Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'J. Fulton' _publ_contact_author_address ; Department of Chemistry University of Sussex Falmer Brighton BN1 9QJ UNITED KINGDOM ; _publ_contact_author_email J.R.FULTON@SUSSEX.AC.UK _publ_section_title ; The synthesis of monomeric terminal lead arylxodies: dependence on reagents and conditions ; _publ_requested_category FM loop_ _publ_author_name 'J. Fulton' 'P. B. Hitchcock' 'Nick C. Johnstone' 'Eric C. Y. Tam' data_(2)-jul1006 _database_code_depnum_ccdc_archive 'CCDC 641614' _audit_creation_date 2006-07-26T09:52:11-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C88 H128 Cl2 Li2 N4 O2 Pb2, 6(C6 D6)' _chemical_formula_sum 'C124 H128 Cl2 D36 Li2 N4 O2 Pb2' _chemical_formula_weight 2277.8 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.2848(2) _cell_length_b 14.8940(4) _cell_length_c 17.3448(4) _cell_angle_alpha 99.340(1) _cell_angle_beta 102.769(1) _cell_angle_gamma 105.893(1) _cell_volume 2891.57(11) _cell_formula_units_Z 1 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 47522 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.15 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.308 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1156 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.00 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.572 _exptl_absorpt_correction_T_max 0.7711 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.383046E-1 _diffrn_orient_matrix_ub_12 0.638724E-1 _diffrn_orient_matrix_ub_13 0.397306E-1 _diffrn_orient_matrix_ub_21 0.789552E-1 _diffrn_orient_matrix_ub_22 -0.85409E-2 _diffrn_orient_matrix_ub_23 0.46033E-2 _diffrn_orient_matrix_ub_31 0.83847E-2 _diffrn_orient_matrix_ub_32 0.318157E-1 _diffrn_orient_matrix_ub_33 -0.458695E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0502 _diffrn_reflns_av_unetI/netI 0.0395 _diffrn_reflns_number 40829 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 3.59 _diffrn_reflns_theta_max 26.34 _diffrn_reflns_theta_full 26.34 _diffrn_measured_fraction_theta_full 0.965 _diffrn_measured_fraction_theta_max 0.965 _reflns_number_total 11385 _reflns_number_gt 10266 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; There are three independent deutero-benzene solvate molecules , two of which are disordered, and all three were included as rigid bodies with isotropic C atoms. 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. ; _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^)+(0.0290P)^2^+5.4675P] 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_number_reflns 11385 _refine_ls_number_parameters 515 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.042 _refine_ls_R_factor_gt 0.0348 _refine_ls_wR_factor_ref 0.0845 _refine_ls_wR_factor_gt 0.0813 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.097 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.223 _refine_diff_density_min -0.905 _refine_diff_density_rms 0.088 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 '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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 Pb Pb 0.283093(13) 0.267014(10) 0.203905(8) 0.03041(6) Uani 1 1 d . . . Li Li 0.0134(6) 0.0508(5) 0.0677(4) 0.0379(16) Uani 1 1 d . . . Cl Cl 0.06572(9) 0.16387(7) 0.19286(6) 0.0377(2) Uani 1 1 d . . . O O 0.1096(2) 0.05593(18) -0.00343(15) 0.0297(6) Uani 1 1 d . . . N1 N 0.2608(3) 0.4111(2) 0.25876(19) 0.0298(7) Uani 1 1 d . . . N2 N 0.3555(3) 0.2689(2) 0.33947(18) 0.0297(7) Uani 1 1 d . . . C1 C 0.2761(3) 0.4489(3) 0.3373(2) 0.0322(9) Uani 1 1 d . . . C2 C 0.3137(4) 0.4090(3) 0.4012(2) 0.0372(9) Uani 1 1 d . . . H2 H 0.3112 0.4412 0.4525 0.045 Uiso 1 1 calc R . . C3 C 0.3547(4) 0.3299(3) 0.4040(2) 0.0332(9) Uani 1 1 d . . . C4 C 0.2559(4) 0.5439(3) 0.3615(3) 0.0416(10) Uani 1 1 d . . . H4A H 0.2636 0.5792 0.319 0.062 Uiso 1 1 calc R . . H4B H 0.3144 0.5818 0.4129 0.062 Uiso 1 1 calc R . . H4C H 0.1765 0.5322 0.3685 0.062 Uiso 1 1 calc R . . C5 C 0.4042(5) 0.3197(3) 0.4894(2) 0.0464(11) Uani 1 1 d . . . H5A H 0.3391 0.2907 0.511 0.07 Uiso 1 1 calc R . . H5B H 0.4512 0.3832 0.5247 0.07 Uiso 1 1 calc R . . H5C H 0.454 0.2785 0.4876 0.07 Uiso 1 1 calc R . . C6 C 0.2339(4) 0.4636(3) 0.1989(2) 0.0318(8) Uani 1 1 d . . . C7 C 0.3261(4) 0.5105(3) 0.1684(3) 0.0399(10) Uani 1 1 d . . . C8 C 0.2994(5) 0.5576(4) 0.1080(3) 0.0545(13) Uani 1 1 d . . . H8 H 0.3599 0.5881 0.086 0.065 Uiso 1 1 calc R . . C9 C 0.1876(5) 0.5614(4) 0.0789(3) 0.0602(15) Uani 1 1 d . . . H9 H 0.1723 0.5957 0.0383 0.072 Uiso 1 1 calc R . . C10 C 0.0976(5) 0.5154(3) 0.1084(3) 0.0496(12) Uani 1 1 d . . . H10 H 0.0205 0.518 0.0875 0.059 Uiso 1 1 calc R . . C11 C 0.1182(4) 0.4652(3) 0.1687(2) 0.0345(9) Uani 1 1 d . . . C12 C 0.4516(4) 0.5122(4) 0.2025(3) 0.0514(12) Uani 1 1 d . . . H12 H 0.4475 0.4515 0.2212 0.062 Uiso 1 1 calc R . . C13 C 0.5216(6) 0.5153(6) 0.1406(5) 0.111(3) Uani 1 1 d . . . H13A H 0.4793 0.4613 0.0932 0.166 Uiso 1 1 calc R . . H13B H 0.5991 0.5105 0.1651 0.166 Uiso 1 1 calc R . . H13C H 0.5316 0.5759 0.1236 0.166 Uiso 1 1 calc R . . C14 C 0.5175(5) 0.5941(6) 0.2747(4) 0.092(2) Uani 1 1 d . . . H14A H 0.5977 0.5924 0.2953 0.138 Uiso 1 1 calc R . . H14B H 0.4771 0.5888 0.3174 0.138 Uiso 1 1 calc R . . H14C H 0.5209 0.6548 0.2589 0.138 Uiso 1 1 calc R . . C15 C 0.0167(4) 0.4169(3) 0.1999(3) 0.0406(10) Uani 1 1 d . . . H15 H 0.0489 0.3901 0.2458 0.049 Uiso 1 1 calc R . . C16 C -0.0404(5) 0.4893(4) 0.2329(4) 0.0688(17) Uani 1 1 d . . . H16A H -0.1051 0.4562 0.253 0.103 Uiso 1 1 calc R . . H16B H -0.0712 0.5177 0.1892 0.103 Uiso 1 1 calc R . . H16C H 0.0188 0.5402 0.2775 0.103 Uiso 1 1 calc R . . C17 C -0.0780(4) 0.3340(3) 0.1348(3) 0.0465(11) Uani 1 1 d . . . H17A H -0.1411 0.3046 0.1579 0.07 Uiso 1 1 calc R . . H17B H -0.0431 0.2858 0.116 0.07 Uiso 1 1 calc R . . H17C H -0.1105 0.3584 0.0888 0.07 Uiso 1 1 calc R . . C18 C 0.4098(3) 0.1956(3) 0.3475(2) 0.0312(8) Uani 1 1 d . . . C19 C 0.3505(4) 0.1093(3) 0.3640(2) 0.0327(9) Uani 1 1 d . . . C20 C 0.4042(4) 0.0375(3) 0.3643(3) 0.0419(10) Uani 1 1 d . . . H20 H 0.3653 -0.0217 0.375 0.05 Uiso 1 1 calc R . . C21 C 0.5123(4) 0.0513(3) 0.3492(3) 0.0496(12) Uani 1 1 d . . . H21 H 0.5468 0.0014 0.3493 0.06 Uiso 1 1 calc R . . C22 C 0.5704(4) 0.1363(3) 0.3342(3) 0.0456(11) Uani 1 1 d . . . H22 H 0.645 0.1448 0.3241 0.055 Uiso 1 1 calc R . . C23 C 0.5215(4) 0.2109(3) 0.3336(2) 0.0377(9) Uani 1 1 d . . . C24 C 0.2323(4) 0.0899(3) 0.3823(3) 0.0372(9) Uani 1 1 d . . . H24 H 0.2077 0.1485 0.3813 0.045 Uiso 1 1 calc R . . C25 C 0.2396(5) 0.0688(4) 0.4668(3) 0.0555(13) Uani 1 1 d . . . H25A H 0.162 0.0567 0.4767 0.083 Uiso 1 1 calc R . . H25B H 0.2967 0.1242 0.5085 0.083 Uiso 1 1 calc R . . H25C H 0.2649 0.0121 0.4691 0.083 Uiso 1 1 calc R . . C26 C 0.1365(4) 0.0043(3) 0.3175(3) 0.0436(10) Uani 1 1 d . . . H26A H 0.0612 -0.0064 0.3308 0.065 Uiso 1 1 calc R . . H26B H 0.1598 -0.0536 0.3169 0.065 Uiso 1 1 calc R . . H26C H 0.128 0.0188 0.2638 0.065 Uiso 1 1 calc R . . C27 C 0.5900(4) 0.3067(4) 0.3204(3) 0.0495(11) Uani 1 1 d . . . H27 H 0.5303 0.3344 0.2936 0.059 Uiso 1 1 calc R . . C28 C 0.6667(7) 0.2977(5) 0.2643(4) 0.097(2) Uani 1 1 d . . . H28A H 0.6187 0.2524 0.2126 0.146 Uiso 1 1 calc R . . H28B H 0.7295 0.2741 0.2897 0.146 Uiso 1 1 calc R . . H28C H 0.7017 0.3607 0.2543 0.146 Uiso 1 1 calc R . . C29 C 0.6602(7) 0.3766(5) 0.3998(4) 0.106(3) Uani 1 1 d . . . H29A H 0.6083 0.3821 0.4346 0.158 Uiso 1 1 calc R . . H29B H 0.6954 0.4397 0.3899 0.158 Uiso 1 1 calc R . . H29C H 0.7228 0.3539 0.4268 0.158 Uiso 1 1 calc R . . C30 C 0.2197(3) 0.1116(3) 0.0060(2) 0.0285(8) Uani 1 1 d . . . C31 C 0.2418(3) 0.1994(3) -0.0207(2) 0.0316(8) Uani 1 1 d . . . C32 C 0.3591(4) 0.2567(3) -0.0065(3) 0.0406(10) Uani 1 1 d . . . H32 H 0.3738 0.3159 -0.0227 0.049 Uiso 1 1 calc R . . C33 C 0.4547(4) 0.2307(3) 0.0300(3) 0.0407(10) Uani 1 1 d . . . C34 C 0.4317(3) 0.1460(3) 0.0544(2) 0.0369(9) Uani 1 1 d . . . H34 H 0.4966 0.1281 0.08 0.044 Uiso 1 1 calc R . . C35 C 0.3182(3) 0.0845(3) 0.0439(2) 0.0296(8) Uani 1 1 d . . . C36 C 0.1419(3) 0.2299(3) -0.0673(2) 0.0338(9) Uani 1 1 d . . . C37 C 0.1869(4) 0.3239(3) -0.0936(3) 0.0493(12) Uani 1 1 d . . . H37A H 0.1196 0.34 -0.1229 0.074 Uiso 1 1 calc R . . H37B H 0.2368 0.3156 -0.1293 0.074 Uiso 1 1 calc R . . H37C H 0.2329 0.3759 -0.0453 0.074 Uiso 1 1 calc R . . C38 C 0.0612(4) 0.2468(3) -0.0141(3) 0.0440(10) Uani 1 1 d . . . H38A H -0.0019 0.2664 -0.0448 0.066 Uiso 1 1 calc R . . H38B H 0.1074 0.2976 0.035 0.066 Uiso 1 1 calc R . . H38C H 0.0266 0.1873 0.0015 0.066 Uiso 1 1 calc R . . C39 C 0.0701(4) 0.1525(3) -0.1465(3) 0.0398(10) Uani 1 1 d . . . H39A H 0.0065 0.1725 -0.1759 0.06 Uiso 1 1 calc R . . H39B H 0.0363 0.0913 -0.133 0.06 Uiso 1 1 calc R . . H39C H 0.122 0.1444 -0.1807 0.06 Uiso 1 1 calc R . . C40 C 0.5800(4) 0.2915(4) 0.0381(4) 0.0602(14) Uani 1 1 d . . . H40A H 0.5786 0.3489 0.0176 0.09 Uiso 0.5 1 calc PR . . H40B H 0.6164 0.254 0.0063 0.09 Uiso 0.5 1 calc PR . . H40C H 0.6258 0.3109 0.0954 0.09 Uiso 0.5 1 calc PR . . H40D H 0.6353 0.2603 0.062 0.09 Uiso 0.5 1 calc PR . . H40E H 0.5975 0.3552 0.0733 0.09 Uiso 0.5 1 calc PR . . H40F H 0.5881 0.2983 -0.0158 0.09 Uiso 0.5 1 calc PR . . C41 C 0.3029(3) -0.0117(3) 0.0686(2) 0.0334(9) Uani 1 1 d . . . C42 C 0.2415(4) -0.0956(3) -0.0068(3) 0.0442(10) Uani 1 1 d . . . H42A H 0.2322 -0.1566 0.0097 0.066 Uiso 1 1 calc R . . H42B H 0.2894 -0.0915 -0.0452 0.066 Uiso 1 1 calc R . . H42C H 0.1638 -0.0924 -0.0329 0.066 Uiso 1 1 calc R . . C43 C 0.2335(4) -0.0201(3) 0.1323(3) 0.0422(10) Uani 1 1 d . . . H43A H 0.2251 -0.0821 0.1467 0.063 Uiso 1 1 calc R . . H43B H 0.1552 -0.0156 0.1097 0.063 Uiso 1 1 calc R . . H43C H 0.2758 0.0321 0.1811 0.063 Uiso 1 1 calc R . . C44 C 0.4212(4) -0.0250(3) 0.1076(3) 0.0421(10) Uani 1 1 d . . . H44A H 0.4063 -0.0873 0.1221 0.063 Uiso 1 1 calc R . . H44B H 0.4641 0.0265 0.1567 0.063 Uiso 1 1 calc R . . H44C H 0.4685 -0.0227 0.0688 0.063 Uiso 1 1 calc R . . C1S C 0.6832(3) 0.9359(3) 0.17455(18) 0.0643(14) Uiso 1 1 d G A 1 H1S H 0.6442 0.9217 0.1181 0.077 Uiso 1 1 calc R A 1 C2S C 0.7675(4) 1.0251(3) 0.2125(2) 0.0714(16) Uiso 1 1 d G A 1 H2S H 0.7862 1.0718 0.1819 0.086 Uiso 1 1 calc R A 1 C3S C 0.8246(3) 1.0459(2) 0.2950(2) 0.0830(19) Uiso 1 1 d G A 1 H3S H 0.8823 1.1069 0.321 0.1 Uiso 1 1 calc R A 1 C4S C 0.7973(4) 0.9776(3) 0.33970(18) 0.0828(19) Uiso 1 1 d G A 1 H4S H 0.8364 0.9918 0.3961 0.099 Uiso 1 1 calc R A 1 C5S C 0.7130(4) 0.8884(3) 0.3018(2) 0.0816(18) Uiso 1 1 d G A 1 H5S H 0.6943 0.8417 0.3323 0.098 Uiso 1 1 calc R A 1 C6S C 0.6559(3) 0.8676(2) 0.2192(2) 0.0781(17) Uiso 1 1 d G A 1 H6S H 0.5982 0.8066 0.1933 0.094 Uiso 1 1 calc R A 1 C7S C 0.4149(4) 0.8033(6) 0.3770(8) 0.048(3) Uiso 0.54(3) 1 d PG B 1 H7S H 0.4979 0.8198 0.3974 0.058 Uiso 0.54(3) 1 calc PR B 1 C8S C 0.3454(13) 0.8003(6) 0.4304(3) 0.049(3) Uiso 0.54(3) 1 d PG B 1 H8S H 0.381 0.8146 0.4874 0.059 Uiso 0.54(3) 1 calc PR B 1 C9S C 0.2238(12) 0.7762(7) 0.4005(9) 0.054(3) Uiso 0.54(3) 1 d PG B 1 H9S H 0.1763 0.7741 0.4371 0.065 Uiso 0.54(3) 1 calc PR B 1 C10S C 0.1717(4) 0.7553(6) 0.3172(10) 0.046(3) Uiso 0.54(3) 1 d PG B 1 H10S H 0.0886 0.7389 0.2967 0.055 Uiso 0.54(3) 1 calc PR B 1 C11S C 0.2412(13) 0.7584(6) 0.2637(4) 0.050(3) Uiso 0.54(3) 1 d PG B 1 H11S H 0.2056 0.7441 0.2068 0.06 Uiso 0.54(3) 1 calc PR B 1 C12S C 0.3628(12) 0.7824(7) 0.2936(7) 0.055(3) Uiso 0.54(3) 1 d PG B 1 H12S H 0.4102 0.7845 0.2571 0.066 Uiso 0.54(3) 1 calc PR B 1 C13S C 0.9682(10) 0.8027(7) 0.5006(6) 0.106(5) Uiso 0.509(9) 1 d PG C 1 H13S H 1.0035 0.8617 0.5407 0.127 Uiso 0.509(9) 1 calc PR C 1 C14S C 0.9321(10) 0.8033(7) 0.4189(7) 0.102(5) Uiso 0.509(9) 1 d PG C 1 H14S H 0.9426 0.8626 0.4032 0.122 Uiso 0.509(9) 1 calc PR C 1 C15S C 0.8805(10) 0.7170(8) 0.3602(5) 0.108(5) Uiso 0.509(9) 1 d PG C 1 H15S H 0.8558 0.7174 0.3044 0.13 Uiso 0.509(9) 1 calc PR C 1 C16S C 0.8650(10) 0.6303(7) 0.3833(7) 0.109(6) Uiso 0.509(9) 1 d PG C 1 H16S H 0.8297 0.5713 0.3431 0.131 Uiso 0.509(9) 1 calc PR C 1 C17S C 0.9011(11) 0.6297(7) 0.4649(8) 0.113(6) Uiso 0.509(9) 1 d PG C 1 H17S H 0.8905 0.5704 0.4807 0.135 Uiso 0.509(9) 1 calc PR C 1 C18S C 0.9527(11) 0.7160(9) 0.5236(5) 0.133(7) Uiso 0.509(9) 1 d PG C 1 H18S H 0.9774 0.7156 0.5794 0.16 Uiso 0.509(9) 1 calc PR C 1 C7T C 0.3807(13) 0.8090(7) 0.4265(5) 0.048(3) Uiso 0.46(3) 1 d PG B 2 H7T H 0.4392 0.8286 0.4774 0.058 Uiso 0.46(3) 1 calc PR B 2 C8T C 0.2625(17) 0.7900(8) 0.4240(8) 0.055(3) Uiso 0.46(3) 1 d PG B 2 H8T H 0.2403 0.7967 0.4732 0.066 Uiso 0.46(3) 1 calc PR B 2 C9T C 0.1768(6) 0.7613(7) 0.3496(13) 0.056(3) Uiso 0.46(3) 1 d PG B 2 H9T H 0.0961 0.7484 0.3479 0.067 Uiso 0.46(3) 1 calc PR B 2 C10T C 0.2093(12) 0.7515(6) 0.2776(8) 0.045(3) Uiso 0.46(3) 1 d PG B 2 H10T H 0.1507 0.7319 0.2267 0.054 Uiso 0.46(3) 1 calc PR B 2 C11T C 0.3274(16) 0.7705(8) 0.2801(5) 0.052(3) Uiso 0.46(3) 1 d PG B 2 H11T H 0.3496 0.7638 0.2309 0.062 Uiso 0.46(3) 1 calc PR B 2 C12T C 0.4131(6) 0.7992(7) 0.3545(10) 0.053(4) Uiso 0.46(3) 1 d PG B 2 H12T H 0.4939 0.8121 0.3562 0.063 Uiso 0.46(3) 1 calc PR B 2 C13T C 0.9061(10) 0.7229(7) 0.4556(7) 0.109(6) Uiso 0.491(9) 1 d PG C 2 H13T H 0.8796 0.764 0.4249 0.13 Uiso 0.491(9) 1 calc PR C 2 C14T C 0.9094(10) 0.6352(8) 0.4160(5) 0.086(4) Uiso 0.491(9) 1 d PG C 2 H14T H 0.8852 0.6163 0.3582 0.104 Uiso 0.491(9) 1 calc PR C 2 C15T C 0.9482(10) 0.5750(7) 0.4609(7) 0.115(6) Uiso 0.491(9) 1 d PG C 2 H15T H 0.9504 0.5151 0.4338 0.138 Uiso 0.491(9) 1 calc PR C 2 C16T C 0.9836(10) 0.6026(8) 0.5454(7) 0.112(6) Uiso 0.491(9) 1 d PG C 2 H16T H 1.0101 0.5615 0.5761 0.134 Uiso 0.491(9) 1 calc PR C 2 C17T C 0.9803(10) 0.6904(9) 0.5851(5) 0.113(6) Uiso 0.491(9) 1 d PG C 2 H17T H 1.0045 0.7092 0.6428 0.136 Uiso 0.491(9) 1 calc PR C 2 C18T C 0.9415(10) 0.7505(7) 0.5402(7) 0.097(5) Uiso 0.491(9) 1 d PG C 2 H18T H 0.9392 0.8105 0.5672 0.116 Uiso 0.491(9) 1 calc PR C 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 Pb 0.03608(9) 0.02668(8) 0.02582(8) 0.00389(6) 0.00530(6) 0.00992(6) Li 0.034(4) 0.038(4) 0.036(4) 0.001(3) 0.011(3) 0.005(3) Cl 0.0394(5) 0.0332(5) 0.0342(5) 0.0028(4) 0.0065(4) 0.0080(4) O 0.0238(13) 0.0286(14) 0.0336(14) 0.0049(11) 0.0069(11) 0.0057(11) N1 0.0350(17) 0.0232(16) 0.0294(17) 0.0055(13) 0.0051(14) 0.0104(14) N2 0.0358(18) 0.0239(16) 0.0262(16) 0.0048(13) 0.0018(13) 0.0111(14) C1 0.036(2) 0.0232(19) 0.033(2) 0.0052(16) 0.0042(17) 0.0090(17) C2 0.052(3) 0.031(2) 0.028(2) 0.0054(17) 0.0083(18) 0.0155(19) C3 0.040(2) 0.027(2) 0.028(2) 0.0053(16) 0.0043(17) 0.0096(17) C4 0.058(3) 0.031(2) 0.034(2) 0.0030(18) 0.005(2) 0.019(2) C5 0.074(3) 0.037(2) 0.028(2) 0.0047(18) 0.004(2) 0.026(2) C6 0.041(2) 0.0219(19) 0.0252(19) 0.0034(15) 0.0019(16) 0.0060(17) C7 0.046(2) 0.029(2) 0.039(2) 0.0059(18) 0.0118(19) 0.0040(19) C8 0.067(3) 0.045(3) 0.047(3) 0.020(2) 0.019(3) 0.004(2) C9 0.088(4) 0.043(3) 0.039(3) 0.022(2) 0.000(3) 0.009(3) C10 0.059(3) 0.041(3) 0.038(2) 0.007(2) -0.007(2) 0.017(2) C11 0.039(2) 0.025(2) 0.032(2) 0.0022(16) 0.0000(17) 0.0089(17) C12 0.042(3) 0.041(3) 0.074(3) 0.020(2) 0.025(2) 0.008(2) C13 0.054(4) 0.150(7) 0.094(5) -0.031(5) 0.031(4) 0.007(4) C14 0.051(3) 0.137(7) 0.066(4) -0.013(4) -0.005(3) 0.033(4) C15 0.035(2) 0.038(2) 0.043(2) 0.0020(19) 0.0040(19) 0.0121(19) C16 0.053(3) 0.048(3) 0.100(5) -0.008(3) 0.028(3) 0.017(3) C17 0.037(2) 0.042(3) 0.050(3) 0.004(2) 0.002(2) 0.009(2) C18 0.038(2) 0.030(2) 0.0226(18) 0.0029(15) 0.0026(16) 0.0120(17) C19 0.040(2) 0.029(2) 0.0253(19) 0.0019(16) 0.0039(16) 0.0114(17) C20 0.054(3) 0.031(2) 0.043(2) 0.0106(19) 0.009(2) 0.019(2) C21 0.057(3) 0.042(3) 0.056(3) 0.008(2) 0.012(2) 0.030(2) C22 0.039(2) 0.053(3) 0.042(3) 0.004(2) 0.008(2) 0.019(2) C23 0.040(2) 0.039(2) 0.031(2) 0.0056(18) 0.0051(18) 0.0135(19) C24 0.042(2) 0.033(2) 0.041(2) 0.0125(18) 0.0153(19) 0.0138(19) C25 0.070(3) 0.062(3) 0.041(3) 0.020(2) 0.023(2) 0.021(3) C26 0.045(3) 0.035(2) 0.047(3) 0.008(2) 0.011(2) 0.010(2) C27 0.040(2) 0.053(3) 0.052(3) 0.017(2) 0.010(2) 0.008(2) C28 0.103(5) 0.093(5) 0.080(5) 0.012(4) 0.053(4) -0.009(4) C29 0.122(6) 0.066(4) 0.078(5) -0.009(4) 0.029(4) -0.033(4) C30 0.0270(19) 0.031(2) 0.0226(18) -0.0009(15) 0.0056(15) 0.0064(16) C31 0.032(2) 0.032(2) 0.0258(19) 0.0040(16) 0.0061(16) 0.0050(17) C32 0.033(2) 0.041(2) 0.041(2) 0.014(2) 0.0064(18) 0.0021(19) C33 0.033(2) 0.041(2) 0.041(2) 0.011(2) 0.0078(18) 0.0037(19) C34 0.029(2) 0.045(2) 0.034(2) 0.0081(19) 0.0052(17) 0.0110(18) C35 0.0277(19) 0.030(2) 0.0274(19) 0.0034(16) 0.0060(15) 0.0071(16) C36 0.032(2) 0.032(2) 0.034(2) 0.0070(17) 0.0055(17) 0.0077(17) C37 0.046(3) 0.046(3) 0.055(3) 0.022(2) 0.006(2) 0.012(2) C38 0.048(3) 0.046(3) 0.042(2) 0.011(2) 0.011(2) 0.023(2) C39 0.034(2) 0.046(3) 0.037(2) 0.0108(19) 0.0055(18) 0.0117(19) C40 0.031(2) 0.065(3) 0.078(4) 0.033(3) 0.008(2) 0.001(2) C41 0.032(2) 0.035(2) 0.035(2) 0.0086(17) 0.0107(17) 0.0124(17) C42 0.044(2) 0.038(2) 0.043(3) 0.003(2) 0.004(2) 0.013(2) C43 0.051(3) 0.040(2) 0.048(3) 0.016(2) 0.024(2) 0.022(2) C44 0.038(2) 0.043(3) 0.046(2) 0.014(2) 0.0085(19) 0.015(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Pb N2 2.315(3) . ? Pb N1 2.315(3) . ? Pb Cl 2.6381(10) . ? Li O 1.849(7) 2 ? Li O 1.885(7) . ? Li Cl 2.358(7) . ? O C30 1.337(4) . ? O Li 1.849(7) 2 ? N1 C1 1.338(5) . ? N1 C6 1.432(5) . ? N2 C3 1.325(5) . ? N2 C18 1.438(5) . ? C1 C2 1.389(5) . ? C1 C4 1.512(5) . ? C2 C3 1.406(6) . ? C2 H2 0.95 . ? C3 C5 1.522(5) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 C11 1.410(6) . ? C6 C7 1.415(6) . ? C7 C8 1.382(6) . ? C7 C12 1.516(7) . ? C8 C9 1.375(8) . ? C8 H8 0.95 . ? C9 C10 1.380(7) . ? C9 H9 0.95 . ? C10 C11 1.400(6) . ? C10 H10 0.95 . ? C11 C15 1.516(6) . ? C12 C14 1.492(8) . ? C12 C13 1.515(8) . ? C12 H12 1 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 C17 1.527(6) . ? C15 C16 1.541(6) . ? C15 H15 1 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 C19 1.401(6) . ? C18 C23 1.409(6) . ? C19 C20 1.402(6) . ? C19 C24 1.516(6) . ? C20 C21 1.377(7) . ? C20 H20 0.95 . ? C21 C22 1.369(7) . ? C21 H21 0.95 . ? C22 C23 1.401(6) . ? C22 H22 0.95 . ? C23 C27 1.526(6) . ? C24 C25 1.537(6) . ? C24 C26 1.550(6) . ? C24 H24 1 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 C29 1.498(8) . ? C27 C28 1.511(8) . ? C27 H27 1 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C30 C31 1.434(5) . ? C30 C35 1.434(5) . ? C31 C32 1.403(6) . ? C31 C36 1.534(5) . ? C32 C33 1.390(6) . ? C32 H32 0.95 . ? C33 C34 1.372(6) . ? C33 C40 1.520(6) . ? C34 C35 1.396(5) . ? C34 H34 0.95 . ? C35 C41 1.537(6) . ? C36 C38 1.537(6) . ? C36 C37 1.539(6) . ? C36 C39 1.546(6) . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C38 H38A 0.98 . ? C38 H38B 0.98 . ? C38 H38C 0.98 . ? C39 H39A 0.98 . ? C39 H39B 0.98 . ? C39 H39C 0.98 . ? C40 H40A 0.98 . ? C40 H40B 0.98 . ? C40 H40C 0.98 . ? C40 H40D 0.98 . ? C40 H40E 0.98 . ? C40 H40F 0.98 . ? C41 C42 1.536(6) . ? C41 C43 1.538(6) . ? C41 C44 1.541(6) . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? C43 H43A 0.98 . ? C43 H43B 0.98 . ? C43 H43C 0.98 . ? C44 H44A 0.98 . ? C44 H44B 0.98 . ? C44 H44C 0.98 . ? C1S C2S 1.39 . ? C1S C6S 1.39 . ? C1S H1S 0.95 . ? C2S C3S 1.39 . ? C2S H2S 0.95 . ? C3S C4S 1.39 . ? C3S H3S 0.95 . ? C4S C5S 1.39 . ? C4S H4S 0.95 . ? C5S C6S 1.39 . ? C5S H5S 0.95 . ? C6S H6S 0.95 . ? C7S C8S 1.39 . ? C7S C12S 1.39 . ? C7S H7S 0.95 . ? C8S C9S 1.39 . ? C8S H8S 0.95 . ? C9S C10S 1.39 . ? C9S H9S 0.95 . ? C10S C11S 1.39 . ? C10S H10S 0.95 . ? C11S C12S 1.39 . ? C11S H11S 0.95 . ? C12S H12S 0.95 . ? C13S C14S 1.39 . ? C13S C18S 1.39 . ? C13S H13S 0.95 . ? C14S C15S 1.39 . ? C14S H14S 0.95 . ? C15S C16S 1.39 . ? C15S H15S 0.95 . ? C16S C17S 1.39 . ? C16S H16S 0.95 . ? C17S C18S 1.39 . ? C17S H17S 0.95 . ? C18S H18S 0.95 . ? C7T C8T 1.39 . ? C7T C12T 1.39 . ? C7T H7T 0.95 . ? C8T C9T 1.39 . ? C8T H8T 0.95 . ? C9T C10T 1.39 . ? C9T H9T 0.95 . ? C10T C11T 1.39 . ? C10T H10T 0.95 . ? C11T C12T 1.39 . ? C11T H11T 0.95 . ? C12T H12T 0.95 . ? C13T C14T 1.39 . ? C13T C18T 1.39 . ? C13T H13T 0.95 . ? C14T C15T 1.39 . ? C14T H14T 0.95 . ? C15T C16T 1.39 . ? C15T H15T 0.95 . ? C16T C17T 1.39 . ? C16T H16T 0.95 . ? C17T C18T 1.39 . ? C17T H17T 0.95 . ? C18T H18T 0.95 . ? 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 Pb N1 82.86(11) . . ? N2 Pb Cl 94.33(8) . . ? N1 Pb Cl 94.14(8) . . ? O Li O 96.8(3) 2 . ? O Li Cl 140.1(4) 2 . ? O Li Cl 123.2(3) . . ? Li Cl Pb 102.19(17) . . ? C30 O Li 145.3(3) . 2 ? C30 O Li 131.0(3) . . ? Li O Li 83.2(3) 2 . ? C1 N1 C6 120.2(3) . . ? C1 N1 Pb 127.0(3) . . ? C6 N1 Pb 112.7(2) . . ? C3 N2 C18 121.6(3) . . ? C3 N2 Pb 127.3(3) . . ? C18 N2 Pb 111.0(2) . . ? N1 C1 C2 125.1(4) . . ? N1 C1 C4 119.4(3) . . ? C2 C1 C4 115.5(4) . . ? C1 C2 C3 131.9(4) . . ? C1 C2 H2 114.1 . . ? C3 C2 H2 114.1 . . ? N2 C3 C2 125.0(4) . . ? N2 C3 C5 120.5(4) . . ? C2 C3 C5 114.5(3) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C11 C6 C7 120.9(4) . . ? C11 C6 N1 121.1(4) . . ? C7 C6 N1 117.9(4) . . ? C8 C7 C6 118.1(4) . . ? C8 C7 C12 120.6(4) . . ? C6 C7 C12 121.4(4) . . ? C9 C8 C7 121.8(5) . . ? C9 C8 H8 119.1 . . ? C7 C8 H8 119.1 . . ? C8 C9 C10 120.1(4) . . ? C8 C9 H9 120 . . ? C10 C9 H9 120 . . ? C9 C10 C11 121.0(5) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C10 C11 C6 118.0(4) . . ? C10 C11 C15 119.0(4) . . ? C6 C11 C15 123.0(4) . . ? C14 C12 C13 108.9(5) . . ? C14 C12 C7 111.9(4) . . ? C13 C12 C7 113.6(5) . . ? C14 C12 H12 107.4 . . ? C13 C12 H12 107.4 . . ? C7 C12 H12 107.4 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C17 112.4(4) . . ? C11 C15 C16 111.4(4) . . ? C17 C15 C16 109.2(4) . . ? C11 C15 H15 107.9 . . ? C17 C15 H15 107.9 . . ? C16 C15 H15 107.9 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 121.1(4) . . ? C19 C18 N2 120.9(4) . . ? C23 C18 N2 117.9(4) . . ? C18 C19 C20 118.0(4) . . ? C18 C19 C24 123.5(4) . . ? C20 C19 C24 118.4(4) . . ? C21 C20 C19 121.2(4) . . ? C21 C20 H20 119.4 . . ? C19 C20 H20 119.4 . . ? C22 C21 C20 120.4(4) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 121.0(4) . . ? C21 C22 H22 119.5 . . ? C23 C22 H22 119.5 . . ? C22 C23 C18 118.2(4) . . ? C22 C23 C27 120.2(4) . . ? C18 C23 C27 121.6(4) . . ? C19 C24 C25 111.5(4) . . ? C19 C24 C26 111.3(3) . . ? C25 C24 C26 108.9(4) . . ? C19 C24 H24 108.3 . . ? C25 C24 H24 108.3 . . ? C26 C24 H24 108.3 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C28 111.0(5) . . ? C29 C27 C23 111.2(4) . . ? C28 C27 C23 114.0(5) . . ? C29 C27 H27 106.8 . . ? C28 C27 H27 106.8 . . ? C23 C27 H27 106.8 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O C30 C31 120.9(3) . . ? O C30 C35 120.3(3) . . ? C31 C30 C35 118.8(3) . . ? C32 C31 C30 118.5(4) . . ? C32 C31 C36 119.3(4) . . ? C30 C31 C36 122.2(3) . . ? C33 C32 C31 122.8(4) . . ? C33 C32 H32 118.6 . . ? C31 C32 H32 118.6 . . ? C34 C33 C32 117.8(4) . . ? C34 C33 C40 121.4(4) . . ? C32 C33 C40 120.8(4) . . ? C33 C34 C35 123.7(4) . . ? C33 C34 H34 118.1 . . ? C35 C34 H34 118.1 . . ? C34 C35 C30 118.4(4) . . ? C34 C35 C41 119.2(3) . . ? C30 C35 C41 122.3(3) . . ? C31 C36 C38 110.7(3) . . ? C31 C36 C37 113.0(3) . . ? C38 C36 C37 106.7(4) . . ? C31 C36 C39 109.9(3) . . ? C38 C36 C39 110.4(3) . . ? C37 C36 C39 106.0(3) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C33 C40 H40A 109.5 . . ? C33 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C33 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C33 C40 H40D 109.5 . . ? H40A C40 H40D 141.1 . . ? H40B C40 H40D 56.3 . . ? H40C C40 H40D 56.3 . . ? C33 C40 H40E 109.5 . . ? H40A C40 H40E 56.3 . . ? H40B C40 H40E 141.1 . . ? H40C C40 H40E 56.3 . . ? H40D C40 H40E 109.5 . . ? C33 C40 H40F 109.5 . . ? H40A C40 H40F 56.3 . . ? H40B C40 H40F 56.3 . . ? H40C C40 H40F 141.1 . . ? H40D C40 H40F 109.5 . . ? H40E C40 H40F 109.5 . . ? C42 C41 C35 110.1(3) . . ? C42 C41 C43 110.5(4) . . ? C35 C41 C43 111.5(3) . . ? C42 C41 C44 105.9(3) . . ? C35 C41 C44 113.0(3) . . ? C43 C41 C44 105.7(3) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? C2S C1S C6S 120 . . ? C2S C1S H1S 120 . . ? C6S C1S H1S 120 . . ? C3S C2S C1S 120 . . ? C3S C2S H2S 120 . . ? C1S C2S H2S 120 . . ? C2S C3S C4S 120 . . ? C2S C3S H3S 120 . . ? C4S C3S H3S 120 . . ? C5S C4S C3S 120 . . ? C5S C4S H4S 120 . . ? C3S C4S H4S 120 . . ? C4S C5S C6S 120 . . ? C4S C5S H5S 120 . . ? C6S C5S H5S 120 . . ? C5S C6S C1S 120 . . ? C5S C6S H6S 120 . . ? C1S C6S H6S 120 . . ? C8S C7S C12S 120 . . ? C8S C7S H7S 120 . . ? C12S C7S H7S 120 . . ? C7S C8S C9S 120 . . ? C7S C8S H8S 120 . . ? C9S C8S H8S 120 . . ? C10S C9S C8S 120 . . ? C10S C9S H9S 120 . . ? C8S C9S H9S 120 . . ? C11S C10S C9S 120 . . ? C11S C10S H10S 120 . . ? C9S C10S H10S 120 . . ? C10S C11S C12S 120 . . ? C10S C11S H11S 120 . . ? C12S C11S H11S 120 . . ? C11S C12S C7S 120 . . ? C11S C12S H12S 120 . . ? C7S C12S H12S 120 . . ? C14S C13S C18S 120 . . ? C14S C13S H13S 120 . . ? C18S C13S H13S 120 . . ? C15S C14S C13S 120 . . ? C15S C14S H14S 120 . . ? C13S C14S H14S 120 . . ? C16S C15S C14S 120 . . ? C16S C15S H15S 120 . . ? C14S C15S H15S 120 . . ? C15S C16S C17S 120 . . ? C15S C16S H16S 120 . . ? C17S C16S H16S 120 . . ? C16S C17S C18S 120 . . ? C16S C17S H17S 120 . . ? C18S C17S H17S 120 . . ? C17S C18S C13S 120 . . ? C17S C18S H18S 120 . . ? C13S C18S H18S 120 . . ? C8T C7T C12T 120 . . ? C8T C7T H7T 120 . . ? C12T C7T H7T 120 . . ? C9T C8T C7T 120 . . ? C9T C8T H8T 120 . . ? C7T C8T H8T 120 . . ? C8T C9T C10T 120 . . ? C8T C9T H9T 120 . . ? C10T C9T H9T 120 . . ? C11T C10T C9T 120 . . ? C11T C10T H10T 120 . . ? C9T C10T H10T 120 . . ? C10T C11T C12T 120 . . ? C10T C11T H11T 120 . . ? C12T C11T H11T 120 . . ? C11T C12T C7T 120 . . ? C11T C12T H12T 120 . . ? C7T C12T H12T 120 . . ? C14T C13T C18T 120 . . ? C14T C13T H13T 120 . . ? C18T C13T H13T 120 . . ? C15T C14T C13T 120 . . ? C15T C14T H14T 120 . . ? C13T C14T H14T 120 . . ? C14T C15T C16T 120 . . ? C14T C15T H15T 120 . . ? C16T C15T H15T 120 . . ? C17T C16T C15T 120 . . ? C17T C16T H16T 120 . . ? C15T C16T H16T 120 . . ? C16T C17T C18T 120 . . ? C16T C17T H17T 120 . . ? C18T C17T H17T 120 . . ? C17T C18T C13T 120 . . ? C17T C18T H18T 120 . . ? C13T C18T H18T 120 . . ? #===END data_(4)-aug1706 _database_code_depnum_ccdc_archive 'CCDC 641615' _audit_creation_date 2006-08-22T08:59:58-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C43 H62 N2 O Pb, C7 H8' _chemical_formula_sum 'C50 H70 N2 O Pb' _chemical_formula_weight 922.27 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' _symmetry_Int_Tables_number 15 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 34.4733(12) _cell_length_b 12.0183(4) _cell_length_c 26.7006(8) _cell_angle_alpha 90 _cell_angle_beta 123.008(2) _cell_angle_gamma 90 _cell_volume 9276.8(5) _cell_formula_units_Z 8 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 135201 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 22.986 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.025 _exptl_crystal_density_diffrn 1.321 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3792 _exptl_special_details ; Diffraction was weak and limited in extent . ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.673 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.6325 _exptl_absorpt_correction_T_max 0.8637 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_detector_area_resol_mean 9 _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 -0.50921E-2 _diffrn_orient_matrix_ub_12 -0.795405E-1 _diffrn_orient_matrix_ub_13 -0.130935E-1 _diffrn_orient_matrix_ub_21 0.13497E-2 _diffrn_orient_matrix_ub_22 0.208817E-1 _diffrn_orient_matrix_ub_23 -0.35275E-1 _diffrn_orient_matrix_ub_31 0.341876E-1 _diffrn_orient_matrix_ub_32 -0.126715E-1 _diffrn_orient_matrix_ub_33 0.240586E-1 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0743 _diffrn_reflns_av_unetI/netI 0.0344 _diffrn_reflns_number 51583 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 37 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -29 _diffrn_reflns_limit_l_max 29 _diffrn_reflns_theta_min 3.41 _diffrn_reflns_theta_max 22.99 _diffrn_reflns_theta_full 22.99 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 6421 _reflns_number_gt 5466 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1986)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; The C6 ring of the toluene solvate was included as a rigid body . 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. ; _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^)+(0.0248P)^2^+85.3262P] 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_number_reflns 6421 _refine_ls_number_parameters 474 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0509 _refine_ls_R_factor_gt 0.0393 _refine_ls_wR_factor_ref 0.0927 _refine_ls_wR_factor_gt 0.0871 _refine_ls_goodness_of_fit_ref 1.142 _refine_ls_restrained_S_all 1.142 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.722 _refine_diff_density_min -0.836 _refine_diff_density_rms 0.095 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _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 Pb Pb 0.647722(9) 0.30106(2) 0.986253(11) 0.03561(10) Uani 1 1 d . . . O O 0.69863(15) 0.3018(4) 1.08239(18) 0.0412(11) Uani 1 1 d . . . N1 N 0.59400(18) 0.2346(4) 1.0039(2) 0.0378(13) Uani 1 1 d . . . N2 N 0.62663(19) 0.4668(4) 1.0052(2) 0.0350(13) Uani 1 1 d . . . C1 C 0.5852(2) 0.2819(6) 1.0409(3) 0.0406(17) Uani 1 1 d . . . C2 C 0.5996(2) 0.3896(6) 1.0642(3) 0.0438(17) Uani 1 1 d . . . H2 H 0.5977 0.4062 1.0977 0.053 Uiso 1 1 calc R . . C3 C 0.6162(2) 0.4761(6) 1.0459(3) 0.0415(17) Uani 1 1 d . . . C4 C 0.5585(3) 0.2185(7) 1.0618(4) 0.058(2) Uani 1 1 d . . . H4A H 0.5252 0.2274 1.0326 0.087 Uiso 1 1 calc R . . H4B H 0.5664 0.2476 1.1006 0.087 Uiso 1 1 calc R . . H4C H 0.5666 0.1394 1.0658 0.087 Uiso 1 1 calc R . . C5 C 0.6222(3) 0.5886(6) 1.0755(3) 0.056(2) Uani 1 1 d . . . H5A H 0.6547 0.6114 1.0963 0.084 Uiso 1 1 calc R . . H5B H 0.6129 0.5829 1.1042 0.084 Uiso 1 1 calc R . . H5C H 0.6028 0.644 1.0449 0.084 Uiso 1 1 calc R . . C6 C 0.5720(2) 0.1303(6) 0.9746(3) 0.0410(17) Uani 1 1 d . . . C7 C 0.5292(3) 0.1323(6) 0.9211(4) 0.054(2) Uani 1 1 d . . . C8 C 0.5099(3) 0.0300(7) 0.8923(4) 0.065(2) Uani 1 1 d . . . H8 H 0.4807 0.0295 0.8556 0.078 Uiso 1 1 calc R . . C9 C 0.5326(3) -0.0690(7) 0.9162(4) 0.061(2) Uani 1 1 d . . . H9 H 0.5188 -0.1372 0.8964 0.073 Uiso 1 1 calc R . . C10 C 0.5747(3) -0.0683(6) 0.9682(4) 0.058(2) Uani 1 1 d . . . H10 H 0.5903 -0.1371 0.9841 0.07 Uiso 1 1 calc R . . C11 C 0.5961(3) 0.0295(6) 0.9992(3) 0.0459(18) Uani 1 1 d . . . C12 C 0.5030(3) 0.2398(8) 0.8925(4) 0.076(3) Uani 1 1 d . . . H12 H 0.5224 0.3035 0.918 0.091 Uiso 1 1 calc R . . C13 C 0.4935(4) 0.2555(10) 0.8314(5) 0.108(4) Uani 1 1 d . . . H13A H 0.4772 0.3261 0.8149 0.161 Uiso 1 1 calc R . . H13B H 0.4742 0.1941 0.8057 0.161 Uiso 1 1 calc R . . H13C H 0.5228 0.2566 0.8335 0.161 Uiso 1 1 calc R . . C14 C 0.4564(4) 0.2416(12) 0.8890(6) 0.135(5) Uani 1 1 d . . . H14A H 0.4624 0.233 0.9291 0.202 Uiso 1 1 calc R . . H14B H 0.4367 0.1804 0.8636 0.202 Uiso 1 1 calc R . . H14C H 0.4406 0.3126 0.872 0.202 Uiso 1 1 calc R . . C15 C 0.6428(3) 0.0245(6) 1.0569(3) 0.056(2) Uani 1 1 d . . . H15 H 0.6524 0.1025 1.0717 0.067 Uiso 1 1 calc R . . C16 C 0.6416(4) -0.0411(8) 1.1053(4) 0.088(3) Uani 1 1 d . . . H16A H 0.6726 -0.0418 1.142 0.133 Uiso 1 1 calc R . . H16B H 0.6317 -0.1176 1.0916 0.133 Uiso 1 1 calc R . . H16C H 0.6199 -0.0058 1.1132 0.133 Uiso 1 1 calc R . . C17 C 0.6801(3) -0.0266(8) 1.0492(5) 0.086(3) Uani 1 1 d . . . H17A H 0.7097 -0.0278 1.0878 0.129 Uiso 1 1 calc R . . H17B H 0.683 0.018 1.0207 0.129 Uiso 1 1 calc R . . H17C H 0.6712 -0.1028 1.0341 0.129 Uiso 1 1 calc R . . C18 C 0.6328(2) 0.5638(5) 0.9784(3) 0.0380(17) Uani 1 1 d . . . C19 C 0.5938(2) 0.6063(6) 0.9262(3) 0.0425(17) Uani 1 1 d . . . C20 C 0.5994(3) 0.6985(6) 0.8999(3) 0.0490(18) Uani 1 1 d . . . H20 H 0.5733 0.7287 0.8647 0.059 Uiso 1 1 calc R . . C21 C 0.6421(3) 0.7478(6) 0.9238(4) 0.053(2) Uani 1 1 d . . . H21 H 0.645 0.8129 0.9058 0.063 Uiso 1 1 calc R . . C22 C 0.6803(3) 0.7031(6) 0.9732(3) 0.0463(18) Uani 1 1 d . . . H22 H 0.7098 0.7353 0.9876 0.056 Uiso 1 1 calc R . . C23 C 0.6772(3) 0.6111(6) 1.0030(3) 0.0417(17) Uani 1 1 d . . . C24 C 0.5467(2) 0.5513(6) 0.8980(3) 0.0494(19) Uani 1 1 d . . . H24 H 0.5521 0.4695 0.9053 0.059 Uiso 1 1 calc R . . C25 C 0.5153(3) 0.5678(10) 0.8309(4) 0.088(3) Uani 1 1 d . . . H25A H 0.4859 0.5294 0.8159 0.132 Uiso 1 1 calc R . . H25B H 0.5302 0.5371 0.8115 0.132 Uiso 1 1 calc R . . H25C H 0.5096 0.6474 0.8219 0.132 Uiso 1 1 calc R . . C26 C 0.5202(3) 0.5894(8) 0.9261(4) 0.076(3) Uani 1 1 d . . . H26A H 0.4904 0.5508 0.9067 0.114 Uiso 1 1 calc R . . H26B H 0.515 0.6699 0.9206 0.114 Uiso 1 1 calc R . . H26C H 0.5384 0.572 0.9688 0.114 Uiso 1 1 calc R . . C27 C 0.7197(2) 0.5648(6) 1.0580(3) 0.0422(17) Uani 1 1 d . . . H27 H 0.7094 0.5093 1.0763 0.051 Uiso 1 1 calc R . . C28 C 0.7474(3) 0.6553(7) 1.1046(3) 0.063(2) Uani 1 1 d . . . H28A H 0.7745 0.6219 1.1398 0.095 Uiso 1 1 calc R . . H28B H 0.7278 0.6906 1.1163 0.095 Uiso 1 1 calc R . . H28C H 0.7576 0.7114 1.0875 0.095 Uiso 1 1 calc R . . C29 C 0.7513(3) 0.5046(7) 1.0429(3) 0.0521(19) Uani 1 1 d . . . H29A H 0.7783 0.4749 1.0796 0.078 Uiso 1 1 calc R . . H29B H 0.7615 0.5571 1.0243 0.078 Uiso 1 1 calc R . . H29C H 0.7342 0.4434 1.0152 0.078 Uiso 1 1 calc R . . C30 C 0.7370(2) 0.2389(5) 1.1129(3) 0.0349(15) Uani 1 1 d . . . C31 C 0.7588(2) 0.2207(5) 1.1750(3) 0.0363(16) Uani 1 1 d . . . C32 C 0.7962(2) 0.1470(6) 1.2027(3) 0.0381(16) Uani 1 1 d . . . H32 H 0.8104 0.1337 1.2442 0.046 Uiso 1 1 calc R . . C33 C 0.8140(2) 0.0917(6) 1.1735(3) 0.0373(16) Uani 1 1 d . . . C34 C 0.7938(2) 0.1165(6) 1.1140(3) 0.0434(17) Uani 1 1 d . . . H34 H 0.8056 0.0826 1.0928 0.052 Uiso 1 1 calc R . . C35 C 0.7568(2) 0.1894(6) 1.0837(3) 0.0440(18) Uani 1 1 d . . . H35 H 0.7445 0.2062 1.043 0.053 Uiso 1 1 calc R . . C36 C 0.7412(2) 0.2765(5) 1.2109(3) 0.0389(17) Uani 1 1 d . . . C37 C 0.7383(3) 0.4045(6) 1.2016(3) 0.0505(19) Uani 1 1 d . . . H37A H 0.7689 0.4336 1.2145 0.076 Uiso 1 1 calc R . . H37B H 0.7276 0.4393 1.2251 0.076 Uiso 1 1 calc R . . H37C H 0.7165 0.4215 1.1592 0.076 Uiso 1 1 calc R . . C38 C 0.7740(3) 0.2553(7) 1.2780(3) 0.052(2) Uani 1 1 d . . . H38A H 0.8048 0.284 1.2915 0.078 Uiso 1 1 calc R . . H38B H 0.7759 0.1752 1.2858 0.078 Uiso 1 1 calc R . . H38C H 0.7622 0.2932 1.2996 0.078 Uiso 1 1 calc R . . C39 C 0.6938(3) 0.2320(6) 1.1910(3) 0.0503(19) Uani 1 1 d . . . H39A H 0.6724 0.2457 1.1481 0.075 Uiso 1 1 calc R . . H39B H 0.6825 0.2698 1.2131 0.075 Uiso 1 1 calc R . . H39C H 0.6959 0.1519 1.1987 0.075 Uiso 1 1 calc R . . C40 C 0.8517(2) 0.0026(6) 1.2037(3) 0.0458(18) Uani 1 1 d . . . C41 C 0.8735(3) -0.0037(7) 1.2711(3) 0.054(2) Uani 1 1 d . . . H41A H 0.8974 -0.0616 1.2882 0.081 Uiso 1 1 calc R . . H41B H 0.8496 -0.0218 1.279 0.081 Uiso 1 1 calc R . . H41C H 0.8875 0.0682 1.2893 0.081 Uiso 1 1 calc R . . C42 C 0.8295(3) -0.1109(7) 1.1768(4) 0.069(2) Uani 1 1 d . . . H42A H 0.8531 -0.1693 1.1953 0.103 Uiso 1 1 calc R . . H42B H 0.816 -0.1098 1.1337 0.103 Uiso 1 1 calc R . . H42C H 0.8051 -0.126 1.1843 0.103 Uiso 1 1 calc R . . C43 C 0.8900(3) 0.0245(9) 1.1921(4) 0.074(3) Uani 1 1 d . . . H43A H 0.9138 -0.0333 1.2115 0.111 Uiso 1 1 calc R . . H43B H 0.904 0.0975 1.2083 0.111 Uiso 1 1 calc R . . H43C H 0.8768 0.0234 1.149 0.111 Uiso 1 1 calc R . . C1S C 0.3958(3) 0.0387(7) 0.6925(3) 0.140(6) Uani 1 1 d G . . C2S C 0.3700(3) 0.0413(10) 0.7182(5) 0.179(10) Uani 1 1 d G . . H2S H 0.3485 0.0999 0.7088 0.215 Uiso 1 1 calc R . . C3S C 0.3756(4) -0.0418(13) 0.7579(4) 0.251(18) Uani 1 1 d G . . H3S H 0.3579 -0.0401 0.7755 0.301 Uiso 1 1 calc R . . C4S C 0.4069(5) -0.1275(10) 0.7717(4) 0.217(14) Uani 1 1 d G . . H4S H 0.4108 -0.1843 0.7988 0.261 Uiso 1 1 calc R . . C5S C 0.4327(4) -0.1301(8) 0.7459(5) 0.168(8) Uani 1 1 d G . . H5S H 0.4542 -0.1887 0.7554 0.202 Uiso 1 1 calc R . . C6S C 0.4271(3) -0.0470(9) 0.7063(4) 0.117(5) Uani 1 1 d G . . H6S H 0.4448 -0.0487 0.6887 0.14 Uiso 1 1 calc R . . C7S C 0.3864(4) 0.1185(9) 0.6549(5) 0.188(9) Uani 1 1 d G . . H7S1 H 0.4058 0.1112 0.6387 0.282 Uiso 0.5 1 calc PR . . H7S2 H 0.3925 0.1902 0.6753 0.282 Uiso 0.5 1 calc PR . . H7S3 H 0.3537 0.1144 0.6223 0.282 Uiso 0.5 1 calc PR . . H7S4 H 0.3622 0.166 0.6522 0.282 Uiso 0.5 1 calc PR . . H7S5 H 0.3755 0.087 0.6155 0.282 Uiso 0.5 1 calc PR . . H7S6 H 0.4143 0.1628 0.6686 0.282 Uiso 0.5 1 calc PR . . 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 Pb 0.04193(16) 0.03535(16) 0.03258(15) -0.00066(12) 0.02226(12) 0.00430(13) O 0.040(3) 0.052(3) 0.031(2) 0.004(2) 0.019(2) 0.012(2) N1 0.040(3) 0.037(3) 0.037(3) -0.002(3) 0.021(3) 0.001(3) N2 0.047(3) 0.028(3) 0.034(3) -0.002(2) 0.025(3) 0.001(3) C1 0.046(4) 0.036(4) 0.049(4) 0.006(3) 0.032(4) 0.007(3) C2 0.052(4) 0.044(4) 0.046(4) 0.001(4) 0.033(4) 0.008(4) C3 0.052(4) 0.032(4) 0.043(4) 0.000(3) 0.028(4) 0.002(3) C4 0.078(6) 0.053(5) 0.068(5) 0.001(4) 0.056(5) 0.002(4) C5 0.085(6) 0.043(5) 0.059(5) -0.009(4) 0.051(5) -0.002(4) C6 0.049(4) 0.034(4) 0.049(4) 0.005(3) 0.033(4) 0.000(3) C7 0.047(5) 0.043(5) 0.060(5) -0.003(4) 0.021(4) -0.002(4) C8 0.046(5) 0.063(6) 0.067(6) -0.013(5) 0.018(4) -0.012(4) C9 0.059(5) 0.041(5) 0.067(6) -0.012(4) 0.024(5) -0.008(4) C10 0.072(6) 0.035(5) 0.064(5) 0.000(4) 0.034(5) 0.005(4) C11 0.054(5) 0.035(4) 0.048(4) 0.001(3) 0.028(4) 0.003(4) C12 0.059(6) 0.060(6) 0.067(6) 0.003(5) 0.008(5) 0.007(5) C13 0.113(9) 0.096(8) 0.096(9) 0.039(7) 0.046(8) 0.024(7) C14 0.111(10) 0.141(12) 0.154(12) 0.036(10) 0.073(10) 0.077(9) C15 0.065(5) 0.032(4) 0.051(5) -0.002(4) 0.020(4) 0.004(4) C16 0.125(9) 0.050(6) 0.068(6) 0.008(5) 0.038(6) 0.010(6) C17 0.058(6) 0.068(6) 0.107(8) -0.017(6) 0.028(6) 0.012(5) C18 0.056(5) 0.032(4) 0.035(4) -0.003(3) 0.030(4) 0.002(3) C19 0.047(4) 0.042(4) 0.043(4) 0.000(3) 0.027(4) 0.009(4) C20 0.058(5) 0.048(5) 0.044(4) 0.008(4) 0.030(4) 0.016(4) C21 0.076(6) 0.040(4) 0.057(5) 0.007(4) 0.046(5) 0.006(4) C22 0.055(5) 0.045(4) 0.050(4) -0.002(4) 0.036(4) -0.003(4) C23 0.061(5) 0.035(4) 0.042(4) -0.001(3) 0.036(4) -0.001(4) C24 0.046(4) 0.047(5) 0.046(4) 0.006(4) 0.020(4) 0.009(4) C25 0.056(6) 0.138(10) 0.057(6) 0.007(6) 0.023(5) 0.004(6) C26 0.070(6) 0.085(7) 0.091(7) 0.004(6) 0.055(6) -0.002(5) C27 0.046(4) 0.045(4) 0.035(4) -0.005(3) 0.022(4) -0.006(3) C28 0.069(6) 0.061(5) 0.046(5) -0.011(4) 0.022(4) -0.013(4) C29 0.047(4) 0.064(5) 0.043(4) 0.000(4) 0.022(4) 0.003(4) C30 0.039(4) 0.036(4) 0.031(4) -0.001(3) 0.020(3) 0.002(3) C31 0.040(4) 0.035(4) 0.036(4) -0.002(3) 0.023(3) 0.002(3) C32 0.041(4) 0.045(4) 0.026(3) -0.003(3) 0.017(3) -0.005(3) C33 0.035(4) 0.041(4) 0.035(4) -0.009(3) 0.019(3) -0.003(3) C34 0.040(4) 0.056(5) 0.039(4) -0.002(3) 0.025(3) 0.007(4) C35 0.044(4) 0.060(5) 0.028(4) 0.008(3) 0.020(3) 0.010(4) C36 0.050(4) 0.039(4) 0.030(4) -0.001(3) 0.024(3) 0.004(3) C37 0.071(5) 0.041(4) 0.055(5) -0.005(4) 0.045(4) 0.002(4) C38 0.064(5) 0.057(5) 0.037(4) -0.005(4) 0.028(4) 0.009(4) C39 0.059(5) 0.057(5) 0.052(5) -0.005(4) 0.041(4) -0.001(4) C40 0.041(4) 0.056(5) 0.037(4) 0.003(4) 0.020(3) 0.010(4) C41 0.047(4) 0.063(5) 0.039(4) 0.005(4) 0.015(4) 0.011(4) C42 0.083(6) 0.051(5) 0.057(5) -0.002(4) 0.028(5) 0.016(5) C43 0.056(5) 0.113(8) 0.062(5) 0.014(5) 0.038(5) 0.021(5) C1S 0.142(14) 0.126(13) 0.102(10) -0.014(10) 0.034(10) -0.062(11) C2S 0.132(12) 0.33(3) 0.126(13) -0.123(15) 0.100(11) -0.137(15) C3S 0.141(18) 0.47(5) 0.15(2) -0.16(3) 0.087(16) -0.16(2) C4S 0.24(3) 0.29(3) 0.082(10) -0.054(14) 0.064(14) -0.20(2) C5S 0.206(18) 0.174(17) 0.085(11) -0.057(11) 0.053(12) -0.094(14) C6S 0.108(10) 0.104(10) 0.105(10) -0.033(8) 0.036(8) 0.004(8) C7S 0.199(17) 0.134(14) 0.119(12) 0.041(10) 0.014(11) -0.075(12) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Pb O 2.182(4) . ? Pb N2 2.270(5) . ? Pb N1 2.288(5) . ? O C30 1.345(8) . ? N1 C1 1.313(8) . ? N1 C6 1.453(9) . ? N2 C3 1.322(8) . ? N2 C18 1.445(8) . ? C1 C2 1.404(10) . ? C1 C4 1.517(10) . ? C2 C3 1.398(10) . ? C2 H2 0.95 . ? C3 C5 1.521(10) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 C7 1.386(10) . ? C6 C11 1.412(10) . ? C7 C8 1.410(11) . ? C7 C12 1.522(11) . ? C8 C9 1.374(11) . ? C8 H8 0.95 . ? C9 C10 1.358(11) . ? C9 H9 0.95 . ? C10 C11 1.394(10) . ? C10 H10 0.95 . ? C11 C15 1.506(10) . ? C12 C13 1.490(14) . ? C12 C14 1.559(15) . ? C12 H12 1 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 C16 1.531(12) . ? C15 C17 1.537(12) . ? C15 H15 1 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 C19 1.404(9) . ? C18 C23 1.414(10) . ? C19 C20 1.379(10) . ? C19 C24 1.520(10) . ? C20 C21 1.380(11) . ? C20 H20 0.95 . ? C21 C22 1.368(10) . ? C21 H21 0.95 . ? C22 C23 1.400(10) . ? C22 H22 0.95 . ? C23 C27 1.507(10) . ? C24 C25 1.519(11) . ? C24 C26 1.533(11) . ? C24 H24 1 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 C29 1.532(10) . ? C27 C28 1.532(10) . ? C27 H27 1 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C30 C31 1.415(9) . ? C30 C35 1.416(9) . ? C31 C32 1.398(9) . ? C31 C36 1.540(9) . ? C32 C33 1.397(9) . ? C32 H32 0.95 . ? C33 C34 1.375(9) . ? C33 C40 1.531(10) . ? C34 C35 1.387(9) . ? C34 H34 0.95 . ? C35 H35 0.95 . ? C36 C39 1.513(10) . ? C36 C38 1.531(9) . ? C36 C37 1.553(10) . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C38 H38A 0.98 . ? C38 H38B 0.98 . ? C38 H38C 0.98 . ? C39 H39A 0.98 . ? C39 H39B 0.98 . ? C39 H39C 0.98 . ? C40 C41 1.528(9) . ? C40 C43 1.536(10) . ? C40 C42 1.538(11) . ? C41 H41A 0.98 . ? C41 H41B 0.98 . ? C41 H41C 0.98 . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? C43 H43A 0.98 . ? C43 H43B 0.98 . ? C43 H43C 0.98 . ? C1S C7S 1.2945 . ? C1S C2S 1.39 . ? C1S C6S 1.39 . ? C2S C3S 1.39 . ? C2S H2S 0.95 . ? C3S C4S 1.39 . ? C3S H3S 0.95 . ? C4S C5S 1.39 . ? C4S H4S 0.95 . ? C5S C6S 1.39 . ? C5S H5S 0.95 . ? C6S H6S 0.95 . ? C7S H7S1 0.98 . ? C7S H7S2 0.98 . ? C7S H7S3 0.98 . ? C7S H7S4 0.98 . ? C7S H7S5 0.98 . ? C7S H7S6 0.98 . ? 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 O Pb N2 83.32(18) . . ? O Pb N1 88.97(18) . . ? N2 Pb N1 82.34(19) . . ? C30 O Pb 127.3(4) . . ? C1 N1 C6 120.8(6) . . ? C1 N1 Pb 123.4(5) . . ? C6 N1 Pb 115.7(4) . . ? C3 N2 C18 121.3(5) . . ? C3 N2 Pb 121.4(4) . . ? C18 N2 Pb 116.4(4) . . ? N1 C1 C2 124.2(6) . . ? N1 C1 C4 119.8(6) . . ? C2 C1 C4 116.1(6) . . ? C3 C2 C1 130.1(6) . . ? C3 C2 H2 115 . . ? C1 C2 H2 115 . . ? N2 C3 C2 124.8(6) . . ? N2 C3 C5 118.7(6) . . ? C2 C3 C5 116.5(6) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 121.3(7) . . ? C7 C6 N1 119.3(6) . . ? C11 C6 N1 119.2(6) . . ? C6 C7 C8 117.9(7) . . ? C6 C7 C12 122.6(7) . . ? C8 C7 C12 119.5(7) . . ? C9 C8 C7 121.5(8) . . ? C9 C8 H8 119.3 . . ? C7 C8 H8 119.3 . . ? C10 C9 C8 119.4(7) . . ? C10 C9 H9 120.3 . . ? C8 C9 H9 120.3 . . ? C9 C10 C11 122.5(7) . . ? C9 C10 H10 118.8 . . ? C11 C10 H10 118.8 . . ? C10 C11 C6 117.4(7) . . ? C10 C11 C15 119.9(7) . . ? C6 C11 C15 122.6(7) . . ? C13 C12 C7 111.9(8) . . ? C13 C12 C14 109.1(9) . . ? C7 C12 C14 110.7(9) . . ? C13 C12 H12 108.4 . . ? C7 C12 H12 108.4 . . ? C14 C12 H12 108.4 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 112.2(7) . . ? C11 C15 C17 112.6(7) . . ? C16 C15 C17 108.4(7) . . ? C11 C15 H15 107.8 . . ? C16 C15 H15 107.8 . . ? C17 C15 H15 107.8 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C19 C18 C23 121.6(6) . . ? C19 C18 N2 117.8(6) . . ? C23 C18 N2 120.6(6) . . ? C20 C19 C18 118.3(7) . . ? C20 C19 C24 120.3(6) . . ? C18 C19 C24 121.4(6) . . ? C19 C20 C21 121.3(7) . . ? C19 C20 H20 119.4 . . ? C21 C20 H20 119.4 . . ? C22 C21 C20 120.1(7) . . ? C22 C21 H21 120 . . ? C20 C21 H21 120 . . ? C21 C22 C23 121.8(7) . . ? C21 C22 H22 119.1 . . ? C23 C22 H22 119.1 . . ? C22 C23 C18 116.9(7) . . ? C22 C23 C27 120.8(7) . . ? C18 C23 C27 122.4(6) . . ? C25 C24 C19 114.2(7) . . ? C25 C24 C26 107.9(7) . . ? C19 C24 C26 112.9(6) . . ? C25 C24 H24 107.2 . . ? C19 C24 H24 107.2 . . ? C26 C24 H24 107.2 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 111.7(5) . . ? C23 C27 C28 112.0(6) . . ? C29 C27 C28 109.3(6) . . ? C23 C27 H27 107.9 . . ? C29 C27 H27 107.9 . . ? C28 C27 H27 107.9 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O C30 C31 121.1(5) . . ? O C30 C35 120.8(6) . . ? C31 C30 C35 118.1(6) . . ? C32 C31 C30 117.9(6) . . ? C32 C31 C36 120.5(6) . . ? C30 C31 C36 121.6(6) . . ? C33 C32 C31 124.4(6) . . ? C33 C32 H32 117.8 . . ? C31 C32 H32 117.8 . . ? C34 C33 C32 116.2(6) . . ? C34 C33 C40 120.8(6) . . ? C32 C33 C40 122.9(6) . . ? C33 C34 C35 122.4(6) . . ? C33 C34 H34 118.8 . . ? C35 C34 H34 118.8 . . ? C34 C35 C30 120.7(6) . . ? C34 C35 H35 119.6 . . ? C30 C35 H35 119.6 . . ? C39 C36 C38 108.6(6) . . ? C39 C36 C31 110.1(5) . . ? C38 C36 C31 111.5(6) . . ? C39 C36 C37 109.3(6) . . ? C38 C36 C37 107.1(6) . . ? C31 C36 C37 110.1(5) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C41 C40 C33 112.8(6) . . ? C41 C40 C43 108.8(6) . . ? C33 C40 C43 110.5(6) . . ? C41 C40 C42 107.8(6) . . ? C33 C40 C42 108.1(6) . . ? C43 C40 C42 108.8(7) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C7S C1S C2S 114.2 . . ? C7S C1S C6S 125.8 . . ? C2S C1S C6S 120 . . ? C3S C2S C1S 120 . . ? C3S C2S H2S 120 . . ? C1S C2S H2S 120 . . ? C4S C3S C2S 120 . . ? C4S C3S H3S 120 . . ? C2S C3S H3S 120 . . ? C3S C4S C5S 120 . . ? C3S C4S H4S 120 . . ? C5S C4S H4S 120 . . ? C6S C5S C4S 120 . . ? C6S C5S H5S 120 . . ? C4S C5S H5S 120 . . ? C5S C6S C1S 120 . . ? C5S C6S H6S 120 . . ? C1S C6S H6S 120 . . ? C1S C7S H7S1 109.5 . . ? C1S C7S H7S2 109.5 . . ? H7S1 C7S H7S2 109.5 . . ? C1S C7S H7S3 109.5 . . ? H7S1 C7S H7S3 109.5 . . ? H7S2 C7S H7S3 109.5 . . ? C1S C7S H7S4 109.5 . . ? H7S1 C7S H7S4 141.1 . . ? H7S2 C7S H7S4 56.3 . . ? H7S3 C7S H7S4 56.3 . . ? C1S C7S H7S5 109.5 . . ? H7S1 C7S H7S5 56.3 . . ? H7S2 C7S H7S5 141.1 . . ? H7S3 C7S H7S5 56.3 . . ? H7S4 C7S H7S5 109.5 . . ? C1S C7S H7S6 109.5 . . ? H7S1 C7S H7S6 56.3 . . ? H7S2 C7S H7S6 56.3 . . ? H7S3 C7S H7S6 141.1 . . ? H7S4 C7S H7S6 109.5 . . ? H7S5 C7S H7S6 109.5 . . ? #===END #===END data_(3)-may907 _database_code_depnum_ccdc_archive 'CCDC 648823' _audit_creation_date 2007-05-09T10:06:29-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.2 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C44 H64 N2 O Pb' _chemical_formula_sum 'C44 H64 N2 O Pb' _chemical_formula_weight 844.16 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.3312(2) _cell_length_b 12.5867(2) _cell_length_c 15.1185(3) _cell_angle_alpha 105.315(1) _cell_angle_beta 100.911(1) _cell_angle_gamma 108.965(1) _cell_volume 2040.66(6) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 13435 _cell_measurement_theta_min 3.395 _cell_measurement_theta_max 26.022 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.15 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.374 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.167 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [c.f. r.h. blessing, acta cryst. (1995), a51, 33-38] ; _exptl_absorpt_correction_T_min 0.4475 _exptl_absorpt_correction_T_max 0.5256 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_source 'Enraf Nonius FR590' _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_detector 'CCD plate' _diffrn_orient_matrix_type 'by Nonius Collect from scalepack cell' _diffrn_orient_matrix_ub_11 0.83955E-1 _diffrn_orient_matrix_ub_12 0.105353E-1 _diffrn_orient_matrix_ub_13 0.305383E-1 _diffrn_orient_matrix_ub_21 0.75696E-2 _diffrn_orient_matrix_ub_22 -0.347024E-1 _diffrn_orient_matrix_ub_23 -0.650117E-1 _diffrn_orient_matrix_ub_31 0.313567E-1 _diffrn_orient_matrix_ub_32 0.82048E-1 _diffrn_orient_matrix_ub_33 -0.38403E-2 _diffrn_measurement_device '95mm CCD camera on \k-goniostat' _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method 'CCD rotation images, thick slices' _diffrn_reflns_av_R_equivalents 0.0345 _diffrn_reflns_av_unetI/netI 0.035 _diffrn_reflns_number 24004 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.43 _diffrn_reflns_theta_max 26.05 _diffrn_reflns_theta_full 26.05 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 8032 _reflns_number_gt 7468 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Collect (Nonius BV, 1997-2000)' _computing_cell_refinement 'HKL Scalepack (Otwinowski & Minor 1997)' _computing_data_reduction 'HKL Denzo and Scalepack (Otwinowski & Minor 1997)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1997)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material 'WinGX publication routines (Farrugia, 1999)' #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _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. ; _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^)+(0.0197P)^2^+1.6891P] 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_number_reflns 8032 _refine_ls_number_parameters 450 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0272 _refine_ls_R_factor_gt 0.0234 _refine_ls_wR_factor_ref 0.0513 _refine_ls_wR_factor_gt 0.05 _refine_ls_goodness_of_fit_ref 1.046 _refine_ls_restrained_S_all 1.046 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.171 _refine_diff_density_min -1.099 _refine_diff_density_rms 0.087 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# 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 0 '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 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _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 Pb Pb 0.705466(9) 0.526422(9) 0.688352(7) 0.01756(4) Uani 1 1 d . . . O O 0.65312(17) 0.34522(16) 0.69791(13) 0.0205(4) Uani 1 1 d . . . N1 N 0.8994(2) 0.5651(2) 0.77218(16) 0.0192(5) Uani 1 1 d . . . N2 N 0.7068(2) 0.64217(19) 0.83494(15) 0.0188(5) Uani 1 1 d . . . C1 C 0.9482(3) 0.6138(2) 0.86672(19) 0.0206(6) Uani 1 1 d . . . C2 C 0.8859(3) 0.6408(3) 0.9325(2) 0.0235(6) Uani 1 1 d . . . H2 H 0.9222 0.6474 0.9961 0.028 Uiso 1 1 calc R . . C3 C 0.7796(3) 0.6593(2) 0.91958(19) 0.0215(6) Uani 1 1 d . . . C4 C 1.0815(3) 0.6475(3) 0.9106(2) 0.0313(7) Uani 1 1 d . . . H4A H 1.1089 0.5959 0.8677 0.047 Uiso 1 1 calc R . . H4B H 1.0951 0.637 0.9731 0.047 Uiso 1 1 calc R . . H4C H 1.1264 0.7315 0.9192 0.047 Uiso 1 1 calc R . . C5 C 0.7473(3) 0.7053(3) 1.0105(2) 0.0325(7) Uani 1 1 d . . . H5A H 0.7684 0.7918 1.028 0.049 Uiso 1 1 calc R . . H5B H 0.792 0.6897 1.0631 0.049 Uiso 1 1 calc R . . H5C H 0.6608 0.664 0.999 0.049 Uiso 1 1 calc R . . C6 C 0.9749(2) 0.5514(3) 0.71164(19) 0.0225(6) Uani 1 1 d . . . C7 C 1.0300(3) 0.6468(3) 0.6814(2) 0.0274(7) Uani 1 1 d . . . C8 C 1.1019(3) 0.6315(3) 0.6229(2) 0.0367(8) Uani 1 1 d . . . H8 H 1.1395 0.6947 0.6016 0.044 Uiso 1 1 calc R . . C9 C 1.1199(3) 0.5276(3) 0.5951(2) 0.0392(8) Uani 1 1 d . . . H9 H 1.1709 0.5199 0.556 0.047 Uiso 1 1 calc R . . C10 C 1.0640(3) 0.4335(3) 0.6237(2) 0.0341(8) Uani 1 1 d . . . H10 H 1.0768 0.3616 0.6034 0.041 Uiso 1 1 calc R . . C11 C 0.9896(3) 0.4421(3) 0.6815(2) 0.0267(7) Uani 1 1 d . . . C12 C 1.0125(3) 0.7638(3) 0.7090(2) 0.0347(8) Uani 1 1 d . . . H12 H 0.9642 0.7617 0.7552 0.042 Uiso 1 1 calc R . . C13 C 0.9420(3) 0.7769(3) 0.6202(3) 0.0407(8) Uani 1 1 d . . . H13A H 0.9858 0.7748 0.5724 0.061 Uiso 1 1 calc R . . H13B H 0.9328 0.8534 0.639 0.061 Uiso 1 1 calc R . . H13C H 0.8625 0.7108 0.5925 0.061 Uiso 1 1 calc R . . C14 C 1.1332(4) 0.8722(3) 0.7590(3) 0.0517(10) Uani 1 1 d . . . H14A H 1.1781 0.8614 0.8144 0.078 Uiso 1 1 calc R . . H14B H 1.1186 0.9454 0.7809 0.078 Uiso 1 1 calc R . . H14C H 1.1801 0.8791 0.7136 0.078 Uiso 1 1 calc R . . C15 C 0.9251(3) 0.3359(3) 0.7094(2) 0.0306(7) Uani 1 1 d . . . H15 H 0.8437 0.3351 0.7089 0.037 Uiso 1 1 calc R . . C16 C 0.9874(3) 0.3445(3) 0.8101(3) 0.0444(9) Uani 1 1 d . . . H16A H 1.0714 0.3562 0.8159 0.067 Uiso 1 1 calc R . . H16B H 0.9461 0.2702 0.8208 0.067 Uiso 1 1 calc R . . H16C H 0.9848 0.4125 0.8581 0.067 Uiso 1 1 calc R . . C17 C 0.9061(4) 0.2148(3) 0.6384(3) 0.0504(10) Uani 1 1 d . . . H17A H 0.8727 0.2102 0.5726 0.076 Uiso 1 1 calc R . . H17B H 0.8502 0.1501 0.652 0.076 Uiso 1 1 calc R . . H17C H 0.9833 0.2066 0.645 0.076 Uiso 1 1 calc R . . C18 C 0.6239(3) 0.7004(2) 0.83332(19) 0.0207(6) Uani 1 1 d . . . C19 C 0.6691(3) 0.8265(3) 0.8584(2) 0.0250(6) Uani 1 1 d . . . C20 C 0.5880(3) 0.8817(3) 0.8563(2) 0.0309(7) Uani 1 1 d . . . H20 H 0.6175 0.9665 0.8746 0.037 Uiso 1 1 calc R . . C21 C 0.4656(3) 0.8158(3) 0.8284(2) 0.0338(8) Uani 1 1 d . . . H21 H 0.4117 0.8552 0.8275 0.041 Uiso 1 1 calc R . . C22 C 0.4219(3) 0.6926(3) 0.8017(2) 0.0301(7) Uani 1 1 d . . . H22 H 0.3375 0.6477 0.782 0.036 Uiso 1 1 calc R . . C23 C 0.4991(3) 0.6327(2) 0.8031(2) 0.0224(6) Uani 1 1 d . . . C24 C 0.8025(3) 0.9032(3) 0.8829(2) 0.0319(7) Uani 1 1 d . . . H24 H 0.8488 0.8534 0.8943 0.038 Uiso 1 1 calc R . . C25 C 0.8272(3) 0.9409(4) 0.7984(3) 0.0542(10) Uani 1 1 d . . . H25A H 0.8013 0.8694 0.7411 0.081 Uiso 1 1 calc R . . H25B H 0.9135 0.9878 0.8138 0.081 Uiso 1 1 calc R . . H25C H 0.7826 0.9899 0.7861 0.081 Uiso 1 1 calc R . . C26 C 0.8469(4) 1.0140(3) 0.9732(3) 0.0605(12) Uani 1 1 d . . . H26A H 0.8032 1.0646 0.9631 0.091 Uiso 1 1 calc R . . H26B H 0.9331 1.0595 0.9868 0.091 Uiso 1 1 calc R . . H26C H 0.8328 0.9893 1.0277 0.091 Uiso 1 1 calc R . . C27 C 0.4453(3) 0.4970(3) 0.7716(2) 0.0255(6) Uani 1 1 d . . . H27 H 0.5126 0.4698 0.7833 0.031 Uiso 1 1 calc R . . C28 C 0.3617(3) 0.4531(3) 0.8293(3) 0.0443(9) Uani 1 1 d . . . H28A H 0.4064 0.4883 0.898 0.066 Uiso 1 1 calc R . . H28B H 0.3312 0.3655 0.8088 0.066 Uiso 1 1 calc R . . H28C H 0.294 0.4776 0.8179 0.066 Uiso 1 1 calc R . . C29 C 0.3774(3) 0.4412(3) 0.6640(2) 0.0335(7) Uani 1 1 d . . . H29A H 0.3124 0.4686 0.6507 0.05 Uiso 1 1 calc R . . H29B H 0.3435 0.3535 0.6449 0.05 Uiso 1 1 calc R . . H29C H 0.433 0.4655 0.6277 0.05 Uiso 1 1 calc R . . C30 C 0.5402(2) 0.2595(2) 0.66555(19) 0.0175(6) Uani 1 1 d . . . C31 C 0.4891(3) 0.2174(2) 0.73347(19) 0.0197(6) Uani 1 1 d . . . C32 C 0.3660(3) 0.1494(2) 0.7043(2) 0.0260(7) Uani 1 1 d . . . H32 H 0.3306 0.1243 0.7498 0.031 Uiso 1 1 calc R . . C33 C 0.2924(3) 0.1166(3) 0.6113(2) 0.0281(7) Uani 1 1 d . . . C34 C 0.3486(3) 0.1416(3) 0.5444(2) 0.0262(7) Uani 1 1 d . . . H34 H 0.3006 0.1121 0.4792 0.031 Uiso 1 1 calc R . . C35 C 0.4720(3) 0.2079(2) 0.56650(19) 0.0213(6) Uani 1 1 d . . . C36 C 0.5688(3) 0.2377(2) 0.83343(19) 0.0243(6) Uani 1 1 d . . . C37 C 0.6690(3) 0.1941(3) 0.8200(2) 0.0296(7) Uani 1 1 d . . . H37A H 0.6334 0.1092 0.7791 0.044 Uiso 1 1 calc R . . H37B H 0.7187 0.2041 0.8828 0.044 Uiso 1 1 calc R . . H37C H 0.719 0.2412 0.7894 0.044 Uiso 1 1 calc R . . C38 C 0.6266(4) 0.3698(3) 0.8997(2) 0.0394(9) Uani 1 1 d . . . H38A H 0.6791 0.4175 0.8709 0.059 Uiso 1 1 calc R . . H38B H 0.6742 0.3771 0.9624 0.059 Uiso 1 1 calc R . . H38C H 0.5635 0.3994 0.9081 0.059 Uiso 1 1 calc R . . C39 C 0.4973(3) 0.1656(3) 0.8859(2) 0.0399(8) Uani 1 1 d . . . H39A H 0.4367 0.1959 0.9007 0.06 Uiso 1 1 calc R . . H39B H 0.5522 0.1739 0.9458 0.06 Uiso 1 1 calc R . . H39C H 0.4575 0.0808 0.8447 0.06 Uiso 1 1 calc R . . C40 C 0.1572(3) 0.0549(3) 0.5847(3) 0.0448(9) Uani 1 1 d . . . H40A H 0.1197 0.0722 0.5301 0.067 Uiso 1 1 calc R . . H40B H 0.1304 0.0843 0.6398 0.067 Uiso 1 1 calc R . . H40C H 0.1339 -0.0319 0.5671 0.067 Uiso 1 1 calc R . . C41 C 0.5202(3) 0.2161(3) 0.4804(2) 0.0274(7) Uani 1 1 d . . . C42 C 0.6556(3) 0.2498(3) 0.5029(2) 0.0444(9) Uani 1 1 d . . . H42A H 0.6984 0.3356 0.5407 0.067 Uiso 1 1 calc R . . H42B H 0.6762 0.2323 0.4427 0.067 Uiso 1 1 calc R . . H42C H 0.6792 0.2033 0.5398 0.067 Uiso 1 1 calc R . . C43 C 0.4858(4) 0.3030(3) 0.4387(2) 0.0430(9) Uani 1 1 d . . . H43A H 0.3985 0.2792 0.4223 0.065 Uiso 1 1 calc R . . H43B H 0.5108 0.3012 0.3807 0.065 Uiso 1 1 calc R . . H43C H 0.5261 0.3844 0.4864 0.065 Uiso 1 1 calc R . . C44 C 0.4651(3) 0.0910(3) 0.4008(2) 0.0390(8) Uani 1 1 d . . . H44A H 0.4861 0.034 0.4263 0.059 Uiso 1 1 calc R . . H44B H 0.4967 0.0956 0.3465 0.059 Uiso 1 1 calc R . . H44C H 0.3774 0.064 0.379 0.059 Uiso 1 1 calc R . . 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 Pb 0.01768(6) 0.01888(6) 0.01479(6) 0.00691(4) 0.00359(4) 0.00552(4) O 0.0199(10) 0.0172(10) 0.0208(10) 0.0078(8) 0.0038(8) 0.0034(8) N1 0.0152(12) 0.0225(12) 0.0186(12) 0.0078(10) 0.0044(9) 0.0060(10) N2 0.0226(13) 0.0174(12) 0.0174(11) 0.0072(9) 0.0058(10) 0.0083(10) C1 0.0220(15) 0.0191(14) 0.0192(14) 0.0081(11) 0.0036(12) 0.0066(12) C2 0.0296(17) 0.0257(15) 0.0168(14) 0.0097(12) 0.0040(12) 0.0128(13) C3 0.0303(16) 0.0188(14) 0.0177(14) 0.0082(11) 0.0078(12) 0.0107(13) C4 0.0198(16) 0.0397(19) 0.0240(16) 0.0051(14) -0.0017(13) 0.0086(14) C5 0.047(2) 0.0443(19) 0.0195(15) 0.0150(14) 0.0147(14) 0.0291(17) C6 0.0143(14) 0.0334(17) 0.0174(14) 0.0071(12) 0.0035(11) 0.0086(13) C7 0.0188(15) 0.0349(17) 0.0250(15) 0.0119(13) 0.0058(12) 0.0059(13) C8 0.0265(18) 0.055(2) 0.0339(18) 0.0216(16) 0.0150(15) 0.0146(16) C9 0.0284(18) 0.070(3) 0.0299(18) 0.0218(17) 0.0141(15) 0.0263(18) C10 0.0276(17) 0.052(2) 0.0271(17) 0.0115(15) 0.0062(14) 0.0243(16) C11 0.0202(15) 0.0392(18) 0.0195(14) 0.0073(13) 0.0026(12) 0.0145(14) C12 0.0348(19) 0.0347(18) 0.0356(18) 0.0181(15) 0.0167(15) 0.0071(15) C13 0.041(2) 0.038(2) 0.047(2) 0.0219(17) 0.0182(17) 0.0122(17) C14 0.049(2) 0.045(2) 0.049(2) 0.0179(18) 0.0117(19) 0.0030(19) C15 0.0298(17) 0.0340(18) 0.0304(17) 0.0094(14) 0.0078(14) 0.0177(15) C16 0.042(2) 0.047(2) 0.045(2) 0.0248(18) 0.0072(17) 0.0151(18) C17 0.056(3) 0.040(2) 0.059(2) 0.0105(18) 0.020(2) 0.0278(19) C18 0.0253(16) 0.0228(15) 0.0171(14) 0.0090(11) 0.0064(12) 0.0117(13) C19 0.0314(17) 0.0222(15) 0.0209(14) 0.0085(12) 0.0047(13) 0.0112(13) C20 0.040(2) 0.0216(16) 0.0339(17) 0.0101(13) 0.0099(15) 0.0166(15) C21 0.039(2) 0.0347(18) 0.0413(19) 0.0176(15) 0.0163(16) 0.0256(16) C22 0.0277(17) 0.0331(18) 0.0369(18) 0.0164(14) 0.0138(14) 0.0155(14) C23 0.0269(16) 0.0229(15) 0.0243(15) 0.0125(12) 0.0119(13) 0.0128(13) C24 0.0295(18) 0.0178(15) 0.0389(18) 0.0067(13) -0.0008(14) 0.0067(13) C25 0.034(2) 0.059(3) 0.064(3) 0.026(2) 0.0154(19) 0.0078(19) C26 0.055(3) 0.032(2) 0.058(3) -0.0055(18) -0.012(2) 0.0063(19) C27 0.0264(16) 0.0244(15) 0.0339(17) 0.0153(13) 0.0154(14) 0.0125(13) C28 0.050(2) 0.036(2) 0.062(2) 0.0268(18) 0.037(2) 0.0176(18) C29 0.0250(17) 0.0269(17) 0.0439(19) 0.0103(14) 0.0052(15) 0.0092(14) C30 0.0183(14) 0.0128(13) 0.0206(14) 0.0064(11) 0.0050(11) 0.0053(11) C31 0.0258(16) 0.0142(13) 0.0213(14) 0.0077(11) 0.0082(12) 0.0087(12) C32 0.0300(17) 0.0212(15) 0.0284(16) 0.0130(13) 0.0128(14) 0.0065(13) C33 0.0215(16) 0.0192(15) 0.0361(17) 0.0081(13) 0.0054(13) 0.0020(13) C34 0.0222(16) 0.0232(15) 0.0231(15) 0.0059(12) -0.0014(12) 0.0029(13) C35 0.0257(16) 0.0180(14) 0.0200(14) 0.0092(11) 0.0056(12) 0.0069(12) C36 0.0367(18) 0.0219(15) 0.0178(14) 0.0114(12) 0.0087(13) 0.0123(13) C37 0.0334(18) 0.0325(17) 0.0235(15) 0.0133(13) 0.0034(13) 0.0142(15) C38 0.069(3) 0.0310(18) 0.0181(15) 0.0064(13) 0.0035(16) 0.0273(18) C39 0.050(2) 0.051(2) 0.0324(18) 0.0271(17) 0.0192(17) 0.0221(18) C40 0.0245(18) 0.042(2) 0.054(2) 0.0145(18) 0.0071(16) 0.0014(16) C41 0.0330(18) 0.0251(16) 0.0167(14) 0.0063(12) 0.0052(13) 0.0046(14) C42 0.041(2) 0.055(2) 0.0280(18) 0.0054(16) 0.0185(16) 0.0111(18) C43 0.067(3) 0.0342(19) 0.0247(17) 0.0154(15) 0.0116(17) 0.0131(18) C44 0.055(2) 0.0301(18) 0.0239(16) 0.0054(14) 0.0131(16) 0.0089(17) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _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 Pb O 2.2118(18) . ? Pb N2 2.302(2) . ? Pb N1 2.309(2) . ? O C30 1.352(3) . ? N1 C1 1.324(3) . ? N1 C6 1.441(3) . ? N2 C3 1.336(4) . ? N2 C18 1.439(4) . ? C1 C2 1.406(4) . ? C1 C4 1.518(4) . ? C2 C3 1.392(4) . ? C2 H2 0.95 . ? C3 C5 1.523(4) . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 C7 1.412(4) . ? C6 C11 1.413(4) . ? C7 C8 1.386(4) . ? C7 C12 1.518(5) . ? C8 C9 1.368(5) . ? C8 H8 0.95 . ? C9 C10 1.385(5) . ? C9 H9 0.95 . ? C10 C11 1.391(4) . ? C10 H10 0.95 . ? C11 C15 1.526(4) . ? C12 C13 1.534(5) . ? C12 C14 1.536(5) . ? C12 H12 1 . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 C16 1.529(4) . ? C15 C17 1.529(4) . ? C15 H15 1 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? C17 H17A 0.98 . ? C17 H17B 0.98 . ? C17 H17C 0.98 . ? C18 C23 1.406(4) . ? C18 C19 1.413(4) . ? C19 C20 1.392(4) . ? C19 C24 1.524(4) . ? C20 C21 1.380(5) . ? C20 H20 0.95 . ? C21 C22 1.379(4) . ? C21 H21 0.95 . ? C22 C23 1.394(4) . ? C22 H22 0.95 . ? C23 C27 1.516(4) . ? C24 C25 1.524(5) . ? C24 C26 1.524(5) . ? C24 H24 1 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 C29 1.529(4) . ? C27 C28 1.533(4) . ? C27 H27 1 . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C30 C35 1.423(4) . ? C30 C31 1.431(4) . ? C31 C32 1.391(4) . ? C31 C36 1.544(4) . ? C32 C33 1.392(4) . ? C32 H32 0.95 . ? C33 C34 1.376(4) . ? C33 C40 1.511(4) . ? C34 C35 1.400(4) . ? C34 H34 0.95 . ? C35 C41 1.543(4) . ? C36 C37 1.531(4) . ? C36 C39 1.535(4) . ? C36 C38 1.535(4) . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C38 H38A 0.98 . ? C38 H38B 0.98 . ? C38 H38C 0.98 . ? C39 H39A 0.98 . ? C39 H39B 0.98 . ? C39 H39C 0.98 . ? C40 H40A 0.98 . ? C40 H40B 0.98 . ? C40 H40C 0.98 . ? C41 C42 1.528(5) . ? C41 C43 1.529(4) . ? C41 C44 1.544(4) . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? C43 H43A 0.98 . ? C43 H43B 0.98 . ? C43 H43C 0.98 . ? C44 H44A 0.98 . ? C44 H44B 0.98 . ? C44 H44C 0.98 . ? 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 O Pb N2 103.00(7) . . ? O Pb N1 87.32(7) . . ? N2 Pb N1 83.06(8) . . ? C30 O Pb 125.91(16) . . ? C1 N1 C6 119.5(2) . . ? C1 N1 Pb 126.04(18) . . ? C6 N1 Pb 113.65(16) . . ? C3 N2 C18 118.9(2) . . ? C3 N2 Pb 124.45(18) . . ? C18 N2 Pb 116.67(16) . . ? N1 C1 C2 124.7(3) . . ? N1 C1 C4 119.8(2) . . ? C2 C1 C4 115.5(2) . . ? C3 C2 C1 130.5(3) . . ? C3 C2 H2 114.8 . . ? C1 C2 H2 114.8 . . ? N2 C3 C2 125.2(3) . . ? N2 C3 C5 118.6(3) . . ? C2 C3 C5 116.2(3) . . ? C1 C4 H4A 109.5 . . ? C1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? C1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? C3 C5 H5A 109.5 . . ? C3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? C3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? C7 C6 C11 121.2(3) . . ? C7 C6 N1 119.1(3) . . ? C11 C6 N1 119.7(3) . . ? C8 C7 C6 118.1(3) . . ? C8 C7 C12 119.1(3) . . ? C6 C7 C12 122.8(3) . . ? C9 C8 C7 121.6(3) . . ? C9 C8 H8 119.2 . . ? C7 C8 H8 119.2 . . ? C8 C9 C10 120.1(3) . . ? C8 C9 H9 119.9 . . ? C10 C9 H9 119.9 . . ? C9 C10 C11 121.4(3) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C10 C11 C6 117.6(3) . . ? C10 C11 C15 120.7(3) . . ? C6 C11 C15 121.8(3) . . ? C7 C12 C13 110.5(3) . . ? C7 C12 C14 111.5(3) . . ? C13 C12 C14 110.5(3) . . ? C7 C12 H12 108.1 . . ? C13 C12 H12 108.1 . . ? C14 C12 H12 108.1 . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C11 C15 C16 113.8(3) . . ? C11 C15 C17 113.3(3) . . ? C16 C15 C17 108.0(3) . . ? C11 C15 H15 107.1 . . ? C16 C15 H15 107.1 . . ? C17 C15 H15 107.1 . . ? C15 C16 H16A 109.5 . . ? C15 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C15 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C15 C17 H17A 109.5 . . ? C15 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C15 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C23 C18 C19 120.2(3) . . ? C23 C18 N2 120.6(2) . . ? C19 C18 N2 119.1(3) . . ? C20 C19 C18 118.6(3) . . ? C20 C19 C24 118.8(3) . . ? C18 C19 C24 122.5(3) . . ? C21 C20 C19 121.4(3) . . ? C21 C20 H20 119.3 . . ? C19 C20 H20 119.3 . . ? C22 C21 C20 119.8(3) . . ? C22 C21 H21 120.1 . . ? C20 C21 H21 120.1 . . ? C21 C22 C23 121.3(3) . . ? C21 C22 H22 119.4 . . ? C23 C22 H22 119.4 . . ? C22 C23 C18 118.7(3) . . ? C22 C23 C27 118.7(3) . . ? C18 C23 C27 122.6(3) . . ? C25 C24 C19 109.9(3) . . ? C25 C24 C26 109.7(3) . . ? C19 C24 C26 112.5(3) . . ? C25 C24 H24 108.2 . . ? C19 C24 H24 108.2 . . ? C26 C24 H24 108.2 . . ? C24 C25 H25A 109.5 . . ? C24 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C24 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C24 C26 H26A 109.5 . . ? C24 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C24 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C23 C27 C29 110.5(2) . . ? C23 C27 C28 111.8(2) . . ? C29 C27 C28 110.1(3) . . ? C23 C27 H27 108.1 . . ? C29 C27 H27 108.1 . . ? C28 C27 H27 108.1 . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? O C30 C35 122.4(2) . . ? O C30 C31 118.5(2) . . ? C35 C30 C31 119.1(2) . . ? C32 C31 C30 118.0(3) . . ? C32 C31 C36 120.5(2) . . ? C30 C31 C36 121.4(2) . . ? C31 C32 C33 122.8(3) . . ? C31 C32 H32 118.6 . . ? C33 C32 H32 118.6 . . ? C34 C33 C32 116.9(3) . . ? C34 C33 C40 121.5(3) . . ? C32 C33 C40 121.5(3) . . ? C33 C34 C35 124.0(3) . . ? C33 C34 H34 118 . . ? C35 C34 H34 118 . . ? C34 C35 C30 116.9(2) . . ? C34 C35 C41 116.3(2) . . ? C30 C35 C41 126.8(3) . . ? C37 C36 C39 107.3(2) . . ? C37 C36 C38 108.6(3) . . ? C39 C36 C38 107.4(3) . . ? C37 C36 C31 108.6(2) . . ? C39 C36 C31 111.7(3) . . ? C38 C36 C31 113.1(2) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C33 C40 H40A 109.5 . . ? C33 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C33 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? C42 C41 C43 109.9(3) . . ? C42 C41 C35 114.2(2) . . ? C43 C41 C35 111.0(3) . . ? C42 C41 C44 103.8(3) . . ? C43 C41 C44 108.3(3) . . ? C35 C41 C44 109.3(2) . . ? C41 C42 H42A 109.5 . . ? C41 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C41 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C41 C43 H43A 109.5 . . ? C41 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C41 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? C41 C44 H44A 109.5 . . ? C41 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? C41 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ?