# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2000 # CCDC Number: 186/2121 data_GERHUS-HITCHCOCK-LAPPERT-9 _audit_creation_method SHELXL _chemical_name_systematic ; ? ; _chemical_name_common '[C6H4((NCH2tBu)2GeC(NCH2tBu)2C6H4]' _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C33 H52 Ge N4' _chemical_formula_weight 577.38 _chemical_melting_point ? _chemical_compound_source ? 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' 'Ge' 'Ge' 0.1547 1.8001 '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' _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 10.146(2) _cell_length_b 16.243(9) _cell_length_c 20.054(4) _cell_angle_alpha 90.00 _cell_angle_beta 101.85(2) _cell_angle_gamma 90.00 _cell_volume 3234.5(20) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.4 _exptl_crystal_size_mid 0.4 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.186 _exptl_crystal_density_method ? _exptl_crystal_F_000 1240 _exptl_absorpt_coefficient_mu 0.973 _exptl_absorpt_correction_type 'psi-scans' _exptl_absorpt_correction_T_min 0.94 _exptl_absorpt_correction_T_max 1.00 _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'Enraf-Nonius CAD4' _diffrn_measurement_method 'omega-2theta scan' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 6018 _diffrn_reflns_av_R_equivalents 0.0359 _diffrn_reflns_av_sigmaI/netI 0.0604 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.08 _diffrn_reflns_theta_max 25.01 _reflns_number_total 5683 _reflns_number_observed 4370 _reflns_observed_criterion >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; The C24 neopentyl group is disordered 0.55:0.44 over two orientations sharing common C27 and C28 sites. Refinement on F^2^ for ALL reflections except for 2 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0349P)^2^+2.0968P] 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 ? _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.0010(2) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5681 _refine_ls_number_parameters 372 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0653 _refine_ls_R_factor_obs 0.0424 _refine_ls_wR_factor_all 0.1036 _refine_ls_wR_factor_obs 0.0918 _refine_ls_goodness_of_fit_all 1.055 _refine_ls_goodness_of_fit_obs 1.081 _refine_ls_restrained_S_all 1.059 _refine_ls_restrained_S_obs 1.081 _refine_ls_shift/esd_max -0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Ge Ge 0.60668(3) 0.43238(2) 0.76070(2) 0.02287(11) Uani 1 d . . N2 N 0.8857(2) 0.44863(14) 0.71405(12) 0.0211(5) Uani 1 d . . N1 N 0.9280(2) 0.3751(2) 0.80608(12) 0.0225(6) Uani 1 d . . N3 N 0.6179(2) 0.4295(2) 0.85670(12) 0.0249(5) Uani 1 d . . N4 N 0.5289(2) 0.32684(15) 0.76180(12) 0.0224(6) Uani 1 d . . C1 C 0.8273(3) 0.3981(2) 0.75372(15) 0.0224(6) Uani 1 d . . C2 C 1.0218(3) 0.4609(2) 0.74277(15) 0.0229(7) Uani 1 d . . C3 C 1.0495(3) 0.4132(2) 0.8013(2) 0.0234(7) Uani 1 d . . C4 C 1.1757(3) 0.4129(2) 0.8441(2) 0.0290(7) Uani 1 d . . H4 H 1.1946(3) 0.3797(2) 0.8839(2) 0.035 Uiso 1 calc R . C5 C 1.2724(3) 0.4631(2) 0.8261(2) 0.0348(8) Uani 1 d . . H5 H 1.3597(3) 0.4650(2) 0.8545(2) 0.042 Uiso 1 calc R . C6 C 1.2451(3) 0.5110(2) 0.7674(2) 0.0345(8) Uani 1 d . . H6 H 1.3143(3) 0.5448(2) 0.7566(2) 0.041 Uiso 1 calc R . C7 C 1.1206(3) 0.5107(2) 0.7243(2) 0.0278(7) Uani 1 d . . H7 H 1.1027(3) 0.5429(2) 0.6840(2) 0.033 Uiso 1 calc R . C8 C 0.9103(3) 0.3211(2) 0.8625(2) 0.0263(7) Uani 1 d . . H8B H 0.8174(3) 0.3283(2) 0.8698(2) 0.032 Uiso 1 calc R . H8A H 0.9726(3) 0.3397(2) 0.9045(2) 0.032 Uiso 1 calc R . C9 C 0.9344(3) 0.2291(2) 0.8529(2) 0.0292(7) Uani 1 d . . C10 C 0.9107(4) 0.1868(2) 0.9173(2) 0.0521(11) Uani 1 d . . H10C H 0.9745(4) 0.2083(2) 0.9569(2) 0.078 Uiso 1 calc R . H10B H 0.9239(4) 0.1274(2) 0.9137(2) 0.078 Uiso 1 calc R . H10A H 0.8184(4) 0.1976(2) 0.9227(2) 0.078 Uiso 1 calc R . C11 C 1.0792(4) 0.2119(2) 0.8455(2) 0.0508(11) Uani 1 d . . H11C H 1.0956(4) 0.2387(2) 0.8042(2) 0.076 Uiso 1 calc R . H11B H 1.0923(4) 0.1523(2) 0.8422(2) 0.076 Uiso 1 calc R . H11A H 1.1422(4) 0.2335(2) 0.8853(2) 0.076 Uiso 1 calc R . C12 C 0.8350(4) 0.1957(2) 0.7912(2) 0.0510(10) Uani 1 d . . H12C H 0.8502(4) 0.2230(2) 0.7498(2) 0.077 Uiso 1 calc R . H12B H 0.7427(4) 0.2066(2) 0.7966(2) 0.077 Uiso 1 calc R . H12A H 0.8481(4) 0.1363(2) 0.7875(2) 0.077 Uiso 1 calc R . C13 C 0.8150(3) 0.4866(2) 0.65064(15) 0.0259(7) Uani 1 d . . H13B H 0.8532(3) 0.5421(2) 0.64719(15) 0.031 Uiso 1 calc R . H13A H 0.7193(3) 0.4937(2) 0.65325(15) 0.031 Uiso 1 calc R . C14 C 0.8209(3) 0.4390(2) 0.58542(15) 0.0273(7) Uani 1 d . . C15 C 0.7388(4) 0.4876(3) 0.5263(2) 0.0477(10) Uani 1 d . . H15C H 0.7775(4) 0.5427(3) 0.5252(2) 0.072 Uiso 1 calc R . H15B H 0.6455(4) 0.4922(3) 0.5321(2) 0.072 Uiso 1 calc R . H15A H 0.7405(4) 0.4591(3) 0.4834(2) 0.072 Uiso 1 calc R . C16 C 0.7616(4) 0.3533(2) 0.5873(2) 0.0462(10) Uani 1 d . . H16C H 0.8147(4) 0.3222(2) 0.6254(2) 0.069 Uiso 1 calc R . H16B H 0.7635(4) 0.3247(2) 0.5444(2) 0.069 Uiso 1 calc R . H16A H 0.6683(4) 0.3577(2) 0.5931(2) 0.069 Uiso 1 calc R . C17 C 0.9656(3) 0.4315(2) 0.5751(2) 0.0402(8) Uani 1 d . . H17C H 1.0043(3) 0.4866(2) 0.5738(2) 0.060 Uiso 1 calc R . H17B H 0.9659(3) 0.4030(2) 0.5321(2) 0.060 Uiso 1 calc R . H17A H 1.0193(3) 0.4002(2) 0.6129(2) 0.060 Uiso 1 calc R . C18 C 0.5718(3) 0.3557(2) 0.87942(15) 0.0237(7) Uani 1 d . . C19 C 0.5213(3) 0.2989(2) 0.82621(14) 0.0228(6) Uani 1 d . . C20 C 0.4700(3) 0.2244(2) 0.8426(2) 0.0333(8) Uani 1 d . . H20 H 0.4361(3) 0.1862(2) 0.8074(2) 0.040 Uiso 1 calc R . C21 C 0.4670(3) 0.2044(2) 0.9098(2) 0.0370(8) Uani 1 d . . H21 H 0.4310(3) 0.1531(2) 0.9200(2) 0.044 Uiso 1 calc R . C22 C 0.5159(3) 0.2586(2) 0.9613(2) 0.0398(9) Uani 1 d . . H22 H 0.5140(3) 0.2448(2) 1.0071(2) 0.048 Uiso 1 calc R . C23 C 0.5688(3) 0.3345(2) 0.9462(2) 0.0350(8) Uani 1 d . . H23 H 0.6031(3) 0.3718(2) 0.9821(2) 0.042 Uiso 1 calc R . C29 C 0.5026(3) 0.2721(2) 0.70323(14) 0.0230(6) Uani 1 d . . H29B H 0.5121(3) 0.2147(2) 0.72017(14) 0.028 Uiso 1 calc R . H29A H 0.5733(3) 0.2813(2) 0.67660(14) 0.028 Uiso 1 calc R . C30 C 0.3644(3) 0.2802(2) 0.65441(15) 0.0267(7) Uani 1 d . . C31 C 0.3497(3) 0.3648(2) 0.6205(2) 0.0371(8) Uani 1 d . . H31C H 0.3540(3) 0.4075(2) 0.6554(2) 0.056 Uiso 1 calc R . H31B H 0.2629(3) 0.3681(2) 0.5884(2) 0.056 Uiso 1 calc R . H31A H 0.4228(3) 0.3731(2) 0.5960(2) 0.056 Uiso 1 calc R . C32 C 0.3577(4) 0.2130(3) 0.6002(2) 0.0488(10) Uani 1 d . . H32C H 0.3671(4) 0.1589(3) 0.6222(2) 0.073 Uiso 1 calc R . H32B H 0.4308(4) 0.2212(3) 0.5756(2) 0.073 Uiso 1 calc R . H32A H 0.2709(4) 0.2161(3) 0.5680(2) 0.073 Uiso 1 calc R . C33 C 0.2489(3) 0.2678(2) 0.6923(2) 0.0361(8) Uani 1 d . . H33C H 0.2575(3) 0.2136(2) 0.7142(2) 0.054 Uiso 1 calc R . H33B H 0.1625(3) 0.2712(2) 0.6598(2) 0.054 Uiso 1 calc R . H33A H 0.2529(3) 0.3107(2) 0.7270(2) 0.054 Uiso 1 calc R . C24 C 0.6776(8) 0.4806(4) 0.9166(4) 0.031(2) Uani 0.551(6) d P 1 H24A H 0.7623(8) 0.4544(4) 0.9405(4) 0.037 Uiso 0.551(6) calc PR 1 H24B H 0.6149(8) 0.4813(4) 0.9485(4) 0.037 Uiso 0.551(6) calc PR 1 C25 C 0.7077(8) 0.5687(5) 0.8998(4) 0.031(2) Uani 0.551(6) d P 1 C26 C 0.5815(6) 0.6146(4) 0.8649(3) 0.035(2) Uani 0.551(6) d P 1 H26A H 0.5429(6) 0.5876(4) 0.8216(3) 0.052 Uiso 0.551(6) calc PR 1 H26B H 0.6047(6) 0.6716(4) 0.8563(3) 0.052 Uiso 0.551(6) calc PR 1 H26C H 0.5155(6) 0.6140(4) 0.8944(3) 0.052 Uiso 0.551(6) calc PR 1 C27 C 0.8320(4) 0.5677(3) 0.8642(2) 0.0649(14) Uani 0.551(6) d P 1 H27A H 0.8096(4) 0.5357(3) 0.8219(2) 0.097 Uiso 0.551(6) calc PR 1 H27B H 0.9093(4) 0.5425(3) 0.8948(2) 0.097 Uiso 0.551(6) calc PR 1 H27C H 0.8547(4) 0.6242(3) 0.8536(2) 0.097 Uiso 0.551(6) calc PR 1 C28 C 0.7514(5) 0.6185(3) 0.9635(2) 0.0565(12) Uani 0.551(6) d P 1 H28A H 0.7724(5) 0.6748(3) 0.9515(2) 0.085 Uiso 0.551(6) calc PR 1 H28B H 0.8318(5) 0.5935(3) 0.9918(2) 0.085 Uiso 0.551(6) calc PR 1 H28C H 0.6788(5) 0.6198(3) 0.9890(2) 0.085 Uiso 0.551(6) calc PR 1 C24A C 0.6246(8) 0.5123(5) 0.8901(4) 0.026(2) Uani 0.449(6) d P 2 H24D H 0.5655(8) 0.5104(5) 0.9237(4) 0.031 Uiso 0.449(6) calc PR 2 H24C H 0.5844(8) 0.5526(5) 0.8547(4) 0.031 Uiso 0.449(6) calc PR 2 C25A C 0.7597(9) 0.5464(5) 0.9263(5) 0.027(2) Uani 0.449(6) d P 2 C26A C 0.8268(7) 0.4876(5) 0.9838(4) 0.038(2) Uani 0.449(6) d P 2 H26F H 0.8399(7) 0.4335(5) 0.9644(4) 0.056 Uiso 0.449(6) calc PR 2 H26E H 0.7690(7) 0.4818(5) 1.0171(4) 0.056 Uiso 0.449(6) calc PR 2 H26D H 0.9143(7) 0.5100(5) 1.0064(4) 0.056 Uiso 0.449(6) calc PR 2 C27A C 0.8320(4) 0.5677(3) 0.8642(2) 0.0649(14) Uani 0.449(6) d P 2 H27F H 0.8399(5459) 0.5175(5459) 0.8382(36) 0.097 Uiso 0.449(6) calc PR 2 H27E H 0.9220(5459) 0.5900(5459) 0.8821(36) 0.097 Uiso 0.449(6) calc PR 2 H27D H 0.7783(5459) 0.6085(5459) 0.8343(36) 0.097 Uiso 0.449(6) calc PR 2 C28A C 0.7514(5) 0.6185(3) 0.9635(2) 0.0565(12) Uani 0.449(6) d P 2 H28F H 0.7098(5459) 0.6622(5459) 0.9326(36) 0.085 Uiso 0.449(6) calc PR 2 H28E H 0.8421(5459) 0.6356(5459) 0.9864(36) 0.085 Uiso 0.449(6) calc PR 2 H28D H 0.6967(5459) 0.6082(5459) 0.9977(36) 0.085 Uiso 0.449(6) calc PR 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge 0.0192(2) 0.0205(2) 0.0279(2) 0.00255(15) 0.00258(12) -0.00144(14) N2 0.0208(12) 0.0211(13) 0.0223(12) 0.0011(10) 0.0070(10) 0.0024(10) N1 0.0201(13) 0.0243(13) 0.0237(13) 0.0022(11) 0.0059(11) 0.0003(11) N3 0.0215(13) 0.0250(13) 0.0278(13) -0.0082(12) 0.0036(10) -0.0036(12) N4 0.0228(13) 0.0223(13) 0.0213(13) 0.0018(11) 0.0030(10) -0.0038(10) C1 0.024(2) 0.0197(15) 0.024(2) 0.0024(13) 0.0073(13) 0.0017(13) C2 0.023(2) 0.0209(15) 0.026(2) -0.0031(13) 0.0071(13) -0.0008(12) C3 0.0203(15) 0.024(2) 0.028(2) -0.0031(13) 0.0080(12) -0.0005(12) C4 0.022(2) 0.031(2) 0.033(2) -0.0006(14) 0.0043(13) 0.0012(13) C5 0.021(2) 0.039(2) 0.044(2) -0.006(2) 0.0053(15) -0.0044(15) C6 0.026(2) 0.030(2) 0.050(2) -0.007(2) 0.015(2) -0.0058(15) C7 0.029(2) 0.023(2) 0.034(2) -0.0003(14) 0.0144(14) -0.0007(13) C8 0.018(2) 0.034(2) 0.027(2) 0.0063(14) 0.0052(13) 0.0004(13) C9 0.023(2) 0.028(2) 0.037(2) 0.0104(15) 0.0060(14) 0.0040(13) C10 0.059(3) 0.045(2) 0.055(3) 0.023(2) 0.017(2) 0.000(2) C11 0.042(2) 0.032(2) 0.085(3) 0.010(2) 0.029(2) 0.009(2) C12 0.060(3) 0.032(2) 0.052(2) 0.000(2) -0.008(2) 0.001(2) C13 0.029(2) 0.024(2) 0.026(2) 0.0041(13) 0.0089(13) 0.0074(13) C14 0.033(2) 0.028(2) 0.0214(15) 0.0021(14) 0.0065(13) 0.0059(14) C15 0.065(3) 0.054(2) 0.023(2) 0.002(2) 0.006(2) 0.020(2) C16 0.063(3) 0.042(2) 0.036(2) -0.009(2) 0.015(2) -0.012(2) C17 0.041(2) 0.050(2) 0.034(2) -0.012(2) 0.017(2) 0.005(2) C18 0.0153(15) 0.029(2) 0.026(2) -0.0012(13) 0.0021(12) 0.0020(13) C19 0.024(2) 0.022(2) 0.022(2) 0.0018(13) 0.0038(12) 0.0033(13) C20 0.042(2) 0.028(2) 0.029(2) 0.0028(15) 0.0049(15) -0.003(2) C21 0.039(2) 0.040(2) 0.033(2) 0.013(2) 0.009(2) -0.003(2) C22 0.036(2) 0.060(2) 0.024(2) 0.010(2) 0.0073(15) -0.002(2) C23 0.027(2) 0.053(2) 0.025(2) -0.004(2) 0.0050(14) -0.006(2) C29 0.0199(15) 0.027(2) 0.023(2) -0.0002(13) 0.0063(12) -0.0001(13) C30 0.023(2) 0.033(2) 0.023(2) -0.0019(14) 0.0028(13) 0.0011(14) C31 0.030(2) 0.048(2) 0.031(2) 0.008(2) 0.0029(15) 0.006(2) C32 0.041(2) 0.063(3) 0.035(2) -0.018(2) -0.010(2) 0.008(2) C33 0.025(2) 0.042(2) 0.040(2) -0.001(2) 0.0057(15) -0.003(2) C24 0.038(4) 0.028(4) 0.028(4) 0.002(3) 0.007(3) -0.004(3) C25 0.024(4) 0.036(4) 0.032(4) -0.006(3) 0.001(3) -0.008(3) C26 0.034(4) 0.028(4) 0.043(4) -0.002(3) 0.010(3) 0.001(3) C27 0.066(3) 0.058(3) 0.087(3) -0.040(3) 0.054(3) -0.044(2) C28 0.071(3) 0.052(3) 0.049(2) -0.019(2) 0.019(2) -0.025(2) C24A 0.030(5) 0.024(4) 0.025(4) -0.006(3) 0.011(4) 0.000(4) C25A 0.026(5) 0.028(5) 0.029(5) -0.012(4) 0.006(4) -0.006(4) C26A 0.030(4) 0.042(5) 0.034(4) -0.002(4) -0.007(3) 0.001(4) C27A 0.066(3) 0.058(3) 0.087(3) -0.040(3) 0.054(3) -0.044(2) C28A 0.071(3) 0.052(3) 0.049(2) -0.019(2) 0.019(2) -0.025(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge N4 1.889(3) . ? Ge N3 1.906(2) . ? Ge C1 2.339(3) . ? N2 C1 1.360(4) . ? N2 C2 1.397(4) . ? N2 C13 1.462(4) . ? N1 C1 1.359(4) . ? N1 C3 1.400(4) . ? N1 C8 1.471(4) . ? N3 C18 1.398(4) . ? N3 C24 1.484(7) . ? N3 C24A 1.497(8) . ? N4 C19 1.386(4) . ? N4 C29 1.453(4) . ? C2 C3 1.387(4) . ? C2 C7 1.396(4) . ? C3 C4 1.387(4) . ? C4 C5 1.380(5) . ? C5 C6 1.391(5) . ? C6 C7 1.375(5) . ? C8 C9 1.533(4) . ? C9 C10 1.525(5) . ? C9 C12 1.526(5) . ? C9 C11 1.533(5) . ? C13 C14 1.531(4) . ? C14 C16 1.520(5) . ? C14 C15 1.523(4) . ? C14 C17 1.528(4) . ? C18 C23 1.390(4) . ? C18 C19 1.424(4) . ? C19 C20 1.383(4) . ? C20 C21 1.393(4) . ? C21 C22 1.370(5) . ? C22 C23 1.402(5) . ? C29 C30 1.542(4) . ? C30 C31 1.527(5) . ? C30 C32 1.532(5) . ? C30 C33 1.535(4) . ? C24 C25 1.516(11) . ? C25 C28 1.501(8) . ? C25 C26 1.522(10) . ? C25 C27 1.572(8) . ? C24A C25A 1.518(12) . ? C25A C28A 1.401(9) . ? C25A C26A 1.544(12) . ? C25A C27A 1.609(9) . ? 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 Ge N3 84.53(10) . . ? N4 Ge C1 101.07(11) . . ? N3 Ge C1 101.25(10) . . ? C1 N2 C2 110.9(2) . . ? C1 N2 C13 124.6(2) . . ? C2 N2 C13 124.5(2) . . ? C1 N1 C3 111.0(2) . . ? C1 N1 C8 124.6(2) . . ? C3 N1 C8 124.3(2) . . ? C18 N3 C24 108.9(3) . . ? C18 N3 C24A 127.7(4) . . ? C18 N3 Ge 113.3(2) . . ? C24 N3 Ge 137.3(3) . . ? C24A N3 Ge 114.7(4) . . ? C19 N4 C29 121.1(2) . . ? C19 N4 Ge 114.3(2) . . ? C29 N4 Ge 123.6(2) . . ? N1 C1 N2 105.7(2) . . ? N1 C1 Ge 126.6(2) . . ? N2 C1 Ge 115.4(2) . . ? C3 C2 C7 121.1(3) . . ? C3 C2 N2 106.3(2) . . ? C7 C2 N2 132.6(3) . . ? C4 C3 C2 121.7(3) . . ? C4 C3 N1 132.1(3) . . ? C2 C3 N1 106.1(2) . . ? C5 C4 C3 116.9(3) . . ? C4 C5 C6 121.5(3) . . ? C7 C6 C5 121.8(3) . . ? C6 C7 C2 116.9(3) . . ? N1 C8 C9 115.9(3) . . ? C10 C9 C12 109.5(3) . . ? C10 C9 C8 106.0(3) . . ? C12 C9 C8 110.6(3) . . ? C10 C9 C11 108.7(3) . . ? C12 C9 C11 110.1(3) . . ? C8 C9 C11 111.8(3) . . ? N2 C13 C14 115.6(2) . . ? C16 C14 C15 109.7(3) . . ? C16 C14 C17 109.1(3) . . ? C15 C14 C17 108.8(3) . . ? C16 C14 C13 110.9(3) . . ? C15 C14 C13 107.0(3) . . ? C17 C14 C13 111.3(3) . . ? C23 C18 N3 127.0(3) . . ? C23 C18 C19 119.1(3) . . ? N3 C18 C19 113.9(3) . . ? C20 C19 N4 127.1(3) . . ? C20 C19 C18 118.9(3) . . ? N4 C19 C18 113.9(3) . . ? C19 C20 C21 121.2(3) . . ? C22 C21 C20 120.3(3) . . ? C21 C22 C23 119.8(3) . . ? C18 C23 C22 120.8(3) . . ? N4 C29 C30 117.0(2) . . ? C31 C30 C32 109.8(3) . . ? C31 C30 C33 108.9(3) . . ? C32 C30 C33 109.3(3) . . ? C31 C30 C29 110.6(3) . . ? C32 C30 C29 107.0(3) . . ? C33 C30 C29 111.2(2) . . ? N3 C24 C25 114.5(6) . . ? C28 C25 C24 110.9(6) . . ? C28 C25 C26 101.6(6) . . ? C24 C25 C26 112.0(6) . . ? C28 C25 C27 105.6(5) . . ? C24 C25 C27 107.9(6) . . ? C26 C25 C27 118.3(6) . . ? N3 C24A C25A 119.7(7) . . ? C28A C25A C26A 100.7(6) . . ? C28A C25A C24A 114.4(7) . . ? C26A C25A C24A 110.3(7) . . ? C28A C25A C27A 108.7(6) . . ? C26A C25A C27A 120.6(7) . . ? C24A C25A C27A 102.6(7) . . ? _refine_diff_density_max 0.422 _refine_diff_density_min -0.479 _refine_diff_density_rms 0.064 #===END data_GERHUS-HITCHCOCK-LAPPERT-10 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[C6H4(NCH2tBu)2CSn(NCH2tBu)2C6H4]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H52 N4 Sn' _chemical_formula_weight 623.48 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' 'Sn' 'Sn' -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 10.396(3) _cell_length_b 16.059(5) _cell_length_c 20.20(4) _cell_angle_alpha 90.00 _cell_angle_beta 103.39(6) _cell_angle_gamma 90.00 _cell_volume 3281(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.30 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.262 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1312 _exptl_absorpt_coefficient_mu 0.805 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.90 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6096 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0897 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 24.99 _reflns_number_total 5767 _reflns_number_gt 4063 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3-for Windows' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; The C24 neopentyl group is disordered with alternative C24,C25 and C27 sites and C26 and C28 in common. In order to include hydrogens dummy atoms C26B and C28B were included with identical parameters to C26 and C28. 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^)+(0.0314P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00078(16) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5767 _refine_ls_number_parameters 371 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0812 _refine_ls_R_factor_gt 0.0472 _refine_ls_wR_factor_ref 0.1079 _refine_ls_wR_factor_gt 0.0942 _refine_ls_goodness_of_fit_ref 1.008 _refine_ls_restrained_S_all 1.008 _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 Sn Sn 0.59554(3) 0.55540(2) 0.249369(18) 0.02102(12) Uani 1 1 d . A . N1 N 0.9273(4) 0.6109(2) 0.3021(2) 0.0213(9) Uani 1 1 d . A . N2 N 0.8865(4) 0.5403(2) 0.2084(2) 0.0210(9) Uani 1 1 d . A . N3 N 0.6102(4) 0.5618(3) 0.3549(2) 0.0248(9) Uani 1 1 d . . . N4 N 0.5254(4) 0.6755(2) 0.25807(19) 0.0216(9) Uani 1 1 d . . . C1 C 0.8281(5) 0.5877(3) 0.2496(3) 0.0218(11) Uani 1 1 d . . . C2 C 1.0220(5) 0.5323(3) 0.2366(3) 0.0238(12) Uani 1 1 d . . . C3 C 1.0486(5) 0.5767(3) 0.2970(3) 0.0210(11) Uani 1 1 d . A . C4 C 1.1743(5) 0.5789(3) 0.3404(3) 0.0311(13) Uani 1 1 d . . . H4 H 1.1920 0.6097 0.3816 0.037 Uiso 1 1 calc R A . C5 C 1.2713(5) 0.5340(3) 0.3201(3) 0.0329(14) Uani 1 1 d . A . H5 H 1.3582 0.5334 0.3482 0.040 Uiso 1 1 calc R . . C6 C 1.2449(5) 0.4892(3) 0.2590(3) 0.0373(15) Uani 1 1 d . . . H6 H 1.3145 0.4591 0.2467 0.045 Uiso 1 1 calc R A . C7 C 1.1197(5) 0.4877(3) 0.2158(3) 0.0317(13) Uani 1 1 d . A . H7 H 1.1020 0.4575 0.1742 0.038 Uiso 1 1 calc R . . C8 C 0.9096(5) 0.6622(3) 0.3599(2) 0.0240(11) Uani 1 1 d . . . H8A H 0.9720 0.6420 0.4015 0.029 Uiso 1 1 calc R A . H8B H 0.8190 0.6529 0.3661 0.029 Uiso 1 1 calc R . . C9 C 0.9302(5) 0.7562(3) 0.3539(3) 0.0297(13) Uani 1 1 d . A . C10 C 0.8984(6) 0.7957(4) 0.4183(3) 0.0463(17) Uani 1 1 d . . . H10A H 0.9104 0.8561 0.4172 0.069 Uiso 1 1 calc R A . H10B H 0.9581 0.7727 0.4590 0.069 Uiso 1 1 calc R . . H10C H 0.8067 0.7831 0.4195 0.069 Uiso 1 1 calc R . . C11 C 0.8345(6) 0.7909(4) 0.2906(3) 0.0457(16) Uani 1 1 d . . . H11A H 0.8492 0.8509 0.2873 0.069 Uiso 1 1 calc R A . H11B H 0.7433 0.7809 0.2940 0.069 Uiso 1 1 calc R . . H11C H 0.8500 0.7631 0.2499 0.069 Uiso 1 1 calc R . . C12 C 1.0726(5) 0.7775(4) 0.3518(3) 0.0441(16) Uani 1 1 d . . . H12A H 1.0814 0.8380 0.3479 0.066 Uiso 1 1 calc R A . H12B H 1.0947 0.7503 0.3124 0.066 Uiso 1 1 calc R . . H12C H 1.1329 0.7580 0.3936 0.066 Uiso 1 1 calc R . . C13 C 0.8181(5) 0.5017(3) 0.1441(2) 0.0234(11) Uani 1 1 d . . . H13A H 0.7285 0.4849 0.1479 0.028 Uiso 1 1 calc R A . H13B H 0.8664 0.4504 0.1372 0.028 Uiso 1 1 calc R . . C14 C 0.8051(5) 0.5577(4) 0.0809(2) 0.0298(12) Uani 1 1 d . A . C15 C 0.7381(7) 0.5047(4) 0.0197(3) 0.0475(17) Uani 1 1 d . . . H15A H 0.6503 0.4877 0.0246 0.071 Uiso 1 1 calc R A . H15B H 0.7919 0.4552 0.0173 0.071 Uiso 1 1 calc R . . H15C H 0.7292 0.5374 -0.0221 0.071 Uiso 1 1 calc R . . C16 C 0.7206(7) 0.6334(4) 0.0861(3) 0.0546(19) Uani 1 1 d . . . H16A H 0.7639 0.6670 0.1255 0.082 Uiso 1 1 calc R A . H16B H 0.6337 0.6152 0.0917 0.082 Uiso 1 1 calc R . . H16C H 0.7096 0.6668 0.0446 0.082 Uiso 1 1 calc R . . C17 C 0.9414(7) 0.5848(5) 0.0728(3) 0.057(2) Uani 1 1 d . . . H17A H 0.9845 0.6187 0.1119 0.086 Uiso 1 1 calc R A . H17B H 0.9318 0.6175 0.0310 0.086 Uiso 1 1 calc R . . H17C H 0.9955 0.5354 0.0702 0.086 Uiso 1 1 calc R . . C18 C 0.5704(5) 0.6384(3) 0.3763(2) 0.0216(11) Uani 1 1 d . A . C19 C 0.5239(5) 0.6985(3) 0.3241(2) 0.0233(11) Uani 1 1 d . A . C20 C 0.4809(5) 0.7754(3) 0.3430(3) 0.0302(13) Uani 1 1 d . . . H20 H 0.4495 0.8158 0.3087 0.036 Uiso 1 1 calc R A . C21 C 0.4826(6) 0.7945(3) 0.4096(3) 0.0354(14) Uani 1 1 d . A . H21 H 0.4533 0.8475 0.4209 0.042 Uiso 1 1 calc R . . C22 C 0.5268(6) 0.7365(4) 0.4598(3) 0.0368(14) Uani 1 1 d . . . H22 H 0.5276 0.7492 0.5059 0.044 Uiso 1 1 calc R A . C23 C 0.5699(5) 0.6600(4) 0.4431(3) 0.0328(13) Uani 1 1 d . A . H23 H 0.6004 0.6205 0.4783 0.039 Uiso 1 1 calc R . . C29 C 0.4928(5) 0.7353(3) 0.2025(2) 0.0222(11) Uani 1 1 d . A . H29A H 0.5552 0.7268 0.1728 0.027 Uiso 1 1 calc R . . H29B H 0.5087 0.7919 0.2221 0.027 Uiso 1 1 calc R . . C30 C 0.3510(5) 0.7327(3) 0.1574(2) 0.0244(12) Uani 1 1 d . . . C31 C 0.3373(6) 0.8068(4) 0.1079(3) 0.0437(16) Uani 1 1 d . A . H31A H 0.3520 0.8589 0.1338 0.066 Uiso 1 1 calc R . . H31B H 0.2483 0.8070 0.0781 0.066 Uiso 1 1 calc R . . H31C H 0.4030 0.8016 0.0803 0.066 Uiso 1 1 calc R . . C32 C 0.3281(5) 0.6519(4) 0.1170(3) 0.0367(14) Uani 1 1 d . A . H32A H 0.3946 0.6464 0.0899 0.055 Uiso 1 1 calc R . . H32B H 0.2396 0.6526 0.0867 0.055 Uiso 1 1 calc R . . H32C H 0.3355 0.6047 0.1484 0.055 Uiso 1 1 calc R . . C33 C 0.2473(5) 0.7413(4) 0.1990(3) 0.0387(15) Uani 1 1 d . A . H33A H 0.2619 0.7933 0.2251 0.058 Uiso 1 1 calc R . . H33B H 0.2539 0.6941 0.2303 0.058 Uiso 1 1 calc R . . H33C H 0.1591 0.7421 0.1684 0.058 Uiso 1 1 calc R . . C24 C 0.6144(12) 0.4815(8) 0.3908(6) 0.027(3) Uani 0.50 1 d P A 1 H24A H 0.5690 0.4399 0.3573 0.032 Uiso 0.50 1 calc PR A 1 H24B H 0.5610 0.4877 0.4252 0.032 Uiso 0.50 1 calc PR A 1 C25 C 0.7461(13) 0.4449(9) 0.4264(7) 0.031(3) Uani 0.50 1 d P A 1 C26 C 0.8199(6) 0.4231(4) 0.3676(3) 0.0512(19) Uani 0.50 1 d P A 1 H26A H 0.8225 0.4726 0.3396 0.077 Uiso 0.50 1 calc PR A 1 H26B H 0.7722 0.3784 0.3391 0.077 Uiso 0.50 1 calc PR A 1 H26C H 0.9104 0.4048 0.3880 0.077 Uiso 0.50 1 calc PR A 1 C27 C 0.8181(12) 0.5078(7) 0.4832(6) 0.047(3) Uani 0.50 1 d P A 1 H27A H 0.8271 0.5621 0.4625 0.070 Uiso 0.50 1 calc PR A 1 H27B H 0.9059 0.4862 0.5049 0.070 Uiso 0.50 1 calc PR A 1 H27C H 0.7658 0.5142 0.5175 0.070 Uiso 0.50 1 calc PR A 1 C28 C 0.7413(7) 0.3740(4) 0.4663(3) 0.0554(19) Uani 0.50 1 d P A 1 H28A H 0.8314 0.3565 0.4881 0.083 Uiso 0.50 1 calc PR A 1 H28B H 0.6960 0.3289 0.4373 0.083 Uiso 0.50 1 calc PR A 1 H28C H 0.6930 0.3870 0.5013 0.083 Uiso 0.50 1 calc PR A 1 C24B C 0.6664(12) 0.5100(7) 0.4167(6) 0.024(3) Uani 0.50 1 d P A 2 H24C H 0.6020 0.5086 0.4459 0.029 Uiso 0.50 1 calc PR A 2 H24D H 0.7478 0.5371 0.4429 0.029 Uiso 0.50 1 calc PR A 2 C25B C 0.6989(12) 0.4218(8) 0.4009(7) 0.022(3) Uani 0.50 1 d P A 2 C26B C 0.8199(6) 0.4231(4) 0.3676(3) 0.0512(19) Uani 0.50 1 d P A 2 H26D H 0.7958 0.4521 0.3238 0.077 Uiso 0.50 1 calc PR A 2 H26E H 0.8464 0.3659 0.3604 0.077 Uiso 0.50 1 calc PR A 2 H26F H 0.8937 0.4522 0.3977 0.077 Uiso 0.50 1 calc PR A 2 C27B C 0.5783(10) 0.3724(6) 0.3647(5) 0.029(3) Uani 0.50 1 d P A 2 H27D H 0.5413 0.3973 0.3201 0.043 Uiso 0.50 1 calc PR A 2 H27E H 0.5118 0.3733 0.3920 0.043 Uiso 0.50 1 calc PR A 2 H27F H 0.6042 0.3147 0.3587 0.043 Uiso 0.50 1 calc PR A 2 C28B C 0.7413(7) 0.3740(4) 0.4663(3) 0.0554(19) Uani 0.50 1 d P A 2 H28D H 0.8222 0.3986 0.4940 0.083 Uiso 0.50 1 calc PR A 2 H28E H 0.7581 0.3158 0.4562 0.083 Uiso 0.50 1 calc PR A 2 H28F H 0.6711 0.3763 0.4913 0.083 Uiso 0.50 1 calc PR A 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn 0.01627(17) 0.01900(18) 0.02665(19) -0.00286(18) 0.00261(12) 0.00048(17) N1 0.020(2) 0.018(2) 0.025(2) -0.0073(18) 0.0030(18) -0.0008(18) N2 0.016(2) 0.023(2) 0.025(2) -0.0042(18) 0.0060(17) -0.0006(18) N3 0.021(2) 0.027(2) 0.025(2) 0.007(2) 0.0038(18) 0.004(2) N4 0.023(2) 0.018(2) 0.021(2) 0.0001(18) -0.0007(18) 0.0081(18) C1 0.019(3) 0.013(2) 0.031(3) 0.002(2) 0.003(2) -0.005(2) C2 0.014(3) 0.019(3) 0.038(3) 0.002(2) 0.007(2) -0.003(2) C3 0.017(2) 0.018(3) 0.030(3) -0.001(2) 0.009(2) -0.001(2) C4 0.024(3) 0.031(3) 0.037(3) 0.002(2) 0.004(2) -0.001(2) C5 0.017(3) 0.030(3) 0.051(4) 0.010(3) 0.006(3) -0.001(2) C6 0.017(3) 0.025(3) 0.073(5) 0.007(3) 0.018(3) 0.003(2) C7 0.029(3) 0.021(3) 0.048(4) -0.001(3) 0.015(3) -0.002(2) C8 0.018(3) 0.030(3) 0.024(3) -0.006(2) 0.005(2) -0.003(2) C9 0.025(3) 0.025(3) 0.038(3) -0.009(2) 0.005(2) -0.001(2) C10 0.044(4) 0.039(4) 0.053(4) -0.020(3) 0.006(3) 0.002(3) C11 0.051(4) 0.032(3) 0.045(4) 0.000(3) -0.008(3) -0.002(3) C12 0.030(3) 0.029(3) 0.076(5) -0.015(3) 0.017(3) -0.015(3) C13 0.020(3) 0.020(3) 0.031(3) -0.006(2) 0.008(2) -0.001(2) C14 0.036(3) 0.028(3) 0.026(3) -0.002(3) 0.009(2) -0.009(3) C15 0.065(4) 0.049(4) 0.025(3) -0.007(3) 0.003(3) -0.006(4) C16 0.088(5) 0.041(4) 0.033(4) 0.008(3) 0.011(4) 0.022(4) C17 0.061(5) 0.078(5) 0.036(4) 0.014(3) 0.019(3) -0.026(4) C18 0.015(2) 0.027(3) 0.019(3) 0.000(2) -0.002(2) -0.001(2) C19 0.020(3) 0.029(3) 0.019(3) -0.002(2) 0.001(2) -0.002(2) C20 0.043(3) 0.021(3) 0.026(3) 0.001(2) 0.008(3) 0.005(3) C21 0.046(4) 0.024(3) 0.038(3) -0.004(3) 0.013(3) 0.004(3) C22 0.039(3) 0.052(4) 0.021(3) -0.009(3) 0.010(3) 0.009(3) C23 0.034(3) 0.045(4) 0.021(3) 0.004(3) 0.009(2) 0.006(3) C29 0.022(3) 0.024(3) 0.021(3) 0.002(2) 0.007(2) 0.002(2) C30 0.018(3) 0.028(3) 0.023(3) 0.002(2) -0.003(2) 0.000(2) C31 0.034(3) 0.055(4) 0.034(3) 0.018(3) -0.010(3) -0.005(3) C32 0.026(3) 0.047(4) 0.031(3) -0.007(3) -0.004(2) -0.004(3) C33 0.021(3) 0.042(4) 0.051(4) -0.004(3) 0.004(3) 0.006(3) C24 0.031(8) 0.025(7) 0.026(7) 0.004(5) 0.009(6) 0.000(6) C25 0.019(7) 0.026(8) 0.045(9) 0.018(7) 0.001(6) 0.003(6) C26 0.048(4) 0.042(4) 0.071(5) 0.030(3) 0.029(4) 0.030(3) C27 0.046(8) 0.035(7) 0.052(8) 0.001(6) -0.004(6) -0.001(6) C28 0.077(5) 0.044(4) 0.049(4) 0.020(3) 0.022(4) 0.025(4) C24B 0.025(7) 0.015(6) 0.029(7) -0.006(5) 0.000(5) 0.005(5) C25B 0.010(6) 0.018(7) 0.032(8) 0.004(5) -0.005(5) 0.002(5) C26B 0.048(4) 0.042(4) 0.071(5) 0.030(3) 0.029(4) 0.030(3) C27B 0.023(6) 0.024(6) 0.037(6) 0.006(5) 0.001(5) 0.009(5) C28B 0.077(5) 0.044(4) 0.049(4) 0.020(3) 0.022(4) 0.025(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn N4 2.083(4) . ? Sn N3 2.104(5) . ? Sn C1 2.472(5) . ? N1 C1 1.349(6) . ? N1 C3 1.401(6) . ? N1 C8 1.474(6) . ? N2 C1 1.369(6) . ? N2 C2 1.398(6) . ? N2 C13 1.467(6) . ? N3 C18 1.399(6) . ? N3 C24 1.474(12) . ? N3 C24B 1.501(12) . ? N4 C19 1.387(6) . ? N4 C29 1.457(6) . ? C2 C3 1.385(7) . ? C2 C7 1.386(7) . ? C3 C4 1.395(7) . ? C4 C5 1.378(7) . ? C5 C6 1.399(8) . ? C6 C7 1.389(8) . ? C8 C9 1.533(7) . ? C9 C12 1.530(7) . ? C9 C11 1.532(8) . ? C9 C10 1.550(8) . ? C13 C14 1.542(7) . ? C14 C16 1.518(8) . ? C14 C17 1.528(8) . ? C14 C15 1.529(7) . ? C18 C23 1.394(7) . ? C18 C19 1.429(7) . ? C19 C20 1.396(7) . ? C20 C21 1.377(8) . ? C21 C22 1.375(8) . ? C22 C23 1.376(8) . ? C29 C30 1.543(6) . ? C30 C33 1.519(7) . ? C30 C32 1.522(7) . ? C30 C31 1.540(7) . ? C24 C25 1.510(17) . ? C25 C28 1.404(14) . ? C25 C27 1.581(18) . ? C25 C26 1.594(16) . ? C24B C25B 1.507(17) . ? C25B C27B 1.520(15) . ? 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 Sn N3 79.30(16) . . ? N4 Sn C1 99.60(16) . . ? N3 Sn C1 98.41(17) . . ? C1 N1 C3 111.8(4) . . ? C1 N1 C8 124.3(4) . . ? C3 N1 C8 123.8(4) . . ? C1 N2 C2 110.6(4) . . ? C1 N2 C13 125.6(4) . . ? C2 N2 C13 123.9(4) . . ? C18 N3 C24 126.5(6) . . ? C18 N3 C24B 108.5(5) . . ? C24 N3 C24B 31.3(5) . . ? C18 N3 Sn 113.5(3) . . ? C24 N3 Sn 116.3(6) . . ? C24B N3 Sn 137.6(5) . . ? C19 N4 C29 120.8(4) . . ? C19 N4 Sn 114.2(3) . . ? C29 N4 Sn 124.7(3) . . ? N1 C1 N2 105.4(4) . . ? N1 C1 Sn 129.0(4) . . ? N2 C1 Sn 117.0(3) . . ? C3 C2 C7 121.5(5) . . ? C3 C2 N2 106.7(4) . . ? C7 C2 N2 131.7(5) . . ? C2 C3 C4 122.3(5) . . ? C2 C3 N1 105.5(4) . . ? C4 C3 N1 132.2(5) . . ? C5 C4 C3 116.3(5) . . ? C4 C5 C6 121.6(5) . . ? C7 C6 C5 121.8(5) . . ? C2 C7 C6 116.5(5) . . ? N1 C8 C9 116.3(4) . . ? C12 C9 C11 109.9(5) . . ? C12 C9 C8 112.1(4) . . ? C11 C9 C8 110.4(4) . . ? C12 C9 C10 109.1(5) . . ? C11 C9 C10 109.2(5) . . ? C8 C9 C10 106.0(5) . . ? N2 C13 C14 114.7(4) . . ? C16 C14 C17 110.2(5) . . ? C16 C14 C15 109.8(5) . . ? C17 C14 C15 109.4(5) . . ? C16 C14 C13 110.5(4) . . ? C17 C14 C13 110.4(5) . . ? C15 C14 C13 106.4(5) . . ? C23 C18 N3 125.8(5) . . ? C23 C18 C19 118.1(5) . . ? N3 C18 C19 116.1(4) . . ? N4 C19 C20 125.0(5) . . ? N4 C19 C18 116.9(4) . . ? C20 C19 C18 118.0(5) . . ? C21 C20 C19 122.1(5) . . ? C22 C21 C20 119.8(5) . . ? C21 C22 C23 119.7(5) . . ? C22 C23 C18 122.3(5) . . ? N4 C29 C30 117.2(4) . . ? C33 C30 C32 109.3(5) . . ? C33 C30 C31 108.5(5) . . ? C32 C30 C31 109.3(5) . . ? C33 C30 C29 112.0(4) . . ? C32 C30 C29 110.4(4) . . ? C31 C30 C29 107.1(4) . . ? N3 C24 C25 119.6(10) . . ? C28 C25 C24 116.1(11) . . ? C28 C25 C27 100.1(10) . . ? C24 C25 C27 108.8(11) . . ? C28 C25 C26 109.7(10) . . ? C24 C25 C26 105.7(10) . . ? C27 C25 C26 116.9(10) . . ? N3 C24B C25B 114.1(10) . . ? C24B C25B C27B 113.1(10) . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 24.99 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 0.621 _refine_diff_density_min -0.942 _refine_diff_density_rms 0.100 #===END data_GERHUS-HITCHCOCK-LAPPERT-11 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common '[C6H4(NCH2tBu)2CPb(NCH2tBu)2C6H4]' _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C33 H52 N4 Pb' _chemical_formula_weight 711.98 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Pb' 'Pb' -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 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 10.421(4) _cell_length_b 16.015(4) _cell_length_c 20.254(10) _cell_angle_alpha 90.00 _cell_angle_beta 102.61(4) _cell_angle_gamma 90.00 _cell_volume 3299(2) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 25 _cell_measurement_theta_min 7 _cell_measurement_theta_max 10 _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.434 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 5.140 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.87 _exptl_absorpt_correction_T_max 1.00 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 ? _diffrn_measurement_method \w--2\q _diffrn_detector_area_resol_mean ? _diffrn_standards_number 2 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 120 _diffrn_standards_decay_% 0 _diffrn_reflns_number 6112 _diffrn_reflns_av_R_equivalents 0.0365 _diffrn_reflns_av_sigmaI/netI 0.0821 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 19 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.04 _diffrn_reflns_theta_max 24.97 _reflns_number_total 5784 _reflns_number_gt 4274 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Enraf-Nonius CAD4' _computing_cell_refinement 'Enraf-Nonius CAD4' _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'ORTEP3 for Windows' _computing_publication_material 'SHELXL-97 (Sheldrick, 1997)' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0206P)^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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00019(6) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 5784 _refine_ls_number_parameters 344 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0705 _refine_ls_R_factor_gt 0.0408 _refine_ls_wR_factor_ref 0.0856 _refine_ls_wR_factor_gt 0.0764 _refine_ls_goodness_of_fit_ref 0.989 _refine_ls_restrained_S_all 0.989 _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 Pb Pb 0.59140(3) 0.546054(17) 0.251867(13) 0.01806(9) Uani 1 1 d . . . N1 N 0.9322(5) 0.6027(3) 0.3040(3) 0.0184(13) Uani 1 1 d . . . N2 N 0.8927(5) 0.5339(3) 0.2102(3) 0.0195(13) Uani 1 1 d . . . N3 N 0.6085(5) 0.5584(4) 0.3625(3) 0.0198(13) Uani 1 1 d . . . N4 N 0.5149(6) 0.6701(3) 0.2617(3) 0.0203(13) Uani 1 1 d . . . C1 C 0.8333(7) 0.5810(4) 0.2511(3) 0.0189(15) Uani 1 1 d . . . C2 C 1.0263(7) 0.5251(4) 0.2382(4) 0.0217(17) Uani 1 1 d . . . C3 C 1.0524(7) 0.5688(4) 0.2989(4) 0.0230(17) Uani 1 1 d . . . C4 C 1.1761(7) 0.5706(5) 0.3413(4) 0.0304(19) Uani 1 1 d . . . H4 H 1.1935 0.6018 0.3822 0.036 Uiso 1 1 calc R . . C5 C 1.2729(7) 0.5245(5) 0.3211(4) 0.033(2) Uani 1 1 d . . . H5 H 1.3582 0.5224 0.3498 0.040 Uiso 1 1 calc R . . C6 C 1.2494(7) 0.4808(4) 0.2599(4) 0.0270(18) Uani 1 1 d . . . H6 H 1.3191 0.4508 0.2473 0.032 Uiso 1 1 calc R . . C7 C 1.1262(7) 0.4806(4) 0.2175(4) 0.0256(18) Uani 1 1 d . . . H7 H 1.1099 0.4514 0.1756 0.031 Uiso 1 1 calc R . . C8 C 0.9111(7) 0.6526(4) 0.3619(3) 0.0241(17) Uani 1 1 d . . . H8A H 0.9731 0.6328 0.4031 0.029 Uiso 1 1 calc R . . H8B H 0.8210 0.6415 0.3681 0.029 Uiso 1 1 calc R . . C9 C 0.9280(7) 0.7472(4) 0.3565(4) 0.0246(17) Uani 1 1 d . . . C10 C 0.9004(9) 0.7862(5) 0.4218(4) 0.042(2) Uani 1 1 d . . . H10A H 0.9108 0.8469 0.4204 0.063 Uiso 1 1 calc R . . H10B H 0.9625 0.7636 0.4612 0.063 Uiso 1 1 calc R . . H10C H 0.8104 0.7728 0.4253 0.063 Uiso 1 1 calc R . . C11 C 0.8286(8) 0.7818(5) 0.2961(4) 0.040(2) Uani 1 1 d . . . H11A H 0.8407 0.8422 0.2932 0.060 Uiso 1 1 calc R . . H11B H 0.7394 0.7701 0.3018 0.060 Uiso 1 1 calc R . . H11C H 0.8419 0.7552 0.2545 0.060 Uiso 1 1 calc R . . C12 C 1.0683(8) 0.7707(5) 0.3511(5) 0.046(2) Uani 1 1 d . . . H12A H 1.0753 0.8316 0.3479 0.069 Uiso 1 1 calc R . . H12B H 1.0882 0.7448 0.3107 0.069 Uiso 1 1 calc R . . H12C H 1.1310 0.7508 0.3914 0.069 Uiso 1 1 calc R . . C13 C 0.8260(7) 0.4966(4) 0.1461(3) 0.0222(16) Uani 1 1 d . . . H13A H 0.7372 0.4789 0.1503 0.027 Uiso 1 1 calc R . . H13B H 0.8748 0.4456 0.1386 0.027 Uiso 1 1 calc R . . C14 C 0.8115(7) 0.5518(5) 0.0835(3) 0.0261(16) Uani 1 1 d . . . C15 C 0.7467(9) 0.4978(6) 0.0227(4) 0.048(2) Uani 1 1 d . . . H15A H 0.8028 0.4496 0.0194 0.073 Uiso 1 1 calc R . . H15B H 0.7352 0.5310 -0.0188 0.073 Uiso 1 1 calc R . . H15C H 0.6607 0.4784 0.0286 0.073 Uiso 1 1 calc R . . C16 C 0.7243(10) 0.6259(5) 0.0886(4) 0.053(3) Uani 1 1 d . . . H16A H 0.6378 0.6062 0.0934 0.079 Uiso 1 1 calc R . . H16B H 0.7142 0.6599 0.0475 0.079 Uiso 1 1 calc R . . H16C H 0.7643 0.6597 0.1280 0.079 Uiso 1 1 calc R . . C17 C 0.9462(9) 0.5800(6) 0.0752(4) 0.055(3) Uani 1 1 d . . . H17A H 1.0007 0.5310 0.0718 0.083 Uiso 1 1 calc R . . H17B H 0.9882 0.6136 0.1144 0.083 Uiso 1 1 calc R . . H17C H 0.9365 0.6137 0.0340 0.083 Uiso 1 1 calc R . . C18 C 0.5674(6) 0.6359(4) 0.3803(3) 0.0199(15) Uani 1 1 d . . . C19 C 0.5162(7) 0.6937(4) 0.3281(3) 0.0184(15) Uani 1 1 d . . . C20 C 0.4701(7) 0.7708(5) 0.3453(4) 0.0253(17) Uani 1 1 d . . . H20 H 0.4341 0.8091 0.3103 0.030 Uiso 1 1 calc R . . C21 C 0.4753(8) 0.7933(5) 0.4126(4) 0.032(2) Uani 1 1 d . . . H21 H 0.4438 0.8462 0.4232 0.039 Uiso 1 1 calc R . . C22 C 0.5270(7) 0.7374(5) 0.4633(4) 0.0307(19) Uani 1 1 d . . . H22 H 0.5316 0.7520 0.5092 0.037 Uiso 1 1 calc R . . C23 C 0.5717(7) 0.6610(5) 0.4476(3) 0.0262(17) Uani 1 1 d . . . H23 H 0.6068 0.6235 0.4833 0.031 Uiso 1 1 calc R . . C24 C 0.6636(7) 0.5041(5) 0.4185(4) 0.0272(18) Uani 1 1 d . . . H24A H 0.5995 0.5004 0.4480 0.033 Uiso 1 1 calc R . . H24B H 0.7435 0.5314 0.4452 0.033 Uiso 1 1 calc R . . C25 C 0.7003(7) 0.4158(5) 0.4029(4) 0.0270(18) Uani 1 1 d . . . C26 C 0.8107(7) 0.4126(5) 0.3623(4) 0.0329(19) Uani 1 1 d . . . H26A H 0.8302 0.3543 0.3536 0.049 Uiso 1 1 calc R . . H26B H 0.8900 0.4395 0.3885 0.049 Uiso 1 1 calc R . . H26C H 0.7814 0.4419 0.3192 0.049 Uiso 1 1 calc R . . C27 C 0.5792(8) 0.3663(5) 0.3662(4) 0.036(2) Uani 1 1 d . . . H27A H 0.6058 0.3095 0.3571 0.055 Uiso 1 1 calc R . . H27B H 0.5402 0.3940 0.3233 0.055 Uiso 1 1 calc R . . H27C H 0.5144 0.3639 0.3947 0.055 Uiso 1 1 calc R . . C28 C 0.7536(8) 0.3722(5) 0.4706(4) 0.038(2) Uani 1 1 d . . . H28A H 0.7776 0.3145 0.4624 0.057 Uiso 1 1 calc R . . H28B H 0.6859 0.3720 0.4974 0.057 Uiso 1 1 calc R . . H28C H 0.8314 0.4020 0.4953 0.057 Uiso 1 1 calc R . . C29 C 0.4888(7) 0.7303(4) 0.2080(3) 0.0211(16) Uani 1 1 d . . . H29A H 0.5554 0.7229 0.1803 0.025 Uiso 1 1 calc R . . H29B H 0.5018 0.7867 0.2284 0.025 Uiso 1 1 calc R . . C30 C 0.3511(7) 0.7279(4) 0.1599(3) 0.0238(17) Uani 1 1 d . . . C31 C 0.3427(8) 0.8006(5) 0.1102(4) 0.041(2) Uani 1 1 d . . . H31A H 0.4128 0.7953 0.0851 0.061 Uiso 1 1 calc R . . H31B H 0.3530 0.8534 0.1352 0.061 Uiso 1 1 calc R . . H31C H 0.2570 0.7997 0.0785 0.061 Uiso 1 1 calc R . . C32 C 0.3310(8) 0.6465(5) 0.1194(4) 0.0338(19) Uani 1 1 d . . . H32A H 0.4003 0.6406 0.0939 0.051 Uiso 1 1 calc R . . H32B H 0.2450 0.6475 0.0879 0.051 Uiso 1 1 calc R . . H32C H 0.3347 0.5992 0.1504 0.051 Uiso 1 1 calc R . . C33 C 0.2416(7) 0.7353(5) 0.1992(4) 0.0327(19) Uani 1 1 d . . . H33A H 0.2529 0.7872 0.2255 0.049 Uiso 1 1 calc R . . H33B H 0.2460 0.6875 0.2299 0.049 Uiso 1 1 calc R . . H33C H 0.1560 0.7358 0.1674 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb 0.01860(14) 0.01932(14) 0.01663(13) -0.00290(15) 0.00463(9) 0.00014(15) N1 0.017(3) 0.021(3) 0.017(3) 0.001(3) 0.005(2) -0.001(3) N2 0.024(3) 0.013(3) 0.024(3) -0.001(3) 0.010(3) -0.007(3) N3 0.022(3) 0.024(4) 0.013(3) 0.001(3) 0.005(2) 0.003(3) N4 0.026(3) 0.018(3) 0.017(3) -0.004(2) 0.007(3) 0.003(3) C1 0.024(4) 0.017(4) 0.019(4) -0.001(3) 0.012(3) -0.004(3) C2 0.015(4) 0.024(4) 0.028(4) 0.005(3) 0.009(3) 0.003(3) C3 0.021(4) 0.024(4) 0.026(4) 0.004(3) 0.009(3) -0.005(3) C4 0.024(4) 0.036(5) 0.029(4) 0.001(3) 0.001(3) -0.006(3) C5 0.022(4) 0.033(5) 0.043(5) 0.005(4) 0.005(4) -0.003(4) C6 0.023(4) 0.016(4) 0.045(5) -0.001(3) 0.015(4) 0.003(3) C7 0.027(4) 0.022(4) 0.031(4) -0.006(3) 0.012(3) -0.005(3) C8 0.023(4) 0.034(5) 0.017(4) 0.000(3) 0.007(3) -0.001(3) C9 0.028(4) 0.018(4) 0.027(4) -0.005(3) 0.005(3) -0.004(3) C10 0.055(6) 0.039(5) 0.033(5) -0.022(4) 0.014(4) -0.009(5) C11 0.056(6) 0.030(5) 0.034(5) 0.004(4) 0.011(4) -0.004(4) C12 0.040(5) 0.027(5) 0.077(7) -0.014(5) 0.026(5) -0.010(4) C13 0.019(4) 0.024(4) 0.024(4) -0.008(3) 0.006(3) -0.006(3) C14 0.038(4) 0.026(4) 0.014(3) -0.003(4) 0.006(3) -0.010(4) C15 0.067(7) 0.055(6) 0.022(4) -0.004(4) 0.008(4) -0.018(5) C16 0.085(8) 0.031(5) 0.037(5) 0.005(4) 0.003(5) 0.014(5) C17 0.057(6) 0.085(8) 0.027(5) 0.015(5) 0.017(4) -0.029(6) C18 0.019(4) 0.023(4) 0.017(4) -0.003(3) 0.003(3) 0.003(3) C19 0.021(4) 0.018(4) 0.015(3) -0.004(3) 0.003(3) -0.003(3) C20 0.032(4) 0.021(4) 0.023(4) 0.007(3) 0.007(3) 0.006(4) C21 0.049(5) 0.017(4) 0.033(5) -0.005(4) 0.014(4) 0.009(4) C22 0.041(5) 0.035(5) 0.019(4) -0.004(4) 0.010(4) 0.001(4) C23 0.032(4) 0.029(5) 0.020(4) -0.002(3) 0.011(3) -0.001(4) C24 0.030(4) 0.022(4) 0.034(4) 0.005(4) 0.017(4) 0.003(4) C25 0.024(4) 0.026(4) 0.031(4) 0.009(3) 0.007(3) 0.015(3) C26 0.032(5) 0.033(5) 0.036(5) 0.001(4) 0.012(4) 0.016(4) C27 0.043(5) 0.028(5) 0.040(5) 0.005(4) 0.013(4) 0.002(4) C28 0.049(5) 0.036(5) 0.029(4) 0.006(4) 0.009(4) 0.005(4) C29 0.032(4) 0.014(4) 0.020(4) 0.001(3) 0.011(3) -0.002(3) C30 0.031(4) 0.018(4) 0.022(4) 0.001(3) 0.005(3) 0.002(3) C31 0.038(5) 0.044(5) 0.031(5) 0.012(4) -0.012(4) -0.003(4) C32 0.030(4) 0.033(5) 0.035(5) -0.006(4) 0.000(4) 0.000(4) C33 0.023(4) 0.037(5) 0.039(5) -0.005(4) 0.008(4) 0.006(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb N4 2.167(5) . ? Pb N3 2.218(5) . ? Pb C1 2.586(7) . ? N1 C1 1.360(8) . ? N1 C3 1.389(9) . ? N1 C8 1.474(8) . ? N2 C1 1.364(8) . ? N2 C2 1.391(9) . ? N2 C13 1.460(8) . ? N3 C18 1.386(9) . ? N3 C24 1.445(9) . ? N4 C19 1.393(8) . ? N4 C29 1.435(8) . ? C2 C3 1.390(10) . ? C2 C7 1.399(9) . ? C3 C4 1.385(10) . ? C4 C5 1.382(10) . ? C5 C6 1.398(10) . ? C6 C7 1.380(10) . ? C8 C9 1.532(10) . ? C9 C11 1.524(10) . ? C9 C12 1.537(10) . ? C9 C10 1.546(10) . ? C13 C14 1.524(10) . ? C14 C16 1.512(11) . ? C14 C17 1.519(10) . ? C14 C15 1.536(10) . ? C18 C23 1.412(9) . ? C18 C19 1.419(9) . ? C19 C20 1.397(10) . ? C20 C21 1.399(10) . ? C21 C22 1.379(10) . ? C22 C23 1.372(10) . ? C24 C25 1.517(10) . ? C25 C28 1.531(10) . ? C25 C27 1.538(10) . ? C25 C26 1.554(10) . ? C29 C30 1.549(10) . ? C30 C33 1.532(10) . ? C30 C31 1.528(10) . ? C30 C32 1.531(10) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N4 Pb N3 77.0(2) . . ? N4 Pb C1 100.4(2) . . ? N3 Pb C1 97.1(2) . . ? C1 N1 C3 112.4(6) . . ? C1 N1 C8 123.1(6) . . ? C3 N1 C8 124.3(6) . . ? C1 N2 C2 110.8(6) . . ? C1 N2 C13 125.1(6) . . ? C2 N2 C13 124.1(6) . . ? C18 N3 C24 115.3(5) . . ? C18 N3 Pb 112.4(4) . . ? C24 N3 Pb 132.1(5) . . ? C19 N4 C29 120.7(6) . . ? C19 N4 Pb 114.3(4) . . ? C29 N4 Pb 123.9(4) . . ? N1 C1 N2 104.7(6) . . ? N1 C1 Pb 128.5(4) . . ? N2 C1 Pb 117.1(4) . . ? N2 C2 C3 107.1(6) . . ? N2 C2 C7 132.3(7) . . ? C3 C2 C7 120.5(7) . . ? C4 C3 C2 122.3(7) . . ? C4 C3 N1 132.7(7) . . ? C2 C3 N1 105.0(6) . . ? C5 C4 C3 116.5(7) . . ? C4 C5 C6 122.1(7) . . ? C5 C6 C7 120.8(7) . . ? C2 C7 C6 117.7(7) . . ? N1 C8 C9 116.1(6) . . ? C11 C9 C12 110.2(7) . . ? C11 C9 C8 110.4(6) . . ? C12 C9 C8 112.0(6) . . ? C11 C9 C10 108.6(6) . . ? C12 C9 C10 108.6(6) . . ? C8 C9 C10 107.0(6) . . ? N2 C13 C14 116.3(6) . . ? C16 C14 C17 110.9(8) . . ? C16 C14 C13 110.6(6) . . ? C17 C14 C13 109.8(6) . . ? C16 C14 C15 109.3(7) . . ? C17 C14 C15 109.5(7) . . ? C13 C14 C15 106.7(6) . . ? N3 C18 C23 124.0(6) . . ? N3 C18 C19 118.5(6) . . ? C23 C18 C19 117.5(6) . . ? N4 C19 C20 123.2(6) . . ? N4 C19 C18 117.8(6) . . ? C20 C19 C18 119.0(6) . . ? C19 C20 C21 121.9(7) . . ? C22 C21 C20 119.0(7) . . ? C21 C22 C23 120.2(7) . . ? C22 C23 C18 122.4(7) . . ? N3 C24 C25 118.2(6) . . ? C24 C25 C28 107.3(6) . . ? C24 C25 C27 111.3(6) . . ? C28 C25 C27 107.3(6) . . ? C24 C25 C26 113.0(6) . . ? C28 C25 C26 107.0(6) . . ? C27 C25 C26 110.6(6) . . ? N4 C29 C30 117.2(6) . . ? C33 C30 C31 110.0(6) . . ? C33 C30 C32 108.3(6) . . ? C31 C30 C32 108.3(6) . . ? C33 C30 C29 111.3(6) . . ? C31 C30 C29 107.9(6) . . ? C32 C30 C29 111.0(6) . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 24.97 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.894 _refine_diff_density_min -0.920 _refine_diff_density_rms 0.145 #===END