.0918 0.7479 0.8715 0.055 Uiso 1 1 calc R . . H34C H 0.9684 0.7640 0.8924 0.055 Uiso 1 1 calc R . . C35 C 0.8527(4) 0.4947(4) 0.9556(4) 0.0377(12) Uani 1 1 d . . . H35A H 0.7836 0.4989 0.9935 0.057 Uiso 1 1 calc R . . H35B H 0.9045 0.4958 0.9977 0.057 Uiso 1 1 calc R . . H35C H 0.8663 0.4246 0.9471 0.057 Uiso 1 1 calc R . . C36 C 0.4675(4) 0.6473(4) 0.9810(5) 0.0400(14) Uani 1 1 d . . . H36A H 0.4451 0.5882 1.0529 0.048 Uiso 1 1 calc R . . H36B H 0.4783 0.6147 0.9285 0.048 Uiso 1 1 calc R . . C37 C 1.1353(4) 0.9565(5) 0.7656(5) 0.0427(14) Uani 1 1 d . . . H37A H 1.1309 1.0352 0.7108 0.064 Uiso 1 1 calc R . . H37B H 1.1860 0.9102 0.7381 0.064 Uiso 1 1 calc R . . H37C H 1.1569 0.9515 0.8317 0.064 Uiso 1 1 calc R . . C38 C 0.9631(4) 0.5861(5) 0.7816(5) 0.0445(14) Uani 1 1 d . . . H38A H 0.9704 0.5193 0.7682 0.067 Uiso 1 1 calc R . . H38B H 1.0182 0.5793 0.8240 0.067 Uiso 1 1 calc R . . H38C H 0.9681 0.6537 0.7124 0.067 Uiso 1 1 calc R . . C41 C 0.3107(8) 0.5136(8) 0.6394(9) 0.046(3) Uiso 0.539(9) 1 d PD A 1 C41' C 0.2760(11) 0.5893(12) 0.6825(12) 0.059(4) Uiso 0.461(9) 1 d PD A 2 C42 C 0.2218(6) 0.5857(7) 0.6464(7) 0.0211(19) Uiso 0.539(9) 1 d PD A 1 H42 H 0.1643 0.5907 0.6111 0.025 Uiso 0.539(9) 1 calc PR A 1 C42' C 0.2225(10) 0.5566(11) 0.6226(12) 0.053(4) Uiso 0.461(9) 1 d PD A 2 H42' H 0.1540 0.5901 0.6070 0.063 Uiso 0.461(9) 1 calc PR A 2 C43 C 0.2147(9) 0.6466(10) 0.6998(10) 0.056(3) Uiso 0.539(9) 1 d PD A 1 H43 H 0.1557 0.6995 0.6973 0.067 Uiso 0.539(9) 1 calc PR A 1 C43' C 0.2686(9) 0.4768(10) 0.5867(10) 0.042(3) Uiso 0.461(9) 1 d PD A 2 H43' H 0.2328 0.4504 0.5507 0.050 Uiso 0.461(9) 1 calc PR A 2 C44 C 0.2977(8) 0.6327(9) 0.7627(9) 0.044(3) Uiso 0.539(9) 1 d PD A 1 H44 H 0.2920 0.6732 0.8049 0.053 Uiso 0.539(9) 1 calc PR A 1 C44' C 0.3712(8) 0.4380(8) 0.6072(9) 0.029(3) Uiso 0.461(9) 1 d PD A 2 H44' H 0.4089 0.3867 0.5808 0.035 Uiso 0.461(9) 1 calc PR A 2 C45 C 0.3788(8) 0.5649(9) 0.7604(10) 0.050(3) Uiso 0.539(9) 1 d PD A 1 H45 H 0.4333 0.5556 0.8013 0.060 Uiso 0.539(9) 1 calc PR A 1 C45' C 0.4182(10) 0.4728(10) 0.6646(11) 0.047(3) Uiso 0.461(9) 1 d PD A 2 H45' H 0.4882 0.4436 0.6766 0.056 Uiso 0.461(9) 1 calc PR A 2 C46 C 0.3894(8) 0.5020(9) 0.6966(8) 0.032(2) Uiso 0.539(9) 1 d PD A 1 H46 H 0.4506 0.4533 0.6948 0.038 Uiso 0.539(9) 1 calc PR A 1 C46' C 0.3727(11) 0.5462(13) 0.7061(13) 0.065(5) Uiso 0.461(9) 1 d PD A 2 H46' H 0.4073 0.5655 0.7488 0.078 Uiso 0.461(9) 1 calc PR A 2 C47 C 0.3195(11) 0.4526(10) 0.5722(11) 0.053(3) Uiso 0.539(9) 1 d P A 1 H47A H 0.3837 0.4669 0.5235 0.080 Uiso 0.539(9) 1 calc PR A 1 H47B H 0.2603 0.4789 0.5295 0.080 Uiso 0.539(9) 1 calc PR A 1 H47C H 0.3203 0.3715 0.6191 0.080 Uiso 0.539(9) 1 calc PR A 1 C47' C 0.2389(17) 0.6860(17) 0.7180(18) 0.091(6) Uiso 0.461(9) 1 d P A 2 H47D H 0.2832 0.6799 0.7706 0.136 Uiso 0.461(9) 1 calc PR A 2 H47E H 0.1672 0.6798 0.7511 0.136 Uiso 0.461(9) 1 calc PR A 2 H47F H 0.2430 0.7592 0.6545 0.136 Uiso 0.461(9) 1 calc PR A 2 C48 C 0.9854(6) 0.5741(4) 0.4596(6) 0.031(2) Uiso 0.50 1 d PG B -1 C49 C 1.0603(5) 0.5047(6) 0.4281(5) 0.037(3) Uiso 0.50 1 d PG B -1 H49 H 1.1030 0.5363 0.3618 0.045 Uiso 0.50 1 calc PR B -1 C50 C 1.0725(6) 0.3892(5) 0.4935(7) 0.053(3) Uiso 0.50 1 d PG B -1 H50 H 1.1237 0.3418 0.4719 0.064 Uiso 0.50 1 calc PR B -1 C51 C 1.0100(7) 0.3430(4) 0.5904(6) 0.055(4) Uiso 0.50 1 d PG B -1 H51 H 1.0184 0.2641 0.6351 0.066 Uiso 0.50 1 calc PR B -1 C52 C 0.9352(6) 0.4124(6) 0.6220(5) 0.051(3) Uiso 0.50 1 d PG B -1 H52 H 0.8925 0.3809 0.6883 0.061 Uiso 0.50 1 calc PR B -1 C53 C 0.9229(5) 0.5280(6) 0.5566(6) 0.052(4) Uiso 0.50 1 d PG B -1 H53 H 0.8718 0.5754 0.5781 0.062 Uiso 0.50 1 calc PR B -1 C54 C 0.9631(10) 0.6986(10) 0.3900(11) 0.048(3) Uiso 0.50 1 d P B -1 H54A H 0.9091 0.7313 0.4284 0.072 Uiso 0.50 1 calc PR B -1 H54B H 0.9395 0.7106 0.3222 0.072 Uiso 0.50 1 calc PR B -1 H54C H 1.0261 0.7350 0.3740 0.072 Uiso 0.50 1 calc PR B -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 0.01831(9) 0.02391(9) 0.01960(10) -0.01010(7) 0.00093(6) -0.00576(6) Cl1 0.0264(6) 0.0313(6) 0.0546(8) -0.0283(6) 0.0101(5) -0.0087(5) N2 0.0155(17) 0.0198(16) 0.0186(18) -0.0092(15) 0.0038(14) -0.0044(13) C2 0.027(2) 0.021(2) 0.024(2) -0.0082(19) 0.0027(19) -0.0018(17) N3 0.0123(17) 0.0183(16) 0.0222(19) -0.0096(15) 0.0014(14) -0.0043(13) C3 0.013(2) 0.036(3) 0.059(4) -0.030(3) 0.001(2) -0.0027(18) N4 0.0136(17) 0.0183(16) 0.0175(18) -0.0084(14) -0.0001(13) -0.0022(12) C4 0.044(3) 0.034(3) 0.019(2) -0.008(2) -0.001(2) -0.005(2) C5 0.0117(19) 0.0151(18) 0.021(2) -0.0068(17) -0.0009(16) 0.0019(14) C6 0.016(2) 0.027(2) 0.043(3) -0.014(2) 0.000(2) -0.0040(17) C7 0.017(2) 0.0135(18) 0.024(2) -0.0055(17) -0.0028(17) -0.0004(15) C8 0.0117(19) 0.0179(18) 0.020(2) -0.0106(17) -0.0001(16) -0.0007(14) C9 0.021(2) 0.023(2) 0.019(2) -0.0115(18) 0.0051(17) -0.0064(16) C10 0.022(2) 0.022(2) 0.019(2) -0.0051(18) -0.0014(17) -0.0093(16) C11 0.021(2) 0.0199(19) 0.012(2) -0.0047(16) 0.0033(16) -0.0083(16) C12 0.023(2) 0.024(2) 0.045(3) -0.012(2) 0.008(2) -0.0067(18) C13 0.016(2) 0.022(2) 0.020(2) -0.0106(18) -0.0002(16) 0.0019(15) C14 0.021(2) 0.022(2) 0.019(2) -0.0087(18) 0.0051(17) -0.0066(16) C15 0.023(2) 0.0176(19) 0.029(2) -0.0067(18) -0.0104(19) 0.0006(16) C16 0.012(2) 0.024(2) 0.038(3) -0.019(2) 0.0063(18) -0.0049(16) C17 0.021(2) 0.024(2) 0.027(2) -0.0110(19) -0.0072(18) 0.0069(17) C18 0.024(2) 0.017(2) 0.031(3) -0.0087(19) -0.0022(19) 0.0018(17) C19 0.025(2) 0.026(2) 0.033(3) -0.016(2) -0.007(2) -0.0067(18) C20 0.032(3) 0.030(2) 0.025(2) -0.012(2) -0.006(2) -0.0117(19) C21 0.022(2) 0.020(2) 0.036(3) -0.014(2) 0.0015(19) -0.0021(17) C22 0.043(3) 0.029(2) 0.027(3) -0.016(2) 0.007(2) -0.004(2) C23 0.031(3) 0.030(2) 0.035(3) -0.010(2) -0.010(2) 0.000(2) C24 0.015(2) 0.032(2) 0.029(3) -0.014(2) -0.0037(18) -0.0019(17) C25 0.037(3) 0.017(2) 0.042(3) -0.015(2) -0.007(2) -0.0035(18) C26 0.029(3) 0.026(2) 0.023(2) -0.0131(19) 0.0045(19) -0.0045(18) C27 0.044(3) 0.034(3) 0.026(3) -0.007(2) -0.005(2) -0.006(2) C28 0.047(3) 0.030(2) 0.031(3) -0.018(2) 0.001(2) -0.014(2) C29 0.016(2) 0.046(3) 0.058(4) -0.028(3) 0.011(2) -0.012(2) C30 0.037(3) 0.023(2) 0.027(3) -0.013(2) 0.004(2) -0.0048(19) C31 0.026(3) 0.030(3) 0.059(4) -0.019(3) 0.003(2) 0.005(2) C32 0.029(3) 0.037(3) 0.049(3) -0.014(3) -0.020(2) 0.002(2) C33 0.058(4) 0.039(3) 0.021(3) -0.015(2) 0.002(2) -0.007(2) C34 0.026(3) 0.038(3) 0.032(3) -0.006(2) -0.001(2) -0.001(2) C35 0.045(3) 0.033(3) 0.031(3) -0.010(2) -0.011(2) 0.003(2) C36 0.028(3) 0.034(3) 0.059(4) -0.021(3) 0.010(2) -0.015(2) C37 0.026(3) 0.050(3) 0.052(4) -0.023(3) 0.006(2) -0.013(2) C38 0.022(3) 0.068(4) 0.035(3) -0.018(3) -0.004(2) 0.005(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; 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 N3 2.311(4) . ? Pb1 N4 2.360(3) . ? Pb1 Cl1 2.5976(11) . ? Pb1 C5 2.806(4) . ? Pb1 Cl1 3.0934(11) 2_776 ? N2 C5 1.387(5) . ? N2 C9 1.482(6) . ? N2 C16 1.493(5) . ? C2 C4 1.514(7) . ? C2 C9 1.544(6) . ? N3 C5 1.365(5) . ? N3 C11 1.424(5) . ? C3 C29 1.507(7) . ? C3 C6 1.543(6) . ? N4 C5 1.339(5) . ? N4 C8 1.418(5) . ? C4 C33 1.526(7) . ? C6 C16 1.529(6) . ? C7 C19 1.393(6) . ? C7 C8 1.422(6) . ? C7 C15 1.518(5) . ? C8 C13 1.420(5) . ? C9 C26 1.526(6) . ? C10 C20 1.396(6) . ? C10 C11 1.417(6) . ? C10 C24 1.520(6) . ? C11 C14 1.411(6) . ? C12 C36 1.524(7) . ? C12 C16 1.532(6) . ? C13 C18 1.393(6) . ? C13 C17 1.509(6) . ? C14 C30 1.386(6) . ? C14 C21 1.528(6) . ? C15 C32 1.524(6) . ? C15 C27 1.530(7) . ? C17 C38 1.521(7) . ? C17 C35 1.529(6) . ? C18 C25 1.382(7) . ? C19 C25 1.376(6) . ? C20 C28 1.366(7) . ? C21 C23 1.533(6) . ? C21 C31 1.540(6) . ? C22 C33 1.522(7) . ? C22 C26 1.533(7) . ? C24 C34 1.524(6) . ? C24 C37 1.529(6) . ? C28 C30 1.389(7) . ? C29 C36 1.524(7) . ? C41 C46 1.360(12) . ? C41 C42 1.403(11) . ? C41 C47 1.477(15) . ? C41' C46' 1.336(15) . ? C41' C42' 1.424(14) . ? C41' C47' 1.56(2) . ? C42 C43 1.314(12) . ? C42' C43' 1.383(14) . ? C43 C44 1.453(13) . ? C43' C44' 1.391(13) . ? C44 C45 1.283(12) . ? C44' C45' 1.359(13) . ? C45 C46 1.455(13) . ? C45' C46' 1.361(14) . ? C48 C49 1.3900 . ? C48 C53 1.3900 . ? C48 C54 1.504(13) . ? C49 C50 1.3900 . ? C50 C51 1.3900 . ? C51 C52 1.3900 . ? C52 C53 1.3900 . ? 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 N3 Pb1 N4 56.69(12) . . ? N3 Pb1 Cl1 101.99(9) . . ? N4 Pb1 Cl1 96.10(8) . . ? N3 Pb1 C5 28.94(12) . . ? N4 Pb1 C5 28.39(12) . . ? Cl1 Pb1 C5 104.68(8) . . ? N3 Pb1 Cl1 93.64(8) . 2_776 ? N4 Pb1 Cl1 148.40(9) . 2_776 ? Cl1 Pb1 Cl1 78.43(3) . 2_776 ? C5 Pb1 Cl1 122.54(9) . 2_776 ? C5 N2 C9 121.0(3) . . ? C5 N2 C16 116.4(4) . . ? C9 N2 C16 122.1(3) . . ? C4 C2 C9 110.8(4) . . ? C5 N3 C11 129.7(3) . . ? C5 N3 Pb1 96.1(3) . . ? C11 N3 Pb1 126.7(2) . . ? C29 C3 C6 111.4(5) . . ? C5 N4 C8 129.2(3) . . ? C5 N4 Pb1 94.6(2) . . ? C8 N4 Pb1 135.2(3) . . ? C2 C4 C33 111.7(4) . . ? N4 C5 N3 110.2(4) . . ? N4 C5 N2 124.4(4) . . ? N3 C5 N2 125.4(4) . . ? N4 C5 Pb1 57.0(2) . . ? N3 C5 Pb1 55.0(2) . . ? N2 C5 Pb1 166.1(3) . . ? C16 C6 C3 110.1(4) . . ? C19 C7 C8 118.9(4) . . ? C19 C7 C15 119.3(4) . . ? C8 C7 C15 121.7(4) . . ? N4 C8 C13 122.7(4) . . ? N4 C8 C7 117.5(3) . . ? C13 C8 C7 119.7(4) . . ? N2 C9 C26 114.6(4) . . ? N2 C9 C2 115.8(3) . . ? C26 C9 C2 110.1(4) . . ? C20 C10 C11 118.6(4) . . ? C20 C10 C24 121.5(4) . . ? C11 C10 C24 119.8(4) . . ? C14 C11 C10 119.7(4) . . ? C14 C11 N3 122.9(4) . . ? C10 C11 N3 117.2(4) . . ? C36 C12 C16 110.8(5) . . ? C18 C13 C8 118.2(4) . . ? C18 C13 C17 118.7(4) . . ? C8 C13 C17 122.9(4) . . ? C30 C14 C11 118.9(4) . . ? C30 C14 C21 119.9(4) . . ? C11 C14 C21 120.6(4) . . ? C7 C15 C32 113.8(4) . . ? C7 C15 C27 109.6(4) . . ? C32 C15 C27 109.8(4) . . ? N2 C16 C6 112.6(3) . . ? N2 C16 C12 115.3(4) . . ? C6 C16 C12 110.7(4) . . ? C13 C17 C38 110.1(4) . . ? C13 C17 C35 113.5(4) . . ? C38 C17 C35 110.0(4) . . ? C25 C18 C13 122.3(4) . . ? C25 C19 C7 121.6(4) . . ? C28 C20 C10 121.1(5) . . ? C14 C21 C23 107.9(4) . . ? C14 C21 C31 115.2(4) . . ? C23 C21 C31 109.2(4) . . ? C33 C22 C26 112.0(4) . . ? C10 C24 C34 113.0(4) . . ? C10 C24 C37 112.4(4) . . ? C34 C24 C37 110.0(4) . . ? C19 C25 C18 119.3(4) . . ? C9 C26 C22 110.4(4) . . ? C20 C28 C30 120.1(5) . . ? C3 C29 C36 110.3(4) . . ? C14 C30 C28 121.0(4) . . ? C22 C33 C4 110.9(4) . . ? C12 C36 C29 112.1(4) . . ? C46 C41 C42 117.6(10) . . ? C46 C41 C47 120.8(10) . . ? C42 C41 C47 121.6(10) . . ? C46' C41' C42' 122.4(13) . . ? C46' C41' C47' 110.4(14) . . ? C42' C41' C47' 126.9(14) . . ? C43 C42 C41 122.7(9) . . ? C43' C42' C41' 121.1(12) . . ? C42 C43 C44 119.7(10) . . ? C42' C43' C44' 115.2(11) . . ? C45 C44 C43 118.8(11) . . ? C45' C44' C43' 120.8(10) . . ? C44 C45 C46 121.6(11) . . ? C44' C45' C46' 125.1(12) . . ? C41 C46 C45 119.4(10) . . ? C41' C46' C45' 115.2(14) . . ? C49 C48 C53 120.0 . . ? C49 C48 C54 123.0(7) . . ? C53 C48 C54 116.9(7) . . ? C48 C49 C50 120.0 . . ? C51 C50 C49 120.0 . . ? C52 C51 C50 120.0 . . ? C53 C52 C51 120.0 . . ? C52 C53 C48 120.0 . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 2.211 _refine_diff_density_min -1.877 _refine_diff_density_rms 0.151