# Electronic Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 2013 ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_WLF014 _audit_creation_date 2013-01-17T12:09:54-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C27 H54 Ge1 N2 O3 Si2' _chemical_formula_sum 'C27 H54 Ge1 N2 O3 Si2' _chemical_formula_weight 583.49 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 13.4042(4) _cell_length_b 17.7120(4) _cell_length_c 13.8889(4) _cell_angle_alpha 90 _cell_angle_beta 99.1210(10) _cell_angle_gamma 90 _cell_volume 3255.74(15) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5366 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 27.24 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.25 _exptl_crystal_density_diffrn 1.19 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1256 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.042 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.690 _exptl_absorpt_correction_T_max 0.771 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0388 _diffrn_reflns_av_unetI/netI 0.0533 _diffrn_reflns_number 19774 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 22 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.02 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.995 _diffrn_measured_fraction_theta_max 0.995 _reflns_number_total 7420 _reflns_number_gt 5797 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0558P)^2^+4.3766P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7420 _refine_ls_number_parameters 330 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0512 _refine_ls_wR_factor_ref 0.1325 _refine_ls_wR_factor_gt 0.123 _refine_ls_goodness_of_fit_ref 1.051 _refine_ls_restrained_S_all 1.051 _refine_ls_shift/su_max 0.086 _refine_ls_shift/su_mean 0.004 _refine_diff_density_max 1.723 _refine_diff_density_min -0.777 _refine_diff_density_rms 0.085 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' 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 Ge1 Ge 0.71139(2) 0.022295(17) 0.70710(2) 0.01933(10) Uani 1 1 d . . . Si1 Si 0.72782(7) -0.05613(5) 0.91839(6) 0.0273(2) Uani 1 1 d . . . Si2 Si 0.76859(7) 0.11112(5) 0.89737(6) 0.0253(2) Uani 1 1 d . . . N1 N 0.74715(19) 0.02157(13) 0.84515(17) 0.0205(5) Uani 1 1 d . . . O1 O 0.66583(16) -0.07792(11) 0.69497(14) 0.0220(4) Uani 1 1 d . . . C2 C 0.6604(2) -0.10743(16) 0.6035(2) 0.0214(6) Uani 1 1 d . . . C3 C 0.5683(2) -0.13330(16) 0.5493(2) 0.0247(6) Uani 1 1 d . . . C4 C 0.5714(3) -0.15765(17) 0.4543(2) 0.0305(7) Uani 1 1 d . . . H4 H 0.5099 -0.1739 0.4164 0.037 Uiso 1 1 calc R . . C5 C 0.6587(3) -0.15975(17) 0.4110(2) 0.0303(8) Uani 1 1 d . . . C6 C 0.7485(3) -0.13866(17) 0.4687(2) 0.0273(7) Uani 1 1 d . . . H6 H 0.81 -0.1417 0.443 0.033 Uiso 1 1 calc R . . C7 C 0.7499(2) -0.11297(16) 0.5644(2) 0.0228(6) Uani 1 1 d . . . C8 C 0.8475(2) -0.09804(19) 0.6307(2) 0.0277(7) Uani 1 1 d . . . H8A H 0.8503 -0.13 0.6895 0.033 Uiso 1 1 calc R . . H8B H 0.9041 -0.1132 0.597 0.033 Uiso 1 1 calc R . . C9 C 0.4713(3) -0.13606(19) 0.5949(3) 0.0317(7) Uani 1 1 d . . . C10 C 0.4398(3) -0.0561(2) 0.6196(3) 0.0431(9) Uani 1 1 d . . . H10A H 0.4944 -0.0325 0.665 0.065 Uiso 1 1 calc R . . H10B H 0.3786 -0.0586 0.6498 0.065 Uiso 1 1 calc R . . H10C H 0.4263 -0.026 0.5597 0.065 Uiso 1 1 calc R . . C11 C 0.4895(3) -0.1856(2) 0.6875(3) 0.0403(9) Uani 1 1 d . . . H11A H 0.5024 -0.2377 0.6694 0.06 Uiso 1 1 calc R . . H11B H 0.4295 -0.1841 0.7197 0.06 Uiso 1 1 calc R . . H11C H 0.548 -0.1663 0.732 0.06 Uiso 1 1 calc R . . C12 C 0.3828(3) -0.1714(2) 0.5258(3) 0.0483(10) Uani 1 1 d . . . H12A H 0.3684 -0.141 0.4663 0.072 Uiso 1 1 calc R . . H12B H 0.3229 -0.1728 0.558 0.072 Uiso 1 1 calc R . . H12C H 0.4007 -0.2228 0.5091 0.072 Uiso 1 1 calc R . . C13 C 0.6518(3) -0.18494(19) 0.3040(2) 0.0398(9) Uani 1 1 d . . . C14 C 0.6001(5) -0.2620(2) 0.2896(3) 0.083(2) Uani 1 1 d . . . H14A H 0.5312 -0.2582 0.3044 0.125 Uiso 1 1 calc R . . H14B H 0.6383 -0.299 0.3333 0.125 Uiso 1 1 calc R . . H14C H 0.5977 -0.2783 0.2218 0.125 Uiso 1 1 calc R . . C15 C 0.5910(3) -0.1271(2) 0.2376(3) 0.0467(10) Uani 1 1 d . . . H15A H 0.5233 -0.1224 0.2554 0.07 Uiso 1 1 calc R . . H15B H 0.5853 -0.1438 0.1697 0.07 Uiso 1 1 calc R . . H15C H 0.6253 -0.0781 0.2452 0.07 Uiso 1 1 calc R . . C16 C 0.7571(4) -0.1914(3) 0.2736(3) 0.0562(12) Uani 1 1 d . . . H16A H 0.75 -0.209 0.2059 0.084 Uiso 1 1 calc R . . H16B H 0.7982 -0.2275 0.3163 0.084 Uiso 1 1 calc R . . H16C H 0.7901 -0.1419 0.2791 0.084 Uiso 1 1 calc R . . N20 N 0.86202(19) -0.01780(16) 0.66180(19) 0.0275(6) Uani 1 1 d . . . C21 C 0.9441(3) -0.0148(2) 0.7494(3) 0.0407(9) Uani 1 1 d . . . H21A H 0.9192 -0.0409 0.804 0.049 Uiso 1 1 calc R . . H21B H 0.9551 0.0388 0.7686 0.049 Uiso 1 1 calc R . . C22 C 1.0514(3) -0.0506(2) 0.7377(3) 0.0423(9) Uani 1 1 d . . . H22A H 1.0913 -0.0622 0.8022 0.051 Uiso 1 1 calc R . . H22B H 1.0424 -0.0975 0.6985 0.051 Uiso 1 1 calc R . . O23 O 1.0976(2) 0.00392(16) 0.6910(2) 0.0484(7) Uani 1 1 d . . . C24 C 1.1973(3) -0.0278(3) 0.6842(3) 0.0520(11) Uani 1 1 d . . . H24A H 1.2359 -0.0336 0.7498 0.078 Uiso 1 1 calc R . . H24B H 1.2334 0.0063 0.6461 0.078 Uiso 1 1 calc R . . H24C H 1.189 -0.0772 0.6521 0.078 Uiso 1 1 calc R . . C25 C 0.8806(3) 0.02648(19) 0.5764(3) 0.0350(8) Uani 1 1 d . . . H25A H 0.8204 0.0227 0.5251 0.042 Uiso 1 1 calc R . . H25B H 0.9382 0.0038 0.5502 0.042 Uiso 1 1 calc R . . C26 C 0.9030(3) 0.1087(2) 0.5975(3) 0.0467(10) Uani 1 1 d . . . H26A H 0.8423 0.1346 0.6135 0.056 Uiso 1 1 calc R . . H26B H 0.9582 0.1139 0.6536 0.056 Uiso 1 1 calc R . . O27 O 0.9312(3) 0.13957(15) 0.5157(2) 0.0598(9) Uani 1 1 d . . . C28 C 0.9520(4) 0.2188(2) 0.5277(4) 0.0694(15) Uani 1 1 d . . . H28A H 0.8906 0.2453 0.5385 0.104 Uiso 1 1 calc R . . H28B H 0.9746 0.2387 0.4689 0.104 Uiso 1 1 calc R . . H28C H 1.0052 0.2266 0.584 0.104 Uiso 1 1 calc R . . C31 C 0.7793(3) -0.14796(19) 0.8813(3) 0.0396(9) Uani 1 1 d . . . H31A H 0.7431 -0.1629 0.8172 0.059 Uiso 1 1 calc R . . H31B H 0.7704 -0.1869 0.9294 0.059 Uiso 1 1 calc R . . H31C H 0.8514 -0.1423 0.8779 0.059 Uiso 1 1 calc R . . C32 C 0.5901(3) -0.0665(2) 0.9233(3) 0.0444(10) Uani 1 1 d . . . H32A H 0.5649 -0.0202 0.9499 0.067 Uiso 1 1 calc R . . H32B H 0.5796 -0.1093 0.9652 0.067 Uiso 1 1 calc R . . H32C H 0.5534 -0.0753 0.8574 0.067 Uiso 1 1 calc R . . C33 C 0.7956(4) -0.0437(2) 1.0467(3) 0.0499(11) Uani 1 1 d . . . H33A H 0.8685 -0.0403 1.0462 0.075 Uiso 1 1 calc R . . H33B H 0.7814 -0.0869 1.0863 0.075 Uiso 1 1 calc R . . H33C H 0.7723 0.0028 1.0743 0.075 Uiso 1 1 calc R . . C34 C 0.7522(4) 0.1873(2) 0.8030(3) 0.0455(10) Uani 1 1 d . . . H34A H 0.8034 0.1816 0.7603 0.068 Uiso 1 1 calc R . . H34B H 0.76 0.2367 0.835 0.068 Uiso 1 1 calc R . . H34C H 0.6847 0.1836 0.7641 0.068 Uiso 1 1 calc R . . C35 C 0.9010(3) 0.1216(2) 0.9638(3) 0.0417(9) Uani 1 1 d . . . H35A H 0.9135 0.0839 1.0159 0.063 Uiso 1 1 calc R . . H35B H 0.9099 0.1723 0.9921 0.063 Uiso 1 1 calc R . . H35C H 0.9488 0.1141 0.9181 0.063 Uiso 1 1 calc R . . C36 C 0.6766(3) 0.1360(2) 0.9814(3) 0.0413(9) Uani 1 1 d . . . H36A H 0.6075 0.1323 0.9459 0.062 Uiso 1 1 calc R . . H36B H 0.6894 0.1877 1.0053 0.062 Uiso 1 1 calc R . . H36C H 0.685 0.101 1.0367 0.062 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 Ge1 0.01954(17) 0.02169(17) 0.01705(16) -0.00043(12) 0.00379(11) -0.00031(12) Si1 0.0413(5) 0.0228(4) 0.0194(4) -0.0005(3) 0.0095(4) -0.0008(4) Si2 0.0318(5) 0.0222(4) 0.0232(4) -0.0070(3) 0.0084(4) -0.0024(3) N1 0.0274(13) 0.0203(12) 0.0144(12) -0.0023(10) 0.0056(10) 0.0004(10) O1 0.0259(11) 0.0236(10) 0.0176(10) -0.0042(8) 0.0067(8) -0.0018(8) C2 0.0315(16) 0.0154(13) 0.0179(14) 0.0020(11) 0.0056(12) 0.0027(11) C3 0.0306(17) 0.0168(14) 0.0263(16) 0.0007(12) 0.0028(13) -0.0034(12) C4 0.042(2) 0.0193(15) 0.0282(17) -0.0028(13) -0.0007(15) -0.0070(13) C5 0.057(2) 0.0158(15) 0.0181(15) -0.0020(12) 0.0053(15) 0.0004(14) C6 0.0427(19) 0.0187(15) 0.0228(16) -0.0008(12) 0.0124(14) 0.0045(13) C7 0.0289(16) 0.0180(14) 0.0219(15) 0.0010(12) 0.0056(12) 0.0048(11) C8 0.0258(16) 0.0370(18) 0.0215(15) 0.0003(14) 0.0071(13) 0.0103(13) C9 0.0301(18) 0.0280(17) 0.0366(19) -0.0025(14) 0.0045(14) -0.0086(13) C10 0.0266(18) 0.041(2) 0.063(3) -0.0077(19) 0.0135(18) -0.0027(15) C11 0.047(2) 0.037(2) 0.040(2) -0.0025(17) 0.0168(17) -0.0158(17) C12 0.038(2) 0.052(2) 0.052(3) -0.002(2) -0.0013(18) -0.0199(18) C13 0.078(3) 0.0226(17) 0.0180(16) -0.0035(13) 0.0061(17) -0.0023(17) C14 0.183(6) 0.037(2) 0.030(2) -0.0143(19) 0.021(3) -0.038(3) C15 0.069(3) 0.043(2) 0.0260(19) -0.0025(17) 0.0009(18) -0.0078(19) C16 0.096(4) 0.050(3) 0.0240(19) -0.0101(18) 0.014(2) 0.023(2) N20 0.0174(13) 0.0448(17) 0.0211(13) -0.0094(12) 0.0053(10) -0.0028(11) C21 0.0252(18) 0.070(3) 0.0263(18) -0.0106(18) 0.0013(14) -0.0019(17) C22 0.058(3) 0.0351(19) 0.0291(19) 0.0073(16) -0.0078(17) -0.0196(17) O23 0.0506(17) 0.0448(15) 0.0492(17) 0.0067(13) 0.0059(14) -0.0021(13) C24 0.028(2) 0.078(3) 0.050(2) -0.011(2) 0.0056(18) 0.0072(19) C25 0.042(2) 0.0388(19) 0.0295(18) -0.0092(15) 0.0213(15) -0.0170(15) C26 0.060(3) 0.043(2) 0.045(2) -0.0137(18) 0.033(2) -0.0185(19) O27 0.089(2) 0.0338(15) 0.066(2) 0.0087(14) 0.0402(18) -0.0075(15) C28 0.085(4) 0.030(2) 0.106(4) 0.022(2) 0.052(3) 0.000(2) C31 0.060(3) 0.0270(18) 0.0317(19) 0.0045(15) 0.0079(17) 0.0099(16) C32 0.057(3) 0.032(2) 0.051(2) -0.0031(17) 0.030(2) -0.0083(17) C33 0.081(3) 0.044(2) 0.0222(18) 0.0039(17) 0.0035(19) -0.003(2) C34 0.077(3) 0.0203(17) 0.039(2) -0.0032(15) 0.010(2) -0.0019(17) C35 0.039(2) 0.047(2) 0.039(2) -0.0135(18) 0.0072(17) -0.0115(17) C36 0.046(2) 0.041(2) 0.041(2) -0.0187(17) 0.0186(18) -0.0021(17) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 O1 1.876(2) . ? Ge1 N1 1.901(2) . ? Ge1 N20 2.319(3) . ? Si1 N1 1.755(3) . ? Si1 C32 1.868(4) . ? Si1 C31 1.871(3) . ? Si1 C33 1.880(4) . ? Si2 N1 1.749(2) . ? Si2 C34 1.870(4) . ? Si2 C35 1.875(4) . ? Si2 C36 1.879(4) . ? O1 C2 1.365(3) . ? C2 C7 1.397(4) . ? C2 C3 1.417(4) . ? C3 C4 1.395(4) . ? C3 C9 1.534(5) . ? C4 C5 1.398(5) . ? C4 H4 0.95 . ? C5 C6 1.388(5) . ? C5 C13 1.540(4) . ? C6 C7 1.401(4) . ? C6 H6 0.95 . ? C7 C8 1.499(4) . ? C8 N20 1.489(4) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 C10 1.532(5) . ? C9 C12 1.536(5) . ? C9 C11 1.543(5) . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 C15 1.525(5) . ? C13 C14 1.530(5) . ? C13 C16 1.541(6) . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? N20 C25 1.476(4) . ? N20 C21 1.507(4) . ? C21 C22 1.603(6) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 O23 1.366(4) . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? O23 C24 1.466(5) . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 C26 1.506(5) . ? C25 H25A 0.99 . ? C25 H25B 0.99 . ? C26 O27 1.368(4) . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? O27 C28 1.436(5) . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C31 H31A 0.98 . ? C31 H31B 0.98 . ? C31 H31C 0.98 . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? C33 H33A 0.98 . ? C33 H33B 0.98 . ? C33 H33C 0.98 . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ge1 N1 96.35(9) . . ? O1 Ge1 N20 88.33(9) . . ? N1 Ge1 N20 100.39(10) . . ? N1 Si1 C32 109.62(16) . . ? N1 Si1 C31 115.31(15) . . ? C32 Si1 C31 109.56(18) . . ? N1 Si1 C33 111.31(16) . . ? C32 Si1 C33 108.0(2) . . ? C31 Si1 C33 102.65(19) . . ? N1 Si2 C34 111.75(15) . . ? N1 Si2 C35 111.99(15) . . ? C34 Si2 C35 105.67(19) . . ? N1 Si2 C36 112.91(15) . . ? C34 Si2 C36 104.51(19) . . ? C35 Si2 C36 109.52(17) . . ? Si2 N1 Si1 120.04(14) . . ? Si2 N1 Ge1 114.25(13) . . ? Si1 N1 Ge1 123.58(13) . . ? C2 O1 Ge1 114.49(17) . . ? O1 C2 C7 117.9(3) . . ? O1 C2 C3 122.1(3) . . ? C7 C2 C3 120.0(3) . . ? C4 C3 C2 116.6(3) . . ? C4 C3 C9 122.3(3) . . ? C2 C3 C9 121.0(3) . . ? C3 C4 C5 124.6(3) . . ? C3 C4 H4 117.7 . . ? C5 C4 H4 117.7 . . ? C6 C5 C4 117.0(3) . . ? C6 C5 C13 123.3(3) . . ? C4 C5 C13 119.8(3) . . ? C5 C6 C7 121.0(3) . . ? C5 C6 H6 119.5 . . ? C7 C6 H6 119.5 . . ? C2 C7 C6 120.6(3) . . ? C2 C7 C8 117.9(3) . . ? C6 C7 C8 121.3(3) . . ? N20 C8 C7 114.1(2) . . ? N20 C8 H8A 108.7 . . ? C7 C8 H8A 108.7 . . ? N20 C8 H8B 108.7 . . ? C7 C8 H8B 108.7 . . ? H8A C8 H8B 107.6 . . ? C10 C9 C3 110.1(3) . . ? C10 C9 C12 107.7(3) . . ? C3 C9 C12 112.1(3) . . ? C10 C9 C11 110.6(3) . . ? C3 C9 C11 109.3(3) . . ? C12 C9 C11 107.0(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C15 C13 C14 109.4(4) . . ? C15 C13 C5 109.5(3) . . ? C14 C13 C5 110.0(3) . . ? C15 C13 C16 108.0(3) . . ? C14 C13 C16 108.2(4) . . ? C5 C13 C16 111.7(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C25 N20 C8 107.8(2) . . ? C25 N20 C21 115.8(3) . . ? C8 N20 C21 108.3(3) . . ? C25 N20 Ge1 108.7(2) . . ? C8 N20 Ge1 106.94(18) . . ? C21 N20 Ge1 109.00(19) . . ? N20 C21 C22 117.1(3) . . ? N20 C21 H21A 108 . . ? C22 C21 H21A 108 . . ? N20 C21 H21B 108 . . ? C22 C21 H21B 108 . . ? H21A C21 H21B 107.3 . . ? O23 C22 C21 104.5(3) . . ? O23 C22 H22A 110.8 . . ? C21 C22 H22A 110.9 . . ? O23 C22 H22B 110.8 . . ? C21 C22 H22B 110.9 . . ? H22A C22 H22B 108.9 . . ? C22 O23 C24 104.3(3) . . ? O23 C24 H24A 109.5 . . ? O23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N20 C25 C26 114.3(3) . . ? N20 C25 H25A 108.7 . . ? C26 C25 H25A 108.7 . . ? N20 C25 H25B 108.7 . . ? C26 C25 H25B 108.7 . . ? H25A C25 H25B 107.6 . . ? O27 C26 C25 107.3(3) . . ? O27 C26 H26A 110.3 . . ? C25 C26 H26A 110.2 . . ? O27 C26 H26B 110.2 . . ? C25 C26 H26B 110.2 . . ? H26A C26 H26B 108.5 . . ? C26 O27 C28 111.6(3) . . ? O27 C28 H28A 109.5 . . ? O27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si1 C31 H31A 109.5 . . ? Si1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si1 C32 H32A 109.5 . . ? Si1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si1 C33 H33A 109.5 . . ? Si1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? 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 . . ? 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 C34 Si2 N1 Si1 -164.6(2) . . . . ? C35 Si2 N1 Si1 77.1(2) . . . . ? C36 Si2 N1 Si1 -47.1(2) . . . . ? C34 Si2 N1 Ge1 -0.6(2) . . . . ? C35 Si2 N1 Ge1 -118.96(18) . . . . ? C36 Si2 N1 Ge1 116.85(18) . . . . ? C32 Si1 N1 Si2 90.3(2) . . . . ? C31 Si1 N1 Si2 -145.53(19) . . . . ? C33 Si1 N1 Si2 -29.1(2) . . . . ? C32 Si1 N1 Ge1 -72.1(2) . . . . ? C31 Si1 N1 Ge1 52.0(2) . . . . ? C33 Si1 N1 Ge1 168.44(19) . . . . ? O1 Ge1 N1 Si2 -166.13(13) . . . . ? N20 Ge1 N1 Si2 104.41(14) . . . . ? O1 Ge1 N1 Si1 -2.79(17) . . . . ? N20 Ge1 N1 Si1 -92.26(17) . . . . ? N1 Ge1 O1 C2 -161.5(2) . . . . ? N20 Ge1 O1 C2 -61.2(2) . . . . ? Ge1 O1 C2 C7 61.9(3) . . . . ? Ge1 O1 C2 C3 -119.3(3) . . . . ? O1 C2 C3 C4 175.9(3) . . . . ? C7 C2 C3 C4 -5.3(4) . . . . ? O1 C2 C3 C9 -5.7(4) . . . . ? C7 C2 C3 C9 173.1(3) . . . . ? C2 C3 C4 C5 1.6(5) . . . . ? C9 C3 C4 C5 -176.8(3) . . . . ? C3 C4 C5 C6 2.5(5) . . . . ? C3 C4 C5 C13 -177.6(3) . . . . ? C4 C5 C6 C7 -3.1(4) . . . . ? C13 C5 C6 C7 177.1(3) . . . . ? O1 C2 C7 C6 -176.3(3) . . . . ? C3 C2 C7 C6 4.9(4) . . . . ? O1 C2 C7 C8 9.7(4) . . . . ? C3 C2 C7 C8 -169.2(3) . . . . ? C5 C6 C7 C2 -0.5(4) . . . . ? C5 C6 C7 C8 173.3(3) . . . . ? C2 C7 C8 N20 -69.0(4) . . . . ? C6 C7 C8 N20 117.0(3) . . . . ? C4 C3 C9 C10 -117.3(3) . . . . ? C2 C3 C9 C10 64.4(4) . . . . ? C4 C3 C9 C12 2.6(4) . . . . ? C2 C3 C9 C12 -175.7(3) . . . . ? C4 C3 C9 C11 121.0(3) . . . . ? C2 C3 C9 C11 -57.2(4) . . . . ? C6 C5 C13 C15 -113.7(4) . . . . ? C4 C5 C13 C15 66.5(4) . . . . ? C6 C5 C13 C14 126.0(4) . . . . ? C4 C5 C13 C14 -53.8(5) . . . . ? C6 C5 C13 C16 5.8(4) . . . . ? C4 C5 C13 C16 -174.0(3) . . . . ? C7 C8 N20 C25 -71.0(3) . . . . ? C7 C8 N20 C21 163.0(3) . . . . ? C7 C8 N20 Ge1 45.7(3) . . . . ? O1 Ge1 N20 C25 124.3(2) . . . . ? N1 Ge1 N20 C25 -139.5(2) . . . . ? O1 Ge1 N20 C8 8.24(19) . . . . ? N1 Ge1 N20 C8 104.39(19) . . . . ? O1 Ge1 N20 C21 -108.6(2) . . . . ? N1 Ge1 N20 C21 -12.4(2) . . . . ? C25 N20 C21 C22 -65.0(4) . . . . ? C8 N20 C21 C22 56.1(4) . . . . ? Ge1 N20 C21 C22 172.1(3) . . . . ? N20 C21 C22 O23 80.4(4) . . . . ? C21 C22 O23 C24 177.6(3) . . . . ? C8 N20 C25 C26 -176.5(3) . . . . ? C21 N20 C25 C26 -55.1(4) . . . . ? Ge1 N20 C25 C26 67.9(3) . . . . ? N20 C25 C26 O27 172.2(3) . . . . ? C25 C26 O27 C28 178.6(4) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 942087' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_WLF01503 _audit_creation_date 2013-01-24T13:37:43-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C27 H54 N2 O3 Pb1 Si2' _chemical_formula_sum 'C27 H54 N2 O3 Pb Si2' _chemical_formula_weight 718.09 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5521(10) _cell_length_b 13.7269(13) _cell_length_c 15.0466(12) _cell_angle_alpha 64.082(3) _cell_angle_beta 69.863(3) _cell_angle_gamma 81.892(3) _cell_volume 1840.3(3) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 2459 _cell_measurement_theta_min 2.62 _cell_measurement_theta_max 21.57 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.1 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.1 _exptl_crystal_density_diffrn 1.296 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 728 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.673 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.385 _exptl_absorpt_correction_T_max 0.627 #----------------------------------------------------------------------------# # SQUEEZE RESULTS # #----------------------------------------------------------------------------# # Note: Data are Listed for all Voids in the P1 Unit Cell # i.e. Centre of Gravity, Solvent Accessible Volume, # Recovered number of Electrons in the Void and # Details about the Squeezed Material loop_ _platon_squeeze_void_nr _platon_squeeze_void_average_x _platon_squeeze_void_average_y _platon_squeeze_void_average_z _platon_squeeze_void_volume _platon_squeeze_void_count_electrons _platon_squeeze_void_content 1 0.500 0.000 0.500 263 50 ' ' _platon_squeeze_details ; ; #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.052 _diffrn_reflns_av_unetI/netI 0.0926 _diffrn_reflns_number 17711 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.973 _diffrn_measured_fraction_theta_max 0.973 _reflns_number_total 8232 _reflns_number_gt 6343 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0557P)^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_number_reflns 8232 _refine_ls_number_parameters 330 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0693 _refine_ls_R_factor_gt 0.0499 _refine_ls_wR_factor_ref 0.1172 _refine_ls_wR_factor_gt 0.1108 _refine_ls_goodness_of_fit_ref 0.998 _refine_ls_restrained_S_all 0.998 _refine_ls_shift/su_max 0.015 _refine_ls_shift/su_mean 0 _refine_diff_density_max 2.093 _refine_diff_density_min -2.096 _refine_diff_density_rms 0.174 _iucr_refine_instructions_details ; .res file for SHELXL : WLF01503.res ................................................................. TITL import in P -1 CELL 0.71073 10.5521 13.7269 15.0466 64.082 69.863 81.892 ZERR 2.00 0.0010 0.0013 0.0012 0.003 0.003 0.003 LATT 1 SFAC C H N O SI PB UNIT 54 108 4 6 4 2 MERG 2 FREE C14 C15 FMAP 2 PLAN 20 ACTA BOND $H CONF LIST 4 WPDB -2 L.S. 4 TEMP -123.00 WGHT 0.055700 FVAR 4.04690 O1 4 1.084004 -0.040454 0.260205 11.00000 0.02941 0.01983 = 0.03323 -0.01151 -0.01337 0.00186 C2 1 0.987581 -0.109246 0.282877 11.00000 0.02851 0.02290 = 0.02120 -0.01402 -0.00874 0.00701 C3 1 0.964372 -0.209859 0.368234 11.00000 0.03187 0.02910 = 0.02898 -0.02015 -0.00889 0.00766 C4 1 0.863226 -0.277668 0.384607 11.00000 0.03863 0.02293 = 0.02459 -0.01380 -0.00222 0.00150 AFIX 43 H4 2 0.848513 -0.346415 0.442455 11.00000 -1.20000 AFIX 0 C5 1 0.782665 -0.249150 0.319910 11.00000 0.02762 0.02253 = 0.02582 -0.01405 -0.00513 0.00060 C6 1 0.806868 -0.148842 0.237166 11.00000 0.02796 0.03083 = 0.02848 -0.01823 -0.00801 0.00009 AFIX 43 H6 2 0.753042 -0.126176 0.192444 11.00000 -1.20000 AFIX 0 C7 1 0.907693 -0.079431 0.216812 11.00000 0.02473 0.02915 = 0.02121 -0.01410 -0.00359 0.00178 C8 1 0.934228 0.027972 0.119777 11.00000 0.02117 0.02894 = 0.02472 -0.01281 -0.00849 0.00484 AFIX 23 H8A 2 1.032153 0.035182 0.081203 11.00000 -1.20000 H8B 2 0.886855 0.026652 0.073812 11.00000 -1.20000 AFIX 0 C9 1 1.051654 -0.249931 0.440141 11.00000 0.04686 0.02934 = 0.03684 -0.01921 -0.02052 0.00755 C10 1 1.044241 -0.171091 0.491918 11.00000 0.07999 0.03507 = 0.05651 -0.02609 -0.04348 0.01838 AFIX 137 H10A 2 1.067748 -0.097426 0.437639 11.00000 -1.50000 H10B 2 1.107882 -0.194394 0.531701 11.00000 -1.50000 H10C 2 0.952458 -0.172147 0.538796 11.00000 -1.50000 AFIX 0 C11 1 1.198338 -0.260358 0.379546 11.00000 0.04783 0.04882 = 0.04856 -0.02180 -0.02751 0.01250 AFIX 137 H11A 2 1.206920 -0.322986 0.362914 11.00000 -1.50000 H11B 2 1.255801 -0.270279 0.421948 11.00000 -1.50000 H11C 2 1.226517 -0.194507 0.314851 11.00000 -1.50000 AFIX 0 C12 1 1.004300 -0.359939 0.533144 11.00000 0.07220 0.03200 = 0.05614 -0.01176 -0.04287 0.01258 AFIX 137 H12A 2 0.908643 -0.356056 0.570832 11.00000 -1.50000 H12B 2 1.057599 -0.377399 0.580096 11.00000 -1.50000 H12C 2 1.016529 -0.416356 0.507677 11.00000 -1.50000 AFIX 0 C13 1 0.676565 -0.328546 0.341929 11.00000 0.04211 0.03282 = 0.04209 -0.00901 -0.01088 -0.01312 C14 1 0.566793 -0.349264 0.444859 11.00000 0.07570 0.07899 = 0.12011 -0.05843 0.00618 -0.02579 AFIX 137 H14A 2 0.524128 -0.280644 0.443523 11.00000 -1.50000 H14B 2 0.606373 -0.381635 0.501520 11.00000 -1.50000 H14C 2 0.498848 -0.398918 0.456133 11.00000 -1.50000 AFIX 0 C15 1 0.588042 -0.280511 0.274546 11.00000 0.07101 0.05644 = 0.22230 -0.02145 -0.08955 -0.01510 AFIX 137 H15A 2 0.642269 -0.262382 0.201710 11.00000 -1.50000 H15B 2 0.546411 -0.214695 0.281616 11.00000 -1.50000 H15C 2 0.517342 -0.332926 0.296084 11.00000 -1.50000 AFIX 0 C16 1 0.733705 -0.429082 0.339494 11.00000 0.06205 0.05560 = 0.18326 -0.07312 -0.03262 0.00144 AFIX 137 H16A 2 0.664052 -0.473043 0.344265 11.00000 -1.50000 H16B 2 0.768313 -0.468434 0.398441 11.00000 -1.50000 H16C 2 0.807730 -0.414353 0.274112 11.00000 -1.50000 AFIX 0 N20 3 0.888996 0.125415 0.143566 11.00000 0.01739 0.02595 = 0.03229 -0.01654 -0.00705 0.00114 C21 1 0.741123 0.117762 0.198339 11.00000 0.01962 0.04060 = 0.04369 -0.02238 -0.00698 -0.00048 AFIX 23 H21A 2 0.722887 0.052986 0.265640 11.00000 -1.20000 H21B 2 0.695620 0.106073 0.156143 11.00000 -1.20000 AFIX 0 C22 1 0.678785 0.212885 0.219421 11.00000 0.03104 0.03333 = 0.05809 -0.02784 -0.01219 0.00639 AFIX 23 H22A 2 0.686690 0.277226 0.152858 11.00000 -1.20000 H22B 2 0.581768 0.198179 0.259673 11.00000 -1.20000 AFIX 0 O23 4 0.744996 0.232808 0.276108 11.00000 0.03242 0.04268 = 0.05323 -0.03164 -0.00881 0.00673 C24 1 0.680731 0.313894 0.310952 11.00000 0.05826 0.04058 = 0.04463 -0.02848 0.00136 0.00239 AFIX 137 H24A 2 0.678904 0.381868 0.250699 11.00000 -1.50000 H24B 2 0.730892 0.325010 0.349860 11.00000 -1.50000 H24C 2 0.588151 0.290631 0.356288 11.00000 -1.50000 AFIX 0 C25 1 0.932587 0.225291 0.045890 11.00000 0.03133 0.01873 = 0.02655 -0.00874 -0.00700 -0.00218 AFIX 23 H25A 2 1.032484 0.227331 0.019408 11.00000 -1.20000 H25B 2 0.902807 0.288578 0.062848 11.00000 -1.20000 AFIX 0 C26 1 0.880884 0.237692 -0.040868 11.00000 0.03973 0.02183 = 0.03846 -0.00950 -0.01420 -0.00186 AFIX 23 H26A 2 0.933218 0.191763 -0.076328 11.00000 -1.20000 H26B 2 0.784634 0.215683 -0.012359 11.00000 -1.20000 AFIX 0 O27 4 0.896204 0.345141 -0.109671 11.00000 0.08442 0.03370 = 0.04226 -0.01280 -0.03539 0.00186 C28 1 0.861439 0.369051 -0.201461 11.00000 0.08042 0.04055 = 0.03157 -0.01306 -0.02595 0.00651 AFIX 137 H28A 2 0.919950 0.328194 -0.239359 11.00000 -1.50000 H28B 2 0.873656 0.446789 -0.246366 11.00000 -1.50000 H28C 2 0.767023 0.348464 -0.181205 11.00000 -1.50000 AFIX 0 N31 3 1.200515 0.207335 0.133007 11.00000 0.02457 0.03267 = 0.03066 -0.01495 -0.00271 -0.00468 C32 1 1.037446 0.381454 0.180401 11.00000 0.04503 0.02793 = 0.05752 -0.02211 -0.02392 0.00558 AFIX 137 H32A 2 0.966492 0.363238 0.161764 11.00000 -1.50000 H32B 2 1.037583 0.459636 0.160452 11.00000 -1.50000 H32C 2 1.020384 0.342539 0.255754 11.00000 -1.50000 AFIX 0 C33 1 1.243047 0.437761 -0.027676 11.00000 0.06515 0.04285 = 0.05978 -0.00795 -0.00536 0.00562 AFIX 137 H33A 2 1.337751 0.430664 -0.065369 11.00000 -1.50000 H33B 2 1.227161 0.511804 -0.032695 11.00000 -1.50000 H33C 2 1.184652 0.422010 -0.058364 11.00000 -1.50000 AFIX 0 C34 1 1.330674 0.367670 0.161220 11.00000 0.05764 0.05396 = 0.12609 -0.06065 -0.04299 0.00550 AFIX 137 H34A 2 1.309838 0.320644 0.235763 11.00000 -1.50000 H34B 2 1.325891 0.443633 0.150597 11.00000 -1.50000 H34C 2 1.421787 0.352379 0.123667 11.00000 -1.50000 AFIX 0 C35 1 1.485618 0.228259 -0.010387 11.00000 0.02312 0.06961 = 0.06385 -0.03442 -0.00727 -0.00341 AFIX 137 H35A 2 1.459523 0.276830 -0.071861 11.00000 -1.50000 H35B 2 1.562142 0.184281 -0.030316 11.00000 -1.50000 H35C 2 1.511590 0.271228 0.018362 11.00000 -1.50000 AFIX 0 C36 1 1.397490 0.040040 0.202283 11.00000 0.03288 0.04795 = 0.05688 -0.02506 -0.02168 0.00315 AFIX 137 H36A 2 1.415418 0.079569 0.237502 11.00000 -1.50000 H36B 2 1.480447 0.005213 0.175967 11.00000 -1.50000 H36C 2 1.327605 -0.015298 0.251694 11.00000 -1.50000 AFIX 0 C37 1 1.304820 0.056707 0.025597 11.00000 0.02560 0.05682 = 0.04369 -0.03181 -0.00912 0.00159 AFIX 137 H37A 2 1.257103 -0.010882 0.078840 11.00000 -1.50000 H37B 2 1.390748 0.039999 -0.017397 11.00000 -1.50000 H37C 2 1.249260 0.099704 -0.018511 11.00000 -1.50000 AFIX 0 SI1 5 1.204608 0.341407 0.110466 11.00000 0.03183 0.02801 = 0.05000 -0.01532 -0.01416 -0.00327 SI2 5 1.338376 0.136593 0.091088 11.00000 0.02264 0.04044 = 0.03824 -0.02050 -0.00925 0.00186 PB1 6 1.015653 0.119542 0.261748 11.00000 0.02896 0.02666 = 0.02625 -0.01478 -0.00823 0.00025 HKLF 4 REM import in P -1 REM R1 = 0.0499 for 6343 Fo > 4sig(Fo) and 0.0693 for all 8232 data REM 330 parameters refined using 0 restraints END WGHT 0.0557 0.0000 REM Highest difference peak 2.09, deepest hole -2.10, 1-sigma level 0.17 Q1 1 1.0253 0.1770 0.1931 11.00000 0.05 2.09 Q2 1 1.0051 0.0751 0.3391 11.00000 0.05 1.96 Q3 1 1.0264 0.1532 0.3087 11.00000 0.05 1.05 Q4 1 0.7427 -0.3602 0.2288 11.00000 0.05 1.03 Q5 1 0.5611 -0.2985 0.3549 11.00000 0.05 0.97 Q6 1 1.0245 0.0968 0.2084 11.00000 0.05 0.92 Q7 1 0.6877 -0.4416 0.4333 11.00000 0.05 0.91 Q8 1 1.3260 0.0769 0.1594 11.00000 0.05 0.69 Q9 1 1.0483 0.1135 0.2575 11.00000 0.05 0.68 Q10 1 0.7969 0.3131 -0.0833 11.00000 0.05 0.67 Q11 1 0.8670 -0.4588 0.5923 11.00000 0.05 0.63 Q12 1 0.8879 0.0708 0.3235 11.00000 0.05 0.63 Q13 1 1.2196 0.2845 0.0622 11.00000 0.05 0.61 Q14 1 0.9617 -0.1736 0.6506 11.00000 0.05 0.58 Q15 1 1.2175 -0.2590 0.2720 11.00000 0.05 0.58 Q16 1 1.1398 0.1746 0.2063 11.00000 0.05 0.57 Q17 1 1.1204 0.1153 0.1793 11.00000 0.05 0.57 Q18 1 0.9035 0.4020 -0.2751 11.00000 0.05 0.57 Q19 1 0.4654 0.0002 0.4822 11.00000 0.05 0.56 Q20 1 1.0549 -0.2292 0.4598 11.00000 0.05 0.56 ; #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group O1 O 1.0840(4) -0.0405(3) 0.2602(3) 0.0265(10) Uani 1 1 d . . . C2 C 0.9876(6) -0.1092(5) 0.2829(5) 0.0229(13) Uani 1 1 d . . . C3 C 0.9644(7) -0.2099(5) 0.3682(5) 0.0280(15) Uani 1 1 d . . . C4 C 0.8632(7) -0.2777(5) 0.3846(5) 0.0296(15) Uani 1 1 d . . . H4 H 0.8485 -0.3464 0.4425 0.036 Uiso 1 1 calc R . . C5 C 0.7827(6) -0.2491(5) 0.3199(5) 0.0248(14) Uani 1 1 d . . . C6 C 0.8069(7) -0.1488(5) 0.2372(5) 0.0271(14) Uani 1 1 d . . . H6 H 0.753 -0.1262 0.1924 0.033 Uiso 1 1 calc R . . C7 C 0.9077(6) -0.0794(5) 0.2168(5) 0.0249(14) Uani 1 1 d . . . C8 C 0.9342(6) 0.0280(5) 0.1198(5) 0.0245(14) Uani 1 1 d . . . H8A H 1.0322 0.0352 0.0812 0.029 Uiso 1 1 calc R . . H8B H 0.8869 0.0267 0.0738 0.029 Uiso 1 1 calc R . . C9 C 1.0517(8) -0.2499(5) 0.4401(5) 0.0344(16) Uani 1 1 d . . . C10 C 1.0442(9) -0.1711(6) 0.4919(6) 0.050(2) Uani 1 1 d . . . H10A H 1.0677 -0.0974 0.4376 0.075 Uiso 1 1 calc R . . H10B H 1.1079 -0.1944 0.5317 0.075 Uiso 1 1 calc R . . H10C H 0.9525 -0.1721 0.5388 0.075 Uiso 1 1 calc R . . C11 C 1.1983(8) -0.2604(6) 0.3795(6) 0.046(2) Uani 1 1 d . . . H11A H 1.2069 -0.323 0.3629 0.069 Uiso 1 1 calc R . . H11B H 1.2558 -0.2703 0.4219 0.069 Uiso 1 1 calc R . . H11C H 1.2265 -0.1945 0.3149 0.069 Uiso 1 1 calc R . . C12 C 1.0043(9) -0.3599(6) 0.5331(6) 0.051(2) Uani 1 1 d . . . H12A H 0.9086 -0.3561 0.5708 0.076 Uiso 1 1 calc R . . H12B H 1.0576 -0.3774 0.5801 0.076 Uiso 1 1 calc R . . H12C H 1.0165 -0.4164 0.5077 0.076 Uiso 1 1 calc R . . C13 C 0.6766(8) -0.3285(6) 0.3419(6) 0.0407(18) Uani 1 1 d . . . C14 C 0.5668(11) -0.3493(9) 0.4449(9) 0.093(4) Uani 1 1 d . . . H14A H 0.5241 -0.2806 0.4435 0.139 Uiso 1 1 calc R . . H14B H 0.6064 -0.3816 0.5015 0.139 Uiso 1 1 calc R . . H14C H 0.4988 -0.3989 0.4561 0.139 Uiso 1 1 calc R . . C15 C 0.5880(11) -0.2805(8) 0.2745(12) 0.116(5) Uani 1 1 d . . . H15A H 0.6423 -0.2624 0.2017 0.175 Uiso 1 1 calc R . . H15B H 0.5464 -0.2147 0.2816 0.175 Uiso 1 1 calc R . . H15C H 0.5173 -0.3329 0.2961 0.175 Uiso 1 1 calc R . . C16 C 0.7337(11) -0.4291(8) 0.3395(10) 0.093(4) Uani 1 1 d . . . H16A H 0.6641 -0.473 0.3443 0.14 Uiso 1 1 calc R . . H16B H 0.7683 -0.4684 0.3984 0.14 Uiso 1 1 calc R . . H16C H 0.8077 -0.4144 0.2741 0.14 Uiso 1 1 calc R . . N20 N 0.8890(5) 0.1254(4) 0.1436(4) 0.0239(11) Uani 1 1 d . . . C21 C 0.7411(7) 0.1178(6) 0.1983(6) 0.0336(16) Uani 1 1 d . . . H21A H 0.7229 0.053 0.2656 0.04 Uiso 1 1 calc R . . H21B H 0.6956 0.1061 0.1561 0.04 Uiso 1 1 calc R . . C22 C 0.6788(7) 0.2129(6) 0.2194(6) 0.0387(18) Uani 1 1 d . . . H22A H 0.6867 0.2772 0.1529 0.046 Uiso 1 1 calc R . . H22B H 0.5818 0.1982 0.2597 0.046 Uiso 1 1 calc R . . O23 O 0.7450(5) 0.2328(4) 0.2761(4) 0.0404(12) Uani 1 1 d . . . C24 C 0.6807(9) 0.3139(6) 0.3110(6) 0.049(2) Uani 1 1 d . . . H24A H 0.6789 0.3819 0.2507 0.074 Uiso 1 1 calc R . . H24B H 0.7309 0.325 0.3499 0.074 Uiso 1 1 calc R . . H24C H 0.5882 0.2906 0.3563 0.074 Uiso 1 1 calc R . . C25 C 0.9326(7) 0.2253(5) 0.0459(5) 0.0262(14) Uani 1 1 d . . . H25A H 1.0325 0.2273 0.0194 0.031 Uiso 1 1 calc R . . H25B H 0.9028 0.2886 0.0628 0.031 Uiso 1 1 calc R . . C26 C 0.8809(7) 0.2377(5) -0.0409(5) 0.0338(16) Uani 1 1 d . . . H26A H 0.9332 0.1918 -0.0763 0.041 Uiso 1 1 calc R . . H26B H 0.7846 0.2157 -0.0124 0.041 Uiso 1 1 calc R . . O27 O 0.8962(6) 0.3451(4) -0.1097(4) 0.0504(15) Uani 1 1 d . . . C28 C 0.8614(9) 0.3691(6) -0.2015(6) 0.050(2) Uani 1 1 d . . . H28A H 0.9199 0.3282 -0.2394 0.075 Uiso 1 1 calc R . . H28B H 0.8737 0.4468 -0.2464 0.075 Uiso 1 1 calc R . . H28C H 0.767 0.3485 -0.1812 0.075 Uiso 1 1 calc R . . N31 N 1.2005(5) 0.2073(4) 0.1330(4) 0.0298(13) Uani 1 1 d . . . C32 C 1.0374(8) 0.3815(6) 0.1804(6) 0.0403(18) Uani 1 1 d . . . H32A H 0.9665 0.3632 0.1618 0.06 Uiso 1 1 calc R . . H32B H 1.0376 0.4596 0.1605 0.06 Uiso 1 1 calc R . . H32C H 1.0204 0.3425 0.2558 0.06 Uiso 1 1 calc R . . C33 C 1.2430(10) 0.4378(7) -0.0277(7) 0.066(3) Uani 1 1 d . . . H33A H 1.3378 0.4307 -0.0654 0.099 Uiso 1 1 calc R . . H33B H 1.2272 0.5118 -0.0327 0.099 Uiso 1 1 calc R . . H33C H 1.1847 0.422 -0.0584 0.099 Uiso 1 1 calc R . . C34 C 1.3307(9) 0.3677(7) 0.1612(9) 0.067(3) Uani 1 1 d . . . H34A H 1.3098 0.3206 0.2358 0.101 Uiso 1 1 calc R . . H34B H 1.3259 0.4436 0.1506 0.101 Uiso 1 1 calc R . . H34C H 1.4218 0.3524 0.1237 0.101 Uiso 1 1 calc R . . C35 C 1.4856(7) 0.2283(7) -0.0104(6) 0.051(2) Uani 1 1 d . . . H35A H 1.4595 0.2768 -0.0719 0.077 Uiso 1 1 calc R . . H35B H 1.5621 0.1843 -0.0303 0.077 Uiso 1 1 calc R . . H35C H 1.5116 0.2712 0.0184 0.077 Uiso 1 1 calc R . . C36 C 1.3975(8) 0.0400(6) 0.2023(6) 0.0429(19) Uani 1 1 d . . . H36A H 1.4154 0.0796 0.2375 0.064 Uiso 1 1 calc R . . H36B H 1.4804 0.0052 0.176 0.064 Uiso 1 1 calc R . . H36C H 1.3276 -0.0153 0.2517 0.064 Uiso 1 1 calc R . . C37 C 1.3048(7) 0.0567(6) 0.0256(6) 0.0386(18) Uani 1 1 d . . . H37A H 1.2571 -0.0109 0.0788 0.058 Uiso 1 1 calc R . . H37B H 1.3907 0.04 -0.0174 0.058 Uiso 1 1 calc R . . H37C H 1.2493 0.0997 -0.0185 0.058 Uiso 1 1 calc R . . Si1 Si 1.2046(2) 0.34141(16) 0.11047(17) 0.0363(5) Uani 1 1 d . . . Si2 Si 1.33838(19) 0.13659(16) 0.09109(16) 0.0325(4) Uani 1 1 d . . . Pb1 Pb 1.01565(3) 0.11954(2) 0.261748(19) 0.02602(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 O1 0.029(3) 0.020(2) 0.033(3) -0.012(2) -0.013(2) 0.0019(19) C2 0.029(4) 0.023(3) 0.021(3) -0.014(3) -0.009(3) 0.007(3) C3 0.032(4) 0.029(4) 0.029(4) -0.020(3) -0.009(3) 0.008(3) C4 0.039(4) 0.023(3) 0.025(3) -0.014(3) -0.002(3) 0.001(3) C5 0.028(4) 0.023(3) 0.026(3) -0.014(3) -0.005(3) 0.001(3) C6 0.028(4) 0.031(4) 0.028(4) -0.018(3) -0.008(3) 0.000(3) C7 0.025(3) 0.029(4) 0.021(3) -0.014(3) -0.004(3) 0.002(3) C8 0.021(3) 0.029(3) 0.025(3) -0.013(3) -0.008(3) 0.005(3) C9 0.047(5) 0.029(4) 0.037(4) -0.019(3) -0.021(3) 0.008(3) C10 0.080(7) 0.035(4) 0.057(5) -0.026(4) -0.043(5) 0.018(4) C11 0.048(5) 0.049(5) 0.049(5) -0.022(4) -0.028(4) 0.012(4) C12 0.072(6) 0.032(4) 0.056(5) -0.012(4) -0.043(5) 0.013(4) C13 0.042(5) 0.033(4) 0.042(4) -0.009(3) -0.011(4) -0.013(3) C14 0.076(8) 0.079(8) 0.120(10) -0.058(7) 0.006(7) -0.026(6) C15 0.071(8) 0.056(7) 0.222(16) -0.021(8) -0.090(10) -0.015(6) C16 0.062(7) 0.056(6) 0.183(13) -0.073(8) -0.033(8) 0.001(5) N20 0.017(3) 0.026(3) 0.032(3) -0.017(2) -0.007(2) 0.001(2) C21 0.020(4) 0.041(4) 0.044(4) -0.022(3) -0.007(3) 0.000(3) C22 0.031(4) 0.033(4) 0.058(5) -0.028(4) -0.012(4) 0.006(3) O23 0.032(3) 0.043(3) 0.053(3) -0.032(3) -0.009(2) 0.007(2) C24 0.058(6) 0.041(5) 0.045(5) -0.028(4) 0.001(4) 0.002(4) C25 0.031(4) 0.019(3) 0.027(3) -0.009(3) -0.007(3) -0.002(3) C26 0.040(4) 0.022(4) 0.038(4) -0.009(3) -0.014(3) -0.002(3) O27 0.084(5) 0.034(3) 0.042(3) -0.013(2) -0.035(3) 0.002(3) C28 0.080(7) 0.041(5) 0.032(4) -0.013(4) -0.026(4) 0.007(4) N31 0.025(3) 0.033(3) 0.031(3) -0.015(3) -0.003(2) -0.005(2) C32 0.045(5) 0.028(4) 0.058(5) -0.022(4) -0.024(4) 0.006(3) C33 0.065(7) 0.043(5) 0.060(6) -0.008(4) -0.005(5) 0.006(5) C34 0.058(6) 0.054(6) 0.126(9) -0.061(6) -0.043(6) 0.006(5) C35 0.023(4) 0.070(6) 0.064(6) -0.034(5) -0.007(4) -0.003(4) C36 0.033(4) 0.048(5) 0.057(5) -0.025(4) -0.022(4) 0.003(4) C37 0.026(4) 0.057(5) 0.044(4) -0.032(4) -0.009(3) 0.002(3) Si1 0.0318(11) 0.0280(11) 0.0500(13) -0.0153(9) -0.0142(10) -0.0033(8) Si2 0.0226(10) 0.0404(12) 0.0382(11) -0.0205(9) -0.0093(8) 0.0019(8) Pb1 0.02896(15) 0.02666(14) 0.02625(14) -0.01478(11) -0.00823(10) 0.00025(9) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag O1 C2 1.339(7) . ? O1 Pb1 2.220(4) . ? C2 C3 1.395(9) . ? C2 C7 1.411(9) . ? C3 C4 1.402(9) . ? C3 C9 1.531(9) . ? C4 C5 1.402(9) . ? C4 H4 0.95 . ? C5 C6 1.376(9) . ? C5 C13 1.525(9) . ? C6 C7 1.393(8) . ? C6 H6 0.95 . ? C7 C8 1.529(8) . ? C8 N20 1.505(7) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 C11 1.526(10) . ? C9 C12 1.540(10) . ? C9 C10 1.567(9) . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 C16 1.437(11) . ? C13 C15 1.493(13) . ? C13 C14 1.515(12) . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? N20 C25 1.484(8) . ? N20 C21 1.487(8) . ? N20 Pb1 2.537(5) . ? C21 C22 1.488(9) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 O23 1.399(8) . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? O23 C24 1.423(8) . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 C26 1.517(9) . ? C25 H25A 0.99 . ? C25 H25B 0.99 . ? C26 O27 1.375(8) . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? O27 C28 1.438(8) . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? N31 Si2 1.721(6) . ? N31 Si1 1.724(6) . ? N31 Pb1 2.243(5) . ? C32 Si1 1.864(8) . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? C33 Si1 1.844(8) . ? C33 H33A 0.98 . ? C33 H33B 0.98 . ? C33 H33C 0.98 . ? C34 Si1 1.886(8) . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 Si2 1.889(8) . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? C36 Si2 1.869(8) . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C37 Si2 1.896(7) . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C2 O1 Pb1 116.5(4) . . ? O1 C2 C3 122.6(6) . . ? O1 C2 C7 118.7(5) . . ? C3 C2 C7 118.7(6) . . ? C2 C3 C4 118.7(6) . . ? C2 C3 C9 121.6(6) . . ? C4 C3 C9 119.6(6) . . ? C3 C4 C5 123.3(6) . . ? C3 C4 H4 118.3 . . ? C5 C4 H4 118.3 . . ? C6 C5 C4 116.6(6) . . ? C6 C5 C13 123.4(6) . . ? C4 C5 C13 120.0(6) . . ? C5 C6 C7 122.2(6) . . ? C5 C6 H6 118.9 . . ? C7 C6 H6 118.9 . . ? C6 C7 C2 120.5(6) . . ? C6 C7 C8 119.2(6) . . ? C2 C7 C8 120.2(6) . . ? N20 C8 C7 113.6(5) . . ? N20 C8 H8A 108.8 . . ? C7 C8 H8A 108.8 . . ? N20 C8 H8B 108.8 . . ? C7 C8 H8B 108.8 . . ? H8A C8 H8B 107.7 . . ? C11 C9 C3 110.5(6) . . ? C11 C9 C12 108.3(6) . . ? C3 C9 C12 113.3(6) . . ? C11 C9 C10 109.3(6) . . ? C3 C9 C10 111.1(6) . . ? C12 C9 C10 104.1(6) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C16 C13 C15 111.8(8) . . ? C16 C13 C14 110.3(8) . . ? C15 C13 C14 96.8(9) . . ? C16 C13 C5 112.6(7) . . ? C15 C13 C5 113.1(6) . . ? C14 C13 C5 111.2(7) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C25 N20 C21 114.1(5) . . ? C25 N20 C8 109.2(5) . . ? C21 N20 C8 109.6(5) . . ? C25 N20 Pb1 107.5(3) . . ? C21 N20 Pb1 110.2(4) . . ? C8 N20 Pb1 105.9(3) . . ? N20 C21 C22 116.1(5) . . ? N20 C21 H21A 108.3 . . ? C22 C21 H21A 108.3 . . ? N20 C21 H21B 108.3 . . ? C22 C21 H21B 108.3 . . ? H21A C21 H21B 107.4 . . ? O23 C22 C21 109.0(6) . . ? O23 C22 H22A 109.9 . . ? C21 C22 H22A 109.9 . . ? O23 C22 H22B 109.9 . . ? C21 C22 H22B 109.9 . . ? H22A C22 H22B 108.3 . . ? C22 O23 C24 112.6(6) . . ? O23 C24 H24A 109.5 . . ? O23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? O23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? N20 C25 C26 115.9(5) . . ? N20 C25 H25A 108.3 . . ? C26 C25 H25A 108.3 . . ? N20 C25 H25B 108.3 . . ? C26 C25 H25B 108.3 . . ? H25A C25 H25B 107.4 . . ? O27 C26 C25 106.9(5) . . ? O27 C26 H26A 110.3 . . ? C25 C26 H26A 110.3 . . ? O27 C26 H26B 110.3 . . ? C25 C26 H26B 110.3 . . ? H26A C26 H26B 108.6 . . ? C26 O27 C28 113.9(5) . . ? O27 C28 H28A 109.5 . . ? O27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? O27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? Si2 N31 Si1 124.5(3) . . ? Si2 N31 Pb1 120.6(3) . . ? Si1 N31 Pb1 112.5(3) . . ? Si1 C32 H32A 109.5 . . ? Si1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si1 C33 H33A 109.5 . . ? Si1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si1 C34 H34A 109.5 . . ? Si1 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si1 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 . . ? Si2 C37 H37A 109.5 . . ? Si2 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si2 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? N31 Si1 C33 114.6(4) . . ? N31 Si1 C32 110.2(3) . . ? C33 Si1 C32 106.1(4) . . ? N31 Si1 C34 112.2(3) . . ? C33 Si1 C34 107.3(5) . . ? C32 Si1 C34 105.9(4) . . ? N31 Si2 C36 110.8(3) . . ? N31 Si2 C35 112.5(3) . . ? C36 Si2 C35 107.5(4) . . ? N31 Si2 C37 113.5(3) . . ? C36 Si2 C37 108.0(3) . . ? C35 Si2 C37 104.2(3) . . ? O1 Pb1 N31 93.75(18) . . ? O1 Pb1 N20 83.91(15) . . ? N31 Pb1 N20 95.83(18) . . ? 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 Pb1 O1 C2 C3 -118.7(5) . . . . ? Pb1 O1 C2 C7 62.4(6) . . . . ? O1 C2 C3 C4 -178.6(6) . . . . ? C7 C2 C3 C4 0.4(9) . . . . ? O1 C2 C3 C9 -2.0(9) . . . . ? C7 C2 C3 C9 177.0(6) . . . . ? C2 C3 C4 C5 -0.6(10) . . . . ? C9 C3 C4 C5 -177.2(6) . . . . ? C3 C4 C5 C6 -0.2(9) . . . . ? C3 C4 C5 C13 178.8(6) . . . . ? C4 C5 C6 C7 1.2(9) . . . . ? C13 C5 C6 C7 -177.7(6) . . . . ? C5 C6 C7 C2 -1.5(9) . . . . ? C5 C6 C7 C8 176.4(6) . . . . ? O1 C2 C7 C6 179.6(6) . . . . ? C3 C2 C7 C6 0.6(9) . . . . ? O1 C2 C7 C8 1.7(8) . . . . ? C3 C2 C7 C8 -177.3(6) . . . . ? C6 C7 C8 N20 108.6(6) . . . . ? C2 C7 C8 N20 -73.5(7) . . . . ? C2 C3 C9 C11 -61.6(8) . . . . ? C4 C3 C9 C11 114.9(7) . . . . ? C2 C3 C9 C12 176.7(6) . . . . ? C4 C3 C9 C12 -6.8(9) . . . . ? C2 C3 C9 C10 59.9(8) . . . . ? C4 C3 C9 C10 -123.6(7) . . . . ? C6 C5 C13 C16 119.4(9) . . . . ? C4 C5 C13 C16 -59.5(10) . . . . ? C6 C5 C13 C15 -8.6(12) . . . . ? C4 C5 C13 C15 172.5(9) . . . . ? C6 C5 C13 C14 -116.2(8) . . . . ? C4 C5 C13 C14 64.9(10) . . . . ? C7 C8 N20 C25 173.9(5) . . . . ? C7 C8 N20 C21 -60.5(7) . . . . ? C7 C8 N20 Pb1 58.3(5) . . . . ? C25 N20 C21 C22 -52.2(7) . . . . ? C8 N20 C21 C22 -175.1(6) . . . . ? Pb1 N20 C21 C22 68.8(6) . . . . ? N20 C21 C22 O23 -56.1(8) . . . . ? C21 C22 O23 C24 -172.5(6) . . . . ? C21 N20 C25 C26 -64.5(7) . . . . ? C8 N20 C25 C26 58.5(7) . . . . ? Pb1 N20 C25 C26 173.1(4) . . . . ? N20 C25 C26 O27 162.2(6) . . . . ? C25 C26 O27 C28 175.3(6) . . . . ? Si2 N31 Si1 C33 65.9(5) . . . . ? Pb1 N31 Si1 C33 -131.5(4) . . . . ? Si2 N31 Si1 C32 -174.5(4) . . . . ? Pb1 N31 Si1 C32 -11.9(4) . . . . ? Si2 N31 Si1 C34 -56.7(5) . . . . ? Pb1 N31 Si1 C34 105.8(4) . . . . ? Si1 N31 Si2 C36 106.0(4) . . . . ? Pb1 N31 Si2 C36 -55.2(4) . . . . ? Si1 N31 Si2 C35 -14.3(5) . . . . ? Pb1 N31 Si2 C35 -175.6(3) . . . . ? Si1 N31 Si2 C37 -132.4(4) . . . . ? Pb1 N31 Si2 C37 66.4(4) . . . . ? C2 O1 Pb1 N31 -146.7(4) . . . . ? C2 O1 Pb1 N20 -51.2(4) . . . . ? Si2 N31 Pb1 O1 -11.0(3) . . . . ? Si1 N31 Pb1 O1 -174.3(3) . . . . ? Si2 N31 Pb1 N20 -95.3(3) . . . . ? Si1 N31 Pb1 N20 101.4(3) . . . . ? C25 N20 Pb1 O1 -123.5(4) . . . . ? C21 N20 Pb1 O1 111.6(4) . . . . ? C8 N20 Pb1 O1 -6.8(3) . . . . ? C25 N20 Pb1 N31 -30.3(4) . . . . ? C21 N20 Pb1 N31 -155.2(4) . . . . ? C8 N20 Pb1 N31 86.4(4) . . . . ? #----------------------------------------------------------------------------# # END OF CIF FILE FOR wlf01503 #----------------------------------------------------------------------------# _database_code_depnum_ccdc_archive 'CCDC 942088' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_WLF013 _audit_creation_date 2013-01-11T17:21:22-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C25 H50 Ge N2 O Si2' _chemical_formula_sum 'C25 H50 Ge N2 O Si2' _chemical_formula_weight 523.44 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.4714(6) _cell_length_b 12.3029(8) _cell_length_c 12.3573(6) _cell_angle_alpha 81.087(3) _cell_angle_beta 75.381(2) _cell_angle_gamma 86.021(3) _cell_volume 1521.07(15) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7125 _cell_measurement_theta_min 2.57 _cell_measurement_theta_max 27.44 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.32 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.15 _exptl_crystal_density_diffrn 1.143 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 564 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.103 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.774 _exptl_absorpt_correction_T_max 0.847 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0465 _diffrn_reflns_av_unetI/netI 0.0491 _diffrn_reflns_number 25015 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 2.95 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_theta_full 27.49 _diffrn_measured_fraction_theta_full 0.993 _diffrn_measured_fraction_theta_max 0.993 _reflns_number_total 6928 _reflns_number_gt 5730 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0327P)^2^+0.3488P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6928 _refine_ls_number_parameters 294 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0465 _refine_ls_R_factor_gt 0.0352 _refine_ls_wR_factor_ref 0.0818 _refine_ls_wR_factor_gt 0.0777 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.431 _refine_diff_density_min -0.271 _refine_diff_density_rms 0.064 _iucr_refine_instructions_details ; .res file for SHELXL : job.res ................................................................. TITL import in P -1 CELL 0.71073 10.4714 12.3029 12.3573 81.087 75.381 86.021 ZERR 2.00 0.0006 0.0008 0.0006 0.003 0.002 0.003 LATT 1 SFAC C H N O GE SI UNIT 50 100 4 2 2 4 MERG 2 FMAP 2 PLAN 20 ACTA BOND $H CONF LIST 4 WPDB -2 L.S. 4 TEMP -123.00 WGHT 0.032700 0.348800 FVAR 0.67396 GE1 5 1.096679 0.780738 0.801087 11.00000 0.01616 0.01613 = 0.02034 -0.00401 -0.00455 0.00066 SI1 6 1.239508 0.564109 0.740120 11.00000 0.02362 0.01613 = 0.03153 -0.00425 -0.00317 0.00286 SI2 6 1.368635 0.772032 0.609904 11.00000 0.01696 0.02346 = 0.02970 0.00105 -0.00140 0.00196 N2 3 1.232381 0.706283 0.702337 11.00000 0.01699 0.01603 = 0.02383 -0.00289 -0.00381 0.00125 C2 1 1.327697 0.891287 0.509506 11.00000 0.03020 0.03237 = 0.02594 0.00323 0.00090 0.00088 AFIX 137 H2A 2 1.259023 0.870771 0.475984 11.00000 -1.50000 H2B 2 1.406953 0.911639 0.449628 11.00000 -1.50000 H2C 2 1.295651 0.953986 0.550259 11.00000 -1.50000 AFIX 0 C3 1 1.478793 0.816497 0.691461 11.00000 0.02270 0.03614 = 0.06387 0.00452 -0.01779 -0.00367 AFIX 137 H3A 2 1.426742 0.858927 0.749331 11.00000 -1.50000 H3B 2 1.547958 0.862396 0.640048 11.00000 -1.50000 H3C 2 1.519458 0.751490 0.727783 11.00000 -1.50000 AFIX 0 C4 1 1.470037 0.676567 0.514496 11.00000 0.03402 0.03862 = 0.04832 0.00241 0.01543 0.00891 AFIX 137 H4A 2 1.489994 0.607908 0.559948 11.00000 -1.50000 H4B 2 1.552637 0.711465 0.472035 11.00000 -1.50000 H4C 2 1.420441 0.660470 0.461676 11.00000 -1.50000 AFIX 0 C5 1 1.391777 0.514332 0.788042 11.00000 0.04132 0.02772 = 0.06059 0.00435 -0.01885 0.00757 AFIX 137 H5A 2 1.469662 0.529843 0.725214 11.00000 -1.50000 H5B 2 1.387762 0.434836 0.813350 11.00000 -1.50000 H5C 2 1.397707 0.552229 0.850676 11.00000 -1.50000 AFIX 0 C6 1 1.224062 0.488152 0.624548 11.00000 0.04283 0.02946 = 0.04947 -0.01957 -0.00858 0.00572 AFIX 137 H6A 2 1.142138 0.512054 0.601990 11.00000 -1.50000 H6B 2 1.222350 0.408917 0.651518 11.00000 -1.50000 H6C 2 1.299596 0.503640 0.559510 11.00000 -1.50000 AFIX 0 C7 1 1.099551 0.519185 0.862433 11.00000 0.04708 0.01763 = 0.04674 -0.00013 0.00621 -0.00048 AFIX 137 H7A 2 1.102905 0.555809 0.926620 11.00000 -1.50000 H7B 2 1.106337 0.439249 0.883530 11.00000 -1.50000 H7C 2 1.015815 0.538875 0.841465 11.00000 -1.50000 AFIX 0 O1 4 1.161795 0.921089 0.741344 11.00000 0.01691 0.01537 = 0.02630 -0.00489 -0.00555 0.00140 C12 1 1.074649 1.008399 0.755422 11.00000 0.01796 0.01507 = 0.01837 -0.00070 -0.00322 0.00028 C13 1 1.095170 1.096102 0.809529 11.00000 0.01860 0.01589 = 0.01782 -0.00058 -0.00378 -0.00333 C14 1 0.997506 1.179570 0.821535 11.00000 0.02458 0.01505 = 0.02491 -0.00395 -0.00639 -0.00284 AFIX 43 H14 2 1.010172 1.239426 0.857525 11.00000 -1.20000 AFIX 0 C15 1 0.882112 1.180587 0.783870 11.00000 0.02163 0.01669 = 0.02689 -0.00228 -0.00730 0.00193 C16 1 0.869070 1.095076 0.726967 11.00000 0.02314 0.02300 = 0.02807 -0.00339 -0.01302 0.00238 AFIX 43 H16 2 0.793377 1.094487 0.697909 11.00000 -1.20000 AFIX 0 C17 1 0.963574 1.010026 0.711120 11.00000 0.02270 0.01631 = 0.02123 -0.00286 -0.00844 -0.00031 C18 1 1.221455 1.100632 0.850174 11.00000 0.01883 0.01836 = 0.02421 -0.00338 -0.00701 -0.00307 C19 1 1.226057 1.206187 0.900418 11.00000 0.02788 0.02419 = 0.03967 -0.01068 -0.01371 -0.00357 AFIX 137 H19A 2 1.221139 1.270292 0.843481 11.00000 -1.50000 H19B 2 1.308796 1.206452 0.923737 11.00000 -1.50000 H19C 2 1.151178 1.209327 0.966170 11.00000 -1.50000 AFIX 0 C20 1 1.341700 1.099830 0.748455 11.00000 0.02039 0.03245 = 0.03523 -0.00841 -0.00054 -0.00891 AFIX 137 H20A 2 1.340305 1.034706 0.712104 11.00000 -1.50000 H20B 2 1.423001 1.097872 0.774378 11.00000 -1.50000 H20C 2 1.338360 1.166400 0.694113 11.00000 -1.50000 AFIX 0 C21 1 1.230198 1.002761 0.942076 11.00000 0.02935 0.02717 = 0.02966 -0.00123 -0.01446 -0.00306 AFIX 137 H21A 2 1.152643 1.004690 1.005794 11.00000 -1.50000 H21B 2 1.310391 1.007380 0.968099 11.00000 -1.50000 H21C 2 1.233135 0.933797 0.910942 11.00000 -1.50000 AFIX 0 C22 1 0.778622 1.275407 0.799261 11.00000 0.02596 0.02071 = 0.03836 -0.00731 -0.01337 0.00544 C23 1 0.640912 1.235057 0.810614 11.00000 0.03086 0.04427 = 0.13183 -0.03848 -0.02318 0.01489 AFIX 137 H23A 2 0.620809 1.174588 0.873416 11.00000 -1.50000 H23B 2 0.637416 1.209007 0.740414 11.00000 -1.50000 H23C 2 0.575931 1.295622 0.825317 11.00000 -1.50000 AFIX 0 C24 1 0.812766 1.363364 0.697487 11.00000 0.07800 0.04205 = 0.07511 0.01543 0.00228 0.03428 AFIX 137 H24A 2 0.746101 1.423481 0.705607 11.00000 -1.50000 H24B 2 0.814687 1.331754 0.628990 11.00000 -1.50000 H24C 2 0.899643 1.391872 0.691890 11.00000 -1.50000 AFIX 0 C25 1 0.773804 1.326622 0.904479 11.00000 0.06491 0.06425 = 0.07778 -0.04457 -0.03638 0.04340 AFIX 137 H25A 2 0.859301 1.358178 0.897870 11.00000 -1.50000 H25B 2 0.754408 1.269975 0.970993 11.00000 -1.50000 H25C 2 0.704595 1.384760 0.912471 11.00000 -1.50000 AFIX 0 C26 1 0.956408 0.924838 0.637572 11.00000 0.02442 0.02265 = 0.02465 -0.00679 -0.01112 0.00218 AFIX 23 H26A 2 0.881227 0.944779 0.602511 11.00000 -1.20000 H26B 2 1.038040 0.927019 0.575908 11.00000 -1.20000 AFIX 0 N27 3 0.940497 0.810551 0.697807 11.00000 0.01750 0.01956 = 0.02342 -0.00782 -0.00587 0.00121 C28 1 0.807369 0.803311 0.779043 11.00000 0.01790 0.03099 = 0.03311 -0.01360 -0.00684 0.00082 AFIX 23 H28A 2 0.740007 0.831610 0.737217 11.00000 -1.20000 H28B 2 0.804327 0.852316 0.836139 11.00000 -1.20000 AFIX 0 C29 1 0.770250 0.689867 0.839724 11.00000 0.02679 0.03396 = 0.04123 -0.00940 -0.00273 -0.00852 AFIX 137 H29A 2 0.765752 0.641722 0.784691 11.00000 -1.50000 H29B 2 0.683970 0.693912 0.893419 11.00000 -1.50000 H29C 2 0.836859 0.660100 0.880573 11.00000 -1.50000 AFIX 0 C30 1 0.961018 0.731278 0.614587 11.00000 0.02512 0.02578 = 0.03246 -0.01616 -0.00946 0.00260 AFIX 23 H30A 2 0.955210 0.655759 0.656736 11.00000 -1.20000 H30B 2 1.051840 0.739029 0.566065 11.00000 -1.20000 AFIX 0 C31 1 0.865570 0.743101 0.538314 11.00000 0.03918 0.04570 = 0.04422 -0.02704 -0.02150 0.00445 AFIX 137 H31A 2 0.775010 0.734583 0.584802 11.00000 -1.50000 H31B 2 0.886854 0.686291 0.488448 11.00000 -1.50000 H31C 2 0.873453 0.816033 0.492632 11.00000 -1.50000 HKLF 4 REM import in P -1 REM R1 = 0.0352 for 5730 Fo > 4sig(Fo) and 0.0465 for all 6928 data REM 294 parameters refined using 0 restraints END WGHT 0.0327 0.3482 REM Highest difference peak 0.43, deepest hole -0.27, 1-sigma level 0.06 Q1 1 1.1005 0.6397 0.5602 11.00000 0.05 0.43 Q2 1 0.8718 0.7999 0.7366 11.00000 0.05 0.41 Q3 1 0.9659 0.9674 0.6804 11.00000 0.05 0.36 Q4 1 1.1674 0.7250 0.7554 11.00000 0.05 0.33 Q5 1 1.1394 0.5430 0.7958 11.00000 0.05 0.32 Q6 1 0.9383 0.8643 0.6673 11.00000 0.05 0.32 Q7 1 0.8257 1.2263 0.7859 11.00000 0.05 0.32 Q8 1 1.2160 1.1458 0.8804 11.00000 0.05 0.31 Q9 1 0.9335 1.0630 0.7006 11.00000 0.05 0.31 Q10 1 1.1108 1.0635 0.7683 11.00000 0.05 0.31 Q11 1 1.2240 1.0581 0.8920 11.00000 0.05 0.31 Q12 1 0.9920 0.7989 0.7394 11.00000 0.05 0.31 Q13 1 1.2772 1.1078 0.8066 11.00000 0.05 0.31 Q14 1 1.0476 1.1383 0.8009 11.00000 0.05 0.30 Q15 1 1.0350 0.7468 0.8770 11.00000 0.05 0.30 Q16 1 1.1486 1.0982 0.8300 11.00000 0.05 0.29 Q17 1 1.3918 0.9042 0.4865 11.00000 0.05 0.28 Q18 1 1.4234 0.7249 0.5624 11.00000 0.05 0.27 Q19 1 1.2359 0.6496 0.7313 11.00000 0.05 0.27 Q20 1 0.8178 1.3650 0.8333 11.00000 0.05 0.27 ; #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1 Ge 1.096679(19) 0.780738(17) 0.801087(17) 0.01743(7) Uani 1 1 d . . . Si1 Si 1.23951(6) 0.56411(5) 0.74012(5) 0.02449(14) Uani 1 1 d . . . Si2 Si 1.36863(5) 0.77203(5) 0.60990(5) 0.02481(14) Uani 1 1 d . . . N2 N 1.23238(15) 0.70628(13) 0.70234(14) 0.0193(4) Uani 1 1 d . . . C2 C 1.3277(2) 0.89129(19) 0.50951(18) 0.0318(5) Uani 1 1 d . . . H2A H 1.259 0.8708 0.476 0.048 Uiso 1 1 calc R . . H2B H 1.407 0.9116 0.4496 0.048 Uiso 1 1 calc R . . H2C H 1.2957 0.954 0.5503 0.048 Uiso 1 1 calc R . . C3 C 1.4788(2) 0.8165(2) 0.6915(2) 0.0407(6) Uani 1 1 d . . . H3A H 1.4267 0.8589 0.7493 0.061 Uiso 1 1 calc R . . H3B H 1.548 0.8624 0.64 0.061 Uiso 1 1 calc R . . H3C H 1.5195 0.7515 0.7278 0.061 Uiso 1 1 calc R . . C4 C 1.4700(2) 0.6766(2) 0.5145(2) 0.0464(7) Uani 1 1 d . . . H4A H 1.49 0.6079 0.5599 0.07 Uiso 1 1 calc R . . H4B H 1.5526 0.7115 0.472 0.07 Uiso 1 1 calc R . . H4C H 1.4204 0.6605 0.4617 0.07 Uiso 1 1 calc R . . C5 C 1.3918(2) 0.5143(2) 0.7880(2) 0.0436(6) Uani 1 1 d . . . H5A H 1.4697 0.5298 0.7252 0.065 Uiso 1 1 calc R . . H5B H 1.3878 0.4348 0.8133 0.065 Uiso 1 1 calc R . . H5C H 1.3977 0.5522 0.8507 0.065 Uiso 1 1 calc R . . C6 C 1.2241(2) 0.4882(2) 0.6245(2) 0.0399(6) Uani 1 1 d . . . H6A H 1.1421 0.5121 0.602 0.06 Uiso 1 1 calc R . . H6B H 1.2224 0.4089 0.6515 0.06 Uiso 1 1 calc R . . H6C H 1.2996 0.5036 0.5595 0.06 Uiso 1 1 calc R . . C7 C 1.0996(2) 0.51919(19) 0.8624(2) 0.0409(6) Uani 1 1 d . . . H7A H 1.1029 0.5558 0.9266 0.061 Uiso 1 1 calc R . . H7B H 1.1063 0.4392 0.8835 0.061 Uiso 1 1 calc R . . H7C H 1.0158 0.5389 0.8415 0.061 Uiso 1 1 calc R . . O1 O 1.16180(12) 0.92109(11) 0.74134(11) 0.0194(3) Uani 1 1 d . . . C12 C 1.07465(18) 1.00840(16) 0.75542(16) 0.0176(4) Uani 1 1 d . . . C13 C 1.09517(18) 1.09610(16) 0.80953(16) 0.0176(4) Uani 1 1 d . . . C14 C 0.99751(19) 1.17957(16) 0.82153(17) 0.0212(4) Uani 1 1 d . . . H14 H 1.0102 1.2394 0.8575 0.025 Uiso 1 1 calc R . . C15 C 0.88211(19) 1.18059(16) 0.78387(17) 0.0217(4) Uani 1 1 d . . . C16 C 0.8691(2) 1.09508(17) 0.72697(17) 0.0237(4) Uani 1 1 d . . . H16 H 0.7934 1.0945 0.6979 0.028 Uiso 1 1 calc R . . C17 C 0.96357(19) 1.01003(16) 0.71112(16) 0.0195(4) Uani 1 1 d . . . C18 C 1.22145(18) 1.10063(16) 0.85017(17) 0.0200(4) Uani 1 1 d . . . C19 C 1.2261(2) 1.20619(18) 0.90042(19) 0.0288(5) Uani 1 1 d . . . H19A H 1.2211 1.2703 0.8435 0.043 Uiso 1 1 calc R . . H19B H 1.3088 1.2065 0.9237 0.043 Uiso 1 1 calc R . . H19C H 1.1512 1.2093 0.9662 0.043 Uiso 1 1 calc R . . C20 C 1.3417(2) 1.09983(19) 0.74845(19) 0.0297(5) Uani 1 1 d . . . H20A H 1.3403 1.0347 0.7121 0.045 Uiso 1 1 calc R . . H20B H 1.423 1.0979 0.7744 0.045 Uiso 1 1 calc R . . H20C H 1.3384 1.1664 0.6941 0.045 Uiso 1 1 calc R . . C21 C 1.2302(2) 1.00276(18) 0.94208(18) 0.0276(5) Uani 1 1 d . . . H21A H 1.1526 1.0047 1.0058 0.041 Uiso 1 1 calc R . . H21B H 1.3104 1.0074 0.9681 0.041 Uiso 1 1 calc R . . H21C H 1.2331 0.9338 0.9109 0.041 Uiso 1 1 calc R . . C22 C 0.7786(2) 1.27541(17) 0.79926(19) 0.0273(5) Uani 1 1 d . . . C23 C 0.6409(2) 1.2351(2) 0.8106(3) 0.0663(10) Uani 1 1 d . . . H23A H 0.6208 1.1746 0.8734 0.1 Uiso 1 1 calc R . . H23B H 0.6374 1.209 0.7404 0.1 Uiso 1 1 calc R . . H23C H 0.5759 1.2956 0.8253 0.1 Uiso 1 1 calc R . . C24 C 0.8128(3) 1.3634(2) 0.6975(3) 0.0732(11) Uani 1 1 d . . . H24A H 0.7461 1.4235 0.7056 0.11 Uiso 1 1 calc R . . H24B H 0.8147 1.3318 0.629 0.11 Uiso 1 1 calc R . . H24C H 0.8996 1.3919 0.6919 0.11 Uiso 1 1 calc R . . C25 C 0.7738(3) 1.3266(3) 0.9045(3) 0.0640(10) Uani 1 1 d . . . H25A H 0.8593 1.3582 0.8979 0.096 Uiso 1 1 calc R . . H25B H 0.7544 1.27 0.971 0.096 Uiso 1 1 calc R . . H25C H 0.7046 1.3848 0.9125 0.096 Uiso 1 1 calc R . . C26 C 0.9564(2) 0.92484(16) 0.63757(17) 0.0227(4) Uani 1 1 d . . . H26A H 0.8812 0.9448 0.6025 0.027 Uiso 1 1 calc R . . H26B H 1.038 0.927 0.5759 0.027 Uiso 1 1 calc R . . N27 N 0.94050(15) 0.81055(13) 0.69781(14) 0.0196(4) Uani 1 1 d . . . C28 C 0.80737(19) 0.80331(18) 0.77904(18) 0.0263(5) Uani 1 1 d . . . H28A H 0.74 0.8316 0.7372 0.032 Uiso 1 1 calc R . . H28B H 0.8043 0.8523 0.8361 0.032 Uiso 1 1 calc R . . C29 C 0.7703(2) 0.68987(19) 0.8397(2) 0.0342(5) Uani 1 1 d . . . H29A H 0.7658 0.6417 0.7847 0.051 Uiso 1 1 calc R . . H29B H 0.684 0.6939 0.8934 0.051 Uiso 1 1 calc R . . H29C H 0.8369 0.6601 0.8806 0.051 Uiso 1 1 calc R . . C30 C 0.9610(2) 0.73128(18) 0.61459(18) 0.0262(5) Uani 1 1 d . . . H30A H 0.9552 0.6558 0.6567 0.031 Uiso 1 1 calc R . . H30B H 1.0518 0.739 0.5661 0.031 Uiso 1 1 calc R . . C31 C 0.8656(2) 0.7431(2) 0.5383(2) 0.0390(6) Uani 1 1 d . . . H31A H 0.775 0.7346 0.5848 0.059 Uiso 1 1 calc R . . H31B H 0.8869 0.6863 0.4884 0.059 Uiso 1 1 calc R . . H31C H 0.8735 0.816 0.4926 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.01616(11) 0.01613(12) 0.02034(12) -0.00401(8) -0.00455(8) 0.00066(8) Si1 0.0236(3) 0.0161(3) 0.0315(3) -0.0043(2) -0.0032(2) 0.0029(2) Si2 0.0170(3) 0.0235(3) 0.0297(3) 0.0011(3) -0.0014(2) 0.0020(2) N2 0.0170(8) 0.0160(9) 0.0238(9) -0.0029(7) -0.0038(7) 0.0012(6) C2 0.0302(12) 0.0324(13) 0.0259(12) 0.0032(10) 0.0009(9) 0.0009(10) C3 0.0227(12) 0.0361(14) 0.0639(18) 0.0045(12) -0.0178(11) -0.0037(10) C4 0.0340(14) 0.0386(15) 0.0483(16) 0.0024(12) 0.0154(11) 0.0089(11) C5 0.0413(15) 0.0277(14) 0.0606(18) 0.0043(12) -0.0188(13) 0.0076(11) C6 0.0428(14) 0.0295(14) 0.0495(16) -0.0196(12) -0.0086(12) 0.0057(11) C7 0.0471(15) 0.0176(12) 0.0467(15) -0.0001(11) 0.0062(12) -0.0005(10) O1 0.0169(7) 0.0154(7) 0.0263(8) -0.0049(6) -0.0056(6) 0.0014(5) C12 0.0180(10) 0.0151(10) 0.0184(10) -0.0007(8) -0.0032(8) 0.0003(7) C13 0.0186(10) 0.0159(10) 0.0178(10) -0.0006(8) -0.0038(8) -0.0033(8) C14 0.0246(11) 0.0151(10) 0.0249(11) -0.0039(8) -0.0064(8) -0.0028(8) C15 0.0216(10) 0.0167(10) 0.0269(11) -0.0023(8) -0.0073(8) 0.0019(8) C16 0.0231(11) 0.0230(11) 0.0281(11) -0.0034(9) -0.0130(9) 0.0024(8) C17 0.0227(10) 0.0163(10) 0.0212(10) -0.0029(8) -0.0084(8) -0.0003(8) C18 0.0188(10) 0.0184(10) 0.0242(11) -0.0034(8) -0.0070(8) -0.0031(8) C19 0.0279(12) 0.0242(12) 0.0397(13) -0.0107(10) -0.0137(10) -0.0036(9) C20 0.0204(11) 0.0325(13) 0.0352(13) -0.0084(10) -0.0005(9) -0.0089(9) C21 0.0293(12) 0.0272(12) 0.0297(12) -0.0012(9) -0.0145(9) -0.0031(9) C22 0.0260(11) 0.0207(11) 0.0384(13) -0.0073(9) -0.0134(10) 0.0054(9) C23 0.0309(15) 0.0443(18) 0.132(3) -0.0385(19) -0.0232(16) 0.0149(13) C24 0.078(2) 0.0421(18) 0.075(2) 0.0154(16) 0.0023(18) 0.0343(16) C25 0.065(2) 0.064(2) 0.078(2) -0.0446(18) -0.0364(17) 0.0434(16) C26 0.0244(11) 0.0227(11) 0.0246(11) -0.0068(9) -0.0111(9) 0.0022(8) N27 0.0175(8) 0.0196(9) 0.0234(9) -0.0078(7) -0.0059(7) 0.0012(7) C28 0.0179(10) 0.0310(12) 0.0331(12) -0.0136(10) -0.0068(9) 0.0008(9) C29 0.0268(12) 0.0340(14) 0.0412(14) -0.0094(11) -0.0027(10) -0.0085(10) C30 0.0251(11) 0.0258(12) 0.0325(12) -0.0162(10) -0.0095(9) 0.0026(9) C31 0.0392(14) 0.0457(16) 0.0442(15) -0.0270(12) -0.0215(11) 0.0045(11) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 O1 1.8724(13) . ? Ge1 N2 1.9073(15) . ? Ge1 N27 2.2942(15) . ? Si1 N2 1.7405(17) . ? Si1 C7 1.864(2) . ? Si1 C6 1.868(2) . ? Si1 C5 1.870(2) . ? Si2 N2 1.7452(17) . ? Si2 C3 1.868(2) . ? Si2 C2 1.869(2) . ? Si2 C4 1.876(2) . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? O1 C12 1.363(2) . ? C12 C17 1.403(3) . ? C12 C13 1.409(3) . ? C13 C14 1.395(3) . ? C13 C18 1.536(3) . ? C14 C15 1.399(3) . ? C14 H14 0.95 . ? C15 C16 1.385(3) . ? C15 C22 1.536(3) . ? C16 C17 1.391(3) . ? C16 H16 0.95 . ? C17 C26 1.507(3) . ? C18 C19 1.532(3) . ? C18 C21 1.537(3) . ? C18 C20 1.539(3) . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 C24 1.512(4) . ? C22 C25 1.519(3) . ? C22 C23 1.524(3) . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 N27 1.485(3) . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? N27 C30 1.492(2) . ? N27 C28 1.497(2) . ? C28 C29 1.505(3) . ? C28 H28A 0.99 . ? C28 H28B 0.99 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C30 C31 1.524(3) . ? C30 H30A 0.99 . ? C30 H30B 0.99 . ? C31 H31A 0.98 . ? C31 H31B 0.98 . ? C31 H31C 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Ge1 N2 94.52(6) . . ? O1 Ge1 N27 90.22(6) . . ? N2 Ge1 N27 100.60(6) . . ? N2 Si1 C7 110.66(9) . . ? N2 Si1 C6 112.49(10) . . ? C7 Si1 C6 105.56(12) . . ? N2 Si1 C5 112.86(10) . . ? C7 Si1 C5 105.09(12) . . ? C6 Si1 C5 109.69(11) . . ? N2 Si2 C3 110.01(10) . . ? N2 Si2 C2 114.94(9) . . ? C3 Si2 C2 109.88(11) . . ? N2 Si2 C4 111.20(10) . . ? C3 Si2 C4 106.85(12) . . ? C2 Si2 C4 103.52(11) . . ? Si1 N2 Si2 119.50(9) . . ? Si1 N2 Ge1 114.38(9) . . ? Si2 N2 Ge1 123.34(9) . . ? Si2 C2 H2A 109.5 . . ? Si2 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si2 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si2 C3 H3A 109.5 . . ? Si2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si2 C4 H4A 109.5 . . ? Si2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si1 C5 H5A 109.5 . . ? Si1 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si1 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si1 C6 H6A 109.5 . . ? Si1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si1 C7 H7A 109.5 . . ? Si1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C12 O1 Ge1 117.26(11) . . ? O1 C12 C17 117.54(17) . . ? O1 C12 C13 122.17(16) . . ? C17 C12 C13 120.28(17) . . ? C14 C13 C12 117.00(16) . . ? C14 C13 C18 121.80(17) . . ? C12 C13 C18 121.17(16) . . ? C13 C14 C15 124.07(18) . . ? C13 C14 H14 118 . . ? C15 C14 H14 118 . . ? C16 C15 C14 116.76(17) . . ? C16 C15 C22 121.68(17) . . ? C14 C15 C22 121.48(18) . . ? C15 C16 C17 121.91(18) . . ? C15 C16 H16 119 . . ? C17 C16 H16 119 . . ? C16 C17 C12 119.81(18) . . ? C16 C17 C26 121.33(17) . . ? C12 C17 C26 118.59(16) . . ? C19 C18 C13 112.15(16) . . ? C19 C18 C21 107.53(17) . . ? C13 C18 C21 110.36(16) . . ? C19 C18 C20 107.04(17) . . ? C13 C18 C20 108.90(16) . . ? C21 C18 C20 110.83(17) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 C25 108.6(2) . . ? C24 C22 C23 109.2(2) . . ? C25 C22 C23 107.1(2) . . ? C24 C22 C15 108.81(19) . . ? C25 C22 C15 112.18(17) . . ? C23 C22 C15 110.87(18) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N27 C26 C17 114.57(16) . . ? N27 C26 H26A 108.6 . . ? C17 C26 H26A 108.6 . . ? N27 C26 H26B 108.6 . . ? C17 C26 H26B 108.6 . . ? H26A C26 H26B 107.6 . . ? C26 N27 C30 109.95(16) . . ? C26 N27 C28 108.59(15) . . ? C30 N27 C28 113.01(15) . . ? C26 N27 Ge1 106.57(11) . . ? C30 N27 Ge1 110.69(11) . . ? C28 N27 Ge1 107.80(12) . . ? N27 C28 C29 115.40(17) . . ? N27 C28 H28A 108.4 . . ? C29 C28 H28A 108.4 . . ? N27 C28 H28B 108.4 . . ? C29 C28 H28B 108.4 . . ? H28A C28 H28B 107.5 . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? N27 C30 C31 116.39(16) . . ? N27 C30 H30A 108.2 . . ? C31 C30 H30A 108.2 . . ? N27 C30 H30B 108.2 . . ? C31 C30 H30B 108.2 . . ? H30A C30 H30B 107.3 . . ? C30 C31 H31A 109.5 . . ? C30 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C30 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 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 C7 Si1 N2 Si2 167.15(12) . . . . ? C6 Si1 N2 Si2 -75.06(13) . . . . ? C5 Si1 N2 Si2 49.71(15) . . . . ? C7 Si1 N2 Ge1 5.39(14) . . . . ? C6 Si1 N2 Ge1 123.19(11) . . . . ? C5 Si1 N2 Ge1 -112.05(12) . . . . ? C3 Si2 N2 Si1 -91.46(13) . . . . ? C2 Si2 N2 Si1 143.89(11) . . . . ? C4 Si2 N2 Si1 26.71(15) . . . . ? C3 Si2 N2 Ge1 68.58(13) . . . . ? C2 Si2 N2 Ge1 -56.06(14) . . . . ? C4 Si2 N2 Ge1 -173.25(12) . . . . ? O1 Ge1 N2 Si1 167.63(9) . . . . ? N27 Ge1 N2 Si1 -101.30(9) . . . . ? O1 Ge1 N2 Si2 6.67(11) . . . . ? N27 Ge1 N2 Si2 97.74(10) . . . . ? N2 Ge1 O1 C12 156.90(13) . . . . ? N27 Ge1 O1 C12 56.26(13) . . . . ? Ge1 O1 C12 C17 -58.7(2) . . . . ? Ge1 O1 C12 C13 122.95(17) . . . . ? O1 C12 C13 C14 -178.43(17) . . . . ? C17 C12 C13 C14 3.3(3) . . . . ? O1 C12 C13 C18 3.3(3) . . . . ? C17 C12 C13 C18 -175.04(18) . . . . ? C12 C13 C14 C15 0.3(3) . . . . ? C18 C13 C14 C15 178.59(19) . . . . ? C13 C14 C15 C16 -3.0(3) . . . . ? C13 C14 C15 C22 -179.72(19) . . . . ? C14 C15 C16 C17 2.1(3) . . . . ? C22 C15 C16 C17 178.88(19) . . . . ? C15 C16 C17 C12 1.3(3) . . . . ? C15 C16 C17 C26 -172.72(19) . . . . ? O1 C12 C17 C16 177.54(18) . . . . ? C13 C12 C17 C16 -4.1(3) . . . . ? O1 C12 C17 C26 -8.3(3) . . . . ? C13 C12 C17 C26 170.07(18) . . . . ? C14 C13 C18 C19 -1.4(3) . . . . ? C12 C13 C18 C19 176.79(18) . . . . ? C14 C13 C18 C21 118.4(2) . . . . ? C12 C13 C18 C21 -63.4(2) . . . . ? C14 C13 C18 C20 -119.7(2) . . . . ? C12 C13 C18 C20 58.5(2) . . . . ? C16 C15 C22 C24 -87.2(3) . . . . ? C14 C15 C22 C24 89.4(3) . . . . ? C16 C15 C22 C25 152.7(2) . . . . ? C14 C15 C22 C25 -30.8(3) . . . . ? C16 C15 C22 C23 33.0(3) . . . . ? C14 C15 C22 C23 -150.5(2) . . . . ? C16 C17 C26 N27 -117.7(2) . . . . ? C12 C17 C26 N27 68.2(2) . . . . ? C17 C26 N27 C30 -168.93(15) . . . . ? C17 C26 N27 C28 67.0(2) . . . . ? C17 C26 N27 Ge1 -48.92(17) . . . . ? O1 Ge1 N27 C26 -2.79(12) . . . . ? N2 Ge1 N27 C26 -97.43(12) . . . . ? O1 Ge1 N27 C30 116.74(13) . . . . ? N2 Ge1 N27 C30 22.10(14) . . . . ? O1 Ge1 N27 C28 -119.20(12) . . . . ? N2 Ge1 N27 C28 146.16(12) . . . . ? C26 N27 C28 C29 174.66(17) . . . . ? C30 N27 C28 C29 52.4(2) . . . . ? Ge1 N27 C28 C29 -70.26(18) . . . . ? C26 N27 C30 C31 -61.4(2) . . . . ? C28 N27 C30 C31 60.1(2) . . . . ? Ge1 N27 C30 C31 -178.84(16) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 942089' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_WLF016 _audit_creation_date 2013-01-17T14:22:35-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C25 H50 N2 O1 Pb1 Si2' _chemical_formula_sum 'C25 H50 N2 O1 Pb1 Si2' _chemical_formula_weight 658.04 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5366(4) _cell_length_b 11.8539(4) _cell_length_c 12.2084(4) _cell_angle_alpha 87.436(2) _cell_angle_beta 81.9730(10) _cell_angle_gamma 87.2970(10) _cell_volume 1507.08(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 5510 _cell_measurement_theta_min 2.36 _cell_measurement_theta_max 26.37 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.26 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.45 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 664 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 5.694 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.360 _exptl_absorpt_correction_T_max 0.505 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0367 _diffrn_reflns_av_unetI/netI 0.0563 _diffrn_reflns_number 15900 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -15 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 3.04 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _reflns_number_total 6818 _reflns_number_gt 5938 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0205P)^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_number_reflns 6818 _refine_ls_number_parameters 294 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0391 _refine_ls_R_factor_gt 0.0306 _refine_ls_wR_factor_ref 0.0569 _refine_ls_wR_factor_gt 0.0547 _refine_ls_goodness_of_fit_ref 1.009 _refine_ls_restrained_S_all 1.009 _refine_ls_shift/su_max 0.008 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.9 _refine_diff_density_min -0.9 _refine_diff_density_rms 0.132 _iucr_refine_instructions_details ; .res file for SHELXL : WLF016.res ................................................................. TITL import in P -1 CELL 0.71073 10.5366 11.8539 12.2084 87.436 81.973 87.297 ZERR 2.00 0.0004 0.0004 0.0004 0.002 0.001 0.001 LATT 1 SFAC C H N O SI PB UNIT 50.00 100.00 4.00 2.00 4.00 2.00 MERG 2 FMAP 2 PLAN 20 ACTA BOND $H CONF WPDB -2 L.S. 4 TEMP -123.00 WGHT 0.020500 FVAR 0.47925 PB1 6 0.594071 0.197655 0.295740 11.00000 0.01522 0.01947 = 0.01784 -0.00178 -0.00159 -0.00078 SI1 5 0.875785 0.180417 0.116249 11.00000 0.01510 0.01952 = 0.02191 -0.00206 -0.00020 -0.00130 SI2 5 0.753061 0.413136 0.168453 11.00000 0.02456 0.01616 = 0.02636 -0.00143 -0.00087 -0.00228 N1 3 0.750180 0.268118 0.174943 11.00000 0.01516 0.01531 = 0.02184 -0.00227 0.00176 -0.00389 O1 4 0.652176 0.023681 0.253636 11.00000 0.01276 0.01587 = 0.02683 -0.00016 -0.00158 -0.00019 C2 1 0.556424 -0.049000 0.280729 11.00000 0.01612 0.01927 = 0.01365 -0.00388 0.00088 -0.00081 C3 1 0.571975 -0.146539 0.349647 11.00000 0.01567 0.02099 = 0.01090 -0.00165 -0.00121 0.00192 C4 1 0.467116 -0.215073 0.375762 11.00000 0.02086 0.01734 = 0.01615 0.00013 -0.00188 -0.00197 AFIX 43 H4 2 0.475997 -0.279812 0.423260 11.00000 -1.20000 AFIX 0 C5 1 0.349410 -0.193980 0.336005 11.00000 0.01701 0.01843 = 0.02162 -0.00402 -0.00295 -0.00192 C6 1 0.341521 -0.101167 0.262962 11.00000 0.01058 0.02317 = 0.02201 -0.00163 -0.00694 -0.00059 AFIX 43 H6 2 0.264424 -0.085998 0.231873 11.00000 -1.20000 AFIX 0 C7 1 0.443104 -0.029880 0.234052 11.00000 0.01921 0.01542 = 0.01694 -0.00087 -0.00220 0.00146 C8 1 0.443323 0.054435 0.137625 11.00000 0.01907 0.02086 = 0.01975 -0.00135 -0.00275 -0.00081 AFIX 23 H8A 2 0.523804 0.041362 0.086582 11.00000 -1.20000 H8B 2 0.371497 0.038057 0.097244 11.00000 -1.20000 AFIX 0 C9 1 0.701859 -0.177404 0.388947 11.00000 0.01698 0.02624 = 0.01914 0.00369 -0.00687 -0.00036 C10 1 0.701094 -0.290369 0.455992 11.00000 0.02288 0.02785 = 0.02962 0.00347 -0.01117 0.00148 AFIX 137 H10A 2 0.636881 -0.285213 0.522072 11.00000 -1.50000 H10B 2 0.786012 -0.307036 0.478305 11.00000 -1.50000 H10C 2 0.679901 -0.350858 0.410329 11.00000 -1.50000 AFIX 0 C11 1 0.805217 -0.190696 0.287305 11.00000 0.01948 0.02926 = 0.02234 -0.00003 -0.00236 0.00382 AFIX 137 H11A 2 0.780537 -0.248527 0.240311 11.00000 -1.50000 H11B 2 0.887617 -0.213505 0.311894 11.00000 -1.50000 H11C 2 0.813230 -0.118509 0.245069 11.00000 -1.50000 AFIX 0 C12 1 0.736783 -0.084980 0.464290 11.00000 0.02499 0.03049 = 0.02305 -0.00453 -0.00727 -0.00195 AFIX 137 H12A 2 0.746291 -0.013131 0.421634 11.00000 -1.50000 H12B 2 0.817654 -0.107232 0.491904 11.00000 -1.50000 H12C 2 0.668474 -0.076164 0.526948 11.00000 -1.50000 AFIX 0 C13 1 0.234926 -0.270280 0.367728 11.00000 0.02009 0.02810 = 0.02579 0.00191 -0.00385 -0.00956 C14 1 0.186845 -0.309761 0.264360 11.00000 0.04781 0.05262 = 0.03474 -0.00053 -0.01241 -0.02861 AFIX 137 H14A 2 0.155924 -0.244195 0.222347 11.00000 -1.50000 H14B 2 0.116589 -0.361024 0.285977 11.00000 -1.50000 H14C 2 0.257099 -0.349455 0.218277 11.00000 -1.50000 AFIX 0 C15 1 0.127194 -0.202496 0.436779 11.00000 0.02769 0.04785 = 0.04893 -0.00089 0.00266 -0.01693 AFIX 137 H15A 2 0.158537 -0.176355 0.502768 11.00000 -1.50000 H15B 2 0.054254 -0.250656 0.459275 11.00000 -1.50000 H15C 2 0.099951 -0.137164 0.392416 11.00000 -1.50000 AFIX 0 C16 1 0.268715 -0.376010 0.436442 11.00000 0.03599 0.03377 = 0.05902 0.01744 -0.01378 -0.01831 AFIX 137 H16A 2 0.341675 -0.417789 0.395956 11.00000 -1.50000 H16B 2 0.194690 -0.424257 0.450003 11.00000 -1.50000 H16C 2 0.291389 -0.353597 0.507306 11.00000 -1.50000 AFIX 0 N20 3 0.432044 0.177269 0.163318 11.00000 0.01497 0.01867 = 0.01900 0.00078 -0.00119 0.00214 C21 1 0.298364 0.203430 0.216516 11.00000 0.01856 0.03069 = 0.01841 0.00133 -0.00183 0.00246 AFIX 23 H21A 2 0.281368 0.156121 0.285457 11.00000 -1.20000 H21B 2 0.238081 0.182309 0.166263 11.00000 -1.20000 AFIX 0 C22 1 0.271279 0.326218 0.244260 11.00000 0.02537 0.03499 = 0.03247 -0.00063 -0.00360 0.00928 AFIX 137 H22A 2 0.335856 0.350321 0.287820 11.00000 -1.50000 H22B 2 0.185866 0.334963 0.287260 11.00000 -1.50000 H22C 2 0.274586 0.372842 0.175656 11.00000 -1.50000 AFIX 0 C23 1 0.469699 0.246600 0.060703 11.00000 0.01967 0.02311 = 0.02011 0.00341 0.00159 0.00026 AFIX 23 H23A 2 0.561300 0.228657 0.034395 11.00000 -1.20000 H23B 2 0.462119 0.327150 0.079820 11.00000 -1.20000 AFIX 0 C24 1 0.393641 0.232339 -0.034927 11.00000 0.03608 0.02449 = 0.02209 0.00266 -0.00605 0.00144 AFIX 137 H24A 2 0.400451 0.153119 -0.055590 11.00000 -1.50000 H24B 2 0.428240 0.280279 -0.098566 11.00000 -1.50000 H24C 2 0.303356 0.254453 -0.012080 11.00000 -1.50000 AFIX 0 C31 1 0.820204 0.076238 0.023759 11.00000 0.02100 0.03013 = 0.02564 -0.00948 0.00041 0.00116 AFIX 137 H31A 2 0.768390 0.020177 0.068863 11.00000 -1.50000 H31B 2 0.894829 0.038060 -0.018224 11.00000 -1.50000 H31C 2 0.768363 0.116064 -0.027671 11.00000 -1.50000 AFIX 0 C32 1 0.957591 0.105692 0.226618 11.00000 0.02238 0.02996 = 0.02681 0.00172 -0.00292 -0.00263 AFIX 137 H32A 2 0.993110 0.161333 0.269659 11.00000 -1.50000 H32B 2 1.027066 0.055441 0.192464 11.00000 -1.50000 H32C 2 0.895517 0.061095 0.275640 11.00000 -1.50000 AFIX 0 C33 1 1.002934 0.259144 0.024774 11.00000 0.02038 0.03173 = 0.03483 -0.00331 0.00418 0.00012 AFIX 137 H33A 2 0.965906 0.296336 -0.037458 11.00000 -1.50000 H33B 2 1.072698 0.206043 -0.003462 11.00000 -1.50000 H33C 2 1.036615 0.316178 0.067461 11.00000 -1.50000 AFIX 0 C34 1 0.890464 0.468638 0.229361 11.00000 0.03165 0.03175 = 0.05872 -0.01259 -0.00306 -0.00837 AFIX 137 H34A 2 0.889533 0.437935 0.305333 11.00000 -1.50000 H34B 2 0.882225 0.551315 0.229833 11.00000 -1.50000 H34C 2 0.971447 0.445672 0.184749 11.00000 -1.50000 AFIX 0 C35 1 0.754891 0.472728 0.023390 11.00000 0.06076 0.02862 = 0.03395 0.01004 -0.00052 0.00475 AFIX 137 H35A 2 0.829600 0.440862 -0.023917 11.00000 -1.50000 H35B 2 0.759737 0.555107 0.022961 11.00000 -1.50000 H35C 2 0.676291 0.453361 -0.004694 11.00000 -1.50000 AFIX 0 C36 1 0.603186 0.477211 0.249660 11.00000 0.02883 0.01838 = 0.03571 -0.00523 -0.00590 0.00302 AFIX 137 H36A 2 0.527662 0.453935 0.219183 11.00000 -1.50000 H36B 2 0.606299 0.559799 0.244496 11.00000 -1.50000 H36C 2 0.597869 0.451130 0.327417 11.00000 -1.50000 HKLF 4 REM import in P -1 REM R1 = 0.0306 for 5938 Fo > 4sig(Fo) and 0.0391 for all 6818 data REM 294 parameters refined using 0 restraints END WGHT 0.0205 0.0000 REM Highest difference peak 0.90, deepest hole -0.90, 1-sigma level 0.13 Q1 1 0.5009 0.1953 0.2389 11.00000 0.05 0.90 Q2 1 0.5659 0.1959 0.3740 11.00000 0.05 0.82 Q3 1 0.5014 0.1535 0.3600 11.00000 0.05 0.77 Q4 1 0.6919 0.2349 0.2336 11.00000 0.05 0.75 Q5 1 0.6310 0.2200 0.1974 11.00000 0.05 0.71 Q6 1 0.5967 0.1485 0.3874 11.00000 0.05 0.64 Q7 1 0.9596 0.2143 0.0663 11.00000 0.05 0.63 Q8 1 0.6811 0.1996 0.3621 11.00000 0.05 0.62 Q9 1 0.5346 0.1583 0.2956 11.00000 0.05 0.59 Q10 1 0.6506 0.1425 0.2831 11.00000 0.05 0.57 Q11 1 0.8557 0.1167 0.0639 11.00000 0.05 0.57 Q12 1 0.7657 0.3849 0.0746 11.00000 0.05 0.56 Q13 1 0.7158 0.1628 0.2012 11.00000 0.05 0.56 Q14 1 0.5001 -0.0956 0.5604 11.00000 0.05 0.54 Q15 1 0.5404 0.2595 0.2915 11.00000 0.05 0.54 Q16 1 0.4064 -0.2304 0.3375 11.00000 0.05 0.53 Q17 1 0.4358 0.2168 0.1046 11.00000 0.05 0.51 Q18 1 0.0000 0.0000 0.5000 10.50000 0.05 0.51 Q19 1 0.7916 0.4579 0.0782 11.00000 0.05 0.51 Q20 1 0.5896 0.0137 0.2835 11.00000 0.05 0.50 ; #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.594071(14) 0.197655(11) 0.295740(12) 0.01754(5) Uani 1 1 d . . . Si1 Si 0.87578(10) 0.18042(8) 0.11625(9) 0.0190(2) Uani 1 1 d . . . Si2 Si 0.75306(11) 0.41314(8) 0.16845(10) 0.0225(2) Uani 1 1 d . . . N1 N 0.7502(3) 0.2681(2) 0.1749(3) 0.0177(7) Uani 1 1 d . . . O1 O 0.6522(2) 0.02368(19) 0.2536(2) 0.0186(6) Uani 1 1 d . . . C2 C 0.5564(3) -0.0490(3) 0.2807(3) 0.0165(8) Uani 1 1 d . . . C3 C 0.5720(3) -0.1465(3) 0.3496(3) 0.0160(8) Uani 1 1 d . . . C4 C 0.4671(3) -0.2151(3) 0.3758(3) 0.0182(8) Uani 1 1 d . . . H4 H 0.476 -0.2798 0.4233 0.022 Uiso 1 1 calc R . . C5 C 0.3494(3) -0.1940(3) 0.3360(3) 0.0189(8) Uani 1 1 d . . . C6 C 0.3415(3) -0.1012(3) 0.2630(3) 0.0181(8) Uani 1 1 d . . . H6 H 0.2644 -0.086 0.2319 0.022 Uiso 1 1 calc R . . C7 C 0.4431(3) -0.0299(3) 0.2341(3) 0.0173(8) Uani 1 1 d . . . C8 C 0.4433(4) 0.0544(3) 0.1376(3) 0.0199(8) Uani 1 1 d . . . H8A H 0.5238 0.0414 0.0866 0.024 Uiso 1 1 calc R . . H8B H 0.3715 0.0381 0.0972 0.024 Uiso 1 1 calc R . . C9 C 0.7019(3) -0.1774(3) 0.3889(3) 0.0205(8) Uani 1 1 d . . . C10 C 0.7011(4) -0.2904(3) 0.4560(3) 0.0263(9) Uani 1 1 d . . . H10A H 0.6369 -0.2852 0.5221 0.039 Uiso 1 1 calc R . . H10B H 0.786 -0.307 0.4783 0.039 Uiso 1 1 calc R . . H10C H 0.6799 -0.3509 0.4103 0.039 Uiso 1 1 calc R . . C11 C 0.8052(4) -0.1907(3) 0.2873(3) 0.0239(9) Uani 1 1 d . . . H11A H 0.7805 -0.2485 0.2403 0.036 Uiso 1 1 calc R . . H11B H 0.8876 -0.2135 0.3119 0.036 Uiso 1 1 calc R . . H11C H 0.8132 -0.1185 0.2451 0.036 Uiso 1 1 calc R . . C12 C 0.7368(4) -0.0850(3) 0.4643(3) 0.0257(9) Uani 1 1 d . . . H12A H 0.7463 -0.0131 0.4216 0.039 Uiso 1 1 calc R . . H12B H 0.8177 -0.1072 0.4919 0.039 Uiso 1 1 calc R . . H12C H 0.6685 -0.0762 0.5269 0.039 Uiso 1 1 calc R . . C13 C 0.2349(4) -0.2703(3) 0.3677(3) 0.0244(9) Uani 1 1 d . . . C14 C 0.1868(5) -0.3098(4) 0.2644(4) 0.0436(12) Uani 1 1 d . . . H14A H 0.1559 -0.2442 0.2223 0.065 Uiso 1 1 calc R . . H14B H 0.1166 -0.361 0.286 0.065 Uiso 1 1 calc R . . H14C H 0.2571 -0.3495 0.2183 0.065 Uiso 1 1 calc R . . C15 C 0.1272(4) -0.2025(4) 0.4368(4) 0.0418(12) Uani 1 1 d . . . H15A H 0.1585 -0.1764 0.5028 0.063 Uiso 1 1 calc R . . H15B H 0.0543 -0.2507 0.4593 0.063 Uiso 1 1 calc R . . H15C H 0.1 -0.1372 0.3924 0.063 Uiso 1 1 calc R . . C16 C 0.2687(4) -0.3760(3) 0.4364(4) 0.0423(12) Uani 1 1 d . . . H16A H 0.3417 -0.4178 0.396 0.063 Uiso 1 1 calc R . . H16B H 0.1947 -0.4243 0.45 0.063 Uiso 1 1 calc R . . H16C H 0.2914 -0.3536 0.5073 0.063 Uiso 1 1 calc R . . N20 N 0.4320(3) 0.1773(2) 0.1633(3) 0.0178(7) Uani 1 1 d . . . C21 C 0.2984(3) 0.2034(3) 0.2165(3) 0.0228(9) Uani 1 1 d . . . H21A H 0.2814 0.1561 0.2855 0.027 Uiso 1 1 calc R . . H21B H 0.2381 0.1823 0.1663 0.027 Uiso 1 1 calc R . . C22 C 0.2713(4) 0.3262(3) 0.2443(4) 0.0313(10) Uani 1 1 d . . . H22A H 0.3359 0.3503 0.2878 0.047 Uiso 1 1 calc R . . H22B H 0.1859 0.335 0.2873 0.047 Uiso 1 1 calc R . . H22C H 0.2746 0.3728 0.1757 0.047 Uiso 1 1 calc R . . C23 C 0.4697(4) 0.2466(3) 0.0607(3) 0.0215(8) Uani 1 1 d . . . H23A H 0.5613 0.2287 0.0344 0.026 Uiso 1 1 calc R . . H23B H 0.4621 0.3272 0.0798 0.026 Uiso 1 1 calc R . . C24 C 0.3936(4) 0.2323(3) -0.0349(3) 0.0276(9) Uani 1 1 d . . . H24A H 0.4005 0.1531 -0.0556 0.041 Uiso 1 1 calc R . . H24B H 0.4282 0.2803 -0.0986 0.041 Uiso 1 1 calc R . . H24C H 0.3034 0.2545 -0.0121 0.041 Uiso 1 1 calc R . . C31 C 0.8202(4) 0.0762(3) 0.0238(3) 0.0258(9) Uani 1 1 d . . . H31A H 0.7684 0.0202 0.0689 0.039 Uiso 1 1 calc R . . H31B H 0.8948 0.0381 -0.0182 0.039 Uiso 1 1 calc R . . H31C H 0.7684 0.1161 -0.0277 0.039 Uiso 1 1 calc R . . C32 C 0.9576(4) 0.1057(3) 0.2266(3) 0.0265(9) Uani 1 1 d . . . H32A H 0.9931 0.1613 0.2697 0.04 Uiso 1 1 calc R . . H32B H 1.0271 0.0554 0.1925 0.04 Uiso 1 1 calc R . . H32C H 0.8955 0.0611 0.2756 0.04 Uiso 1 1 calc R . . C33 C 1.0029(4) 0.2591(3) 0.0248(4) 0.0297(10) Uani 1 1 d . . . H33A H 0.9659 0.2963 -0.0375 0.045 Uiso 1 1 calc R . . H33B H 1.0727 0.206 -0.0035 0.045 Uiso 1 1 calc R . . H33C H 1.0366 0.3162 0.0675 0.045 Uiso 1 1 calc R . . C34 C 0.8905(4) 0.4686(3) 0.2294(4) 0.0405(12) Uani 1 1 d . . . H34A H 0.8895 0.4379 0.3053 0.061 Uiso 1 1 calc R . . H34B H 0.8822 0.5513 0.2298 0.061 Uiso 1 1 calc R . . H34C H 0.9714 0.4457 0.1847 0.061 Uiso 1 1 calc R . . C35 C 0.7549(5) 0.4727(3) 0.0234(4) 0.0422(12) Uani 1 1 d . . . H35A H 0.8296 0.4409 -0.0239 0.063 Uiso 1 1 calc R . . H35B H 0.7597 0.5551 0.023 0.063 Uiso 1 1 calc R . . H35C H 0.6763 0.4534 -0.0047 0.063 Uiso 1 1 calc R . . C36 C 0.6032(4) 0.4772(3) 0.2497(3) 0.0275(9) Uani 1 1 d . . . H36A H 0.5277 0.4539 0.2192 0.041 Uiso 1 1 calc R . . H36B H 0.6063 0.5598 0.2445 0.041 Uiso 1 1 calc R . . H36C H 0.5979 0.4511 0.3274 0.041 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 Pb1 0.01522(7) 0.01947(8) 0.01784(8) -0.00178(5) -0.00159(5) -0.00078(5) Si1 0.0151(5) 0.0195(5) 0.0219(6) -0.0021(4) -0.0002(4) -0.0013(4) Si2 0.0246(6) 0.0162(5) 0.0264(6) -0.0014(5) -0.0009(5) -0.0023(4) N1 0.0152(16) 0.0153(15) 0.0218(18) -0.0023(13) 0.0018(13) -0.0039(12) O1 0.0128(13) 0.0159(12) 0.0268(15) -0.0002(11) -0.0016(11) -0.0002(10) C2 0.0161(19) 0.0193(18) 0.0136(19) -0.0039(15) 0.0009(15) -0.0008(14) C3 0.0157(19) 0.0210(18) 0.0109(18) -0.0016(15) -0.0012(15) 0.0019(14) C4 0.021(2) 0.0173(18) 0.016(2) 0.0001(15) -0.0019(16) -0.0020(15) C5 0.017(2) 0.0184(18) 0.022(2) -0.0040(16) -0.0030(16) -0.0019(15) C6 0.0106(18) 0.0232(19) 0.022(2) -0.0016(16) -0.0069(16) -0.0006(14) C7 0.019(2) 0.0154(17) 0.017(2) -0.0009(15) -0.0022(16) 0.0015(14) C8 0.019(2) 0.0209(19) 0.020(2) -0.0013(16) -0.0027(16) -0.0008(15) C9 0.017(2) 0.026(2) 0.019(2) 0.0037(17) -0.0069(16) -0.0004(15) C10 0.023(2) 0.028(2) 0.030(2) 0.0035(18) -0.0112(18) 0.0015(17) C11 0.019(2) 0.029(2) 0.022(2) 0.0000(18) -0.0024(17) 0.0038(16) C12 0.025(2) 0.030(2) 0.023(2) -0.0045(18) -0.0073(18) -0.0020(17) C13 0.020(2) 0.028(2) 0.026(2) 0.0019(18) -0.0038(18) -0.0096(16) C14 0.048(3) 0.053(3) 0.035(3) -0.001(2) -0.012(2) -0.029(2) C15 0.028(3) 0.048(3) 0.049(3) -0.001(2) 0.003(2) -0.017(2) C16 0.036(3) 0.034(2) 0.059(3) 0.017(2) -0.014(2) -0.018(2) N20 0.0150(16) 0.0187(15) 0.0190(17) 0.0008(13) -0.0012(13) 0.0021(12) C21 0.019(2) 0.031(2) 0.018(2) 0.0013(17) -0.0018(16) 0.0025(16) C22 0.025(2) 0.035(2) 0.032(3) -0.001(2) -0.0036(19) 0.0093(18) C23 0.020(2) 0.0231(19) 0.020(2) 0.0034(17) 0.0016(16) 0.0003(15) C24 0.036(3) 0.024(2) 0.022(2) 0.0027(18) -0.0060(19) 0.0014(18) C31 0.021(2) 0.030(2) 0.026(2) -0.0095(18) 0.0004(18) 0.0012(17) C32 0.022(2) 0.030(2) 0.027(2) 0.0017(19) -0.0029(18) -0.0026(17) C33 0.020(2) 0.032(2) 0.035(3) -0.003(2) 0.0042(19) 0.0001(17) C34 0.032(3) 0.032(2) 0.059(3) -0.013(2) -0.003(2) -0.0084(19) C35 0.061(3) 0.029(2) 0.034(3) 0.010(2) -0.001(2) 0.005(2) C36 0.029(2) 0.0184(19) 0.036(3) -0.0052(18) -0.0059(19) 0.0030(16) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 O1 2.186(2) . ? Pb1 N1 2.218(3) . ? Pb1 N20 2.536(3) . ? Si1 N1 1.737(3) . ? Si1 C32 1.868(4) . ? Si1 C33 1.876(4) . ? Si1 C31 1.876(4) . ? Si2 N1 1.719(3) . ? Si2 C35 1.875(4) . ? Si2 C34 1.875(4) . ? Si2 C36 1.890(4) . ? O1 C2 1.354(4) . ? C2 C7 1.398(5) . ? C2 C3 1.416(5) . ? C3 C4 1.395(5) . ? C3 C9 1.535(5) . ? C4 C5 1.402(5) . ? C4 H4 0.95 . ? C5 C6 1.392(5) . ? C5 C13 1.538(5) . ? C6 C7 1.392(5) . ? C6 H6 0.95 . ? C7 C8 1.510(5) . ? C8 N20 1.499(4) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 C10 1.538(5) . ? C9 C11 1.541(5) . ? C9 C12 1.551(5) . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 H12A 0.98 . ? C12 H12B 0.98 . ? C12 H12C 0.98 . ? C13 C14 1.524(5) . ? C13 C16 1.532(5) . ? C13 C15 1.534(6) . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 H16A 0.98 . ? C16 H16B 0.98 . ? C16 H16C 0.98 . ? N20 C23 1.484(4) . ? N20 C21 1.491(4) . ? C21 C22 1.514(5) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 C24 1.525(5) . ? C23 H23A 0.99 . ? C23 H23B 0.99 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C31 H31A 0.98 . ? C31 H31B 0.98 . ? C31 H31C 0.98 . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? C33 H33A 0.98 . ? C33 H33B 0.98 . ? C33 H33C 0.98 . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pb1 N1 92.61(9) . . ? O1 Pb1 N20 83.97(9) . . ? N1 Pb1 N20 97.93(10) . . ? N1 Si1 C32 110.33(17) . . ? N1 Si1 C33 113.07(16) . . ? C32 Si1 C33 106.18(18) . . ? N1 Si1 C31 111.82(16) . . ? C32 Si1 C31 110.61(18) . . ? C33 Si1 C31 104.56(19) . . ? N1 Si2 C35 112.08(18) . . ? N1 Si2 C34 113.33(18) . . ? C35 Si2 C34 109.3(2) . . ? N1 Si2 C36 110.69(16) . . ? C35 Si2 C36 105.3(2) . . ? C34 Si2 C36 105.65(19) . . ? Si2 N1 Si1 123.63(17) . . ? Si2 N1 Pb1 114.75(15) . . ? Si1 N1 Pb1 120.26(15) . . ? C2 O1 Pb1 112.9(2) . . ? O1 C2 C7 118.7(3) . . ? O1 C2 C3 121.3(3) . . ? C7 C2 C3 119.9(3) . . ? C4 C3 C2 117.5(3) . . ? C4 C3 C9 121.9(3) . . ? C2 C3 C9 120.6(3) . . ? C3 C4 C5 123.8(3) . . ? C3 C4 H4 118.1 . . ? C5 C4 H4 118.1 . . ? C6 C5 C4 116.6(3) . . ? C6 C5 C13 120.9(3) . . ? C4 C5 C13 122.5(3) . . ? C5 C6 C7 122.0(3) . . ? C5 C6 H6 119 . . ? C7 C6 H6 119 . . ? C6 C7 C2 120.0(3) . . ? C6 C7 C8 120.8(3) . . ? C2 C7 C8 118.2(3) . . ? N20 C8 C7 117.3(3) . . ? N20 C8 H8A 108 . . ? C7 C8 H8A 108 . . ? N20 C8 H8B 108 . . ? C7 C8 H8B 108 . . ? H8A C8 H8B 107.2 . . ? C3 C9 C10 112.4(3) . . ? C3 C9 C11 109.2(3) . . ? C10 C9 C11 106.9(3) . . ? C3 C9 C12 110.1(3) . . ? C10 C9 C12 107.4(3) . . ? C11 C9 C12 110.9(3) . . ? C9 C10 H10A 109.5 . . ? C9 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C9 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C9 C11 H11A 109.5 . . ? C9 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C9 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C9 C12 H12A 109.5 . . ? C9 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C9 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C16 107.4(3) . . ? C14 C13 C15 109.5(4) . . ? C16 C13 C15 108.1(4) . . ? C14 C13 C5 110.5(3) . . ? C16 C13 C5 112.6(3) . . ? C15 C13 C5 108.5(3) . . ? C13 C14 H14A 109.5 . . ? C13 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C13 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C13 C15 H15A 109.5 . . ? C13 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C13 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C13 C16 H16A 109.5 . . ? C13 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C13 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C23 N20 C21 113.4(3) . . ? C23 N20 C8 109.6(3) . . ? C21 N20 C8 108.2(3) . . ? C23 N20 Pb1 109.3(2) . . ? C21 N20 Pb1 111.8(2) . . ? C8 N20 Pb1 104.1(2) . . ? N20 C21 C22 114.2(3) . . ? N20 C21 H21A 108.7 . . ? C22 C21 H21A 108.7 . . ? N20 C21 H21B 108.7 . . ? C22 C21 H21B 108.7 . . ? H21A C21 H21B 107.6 . . ? C21 C22 H22A 109.5 . . ? C21 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C21 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? N20 C23 C24 116.6(3) . . ? N20 C23 H23A 108.1 . . ? C24 C23 H23A 108.1 . . ? N20 C23 H23B 108.1 . . ? C24 C23 H23B 108.1 . . ? H23A C23 H23B 107.3 . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? Si1 C31 H31A 109.5 . . ? Si1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si1 C32 H32A 109.5 . . ? Si1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si1 C33 H33A 109.5 . . ? Si1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? 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 . . ? 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 C35 Si2 N1 Si1 66.3(3) . . . . ? C34 Si2 N1 Si1 -58.0(3) . . . . ? C36 Si2 N1 Si1 -176.5(2) . . . . ? C35 Si2 N1 Pb1 -127.1(2) . . . . ? C34 Si2 N1 Pb1 108.7(2) . . . . ? C36 Si2 N1 Pb1 -9.8(2) . . . . ? C32 Si1 N1 Si2 109.0(2) . . . . ? C33 Si1 N1 Si2 -9.8(3) . . . . ? C31 Si1 N1 Si2 -127.5(2) . . . . ? C32 Si1 N1 Pb1 -57.0(2) . . . . ? C33 Si1 N1 Pb1 -175.73(18) . . . . ? C31 Si1 N1 Pb1 66.6(2) . . . . ? O1 Pb1 N1 Si2 179.21(16) . . . . ? N20 Pb1 N1 Si2 94.94(17) . . . . ? O1 Pb1 N1 Si1 -13.66(18) . . . . ? N20 Pb1 N1 Si1 -97.93(18) . . . . ? N1 Pb1 O1 C2 -158.3(2) . . . . ? N20 Pb1 O1 C2 -60.6(2) . . . . ? Pb1 O1 C2 C7 59.1(4) . . . . ? Pb1 O1 C2 C3 -124.7(3) . . . . ? O1 C2 C3 C4 178.3(3) . . . . ? C7 C2 C3 C4 -5.5(5) . . . . ? O1 C2 C3 C9 -4.5(5) . . . . ? C7 C2 C3 C9 171.7(3) . . . . ? C2 C3 C4 C5 1.3(5) . . . . ? C9 C3 C4 C5 -175.8(3) . . . . ? C3 C4 C5 C6 2.6(5) . . . . ? C3 C4 C5 C13 -179.1(3) . . . . ? C4 C5 C6 C7 -2.6(5) . . . . ? C13 C5 C6 C7 179.1(3) . . . . ? C5 C6 C7 C2 -1.5(5) . . . . ? C5 C6 C7 C8 166.9(3) . . . . ? O1 C2 C7 C6 -178.0(3) . . . . ? C3 C2 C7 C6 5.6(5) . . . . ? O1 C2 C7 C8 13.2(5) . . . . ? C3 C2 C7 C8 -163.1(3) . . . . ? C6 C7 C8 N20 112.6(4) . . . . ? C2 C7 C8 N20 -78.7(4) . . . . ? C4 C3 C9 C10 1.1(5) . . . . ? C2 C3 C9 C10 -176.0(3) . . . . ? C4 C3 C9 C11 119.5(4) . . . . ? C2 C3 C9 C11 -57.6(4) . . . . ? C4 C3 C9 C12 -118.6(4) . . . . ? C2 C3 C9 C12 64.3(4) . . . . ? C6 C5 C13 C14 52.2(5) . . . . ? C4 C5 C13 C14 -126.0(4) . . . . ? C6 C5 C13 C16 172.4(4) . . . . ? C4 C5 C13 C16 -5.8(5) . . . . ? C6 C5 C13 C15 -67.9(5) . . . . ? C4 C5 C13 C15 113.9(4) . . . . ? C7 C8 N20 C23 164.4(3) . . . . ? C7 C8 N20 C21 -71.5(4) . . . . ? C7 C8 N20 Pb1 47.6(3) . . . . ? O1 Pb1 N20 C23 -108.7(2) . . . . ? N1 Pb1 N20 C23 -16.9(2) . . . . ? O1 Pb1 N20 C21 125.0(2) . . . . ? N1 Pb1 N20 C21 -143.2(2) . . . . ? O1 Pb1 N20 C8 8.4(2) . . . . ? N1 Pb1 N20 C8 100.2(2) . . . . ? C23 N20 C21 C22 -56.4(4) . . . . ? C8 N20 C21 C22 -178.2(3) . . . . ? Pb1 N20 C21 C22 67.6(3) . . . . ? C21 N20 C23 C24 -62.7(4) . . . . ? C8 N20 C23 C24 58.4(4) . . . . ? Pb1 N20 C23 C24 171.9(3) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 942090' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_SR31 _audit_creation_date 2012-03-20T10:22:45-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C50 H84 N2 O10 Pb, C6 H6' _chemical_formula_sum 'C56 H90 N2 O10 Pb' _chemical_formula_weight 1158.49 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 14.0101(4) _cell_length_b 27.8363(7) _cell_length_c 14.9256(4) _cell_angle_alpha 90 _cell_angle_beta 101.4870(10) _cell_angle_gamma 90 _cell_volume 5704.2(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9903 _cell_measurement_theta_min 2.6 _cell_measurement_theta_max 27.1 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description stick _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.1 _exptl_crystal_size_min 0.09 _exptl_crystal_density_diffrn 1.349 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2408 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 3.013 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.659 _exptl_absorpt_correction_T_max 0.763 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0354 _diffrn_reflns_av_unetI/netI 0.0417 _diffrn_reflns_number 48821 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -33 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.44 _diffrn_reflns_theta_full 27.44 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _reflns_number_total 12869 _reflns_number_gt 10211 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0230P)^2^+5.0935P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 12869 _refine_ls_number_parameters 634 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.046 _refine_ls_R_factor_gt 0.029 _refine_ls_wR_factor_ref 0.0617 _refine_ls_wR_factor_gt 0.0572 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.009 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.918 _refine_diff_density_min -0.81 _refine_diff_density_rms 0.083 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.640989(8) 0.281957(4) 0.412122(7) 0.02110(4) Uani 1 1 d . . . O1 O 0.57731(14) 0.31212(7) 0.27315(12) 0.0225(4) Uani 1 1 d . . . N1 N 0.48038(17) 0.32767(8) 0.44890(14) 0.0182(5) Uani 1 1 d . . . C2 C 0.4453(2) 0.29783(10) 0.51798(17) 0.0218(6) Uani 1 1 d . . . H2A H 0.4367 0.2645 0.4948 0.026 Uiso 1 1 calc R . . H2B H 0.3805 0.3098 0.5245 0.026 Uiso 1 1 calc R . . C3 C 0.5111(2) 0.29697(10) 0.61160(18) 0.0273(7) Uani 1 1 d . . . H3A H 0.4969 0.2683 0.6458 0.033 Uiso 1 1 calc R . . H3B H 0.5801 0.2955 0.6054 0.033 Uiso 1 1 calc R . . O4 O 0.49438(17) 0.33933(8) 0.65926(13) 0.0367(5) Uani 1 1 d . . . C5 C 0.5532(2) 0.34458(12) 0.74734(19) 0.0342(8) Uani 1 1 d . . . H5A H 0.6228 0.3411 0.7445 0.041 Uiso 1 1 calc R . . H5B H 0.5365 0.3198 0.7892 0.041 Uiso 1 1 calc R . . C6 C 0.5336(3) 0.39408(12) 0.7807(2) 0.0385(8) Uani 1 1 d . . . H6A H 0.5814 0.4018 0.8372 0.046 Uiso 1 1 calc R . . H6B H 0.5395 0.4184 0.7337 0.046 Uiso 1 1 calc R . . O7 O 0.43854(18) 0.39429(8) 0.79833(16) 0.0429(6) Uani 1 1 d . . . C8 C 0.4018(3) 0.43957(13) 0.8225(2) 0.0460(9) Uani 1 1 d . . . H8A H 0.437 0.4483 0.8846 0.055 Uiso 1 1 calc R . . H8B H 0.3323 0.4354 0.8253 0.055 Uiso 1 1 calc R . . C9 C 0.4100(3) 0.48051(13) 0.7599(2) 0.0436(9) Uani 1 1 d . . . H9A H 0.3759 0.5088 0.7786 0.052 Uiso 1 1 calc R . . H9B H 0.4795 0.4891 0.7652 0.052 Uiso 1 1 calc R . . O10 O 0.37001(19) 0.46928(9) 0.66874(17) 0.0487(6) Uani 1 1 d . . . C11 C 0.3865(3) 0.50711(13) 0.6091(3) 0.0481(10) Uani 1 1 d . . . H11A H 0.4552 0.5179 0.6249 0.058 Uiso 1 1 calc R . . H11B H 0.3439 0.5348 0.6149 0.058 Uiso 1 1 calc R . . C12 C 0.3640(3) 0.48794(13) 0.5140(3) 0.0542(11) Uani 1 1 d . . . H12A H 0.2999 0.4717 0.5035 0.065 Uiso 1 1 calc R . . H12B H 0.3594 0.515 0.4704 0.065 Uiso 1 1 calc R . . O13 O 0.4359(2) 0.45481(9) 0.4963(2) 0.0706(9) Uani 1 1 d . . . C14 C 0.4091(2) 0.40689(10) 0.4915(2) 0.0287(7) Uani 1 1 d . . . H14A H 0.3525 0.4017 0.4409 0.034 Uiso 1 1 calc R . . H14B H 0.3912 0.3965 0.5494 0.034 Uiso 1 1 calc R . . C15 C 0.4969(2) 0.37867(10) 0.47445(18) 0.0229(6) Uani 1 1 d . . . H15A H 0.5225 0.395 0.4252 0.028 Uiso 1 1 calc R . . H15B H 0.5482 0.3803 0.5305 0.028 Uiso 1 1 calc R . . O21 O 0.53502(14) 0.21719(7) 0.38402(13) 0.0244(4) Uani 1 1 d . . . N21 N 0.73285(19) 0.22334(9) 0.3148(2) 0.0343(6) Uani 1 1 d . . . C22 C 0.7908(3) 0.25435(12) 0.2647(3) 0.0467(10) Uani 1 1 d . . . H22A H 0.7459 0.2756 0.2228 0.056 Uiso 1 1 calc R . . H22B H 0.8248 0.2338 0.2269 0.056 Uiso 1 1 calc R . . C23 C 0.8652(3) 0.28495(13) 0.3269(3) 0.0573(12) Uani 1 1 d . . . H23A H 0.9066 0.2644 0.3732 0.069 Uiso 1 1 calc R . . H23B H 0.9076 0.3014 0.2908 0.069 Uiso 1 1 calc R . . O24 O 0.81587(16) 0.31937(8) 0.37076(16) 0.0394(6) Uani 1 1 d . . . C25 C 0.8798(3) 0.34826(17) 0.4362(4) 0.0689(13) Uani 1 1 d . . . H25A H 0.9372 0.3579 0.411 0.083 Uiso 1 1 calc R . . H25B H 0.9031 0.3295 0.4926 0.083 Uiso 1 1 calc R . . C26 C 0.8269(3) 0.39178(15) 0.4579(3) 0.0583(11) Uani 1 1 d . . . H26A H 0.8735 0.4132 0.4977 0.07 Uiso 1 1 calc R . . H26B H 0.8015 0.4093 0.4004 0.07 Uiso 1 1 calc R . . O27 O 0.7489(2) 0.38176(10) 0.50156(16) 0.0548(7) Uani 1 1 d . . . C28 C 0.7631(4) 0.38727(18) 0.5978(3) 0.0722(14) Uani 1 1 d . . . H28A H 0.6989 0.387 0.6161 0.087 Uiso 1 1 calc R . . H28B H 0.7939 0.4188 0.6152 0.087 Uiso 1 1 calc R . . C29 C 0.8263(4) 0.3480(2) 0.6491(3) 0.0782(15) Uani 1 1 d . . . H29A H 0.8929 0.3501 0.6366 0.094 Uiso 1 1 calc R . . H29B H 0.8305 0.3519 0.7157 0.094 Uiso 1 1 calc R . . O30 O 0.7849(2) 0.30243(13) 0.62048(19) 0.0679(9) Uani 1 1 d . . . C31 C 0.8479(4) 0.2631(2) 0.6520(3) 0.0938(19) Uani 1 1 d . . . H31A H 0.8546 0.2594 0.7189 0.113 Uiso 1 1 calc R . . H31B H 0.9133 0.2691 0.6387 0.113 Uiso 1 1 calc R . . C32 C 0.8057(4) 0.2184(2) 0.6047(3) 0.0873(18) Uani 1 1 d . . . H32A H 0.8419 0.1899 0.6334 0.105 Uiso 1 1 calc R . . H32B H 0.7367 0.215 0.61 0.105 Uiso 1 1 calc R . . O33 O 0.81264(19) 0.22127(10) 0.5104(2) 0.0580(8) Uani 1 1 d . . . C34 C 0.7826(3) 0.17790(15) 0.4615(3) 0.0632(13) Uani 1 1 d . . . H34A H 0.7136 0.171 0.4627 0.076 Uiso 1 1 calc R . . H34B H 0.8228 0.1506 0.4901 0.076 Uiso 1 1 calc R . . C35 C 0.7951(3) 0.18445(13) 0.3651(3) 0.0504(10) Uani 1 1 d . . . H35A H 0.7794 0.1538 0.3318 0.06 Uiso 1 1 calc R . . H35B H 0.8642 0.192 0.3655 0.06 Uiso 1 1 calc R . . C41 C 0.4114(2) 0.32146(10) 0.35950(17) 0.0186(6) Uani 1 1 d . . . H41A H 0.3443 0.3273 0.3688 0.022 Uiso 1 1 calc R . . H41B H 0.4148 0.2877 0.3393 0.022 Uiso 1 1 calc R . . C42 C 0.43051(19) 0.35416(9) 0.28439(17) 0.0169(5) Uani 1 1 d . . . C43 C 0.5132(2) 0.34700(9) 0.24399(17) 0.0179(6) Uani 1 1 d . . . C44 C 0.5224(2) 0.37666(9) 0.16820(17) 0.0196(6) Uani 1 1 d . . . C45 C 0.4521(2) 0.41182(10) 0.13934(18) 0.0216(6) Uani 1 1 d . . . H45 H 0.4596 0.4315 0.0892 0.026 Uiso 1 1 calc R . . C46 C 0.3716(2) 0.42009(9) 0.17908(18) 0.0193(6) Uani 1 1 d . . . C47 C 0.3625(2) 0.38984(9) 0.25163(17) 0.0193(6) Uani 1 1 d . . . H47 H 0.3078 0.3937 0.2797 0.023 Uiso 1 1 calc R . . C48 C 0.6065(2) 0.36919(11) 0.11734(19) 0.0271(7) Uani 1 1 d . . . C49 C 0.7045(2) 0.37694(11) 0.1833(2) 0.0331(7) Uani 1 1 d . . . H49A H 0.7107 0.4107 0.2019 0.05 Uiso 1 1 calc R . . H49B H 0.7578 0.3684 0.1526 0.05 Uiso 1 1 calc R . . H49C H 0.7076 0.3566 0.2374 0.05 Uiso 1 1 calc R . . C50 C 0.5998(3) 0.31825(12) 0.0758(2) 0.0378(8) Uani 1 1 d . . . H50A H 0.5998 0.2945 0.1242 0.057 Uiso 1 1 calc R . . H50B H 0.6558 0.3126 0.0469 0.057 Uiso 1 1 calc R . . H50C H 0.5395 0.3153 0.0298 0.057 Uiso 1 1 calc R . . C51 C 0.6031(3) 0.40459(13) 0.0375(2) 0.0414(9) Uani 1 1 d . . . H51A H 0.5419 0.4004 -0.0068 0.062 Uiso 1 1 calc R . . H51B H 0.6581 0.3984 0.0076 0.062 Uiso 1 1 calc R . . H51C H 0.6071 0.4376 0.0609 0.062 Uiso 1 1 calc R . . C52 C 0.2954(2) 0.45917(10) 0.14598(19) 0.0226(6) Uani 1 1 d . . . C53 C 0.2881(2) 0.49265(11) 0.2272(2) 0.0327(7) Uani 1 1 d . . . H53A H 0.2645 0.4743 0.2744 0.049 Uiso 1 1 calc R . . H53B H 0.2427 0.5189 0.2057 0.049 Uiso 1 1 calc R . . H53C H 0.3525 0.5059 0.2528 0.049 Uiso 1 1 calc R . . C54 C 0.1962(2) 0.43647(12) 0.1094(2) 0.0344(7) Uani 1 1 d . . . H54A H 0.1998 0.4167 0.0558 0.052 Uiso 1 1 calc R . . H54B H 0.1475 0.4618 0.092 0.052 Uiso 1 1 calc R . . H54C H 0.1776 0.4163 0.1569 0.052 Uiso 1 1 calc R . . C55 C 0.3225(2) 0.48990(11) 0.0694(2) 0.0342(8) Uani 1 1 d . . . H55A H 0.3857 0.5053 0.0916 0.051 Uiso 1 1 calc R . . H55B H 0.2727 0.5146 0.051 0.051 Uiso 1 1 calc R . . H55C H 0.3264 0.4694 0.0169 0.051 Uiso 1 1 calc R . . C61 C 0.6499(2) 0.20332(11) 0.2474(2) 0.0318(7) Uani 1 1 d . . . H61A H 0.6749 0.1912 0.1941 0.038 Uiso 1 1 calc R . . H61B H 0.6037 0.2297 0.2255 0.038 Uiso 1 1 calc R . . C62 C 0.5954(2) 0.16353(10) 0.28268(19) 0.0250(6) Uani 1 1 d . . . C63 C 0.6004(2) 0.11720(11) 0.2485(2) 0.0290(7) Uani 1 1 d . . . H63 H 0.6379 0.112 0.2029 0.035 Uiso 1 1 calc R . . C64 C 0.5534(2) 0.07838(10) 0.2782(2) 0.0268(7) Uani 1 1 d . . . C65 C 0.5010(2) 0.08809(10) 0.34717(19) 0.0252(6) Uani 1 1 d . . . H65 H 0.4688 0.062 0.3696 0.03 Uiso 1 1 calc R . . C66 C 0.4927(2) 0.13332(10) 0.38493(18) 0.0217(6) Uani 1 1 d . . . C67 C 0.5409(2) 0.17303(10) 0.35202(18) 0.0214(6) Uani 1 1 d . . . C68 C 0.5622(2) 0.02702(11) 0.2427(2) 0.0327(7) Uani 1 1 d . . . C69 C 0.6272(4) -0.00226(14) 0.3185(3) 0.0689(13) Uani 1 1 d . . . H69A H 0.5969 -0.0036 0.3722 0.103 Uiso 1 1 calc R . . H69B H 0.6912 0.0131 0.3351 0.103 Uiso 1 1 calc R . . H69C H 0.6349 -0.0349 0.2964 0.103 Uiso 1 1 calc R . . C70 C 0.4632(3) 0.00348(15) 0.2186(4) 0.0807(17) Uani 1 1 d . . . H70A H 0.4359 0.0002 0.2739 0.121 Uiso 1 1 calc R . . H70B H 0.4697 -0.0284 0.1925 0.121 Uiso 1 1 calc R . . H70C H 0.4198 0.0233 0.1739 0.121 Uiso 1 1 calc R . . C71 C 0.6088(4) 0.02621(14) 0.1584(3) 0.0685(14) Uani 1 1 d . . . H71A H 0.6106 -0.0069 0.1364 0.103 Uiso 1 1 calc R . . H71B H 0.6753 0.0388 0.1746 0.103 Uiso 1 1 calc R . . H71C H 0.5705 0.0462 0.1103 0.103 Uiso 1 1 calc R . . C72 C 0.4326(2) 0.14042(10) 0.45974(19) 0.0248(6) Uani 1 1 d . . . C73 C 0.3454(2) 0.17373(11) 0.4234(2) 0.0310(7) Uani 1 1 d . . . H73A H 0.369 0.2036 0.4005 0.047 Uiso 1 1 calc R . . H73B H 0.3113 0.1812 0.473 0.047 Uiso 1 1 calc R . . H73C H 0.3006 0.1576 0.3737 0.047 Uiso 1 1 calc R . . C74 C 0.4963(2) 0.16213(11) 0.54609(19) 0.0318(7) Uani 1 1 d . . . H74A H 0.5481 0.1394 0.5716 0.048 Uiso 1 1 calc R . . H74B H 0.4561 0.1686 0.5914 0.048 Uiso 1 1 calc R . . H74C H 0.5254 0.1922 0.5303 0.048 Uiso 1 1 calc R . . C75 C 0.3914(3) 0.09296(11) 0.4886(2) 0.0413(9) Uani 1 1 d . . . H75A H 0.3499 0.078 0.4352 0.062 Uiso 1 1 calc R . . H75B H 0.3528 0.0994 0.5353 0.062 Uiso 1 1 calc R . . H75C H 0.4452 0.0712 0.5135 0.062 Uiso 1 1 calc R . . C81 C 0.1472(3) 0.27830(18) 0.3884(4) 0.0663(13) Uani 1 1 d . . . H81 H 0.1515 0.2443 0.3845 0.08 Uiso 1 1 calc R . . C82 C 0.1255(3) 0.3067(3) 0.3083(4) 0.092(2) Uani 1 1 d . . . H82 H 0.1155 0.2925 0.2494 0.11 Uiso 1 1 calc R . . C83 C 0.1191(3) 0.3566(2) 0.3189(4) 0.0786(18) Uani 1 1 d . . . H83 H 0.1032 0.3765 0.2663 0.094 Uiso 1 1 calc R . . C84 C 0.1353(3) 0.37680(18) 0.4023(4) 0.0689(14) Uani 1 1 d . . . H84 H 0.1314 0.4107 0.4083 0.083 Uiso 1 1 calc R . . C85 C 0.1571(3) 0.34895(17) 0.4773(3) 0.0600(11) Uani 1 1 d . . . H85 H 0.1695 0.3635 0.5361 0.072 Uiso 1 1 calc R . . C86 C 0.1617(3) 0.30059(16) 0.4706(3) 0.0561(11) Uani 1 1 d . . . H86 H 0.1755 0.2818 0.5248 0.067 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Pb1 0.01673(6) 0.01962(6) 0.02639(5) 0.00635(5) 0.00290(4) 0.00066(5) O1 0.0210(11) 0.0229(10) 0.0247(10) 0.0056(8) 0.0074(8) 0.0053(9) N1 0.0209(13) 0.0152(11) 0.0177(10) 0.0019(9) 0.0022(9) -0.0004(9) C2 0.0267(17) 0.0198(14) 0.0195(13) 0.0023(11) 0.0057(12) 0.0001(12) C3 0.0385(19) 0.0220(15) 0.0219(14) 0.0022(11) 0.0068(13) 0.0056(13) O4 0.0555(16) 0.0293(12) 0.0204(10) -0.0045(9) -0.0040(10) 0.0120(11) C5 0.036(2) 0.047(2) 0.0179(14) -0.0025(13) 0.0014(13) 0.0000(16) C6 0.043(2) 0.044(2) 0.0303(16) -0.0096(14) 0.0119(15) -0.0102(17) O7 0.0510(16) 0.0339(13) 0.0522(14) -0.0038(11) 0.0303(12) -0.0039(11) C8 0.051(2) 0.043(2) 0.048(2) -0.0003(17) 0.0188(18) 0.0045(18) C9 0.052(2) 0.036(2) 0.044(2) -0.0091(16) 0.0121(18) 0.0017(17) O10 0.0509(17) 0.0435(15) 0.0515(15) 0.0088(12) 0.0096(13) -0.0055(12) C11 0.060(3) 0.0300(19) 0.059(2) 0.0134(17) 0.024(2) 0.0109(18) C12 0.072(3) 0.0262(19) 0.069(3) -0.0030(18) 0.026(2) 0.0140(19) O13 0.071(2) 0.0217(13) 0.133(3) -0.0180(15) 0.053(2) -0.0048(13) C14 0.0365(19) 0.0173(15) 0.0303(15) -0.0029(12) 0.0018(14) 0.0017(13) C15 0.0263(17) 0.0189(14) 0.0222(13) -0.0022(11) 0.0015(12) -0.0033(12) O21 0.0252(11) 0.0156(9) 0.0352(10) -0.0009(9) 0.0130(9) -0.0010(9) N21 0.0253(15) 0.0214(14) 0.0619(18) 0.0087(12) 0.0225(13) 0.0048(11) C22 0.044(2) 0.0295(19) 0.079(3) 0.0057(18) 0.043(2) 0.0001(17) C23 0.030(2) 0.037(2) 0.113(4) 0.012(2) 0.034(2) 0.0002(18) O24 0.0203(12) 0.0376(13) 0.0601(15) 0.0098(11) 0.0073(11) -0.0043(10) C25 0.026(2) 0.074(3) 0.104(4) -0.005(3) 0.008(2) -0.014(2) C26 0.047(3) 0.055(3) 0.073(3) 0.001(2) 0.014(2) -0.025(2) O27 0.0593(18) 0.0663(18) 0.0366(13) 0.0004(12) 0.0040(13) -0.0294(15) C28 0.064(3) 0.092(4) 0.054(3) -0.005(2) -0.004(2) -0.027(3) C29 0.057(3) 0.119(5) 0.046(2) -0.001(3) -0.022(2) -0.007(3) O30 0.0512(19) 0.098(2) 0.0452(16) 0.0215(16) -0.0135(14) 0.0061(17) C31 0.084(4) 0.125(5) 0.058(3) 0.046(3) -0.023(3) 0.017(4) C32 0.075(4) 0.103(4) 0.078(3) 0.065(3) -0.001(3) 0.025(3) O33 0.0405(16) 0.0596(19) 0.0704(18) 0.0396(15) 0.0029(14) 0.0124(14) C34 0.030(2) 0.045(2) 0.111(4) 0.049(3) 0.004(2) 0.0111(19) C35 0.0218(19) 0.031(2) 0.100(3) 0.014(2) 0.017(2) 0.0106(15) C41 0.0184(15) 0.0178(14) 0.0196(13) 0.0015(10) 0.0039(11) 0.0011(11) C42 0.0176(15) 0.0147(13) 0.0174(12) -0.0005(10) 0.0010(11) -0.0027(11) C43 0.0181(15) 0.0159(13) 0.0193(12) 0.0002(10) 0.0028(11) -0.0007(11) C44 0.0215(16) 0.0175(14) 0.0203(13) 0.0014(11) 0.0055(11) 0.0006(12) C45 0.0249(17) 0.0204(14) 0.0197(13) 0.0037(11) 0.0048(12) -0.0019(12) C46 0.0183(15) 0.0160(14) 0.0225(13) -0.0006(10) 0.0018(11) -0.0017(11) C47 0.0142(15) 0.0216(14) 0.0223(13) -0.0018(11) 0.0037(11) -0.0007(11) C48 0.0278(18) 0.0296(16) 0.0276(15) 0.0091(12) 0.0146(13) 0.0061(13) C49 0.0255(18) 0.0278(17) 0.0494(19) 0.0123(14) 0.0155(15) 0.0031(14) C50 0.043(2) 0.041(2) 0.0349(17) -0.0009(15) 0.0214(16) 0.0074(16) C51 0.041(2) 0.050(2) 0.0404(18) 0.0212(16) 0.0252(16) 0.0127(17) C52 0.0202(16) 0.0218(15) 0.0262(14) 0.0069(11) 0.0058(12) 0.0042(12) C53 0.0302(19) 0.0269(17) 0.0422(18) 0.0031(14) 0.0098(15) 0.0081(14) C54 0.0240(18) 0.0347(19) 0.0418(18) 0.0063(14) 0.0006(14) 0.0031(14) C55 0.0340(19) 0.0313(18) 0.0389(17) 0.0173(14) 0.0113(15) 0.0113(15) C61 0.036(2) 0.0235(16) 0.0431(18) 0.0020(13) 0.0253(15) 0.0013(14) C62 0.0282(17) 0.0189(15) 0.0308(15) 0.0022(12) 0.0131(13) 0.0020(12) C63 0.0313(19) 0.0258(16) 0.0333(16) 0.0017(13) 0.0148(14) 0.0035(14) C64 0.0263(18) 0.0204(15) 0.0347(16) -0.0002(12) 0.0090(13) 0.0032(13) C65 0.0231(17) 0.0196(15) 0.0336(15) 0.0026(12) 0.0069(13) -0.0021(12) C66 0.0206(16) 0.0177(14) 0.0271(14) 0.0024(11) 0.0058(12) 0.0023(12) C67 0.0202(16) 0.0165(14) 0.0275(14) 0.0027(11) 0.0053(12) 0.0035(12) C68 0.0307(19) 0.0199(15) 0.051(2) -0.0041(14) 0.0168(16) 0.0014(14) C69 0.089(4) 0.032(2) 0.085(3) 0.000(2) 0.017(3) 0.022(2) C70 0.053(3) 0.047(3) 0.152(5) -0.059(3) 0.044(3) -0.017(2) C71 0.098(4) 0.038(2) 0.084(3) -0.022(2) 0.052(3) -0.006(2) C72 0.0263(17) 0.0198(15) 0.0311(15) 0.0012(12) 0.0122(13) -0.0007(12) C73 0.0242(18) 0.0306(17) 0.0398(17) -0.0071(14) 0.0097(14) -0.0016(14) C74 0.038(2) 0.0317(18) 0.0281(15) 0.0056(13) 0.0116(14) 0.0061(15) C75 0.055(2) 0.0276(18) 0.052(2) 0.0009(15) 0.0354(18) -0.0052(16) C81 0.038(3) 0.070(3) 0.087(4) -0.007(3) 0.003(2) -0.013(2) C82 0.034(3) 0.178(7) 0.063(3) -0.033(4) 0.008(2) -0.039(4) C83 0.034(3) 0.132(5) 0.067(3) 0.054(3) 0.002(2) -0.016(3) C84 0.035(2) 0.070(3) 0.101(4) 0.038(3) 0.011(2) 0.002(2) C85 0.046(3) 0.068(3) 0.068(3) 0.008(2) 0.016(2) -0.002(2) C86 0.043(2) 0.060(3) 0.061(3) 0.020(2) 0.000(2) -0.008(2) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 O1 2.2509(18) . ? Pb1 O21 2.3201(19) . ? Pb1 N21 2.678(3) . ? Pb1 N1 2.734(2) . ? O1 C43 1.336(3) . ? N1 C15 1.476(3) . ? N1 C2 1.482(3) . ? N1 C41 1.494(3) . ? C2 C3 1.513(4) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 O4 1.420(3) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? O4 C5 1.413(3) . ? C5 C6 1.509(4) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 O7 1.408(4) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? O7 C8 1.434(4) . ? C8 C9 1.493(5) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 O10 1.399(4) . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? O10 C11 1.427(4) . ? C11 C12 1.491(5) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 O13 1.428(4) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? O13 C14 1.384(4) . ? C14 C15 1.523(4) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? O21 C67 1.327(3) . ? N21 C22 1.485(4) . ? N21 C61 1.486(4) . ? N21 C35 1.495(4) . ? C22 C23 1.513(6) . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? C23 O24 1.416(4) . ? C23 H23A 0.99 . ? C23 H23B 0.99 . ? O24 C25 1.433(5) . ? C25 C26 1.490(6) . ? C25 H25A 0.99 . ? C25 H25B 0.99 . ? C26 O27 1.407(4) . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? O27 C28 1.419(5) . ? C28 C29 1.515(7) . ? C28 H28A 0.99 . ? C28 H28B 0.99 . ? C29 O30 1.425(6) . ? C29 H29A 0.99 . ? C29 H29B 0.99 . ? O30 C31 1.426(6) . ? C31 C32 1.494(7) . ? C31 H31A 0.99 . ? C31 H31B 0.99 . ? C32 O33 1.432(6) . ? C32 H32A 0.99 . ? C32 H32B 0.99 . ? O33 C34 1.430(5) . ? C34 C35 1.494(6) . ? C34 H34A 0.99 . ? C34 H34B 0.99 . ? C35 H35A 0.99 . ? C35 H35B 0.99 . ? C41 C42 1.509(3) . ? C41 H41A 0.99 . ? C41 H41B 0.99 . ? C42 C47 1.396(4) . ? C42 C43 1.422(4) . ? C43 C44 1.427(3) . ? C44 C45 1.394(4) . ? C44 C48 1.537(4) . ? C45 C46 1.394(4) . ? C45 H45 0.95 . ? C46 C47 1.398(4) . ? C46 C52 1.536(4) . ? C47 H47 0.95 . ? C48 C49 1.537(4) . ? C48 C51 1.539(4) . ? C48 C50 1.543(4) . ? C49 H49A 0.98 . ? C49 H49B 0.98 . ? C49 H49C 0.98 . ? C50 H50A 0.98 . ? C50 H50B 0.98 . ? C50 H50C 0.98 . ? C51 H51A 0.98 . ? C51 H51B 0.98 . ? C51 H51C 0.98 . ? C52 C54 1.525(4) . ? C52 C55 1.534(4) . ? C52 C53 1.548(4) . ? C53 H53A 0.98 . ? C53 H53B 0.98 . ? C53 H53C 0.98 . ? C54 H54A 0.98 . ? C54 H54B 0.98 . ? C54 H54C 0.98 . ? C55 H55A 0.98 . ? C55 H55B 0.98 . ? C55 H55C 0.98 . ? C61 C62 1.500(4) . ? C61 H61A 0.99 . ? C61 H61B 0.99 . ? C62 C63 1.394(4) . ? C62 C67 1.428(4) . ? C63 C64 1.384(4) . ? C63 H63 0.95 . ? C64 C65 1.405(4) . ? C64 C68 1.538(4) . ? C65 C66 1.394(4) . ? C65 H65 0.95 . ? C66 C67 1.432(4) . ? C66 C72 1.539(4) . ? C68 C70 1.511(5) . ? C68 C71 1.529(5) . ? C68 C69 1.537(5) . ? C69 H69A 0.98 . ? C69 H69B 0.98 . ? C69 H69C 0.98 . ? C70 H70A 0.98 . ? C70 H70B 0.98 . ? C70 H70C 0.98 . ? C71 H71A 0.98 . ? C71 H71B 0.98 . ? C71 H71C 0.98 . ? C72 C75 1.537(4) . ? C72 C74 1.538(4) . ? C72 C73 1.544(4) . ? C73 H73A 0.98 . ? C73 H73B 0.98 . ? C73 H73C 0.98 . ? C74 H74A 0.98 . ? C74 H74B 0.98 . ? C74 H74C 0.98 . ? C75 H75A 0.98 . ? C75 H75B 0.98 . ? C75 H75C 0.98 . ? C81 C86 1.354(6) . ? C81 C82 1.414(8) . ? C81 H81 0.95 . ? C82 C83 1.403(8) . ? C82 H82 0.95 . ? C83 C84 1.342(7) . ? C83 H83 0.95 . ? C84 C85 1.346(6) . ? C84 H84 0.95 . ? C85 C86 1.352(6) . ? C85 H85 0.95 . ? C86 H86 0.95 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Pb1 O21 90.08(7) . . ? O1 Pb1 N21 82.68(8) . . ? O21 Pb1 N21 77.75(7) . . ? O1 Pb1 N1 79.65(6) . . ? O21 Pb1 N1 82.84(7) . . ? N21 Pb1 N1 153.64(8) . . ? C43 O1 Pb1 133.55(16) . . ? C15 N1 C2 114.6(2) . . ? C15 N1 C41 112.5(2) . . ? C2 N1 C41 108.1(2) . . ? C15 N1 Pb1 113.99(16) . . ? C2 N1 Pb1 106.22(16) . . ? C41 N1 Pb1 100.30(14) . . ? N1 C2 C3 115.2(2) . . ? N1 C2 H2A 108.5 . . ? C3 C2 H2A 108.5 . . ? N1 C2 H2B 108.5 . . ? C3 C2 H2B 108.5 . . ? H2A C2 H2B 107.5 . . ? O4 C3 C2 108.6(2) . . ? O4 C3 H3A 110 . . ? C2 C3 H3A 110 . . ? O4 C3 H3B 110 . . ? C2 C3 H3B 110 . . ? H3A C3 H3B 108.4 . . ? C5 O4 C3 115.4(2) . . ? O4 C5 C6 106.9(3) . . ? O4 C5 H5A 110.3 . . ? C6 C5 H5A 110.3 . . ? O4 C5 H5B 110.3 . . ? C6 C5 H5B 110.3 . . ? H5A C5 H5B 108.6 . . ? O7 C6 C5 107.8(3) . . ? O7 C6 H6A 110.1 . . ? C5 C6 H6A 110.1 . . ? O7 C6 H6B 110.1 . . ? C5 C6 H6B 110.1 . . ? H6A C6 H6B 108.5 . . ? C6 O7 C8 116.8(3) . . ? O7 C8 C9 115.9(3) . . ? O7 C8 H8A 108.3 . . ? C9 C8 H8A 108.3 . . ? O7 C8 H8B 108.3 . . ? C9 C8 H8B 108.3 . . ? H8A C8 H8B 107.4 . . ? O10 C9 C8 111.8(3) . . ? O10 C9 H9A 109.2 . . ? C8 C9 H9A 109.2 . . ? O10 C9 H9B 109.2 . . ? C8 C9 H9B 109.2 . . ? H9A C9 H9B 107.9 . . ? C9 O10 C11 111.0(3) . . ? O10 C11 C12 107.4(3) . . ? O10 C11 H11A 110.2 . . ? C12 C11 H11A 110.2 . . ? O10 C11 H11B 110.2 . . ? C12 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? O13 C12 C11 112.6(4) . . ? O13 C12 H12A 109.1 . . ? C11 C12 H12A 109.1 . . ? O13 C12 H12B 109.1 . . ? C11 C12 H12B 109.1 . . ? H12A C12 H12B 107.8 . . ? C14 O13 C12 116.0(3) . . ? O13 C14 C15 106.6(3) . . ? O13 C14 H14A 110.4 . . ? C15 C14 H14A 110.4 . . ? O13 C14 H14B 110.4 . . ? C15 C14 H14B 110.4 . . ? H14A C14 H14B 108.6 . . ? N1 C15 C14 116.7(2) . . ? N1 C15 H15A 108.1 . . ? C14 C15 H15A 108.1 . . ? N1 C15 H15B 108.1 . . ? C14 C15 H15B 108.1 . . ? H15A C15 H15B 107.3 . . ? C67 O21 Pb1 134.56(17) . . ? C22 N21 C61 108.0(3) . . ? C22 N21 C35 110.6(3) . . ? C61 N21 C35 111.6(3) . . ? C22 N21 Pb1 106.80(18) . . ? C61 N21 Pb1 101.56(17) . . ? C35 N21 Pb1 117.6(2) . . ? N21 C22 C23 113.4(3) . . ? N21 C22 H22A 108.9 . . ? C23 C22 H22A 108.9 . . ? N21 C22 H22B 108.9 . . ? C23 C22 H22B 108.9 . . ? H22A C22 H22B 107.7 . . ? O24 C23 C22 108.9(3) . . ? O24 C23 H23A 109.9 . . ? C22 C23 H23A 109.9 . . ? O24 C23 H23B 109.9 . . ? C22 C23 H23B 109.9 . . ? H23A C23 H23B 108.3 . . ? C23 O24 C25 113.5(3) . . ? O24 C25 C26 109.5(3) . . ? O24 C25 H25A 109.8 . . ? C26 C25 H25A 109.8 . . ? O24 C25 H25B 109.8 . . ? C26 C25 H25B 109.8 . . ? H25A C25 H25B 108.2 . . ? O27 C26 C25 113.9(3) . . ? O27 C26 H26A 108.8 . . ? C25 C26 H26A 108.8 . . ? O27 C26 H26B 108.8 . . ? C25 C26 H26B 108.8 . . ? H26A C26 H26B 107.7 . . ? C26 O27 C28 118.9(3) . . ? O27 C28 C29 112.5(4) . . ? O27 C28 H28A 109.1 . . ? C29 C28 H28A 109.1 . . ? O27 C28 H28B 109.1 . . ? C29 C28 H28B 109.1 . . ? H28A C28 H28B 107.8 . . ? O30 C29 C28 109.2(3) . . ? O30 C29 H29A 109.8 . . ? C28 C29 H29A 109.8 . . ? O30 C29 H29B 109.8 . . ? C28 C29 H29B 109.8 . . ? H29A C29 H29B 108.3 . . ? C29 O30 C31 113.4(4) . . ? O30 C31 C32 108.9(4) . . ? O30 C31 H31A 109.9 . . ? C32 C31 H31A 109.9 . . ? O30 C31 H31B 109.9 . . ? C32 C31 H31B 109.9 . . ? H31A C31 H31B 108.3 . . ? O33 C32 C31 108.6(4) . . ? O33 C32 H32A 110 . . ? C31 C32 H32A 110 . . ? O33 C32 H32B 110 . . ? C31 C32 H32B 110 . . ? H32A C32 H32B 108.3 . . ? C34 O33 C32 112.5(4) . . ? O33 C34 C35 108.0(3) . . ? O33 C34 H34A 110.1 . . ? C35 C34 H34A 110.1 . . ? O33 C34 H34B 110.1 . . ? C35 C34 H34B 110.1 . . ? H34A C34 H34B 108.4 . . ? C34 C35 N21 113.8(3) . . ? C34 C35 H35A 108.8 . . ? N21 C35 H35A 108.8 . . ? C34 C35 H35B 108.8 . . ? N21 C35 H35B 108.8 . . ? H35A C35 H35B 107.7 . . ? N1 C41 C42 114.5(2) . . ? N1 C41 H41A 108.6 . . ? C42 C41 H41A 108.6 . . ? N1 C41 H41B 108.6 . . ? C42 C41 H41B 108.6 . . ? H41A C41 H41B 107.6 . . ? C47 C42 C43 120.5(2) . . ? C47 C42 C41 118.6(2) . . ? C43 C42 C41 120.7(2) . . ? O1 C43 C42 121.0(2) . . ? O1 C43 C44 121.2(2) . . ? C42 C43 C44 117.7(2) . . ? C45 C44 C43 118.8(2) . . ? C45 C44 C48 120.4(2) . . ? C43 C44 C48 120.8(2) . . ? C46 C45 C44 124.5(2) . . ? C46 C45 H45 117.8 . . ? C44 C45 H45 117.8 . . ? C45 C46 C47 115.9(2) . . ? C45 C46 C52 123.4(2) . . ? C47 C46 C52 120.7(2) . . ? C42 C47 C46 122.6(2) . . ? C42 C47 H47 118.7 . . ? C46 C47 H47 118.7 . . ? C44 C48 C49 109.9(2) . . ? C44 C48 C51 112.8(2) . . ? C49 C48 C51 106.9(3) . . ? C44 C48 C50 109.4(2) . . ? C49 C48 C50 111.2(3) . . ? C51 C48 C50 106.7(3) . . ? C48 C49 H49A 109.5 . . ? C48 C49 H49B 109.5 . . ? H49A C49 H49B 109.5 . . ? C48 C49 H49C 109.5 . . ? H49A C49 H49C 109.5 . . ? H49B C49 H49C 109.5 . . ? C48 C50 H50A 109.5 . . ? C48 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C48 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C48 C51 H51A 109.5 . . ? C48 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C48 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C54 C52 C55 107.9(2) . . ? C54 C52 C46 110.3(2) . . ? C55 C52 C46 112.0(2) . . ? C54 C52 C53 109.4(2) . . ? C55 C52 C53 108.2(2) . . ? C46 C52 C53 108.9(2) . . ? C52 C53 H53A 109.5 . . ? C52 C53 H53B 109.5 . . ? H53A C53 H53B 109.5 . . ? C52 C53 H53C 109.5 . . ? H53A C53 H53C 109.5 . . ? H53B C53 H53C 109.5 . . ? C52 C54 H54A 109.5 . . ? C52 C54 H54B 109.5 . . ? H54A C54 H54B 109.5 . . ? C52 C54 H54C 109.5 . . ? H54A C54 H54C 109.5 . . ? H54B C54 H54C 109.5 . . ? C52 C55 H55A 109.5 . . ? C52 C55 H55B 109.5 . . ? H55A C55 H55B 109.5 . . ? C52 C55 H55C 109.5 . . ? H55A C55 H55C 109.5 . . ? H55B C55 H55C 109.5 . . ? N21 C61 C62 115.1(3) . . ? N21 C61 H61A 108.5 . . ? C62 C61 H61A 108.5 . . ? N21 C61 H61B 108.5 . . ? C62 C61 H61B 108.5 . . ? H61A C61 H61B 107.5 . . ? C63 C62 C67 120.7(3) . . ? C63 C62 C61 119.2(2) . . ? C67 C62 C61 120.1(2) . . ? C64 C63 C62 122.9(3) . . ? C64 C63 H63 118.5 . . ? C62 C63 H63 118.5 . . ? C63 C64 C65 115.9(3) . . ? C63 C64 C68 122.7(3) . . ? C65 C64 C68 121.4(3) . . ? C66 C65 C64 124.6(3) . . ? C66 C65 H65 117.7 . . ? C64 C65 H65 117.7 . . ? C65 C66 C67 118.4(2) . . ? C65 C66 C72 120.7(2) . . ? C67 C66 C72 120.8(2) . . ? O21 C67 C62 120.8(2) . . ? O21 C67 C66 121.6(2) . . ? C62 C67 C66 117.5(2) . . ? C70 C68 C71 108.7(3) . . ? C70 C68 C69 109.1(4) . . ? C71 C68 C69 108.0(3) . . ? C70 C68 C64 110.7(3) . . ? C71 C68 C64 111.9(3) . . ? C69 C68 C64 108.4(3) . . ? C68 C69 H69A 109.5 . . ? C68 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C68 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C68 C70 H70A 109.5 . . ? C68 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C68 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C68 C71 H71A 109.5 . . ? C68 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C68 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C75 C72 C74 106.9(2) . . ? C75 C72 C66 112.5(2) . . ? C74 C72 C66 110.4(2) . . ? C75 C72 C73 107.4(3) . . ? C74 C72 C73 110.2(2) . . ? C66 C72 C73 109.3(2) . . ? C72 C73 H73A 109.5 . . ? C72 C73 H73B 109.5 . . ? H73A C73 H73B 109.5 . . ? C72 C73 H73C 109.5 . . ? H73A C73 H73C 109.5 . . ? H73B C73 H73C 109.5 . . ? C72 C74 H74A 109.5 . . ? C72 C74 H74B 109.5 . . ? H74A C74 H74B 109.5 . . ? C72 C74 H74C 109.5 . . ? H74A C74 H74C 109.5 . . ? H74B C74 H74C 109.5 . . ? C72 C75 H75A 109.5 . . ? C72 C75 H75B 109.5 . . ? H75A C75 H75B 109.5 . . ? C72 C75 H75C 109.5 . . ? H75A C75 H75C 109.5 . . ? H75B C75 H75C 109.5 . . ? C86 C81 C82 118.5(5) . . ? C86 C81 H81 120.7 . . ? C82 C81 H81 120.7 . . ? C83 C82 C81 117.8(5) . . ? C83 C82 H82 121.1 . . ? C81 C82 H82 121.1 . . ? C84 C83 C82 121.1(4) . . ? C84 C83 H83 119.5 . . ? C82 C83 H83 119.5 . . ? C83 C84 C85 119.9(5) . . ? C83 C84 H84 120 . . ? C85 C84 H84 120 . . ? C84 C85 C86 121.2(5) . . ? C84 C85 H85 119.4 . . ? C86 C85 H85 119.4 . . ? C85 C86 C81 121.5(4) . . ? C85 C86 H86 119.3 . . ? C81 C86 H86 119.3 . . ? 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 O21 Pb1 O1 C43 101.2(2) . . . . ? N21 Pb1 O1 C43 178.8(2) . . . . ? N1 Pb1 O1 C43 18.5(2) . . . . ? O1 Pb1 N1 C15 -87.78(16) . . . . ? O21 Pb1 N1 C15 -179.18(17) . . . . ? N21 Pb1 N1 C15 -136.48(18) . . . . ? O1 Pb1 N1 C2 145.10(17) . . . . ? O21 Pb1 N1 C2 53.71(16) . . . . ? N21 Pb1 N1 C2 96.4(2) . . . . ? O1 Pb1 N1 C41 32.63(14) . . . . ? O21 Pb1 N1 C41 -58.77(14) . . . . ? N21 Pb1 N1 C41 -16.1(2) . . . . ? C15 N1 C2 C3 -58.0(3) . . . . ? C41 N1 C2 C3 175.7(2) . . . . ? Pb1 N1 C2 C3 68.7(2) . . . . ? N1 C2 C3 O4 80.5(3) . . . . ? C2 C3 O4 C5 -178.0(2) . . . . ? C3 O4 C5 C6 172.8(3) . . . . ? O4 C5 C6 O7 69.9(3) . . . . ? C5 C6 O7 C8 -174.1(3) . . . . ? C6 O7 C8 C9 51.1(4) . . . . ? O7 C8 C9 O10 52.4(5) . . . . ? C8 C9 O10 C11 -174.6(3) . . . . ? C9 O10 C11 C12 166.5(3) . . . . ? O10 C11 C12 O13 -72.2(4) . . . . ? C11 C12 O13 C14 106.1(4) . . . . ? C12 O13 C14 C15 -178.8(3) . . . . ? C2 N1 C15 C14 -60.1(3) . . . . ? C41 N1 C15 C14 63.9(3) . . . . ? Pb1 N1 C15 C14 177.20(18) . . . . ? O13 C14 C15 N1 -168.5(3) . . . . ? O1 Pb1 O21 C67 94.4(2) . . . . ? N21 Pb1 O21 C67 11.9(2) . . . . ? N1 Pb1 O21 C67 174.0(2) . . . . ? O1 Pb1 N21 C22 59.0(2) . . . . ? O21 Pb1 N21 C22 150.7(2) . . . . ? N1 Pb1 N21 C22 107.2(2) . . . . ? O1 Pb1 N21 C61 -53.96(16) . . . . ? O21 Pb1 N21 C61 37.71(16) . . . . ? N1 Pb1 N21 C61 -5.8(3) . . . . ? O1 Pb1 N21 C35 -176.0(2) . . . . ? O21 Pb1 N21 C35 -84.3(2) . . . . ? N1 Pb1 N21 C35 -127.9(2) . . . . ? C61 N21 C22 C23 168.2(3) . . . . ? C35 N21 C22 C23 -69.4(4) . . . . ? Pb1 N21 C22 C23 59.7(3) . . . . ? N21 C22 C23 O24 -67.3(4) . . . . ? C22 C23 O24 C25 176.0(3) . . . . ? C23 O24 C25 C26 163.3(3) . . . . ? O24 C25 C26 O27 64.7(5) . . . . ? C25 C26 O27 C28 99.9(5) . . . . ? C26 O27 C28 C29 -72.9(5) . . . . ? O27 C28 C29 O30 -55.6(5) . . . . ? C28 C29 O30 C31 169.1(4) . . . . ? C29 O30 C31 C32 -169.8(4) . . . . ? O30 C31 C32 O33 69.6(6) . . . . ? C31 C32 O33 C34 174.3(4) . . . . ? C32 O33 C34 C35 -178.6(3) . . . . ? O33 C34 C35 N21 -62.9(4) . . . . ? C22 N21 C35 C34 134.0(3) . . . . ? C61 N21 C35 C34 -105.8(4) . . . . ? Pb1 N21 C35 C34 10.9(4) . . . . ? C15 N1 C41 C42 45.6(3) . . . . ? C2 N1 C41 C42 173.1(2) . . . . ? Pb1 N1 C41 C42 -75.9(2) . . . . ? N1 C41 C42 C47 -112.6(3) . . . . ? N1 C41 C42 C43 71.1(3) . . . . ? Pb1 O1 C43 C42 -38.4(4) . . . . ? Pb1 O1 C43 C44 145.0(2) . . . . ? C47 C42 C43 O1 -178.2(2) . . . . ? C41 C42 C43 O1 -1.9(4) . . . . ? C47 C42 C43 C44 -1.4(4) . . . . ? C41 C42 C43 C44 174.8(2) . . . . ? O1 C43 C44 C45 178.6(2) . . . . ? C42 C43 C44 C45 1.8(4) . . . . ? O1 C43 C44 C48 0.3(4) . . . . ? C42 C43 C44 C48 -176.5(2) . . . . ? C43 C44 C45 C46 -0.6(4) . . . . ? C48 C44 C45 C46 177.7(3) . . . . ? C44 C45 C46 C47 -1.1(4) . . . . ? C44 C45 C46 C52 179.9(3) . . . . ? C43 C42 C47 C46 -0.3(4) . . . . ? C41 C42 C47 C46 -176.6(2) . . . . ? C45 C46 C47 C42 1.5(4) . . . . ? C52 C46 C47 C42 -179.4(2) . . . . ? C45 C44 C48 C49 120.6(3) . . . . ? C43 C44 C48 C49 -61.1(3) . . . . ? C45 C44 C48 C51 1.5(4) . . . . ? C43 C44 C48 C51 179.7(3) . . . . ? C45 C44 C48 C50 -117.1(3) . . . . ? C43 C44 C48 C50 61.2(3) . . . . ? C45 C46 C52 C54 116.1(3) . . . . ? C47 C46 C52 C54 -62.9(3) . . . . ? C45 C46 C52 C55 -4.1(4) . . . . ? C47 C46 C52 C55 176.9(3) . . . . ? C45 C46 C52 C53 -123.8(3) . . . . ? C47 C46 C52 C53 57.2(3) . . . . ? C22 N21 C61 C62 168.2(2) . . . . ? C35 N21 C61 C62 46.5(3) . . . . ? Pb1 N21 C61 C62 -79.7(2) . . . . ? N21 C61 C62 C63 -112.1(3) . . . . ? N21 C61 C62 C67 66.4(4) . . . . ? C67 C62 C63 C64 0.6(5) . . . . ? C61 C62 C63 C64 179.1(3) . . . . ? C62 C63 C64 C65 -1.3(5) . . . . ? C62 C63 C64 C68 -177.8(3) . . . . ? C63 C64 C65 C66 1.0(5) . . . . ? C68 C64 C65 C66 177.7(3) . . . . ? C64 C65 C66 C67 -0.1(4) . . . . ? C64 C65 C66 C72 179.4(3) . . . . ? Pb1 O21 C67 C62 -35.2(4) . . . . ? Pb1 O21 C67 C66 145.2(2) . . . . ? C63 C62 C67 O21 -179.3(3) . . . . ? C61 C62 C67 O21 2.2(4) . . . . ? C63 C62 C67 C66 0.3(4) . . . . ? C61 C62 C67 C66 -178.2(3) . . . . ? C65 C66 C67 O21 179.1(3) . . . . ? C72 C66 C67 O21 -0.5(4) . . . . ? C65 C66 C67 C62 -0.5(4) . . . . ? C72 C66 C67 C62 179.9(3) . . . . ? C63 C64 C68 C70 -133.8(4) . . . . ? C65 C64 C68 C70 49.8(5) . . . . ? C63 C64 C68 C71 -12.4(5) . . . . ? C65 C64 C68 C71 171.2(3) . . . . ? C63 C64 C68 C69 106.7(4) . . . . ? C65 C64 C68 C69 -69.7(4) . . . . ? C65 C66 C72 C75 3.3(4) . . . . ? C67 C66 C72 C75 -177.1(3) . . . . ? C65 C66 C72 C74 122.7(3) . . . . ? C67 C66 C72 C74 -57.8(3) . . . . ? C65 C66 C72 C73 -116.0(3) . . . . ? C67 C66 C72 C73 63.6(3) . . . . ? C86 C81 C82 C83 -0.7(6) . . . . ? C81 C82 C83 C84 1.4(7) . . . . ? C82 C83 C84 C85 -0.6(7) . . . . ? C83 C84 C85 C86 -1.0(7) . . . . ? C84 C85 C86 C81 1.8(7) . . . . ? C82 C81 C86 C85 -0.9(7) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 942091' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_WLF025 _audit_creation_date 2013-05-27T10:00:57-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C25 H42 Cl Ge N O5' _chemical_formula_sum 'C25 H42 Cl Ge N O5' _chemical_formula_weight 544.64 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 14.4685(7) _cell_length_b 10.9550(5) _cell_length_c 18.4462(10) _cell_angle_alpha 90 _cell_angle_beta 112.213(2) _cell_angle_gamma 90 _cell_volume 2706.8(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 4733 _cell_measurement_theta_min 2.39 _cell_measurement_theta_max 27.33 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description stick _exptl_crystal_colour colourless _exptl_crystal_size_max 0.6 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.04 _exptl_crystal_density_diffrn 1.336 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1152 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.264 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.783 _exptl_absorpt_correction_T_max 0.951 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0538 _diffrn_reflns_av_unetI/netI 0.0595 _diffrn_reflns_number 23337 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -23 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 2.93 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.999 _diffrn_measured_fraction_theta_max 0.999 _reflns_number_total 6197 _reflns_number_gt 4638 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 2012), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0579P)^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_number_reflns 6197 _refine_ls_number_parameters 308 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.065 _refine_ls_R_factor_gt 0.0412 _refine_ls_wR_factor_ref 0.1164 _refine_ls_wR_factor_gt 0.1005 _refine_ls_goodness_of_fit_ref 1.081 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0 _refine_diff_density_max 1.087 _refine_diff_density_min -0.862 _refine_diff_density_rms 0.173 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 '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' 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 Ge1 Ge 0.42365(2) 0.45014(2) 0.878043(16) 0.02012(10) Uani 1 1 d . . . Cl1 Cl 0.44527(5) 0.65494(6) 0.86113(4) 0.02724(17) Uani 1 1 d . . . C1 C 0.26575(19) 0.5217(2) 0.71181(14) 0.0181(5) Uani 1 1 d . . . H1A H 0.3206 0.5663 0.7037 0.022 Uiso 1 1 calc R . . H1B H 0.2373 0.5769 0.7405 0.022 Uiso 1 1 calc R . . C2 C 0.1856(2) 0.4954(2) 0.63246(15) 0.0225(6) Uani 1 1 d . . . H2A H 0.2151 0.4586 0.5971 0.027 Uiso 1 1 calc R . . H2B H 0.1353 0.4384 0.6375 0.027 Uiso 1 1 calc R . . O3 O 0.14133(14) 0.61042(17) 0.60300(10) 0.0278(4) Uani 1 1 d . . . C4 C 0.1006(2) 0.6218(3) 0.51965(15) 0.0285(6) Uani 1 1 d . . . H4A H 0.0401 0.6735 0.5037 0.034 Uiso 1 1 calc R . . H4B H 0.0805 0.5401 0.496 0.034 Uiso 1 1 calc R . . C5 C 0.1732(2) 0.6765(3) 0.48885(17) 0.0345(7) Uani 1 1 d . A . H5A H 0.1378 0.7023 0.4338 0.041 Uiso 1 1 calc R . . H5B H 0.2049 0.7494 0.5201 0.041 Uiso 1 1 calc R . . O6 O 0.24773(16) 0.5881(2) 0.49336(13) 0.0404(5) Uani 1 1 d . . . C7A C 0.3270(3) 0.6378(4) 0.4760(2) 0.0584(11) Uani 0.822(5) 1 d P A 1 H7A1 H 0.3009 0.7044 0.4373 0.07 Uiso 0.822(5) 1 calc PR A 1 H7A2 H 0.3543 0.5738 0.4517 0.07 Uiso 0.822(5) 1 calc PR A 1 C8A C 0.4057(3) 0.6846(4) 0.5437(2) 0.0411(11) Uani 0.822(5) 1 d P A 1 H8A1 H 0.3786 0.7407 0.5728 0.049 Uiso 0.822(5) 1 calc PR A 1 H8A2 H 0.4546 0.7298 0.5282 0.049 Uiso 0.822(5) 1 calc PR A 1 O9A O 0.45399(18) 0.5784(2) 0.59286(14) 0.0577(7) Uani 0.822(5) 1 d P A 1 C7B C 0.3270(3) 0.6378(4) 0.4760(2) 0.0584(11) Uani 0.178(5) 1 d P A 2 H7B1 H 0.3323 0.7245 0.492 0.07 Uiso 0.178(5) 1 calc PR A 2 H7B2 H 0.3046 0.6375 0.4182 0.07 Uiso 0.178(5) 1 calc PR A 2 C8B C 0.4267(13) 0.5907(18) 0.5053(11) 0.0411(11) Uani 0.178(5) 1 d P A 2 H8B1 H 0.4727 0.6476 0.494 0.049 Uiso 0.178(5) 1 calc PR A 2 H8B2 H 0.4294 0.5105 0.4815 0.049 Uiso 0.178(5) 1 calc PR A 2 O9B O 0.45399(18) 0.5784(2) 0.59286(14) 0.0577(7) Uani 0.178(5) 1 d P A 2 C10 C 0.5208(2) 0.6145(3) 0.6655(2) 0.0460(9) Uani 1 1 d . . . H10A H 0.4866 0.6687 0.6905 0.055 Uiso 1 1 calc R A 1 H10B H 0.5759 0.6612 0.6593 0.055 Uiso 1 1 calc R A 1 C11 C 0.5620(2) 0.5068(3) 0.71628(18) 0.0342(7) Uani 1 1 d . A . H11A H 0.5846 0.4467 0.6864 0.041 Uiso 1 1 calc R . . H11B H 0.6214 0.533 0.7617 0.041 Uiso 1 1 calc R . . O12 O 0.49500(14) 0.44772(17) 0.74452(11) 0.0294(5) Uani 1 1 d . . . C13 C 0.42033(19) 0.3768(3) 0.68732(15) 0.0254(6) Uani 1 1 d . A . H13A H 0.4519 0.3112 0.6677 0.03 Uiso 1 1 calc R . . H13B H 0.3807 0.429 0.6425 0.03 Uiso 1 1 calc R . . C14 C 0.35345(19) 0.3220(2) 0.72464(15) 0.0206(6) Uani 1 1 d . . . H14A H 0.2987 0.2772 0.6841 0.025 Uiso 1 1 calc R A . H14B H 0.3925 0.2621 0.7647 0.025 Uiso 1 1 calc R . . N15 N 0.30910(15) 0.41343(18) 0.76226(12) 0.0169(4) Uani 1 1 d . A . C16 C 0.23197(18) 0.3470(2) 0.78377(15) 0.0193(5) Uani 1 1 d . . . H16A H 0.184 0.3068 0.7364 0.023 Uiso 1 1 calc R A . H16B H 0.2654 0.2825 0.8224 0.023 Uiso 1 1 calc R . . C17 C 0.17591(19) 0.4291(2) 0.81747(14) 0.0186(5) Uani 1 1 d . A . C18 C 0.0738(2) 0.4447(2) 0.77997(15) 0.0218(6) Uani 1 1 d . . . H18 H 0.0398 0.4052 0.7313 0.026 Uiso 1 1 calc R A . C19 C 0.01994(19) 0.5172(2) 0.81217(15) 0.0221(6) Uani 1 1 d . A . C20 C 0.0730(2) 0.5701(2) 0.88467(15) 0.0225(6) Uani 1 1 d . . . H20 H 0.0368 0.6168 0.9084 0.027 Uiso 1 1 calc R A . C21 C 0.1767(2) 0.5588(2) 0.92501(15) 0.0206(6) Uani 1 1 d . A . C22 C 0.22822(18) 0.4885(2) 0.88866(14) 0.0189(5) Uani 1 1 d . . . C23 C -0.0922(2) 0.5387(3) 0.76658(17) 0.0273(6) Uani 1 1 d . . . C24 C -0.1474(2) 0.4152(3) 0.75147(19) 0.0382(8) Uani 1 1 d . A . H24A H -0.1374 0.3758 0.8016 0.057 Uiso 1 1 calc R . . H24B H -0.121 0.3624 0.7209 0.057 Uiso 1 1 calc R . . H24C H -0.2189 0.4287 0.7223 0.057 Uiso 1 1 calc R . . C25 C -0.1387(2) 0.6212(3) 0.81076(18) 0.0371(8) Uani 1 1 d . A . H25A H -0.1288 0.5846 0.8616 0.056 Uiso 1 1 calc R . . H25B H -0.2103 0.6301 0.7801 0.056 Uiso 1 1 calc R . . H25C H -0.1067 0.7016 0.8188 0.056 Uiso 1 1 calc R . . C26 C -0.1080(2) 0.5984(3) 0.68759(17) 0.0421(8) Uani 1 1 d . A . H26A H -0.1796 0.6099 0.6578 0.063 Uiso 1 1 calc R . . H26B H -0.0801 0.5457 0.658 0.063 Uiso 1 1 calc R . . H26C H -0.0743 0.6778 0.6965 0.063 Uiso 1 1 calc R . . C27 C 0.23074(19) 0.6205(3) 1.00449(14) 0.0235(6) Uani 1 1 d . . . C28 C 0.3055(2) 0.7159(3) 0.99763(16) 0.0298(7) Uani 1 1 d . A . H28A H 0.3509 0.6768 0.9765 0.045 Uiso 1 1 calc R . . H28B H 0.3441 0.7496 1.0495 0.045 Uiso 1 1 calc R . . H28C H 0.269 0.7818 0.9625 0.045 Uiso 1 1 calc R . . C29 C 0.2870(2) 0.5242(3) 1.06628(16) 0.0316(7) Uani 1 1 d . A . H29A H 0.2394 0.4643 1.0712 0.047 Uiso 1 1 calc R . . H29B H 0.3213 0.5644 1.1169 0.047 Uiso 1 1 calc R . . H29C H 0.3361 0.4828 1.0501 0.047 Uiso 1 1 calc R . . C30 C 0.1586(2) 0.6867(3) 1.03413(16) 0.0347(7) Uani 1 1 d . A . H30A H 0.1223 0.7497 0.9963 0.052 Uiso 1 1 calc R . . H30B H 0.1963 0.7249 1.0848 0.052 Uiso 1 1 calc R . . H30C H 0.1109 0.628 1.0402 0.052 Uiso 1 1 calc R . . O31 O 0.32901(13) 0.47118(16) 0.92270(10) 0.0215(4) Uani 1 1 d . A . 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 Ge1 0.01611(16) 0.01894(17) 0.02286(16) 0.00229(11) 0.00461(12) 0.00223(12) Cl1 0.0269(4) 0.0210(4) 0.0289(3) -0.0009(3) 0.0050(3) -0.0039(3) C1 0.0193(13) 0.0146(13) 0.0196(12) 0.0022(10) 0.0065(11) 0.0017(11) C2 0.0257(15) 0.0155(13) 0.0244(13) -0.0003(11) 0.0074(12) 0.0012(12) O3 0.0349(11) 0.0224(10) 0.0221(9) 0.0033(8) 0.0062(9) 0.0095(9) C4 0.0254(15) 0.0313(17) 0.0228(14) 0.0057(12) 0.0022(12) 0.0025(14) C5 0.0341(17) 0.0346(18) 0.0343(16) 0.0082(14) 0.0124(14) 0.0033(15) O6 0.0361(12) 0.0413(13) 0.0506(13) 0.0146(11) 0.0243(11) 0.0085(11) C7A 0.042(2) 0.084(3) 0.058(2) 0.037(2) 0.0291(19) 0.015(2) C8A 0.038(2) 0.042(2) 0.042(2) 0.0198(18) 0.0139(18) -0.008(2) O9A 0.0418(14) 0.0761(18) 0.0444(14) 0.0232(13) 0.0041(12) -0.0191(13) C7B 0.042(2) 0.084(3) 0.058(2) 0.037(2) 0.0291(19) 0.015(2) C8B 0.038(2) 0.042(2) 0.042(2) 0.0198(18) 0.0139(18) -0.008(2) O9B 0.0418(14) 0.0761(18) 0.0444(14) 0.0232(13) 0.0041(12) -0.0191(13) C10 0.0343(18) 0.051(2) 0.052(2) 0.0119(18) 0.0158(16) -0.0086(18) C11 0.0199(15) 0.0455(19) 0.0348(16) 0.0047(15) 0.0077(13) -0.0080(15) O12 0.0235(10) 0.0376(12) 0.0263(10) -0.0010(9) 0.0085(9) -0.0087(9) C13 0.0244(14) 0.0256(15) 0.0297(14) -0.0041(12) 0.0142(12) -0.0007(13) C14 0.0211(13) 0.0146(13) 0.0266(13) -0.0026(11) 0.0096(11) 0.0023(11) N15 0.0184(11) 0.0133(10) 0.0205(10) 0.0004(9) 0.0090(9) 0.0000(9) C16 0.0200(13) 0.0160(13) 0.0235(13) 0.0004(11) 0.0101(11) -0.0033(11) C17 0.0181(13) 0.0168(13) 0.0215(13) 0.0013(10) 0.0082(11) -0.0019(11) C18 0.0230(14) 0.0239(14) 0.0177(12) 0.0003(11) 0.0067(11) -0.0043(12) C19 0.0193(13) 0.0239(14) 0.0236(13) 0.0061(11) 0.0089(11) -0.0016(12) C20 0.0229(14) 0.0248(15) 0.0230(13) 0.0045(11) 0.0124(11) 0.0039(12) C21 0.0231(14) 0.0205(14) 0.0191(12) 0.0037(10) 0.0091(11) -0.0002(12) C22 0.0177(13) 0.0185(13) 0.0201(13) 0.0051(10) 0.0065(11) -0.0001(11) C23 0.0166(14) 0.0340(17) 0.0304(15) 0.0080(12) 0.0078(12) 0.0005(13) C24 0.0211(15) 0.0416(19) 0.0478(19) 0.0062(16) 0.0084(14) -0.0016(15) C25 0.0157(14) 0.042(2) 0.053(2) 0.0029(16) 0.0130(14) 0.0047(14) C26 0.0242(16) 0.061(2) 0.0344(17) 0.0206(16) 0.0038(14) 0.0050(16) C27 0.0244(14) 0.0277(15) 0.0162(12) -0.0002(11) 0.0053(11) 0.0021(13) C28 0.0388(17) 0.0260(16) 0.0233(14) -0.0059(12) 0.0104(13) -0.0061(14) C29 0.0318(17) 0.0420(18) 0.0204(14) 0.0042(13) 0.0091(13) 0.0022(15) C30 0.0367(17) 0.0422(19) 0.0262(15) -0.0064(14) 0.0131(13) 0.0060(15) O31 0.0166(9) 0.0259(10) 0.0193(9) 0.0013(7) 0.0035(8) 0.0025(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 O31 1.8599(17) . ? Ge1 N15 2.189(2) . ? Ge1 Cl1 2.3027(7) . ? C1 N15 1.492(3) . ? C1 C2 1.512(4) . ? C1 H1A 0.99 . ? C1 H1B 0.99 . ? C2 O3 1.425(3) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? O3 C4 1.429(3) . ? C4 C5 1.495(4) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 O6 1.429(3) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? O6 C7A 1.411(4) . ? C7A C8A 1.430(5) . ? C7A H7A1 0.99 . ? C7A H7A2 0.99 . ? C8A O9A 1.478(4) . ? C8A H8A1 0.99 . ? C8A H8A2 0.99 . ? O9A C10 1.381(4) . ? C8B H8B1 0.99 . ? C8B H8B2 0.99 . ? C10 C11 1.485(4) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C11 O12 1.418(3) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? O12 C13 1.422(3) . ? C13 C14 1.508(3) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 N15 1.495(3) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? N15 C16 1.506(3) . ? C16 C17 1.495(3) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C17 C18 1.384(4) . ? C17 C22 1.403(3) . ? C18 C19 1.394(4) . ? C18 H18 0.95 . ? C19 C20 1.392(4) . ? C19 C23 1.537(4) . ? C20 C21 1.405(4) . ? C20 H20 0.95 . ? C21 C22 1.406(3) . ? C21 C27 1.534(3) . ? C22 O31 1.365(3) . ? C23 C25 1.533(4) . ? C23 C26 1.534(4) . ? C23 C24 1.543(4) . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 C30 1.532(4) . ? C27 C29 1.540(4) . ? C27 C28 1.543(4) . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C30 H30A 0.98 . ? C30 H30B 0.98 . ? C30 H30C 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O31 Ge1 N15 92.42(7) . . ? O31 Ge1 Cl1 95.72(6) . . ? N15 Ge1 Cl1 97.95(6) . . ? N15 C1 C2 116.1(2) . . ? N15 C1 H1A 108.3 . . ? C2 C1 H1A 108.3 . . ? N15 C1 H1B 108.3 . . ? C2 C1 H1B 108.3 . . ? H1A C1 H1B 107.4 . . ? O3 C2 C1 105.7(2) . . ? O3 C2 H2A 110.6 . . ? C1 C2 H2A 110.6 . . ? O3 C2 H2B 110.6 . . ? C1 C2 H2B 110.6 . . ? H2A C2 H2B 108.7 . . ? C2 O3 C4 115.5(2) . . ? O3 C4 C5 112.4(2) . . ? O3 C4 H4A 109.1 . . ? C5 C4 H4A 109.1 . . ? O3 C4 H4B 109.1 . . ? C5 C4 H4B 109.1 . . ? H4A C4 H4B 107.9 . . ? O6 C5 C4 109.2(2) . . ? O6 C5 H5A 109.8 . . ? C4 C5 H5A 109.8 . . ? O6 C5 H5B 109.8 . . ? C4 C5 H5B 109.8 . . ? H5A C5 H5B 108.3 . . ? C7A O6 C5 112.7(3) . . ? O6 C7A C8A 112.8(3) . . ? O6 C7A H7A1 109 . . ? C8A C7A H7A1 109 . . ? O6 C7A H7A2 109 . . ? C8A C7A H7A2 109 . . ? H7A1 C7A H7A2 107.8 . . ? C7A C8A O9A 106.8(3) . . ? C7A C8A H8A1 110.4 . . ? O9A C8A H8A1 110.4 . . ? C7A C8A H8A2 110.4 . . ? O9A C8A H8A2 110.4 . . ? H8A1 C8A H8A2 108.6 . . ? C10 O9A C8A 111.4(3) . . ? H8B1 C8B H8B2 108.9 . . ? O9A C10 C11 110.5(3) . . ? O9A C10 H10A 109.5 . . ? C11 C10 H10A 109.5 . . ? O9A C10 H10B 109.5 . . ? C11 C10 H10B 109.5 . . ? H10A C10 H10B 108.1 . . ? O12 C11 C10 115.3(2) . . ? O12 C11 H11A 108.5 . . ? C10 C11 H11A 108.5 . . ? O12 C11 H11B 108.5 . . ? C10 C11 H11B 108.5 . . ? H11A C11 H11B 107.5 . . ? C11 O12 C13 114.2(2) . . ? O12 C13 C14 108.5(2) . . ? O12 C13 H13A 110 . . ? C14 C13 H13A 110 . . ? O12 C13 H13B 110 . . ? C14 C13 H13B 110 . . ? H13A C13 H13B 108.4 . . ? N15 C14 C13 114.0(2) . . ? N15 C14 H14A 108.7 . . ? C13 C14 H14A 108.7 . . ? N15 C14 H14B 108.7 . . ? C13 C14 H14B 108.7 . . ? H14A C14 H14B 107.6 . . ? C1 N15 C14 113.36(19) . . ? C1 N15 C16 111.71(19) . . ? C14 N15 C16 106.84(19) . . ? C1 N15 Ge1 116.56(15) . . ? C14 N15 Ge1 106.05(15) . . ? C16 N15 Ge1 101.24(14) . . ? C17 C16 N15 113.1(2) . . ? C17 C16 H16A 109 . . ? N15 C16 H16A 109 . . ? C17 C16 H16B 109 . . ? N15 C16 H16B 109 . . ? H16A C16 H16B 107.8 . . ? C18 C17 C22 120.5(2) . . ? C18 C17 C16 120.7(2) . . ? C22 C17 C16 118.8(2) . . ? C17 C18 C19 121.4(2) . . ? C17 C18 H18 119.3 . . ? C19 C18 H18 119.3 . . ? C20 C19 C18 116.9(2) . . ? C20 C19 C23 123.1(2) . . ? C18 C19 C23 119.9(2) . . ? C19 C20 C21 124.2(2) . . ? C19 C20 H20 117.9 . . ? C21 C20 H20 117.9 . . ? C20 C21 C22 116.6(2) . . ? C20 C21 C27 121.6(2) . . ? C22 C21 C27 121.8(2) . . ? O31 C22 C17 118.1(2) . . ? O31 C22 C21 121.6(2) . . ? C17 C22 C21 120.3(2) . . ? C25 C23 C26 108.4(3) . . ? C25 C23 C19 112.6(2) . . ? C26 C23 C19 109.4(2) . . ? C25 C23 C24 108.2(2) . . ? C26 C23 C24 108.8(3) . . ? C19 C23 C24 109.4(2) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C30 C27 C21 112.3(2) . . ? C30 C27 C29 107.5(2) . . ? C21 C27 C29 110.0(2) . . ? C30 C27 C28 107.6(2) . . ? C21 C27 C28 109.9(2) . . ? C29 C27 C28 109.5(2) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C22 O31 Ge1 130.59(15) . . ? 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 N15 C1 C2 O3 167.65(19) . . . . ? C1 C2 O3 C4 151.3(2) . . . . ? C2 O3 C4 C5 -93.8(3) . . . . ? O3 C4 C5 O6 73.9(3) . . . . ? C4 C5 O6 C7A -171.4(3) . . . . ? C5 O6 C7A C8A 89.5(4) . . . . ? O6 C7A C8A O9A 68.8(4) . . . . ? C7A C8A O9A C10 -170.4(3) . . . . ? C8A O9A C10 C11 175.2(3) . . . . ? O9A C10 C11 O12 -72.9(4) . . . . ? C10 C11 O12 C13 74.5(3) . . . . ? C11 O12 C13 C14 -178.7(2) . . . . ? O12 C13 C14 N15 54.7(3) . . . . ? C2 C1 N15 C14 57.3(3) . . . . ? C2 C1 N15 C16 -63.5(3) . . . . ? C2 C1 N15 Ge1 -179.14(16) . . . . ? C13 C14 N15 C1 47.0(3) . . . . ? C13 C14 N15 C16 170.5(2) . . . . ? C13 C14 N15 Ge1 -82.1(2) . . . . ? O31 Ge1 N15 C1 86.96(16) . . . . ? Cl1 Ge1 N15 C1 -9.17(16) . . . . ? O31 Ge1 N15 C14 -145.81(15) . . . . ? Cl1 Ge1 N15 C14 118.07(14) . . . . ? O31 Ge1 N15 C16 -34.43(14) . . . . ? Cl1 Ge1 N15 C16 -130.55(13) . . . . ? C1 N15 C16 C17 -51.7(3) . . . . ? C14 N15 C16 C17 -176.2(2) . . . . ? Ge1 N15 C16 C17 73.1(2) . . . . ? N15 C16 C17 C18 117.5(3) . . . . ? N15 C16 C17 C22 -63.7(3) . . . . ? C22 C17 C18 C19 -1.3(4) . . . . ? C16 C17 C18 C19 177.5(2) . . . . ? C17 C18 C19 C20 -1.8(4) . . . . ? C17 C18 C19 C23 176.3(2) . . . . ? C18 C19 C20 C21 2.7(4) . . . . ? C23 C19 C20 C21 -175.4(2) . . . . ? C19 C20 C21 C22 -0.4(4) . . . . ? C19 C20 C21 C27 179.4(2) . . . . ? C18 C17 C22 O31 -179.2(2) . . . . ? C16 C17 C22 O31 2.0(3) . . . . ? C18 C17 C22 C21 3.7(4) . . . . ? C16 C17 C22 C21 -175.1(2) . . . . ? C20 C21 C22 O31 -179.8(2) . . . . ? C27 C21 C22 O31 0.4(4) . . . . ? C20 C21 C22 C17 -2.8(4) . . . . ? C27 C21 C22 C17 177.4(2) . . . . ? C20 C19 C23 C25 -1.6(4) . . . . ? C18 C19 C23 C25 -179.6(2) . . . . ? C20 C19 C23 C26 119.1(3) . . . . ? C18 C19 C23 C26 -59.0(3) . . . . ? C20 C19 C23 C24 -121.9(3) . . . . ? C18 C19 C23 C24 60.1(3) . . . . ? C20 C21 C27 C30 3.1(3) . . . . ? C22 C21 C27 C30 -177.2(2) . . . . ? C20 C21 C27 C29 122.7(3) . . . . ? C22 C21 C27 C29 -57.5(3) . . . . ? C20 C21 C27 C28 -116.7(3) . . . . ? C22 C21 C27 C28 63.1(3) . . . . ? C17 C22 O31 Ge1 34.6(3) . . . . ? C21 C22 O31 Ge1 -148.29(19) . . . . ? N15 Ge1 O31 C22 -14.8(2) . . . . ? Cl1 Ge1 O31 C22 83.5(2) . . . . ? #----------------------------------------------------------------------------# # END OF CIF FILE FOR WLF025 # #----------------------------------------------------------------------------# _database_code_depnum_ccdc_archive 'CCDC 942092' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_SR15 _audit_creation_date 2012-02-02T09:35:15-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C31 H60 Ge N2 O5 Si2' _chemical_formula_sum 'C31 H60 Ge N2 O5 Si2' _chemical_formula_weight 669.58 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 13.0369(18) _cell_length_b 15.596(2) _cell_length_c 18.084(3) _cell_angle_alpha 90 _cell_angle_beta 98.921(6) _cell_angle_gamma 90 _cell_volume 3632.4(9) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9932 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 27.38 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.224 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.947 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.867 _exptl_absorpt_correction_T_max 0.936 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0355 _diffrn_reflns_av_unetI/netI 0.0361 _diffrn_reflns_number 29717 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 20 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 3.05 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.987 _diffrn_measured_fraction_theta_max 0.987 _reflns_number_total 8212 _reflns_number_gt 6879 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0323P)^2^+1.1022P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 8212 _refine_ls_number_parameters 382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0388 _refine_ls_R_factor_gt 0.0287 _refine_ls_wR_factor_ref 0.0719 _refine_ls_wR_factor_gt 0.0675 _refine_ls_goodness_of_fit_ref 1.021 _refine_ls_restrained_S_all 1.021 _refine_ls_shift/su_max 0.013 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.371 _refine_diff_density_min -0.212 _refine_diff_density_rms 0.052 _iucr_refine_instructions_details ; .res file for SHELXL : job.res ................................................................. TITL import in P 21/n CELL 0.71073 13.0369 15.5960 18.0840 90.000 98.921 90.000 ZERR 4.00 0.0018 0.0020 0.0030 0.000 0.006 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O SI GE UNIT 124 240 8 20 8 4 MERG 2 FMAP 2 PLAN 20 ACTA BOND $H CONF LIST 4 WPDB -2 L.S. 4 TEMP -123.00 WGHT 0.032300 1.102200 FVAR 0.42131 GE1 6 0.853384 0.085584 0.255482 11.00000 0.01690 0.01532 = 0.01541 -0.00116 0.00357 0.00013 SI1 5 0.824521 -0.059369 0.138717 11.00000 0.01876 0.02399 = 0.01836 -0.00677 0.00257 -0.00083 SI2 5 1.044568 -0.029824 0.216872 11.00000 0.01650 0.02110 = 0.02096 -0.00146 0.00376 0.00116 N1 3 0.808604 0.020787 0.361341 11.00000 0.01787 0.01322 = 0.01766 -0.00319 0.00469 -0.00254 C2 1 0.786761 -0.072690 0.349852 11.00000 0.02114 0.01428 = 0.02098 -0.00364 0.00566 -0.00416 AFIX 23 H2A 2 0.848331 -0.100281 0.334197 11.00000 -1.20000 H2B 2 0.728138 -0.079517 0.308381 11.00000 -1.20000 AFIX 0 C3 1 0.760272 -0.119860 0.418486 11.00000 0.03809 0.01728 = 0.02610 -0.00275 0.00965 -0.00990 AFIX 23 H3A 2 0.821416 -0.121742 0.458459 11.00000 -1.20000 H3B 2 0.702761 -0.090605 0.438187 11.00000 -1.20000 AFIX 0 O4 4 0.730256 -0.204185 0.394245 11.00000 0.03543 0.01555 = 0.03170 -0.00161 0.01091 -0.00779 C5 1 0.697541 -0.255306 0.451829 11.00000 0.04062 0.01963 = 0.03633 0.00745 0.00624 -0.00657 AFIX 23 H5A 2 0.726711 -0.231087 0.501232 11.00000 -1.20000 H5B 2 0.725176 -0.314150 0.449075 11.00000 -1.20000 AFIX 0 C6 1 0.580515 -0.259250 0.445186 11.00000 0.04211 0.02682 = 0.03146 0.00435 0.00781 -0.01503 AFIX 23 H6A 2 0.550611 -0.282876 0.395710 11.00000 -1.20000 H6B 2 0.560828 -0.297528 0.484344 11.00000 -1.20000 AFIX 0 O7 4 0.540513 -0.175515 0.453514 11.00000 0.02684 0.03238 = 0.03331 -0.00241 0.00807 -0.01017 C8 1 0.429558 -0.173399 0.441995 11.00000 0.02777 0.04645 = 0.03029 0.00349 0.00657 -0.01641 AFIX 23 H8A 2 0.403375 -0.206441 0.481931 11.00000 -1.20000 H8B 2 0.402159 -0.200141 0.393278 11.00000 -1.20000 AFIX 0 C9 1 0.392801 -0.082457 0.442956 11.00000 0.02376 0.05178 = 0.02332 -0.00114 0.00949 -0.01093 AFIX 23 H9A 2 0.316381 -0.081414 0.440250 11.00000 -1.20000 H9B 2 0.424060 -0.054584 0.490308 11.00000 -1.20000 AFIX 0 O10 4 0.421347 -0.036609 0.381076 11.00000 0.03201 0.03362 = 0.02783 -0.00229 0.01621 -0.00473 C11 1 0.386320 0.050228 0.378918 11.00000 0.01934 0.03928 = 0.03560 -0.01141 0.00947 -0.00339 AFIX 23 H11A 2 0.403075 0.076176 0.429307 11.00000 -1.20000 H11B 2 0.310067 0.052095 0.363670 11.00000 -1.20000 AFIX 0 C12 1 0.438565 0.100081 0.323976 11.00000 0.01842 0.03165 = 0.03722 -0.00008 0.00418 0.00346 AFIX 23 H12A 2 0.433265 0.067471 0.276567 11.00000 -1.20000 H12B 2 0.401963 0.155330 0.313018 11.00000 -1.20000 AFIX 0 O13 4 0.546120 0.116544 0.351816 11.00000 0.01725 0.02463 = 0.04445 -0.00980 0.01037 -0.00024 C14 1 0.615855 0.054361 0.329903 11.00000 0.01831 0.02447 = 0.02979 -0.00694 0.00920 -0.00023 AFIX 23 H14A 2 0.623596 0.061926 0.276695 11.00000 -1.20000 H14B 2 0.590550 -0.004462 0.337008 11.00000 -1.20000 AFIX 0 C15 1 0.718452 0.070480 0.380674 11.00000 0.02064 0.01819 = 0.02198 -0.00478 0.00911 -0.00227 AFIX 23 H15A 2 0.734874 0.132366 0.379096 11.00000 -1.20000 H15B 2 0.709759 0.056387 0.432720 11.00000 -1.20000 AFIX 0 N21 3 0.910922 -0.010455 0.210418 11.00000 0.01681 0.01892 = 0.01642 -0.00362 0.00277 0.00104 C22 1 0.690910 -0.011841 0.133036 11.00000 0.02061 0.03664 = 0.02936 -0.00988 -0.00230 0.00128 AFIX 137 H22A 2 0.665411 -0.020785 0.180657 11.00000 -1.50000 H22B 2 0.643837 -0.039729 0.092640 11.00000 -1.50000 H22C 2 0.693875 0.049753 0.122851 11.00000 -1.50000 AFIX 0 C23 1 0.807091 -0.177232 0.152418 11.00000 0.03154 0.02670 = 0.04223 -0.01074 0.00328 -0.00574 AFIX 137 H23A 2 0.870217 -0.207639 0.144381 11.00000 -1.50000 H23B 2 0.748141 -0.197861 0.116544 11.00000 -1.50000 H23C 2 0.793796 -0.187853 0.203498 11.00000 -1.50000 AFIX 0 C24 1 0.863488 -0.039206 0.044054 11.00000 0.03401 0.05308 = 0.02111 -0.00734 0.00419 -0.00211 AFIX 137 H24A 2 0.863110 0.022607 0.034272 11.00000 -1.50000 H24B 2 0.814231 -0.067733 0.005369 11.00000 -1.50000 H24C 2 0.933371 -0.062014 0.043335 11.00000 -1.50000 AFIX 0 C25 1 1.070913 -0.135789 0.173695 11.00000 0.02526 0.03384 = 0.04496 -0.01167 0.00492 0.00885 AFIX 137 H25A 2 1.045208 -0.182384 0.202234 11.00000 -1.50000 H25B 2 1.145824 -0.142541 0.174551 11.00000 -1.50000 H25C 2 1.035427 -0.137620 0.121816 11.00000 -1.50000 AFIX 0 C26 1 1.113831 -0.039004 0.315400 11.00000 0.02224 0.02718 = 0.02861 0.00081 -0.00124 0.00246 AFIX 137 H26A 2 1.116699 0.017425 0.339473 11.00000 -1.50000 H26B 2 1.184560 -0.060063 0.314972 11.00000 -1.50000 H26C 2 1.076454 -0.079176 0.343282 11.00000 -1.50000 AFIX 0 C27 1 1.108916 0.055133 0.166853 11.00000 0.02733 0.03958 = 0.03076 0.00299 0.01082 -0.00260 AFIX 137 H27A 2 1.081564 0.053129 0.113256 11.00000 -1.50000 H27B 2 1.184021 0.045107 0.174298 11.00000 -1.50000 H27C 2 1.094809 0.111584 0.186853 11.00000 -1.50000 AFIX 0 O28 4 0.980202 0.122595 0.311588 11.00000 0.01902 0.01778 = 0.01693 -0.00423 0.00552 -0.00340 C29 1 0.976161 0.166860 0.376512 11.00000 0.01434 0.01691 = 0.01720 -0.00301 0.00176 -0.00058 C30 1 1.015500 0.251229 0.388475 11.00000 0.01499 0.01617 = 0.02038 0.00070 0.00252 -0.00195 C31 1 1.002308 0.291431 0.456000 11.00000 0.01772 0.01422 = 0.02392 -0.00286 0.00156 -0.00251 AFIX 43 H31 2 1.028417 0.348010 0.464661 11.00000 -1.20000 AFIX 0 C32 1 0.952907 0.253176 0.511519 11.00000 0.01571 0.01729 = 0.01818 -0.00233 -0.00043 0.00040 C33 1 0.920627 0.168529 0.499017 11.00000 0.02009 0.01921 = 0.01672 0.00060 0.00333 -0.00270 AFIX 43 H33 2 0.889722 0.139445 0.536135 11.00000 -1.20000 AFIX 0 C34 1 0.932649 0.125393 0.433139 11.00000 0.01690 0.01571 = 0.01741 -0.00104 0.00064 -0.00116 C35 1 0.899689 0.032810 0.422275 11.00000 0.02100 0.01634 = 0.01702 -0.00011 0.00358 -0.00371 AFIX 23 H35A 2 0.958953 -0.001204 0.410057 11.00000 -1.20000 H35B 2 0.881530 0.010459 0.469825 11.00000 -1.20000 AFIX 0 C36 1 1.067886 0.297570 0.328791 11.00000 0.02333 0.01827 = 0.02476 -0.00130 0.00863 -0.00530 C37 1 1.109932 0.386402 0.355420 11.00000 0.04235 0.02055 = 0.04100 -0.00377 0.01929 -0.01205 AFIX 137 H37A 2 1.160521 0.380036 0.401182 11.00000 -1.50000 H37B 2 1.052411 0.422707 0.365669 11.00000 -1.50000 H37C 2 1.143631 0.413012 0.316361 11.00000 -1.50000 AFIX 0 C38 1 1.160159 0.244172 0.310263 11.00000 0.02514 0.02617 = 0.03721 -0.00377 0.01478 -0.00501 AFIX 137 H38A 2 1.187697 0.270586 0.268251 11.00000 -1.50000 H38B 2 1.136729 0.185764 0.296646 11.00000 -1.50000 H38C 2 1.214693 0.242230 0.354115 11.00000 -1.50000 AFIX 0 C39 1 0.986475 0.311558 0.258214 11.00000 0.03956 0.03019 = 0.02611 0.00783 0.00904 -0.00145 AFIX 137 H39A 2 0.927106 0.343169 0.271722 11.00000 -1.50000 H39B 2 0.962981 0.255876 0.236862 11.00000 -1.50000 H39C 2 1.017653 0.344512 0.221252 11.00000 -1.50000 AFIX 0 C40 1 0.938147 0.300149 0.584183 11.00000 0.02065 0.01865 = 0.01932 -0.00395 0.00257 0.00016 C41 1 0.832346 0.277508 0.607208 11.00000 0.02632 0.02765 = 0.03268 -0.00838 0.01057 -0.00046 AFIX 137 H41A 2 0.776606 0.291503 0.566118 11.00000 -1.50000 H41B 2 0.822896 0.310535 0.651760 11.00000 -1.50000 H41C 2 0.830310 0.216100 0.618377 11.00000 -1.50000 AFIX 0 C42 1 1.026252 0.273944 0.647388 11.00000 0.03037 0.03097 = 0.02016 -0.00533 -0.00014 0.00528 AFIX 137 H42A 2 1.022967 0.212050 0.656078 11.00000 -1.50000 H42B 2 1.018212 0.304727 0.693384 11.00000 -1.50000 H42C 2 1.093479 0.288426 0.632804 11.00000 -1.50000 AFIX 0 C43 1 0.940538 0.398037 0.575097 11.00000 0.03906 0.01973 = 0.02698 -0.00613 0.00561 -0.00083 AFIX 137 H43A 2 1.008859 0.415609 0.564308 11.00000 -1.50000 H43B 2 0.927377 0.425480 0.621466 11.00000 -1.50000 H43C 2 0.886903 0.415463 0.533720 11.00000 -1.50000 HKLF 4 REM import in P 21/n REM R1 = 0.0287 for 6879 Fo > 4sig(Fo) and 0.0388 for all 8212 data REM 382 parameters refined using 0 restraints END WGHT 0.0295 1.2091 REM Highest difference peak 0.37, deepest hole -0.21, 1-sigma level 0.05 Q1 1 0.9476 0.2786 0.4763 11.00000 0.05 0.37 Q2 1 0.8185 -0.1215 0.1491 11.00000 0.05 0.37 Q3 1 1.0449 0.2734 0.3565 11.00000 0.05 0.34 Q4 1 0.9511 0.2778 0.5498 11.00000 0.05 0.33 Q5 1 0.7568 -0.0273 0.1466 11.00000 0.05 0.31 Q6 1 0.9143 0.0837 0.4278 11.00000 0.05 0.31 Q7 1 0.8969 0.2833 0.6005 11.00000 0.05 0.31 Q8 1 0.7991 -0.0243 0.3581 11.00000 0.05 0.30 Q9 1 1.0170 0.2003 0.3890 11.00000 0.05 0.29 Q10 1 0.7873 -0.0952 0.3851 11.00000 0.05 0.29 Q11 1 0.8520 0.0312 0.3892 11.00000 0.05 0.29 Q12 1 0.8531 -0.0455 0.0893 11.00000 0.05 0.29 Q13 1 1.0700 0.0228 0.1860 11.00000 0.05 0.29 Q14 1 1.0576 -0.0827 0.1889 11.00000 0.05 0.28 Q15 1 1.0859 -0.0356 0.2680 11.00000 0.05 0.28 Q16 1 0.9803 0.2915 0.6113 11.00000 0.05 0.27 Q17 1 0.9018 0.1498 0.4500 11.00000 0.05 0.27 Q18 1 1.0352 0.3069 0.2946 11.00000 0.05 0.26 Q19 1 0.9276 0.1507 0.3994 11.00000 0.05 0.26 Q20 1 0.9947 0.2600 0.4926 11.00000 0.05 0.26 ; #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 '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' 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 Ge1 Ge 0.853384(12) 0.085584(10) 0.255482(8) 0.01576(5) Uani 1 1 d . . . Si1 Si 0.82452(3) -0.05937(3) 0.13872(2) 0.02040(10) Uani 1 1 d . . . Si2 Si 1.04457(3) -0.02982(3) 0.21687(2) 0.01943(10) Uani 1 1 d . . . N1 N 0.80860(10) 0.02079(8) 0.36134(7) 0.0160(3) Uani 1 1 d . . . C2 C 0.78676(13) -0.07269(9) 0.34985(9) 0.0185(3) Uani 1 1 d . . . H2A H 0.8483 -0.1003 0.3342 0.022 Uiso 1 1 calc R . . H2B H 0.7281 -0.0795 0.3084 0.022 Uiso 1 1 calc R . . C3 C 0.76027(15) -0.11986(10) 0.41849(9) 0.0267(4) Uani 1 1 d . . . H3A H 0.8214 -0.1217 0.4585 0.032 Uiso 1 1 calc R . . H3B H 0.7028 -0.0906 0.4382 0.032 Uiso 1 1 calc R . . O4 O 0.73026(9) -0.20419(7) 0.39425(7) 0.0270(3) Uani 1 1 d . . . C5 C 0.69754(15) -0.25531(11) 0.45183(10) 0.0322(4) Uani 1 1 d . . . H5A H 0.7267 -0.2311 0.5012 0.039 Uiso 1 1 calc R . . H5B H 0.7252 -0.3142 0.4491 0.039 Uiso 1 1 calc R . . C6 C 0.58052(15) -0.25925(11) 0.44519(10) 0.0332(4) Uani 1 1 d . . . H6A H 0.5506 -0.2829 0.3957 0.04 Uiso 1 1 calc R . . H6B H 0.5608 -0.2975 0.4843 0.04 Uiso 1 1 calc R . . O7 O 0.54051(9) -0.17552(8) 0.45351(7) 0.0305(3) Uani 1 1 d . . . C8 C 0.42956(14) -0.17340(13) 0.44199(10) 0.0346(4) Uani 1 1 d . . . H8A H 0.4034 -0.2064 0.4819 0.042 Uiso 1 1 calc R . . H8B H 0.4022 -0.2001 0.3933 0.042 Uiso 1 1 calc R . . C9 C 0.39280(15) -0.08246(12) 0.44296(10) 0.0323(4) Uani 1 1 d . . . H9A H 0.3164 -0.0814 0.4403 0.039 Uiso 1 1 calc R . . H9B H 0.4241 -0.0546 0.4903 0.039 Uiso 1 1 calc R . . O10 O 0.42135(10) -0.03661(8) 0.38108(7) 0.0299(3) Uani 1 1 d . . . C11 C 0.38632(14) 0.05023(12) 0.37892(10) 0.0309(4) Uani 1 1 d . . . H11A H 0.4031 0.0762 0.4293 0.037 Uiso 1 1 calc R . . H11B H 0.3101 0.0521 0.3637 0.037 Uiso 1 1 calc R . . C12 C 0.43856(13) 0.10008(11) 0.32398(10) 0.0291(4) Uani 1 1 d . . . H12A H 0.4333 0.0675 0.2766 0.035 Uiso 1 1 calc R . . H12B H 0.402 0.1553 0.313 0.035 Uiso 1 1 calc R . . O13 O 0.54612(9) 0.11654(7) 0.35182(7) 0.0282(3) Uani 1 1 d . . . C14 C 0.61586(12) 0.05436(11) 0.32990(9) 0.0236(4) Uani 1 1 d . . . H14A H 0.6236 0.0619 0.2767 0.028 Uiso 1 1 calc R . . H14B H 0.5905 -0.0045 0.337 0.028 Uiso 1 1 calc R . . C15 C 0.71845(12) 0.07048(10) 0.38067(9) 0.0197(3) Uani 1 1 d . . . H15A H 0.7349 0.1324 0.3791 0.024 Uiso 1 1 calc R . . H15B H 0.7098 0.0564 0.4327 0.024 Uiso 1 1 calc R . . N21 N 0.91092(10) -0.01046(8) 0.21042(7) 0.0174(3) Uani 1 1 d . . . C22 C 0.69091(13) -0.01184(12) 0.13304(10) 0.0295(4) Uani 1 1 d . . . H22A H 0.6654 -0.0208 0.1807 0.044 Uiso 1 1 calc R . . H22B H 0.6438 -0.0397 0.0926 0.044 Uiso 1 1 calc R . . H22C H 0.6939 0.0498 0.1229 0.044 Uiso 1 1 calc R . . C23 C 0.80709(15) -0.17723(11) 0.15242(11) 0.0337(4) Uani 1 1 d . . . H23A H 0.8702 -0.2076 0.1444 0.051 Uiso 1 1 calc R . . H23B H 0.7481 -0.1979 0.1165 0.051 Uiso 1 1 calc R . . H23C H 0.7938 -0.1879 0.2035 0.051 Uiso 1 1 calc R . . C24 C 0.86349(15) -0.03921(14) 0.04405(10) 0.0361(4) Uani 1 1 d . . . H24A H 0.8631 0.0226 0.0343 0.054 Uiso 1 1 calc R . . H24B H 0.8142 -0.0677 0.0054 0.054 Uiso 1 1 calc R . . H24C H 0.9334 -0.062 0.0433 0.054 Uiso 1 1 calc R . . C25 C 1.07091(14) -0.13579(12) 0.17369(11) 0.0347(4) Uani 1 1 d . . . H25A H 1.0452 -0.1824 0.2022 0.052 Uiso 1 1 calc R . . H25B H 1.1458 -0.1425 0.1746 0.052 Uiso 1 1 calc R . . H25C H 1.0354 -0.1376 0.1218 0.052 Uiso 1 1 calc R . . C26 C 1.11383(13) -0.03900(11) 0.31540(9) 0.0266(4) Uani 1 1 d . . . H26A H 1.1167 0.0174 0.3395 0.04 Uiso 1 1 calc R . . H26B H 1.1846 -0.0601 0.315 0.04 Uiso 1 1 calc R . . H26C H 1.0765 -0.0792 0.3433 0.04 Uiso 1 1 calc R . . C27 C 1.10892(15) 0.05513(12) 0.16685(10) 0.0319(4) Uani 1 1 d . . . H27A H 1.0816 0.0531 0.1133 0.048 Uiso 1 1 calc R . . H27B H 1.184 0.0451 0.1743 0.048 Uiso 1 1 calc R . . H27C H 1.0948 0.1116 0.1869 0.048 Uiso 1 1 calc R . . O28 O 0.98020(8) 0.12259(6) 0.31159(6) 0.0176(2) Uani 1 1 d . . . C29 C 0.97616(11) 0.16686(9) 0.37651(8) 0.0162(3) Uani 1 1 d . . . C30 C 1.01550(12) 0.25123(9) 0.38848(8) 0.0172(3) Uani 1 1 d . . . C31 C 1.00231(12) 0.29143(9) 0.45600(9) 0.0188(3) Uani 1 1 d . . . H31 H 1.0284 0.348 0.4647 0.023 Uiso 1 1 calc R . . C32 C 0.95291(12) 0.25318(9) 0.51152(8) 0.0174(3) Uani 1 1 d . . . C33 C 0.92063(12) 0.16853(10) 0.49902(8) 0.0186(3) Uani 1 1 d . . . H33 H 0.8897 0.1394 0.5361 0.022 Uiso 1 1 calc R . . C34 C 0.93265(12) 0.12539(9) 0.43314(8) 0.0169(3) Uani 1 1 d . . . C35 C 0.89969(12) 0.03281(9) 0.42228(8) 0.0181(3) Uani 1 1 d . . . H35A H 0.959 -0.0012 0.4101 0.022 Uiso 1 1 calc R . . H35B H 0.8815 0.0105 0.4698 0.022 Uiso 1 1 calc R . . C36 C 1.06789(13) 0.29757(10) 0.32879(9) 0.0216(3) Uani 1 1 d . . . C37 C 1.10993(16) 0.38640(11) 0.35542(11) 0.0333(4) Uani 1 1 d . . . H37A H 1.1605 0.38 0.4012 0.05 Uiso 1 1 calc R . . H37B H 1.0524 0.4227 0.3657 0.05 Uiso 1 1 calc R . . H37C H 1.1436 0.413 0.3164 0.05 Uiso 1 1 calc R . . C38 C 1.16016(14) 0.24417(11) 0.31026(10) 0.0285(4) Uani 1 1 d . . . H38A H 1.1877 0.2706 0.2683 0.043 Uiso 1 1 calc R . . H38B H 1.1367 0.1858 0.2966 0.043 Uiso 1 1 calc R . . H38C H 1.2147 0.2422 0.3541 0.043 Uiso 1 1 calc R . . C39 C 0.98647(15) 0.31156(12) 0.25821(10) 0.0315(4) Uani 1 1 d . . . H39A H 0.9271 0.3432 0.2717 0.047 Uiso 1 1 calc R . . H39B H 0.963 0.2559 0.2369 0.047 Uiso 1 1 calc R . . H39C H 1.0177 0.3445 0.2213 0.047 Uiso 1 1 calc R . . C40 C 0.93815(12) 0.30015(10) 0.58418(8) 0.0196(3) Uani 1 1 d . . . C41 C 0.83235(14) 0.27751(11) 0.60721(10) 0.0282(4) Uani 1 1 d . . . H41A H 0.7766 0.2915 0.5661 0.042 Uiso 1 1 calc R . . H41B H 0.8229 0.3105 0.6518 0.042 Uiso 1 1 calc R . . H41C H 0.8303 0.2161 0.6184 0.042 Uiso 1 1 calc R . . C42 C 1.02625(14) 0.27394(11) 0.64739(9) 0.0276(4) Uani 1 1 d . . . H42A H 1.023 0.2121 0.6561 0.041 Uiso 1 1 calc R . . H42B H 1.0182 0.3047 0.6934 0.041 Uiso 1 1 calc R . . H42C H 1.0935 0.2884 0.6328 0.041 Uiso 1 1 calc R . . C43 C 0.94054(15) 0.39804(10) 0.57510(10) 0.0285(4) Uani 1 1 d . . . H43A H 1.0089 0.4156 0.5643 0.043 Uiso 1 1 calc R . . H43B H 0.9274 0.4255 0.6215 0.043 Uiso 1 1 calc R . . H43C H 0.8869 0.4155 0.5337 0.043 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 Ge1 0.01690(9) 0.01532(8) 0.01541(8) -0.00116(6) 0.00357(6) 0.00013(6) Si1 0.0188(2) 0.0240(2) 0.0184(2) -0.00677(17) 0.00257(17) -0.00083(18) Si2 0.0165(2) 0.0211(2) 0.0210(2) -0.00146(17) 0.00376(17) 0.00116(18) N1 0.0179(7) 0.0132(6) 0.0177(6) -0.0032(5) 0.0047(5) -0.0025(5) C2 0.0211(8) 0.0143(7) 0.0210(8) -0.0036(6) 0.0057(6) -0.0042(6) C3 0.0381(10) 0.0173(7) 0.0261(9) -0.0027(7) 0.0097(8) -0.0099(7) O4 0.0354(7) 0.0156(5) 0.0317(6) -0.0016(5) 0.0109(5) -0.0078(5) C5 0.0406(11) 0.0196(8) 0.0363(10) 0.0074(7) 0.0062(8) -0.0066(8) C6 0.0421(11) 0.0268(9) 0.0315(10) 0.0044(8) 0.0078(8) -0.0150(8) O7 0.0268(7) 0.0324(7) 0.0333(7) -0.0024(5) 0.0081(5) -0.0102(5) C8 0.0278(10) 0.0465(11) 0.0303(10) 0.0035(8) 0.0066(8) -0.0164(9) C9 0.0238(10) 0.0518(12) 0.0233(9) -0.0011(8) 0.0095(7) -0.0109(8) O10 0.0320(7) 0.0336(7) 0.0278(6) -0.0023(5) 0.0162(5) -0.0047(6) C11 0.0193(9) 0.0393(10) 0.0356(10) -0.0114(8) 0.0095(8) -0.0034(8) C12 0.0184(9) 0.0317(9) 0.0372(10) -0.0001(8) 0.0042(7) 0.0035(7) O13 0.0173(6) 0.0246(6) 0.0444(7) -0.0098(6) 0.0104(5) -0.0002(5) C14 0.0183(8) 0.0245(8) 0.0298(9) -0.0069(7) 0.0092(7) -0.0002(7) C15 0.0206(8) 0.0182(7) 0.0220(8) -0.0048(6) 0.0091(7) -0.0023(6) N21 0.0168(7) 0.0189(6) 0.0164(6) -0.0036(5) 0.0028(5) 0.0010(5) C22 0.0206(9) 0.0366(10) 0.0294(9) -0.0099(8) -0.0023(7) 0.0013(8) C23 0.0315(10) 0.0267(9) 0.0422(11) -0.0107(8) 0.0033(8) -0.0057(8) C24 0.0340(11) 0.0531(12) 0.0211(9) -0.0073(8) 0.0042(8) -0.0021(9) C25 0.0253(10) 0.0338(10) 0.0450(11) -0.0117(9) 0.0049(8) 0.0088(8) C26 0.0222(9) 0.0272(9) 0.0286(9) 0.0008(7) -0.0012(7) 0.0025(7) C27 0.0273(10) 0.0396(10) 0.0308(9) 0.0030(8) 0.0108(8) -0.0026(8) O28 0.0190(6) 0.0178(5) 0.0169(5) -0.0042(4) 0.0055(4) -0.0034(4) C29 0.0143(8) 0.0169(7) 0.0172(7) -0.0030(6) 0.0018(6) -0.0006(6) C30 0.0150(8) 0.0162(7) 0.0204(7) 0.0007(6) 0.0025(6) -0.0019(6) C31 0.0177(8) 0.0142(7) 0.0239(8) -0.0029(6) 0.0016(6) -0.0025(6) C32 0.0157(8) 0.0173(7) 0.0182(7) -0.0023(6) -0.0004(6) 0.0004(6) C33 0.0201(8) 0.0192(7) 0.0167(7) 0.0006(6) 0.0033(6) -0.0027(6) C34 0.0169(8) 0.0157(7) 0.0174(7) -0.0010(6) 0.0006(6) -0.0012(6) C35 0.0210(8) 0.0163(7) 0.0170(7) -0.0001(6) 0.0036(6) -0.0037(6) C36 0.0233(9) 0.0183(7) 0.0248(8) -0.0013(6) 0.0086(7) -0.0053(7) C37 0.0423(11) 0.0206(8) 0.0410(10) -0.0038(8) 0.0193(9) -0.0120(8) C38 0.0251(9) 0.0262(8) 0.0372(10) -0.0038(8) 0.0148(8) -0.0050(7) C39 0.0396(11) 0.0302(9) 0.0261(9) 0.0078(8) 0.0090(8) -0.0014(8) C40 0.0206(8) 0.0187(7) 0.0193(8) -0.0039(6) 0.0026(6) 0.0002(6) C41 0.0263(9) 0.0277(9) 0.0327(9) -0.0084(7) 0.0106(7) -0.0005(8) C42 0.0304(10) 0.0310(9) 0.0202(8) -0.0053(7) -0.0001(7) 0.0053(8) C43 0.0391(11) 0.0197(8) 0.0270(9) -0.0061(7) 0.0056(8) -0.0008(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 O28 1.8910(10) . ? Ge1 N21 1.9131(12) . ? Ge1 N1 2.3181(13) . ? Si1 N21 1.7547(13) . ? Si1 C23 1.8734(18) . ? Si1 C22 1.8811(18) . ? Si1 C24 1.8861(18) . ? Si2 N21 1.7543(14) . ? Si2 C26 1.8739(17) . ? Si2 C27 1.8743(18) . ? Si2 C25 1.8820(18) . ? N1 C2 1.4937(18) . ? N1 C15 1.4939(19) . ? N1 C35 1.5012(19) . ? C2 C3 1.528(2) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 O4 1.4219(19) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? O4 C5 1.428(2) . ? C5 C6 1.513(3) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 O7 1.423(2) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? O7 C8 1.429(2) . ? C8 C9 1.498(3) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 O10 1.425(2) . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? O10 C11 1.428(2) . ? C11 C12 1.505(3) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 O13 1.438(2) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? O13 C14 1.4268(19) . ? C14 C15 1.521(2) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 H27A 0.98 . ? C27 H27B 0.98 . ? C27 H27C 0.98 . ? O28 C29 1.3700(17) . ? C29 C34 1.403(2) . ? C29 C30 1.417(2) . ? C30 C31 1.407(2) . ? C30 C36 1.543(2) . ? C31 C32 1.407(2) . ? C31 H31 0.95 . ? C32 C33 1.393(2) . ? C32 C40 1.542(2) . ? C33 C34 1.398(2) . ? C33 H33 0.95 . ? C34 C35 1.511(2) . ? C35 H35A 0.99 . ? C35 H35B 0.99 . ? C36 C37 1.539(2) . ? C36 C38 1.542(2) . ? C36 C39 1.544(2) . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C38 H38A 0.98 . ? C38 H38B 0.98 . ? C38 H38C 0.98 . ? C39 H39A 0.98 . ? C39 H39B 0.98 . ? C39 H39C 0.98 . ? C40 C43 1.536(2) . ? C40 C41 1.542(2) . ? C40 C42 1.545(2) . ? C41 H41A 0.98 . ? C41 H41B 0.98 . ? C41 H41C 0.98 . ? C42 H42A 0.98 . ? C42 H42B 0.98 . ? C42 H42C 0.98 . ? C43 H43A 0.98 . ? C43 H43B 0.98 . ? C43 H43C 0.98 . ? 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 O28 Ge1 N21 95.72(5) . . ? O28 Ge1 N1 90.07(4) . . ? N21 Ge1 N1 100.14(5) . . ? N21 Si1 C23 113.95(8) . . ? N21 Si1 C22 110.60(7) . . ? C23 Si1 C22 105.28(9) . . ? N21 Si1 C24 111.46(8) . . ? C23 Si1 C24 109.81(9) . . ? C22 Si1 C24 105.20(9) . . ? N21 Si2 C26 113.80(7) . . ? N21 Si2 C27 111.13(8) . . ? C26 Si2 C27 109.10(8) . . ? N21 Si2 C25 111.52(7) . . ? C26 Si2 C25 103.61(8) . . ? C27 Si2 C25 107.24(9) . . ? C2 N1 C15 113.51(12) . . ? C2 N1 C35 109.64(11) . . ? C15 N1 C35 108.96(11) . . ? C2 N1 Ge1 112.19(9) . . ? C15 N1 Ge1 105.97(9) . . ? C35 N1 Ge1 106.25(9) . . ? N1 C2 C3 114.79(12) . . ? N1 C2 H2A 108.6 . . ? C3 C2 H2A 108.6 . . ? N1 C2 H2B 108.6 . . ? C3 C2 H2B 108.6 . . ? H2A C2 H2B 107.5 . . ? O4 C3 C2 106.32(13) . . ? O4 C3 H3A 110.5 . . ? C2 C3 H3A 110.5 . . ? O4 C3 H3B 110.5 . . ? C2 C3 H3B 110.5 . . ? H3A C3 H3B 108.7 . . ? C3 O4 C5 112.99(13) . . ? O4 C5 C6 112.10(15) . . ? O4 C5 H5A 109.2 . . ? C6 C5 H5A 109.2 . . ? O4 C5 H5B 109.2 . . ? C6 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? O7 C6 C5 109.63(14) . . ? O7 C6 H6A 109.7 . . ? C5 C6 H6A 109.7 . . ? O7 C6 H6B 109.7 . . ? C5 C6 H6B 109.7 . . ? H6A C6 H6B 108.2 . . ? C6 O7 C8 112.64(14) . . ? O7 C8 C9 109.78(15) . . ? O7 C8 H8A 109.7 . . ? C9 C8 H8A 109.7 . . ? O7 C8 H8B 109.7 . . ? C9 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? O10 C9 C8 110.06(15) . . ? O10 C9 H9A 109.6 . . ? C8 C9 H9A 109.6 . . ? O10 C9 H9B 109.6 . . ? C8 C9 H9B 109.6 . . ? H9A C9 H9B 108.2 . . ? C9 O10 C11 112.09(13) . . ? O10 C11 C12 109.42(14) . . ? O10 C11 H11A 109.8 . . ? C12 C11 H11A 109.8 . . ? O10 C11 H11B 109.8 . . ? C12 C11 H11B 109.8 . . ? H11A C11 H11B 108.2 . . ? O13 C12 C11 112.19(15) . . ? O13 C12 H12A 109.2 . . ? C11 C12 H12A 109.2 . . ? O13 C12 H12B 109.2 . . ? C11 C12 H12B 109.2 . . ? H12A C12 H12B 107.9 . . ? C14 O13 C12 114.22(13) . . ? O13 C14 C15 104.98(12) . . ? O13 C14 H14A 110.8 . . ? C15 C14 H14A 110.8 . . ? O13 C14 H14B 110.8 . . ? C15 C14 H14B 110.8 . . ? H14A C14 H14B 108.8 . . ? N1 C15 C14 115.02(12) . . ? N1 C15 H15A 108.5 . . ? C14 C15 H15A 108.5 . . ? N1 C15 H15B 108.5 . . ? C14 C15 H15B 108.5 . . ? H15A C15 H15B 107.5 . . ? Si2 N21 Si1 119.43(7) . . ? Si2 N21 Ge1 123.88(7) . . ? Si1 N21 Ge1 113.95(7) . . ? Si1 C22 H22A 109.5 . . ? Si1 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? Si1 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? Si1 C23 H23A 109.5 . . ? Si1 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? Si1 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? 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 . . ? Si2 C25 H25A 109.5 . . ? Si2 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? Si2 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? Si2 C26 H26A 109.5 . . ? Si2 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? Si2 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? Si2 C27 H27A 109.5 . . ? Si2 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? Si2 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 O28 Ge1 117.84(9) . . ? O28 C29 C34 117.83(13) . . ? O28 C29 C30 122.53(13) . . ? C34 C29 C30 119.63(13) . . ? C31 C30 C29 117.16(14) . . ? C31 C30 C36 121.68(13) . . ? C29 C30 C36 121.14(13) . . ? C30 C31 C32 124.16(14) . . ? C30 C31 H31 117.9 . . ? C32 C31 H31 117.9 . . ? C33 C32 C31 116.50(14) . . ? C33 C32 C40 120.92(14) . . ? C31 C32 C40 122.55(13) . . ? C32 C33 C34 121.55(14) . . ? C32 C33 H33 119.2 . . ? C34 C33 H33 119.2 . . ? C33 C34 C29 120.77(13) . . ? C33 C34 C35 120.24(13) . . ? C29 C34 C35 118.99(13) . . ? N1 C35 C34 113.05(12) . . ? N1 C35 H35A 109 . . ? C34 C35 H35A 109 . . ? N1 C35 H35B 109 . . ? C34 C35 H35B 109 . . ? H35A C35 H35B 107.8 . . ? C37 C36 C38 107.58(14) . . ? C37 C36 C30 112.17(13) . . ? C38 C36 C30 110.11(13) . . ? C37 C36 C39 107.29(14) . . ? C38 C36 C39 110.87(14) . . ? C30 C36 C39 108.80(13) . . ? C36 C37 H37A 109.5 . . ? C36 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? C36 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? C36 C38 H38A 109.5 . . ? C36 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C36 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C36 C39 H39A 109.5 . . ? C36 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C36 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C43 C40 C32 111.94(13) . . ? C43 C40 C41 106.87(14) . . ? C32 C40 C41 110.87(13) . . ? C43 C40 C42 108.48(13) . . ? C32 C40 C42 109.15(13) . . ? C41 C40 C42 109.46(14) . . ? C40 C41 H41A 109.5 . . ? C40 C41 H41B 109.5 . . ? H41A C41 H41B 109.5 . . ? C40 C41 H41C 109.5 . . ? H41A C41 H41C 109.5 . . ? H41B C41 H41C 109.5 . . ? C40 C42 H42A 109.5 . . ? C40 C42 H42B 109.5 . . ? H42A C42 H42B 109.5 . . ? C40 C42 H42C 109.5 . . ? H42A C42 H42C 109.5 . . ? H42B C42 H42C 109.5 . . ? C40 C43 H43A 109.5 . . ? C40 C43 H43B 109.5 . . ? H43A C43 H43B 109.5 . . ? C40 C43 H43C 109.5 . . ? H43A C43 H43C 109.5 . . ? H43B C43 H43C 109.5 . . ? 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 O28 Ge1 N1 C2 -122.98(10) . . . . ? N21 Ge1 N1 C2 -27.16(11) . . . . ? O28 Ge1 N1 C15 112.63(9) . . . . ? N21 Ge1 N1 C15 -151.55(9) . . . . ? O28 Ge1 N1 C35 -3.19(9) . . . . ? N21 Ge1 N1 C35 92.63(9) . . . . ? C15 N1 C2 C3 -61.85(18) . . . . ? C35 N1 C2 C3 60.25(17) . . . . ? Ge1 N1 C2 C3 178.05(11) . . . . ? N1 C2 C3 O4 173.23(13) . . . . ? C2 C3 O4 C5 -176.85(14) . . . . ? C3 O4 C5 C6 99.52(17) . . . . ? O4 C5 C6 O7 -62.29(19) . . . . ? C5 C6 O7 C8 175.39(14) . . . . ? C6 O7 C8 C9 -173.62(14) . . . . ? O7 C8 C9 O10 65.14(18) . . . . ? C8 C9 O10 C11 179.00(14) . . . . ? C9 O10 C11 C12 167.28(14) . . . . ? O10 C11 C12 O13 -72.94(18) . . . . ? C11 C12 O13 C14 93.41(17) . . . . ? C12 O13 C14 C15 -165.62(13) . . . . ? C2 N1 C15 C14 -49.03(17) . . . . ? C35 N1 C15 C14 -171.50(13) . . . . ? Ge1 N1 C15 C14 74.53(14) . . . . ? O13 C14 C15 N1 -171.89(12) . . . . ? C26 Si2 N21 Si1 -142.30(8) . . . . ? C27 Si2 N21 Si1 94.07(10) . . . . ? C25 Si2 N21 Si1 -25.53(11) . . . . ? C26 Si2 N21 Ge1 57.58(11) . . . . ? C27 Si2 N21 Ge1 -66.05(11) . . . . ? C25 Si2 N21 Ge1 174.35(9) . . . . ? C23 Si1 N21 Si2 72.62(11) . . . . ? C22 Si1 N21 Si2 -169.01(9) . . . . ? C24 Si1 N21 Si2 -52.34(11) . . . . ? C23 Si1 N21 Ge1 -125.37(9) . . . . ? C22 Si1 N21 Ge1 -7.00(10) . . . . ? C24 Si1 N21 Ge1 109.66(9) . . . . ? O28 Ge1 N21 Si2 -9.24(9) . . . . ? N1 Ge1 N21 Si2 -100.33(8) . . . . ? O28 Ge1 N21 Si1 -170.32(7) . . . . ? N1 Ge1 N21 Si1 98.58(7) . . . . ? N21 Ge1 O28 C29 -152.83(10) . . . . ? N1 Ge1 O28 C29 -52.63(10) . . . . ? Ge1 O28 C29 C34 60.43(16) . . . . ? Ge1 O28 C29 C30 -120.65(13) . . . . ? O28 C29 C30 C31 177.02(13) . . . . ? C34 C29 C30 C31 -4.1(2) . . . . ? O28 C29 C30 C36 -1.4(2) . . . . ? C34 C29 C30 C36 177.52(14) . . . . ? C29 C30 C31 C32 0.0(2) . . . . ? C36 C30 C31 C32 178.35(14) . . . . ? C30 C31 C32 C33 3.4(2) . . . . ? C30 C31 C32 C40 -178.79(14) . . . . ? C31 C32 C33 C34 -2.8(2) . . . . ? C40 C32 C33 C34 179.41(14) . . . . ? C32 C33 C34 C29 -1.2(2) . . . . ? C32 C33 C34 C35 178.21(14) . . . . ? O28 C29 C34 C33 -176.27(13) . . . . ? C30 C29 C34 C33 4.8(2) . . . . ? O28 C29 C34 C35 4.3(2) . . . . ? C30 C29 C34 C35 -174.66(13) . . . . ? C2 N1 C35 C34 175.23(12) . . . . ? C15 N1 C35 C34 -59.99(16) . . . . ? Ge1 N1 C35 C34 53.79(13) . . . . ? C33 C34 C35 N1 112.80(15) . . . . ? C29 C34 C35 N1 -67.76(18) . . . . ? C31 C30 C36 C37 4.8(2) . . . . ? C29 C30 C36 C37 -176.88(15) . . . . ? C31 C30 C36 C38 124.56(16) . . . . ? C29 C30 C36 C38 -57.11(19) . . . . ? C31 C30 C36 C39 -113.76(16) . . . . ? C29 C30 C36 C39 64.57(19) . . . . ? C33 C32 C40 C43 -158.98(15) . . . . ? C31 C32 C40 C43 23.4(2) . . . . ? C33 C32 C40 C41 -39.7(2) . . . . ? C31 C32 C40 C41 142.59(15) . . . . ? C33 C32 C40 C42 80.91(18) . . . . ? C31 C32 C40 C42 -96.75(17) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 942093' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_SR34 _audit_creation_date 2012-03-13T08:46:14-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C32 H60 F3 Ge Li N2 O8 S Si2' _chemical_formula_sum 'C32 H60 F3 Ge Li N2 O8 S Si2' _chemical_formula_weight 825.59 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.1913(2) _cell_length_b 11.3799(2) _cell_length_c 21.3025(4) _cell_angle_alpha 97.0250(10) _cell_angle_beta 100.1770(10) _cell_angle_gamma 98.1600(10) _cell_volume 2145.92(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9968 _cell_measurement_theta_min 2.66 _cell_measurement_theta_max 27.3 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.07 _exptl_crystal_density_diffrn 1.278 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 872 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.875 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.869 _exptl_absorpt_correction_T_max 0.941 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0334 _diffrn_reflns_av_unetI/netI 0.0371 _diffrn_reflns_number 34506 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.991 _diffrn_measured_fraction_theta_max 0.991 _reflns_number_total 9720 _reflns_number_gt 8085 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0351P)^2^+0.8331P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 9720 _refine_ls_number_parameters 463 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0448 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0813 _refine_ls_wR_factor_gt 0.0763 _refine_ls_goodness_of_fit_ref 1.032 _refine_ls_restrained_S_all 1.032 _refine_ls_shift/su_max 0.01 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.491 _refine_diff_density_min -0.341 _refine_diff_density_rms 0.054 _iucr_refine_instructions_details ; .res file for SHELXL : job.res ................................................................. TITL import in P -1 CELL 0.71073 9.1913 11.3799 21.3025 97.025 100.177 98.160 ZERR 2.00 0.0002 0.0002 0.0004 0.001 0.001 0.001 LATT 1 SFAC C H N O F SI S GE LI UNIT 64.00 120.00 4.00 16.00 6.00 4.00 2.00 2.00 2.00 MERG 2 FMAP 2 PLAN 20 ACTA BOND $H CONF LIST 4 WPDB -2 L.S. 4 TEMP -123.00 WGHT 0.035100 0.833100 FVAR 0.42096 SI1 6 0.164234 0.144005 0.363416 11.00000 0.02402 0.02787 = 0.02551 0.00067 0.00600 0.00639 SI2 6 0.234014 -0.097498 0.392051 11.00000 0.03823 0.02325 = 0.04222 0.00980 0.02046 0.00224 N1 3 0.282232 0.035891 0.362169 11.00000 0.02202 0.02084 = 0.02313 0.00244 0.00751 0.00065 C2 1 0.152187 0.230581 0.294011 11.00000 0.04864 0.05903 = 0.04651 0.02258 0.01599 0.03400 AFIX 137 H2A 2 0.250788 0.277405 0.294855 11.00000 -1.50000 H2B 2 0.079333 0.284970 0.297379 11.00000 -1.50000 H2C 2 0.120128 0.174729 0.253434 11.00000 -1.50000 AFIX 0 C3 1 0.222501 0.252355 0.439746 11.00000 0.04694 0.03636 = 0.04122 -0.00829 0.01225 0.00863 AFIX 137 H3A 2 0.204670 0.211082 0.476133 11.00000 -1.50000 H3B 2 0.164103 0.317914 0.437455 11.00000 -1.50000 H3C 2 0.329404 0.285110 0.445833 11.00000 -1.50000 AFIX 0 C4 1 -0.035957 0.073532 0.356488 11.00000 0.02700 0.05342 = 0.05696 -0.00008 0.00762 0.00759 AFIX 137 H4A 2 -0.069475 0.018473 0.315684 11.00000 -1.50000 H4B 2 -0.098602 0.136338 0.357587 11.00000 -1.50000 H4C 2 -0.044561 0.028906 0.392566 11.00000 -1.50000 AFIX 0 C5 1 0.187361 -0.069393 0.473905 11.00000 0.06210 0.05143 = 0.04433 0.02392 0.02430 0.01085 AFIX 137 H5A 2 0.278935 -0.034662 0.505620 11.00000 -1.50000 H5B 2 0.143147 -0.145361 0.485438 11.00000 -1.50000 H5C 2 0.115539 -0.013418 0.473575 11.00000 -1.50000 AFIX 0 C6 1 0.071283 -0.200133 0.336901 11.00000 0.07564 0.03538 = 0.06594 -0.00314 0.02868 -0.02250 AFIX 137 H6A 2 -0.022425 -0.173153 0.343243 11.00000 -1.50000 H6B 2 0.069749 -0.282174 0.346700 11.00000 -1.50000 H6C 2 0.081633 -0.198613 0.291990 11.00000 -1.50000 AFIX 0 C7 1 0.391822 -0.185744 0.399003 11.00000 0.07134 0.03968 = 0.11102 0.04404 0.05081 0.02637 AFIX 137 H7A 2 0.418745 -0.202723 0.356701 11.00000 -1.50000 H7B 2 0.360453 -0.261503 0.414128 11.00000 -1.50000 H7C 2 0.478834 -0.139180 0.429817 11.00000 -1.50000 AFIX 0 GE1 8 0.484618 0.065174 0.351457 11.00000 0.01997 0.01854 = 0.01931 0.00313 0.00365 0.00174 O11 4 0.487748 0.225497 0.339229 11.00000 0.02562 0.01695 = 0.02003 0.00137 0.00913 -0.00107 C12 1 0.582429 0.272023 0.302427 11.00000 0.02425 0.01623 = 0.01787 0.00385 0.00648 0.00378 C13 1 0.698937 0.370017 0.327729 11.00000 0.02527 0.01598 = 0.01799 0.00205 0.00564 0.00335 C14 1 0.787968 0.411786 0.285191 11.00000 0.02249 0.01672 = 0.02285 0.00172 0.00445 -0.00050 AFIX 43 H14 2 0.867604 0.477111 0.301666 11.00000 -1.20000 AFIX 0 C15 1 0.766479 0.363088 0.220163 11.00000 0.02655 0.02032 = 0.02170 0.00572 0.00890 0.00627 C16 1 0.650151 0.267201 0.197287 11.00000 0.02966 0.02073 = 0.01540 0.00054 0.00494 0.00537 AFIX 43 H16 2 0.632379 0.231945 0.153260 11.00000 -1.20000 AFIX 0 C17 1 0.558896 0.221426 0.237254 11.00000 0.02377 0.01660 = 0.01883 0.00210 0.00413 0.00370 C18 1 0.726008 0.430856 0.398412 11.00000 0.03087 0.02129 = 0.01792 -0.00128 0.00668 -0.00279 C19 1 0.857774 0.536193 0.414264 11.00000 0.04237 0.03383 = 0.02304 -0.00727 0.00924 -0.01256 AFIX 137 H19A 2 0.949022 0.507215 0.405935 11.00000 -1.50000 H19B 2 0.872680 0.570954 0.459811 11.00000 -1.50000 H19C 2 0.835641 0.597579 0.387154 11.00000 -1.50000 AFIX 0 C20 1 0.584909 0.480713 0.411412 11.00000 0.04295 0.02416 = 0.02828 -0.00314 0.01539 0.00154 AFIX 137 H20A 2 0.566864 0.543673 0.384863 11.00000 -1.50000 H20B 2 0.599918 0.514426 0.457119 11.00000 -1.50000 H20C 2 0.498275 0.415726 0.400515 11.00000 -1.50000 AFIX 0 C21 1 0.763903 0.341139 0.444596 11.00000 0.04544 0.03426 = 0.01927 0.00302 0.00146 -0.00077 AFIX 137 H21A 2 0.680245 0.274056 0.437339 11.00000 -1.50000 H21B 2 0.781093 0.381402 0.489275 11.00000 -1.50000 H21C 2 0.854558 0.310692 0.436654 11.00000 -1.50000 AFIX 0 C22 1 0.862332 0.413286 0.173820 11.00000 0.03011 0.02518 = 0.02322 0.00446 0.01280 0.00524 C23 1 0.931779 0.312467 0.141320 11.00000 0.03228 0.03316 = 0.02775 0.00631 0.01271 0.01072 AFIX 137 H23A 2 0.987201 0.343822 0.109950 11.00000 -1.50000 H23B 2 0.851961 0.246404 0.119169 11.00000 -1.50000 H23C 2 1.000357 0.283036 0.174163 11.00000 -1.50000 AFIX 0 C24 1 0.987079 0.515125 0.208427 11.00000 0.04825 0.03576 = 0.04177 0.00113 0.02712 -0.00828 AFIX 137 H24A 2 0.943500 0.579662 0.229095 11.00000 -1.50000 H24B 2 1.043123 0.546157 0.177173 11.00000 -1.50000 H24C 2 1.054940 0.485131 0.241297 11.00000 -1.50000 AFIX 0 C25 1 0.761154 0.461722 0.120951 11.00000 0.04792 0.04168 = 0.03327 0.01955 0.02347 0.02196 AFIX 137 H25A 2 0.709240 0.521171 0.140980 11.00000 -1.50000 H25B 2 0.687175 0.395316 0.094845 11.00000 -1.50000 H25C 2 0.822564 0.499549 0.093331 11.00000 -1.50000 AFIX 0 C26 1 0.430092 0.119726 0.210248 11.00000 0.02388 0.01920 = 0.01786 0.00071 0.00263 0.00354 AFIX 23 H26A 2 0.335553 0.146304 0.217422 11.00000 -1.20000 H26B 2 0.423078 0.100536 0.163100 11.00000 -1.20000 AFIX 0 N31 3 0.445830 0.008793 0.239867 11.00000 0.01741 0.01468 = 0.02303 0.00005 0.00385 0.00056 C32 1 0.304949 -0.080593 0.219893 11.00000 0.01721 0.02095 = 0.02842 -0.00379 0.00661 -0.00059 AFIX 23 H32A 2 0.229233 -0.050182 0.242419 11.00000 -1.20000 H32B 2 0.325016 -0.155593 0.236333 11.00000 -1.20000 AFIX 0 C33 1 0.234034 -0.113532 0.148988 11.00000 0.01825 0.02490 = 0.03219 -0.00662 0.00045 0.00301 AFIX 23 H33A 2 0.133108 -0.161423 0.144674 11.00000 -1.20000 H33B 2 0.221362 -0.038991 0.130584 11.00000 -1.20000 AFIX 0 O34 4 0.319143 -0.180033 0.112765 11.00000 0.02898 0.04537 = 0.02040 -0.00434 0.00074 0.01736 C35 1 0.236367 -0.225506 0.047979 11.00000 0.03307 0.05018 = 0.02038 0.00089 0.00212 0.01540 AFIX 23 H35A 2 0.298511 -0.204261 0.016211 11.00000 -1.20000 H35B 2 0.144460 -0.189217 0.039507 11.00000 -1.20000 AFIX 0 C36 1 0.195461 -0.359349 0.041505 11.00000 0.02313 0.05714 = 0.02124 -0.00191 0.00136 0.00212 AFIX 23 H36A 2 0.141669 -0.381891 0.075762 11.00000 -1.20000 H36B 2 0.130614 -0.392418 -0.001034 11.00000 -1.20000 AFIX 0 O37 4 0.335031 -0.403597 0.047788 11.00000 0.02668 0.03304 = 0.03091 -0.00305 0.00312 0.00017 C38 1 0.328786 -0.528684 0.052360 11.00000 0.04179 0.03197 = 0.04405 -0.01179 0.00239 -0.00222 AFIX 23 H38A 2 0.415333 -0.557224 0.037252 11.00000 -1.20000 H38B 2 0.235858 -0.574973 0.024243 11.00000 -1.20000 AFIX 0 C39 1 0.331634 -0.549726 0.120854 11.00000 0.03596 0.02525 = 0.05295 -0.00317 0.00594 -0.00652 AFIX 23 H39A 2 0.233772 -0.542325 0.132918 11.00000 -1.20000 H39B 2 0.353916 -0.630862 0.126384 11.00000 -1.20000 AFIX 0 O40 4 0.447055 -0.459692 0.159512 11.00000 0.02813 0.02393 = 0.03306 0.00029 0.00497 -0.00177 C41 1 0.460272 -0.456493 0.227282 11.00000 0.03218 0.02535 = 0.03846 0.01130 0.01106 0.00873 AFIX 23 H41A 2 0.492210 -0.530685 0.240676 11.00000 -1.20000 H41B 2 0.363317 -0.448488 0.240108 11.00000 -1.20000 AFIX 0 C42 1 0.576219 -0.349236 0.257312 11.00000 0.03230 0.02559 = 0.02987 0.00921 0.00454 0.01157 AFIX 23 H42A 2 0.583781 -0.335351 0.304656 11.00000 -1.20000 H42B 2 0.675438 -0.361352 0.248196 11.00000 -1.20000 AFIX 0 O43 4 0.529261 -0.249075 0.229499 11.00000 0.02354 0.01793 = 0.02816 0.00480 0.00068 0.00343 C44 1 0.629317 -0.138825 0.256451 11.00000 0.02047 0.02320 = 0.02707 -0.00182 0.00149 0.00363 AFIX 23 H44A 2 0.732443 -0.147576 0.251404 11.00000 -1.20000 H44B 2 0.629607 -0.120853 0.303138 11.00000 -1.20000 AFIX 0 C45 1 0.581984 -0.036340 0.223349 11.00000 0.01742 0.01855 = 0.02897 -0.00033 0.00468 0.00032 AFIX 23 H45A 2 0.666849 0.031537 0.234041 11.00000 -1.20000 H45B 2 0.563107 -0.062386 0.176142 11.00000 -1.20000 AFIX 0 S1 7 0.792364 -0.183183 0.095232 11.00000 0.02452 0.02894 = 0.04169 0.00019 0.01479 -0.00027 LI51 9 0.472490 -0.296257 0.129701 11.00000 0.02075 0.02453 = 0.03019 0.00221 0.00425 -0.00081 O52 4 0.648538 -0.246780 0.099355 11.00000 0.02578 0.03792 = 0.06695 0.00860 0.02047 -0.00041 O53 4 0.867260 -0.104477 0.152770 11.00000 0.03886 0.07218 = 0.05975 -0.02954 0.01396 -0.00156 C55 1 0.742284 -0.082873 0.038328 11.00000 0.09764 0.06486 = 0.08698 0.03840 0.05775 0.03626 F56 5 0.669009 -0.143415 -0.017778 11.00000 0.18794 0.17666 = 0.05186 0.03996 0.02358 0.10225 F57 5 0.865511 -0.014243 0.029726 11.00000 0.17169 0.08759 = 0.21156 0.08874 0.14400 0.03728 F58 5 0.655279 -0.008434 0.060345 11.00000 0.13016 0.07787 = 0.12631 0.05742 0.06968 0.06755 O54 4 0.883307 -0.254841 0.064051 11.00000 0.02842 0.03713 = 0.05523 -0.01059 0.01633 -0.00008 HKLF 4 REM import in P -1 REM R1 = 0.0332 for 8085 Fo > 4sig(Fo) and 0.0448 for all 9720 data REM 463 parameters refined using 0 restraints END WGHT 0.0340 0.8519 REM Highest difference peak 0.49, deepest hole -0.34, 1-sigma level 0.05 Q1 1 0.2617 -0.2400 0.1184 11.00000 0.05 0.49 Q2 1 0.7262 -0.1959 0.0540 11.00000 0.05 0.40 Q3 1 0.5176 -0.4720 0.1360 11.00000 0.05 0.36 Q4 1 0.5663 0.2429 0.2692 11.00000 0.05 0.32 Q5 1 0.5094 -0.0194 0.2357 11.00000 0.05 0.30 Q6 1 0.7412 0.3932 0.3079 11.00000 0.05 0.30 Q7 1 0.1795 0.1979 0.3309 11.00000 0.05 0.30 Q8 1 0.8172 0.3928 0.1989 11.00000 0.05 0.30 Q9 1 0.7241 0.0025 0.0894 11.00000 0.05 0.29 Q10 1 0.7249 0.4005 0.3657 11.00000 0.05 0.29 Q11 1 0.6097 0.2378 0.2224 11.00000 0.05 0.29 Q12 1 0.6649 -0.0172 0.0244 11.00000 0.05 0.29 Q13 1 0.5882 0.0786 0.3771 11.00000 0.05 0.29 Q14 1 0.7688 -0.0401 0.0080 11.00000 0.05 0.29 Q15 1 0.5144 -0.3982 0.2367 11.00000 0.05 0.28 Q16 1 0.2088 0.1854 0.4130 11.00000 0.05 0.28 Q17 1 0.7437 0.3941 0.4204 11.00000 0.05 0.28 Q18 1 0.5918 -0.0552 0.0574 11.00000 0.05 0.27 Q19 1 0.3752 -0.0385 0.2331 11.00000 0.05 0.27 Q20 1 0.8271 -0.1672 0.1498 11.00000 0.05 0.27 ; #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' S S 0.1246 0.1234 '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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Si1 Si 0.16423(6) 0.14400(5) 0.36342(2) 0.02575(12) Uani 1 1 d . . . Si2 Si 0.23401(7) -0.09750(5) 0.39205(3) 0.03288(14) Uani 1 1 d . . . N1 N 0.28223(16) 0.03589(13) 0.36217(7) 0.0220(3) Uani 1 1 d . . . C2 C 0.1522(3) 0.2306(2) 0.29401(11) 0.0468(6) Uani 1 1 d . . . H2A H 0.2508 0.2774 0.2949 0.07 Uiso 1 1 calc R . . H2B H 0.0793 0.285 0.2974 0.07 Uiso 1 1 calc R . . H2C H 0.1201 0.1747 0.2534 0.07 Uiso 1 1 calc R . . C3 C 0.2225(3) 0.2524(2) 0.43975(11) 0.0421(5) Uani 1 1 d . . . H3A H 0.2047 0.2111 0.4761 0.063 Uiso 1 1 calc R . . H3B H 0.1641 0.3179 0.4375 0.063 Uiso 1 1 calc R . . H3C H 0.3294 0.2851 0.4458 0.063 Uiso 1 1 calc R . . C4 C -0.0360(2) 0.0735(2) 0.35649(12) 0.0465(6) Uani 1 1 d . . . H4A H -0.0695 0.0185 0.3157 0.07 Uiso 1 1 calc R . . H4B H -0.0986 0.1363 0.3576 0.07 Uiso 1 1 calc R . . H4C H -0.0446 0.0289 0.3926 0.07 Uiso 1 1 calc R . . C5 C 0.1874(3) -0.0694(2) 0.47391(11) 0.0493(6) Uani 1 1 d . . . H5A H 0.2789 -0.0347 0.5056 0.074 Uiso 1 1 calc R . . H5B H 0.1431 -0.1454 0.4854 0.074 Uiso 1 1 calc R . . H5C H 0.1155 -0.0134 0.4736 0.074 Uiso 1 1 calc R . . C6 C 0.0713(3) -0.2001(2) 0.33690(14) 0.0612(8) Uani 1 1 d . . . H6A H -0.0224 -0.1732 0.3432 0.092 Uiso 1 1 calc R . . H6B H 0.0697 -0.2822 0.3467 0.092 Uiso 1 1 calc R . . H6C H 0.0816 -0.1986 0.292 0.092 Uiso 1 1 calc R . . C7 C 0.3918(3) -0.1857(2) 0.39900(16) 0.0654(9) Uani 1 1 d . . . H7A H 0.4187 -0.2027 0.3567 0.098 Uiso 1 1 calc R . . H7B H 0.3605 -0.2615 0.4141 0.098 Uiso 1 1 calc R . . H7C H 0.4788 -0.1392 0.4298 0.098 Uiso 1 1 calc R . . Ge1 Ge 0.48462(2) 0.065174(16) 0.351457(9) 0.01943(6) Uani 1 1 d . . . O11 O 0.48775(13) 0.22550(10) 0.33923(6) 0.0209(3) Uani 1 1 d . . . C12 C 0.58243(19) 0.27202(15) 0.30243(8) 0.0190(3) Uani 1 1 d . . . C13 C 0.69894(19) 0.37002(15) 0.32773(8) 0.0196(4) Uani 1 1 d . . . C14 C 0.7880(2) 0.41179(15) 0.28519(8) 0.0212(4) Uani 1 1 d . . . H14 H 0.8676 0.4771 0.3017 0.025 Uiso 1 1 calc R . . C15 C 0.7665(2) 0.36309(15) 0.22016(8) 0.0219(4) Uani 1 1 d . . . C16 C 0.6502(2) 0.26720(15) 0.19729(8) 0.0219(4) Uani 1 1 d . . . H16 H 0.6324 0.2319 0.1533 0.026 Uiso 1 1 calc R . . C17 C 0.55890(19) 0.22143(15) 0.23725(8) 0.0198(4) Uani 1 1 d . . . C18 C 0.7260(2) 0.43086(16) 0.39841(8) 0.0242(4) Uani 1 1 d . . . C19 C 0.8578(2) 0.53619(18) 0.41426(10) 0.0356(5) Uani 1 1 d . . . H19A H 0.949 0.5072 0.4059 0.053 Uiso 1 1 calc R . . H19B H 0.8727 0.571 0.4598 0.053 Uiso 1 1 calc R . . H19C H 0.8356 0.5976 0.3872 0.053 Uiso 1 1 calc R . . C20 C 0.5849(2) 0.48071(17) 0.41141(10) 0.0318(4) Uani 1 1 d . . . H20A H 0.5669 0.5437 0.3849 0.048 Uiso 1 1 calc R . . H20B H 0.5999 0.5144 0.4571 0.048 Uiso 1 1 calc R . . H20C H 0.4983 0.4157 0.4005 0.048 Uiso 1 1 calc R . . C21 C 0.7639(2) 0.34114(18) 0.44460(9) 0.0344(5) Uani 1 1 d . . . H21A H 0.6802 0.2741 0.4373 0.052 Uiso 1 1 calc R . . H21B H 0.7811 0.3814 0.4893 0.052 Uiso 1 1 calc R . . H21C H 0.8546 0.3107 0.4367 0.052 Uiso 1 1 calc R . . C22 C 0.8623(2) 0.41329(16) 0.17382(9) 0.0251(4) Uani 1 1 d . . . C23 C 0.9318(2) 0.31247(18) 0.14132(9) 0.0296(4) Uani 1 1 d . . . H23A H 0.9872 0.3438 0.1099 0.044 Uiso 1 1 calc R . . H23B H 0.852 0.2464 0.1192 0.044 Uiso 1 1 calc R . . H23C H 1.0004 0.283 0.1742 0.044 Uiso 1 1 calc R . . C24 C 0.9871(3) 0.51513(19) 0.20843(11) 0.0416(5) Uani 1 1 d . . . H24A H 0.9435 0.5797 0.2291 0.062 Uiso 1 1 calc R . . H24B H 1.0431 0.5462 0.1772 0.062 Uiso 1 1 calc R . . H24C H 1.0549 0.4851 0.2413 0.062 Uiso 1 1 calc R . . C25 C 0.7612(2) 0.4617(2) 0.12095(10) 0.0364(5) Uani 1 1 d . . . H25A H 0.7092 0.5212 0.141 0.055 Uiso 1 1 calc R . . H25B H 0.6872 0.3953 0.0948 0.055 Uiso 1 1 calc R . . H25C H 0.8226 0.4995 0.0933 0.055 Uiso 1 1 calc R . . C26 C 0.4301(2) 0.11973(15) 0.21025(8) 0.0207(4) Uani 1 1 d . . . H26A H 0.3356 0.1463 0.2174 0.025 Uiso 1 1 calc R . . H26B H 0.4231 0.1005 0.1631 0.025 Uiso 1 1 calc R . . N31 N 0.44583(15) 0.00879(12) 0.23987(7) 0.0188(3) Uani 1 1 d . . . C32 C 0.30495(19) -0.08059(16) 0.21989(9) 0.0230(4) Uani 1 1 d . . . H32A H 0.2292 -0.0502 0.2424 0.028 Uiso 1 1 calc R . . H32B H 0.325 -0.1556 0.2363 0.028 Uiso 1 1 calc R . . C33 C 0.2340(2) -0.11353(17) 0.14899(9) 0.0267(4) Uani 1 1 d . . . H33A H 0.1331 -0.1614 0.1447 0.032 Uiso 1 1 calc R . . H33B H 0.2214 -0.039 0.1306 0.032 Uiso 1 1 calc R . . O34 O 0.31914(15) -0.18003(13) 0.11276(6) 0.0318(3) Uani 1 1 d . . . C35 C 0.2364(2) -0.2255(2) 0.04798(9) 0.0345(5) Uani 1 1 d . . . H35A H 0.2985 -0.2043 0.0162 0.041 Uiso 1 1 calc R . . H35B H 0.1445 -0.1892 0.0395 0.041 Uiso 1 1 calc R . . C36 C 0.1955(2) -0.3593(2) 0.04150(10) 0.0353(5) Uani 1 1 d . . . H36A H 0.1417 -0.3819 0.0758 0.042 Uiso 1 1 calc R . . H36B H 0.1306 -0.3924 -0.001 0.042 Uiso 1 1 calc R . . O37 O 0.33503(15) -0.40360(12) 0.04779(6) 0.0317(3) Uani 1 1 d . . . C38 C 0.3288(3) -0.52868(19) 0.05236(11) 0.0424(5) Uani 1 1 d . . . H38A H 0.4153 -0.5572 0.0373 0.051 Uiso 1 1 calc R . . H38B H 0.2359 -0.575 0.0242 0.051 Uiso 1 1 calc R . . C39 C 0.3316(2) -0.54973(19) 0.12085(11) 0.0403(5) Uani 1 1 d . . . H39A H 0.2338 -0.5423 0.1329 0.048 Uiso 1 1 calc R . . H39B H 0.3539 -0.6309 0.1264 0.048 Uiso 1 1 calc R . . O40 O 0.44705(14) -0.45969(11) 0.15951(6) 0.0295(3) Uani 1 1 d . . . C41 C 0.4603(2) -0.45649(17) 0.22728(10) 0.0305(4) Uani 1 1 d . . . H41A H 0.4922 -0.5307 0.2407 0.037 Uiso 1 1 calc R . . H41B H 0.3633 -0.4485 0.2401 0.037 Uiso 1 1 calc R . . C42 C 0.5762(2) -0.34924(16) 0.25731(9) 0.0284(4) Uani 1 1 d . . . H42A H 0.5838 -0.3354 0.3047 0.034 Uiso 1 1 calc R . . H42B H 0.6754 -0.3614 0.2482 0.034 Uiso 1 1 calc R . . O43 O 0.52926(13) -0.24907(10) 0.22950(6) 0.0237(3) Uani 1 1 d . . . C44 C 0.6293(2) -0.13883(16) 0.25645(9) 0.0245(4) Uani 1 1 d . . . H44A H 0.7324 -0.1476 0.2514 0.029 Uiso 1 1 calc R . . H44B H 0.6296 -0.1209 0.3031 0.029 Uiso 1 1 calc R . . C45 C 0.58198(19) -0.03634(15) 0.22335(9) 0.0222(4) Uani 1 1 d . . . H45A H 0.6668 0.0315 0.234 0.027 Uiso 1 1 calc R . . H45B H 0.5631 -0.0624 0.1761 0.027 Uiso 1 1 calc R . . S1 S 0.79236(5) -0.18318(4) 0.09523(3) 0.03160(12) Uani 1 1 d . . . Li51 Li 0.4725(3) -0.2963(3) 0.12970(15) 0.0259(7) Uani 1 1 d . . . O52 O 0.64854(16) -0.24678(13) 0.09935(8) 0.0427(4) Uani 1 1 d . . . O53 O 0.86726(18) -0.10448(17) 0.15277(9) 0.0609(5) Uani 1 1 d . . . C55 C 0.7423(4) -0.0829(3) 0.03833(18) 0.0737(10) Uani 1 1 d . . . F56 F 0.6690(3) -0.1434(3) -0.01778(10) 0.1297(10) Uani 1 1 d . . . F57 F 0.8655(3) -0.01424(19) 0.02973(14) 0.1365(11) Uani 1 1 d . . . F58 F 0.6553(2) -0.00843(17) 0.06035(10) 0.0973(7) Uani 1 1 d . . . O54 O 0.88331(16) -0.25484(13) 0.06405(8) 0.0413(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Si1 0.0240(3) 0.0279(3) 0.0255(3) 0.0007(2) 0.0060(2) 0.0064(2) Si2 0.0382(3) 0.0232(3) 0.0422(3) 0.0098(2) 0.0205(3) 0.0022(2) N1 0.0220(8) 0.0208(7) 0.0231(8) 0.0024(6) 0.0075(6) 0.0006(6) C2 0.0486(14) 0.0590(15) 0.0465(14) 0.0226(12) 0.0160(11) 0.0340(12) C3 0.0469(13) 0.0364(12) 0.0412(13) -0.0083(10) 0.0122(10) 0.0086(10) C4 0.0270(11) 0.0534(15) 0.0570(15) -0.0001(12) 0.0076(10) 0.0076(10) C5 0.0621(16) 0.0514(14) 0.0443(14) 0.0239(12) 0.0243(12) 0.0109(13) C6 0.0756(19) 0.0354(13) 0.0659(18) -0.0031(12) 0.0287(15) -0.0225(13) C7 0.0713(19) 0.0397(14) 0.111(2) 0.0440(15) 0.0508(18) 0.0264(14) Ge1 0.01997(10) 0.01854(10) 0.01931(10) 0.00313(7) 0.00365(7) 0.00174(7) O11 0.0256(6) 0.0170(6) 0.0200(6) 0.0014(5) 0.0091(5) -0.0011(5) C12 0.0243(9) 0.0162(8) 0.0179(8) 0.0038(7) 0.0065(7) 0.0038(7) C13 0.0253(9) 0.0160(8) 0.0180(8) 0.0020(7) 0.0056(7) 0.0033(7) C14 0.0225(9) 0.0167(8) 0.0228(9) 0.0017(7) 0.0045(7) -0.0005(7) C15 0.0265(9) 0.0203(9) 0.0217(9) 0.0057(7) 0.0089(7) 0.0063(7) C16 0.0297(10) 0.0207(9) 0.0154(8) 0.0005(7) 0.0049(7) 0.0054(8) C17 0.0238(9) 0.0166(8) 0.0188(9) 0.0021(7) 0.0041(7) 0.0037(7) C18 0.0309(10) 0.0213(9) 0.0179(9) -0.0013(7) 0.0067(7) -0.0028(8) C19 0.0424(12) 0.0338(11) 0.0230(10) -0.0073(8) 0.0092(9) -0.0126(9) C20 0.0429(12) 0.0242(10) 0.0283(10) -0.0031(8) 0.0154(9) 0.0015(9) C21 0.0454(13) 0.0343(11) 0.0193(10) 0.0030(8) 0.0015(9) -0.0008(10) C22 0.0301(10) 0.0252(9) 0.0232(9) 0.0045(8) 0.0128(8) 0.0052(8) C23 0.0323(11) 0.0332(11) 0.0278(10) 0.0063(8) 0.0127(8) 0.0107(9) C24 0.0482(13) 0.0358(12) 0.0418(13) 0.0011(10) 0.0271(11) -0.0083(10) C25 0.0479(13) 0.0417(12) 0.0333(11) 0.0196(10) 0.0235(10) 0.0220(10) C26 0.0239(9) 0.0192(9) 0.0179(8) 0.0007(7) 0.0026(7) 0.0035(7) N31 0.0174(7) 0.0147(7) 0.0230(8) 0.0001(6) 0.0038(6) 0.0006(6) C32 0.0172(9) 0.0210(9) 0.0284(10) -0.0038(7) 0.0066(7) -0.0006(7) C33 0.0182(9) 0.0249(10) 0.0322(10) -0.0066(8) 0.0004(7) 0.0030(7) O34 0.0290(7) 0.0454(8) 0.0204(7) -0.0043(6) 0.0007(5) 0.0174(6) C35 0.0331(11) 0.0502(13) 0.0204(10) 0.0009(9) 0.0021(8) 0.0154(10) C36 0.0231(10) 0.0571(14) 0.0212(10) -0.0019(9) 0.0014(8) 0.0021(9) O37 0.0267(7) 0.0330(8) 0.0309(8) -0.0031(6) 0.0031(6) 0.0002(6) C38 0.0418(13) 0.0320(12) 0.0441(13) -0.0118(10) 0.0024(10) -0.0022(10) C39 0.0360(12) 0.0253(11) 0.0529(14) -0.0032(10) 0.0059(10) -0.0065(9) O40 0.0281(7) 0.0239(7) 0.0331(8) 0.0003(6) 0.0050(6) -0.0018(6) C41 0.0322(11) 0.0253(10) 0.0385(11) 0.0113(9) 0.0111(9) 0.0087(8) C42 0.0323(10) 0.0256(10) 0.0299(10) 0.0092(8) 0.0045(8) 0.0116(8) O43 0.0235(6) 0.0179(6) 0.0282(7) 0.0048(5) 0.0007(5) 0.0034(5) C44 0.0205(9) 0.0232(9) 0.0271(10) -0.0018(8) 0.0015(7) 0.0036(7) C45 0.0174(8) 0.0186(9) 0.0290(10) -0.0003(7) 0.0047(7) 0.0003(7) S1 0.0245(2) 0.0289(3) 0.0417(3) 0.0002(2) 0.0148(2) -0.0003(2) Li51 0.0207(15) 0.0245(16) 0.0302(17) 0.0022(13) 0.0042(13) -0.0008(13) O52 0.0258(8) 0.0379(8) 0.0670(11) 0.0086(8) 0.0205(7) -0.0004(6) O53 0.0389(9) 0.0722(12) 0.0598(11) -0.0295(10) 0.0140(8) -0.0016(9) C55 0.098(2) 0.0649(19) 0.087(2) 0.0384(18) 0.058(2) 0.0363(18) F56 0.188(3) 0.177(2) 0.0519(13) 0.0400(14) 0.0236(14) 0.102(2) F57 0.172(2) 0.0876(15) 0.212(3) 0.0887(17) 0.144(2) 0.0373(16) F58 0.1302(17) 0.0779(12) 0.1263(17) 0.0574(12) 0.0697(14) 0.0676(12) O54 0.0284(8) 0.0371(8) 0.0552(10) -0.0106(7) 0.0163(7) -0.0001(6) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Si1 N1 1.7526(15) . ? Si1 C3 1.862(2) . ? Si1 C2 1.870(2) . ? Si1 C4 1.873(2) . ? Si2 N1 1.7467(15) . ? Si2 C5 1.869(2) . ? Si2 C7 1.873(2) . ? Si2 C6 1.879(3) . ? N1 Ge1 1.9016(14) . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? Ge1 O11 1.8712(11) . ? Ge1 N31 2.3350(14) . ? O11 C12 1.365(2) . ? C12 C17 1.403(2) . ? C12 C13 1.411(2) . ? C13 C14 1.405(2) . ? C13 C18 1.540(2) . ? C14 C15 1.396(2) . ? C14 H14 0.95 . ? C15 C16 1.388(3) . ? C15 C22 1.543(2) . ? C16 C17 1.392(2) . ? C16 H16 0.95 . ? C17 C26 1.510(2) . ? C18 C21 1.535(3) . ? C18 C19 1.537(3) . ? C18 C20 1.542(3) . ? C19 H19A 0.98 . ? C19 H19B 0.98 . ? C19 H19C 0.98 . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 C24 1.522(3) . ? C22 C25 1.538(3) . ? C22 C23 1.540(2) . ? C23 H23A 0.98 . ? C23 H23B 0.98 . ? C23 H23C 0.98 . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 N31 1.492(2) . ? C26 H26A 0.99 . ? C26 H26B 0.99 . ? N31 C32 1.489(2) . ? N31 C45 1.499(2) . ? C32 C33 1.514(3) . ? C32 H32A 0.99 . ? C32 H32B 0.99 . ? C33 O34 1.421(2) . ? C33 H33A 0.99 . ? C33 H33B 0.99 . ? O34 C35 1.447(2) . ? O34 Li51 2.081(3) . ? C35 C36 1.499(3) . ? C35 H35A 0.99 . ? C35 H35B 0.99 . ? C36 O37 1.434(2) . ? C36 H36A 0.99 . ? C36 H36B 0.99 . ? O37 C38 1.432(3) . ? O37 Li51 2.096(3) . ? C38 C39 1.504(3) . ? C38 H38A 0.99 . ? C38 H38B 0.99 . ? C39 O40 1.425(2) . ? C39 H39A 0.99 . ? C39 H39B 0.99 . ? O40 C41 1.423(2) . ? O40 Li51 2.033(3) . ? C41 C42 1.495(3) . ? C41 H41A 0.99 . ? C41 H41B 0.99 . ? C42 O43 1.432(2) . ? C42 H42A 0.99 . ? C42 H42B 0.99 . ? O43 C44 1.435(2) . ? O43 Li51 2.081(3) . ? C44 C45 1.511(2) . ? C44 H44A 0.99 . ? C44 H44B 0.99 . ? C45 H45A 0.99 . ? C45 H45B 0.99 . ? S1 O53 1.4271(17) . ? S1 O54 1.4360(14) . ? S1 O52 1.4367(14) . ? S1 C55 1.810(3) . ? Li51 O52 1.885(3) . ? C55 F56 1.319(4) . ? C55 F57 1.336(4) . ? C55 F58 1.343(3) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N1 Si1 C3 110.38(9) . . ? N1 Si1 C2 115.29(8) . . ? C3 Si1 C2 108.51(11) . . ? N1 Si1 C4 111.60(9) . . ? C3 Si1 C4 108.51(11) . . ? C2 Si1 C4 102.10(11) . . ? N1 Si2 C5 112.05(9) . . ? N1 Si2 C7 111.13(9) . . ? C5 Si2 C7 107.27(13) . . ? N1 Si2 C6 112.23(10) . . ? C5 Si2 C6 108.55(12) . . ? C7 Si2 C6 105.26(14) . . ? Si2 N1 Si1 119.19(8) . . ? Si2 N1 Ge1 113.97(8) . . ? Si1 N1 Ge1 124.89(8) . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? O11 Ge1 N1 96.23(6) . . ? O11 Ge1 N31 89.49(5) . . ? N1 Ge1 N31 99.04(6) . . ? C12 O11 Ge1 118.11(10) . . ? O11 C12 C17 118.05(15) . . ? O11 C12 C13 121.94(15) . . ? C17 C12 C13 119.99(15) . . ? C14 C13 C12 117.07(15) . . ? C14 C13 C18 121.10(15) . . ? C12 C13 C18 121.82(15) . . ? C15 C14 C13 123.96(16) . . ? C15 C14 H14 118 . . ? C13 C14 H14 118 . . ? C16 C15 C14 117.00(16) . . ? C16 C15 C22 119.97(16) . . ? C14 C15 C22 123.01(16) . . ? C15 C16 C17 121.62(16) . . ? C15 C16 H16 119.2 . . ? C17 C16 H16 119.2 . . ? C16 C17 C12 120.36(16) . . ? C16 C17 C26 120.22(15) . . ? C12 C17 C26 119.38(15) . . ? C21 C18 C19 106.93(16) . . ? C21 C18 C13 110.60(14) . . ? C19 C18 C13 112.14(15) . . ? C21 C18 C20 109.74(15) . . ? C19 C18 C20 107.68(16) . . ? C13 C18 C20 109.67(15) . . ? C18 C19 H19A 109.5 . . ? C18 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C18 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C18 C20 H20A 109.5 . . ? C18 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C18 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C18 C21 H21A 109.5 . . ? C18 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C18 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C24 C22 C25 108.31(17) . . ? C24 C22 C23 109.12(16) . . ? C25 C22 C23 108.35(15) . . ? C24 C22 C15 112.02(15) . . ? C25 C22 C15 109.00(15) . . ? C23 C22 C15 109.96(15) . . ? C22 C23 H23A 109.5 . . ? C22 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C22 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C22 C24 H24A 109.5 . . ? C22 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C22 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C22 C25 H25A 109.5 . . ? C22 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C22 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? N31 C26 C17 113.14(13) . . ? N31 C26 H26A 109 . . ? C17 C26 H26A 109 . . ? N31 C26 H26B 109 . . ? C17 C26 H26B 109 . . ? H26A C26 H26B 107.8 . . ? C32 N31 C26 110.69(13) . . ? C32 N31 C45 114.30(13) . . ? C26 N31 C45 108.15(13) . . ? C32 N31 Ge1 107.69(10) . . ? C26 N31 Ge1 106.83(10) . . ? C45 N31 Ge1 108.91(10) . . ? N31 C32 C33 119.29(15) . . ? N31 C32 H32A 107.5 . . ? C33 C32 H32A 107.5 . . ? N31 C32 H32B 107.5 . . ? C33 C32 H32B 107.5 . . ? H32A C32 H32B 107 . . ? O34 C33 C32 113.45(14) . . ? O34 C33 H33A 108.9 . . ? C32 C33 H33A 108.9 . . ? O34 C33 H33B 108.9 . . ? C32 C33 H33B 108.9 . . ? H33A C33 H33B 107.7 . . ? C33 O34 C35 111.32(13) . . ? C33 O34 Li51 137.33(14) . . ? C35 O34 Li51 104.09(14) . . ? O34 C35 C36 108.72(16) . . ? O34 C35 H35A 109.9 . . ? C36 C35 H35A 109.9 . . ? O34 C35 H35B 109.9 . . ? C36 C35 H35B 109.9 . . ? H35A C35 H35B 108.3 . . ? O37 C36 C35 105.46(16) . . ? O37 C36 H36A 110.6 . . ? C35 C36 H36A 110.6 . . ? O37 C36 H36B 110.6 . . ? C35 C36 H36B 110.6 . . ? H36A C36 H36B 108.8 . . ? C38 O37 C36 116.60(16) . . ? C38 O37 Li51 111.30(14) . . ? C36 O37 Li51 104.83(14) . . ? O37 C38 C39 110.55(17) . . ? O37 C38 H38A 109.5 . . ? C39 C38 H38A 109.5 . . ? O37 C38 H38B 109.5 . . ? C39 C38 H38B 109.5 . . ? H38A C38 H38B 108.1 . . ? O40 C39 C38 105.72(17) . . ? O40 C39 H39A 110.6 . . ? C38 C39 H39A 110.6 . . ? O40 C39 H39B 110.6 . . ? C38 C39 H39B 110.6 . . ? H39A C39 H39B 108.7 . . ? C41 O40 C39 115.08(15) . . ? C41 O40 Li51 115.06(14) . . ? C39 O40 Li51 116.53(15) . . ? O40 C41 C42 105.46(15) . . ? O40 C41 H41A 110.6 . . ? C42 C41 H41A 110.6 . . ? O40 C41 H41B 110.6 . . ? C42 C41 H41B 110.6 . . ? H41A C41 H41B 108.8 . . ? O43 C42 C41 106.68(15) . . ? O43 C42 H42A 110.4 . . ? C41 C42 H42A 110.4 . . ? O43 C42 H42B 110.4 . . ? C41 C42 H42B 110.4 . . ? H42A C42 H42B 108.6 . . ? C42 O43 C44 112.06(13) . . ? C42 O43 Li51 108.90(13) . . ? C44 O43 Li51 119.03(13) . . ? O43 C44 C45 110.76(14) . . ? O43 C44 H44A 109.5 . . ? C45 C44 H44A 109.5 . . ? O43 C44 H44B 109.5 . . ? C45 C44 H44B 109.5 . . ? H44A C44 H44B 108.1 . . ? N31 C45 C44 116.18(14) . . ? N31 C45 H45A 108.2 . . ? C44 C45 H45A 108.2 . . ? N31 C45 H45B 108.2 . . ? C44 C45 H45B 108.2 . . ? H45A C45 H45B 107.4 . . ? O53 S1 O54 116.08(10) . . ? O53 S1 O52 114.10(10) . . ? O54 S1 O52 114.59(9) . . ? O53 S1 C55 103.99(15) . . ? O54 S1 C55 103.40(12) . . ? O52 S1 C55 102.28(13) . . ? O52 Li51 O40 117.83(16) . . ? O52 Li51 O43 105.45(15) . . ? O40 Li51 O43 78.32(12) . . ? O52 Li51 O34 111.25(16) . . ? O40 Li51 O34 130.15(16) . . ? O43 Li51 O34 97.17(14) . . ? O52 Li51 O37 102.34(16) . . ? O40 Li51 O37 78.46(12) . . ? O43 Li51 O37 149.81(17) . . ? O34 Li51 O37 83.41(12) . . ? S1 O52 Li51 161.68(15) . . ? F56 C55 F57 109.2(3) . . ? F56 C55 F58 108.2(3) . . ? F57 C55 F58 107.0(3) . . ? F56 C55 S1 111.1(2) . . ? F57 C55 S1 110.1(3) . . ? F58 C55 S1 111.2(2) . . ? 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 C5 Si2 N1 Si1 -50.06(14) . . . . ? C7 Si2 N1 Si1 -170.05(13) . . . . ? C6 Si2 N1 Si1 72.38(14) . . . . ? C5 Si2 N1 Ge1 114.82(11) . . . . ? C7 Si2 N1 Ge1 -5.17(15) . . . . ? C6 Si2 N1 Ge1 -122.74(12) . . . . ? C3 Si1 N1 Si2 91.20(12) . . . . ? C2 Si1 N1 Si2 -145.43(12) . . . . ? C4 Si1 N1 Si2 -29.55(14) . . . . ? C3 Si1 N1 Ge1 -71.90(13) . . . . ? C2 Si1 N1 Ge1 51.47(14) . . . . ? C4 Si1 N1 Ge1 167.34(11) . . . . ? Si2 N1 Ge1 O11 -167.36(8) . . . . ? Si1 N1 Ge1 O11 -3.48(10) . . . . ? Si2 N1 Ge1 N31 102.16(8) . . . . ? Si1 N1 Ge1 N31 -93.96(10) . . . . ? N1 Ge1 O11 C12 -151.46(12) . . . . ? N31 Ge1 O11 C12 -52.42(12) . . . . ? Ge1 O11 C12 C17 62.94(17) . . . . ? Ge1 O11 C12 C13 -118.63(14) . . . . ? O11 C12 C13 C14 -178.96(15) . . . . ? C17 C12 C13 C14 -0.6(2) . . . . ? O11 C12 C13 C18 -0.3(2) . . . . ? C17 C12 C13 C18 178.15(15) . . . . ? C12 C13 C14 C15 0.7(2) . . . . ? C18 C13 C14 C15 -177.98(15) . . . . ? C13 C14 C15 C16 -0.4(3) . . . . ? C13 C14 C15 C22 177.84(16) . . . . ? C14 C15 C16 C17 0.0(2) . . . . ? C22 C15 C16 C17 -178.37(15) . . . . ? C15 C16 C17 C12 0.2(3) . . . . ? C15 C16 C17 C26 177.94(15) . . . . ? O11 C12 C17 C16 178.60(15) . . . . ? C13 C12 C17 C16 0.1(2) . . . . ? O11 C12 C17 C26 0.8(2) . . . . ? C13 C12 C17 C26 -177.66(15) . . . . ? C14 C13 C18 C21 -119.89(18) . . . . ? C12 C13 C18 C21 61.5(2) . . . . ? C14 C13 C18 C19 -0.6(2) . . . . ? C12 C13 C18 C19 -179.29(16) . . . . ? C14 C13 C18 C20 118.94(18) . . . . ? C12 C13 C18 C20 -59.7(2) . . . . ? C16 C15 C22 C24 -178.06(17) . . . . ? C14 C15 C22 C24 3.7(2) . . . . ? C16 C15 C22 C25 62.1(2) . . . . ? C14 C15 C22 C25 -116.14(19) . . . . ? C16 C15 C22 C23 -56.5(2) . . . . ? C14 C15 C22 C23 125.22(18) . . . . ? C16 C17 C26 N31 117.68(17) . . . . ? C12 C17 C26 N31 -64.5(2) . . . . ? C17 C26 N31 C32 170.33(14) . . . . ? C17 C26 N31 C45 -63.74(18) . . . . ? C17 C26 N31 Ge1 53.35(15) . . . . ? O11 Ge1 N31 C32 -122.98(10) . . . . ? N1 Ge1 N31 C32 -26.75(11) . . . . ? O11 Ge1 N31 C26 -4.04(10) . . . . ? N1 Ge1 N31 C26 92.19(11) . . . . ? O11 Ge1 N31 C45 112.56(10) . . . . ? N1 Ge1 N31 C45 -151.22(10) . . . . ? C26 N31 C32 C33 50.72(19) . . . . ? C45 N31 C32 C33 -71.68(19) . . . . ? Ge1 N31 C32 C33 167.17(12) . . . . ? N31 C32 C33 O34 69.0(2) . . . . ? C32 C33 O34 C35 170.92(16) . . . . ? C32 C33 O34 Li51 26.9(3) . . . . ? C33 O34 C35 C36 -110.44(17) . . . . ? Li51 O34 C35 C36 45.31(19) . . . . ? O34 C35 C36 O37 -65.56(19) . . . . ? C35 C36 O37 C38 171.56(16) . . . . ? C35 C36 O37 Li51 47.99(18) . . . . ? C36 O37 C38 C39 -84.2(2) . . . . ? Li51 O37 C38 C39 35.9(2) . . . . ? O37 C38 C39 O40 -45.5(2) . . . . ? C38 C39 O40 C41 174.69(16) . . . . ? C38 C39 O40 Li51 35.5(2) . . . . ? C39 O40 C41 C42 -174.61(15) . . . . ? Li51 O40 C41 C42 -34.87(19) . . . . ? O40 C41 C42 O43 53.63(18) . . . . ? C41 C42 O43 C44 177.77(15) . . . . ? C41 C42 O43 Li51 -48.43(18) . . . . ? C42 O43 C44 C45 176.58(14) . . . . ? Li51 O43 C44 C45 47.93(19) . . . . ? C32 N31 C45 C44 -64.20(19) . . . . ? C26 N31 C45 C44 172.02(14) . . . . ? Ge1 N31 C45 C44 56.27(16) . . . . ? O43 C44 C45 N31 73.75(19) . . . . ? C41 O40 Li51 O52 109.00(19) . . . . ? C39 O40 Li51 O52 -111.9(2) . . . . ? C41 O40 Li51 O43 7.55(16) . . . . ? C39 O40 Li51 O43 146.69(15) . . . . ? C41 O40 Li51 O34 -82.0(2) . . . . ? C39 O40 Li51 O34 57.1(3) . . . . ? C41 O40 Li51 O37 -153.02(13) . . . . ? C39 O40 Li51 O37 -13.88(17) . . . . ? C42 O43 Li51 O52 -92.73(17) . . . . ? C44 O43 Li51 O52 37.4(2) . . . . ? C42 O43 Li51 O40 23.21(14) . . . . ? C44 O43 Li51 O40 153.30(12) . . . . ? C42 O43 Li51 O34 152.83(13) . . . . ? C44 O43 Li51 O34 -77.08(16) . . . . ? C42 O43 Li51 O37 63.6(4) . . . . ? C44 O43 Li51 O37 -166.3(3) . . . . ? C33 O34 Li51 O52 -127.9(2) . . . . ? C35 O34 Li51 O52 86.47(19) . . . . ? C33 O34 Li51 O40 62.5(3) . . . . ? C35 O34 Li51 O40 -83.1(2) . . . . ? C33 O34 Li51 O43 -18.2(3) . . . . ? C35 O34 Li51 O43 -163.84(14) . . . . ? C33 O34 Li51 O37 131.39(19) . . . . ? C35 O34 Li51 O37 -14.25(15) . . . . ? C38 O37 Li51 O52 103.41(17) . . . . ? C36 O37 Li51 O52 -129.69(15) . . . . ? C38 O37 Li51 O40 -12.89(16) . . . . ? C36 O37 Li51 O40 114.01(14) . . . . ? C38 O37 Li51 O43 -53.3(4) . . . . ? C36 O37 Li51 O43 73.6(3) . . . . ? C38 O37 Li51 O34 -146.21(14) . . . . ? C36 O37 Li51 O34 -19.31(15) . . . . ? O53 S1 O52 Li51 8.6(5) . . . . ? O54 S1 O52 Li51 145.9(4) . . . . ? C55 S1 O52 Li51 -103.0(5) . . . . ? O40 Li51 O52 S1 -109.5(4) . . . . ? O43 Li51 O52 S1 -24.8(5) . . . . ? O34 Li51 O52 S1 79.5(5) . . . . ? O37 Li51 O52 S1 167.1(4) . . . . ? O53 S1 C55 F56 -179.0(2) . . . . ? O54 S1 C55 F56 59.3(2) . . . . ? O52 S1 C55 F56 -60.0(2) . . . . ? O53 S1 C55 F57 59.9(2) . . . . ? O54 S1 C55 F57 -61.8(3) . . . . ? O52 S1 C55 F57 178.9(2) . . . . ? O53 S1 C55 F58 -58.5(3) . . . . ? O54 S1 C55 F58 179.9(2) . . . . ? O52 S1 C55 F58 60.5(3) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 942094' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_job _audit_creation_date 2011-10-14T15:55:00-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C26 H43 B0 F3 Li N O8 S' _chemical_formula_sum 'C26 H43 B0 F3 Li N O8 S' _chemical_formula_weight 593.61 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 9.4732(13) _cell_length_b 27.781(4) _cell_length_c 12.5458(14) _cell_angle_alpha 90 _cell_angle_beta 109.382(6) _cell_angle_gamma 90 _cell_volume 3114.6(7) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6251 _cell_measurement_theta_min 2.28 _cell_measurement_theta_max 26.95 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.58 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.21 _exptl_crystal_density_diffrn 1.266 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.166 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.835 _exptl_absorpt_correction_T_max 0.966 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0 _diffrn_reflns_av_unetI/netI 0.074 _diffrn_reflns_number 7023 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 36 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.47 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.98 _diffrn_measured_fraction_theta_max 0.98 _reflns_number_total 7023 _reflns_number_gt 5291 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999))' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1067P)^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_number_reflns 7023 _refine_ls_number_parameters 382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0847 _refine_ls_R_factor_gt 0.059 _refine_ls_wR_factor_ref 0.1817 _refine_ls_wR_factor_gt 0.1599 _refine_ls_goodness_of_fit_ref 1.078 _refine_ls_restrained_S_all 1.078 _refine_ls_shift/su_max 0.048 _refine_ls_shift/su_mean 0.002 _refine_diff_density_max 0.391 _refine_diff_density_min -0.488 _refine_diff_density_rms 0.103 #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' B B 0.0013 0.0007 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Li1 Li 0.8063(6) 0.20448(17) 0.4463(4) 0.0340(11) Uani 1 1 d . . . N1 N 0.5821(3) 0.09835(7) 0.40357(19) 0.0289(5) Uani 1 1 d . . . C2 C 0.4744(3) 0.11698(10) 0.2982(3) 0.0364(7) Uani 1 1 d . . . H2A H 0.3718 0.1114 0.2997 0.044 Uiso 1 1 calc R . . H2B H 0.4853 0.0985 0.2339 0.044 Uiso 1 1 calc R . . C3 C 0.4928(3) 0.17007(11) 0.2785(3) 0.0400(7) Uani 1 1 d . . . H3A H 0.426 0.1791 0.202 0.048 Uiso 1 1 calc R . . H3B H 0.4635 0.1893 0.3343 0.048 Uiso 1 1 calc R . . O4 O 0.6455(2) 0.18086(6) 0.28872(15) 0.0326(5) Uani 1 1 d . . . C5 C 0.6534(4) 0.21550(12) 0.2065(3) 0.0448(8) Uani 1 1 d . . . H5A H 0.6043 0.2458 0.2164 0.054 Uiso 1 1 calc R . . H5B H 0.6014 0.2031 0.1294 0.054 Uiso 1 1 calc R . . C6 C 0.8152(4) 0.22449(11) 0.2224(2) 0.0434(8) Uani 1 1 d . . . H6A H 0.8663 0.194 0.2169 0.052 Uiso 1 1 calc R . . H6B H 0.825 0.247 0.164 0.052 Uiso 1 1 calc R . . O7 O 0.8787(3) 0.24504(7) 0.33243(17) 0.0382(5) Uani 1 1 d . . . C8 C 1.0381(4) 0.24899(12) 0.3670(3) 0.0456(8) Uani 1 1 d . . . H8A H 1.0719 0.2764 0.4197 0.055 Uiso 1 1 calc R . . H8B H 1.0691 0.2552 0.3002 0.055 Uiso 1 1 calc R . . C9 C 1.1089(4) 0.20380(12) 0.4235(3) 0.0450(8) Uani 1 1 d . . . H9A H 1.091 0.1772 0.3682 0.054 Uiso 1 1 calc R . . H9B H 1.2182 0.2082 0.4594 0.054 Uiso 1 1 calc R . . O10 O 1.0393(2) 0.19347(7) 0.50810(17) 0.0374(5) Uani 1 1 d . . . C11 C 1.0825(4) 0.14820(11) 0.5629(3) 0.0465(8) Uani 1 1 d . . . H11A H 1.1883 0.1491 0.6127 0.056 Uiso 1 1 calc R . . H11B H 1.0708 0.1223 0.5064 0.056 Uiso 1 1 calc R . . C12 C 0.9810(4) 0.13956(12) 0.6309(3) 0.0476(8) Uani 1 1 d . . . H12A H 0.9986 0.107 0.6651 0.057 Uiso 1 1 calc R . . H12B H 1.0005 0.1636 0.6924 0.057 Uiso 1 1 calc R . . O13 O 0.8281(2) 0.14372(7) 0.55515(16) 0.0332(5) Uani 1 1 d . . . C14 C 0.7205(4) 0.12257(10) 0.5995(2) 0.0381(7) Uani 1 1 d . . . H14A H 0.7135 0.1418 0.6639 0.046 Uiso 1 1 calc R . . H14B H 0.7516 0.0895 0.6264 0.046 Uiso 1 1 calc R . . C15 C 0.5709(4) 0.12150(10) 0.5063(3) 0.0375(7) Uani 1 1 d . . . H15A H 0.4981 0.1036 0.5325 0.045 Uiso 1 1 calc R . . H15B H 0.5335 0.1548 0.4883 0.045 Uiso 1 1 calc R . . C20 C 0.5724(3) 0.04501(9) 0.4081(2) 0.0315(6) Uani 1 1 d . . . H20A H 0.4665 0.0356 0.3912 0.038 Uiso 1 1 calc R . . H20B H 0.6288 0.0339 0.4855 0.038 Uiso 1 1 calc R . . C21 C 0.6339(3) 0.02034(9) 0.3255(2) 0.0256(6) Uani 1 1 d . . . C22 C 0.5577(3) -0.01804(9) 0.2592(2) 0.0276(6) Uani 1 1 d . A . H22 H 0.4621 -0.0269 0.262 0.033 Uiso 1 1 calc R . . C23 C 0.6178(3) -0.04364(9) 0.1890(2) 0.0277(6) Uani 1 1 d . . . C24 C 0.7597(3) -0.02956(9) 0.1879(2) 0.0269(6) Uani 1 1 d . A . H24 H 0.8035 -0.0473 0.1422 0.032 Uiso 1 1 calc R . . C25 C 0.8403(3) 0.00931(9) 0.2509(2) 0.0243(5) Uani 1 1 d . . . C26 C 0.7741(3) 0.03433(9) 0.3190(2) 0.0245(5) Uani 1 1 d . A . C27A C 0.5314(3) -0.08488(10) 0.1138(2) 0.0338(6) Uani 0.625(4) 1 d P A 1 C28A C 0.4165(8) -0.0651(2) 0.0112(5) 0.0619(17) Uani 0.625(4) 1 d P A 1 H28A H 0.3507 -0.0911 -0.0295 0.093 Uiso 0.625(4) 1 calc PR A 1 H28B H 0.466 -0.0504 -0.0381 0.093 Uiso 0.625(4) 1 calc PR A 1 H28C H 0.3571 -0.0406 0.0335 0.093 Uiso 0.625(4) 1 calc PR A 1 C29A C 0.4486(7) -0.1161(2) 0.1798(5) 0.0572(14) Uani 0.625(4) 1 d P A 1 H29A H 0.3726 -0.0964 0.1965 0.086 Uiso 0.625(4) 1 calc PR A 1 H29B H 0.5213 -0.1276 0.2507 0.086 Uiso 0.625(4) 1 calc PR A 1 H29C H 0.4003 -0.1437 0.1334 0.086 Uiso 0.625(4) 1 calc PR A 1 C30A C 0.6361(7) -0.1213(2) 0.0817(6) 0.0583(14) Uani 0.625(4) 1 d P A 1 H30A H 0.5764 -0.1481 0.0388 0.087 Uiso 0.625(4) 1 calc PR A 1 H30B H 0.7106 -0.1337 0.1507 0.087 Uiso 0.625(4) 1 calc PR A 1 H30C H 0.6871 -0.105 0.0355 0.087 Uiso 0.625(4) 1 calc PR A 1 C27B C 0.5314(3) -0.08488(10) 0.1138(2) 0.0338(6) Uani 0.375(4) 1 d P A 2 C28B C 0.5279(14) -0.0747(3) -0.0113(9) 0.0619(17) Uani 0.375(4) 1 d P A 2 H28D H 0.4626 -0.0983 -0.0627 0.093 Uiso 0.375(4) 1 calc PR A 2 H28E H 0.6294 -0.0774 -0.0149 0.093 Uiso 0.375(4) 1 calc PR A 2 H28F H 0.4896 -0.0422 -0.0338 0.093 Uiso 0.375(4) 1 calc PR A 2 C29B C 0.3651(12) -0.0862(3) 0.1041(9) 0.0572(14) Uani 0.375(4) 1 d P A 2 H29D H 0.319 -0.055 0.0772 0.086 Uiso 0.375(4) 1 calc PR A 2 H29E H 0.3567 -0.0931 0.1783 0.086 Uiso 0.375(4) 1 calc PR A 2 H29F H 0.3137 -0.1114 0.0505 0.086 Uiso 0.375(4) 1 calc PR A 2 C30B C 0.6099(13) -0.1323(3) 0.1577(10) 0.0583(14) Uani 0.375(4) 1 d P A 2 H30D H 0.5735 -0.1572 0.0997 0.087 Uiso 0.375(4) 1 calc PR A 2 H30E H 0.5886 -0.1419 0.2259 0.087 Uiso 0.375(4) 1 calc PR A 2 H30F H 0.7181 -0.1284 0.1756 0.087 Uiso 0.375(4) 1 calc PR A 2 C31 C 0.9955(3) 0.02375(10) 0.2467(2) 0.0316(6) Uani 1 1 d . A . C32 C 1.0473(4) -0.00977(12) 0.1691(3) 0.0441(8) Uani 1 1 d . . . H32A H 1.0488 -0.0431 0.195 0.066 Uiso 1 1 calc R A . H32B H 1.148 -0.0005 0.1714 0.066 Uiso 1 1 calc R . . H32C H 0.978 -0.0071 0.0915 0.066 Uiso 1 1 calc R . . C33 C 1.1116(3) 0.02041(12) 0.3656(3) 0.0419(7) Uani 1 1 d . . . H33A H 1.0887 0.0444 0.4147 0.063 Uiso 1 1 calc R A . H33B H 1.2116 0.0265 0.3616 0.063 Uiso 1 1 calc R . . H33C H 1.1086 -0.0118 0.3964 0.063 Uiso 1 1 calc R . . C34 C 0.9901(4) 0.07571(12) 0.2001(3) 0.0473(8) Uani 1 1 d . . . H34A H 0.9211 0.0768 0.1221 0.071 Uiso 1 1 calc R A . H34B H 1.0904 0.0852 0.2017 0.071 Uiso 1 1 calc R . . H34C H 0.9554 0.0979 0.247 0.071 Uiso 1 1 calc R . . O35 O 0.8470(2) 0.07279(7) 0.38230(17) 0.0318(4) Uani 1 1 d . . . H35 H 0.7862 0.0891 0.4031 0.048 Uiso 1 1 calc R A . S1 S 0.60625(8) 0.26778(2) 0.56127(6) 0.03094(19) Uani 1 1 d . . . O101 O 0.6596(2) 0.29663(8) 0.66185(18) 0.0459(6) Uani 1 1 d . . . O102 O 0.5066(3) 0.22905(7) 0.56473(19) 0.0426(5) Uani 1 1 d . . . O103 O 0.7188(3) 0.25497(9) 0.5111(2) 0.0512(6) Uani 1 1 d . . . C101 C 0.4822(4) 0.30921(12) 0.4591(3) 0.0474(8) Uani 1 1 d . . . F101 F 0.3690(3) 0.32264(8) 0.49316(19) 0.0666(6) Uani 1 1 d . . . F102 F 0.4227(3) 0.28749(9) 0.35755(17) 0.0848(8) Uani 1 1 d . . . F103 F 0.5500(3) 0.34774(8) 0.4420(2) 0.0822(8) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Li1 0.032(3) 0.037(3) 0.039(3) 0.000(2) 0.019(2) 0.000(2) N1 0.0254(12) 0.0245(11) 0.0382(12) -0.0030(9) 0.0122(10) -0.0038(9) C2 0.0192(14) 0.0342(15) 0.0506(18) -0.0008(13) 0.0044(13) -0.0003(12) C3 0.0210(15) 0.0378(15) 0.0549(18) 0.0071(14) 0.0041(14) 0.0066(12) O4 0.0253(11) 0.0344(10) 0.0356(10) 0.0112(8) 0.0070(8) 0.0009(8) C5 0.049(2) 0.0510(18) 0.0332(15) 0.0161(14) 0.0115(14) 0.0063(16) C6 0.051(2) 0.0530(19) 0.0296(15) 0.0068(13) 0.0181(14) -0.0025(16) O7 0.0464(13) 0.0373(11) 0.0416(11) -0.0059(9) 0.0289(10) -0.0074(10) C8 0.054(2) 0.0450(17) 0.0503(18) -0.0146(15) 0.0334(17) -0.0237(16) C9 0.0337(18) 0.059(2) 0.0484(18) -0.0224(15) 0.0223(15) -0.0166(15) O10 0.0343(12) 0.0383(11) 0.0409(11) -0.0098(9) 0.0142(10) -0.0066(9) C11 0.0327(19) 0.0446(18) 0.0523(19) -0.0069(15) 0.0008(15) -0.0006(14) C12 0.045(2) 0.0441(18) 0.0377(16) 0.0043(13) -0.0072(14) -0.0051(15) O13 0.0322(11) 0.0357(10) 0.0282(10) 0.0040(8) 0.0055(8) -0.0037(9) C14 0.053(2) 0.0349(15) 0.0318(15) -0.0031(12) 0.0207(14) -0.0084(14) C15 0.0391(18) 0.0334(15) 0.0501(17) -0.0069(13) 0.0284(15) -0.0033(13) C20 0.0283(15) 0.0262(13) 0.0430(16) -0.0018(11) 0.0159(13) -0.0056(11) C21 0.0201(14) 0.0255(13) 0.0301(13) 0.0013(10) 0.0067(11) -0.0008(10) C22 0.0163(13) 0.0308(13) 0.0343(14) 0.0010(11) 0.0066(11) -0.0050(10) C23 0.0251(14) 0.0260(13) 0.0285(13) 0.0010(10) 0.0043(11) -0.0029(11) C24 0.0259(15) 0.0288(13) 0.0263(13) 0.0024(10) 0.0092(11) 0.0036(10) C25 0.0171(13) 0.0291(13) 0.0256(12) 0.0052(10) 0.0059(10) 0.0004(10) C26 0.0155(13) 0.0260(12) 0.0282(13) 0.0000(10) 0.0022(10) -0.0018(10) C27A 0.0331(16) 0.0306(14) 0.0330(14) -0.0055(11) 0.0047(12) -0.0059(12) C28A 0.062(4) 0.044(3) 0.054(3) -0.010(2) -0.015(3) -0.010(3) C29A 0.060(4) 0.050(3) 0.067(4) -0.024(2) 0.029(3) -0.035(3) C30A 0.051(3) 0.048(3) 0.077(4) -0.026(3) 0.023(3) -0.012(2) C27B 0.0331(16) 0.0306(14) 0.0330(14) -0.0055(11) 0.0047(12) -0.0059(12) C28B 0.062(4) 0.044(3) 0.054(3) -0.010(2) -0.015(3) -0.010(3) C29B 0.060(4) 0.050(3) 0.067(4) -0.024(2) 0.029(3) -0.035(3) C30B 0.051(3) 0.048(3) 0.077(4) -0.026(3) 0.023(3) -0.012(2) C31 0.0214(14) 0.0378(15) 0.0369(15) 0.0010(12) 0.0113(12) -0.0039(11) C32 0.0345(18) 0.057(2) 0.0508(18) -0.0020(15) 0.0269(15) -0.0001(15) C33 0.0165(15) 0.0556(19) 0.0497(18) -0.0040(15) 0.0057(13) 0.0000(13) C34 0.0366(19) 0.0493(19) 0.058(2) 0.0121(15) 0.0178(16) -0.0117(15) O35 0.0193(10) 0.0326(10) 0.0439(11) -0.0112(8) 0.0110(9) -0.0084(8) S1 0.0251(4) 0.0378(4) 0.0347(4) -0.0032(3) 0.0162(3) 0.0035(3) O101 0.0285(12) 0.0650(15) 0.0435(12) -0.0172(10) 0.0107(10) -0.0047(10) O102 0.0437(13) 0.0364(11) 0.0561(13) -0.0091(10) 0.0280(11) -0.0028(10) O103 0.0454(14) 0.0579(14) 0.0682(15) -0.0018(12) 0.0428(12) 0.0079(12) C101 0.051(2) 0.053(2) 0.0421(18) 0.0058(15) 0.0205(16) 0.0096(17) F101 0.0547(14) 0.0781(14) 0.0691(14) 0.0176(11) 0.0235(11) 0.0378(12) F102 0.107(2) 0.0937(18) 0.0370(11) -0.0023(11) 0.0024(12) 0.0162(16) F103 0.109(2) 0.0582(14) 0.0931(18) 0.0248(13) 0.0511(17) 0.0033(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Li1 O103 1.940(5) . ? Li1 O10 2.105(5) . ? Li1 O7 2.105(5) . ? Li1 O13 2.138(5) . ? Li1 O4 2.159(5) . ? N1 C2 1.470(4) . ? N1 C15 1.476(4) . ? N1 C20 1.487(3) . ? C2 C3 1.515(4) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 O4 1.441(3) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? O4 C5 1.430(3) . ? C5 C6 1.500(5) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 O7 1.429(4) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? O7 C8 1.430(4) . ? C8 C9 1.488(5) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 O10 1.451(4) . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? O10 C11 1.426(4) . ? C11 C12 1.502(5) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 O13 1.449(4) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? O13 C14 1.439(3) . ? C14 C15 1.508(5) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C20 C21 1.510(4) . ? C20 H20A 0.99 . ? C20 H20B 0.99 . ? C21 C22 1.397(4) . ? C21 C26 1.412(3) . ? C22 C23 1.392(4) . ? C22 H22 0.95 . ? C23 C24 1.405(4) . ? C23 C27A 1.537(4) . ? C24 C25 1.405(4) . ? C24 H24 0.95 . ? C25 C26 1.401(4) . ? C25 C31 1.541(4) . ? C26 O35 1.373(3) . ? C27A C28A 1.488(6) . ? C27A C30A 1.561(6) . ? C27A C29A 1.577(6) . ? C28A H28A 0.98 . ? C28A H28B 0.98 . ? C28A H28C 0.98 . ? C29A H29A 0.98 . ? C29A H29B 0.98 . ? C29A H29C 0.98 . ? C30A H30A 0.98 . ? C30A H30B 0.98 . ? C30A H30C 0.98 . ? C28B H28D 0.98 . ? C28B H28E 0.98 . ? C28B H28F 0.98 . ? C29B H29D 0.98 . ? C29B H29E 0.98 . ? C29B H29F 0.98 . ? C30B H30D 0.98 . ? C30B H30E 0.98 . ? C30B H30F 0.98 . ? C31 C33 1.534(4) . ? C31 C32 1.541(4) . ? C31 C34 1.552(4) . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? C33 H33A 0.98 . ? C33 H33B 0.98 . ? C33 H33C 0.98 . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? O35 H35 0.84 . ? S1 O101 1.438(2) . ? S1 O102 1.441(2) . ? S1 O103 1.450(2) . ? S1 C101 1.831(3) . ? C101 F103 1.302(4) . ? C101 F101 1.333(4) . ? C101 F102 1.352(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O103 Li1 O10 119.5(3) . . ? O103 Li1 O7 100.3(2) . . ? O10 Li1 O7 77.86(18) . . ? O103 Li1 O13 105.5(2) . . ? O10 Li1 O13 77.46(19) . . ? O7 Li1 O13 150.7(3) . . ? O103 Li1 O4 109.5(3) . . ? O10 Li1 O4 128.9(2) . . ? O7 Li1 O4 80.27(18) . . ? O13 Li1 O4 103.5(2) . . ? C2 N1 C15 113.7(2) . . ? C2 N1 C20 110.6(2) . . ? C15 N1 C20 112.2(2) . . ? N1 C2 C3 114.0(2) . . ? N1 C2 H2A 108.8 . . ? C3 C2 H2A 108.8 . . ? N1 C2 H2B 108.8 . . ? C3 C2 H2B 108.8 . . ? H2A C2 H2B 107.6 . . ? O4 C3 C2 110.7(2) . . ? O4 C3 H3A 109.5 . . ? C2 C3 H3A 109.5 . . ? O4 C3 H3B 109.5 . . ? C2 C3 H3B 109.5 . . ? H3A C3 H3B 108.1 . . ? C5 O4 C3 111.5(2) . . ? C5 O4 Li1 105.4(2) . . ? C3 O4 Li1 121.8(2) . . ? O4 C5 C6 108.2(2) . . ? O4 C5 H5A 110.1 . . ? C6 C5 H5A 110.1 . . ? O4 C5 H5B 110.1 . . ? C6 C5 H5B 110.1 . . ? H5A C5 H5B 108.4 . . ? O7 C6 C5 106.2(2) . . ? O7 C6 H6A 110.5 . . ? C5 C6 H6A 110.5 . . ? O7 C6 H6B 110.5 . . ? C5 C6 H6B 110.5 . . ? H6A C6 H6B 108.7 . . ? C6 O7 C8 112.8(2) . . ? C6 O7 Li1 108.3(2) . . ? C8 O7 Li1 112.6(2) . . ? O7 C8 C9 110.1(2) . . ? O7 C8 H8A 109.6 . . ? C9 C8 H8A 109.6 . . ? O7 C8 H8B 109.6 . . ? C9 C8 H8B 109.6 . . ? H8A C8 H8B 108.2 . . ? O10 C9 C8 105.9(2) . . ? O10 C9 H9A 110.6 . . ? C8 C9 H9A 110.6 . . ? O10 C9 H9B 110.6 . . ? C8 C9 H9B 110.6 . . ? H9A C9 H9B 108.7 . . ? C11 O10 C9 113.5(2) . . ? C11 O10 Li1 113.8(2) . . ? C9 O10 Li1 112.1(2) . . ? O10 C11 C12 106.2(3) . . ? O10 C11 H11A 110.5 . . ? C12 C11 H11A 110.5 . . ? O10 C11 H11B 110.5 . . ? C12 C11 H11B 110.5 . . ? H11A C11 H11B 108.7 . . ? O13 C12 C11 107.7(3) . . ? O13 C12 H12A 110.2 . . ? C11 C12 H12A 110.2 . . ? O13 C12 H12B 110.2 . . ? C11 C12 H12B 110.2 . . ? H12A C12 H12B 108.5 . . ? C14 O13 C12 113.3(2) . . ? C14 O13 Li1 129.7(2) . . ? C12 O13 Li1 110.2(2) . . ? O13 C14 C15 108.2(2) . . ? O13 C14 H14A 110.1 . . ? C15 C14 H14A 110.1 . . ? O13 C14 H14B 110 . . ? C15 C14 H14B 110 . . ? H14A C14 H14B 108.4 . . ? N1 C15 C14 111.3(2) . . ? N1 C15 H15A 109.4 . . ? C14 C15 H15A 109.4 . . ? N1 C15 H15B 109.4 . . ? C14 C15 H15B 109.4 . . ? H15A C15 H15B 108 . . ? N1 C20 C21 112.6(2) . . ? N1 C20 H20A 109.1 . . ? C21 C20 H20A 109.1 . . ? N1 C20 H20B 109.1 . . ? C21 C20 H20B 109.1 . . ? H20A C20 H20B 107.8 . . ? C22 C21 C26 119.0(2) . . ? C22 C21 C20 121.0(2) . . ? C26 C21 C20 119.9(2) . . ? C23 C22 C21 121.9(3) . . ? C23 C22 H22 119.1 . . ? C21 C22 H22 119.1 . . ? C22 C23 C24 117.2(2) . . ? C22 C23 C27A 121.6(3) . . ? C24 C23 C27A 121.2(2) . . ? C25 C24 C23 123.5(2) . . ? C25 C24 H24 118.2 . . ? C23 C24 H24 118.2 . . ? C26 C25 C24 117.0(2) . . ? C26 C25 C31 121.1(2) . . ? C24 C25 C31 121.9(2) . . ? O35 C26 C25 119.8(2) . . ? O35 C26 C21 118.9(2) . . ? C25 C26 C21 121.3(2) . . ? C28A C27A C23 110.1(3) . . ? C28A C27A C30A 111.2(4) . . ? C23 C27A C30A 112.8(3) . . ? C28A C27A C29A 108.0(4) . . ? C23 C27A C29A 110.1(3) . . ? C30A C27A C29A 104.4(4) . . ? H28D C28B H28E 109.5 . . ? H28D C28B H28F 109.5 . . ? H28E C28B H28F 109.5 . . ? H29D C29B H29E 109.5 . . ? H29D C29B H29F 109.5 . . ? H29E C29B H29F 109.5 . . ? H30D C30B H30E 109.5 . . ? H30D C30B H30F 109.5 . . ? H30E C30B H30F 109.5 . . ? C33 C31 C32 107.6(2) . . ? C33 C31 C25 109.6(2) . . ? C32 C31 C25 111.8(2) . . ? C33 C31 C34 110.2(2) . . ? C32 C31 C34 107.5(2) . . ? C25 C31 C34 110.0(2) . . ? C31 C32 H32A 109.5 . . ? C31 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? C31 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? C31 C33 H33A 109.5 . . ? C31 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C31 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C31 C34 H34A 109.5 . . ? C31 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C31 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C26 O35 H35 109.5 . . ? O101 S1 O102 115.65(13) . . ? O101 S1 O103 114.99(14) . . ? O102 S1 O103 114.37(13) . . ? O101 S1 C101 102.78(15) . . ? O102 S1 C101 102.47(16) . . ? O103 S1 C101 104.11(15) . . ? S1 O103 Li1 146.8(2) . . ? F103 C101 F101 108.4(3) . . ? F103 C101 F102 106.6(3) . . ? F101 C101 F102 107.4(3) . . ? F103 C101 S1 113.3(3) . . ? F101 C101 S1 110.4(2) . . ? F102 C101 S1 110.4(2) . . ? 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 C15 N1 C2 C3 61.5(3) . . . . ? C20 N1 C2 C3 -171.2(2) . . . . ? N1 C2 C3 O4 51.8(3) . . . . ? C2 C3 O4 C5 141.3(3) . . . . ? C2 C3 O4 Li1 -93.1(3) . . . . ? O103 Li1 O4 C5 81.1(3) . . . . ? O10 Li1 O4 C5 -82.1(3) . . . . ? O7 Li1 O4 C5 -16.5(2) . . . . ? O13 Li1 O4 C5 -166.8(2) . . . . ? O103 Li1 O4 C3 -47.2(3) . . . . ? O10 Li1 O4 C3 149.7(3) . . . . ? O7 Li1 O4 C3 -144.7(2) . . . . ? O13 Li1 O4 C3 65.0(3) . . . . ? C3 O4 C5 C6 -179.7(2) . . . . ? Li1 O4 C5 C6 46.1(3) . . . . ? O4 C5 C6 O7 -63.4(3) . . . . ? C5 C6 O7 C8 171.1(2) . . . . ? C5 C6 O7 Li1 45.8(3) . . . . ? O103 Li1 O7 C6 -125.0(3) . . . . ? O10 Li1 O7 C6 116.8(2) . . . . ? O13 Li1 O7 C6 83.6(6) . . . . ? O4 Li1 O7 C6 -16.8(2) . . . . ? O103 Li1 O7 C8 109.6(3) . . . . ? O10 Li1 O7 C8 -8.7(2) . . . . ? O13 Li1 O7 C8 -41.8(6) . . . . ? O4 Li1 O7 C8 -142.2(2) . . . . ? C6 O7 C8 C9 -88.0(3) . . . . ? Li1 O7 C8 C9 35.0(3) . . . . ? O7 C8 C9 O10 -50.3(3) . . . . ? C8 C9 O10 C11 173.6(2) . . . . ? C8 C9 O10 Li1 42.9(3) . . . . ? O103 Li1 O10 C11 114.5(3) . . . . ? O7 Li1 O10 C11 -150.4(2) . . . . ? O13 Li1 O10 C11 13.7(2) . . . . ? O4 Li1 O10 C11 -83.7(3) . . . . ? O103 Li1 O10 C9 -114.8(3) . . . . ? O7 Li1 O10 C9 -19.8(2) . . . . ? O13 Li1 O10 C9 144.3(2) . . . . ? O4 Li1 O10 C9 46.9(3) . . . . ? C9 O10 C11 C12 -170.1(2) . . . . ? Li1 O10 C11 C12 -40.2(3) . . . . ? O10 C11 C12 O13 54.2(3) . . . . ? C11 C12 O13 C14 162.4(2) . . . . ? C11 C12 O13 Li1 -43.4(3) . . . . ? O103 Li1 O13 C14 48.3(4) . . . . ? O10 Li1 O13 C14 165.8(2) . . . . ? O7 Li1 O13 C14 -161.0(5) . . . . ? O4 Li1 O13 C14 -66.8(3) . . . . ? O103 Li1 O13 C12 -100.4(3) . . . . ? O10 Li1 O13 C12 17.1(2) . . . . ? O7 Li1 O13 C12 50.3(6) . . . . ? O4 Li1 O13 C12 144.5(2) . . . . ? C12 O13 C14 C15 -170.4(2) . . . . ? Li1 O13 C14 C15 41.7(3) . . . . ? C2 N1 C15 C14 -149.7(2) . . . . ? C20 N1 C15 C14 83.8(3) . . . . ? O13 C14 C15 N1 52.5(3) . . . . ? C2 N1 C20 C21 71.0(3) . . . . ? C15 N1 C20 C21 -160.8(2) . . . . ? N1 C20 C21 C22 -135.7(3) . . . . ? N1 C20 C21 C26 47.6(3) . . . . ? C26 C21 C22 C23 1.7(4) . . . . ? C20 C21 C22 C23 -175.0(2) . . . . ? C21 C22 C23 C24 0.4(4) . . . . ? C21 C22 C23 C27A -178.3(2) . . . . ? C22 C23 C24 C25 -1.8(4) . . . . ? C27A C23 C24 C25 176.9(2) . . . . ? C23 C24 C25 C26 1.0(4) . . . . ? C23 C24 C25 C31 -179.6(2) . . . . ? C24 C25 C26 O35 -179.8(2) . . . . ? C31 C25 C26 O35 0.8(4) . . . . ? C24 C25 C26 C21 1.3(4) . . . . ? C31 C25 C26 C21 -178.1(2) . . . . ? C22 C21 C26 O35 178.5(2) . . . . ? C20 C21 C26 O35 -4.8(4) . . . . ? C22 C21 C26 C25 -2.6(4) . . . . ? C20 C21 C26 C25 174.1(2) . . . . ? C22 C23 C27A C28A 78.7(5) . . . . ? C24 C23 C27A C28A -99.9(4) . . . . ? C22 C23 C27A C30A -156.4(4) . . . . ? C24 C23 C27A C30A 24.9(4) . . . . ? C22 C23 C27A C29A -40.3(4) . . . . ? C24 C23 C27A C29A 141.1(4) . . . . ? C26 C25 C31 C33 59.1(3) . . . . ? C24 C25 C31 C33 -120.3(3) . . . . ? C26 C25 C31 C32 178.3(2) . . . . ? C24 C25 C31 C32 -1.1(4) . . . . ? C26 C25 C31 C34 -62.3(3) . . . . ? C24 C25 C31 C34 118.3(3) . . . . ? O101 S1 O103 Li1 133.7(4) . . . . ? O102 S1 O103 Li1 -3.7(5) . . . . ? C101 S1 O103 Li1 -114.7(4) . . . . ? O10 Li1 O103 S1 -128.3(4) . . . . ? O7 Li1 O103 S1 149.9(3) . . . . ? O13 Li1 O103 S1 -44.2(5) . . . . ? O4 Li1 O103 S1 66.7(5) . . . . ? O101 S1 C101 F103 59.8(3) . . . . ? O102 S1 C101 F103 -179.9(2) . . . . ? O103 S1 C101 F103 -60.4(3) . . . . ? O101 S1 C101 F101 -62.0(3) . . . . ? O102 S1 C101 F101 58.3(3) . . . . ? O103 S1 C101 F101 177.7(2) . . . . ? O101 S1 C101 F102 179.3(2) . . . . ? O102 S1 C101 F102 -60.4(3) . . . . ? O103 S1 C101 F102 59.1(3) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 942095' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_SR44 _audit_creation_date 2012-03-26T16:19:14-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.4 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C31 H60 N2 O5 Pb Si2' _chemical_formula_sum 'C31 H60 N2 O5 Pb Si2' _chemical_formula_weight 804.18 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 12.1963(3) _cell_length_b 12.2480(4) _cell_length_c 14.3540(3) _cell_angle_alpha 66.5600(10) _cell_angle_beta 68.9620(10) _cell_angle_gamma 75.4680(10) _cell_volume 1821.43(8) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8333 _cell_measurement_theta_min 2.4 _cell_measurement_theta_max 27.38 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.19 _exptl_crystal_density_diffrn 1.466 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 820 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 4.734 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.224 _exptl_absorpt_correction_T_max 0.407 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0413 _diffrn_reflns_av_unetI/netI 0.0525 _diffrn_reflns_number 20820 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.985 _diffrn_measured_fraction_theta_max 0.985 _reflns_number_total 8228 _reflns_number_gt 7419 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 1999), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0190P)^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_number_reflns 8228 _refine_ls_number_parameters 382 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0321 _refine_ls_R_factor_gt 0.0269 _refine_ls_wR_factor_ref 0.0574 _refine_ls_wR_factor_gt 0.0558 _refine_ls_goodness_of_fit_ref 1.012 _refine_ls_restrained_S_all 1.012 _refine_ls_shift/su_max 0.007 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.6 _refine_diff_density_min -1.159 _refine_diff_density_rms 0.117 _iucr_refine_instructions_details ; .res file for SHELXL : job.res ................................................................. TITL import in P -1 CELL 0.71073 12.1963 12.2480 14.3540 66.560 68.962 75.468 ZERR 2.00 0.0003 0.0004 0.0003 0.001 0.001 0.001 LATT 1 SFAC C H N O SI PB UNIT 62 120 4 10 4 2 MERG 2 FMAP 2 PLAN 20 ACTA BOND $H CONF WPDB -2 L.S. 4 TEMP -123.00 WGHT 0.019000 FVAR 0.43135 PB1 6 0.832310 0.204024 0.792225 11.00000 0.01153 0.01657 = 0.01165 -0.00484 -0.00276 -0.00203 N1 3 0.782981 0.206336 0.655568 11.00000 0.02050 0.01655 = 0.01129 -0.00439 -0.00591 -0.00111 SI1 5 0.780767 0.072724 0.642591 11.00000 0.01903 0.01664 = 0.01513 -0.00680 -0.00536 -0.00109 C2 1 0.662705 -0.014061 0.753505 11.00000 0.02330 0.02067 = 0.02430 -0.01233 -0.00368 -0.00525 AFIX 137 H2A 2 0.684575 -0.044640 0.819601 11.00000 -1.50000 H2B 2 0.654524 -0.081466 0.737068 11.00000 -1.50000 H2C 2 0.587291 0.038550 0.761833 11.00000 -1.50000 AFIX 0 C3 1 0.928801 -0.020295 0.637682 11.00000 0.02523 0.02598 = 0.01485 -0.00902 -0.00161 0.00444 AFIX 137 H3A 2 0.989845 0.024912 0.578567 11.00000 -1.50000 H3B 2 0.927758 -0.094448 0.627413 11.00000 -1.50000 H3C 2 0.946312 -0.040056 0.704496 11.00000 -1.50000 AFIX 0 C4 1 0.745571 0.093611 0.518705 11.00000 0.03965 0.03330 = 0.02193 -0.01359 -0.01108 -0.00328 AFIX 137 H4A 2 0.665018 0.135039 0.522024 11.00000 -1.50000 H4B 2 0.751372 0.015074 0.513076 11.00000 -1.50000 H4C 2 0.801998 0.141596 0.456515 11.00000 -1.50000 AFIX 0 SI2 5 0.787520 0.342267 0.553452 11.00000 0.02472 0.01663 = 0.01259 -0.00199 -0.00364 -0.00340 C5 1 0.911753 0.343254 0.429383 11.00000 0.04409 0.03778 = 0.02163 -0.00756 0.00272 -0.01606 AFIX 137 H5A 2 0.987275 0.316782 0.446287 11.00000 -1.50000 H5B 2 0.912497 0.424717 0.377335 11.00000 -1.50000 H5C 2 0.900359 0.288777 0.399741 11.00000 -1.50000 AFIX 0 C6 1 0.644680 0.396775 0.518683 11.00000 0.04069 0.02543 = 0.03889 0.00536 -0.01846 0.00301 AFIX 137 H6A 2 0.625021 0.335762 0.501246 11.00000 -1.50000 H6B 2 0.652811 0.471206 0.457331 11.00000 -1.50000 H6C 2 0.581439 0.411890 0.579274 11.00000 -1.50000 AFIX 0 C7 1 0.812035 0.459839 0.593904 11.00000 0.07300 0.01920 = 0.02536 -0.00029 -0.01673 -0.01182 AFIX 137 H7A 2 0.750071 0.463957 0.659116 11.00000 -1.50000 H7B 2 0.809178 0.537809 0.537242 11.00000 -1.50000 H7C 2 0.889688 0.439286 0.606525 11.00000 -1.50000 AFIX 0 O11 4 0.822153 0.007798 0.871423 11.00000 0.01910 0.01634 = 0.01084 -0.00296 -0.00378 0.00106 C12 1 0.796791 -0.032926 0.977322 11.00000 0.01022 0.01411 = 0.01213 -0.00395 -0.00443 -0.00308 C13 1 0.867656 -0.133917 1.030662 11.00000 0.01199 0.01345 = 0.01517 -0.00389 -0.00517 -0.00120 C14 1 0.838032 -0.165912 1.140921 11.00000 0.01597 0.01319 = 0.01570 -0.00246 -0.00769 -0.00015 AFIX 43 H14 2 0.885197 -0.231933 1.177193 11.00000 -1.20000 AFIX 0 C15 1 0.743964 -0.107512 1.201282 11.00000 0.01579 0.01217 = 0.01129 -0.00019 -0.00417 -0.00629 C16 1 0.671387 -0.015878 1.147377 11.00000 0.01104 0.01313 = 0.01351 -0.00402 -0.00021 -0.00324 AFIX 43 H16 2 0.604023 0.023030 1.186489 11.00000 -1.20000 AFIX 0 C17 1 0.694974 0.020182 1.037703 11.00000 0.01490 0.00972 = 0.01286 -0.00121 -0.00503 -0.00219 C18 1 0.602319 0.099246 0.985044 11.00000 0.00856 0.01710 = 0.01520 -0.00449 -0.00278 -0.00232 AFIX 23 H18A 2 0.591345 0.059760 0.941315 11.00000 -1.20000 H18B 2 0.526596 0.102464 1.041437 11.00000 -1.20000 AFIX 0 C19 1 0.967570 -0.206033 0.969157 11.00000 0.01421 0.01836 = 0.01675 -0.00696 -0.00608 0.00045 C20 1 1.024747 -0.317197 1.042813 11.00000 0.01860 0.02346 = 0.02542 -0.01006 -0.00979 0.00519 AFIX 137 H20A 2 1.084882 -0.362729 1.000610 11.00000 -1.50000 H20B 2 0.963815 -0.367890 1.094947 11.00000 -1.50000 H20C 2 1.061975 -0.291803 1.079813 11.00000 -1.50000 AFIX 0 C21 1 0.916824 -0.253121 0.910486 11.00000 0.02353 0.02133 = 0.02174 -0.00973 -0.01007 0.00120 AFIX 137 H21A 2 0.874376 -0.185929 0.865867 11.00000 -1.50000 H21B 2 0.862113 -0.310827 0.962348 11.00000 -1.50000 H21C 2 0.981642 -0.292614 0.865853 11.00000 -1.50000 AFIX 0 C22 1 1.065302 -0.127285 0.891261 11.00000 0.01414 0.02589 = 0.02784 -0.01194 -0.00348 0.00114 AFIX 137 H22A 2 1.031500 -0.056150 0.842521 11.00000 -1.50000 H22B 2 1.127501 -0.173148 0.850623 11.00000 -1.50000 H22C 2 1.099207 -0.102358 0.930982 11.00000 -1.50000 AFIX 0 C23 1 0.715452 -0.151260 1.322383 11.00000 0.02369 0.01520 = 0.00981 -0.00169 -0.00496 -0.00553 C24 1 0.633133 -0.058161 1.369322 11.00000 0.06374 0.04097 = 0.01889 -0.01549 -0.01777 0.01872 AFIX 137 H24A 2 0.669039 0.016447 1.337400 11.00000 -1.50000 H24B 2 0.620153 -0.088200 1.446256 11.00000 -1.50000 H24C 2 0.557165 -0.042742 1.354554 11.00000 -1.50000 AFIX 0 C25 1 0.828103 -0.180899 1.356884 11.00000 0.03234 0.06797 = 0.01732 -0.00411 -0.01037 -0.01093 AFIX 137 H25A 2 0.882274 -0.242782 1.329833 11.00000 -1.50000 H25B 2 0.807060 -0.210376 1.434570 11.00000 -1.50000 H25C 2 0.866838 -0.108448 1.328259 11.00000 -1.50000 AFIX 0 C26 1 0.655103 -0.264105 1.369156 11.00000 0.07509 0.04683 = 0.01561 -0.00232 0.00082 -0.04232 AFIX 137 H26A 2 0.579780 -0.244640 1.352499 11.00000 -1.50000 H26B 2 0.640223 -0.295694 1.446359 11.00000 -1.50000 H26C 2 0.706481 -0.324582 1.338703 11.00000 -1.50000 AFIX 0 N31 3 0.624148 0.225721 0.915930 11.00000 0.01318 0.01170 = 0.01309 -0.00345 -0.00440 0.00094 C32 1 0.538219 0.278085 0.852348 11.00000 0.01346 0.01888 = 0.01566 0.00231 -0.00453 0.00132 AFIX 23 H32A 2 0.551885 0.230070 0.806776 11.00000 -1.20000 H32B 2 0.555417 0.360323 0.804900 11.00000 -1.20000 AFIX 0 C33 1 0.405804 0.284342 0.916985 11.00000 0.01068 0.02394 = 0.02905 0.00077 -0.00732 -0.00161 AFIX 23 H33A 2 0.363279 0.246234 0.893137 11.00000 -1.20000 H33B 2 0.398289 0.238918 0.993033 11.00000 -1.20000 AFIX 0 O34 4 0.352694 0.405080 0.904684 11.00000 0.02199 0.02068 = 0.02085 -0.00774 -0.00895 0.00386 C35 1 0.319675 0.464244 0.809198 11.00000 0.02012 0.02726 = 0.02805 -0.00538 -0.01410 0.00241 AFIX 23 H35A 2 0.238926 0.449077 0.821001 11.00000 -1.20000 H35B 2 0.375101 0.433034 0.752895 11.00000 -1.20000 AFIX 0 C36 1 0.322959 0.596105 0.775563 11.00000 0.02004 0.03093 = 0.03710 -0.00388 -0.01286 0.00422 AFIX 23 H36A 2 0.285141 0.640809 0.718095 11.00000 -1.20000 H36B 2 0.280199 0.624937 0.836185 11.00000 -1.20000 AFIX 0 O37 4 0.444593 0.613506 0.738900 11.00000 0.02750 0.01829 = 0.04235 -0.00596 -0.01298 -0.00010 C38 1 0.461519 0.734107 0.709234 11.00000 0.03805 0.01791 = 0.02881 -0.00464 -0.01918 0.00332 AFIX 23 H38A 2 0.418689 0.763900 0.769276 11.00000 -1.20000 H38B 2 0.430173 0.784875 0.648566 11.00000 -1.20000 AFIX 0 C39 1 0.590762 0.740387 0.678874 11.00000 0.04318 0.01777 = 0.02135 -0.00042 -0.01657 -0.00481 AFIX 23 H39A 2 0.634812 0.700970 0.625371 11.00000 -1.20000 H39B 2 0.605959 0.825163 0.647693 11.00000 -1.20000 AFIX 0 O40 4 0.628970 0.681111 0.771743 11.00000 0.02448 0.02127 = 0.01728 -0.00257 -0.00876 0.00069 C41 1 0.754671 0.654605 0.748639 11.00000 0.02876 0.01598 = 0.02650 -0.00690 -0.00779 -0.00266 AFIX 23 H41A 2 0.788835 0.725489 0.737902 11.00000 -1.20000 H41B 2 0.788296 0.634761 0.682595 11.00000 -1.20000 AFIX 0 C42 1 0.785422 0.550164 0.839424 11.00000 0.01737 0.02003 = 0.03172 -0.00759 -0.00917 -0.00287 AFIX 23 H42A 2 0.872449 0.536724 0.825590 11.00000 -1.20000 H42B 2 0.749700 0.570779 0.905043 11.00000 -1.20000 AFIX 0 O43 4 0.746073 0.441006 0.856656 11.00000 0.01573 0.01379 = 0.02290 -0.00478 -0.00002 -0.00314 C44 1 0.629407 0.425038 0.929240 11.00000 0.01814 0.01896 = 0.02483 -0.01002 -0.00007 -0.00270 AFIX 23 H44A 2 0.569748 0.464669 0.890094 11.00000 -1.20000 H44B 2 0.614991 0.462842 0.982739 11.00000 -1.20000 AFIX 0 C45 1 0.616910 0.293738 0.983973 11.00000 0.01993 0.01809 = 0.01387 -0.00748 -0.00104 -0.00148 AFIX 23 H45A 2 0.679441 0.255473 1.020024 11.00000 -1.20000 H45B 2 0.539659 0.285632 1.039703 11.00000 -1.20000 HKLF 4 REM import in P -1 REM R1 = 0.0269 for 7419 Fo > 4sig(Fo) and 0.0321 for all 8228 data REM 382 parameters refined using 0 restraints END WGHT 0.0187 0.0000 REM Highest difference peak 0.60, deepest hole -1.16, 1-sigma level 0.12 Q1 1 0.8421 0.1357 0.8496 11.00000 0.05 0.60 Q2 1 0.8193 0.2975 0.7217 11.00000 0.05 0.58 Q3 1 0.7944 0.1567 0.7332 11.00000 0.05 0.55 Q4 1 0.8612 0.2557 0.8435 11.00000 0.05 0.54 Q5 1 0.7582 0.2206 0.7951 11.00000 0.05 0.54 Q6 1 0.8182 0.2764 0.7989 11.00000 0.05 0.49 Q7 1 0.6073 0.3645 0.4063 11.00000 0.05 0.46 Q8 1 0.6438 0.9209 0.6436 11.00000 0.05 0.46 Q9 1 0.9000 0.1540 0.7515 11.00000 0.05 0.45 Q10 1 1.0045 -0.2593 1.0016 11.00000 0.05 0.43 Q11 1 0.7580 0.4602 0.9957 11.00000 0.05 0.43 Q12 1 0.8417 0.1438 0.7830 11.00000 0.05 0.43 Q13 1 0.7837 0.2663 0.6264 11.00000 0.05 0.43 Q14 1 1.1608 -0.2807 0.9691 11.00000 0.05 0.42 Q15 1 0.7641 -0.1441 1.1666 11.00000 0.05 0.42 Q16 1 0.5350 0.2509 0.7610 11.00000 0.05 0.41 Q17 1 0.8577 0.3571 0.3662 11.00000 0.05 0.41 Q18 1 0.8999 -0.1822 1.0020 11.00000 0.05 0.41 Q19 1 0.8458 0.2843 0.6589 11.00000 0.05 0.41 Q20 1 0.7444 0.3022 0.9867 11.00000 0.05 0.41 ; #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Pb Pb -3.3944 10.1111 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Pb1 Pb 0.832310(10) 0.204024(10) 0.792225(8) 0.01337(4) Uani 1 1 d . . . N1 N 0.7830(2) 0.2063(2) 0.65557(19) 0.0161(6) Uani 1 1 d . . . Si1 Si 0.78077(8) 0.07272(8) 0.64259(7) 0.01659(19) Uani 1 1 d . . . C2 C 0.6627(3) -0.0141(3) 0.7535(2) 0.0217(7) Uani 1 1 d . . . H2A H 0.6846 -0.0446 0.8196 0.033 Uiso 1 1 calc R . . H2B H 0.6545 -0.0815 0.7371 0.033 Uiso 1 1 calc R . . H2C H 0.5873 0.0386 0.7618 0.033 Uiso 1 1 calc R . . C3 C 0.9288(3) -0.0203(3) 0.6377(2) 0.0241(8) Uani 1 1 d . . . H3A H 0.9898 0.0249 0.5786 0.036 Uiso 1 1 calc R . . H3B H 0.9278 -0.0944 0.6274 0.036 Uiso 1 1 calc R . . H3C H 0.9463 -0.0401 0.7045 0.036 Uiso 1 1 calc R . . C4 C 0.7456(3) 0.0936(3) 0.5187(3) 0.0299(9) Uani 1 1 d . . . H4A H 0.665 0.135 0.522 0.045 Uiso 1 1 calc R . . H4B H 0.7514 0.0151 0.5131 0.045 Uiso 1 1 calc R . . H4C H 0.802 0.1416 0.4565 0.045 Uiso 1 1 calc R . . Si2 Si 0.78752(8) 0.34227(8) 0.55345(7) 0.0193(2) Uani 1 1 d . . . C5 C 0.9118(4) 0.3433(4) 0.4294(3) 0.0368(10) Uani 1 1 d . . . H5A H 0.9873 0.3168 0.4463 0.055 Uiso 1 1 calc R . . H5B H 0.9125 0.4247 0.3773 0.055 Uiso 1 1 calc R . . H5C H 0.9004 0.2888 0.3997 0.055 Uiso 1 1 calc R . . C6 C 0.6447(3) 0.3968(3) 0.5187(3) 0.0398(10) Uani 1 1 d . . . H6A H 0.625 0.3358 0.5012 0.06 Uiso 1 1 calc R . . H6B H 0.6528 0.4712 0.4573 0.06 Uiso 1 1 calc R . . H6C H 0.5814 0.4119 0.5793 0.06 Uiso 1 1 calc R . . C7 C 0.8120(4) 0.4598(3) 0.5939(3) 0.0397(10) Uani 1 1 d . . . H7A H 0.7501 0.464 0.6591 0.06 Uiso 1 1 calc R . . H7B H 0.8092 0.5378 0.5372 0.06 Uiso 1 1 calc R . . H7C H 0.8897 0.4393 0.6065 0.06 Uiso 1 1 calc R . . O11 O 0.82215(19) 0.00780(19) 0.87142(15) 0.0168(5) Uani 1 1 d . . . C12 C 0.7968(3) -0.0329(3) 0.9773(2) 0.0117(6) Uani 1 1 d . . . C13 C 0.8677(3) -0.1339(3) 1.0307(2) 0.0136(6) Uani 1 1 d . . . C14 C 0.8380(3) -0.1659(3) 1.1409(2) 0.0152(6) Uani 1 1 d . . . H14 H 0.8852 -0.2319 1.1772 0.018 Uiso 1 1 calc R . . C15 C 0.7440(3) -0.1075(3) 1.2013(2) 0.0134(6) Uani 1 1 d . . . C16 C 0.6714(3) -0.0159(3) 1.1474(2) 0.0134(6) Uani 1 1 d . . . H16 H 0.604 0.023 1.1865 0.016 Uiso 1 1 calc R . . C17 C 0.6950(3) 0.0202(3) 1.0377(2) 0.0130(6) Uani 1 1 d . . . C18 C 0.6023(3) 0.0992(3) 0.9850(2) 0.0140(6) Uani 1 1 d . . . H18A H 0.5913 0.0598 0.9413 0.017 Uiso 1 1 calc R . . H18B H 0.5266 0.1025 1.0414 0.017 Uiso 1 1 calc R . . C19 C 0.9676(3) -0.2060(3) 0.9692(2) 0.0162(7) Uani 1 1 d . . . C20 C 1.0247(3) -0.3172(3) 1.0428(3) 0.0225(7) Uani 1 1 d . . . H20A H 1.0849 -0.3627 1.0006 0.034 Uiso 1 1 calc R . . H20B H 0.9638 -0.3679 1.0949 0.034 Uiso 1 1 calc R . . H20C H 1.062 -0.2918 1.0798 0.034 Uiso 1 1 calc R . . C21 C 0.9168(3) -0.2531(3) 0.9105(3) 0.0212(7) Uani 1 1 d . . . H21A H 0.8744 -0.1859 0.8659 0.032 Uiso 1 1 calc R . . H21B H 0.8621 -0.3108 0.9623 0.032 Uiso 1 1 calc R . . H21C H 0.9816 -0.2926 0.8659 0.032 Uiso 1 1 calc R . . C22 C 1.0653(3) -0.1273(3) 0.8913(3) 0.0232(7) Uani 1 1 d . . . H22A H 1.0315 -0.0562 0.8425 0.035 Uiso 1 1 calc R . . H22B H 1.1275 -0.1731 0.8506 0.035 Uiso 1 1 calc R . . H22C H 1.0992 -0.1024 0.931 0.035 Uiso 1 1 calc R . . C23 C 0.7155(3) -0.1513(3) 1.3224(2) 0.0165(7) Uani 1 1 d . . . C24 C 0.6331(4) -0.0582(4) 1.3693(3) 0.0428(12) Uani 1 1 d . . . H24A H 0.669 0.0164 1.3374 0.064 Uiso 1 1 calc R . . H24B H 0.6202 -0.0882 1.4463 0.064 Uiso 1 1 calc R . . H24C H 0.5572 -0.0427 1.3546 0.064 Uiso 1 1 calc R . . C25 C 0.8281(3) -0.1809(4) 1.3569(3) 0.0408(11) Uani 1 1 d . . . H25A H 0.8823 -0.2428 1.3298 0.061 Uiso 1 1 calc R . . H25B H 0.8071 -0.2104 1.4346 0.061 Uiso 1 1 calc R . . H25C H 0.8668 -0.1084 1.3283 0.061 Uiso 1 1 calc R . . C26 C 0.6551(4) -0.2641(4) 1.3692(3) 0.0459(12) Uani 1 1 d . . . H26A H 0.5798 -0.2446 1.3525 0.069 Uiso 1 1 calc R . . H26B H 0.6402 -0.2957 1.4464 0.069 Uiso 1 1 calc R . . H26C H 0.7065 -0.3246 1.3387 0.069 Uiso 1 1 calc R . . N31 N 0.6241(2) 0.2257(2) 0.91593(18) 0.0132(5) Uani 1 1 d . . . C32 C 0.5382(3) 0.2781(3) 0.8523(2) 0.0193(7) Uani 1 1 d . . . H32A H 0.5519 0.2301 0.8068 0.023 Uiso 1 1 calc R . . H32B H 0.5554 0.3603 0.8049 0.023 Uiso 1 1 calc R . . C33 C 0.4058(3) 0.2843(3) 0.9170(3) 0.0241(8) Uani 1 1 d . . . H33A H 0.3633 0.2462 0.8931 0.029 Uiso 1 1 calc R . . H33B H 0.3983 0.2389 0.993 0.029 Uiso 1 1 calc R . . O34 O 0.3527(2) 0.4051(2) 0.90468(17) 0.0215(5) Uani 1 1 d . . . C35 C 0.3197(3) 0.4642(3) 0.8092(3) 0.0255(8) Uani 1 1 d . . . H35A H 0.2389 0.4491 0.821 0.031 Uiso 1 1 calc R . . H35B H 0.3751 0.433 0.7529 0.031 Uiso 1 1 calc R . . C36 C 0.3230(3) 0.5961(3) 0.7756(3) 0.0321(9) Uani 1 1 d . . . H36A H 0.2851 0.6408 0.7181 0.038 Uiso 1 1 calc R . . H36B H 0.2802 0.6249 0.8362 0.038 Uiso 1 1 calc R . . O37 O 0.4446(2) 0.6135(2) 0.7389(2) 0.0306(6) Uani 1 1 d . . . C38 C 0.4615(3) 0.7341(3) 0.7092(3) 0.0279(8) Uani 1 1 d . . . H38A H 0.4187 0.7639 0.7693 0.034 Uiso 1 1 calc R . . H38B H 0.4302 0.7849 0.6486 0.034 Uiso 1 1 calc R . . C39 C 0.5908(3) 0.7404(3) 0.6789(3) 0.0272(8) Uani 1 1 d . . . H39A H 0.6348 0.701 0.6254 0.033 Uiso 1 1 calc R . . H39B H 0.606 0.8252 0.6477 0.033 Uiso 1 1 calc R . . O40 O 0.6290(2) 0.6811(2) 0.77174(16) 0.0223(5) Uani 1 1 d . . . C41 C 0.7547(3) 0.6546(3) 0.7486(3) 0.0240(8) Uani 1 1 d . . . H41A H 0.7888 0.7255 0.7379 0.029 Uiso 1 1 calc R . . H41B H 0.7883 0.6348 0.6826 0.029 Uiso 1 1 calc R . . C42 C 0.7854(3) 0.5502(3) 0.8394(3) 0.0228(7) Uani 1 1 d . . . H42A H 0.8724 0.5367 0.8256 0.027 Uiso 1 1 calc R . . H42B H 0.7497 0.5708 0.905 0.027 Uiso 1 1 calc R . . O43 O 0.74607(19) 0.44101(19) 0.85666(17) 0.0194(5) Uani 1 1 d . . . C44 C 0.6294(3) 0.4250(3) 0.9292(3) 0.0215(7) Uani 1 1 d . . . H44A H 0.5697 0.4647 0.8901 0.026 Uiso 1 1 calc R . . H44B H 0.615 0.4628 0.9827 0.026 Uiso 1 1 calc R . . C45 C 0.6169(3) 0.2937(3) 0.9840(2) 0.0179(7) Uani 1 1 d . . . H45A H 0.6794 0.2555 1.02 0.022 Uiso 1 1 calc R . . H45B H 0.5397 0.2856 1.0397 0.022 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 Pb1 0.01153(6) 0.01657(6) 0.01165(6) -0.00484(4) -0.00276(4) -0.00203(4) N1 0.0205(14) 0.0165(13) 0.0113(12) -0.0044(10) -0.0059(11) -0.0011(11) Si1 0.0190(5) 0.0166(4) 0.0151(4) -0.0068(4) -0.0054(4) -0.0011(4) C2 0.0233(18) 0.0207(17) 0.0243(17) -0.0123(14) -0.0037(14) -0.0052(14) C3 0.0252(19) 0.0260(19) 0.0149(16) -0.0090(14) -0.0016(14) 0.0044(15) C4 0.040(2) 0.033(2) 0.0219(18) -0.0136(16) -0.0111(17) -0.0033(17) Si2 0.0247(5) 0.0166(4) 0.0126(4) -0.0020(4) -0.0036(4) -0.0034(4) C5 0.044(3) 0.038(2) 0.0216(19) -0.0076(17) 0.0027(17) -0.0161(19) C6 0.041(2) 0.025(2) 0.039(2) 0.0054(17) -0.0185(19) 0.0030(18) C7 0.073(3) 0.0192(19) 0.025(2) -0.0003(16) -0.017(2) -0.0118(19) O11 0.0191(12) 0.0163(11) 0.0108(10) -0.0030(9) -0.0038(9) 0.0011(9) C12 0.0102(15) 0.0141(15) 0.0121(14) -0.0039(12) -0.0044(12) -0.0031(11) C13 0.0120(15) 0.0134(15) 0.0152(15) -0.0039(12) -0.0052(12) -0.0012(12) C14 0.0160(16) 0.0132(15) 0.0157(15) -0.0025(12) -0.0077(13) -0.0002(12) C15 0.0158(16) 0.0122(14) 0.0113(14) -0.0002(12) -0.0042(12) -0.0063(12) C16 0.0110(15) 0.0131(15) 0.0135(14) -0.0040(12) -0.0002(12) -0.0032(11) C17 0.0149(16) 0.0097(14) 0.0129(14) -0.0012(12) -0.0050(12) -0.0022(12) C18 0.0086(15) 0.0171(16) 0.0152(14) -0.0045(12) -0.0028(12) -0.0023(12) C19 0.0142(16) 0.0184(16) 0.0168(15) -0.0070(13) -0.0061(13) 0.0004(12) C20 0.0186(18) 0.0235(18) 0.0254(17) -0.0101(15) -0.0098(14) 0.0052(14) C21 0.0235(18) 0.0213(17) 0.0217(17) -0.0097(14) -0.0101(14) 0.0012(14) C22 0.0141(17) 0.0259(18) 0.0278(18) -0.0119(15) -0.0035(14) 0.0011(14) C23 0.0237(18) 0.0152(16) 0.0098(14) -0.0017(12) -0.0050(13) -0.0055(13) C24 0.064(3) 0.041(2) 0.0189(18) -0.0155(17) -0.0178(19) 0.019(2) C25 0.032(2) 0.068(3) 0.0173(18) -0.0041(19) -0.0104(17) -0.011(2) C26 0.075(3) 0.047(3) 0.0156(18) -0.0023(17) 0.0008(19) -0.042(2) N31 0.0132(13) 0.0117(13) 0.0131(12) -0.0035(10) -0.0044(10) 0.0009(10) C32 0.0135(16) 0.0189(16) 0.0157(15) 0.0023(13) -0.0045(13) 0.0013(13) C33 0.0107(16) 0.0239(18) 0.0291(18) 0.0008(15) -0.0073(14) -0.0016(13) O34 0.0220(13) 0.0207(12) 0.0209(12) -0.0077(10) -0.0090(10) 0.0039(10) C35 0.0201(18) 0.0273(19) 0.0281(18) -0.0054(15) -0.0141(15) 0.0024(15) C36 0.0200(19) 0.031(2) 0.037(2) -0.0039(17) -0.0129(17) 0.0042(16) O37 0.0275(14) 0.0183(13) 0.0424(15) -0.0060(11) -0.0130(12) -0.0001(10) C38 0.038(2) 0.0179(17) 0.0288(19) -0.0046(15) -0.0192(17) 0.0033(15) C39 0.043(2) 0.0178(17) 0.0214(17) -0.0004(14) -0.0166(16) -0.0048(16) O40 0.0245(13) 0.0213(12) 0.0173(11) -0.0026(10) -0.0088(10) 0.0007(10) C41 0.029(2) 0.0160(17) 0.0265(18) -0.0069(14) -0.0078(15) -0.0027(14) C42 0.0174(17) 0.0200(17) 0.0317(19) -0.0076(15) -0.0092(15) -0.0029(13) O43 0.0157(12) 0.0138(11) 0.0229(12) -0.0048(9) 0.0000(9) -0.0031(9) C44 0.0181(17) 0.0190(17) 0.0248(17) -0.0100(14) -0.0001(14) -0.0027(13) C45 0.0199(17) 0.0181(16) 0.0139(15) -0.0075(13) -0.0010(13) -0.0015(13) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Pb1 O11 2.227(2) . ? Pb1 N1 2.237(2) . ? Pb1 N31 2.543(2) . ? N1 Si2 1.723(3) . ? N1 Si1 1.727(3) . ? Si1 C3 1.872(3) . ? Si1 C2 1.875(3) . ? Si1 C4 1.882(3) . ? C2 H2A 0.98 . ? C2 H2B 0.98 . ? C2 H2C 0.98 . ? C3 H3A 0.98 . ? C3 H3B 0.98 . ? C3 H3C 0.98 . ? C4 H4A 0.98 . ? C4 H4B 0.98 . ? C4 H4C 0.98 . ? Si2 C7 1.872(4) . ? Si2 C6 1.872(4) . ? Si2 C5 1.877(4) . ? C5 H5A 0.98 . ? C5 H5B 0.98 . ? C5 H5C 0.98 . ? C6 H6A 0.98 . ? C6 H6B 0.98 . ? C6 H6C 0.98 . ? C7 H7A 0.98 . ? C7 H7B 0.98 . ? C7 H7C 0.98 . ? O11 C12 1.339(3) . ? C12 C17 1.410(4) . ? C12 C13 1.431(4) . ? C13 C14 1.399(4) . ? C13 C19 1.534(4) . ? C14 C15 1.395(4) . ? C14 H14 0.95 . ? C15 C16 1.394(4) . ? C15 C23 1.532(4) . ? C16 C17 1.393(4) . ? C16 H16 0.95 . ? C17 C18 1.506(4) . ? C18 N31 1.500(4) . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C19 C22 1.537(4) . ? C19 C21 1.538(4) . ? C19 C20 1.538(4) . ? C20 H20A 0.98 . ? C20 H20B 0.98 . ? C20 H20C 0.98 . ? C21 H21A 0.98 . ? C21 H21B 0.98 . ? C21 H21C 0.98 . ? C22 H22A 0.98 . ? C22 H22B 0.98 . ? C22 H22C 0.98 . ? C23 C24 1.521(5) . ? C23 C26 1.523(5) . ? C23 C25 1.536(5) . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? N31 C45 1.485(4) . ? N31 C32 1.492(4) . ? C32 C33 1.547(4) . ? C32 H32A 0.99 . ? C32 H32B 0.99 . ? C33 O34 1.425(4) . ? C33 H33A 0.99 . ? C33 H33B 0.99 . ? O34 C35 1.423(4) . ? C35 C36 1.497(5) . ? C35 H35A 0.99 . ? C35 H35B 0.99 . ? C36 O37 1.425(4) . ? C36 H36A 0.99 . ? C36 H36B 0.99 . ? O37 C38 1.413(4) . ? C38 C39 1.490(5) . ? C38 H38A 0.99 . ? C38 H38B 0.99 . ? C39 O40 1.424(4) . ? C39 H39A 0.99 . ? C39 H39B 0.99 . ? O40 C41 1.427(4) . ? C41 C42 1.503(4) . ? C41 H41A 0.99 . ? C41 H41B 0.99 . ? C42 O43 1.433(4) . ? C42 H42A 0.99 . ? C42 H42B 0.99 . ? O43 C44 1.436(4) . ? C44 C45 1.503(4) . ? C44 H44A 0.99 . ? C44 H44B 0.99 . ? C45 H45A 0.99 . ? C45 H45B 0.99 . ? 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 O11 Pb1 N1 91.51(8) . . ? O11 Pb1 N31 84.68(8) . . ? N1 Pb1 N31 97.97(8) . . ? Si2 N1 Si1 123.58(14) . . ? Si2 N1 Pb1 114.52(14) . . ? Si1 N1 Pb1 119.74(13) . . ? N1 Si1 C3 110.00(15) . . ? N1 Si1 C2 111.83(14) . . ? C3 Si1 C2 109.90(15) . . ? N1 Si1 C4 113.25(15) . . ? C3 Si1 C4 107.26(15) . . ? C2 Si1 C4 104.36(16) . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N1 Si2 C7 110.06(15) . . ? N1 Si2 C6 112.12(16) . . ? C7 Si2 C6 106.18(19) . . ? N1 Si2 C5 114.25(16) . . ? C7 Si2 C5 104.97(19) . . ? C6 Si2 C5 108.71(18) . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C12 O11 Pb1 115.74(18) . . ? O11 C12 C17 119.5(2) . . ? O11 C12 C13 121.0(3) . . ? C17 C12 C13 119.3(3) . . ? C14 C13 C12 116.9(3) . . ? C14 C13 C19 122.2(3) . . ? C12 C13 C19 120.9(3) . . ? C15 C14 C13 124.5(3) . . ? C15 C14 H14 117.8 . . ? C13 C14 H14 117.8 . . ? C14 C15 C16 116.8(3) . . ? C14 C15 C23 121.0(3) . . ? C16 C15 C23 122.0(3) . . ? C17 C16 C15 121.8(3) . . ? C17 C16 H16 119.1 . . ? C15 C16 H16 119.1 . . ? C16 C17 C12 120.2(3) . . ? C16 C17 C18 120.3(3) . . ? C12 C17 C18 118.6(2) . . ? N31 C18 C17 117.9(2) . . ? N31 C18 H18A 107.8 . . ? C17 C18 H18A 107.8 . . ? N31 C18 H18B 107.8 . . ? C17 C18 H18B 107.8 . . ? H18A C18 H18B 107.2 . . ? C13 C19 C22 110.0(3) . . ? C13 C19 C21 109.5(3) . . ? C22 C19 C21 111.2(3) . . ? C13 C19 C20 112.3(2) . . ? C22 C19 C20 107.7(3) . . ? C21 C19 C20 106.2(3) . . ? C19 C20 H20A 109.5 . . ? C19 C20 H20B 109.5 . . ? H20A C20 H20B 109.5 . . ? C19 C20 H20C 109.5 . . ? H20A C20 H20C 109.5 . . ? H20B C20 H20C 109.5 . . ? C19 C21 H21A 109.5 . . ? C19 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C19 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C19 C22 H22A 109.5 . . ? C19 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C19 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C24 C23 C26 108.4(3) . . ? C24 C23 C15 112.2(3) . . ? C26 C23 C15 108.5(3) . . ? C24 C23 C25 107.3(3) . . ? C26 C23 C25 108.8(3) . . ? C15 C23 C25 111.5(3) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C45 N31 C32 113.7(2) . . ? C45 N31 C18 108.8(2) . . ? C32 N31 C18 108.9(2) . . ? C45 N31 Pb1 111.57(18) . . ? C32 N31 Pb1 109.27(17) . . ? C18 N31 Pb1 104.14(16) . . ? N31 C32 C33 115.8(2) . . ? N31 C32 H32A 108.3 . . ? C33 C32 H32A 108.3 . . ? N31 C32 H32B 108.3 . . ? C33 C32 H32B 108.3 . . ? H32A C32 H32B 107.4 . . ? O34 C33 C32 111.6(3) . . ? O34 C33 H33A 109.3 . . ? C32 C33 H33A 109.3 . . ? O34 C33 H33B 109.3 . . ? C32 C33 H33B 109.3 . . ? H33A C33 H33B 108 . . ? C35 O34 C33 113.1(2) . . ? O34 C35 C36 108.9(3) . . ? O34 C35 H35A 109.9 . . ? C36 C35 H35A 109.9 . . ? O34 C35 H35B 109.9 . . ? C36 C35 H35B 109.9 . . ? H35A C35 H35B 108.3 . . ? O37 C36 C35 106.8(3) . . ? O37 C36 H36A 110.4 . . ? C35 C36 H36A 110.4 . . ? O37 C36 H36B 110.4 . . ? C35 C36 H36B 110.4 . . ? H36A C36 H36B 108.6 . . ? C38 O37 C36 113.3(3) . . ? O37 C38 C39 108.6(3) . . ? O37 C38 H38A 110 . . ? C39 C38 H38A 110 . . ? O37 C38 H38B 110 . . ? C39 C38 H38B 110 . . ? H38A C38 H38B 108.4 . . ? O40 C39 C38 108.3(3) . . ? O40 C39 H39A 110 . . ? C38 C39 H39A 110 . . ? O40 C39 H39B 110 . . ? C38 C39 H39B 110 . . ? H39A C39 H39B 108.4 . . ? C39 O40 C41 113.0(3) . . ? O40 C41 C42 109.3(3) . . ? O40 C41 H41A 109.8 . . ? C42 C41 H41A 109.8 . . ? O40 C41 H41B 109.8 . . ? C42 C41 H41B 109.8 . . ? H41A C41 H41B 108.3 . . ? O43 C42 C41 113.8(3) . . ? O43 C42 H42A 108.8 . . ? C41 C42 H42A 108.8 . . ? O43 C42 H42B 108.8 . . ? C41 C42 H42B 108.8 . . ? H42A C42 H42B 107.7 . . ? C42 O43 C44 113.6(2) . . ? O43 C44 C45 110.2(3) . . ? O43 C44 H44A 109.6 . . ? C45 C44 H44A 109.6 . . ? O43 C44 H44B 109.6 . . ? C45 C44 H44B 109.6 . . ? H44A C44 H44B 108.1 . . ? N31 C45 C44 116.6(3) . . ? N31 C45 H45A 108.1 . . ? C44 C45 H45A 108.1 . . ? N31 C45 H45B 108.1 . . ? C44 C45 H45B 108.1 . . ? H45A C45 H45B 107.3 . . ? 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 O11 Pb1 N1 Si2 -174.75(13) . . . . ? N31 Pb1 N1 Si2 100.40(14) . . . . ? O11 Pb1 N1 Si1 -10.89(15) . . . . ? N31 Pb1 N1 Si1 -95.73(15) . . . . ? Si2 N1 Si1 C3 105.59(19) . . . . ? Pb1 N1 Si1 C3 -56.74(18) . . . . ? Si2 N1 Si1 C2 -131.99(18) . . . . ? Pb1 N1 Si1 C2 65.67(19) . . . . ? Si2 N1 Si1 C4 -14.4(2) . . . . ? Pb1 N1 Si1 C4 -176.75(15) . . . . ? Si1 N1 Si2 C7 -171.4(2) . . . . ? Pb1 N1 Si2 C7 -8.3(2) . . . . ? Si1 N1 Si2 C6 70.6(2) . . . . ? Pb1 N1 Si2 C6 -126.22(17) . . . . ? Si1 N1 Si2 C5 -53.6(2) . . . . ? Pb1 N1 Si2 C5 109.52(18) . . . . ? N1 Pb1 O11 C12 -153.18(19) . . . . ? N31 Pb1 O11 C12 -55.31(19) . . . . ? Pb1 O11 C12 C17 54.0(3) . . . . ? Pb1 O11 C12 C13 -129.6(2) . . . . ? O11 C12 C13 C14 176.7(3) . . . . ? C17 C12 C13 C14 -6.8(4) . . . . ? O11 C12 C13 C19 -5.9(4) . . . . ? C17 C12 C13 C19 170.5(3) . . . . ? C12 C13 C14 C15 1.1(5) . . . . ? C19 C13 C14 C15 -176.3(3) . . . . ? C13 C14 C15 C16 4.0(5) . . . . ? C13 C14 C15 C23 178.0(3) . . . . ? C14 C15 C16 C17 -3.3(5) . . . . ? C23 C15 C16 C17 -177.3(3) . . . . ? C15 C16 C17 C12 -2.4(5) . . . . ? C15 C16 C17 C18 166.6(3) . . . . ? O11 C12 C17 C16 -175.9(3) . . . . ? C13 C12 C17 C16 7.6(4) . . . . ? O11 C12 C17 C18 14.9(4) . . . . ? C13 C12 C17 C18 -161.6(3) . . . . ? C16 C17 C18 N31 111.1(3) . . . . ? C12 C17 C18 N31 -79.7(4) . . . . ? C14 C13 C19 C22 -117.4(3) . . . . ? C12 C13 C19 C22 65.3(4) . . . . ? C14 C13 C19 C21 120.2(3) . . . . ? C12 C13 C19 C21 -57.1(4) . . . . ? C14 C13 C19 C20 2.5(4) . . . . ? C12 C13 C19 C20 -174.7(3) . . . . ? C14 C15 C23 C24 164.8(3) . . . . ? C16 C15 C23 C24 -21.5(4) . . . . ? C14 C15 C23 C26 -75.4(4) . . . . ? C16 C15 C23 C26 98.3(4) . . . . ? C14 C15 C23 C25 44.4(4) . . . . ? C16 C15 C23 C25 -141.9(3) . . . . ? C17 C18 N31 C45 -68.9(3) . . . . ? C17 C18 N31 C32 166.7(2) . . . . ? C17 C18 N31 Pb1 50.2(3) . . . . ? O11 Pb1 N31 C45 121.57(18) . . . . ? N1 Pb1 N31 C45 -147.64(18) . . . . ? O11 Pb1 N31 C32 -111.87(19) . . . . ? N1 Pb1 N31 C32 -21.1(2) . . . . ? O11 Pb1 N31 C18 4.39(17) . . . . ? N1 Pb1 N31 C18 95.18(18) . . . . ? C45 N31 C32 C33 -61.1(4) . . . . ? C18 N31 C32 C33 60.4(3) . . . . ? Pb1 N31 C32 C33 173.6(2) . . . . ? N31 C32 C33 O34 111.5(3) . . . . ? C32 C33 O34 C35 80.9(3) . . . . ? C33 O34 C35 C36 -152.1(3) . . . . ? O34 C35 C36 O37 71.4(3) . . . . ? C35 C36 O37 C38 -177.0(3) . . . . ? C36 O37 C38 C39 176.5(3) . . . . ? O37 C38 C39 O40 -68.1(3) . . . . ? C38 C39 O40 C41 164.9(3) . . . . ? C39 O40 C41 C42 -155.3(3) . . . . ? O40 C41 C42 O43 63.3(4) . . . . ? C41 C42 O43 C44 -90.2(3) . . . . ? C42 O43 C44 C45 -152.3(3) . . . . ? C32 N31 C45 C44 -55.0(4) . . . . ? C18 N31 C45 C44 -176.5(3) . . . . ? Pb1 N31 C45 C44 69.2(3) . . . . ? O43 C44 C45 N31 -65.1(4) . . . . ? _database_code_depnum_ccdc_archive 'CCDC 942096' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_WLF021 _audit_creation_date 2013-04-23T11:26:58-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C25 H42 Cl N O5 Sn' _chemical_formula_sum 'C25 H42 Cl N O5 Sn' _chemical_formula_weight 590.74 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/n' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_Int_Tables_number 14 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 14.4474(6) _cell_length_b 10.9372(5) _cell_length_c 18.6881(7) _cell_angle_alpha 90 _cell_angle_beta 111.8890(10) _cell_angle_gamma 90 _cell_volume 2740.1(2) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7979 _cell_measurement_theta_min 2.2 _cell_measurement_theta_max 27.49 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description board _exptl_crystal_colour colourless _exptl_crystal_size_max 0.56 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.08 _exptl_crystal_density_diffrn 1.432 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1224 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 1.063 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.701 _exptl_absorpt_correction_T_max 0.918 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0435 _diffrn_reflns_av_unetI/netI 0.0423 _diffrn_reflns_number 22244 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.996 _diffrn_measured_fraction_theta_max 0.996 _reflns_number_total 6259 _reflns_number_gt 5399 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 2012), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0283P)^2^+1.9296P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 6259 _refine_ls_number_parameters 304 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0384 _refine_ls_R_factor_gt 0.0307 _refine_ls_wR_factor_ref 0.0748 _refine_ls_wR_factor_gt 0.0707 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_restrained_S_all 1.024 _refine_ls_shift/su_max 0.011 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 1.418 _refine_diff_density_min -0.574 _refine_diff_density_rms 0.079 _iucr_refine_instructions_details ; .res file for SHELXL : job.res ................................................................. TITL import in P 21/n CELL 0.71073 14.4474 10.9372 18.6881 90.000 111.889 90.000 ZERR 4.00 0.0006 0.0005 0.0007 0.000 0.001 0.000 LATT 1 SYMM 1/2 - X, 1/2 + Y, 1/2 - Z SFAC C H N O CL SN UNIT 100 168 4 20 4 4 MERG 2 FMAP 2 PLAN 20 ACTA BOND $H CONF LIST 4 WPDB -2 L.S. 4 TEMP -123.00 WGHT 0.028300 1.929600 FVAR 0.36261 SN1 6 0.067938 0.059988 0.616618 11.00000 0.01487 0.02055 = 0.02009 0.00190 0.00319 0.00273 CL2 5 0.047794 -0.161209 0.632432 11.00000 0.02871 0.02225 = 0.02884 -0.00119 0.00357 -0.00335 N1 3 0.195057 0.095419 0.737863 11.00000 0.01804 0.01250 = 0.01820 0.00010 0.00754 0.00059 C2 1 0.235864 -0.013922 0.786747 11.00000 0.01868 0.01398 = 0.02009 0.00071 0.00682 0.00061 AFIX 23 H2A 2 0.265213 -0.069027 0.758832 11.00000 -1.20000 H2B 2 0.179870 -0.058173 0.793462 11.00000 -1.20000 AFIX 0 C3 1 0.314817 0.011912 0.866424 11.00000 0.02476 0.01907 = 0.02038 0.00140 0.00380 0.00019 AFIX 23 H3A 2 0.366769 0.067500 0.862446 11.00000 -1.20000 H3B 2 0.284174 0.050078 0.900303 11.00000 -1.20000 AFIX 0 O4 4 0.356737 -0.104173 0.896165 11.00000 0.03410 0.02101 = 0.01902 0.00237 0.00528 0.00729 C5 1 0.395734 -0.112739 0.978548 11.00000 0.02449 0.02894 = 0.02013 0.00479 0.00194 0.00032 AFIX 23 H5A 2 0.414267 -0.030040 1.000834 11.00000 -1.20000 H5B 2 0.456906 -0.163436 0.995595 11.00000 -1.20000 AFIX 0 C6 1 0.321916 -0.167748 1.008260 11.00000 0.03562 0.02914 = 0.02984 0.00901 0.01164 0.00487 AFIX 23 H6A 2 0.291849 -0.241878 0.978171 11.00000 -1.20000 H6B 2 0.355942 -0.191646 1.062955 11.00000 -1.20000 AFIX 0 O7 4 0.246028 -0.079925 1.001346 11.00000 0.03388 0.03925 = 0.04451 0.00848 0.02027 0.00362 C8 1 0.163838 -0.131306 1.014594 11.00000 0.03930 0.06974 = 0.04258 0.02321 0.02199 0.00926 AFIX 23 H8A 2 0.133136 -0.067899 1.036474 11.00000 -1.20000 H8B 2 0.187866 -0.197955 1.052948 11.00000 -1.20000 AFIX 0 C9 1 0.088649 -0.179605 0.944325 11.00000 0.04083 0.05305 = 0.05117 0.02298 0.01301 -0.00752 AFIX 23 H9A 2 0.119979 -0.234696 0.917834 11.00000 -1.20000 H9B 2 0.037969 -0.226569 0.956723 11.00000 -1.20000 AFIX 0 O10 4 0.042398 -0.076417 0.895183 11.00000 0.03639 0.05637 = 0.03581 0.01218 0.00421 -0.01215 C11 1 -0.019701 -0.112436 0.821485 11.00000 0.02864 0.04544 = 0.04698 0.00890 0.01147 -0.00767 AFIX 23 H11A 2 -0.075206 -0.162382 0.824634 11.00000 -1.20000 H11B 2 0.018386 -0.163339 0.798223 11.00000 -1.20000 AFIX 0 C12 1 -0.060754 -0.003286 0.771947 11.00000 0.01747 0.04474 = 0.03385 0.00712 0.00728 -0.00532 AFIX 23 H12A 2 -0.117188 -0.029842 0.725253 11.00000 -1.20000 H12B 2 -0.087509 0.054114 0.800423 11.00000 -1.20000 AFIX 0 O13 4 0.009535 0.060767 0.748441 11.00000 0.02156 0.03374 = 0.02550 -0.00102 0.00824 -0.00509 C14 1 0.080059 0.132250 0.808211 11.00000 0.02209 0.02269 = 0.02684 -0.00365 0.01160 0.00027 AFIX 23 H14A 2 0.116643 0.079938 0.853111 11.00000 -1.20000 H14B 2 0.045328 0.197371 0.825277 11.00000 -1.20000 AFIX 0 C15 1 0.151657 0.187930 0.775569 11.00000 0.02347 0.01518 = 0.02586 -0.00340 0.01096 0.00058 AFIX 23 H15A 2 0.116198 0.251162 0.737245 11.00000 -1.20000 H15B 2 0.206509 0.228628 0.817660 11.00000 -1.20000 AFIX 0 C21 1 0.272698 0.159563 0.715938 11.00000 0.01938 0.01637 = 0.02135 0.00125 0.00891 -0.00234 AFIX 23 H21A 2 0.239637 0.222918 0.676930 11.00000 -1.20000 H21B 2 0.320086 0.201425 0.762008 11.00000 -1.20000 AFIX 0 C22 1 0.329852 0.075752 0.684212 11.00000 0.01717 0.01979 = 0.01786 0.00245 0.00724 -0.00052 C23 1 0.432264 0.059180 0.724272 11.00000 0.01849 0.02483 = 0.01786 0.00077 0.00535 -0.00386 AFIX 43 H23 2 0.463874 0.098995 0.772459 11.00000 -1.20000 AFIX 0 C24 1 0.488957 -0.013921 0.695478 11.00000 0.01705 0.02499 = 0.02216 0.00664 0.00742 -0.00036 C25 1 0.439575 -0.065812 0.622846 11.00000 0.02266 0.02459 = 0.02254 0.00576 0.01252 0.00477 AFIX 43 H25 2 0.477927 -0.112137 0.600850 11.00000 -1.20000 AFIX 0 C26 1 0.336811 -0.053858 0.580255 11.00000 0.02338 0.02299 = 0.01581 0.00437 0.00838 0.00267 C27 1 0.281173 0.017114 0.613088 11.00000 0.01796 0.01962 = 0.01859 0.00442 0.00619 0.00062 C28 1 0.599846 -0.035147 0.743491 11.00000 0.01614 0.03347 = 0.03030 0.00934 0.00659 0.00153 C29 1 0.609743 -0.093890 0.820639 11.00000 0.02349 0.05931 = 0.03217 0.01928 0.00224 0.00183 AFIX 137 H29A 2 0.575925 -0.042652 0.846419 11.00000 -1.50000 H29B 2 0.680487 -0.101254 0.853517 11.00000 -1.50000 H29C 2 0.579133 -0.175252 0.811214 11.00000 -1.50000 AFIX 0 C30 1 0.656039 0.087542 0.759483 11.00000 0.02176 0.04320 = 0.04765 0.00482 0.00881 -0.00333 AFIX 137 H30A 2 0.649646 0.125964 0.710489 11.00000 -1.50000 H30B 2 0.726698 0.073225 0.790362 11.00000 -1.50000 H30C 2 0.627558 0.141568 0.787781 11.00000 -1.50000 AFIX 0 C31 1 0.649355 -0.120969 0.703507 11.00000 0.02039 0.04428 = 0.05101 0.00516 0.01445 0.00643 AFIX 137 H31A 2 0.614971 -0.200040 0.693865 11.00000 -1.50000 H31B 2 0.719526 -0.132839 0.736687 11.00000 -1.50000 H31C 2 0.645222 -0.084899 0.654404 11.00000 -1.50000 AFIX 0 C32 1 0.286610 -0.115226 0.501288 11.00000 0.02499 0.03215 = 0.01550 0.00061 0.00649 0.00707 C33 1 0.211865 -0.211477 0.506034 11.00000 0.03398 0.03275 = 0.02149 -0.00772 0.00668 0.00033 AFIX 137 H33A 2 0.248024 -0.279486 0.538657 11.00000 -1.50000 H33B 2 0.172918 -0.241964 0.454176 11.00000 -1.50000 H33C 2 0.166907 -0.174465 0.528299 11.00000 -1.50000 AFIX 0 C34 1 0.232906 -0.018836 0.440054 11.00000 0.04339 0.04538 = 0.01817 0.00753 0.01124 0.01159 AFIX 137 H34A 2 0.180137 0.019840 0.453213 11.00000 -1.50000 H34B 2 0.203459 -0.058276 0.389485 11.00000 -1.50000 H34C 2 0.280868 0.043405 0.438409 11.00000 -1.50000 AFIX 0 C35 1 0.362121 -0.180943 0.474645 11.00000 0.04187 0.05044 = 0.02539 -0.00432 0.01668 0.01055 AFIX 137 H35A 2 0.411149 -0.121851 0.470971 11.00000 -1.50000 H35B 2 0.327049 -0.218166 0.424010 11.00000 -1.50000 H35C 2 0.396339 -0.244738 0.511956 11.00000 -1.50000 AFIX 0 O36 4 0.181873 0.033478 0.576193 11.00000 0.01787 0.02802 = 0.01783 -0.00020 0.00383 0.00282 HKLF 4 REM import in P 21/n REM R1 = 0.0307 for 5399 Fo > 4sig(Fo) and 0.0384 for all 6259 data REM 304 parameters refined using 0 restraints END WGHT 0.0275 1.9791 REM Highest difference peak 1.42, deepest hole -0.57, 1-sigma level 0.08 Q1 1 0.0220 -0.0024 0.9122 11.00000 0.05 1.42 Q2 1 0.0588 -0.0806 0.9810 11.00000 0.05 1.03 Q3 1 0.0647 0.1487 0.6120 11.00000 0.05 0.61 Q4 1 0.0676 -0.0362 0.6184 11.00000 0.05 0.54 Q5 1 0.0590 0.0578 0.5670 11.00000 0.05 0.47 Q6 1 0.2060 -0.1069 0.9624 11.00000 0.05 0.43 Q7 1 0.5492 -0.0295 0.7128 11.00000 0.05 0.38 Q8 1 0.1491 -0.1831 0.9834 11.00000 0.05 0.38 Q9 1 0.0683 0.0632 0.6605 11.00000 0.05 0.38 Q10 1 0.3781 0.0651 0.7086 11.00000 0.05 0.37 Q11 1 0.4614 -0.0556 0.6648 11.00000 0.05 0.33 Q12 1 0.6019 -0.0652 0.7751 11.00000 0.05 0.32 Q13 1 0.2575 -0.0766 0.4724 11.00000 0.05 0.31 Q14 1 0.0409 -0.1428 0.6758 11.00000 0.05 0.31 Q15 1 0.3088 -0.0887 0.5390 11.00000 0.05 0.30 Q16 1 0.3187 0.0619 0.6504 11.00000 0.05 0.30 Q17 1 0.0546 -0.1138 0.6032 11.00000 0.05 0.30 Q18 1 0.2225 -0.0011 0.5960 11.00000 0.05 0.29 Q19 1 0.2398 -0.1413 0.4995 11.00000 0.05 0.29 Q20 1 0.3178 -0.1463 0.4917 11.00000 0.05 0.29 ; # End of res file #----------------------------------------------------------------------------# #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' 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 0.067938(11) 0.059988(15) 0.616618(8) 0.01946(6) Uani 1 1 d . . . Cl2 Cl 0.04779(4) -0.16121(6) 0.63243(3) 0.02867(14) Uani 1 1 d . . . N1 N 0.19506(13) 0.09542(17) 0.73786(10) 0.0160(4) Uani 1 1 d . . . C2 C 0.23586(16) -0.0139(2) 0.78675(12) 0.0177(4) Uani 1 1 d . . . H2A H 0.2652 -0.069 0.7588 0.021 Uiso 1 1 calc R . . H2B H 0.1799 -0.0582 0.7935 0.021 Uiso 1 1 calc R . . C3 C 0.31482(17) 0.0119(2) 0.86642(13) 0.0227(5) Uani 1 1 d . . . H3A H 0.3668 0.0675 0.8624 0.027 Uiso 1 1 calc R . . H3B H 0.2842 0.0501 0.9003 0.027 Uiso 1 1 calc R . . O4 O 0.35674(13) -0.10417(16) 0.89617(9) 0.0260(4) Uani 1 1 d . . . C5 C 0.39573(18) -0.1127(2) 0.97855(13) 0.0264(5) Uani 1 1 d . . . H5A H 0.4143 -0.03 1.0008 0.032 Uiso 1 1 calc R . . H5B H 0.4569 -0.1634 0.9956 0.032 Uiso 1 1 calc R . . C6 C 0.32192(19) -0.1677(3) 1.00826(15) 0.0317(6) Uani 1 1 d . . . H6A H 0.2918 -0.2419 0.9782 0.038 Uiso 1 1 calc R . . H6B H 0.3559 -0.1916 1.063 0.038 Uiso 1 1 calc R . . O7 O 0.24603(15) -0.07992(18) 1.00135(12) 0.0376(5) Uani 1 1 d . . . C8 C 0.1638(2) -0.1313(3) 1.01459(17) 0.0486(8) Uani 1 1 d . . . H8A H 0.1331 -0.0679 1.0365 0.058 Uiso 1 1 calc R . . H8B H 0.1879 -0.198 1.0529 0.058 Uiso 1 1 calc R . . C9 C 0.0886(2) -0.1796(3) 0.94432(18) 0.0495(8) Uani 1 1 d . . . H9A H 0.12 -0.2347 0.9178 0.059 Uiso 1 1 calc R . . H9B H 0.038 -0.2266 0.9567 0.059 Uiso 1 1 calc R . . O10 O 0.04240(15) -0.0764(2) 0.89518(11) 0.0455(5) Uani 1 1 d . . . C11 C -0.0197(2) -0.1124(3) 0.82148(16) 0.0411(7) Uani 1 1 d . . . H11A H -0.0752 -0.1624 0.8246 0.049 Uiso 1 1 calc R . . H11B H 0.0184 -0.1633 0.7982 0.049 Uiso 1 1 calc R . . C12 C -0.06075(18) -0.0033(3) 0.77195(15) 0.0327(6) Uani 1 1 d . . . H12A H -0.1172 -0.0298 0.7253 0.039 Uiso 1 1 calc R . . H12B H -0.0875 0.0541 0.8004 0.039 Uiso 1 1 calc R . . O13 O 0.00954(13) 0.06077(16) 0.74844(10) 0.0271(4) Uani 1 1 d . . . C14 C 0.08006(17) 0.1322(2) 0.80821(13) 0.0232(5) Uani 1 1 d . . . H14A H 0.1166 0.0799 0.8531 0.028 Uiso 1 1 calc R . . H14B H 0.0453 0.1974 0.8253 0.028 Uiso 1 1 calc R . . C15 C 0.15166(17) 0.1879(2) 0.77557(13) 0.0210(5) Uani 1 1 d . . . H15A H 0.1162 0.2512 0.7372 0.025 Uiso 1 1 calc R . . H15B H 0.2065 0.2286 0.8177 0.025 Uiso 1 1 calc R . . C21 C 0.27270(16) 0.1596(2) 0.71594(12) 0.0187(5) Uani 1 1 d . . . H21A H 0.2396 0.2229 0.6769 0.022 Uiso 1 1 calc R . . H21B H 0.3201 0.2014 0.762 0.022 Uiso 1 1 calc R . . C22 C 0.32985(16) 0.0758(2) 0.68421(12) 0.0181(5) Uani 1 1 d . . . C23 C 0.43226(17) 0.0592(2) 0.72427(13) 0.0208(5) Uani 1 1 d . . . H23 H 0.4639 0.099 0.7725 0.025 Uiso 1 1 calc R . . C24 C 0.48896(16) -0.0139(2) 0.69548(13) 0.0214(5) Uani 1 1 d . . . C25 C 0.43958(18) -0.0658(2) 0.62285(13) 0.0221(5) Uani 1 1 d . . . H25 H 0.4779 -0.1121 0.6009 0.026 Uiso 1 1 calc R . . C26 C 0.33681(17) -0.0539(2) 0.58025(12) 0.0204(5) Uani 1 1 d . . . C27 C 0.28117(16) 0.0171(2) 0.61309(12) 0.0189(5) Uani 1 1 d . . . C28 C 0.59985(18) -0.0351(2) 0.74349(15) 0.0272(6) Uani 1 1 d . . . C29 C 0.6097(2) -0.0939(3) 0.82064(15) 0.0407(7) Uani 1 1 d . . . H29A H 0.5759 -0.0427 0.8464 0.061 Uiso 1 1 calc R . . H29B H 0.6805 -0.1013 0.8535 0.061 Uiso 1 1 calc R . . H29C H 0.5791 -0.1753 0.8112 0.061 Uiso 1 1 calc R . . C30 C 0.6560(2) 0.0875(3) 0.75948(17) 0.0387(7) Uani 1 1 d . . . H30A H 0.6496 0.126 0.7105 0.058 Uiso 1 1 calc R . . H30B H 0.7267 0.0732 0.7904 0.058 Uiso 1 1 calc R . . H30C H 0.6276 0.1416 0.7878 0.058 Uiso 1 1 calc R . . C31 C 0.64936(19) -0.1210(3) 0.70351(17) 0.0382(7) Uani 1 1 d . . . H31A H 0.615 -0.2 0.6939 0.057 Uiso 1 1 calc R . . H31B H 0.7195 -0.1328 0.7367 0.057 Uiso 1 1 calc R . . H31C H 0.6452 -0.0849 0.6544 0.057 Uiso 1 1 calc R . . C32 C 0.28661(18) -0.1152(2) 0.50129(12) 0.0245(5) Uani 1 1 d . . . C33 C 0.21187(19) -0.2115(3) 0.50603(14) 0.0305(6) Uani 1 1 d . . . H33A H 0.248 -0.2795 0.5387 0.046 Uiso 1 1 calc R . . H33B H 0.1729 -0.242 0.4542 0.046 Uiso 1 1 calc R . . H33C H 0.1669 -0.1745 0.5283 0.046 Uiso 1 1 calc R . . C34 C 0.2329(2) -0.0188(3) 0.44005(14) 0.0357(7) Uani 1 1 d . . . H34A H 0.1801 0.0198 0.4532 0.054 Uiso 1 1 calc R . . H34B H 0.2035 -0.0583 0.3895 0.054 Uiso 1 1 calc R . . H34C H 0.2809 0.0434 0.4384 0.054 Uiso 1 1 calc R . . C35 C 0.3621(2) -0.1809(3) 0.47464(15) 0.0380(7) Uani 1 1 d . . . H35A H 0.4111 -0.1219 0.471 0.057 Uiso 1 1 calc R . . H35B H 0.327 -0.2182 0.424 0.057 Uiso 1 1 calc R . . H35C H 0.3963 -0.2447 0.512 0.057 Uiso 1 1 calc R . . O36 O 0.18187(12) 0.03348(15) 0.57619(9) 0.0221(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.01487(9) 0.02055(10) 0.02009(9) 0.00190(6) 0.00319(6) 0.00273(6) Cl2 0.0287(3) 0.0223(3) 0.0288(3) -0.0012(2) 0.0036(2) -0.0034(2) N1 0.0180(9) 0.0125(9) 0.0182(9) 0.0001(7) 0.0075(7) 0.0006(7) C2 0.0187(11) 0.0140(12) 0.0201(10) 0.0007(9) 0.0068(9) 0.0006(8) C3 0.0248(12) 0.0191(13) 0.0204(11) 0.0014(9) 0.0038(9) 0.0002(9) O4 0.0341(10) 0.0210(9) 0.0190(8) 0.0024(7) 0.0053(7) 0.0073(7) C5 0.0245(12) 0.0289(15) 0.0201(11) 0.0048(10) 0.0019(9) 0.0003(10) C6 0.0356(14) 0.0291(16) 0.0298(13) 0.0090(11) 0.0116(11) 0.0049(11) O7 0.0339(11) 0.0393(12) 0.0445(11) 0.0085(9) 0.0203(9) 0.0036(8) C8 0.0393(17) 0.070(2) 0.0426(16) 0.0232(16) 0.0220(14) 0.0093(16) C9 0.0408(17) 0.053(2) 0.0512(18) 0.0230(16) 0.0130(14) -0.0075(15) O10 0.0364(11) 0.0564(15) 0.0358(11) 0.0122(10) 0.0042(9) -0.0121(10) C11 0.0286(14) 0.0454(19) 0.0470(17) 0.0089(14) 0.0115(13) -0.0077(13) C12 0.0175(12) 0.0447(18) 0.0338(14) 0.0071(12) 0.0073(10) -0.0053(11) O13 0.0216(9) 0.0337(11) 0.0255(8) -0.0010(7) 0.0082(7) -0.0051(7) C14 0.0221(12) 0.0227(14) 0.0268(12) -0.0037(10) 0.0116(10) 0.0003(9) C15 0.0235(11) 0.0152(12) 0.0259(11) -0.0034(9) 0.0110(9) 0.0006(9) C21 0.0194(11) 0.0164(12) 0.0214(10) 0.0013(9) 0.0089(9) -0.0023(9) C22 0.0172(11) 0.0198(13) 0.0179(10) 0.0025(9) 0.0072(8) -0.0005(8) C23 0.0185(11) 0.0248(14) 0.0179(10) 0.0008(9) 0.0053(9) -0.0039(9) C24 0.0171(11) 0.0250(13) 0.0222(11) 0.0066(10) 0.0074(9) -0.0004(9) C25 0.0227(12) 0.0246(14) 0.0225(11) 0.0058(9) 0.0125(9) 0.0048(9) C26 0.0234(12) 0.0230(13) 0.0158(10) 0.0044(9) 0.0084(9) 0.0027(9) C27 0.0180(11) 0.0196(12) 0.0186(10) 0.0044(9) 0.0062(9) 0.0006(9) C28 0.0161(11) 0.0335(15) 0.0303(13) 0.0093(11) 0.0066(10) 0.0015(10) C29 0.0235(13) 0.059(2) 0.0322(14) 0.0193(14) 0.0022(11) 0.0018(13) C30 0.0218(13) 0.0432(18) 0.0477(17) 0.0048(14) 0.0088(12) -0.0033(12) C31 0.0204(13) 0.0443(18) 0.0510(17) 0.0052(14) 0.0144(12) 0.0064(12) C32 0.0250(12) 0.0322(15) 0.0155(10) 0.0006(10) 0.0065(9) 0.0071(10) C33 0.0340(14) 0.0327(16) 0.0215(11) -0.0077(11) 0.0067(10) 0.0003(11) C34 0.0434(16) 0.0454(18) 0.0182(12) 0.0075(12) 0.0112(11) 0.0116(13) C35 0.0419(16) 0.0504(19) 0.0254(12) -0.0043(12) 0.0167(12) 0.0106(14) O36 0.0179(8) 0.0280(10) 0.0178(7) -0.0002(7) 0.0038(6) 0.0028(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 O36 2.0716(16) . ? Sn1 N1 2.3568(17) . ? Sn1 Cl2 2.4676(7) . ? N1 C2 1.487(3) . ? N1 C15 1.498(3) . ? N1 C21 1.504(3) . ? C2 C3 1.527(3) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? C3 O4 1.427(3) . ? C3 H3A 0.99 . ? C3 H3B 0.99 . ? O4 C5 1.432(3) . ? C5 C6 1.500(3) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? C6 O7 1.427(3) . ? C6 H6A 0.99 . ? C6 H6B 0.99 . ? O7 C8 1.416(3) . ? C8 C9 1.456(4) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? C9 O10 1.451(4) . ? C9 H9A 0.99 . ? C9 H9B 0.99 . ? O10 C11 1.391(3) . ? C11 C12 1.491(4) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? C12 O13 1.431(3) . ? C12 H12A 0.99 . ? C12 H12B 0.99 . ? O13 C14 1.431(3) . ? C14 C15 1.511(3) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? C15 H15A 0.99 . ? C15 H15B 0.99 . ? C21 C22 1.496(3) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 C23 1.399(3) . ? C22 C27 1.406(3) . ? C23 C24 1.389(3) . ? C23 H23 0.95 . ? C24 C25 1.397(3) . ? C24 C28 1.534(3) . ? C25 C26 1.405(3) . ? C25 H25 0.95 . ? C26 C27 1.412(3) . ? C26 C32 1.535(3) . ? C27 O36 1.352(3) . ? C28 C31 1.533(4) . ? C28 C29 1.536(4) . ? C28 C30 1.539(4) . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C30 H30A 0.98 . ? C30 H30B 0.98 . ? C30 H30C 0.98 . ? C31 H31A 0.98 . ? C31 H31B 0.98 . ? C31 H31C 0.98 . ? C32 C33 1.534(4) . ? C32 C34 1.537(3) . ? C32 C35 1.536(3) . ? C33 H33A 0.98 . ? C33 H33B 0.98 . ? C33 H33C 0.98 . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O36 Sn1 N1 86.17(6) . . ? O36 Sn1 Cl2 92.96(5) . . ? N1 Sn1 Cl2 97.50(5) . . ? C2 N1 C15 113.20(17) . . ? C2 N1 C21 112.18(17) . . ? C15 N1 C21 107.38(17) . . ? C2 N1 Sn1 116.54(13) . . ? C15 N1 Sn1 104.51(12) . . ? C21 N1 Sn1 102.00(12) . . ? N1 C2 C3 115.55(19) . . ? N1 C2 H2A 108.4 . . ? C3 C2 H2A 108.4 . . ? N1 C2 H2B 108.4 . . ? C3 C2 H2B 108.4 . . ? H2A C2 H2B 107.5 . . ? O4 C3 C2 105.63(18) . . ? O4 C3 H3A 110.6 . . ? C2 C3 H3A 110.6 . . ? O4 C3 H3B 110.6 . . ? C2 C3 H3B 110.6 . . ? H3A C3 H3B 108.7 . . ? C3 O4 C5 114.63(18) . . ? O4 C5 C6 112.0(2) . . ? O4 C5 H5A 109.2 . . ? C6 C5 H5A 109.2 . . ? O4 C5 H5B 109.2 . . ? C6 C5 H5B 109.2 . . ? H5A C5 H5B 107.9 . . ? O7 C6 C5 109.0(2) . . ? O7 C6 H6A 109.9 . . ? C5 C6 H6A 109.9 . . ? O7 C6 H6B 109.9 . . ? C5 C6 H6B 109.9 . . ? H6A C6 H6B 108.3 . . ? C8 O7 C6 112.5(2) . . ? O7 C8 C9 112.2(2) . . ? O7 C8 H8A 109.2 . . ? C9 C8 H8A 109.2 . . ? O7 C8 H8B 109.2 . . ? C9 C8 H8B 109.2 . . ? H8A C8 H8B 107.9 . . ? O10 C9 C8 107.5(3) . . ? O10 C9 H9A 110.2 . . ? C8 C9 H9A 110.2 . . ? O10 C9 H9B 110.2 . . ? C8 C9 H9B 110.2 . . ? H9A C9 H9B 108.5 . . ? C11 O10 C9 112.4(2) . . ? O10 C11 C12 110.4(3) . . ? O10 C11 H11A 109.6 . . ? C12 C11 H11A 109.6 . . ? O10 C11 H11B 109.6 . . ? C12 C11 H11B 109.6 . . ? H11A C11 H11B 108.1 . . ? O13 C12 C11 114.8(2) . . ? O13 C12 H12A 108.6 . . ? C11 C12 H12A 108.6 . . ? O13 C12 H12B 108.6 . . ? C11 C12 H12B 108.6 . . ? H12A C12 H12B 107.6 . . ? C12 O13 C14 114.08(18) . . ? O13 C14 C15 107.48(18) . . ? O13 C14 H14A 110.2 . . ? C15 C14 H14A 110.2 . . ? O13 C14 H14B 110.2 . . ? C15 C14 H14B 110.2 . . ? H14A C14 H14B 108.5 . . ? N1 C15 C14 112.79(19) . . ? N1 C15 H15A 109 . . ? C14 C15 H15A 109 . . ? N1 C15 H15B 109 . . ? C14 C15 H15B 109 . . ? H15A C15 H15B 107.8 . . ? C22 C21 N1 113.58(18) . . ? C22 C21 H21A 108.8 . . ? N1 C21 H21A 108.8 . . ? C22 C21 H21B 108.8 . . ? N1 C21 H21B 108.8 . . ? H21A C21 H21B 107.7 . . ? C23 C22 C27 120.2(2) . . ? C23 C22 C21 119.8(2) . . ? C27 C22 C21 119.92(19) . . ? C24 C23 C22 121.8(2) . . ? C24 C23 H23 119.1 . . ? C22 C23 H23 119.1 . . ? C23 C24 C25 116.7(2) . . ? C23 C24 C28 119.9(2) . . ? C25 C24 C28 123.4(2) . . ? C24 C25 C26 124.2(2) . . ? C24 C25 H25 117.9 . . ? C26 C25 H25 117.9 . . ? C25 C26 C27 117.2(2) . . ? C25 C26 C32 121.6(2) . . ? C27 C26 C32 121.1(2) . . ? O36 C27 C22 118.9(2) . . ? O36 C27 C26 121.3(2) . . ? C22 C27 C26 119.8(2) . . ? C31 C28 C24 112.5(2) . . ? C31 C28 C29 107.7(2) . . ? C24 C28 C29 108.9(2) . . ? C31 C28 C30 108.7(2) . . ? C24 C28 C30 110.0(2) . . ? C29 C28 C30 109.0(2) . . ? C28 C29 H29A 109.5 . . ? C28 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C28 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C28 C30 H30A 109.5 . . ? C28 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C28 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C28 C31 H31A 109.5 . . ? C28 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C28 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C33 C32 C26 109.57(19) . . ? C33 C32 C34 110.1(2) . . ? C26 C32 C34 110.0(2) . . ? C33 C32 C35 107.3(2) . . ? C26 C32 C35 112.2(2) . . ? C34 C32 C35 107.6(2) . . ? C32 C33 H33A 109.5 . . ? C32 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? C32 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C32 C34 H34A 109.5 . . ? C32 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? C32 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? C32 C35 H35A 109.5 . . ? C32 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C32 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C27 O36 Sn1 131.98(14) . . ? 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 O36 Sn1 N1 C2 -87.07(15) . . . . ? Cl2 Sn1 N1 C2 5.42(14) . . . . ? O36 Sn1 N1 C15 147.19(14) . . . . ? Cl2 Sn1 N1 C15 -120.32(13) . . . . ? O36 Sn1 N1 C21 35.45(13) . . . . ? Cl2 Sn1 N1 C21 127.94(12) . . . . ? C15 N1 C2 C3 -56.1(2) . . . . ? C21 N1 C2 C3 65.6(2) . . . . ? Sn1 N1 C2 C3 -177.38(15) . . . . ? N1 C2 C3 O4 -168.74(18) . . . . ? C2 C3 O4 C5 -152.38(19) . . . . ? C3 O4 C5 C6 96.0(3) . . . . ? O4 C5 C6 O7 -73.8(3) . . . . ? C5 C6 O7 C8 169.0(2) . . . . ? C6 O7 C8 C9 -88.8(3) . . . . ? O7 C8 C9 O10 -69.1(3) . . . . ? C8 C9 O10 C11 170.6(2) . . . . ? C9 O10 C11 C12 -176.7(2) . . . . ? O10 C11 C12 O13 72.9(3) . . . . ? C11 C12 O13 C14 -74.6(3) . . . . ? C12 O13 C14 C15 177.0(2) . . . . ? C2 N1 C15 C14 -49.5(2) . . . . ? C21 N1 C15 C14 -173.86(18) . . . . ? Sn1 N1 C15 C14 78.33(18) . . . . ? O13 C14 C15 N1 -51.2(2) . . . . ? C2 N1 C21 C22 49.5(2) . . . . ? C15 N1 C21 C22 174.47(17) . . . . ? Sn1 N1 C21 C22 -75.96(18) . . . . ? N1 C21 C22 C23 -115.5(2) . . . . ? N1 C21 C22 C27 66.6(3) . . . . ? C27 C22 C23 C24 0.5(3) . . . . ? C21 C22 C23 C24 -177.4(2) . . . . ? C22 C23 C24 C25 2.8(3) . . . . ? C22 C23 C24 C28 -176.6(2) . . . . ? C23 C24 C25 C26 -3.7(3) . . . . ? C28 C24 C25 C26 175.7(2) . . . . ? C24 C25 C26 C27 1.1(3) . . . . ? C24 C25 C26 C32 -178.8(2) . . . . ? C23 C22 C27 O36 179.1(2) . . . . ? C21 C22 C27 O36 -3.0(3) . . . . ? C23 C22 C27 C26 -3.1(3) . . . . ? C21 C22 C27 C26 174.8(2) . . . . ? C25 C26 C27 O36 -180.0(2) . . . . ? C32 C26 C27 O36 0.0(3) . . . . ? C25 C26 C27 C22 2.3(3) . . . . ? C32 C26 C27 C22 -177.7(2) . . . . ? C23 C24 C28 C31 178.3(2) . . . . ? C25 C24 C28 C31 -1.0(3) . . . . ? C23 C24 C28 C29 59.0(3) . . . . ? C25 C24 C28 C29 -120.3(3) . . . . ? C23 C24 C28 C30 -60.3(3) . . . . ? C25 C24 C28 C30 120.3(3) . . . . ? C25 C26 C32 C33 115.5(2) . . . . ? C27 C26 C32 C33 -64.4(3) . . . . ? C25 C26 C32 C34 -123.3(2) . . . . ? C27 C26 C32 C34 56.7(3) . . . . ? C25 C26 C32 C35 -3.6(3) . . . . ? C27 C26 C32 C35 176.4(2) . . . . ? C22 C27 O36 Sn1 -32.8(3) . . . . ? C26 C27 O36 Sn1 149.40(17) . . . . ? N1 Sn1 O36 C27 13.1(2) . . . . ? Cl2 Sn1 O36 C27 -84.2(2) . . . . ? #----------------------------------------------------------------------------# # END OF CIF FILE FOR WLF021 # #----------------------------------------------------------------------------# _database_code_depnum_ccdc_archive 'CCDC 942097' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_WLF020 _audit_creation_date 2013-04-05T17:48:50-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C32 H60 F3 Li N2 O8 S Si2 Sn' _chemical_formula_sum 'C32 H60 F3 Li N2 O8 S Si2 Sn' _chemical_formula_weight 871.69 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.8219(2) _cell_length_b 11.8940(2) _cell_length_c 21.6592(3) _cell_angle_alpha 74.5550(10) _cell_angle_beta 78.5080(10) _cell_angle_gamma 80.5870(10) _cell_volume 2131.92(7) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 8648 _cell_measurement_theta_min 2.24 _cell_measurement_theta_max 27.47 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description fragment _exptl_crystal_colour colourless _exptl_crystal_size_max 0.35 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_diffrn 1.358 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 908 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.762 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.845 _exptl_absorpt_correction_T_max 0.913 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0329 _diffrn_reflns_av_unetI/netI 0.0475 _diffrn_reflns_number 22861 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -24 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 2.92 _diffrn_reflns_theta_max 27.48 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.988 _diffrn_measured_fraction_theta_max 0.988 _reflns_number_total 9691 _reflns_number_gt 8442 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 2012), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0315P)^2^+0.4753P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 9691 _refine_ls_number_parameters 463 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0397 _refine_ls_R_factor_gt 0.0324 _refine_ls_wR_factor_ref 0.0742 _refine_ls_wR_factor_gt 0.0706 _refine_ls_goodness_of_fit_ref 1.023 _refine_ls_restrained_S_all 1.023 _refine_ls_shift/su_max 0.037 _refine_ls_shift/su_mean 0.001 _refine_diff_density_max 0.439 _refine_diff_density_min -0.355 _refine_diff_density_rms 0.072 _iucr_refine_instructions_details ; .res file for SHELXL : WLF020.res ................................................................. TITL import in P -1 CELL 0.71073 8.8219 11.8940 21.6592 74.555 78.508 80.587 ZERR 2.00 0.0002 0.0002 0.0003 0.001 0.001 0.001 LATT 1 SFAC C H O CL SN SI S F N LI UNIT 64.00 120.00 16.00 0.00 2.00 4.00 2.00 6.00 4.00 2.00 MERG 2 FMAP 2 PLAN 20 ACTA BOND $H CONF LIST 4 WPDB -2 L.S. 4 TEMP -123.00 WGHT 0.031500 0.475300 FVAR 0.50890 SN1 5 0.297335 0.080748 0.647905 11.00000 0.01702 0.02023 = 0.01586 -0.00390 -0.00204 -0.00096 SI1 6 0.682211 0.103987 0.625825 11.00000 0.01907 0.02638 = 0.02783 -0.00752 -0.00091 -0.00315 SI2 6 0.579486 -0.121615 0.618106 11.00000 0.02776 0.02090 = 0.02508 -0.00889 -0.00021 0.00090 LI 10 0.093728 -0.296345 0.887155 11.00000 0.01922 0.02711 = 0.02725 -0.00576 -0.00345 -0.00025 C1 1 0.363363 -0.088991 0.789413 11.00000 0.01506 0.02045 = 0.02085 -0.00204 -0.00133 -0.00211 AFIX 23 H1A 2 0.463970 -0.061947 0.765575 11.00000 -1.20000 H1B 2 0.351601 -0.159569 0.775578 11.00000 -1.20000 AFIX 0 C2 1 0.375248 -0.126736 0.860855 11.00000 0.01622 0.02323 = 0.02140 0.00107 -0.00440 -0.00334 AFIX 23 H2A 2 0.468925 -0.184235 0.867245 11.00000 -1.20000 H2B 2 0.387301 -0.057638 0.875987 11.00000 -1.20000 AFIX 0 O3 3 0.239594 -0.178813 0.898984 11.00000 0.01770 0.02769 = 0.01693 0.00035 -0.00293 -0.00471 C4 1 0.262229 -0.231028 0.965239 11.00000 0.02260 0.03123 = 0.01563 -0.00245 -0.00337 -0.00283 AFIX 23 H4A 2 0.161847 -0.224368 0.994872 11.00000 -1.20000 H4B 2 0.335995 -0.189073 0.977122 11.00000 -1.20000 AFIX 0 C5 1 0.325540 -0.357964 0.972055 11.00000 0.02211 0.03296 = 0.02400 0.00132 -0.00729 -0.00171 AFIX 23 H5A 2 0.427349 -0.365756 0.943482 11.00000 -1.20000 H5B 2 0.339340 -0.395887 1.017491 11.00000 -1.20000 AFIX 0 O6 3 0.213105 -0.410305 0.953358 11.00000 0.02164 0.02361 = 0.03172 -0.00110 -0.00458 -0.00147 C7 1 0.266955 -0.520851 0.937961 11.00000 0.03176 0.02193 = 0.04566 -0.00265 -0.00597 0.00327 AFIX 23 H7A 2 0.296173 -0.580434 0.976624 11.00000 -1.20000 H7B 2 0.358828 -0.514126 0.903040 11.00000 -1.20000 AFIX 0 C8 1 0.132668 -0.554404 0.915744 11.00000 0.03612 0.01914 = 0.04068 -0.00055 -0.00198 -0.00334 AFIX 23 H8A 2 0.168490 -0.623081 0.896708 11.00000 -1.20000 H8B 2 0.049700 -0.576477 0.953373 11.00000 -1.20000 AFIX 0 O9 3 0.072008 -0.457769 0.868343 11.00000 0.02820 0.02343 = 0.02996 -0.00303 -0.00041 -0.00335 C10 1 0.148671 -0.450812 0.802672 11.00000 0.03854 0.02666 = 0.03479 -0.01318 0.00204 -0.00753 AFIX 23 H10A 2 0.127841 -0.516933 0.787067 11.00000 -1.20000 H10B 2 0.262623 -0.453436 0.799589 11.00000 -1.20000 AFIX 0 C11 1 0.083178 -0.336319 0.763479 11.00000 0.04059 0.02923 = 0.02779 -0.01028 -0.00205 -0.01445 AFIX 23 H11A 2 0.130223 -0.326194 0.717139 11.00000 -1.20000 H11B 2 -0.030970 -0.333699 0.767232 11.00000 -1.20000 AFIX 0 O12 3 0.118794 -0.245120 0.788356 11.00000 0.02467 0.02116 = 0.02353 -0.00596 -0.00405 -0.00578 C13 1 0.052789 -0.131343 0.755736 11.00000 0.02091 0.02732 = 0.02178 -0.00198 -0.00567 -0.00590 AFIX 23 H13A 2 -0.060466 -0.131766 0.758402 11.00000 -1.20000 H13B 2 0.100322 -0.114472 0.709288 11.00000 -1.20000 AFIX 0 C14 1 0.078922 -0.035835 0.785056 11.00000 0.01561 0.02224 = 0.02048 0.00006 -0.00265 -0.00162 AFIX 23 H14A 2 0.002298 0.033200 0.772229 11.00000 -1.20000 H14B 2 0.055859 -0.063773 0.832894 11.00000 -1.20000 AFIX 0 N15 9 0.237365 0.004168 0.767561 11.00000 0.01569 0.01729 = 0.01720 -0.00242 -0.00215 -0.00096 C16 1 0.231903 0.107314 0.795507 11.00000 0.02040 0.02029 = 0.01756 -0.00367 -0.00260 -0.00190 AFIX 23 H16A 2 0.339012 0.127777 0.789812 11.00000 -1.20000 H16B 2 0.192477 0.084920 0.842693 11.00000 -1.20000 AFIX 0 C17 1 0.130339 0.213948 0.764768 11.00000 0.02133 0.01956 = 0.01810 -0.00446 -0.00361 -0.00101 C18 1 -0.016185 0.247136 0.797373 11.00000 0.02666 0.02136 = 0.01972 -0.00547 0.00049 -0.00179 AFIX 43 H18 2 -0.052155 0.201946 0.839538 11.00000 -1.20000 AFIX 0 C19 1 -0.110565 0.345288 0.769202 11.00000 0.02180 0.02378 = 0.02239 -0.00909 -0.00083 -0.00083 C20 1 -0.047952 0.412278 0.708922 11.00000 0.02729 0.01967 = 0.02519 -0.00720 -0.00456 0.00440 AFIX 43 H20 2 -0.108865 0.481974 0.690198 11.00000 -1.20000 AFIX 0 C21 1 0.098349 0.383648 0.674291 11.00000 0.02781 0.01763 = 0.01734 -0.00425 -0.00327 -0.00106 C22 1 0.186330 0.278263 0.702478 11.00000 0.02025 0.01969 = 0.01847 -0.00592 -0.00205 -0.00298 C23 1 -0.276105 0.382217 0.802540 11.00000 0.02052 0.02696 = 0.03501 -0.01146 0.00244 0.00312 C24 1 -0.336646 0.280893 0.857849 11.00000 0.02859 0.03622 = 0.04355 -0.00867 0.01332 -0.00072 AFIX 137 H24A 2 -0.269234 0.260155 0.891074 11.00000 -1.50000 H24B 2 -0.336219 0.212545 0.840609 11.00000 -1.50000 H24C 2 -0.443112 0.305333 0.877151 11.00000 -1.50000 AFIX 0 C25 1 -0.389188 0.417535 0.753619 11.00000 0.02397 0.04380 = 0.05297 -0.01292 -0.00506 0.00699 AFIX 137 H25A 2 -0.495043 0.434539 0.776155 11.00000 -1.50000 H25B 2 -0.385933 0.353032 0.732951 11.00000 -1.50000 H25C 2 -0.359013 0.487653 0.720419 11.00000 -1.50000 AFIX 0 C26 1 -0.271248 0.487273 0.829866 11.00000 0.02743 0.03862 = 0.05002 -0.02113 0.01075 -0.00418 AFIX 137 H26A 2 -0.200134 0.465060 0.861715 11.00000 -1.50000 H26B 2 -0.375932 0.511671 0.850943 11.00000 -1.50000 H26C 2 -0.234563 0.552463 0.794466 11.00000 -1.50000 AFIX 0 C27 1 0.162766 0.464046 0.608869 11.00000 0.03526 0.01973 = 0.01847 -0.00170 0.00017 0.00050 C28 1 0.051230 0.576715 0.590552 11.00000 0.05415 0.02755 = 0.02555 0.00409 0.00165 0.00819 AFIX 137 H28A 2 0.034643 0.619951 0.624499 11.00000 -1.50000 H28B 2 -0.048672 0.556093 0.586303 11.00000 -1.50000 H28C 2 0.096604 0.625936 0.549175 11.00000 -1.50000 AFIX 0 C29 1 0.317379 0.499771 0.613947 11.00000 0.04083 0.02456 = 0.03259 -0.00429 0.00600 -0.00972 AFIX 137 H29A 2 0.389963 0.429216 0.626521 11.00000 -1.50000 H29B 2 0.300080 0.545552 0.646754 11.00000 -1.50000 H29C 2 0.361414 0.547493 0.571829 11.00000 -1.50000 AFIX 0 C30 1 0.185950 0.400650 0.553950 11.00000 0.04953 0.03332 = 0.01892 -0.00469 -0.00308 0.00000 AFIX 137 H30A 2 0.216044 0.455530 0.512217 11.00000 -1.50000 H30B 2 0.088500 0.371419 0.553718 11.00000 -1.50000 H30C 2 0.268111 0.334521 0.560849 11.00000 -1.50000 AFIX 0 O31 3 0.324071 0.235469 0.670735 11.00000 0.01850 0.01867 = 0.02115 -0.00462 0.00238 -0.00069 N32 9 0.536506 0.017179 0.632350 11.00000 0.01879 0.02042 = 0.01973 -0.00614 -0.00115 0.00142 C33 1 0.696630 0.122521 0.707044 11.00000 0.03608 0.04481 = 0.04423 -0.01988 -0.00831 -0.01216 AFIX 137 H33A 2 0.598477 0.163068 0.724843 11.00000 -1.50000 H33B 2 0.781821 0.169032 0.702768 11.00000 -1.50000 H33C 2 0.717185 0.045221 0.736286 11.00000 -1.50000 AFIX 0 C34 1 0.647221 0.250113 0.569329 11.00000 0.03370 0.03509 = 0.05043 0.00428 0.00698 -0.00945 AFIX 137 H34A 2 0.651039 0.240039 0.525566 11.00000 -1.50000 H34B 2 0.727655 0.298565 0.568606 11.00000 -1.50000 H34C 2 0.544522 0.288770 0.584030 11.00000 -1.50000 AFIX 0 C35 1 0.880088 0.041559 0.590645 11.00000 0.01955 0.05657 = 0.06318 -0.02793 -0.00105 -0.00370 AFIX 137 H35A 2 0.904274 -0.038960 0.615751 11.00000 -1.50000 H35B 2 0.958335 0.089862 0.592441 11.00000 -1.50000 H35C 2 0.880916 0.041197 0.545386 11.00000 -1.50000 AFIX 0 C36 1 0.679251 -0.125113 0.533767 11.00000 0.04503 0.04597 = 0.03490 -0.02122 0.00160 -0.00035 AFIX 137 H36A 2 0.617812 -0.072047 0.502391 11.00000 -1.50000 H36B 2 0.689172 -0.205248 0.528198 11.00000 -1.50000 H36C 2 0.783021 -0.099877 0.526540 11.00000 -1.50000 AFIX 0 C37 1 0.699854 -0.222749 0.677037 11.00000 0.05559 0.03356 = 0.04058 -0.00423 -0.00909 0.01596 AFIX 137 H37A 2 0.802416 -0.195606 0.669980 11.00000 -1.50000 H37B 2 0.712488 -0.302379 0.670482 11.00000 -1.50000 H37C 2 0.647636 -0.223178 0.721483 11.00000 -1.50000 AFIX 0 C38 1 0.397564 -0.192010 0.628970 11.00000 0.04365 0.03216 = 0.05470 -0.02327 0.00532 -0.01287 AFIX 137 H38A 2 0.344656 -0.201870 0.674053 11.00000 -1.50000 H38B 2 0.424666 -0.268976 0.618695 11.00000 -1.50000 H38C 2 0.328295 -0.141975 0.599838 11.00000 -1.50000 AFIX 0 C41 1 -0.223951 -0.062183 0.971550 11.00000 0.04822 0.04270 = 0.05128 -0.02049 0.01485 -0.01268 F42 8 -0.347700 0.017384 0.971002 11.00000 0.06462 0.04796 = 0.16858 -0.05473 0.04150 -0.00436 F43 8 -0.208898 -0.111149 1.032906 11.00000 0.14312 0.10758 = 0.03893 -0.03538 0.01261 -0.06588 F44 8 -0.100510 -0.005171 0.944163 11.00000 0.05738 0.05286 = 0.07030 -0.02790 0.01318 -0.03097 S1 7 -0.243127 -0.171107 0.929906 11.00000 0.01531 0.02718 = 0.02755 -0.00311 -0.00128 -0.00218 O45 3 -0.097647 -0.246590 0.935133 11.00000 0.01764 0.03422 = 0.04365 -0.01098 -0.00109 0.00278 O46 3 -0.258040 -0.104646 0.865460 11.00000 0.03093 0.06536 = 0.03476 0.01080 -0.00855 -0.01471 O47 3 -0.376864 -0.225449 0.967556 11.00000 0.01754 0.03324 = 0.04004 0.00415 -0.00091 -0.00502 HKLF 4 REM import in P -1 REM R1 = 0.0324 for 8442 Fo > 4sig(Fo) and 0.0397 for all 9691 data REM 463 parameters refined using 0 restraints END WGHT 0.0295 0.5446 REM Highest difference peak 0.44, deepest hole -0.35, 1-sigma level 0.07 Q1 1 0.2883 0.0449 0.6126 11.00000 0.05 0.44 Q2 1 0.1416 0.3248 0.6804 11.00000 0.05 0.41 Q3 1 0.6375 -0.1775 0.6479 11.00000 0.05 0.41 Q4 1 0.2984 0.0161 0.6256 11.00000 0.05 0.41 Q5 1 -0.2481 -0.1014 0.9506 11.00000 0.05 0.40 Q6 1 0.4889 -0.1448 0.6085 11.00000 0.05 0.37 Q7 1 0.1338 0.4250 0.6431 11.00000 0.05 0.37 Q8 1 -0.2010 0.3540 0.7851 11.00000 0.05 0.36 Q9 1 0.6415 0.1743 0.5951 11.00000 0.05 0.36 Q10 1 0.1809 0.1717 0.7823 11.00000 0.05 0.36 Q11 1 0.2373 0.1543 0.6444 11.00000 0.05 0.35 Q12 1 0.0985 0.5107 0.6002 11.00000 0.05 0.35 Q13 1 0.5290 -0.0546 0.6333 11.00000 0.05 0.35 Q14 1 0.1505 0.2308 0.7303 11.00000 0.05 0.34 Q15 1 0.2780 -0.3007 0.9769 11.00000 0.05 0.34 Q16 1 -0.0499 0.3116 0.7889 11.00000 0.05 0.34 Q17 1 0.3066 0.1213 0.6809 11.00000 0.05 0.34 Q18 1 0.1835 0.0775 0.6468 11.00000 0.05 0.33 Q19 1 0.6473 -0.1148 0.5708 11.00000 0.05 0.33 Q20 1 -0.3665 0.0415 0.9623 11.00000 0.05 0.32 ; # End of res file #----------------------------------------------------------------------------# #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 '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' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' F F 0.0171 0.0103 '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' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.297335(16) 0.080748(13) 0.647905(7) 0.01803(5) Uani 1 1 d . . . Si1 Si 0.68221(7) 0.10399(6) 0.62582(3) 0.02460(14) Uani 1 1 d . . . Si2 Si 0.57949(7) -0.12162(6) 0.61811(3) 0.02496(14) Uani 1 1 d . . . Li Li 0.0937(4) -0.2963(4) 0.88716(18) 0.0250(8) Uani 1 1 d . . . C1 C 0.3634(2) -0.08899(19) 0.78941(10) 0.0196(4) Uani 1 1 d . . . H1A H 0.464 -0.0619 0.7656 0.024 Uiso 1 1 calc R . . H1B H 0.3516 -0.1596 0.7756 0.024 Uiso 1 1 calc R . . C2 C 0.3752(2) -0.1267(2) 0.86085(10) 0.0212(5) Uani 1 1 d . . . H2A H 0.4689 -0.1842 0.8672 0.025 Uiso 1 1 calc R . . H2B H 0.3873 -0.0576 0.876 0.025 Uiso 1 1 calc R . . O3 O 0.23959(16) -0.17881(14) 0.89898(7) 0.0216(3) Uani 1 1 d . . . C4 C 0.2622(3) -0.2310(2) 0.96524(10) 0.0238(5) Uani 1 1 d . . . H4A H 0.1618 -0.2244 0.9949 0.029 Uiso 1 1 calc R . . H4B H 0.336 -0.1891 0.9771 0.029 Uiso 1 1 calc R . . C5 C 0.3255(3) -0.3580(2) 0.97206(11) 0.0276(5) Uani 1 1 d . . . H5A H 0.4273 -0.3658 0.9435 0.033 Uiso 1 1 calc R . . H5B H 0.3393 -0.3959 1.0175 0.033 Uiso 1 1 calc R . . O6 O 0.21310(17) -0.41031(14) 0.95336(8) 0.0269(4) Uani 1 1 d . . . C7 C 0.2670(3) -0.5209(2) 0.93796(13) 0.0350(6) Uani 1 1 d . . . H7A H 0.2962 -0.5804 0.9766 0.042 Uiso 1 1 calc R . . H7B H 0.3588 -0.5141 0.903 0.042 Uiso 1 1 calc R . . C8 C 0.1327(3) -0.5544(2) 0.91574(13) 0.0339(6) Uani 1 1 d . . . H8A H 0.1685 -0.6231 0.8967 0.041 Uiso 1 1 calc R . . H8B H 0.0497 -0.5765 0.9534 0.041 Uiso 1 1 calc R . . O9 O 0.07201(18) -0.45777(14) 0.86834(7) 0.0285(4) Uani 1 1 d . . . C10 C 0.1487(3) -0.4508(2) 0.80267(12) 0.0329(6) Uani 1 1 d . . . H10A H 0.1278 -0.5169 0.7871 0.04 Uiso 1 1 calc R . . H10B H 0.2626 -0.4534 0.7996 0.04 Uiso 1 1 calc R . . C11 C 0.0832(3) -0.3363(2) 0.76348(11) 0.0312(6) Uani 1 1 d . . . H11A H 0.1302 -0.3262 0.7171 0.037 Uiso 1 1 calc R . . H11B H -0.031 -0.3337 0.7672 0.037 Uiso 1 1 calc R . . O12 O 0.11879(17) -0.24512(13) 0.78836(7) 0.0226(3) Uani 1 1 d . . . C13 C 0.0528(3) -0.1313(2) 0.75574(10) 0.0234(5) Uani 1 1 d . . . H13A H -0.0605 -0.1318 0.7584 0.028 Uiso 1 1 calc R . . H13B H 0.1003 -0.1145 0.7093 0.028 Uiso 1 1 calc R . . C14 C 0.0789(2) -0.03583(19) 0.78506(10) 0.0206(4) Uani 1 1 d . . . H14A H 0.0023 0.0332 0.7722 0.025 Uiso 1 1 calc R . . H14B H 0.0559 -0.0638 0.8329 0.025 Uiso 1 1 calc R . . N15 N 0.23736(19) 0.00417(15) 0.76756(8) 0.0173(4) Uani 1 1 d . . . C16 C 0.2319(2) 0.10731(19) 0.79551(10) 0.0197(4) Uani 1 1 d . . . H16A H 0.339 0.1278 0.7898 0.024 Uiso 1 1 calc R . . H16B H 0.1925 0.0849 0.8427 0.024 Uiso 1 1 calc R . . C17 C 0.1303(2) 0.21395(19) 0.76477(10) 0.0198(4) Uani 1 1 d . . . C18 C -0.0162(3) 0.2471(2) 0.79737(11) 0.0232(5) Uani 1 1 d . . . H18 H -0.0522 0.2019 0.8395 0.028 Uiso 1 1 calc R . . C19 C -0.1106(2) 0.3453(2) 0.76920(10) 0.0226(5) Uani 1 1 d . . . C20 C -0.0480(3) 0.4123(2) 0.70892(11) 0.0245(5) Uani 1 1 d . . . H20 H -0.1089 0.482 0.6902 0.029 Uiso 1 1 calc R . . C21 C 0.0983(3) 0.38365(19) 0.67429(10) 0.0212(5) Uani 1 1 d . . . C22 C 0.1863(2) 0.27826(19) 0.70248(10) 0.0193(4) Uani 1 1 d . . . C23 C -0.2761(3) 0.3822(2) 0.80254(12) 0.0284(5) Uani 1 1 d . . . C24 C -0.3366(3) 0.2809(2) 0.85785(13) 0.0394(7) Uani 1 1 d . . . H24A H -0.2692 0.2602 0.8911 0.059 Uiso 1 1 calc R . . H24B H -0.3362 0.2125 0.8406 0.059 Uiso 1 1 calc R . . H24C H -0.4431 0.3053 0.8772 0.059 Uiso 1 1 calc R . . C25 C -0.3892(3) 0.4175(3) 0.75362(14) 0.0415(7) Uani 1 1 d . . . H25A H -0.495 0.4345 0.7762 0.062 Uiso 1 1 calc R . . H25B H -0.3859 0.353 0.733 0.062 Uiso 1 1 calc R . . H25C H -0.359 0.4877 0.7204 0.062 Uiso 1 1 calc R . . C26 C -0.2712(3) 0.4873(2) 0.82987(14) 0.0391(7) Uani 1 1 d . . . H26A H -0.2001 0.4651 0.8617 0.059 Uiso 1 1 calc R . . H26B H -0.3759 0.5117 0.8509 0.059 Uiso 1 1 calc R . . H26C H -0.2346 0.5525 0.7945 0.059 Uiso 1 1 calc R . . C27 C 0.1628(3) 0.4640(2) 0.60887(10) 0.0261(5) Uani 1 1 d . . . C28 C 0.0512(3) 0.5767(2) 0.59055(12) 0.0405(7) Uani 1 1 d . . . H28A H 0.0346 0.62 0.6245 0.061 Uiso 1 1 calc R . . H28B H -0.0487 0.5561 0.5863 0.061 Uiso 1 1 calc R . . H28C H 0.0966 0.6259 0.5492 0.061 Uiso 1 1 calc R . . C29 C 0.3174(3) 0.4998(2) 0.61395(12) 0.0342(6) Uani 1 1 d . . . H29A H 0.39 0.4292 0.6265 0.051 Uiso 1 1 calc R . . H29B H 0.3001 0.5456 0.6468 0.051 Uiso 1 1 calc R . . H29C H 0.3614 0.5475 0.5718 0.051 Uiso 1 1 calc R . . C30 C 0.1860(3) 0.4006(2) 0.55395(11) 0.0352(6) Uani 1 1 d . . . H30A H 0.216 0.4555 0.5122 0.053 Uiso 1 1 calc R . . H30B H 0.0885 0.3714 0.5537 0.053 Uiso 1 1 calc R . . H30C H 0.2681 0.3345 0.5608 0.053 Uiso 1 1 calc R . . O31 O 0.32407(16) 0.23547(13) 0.67073(7) 0.0205(3) Uani 1 1 d . . . N32 N 0.53651(19) 0.01718(16) 0.63235(8) 0.0201(4) Uani 1 1 d . . . C33 C 0.6966(3) 0.1225(3) 0.70704(13) 0.0388(6) Uani 1 1 d . . . H33A H 0.5985 0.1631 0.7248 0.058 Uiso 1 1 calc R . . H33B H 0.7818 0.169 0.7028 0.058 Uiso 1 1 calc R . . H33C H 0.7172 0.0452 0.7363 0.058 Uiso 1 1 calc R . . C34 C 0.6472(3) 0.2501(2) 0.56933(14) 0.0439(7) Uani 1 1 d . . . H34A H 0.651 0.24 0.5256 0.066 Uiso 1 1 calc R . . H34B H 0.7277 0.2986 0.5686 0.066 Uiso 1 1 calc R . . H34C H 0.5445 0.2888 0.584 0.066 Uiso 1 1 calc R . . C35 C 0.8801(3) 0.0416(3) 0.59065(15) 0.0447(7) Uani 1 1 d . . . H35A H 0.9043 -0.039 0.6158 0.067 Uiso 1 1 calc R . . H35B H 0.9583 0.0899 0.5924 0.067 Uiso 1 1 calc R . . H35C H 0.8809 0.0412 0.5454 0.067 Uiso 1 1 calc R . . C36 C 0.6793(3) -0.1251(3) 0.53377(12) 0.0415(7) Uani 1 1 d . . . H36A H 0.6178 -0.072 0.5024 0.062 Uiso 1 1 calc R . . H36B H 0.6892 -0.2052 0.5282 0.062 Uiso 1 1 calc R . . H36C H 0.783 -0.0999 0.5265 0.062 Uiso 1 1 calc R . . C37 C 0.6999(3) -0.2227(3) 0.67704(13) 0.0465(7) Uani 1 1 d . . . H37A H 0.8024 -0.1956 0.67 0.07 Uiso 1 1 calc R . . H37B H 0.7125 -0.3024 0.6705 0.07 Uiso 1 1 calc R . . H37C H 0.6476 -0.2232 0.7215 0.07 Uiso 1 1 calc R . . C38 C 0.3976(3) -0.1920(2) 0.62897(14) 0.0419(7) Uani 1 1 d . . . H38A H 0.3447 -0.2019 0.6741 0.063 Uiso 1 1 calc R . . H38B H 0.4247 -0.269 0.6187 0.063 Uiso 1 1 calc R . . H38C H 0.3283 -0.142 0.5998 0.063 Uiso 1 1 calc R . . C41 C -0.2240(3) -0.0622(3) 0.97155(15) 0.0481(8) Uani 1 1 d . . . F42 F -0.3477(2) 0.01738(18) 0.97100(13) 0.0971(9) Uani 1 1 d . . . F43 F -0.2089(3) -0.1111(2) 1.03291(9) 0.0910(8) Uani 1 1 d . . . F44 F -0.1005(2) -0.00517(16) 0.94416(9) 0.0582(5) Uani 1 1 d . . . S1 S -0.24313(6) -0.17111(5) 0.92991(3) 0.02438(13) Uani 1 1 d . . . O45 O -0.09765(17) -0.24659(15) 0.93513(8) 0.0328(4) Uani 1 1 d . . . O46 O -0.2580(2) -0.10465(19) 0.86546(9) 0.0466(5) Uani 1 1 d . . . O47 O -0.37686(17) -0.22545(15) 0.96756(8) 0.0331(4) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.01702(8) 0.02023(9) 0.01586(8) -0.00390(6) -0.00204(5) -0.00096(6) Si1 0.0191(3) 0.0264(4) 0.0278(3) -0.0075(3) -0.0009(3) -0.0031(3) Si2 0.0278(3) 0.0209(3) 0.0251(3) -0.0089(3) -0.0002(3) 0.0009(3) Li 0.0192(18) 0.027(2) 0.027(2) -0.0058(17) -0.0034(15) -0.0003(16) C1 0.0151(10) 0.0205(11) 0.0208(11) -0.0020(9) -0.0013(8) -0.0021(8) C2 0.0162(10) 0.0232(12) 0.0214(11) 0.0011(9) -0.0044(8) -0.0033(9) O3 0.0177(7) 0.0277(9) 0.0169(7) 0.0004(6) -0.0029(6) -0.0047(6) C4 0.0226(11) 0.0312(13) 0.0156(10) -0.0024(9) -0.0034(9) -0.0028(10) C5 0.0221(11) 0.0330(14) 0.0240(12) 0.0013(10) -0.0073(9) -0.0017(10) O6 0.0216(8) 0.0236(9) 0.0317(9) -0.0011(7) -0.0046(7) -0.0015(7) C7 0.0318(13) 0.0219(13) 0.0457(15) -0.0027(11) -0.0060(11) 0.0033(11) C8 0.0361(14) 0.0191(13) 0.0407(15) -0.0006(11) -0.0020(11) -0.0033(11) O9 0.0282(8) 0.0234(9) 0.0300(9) -0.0030(7) -0.0004(7) -0.0033(7) C10 0.0385(14) 0.0267(14) 0.0348(14) -0.0132(11) 0.0020(11) -0.0075(11) C11 0.0406(14) 0.0292(14) 0.0278(13) -0.0103(11) -0.0020(11) -0.0144(11) O12 0.0247(8) 0.0212(8) 0.0235(8) -0.0060(7) -0.0041(6) -0.0058(6) C13 0.0209(11) 0.0273(13) 0.0218(11) -0.0020(10) -0.0057(9) -0.0059(9) C14 0.0156(10) 0.0222(12) 0.0205(11) 0.0001(9) -0.0026(8) -0.0016(9) N15 0.0157(8) 0.0173(9) 0.0172(9) -0.0024(7) -0.0021(7) -0.0010(7) C16 0.0204(10) 0.0203(12) 0.0176(10) -0.0037(9) -0.0026(8) -0.0019(9) C17 0.0213(10) 0.0196(11) 0.0181(10) -0.0045(9) -0.0036(8) -0.0010(9) C18 0.0267(11) 0.0214(12) 0.0197(11) -0.0055(9) 0.0005(9) -0.0018(9) C19 0.0218(11) 0.0238(12) 0.0224(11) -0.0091(10) -0.0008(9) -0.0008(9) C20 0.0273(12) 0.0197(12) 0.0252(12) -0.0072(10) -0.0046(9) 0.0044(9) C21 0.0278(11) 0.0176(11) 0.0173(10) -0.0042(9) -0.0033(9) -0.0011(9) C22 0.0203(10) 0.0197(11) 0.0185(10) -0.0059(9) -0.0021(8) -0.0030(9) C23 0.0205(11) 0.0270(13) 0.0350(13) -0.0115(11) 0.0024(10) 0.0031(10) C24 0.0286(13) 0.0362(16) 0.0436(16) -0.0087(13) 0.0133(12) -0.0007(12) C25 0.0240(13) 0.0438(17) 0.0530(17) -0.0129(14) -0.0051(12) 0.0070(12) C26 0.0274(13) 0.0386(16) 0.0500(17) -0.0211(14) 0.0108(12) -0.0042(12) C27 0.0353(13) 0.0197(12) 0.0185(11) -0.0017(9) 0.0002(9) 0.0005(10) C28 0.0542(17) 0.0275(14) 0.0256(13) 0.0041(11) 0.0016(12) 0.0082(13) C29 0.0408(14) 0.0246(13) 0.0326(13) -0.0043(11) 0.0060(11) -0.0097(11) C30 0.0495(16) 0.0333(15) 0.0189(12) -0.0047(11) -0.0031(11) 0.0000(12) O31 0.0185(7) 0.0187(8) 0.0212(8) -0.0046(6) 0.0024(6) -0.0007(6) N32 0.0188(9) 0.0204(10) 0.0197(9) -0.0061(8) -0.0012(7) 0.0014(7) C33 0.0361(14) 0.0448(17) 0.0442(16) -0.0199(14) -0.0083(12) -0.0122(13) C34 0.0337(14) 0.0351(16) 0.0504(17) 0.0043(13) 0.0070(13) -0.0094(12) C35 0.0196(12) 0.057(2) 0.0632(19) -0.0279(16) -0.0011(12) -0.0037(12) C36 0.0450(16) 0.0460(18) 0.0349(15) -0.0212(13) 0.0016(12) -0.0004(13) C37 0.0556(18) 0.0336(16) 0.0406(16) -0.0042(13) -0.0091(14) 0.0160(14) C38 0.0436(16) 0.0322(15) 0.0547(18) -0.0233(14) 0.0053(13) -0.0129(12) C41 0.0482(17) 0.0427(18) 0.0513(19) -0.0205(15) 0.0149(14) -0.0127(14) F42 0.0646(13) 0.0480(13) 0.169(2) -0.0547(15) 0.0415(14) -0.0044(10) F43 0.143(2) 0.1076(19) 0.0389(11) -0.0354(12) 0.0126(12) -0.0659(16) F44 0.0574(11) 0.0529(11) 0.0703(12) -0.0279(10) 0.0132(9) -0.0310(9) S1 0.0153(2) 0.0272(3) 0.0275(3) -0.0031(2) -0.0013(2) -0.0022(2) O45 0.0176(8) 0.0342(10) 0.0436(10) -0.0110(8) -0.0011(7) 0.0028(7) O46 0.0309(9) 0.0654(14) 0.0348(10) 0.0108(10) -0.0085(8) -0.0147(9) O47 0.0175(8) 0.0332(10) 0.0400(10) 0.0041(8) -0.0009(7) -0.0050(7) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 O31 2.0880(15) . ? Sn1 N32 2.1137(17) . ? Sn1 N15 2.4860(17) . ? Si1 N32 1.7385(19) . ? Si1 C33 1.861(2) . ? Si1 C34 1.859(3) . ? Si1 C35 1.878(2) . ? Si2 N32 1.7274(18) . ? Si2 C36 1.871(2) . ? Si2 C37 1.873(3) . ? Si2 C38 1.875(3) . ? Li O45 1.893(4) . ? Li O6 2.025(4) . ? Li O12 2.040(4) . ? Li O9 2.111(4) . ? Li O3 2.142(4) . ? Li C4 2.784(4) . ? C1 N15 1.488(3) . ? C1 C2 1.512(3) . ? C1 H1A 0.99 . ? C1 H1B 0.99 . ? C2 O3 1.440(2) . ? C2 H2A 0.99 . ? C2 H2B 0.99 . ? O3 C4 1.444(2) . ? C4 C5 1.501(3) . ? C4 H4A 0.99 . ? C4 H4B 0.99 . ? C5 O6 1.425(3) . ? C5 H5A 0.99 . ? C5 H5B 0.99 . ? O6 C7 1.425(3) . ? C7 C8 1.509(4) . ? C7 H7A 0.99 . ? C7 H7B 0.99 . ? C8 O9 1.432(3) . ? C8 H8A 0.99 . ? C8 H8B 0.99 . ? O9 C10 1.435(3) . ? C10 C11 1.494(3) . ? C10 H10A 0.99 . ? C10 H10B 0.99 . ? C11 O12 1.434(3) . ? C11 H11A 0.99 . ? C11 H11B 0.99 . ? O12 C13 1.438(3) . ? C13 C14 1.508(3) . ? C13 H13A 0.99 . ? C13 H13B 0.99 . ? C14 N15 1.495(3) . ? C14 H14A 0.99 . ? C14 H14B 0.99 . ? N15 C16 1.496(3) . ? C16 C17 1.507(3) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? C17 C18 1.394(3) . ? C17 C22 1.399(3) . ? C18 C19 1.391(3) . ? C18 H18 0.95 . ? C19 C20 1.395(3) . ? C19 C23 1.545(3) . ? C20 C21 1.397(3) . ? C20 H20 0.95 . ? C21 C22 1.417(3) . ? C21 C27 1.543(3) . ? C22 O31 1.364(2) . ? C23 C26 1.528(3) . ? C23 C25 1.530(3) . ? C23 C24 1.536(4) . ? C24 H24A 0.98 . ? C24 H24B 0.98 . ? C24 H24C 0.98 . ? C25 H25A 0.98 . ? C25 H25B 0.98 . ? C25 H25C 0.98 . ? C26 H26A 0.98 . ? C26 H26B 0.98 . ? C26 H26C 0.98 . ? C27 C29 1.526(3) . ? C27 C30 1.535(3) . ? C27 C28 1.537(3) . ? C28 H28A 0.98 . ? C28 H28B 0.98 . ? C28 H28C 0.98 . ? C29 H29A 0.98 . ? C29 H29B 0.98 . ? C29 H29C 0.98 . ? C30 H30A 0.98 . ? C30 H30B 0.98 . ? C30 H30C 0.98 . ? C33 H33A 0.98 . ? C33 H33B 0.98 . ? C33 H33C 0.98 . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? C36 H36A 0.98 . ? C36 H36B 0.98 . ? C36 H36C 0.98 . ? C37 H37A 0.98 . ? C37 H37B 0.98 . ? C37 H37C 0.98 . ? C38 H38A 0.98 . ? C38 H38B 0.98 . ? C38 H38C 0.98 . ? C41 F42 1.322(3) . ? C41 F43 1.325(4) . ? C41 F44 1.329(3) . ? C41 S1 1.810(3) . ? S1 O46 1.4290(19) . ? S1 O47 1.4353(16) . ? S1 O45 1.4467(16) . ? 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 O31 Sn1 N32 96.86(6) . . ? O31 Sn1 N15 84.41(6) . . ? N32 Sn1 N15 99.47(6) . . ? N32 Si1 C33 110.49(11) . . ? N32 Si1 C34 111.37(11) . . ? C33 Si1 C34 109.95(14) . . ? N32 Si1 C35 113.42(11) . . ? C33 Si1 C35 107.22(12) . . ? C34 Si1 C35 104.14(13) . . ? N32 Si2 C36 114.50(11) . . ? N32 Si2 C37 111.81(11) . . ? C36 Si2 C37 108.62(12) . . ? N32 Si2 C38 111.06(10) . . ? C36 Si2 C38 104.64(13) . . ? C37 Si2 C38 105.60(14) . . ? O45 Li O6 105.55(19) . . ? O45 Li O12 117.6(2) . . ? O6 Li O12 136.29(19) . . ? O45 Li O9 107.82(19) . . ? O6 Li O9 79.19(15) . . ? O12 Li O9 81.14(15) . . ? O45 Li O3 100.42(18) . . ? O6 Li O3 81.44(15) . . ? O12 Li O3 96.91(17) . . ? O9 Li O3 149.11(19) . . ? O45 Li C4 91.55(15) . . ? O6 Li C4 55.34(11) . . ? O12 Li C4 126.38(18) . . ? O9 Li C4 134.10(18) . . ? O3 Li C4 30.69(8) . . ? N15 C1 C2 118.83(17) . . ? N15 C1 H1A 107.6 . . ? C2 C1 H1A 107.6 . . ? N15 C1 H1B 107.6 . . ? C2 C1 H1B 107.6 . . ? H1A C1 H1B 107 . . ? O3 C2 C1 111.61(16) . . ? O3 C2 H2A 109.3 . . ? C1 C2 H2A 109.3 . . ? O3 C2 H2B 109.3 . . ? C1 C2 H2B 109.3 . . ? H2A C2 H2B 108 . . ? C2 O3 C4 111.13(15) . . ? C2 O3 Li 135.04(16) . . ? C4 O3 Li 100.09(16) . . ? O3 C4 C5 109.39(17) . . ? O3 C4 Li 49.22(12) . . ? C5 C4 Li 78.87(15) . . ? O3 C4 H4A 109.8 . . ? C5 C4 H4A 109.8 . . ? Li C4 H4A 85.8 . . ? O3 C4 H4B 109.8 . . ? C5 C4 H4B 109.8 . . ? Li C4 H4B 158.7 . . ? H4A C4 H4B 108.2 . . ? O6 C5 C4 105.69(17) . . ? O6 C5 H5A 110.6 . . ? C4 C5 H5A 110.6 . . ? O6 C5 H5B 110.6 . . ? C4 C5 H5B 110.6 . . ? H5A C5 H5B 108.7 . . ? C5 O6 C7 115.42(17) . . ? C5 O6 Li 113.01(17) . . ? C7 O6 Li 113.62(18) . . ? O6 C7 C8 105.73(19) . . ? O6 C7 H7A 110.6 . . ? C8 C7 H7A 110.6 . . ? O6 C7 H7B 110.6 . . ? C8 C7 H7B 110.6 . . ? H7A C7 H7B 108.7 . . ? O9 C8 C7 109.9(2) . . ? O9 C8 H8A 109.7 . . ? C7 C8 H8A 109.7 . . ? O9 C8 H8B 109.7 . . ? C7 C8 H8B 109.7 . . ? H8A C8 H8B 108.2 . . ? C8 O9 C10 115.00(17) . . ? C8 O9 Li 110.75(17) . . ? C10 O9 Li 105.19(17) . . ? O9 C10 C11 105.89(18) . . ? O9 C10 H10A 110.6 . . ? C11 C10 H10A 110.6 . . ? O9 C10 H10B 110.6 . . ? C11 C10 H10B 110.6 . . ? H10A C10 H10B 108.7 . . ? O12 C11 C10 107.41(19) . . ? O12 C11 H11A 110.2 . . ? C10 C11 H11A 110.2 . . ? O12 C11 H11B 110.2 . . ? C10 C11 H11B 110.2 . . ? H11A C11 H11B 108.5 . . ? C11 O12 C13 111.45(17) . . ? C11 O12 Li 109.85(17) . . ? C13 O12 Li 121.45(16) . . ? O12 C13 C14 111.83(17) . . ? O12 C13 H13A 109.3 . . ? C14 C13 H13A 109.3 . . ? O12 C13 H13B 109.3 . . ? C14 C13 H13B 109.3 . . ? H13A C13 H13B 107.9 . . ? N15 C14 C13 117.04(17) . . ? N15 C14 H14A 108 . . ? C13 C14 H14A 108 . . ? N15 C14 H14B 108 . . ? C13 C14 H14B 108 . . ? H14A C14 H14B 107.3 . . ? C1 N15 C14 113.87(17) . . ? C1 N15 C16 110.76(16) . . ? C14 N15 C16 107.94(15) . . ? C1 N15 Sn1 109.30(11) . . ? C14 N15 Sn1 109.21(12) . . ? C16 N15 Sn1 105.42(12) . . ? N15 C16 C17 113.30(17) . . ? N15 C16 H16A 108.9 . . ? C17 C16 H16A 108.9 . . ? N15 C16 H16B 108.9 . . ? C17 C16 H16B 108.9 . . ? H16A C16 H16B 107.7 . . ? C18 C17 C22 120.8(2) . . ? C18 C17 C16 120.83(19) . . ? C22 C17 C16 118.32(18) . . ? C19 C18 C17 121.1(2) . . ? C19 C18 H18 119.5 . . ? C17 C18 H18 119.5 . . ? C18 C19 C20 116.90(19) . . ? C18 C19 C23 122.7(2) . . ? C20 C19 C23 120.4(2) . . ? C19 C20 C21 124.3(2) . . ? C19 C20 H20 117.8 . . ? C21 C20 H20 117.8 . . ? C20 C21 C22 117.00(19) . . ? C20 C21 C27 121.6(2) . . ? C22 C21 C27 121.39(18) . . ? O31 C22 C17 118.07(19) . . ? O31 C22 C21 122.41(18) . . ? C17 C22 C21 119.52(18) . . ? C26 C23 C25 108.9(2) . . ? C26 C23 C24 109.4(2) . . ? C25 C23 C24 108.2(2) . . ? C26 C23 C19 108.83(19) . . ? C25 C23 C19 110.45(19) . . ? C24 C23 C19 110.94(19) . . ? C23 C24 H24A 109.5 . . ? C23 C24 H24B 109.5 . . ? H24A C24 H24B 109.5 . . ? C23 C24 H24C 109.5 . . ? H24A C24 H24C 109.5 . . ? H24B C24 H24C 109.5 . . ? C23 C25 H25A 109.5 . . ? C23 C25 H25B 109.5 . . ? H25A C25 H25B 109.5 . . ? C23 C25 H25C 109.5 . . ? H25A C25 H25C 109.5 . . ? H25B C25 H25C 109.5 . . ? C23 C26 H26A 109.5 . . ? C23 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C23 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C29 C27 C30 110.02(19) . . ? C29 C27 C28 107.9(2) . . ? C30 C27 C28 107.3(2) . . ? C29 C27 C21 109.18(19) . . ? C30 C27 C21 110.6(2) . . ? C28 C27 C21 111.82(18) . . ? C27 C28 H28A 109.5 . . ? C27 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C27 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C27 C29 H29A 109.5 . . ? C27 C29 H29B 109.5 . . ? H29A C29 H29B 109.5 . . ? C27 C29 H29C 109.5 . . ? H29A C29 H29C 109.5 . . ? H29B C29 H29C 109.5 . . ? C27 C30 H30A 109.5 . . ? C27 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C27 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C22 O31 Sn1 109.71(12) . . ? Si2 N32 Si1 121.49(10) . . ? Si2 N32 Sn1 115.83(9) . . ? Si1 N32 Sn1 122.36(9) . . ? Si1 C33 H33A 109.5 . . ? Si1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? Si1 C34 H34A 109.5 . . ? Si1 C34 H34B 109.5 . . ? H34A C34 H34B 109.5 . . ? Si1 C34 H34C 109.5 . . ? H34A C34 H34C 109.5 . . ? H34B C34 H34C 109.5 . . ? Si1 C35 H35A 109.5 . . ? Si1 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? Si1 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 . . ? Si2 C37 H37A 109.5 . . ? Si2 C37 H37B 109.5 . . ? H37A C37 H37B 109.5 . . ? Si2 C37 H37C 109.5 . . ? H37A C37 H37C 109.5 . . ? H37B C37 H37C 109.5 . . ? Si2 C38 H38A 109.5 . . ? Si2 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? Si2 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? F42 C41 F43 107.9(2) . . ? F42 C41 F44 107.1(3) . . ? F43 C41 F44 107.3(3) . . ? F42 C41 S1 110.9(2) . . ? F43 C41 S1 111.2(2) . . ? F44 C41 S1 112.25(18) . . ? O46 S1 O47 116.46(10) . . ? O46 S1 O45 114.39(11) . . ? O47 S1 O45 113.76(10) . . ? O46 S1 C41 104.00(14) . . ? O47 S1 C41 103.98(12) . . ? O45 S1 C41 101.88(13) . . ? S1 O45 Li 143.86(17) . . ? 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 N15 C1 C2 O3 63.4(2) . . . . ? C1 C2 O3 C4 170.95(17) . . . . ? C1 C2 O3 Li 40.2(3) . . . . ? O45 Li O3 C2 -150.69(19) . . . . ? O6 Li O3 C2 105.0(2) . . . . ? O12 Li O3 C2 -30.9(3) . . . . ? O9 Li O3 C2 53.4(5) . . . . ? C4 Li O3 C2 134.1(3) . . . . ? O45 Li O3 C4 75.18(19) . . . . ? O6 Li O3 C4 -29.18(15) . . . . ? O12 Li O3 C4 -165.07(15) . . . . ? O9 Li O3 C4 -80.8(4) . . . . ? C2 O3 C4 C5 -92.1(2) . . . . ? Li O3 C4 C5 55.0(2) . . . . ? C2 O3 C4 Li -147.07(19) . . . . ? O45 Li C4 O3 -108.0(2) . . . . ? O6 Li C4 O3 144.12(18) . . . . ? O12 Li C4 O3 18.52(19) . . . . ? O9 Li C4 O3 135.1(3) . . . . ? O45 Li C4 C5 123.95(19) . . . . ? O6 Li C4 C5 16.06(13) . . . . ? O12 Li C4 C5 -109.5(2) . . . . ? O9 Li C4 C5 7.0(3) . . . . ? O3 Li C4 C5 -128.07(19) . . . . ? O3 C4 C5 O6 -58.8(2) . . . . ? Li C4 C5 O6 -19.62(15) . . . . ? C4 C5 O6 C7 162.61(19) . . . . ? C4 C5 O6 Li 29.5(2) . . . . ? O45 Li O6 C5 -99.0(2) . . . . ? O12 Li O6 C5 90.6(3) . . . . ? O9 Li O6 C5 155.34(15) . . . . ? O3 Li O6 C5 -0.47(18) . . . . ? C4 Li O6 C5 -18.08(14) . . . . ? O45 Li O6 C7 127.0(2) . . . . ? O12 Li O6 C7 -43.4(4) . . . . ? O9 Li O6 C7 21.34(19) . . . . ? O3 Li O6 C7 -134.47(16) . . . . ? C4 Li O6 C7 -152.08(17) . . . . ? C5 O6 C7 C8 -176.44(19) . . . . ? Li O6 C7 C8 -43.6(2) . . . . ? O6 C7 C8 O9 49.0(3) . . . . ? C7 C8 O9 C10 86.6(2) . . . . ? C7 C8 O9 Li -32.5(2) . . . . ? O45 Li O9 C8 -95.8(2) . . . . ? O6 Li O9 C8 7.20(18) . . . . ? O12 Li O9 C8 147.96(15) . . . . ? O3 Li O9 C8 59.3(4) . . . . ? C4 Li O9 C8 14.7(3) . . . . ? O45 Li O9 C10 139.3(2) . . . . ? O6 Li O9 C10 -117.64(16) . . . . ? O12 Li O9 C10 23.13(18) . . . . ? O3 Li O9 C10 -65.5(4) . . . . ? C4 Li O9 C10 -110.1(2) . . . . ? C8 O9 C10 C11 -172.16(19) . . . . ? Li O9 C10 C11 -50.0(2) . . . . ? O9 C10 C11 O12 60.7(2) . . . . ? C10 C11 O12 C13 -176.89(17) . . . . ? C10 C11 O12 Li -39.3(2) . . . . ? O45 Li O12 C11 -96.2(2) . . . . ? O6 Li O12 C11 73.4(3) . . . . ? O9 Li O12 C11 9.34(18) . . . . ? O3 Li O12 C11 158.20(16) . . . . ? C4 Li O12 C11 148.80(19) . . . . ? O45 Li O12 C13 36.4(3) . . . . ? O6 Li O12 C13 -154.0(3) . . . . ? O9 Li O12 C13 141.91(16) . . . . ? O3 Li O12 C13 -69.2(2) . . . . ? C4 Li O12 C13 -78.6(2) . . . . ? C11 O12 C13 C14 175.55(17) . . . . ? Li O12 C13 C14 43.6(2) . . . . ? O12 C13 C14 N15 77.6(2) . . . . ? C2 C1 N15 C14 -73.2(2) . . . . ? C2 C1 N15 C16 48.7(2) . . . . ? C2 C1 N15 Sn1 164.42(15) . . . . ? C13 C14 N15 C1 -62.9(2) . . . . ? C13 C14 N15 C16 173.65(18) . . . . ? C13 C14 N15 Sn1 59.5(2) . . . . ? O31 Sn1 N15 C1 -112.85(13) . . . . ? N32 Sn1 N15 C1 -16.80(14) . . . . ? O31 Sn1 N15 C14 121.99(13) . . . . ? N32 Sn1 N15 C14 -141.97(13) . . . . ? O31 Sn1 N15 C16 6.24(12) . . . . ? N32 Sn1 N15 C16 102.28(12) . . . . ? C1 N15 C16 C17 168.10(17) . . . . ? C14 N15 C16 C17 -66.6(2) . . . . ? Sn1 N15 C16 C17 49.99(18) . . . . ? N15 C16 C17 C18 104.8(2) . . . . ? N15 C16 C17 C22 -74.7(2) . . . . ? C22 C17 C18 C19 -0.4(3) . . . . ? C16 C17 C18 C19 -179.9(2) . . . . ? C17 C18 C19 C20 -3.8(3) . . . . ? C17 C18 C19 C23 177.5(2) . . . . ? C18 C19 C20 C21 3.4(3) . . . . ? C23 C19 C20 C21 -177.9(2) . . . . ? C19 C20 C21 C22 1.1(3) . . . . ? C19 C20 C21 C27 -177.9(2) . . . . ? C18 C17 C22 O31 -174.11(19) . . . . ? C16 C17 C22 O31 5.4(3) . . . . ? C18 C17 C22 C21 5.0(3) . . . . ? C16 C17 C22 C21 -175.45(19) . . . . ? C20 C21 C22 O31 173.83(19) . . . . ? C27 C21 C22 O31 -7.2(3) . . . . ? C20 C21 C22 C17 -5.3(3) . . . . ? C27 C21 C22 C17 173.7(2) . . . . ? C18 C19 C23 C26 103.9(3) . . . . ? C20 C19 C23 C26 -74.7(3) . . . . ? C18 C19 C23 C25 -136.5(2) . . . . ? C20 C19 C23 C25 44.8(3) . . . . ? C18 C19 C23 C24 -16.6(3) . . . . ? C20 C19 C23 C24 164.8(2) . . . . ? C20 C21 C27 C29 122.1(2) . . . . ? C22 C21 C27 C29 -56.9(3) . . . . ? C20 C21 C27 C30 -116.8(2) . . . . ? C22 C21 C27 C30 64.3(3) . . . . ? C20 C21 C27 C28 2.7(3) . . . . ? C22 C21 C27 C28 -176.2(2) . . . . ? C17 C22 O31 Sn1 67.6(2) . . . . ? C21 C22 O31 Sn1 -111.50(19) . . . . ? N32 Sn1 O31 C22 -161.31(13) . . . . ? N15 Sn1 O31 C22 -62.41(13) . . . . ? C36 Si2 N32 Si1 -61.67(16) . . . . ? C37 Si2 N32 Si1 62.40(16) . . . . ? C38 Si2 N32 Si1 -179.91(13) . . . . ? C36 Si2 N32 Sn1 111.95(13) . . . . ? C37 Si2 N32 Sn1 -123.98(13) . . . . ? C38 Si2 N32 Sn1 -6.29(15) . . . . ? C33 Si1 N32 Si2 -111.89(14) . . . . ? C34 Si1 N32 Si2 125.61(14) . . . . ? C35 Si1 N32 Si2 8.52(17) . . . . ? C33 Si1 N32 Sn1 74.91(14) . . . . ? C34 Si1 N32 Sn1 -47.59(15) . . . . ? C35 Si1 N32 Sn1 -164.68(13) . . . . ? O31 Sn1 N32 Si2 174.52(9) . . . . ? N15 Sn1 N32 Si2 89.08(10) . . . . ? O31 Sn1 N32 Si1 -11.92(11) . . . . ? N15 Sn1 N32 Si1 -97.36(11) . . . . ? F42 C41 S1 O46 59.9(2) . . . . ? F43 C41 S1 O46 180.0(2) . . . . ? F44 C41 S1 O46 -59.9(3) . . . . ? F42 C41 S1 O47 -62.5(2) . . . . ? F43 C41 S1 O47 57.6(2) . . . . ? F44 C41 S1 O47 177.8(2) . . . . ? F42 C41 S1 O45 179.1(2) . . . . ? F43 C41 S1 O45 -60.9(2) . . . . ? F44 C41 S1 O45 59.3(3) . . . . ? O46 S1 O45 Li -0.5(3) . . . . ? O47 S1 O45 Li 136.8(3) . . . . ? C41 S1 O45 Li -112.0(3) . . . . ? O6 Li O45 S1 178.79(19) . . . . ? O12 Li O45 S1 -8.7(4) . . . . ? O9 Li O45 S1 -97.8(3) . . . . ? O3 Li O45 S1 94.9(3) . . . . ? C4 Li O45 S1 124.5(2) . . . . ? #----------------------------------------------------------------------------# # END OF CIF FILE FOR WLF020 #----------------------------------------------------------------------------# _database_code_depnum_ccdc_archive 'CCDC 942098' ####################################################################### # # Cambridge Crystallographic Data Centre # CCDC # ####################################################################### # # This CIF contains data from an original supplementary publication # deposited with the CCDC, and may include chemical, crystal, # experimental, refinement, atomic coordinates, # anisotropic displacement parameters and molecular geometry data, # as required by the journal to which it was submitted. # # This CIF is provided on the understanding that it is used for bona # fide research purposes only. It may contain copyright material # of the CCDC or of third parties, and may not be copied or further # disseminated in any form, whether machine-readable or not, # except for the purpose of generating routine backup copies # on your local computer system. # # For further information on the CCDC, data deposition and # data retrieval see: # www.ccdc.cam.ac.uk # # Bona fide researchers may freely download Mercury and enCIFer # from this site to visualise CIF-encoded structures and # to carry out CIF format checking respectively. # data_WLF024 _audit_creation_date 2013-05-16T14:15:55-00:00 _audit_creation_method 'WinGX routine CIF_UPDATE' _audit_conform_dict_name cif_core.dic _audit_conform_dict_version 2.3 _audit_conform_dict_location ftp://ftp.iucr.org/pub/cif_core.dic #----------------------------------------------------------------------------# # CHEMICAL INFORMATION # #----------------------------------------------------------------------------# _chemical_name_systematic ; ? ; _chemical_formula_moiety 'C29 H56 N2 O4 Si2 Sn1' _chemical_formula_sum 'C29 H56 N2 O4 Si2 Sn' _chemical_formula_weight 671.63 _chemical_compound_source 'synthesis as described' #----------------------------------------------------------------------------# # UNIT CELL INFORMATION # #----------------------------------------------------------------------------# _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' _symmetry_Int_Tables_number 2 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.7245(3) _cell_length_b 13.2277(4) _cell_length_c 13.3588(4) _cell_angle_alpha 70.5920(10) _cell_angle_beta 85.7950(10) _cell_angle_gamma 77.0520(10) _cell_volume 1741.95(9) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 9757 _cell_measurement_theta_min 2.53 _cell_measurement_theta_max 27.44 _cell_measurement_wavelength 0.71073 #----------------------------------------------------------------------------# # CRYSTAL INFORMATION # #----------------------------------------------------------------------------# _exptl_crystal_description prism _exptl_crystal_colour colourless _exptl_crystal_size_max 0.38 _exptl_crystal_size_mid 0.34 _exptl_crystal_size_min 0.14 _exptl_crystal_density_diffrn 1.28 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 708 _exptl_special_details ; ? ; #----------------------------------------------------------------------------# # ABSORPTION CORRECTION # #----------------------------------------------------------------------------# _exptl_absorpt_coefficient_mu 0.834 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; [Sheldrick, G.M. (2002). SADABS Bruker AXS Inc., Madison, Wisconsin, USA] ; _exptl_absorpt_correction_T_min 0.759 _exptl_absorpt_correction_T_max 0.890 #----------------------------------------------------------------------------# # DATA COLLECTION # #----------------------------------------------------------------------------# _diffrn_measurement_device_type 'APEXII, Bruker-AXS' _diffrn_measurement_method 'CCD rotation images, thin slices' _diffrn_detector 'CCD plate' _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_monochromator graphite _diffrn_radiation_probe x-ray _diffrn_reflns_av_R_equivalents 0.0243 _diffrn_reflns_av_unetI/netI 0.0298 _diffrn_reflns_number 21981 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 2.97 _diffrn_reflns_theta_max 27.46 _diffrn_reflns_theta_full 27.46 _diffrn_measured_fraction_theta_full 0.98 _diffrn_measured_fraction_theta_max 0.98 _reflns_number_total 7802 _reflns_number_gt 7123 _reflns_threshold_expression >2sigma(I) #----------------------------------------------------------------------------# # COMPUTER PROGRAMS USED # #----------------------------------------------------------------------------# _computing_data_collection 'Bruker APEX2 (Bruker, 2006)' _computing_cell_refinement 'Bruker APEX2 (Bruker, 2006)' _computing_data_reduction 'Bruker APEX2 (Bruker, 2006)' _computing_structure_solution 'SIR97 (Altomare et al., 1999)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Ortep-3 for Windows (Farrugia, 1997)' _computing_publication_material ; WinGX publication routines (Farrugia, 2012), CRYSCAL (T. Roisnel, local program) ; #----------------------------------------------------------------------------# # REFINEMENT INFORMATION # #----------------------------------------------------------------------------# _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0206P)^2^+0.5906P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_number_reflns 7802 _refine_ls_number_parameters 355 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0258 _refine_ls_R_factor_gt 0.0219 _refine_ls_wR_factor_ref 0.0516 _refine_ls_wR_factor_gt 0.05 _refine_ls_goodness_of_fit_ref 1.026 _refine_ls_restrained_S_all 1.026 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0 _refine_diff_density_max 0.338 _refine_diff_density_min -0.272 _refine_diff_density_rms 0.054 _iucr_refine_instructions_details ; .res file for SHELXL : WLF024.res ................................................................. TITL import in P -1 CELL 0.71073 10.7245 13.2277 13.3588 70.592 85.795 77.052 ZERR 2.00 0.0003 0.0004 0.0004 0.001 0.001 0.001 LATT 1 SFAC C H N O SI SN UNIT 58.00 112.00 4.00 8.00 4.00 2.00 MERG 2 FMAP 2 PLAN 20 ACTA BOND $H CONF LIST 4 WPDB -2 L.S. 4 TEMP -123.00 WGHT 0.020600 0.590600 FVAR 0.61103 SN1 6 0.113164 0.707465 0.639555 11.00000 0.01860 0.01821 = 0.01707 -0.00660 0.00228 -0.00562 SI1 5 0.380266 0.640755 0.786932 11.00000 0.01786 0.02181 = 0.02236 -0.00172 0.00108 -0.00172 SI2 5 0.248382 0.878904 0.695312 11.00000 0.02033 0.01833 = 0.02076 -0.00448 -0.00212 -0.00628 O1 4 0.180052 0.539744 0.697296 11.00000 0.02038 0.01830 = 0.02881 -0.01024 0.00660 -0.00671 C2 1 0.099075 0.469698 0.720624 11.00000 0.01992 0.01568 = 0.01906 -0.00386 0.00126 -0.00348 C3 1 0.116739 0.382183 0.678098 11.00000 0.02261 0.01591 = 0.01804 -0.00479 0.00231 -0.00210 C4 1 0.028609 0.314177 0.707315 11.00000 0.02779 0.01579 = 0.02288 -0.00864 0.00172 -0.00527 AFIX 43 H4 2 0.039324 0.255916 0.678725 11.00000 -1.20000 AFIX 0 C5 1 -0.074748 0.326229 0.776131 11.00000 0.02420 0.01773 = 0.02221 -0.00453 0.00256 -0.00612 C6 1 -0.087877 0.411291 0.817340 11.00000 0.02278 0.01896 = 0.02044 -0.00536 0.00505 -0.00387 AFIX 43 H6 2 -0.156718 0.422072 0.864252 11.00000 -1.20000 AFIX 0 C7 1 -0.002086 0.481682 0.791460 11.00000 0.02238 0.01506 = 0.01926 -0.00555 0.00150 -0.00253 C8 1 0.229068 0.362804 0.603637 11.00000 0.02636 0.01913 = 0.02542 -0.01073 0.00832 -0.00432 C9 1 0.356451 0.344687 0.659357 11.00000 0.02494 0.03193 = 0.04480 -0.01921 0.00607 -0.00007 AFIX 137 H9A 2 0.357520 0.408323 0.681102 11.00000 -1.50000 H9B 2 0.427429 0.335423 0.610413 11.00000 -1.50000 H9C 2 0.365636 0.278760 0.722089 11.00000 -1.50000 AFIX 0 C10 1 0.233295 0.260388 0.572167 11.00000 0.03962 0.03029 = 0.03750 -0.02068 0.01482 -0.00869 AFIX 137 H10A 2 0.241188 0.195813 0.636152 11.00000 -1.50000 H10B 2 0.306982 0.250523 0.525832 11.00000 -1.50000 H10C 2 0.154410 0.269527 0.534450 11.00000 -1.50000 AFIX 0 C11 1 0.216260 0.461812 0.500768 11.00000 0.04291 0.02943 = 0.02782 -0.00773 0.01525 -0.00491 AFIX 137 H11A 2 0.134822 0.472082 0.466074 11.00000 -1.50000 H11B 2 0.287095 0.448455 0.452930 11.00000 -1.50000 H11C 2 0.218714 0.527879 0.517863 11.00000 -1.50000 AFIX 0 C12 1 -0.166214 0.246534 0.802674 11.00000 0.02793 0.01881 = 0.03125 -0.00639 0.00469 -0.00995 C13 1 -0.235591 0.260409 0.700635 11.00000 0.04347 0.03700 = 0.04144 -0.00952 -0.00151 -0.02267 AFIX 137 H13A 2 -0.283221 0.336312 0.671374 11.00000 -1.50000 H13B 2 -0.295089 0.210644 0.717014 11.00000 -1.50000 H13C 2 -0.172659 0.243111 0.648515 11.00000 -1.50000 AFIX 0 C14 1 -0.089668 0.127791 0.848527 11.00000 0.03693 0.02104 = 0.05445 -0.00392 0.00279 -0.01250 AFIX 137 H14A 2 -0.028701 0.110258 0.795297 11.00000 -1.50000 H14B 2 -0.148520 0.077362 0.867516 11.00000 -1.50000 H14C 2 -0.043084 0.120207 0.911940 11.00000 -1.50000 AFIX 0 C15 1 -0.267133 0.268073 0.884524 11.00000 0.03782 0.03406 = 0.04919 -0.01402 0.01796 -0.02043 AFIX 137 H15A 2 -0.224654 0.259834 0.950132 11.00000 -1.50000 H15B 2 -0.322925 0.215389 0.899472 11.00000 -1.50000 H15C 2 -0.318426 0.342783 0.856367 11.00000 -1.50000 AFIX 0 C16 1 -0.010784 0.564099 0.848784 11.00000 0.02356 0.01841 = 0.01850 -0.00683 0.00355 -0.00430 AFIX 23 H16A 2 -0.075999 0.551086 0.905368 11.00000 -1.20000 H16B 2 0.072446 0.550912 0.883555 11.00000 -1.20000 AFIX 0 N17 3 -0.044232 0.682059 0.779946 11.00000 0.01812 0.01698 = 0.01875 -0.00917 0.00204 -0.00379 C18 1 -0.036963 0.753100 0.844864 11.00000 0.01973 0.02002 = 0.02073 -0.01025 0.00113 -0.00558 AFIX 23 H18A 2 -0.059071 0.830623 0.798725 11.00000 -1.20000 H18B 2 0.052761 0.738221 0.868191 11.00000 -1.20000 AFIX 0 C19 1 -0.122562 0.739441 0.942519 11.00000 0.02642 0.02158 = 0.02033 -0.01085 0.00133 -0.00288 AFIX 23 H19A 2 -0.207233 0.729801 0.927088 11.00000 -1.20000 H19B 2 -0.082927 0.675110 1.002401 11.00000 -1.20000 AFIX 0 O20 4 -0.134678 0.837976 0.966760 11.00000 0.02947 0.03093 = 0.03221 -0.02253 0.00538 -0.00715 C21 1 -0.241790 0.857552 1.032807 11.00000 0.04343 0.03755 = 0.02932 -0.02248 0.01029 -0.00526 AFIX 23 H21A 2 -0.230652 0.913249 1.063923 11.00000 -1.20000 H21B 2 -0.244719 0.788945 1.091849 11.00000 -1.20000 AFIX 0 C22 1 -0.366515 0.896702 0.973205 11.00000 0.03285 0.03139 = 0.03914 -0.02039 0.01813 -0.00831 AFIX 23 H22A 2 -0.377082 0.843247 0.938987 11.00000 -1.20000 H22B 2 -0.438700 0.903578 1.022818 11.00000 -1.20000 AFIX 0 O23 4 -0.366109 1.001181 0.894193 11.00000 0.03437 0.02733 = 0.04145 -0.01896 0.00663 -0.00943 C24 1 -0.424970 1.019777 0.796391 11.00000 0.02215 0.02393 = 0.04712 -0.01657 0.00237 -0.00249 AFIX 23 H24A 2 -0.463253 1.098937 0.765581 11.00000 -1.20000 H24B 2 -0.495146 0.979426 0.809803 11.00000 -1.20000 AFIX 0 C25 1 -0.333589 0.984448 0.716699 11.00000 0.02668 0.01946 = 0.03427 -0.00946 0.00052 -0.00450 AFIX 23 H25A 2 -0.375097 1.011897 0.646140 11.00000 -1.20000 H25B 2 -0.256396 1.015472 0.710462 11.00000 -1.20000 AFIX 0 O26 4 -0.298460 0.868077 0.751028 11.00000 0.02272 0.01837 = 0.02491 -0.00985 0.00433 -0.00194 C27 1 -0.228285 0.824897 0.674248 11.00000 0.02006 0.02435 = 0.02173 -0.01010 0.00116 -0.00375 AFIX 23 H27A 2 -0.159211 0.864786 0.643978 11.00000 -1.20000 H27B 2 -0.285572 0.833487 0.615800 11.00000 -1.20000 AFIX 0 C28 1 -0.171636 0.704322 0.728886 11.00000 0.01854 0.02178 = 0.02283 -0.01219 0.00178 -0.00486 AFIX 23 H28A 2 -0.232321 0.673330 0.783845 11.00000 -1.20000 H28B 2 -0.162533 0.665562 0.675984 11.00000 -1.20000 AFIX 0 N29 3 0.247985 0.740546 0.725807 11.00000 0.01750 0.01882 = 0.01999 -0.00495 -0.00032 -0.00504 C30 1 0.340981 0.517252 0.891821 11.00000 0.03074 0.03000 = 0.03272 0.00420 -0.00599 -0.00563 AFIX 137 H30A 2 0.286382 0.540338 0.945801 11.00000 -1.50000 H30B 2 0.420212 0.467722 0.924990 11.00000 -1.50000 H30C 2 0.295800 0.479097 0.859538 11.00000 -1.50000 AFIX 0 C31 1 0.485890 0.597261 0.683995 11.00000 0.03191 0.03668 = 0.04188 -0.01265 0.01022 0.00086 AFIX 137 H31A 2 0.436143 0.572073 0.641881 11.00000 -1.50000 H31B 2 0.556870 0.537405 0.718905 11.00000 -1.50000 H31C 2 0.519904 0.659554 0.637358 11.00000 -1.50000 AFIX 0 C32 1 0.481178 0.693003 0.859956 11.00000 0.02338 0.03678 = 0.02930 -0.00088 -0.00630 -0.00571 AFIX 137 H32A 2 0.503435 0.760642 0.811983 11.00000 -1.50000 H32B 2 0.559594 0.637563 0.885386 11.00000 -1.50000 H32C 2 0.433075 0.708024 0.920544 11.00000 -1.50000 AFIX 0 C33 1 0.107275 0.968373 0.610588 11.00000 0.03262 0.01913 = 0.04073 -0.00112 -0.01274 -0.00579 AFIX 137 H33A 2 0.109744 0.951587 0.544236 11.00000 -1.50000 H33B 2 0.110505 1.045610 0.594602 11.00000 -1.50000 H33C 2 0.027974 0.954588 0.648735 11.00000 -1.50000 AFIX 0 C34 1 0.236933 0.924310 0.814808 11.00000 0.03209 0.02812 = 0.03226 -0.01342 0.00070 -0.00838 AFIX 137 H34A 2 0.157777 0.910712 0.853305 11.00000 -1.50000 H34B 2 0.236468 1.002859 0.792400 11.00000 -1.50000 H34C 2 0.310556 0.883145 0.861319 11.00000 -1.50000 AFIX 0 C35 1 0.391467 0.916970 0.614075 11.00000 0.03129 0.03335 = 0.02655 -0.00415 0.00168 -0.01532 AFIX 137 H35A 2 0.469318 0.879863 0.656526 11.00000 -1.50000 H35B 2 0.383636 0.996548 0.592456 11.00000 -1.50000 H35C 2 0.396135 0.894370 0.550840 11.00000 -1.50000 HKLF 4 REM import in P -1 REM R1 = 0.0219 for 7123 Fo > 4sig(Fo) and 0.0258 for all 7802 data REM 355 parameters refined using 0 restraints END WGHT 0.0206 0.5959 REM Highest difference peak 0.34, deepest hole -0.27, 1-sigma level 0.05 Q1 1 0.3213 0.9010 0.6464 11.00000 0.05 0.34 Q2 1 0.2622 0.7991 0.7076 11.00000 0.05 0.34 Q3 1 -0.0050 0.5195 0.8166 11.00000 0.05 0.33 Q4 1 -0.0262 0.6238 0.8096 11.00000 0.05 0.33 Q5 1 0.1809 0.3697 0.6515 11.00000 0.05 0.33 Q6 1 0.2197 0.3154 0.5841 11.00000 0.05 0.33 Q7 1 0.4378 0.6080 0.7461 11.00000 0.05 0.31 Q8 1 0.0620 0.6985 0.5861 11.00000 0.05 0.31 Q9 1 -0.0827 0.7389 0.8940 11.00000 0.05 0.31 Q10 1 0.1727 0.9239 0.6537 11.00000 0.05 0.31 Q11 1 -0.1194 0.2863 0.7900 11.00000 0.05 0.30 Q12 1 -0.1174 0.6954 0.7571 11.00000 0.05 0.30 Q13 1 -0.1910 0.7663 0.7033 11.00000 0.05 0.30 Q14 1 -0.0215 0.3253 0.7460 11.00000 0.05 0.28 Q15 1 -0.2622 0.8519 0.7107 11.00000 0.05 0.28 Q16 1 -0.0736 0.3593 0.7990 11.00000 0.05 0.28 Q17 1 -0.0982 0.3790 0.7797 11.00000 0.05 0.28 Q18 1 0.1393 0.5053 0.7073 11.00000 0.05 0.28 Q19 1 0.0779 0.7610 0.5781 11.00000 0.05 0.27 Q20 1 -0.3826 0.9995 0.7555 11.00000 0.05 0.27 ; # End of res file #----------------------------------------------------------------------------# #----------------------------------------------------------------------------# # ATOMIC TYPES, COORDINATES AND THERMAL PARAMETERS # #----------------------------------------------------------------------------# loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0 0 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.006 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' 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 0.113164(10) 0.707465(8) 0.639555(8) 0.01757(4) Uani 1 1 d . . . Si1 Si 0.38027(4) 0.64075(4) 0.78693(4) 0.02254(10) Uani 1 1 d . . . Si2 Si 0.24838(4) 0.87890(3) 0.69531(3) 0.01981(9) Uani 1 1 d . . . O1 O 0.18005(10) 0.53974(9) 0.69730(9) 0.0218(2) Uani 1 1 d . . . C2 C 0.09907(15) 0.46970(12) 0.72062(12) 0.0188(3) Uani 1 1 d . . . C3 C 0.11674(15) 0.38218(12) 0.67810(12) 0.0195(3) Uani 1 1 d . . . C4 C 0.02861(16) 0.31418(12) 0.70732(13) 0.0215(3) Uani 1 1 d . . . H4 H 0.0393 0.2559 0.6787 0.026 Uiso 1 1 calc R . . C5 C -0.07475(16) 0.32623(13) 0.77613(13) 0.0217(3) Uani 1 1 d . . . C6 C -0.08788(15) 0.41129(12) 0.81734(13) 0.0214(3) Uani 1 1 d . . . H6 H -0.1567 0.4221 0.8643 0.026 Uiso 1 1 calc R . . C7 C -0.00209(15) 0.48168(12) 0.79146(12) 0.0192(3) Uani 1 1 d . . . C8 C 0.22907(16) 0.36280(13) 0.60364(13) 0.0233(3) Uani 1 1 d . . . C9 C 0.35645(17) 0.34469(15) 0.65936(16) 0.0335(4) Uani 1 1 d . . . H9A H 0.3575 0.4083 0.6811 0.05 Uiso 1 1 calc R . . H9B H 0.4274 0.3354 0.6104 0.05 Uiso 1 1 calc R . . H9C H 0.3656 0.2788 0.7221 0.05 Uiso 1 1 calc R . . C10 C 0.23329(19) 0.26039(15) 0.57217(16) 0.0339(4) Uani 1 1 d . . . H10A H 0.2412 0.1958 0.6362 0.051 Uiso 1 1 calc R . . H10B H 0.307 0.2505 0.5258 0.051 Uiso 1 1 calc R . . H10C H 0.1544 0.2695 0.5344 0.051 Uiso 1 1 calc R . . C11 C 0.21626(19) 0.46181(15) 0.50077(15) 0.0351(4) Uani 1 1 d . . . H11A H 0.1348 0.4721 0.4661 0.053 Uiso 1 1 calc R . . H11B H 0.2871 0.4485 0.4529 0.053 Uiso 1 1 calc R . . H11C H 0.2187 0.5279 0.5179 0.053 Uiso 1 1 calc R . . C12 C -0.16621(16) 0.24653(13) 0.80267(14) 0.0259(4) Uani 1 1 d . . . C13 C -0.2356(2) 0.26041(16) 0.70064(16) 0.0390(5) Uani 1 1 d . . . H13A H -0.2832 0.3363 0.6714 0.059 Uiso 1 1 calc R . . H13B H -0.2951 0.2106 0.717 0.059 Uiso 1 1 calc R . . H13C H -0.1727 0.2431 0.6485 0.059 Uiso 1 1 calc R . . C14 C -0.08967(19) 0.12779(14) 0.84853(18) 0.0387(5) Uani 1 1 d . . . H14A H -0.0287 0.1103 0.7953 0.058 Uiso 1 1 calc R . . H14B H -0.1485 0.0774 0.8675 0.058 Uiso 1 1 calc R . . H14C H -0.0431 0.1202 0.9119 0.058 Uiso 1 1 calc R . . C15 C -0.26713(19) 0.26807(16) 0.88452(17) 0.0391(5) Uani 1 1 d . . . H15A H -0.2247 0.2598 0.9501 0.059 Uiso 1 1 calc R . . H15B H -0.3229 0.2154 0.8995 0.059 Uiso 1 1 calc R . . H15C H -0.3184 0.3428 0.8564 0.059 Uiso 1 1 calc R . . C16 C -0.01078(16) 0.56410(12) 0.84878(12) 0.0202(3) Uani 1 1 d . . . H16A H -0.076 0.5511 0.9054 0.024 Uiso 1 1 calc R . . H16B H 0.0724 0.5509 0.8836 0.024 Uiso 1 1 calc R . . N17 N -0.04423(12) 0.68206(10) 0.77995(10) 0.0172(3) Uani 1 1 d . . . C18 C -0.03696(15) 0.75310(13) 0.84486(12) 0.0191(3) Uani 1 1 d . . . H18A H -0.0591 0.8306 0.7987 0.023 Uiso 1 1 calc R . . H18B H 0.0528 0.7382 0.8682 0.023 Uiso 1 1 calc R . . C19 C -0.12256(16) 0.73944(13) 0.94252(13) 0.0222(3) Uani 1 1 d . . . H19A H -0.2072 0.7298 0.9271 0.027 Uiso 1 1 calc R . . H19B H -0.0829 0.6751 1.0024 0.027 Uiso 1 1 calc R . . O20 O -0.13468(11) 0.83798(10) 0.96676(10) 0.0279(3) Uani 1 1 d . . . C21 C -0.24179(18) 0.85755(16) 1.03281(15) 0.0349(4) Uani 1 1 d . . . H21A H -0.2307 0.9132 1.0639 0.042 Uiso 1 1 calc R . . H21B H -0.2447 0.7889 1.0918 0.042 Uiso 1 1 calc R . . C22 C -0.36651(18) 0.89670(15) 0.97321(15) 0.0329(4) Uani 1 1 d . . . H22A H -0.3771 0.8432 0.939 0.039 Uiso 1 1 calc R . . H22B H -0.4387 0.9036 1.0228 0.039 Uiso 1 1 calc R . . O23 O -0.36611(12) 1.00118(10) 0.89419(11) 0.0323(3) Uani 1 1 d . . . C24 C -0.42497(16) 1.01978(14) 0.79639(16) 0.0303(4) Uani 1 1 d . . . H24A H -0.4633 1.0989 0.7656 0.036 Uiso 1 1 calc R . . H24B H -0.4951 0.9794 0.8098 0.036 Uiso 1 1 calc R . . C25 C -0.33359(17) 0.98445(13) 0.71670(14) 0.0267(4) Uani 1 1 d . . . H25A H -0.3751 1.0119 0.6461 0.032 Uiso 1 1 calc R . . H25B H -0.2564 1.0155 0.7105 0.032 Uiso 1 1 calc R . . O26 O -0.29846(10) 0.86808(9) 0.75103(9) 0.0219(2) Uani 1 1 d . . . C27 C -0.22828(15) 0.82490(13) 0.67425(13) 0.0216(3) Uani 1 1 d . . . H27A H -0.1592 0.8648 0.644 0.026 Uiso 1 1 calc R . . H27B H -0.2856 0.8335 0.6158 0.026 Uiso 1 1 calc R . . C28 C -0.17164(15) 0.70432(12) 0.72889(13) 0.0198(3) Uani 1 1 d . . . H28A H -0.2323 0.6733 0.7838 0.024 Uiso 1 1 calc R . . H28B H -0.1625 0.6656 0.676 0.024 Uiso 1 1 calc R . . N29 N 0.24799(12) 0.74055(10) 0.72581(10) 0.0189(3) Uani 1 1 d . . . C30 C 0.34098(18) 0.51725(15) 0.89182(15) 0.0346(4) Uani 1 1 d . . . H30A H 0.2864 0.5403 0.9458 0.052 Uiso 1 1 calc R . . H30B H 0.4202 0.4677 0.925 0.052 Uiso 1 1 calc R . . H30C H 0.2958 0.4791 0.8595 0.052 Uiso 1 1 calc R . . C31 C 0.48589(19) 0.59726(16) 0.68400(17) 0.0387(5) Uani 1 1 d . . . H31A H 0.4361 0.5721 0.6419 0.058 Uiso 1 1 calc R . . H31B H 0.5569 0.5374 0.7189 0.058 Uiso 1 1 calc R . . H31C H 0.5199 0.6596 0.6374 0.058 Uiso 1 1 calc R . . C32 C 0.48118(17) 0.69300(15) 0.85996(15) 0.0321(4) Uani 1 1 d . . . H32A H 0.5034 0.7606 0.812 0.048 Uiso 1 1 calc R . . H32B H 0.5596 0.6376 0.8854 0.048 Uiso 1 1 calc R . . H32C H 0.4331 0.708 0.9205 0.048 Uiso 1 1 calc R . . C33 C 0.10727(18) 0.96837(14) 0.61059(15) 0.0323(4) Uani 1 1 d . . . H33A H 0.1097 0.9516 0.5442 0.048 Uiso 1 1 calc R . . H33B H 0.1105 1.0456 0.5946 0.048 Uiso 1 1 calc R . . H33C H 0.028 0.9546 0.6487 0.048 Uiso 1 1 calc R . . C34 C 0.23693(18) 0.92431(15) 0.81481(14) 0.0296(4) Uani 1 1 d . . . H34A H 0.1578 0.9107 0.8533 0.044 Uiso 1 1 calc R . . H34B H 0.2365 1.0029 0.7924 0.044 Uiso 1 1 calc R . . H34C H 0.3106 0.8831 0.8613 0.044 Uiso 1 1 calc R . . C35 C 0.39147(17) 0.91697(15) 0.61408(14) 0.0305(4) Uani 1 1 d . . . H35A H 0.4693 0.8799 0.6565 0.046 Uiso 1 1 calc R . . H35B H 0.3836 0.9965 0.5925 0.046 Uiso 1 1 calc R . . H35C H 0.3961 0.8944 0.5508 0.046 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 0.01860(6) 0.01821(6) 0.01707(6) -0.00660(4) 0.00228(4) -0.00562(4) Si1 0.0179(2) 0.0218(2) 0.0224(2) -0.00172(17) 0.00108(18) -0.00172(17) Si2 0.0203(2) 0.0183(2) 0.0208(2) -0.00448(17) -0.00212(17) -0.00628(17) O1 0.0204(6) 0.0183(5) 0.0288(6) -0.0102(5) 0.0066(5) -0.0067(4) C2 0.0199(8) 0.0157(7) 0.0191(8) -0.0039(6) 0.0013(6) -0.0035(6) C3 0.0226(8) 0.0159(7) 0.0180(7) -0.0048(6) 0.0023(6) -0.0021(6) C4 0.0278(9) 0.0158(7) 0.0229(8) -0.0086(6) 0.0017(7) -0.0053(6) C5 0.0242(8) 0.0177(7) 0.0222(8) -0.0045(6) 0.0026(7) -0.0061(6) C6 0.0228(8) 0.0190(8) 0.0204(8) -0.0054(6) 0.0051(6) -0.0039(6) C7 0.0224(8) 0.0151(7) 0.0193(8) -0.0056(6) 0.0015(6) -0.0025(6) C8 0.0264(9) 0.0191(8) 0.0254(8) -0.0107(6) 0.0083(7) -0.0043(6) C9 0.0249(9) 0.0319(10) 0.0448(11) -0.0192(8) 0.0061(8) -0.0001(7) C10 0.0396(11) 0.0303(10) 0.0375(10) -0.0207(8) 0.0148(8) -0.0087(8) C11 0.0429(11) 0.0294(10) 0.0278(10) -0.0077(8) 0.0153(8) -0.0049(8) C12 0.0279(9) 0.0188(8) 0.0312(9) -0.0064(7) 0.0047(7) -0.0100(7) C13 0.0435(12) 0.0370(11) 0.0414(11) -0.0095(9) -0.0015(9) -0.0227(9) C14 0.0369(11) 0.0210(9) 0.0544(13) -0.0039(8) 0.0028(9) -0.0125(8) C15 0.0378(11) 0.0341(10) 0.0492(12) -0.0140(9) 0.0180(9) -0.0204(9) C16 0.0236(8) 0.0184(7) 0.0185(8) -0.0068(6) 0.0035(6) -0.0043(6) N17 0.0181(7) 0.0170(6) 0.0187(6) -0.0092(5) 0.0020(5) -0.0038(5) C18 0.0197(8) 0.0200(8) 0.0207(8) -0.0103(6) 0.0011(6) -0.0056(6) C19 0.0264(9) 0.0216(8) 0.0203(8) -0.0108(6) 0.0013(7) -0.0029(6) O20 0.0295(7) 0.0309(6) 0.0322(7) -0.0225(5) 0.0054(5) -0.0072(5) C21 0.0434(11) 0.0375(10) 0.0293(10) -0.0225(8) 0.0103(8) -0.0053(9) C22 0.0328(10) 0.0314(10) 0.0391(11) -0.0204(8) 0.0181(8) -0.0083(8) O23 0.0344(7) 0.0273(6) 0.0414(8) -0.0190(6) 0.0066(6) -0.0094(5) C24 0.0222(9) 0.0239(9) 0.0471(11) -0.0166(8) 0.0024(8) -0.0025(7) C25 0.0267(9) 0.0195(8) 0.0343(10) -0.0095(7) 0.0005(7) -0.0045(7) O26 0.0227(6) 0.0184(5) 0.0249(6) -0.0099(5) 0.0043(5) -0.0019(4) C27 0.0201(8) 0.0244(8) 0.0217(8) -0.0101(6) 0.0012(6) -0.0037(6) C28 0.0185(8) 0.0218(8) 0.0228(8) -0.0122(6) 0.0018(6) -0.0049(6) N29 0.0175(7) 0.0188(6) 0.0200(7) -0.0049(5) -0.0003(5) -0.0050(5) C30 0.0307(10) 0.0300(10) 0.0327(10) 0.0042(8) -0.0060(8) -0.0056(8) C31 0.0319(10) 0.0367(11) 0.0419(11) -0.0127(9) 0.0102(9) 0.0009(8) C32 0.0234(9) 0.0368(10) 0.0293(9) -0.0009(8) -0.0063(7) -0.0057(8) C33 0.0326(10) 0.0191(8) 0.0407(11) -0.0011(7) -0.0127(8) -0.0058(7) C34 0.0321(10) 0.0281(9) 0.0323(10) -0.0134(7) 0.0007(8) -0.0084(7) C35 0.0313(10) 0.0333(10) 0.0265(9) -0.0041(7) 0.0017(7) -0.0153(8) #----------------------------------------------------------------------------# # MOLECULAR GEOMETRY # #----------------------------------------------------------------------------# _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 O1 2.0645(10) . ? Sn1 N29 2.1149(13) . ? Sn1 N17 2.4188(13) . ? Si1 N29 1.7424(13) . ? Si1 C30 1.8736(18) . ? Si1 C31 1.874(2) . ? Si1 C32 1.8811(19) . ? Si2 N29 1.7387(13) . ? Si2 C34 1.8707(18) . ? Si2 C35 1.8775(18) . ? Si2 C33 1.8789(17) . ? O1 C2 1.3560(18) . ? C2 C7 1.403(2) . ? C2 C3 1.422(2) . ? C3 C4 1.396(2) . ? C3 C8 1.537(2) . ? C4 C5 1.403(2) . ? C4 H4 0.95 . ? C5 C6 1.385(2) . ? C5 C12 1.537(2) . ? C6 C7 1.399(2) . ? C6 H6 0.95 . ? C7 C16 1.511(2) . ? C8 C9 1.537(3) . ? C8 C10 1.537(2) . ? C8 C11 1.541(2) . ? C9 H9A 0.98 . ? C9 H9B 0.98 . ? C9 H9C 0.98 . ? C10 H10A 0.98 . ? C10 H10B 0.98 . ? C10 H10C 0.98 . ? C11 H11A 0.98 . ? C11 H11B 0.98 . ? C11 H11C 0.98 . ? C12 C15 1.531(3) . ? C12 C13 1.538(3) . ? C12 C14 1.540(2) . ? C13 H13A 0.98 . ? C13 H13B 0.98 . ? C13 H13C 0.98 . ? C14 H14A 0.98 . ? C14 H14B 0.98 . ? C14 H14C 0.98 . ? C15 H15A 0.98 . ? C15 H15B 0.98 . ? C15 H15C 0.98 . ? C16 N17 1.5010(19) . ? C16 H16A 0.99 . ? C16 H16B 0.99 . ? N17 C18 1.4918(19) . ? N17 C28 1.4972(19) . ? C18 C19 1.523(2) . ? C18 H18A 0.99 . ? C18 H18B 0.99 . ? C19 O20 1.4209(19) . ? C19 H19A 0.99 . ? C19 H19B 0.99 . ? O20 C21 1.427(2) . ? C21 C22 1.504(3) . ? C21 H21A 0.99 . ? C21 H21B 0.99 . ? C22 O23 1.434(2) . ? C22 H22A 0.99 . ? C22 H22B 0.99 . ? O23 C24 1.416(2) . ? C24 C25 1.511(2) . ? C24 H24A 0.99 . ? C24 H24B 0.99 . ? C25 O26 1.4206(19) . ? C25 H25A 0.99 . ? C25 H25B 0.99 . ? O26 C27 1.4241(19) . ? C27 C28 1.517(2) . ? C27 H27A 0.99 . ? C27 H27B 0.99 . ? C28 H28A 0.99 . ? C28 H28B 0.99 . ? C30 H30A 0.98 . ? C30 H30B 0.98 . ? C30 H30C 0.98 . ? C31 H31A 0.98 . ? C31 H31B 0.98 . ? C31 H31C 0.98 . ? C32 H32A 0.98 . ? C32 H32B 0.98 . ? C32 H32C 0.98 . ? C33 H33A 0.98 . ? C33 H33B 0.98 . ? C33 H33C 0.98 . ? C34 H34A 0.98 . ? C34 H34B 0.98 . ? C34 H34C 0.98 . ? C35 H35A 0.98 . ? C35 H35B 0.98 . ? C35 H35C 0.98 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag O1 Sn1 N29 93.78(5) . . ? O1 Sn1 N17 86.55(4) . . ? N29 Sn1 N17 95.62(5) . . ? N29 Si1 C30 114.83(8) . . ? N29 Si1 C31 109.64(8) . . ? C30 Si1 C31 109.76(9) . . ? N29 Si1 C32 112.32(8) . . ? C30 Si1 C32 103.22(8) . . ? C31 Si1 C32 106.61(9) . . ? N29 Si2 C34 113.41(7) . . ? N29 Si2 C35 112.05(8) . . ? C34 Si2 C35 109.73(9) . . ? N29 Si2 C33 111.50(7) . . ? C34 Si2 C33 105.03(9) . . ? C35 Si2 C33 104.53(8) . . ? C2 O1 Sn1 121.33(9) . . ? O1 C2 C7 119.07(14) . . ? O1 C2 C3 121.68(14) . . ? C7 C2 C3 119.22(14) . . ? C4 C3 C2 117.36(14) . . ? C4 C3 C8 121.39(14) . . ? C2 C3 C8 121.25(14) . . ? C3 C4 C5 124.29(15) . . ? C3 C4 H4 117.9 . . ? C5 C4 H4 117.9 . . ? C6 C5 C4 116.79(15) . . ? C6 C5 C12 123.35(15) . . ? C4 C5 C12 119.86(15) . . ? C5 C6 C7 121.50(15) . . ? C5 C6 H6 119.3 . . ? C7 C6 H6 119.3 . . ? C6 C7 C2 120.81(15) . . ? C6 C7 C16 119.34(14) . . ? C2 C7 C16 119.56(14) . . ? C3 C8 C9 109.94(14) . . ? C3 C8 C10 112.26(14) . . ? C9 C8 C10 106.85(14) . . ? C3 C8 C11 109.75(13) . . ? C9 C8 C11 110.47(15) . . ? C10 C8 C11 107.51(15) . . ? C8 C9 H9A 109.5 . . ? C8 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C8 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C8 C10 H10A 109.5 . . ? C8 C10 H10B 109.5 . . ? H10A C10 H10B 109.5 . . ? C8 C10 H10C 109.5 . . ? H10A C10 H10C 109.5 . . ? H10B C10 H10C 109.5 . . ? C8 C11 H11A 109.5 . . ? C8 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C8 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C15 C12 C5 112.11(15) . . ? C15 C12 C13 108.28(16) . . ? C5 C12 C13 108.91(14) . . ? C15 C12 C14 107.99(15) . . ? C5 C12 C14 109.66(14) . . ? C13 C12 C14 109.86(16) . . ? C12 C13 H13A 109.5 . . ? C12 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C12 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C12 C14 H14A 109.5 . . ? C12 C14 H14B 109.5 . . ? H14A C14 H14B 109.5 . . ? C12 C14 H14C 109.5 . . ? H14A C14 H14C 109.5 . . ? H14B C14 H14C 109.5 . . ? C12 C15 H15A 109.5 . . ? C12 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C12 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? N17 C16 C7 115.05(12) . . ? N17 C16 H16A 108.5 . . ? C7 C16 H16A 108.5 . . ? N17 C16 H16B 108.5 . . ? C7 C16 H16B 108.5 . . ? H16A C16 H16B 107.5 . . ? C18 N17 C28 114.40(12) . . ? C18 N17 C16 108.94(11) . . ? C28 N17 C16 109.28(12) . . ? C18 N17 Sn1 109.59(9) . . ? C28 N17 Sn1 107.28(9) . . ? C16 N17 Sn1 107.09(9) . . ? N17 C18 C19 116.05(13) . . ? N17 C18 H18A 108.3 . . ? C19 C18 H18A 108.3 . . ? N17 C18 H18B 108.3 . . ? C19 C18 H18B 108.3 . . ? H18A C18 H18B 107.4 . . ? O20 C19 C18 104.85(13) . . ? O20 C19 H19A 110.8 . . ? C18 C19 H19A 110.8 . . ? O20 C19 H19B 110.8 . . ? C18 C19 H19B 110.8 . . ? H19A C19 H19B 108.9 . . ? C19 O20 C21 113.36(13) . . ? O20 C21 C22 112.50(15) . . ? O20 C21 H21A 109.1 . . ? C22 C21 H21A 109.1 . . ? O20 C21 H21B 109.1 . . ? C22 C21 H21B 109.1 . . ? H21A C21 H21B 107.8 . . ? O23 C22 C21 108.72(15) . . ? O23 C22 H22A 109.9 . . ? C21 C22 H22A 109.9 . . ? O23 C22 H22B 109.9 . . ? C21 C22 H22B 109.9 . . ? H22A C22 H22B 108.3 . . ? C24 O23 C22 115.79(14) . . ? O23 C24 C25 113.37(14) . . ? O23 C24 H24A 108.9 . . ? C25 C24 H24A 108.9 . . ? O23 C24 H24B 108.9 . . ? C25 C24 H24B 108.9 . . ? H24A C24 H24B 107.7 . . ? O26 C25 C24 109.02(14) . . ? O26 C25 H25A 109.9 . . ? C24 C25 H25A 109.9 . . ? O26 C25 H25B 109.9 . . ? C24 C25 H25B 109.9 . . ? H25A C25 H25B 108.3 . . ? C25 O26 C27 113.88(12) . . ? O26 C27 C28 108.13(13) . . ? O26 C27 H27A 110.1 . . ? C28 C27 H27A 110.1 . . ? O26 C27 H27B 110.1 . . ? C28 C27 H27B 110.1 . . ? H27A C27 H27B 108.4 . . ? N17 C28 C27 114.43(13) . . ? N17 C28 H28A 108.7 . . ? C27 C28 H28A 108.7 . . ? N17 C28 H28B 108.7 . . ? C27 C28 H28B 108.7 . . ? H28A C28 H28B 107.6 . . ? Si2 N29 Si1 120.31(8) . . ? Si2 N29 Sn1 114.58(6) . . ? Si1 N29 Sn1 121.87(7) . . ? Si1 C30 H30A 109.5 . . ? Si1 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? Si1 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? Si1 C31 H31A 109.5 . . ? Si1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Si1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Si1 C32 H32A 109.5 . . ? Si1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Si1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Si2 C33 H33A 109.5 . . ? Si2 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Si2 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? 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 . . ? 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 N29 Sn1 O1 C2 142.48(12) . . . . ? N17 Sn1 O1 C2 47.07(11) . . . . ? Sn1 O1 C2 C7 -55.16(17) . . . . ? Sn1 O1 C2 C3 127.10(13) . . . . ? O1 C2 C3 C4 179.66(14) . . . . ? C7 C2 C3 C4 1.9(2) . . . . ? O1 C2 C3 C8 0.1(2) . . . . ? C7 C2 C3 C8 -177.61(14) . . . . ? C2 C3 C4 C5 -0.6(2) . . . . ? C8 C3 C4 C5 178.98(15) . . . . ? C3 C4 C5 C6 -0.4(2) . . . . ? C3 C4 C5 C12 179.87(15) . . . . ? C4 C5 C6 C7 0.0(2) . . . . ? C12 C5 C6 C7 179.71(15) . . . . ? C5 C6 C7 C2 1.4(2) . . . . ? C5 C6 C7 C16 -172.47(14) . . . . ? O1 C2 C7 C6 179.82(14) . . . . ? C3 C2 C7 C6 -2.4(2) . . . . ? O1 C2 C7 C16 -6.3(2) . . . . ? C3 C2 C7 C16 171.49(13) . . . . ? C4 C3 C8 C9 -121.32(16) . . . . ? C2 C3 C8 C9 58.19(19) . . . . ? C4 C3 C8 C10 -2.5(2) . . . . ? C2 C3 C8 C10 176.99(15) . . . . ? C4 C3 C8 C11 116.98(17) . . . . ? C2 C3 C8 C11 -63.5(2) . . . . ? C6 C5 C12 C15 -3.5(2) . . . . ? C4 C5 C12 C15 176.15(15) . . . . ? C6 C5 C12 C13 116.26(18) . . . . ? C4 C5 C12 C13 -64.0(2) . . . . ? C6 C5 C12 C14 -123.49(18) . . . . ? C4 C5 C12 C14 56.2(2) . . . . ? C6 C7 C16 N17 -116.33(16) . . . . ? C2 C7 C16 N17 69.72(18) . . . . ? C7 C16 N17 C18 -174.59(13) . . . . ? C7 C16 N17 C28 59.76(17) . . . . ? C7 C16 N17 Sn1 -56.14(14) . . . . ? O1 Sn1 N17 C18 124.93(9) . . . . ? N29 Sn1 N17 C18 31.46(9) . . . . ? O1 Sn1 N17 C28 -110.32(9) . . . . ? N29 Sn1 N17 C28 156.21(9) . . . . ? O1 Sn1 N17 C16 6.90(9) . . . . ? N29 Sn1 N17 C16 -86.57(9) . . . . ? C28 N17 C18 C19 64.48(17) . . . . ? C16 N17 C18 C19 -58.13(16) . . . . ? Sn1 N17 C18 C19 -175.00(10) . . . . ? N17 C18 C19 O20 -159.36(12) . . . . ? C18 C19 O20 C21 160.86(13) . . . . ? C19 O20 C21 C22 -75.55(19) . . . . ? O20 C21 C22 O23 -64.11(19) . . . . ? C21 C22 O23 C24 142.61(15) . . . . ? C22 O23 C24 C25 -90.32(18) . . . . ? O23 C24 C25 O26 70.29(18) . . . . ? C24 C25 O26 C27 170.84(13) . . . . ? C25 O26 C27 C28 167.26(13) . . . . ? C18 N17 C28 C27 46.41(18) . . . . ? C16 N17 C28 C27 168.85(13) . . . . ? Sn1 N17 C28 C27 -75.37(13) . . . . ? O26 C27 C28 N17 -87.01(16) . . . . ? C34 Si2 N29 Si1 -71.05(11) . . . . ? C35 Si2 N29 Si1 53.86(11) . . . . ? C33 Si2 N29 Si1 170.64(9) . . . . ? C34 Si2 N29 Sn1 128.92(8) . . . . ? C35 Si2 N29 Sn1 -106.17(8) . . . . ? C33 Si2 N29 Sn1 10.61(11) . . . . ? C30 Si1 N29 Si2 140.17(10) . . . . ? C31 Si1 N29 Si2 -95.72(11) . . . . ? C32 Si1 N29 Si2 22.62(12) . . . . ? C30 Si1 N29 Sn1 -61.28(11) . . . . ? C31 Si1 N29 Sn1 62.83(11) . . . . ? C32 Si1 N29 Sn1 -178.83(8) . . . . ? O1 Sn1 N29 Si2 172.96(7) . . . . ? N17 Sn1 N29 Si2 -100.14(7) . . . . ? O1 Sn1 N29 Si1 13.28(8) . . . . ? N17 Sn1 N29 Si1 100.17(8) . . . . ? #----------------------------------------------------------------------------# # END OF CIF FILE FOR WLF024 # #----------------------------------------------------------------------------# _database_code_depnum_ccdc_archive 'CCDC 942099'