# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2012 data_global _journal_name_full 'Dalton Trans.' _journal_coden_cambridge 0222 _journal_year ? _journal_volume ? _journal_page_first ? _publ_contact_author_name 'Alexandr Piskunov' _publ_contact_author_email pial@iomc.ras.ru loop_ _publ_author_name A.Piskunov O.Trofimova G.Fukin S.Ketkov I.Smolyaninov V.Cherkasov # Attachment '- copmlex1.cif' data_snoonnm _database_code_depnum_ccdc_archive 'CCDC 872115' #TrackingRef '- copmlex1.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H50 Cl2 N2 O2 Sn' _chemical_formula_weight 696.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.9657(4) _cell_length_b 18.2113(6) _cell_length_c 17.0576(6) _cell_angle_alpha 90.00 _cell_angle_beta 98.1810(10) _cell_angle_gamma 90.00 _cell_volume 3371.7(2) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 900 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.05 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.372 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1448 _exptl_absorpt_coefficient_mu 0.947 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8332 _exptl_absorpt_correction_T_max 0.9631 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 28608 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0419 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.18 _diffrn_reflns_theta_max 26.00 _reflns_number_total 6605 _reflns_number_gt 5073 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0385P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 6605 _refine_ls_number_parameters 375 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0523 _refine_ls_R_factor_gt 0.0321 _refine_ls_wR_factor_ref 0.0725 _refine_ls_wR_factor_gt 0.0674 _refine_ls_goodness_of_fit_ref 1.000 _refine_ls_restrained_S_all 1.000 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn -0.276050(14) 0.115130(9) 0.558430(9) 0.01686(4) Uani 1 1 d . . . O1 O -0.19049(14) 0.01360(9) 0.61836(10) 0.0228(4) Uani 1 1 d . . . O2 O -0.24153(15) 0.22543(9) 0.50432(10) 0.0233(4) Uani 1 1 d . . . N1 N -0.42721(17) 0.04391(10) 0.59520(11) 0.0175(4) Uani 1 1 d . . . N2 N -0.45881(17) 0.16369(10) 0.50676(11) 0.0174(4) Uani 1 1 d . . . C1 C -0.2596(2) -0.02473(13) 0.65839(14) 0.0188(5) Uani 1 1 d . . . C2 C -0.3893(2) -0.01201(12) 0.64824(14) 0.0174(5) Uani 1 1 d . . . C3 C -0.4692(2) -0.05142(12) 0.69074(13) 0.0180(5) Uani 1 1 d . . . H3A H -0.5554 -0.0425 0.6810 0.022 Uiso 1 1 calc R . . C4 C -0.4229(2) -0.10261(12) 0.74602(14) 0.0175(5) Uani 1 1 d . . . C5 C -0.2934(2) -0.11557(13) 0.75599(13) 0.0179(5) Uani 1 1 d . . . H5A H -0.2609 -0.1512 0.7941 0.021 Uiso 1 1 calc R . . C6 C -0.2122(2) -0.08033(13) 0.71451(14) 0.0176(5) Uani 1 1 d . . . C7 C -0.5020(2) -0.14289(13) 0.79992(14) 0.0186(5) Uani 1 1 d . . . C8 C -0.4648(2) -0.11593(14) 0.88546(14) 0.0243(6) Uani 1 1 d . . . H8A H -0.4778 -0.0628 0.8878 0.036 Uiso 1 1 calc R . . H8B H -0.3777 -0.1271 0.9027 0.036 Uiso 1 1 calc R . . H8C H -0.5153 -0.1408 0.9204 0.036 Uiso 1 1 calc R . . C9 C -0.4811(2) -0.22605(12) 0.79668(15) 0.0221(6) Uani 1 1 d . . . H9A H -0.5070 -0.2437 0.7426 0.033 Uiso 1 1 calc R . . H9B H -0.5295 -0.2508 0.8330 0.033 Uiso 1 1 calc R . . H9C H -0.3935 -0.2368 0.8124 0.033 Uiso 1 1 calc R . . C10 C -0.6401(2) -0.12792(13) 0.77597(16) 0.0248(6) Uani 1 1 d . . . H10A H -0.6662 -0.1465 0.7223 0.037 Uiso 1 1 calc R . . H10B H -0.6553 -0.0749 0.7773 0.037 Uiso 1 1 calc R . . H10C H -0.6869 -0.1528 0.8130 0.037 Uiso 1 1 calc R . . C11 C -0.0749(2) -0.09914(13) 0.72456(14) 0.0200(6) Uani 1 1 d . . . C12 C 0.0055(2) -0.03132(13) 0.74914(16) 0.0275(6) Uani 1 1 d . . . H12A H -0.0112 -0.0137 0.8009 0.041 Uiso 1 1 calc R . . H12B H -0.0137 0.0076 0.7096 0.041 Uiso 1 1 calc R . . H12C H 0.0927 -0.0447 0.7526 0.041 Uiso 1 1 calc R . . C13 C -0.0439(2) -0.12916(14) 0.64495(15) 0.0251(6) Uani 1 1 d . . . H13A H -0.0943 -0.1727 0.6297 0.038 Uiso 1 1 calc R . . H13B H 0.0435 -0.1425 0.6508 0.038 Uiso 1 1 calc R . . H13C H -0.0612 -0.0914 0.6040 0.038 Uiso 1 1 calc R . . C14 C -0.0395(2) -0.15857(13) 0.78744(14) 0.0234(6) Uani 1 1 d . . . H14A H -0.0846 -0.2039 0.7716 0.035 Uiso 1 1 calc R . . H14B H -0.0605 -0.1418 0.8385 0.035 Uiso 1 1 calc R . . H14C H 0.0493 -0.1680 0.7924 0.035 Uiso 1 1 calc R . . C15 C -0.5393(2) 0.06549(13) 0.57111(14) 0.0197(5) Uani 1 1 d . . . H15A H -0.6078 0.0401 0.5865 0.024 Uiso 1 1 calc R . . C16 C -0.5566(2) 0.12809(12) 0.52121(14) 0.0210(6) Uani 1 1 d . . . H16A H -0.6368 0.1436 0.4990 0.025 Uiso 1 1 calc R . . C17 C -0.3377(2) 0.26052(13) 0.46853(14) 0.0186(5) Uani 1 1 d . . . C18 C -0.4569(2) 0.22876(12) 0.46460(14) 0.0178(5) Uani 1 1 d . . . C19 C -0.5628(2) 0.26244(12) 0.42415(13) 0.0168(5) Uani 1 1 d . . . H19A H -0.6401 0.2382 0.4204 0.020 Uiso 1 1 calc R . . C20 C -0.5552(2) 0.33021(13) 0.39009(14) 0.0179(5) Uani 1 1 d . . . C21 C -0.4374(2) 0.36331(13) 0.39722(14) 0.0196(5) Uani 1 1 d . . . H21A H -0.4321 0.4108 0.3749 0.023 Uiso 1 1 calc R . . C22 C -0.3299(2) 0.33217(13) 0.43402(13) 0.0172(5) Uani 1 1 d . . . C23 C -0.6682(2) 0.37149(12) 0.34760(14) 0.0190(5) Uani 1 1 d . . . C24 C -0.7791(2) 0.32043(14) 0.32625(16) 0.0250(6) Uani 1 1 d . . . H24A H -0.8475 0.3481 0.2968 0.038 Uiso 1 1 calc R . . H24B H -0.8045 0.3006 0.3749 0.038 Uiso 1 1 calc R . . H24C H -0.7562 0.2799 0.2934 0.038 Uiso 1 1 calc R . . C25 C -0.7032(2) 0.43177(14) 0.40316(16) 0.0272(6) Uani 1 1 d . . . H25A H -0.6327 0.4645 0.4177 0.041 Uiso 1 1 calc R . . H25B H -0.7264 0.4092 0.4511 0.041 Uiso 1 1 calc R . . H25C H -0.7729 0.4600 0.3762 0.041 Uiso 1 1 calc R . . C26 C -0.6392(2) 0.40674(14) 0.27077(14) 0.0251(6) Uani 1 1 d . . . H26A H -0.5705 0.4412 0.2830 0.038 Uiso 1 1 calc R . . H26B H -0.7120 0.4331 0.2451 0.038 Uiso 1 1 calc R . . H26C H -0.6166 0.3684 0.2352 0.038 Uiso 1 1 calc R . . C27 C -0.2051(2) 0.37162(13) 0.43870(15) 0.0216(6) Uani 1 1 d . . . C28 C -0.2166(2) 0.44776(14) 0.40068(17) 0.0297(7) Uani 1 1 d . . . H28A H -0.2496 0.4431 0.3444 0.045 Uiso 1 1 calc R . . H28B H -0.1353 0.4710 0.4060 0.045 Uiso 1 1 calc R . . H28C H -0.2724 0.4780 0.4272 0.045 Uiso 1 1 calc R . . C29 C -0.1165(2) 0.32630(15) 0.39668(15) 0.0279(6) Uani 1 1 d . . . H29A H -0.1478 0.3237 0.3400 0.042 Uiso 1 1 calc R . . H29B H -0.1100 0.2766 0.4189 0.042 Uiso 1 1 calc R . . H29C H -0.0351 0.3496 0.4041 0.042 Uiso 1 1 calc R . . C30 C -0.1509(2) 0.38188(14) 0.52647(15) 0.0274(6) Uani 1 1 d . . . H30A H -0.1392 0.3337 0.5521 0.041 Uiso 1 1 calc R . . H30B H -0.2076 0.4113 0.5531 0.041 Uiso 1 1 calc R . . H30C H -0.0714 0.4071 0.5300 0.041 Uiso 1 1 calc R . . C31 C -0.2118(2) 0.07018(15) 0.45751(14) 0.0263(6) Uani 1 1 d . . . H31A H -0.2163 0.0165 0.4595 0.040 Uiso 1 1 calc R . . H31B H -0.1262 0.0853 0.4567 0.040 Uiso 1 1 calc R . . H31C H -0.2632 0.0880 0.4095 0.040 Uiso 1 1 calc R . . C32 C -0.2226(2) 0.16673(14) 0.66958(15) 0.0267(6) Uani 1 1 d . . . H32A H -0.2688 0.1452 0.7091 0.040 Uiso 1 1 calc R . . H32B H -0.2402 0.2194 0.6648 0.040 Uiso 1 1 calc R . . H32C H -0.1342 0.1593 0.6862 0.040 Uiso 1 1 calc R . . C1S C 0.0513(2) 0.20591(14) 0.55813(18) 0.0319(7) Uani 1 1 d . . . H1SA H 0.0047 0.2316 0.5956 0.038 Uiso 1 1 calc R . . H1SB H -0.0031 0.2016 0.5068 0.038 Uiso 1 1 calc R . . Cl1S Cl 0.18178(7) 0.25853(4) 0.54493(4) 0.03659(17) Uani 1 1 d . . . Cl2S Cl 0.09032(7) 0.11787(4) 0.59444(5) 0.0458(2) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.01426(8) 0.01778(8) 0.01861(8) 0.00291(7) 0.00260(6) 0.00010(7) O1 0.0167(8) 0.0240(9) 0.0289(9) 0.0097(7) 0.0078(7) 0.0022(7) O2 0.0163(9) 0.0210(9) 0.0311(10) 0.0071(7) -0.0015(8) -0.0005(7) N1 0.0149(10) 0.0183(10) 0.0193(10) 0.0004(8) 0.0026(8) -0.0003(8) N2 0.0169(10) 0.0170(10) 0.0185(10) 0.0022(8) 0.0033(8) 0.0009(8) C1 0.0182(12) 0.0195(12) 0.0190(12) -0.0028(10) 0.0032(10) -0.0012(10) C2 0.0176(12) 0.0164(11) 0.0181(12) 0.0013(9) 0.0017(10) 0.0015(10) C3 0.0153(12) 0.0193(12) 0.0195(12) -0.0018(10) 0.0034(10) -0.0010(10) C4 0.0178(12) 0.0161(12) 0.0194(12) 0.0006(9) 0.0050(10) 0.0010(9) C5 0.0187(11) 0.0172(11) 0.0172(11) 0.0033(10) 0.0008(9) 0.0015(10) C6 0.0150(12) 0.0196(12) 0.0179(12) 0.0001(10) 0.0015(10) -0.0002(10) C7 0.0172(12) 0.0191(11) 0.0203(12) 0.0033(10) 0.0057(10) 0.0011(10) C8 0.0278(13) 0.0254(13) 0.0208(12) -0.0005(11) 0.0076(10) -0.0010(11) C9 0.0227(13) 0.0179(12) 0.0266(13) 0.0021(10) 0.0063(11) -0.0007(10) C10 0.0179(12) 0.0253(14) 0.0322(14) 0.0106(11) 0.0067(11) -0.0003(10) C11 0.0159(12) 0.0217(13) 0.0224(13) 0.0034(10) 0.0026(10) 0.0012(10) C12 0.0193(13) 0.0261(13) 0.0360(16) 0.0021(12) 0.0002(12) -0.0020(11) C13 0.0218(13) 0.0295(15) 0.0255(13) 0.0049(11) 0.0089(11) 0.0028(11) C14 0.0157(12) 0.0266(13) 0.0271(14) 0.0050(11) 0.0008(11) 0.0020(11) C15 0.0165(12) 0.0198(12) 0.0231(13) 0.0016(10) 0.0039(10) -0.0011(10) C16 0.0167(12) 0.0216(13) 0.0241(13) 0.0030(10) 0.0009(10) 0.0008(10) C17 0.0199(12) 0.0207(12) 0.0152(12) 0.0009(10) 0.0029(10) 0.0024(10) C18 0.0192(12) 0.0156(11) 0.0187(12) 0.0013(9) 0.0026(10) -0.0003(10) C19 0.0152(12) 0.0159(11) 0.0197(12) 0.0003(9) 0.0040(10) 0.0000(9) C20 0.0178(12) 0.0197(12) 0.0160(12) 0.0005(9) 0.0016(10) 0.0036(10) C21 0.0232(13) 0.0173(12) 0.0183(12) 0.0004(9) 0.0032(10) -0.0007(10) C22 0.0166(12) 0.0181(12) 0.0173(12) -0.0008(9) 0.0040(9) -0.0026(9) C23 0.0183(12) 0.0177(12) 0.0199(12) 0.0018(9) -0.0006(10) 0.0014(9) C24 0.0176(13) 0.0255(13) 0.0307(14) 0.0052(11) -0.0011(11) 0.0011(11) C25 0.0253(14) 0.0264(14) 0.0302(15) -0.0021(12) 0.0049(12) 0.0071(11) C26 0.0267(14) 0.0246(13) 0.0230(13) 0.0067(10) -0.0004(11) 0.0005(11) C27 0.0169(13) 0.0222(13) 0.0253(13) 0.0061(10) 0.0014(10) -0.0031(10) C28 0.0195(13) 0.0307(14) 0.0384(16) 0.0097(13) 0.0024(12) -0.0053(11) C29 0.0208(13) 0.0366(15) 0.0275(14) 0.0104(12) 0.0077(11) 0.0050(12) C30 0.0247(13) 0.0256(13) 0.0293(14) 0.0010(12) -0.0044(11) -0.0042(12) C31 0.0233(14) 0.0359(15) 0.0205(14) -0.0012(11) 0.0058(11) -0.0066(12) C32 0.0252(14) 0.0300(14) 0.0242(14) -0.0031(11) 0.0009(11) 0.0001(11) C1S 0.0253(14) 0.0263(14) 0.0424(17) -0.0034(13) -0.0007(13) -0.0002(12) Cl1S 0.0304(4) 0.0407(4) 0.0404(4) -0.0075(3) 0.0113(3) -0.0080(3) Cl2S 0.0462(4) 0.0383(4) 0.0518(5) 0.0142(4) 0.0028(4) 0.0048(4) _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 Sn1 C31 2.115(2) . ? Sn1 C32 2.122(2) . ? Sn1 O1 2.2518(16) . ? Sn1 N2 2.2523(19) . ? Sn1 N1 2.2626(19) . ? Sn1 O2 2.2649(16) . ? O1 C1 1.295(3) . ? O2 C17 1.308(3) . ? N1 C15 1.301(3) . ? N1 C2 1.386(3) . ? N2 C16 1.306(3) . ? N2 C18 1.388(3) . ? C1 C2 1.426(3) . ? C1 C6 1.439(3) . ? C2 C3 1.410(3) . ? C3 C4 1.371(3) . ? C4 C5 1.426(3) . ? C4 C7 1.537(3) . ? C5 C6 1.372(3) . ? C6 C11 1.530(3) . ? C7 C9 1.534(3) . ? C7 C10 1.535(3) . ? C7 C8 1.539(3) . ? C11 C14 1.534(3) . ? C11 C12 1.541(3) . ? C11 C13 1.546(3) . ? C15 C16 1.419(3) . ? C17 C18 1.422(3) . ? C17 C22 1.439(3) . ? C18 C19 1.405(3) . ? C19 C20 1.372(3) . ? C20 C21 1.415(3) . ? C20 C23 1.539(3) . ? C21 C22 1.377(3) . ? C22 C27 1.537(3) . ? C23 C26 1.533(3) . ? C23 C24 1.533(3) . ? C23 C25 1.534(3) . ? C27 C29 1.528(4) . ? C27 C28 1.528(3) . ? C27 C30 1.542(3) . ? C1S Cl2S 1.750(3) . ? C1S Cl1S 1.763(3) . ? 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 C31 Sn1 C32 144.75(10) . . ? C31 Sn1 O1 83.47(8) . . ? C32 Sn1 O1 85.05(8) . . ? C31 Sn1 N2 102.37(8) . . ? C32 Sn1 N2 107.03(9) . . ? O1 Sn1 N2 142.20(6) . . ? C31 Sn1 N1 110.22(9) . . ? C32 Sn1 N1 97.26(9) . . ? O1 Sn1 N1 71.20(6) . . ? N2 Sn1 N1 71.78(7) . . ? C31 Sn1 O2 85.25(9) . . ? C32 Sn1 O2 86.01(8) . . ? O1 Sn1 O2 146.12(6) . . ? N2 Sn1 O2 71.53(6) . . ? N1 Sn1 O2 142.46(6) . . ? C1 O1 Sn1 116.40(14) . . ? C17 O2 Sn1 116.94(14) . . ? C15 N1 C2 127.6(2) . . ? C15 N1 Sn1 115.86(16) . . ? C2 N1 Sn1 116.01(15) . . ? C16 N2 C18 126.5(2) . . ? C16 N2 Sn1 116.10(15) . . ? C18 N2 Sn1 117.39(15) . . ? O1 C1 C2 119.8(2) . . ? O1 C1 C6 123.2(2) . . ? C2 C1 C6 117.0(2) . . ? N1 C2 C3 124.0(2) . . ? N1 C2 C1 113.6(2) . . ? C3 C2 C1 122.4(2) . . ? C4 C3 C2 120.2(2) . . ? C3 C4 C5 117.4(2) . . ? C3 C4 C7 123.4(2) . . ? C5 C4 C7 119.1(2) . . ? C6 C5 C4 124.7(2) . . ? C5 C6 C1 118.2(2) . . ? C5 C6 C11 122.5(2) . . ? C1 C6 C11 119.3(2) . . ? C9 C7 C10 108.2(2) . . ? C9 C7 C4 110.47(19) . . ? C10 C7 C4 112.03(19) . . ? C9 C7 C8 109.2(2) . . ? C10 C7 C8 108.3(2) . . ? C4 C7 C8 108.59(19) . . ? C6 C11 C14 112.5(2) . . ? C6 C11 C12 111.54(19) . . ? C14 C11 C12 107.3(2) . . ? C6 C11 C13 108.49(19) . . ? C14 C11 C13 107.41(19) . . ? C12 C11 C13 109.5(2) . . ? N1 C15 C16 118.1(2) . . ? N2 C16 C15 118.0(2) . . ? O2 C17 C18 119.9(2) . . ? O2 C17 C22 122.9(2) . . ? C18 C17 C22 117.2(2) . . ? N2 C18 C19 123.7(2) . . ? N2 C18 C17 113.8(2) . . ? C19 C18 C17 122.4(2) . . ? C20 C19 C18 120.4(2) . . ? C19 C20 C21 117.2(2) . . ? C19 C20 C23 123.1(2) . . ? C21 C20 C23 119.7(2) . . ? C22 C21 C20 125.2(2) . . ? C21 C22 C17 117.5(2) . . ? C21 C22 C27 122.0(2) . . ? C17 C22 C27 120.5(2) . . ? C26 C23 C24 107.8(2) . . ? C26 C23 C25 109.2(2) . . ? C24 C23 C25 108.7(2) . . ? C26 C23 C20 110.9(2) . . ? C24 C23 C20 111.94(19) . . ? C25 C23 C20 108.29(19) . . ? C29 C27 C28 108.1(2) . . ? C29 C27 C22 110.1(2) . . ? C28 C27 C22 112.5(2) . . ? C29 C27 C30 109.8(2) . . ? C28 C27 C30 107.4(2) . . ? C22 C27 C30 108.9(2) . . ? Cl2S C1S Cl1S 112.40(15) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.848 _refine_diff_density_min -0.520 _refine_diff_density_rms 0.081 _publ_section_references ; Bruker (2003) SAINTPlus Data Reduction and Correction Program v. 6.45a, Bruker AXS, Madison, Wisconsin, USA. Bruker (2005) SMART. Bruker Molecular Analysis Research Tool, v. 5.632 Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (1998a). SADABS v.2.01, Bruker/Siemens Area Detector Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (2000). SHELXTL v. 6.12, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. ; data_snoonn1m _database_code_depnum_ccdc_archive 'CCDC 872116' #TrackingRef '- complex3.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H60 N2 O2 Sn' _chemical_formula_weight 695.57 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c 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 16.2139(5) _cell_length_b 25.7750(8) _cell_length_c 18.4703(5) _cell_angle_alpha 90.00 _cell_angle_beta 103.8960(10) _cell_angle_gamma 90.00 _cell_volume 7493.1(4) _cell_formula_units_Z 8 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 950 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _exptl_crystal_description prism _exptl_crystal_colour green _exptl_crystal_size_max 0.65 _exptl_crystal_size_mid 0.60 _exptl_crystal_size_min 0.41 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.233 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2944 _exptl_absorpt_coefficient_mu 0.714 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6539 _exptl_absorpt_correction_T_max 0.7584 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 48606 _diffrn_reflns_av_R_equivalents 0.0195 _diffrn_reflns_av_sigmaI/netI 0.0217 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 20 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 28 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.58 _diffrn_reflns_theta_max 27.00 _reflns_number_total 16333 _reflns_number_gt 14129 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0384P)^2^+3.3118P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patt _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 16333 _refine_ls_number_parameters 811 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0362 _refine_ls_R_factor_gt 0.0284 _refine_ls_wR_factor_ref 0.0711 _refine_ls_wR_factor_gt 0.0680 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1A Sn 0.093476(7) 0.380741(4) 0.254574(6) 0.01478(4) Uani 1 1 d . . . O1A O -0.01528(7) 0.43276(5) 0.20055(7) 0.0187(3) Uani 1 1 d . . . O2A O 0.23676(8) 0.37211(5) 0.28796(7) 0.0183(3) Uani 1 1 d . . . N1A N -0.02941(9) 0.33764(6) 0.25087(8) 0.0170(3) Uani 1 1 d . . . N2A N 0.12530(9) 0.30364(6) 0.31322(8) 0.0167(3) Uani 1 1 d . . . C1A C -0.09146(11) 0.41311(7) 0.18794(10) 0.0180(4) Uani 1 1 d . . . C2A C -0.10367(11) 0.36218(7) 0.21472(10) 0.0167(3) Uani 1 1 d . . . C3A C -0.18510(11) 0.33999(7) 0.20367(10) 0.0184(3) Uani 1 1 d . . . H3AA H -0.1910 0.3061 0.2221 0.022 Uiso 1 1 calc R . . C4A C -0.25592(11) 0.36645(7) 0.16672(9) 0.0172(3) Uani 1 1 d . . . C5A C -0.24343(11) 0.41645(7) 0.13886(10) 0.0192(4) Uani 1 1 d . . . H5AA H -0.2922 0.4346 0.1118 0.023 Uiso 1 1 calc R . . C6A C -0.16532(11) 0.44069(7) 0.14825(10) 0.0177(3) Uani 1 1 d . . . C7A C -0.34452(11) 0.34202(7) 0.15248(10) 0.0186(4) Uani 1 1 d . . . C8A C -0.35466(12) 0.30418(8) 0.08653(11) 0.0258(4) Uani 1 1 d . . . H8AA H -0.3449 0.3227 0.0430 0.039 Uiso 1 1 calc R . . H8AB H -0.4123 0.2897 0.0746 0.039 Uiso 1 1 calc R . . H8AC H -0.3132 0.2760 0.1000 0.039 Uiso 1 1 calc R . . C9A C -0.41501(11) 0.38285(7) 0.13405(11) 0.0221(4) Uani 1 1 d . . . H9AA H -0.4056 0.4090 0.1737 0.033 Uiso 1 1 calc R . . H9AB H -0.4702 0.3661 0.1302 0.033 Uiso 1 1 calc R . . H9AC H -0.4144 0.3995 0.0865 0.033 Uiso 1 1 calc R . . C10A C -0.35561(12) 0.31140(8) 0.22102(11) 0.0251(4) Uani 1 1 d . . . H10A H -0.3478 0.3348 0.2640 0.038 Uiso 1 1 calc R . . H10B H -0.3133 0.2836 0.2321 0.038 Uiso 1 1 calc R . . H10C H -0.4128 0.2964 0.2106 0.038 Uiso 1 1 calc R . . C11A C -0.15654(11) 0.49587(7) 0.11935(10) 0.0216(4) Uani 1 1 d . . . C12A C -0.09378(13) 0.49726(8) 0.06901(11) 0.0282(4) Uani 1 1 d . . . H12A H -0.0373 0.4869 0.0979 0.042 Uiso 1 1 calc R . . H12B H -0.0912 0.5325 0.0498 0.042 Uiso 1 1 calc R . . H12C H -0.1128 0.4733 0.0272 0.042 Uiso 1 1 calc R . . C13A C -0.12595(13) 0.53213(8) 0.18624(12) 0.0290(4) Uani 1 1 d . . . H13A H -0.0709 0.5200 0.2161 0.044 Uiso 1 1 calc R . . H13B H -0.1675 0.5321 0.2170 0.044 Uiso 1 1 calc R . . H13C H -0.1199 0.5674 0.1684 0.044 Uiso 1 1 calc R . . C14A C -0.24171(13) 0.51668(8) 0.07313(13) 0.0347(5) Uani 1 1 d . . . H14A H -0.2643 0.4929 0.0317 0.052 Uiso 1 1 calc R . . H14B H -0.2331 0.5510 0.0533 0.052 Uiso 1 1 calc R . . H14C H -0.2821 0.5194 0.1049 0.052 Uiso 1 1 calc R . . C15A C -0.02247(11) 0.29206(7) 0.28150(10) 0.0190(4) Uani 1 1 d . . . H15A H -0.0712 0.2714 0.2807 0.023 Uiso 1 1 calc R . . C16A C 0.06092(11) 0.27402(7) 0.31640(10) 0.0188(4) Uani 1 1 d . . . H16A H 0.0693 0.2415 0.3412 0.023 Uiso 1 1 calc R . . C17A C 0.26649(11) 0.33264(7) 0.32926(9) 0.0156(3) Uani 1 1 d . . . C18A C 0.21026(11) 0.29395(7) 0.34492(10) 0.0170(3) Uani 1 1 d . . . C19A C 0.23959(11) 0.25156(7) 0.39191(10) 0.0181(3) Uani 1 1 d . . . H19A H 0.2003 0.2263 0.4006 0.022 Uiso 1 1 calc R . . C20A C 0.32426(11) 0.24623(7) 0.42537(10) 0.0170(3) Uani 1 1 d . . . C21A C 0.38080(11) 0.28421(7) 0.40871(9) 0.0170(3) Uani 1 1 d . . . H21A H 0.4396 0.2806 0.4316 0.020 Uiso 1 1 calc R . . C22A C 0.35614(11) 0.32595(7) 0.36164(9) 0.0158(3) Uani 1 1 d . . . C23A C 0.35790(11) 0.20293(7) 0.48163(10) 0.0198(4) Uani 1 1 d . . . C24A C 0.28924(13) 0.16322(8) 0.48550(13) 0.0340(5) Uani 1 1 d . . . H24A H 0.2672 0.1479 0.4361 0.051 Uiso 1 1 calc R . . H24B H 0.2429 0.1804 0.5018 0.051 Uiso 1 1 calc R . . H24C H 0.3136 0.1359 0.5211 0.051 Uiso 1 1 calc R . . C25A C 0.39032(14) 0.22742(8) 0.55931(10) 0.0281(4) Uani 1 1 d . . . H25A H 0.4117 0.2001 0.5959 0.042 Uiso 1 1 calc R . . H25B H 0.3437 0.2458 0.5734 0.042 Uiso 1 1 calc R . . H25C H 0.4362 0.2519 0.5581 0.042 Uiso 1 1 calc R . . C26A C 0.43025(13) 0.17370(8) 0.45935(11) 0.0259(4) Uani 1 1 d . . . H26A H 0.4089 0.1576 0.4103 0.039 Uiso 1 1 calc R . . H26B H 0.4521 0.1467 0.4964 0.039 Uiso 1 1 calc R . . H26C H 0.4760 0.1980 0.4571 0.039 Uiso 1 1 calc R . . C27A C 0.41933(11) 0.36467(7) 0.34183(10) 0.0174(3) Uani 1 1 d . . . C28A C 0.40110(12) 0.42062(7) 0.36335(11) 0.0212(4) Uani 1 1 d . . . H28A H 0.4026 0.4220 0.4167 0.032 Uiso 1 1 calc R . . H28B H 0.3448 0.4313 0.3344 0.032 Uiso 1 1 calc R . . H28C H 0.4443 0.4440 0.3527 0.032 Uiso 1 1 calc R . . C29A C 0.41276(12) 0.36157(8) 0.25737(10) 0.0221(4) Uani 1 1 d . . . H29A H 0.4246 0.3260 0.2440 0.033 Uiso 1 1 calc R . . H29B H 0.4542 0.3852 0.2443 0.033 Uiso 1 1 calc R . . H29C H 0.3553 0.3715 0.2301 0.033 Uiso 1 1 calc R . . C30A C 0.51150(11) 0.35267(7) 0.38189(10) 0.0203(4) Uani 1 1 d . . . H30A H 0.5269 0.3181 0.3672 0.030 Uiso 1 1 calc R . . H30B H 0.5174 0.3535 0.4359 0.030 Uiso 1 1 calc R . . H30C H 0.5492 0.3787 0.3682 0.030 Uiso 1 1 calc R . . C31A C 0.10950(12) 0.36364(7) 0.14210(10) 0.0210(4) Uani 1 1 d . . . C32A C 0.02361(14) 0.35604(11) 0.08690(12) 0.0381(5) Uani 1 1 d . . . H32A H 0.0326 0.3461 0.0382 0.057 Uiso 1 1 calc R . . H32B H -0.0087 0.3885 0.0821 0.057 Uiso 1 1 calc R . . H32C H -0.0081 0.3286 0.1051 0.057 Uiso 1 1 calc R . . C33A C 0.15657(14) 0.40902(8) 0.11750(11) 0.0286(4) Uani 1 1 d . . . H33A H 0.1646 0.4022 0.0675 0.043 Uiso 1 1 calc R . . H33B H 0.2121 0.4132 0.1526 0.043 Uiso 1 1 calc R . . H33C H 0.1233 0.4408 0.1167 0.043 Uiso 1 1 calc R . . C34A C 0.16130(15) 0.31387(8) 0.14524(11) 0.0312(5) Uani 1 1 d . . . H34A H 0.1678 0.3054 0.0952 0.047 Uiso 1 1 calc R . . H34B H 0.1319 0.2854 0.1637 0.047 Uiso 1 1 calc R . . H34C H 0.2175 0.3188 0.1789 0.047 Uiso 1 1 calc R . . C35A C 0.10612(11) 0.43076(7) 0.35316(10) 0.0181(4) Uani 1 1 d . . . C36A C 0.17291(12) 0.41011(8) 0.41981(10) 0.0227(4) Uani 1 1 d . . . H36A H 0.1719 0.4308 0.4641 0.034 Uiso 1 1 calc R . . H36B H 0.2293 0.4125 0.4093 0.034 Uiso 1 1 calc R . . H36C H 0.1604 0.3738 0.4287 0.034 Uiso 1 1 calc R . . C37A C 0.13195(13) 0.48465(7) 0.33181(11) 0.0256(4) Uani 1 1 d . . . H37A H 0.1361 0.5084 0.3740 0.038 Uiso 1 1 calc R . . H37B H 0.0891 0.4976 0.2887 0.038 Uiso 1 1 calc R . . H37C H 0.1871 0.4825 0.3191 0.038 Uiso 1 1 calc R . . C38A C 0.02033(12) 0.43354(8) 0.37366(11) 0.0262(4) Uani 1 1 d . . . H38A H 0.0251 0.4562 0.4171 0.039 Uiso 1 1 calc R . . H38B H 0.0034 0.3987 0.3857 0.039 Uiso 1 1 calc R . . H38C H -0.0225 0.4475 0.3314 0.039 Uiso 1 1 calc R . . Sn1B Sn 0.521621(7) 0.097626(4) 0.244359(6) 0.01478(4) Uani 1 1 d . . . O1B O 0.41210(8) 0.04549(5) 0.19137(7) 0.0170(2) Uani 1 1 d . . . O2B O 0.66532(8) 0.10546(5) 0.27463(7) 0.0169(2) Uani 1 1 d . . . N1B N 0.39934(9) 0.14135(6) 0.24050(8) 0.0164(3) Uani 1 1 d . . . N2B N 0.55546(9) 0.17514(6) 0.30123(8) 0.0166(3) Uani 1 1 d . . . C1B C 0.33631(11) 0.06546(7) 0.17904(9) 0.0166(3) Uani 1 1 d . . . C2B C 0.32446(11) 0.11681(7) 0.20448(10) 0.0165(3) Uani 1 1 d . . . C3B C 0.24412(11) 0.14042(7) 0.19027(10) 0.0188(4) Uani 1 1 d . . . H3BA H 0.2388 0.1748 0.2072 0.023 Uiso 1 1 calc R . . C4B C 0.17291(11) 0.11416(7) 0.15201(10) 0.0174(3) Uani 1 1 d . . . C5B C 0.18446(11) 0.06336(7) 0.12739(9) 0.0174(3) Uani 1 1 d . . . H5BA H 0.1355 0.0451 0.1011 0.021 Uiso 1 1 calc R . . C6B C 0.26202(11) 0.03835(7) 0.13893(9) 0.0157(3) Uani 1 1 d . . . C7B C 0.08577(11) 0.14075(7) 0.13240(10) 0.0204(4) Uani 1 1 d . . . C8B C 0.07067(12) 0.17094(8) 0.20013(11) 0.0258(4) Uani 1 1 d . . . H8BA H 0.0708 0.1467 0.2411 0.039 Uiso 1 1 calc R . . H8BB H 0.0157 0.1887 0.1861 0.039 Uiso 1 1 calc R . . H8BC H 0.1160 0.1966 0.2162 0.039 Uiso 1 1 calc R . . C9B C 0.08366(12) 0.17897(8) 0.06783(11) 0.0263(4) Uani 1 1 d . . . H9BA H 0.1302 0.2040 0.0826 0.039 Uiso 1 1 calc R . . H9BB H 0.0293 0.1975 0.0561 0.039 Uiso 1 1 calc R . . H9BC H 0.0902 0.1598 0.0238 0.039 Uiso 1 1 calc R . . C10B C 0.01254(12) 0.10198(8) 0.10818(13) 0.0294(5) Uani 1 1 d . . . H10D H 0.0153 0.0761 0.1475 0.044 Uiso 1 1 calc R . . H10E H 0.0173 0.0847 0.0621 0.044 Uiso 1 1 calc R . . H10F H -0.0418 0.1205 0.0994 0.044 Uiso 1 1 calc R . . C11B C 0.26979(11) -0.01675(7) 0.10999(10) 0.0176(3) Uani 1 1 d . . . C12B C 0.32840(12) -0.01755(7) 0.05566(10) 0.0216(4) Uani 1 1 d . . . H12D H 0.3849 -0.0050 0.0813 0.032 Uiso 1 1 calc R . . H12E H 0.3047 0.0049 0.0129 0.032 Uiso 1 1 calc R . . H12F H 0.3329 -0.0531 0.0382 0.032 Uiso 1 1 calc R . . C13B C 0.30560(13) -0.05301(7) 0.17631(11) 0.0236(4) Uani 1 1 d . . . H13D H 0.3626 -0.0413 0.2022 0.035 Uiso 1 1 calc R . . H13E H 0.3088 -0.0885 0.1580 0.035 Uiso 1 1 calc R . . H13F H 0.2683 -0.0523 0.2109 0.035 Uiso 1 1 calc R . . C14B C 0.18346(12) -0.03885(7) 0.06827(11) 0.0235(4) Uani 1 1 d . . . H14D H 0.1581 -0.0161 0.0264 0.035 Uiso 1 1 calc R . . H14E H 0.1457 -0.0410 0.1024 0.035 Uiso 1 1 calc R . . H14F H 0.1915 -0.0736 0.0494 0.035 Uiso 1 1 calc R . . C15B C 0.40804(11) 0.18844(7) 0.26639(10) 0.0191(4) Uani 1 1 d . . . H15B H 0.3600 0.2102 0.2632 0.023 Uiso 1 1 calc R . . C16B C 0.49194(11) 0.20650(7) 0.29981(10) 0.0184(4) Uani 1 1 d . . . H16B H 0.5012 0.2404 0.3204 0.022 Uiso 1 1 calc R . . C17B C 0.69616(11) 0.14647(7) 0.31386(10) 0.0169(3) Uani 1 1 d . . . C18B C 0.64093(11) 0.18486(7) 0.33204(9) 0.0165(3) Uani 1 1 d . . . C19B C 0.67160(11) 0.22740(7) 0.37834(9) 0.0165(3) Uani 1 1 d . . . H19B H 0.6327 0.2515 0.3905 0.020 Uiso 1 1 calc R . . C20B C 0.75727(11) 0.23434(7) 0.40606(10) 0.0173(3) Uani 1 1 d . . . C21B C 0.81255(11) 0.19774(7) 0.38452(10) 0.0188(4) Uani 1 1 d . . . H21B H 0.8720 0.2031 0.4021 0.023 Uiso 1 1 calc R . . C22B C 0.78634(11) 0.15513(7) 0.34014(10) 0.0182(3) Uani 1 1 d . . . C23B C 0.79611(11) 0.27833(7) 0.45919(10) 0.0176(3) Uani 1 1 d . . . C24B C 0.72809(11) 0.31373(7) 0.47756(10) 0.0217(4) Uani 1 1 d . . . H24D H 0.6904 0.2932 0.5006 0.033 Uiso 1 1 calc R . . H24E H 0.6949 0.3297 0.4316 0.033 Uiso 1 1 calc R . . H24F H 0.7555 0.3409 0.5122 0.033 Uiso 1 1 calc R . . C25B C 0.85449(12) 0.31168(7) 0.42336(11) 0.0225(4) Uani 1 1 d . . . H25D H 0.8216 0.3259 0.3760 0.034 Uiso 1 1 calc R . . H25E H 0.9008 0.2902 0.4143 0.034 Uiso 1 1 calc R . . H25F H 0.8782 0.3402 0.4570 0.034 Uiso 1 1 calc R . . C26B C 0.84934(12) 0.25491(7) 0.53235(10) 0.0226(4) Uani 1 1 d . . . H26D H 0.8137 0.2316 0.5538 0.034 Uiso 1 1 calc R . . H26E H 0.8711 0.2829 0.5677 0.034 Uiso 1 1 calc R . . H26F H 0.8971 0.2353 0.5220 0.034 Uiso 1 1 calc R . . C27B C 0.84971(12) 0.11786(7) 0.31739(11) 0.0213(4) Uani 1 1 d . . . C28B C 0.94190(12) 0.13336(9) 0.35135(13) 0.0306(5) Uani 1 1 d . . . H28D H 0.9522 0.1682 0.3343 0.046 Uiso 1 1 calc R . . H28E H 0.9801 0.1086 0.3356 0.046 Uiso 1 1 calc R . . H28F H 0.9525 0.1332 0.4059 0.046 Uiso 1 1 calc R . . C29B C 0.83751(13) 0.06240(8) 0.34434(12) 0.0267(4) Uani 1 1 d . . . H29D H 0.8440 0.0626 0.3985 0.040 Uiso 1 1 calc R . . H29E H 0.8802 0.0394 0.3319 0.040 Uiso 1 1 calc R . . H29F H 0.7805 0.0500 0.3198 0.040 Uiso 1 1 calc R . . C30B C 0.83540(13) 0.11847(8) 0.23199(11) 0.0262(4) Uani 1 1 d . . . H30D H 0.8424 0.1539 0.2152 0.039 Uiso 1 1 calc R . . H30E H 0.7778 0.1063 0.2090 0.039 Uiso 1 1 calc R . . H30F H 0.8769 0.0956 0.2173 0.039 Uiso 1 1 calc R . . C31B C 0.53626(11) 0.04680(7) 0.34234(10) 0.0190(4) Uani 1 1 d . . . C32B C 0.59638(12) 0.07065(8) 0.41099(10) 0.0255(4) Uani 1 1 d . . . H32D H 0.6006 0.0476 0.4539 0.038 Uiso 1 1 calc R . . H32E H 0.5743 0.1044 0.4217 0.038 Uiso 1 1 calc R . . H32F H 0.6528 0.0752 0.4013 0.038 Uiso 1 1 calc R . . C33B C 0.57299(14) -0.00454(8) 0.32219(12) 0.0284(4) Uani 1 1 d . . . H33D H 0.5807 -0.0285 0.3645 0.043 Uiso 1 1 calc R . . H33E H 0.6280 0.0019 0.3106 0.043 Uiso 1 1 calc R . . H33F H 0.5338 -0.0198 0.2787 0.043 Uiso 1 1 calc R . . C34B C 0.45016(12) 0.03698(8) 0.35961(10) 0.0238(4) Uani 1 1 d . . . H34D H 0.4575 0.0139 0.4029 0.036 Uiso 1 1 calc R . . H34E H 0.4119 0.0207 0.3164 0.036 Uiso 1 1 calc R . . H34F H 0.4258 0.0700 0.3706 0.036 Uiso 1 1 calc R . . C35B C 0.53187(12) 0.11616(7) 0.13053(10) 0.0196(4) Uani 1 1 d . . . C36B C 0.44400(12) 0.12414(8) 0.07859(10) 0.0238(4) Uani 1 1 d . . . H36D H 0.4502 0.1351 0.0294 0.036 Uiso 1 1 calc R . . H36E H 0.4133 0.1509 0.0993 0.036 Uiso 1 1 calc R . . H36F H 0.4121 0.0915 0.0738 0.036 Uiso 1 1 calc R . . C37B C 0.57651(14) 0.07077(8) 0.10262(11) 0.0292(4) Uani 1 1 d . . . H37D H 0.5834 0.0785 0.0525 0.044 Uiso 1 1 calc R . . H37E H 0.5423 0.0393 0.1011 0.044 Uiso 1 1 calc R . . H37F H 0.6325 0.0654 0.1365 0.044 Uiso 1 1 calc R . . C38B C 0.58323(13) 0.16593(8) 0.13208(11) 0.0255(4) Uani 1 1 d . . . H38D H 0.5885 0.1741 0.0815 0.038 Uiso 1 1 calc R . . H38E H 0.6399 0.1612 0.1649 0.038 Uiso 1 1 calc R . . H38F H 0.5543 0.1945 0.1508 0.038 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 Sn1A 0.01334(6) 0.01558(7) 0.01537(6) 0.00110(4) 0.00334(4) -0.00077(4) O1A 0.0132(6) 0.0204(6) 0.0212(6) 0.0029(5) 0.0018(5) -0.0019(5) O2A 0.0155(6) 0.0176(6) 0.0223(6) 0.0052(5) 0.0056(5) 0.0007(5) N1A 0.0135(7) 0.0196(7) 0.0173(7) 0.0000(6) 0.0024(6) 0.0002(5) N2A 0.0138(7) 0.0193(7) 0.0171(7) -0.0003(6) 0.0041(6) -0.0007(5) C1A 0.0162(9) 0.0217(9) 0.0156(8) -0.0004(7) 0.0027(7) -0.0008(7) C2A 0.0140(8) 0.0181(8) 0.0179(8) -0.0003(7) 0.0036(6) 0.0002(6) C3A 0.0193(9) 0.0176(9) 0.0188(8) 0.0009(7) 0.0056(7) -0.0015(7) C4A 0.0141(8) 0.0209(9) 0.0167(8) -0.0043(7) 0.0035(6) -0.0030(7) C5A 0.0168(9) 0.0215(9) 0.0181(8) -0.0004(7) 0.0016(7) 0.0016(7) C6A 0.0179(9) 0.0182(9) 0.0164(8) 0.0003(7) 0.0029(7) -0.0009(7) C7A 0.0127(8) 0.0223(9) 0.0200(9) -0.0022(7) 0.0025(7) -0.0016(7) C8A 0.0189(9) 0.0264(10) 0.0315(10) -0.0100(8) 0.0046(8) -0.0028(7) C9A 0.0138(9) 0.0228(10) 0.0289(10) -0.0033(8) 0.0036(7) -0.0008(7) C10A 0.0188(9) 0.0289(10) 0.0273(10) 0.0034(8) 0.0053(8) -0.0047(7) C11A 0.0175(9) 0.0200(9) 0.0255(9) 0.0050(7) 0.0015(7) 0.0000(7) C12A 0.0301(11) 0.0298(11) 0.0246(10) 0.0089(8) 0.0064(8) 0.0010(8) C13A 0.0321(11) 0.0196(10) 0.0355(11) -0.0013(8) 0.0082(9) -0.0036(8) C14A 0.0217(10) 0.0258(11) 0.0516(14) 0.0149(10) -0.0011(9) 0.0001(8) C15A 0.0156(8) 0.0185(9) 0.0233(9) 0.0002(7) 0.0055(7) -0.0024(7) C16A 0.0191(9) 0.0165(8) 0.0210(9) 0.0027(7) 0.0050(7) 0.0004(7) C17A 0.0161(8) 0.0149(8) 0.0168(8) -0.0012(6) 0.0060(7) 0.0011(6) C18A 0.0155(8) 0.0168(8) 0.0191(8) 0.0005(7) 0.0050(7) -0.0008(6) C19A 0.0173(9) 0.0175(8) 0.0205(9) 0.0018(7) 0.0066(7) -0.0004(6) C20A 0.0177(9) 0.0160(8) 0.0175(8) -0.0002(7) 0.0043(7) 0.0016(6) C21A 0.0146(8) 0.0181(8) 0.0187(8) -0.0014(7) 0.0045(7) 0.0025(6) C22A 0.0146(8) 0.0165(8) 0.0176(8) -0.0014(6) 0.0062(7) 0.0002(6) C23A 0.0194(9) 0.0193(9) 0.0199(9) 0.0033(7) 0.0033(7) 0.0014(7) C24A 0.0280(11) 0.0284(11) 0.0430(12) 0.0182(10) 0.0034(9) -0.0010(8) C25A 0.0356(11) 0.0290(11) 0.0199(9) 0.0018(8) 0.0070(8) 0.0072(8) C26A 0.0306(11) 0.0244(10) 0.0222(9) 0.0039(8) 0.0056(8) 0.0100(8) C27A 0.0145(8) 0.0177(8) 0.0209(9) 0.0000(7) 0.0061(7) -0.0011(6) C28A 0.0196(9) 0.0170(9) 0.0278(10) -0.0016(7) 0.0074(7) -0.0008(7) C29A 0.0196(9) 0.0256(10) 0.0233(9) 0.0018(8) 0.0094(7) -0.0016(7) C30A 0.0154(8) 0.0204(9) 0.0253(9) -0.0010(7) 0.0055(7) -0.0013(7) C31A 0.0228(9) 0.0235(9) 0.0178(9) -0.0026(7) 0.0069(7) -0.0011(7) C32A 0.0306(12) 0.0604(16) 0.0220(10) -0.0124(10) 0.0038(9) -0.0046(10) C33A 0.0391(12) 0.0256(10) 0.0256(10) 0.0051(8) 0.0164(9) 0.0029(8) C34A 0.0503(13) 0.0228(10) 0.0237(10) -0.0021(8) 0.0150(9) 0.0039(9) C35A 0.0179(9) 0.0191(9) 0.0174(8) -0.0013(7) 0.0045(7) 0.0010(7) C36A 0.0240(10) 0.0275(10) 0.0159(9) -0.0012(7) 0.0036(7) 0.0022(7) C37A 0.0310(11) 0.0210(10) 0.0239(10) -0.0017(8) 0.0047(8) -0.0025(8) C38A 0.0217(10) 0.0357(11) 0.0230(10) -0.0047(8) 0.0087(8) 0.0020(8) Sn1B 0.01536(6) 0.01396(6) 0.01544(6) -0.00068(4) 0.00453(5) 0.00045(4) O1B 0.0170(6) 0.0158(6) 0.0185(6) -0.0008(5) 0.0046(5) 0.0010(5) O2B 0.0146(6) 0.0159(6) 0.0207(6) -0.0020(5) 0.0051(5) 0.0007(5) N1B 0.0149(7) 0.0181(7) 0.0157(7) -0.0010(6) 0.0028(6) -0.0002(5) N2B 0.0175(7) 0.0169(7) 0.0167(7) -0.0003(6) 0.0065(6) 0.0001(5) C1B 0.0186(9) 0.0175(9) 0.0148(8) 0.0016(6) 0.0061(7) 0.0002(6) C2B 0.0155(8) 0.0189(9) 0.0153(8) -0.0013(6) 0.0041(7) -0.0007(6) C3B 0.0197(9) 0.0177(9) 0.0194(9) -0.0029(7) 0.0051(7) 0.0015(7) C4B 0.0157(9) 0.0195(9) 0.0177(8) -0.0003(7) 0.0052(7) 0.0018(6) C5B 0.0177(9) 0.0189(9) 0.0155(8) 0.0004(7) 0.0041(7) -0.0021(6) C6B 0.0181(8) 0.0165(8) 0.0136(8) 0.0009(6) 0.0058(6) 0.0010(6) C7B 0.0151(9) 0.0219(9) 0.0233(9) -0.0026(7) 0.0030(7) 0.0025(7) C8B 0.0224(10) 0.0291(10) 0.0268(10) -0.0037(8) 0.0077(8) 0.0054(8) C9B 0.0237(10) 0.0281(10) 0.0261(10) 0.0018(8) 0.0042(8) 0.0074(8) C10B 0.0158(9) 0.0271(10) 0.0438(12) -0.0081(9) 0.0039(9) 0.0010(7) C11B 0.0194(9) 0.0150(8) 0.0189(8) -0.0008(7) 0.0058(7) -0.0004(6) C12B 0.0224(9) 0.0213(9) 0.0223(9) -0.0046(7) 0.0075(7) -0.0005(7) C13B 0.0295(10) 0.0170(9) 0.0245(9) 0.0027(7) 0.0066(8) 0.0013(7) C14B 0.0215(9) 0.0180(9) 0.0311(10) -0.0048(8) 0.0065(8) -0.0026(7) C15B 0.0180(9) 0.0190(9) 0.0198(9) -0.0018(7) 0.0036(7) 0.0027(7) C16B 0.0187(9) 0.0155(8) 0.0214(9) -0.0032(7) 0.0054(7) -0.0003(7) C17B 0.0185(9) 0.0159(8) 0.0170(8) 0.0011(6) 0.0058(7) 0.0000(6) C18B 0.0153(8) 0.0170(8) 0.0175(8) 0.0016(7) 0.0043(7) 0.0005(6) C19B 0.0177(8) 0.0151(8) 0.0175(8) 0.0009(6) 0.0056(7) 0.0028(6) C20B 0.0180(9) 0.0168(8) 0.0172(8) 0.0016(7) 0.0046(7) -0.0006(6) C21B 0.0139(8) 0.0211(9) 0.0215(9) 0.0001(7) 0.0044(7) 0.0005(7) C22B 0.0171(9) 0.0193(9) 0.0190(9) 0.0006(7) 0.0060(7) 0.0013(7) C23B 0.0161(8) 0.0172(8) 0.0185(8) -0.0013(7) 0.0020(7) -0.0002(6) C24B 0.0197(9) 0.0212(9) 0.0235(9) -0.0057(7) 0.0036(7) 0.0002(7) C25B 0.0207(9) 0.0215(9) 0.0255(9) -0.0015(7) 0.0061(7) -0.0024(7) C26B 0.0199(9) 0.0247(10) 0.0211(9) -0.0007(7) 0.0010(7) -0.0011(7) C27B 0.0193(9) 0.0205(9) 0.0253(10) -0.0027(7) 0.0075(7) 0.0027(7) C28B 0.0178(10) 0.0322(11) 0.0420(12) -0.0090(9) 0.0077(9) 0.0056(8) C29B 0.0259(10) 0.0232(10) 0.0318(11) 0.0013(8) 0.0088(8) 0.0070(8) C30B 0.0260(10) 0.0284(10) 0.0276(10) -0.0023(8) 0.0128(8) 0.0045(8) C31B 0.0213(9) 0.0178(9) 0.0179(8) 0.0016(7) 0.0047(7) 0.0009(7) C32B 0.0259(10) 0.0299(11) 0.0188(9) 0.0037(8) 0.0018(8) -0.0035(8) C33B 0.0354(11) 0.0207(10) 0.0312(11) 0.0045(8) 0.0119(9) 0.0071(8) C34B 0.0259(10) 0.0257(10) 0.0203(9) 0.0023(7) 0.0066(8) -0.0036(8) C35B 0.0236(9) 0.0187(9) 0.0179(9) 0.0006(7) 0.0077(7) -0.0022(7) C36B 0.0267(10) 0.0271(10) 0.0172(9) 0.0041(7) 0.0046(7) -0.0043(8) C37B 0.0388(12) 0.0286(11) 0.0239(10) -0.0014(8) 0.0148(9) 0.0048(9) C38B 0.0277(10) 0.0262(10) 0.0227(9) 0.0031(8) 0.0064(8) -0.0070(8) _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 Sn1A C31A 2.1992(18) . ? Sn1A C35A 2.2001(17) . ? Sn1A O1A 2.2488(12) . ? Sn1A N2A 2.2628(15) . ? Sn1A O2A 2.2669(12) . ? Sn1A N1A 2.2679(14) . ? O1A C1A 1.303(2) . ? O2A C17A 1.293(2) . ? N1A C15A 1.297(2) . ? N1A C2A 1.382(2) . ? N2A C16A 1.306(2) . ? N2A C18A 1.384(2) . ? C1A C2A 1.433(2) . ? C1A C6A 1.434(2) . ? C2A C3A 1.408(2) . ? C3A C4A 1.369(2) . ? C4A C5A 1.420(3) . ? C4A C7A 1.532(2) . ? C5A C6A 1.385(2) . ? C6A C11A 1.537(2) . ? C7A C9A 1.531(2) . ? C7A C8A 1.538(2) . ? C7A C10A 1.539(3) . ? C11A C13A 1.534(3) . ? C11A C12A 1.535(3) . ? C11A C14A 1.535(3) . ? C15A C16A 1.429(2) . ? C17A C18A 1.427(2) . ? C17A C22A 1.443(2) . ? C18A C19A 1.405(2) . ? C19A C20A 1.370(2) . ? C20A C21A 1.424(2) . ? C20A C23A 1.533(2) . ? C21A C22A 1.381(2) . ? C22A C27A 1.536(2) . ? C23A C24A 1.526(3) . ? C23A C26A 1.531(3) . ? C23A C25A 1.540(3) . ? C27A C30A 1.532(2) . ? C27A C29A 1.540(2) . ? C27A C28A 1.543(2) . ? C31A C33A 1.524(3) . ? C31A C34A 1.527(3) . ? C31A C32A 1.528(3) . ? C35A C36A 1.527(2) . ? C35A C38A 1.529(3) . ? C35A C37A 1.530(3) . ? Sn1B C31B 2.2003(18) . ? Sn1B C35B 2.2009(18) . ? Sn1B O1B 2.2544(12) . ? Sn1B N2B 2.2626(14) . ? Sn1B N1B 2.2668(14) . ? Sn1B O2B 2.2707(12) . ? O1B C1B 1.301(2) . ? O2B C17B 1.311(2) . ? N1B C15B 1.300(2) . ? N1B C2B 1.389(2) . ? N2B C16B 1.305(2) . ? N2B C18B 1.389(2) . ? C1B C2B 1.433(2) . ? C1B C6B 1.435(2) . ? C2B C3B 1.404(2) . ? C3B C4B 1.378(2) . ? C4B C5B 1.413(2) . ? C4B C7B 1.533(2) . ? C5B C6B 1.383(2) . ? C6B C11B 1.533(2) . ? C7B C10B 1.534(3) . ? C7B C9B 1.541(3) . ? C7B C8B 1.542(3) . ? C11B C14B 1.536(2) . ? C11B C12B 1.539(2) . ? C11B C13B 1.539(2) . ? C15B C16B 1.430(2) . ? C17B C18B 1.428(2) . ? C17B C22B 1.443(2) . ? C18B C19B 1.406(2) . ? C19B C20B 1.372(2) . ? C20B C21B 1.422(2) . ? C20B C23B 1.533(2) . ? C21B C22B 1.375(3) . ? C22B C27B 1.537(2) . ? C23B C24B 1.531(2) . ? C23B C25B 1.541(2) . ? C23B C26B 1.541(2) . ? C27B C28B 1.529(3) . ? C27B C30B 1.538(3) . ? C27B C29B 1.542(3) . ? C31B C34B 1.526(3) . ? C31B C32B 1.530(2) . ? C31B C33B 1.533(3) . ? C35B C38B 1.526(2) . ? C35B C36B 1.528(3) . ? C35B C37B 1.529(3) . ? 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 C31A Sn1A C35A 152.94(7) . . ? C31A Sn1A O1A 87.61(6) . . ? C35A Sn1A O1A 85.71(6) . . ? C31A Sn1A N2A 102.19(6) . . ? C35A Sn1A N2A 98.81(6) . . ? O1A Sn1A N2A 143.16(5) . . ? C31A Sn1A O2A 83.77(6) . . ? C35A Sn1A O2A 86.94(6) . . ? O1A Sn1A O2A 145.32(4) . . ? N2A Sn1A O2A 71.49(5) . . ? C31A Sn1A N1A 100.11(6) . . ? C35A Sn1A N1A 102.63(6) . . ? O1A Sn1A N1A 71.89(5) . . ? N2A Sn1A N1A 71.45(5) . . ? O2A Sn1A N1A 142.72(5) . . ? C1A O1A Sn1A 117.15(11) . . ? C17A O2A Sn1A 116.75(11) . . ? C15A N1A C2A 126.84(15) . . ? C15A N1A Sn1A 116.55(11) . . ? C2A N1A Sn1A 116.59(11) . . ? C16A N2A C18A 126.91(16) . . ? C16A N2A Sn1A 116.24(12) . . ? C18A N2A Sn1A 116.77(11) . . ? O1A C1A C2A 119.85(15) . . ? O1A C1A C6A 122.57(16) . . ? C2A C1A C6A 117.58(16) . . ? N1A C2A C3A 124.20(16) . . ? N1A C2A C1A 114.17(15) . . ? C3A C2A C1A 121.63(16) . . ? C4A C3A C2A 121.01(17) . . ? C3A C4A C5A 117.21(16) . . ? C3A C4A C7A 121.38(16) . . ? C5A C4A C7A 121.34(16) . . ? C6A C5A C4A 124.73(16) . . ? C5A C6A C1A 117.81(16) . . ? C5A C6A C11A 122.13(16) . . ? C1A C6A C11A 120.03(15) . . ? C9A C7A C4A 112.01(15) . . ? C9A C7A C8A 109.14(15) . . ? C4A C7A C8A 108.30(15) . . ? C9A C7A C10A 107.88(15) . . ? C4A C7A C10A 111.07(14) . . ? C8A C7A C10A 108.36(16) . . ? C13A C11A C12A 109.91(16) . . ? C13A C11A C14A 107.97(17) . . ? C12A C11A C14A 107.07(16) . . ? C13A C11A C6A 108.85(15) . . ? C12A C11A C6A 111.23(16) . . ? C14A C11A C6A 111.74(15) . . ? N1A C15A C16A 117.71(16) . . ? N2A C16A C15A 118.00(16) . . ? O2A C17A C18A 120.23(15) . . ? O2A C17A C22A 122.28(16) . . ? C18A C17A C22A 117.48(15) . . ? N2A C18A C19A 123.81(16) . . ? N2A C18A C17A 114.05(15) . . ? C19A C18A C17A 122.05(16) . . ? C20A C19A C18A 120.68(16) . . ? C19A C20A C21A 117.44(16) . . ? C19A C20A C23A 122.23(16) . . ? C21A C20A C23A 120.27(15) . . ? C22A C21A C20A 124.58(16) . . ? C21A C22A C17A 117.68(16) . . ? C21A C22A C27A 123.20(15) . . ? C17A C22A C27A 119.12(15) . . ? C24A C23A C26A 107.28(16) . . ? C24A C23A C20A 112.03(15) . . ? C26A C23A C20A 110.29(15) . . ? C24A C23A C25A 108.72(17) . . ? C26A C23A C25A 109.87(15) . . ? C20A C23A C25A 108.62(15) . . ? C30A C27A C22A 112.52(15) . . ? C30A C27A C29A 107.52(14) . . ? C22A C27A C29A 108.65(14) . . ? C30A C27A C28A 106.82(14) . . ? C22A C27A C28A 111.46(14) . . ? C29A C27A C28A 109.79(15) . . ? C33A C31A C34A 110.23(16) . . ? C33A C31A C32A 109.93(17) . . ? C34A C31A C32A 108.81(17) . . ? C33A C31A Sn1A 108.00(12) . . ? C34A C31A Sn1A 108.74(12) . . ? C32A C31A Sn1A 111.13(13) . . ? C36A C35A C38A 109.15(15) . . ? C36A C35A C37A 109.83(15) . . ? C38A C35A C37A 110.06(16) . . ? C36A C35A Sn1A 111.73(12) . . ? C38A C35A Sn1A 108.85(12) . . ? C37A C35A Sn1A 107.19(12) . . ? C31B Sn1B C35B 153.76(7) . . ? C31B Sn1B O1B 85.43(6) . . ? C35B Sn1B O1B 86.96(6) . . ? C31B Sn1B N2B 100.23(6) . . ? C35B Sn1B N2B 100.74(6) . . ? O1B Sn1B N2B 143.69(5) . . ? C31B Sn1B N1B 104.04(6) . . ? C35B Sn1B N1B 97.36(6) . . ? O1B Sn1B N1B 72.00(5) . . ? N2B Sn1B N1B 71.84(5) . . ? C31B Sn1B O2B 87.06(6) . . ? C35B Sn1B O2B 84.69(6) . . ? O1B Sn1B O2B 144.54(4) . . ? N2B Sn1B O2B 71.77(5) . . ? N1B Sn1B O2B 143.28(5) . . ? C1B O1B Sn1B 116.91(11) . . ? C17B O2B Sn1B 116.13(11) . . ? C15B N1B C2B 127.35(15) . . ? C15B N1B Sn1B 115.84(11) . . ? C2B N1B Sn1B 116.49(11) . . ? C16B N2B C18B 127.00(15) . . ? C16B N2B Sn1B 115.82(12) . . ? C18B N2B Sn1B 117.16(11) . . ? O1B C1B C2B 120.23(15) . . ? O1B C1B C6B 122.56(16) . . ? C2B C1B C6B 117.19(15) . . ? N1B C2B C3B 123.86(16) . . ? N1B C2B C1B 114.03(15) . . ? C3B C2B C1B 122.04(16) . . ? C4B C3B C2B 120.55(17) . . ? C3B C4B C5B 117.43(16) . . ? C3B C4B C7B 120.84(16) . . ? C5B C4B C7B 121.59(16) . . ? C6B C5B C4B 124.61(16) . . ? C5B C6B C1B 118.16(16) . . ? C5B C6B C11B 121.72(15) . . ? C1B C6B C11B 120.12(15) . . ? C4B C7B C10B 112.49(15) . . ? C4B C7B C9B 108.45(15) . . ? C10B C7B C9B 108.61(16) . . ? C4B C7B C8B 110.53(15) . . ? C10B C7B C8B 107.61(16) . . ? C9B C7B C8B 109.09(16) . . ? C6B C11B C14B 112.16(14) . . ? C6B C11B C12B 110.80(14) . . ? C14B C11B C12B 107.39(15) . . ? C6B C11B C13B 109.38(14) . . ? C14B C11B C13B 107.35(15) . . ? C12B C11B C13B 109.67(15) . . ? N1B C15B C16B 118.09(16) . . ? N2B C16B C15B 118.13(16) . . ? O2B C17B C18B 120.75(15) . . ? O2B C17B C22B 122.12(16) . . ? C18B C17B C22B 117.13(15) . . ? N2B C18B C19B 124.22(16) . . ? N2B C18B C17B 113.53(15) . . ? C19B C18B C17B 122.23(16) . . ? C20B C19B C18B 120.48(16) . . ? C19B C20B C21B 117.31(16) . . ? C19B C20B C23B 123.98(16) . . ? C21B C20B C23B 118.70(15) . . ? C22B C21B C20B 124.83(16) . . ? C21B C22B C17B 117.84(16) . . ? C21B C22B C27B 122.07(16) . . ? C17B C22B C27B 120.08(16) . . ? C24B C23B C20B 112.07(14) . . ? C24B C23B C25B 108.19(15) . . ? C20B C23B C25B 109.76(14) . . ? C24B C23B C26B 108.71(15) . . ? C20B C23B C26B 109.22(14) . . ? C25B C23B C26B 108.83(14) . . ? C28B C27B C22B 112.11(15) . . ? C28B C27B C30B 108.05(16) . . ? C22B C27B C30B 109.13(15) . . ? C28B C27B C29B 107.37(16) . . ? C22B C27B C29B 110.20(15) . . ? C30B C27B C29B 109.95(16) . . ? C34B C31B C32B 109.03(15) . . ? C34B C31B C33B 109.62(16) . . ? C32B C31B C33B 109.91(16) . . ? C34B C31B Sn1B 110.32(12) . . ? C32B C31B Sn1B 111.32(12) . . ? C33B C31B Sn1B 106.60(12) . . ? C38B C35B C36B 108.72(15) . . ? C38B C35B C37B 110.44(17) . . ? C36B C35B C37B 109.68(16) . . ? C38B C35B Sn1B 109.31(12) . . ? C36B C35B Sn1B 110.85(12) . . ? C37B C35B Sn1B 107.84(12) . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.00 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.345 _refine_diff_density_min -0.703 _refine_diff_density_rms 0.073 _publ_section_references ; Bruker (2003) SAINTPlus Data Reduction and Correction Program v. 6.45a, Bruker AXS, Madison, Wisconsin, USA. Bruker (2005) SMART. Bruker Molecular Analysis Research Tool, v. 5.632 Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (1998a). SADABS v.2.01, Bruker/Siemens Area Detector Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (2000). SHELXTL v. 6.12, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. ; # Attachment '- complex5.cif' data_pboonnm _database_code_depnum_ccdc_archive 'CCDC 872117' #TrackingRef '- complex5.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C43 H54 Cl2 N2 O2 Pb' _chemical_formula_weight 908.97 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.1974(3) _cell_length_b 13.8984(4) _cell_length_c 15.4418(4) _cell_angle_alpha 69.3860(10) _cell_angle_beta 80.3170(10) _cell_angle_gamma 89.5930(10) _cell_volume 2016.00(10) _cell_formula_units_Z 2 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used 950 _cell_measurement_theta_min 2 _cell_measurement_theta_max 30 _exptl_crystal_description plate _exptl_crystal_colour black _exptl_crystal_size_max 0.42 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.04 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.497 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 916 _exptl_absorpt_coefficient_mu 4.354 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.2621 _exptl_absorpt_correction_T_max 0.8451 _exptl_absorpt_process_details 'SADABS (Sheldrick, 1998)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 12739 _diffrn_reflns_av_R_equivalents 0.0114 _diffrn_reflns_av_sigmaI/netI 0.0201 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.27 _diffrn_reflns_theta_max 26.50 _reflns_number_total 8283 _reflns_number_gt 7895 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0358P)^2^+0.5085P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary patt _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8283 _refine_ls_number_parameters 471 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0216 _refine_ls_R_factor_gt 0.0200 _refine_ls_wR_factor_ref 0.0519 _refine_ls_wR_factor_gt 0.0513 _refine_ls_goodness_of_fit_ref 1.068 _refine_ls_restrained_S_all 1.068 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb -0.474168(6) -0.244889(4) -0.323740(4) 0.01222(2) Uani 1 1 d . . . O1 O -0.61198(13) -0.25880(10) -0.17570(9) 0.0139(3) Uani 1 1 d . . . O2 O -0.36462(14) -0.30801(10) -0.43782(10) 0.0158(3) Uani 1 1 d . . . N1 N -0.50642(15) -0.07971(12) -0.30602(11) 0.0133(3) Uani 1 1 d . . . N2 N -0.34973(16) -0.11009(12) -0.45264(11) 0.0139(3) Uani 1 1 d . . . C1 C -0.62940(18) -0.17591(14) -0.15508(14) 0.0130(4) Uani 1 1 d . . . C2 C -0.58050(18) -0.07724(14) -0.22291(14) 0.0140(4) Uani 1 1 d . . . C3 C -0.60342(19) 0.01432(14) -0.20416(14) 0.0150(4) Uani 1 1 d . . . H3A H -0.5728 0.0787 -0.2517 0.018 Uiso 1 1 calc R . . C4 C -0.66911(19) 0.01156(14) -0.11832(14) 0.0145(4) Uani 1 1 d . . . C5 C -0.71298(19) -0.08647(14) -0.04953(14) 0.0145(4) Uani 1 1 d . . . H5A H -0.7575 -0.0888 0.0104 0.017 Uiso 1 1 calc R . . C6 C -0.69529(18) -0.17848(14) -0.06384(14) 0.0138(4) Uani 1 1 d . . . C7 C -0.6951(2) 0.10903(14) -0.09409(15) 0.0176(4) Uani 1 1 d . . . C8 C -0.6204(2) 0.10653(16) -0.01479(16) 0.0222(4) Uani 1 1 d . . . H8A H -0.5243 0.1064 -0.0363 0.033 Uiso 1 1 calc R . . H8B H -0.6495 0.0442 0.0402 0.033 Uiso 1 1 calc R . . H8C H -0.6396 0.1674 0.0022 0.033 Uiso 1 1 calc R . . C9 C -0.8453(2) 0.11358(17) -0.06112(18) 0.0262(5) Uani 1 1 d . . . H9A H -0.8933 0.1166 -0.1119 0.039 Uiso 1 1 calc R . . H9B H -0.8613 0.1750 -0.0445 0.039 Uiso 1 1 calc R . . H9C H -0.8771 0.0519 -0.0060 0.039 Uiso 1 1 calc R . . C10 C -0.6491(3) 0.20676(16) -0.17867(17) 0.0296(5) Uani 1 1 d . . . H10A H -0.5523 0.2082 -0.1980 0.044 Uiso 1 1 calc R . . H10B H -0.6723 0.2671 -0.1616 0.044 Uiso 1 1 calc R . . H10C H -0.6931 0.2078 -0.2307 0.044 Uiso 1 1 calc R . . C11 C -0.74569(19) -0.28232(14) 0.01330(14) 0.0152(4) Uani 1 1 d . . . C12 C -0.6285(2) -0.35317(15) 0.03299(15) 0.0185(4) Uani 1 1 d . . . H12A H -0.5659 -0.3240 0.0601 0.028 Uiso 1 1 calc R . . H12B H -0.5827 -0.3589 -0.0259 0.028 Uiso 1 1 calc R . . H12C H -0.6626 -0.4216 0.0773 0.028 Uiso 1 1 calc R . . C13 C -0.8541(2) -0.33153(15) -0.01918(15) 0.0195(4) Uani 1 1 d . . . H13A H -0.9302 -0.2877 -0.0265 0.029 Uiso 1 1 calc R . . H13B H -0.8832 -0.3997 0.0278 0.029 Uiso 1 1 calc R . . H13C H -0.8177 -0.3384 -0.0795 0.029 Uiso 1 1 calc R . . C14 C -0.8088(2) -0.27110(15) 0.10622(15) 0.0216(5) Uani 1 1 d . . . H14A H -0.8856 -0.2282 0.0966 0.032 Uiso 1 1 calc R . . H14B H -0.7430 -0.2387 0.1284 0.032 Uiso 1 1 calc R . . H14C H -0.8382 -0.3393 0.1532 0.032 Uiso 1 1 calc R . . C15 C -0.45063(19) -0.00055(14) -0.37693(14) 0.0147(4) Uani 1 1 d . . . H15 H -0.462(2) 0.0649(19) -0.3803(17) 0.021(6) Uiso 1 1 d . . . C16 C -0.36588(19) -0.01696(14) -0.45424(14) 0.0152(4) Uani 1 1 d . . . H16 H -0.321(3) 0.043(2) -0.5029(19) 0.027(7) Uiso 1 1 d . . . C17 C -0.27808(19) -0.24548(14) -0.50662(14) 0.0137(4) Uani 1 1 d . . . C18 C -0.26422(19) -0.13935(14) -0.51813(13) 0.0138(4) Uani 1 1 d . . . C19 C -0.16624(19) -0.07143(14) -0.58695(14) 0.0153(4) Uani 1 1 d . . . H19A H -0.1592 -0.0016 -0.5917 0.018 Uiso 1 1 calc R . . C20 C -0.08011(19) -0.10533(15) -0.64776(14) 0.0150(4) Uani 1 1 d . . . C21 C -0.09933(19) -0.20865(15) -0.64042(14) 0.0159(4) Uani 1 1 d . . . H21A H -0.0435 -0.2314 -0.6843 0.019 Uiso 1 1 calc R . . C22 C -0.1937(2) -0.27899(14) -0.57377(14) 0.0153(4) Uani 1 1 d . . . C23 C 0.03278(19) -0.03178(15) -0.71779(14) 0.0169(4) Uani 1 1 d . . . C24 C 0.1163(2) 0.01138(16) -0.66379(15) 0.0220(5) Uani 1 1 d . . . H24A H 0.1572 -0.0452 -0.6204 0.033 Uiso 1 1 calc R . . H24B H 0.0585 0.0463 -0.6282 0.033 Uiso 1 1 calc R . . H24C H 0.1862 0.0605 -0.7085 0.033 Uiso 1 1 calc R . . C25 C -0.0259(2) 0.05805(16) -0.78930(15) 0.0201(4) Uani 1 1 d . . . H25A H -0.0775 0.0310 -0.8247 0.030 Uiso 1 1 calc R . . H25B H 0.0467 0.1054 -0.8328 0.030 Uiso 1 1 calc R . . H25C H -0.0842 0.0949 -0.7559 0.030 Uiso 1 1 calc R . . C26 C 0.1279(2) -0.08544(17) -0.77172(16) 0.0238(5) Uani 1 1 d . . . H26A H 0.1614 -0.1455 -0.7270 0.036 Uiso 1 1 calc R . . H26B H 0.2028 -0.0374 -0.8106 0.036 Uiso 1 1 calc R . . H26C H 0.0802 -0.1077 -0.8121 0.036 Uiso 1 1 calc R . . C27 C -0.2081(2) -0.39098(15) -0.56914(15) 0.0175(4) Uani 1 1 d . . . C28 C -0.1127(2) -0.41007(16) -0.64864(16) 0.0236(5) Uani 1 1 d . . . H28A H -0.1291 -0.3624 -0.7094 0.035 Uiso 1 1 calc R . . H28B H -0.1275 -0.4811 -0.6450 0.035 Uiso 1 1 calc R . . H28C H -0.0205 -0.3990 -0.6424 0.035 Uiso 1 1 calc R . . C29 C -0.1775(2) -0.46451(15) -0.47456(16) 0.0231(5) Uani 1 1 d . . . H29A H -0.0900 -0.4445 -0.4660 0.035 Uiso 1 1 calc R . . H29B H -0.1772 -0.5351 -0.4743 0.035 Uiso 1 1 calc R . . H29C H -0.2459 -0.4607 -0.4233 0.035 Uiso 1 1 calc R . . C30 C -0.3509(2) -0.41633(15) -0.57745(16) 0.0221(5) Uani 1 1 d . . . H30A H -0.3709 -0.3701 -0.6377 0.033 Uiso 1 1 calc R . . H30B H -0.4139 -0.4073 -0.5258 0.033 Uiso 1 1 calc R . . H30C H -0.3591 -0.4878 -0.5741 0.033 Uiso 1 1 calc R . . C31 C -0.65560(19) -0.25005(14) -0.37960(14) 0.0146(4) Uani 1 1 d . . . C32 C -0.6484(2) -0.26328(15) -0.46550(15) 0.0189(4) Uani 1 1 d . . . H32A H -0.5654 -0.2742 -0.4982 0.023 Uiso 1 1 calc R . . C33 C -0.7640(2) -0.26035(16) -0.50297(17) 0.0248(5) Uani 1 1 d . . . H33A H -0.7598 -0.2688 -0.5618 0.030 Uiso 1 1 calc R . . C34 C -0.8857(2) -0.24510(16) -0.45483(17) 0.0259(5) Uani 1 1 d . . . H34A H -0.9643 -0.2431 -0.4807 0.031 Uiso 1 1 calc R . . C35 C -0.8920(2) -0.23292(16) -0.36908(16) 0.0230(5) Uani 1 1 d . . . H35A H -0.9753 -0.2228 -0.3362 0.028 Uiso 1 1 calc R . . C36 C -0.7773(2) -0.23531(15) -0.33055(15) 0.0193(4) Uani 1 1 d . . . H36A H -0.7819 -0.2270 -0.2716 0.023 Uiso 1 1 calc R . . C37 C -0.31843(19) -0.30088(14) -0.24038(14) 0.0151(4) Uani 1 1 d . . . C38 C -0.2286(2) -0.36695(15) -0.26379(15) 0.0184(4) Uani 1 1 d . . . H38A H -0.2343 -0.3868 -0.3160 0.022 Uiso 1 1 calc R . . C39 C -0.1302(2) -0.40391(16) -0.21014(16) 0.0209(4) Uani 1 1 d . . . H39A H -0.0685 -0.4493 -0.2257 0.025 Uiso 1 1 calc R . . C40 C -0.1216(2) -0.37484(16) -0.13389(16) 0.0206(4) Uani 1 1 d . . . H40A H -0.0547 -0.4008 -0.0970 0.025 Uiso 1 1 calc R . . C41 C -0.2112(2) -0.30767(16) -0.11155(15) 0.0199(4) Uani 1 1 d . . . H41A H -0.2046 -0.2871 -0.0598 0.024 Uiso 1 1 calc R . . C42 C -0.3109(2) -0.27024(15) -0.16471(15) 0.0175(4) Uani 1 1 d . . . H42A H -0.3725 -0.2246 -0.1494 0.021 Uiso 1 1 calc R . . C1S C -0.6563(2) -0.50352(17) -0.13372(16) 0.0235(5) Uani 1 1 d . . . H1SA H -0.6236 -0.5506 -0.0778 0.028 Uiso 1 1 calc R . . H1SB H -0.6551 -0.4335 -0.1308 0.028 Uiso 1 1 calc R . . Cl1S Cl -0.82142(5) -0.54337(4) -0.13127(4) 0.02900(12) Uani 1 1 d . . . Cl2S Cl -0.54879(6) -0.50274(4) -0.23683(4) 0.02548(11) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.01245(4) 0.00989(3) 0.01347(4) -0.00405(3) -0.00022(3) -0.00064(3) O1 0.0159(6) 0.0100(6) 0.0153(6) -0.0047(5) -0.0005(5) -0.0007(5) O2 0.0173(7) 0.0115(6) 0.0173(7) -0.0056(5) 0.0020(5) -0.0025(5) N1 0.0119(7) 0.0126(7) 0.0154(8) -0.0052(6) -0.0019(6) 0.0016(6) N2 0.0140(7) 0.0130(7) 0.0142(8) -0.0053(6) -0.0007(6) -0.0004(6) C1 0.0105(8) 0.0134(8) 0.0154(9) -0.0056(7) -0.0019(7) 0.0003(7) C2 0.0128(8) 0.0136(8) 0.0158(9) -0.0062(7) -0.0010(7) 0.0013(7) C3 0.0171(9) 0.0125(8) 0.0147(9) -0.0045(7) -0.0017(7) 0.0000(7) C4 0.0129(8) 0.0135(8) 0.0190(9) -0.0082(7) -0.0025(7) 0.0016(7) C5 0.0128(8) 0.0150(8) 0.0155(9) -0.0061(7) -0.0008(7) 0.0019(7) C6 0.0120(8) 0.0138(8) 0.0149(9) -0.0048(7) -0.0011(7) -0.0007(7) C7 0.0205(9) 0.0134(8) 0.0208(10) -0.0087(8) -0.0033(8) 0.0029(7) C8 0.0251(10) 0.0206(9) 0.0269(11) -0.0146(8) -0.0076(8) 0.0039(8) C9 0.0204(10) 0.0265(10) 0.0392(12) -0.0214(9) -0.0045(9) 0.0056(8) C10 0.0469(14) 0.0142(9) 0.0267(12) -0.0099(9) 0.0019(10) 0.0033(9) C11 0.0165(9) 0.0122(8) 0.0147(9) -0.0042(7) 0.0015(7) -0.0012(7) C12 0.0197(9) 0.0150(9) 0.0186(10) -0.0035(8) -0.0029(7) 0.0000(7) C13 0.0171(9) 0.0168(9) 0.0225(10) -0.0065(8) 0.0014(8) -0.0034(8) C14 0.0299(11) 0.0146(9) 0.0160(10) -0.0038(8) 0.0038(8) -0.0011(8) C15 0.0178(9) 0.0099(8) 0.0180(9) -0.0063(7) -0.0042(7) 0.0021(7) C16 0.0156(9) 0.0121(8) 0.0164(9) -0.0041(7) -0.0008(7) -0.0011(7) C17 0.0127(8) 0.0126(8) 0.0148(9) -0.0039(7) -0.0019(7) -0.0002(7) C18 0.0146(9) 0.0139(8) 0.0132(9) -0.0057(7) -0.0011(7) 0.0016(7) C19 0.0164(9) 0.0120(8) 0.0161(9) -0.0039(7) -0.0016(7) -0.0009(7) C20 0.0147(9) 0.0139(8) 0.0146(9) -0.0030(7) -0.0015(7) -0.0014(7) C21 0.0138(9) 0.0178(9) 0.0172(9) -0.0086(7) -0.0004(7) 0.0012(7) C22 0.0169(9) 0.0144(8) 0.0160(9) -0.0069(7) -0.0038(7) 0.0023(7) C23 0.0142(9) 0.0169(9) 0.0174(9) -0.0054(8) 0.0015(7) -0.0009(7) C24 0.0175(9) 0.0228(10) 0.0228(10) -0.0059(8) -0.0009(8) -0.0055(8) C25 0.0192(10) 0.0192(9) 0.0187(10) -0.0040(8) -0.0008(8) -0.0028(8) C26 0.0189(10) 0.0247(10) 0.0239(11) -0.0086(9) 0.0065(8) -0.0021(8) C27 0.0214(10) 0.0118(8) 0.0195(10) -0.0073(7) -0.0001(8) 0.0000(7) C28 0.0312(11) 0.0174(9) 0.0222(10) -0.0103(8) 0.0019(9) 0.0013(8) C29 0.0335(11) 0.0136(9) 0.0217(10) -0.0066(8) -0.0034(9) 0.0065(8) C30 0.0256(10) 0.0161(9) 0.0263(11) -0.0112(8) -0.0008(8) -0.0039(8) C31 0.0156(9) 0.0075(8) 0.0193(9) -0.0022(7) -0.0053(7) -0.0002(7) C32 0.0239(10) 0.0144(9) 0.0194(10) -0.0061(8) -0.0062(8) 0.0000(8) C33 0.0324(11) 0.0186(9) 0.0260(11) -0.0083(8) -0.0114(9) -0.0004(9) C34 0.0249(10) 0.0194(10) 0.0323(12) -0.0033(9) -0.0148(9) -0.0021(8) C35 0.0158(9) 0.0201(10) 0.0289(11) -0.0037(9) -0.0038(8) -0.0013(8) C36 0.0186(9) 0.0176(9) 0.0200(10) -0.0048(8) -0.0029(8) -0.0009(8) C37 0.0149(9) 0.0117(8) 0.0160(9) -0.0025(7) -0.0010(7) -0.0024(7) C38 0.0185(9) 0.0172(9) 0.0187(10) -0.0070(8) -0.0001(7) -0.0005(7) C39 0.0179(9) 0.0175(9) 0.0260(11) -0.0066(8) -0.0028(8) 0.0031(8) C40 0.0175(9) 0.0171(9) 0.0248(11) -0.0027(8) -0.0073(8) -0.0008(8) C41 0.0226(10) 0.0186(9) 0.0197(10) -0.0076(8) -0.0048(8) -0.0021(8) C42 0.0182(9) 0.0151(9) 0.0199(10) -0.0072(8) -0.0028(7) 0.0008(7) C1S 0.0243(10) 0.0229(10) 0.0238(11) -0.0091(9) -0.0040(8) -0.0021(8) Cl1S 0.0222(2) 0.0312(3) 0.0360(3) -0.0150(2) -0.0050(2) 0.0010(2) Cl2S 0.0277(3) 0.0195(2) 0.0281(3) -0.0093(2) 0.0002(2) -0.0018(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 C37 2.179(2) . ? Pb1 C31 2.180(2) . ? Pb1 O2 2.3522(14) . ? Pb1 N2 2.3749(15) . ? Pb1 O1 2.4187(13) . ? Pb1 N1 2.4196(16) . ? O1 C1 1.302(2) . ? O2 C17 1.307(2) . ? N1 C15 1.298(2) . ? N1 C2 1.387(2) . ? N2 C16 1.296(2) . ? N2 C18 1.392(2) . ? C1 C2 1.431(3) . ? C1 C6 1.444(3) . ? C2 C3 1.411(3) . ? C3 C4 1.369(3) . ? C4 C5 1.419(3) . ? C4 C7 1.538(3) . ? C5 C6 1.378(3) . ? C6 C11 1.536(3) . ? C7 C10 1.525(3) . ? C7 C8 1.538(3) . ? C7 C9 1.539(3) . ? C11 C14 1.531(3) . ? C11 C13 1.543(3) . ? C11 C12 1.544(3) . ? C15 C16 1.437(3) . ? C17 C18 1.427(3) . ? C17 C22 1.437(3) . ? C18 C19 1.403(3) . ? C19 C20 1.380(3) . ? C20 C21 1.412(3) . ? C20 C23 1.536(3) . ? C21 C22 1.383(3) . ? C22 C27 1.540(3) . ? C23 C26 1.532(3) . ? C23 C25 1.542(3) . ? C23 C24 1.542(3) . ? C27 C28 1.532(3) . ? C27 C30 1.538(3) . ? C27 C29 1.540(3) . ? C31 C32 1.392(3) . ? C31 C36 1.394(3) . ? C32 C33 1.393(3) . ? C33 C34 1.391(3) . ? C34 C35 1.384(3) . ? C35 C36 1.394(3) . ? C37 C38 1.387(3) . ? C37 C42 1.391(3) . ? C38 C39 1.389(3) . ? C39 C40 1.388(3) . ? C40 C41 1.391(3) . ? C41 C42 1.396(3) . ? C1S Cl1S 1.766(2) . ? C1S Cl2S 1.771(2) . ? 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 C37 Pb1 C31 158.15(7) . . ? C37 Pb1 O2 89.67(6) . . ? C31 Pb1 O2 87.50(6) . . ? C37 Pb1 N2 99.49(6) . . ? C31 Pb1 N2 99.71(6) . . ? O2 Pb1 N2 69.13(5) . . ? C37 Pb1 O1 85.00(6) . . ? C31 Pb1 O1 88.49(6) . . ? O2 Pb1 O1 155.10(4) . . ? N2 Pb1 O1 135.75(5) . . ? C37 Pb1 N1 100.51(6) . . ? C31 Pb1 N1 96.13(6) . . ? O2 Pb1 N1 137.59(5) . . ? N2 Pb1 N1 68.61(5) . . ? O1 Pb1 N1 67.29(5) . . ? C1 O1 Pb1 118.55(11) . . ? C17 O2 Pb1 117.60(12) . . ? C15 N1 C2 125.97(17) . . ? C15 N1 Pb1 115.53(13) . . ? C2 N1 Pb1 118.49(11) . . ? C16 N2 C18 126.37(16) . . ? C16 N2 Pb1 117.08(13) . . ? C18 N2 Pb1 116.53(12) . . ? O1 C1 C2 120.53(17) . . ? O1 C1 C6 122.51(16) . . ? C2 C1 C6 116.94(17) . . ? N1 C2 C3 123.37(16) . . ? N1 C2 C1 114.82(16) . . ? C3 C2 C1 121.78(17) . . ? C4 C3 C2 120.87(17) . . ? C3 C4 C5 117.50(17) . . ? C3 C4 C7 122.84(17) . . ? C5 C4 C7 119.66(17) . . ? C6 C5 C4 124.43(18) . . ? C5 C6 C1 118.35(17) . . ? C5 C6 C11 122.05(17) . . ? C1 C6 C11 119.59(17) . . ? C10 C7 C4 111.85(17) . . ? C10 C7 C8 108.67(18) . . ? C4 C7 C8 109.49(16) . . ? C10 C7 C9 107.92(18) . . ? C4 C7 C9 109.75(16) . . ? C8 C7 C9 109.11(18) . . ? C14 C11 C6 112.62(16) . . ? C14 C11 C13 107.21(16) . . ? C6 C11 C13 108.74(16) . . ? C14 C11 C12 107.38(17) . . ? C6 C11 C12 109.87(15) . . ? C13 C11 C12 111.01(16) . . ? N1 C15 C16 119.06(17) . . ? N2 C16 C15 119.33(17) . . ? O2 C17 C18 120.54(17) . . ? O2 C17 C22 122.44(17) . . ? C18 C17 C22 117.03(16) . . ? N2 C18 C19 122.73(17) . . ? N2 C18 C17 114.95(16) . . ? C19 C18 C17 122.22(18) . . ? C20 C19 C18 120.51(18) . . ? C19 C20 C21 117.28(17) . . ? C19 C20 C23 119.62(17) . . ? C21 C20 C23 123.08(18) . . ? C22 C21 C20 124.58(19) . . ? C21 C22 C17 118.14(18) . . ? C21 C22 C27 121.80(18) . . ? C17 C22 C27 120.05(17) . . ? C26 C23 C20 112.55(16) . . ? C26 C23 C25 108.57(17) . . ? C20 C23 C25 110.00(16) . . ? C26 C23 C24 107.10(17) . . ? C20 C23 C24 109.26(17) . . ? C25 C23 C24 109.28(17) . . ? C28 C27 C30 107.83(18) . . ? C28 C27 C22 111.91(16) . . ? C30 C27 C22 110.15(16) . . ? C28 C27 C29 108.45(17) . . ? C30 C27 C29 108.99(17) . . ? C22 C27 C29 109.44(17) . . ? C32 C31 C36 120.68(19) . . ? C32 C31 Pb1 119.94(14) . . ? C36 C31 Pb1 119.31(15) . . ? C31 C32 C33 119.3(2) . . ? C34 C33 C32 120.4(2) . . ? C35 C34 C33 119.8(2) . . ? C34 C35 C36 120.6(2) . . ? C35 C36 C31 119.2(2) . . ? C38 C37 C42 121.13(19) . . ? C38 C37 Pb1 119.17(15) . . ? C42 C37 Pb1 119.70(14) . . ? C37 C38 C39 119.4(2) . . ? C40 C39 C38 120.3(2) . . ? C39 C40 C41 119.9(2) . . ? C40 C41 C42 120.4(2) . . ? C37 C42 C41 118.90(19) . . ? Cl1S C1S Cl2S 111.53(13) . . ? _diffrn_measured_fraction_theta_max 0.991 _diffrn_reflns_theta_full 26.50 _diffrn_measured_fraction_theta_full 0.991 _refine_diff_density_max 1.616 _refine_diff_density_min -1.312 _refine_diff_density_rms 0.086 _publ_section_references ; Bruker (2003) SAINTPlus Data Reduction and Correction Program v. 6.45a, Bruker AXS, Madison, Wisconsin, USA. Bruker (2005) SMART. Bruker Molecular Analysis Research Tool, v. 5.632 Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (1998a). SADABS v.2.01, Bruker/Siemens Area Detector Absorption Correction Program, Bruker AXS, Madison, Wisconsin, USA. Sheldrick G.M. (2000). SHELXTL v. 6.12, Structure Determination Software Suite, Bruker AXS, Madison, Wisconsin, USA. ;