# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2009 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Zhong-Xia Wang' 'Zuo-Yun Chai' _publ_contact_author_name 'Zhong-Xia Wang' _publ_contact_author_email ZXWANG@USTC.EDU.CN _publ_section_title ; Synthesis and characterization of Sn(II), Pb(II) and Yb(II) complexes supported by [C(Ph2P=NSiMe3){6-(2-RC5H3N)}] 2- or [CH(Ph2P=NSiMe3){6-(2-RC5H3N)}]- (R = 3,5-dimethyl-1-pyrazolyl or iminophosphoranyl) ligands ; # Attachment 'crystal_data.cif' data_3 _database_code_depnum_ccdc_archive 'CCDC 725691' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C58 H72 N8 P2 Si2 Sn2' _chemical_formula_weight 1236.74 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' P P 0.1023 0.0942 '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' Sn Sn -0.6537 1.4246 '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 9.9696(13) _cell_length_b 12.8011(17) _cell_length_c 12.8842(17) _cell_angle_alpha 100.983(2) _cell_angle_beta 108.444(2) _cell_angle_gamma 91.686(2) _cell_volume 1524.2(3) _cell_formula_units_Z 1 _cell_measurement_temperature 294(2) _cell_measurement_reflns_used 4050 _cell_measurement_theta_min 2.71 _cell_measurement_theta_max 26.35 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.14 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas none _exptl_crystal_density_diffrn 1.347 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 634 _exptl_absorpt_coefficient_mu 0.953 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.700708 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 294(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 7769 _diffrn_reflns_av_R_equivalents 0.0221 _diffrn_reflns_av_sigmaI/netI 0.0438 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 9 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.02 _reflns_number_total 5337 _reflns_number_gt 4411 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0390P)^2^+0.4151P] 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 5337 _refine_ls_number_parameters 330 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0451 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0827 _refine_ls_wR_factor_gt 0.0735 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.035 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.32992(2) 1.027306(18) 0.950857(19) 0.04029(9) Uani 1 1 d . . . P1 P 0.45415(9) 0.92928(7) 0.78502(7) 0.0378(2) Uani 1 1 d . . . Si1 Si 0.34430(11) 1.13734(8) 0.72073(8) 0.0487(2) Uani 1 1 d . . . N1 N 0.4089(3) 1.0491(2) 0.8075(2) 0.0401(6) Uani 1 1 d . . . N2 N 0.3351(3) 0.7657(2) 0.9698(2) 0.0436(7) Uani 1 1 d . . . N3 N 0.2059(4) 0.6542(2) 1.0348(3) 0.0583(8) Uani 1 1 d . . . N4 N 0.2261(4) 0.5789(3) 1.1002(3) 0.0669(9) Uani 1 1 d . . . C1 C 0.4600(3) 0.8920(2) 0.9089(3) 0.0387(7) Uani 1 1 d . . . C2 C 0.4304(4) 0.7813(3) 0.9177(3) 0.0415(8) Uani 1 1 d . . . C3 C 0.4986(4) 0.6958(3) 0.8788(3) 0.0534(9) Uani 1 1 d . . . H3 H 0.5677 0.7076 0.8468 0.064 Uiso 1 1 calc R . . C4 C 0.4626(5) 0.5941(3) 0.8882(3) 0.0634(11) Uani 1 1 d . . . H4 H 0.5062 0.5367 0.8614 0.076 Uiso 1 1 calc R . . C5 C 0.3624(5) 0.5776(3) 0.9374(3) 0.0601(10) Uani 1 1 d . . . H5 H 0.3345 0.5094 0.9427 0.072 Uiso 1 1 calc R . . C6 C 0.3046(4) 0.6661(3) 0.9787(3) 0.0483(9) Uani 1 1 d . . . C7 C 0.0295(5) 0.7812(4) 0.9592(5) 0.0836(14) Uani 1 1 d . . . H7A H 0.0877 0.8480 0.9903 0.125 Uiso 1 1 calc R . . H7B H -0.0664 0.7919 0.9563 0.125 Uiso 1 1 calc R . . H7C H 0.0315 0.7541 0.8849 0.125 Uiso 1 1 calc R . . C8 C 0.0849(5) 0.7030(3) 1.0305(4) 0.0654(11) Uani 1 1 d . . . C9 C 0.0286(5) 0.6575(4) 1.0974(4) 0.0793(14) Uani 1 1 d . . . H9 H -0.0544 0.6738 1.1127 0.095 Uiso 1 1 calc R . . C10 C 0.1174(6) 0.5825(4) 1.1384(4) 0.0736(13) Uani 1 1 d . . . C11 C 0.1018(7) 0.5097(4) 1.2131(5) 0.108(2) Uani 1 1 d . . . H11A H 0.1431 0.4447 1.1957 0.163 Uiso 1 1 d R . . H11B H 0.0028 0.4937 1.2016 0.163 Uiso 1 1 d R . . H11C H 0.1494 0.5443 1.2898 0.163 Uiso 1 1 d R . . C12 C 0.3253(4) 0.8420(3) 0.6630(3) 0.0449(8) Uani 1 1 d . . . C13 C 0.3302(4) 0.8360(3) 0.5558(3) 0.0610(10) Uani 1 1 d . . . H13 H 0.4063 0.8714 0.5454 0.073 Uiso 1 1 calc R . . C14 C 0.2233(5) 0.7779(4) 0.4642(3) 0.0754(13) Uani 1 1 d . . . H14 H 0.2280 0.7739 0.3926 0.090 Uiso 1 1 calc R . . C15 C 0.1107(5) 0.7264(4) 0.4784(4) 0.0755(14) Uani 1 1 d . . . H15 H 0.0386 0.6876 0.4164 0.091 Uiso 1 1 calc R . . C16 C 0.1034(4) 0.7315(4) 0.5836(4) 0.0704(12) Uani 1 1 d . . . H16 H 0.0268 0.6957 0.5927 0.085 Uiso 1 1 calc R . . C17 C 0.2095(4) 0.7898(3) 0.6769(3) 0.0541(9) Uani 1 1 d . . . H17 H 0.2034 0.7939 0.7481 0.065 Uiso 1 1 calc R . . C18 C 0.6199(3) 0.9270(3) 0.7539(3) 0.0421(8) Uani 1 1 d . . . C19 C 0.7136(4) 1.0189(3) 0.7906(3) 0.0542(9) Uani 1 1 d . . . H19 H 0.6892 1.0816 0.8270 0.065 Uiso 1 1 calc R . . C20 C 0.8437(4) 1.0172(4) 0.7729(4) 0.0690(12) Uani 1 1 d . . . H20 H 0.9057 1.0792 0.7968 0.083 Uiso 1 1 calc R . . C21 C 0.8818(5) 0.9248(4) 0.7205(4) 0.0761(13) Uani 1 1 d . . . H21 H 0.9693 0.9242 0.7091 0.091 Uiso 1 1 calc R . . C22 C 0.7903(5) 0.8331(4) 0.6848(4) 0.0712(12) Uani 1 1 d . . . H22 H 0.8160 0.7704 0.6493 0.085 Uiso 1 1 calc R . . C23 C 0.6598(4) 0.8337(3) 0.7017(3) 0.0546(9) Uani 1 1 d . . . H23 H 0.5986 0.7713 0.6780 0.066 Uiso 1 1 calc R . . C24 C 0.1666(6) 1.0863(4) 0.6188(5) 0.114(2) Uani 1 1 d . . . H24A H 0.1717 1.0175 0.5755 0.171 Uiso 1 1 calc R . . H24B H 0.1354 1.1351 0.5699 0.171 Uiso 1 1 calc R . . H24C H 0.1005 1.0797 0.6581 0.171 Uiso 1 1 calc R . . C25 C 0.4636(7) 1.1641(6) 0.6424(6) 0.134(3) Uani 1 1 d . . . H25A H 0.5537 1.1972 0.6941 0.200 Uiso 1 1 calc R . . H25B H 0.4220 1.2109 0.5935 0.200 Uiso 1 1 calc R . . H25C H 0.4771 1.0980 0.5989 0.200 Uiso 1 1 calc R . . C26 C 0.3265(7) 1.2640(4) 0.8095(4) 0.0963(18) Uani 1 1 d . . . H26A H 0.2767 1.2492 0.8587 0.144 Uiso 1 1 calc R . . H26B H 0.2743 1.3094 0.7630 0.144 Uiso 1 1 calc R . . H26C H 0.4191 1.2991 0.8531 0.144 Uiso 1 1 calc R . . C27 C 0.2404(9) 0.4556(6) 0.5815(7) 0.148(3) Uani 1 1 d D . . H27A H 0.1671 0.4628 0.5146 0.221 Uiso 1 1 calc R . . H27B H 0.2164 0.4890 0.6457 0.221 Uiso 1 1 calc R . . H27C H 0.2492 0.3811 0.5818 0.221 Uiso 1 1 calc R . . C28 C 0.3764(10) 0.5075(7) 0.5854(8) 0.178(4) Uani 1 1 d D . . H28A H 0.3655 0.5827 0.5865 0.213 Uiso 1 1 calc R . . H28B H 0.4474 0.5029 0.6556 0.213 Uiso 1 1 calc R . . C29 C 0.4308(9) 0.4664(7) 0.4966(8) 0.169(4) Uani 1 1 d D . . H29A H 0.3583 0.4657 0.4254 0.203 Uiso 1 1 calc R . . H29B H 0.4514 0.3932 0.4992 0.203 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 Sn1 0.04073(14) 0.04795(15) 0.03576(14) 0.00957(10) 0.01628(10) 0.01331(10) P1 0.0416(5) 0.0422(5) 0.0311(4) 0.0064(4) 0.0146(4) 0.0103(4) Si1 0.0584(6) 0.0540(6) 0.0404(5) 0.0196(5) 0.0188(5) 0.0188(5) N1 0.0479(16) 0.0436(15) 0.0332(14) 0.0110(12) 0.0167(12) 0.0135(13) N2 0.0500(16) 0.0359(15) 0.0432(16) 0.0067(13) 0.0137(14) 0.0073(12) N3 0.065(2) 0.0512(19) 0.062(2) 0.0127(16) 0.0252(17) -0.0005(16) N4 0.085(3) 0.056(2) 0.062(2) 0.0162(17) 0.025(2) -0.0068(18) C1 0.0456(18) 0.0382(18) 0.0358(17) 0.0084(14) 0.0174(15) 0.0102(14) C2 0.0496(19) 0.0424(19) 0.0319(17) 0.0067(14) 0.0125(15) 0.0114(15) C3 0.066(2) 0.053(2) 0.050(2) 0.0141(18) 0.0267(19) 0.0226(18) C4 0.094(3) 0.045(2) 0.058(2) 0.0100(19) 0.032(2) 0.026(2) C5 0.086(3) 0.037(2) 0.058(2) 0.0129(18) 0.023(2) 0.0093(19) C6 0.053(2) 0.043(2) 0.045(2) 0.0096(16) 0.0106(17) 0.0047(16) C7 0.064(3) 0.088(3) 0.104(4) 0.029(3) 0.028(3) 0.021(3) C8 0.063(3) 0.062(3) 0.070(3) 0.006(2) 0.025(2) -0.002(2) C9 0.076(3) 0.083(3) 0.088(3) 0.005(3) 0.048(3) -0.008(3) C10 0.094(3) 0.062(3) 0.065(3) 0.002(2) 0.036(3) -0.017(3) C11 0.167(6) 0.085(4) 0.085(4) 0.010(3) 0.065(4) -0.030(4) C12 0.0463(19) 0.046(2) 0.0389(19) 0.0027(16) 0.0122(16) 0.0113(16) C13 0.061(2) 0.078(3) 0.041(2) 0.005(2) 0.0168(19) 0.003(2) C14 0.072(3) 0.102(4) 0.039(2) -0.006(2) 0.012(2) 0.008(3) C15 0.057(3) 0.088(3) 0.058(3) -0.016(2) 0.004(2) 0.010(2) C16 0.046(2) 0.079(3) 0.074(3) -0.004(2) 0.015(2) 0.002(2) C17 0.043(2) 0.066(2) 0.049(2) 0.0015(19) 0.0153(17) 0.0112(18) C18 0.0447(19) 0.052(2) 0.0318(17) 0.0081(15) 0.0148(15) 0.0116(16) C19 0.052(2) 0.063(2) 0.050(2) 0.0120(19) 0.0208(18) 0.0083(19) C20 0.055(2) 0.075(3) 0.082(3) 0.012(2) 0.033(2) 0.000(2) C21 0.053(2) 0.104(4) 0.082(3) 0.016(3) 0.038(2) 0.021(3) C22 0.072(3) 0.080(3) 0.070(3) 0.006(2) 0.038(2) 0.029(3) C23 0.061(2) 0.057(2) 0.049(2) 0.0060(18) 0.0240(19) 0.0152(19) C24 0.102(4) 0.092(4) 0.108(5) 0.029(3) -0.027(3) 0.024(3) C25 0.149(6) 0.179(6) 0.165(6) 0.138(6) 0.114(5) 0.092(5) C26 0.151(5) 0.068(3) 0.070(3) 0.022(3) 0.028(3) 0.054(3) C27 0.137(6) 0.121(6) 0.165(8) 0.030(5) 0.025(6) -0.024(5) C28 0.182(9) 0.160(8) 0.149(8) -0.023(7) 0.030(7) 0.008(7) C29 0.190(10) 0.145(8) 0.134(7) -0.015(6) 0.025(7) 0.011(6) _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 C1 2.278(3) . ? Sn1 N1 2.283(3) . ? Sn1 C1 2.342(3) 2_677 ? Sn1 P1 2.9014(9) . ? P1 N1 1.611(3) . ? P1 C1 1.735(3) . ? P1 C18 1.819(3) . ? P1 C12 1.827(3) . ? Si1 N1 1.734(3) . ? Si1 C26 1.846(4) . ? Si1 C25 1.849(5) . ? Si1 C24 1.850(5) . ? N2 C6 1.336(4) . ? N2 C2 1.355(4) . ? N3 C8 1.365(5) . ? N3 N4 1.376(4) . ? N3 C6 1.414(5) . ? N4 C10 1.322(6) . ? C1 C2 1.472(5) . ? C1 Sn1 2.342(3) 2_677 ? C2 C3 1.400(4) . ? C3 C4 1.379(5) . ? C3 H3 0.9300 . ? C4 C5 1.372(6) . ? C4 H4 0.9300 . ? C5 C6 1.378(5) . ? C5 H5 0.9300 . ? C7 C8 1.487(6) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 C9 1.370(6) . ? C9 C10 1.390(7) . ? C9 H9 0.9300 . ? C10 C11 1.499(7) . ? C11 H11A 0.9600 . ? C11 H11B 0.9600 . ? C11 H11C 0.9600 . ? C12 C13 1.385(5) . ? C12 C17 1.394(5) . ? C13 C14 1.380(6) . ? C13 H13 0.9300 . ? C14 C15 1.365(6) . ? C14 H14 0.9300 . ? C15 C16 1.370(6) . ? C15 H15 0.9300 . ? C16 C17 1.388(5) . ? C16 H16 0.9300 . ? C17 H17 0.9300 . ? C18 C19 1.388(5) . ? C18 C23 1.388(5) . ? C19 C20 1.385(5) . ? C19 H19 0.9300 . ? C20 C21 1.373(6) . ? C20 H20 0.9300 . ? C21 C22 1.374(6) . ? C21 H21 0.9300 . ? C22 C23 1.385(5) . ? C22 H22 0.9300 . ? C23 H23 0.9300 . ? C24 H24A 0.9600 . ? C24 H24B 0.9600 . ? C24 H24C 0.9600 . ? C25 H25A 0.9600 . ? C25 H25B 0.9600 . ? C25 H25C 0.9600 . ? C26 H26A 0.9600 . ? C26 H26B 0.9600 . ? C26 H26C 0.9600 . ? C27 C28 1.474(7) . ? C27 H27A 0.9600 . ? C27 H27B 0.9600 . ? C27 H27C 0.9600 . ? C28 C29 1.435(8) . ? C28 H28A 0.9700 . ? C28 H28B 0.9700 . ? C29 C29 1.574(16) 2_666 ? C29 H29A 0.9700 . ? C29 H29B 0.9700 . ? 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 C1 Sn1 N1 68.86(10) . . ? C1 Sn1 C1 86.36(11) . 2_677 ? N1 Sn1 C1 94.29(10) . 2_677 ? C1 Sn1 P1 36.72(8) . . ? N1 Sn1 P1 33.60(7) . . ? C1 Sn1 P1 98.14(8) 2_677 . ? N1 P1 C1 100.75(14) . . ? N1 P1 C18 111.48(15) . . ? C1 P1 C18 115.53(15) . . ? N1 P1 C12 112.60(15) . . ? C1 P1 C12 112.13(17) . . ? C18 P1 C12 104.66(15) . . ? N1 P1 Sn1 51.64(10) . . ? C1 P1 Sn1 51.72(10) . . ? C18 P1 Sn1 142.17(11) . . ? C12 P1 Sn1 113.11(11) . . ? N1 Si1 C26 107.65(18) . . ? N1 Si1 C25 112.4(2) . . ? C26 Si1 C25 109.1(3) . . ? N1 Si1 C24 111.3(2) . . ? C26 Si1 C24 107.9(3) . . ? C25 Si1 C24 108.3(3) . . ? P1 N1 Si1 133.03(17) . . ? P1 N1 Sn1 94.77(12) . . ? Si1 N1 Sn1 123.97(13) . . ? C6 N2 C2 117.9(3) . . ? C8 N3 N4 112.4(3) . . ? C8 N3 C6 129.8(4) . . ? N4 N3 C6 117.7(3) . . ? C10 N4 N3 104.7(4) . . ? C2 C1 P1 123.9(2) . . ? C2 C1 Sn1 123.4(2) . . ? P1 C1 Sn1 91.56(13) . . ? C2 C1 Sn1 110.7(2) . 2_677 ? P1 C1 Sn1 108.67(16) . 2_677 ? Sn1 C1 Sn1 93.64(11) . 2_677 ? N2 C2 C3 120.5(3) . . ? N2 C2 C1 116.2(3) . . ? C3 C2 C1 123.2(3) . . ? C4 C3 C2 119.6(4) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C5 C4 C3 119.8(4) . . ? C5 C4 H4 120.1 . . ? C3 C4 H4 120.1 . . ? C4 C5 C6 117.4(4) . . ? C4 C5 H5 121.3 . . ? C6 C5 H5 121.3 . . ? N2 C6 C5 124.5(4) . . ? N2 C6 N3 115.8(3) . . ? C5 C6 N3 119.7(3) . . ? C8 C7 H7A 109.5 . . ? C8 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? C8 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N3 C8 C9 104.4(4) . . ? N3 C8 C7 124.4(4) . . ? C9 C8 C7 131.0(4) . . ? C8 C9 C10 107.9(4) . . ? C8 C9 H9 126.0 . . ? C10 C9 H9 126.0 . . ? N4 C10 C9 110.6(4) . . ? N4 C10 C11 120.4(5) . . ? C9 C10 C11 129.0(5) . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C13 C12 C17 118.9(3) . . ? C13 C12 P1 122.0(3) . . ? C17 C12 P1 118.7(3) . . ? C14 C13 C12 120.6(4) . . ? C14 C13 H13 119.7 . . ? C12 C13 H13 119.7 . . ? C15 C14 C13 120.1(4) . . ? C15 C14 H14 119.9 . . ? C13 C14 H14 119.9 . . ? C14 C15 C16 120.2(4) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C15 C16 C17 120.6(4) . . ? C15 C16 H16 119.7 . . ? C17 C16 H16 119.7 . . ? C16 C17 C12 119.5(4) . . ? C16 C17 H17 120.3 . . ? C12 C17 H17 120.3 . . ? C19 C18 C23 119.0(3) . . ? C19 C18 P1 119.1(3) . . ? C23 C18 P1 121.7(3) . . ? C20 C19 C18 120.0(4) . . ? C20 C19 H19 120.0 . . ? C18 C19 H19 120.0 . . ? C21 C20 C19 120.6(4) . . ? C21 C20 H20 119.7 . . ? C19 C20 H20 119.7 . . ? C20 C21 C22 119.8(4) . . ? C20 C21 H21 120.1 . . ? C22 C21 H21 120.1 . . ? C21 C22 C23 120.2(4) . . ? C21 C22 H22 119.9 . . ? C23 C22 H22 119.9 . . ? C22 C23 C18 120.4(4) . . ? C22 C23 H23 119.8 . . ? C18 C23 H23 119.8 . . ? Si1 C24 H24A 109.5 . . ? Si1 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? Si1 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si1 C25 H25A 109.5 . . ? Si1 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si1 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si1 C26 H26A 109.5 . . ? Si1 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si1 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C28 C27 H27A 109.5 . . ? C28 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C28 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C27 117.3(8) . . ? C29 C28 H28A 108.0 . . ? C27 C28 H28A 108.0 . . ? C29 C28 H28B 108.0 . . ? C27 C28 H28B 108.0 . . ? H28A C28 H28B 107.2 . . ? C28 C29 C29 113.1(9) . 2_666 ? C28 C29 H29A 109.0 . . ? C29 C29 H29A 109.0 2_666 . ? C28 C29 H29B 109.0 . . ? C29 C29 H29B 109.0 2_666 . ? H29A C29 H29B 107.8 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C1 Sn1 P1 N1 -158.09(19) . . . . ? C1 Sn1 P1 N1 -85.49(15) 2_677 . . . ? N1 Sn1 P1 C1 158.09(19) . . . . ? C1 Sn1 P1 C1 72.60(18) 2_677 . . . ? C1 Sn1 P1 C18 -83.0(2) . . . . ? N1 Sn1 P1 C18 75.1(2) . . . . ? C1 Sn1 P1 C18 -10.4(2) 2_677 . . . ? C1 Sn1 P1 C12 100.66(19) . . . . ? N1 Sn1 P1 C12 -101.25(18) . . . . ? C1 Sn1 P1 C12 173.26(15) 2_677 . . . ? C1 P1 N1 Si1 -165.0(2) . . . . ? C18 P1 N1 Si1 71.9(3) . . . . ? C12 P1 N1 Si1 -45.4(3) . . . . ? Sn1 P1 N1 Si1 -147.7(3) . . . . ? C1 P1 N1 Sn1 -17.34(15) . . . . ? C18 P1 N1 Sn1 -140.44(12) . . . . ? C12 P1 N1 Sn1 102.28(15) . . . . ? C26 Si1 N1 P1 -176.9(3) . . . . ? C25 Si1 N1 P1 -56.7(4) . . . . ? C24 Si1 N1 P1 65.0(3) . . . . ? C26 Si1 N1 Sn1 43.1(3) . . . . ? C25 Si1 N1 Sn1 163.3(3) . . . . ? C24 Si1 N1 Sn1 -75.0(3) . . . . ? C1 Sn1 N1 P1 13.84(12) . . . . ? C1 Sn1 N1 P1 98.26(13) 2_677 . . . ? C1 Sn1 N1 Si1 165.7(2) . . . . ? C1 Sn1 N1 Si1 -109.89(17) 2_677 . . . ? P1 Sn1 N1 Si1 151.9(3) . . . . ? C8 N3 N4 C10 -1.1(5) . . . . ? C6 N3 N4 C10 -177.8(3) . . . . ? N1 P1 C1 C2 150.3(3) . . . . ? C18 P1 C1 C2 -89.5(3) . . . . ? C12 P1 C1 C2 30.3(3) . . . . ? Sn1 P1 C1 C2 133.0(3) . . . . ? N1 P1 C1 Sn1 17.32(15) . . . . ? C18 P1 C1 Sn1 137.57(14) . . . . ? C12 P1 C1 Sn1 -102.64(15) . . . . ? N1 P1 C1 Sn1 -77.05(16) . . . 2_677 ? C18 P1 C1 Sn1 43.2(2) . . . 2_677 ? C12 P1 C1 Sn1 162.99(14) . . . 2_677 ? Sn1 P1 C1 Sn1 -94.37(15) . . . 2_677 ? N1 Sn1 C1 C2 -146.2(3) . . . . ? C1 Sn1 C1 C2 117.8(3) 2_677 . . . ? P1 Sn1 C1 C2 -133.4(3) . . . . ? N1 Sn1 C1 P1 -12.79(11) . . . . ? C1 Sn1 C1 P1 -108.82(16) 2_677 . . . ? N1 Sn1 C1 Sn1 96.03(12) . . . 2_677 ? C1 Sn1 C1 Sn1 -0.002(2) 2_677 . . 2_677 ? P1 Sn1 C1 Sn1 108.82(16) . . . 2_677 ? C6 N2 C2 C3 -2.5(5) . . . . ? C6 N2 C2 C1 179.5(3) . . . . ? P1 C1 C2 N2 -129.2(3) . . . . ? Sn1 C1 C2 N2 -10.4(4) . . . . ? Sn1 C1 C2 N2 98.9(3) 2_677 . . . ? P1 C1 C2 C3 52.9(4) . . . . ? Sn1 C1 C2 C3 171.7(3) . . . . ? Sn1 C1 C2 C3 -79.0(3) 2_677 . . . ? N2 C2 C3 C4 3.5(5) . . . . ? C1 C2 C3 C4 -178.7(3) . . . . ? C2 C3 C4 C5 -1.2(6) . . . . ? C3 C4 C5 C6 -1.9(6) . . . . ? C2 N2 C6 C5 -0.7(5) . . . . ? C2 N2 C6 N3 179.3(3) . . . . ? C4 C5 C6 N2 3.0(6) . . . . ? C4 C5 C6 N3 -177.0(4) . . . . ? C8 N3 C6 N2 39.6(5) . . . . ? N4 N3 C6 N2 -144.3(3) . . . . ? C8 N3 C6 C5 -140.4(4) . . . . ? N4 N3 C6 C5 35.7(5) . . . . ? N4 N3 C8 C9 1.0(5) . . . . ? C6 N3 C8 C9 177.2(4) . . . . ? N4 N3 C8 C7 -174.8(4) . . . . ? C6 N3 C8 C7 1.4(7) . . . . ? N3 C8 C9 C10 -0.5(5) . . . . ? C7 C8 C9 C10 174.9(5) . . . . ? N3 N4 C10 C9 0.7(5) . . . . ? N3 N4 C10 C11 179.4(4) . . . . ? C8 C9 C10 N4 -0.1(5) . . . . ? C8 C9 C10 C11 -178.7(5) . . . . ? N1 P1 C12 C13 86.2(3) . . . . ? C1 P1 C12 C13 -161.0(3) . . . . ? C18 P1 C12 C13 -35.1(3) . . . . ? Sn1 P1 C12 C13 142.6(3) . . . . ? N1 P1 C12 C17 -86.2(3) . . . . ? C1 P1 C12 C17 26.6(3) . . . . ? C18 P1 C12 C17 152.5(3) . . . . ? Sn1 P1 C12 C17 -29.8(3) . . . . ? C17 C12 C13 C14 -0.9(6) . . . . ? P1 C12 C13 C14 -173.3(3) . . . . ? C12 C13 C14 C15 0.5(7) . . . . ? C13 C14 C15 C16 -0.3(7) . . . . ? C14 C15 C16 C17 0.6(7) . . . . ? C15 C16 C17 C12 -1.0(6) . . . . ? C13 C12 C17 C16 1.1(6) . . . . ? P1 C12 C17 C16 173.8(3) . . . . ? N1 P1 C18 C19 23.2(3) . . . . ? C1 P1 C18 C19 -91.0(3) . . . . ? C12 P1 C18 C19 145.2(3) . . . . ? Sn1 P1 C18 C19 -31.3(4) . . . . ? N1 P1 C18 C23 -161.6(3) . . . . ? C1 P1 C18 C23 84.2(3) . . . . ? C12 P1 C18 C23 -39.6(3) . . . . ? Sn1 P1 C18 C23 143.9(2) . . . . ? C23 C18 C19 C20 1.3(6) . . . . ? P1 C18 C19 C20 176.6(3) . . . . ? C18 C19 C20 C21 -0.8(6) . . . . ? C19 C20 C21 C22 0.1(7) . . . . ? C20 C21 C22 C23 0.0(7) . . . . ? C21 C22 C23 C18 0.5(6) . . . . ? C19 C18 C23 C22 -1.1(5) . . . . ? P1 C18 C23 C22 -176.3(3) . . . . ? C27 C28 C29 C29 175.1(10) . . . 2_666 ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.484 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.066 #====END data_4 _database_code_depnum_ccdc_archive 'CCDC 725692' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C59 H66 N8 P2 Pb2 Si2' _chemical_formula_weight 1419.70 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.9080(9) _cell_length_b 12.6483(12) _cell_length_c 12.8690(12) _cell_angle_alpha 98.5150(10) _cell_angle_beta 107.2790(10) _cell_angle_gamma 98.784(2) _cell_volume 1489.6(2) _cell_formula_units_Z 1 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 5289 _cell_measurement_theta_min 2.61 _cell_measurement_theta_max 26.36 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.14 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.583 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 698 _exptl_absorpt_coefficient_mu 5.781 _exptl_absorpt_correction_type MULTI-SCAN _exptl_absorpt_correction_T_min 0.771502 _exptl_absorpt_correction_T_max 1.000000 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 8465 _diffrn_reflns_av_R_equivalents 0.0169 _diffrn_reflns_av_sigmaI/netI 0.0342 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 1.66 _diffrn_reflns_theta_max 26.38 _reflns_number_total 5991 _reflns_number_gt 5201 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0310P)^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 5991 _refine_ls_number_parameters 354 _refine_ls_number_restraints 86 _refine_ls_R_factor_all 0.0333 _refine_ls_R_factor_gt 0.0245 _refine_ls_wR_factor_ref 0.0590 _refine_ls_wR_factor_gt 0.0552 _refine_ls_goodness_of_fit_ref 1.013 _refine_ls_restrained_S_all 1.014 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb -0.175230(9) 0.523888(7) -0.043005(7) 0.04278(3) Uani 1 1 d . . . P1 P 0.06655(6) 0.58057(5) 0.21825(5) 0.03903(15) Uani 1 1 d . . . Si1 Si 0.14562(8) 0.37076(6) 0.28848(6) 0.04676(18) Uani 1 1 d . . . C1 C -0.0974(3) 0.5862(2) 0.25335(19) 0.0456(6) Uani 1 1 d . . . N1 N 0.0933(2) 0.45827(15) 0.20081(15) 0.0410(5) Uani 1 1 d . . . N2 N 0.1919(2) 0.74136(16) 0.01707(16) 0.0448(5) Uani 1 1 d . . . N3 N 0.3275(2) 0.85374(19) -0.06024(18) 0.0583(7) Uani 1 1 d . . . N4 N 0.3180(3) 0.9316(2) -0.1251(2) 0.0697(8) Uani 1 1 d . . . C2 C -0.1215(3) 0.6838(2) 0.3034(2) 0.0580(7) Uani 1 1 d . . . H2 H -0.0494 0.7468 0.3247 0.070 Uiso 1 1 calc R . . C3 C -0.2502(3) 0.6882(3) 0.3214(3) 0.0771(9) Uani 1 1 d . . . H3 H -0.2645 0.7535 0.3559 0.092 Uiso 1 1 calc R . . C4 C -0.3586(3) 0.5955(3) 0.2884(3) 0.0832(11) Uani 1 1 d . . . H4 H -0.4466 0.5991 0.2993 0.100 Uiso 1 1 calc R . . C5 C -0.3373(3) 0.4984(3) 0.2397(3) 0.0764(10) Uani 1 1 d . . . H5 H -0.4098 0.4357 0.2190 0.092 Uiso 1 1 calc R . . C6 C -0.2062(3) 0.4940(2) 0.2213(2) 0.0571(8) Uani 1 1 d . . . H6 H -0.1921 0.4283 0.1872 0.068 Uiso 1 1 calc R . . C7 C 0.2092(3) 0.6724(2) 0.33522(19) 0.0439(6) Uani 1 1 d . . . C8 C 0.2095(3) 0.6746(2) 0.4435(2) 0.0581(8) Uani 1 1 d . . . H8 H 0.1299 0.6364 0.4561 0.070 Uiso 1 1 calc R . . C9 C 0.3266(3) 0.7330(3) 0.5326(2) 0.0717(10) Uani 1 1 d . . . H9 H 0.3260 0.7327 0.6047 0.086 Uiso 1 1 calc R . . C10 C 0.4440(3) 0.7915(3) 0.5156(3) 0.0726(10) Uani 1 1 d . . . H10 H 0.5225 0.8312 0.5759 0.087 Uiso 1 1 calc R . . C11 C 0.4449(3) 0.7910(3) 0.4090(3) 0.0682(9) Uani 1 1 d . . . H11 H 0.5240 0.8309 0.3972 0.082 Uiso 1 1 calc R . . C12 C 0.3281(3) 0.7314(2) 0.3188(2) 0.0534(7) Uani 1 1 d . . . H12 H 0.3300 0.7311 0.2470 0.064 Uiso 1 1 calc R . . C13 C 0.0604(2) 0.61552(19) 0.09126(18) 0.0412(6) Uani 1 1 d . . . C14 C 0.0977(3) 0.72615(19) 0.07443(19) 0.0422(6) Uani 1 1 d . . . C15 C 0.0399(3) 0.8127(2) 0.1110(2) 0.0530(7) Uani 1 1 d . . . H15 H -0.0258 0.8015 0.1490 0.064 Uiso 1 1 calc R . . C16 C 0.0798(3) 0.9150(2) 0.0907(2) 0.0616(8) Uani 1 1 d . . . H16 H 0.0414 0.9728 0.1151 0.074 Uiso 1 1 calc R . . C17 C 0.1767(3) 0.9311(2) 0.0343(2) 0.0609(8) Uani 1 1 d . . . H17 H 0.2064 0.9995 0.0205 0.073 Uiso 1 1 calc R . . C18 C 0.2282(3) 0.8416(2) -0.0010(2) 0.0495(7) Uani 1 1 d . . . C19 C 0.4884(3) 0.7263(3) 0.0117(3) 0.0800(11) Uani 1 1 d . . . H19A H 0.4886 0.7528 0.0856 0.120 Uiso 1 1 calc R . . H19B H 0.5841 0.7186 0.0139 0.120 Uiso 1 1 calc R . . H19C H 0.4232 0.6565 -0.0185 0.120 Uiso 1 1 calc R . . C20 C 0.4412(3) 0.8042(2) -0.0589(2) 0.0612(8) Uani 1 1 d . . . C21 C 0.5023(4) 0.8503(3) -0.1278(3) 0.0793(10) Uani 1 1 d . . . H21 H 0.5813 0.8331 -0.1463 0.095 Uiso 1 1 calc R . . C22 C 0.4253(4) 0.9274(3) -0.1653(3) 0.0767(10) Uani 1 1 d . . . C23 C 0.4530(4) 1.0055(3) -0.2383(3) 0.0997(14) Uani 1 1 d . . . H23A H 0.4453 0.9647 -0.3097 0.150 Uiso 1 1 calc R . . H23B H 0.5483 1.0502 -0.2042 0.150 Uiso 1 1 calc R . . H23C H 0.3830 1.0511 -0.2473 0.150 Uiso 1 1 calc R . . C24 C 0.3300(4) 0.4241(3) 0.3878(3) 0.1038(15) Uani 1 1 d . . . H24A H 0.3951 0.4429 0.3479 0.156 Uiso 1 1 calc R . . H24B H 0.3602 0.3691 0.4282 0.156 Uiso 1 1 calc R . . H24C H 0.3305 0.4878 0.4388 0.156 Uiso 1 1 calc R . . C25 C 0.0220(4) 0.3442(3) 0.3686(3) 0.1086(11) Uani 1 1 d . . . H25A H 0.0132 0.4123 0.4074 0.163 Uiso 1 1 calc R . . H25B H 0.0598 0.3008 0.4212 0.163 Uiso 1 1 calc R . . H25C H -0.0713 0.3055 0.3188 0.163 Uiso 1 1 calc R . . C26 C 0.1485(4) 0.2420(2) 0.2018(3) 0.0841(11) Uani 1 1 d . . . H26A H 0.0524 0.2089 0.1530 0.126 Uiso 1 1 calc R . . H26B H 0.1841 0.1931 0.2487 0.126 Uiso 1 1 calc R . . H26C H 0.2105 0.2568 0.1586 0.126 Uiso 1 1 calc R . . C27 C 0.0778(5) 0.9596(4) 0.5520(4) 0.094(3) Uani 0.50 1 d PGDU . 1 H27A H 0.1078 0.9283 0.6165 0.113 Uiso 0.50 1 d PR . 1 C28 C 0.1610(6) 0.9624(5) 0.4821(5) 0.134(3) Uani 0.50 1 d PGU . 1 H28A H 0.2483 0.9347 0.4995 0.161 Uiso 0.50 1 d PR . 1 C29 C 0.1180(8) 1.0054(6) 0.3870(5) 0.129(3) Uani 0.50 1 d PGU . 1 H29A H 0.1755 1.0073 0.3387 0.155 Uiso 0.50 1 d PR . 1 C30 C -0.0084(8) 1.0456(6) 0.3618(5) 0.126(3) Uani 0.50 1 d PGU . 1 H30A H -0.0381 1.0752 0.2961 0.152 Uiso 0.50 1 d PR . 1 C31 C -0.0917(7) 1.0428(6) 0.4317(5) 0.162(5) Uani 0.50 1 d PGDU . 1 H31A H -0.1789 1.0705 0.4143 0.194 Uiso 0.50 1 d PR . 1 C32 C -0.0486(6) 0.9998(5) 0.5267(4) 0.109(3) Uani 0.50 1 d PGU . 1 C33 C -0.1466(8) 0.9936(10) 0.6005(7) 0.188(5) Uani 0.50 1 d PDU . 1 H33A H -0.2280 1.0261 0.5721 0.282 Uiso 0.50 1 d PR . 1 H33B H -0.1802 0.9188 0.6022 0.282 Uiso 0.50 1 d PR . 1 H33C H -0.0907 1.0329 0.6744 0.282 Uiso 0.50 1 d PR . 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.04671(4) 0.04887(5) 0.04023(4) 0.01306(3) 0.01924(3) 0.01808(4) P1 0.0467(3) 0.0414(3) 0.0337(3) 0.0102(2) 0.0169(2) 0.0131(2) Si1 0.0558(4) 0.0485(4) 0.0399(3) 0.0186(3) 0.0145(3) 0.0157(3) C1 0.0506(12) 0.0548(14) 0.0378(11) 0.0138(10) 0.0195(9) 0.0159(11) N1 0.0519(10) 0.0420(10) 0.0342(9) 0.0129(8) 0.0167(8) 0.0145(8) N2 0.0499(10) 0.0425(10) 0.0434(10) 0.0126(8) 0.0150(8) 0.0108(9) N3 0.0610(12) 0.0562(13) 0.0558(12) 0.0193(10) 0.0193(10) -0.0008(11) N4 0.0794(16) 0.0620(14) 0.0614(13) 0.0237(11) 0.0184(12) -0.0051(13) C2 0.0666(14) 0.0621(16) 0.0581(14) 0.0144(12) 0.0335(12) 0.0229(13) C3 0.0849(17) 0.085(2) 0.0833(19) 0.0200(16) 0.0476(15) 0.0408(16) C4 0.0637(15) 0.117(3) 0.088(2) 0.0251(19) 0.0428(14) 0.0356(17) C5 0.0569(15) 0.092(2) 0.086(2) 0.0163(18) 0.0352(14) 0.0087(16) C6 0.0558(14) 0.0647(17) 0.0547(14) 0.0135(13) 0.0214(12) 0.0167(13) C7 0.0505(12) 0.0447(13) 0.0397(12) 0.0091(10) 0.0158(10) 0.0164(10) C8 0.0646(15) 0.0639(17) 0.0452(13) 0.0097(12) 0.0197(12) 0.0097(14) C9 0.0806(19) 0.082(2) 0.0433(15) 0.0009(15) 0.0122(14) 0.0163(17) C10 0.0626(18) 0.077(2) 0.0609(18) -0.0027(16) 0.0027(15) 0.0141(16) C11 0.0506(15) 0.0714(19) 0.079(2) 0.0118(16) 0.0195(14) 0.0070(14) C12 0.0529(13) 0.0625(16) 0.0481(13) 0.0105(12) 0.0196(11) 0.0164(12) C13 0.0504(12) 0.0419(12) 0.0368(11) 0.0130(9) 0.0181(9) 0.0134(10) C14 0.0488(12) 0.0395(12) 0.0344(11) 0.0073(9) 0.0073(10) 0.0109(10) C15 0.0691(14) 0.0500(14) 0.0509(13) 0.0170(11) 0.0264(11) 0.0251(12) C16 0.0798(17) 0.0432(14) 0.0634(16) 0.0123(12) 0.0194(14) 0.0241(13) C17 0.0697(17) 0.0429(13) 0.0664(17) 0.0181(12) 0.0159(14) 0.0072(13) C18 0.0516(13) 0.0453(13) 0.0484(13) 0.0142(11) 0.0109(11) 0.0075(11) C19 0.0704(17) 0.081(2) 0.093(2) 0.0147(18) 0.0313(17) 0.0238(17) C20 0.0585(15) 0.0565(17) 0.0639(16) 0.0057(14) 0.0220(13) 0.0005(13) C21 0.0789(18) 0.069(2) 0.085(2) -0.0046(17) 0.0427(16) -0.0119(17) C22 0.090(2) 0.068(2) 0.0572(16) 0.0011(15) 0.0272(15) -0.0213(18) C23 0.128(3) 0.092(3) 0.0659(19) 0.0199(18) 0.0341(19) -0.024(2) C24 0.093(3) 0.086(2) 0.099(3) 0.025(2) -0.024(2) 0.023(2) C25 0.142(2) 0.127(2) 0.126(2) 0.0943(17) 0.0921(18) 0.068(2) C26 0.125(3) 0.0616(17) 0.0682(19) 0.0200(15) 0.0175(18) 0.0479(17) C27 0.106(5) 0.085(4) 0.087(4) 0.038(3) 0.010(4) 0.030(4) C28 0.134(6) 0.113(5) 0.139(6) 0.022(5) 0.018(5) 0.032(5) C29 0.144(5) 0.120(6) 0.118(5) 0.001(4) 0.057(4) 0.004(5) C30 0.126(5) 0.125(5) 0.126(5) 0.044(4) 0.031(4) 0.024(4) C31 0.166(7) 0.158(7) 0.156(7) 0.042(5) 0.041(5) 0.027(6) C32 0.111(5) 0.102(5) 0.108(5) 0.019(4) 0.035(4) 0.007(4) C33 0.203(7) 0.177(7) 0.172(7) 0.020(6) 0.061(6) 0.021(6) _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 C13 2.345(2) 2_565 ? Pb1 N1 2.428(2) 2_565 ? Pb1 C13 2.442(2) . ? Pb1 P1 2.9976(7) 2_565 ? Pb1 Pb1 3.4933(3) 2_565 ? P1 N1 1.604(2) . ? P1 C13 1.741(2) . ? P1 C1 1.819(3) . ? P1 C7 1.825(2) . ? P1 Pb1 2.9976(7) 2_565 ? Si1 N1 1.722(2) . ? Si1 C26 1.842(3) . ? Si1 C25 1.845(4) . ? Si1 C24 1.846(3) . ? C1 C6 1.380(4) . ? C1 C2 1.393(4) . ? N1 Pb1 2.427(2) 2_565 ? N2 C18 1.337(3) . ? N2 C14 1.360(3) . ? N3 C20 1.368(4) . ? N3 N4 1.378(3) . ? N3 C18 1.417(4) . ? N4 C22 1.318(5) . ? C2 C3 1.370(4) . ? C3 C4 1.380(5) . ? C4 C5 1.370(5) . ? C5 C6 1.395(4) . ? C7 C12 1.384(4) . ? C7 C8 1.389(4) . ? C8 C9 1.380(4) . ? C9 C10 1.373(5) . ? C10 C11 1.373(5) . ? C11 C12 1.389(4) . ? C13 C14 1.456(3) . ? C13 Pb1 2.345(2) 2_565 ? C14 C15 1.396(4) . ? C15 C16 1.379(4) . ? C16 C17 1.373(4) . ? C17 C18 1.383(4) . ? C19 C20 1.473(5) . ? C20 C21 1.363(5) . ? C21 C22 1.383(5) . ? C22 C23 1.508(5) . ? C27 C31 0.224(9) 2_576 ? C27 C32 1.182(9) 2_576 ? C27 C28 1.3900 . ? C27 C32 1.3900 . ? C27 C30 1.473(10) 2_576 ? C28 C33 1.252(12) 2_576 ? C28 C32 1.259(11) 2_576 ? C28 C29 1.3900 . ? C28 C31 1.473(11) 2_576 ? C29 C33 0.279(11) 2_576 ? C29 C30 1.3900 . ? C29 C32 1.473(10) 2_576 ? C30 C31 1.3900 . ? C30 C27 1.473(10) 2_576 ? C30 C32 1.602(9) 2_576 ? C30 C33 1.644(12) 2_576 ? C31 C27 0.224(9) 2_576 ? C31 C32 1.3900 . ? C31 C28 1.473(14) 2_576 ? C31 C32 1.542(10) 2_576 ? C32 C27 1.182(10) 2_576 ? C32 C28 1.259(10) 2_576 ? C32 C32 1.340(11) 2_576 ? C32 C29 1.473(11) 2_576 ? C32 C31 1.542(10) 2_576 ? C32 C33 1.548(7) . ? C32 C30 1.602(11) 2_576 ? C33 C29 0.279(12) 2_576 ? C33 C28 1.252(15) 2_576 ? C33 C30 1.644(13) 2_576 ? 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 C13 Pb1 N1 66.25(8) 2_565 2_565 ? C13 Pb1 C13 86.28(8) 2_565 . ? N1 Pb1 C13 92.85(7) 2_565 . ? C13 Pb1 P1 35.45(6) 2_565 2_565 ? N1 Pb1 P1 32.26(5) 2_565 2_565 ? C13 Pb1 P1 97.04(6) . 2_565 ? C13 Pb1 Pb1 44.23(5) 2_565 2_565 ? N1 Pb1 Pb1 76.37(4) 2_565 2_565 ? C13 Pb1 Pb1 42.05(6) . 2_565 ? P1 Pb1 Pb1 62.546(12) 2_565 2_565 ? N1 P1 C13 102.42(11) . . ? N1 P1 C1 111.47(11) . . ? C13 P1 C1 114.03(11) . . ? N1 P1 C7 112.38(11) . . ? C13 P1 C7 112.61(11) . . ? C1 P1 C7 104.23(11) . . ? N1 P1 Pb1 53.90(7) . 2_565 ? C13 P1 Pb1 51.35(8) . 2_565 ? C1 P1 Pb1 142.43(8) . 2_565 ? C7 P1 Pb1 113.34(9) . 2_565 ? N1 Si1 C26 107.32(12) . . ? N1 Si1 C25 112.14(14) . . ? C26 Si1 C25 109.99(17) . . ? N1 Si1 C24 111.91(15) . . ? C26 Si1 C24 107.21(18) . . ? C25 Si1 C24 108.15(19) . . ? C6 C1 C2 118.7(2) . . ? C6 C1 P1 119.4(2) . . ? C2 C1 P1 121.64(19) . . ? P1 N1 Si1 134.38(12) . . ? P1 N1 Pb1 93.84(9) . 2_565 ? Si1 N1 Pb1 123.90(10) . 2_565 ? C18 N2 C14 117.8(2) . . ? C20 N3 N4 112.3(3) . . ? C20 N3 C18 130.0(2) . . ? N4 N3 C18 117.5(2) . . ? C22 N4 N3 103.9(3) . . ? C3 C2 C1 120.8(3) . . ? C2 C3 C4 119.9(3) . . ? C5 C4 C3 120.4(3) . . ? C4 C5 C6 119.6(3) . . ? C1 C6 C5 120.5(3) . . ? C12 C7 C8 118.4(2) . . ? C12 C7 P1 120.35(19) . . ? C8 C7 P1 120.8(2) . . ? C9 C8 C7 120.7(3) . . ? C10 C9 C8 120.5(3) . . ? C9 C10 C11 119.5(3) . . ? C10 C11 C12 120.4(3) . . ? C7 C12 C11 120.5(3) . . ? C14 C13 P1 125.32(17) . . ? C14 C13 Pb1 122.65(17) . 2_565 ? P1 C13 Pb1 93.20(10) . 2_565 ? C14 C13 Pb1 109.48(15) . . ? P1 C13 Pb1 107.36(11) . . ? Pb1 C13 Pb1 93.72(8) 2_565 . ? N2 C14 C15 120.4(2) . . ? N2 C14 C13 115.9(2) . . ? C15 C14 C13 123.7(2) . . ? C16 C15 C14 120.1(3) . . ? C17 C16 C15 119.7(3) . . ? C16 C17 C18 117.3(3) . . ? N2 C18 C17 124.7(3) . . ? N2 C18 N3 115.8(2) . . ? C17 C18 N3 119.4(2) . . ? C21 C20 N3 104.6(3) . . ? C21 C20 C19 130.2(3) . . ? N3 C20 C19 125.0(3) . . ? C20 C21 C22 107.6(3) . . ? N4 C22 C21 111.6(3) . . ? N4 C22 C23 119.3(4) . . ? C21 C22 C23 129.0(4) . . ? C31 C27 C32 156(3) 2_576 2_576 ? C31 C27 C28 108(3) 2_576 . ? C32 C27 C28 57.9(5) 2_576 . ? C31 C27 C32 130(3) 2_576 . ? C32 C27 C32 62.2(5) 2_576 . ? C28 C27 C32 120.0 . . ? C31 C27 C30 64(3) 2_576 2_576 ? C32 C27 C30 129.8(8) 2_576 2_576 ? C28 C27 C30 171.7(5) . 2_576 ? C32 C27 C30 68.0(5) . 2_576 ? C33 C28 C32 76.1(6) 2_576 2_576 ? C33 C28 C29 10.6(5) 2_576 . ? C32 C28 C29 67.4(4) 2_576 . ? C33 C28 C27 128.8(6) 2_576 . ? C32 C28 C27 52.7(4) 2_576 . ? C29 C28 C27 120.0 . . ? C33 C28 C31 136.3(8) 2_576 2_576 ? C32 C28 C31 60.6(4) 2_576 2_576 ? C29 C28 C31 127.9(4) . 2_576 ? C27 C28 C31 8.3(4) . 2_576 ? C33 C29 C28 55(2) 2_576 . ? C33 C29 C30 153(3) 2_576 . ? C28 C29 C30 120.0 . . ? C33 C29 C32 100(2) 2_576 2_576 ? C28 C29 C32 52.1(4) . 2_576 ? C30 C29 C32 68.0(4) . 2_576 ? C31 C30 C29 120.0 . . ? C31 C30 C27 8.3(4) . 2_576 ? C29 C30 C27 112.0(4) . 2_576 ? C31 C30 C32 61.6(4) . 2_576 ? C29 C30 C32 58.5(4) . 2_576 ? C27 C30 C32 53.5(3) 2_576 2_576 ? C31 C30 C33 118.5(4) . 2_576 ? C29 C30 C33 4.4(5) . 2_576 ? C27 C30 C33 110.4(6) 2_576 2_576 ? C32 C30 C33 57.0(4) 2_576 2_576 ? C27 C31 C30 108(3) 2_576 . ? C27 C31 C32 20(3) 2_576 . ? C30 C31 C32 120.0 . . ? C27 C31 C28 64(3) 2_576 2_576 ? C30 C31 C28 171.7(5) . 2_576 ? C32 C31 C28 52.1(5) . 2_576 ? C27 C31 C32 44(2) 2_576 2_576 ? C30 C31 C32 66.0(4) . 2_576 ? C32 C31 C32 54.1(4) . 2_576 ? C28 C31 C32 105.9(6) 2_576 2_576 ? C27 C32 C28 69.3(7) 2_576 2_576 ? C27 C32 C32 66.6(5) 2_576 2_576 ? C28 C32 C32 135.8(9) 2_576 2_576 ? C27 C32 C31 3.8(5) 2_576 . ? C28 C32 C31 67.4(7) 2_576 . ? C32 C32 C31 68.8(4) 2_576 . ? C27 C32 C27 117.8(5) 2_576 . ? C28 C32 C27 172.1(7) 2_576 . ? C32 C32 C27 51.3(4) 2_576 . ? C31 C32 C27 120.0 . . ? C27 C32 C29 129.8(9) 2_576 2_576 ? C28 C32 C29 60.6(4) 2_576 2_576 ? C32 C32 C29 162.5(8) 2_576 2_576 ? C31 C32 C29 127.9(6) . 2_576 ? C27 C32 C29 112.0(6) . 2_576 ? C27 C32 C31 123.6(8) 2_576 2_576 ? C28 C32 C31 165.7(9) 2_576 2_576 ? C32 C32 C31 57.2(4) 2_576 2_576 ? C31 C32 C31 125.9(4) . 2_576 ? C27 C32 C31 6.4(4) . 2_576 ? C29 C32 C31 105.9(7) 2_576 2_576 ? C27 C32 C33 121.0(7) 2_576 . ? C28 C32 C33 51.7(7) 2_576 . ? C32 C32 C33 172.4(6) 2_576 . ? C31 C32 C33 118.8(4) . . ? C27 C32 C33 121.1(4) . . ? C29 C32 C33 10.2(5) 2_576 . ? C31 C32 C33 115.2(5) 2_576 . ? C27 C32 C30 173.5(9) 2_576 2_576 ? C28 C32 C30 114.0(7) 2_576 2_576 ? C32 C32 C30 109.5(6) 2_576 2_576 ? C31 C32 C30 177.2(5) . 2_576 ? C27 C32 C30 58.5(5) . 2_576 ? C29 C32 C30 53.5(4) 2_576 2_576 ? C31 C32 C30 52.4(3) 2_576 2_576 ? C33 C32 C30 62.9(5) . 2_576 ? C29 C33 C28 114(3) 2_576 2_576 ? C29 C33 C32 69(2) 2_576 . ? C28 C33 C32 52.1(5) 2_576 . ? C29 C33 C30 23(3) 2_576 2_576 ? C28 C33 C30 111.8(8) 2_576 2_576 ? C32 C33 C30 60.2(4) . 2_576 ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N1 P1 C1 C6 -24.7(2) . . . . ? C13 P1 C1 C6 90.6(2) . . . . ? C7 P1 C1 C6 -146.2(2) . . . . ? Pb1 P1 C1 C6 33.4(3) 2_565 . . . ? N1 P1 C1 C2 160.9(2) . . . . ? C13 P1 C1 C2 -83.7(2) . . . . ? C7 P1 C1 C2 39.5(2) . . . . ? Pb1 P1 C1 C2 -140.89(17) 2_565 . . . ? C13 P1 N1 Si1 165.78(17) . . . . ? C1 P1 N1 Si1 -71.91(19) . . . . ? C7 P1 N1 Si1 44.7(2) . . . . ? Pb1 P1 N1 Si1 148.0(2) 2_565 . . . ? C13 P1 N1 Pb1 17.80(10) . . . 2_565 ? C1 P1 N1 Pb1 140.11(9) . . . 2_565 ? C7 P1 N1 Pb1 -103.29(10) . . . 2_565 ? C26 Si1 N1 P1 179.19(19) . . . . ? C25 Si1 N1 P1 58.3(2) . . . . ? C24 Si1 N1 P1 -63.5(2) . . . . ? C26 Si1 N1 Pb1 -40.41(17) . . . 2_565 ? C25 Si1 N1 Pb1 -161.31(14) . . . 2_565 ? C24 Si1 N1 Pb1 76.94(19) . . . 2_565 ? C20 N3 N4 C22 1.3(3) . . . . ? C18 N3 N4 C22 177.5(2) . . . . ? C6 C1 C2 C3 0.6(4) . . . . ? P1 C1 C2 C3 175.0(2) . . . . ? C1 C2 C3 C4 -1.0(5) . . . . ? C2 C3 C4 C5 1.4(5) . . . . ? C3 C4 C5 C6 -1.4(5) . . . . ? C2 C1 C6 C5 -0.6(4) . . . . ? P1 C1 C6 C5 -175.1(2) . . . . ? C4 C5 C6 C1 1.0(5) . . . . ? N1 P1 C7 C12 91.5(2) . . . . ? C13 P1 C7 C12 -23.5(3) . . . . ? C1 P1 C7 C12 -147.6(2) . . . . ? Pb1 P1 C7 C12 32.6(2) 2_565 . . . ? N1 P1 C7 C8 -80.6(2) . . . . ? C13 P1 C7 C8 164.3(2) . . . . ? C1 P1 C7 C8 40.2(3) . . . . ? Pb1 P1 C7 C8 -139.5(2) 2_565 . . . ? C12 C7 C8 C9 -0.9(4) . . . . ? P1 C7 C8 C9 171.4(2) . . . . ? C7 C8 C9 C10 1.1(5) . . . . ? C8 C9 C10 C11 -0.5(5) . . . . ? C9 C10 C11 C12 -0.3(5) . . . . ? C8 C7 C12 C11 0.1(4) . . . . ? P1 C7 C12 C11 -172.2(2) . . . . ? C10 C11 C12 C7 0.5(5) . . . . ? N1 P1 C13 C14 -153.0(2) . . . . ? C1 P1 C13 C14 86.4(2) . . . . ? C7 P1 C13 C14 -32.1(3) . . . . ? Pb1 P1 C13 C14 -134.6(2) 2_565 . . . ? N1 P1 C13 Pb1 -18.44(10) . . . 2_565 ? C1 P1 C13 Pb1 -139.00(10) . . . 2_565 ? C7 P1 C13 Pb1 102.50(11) . . . 2_565 ? N1 P1 C13 Pb1 76.47(12) . . . . ? C1 P1 C13 Pb1 -44.09(14) . . . . ? C7 P1 C13 Pb1 -162.60(10) . . . . ? Pb1 P1 C13 Pb1 94.91(10) 2_565 . . . ? C13 Pb1 C13 C14 126.6(2) 2_565 . . . ? N1 Pb1 C13 C14 60.65(17) 2_565 . . . ? P1 Pb1 C13 C14 92.77(16) 2_565 . . . ? Pb1 Pb1 C13 C14 126.6(2) 2_565 . . . ? C13 Pb1 C13 P1 -94.53(12) 2_565 . . . ? N1 Pb1 C13 P1 -160.49(11) 2_565 . . . ? P1 Pb1 C13 P1 -128.37(10) 2_565 . . . ? Pb1 Pb1 C13 P1 -94.53(13) 2_565 . . . ? C13 Pb1 C13 Pb1 0.0 2_565 . . 2_565 ? N1 Pb1 C13 Pb1 -65.96(8) 2_565 . . 2_565 ? P1 Pb1 C13 Pb1 -33.85(7) 2_565 . . 2_565 ? C18 N2 C14 C15 1.1(3) . . . . ? C18 N2 C14 C13 179.5(2) . . . . ? P1 C13 C14 N2 129.7(2) . . . . ? Pb1 C13 C14 N2 7.3(3) 2_565 . . . ? Pb1 C13 C14 N2 -100.64(19) . . . . ? P1 C13 C14 C15 -52.0(3) . . . . ? Pb1 C13 C14 C15 -174.35(17) 2_565 . . . ? Pb1 C13 C14 C15 77.7(2) . . . . ? N2 C14 C15 C16 -1.1(4) . . . . ? C13 C14 C15 C16 -179.4(2) . . . . ? C14 C15 C16 C17 0.1(4) . . . . ? C15 C16 C17 C18 0.9(4) . . . . ? C14 N2 C18 C17 -0.1(3) . . . . ? C14 N2 C18 N3 179.50(19) . . . . ? C16 C17 C18 N2 -0.9(4) . . . . ? C16 C17 C18 N3 179.5(2) . . . . ? C20 N3 C18 N2 -34.6(4) . . . . ? N4 N3 C18 N2 150.0(2) . . . . ? C20 N3 C18 C17 145.0(3) . . . . ? N4 N3 C18 C17 -30.4(3) . . . . ? N4 N3 C20 C21 -1.8(3) . . . . ? C18 N3 C20 C21 -177.4(2) . . . . ? N4 N3 C20 C19 173.3(3) . . . . ? C18 N3 C20 C19 -2.3(4) . . . . ? N3 C20 C21 C22 1.5(3) . . . . ? C19 C20 C21 C22 -173.2(3) . . . . ? N3 N4 C22 C21 -0.3(3) . . . . ? N3 N4 C22 C23 -177.8(2) . . . . ? C20 C21 C22 N4 -0.8(4) . . . . ? C20 C21 C22 C23 176.4(3) . . . . ? C31 C27 C28 C33 -155(3) 2_576 . . 2_576 ? C32 C27 C28 C33 3.4(8) 2_576 . . 2_576 ? C32 C27 C28 C33 7.1(9) . . . 2_576 ? C30 C27 C28 C33 -155(4) 2_576 . . 2_576 ? C31 C27 C28 C32 -159(3) 2_576 . . 2_576 ? C32 C27 C28 C32 3.7(5) . . . 2_576 ? C30 C27 C28 C32 -159(4) 2_576 . . 2_576 ? C31 C27 C28 C29 -163(3) 2_576 . . . ? C32 C27 C28 C29 -3.7(5) 2_576 . . . ? C32 C27 C28 C29 0.0 . . . . ? C30 C27 C28 C29 -163(4) 2_576 . . . ? C32 C27 C28 C31 159(3) 2_576 . . 2_576 ? C32 C27 C28 C31 163(3) . . . 2_576 ? C30 C27 C28 C31 0(2) 2_576 . . 2_576 ? C32 C28 C29 C33 145(4) 2_576 . . 2_576 ? C27 C28 C29 C33 148(4) . . . 2_576 ? C31 C28 C29 C33 145(4) 2_576 . . 2_576 ? C33 C28 C29 C30 -148(4) 2_576 . . . ? C32 C28 C29 C30 -3.2(5) 2_576 . . . ? C27 C28 C29 C30 0.0 . . . . ? C31 C28 C29 C30 -3.2(5) 2_576 . . . ? C33 C28 C29 C32 -145(4) 2_576 . . 2_576 ? C27 C28 C29 C32 3.2(5) . . . 2_576 ? C31 C28 C29 C32 0.0(4) 2_576 . . 2_576 ? C33 C29 C30 C31 -72(6) 2_576 . . . ? C28 C29 C30 C31 0.0 . . . . ? C32 C29 C30 C31 -2.7(4) 2_576 . . . ? C33 C29 C30 C27 -69(5) 2_576 . . 2_576 ? C28 C29 C30 C27 2.7(4) . . . 2_576 ? C32 C29 C30 C27 0.00(19) 2_576 . . 2_576 ? C33 C29 C30 C32 -69(5) 2_576 . . 2_576 ? C28 C29 C30 C32 2.7(4) . . . 2_576 ? C28 C29 C30 C33 72(6) . . . 2_576 ? C32 C29 C30 C33 69(5) 2_576 . . 2_576 ? C29 C30 C31 C27 17(3) . . . 2_576 ? C32 C30 C31 C27 15(3) 2_576 . . 2_576 ? C33 C30 C31 C27 13(3) 2_576 . . 2_576 ? C29 C30 C31 C32 0.0 . . . . ? C27 C30 C31 C32 -17(3) 2_576 . . . ? C32 C30 C31 C32 -2.6(4) 2_576 . . . ? C33 C30 C31 C32 -4.8(6) 2_576 . . . ? C29 C30 C31 C28 17(5) . . . 2_576 ? C27 C30 C31 C28 0(3) 2_576 . . 2_576 ? C32 C30 C31 C28 15(5) 2_576 . . 2_576 ? C33 C30 C31 C28 13(5) 2_576 . . 2_576 ? C29 C30 C31 C32 2.6(4) . . . 2_576 ? C27 C30 C31 C32 -15(3) 2_576 . . 2_576 ? C33 C30 C31 C32 -2.2(5) 2_576 . . 2_576 ? C30 C31 C32 C27 56(8) . . . 2_576 ? C28 C31 C32 C27 -121(8) 2_576 . . 2_576 ? C32 C31 C32 C27 53(8) 2_576 . . 2_576 ? C27 C31 C32 C28 121(8) 2_576 . . 2_576 ? C30 C31 C32 C28 176.8(10) . . . 2_576 ? C32 C31 C32 C28 173.9(13) 2_576 . . 2_576 ? C27 C31 C32 C32 -53(8) 2_576 . . 2_576 ? C30 C31 C32 C32 3.0(4) . . . 2_576 ? C28 C31 C32 C32 -173.9(13) 2_576 . . 2_576 ? C27 C31 C32 C27 -56(8) 2_576 . . . ? C30 C31 C32 C27 0.0 . . . . ? C28 C31 C32 C27 -176.8(10) 2_576 . . . ? C32 C31 C32 C27 -3.0(4) 2_576 . . . ? C27 C31 C32 C29 121(8) 2_576 . . 2_576 ? C30 C31 C32 C29 176.8(10) . . . 2_576 ? C28 C31 C32 C29 0.0(4) 2_576 . . 2_576 ? C32 C31 C32 C29 173.9(12) 2_576 . . 2_576 ? C27 C31 C32 C31 -53(8) 2_576 . . 2_576 ? C30 C31 C32 C31 2.9(4) . . . 2_576 ? C28 C31 C32 C31 -173.9(12) 2_576 . . 2_576 ? C32 C31 C32 C31 0.0(3) 2_576 . . 2_576 ? C27 C31 C32 C33 126(8) 2_576 . . . ? C30 C31 C32 C33 -177.6(7) . . . . ? C28 C31 C32 C33 5.5(8) 2_576 . . . ? C32 C31 C32 C33 179.4(8) 2_576 . . . ? C27 C31 C32 C30 0(8) 2_576 . . 2_576 ? C30 C31 C32 C30 56(10) . . . 2_576 ? C28 C31 C32 C30 -121(11) 2_576 . . 2_576 ? C32 C31 C32 C30 53(10) 2_576 . . 2_576 ? C31 C27 C32 C27 155(4) 2_576 . . 2_576 ? C32 C27 C32 C27 0.0(2) 2_576 . . 2_576 ? C28 C27 C32 C27 -3.5(6) . . . 2_576 ? C30 C27 C32 C27 173.8(11) 2_576 . . 2_576 ? C31 C27 C32 C28 0(6) 2_576 . . 2_576 ? C32 C27 C32 C28 -155(7) 2_576 . . 2_576 ? C28 C27 C32 C28 -158(7) . . . 2_576 ? C30 C27 C32 C28 19(6) 2_576 . . 2_576 ? C31 C27 C32 C32 155(4) 2_576 . . 2_576 ? C28 C27 C32 C32 -3.5(5) . . . 2_576 ? C30 C27 C32 C32 173.8(9) 2_576 . . 2_576 ? C31 C27 C32 C31 158(3) 2_576 . . . ? C32 C27 C32 C31 3.5(5) 2_576 . . . ? C28 C27 C32 C31 0.0 . . . . ? C30 C27 C32 C31 177.3(6) 2_576 . . . ? C31 C27 C32 C29 -19(3) 2_576 . . 2_576 ? C32 C27 C32 C29 -173.8(11) 2_576 . . 2_576 ? C28 C27 C32 C29 -177.3(8) . . . 2_576 ? C30 C27 C32 C29 0.0(4) 2_576 . . 2_576 ? C32 C27 C32 C31 -155(4) 2_576 . . 2_576 ? C28 C27 C32 C31 -158(3) . . . 2_576 ? C30 C27 C32 C31 19(3) 2_576 . . 2_576 ? C31 C27 C32 C33 -24(3) 2_576 . . . ? C32 C27 C32 C33 -178.9(9) 2_576 . . . ? C28 C27 C32 C33 177.6(7) . . . . ? C30 C27 C32 C33 -5.1(6) 2_576 . . . ? C31 C27 C32 C30 -19(3) 2_576 . . 2_576 ? C32 C27 C32 C30 -173.8(9) 2_576 . . 2_576 ? C28 C27 C32 C30 -177.3(6) . . . 2_576 ? C27 C32 C33 C29 -151(4) 2_576 . . 2_576 ? C28 C32 C33 C29 -148(4) 2_576 . . 2_576 ? C32 C32 C33 C29 21(6) 2_576 . . 2_576 ? C31 C32 C33 C29 -155(3) . . . 2_576 ? C27 C32 C33 C29 28(4) . . . 2_576 ? C31 C32 C33 C29 25(3) 2_576 . . 2_576 ? C30 C32 C33 C29 23(3) 2_576 . . 2_576 ? C27 C32 C33 C28 -3.0(6) 2_576 . . 2_576 ? C32 C32 C33 C28 169(6) 2_576 . . 2_576 ? C31 C32 C33 C28 -6.5(9) . . . 2_576 ? C27 C32 C33 C28 175.9(11) . . . 2_576 ? C29 C32 C33 C28 148(4) 2_576 . . 2_576 ? C31 C32 C33 C28 173.0(12) 2_576 . . 2_576 ? C30 C32 C33 C28 171.0(12) 2_576 . . 2_576 ? C27 C32 C33 C30 -174.0(11) 2_576 . . 2_576 ? C28 C32 C33 C30 -171.0(12) 2_576 . . 2_576 ? C32 C32 C33 C30 -2(6) 2_576 . . 2_576 ? C31 C32 C33 C30 -177.5(6) . . . 2_576 ? C27 C32 C33 C30 4.9(6) . . . 2_576 ? C29 C32 C33 C30 -23(3) 2_576 . . 2_576 ? C31 C32 C33 C30 2.0(4) 2_576 . . 2_576 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 26.38 _diffrn_measured_fraction_theta_full 0.983 _refine_diff_density_max 0.783 _refine_diff_density_min -0.470 _refine_diff_density_rms 0.079 #====END data_10 _database_code_depnum_ccdc_archive 'CCDC 725693' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C76 H90 N6 O P4 Pb2 Si4' _chemical_formula_weight 1754.16 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' P P 0.1023 0.0942 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pbca loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 20.789(2) _cell_length_b 17.829(2) _cell_length_c 22.813(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 8455.3(17) _cell_formula_units_Z 4 _cell_measurement_temperature 298(2) _cell_measurement_reflns_used 4597 _cell_measurement_theta_min 2.643 _cell_measurement_theta_max 24.843 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.23 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.378 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3504 _exptl_absorpt_coefficient_mu 4.152 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.4485 _exptl_absorpt_correction_T_max 0.5563 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 298(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 40850 _diffrn_reflns_av_R_equivalents 0.1288 _diffrn_reflns_av_sigmaI/netI 0.1232 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 23 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.75 _diffrn_reflns_theta_max 25.01 _reflns_number_total 7463 _reflns_number_gt 3417 _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^)+(0.0625P)^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 7463 _refine_ls_number_parameters 442 _refine_ls_number_restraints 88 _refine_ls_R_factor_all 0.1473 _refine_ls_R_factor_gt 0.0496 _refine_ls_wR_factor_ref 0.1536 _refine_ls_wR_factor_gt 0.1214 _refine_ls_goodness_of_fit_ref 0.999 _refine_ls_restrained_S_all 1.000 _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 0.54556(2) 0.42010(2) 0.47930(2) 0.04783(17) Uani 1 1 d . . . N1 N 0.4232(4) 0.5893(5) 0.3666(4) 0.044(2) Uani 1 1 d . . . N2 N 0.4379(4) 0.3712(5) 0.4843(4) 0.049(3) Uani 1 1 d . . . N3 N 0.3704(5) 0.7468(6) 0.2517(4) 0.076(3) Uani 1 1 d . . . P1 P 0.40743(14) 0.43253(17) 0.44014(14) 0.0461(8) Uani 1 1 d . . . P2 P 0.36042(18) 0.69705(19) 0.30543(15) 0.0581(9) Uani 1 1 d . . . Si1 Si 0.42208(18) 0.2798(2) 0.50359(17) 0.0601(11) Uani 1 1 d . . . Si2 Si 0.3536(2) 0.7607(3) 0.18123(18) 0.0807(13) Uani 1 1 d . . . O1 O 1.0049(12) 0.5132(16) 0.4179(11) 0.160(8) Uani 0.50 1 d PDU . . C1 C 0.4678(5) 0.5001(6) 0.4351(5) 0.043(3) Uani 1 1 d . . . C2 C 0.4741(5) 0.5491(6) 0.3842(5) 0.043(3) Uani 1 1 d . . . C3 C 0.5341(6) 0.5603(7) 0.3584(6) 0.061(4) Uani 1 1 d . . . H3 H 0.5696 0.5332 0.3713 0.074 Uiso 1 1 calc R . . C4 C 0.5404(7) 0.6107(8) 0.3145(6) 0.073(4) Uani 1 1 d . . . H4 H 0.5803 0.6173 0.2968 0.088 Uiso 1 1 calc R . . C5 C 0.4883(7) 0.6528(8) 0.2956(6) 0.072(4) Uani 1 1 d . . . H5 H 0.4924 0.6879 0.2657 0.086 Uiso 1 1 calc R . . C6 C 0.4302(6) 0.6405(7) 0.3228(6) 0.055(3) Uani 1 1 d . . . C7 C 0.3890(6) 0.3946(6) 0.3702(5) 0.052(3) Uani 1 1 d . . . C8 C 0.3280(6) 0.3728(7) 0.3522(6) 0.060(4) Uani 1 1 d . . . H8 H 0.2930 0.3822 0.3766 0.072 Uiso 1 1 calc R . . C9 C 0.3175(8) 0.3367(7) 0.2979(7) 0.073(4) Uani 1 1 d . . . H9 H 0.2763 0.3230 0.2861 0.088 Uiso 1 1 calc R . . C10 C 0.3701(10) 0.3223(8) 0.2630(7) 0.089(5) Uani 1 1 d . . . H10 H 0.3646 0.2978 0.2273 0.107 Uiso 1 1 calc R . . C11 C 0.4303(8) 0.3436(9) 0.2802(7) 0.095(5) Uani 1 1 d . . . H11 H 0.4656 0.3335 0.2564 0.114 Uiso 1 1 calc R . . C12 C 0.4386(6) 0.3804(8) 0.3331(6) 0.069(4) Uani 1 1 d . . . H12 H 0.4797 0.3959 0.3436 0.082 Uiso 1 1 calc R . . C13 C 0.3338(6) 0.4701(7) 0.4698(6) 0.049(3) Uani 1 1 d . . . C14 C 0.3202(6) 0.4587(7) 0.5300(6) 0.061(4) Uani 1 1 d . . . H14 H 0.3469 0.4276 0.5518 0.073 Uiso 1 1 calc R . . C15 C 0.2693(8) 0.4919(8) 0.5566(7) 0.080(4) Uani 1 1 d . . . H15 H 0.2621 0.4848 0.5965 0.096 Uiso 1 1 calc R . . C16 C 0.2282(7) 0.5363(8) 0.5240(8) 0.080(5) Uani 1 1 d . . . H16 H 0.1921 0.5575 0.5413 0.096 Uiso 1 1 calc R . . C17 C 0.2411(7) 0.5490(7) 0.4657(7) 0.071(4) Uani 1 1 d . . . H17 H 0.2150 0.5810 0.4440 0.086 Uiso 1 1 calc R . . C18 C 0.2927(6) 0.5141(7) 0.4394(6) 0.059(4) Uani 1 1 d . . . H18 H 0.2995 0.5212 0.3995 0.071 Uiso 1 1 calc R . . C19 C 0.4927(8) 0.2449(9) 0.5373(8) 0.129(7) Uani 1 1 d . . . H19A H 0.5254 0.2377 0.5081 0.194 Uiso 1 1 calc R . . H19B H 0.4834 0.1979 0.5559 0.194 Uiso 1 1 calc R . . H19C H 0.5075 0.2802 0.5660 0.194 Uiso 1 1 calc R . . C20 C 0.3996(8) 0.2210(7) 0.4414(7) 0.116(6) Uani 1 1 d . . . H20A H 0.3624 0.2418 0.4225 0.174 Uiso 1 1 calc R . . H20B H 0.3899 0.1713 0.4550 0.174 Uiso 1 1 calc R . . H20C H 0.4346 0.2189 0.4140 0.174 Uiso 1 1 calc R . . C21 C 0.3554(8) 0.2703(9) 0.5560(7) 0.125(6) Uani 1 1 d U . . H21A H 0.3612 0.3053 0.5875 0.188 Uiso 1 1 calc R . . H21B H 0.3547 0.2202 0.5713 0.188 Uiso 1 1 calc R . . H21C H 0.3155 0.2806 0.5364 0.188 Uiso 1 1 calc R . . C22 C 0.2942(7) 0.6295(8) 0.3003(6) 0.059(4) Uani 1 1 d . . . C23 C 0.3045(7) 0.5643(8) 0.2700(6) 0.078(4) Uani 1 1 d . . . H23 H 0.3450 0.5520 0.2557 0.093 Uiso 1 1 calc R . . C24 C 0.2516(10) 0.5171(9) 0.2614(8) 0.104(6) Uani 1 1 d . . . H24 H 0.2582 0.4712 0.2431 0.124 Uiso 1 1 calc R . . C25 C 0.1926(9) 0.5347(10) 0.2781(9) 0.103(6) Uani 1 1 d . . . H25 H 0.1580 0.5036 0.2694 0.123 Uiso 1 1 calc R . . C26 C 0.1842(8) 0.5986(10) 0.3079(7) 0.088(5) Uani 1 1 d . . . H26 H 0.1434 0.6108 0.3217 0.106 Uiso 1 1 calc R . . C27 C 0.2340(7) 0.6459(8) 0.3185(6) 0.072(4) Uani 1 1 d . . . H27 H 0.2266 0.6905 0.3386 0.087 Uiso 1 1 calc R . . C28 C 0.3461(5) 0.7503(7) 0.3706(5) 0.048(3) Uani 1 1 d . . . C29 C 0.3316(6) 0.7198(7) 0.4246(6) 0.063(4) Uani 1 1 d . . . H29 H 0.3293 0.6679 0.4280 0.076 Uiso 1 1 calc R . . C30 C 0.3204(7) 0.7628(10) 0.4734(7) 0.080(4) Uani 1 1 d . . . H30 H 0.3086 0.7401 0.5085 0.096 Uiso 1 1 calc R . . C31 C 0.3265(8) 0.8382(11) 0.4703(9) 0.102(6) Uani 1 1 d . . . H31 H 0.3205 0.8677 0.5035 0.123 Uiso 1 1 calc R . . C32 C 0.3413(8) 0.8702(9) 0.4181(10) 0.096(6) Uani 1 1 d . . . H32 H 0.3450 0.9221 0.4162 0.115 Uiso 1 1 calc R . . C33 C 0.3513(6) 0.8287(8) 0.3676(7) 0.068(4) Uani 1 1 d . . . H33 H 0.3612 0.8524 0.3324 0.082 Uiso 1 1 calc R . . C34 C 0.4191(8) 0.7313(10) 0.1343(7) 0.121(6) Uani 1 1 d . . . H34A H 0.4131 0.7518 0.0957 0.182 Uiso 1 1 calc R . . H34B H 0.4199 0.6775 0.1320 0.182 Uiso 1 1 calc R . . H34C H 0.4591 0.7490 0.1501 0.182 Uiso 1 1 calc R . . C35 C 0.3423(10) 0.8635(11) 0.1683(9) 0.158(8) Uani 1 1 d U . . H35A H 0.3548 0.8907 0.2028 0.237 Uiso 1 1 calc R . . H35B H 0.2979 0.8734 0.1598 0.237 Uiso 1 1 calc R . . H35C H 0.3684 0.8790 0.1358 0.237 Uiso 1 1 calc R . . C36 C 0.2823(9) 0.7144(12) 0.1568(8) 0.157(8) Uani 1 1 d U . . H36A H 0.2849 0.6620 0.1661 0.235 Uiso 1 1 calc R . . H36B H 0.2781 0.7204 0.1151 0.235 Uiso 1 1 calc R . . H36C H 0.2456 0.7359 0.1760 0.235 Uiso 1 1 calc R . . C37 C 1.0254(13) 0.515(2) 0.3593(14) 0.140(8) Uani 0.50 1 d PDU . . H37A H 1.0647 0.4865 0.3548 0.168 Uiso 0.50 1 calc PR . . H37B H 1.0340 0.5666 0.3477 0.168 Uiso 0.50 1 calc PR . . C38 C 0.9739(16) 0.483(2) 0.3221(10) 0.150(8) Uani 0.50 1 d PDU . . H38A H 0.9883 0.4368 0.3039 0.180 Uiso 0.50 1 calc PR . . H38B H 0.9617 0.5181 0.2915 0.180 Uiso 0.50 1 calc PR . . C39 C 0.9177(12) 0.468(2) 0.3629(14) 0.146(8) Uani 0.50 1 d PDU . . H39A H 0.8814 0.4999 0.3528 0.175 Uiso 0.50 1 calc PR . . H39B H 0.9043 0.4162 0.3603 0.175 Uiso 0.50 1 calc PR . . C40 C 0.9409(14) 0.486(2) 0.4231(11) 0.144(8) Uani 0.50 1 d PDU . . H40A H 0.9136 0.5233 0.4412 0.172 Uiso 0.50 1 calc PR . . H40B H 0.9402 0.4409 0.4473 0.172 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.0457(2) 0.0394(3) 0.0584(3) -0.0025(3) 0.0026(3) 0.0022(3) N1 0.044(5) 0.043(6) 0.045(6) -0.008(5) 0.001(5) -0.002(5) N2 0.048(6) 0.036(5) 0.064(7) 0.007(5) 0.000(5) -0.004(4) N3 0.093(8) 0.071(8) 0.065(8) 0.018(7) -0.023(6) -0.008(7) P1 0.0433(17) 0.042(2) 0.053(2) -0.0014(16) 0.0012(15) -0.0024(15) P2 0.071(2) 0.049(2) 0.055(2) 0.0077(18) -0.0097(19) 0.0004(19) Si1 0.059(2) 0.047(2) 0.074(3) 0.0070(19) 0.0078(19) -0.0144(19) Si2 0.085(3) 0.095(4) 0.061(3) 0.022(3) 0.000(2) 0.022(3) O1 0.147(16) 0.167(17) 0.165(19) 0.017(16) 0.023(15) -0.017(14) C1 0.031(7) 0.053(8) 0.045(7) 0.003(6) 0.001(5) 0.001(5) C2 0.040(7) 0.042(7) 0.049(8) -0.009(6) 0.007(6) -0.002(6) C3 0.070(10) 0.063(10) 0.051(8) 0.013(7) 0.006(7) -0.003(7) C4 0.046(8) 0.094(11) 0.080(10) -0.002(9) 0.017(8) 0.000(9) C5 0.074(10) 0.082(11) 0.060(10) 0.009(8) 0.015(8) -0.008(9) C6 0.069(9) 0.052(9) 0.045(8) -0.002(7) 0.003(7) 0.006(7) C7 0.046(8) 0.041(8) 0.067(9) -0.005(6) 0.009(7) -0.003(6) C8 0.064(9) 0.044(8) 0.071(10) -0.003(7) 0.007(8) 0.002(7) C9 0.090(12) 0.056(10) 0.073(11) -0.009(8) -0.026(9) -0.018(8) C10 0.138(16) 0.067(11) 0.063(11) -0.021(8) 0.004(11) -0.009(11) C11 0.080(12) 0.110(14) 0.094(13) -0.028(11) 0.025(10) -0.015(10) C12 0.064(10) 0.079(10) 0.063(10) -0.021(8) -0.005(8) -0.009(8) C13 0.047(7) 0.045(8) 0.055(9) -0.006(7) -0.004(7) -0.014(6) C14 0.049(8) 0.050(8) 0.084(12) -0.014(8) 0.005(8) 0.005(6) C15 0.089(12) 0.074(11) 0.078(11) -0.015(9) 0.022(10) -0.003(10) C16 0.064(10) 0.054(10) 0.123(15) -0.026(11) 0.030(11) -0.003(8) C17 0.057(9) 0.054(9) 0.104(13) 0.007(8) 0.021(9) 0.006(7) C18 0.050(8) 0.054(9) 0.072(10) 0.003(8) 0.007(7) 0.002(7) C19 0.130(15) 0.070(12) 0.19(2) 0.016(12) -0.014(14) -0.026(11) C20 0.173(18) 0.046(10) 0.130(15) 0.020(10) -0.029(13) -0.020(10) C21 0.125(9) 0.113(9) 0.137(10) 0.011(8) 0.035(8) -0.004(8) C22 0.070(10) 0.053(10) 0.054(9) 0.010(7) -0.020(7) 0.014(8) C23 0.087(11) 0.063(11) 0.083(11) -0.009(9) -0.019(9) 0.008(9) C24 0.126(16) 0.059(12) 0.126(16) -0.025(10) -0.049(14) 0.009(12) C25 0.086(14) 0.080(15) 0.142(18) -0.006(12) -0.039(12) -0.016(11) C26 0.074(11) 0.087(14) 0.104(14) -0.004(10) -0.024(10) -0.002(10) C27 0.079(11) 0.056(10) 0.081(11) -0.003(8) -0.019(9) 0.010(9) C28 0.051(7) 0.047(8) 0.045(8) 0.001(6) -0.011(6) -0.001(6) C29 0.070(9) 0.051(9) 0.069(10) -0.010(8) -0.011(8) 0.011(7) C30 0.081(10) 0.092(13) 0.067(10) -0.019(11) 0.002(9) 0.011(9) C31 0.097(13) 0.094(16) 0.115(17) -0.050(14) -0.025(13) 0.013(11) C32 0.080(12) 0.053(11) 0.153(19) -0.035(13) -0.032(13) 0.012(9) C33 0.070(10) 0.045(9) 0.090(12) 0.002(8) -0.013(8) 0.005(7) C34 0.117(13) 0.131(17) 0.116(15) -0.008(13) 0.020(12) 0.032(13) C35 0.175(11) 0.155(11) 0.145(11) 0.024(9) 0.013(9) 0.034(9) C36 0.147(11) 0.185(12) 0.138(11) 0.016(9) -0.017(8) -0.013(9) C37 0.122(17) 0.151(18) 0.15(2) 0.027(17) 0.040(15) -0.024(14) C38 0.138(18) 0.161(18) 0.151(19) 0.015(17) 0.027(15) -0.027(15) C39 0.126(17) 0.161(18) 0.15(2) 0.017(17) 0.028(15) -0.031(14) C40 0.121(17) 0.160(18) 0.15(2) 0.020(17) 0.035(16) -0.023(14) _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 C1 2.380(10) . ? Pb1 N2 2.404(8) . ? Pb1 C1 2.431(11) 5_666 ? Pb1 Pb1 3.5491(9) 5_666 ? N1 C2 1.340(13) . ? N1 C6 1.362(14) . ? N2 P1 1.616(9) . ? N2 Si1 1.721(9) . ? N3 P2 1.526(10) . ? N3 Si2 1.665(10) . ? P1 C1 1.743(11) . ? P1 C7 1.775(13) . ? P1 C13 1.801(12) . ? P2 C28 1.789(12) . ? P2 C6 1.811(13) . ? P2 C22 1.832(14) . ? Si1 C19 1.770(16) . ? Si1 C20 1.825(15) . ? Si1 C21 1.838(15) . ? Si2 C36 1.785(18) . ? Si2 C34 1.811(15) . ? Si2 C35 1.871(19) . ? O1 C37 1.402(16) . ? O1 C40 1.422(16) . ? C1 C2 1.459(15) . ? C1 Pb1 2.431(11) 5_666 ? C2 C3 1.393(15) . ? C3 C4 1.352(17) . ? C3 H3 0.9300 . ? C4 C5 1.387(17) . ? C4 H4 0.9300 . ? C5 C6 1.374(16) . ? C5 H5 0.9300 . ? C7 C12 1.357(15) . ? C7 C8 1.390(15) . ? C8 C9 1.413(17) . ? C8 H8 0.9300 . ? C9 C10 1.378(19) . ? C9 H9 0.9300 . ? C10 C11 1.365(19) . ? C10 H10 0.9300 . ? C11 C12 1.384(18) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C18 1.352(16) . ? C13 C14 1.417(16) . ? C14 C15 1.356(17) . ? C14 H14 0.9300 . ? C15 C16 1.383(19) . ? C15 H15 0.9300 . ? C16 C17 1.375(19) . ? C16 H16 0.9300 . ? C17 C18 1.378(16) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C27 1.351(17) . ? C22 C23 1.367(17) . ? C23 C24 1.40(2) . ? C23 H23 0.9300 . ? C24 C25 1.32(2) . ? C24 H24 0.9300 . ? C25 C26 1.34(2) . ? C25 H25 0.9300 . ? C26 C27 1.358(18) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.379(15) . ? C28 C33 1.404(16) . ? C29 C30 1.373(17) . ? C29 H29 0.9300 . ? C30 C31 1.35(2) . ? C30 H30 0.9300 . ? C31 C32 1.36(2) . ? C31 H31 0.9300 . ? C32 C33 1.38(2) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 C38 1.483(17) . ? C37 H37A 0.9700 . ? C37 H37B 0.9700 . ? C38 C39 1.518(17) . ? C38 H38A 0.9700 . ? C38 H38B 0.9700 . ? C39 C40 1.489(17) . ? C39 H39A 0.9700 . ? C39 H39B 0.9700 . ? C40 H40A 0.9700 . ? C40 H40B 0.9700 . ? 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 C1 Pb1 N2 66.7(3) . . ? C1 Pb1 C1 84.9(4) . 5_666 ? N2 Pb1 C1 93.9(3) . 5_666 ? C1 Pb1 Pb1 43.0(3) . 5_666 ? N2 Pb1 Pb1 77.4(2) . 5_666 ? C1 Pb1 Pb1 41.9(2) 5_666 5_666 ? C2 N1 C6 119.6(10) . . ? P1 N2 Si1 136.5(6) . . ? P1 N2 Pb1 95.2(4) . . ? Si1 N2 Pb1 122.3(4) . . ? P2 N3 Si2 146.5(7) . . ? N2 P1 C1 103.1(5) . . ? N2 P1 C7 112.8(5) . . ? C1 P1 C7 111.1(6) . . ? N2 P1 C13 110.5(5) . . ? C1 P1 C13 112.3(5) . . ? C7 P1 C13 107.2(6) . . ? N3 P2 C28 112.4(6) . . ? N3 P2 C6 113.0(6) . . ? C28 P2 C6 104.3(6) . . ? N3 P2 C22 115.6(6) . . ? C28 P2 C22 106.1(6) . . ? C6 P2 C22 104.5(6) . . ? N2 Si1 C19 106.6(6) . . ? N2 Si1 C20 113.3(6) . . ? C19 Si1 C20 110.4(8) . . ? N2 Si1 C21 113.4(6) . . ? C19 Si1 C21 108.1(8) . . ? C20 Si1 C21 105.0(8) . . ? N3 Si2 C36 114.0(7) . . ? N3 Si2 C34 111.7(7) . . ? C36 Si2 C34 107.8(9) . . ? N3 Si2 C35 108.9(8) . . ? C36 Si2 C35 107.5(9) . . ? C34 Si2 C35 106.5(9) . . ? C37 O1 C40 111.9(11) . . ? C2 C1 P1 122.1(8) . . ? C2 C1 Pb1 129.3(7) . . ? P1 C1 Pb1 92.7(5) . . ? C2 C1 Pb1 107.4(7) . 5_666 ? P1 C1 Pb1 105.7(5) . 5_666 ? Pb1 C1 Pb1 95.1(4) . 5_666 ? N1 C2 C3 120.3(11) . . ? N1 C2 C1 119.1(10) . . ? C3 C2 C1 120.2(11) . . ? C4 C3 C2 119.6(13) . . ? C4 C3 H3 120.2 . . ? C2 C3 H3 120.2 . . ? C3 C4 C5 121.0(13) . . ? C3 C4 H4 119.5 . . ? C5 C4 H4 119.5 . . ? C6 C5 C4 117.4(13) . . ? C6 C5 H5 121.3 . . ? C4 C5 H5 121.3 . . ? N1 C6 C5 122.1(12) . . ? N1 C6 P2 116.6(10) . . ? C5 C6 P2 121.1(11) . . ? C12 C7 C8 117.3(12) . . ? C12 C7 P1 117.9(10) . . ? C8 C7 P1 124.6(10) . . ? C7 C8 C9 121.8(13) . . ? C7 C8 H8 119.1 . . ? C9 C8 H8 119.1 . . ? C10 C9 C8 118.0(14) . . ? C10 C9 H9 121.0 . . ? C8 C9 H9 121.0 . . ? C11 C10 C9 120.7(14) . . ? C11 C10 H10 119.7 . . ? C9 C10 H10 119.7 . . ? C10 C11 C12 119.7(14) . . ? C10 C11 H11 120.1 . . ? C12 C11 H11 120.1 . . ? C7 C12 C11 122.5(13) . . ? C7 C12 H12 118.7 . . ? C11 C12 H12 118.7 . . ? C18 C13 C14 117.0(11) . . ? C18 C13 P1 124.1(10) . . ? C14 C13 P1 118.7(9) . . ? C15 C14 C13 121.9(13) . . ? C15 C14 H14 119.1 . . ? C13 C14 H14 119.1 . . ? C14 C15 C16 119.3(15) . . ? C14 C15 H15 120.3 . . ? C16 C15 H15 120.3 . . ? C17 C16 C15 119.7(14) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 119.9(14) . . ? C16 C17 H17 120.1 . . ? C18 C17 H17 120.1 . . ? C13 C18 C17 122.1(13) . . ? C13 C18 H18 118.9 . . ? C17 C18 H18 118.9 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si1 C21 H21A 109.5 . . ? Si1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C27 C22 C23 118.9(14) . . ? C27 C22 P2 122.2(12) . . ? C23 C22 P2 118.3(12) . . ? C22 C23 C24 117.4(15) . . ? C22 C23 H23 121.3 . . ? C24 C23 H23 121.3 . . ? C25 C24 C23 123.1(16) . . ? C25 C24 H24 118.5 . . ? C23 C24 H24 118.5 . . ? C24 C25 C26 118.0(17) . . ? C24 C25 H25 121.0 . . ? C26 C25 H25 121.0 . . ? C25 C26 C27 121.3(17) . . ? C25 C26 H26 119.3 . . ? C27 C26 H26 119.3 . . ? C22 C27 C26 121.2(15) . . ? C22 C27 H27 119.4 . . ? C26 C27 H27 119.4 . . ? C29 C28 C33 116.9(12) . . ? C29 C28 P2 124.7(10) . . ? C33 C28 P2 118.4(10) . . ? C30 C29 C28 122.8(14) . . ? C30 C29 H29 118.6 . . ? C28 C29 H29 118.6 . . ? C31 C30 C29 119.8(17) . . ? C31 C30 H30 120.1 . . ? C29 C30 H30 120.1 . . ? C30 C31 C32 119.1(18) . . ? C30 C31 H31 120.5 . . ? C32 C31 H31 120.5 . . ? C31 C32 C33 122.7(17) . . ? C31 C32 H32 118.7 . . ? C33 C32 H32 118.7 . . ? C32 C33 C28 118.7(14) . . ? C32 C33 H33 120.6 . . ? C28 C33 H33 120.6 . . ? Si2 C34 H34A 109.5 . . ? Si2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si2 C35 H35A 109.5 . . ? Si2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si2 C36 H36A 109.5 . . ? Si2 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si2 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? O1 C37 C38 108.4(11) . . ? O1 C37 H37A 110.0 . . ? C38 C37 H37A 110.0 . . ? O1 C37 H37B 110.0 . . ? C38 C37 H37B 110.0 . . ? H37A C37 H37B 108.4 . . ? C37 C38 C39 105.8(10) . . ? C37 C38 H38A 110.6 . . ? C39 C38 H38A 110.6 . . ? C37 C38 H38B 110.6 . . ? C39 C38 H38B 110.6 . . ? H38A C38 H38B 108.7 . . ? C40 C39 C38 106.2(10) . . ? C40 C39 H39A 110.5 . . ? C38 C39 H39A 110.5 . . ? C40 C39 H39B 110.5 . . ? C38 C39 H39B 110.5 . . ? H39A C39 H39B 108.7 . . ? O1 C40 C39 107.4(10) . . ? O1 C40 H40A 110.2 . . ? C39 C40 H40A 110.2 . . ? O1 C40 H40B 110.2 . . ? C39 C40 H40B 110.2 . . ? H40A C40 H40B 108.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.476 _refine_diff_density_min -0.827 _refine_diff_density_rms 0.144 #====END data_11 _database_code_depnum_ccdc_archive 'CCDC 725694' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C49 H65 N4 P2 Si3 Sn' _chemical_formula_weight 974.95 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 '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 Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4319(16) _cell_length_b 15.457(3) _cell_length_c 17.668(3) _cell_angle_alpha 80.404(3) _cell_angle_beta 72.936(3) _cell_angle_gamma 71.534(2) _cell_volume 2574.7(7) _cell_formula_units_Z 2 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3708 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 26.25 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas NONE _exptl_crystal_density_diffrn 1.258 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1018 _exptl_absorpt_coefficient_mu 0.664 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.900 _exptl_absorpt_correction_T_max 0.936 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 0 _diffrn_standards_interval_count 0 _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 10880 _diffrn_reflns_av_R_equivalents 0.0250 _diffrn_reflns_av_sigmaI/netI 0.0592 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.39 _diffrn_reflns_theta_max 25.02 _reflns_number_total 8408 _reflns_number_gt 5929 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _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^)+(0.0522P)^2^+1.8784P] 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 8408 _refine_ls_number_parameters 543 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.0766 _refine_ls_R_factor_gt 0.0456 _refine_ls_wR_factor_ref 0.1250 _refine_ls_wR_factor_gt 0.1057 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.052 _refine_ls_shift/su_max 0.005 _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 -0.00435(4) 0.97465(2) 0.70997(2) 0.04985(13) Uani 1 1 d . . . P1 P 0.34454(13) 0.69669(8) 0.60778(7) 0.0426(3) Uani 1 1 d . . . P2 P 0.15320(13) 1.12628(8) 0.70479(7) 0.0434(3) Uani 1 1 d . . . Si1 Si 0.55106(16) 0.57399(10) 0.69428(10) 0.0593(4) Uani 1 1 d . . . Si2 Si 0.05854(17) 0.85557(10) 0.88410(8) 0.0595(4) Uani 1 1 d . . . Si3 Si -0.19535(18) 0.86313(13) 0.83285(12) 0.0825(6) Uani 1 1 d . . . N1 N 0.4868(4) 0.6363(3) 0.6203(2) 0.0552(11) Uani 1 1 d . . . N2 N 0.2247(4) 0.9499(2) 0.6789(2) 0.0426(9) Uani 1 1 d . . . N3 N 0.0159(4) 1.0968(2) 0.7529(2) 0.0489(10) Uani 1 1 d . . . N4 N -0.0424(4) 0.8916(3) 0.8168(2) 0.0515(10) Uani 1 1 d . . . C1 C 0.2178(5) 0.6325(3) 0.6306(3) 0.0451(11) Uani 1 1 d . . . C2 C 0.1105(6) 0.6404(4) 0.6960(4) 0.0764(17) Uani 1 1 d . . . H2 H 0.0929 0.6860 0.7291 0.092 Uiso 1 1 calc R . . C3 C 0.0252(7) 0.5830(5) 0.7157(4) 0.088(2) Uani 1 1 d . . . H3 H -0.0493 0.5910 0.7609 0.105 Uiso 1 1 calc R . . C4 C 0.0498(7) 0.5171(4) 0.6704(5) 0.0786(19) Uani 1 1 d . . . H4 H -0.0049 0.4768 0.6850 0.094 Uiso 1 1 calc R . . C5 C 0.1529(8) 0.5078(4) 0.6035(5) 0.096(2) Uani 1 1 d . . . H5 H 0.1675 0.4629 0.5703 0.115 Uiso 1 1 calc R . . C6 C 0.2375(7) 0.5651(4) 0.5841(4) 0.0808(19) Uani 1 1 d . . . H6 H 0.3101 0.5575 0.5380 0.097 Uiso 1 1 calc R . . C7 C 0.3703(5) 0.7299(4) 0.5025(3) 0.0524(13) Uani 1 1 d . . . C8 C 0.4690(6) 0.6708(5) 0.4493(4) 0.0767(18) Uani 1 1 d . . . H8 H 0.5238 0.6156 0.4675 0.092 Uiso 1 1 calc R . . C9 C 0.4860(10) 0.6946(8) 0.3680(5) 0.120(4) Uani 1 1 d . . . H9 H 0.5504 0.6542 0.3317 0.144 Uiso 1 1 calc R . . C10 C 0.4086(12) 0.7767(10) 0.3415(5) 0.134(5) Uani 1 1 d . . . H10 H 0.4215 0.7928 0.2873 0.161 Uiso 1 1 calc R . . C11 C 0.3140(9) 0.8343(7) 0.3934(5) 0.111(3) Uani 1 1 d . . . H11 H 0.2615 0.8901 0.3748 0.134 Uiso 1 1 calc R . . C12 C 0.2934(6) 0.8118(4) 0.4739(3) 0.0713(17) Uani 1 1 d . . . H12 H 0.2270 0.8525 0.5092 0.086 Uiso 1 1 calc R . . C13 C 0.5977(8) 0.6459(5) 0.7493(4) 0.109(3) Uani 1 1 d . . . H13A H 0.6725 0.6685 0.7151 0.164 Uiso 1 1 calc R . . H13B H 0.6270 0.6102 0.7944 0.164 Uiso 1 1 calc R . . H13C H 0.5177 0.6966 0.7671 0.164 Uiso 1 1 calc R . . C14 C 0.4284(7) 0.5158(4) 0.7680(4) 0.088(2) Uani 1 1 d . . . H14A H 0.3458 0.5610 0.7927 0.133 Uiso 1 1 calc R . . H14B H 0.4733 0.4796 0.8077 0.133 Uiso 1 1 calc R . . H14C H 0.4032 0.4769 0.7412 0.133 Uiso 1 1 calc R . . C15 C 0.7113(6) 0.4844(4) 0.6500(4) 0.090(2) Uani 1 1 d . . . H15A H 0.6872 0.4452 0.6230 0.135 Uiso 1 1 calc R . . H15B H 0.7528 0.4489 0.6912 0.135 Uiso 1 1 calc R . . H15C H 0.7767 0.5129 0.6128 0.135 Uiso 1 1 calc R . . C16 C 0.2574(5) 0.7962(3) 0.6556(3) 0.0480(12) Uani 1 1 d . . . H16 H 0.1676 0.8011 0.6880 0.058 Uiso 1 1 calc R . . C17 C 0.3111(5) 0.8684(3) 0.6491(3) 0.0410(11) Uani 1 1 d . . . C18 C 0.4526(5) 0.8641(3) 0.6112(3) 0.0534(13) Uani 1 1 d . . . H18 H 0.5124 0.8105 0.5892 0.064 Uiso 1 1 calc R . . C19 C 0.5025(5) 0.9353(4) 0.6063(3) 0.0611(14) Uani 1 1 d . . . H19 H 0.5960 0.9306 0.5815 0.073 Uiso 1 1 calc R . . C20 C 0.4131(5) 1.0169(3) 0.6386(3) 0.0566(13) Uani 1 1 d . . . H20 H 0.4463 1.0667 0.6364 0.068 Uiso 1 1 calc R . . C21 C 0.2779(5) 1.0211(3) 0.6728(3) 0.0442(11) Uani 1 1 d . . . C22 C 0.1354(5) 1.1992(3) 0.6157(3) 0.0468(12) Uani 1 1 d . . . C23 C 0.2364(5) 1.2407(3) 0.5730(3) 0.0502(12) Uani 1 1 d . . . H23 H 0.3125 1.2351 0.5926 0.060 Uiso 1 1 calc R . . C24 C 0.2261(6) 1.2900(3) 0.5022(3) 0.0579(14) Uani 1 1 d . . . H24 H 0.2951 1.3176 0.4736 0.069 Uiso 1 1 calc R . . C25 C 0.1157(7) 1.2984(4) 0.4740(4) 0.0825(19) Uani 1 1 d . . . H25 H 0.1083 1.3326 0.4262 0.099 Uiso 1 1 calc R . . C26 C 0.0151(8) 1.2575(5) 0.5145(4) 0.109(3) Uani 1 1 d . . . H26 H -0.0605 1.2634 0.4944 0.130 Uiso 1 1 calc R . . C27 C 0.0255(6) 1.2072(4) 0.5857(4) 0.0789(19) Uani 1 1 d . . . H27 H -0.0428 1.1785 0.6134 0.095 Uiso 1 1 calc R . . C28 C 0.2198(5) 1.1804(3) 0.7605(3) 0.0474(12) Uani 1 1 d . . . C29 C 0.1771(6) 1.2740(4) 0.7614(3) 0.0635(15) Uani 1 1 d . . . H29 H 0.1189 1.3093 0.7298 0.076 Uiso 1 1 calc R . . C30 C 0.2190(8) 1.3158(5) 0.8080(4) 0.085(2) Uani 1 1 d . . . H30 H 0.1879 1.3791 0.8090 0.102 Uiso 1 1 calc R . . C31 C 0.3064(8) 1.2648(6) 0.8532(4) 0.090(2) Uani 1 1 d . . . H31 H 0.3352 1.2933 0.8850 0.108 Uiso 1 1 calc R . . C32 C 0.3509(7) 1.1733(5) 0.8521(3) 0.0779(18) Uani 1 1 d . . . H32 H 0.4119 1.1390 0.8824 0.093 Uiso 1 1 calc R . . C33 C 0.3078(5) 1.1297(4) 0.8067(3) 0.0598(14) Uani 1 1 d . . . H33 H 0.3379 1.0662 0.8072 0.072 Uiso 1 1 calc R . . C34 C -0.1008(5) 1.1546(3) 0.8030(3) 0.0489(12) Uani 1 1 d . . . C35 C -0.1523(7) 1.2454(4) 0.7868(4) 0.097(2) Uani 1 1 d . . . H35 H -0.1109 1.2734 0.7393 0.117 Uiso 1 1 calc R . . C36 C -0.2651(7) 1.2977(5) 0.8392(4) 0.108(3) Uani 1 1 d . . . H36 H -0.2940 1.3606 0.8272 0.129 Uiso 1 1 calc R . . C37 C -0.3346(6) 1.2612(5) 0.9069(4) 0.0715(16) Uani 1 1 d . . . C38 C -0.2878(7) 1.1708(5) 0.9220(4) 0.086(2) Uani 1 1 d . . . H38 H -0.3339 1.1429 0.9681 0.104 Uiso 1 1 calc R . . C39 C -0.1732(6) 1.1176(4) 0.8713(3) 0.0743(17) Uani 1 1 d . . . H39 H -0.1444 1.0549 0.8841 0.089 Uiso 1 1 calc R . . C40 C -0.4559(7) 1.3190(5) 0.9654(4) 0.097(2) Uani 1 1 d . . . H40A H -0.5180 1.2834 0.9942 0.146 Uiso 1 1 calc R . . H40B H -0.5055 1.3713 0.9372 0.146 Uiso 1 1 calc R . . H40C H -0.4210 1.3391 1.0019 0.146 Uiso 1 1 calc R . . C41 C 0.1859(7) 0.9211(4) 0.8693(3) 0.0800(18) Uani 1 1 d . . . H41A H 0.2529 0.9098 0.8189 0.120 Uiso 1 1 calc R . . H41B H 0.2334 0.9022 0.9110 0.120 Uiso 1 1 calc R . . H41C H 0.1376 0.9852 0.8705 0.120 Uiso 1 1 calc R . . C42 C -0.0497(8) 0.8686(6) 0.9887(4) 0.110(3) Uani 1 1 d . . . H42A H -0.1216 0.8387 0.9987 0.165 Uiso 1 1 calc R . . H42B H -0.0919 0.9324 0.9966 0.165 Uiso 1 1 calc R . . H42C H 0.0086 0.8414 1.0244 0.165 Uiso 1 1 calc R . . C43 C 0.1622(8) 0.7343(4) 0.8773(4) 0.095(2) Uani 1 1 d . . . H43A H 0.1004 0.6966 0.8882 0.142 Uiso 1 1 calc R . . H43B H 0.2171 0.7172 0.9154 0.142 Uiso 1 1 calc R . . H43C H 0.2230 0.7261 0.8248 0.142 Uiso 1 1 calc R . . C44 C -0.1919(8) 0.7496(5) 0.8858(4) 0.104(2) Uani 1 1 d . . . H44A H -0.1115 0.7045 0.8587 0.156 Uiso 1 1 calc R . . H44B H -0.2753 0.7349 0.8871 0.156 Uiso 1 1 calc R . . H44C H -0.1869 0.7501 0.9391 0.156 Uiso 1 1 calc R . . C45 C -0.2337(10) 0.8587(7) 0.7382(5) 0.144(3) Uani 1 1 d U . . H45A H -0.2725 0.9197 0.7171 0.216 Uiso 1 1 calc R . . H45B H -0.2996 0.8242 0.7473 0.216 Uiso 1 1 calc R . . H45C H -0.1489 0.8298 0.7009 0.216 Uiso 1 1 calc R . . C46 C -0.3458(9) 0.9448(7) 0.8930(6) 0.167(4) Uani 1 1 d U . . H46A H -0.3242 0.9519 0.9404 0.251 Uiso 1 1 calc R . . H46B H -0.4261 0.9222 0.9070 0.251 Uiso 1 1 calc R . . H46C H -0.3654 1.0030 0.8629 0.251 Uiso 1 1 calc R . . C49 C 0.9867(13) 0.4822(9) 0.9719(6) 0.169(5) Uani 1 1 d DU . . H49A H 1.0299 0.4166 0.9729 0.203 Uiso 1 1 calc R . . H49B H 1.0223 0.5098 0.9196 0.203 Uiso 1 1 calc R . . C47 C 0.8329(13) 0.5031(9) 0.9911(8) 0.193(5) Uani 1 1 d DU . . H47A H 0.7914 0.5685 0.9947 0.232 Uiso 1 1 calc R . . H47B H 0.8000 0.4725 1.0424 0.232 Uiso 1 1 calc R . . C48 C 0.7868(18) 0.4736(11) 0.9305(9) 0.280(9) Uani 1 1 d DU . . H48A H 0.8020 0.5125 0.8823 0.420 Uiso 1 1 calc R . . H48B H 0.6891 0.4777 0.9496 0.420 Uiso 1 1 calc R . . H48C H 0.8394 0.4115 0.9202 0.420 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 Sn1 0.0446(2) 0.0490(2) 0.0549(2) 0.00569(15) -0.01040(17) -0.01913(16) P1 0.0383(7) 0.0389(7) 0.0497(7) -0.0031(5) -0.0084(6) -0.0128(5) P2 0.0415(7) 0.0356(6) 0.0489(7) 0.0013(5) -0.0062(6) -0.0128(5) Si1 0.0504(9) 0.0539(9) 0.0751(11) 0.0080(7) -0.0226(8) -0.0178(7) Si2 0.0738(11) 0.0536(9) 0.0439(8) 0.0027(7) -0.0043(7) -0.0218(8) Si3 0.0560(11) 0.0731(12) 0.1078(15) 0.0082(10) 0.0008(10) -0.0319(9) N1 0.046(2) 0.050(2) 0.069(3) 0.002(2) -0.016(2) -0.016(2) N2 0.041(2) 0.039(2) 0.042(2) -0.0010(17) -0.0029(18) -0.0132(18) N3 0.040(2) 0.037(2) 0.057(3) 0.0028(18) 0.003(2) -0.0108(18) N4 0.047(2) 0.045(2) 0.058(3) 0.0035(19) 0.000(2) -0.0211(19) C1 0.035(3) 0.042(3) 0.056(3) 0.004(2) -0.012(2) -0.012(2) C2 0.072(4) 0.083(4) 0.081(4) -0.012(3) -0.005(4) -0.041(4) C3 0.072(4) 0.082(5) 0.109(5) -0.007(4) 0.001(4) -0.044(4) C4 0.066(4) 0.051(4) 0.124(6) 0.022(4) -0.032(4) -0.032(3) C5 0.103(6) 0.057(4) 0.140(7) -0.018(4) -0.025(5) -0.038(4) C6 0.086(5) 0.050(3) 0.110(5) -0.029(3) -0.002(4) -0.034(3) C7 0.044(3) 0.069(4) 0.051(3) -0.004(3) -0.006(3) -0.032(3) C8 0.064(4) 0.106(5) 0.068(4) -0.028(4) 0.004(3) -0.044(4) C9 0.113(7) 0.208(11) 0.068(6) -0.055(6) 0.027(5) -0.110(8) C10 0.131(10) 0.256(15) 0.060(5) 0.019(7) -0.018(6) -0.140(10) C11 0.097(6) 0.175(9) 0.082(6) 0.060(6) -0.046(5) -0.080(6) C12 0.062(4) 0.092(5) 0.068(4) 0.021(3) -0.027(3) -0.037(3) C13 0.121(6) 0.132(7) 0.110(6) -0.008(5) -0.056(5) -0.062(5) C14 0.074(4) 0.081(5) 0.092(5) 0.019(4) -0.009(4) -0.023(4) C15 0.058(4) 0.077(4) 0.111(5) 0.019(4) -0.012(4) -0.009(3) C16 0.038(3) 0.046(3) 0.053(3) -0.008(2) 0.004(2) -0.016(2) C17 0.040(3) 0.040(3) 0.041(3) -0.003(2) -0.005(2) -0.014(2) C18 0.046(3) 0.042(3) 0.066(3) -0.011(2) -0.006(3) -0.010(2) C19 0.037(3) 0.057(3) 0.081(4) -0.011(3) 0.002(3) -0.015(3) C20 0.048(3) 0.042(3) 0.080(4) -0.006(3) -0.006(3) -0.022(2) C21 0.042(3) 0.042(3) 0.047(3) -0.001(2) -0.007(2) -0.015(2) C22 0.044(3) 0.039(3) 0.053(3) 0.003(2) -0.009(2) -0.013(2) C23 0.044(3) 0.050(3) 0.053(3) 0.001(2) -0.006(2) -0.017(2) C24 0.062(4) 0.047(3) 0.057(3) 0.005(2) -0.002(3) -0.022(3) C25 0.088(5) 0.086(5) 0.075(4) 0.033(3) -0.035(4) -0.034(4) C26 0.104(6) 0.134(6) 0.116(6) 0.068(5) -0.074(5) -0.069(5) C27 0.060(4) 0.089(4) 0.095(5) 0.041(4) -0.036(4) -0.041(3) C28 0.047(3) 0.046(3) 0.046(3) -0.008(2) 0.001(2) -0.018(2) C29 0.075(4) 0.051(3) 0.059(3) -0.013(3) -0.009(3) -0.014(3) C30 0.111(6) 0.070(4) 0.075(4) -0.032(4) 0.001(4) -0.036(4) C31 0.116(6) 0.109(6) 0.058(4) -0.022(4) -0.015(4) -0.049(5) C32 0.080(5) 0.107(6) 0.057(4) 0.000(4) -0.021(3) -0.040(4) C33 0.058(3) 0.059(3) 0.063(4) 0.000(3) -0.014(3) -0.022(3) C34 0.044(3) 0.044(3) 0.053(3) -0.004(2) -0.004(3) -0.011(2) C35 0.081(5) 0.058(4) 0.091(5) 0.011(3) 0.030(4) 0.009(3) C36 0.089(5) 0.063(4) 0.110(6) 0.010(4) 0.016(5) 0.016(4) C37 0.049(4) 0.079(4) 0.071(4) -0.009(3) -0.003(3) -0.006(3) C38 0.084(5) 0.091(5) 0.060(4) -0.003(4) 0.010(4) -0.019(4) C39 0.079(4) 0.059(4) 0.059(4) 0.000(3) 0.006(3) -0.009(3) C40 0.065(4) 0.107(6) 0.093(5) -0.033(4) 0.007(4) 0.001(4) C41 0.105(5) 0.087(5) 0.064(4) 0.014(3) -0.035(4) -0.046(4) C42 0.141(7) 0.132(7) 0.053(4) -0.006(4) 0.001(4) -0.059(6) C43 0.124(6) 0.062(4) 0.091(5) 0.005(3) -0.043(4) -0.008(4) C44 0.106(6) 0.104(6) 0.104(6) 0.012(4) 0.003(4) -0.070(5) C45 0.143(6) 0.170(7) 0.164(7) 0.050(5) -0.071(5) -0.108(6) C46 0.104(6) 0.146(7) 0.224(8) -0.023(6) 0.009(6) -0.040(5) C49 0.171(7) 0.133(7) 0.152(8) -0.008(6) 0.002(7) -0.014(6) C47 0.209(9) 0.148(8) 0.196(9) 0.024(7) -0.029(7) -0.054(7) C48 0.304(12) 0.258(12) 0.274(12) -0.015(9) -0.053(9) -0.096(9) _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 N4 2.108(4) . ? Sn1 N2 2.209(4) . ? Sn1 N3 2.239(4) . ? P1 N1 1.539(4) . ? P1 C16 1.733(5) . ? P1 C7 1.808(5) . ? P1 C1 1.811(5) . ? P2 N3 1.597(4) . ? P2 C21 1.786(5) . ? P2 C28 1.787(5) . ? P2 C22 1.797(5) . ? Si1 N1 1.664(4) . ? Si1 C13 1.844(7) . ? Si1 C15 1.858(6) . ? Si1 C14 1.872(6) . ? Si2 N4 1.724(4) . ? Si2 C43 1.847(6) . ? Si2 C41 1.849(6) . ? Si2 C42 1.867(6) . ? Si3 N4 1.720(4) . ? Si3 C44 1.841(6) . ? Si3 C46 1.844(9) . ? Si3 C45 1.847(9) . ? N2 C21 1.357(6) . ? N2 C17 1.378(6) . ? N3 C34 1.417(6) . ? C1 C2 1.343(7) . ? C1 C6 1.362(7) . ? C2 C3 1.384(8) . ? C2 H2 0.9300 . ? C3 C4 1.315(9) . ? C3 H3 0.9300 . ? C4 C5 1.338(9) . ? C4 H4 0.9300 . ? C5 C6 1.377(8) . ? C5 H5 0.9300 . ? C6 H6 0.9300 . ? C7 C12 1.373(7) . ? C7 C8 1.378(8) . ? C8 C9 1.396(10) . ? C8 H8 0.9300 . ? C9 C10 1.362(13) . ? C9 H9 0.9300 . ? C10 C11 1.338(13) . ? C10 H10 0.9300 . ? C11 C12 1.376(9) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 H13A 0.9600 . ? C13 H13B 0.9600 . ? C13 H13C 0.9600 . ? C14 H14A 0.9600 . ? C14 H14B 0.9600 . ? C14 H14C 0.9600 . ? C15 H15A 0.9600 . ? C15 H15B 0.9600 . ? C15 H15C 0.9600 . ? C16 C17 1.374(6) . ? C16 H16 0.9300 . ? C17 C18 1.416(7) . ? C18 C19 1.339(7) . ? C18 H18 0.9300 . ? C19 C20 1.404(7) . ? C19 H19 0.9300 . ? C20 C21 1.347(7) . ? C20 H20 0.9300 . ? C22 C27 1.362(7) . ? C22 C23 1.375(6) . ? C23 C24 1.366(6) . ? C23 H23 0.9300 . ? C24 C25 1.346(8) . ? C24 H24 0.9300 . ? C25 C26 1.357(9) . ? C25 H25 0.9300 . ? C26 C27 1.378(8) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.374(7) . ? C28 C33 1.377(7) . ? C29 C30 1.361(8) . ? C29 H29 0.9300 . ? C30 C31 1.361(9) . ? C30 H30 0.9300 . ? C31 C32 1.342(9) . ? C31 H31 0.9300 . ? C32 C33 1.373(8) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 C35 1.348(7) . ? C34 C39 1.365(7) . ? C35 C36 1.379(8) . ? C35 H35 0.9300 . ? C36 C37 1.341(8) . ? C36 H36 0.9300 . ? C37 C38 1.334(8) . ? C37 C40 1.515(8) . ? C38 C39 1.379(8) . ? C38 H38 0.9300 . ? C39 H39 0.9300 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? C43 H43A 0.9600 . ? C43 H43B 0.9600 . ? C43 H43C 0.9600 . ? C44 H44A 0.9600 . ? C44 H44B 0.9600 . ? C44 H44C 0.9600 . ? C45 H45A 0.9600 . ? C45 H45B 0.9600 . ? C45 H45C 0.9600 . ? C46 H46A 0.9600 . ? C46 H46B 0.9600 . ? C46 H46C 0.9600 . ? C49 C49 1.343(19) 2_767 ? C49 C47 1.477(9) . ? C49 H49A 0.9700 . ? C49 H49B 0.9700 . ? C47 C48 1.480(9) . ? C47 H47A 0.9700 . ? C47 H47B 0.9700 . ? C48 H48A 0.9600 . ? C48 H48B 0.9600 . ? C48 H48C 0.9600 . ? 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 N4 Sn1 N2 102.79(14) . . ? N4 Sn1 N3 101.47(14) . . ? N2 Sn1 N3 77.77(14) . . ? N1 P1 C16 121.0(2) . . ? N1 P1 C7 107.0(2) . . ? C16 P1 C7 106.4(2) . . ? N1 P1 C1 111.7(2) . . ? C16 P1 C1 105.0(2) . . ? C7 P1 C1 104.5(2) . . ? N3 P2 C21 103.8(2) . . ? N3 P2 C28 115.2(2) . . ? C21 P2 C28 110.4(2) . . ? N3 P2 C22 114.2(2) . . ? C21 P2 C22 105.8(2) . . ? C28 P2 C22 107.1(2) . . ? N1 Si1 C13 110.6(3) . . ? N1 Si1 C15 107.7(3) . . ? C13 Si1 C15 109.0(3) . . ? N1 Si1 C14 114.0(3) . . ? C13 Si1 C14 107.4(3) . . ? C15 Si1 C14 108.1(3) . . ? N4 Si2 C43 112.2(3) . . ? N4 Si2 C41 112.8(2) . . ? C43 Si2 C41 106.0(3) . . ? N4 Si2 C42 112.0(3) . . ? C43 Si2 C42 107.5(3) . . ? C41 Si2 C42 105.9(3) . . ? N4 Si3 C44 113.7(3) . . ? N4 Si3 C46 111.9(4) . . ? C44 Si3 C46 105.8(4) . . ? N4 Si3 C45 111.3(3) . . ? C44 Si3 C45 105.1(4) . . ? C46 Si3 C45 108.5(5) . . ? P1 N1 Si1 138.1(3) . . ? C21 N2 C17 119.6(4) . . ? C21 N2 Sn1 119.4(3) . . ? C17 N2 Sn1 119.4(3) . . ? C34 N3 P2 123.4(3) . . ? C34 N3 Sn1 120.5(3) . . ? P2 N3 Sn1 114.1(2) . . ? Si3 N4 Si2 121.4(2) . . ? Si3 N4 Sn1 111.4(2) . . ? Si2 N4 Sn1 127.2(2) . . ? C2 C1 C6 116.2(5) . . ? C2 C1 P1 124.1(4) . . ? C6 C1 P1 119.4(4) . . ? C1 C2 C3 122.2(6) . . ? C1 C2 H2 118.9 . . ? C3 C2 H2 118.9 . . ? C4 C3 C2 119.9(7) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 120.3(6) . . ? C3 C4 H4 119.8 . . ? C5 C4 H4 119.8 . . ? C4 C5 C6 119.5(7) . . ? C4 C5 H5 120.2 . . ? C6 C5 H5 120.2 . . ? C1 C6 C5 121.8(6) . . ? C1 C6 H6 119.1 . . ? C5 C6 H6 119.1 . . ? C12 C7 C8 118.9(6) . . ? C12 C7 P1 121.9(4) . . ? C8 C7 P1 119.1(5) . . ? C7 C8 C9 119.4(7) . . ? C7 C8 H8 120.3 . . ? C9 C8 H8 120.3 . . ? C10 C9 C8 120.2(9) . . ? C10 C9 H9 119.9 . . ? C8 C9 H9 119.9 . . ? C11 C10 C9 120.2(9) . . ? C11 C10 H10 119.9 . . ? C9 C10 H10 119.9 . . ? C10 C11 C12 120.8(9) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C7 C12 C11 120.5(7) . . ? C7 C12 H12 119.8 . . ? C11 C12 H12 119.8 . . ? Si1 C13 H13A 109.5 . . ? Si1 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? Si1 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? Si1 C14 H14A 109.5 . . ? Si1 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? Si1 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? Si1 C15 H15A 109.5 . . ? Si1 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? Si1 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C17 C16 P1 124.8(4) . . ? C17 C16 H16 117.6 . . ? P1 C16 H16 117.6 . . ? C16 C17 N2 119.6(4) . . ? C16 C17 C18 122.8(4) . . ? N2 C17 C18 117.5(4) . . ? C19 C18 C17 121.6(5) . . ? C19 C18 H18 119.2 . . ? C17 C18 H18 119.2 . . ? C18 C19 C20 119.8(5) . . ? C18 C19 H19 120.1 . . ? C20 C19 H19 120.1 . . ? C21 C20 C19 118.1(5) . . ? C21 C20 H20 121.0 . . ? C19 C20 H20 121.0 . . ? C20 C21 N2 123.3(4) . . ? C20 C21 P2 120.8(4) . . ? N2 C21 P2 115.6(3) . . ? C27 C22 C23 118.9(5) . . ? C27 C22 P2 119.2(4) . . ? C23 C22 P2 121.6(4) . . ? C24 C23 C22 120.7(5) . . ? C24 C23 H23 119.7 . . ? C22 C23 H23 119.7 . . ? C25 C24 C23 119.8(5) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C24 C25 C26 120.9(6) . . ? C24 C25 H25 119.6 . . ? C26 C25 H25 119.6 . . ? C25 C26 C27 119.6(6) . . ? C25 C26 H26 120.2 . . ? C27 C26 H26 120.2 . . ? C22 C27 C26 120.2(5) . . ? C22 C27 H27 119.9 . . ? C26 C27 H27 119.9 . . ? C29 C28 C33 118.6(5) . . ? C29 C28 P2 120.1(4) . . ? C33 C28 P2 121.1(4) . . ? C30 C29 C28 120.8(6) . . ? C30 C29 H29 119.6 . . ? C28 C29 H29 119.6 . . ? C29 C30 C31 119.9(6) . . ? C29 C30 H30 120.0 . . ? C31 C30 H30 120.0 . . ? C32 C31 C30 120.1(6) . . ? C32 C31 H31 120.0 . . ? C30 C31 H31 120.0 . . ? C31 C32 C33 120.9(6) . . ? C31 C32 H32 119.5 . . ? C33 C32 H32 119.5 . . ? C32 C33 C28 119.6(6) . . ? C32 C33 H33 120.2 . . ? C28 C33 H33 120.2 . . ? C35 C34 C39 115.7(5) . . ? C35 C34 N3 124.7(5) . . ? C39 C34 N3 119.5(4) . . ? C34 C35 C36 121.5(6) . . ? C34 C35 H35 119.3 . . ? C36 C35 H35 119.3 . . ? C37 C36 C35 122.4(6) . . ? C37 C36 H36 118.8 . . ? C35 C36 H36 118.8 . . ? C38 C37 C36 116.5(6) . . ? C38 C37 C40 121.1(6) . . ? C36 C37 C40 122.3(6) . . ? C37 C38 C39 122.0(6) . . ? C37 C38 H38 119.0 . . ? C39 C38 H38 119.0 . . ? C34 C39 C38 121.8(6) . . ? C34 C39 H39 119.1 . . ? C38 C39 H39 119.1 . . ? C37 C40 H40A 109.5 . . ? C37 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? C37 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? Si2 C41 H41A 109.5 . . ? Si2 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si2 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si2 C42 H42A 109.5 . . ? Si2 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si2 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? Si2 C43 H43A 109.5 . . ? Si2 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? Si2 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? Si3 C44 H44A 109.5 . . ? Si3 C44 H44B 109.5 . . ? H44A C44 H44B 109.5 . . ? Si3 C44 H44C 109.5 . . ? H44A C44 H44C 109.5 . . ? H44B C44 H44C 109.5 . . ? Si3 C45 H45A 109.5 . . ? Si3 C45 H45B 109.5 . . ? H45A C45 H45B 109.5 . . ? Si3 C45 H45C 109.5 . . ? H45A C45 H45C 109.5 . . ? H45B C45 H45C 109.5 . . ? Si3 C46 H46A 109.5 . . ? Si3 C46 H46B 109.5 . . ? H46A C46 H46B 109.5 . . ? Si3 C46 H46C 109.5 . . ? H46A C46 H46C 109.5 . . ? H46B C46 H46C 109.5 . . ? C49 C49 C47 105.8(13) 2_767 . ? C49 C49 H49A 110.6 2_767 . ? C47 C49 H49A 110.6 . . ? C49 C49 H49B 110.6 2_767 . ? C47 C49 H49B 110.6 . . ? H49A C49 H49B 108.7 . . ? C49 C47 C48 112.0(13) . . ? C49 C47 H47A 109.2 . . ? C48 C47 H47A 109.2 . . ? C49 C47 H47B 109.2 . . ? C48 C47 H47B 109.2 . . ? H47A C47 H47B 107.9 . . ? C47 C48 H48A 109.5 . . ? C47 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C47 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C16 P1 N1 Si1 63.5(5) . . . . ? C7 P1 N1 Si1 -174.7(4) . . . . ? C1 P1 N1 Si1 -60.9(5) . . . . ? C13 Si1 N1 P1 -86.2(5) . . . . ? C15 Si1 N1 P1 154.8(4) . . . . ? C14 Si1 N1 P1 34.9(5) . . . . ? N4 Sn1 N2 C21 -119.6(3) . . . . ? N3 Sn1 N2 C21 -20.4(3) . . . . ? N4 Sn1 N2 C17 74.7(3) . . . . ? N3 Sn1 N2 C17 173.9(3) . . . . ? C21 P2 N3 C34 166.4(4) . . . . ? C28 P2 N3 C34 45.6(5) . . . . ? C22 P2 N3 C34 -79.0(4) . . . . ? C21 P2 N3 Sn1 -29.9(3) . . . . ? C28 P2 N3 Sn1 -150.6(2) . . . . ? C22 P2 N3 Sn1 84.8(3) . . . . ? N4 Sn1 N3 C34 -66.5(3) . . . . ? N2 Sn1 N3 C34 -167.3(4) . . . . ? N4 Sn1 N3 P2 129.3(2) . . . . ? N2 Sn1 N3 P2 28.5(2) . . . . ? C44 Si3 N4 Si2 -33.5(4) . . . . ? C46 Si3 N4 Si2 86.4(5) . . . . ? C45 Si3 N4 Si2 -151.9(4) . . . . ? C44 Si3 N4 Sn1 147.8(3) . . . . ? C46 Si3 N4 Sn1 -92.3(4) . . . . ? C45 Si3 N4 Sn1 29.3(4) . . . . ? C43 Si2 N4 Si3 77.3(4) . . . . ? C41 Si2 N4 Si3 -163.1(3) . . . . ? C42 Si2 N4 Si3 -43.8(4) . . . . ? C43 Si2 N4 Sn1 -104.2(3) . . . . ? C41 Si2 N4 Sn1 15.4(4) . . . . ? C42 Si2 N4 Sn1 134.8(3) . . . . ? N2 Sn1 N4 Si3 -156.2(2) . . . . ? N3 Sn1 N4 Si3 124.0(2) . . . . ? N2 Sn1 N4 Si2 25.2(3) . . . . ? N3 Sn1 N4 Si2 -54.7(3) . . . . ? N1 P1 C1 C2 106.3(5) . . . . ? C16 P1 C1 C2 -26.5(5) . . . . ? C7 P1 C1 C2 -138.3(5) . . . . ? N1 P1 C1 C6 -66.7(5) . . . . ? C16 P1 C1 C6 160.5(4) . . . . ? C7 P1 C1 C6 48.7(5) . . . . ? C6 C1 C2 C3 0.6(9) . . . . ? P1 C1 C2 C3 -172.6(5) . . . . ? C1 C2 C3 C4 1.2(11) . . . . ? C2 C3 C4 C5 -2.9(11) . . . . ? C3 C4 C5 C6 2.9(11) . . . . ? C2 C1 C6 C5 -0.6(9) . . . . ? P1 C1 C6 C5 173.0(5) . . . . ? C4 C5 C6 C1 -1.1(11) . . . . ? N1 P1 C7 C12 -149.2(4) . . . . ? C16 P1 C7 C12 -18.6(5) . . . . ? C1 P1 C7 C12 92.2(4) . . . . ? N1 P1 C7 C8 31.6(5) . . . . ? C16 P1 C7 C8 162.2(4) . . . . ? C1 P1 C7 C8 -87.0(4) . . . . ? C12 C7 C8 C9 -1.5(8) . . . . ? P1 C7 C8 C9 177.8(5) . . . . ? C7 C8 C9 C10 2.0(11) . . . . ? C8 C9 C10 C11 -1.2(13) . . . . ? C9 C10 C11 C12 0.1(13) . . . . ? C8 C7 C12 C11 0.4(8) . . . . ? P1 C7 C12 C11 -178.8(5) . . . . ? C10 C11 C12 C7 0.3(11) . . . . ? N1 P1 C16 C17 58.0(5) . . . . ? C7 P1 C16 C17 -64.2(5) . . . . ? C1 P1 C16 C17 -174.6(4) . . . . ? P1 C16 C17 N2 169.2(3) . . . . ? P1 C16 C17 C18 -9.4(7) . . . . ? C21 N2 C17 C16 179.7(4) . . . . ? Sn1 N2 C17 C16 -14.6(5) . . . . ? C21 N2 C17 C18 -1.6(6) . . . . ? Sn1 N2 C17 C18 164.1(3) . . . . ? C16 C17 C18 C19 -179.5(5) . . . . ? N2 C17 C18 C19 1.9(7) . . . . ? C17 C18 C19 C20 -0.6(8) . . . . ? C18 C19 C20 C21 -1.0(8) . . . . ? C19 C20 C21 N2 1.3(8) . . . . ? C19 C20 C21 P2 -172.6(4) . . . . ? C17 N2 C21 C20 0.1(7) . . . . ? Sn1 N2 C21 C20 -165.6(4) . . . . ? C17 N2 C21 P2 174.2(3) . . . . ? Sn1 N2 C21 P2 8.5(5) . . . . ? N3 P2 C21 C20 -171.5(4) . . . . ? C28 P2 C21 C20 -47.5(5) . . . . ? C22 P2 C21 C20 68.0(5) . . . . ? N3 P2 C21 N2 14.2(4) . . . . ? C28 P2 C21 N2 138.2(3) . . . . ? C22 P2 C21 N2 -106.3(4) . . . . ? N3 P2 C22 C27 -14.8(5) . . . . ? C21 P2 C22 C27 98.7(5) . . . . ? C28 P2 C22 C27 -143.6(5) . . . . ? N3 P2 C22 C23 171.2(4) . . . . ? C21 P2 C22 C23 -75.4(5) . . . . ? C28 P2 C22 C23 42.4(5) . . . . ? C27 C22 C23 C24 0.7(8) . . . . ? P2 C22 C23 C24 174.8(4) . . . . ? C22 C23 C24 C25 0.3(8) . . . . ? C23 C24 C25 C26 -0.8(10) . . . . ? C24 C25 C26 C27 0.4(12) . . . . ? C23 C22 C27 C26 -1.2(10) . . . . ? P2 C22 C27 C26 -175.4(6) . . . . ? C25 C26 C27 C22 0.6(12) . . . . ? N3 P2 C28 C29 -91.5(4) . . . . ? C21 P2 C28 C29 151.5(4) . . . . ? C22 P2 C28 C29 36.7(5) . . . . ? N3 P2 C28 C33 84.7(5) . . . . ? C21 P2 C28 C33 -32.4(5) . . . . ? C22 P2 C28 C33 -147.1(4) . . . . ? C33 C28 C29 C30 -1.1(8) . . . . ? P2 C28 C29 C30 175.2(5) . . . . ? C28 C29 C30 C31 1.3(10) . . . . ? C29 C30 C31 C32 -0.2(11) . . . . ? C30 C31 C32 C33 -1.1(10) . . . . ? C31 C32 C33 C28 1.3(9) . . . . ? C29 C28 C33 C32 -0.2(8) . . . . ? P2 C28 C33 C32 -176.5(4) . . . . ? P2 N3 C34 C35 39.6(8) . . . . ? Sn1 N3 C34 C35 -123.2(6) . . . . ? P2 N3 C34 C39 -143.7(5) . . . . ? Sn1 N3 C34 C39 53.5(6) . . . . ? C39 C34 C35 C36 4.3(11) . . . . ? N3 C34 C35 C36 -178.8(7) . . . . ? C34 C35 C36 C37 -3.7(13) . . . . ? C35 C36 C37 C38 1.0(12) . . . . ? C35 C36 C37 C40 178.2(7) . . . . ? C36 C37 C38 C39 0.6(11) . . . . ? C40 C37 C38 C39 -176.7(6) . . . . ? C35 C34 C39 C38 -2.8(9) . . . . ? N3 C34 C39 C38 -179.8(6) . . . . ? C37 C38 C39 C34 0.3(11) . . . . ? C49 C49 C47 C48 175.9(15) 2_767 . . . ? _diffrn_measured_fraction_theta_max 0.924 _diffrn_reflns_theta_full 25.02 _diffrn_measured_fraction_theta_full 0.924 _refine_diff_density_max 0.964 _refine_diff_density_min -0.366 _refine_diff_density_rms 0.068 #====END data_12 _database_code_depnum_ccdc_archive 'CCDC 725695' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H60 N4 P2 Si4 Yb' _chemical_formula_weight 968.28 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Yb Yb -0.3850 5.5486 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 14.9293(17) _cell_length_b 13.9411(15) _cell_length_c 23.677(2) _cell_angle_alpha 90.00 _cell_angle_beta 105.018(2) _cell_angle_gamma 90.00 _cell_volume 4759.6(9) _cell_formula_units_Z 4 _cell_measurement_temperature 293(2) _cell_measurement_reflns_used 3235 _cell_measurement_theta_min 2.304 _cell_measurement_theta_max 25.214 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.351 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1984 _exptl_absorpt_coefficient_mu 2.165 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6714 _exptl_absorpt_correction_T_max 0.8290 _exptl_absorpt_process_details sadabs _exptl_special_details ; ? ; _diffrn_ambient_temperature 293(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 24375 _diffrn_reflns_av_R_equivalents 0.1532 _diffrn_reflns_av_sigmaI/netI 0.1744 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -28 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 1.46 _diffrn_reflns_theta_max 25.01 _reflns_number_total 8345 _reflns_number_gt 3701 _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^)+(0.0481P)^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 8345 _refine_ls_number_parameters 478 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.1679 _refine_ls_R_factor_gt 0.0681 _refine_ls_wR_factor_ref 0.1604 _refine_ls_wR_factor_gt 0.1337 _refine_ls_goodness_of_fit_ref 0.995 _refine_ls_restrained_S_all 0.995 _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 Yb1 Yb -0.00641(3) 0.75229(5) 0.777000(19) 0.04598(17) Uani 1 1 d . . . N1 N 0.1145(6) 0.6604(7) 0.7579(4) 0.046(2) Uani 1 1 d . . . N2 N -0.0017(7) 0.5979(7) 0.8337(4) 0.054(3) Uani 1 1 d . . . N3 N -0.0609(6) 0.7572(7) 0.6703(3) 0.051(2) Uani 1 1 d . . . N4 N 0.0408(7) 0.8836(7) 0.8390(4) 0.058(3) Uani 1 1 d . . . P1 P 0.0650(2) 0.5237(2) 0.81826(13) 0.0477(8) Uani 1 1 d . . . P2 P 0.0220(2) 0.7887(2) 0.64664(12) 0.0444(8) Uani 1 1 d . . . Si1 Si -0.0618(3) 0.6024(3) 0.88641(15) 0.0560(10) Uani 1 1 d . . . Si2 Si -0.1594(2) 0.6921(3) 0.64181(14) 0.0533(9) Uani 1 1 d . . . Si3 Si -0.0391(3) 0.9697(3) 0.83094(16) 0.0652(11) Uani 1 1 d . . . Si4 Si 0.1498(3) 0.8902(3) 0.88070(14) 0.0584(10) Uani 1 1 d . . . C1 C 0.1514(8) 0.5839(8) 0.7923(5) 0.049(3) Uani 1 1 d . . . C2 C 0.2432(9) 0.5628(9) 0.8043(5) 0.053(3) Uani 1 1 d . . . H2 H 0.2667 0.5092 0.8266 0.064 Uiso 1 1 calc R . . C3 C 0.3011(9) 0.6213(9) 0.7833(5) 0.054(3) Uani 1 1 d . . . H3 H 0.3644 0.6087 0.7924 0.065 Uiso 1 1 calc R . . C4 C 0.2664(8) 0.6963(9) 0.7497(5) 0.052(3) Uani 1 1 d . . . H4 H 0.3063 0.7370 0.7367 0.062 Uiso 1 1 calc R . . C5 C 0.1707(9) 0.7150(8) 0.7336(5) 0.047(3) Uani 1 1 d . . . C6 C 0.1306(8) 0.7917(9) 0.6965(4) 0.050(3) Uani 1 1 d . . . H6 H 0.1649 0.8479 0.6989 0.060 Uiso 1 1 calc R . . C7 C 0.0093(10) 0.4427(9) 0.7593(5) 0.057(3) Uani 1 1 d . . . C8 C 0.0620(10) 0.4034(9) 0.7251(5) 0.061(3) Uani 1 1 d . . . H8 H 0.1242 0.4196 0.7313 0.073 Uiso 1 1 calc R . . C9 C 0.0203(11) 0.3384(10) 0.6809(6) 0.068(4) Uani 1 1 d . . . H9 H 0.0539 0.3124 0.6566 0.081 Uiso 1 1 calc R . . C10 C -0.0658(11) 0.3151(10) 0.6745(6) 0.070(4) Uani 1 1 d . . . H10 H -0.0928 0.2720 0.6450 0.084 Uiso 1 1 calc R . . C11 C -0.1172(10) 0.3491(10) 0.7075(6) 0.072(4) Uani 1 1 d . . . H11 H -0.1780 0.3281 0.7022 0.086 Uiso 1 1 calc R . . C12 C -0.0795(10) 0.4176(10) 0.7511(5) 0.064(4) Uani 1 1 d . . . H12 H -0.1156 0.4446 0.7736 0.077 Uiso 1 1 calc R . . C13 C 0.1266(9) 0.4475(10) 0.8776(5) 0.058(3) Uani 1 1 d . . . C14 C 0.1834(9) 0.4905(10) 0.9250(5) 0.064(4) Uani 1 1 d . . . H14 H 0.1889 0.5569 0.9258 0.076 Uiso 1 1 calc R . . C15 C 0.2332(9) 0.4376(11) 0.9723(6) 0.069(4) Uani 1 1 d . . . H15 H 0.2698 0.4676 1.0054 0.083 Uiso 1 1 calc R . . C16 C 0.2268(10) 0.3400(11) 0.9689(6) 0.073(4) Uani 1 1 d . . . H16 H 0.2626 0.3033 0.9992 0.088 Uiso 1 1 calc R . . C17 C 0.1706(10) 0.2956(11) 0.9233(6) 0.077(4) Uani 1 1 d . . . H17 H 0.1652 0.2291 0.9236 0.092 Uiso 1 1 calc R . . C18 C 0.1199(9) 0.3477(10) 0.8753(6) 0.068(4) Uani 1 1 d . . . H18 H 0.0828 0.3168 0.8427 0.082 Uiso 1 1 calc R . . C19 C -0.1167(11) 0.4891(11) 0.8961(6) 0.095(5) Uani 1 1 d . . . H19A H -0.0714 0.4386 0.9021 0.143 Uiso 1 1 calc R . . H19B H -0.1656 0.4755 0.8618 0.143 Uiso 1 1 calc R . . H19C H -0.1418 0.4934 0.9294 0.143 Uiso 1 1 calc R . . C20 C 0.0075(11) 0.6420(12) 0.9572(6) 0.094(5) Uani 1 1 d . . . H20A H 0.0408 0.5884 0.9780 0.141 Uiso 1 1 calc R . . H20B H -0.0323 0.6686 0.9791 0.141 Uiso 1 1 calc R . . H20C H 0.0507 0.6900 0.9519 0.141 Uiso 1 1 calc R . . C21 C -0.1534(10) 0.6941(12) 0.8661(6) 0.098(5) Uani 1 1 d . . . H21A H -0.1263 0.7541 0.8594 0.147 Uiso 1 1 calc R . . H21B H -0.1833 0.7013 0.8972 0.147 Uiso 1 1 calc R . . H21C H -0.1982 0.6746 0.8311 0.147 Uiso 1 1 calc R . . C22 C 0.0301(9) 0.7229(8) 0.5823(5) 0.053(3) Uani 1 1 d . . . C23 C -0.0338(8) 0.7349(9) 0.5302(5) 0.057(3) Uani 1 1 d . . . H23 H -0.0793 0.7814 0.5273 0.068 Uiso 1 1 calc R . . C24 C -0.0337(9) 0.6802(10) 0.4808(5) 0.061(3) Uani 1 1 d . . . H24 H -0.0803 0.6873 0.4463 0.074 Uiso 1 1 calc R . . C25 C 0.0345(10) 0.6179(9) 0.4844(6) 0.062(4) Uani 1 1 d . . . H25 H 0.0382 0.5829 0.4516 0.075 Uiso 1 1 calc R . . C26 C 0.0956(10) 0.6057(10) 0.5333(6) 0.071(4) Uani 1 1 d . . . H26 H 0.1414 0.5598 0.5350 0.086 Uiso 1 1 calc R . . C27 C 0.0975(9) 0.6582(9) 0.5850(5) 0.059(3) Uani 1 1 d . . . H27 H 0.1437 0.6481 0.6193 0.071 Uiso 1 1 calc R . . C28 C 0.0069(9) 0.9101(9) 0.6204(5) 0.050(3) Uani 1 1 d . . . C29 C 0.0625(9) 0.9524(9) 0.5904(5) 0.054(3) Uani 1 1 d . . . H29 H 0.1110 0.9175 0.5826 0.065 Uiso 1 1 calc R . . C30 C 0.0484(9) 1.0463(10) 0.5713(5) 0.061(3) Uani 1 1 d . . . H30 H 0.0867 1.0746 0.5507 0.073 Uiso 1 1 calc R . . C31 C -0.0219(10) 1.0959(10) 0.5831(5) 0.061(4) Uani 1 1 d . . . H31 H -0.0296 1.1599 0.5719 0.073 Uiso 1 1 calc R . . C32 C -0.0802(10) 1.0579(9) 0.6099(5) 0.062(4) Uani 1 1 d . . . H32 H -0.1301 1.0930 0.6156 0.074 Uiso 1 1 calc R . . C33 C -0.0653(9) 0.9633(9) 0.6296(5) 0.056(3) Uani 1 1 d . . . H33 H -0.1051 0.9358 0.6494 0.068 Uiso 1 1 calc R . . C34 C -0.2453(9) 0.7627(10) 0.5869(6) 0.080(4) Uani 1 1 d . . . H34A H -0.2757 0.8074 0.6066 0.120 Uiso 1 1 calc R . . H34B H -0.2905 0.7202 0.5634 0.120 Uiso 1 1 calc R . . H34C H -0.2142 0.7970 0.5624 0.120 Uiso 1 1 calc R . . C35 C -0.1394(9) 0.5757(9) 0.6102(5) 0.069(4) Uani 1 1 d . . . H35A H -0.1284 0.5858 0.5724 0.103 Uiso 1 1 calc R . . H35B H -0.1929 0.5356 0.6062 0.103 Uiso 1 1 calc R . . H35C H -0.0864 0.5450 0.6355 0.103 Uiso 1 1 calc R . . C36 C -0.2118(10) 0.6716(11) 0.7039(5) 0.080(4) Uani 1 1 d . . . H36A H -0.1750 0.6261 0.7304 0.120 Uiso 1 1 calc R . . H36B H -0.2736 0.6470 0.6893 0.120 Uiso 1 1 calc R . . H36C H -0.2140 0.7310 0.7239 0.120 Uiso 1 1 calc R . . C37 C -0.1446(9) 0.9332(11) 0.7736(5) 0.079(4) Uani 1 1 d . . . H37A H -0.1341 0.9424 0.7356 0.118 Uiso 1 1 calc R . . H37B H -0.1963 0.9717 0.7769 0.118 Uiso 1 1 calc R . . H37C H -0.1577 0.8668 0.7786 0.118 Uiso 1 1 calc R . . C38 C -0.0814(10) 0.9920(11) 0.8964(6) 0.095(5) Uani 1 1 d . . . H38A H -0.0743 0.9348 0.9198 0.142 Uiso 1 1 calc R . . H38B H -0.1457 1.0096 0.8847 0.142 Uiso 1 1 calc R . . H38C H -0.0462 1.0431 0.9189 0.142 Uiso 1 1 calc R . . C39 C -0.0021(11) 1.0863(11) 0.8077(7) 0.101(5) Uani 1 1 d . . . H39A H 0.0353 1.1195 0.8411 0.151 Uiso 1 1 calc R . . H39B H -0.0558 1.1242 0.7901 0.151 Uiso 1 1 calc R . . H39C H 0.0335 1.0759 0.7798 0.151 Uiso 1 1 calc R . . C40 C 0.2302(9) 0.9489(10) 0.8443(5) 0.080(4) Uani 1 1 d . . . H40A H 0.2215 0.9227 0.8057 0.120 Uiso 1 1 calc R . . H40B H 0.2929 0.9379 0.8665 0.120 Uiso 1 1 calc R . . H40C H 0.2181 1.0165 0.8416 0.120 Uiso 1 1 calc R . . C41 C 0.1997(9) 0.7682(9) 0.9007(6) 0.075(4) Uani 1 1 d . . . H41A H 0.1585 0.7316 0.9174 0.112 Uiso 1 1 calc R . . H41B H 0.2588 0.7740 0.9287 0.112 Uiso 1 1 calc R . . H41C H 0.2074 0.7364 0.8663 0.112 Uiso 1 1 calc R . . C42 C 0.1651(9) 0.9535(10) 0.9522(5) 0.081(4) Uani 1 1 d . . . H42A H 0.1441 1.0186 0.9453 0.122 Uiso 1 1 calc R . . H42B H 0.2295 0.9530 0.9731 0.122 Uiso 1 1 calc R . . H42C H 0.1295 0.9214 0.9750 0.122 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 Yb1 0.0515(3) 0.0474(3) 0.0339(2) 0.0015(3) 0.00177(19) 0.0036(4) N1 0.049(6) 0.047(6) 0.038(5) 0.004(5) 0.004(5) 0.001(5) N2 0.061(7) 0.057(7) 0.044(6) 0.006(5) 0.013(6) 0.009(6) N3 0.056(6) 0.052(6) 0.038(5) 0.000(6) -0.001(4) 0.003(6) N4 0.064(7) 0.066(8) 0.042(6) -0.015(5) 0.010(6) -0.001(6) P1 0.054(2) 0.049(2) 0.0367(17) 0.0100(15) 0.0059(16) 0.0082(16) P2 0.0477(19) 0.0474(18) 0.0326(16) -0.0002(13) 0.0008(15) 0.0007(14) Si1 0.064(2) 0.065(3) 0.039(2) 0.0087(17) 0.0140(18) 0.0043(19) Si2 0.055(2) 0.058(2) 0.0398(19) -0.0031(17) -0.0003(17) -0.0015(18) Si3 0.073(3) 0.062(3) 0.056(2) -0.0094(19) 0.009(2) 0.009(2) Si4 0.067(3) 0.063(2) 0.040(2) -0.0102(17) 0.0031(19) -0.0105(19) C1 0.054(8) 0.052(8) 0.038(7) 0.003(6) 0.008(6) 0.008(6) C2 0.056(9) 0.057(8) 0.041(7) 0.003(6) 0.004(7) 0.005(7) C3 0.055(8) 0.060(9) 0.043(7) 0.001(6) 0.003(6) 0.004(7) C4 0.053(9) 0.059(8) 0.040(7) 0.003(6) 0.007(6) 0.003(6) C5 0.051(8) 0.051(8) 0.036(7) -0.002(5) 0.006(6) 0.001(6) C6 0.056(8) 0.051(7) 0.037(7) 0.001(6) 0.000(6) 0.003(6) C7 0.062(10) 0.058(8) 0.047(8) 0.003(6) 0.006(7) 0.006(7) C8 0.064(9) 0.063(9) 0.050(8) 0.000(7) 0.004(7) 0.006(7) C9 0.070(11) 0.070(10) 0.059(9) -0.011(7) 0.009(8) 0.005(8) C10 0.072(11) 0.068(10) 0.063(9) -0.011(8) 0.003(8) 0.002(8) C11 0.069(10) 0.072(11) 0.066(10) -0.009(8) 0.004(8) -0.002(8) C12 0.067(10) 0.066(10) 0.056(9) -0.003(7) 0.008(8) 0.002(7) C13 0.065(9) 0.061(9) 0.044(8) 0.008(6) 0.008(7) 0.008(7) C14 0.069(9) 0.068(10) 0.048(8) 0.008(7) 0.004(7) 0.011(7) C15 0.076(11) 0.075(11) 0.049(8) 0.012(8) 0.006(8) 0.013(8) C16 0.080(11) 0.077(11) 0.055(9) 0.015(8) 0.003(9) 0.015(8) C17 0.085(11) 0.073(10) 0.060(9) 0.017(8) -0.004(9) 0.012(8) C18 0.075(10) 0.067(10) 0.054(9) 0.009(7) 0.001(8) 0.010(8) C19 0.106(13) 0.105(14) 0.078(11) 0.004(9) 0.030(10) -0.009(11) C20 0.096(12) 0.118(15) 0.066(10) -0.008(9) 0.017(9) 0.007(10) C21 0.099(13) 0.119(14) 0.081(11) 0.003(10) 0.032(10) 0.025(11) C22 0.059(8) 0.053(10) 0.041(7) -0.003(5) 0.004(6) 0.002(6) C23 0.065(8) 0.057(9) 0.042(6) -0.004(7) 0.003(6) 0.001(7) C24 0.073(10) 0.062(9) 0.042(8) -0.004(7) 0.002(7) 0.003(8) C25 0.077(10) 0.061(9) 0.044(8) -0.008(7) 0.005(8) 0.004(8) C26 0.080(10) 0.068(10) 0.057(9) -0.006(7) 0.001(8) 0.011(8) C27 0.065(9) 0.059(9) 0.045(8) -0.004(6) 0.000(7) 0.006(7) C28 0.058(9) 0.050(8) 0.038(7) 0.001(6) 0.005(6) 0.001(6) C29 0.062(9) 0.052(8) 0.042(7) 0.003(6) 0.001(7) -0.001(6) C30 0.068(10) 0.058(9) 0.050(8) 0.009(7) 0.002(7) -0.007(7) C31 0.067(10) 0.056(9) 0.052(8) 0.006(7) 0.001(7) 0.001(7) C32 0.070(10) 0.057(9) 0.052(8) 0.004(7) 0.006(7) 0.003(7) C33 0.063(9) 0.054(9) 0.048(8) 0.004(6) 0.007(7) 0.001(7) C34 0.073(9) 0.079(11) 0.074(9) -0.007(8) -0.008(7) 0.006(9) C35 0.070(10) 0.062(9) 0.064(9) -0.003(7) -0.001(8) -0.011(7) C36 0.078(10) 0.083(11) 0.075(10) -0.006(8) 0.013(9) -0.016(8) C37 0.084(11) 0.090(12) 0.058(9) -0.001(8) 0.011(8) 0.009(9) C38 0.092(12) 0.111(14) 0.076(11) -0.017(9) 0.013(9) 0.021(10) C39 0.098(13) 0.096(13) 0.094(12) -0.002(10) -0.001(10) 0.004(10) C40 0.085(11) 0.088(12) 0.060(9) -0.003(8) 0.007(8) -0.015(8) C41 0.070(8) 0.075(12) 0.068(9) -0.013(7) -0.003(7) -0.001(8) C42 0.081(11) 0.094(12) 0.057(9) -0.020(8) -0.002(8) 0.001(9) _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 Yb1 N4 2.338(10) . ? Yb1 N1 2.352(9) . ? Yb1 N3 2.446(8) . ? Yb1 N2 2.529(9) . ? Yb1 C5 3.119(12) . ? Yb1 C6 3.185(11) . ? Yb1 P2 3.263(3) . ? N1 C5 1.364(13) . ? N1 C1 1.368(13) . ? N2 P1 1.544(10) . ? N2 Si1 1.717(9) . ? N3 P2 1.549(9) . ? N3 Si2 1.711(10) . ? N4 Si3 1.668(11) . ? N4 Si4 1.674(11) . ? P1 C1 1.777(12) . ? P1 C13 1.810(12) . ? P1 C7 1.819(13) . ? P2 C6 1.741(12) . ? P2 C28 1.797(12) . ? P2 C22 1.808(11) . ? Si1 C20 1.812(14) . ? Si1 C19 1.821(15) . ? Si1 C21 1.841(15) . ? Si2 C35 1.844(12) . ? Si2 C34 1.854(13) . ? Si2 C36 1.857(12) . ? Si3 C38 1.846(13) . ? Si3 C39 1.847(16) . ? Si3 C37 1.864(14) . ? Si4 C40 1.841(13) . ? Si4 C41 1.867(13) . ? Si4 C42 1.870(12) . ? C1 C2 1.359(15) . ? C2 C3 1.371(15) . ? C2 H2 0.9300 . ? C3 C4 1.335(15) . ? C3 H3 0.9300 . ? C4 C5 1.404(15) . ? C4 H4 0.9300 . ? C5 C6 1.415(15) . ? C6 H6 0.9300 . ? C7 C12 1.336(16) . ? C7 C8 1.380(15) . ? C8 C9 1.402(17) . ? C8 H8 0.9300 . ? C9 C10 1.296(17) . ? C9 H9 0.9300 . ? C10 C11 1.318(16) . ? C10 H10 0.9300 . ? C11 C12 1.412(17) . ? C11 H11 0.9300 . ? C12 H12 0.9300 . ? C13 C14 1.358(17) . ? C13 C18 1.395(17) . ? C14 C15 1.385(16) . ? C14 H14 0.9300 . ? C15 C16 1.365(18) . ? C15 H15 0.9300 . ? C16 C17 1.334(18) . ? C16 H16 0.9300 . ? C17 C18 1.395(16) . ? C17 H17 0.9300 . ? C18 H18 0.9300 . ? C19 H19A 0.9600 . ? C19 H19B 0.9600 . ? C19 H19C 0.9600 . ? C20 H20A 0.9600 . ? C20 H20B 0.9600 . ? C20 H20C 0.9600 . ? C21 H21A 0.9600 . ? C21 H21B 0.9600 . ? C21 H21C 0.9600 . ? C22 C27 1.341(15) . ? C22 C23 1.361(15) . ? C23 C24 1.396(15) . ? C23 H23 0.9300 . ? C24 C25 1.324(16) . ? C24 H24 0.9300 . ? C25 C26 1.288(17) . ? C25 H25 0.9300 . ? C26 C27 1.419(16) . ? C26 H26 0.9300 . ? C27 H27 0.9300 . ? C28 C29 1.358(15) . ? C28 C33 1.371(15) . ? C29 C30 1.384(16) . ? C29 H29 0.9300 . ? C30 C31 1.346(16) . ? C30 H30 0.9300 . ? C31 C32 1.314(15) . ? C31 H31 0.9300 . ? C32 C33 1.398(16) . ? C32 H32 0.9300 . ? C33 H33 0.9300 . ? C34 H34A 0.9600 . ? C34 H34B 0.9600 . ? C34 H34C 0.9600 . ? C35 H35A 0.9600 . ? C35 H35B 0.9600 . ? C35 H35C 0.9600 . ? C36 H36A 0.9600 . ? C36 H36B 0.9600 . ? C36 H36C 0.9600 . ? C37 H37A 0.9600 . ? C37 H37B 0.9600 . ? C37 H37C 0.9600 . ? C38 H38A 0.9600 . ? C38 H38B 0.9600 . ? C38 H38C 0.9600 . ? C39 H39A 0.9600 . ? C39 H39B 0.9600 . ? C39 H39C 0.9600 . ? C40 H40A 0.9600 . ? C40 H40B 0.9600 . ? C40 H40C 0.9600 . ? C41 H41A 0.9600 . ? C41 H41B 0.9600 . ? C41 H41C 0.9600 . ? C42 H42A 0.9600 . ? C42 H42B 0.9600 . ? C42 H42C 0.9600 . ? 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 N4 Yb1 N1 115.2(3) . . ? N4 Yb1 N3 126.3(4) . . ? N1 Yb1 N3 83.3(3) . . ? N4 Yb1 N2 111.8(3) . . ? N1 Yb1 N2 73.8(3) . . ? N3 Yb1 N2 121.9(3) . . ? N4 Yb1 C5 101.2(3) . . ? N1 Yb1 C5 24.0(3) . . ? N3 Yb1 C5 75.4(3) . . ? N2 Yb1 C5 97.1(3) . . ? N4 Yb1 C6 96.0(3) . . ? N1 Yb1 C6 48.3(3) . . ? N3 Yb1 C6 58.0(3) . . ? N2 Yb1 C6 122.1(3) . . ? C5 Yb1 C6 25.9(3) . . ? N4 Yb1 P2 112.4(2) . . ? N1 Yb1 P2 66.9(2) . . ? N3 Yb1 P2 26.9(2) . . ? N2 Yb1 P2 130.0(2) . . ? C5 Yb1 P2 52.0(2) . . ? C6 Yb1 P2 31.3(2) . . ? C5 N1 C1 119.3(10) . . ? C5 N1 Yb1 111.3(7) . . ? C1 N1 Yb1 121.3(7) . . ? P1 N2 Si1 133.4(6) . . ? P1 N2 Yb1 112.1(5) . . ? Si1 N2 Yb1 114.0(5) . . ? P2 N3 Si2 133.9(5) . . ? P2 N3 Yb1 107.4(4) . . ? Si2 N3 Yb1 114.5(4) . . ? Si3 N4 Si4 125.8(6) . . ? Si3 N4 Yb1 113.7(5) . . ? Si4 N4 Yb1 120.1(5) . . ? N2 P1 C1 109.6(5) . . ? N2 P1 C13 116.0(5) . . ? C1 P1 C13 106.1(6) . . ? N2 P1 C7 113.7(6) . . ? C1 P1 C7 104.8(6) . . ? C13 P1 C7 105.7(6) . . ? N3 P2 C6 116.9(5) . . ? N3 P2 C28 110.6(6) . . ? C6 P2 C28 102.9(6) . . ? N3 P2 C22 113.3(5) . . ? C6 P2 C22 109.2(5) . . ? C28 P2 C22 102.5(5) . . ? N3 P2 Yb1 45.7(3) . . ? C6 P2 Yb1 71.9(4) . . ? C28 P2 Yb1 116.0(4) . . ? C22 P2 Yb1 140.5(4) . . ? N2 Si1 C20 113.7(6) . . ? N2 Si1 C19 113.3(6) . . ? C20 Si1 C19 108.4(7) . . ? N2 Si1 C21 109.2(6) . . ? C20 Si1 C21 103.7(7) . . ? C19 Si1 C21 107.9(8) . . ? N3 Si2 C35 114.5(5) . . ? N3 Si2 C34 111.3(6) . . ? C35 Si2 C34 109.8(6) . . ? N3 Si2 C36 105.4(5) . . ? C35 Si2 C36 109.3(6) . . ? C34 Si2 C36 106.2(6) . . ? N4 Si3 C38 114.5(6) . . ? N4 Si3 C39 114.1(6) . . ? C38 Si3 C39 107.2(7) . . ? N4 Si3 C37 109.3(6) . . ? C38 Si3 C37 104.4(6) . . ? C39 Si3 C37 106.5(7) . . ? N4 Si4 C40 113.6(6) . . ? N4 Si4 C41 111.3(6) . . ? C40 Si4 C41 105.0(6) . . ? N4 Si4 C42 115.6(6) . . ? C40 Si4 C42 105.8(6) . . ? C41 Si4 C42 104.7(6) . . ? C2 C1 N1 121.4(11) . . ? C2 C1 P1 127.5(10) . . ? N1 C1 P1 111.0(9) . . ? C1 C2 C3 119.5(12) . . ? C1 C2 H2 120.3 . . ? C3 C2 H2 120.3 . . ? C4 C3 C2 119.9(12) . . ? C4 C3 H3 120.1 . . ? C2 C3 H3 120.1 . . ? C3 C4 C5 121.1(12) . . ? C3 C4 H4 119.4 . . ? C5 C4 H4 119.4 . . ? N1 C5 C4 118.4(11) . . ? N1 C5 C6 118.4(11) . . ? C4 C5 C6 123.0(11) . . ? N1 C5 Yb1 44.6(5) . . ? C4 C5 Yb1 146.3(8) . . ? C6 C5 Yb1 79.7(7) . . ? C5 C6 P2 124.9(10) . . ? C5 C6 Yb1 74.4(6) . . ? P2 C6 Yb1 76.8(4) . . ? C5 C6 H6 117.5 . . ? P2 C6 H6 117.5 . . ? Yb1 C6 H6 122.5 . . ? C12 C7 C8 120.3(13) . . ? C12 C7 P1 120.8(10) . . ? C8 C7 P1 118.7(10) . . ? C7 C8 C9 119.0(13) . . ? C7 C8 H8 120.5 . . ? C9 C8 H8 120.5 . . ? C10 C9 C8 119.0(13) . . ? C10 C9 H9 120.5 . . ? C8 C9 H9 120.5 . . ? C9 C10 C11 123.6(15) . . ? C9 C10 H10 118.2 . . ? C11 C10 H10 118.2 . . ? C10 C11 C12 119.6(14) . . ? C10 C11 H11 120.2 . . ? C12 C11 H11 120.2 . . ? C7 C12 C11 118.5(13) . . ? C7 C12 H12 120.8 . . ? C11 C12 H12 120.8 . . ? C14 C13 C18 119.7(12) . . ? C14 C13 P1 117.8(11) . . ? C18 C13 P1 122.5(10) . . ? C13 C14 C15 121.5(14) . . ? C13 C14 H14 119.2 . . ? C15 C14 H14 119.2 . . ? C16 C15 C14 117.9(14) . . ? C16 C15 H15 121.1 . . ? C14 C15 H15 121.1 . . ? C17 C16 C15 122.0(14) . . ? C17 C16 H16 119.0 . . ? C15 C16 H16 119.0 . . ? C16 C17 C18 120.8(15) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C13 C18 C17 118.0(14) . . ? C13 C18 H18 121.0 . . ? C17 C18 H18 121.0 . . ? Si1 C19 H19A 109.5 . . ? Si1 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? Si1 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? Si1 C20 H20A 109.5 . . ? Si1 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? Si1 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? Si1 C21 H21A 109.5 . . ? Si1 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? Si1 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C27 C22 C23 117.8(11) . . ? C27 C22 P2 121.0(10) . . ? C23 C22 P2 121.2(9) . . ? C22 C23 C24 122.7(12) . . ? C22 C23 H23 118.6 . . ? C24 C23 H23 118.6 . . ? C25 C24 C23 118.2(13) . . ? C25 C24 H24 120.9 . . ? C23 C24 H24 120.9 . . ? C26 C25 C24 119.8(13) . . ? C26 C25 H25 120.1 . . ? C24 C25 H25 120.1 . . ? C25 C26 C27 124.0(14) . . ? C25 C26 H26 118.0 . . ? C27 C26 H26 118.0 . . ? C22 C27 C26 117.3(12) . . ? C22 C27 H27 121.3 . . ? C26 C27 H27 121.3 . . ? C29 C28 C33 117.4(12) . . ? C29 C28 P2 123.4(10) . . ? C33 C28 P2 119.2(9) . . ? C28 C29 C30 121.4(12) . . ? C28 C29 H29 119.3 . . ? C30 C29 H29 119.3 . . ? C31 C30 C29 118.5(12) . . ? C31 C30 H30 120.7 . . ? C29 C30 H30 120.7 . . ? C32 C31 C30 122.9(13) . . ? C32 C31 H31 118.5 . . ? C30 C31 H31 118.5 . . ? C31 C32 C33 118.3(13) . . ? C31 C32 H32 120.9 . . ? C33 C32 H32 120.9 . . ? C28 C33 C32 121.4(12) . . ? C28 C33 H33 119.3 . . ? C32 C33 H33 119.3 . . ? Si2 C34 H34A 109.5 . . ? Si2 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si2 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si2 C35 H35A 109.5 . . ? Si2 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si2 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? Si2 C36 H36A 109.5 . . ? Si2 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? Si2 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? Si3 C37 H37A 109.5 . . ? Si3 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si3 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si3 C38 H38A 109.5 . . ? Si3 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si3 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? Si3 C39 H39A 109.5 . . ? Si3 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? Si3 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? Si4 C40 H40A 109.5 . . ? Si4 C40 H40B 109.5 . . ? H40A C40 H40B 109.5 . . ? Si4 C40 H40C 109.5 . . ? H40A C40 H40C 109.5 . . ? H40B C40 H40C 109.5 . . ? Si4 C41 H41A 109.5 . . ? Si4 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? Si4 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? Si4 C42 H42A 109.5 . . ? Si4 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? Si4 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag N4 Yb1 N1 C5 -58.1(8) . . . . ? N3 Yb1 N1 C5 69.0(7) . . . . ? N2 Yb1 N1 C5 -165.0(8) . . . . ? C6 Yb1 N1 C5 16.6(6) . . . . ? P2 Yb1 N1 C5 46.8(7) . . . . ? N4 Yb1 N1 C1 90.4(9) . . . . ? N3 Yb1 N1 C1 -142.5(9) . . . . ? N2 Yb1 N1 C1 -16.5(9) . . . . ? C5 Yb1 N1 C1 148.5(13) . . . . ? C6 Yb1 N1 C1 165.1(11) . . . . ? P2 Yb1 N1 C1 -164.7(9) . . . . ? N4 Yb1 N2 P1 -119.7(5) . . . . ? N1 Yb1 N2 P1 -8.5(5) . . . . ? N3 Yb1 N2 P1 62.6(6) . . . . ? C5 Yb1 N2 P1 -14.6(6) . . . . ? C6 Yb1 N2 P1 -7.1(7) . . . . ? P2 Yb1 N2 P1 30.7(7) . . . . ? N4 Yb1 N2 Si1 53.3(6) . . . . ? N1 Yb1 N2 Si1 164.5(6) . . . . ? N3 Yb1 N2 Si1 -124.4(5) . . . . ? C5 Yb1 N2 Si1 158.4(5) . . . . ? C6 Yb1 N2 Si1 165.9(4) . . . . ? P2 Yb1 N2 Si1 -156.4(3) . . . . ? N4 Yb1 N3 P2 66.2(6) . . . . ? N1 Yb1 N3 P2 -50.2(5) . . . . ? N2 Yb1 N3 P2 -116.4(5) . . . . ? C5 Yb1 N3 P2 -27.1(5) . . . . ? C6 Yb1 N3 P2 -6.0(4) . . . . ? N4 Yb1 N3 Si2 -133.7(5) . . . . ? N1 Yb1 N3 Si2 109.9(5) . . . . ? N2 Yb1 N3 Si2 43.7(6) . . . . ? C5 Yb1 N3 Si2 133.0(6) . . . . ? C6 Yb1 N3 Si2 154.1(7) . . . . ? P2 Yb1 N3 Si2 160.1(9) . . . . ? N1 Yb1 N4 Si3 156.7(4) . . . . ? N3 Yb1 N4 Si3 56.0(6) . . . . ? N2 Yb1 N4 Si3 -121.6(5) . . . . ? C5 Yb1 N4 Si3 136.0(5) . . . . ? C6 Yb1 N4 Si3 110.3(5) . . . . ? P2 Yb1 N4 Si3 82.6(5) . . . . ? N1 Yb1 N4 Si4 -16.9(7) . . . . ? N3 Yb1 N4 Si4 -117.6(6) . . . . ? N2 Yb1 N4 Si4 64.8(6) . . . . ? C5 Yb1 N4 Si4 -37.6(6) . . . . ? C6 Yb1 N4 Si4 -63.3(6) . . . . ? P2 Yb1 N4 Si4 -91.0(5) . . . . ? Si1 N2 P1 C1 -145.9(8) . . . . ? Yb1 N2 P1 C1 25.2(7) . . . . ? Si1 N2 P1 C13 -25.8(12) . . . . ? Yb1 N2 P1 C13 145.4(6) . . . . ? Si1 N2 P1 C7 97.2(9) . . . . ? Yb1 N2 P1 C7 -91.7(6) . . . . ? Si2 N3 P2 C6 -144.1(8) . . . . ? Yb1 N3 P2 C6 10.5(7) . . . . ? Si2 N3 P2 C28 98.7(9) . . . . ? Yb1 N3 P2 C28 -106.7(5) . . . . ? Si2 N3 P2 C22 -15.7(11) . . . . ? Yb1 N3 P2 C22 138.9(5) . . . . ? Si2 N3 P2 Yb1 -154.6(12) . . . . ? N4 Yb1 P2 N3 -127.1(6) . . . . ? N1 Yb1 P2 N3 123.9(6) . . . . ? N2 Yb1 P2 N3 82.7(6) . . . . ? C5 Yb1 P2 N3 146.0(6) . . . . ? C6 Yb1 P2 N3 170.1(7) . . . . ? N4 Yb1 P2 C6 62.8(5) . . . . ? N1 Yb1 P2 C6 -46.2(5) . . . . ? N3 Yb1 P2 C6 -170.1(7) . . . . ? N2 Yb1 P2 C6 -87.4(5) . . . . ? C5 Yb1 P2 C6 -24.1(5) . . . . ? N4 Yb1 P2 C28 -33.1(6) . . . . ? N1 Yb1 P2 C28 -142.1(5) . . . . ? N3 Yb1 P2 C28 94.0(7) . . . . ? N2 Yb1 P2 C28 176.7(5) . . . . ? C5 Yb1 P2 C28 -120.0(5) . . . . ? C6 Yb1 P2 C28 -95.9(6) . . . . ? N4 Yb1 P2 C22 161.3(7) . . . . ? N1 Yb1 P2 C22 52.3(7) . . . . ? N3 Yb1 P2 C22 -71.6(8) . . . . ? N2 Yb1 P2 C22 11.1(8) . . . . ? C5 Yb1 P2 C22 74.4(7) . . . . ? C6 Yb1 P2 C22 98.5(8) . . . . ? P1 N2 Si1 C20 81.1(11) . . . . ? Yb1 N2 Si1 C20 -89.9(7) . . . . ? P1 N2 Si1 C19 -43.3(11) . . . . ? Yb1 N2 Si1 C19 145.7(6) . . . . ? P1 N2 Si1 C21 -163.6(9) . . . . ? Yb1 N2 Si1 C21 25.4(8) . . . . ? P2 N3 Si2 C35 50.9(11) . . . . ? Yb1 N3 Si2 C35 -102.4(6) . . . . ? P2 N3 Si2 C34 -74.3(10) . . . . ? Yb1 N3 Si2 C34 132.5(6) . . . . ? P2 N3 Si2 C36 171.1(9) . . . . ? Yb1 N3 Si2 C36 17.8(7) . . . . ? Si4 N4 Si3 C38 -69.7(10) . . . . ? Yb1 N4 Si3 C38 117.1(7) . . . . ? Si4 N4 Si3 C39 54.4(9) . . . . ? Yb1 N4 Si3 C39 -118.8(7) . . . . ? Si4 N4 Si3 C37 173.5(7) . . . . ? Yb1 N4 Si3 C37 0.3(7) . . . . ? Si3 N4 Si4 C40 -84.2(8) . . . . ? Yb1 N4 Si4 C40 88.5(7) . . . . ? Si3 N4 Si4 C41 157.6(7) . . . . ? Yb1 N4 Si4 C41 -29.6(7) . . . . ? Si3 N4 Si4 C42 38.4(10) . . . . ? Yb1 N4 Si4 C42 -148.8(6) . . . . ? C5 N1 C1 C2 2.0(16) . . . . ? Yb1 N1 C1 C2 -144.0(9) . . . . ? C5 N1 C1 P1 -179.6(7) . . . . ? Yb1 N1 C1 P1 34.4(11) . . . . ? N2 P1 C1 C2 139.6(11) . . . . ? C13 P1 C1 C2 13.6(13) . . . . ? C7 P1 C1 C2 -98.0(12) . . . . ? N2 P1 C1 N1 -38.7(10) . . . . ? C13 P1 C1 N1 -164.7(8) . . . . ? C7 P1 C1 N1 83.7(9) . . . . ? N1 C1 C2 C3 2.4(17) . . . . ? P1 C1 C2 C3 -175.7(9) . . . . ? C1 C2 C3 C4 -2.2(17) . . . . ? C2 C3 C4 C5 -2.2(18) . . . . ? C1 N1 C5 C4 -6.3(15) . . . . ? Yb1 N1 C5 C4 142.9(9) . . . . ? C1 N1 C5 C6 177.8(10) . . . . ? Yb1 N1 C5 C6 -33.0(12) . . . . ? C1 N1 C5 Yb1 -149.2(12) . . . . ? C3 C4 C5 N1 6.5(17) . . . . ? C3 C4 C5 C6 -177.8(11) . . . . ? C3 C4 C5 Yb1 56(2) . . . . ? N4 Yb1 C5 N1 128.5(7) . . . . ? N3 Yb1 C5 N1 -106.6(8) . . . . ? N2 Yb1 C5 N1 14.5(8) . . . . ? C6 Yb1 C5 N1 -150.9(11) . . . . ? P2 Yb1 C5 N1 -121.8(8) . . . . ? N4 Yb1 C5 C4 55.7(16) . . . . ? N1 Yb1 C5 C4 -72.7(16) . . . . ? N3 Yb1 C5 C4 -179.4(16) . . . . ? N2 Yb1 C5 C4 -58.2(16) . . . . ? C6 Yb1 C5 C4 136.4(19) . . . . ? P2 Yb1 C5 C4 165.4(17) . . . . ? N4 Yb1 C5 C6 -80.7(7) . . . . ? N1 Yb1 C5 C6 150.9(11) . . . . ? N3 Yb1 C5 C6 44.2(7) . . . . ? N2 Yb1 C5 C6 165.4(7) . . . . ? P2 Yb1 C5 C6 29.1(6) . . . . ? N1 C5 C6 P2 -38.2(14) . . . . ? C4 C5 C6 P2 146.1(10) . . . . ? Yb1 C5 C6 P2 -61.1(8) . . . . ? N1 C5 C6 Yb1 22.9(8) . . . . ? C4 C5 C6 Yb1 -152.8(11) . . . . ? N3 P2 C6 C5 52.1(11) . . . . ? C28 P2 C6 C5 173.4(9) . . . . ? C22 P2 C6 C5 -78.2(10) . . . . ? Yb1 P2 C6 C5 60.0(9) . . . . ? N3 P2 C6 Yb1 -7.9(5) . . . . ? C28 P2 C6 Yb1 113.4(4) . . . . ? C22 P2 C6 Yb1 -138.2(4) . . . . ? N4 Yb1 C6 C5 103.3(7) . . . . ? N1 Yb1 C6 C5 -15.4(6) . . . . ? N3 Yb1 C6 C5 -127.3(8) . . . . ? N2 Yb1 C6 C5 -17.2(8) . . . . ? P2 Yb1 C6 C5 -132.5(9) . . . . ? N4 Yb1 C6 P2 -124.2(4) . . . . ? N1 Yb1 C6 P2 117.1(6) . . . . ? N3 Yb1 C6 P2 5.3(4) . . . . ? N2 Yb1 C6 P2 115.4(4) . . . . ? C5 Yb1 C6 P2 132.5(9) . . . . ? N2 P1 C7 C12 -31.1(13) . . . . ? C1 P1 C7 C12 -150.8(11) . . . . ? C13 P1 C7 C12 97.3(11) . . . . ? N2 P1 C7 C8 152.5(9) . . . . ? C1 P1 C7 C8 32.8(11) . . . . ? C13 P1 C7 C8 -79.1(11) . . . . ? C12 C7 C8 C9 1.5(19) . . . . ? P1 C7 C8 C9 177.8(10) . . . . ? C7 C8 C9 C10 -2(2) . . . . ? C8 C9 C10 C11 0(2) . . . . ? C9 C10 C11 C12 3(2) . . . . ? C8 C7 C12 C11 1.0(19) . . . . ? P1 C7 C12 C11 -175.4(10) . . . . ? C10 C11 C12 C7 -3(2) . . . . ? N2 P1 C13 C14 -60.4(12) . . . . ? C1 P1 C13 C14 61.6(11) . . . . ? C7 P1 C13 C14 172.5(10) . . . . ? N2 P1 C13 C18 121.7(11) . . . . ? C1 P1 C13 C18 -116.3(11) . . . . ? C7 P1 C13 C18 -5.4(12) . . . . ? C18 C13 C14 C15 -1.9(19) . . . . ? P1 C13 C14 C15 -179.9(9) . . . . ? C13 C14 C15 C16 2.8(19) . . . . ? C14 C15 C16 C17 -4(2) . . . . ? C15 C16 C17 C18 4(2) . . . . ? C14 C13 C18 C17 1.8(19) . . . . ? P1 C13 C18 C17 179.7(9) . . . . ? C16 C17 C18 C13 -3(2) . . . . ? N3 P2 C22 C27 -108.5(11) . . . . ? C6 P2 C22 C27 23.7(12) . . . . ? C28 P2 C22 C27 132.4(11) . . . . ? Yb1 P2 C22 C27 -60.9(13) . . . . ? N3 P2 C22 C23 69.2(11) . . . . ? C6 P2 C22 C23 -158.6(10) . . . . ? C28 P2 C22 C23 -50.0(11) . . . . ? Yb1 P2 C22 C23 116.8(9) . . . . ? C27 C22 C23 C24 2.7(18) . . . . ? P2 C22 C23 C24 -175.1(10) . . . . ? C22 C23 C24 C25 -3.7(19) . . . . ? C23 C24 C25 C26 3(2) . . . . ? C24 C25 C26 C27 -2(2) . . . . ? C23 C22 C27 C26 -1.4(18) . . . . ? P2 C22 C27 C26 176.4(9) . . . . ? C25 C26 C27 C22 1(2) . . . . ? N3 P2 C28 C29 -171.2(9) . . . . ? C6 P2 C28 C29 63.2(11) . . . . ? C22 P2 C28 C29 -50.2(11) . . . . ? Yb1 P2 C28 C29 139.1(9) . . . . ? N3 P2 C28 C33 7.4(11) . . . . ? C6 P2 C28 C33 -118.2(10) . . . . ? C22 P2 C28 C33 128.4(10) . . . . ? Yb1 P2 C28 C33 -42.3(11) . . . . ? C33 C28 C29 C30 1.6(17) . . . . ? P2 C28 C29 C30 -179.7(9) . . . . ? C28 C29 C30 C31 0.3(18) . . . . ? C29 C30 C31 C32 -3.0(19) . . . . ? C30 C31 C32 C33 3.5(19) . . . . ? C29 C28 C33 C32 -1.1(18) . . . . ? P2 C28 C33 C32 -179.8(9) . . . . ? C31 C32 C33 C28 -1.4(18) . . . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 25.01 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 3.544 _refine_diff_density_min -1.386 _refine_diff_density_rms 0.155 #====END