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 'Jennifer Robin 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 ; Synthesis and theoretical studies on rare three-coordinate lead complexes ; _publ_requested_category FM loop_ _publ_author_name 'J. Fulton' 'Matthew Chen' 'Peter B. Hitchcock' 'Nick C. Johnstone' 'M. Lappert' ; A.V.Protchenko ; data_(2)-sep603 _database_code_depnum_ccdc_archive 'CCDC 638198' _audit_creation_date 2003-09-09T11:32:00-00:00 _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_name_common (PbCl(C6H3iPr2NC(Me)CHC(Me)NC6H3iPr2)) _chemical_formula_moiety 'C29 H41 Cl1 N2 Pb1' _chemical_formula_sum 'C29 H41 Cl1 N2 Pb1' _chemical_formula_weight 660.28 _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 10.4070(1) _cell_length_b 12.0343(1) _cell_length_c 12.4700(2) _cell_angle_alpha 89.464(1) _cell_angle_beta 72.864(1) _cell_angle_gamma 70.868(1) _cell_volume 1403.40(3) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 20697 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 27.485 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.2 _exptl_crystal_density_diffrn 1.563 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 6.125 _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 0.2365 _exptl_absorpt_correction_T_max 0.3722 #----------------------------------------------------------------------------# # 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 0.583376E-1 _diffrn_orient_matrix_ub_12 -0.181112E-1 _diffrn_orient_matrix_ub_13 -0.813673E-1 _diffrn_orient_matrix_ub_21 0.896111E-1 _diffrn_orient_matrix_ub_22 -0.241562E-1 _diffrn_orient_matrix_ub_23 0.219229E-1 _diffrn_orient_matrix_ub_31 -0.919E-4 _diffrn_orient_matrix_ub_32 -0.830495E-1 _diffrn_orient_matrix_ub_33 0.27016E-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 0.0463 _diffrn_reflns_av_unetI/netI 0.029 _diffrn_reflns_number 27534 _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 -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 3.72 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 6372 _reflns_number_gt 6022 _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^)+(0.0136P)^2^+1.2568P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 6372 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0223 _refine_ls_R_factor_gt 0.0197 _refine_ls_wR_factor_ref 0.0453 _refine_ls_wR_factor_gt 0.0443 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.793 _refine_diff_density_min -1.213 _refine_diff_density_rms 0.082 #----------------------------------------------------------------------------# # 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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 0.424675(9) 0.668966(7) 0.616637(7) 0.02261(4) Uani 1 1 d . . . Cl Cl 0.59262(7) 0.78497(7) 0.61493(6) 0.03873(16) Uani 1 1 d . . . N1 N 0.3355(2) 0.78393(17) 0.49008(17) 0.0206(4) Uani 1 1 d . . . N2 N 0.2345(2) 0.80442(17) 0.74474(17) 0.0210(4) Uani 1 1 d . . . C1 C 0.2533(3) 0.8962(2) 0.5114(2) 0.0228(5) Uani 1 1 d . . . C2 C 0.1917(3) 0.9577(2) 0.6197(2) 0.0248(5) Uani 1 1 d . . . H2 H 0.1556 1.0413 0.6205 0.03 Uiso 1 1 calc R . . C3 C 0.1751(2) 0.9162(2) 0.7257(2) 0.0212(5) Uani 1 1 d . . . C4 C 0.2168(3) 0.9663(2) 0.4167(2) 0.0329(6) Uani 1 1 d . . . H4A H 0.2705 1.021 0.3992 0.049 Uiso 1 1 calc R . . H4B H 0.1141 1.0112 0.4398 0.049 Uiso 1 1 calc R . . H4C H 0.2421 0.9122 0.3497 0.049 Uiso 1 1 calc R . . C5 C 0.0789(3) 1.0062(2) 0.8254(2) 0.0302(6) Uani 1 1 d . . . H5A H 0.0267 0.9679 0.8837 0.045 Uiso 1 1 calc R . . H5B H 0.0106 1.0704 0.8007 0.045 Uiso 1 1 calc R . . H5C H 0.1371 1.0385 0.8562 0.045 Uiso 1 1 calc R . . C6 C 0.3818(3) 0.7184(2) 0.3819(2) 0.0208(5) Uani 1 1 d . . . C7 C 0.5088(3) 0.7165(2) 0.2999(2) 0.0249(5) Uani 1 1 d . . . C8 C 0.5592(3) 0.6379(3) 0.2033(2) 0.0315(6) Uani 1 1 d . . . H8 H 0.6459 0.6341 0.1477 0.038 Uiso 1 1 calc R . . C9 C 0.4865(3) 0.5652(2) 0.1861(2) 0.0302(6) Uani 1 1 d . . . H9 H 0.5243 0.511 0.1204 0.036 Uiso 1 1 calc R . . C10 C 0.3583(3) 0.5721(2) 0.2655(2) 0.0273(5) Uani 1 1 d . . . H10 H 0.3062 0.5248 0.2522 0.033 Uiso 1 1 calc R . . C11 C 0.3043(3) 0.6473(2) 0.3646(2) 0.0221(5) Uani 1 1 d . . . C12 C 0.5885(3) 0.7989(2) 0.3124(2) 0.0288(6) Uani 1 1 d . . . H12 H 0.5388 0.8454 0.3879 0.035 Uiso 1 1 calc R . . C13 C 0.5863(3) 0.8860(3) 0.2216(3) 0.0399(7) Uani 1 1 d . . . H13A H 0.6377 0.9384 0.2316 0.06 Uiso 1 1 calc R . . H13B H 0.4871 0.9333 0.2285 0.06 Uiso 1 1 calc R . . H13C H 0.6327 0.842 0.1467 0.06 Uiso 1 1 calc R . . C14 C 0.7428(3) 0.7308(3) 0.3065(3) 0.0405(7) Uani 1 1 d . . . H14A H 0.7904 0.7867 0.3154 0.061 Uiso 1 1 calc R . . H14B H 0.7932 0.6838 0.2334 0.061 Uiso 1 1 calc R . . H14C H 0.7441 0.6783 0.367 0.061 Uiso 1 1 calc R . . C15 C 0.1634(3) 0.6528(2) 0.4507(2) 0.0247(5) Uani 1 1 d . . . H15 H 0.1428 0.7121 0.5146 0.03 Uiso 1 1 calc R . . C16 C 0.0401(3) 0.6941(3) 0.4003(3) 0.0430(7) Uani 1 1 d . . . H16A H -0.0492 0.6974 0.4576 0.065 Uiso 1 1 calc R . . H16B H 0.0589 0.6385 0.336 0.065 Uiso 1 1 calc R . . H16C H 0.0314 0.7728 0.375 0.065 Uiso 1 1 calc R . . C17 C 0.1721(3) 0.5344(3) 0.4984(3) 0.0370(7) Uani 1 1 d . . . H17A H 0.0801 0.5413 0.5538 0.056 Uiso 1 1 calc R . . H17B H 0.2472 0.5117 0.5348 0.056 Uiso 1 1 calc R . . H17C H 0.1945 0.474 0.4371 0.056 Uiso 1 1 calc R . . C18 C 0.1934(3) 0.7633(2) 0.8540(2) 0.0228(5) Uani 1 1 d . . . C19 C 0.2617(3) 0.7718(2) 0.9339(2) 0.0242(5) Uani 1 1 d . . . C20 C 0.2246(3) 0.7237(2) 1.0359(2) 0.0314(6) Uani 1 1 d . . . H20 H 0.2701 0.7287 1.0906 0.038 Uiso 1 1 calc R . . C21 C 0.1235(3) 0.6690(3) 1.0589(2) 0.0370(7) Uani 1 1 d . . . H21 H 0.0995 0.637 1.1289 0.044 Uiso 1 1 calc R . . C22 C 0.0566(3) 0.6607(3) 0.9794(2) 0.0352(6) Uani 1 1 d . . . H22 H -0.0136 0.6234 0.9962 0.042 Uiso 1 1 calc R . . C23 C 0.0903(3) 0.7060(2) 0.8757(2) 0.0267(5) Uani 1 1 d . . . C24 C 0.3747(3) 0.8307(2) 0.9137(2) 0.0271(5) Uani 1 1 d . . . H24 H 0.3836 0.8644 0.8393 0.033 Uiso 1 1 calc R . . C25 C 0.3308(4) 0.9322(3) 1.0048(3) 0.0429(8) Uani 1 1 d . . . H25A H 0.4053 0.9684 0.9901 0.064 Uiso 1 1 calc R . . H25B H 0.3185 0.9015 1.0789 0.064 Uiso 1 1 calc R . . H25C H 0.2405 0.9916 1.0039 0.064 Uiso 1 1 calc R . . C26 C 0.5211(3) 0.7411(3) 0.9085(3) 0.0421(7) Uani 1 1 d . . . H26A H 0.5915 0.7814 0.8956 0.063 Uiso 1 1 calc R . . H26B H 0.551 0.6794 0.8466 0.063 Uiso 1 1 calc R . . H26C H 0.5142 0.7052 0.9799 0.063 Uiso 1 1 calc R . . C27 C 0.0184(3) 0.6940(2) 0.7882(2) 0.0297(6) Uani 1 1 d . . . H27 H 0.0924 0.6774 0.7124 0.036 Uiso 1 1 calc R . . C28 C -0.1031(4) 0.8074(3) 0.7864(3) 0.0476(8) Uani 1 1 d . . . H28A H -0.1455 0.7954 0.7289 0.071 Uiso 1 1 calc R . . H28B H -0.0652 0.8723 0.7687 0.071 Uiso 1 1 calc R . . H28C H -0.1763 0.8272 0.8604 0.071 Uiso 1 1 calc R . . C29 C -0.0416(4) 0.5923(3) 0.8041(3) 0.0426(7) Uani 1 1 d . . . H29A H -0.0854 0.5887 0.7452 0.064 Uiso 1 1 calc R . . H29B H -0.1138 0.6056 0.8783 0.064 Uiso 1 1 calc R . . H29C H 0.0361 0.5176 0.7989 0.064 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 0.02377(5) 0.02084(5) 0.02038(5) 0.00270(3) -0.00730(4) -0.00353(4) Cl 0.0310(3) 0.0552(4) 0.0331(4) -0.0004(3) -0.0076(3) -0.0205(3) N1 0.0223(10) 0.0221(10) 0.0192(10) 0.0046(8) -0.0075(8) -0.0090(8) N2 0.0218(10) 0.0225(10) 0.0196(10) 0.0031(8) -0.0054(8) -0.0097(8) C1 0.0227(12) 0.0221(12) 0.0262(13) 0.0069(10) -0.0082(10) -0.0108(10) C2 0.0263(12) 0.0184(11) 0.0291(13) 0.0039(10) -0.0082(11) -0.0072(10) C3 0.0173(11) 0.0212(11) 0.0254(12) -0.0015(9) -0.0047(10) -0.0084(9) C4 0.0396(15) 0.0268(13) 0.0304(14) 0.0110(11) -0.0159(13) -0.0045(12) C5 0.0287(13) 0.0263(13) 0.0295(14) -0.0021(11) -0.0029(11) -0.0068(11) C6 0.0229(12) 0.0207(11) 0.0185(11) 0.0051(9) -0.0084(10) -0.0054(9) C7 0.0256(12) 0.0283(13) 0.0215(12) 0.0070(10) -0.0076(10) -0.0100(10) C8 0.0296(14) 0.0379(15) 0.0231(13) 0.0031(11) -0.0038(11) -0.0102(12) C9 0.0388(15) 0.0286(13) 0.0205(13) -0.0001(10) -0.0085(11) -0.0083(12) C10 0.0354(14) 0.0253(12) 0.0249(13) 0.0045(10) -0.0130(11) -0.0117(11) C11 0.0233(12) 0.0209(11) 0.0236(12) 0.0053(10) -0.0103(10) -0.0067(10) C12 0.0269(13) 0.0328(14) 0.0265(13) 0.0043(11) -0.0054(11) -0.0126(11) C13 0.0411(17) 0.0411(16) 0.0441(18) 0.0186(14) -0.0143(14) -0.0217(14) C14 0.0320(15) 0.0505(18) 0.0427(18) 0.0101(15) -0.0132(14) -0.0176(14) C15 0.0243(12) 0.0255(12) 0.0259(13) 0.0001(10) -0.0086(10) -0.0098(10) C16 0.0287(15) 0.0470(18) 0.0511(19) 0.0069(15) -0.0164(14) -0.0063(13) C17 0.0352(15) 0.0356(15) 0.0390(16) 0.0086(13) -0.0066(13) -0.0149(13) C18 0.0252(12) 0.0200(11) 0.0206(12) 0.0008(9) -0.0036(10) -0.0074(10) C19 0.0272(13) 0.0228(12) 0.0203(12) 0.0006(10) -0.0045(10) -0.0079(10) C20 0.0366(15) 0.0358(15) 0.0242(13) 0.0055(11) -0.0101(12) -0.0149(12) C21 0.0481(18) 0.0409(16) 0.0243(14) 0.0102(12) -0.0073(13) -0.0218(14) C22 0.0414(16) 0.0388(16) 0.0290(14) 0.0059(12) -0.0031(13) -0.0253(13) C23 0.0285(13) 0.0268(13) 0.0236(13) 0.0011(10) -0.0036(11) -0.0119(11) C24 0.0276(13) 0.0347(14) 0.0226(12) 0.0039(11) -0.0083(11) -0.0148(11) C25 0.0500(19) 0.0511(19) 0.0359(16) -0.0038(14) -0.0085(15) -0.0318(16) C26 0.0313(15) 0.0546(19) 0.0427(18) 0.0131(15) -0.0147(14) -0.0150(14) C27 0.0328(14) 0.0338(14) 0.0266(13) 0.0011(11) -0.0052(11) -0.0202(12) C28 0.0468(19) 0.0427(18) 0.069(2) 0.0102(16) -0.0317(18) -0.0233(15) C29 0.0496(18) 0.0413(17) 0.0457(18) 0.0023(14) -0.0134(15) -0.0282(15) #----------------------------------------------------------------------------# # 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 2.280(2) . ? Pb N1 2.290(2) . ? Pb Cl 2.5653(7) . ? N1 C1 1.320(3) . ? N1 C6 1.435(3) . ? N2 C3 1.335(3) . ? N2 C18 1.438(3) . ? C1 C2 1.407(4) . ? C1 C4 1.512(3) . ? C2 C3 1.392(4) . ? C3 C5 1.517(3) . ? C6 C7 1.407(3) . ? C6 C11 1.410(3) . ? C7 C8 1.394(4) . ? C7 C12 1.520(4) . ? C8 C9 1.385(4) . ? C9 C10 1.385(4) . ? C10 C11 1.392(4) . ? C11 C15 1.522(4) . ? C12 C14 1.525(4) . ? C12 C13 1.537(4) . ? C15 C17 1.524(4) . ? C15 C16 1.530(4) . ? C18 C19 1.406(3) . ? C18 C23 1.417(3) . ? C19 C20 1.395(4) . ? C19 C24 1.522(3) . ? C20 C21 1.377(4) . ? C21 C22 1.390(4) . ? C22 C23 1.391(4) . ? C23 C27 1.526(4) . ? C24 C25 1.531(4) . ? C24 C26 1.534(4) . ? C27 C28 1.532(4) . ? C27 C29 1.533(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Pb N1 82.77(7) . . ? N2 Pb Cl 93.27(5) . . ? N1 Pb Cl 91.13(5) . . ? C1 N1 C6 123.4(2) . . ? C1 N1 Pb 125.44(16) . . ? C6 N1 Pb 111.19(14) . . ? C3 N2 C18 121.8(2) . . ? C3 N2 Pb 123.92(16) . . ? C18 N2 Pb 113.87(14) . . ? N1 C1 C2 124.2(2) . . ? N1 C1 C4 120.1(2) . . ? C2 C1 C4 115.7(2) . . ? C3 C2 C1 130.6(2) . . ? N2 C3 C2 124.9(2) . . ? N2 C3 C5 118.9(2) . . ? C2 C3 C5 116.2(2) . . ? C7 C6 C11 121.0(2) . . ? C7 C6 N1 120.6(2) . . ? C11 C6 N1 118.1(2) . . ? C8 C7 C6 117.8(2) . . ? C8 C7 C12 120.0(2) . . ? C6 C7 C12 122.1(2) . . ? C9 C8 C7 122.0(3) . . ? C8 C9 C10 119.4(2) . . ? C9 C10 C11 121.1(2) . . ? C10 C11 C6 118.6(2) . . ? C10 C11 C15 120.0(2) . . ? C6 C11 C15 121.3(2) . . ? C7 C12 C14 111.8(2) . . ? C7 C12 C13 110.9(2) . . ? C14 C12 C13 109.5(2) . . ? C11 C15 C17 111.7(2) . . ? C11 C15 C16 111.2(2) . . ? C17 C15 C16 110.4(2) . . ? C19 C18 C23 121.0(2) . . ? C19 C18 N2 120.6(2) . . ? C23 C18 N2 118.3(2) . . ? C20 C19 C18 118.4(2) . . ? C20 C19 C24 118.7(2) . . ? C18 C19 C24 122.9(2) . . ? C21 C20 C19 121.3(3) . . ? C20 C21 C22 119.9(3) . . ? C21 C22 C23 121.3(3) . . ? C22 C23 C18 118.0(2) . . ? C22 C23 C27 120.8(2) . . ? C18 C23 C27 121.1(2) . . ? C19 C24 C25 111.1(2) . . ? C19 C24 C26 111.3(2) . . ? C25 C24 C26 110.2(2) . . ? C23 C27 C28 112.6(2) . . ? C23 C27 C29 113.3(2) . . ? C28 C27 C29 108.0(2) . . ? #===END data_(3)-jul1206 _database_code_depnum_ccdc_archive 'CCDC 638199' _audit_creation_date 2006-07-28T09:42:20-00:00 _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 'C29 H41 Br N2 Pb' _chemical_formula_sum 'C29 H41 Br N2 Pb' _chemical_formula_weight 704.74 _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 10.4137(2) _cell_length_b 12.0840(4) _cell_length_c 12.4677(4) _cell_angle_alpha 89.224(2) _cell_angle_beta 72.815(2) _cell_angle_gamma 70.638(2) _cell_volume 1407.89(7) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 18106 _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 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 692 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 7.429 _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 0.2382 _exptl_absorpt_correction_T_max 0.3280 #----------------------------------------------------------------------------# # 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 0.621679E-1 _diffrn_orient_matrix_ub_12 -0.739728E-1 _diffrn_orient_matrix_ub_13 0.212892E-1 _diffrn_orient_matrix_ub_21 -0.741305E-1 _diffrn_orient_matrix_ub_22 -0.370827E-1 _diffrn_orient_matrix_ub_23 0.00519 _diffrn_orient_matrix_ub_31 0.457059E-1 _diffrn_orient_matrix_ub_32 -0.302472E-1 _diffrn_orient_matrix_ub_33 -0.814292E-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 0.0428 _diffrn_reflns_av_unetI/netI 0.032 _diffrn_reflns_number 19313 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.44 _diffrn_reflns_theta_max 26.07 _diffrn_reflns_theta_full 26.07 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 5529 _reflns_number_gt 5215 _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 four small residual peaks (ca. 2 electrons) which make no chemical sense and are assumed to be spurious. 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^)+(0.0020P)^2^+12.8902P] 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 5529 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0401 _refine_ls_R_factor_gt 0.0372 _refine_ls_wR_factor_ref 0.0949 _refine_ls_wR_factor_gt 0.0939 _refine_ls_goodness_of_fit_ref 1.26 _refine_ls_restrained_S_all 1.26 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.395 _refine_diff_density_min -1.176 _refine_diff_density_rms 0.153 #----------------------------------------------------------------------------# # 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' Br Br -0.2901 2.4595 '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' 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 0.42533(3) 0.66864(2) 0.61588(2) 0.02502(9) Uani 1 1 d . . . Br Br 0.60253(8) 0.79139(8) 0.61222(7) 0.03854(19) Uani 1 1 d . . . N1 N 0.3352(6) 0.7819(5) 0.4883(5) 0.0206(11) Uani 1 1 d . . . N2 N 0.2348(6) 0.8041(5) 0.7437(5) 0.0222(11) Uani 1 1 d . . . C1 C 0.2521(7) 0.8941(6) 0.5089(6) 0.0247(14) Uani 1 1 d . . . C2 C 0.1923(7) 0.9558(6) 0.6170(6) 0.0260(14) Uani 1 1 d . . . H2 H 0.1572 1.0391 0.6172 0.031 Uiso 1 1 calc R . . C3 C 0.1761(7) 0.9152(6) 0.7234(6) 0.0227(13) Uani 1 1 d . . . C4 C 0.2151(8) 0.9619(7) 0.4123(6) 0.0319(16) Uani 1 1 d . . . H4A H 0.2551 1.0256 0.4017 0.048 Uiso 1 1 calc R . . H4B H 0.1109 0.9954 0.4298 0.048 Uiso 1 1 calc R . . H4C H 0.2555 0.9085 0.3429 0.048 Uiso 1 1 calc R . . C5 C 0.0795(8) 1.0056(6) 0.8226(6) 0.0301(16) Uani 1 1 d . . . H5A H 0.0145 0.9721 0.8749 0.045 Uiso 1 1 calc R . . H5B H 0.0236 1.076 0.7952 0.045 Uiso 1 1 calc R . . H5C H 0.1381 1.027 0.8617 0.045 Uiso 1 1 calc R . . C6 C 0.3811(7) 0.7166(6) 0.3800(5) 0.0218(13) Uani 1 1 d . . . C7 C 0.5075(7) 0.7133(6) 0.2977(6) 0.0263(14) Uani 1 1 d . . . C8 C 0.5622(9) 0.6332(6) 0.1987(7) 0.0332(17) Uani 1 1 d . . . H8 H 0.6495 0.6279 0.143 0.04 Uiso 1 1 calc R . . C9 C 0.4841(9) 0.5626(6) 0.1859(6) 0.0341(17) Uani 1 1 d . . . H9 H 0.5194 0.5084 0.1207 0.041 Uiso 1 1 calc R . . C10 C 0.3558(8) 0.5701(6) 0.2665(6) 0.0297(15) Uani 1 1 d . . . H10 H 0.304 0.5223 0.2547 0.036 Uiso 1 1 calc R . . C11 C 0.3020(7) 0.6469(6) 0.3648(6) 0.0247(14) Uani 1 1 d . . . C12 C 0.5885(8) 0.7954(7) 0.3078(6) 0.0325(16) Uani 1 1 d . . . H12 H 0.5403 0.8421 0.3831 0.039 Uiso 1 1 calc R . . C13 C 0.5859(10) 0.8809(8) 0.2172(7) 0.044(2) Uani 1 1 d . . . H13A H 0.6369 0.9333 0.2267 0.066 Uiso 1 1 calc R . . H13B H 0.4865 0.9278 0.2239 0.066 Uiso 1 1 calc R . . H13C H 0.6325 0.8367 0.1426 0.066 Uiso 1 1 calc R . . C14 C 0.7449(8) 0.7271(8) 0.2998(8) 0.043(2) Uani 1 1 d . . . H14A H 0.7922 0.7828 0.3086 0.065 Uiso 1 1 calc R . . H14B H 0.7945 0.6814 0.2261 0.065 Uiso 1 1 calc R . . H14C H 0.7479 0.6737 0.3595 0.065 Uiso 1 1 calc R . . C15 C 0.1618(7) 0.6534(6) 0.4501(6) 0.0268(15) Uani 1 1 d . . . H15 H 0.1418 0.7127 0.5134 0.032 Uiso 1 1 calc R . . C16 C 0.0361(8) 0.6980(8) 0.3978(7) 0.0398(19) Uani 1 1 d . . . H16A H -0.0537 0.7016 0.4545 0.06 Uiso 1 1 calc R . . H16B H 0.055 0.6436 0.3329 0.06 Uiso 1 1 calc R . . H16C H 0.0285 0.7767 0.3732 0.06 Uiso 1 1 calc R . . C17 C 0.1693(9) 0.5375(7) 0.4989(7) 0.0395(19) Uani 1 1 d . . . H17A H 0.0769 0.5454 0.5542 0.059 Uiso 1 1 calc R . . H17B H 0.2441 0.5151 0.5359 0.059 Uiso 1 1 calc R . . H17C H 0.1919 0.4768 0.4383 0.059 Uiso 1 1 calc R . . C18 C 0.1926(7) 0.7641(6) 0.8535(6) 0.0231(14) Uani 1 1 d . . . C19 C 0.2601(7) 0.7722(6) 0.9344(6) 0.0255(14) Uani 1 1 d . . . C20 C 0.2221(8) 0.7247(7) 1.0344(6) 0.0335(17) Uani 1 1 d . . . H20 H 0.2667 0.7301 1.0895 0.04 Uiso 1 1 calc R . . C21 C 0.1217(9) 0.6693(7) 1.0581(7) 0.0385(18) Uani 1 1 d . . . H21 H 0.0979 0.6373 1.1282 0.046 Uiso 1 1 calc R . . C22 C 0.0566(9) 0.6612(7) 0.9788(7) 0.0384(18) Uani 1 1 d . . . H22 H -0.0129 0.6234 0.9952 0.046 Uiso 1 1 calc R . . C23 C 0.0898(8) 0.7066(6) 0.8756(6) 0.0286(15) Uani 1 1 d . . . C24 C 0.3726(8) 0.8310(7) 0.9142(6) 0.0304(16) Uani 1 1 d . . . H24 H 0.3823 0.864 0.8394 0.037 Uiso 1 1 calc R . . C25 C 0.3270(10) 0.9331(8) 1.0051(7) 0.045(2) Uani 1 1 d . . . H25A H 0.4012 0.9693 0.9905 0.068 Uiso 1 1 calc R . . H25B H 0.314 0.903 1.0795 0.068 Uiso 1 1 calc R . . H25C H 0.2367 0.9921 1.0032 0.068 Uiso 1 1 calc R . . C26 C 0.5185(9) 0.7431(8) 0.9113(8) 0.045(2) Uani 1 1 d . . . H26A H 0.5881 0.7839 0.8984 0.068 Uiso 1 1 calc R . . H26B H 0.5502 0.6807 0.8502 0.068 Uiso 1 1 calc R . . H26C H 0.5108 0.7084 0.9834 0.068 Uiso 1 1 calc R . . C27 C 0.0166(8) 0.6961(6) 0.7877(6) 0.0303(16) Uani 1 1 d . . . H27 H 0.0905 0.6794 0.7118 0.036 Uiso 1 1 calc R . . C28 C -0.1030(10) 0.8094(7) 0.7861(9) 0.049(2) Uani 1 1 d . . . H28A H -0.1463 0.7984 0.7289 0.074 Uiso 1 1 calc R . . H28B H -0.064 0.8732 0.768 0.074 Uiso 1 1 calc R . . H28C H -0.176 0.8295 0.8603 0.074 Uiso 1 1 calc R . . C29 C -0.0434(10) 0.5946(8) 0.8042(8) 0.045(2) Uani 1 1 d . . . H29A H -0.0872 0.591 0.7454 0.067 Uiso 1 1 calc R . . H29B H -0.1157 0.6081 0.8784 0.067 Uiso 1 1 calc R . . H29C H 0.0344 0.5201 0.7994 0.067 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 0.02552(14) 0.02415(14) 0.02430(14) 0.00261(9) -0.00949(10) -0.00554(10) Br 0.0312(4) 0.0544(5) 0.0345(4) -0.0010(3) -0.0089(3) -0.0211(4) N1 0.022(3) 0.021(3) 0.023(3) 0.006(2) -0.011(2) -0.009(2) N2 0.022(3) 0.023(3) 0.021(3) 0.001(2) -0.004(2) -0.007(2) C1 0.022(3) 0.026(4) 0.030(4) 0.005(3) -0.010(3) -0.013(3) C2 0.024(3) 0.023(3) 0.031(4) 0.003(3) -0.009(3) -0.009(3) C3 0.020(3) 0.022(3) 0.028(4) 0.000(3) -0.008(3) -0.009(3) C4 0.033(4) 0.032(4) 0.029(4) 0.010(3) -0.009(3) -0.011(3) C5 0.025(4) 0.028(4) 0.033(4) 0.000(3) -0.006(3) -0.006(3) C6 0.026(3) 0.020(3) 0.023(3) 0.005(3) -0.012(3) -0.008(3) C7 0.024(3) 0.032(4) 0.025(4) 0.005(3) -0.009(3) -0.012(3) C8 0.043(4) 0.029(4) 0.036(4) 0.006(3) -0.022(4) -0.014(3) C9 0.047(5) 0.029(4) 0.024(4) 0.001(3) -0.014(3) -0.008(3) C10 0.033(4) 0.030(4) 0.029(4) 0.004(3) -0.012(3) -0.013(3) C11 0.028(4) 0.023(3) 0.026(4) 0.005(3) -0.012(3) -0.009(3) C12 0.031(4) 0.039(4) 0.029(4) 0.002(3) -0.007(3) -0.016(3) C13 0.048(5) 0.048(5) 0.045(5) 0.017(4) -0.015(4) -0.029(4) C14 0.030(4) 0.059(6) 0.046(5) 0.008(4) -0.015(4) -0.018(4) C15 0.027(4) 0.027(4) 0.031(4) 0.000(3) -0.010(3) -0.015(3) C16 0.022(4) 0.052(5) 0.042(5) -0.004(4) -0.007(3) -0.011(4) C17 0.039(4) 0.039(4) 0.043(5) 0.006(4) -0.008(4) -0.020(4) C18 0.021(3) 0.021(3) 0.024(3) -0.001(3) -0.004(3) -0.005(3) C19 0.022(3) 0.030(4) 0.025(4) 0.001(3) -0.005(3) -0.010(3) C20 0.038(4) 0.045(4) 0.023(4) 0.008(3) -0.016(3) -0.016(4) C21 0.046(5) 0.045(5) 0.029(4) 0.013(3) -0.010(4) -0.023(4) C22 0.046(5) 0.043(5) 0.034(4) 0.008(3) -0.008(4) -0.029(4) C23 0.029(4) 0.030(4) 0.028(4) -0.001(3) -0.007(3) -0.013(3) C24 0.030(4) 0.040(4) 0.025(4) 0.002(3) -0.009(3) -0.017(3) C25 0.056(5) 0.055(5) 0.036(5) -0.002(4) -0.011(4) -0.036(5) C26 0.034(4) 0.060(6) 0.045(5) 0.012(4) -0.016(4) -0.019(4) C27 0.033(4) 0.036(4) 0.028(4) 0.000(3) -0.009(3) -0.020(3) C28 0.053(5) 0.040(5) 0.077(7) 0.014(4) -0.044(5) -0.022(4) C29 0.049(5) 0.046(5) 0.048(5) -0.001(4) -0.014(4) -0.028(4) #----------------------------------------------------------------------------# # 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 2.281(5) . ? Pb N1 2.292(5) . ? Pb Br 2.7149(8) . ? N1 C1 1.324(9) . ? N1 C6 1.439(8) . ? N2 C3 1.333(8) . ? N2 C18 1.439(8) . ? C1 C2 1.408(10) . ? C1 C4 1.520(9) . ? C2 C3 1.392(10) . ? C2 H2 0.95 . ? C3 C5 1.519(9) . ? 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 1.399(9) . ? C6 C11 1.408(9) . ? C7 C8 1.426(10) . ? C7 C12 1.527(10) . ? C8 C9 1.399(11) . ? C8 H8 0.95 . ? C9 C10 1.389(11) . ? C9 H9 0.95 . ? C10 C11 1.399(10) . ? C10 H10 0.95 . ? C11 C15 1.509(10) . ? C12 C13 1.521(11) . ? C12 C14 1.536(11) . ? 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 1.507(10) . ? C15 C16 1.567(10) . ? 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 1.410(9) . ? C18 C23 1.421(9) . ? C19 C20 1.372(10) . ? C19 C24 1.521(10) . ? C20 C21 1.380(11) . ? C20 H20 0.95 . ? C21 C22 1.374(11) . ? C21 H21 0.95 . ? C22 C23 1.387(10) . ? C22 H22 0.95 . ? C23 C27 1.536(10) . ? C24 C26 1.529(11) . ? C24 C25 1.537(10) . ? 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 C28 1.519(11) . ? C27 C29 1.537(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 . ? 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 82.93(19) . . ? N2 Pb Br 93.28(14) . . ? N1 Pb Br 91.31(13) . . ? C1 N1 C6 122.9(5) . . ? C1 N1 Pb 125.3(4) . . ? C6 N1 Pb 111.8(4) . . ? C3 N2 C18 121.9(5) . . ? C3 N2 Pb 123.5(4) . . ? C18 N2 Pb 114.3(4) . . ? N1 C1 C2 123.8(6) . . ? N1 C1 C4 119.4(6) . . ? C2 C1 C4 116.8(6) . . ? C3 C2 C1 130.8(6) . . ? C3 C2 H2 114.6 . . ? C1 C2 H2 114.6 . . ? N2 C3 C2 125.2(6) . . ? N2 C3 C5 118.7(6) . . ? C2 C3 C5 116.2(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(6) . . ? C7 C6 N1 121.1(6) . . ? C11 C6 N1 117.3(6) . . ? C6 C7 C8 119.7(6) . . ? C6 C7 C12 122.3(6) . . ? C8 C7 C12 118.0(6) . . ? C9 C8 C7 118.3(7) . . ? C9 C8 H8 120.9 . . ? C7 C8 H8 120.9 . . ? C10 C9 C8 121.4(7) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C9 C10 C11 121.0(7) . . ? C9 C10 H10 119.5 . . ? C11 C10 H10 119.5 . . ? C10 C11 C6 118.3(6) . . ? C10 C11 C15 119.5(6) . . ? C6 C11 C15 122.2(6) . . ? C13 C12 C7 111.3(6) . . ? C13 C12 C14 108.7(7) . . ? C7 C12 C14 112.1(6) . . ? C13 C12 H12 108.2 . . ? C7 C12 H12 108.2 . . ? C14 C12 H12 108.2 . . ? 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 . . ? C17 C15 C11 111.8(6) . . ? C17 C15 C16 111.5(6) . . ? C11 C15 C16 110.9(6) . . ? C17 C15 H15 107.5 . . ? C11 C15 H15 107.5 . . ? C16 C15 H15 107.5 . . ? 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 120.4(6) . . ? C19 C18 N2 121.0(6) . . ? C23 C18 N2 118.4(6) . . ? C20 C19 C18 118.1(6) . . ? C20 C19 C24 119.5(6) . . ? C18 C19 C24 122.4(6) . . ? C19 C20 C21 122.6(7) . . ? C19 C20 H20 118.7 . . ? C21 C20 H20 118.7 . . ? C22 C21 C20 119.1(7) . . ? C22 C21 H21 120.4 . . ? C20 C21 H21 120.4 . . ? C21 C22 C23 121.7(7) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C22 C23 C18 118.2(7) . . ? C22 C23 C27 121.0(7) . . ? C18 C23 C27 120.8(6) . . ? C19 C24 C26 111.7(6) . . ? C19 C24 C25 111.0(6) . . ? C26 C24 C25 109.6(7) . . ? C19 C24 H24 108.2 . . ? C26 C24 H24 108.2 . . ? C25 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 . . ? C28 C27 C23 112.5(6) . . ? C28 C27 C29 108.7(7) . . ? C23 C27 C29 112.8(6) . . ? C28 C27 H27 107.5 . . ? C23 C27 H27 107.5 . . ? C29 C27 H27 107.5 . . ? 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 . . ? #===END data_(4)-jul1406 _database_code_depnum_ccdc_archive 'CCDC 638200' _audit_creation_date 2006-08-01T10:14:12-00:00 _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 'C29 H41 I N2 Pb' _chemical_formula_sum 'C29 H41 I N2 Pb' _chemical_formula_weight 751.73 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/C' _symmetry_space_group_name_Hall '-P 2ybc' _symmetry_Int_Tables_number 14 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 22.3656(5) _cell_length_b 11.2144(3) _cell_length_c 11.6021(3) _cell_angle_alpha 90 _cell_angle_beta 101.411(1) _cell_angle_gamma 90 _cell_volume 2852.48(12) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 80710 _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 0.1 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.02 _exptl_crystal_density_diffrn 1.75 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1456 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 7.015 _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 0.5093 _exptl_absorpt_correction_T_max 0.8175 #----------------------------------------------------------------------------# # 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 0.1521E-3 _diffrn_orient_matrix_ub_12 -0.44118E-1 _diffrn_orient_matrix_ub_13 0.388712E-1 _diffrn_orient_matrix_ub_21 0.27813E-2 _diffrn_orient_matrix_ub_22 -0.774512E-1 _diffrn_orient_matrix_ub_23 -0.21827E-1 _diffrn_orient_matrix_ub_31 0.878852E-1 _diffrn_orient_matrix_ub_32 0.25274E-2 _diffrn_orient_matrix_ub_33 0.96524E-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 0.0601 _diffrn_reflns_av_unetI/netI 0.0334 _diffrn_reflns_number 37364 _diffrn_reflns_limit_h_min -27 _diffrn_reflns_limit_h_max 27 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.51 _diffrn_reflns_theta_max 25.99 _diffrn_reflns_theta_full 25.99 _diffrn_measured_fraction_theta_full 0.997 _diffrn_measured_fraction_theta_max 0.997 _reflns_number_total 5590 _reflns_number_gt 4963 _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 ; 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^)+(0.0095P)^2^+18.2229P] 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 5590 _refine_ls_number_parameters 300 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0739 _refine_ls_wR_factor_gt 0.0714 _refine_ls_goodness_of_fit_ref 1.166 _refine_ls_restrained_S_all 1.166 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.218 _refine_diff_density_min -1.261 _refine_diff_density_rms 0.134 #----------------------------------------------------------------------------# # 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' I I -0.4742 1.8119 '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' 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 0.760980(10) 0.68117(2) 0.661991(19) 0.02241(7) Uani 1 1 d . . . I I 0.72384(2) 0.87631(4) 0.49200(4) 0.03716(12) Uani 1 1 d . . . N1 N 0.8116(2) 0.5877(4) 0.5318(4) 0.0201(10) Uani 1 1 d . . . N2 N 0.6817(2) 0.5606(4) 0.5753(4) 0.0208(10) Uani 1 1 d . . . C1 C 0.7823(3) 0.5483(5) 0.4273(5) 0.0212(12) Uani 1 1 d . . . C2 C 0.7193(3) 0.5333(5) 0.3943(5) 0.0215(12) Uani 1 1 d . . . H2 H 0.7045 0.5253 0.312 0.026 Uiso 1 1 calc R . . C3 C 0.6738(2) 0.5281(5) 0.4630(5) 0.0214(12) Uani 1 1 d . . . C4 C 0.8200(3) 0.5109(6) 0.3388(5) 0.0292(14) Uani 1 1 d . . . H4A H 0.8424 0.4378 0.3659 0.044 Uiso 1 1 calc R . . H4B H 0.8489 0.5744 0.3305 0.044 Uiso 1 1 calc R . . H4C H 0.7931 0.4962 0.2626 0.044 Uiso 1 1 calc R . . C5 C 0.6128(3) 0.4772(6) 0.4044(6) 0.0298(14) Uani 1 1 d . . . H5A H 0.5816 0.5395 0.3974 0.045 Uiso 1 1 calc R . . H5B H 0.602 0.4113 0.4519 0.045 Uiso 1 1 calc R . . H5C H 0.6153 0.4478 0.326 0.045 Uiso 1 1 calc R . . C6 C 0.8766(2) 0.5769(5) 0.5651(5) 0.0202(12) Uani 1 1 d . . . C7 C 0.9012(3) 0.4711(5) 0.6208(5) 0.0249(13) Uani 1 1 d . . . C8 C 0.9641(3) 0.4634(6) 0.6611(5) 0.0311(14) Uani 1 1 d . . . H8 H 0.9812 0.3924 0.6984 0.037 Uiso 1 1 calc R . . C9 C 1.0019(3) 0.5574(6) 0.6474(5) 0.0316(14) Uani 1 1 d . . . H9 H 1.0447 0.5511 0.6757 0.038 Uiso 1 1 calc R . . C10 C 0.9776(3) 0.6609(6) 0.5925(5) 0.0304(14) Uani 1 1 d . . . H10 H 1.0039 0.7255 0.5845 0.037 Uiso 1 1 calc R . . C11 C 0.9151(3) 0.6723(5) 0.5488(5) 0.0221(12) Uani 1 1 d . . . C12 C 0.8616(3) 0.3666(5) 0.6417(6) 0.0317(14) Uani 1 1 d . . . H12 H 0.8184 0.3852 0.6035 0.038 Uiso 1 1 calc R . . C13 C 0.8641(4) 0.3490(7) 0.7719(7) 0.051(2) Uani 1 1 d . . . H13A H 0.8381 0.2816 0.7837 0.077 Uiso 1 1 calc R . . H13B H 0.8495 0.4214 0.805 0.077 Uiso 1 1 calc R . . H13C H 0.9062 0.3328 0.8114 0.077 Uiso 1 1 calc R . . C14 C 0.8800(4) 0.2503(6) 0.5881(7) 0.052(2) Uani 1 1 d . . . H14A H 0.8531 0.1855 0.6031 0.079 Uiso 1 1 calc R . . H14B H 0.9223 0.2307 0.6239 0.079 Uiso 1 1 calc R . . H14C H 0.8764 0.2604 0.5031 0.079 Uiso 1 1 calc R . . C15 C 0.8918(3) 0.7854(5) 0.4845(5) 0.0270(13) Uani 1 1 d . . . H15 H 0.8471 0.7754 0.4534 0.032 Uiso 1 1 calc R . . C16 C 0.9228(3) 0.8080(6) 0.3791(6) 0.0362(15) Uani 1 1 d . . . H16A H 0.9066 0.8814 0.3389 0.054 Uiso 1 1 calc R . . H16B H 0.9146 0.7408 0.3242 0.054 Uiso 1 1 calc R . . H16C H 0.9669 0.8161 0.4071 0.054 Uiso 1 1 calc R . . C17 C 0.9004(3) 0.8938(6) 0.5657(6) 0.0406(17) Uani 1 1 d . . . H17A H 0.8846 0.965 0.5209 0.061 Uiso 1 1 calc R . . H17B H 0.9439 0.9045 0.5987 0.061 Uiso 1 1 calc R . . H17C H 0.8783 0.8815 0.6297 0.061 Uiso 1 1 calc R . . C18 C 0.6360(3) 0.5359(5) 0.6435(5) 0.0252(13) Uani 1 1 d . . . C19 C 0.6418(3) 0.4345(6) 0.7156(6) 0.0315(14) Uani 1 1 d . . . C20 C 0.5992(3) 0.4157(7) 0.7861(6) 0.0392(16) Uani 1 1 d . . . H20 H 0.6031 0.3474 0.8355 0.047 Uiso 1 1 calc R . . C21 C 0.5521(3) 0.4923(7) 0.7864(6) 0.0395(17) Uani 1 1 d . . . H21 H 0.5238 0.478 0.836 0.047 Uiso 1 1 calc R . . C22 C 0.5458(3) 0.5917(6) 0.7137(6) 0.0350(15) Uani 1 1 d . . . H22 H 0.5126 0.6446 0.7135 0.042 Uiso 1 1 calc R . . C23 C 0.5867(3) 0.6157(5) 0.6412(5) 0.0267(13) Uani 1 1 d . . . C24 C 0.6937(4) 0.3459(7) 0.7197(7) 0.050(2) Uani 1 1 d . . . H24 H 0.728 0.3875 0.6926 0.06 Uiso 1 1 calc R . . C25 C 0.7179(4) 0.2967(6) 0.8427(7) 0.050(2) Uani 1 1 d . . . H25A H 0.7514 0.2411 0.8402 0.075 Uiso 1 1 calc R . . H25B H 0.685 0.2549 0.8707 0.075 Uiso 1 1 calc R . . H25C H 0.7327 0.3626 0.8962 0.075 Uiso 1 1 calc R . . C26 C 0.6726(6) 0.2413(10) 0.6352(8) 0.108(5) Uani 1 1 d . . . H26A H 0.7064 0.1849 0.638 0.163 Uiso 1 1 calc R . . H26B H 0.6599 0.2718 0.555 0.163 Uiso 1 1 calc R . . H26C H 0.6382 0.2007 0.659 0.163 Uiso 1 1 calc R . . C27 C 0.5785(3) 0.7280(5) 0.5680(6) 0.0299(14) Uani 1 1 d . . . H27 H 0.6085 0.7258 0.5146 0.036 Uiso 1 1 calc R . . C28 C 0.5928(3) 0.8373(6) 0.6475(7) 0.0448(18) Uani 1 1 d . . . H28A H 0.5875 0.9097 0.5993 0.067 Uiso 1 1 calc R . . H28B H 0.635 0.8326 0.6911 0.067 Uiso 1 1 calc R . . H28C H 0.565 0.8395 0.7031 0.067 Uiso 1 1 calc R . . C29 C 0.5142(3) 0.7373(7) 0.4911(7) 0.0423(17) Uani 1 1 d . . . H29A H 0.511 0.8112 0.4452 0.064 Uiso 1 1 calc R . . H29B H 0.4838 0.7378 0.5415 0.064 Uiso 1 1 calc R . . H29C H 0.5069 0.6688 0.4377 0.064 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 0.02100(12) 0.02513(12) 0.02177(11) -0.00285(9) 0.00589(8) -0.00097(9) I 0.0331(2) 0.0284(2) 0.0521(3) 0.0099(2) 0.0137(2) 0.00601(18) N1 0.014(2) 0.023(2) 0.025(3) -0.001(2) 0.0064(19) -0.0001(18) N2 0.018(2) 0.023(2) 0.023(3) 0.000(2) 0.008(2) -0.0033(19) C1 0.025(3) 0.022(3) 0.019(3) 0.004(2) 0.010(2) 0.005(2) C2 0.024(3) 0.024(3) 0.016(3) 0.000(2) 0.002(2) 0.003(2) C3 0.020(3) 0.018(3) 0.024(3) 0.002(2) -0.001(2) 0.004(2) C4 0.028(3) 0.031(3) 0.028(3) 0.002(3) 0.006(3) 0.000(3) C5 0.021(3) 0.033(3) 0.034(4) -0.006(3) 0.004(3) -0.003(3) C6 0.017(3) 0.030(3) 0.015(3) -0.002(2) 0.005(2) 0.004(2) C7 0.027(3) 0.026(3) 0.022(3) -0.001(2) 0.006(2) 0.003(2) C8 0.031(3) 0.034(4) 0.026(3) -0.003(3) 0.002(3) 0.011(3) C9 0.019(3) 0.049(4) 0.027(3) 0.001(3) 0.005(3) 0.004(3) C10 0.020(3) 0.040(4) 0.032(3) -0.002(3) 0.004(3) -0.001(3) C11 0.021(3) 0.029(3) 0.018(3) -0.003(2) 0.007(2) 0.004(2) C12 0.030(3) 0.027(3) 0.036(4) 0.005(3) 0.002(3) 0.004(3) C13 0.062(5) 0.050(5) 0.045(5) 0.007(4) 0.018(4) -0.007(4) C14 0.067(6) 0.032(4) 0.060(5) -0.003(4) 0.018(4) -0.001(4) C15 0.023(3) 0.034(3) 0.024(3) 0.003(3) 0.004(2) -0.005(2) C16 0.038(4) 0.041(4) 0.030(3) 0.009(3) 0.009(3) 0.001(3) C17 0.046(4) 0.035(4) 0.040(4) -0.001(3) 0.006(3) -0.004(3) C18 0.022(3) 0.026(3) 0.029(3) -0.002(3) 0.009(3) -0.007(2) C19 0.033(4) 0.032(3) 0.033(4) 0.002(3) 0.015(3) -0.004(3) C20 0.036(4) 0.046(4) 0.041(4) 0.008(3) 0.019(3) -0.003(3) C21 0.033(4) 0.051(4) 0.039(4) -0.007(3) 0.018(3) -0.011(3) C22 0.020(3) 0.047(4) 0.039(4) -0.009(3) 0.010(3) -0.005(3) C23 0.019(3) 0.033(3) 0.028(3) -0.004(3) 0.005(2) -0.004(3) C24 0.050(5) 0.045(4) 0.066(5) 0.024(4) 0.036(4) 0.012(4) C25 0.053(5) 0.034(4) 0.064(5) 0.010(4) 0.013(4) 0.007(3) C26 0.192(13) 0.092(8) 0.036(5) -0.001(5) 0.010(6) 0.090(9) C27 0.020(3) 0.030(3) 0.041(4) -0.004(3) 0.009(3) 0.001(3) C28 0.037(4) 0.038(4) 0.064(5) -0.011(4) 0.021(4) 0.000(3) C29 0.028(4) 0.046(4) 0.052(4) 0.008(4) 0.005(3) 0.004(3) #----------------------------------------------------------------------------# # 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 2.298(4) . ? Pb N1 2.311(4) . ? Pb I 2.9531(5) . ? N1 C1 1.334(7) . ? N1 C6 1.434(7) . ? N2 C3 1.330(7) . ? N2 C18 1.439(7) . ? C1 C2 1.396(8) . ? C1 C4 1.511(8) . ? C2 C3 1.413(8) . ? C2 H2 0.95 . ? C3 C5 1.510(8) . ? 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 1.409(8) . ? C6 C11 1.409(8) . ? C7 C8 1.396(8) . ? C7 C12 1.518(8) . ? C8 C9 1.380(9) . ? C8 H8 0.95 . ? C9 C10 1.382(9) . ? C9 H9 0.95 . ? C10 C11 1.394(8) . ? C10 H10 0.95 . ? C11 C15 1.511(8) . ? C12 C13 1.514(9) . ? C12 C14 1.536(9) . ? 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(9) . ? C15 C16 1.542(8) . ? 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 1.402(8) . ? C18 C23 1.416(8) . ? C19 C20 1.390(9) . ? C19 C24 1.522(9) . ? C20 C21 1.360(10) . ? C20 H20 0.95 . ? C21 C22 1.388(10) . ? C21 H21 0.95 . ? C22 C23 1.385(8) . ? C22 H22 0.95 . ? C23 C27 1.510(9) . ? C24 C25 1.526(10) . ? C24 C26 1.541(13) . ? 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 C28 1.529(9) . ? C27 C29 1.538(9) . ? 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 . ? 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 83.26(16) . . ? N2 Pb I 93.02(11) . . ? N1 Pb I 90.52(11) . . ? C1 N1 C6 120.4(4) . . ? C1 N1 Pb 121.9(4) . . ? C6 N1 Pb 117.7(3) . . ? C3 N2 C18 121.0(5) . . ? C3 N2 Pb 122.1(4) . . ? C18 N2 Pb 116.3(3) . . ? N1 C1 C2 125.3(5) . . ? N1 C1 C4 118.0(5) . . ? C2 C1 C4 116.7(5) . . ? C1 C2 C3 130.6(5) . . ? C1 C2 H2 114.7 . . ? C3 C2 H2 114.7 . . ? N2 C3 C2 124.8(5) . . ? N2 C3 C5 118.6(5) . . ? C2 C3 C5 116.6(5) . . ? 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 120.5(5) . . ? C7 C6 N1 118.5(5) . . ? C11 C6 N1 120.9(5) . . ? C8 C7 C6 118.8(5) . . ? C8 C7 C12 118.7(5) . . ? C6 C7 C12 122.4(5) . . ? C9 C8 C7 121.0(6) . . ? C9 C8 H8 119.5 . . ? C7 C8 H8 119.5 . . ? C8 C9 C10 119.9(6) . . ? C8 C9 H9 120 . . ? C10 C9 H9 120 . . ? C9 C10 C11 121.3(6) . . ? C9 C10 H10 119.3 . . ? C11 C10 H10 119.3 . . ? C10 C11 C6 118.4(5) . . ? C10 C11 C15 118.7(5) . . ? C6 C11 C15 122.9(5) . . ? C13 C12 C7 110.6(6) . . ? C13 C12 C14 109.5(6) . . ? C7 C12 C14 112.3(6) . . ? C13 C12 H12 108.1 . . ? C7 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 C17 112.0(5) . . ? C11 C15 C16 111.3(5) . . ? C17 C15 C16 109.7(5) . . ? 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 120.3(5) . . ? C19 C18 N2 119.4(5) . . ? C23 C18 N2 120.2(5) . . ? C20 C19 C18 118.7(6) . . ? C20 C19 C24 119.3(6) . . ? C18 C19 C24 122.0(5) . . ? C21 C20 C19 121.8(7) . . ? C21 C20 H20 119.1 . . ? C19 C20 H20 119.1 . . ? C20 C21 C22 119.4(6) . . ? C20 C21 H21 120.3 . . ? C22 C21 H21 120.3 . . ? C23 C22 C21 121.6(6) . . ? C23 C22 H22 119.2 . . ? C21 C22 H22 119.2 . . ? C22 C23 C18 118.1(6) . . ? C22 C23 C27 118.8(6) . . ? C18 C23 C27 123.0(5) . . ? C19 C24 C25 113.1(6) . . ? C19 C24 C26 110.0(7) . . ? C25 C24 C26 109.1(6) . . ? C19 C24 H24 108.2 . . ? C25 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 C28 110.0(6) . . ? C23 C27 C29 112.3(5) . . ? C28 C27 C29 110.8(6) . . ? C23 C27 H27 107.9 . . ? C28 C27 H27 107.9 . . ? C29 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 . . ? #===END data_(5)-oct603 _database_code_depnum_ccdc_archive 'CCDC 638201' _audit_creation_date 2003-10-06T14:21:17-00:00 _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 'C35 H59 N3 Pb1 Si2, 0.5(C6 H6)' _chemical_formula_sum 'C38 H62 N3 Pb Si2' _chemical_formula_weight 824.28 _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 11.9346(1) _cell_length_b 13.3033(1) _cell_length_c 14.6879(2) _cell_angle_alpha 97.37 _cell_angle_beta 100.251(1) _cell_angle_gamma 115.650(1) _cell_volume 2012.49(4) _cell_formula_units_Z 2 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 12023 _cell_measurement_theta_min 3.705 _cell_measurement_theta_max 25.028 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour yellow _exptl_crystal_size_max 0.2 _exptl_crystal_size_mid 0.2 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.36 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 842 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.279 _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 0.407 _exptl_absorpt_correction_T_max 0.619 #----------------------------------------------------------------------------# # 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 0.335227E-1 _diffrn_orient_matrix_ub_12 0.322713E-1 _diffrn_orient_matrix_ub_13 0.702573E-1 _diffrn_orient_matrix_ub_21 0.892339E-1 _diffrn_orient_matrix_ub_22 0.193091E-1 _diffrn_orient_matrix_ub_23 -0.48403E-2 _diffrn_orient_matrix_ub_31 0.136182E-1 _diffrn_orient_matrix_ub_32 0.770218E-1 _diffrn_orient_matrix_ub_33 -0.99108E-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 0.0405 _diffrn_reflns_av_unetI/netI 0.0371 _diffrn_reflns_number 21146 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.71 _diffrn_reflns_theta_max 25.04 _diffrn_reflns_theta_full 25.04 _diffrn_measured_fraction_theta_full 0.982 _diffrn_measured_fraction_theta_max 0.982 _reflns_number_total 6985 _reflns_number_gt 6494 _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^)+(0.0224P)^2^+2.6530P] 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 riding _refine_ls_extinction_method none _refine_ls_number_reflns 6985 _refine_ls_number_parameters 399 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0289 _refine_ls_R_factor_gt 0.025 _refine_ls_wR_factor_ref 0.0578 _refine_ls_wR_factor_gt 0.0562 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.598 _refine_diff_density_min -1.119 _refine_diff_density_rms 0.086 #----------------------------------------------------------------------------# # 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' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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 0.661476(11) 0.742396(10) 0.679046(9) 0.02119(5) Uani 1 1 d . . . Si1 Si 0.66435(12) 0.97969(10) 0.64651(9) 0.0421(3) Uani 1 1 d . . . Si2 Si 0.79282(10) 1.01568(8) 0.85074(8) 0.0326(2) Uani 1 1 d . . . N1 N 0.6002(3) 0.6537(2) 0.8021(2) 0.0234(6) Uani 1 1 d . . . N2 N 0.8519(3) 0.7328(2) 0.7347(2) 0.0239(6) Uani 1 1 d . . . N3 N 0.7231(3) 0.9312(2) 0.7370(2) 0.0272(7) Uani 1 1 d . . . C1 C 0.6789(3) 0.6425(3) 0.8716(3) 0.0269(8) Uani 1 1 d . . . C2 C 0.8100(3) 0.6778(3) 0.8810(3) 0.0267(8) Uani 1 1 d . . . H2 H 0.8554 0.6791 0.9416 0.032 Uiso 1 1 calc R . . C3 C 0.8864(3) 0.7115(3) 0.8174(3) 0.0235(7) Uani 1 1 d . . . C4 C 0.6262(4) 0.5848(4) 0.9481(3) 0.0494(12) Uani 1 1 d . . . H4A H 0.5407 0.5786 0.9449 0.074 Uiso 1 1 calc R . . H4B H 0.6842 0.6306 1.0108 0.074 Uiso 1 1 calc R . . H4C H 0.6199 0.5081 0.9382 0.074 Uiso 1 1 calc R . . C5 C 1.0200(3) 0.7219(3) 0.8497(3) 0.0345(9) Uani 1 1 d . . . H5A H 1.0465 0.7 0.7942 0.052 Uiso 1 1 calc R . . H5B H 1.0185 0.6711 0.8928 0.052 Uiso 1 1 calc R . . H5C H 1.0812 0.8013 0.8829 0.052 Uiso 1 1 calc R . . C6 C 0.4631(3) 0.5841(3) 0.7835(3) 0.0314(8) Uani 1 1 d . . . C7 C 0.4083(4) 0.4671(4) 0.7426(3) 0.0452(11) Uani 1 1 d . . . C8 C 0.2740(4) 0.4015(4) 0.7212(4) 0.0616(14) Uani 1 1 d . . . H8 H 0.2352 0.3216 0.694 0.074 Uiso 1 1 calc R . . C9 C 0.1979(4) 0.4505(5) 0.7390(4) 0.0667(15) Uani 1 1 d . . . H9 H 0.1072 0.4046 0.7244 0.08 Uiso 1 1 calc R . . C10 C 0.2519(4) 0.5650(5) 0.7777(4) 0.0565(13) Uani 1 1 d . . . H10 H 0.1978 0.598 0.7891 0.068 Uiso 1 1 calc R . . C11 C 0.3847(3) 0.6349(4) 0.8010(3) 0.0399(10) Uani 1 1 d . . . C12 C 0.4861(5) 0.4088(4) 0.7148(4) 0.0594(14) Uani 1 1 d . . . H12 H 0.5794 0.4654 0.7395 0.071 Uiso 1 1 calc R . . C13 C 0.4552(6) 0.3762(5) 0.6058(5) 0.094(2) Uani 1 1 d . . . H13A H 0.5054 0.339 0.5871 0.141 Uiso 1 1 calc R . . H13B H 0.4773 0.4455 0.5811 0.141 Uiso 1 1 calc R . . H13C H 0.3631 0.3234 0.5797 0.141 Uiso 1 1 calc R . . C14 C 0.4630(7) 0.3052(5) 0.7566(7) 0.115(3) Uani 1 1 d . . . H14A H 0.516 0.2715 0.7372 0.173 Uiso 1 1 calc R . . H14B H 0.3719 0.2484 0.7335 0.173 Uiso 1 1 calc R . . H14C H 0.4862 0.3289 0.8261 0.173 Uiso 1 1 calc R . . C15 C 0.4422(4) 0.7608(4) 0.8501(4) 0.0498(12) Uani 1 1 d . . . H15 H 0.5231 0.8035 0.8307 0.06 Uiso 1 1 calc R . . C16 C 0.3553(5) 0.8148(6) 0.8234(7) 0.104(3) Uani 1 1 d . . . H16A H 0.3986 0.8955 0.8574 0.157 Uiso 1 1 calc R . . H16B H 0.2745 0.7742 0.8409 0.157 Uiso 1 1 calc R . . H16C H 0.3368 0.8094 0.7547 0.157 Uiso 1 1 calc R . . C17 C 0.4791(6) 0.7782(5) 0.9595(4) 0.0806(18) Uani 1 1 d . . . H17A H 0.5164 0.8599 0.9895 0.121 Uiso 1 1 calc R . . H17B H 0.5423 0.7511 0.9779 0.121 Uiso 1 1 calc R . . H17C H 0.402 0.7348 0.9804 0.121 Uiso 1 1 calc R . . C18 C 0.9279(3) 0.7402(3) 0.6668(3) 0.0284(8) Uani 1 1 d . . . C19 C 0.8970(4) 0.6391(3) 0.6007(3) 0.0343(9) Uani 1 1 d . . . C20 C 0.9736(5) 0.6458(4) 0.5378(4) 0.0521(12) Uani 1 1 d . . . H20 H 0.9545 0.5786 0.4932 0.063 Uiso 1 1 calc R . . C21 C 1.0763(5) 0.7482(5) 0.5393(4) 0.0648(15) Uani 1 1 d . . . H21 H 1.1289 0.7508 0.4972 0.078 Uiso 1 1 calc R . . C22 C 1.1024(5) 0.8464(4) 0.6015(4) 0.0626(15) Uani 1 1 d . . . H22 H 1.1724 0.9168 0.6008 0.075 Uiso 1 1 calc R . . C23 C 1.0292(4) 0.8464(3) 0.6661(3) 0.0419(10) Uani 1 1 d . . . C24 C 0.7876(4) 0.5243(3) 0.5981(3) 0.0357(9) Uani 1 1 d . . . H24 H 0.7205 0.5384 0.621 0.043 Uiso 1 1 calc R . . C25 C 0.8314(5) 0.4607(4) 0.6641(4) 0.0612(14) Uani 1 1 d . . . H25A H 0.7581 0.3869 0.6607 0.092 Uiso 1 1 calc R . . H25B H 0.865 0.5069 0.7295 0.092 Uiso 1 1 calc R . . H25C H 0.8991 0.4477 0.6442 0.092 Uiso 1 1 calc R . . C26 C 0.7241(5) 0.4464(5) 0.4974(4) 0.0640(14) Uani 1 1 d . . . H26A H 0.6537 0.3735 0.4996 0.096 Uiso 1 1 calc R . . H26B H 0.7882 0.432 0.4728 0.096 Uiso 1 1 calc R . . H26C H 0.69 0.4841 0.4556 0.096 Uiso 1 1 calc R . . C27 C 1.0631(4) 0.9585(3) 0.7306(4) 0.0499(12) Uani 1 1 d . . . H27 H 1.0005 0.9437 0.7705 0.06 Uiso 1 1 calc R . . C28 C 1.1999(5) 1.0139(4) 0.7972(4) 0.0654(15) Uani 1 1 d . . . H28A H 1.2174 1.0863 0.8379 0.098 Uiso 1 1 calc R . . H28B H 1.2626 1.0289 0.7592 0.098 Uiso 1 1 calc R . . H28C H 1.2066 0.9619 0.837 0.098 Uiso 1 1 calc R . . C29 C 1.0512(5) 1.0422(4) 0.6711(5) 0.0717(17) Uani 1 1 d . . . H29A H 1.0728 1.1147 0.7136 0.108 Uiso 1 1 calc R . . H29B H 0.9628 1.009 0.6315 0.108 Uiso 1 1 calc R . . H29C H 1.1106 1.0563 0.6303 0.108 Uiso 1 1 calc R . . C30 C 0.6852(7) 0.9261(5) 0.5309(4) 0.0777(19) Uani 1 1 d . . . H30A H 0.645 0.8423 0.5166 0.116 Uiso 1 1 calc R . . H30B H 0.7772 0.9574 0.5344 0.116 Uiso 1 1 calc R . . H30C H 0.6442 0.9505 0.4805 0.116 Uiso 1 1 calc R . . C31 C 0.7441(7) 1.1393(4) 0.6634(4) 0.081(2) Uani 1 1 d . . . H31A H 0.7368 1.1743 0.7235 0.122 Uiso 1 1 calc R . . H31B H 0.7021 1.1597 0.6107 0.122 Uiso 1 1 calc R . . H31C H 0.8353 1.1674 0.665 0.122 Uiso 1 1 calc R . . C32 C 0.4864(6) 0.9281(7) 0.6279(6) 0.118(3) Uani 1 1 d . . . H32A H 0.4698 0.9543 0.6871 0.177 Uiso 1 1 calc R . . H32B H 0.4409 0.8442 0.6095 0.177 Uiso 1 1 calc R . . H32C H 0.4559 0.9589 0.5775 0.177 Uiso 1 1 calc R . . C33 C 0.9540(4) 1.1411(4) 0.8655(4) 0.0519(12) Uani 1 1 d . . . H33A H 0.946 1.1876 0.8206 0.078 Uiso 1 1 calc R . . H33B H 1.015 1.1134 0.8529 0.078 Uiso 1 1 calc R . . H33C H 0.9854 1.1877 0.9306 0.078 Uiso 1 1 calc R . . C34 C 0.6918(5) 1.0783(4) 0.8930(4) 0.0526(12) Uani 1 1 d . . . H34A H 0.674 1.1216 0.8483 0.079 Uiso 1 1 calc R . . H34B H 0.7384 1.1296 0.9561 0.079 Uiso 1 1 calc R . . H34C H 0.6105 1.0163 0.8965 0.079 Uiso 1 1 calc R . . C35 C 0.8214(5) 0.9360(4) 0.9392(3) 0.0524(12) Uani 1 1 d . . . H35A H 0.8741 0.9016 0.9204 0.079 Uiso 1 1 calc R . . H35B H 0.7387 0.8755 0.9422 0.079 Uiso 1 1 calc R . . H35C H 0.8664 0.9888 1.0019 0.079 Uiso 1 1 calc R . . C36 C 0.9011(8) 0.5007(7) 1.0325(6) 0.082(2) Uani 1 1 d . . . H36 H 0.8313 0.5011 1.055 0.098 Uiso 1 1 calc R . . C37 C 0.8780(6) 0.4350(5) 0.9461(5) 0.0774(19) Uani 1 1 d . . . H37 H 0.792 0.389 0.9082 0.093 Uiso 1 1 calc R . . C38 C 0.9774(9) 0.4345(5) 0.9133(4) 0.079(2) Uani 1 1 d . . . H38 H 0.9612 0.3888 0.8525 0.095 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 0.02125(7) 0.01954(8) 0.02167(8) 0.00429(5) 0.00472(5) 0.00901(6) Si1 0.0553(7) 0.0326(6) 0.0383(7) 0.0141(5) 0.0015(6) 0.0230(5) Si2 0.0401(6) 0.0248(5) 0.0315(6) 0.0017(4) 0.0033(5) 0.0175(5) N1 0.0203(14) 0.0239(15) 0.0287(17) 0.0108(12) 0.0119(12) 0.0093(12) N2 0.0220(14) 0.0238(15) 0.0317(18) 0.0109(13) 0.0131(13) 0.0125(12) N3 0.0333(16) 0.0218(15) 0.0263(17) 0.0046(12) 0.0048(13) 0.0141(13) C1 0.0277(18) 0.0253(18) 0.031(2) 0.0107(15) 0.0124(16) 0.0120(15) C2 0.0287(18) 0.0294(19) 0.025(2) 0.0126(15) 0.0067(15) 0.0142(16) C3 0.0214(17) 0.0179(16) 0.031(2) 0.0076(14) 0.0069(15) 0.0089(14) C4 0.045(2) 0.068(3) 0.050(3) 0.038(2) 0.025(2) 0.028(2) C5 0.0232(18) 0.038(2) 0.047(3) 0.0152(19) 0.0112(17) 0.0165(17) C6 0.0205(17) 0.038(2) 0.032(2) 0.0135(17) 0.0127(16) 0.0067(16) C7 0.031(2) 0.040(2) 0.048(3) 0.003(2) 0.020(2) -0.0004(18) C8 0.039(3) 0.049(3) 0.060(3) -0.007(2) 0.023(2) -0.011(2) C9 0.027(2) 0.084(4) 0.063(4) 0.004(3) 0.020(2) 0.003(2) C10 0.029(2) 0.080(4) 0.062(3) 0.021(3) 0.023(2) 0.021(2) C11 0.0230(19) 0.055(3) 0.045(3) 0.019(2) 0.0143(18) 0.0172(19) C12 0.047(3) 0.025(2) 0.089(4) 0.001(2) 0.031(3) 0.001(2) C13 0.063(4) 0.071(4) 0.101(5) -0.038(4) 0.038(4) -0.002(3) C14 0.104(5) 0.048(4) 0.216(10) 0.053(5) 0.078(6) 0.034(4) C15 0.041(2) 0.053(3) 0.073(4) 0.022(2) 0.033(2) 0.028(2) C16 0.047(3) 0.083(4) 0.216(9) 0.063(5) 0.051(4) 0.045(3) C17 0.100(5) 0.062(3) 0.075(4) 0.003(3) 0.045(4) 0.029(3) C18 0.0264(18) 0.034(2) 0.036(2) 0.0167(17) 0.0182(16) 0.0188(16) C19 0.038(2) 0.039(2) 0.038(2) 0.0120(18) 0.0189(18) 0.0246(18) C20 0.058(3) 0.059(3) 0.052(3) 0.011(2) 0.033(2) 0.032(2) C21 0.069(3) 0.074(4) 0.071(4) 0.025(3) 0.054(3) 0.036(3) C22 0.059(3) 0.057(3) 0.092(4) 0.035(3) 0.057(3) 0.025(3) C23 0.040(2) 0.037(2) 0.060(3) 0.020(2) 0.029(2) 0.0193(19) C24 0.036(2) 0.035(2) 0.037(2) 0.0017(17) 0.0126(18) 0.0187(18) C25 0.074(3) 0.035(2) 0.068(4) 0.010(2) 0.008(3) 0.024(2) C26 0.051(3) 0.069(3) 0.053(3) -0.008(3) 0.008(2) 0.019(3) C27 0.046(3) 0.030(2) 0.085(4) 0.022(2) 0.041(3) 0.015(2) C28 0.059(3) 0.043(3) 0.085(4) 0.013(3) 0.030(3) 0.012(2) C29 0.073(4) 0.049(3) 0.109(5) 0.039(3) 0.044(3) 0.031(3) C30 0.148(6) 0.054(3) 0.033(3) 0.018(2) 0.017(3) 0.049(4) C31 0.153(6) 0.040(3) 0.056(4) 0.020(2) 0.016(4) 0.052(3) C32 0.067(4) 0.176(8) 0.131(7) 0.094(6) 0.003(4) 0.066(5) C33 0.049(3) 0.033(2) 0.059(3) -0.008(2) 0.000(2) 0.017(2) C34 0.062(3) 0.044(3) 0.057(3) 0.001(2) 0.020(2) 0.030(2) C35 0.072(3) 0.038(2) 0.036(3) 0.0002(19) -0.004(2) 0.026(2) C36 0.114(6) 0.122(6) 0.089(5) 0.082(5) 0.062(5) 0.097(5) C37 0.068(4) 0.059(3) 0.085(5) 0.041(3) -0.001(3) 0.013(3) C38 0.153(7) 0.072(4) 0.050(4) 0.024(3) 0.030(4) 0.082(5) #----------------------------------------------------------------------------# # 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 N3 2.281(3) . ? Pb N2 2.338(3) . ? Pb N1 2.338(3) . ? Si1 N3 1.718(3) . ? Si1 C30 1.857(6) . ? Si1 C31 1.873(5) . ? Si1 C32 1.881(6) . ? Si2 N3 1.721(3) . ? Si2 C35 1.854(4) . ? Si2 C33 1.874(5) . ? Si2 C34 1.880(4) . ? N1 C1 1.328(4) . ? N1 C6 1.440(4) . ? N2 C3 1.318(4) . ? N2 C18 1.448(4) . ? C1 C2 1.399(5) . ? C1 C4 1.518(5) . ? C2 C3 1.401(5) . ? C3 C5 1.519(5) . ? C6 C7 1.396(6) . ? C6 C11 1.410(5) . ? C7 C8 1.404(6) . ? C7 C12 1.519(6) . ? C8 C9 1.369(7) . ? C9 C10 1.363(7) . ? C10 C11 1.394(6) . ? C11 C15 1.521(6) . ? C12 C14 1.516(8) . ? C12 C13 1.536(8) . ? C15 C16 1.521(6) . ? C15 C17 1.548(8) . ? C18 C23 1.409(5) . ? C18 C19 1.413(5) . ? C19 C20 1.396(6) . ? C19 C24 1.510(5) . ? C20 C21 1.376(7) . ? C21 C22 1.372(7) . ? C22 C23 1.399(6) . ? C23 C27 1.504(6) . ? C24 C25 1.529(6) . ? C24 C26 1.537(6) . ? C27 C29 1.538(7) . ? C27 C28 1.540(7) . ? C36 C38 1.345(10) 2_767 ? C36 C37 1.355(10) . ? C37 C38 1.360(9) . ? C38 C36 1.345(10) 2_767 ? 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 Pb N2 101.74(10) . . ? N3 Pb N1 104.91(10) . . ? N2 Pb N1 83.54(9) . . ? N3 Si1 C30 112.2(2) . . ? N3 Si1 C31 114.8(2) . . ? C30 Si1 C31 104.5(3) . . ? N3 Si1 C32 111.1(2) . . ? C30 Si1 C32 106.0(4) . . ? C31 Si1 C32 107.8(3) . . ? N3 Si2 C35 112.59(17) . . ? N3 Si2 C33 113.9(2) . . ? C35 Si2 C33 105.0(2) . . ? N3 Si2 C34 112.81(19) . . ? C35 Si2 C34 106.3(2) . . ? C33 Si2 C34 105.5(2) . . ? C1 N1 C6 119.8(3) . . ? C1 N1 Pb 125.1(2) . . ? C6 N1 Pb 113.2(2) . . ? C3 N2 C18 119.7(3) . . ? C3 N2 Pb 125.0(2) . . ? C18 N2 Pb 115.0(2) . . ? Si1 N3 Si2 120.73(16) . . ? Si1 N3 Pb 107.35(14) . . ? Si2 N3 Pb 131.26(15) . . ? N1 C1 C2 125.8(3) . . ? N1 C1 C4 119.4(3) . . ? C2 C1 C4 114.8(3) . . ? C1 C2 C3 131.7(3) . . ? N2 C3 C2 126.0(3) . . ? N2 C3 C5 119.3(3) . . ? C2 C3 C5 114.6(3) . . ? C7 C6 C11 120.6(3) . . ? C7 C6 N1 119.1(3) . . ? C11 C6 N1 120.2(3) . . ? C6 C7 C8 118.3(4) . . ? C6 C7 C12 123.2(3) . . ? C8 C7 C12 118.3(4) . . ? C9 C8 C7 121.1(5) . . ? C10 C9 C8 120.2(4) . . ? C9 C10 C11 121.6(4) . . ? C10 C11 C6 118.2(4) . . ? C10 C11 C15 120.0(4) . . ? C6 C11 C15 121.7(3) . . ? C14 C12 C7 112.8(4) . . ? C14 C12 C13 111.2(5) . . ? C7 C12 C13 108.8(5) . . ? C11 C15 C16 114.1(4) . . ? C11 C15 C17 110.9(4) . . ? C16 C15 C17 108.9(5) . . ? C23 C18 C19 121.0(3) . . ? C23 C18 N2 120.6(3) . . ? C19 C18 N2 118.5(3) . . ? C20 C19 C18 118.3(4) . . ? C20 C19 C24 119.2(4) . . ? C18 C19 C24 122.5(3) . . ? C21 C20 C19 121.2(4) . . ? C22 C21 C20 119.9(4) . . ? C21 C22 C23 122.1(4) . . ? C22 C23 C18 117.5(4) . . ? C22 C23 C27 118.5(4) . . ? C18 C23 C27 124.0(4) . . ? C19 C24 C25 111.7(3) . . ? C19 C24 C26 112.8(4) . . ? C25 C24 C26 108.8(4) . . ? C23 C27 C29 110.0(5) . . ? C23 C27 C28 112.4(4) . . ? C29 C27 C28 109.4(4) . . ? C38 C36 C37 120.2(6) 2_767 . ? C36 C37 C38 120.2(6) . . ? C36 C38 C37 119.6(6) 2_767 . ? #===END