# Supplementary Material (ESI) for Chemical Science # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Chemical Science' _journal_coden_cambridge 1475 _publ_section_title ;Substituent Effects in Ditetrel Alkyne Analogues: Multiple vs Single Bonded Isomers ; _publ_contact_author_name 'Philip Power' _publ_contact_author_email pppower@ucdavis.edu loop_ _publ_author_name 'Yang Peng.' 'Roland Fischer' 'William Merrill' 'Jelena Fisher' 'Lihung Pu.' 'Bobby Ellis' 'James Fettinger' 'Rolfe H. Herber' 'Philip Power' # Attachment '-4-ClArGe-2.cif.txt' data_tw54 _database_code_depnum_ccdc_archive 'CCDC 771266' #TrackingRef '-4-ClArGe-2.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H72 Cl2 Ge2, 2(C4 H8 O)' _chemical_formula_sum 'C68 H88 Cl2 Ge2 O2' _chemical_formula_weight 1153.46 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'I 2/m' _symmetry_space_group_name_Hall '-I 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 14.3831(17) _cell_length_b 10.9750(13) _cell_length_c 19.628(2) _cell_angle_alpha 90.00 _cell_angle_beta 95.579(2) _cell_angle_gamma 90.00 _cell_volume 3083.8(6) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 4883 _cell_measurement_theta_min 2.34 _cell_measurement_theta_max 25.29 _exptl_crystal_description Plate _exptl_crystal_colour Orange _exptl_crystal_size_max 0.54 _exptl_crystal_size_mid 0.38 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.242 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1220 _exptl_absorpt_coefficient_mu 1.104 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5871 _exptl_absorpt_correction_T_max 0.7776 _exptl_absorpt_process_details 'TWINABS V1.05 (Sheldrick, 2003 (private commu' _exptl_special_details ; An orange plate with approximate orthogonal dimensions 0.54 x 0.38 x 0.24mm3 was placed and optically centered on the Bruker SMART(1) CCD system at -183\%C(90K). Indexing of the unit cell was attempted using a random set of reflections collected from three series of 0.3\% wide omega-scans, 10 seconds per frame, and 25 frames per series that were well distributed in reciprocal space. Four omega-scan data frame series were collected [MoKa] with 0.3\% wide scans, 30 seconds per frame with 606, 455, 606, 391 frames collected per series at varying phi angles (phi=0\%, 90\%, 180\%, 270\%), respectively. The crystal to detector distance was 4.23cm, thus providing a complete sphere of data to 2thetamax=55.22\%. ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD' _diffrn_measurement_method '\w and \f' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 2958 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0437 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.68 _diffrn_reflns_theta_max 25.25 _reflns_number_total 2958 _reflns_number_gt 2331 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Version 5.054) (Bruker, 2002)' _computing_cell_refinement 'SAINT (7.23A) (Bruker, 2008)' _computing_data_reduction 'SAINT (7.23A) (Bruker, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL97 _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. 213_ALERT_2_A Atom C10 has ADP max/min Ratio ..... 7.40 prola 220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 10.00 Ratio 222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 8.27 Ratio #============================================================================== 213_ALERT_2_B Atom C9 has ADP max/min Ratio ..... 5.00 prola #============================================================================== The librational motion of atoms C9 and C10 are expected due to the ligands motion back and forth in the plane. We are 'seeing' a composite atom at both sites. Structural determination and Refinement: All crystallographic calculations were performed on a Personal computer (PC) with a Pentium 3.20GHz processor and 4GB of extended memory. Data collected were corrected for Lorentz and polarization effects and absorption using Blessing's method and merged as incorporated into the program SADABS(2,3). The SHELXTL(4) program package was now implemented to determine, based upon intensity statistics and systematic absences, the centrosymmetric monoclinic space group I2/m (no.12). The structure was determined by direct methods using the program XS(5). All of the non-hydrogen atoms within the molecule of interest were located from a series of difference-Fourier least-square cycles and convergence proceeded quickly. Refinement of the structure was achieved using the program XL(5). There was evidence for minor twinning being present so reflections were thresholded in SMART(1) and these reflections were input into Cellnow(6) that determined the twin relationships between the two components (~75:25) and generated the orientation matrices for the components and output a useable multiple matrice input file for the integration program SAINT(1). Saint was run four times using the output optimized merged matrix file from the previous run. Data collected were now corrected for Lorentz and polarization effects and absorption using Blessing's method and merged as incorporated into the program TWINABS(2,7), generating both HKLF4 and HKLF5 files. Refinement of the structure recommenced using the HKLF5 file with the BASF value about 26%. The HKLF4 and HKLF5 files were now used and the HKLF5 file generated superior results so was implemented through to convergence. All of the full occupancy non-hydrogen atoms were refined anisotropically. One isopropyl group was optimized for disorder. A THF solvent molecule was also located near a special position and was refined at half occupancy. All of the hydrogen atoms were placed in calculated positions throughout the final convergence cycle. The final structure was refined to convergence with R(F)=6.96%, wR(F2)=15.11%, GOF=1.071 for all 2958 unique reflections [R(F)=5.43%, wR(F2)=14.59% for those 2331 data with Fo > 4sigma(Fo)]. A final difference-Fourier map possessed one peak about 1.2e-/A2 that was found to be meaningless while the remainder of the map was featureless indicating that the structure is complete. References: 1. Bruker (2002) SMART (Version 5.054) and SAINT (Version 7.23a). Bruker AXS Inc., Madison, Wisconsin, USA. 2. An Empirical Correction for Absorption Anisotropy, Blessing, R. H. (1995). Acta Cryst., A51, 33-38. 3. Sheldrick, G.M., SADABS Version 2006/1, 'Siemens Area Detector Absorption Correction' Universit\"at G ttingen: G ttingen, Germany. 4. Sheldrick, G.M., (2002). SHELXTL. Version 6.1. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. 5. Sheldrick, G. M., (1997). SHELXS97 and SHELXL97. Universit\"at G ttingen: G ttingen, Germany. 6. Sheldrick, G.M., CELLNOW, Twin matrix determination program, Universit\"at G ttingen: G ttingen, Germany. 7. Sheldrick, G.M., TWINABS Version 1.05 'An Empirical Correction for Absorption Anisotropy applied to Twinned crystals'. Universit\"at G ttingen: G ttingen, Germany, 2003. ; _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^)+(0.0947P)^2^+1.6666P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2958 _refine_ls_number_parameters 213 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0696 _refine_ls_R_factor_gt 0.0543 _refine_ls_wR_factor_ref 0.1511 _refine_ls_wR_factor_gt 0.1459 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.070 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1 Ge 0.92350(4) 0.0000 0.47614(3) 0.0328(2) Uani 1 2 d S . . Cl1 Cl 0.55040(9) 0.0000 0.63888(7) 0.0355(4) Uani 1 2 d S . . C1 C 0.8141(3) 0.0000 0.5297(3) 0.0149(10) Uani 1 2 d S . . C2 C 0.8193(3) 0.0000 0.6014(2) 0.0162(11) Uani 1 2 d S . . C3 C 0.7380(4) 0.0000 0.6347(3) 0.0185(11) Uani 1 2 d S . . H3 H 0.7421 0.0000 0.6833 0.022 Uiso 1 2 calc SR . . C4 C 0.6518(3) 0.0000 0.5973(3) 0.0207(11) Uani 1 2 d S . . C5 C 0.6444(4) 0.0000 0.5270(3) 0.0207(12) Uani 1 2 d S . . H5 H 0.5845 0.0000 0.5018 0.025 Uiso 1 2 calc SR . . C6 C 0.7257(3) 0.0000 0.4923(2) 0.0159(10) Uani 1 2 d S . . C7 C 0.9104(4) 0.0000 0.6449(3) 0.0253(13) Uani 1 2 d S . . C8 C 0.9508(3) -0.1111(6) 0.6664(2) 0.0515(15) Uani 1 1 d D . . C9 C 1.0361(4) -0.1038(10) 0.7090(3) 0.099(3) Uani 1 1 d . A . H9 H 1.0649 -0.1776 0.7251 0.119 Uiso 1 1 calc R . . C10 C 1.0781(6) 0.0000 0.7275(5) 0.152(10) Uani 1 2 d S . . H10 H 1.1372 0.0000 0.7537 0.182 Uiso 1 2 calc PR A . C11 C 0.9005(7) -0.2308(8) 0.6527(6) 0.074(2) Uani 0.46 1 d PDU A 1 H11 H 0.8434 -0.2303 0.6193 0.089 Uiso 0.46 1 calc PR A 1 C12 C 0.8878(11) -0.2653(14) 0.7280(6) 0.089(4) Uani 0.46 1 d PDU A 1 H12A H 0.9403 -0.2330 0.7582 0.133 Uiso 0.46 1 calc PR A 1 H12B H 0.8859 -0.3542 0.7324 0.133 Uiso 0.46 1 calc PR A 1 H12C H 0.8293 -0.2305 0.7409 0.133 Uiso 0.46 1 calc PR A 1 C13 C 0.9853(9) -0.3072(12) 0.6340(7) 0.064(3) Uani 0.46 1 d PDU A 1 H13A H 1.0173 -0.2637 0.5994 0.097 Uiso 0.46 1 calc PR A 1 H13B H 0.9634 -0.3863 0.6156 0.097 Uiso 0.46 1 calc PR A 1 H13C H 1.0287 -0.3199 0.6750 0.097 Uiso 0.46 1 calc PR A 1 C11A C 0.9075(8) -0.2318(6) 0.6438(6) 0.074(2) Uani 0.54 1 d PDU A 2 H11A H 0.8498 -0.2030 0.6160 0.089 Uiso 0.54 1 calc PR A 2 C12A C 0.8639(10) -0.3139(13) 0.6968(6) 0.091(4) Uani 0.54 1 d PDU A 2 H12D H 0.9138 -0.3529 0.7267 0.136 Uiso 0.54 1 calc PR A 2 H12E H 0.8248 -0.3765 0.6727 0.136 Uiso 0.54 1 calc PR A 2 H12F H 0.8255 -0.2639 0.7245 0.136 Uiso 0.54 1 calc PR A 2 C13A C 0.9466(9) -0.3218(10) 0.5925(6) 0.066(3) Uani 0.54 1 d PDU A 2 H13D H 0.9492 -0.2812 0.5483 0.099 Uiso 0.54 1 calc PR A 2 H13E H 0.9057 -0.3931 0.5867 0.099 Uiso 0.54 1 calc PR A 2 H13F H 1.0095 -0.3477 0.6103 0.099 Uiso 0.54 1 calc PR A 2 C14 C 0.7095(3) 0.0000 0.4157(2) 0.0159(11) Uani 1 2 d S . . C15 C 0.6987(2) 0.1110(3) 0.38030(18) 0.0199(8) Uani 1 1 d . . . C16 C 0.6794(3) 0.1087(4) 0.30927(19) 0.0272(9) Uani 1 1 d . . . H16 H 0.6741 0.1834 0.2848 0.033 Uiso 1 1 calc R . . C17 C 0.6678(4) 0.0000 0.2738(3) 0.0303(14) Uani 1 2 d S . . H17 H 0.6521 0.0000 0.2256 0.036 Uiso 1 2 calc SR . . C18 C 0.7037(3) 0.2318(4) 0.4177(2) 0.0305(10) Uani 1 1 d . . . H18 H 0.7295 0.2162 0.4661 0.037 Uiso 1 1 calc R . . C19 C 0.7694(5) 0.3213(5) 0.3861(4) 0.0709(19) Uani 1 1 d . . . H19A H 0.8311 0.2838 0.3850 0.106 Uiso 1 1 calc R . . H19B H 0.7753 0.3959 0.4136 0.106 Uiso 1 1 calc R . . H19C H 0.7439 0.3414 0.3393 0.106 Uiso 1 1 calc R . . C20 C 0.6068(4) 0.2863(5) 0.4191(3) 0.0514(14) Uani 1 1 d . . . H20A H 0.5798 0.3022 0.3721 0.077 Uiso 1 1 calc R . . H20B H 0.6111 0.3628 0.4449 0.077 Uiso 1 1 calc R . . H20C H 0.5668 0.2290 0.4411 0.077 Uiso 1 1 calc R . . O21 O 0.2991(5) 0.5356(6) 0.4402(4) 0.068(3) Uiso 0.50 1 d PD B -1 C21 C 0.3788(8) 0.5610(11) 0.4077(6) 0.076(4) Uiso 0.50 1 d PD B -1 H21A H 0.4353 0.5546 0.4406 0.091 Uiso 0.50 1 calc PR B -1 H21B H 0.3755 0.6447 0.3887 0.091 Uiso 0.50 1 calc PR B -1 C22 C 0.3828(7) 0.4684(9) 0.3506(5) 0.066(4) Uiso 0.50 1 d PD B -1 H22A H 0.4472 0.4536 0.3389 0.079 Uiso 0.50 1 calc PR B -1 H22B H 0.3419 0.4905 0.3089 0.079 Uiso 0.50 1 calc PR B -1 C23 C 0.3442(7) 0.3618(9) 0.3893(6) 0.059(3) Uiso 0.50 1 d PD B -1 H23A H 0.3224 0.2954 0.3576 0.070 Uiso 0.50 1 calc PR B -1 H23B H 0.3921 0.3292 0.4242 0.070 Uiso 0.50 1 calc PR B -1 C24 C 0.2679(7) 0.4140(9) 0.4209(6) 0.055(3) Uiso 0.50 1 d PD B -1 H24A H 0.2544 0.3663 0.4616 0.066 Uiso 0.50 1 calc PR B -1 H24B H 0.2109 0.4169 0.3883 0.066 Uiso 0.50 1 calc PR B -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.0136(3) 0.0671(5) 0.0177(3) 0.000 0.0018(2) 0.000 Cl1 0.0138(7) 0.0712(11) 0.0219(7) 0.000 0.0041(5) 0.000 C1 0.016(3) 0.011(3) 0.018(2) 0.000 0.0020(19) 0.000 C2 0.015(3) 0.018(3) 0.015(2) 0.000 -0.002(2) 0.000 C3 0.020(3) 0.021(3) 0.014(2) 0.000 -0.001(2) 0.000 C4 0.013(3) 0.027(3) 0.024(3) 0.000 0.009(2) 0.000 C5 0.011(2) 0.030(3) 0.021(3) 0.000 -0.003(2) 0.000 C6 0.017(3) 0.015(3) 0.016(2) 0.000 -0.001(2) 0.000 C7 0.015(3) 0.051(4) 0.010(2) 0.000 0.001(2) 0.000 C8 0.025(2) 0.099(5) 0.032(2) 0.031(3) 0.0105(19) 0.026(3) C9 0.028(3) 0.224(10) 0.046(4) 0.072(5) 0.016(3) 0.058(5) C10 0.008(5) 0.42(3) 0.028(5) 0.000 0.003(4) 0.000 C11 0.047(4) 0.051(4) 0.132(7) 0.062(4) 0.048(4) 0.033(3) C12 0.131(11) 0.071(9) 0.066(9) 0.001(6) 0.021(8) -0.067(7) C13 0.073(8) 0.055(6) 0.068(8) -0.004(6) 0.018(6) -0.009(6) C11A 0.047(4) 0.051(4) 0.132(7) 0.062(4) 0.048(4) 0.032(3) C12A 0.133(10) 0.077(9) 0.065(8) 0.000(6) 0.029(8) -0.062(7) C13A 0.077(8) 0.060(5) 0.064(7) -0.009(6) 0.021(6) -0.023(5) C14 0.012(3) 0.019(3) 0.017(2) 0.000 -0.0022(19) 0.000 C15 0.0158(18) 0.024(2) 0.0196(19) 0.0019(16) 0.0011(14) 0.0023(15) C16 0.022(2) 0.036(2) 0.023(2) 0.0129(18) 0.0000(16) 0.0097(17) C17 0.021(3) 0.055(4) 0.015(3) 0.000 -0.001(2) 0.000 C18 0.032(2) 0.019(2) 0.039(2) 0.0010(18) -0.0032(19) 0.0008(17) C19 0.086(5) 0.025(3) 0.105(5) -0.003(3) 0.025(4) -0.015(3) C20 0.057(3) 0.050(3) 0.046(3) -0.010(3) -0.004(2) 0.026(3) _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 C1 1.975(5) . ? Ge1 Ge1 2.3062(12) 5_756 ? Cl1 C4 1.739(5) . ? C1 C2 1.401(7) . ? C1 C6 1.406(7) . ? C2 C3 1.394(7) . ? C2 C7 1.494(7) . ? C3 C4 1.379(7) . ? C3 H3 0.9500 . ? C4 C5 1.374(7) . ? C5 C6 1.410(7) . ? C5 H5 0.9500 . ? C6 C14 1.497(7) . ? C7 C8 1.399(6) 6 ? C7 C8 1.399(6) . ? C8 C9 1.418(8) . ? C8 C11 1.511(8) . ? C8 C11A 1.511(8) . ? C9 C10 1.323(10) . ? C9 H9 0.9500 . ? C10 C9 1.323(10) 6 ? C10 H10 0.9500 . ? C11 C13 1.554(6) . ? C11 C12 1.554(6) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C11A C13A 1.554(6) . ? C11A C12A 1.554(6) . ? C11A H11A 1.0000 . ? C12A H12D 0.9800 . ? C12A H12E 0.9800 . ? C12A H12F 0.9800 . ? C13A H13D 0.9800 . ? C13A H13E 0.9800 . ? C13A H13F 0.9800 . ? C14 C15 1.404(4) . ? C14 C15 1.404(4) 6 ? C15 C16 1.395(5) . ? C15 C18 1.514(5) . ? C16 C17 1.383(5) . ? C16 H16 0.9500 . ? C17 C16 1.383(5) 6 ? C17 H17 0.9500 . ? C18 C20 1.520(6) . ? C18 C19 1.536(6) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? O21 C21 1.394(12) . ? O21 C24 1.447(12) . ? C21 C22 1.518(12) . ? C21 H21A 0.9900 . ? C21 H21B 0.9900 . ? C22 C23 1.529(12) . ? C22 H22A 0.9900 . ? C22 H22B 0.9900 . ? C23 C24 1.430(12) . ? C23 H23A 0.9900 . ? C23 H23B 0.9900 . ? C24 H24A 0.9900 . ? C24 H24B 0.9900 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ge1 Ge1 124.16(15) . 5_756 ? C2 C1 C6 118.8(4) . . ? C2 C1 Ge1 124.6(4) . . ? C6 C1 Ge1 116.7(4) . . ? C3 C2 C1 120.5(4) . . ? C3 C2 C7 117.4(4) . . ? C1 C2 C7 122.1(4) . . ? C4 C3 C2 120.1(5) . . ? C4 C3 H3 120.0 . . ? C2 C3 H3 120.0 . . ? C5 C4 C3 120.9(5) . . ? C5 C4 Cl1 119.0(4) . . ? C3 C4 Cl1 120.1(4) . . ? C4 C5 C6 119.9(5) . . ? C4 C5 H5 120.0 . . ? C6 C5 H5 120.0 . . ? C1 C6 C5 119.9(4) . . ? C1 C6 C14 124.7(4) . . ? C5 C6 C14 115.5(4) . . ? C8 C7 C8 121.4(6) 6 . ? C8 C7 C2 119.3(3) 6 . ? C8 C7 C2 119.3(3) . . ? C7 C8 C9 116.0(6) . . ? C7 C8 C11 121.7(6) . . ? C9 C8 C11 121.8(7) . . ? C7 C8 C11A 121.9(6) . . ? C9 C8 C11A 122.1(7) . . ? C11 C8 C11A 8.0(7) . . ? C10 C9 C8 123.8(8) . . ? C10 C9 H9 118.1 . . ? C8 C9 H9 118.1 . . ? C9 C10 C9 118.8(9) 6 . ? C9 C10 H10 120.6 6 . ? C9 C10 H10 120.6 . . ? C8 C11 C13 97.9(8) . . ? C8 C11 C12 98.1(8) . . ? C13 C11 C12 105.1(6) . . ? C8 C11 H11 117.5 . . ? C13 C11 H11 117.5 . . ? C12 C11 H11 117.5 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C8 C11A C13A 125.6(7) . . ? C8 C11A C12A 119.6(8) . . ? C13A C11A C12A 105.1(6) . . ? C8 C11A H11A 100.4 . . ? C13A C11A H11A 100.4 . . ? C12A C11A H11A 100.4 . . ? C11A C12A H12D 109.5 . . ? C11A C12A H12E 109.5 . . ? H12D C12A H12E 109.5 . . ? C11A C12A H12F 109.5 . . ? H12D C12A H12F 109.5 . . ? H12E C12A H12F 109.5 . . ? C11A C13A H13D 109.5 . . ? C11A C13A H13E 109.5 . . ? H13D C13A H13E 109.5 . . ? C11A C13A H13F 109.5 . . ? H13D C13A H13F 109.5 . . ? H13E C13A H13F 109.5 . . ? C15 C14 C15 120.4(4) . 6 ? C15 C14 C6 119.7(2) . . ? C15 C14 C6 119.7(2) 6 . ? C16 C15 C14 118.7(4) . . ? C16 C15 C18 119.8(3) . . ? C14 C15 C18 121.4(3) . . ? C17 C16 C15 121.5(4) . . ? C17 C16 H16 119.3 . . ? C15 C16 H16 119.3 . . ? C16 C17 C16 119.1(5) 6 . ? C16 C17 H17 120.4 6 . ? C16 C17 H17 120.4 . . ? C15 C18 C20 110.6(4) . . ? C15 C18 C19 111.5(4) . . ? C20 C18 C19 110.9(4) . . ? C15 C18 H18 107.9 . . ? C20 C18 H18 107.9 . . ? C19 C18 H18 107.9 . . ? 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 . . ? C21 O21 C24 108.2(8) . . ? O21 C21 C22 107.2(9) . . ? O21 C21 H21A 110.3 . . ? C22 C21 H21A 110.3 . . ? O21 C21 H21B 110.3 . . ? C22 C21 H21B 110.3 . . ? H21A C21 H21B 108.5 . . ? C21 C22 C23 96.0(8) . . ? C21 C22 H22A 112.6 . . ? C23 C22 H22A 112.6 . . ? C21 C22 H22B 112.6 . . ? C23 C22 H22B 112.6 . . ? H22A C22 H22B 110.1 . . ? C24 C23 C22 103.9(9) . . ? C24 C23 H23A 111.0 . . ? C22 C23 H23A 111.0 . . ? C24 C23 H23B 111.0 . . ? C22 C23 H23B 111.0 . . ? H23A C23 H23B 109.0 . . ? C23 C24 O21 104.6(8) . . ? C23 C24 H24A 110.8 . . ? O21 C24 H24A 110.8 . . ? C23 C24 H24B 110.8 . . ? O21 C24 H24B 110.8 . . ? H24A C24 H24B 108.9 . . ? 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 Ge1 Ge1 C1 C2 0.000(1) 5_756 . . . ? Ge1 Ge1 C1 C6 180.0 5_756 . . . ? C6 C1 C2 C3 0.000(2) . . . . ? Ge1 C1 C2 C3 180.000(1) . . . . ? C6 C1 C2 C7 180.000(1) . . . . ? Ge1 C1 C2 C7 0.000(1) . . . . ? C1 C2 C3 C4 0.000(2) . . . . ? C7 C2 C3 C4 180.000(1) . . . . ? C2 C3 C4 C5 0.000(2) . . . . ? C2 C3 C4 Cl1 180.0 . . . . ? C3 C4 C5 C6 0.000(2) . . . . ? Cl1 C4 C5 C6 180.000(1) . . . . ? C2 C1 C6 C5 0.000(1) . . . . ? Ge1 C1 C6 C5 180.0 . . . . ? C2 C1 C6 C14 180.000(1) . . . . ? Ge1 C1 C6 C14 0.000(1) . . . . ? C4 C5 C6 C1 0.000(1) . . . . ? C4 C5 C6 C14 180.000(1) . . . . ? C3 C2 C7 C8 -88.2(4) . . . 6 ? C1 C2 C7 C8 91.8(4) . . . 6 ? C3 C2 C7 C8 88.2(4) . . . . ? C1 C2 C7 C8 -91.8(4) . . . . ? C8 C7 C8 C9 -2.1(8) 6 . . . ? C2 C7 C8 C9 -178.5(4) . . . . ? C8 C7 C8 C11 170.3(6) 6 . . . ? C2 C7 C8 C11 -6.1(8) . . . . ? C8 C7 C8 C11A 179.6(5) 6 . . . ? C2 C7 C8 C11A 3.3(8) . . . . ? C7 C8 C9 C10 -1.0(10) . . . . ? C11 C8 C9 C10 -173.4(9) . . . . ? C11A C8 C9 C10 177.2(8) . . . . ? C8 C9 C10 C9 4.0(15) . . . 6 ? C7 C8 C11 C13 139.4(6) . . . . ? C9 C8 C11 C13 -48.6(9) . . . . ? C11A C8 C11 C13 46(6) . . . . ? C7 C8 C11 C12 -114.0(7) . . . . ? C9 C8 C11 C12 58.0(9) . . . . ? C11A C8 C11 C12 152(6) . . . . ? C7 C8 C11A C13A 108.3(11) . . . . ? C9 C8 C11A C13A -69.8(13) . . . . ? C11 C8 C11A C13A -160(7) . . . . ? C7 C8 C11A C12A -110.9(10) . . . . ? C9 C8 C11A C12A 70.9(11) . . . . ? C11 C8 C11A C12A -20(6) . . . . ? C1 C6 C14 C15 -92.2(4) . . . . ? C5 C6 C14 C15 87.8(4) . . . . ? C1 C6 C14 C15 92.2(4) . . . 6 ? C5 C6 C14 C15 -87.8(4) . . . 6 ? C15 C14 C15 C16 -1.5(7) 6 . . . ? C6 C14 C15 C16 -177.1(4) . . . . ? C15 C14 C15 C18 176.0(3) 6 . . . ? C6 C14 C15 C18 0.4(6) . . . . ? C14 C15 C16 C17 2.1(6) . . . . ? C18 C15 C16 C17 -175.4(4) . . . . ? C15 C16 C17 C16 -2.6(8) . . . 6 ? C16 C15 C18 C20 72.5(5) . . . . ? C14 C15 C18 C20 -105.0(5) . . . . ? C16 C15 C18 C19 -51.4(5) . . . . ? C14 C15 C18 C19 131.1(5) . . . . ? C24 O21 C21 C22 16.4(12) . . . . ? O21 C21 C22 C23 -36.2(11) . . . . ? C21 C22 C23 C24 43.8(11) . . . . ? C22 C23 C24 O21 -36.6(11) . . . . ? C21 O21 C24 C23 12.9(12) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.206 _refine_diff_density_min -0.472 _refine_diff_density_rms 0.094 # Attachment '-4-ClArSn-2.cif.txt' data_tw4c56s _database_code_depnum_ccdc_archive 'CCDC 771267' #TrackingRef '-4-ClArSn-2.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H72 Cl2 Sn2, 2(C6 H6)' _chemical_formula_sum 'C72 H84 Cl2 Sn2' _chemical_formula_weight 1257.71 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'I 2/m' _symmetry_space_group_name_Hall '-I 2y' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z' 'x+1/2, y+1/2, z+1/2' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z' '-x+1/2, -y+1/2, -z+1/2' 'x+1/2, -y+1/2, z+1/2' _cell_length_a 14.908(4) _cell_length_b 11.003(3) _cell_length_c 19.380(5) _cell_angle_alpha 90.00 _cell_angle_beta 98.493(4) _cell_angle_gamma 90.00 _cell_volume 3144.1(15) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 6516 _cell_measurement_theta_min 2.309 _cell_measurement_theta_max 21.198 _exptl_crystal_description Plate _exptl_crystal_colour 'clear blue' _exptl_crystal_size_max 0.19 _exptl_crystal_size_mid 0.09 _exptl_crystal_size_min 0.01 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.329 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1300 _exptl_absorpt_coefficient_mu 0.920 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8447 _exptl_absorpt_correction_T_max 0.9909 _exptl_absorpt_process_details 'TWINABS V1.05 (Sheldrick, 2003 (private commu' _exptl_special_details ; A blue plate with approximate orthogonal dimensions 0.19 x 0.09 x 0.01mm3 was placed and optically centered on the Bruker SMART APEX(Ref 1) CCD system at -183C. The initial unit cell was indexed using a least-squares analysis of a random set of reflections collected from three series of 0.3deg wide omega-scans, 20 seconds per frame, and 30 frames per series that were well distributed in reciprocal space. Four omega-scan data frame series were collected [MoKa] with 0.3deg wide scans, 60 seconds per frame and 606 frames collected per series at varying phi angles (phi=0deg, 90deg, 180deg, 270deg. The crystal to detector distance was 4.96cm, thus providing a complete sphere of data to 2Thetamax=56.18deg. ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method '\w and \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 2920 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0942 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 23 _diffrn_reflns_theta_min 1.86 _diffrn_reflns_theta_max 25.25 _reflns_number_total 2926 _reflns_number_gt 2110 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (1.0.27) (Bruker, 2004)' _computing_cell_refinement 'SAINT (7.16b) (Bruker, 2004)' _computing_data_reduction 'SAINT (7.16b) (Bruker, 2004)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL97 _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. All crystallographic calculations were performed on a Personal computer (PC) with a Pentium 3.20GHz processor and 1GB of extended memory. During the initial unit cell determination it was quickly recognized that the crystal was twinned. Several crystals were attempted but all possessed the same disorder pattern so a small but diffracting crystal was chosen. Data collection was begun and the relative contributions from the four twin domains were determined using frames from the various data collection series that yielded 5158 reflections via a thresholding routine. These reflections were input into Cellnow(Ref 4) that determined the twin relationships between the four domains and generated the orientation matrices for each and output a useable multiple matrice input file for SAINT(Ref 1). The second domain is rotated, relative to the first, by approximately 179.7?about the real axis [1.000 -0.008 0.992], third relative to first by approximately 179.7?about the real axis [1.000 -0.028 0.525], and fourth to first by approximately 1.2? about the real axis [0.216 1.000 0.268]. The twin matrices corresponding to all domains were input into SAINT and the data were processed. At the completion of the run, the optimized merged matrix was re-input and the data were processed another five times cyclically until improvement became minimal. A total of 13425, 13302, 13523, 13373 reflections were collected for domains one though four respectively, with 12541 involving two domains, 24 involving three, and 212 all four. Data collected were corrected for Lorentz and polarization effects and absorption using Blessings method and merged as incorporated into the program TWINABS(Ref 2-3) yielding 8115 reflections being written to the HKLF5 format file based upon domain one. Any additional reflections were generated due to overlaps. Strip_redV12(Ref 5) was used to remove redundant and bug?reflections. The major domain was now used for structure determination. The SHELXTL(Ref 6) program package was now implemented to determine based upon intensity statistics and systematic absences, the non-standard centrosymmetric monoclinic space group I2/m (no. 15). The structure was determined by direct methods using the program XS(Ref 7). The four domains were determined to exist with a ratio of 0.340:0.228:0.240:0.192. Refinement of the structure was achieved using the program XL(Ref 7). All of the non-hydrogen atoms within the molecule were refined anisotropically. Hydrogen atoms were placed in calculated positions during the final the refinement process. The final structure was refined to convergence with R(F)=10.96%, wR(F2)=24.19%, GOF=1.047 for all 2920 reflections [R(F)=7.92%, wR(F2)=23.01% for those 2110 data with Fo > 4sigma(Fo)]. A final difference-Fourier map produced two large peaks both within one Angstrom of the central Sn atom while the remainder of the map was featureless indicating that the structure is therefore both correct and complete. Due to libration some of the atoms thermal parameters are elongated and this may also be due to the weakness of the data and the twinning present. References: 1. Bruker (2004) SMART APEX (Version 1.027) and SAINT (Version 7.16b). Bruker AXS Inc., Madison, Wisconsin, USA. 2. An Empirical Correction for Absorption Anisotropy, Blessing, R. H. (1995). Acta Cryst., A51, 33-38. 3. Sheldrick, G.M., (private communication) TWINABS An Empirical Correction for Absorption Anisotropy applied to Twinned crystals?v1.05. Universit\"at G ttingen: G ttingen, Germany, 2003. 4. Sheldrick, G.M., (private communication) CELLNOW, Twin matrix determination program, Universit\"at G ttingen: G ttingen, Germany, 2003. 5. Strip_RedV12, Victor Young and William W. Brennessel, University of Minnesota, private communication. 6. Sheldrick, G.M., (2002). SHELXTL. Version 6.1. Siemens Analytical X-ray Instruments Inc., Madison, Wisconsin, USA. 7. Sheldrick, G. M., (1997). SHELXS97 and SHELXL97. Universit\"at G ttingen: G ttingen, Germany. ; _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^)+(0.1619P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2926 _refine_ls_number_parameters 210 _refine_ls_number_restraints 18 _refine_ls_R_factor_all 0.1096 _refine_ls_R_factor_gt 0.0792 _refine_ls_wR_factor_ref 0.2419 _refine_ls_wR_factor_gt 0.2301 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.044 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.08699(7) 0.0000 1.02919(6) 0.0290(4) Uani 1 2 d S . . Cl1 Cl 0.4469(2) 0.0000 0.86047(16) 0.0233(8) Uani 1 2 d S . . C1 C 0.1960(9) 0.0000 0.9672(7) 0.016(3) Uani 1 2 d S . . C2 C 0.2853(8) 0.0000 1.0059(7) 0.018(3) Uani 1 2 d S . . C3 C 0.3608(9) 0.0000 0.9732(7) 0.019(3) Uani 1 2 d SU . . H3 H 0.4198 0.0000 0.9997 0.022 Uiso 1 2 calc SR . . C4 C 0.3498(8) 0.0000 0.9016(6) 0.016(3) Uani 1 2 d S . . C5 C 0.2640(8) 0.0000 0.8604(7) 0.014(3) Uani 1 2 d SU . . H5 H 0.2581 0.0000 0.8109 0.017 Uiso 1 2 calc SR . . C6 C 0.1884(8) 0.0000 0.8939(7) 0.015(3) Uani 1 2 d S . . C7 C 0.2979(8) 0.0000 1.0849(7) 0.017(3) Uani 1 2 d S . . C8 C 0.3041(6) 0.1101(9) 1.1215(5) 0.017(2) Uani 1 1 d . . . C9 C 0.3204(6) 0.1077(10) 1.1945(5) 0.025(2) Uani 1 1 d . . . H9 H 0.3240 0.1823 1.2194 0.030 Uiso 1 1 calc R . . C10 C 0.3313(9) 0.0000 1.2313(7) 0.029(4) Uani 1 2 d S . . H10 H 0.3459 0.0000 1.2807 0.035 Uiso 1 2 calc SR . . C11 C 0.2989(7) 0.2318(9) 1.0845(5) 0.026(2) Uani 1 1 d . . . H11 H 0.2765 0.2159 1.0341 0.032 Uiso 1 1 calc R . . C12 C 0.2300(12) 0.3166(14) 1.1112(9) 0.081(6) Uani 1 1 d . . . H12A H 0.1719 0.2743 1.1095 0.121 Uiso 1 1 calc R . . H12B H 0.2217 0.3893 1.0818 0.121 Uiso 1 1 calc R . . H12C H 0.2523 0.3403 1.1594 0.121 Uiso 1 1 calc R . . C13 C 0.3923(9) 0.2885(13) 1.0884(6) 0.046(3) Uani 1 1 d . . . H13A H 0.4141 0.3131 1.1365 0.069 Uiso 1 1 calc R . . H13B H 0.3888 0.3599 1.0579 0.069 Uiso 1 1 calc R . . H13C H 0.4343 0.2291 1.0732 0.069 Uiso 1 1 calc R . . C14 C 0.0959(8) 0.0000 0.8530(6) 0.016(3) Uani 1 2 d SU . . C15 C 0.0511(6) 0.1106(10) 0.8334(5) 0.024(2) Uani 1 1 d . . . C16 C -0.0353(7) 0.1075(12) 0.7989(6) 0.038(3) Uani 1 1 d . . . H16 H -0.0663 0.1823 0.7885 0.046 Uiso 1 1 calc R . . C17 C -0.0801(12) 0.0000 0.7784(9) 0.049(6) Uani 1 2 d S . . H17 H -0.1388 0.0000 0.7514 0.059 Uiso 1 2 calc SR . . C18 C 0.0991(7) 0.2321(10) 0.8527(7) 0.038(3) Uani 1 1 d . . . H18 H 0.1541 0.2156 0.8876 0.045 Uiso 1 1 calc R . . C19 C 0.0393(11) 0.3193(13) 0.8847(12) 0.096(8) Uani 1 1 d . . . H19A H -0.0208 0.3214 0.8564 0.143 Uiso 1 1 calc R . . H19B H 0.0662 0.4007 0.8864 0.143 Uiso 1 1 calc R . . H19C H 0.0337 0.2926 0.9321 0.143 Uiso 1 1 calc R . . C20 C 0.1295(10) 0.2869(19) 0.7886(8) 0.088(7) Uani 1 1 d . . . H20A H 0.0763 0.3115 0.7557 0.132 Uiso 1 1 calc R . . H20B H 0.1644 0.2266 0.7665 0.132 Uiso 1 1 calc R . . H20C H 0.1676 0.3581 0.8021 0.132 Uiso 1 1 calc R . . C31 C 0.2745(9) 0.4343(19) 0.9358(7) 0.032(8) Uani 0.50 1 d PG . . H31 H 0.2294 0.4109 0.9631 0.038 Uiso 0.50 1 calc PR . . C32 C 0.3218(11) 0.3462(15) 0.9045(10) 0.035(5) Uani 0.50 1 d PG . . H32 H 0.3091 0.2626 0.9104 0.042 Uiso 0.50 1 calc PR . . C33 C 0.3878(9) 0.3805(18) 0.8646(8) 0.039(7) Uani 0.50 1 d PG . . H33 H 0.4200 0.3202 0.8432 0.047 Uiso 0.50 1 calc PR . . C34 C 0.4064(9) 0.5006(19) 0.8560(8) 0.048(5) Uani 1 2 d SG . . H34 H 0.4516 0.5234 0.8287 0.058 Uiso 0.50 1 calc PR . . C35 C 0.3591(13) 0.5910(16) 0.8873(11) 0.061(10) Uani 0.50 1 d PG . . H35 H 0.3721 0.6745 0.8813 0.073 Uiso 0.50 1 calc PR . . C36 C 0.2931(11) 0.5567(17) 0.9273(9) 0.040(9) Uani 0.50 1 d PG . . H36 H 0.2608 0.6169 0.9487 0.048 Uiso 0.50 1 calc PR . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.0165(6) 0.0476(7) 0.0222(6) 0.000 0.0010(3) 0.000 Cl1 0.0171(15) 0.032(2) 0.0207(17) 0.000 0.0023(13) 0.000 C1 0.023(7) 0.009(7) 0.016(6) 0.000 0.002(5) 0.000 C2 0.016(6) 0.017(8) 0.020(7) 0.000 -0.007(5) 0.000 C3 0.019(4) 0.019(4) 0.017(4) 0.000 0.000(3) 0.000 C4 0.011(6) 0.027(8) 0.009(6) 0.000 -0.005(5) 0.000 C5 0.015(3) 0.013(4) 0.013(3) 0.000 -0.001(3) 0.000 C6 0.015(6) 0.007(7) 0.018(6) 0.000 -0.011(5) 0.000 C7 0.005(5) 0.025(8) 0.018(6) 0.000 -0.008(5) 0.000 C8 0.019(4) 0.014(5) 0.018(5) -0.002(4) 0.000(4) 0.000(4) C9 0.027(5) 0.020(6) 0.026(5) -0.005(4) -0.002(4) -0.007(4) C10 0.012(6) 0.058(12) 0.013(7) 0.000 -0.010(5) 0.000 C11 0.035(6) 0.015(6) 0.029(5) -0.005(5) 0.004(5) 0.000(4) C12 0.117(14) 0.048(10) 0.093(12) 0.040(9) 0.071(11) 0.057(10) C13 0.056(8) 0.047(8) 0.033(6) 0.011(6) 0.000(6) -0.017(7) C14 0.015(4) 0.016(4) 0.016(4) 0.000 -0.001(3) 0.000 C15 0.030(5) 0.026(6) 0.016(5) 0.010(4) 0.003(4) 0.005(4) C16 0.025(5) 0.057(9) 0.030(6) 0.025(6) -0.001(4) 0.022(6) C17 0.027(9) 0.095(18) 0.023(8) 0.000 -0.004(7) 0.000 C18 0.036(6) 0.019(6) 0.061(8) 0.018(6) 0.016(6) 0.014(5) C19 0.068(11) 0.022(8) 0.21(2) -0.034(11) 0.066(14) -0.005(7) C20 0.060(9) 0.137(17) 0.058(9) 0.075(11) -0.018(7) -0.051(10) C31 0.030(12) 0.024(18) 0.038(16) -0.010(13) -0.007(11) 0.000(12) C32 0.032(13) 0.029(15) 0.040(13) 0.003(12) -0.008(10) 0.016(11) C33 0.017(12) 0.040(19) 0.057(16) -0.034(14) -0.004(10) 0.007(11) C34 0.027(9) 0.064(15) 0.055(12) 0.000 0.013(8) 0.000 C35 0.05(2) 0.032(19) 0.10(3) -0.001(19) 0.011(18) -0.039(16) C36 0.050(16) 0.05(2) 0.024(14) -0.032(14) 0.009(13) -0.012(15) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C1 2.159(12) . ? Sn1 Sn1 2.672(2) 5_557 ? Cl1 C4 1.753(12) . ? C1 C6 1.408(18) . ? C1 C2 1.428(18) . ? C2 C3 1.371(18) . ? C2 C7 1.516(18) . ? C3 C4 1.374(17) . ? C3 H3 0.9500 . ? C4 C5 1.404(17) . ? C5 C6 1.382(19) . ? C5 H5 0.9500 . ? C6 C14 1.485(17) . ? C7 C8 1.400(11) 6 ? C7 C8 1.400(11) . ? C8 C9 1.400(13) . ? C8 C11 1.515(14) . ? C9 C10 1.380(12) . ? C9 H9 0.9500 . ? C10 C9 1.380(12) 6 ? C10 H10 0.9500 . ? C11 C13 1.517(16) . ? C11 C12 1.533(15) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.413(12) 6 ? C14 C15 1.413(12) . ? C15 C16 1.361(15) . ? C15 C18 1.536(16) . ? C16 C17 1.388(16) . ? C16 H16 0.9500 . ? C17 C16 1.388(16) 6 ? C17 H17 0.9500 . ? C18 C19 1.504(16) . ? C18 C20 1.509(16) . ? C18 H18 1.0000 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C31 C32 1.3900 . ? C31 C36 1.3900 . ? C31 H31 0.9500 . ? C32 C33 1.3900 . ? C32 H32 0.9500 . ? C33 C34 1.3658 . ? C33 H33 0.9500 . ? C34 C35 1.4076 . ? C34 H34 0.9500 . ? C35 C36 1.3900 . ? C35 H35 0.9500 . ? C36 H36 0.9500 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Sn1 Sn1 121.8(4) . 5_557 ? C6 C1 C2 117.4(11) . . ? C6 C1 Sn1 127.3(10) . . ? C2 C1 Sn1 115.3(9) . . ? C3 C2 C1 121.6(12) . . ? C3 C2 C7 118.6(11) . . ? C1 C2 C7 119.9(11) . . ? C2 C3 C4 118.8(12) . . ? C2 C3 H3 120.6 . . ? C4 C3 H3 120.6 . . ? C3 C4 C5 122.6(11) . . ? C3 C4 Cl1 118.4(9) . . ? C5 C4 Cl1 119.0(9) . . ? C6 C5 C4 118.0(11) . . ? C6 C5 H5 121.0 . . ? C4 C5 H5 121.0 . . ? C5 C6 C1 121.6(11) . . ? C5 C6 C14 120.4(11) . . ? C1 C6 C14 117.9(12) . . ? C8 C7 C8 119.9(11) 6 . ? C8 C7 C2 120.0(6) 6 . ? C8 C7 C2 120.0(6) . . ? C9 C8 C7 118.9(9) . . ? C9 C8 C11 118.9(9) . . ? C7 C8 C11 122.1(8) . . ? C10 C9 C8 121.8(10) . . ? C10 C9 H9 119.1 . . ? C8 C9 H9 119.1 . . ? C9 C10 C9 118.4(12) 6 . ? C9 C10 H10 120.8 6 . ? C9 C10 H10 120.8 . . ? C8 C11 C13 111.0(9) . . ? C8 C11 C12 111.6(9) . . ? C13 C11 C12 112.9(11) . . ? C8 C11 H11 107.0 . . ? C13 C11 H11 107.0 . . ? C12 C11 H11 107.0 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C15 118.9(12) 6 . ? C15 C14 C6 120.5(6) 6 . ? C15 C14 C6 120.5(6) . . ? C16 C15 C14 119.1(10) . . ? C16 C15 C18 121.0(10) . . ? C14 C15 C18 119.9(8) . . ? C15 C16 C17 122.9(12) . . ? C15 C16 H16 118.6 . . ? C17 C16 H16 118.6 . . ? C16 C17 C16 116.9(15) . 6 ? C16 C17 H17 121.5 . . ? C16 C17 H17 121.5 6 . ? C19 C18 C20 110.6(14) . . ? C19 C18 C15 111.8(10) . . ? C20 C18 C15 109.5(12) . . ? C19 C18 H18 108.3 . . ? C20 C18 H18 108.3 . . ? C15 C18 H18 108.3 . . ? 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 . . ? C32 C31 C36 120.0 . . ? C32 C31 H31 120.0 . . ? C36 C31 H31 120.0 . . ? C33 C32 C31 120.0 . . ? C33 C32 H32 120.0 . . ? C31 C32 H32 120.0 . . ? C32 C33 C34 120.3 . . ? C32 C33 H33 119.9 . . ? C34 C33 H33 119.9 . . ? C33 C34 C35 120.5 . . ? C33 C34 H34 119.8 . . ? C35 C34 H34 119.8 . . ? C34 C35 C36 119.3 . . ? C34 C35 H35 120.4 . . ? C36 C35 H35 120.4 . . ? C35 C36 C31 120.0 . . ? C35 C36 H36 120.0 . . ? C31 C36 H36 120.0 . . ? _diffrn_measured_fraction_theta_max 0.943 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 0.943 _refine_diff_density_max 3.167 _refine_diff_density_min -1.641 _refine_diff_density_rms 0.225 # Attachment '-4-Me3GeArSn-2.cif.txt' data_jf1604f1 _database_code_depnum_ccdc_archive 'CCDC 771268' #TrackingRef '-4-Me3GeArSn-2.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H90 Ge2 Sn2, 2(C6 H6)' _chemical_formula_sum 'C78 H102 Ge2 Sn2' _chemical_formula_weight 1422.16 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.753(3) _cell_length_b 11.666(3) _cell_length_c 23.950(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.305(3) _cell_angle_gamma 90.00 _cell_volume 3563.3(14) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9917 _cell_measurement_theta_min 2.91 _cell_measurement_theta_max 27.45 _exptl_crystal_description plate _exptl_crystal_colour orange _exptl_crystal_size_max 0.43 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.325 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1468 _exptl_absorpt_coefficient_mu 1.568 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.5520 _exptl_absorpt_correction_T_max 0.8464 _exptl_absorpt_process_details 'SADABS 2008/2 (Sheldrick, 2008)' _exptl_special_details ; An orange plate with approximate orthogonal dimensions 0.43 x 0.28 x 0.11mm3 was placed and optically centered on the Bruker APEXII(1) CCD diffractometer at -183\%C. The initial unit cell was indexed using a least-squares analysis of a random set of reflections collected from three series of 0.3\% wide omega-scans, 10 seconds per frame, and 30 frames per series that were well distributed in reciprocal space. Four omega-scan data frame series were collected [MoKa] with 0.3\% wide scans, 35 seconds per frame at varying phi angles. ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII CCD' _diffrn_measurement_method '\w and \f' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 29735 _diffrn_reflns_av_R_equivalents 0.0374 _diffrn_reflns_av_sigmaI/netI 0.0322 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 2.91 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8144 _reflns_number_gt 6954 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (2009-7) (Bruker, 2009)' _computing_cell_refinement 'SAINT (7.60A) (Bruker, 2008)' _computing_data_reduction 'SAINT (7.60A) (Bruker, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. 220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 7.65 Ratio 222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 7.76 Ratio Several atoms possessed larger amounts of libration. Structural determination and Refinement: The crystal to detector distance was 5.23cm, thus providing a complete sphere of data to 2thetamax=55.06\%. A total of 39321 reflections were collected and corrected for Lorentz and polarization effects and absorption using face indexing and Blessing's method as incorporated into the program SADABS(2,3,6) with 8552 unique. All crystallographic calculations were performed on a Personal computer (PC) with a Pentium 3.20GHz processor and 4GB of extended memory. The SHELXTL(4) program package was implemented to determine the probable space group and set up the initial files. System symmetry, systematic absences and intensity statistics indicated the centrosymmetric monoclinic space group P21/c (no. 14). The structure was determined by direct methods with the successful location of nearly all of the non-hydrogen atoms of the molecule using the program XS5,6. The structure was refined with XL(5,6). The 39321 data collected were merged based upon identical indices yielding 30534 data [R(int)=0.0248] that were further truncated to 2thetamax=55.0\% and merged during least-squares refinement to 8144 unique data [R(int)=0.0374]. A series of least-squares difference-Fourier map cycles were required to locate the remaining hydrogen atoms and understand the whole molecule disorder observed. A variety of twin approaches were also attempted with up to three components to eliminate one large spurious peak. A disorder was optimized initially for Ge1 but when combined with the system symmetry and the large peak and its symmetry related position it is believed that this disorder and odd peak are actually 8% Sn and Ge atoms that are part of a whole molecule disorder. The FRAG4 instruction was used to generate the necessary molecule and this fragment was utilized as a whole molecule disorder at 8%. The 8% benzene portion was not located as it did not refine in the exact same position as the majority portion. All non-hydrogen atoms were refined anisotropically and all hydrogen atoms were allowed to refine freely (xyzU) during the final convergence stage. The final structure was refined to convergence with R(F)=8.09%, wR(F2)=17.12%, GOF=1.214 for all 8144 unique reflections [R(F)=7.06%, wR(F2)=16.83% for those 6954 data with Fo > 4sigma(Fo)]. The final difference-Fourier map was featureless indicating that the structure is both correct and complete. An empirical correction for extinction was also attempted but found to be negative and therefore not applied. References: 1. Bruker (2009) SMART APEX (Version 2009-7) and Bruker (2008) SAINT (Version 7.60A). Bruker AXS Inc., Madison, Wisconsin, USA. 2. An Empirical Correction for Absorption Anisotropy, Blessing, R. H. (1995). Acta Cryst., A51, 33-38. 3. Sheldrick, G.M., SADABS (2008/2), 'Siemens Area Detector Absorption Correction' Universit\"at G ttingen: G ttingen, Germany. 4. Sheldrick, G.M., (2002). SHELXTL. Version 6.1. Bruker AXS Inc., Madison, Wisconsin, USA. 5. Sheldrick, G. M., (1997). SHELXS97 and SHELXL97. Universit\"at G ttingen: G ttingen, Germany. 6. A short history of SHELX, George M. Sheldrick, Acta Cryst. (2008). A64, 112-122 ; _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^)+(0.0287P)^2^+37.2980P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8144 _refine_ls_number_parameters 413 _refine_ls_number_restraints 386 _refine_ls_R_factor_all 0.0809 _refine_ls_R_factor_gt 0.0706 _refine_ls_wR_factor_ref 0.1712 _refine_ls_wR_factor_gt 0.1683 _refine_ls_goodness_of_fit_ref 1.214 _refine_ls_restrained_S_all 1.187 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1_1 Sn 0.02490(4) 1.07101(4) 0.052510(18) 0.02263(13) Uani 0.92 1 d P . 1 Ge1_1 Ge 0.41545(8) 0.77605(9) 0.19677(4) 0.02310(18) Uani 0.92 1 d PU A 1 C1_1 C 0.1447(5) 0.9567(5) 0.0885(2) 0.0162(11) Uani 0.92 1 d PU A 1 C2_1 C 0.2503(5) 0.9822(5) 0.0795(2) 0.0170(11) Uani 0.92 1 d PU A 1 C3_1 C 0.3295(5) 0.9240(5) 0.1088(2) 0.0190(12) Uani 0.92 1 d PU A 1 H3_1 H 0.4008 0.9417 0.1014 0.023 Uiso 0.92 1 calc PR A 1 C4_1 C 0.3057(5) 0.8409(5) 0.1486(2) 0.0190(12) Uani 0.92 1 d PU A 1 C5_1 C 0.2007(5) 0.8157(5) 0.1577(2) 0.0186(12) Uani 0.92 1 d PU A 1 H5_1 H 0.1827 0.7586 0.1842 0.022 Uiso 0.92 1 calc PR A 1 C6_1 C 0.1204(5) 0.8732(5) 0.1284(2) 0.0163(11) Uani 0.92 1 d PU A 1 C7_1 C 0.5085(6) 0.9033(7) 0.2174(4) 0.0388(18) Uani 0.92 1 d PU A 1 H7A_1 H 0.5653 0.8747 0.2413 0.058 Uiso 0.92 1 calc PR A 1 H7B_1 H 0.4685 0.9616 0.2376 0.058 Uiso 0.92 1 calc PR A 1 H7C_1 H 0.5382 0.9372 0.1835 0.058 Uiso 0.92 1 calc PR A 1 C8_1 C 0.4949(7) 0.6604(8) 0.1590(4) 0.045(2) Uani 0.92 1 d PU A 1 H8A_1 H 0.5555 0.6387 0.1820 0.067 Uiso 0.92 1 calc PR A 1 H8B_1 H 0.5191 0.6903 0.1231 0.067 Uiso 0.92 1 calc PR A 1 H8C_1 H 0.4506 0.5929 0.1526 0.067 Uiso 0.92 1 calc PR A 1 C9_1 C 0.3512(3) 0.7155(6) 0.2634(2) 0.0358(17) Uani 0.92 1 d PU A 1 H9A_1 H 0.3179 0.6418 0.2548 0.054 Uiso 0.92 1 calc PR A 1 H9B_1 H 0.2982 0.7695 0.2769 0.054 Uiso 0.92 1 calc PR A 1 H9C_1 H 0.4050 0.7044 0.2923 0.054 Uiso 0.92 1 calc PR A 1 C10_1 C 0.2804(3) 1.0816(3) 0.04315(13) 0.0178(11) Uani 0.92 1 d PRU A 1 C11_1 C 0.3047(3) 1.0666(3) -0.01452(13) 0.0172(11) Uani 0.92 1 d PRU A 1 C12_1 C 0.3369(3) 1.1607(3) -0.04420(13) 0.0214(12) Uani 0.92 1 d PRU A 1 H12_1 H 0.3538 1.1515 -0.0825 0.026 Uiso 0.92 1 calc PR A 1 C13_1 C 0.3456(6) 1.2678(7) -0.0207(3) 0.0236(17) Uani 0.92 1 d PU A 1 H13_1 H 0.3681 1.3308 -0.0427 0.028 Uiso 0.92 1 calc PR A 1 C14_1 C 0.3216(5) 1.2840(6) 0.0352(3) 0.0225(13) Uani 0.92 1 d PU A 1 H14_1 H 0.3280 1.3580 0.0514 0.027 Uiso 0.92 1 calc PR A 1 C15_1 C 0.2879(5) 1.1917(5) 0.0676(2) 0.0191(12) Uani 0.92 1 d PU A 1 C16_1 C 0.2994(5) 0.9490(5) -0.0409(2) 0.0207(12) Uani 0.92 1 d PU A 1 H16_1 H 0.2563 0.8983 -0.0164 0.025 Uiso 0.92 1 calc PR A 1 C17_1 C 0.2488(7) 0.9516(6) -0.0990(3) 0.0339(17) Uani 0.92 1 d PU A 1 H17A_1 H 0.1841 0.9968 -0.0977 0.051 Uiso 0.92 1 calc PR A 1 H17B_1 H 0.2325 0.8732 -0.1109 0.051 Uiso 0.92 1 calc PR A 1 H17C_1 H 0.2975 0.9865 -0.1255 0.051 Uiso 0.92 1 calc PR A 1 C18_1 C 0.4083(6) 0.8985(6) -0.0450(3) 0.0311(16) Uani 0.92 1 d PU A 1 H18A_1 H 0.4532 0.9503 -0.0664 0.047 Uiso 0.92 1 calc PR A 1 H18B_1 H 0.4046 0.8239 -0.0638 0.047 Uiso 0.92 1 calc PR A 1 H18C_1 H 0.4376 0.8884 -0.0074 0.047 Uiso 0.92 1 calc PR A 1 C19_1 C 0.2654(6) 1.2106(6) 0.1292(3) 0.0247(14) Uani 0.92 1 d PU A 1 H19_1 H 0.2256 1.1423 0.1429 0.030 Uiso 0.92 1 calc PR A 1 C20_1 C 0.1980(7) 1.3162(7) 0.1400(3) 0.0379(18) Uani 0.92 1 d PU A 1 H20A_1 H 0.2383 1.3854 0.1312 0.057 Uiso 0.92 1 calc PR A 1 H20B_1 H 0.1774 1.3180 0.1793 0.057 Uiso 0.92 1 calc PR A 1 H20C_1 H 0.1352 1.3132 0.1163 0.057 Uiso 0.92 1 calc PR A 1 C21_1 C 0.3679(6) 1.2169(8) 0.1626(3) 0.0386(18) Uani 0.92 1 d PU A 1 H21A_1 H 0.4091 1.2827 0.1499 0.058 Uiso 0.92 1 calc PR A 1 H21B_1 H 0.4081 1.1463 0.1570 0.058 Uiso 0.92 1 calc PR A 1 H21C_1 H 0.3520 1.2257 0.2024 0.058 Uiso 0.92 1 calc PR A 1 C22_1 C 0.0086(5) 0.8498(5) 0.1443(2) 0.0168(11) Uani 0.92 1 d PU A 1 C23_1 C -0.0371(5) 0.9133(5) 0.1877(2) 0.0177(11) Uani 0.92 1 d PU A 1 C24_1 C -0.1378(5) 0.8850(6) 0.2056(3) 0.0220(13) Uani 0.92 1 d PU A 1 H24_1 H -0.1694 0.9280 0.2346 0.026 Uiso 0.92 1 calc PR A 1 C25_1 C -0.1919(5) 0.7951(6) 0.1814(3) 0.0229(13) Uani 0.92 1 d PU A 1 H25_1 H -0.2600 0.7752 0.1941 0.027 Uiso 0.92 1 calc PR A 1 C26_1 C -0.1459(5) 0.7350(6) 0.1390(3) 0.0199(12) Uani 0.92 1 d PU A 1 H26_1 H -0.1842 0.6739 0.1223 0.024 Uiso 0.92 1 calc PR A 1 C27_1 C -0.0465(5) 0.7586(5) 0.1191(2) 0.0172(11) Uani 0.92 1 d PU A 1 C28_1 C 0.0239(5) 1.0081(5) 0.2171(3) 0.0226(13) Uani 0.92 1 d PU A 1 H28_1 H 0.0814 1.0329 0.1916 0.027 Uiso 0.92 1 calc PR A 1 C29_1 C -0.0426(6) 1.1137(6) 0.2303(3) 0.0334(16) Uani 0.92 1 d PU A 1 H29A_1 H -0.0719 1.1449 0.1956 0.050 Uiso 0.92 1 calc PR A 1 H29B_1 H 0.0014 1.1719 0.2484 0.050 Uiso 0.92 1 calc PR A 1 H29C_1 H -0.0998 1.0920 0.2554 0.050 Uiso 0.92 1 calc PR A 1 C30_1 C 0.0752(6) 0.9603(6) 0.2707(3) 0.0273(14) Uani 0.92 1 d PU A 1 H30A_1 H 0.1120 1.0221 0.2903 0.041 Uiso 0.92 1 calc PR A 1 H30B_1 H 0.1253 0.9000 0.2608 0.041 Uiso 0.92 1 calc PR A 1 H30C_1 H 0.0209 0.9282 0.2949 0.041 Uiso 0.92 1 calc PR A 1 C31_1 C 0.0022(5) 0.6886(5) 0.0721(2) 0.0216(13) Uani 0.92 1 d PU A 1 H31_1 H 0.0574 0.7371 0.0544 0.026 Uiso 0.92 1 calc PR A 1 C32_1 C -0.0768(6) 0.6568(6) 0.0267(3) 0.0269(14) Uani 0.92 1 d PU A 1 H32A_1 H -0.1263 0.6001 0.0413 0.040 Uiso 0.92 1 calc PR A 1 H32B_1 H -0.0398 0.6243 -0.0054 0.040 Uiso 0.92 1 calc PR A 1 H32C_1 H -0.1152 0.7255 0.0149 0.040 Uiso 0.92 1 calc PR A 1 C33_1 C 0.0562(6) 0.5816(6) 0.0954(3) 0.0287(14) Uani 0.92 1 d PU A 1 H33A_1 H 0.1104 0.6045 0.1223 0.043 Uiso 0.92 1 calc PR A 1 H33B_1 H 0.0887 0.5389 0.0647 0.043 Uiso 0.92 1 calc PR A 1 H33C_1 H 0.0044 0.5330 0.1139 0.043 Uiso 0.92 1 calc PR A 1 C41_1 C 0.2043(6) 0.8467(7) 0.4586(3) 0.0349(16) Uani 0.92 1 d PU B 1 H41_1 H 0.1358 0.8184 0.4656 0.042 Uiso 0.92 1 calc PR B 1 C42_1 C 0.2768(7) 0.8516(7) 0.5013(4) 0.0397(18) Uani 0.92 1 d PU B 1 H42_1 H 0.2581 0.8260 0.5375 0.048 Uiso 0.92 1 calc PR B 1 C43_1 C 0.3751(8) 0.8927(7) 0.4920(5) 0.051(2) Uani 0.92 1 d PU B 1 H43_1 H 0.4243 0.8984 0.5219 0.062 Uiso 0.92 1 calc PR B 1 C44_1 C 0.4021(7) 0.9255(7) 0.4394(5) 0.051(2) Uani 0.92 1 d PU B 1 H44_1 H 0.4719 0.9496 0.4323 0.061 Uiso 0.92 1 calc PR B 1 C45_1 C 0.3301(8) 0.9245(7) 0.3962(4) 0.046(2) Uani 0.92 1 d PU B 1 H45_1 H 0.3486 0.9522 0.3603 0.055 Uiso 0.92 1 calc PR B 1 C46_1 C 0.2302(7) 0.8822(7) 0.4062(3) 0.0385(18) Uani 0.92 1 d PU B 1 H46_1 H 0.1802 0.8781 0.3767 0.046 Uiso 0.92 1 calc PR B 1 Sn2_2 Sn 0.0101(5) 0.4265(6) 0.0558(3) 0.0441(15) Uiso 0.08 1 d PG . 2 Ge2_2 Ge 0.3893(8) 0.7552(10) 0.1907(5) 0.022(3) Uiso 0.08 1 d PGU . 2 C1_2 C 0.1304(5) 0.5458(5) 0.0866(3) 0.032(15) Uiso 0.08 1 d PGU . 2 C2_2 C 0.1015(5) 0.6314(6) 0.1241(4) 0.044(16) Uiso 0.08 1 d PGU . 2 C3_2 C 0.1774(6) 0.6970(7) 0.1521(4) 0.039(14) Uiso 0.08 1 d PGU . 2 H3_2 H 0.1555 0.7557 0.1770 0.058 Uiso 0.08 1 d PG . 2 C4_2 C 0.2841(6) 0.6779(7) 0.1442(4) 0.049(19) Uiso 0.08 1 d PGU . 2 C5_2 C 0.3130(5) 0.5925(9) 0.1068(4) 0.047(19) Uiso 0.08 1 d PGU . 2 H5_2 H 0.3853 0.5788 0.1002 0.070 Uiso 0.08 1 d PG . 2 C6_2 C 0.2382(5) 0.5262(8) 0.0785(4) 0.039(16) Uiso 0.08 1 d PGU . 2 C7_2 C 0.3325(11) 0.7563(14) 0.2671(5) 0.07(3) Uiso 0.08 1 d PGU . 2 H7A_2 H 0.3817 0.7957 0.2921 0.108 Uiso 0.08 1 d PG . 2 H7B_2 H 0.3226 0.6773 0.2799 0.108 Uiso 0.08 1 d PG . 2 H7C_2 H 0.2650 0.7964 0.2672 0.108 Uiso 0.08 1 d PG . 2 C8_2 C 0.4146(11) 0.9091(10) 0.1680(7) 0.050(18) Uiso 0.08 1 d PGU . 2 H8A_2 H 0.4591 0.9473 0.1958 0.075 Uiso 0.08 1 d PG . 2 H8B_2 H 0.3477 0.9500 0.1648 0.075 Uiso 0.08 1 d PG . 2 H8C_2 H 0.4499 0.9091 0.1318 0.075 Uiso 0.08 1 d PG . 2 C9_2 C 0.5168(7) 0.6663(12) 0.1905(7) 0.06(3) Uiso 0.08 1 d PGU . 2 H9A_2 H 0.5544 0.6796 0.1555 0.086 Uiso 0.08 1 d PG . 2 H9B_2 H 0.4996 0.5847 0.1937 0.086 Uiso 0.08 1 d PG . 2 H9C_2 H 0.5611 0.6893 0.2221 0.086 Uiso 0.08 1 d PG . 2 C10_2 C -0.0116(6) 0.6453(10) 0.1402(6) 0.035(12) Uiso 0.08 1 d PGU . 2 C11_2 C -0.0783(7) 0.7262(10) 0.1128(8) 0.029(10) Uiso 0.08 1 d PGU . 2 C12_2 C -0.1789(7) 0.7381(15) 0.1319(11) 0.017(12) Uiso 0.08 1 d PGU . 2 H12_2 H -0.2242 0.7914 0.1139 0.025 Uiso 0.08 1 d PG . 2 C13_2 C -0.2163(7) 0.676(2) 0.1756(10) 0.042(12) Uiso 0.08 1 d PGU . 2 H13_2 H -0.2861 0.6879 0.1880 0.063 Uiso 0.08 1 d PG . 2 C14_2 C -0.1528(8) 0.596(2) 0.2022(7) 0.05(2) Uiso 0.08 1 d PGU . 2 H14_2 H -0.1797 0.5523 0.2324 0.077 Uiso 0.08 1 d PG . 2 C15_2 C -0.0508(7) 0.5795(15) 0.1849(5) 0.042(16) Uiso 0.08 1 d PGU . 2 C16_2 C -0.0367(11) 0.7997(7) 0.0660(9) 0.037(12) Uiso 0.08 1 d PGU . 2 H16_2 H 0.0291 0.7637 0.0517 0.056 Uiso 0.08 1 d PG . 2 C17_2 C -0.1144(14) 0.8102(8) 0.0173(11) 0.13(6) Uiso 0.08 1 d PGU . 2 H17A_2 H -0.1422 0.7343 0.0079 0.194 Uiso 0.08 1 d PG . 2 H17B_2 H -0.0785 0.8423 -0.0153 0.194 Uiso 0.08 1 d PG . 2 H17C_2 H -0.1722 0.8609 0.0280 0.194 Uiso 0.08 1 d PG . 2 C18_2 C -0.0102(14) 0.9178(7) 0.0872(11) 0.10(3) Uiso 0.08 1 d PGU . 2 H18A_2 H -0.0727 0.9525 0.1038 0.153 Uiso 0.08 1 d PG . 2 H18B_2 H 0.0138 0.9655 0.0561 0.153 Uiso 0.08 1 d PG . 2 H18C_2 H 0.0454 0.9123 0.1155 0.153 Uiso 0.08 1 d PG . 2 C19_2 C 0.0190(11) 0.4934(16) 0.2160(3) 0.05(2) Uiso 0.08 1 d PGU . 2 H19_2 H 0.0818 0.4779 0.1924 0.074 Uiso 0.08 1 d PG . 2 C20_2 C -0.0352(14) 0.3804(18) 0.2268(3) 0.08(4) Uiso 0.08 1 d PGU . 2 H20A_2 H -0.0891 0.3910 0.2554 0.117 Uiso 0.08 1 d PG . 2 H20B_2 H 0.0163 0.3240 0.2399 0.117 Uiso 0.08 1 d PG . 2 H20C_2 H -0.0681 0.3530 0.1923 0.117 Uiso 0.08 1 d PG . 2 C21_2 C 0.0569(13) 0.5464(19) 0.2709(3) 0.06(3) Uiso 0.08 1 d PGU . 2 H21A_2 H -0.0027 0.5557 0.2962 0.093 Uiso 0.08 1 d PG . 2 H21B_2 H 0.0885 0.6214 0.2635 0.093 Uiso 0.08 1 d PG . 2 H21C_2 H 0.1093 0.4960 0.2882 0.093 Uiso 0.08 1 d PG . 2 C22_2 C 0.2749(5) 0.4279(11) 0.0432(6) 0.051(18) Uiso 0.08 1 d PGU . 2 C23_2 C 0.2918(7) 0.3204(10) 0.0681(8) 0.06(2) Uiso 0.08 1 d PGU . 2 C24_2 C 0.3344(8) 0.2321(14) 0.0363(11) 0.05(2) Uiso 0.08 1 d PGU . 2 H24_2 H 0.3449 0.1588 0.0527 0.070 Uiso 0.08 1 d PG . 2 C25_2 C 0.3617(8) 0.2500(19) -0.0189(11) 0.03(3) Uiso 0.08 1 d PGU . 2 H25_2 H 0.3926 0.1900 -0.0400 0.042 Uiso 0.08 1 d PG . 2 C26_2 C 0.3439(9) 0.354(2) -0.0425(8) 0.042(18) Uiso 0.08 1 d PGU . 2 H26_2 H 0.3611 0.3641 -0.0807 0.063 Uiso 0.08 1 d PG . 2 C27_2 C 0.3019(8) 0.4460(17) -0.0138(6) 0.043(17) Uiso 0.08 1 d PGU . 2 C28_2 C 0.2684(10) 0.3009(7) 0.1297(8) 0.07(3) Uiso 0.08 1 d PGU . 2 H28_2 H 0.2181 0.3617 0.1418 0.101 Uiso 0.08 1 d PG . 2 C29_2 C 0.2184(14) 0.1852(6) 0.1416(10) 0.09(5) Uiso 0.08 1 d PGU . 2 H29A_2 H 0.1521 0.1790 0.1210 0.137 Uiso 0.08 1 d PG . 2 H29B_2 H 0.2049 0.1783 0.1817 0.137 Uiso 0.08 1 d PG . 2 H29C_2 H 0.2659 0.1239 0.1298 0.137 Uiso 0.08 1 d PG . 2 C30_2 C 0.3702(12) 0.3159(9) 0.1639(10) 0.12(5) Uiso 0.08 1 d PGU . 2 H30A_2 H 0.3563 0.2991 0.2033 0.174 Uiso 0.08 1 d PG . 2 H30B_2 H 0.3952 0.3950 0.1603 0.174 Uiso 0.08 1 d PG . 2 H30C_2 H 0.4237 0.2631 0.1499 0.174 Uiso 0.08 1 d PG . 2 C31_2 C 0.2847(12) 0.5626(19) -0.0407(4) 0.05(2) Uiso 0.08 1 d PGU . 2 H31_2 H 0.2292 0.6029 -0.0189 0.078 Uiso 0.08 1 d PG . 2 C32_2 C 0.2454(16) 0.553(2) -0.1007(4) 0.04(2) Uiso 0.08 1 d PGU . 2 H32A_2 H 0.3023 0.5256 -0.1246 0.055 Uiso 0.08 1 d PG . 2 H32B_2 H 0.2220 0.6285 -0.1137 0.055 Uiso 0.08 1 d PG . 2 H32C_2 H 0.1867 0.4989 -0.1024 0.055 Uiso 0.08 1 d PG . 2 C33_2 C 0.3841(13) 0.635(2) -0.0370(5) 0.09(5) Uiso 0.08 1 d PGU . 2 H33A_2 H 0.4070 0.6403 0.0020 0.139 Uiso 0.08 1 d PG . 2 H33B_2 H 0.3696 0.7121 -0.0514 0.139 Uiso 0.08 1 d PG . 2 H33C_2 H 0.4394 0.5993 -0.0593 0.139 Uiso 0.08 1 d PG . 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1_1 0.0285(2) 0.0170(2) 0.0224(2) -0.00011(17) -0.00369(16) 0.00536(18) Ge1_1 0.0218(4) 0.0268(5) 0.0207(4) 0.0094(3) 0.0003(3) 0.0020(4) C1_1 0.023(3) 0.012(3) 0.013(3) -0.003(2) -0.001(2) 0.002(2) C2_1 0.027(3) 0.012(3) 0.012(2) 0.000(2) 0.002(2) 0.001(2) C3_1 0.026(3) 0.020(3) 0.012(2) -0.001(2) 0.005(2) -0.001(2) C4_1 0.026(3) 0.016(3) 0.015(3) 0.002(2) 0.000(2) 0.003(2) C5_1 0.027(3) 0.011(3) 0.018(3) 0.003(2) 0.002(2) 0.000(2) C6_1 0.023(3) 0.014(3) 0.012(2) 0.001(2) 0.001(2) -0.001(2) C7_1 0.036(4) 0.034(4) 0.046(5) 0.010(3) -0.016(3) -0.002(3) C8_1 0.047(5) 0.041(5) 0.047(5) 0.006(4) 0.012(4) 0.016(4) C9_1 0.032(4) 0.052(5) 0.024(4) 0.013(3) -0.002(3) 0.004(4) C10_1 0.021(3) 0.013(3) 0.019(3) 0.004(2) 0.000(2) -0.002(2) C11_1 0.023(3) 0.016(3) 0.012(2) 0.001(2) 0.001(2) -0.001(2) C12_1 0.027(3) 0.018(3) 0.019(3) 0.000(2) 0.002(2) 0.001(2) C13_1 0.030(3) 0.016(3) 0.025(4) 0.010(3) 0.000(3) -0.001(3) C14_1 0.031(3) 0.015(3) 0.022(3) 0.002(2) -0.003(2) -0.002(3) C15_1 0.022(3) 0.018(3) 0.017(3) -0.004(2) 0.003(2) -0.003(2) C16_1 0.035(3) 0.010(3) 0.017(3) 0.001(2) 0.004(2) -0.005(2) C17_1 0.064(5) 0.024(4) 0.014(3) -0.002(2) -0.003(3) -0.009(3) C18_1 0.034(4) 0.016(3) 0.043(4) -0.005(3) 0.013(3) 0.000(3) C19_1 0.035(4) 0.019(3) 0.020(3) -0.001(2) -0.001(3) -0.003(3) C20_1 0.054(5) 0.034(4) 0.026(4) -0.008(3) 0.005(3) 0.006(4) C21_1 0.044(4) 0.045(5) 0.027(4) -0.013(3) -0.010(3) -0.007(4) C22_1 0.024(3) 0.012(3) 0.014(3) 0.003(2) 0.001(2) 0.004(2) C23_1 0.027(3) 0.014(3) 0.011(2) 0.000(2) 0.000(2) 0.004(2) C24_1 0.029(3) 0.022(3) 0.016(3) 0.002(2) 0.005(2) 0.003(3) C25_1 0.024(3) 0.025(3) 0.020(3) 0.006(2) 0.004(2) 0.000(3) C26_1 0.021(3) 0.023(3) 0.016(3) 0.003(2) -0.001(2) -0.002(2) C27_1 0.026(3) 0.014(3) 0.012(3) -0.001(2) 0.000(2) -0.004(2) C28_1 0.029(3) 0.020(3) 0.019(3) -0.003(2) 0.003(2) 0.001(3) C29_1 0.042(4) 0.022(4) 0.036(4) -0.007(3) 0.000(3) 0.004(3) C30_1 0.037(4) 0.022(3) 0.022(3) -0.006(3) -0.004(3) 0.001(3) C31_1 0.032(3) 0.019(3) 0.013(3) -0.001(2) 0.002(2) -0.006(3) C32_1 0.034(4) 0.029(4) 0.018(3) -0.007(3) 0.002(3) -0.009(3) C33_1 0.044(4) 0.016(3) 0.026(3) -0.004(3) 0.002(3) 0.003(3) C41_1 0.032(4) 0.029(4) 0.044(4) -0.002(3) 0.006(3) 0.007(3) C42_1 0.052(5) 0.029(4) 0.038(4) -0.007(3) 0.001(4) 0.014(4) C43_1 0.055(5) 0.030(4) 0.068(6) -0.019(4) -0.015(5) 0.008(4) C44_1 0.039(4) 0.024(4) 0.090(7) -0.015(4) 0.015(5) -0.005(3) C45_1 0.074(6) 0.022(4) 0.042(4) 0.004(3) 0.019(4) -0.002(4) C46_1 0.054(5) 0.029(4) 0.033(4) 0.000(3) 0.001(3) 0.008(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1_1 C1_1 2.200(6) . ? Sn1_1 Sn1_1 3.0754(10) 3_575 ? Ge1_1 C8_1 1.917(8) . ? Ge1_1 C9_1 1.931(3) . ? Ge1_1 C4_1 1.961(6) . ? Ge1_1 C7_1 1.962(8) . ? C1_1 C2_1 1.397(8) . ? C1_1 C6_1 1.401(8) . ? C2_1 C3_1 1.402(8) . ? C2_1 C10_1 1.500(6) . ? C3_1 C4_1 1.394(8) . ? C3_1 H3_1 0.9500 . ? C4_1 C5_1 1.389(9) . ? C5_1 C6_1 1.408(8) . ? C5_1 H5_1 0.9500 . ? C6_1 C22_1 1.503(8) . ? C7_1 H7A_1 0.9800 . ? C7_1 H7B_1 0.9800 . ? C7_1 H7C_1 0.9800 . ? C8_1 H8A_1 0.9800 . ? C8_1 H8B_1 0.9800 . ? C8_1 H8C_1 0.9800 . ? C9_1 H9A_1 0.9800 . ? C9_1 H9B_1 0.9800 . ? C9_1 H9C_1 0.9800 . ? C10_1 C15_1 1.415(7) . ? C10_1 C11_1 1.4279 . ? C11_1 C12_1 1.3719 . ? C11_1 C16_1 1.512(7) . ? C12_1 C13_1 1.375(8) . ? C12_1 H12_1 0.9500 . ? C13_1 C14_1 1.387(9) . ? C13_1 H13_1 0.9500 . ? C14_1 C15_1 1.397(9) . ? C14_1 H14_1 0.9500 . ? C15_1 C19_1 1.521(8) . ? C16_1 C18_1 1.512(9) . ? C16_1 C17_1 1.530(9) . ? C16_1 H16_1 1.0000 . ? C17_1 H17A_1 0.9800 . ? C17_1 H17B_1 0.9800 . ? C17_1 H17C_1 0.9800 . ? C18_1 H18A_1 0.9800 . ? C18_1 H18B_1 0.9800 . ? C18_1 H18C_1 0.9800 . ? C19_1 C20_1 1.525(10) . ? C19_1 C21_1 1.530(10) . ? C19_1 H19_1 1.0000 . ? C20_1 H20A_1 0.9800 . ? C20_1 H20B_1 0.9800 . ? C20_1 H20C_1 0.9800 . ? C21_1 H21A_1 0.9800 . ? C21_1 H21B_1 0.9800 . ? C21_1 H21C_1 0.9800 . ? C22_1 C23_1 1.406(8) . ? C22_1 C27_1 1.409(8) . ? C23_1 C24_1 1.395(9) . ? C23_1 C28_1 1.521(8) . ? C24_1 C25_1 1.381(9) . ? C24_1 H24_1 0.9500 . ? C25_1 C26_1 1.369(9) . ? C25_1 H25_1 0.9500 . ? C26_1 C27_1 1.384(9) . ? C26_1 H26_1 0.9500 . ? C27_1 C31_1 1.526(8) . ? C28_1 C29_1 1.530(9) . ? C28_1 C30_1 1.542(9) . ? C28_1 H28_1 1.0000 . ? C29_1 H29A_1 0.9800 . ? C29_1 H29B_1 0.9800 . ? C29_1 H29C_1 0.9800 . ? C30_1 H30A_1 0.9800 . ? C30_1 H30B_1 0.9800 . ? C30_1 H30C_1 0.9800 . ? C31_1 C32_1 1.524(9) . ? C31_1 C33_1 1.529(9) . ? C31_1 H31_1 1.0000 . ? C32_1 H32A_1 0.9800 . ? C32_1 H32B_1 0.9800 . ? C32_1 H32C_1 0.9800 . ? C33_1 H33A_1 0.9800 . ? C33_1 H33B_1 0.9800 . ? C33_1 H33C_1 0.9800 . ? C41_1 C46_1 1.363(11) . ? C41_1 C42_1 1.376(11) . ? C41_1 H41_1 0.9500 . ? C42_1 C43_1 1.361(13) . ? C42_1 H42_1 0.9500 . ? C43_1 C44_1 1.363(15) . ? C43_1 H43_1 0.9500 . ? C44_1 C45_1 1.379(14) . ? C44_1 H44_1 0.9500 . ? C45_1 C46_1 1.388(13) . ? C45_1 H45_1 0.9500 . ? C46_1 H46_1 0.9500 . ? Sn2_2 C1_2 2.1968 . ? Sn2_2 Sn2_2 3.184(14) 3_565 ? Ge2_2 C8_2 1.9040 . ? Ge2_2 C9_2 1.9287 . ? Ge2_2 C4_2 1.9582 . ? Ge2_2 C7_2 1.9705 . ? C1_2 C2_2 1.3934 . ? C1_2 C6_2 1.4084 . ? C2_2 C3_2 1.4030 . ? C2_2 C10_2 1.5029 . ? C3_2 C4_2 1.3939 . ? C3_2 H3_2 0.9500 . ? C4_2 C5_2 1.3915 . ? C5_2 C6_2 1.3998 . ? C5_2 H5_2 0.9500 . ? C6_2 C22_2 1.5003 . ? C7_2 H7A_2 0.9800 . ? C7_2 H7B_2 0.9800 . ? C7_2 H7C_2 0.9800 . ? C8_2 H8A_2 0.9800 . ? C8_2 H8B_2 0.9800 . ? C8_2 H8C_2 0.9800 . ? C9_2 H9A_2 0.9800 . ? C9_2 H9B_2 0.9800 . ? C9_2 H9C_2 0.9800 . ? C10_2 C15_2 1.4127 . ? C10_2 C11_2 1.4279 . ? C11_2 C12_2 1.3722 . ? C11_2 C16_2 1.5098 . ? C12_2 C13_2 1.3594 . ? C12_2 H12_2 0.9500 . ? C13_2 C14_2 1.3917 . ? C13_2 H13_2 0.9500 . ? C14_2 C15_2 1.3803 . ? C14_2 H14_2 0.9500 . ? C15_2 C19_2 1.5318 . ? C16_2 C18_2 1.5062 . ? C16_2 C17_2 1.5315 . ? C16_2 H16_2 1.0000 . ? C17_2 H17A_2 0.9800 . ? C17_2 H17B_2 0.9800 . ? C17_2 H17C_2 0.9800 . ? C18_2 H18A_2 0.9800 . ? C18_2 H18B_2 0.9800 . ? C18_2 H18C_2 0.9800 . ? C19_2 C20_2 1.5115 . ? C19_2 C21_2 1.5299 . ? C19_2 H19_2 1.0000 . ? C20_2 H20A_2 0.9800 . ? C20_2 H20B_2 0.9800 . ? C20_2 H20C_2 0.9799 . ? C21_2 H21A_2 0.9800 . ? C21_2 H21B_2 0.9800 . ? C21_2 H21C_2 0.9800 . ? C22_2 C23_2 1.4047 . ? C22_2 C27_2 1.4240 . ? C23_2 C24_2 1.3933 . ? C23_2 C28_2 1.5244 . ? C24_2 C25_2 1.3844 . ? C24_2 H24_2 0.9500 . ? C25_2 C26_2 1.3564 . ? C25_2 H25_2 0.9500 . ? C26_2 C27_2 1.3848 . ? C26_2 H26_2 0.9500 . ? C27_2 C31_2 1.5211 . ? C28_2 C29_2 1.5203 . ? C28_2 C30_2 1.5416 . ? C28_2 H28_2 1.0000 . ? C29_2 H29A_2 0.9800 . ? C29_2 H29B_2 0.9800 . ? C29_2 H29C_2 0.9800 . ? C30_2 H30A_2 0.9800 . ? C30_2 H30B_2 0.9800 . ? C30_2 H30C_2 0.9800 . ? C31_2 C32_2 1.5225 . ? C31_2 C33_2 1.5260 . ? C31_2 H31_2 1.0000 . ? C32_2 H32A_2 0.9800 . ? C32_2 H32B_2 0.9800 . ? C32_2 H32C_2 0.9800 . ? C33_2 H33A_2 0.9800 . ? C33_2 H33B_2 0.9800 . ? C33_2 H33C_2 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1_1 Sn1_1 Sn1_1 97.69(14) . 3_575 ? C8_1 Ge1_1 C9_1 111.1(3) . . ? C8_1 Ge1_1 C4_1 111.8(3) . . ? C9_1 Ge1_1 C4_1 108.8(2) . . ? C8_1 Ge1_1 C7_1 109.3(4) . . ? C9_1 Ge1_1 C7_1 109.1(4) . . ? C4_1 Ge1_1 C7_1 106.6(3) . . ? C2_1 C1_1 C6_1 118.1(5) . . ? C2_1 C1_1 Sn1_1 118.6(4) . . ? C6_1 C1_1 Sn1_1 122.2(4) . . ? C1_1 C2_1 C3_1 120.8(5) . . ? C1_1 C2_1 C10_1 120.3(5) . . ? C3_1 C2_1 C10_1 118.6(5) . . ? C4_1 C3_1 C2_1 121.4(6) . . ? C4_1 C3_1 H3_1 119.3 . . ? C2_1 C3_1 H3_1 119.3 . . ? C5_1 C4_1 C3_1 117.8(6) . . ? C5_1 C4_1 Ge1_1 120.8(4) . . ? C3_1 C4_1 Ge1_1 120.9(5) . . ? C4_1 C5_1 C6_1 121.4(5) . . ? C4_1 C5_1 H5_1 119.3 . . ? C6_1 C5_1 H5_1 119.3 . . ? C1_1 C6_1 C5_1 120.5(5) . . ? C1_1 C6_1 C22_1 120.9(5) . . ? C5_1 C6_1 C22_1 118.4(5) . . ? C15_1 C10_1 C11_1 119.8(3) . . ? C15_1 C10_1 C2_1 118.6(4) . . ? C11_1 C10_1 C2_1 121.6(2) . . ? C12_1 C11_1 C10_1 118.0 . . ? C12_1 C11_1 C16_1 121.5(3) . . ? C10_1 C11_1 C16_1 120.4(3) . . ? C11_1 C12_1 C13_1 122.6(3) . . ? C11_1 C12_1 H12_1 118.7 . . ? C13_1 C12_1 H12_1 118.7 . . ? C12_1 C13_1 C14_1 120.1(6) . . ? C12_1 C13_1 H13_1 120.0 . . ? C14_1 C13_1 H13_1 120.0 . . ? C13_1 C14_1 C15_1 120.1(6) . . ? C13_1 C14_1 H14_1 119.9 . . ? C15_1 C14_1 H14_1 119.9 . . ? C14_1 C15_1 C10_1 119.3(5) . . ? C14_1 C15_1 C19_1 119.2(6) . . ? C10_1 C15_1 C19_1 121.4(5) . . ? C11_1 C16_1 C18_1 109.9(5) . . ? C11_1 C16_1 C17_1 112.3(5) . . ? C18_1 C16_1 C17_1 109.4(6) . . ? C11_1 C16_1 H16_1 108.4 . . ? C18_1 C16_1 H16_1 108.4 . . ? C17_1 C16_1 H16_1 108.4 . . ? C15_1 C19_1 C20_1 112.9(6) . . ? C15_1 C19_1 C21_1 110.5(6) . . ? C20_1 C19_1 C21_1 110.7(6) . . ? C15_1 C19_1 H19_1 107.5 . . ? C20_1 C19_1 H19_1 107.5 . . ? C21_1 C19_1 H19_1 107.5 . . ? C23_1 C22_1 C27_1 120.5(6) . . ? C23_1 C22_1 C6_1 119.3(5) . . ? C27_1 C22_1 C6_1 120.0(5) . . ? C24_1 C23_1 C22_1 119.1(6) . . ? C24_1 C23_1 C28_1 120.0(5) . . ? C22_1 C23_1 C28_1 120.8(5) . . ? C25_1 C24_1 C23_1 120.7(6) . . ? C25_1 C24_1 H24_1 119.6 . . ? C23_1 C24_1 H24_1 119.6 . . ? C26_1 C25_1 C24_1 119.0(6) . . ? C26_1 C25_1 H25_1 120.5 . . ? C24_1 C25_1 H25_1 120.5 . . ? C25_1 C26_1 C27_1 123.4(6) . . ? C25_1 C26_1 H26_1 118.3 . . ? C27_1 C26_1 H26_1 118.3 . . ? C26_1 C27_1 C22_1 117.3(5) . . ? C26_1 C27_1 C31_1 121.6(5) . . ? C22_1 C27_1 C31_1 121.1(5) . . ? C23_1 C28_1 C29_1 113.5(6) . . ? C23_1 C28_1 C30_1 109.6(5) . . ? C29_1 C28_1 C30_1 110.6(5) . . ? C23_1 C28_1 H28_1 107.6 . . ? C29_1 C28_1 H28_1 107.6 . . ? C30_1 C28_1 H28_1 107.6 . . ? C32_1 C31_1 C27_1 112.7(5) . . ? C32_1 C31_1 C33_1 110.9(5) . . ? C27_1 C31_1 C33_1 110.6(5) . . ? C32_1 C31_1 H31_1 107.4 . . ? C27_1 C31_1 H31_1 107.4 . . ? C33_1 C31_1 H31_1 107.4 . . ? C46_1 C41_1 C42_1 120.4(8) . . ? C46_1 C41_1 H41_1 119.8 . . ? C42_1 C41_1 H41_1 119.8 . . ? C43_1 C42_1 C41_1 120.6(9) . . ? C43_1 C42_1 H42_1 119.7 . . ? C41_1 C42_1 H42_1 119.7 . . ? C42_1 C43_1 C44_1 119.1(9) . . ? C42_1 C43_1 H43_1 120.5 . . ? C44_1 C43_1 H43_1 120.5 . . ? C43_1 C44_1 C45_1 121.4(8) . . ? C43_1 C44_1 H44_1 119.3 . . ? C45_1 C44_1 H44_1 119.3 . . ? C44_1 C45_1 C46_1 118.8(8) . . ? C44_1 C45_1 H45_1 120.6 . . ? C46_1 C45_1 H45_1 120.6 . . ? C41_1 C46_1 C45_1 119.6(8) . . ? C41_1 C46_1 H46_1 120.2 . . ? C45_1 C46_1 H46_1 120.2 . . ? C1_2 Sn2_2 Sn2_2 89.7(3) . 3_565 ? C8_2 Ge2_2 C9_2 111.2 . . ? C8_2 Ge2_2 C4_2 112.9 . . ? C9_2 Ge2_2 C4_2 109.0 . . ? C8_2 Ge2_2 C7_2 108.8 . . ? C9_2 Ge2_2 C7_2 108.7 . . ? C4_2 Ge2_2 C7_2 106.1 . . ? C2_2 C1_2 C6_2 117.9 . . ? C2_2 C1_2 Sn2_2 118.9 . . ? C6_2 C1_2 Sn2_2 122.1 . . ? C1_2 C2_2 C3_2 121.0 . . ? C1_2 C2_2 C10_2 120.0 . . ? C3_2 C2_2 C10_2 118.6 . . ? C4_2 C3_2 C2_2 121.3 . . ? C4_2 C3_2 H3_2 119.4 . . ? C2_2 C3_2 H3_2 119.4 . . ? C5_2 C4_2 C3_2 117.7 . . ? C5_2 C4_2 Ge2_2 120.9 . . ? C3_2 C4_2 Ge2_2 121.0 . . ? C4_2 C5_2 C6_2 121.8 . . ? C4_2 C5_2 H5_2 119.1 . . ? C6_2 C5_2 H5_2 119.1 . . ? C5_2 C6_2 C1_2 120.4 . . ? C5_2 C6_2 C22_2 118.8 . . ? C1_2 C6_2 C22_2 120.6 . . ? Ge2_2 C7_2 H7A_2 109.5 . . ? Ge2_2 C7_2 H7B_2 109.5 . . ? H7A_2 C7_2 H7B_2 109.5 . . ? Ge2_2 C7_2 H7C_2 109.5 . . ? H7A_2 C7_2 H7C_2 109.5 . . ? H7B_2 C7_2 H7C_2 109.5 . . ? Ge2_2 C8_2 H8A_2 109.5 . . ? Ge2_2 C8_2 H8B_2 109.5 . . ? H8A_2 C8_2 H8B_2 109.5 . . ? Ge2_2 C8_2 H8C_2 109.5 . . ? H8A_2 C8_2 H8C_2 109.5 . . ? H8B_2 C8_2 H8C_2 109.5 . . ? Ge2_2 C9_2 H9A_2 109.5 . . ? Ge2_2 C9_2 H9B_2 109.5 . . ? H9A_2 C9_2 H9B_2 109.5 . . ? Ge2_2 C9_2 H9C_2 109.5 . . ? H9A_2 C9_2 H9C_2 109.5 . . ? H9B_2 C9_2 H9C_2 109.5 . . ? C15_2 C10_2 C11_2 119.7 . . ? C15_2 C10_2 C2_2 118.7 . . ? C11_2 C10_2 C2_2 121.6 . . ? C12_2 C11_2 C10_2 118.0 . . ? C12_2 C11_2 C16_2 121.5 . . ? C10_2 C11_2 C16_2 120.4 . . ? C13_2 C12_2 C11_2 122.4 . . ? C13_2 C12_2 H12_2 118.8 . . ? C11_2 C12_2 H12_2 118.8 . . ? C12_2 C13_2 C14_2 120.3 . . ? C12_2 C13_2 H13_2 119.8 . . ? C14_2 C13_2 H13_2 119.8 . . ? C15_2 C14_2 C13_2 120.2 . . ? C15_2 C14_2 H14_2 119.9 . . ? C13_2 C14_2 H14_2 119.9 . . ? C14_2 C15_2 C10_2 119.4 . . ? C14_2 C15_2 C19_2 119.4 . . ? C10_2 C15_2 C19_2 121.2 . . ? C18_2 C16_2 C11_2 110.3 . . ? C18_2 C16_2 C17_2 109.1 . . ? C11_2 C16_2 C17_2 112.5 . . ? C18_2 C16_2 H16_2 108.3 . . ? C11_2 C16_2 H16_2 108.3 . . ? C17_2 C16_2 H16_2 108.3 . . ? C16_2 C17_2 H17A_2 109.5 . . ? C16_2 C17_2 H17B_2 109.5 . . ? H17A_2 C17_2 H17B_2 109.5 . . ? C16_2 C17_2 H17C_2 109.5 . . ? H17A_2 C17_2 H17C_2 109.5 . . ? H17B_2 C17_2 H17C_2 109.5 . . ? C16_2 C18_2 H18A_2 109.5 . . ? C16_2 C18_2 H18B_2 109.5 . . ? H18A_2 C18_2 H18B_2 109.5 . . ? C16_2 C18_2 H18C_2 109.5 . . ? H18A_2 C18_2 H18C_2 109.5 . . ? H18B_2 C18_2 H18C_2 109.5 . . ? C20_2 C19_2 C21_2 110.3 . . ? C20_2 C19_2 C15_2 113.0 . . ? C21_2 C19_2 C15_2 109.4 . . ? C20_2 C19_2 H19_2 108.0 . . ? C21_2 C19_2 H19_2 108.0 . . ? C15_2 C19_2 H19_2 108.0 . . ? C19_2 C20_2 H20A_2 109.5 . . ? C19_2 C20_2 H20B_2 109.5 . . ? H20A_2 C20_2 H20B_2 109.5 . . ? C19_2 C20_2 H20C_2 109.5 . . ? H20A_2 C20_2 H20C_2 109.5 . . ? H20B_2 C20_2 H20C_2 109.5 . . ? C19_2 C21_2 H21A_2 109.5 . . ? C19_2 C21_2 H21B_2 109.5 . . ? H21A_2 C21_2 H21B_2 109.5 . . ? C19_2 C21_2 H21C_2 109.5 . . ? H21A_2 C21_2 H21C_2 109.5 . . ? H21B_2 C21_2 H21C_2 109.5 . . ? C23_2 C22_2 C27_2 120.1 . . ? C23_2 C22_2 C6_2 119.4 . . ? C27_2 C22_2 C6_2 120.3 . . ? C24_2 C23_2 C22_2 119.2 . . ? C24_2 C23_2 C28_2 119.8 . . ? C22_2 C23_2 C28_2 120.9 . . ? C25_2 C24_2 C23_2 120.7 . . ? C25_2 C24_2 H24_2 119.6 . . ? C23_2 C24_2 H24_2 119.6 . . ? C26_2 C25_2 C24_2 119.3 . . ? C26_2 C25_2 H25_2 120.3 . . ? C24_2 C25_2 H25_2 120.3 . . ? C25_2 C26_2 C27_2 123.4 . . ? C25_2 C26_2 H26_2 118.3 . . ? C27_2 C26_2 H26_2 118.3 . . ? C26_2 C27_2 C22_2 117.2 . . ? C26_2 C27_2 C31_2 122.5 . . ? C22_2 C27_2 C31_2 120.3 . . ? C29_2 C28_2 C23_2 113.5 . . ? C29_2 C28_2 C30_2 110.7 . . ? C23_2 C28_2 C30_2 109.2 . . ? C29_2 C28_2 H28_2 107.7 . . ? C23_2 C28_2 H28_2 107.7 . . ? C30_2 C28_2 H28_2 107.7 . . ? C28_2 C29_2 H29A_2 109.5 . . ? C28_2 C29_2 H29B_2 109.5 . . ? H29A_2 C29_2 H29B_2 109.5 . . ? C28_2 C29_2 H29C_2 109.5 . . ? H29A_2 C29_2 H29C_2 109.5 . . ? H29B_2 C29_2 H29C_2 109.5 . . ? C28_2 C30_2 H30A_2 109.5 . . ? C28_2 C30_2 H30B_2 109.5 . . ? H30A_2 C30_2 H30B_2 109.5 . . ? C28_2 C30_2 H30C_2 109.5 . . ? H30A_2 C30_2 H30C_2 109.5 . . ? H30B_2 C30_2 H30C_2 109.5 . . ? C27_2 C31_2 C32_2 112.4 . . ? C27_2 C31_2 C33_2 110.7 . . ? C32_2 C31_2 C33_2 111.4 . . ? C27_2 C31_2 H31_2 107.4 . . ? C32_2 C31_2 H31_2 107.4 . . ? C33_2 C31_2 H31_2 107.4 . . ? C31_2 C32_2 H32A_2 109.5 . . ? C31_2 C32_2 H32B_2 109.5 . . ? H32A_2 C32_2 H32B_2 109.5 . . ? C31_2 C32_2 H32C_2 109.5 . . ? H32A_2 C32_2 H32C_2 109.5 . . ? H32B_2 C32_2 H32C_2 109.5 . . ? C31_2 C33_2 H33A_2 109.5 . . ? C31_2 C33_2 H33B_2 109.5 . . ? H33A_2 C33_2 H33B_2 109.5 . . ? C31_2 C33_2 H33C_2 109.5 . . ? H33A_2 C33_2 H33C_2 109.5 . . ? H33B_2 C33_2 H33C_2 109.5 . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 3.871 _refine_diff_density_min -1.909 _refine_diff_density_rms 0.149 # Attachment '-4-Me3SiArGe-2.cif.txt' data_rf25ffmi _database_code_depnum_ccdc_archive 'CCDC 771269' #TrackingRef '-4-Me3SiArGe-2.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C66 H90 Ge2 Si2), 0.5(C4 H10 O)' _chemical_formula_sum 'C67 H92.50 Ge2 O0.25 Si2' _chemical_formula_weight 1103.27 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.9150(8) _cell_length_b 45.098(3) _cell_length_c 22.5681(14) _cell_angle_alpha 90.00 _cell_angle_beta 98.6700(10) _cell_angle_gamma 90.00 _cell_volume 12994.3(14) _cell_formula_units_Z 8 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9776 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 22.28 _exptl_crystal_description Block _exptl_crystal_colour Red _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.24 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.128 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4708 _exptl_absorpt_coefficient_mu 0.998 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.7695 _exptl_absorpt_correction_T_max 0.7949 _exptl_absorpt_process_details 'SADABS 2006/1 (Sheldrick, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII CCD' _diffrn_measurement_method '\w and \f' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 90292 _diffrn_reflns_av_R_equivalents 0.1368 _diffrn_reflns_av_sigmaI/netI 0.1249 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -54 _diffrn_reflns_limit_k_max 54 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 1.63 _diffrn_reflns_theta_max 25.25 _reflns_number_total 23543 _reflns_number_gt 13403 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (2.0-2) (Bruker, 2006)' _computing_cell_refinement 'SAINT (7.23A) (Bruker, 2008)' _computing_data_reduction 'SAINT (7.23A) (Bruker, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL97 _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. 220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.34 Ratio 220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 6.30 Ratio 222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 6.11 Ratio 222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 7.30 Ratio 242_ALERT_2_A Check Low Ueq as Compared to Neighbors for Si4 The data are quite weak, Z'=2, and the molecules terphenyl ligands tend to have large amounts of libration. #============================================================================== 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for Si1 242_ALERT_2_B Check Low Ueq as Compared to Neighbors for C13 413_ALERT_2_B Short Inter XH3 .. XHn H15B .. H15K .. 1.96 Ang. #============================================================================== Alert 413- Both hydrogen atoms calculated via HFIX instructions with the former based upon an electron density search about the methyl carbon and the latter idealized completely and at half occupancy. ; _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^)+(0.0888P)^2^+0.3829P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 23543 _refine_ls_number_parameters 1322 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.1435 _refine_ls_R_factor_gt 0.0787 _refine_ls_wR_factor_ref 0.1932 _refine_ls_wR_factor_gt 0.1695 _refine_ls_goodness_of_fit_ref 1.050 _refine_ls_restrained_S_all 1.050 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1 Ge 0.55764(5) 0.131701(15) 0.39711(3) 0.02992(18) Uani 1 1 d . . . Ge2 Ge 0.47835(6) 0.130000(15) 0.47896(3) 0.02925(17) Uani 1 1 d . . . Si1 Si 0.57798(14) 0.03050(4) 0.18298(8) 0.0303(4) Uani 1 1 d . . . Si2 Si 0.48766(14) 0.22231(4) 0.70993(7) 0.0266(4) Uani 1 1 d . . . C1 C 0.5491(4) 0.10287(12) 0.3309(2) 0.0204(13) Uani 1 1 d . . . C2 C 0.6354(5) 0.10340(13) 0.2996(3) 0.0250(14) Uani 1 1 d . . . C3 C 0.6437(5) 0.08266(13) 0.2549(2) 0.0258(14) Uani 1 1 d . . . H3 H 0.7033 0.0832 0.2349 0.031 Uiso 1 1 calc R . . C4 C 0.5665(4) 0.06094(13) 0.2383(2) 0.0237(13) Uani 1 1 d . . . C5 C 0.4785(4) 0.06204(13) 0.2684(2) 0.0222(13) Uani 1 1 d . . . H5 H 0.4234 0.0483 0.2574 0.027 Uiso 1 1 calc R . . C6 C 0.4688(5) 0.08233(12) 0.3134(2) 0.0217(13) Uani 1 1 d . . . C7 C 0.7206(5) 0.12627(14) 0.3156(3) 0.0300(15) Uani 1 1 d . . . C8 C 0.8081(5) 0.11931(17) 0.3588(3) 0.0425(18) Uani 1 1 d . . . C9 C 0.8875(6) 0.1414(2) 0.3705(3) 0.053(2) Uani 1 1 d . . . H9 H 0.9483 0.1374 0.3987 0.064 Uiso 1 1 calc R . . C10 C 0.8779(7) 0.1679(2) 0.3423(4) 0.060(2) Uani 1 1 d . . . H10 H 0.9314 0.1823 0.3515 0.072 Uiso 1 1 calc R . . C11 C 0.7926(6) 0.17429(17) 0.3008(3) 0.047(2) Uani 1 1 d . . . H11 H 0.7878 0.1931 0.2818 0.057 Uiso 1 1 calc R . . C12 C 0.7122(5) 0.15368(14) 0.2859(3) 0.0337(16) Uani 1 1 d . . . C13 C 0.8186(6) 0.08973(18) 0.3874(3) 0.050(2) Uani 1 1 d . . . H13 H 0.7478 0.0803 0.3801 0.061 Uiso 1 1 calc R . . C14 C 0.8529(9) 0.0900(2) 0.4549(4) 0.098(4) Uani 1 1 d . . . H14A H 0.9262 0.0964 0.4638 0.147 Uiso 1 1 calc R . . H14B H 0.8457 0.0701 0.4710 0.147 Uiso 1 1 calc R . . H14C H 0.8088 0.1039 0.4735 0.147 Uiso 1 1 calc R . . C15 C 0.8921(8) 0.0704(3) 0.3553(5) 0.110(4) Uani 1 1 d . . . H15A H 0.8727 0.0724 0.3118 0.165 Uiso 1 1 calc R . . H15B H 0.8854 0.0495 0.3666 0.165 Uiso 1 1 calc R . . H15C H 0.9647 0.0768 0.3670 0.165 Uiso 1 1 calc R . . C16 C 0.6211(6) 0.16122(14) 0.2380(3) 0.0391(18) Uani 1 1 d . . . H16 H 0.5934 0.1421 0.2194 0.047 Uiso 1 1 calc R . . C17 C 0.5325(5) 0.17615(15) 0.2633(3) 0.0411(18) Uani 1 1 d . . . H17A H 0.5108 0.1637 0.2948 0.062 Uiso 1 1 calc R . . H17B H 0.4730 0.1790 0.2313 0.062 Uiso 1 1 calc R . . H17C H 0.5561 0.1954 0.2802 0.062 Uiso 1 1 calc R . . C18 C 0.6511(6) 0.18076(16) 0.1873(3) 0.051(2) Uani 1 1 d . . . H18A H 0.6665 0.2009 0.2024 0.076 Uiso 1 1 calc R . . H18B H 0.5928 0.1813 0.1541 0.076 Uiso 1 1 calc R . . H18C H 0.7132 0.1725 0.1732 0.076 Uiso 1 1 calc R . . C19 C 0.3726(5) 0.08094(13) 0.3422(3) 0.0270(14) Uani 1 1 d . . . C20 C 0.2832(5) 0.09738(14) 0.3185(3) 0.0311(15) Uani 1 1 d . . . C21 C 0.1920(6) 0.09399(17) 0.3450(3) 0.048(2) Uani 1 1 d . . . H21 H 0.1301 0.1045 0.3295 0.057 Uiso 1 1 calc R . . C22 C 0.1926(6) 0.07559(19) 0.3932(3) 0.054(2) Uani 1 1 d . . . H22 H 0.1308 0.0738 0.4111 0.065 Uiso 1 1 calc R . . C23 C 0.2798(6) 0.05950(17) 0.4167(3) 0.046(2) Uani 1 1 d . . . H23 H 0.2776 0.0470 0.4503 0.055 Uiso 1 1 calc R . . C24 C 0.3708(5) 0.06159(14) 0.3912(3) 0.0324(16) Uani 1 1 d . . . C25 C 0.2832(5) 0.11727(15) 0.2640(3) 0.0405(17) Uani 1 1 d . . . H25 H 0.3579 0.1221 0.2613 0.049 Uiso 1 1 calc R . . C26 C 0.2260(6) 0.14638(16) 0.2676(4) 0.057(2) Uani 1 1 d . . . H26A H 0.1511 0.1425 0.2667 0.086 Uiso 1 1 calc R . . H26B H 0.2361 0.1589 0.2335 0.086 Uiso 1 1 calc R . . H26C H 0.2538 0.1565 0.3050 0.086 Uiso 1 1 calc R . . C27 C 0.2387(6) 0.10087(16) 0.2067(3) 0.050(2) Uani 1 1 d . . . H27A H 0.2832 0.0838 0.2012 0.074 Uiso 1 1 calc R . . H27B H 0.2365 0.1143 0.1724 0.074 Uiso 1 1 calc R . . H27C H 0.1676 0.0940 0.2096 0.074 Uiso 1 1 calc R . . C28 C 0.4645(6) 0.04292(15) 0.4148(3) 0.0400(18) Uani 1 1 d . . . H28 H 0.5272 0.0521 0.4010 0.048 Uiso 1 1 calc R . . C29 C 0.4863(7) 0.04089(16) 0.4830(3) 0.061(2) Uani 1 1 d . . . H29A H 0.4837 0.0608 0.5003 0.092 Uiso 1 1 calc R . . H29B H 0.5559 0.0323 0.4954 0.092 Uiso 1 1 calc R . . H29C H 0.4333 0.0283 0.4973 0.092 Uiso 1 1 calc R . . C31 C 0.4973(9) 0.0393(2) 0.1106(4) 0.108(4) Uani 1 1 d . . . H31A H 0.5022 0.0231 0.0823 0.161 Uiso 1 1 calc R . . H31B H 0.5227 0.0577 0.0946 0.161 Uiso 1 1 calc R . . H31C H 0.4242 0.0419 0.1165 0.161 Uiso 1 1 calc R . . C32 C 0.5313(6) -0.00440(15) 0.2128(4) 0.062(3) Uani 1 1 d . . . H32A H 0.4577 -0.0022 0.2179 0.093 Uiso 1 1 calc R . . H32B H 0.5735 -0.0089 0.2516 0.093 Uiso 1 1 calc R . . H32C H 0.5380 -0.0206 0.1846 0.093 Uiso 1 1 calc R . . C33 C 0.7150(6) 0.02487(16) 0.1726(4) 0.056(2) Uani 1 1 d . . . H33A H 0.7579 0.0214 0.2116 0.083 Uiso 1 1 calc R . . H33B H 0.7404 0.0426 0.1541 0.083 Uiso 1 1 calc R . . H33C H 0.7197 0.0077 0.1466 0.083 Uiso 1 1 calc R . . C34 C 0.4968(5) 0.15779(13) 0.5467(2) 0.0229(14) Uani 1 1 d . . . C35 C 0.4511(4) 0.14821(12) 0.5961(2) 0.0217(13) Uani 1 1 d . . . C36 C 0.4511(5) 0.16696(13) 0.6453(2) 0.0249(14) Uani 1 1 d . . . H36 H 0.4195 0.1603 0.6782 0.030 Uiso 1 1 calc R . . C37 C 0.4955(5) 0.19517(13) 0.6478(2) 0.0242(14) Uani 1 1 d . . . C38 C 0.5411(5) 0.20372(13) 0.5981(2) 0.0240(14) Uani 1 1 d . . . H38 H 0.5731 0.2227 0.5989 0.029 Uiso 1 1 calc R . . C39 C 0.5425(4) 0.18641(13) 0.5480(2) 0.0229(13) Uani 1 1 d . . . C40 C 0.3949(5) 0.11924(13) 0.5934(3) 0.0289(15) Uani 1 1 d . . . C41 C 0.2893(6) 0.11779(14) 0.5665(3) 0.0344(16) Uani 1 1 d . . . C42 C 0.2370(6) 0.09063(17) 0.5637(3) 0.048(2) Uani 1 1 d . . . H42 H 0.1659 0.0897 0.5454 0.058 Uiso 1 1 calc R . . C43 C 0.2857(7) 0.06548(19) 0.5867(3) 0.056(2) Uani 1 1 d . . . H43 H 0.2487 0.0472 0.5844 0.067 Uiso 1 1 calc R . . C44 C 0.3883(7) 0.06667(15) 0.6132(3) 0.053(2) Uani 1 1 d . . . H44 H 0.4213 0.0489 0.6291 0.063 Uiso 1 1 calc R . . C45 C 0.4477(6) 0.09353(14) 0.6180(3) 0.0382(18) Uani 1 1 d . . . C46 C 0.5587(6) 0.09504(16) 0.6492(3) 0.052(2) Uani 1 1 d . . . H46 H 0.5832 0.1160 0.6481 0.062 Uiso 1 1 calc R . . C47 C 0.5680(8) 0.0853(2) 0.7152(3) 0.093(3) Uani 1 1 d . . . H47A H 0.5265 0.0987 0.7366 0.139 Uiso 1 1 calc R . . H47B H 0.6416 0.0861 0.7339 0.139 Uiso 1 1 calc R . . H47C H 0.5418 0.0650 0.7172 0.139 Uiso 1 1 calc R . . C48 C 0.6320(7) 0.0753(2) 0.6173(4) 0.087(3) Uani 1 1 d . . . H48A H 0.6077 0.0547 0.6167 0.131 Uiso 1 1 calc R . . H48B H 0.7035 0.0765 0.6390 0.131 Uiso 1 1 calc R . . H48C H 0.6309 0.0823 0.5761 0.131 Uiso 1 1 calc R . . C50 C 0.1578(7) 0.1544(2) 0.5916(4) 0.086(3) Uani 1 1 d . . . H50A H 0.1156 0.1373 0.6002 0.130 Uiso 1 1 calc R . . H50B H 0.1114 0.1706 0.5753 0.130 Uiso 1 1 calc R . . H50C H 0.2011 0.1610 0.6287 0.130 Uiso 1 1 calc R . . C51 C 0.1636(7) 0.14249(18) 0.4835(4) 0.070(3) Uani 1 1 d . . . H51A H 0.2096 0.1375 0.4542 0.105 Uiso 1 1 calc R . . H51B H 0.1279 0.1613 0.4722 0.105 Uiso 1 1 calc R . . H51C H 0.1115 0.1267 0.4843 0.105 Uiso 1 1 calc R . . C52 C 0.5900(5) 0.19857(12) 0.4961(2) 0.0217(13) Uani 1 1 d . . . C53 C 0.6964(4) 0.19586(13) 0.4949(2) 0.0230(13) Uani 1 1 d . . . C54 C 0.7389(5) 0.20789(14) 0.4469(3) 0.0315(15) Uani 1 1 d . . . H54 H 0.8117 0.2061 0.4452 0.038 Uiso 1 1 calc R . . C55 C 0.6729(5) 0.22266(14) 0.4012(3) 0.0309(15) Uani 1 1 d . . . H55 H 0.7012 0.2310 0.3685 0.037 Uiso 1 1 calc R . . C56 C 0.5691(5) 0.22506(13) 0.4034(3) 0.0344(16) Uani 1 1 d . . . H56 H 0.5260 0.2353 0.3722 0.041 Uiso 1 1 calc R . . C57 C 0.5237(5) 0.21304(13) 0.4497(2) 0.0243(14) Uani 1 1 d . . . C58 C 0.7702(5) 0.18095(14) 0.5462(3) 0.0328(15) Uani 1 1 d . . . H58 H 0.7271 0.1670 0.5667 0.039 Uiso 1 1 calc R . . C59 C 0.8161(6) 0.20368(16) 0.5918(3) 0.052(2) Uani 1 1 d . . . H59A H 0.8559 0.2184 0.5725 0.077 Uiso 1 1 calc R . . H59B H 0.8629 0.1938 0.6241 0.077 Uiso 1 1 calc R . . H59C H 0.7595 0.2136 0.6085 0.077 Uiso 1 1 calc R . . C60 C 0.8551(6) 0.16301(19) 0.5238(3) 0.060(2) Uani 1 1 d . . . H60A H 0.8240 0.1504 0.4904 0.090 Uiso 1 1 calc R . . H60B H 0.8900 0.1505 0.5564 0.090 Uiso 1 1 calc R . . H60C H 0.9064 0.1764 0.5102 0.090 Uiso 1 1 calc R . . C61 C 0.4074(5) 0.21702(14) 0.4524(3) 0.0302(15) Uani 1 1 d . . . H61 H 0.3852 0.2011 0.4788 0.036 Uiso 1 1 calc R . . C62 C 0.3884(6) 0.24730(16) 0.4804(3) 0.050(2) Uani 1 1 d . . . H62A H 0.4230 0.2477 0.5222 0.075 Uiso 1 1 calc R . . H62B H 0.3130 0.2504 0.4791 0.075 Uiso 1 1 calc R . . H62C H 0.4170 0.2631 0.4578 0.075 Uiso 1 1 calc R . . C63 C 0.3402(5) 0.21437(16) 0.3904(3) 0.0435(18) Uani 1 1 d . . . H63A H 0.3522 0.2317 0.3660 0.065 Uiso 1 1 calc R . . H63B H 0.2660 0.2135 0.3950 0.065 Uiso 1 1 calc R . . H63C H 0.3594 0.1963 0.3705 0.065 Uiso 1 1 calc R . . C64 C 0.4096(5) 0.20635(14) 0.7653(3) 0.0355(16) Uani 1 1 d . . . H64A H 0.4428 0.1880 0.7819 0.053 Uiso 1 1 calc R . . H64B H 0.3385 0.2020 0.7453 0.053 Uiso 1 1 calc R . . H64C H 0.4065 0.2206 0.7977 0.053 Uiso 1 1 calc R . . C65 C 0.6222(5) 0.23217(14) 0.7475(3) 0.0350(16) Uani 1 1 d . . . H65A H 0.6182 0.2491 0.7742 0.052 Uiso 1 1 calc R . . H65B H 0.6659 0.2373 0.7171 0.052 Uiso 1 1 calc R . . H65C H 0.6530 0.2152 0.7709 0.052 Uiso 1 1 calc R . . C66 C 0.4199(5) 0.25611(14) 0.6747(3) 0.0355(16) Uani 1 1 d . . . H66A H 0.3542 0.2503 0.6498 0.053 Uiso 1 1 calc R . . H66B H 0.4653 0.2660 0.6497 0.053 Uiso 1 1 calc R . . H66C H 0.4048 0.2697 0.7062 0.053 Uiso 1 1 calc R . . C67 C 1.0021(5) 0.41738(13) 0.3626(2) 0.0235(13) Uani 1 1 d . . . Ge3 Ge 0.94597(5) 0.357436(16) 0.46780(3) 0.03309(19) Uani 1 1 d . . . Ge4 Ge 1.04967(5) 0.384237(15) 0.41672(3) 0.03090(18) Uani 1 1 d . . . Si3 Si 1.05327(14) 0.26118(4) 0.69280(7) 0.0279(4) Uani 1 1 d . . . Si4 Si 0.90070(15) 0.49928(4) 0.23734(8) 0.0337(4) Uani 1 1 d . . . C68 C 0.9024(4) 0.41861(12) 0.3275(2) 0.0210(13) Uani 1 1 d . . . C69 C 0.8773(5) 0.44299(12) 0.2909(2) 0.0227(13) Uani 1 1 d . . . H69 H 0.8099 0.4435 0.2673 0.027 Uiso 1 1 calc R . . C70 C 0.9443(5) 0.46683(12) 0.2864(2) 0.0219(13) Uani 1 1 d . . . C71 C 1.0436(5) 0.46456(13) 0.3210(2) 0.0266(14) Uani 1 1 d . . . H71 H 1.0923 0.4802 0.3196 0.032 Uiso 1 1 calc R . . C72 C 1.1855(4) 0.43869(13) 0.3889(3) 0.0262(14) Uani 1 1 d . . . C73 C 1.2606(5) 0.42398(15) 0.3607(3) 0.0340(16) Uani 1 1 d . . . C74 C 1.3644(5) 0.42442(16) 0.3872(3) 0.0390(17) Uani 1 1 d . . . H74 H 1.4155 0.4144 0.3686 0.047 Uiso 1 1 calc R . . C75 C 1.3945(5) 0.43927(16) 0.4404(3) 0.0417(18) Uani 1 1 d . . . H75 H 1.4662 0.4397 0.4578 0.050 Uiso 1 1 calc R . . C76 C 1.3206(5) 0.45345(16) 0.4681(3) 0.0381(17) Uani 1 1 d . . . H76 H 1.3423 0.4635 0.5049 0.046 Uiso 1 1 calc R . . C77 C 1.1366(5) 0.46928(14) 0.4768(3) 0.0321(15) Uani 1 1 d . . . H77 H 1.0652 0.4635 0.4565 0.039 Uiso 1 1 calc R . . C78 C 1.2316(6) 0.40882(15) 0.2996(3) 0.0378(17) Uani 1 1 d . . . H78 H 1.1537 0.4066 0.2928 0.045 Uiso 1 1 calc R . . C79 C 1.0737(5) 0.44004(13) 0.3578(2) 0.0255(14) Uani 1 1 d . . . C80 C 1.2163(5) 0.45347(14) 0.4442(3) 0.0297(15) Uani 1 1 d . . . C81 C 1.1458(5) 0.45951(18) 0.5421(3) 0.050(2) Uani 1 1 d . . . H81A H 1.1403 0.4379 0.5439 0.074 Uiso 1 1 calc R . . H81B H 1.0894 0.4685 0.5604 0.074 Uiso 1 1 calc R . . H81C H 1.2137 0.4658 0.5638 0.074 Uiso 1 1 calc R . . C82 C 0.8231(5) 0.39481(13) 0.3270(2) 0.0243(14) Uani 1 1 d . . . C83 C 0.8248(6) 0.37007(14) 0.2890(3) 0.0386(17) Uani 1 1 d . . . C84 C 0.7434(7) 0.34991(16) 0.2858(3) 0.054(2) Uani 1 1 d . . . H84 H 0.7426 0.3333 0.2598 0.065 Uiso 1 1 calc R . . C85 C 0.6646(7) 0.35314(18) 0.3188(4) 0.063(3) Uani 1 1 d . . . H85 H 0.6094 0.3390 0.3153 0.075 Uiso 1 1 calc R . . C86 C 0.6643(6) 0.37689(16) 0.3575(3) 0.0427(18) Uani 1 1 d . . . H86 H 0.6096 0.3787 0.3811 0.051 Uiso 1 1 calc R . . C87 C 0.7421(5) 0.39794(13) 0.3621(3) 0.0269(14) Uani 1 1 d . . . C88 C 0.9108(6) 0.36644(15) 0.2505(3) 0.048(2) Uani 1 1 d . . . H88 H 0.9671 0.3809 0.2658 0.058 Uiso 1 1 calc R . . C89 C 0.8725(8) 0.37465(19) 0.1851(3) 0.076(3) Uani 1 1 d . . . H89A H 0.8105 0.3628 0.1700 0.114 Uiso 1 1 calc R . . H89B H 0.9280 0.3706 0.1610 0.114 Uiso 1 1 calc R . . H89C H 0.8545 0.3958 0.1825 0.114 Uiso 1 1 calc R . . C90 C 0.9610(7) 0.33578(17) 0.2557(4) 0.069(3) Uani 1 1 d . . . H90A H 0.9949 0.3325 0.2970 0.104 Uiso 1 1 calc R . . H90B H 1.0135 0.3345 0.2286 0.104 Uiso 1 1 calc R . . H90C H 0.9070 0.3207 0.2448 0.104 Uiso 1 1 calc R . . C91 C 0.7397(5) 0.42480(14) 0.4032(3) 0.0311(15) Uani 1 1 d . . . H91 H 0.8117 0.4335 0.4103 0.037 Uiso 1 1 calc R . . C92 C 0.7100(5) 0.41653(16) 0.4639(3) 0.0441(18) Uani 1 1 d . . . H92A H 0.6364 0.4104 0.4587 0.066 Uiso 1 1 calc R . . H92B H 0.7200 0.4337 0.4907 0.066 Uiso 1 1 calc R . . H92C H 0.7545 0.4002 0.4813 0.066 Uiso 1 1 calc R . . C93 C 0.6651(5) 0.44845(16) 0.3733(3) 0.0444(19) Uani 1 1 d . . . H93A H 0.6900 0.4555 0.3368 0.067 Uiso 1 1 calc R . . H93B H 0.6625 0.4651 0.4010 0.067 Uiso 1 1 calc R . . H93C H 0.5949 0.4400 0.3629 0.067 Uiso 1 1 calc R . . C94 C 0.9884(4) 0.32997(13) 0.5346(2) 0.0228(13) Uani 1 1 d . . . C95 C 1.0769(5) 0.31174(13) 0.5395(2) 0.0259(14) Uani 1 1 d . . . C96 C 1.0970(5) 0.29204(13) 0.5874(2) 0.0255(14) Uani 1 1 d . . . H96 H 1.1580 0.2800 0.5908 0.031 Uiso 1 1 calc R . . C97 C 1.0307(5) 0.28937(12) 0.6307(2) 0.0224(13) Uani 1 1 d . . . C98 C 0.9422(5) 0.30736(12) 0.6243(2) 0.0250(14) Uani 1 1 d . . . H98 H 0.8962 0.3060 0.6533 0.030 Uiso 1 1 calc R . . C99 C 0.6667(6) 0.30522(15) 0.4455(3) 0.049(2) Uani 1 1 d . . . H99A H 0.5920 0.3090 0.4457 0.073 Uiso 1 1 calc R . . H99B H 0.6752 0.2864 0.4251 0.073 Uiso 1 1 calc R . . H99C H 0.6965 0.3213 0.4243 0.073 Uiso 1 1 calc R . . C100 C 0.9212(5) 0.38586(13) 0.6358(3) 0.0289(14) Uani 1 1 d . . . H100 H 0.9803 0.3725 0.6296 0.035 Uiso 1 1 calc R . . C101 C 0.7233(5) 0.30357(13) 0.5099(3) 0.0272(14) Uani 1 1 d . . . H101 H 0.7972 0.2974 0.5085 0.033 Uiso 1 1 calc R . . C102 C 0.9182(5) 0.32749(12) 0.5766(2) 0.0234(13) Uani 1 1 d . . . C103 C 0.7264(5) 0.33328(13) 0.5411(2) 0.0236(13) Uani 1 1 d . . . C104 C 0.8193(5) 0.34518(13) 0.5723(2) 0.0248(14) Uani 1 1 d . . . C105 C 0.8209(4) 0.37222(13) 0.6034(2) 0.0229(13) Uani 1 1 d . . . C106 C 0.7258(5) 0.38663(13) 0.6043(3) 0.0290(15) Uani 1 1 d . . . H106 H 0.7246 0.4045 0.6265 0.035 Uiso 1 1 calc R . . C107 C 0.6326(5) 0.37542(14) 0.5737(3) 0.0320(15) Uani 1 1 d . . . H107 H 0.5685 0.3857 0.5741 0.038 Uiso 1 1 calc R . . C108 C 0.6348(5) 0.34893(13) 0.5424(3) 0.0303(15) Uani 1 1 d . . . H108 H 0.5712 0.3413 0.5212 0.036 Uiso 1 1 calc R . . C109 C 0.9199(6) 0.38813(17) 0.7033(3) 0.052(2) Uani 1 1 d . . . H10A H 0.9887 0.3947 0.7233 0.078 Uiso 1 1 calc R . . H10B H 0.9035 0.3687 0.7189 0.078 Uiso 1 1 calc R . . H10C H 0.8665 0.4025 0.7110 0.078 Uiso 1 1 calc R . . C110 C 1.1115(5) 0.29239(13) 0.4412(3) 0.0305(15) Uani 1 1 d . . . C111 C 1.1438(5) 0.31128(13) 0.4906(3) 0.0265(14) Uani 1 1 d . . . C112 C 1.2329(5) 0.32958(14) 0.4937(3) 0.0298(15) Uani 1 1 d . . . C113 C 1.3448(6) 0.33202(17) 0.5942(3) 0.050(2) Uani 1 1 d . . . H11A H 1.3119 0.3137 0.6053 0.076 Uiso 1 1 calc R . . H11B H 1.3633 0.3444 0.6299 0.076 Uiso 1 1 calc R . . H11C H 1.4082 0.3272 0.5772 0.076 Uiso 1 1 calc R . . C114 C 1.2569(6) 0.31056(16) 0.3973(3) 0.0436(19) Uani 1 1 d . . . H114 H 1.2967 0.3102 0.3652 0.052 Uiso 1 1 calc R . . C115 C 1.1695(6) 0.29261(15) 0.3940(3) 0.0418(18) Uani 1 1 d . . . H115 H 1.1492 0.2805 0.3598 0.050 Uiso 1 1 calc R . . C116 C 1.2882(5) 0.32881(15) 0.4451(3) 0.0397(18) Uani 1 1 d . . . H116 H 1.3481 0.3411 0.4452 0.048 Uiso 1 1 calc R . . C117 C 1.2670(5) 0.34904(14) 0.5471(3) 0.0348(16) Uani 1 1 d . . . H117 H 1.2034 0.3535 0.5658 0.042 Uiso 1 1 calc R . . C118 C 1.3139(5) 0.37867(15) 0.5322(3) 0.0453(19) Uani 1 1 d . . . H11D H 1.3815 0.3753 0.5186 0.068 Uiso 1 1 calc R . . H11E H 1.3241 0.3912 0.5681 0.068 Uiso 1 1 calc R . . H11F H 1.2662 0.3886 0.5004 0.068 Uiso 1 1 calc R . . C119 C 0.9402(7) 0.2739(2) 0.3822(3) 0.079(3) Uani 1 1 d . . . H11G H 0.9056 0.2933 0.3808 0.118 Uiso 1 1 calc R . . H11H H 0.8876 0.2582 0.3818 0.118 Uiso 1 1 calc R . . H11I H 0.9763 0.2717 0.3472 0.118 Uiso 1 1 calc R . . C120 C 1.0199(5) 0.27151(15) 0.4396(3) 0.0360(16) Uani 1 1 d . . . H120 H 0.9822 0.2774 0.4734 0.043 Uiso 1 1 calc R . . C121 C 0.9922(7) 0.52991(16) 0.2528(4) 0.069(3) Uani 1 1 d . . . H12A H 1.0588 0.5247 0.2397 0.104 Uiso 1 1 calc R . . H12B H 1.0041 0.5340 0.2960 0.104 Uiso 1 1 calc R . . H12C H 0.9632 0.5476 0.2312 0.104 Uiso 1 1 calc R . . C122 C 0.7724(7) 0.5114(2) 0.2532(6) 0.131(6) Uani 1 1 d . . . H12D H 0.7751 0.5139 0.2966 0.197 Uiso 1 1 calc R . . H12E H 0.7197 0.4964 0.2386 0.197 Uiso 1 1 calc R . . H12F H 0.7538 0.5303 0.2330 0.197 Uiso 1 1 calc R . . C123 C 0.9262(5) 0.25354(14) 0.7188(3) 0.0338(16) Uani 1 1 d . . . H12G H 0.8719 0.2504 0.6840 0.051 Uiso 1 1 calc R . . H12H H 0.9069 0.2705 0.7421 0.051 Uiso 1 1 calc R . . H12I H 0.9326 0.2357 0.7439 0.051 Uiso 1 1 calc R . . C124 C 1.1058(5) 0.22636(14) 0.6633(3) 0.0401(17) Uani 1 1 d . . . H12J H 1.1195 0.2118 0.6957 0.060 Uiso 1 1 calc R . . H12K H 1.1710 0.2308 0.6479 0.060 Uiso 1 1 calc R . . H12L H 1.0543 0.2183 0.6310 0.060 Uiso 1 1 calc R . . C125 C 1.1497(7) 0.27568(17) 0.7562(3) 0.061(2) Uani 1 1 d . . . H12M H 1.1224 0.2939 0.7717 0.091 Uiso 1 1 calc R . . H12N H 1.2162 0.2799 0.7420 0.091 Uiso 1 1 calc R . . H12O H 1.1610 0.2608 0.7882 0.091 Uiso 1 1 calc R . . C126 C 0.6732(6) 0.28000(14) 0.5447(3) 0.0394(17) Uani 1 1 d . . . H12P H 0.7150 0.2774 0.5843 0.059 Uiso 1 1 calc R . . H12Q H 0.6700 0.2612 0.5228 0.059 Uiso 1 1 calc R . . H12R H 0.6021 0.2862 0.5493 0.059 Uiso 1 1 calc R . . C127 C 0.2289(5) 0.14554(16) 0.5457(3) 0.0457(19) Uani 1 1 d . . . H127 H 0.2806 0.1619 0.5438 0.055 Uiso 1 1 calc R . . C128 C 0.8906(11) 0.4882(2) 0.1576(3) 0.117(5) Uani 1 1 d . . . H12S H 0.8832 0.5060 0.1323 0.176 Uiso 1 1 calc R . . H12T H 0.8293 0.4754 0.1470 0.176 Uiso 1 1 calc R . . H12U H 0.9540 0.4774 0.1515 0.176 Uiso 1 1 calc R . . C129 C 1.2761(8) 0.37840(18) 0.2967(4) 0.073(3) Uani 1 1 d . . . H12V H 1.2409 0.3682 0.2609 0.109 Uiso 1 1 calc R . . H12W H 1.2653 0.3672 0.3325 0.109 Uiso 1 1 calc R . . H12$ H 1.3513 0.3798 0.2949 0.109 Uiso 1 1 calc R . . C130 C 1.2585(8) 0.4278(2) 0.2505(3) 0.080(3) Uani 1 1 d . . . H13A H 1.3348 0.4294 0.2536 0.120 Uiso 1 1 calc R . . H13B H 1.2286 0.4477 0.2537 0.120 Uiso 1 1 calc R . . H13C H 1.2298 0.4191 0.2118 0.120 Uiso 1 1 calc R . . C131 C 1.1454(6) 0.50262(16) 0.4720(3) 0.052(2) Uani 1 1 d . . . H13D H 1.2176 0.5087 0.4864 0.078 Uiso 1 1 calc R . . H13E H 1.0981 0.5121 0.4963 0.078 Uiso 1 1 calc R . . H13F H 1.1262 0.5086 0.4300 0.078 Uiso 1 1 calc R . . C132 C 1.0555(6) 0.23960(18) 0.4516(5) 0.077(3) Uani 1 1 d . . . H13G H 1.1033 0.2340 0.4237 0.116 Uiso 1 1 calc R . . H13H H 0.9944 0.2264 0.4460 0.116 Uiso 1 1 calc R . . H13I H 1.0917 0.2378 0.4929 0.116 Uiso 1 1 calc R . . C133 C 0.9429(5) 0.41614(15) 0.6106(3) 0.0406(17) Uani 1 1 d . . . H13J H 0.9350 0.4150 0.5668 0.061 Uiso 1 1 calc R . . H13K H 1.0145 0.4223 0.6265 0.061 Uiso 1 1 calc R . . H13L H 0.8932 0.4306 0.6223 0.061 Uiso 1 1 calc R . . C134 C 0.4523(6) 0.01154(15) 0.3885(3) 0.054(2) Uani 1 1 d . . . H13M H 0.3880 0.0026 0.3984 0.081 Uiso 1 1 calc R . . H13N H 0.5126 -0.0005 0.4053 0.081 Uiso 1 1 calc R . . H13O H 0.4485 0.0126 0.3448 0.081 Uiso 1 1 calc R . . C151 C 0.0161(17) 0.49520(15) -0.0026(4) 0.123(8) Uiso 0.50 1 d PRD A -1 H15D H -0.0012 0.4829 0.0304 0.184 Uiso 0.50 1 calc PR B -1 H15E H -0.0026 0.4846 -0.0406 0.184 Uiso 0.50 1 calc PR C -1 H15F H -0.0232 0.5138 -0.0039 0.184 Uiso 0.50 1 calc PR D -1 C152 C 0.1253(13) 0.5014(4) 0.0068(7) 0.075(5) Uiso 0.50 1 d PD A -1 H15G H 0.1655 0.4846 -0.0064 0.090 Uiso 0.50 1 calc PR A -1 H15H H 0.1408 0.5195 -0.0152 0.090 Uiso 0.50 1 calc PR A -1 O153 O 0.1480(9) 0.5055(3) 0.0667(5) 0.075(3) Uiso 0.50 1 d PD A -1 C154 C 0.2493(10) 0.5142(3) 0.0812(6) 0.044(4) Uiso 0.50 1 d PD A -1 H15I H 0.2572 0.5352 0.0698 0.053 Uiso 0.50 1 calc PR A -1 H15J H 0.2956 0.5018 0.0602 0.053 Uiso 0.50 1 calc PR A -1 C155 C 0.2755(14) 0.5107(4) 0.1447(7) 0.072(5) Uiso 0.50 1 d PD A -1 H15K H 0.2370 0.5254 0.1649 0.108 Uiso 0.50 1 calc PR A -1 H15L H 0.3509 0.5137 0.1565 0.108 Uiso 0.50 1 calc PR A -1 H15M H 0.2564 0.4907 0.1560 0.108 Uiso 0.50 1 calc PR A -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.0355(4) 0.0341(4) 0.0213(3) -0.0065(3) 0.0080(3) -0.0076(3) Ge2 0.0372(4) 0.0318(4) 0.0194(3) -0.0043(3) 0.0065(3) -0.0055(3) Si1 0.0294(11) 0.0351(10) 0.0252(9) -0.0104(8) 0.0006(8) 0.0029(8) Si2 0.0297(10) 0.0301(10) 0.0208(9) -0.0039(7) 0.0069(7) 0.0000(8) C1 0.021(3) 0.027(3) 0.012(3) 0.002(2) -0.003(2) 0.001(3) C2 0.021(3) 0.028(3) 0.025(3) 0.001(3) 0.002(3) -0.003(3) C3 0.020(3) 0.036(4) 0.023(3) 0.000(3) 0.008(3) -0.004(3) C4 0.018(3) 0.032(4) 0.019(3) 0.001(3) -0.002(2) 0.002(3) C5 0.019(3) 0.030(3) 0.017(3) -0.002(3) 0.002(2) -0.002(3) C6 0.023(3) 0.023(3) 0.019(3) 0.002(2) 0.003(3) -0.003(3) C7 0.018(3) 0.041(4) 0.033(4) -0.018(3) 0.012(3) -0.009(3) C8 0.033(4) 0.058(5) 0.035(4) -0.013(4) 0.001(3) -0.001(4) C9 0.028(4) 0.100(7) 0.028(4) -0.024(4) -0.005(3) -0.008(4) C10 0.062(6) 0.076(6) 0.047(5) -0.021(5) 0.028(5) -0.044(5) C11 0.055(5) 0.050(5) 0.041(4) -0.017(4) 0.025(4) -0.015(4) C12 0.041(4) 0.038(4) 0.024(3) -0.012(3) 0.012(3) -0.018(3) C13 0.041(5) 0.072(6) 0.033(4) -0.011(4) -0.012(3) 0.012(4) C14 0.123(10) 0.105(8) 0.049(6) 0.005(5) -0.037(6) -0.022(7) C15 0.093(9) 0.143(10) 0.089(8) 0.013(7) 0.000(7) 0.073(8) C16 0.062(5) 0.026(4) 0.033(4) -0.001(3) 0.019(4) -0.012(3) C17 0.048(5) 0.046(4) 0.032(4) 0.007(3) 0.014(3) 0.000(4) C18 0.075(6) 0.046(5) 0.039(4) -0.001(4) 0.033(4) 0.000(4) C19 0.035(4) 0.027(3) 0.021(3) -0.008(3) 0.009(3) -0.012(3) C20 0.023(4) 0.037(4) 0.036(4) -0.013(3) 0.014(3) -0.008(3) C21 0.029(4) 0.056(5) 0.062(5) -0.016(4) 0.019(4) -0.004(4) C22 0.040(5) 0.076(6) 0.051(5) -0.023(4) 0.024(4) -0.028(4) C23 0.057(5) 0.053(5) 0.033(4) -0.009(4) 0.020(4) -0.021(4) C24 0.041(4) 0.040(4) 0.017(3) -0.013(3) 0.007(3) -0.011(3) C25 0.027(4) 0.036(4) 0.056(5) 0.005(4) 0.001(3) 0.006(3) C26 0.044(5) 0.044(5) 0.080(6) 0.001(4) -0.002(4) 0.006(4) C27 0.053(5) 0.059(5) 0.034(4) 0.004(4) 0.000(4) 0.004(4) C28 0.059(5) 0.038(4) 0.025(4) -0.001(3) 0.012(3) -0.012(4) C29 0.119(8) 0.035(4) 0.027(4) -0.001(3) 0.002(4) -0.018(5) C31 0.140(10) 0.102(8) 0.058(6) -0.051(6) -0.058(6) 0.073(7) C32 0.063(6) 0.039(4) 0.096(7) -0.026(4) 0.047(5) -0.024(4) C33 0.064(6) 0.045(5) 0.066(5) -0.021(4) 0.039(5) -0.012(4) C34 0.029(4) 0.027(3) 0.011(3) -0.002(2) -0.003(2) 0.006(3) C35 0.022(3) 0.024(3) 0.019(3) 0.000(2) 0.002(2) 0.004(3) C36 0.024(4) 0.037(4) 0.013(3) -0.001(3) 0.002(2) 0.002(3) C37 0.025(4) 0.026(3) 0.021(3) -0.003(3) 0.000(3) 0.001(3) C38 0.026(4) 0.024(3) 0.019(3) -0.003(3) -0.005(3) 0.000(3) C39 0.019(3) 0.032(4) 0.017(3) -0.005(3) 0.000(2) 0.004(3) C40 0.043(4) 0.025(3) 0.020(3) -0.005(3) 0.010(3) 0.000(3) C41 0.049(5) 0.028(4) 0.028(4) -0.010(3) 0.012(3) -0.009(3) C42 0.056(5) 0.057(5) 0.032(4) -0.012(4) 0.011(4) -0.024(4) C43 0.083(7) 0.061(6) 0.021(4) -0.009(4) -0.005(4) -0.035(5) C44 0.106(7) 0.024(4) 0.029(4) -0.001(3) 0.014(4) 0.000(4) C45 0.070(5) 0.028(4) 0.013(3) -0.005(3) -0.004(3) 0.004(4) C46 0.072(6) 0.035(4) 0.040(4) -0.005(3) -0.021(4) 0.021(4) C47 0.129(10) 0.112(8) 0.025(4) 0.003(5) -0.024(5) 0.000(7) C48 0.070(7) 0.106(8) 0.072(6) -0.040(6) -0.031(5) 0.030(6) C50 0.057(6) 0.106(8) 0.098(8) -0.048(6) 0.019(6) 0.011(6) C51 0.055(6) 0.063(6) 0.082(6) -0.027(5) -0.023(5) 0.011(5) C52 0.034(4) 0.022(3) 0.010(3) 0.000(2) 0.005(3) -0.002(3) C53 0.019(3) 0.034(4) 0.015(3) -0.001(3) -0.001(2) -0.005(3) C54 0.027(4) 0.045(4) 0.023(3) -0.003(3) 0.004(3) -0.004(3) C55 0.030(4) 0.043(4) 0.020(3) -0.001(3) 0.005(3) -0.006(3) C56 0.051(5) 0.027(4) 0.022(3) 0.005(3) -0.003(3) 0.001(3) C57 0.021(3) 0.032(3) 0.018(3) -0.005(3) -0.004(3) -0.005(3) C58 0.031(4) 0.045(4) 0.021(3) 0.004(3) 0.001(3) -0.002(3) C59 0.053(5) 0.056(5) 0.039(4) 0.007(4) -0.015(4) -0.002(4) C60 0.053(5) 0.084(6) 0.040(4) 0.011(4) 0.000(4) 0.031(5) C61 0.025(4) 0.035(4) 0.028(3) 0.003(3) -0.005(3) -0.003(3) C62 0.037(5) 0.063(5) 0.049(5) -0.007(4) 0.002(4) 0.007(4) C63 0.037(4) 0.055(5) 0.036(4) -0.005(3) -0.004(3) 0.003(4) C64 0.041(4) 0.040(4) 0.029(4) -0.007(3) 0.021(3) -0.005(3) C65 0.038(4) 0.036(4) 0.032(4) -0.011(3) 0.006(3) -0.006(3) C66 0.032(4) 0.034(4) 0.041(4) -0.002(3) 0.010(3) 0.000(3) C67 0.025(4) 0.028(3) 0.016(3) -0.001(3) -0.001(3) 0.002(3) Ge3 0.0285(4) 0.0440(4) 0.0280(4) 0.0145(3) 0.0084(3) 0.0092(3) Ge4 0.0258(4) 0.0380(4) 0.0284(4) 0.0121(3) 0.0022(3) 0.0041(3) Si3 0.0302(10) 0.0289(10) 0.0226(9) 0.0046(7) -0.0023(7) -0.0028(8) Si4 0.0346(11) 0.0312(10) 0.0331(10) 0.0105(8) -0.0017(8) -0.0030(8) C68 0.023(3) 0.022(3) 0.018(3) -0.002(2) 0.005(3) -0.001(3) C69 0.025(3) 0.031(3) 0.011(3) 0.002(2) -0.002(2) 0.004(3) C70 0.023(3) 0.026(3) 0.016(3) 0.003(2) 0.002(2) 0.000(3) C71 0.025(4) 0.033(4) 0.023(3) 0.002(3) 0.005(3) -0.004(3) C72 0.015(3) 0.037(4) 0.026(3) 0.010(3) 0.002(3) -0.002(3) C73 0.024(4) 0.053(4) 0.025(3) 0.004(3) 0.005(3) 0.000(3) C74 0.022(4) 0.067(5) 0.030(4) 0.005(3) 0.010(3) 0.005(3) C75 0.019(4) 0.064(5) 0.040(4) 0.015(4) 0.000(3) 0.008(3) C76 0.029(4) 0.063(5) 0.022(3) 0.011(3) 0.002(3) -0.002(3) C77 0.024(4) 0.044(4) 0.028(3) -0.004(3) 0.003(3) -0.005(3) C78 0.037(4) 0.045(4) 0.033(4) 0.007(3) 0.010(3) 0.006(3) C79 0.023(4) 0.034(4) 0.021(3) 0.002(3) 0.008(3) 0.003(3) C80 0.024(4) 0.042(4) 0.024(3) 0.009(3) 0.006(3) 0.000(3) C81 0.029(4) 0.080(6) 0.041(4) 0.013(4) 0.008(3) 0.003(4) C82 0.028(4) 0.025(3) 0.017(3) 0.007(3) -0.005(3) -0.001(3) C83 0.058(5) 0.030(4) 0.025(3) 0.001(3) -0.004(3) -0.007(4) C84 0.090(7) 0.033(4) 0.034(4) -0.003(3) -0.008(4) -0.020(4) C85 0.070(6) 0.053(5) 0.059(5) 0.017(4) -0.012(5) -0.037(5) C86 0.036(4) 0.052(5) 0.039(4) 0.010(4) 0.002(3) -0.017(4) C87 0.027(4) 0.028(3) 0.022(3) 0.013(3) -0.008(3) -0.006(3) C88 0.075(6) 0.026(4) 0.043(4) -0.005(3) 0.010(4) 0.006(4) C89 0.123(9) 0.068(6) 0.044(5) 0.002(4) 0.030(5) 0.022(6) C90 0.107(8) 0.046(5) 0.053(5) -0.013(4) 0.006(5) 0.013(5) C91 0.016(3) 0.042(4) 0.035(4) 0.012(3) 0.004(3) 0.002(3) C92 0.037(4) 0.058(5) 0.040(4) 0.011(4) 0.013(3) 0.010(4) C93 0.035(4) 0.055(5) 0.044(4) 0.016(4) 0.008(3) 0.013(4) C94 0.021(3) 0.027(3) 0.023(3) 0.002(3) 0.011(3) 0.003(3) C95 0.029(4) 0.029(3) 0.020(3) -0.001(3) 0.003(3) -0.002(3) C96 0.027(4) 0.029(3) 0.020(3) 0.001(3) 0.001(3) 0.005(3) C97 0.025(4) 0.023(3) 0.019(3) 0.000(2) 0.005(3) 0.001(3) C98 0.032(4) 0.028(3) 0.017(3) 0.003(3) 0.010(3) 0.005(3) C99 0.075(6) 0.038(4) 0.031(4) -0.003(3) 0.002(4) -0.004(4) C100 0.025(4) 0.032(4) 0.031(3) -0.001(3) 0.007(3) -0.002(3) C101 0.028(4) 0.025(3) 0.029(3) 0.002(3) 0.007(3) -0.003(3) C102 0.025(4) 0.022(3) 0.024(3) -0.001(3) 0.007(3) 0.000(3) C103 0.022(3) 0.031(3) 0.019(3) 0.005(3) 0.007(3) 0.001(3) C104 0.029(4) 0.025(3) 0.022(3) 0.007(3) 0.012(3) 0.005(3) C105 0.023(3) 0.028(3) 0.019(3) 0.004(3) 0.008(3) 0.003(3) C106 0.036(4) 0.026(3) 0.028(3) 0.000(3) 0.012(3) 0.002(3) C107 0.022(4) 0.035(4) 0.040(4) 0.004(3) 0.009(3) 0.008(3) C108 0.025(4) 0.034(4) 0.031(4) -0.002(3) 0.003(3) -0.003(3) C109 0.055(5) 0.065(5) 0.036(4) 0.002(4) 0.009(4) -0.014(4) C110 0.037(4) 0.030(4) 0.025(3) 0.001(3) 0.006(3) 0.013(3) C111 0.032(4) 0.026(3) 0.023(3) 0.009(3) 0.011(3) 0.012(3) C112 0.027(4) 0.033(4) 0.032(4) 0.007(3) 0.010(3) 0.010(3) C113 0.038(5) 0.069(5) 0.041(4) 0.012(4) -0.005(3) 0.006(4) C114 0.049(5) 0.047(5) 0.043(4) 0.014(4) 0.032(4) 0.022(4) C115 0.059(5) 0.041(4) 0.029(4) 0.003(3) 0.018(4) 0.009(4) C116 0.034(4) 0.043(4) 0.048(4) 0.013(4) 0.024(3) 0.012(3) C117 0.025(4) 0.045(4) 0.034(4) 0.009(3) 0.005(3) 0.000(3) C118 0.036(4) 0.049(5) 0.048(4) 0.013(4) -0.003(3) -0.005(3) C119 0.068(7) 0.113(8) 0.046(5) 0.006(5) -0.024(5) -0.026(6) C120 0.033(4) 0.047(4) 0.029(3) -0.010(3) 0.008(3) 0.007(3) C121 0.066(6) 0.040(5) 0.091(7) 0.025(5) -0.019(5) -0.014(4) C122 0.066(7) 0.097(8) 0.245(15) 0.120(9) 0.072(9) 0.051(6) C123 0.045(4) 0.031(4) 0.026(3) 0.009(3) 0.006(3) -0.001(3) C124 0.032(4) 0.031(4) 0.057(5) 0.012(3) 0.006(3) 0.002(3) C125 0.077(6) 0.059(5) 0.038(4) 0.015(4) -0.020(4) -0.025(5) C126 0.054(5) 0.037(4) 0.030(4) -0.002(3) 0.014(3) -0.010(3) C127 0.033(4) 0.044(4) 0.059(5) -0.021(4) 0.006(4) -0.006(3) C128 0.244(15) 0.059(6) 0.031(5) 0.016(4) -0.035(7) 0.001(8) C129 0.101(8) 0.059(6) 0.059(6) 0.002(5) 0.014(5) 0.021(5) C130 0.130(9) 0.080(7) 0.035(5) 0.008(4) 0.028(5) -0.018(6) C131 0.051(5) 0.057(5) 0.051(5) -0.012(4) 0.018(4) -0.002(4) C132 0.046(6) 0.058(6) 0.129(9) -0.011(6) 0.021(6) -0.005(4) C133 0.039(4) 0.048(4) 0.033(4) 0.003(3) 0.001(3) -0.007(3) C134 0.086(7) 0.042(5) 0.033(4) 0.004(3) 0.007(4) 0.007(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Ge1 C1 1.971(5) . ? Ge1 Ge2 2.2444(9) . ? Ge2 C34 1.963(5) . ? Si1 C33 1.837(7) . ? Si1 C31 1.843(8) . ? Si1 C32 1.848(7) . ? Si1 C4 1.876(6) . ? Si2 C64 1.864(6) . ? Si2 C65 1.868(6) . ? Si2 C66 1.874(6) . ? Si2 C37 1.876(6) . ? C1 C6 1.402(8) . ? C1 C2 1.407(8) . ? C2 C3 1.392(8) . ? C2 C7 1.512(8) . ? C3 C4 1.407(8) . ? C3 H3 0.9500 . ? C4 C5 1.411(8) . ? C5 C6 1.387(7) . ? C5 H5 0.9500 . ? C6 C19 1.489(8) . ? C7 C12 1.403(9) . ? C7 C8 1.411(9) . ? C8 C9 1.426(10) . ? C8 C13 1.480(10) . ? C9 C10 1.350(11) . ? C9 H9 0.9500 . ? C10 C11 1.364(11) . ? C10 H10 0.9500 . ? C11 C12 1.396(9) . ? C11 H11 0.9500 . ? C12 C16 1.512(9) . ? C13 C14 1.521(10) . ? C13 C15 1.549(11) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.513(9) . ? C16 C18 1.538(8) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.409(9) . ? C19 C24 1.411(8) . ? C20 C21 1.407(9) . ? C20 C25 1.521(9) . ? C21 C22 1.366(10) . ? C21 H21 0.9500 . ? C22 C23 1.376(11) . ? C22 H22 0.9500 . ? C23 C24 1.388(9) . ? C23 H23 0.9500 . ? C24 C28 1.504(9) . ? C25 C26 1.515(9) . ? C25 C27 1.526(9) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.526(9) . ? C28 C134 1.534(9) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C34 C35 1.407(8) . ? C34 C39 1.418(8) . ? C35 C36 1.394(7) . ? C35 C40 1.491(8) . ? C36 C37 1.393(8) . ? C36 H36 0.9500 . ? C37 C38 1.398(8) . ? C38 C39 1.376(7) . ? C38 H38 0.9500 . ? C39 C52 1.505(7) . ? C40 C41 1.409(9) . ? C40 C45 1.415(9) . ? C41 C42 1.396(9) . ? C41 C127 1.512(9) . ? C42 C43 1.361(11) . ? C42 H42 0.9500 . ? C43 C44 1.371(11) . ? C43 H43 0.9500 . ? C44 C45 1.429(10) . ? C44 H44 0.9500 . ? C45 C46 1.501(10) . ? C46 C47 1.541(10) . ? C46 C48 1.551(11) . ? C46 H46 1.0000 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C48 H48A 0.9800 . ? C48 H48B 0.9800 . ? C48 H48C 0.9800 . ? C50 C127 1.538(10) . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 C127 1.530(10) . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C53 1.383(8) . ? C52 C57 1.409(8) . ? C53 C54 1.396(8) . ? C53 C58 1.539(8) . ? C54 C55 1.403(8) . ? C54 H54 0.9500 . ? C55 C56 1.353(9) . ? C55 H55 0.9500 . ? C56 C57 1.384(8) . ? C56 H56 0.9500 . ? C57 C61 1.522(8) . ? C58 C60 1.509(9) . ? C58 C59 1.510(9) . ? C58 H58 1.0000 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 H60A 0.9800 . ? C60 H60B 0.9800 . ? C60 H60C 0.9800 . ? C61 C63 1.536(8) . ? C61 C62 1.540(9) . ? C61 H61 1.0000 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 H64A 0.9800 . ? C64 H64B 0.9800 . ? C64 H64C 0.9800 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 C79 1.394(8) . ? C67 C68 1.407(8) . ? C67 Ge4 1.969(6) . ? Ge3 C94 1.964(6) . ? Ge3 Ge4 2.2470(10) . ? Si3 C123 1.857(6) . ? Si3 C125 1.868(7) . ? Si3 C124 1.872(6) . ? Si3 C97 1.882(6) . ? Si4 C121 1.818(7) . ? Si4 C122 1.830(9) . ? Si4 C128 1.852(8) . ? Si4 C70 1.870(6) . ? C68 C69 1.384(7) . ? C68 C82 1.483(8) . ? C69 C70 1.394(8) . ? C69 H69 0.9500 . ? C70 C71 1.401(8) . ? C71 C79 1.401(8) . ? C71 H71 0.9500 . ? C72 C73 1.404(8) . ? C72 C80 1.417(8) . ? C72 C79 1.508(8) . ? C73 C74 1.382(9) . ? C73 C78 1.535(9) . ? C74 C75 1.377(9) . ? C74 H74 0.9500 . ? C75 C76 1.376(9) . ? C75 H75 0.9500 . ? C76 C80 1.374(8) . ? C76 H76 0.9500 . ? C77 C131 1.513(9) . ? C77 C81 1.525(9) . ? C77 C80 1.529(8) . ? C77 H77 1.0000 . ? C78 C130 1.483(9) . ? C78 C129 1.492(10) . ? C78 H78 1.0000 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 C83 1.409(8) . ? C82 C87 1.412(8) . ? C83 C84 1.384(10) . ? C83 C88 1.520(10) . ? C84 C85 1.356(11) . ? C84 H84 0.9500 . ? C85 C86 1.382(10) . ? C85 H85 0.9500 . ? C86 C87 1.375(8) . ? C86 H86 0.9500 . ? C87 C91 1.529(9) . ? C88 C90 1.524(9) . ? C88 C89 1.529(10) . ? C88 H88 1.0000 . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? C90 H90A 0.9800 . ? C90 H90B 0.9800 . ? C90 H90C 0.9800 . ? C91 C93 1.525(8) . ? C91 C92 1.525(8) . ? C91 H91 1.0000 . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? C93 H93A 0.9800 . ? C93 H93B 0.9800 . ? C93 H93C 0.9800 . ? C94 C95 1.399(8) . ? C94 C102 1.412(7) . ? C95 C96 1.394(8) . ? C95 C111 1.500(8) . ? C96 C97 1.397(8) . ? C96 H96 0.9500 . ? C97 C98 1.391(8) . ? C98 C102 1.406(8) . ? C98 H98 0.9500 . ? C99 C101 1.529(8) . ? C99 H99A 0.9800 . ? C99 H99B 0.9800 . ? C99 H99C 0.9800 . ? C100 C105 1.518(8) . ? C100 C133 1.521(8) . ? C100 C109 1.530(8) . ? C100 H100 1.0000 . ? C101 C103 1.511(8) . ? C101 C126 1.522(8) . ? C101 H101 1.0000 . ? C102 C104 1.496(8) . ? C103 C108 1.381(8) . ? C103 C104 1.404(8) . ? C104 C105 1.405(8) . ? C105 C106 1.393(8) . ? C106 C107 1.390(9) . ? C106 H106 0.9500 . ? C107 C108 1.390(8) . ? C107 H107 0.9500 . ? C108 H108 0.9500 . ? C109 H10A 0.9800 . ? C109 H10B 0.9800 . ? C109 H10C 0.9800 . ? C110 C115 1.392(8) . ? C110 C111 1.415(8) . ? C110 C120 1.509(9) . ? C111 C112 1.409(9) . ? C112 C116 1.397(8) . ? C112 C117 1.501(9) . ? C113 C117 1.552(9) . ? C113 H11A 0.9800 . ? C113 H11B 0.9800 . ? C113 H11C 0.9800 . ? C114 C116 1.369(10) . ? C114 C115 1.381(10) . ? C114 H114 0.9500 . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C117 C118 1.525(9) . ? C117 H117 1.0000 . ? C118 H11D 0.9800 . ? C118 H11E 0.9800 . ? C118 H11F 0.9800 . ? C119 C120 1.533(9) . ? C119 H11G 0.9800 . ? C119 H11H 0.9800 . ? C119 H11I 0.9800 . ? C120 C132 1.523(10) . ? C120 H120 1.0000 . ? C121 H12A 0.9800 . ? C121 H12B 0.9800 . ? C121 H12C 0.9800 . ? C122 H12D 0.9800 . ? C122 H12E 0.9800 . ? C122 H12F 0.9800 . ? C123 H12G 0.9800 . ? C123 H12H 0.9800 . ? C123 H12I 0.9800 . ? C124 H12J 0.9800 . ? C124 H12K 0.9800 . ? C124 H12L 0.9800 . ? C125 H12M 0.9800 . ? C125 H12N 0.9800 . ? C125 H12O 0.9800 . ? C126 H12P 0.9800 . ? C126 H12Q 0.9800 . ? C126 H12R 0.9800 . ? C127 H127 1.0000 . ? C128 H12S 0.9800 . ? C128 H12T 0.9800 . ? C128 H12U 0.9800 . ? C129 H12V 0.9800 . ? C129 H12W 0.9800 . ? C129 H12$ 0.9800 . ? C130 H13A 0.9800 . ? C130 H13B 0.9800 . ? C130 H13C 0.9800 . ? C131 H13D 0.9800 . ? C131 H13E 0.9800 . ? C131 H13F 0.9800 . ? C132 H13G 0.9800 . ? C132 H13H 0.9800 . ? C132 H13I 0.9800 . ? C133 H13J 0.9800 . ? C133 H13K 0.9800 . ? C133 H13L 0.9800 . ? C134 H13M 0.9800 . ? C134 H13N 0.9800 . ? C134 H13O 0.9800 . ? C151 C152 1.422(18) . ? C151 H15D 0.9800 . ? C151 H15E 0.9800 . ? C151 H15F 0.9800 . ? C152 O153 1.353(13) . ? C152 H15G 0.9900 . ? C152 H15H 0.9900 . ? O153 C154 1.358(13) . ? C154 C155 1.429(17) . ? C154 H15I 0.9900 . ? C154 H15J 0.9900 . ? C155 H15K 0.9800 . ? C155 H15L 0.9800 . ? C155 H15M 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ge1 Ge2 128.40(17) . . ? C34 Ge2 Ge1 127.03(18) . . ? C33 Si1 C31 110.1(5) . . ? C33 Si1 C32 107.6(4) . . ? C31 Si1 C32 109.5(5) . . ? C33 Si1 C4 111.1(3) . . ? C31 Si1 C4 109.9(3) . . ? C32 Si1 C4 108.6(3) . . ? C64 Si2 C65 110.4(3) . . ? C64 Si2 C66 109.5(3) . . ? C65 Si2 C66 110.0(3) . . ? C64 Si2 C37 110.2(3) . . ? C65 Si2 C37 110.0(3) . . ? C66 Si2 C37 106.7(3) . . ? C6 C1 C2 118.5(5) . . ? C6 C1 Ge1 127.1(4) . . ? C2 C1 Ge1 114.3(4) . . ? C3 C2 C1 120.4(5) . . ? C3 C2 C7 119.9(5) . . ? C1 C2 C7 119.7(5) . . ? C2 C3 C4 122.1(5) . . ? C2 C3 H3 118.9 . . ? C4 C3 H3 118.9 . . ? C3 C4 C5 115.9(5) . . ? C3 C4 Si1 124.2(4) . . ? C5 C4 Si1 119.8(4) . . ? C6 C5 C4 123.0(5) . . ? C6 C5 H5 118.5 . . ? C4 C5 H5 118.5 . . ? C5 C6 C1 119.9(5) . . ? C5 C6 C19 117.8(5) . . ? C1 C6 C19 122.4(5) . . ? C12 C7 C8 121.5(6) . . ? C12 C7 C2 119.1(6) . . ? C8 C7 C2 119.4(6) . . ? C7 C8 C9 116.8(7) . . ? C7 C8 C13 120.9(6) . . ? C9 C8 C13 122.2(7) . . ? C10 C9 C8 121.2(7) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C11 121.2(7) . . ? C9 C10 H10 119.4 . . ? C11 C10 H10 119.4 . . ? C10 C11 C12 121.3(8) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C11 C12 C7 118.0(7) . . ? C11 C12 C16 119.5(6) . . ? C7 C12 C16 122.4(5) . . ? C8 C13 C14 115.0(7) . . ? C8 C13 C15 109.0(7) . . ? C14 C13 C15 111.6(7) . . ? C8 C13 H13 106.9 . . ? C14 C13 H13 106.9 . . ? C15 C13 H13 106.9 . . ? 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 . . ? C12 C16 C17 112.4(5) . . ? C12 C16 C18 113.9(6) . . ? C17 C16 C18 108.4(6) . . ? C12 C16 H16 107.3 . . ? C17 C16 H16 107.3 . . ? C18 C16 H16 107.3 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 121.0(6) . . ? C20 C19 C6 120.1(5) . . ? C24 C19 C6 118.8(6) . . ? C21 C20 C19 118.1(6) . . ? C21 C20 C25 120.7(6) . . ? C19 C20 C25 121.2(5) . . ? C22 C21 C20 120.0(7) . . ? C22 C21 H21 120.0 . . ? C20 C21 H21 120.0 . . ? C21 C22 C23 122.2(7) . . ? C21 C22 H22 118.9 . . ? C23 C22 H22 118.9 . . ? C22 C23 C24 120.0(7) . . ? C22 C23 H23 120.0 . . ? C24 C23 H23 120.0 . . ? C23 C24 C19 118.8(7) . . ? C23 C24 C28 120.2(6) . . ? C19 C24 C28 121.1(6) . . ? C26 C25 C20 114.1(6) . . ? C26 C25 C27 109.9(6) . . ? C20 C25 C27 110.7(5) . . ? C26 C25 H25 107.3 . . ? C20 C25 H25 107.3 . . ? C27 C25 H25 107.3 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 C29 114.0(6) . . ? C24 C28 C134 110.4(6) . . ? C29 C28 C134 109.2(5) . . ? C24 C28 H28 107.7 . . ? C29 C28 H28 107.7 . . ? C134 C28 H28 107.7 . . ? 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 . . ? 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 . . ? C35 C34 C39 119.1(5) . . ? C35 C34 Ge2 113.9(4) . . ? C39 C34 Ge2 126.8(4) . . ? C36 C35 C34 119.7(5) . . ? C36 C35 C40 120.4(5) . . ? C34 C35 C40 119.7(5) . . ? C37 C36 C35 122.5(5) . . ? C37 C36 H36 118.8 . . ? C35 C36 H36 118.8 . . ? C36 C37 C38 116.1(5) . . ? C36 C37 Si2 123.9(4) . . ? C38 C37 Si2 119.8(4) . . ? C39 C38 C37 124.2(6) . . ? C39 C38 H38 117.9 . . ? C37 C38 H38 117.9 . . ? C38 C39 C34 118.4(5) . . ? C38 C39 C52 119.3(5) . . ? C34 C39 C52 122.2(5) . . ? C41 C40 C45 120.6(6) . . ? C41 C40 C35 119.5(5) . . ? C45 C40 C35 119.9(6) . . ? C42 C41 C40 119.4(7) . . ? C42 C41 C127 119.2(7) . . ? C40 C41 C127 121.1(6) . . ? C43 C42 C41 121.4(8) . . ? C43 C42 H42 119.3 . . ? C41 C42 H42 119.3 . . ? C42 C43 C44 119.6(7) . . ? C42 C43 H43 120.2 . . ? C44 C43 H43 120.2 . . ? C43 C44 C45 122.6(7) . . ? C43 C44 H44 118.7 . . ? C45 C44 H44 118.7 . . ? C40 C45 C44 116.3(7) . . ? C40 C45 C46 121.1(6) . . ? C44 C45 C46 122.5(6) . . ? C45 C46 C47 111.7(7) . . ? C45 C46 C48 111.3(6) . . ? C47 C46 C48 108.7(7) . . ? C45 C46 H46 108.3 . . ? C47 C46 H46 108.3 . . ? C48 C46 H46 108.3 . . ? C46 C47 H47A 109.5 . . ? C46 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C46 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C46 C48 H48A 109.5 . . ? C46 C48 H48B 109.5 . . ? H48A C48 H48B 109.5 . . ? C46 C48 H48C 109.5 . . ? H48A C48 H48C 109.5 . . ? H48B C48 H48C 109.5 . . ? C127 C50 H50A 109.5 . . ? C127 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C127 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C127 C51 H51A 109.5 . . ? C127 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C127 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C53 C52 C57 121.4(5) . . ? C53 C52 C39 120.4(5) . . ? C57 C52 C39 118.2(5) . . ? C52 C53 C54 119.3(5) . . ? C52 C53 C58 121.9(5) . . ? C54 C53 C58 118.8(5) . . ? C53 C54 C55 119.2(6) . . ? C53 C54 H54 120.4 . . ? C55 C54 H54 120.4 . . ? C56 C55 C54 120.4(6) . . ? C56 C55 H55 119.8 . . ? C54 C55 H55 119.8 . . ? C55 C56 C57 122.2(6) . . ? C55 C56 H56 118.9 . . ? C57 C56 H56 118.9 . . ? C56 C57 C52 117.5(5) . . ? C56 C57 C61 121.1(5) . . ? C52 C57 C61 121.2(5) . . ? C60 C58 C59 111.2(6) . . ? C60 C58 C53 112.5(5) . . ? C59 C58 C53 110.6(5) . . ? C60 C58 H58 107.5 . . ? C59 C58 H58 107.5 . . ? C53 C58 H58 107.5 . . ? C58 C59 H59A 109.5 . . ? C58 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C58 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C58 C60 H60A 109.5 . . ? C58 C60 H60B 109.5 . . ? H60A C60 H60B 109.5 . . ? C58 C60 H60C 109.5 . . ? H60A C60 H60C 109.5 . . ? H60B C60 H60C 109.5 . . ? C57 C61 C63 112.4(5) . . ? C57 C61 C62 109.9(5) . . ? C63 C61 C62 109.8(5) . . ? C57 C61 H61 108.2 . . ? C63 C61 H61 108.2 . . ? C62 C61 H61 108.2 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? Si2 C64 H64A 109.5 . . ? Si2 C64 H64B 109.5 . . ? H64A C64 H64B 109.5 . . ? Si2 C64 H64C 109.5 . . ? H64A C64 H64C 109.5 . . ? H64B C64 H64C 109.5 . . ? Si2 C65 H65A 109.5 . . ? Si2 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? Si2 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? Si2 C66 H66A 109.5 . . ? Si2 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? Si2 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C79 C67 C68 119.2(5) . . ? C79 C67 Ge4 117.2(4) . . ? C68 C67 Ge4 123.6(4) . . ? C94 Ge3 Ge4 127.90(17) . . ? C67 Ge4 Ge3 124.89(18) . . ? C123 Si3 C125 110.0(3) . . ? C123 Si3 C124 110.0(3) . . ? C125 Si3 C124 109.3(4) . . ? C123 Si3 C97 108.4(3) . . ? C125 Si3 C97 110.2(3) . . ? C124 Si3 C97 109.0(3) . . ? C121 Si4 C122 108.5(5) . . ? C121 Si4 C128 109.9(5) . . ? C122 Si4 C128 109.7(6) . . ? C121 Si4 C70 110.6(3) . . ? C122 Si4 C70 108.5(3) . . ? C128 Si4 C70 109.6(3) . . ? C69 C68 C67 118.7(5) . . ? C69 C68 C82 118.1(5) . . ? C67 C68 C82 123.3(5) . . ? C68 C69 C70 124.3(5) . . ? C68 C69 H69 117.8 . . ? C70 C69 H69 117.8 . . ? C69 C70 C71 115.4(5) . . ? C69 C70 Si4 120.8(4) . . ? C71 C70 Si4 123.8(4) . . ? C70 C71 C79 122.5(6) . . ? C70 C71 H71 118.8 . . ? C79 C71 H71 118.8 . . ? C73 C72 C80 119.9(6) . . ? C73 C72 C79 119.1(5) . . ? C80 C72 C79 120.8(5) . . ? C74 C73 C72 119.2(6) . . ? C74 C73 C78 119.0(6) . . ? C72 C73 C78 121.7(6) . . ? C75 C74 C73 120.8(6) . . ? C75 C74 H74 119.6 . . ? C73 C74 H74 119.6 . . ? C76 C75 C74 119.9(6) . . ? C76 C75 H75 120.1 . . ? C74 C75 H75 120.1 . . ? C80 C76 C75 121.8(6) . . ? C80 C76 H76 119.1 . . ? C75 C76 H76 119.1 . . ? C131 C77 C81 111.2(6) . . ? C131 C77 C80 111.4(5) . . ? C81 C77 C80 111.7(5) . . ? C131 C77 H77 107.4 . . ? C81 C77 H77 107.4 . . ? C80 C77 H77 107.4 . . ? C130 C78 C129 111.4(6) . . ? C130 C78 C73 111.2(6) . . ? C129 C78 C73 113.9(6) . . ? C130 C78 H78 106.6 . . ? C129 C78 H78 106.6 . . ? C73 C78 H78 106.6 . . ? C67 C79 C71 119.8(6) . . ? C67 C79 C72 122.3(5) . . ? C71 C79 C72 117.9(5) . . ? C76 C80 C72 118.3(6) . . ? C76 C80 C77 120.1(6) . . ? C72 C80 C77 121.5(5) . . ? C77 C81 H81A 109.5 . . ? C77 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C77 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C83 C82 C87 120.1(6) . . ? C83 C82 C68 120.3(5) . . ? C87 C82 C68 119.5(5) . . ? C84 C83 C82 118.1(7) . . ? C84 C83 C88 121.0(6) . . ? C82 C83 C88 120.9(6) . . ? C85 C84 C83 121.9(7) . . ? C85 C84 H84 119.1 . . ? C83 C84 H84 119.1 . . ? C84 C85 C86 120.2(7) . . ? C84 C85 H85 119.9 . . ? C86 C85 H85 119.9 . . ? C87 C86 C85 120.8(7) . . ? C87 C86 H86 119.6 . . ? C85 C86 H86 119.6 . . ? C86 C87 C82 118.9(6) . . ? C86 C87 C91 120.8(6) . . ? C82 C87 C91 120.3(5) . . ? C83 C88 C90 113.1(6) . . ? C83 C88 C89 111.6(7) . . ? C90 C88 C89 111.5(6) . . ? C83 C88 H88 106.7 . . ? C90 C88 H88 106.7 . . ? C89 C88 H88 106.7 . . ? C88 C89 H89A 109.5 . . ? C88 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C88 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? C88 C90 H90A 109.5 . . ? C88 C90 H90B 109.5 . . ? H90A C90 H90B 109.5 . . ? C88 C90 H90C 109.5 . . ? H90A C90 H90C 109.5 . . ? H90B C90 H90C 109.5 . . ? C93 C91 C92 109.9(5) . . ? C93 C91 C87 110.8(5) . . ? C92 C91 C87 112.4(5) . . ? C93 C91 H91 107.8 . . ? C92 C91 H91 107.8 . . ? C87 C91 H91 107.8 . . ? C91 C92 H92A 109.5 . . ? C91 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C91 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? C91 C93 H93A 109.5 . . ? C91 C93 H93B 109.5 . . ? H93A C93 H93B 109.5 . . ? C91 C93 H93C 109.5 . . ? H93A C93 H93C 109.5 . . ? H93B C93 H93C 109.5 . . ? C95 C94 C102 120.0(5) . . ? C95 C94 Ge3 124.1(4) . . ? C102 C94 Ge3 115.6(4) . . ? C96 C95 C94 119.3(5) . . ? C96 C95 C111 120.1(5) . . ? C94 C95 C111 120.3(5) . . ? C95 C96 C97 122.4(6) . . ? C95 C96 H96 118.8 . . ? C97 C96 H96 118.8 . . ? C98 C97 C96 117.2(5) . . ? C98 C97 Si3 120.3(4) . . ? C96 C97 Si3 122.4(4) . . ? C97 C98 C102 122.7(5) . . ? C97 C98 H98 118.7 . . ? C102 C98 H98 118.7 . . ? C101 C99 H99A 109.5 . . ? C101 C99 H99B 109.5 . . ? H99A C99 H99B 109.5 . . ? C101 C99 H99C 109.5 . . ? H99A C99 H99C 109.5 . . ? H99B C99 H99C 109.5 . . ? C105 C100 C133 112.1(5) . . ? C105 C100 C109 111.7(5) . . ? C133 C100 C109 110.0(5) . . ? C105 C100 H100 107.6 . . ? C133 C100 H100 107.6 . . ? C109 C100 H100 107.6 . . ? C103 C101 C126 111.3(5) . . ? C103 C101 C99 112.0(5) . . ? C126 C101 C99 110.2(5) . . ? C103 C101 H101 107.7 . . ? C126 C101 H101 107.7 . . ? C99 C101 H101 107.7 . . ? C98 C102 C94 118.3(5) . . ? C98 C102 C104 118.8(5) . . ? C94 C102 C104 122.9(5) . . ? C108 C103 C104 117.6(5) . . ? C108 C103 C101 120.0(5) . . ? C104 C103 C101 122.3(5) . . ? C103 C104 C105 122.0(5) . . ? C103 C104 C102 119.0(5) . . ? C105 C104 C102 118.9(5) . . ? C106 C105 C104 117.8(6) . . ? C106 C105 C100 119.6(5) . . ? C104 C105 C100 122.6(5) . . ? C107 C106 C105 121.5(6) . . ? C107 C106 H106 119.3 . . ? C105 C106 H106 119.3 . . ? C108 C107 C106 118.9(6) . . ? C108 C107 H107 120.6 . . ? C106 C107 H107 120.6 . . ? C103 C108 C107 122.2(6) . . ? C103 C108 H108 118.9 . . ? C107 C108 H108 118.9 . . ? C100 C109 H10A 109.5 . . ? C100 C109 H10B 109.5 . . ? H10A C109 H10B 109.5 . . ? C100 C109 H10C 109.5 . . ? H10A C109 H10C 109.5 . . ? H10B C109 H10C 109.5 . . ? C115 C110 C111 118.0(6) . . ? C115 C110 C120 119.8(6) . . ? C111 C110 C120 122.1(5) . . ? C112 C111 C110 122.2(5) . . ? C112 C111 C95 120.8(5) . . ? C110 C111 C95 116.9(5) . . ? C116 C112 C111 117.2(6) . . ? C116 C112 C117 121.4(6) . . ? C111 C112 C117 121.4(5) . . ? C117 C113 H11A 109.5 . . ? C117 C113 H11B 109.5 . . ? H11A C113 H11B 109.5 . . ? C117 C113 H11C 109.5 . . ? H11A C113 H11C 109.5 . . ? H11B C113 H11C 109.5 . . ? C116 C114 C115 122.5(6) . . ? C116 C114 H114 118.8 . . ? C115 C114 H114 118.8 . . ? C114 C115 C110 119.5(7) . . ? C114 C115 H115 120.3 . . ? C110 C115 H115 120.3 . . ? C114 C116 C112 120.6(7) . . ? C114 C116 H116 119.7 . . ? C112 C116 H116 119.7 . . ? C112 C117 C118 114.5(5) . . ? C112 C117 C113 110.0(6) . . ? C118 C117 C113 110.3(6) . . ? C112 C117 H117 107.2 . . ? C118 C117 H117 107.2 . . ? C113 C117 H117 107.2 . . ? C117 C118 H11D 109.5 . . ? C117 C118 H11E 109.5 . . ? H11D C118 H11E 109.5 . . ? C117 C118 H11F 109.5 . . ? H11D C118 H11F 109.5 . . ? H11E C118 H11F 109.5 . . ? C120 C119 H11G 109.5 . . ? C120 C119 H11H 109.5 . . ? H11G C119 H11H 109.5 . . ? C120 C119 H11I 109.5 . . ? H11G C119 H11I 109.5 . . ? H11H C119 H11I 109.5 . . ? C110 C120 C132 111.8(6) . . ? C110 C120 C119 113.7(6) . . ? C132 C120 C119 111.2(7) . . ? C110 C120 H120 106.6 . . ? C132 C120 H120 106.6 . . ? C119 C120 H120 106.6 . . ? Si4 C121 H12A 109.5 . . ? Si4 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? Si4 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? Si4 C122 H12D 109.5 . . ? Si4 C122 H12E 109.5 . . ? H12D C122 H12E 109.5 . . ? Si4 C122 H12F 109.5 . . ? H12D C122 H12F 109.5 . . ? H12E C122 H12F 109.5 . . ? Si3 C123 H12G 109.5 . . ? Si3 C123 H12H 109.5 . . ? H12G C123 H12H 109.5 . . ? Si3 C123 H12I 109.5 . . ? H12G C123 H12I 109.5 . . ? H12H C123 H12I 109.5 . . ? Si3 C124 H12J 109.5 . . ? Si3 C124 H12K 109.5 . . ? H12J C124 H12K 109.5 . . ? Si3 C124 H12L 109.5 . . ? H12J C124 H12L 109.5 . . ? H12K C124 H12L 109.5 . . ? Si3 C125 H12M 109.5 . . ? Si3 C125 H12N 109.5 . . ? H12M C125 H12N 109.5 . . ? Si3 C125 H12O 109.5 . . ? H12M C125 H12O 109.5 . . ? H12N C125 H12O 109.5 . . ? C101 C126 H12P 109.5 . . ? C101 C126 H12Q 109.5 . . ? H12P C126 H12Q 109.5 . . ? C101 C126 H12R 109.5 . . ? H12P C126 H12R 109.5 . . ? H12Q C126 H12R 109.5 . . ? C41 C127 C51 113.4(6) . . ? C41 C127 C50 109.8(7) . . ? C51 C127 C50 109.8(7) . . ? C41 C127 H127 107.9 . . ? C51 C127 H127 107.9 . . ? C50 C127 H127 107.9 . . ? Si4 C128 H12S 109.5 . . ? Si4 C128 H12T 109.5 . . ? H12S C128 H12T 109.5 . . ? Si4 C128 H12U 109.5 . . ? H12S C128 H12U 109.5 . . ? H12T C128 H12U 109.5 . . ? C78 C129 H12V 109.5 . . ? C78 C129 H12W 109.5 . . ? H12V C129 H12W 109.5 . . ? C78 C129 H12$ 109.5 . . ? H12V C129 H12$ 109.5 . . ? H12W C129 H12$ 109.5 . . ? C78 C130 H13A 109.5 . . ? C78 C130 H13B 109.5 . . ? H13A C130 H13B 109.5 . . ? C78 C130 H13C 109.5 . . ? H13A C130 H13C 109.5 . . ? H13B C130 H13C 109.5 . . ? C77 C131 H13D 109.5 . . ? C77 C131 H13E 109.5 . . ? H13D C131 H13E 109.5 . . ? C77 C131 H13F 109.5 . . ? H13D C131 H13F 109.5 . . ? H13E C131 H13F 109.5 . . ? C120 C132 H13G 109.5 . . ? C120 C132 H13H 109.5 . . ? H13G C132 H13H 109.5 . . ? C120 C132 H13I 109.5 . . ? H13G C132 H13I 109.5 . . ? H13H C132 H13I 109.5 . . ? C100 C133 H13J 109.5 . . ? C100 C133 H13K 109.5 . . ? H13J C133 H13K 109.5 . . ? C100 C133 H13L 109.5 . . ? H13J C133 H13L 109.5 . . ? H13K C133 H13L 109.5 . . ? C28 C134 H13M 109.5 . . ? C28 C134 H13N 109.5 . . ? H13M C134 H13N 109.5 . . ? C28 C134 H13O 109.5 . . ? H13M C134 H13O 109.5 . . ? H13N C134 H13O 109.5 . . ? C152 C151 H15D 109.5 . . ? C152 C151 H15E 109.5 . . ? H15D C151 H15E 109.5 . . ? C152 C151 H15F 109.5 . . ? H15D C151 H15F 109.5 . . ? H15E C151 H15F 109.5 . . ? O153 C152 C151 103.6(12) . . ? O153 C152 H15G 111.0 . . ? C151 C152 H15G 111.0 . . ? O153 C152 H15H 111.0 . . ? C151 C152 H15H 111.0 . . ? H15G C152 H15H 109.0 . . ? C152 O153 C154 109.6(13) . . ? O153 C154 C155 106.4(13) . . ? O153 C154 H15I 110.4 . . ? C155 C154 H15I 110.4 . . ? O153 C154 H15J 110.4 . . ? C155 C154 H15J 110.4 . . ? H15I C154 H15J 108.6 . . ? C154 C155 H15K 109.5 . . ? C154 C155 H15L 109.5 . . ? H15K C155 H15L 109.5 . . ? C154 C155 H15M 109.5 . . ? H15K C155 H15M 109.5 . . ? H15L C155 H15M 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 C1 Ge1 Ge2 C34 175.3(3) . . . . ? Ge2 Ge1 C1 C6 22.9(6) . . . . ? Ge2 Ge1 C1 C2 -156.0(3) . . . . ? C6 C1 C2 C3 -4.1(8) . . . . ? Ge1 C1 C2 C3 174.9(4) . . . . ? C6 C1 C2 C7 177.1(5) . . . . ? Ge1 C1 C2 C7 -3.8(7) . . . . ? C1 C2 C3 C4 1.3(9) . . . . ? C7 C2 C3 C4 -180.0(6) . . . . ? C2 C3 C4 C5 2.0(8) . . . . ? C2 C3 C4 Si1 -174.8(4) . . . . ? C33 Si1 C4 C3 19.0(6) . . . . ? C31 Si1 C4 C3 -103.1(7) . . . . ? C32 Si1 C4 C3 137.1(5) . . . . ? C33 Si1 C4 C5 -157.7(5) . . . . ? C31 Si1 C4 C5 80.2(6) . . . . ? C32 Si1 C4 C5 -39.6(6) . . . . ? C3 C4 C5 C6 -2.5(8) . . . . ? Si1 C4 C5 C6 174.4(4) . . . . ? C4 C5 C6 C1 -0.3(9) . . . . ? C4 C5 C6 C19 -179.2(5) . . . . ? C2 C1 C6 C5 3.6(8) . . . . ? Ge1 C1 C6 C5 -175.3(4) . . . . ? C2 C1 C6 C19 -177.5(5) . . . . ? Ge1 C1 C6 C19 3.6(8) . . . . ? C3 C2 C7 C12 90.9(7) . . . . ? C1 C2 C7 C12 -90.3(7) . . . . ? C3 C2 C7 C8 -87.4(7) . . . . ? C1 C2 C7 C8 91.3(7) . . . . ? C12 C7 C8 C9 -0.3(9) . . . . ? C2 C7 C8 C9 178.0(6) . . . . ? C12 C7 C8 C13 -176.7(6) . . . . ? C2 C7 C8 C13 1.5(9) . . . . ? C7 C8 C9 C10 1.3(10) . . . . ? C13 C8 C9 C10 177.7(7) . . . . ? C8 C9 C10 C11 -1.1(11) . . . . ? C9 C10 C11 C12 -0.2(11) . . . . ? C10 C11 C12 C7 1.2(10) . . . . ? C10 C11 C12 C16 -177.6(6) . . . . ? C8 C7 C12 C11 -0.9(9) . . . . ? C2 C7 C12 C11 -179.2(5) . . . . ? C8 C7 C12 C16 177.9(6) . . . . ? C2 C7 C12 C16 -0.4(9) . . . . ? C7 C8 C13 C14 -135.5(8) . . . . ? C9 C8 C13 C14 48.3(10) . . . . ? C7 C8 C13 C15 98.3(8) . . . . ? C9 C8 C13 C15 -78.0(9) . . . . ? C11 C12 C16 C17 -90.1(7) . . . . ? C7 C12 C16 C17 91.1(7) . . . . ? C11 C12 C16 C18 33.6(8) . . . . ? C7 C12 C16 C18 -145.1(6) . . . . ? C5 C6 C19 C20 -89.5(7) . . . . ? C1 C6 C19 C20 91.6(7) . . . . ? C5 C6 C19 C24 86.7(7) . . . . ? C1 C6 C19 C24 -92.2(7) . . . . ? C24 C19 C20 C21 0.1(9) . . . . ? C6 C19 C20 C21 176.3(6) . . . . ? C24 C19 C20 C25 -177.4(5) . . . . ? C6 C19 C20 C25 -1.2(9) . . . . ? C19 C20 C21 C22 1.2(10) . . . . ? C25 C20 C21 C22 178.7(6) . . . . ? C20 C21 C22 C23 -1.2(11) . . . . ? C21 C22 C23 C24 -0.2(11) . . . . ? C22 C23 C24 C19 1.6(10) . . . . ? C22 C23 C24 C28 -177.0(6) . . . . ? C20 C19 C24 C23 -1.5(9) . . . . ? C6 C19 C24 C23 -177.7(5) . . . . ? C20 C19 C24 C28 177.1(5) . . . . ? C6 C19 C24 C28 0.9(8) . . . . ? C21 C20 C25 C26 42.0(9) . . . . ? C19 C20 C25 C26 -140.5(6) . . . . ? C21 C20 C25 C27 -82.6(8) . . . . ? C19 C20 C25 C27 94.9(7) . . . . ? C23 C24 C28 C29 -41.9(9) . . . . ? C19 C24 C28 C29 139.5(6) . . . . ? C23 C24 C28 C134 81.4(7) . . . . ? C19 C24 C28 C134 -97.2(7) . . . . ? Ge1 Ge2 C34 C35 -169.4(3) . . . . ? Ge1 Ge2 C34 C39 16.0(6) . . . . ? C39 C34 C35 C36 0.3(8) . . . . ? Ge2 C34 C35 C36 -174.8(4) . . . . ? C39 C34 C35 C40 175.0(5) . . . . ? Ge2 C34 C35 C40 -0.1(7) . . . . ? C34 C35 C36 C37 -0.4(9) . . . . ? C40 C35 C36 C37 -175.0(6) . . . . ? C35 C36 C37 C38 -0.3(9) . . . . ? C35 C36 C37 Si2 174.8(4) . . . . ? C64 Si2 C37 C36 -1.6(6) . . . . ? C65 Si2 C37 C36 120.4(5) . . . . ? C66 Si2 C37 C36 -120.3(5) . . . . ? C64 Si2 C37 C38 173.3(5) . . . . ? C65 Si2 C37 C38 -64.8(5) . . . . ? C66 Si2 C37 C38 54.5(5) . . . . ? C36 C37 C38 C39 1.1(9) . . . . ? Si2 C37 C38 C39 -174.1(5) . . . . ? C37 C38 C39 C34 -1.2(9) . . . . ? C37 C38 C39 C52 177.4(5) . . . . ? C35 C34 C39 C38 0.4(8) . . . . ? Ge2 C34 C39 C38 174.8(4) . . . . ? C35 C34 C39 C52 -178.2(5) . . . . ? Ge2 C34 C39 C52 -3.8(8) . . . . ? C36 C35 C40 C41 90.4(7) . . . . ? C34 C35 C40 C41 -84.1(7) . . . . ? C36 C35 C40 C45 -89.2(7) . . . . ? C34 C35 C40 C45 96.3(7) . . . . ? C45 C40 C41 C42 -0.6(9) . . . . ? C35 C40 C41 C42 179.8(5) . . . . ? C45 C40 C41 C127 173.7(6) . . . . ? C35 C40 C41 C127 -5.9(9) . . . . ? C40 C41 C42 C43 0.3(10) . . . . ? C127 C41 C42 C43 -174.1(6) . . . . ? C41 C42 C43 C44 0.0(11) . . . . ? C42 C43 C44 C45 0.1(11) . . . . ? C41 C40 C45 C44 0.7(9) . . . . ? C35 C40 C45 C44 -179.7(5) . . . . ? C41 C40 C45 C46 -177.4(6) . . . . ? C35 C40 C45 C46 2.2(9) . . . . ? C43 C44 C45 C40 -0.4(10) . . . . ? C43 C44 C45 C46 177.6(7) . . . . ? C40 C45 C46 C47 119.0(7) . . . . ? C44 C45 C46 C47 -58.9(9) . . . . ? C40 C45 C46 C48 -119.2(7) . . . . ? C44 C45 C46 C48 62.8(9) . . . . ? C38 C39 C52 C53 86.6(7) . . . . ? C34 C39 C52 C53 -94.9(7) . . . . ? C38 C39 C52 C57 -92.5(7) . . . . ? C34 C39 C52 C57 86.1(7) . . . . ? C57 C52 C53 C54 0.4(9) . . . . ? C39 C52 C53 C54 -178.6(5) . . . . ? C57 C52 C53 C58 178.1(5) . . . . ? C39 C52 C53 C58 -0.9(8) . . . . ? C52 C53 C54 C55 0.5(9) . . . . ? C58 C53 C54 C55 -177.3(5) . . . . ? C53 C54 C55 C56 -0.4(9) . . . . ? C54 C55 C56 C57 -0.6(10) . . . . ? C55 C56 C57 C52 1.5(9) . . . . ? C55 C56 C57 C61 177.7(6) . . . . ? C53 C52 C57 C56 -1.4(8) . . . . ? C39 C52 C57 C56 177.7(5) . . . . ? C53 C52 C57 C61 -177.6(5) . . . . ? C39 C52 C57 C61 1.4(8) . . . . ? C52 C53 C58 C60 142.9(6) . . . . ? C54 C53 C58 C60 -39.4(8) . . . . ? C52 C53 C58 C59 -92.2(7) . . . . ? C54 C53 C58 C59 85.5(7) . . . . ? C56 C57 C61 C63 39.8(8) . . . . ? C52 C57 C61 C63 -144.1(6) . . . . ? C56 C57 C61 C62 -82.8(7) . . . . ? C52 C57 C61 C62 93.3(7) . . . . ? C79 C67 Ge4 Ge3 149.3(4) . . . . ? C68 C67 Ge4 Ge3 -33.3(5) . . . . ? C94 Ge3 Ge4 C67 -166.1(3) . . . . ? C79 C67 C68 C69 -2.5(8) . . . . ? Ge4 C67 C68 C69 -179.9(4) . . . . ? C79 C67 C68 C82 176.5(5) . . . . ? Ge4 C67 C68 C82 -0.8(8) . . . . ? C67 C68 C69 C70 -0.3(8) . . . . ? C82 C68 C69 C70 -179.4(5) . . . . ? C68 C69 C70 C71 1.5(8) . . . . ? C68 C69 C70 Si4 -177.9(4) . . . . ? C121 Si4 C70 C69 167.6(5) . . . . ? C122 Si4 C70 C69 48.6(7) . . . . ? C128 Si4 C70 C69 -71.1(7) . . . . ? C121 Si4 C70 C71 -11.8(6) . . . . ? C122 Si4 C70 C71 -130.8(7) . . . . ? C128 Si4 C70 C71 109.4(6) . . . . ? C69 C70 C71 C79 0.0(8) . . . . ? Si4 C70 C71 C79 179.4(4) . . . . ? C80 C72 C73 C74 -0.7(9) . . . . ? C79 C72 C73 C74 175.6(6) . . . . ? C80 C72 C73 C78 -177.3(6) . . . . ? C79 C72 C73 C78 -1.0(9) . . . . ? C72 C73 C74 C75 -0.5(10) . . . . ? C78 C73 C74 C75 176.2(6) . . . . ? C73 C74 C75 C76 1.1(10) . . . . ? C74 C75 C76 C80 -0.4(10) . . . . ? C74 C73 C78 C130 -77.2(9) . . . . ? C72 C73 C78 C130 99.5(8) . . . . ? C74 C73 C78 C129 49.6(9) . . . . ? C72 C73 C78 C129 -133.7(7) . . . . ? C68 C67 C79 C71 4.0(8) . . . . ? Ge4 C67 C79 C71 -178.5(4) . . . . ? C68 C67 C79 C72 -173.4(5) . . . . ? Ge4 C67 C79 C72 4.1(7) . . . . ? C70 C71 C79 C67 -2.7(9) . . . . ? C70 C71 C79 C72 174.8(5) . . . . ? C73 C72 C79 C67 85.5(7) . . . . ? C80 C72 C79 C67 -98.2(7) . . . . ? C73 C72 C79 C71 -91.9(7) . . . . ? C80 C72 C79 C71 84.3(7) . . . . ? C75 C76 C80 C72 -0.8(10) . . . . ? C75 C76 C80 C77 179.5(6) . . . . ? C73 C72 C80 C76 1.3(9) . . . . ? C79 C72 C80 C76 -174.9(6) . . . . ? C73 C72 C80 C77 -178.9(6) . . . . ? C79 C72 C80 C77 4.8(9) . . . . ? C131 C77 C80 C76 73.1(8) . . . . ? C81 C77 C80 C76 -51.9(8) . . . . ? C131 C77 C80 C72 -106.7(7) . . . . ? C81 C77 C80 C72 128.3(6) . . . . ? C69 C68 C82 C83 94.0(7) . . . . ? C67 C68 C82 C83 -85.0(7) . . . . ? C69 C68 C82 C87 -82.3(7) . . . . ? C67 C68 C82 C87 98.6(7) . . . . ? C87 C82 C83 C84 2.5(9) . . . . ? C68 C82 C83 C84 -173.8(6) . . . . ? C87 C82 C83 C88 179.5(6) . . . . ? C68 C82 C83 C88 3.2(9) . . . . ? C82 C83 C84 C85 -1.4(11) . . . . ? C88 C83 C84 C85 -178.4(7) . . . . ? C83 C84 C85 C86 -0.6(12) . . . . ? C84 C85 C86 C87 1.5(11) . . . . ? C85 C86 C87 C82 -0.4(10) . . . . ? C85 C86 C87 C91 177.8(6) . . . . ? C83 C82 C87 C86 -1.6(9) . . . . ? C68 C82 C87 C86 174.7(5) . . . . ? C83 C82 C87 C91 -179.8(5) . . . . ? C68 C82 C87 C91 -3.5(8) . . . . ? C84 C83 C88 C90 -52.2(9) . . . . ? C82 C83 C88 C90 130.8(7) . . . . ? C84 C83 C88 C89 74.4(9) . . . . ? C82 C83 C88 C89 -102.5(8) . . . . ? C86 C87 C91 C93 -80.0(7) . . . . ? C82 C87 C91 C93 98.1(6) . . . . ? C86 C87 C91 C92 43.5(8) . . . . ? C82 C87 C91 C92 -138.4(6) . . . . ? Ge4 Ge3 C94 C95 -35.6(6) . . . . ? Ge4 Ge3 C94 C102 149.7(4) . . . . ? C102 C94 C95 C96 -2.5(9) . . . . ? Ge3 C94 C95 C96 -177.0(4) . . . . ? C102 C94 C95 C111 171.7(5) . . . . ? Ge3 C94 C95 C111 -2.8(8) . . . . ? C94 C95 C96 C97 1.2(9) . . . . ? C111 C95 C96 C97 -173.1(5) . . . . ? C95 C96 C97 C98 0.0(9) . . . . ? C95 C96 C97 Si3 176.2(4) . . . . ? C123 Si3 C97 C98 20.2(6) . . . . ? C125 Si3 C97 C98 -100.2(6) . . . . ? C124 Si3 C97 C98 139.8(5) . . . . ? C123 Si3 C97 C96 -155.9(5) . . . . ? C125 Si3 C97 C96 83.7(6) . . . . ? C124 Si3 C97 C96 -36.3(6) . . . . ? C96 C97 C98 C102 0.3(9) . . . . ? Si3 C97 C98 C102 -176.0(4) . . . . ? C97 C98 C102 C94 -1.7(9) . . . . ? C97 C98 C102 C104 178.0(5) . . . . ? C95 C94 C102 C98 2.8(9) . . . . ? Ge3 C94 C102 C98 177.7(4) . . . . ? C95 C94 C102 C104 -176.9(5) . . . . ? Ge3 C94 C102 C104 -1.9(8) . . . . ? C126 C101 C103 C108 -70.6(7) . . . . ? C99 C101 C103 C108 53.2(7) . . . . ? C126 C101 C103 C104 105.6(6) . . . . ? C99 C101 C103 C104 -130.6(6) . . . . ? C108 C103 C104 C105 -0.9(8) . . . . ? C101 C103 C104 C105 -177.2(5) . . . . ? C108 C103 C104 C102 174.4(5) . . . . ? C101 C103 C104 C102 -1.9(8) . . . . ? C98 C102 C104 C103 -88.3(7) . . . . ? C94 C102 C104 C103 91.3(7) . . . . ? C98 C102 C104 C105 87.1(7) . . . . ? C94 C102 C104 C105 -93.2(7) . . . . ? C103 C104 C105 C106 2.5(8) . . . . ? C102 C104 C105 C106 -172.9(5) . . . . ? C103 C104 C105 C100 -178.1(5) . . . . ? C102 C104 C105 C100 6.6(8) . . . . ? C133 C100 C105 C106 -61.4(7) . . . . ? C109 C100 C105 C106 62.6(7) . . . . ? C133 C100 C105 C104 119.2(6) . . . . ? C109 C100 C105 C104 -116.9(6) . . . . ? C104 C105 C106 C107 -2.6(8) . . . . ? C100 C105 C106 C107 177.9(5) . . . . ? C105 C106 C107 C108 1.2(9) . . . . ? C104 C103 C108 C107 -0.6(9) . . . . ? C101 C103 C108 C107 175.8(5) . . . . ? C106 C107 C108 C103 0.5(9) . . . . ? C115 C110 C111 C112 -1.3(9) . . . . ? C120 C110 C111 C112 176.3(6) . . . . ? C115 C110 C111 C95 177.0(5) . . . . ? C120 C110 C111 C95 -5.4(8) . . . . ? C96 C95 C111 C112 -91.7(7) . . . . ? C94 C95 C111 C112 94.1(7) . . . . ? C96 C95 C111 C110 89.9(7) . . . . ? C94 C95 C111 C110 -84.2(7) . . . . ? C110 C111 C112 C116 1.1(9) . . . . ? C95 C111 C112 C116 -177.1(5) . . . . ? C110 C111 C112 C117 -178.8(5) . . . . ? C95 C111 C112 C117 2.9(9) . . . . ? C116 C114 C115 C110 -1.3(10) . . . . ? C111 C110 C115 C114 1.3(9) . . . . ? C120 C110 C115 C114 -176.3(6) . . . . ? C115 C114 C116 C112 1.2(10) . . . . ? C111 C112 C116 C114 -1.0(9) . . . . ? C117 C112 C116 C114 178.9(6) . . . . ? C116 C112 C117 C118 35.3(9) . . . . ? C111 C112 C117 C118 -144.8(6) . . . . ? C116 C112 C117 C113 -89.6(7) . . . . ? C111 C112 C117 C113 90.4(7) . . . . ? C115 C110 C120 C132 73.8(8) . . . . ? C111 C110 C120 C132 -103.7(7) . . . . ? C115 C110 C120 C119 -53.1(9) . . . . ? C111 C110 C120 C119 129.3(7) . . . . ? C42 C41 C127 C51 -50.4(9) . . . . ? C40 C41 C127 C51 135.3(7) . . . . ? C42 C41 C127 C50 72.9(8) . . . . ? C40 C41 C127 C50 -101.4(7) . . . . ? C151 C152 O153 C154 -174.5(11) . . . . ? C152 O153 C154 C155 -165.5(14) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.780 _refine_diff_density_min -1.071 _refine_diff_density_rms 0.093 # Attachment '-4-Me3SiArSn-2.cif.txt' data_jf1516ffmi _database_code_depnum_ccdc_archive 'CCDC 771270' #TrackingRef '-4-Me3SiArSn-2.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H90 Si2 Sn2, 2(C7 H8)' _chemical_formula_sum 'C80 H106 Si2 Sn2' _chemical_formula_weight 1361.21 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P 21/c' _symmetry_space_group_name_Hall '-P 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 12.7007(4) _cell_length_b 11.7079(4) _cell_length_c 24.3198(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.1380(10) _cell_angle_gamma 90.00 _cell_volume 3616.3(2) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 8535 _cell_measurement_theta_min 2.90 _cell_measurement_theta_max 30.13 _exptl_crystal_description Block _exptl_crystal_colour brown _exptl_crystal_size_max 0.52 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.250 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1428 _exptl_absorpt_coefficient_mu 0.765 _exptl_absorpt_correction_type Analytical _exptl_absorpt_correction_T_min 0.6914 _exptl_absorpt_correction_T_max 0.8797 _exptl_absorpt_process_details 'SADABS 2007/1 (Sheldrick, 2007)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 39562 _diffrn_reflns_av_R_equivalents 0.0244 _diffrn_reflns_av_sigmaI/netI 0.0200 _diffrn_reflns_limit_h_min -17 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -34 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.90 _diffrn_reflns_theta_max 30.00 _reflns_number_total 10499 _reflns_number_gt 9249 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (2.0-2) (Bruker, 2006)' _computing_cell_refinement 'SAINT (7.23A) (Bruker, 2005)' _computing_data_reduction 'SAINT (7.23A) (Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL97 _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. All of the hydrogen atoms were located directly from difference-Fourier maps and allowed to refine freely. The lone Deviating Methyl group C47 H-C-H Bond Angle = 98.00 Deg. is located in the toluene solvent molecule. ; _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^)+(0.0392P)^2^+0.8109P] 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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10499 _refine_ls_number_parameters 591 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0287 _refine_ls_R_factor_gt 0.0240 _refine_ls_wR_factor_ref 0.0660 _refine_ls_wR_factor_gt 0.0638 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.023124(7) 1.071707(7) 0.948900(3) 0.02045(3) Uani 1 1 d . . . Si1 Si 0.40785(3) 0.79793(3) 0.798207(14) 0.01584(7) Uani 1 1 d . . . C1 C 0.14409(9) 0.96205(10) 0.91074(5) 0.0132(2) Uani 1 1 d . . . C2 C 0.11799(9) 0.88103(9) 0.87017(4) 0.01233(19) Uani 1 1 d . . . C3 C 0.19689(9) 0.82889(10) 0.83883(5) 0.0137(2) Uani 1 1 d . . . H3 H 0.1768(12) 0.7755(13) 0.8114(6) 0.014(3) Uiso 1 1 d . . . C4 C 0.30348(9) 0.85544(10) 0.84552(5) 0.0138(2) Uani 1 1 d . . . C5 C 0.32852(9) 0.93640(10) 0.88633(5) 0.0148(2) Uani 1 1 d . . . H5 H 0.3995(13) 0.9612(14) 0.8913(6) 0.016(4) Uiso 1 1 d . . . C6 C 0.25084(9) 0.98958(9) 0.91797(4) 0.01298(19) Uani 1 1 d . . . C7 C 0.00523(9) 0.85707(10) 0.85597(4) 0.0136(2) Uani 1 1 d . . . C8 C -0.04938(9) 0.76655(10) 0.88169(5) 0.0151(2) Uani 1 1 d . . . C9 C -0.15054(10) 0.73912(11) 0.86313(5) 0.0191(2) Uani 1 1 d . . . H9 H -0.1892(13) 0.6769(15) 0.8791(7) 0.024(4) Uiso 1 1 d . . . C10 C -0.19659(10) 0.80076(12) 0.82089(5) 0.0216(2) Uani 1 1 d . . . H10 H -0.2632(15) 0.7785(16) 0.8097(7) 0.031(5) Uiso 1 1 d . . . C11 C -0.14381(10) 0.89178(12) 0.79696(5) 0.0198(2) Uani 1 1 d . . . H11 H -0.1797(14) 0.9345(13) 0.7697(7) 0.023(4) Uiso 1 1 d . . . C12 C -0.04254(10) 0.92154(10) 0.81381(5) 0.0162(2) Uani 1 1 d . . . C13 C 0.00235(10) 0.69765(10) 0.92726(5) 0.0172(2) Uani 1 1 d . . . C14 C -0.07533(12) 0.66232(13) 0.97252(6) 0.0251(3) Uani 1 1 d . . . H14A H -0.1176(14) 0.7243(16) 0.9849(7) 0.029(4) Uiso 1 1 d . . . H14B H -0.0375(13) 0.6296(15) 1.0025(7) 0.024(4) Uiso 1 1 d . . . H14C H -0.1278(16) 0.6051(18) 0.9593(8) 0.035(5) Uiso 1 1 d . . . C15 C 0.05722(12) 0.59158(12) 0.90393(6) 0.0239(3) Uani 1 1 d . . . H15A H 0.0917(14) 0.5488(15) 0.9332(7) 0.025(4) Uiso 1 1 d . . . H15B H 0.1119(14) 0.6111(16) 0.8761(7) 0.028(4) Uiso 1 1 d . . . H15C H 0.0033(16) 0.5407(17) 0.8873(8) 0.034(5) Uiso 1 1 d . . . C16 C 0.01634(10) 1.01823(11) 0.78512(5) 0.0193(2) Uani 1 1 d . . . H16 H 0.0539(12) 0.7468(13) 0.9433(6) 0.014(3) Uiso 1 1 d . . . C17 C -0.05100(13) 1.12422(13) 0.77571(7) 0.0315(3) Uani 1 1 d . . . H17A H -0.1075(17) 1.1057(18) 0.7522(8) 0.040(5) Uiso 1 1 d . . . H17B H -0.0091(15) 1.1841(17) 0.7608(8) 0.039(5) Uiso 1 1 d . . . H17C H -0.0808(16) 1.1504(18) 0.8088(8) 0.041(5) Uiso 1 1 d . . . C18 C 0.06164(13) 0.97539(14) 0.73029(6) 0.0296(3) Uani 1 1 d . . . H18A H 0.1123(19) 0.9116(19) 0.7363(9) 0.050(6) Uiso 1 1 d . . . H18B H 0.0997(16) 1.0345(19) 0.7111(8) 0.038(5) Uiso 1 1 d . . . H18C H 0.0034(18) 0.9475(17) 0.7056(9) 0.044(6) Uiso 1 1 d . . . C19 C 0.28077(9) 1.08627(10) 0.95543(5) 0.0136(2) Uani 1 1 d . . . H19 H 0.0730(13) 1.0410(14) 0.8068(7) 0.019(4) Uiso 1 1 d . . . C20 C 0.28957(9) 1.19717(10) 0.93275(5) 0.0161(2) Uani 1 1 d . . . C21 C 0.32367(10) 1.28635(11) 0.96632(5) 0.0193(2) Uani 1 1 d . . . H21 H 0.3279(13) 1.3602(15) 0.9520(7) 0.022(4) Uiso 1 1 d . . . C22 C 0.34778(10) 1.26766(11) 1.02121(5) 0.0202(2) Uani 1 1 d . . . H22 H 0.3673(14) 1.3285(16) 1.0423(7) 0.025(4) Uiso 1 1 d . . . C23 C 0.33686(10) 1.15941(11) 1.04353(5) 0.0187(2) Uani 1 1 d . . . H23 H 0.3518(12) 1.1464(13) 1.0814(6) 0.016(4) Uiso 1 1 d . . . C24 C 0.30373(9) 1.06717(9) 1.01141(5) 0.0150(2) Uani 1 1 d . . . C25 C 0.26611(11) 1.22015(11) 0.87236(5) 0.0205(2) Uani 1 1 d . . . H25 H 0.2289(13) 1.1567(15) 0.8582(7) 0.025(4) Uiso 1 1 d . . . C26 C 0.36865(14) 1.22951(16) 0.83951(7) 0.0338(3) Uani 1 1 d . . . H26A H 0.4070(16) 1.2961(19) 0.8526(8) 0.042(5) Uiso 1 1 d . . . H26B H 0.3560(16) 1.2418(18) 0.8002(9) 0.045(6) Uiso 1 1 d . . . H26C H 0.4116(16) 1.1678(18) 0.8439(8) 0.037(5) Uiso 1 1 d . . . C27 C 0.19696(15) 1.32578(14) 0.86390(7) 0.0342(3) Uani 1 1 d . . . H27A H 0.1304(17) 1.3207(18) 0.8860(9) 0.045(6) Uiso 1 1 d . . . H27B H 0.1785(16) 1.3345(18) 0.8260(8) 0.041(5) Uiso 1 1 d . . . H27C H 0.2372(17) 1.3960(19) 0.8741(8) 0.040(5) Uiso 1 1 d . . . C28 C 0.29990(10) 0.94833(10) 1.03655(5) 0.0178(2) Uani 1 1 d . . . C29 C 0.25404(17) 0.94813(14) 1.09469(6) 0.0354(4) Uani 1 1 d . . . H29A H 0.3051(18) 0.982(2) 1.1191(9) 0.053(6) Uiso 1 1 d . . . H29B H 0.2409(16) 0.8702(19) 1.1059(8) 0.042(5) Uiso 1 1 d . . . H29C H 0.1868(19) 0.989(2) 1.0974(9) 0.054(6) Uiso 1 1 d . . . C30 C 0.41027(13) 0.89629(14) 1.03706(8) 0.0342(4) Uani 1 1 d . . . H30A H 0.4584(18) 0.9430(18) 1.0586(9) 0.043(6) Uiso 1 1 d . . . H30B H 0.4410(18) 0.887(2) 1.0004(10) 0.052(6) Uiso 1 1 d . . . H30C H 0.4080(16) 0.8262(19) 1.0540(8) 0.044(5) Uiso 1 1 d . . . C31 C 0.34663(12) 0.71627(14) 0.74057(6) 0.0266(3) Uani 1 1 d . . . H31 H 0.2587(12) 0.9005(13) 1.0129(6) 0.015(4) Uiso 1 1 d . . . H31A H 0.3999(18) 0.7016(19) 0.7142(9) 0.051(6) Uiso 1 1 d . . . H31B H 0.2952(16) 0.7584(18) 0.7243(8) 0.042(5) Uiso 1 1 d . . . H31C H 0.3156(16) 0.6455(19) 0.7555(8) 0.044(6) Uiso 1 1 d . . . C32 C 0.48532(15) 0.92193(13) 0.77166(8) 0.0344(4) Uani 1 1 d . . . H32A H 0.5172(18) 0.9591(19) 0.8018(9) 0.047(6) Uiso 1 1 d . . . H32B H 0.4394(18) 0.979(2) 0.7532(9) 0.051(6) Uiso 1 1 d . . . H32C H 0.5374(19) 0.898(2) 0.7473(10) 0.055(6) Uiso 1 1 d . . . C33 C 0.49725(11) 0.69846(13) 0.83560(6) 0.0266(3) Uani 1 1 d . . . H33A H 0.5535(16) 0.6693(17) 0.8121(8) 0.038(5) Uiso 1 1 d . . . H33B H 0.4568(17) 0.6349(19) 0.8492(8) 0.042(5) Uiso 1 1 d . . . H33C H 0.5252(18) 0.732(2) 0.8674(9) 0.055(6) Uiso 1 1 d . . . C41 C 0.69055(12) 0.37769(12) 0.98128(6) 0.0263(3) Uani 1 1 d . . . C42 C 0.78736(13) 0.35825(14) 0.95649(7) 0.0320(3) Uani 1 1 d . . . H42 H 0.8406(15) 0.3262(17) 0.9766(8) 0.035(5) Uiso 1 1 d . . . C43 C 0.80364(15) 0.38281(16) 0.90116(7) 0.0389(4) Uani 1 1 d . . . H43 H 0.8703(17) 0.3693(18) 0.8853(8) 0.042(5) Uiso 1 1 d . . . C44 C 0.72311(18) 0.42618(14) 0.87009(7) 0.0408(4) Uani 1 1 d . . . H44 H 0.738(2) 0.440(2) 0.8339(11) 0.063(8) Uiso 1 1 d . . . C45 C 0.62590(17) 0.44416(13) 0.89369(7) 0.0383(4) Uani 1 1 d . . . H45 H 0.5686(18) 0.475(2) 0.8707(9) 0.049(6) Uiso 1 1 d . . . C46 C 0.60907(14) 0.42035(12) 0.94887(7) 0.0313(3) Uani 1 1 d . . . H46 H 0.5443(18) 0.4302(17) 0.9649(9) 0.042(6) Uiso 1 1 d . . . C47 C 0.67197(19) 0.35039(18) 1.04091(7) 0.0425(4) Uani 1 1 d . . . H47A H 0.719(2) 0.296(3) 1.0546(12) 0.089(10) Uiso 1 1 d . . . H47B H 0.603(2) 0.328(3) 1.0479(11) 0.078(9) Uiso 1 1 d . . . H47C H 0.688(2) 0.412(2) 1.0672(12) 0.071(8) Uiso 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 0.02230(5) 0.01969(5) 0.01940(5) 0.00013(3) 0.00564(3) 0.00760(3) Si1 0.01469(14) 0.01616(15) 0.01668(15) -0.00364(11) 0.00227(11) 0.00108(11) C1 0.0150(5) 0.0123(5) 0.0124(5) 0.0004(4) 0.0010(4) 0.0006(4) C2 0.0134(5) 0.0115(5) 0.0120(5) 0.0011(4) -0.0003(4) -0.0004(4) C3 0.0157(5) 0.0125(5) 0.0128(5) -0.0014(4) -0.0008(4) 0.0001(4) C4 0.0147(5) 0.0134(5) 0.0134(5) -0.0005(4) 0.0010(4) 0.0010(4) C5 0.0135(5) 0.0156(5) 0.0151(5) -0.0012(4) -0.0003(4) 0.0003(4) C6 0.0151(5) 0.0118(5) 0.0120(5) -0.0003(4) -0.0003(4) -0.0004(4) C7 0.0134(5) 0.0148(5) 0.0127(5) -0.0031(4) 0.0003(4) 0.0004(4) C8 0.0156(5) 0.0156(5) 0.0140(5) -0.0015(4) 0.0012(4) -0.0010(4) C9 0.0172(5) 0.0204(6) 0.0197(6) -0.0029(4) 0.0013(4) -0.0050(4) C10 0.0146(5) 0.0281(7) 0.0220(6) -0.0056(5) -0.0023(4) -0.0032(5) C11 0.0177(6) 0.0251(6) 0.0164(5) -0.0009(5) -0.0027(4) 0.0032(5) C12 0.0161(5) 0.0179(5) 0.0146(5) -0.0014(4) -0.0001(4) 0.0020(4) C13 0.0188(5) 0.0157(5) 0.0171(5) 0.0017(4) -0.0002(4) -0.0021(4) C14 0.0260(7) 0.0285(7) 0.0207(6) 0.0045(5) 0.0024(5) -0.0050(5) C15 0.0290(7) 0.0179(6) 0.0250(6) 0.0005(5) -0.0013(5) 0.0025(5) C16 0.0190(6) 0.0199(6) 0.0191(6) 0.0045(4) -0.0027(4) 0.0003(4) C17 0.0327(8) 0.0231(7) 0.0387(8) 0.0096(6) 0.0018(7) 0.0069(6) C18 0.0346(8) 0.0307(8) 0.0234(7) 0.0070(6) 0.0085(6) 0.0003(6) C19 0.0125(5) 0.0132(5) 0.0150(5) -0.0029(4) 0.0012(4) -0.0006(4) C20 0.0169(5) 0.0149(5) 0.0167(5) -0.0010(4) 0.0018(4) -0.0005(4) C21 0.0222(6) 0.0133(5) 0.0224(6) -0.0011(4) 0.0011(5) -0.0028(4) C22 0.0223(6) 0.0158(6) 0.0224(6) -0.0061(4) -0.0010(5) -0.0027(4) C23 0.0207(6) 0.0182(6) 0.0170(5) -0.0036(4) -0.0024(4) -0.0014(4) C24 0.0147(5) 0.0143(5) 0.0159(5) -0.0018(4) -0.0001(4) -0.0009(4) C25 0.0268(6) 0.0164(6) 0.0182(6) 0.0014(4) 0.0005(5) -0.0024(5) C26 0.0392(9) 0.0379(9) 0.0244(7) 0.0041(6) 0.0110(6) -0.0045(7) C27 0.0475(10) 0.0288(8) 0.0263(7) 0.0052(6) -0.0046(7) 0.0098(7) C28 0.0221(6) 0.0147(5) 0.0167(5) -0.0007(4) -0.0023(4) -0.0026(4) C29 0.0617(12) 0.0253(7) 0.0193(7) -0.0011(5) 0.0055(7) -0.0115(7) C30 0.0266(7) 0.0184(6) 0.0576(11) 0.0052(7) -0.0117(7) 0.0004(5) C31 0.0224(6) 0.0354(8) 0.0221(6) -0.0108(6) -0.0013(5) 0.0040(6) C32 0.0394(9) 0.0237(7) 0.0402(9) -0.0055(6) 0.0228(7) -0.0057(6) C33 0.0209(6) 0.0299(7) 0.0290(7) -0.0046(6) -0.0028(5) 0.0079(5) C41 0.0367(8) 0.0179(6) 0.0242(6) 0.0001(5) -0.0002(5) -0.0067(5) C42 0.0298(7) 0.0290(7) 0.0373(8) -0.0024(6) -0.0060(6) -0.0078(6) C43 0.0389(9) 0.0385(9) 0.0395(9) -0.0096(7) 0.0100(7) -0.0175(7) C44 0.0668(13) 0.0304(8) 0.0252(8) 0.0004(6) 0.0027(8) -0.0186(8) C45 0.0572(11) 0.0214(7) 0.0363(9) 0.0043(6) -0.0110(8) 0.0030(7) C46 0.0360(8) 0.0209(7) 0.0370(8) -0.0015(6) 0.0010(7) 0.0041(6) C47 0.0618(12) 0.0406(10) 0.0251(8) 0.0027(7) 0.0008(8) -0.0161(9) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C1 2.2084(11) . ? Sn1 Sn1 3.05765(18) 3_577 ? Si1 C33 1.8621(15) . ? Si1 C31 1.8650(14) . ? Si1 C32 1.8696(16) . ? Si1 C4 1.8820(12) . ? C1 C6 1.4043(16) . ? C1 C2 1.4075(15) . ? C2 C3 1.4005(15) . ? C2 C7 1.4990(15) . ? C3 C4 1.3982(16) . ? C3 H3 0.948(15) . ? C4 C5 1.4082(16) . ? C5 C6 1.3989(16) . ? C5 H5 0.954(16) . ? C6 C19 1.5014(15) . ? C7 C12 1.4093(16) . ? C7 C8 1.4133(16) . ? C8 C9 1.3981(16) . ? C8 C13 1.5190(16) . ? C9 C10 1.3839(18) . ? C9 H9 0.961(18) . ? C10 C11 1.3876(19) . ? C10 H10 0.926(19) . ? C11 C12 1.3933(17) . ? C11 H11 0.947(17) . ? C12 C16 1.5264(17) . ? C13 C15 1.5336(18) . ? C13 C14 1.5366(18) . ? C13 H16 0.955(15) . ? C14 H14A 0.952(19) . ? C14 H14B 0.953(17) . ? C14 H14C 1.00(2) . ? C15 H15A 0.973(18) . ? C15 H15B 0.999(19) . ? C15 H15C 0.99(2) . ? C16 C17 1.5241(19) . ? C16 C18 1.538(2) . ? C16 H19 0.930(17) . ? C17 H17A 0.94(2) . ? C17 H17B 0.95(2) . ? C17 H17C 0.94(2) . ? C18 H18A 1.00(2) . ? C18 H18B 0.96(2) . ? C18 H18C 1.01(2) . ? C19 C24 1.4095(16) . ? C19 C20 1.4152(16) . ? C20 C21 1.3937(17) . ? C20 C25 1.5218(17) . ? C21 C22 1.3864(18) . ? C21 H21 0.934(17) . ? C22 C23 1.3857(18) . ? C22 H22 0.912(18) . ? C23 C24 1.3971(16) . ? C23 H23 0.952(16) . ? C24 C28 1.5205(16) . ? C25 C27 1.530(2) . ? C25 C26 1.534(2) . ? C25 H25 0.946(17) . ? C26 H26A 0.97(2) . ? C26 H26B 0.98(2) . ? C26 H26C 0.91(2) . ? C27 H27A 1.01(2) . ? C27 H27B 0.96(2) . ? C27 H27C 1.00(2) . ? C28 C30 1.529(2) . ? C28 C29 1.531(2) . ? C28 H31 0.958(16) . ? C29 H29A 0.96(2) . ? C29 H29B 0.97(2) . ? C29 H29C 0.98(2) . ? C30 H30A 0.97(2) . ? C30 H30B 0.98(2) . ? C30 H30C 0.92(2) . ? C31 H31A 0.95(2) . ? C31 H31B 0.91(2) . ? C31 H31C 0.99(2) . ? C32 H32A 0.94(2) . ? C32 H32B 0.99(2) . ? C32 H32C 0.93(2) . ? C33 H33A 0.98(2) . ? C33 H33B 0.96(2) . ? C33 H33C 0.94(2) . ? C41 C42 1.390(2) . ? C41 C46 1.392(2) . ? C41 C47 1.504(2) . ? C42 C43 1.392(2) . ? C42 H42 0.91(2) . ? C43 C44 1.368(3) . ? C43 H43 0.95(2) . ? C44 C45 1.379(3) . ? C44 H44 0.91(3) . ? C45 C46 1.388(2) . ? C45 H45 0.98(2) . ? C46 H46 0.92(2) . ? C47 H47A 0.93(3) . ? C47 H47B 0.93(3) . ? C47 H47C 0.99(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 C1 Sn1 Sn1 99.07(3) . 3_577 ? C33 Si1 C31 107.40(7) . . ? C33 Si1 C32 109.48(8) . . ? C31 Si1 C32 110.94(8) . . ? C33 Si1 C4 110.77(6) . . ? C31 Si1 C4 110.48(6) . . ? C32 Si1 C4 107.78(6) . . ? C6 C1 C2 117.92(10) . . ? C6 C1 Sn1 119.10(8) . . ? C2 C1 Sn1 121.57(8) . . ? C3 C2 C1 120.50(10) . . ? C3 C2 C7 118.52(10) . . ? C1 C2 C7 120.73(10) . . ? C4 C3 C2 122.25(10) . . ? C4 C3 H3 119.1(9) . . ? C2 C3 H3 118.6(9) . . ? C3 C4 C5 116.65(10) . . ? C3 C4 Si1 122.18(9) . . ? C5 C4 Si1 120.90(9) . . ? C6 C5 C4 121.93(11) . . ? C6 C5 H5 117.6(10) . . ? C4 C5 H5 120.3(10) . . ? C5 C6 C1 120.72(10) . . ? C5 C6 C19 119.44(10) . . ? C1 C6 C19 119.48(10) . . ? C12 C7 C8 120.85(11) . . ? C12 C7 C2 118.48(10) . . ? C8 C7 C2 120.52(10) . . ? C9 C8 C7 118.74(11) . . ? C9 C8 C13 120.61(11) . . ? C7 C8 C13 120.62(10) . . ? C10 C9 C8 120.42(12) . . ? C10 C9 H9 118.7(10) . . ? C8 C9 H9 120.9(10) . . ? C9 C10 C11 120.53(11) . . ? C9 C10 H10 117.1(11) . . ? C11 C10 H10 122.3(11) . . ? C10 C11 C12 121.02(12) . . ? C10 C11 H11 117.9(11) . . ? C12 C11 H11 121.1(11) . . ? C11 C12 C7 118.39(11) . . ? C11 C12 C16 120.27(11) . . ? C7 C12 C16 121.28(11) . . ? C8 C13 C15 110.86(10) . . ? C8 C13 C14 112.85(11) . . ? C15 C13 C14 109.88(11) . . ? C8 C13 H16 105.9(9) . . ? C15 C13 H16 109.1(9) . . ? C14 C13 H16 108.1(9) . . ? C13 C14 H14A 112.6(11) . . ? C13 C14 H14B 109.4(10) . . ? H14A C14 H14B 110.4(15) . . ? C13 C14 H14C 112.3(11) . . ? H14A C14 H14C 103.7(16) . . ? H14B C14 H14C 108.2(15) . . ? C13 C15 H15A 110.5(10) . . ? C13 C15 H15B 112.5(11) . . ? H15A C15 H15B 107.6(15) . . ? C13 C15 H15C 108.8(12) . . ? H15A C15 H15C 107.3(15) . . ? H15B C15 H15C 110.0(15) . . ? C17 C16 C12 113.40(11) . . ? C17 C16 C18 110.26(12) . . ? C12 C16 C18 109.83(11) . . ? C17 C16 H19 106.6(10) . . ? C12 C16 H19 109.4(10) . . ? C18 C16 H19 107.2(10) . . ? C16 C17 H17A 109.3(13) . . ? C16 C17 H17B 110.0(12) . . ? H17A C17 H17B 111.4(17) . . ? C16 C17 H17C 111.3(12) . . ? H17A C17 H17C 106.6(18) . . ? H17B C17 H17C 108.1(17) . . ? C16 C18 H18A 111.2(13) . . ? C16 C18 H18B 112.0(12) . . ? H18A C18 H18B 106.5(18) . . ? C16 C18 H18C 110.3(13) . . ? H18A C18 H18C 108.5(17) . . ? H18B C18 H18C 108.3(17) . . ? C24 C19 C20 120.37(10) . . ? C24 C19 C6 121.20(10) . . ? C20 C19 C6 118.39(10) . . ? C21 C20 C19 118.93(11) . . ? C21 C20 C25 119.51(11) . . ? C19 C20 C25 121.52(10) . . ? C22 C21 C20 120.89(12) . . ? C22 C21 H21 119.5(10) . . ? C20 C21 H21 119.5(10) . . ? C23 C22 C21 119.96(11) . . ? C23 C22 H22 121.4(11) . . ? C21 C22 H22 118.6(11) . . ? C22 C23 C24 121.22(11) . . ? C22 C23 H23 120.4(10) . . ? C24 C23 H23 118.4(10) . . ? C23 C24 C19 118.60(11) . . ? C23 C24 C28 119.50(11) . . ? C19 C24 C28 121.78(10) . . ? C20 C25 C27 112.56(11) . . ? C20 C25 C26 110.54(12) . . ? C27 C25 C26 111.10(13) . . ? C20 C25 H25 108.1(10) . . ? C27 C25 H25 107.5(10) . . ? C26 C25 H25 106.9(10) . . ? C25 C26 H26A 108.2(12) . . ? C25 C26 H26B 112.4(12) . . ? H26A C26 H26B 106.4(17) . . ? C25 C26 H26C 113.1(13) . . ? H26A C26 H26C 107.3(17) . . ? H26B C26 H26C 109.0(17) . . ? C25 C27 H27A 111.3(12) . . ? C25 C27 H27B 110.8(12) . . ? H27A C27 H27B 108.5(17) . . ? C25 C27 H27C 109.8(12) . . ? H27A C27 H27C 110.3(17) . . ? H27B C27 H27C 106.0(17) . . ? C24 C28 C30 109.74(11) . . ? C24 C28 C29 112.67(11) . . ? C30 C28 C29 110.05(14) . . ? C24 C28 H31 108.1(9) . . ? C30 C28 H31 105.7(10) . . ? C29 C28 H31 110.3(9) . . ? C28 C29 H29A 108.2(14) . . ? C28 C29 H29B 109.2(12) . . ? H29A C29 H29B 109.3(18) . . ? C28 C29 H29C 113.1(13) . . ? H29A C29 H29C 109.9(19) . . ? H29B C29 H29C 107.1(19) . . ? C28 C30 H30A 110.8(13) . . ? C28 C30 H30B 113.9(14) . . ? H30A C30 H30B 107.5(19) . . ? C28 C30 H30C 109.3(14) . . ? H30A C30 H30C 106.3(17) . . ? H30B C30 H30C 108.8(19) . . ? Si1 C31 H31A 107.7(14) . . ? Si1 C31 H31B 110.3(13) . . ? H31A C31 H31B 108.5(18) . . ? Si1 C31 H31C 108.6(12) . . ? H31A C31 H31C 112.5(18) . . ? H31B C31 H31C 109.2(18) . . ? Si1 C32 H32A 108.4(14) . . ? Si1 C32 H32B 111.6(13) . . ? H32A C32 H32B 107.0(19) . . ? Si1 C32 H32C 111.2(15) . . ? H32A C32 H32C 109(2) . . ? H32B C32 H32C 109(2) . . ? Si1 C33 H33A 112.2(11) . . ? Si1 C33 H33B 109.0(13) . . ? H33A C33 H33B 108.8(16) . . ? Si1 C33 H33C 111.9(14) . . ? H33A C33 H33C 110.6(18) . . ? H33B C33 H33C 103.9(18) . . ? C42 C41 C46 118.06(14) . . ? C42 C41 C47 121.64(16) . . ? C46 C41 C47 120.27(16) . . ? C41 C42 C43 121.28(16) . . ? C41 C42 H42 119.3(12) . . ? C43 C42 H42 119.3(12) . . ? C44 C43 C42 119.88(17) . . ? C44 C43 H43 120.4(13) . . ? C42 C43 H43 119.7(13) . . ? C43 C44 C45 119.71(16) . . ? C43 C44 H44 116.3(17) . . ? C45 C44 H44 124.0(17) . . ? C44 C45 C46 120.81(17) . . ? C44 C45 H45 118.7(13) . . ? C46 C45 H45 120.5(13) . . ? C45 C46 C41 120.24(16) . . ? C45 C46 H46 121.7(15) . . ? C41 C46 H46 118.0(15) . . ? C41 C47 H47A 112.8(19) . . ? C41 C47 H47B 112.7(17) . . ? H47A C47 H47B 111(3) . . ? C41 C47 H47C 115.7(16) . . ? H47A C47 H47C 97(2) . . ? H47B C47 H47C 107(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 30.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.768 _refine_diff_density_min -0.349 _refine_diff_density_rms 0.062 # Attachment '-4-MeOArSn-2.cif.txt' data_tw52s _database_code_depnum_ccdc_archive 'CCDC 771271' #TrackingRef '-4-MeOArSn-2.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H78 O2 Sn2, 2(C7 H8)' _chemical_formula_sum 'C76 H94 O2 Sn2' _chemical_formula_weight 1276.89 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.851(2) _cell_length_b 12.507(2) _cell_length_c 13.880(3) _cell_angle_alpha 96.444(3) _cell_angle_beta 97.785(3) _cell_angle_gamma 114.634(3) _cell_volume 1666.5(6) _cell_formula_units_Z 1 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 7309 _cell_measurement_theta_min 2.14 _cell_measurement_theta_max 27.50 _exptl_crystal_description Plate _exptl_crystal_colour Green _exptl_crystal_size_max 0.63 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.272 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 666 _exptl_absorpt_coefficient_mu 0.793 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6349 _exptl_absorpt_correction_T_max 0.9108 _exptl_absorpt_process_details 'TWINABS V1.05 (Sheldrick, 2003)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD' _diffrn_measurement_method '\w and \f' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 7273 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0406 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.51 _diffrn_reflns_theta_max 27.54 _reflns_number_total 7273 _reflns_number_gt 6857 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Version 5.054) (Bruker, 2002)' _computing_cell_refinement 'SAINT (7.23A) (Bruker, 2006)' _computing_data_reduction 'SAINT (7.23A) (Bruker, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL97 _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. The A and B alerts that follow are attributed to the twinning and HKLF5 file used to refine the structure. 029_ALERT_3_A _diffrn_measured_fraction_theta_full Low ....... 0.93 971_ALERT_2_A Large Calcd. Non-Metal Positive Residual Density 7.37 eA-3 971_ALERT_2_A Large Calcd. Non-Metal Positive Residual Density 5.74 eA-3 971_ALERT_2_A Large Calcd. Non-Metal Positive Residual Density 4.89 eA-3 971_ALERT_2_A Large Calcd. Non-Metal Positive Residual Density 4.25 eA-3 972_ALERT_2_A Large Calcd. Non-Metal Negative Residual Density -10.98 eA-3 972_ALERT_2_A Large Calcd. Non-Metal Negative Residual Density -3.73 eA-3 972_ALERT_2_A Large Calcd. Non-Metal Negative Residual Density -3.72 eA-3 972_ALERT_2_A Large Calcd. Non-Metal Negative Residual Density -3.63 eA-3 #============================================================================== 971_ALERT_2_B Large Calcd. Non-Metal Positive Residual Density 3.38 eA-3 971_ALERT_2_B Large Calcd. Non-Metal Positive Residual Density 3.02 eA-3 971_ALERT_2_B Large Calcd. Non-Metal Positive Residual Density 2.54 eA-3 972_ALERT_2_B Large Calcd. Non-Metal Negative Residual Density -3.29 eA-3 972_ALERT_2_B Large Calcd. Non-Metal Negative Residual Density -3.15 eA-3 972_ALERT_2_B Large Calcd. Non-Metal Negative Residual Density -3.05 eA-3 972_ALERT_2_B Large Calcd. Non-Metal Negative Residual Density -2.99 eA-3 972_ALERT_2_B Large Calcd. Non-Metal Negative Residual Density -2.96 eA-3 972_ALERT_2_B Large Calcd. Non-Metal Negative Residual Density -2.93 eA-3 972_ALERT_2_B Large Calcd. Non-Metal Negative Residual Density -2.93 eA-3 972_ALERT_2_B Large Calcd. Non-Metal Negative Residual Density -2.83 eA-3 972_ALERT_2_B Large Calcd. Non-Metal Negative Residual Density -2.83 eA-3 972_ALERT_2_B Large Calcd. Non-Metal Negative Residual Density -2.81 eA-3 972_ALERT_2_B Large Calcd. Non-Metal Negative Residual Density -2.79 eA-3 972_ALERT_2_B Large Calcd. Non-Metal Negative Residual Density -2.77 eA-3 972_ALERT_2_B Large Calcd. Non-Metal Negative Residual Density -2.70 eA-3 972_ALERT_2_B Large Calcd. Non-Metal Negative Residual Density -2.70 eA-3 972_ALERT_2_B Large Calcd. Non-Metal Negative Residual Density -2.69 eA-3 972_ALERT_2_B Large Calcd. Non-Metal Negative Residual Density -2.65 eA-3 972_ALERT_2_B Large Calcd. Non-Metal Negative Residual Density -2.61 eA-3 972_ALERT_2_B Large Calcd. Non-Metal Negative Residual Density -2.60 eA-3 972_ALERT_2_B Large Calcd. Non-Metal Negative Residual Density -2.60 eA-3 #============================================================================== The following query alerts are due to the three component HKLF5 file not being compatible with the current CIF generation. #============================================================================== The Following Improvement and Query ALERTS were generated - (Acta-Mode) <<< #============================================================================== 924_ALERT_1_A The Reported and Calculated Rho(min) Differ by . 18.11 eA-3 925_ALERT_1_A The Reported and Calculated Rho(max) Differ by . 5.39 eA-3 926_ALERT_1_A Reported and Calculated R1 * 100.0 Differ by . -21.38 927_ALERT_1_A Reported and Calculated wR2 * 100.0 Differ by . -45.83 928_ALERT_1_A Reported and Calculated S value Differ by . -3.16 ; _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^)+(0.0492P)^2^+13.5877P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 7273 _refine_ls_number_parameters 373 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0662 _refine_ls_R_factor_gt 0.0623 _refine_ls_wR_factor_ref 0.1696 _refine_ls_wR_factor_gt 0.1678 _refine_ls_goodness_of_fit_ref 1.163 _refine_ls_restrained_S_all 1.164 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.94861(6) 0.89425(5) 0.94080(4) 0.01656(13) Uani 1 1 d . . . O1 O 0.9131(6) 0.8097(5) 0.4770(4) 0.0222(12) Uani 1 1 d . . . C1 C 0.9382(7) 0.8694(7) 0.7825(5) 0.0156(14) Uani 1 1 d . . . C2 C 0.9908(7) 0.9650(7) 0.7304(6) 0.0138(14) Uani 1 1 d . . . C3 C 0.9799(7) 0.9396(7) 0.6287(6) 0.0152(15) Uani 1 1 d . . . H3 H 1.0155 1.0036 0.5939 0.018 Uiso 1 1 calc R . . C4 C 0.9177(7) 0.8219(7) 0.5768(5) 0.0148(13) Uani 1 1 d . . . C5 C 0.8659(8) 0.7275(7) 0.6273(6) 0.0176(15) Uani 1 1 d . . . H5 H 0.8235 0.6469 0.5927 0.021 Uiso 1 1 calc R . . C6 C 0.8772(7) 0.7528(7) 0.7291(6) 0.0147(14) Uani 1 1 d . . . C7 C 0.8571(9) 0.6916(8) 0.4212(6) 0.0276(19) Uani 1 1 d . . . H7A H 0.9151 0.6527 0.4430 0.041 Uiso 1 1 calc R . . H7B H 0.8547 0.6949 0.3508 0.041 Uiso 1 1 calc R . . H7C H 0.7630 0.6456 0.4312 0.041 Uiso 1 1 calc R . . C8 C 0.8190(7) 0.6481(6) 0.7824(5) 0.0130(14) Uani 1 1 d U . . C9 C 0.6823(8) 0.6064(7) 0.7950(6) 0.0161(15) Uani 1 1 d . . . C10 C 0.6305(9) 0.5088(8) 0.8452(6) 0.0237(17) Uani 1 1 d . . . H10 H 0.5383 0.4800 0.8556 0.028 Uiso 1 1 calc R . . C11 C 0.7120(9) 0.4551(6) 0.8790(6) 0.0201(15) Uani 1 1 d . . . H11 H 0.6750 0.3882 0.9105 0.024 Uiso 1 1 calc R . . C12 C 0.8466(9) 0.4988(7) 0.8668(7) 0.0233(17) Uani 1 1 d . . . H12 H 0.9023 0.4620 0.8911 0.028 Uiso 1 1 calc R . . C13 C 0.9039(8) 0.5962(7) 0.8197(6) 0.0181(15) Uani 1 1 d . . . C14 C 0.5859(8) 0.6605(7) 0.7569(6) 0.0203(16) Uani 1 1 d . . . H14 H 0.6404 0.7298 0.7266 0.024 Uiso 1 1 calc R . . C15 C 0.5325(10) 0.7068(9) 0.8388(7) 0.031(2) Uani 1 1 d . . . H15A H 0.4677 0.6392 0.8635 0.047 Uiso 1 1 calc R . . H15B H 0.4848 0.7525 0.8133 0.047 Uiso 1 1 calc R . . H15C H 0.6102 0.7589 0.8929 0.047 Uiso 1 1 calc R . . C16 C 0.4664(9) 0.5687(8) 0.6759(7) 0.030(2) Uani 1 1 d . . . H16A H 0.5036 0.5427 0.6222 0.045 Uiso 1 1 calc R . . H16B H 0.4077 0.6051 0.6500 0.045 Uiso 1 1 calc R . . H16C H 0.4115 0.4994 0.7036 0.045 Uiso 1 1 calc R . . C17 C 1.0536(8) 0.6425(7) 0.8078(6) 0.0174(15) Uani 1 1 d . . . H17 H 1.0799 0.7205 0.7847 0.021 Uiso 1 1 calc R . . C18 C 1.0667(11) 0.5546(9) 0.7277(7) 0.032(2) Uani 1 1 d . . . H18A H 1.1646 0.5800 0.7253 0.047 Uiso 1 1 calc R . . H18B H 1.0163 0.5536 0.6632 0.047 Uiso 1 1 calc R . . H18C H 1.0277 0.4740 0.7434 0.047 Uiso 1 1 calc R . . C19 C 1.1532(9) 0.6645(10) 0.9044(7) 0.031(2) Uani 1 1 d . . . H19A H 1.1369 0.7140 0.9563 0.047 Uiso 1 1 calc R . . H19B H 1.2487 0.7059 0.8953 0.047 Uiso 1 1 calc R . . H19C H 1.1382 0.5876 0.9237 0.047 Uiso 1 1 calc R . . C20 C 1.0606(8) 1.0920(7) 0.7864(6) 0.0166(15) Uani 1 1 d . . . C21 C 1.2014(8) 1.1459(7) 0.8245(6) 0.0166(14) Uani 1 1 d . . . C22 C 1.2620(9) 1.2641(7) 0.8780(6) 0.0207(16) Uani 1 1 d . . . H22 H 1.3583 1.3024 0.9060 0.025 Uiso 1 1 calc R . . C23 C 1.1816(10) 1.3256(7) 0.8903(6) 0.0256(19) Uani 1 1 d . . . H23 H 1.2239 1.4063 0.9247 0.031 Uiso 1 1 calc R . . C24 C 1.0428(9) 1.2702(7) 0.8531(6) 0.0234(17) Uani 1 1 d . . . H24 H 0.9890 1.3123 0.8640 0.028 Uiso 1 1 calc R . . C25 C 0.9774(8) 1.1531(7) 0.7992(6) 0.0177(15) Uani 1 1 d . . . C26 C 1.2935(8) 1.0845(8) 0.8079(6) 0.0206(16) Uani 1 1 d . . . H26 H 1.2306 0.9978 0.7819 0.025 Uiso 1 1 calc R . . C27 C 1.3715(9) 1.1314(9) 0.7272(7) 0.029(2) Uani 1 1 d . . . H27A H 1.3054 1.1207 0.6672 0.044 Uiso 1 1 calc R . . H27B H 1.4252 1.0872 0.7130 0.044 Uiso 1 1 calc R . . H27C H 1.4342 1.2167 0.7495 0.044 Uiso 1 1 calc R . . C28 C 1.3882(9) 1.0905(9) 0.9015(7) 0.031(2) Uani 1 1 d . . . H28A H 1.4596 1.1730 0.9250 0.047 Uiso 1 1 calc R . . H28B H 1.4321 1.0377 0.8875 0.047 Uiso 1 1 calc R . . H28C H 1.3339 1.0647 0.9527 0.047 Uiso 1 1 calc R . . C29 C 0.8240(8) 1.0960(7) 0.7527(6) 0.0187(15) Uani 1 1 d . . . H29 H 0.7929 1.0078 0.7338 0.022 Uiso 1 1 calc R . . C30 C 0.7995(10) 1.1422(9) 0.6591(7) 0.034(2) Uani 1 1 d . . . H30A H 0.8393 1.2298 0.6742 0.051 Uiso 1 1 calc R . . H30B H 0.6998 1.1093 0.6331 0.051 Uiso 1 1 calc R . . H30C H 0.8436 1.1175 0.6097 0.051 Uiso 1 1 calc R . . C31 C 0.7388(9) 1.1151(10) 0.8242(7) 0.035(2) Uani 1 1 d . . . H31A H 0.7541 1.0824 0.8832 0.053 Uiso 1 1 calc R . . H31B H 0.6405 1.0743 0.7925 0.053 Uiso 1 1 calc R . . H31C H 0.7665 1.2010 0.8434 0.053 Uiso 1 1 calc R . . C41 C 0.3303(9) 0.7724(7) 0.5600(6) 0.0218(16) Uani 1 1 d . . . C42 C 0.2716(9) 0.6739(7) 0.4843(7) 0.0265(17) Uani 1 1 d . . . H42 H 0.1740 0.6271 0.4694 0.032 Uiso 1 1 calc R . . C43 C 0.3541(13) 0.6422(9) 0.4292(7) 0.039(3) Uani 1 1 d . . . H43 H 0.3125 0.5755 0.3760 0.047 Uiso 1 1 calc R . . C44 C 0.4937(12) 0.7068(10) 0.4517(9) 0.042(3) Uani 1 1 d . . . H44 H 0.5494 0.6842 0.4148 0.050 Uiso 1 1 calc R . . C45 C 0.5558(10) 0.8054(10) 0.5280(8) 0.038(2) Uani 1 1 d . . . H45 H 0.6535 0.8511 0.5429 0.046 Uiso 1 1 calc R . . C46 C 0.4723(9) 0.8371(8) 0.5832(7) 0.029(2) Uani 1 1 d . . . H46 H 0.5141 0.9035 0.6367 0.035 Uiso 1 1 calc R . . C47 C 0.2412(10) 0.8109(10) 0.6153(8) 0.037(2) Uani 1 1 d . . . H47A H 0.2990 0.8697 0.6751 0.055 Uiso 1 1 calc R . . H47B H 0.1709 0.7410 0.6339 0.055 Uiso 1 1 calc R . . H47C H 0.1957 0.8470 0.5730 0.055 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 0.0223(3) 0.01337(19) 0.01114(19) 0.00114(18) 0.00362(17) 0.0053(2) O1 0.029(3) 0.018(3) 0.014(3) 0.001(2) 0.004(2) 0.005(2) C1 0.018(4) 0.016(3) 0.016(3) 0.004(3) 0.005(3) 0.011(3) C2 0.015(3) 0.015(4) 0.014(4) 0.008(3) 0.002(3) 0.008(3) C3 0.012(3) 0.015(4) 0.016(4) 0.001(3) 0.002(3) 0.005(3) C4 0.015(3) 0.017(3) 0.012(3) 0.002(3) 0.002(3) 0.007(3) C5 0.019(4) 0.012(3) 0.019(4) 0.003(3) 0.003(3) 0.005(3) C6 0.012(3) 0.013(3) 0.021(4) 0.007(3) 0.005(3) 0.006(3) C7 0.033(5) 0.020(4) 0.017(4) -0.006(3) 0.002(3) 0.002(4) C8 0.015(2) 0.010(2) 0.010(2) -0.0015(15) -0.0001(15) 0.0034(16) C9 0.016(3) 0.014(4) 0.012(4) -0.003(3) -0.004(3) 0.004(3) C10 0.027(4) 0.022(4) 0.018(4) 0.001(3) 0.003(3) 0.008(3) C11 0.027(4) 0.011(3) 0.020(4) 0.008(3) 0.008(3) 0.003(3) C12 0.030(4) 0.016(4) 0.026(5) 0.005(3) 0.003(3) 0.013(3) C13 0.021(4) 0.015(3) 0.017(4) 0.000(3) 0.003(3) 0.007(3) C14 0.016(4) 0.019(4) 0.026(4) 0.006(3) 0.002(3) 0.009(3) C15 0.030(5) 0.041(5) 0.030(5) 0.005(4) 0.009(4) 0.022(4) C16 0.028(5) 0.025(4) 0.031(5) 0.003(4) -0.005(4) 0.010(4) C17 0.019(4) 0.017(4) 0.020(4) 0.003(3) 0.002(3) 0.012(3) C18 0.039(5) 0.034(5) 0.033(5) 0.013(4) 0.018(4) 0.022(4) C19 0.021(4) 0.047(5) 0.025(4) 0.006(4) -0.001(3) 0.015(4) C20 0.029(4) 0.013(3) 0.013(4) 0.008(3) 0.005(3) 0.013(3) C21 0.020(4) 0.014(3) 0.016(4) 0.003(3) 0.008(3) 0.006(3) C22 0.025(4) 0.015(4) 0.017(4) 0.000(3) 0.002(3) 0.006(3) C23 0.046(5) 0.016(4) 0.014(4) 0.005(3) 0.007(4) 0.011(4) C24 0.036(5) 0.015(4) 0.028(4) 0.008(3) 0.010(4) 0.016(4) C25 0.019(4) 0.017(4) 0.019(4) 0.004(3) 0.005(3) 0.009(3) C26 0.014(4) 0.030(4) 0.016(4) 0.002(3) 0.003(3) 0.009(3) C27 0.025(4) 0.038(5) 0.025(5) 0.010(4) 0.012(4) 0.011(4) C28 0.029(5) 0.041(6) 0.029(5) 0.009(4) 0.007(4) 0.019(4) C29 0.020(4) 0.023(4) 0.016(4) 0.006(3) 0.003(3) 0.012(3) C30 0.028(5) 0.038(5) 0.034(5) 0.019(4) 0.001(4) 0.011(4) C31 0.024(4) 0.052(6) 0.033(5) 0.007(5) 0.004(4) 0.019(4) C41 0.028(4) 0.020(4) 0.023(4) 0.009(3) 0.006(3) 0.014(3) C42 0.025(4) 0.022(4) 0.028(4) 0.004(3) 0.000(3) 0.008(3) C43 0.073(8) 0.025(5) 0.018(4) 0.002(4) 0.006(4) 0.022(5) C44 0.060(7) 0.042(6) 0.051(7) 0.026(5) 0.037(6) 0.036(6) C45 0.028(5) 0.037(5) 0.060(7) 0.019(5) 0.023(5) 0.018(4) C46 0.024(4) 0.026(5) 0.033(5) 0.002(4) 0.002(3) 0.009(4) C47 0.028(5) 0.037(5) 0.055(6) 0.014(5) 0.019(4) 0.020(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C1 2.165(7) . ? Sn1 Sn1 2.6476(12) 2_777 ? O1 C4 1.368(9) . ? O1 C7 1.422(9) . ? C1 C6 1.391(10) . ? C1 C2 1.420(10) . ? C2 C3 1.389(11) . ? C2 C20 1.504(11) . ? C3 C4 1.394(10) . ? C3 H3 0.9500 . ? C4 C5 1.394(11) . ? C5 C6 1.390(11) . ? C5 H5 0.9500 . ? C6 C8 1.522(10) . ? C7 H7A 0.9800 . ? C7 H7B 0.9800 . ? C7 H7C 0.9800 . ? C8 C9 1.396(10) . ? C8 C13 1.408(10) . ? C9 C10 1.420(12) . ? C9 C14 1.533(10) . ? C10 C11 1.380(12) . ? C10 H10 0.9500 . ? C11 C12 1.372(12) . ? C11 H11 0.9500 . ? C12 C13 1.399(12) . ? C12 H12 0.9500 . ? C13 C17 1.520(11) . ? C14 C15 1.508(11) . ? C14 C16 1.529(11) . ? C14 H14 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C19 1.522(11) . ? C17 C18 1.538(11) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C20 C21 1.382(11) . ? C20 C25 1.421(10) . ? C21 C22 1.408(10) . ? C21 C26 1.518(10) . ? C22 C23 1.397(12) . ? C22 H22 0.9500 . ? C23 C24 1.362(13) . ? C23 H23 0.9500 . ? C24 C25 1.397(11) . ? C24 H24 0.9500 . ? C25 C29 1.521(11) . ? C26 C28 1.517(12) . ? C26 C27 1.518(11) . ? C26 H26 1.0000 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 H28A 0.9800 . ? C28 H28B 0.9800 . ? C28 H28C 0.9800 . ? C29 C31 1.509(12) . ? C29 C30 1.514(12) . ? C29 H29 1.0000 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C41 C46 1.378(12) . ? C41 C42 1.379(11) . ? C41 C47 1.504(12) . ? C42 C43 1.399(14) . ? C42 H42 0.9500 . ? C43 C44 1.356(16) . ? C43 H43 0.9500 . ? C44 C45 1.384(16) . ? C44 H44 0.9500 . ? C45 C46 1.409(12) . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Sn1 Sn1 124.2(2) . 2_777 ? C4 O1 C7 117.5(6) . . ? C6 C1 C2 118.2(6) . . ? C6 C1 Sn1 117.9(6) . . ? C2 C1 Sn1 123.9(5) . . ? C3 C2 C1 119.4(7) . . ? C3 C2 C20 121.0(7) . . ? C1 C2 C20 119.5(7) . . ? C2 C3 C4 121.2(7) . . ? C2 C3 H3 119.4 . . ? C4 C3 H3 119.4 . . ? O1 C4 C3 115.2(7) . . ? O1 C4 C5 125.1(7) . . ? C3 C4 C5 119.8(7) . . ? C6 C5 C4 119.0(7) . . ? C6 C5 H5 120.5 . . ? C4 C5 H5 120.5 . . ? C5 C6 C1 122.3(7) . . ? C5 C6 C8 117.9(7) . . ? C1 C6 C8 119.7(7) . . ? O1 C7 H7A 109.5 . . ? O1 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? O1 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? C9 C8 C13 121.0(7) . . ? C9 C8 C6 119.2(6) . . ? C13 C8 C6 119.8(6) . . ? C8 C9 C10 118.1(7) . . ? C8 C9 C14 123.2(7) . . ? C10 C9 C14 118.8(7) . . ? C11 C10 C9 121.1(8) . . ? C11 C10 H10 119.5 . . ? C9 C10 H10 119.5 . . ? C12 C11 C10 119.7(7) . . ? C12 C11 H11 120.1 . . ? C10 C11 H11 120.1 . . ? C11 C12 C13 121.7(7) . . ? C11 C12 H12 119.2 . . ? C13 C12 H12 119.2 . . ? C12 C13 C8 118.4(7) . . ? C12 C13 C17 120.2(7) . . ? C8 C13 C17 121.4(7) . . ? C15 C14 C16 111.0(7) . . ? C15 C14 C9 112.4(7) . . ? C16 C14 C9 110.0(7) . . ? C15 C14 H14 107.8 . . ? C16 C14 H14 107.8 . . ? C9 C14 H14 107.8 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C13 C17 C19 112.7(7) . . ? C13 C17 C18 109.7(7) . . ? C19 C17 C18 110.6(7) . . ? C13 C17 H17 107.9 . . ? C19 C17 H17 107.9 . . ? C18 C17 H17 107.9 . . ? C17 C18 H18A 109.5 . . ? C17 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C17 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C17 C19 H19A 109.5 . . ? C17 C19 H19B 109.5 . . ? H19A C19 H19B 109.5 . . ? C17 C19 H19C 109.5 . . ? H19A C19 H19C 109.5 . . ? H19B C19 H19C 109.5 . . ? C21 C20 C25 121.8(7) . . ? C21 C20 C2 120.3(6) . . ? C25 C20 C2 118.0(7) . . ? C20 C21 C22 118.3(7) . . ? C20 C21 C26 122.7(7) . . ? C22 C21 C26 118.9(7) . . ? C23 C22 C21 120.5(8) . . ? C23 C22 H22 119.8 . . ? C21 C22 H22 119.8 . . ? C24 C23 C22 120.2(7) . . ? C24 C23 H23 119.9 . . ? C22 C23 H23 119.9 . . ? C23 C24 C25 121.7(7) . . ? C23 C24 H24 119.2 . . ? C25 C24 H24 119.2 . . ? C24 C25 C20 117.5(7) . . ? C24 C25 C29 120.7(7) . . ? C20 C25 C29 121.7(7) . . ? C28 C26 C27 112.7(7) . . ? C28 C26 C21 114.0(7) . . ? C27 C26 C21 109.6(7) . . ? C28 C26 H26 106.7 . . ? C27 C26 H26 106.7 . . ? C21 C26 H26 106.7 . . ? C26 C27 H27A 109.5 . . ? C26 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C26 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C26 C28 H28A 109.5 . . ? C26 C28 H28B 109.5 . . ? H28A C28 H28B 109.5 . . ? C26 C28 H28C 109.5 . . ? H28A C28 H28C 109.5 . . ? H28B C28 H28C 109.5 . . ? C31 C29 C30 110.9(7) . . ? C31 C29 C25 111.9(7) . . ? C30 C29 C25 110.7(7) . . ? C31 C29 H29 107.7 . . ? C30 C29 H29 107.7 . . ? C25 C29 H29 107.7 . . ? C29 C30 H30A 109.5 . . ? C29 C30 H30B 109.5 . . ? H30A C30 H30B 109.5 . . ? C29 C30 H30C 109.5 . . ? H30A C30 H30C 109.5 . . ? H30B C30 H30C 109.5 . . ? C29 C31 H31A 109.5 . . ? C29 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? C29 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C46 C41 C42 119.1(8) . . ? C46 C41 C47 120.1(8) . . ? C42 C41 C47 120.8(8) . . ? C41 C42 C43 120.7(9) . . ? C41 C42 H42 119.7 . . ? C43 C42 H42 119.7 . . ? C44 C43 C42 120.0(9) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 120.7(9) . . ? C43 C44 H44 119.7 . . ? C45 C44 H44 119.7 . . ? C44 C45 C46 119.2(9) . . ? C44 C45 H45 120.4 . . ? C46 C45 H45 120.4 . . ? C41 C46 C45 120.3(9) . . ? C41 C46 H46 119.8 . . ? C45 C46 H46 119.8 . . ? C41 C47 H47A 109.5 . . ? C41 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C41 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 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 Sn1 Sn1 C1 C6 -177.9(4) 2_777 . . . ? Sn1 Sn1 C1 C2 2.6(7) 2_777 . . . ? C6 C1 C2 C3 0.0(10) . . . . ? Sn1 C1 C2 C3 179.5(5) . . . . ? C6 C1 C2 C20 -178.4(7) . . . . ? Sn1 C1 C2 C20 1.1(9) . . . . ? C1 C2 C3 C4 0.3(11) . . . . ? C20 C2 C3 C4 178.7(6) . . . . ? C7 O1 C4 C3 176.9(7) . . . . ? C7 O1 C4 C5 -3.2(11) . . . . ? C2 C3 C4 O1 179.6(6) . . . . ? C2 C3 C4 C5 -0.4(11) . . . . ? O1 C4 C5 C6 -179.8(7) . . . . ? C3 C4 C5 C6 0.1(10) . . . . ? C4 C5 C6 C1 0.2(11) . . . . ? C4 C5 C6 C8 179.6(6) . . . . ? C2 C1 C6 C5 -0.3(10) . . . . ? Sn1 C1 C6 C5 -179.8(5) . . . . ? C2 C1 C6 C8 -179.7(6) . . . . ? Sn1 C1 C6 C8 0.8(8) . . . . ? C5 C6 C8 C9 -91.4(8) . . . . ? C1 C6 C8 C9 88.0(9) . . . . ? C5 C6 C8 C13 89.8(9) . . . . ? C1 C6 C8 C13 -90.8(8) . . . . ? C13 C8 C9 C10 -1.1(11) . . . . ? C6 C8 C9 C10 -179.9(7) . . . . ? C13 C8 C9 C14 179.3(7) . . . . ? C6 C8 C9 C14 0.5(11) . . . . ? C8 C9 C10 C11 -1.1(11) . . . . ? C14 C9 C10 C11 178.5(7) . . . . ? C9 C10 C11 C12 2.0(12) . . . . ? C10 C11 C12 C13 -0.8(12) . . . . ? C11 C12 C13 C8 -1.4(12) . . . . ? C11 C12 C13 C17 179.8(7) . . . . ? C9 C8 C13 C12 2.3(11) . . . . ? C6 C8 C13 C12 -179.0(7) . . . . ? C9 C8 C13 C17 -178.9(7) . . . . ? C6 C8 C13 C17 -0.2(11) . . . . ? C8 C9 C14 C15 -121.4(9) . . . . ? C10 C9 C14 C15 59.0(10) . . . . ? C8 C9 C14 C16 114.4(8) . . . . ? C10 C9 C14 C16 -65.2(10) . . . . ? C12 C13 C17 C19 -50.3(10) . . . . ? C8 C13 C17 C19 131.0(8) . . . . ? C12 C13 C17 C18 73.4(10) . . . . ? C8 C13 C17 C18 -105.3(8) . . . . ? C3 C2 C20 C21 -89.1(9) . . . . ? C1 C2 C20 C21 89.2(9) . . . . ? C3 C2 C20 C25 91.3(9) . . . . ? C1 C2 C20 C25 -90.3(9) . . . . ? C25 C20 C21 C22 0.7(12) . . . . ? C2 C20 C21 C22 -178.8(7) . . . . ? C25 C20 C21 C26 -177.2(7) . . . . ? C2 C20 C21 C26 3.3(11) . . . . ? C20 C21 C22 C23 -1.3(12) . . . . ? C26 C21 C22 C23 176.7(7) . . . . ? C21 C22 C23 C24 2.1(12) . . . . ? C22 C23 C24 C25 -2.1(13) . . . . ? C23 C24 C25 C20 1.5(12) . . . . ? C23 C24 C25 C29 -175.9(8) . . . . ? C21 C20 C25 C24 -0.7(12) . . . . ? C2 C20 C25 C24 178.8(7) . . . . ? C21 C20 C25 C29 176.6(7) . . . . ? C2 C20 C25 C29 -3.8(11) . . . . ? C20 C21 C26 C28 -131.2(8) . . . . ? C22 C21 C26 C28 50.8(11) . . . . ? C20 C21 C26 C27 101.3(9) . . . . ? C22 C21 C26 C27 -76.6(9) . . . . ? C24 C25 C29 C31 -47.0(11) . . . . ? C20 C25 C29 C31 135.7(8) . . . . ? C24 C25 C29 C30 77.2(10) . . . . ? C20 C25 C29 C30 -100.1(9) . . . . ? C46 C41 C42 C43 -2.3(13) . . . . ? C47 C41 C42 C43 176.3(9) . . . . ? C41 C42 C43 C44 1.7(14) . . . . ? C42 C43 C44 C45 -1.0(15) . . . . ? C43 C44 C45 C46 0.9(16) . . . . ? C42 C41 C46 C45 2.2(13) . . . . ? C47 C41 C46 C45 -176.4(9) . . . . ? C44 C45 C46 C41 -1.5(15) . . . . ? _diffrn_measured_fraction_theta_max 0.933 _diffrn_reflns_theta_full 27.54 _diffrn_measured_fraction_theta_full 0.933 _refine_diff_density_max 1.978 _refine_diff_density_min -1.739 _refine_diff_density_rms 0.165 # Attachment '-4-tBuArSn-2.CIF.txt' data_rw35 _database_code_depnum_ccdc_archive 'CCDC 771272' #TrackingRef '-4-tBuArSn-2.CIF.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C82 H106 Sn2' _chemical_formula_weight 1329.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 10.5215(6) _cell_length_b 12.0825(7) _cell_length_c 15.3370(9) _cell_angle_alpha 103.2180(10) _cell_angle_beta 107.0010(10) _cell_angle_gamma 91.5410(10) _cell_volume 1805.90(18) _cell_formula_units_Z 1 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 8266 _cell_measurement_theta_min 2.9631 _cell_measurement_theta_max 29.5496 _exptl_crystal_description plate _exptl_crystal_colour green _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.222 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 698 _exptl_absorpt_coefficient_mu 0.733 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.8212 _exptl_absorpt_correction_T_max 0.9574 _exptl_absorpt_process_details 'SADABS 2008/2 (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEXII' _diffrn_measurement_method '\w and \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23153 _diffrn_reflns_av_R_equivalents 0.0327 _diffrn_reflns_av_sigmaI/netI 0.0459 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 29.57 _reflns_number_total 10013 _reflns_number_gt 8407 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEXII software' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _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. Hydrogen atoms were located directly from difference-Fourier maps. Hydrogen atoms were freely refined accounting for angle deviations. ; _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^)+(0.1000P)^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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 10013 _refine_ls_number_parameters 591 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0441 _refine_ls_R_factor_gt 0.0328 _refine_ls_wR_factor_ref 0.1041 _refine_ls_wR_factor_gt 0.0930 _refine_ls_goodness_of_fit_ref 0.767 _refine_ls_restrained_S_all 0.767 _refine_ls_shift/su_max 0.003 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.526570(15) 0.530503(11) 0.592512(10) 0.01909(6) Uani 1 1 d . . . C1 C 0.59481(19) 0.70373(17) 0.67756(14) 0.0141(3) Uani 1 1 d . . . C2 C 0.61597(19) 0.79743(17) 0.64174(13) 0.0142(3) Uani 1 1 d . . . C3 C 0.6677(2) 0.90351(17) 0.70290(14) 0.0149(4) Uani 1 1 d . . . H3 H 0.680(3) 0.959(2) 0.6774(18) 0.014(6) Uiso 1 1 d . . . C4 C 0.70355(19) 0.92092(16) 0.80095(14) 0.0137(3) Uani 1 1 d . . . C5 C 0.68015(19) 0.82749(17) 0.83580(13) 0.0148(4) Uani 1 1 d . . . H5 H 0.704(3) 0.836(2) 0.9006(19) 0.017(6) Uiso 1 1 d . . . C6 C 0.62647(19) 0.72043(17) 0.77555(14) 0.0141(3) Uani 1 1 d . . . C7 C 0.58856(19) 0.77995(16) 0.53772(13) 0.0136(3) Uani 1 1 d . . . C8 C 0.4601(2) 0.78999(17) 0.48009(14) 0.0158(4) Uani 1 1 d . . . C9 C 0.4375(2) 0.77007(19) 0.38326(15) 0.0191(4) Uani 1 1 d . . . H9 H 0.360(3) 0.773(2) 0.3468(19) 0.014(6) Uiso 1 1 d . . . C10 C 0.5392(2) 0.74216(19) 0.34376(15) 0.0215(4) Uani 1 1 d . . . H10 H 0.526(3) 0.730(3) 0.277(2) 0.027(7) Uiso 1 1 d . . . C11 C 0.6655(2) 0.73242(19) 0.40128(15) 0.0190(4) Uani 1 1 d . . . H11 H 0.730(3) 0.715(2) 0.3743(19) 0.015(6) Uiso 1 1 d . . . C12 C 0.6928(2) 0.75025(17) 0.49844(14) 0.0157(4) Uani 1 1 d . . . C13 C 0.6080(2) 0.62144(17) 0.81596(13) 0.0140(3) Uani 1 1 d . . . C14 C 0.4846(2) 0.59410(17) 0.82838(13) 0.0157(4) Uani 1 1 d . . . C15 C 0.4716(2) 0.50320(19) 0.86857(15) 0.0192(4) Uani 1 1 d . . . H15 H 0.398(3) 0.482(3) 0.883(2) 0.035(8) Uiso 1 1 d . . . C16 C 0.5789(2) 0.44069(19) 0.89649(15) 0.0208(4) Uani 1 1 d . . . H16 H 0.573(3) 0.375(3) 0.926(2) 0.037(9) Uiso 1 1 d . . . C17 C 0.6998(2) 0.46709(19) 0.88306(15) 0.0203(4) Uani 1 1 d . . . H17 H 0.775(3) 0.422(2) 0.902(2) 0.021(7) Uiso 1 1 d . . . C18 C 0.7167(2) 0.55679(17) 0.84230(14) 0.0165(4) Uani 1 1 d . . . C19 C 0.7702(2) 1.03727(18) 0.86504(14) 0.0182(4) Uani 1 1 d . . . C20 C 0.8120(2) 1.0363(2) 0.96932(15) 0.0228(4) Uani 1 1 d . . . H20A H 0.869(3) 0.980(3) 0.985(2) 0.027(7) Uiso 1 1 d . . . H20B H 0.724(3) 1.030(3) 0.985(2) 0.028(8) Uiso 1 1 d . . . H20C H 0.862(3) 1.106(3) 1.004(2) 0.037(8) Uiso 1 1 d . . . C21 C 0.6730(3) 1.1293(2) 0.85005(18) 0.0287(5) Uani 1 1 d . . . H21A H 0.598(3) 1.112(3) 0.868(2) 0.027(7) Uiso 1 1 d . . . H21B H 0.641(3) 1.136(3) 0.789(2) 0.028(7) Uiso 1 1 d . . . H21C H 0.715(3) 1.204(3) 0.890(2) 0.033(8) Uiso 1 1 d . . . C22 C 0.8954(3) 1.0688(2) 0.84070(19) 0.0317(6) Uani 1 1 d . . . H22A H 0.941(3) 1.139(3) 0.883(2) 0.037(9) Uiso 1 1 d . . . H22B H 0.875(3) 1.076(3) 0.781(2) 0.034(8) Uiso 1 1 d . . . H22C H 0.955(3) 1.010(3) 0.844(2) 0.042(9) Uiso 1 1 d . . . C23 C 0.3478(2) 0.82437(19) 0.52180(15) 0.0182(4) Uani 1 1 d . . . H23 H 0.372(3) 0.820(3) 0.582(2) 0.027(7) Uiso 1 1 d . . . C24 C 0.2175(3) 0.7481(3) 0.4688(3) 0.0499(9) Uani 1 1 d . . . H24C H 0.152(4) 0.761(3) 0.496(3) 0.042(9) Uiso 1 1 d . . . H24B H 0.242(5) 0.665(5) 0.479(4) 0.092(17) Uiso 1 1 d . . . H24A H 0.177(5) 0.759(4) 0.401(4) 0.092(17) Uiso 1 1 d . . . C25 C 0.3256(4) 0.9483(3) 0.5245(3) 0.0443(8) Uani 1 1 d . . . H25A H 0.257(4) 0.964(4) 0.549(3) 0.060(12) Uiso 1 1 d . . . H25B H 0.395(5) 1.001(4) 0.556(3) 0.078(15) Uiso 1 1 d . . . H25C H 0.303(4) 0.968(3) 0.462(3) 0.048(10) Uiso 1 1 d . . . C26 C 0.8321(2) 0.7394(2) 0.56007(15) 0.0198(4) Uani 1 1 d . . . H26 H 0.825(3) 0.726(2) 0.6186(19) 0.015(6) Uiso 1 1 d . . . C27 C 0.8940(2) 0.6356(2) 0.51721(19) 0.0274(5) Uani 1 1 d . . . H27A H 0.976(3) 0.629(3) 0.559(2) 0.030(8) Uiso 1 1 d . . . H27B H 0.836(3) 0.564(3) 0.500(2) 0.037(9) Uiso 1 1 d . . . H27C H 0.910(3) 0.642(3) 0.455(2) 0.037(8) Uiso 1 1 d . . . C28 C 0.9238(2) 0.8489(2) 0.5815(2) 0.0316(6) Uani 1 1 d . . . H28C H 0.887(3) 0.917(3) 0.614(2) 0.026(7) Uiso 1 1 d . . . H28B H 0.934(4) 0.871(3) 0.528(3) 0.050(10) Uiso 1 1 d . . . H28A H 1.010(4) 0.838(3) 0.614(3) 0.053(10) Uiso 1 1 d . . . C29 C 0.8505(2) 0.5839(2) 0.82875(17) 0.0214(4) Uani 1 1 d . . . H29 H 0.839(3) 0.628(2) 0.789(2) 0.021(7) Uiso 1 1 d . . . C30 C 0.9562(3) 0.6359(3) 0.9234(2) 0.0389(6) Uani 1 1 d . . . H30A H 1.042(4) 0.653(3) 0.916(3) 0.053(11) Uiso 1 1 d . . . H30B H 0.935(4) 0.694(4) 0.961(3) 0.061(12) Uiso 1 1 d . . . H30C H 0.973(4) 0.582(4) 0.967(3) 0.069(13) Uiso 1 1 d . . . C31 C 0.8957(3) 0.4778(3) 0.7740(3) 0.0419(7) Uani 1 1 d . . . H31A H 0.827(4) 0.451(3) 0.713(3) 0.047(10) Uiso 1 1 d . . . H31B H 0.975(4) 0.491(3) 0.766(3) 0.055(11) Uiso 1 1 d . . . H31C H 0.917(4) 0.416(4) 0.813(3) 0.067(13) Uiso 1 1 d . . . C32 C 0.3656(2) 0.66212(19) 0.80108(15) 0.0192(4) Uani 1 1 d . . . H32 H 0.391(2) 0.719(2) 0.7741(18) 0.012(6) Uiso 1 1 d . . . C33 C 0.2457(3) 0.5866(3) 0.7279(2) 0.0350(6) Uani 1 1 d . . . H33C H 0.173(3) 0.630(3) 0.713(2) 0.031(8) Uiso 1 1 d . . . H33B H 0.220(3) 0.524(3) 0.751(2) 0.036(9) Uiso 1 1 d . . . H33A H 0.267(4) 0.555(3) 0.672(3) 0.053(11) Uiso 1 1 d . . . C34 C 0.3267(3) 0.7212(3) 0.88777(19) 0.0331(6) Uani 1 1 d . . . H34A H 0.244(3) 0.768(3) 0.869(2) 0.028(7) Uiso 1 1 d . . . H34B H 0.394(4) 0.763(3) 0.933(3) 0.051(11) Uiso 1 1 d . . . H34C H 0.294(3) 0.665(3) 0.919(3) 0.041(9) Uiso 1 1 d . . . C101 C 0.2659(2) 0.0887(2) 0.80170(17) 0.0264(5) Uani 1 1 d . . . C102 C 0.3204(3) 0.1569(2) 0.89278(17) 0.0270(5) Uani 1 1 d . . . H102 H 0.389(4) 0.126(4) 0.941(3) 0.068(13) Uiso 1 1 d . . . C103 C 0.2812(3) 0.2648(2) 0.91999(18) 0.0286(5) Uani 1 1 d . . . H103 H 0.309(4) 0.301(4) 0.980(3) 0.068(13) Uiso 1 1 d . . . C104 C 0.1839(3) 0.3055(2) 0.85621(18) 0.0281(5) Uani 1 1 d . . . H104 H 0.154(3) 0.379(3) 0.872(2) 0.031(8) Uiso 1 1 d . . . C105 C 0.1267(3) 0.2383(2) 0.76487(18) 0.0296(5) Uani 1 1 d . . . H105 H 0.060(3) 0.270(3) 0.720(2) 0.032(8) Uiso 1 1 d . . . C106 C 0.1673(2) 0.1314(2) 0.73898(17) 0.0287(5) Uani 1 1 d . . . H106 H 0.133(3) 0.090(2) 0.681(2) 0.021(7) Uiso 1 1 d . . . C107 C 0.3115(4) -0.0280(3) 0.7730(3) 0.0451(8) Uani 1 1 d . . . H17C H 0.246(5) -0.087(4) 0.733(4) 0.081(15) Uiso 1 1 d . . . H17B H 0.359(6) -0.031(5) 0.741(4) 0.10(2) Uiso 1 1 d . . . H17A H 0.362(5) -0.051(4) 0.821(4) 0.072(14) Uiso 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 0.02721(9) 0.01359(8) 0.01553(8) 0.00027(5) 0.00815(6) -0.00294(5) C1 0.0145(8) 0.0141(9) 0.0146(8) 0.0023(7) 0.0069(7) -0.0010(7) C2 0.0150(8) 0.0160(9) 0.0123(8) 0.0033(7) 0.0056(7) 0.0012(7) C3 0.0178(9) 0.0122(9) 0.0164(9) 0.0047(7) 0.0070(7) 0.0007(7) C4 0.0136(8) 0.0121(8) 0.0149(8) 0.0019(7) 0.0046(7) 0.0005(6) C5 0.0156(9) 0.0174(9) 0.0111(8) 0.0034(7) 0.0038(7) 0.0015(7) C6 0.0137(8) 0.0143(9) 0.0153(9) 0.0049(7) 0.0053(7) 0.0014(7) C7 0.0169(9) 0.0121(8) 0.0124(8) 0.0037(7) 0.0051(7) -0.0014(7) C8 0.0189(9) 0.0127(9) 0.0165(9) 0.0038(7) 0.0064(7) 0.0014(7) C9 0.0202(10) 0.0203(10) 0.0152(9) 0.0042(8) 0.0030(8) 0.0024(8) C10 0.0309(11) 0.0228(11) 0.0126(9) 0.0052(8) 0.0084(8) 0.0058(8) C11 0.0221(10) 0.0213(10) 0.0168(9) 0.0057(8) 0.0100(8) 0.0034(8) C12 0.0172(9) 0.0158(9) 0.0132(8) 0.0035(7) 0.0037(7) -0.0006(7) C13 0.0186(9) 0.0128(8) 0.0107(8) 0.0025(7) 0.0047(7) 0.0022(7) C14 0.0187(9) 0.0157(9) 0.0124(8) 0.0030(7) 0.0050(7) 0.0008(7) C15 0.0215(10) 0.0197(10) 0.0180(9) 0.0039(8) 0.0092(8) -0.0034(8) C16 0.0308(11) 0.0156(9) 0.0178(9) 0.0067(8) 0.0085(8) 0.0005(8) C17 0.0243(10) 0.0183(10) 0.0178(9) 0.0052(8) 0.0050(8) 0.0054(8) C18 0.0179(9) 0.0161(9) 0.0155(9) 0.0029(7) 0.0061(7) 0.0008(7) C19 0.0220(10) 0.0156(9) 0.0150(9) 0.0013(7) 0.0052(7) -0.0024(7) C20 0.0317(12) 0.0176(10) 0.0147(9) 0.0004(8) 0.0036(8) -0.0046(9) C21 0.0397(14) 0.0164(10) 0.0246(11) 0.0013(9) 0.0042(10) 0.0057(9) C22 0.0317(13) 0.0339(14) 0.0241(12) -0.0037(10) 0.0105(10) -0.0177(11) C23 0.0169(9) 0.0210(10) 0.0180(9) 0.0067(8) 0.0057(7) 0.0044(7) C24 0.0227(13) 0.0493(19) 0.066(2) -0.0194(16) 0.0227(14) -0.0093(12) C25 0.063(2) 0.0251(14) 0.071(2) 0.0203(15) 0.0509(19) 0.0214(14) C26 0.0146(9) 0.0261(11) 0.0191(9) 0.0044(8) 0.0067(7) 0.0033(8) C27 0.0205(11) 0.0273(12) 0.0307(12) 0.0028(10) 0.0056(9) 0.0049(9) C28 0.0184(11) 0.0287(13) 0.0394(14) -0.0039(11) 0.0063(10) -0.0016(9) C29 0.0184(10) 0.0222(10) 0.0272(11) 0.0098(9) 0.0094(8) 0.0045(8) C30 0.0256(13) 0.0464(17) 0.0376(15) 0.0036(13) 0.0055(11) -0.0093(12) C31 0.0296(14) 0.0382(16) 0.060(2) -0.0024(14) 0.0279(14) 0.0050(12) C32 0.0163(9) 0.0229(10) 0.0218(10) 0.0083(8) 0.0087(8) 0.0054(8) C33 0.0209(12) 0.0441(16) 0.0319(13) 0.0044(12) -0.0002(10) 0.0032(11) C34 0.0317(13) 0.0427(15) 0.0249(12) 0.0044(11) 0.0106(10) 0.0158(12) C101 0.0280(11) 0.0250(11) 0.0261(11) 0.0031(9) 0.0112(9) -0.0026(9) C102 0.0301(12) 0.0288(12) 0.0236(11) 0.0092(9) 0.0086(9) -0.0015(9) C103 0.0327(12) 0.0295(12) 0.0227(11) 0.0018(9) 0.0113(9) -0.0054(10) C104 0.0306(12) 0.0257(12) 0.0304(12) 0.0044(10) 0.0150(10) 0.0009(9) C105 0.0250(11) 0.0382(14) 0.0280(12) 0.0112(10) 0.0095(9) 0.0010(10) C106 0.0271(12) 0.0360(13) 0.0205(11) 0.0024(10) 0.0077(9) -0.0037(10) C107 0.0491(18) 0.0327(16) 0.0435(17) -0.0033(13) 0.0089(15) 0.0072(13) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C1 2.173(2) . ? Sn1 Sn1 2.6461(3) 2_666 ? C1 C6 1.405(3) . ? C1 C2 1.406(3) . ? C2 C3 1.390(3) . ? C2 C7 1.499(3) . ? C3 C4 1.403(3) . ? C3 H3 0.88(3) . ? C4 C5 1.400(3) . ? C4 C19 1.532(3) . ? C5 C6 1.398(3) . ? C5 H5 0.93(3) . ? C6 C13 1.500(3) . ? C7 C8 1.408(3) . ? C7 C12 1.415(3) . ? C8 C9 1.395(3) . ? C8 C23 1.524(3) . ? C9 C10 1.389(3) . ? C9 H9 0.85(3) . ? C10 C11 1.388(3) . ? C10 H10 0.97(3) . ? C11 C12 1.396(3) . ? C11 H11 0.90(3) . ? C12 C26 1.522(3) . ? C13 C14 1.408(3) . ? C13 C18 1.415(3) . ? C14 C15 1.398(3) . ? C14 C32 1.525(3) . ? C15 C16 1.393(3) . ? C15 H15 0.91(3) . ? C16 C17 1.386(3) . ? C16 H16 1.00(3) . ? C17 C18 1.401(3) . ? C17 H17 0.98(3) . ? C18 C29 1.520(3) . ? C19 C22 1.531(3) . ? C19 C20 1.533(3) . ? C19 C21 1.541(3) . ? C20 H20A 0.94(3) . ? C20 H20B 1.02(3) . ? C20 H20C 0.94(4) . ? C21 H21A 0.94(3) . ? C21 H21B 0.92(3) . ? C21 H21C 0.98(3) . ? C22 H22A 0.95(3) . ? C22 H22B 0.91(3) . ? C22 H22C 0.96(4) . ? C23 C25 1.515(3) . ? C23 C24 1.525(4) . ? C23 H23 0.90(3) . ? C24 H24C 0.91(4) . ? C24 H24B 1.08(5) . ? C24 H24A 1.05(5) . ? C25 H25A 0.91(4) . ? C25 H25B 0.90(5) . ? C25 H25C 1.01(4) . ? C26 C28 1.529(3) . ? C26 C27 1.531(3) . ? C26 H26 0.97(3) . ? C27 H27A 0.93(3) . ? C27 H27B 0.98(4) . ? C27 H27C 1.03(3) . ? C28 H28C 1.01(3) . ? C28 H28B 0.95(4) . ? C28 H28A 0.92(4) . ? C29 C30 1.530(4) . ? C29 C31 1.533(4) . ? C29 H29 0.88(3) . ? C30 H30A 0.96(4) . ? C30 H30B 0.88(4) . ? C30 H30C 1.02(5) . ? C31 H31A 0.98(4) . ? C31 H31B 0.89(4) . ? C31 H31C 1.04(5) . ? C32 C33 1.525(3) . ? C32 C34 1.531(3) . ? C32 H32 0.95(3) . ? C33 H33C 0.94(3) . ? C33 H33B 0.97(3) . ? C33 H33A 0.95(4) . ? C34 H34A 1.05(3) . ? C34 H34B 0.88(4) . ? C34 H34C 1.02(4) . ? C101 C102 1.392(3) . ? C101 C106 1.393(4) . ? C101 C107 1.512(4) . ? C102 C103 1.387(4) . ? C102 H102 1.01(4) . ? C103 C104 1.382(4) . ? C103 H103 0.88(4) . ? C104 C105 1.394(4) . ? C104 H104 0.95(3) . ? C105 C106 1.379(4) . ? C105 H105 0.98(3) . ? C106 H106 0.87(3) . ? C107 H17C 0.94(5) . ? C107 H17B 0.79(6) . ? C107 H17A 0.88(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Sn1 Sn1 123.98(5) . 2_666 ? C6 C1 C2 118.49(18) . . ? C6 C1 Sn1 116.81(14) . . ? C2 C1 Sn1 124.60(14) . . ? C3 C2 C1 120.01(18) . . ? C3 C2 C7 120.74(18) . . ? C1 C2 C7 119.18(17) . . ? C2 C3 C4 122.26(18) . . ? C2 C3 H3 116.8(17) . . ? C4 C3 H3 120.9(17) . . ? C5 C4 C3 117.23(18) . . ? C5 C4 C19 122.78(18) . . ? C3 C4 C19 119.95(18) . . ? C6 C5 C4 121.45(18) . . ? C6 C5 H5 119.4(17) . . ? C4 C5 H5 119.1(17) . . ? C5 C6 C1 120.52(18) . . ? C5 C6 C13 119.72(17) . . ? C1 C6 C13 119.70(17) . . ? C8 C7 C12 120.82(18) . . ? C8 C7 C2 120.27(17) . . ? C12 C7 C2 118.88(17) . . ? C9 C8 C7 118.57(19) . . ? C9 C8 C23 120.13(18) . . ? C7 C8 C23 121.29(18) . . ? C10 C9 C8 121.3(2) . . ? C10 C9 H9 118.4(18) . . ? C8 C9 H9 120.2(18) . . ? C11 C10 C9 119.61(19) . . ? C11 C10 H10 117.8(17) . . ? C9 C10 H10 122.6(17) . . ? C10 C11 C12 121.3(2) . . ? C10 C11 H11 118.0(17) . . ? C12 C11 H11 120.6(17) . . ? C11 C12 C7 118.36(18) . . ? C11 C12 C26 120.36(18) . . ? C7 C12 C26 121.27(17) . . ? C14 C13 C18 120.55(18) . . ? C14 C13 C6 120.37(17) . . ? C18 C13 C6 119.08(18) . . ? C15 C14 C13 118.98(19) . . ? C15 C14 C32 119.07(19) . . ? C13 C14 C32 121.94(18) . . ? C16 C15 C14 120.8(2) . . ? C16 C15 H15 113(2) . . ? C14 C15 H15 126(2) . . ? C17 C16 C15 120.0(2) . . ? C17 C16 H16 117.3(19) . . ? C15 C16 H16 122.7(19) . . ? C16 C17 C18 121.1(2) . . ? C16 C17 H17 119.8(17) . . ? C18 C17 H17 119.2(17) . . ? C17 C18 C13 118.61(19) . . ? C17 C18 C29 119.83(19) . . ? C13 C18 C29 121.55(19) . . ? C22 C19 C4 109.10(18) . . ? C22 C19 C20 108.26(19) . . ? C4 C19 C20 112.06(17) . . ? C22 C19 C21 109.2(2) . . ? C4 C19 C21 109.85(18) . . ? C20 C19 C21 108.32(19) . . ? C19 C20 H20A 114.8(19) . . ? C19 C20 H20B 104.8(17) . . ? H20A C20 H20B 114(3) . . ? C19 C20 H20C 108(2) . . ? H20A C20 H20C 105(3) . . ? H20B C20 H20C 111(3) . . ? C19 C21 H21A 109.0(18) . . ? C19 C21 H21B 114.9(18) . . ? H21A C21 H21B 107(3) . . ? C19 C21 H21C 110.7(19) . . ? H21A C21 H21C 107(3) . . ? H21B C21 H21C 108(3) . . ? C19 C22 H22A 110(2) . . ? C19 C22 H22B 112(2) . . ? H22A C22 H22B 109(3) . . ? C19 C22 H22C 111(2) . . ? H22A C22 H22C 109(3) . . ? H22B C22 H22C 105(3) . . ? C25 C23 C8 110.52(19) . . ? C25 C23 C24 110.1(3) . . ? C8 C23 C24 112.50(19) . . ? C25 C23 H23 106.0(19) . . ? C8 C23 H23 109.1(19) . . ? C24 C23 H23 108(2) . . ? C23 C24 H24C 114(2) . . ? C23 C24 H24B 104(3) . . ? H24C C24 H24B 102(4) . . ? C23 C24 H24A 112(3) . . ? H24C C24 H24A 106(3) . . ? H24B C24 H24A 120(4) . . ? C23 C25 H25A 107(3) . . ? C23 C25 H25B 118(3) . . ? H25A C25 H25B 109(4) . . ? C23 C25 H25C 115(2) . . ? H25A C25 H25C 109(3) . . ? H25B C25 H25C 99(4) . . ? C12 C26 C28 110.60(19) . . ? C12 C26 C27 112.78(18) . . ? C28 C26 C27 110.56(19) . . ? C12 C26 H26 108.2(15) . . ? C28 C26 H26 109.4(16) . . ? C27 C26 H26 105.0(15) . . ? C26 C27 H27A 109.9(19) . . ? C26 C27 H27B 113(2) . . ? H27A C27 H27B 110(3) . . ? C26 C27 H27C 112.0(18) . . ? H27A C27 H27C 108(3) . . ? H27B C27 H27C 104(3) . . ? C26 C28 H28C 111.0(17) . . ? C26 C28 H28B 115(2) . . ? H28C C28 H28B 103(3) . . ? C26 C28 H28A 110(2) . . ? H28C C28 H28A 114(3) . . ? H28B C28 H28A 103(3) . . ? C18 C29 C30 110.9(2) . . ? C18 C29 C31 111.3(2) . . ? C30 C29 C31 111.2(2) . . ? C18 C29 H29 108.6(18) . . ? C30 C29 H29 113.5(19) . . ? C31 C29 H29 100.9(19) . . ? C29 C30 H30A 112(2) . . ? C29 C30 H30B 117(3) . . ? H30A C30 H30B 111(4) . . ? C29 C30 H30C 113(3) . . ? H30A C30 H30C 105(3) . . ? H30B C30 H30C 98(4) . . ? C29 C31 H31A 108(2) . . ? C29 C31 H31B 113(3) . . ? H31A C31 H31B 110(3) . . ? C29 C31 H31C 111(2) . . ? H31A C31 H31C 114(3) . . ? H31B C31 H31C 100(3) . . ? C14 C32 C33 111.6(2) . . ? C14 C32 C34 110.84(18) . . ? C33 C32 C34 109.9(2) . . ? C14 C32 H32 107.7(15) . . ? C33 C32 H32 107.9(16) . . ? C34 C32 H32 108.7(16) . . ? C32 C33 H33C 110(2) . . ? C32 C33 H33B 111(2) . . ? H33C C33 H33B 109(3) . . ? C32 C33 H33A 110(2) . . ? H33C C33 H33A 109(3) . . ? H33B C33 H33A 108(3) . . ? C32 C34 H34A 111.0(16) . . ? C32 C34 H34B 113(3) . . ? H34A C34 H34B 112(3) . . ? C32 C34 H34C 113(2) . . ? H34A C34 H34C 103(3) . . ? H34B C34 H34C 104(3) . . ? C102 C101 C106 117.6(2) . . ? C102 C101 C107 120.8(3) . . ? C106 C101 C107 121.6(2) . . ? C103 C102 C101 121.6(2) . . ? C103 C102 H102 119(3) . . ? C101 C102 H102 119(3) . . ? C104 C103 C102 119.7(2) . . ? C104 C103 H103 121(3) . . ? C102 C103 H103 119(3) . . ? C103 C104 C105 119.8(2) . . ? C103 C104 H104 122.4(19) . . ? C105 C104 H104 117.9(19) . . ? C106 C105 C104 119.7(2) . . ? C106 C105 H105 121.8(19) . . ? C104 C105 H105 118.4(19) . . ? C105 C106 C101 121.6(2) . . ? C105 C106 H106 119.5(18) . . ? C101 C106 H106 118.8(18) . . ? C101 C107 H17C 118(3) . . ? C101 C107 H17B 114(4) . . ? H17C C107 H17B 97(5) . . ? C101 C107 H17A 113(3) . . ? H17C C107 H17A 110(4) . . ? H17B C107 H17A 102(5) . . ? _diffrn_measured_fraction_theta_max 0.989 _diffrn_reflns_theta_full 29.57 _diffrn_measured_fraction_theta_full 0.989 _refine_diff_density_max 0.629 _refine_diff_density_min -0.711 _refine_diff_density_rms 0.081 # Attachment '-CGe-2.cif.txt' data_py25fmi _database_code_depnum_ccdc_archive 'CCDC 771273' #TrackingRef '-CGe-2.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '2(C84 H122 Ge2), 5(C7 H8)' _chemical_formula_sum 'C203 H284 Ge4' _chemical_formula_weight 3014.76 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c _symmetry_Space_group_name_Hall '-p 2ybc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 15.153(4) _cell_length_b 22.600(6) _cell_length_c 26.212(7) _cell_angle_alpha 90.00 _cell_angle_beta 100.842(4) _cell_angle_gamma 90.00 _cell_volume 8816(4) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9302 _cell_measurement_theta_min 2.26 _cell_measurement_theta_max 23.25 _exptl_crystal_description plate _exptl_crystal_colour red _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.18 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.136 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 3260 _exptl_absorpt_coefficient_mu 0.727 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker APEX-II CCD' _diffrn_measurement_method '\f and \w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 15965 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0952 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 17 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.20 _diffrn_reflns_theta_max 25.25 _reflns_number_total 15965 _reflns_number_gt 8634 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker APEX2' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1499P)^2^+4.8191P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment Constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15963 _refine_ls_number_parameters 933 _refine_ls_number_restraints 51 _refine_ls_R_factor_all 0.1798 _refine_ls_R_factor_gt 0.0974 _refine_ls_wR_factor_ref 0.2985 _refine_ls_wR_factor_gt 0.2632 _refine_ls_goodness_of_fit_ref 1.151 _refine_ls_restrained_S_all 1.179 _refine_ls_shift/su_max 0.033 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge1 Ge 0.30580(7) 0.28026(5) 0.10485(4) 0.0588(4) Uani 0.8327(17) 1 d P A 1 Ge2 Ge 0.19548(7) 0.33959(5) 0.11703(4) 0.0690(4) Uani 0.8327(17) 1 d P A 1 Ge1A Ge 0.2424(5) 0.2549(3) 0.0957(3) 0.096(3) Uani 0.1673(17) 1 d P A 2 Ge2A Ge 0.2479(4) 0.3499(3) 0.1287(2) 0.0690(4) Uani 0.1673(17) 1 d P A 2 C1 C 0.3183(4) 0.2095(3) 0.0596(2) 0.0363(14) Uani 1 1 d . . . C2 C 0.3783(4) 0.1665(2) 0.0856(2) 0.0338(13) Uani 1 1 d . A . C3 C 0.4024(4) 0.1182(3) 0.0580(2) 0.0352(13) Uani 1 1 d . . . C4 C 0.3700(4) 0.1157(2) 0.0043(2) 0.0329(13) Uani 1 1 d . A . H4 H 0.3878 0.0835 -0.0148 0.040 Uiso 1 1 calc R . . C5 C 0.3129(4) 0.1584(3) -0.0223(2) 0.0325(13) Uani 1 1 d . . . C6 C 0.2833(3) 0.2055(2) 0.00553(19) 0.0310(12) Uani 1 1 d . A . C7 C 0.4620(4) 0.0686(3) 0.0838(2) 0.0391(14) Uani 1 1 d . A . H7 H 0.4775 0.0772 0.1218 0.047 Uiso 1 1 calc R . . C8 C 0.4113(5) 0.0094(3) 0.0769(2) 0.0523(18) Uani 1 1 d . . . H8A H 0.3567 0.0125 0.0916 0.078 Uiso 1 1 calc R A . H8B H 0.4499 -0.0219 0.0948 0.078 Uiso 1 1 calc R . . H8C H 0.3951 0.0000 0.0398 0.078 Uiso 1 1 calc R . . C9 C 0.5494(4) 0.0637(3) 0.0634(2) 0.0500(17) Uani 1 1 d . . . H9A H 0.5361 0.0537 0.0264 0.075 Uiso 1 1 calc R A . H9B H 0.5871 0.0327 0.0825 0.075 Uiso 1 1 calc R . . H9C H 0.5814 0.1016 0.0682 0.075 Uiso 1 1 calc R . . C10 C 0.2840(4) 0.1509(3) -0.0809(2) 0.0424(15) Uani 1 1 d . A . H10 H 0.2472 0.1862 -0.0945 0.051 Uiso 1 1 calc R . . C11 C 0.2253(4) 0.0957(3) -0.0943(3) 0.0559(18) Uani 1 1 d . . . H11A H 0.2604 0.0603 -0.0823 0.084 Uiso 1 1 calc R A . H11B H 0.2046 0.0936 -0.1320 0.084 Uiso 1 1 calc R . . H11C H 0.1732 0.0981 -0.0772 0.084 Uiso 1 1 calc R . . C12 C 0.3636(4) 0.1480(3) -0.1081(2) 0.0473(16) Uani 1 1 d . . . H12A H 0.4020 0.1827 -0.0986 0.071 Uiso 1 1 calc R A . H12B H 0.3422 0.1475 -0.1458 0.071 Uiso 1 1 calc R . . H12C H 0.3981 0.1120 -0.0975 0.071 Uiso 1 1 calc R . . C13 C 0.4145(4) 0.1741(2) 0.14299(19) 0.0345(13) Uani 1 1 d . . . C14 C 0.3700(4) 0.1471(3) 0.1794(2) 0.0366(14) Uani 1 1 d . A . C15 C 0.4049(4) 0.1556(3) 0.2321(2) 0.0349(13) Uani 1 1 d . . . H15 H 0.3739 0.1389 0.2569 0.042 Uiso 1 1 calc R A . C16 C 0.4825(4) 0.1871(2) 0.2496(2) 0.0333(13) Uani 1 1 d . A . C17 C 0.5273(4) 0.2119(2) 0.2128(2) 0.0326(13) Uani 1 1 d . . . H17 H 0.5814 0.2333 0.2242 0.039 Uiso 1 1 calc R A . C18 C 0.4943(4) 0.2058(2) 0.1595(2) 0.0334(13) Uani 1 1 d . A . C19 C 0.2883(4) 0.1083(3) 0.1629(2) 0.0432(15) Uani 1 1 d . . . H19 H 0.2790 0.1035 0.1243 0.052 Uiso 1 1 calc R A . C20 C 0.3028(5) 0.0465(3) 0.1873(3) 0.0586(19) Uani 1 1 d . A . H20A H 0.3593 0.0299 0.1805 0.088 Uiso 1 1 calc R . . H20B H 0.2529 0.0206 0.1721 0.088 Uiso 1 1 calc R . . H20C H 0.3057 0.0494 0.2249 0.088 Uiso 1 1 calc R . . C21 C 0.2025(4) 0.1359(4) 0.1759(3) 0.072(2) Uani 1 1 d . A . H21A H 0.2072 0.1372 0.2137 0.107 Uiso 1 1 calc R . . H21B H 0.1504 0.1118 0.1606 0.107 Uiso 1 1 calc R . . H21C H 0.1951 0.1761 0.1619 0.107 Uiso 1 1 calc R . . C22 C 0.5182(4) 0.1928(3) 0.3082(2) 0.0357(13) Uani 1 1 d . . . H22 H 0.4683 0.2090 0.3241 0.043 Uiso 1 1 calc R A . C23 C 0.5410(4) 0.1318(3) 0.3317(2) 0.0432(15) Uani 1 1 d . A . H23A H 0.4868 0.1071 0.3260 0.065 Uiso 1 1 calc R . . H23B H 0.5640 0.1357 0.3690 0.065 Uiso 1 1 calc R . . H23C H 0.5868 0.1132 0.3151 0.065 Uiso 1 1 calc R . . C24 C 0.5976(4) 0.2336(3) 0.3232(2) 0.0476(16) Uani 1 1 d . A . H24A H 0.6495 0.2173 0.3105 0.071 Uiso 1 1 calc R . . H24B H 0.6122 0.2374 0.3611 0.071 Uiso 1 1 calc R . . H24C H 0.5828 0.2726 0.3076 0.071 Uiso 1 1 calc R . . C25 C 0.5478(4) 0.2327(3) 0.1219(2) 0.0403(14) Uani 1 1 d . . . H25 H 0.5181 0.2208 0.0861 0.048 Uiso 1 1 calc R A . C26 C 0.5496(5) 0.3017(3) 0.1240(3) 0.0583(19) Uani 1 1 d . A . H26A H 0.4879 0.3169 0.1160 0.087 Uiso 1 1 calc R . . H26B H 0.5835 0.3169 0.0985 0.087 Uiso 1 1 calc R . . H26C H 0.5783 0.3147 0.1589 0.087 Uiso 1 1 calc R . . C27 C 0.6442(4) 0.2105(3) 0.1305(3) 0.0519(17) Uani 1 1 d . A . H27A H 0.6769 0.2249 0.1641 0.078 Uiso 1 1 calc R . . H27B H 0.6734 0.2252 0.1027 0.078 Uiso 1 1 calc R . . H27C H 0.6445 0.1672 0.1304 0.078 Uiso 1 1 calc R . . C28 C 0.2169(3) 0.2504(3) -0.0211(2) 0.0320(12) Uani 1 1 d . . . C29 C 0.2466(3) 0.3042(2) -0.0394(2) 0.0308(12) Uani 1 1 d . A . C30 C 0.1829(3) 0.3450(2) -0.0628(2) 0.0312(12) Uani 1 1 d . . . H30 H 0.2032 0.3811 -0.0752 0.037 Uiso 1 1 calc R A . C31 C 0.0910(3) 0.3353(2) -0.0688(2) 0.0298(12) Uani 1 1 d . A . C32 C 0.0635(3) 0.2821(2) -0.0503(2) 0.0312(12) Uani 1 1 d . . . H32 H 0.0011 0.2749 -0.0529 0.037 Uiso 1 1 calc R A . C33 C 0.1248(4) 0.2385(2) -0.0280(2) 0.0327(13) Uani 1 1 d . A . C34 C 0.3456(4) 0.3174(3) -0.0368(2) 0.0373(14) Uani 1 1 d . . . H34 H 0.3811 0.2845 -0.0173 0.045 Uiso 1 1 calc R A . C35 C 0.3759(4) 0.3755(3) -0.0089(3) 0.0532(17) Uani 1 1 d . A . H35A H 0.3401 0.4083 -0.0265 0.080 Uiso 1 1 calc R . . H35B H 0.4396 0.3823 -0.0096 0.080 Uiso 1 1 calc R . . H35C H 0.3675 0.3732 0.0272 0.080 Uiso 1 1 calc R . . C36 C 0.3665(4) 0.3187(3) -0.0915(2) 0.0489(16) Uani 1 1 d . A . H36A H 0.3349 0.3520 -0.1108 0.073 Uiso 1 1 calc R . . H36B H 0.3466 0.2816 -0.1094 0.073 Uiso 1 1 calc R . . H36C H 0.4314 0.3234 -0.0895 0.073 Uiso 1 1 calc R . . C37 C 0.0220(4) 0.3795(2) -0.0961(2) 0.0341(13) Uani 1 1 d . . . H37 H -0.0387 0.3659 -0.0913 0.041 Uiso 1 1 calc R A . C38 C 0.0363(4) 0.4418(2) -0.0740(2) 0.0431(15) Uani 1 1 d . A . H38A H 0.0959 0.4560 -0.0777 0.065 Uiso 1 1 calc R . . H38B H 0.0321 0.4413 -0.0371 0.065 Uiso 1 1 calc R . . H38C H -0.0098 0.4682 -0.0929 0.065 Uiso 1 1 calc R . . C39 C 0.0220(5) 0.3807(3) -0.1542(2) 0.0545(18) Uani 1 1 d . A . H39A H -0.0245 0.4081 -0.1713 0.082 Uiso 1 1 calc R . . H39B H 0.0097 0.3410 -0.1686 0.082 Uiso 1 1 calc R . . H39C H 0.0809 0.3940 -0.1600 0.082 Uiso 1 1 calc R . . C40 C 0.0880(4) 0.1817(3) -0.0097(2) 0.0447(16) Uani 1 1 d . . . H40 H 0.1383 0.1524 -0.0049 0.054 Uiso 1 1 calc R A . C41 C 0.0131(4) 0.1558(3) -0.0503(4) 0.077(3) Uani 1 1 d . A . H41A H -0.0398 0.1815 -0.0540 0.115 Uiso 1 1 calc R . . H41B H -0.0023 0.1163 -0.0393 0.115 Uiso 1 1 calc R . . H41C H 0.0331 0.1530 -0.0836 0.115 Uiso 1 1 calc R . . C42 C 0.0600(6) 0.1883(4) 0.0431(3) 0.083(3) Uani 1 1 d . A . H42A H 0.1107 0.2038 0.0684 0.125 Uiso 1 1 calc R . . H42B H 0.0422 0.1497 0.0547 0.125 Uiso 1 1 calc R . . H42C H 0.0093 0.2158 0.0400 0.125 Uiso 1 1 calc R . . C43 C 0.1826(3) 0.3984(2) 0.17159(19) 0.0270(11) Uani 1 1 d . . . C44 C 0.2384(3) 0.4482(2) 0.18628(19) 0.0292(12) Uani 1 1 d . A . C45 C 0.2138(3) 0.4896(2) 0.22116(19) 0.0249(11) Uani 1 1 d . . . C46 C 0.1316(3) 0.4828(2) 0.23753(19) 0.0266(11) Uani 1 1 d . A . H46 H 0.1140 0.5122 0.2596 0.032 Uiso 1 1 calc R . . C47 C 0.0740(3) 0.4347(2) 0.22290(19) 0.0260(11) Uani 1 1 d . . . C48 C 0.1024(3) 0.3914(2) 0.19080(19) 0.0275(12) Uani 1 1 d . A . C49 C 0.2741(3) 0.5410(2) 0.2431(2) 0.0312(12) Uani 1 1 d . A . H49 H 0.3306 0.5383 0.2288 0.037 Uiso 1 1 calc R . . C50 C 0.2306(4) 0.6010(3) 0.2270(3) 0.0449(15) Uani 1 1 d . . . H50A H 0.2120 0.6023 0.1891 0.067 Uiso 1 1 calc R A . H50B H 0.2740 0.6327 0.2383 0.067 Uiso 1 1 calc R . . H50C H 0.1779 0.6064 0.2432 0.067 Uiso 1 1 calc R . . C51 C 0.2997(4) 0.5373(3) 0.3025(2) 0.0405(14) Uani 1 1 d . . . H51A H 0.2468 0.5461 0.3178 0.061 Uiso 1 1 calc R A . H51B H 0.3472 0.5661 0.3151 0.061 Uiso 1 1 calc R . . H51C H 0.3213 0.4974 0.3127 0.061 Uiso 1 1 calc R . . C52 C -0.0142(3) 0.4308(2) 0.2422(2) 0.0300(12) Uani 1 1 d . A . H52 H -0.0450 0.3934 0.2283 0.036 Uiso 1 1 calc R . . C53 C -0.0761(4) 0.4832(3) 0.2214(2) 0.0423(15) Uani 1 1 d . . . H53A H -0.0478 0.5204 0.2350 0.063 Uiso 1 1 calc R A . H53B H -0.1339 0.4787 0.2326 0.063 Uiso 1 1 calc R . . H53C H -0.0860 0.4836 0.1834 0.063 Uiso 1 1 calc R . . C54 C -0.0011(4) 0.4288(3) 0.3011(2) 0.0514(17) Uani 1 1 d . . . H54A H 0.0373 0.3951 0.3141 0.077 Uiso 1 1 calc R A . H54B H -0.0595 0.4245 0.3115 0.077 Uiso 1 1 calc R . . H54C H 0.0276 0.4655 0.3156 0.077 Uiso 1 1 calc R . . C55 C 0.3227(3) 0.4571(2) 0.16490(19) 0.0281(12) Uani 1 1 d . . . C56 C 0.3209(4) 0.4875(3) 0.1183(2) 0.0336(13) Uani 1 1 d . A . C57 C 0.4004(4) 0.4974(3) 0.0997(2) 0.0389(14) Uani 1 1 d . . . H57 H 0.3973 0.5169 0.0673 0.047 Uiso 1 1 calc R A . C58 C 0.4823(4) 0.4798(3) 0.1266(2) 0.0407(15) Uani 1 1 d . A . C59 C 0.4848(4) 0.4491(3) 0.1734(2) 0.0385(14) Uani 1 1 d . . . H59 H 0.5411 0.4356 0.1921 0.046 Uiso 1 1 calc R A . C60 C 0.4065(4) 0.4375(2) 0.1938(2) 0.0336(13) Uani 1 1 d . A . C61 C 0.2331(4) 0.5135(3) 0.0874(2) 0.0372(14) Uani 1 1 d . . . H61 H 0.1853 0.5072 0.1084 0.045 Uiso 1 1 calc R A . C62 C 0.2408(4) 0.5796(3) 0.0792(3) 0.0576(19) Uani 1 1 d . A . H62A H 0.2609 0.5991 0.1128 0.086 Uiso 1 1 calc R . . H62B H 0.1821 0.5954 0.0628 0.086 Uiso 1 1 calc R . . H62C H 0.2845 0.5871 0.0567 0.086 Uiso 1 1 calc R . . C63 C 0.2029(5) 0.4820(4) 0.0352(3) 0.066(2) Uani 1 1 d . A . H63A H 0.2489 0.4868 0.0138 0.099 Uiso 1 1 calc R . . H63B H 0.1462 0.4992 0.0172 0.099 Uiso 1 1 calc R . . H63C H 0.1943 0.4398 0.0413 0.099 Uiso 1 1 calc R . . C64 C 0.5679(4) 0.4963(3) 0.1062(2) 0.0517(17) Uani 1 1 d . . . H64 H 0.5553 0.5365 0.0906 0.062 Uiso 1 1 calc R A . C65 C 0.5824(5) 0.4587(4) 0.0628(3) 0.074(2) Uani 1 1 d . A . H65A H 0.6352 0.4728 0.0498 0.111 Uiso 1 1 calc R . . H65B H 0.5294 0.4606 0.0349 0.111 Uiso 1 1 calc R . . H65C H 0.5922 0.4178 0.0748 0.111 Uiso 1 1 calc R . . C66 C 0.6491(4) 0.5043(3) 0.1472(2) 0.0517(17) Uani 1 1 d . A . H66A H 0.6655 0.4665 0.1646 0.078 Uiso 1 1 calc R . . H66B H 0.6364 0.5334 0.1726 0.078 Uiso 1 1 calc R . . H66C H 0.6989 0.5185 0.1314 0.078 Uiso 1 1 calc R . . C67 C 0.4132(4) 0.4075(2) 0.2456(2) 0.0349(13) Uani 1 1 d . . . H67 H 0.3530 0.4093 0.2558 0.042 Uiso 1 1 calc R A . C68 C 0.4818(4) 0.4392(3) 0.2879(2) 0.0469(16) Uani 1 1 d . A . H68A H 0.5419 0.4366 0.2792 0.070 Uiso 1 1 calc R . . H68B H 0.4822 0.4203 0.3216 0.070 Uiso 1 1 calc R . . H68C H 0.4648 0.4809 0.2897 0.070 Uiso 1 1 calc R . . C69 C 0.4399(5) 0.3429(3) 0.2434(3) 0.0568(19) Uani 1 1 d . A . H69A H 0.3954 0.3221 0.2177 0.085 Uiso 1 1 calc R . . H69B H 0.4426 0.3248 0.2776 0.085 Uiso 1 1 calc R . . H69C H 0.4991 0.3402 0.2335 0.085 Uiso 1 1 calc R . . C70 C 0.0498(4) 0.3341(2) 0.1802(2) 0.0288(12) Uani 1 1 d . . . C71 C -0.0193(4) 0.3269(2) 0.1359(2) 0.0329(13) Uani 1 1 d . A . C72 C -0.0623(4) 0.2728(3) 0.1282(2) 0.0436(15) Uani 1 1 d . . . H72 H -0.1081 0.2677 0.0983 0.052 Uiso 1 1 calc R A . C73 C -0.0411(4) 0.2254(3) 0.1623(2) 0.0459(16) Uani 1 1 d . A . C74 C 0.0262(4) 0.2340(2) 0.2059(2) 0.0394(14) Uani 1 1 d . . . H74 H 0.0417 0.2023 0.2297 0.047 Uiso 1 1 calc R A . C75 C 0.0713(4) 0.2874(2) 0.2156(2) 0.0324(13) Uani 1 1 d . A . C76 C -0.0491(4) 0.3773(2) 0.0990(2) 0.0368(14) Uani 1 1 d . . . H76 H -0.0108 0.4125 0.1111 0.044 Uiso 1 1 calc R A . C77 C -0.0372(5) 0.3624(3) 0.0437(2) 0.0468(16) Uani 1 1 d . A . H77A H 0.0261 0.3537 0.0437 0.070 Uiso 1 1 calc R . . H77B H -0.0564 0.3962 0.0208 0.070 Uiso 1 1 calc R . . H77C H -0.0738 0.3278 0.0312 0.070 Uiso 1 1 calc R . . C78 C -0.1474(4) 0.3938(3) 0.0993(2) 0.0421(15) Uani 1 1 d . A . H78A H -0.1862 0.3598 0.0876 0.063 Uiso 1 1 calc R . . H78B H -0.1650 0.4273 0.0759 0.063 Uiso 1 1 calc R . . H78C H -0.1538 0.4047 0.1346 0.063 Uiso 1 1 calc R . . C79 C -0.0979(6) 0.1673(3) 0.1552(3) 0.069(2) Uani 1 1 d . . . H79 H -0.1453 0.1737 0.1765 0.082 Uiso 1 1 calc R A . C80 C -0.1474(5) 0.1561(3) 0.1035(4) 0.078(3) Uani 1 1 d . A . H80A H -0.1052 0.1492 0.0800 0.117 Uiso 1 1 calc R . . H80B H -0.1852 0.1904 0.0914 0.117 Uiso 1 1 calc R . . H80C H -0.1854 0.1211 0.1040 0.117 Uiso 1 1 calc R . . C81 C -0.0448(4) 0.1142(3) 0.1801(3) 0.0547(18) Uani 1 1 d . A . H81A H -0.0813 0.0783 0.1727 0.082 Uiso 1 1 calc R . . H81B H -0.0290 0.1201 0.2178 0.082 Uiso 1 1 calc R . . H81C H 0.0102 0.1099 0.1659 0.082 Uiso 1 1 calc R . . C82 C 0.1400(4) 0.2942(3) 0.2665(2) 0.0407(15) Uani 1 1 d . . . H82 H 0.1539 0.3374 0.2708 0.049 Uiso 1 1 calc R A . C83 C 0.2273(6) 0.2633(4) 0.2648(4) 0.102(4) Uani 1 1 d . A . H83A H 0.2718 0.2741 0.2956 0.153 Uiso 1 1 calc R . . H83B H 0.2491 0.2752 0.2334 0.153 Uiso 1 1 calc R . . H83C H 0.2178 0.2204 0.2644 0.153 Uiso 1 1 calc R . . C84 C 0.0985(7) 0.2753(4) 0.3130(3) 0.093(3) Uani 1 1 d . A . H84A H 0.1001 0.2321 0.3160 0.140 Uiso 1 1 calc R . . H84B H 0.0360 0.2889 0.3079 0.140 Uiso 1 1 calc R . . H84C H 0.1328 0.2929 0.3449 0.140 Uiso 1 1 calc R . . C91 C 0.1829(6) 0.7073(3) 0.6853(2) 0.042(2) Uiso 0.597(8) 1 d PGDU B 1 C92 C 0.2188(5) 0.6650(3) 0.65664(19) 0.049(3) Uiso 0.597(8) 1 d PGDU B 1 H92 H 0.2140 0.6698 0.6202 0.058 Uiso 0.597(8) 1 calc PR B 1 C93 C 0.2618(5) 0.6155(3) 0.6812(2) 0.048(3) Uiso 0.597(8) 1 d PGU B 1 H93 H 0.2863 0.5865 0.6616 0.058 Uiso 0.597(8) 1 calc PR B 1 C94 C 0.2688(5) 0.6083(3) 0.7345(3) 0.051(3) Uiso 0.597(8) 1 d PGU B 1 H94 H 0.2982 0.5745 0.7513 0.062 Uiso 0.597(8) 1 calc PR B 1 C95 C 0.2329(5) 0.6507(3) 0.76320(19) 0.048(2) Uiso 0.597(8) 1 d PGU B 1 H95 H 0.2377 0.6458 0.7996 0.058 Uiso 0.597(8) 1 calc PR B 1 C96 C 0.1899(6) 0.7002(3) 0.7386(2) 0.061(3) Uiso 0.597(8) 1 d PGDU B 1 H96 H 0.1654 0.7291 0.7582 0.074 Uiso 0.597(8) 1 calc PR B 1 C97 C 0.1371(10) 0.7588(5) 0.6568(4) 0.081(4) Uiso 0.597(8) 1 d PDU B 1 H97A H 0.1819 0.7883 0.6516 0.121 Uiso 0.597(8) 1 calc PR B 1 H97B H 0.0954 0.7763 0.6769 0.121 Uiso 0.597(8) 1 calc PR B 1 H97C H 0.1037 0.7457 0.6229 0.121 Uiso 0.597(8) 1 calc PR B 1 C91A C 0.1870(9) 0.7099(5) 0.6943(3) 0.050(4) Uiso 0.403(8) 1 d PGDU B 2 C92A C 0.2367(8) 0.6597(5) 0.6876(3) 0.051(3) Uiso 0.403(8) 1 d PGDU B 2 H92A H 0.2493 0.6506 0.6543 0.061 Uiso 0.403(8) 1 calc PR B 2 C93A C 0.2679(8) 0.6228(4) 0.7296(4) 0.058(4) Uiso 0.403(8) 1 d PGU B 2 H93A H 0.3018 0.5886 0.7250 0.069 Uiso 0.403(8) 1 calc PR B 2 C94A C 0.2494(8) 0.6361(4) 0.7783(3) 0.044(3) Uiso 0.403(8) 1 d PGU B 2 H94A H 0.2707 0.6109 0.8070 0.053 Uiso 0.403(8) 1 calc PR B 2 C95A C 0.1998(8) 0.6863(4) 0.7850(3) 0.054(4) Uiso 0.403(8) 1 d PGU B 2 H95A H 0.1871 0.6954 0.8183 0.065 Uiso 0.403(8) 1 calc PR B 2 C96A C 0.1686(9) 0.7232(4) 0.7430(3) 0.063(4) Uiso 0.403(8) 1 d PGDU B 2 H96A H 0.1346 0.7574 0.7476 0.076 Uiso 0.403(8) 1 calc PR B 2 C97A C 0.1698(19) 0.7505(9) 0.6472(8) 0.109(8) Uiso 0.403(8) 1 d PDU B 2 H97D H 0.2261 0.7697 0.6433 0.164 Uiso 0.403(8) 1 calc PR B 2 H97E H 0.1256 0.7807 0.6520 0.164 Uiso 0.403(8) 1 calc PR B 2 H97F H 0.1465 0.7272 0.6160 0.164 Uiso 0.403(8) 1 calc PR B 2 C101 C 0.2969(5) 0.8212(3) 0.0238(3) 0.0564(18) Uani 1 1 d . . . C102 C 0.2469(5) 0.7700(3) 0.0168(3) 0.0583(19) Uani 1 1 d . . . H102 H 0.1839 0.7722 0.0157 0.070 Uiso 1 1 calc R . . C103 C 0.2848(6) 0.7162(3) 0.0115(3) 0.067(2) Uani 1 1 d . . . H103 H 0.2497 0.6811 0.0069 0.080 Uiso 1 1 calc R . . C104 C 0.3792(7) 0.7150(4) 0.0132(3) 0.085(3) Uani 1 1 d . . . H104 H 0.4086 0.6788 0.0088 0.102 Uiso 1 1 calc R . . C105 C 0.4278(6) 0.7671(5) 0.0212(3) 0.074(2) Uani 1 1 d . . . H105 H 0.4912 0.7662 0.0240 0.089 Uiso 1 1 calc R . . C106 C 0.3875(5) 0.8175(4) 0.0251(3) 0.069(2) Uani 1 1 d . . . H106 H 0.4222 0.8528 0.0290 0.082 Uiso 1 1 calc R . . C107 C 0.2538(7) 0.8814(4) 0.0267(4) 0.097(3) Uani 1 1 d . . . H10A H 0.2798 0.9004 0.0597 0.145 Uiso 1 1 calc R . . H10B H 0.1889 0.8765 0.0246 0.145 Uiso 1 1 calc R . . H10C H 0.2647 0.9060 -0.0022 0.145 Uiso 1 1 calc R . . C111 C 1.0489(6) 1.0074(6) 0.0238(4) 0.065(4) Uiso 0.50 1 d PGD C -1 C112 C 1.0545(6) 0.9944(5) -0.0273(4) 0.066(5) Uiso 0.50 1 d PGD C -1 H112 H 1.1114 0.9937 -0.0376 0.079 Uiso 0.50 1 calc PR C -1 C113 C 0.9769(8) 0.9826(6) -0.0634(3) 0.083(5) Uiso 0.50 1 d PG C -1 H113 H 0.9808 0.9738 -0.0984 0.100 Uiso 0.50 1 calc PR C -1 C114 C 0.8937(6) 0.9837(7) -0.0485(5) 0.102(7) Uiso 0.50 1 d PG C -1 H114 H 0.8406 0.9757 -0.0731 0.123 Uiso 0.50 1 calc PR C -1 C115 C 0.8881(6) 0.9967(6) 0.0027(5) 0.093(6) Uiso 0.50 1 d PG C -1 H115 H 0.8312 0.9975 0.0129 0.111 Uiso 0.50 1 calc PR C -1 C116 C 0.9656(8) 1.0085(6) 0.0388(4) 0.092(7) Uiso 0.50 1 d PGD C -1 H116 H 0.9618 1.0173 0.0738 0.111 Uiso 0.50 1 calc PR C -1 C117 C 1.1303(10) 1.013(2) 0.0628(7) 0.24(2) Uiso 0.50 1 d PD C -1 H11D H 1.1481 0.9739 0.0775 0.359 Uiso 0.50 1 calc PR C -1 H11E H 1.1193 1.0395 0.0905 0.359 Uiso 0.50 1 calc PR C -1 H11F H 1.1785 1.0291 0.0468 0.359 Uiso 0.50 1 calc PR C -1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.0520(6) 0.0706(7) 0.0501(6) -0.0173(5) -0.0001(5) 0.0274(5) Ge2 0.0355(6) 0.0859(7) 0.0760(7) -0.0555(6) -0.0145(5) 0.0175(5) Ge1A 0.085(5) 0.078(4) 0.115(5) -0.077(4) -0.009(4) 0.024(3) Ge2A 0.0355(6) 0.0859(7) 0.0760(7) -0.0555(6) -0.0145(5) 0.0175(5) C1 0.040(3) 0.045(4) 0.026(3) 0.004(3) 0.009(2) 0.016(3) C2 0.038(3) 0.037(3) 0.026(3) 0.003(2) 0.006(2) 0.007(3) C3 0.039(3) 0.043(3) 0.022(3) -0.002(2) 0.003(2) 0.011(3) C4 0.034(3) 0.038(3) 0.025(3) 0.001(2) 0.003(2) 0.012(2) C5 0.031(3) 0.043(3) 0.022(3) 0.004(2) 0.002(2) 0.004(2) C6 0.030(3) 0.040(3) 0.023(3) 0.008(2) 0.004(2) 0.013(2) C7 0.051(4) 0.040(3) 0.023(3) 0.001(2) 0.000(3) 0.021(3) C8 0.077(5) 0.036(4) 0.040(4) 0.003(3) 0.003(3) 0.019(3) C9 0.053(4) 0.054(4) 0.037(4) -0.004(3) -0.006(3) 0.024(3) C10 0.038(3) 0.057(4) 0.028(3) -0.001(3) -0.004(3) 0.011(3) C11 0.048(4) 0.068(5) 0.042(4) -0.012(3) -0.016(3) 0.005(3) C12 0.057(4) 0.066(4) 0.019(3) 0.001(3) 0.006(3) 0.012(3) C13 0.046(3) 0.041(3) 0.018(3) 0.002(2) 0.009(2) 0.020(3) C14 0.033(3) 0.045(4) 0.032(3) -0.001(3) 0.005(2) 0.013(3) C15 0.037(3) 0.047(4) 0.023(3) 0.006(2) 0.010(2) 0.008(3) C16 0.041(3) 0.038(3) 0.019(3) 0.001(2) 0.002(2) 0.016(3) C17 0.042(3) 0.026(3) 0.029(3) 0.003(2) 0.005(2) 0.012(2) C18 0.042(3) 0.031(3) 0.026(3) 0.004(2) 0.005(2) 0.011(3) C19 0.040(3) 0.053(4) 0.037(3) -0.001(3) 0.007(3) 0.012(3) C20 0.067(5) 0.060(5) 0.045(4) 0.008(3) 0.001(3) -0.013(4) C21 0.038(4) 0.085(6) 0.093(6) -0.017(5) 0.015(4) -0.004(4) C22 0.041(3) 0.043(3) 0.023(3) 0.000(2) 0.005(2) 0.012(3) C23 0.051(4) 0.050(4) 0.028(3) 0.007(3) 0.006(3) 0.008(3) C24 0.060(4) 0.049(4) 0.029(3) 0.002(3) -0.004(3) 0.000(3) C25 0.057(4) 0.041(4) 0.025(3) 0.003(2) 0.013(3) 0.004(3) C26 0.089(5) 0.043(4) 0.048(4) 0.006(3) 0.026(4) 0.003(4) C27 0.057(4) 0.059(4) 0.043(4) 0.002(3) 0.020(3) 0.001(3) C28 0.028(3) 0.041(3) 0.026(3) 0.004(2) 0.003(2) 0.006(2) C29 0.028(3) 0.037(3) 0.026(3) 0.003(2) 0.000(2) 0.003(2) C30 0.033(3) 0.032(3) 0.028(3) 0.003(2) 0.002(2) -0.003(2) C31 0.032(3) 0.030(3) 0.025(3) -0.001(2) 0.000(2) 0.004(2) C32 0.024(3) 0.035(3) 0.034(3) 0.006(2) 0.002(2) 0.005(2) C33 0.033(3) 0.034(3) 0.031(3) 0.006(2) 0.005(2) 0.006(2) C34 0.030(3) 0.044(4) 0.036(3) 0.005(3) 0.001(2) 0.004(3) C35 0.035(3) 0.063(5) 0.059(4) -0.006(4) 0.000(3) -0.007(3) C36 0.043(4) 0.059(4) 0.045(4) 0.000(3) 0.009(3) 0.000(3) C37 0.032(3) 0.026(3) 0.041(3) 0.001(2) -0.001(3) 0.005(2) C38 0.045(4) 0.034(3) 0.047(4) 0.001(3) 0.001(3) 0.004(3) C39 0.070(5) 0.044(4) 0.040(4) 0.001(3) -0.013(3) 0.022(3) C40 0.039(3) 0.041(4) 0.057(4) 0.021(3) 0.019(3) 0.011(3) C41 0.035(4) 0.039(4) 0.146(8) 0.032(5) -0.008(4) -0.008(3) C42 0.110(7) 0.061(5) 0.099(7) 0.028(5) 0.071(6) 0.018(5) C43 0.032(3) 0.020(3) 0.027(3) 0.000(2) 0.001(2) 0.002(2) C44 0.030(3) 0.037(3) 0.019(3) 0.004(2) -0.001(2) 0.003(2) C45 0.028(3) 0.023(3) 0.022(3) -0.001(2) -0.001(2) 0.002(2) C46 0.027(3) 0.029(3) 0.023(3) -0.002(2) 0.003(2) 0.000(2) C47 0.030(3) 0.026(3) 0.021(3) 0.000(2) 0.001(2) 0.001(2) C48 0.034(3) 0.024(3) 0.022(3) 0.002(2) -0.002(2) -0.003(2) C49 0.027(3) 0.029(3) 0.037(3) -0.005(2) 0.005(2) -0.005(2) C50 0.046(4) 0.035(3) 0.053(4) 0.001(3) 0.008(3) -0.008(3) C51 0.038(3) 0.046(4) 0.036(3) -0.013(3) 0.005(3) -0.004(3) C52 0.029(3) 0.032(3) 0.028(3) -0.004(2) 0.001(2) -0.004(2) C53 0.035(3) 0.042(4) 0.050(4) -0.006(3) 0.008(3) 0.002(3) C54 0.044(4) 0.074(5) 0.036(4) 0.009(3) 0.009(3) -0.008(3) C55 0.028(3) 0.035(3) 0.021(3) -0.007(2) 0.005(2) -0.003(2) C56 0.030(3) 0.042(3) 0.027(3) -0.010(2) 0.000(2) -0.001(2) C57 0.030(3) 0.062(4) 0.023(3) -0.009(3) 0.002(2) -0.008(3) C58 0.031(3) 0.061(4) 0.030(3) -0.014(3) 0.006(3) -0.006(3) C59 0.024(3) 0.055(4) 0.035(3) -0.008(3) 0.003(2) 0.001(3) C60 0.030(3) 0.040(3) 0.029(3) -0.007(2) 0.001(2) 0.004(2) C61 0.032(3) 0.055(4) 0.022(3) 0.000(3) 0.001(2) 0.001(3) C62 0.043(4) 0.062(5) 0.059(4) 0.012(4) -0.011(3) 0.002(3) C63 0.054(4) 0.086(6) 0.047(4) -0.012(4) -0.015(3) 0.005(4) C64 0.036(3) 0.079(5) 0.041(4) -0.006(3) 0.010(3) -0.008(3) C65 0.065(5) 0.096(6) 0.071(5) -0.038(5) 0.037(4) -0.034(4) C66 0.037(3) 0.073(5) 0.044(4) 0.002(3) 0.004(3) -0.008(3) C67 0.031(3) 0.041(3) 0.029(3) -0.003(2) -0.003(2) 0.009(2) C68 0.036(3) 0.070(5) 0.033(3) -0.007(3) 0.001(3) 0.002(3) C69 0.072(5) 0.046(4) 0.047(4) -0.001(3) -0.004(4) 0.023(3) C70 0.038(3) 0.022(3) 0.025(3) -0.002(2) 0.000(2) -0.002(2) C71 0.038(3) 0.028(3) 0.029(3) 0.000(2) 0.000(2) -0.005(2) C72 0.054(4) 0.037(4) 0.031(3) -0.004(3) -0.013(3) -0.009(3) C73 0.061(4) 0.036(3) 0.033(3) -0.001(3) -0.012(3) -0.010(3) C74 0.055(4) 0.028(3) 0.031(3) 0.004(2) -0.005(3) -0.001(3) C75 0.038(3) 0.024(3) 0.029(3) -0.002(2) -0.007(2) -0.004(2) C76 0.050(4) 0.031(3) 0.024(3) 0.003(2) -0.007(3) -0.005(3) C77 0.060(4) 0.048(4) 0.031(3) 0.006(3) 0.006(3) 0.003(3) C78 0.051(4) 0.041(4) 0.031(3) 0.001(3) -0.002(3) 0.001(3) C79 0.103(6) 0.035(4) 0.053(4) 0.005(3) -0.021(4) -0.029(4) C80 0.061(5) 0.052(5) 0.114(7) 0.001(5) 0.000(5) -0.021(4) C81 0.044(4) 0.034(4) 0.084(5) 0.007(3) 0.007(4) -0.005(3) C82 0.054(4) 0.032(3) 0.028(3) 0.002(2) -0.013(3) -0.004(3) C83 0.092(7) 0.098(7) 0.087(6) -0.042(5) -0.058(5) 0.036(5) C84 0.129(8) 0.109(7) 0.027(4) 0.022(4) -0.020(4) -0.072(6) C101 0.061(5) 0.050(4) 0.059(5) 0.000(3) 0.012(4) -0.001(3) C102 0.041(4) 0.058(5) 0.075(5) 0.000(4) 0.010(4) -0.005(3) C103 0.085(6) 0.050(5) 0.050(4) -0.001(3) -0.026(4) -0.003(4) C104 0.123(8) 0.083(7) 0.037(4) -0.001(4) -0.016(5) 0.061(6) C105 0.056(5) 0.109(8) 0.058(5) 0.014(5) 0.014(4) 0.014(5) C106 0.046(4) 0.087(6) 0.070(5) 0.025(5) 0.004(4) -0.006(4) C107 0.100(7) 0.069(6) 0.125(9) -0.023(6) 0.029(6) 0.003(5) _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 C1 2.021(6) . ? Ge1 Ge2 2.2125(13) . ? Ge2 C43 1.989(5) . ? Ge1A C1 1.918(8) . ? Ge1A Ge2A 2.311(7) . ? Ge2A C43 1.966(7) . ? C1 C2 1.416(7) . ? C1 C6 1.420(7) . ? C2 C3 1.395(8) . ? C2 C13 1.510(7) . ? C3 C4 1.404(7) . ? C3 C7 1.516(7) . ? C4 C5 1.392(7) . ? C4 H4 0.9500 . ? C5 C6 1.410(7) . ? C5 C10 1.525(7) . ? C6 C28 1.506(7) . ? C7 C9 1.523(9) . ? C7 C8 1.534(9) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C12 1.513(8) . ? C10 C11 1.534(9) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C14 1.408(8) . ? C13 C18 1.403(8) . ? C14 C15 1.395(8) . ? C14 C19 1.512(8) . ? C15 C16 1.377(8) . ? C15 H15 0.9500 . ? C16 C17 1.397(8) . ? C16 C22 1.535(7) . ? C17 C18 1.398(7) . ? C17 H17 0.9500 . ? C18 C25 1.516(8) . ? C19 C20 1.536(9) . ? C19 C21 1.537(9) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.508(8) . ? C22 C23 1.522(8) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C27 1.520(9) . ? C25 C26 1.560(9) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C33 1.400(7) . ? C28 C29 1.411(8) . ? C29 C30 1.390(7) . ? C29 C34 1.519(7) . ? C30 C31 1.390(7) . ? C30 H30 0.9500 . ? C31 C32 1.389(7) . ? C31 C37 1.524(7) . ? C32 C33 1.404(7) . ? C32 H32 0.9500 . ? C33 C40 1.512(8) . ? C34 C36 1.525(8) . ? C34 C35 1.532(9) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C39 1.523(8) . ? C37 C38 1.523(8) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.518(10) . ? C40 C42 1.529(9) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C48 1.409(7) . ? C43 C44 1.416(7) . ? C44 C45 1.408(7) . ? C44 C55 1.503(7) . ? C45 C46 1.400(7) . ? C45 C49 1.522(7) . ? C46 C47 1.403(7) . ? C46 H46 0.9500 . ? C47 C48 1.409(7) . ? C47 C52 1.519(7) . ? C48 C70 1.518(7) . ? C49 C50 1.531(8) . ? C49 C51 1.535(8) . ? C49 H49 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C54 1.520(8) . ? C52 C53 1.544(8) . ? C52 H52 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.398(7) . ? C55 C60 1.422(7) . ? C56 C57 1.399(8) . ? C56 C61 1.538(7) . ? C57 C58 1.366(8) . ? C57 H57 0.9500 . ? C58 C59 1.405(8) . ? C58 C64 1.538(8) . ? C59 C60 1.414(8) . ? C59 H59 0.9500 . ? C60 C67 1.502(8) . ? C61 C62 1.518(9) . ? C61 C63 1.533(8) . ? C61 H61 1.0000 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C65 1.467(9) . ? C64 C66 1.485(8) . ? C64 H64 1.0000 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C67 C69 1.519(8) . ? C67 C68 1.546(8) . ? C67 H67 1.0000 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 C75 1.403(7) . ? C70 C71 1.418(7) . ? C71 C72 1.383(8) . ? C71 C76 1.508(7) . ? C72 C73 1.394(8) . ? C72 H72 0.9500 . ? C73 C74 1.395(8) . ? C73 C79 1.561(8) . ? C74 C75 1.385(7) . ? C74 H74 0.9500 . ? C75 C82 1.538(7) . ? C76 C77 1.532(8) . ? C76 C78 1.537(8) . ? C76 H76 1.0000 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 C80 1.441(10) . ? C79 C81 1.524(9) . ? C79 H79 1.0000 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C82 C83 1.504(10) . ? C82 C84 1.536(10) . ? C82 H82 1.0000 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? C91 C92 1.3900 . ? C91 C96 1.3900 . ? C91 C97 1.483(7) . ? C92 C93 1.3900 . ? C92 H92 0.9500 . ? C93 C94 1.3900 . ? C93 H93 0.9500 . ? C94 C95 1.3900 . ? C94 H94 0.9500 . ? C95 C96 1.3900 . ? C95 H95 0.9500 . ? C96 H96 0.9500 . ? C97 H97A 0.9800 . ? C97 H97B 0.9800 . ? C97 H97C 0.9800 . ? C91A C92A 1.3900 . ? C91A C96A 1.3900 . ? C91A C97A 1.522(9) . ? C92A C93A 1.3900 . ? C92A H92A 0.9500 . ? C93A C94A 1.3900 . ? C93A H93A 0.9500 . ? C94A C95A 1.3900 . ? C94A H94A 0.9500 . ? C95A C96A 1.3900 . ? C95A H95A 0.9500 . ? C96A H96A 0.9500 . ? C97A H97D 0.9800 . ? C97A H97E 0.9800 . ? C97A H97F 0.9800 . ? C101 C102 1.378(9) . ? C101 C106 1.369(10) . ? C101 C107 1.516(11) . ? C102 C103 1.361(10) . ? C102 H102 0.9500 . ? C103 C104 1.424(12) . ? C103 H103 0.9500 . ? C104 C105 1.384(12) . ? C104 H104 0.9500 . ? C105 C106 1.306(12) . ? C105 H105 0.9500 . ? C106 H106 0.9500 . ? C107 H10A 0.9800 . ? C107 H10B 0.9800 . ? C107 H10C 0.9800 . ? C111 C112 1.3900 . ? C111 C116 1.3900 . ? C111 C117 1.452(8) . ? C112 C113 1.3900 . ? C112 H112 0.9500 . ? C113 C114 1.3900 . ? C113 H113 0.9500 . ? C114 C115 1.3900 . ? C114 H114 0.9500 . ? C115 C116 1.3900 . ? C115 H115 0.9500 . ? C116 H116 0.9500 . ? C117 H11D 0.9800 . ? C117 H11E 0.9800 . ? C117 H11F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ge1 Ge2 136.13(17) . . ? C43 Ge2 Ge1 133.48(15) . . ? C1 Ge1A Ge2A 134.4(5) . . ? C43 Ge2A Ge1A 138.2(4) . . ? C2 C1 C6 121.5(5) . . ? C2 C1 Ge1A 121.4(5) . . ? C6 C1 Ge1A 112.4(4) . . ? C2 C1 Ge1 112.5(4) . . ? C6 C1 Ge1 125.3(4) . . ? C3 C2 C1 119.6(5) . . ? C3 C2 C13 121.6(5) . . ? C1 C2 C13 118.8(5) . . ? C2 C3 C4 118.4(5) . . ? C2 C3 C7 122.7(5) . . ? C4 C3 C7 118.9(5) . . ? C5 C4 C3 122.8(5) . . ? C5 C4 H4 118.6 . . ? C3 C4 H4 118.6 . . ? C4 C5 C6 119.5(5) . . ? C4 C5 C10 117.5(5) . . ? C6 C5 C10 123.1(5) . . ? C5 C6 C1 118.0(5) . . ? C5 C6 C28 121.2(5) . . ? C1 C6 C28 120.8(5) . . ? C3 C7 C9 112.4(5) . . ? C3 C7 C8 110.4(5) . . ? C9 C7 C8 110.2(5) . . ? C3 C7 H7 107.9 . . ? C9 C7 H7 107.9 . . ? C8 C7 H7 107.9 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C12 C10 C5 112.1(5) . . ? C12 C10 C11 109.7(5) . . ? C5 C10 C11 111.4(5) . . ? C12 C10 H10 107.8 . . ? C5 C10 H10 107.8 . . ? C11 C10 H10 107.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C14 C13 C18 120.4(5) . . ? C14 C13 C2 119.7(5) . . ? C18 C13 C2 119.8(5) . . ? C15 C14 C13 118.1(5) . . ? C15 C14 C19 120.1(5) . . ? C13 C14 C19 121.8(5) . . ? C16 C15 C14 122.8(5) . . ? C16 C15 H15 118.6 . . ? C14 C15 H15 118.6 . . ? C15 C16 C17 118.2(5) . . ? C15 C16 C22 119.7(5) . . ? C17 C16 C22 122.1(5) . . ? C16 C17 C18 121.4(5) . . ? C16 C17 H17 119.3 . . ? C18 C17 H17 119.3 . . ? C17 C18 C13 119.0(5) . . ? C17 C18 C25 118.3(5) . . ? C13 C18 C25 122.6(5) . . ? C14 C19 C20 111.2(5) . . ? C14 C19 C21 112.5(5) . . ? C20 C19 C21 109.7(6) . . ? C14 C19 H19 107.8 . . ? C20 C19 H19 107.8 . . ? C21 C19 H19 107.8 . . ? 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 . . ? C24 C22 C23 109.9(5) . . ? C24 C22 C16 115.2(5) . . ? C23 C22 C16 109.9(5) . . ? C24 C22 H22 107.2 . . ? C23 C22 H22 107.2 . . ? C16 C22 H22 107.2 . . ? 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 . . ? C18 C25 C27 112.8(5) . . ? C18 C25 C26 112.7(5) . . ? C27 C25 C26 108.4(5) . . ? C18 C25 H25 107.6 . . ? C27 C25 H25 107.6 . . ? C26 C25 H25 107.6 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C33 C28 C29 119.8(5) . . ? C33 C28 C6 119.5(5) . . ? C29 C28 C6 120.7(5) . . ? C30 C29 C28 118.8(5) . . ? C30 C29 C34 119.2(5) . . ? C28 C29 C34 121.9(5) . . ? C31 C30 C29 122.8(5) . . ? C31 C30 H30 118.6 . . ? C29 C30 H30 118.6 . . ? C32 C31 C30 117.2(5) . . ? C32 C31 C37 120.5(5) . . ? C30 C31 C37 122.2(5) . . ? C31 C32 C33 122.3(5) . . ? C31 C32 H32 118.8 . . ? C33 C32 H32 118.8 . . ? C32 C33 C28 118.9(5) . . ? C32 C33 C40 118.2(5) . . ? C28 C33 C40 122.8(5) . . ? C29 C34 C36 109.9(5) . . ? C29 C34 C35 113.2(5) . . ? C36 C34 C35 109.6(5) . . ? C29 C34 H34 108.0 . . ? C36 C34 H34 108.0 . . ? C35 C34 H34 108.0 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C39 C37 C31 110.7(5) . . ? C39 C37 C38 109.6(5) . . ? C31 C37 C38 113.1(4) . . ? C39 C37 H37 107.8 . . ? C31 C37 H37 107.8 . . ? C38 C37 H37 107.8 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C33 C40 C41 112.2(5) . . ? C33 C40 C42 112.6(6) . . ? C41 C40 C42 111.9(6) . . ? C33 C40 H40 106.6 . . ? C41 C40 H40 106.6 . . ? C42 C40 H40 106.6 . . ? 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 . . ? C48 C43 C44 120.2(5) . . ? C48 C43 Ge2A 134.6(4) . . ? C44 C43 Ge2A 105.0(4) . . ? C48 C43 Ge2 113.0(4) . . ? C44 C43 Ge2 126.3(4) . . ? C45 C44 C43 119.2(5) . . ? C45 C44 C55 120.0(5) . . ? C43 C44 C55 120.8(5) . . ? C46 C45 C44 119.0(5) . . ? C46 C45 C49 118.2(4) . . ? C44 C45 C49 122.7(5) . . ? C45 C46 C47 123.0(5) . . ? C45 C46 H46 118.5 . . ? C47 C46 H46 118.5 . . ? C46 C47 C48 117.3(5) . . ? C46 C47 C52 119.6(4) . . ? C48 C47 C52 123.1(4) . . ? C47 C48 C43 121.0(5) . . ? C47 C48 C70 119.5(5) . . ? C43 C48 C70 119.3(5) . . ? C45 C49 C50 112.0(4) . . ? C45 C49 C51 111.1(4) . . ? C50 C49 C51 110.0(5) . . ? C45 C49 H49 107.9 . . ? C50 C49 H49 107.9 . . ? C51 C49 H49 107.9 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C47 C52 C54 112.6(4) . . ? C47 C52 C53 110.7(4) . . ? C54 C52 C53 109.7(5) . . ? C47 C52 H52 107.9 . . ? C54 C52 H52 107.9 . . ? C53 C52 H52 107.9 . . ? 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 . . ? C56 C55 C60 119.2(5) . . ? C56 C55 C44 120.9(5) . . ? C60 C55 C44 119.7(5) . . ? C57 C56 C55 120.4(5) . . ? C57 C56 C61 118.2(5) . . ? C55 C56 C61 121.4(5) . . ? C58 C57 C56 122.1(5) . . ? C58 C57 H57 118.9 . . ? C56 C57 H57 118.9 . . ? C57 C58 C59 117.8(5) . . ? C57 C58 C64 119.6(6) . . ? C59 C58 C64 122.5(5) . . ? C60 C59 C58 122.4(5) . . ? C60 C59 H59 118.8 . . ? C58 C59 H59 118.8 . . ? C59 C60 C55 118.0(5) . . ? C59 C60 C67 120.4(5) . . ? C55 C60 C67 121.7(5) . . ? C62 C61 C63 110.4(5) . . ? C62 C61 C56 111.6(5) . . ? C63 C61 C56 112.1(5) . . ? C62 C61 H61 107.5 . . ? C63 C61 H61 107.5 . . ? C56 C61 H61 107.5 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C65 C64 C66 114.1(6) . . ? C65 C64 C58 112.8(6) . . ? C66 C64 C58 114.5(5) . . ? C65 C64 H64 104.7 . . ? C66 C64 H64 104.7 . . ? C58 C64 H64 104.7 . . ? C64 C65 H65A 109.5 . . ? C64 C65 H65B 109.5 . . ? H65A C65 H65B 109.5 . . ? C64 C65 H65C 109.5 . . ? H65A C65 H65C 109.5 . . ? H65B C65 H65C 109.5 . . ? C64 C66 H66A 109.5 . . ? C64 C66 H66B 109.5 . . ? H66A C66 H66B 109.5 . . ? C64 C66 H66C 109.5 . . ? H66A C66 H66C 109.5 . . ? H66B C66 H66C 109.5 . . ? C60 C67 C69 112.0(5) . . ? C60 C67 C68 111.2(5) . . ? C69 C67 C68 108.9(5) . . ? C60 C67 H67 108.2 . . ? C69 C67 H67 108.2 . . ? C68 C67 H67 108.2 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C67 C69 H69A 109.5 . . ? C67 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C67 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C75 C70 C71 119.9(5) . . ? C75 C70 C48 118.2(4) . . ? C71 C70 C48 122.0(4) . . ? C72 C71 C70 118.5(5) . . ? C72 C71 C76 119.9(5) . . ? C70 C71 C76 121.6(5) . . ? C71 C72 C73 122.7(5) . . ? C71 C72 H72 118.7 . . ? C73 C72 H72 118.7 . . ? C72 C73 C74 117.6(5) . . ? C72 C73 C79 120.9(5) . . ? C74 C73 C79 121.2(5) . . ? C75 C74 C73 122.1(5) . . ? C75 C74 H74 119.0 . . ? C73 C74 H74 119.0 . . ? C74 C75 C70 119.3(5) . . ? C74 C75 C82 118.5(5) . . ? C70 C75 C82 122.2(5) . . ? C71 C76 C77 111.5(5) . . ? C71 C76 C78 110.7(5) . . ? C77 C76 C78 110.1(5) . . ? C71 C76 H76 108.1 . . ? C77 C76 H76 108.1 . . ? C78 C76 H76 108.1 . . ? C76 C77 H77A 109.5 . . ? C76 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C76 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C76 C78 H78A 109.5 . . ? C76 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C76 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C80 C79 C81 113.8(6) . . ? C80 C79 C73 116.0(6) . . ? C81 C79 C73 112.1(6) . . ? C80 C79 H79 104.5 . . ? C81 C79 H79 104.5 . . ? C73 C79 H79 104.5 . . ? C79 C80 H80A 109.5 . . ? C79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C79 C81 H81A 109.5 . . ? C79 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C79 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C83 C82 C84 112.8(7) . . ? C83 C82 C75 112.6(5) . . ? C84 C82 C75 110.4(5) . . ? C83 C82 H82 106.9 . . ? C84 C82 H82 106.9 . . ? C75 C82 H82 106.9 . . ? C82 C83 H83A 109.5 . . ? C82 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C82 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C82 C84 H84A 109.5 . . ? C82 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C82 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C92 C91 C96 120.0 . . ? C92 C91 C97 117.4(4) . . ? C96 C91 C97 122.6(4) . . ? C91 C92 C93 120.0 . . ? C91 C92 H92 120.0 . . ? C93 C92 H92 120.0 . . ? C94 C93 C92 120.0 . . ? C94 C93 H93 120.0 . . ? C92 C93 H93 120.0 . . ? C93 C94 C95 120.0 . . ? C93 C94 H94 120.0 . . ? C95 C94 H94 120.0 . . ? C96 C95 C94 120.0 . . ? C96 C95 H95 120.0 . . ? C94 C95 H95 120.0 . . ? C95 C96 C91 120.0 . . ? C95 C96 H96 120.0 . . ? C91 C96 H96 120.0 . . ? C91 C97 H97A 109.5 . . ? C91 C97 H97B 109.5 . . ? H97A C97 H97B 109.5 . . ? C91 C97 H97C 109.5 . . ? H97A C97 H97C 109.5 . . ? H97B C97 H97C 109.5 . . ? C92A C91A C96A 120.0 . . ? C92A C91A C97A 113.8(8) . . ? C96A C91A C97A 125.6(8) . . ? C91A C92A C93A 120.0 . . ? C91A C92A H92A 120.0 . . ? C93A C92A H92A 120.0 . . ? C94A C93A C92A 120.0 . . ? C94A C93A H93A 120.0 . . ? C92A C93A H93A 120.0 . . ? C93A C94A C95A 120.0 . . ? C93A C94A H94A 120.0 . . ? C95A C94A H94A 120.0 . . ? C94A C95A C96A 120.0 . . ? C94A C95A H95A 120.0 . . ? C96A C95A H95A 120.0 . . ? C95A C96A C91A 120.0 . . ? C95A C96A H96A 120.0 . . ? C91A C96A H96A 120.0 . . ? C91A C97A H97D 109.5 . . ? C91A C97A H97E 109.5 . . ? H97D C97A H97E 109.5 . . ? C91A C97A H97F 109.5 . . ? H97D C97A H97F 109.5 . . ? H97E C97A H97F 109.5 . . ? C102 C101 C106 118.5(7) . . ? C102 C101 C107 121.9(7) . . ? C106 C101 C107 119.5(7) . . ? C103 C102 C101 122.1(7) . . ? C103 C102 H102 119.0 . . ? C101 C102 H102 119.0 . . ? C102 C103 C104 117.1(7) . . ? C102 C103 H103 121.5 . . ? C104 C103 H103 121.5 . . ? C105 C104 C103 119.4(7) . . ? C105 C104 H104 120.3 . . ? C103 C104 H104 120.3 . . ? C106 C105 C104 120.7(8) . . ? C106 C105 H105 119.6 . . ? C104 C105 H105 119.6 . . ? C105 C106 C101 122.2(8) . . ? C105 C106 H106 118.9 . . ? C101 C106 H106 118.9 . . ? C101 C107 H10A 109.5 . . ? C101 C107 H10B 109.5 . . ? H10A C107 H10B 109.5 . . ? C101 C107 H10C 109.5 . . ? H10A C107 H10C 109.5 . . ? H10B C107 H10C 109.5 . . ? C112 C111 C116 120.0 . . ? C112 C111 C117 119.9(4) . . ? C116 C111 C117 119.7(4) . . ? C113 C112 C111 120.0 . . ? C113 C112 H112 120.0 . . ? C111 C112 H112 120.0 . . ? C112 C113 C114 120.0 . . ? C112 C113 H113 120.0 . . ? C114 C113 H113 120.0 . . ? C113 C114 C115 120.0 . . ? C113 C114 H114 120.0 . . ? C115 C114 H114 120.0 . . ? C116 C115 C114 120.0 . . ? C116 C115 H115 120.0 . . ? C114 C115 H115 120.0 . . ? C115 C116 C111 120.0 . . ? C115 C116 H116 120.0 . . ? C111 C116 H116 120.0 . . ? C111 C117 H11D 109.5 . . ? C111 C117 H11E 109.5 . . ? H11D C117 H11E 109.5 . . ? C111 C117 H11F 109.5 . . ? H11D C117 H11F 109.5 . . ? H11E C117 H11F 109.5 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.377 _refine_diff_density_min -1.773 _refine_diff_density_rms 0.093 # Attachment '-CSn-2.cif.txt' data_rf26f3mi _database_code_depnum_ccdc_archive 'CCDC 771274' #TrackingRef '-CSn-2.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety '3(C84 H122 Sn2), 0.5(C4 H10 O)' _chemical_formula_sum 'C254 H371 O0.50 Sn6' _chemical_formula_weight 4144.65 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 15.1577(10) _cell_length_b 22.7946(15) _cell_length_c 36.174(3) _cell_angle_alpha 75.1150(10) _cell_angle_beta 84.2180(10) _cell_angle_gamma 78.7320(10) _cell_volume 11829.4(14) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 9459 _cell_measurement_theta_min 2.18 _cell_measurement_theta_max 27.29 _exptl_crystal_description Block _exptl_crystal_colour Green _exptl_crystal_size_max 0.61 _exptl_crystal_size_mid 0.21 _exptl_crystal_size_min 0.19 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.164 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 4398 _exptl_absorpt_coefficient_mu 0.673 _exptl_absorpt_correction_type Multi-scan _exptl_absorpt_correction_T_min 0.6861 _exptl_absorpt_correction_T_max 0.8844 _exptl_absorpt_process_details 'SADABS 2006/1 (Sheldrick, 2006)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD' _diffrn_measurement_method '\w and \f' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 84959 _diffrn_reflns_av_R_equivalents 0.0751 _diffrn_reflns_av_sigmaI/netI 0.1410 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -27 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_min -43 _diffrn_reflns_limit_l_max 43 _diffrn_reflns_theta_min 1.17 _diffrn_reflns_theta_max 25.25 _reflns_number_total 42862 _reflns_number_gt 21641 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Version 5.054) (Bruker, 2002)' _computing_cell_refinement 'SAINT (7.60A) (Bruker, 2008)' _computing_data_reduction 'SAINT (7.60A) (Bruker, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL97 _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. #============================================================================== The Following Model and Quality ALERTS were generated - (Acta-Mode) <<< #============================================================================== Format: alert-number_ALERT_alert-type_alert-level text 201_ALERT_2_A Isotropic non-H Atoms in Main Residue(s) ....... 18 213_ALERT_2_A Atom C109 has ADP max/min Ratio ..... 8.10 prola 220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 5.11 Ratio 220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 7.75 Ratio 222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 5.53 Ratio 222_ALERT_3_A Large Non-Solvent H Ueq(max)/Ueq(min) ... 8.00 Ratio 412_ALERT_2_A Short Intra XH3 .. XHn H25F .. H26P .. 1.56 Ang. 432_ALERT_2_A Short Inter X...Y Contact C73 .. C80A .. 2.70 Ang. 432_ALERT_2_A Short Inter X...Y Contact C79 .. C80A .. 2.09 Ang. 432_ALERT_2_A Short Inter X...Y Contact C79A .. C80A .. 1.50 Ang. 432_ALERT_2_A Short Inter X...Y Contact C80 .. C80A .. 1.73 Ang. 432_ALERT_2_A Short Inter X...Y Contact C80A .. C81A .. 2.50 Ang. #============================================================================== 201 - The isotropic atoms were either partial occupancy isopropyl ligands or two atoms (C220 and C250) that were attempted to refine isotropically but refined with large Uxx values and attempts at disorder refinement for those two were unsuccessful. 213-222 Four molecules each with disorders and libration 412 This short contact is between two hydrogen atoms wherein one is partial occupancy at 35% (H26P) while the other isopropyl group indicates that it should also be refined in parts but all attempts at sorting this disorder out proved unsuccessful. Therefore, this dubious short contact remains. 432 atoms in different part instructions that are NOT bound to one another. ; _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^)+(0.1014P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 42862 _refine_ls_number_parameters 2421 _refine_ls_number_restraints 47 _refine_ls_R_factor_all 0.1483 _refine_ls_R_factor_gt 0.0716 _refine_ls_wR_factor_ref 0.1980 _refine_ls_wR_factor_gt 0.1733 _refine_ls_goodness_of_fit_ref 0.955 _refine_ls_restrained_S_all 0.957 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.68787(4) 0.80620(2) 0.356588(19) 0.05352(19) Uani 1 1 d . . . Sn2 Sn 0.54104(4) 0.76710(2) 0.398912(17) 0.04427(16) Uani 1 1 d . . . C1 C 0.7073(5) 0.9029(3) 0.3391(2) 0.0332(18) Uani 1 1 d . . . C2 C 0.6828(5) 0.9440(3) 0.36267(19) 0.0304(17) Uani 1 1 d . . . C3 C 0.7054(4) 1.0033(3) 0.3510(2) 0.0318(17) Uani 1 1 d . . . C4 C 0.7519(4) 1.0197(3) 0.3156(2) 0.0296(17) Uani 1 1 d . . . H4 H 0.7646 1.0604 0.3072 0.036 Uiso 1 1 calc R . . C5 C 0.7801(4) 0.9793(3) 0.2924(2) 0.0260(16) Uani 1 1 d . . . C6 C 0.7583(4) 0.9196(3) 0.3048(2) 0.0286(16) Uani 1 1 d . . . C7 C 0.6853(5) 1.0496(3) 0.3757(2) 0.0325(17) Uani 1 1 d . . . H7 H 0.6541 1.0301 0.4002 0.039 Uiso 1 1 calc R . . C8 C 0.6209(5) 1.1091(3) 0.3560(2) 0.0403(19) Uani 1 1 d . . . H8A H 0.6502 1.1293 0.3320 0.060 Uiso 1 1 calc R . . H8B H 0.6070 1.1372 0.3730 0.060 Uiso 1 1 calc R . . H8C H 0.5650 1.0981 0.3505 0.060 Uiso 1 1 calc R . . C9 C 0.7692(5) 1.0672(4) 0.3857(2) 0.042(2) Uani 1 1 d . . . H9A H 0.8126 1.0297 0.3956 0.063 Uiso 1 1 calc R . . H9B H 0.7537 1.0909 0.4053 0.063 Uiso 1 1 calc R . . H9C H 0.7959 1.0923 0.3627 0.063 Uiso 1 1 calc R . . C10 C 0.8341(4) 1.0002(3) 0.2549(2) 0.0293(17) Uani 1 1 d . . . H10 H 0.8629 0.9628 0.2457 0.035 Uiso 1 1 calc R . . C11 C 0.9079(5) 1.0337(4) 0.2595(2) 0.046(2) Uani 1 1 d . . . H11A H 0.8808 1.0731 0.2655 0.069 Uiso 1 1 calc R . . H11B H 0.9452 1.0414 0.2356 0.069 Uiso 1 1 calc R . . H11C H 0.9455 1.0083 0.2803 0.069 Uiso 1 1 calc R . . C12 C 0.7723(5) 1.0427(3) 0.2239(2) 0.044(2) Uani 1 1 d . . . H12A H 0.7259 1.0209 0.2197 0.066 Uiso 1 1 calc R . . H12B H 0.8081 1.0545 0.2000 0.066 Uiso 1 1 calc R . . H12C H 0.7434 1.0799 0.2323 0.066 Uiso 1 1 calc R . . C13 C 0.6318(6) 0.9240(3) 0.4007(2) 0.042(2) Uani 1 1 d . A . C14 C 0.5381(5) 0.9427(3) 0.4038(2) 0.0359(18) Uani 1 1 d . . . C15 C 0.4914(5) 0.9232(3) 0.4390(2) 0.0366(19) Uani 1 1 d . A . H15 H 0.4277 0.9342 0.4407 0.044 Uiso 1 1 calc R . . C16 C 0.5346(6) 0.8892(3) 0.4708(2) 0.045(2) Uani 1 1 d . . . C17 C 0.6265(8) 0.8714(4) 0.4677(2) 0.072(3) Uani 1 1 d . A . H17 H 0.6569 0.8461 0.4895 0.086 Uiso 1 1 calc R . . C18 C 0.6778(6) 0.8895(5) 0.4328(3) 0.072(3) Uani 1 1 d D . . C19 C 0.4840(5) 0.9815(3) 0.37010(19) 0.0284(16) Uani 1 1 d . . . H19 H 0.5271 1.0016 0.3504 0.034 Uiso 1 1 calc R . . C20 C 0.4402(5) 0.9419(4) 0.3514(2) 0.046(2) Uani 1 1 d . . . H20A H 0.4871 0.9123 0.3420 0.069 Uiso 1 1 calc R . . H20B H 0.4055 0.9684 0.3300 0.069 Uiso 1 1 calc R . . H20C H 0.3999 0.9195 0.3704 0.069 Uiso 1 1 calc R . . C21 C 0.4127(5) 1.0333(3) 0.3809(2) 0.042(2) Uani 1 1 d . . . H21A H 0.3636 1.0154 0.3967 0.063 Uiso 1 1 calc R . . H21B H 0.3888 1.0622 0.3576 0.063 Uiso 1 1 calc R . . H21C H 0.4404 1.0553 0.3953 0.063 Uiso 1 1 calc R . . C22 C 0.4833(7) 0.8720(4) 0.5101(2) 0.054(2) Uani 0.63 1 d P A 1 H22 H 0.4967 0.8263 0.5207 0.065 Uiso 0.63 1 calc PR A 1 C23 C 0.3726(10) 0.8953(7) 0.5081(5) 0.071(4) Uiso 0.63 1 d P A 1 H23A H 0.3435 0.8811 0.5334 0.106 Uiso 0.63 1 calc PR A 1 H23B H 0.3499 0.8782 0.4894 0.106 Uiso 0.63 1 calc PR A 1 H23C H 0.3592 0.9405 0.5002 0.106 Uiso 0.63 1 calc PR A 1 C24 C 0.5135(9) 0.9039(6) 0.5372(4) 0.048(3) Uiso 0.63 1 d P A 1 H24A H 0.5788 0.8920 0.5392 0.072 Uiso 0.63 1 calc PR A 1 H24B H 0.4833 0.8917 0.5625 0.072 Uiso 0.63 1 calc PR A 1 H24C H 0.4979 0.9487 0.5273 0.072 Uiso 0.63 1 calc PR A 1 C22A C 0.4833(7) 0.8720(4) 0.5101(2) 0.054(2) Uani 0.37 1 d P A 2 H22A H 0.4277 0.8569 0.5066 0.065 Uiso 0.37 1 calc PR A 2 C23A C 0.457(2) 0.9257(12) 0.5282(8) 0.071(4) Uiso 0.37 1 d P A 2 H23D H 0.5108 0.9429 0.5297 0.106 Uiso 0.37 1 calc PR A 2 H23E H 0.4304 0.9119 0.5540 0.106 Uiso 0.37 1 calc PR A 2 H23F H 0.4133 0.9575 0.5126 0.106 Uiso 0.37 1 calc PR A 2 C24A C 0.5535(15) 0.8135(10) 0.5375(7) 0.053(6) Uiso 0.37 1 d P A 2 H24D H 0.5770 0.7821 0.5232 0.080 Uiso 0.37 1 calc PR A 2 H24E H 0.5204 0.7951 0.5610 0.080 Uiso 0.37 1 calc PR A 2 H24F H 0.6037 0.8295 0.5442 0.080 Uiso 0.37 1 calc PR A 2 C25 C 0.7804(9) 0.8855(7) 0.4364(6) 0.073(6) Uiso 0.55 1 d PD A 1 H25 H 0.8044 0.9031 0.4099 0.088 Uiso 0.55 1 calc PR A 1 C26 C 0.8274(13) 0.8193(8) 0.4465(5) 0.080(5) Uiso 0.55 1 d PD A 1 H26A H 0.8922 0.8173 0.4404 0.120 Uiso 0.55 1 calc PR A 1 H26B H 0.8037 0.7959 0.4317 0.120 Uiso 0.55 1 calc PR A 1 H26C H 0.8167 0.8016 0.4739 0.120 Uiso 0.55 1 calc PR A 1 C27 C 0.8136(12) 0.9190(8) 0.4614(5) 0.076(6) Uiso 0.55 1 d PD A 1 H27A H 0.7733 0.9586 0.4603 0.114 Uiso 0.55 1 calc PR A 1 H27B H 0.8746 0.9263 0.4523 0.114 Uiso 0.55 1 calc PR A 1 H27C H 0.8146 0.8940 0.4878 0.114 Uiso 0.55 1 calc PR A 1 C25D C 0.7718(9) 0.8505(5) 0.4279(4) 0.034(4) Uiso 0.45 1 d PD A 2 H25A H 0.7860 0.8521 0.4001 0.041 Uiso 0.45 1 calc PR A 2 C26D C 0.8278(15) 0.8888(9) 0.4402(7) 0.080(5) Uiso 0.45 1 d PD A 2 H26D H 0.7934 0.9082 0.4597 0.120 Uiso 0.45 1 calc PR A 2 H26E H 0.8436 0.9208 0.4181 0.120 Uiso 0.45 1 calc PR A 2 H26F H 0.8829 0.8624 0.4510 0.120 Uiso 0.45 1 calc PR A 2 C27D C 0.7940(11) 0.7851(6) 0.4506(5) 0.037(4) Uiso 0.45 1 d PD A 2 H27D H 0.8584 0.7696 0.4467 0.055 Uiso 0.45 1 calc PR A 2 H27E H 0.7589 0.7597 0.4421 0.055 Uiso 0.45 1 calc PR A 2 H27F H 0.7794 0.7832 0.4778 0.055 Uiso 0.45 1 calc PR A 2 C28 C 0.7969(4) 0.8697(3) 0.2836(2) 0.0287(17) Uani 1 1 d . B . C29 C 0.8798(5) 0.8324(3) 0.2950(2) 0.0335(18) Uani 1 1 d . . . C30 C 0.9164(5) 0.7841(3) 0.2774(2) 0.0398(19) Uani 1 1 d . B . H30 H 0.9715 0.7582 0.2857 0.048 Uiso 1 1 calc R . . C31 C 0.8735(5) 0.7733(3) 0.2481(2) 0.040(2) Uani 1 1 d . . . C32 C 0.7919(5) 0.8108(3) 0.2375(2) 0.0382(19) Uani 1 1 d . B . H32 H 0.7610 0.8032 0.2181 0.046 Uiso 1 1 calc R . . C33 C 0.7534(5) 0.8596(3) 0.2542(2) 0.0329(18) Uani 1 1 d . . . C34 C 0.9349(5) 0.8453(3) 0.3240(2) 0.039(2) Uani 1 1 d . . . H34 H 0.8968 0.8777 0.3356 0.047 Uiso 1 1 calc R . . C35 C 0.9653(6) 0.7897(4) 0.3562(3) 0.055(2) Uani 1 1 d . . . H35A H 0.9133 0.7707 0.3680 0.083 Uiso 1 1 calc R . . H35B H 0.9925 0.8028 0.3756 0.083 Uiso 1 1 calc R . . H35C H 1.0098 0.7596 0.3460 0.083 Uiso 1 1 calc R . . C36 C 1.0172(6) 0.8714(4) 0.3028(3) 0.064(3) Uani 1 1 d . . . H36A H 1.0577 0.8394 0.2926 0.096 Uiso 1 1 calc R . . H36B H 1.0491 0.8847 0.3206 0.096 Uiso 1 1 calc R . . H36C H 0.9973 0.9067 0.2816 0.096 Uiso 1 1 calc R . . C37 C 0.9145(5) 0.7228(3) 0.2282(2) 0.052(2) Uani 0.58 1 d PD B 1 H37 H 0.8689 0.7205 0.2107 0.062 Uiso 0.58 1 calc PR B 1 C38 C 0.9337(11) 0.6612(6) 0.2555(4) 0.066(4) Uiso 0.58 1 d PD B 1 H38A H 0.9508 0.6293 0.2411 0.099 Uiso 0.58 1 calc PR B 1 H38B H 0.8798 0.6536 0.2720 0.099 Uiso 0.58 1 calc PR B 1 H38C H 0.9833 0.6602 0.2712 0.099 Uiso 0.58 1 calc PR B 1 C39 C 0.9938(10) 0.7397(8) 0.2042(5) 0.067(5) Uiso 0.58 1 d PD B 1 H39A H 0.9819 0.7838 0.1917 0.100 Uiso 0.58 1 calc PR B 1 H39B H 1.0068 0.7159 0.1847 0.100 Uiso 0.58 1 calc PR B 1 H39C H 1.0456 0.7306 0.2202 0.100 Uiso 0.58 1 calc PR B 1 C37A C 0.9145(5) 0.7228(3) 0.2282(2) 0.052(2) Uani 0.42 1 d P B 2 H37A H 0.9027 0.7435 0.2008 0.062 Uiso 0.42 1 calc PR B 2 C38A C 0.8702(12) 0.6692(8) 0.2345(7) 0.066(4) Uiso 0.42 1 d PD B 2 H38D H 0.9119 0.6356 0.2265 0.099 Uiso 0.42 1 calc PR B 2 H38E H 0.8165 0.6804 0.2195 0.099 Uiso 0.42 1 calc PR B 2 H38F H 0.8526 0.6559 0.2618 0.099 Uiso 0.42 1 calc PR B 2 C39A C 1.0143(8) 0.7070(10) 0.2269(7) 0.072(7) Uiso 0.42 1 d PD B 2 H39D H 1.0339 0.6805 0.2517 0.108 Uiso 0.42 1 calc PR B 2 H39E H 1.0397 0.7449 0.2216 0.108 Uiso 0.42 1 calc PR B 2 H39F H 1.0353 0.6852 0.2067 0.108 Uiso 0.42 1 calc PR B 2 C40 C 0.6675(4) 0.9005(3) 0.2385(2) 0.0328(17) Uani 1 1 d . B . H40 H 0.6564 0.9369 0.2500 0.039 Uiso 1 1 calc R . . C41 C 0.5852(5) 0.8687(4) 0.2496(2) 0.046(2) Uani 1 1 d . . . H41A H 0.5950 0.8315 0.2398 0.070 Uiso 1 1 calc R B . H41B H 0.5317 0.8970 0.2385 0.070 Uiso 1 1 calc R . . H41C H 0.5761 0.8574 0.2776 0.070 Uiso 1 1 calc R . . C42 C 0.6756(5) 0.9250(4) 0.1951(2) 0.046(2) Uani 1 1 d . . . H42A H 0.7304 0.9431 0.1880 0.069 Uiso 1 1 calc R B . H42B H 0.6229 0.9567 0.1867 0.069 Uiso 1 1 calc R . . H42C H 0.6787 0.8911 0.1827 0.069 Uiso 1 1 calc R . . C43 C 0.4841(4) 0.6854(3) 0.39832(18) 0.0276(16) Uani 1 1 d . . . C44 C 0.5376(4) 0.6275(3) 0.39802(19) 0.0257(16) Uani 1 1 d . . . C45 C 0.4968(5) 0.5767(3) 0.4010(2) 0.0371(19) Uani 1 1 d . . . C46 C 0.4028(5) 0.5855(3) 0.4039(2) 0.0372(19) Uani 1 1 d . . . H46 H 0.3749 0.5508 0.4063 0.045 Uiso 1 1 calc R . . C47 C 0.3483(4) 0.6410(3) 0.40364(19) 0.0298(17) Uani 1 1 d . . . C48 C 0.3885(5) 0.6918(3) 0.40249(19) 0.0298(17) Uani 1 1 d . . . C49 C 0.5508(5) 0.5137(4) 0.4017(3) 0.058(3) Uani 1 1 d . . . H49 H 0.6160 0.5168 0.4002 0.070 Uiso 1 1 calc R . . C50 C 0.5314(6) 0.4670(4) 0.4397(3) 0.081(4) Uani 1 1 d . . . H50A H 0.5447 0.4818 0.4613 0.122 Uiso 1 1 calc R . . H50B H 0.5693 0.4268 0.4400 0.122 Uiso 1 1 calc R . . H50C H 0.4678 0.4629 0.4418 0.122 Uiso 1 1 calc R . . C51 C 0.5347(6) 0.4895(4) 0.3689(3) 0.084(4) Uani 1 1 d . . . H51A H 0.4738 0.4796 0.3719 0.126 Uiso 1 1 calc R . . H51B H 0.5790 0.4521 0.3682 0.126 Uiso 1 1 calc R . . H51C H 0.5406 0.5207 0.3449 0.126 Uiso 1 1 calc R . . C52 C 0.2462(4) 0.6462(4) 0.4037(2) 0.0346(18) Uani 1 1 d . . . H52 H 0.2177 0.6895 0.4040 0.042 Uiso 1 1 calc R . . C53 C 0.2118(5) 0.6030(4) 0.4400(2) 0.050(2) Uani 1 1 d . . . H53A H 0.2344 0.5600 0.4392 0.075 Uiso 1 1 calc R . . H53B H 0.1458 0.6106 0.4414 0.075 Uiso 1 1 calc R . . H53C H 0.2333 0.6109 0.4627 0.075 Uiso 1 1 calc R . . C54 C 0.2190(5) 0.6322(4) 0.3678(2) 0.057(3) Uani 1 1 d . . . H54A H 0.2380 0.6620 0.3451 0.086 Uiso 1 1 calc R . . H54B H 0.1535 0.6353 0.3688 0.086 Uiso 1 1 calc R . . H54C H 0.2482 0.5904 0.3665 0.086 Uiso 1 1 calc R . . C55 C 0.6375(4) 0.6249(3) 0.3928(2) 0.0244(16) Uani 1 1 d . C . C56 C 0.6891(5) 0.6132(3) 0.4250(2) 0.0359(19) Uani 1 1 d . . . C57 C 0.7817(5) 0.6152(3) 0.4186(2) 0.0364(18) Uani 1 1 d . C . H57 H 0.8170 0.6080 0.4402 0.044 Uiso 1 1 calc R . . C58 C 0.8233(5) 0.6270(3) 0.3826(2) 0.0371(19) Uani 1 1 d . . . C59 C 0.7702(5) 0.6366(3) 0.3512(2) 0.0362(19) Uani 1 1 d . C . H59 H 0.7981 0.6448 0.3262 0.043 Uiso 1 1 calc R . . C60 C 0.6790(4) 0.6346(3) 0.3553(2) 0.0306(17) Uani 1 1 d . . . C61 C 0.6500(5) 0.5959(3) 0.4652(2) 0.041(2) Uani 1 1 d . . . H61 H 0.5841 0.5971 0.4637 0.050 Uiso 1 1 calc R . . C62 C 0.6913(6) 0.5300(4) 0.4854(2) 0.056(2) Uani 1 1 d . . . H62A H 0.6928 0.5026 0.4684 0.083 Uiso 1 1 calc R . . H62B H 0.6548 0.5161 0.5088 0.083 Uiso 1 1 calc R . . H62C H 0.7527 0.5291 0.4921 0.083 Uiso 1 1 calc R . . C63 C 0.6597(6) 0.6412(4) 0.4885(2) 0.064(3) Uani 1 1 d . . . H63A H 0.7233 0.6372 0.4934 0.096 Uiso 1 1 calc R . . H63B H 0.6248 0.6320 0.5130 0.096 Uiso 1 1 calc R . . H63C H 0.6373 0.6834 0.4742 0.096 Uiso 1 1 calc R . . C64 C 0.9245(5) 0.6284(4) 0.3766(2) 0.051(2) Uani 0.75 1 d PD C 1 H64 H 0.9334 0.6631 0.3540 0.061 Uiso 0.75 1 calc PR C 1 C65 C 0.9762(8) 0.5692(5) 0.3676(4) 0.070(4) Uiso 0.75 1 d PD C 1 H65A H 0.9685 0.5343 0.3894 0.106 Uiso 0.75 1 calc PR C 1 H65B H 1.0403 0.5719 0.3630 0.106 Uiso 0.75 1 calc PR C 1 H65C H 0.9533 0.5632 0.3447 0.106 Uiso 0.75 1 calc PR C 1 C66 C 0.9607(7) 0.6410(5) 0.4114(3) 0.050(3) Uiso 0.75 1 d PD C 1 H66A H 0.9612 0.6048 0.4330 0.075 Uiso 0.75 1 calc PR C 1 H66B H 0.9218 0.6768 0.4183 0.075 Uiso 0.75 1 calc PR C 1 H66C H 1.0220 0.6495 0.4050 0.075 Uiso 0.75 1 calc PR C 1 C64A C 0.9245(5) 0.6284(4) 0.3766(2) 0.051(2) Uani 0.25 1 d P C 2 H64A H 0.9406 0.6603 0.3879 0.061 Uiso 0.25 1 calc PR C 2 C65A C 0.958(2) 0.6379(15) 0.3336(4) 0.070(4) Uiso 0.25 1 d PD C 2 H65D H 0.9588 0.6001 0.3254 0.106 Uiso 0.25 1 calc PR C 2 H65E H 1.0187 0.6478 0.3304 0.106 Uiso 0.25 1 calc PR C 2 H65F H 0.9170 0.6720 0.3180 0.106 Uiso 0.25 1 calc PR C 2 C66A C 0.9714(19) 0.5624(8) 0.3972(7) 0.046(8) Uiso 0.25 1 d PD C 2 H66D H 0.9607 0.5565 0.4249 0.070 Uiso 0.25 1 calc PR C 2 H66E H 1.0363 0.5577 0.3907 0.070 Uiso 0.25 1 calc PR C 2 H66F H 0.9466 0.5316 0.3888 0.070 Uiso 0.25 1 calc PR C 2 C67 C 0.6274(5) 0.6419(3) 0.3201(2) 0.0341(18) Uani 1 1 d . C . H67 H 0.5666 0.6318 0.3296 0.041 Uiso 1 1 calc R . . C68 C 0.6696(5) 0.5972(4) 0.2967(2) 0.048(2) Uani 1 1 d . . . H68A H 0.7276 0.6075 0.2851 0.072 Uiso 1 1 calc R C . H68B H 0.6297 0.5996 0.2764 0.072 Uiso 1 1 calc R . . H68C H 0.6791 0.5553 0.3132 0.072 Uiso 1 1 calc R . . C69 C 0.6117(6) 0.7080(3) 0.2948(2) 0.048(2) Uani 1 1 d . . . H69A H 0.6697 0.7218 0.2874 0.072 Uiso 1 1 calc R C . H69B H 0.5735 0.7355 0.3092 0.072 Uiso 1 1 calc R . . H69C H 0.5819 0.7090 0.2718 0.072 Uiso 1 1 calc R . . C70 C 0.3342(5) 0.7525(3) 0.4048(2) 0.0364(19) Uani 1 1 d . D . C71 C 0.3077(5) 0.7625(4) 0.4421(3) 0.054(2) Uani 1 1 d . . . C72 C 0.2563(7) 0.8186(4) 0.4451(3) 0.080(4) Uani 1 1 d . D . H72 H 0.2382 0.8257 0.4698 0.097 Uiso 1 1 calc R . . C73 C 0.2310(7) 0.8642(4) 0.4131(3) 0.082(4) Uani 1 1 d D . . C74 C 0.2539(6) 0.8541(4) 0.3770(3) 0.061(3) Uani 1 1 d . D . H74 H 0.2331 0.8850 0.3550 0.073 Uiso 1 1 calc R . . C75 C 0.3079(5) 0.7984(3) 0.3726(2) 0.040(2) Uani 1 1 d . . . C76 C 0.3338(6) 0.7132(4) 0.4786(2) 0.050(2) Uani 1 1 d . . . H76 H 0.3556 0.6733 0.4711 0.060 Uiso 1 1 calc R . . C77 C 0.4100(7) 0.7262(5) 0.4977(3) 0.078(3) Uani 1 1 d . . . H77A H 0.3904 0.7647 0.5059 0.117 Uiso 1 1 calc R . . H77B H 0.4622 0.7301 0.4795 0.117 Uiso 1 1 calc R . . H77C H 0.4265 0.6922 0.5200 0.117 Uiso 1 1 calc R . . C78 C 0.2538(6) 0.7043(5) 0.5072(3) 0.074(3) Uani 1 1 d . . . H78A H 0.2719 0.6693 0.5289 0.110 Uiso 1 1 calc R . . H78B H 0.2047 0.6960 0.4947 0.110 Uiso 1 1 calc R . . H78C H 0.2333 0.7417 0.5165 0.110 Uiso 1 1 calc R . . C79 C 0.1528(10) 0.9208(6) 0.4104(6) 0.066(6) Uiso 0.50 1 d PD D 1 H79 H 0.1367 0.9152 0.4384 0.079 Uiso 0.50 1 calc PR D 1 C80 C 0.1943(13) 0.9756(9) 0.4044(7) 0.093(5) Uiso 0.50 1 d PD D 1 H80A H 0.2143 0.9884 0.3774 0.140 Uiso 0.50 1 calc PR D 1 H80B H 0.2463 0.9659 0.4204 0.140 Uiso 0.50 1 calc PR D 1 H80C H 0.1502 1.0091 0.4115 0.140 Uiso 0.50 1 calc PR D 1 C81 C 0.0623(12) 0.9275(11) 0.3975(8) 0.112(7) Uiso 0.50 1 d PD D 1 H81A H 0.0219 0.9133 0.4195 0.168 Uiso 0.50 1 calc PR D 1 H81B H 0.0640 0.9027 0.3789 0.168 Uiso 0.50 1 calc PR D 1 H81C H 0.0402 0.9709 0.3855 0.168 Uiso 0.50 1 calc PR D 1 C79A C 0.1807(12) 0.9284(7) 0.4203(6) 0.076(7) Uiso 0.50 1 d PD D 2 H79A H 0.1916 0.9609 0.3966 0.092 Uiso 0.50 1 calc PR D 2 C80A C 0.1974(14) 0.9512(10) 0.4538(6) 0.093(5) Uiso 0.50 1 d PD D 2 H80D H 0.1687 0.9945 0.4504 0.140 Uiso 0.50 1 calc PR D 2 H80E H 0.2624 0.9474 0.4557 0.140 Uiso 0.50 1 calc PR D 2 H80F H 0.1721 0.9265 0.4774 0.140 Uiso 0.50 1 calc PR D 2 C81A C 0.0837(14) 0.9199(13) 0.4208(7) 0.112(7) Uiso 0.50 1 d PD D 2 H81D H 0.0498 0.9323 0.4429 0.168 Uiso 0.50 1 calc PR D 2 H81E H 0.0821 0.8764 0.4227 0.168 Uiso 0.50 1 calc PR D 2 H81F H 0.0565 0.9454 0.3972 0.168 Uiso 0.50 1 calc PR D 2 C82 C 0.3291(5) 0.7871(4) 0.3329(2) 0.045(2) Uani 1 1 d . D . H82 H 0.3664 0.7450 0.3357 0.054 Uiso 1 1 calc R . . C83 C 0.3809(6) 0.8318(4) 0.3066(3) 0.063(3) Uani 1 1 d . . . H83A H 0.3446 0.8733 0.3022 0.095 Uiso 1 1 calc R D . H83B H 0.3953 0.8202 0.2821 0.095 Uiso 1 1 calc R . . H83C H 0.4369 0.8313 0.3182 0.095 Uiso 1 1 calc R . . C84 C 0.2405(7) 0.7878(6) 0.3141(3) 0.099(4) Uani 1 1 d . . . H84A H 0.2080 0.8303 0.3065 0.149 Uiso 1 1 calc R D . H84B H 0.2026 0.7627 0.3326 0.149 Uiso 1 1 calc R . . H84C H 0.2553 0.7708 0.2915 0.149 Uiso 1 1 calc R . . Sn3 Sn 0.02635(3) 0.31701(2) 0.302378(13) 0.02243(12) Uani 1 1 d . . . Sn4 Sn 0.12735(3) 0.26365(2) 0.249392(13) 0.02277(12) Uani 1 1 d . . . C101 C 0.0760(4) 0.3258(3) 0.35550(18) 0.0195(14) Uani 1 1 d . . . C102 C 0.1609(4) 0.3418(3) 0.3558(2) 0.0283(17) Uani 1 1 d . . . C103 C 0.1854(4) 0.3543(4) 0.3885(2) 0.045(2) Uani 1 1 d . . . C104 C 0.1247(5) 0.3492(4) 0.4208(2) 0.055(3) Uani 1 1 d . . . H104 H 0.1424 0.3557 0.4437 0.066 Uiso 1 1 calc R . . C105 C 0.0409(4) 0.3352(3) 0.4205(2) 0.0331(18) Uani 1 1 d . . . C106 C 0.0161(4) 0.3232(3) 0.38780(18) 0.0218(15) Uani 1 1 d . . . C107 C 0.2749(5) 0.3731(6) 0.3910(3) 0.086(4) Uani 1 1 d . . . H107 H 0.3059 0.3791 0.3649 0.104 Uiso 1 1 calc R . . C108 C 0.2607(6) 0.4356(6) 0.4026(3) 0.097(4) Uani 1 1 d . . . H10A H 0.2195 0.4666 0.3853 0.145 Uiso 1 1 calc R . . H10B H 0.3188 0.4492 0.4009 0.145 Uiso 1 1 calc R . . H10C H 0.2349 0.4303 0.4290 0.145 Uiso 1 1 calc R . . C109 C 0.3360(6) 0.3224(7) 0.4184(4) 0.155(8) Uani 1 1 d . . . H10D H 0.3166 0.3235 0.4449 0.232 Uiso 1 1 calc R . . H10E H 0.3984 0.3292 0.4134 0.232 Uiso 1 1 calc R . . H10F H 0.3321 0.2821 0.4144 0.232 Uiso 1 1 calc R . . C110 C -0.0228(5) 0.3349(4) 0.45630(19) 0.045(2) Uani 1 1 d . . . H110 H -0.0815 0.3263 0.4505 0.054 Uiso 1 1 calc R . . C111 C 0.0148(7) 0.2827(6) 0.4908(3) 0.102(5) Uani 1 1 d . . . H11D H 0.0082 0.2427 0.4870 0.152 Uiso 1 1 calc R . . H11E H -0.0188 0.2892 0.5144 0.152 Uiso 1 1 calc R . . H11F H 0.0786 0.2833 0.4927 0.152 Uiso 1 1 calc R . . C112 C -0.0414(6) 0.3974(4) 0.4668(3) 0.062(3) Uani 1 1 d . . . H11G H -0.0870 0.3965 0.4881 0.093 Uiso 1 1 calc R . . H11H H -0.0634 0.4300 0.4446 0.093 Uiso 1 1 calc R . . H11I H 0.0144 0.4055 0.4745 0.093 Uiso 1 1 calc R . . C113 C 0.2209(4) 0.3447(3) 0.31997(19) 0.0256(16) Uani 1 1 d . . . C114 C 0.2870(4) 0.2935(3) 0.3168(2) 0.0266(16) Uani 1 1 d . . . C115 C 0.3397(4) 0.2955(3) 0.2830(2) 0.0311(17) Uani 1 1 d . . . H115 H 0.3819 0.2600 0.2801 0.037 Uiso 1 1 calc R . . C116 C 0.3321(4) 0.3485(3) 0.2529(2) 0.0340(18) Uani 1 1 d . . . C117 C 0.2699(4) 0.3987(3) 0.2573(2) 0.0332(18) Uani 1 1 d . . . H117 H 0.2652 0.4352 0.2372 0.040 Uiso 1 1 calc R . . C118 C 0.2133(5) 0.3985(3) 0.2899(2) 0.0363(19) Uani 1 1 d . . . C119 C 0.3001(4) 0.2362(3) 0.3489(2) 0.0293(17) Uani 1 1 d . . . H119 H 0.2730 0.2480 0.3729 0.035 Uiso 1 1 calc R . . C120 C 0.2518(5) 0.1862(4) 0.3432(2) 0.044(2) Uani 1 1 d . . . H12D H 0.1867 0.2013 0.3431 0.067 Uiso 1 1 calc R . . H12E H 0.2648 0.1492 0.3641 0.067 Uiso 1 1 calc R . . H12F H 0.2731 0.1760 0.3187 0.067 Uiso 1 1 calc R . . C121 C 0.4002(4) 0.2086(3) 0.3554(2) 0.0339(18) Uani 1 1 d . . . H12G H 0.4275 0.1928 0.3333 0.051 Uiso 1 1 calc R . . H12H H 0.4050 0.1748 0.3786 0.051 Uiso 1 1 calc R . . H12I H 0.4317 0.2406 0.3584 0.051 Uiso 1 1 calc R . . C122 C 0.3966(5) 0.3476(4) 0.2178(2) 0.042(2) Uani 1 1 d . . . H122 H 0.3996 0.3070 0.2115 0.050 Uiso 1 1 calc R . . C123 C 0.3647(6) 0.3978(4) 0.1825(2) 0.053(2) Uani 1 1 d . . . H12J H 0.3025 0.3962 0.1782 0.080 Uiso 1 1 calc R . . H12K H 0.4036 0.3912 0.1601 0.080 Uiso 1 1 calc R . . H12L H 0.3676 0.4383 0.1865 0.080 Uiso 1 1 calc R . . C124 C 0.4922(5) 0.3511(4) 0.2265(3) 0.054(2) Uani 1 1 d . . . H12M H 0.5344 0.3425 0.2054 0.081 Uiso 1 1 calc R . . H12N H 0.5096 0.3206 0.2503 0.081 Uiso 1 1 calc R . . H12O H 0.4936 0.3925 0.2295 0.081 Uiso 1 1 calc R . . C125 C 0.1458(5) 0.4575(3) 0.2925(2) 0.040(2) Uani 1 1 d . . . H125 H 0.1049 0.4472 0.3158 0.048 Uiso 1 1 calc R . . C126 C 0.0892(6) 0.4826(3) 0.2589(3) 0.055(3) Uani 1 1 d . . . H12P H 0.1274 0.4956 0.2359 0.083 Uiso 1 1 calc R . . H12Q H 0.0448 0.5182 0.2631 0.083 Uiso 1 1 calc R . . H12R H 0.0578 0.4507 0.2556 0.083 Uiso 1 1 calc R . . C127 C 0.1975(6) 0.5070(4) 0.2978(3) 0.070(3) Uani 1 1 d . . . H12S H 0.2360 0.5195 0.2748 0.105 Uiso 1 1 calc R . . H12T H 0.2349 0.4898 0.3200 0.105 Uiso 1 1 calc R . . H12U H 0.1543 0.5431 0.3021 0.105 Uiso 1 1 calc R . . C128 C -0.0758(4) 0.3110(3) 0.38357(18) 0.0208(14) Uani 1 1 d . . . C129 C -0.1448(4) 0.3610(3) 0.36970(19) 0.0229(15) Uani 1 1 d . . . C130 C -0.2273(4) 0.3495(3) 0.3623(2) 0.0316(17) Uani 1 1 d . . . H130 H -0.2730 0.3836 0.3528 0.038 Uiso 1 1 calc R . . C131 C -0.2453(5) 0.2913(4) 0.3682(2) 0.040(2) Uani 1 1 d . . . C132 C -0.1786(5) 0.2423(4) 0.3837(2) 0.045(2) Uani 1 1 d . . . H132 H -0.1905 0.2015 0.3889 0.054 Uiso 1 1 calc R . . C133 C -0.0950(5) 0.2509(3) 0.3920(2) 0.0322(18) Uani 1 1 d . . . C134 C -0.1326(4) 0.4271(3) 0.3655(2) 0.0286(16) Uani 1 1 d . . . H134 H -0.0722 0.4262 0.3747 0.034 Uiso 1 1 calc R . . C135 C -0.1358(6) 0.4642(3) 0.3231(2) 0.049(2) Uani 1 1 d . . . H13A H -0.1944 0.4653 0.3134 0.074 Uiso 1 1 calc R . . H13B H -0.0878 0.4444 0.3077 0.074 Uiso 1 1 calc R . . H13C H -0.1273 0.5064 0.3212 0.074 Uiso 1 1 calc R . . C136 C -0.2038(5) 0.4587(3) 0.3899(2) 0.042(2) Uani 1 1 d . . . H13D H -0.2633 0.4626 0.3802 0.063 Uiso 1 1 calc R . . H13E H -0.1916 0.4997 0.3889 0.063 Uiso 1 1 calc R . . H13F H -0.2026 0.4341 0.4165 0.063 Uiso 1 1 calc R . . C137 C -0.3352(6) 0.2780(5) 0.3609(3) 0.065(3) Uani 1 1 d . . . H137 H -0.3230 0.2401 0.3509 0.078 Uiso 1 1 calc R . . C138 C -0.3902(6) 0.3287(6) 0.3320(3) 0.084(4) Uani 1 1 d . . . H13G H -0.4059 0.3661 0.3416 0.126 Uiso 1 1 calc R . . H13H H -0.4454 0.3153 0.3280 0.126 Uiso 1 1 calc R . . H13I H -0.3547 0.3375 0.3076 0.126 Uiso 1 1 calc R . . C139 C -0.3902(6) 0.2635(5) 0.3992(3) 0.082(4) Uani 1 1 d . . . H13J H -0.3558 0.2289 0.4172 0.122 Uiso 1 1 calc R . . H13K H -0.4471 0.2525 0.3950 0.122 Uiso 1 1 calc R . . H13L H -0.4029 0.2999 0.4099 0.122 Uiso 1 1 calc R . . C140 C -0.0253(6) 0.1960(3) 0.4097(2) 0.047(2) Uani 1 1 d . . . H140 H 0.0301 0.2112 0.4133 0.057 Uiso 1 1 calc R . . C141 C -0.0004(6) 0.1510(3) 0.3837(3) 0.055(3) Uani 1 1 d . . . H14A H -0.0532 0.1334 0.3816 0.083 Uiso 1 1 calc R . . H14B H 0.0482 0.1178 0.3947 0.083 Uiso 1 1 calc R . . H14C H 0.0196 0.1730 0.3582 0.083 Uiso 1 1 calc R . . C142 C -0.0621(8) 0.1618(6) 0.4496(3) 0.102(4) Uiso 1 1 d . . . H14D H -0.0871 0.1917 0.4647 0.154 Uiso 1 1 calc R . . H14E H -0.0130 0.1319 0.4630 0.154 Uiso 1 1 calc R . . H14F H -0.1094 0.1402 0.4460 0.154 Uiso 1 1 calc R . . C143 C 0.0722(4) 0.2217(3) 0.21057(19) 0.0244(15) Uani 1 1 d . . . C144 C -0.0111(4) 0.2479(3) 0.19357(19) 0.0286(17) Uani 1 1 d . . . C145 C -0.0413(4) 0.2210(3) 0.1684(2) 0.0327(18) Uani 1 1 d . . . C146 C 0.0136(5) 0.1694(4) 0.1585(2) 0.041(2) Uani 1 1 d . . . H146 H -0.0078 0.1505 0.1414 0.050 Uiso 1 1 calc R . . C147 C 0.0992(4) 0.1451(3) 0.1731(2) 0.0343(18) Uani 1 1 d . . . C148 C 0.1263(4) 0.1714(3) 0.2000(2) 0.0288(17) Uani 1 1 d . . . C149 C -0.1323(5) 0.2466(4) 0.1496(2) 0.042(2) Uani 1 1 d . . . H149 H -0.1639 0.2811 0.1610 0.050 Uiso 1 1 calc R . . C150 C -0.1183(6) 0.2727(5) 0.1065(2) 0.067(3) Uani 1 1 d . . . H15A H -0.0842 0.3064 0.1019 0.101 Uiso 1 1 calc R . . H15B H -0.1770 0.2882 0.0952 0.101 Uiso 1 1 calc R . . H15C H -0.0848 0.2401 0.0948 0.101 Uiso 1 1 calc R . . C151 C -0.1916(5) 0.1985(4) 0.1575(3) 0.056(3) Uani 1 1 d . . . H15D H -0.2507 0.2173 0.1472 0.084 Uiso 1 1 calc R . . H15E H -0.1990 0.1817 0.1852 0.084 Uiso 1 1 calc R . . H15F H -0.1639 0.1652 0.1452 0.084 Uiso 1 1 calc R . . C152 C 0.1574(5) 0.0903(4) 0.1608(2) 0.039(2) Uani 1 1 d . . . H152 H 0.2177 0.0836 0.1716 0.047 Uiso 1 1 calc R . . C153 C 0.1715(5) 0.1036(5) 0.1169(3) 0.063(3) Uani 1 1 d . . . H15G H 0.1143 0.1061 0.1056 0.094 Uiso 1 1 calc R . . H15H H 0.2161 0.0704 0.1098 0.094 Uiso 1 1 calc R . . H15I H 0.1931 0.1429 0.1072 0.094 Uiso 1 1 calc R . . C154 C 0.1177(5) 0.0312(4) 0.1768(3) 0.060(3) Uani 1 1 d . . . H15J H 0.1131 0.0222 0.2048 0.089 Uiso 1 1 calc R . . H15K H 0.1569 -0.0032 0.1686 0.089 Uiso 1 1 calc R . . H15L H 0.0576 0.0370 0.1672 0.089 Uiso 1 1 calc R . . C155 C -0.0655(4) 0.3048(3) 0.20414(18) 0.0239(15) Uani 1 1 d . . . C156 C -0.1394(4) 0.2983(3) 0.23183(19) 0.0240(16) Uani 1 1 d . . . C157 C -0.1876(4) 0.3505(3) 0.24122(18) 0.0294(17) Uani 1 1 d . . . H157 H -0.2365 0.3463 0.2597 0.035 Uiso 1 1 calc R . . C158 C -0.1681(5) 0.4098(3) 0.22473(19) 0.0302(17) Uani 1 1 d . . . C159 C -0.0956(4) 0.4140(3) 0.19837(18) 0.0296(17) Uani 1 1 d . . . H159 H -0.0809 0.4536 0.1868 0.035 Uiso 1 1 calc R . . C160 C -0.0428(4) 0.3625(3) 0.18803(19) 0.0298(17) Uani 1 1 d . . . C161 C -0.1657(4) 0.2361(3) 0.2495(2) 0.0334(18) Uani 1 1 d . . . H161 H -0.1352 0.2074 0.2335 0.040 Uiso 1 1 calc R . . C162 C -0.1335(5) 0.2097(3) 0.2896(2) 0.0356(18) Uani 1 1 d . . . H16A H -0.0675 0.2012 0.2886 0.053 Uiso 1 1 calc R . . H16B H -0.1565 0.1714 0.3010 0.053 Uiso 1 1 calc R . . H16C H -0.1556 0.2395 0.3052 0.053 Uiso 1 1 calc R . . C163 C -0.2678(5) 0.2386(4) 0.2491(3) 0.053(2) Uani 1 1 d . . . H16D H -0.2991 0.2600 0.2683 0.079 Uiso 1 1 calc R . . H16E H -0.2806 0.1966 0.2552 0.079 Uiso 1 1 calc R . . H16F H -0.2887 0.2610 0.2237 0.079 Uiso 1 1 calc R . . C164 C -0.2301(5) 0.4653(3) 0.2339(2) 0.041(2) Uani 1 1 d . . . H164 H -0.2490 0.4541 0.2617 0.049 Uiso 1 1 calc R . . C165 C -0.1855(6) 0.5217(3) 0.2269(2) 0.046(2) Uani 1 1 d . . . H16G H -0.1295 0.5107 0.2405 0.069 Uiso 1 1 calc R . . H16H H -0.2263 0.5544 0.2363 0.069 Uiso 1 1 calc R . . H16I H -0.1717 0.5365 0.1994 0.069 Uiso 1 1 calc R . . C166 C -0.3147(5) 0.4799(4) 0.2114(2) 0.059(3) Uani 1 1 d . . . H16J H -0.3573 0.5134 0.2192 0.088 Uiso 1 1 calc R . . H16K H -0.3427 0.4431 0.2165 0.088 Uiso 1 1 calc R . . H16L H -0.2987 0.4926 0.1839 0.088 Uiso 1 1 calc R . . C167 C 0.0335(5) 0.3731(3) 0.1576(2) 0.0346(18) Uani 1 1 d . . . H167 H 0.0695 0.3318 0.1563 0.042 Uiso 1 1 calc R . . C168 C 0.0972(5) 0.4113(3) 0.1665(2) 0.046(2) Uani 1 1 d . . . H16M H 0.0655 0.4537 0.1646 0.069 Uiso 1 1 calc R . . H16N H 0.1493 0.4116 0.1481 0.069 Uiso 1 1 calc R . . H16O H 0.1178 0.3933 0.1925 0.069 Uiso 1 1 calc R . . C169 C -0.0055(5) 0.4042(4) 0.1178(2) 0.061(3) Uani 1 1 d . . . H16P H -0.0531 0.3831 0.1140 0.091 Uiso 1 1 calc R . . H16Q H 0.0425 0.4015 0.0977 0.091 Uiso 1 1 calc R . . H16R H -0.0306 0.4476 0.1166 0.091 Uiso 1 1 calc R . . C170 C 0.2187(4) 0.1498(3) 0.21590(19) 0.0210(15) Uani 1 1 d . . . C171 C 0.2915(4) 0.1762(3) 0.19651(19) 0.0242(15) Uani 1 1 d . . . C172 C 0.3747(4) 0.1612(3) 0.21288(19) 0.0240(15) Uani 1 1 d . . . H172 H 0.4236 0.1792 0.1993 0.029 Uiso 1 1 calc R . . C173 C 0.3880(4) 0.1207(3) 0.24842(19) 0.0238(15) Uani 1 1 d . . . C174 C 0.3151(4) 0.0944(3) 0.2665(2) 0.0264(16) Uani 1 1 d . . . H174 H 0.3230 0.0661 0.2908 0.032 Uiso 1 1 calc R . . C175 C 0.2319(4) 0.1069(3) 0.2514(2) 0.0254(16) Uani 1 1 d . . . C176 C 0.2844(5) 0.2178(3) 0.15572(19) 0.0316(17) Uani 1 1 d . . . H176 H 0.2219 0.2211 0.1479 0.038 Uiso 1 1 calc R . . C177 C 0.2986(6) 0.2815(3) 0.1539(2) 0.044(2) Uani 1 1 d . . . H17A H 0.2620 0.2968 0.1746 0.066 Uiso 1 1 calc R . . H17B H 0.2809 0.3088 0.1291 0.066 Uiso 1 1 calc R . . H17C H 0.3624 0.2808 0.1570 0.066 Uiso 1 1 calc R . . C178 C 0.3498(5) 0.1886(4) 0.1274(2) 0.040(2) Uani 1 1 d . . . H17D H 0.3356 0.2111 0.1011 0.060 Uiso 1 1 calc R . . H17E H 0.3438 0.1454 0.1312 0.060 Uiso 1 1 calc R . . H17F H 0.4117 0.1908 0.1318 0.060 Uiso 1 1 calc R . . C179 C 0.4788(4) 0.1027(3) 0.26619(19) 0.0274(16) Uani 1 1 d . . . H179 H 0.4673 0.0973 0.2945 0.033 Uiso 1 1 calc R . . C180 C 0.5399(4) 0.1493(3) 0.2529(2) 0.0308(17) Uani 1 1 d . . . H18A H 0.5577 0.1526 0.2257 0.046 Uiso 1 1 calc R . . H18B H 0.5938 0.1363 0.2679 0.046 Uiso 1 1 calc R . . H18C H 0.5083 0.1895 0.2563 0.046 Uiso 1 1 calc R . . C181 C 0.5245(5) 0.0394(3) 0.2593(2) 0.0376(19) Uani 1 1 d . . . H18D H 0.5468 0.0445 0.2325 0.056 Uiso 1 1 calc R . . H18E H 0.4807 0.0115 0.2651 0.056 Uiso 1 1 calc R . . H18F H 0.5750 0.0222 0.2761 0.056 Uiso 1 1 calc R . . C182 C 0.1573(5) 0.0722(3) 0.2720(2) 0.0328(18) Uani 1 1 d . . . H182 H 0.1052 0.0838 0.2551 0.039 Uiso 1 1 calc R . . C183 C 0.1242(5) 0.0875(4) 0.3099(2) 0.051(2) Uani 1 1 d . . . H18G H 0.1714 0.0706 0.3283 0.076 Uiso 1 1 calc R . . H18H H 0.0702 0.0695 0.3197 0.076 Uiso 1 1 calc R . . H18I H 0.1095 0.1324 0.3062 0.076 Uiso 1 1 calc R . . C184 C 0.1916(5) 0.0016(3) 0.2784(3) 0.047(2) Uani 1 1 d . . . H18J H 0.2143 -0.0079 0.2539 0.071 Uiso 1 1 calc R . . H18K H 0.1419 -0.0205 0.2891 0.071 Uiso 1 1 calc R . . H18L H 0.2402 -0.0112 0.2963 0.071 Uiso 1 1 calc R . . Sn5 Sn 0.42424(5) 0.74623(4) 0.08314(2) 0.0343(2) Uani 0.65 1 d P E 1 Sn6 Sn 0.26130(5) 0.77659(4) 0.05648(2) 0.0324(2) Uani 0.65 1 d P E 1 Sn5A Sn 0.39192(12) 0.71527(11) 0.04950(7) 0.0376(5) Uani 0.30 1 d P E 2 Sn6A Sn 0.28177(11) 0.76553(10) 0.09821(5) 0.0429(5) Uani 0.30 1 d P E 2 Sn5B Sn 0.3834(14) 0.6899(9) 0.0646(6) 0.081(7) Uiso 0.05 1 d P E 3 Sn6B Sn 0.2845(7) 0.8090(5) 0.0630(3) 0.025(2) Uiso 0.05 1 d P E 3 C201 C 0.5457(5) 0.6948(4) 0.0568(3) 0.051(2) Uani 1 1 d . . . C202 C 0.5947(5) 0.6509(3) 0.0859(2) 0.044(2) Uani 1 1 d . E . C203 C 0.6818(4) 0.6231(3) 0.0774(2) 0.0323(17) Uani 1 1 d . . . C204 C 0.7183(4) 0.6421(3) 0.04013(19) 0.0298(17) Uani 1 1 d . E . H204 H 0.7792 0.6253 0.0345 0.036 Uiso 1 1 calc R . . C205 C 0.6712(5) 0.6834(3) 0.0113(2) 0.0320(17) Uani 1 1 d . . . C206 C 0.5814(5) 0.7103(3) 0.0193(2) 0.043(2) Uani 1 1 d . E . C207 C 0.7388(5) 0.5727(3) 0.1058(2) 0.0344(18) Uani 1 1 d . E . H207 H 0.7011 0.5628 0.1302 0.041 Uiso 1 1 calc R . . C208 C 0.7668(5) 0.5139(3) 0.0918(2) 0.047(2) Uani 1 1 d . . . H20D H 0.7143 0.5039 0.0825 0.071 Uiso 1 1 calc R E . H20E H 0.7910 0.4799 0.1129 0.071 Uiso 1 1 calc R . . H20F H 0.8131 0.5200 0.0709 0.071 Uiso 1 1 calc R . . C209 C 0.8216(5) 0.5926(4) 0.1150(2) 0.050(2) Uani 1 1 d . . . H20G H 0.8628 0.5985 0.0922 0.075 Uiso 1 1 calc R E . H20H H 0.8518 0.5607 0.1358 0.075 Uiso 1 1 calc R . . H20I H 0.8041 0.6314 0.1229 0.075 Uiso 1 1 calc R . . C210 C 0.7211(5) 0.7000(4) -0.0283(2) 0.049(2) Uani 1 1 d . E . H210 H 0.6773 0.7286 -0.0465 0.059 Uiso 1 1 calc R . . C211 C 0.7573(7) 0.6431(5) -0.0438(2) 0.075(3) Uani 1 1 d . . . H21D H 0.8016 0.6148 -0.0267 0.112 Uiso 1 1 calc R E . H21E H 0.7860 0.6557 -0.0694 0.112 Uiso 1 1 calc R . . H21F H 0.7075 0.6223 -0.0453 0.112 Uiso 1 1 calc R . . C212 C 0.7980(6) 0.7335(4) -0.0263(3) 0.070(3) Uani 1 1 d . . . H21G H 0.7745 0.7692 -0.0156 0.104 Uiso 1 1 calc R E . H21H H 0.8250 0.7474 -0.0521 0.104 Uiso 1 1 calc R . . H21I H 0.8439 0.7053 -0.0099 0.104 Uiso 1 1 calc R . . C213 C 0.5474(5) 0.6339(4) 0.1265(3) 0.050(2) Uani 1 1 d . . . C214 C 0.5524(6) 0.6657(4) 0.1544(3) 0.057(3) Uani 1 1 d . E . C215 C 0.5024(6) 0.6499(4) 0.1890(3) 0.064(3) Uani 1 1 d . . . H215 H 0.5041 0.6721 0.2078 0.077 Uiso 1 1 calc R E . C216 C 0.4516(6) 0.6048(5) 0.1973(3) 0.060(3) Uani 1 1 d . E . C217 C 0.4488(5) 0.5733(4) 0.1701(3) 0.063(3) Uani 1 1 d . . . H217 H 0.4136 0.5416 0.1755 0.076 Uiso 1 1 calc R E . C218 C 0.4964(6) 0.5863(4) 0.1344(3) 0.054(2) Uani 1 1 d . E . C219 C 0.6129(6) 0.7127(3) 0.1496(3) 0.066(3) Uani 1 1 d . . . H219 H 0.6452 0.7170 0.1237 0.079 Uiso 1 1 calc R E . C220 C 0.5590(9) 0.7759(6) 0.1523(4) 0.119(5) Uiso 1 1 d . E . H22B H 0.5135 0.7896 0.1330 0.178 Uiso 1 1 calc R . . H22C H 0.5998 0.8058 0.1476 0.178 Uiso 1 1 calc R . . H22D H 0.5292 0.7728 0.1778 0.178 Uiso 1 1 calc R . . C221 C 0.6826(8) 0.6917(5) 0.1799(3) 0.079(3) Uani 1 1 d . E . H22E H 0.6523 0.6909 0.2052 0.118 Uiso 1 1 calc R . . H22F H 0.7254 0.7203 0.1747 0.118 Uiso 1 1 calc R . . H22G H 0.7151 0.6502 0.1794 0.118 Uiso 1 1 calc R . . C222 C 0.3988(6) 0.5844(4) 0.2351(3) 0.071(3) Uani 1 1 d . . . H222 H 0.3372 0.5802 0.2297 0.085 Uiso 1 1 calc R E . C223 C 0.3900(8) 0.6331(5) 0.2613(3) 0.099(4) Uani 1 1 d . E . H22H H 0.3528 0.6199 0.2846 0.149 Uiso 1 1 calc R . . H22I H 0.3618 0.6740 0.2469 0.149 Uiso 1 1 calc R . . H22J H 0.4500 0.6350 0.2682 0.149 Uiso 1 1 calc R . . C224 C 0.4447(6) 0.5244(4) 0.2585(3) 0.059(3) Uani 1 1 d . E . H22K H 0.4546 0.4934 0.2435 0.089 Uiso 1 1 calc R . . H22L H 0.4068 0.5111 0.2816 0.089 Uiso 1 1 calc R . . H22M H 0.5027 0.5295 0.2659 0.089 Uiso 1 1 calc R . . C225 C 0.4962(6) 0.5478(4) 0.1056(3) 0.069(3) Uani 1 1 d . . . H225 H 0.5309 0.5659 0.0818 0.082 Uiso 1 1 calc R E . C226 C 0.4030(6) 0.5444(5) 0.0945(3) 0.076(3) Uani 1 1 d . E . H22N H 0.3695 0.5237 0.1171 0.113 Uiso 1 1 calc R . . H22O H 0.4095 0.5212 0.0747 0.113 Uiso 1 1 calc R . . H22P H 0.3703 0.5863 0.0845 0.113 Uiso 1 1 calc R . . C227 C 0.5444(6) 0.4798(4) 0.1216(3) 0.076(3) Uani 1 1 d . E . H22Q H 0.6046 0.4799 0.1293 0.114 Uiso 1 1 calc R . . H22R H 0.5499 0.4570 0.1017 0.114 Uiso 1 1 calc R . . H22S H 0.5090 0.4600 0.1438 0.114 Uiso 1 1 calc R . . C228 C 0.5234(5) 0.7516(4) -0.0118(2) 0.047(2) Uani 1 1 d . . . C229 C 0.4690(6) 0.7272(4) -0.0310(3) 0.075(3) Uani 1 1 d D E . C230 C 0.4107(6) 0.7655(4) -0.0576(3) 0.064(3) Uani 1 1 d . . . H230 H 0.3722 0.7481 -0.0692 0.077 Uiso 1 1 calc R E . C231 C 0.4070(5) 0.8289(3) -0.0676(2) 0.0399(19) Uani 1 1 d . E . C232 C 0.4616(5) 0.8527(3) -0.0493(2) 0.0347(18) Uani 1 1 d . . . H232 H 0.4590 0.8961 -0.0557 0.042 Uiso 1 1 calc R E . C233 C 0.5212(4) 0.8159(3) -0.0213(2) 0.0345(18) Uani 1 1 d . E . C234 C 0.4835(11) 0.6574(6) -0.0338(5) 0.058(4) Uiso 0.46 1 d PD E 1 H234 H 0.5211 0.6316 -0.0123 0.070 Uiso 0.46 1 calc PR E 1 C235 C 0.3917(11) 0.6331(10) -0.0295(6) 0.071(6) Uiso 0.46 1 d PD E 1 H23G H 0.3607 0.6495 -0.0535 0.107 Uiso 0.46 1 calc PR E 1 H23H H 0.3537 0.6468 -0.0087 0.107 Uiso 0.46 1 calc PR E 1 H23I H 0.4036 0.5879 -0.0237 0.107 Uiso 0.46 1 calc PR E 1 C236 C 0.5291(12) 0.6420(9) -0.0720(5) 0.060(6) Uiso 0.46 1 d PD E 1 H23J H 0.5170 0.6021 -0.0736 0.091 Uiso 0.46 1 calc PR E 1 H23K H 0.5943 0.6402 -0.0722 0.091 Uiso 0.46 1 calc PR E 1 H23L H 0.5044 0.6742 -0.0939 0.091 Uiso 0.46 1 calc PR E 1 C23D C 0.4628(9) 0.6571(6) -0.0131(4) 0.058(4) Uiso 0.54 1 d PD E 2 H23M H 0.5033 0.6383 0.0086 0.070 Uiso 0.54 1 calc PR E 2 C23E C 0.3654(9) 0.6434(8) -0.0025(5) 0.062(5) Uiso 0.54 1 d PD E 2 H23N H 0.3303 0.6574 -0.0255 0.093 Uiso 0.54 1 calc PR E 2 H23O H 0.3368 0.6651 0.0169 0.093 Uiso 0.54 1 calc PR E 2 H23P H 0.3680 0.5989 0.0077 0.093 Uiso 0.54 1 calc PR E 2 C23F C 0.4987(12) 0.6333(9) -0.0497(5) 0.079(6) Uiso 0.54 1 d PD E 2 H23Q H 0.4829 0.5927 -0.0471 0.119 Uiso 0.54 1 calc PR E 2 H23R H 0.5644 0.6301 -0.0527 0.119 Uiso 0.54 1 calc PR E 2 H23S H 0.4714 0.6623 -0.0723 0.119 Uiso 0.54 1 calc PR E 2 C237 C 0.3466(5) 0.8681(4) -0.0991(2) 0.045(2) Uani 1 1 d . . . H237 H 0.2937 0.8472 -0.0979 0.054 Uiso 1 1 calc R E . C238 C 0.3093(6) 0.9330(4) -0.0950(3) 0.059(3) Uani 1 1 d . E . H23T H 0.2834 0.9314 -0.0689 0.088 Uiso 1 1 calc R . . H23U H 0.2624 0.9524 -0.1133 0.088 Uiso 1 1 calc R . . H23V H 0.3579 0.9572 -0.1002 0.088 Uiso 1 1 calc R . . C239 C 0.3929(5) 0.8712(4) -0.1390(3) 0.064(3) Uani 1 1 d . E . H23W H 0.4425 0.8943 -0.1422 0.096 Uiso 1 1 calc R . . H23X H 0.3492 0.8921 -0.1585 0.096 Uiso 1 1 calc R . . H23Y H 0.4167 0.8294 -0.1419 0.096 Uiso 1 1 calc R . . C240 C 0.5811(5) 0.8454(3) -0.0039(2) 0.039(2) Uani 1 1 d . . . H240 H 0.6198 0.8117 0.0141 0.047 Uiso 1 1 calc R E . C241 C 0.5296(7) 0.8902(5) 0.0194(3) 0.076(3) Uani 1 1 d . E . H24G H 0.4969 0.9265 0.0021 0.114 Uiso 1 1 calc R . . H24H H 0.5723 0.9030 0.0330 0.114 Uiso 1 1 calc R . . H24I H 0.4868 0.8696 0.0379 0.114 Uiso 1 1 calc R . . C242 C 0.6427(6) 0.8795(4) -0.0334(2) 0.051(2) Uani 1 1 d . E . H24J H 0.6765 0.8517 -0.0486 0.077 Uiso 1 1 calc R . . H24K H 0.6849 0.8941 -0.0205 0.077 Uiso 1 1 calc R . . H24L H 0.6068 0.9148 -0.0503 0.077 Uiso 1 1 calc R . . C243 C 0.1370(4) 0.8090(3) 0.0881(2) 0.0279(16) Uani 1 1 d . . . C244 C 0.1209(5) 0.8593(3) 0.1047(2) 0.0302(17) Uani 1 1 d . E . C245 C 0.0323(4) 0.8849(3) 0.11343(19) 0.0266(16) Uani 1 1 d . . . C246 C -0.0376(4) 0.8599(3) 0.10498(19) 0.0297(17) Uani 1 1 d . E . H246 H -0.0976 0.8772 0.1115 0.036 Uiso 1 1 calc R . . C247 C -0.0240(4) 0.8111(3) 0.08756(18) 0.0256(16) Uani 1 1 d . . . C248 C 0.0657(5) 0.7850(3) 0.07960(18) 0.0278(16) Uani 1 1 d . E . C249 C 0.0094(6) 0.9387(4) 0.1325(2) 0.049(2) Uani 1 1 d . E . H249 H 0.0664 0.9541 0.1332 0.059 Uiso 1 1 calc R . . C250 C -0.0556(7) 0.9912(5) 0.1108(3) 0.074(3) Uiso 1 1 d . . . H25B H -0.0410 0.9965 0.0833 0.111 Uiso 1 1 calc R E . H25C H -0.0516 1.0291 0.1182 0.111 Uiso 1 1 calc R . . H25D H -0.1170 0.9825 0.1168 0.111 Uiso 1 1 calc R . . C251 C -0.0264(7) 0.9153(5) 0.1751(3) 0.085(3) Uiso 1 1 d . . . H25E H -0.0280 0.9471 0.1891 0.128 Uiso 1 1 calc R E . H25F H 0.0138 0.8776 0.1875 0.128 Uiso 1 1 calc R . . H25G H -0.0872 0.9065 0.1754 0.128 Uiso 1 1 calc R . . C252 C -0.1060(5) 0.7903(4) 0.0780(2) 0.0372(19) Uani 1 1 d . E . H252 H -0.0846 0.7571 0.0640 0.045 Uiso 1 1 calc R . . C253 C -0.1671(6) 0.8431(4) 0.0516(2) 0.059(3) Uani 1 1 d . . . H25H H -0.1881 0.8766 0.0645 0.089 Uiso 1 1 calc R E . H25I H -0.2190 0.8279 0.0458 0.089 Uiso 1 1 calc R . . H25J H -0.1330 0.8584 0.0277 0.089 Uiso 1 1 calc R . . C254 C -0.1603(5) 0.7631(4) 0.1144(2) 0.050(2) Uani 1 1 d . . . H25K H -0.1225 0.7270 0.1299 0.074 Uiso 1 1 calc R E . H25L H -0.2133 0.7506 0.1074 0.074 Uiso 1 1 calc R . . H25M H -0.1797 0.7942 0.1293 0.074 Uiso 1 1 calc R . . C255 C 0.2005(5) 0.8820(4) 0.1131(2) 0.0360(18) Uani 1 1 d . . . C256 C 0.2370(5) 0.8585(4) 0.1494(2) 0.045(2) Uani 1 1 d . E . C257 C 0.3150(6) 0.8779(5) 0.1563(3) 0.062(3) Uani 1 1 d . . . H257 H 0.3412 0.8605 0.1803 0.075 Uiso 1 1 calc R E . C258 C 0.3549(6) 0.9206(4) 0.1298(3) 0.049(2) Uani 1 1 d . E . C259 C 0.3174(5) 0.9438(3) 0.0943(2) 0.0373(19) Uani 1 1 d . . . H259 H 0.3442 0.9738 0.0757 0.045 Uiso 1 1 calc R E . C260 C 0.2418(5) 0.9249(3) 0.0848(2) 0.0332(18) Uani 1 1 d . E . C261 C 0.1992(7) 0.8093(5) 0.1796(3) 0.082(3) Uani 0.65 1 d PD E 1 H261 H 0.1353 0.8112 0.1741 0.098 Uiso 0.65 1 calc PR E 1 C262 C 0.2533(10) 0.7427(5) 0.1785(4) 0.067(4) Uiso 0.65 1 d PD E 1 H2FC H 0.3175 0.7413 0.1810 0.100 Uiso 0.65 1 calc PR E 1 H2FD H 0.2448 0.7337 0.1542 0.100 Uiso 0.65 1 calc PR E 1 H2FE H 0.2309 0.7119 0.1998 0.100 Uiso 0.65 1 calc PR E 1 C263 C 0.2007(10) 0.8160(7) 0.2206(3) 0.066(4) Uiso 0.65 1 d PD E 1 H26G H 0.2632 0.8110 0.2274 0.099 Uiso 0.65 1 calc PR E 1 H26H H 0.1713 0.7844 0.2384 0.099 Uiso 0.65 1 calc PR E 1 H26I H 0.1685 0.8570 0.2224 0.099 Uiso 0.65 1 calc PR E 1 C26A C 0.1992(7) 0.8093(5) 0.1796(3) 0.082(3) Uani 0.35 1 d PD E 2 H26J H 0.1528 0.7928 0.1694 0.098 Uiso 0.35 1 calc PR E 2 C26B C 0.2617(15) 0.7575(9) 0.2066(7) 0.067(4) Uiso 0.35 1 d PD E 2 H26K H 0.3233 0.7537 0.1952 0.100 Uiso 0.35 1 calc PR E 2 H26L H 0.2404 0.7183 0.2104 0.100 Uiso 0.35 1 calc PR E 2 H26M H 0.2609 0.7676 0.2314 0.100 Uiso 0.35 1 calc PR E 2 C26C C 0.155(2) 0.8559(13) 0.2049(9) 0.133(15) Uiso 0.35 1 d PD E 2 H26N H 0.2020 0.8740 0.2123 0.199 Uiso 0.35 1 calc PR E 2 H26O H 0.1245 0.8338 0.2279 0.199 Uiso 0.35 1 calc PR E 2 H26P H 0.1111 0.8887 0.1900 0.199 Uiso 0.35 1 calc PR E 2 C264 C 0.4371(6) 0.9422(4) 0.1397(3) 0.056(2) Uani 1 1 d . . . H264 H 0.4640 0.9089 0.1615 0.067 Uiso 1 1 calc R E . C265 C 0.5094(6) 0.9480(5) 0.1086(3) 0.066(3) Uani 1 1 d . E . H26Q H 0.5286 0.9084 0.1017 0.099 Uiso 1 1 calc R . . H26R H 0.5608 0.9597 0.1175 0.099 Uiso 1 1 calc R . . H26S H 0.4863 0.9796 0.0861 0.099 Uiso 1 1 calc R . . C266 C 0.4068(6) 0.9992(4) 0.1553(4) 0.086(4) Uani 1 1 d . E . H26T H 0.4587 1.0097 0.1647 0.129 Uiso 1 1 calc R . . H26U H 0.3615 0.9910 0.1764 0.129 Uiso 1 1 calc R . . H26V H 0.3807 1.0338 0.1349 0.129 Uiso 1 1 calc R . . C267 C 0.2024(5) 0.9523(3) 0.0459(2) 0.0349(18) Uani 1 1 d . . . H267 H 0.1592 0.9260 0.0430 0.042 Uiso 1 1 calc R E . C268 C 0.2708(6) 0.9547(4) 0.0121(2) 0.058(2) Uani 1 1 d . E . H26W H 0.3081 0.9854 0.0118 0.087 Uiso 1 1 calc R . . H26X H 0.2392 0.9661 -0.0117 0.087 Uiso 1 1 calc R . . H26Y H 0.3091 0.9141 0.0145 0.087 Uiso 1 1 calc R . . C269 C 0.1496(6) 1.0171(4) 0.0432(3) 0.052(2) Uani 1 1 d . E . H26Z H 0.1906 1.0444 0.0451 0.078 Uiso 1 1 calc R . . H2FA H 0.1033 1.0163 0.0642 0.078 Uiso 1 1 calc R . . H2FB H 0.1209 1.0323 0.0186 0.078 Uiso 1 1 calc R . . C270 C 0.0844(5) 0.7326(3) 0.0601(2) 0.040(2) Uani 1 1 d . . . C271 C 0.0893(6) 0.7460(4) 0.0194(2) 0.048(2) Uani 1 1 d . E . C272 C 0.1105(7) 0.6982(4) 0.0017(3) 0.064(3) Uani 1 1 d . . . H272 H 0.1125 0.7074 -0.0254 0.076 Uiso 1 1 calc R E . C273 C 0.1289(6) 0.6378(4) 0.0215(2) 0.047(2) Uani 1 1 d . E . C274 C 0.1248(5) 0.6245(4) 0.0610(2) 0.046(2) Uani 1 1 d . . . H274 H 0.1355 0.5827 0.0752 0.056 Uiso 1 1 calc R E . C275 C 0.1049(5) 0.6720(4) 0.0806(2) 0.041(2) Uani 1 1 d . E . C276 C 0.0662(7) 0.8125(4) -0.0066(3) 0.065(3) Uani 1 1 d . . . H276 H 0.0507 0.8417 0.0105 0.078 Uiso 1 1 calc R E . C277 C 0.1437(9) 0.8309(5) -0.0330(3) 0.107(5) Uani 1 1 d . E . H27G H 0.1971 0.8239 -0.0182 0.160 Uiso 1 1 calc R . . H27H H 0.1290 0.8747 -0.0460 0.160 Uiso 1 1 calc R . . H27I H 0.1558 0.8062 -0.0520 0.160 Uiso 1 1 calc R . . C278 C -0.0175(9) 0.8193(5) -0.0300(3) 0.088(4) Uani 1 1 d . E . H27J H -0.0351 0.8625 -0.0437 0.132 Uiso 1 1 calc R . . H27K H -0.0675 0.8060 -0.0125 0.132 Uiso 1 1 calc R . . H27L H -0.0026 0.7936 -0.0485 0.132 Uiso 1 1 calc R . . C279 C 0.1438(8) 0.5860(4) 0.0002(3) 0.070(3) Uani 1 1 d . . . H279 H 0.1768 0.6013 -0.0247 0.084 Uiso 1 1 calc R E . C280 C 0.1996(8) 0.5287(4) 0.0198(3) 0.093(4) Uani 1 1 d . E . H28A H 0.1707 0.5126 0.0448 0.139 Uiso 1 1 calc R . . H28B H 0.2590 0.5369 0.0233 0.139 Uiso 1 1 calc R . . H28C H 0.2066 0.4984 0.0043 0.139 Uiso 1 1 calc R . . C281 C 0.0521(9) 0.5763(5) -0.0097(3) 0.100(4) Uani 1 1 d . E . H28D H 0.0617 0.5488 -0.0271 0.150 Uiso 1 1 calc R . . H28E H 0.0170 0.6162 -0.0222 0.150 Uiso 1 1 calc R . . H28F H 0.0194 0.5579 0.0138 0.150 Uiso 1 1 calc R . . C282 C 0.1014(5) 0.6543(3) 0.1247(2) 0.040(2) Uani 1 1 d . . . H282 H 0.0881 0.6934 0.1335 0.048 Uiso 1 1 calc R E . C283 C 0.1919(5) 0.6171(4) 0.1413(3) 0.062(3) Uani 1 1 d . E . H28G H 0.2035 0.5765 0.1356 0.093 Uiso 1 1 calc R . . H28H H 0.1886 0.6121 0.1691 0.093 Uiso 1 1 calc R . . H28I H 0.2409 0.6394 0.1297 0.093 Uiso 1 1 calc R . . C284 C 0.0267(5) 0.6183(4) 0.1412(3) 0.052(2) Uani 1 1 d . E . H28J H -0.0312 0.6432 0.1326 0.078 Uiso 1 1 calc R . . H28K H 0.0258 0.6084 0.1692 0.078 Uiso 1 1 calc R . . H28L H 0.0371 0.5801 0.1325 0.078 Uiso 1 1 calc R . . C301 C 0.7883(19) 0.8490(12) 0.5585(8) 0.124(10) Uiso 0.50 1 d PD F 1 H30A H 0.8152 0.8232 0.5410 0.186 Uiso 0.50 1 calc PR F 1 H30B H 0.7328 0.8355 0.5710 0.186 Uiso 0.50 1 calc PR F 1 H30C H 0.8309 0.8453 0.5780 0.186 Uiso 0.50 1 calc PR F 1 C302 C 0.766(2) 0.9193(14) 0.5349(9) 0.149(12) Uiso 0.50 1 d PD F 1 H30D H 0.7333 0.9241 0.5116 0.179 Uiso 0.50 1 calc PR F 1 H30E H 0.7317 0.9465 0.5508 0.179 Uiso 0.50 1 calc PR F 1 O303 O 0.8588(15) 0.9287(10) 0.5261(6) 0.149(8) Uiso 0.50 1 d P F 1 C304 C 0.837(2) 0.9961(18) 0.4995(12) 0.193(16) Uiso 0.50 1 d PD F 1 H30F H 0.8047 1.0270 0.5133 0.231 Uiso 0.50 1 calc PR F 1 H30G H 0.8048 0.9983 0.4765 0.231 Uiso 0.50 1 calc PR F 1 C305 C 0.942(3) 0.999(2) 0.4908(14) 0.26(2) Uiso 0.50 1 d PD F 1 H30H H 0.9708 0.9912 0.5150 0.383 Uiso 0.50 1 calc PR F 1 H30I H 0.9489 1.0395 0.4748 0.383 Uiso 0.50 1 calc PR F 1 H30J H 0.9695 0.9670 0.4772 0.383 Uiso 0.50 1 calc PR F 1 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.0447(4) 0.0265(3) 0.0697(4) 0.0126(3) 0.0115(3) 0.0009(3) Sn2 0.0459(4) 0.0269(3) 0.0504(4) 0.0005(3) 0.0116(3) -0.0039(3) C1 0.024(4) 0.023(4) 0.041(5) 0.004(3) 0.000(3) 0.006(3) C2 0.027(4) 0.028(4) 0.026(4) 0.008(3) -0.002(3) 0.001(3) C3 0.018(4) 0.035(4) 0.033(4) -0.002(3) -0.008(3) 0.010(3) C4 0.021(4) 0.027(4) 0.036(4) -0.002(3) -0.003(3) 0.000(3) C5 0.017(3) 0.022(4) 0.035(4) 0.000(3) -0.005(3) 0.000(3) C6 0.019(4) 0.029(4) 0.032(4) -0.004(3) -0.002(3) 0.005(3) C7 0.030(4) 0.041(4) 0.024(4) -0.004(3) 0.000(3) -0.009(3) C8 0.050(5) 0.036(4) 0.034(5) -0.012(4) 0.004(4) -0.003(4) C9 0.043(5) 0.052(5) 0.034(5) -0.014(4) -0.009(4) -0.008(4) C10 0.027(4) 0.019(3) 0.036(4) -0.001(3) 0.006(3) -0.001(3) C11 0.038(5) 0.045(5) 0.054(5) -0.020(4) 0.022(4) -0.009(4) C12 0.050(5) 0.032(4) 0.037(5) 0.003(4) 0.012(4) 0.003(4) C13 0.050(5) 0.039(5) 0.026(4) 0.004(4) 0.003(4) -0.004(4) C14 0.047(5) 0.032(4) 0.031(4) -0.008(3) 0.005(4) -0.015(4) C15 0.049(5) 0.040(4) 0.025(4) -0.010(4) 0.008(4) -0.021(4) C16 0.070(6) 0.026(4) 0.036(5) -0.004(4) 0.013(4) -0.015(4) C17 0.100(9) 0.060(6) 0.030(5) 0.014(5) -0.014(5) 0.018(6) C18 0.057(6) 0.093(8) 0.035(5) 0.011(5) -0.003(5) 0.023(6) C19 0.032(4) 0.022(4) 0.026(4) -0.003(3) 0.010(3) -0.004(3) C20 0.045(5) 0.041(5) 0.050(5) -0.014(4) -0.005(4) 0.001(4) C21 0.038(5) 0.040(5) 0.043(5) -0.007(4) 0.013(4) -0.002(4) C22 0.093(7) 0.045(5) 0.029(5) -0.003(4) 0.008(5) -0.039(5) C22A 0.093(7) 0.045(5) 0.029(5) -0.003(4) 0.008(5) -0.039(5) C28 0.024(4) 0.017(3) 0.038(4) 0.005(3) -0.006(3) -0.001(3) C29 0.026(4) 0.020(4) 0.053(5) -0.007(3) -0.003(4) 0.000(3) C30 0.033(4) 0.027(4) 0.055(5) -0.006(4) -0.010(4) 0.002(3) C31 0.045(5) 0.026(4) 0.045(5) -0.005(4) -0.005(4) 0.001(4) C32 0.031(4) 0.032(4) 0.049(5) -0.010(4) -0.005(4) 0.002(4) C33 0.021(4) 0.028(4) 0.039(5) 0.004(3) 0.003(3) 0.003(3) C34 0.029(4) 0.026(4) 0.062(6) -0.012(4) -0.013(4) 0.005(3) C35 0.054(6) 0.041(5) 0.067(6) -0.012(5) -0.021(5) 0.010(4) C36 0.041(5) 0.041(5) 0.110(8) -0.011(5) -0.020(5) -0.011(4) C37 0.044(5) 0.036(5) 0.078(7) -0.028(5) -0.019(5) 0.014(4) C37A 0.044(5) 0.036(5) 0.078(7) -0.028(5) -0.019(5) 0.014(4) C40 0.023(4) 0.028(4) 0.041(5) -0.001(3) -0.001(3) 0.001(3) C41 0.034(5) 0.038(5) 0.056(6) 0.007(4) -0.006(4) -0.003(4) C42 0.030(4) 0.052(5) 0.042(5) 0.005(4) 0.002(4) 0.002(4) C43 0.028(4) 0.024(4) 0.021(4) 0.002(3) 0.011(3) 0.002(3) C44 0.021(4) 0.022(4) 0.026(4) 0.004(3) 0.014(3) -0.005(3) C45 0.027(4) 0.028(4) 0.051(5) -0.007(4) 0.014(4) -0.003(3) C46 0.030(4) 0.028(4) 0.043(5) -0.001(4) 0.017(4) -0.001(3) C47 0.020(4) 0.033(4) 0.025(4) -0.001(3) 0.013(3) 0.005(3) C48 0.030(4) 0.027(4) 0.021(4) 0.005(3) 0.005(3) 0.004(3) C49 0.029(5) 0.031(5) 0.109(8) -0.021(5) 0.010(5) 0.007(4) C50 0.039(5) 0.021(4) 0.148(10) 0.027(5) 0.017(6) 0.003(4) C51 0.049(6) 0.066(7) 0.155(11) -0.071(8) 0.037(7) -0.017(5) C52 0.019(4) 0.053(5) 0.027(4) -0.008(4) 0.005(3) 0.000(3) C53 0.015(4) 0.077(6) 0.044(5) 0.008(5) 0.006(4) -0.008(4) C54 0.036(5) 0.087(7) 0.038(5) -0.003(5) -0.007(4) 0.003(5) C55 0.016(3) 0.006(3) 0.040(4) 0.004(3) 0.013(3) 0.006(3) C56 0.035(4) 0.025(4) 0.036(5) 0.003(3) 0.009(4) 0.004(3) C57 0.041(5) 0.028(4) 0.037(5) -0.004(3) -0.009(4) 0.000(4) C58 0.025(4) 0.028(4) 0.052(5) 0.001(4) 0.008(4) -0.010(3) C59 0.027(4) 0.036(4) 0.035(5) 0.003(4) 0.018(4) -0.005(3) C60 0.020(4) 0.018(3) 0.041(5) 0.003(3) 0.009(3) 0.008(3) C61 0.038(5) 0.044(5) 0.034(5) -0.007(4) -0.001(4) 0.009(4) C62 0.048(5) 0.055(5) 0.041(5) 0.013(4) 0.011(4) 0.006(4) C63 0.059(6) 0.084(7) 0.043(6) -0.017(5) 0.000(5) 0.002(5) C64 0.033(5) 0.046(5) 0.064(6) 0.000(4) 0.014(4) -0.013(4) C64A 0.033(5) 0.046(5) 0.064(6) 0.000(4) 0.014(4) -0.013(4) C67 0.030(4) 0.036(4) 0.029(4) -0.003(3) 0.012(3) 0.000(3) C68 0.039(5) 0.048(5) 0.051(5) -0.016(4) 0.003(4) 0.011(4) C69 0.052(5) 0.043(5) 0.037(5) 0.003(4) -0.002(4) 0.002(4) C70 0.024(4) 0.028(4) 0.048(5) -0.006(4) 0.013(4) 0.005(3) C71 0.038(5) 0.043(5) 0.060(6) 0.002(4) 0.029(4) 0.004(4) C72 0.083(8) 0.046(6) 0.086(8) -0.012(6) 0.054(6) 0.014(5) C73 0.073(7) 0.050(6) 0.090(8) -0.004(6) 0.047(6) 0.021(5) C74 0.040(5) 0.042(5) 0.068(7) 0.017(5) 0.010(5) 0.020(4) C75 0.023(4) 0.034(4) 0.045(5) 0.007(4) 0.013(4) 0.007(3) C76 0.077(7) 0.034(5) 0.030(5) -0.009(4) 0.027(4) -0.002(4) C77 0.065(7) 0.084(8) 0.066(7) -0.004(6) 0.009(6) 0.005(6) C78 0.070(7) 0.097(8) 0.045(6) 0.000(6) 0.022(5) -0.028(6) C82 0.030(4) 0.049(5) 0.041(5) 0.009(4) -0.009(4) 0.005(4) C83 0.059(6) 0.068(6) 0.061(6) -0.014(5) 0.019(5) -0.021(5) C84 0.063(7) 0.149(11) 0.064(7) 0.041(7) -0.013(6) -0.047(7) Sn3 0.0175(2) 0.0244(2) 0.0276(3) -0.0128(2) -0.0004(2) -0.00056(19) Sn4 0.0190(2) 0.0247(2) 0.0268(3) -0.0128(2) -0.0005(2) -0.00050(19) C101 0.016(3) 0.019(3) 0.027(4) -0.014(3) 0.003(3) 0.001(3) C102 0.011(3) 0.046(4) 0.035(4) -0.027(4) 0.002(3) -0.001(3) C103 0.012(4) 0.087(6) 0.052(5) -0.056(5) 0.005(3) -0.001(4) C104 0.019(4) 0.115(8) 0.044(5) -0.054(5) -0.009(4) 0.010(5) C105 0.019(4) 0.053(5) 0.026(4) -0.014(4) -0.005(3) 0.006(3) C106 0.017(3) 0.018(3) 0.028(4) -0.010(3) -0.001(3) 0.008(3) C107 0.023(5) 0.183(12) 0.103(8) -0.116(9) 0.016(5) -0.036(6) C108 0.041(6) 0.174(12) 0.128(10) -0.124(10) 0.033(6) -0.046(7) C109 0.019(5) 0.285(18) 0.241(16) -0.244(16) -0.050(8) 0.043(8) C110 0.027(4) 0.081(6) 0.016(4) -0.010(4) 0.000(3) 0.011(4) C111 0.073(8) 0.158(12) 0.032(6) 0.001(6) -0.007(5) 0.050(8) C112 0.040(5) 0.100(8) 0.054(6) -0.050(6) 0.010(4) 0.003(5) C113 0.014(3) 0.040(4) 0.031(4) -0.023(3) 0.006(3) -0.009(3) C114 0.016(3) 0.037(4) 0.035(4) -0.025(3) 0.000(3) -0.003(3) C115 0.020(4) 0.031(4) 0.047(5) -0.022(4) 0.006(3) -0.003(3) C116 0.017(4) 0.042(5) 0.049(5) -0.024(4) 0.015(3) -0.012(3) C117 0.026(4) 0.031(4) 0.043(5) -0.014(4) 0.018(3) -0.009(3) C118 0.021(4) 0.029(4) 0.066(6) -0.025(4) 0.008(4) -0.006(3) C119 0.014(3) 0.044(4) 0.028(4) -0.012(3) 0.000(3) 0.003(3) C120 0.027(4) 0.046(5) 0.050(5) 0.005(4) -0.001(4) -0.006(4) C121 0.021(4) 0.036(4) 0.048(5) -0.020(4) -0.004(3) 0.003(3) C122 0.040(5) 0.038(5) 0.054(5) -0.022(4) 0.015(4) -0.015(4) C123 0.060(6) 0.048(5) 0.049(6) -0.012(4) 0.030(5) -0.020(5) C124 0.023(4) 0.066(6) 0.077(7) -0.031(5) 0.023(4) -0.015(4) C125 0.022(4) 0.028(4) 0.072(6) -0.025(4) 0.021(4) -0.002(3) C126 0.049(5) 0.023(4) 0.081(7) -0.011(4) 0.022(5) 0.007(4) C127 0.046(5) 0.056(6) 0.131(9) -0.068(6) 0.034(6) -0.021(5) C128 0.016(3) 0.026(4) 0.023(4) -0.010(3) 0.010(3) -0.011(3) C129 0.016(3) 0.023(4) 0.030(4) -0.012(3) 0.002(3) 0.000(3) C130 0.013(3) 0.048(5) 0.044(5) -0.027(4) 0.003(3) -0.008(3) C131 0.017(4) 0.056(5) 0.060(6) -0.045(5) 0.011(4) -0.005(4) C132 0.043(5) 0.041(5) 0.068(6) -0.037(4) 0.037(4) -0.034(4) C133 0.037(4) 0.026(4) 0.033(4) -0.012(3) 0.018(3) -0.006(3) C134 0.016(4) 0.025(4) 0.042(5) -0.006(3) -0.002(3) 0.000(3) C135 0.058(6) 0.029(4) 0.047(5) -0.001(4) -0.001(4) 0.012(4) C136 0.030(4) 0.031(4) 0.064(6) -0.023(4) 0.013(4) 0.001(3) C137 0.035(5) 0.116(8) 0.087(7) -0.089(7) 0.035(5) -0.048(6) C138 0.030(5) 0.167(12) 0.094(8) -0.092(9) 0.003(5) -0.032(7) C139 0.038(5) 0.133(10) 0.107(9) -0.076(8) 0.040(5) -0.053(6) C140 0.055(5) 0.020(4) 0.051(5) 0.004(4) 0.022(4) 0.002(4) C141 0.055(6) 0.019(4) 0.082(7) -0.014(4) 0.023(5) 0.004(4) C143 0.010(3) 0.035(4) 0.030(4) -0.016(3) -0.002(3) 0.003(3) C144 0.021(4) 0.048(4) 0.021(4) -0.020(3) 0.006(3) -0.004(3) C145 0.021(4) 0.043(4) 0.035(4) -0.017(4) 0.006(3) -0.002(3) C146 0.027(4) 0.065(6) 0.047(5) -0.042(4) 0.002(4) -0.007(4) C147 0.017(4) 0.045(5) 0.050(5) -0.029(4) -0.001(3) -0.003(3) C148 0.016(4) 0.032(4) 0.041(4) -0.020(3) 0.001(3) 0.003(3) C149 0.030(4) 0.068(6) 0.038(5) -0.042(4) -0.011(4) 0.010(4) C150 0.053(6) 0.108(8) 0.042(6) -0.033(6) -0.013(5) 0.007(6) C151 0.035(5) 0.071(6) 0.076(7) -0.039(5) -0.025(5) 0.001(5) C152 0.029(4) 0.052(5) 0.052(5) -0.043(4) 0.006(4) -0.009(4) C153 0.033(5) 0.096(7) 0.074(7) -0.063(6) -0.002(5) 0.007(5) C154 0.032(5) 0.054(6) 0.109(8) -0.057(6) 0.015(5) -0.008(4) C155 0.013(3) 0.036(4) 0.023(4) -0.015(3) -0.002(3) 0.006(3) C156 0.019(4) 0.029(4) 0.028(4) -0.017(3) -0.012(3) 0.008(3) C157 0.019(4) 0.047(5) 0.016(4) -0.008(3) 0.000(3) 0.009(3) C158 0.029(4) 0.031(4) 0.021(4) -0.006(3) 0.001(3) 0.016(3) C159 0.031(4) 0.031(4) 0.015(4) -0.002(3) -0.001(3) 0.016(3) C160 0.021(4) 0.044(5) 0.019(4) -0.012(3) 0.002(3) 0.009(3) C161 0.020(4) 0.038(4) 0.051(5) -0.030(4) 0.010(3) -0.006(3) C162 0.042(5) 0.040(4) 0.029(4) -0.010(4) 0.004(4) -0.019(4) C163 0.017(4) 0.077(6) 0.080(7) -0.044(5) 0.008(4) -0.015(4) C164 0.038(5) 0.036(4) 0.034(5) -0.001(4) 0.017(4) 0.010(4) C165 0.062(6) 0.026(4) 0.032(5) 0.003(3) 0.018(4) 0.016(4) C166 0.034(5) 0.054(6) 0.062(6) 0.004(5) 0.012(4) 0.023(4) C167 0.023(4) 0.043(5) 0.030(4) -0.007(4) 0.007(3) 0.007(3) C168 0.040(5) 0.035(4) 0.044(5) 0.007(4) 0.017(4) 0.004(4) C169 0.040(5) 0.094(7) 0.029(5) -0.006(5) 0.008(4) 0.014(5) C170 0.015(3) 0.018(3) 0.034(4) -0.020(3) 0.002(3) 0.002(3) C171 0.020(4) 0.023(4) 0.032(4) -0.017(3) -0.002(3) 0.002(3) C172 0.014(3) 0.027(4) 0.032(4) -0.012(3) 0.011(3) -0.007(3) C173 0.017(3) 0.024(4) 0.029(4) -0.008(3) 0.006(3) -0.003(3) C174 0.020(4) 0.015(3) 0.038(4) -0.003(3) 0.004(3) 0.003(3) C175 0.018(4) 0.014(3) 0.044(5) -0.011(3) 0.003(3) 0.000(3) C176 0.023(4) 0.041(4) 0.029(4) -0.009(3) 0.003(3) 0.000(3) C177 0.052(5) 0.036(5) 0.030(4) 0.006(4) 0.003(4) 0.002(4) C178 0.035(4) 0.053(5) 0.027(4) -0.013(4) 0.003(3) 0.005(4) C179 0.015(3) 0.036(4) 0.024(4) -0.004(3) 0.000(3) 0.007(3) C180 0.018(4) 0.039(4) 0.034(4) -0.007(3) 0.002(3) -0.006(3) C181 0.020(4) 0.035(4) 0.046(5) -0.001(4) 0.005(3) 0.009(3) C182 0.024(4) 0.023(4) 0.054(5) -0.017(4) 0.009(4) -0.004(3) C183 0.037(5) 0.035(5) 0.075(6) -0.018(4) 0.031(4) -0.007(4) C184 0.038(5) 0.025(4) 0.076(6) -0.012(4) 0.011(4) -0.007(4) Sn5 0.0181(4) 0.0439(5) 0.0393(5) -0.0136(4) -0.0008(3) 0.0029(3) Sn6 0.0188(4) 0.0393(5) 0.0374(5) -0.0136(4) -0.0031(3) 0.0059(4) Sn5A 0.0188(9) 0.0460(13) 0.0492(14) -0.0229(12) 0.0066(9) 0.0027(9) Sn6A 0.0191(9) 0.0722(14) 0.0358(11) -0.0254(10) 0.0017(8) 0.0103(9) C201 0.021(4) 0.041(5) 0.065(6) 0.015(4) 0.012(4) 0.008(4) C202 0.031(4) 0.026(4) 0.060(6) 0.008(4) 0.016(4) -0.005(3) C203 0.021(4) 0.027(4) 0.043(5) -0.001(3) 0.001(3) -0.001(3) C204 0.020(4) 0.039(4) 0.027(4) -0.008(3) 0.006(3) 0.000(3) C205 0.021(4) 0.037(4) 0.033(4) -0.002(3) -0.003(3) -0.003(3) C206 0.025(4) 0.028(4) 0.064(6) 0.012(4) 0.005(4) -0.011(3) C207 0.027(4) 0.033(4) 0.032(4) 0.004(3) 0.007(3) 0.001(3) C208 0.034(5) 0.037(5) 0.057(6) 0.004(4) -0.003(4) 0.008(4) C209 0.049(5) 0.066(6) 0.035(5) -0.010(4) 0.004(4) -0.013(5) C210 0.039(5) 0.052(5) 0.042(5) 0.007(4) -0.010(4) 0.005(4) C211 0.081(8) 0.099(8) 0.034(5) -0.018(5) -0.009(5) 0.011(6) C212 0.042(5) 0.069(7) 0.076(7) 0.009(6) 0.017(5) -0.003(5) C213 0.033(5) 0.036(5) 0.056(6) 0.019(4) 0.018(4) 0.002(4) C214 0.039(5) 0.035(5) 0.070(7) 0.002(5) 0.032(5) 0.021(4) C215 0.047(5) 0.039(5) 0.069(7) 0.017(5) 0.034(5) 0.021(4) C216 0.039(5) 0.054(6) 0.060(7) 0.013(5) 0.015(5) 0.011(5) C217 0.022(4) 0.046(5) 0.092(8) 0.029(5) 0.017(5) -0.005(4) C218 0.038(5) 0.038(5) 0.072(7) 0.000(5) 0.016(5) 0.003(4) C219 0.063(6) 0.021(4) 0.087(8) 0.003(5) 0.055(6) 0.008(4) C221 0.129(10) 0.061(7) 0.046(6) -0.010(5) 0.034(7) -0.041(7) C222 0.042(5) 0.072(7) 0.058(6) 0.031(5) 0.024(5) 0.011(5) C223 0.093(9) 0.082(8) 0.081(8) 0.009(7) 0.050(7) 0.015(7) C224 0.047(5) 0.058(6) 0.058(6) 0.008(5) 0.007(5) -0.009(5) C225 0.035(5) 0.056(6) 0.093(8) 0.016(6) 0.019(5) -0.012(5) C226 0.040(6) 0.087(8) 0.072(7) 0.023(6) 0.006(5) -0.006(5) C227 0.044(6) 0.055(6) 0.127(10) -0.015(6) 0.001(6) -0.015(5) C228 0.022(4) 0.038(5) 0.064(6) 0.012(4) 0.000(4) 0.000(4) C229 0.037(5) 0.042(5) 0.142(10) -0.008(6) -0.033(6) -0.001(4) C230 0.039(5) 0.035(5) 0.120(9) -0.009(5) -0.035(6) -0.009(4) C231 0.030(4) 0.035(4) 0.050(5) 0.000(4) -0.003(4) -0.006(4) C232 0.023(4) 0.029(4) 0.046(5) 0.000(4) 0.006(3) -0.005(3) C233 0.016(4) 0.037(4) 0.039(5) 0.009(4) 0.002(3) -0.002(3) C237 0.026(4) 0.050(5) 0.053(6) -0.004(4) -0.002(4) -0.004(4) C238 0.054(6) 0.048(5) 0.068(6) -0.009(5) -0.032(5) 0.016(4) C239 0.026(5) 0.071(6) 0.076(7) 0.003(5) 0.000(5) 0.007(4) C240 0.033(4) 0.034(4) 0.038(5) 0.000(4) 0.006(4) 0.009(4) C241 0.060(7) 0.108(9) 0.061(7) -0.037(6) -0.007(5) 0.007(6) C242 0.051(5) 0.036(5) 0.067(6) -0.012(4) -0.004(5) -0.009(4) C243 0.025(4) 0.023(4) 0.036(4) -0.010(3) -0.005(3) 0.000(3) C244 0.026(4) 0.037(4) 0.030(4) -0.006(3) -0.002(3) -0.017(3) C245 0.028(4) 0.030(4) 0.026(4) -0.015(3) 0.010(3) -0.011(3) C246 0.018(4) 0.033(4) 0.032(4) -0.003(3) 0.004(3) 0.000(3) C247 0.027(4) 0.027(4) 0.021(4) 0.000(3) -0.003(3) -0.007(3) C248 0.035(4) 0.031(4) 0.016(4) -0.007(3) 0.013(3) -0.009(3) C249 0.045(5) 0.043(5) 0.068(6) -0.030(5) 0.033(4) -0.020(4) C252 0.038(5) 0.048(5) 0.032(4) -0.013(4) 0.007(4) -0.023(4) C253 0.047(5) 0.081(7) 0.053(6) -0.007(5) -0.021(5) -0.017(5) C254 0.038(5) 0.054(5) 0.061(6) -0.015(5) 0.015(4) -0.026(4) C255 0.032(4) 0.050(5) 0.028(4) -0.013(4) -0.001(3) -0.009(4) C256 0.040(5) 0.066(6) 0.030(5) -0.008(4) 0.000(4) -0.018(4) C257 0.047(6) 0.104(8) 0.041(5) -0.008(5) -0.013(4) -0.032(6) C258 0.043(5) 0.065(6) 0.052(6) -0.029(5) -0.009(4) -0.018(5) C259 0.032(4) 0.036(4) 0.047(5) -0.016(4) 0.012(4) -0.014(4) C260 0.028(4) 0.035(4) 0.042(5) -0.023(4) 0.006(3) -0.005(3) C261 0.066(7) 0.121(10) 0.062(7) -0.005(7) 0.003(6) -0.053(7) C26A 0.066(7) 0.121(10) 0.062(7) -0.005(7) 0.003(6) -0.053(7) C264 0.042(5) 0.067(6) 0.069(7) -0.026(5) -0.014(5) -0.015(5) C265 0.045(6) 0.088(7) 0.070(7) -0.011(6) -0.018(5) -0.030(5) C266 0.044(6) 0.058(6) 0.171(12) -0.056(7) -0.050(7) 0.011(5) C267 0.033(4) 0.040(4) 0.038(5) -0.019(4) 0.013(4) -0.016(4) C268 0.055(6) 0.070(6) 0.051(6) -0.023(5) 0.019(5) -0.016(5) C269 0.049(5) 0.046(5) 0.065(6) -0.022(5) 0.003(5) -0.008(4) C270 0.046(5) 0.029(4) 0.053(5) -0.024(4) 0.012(4) -0.010(4) C271 0.072(6) 0.038(5) 0.040(5) -0.025(4) 0.015(4) -0.010(4) C272 0.104(8) 0.036(5) 0.051(6) -0.019(4) 0.026(5) -0.016(5) C273 0.057(6) 0.041(5) 0.051(6) -0.024(4) 0.015(4) -0.014(4) C274 0.051(5) 0.028(4) 0.056(6) -0.003(4) 0.003(4) -0.010(4) C275 0.035(4) 0.044(5) 0.050(5) -0.024(4) 0.013(4) -0.016(4) C276 0.115(9) 0.031(5) 0.043(6) -0.012(4) 0.026(6) -0.012(5) C277 0.159(13) 0.063(7) 0.102(9) -0.021(7) 0.059(9) -0.060(8) C278 0.153(12) 0.065(7) 0.038(6) -0.015(5) -0.011(7) 0.007(7) C279 0.112(9) 0.040(5) 0.066(7) -0.031(5) 0.008(6) -0.018(6) C280 0.141(11) 0.046(6) 0.094(9) -0.039(6) -0.006(8) 0.006(7) C281 0.158(13) 0.070(8) 0.097(9) -0.050(7) 0.001(9) -0.047(8) C282 0.035(4) 0.031(4) 0.055(5) -0.015(4) 0.011(4) -0.005(4) C283 0.033(5) 0.057(6) 0.093(8) -0.016(5) -0.006(5) -0.001(4) C284 0.042(5) 0.047(5) 0.061(6) -0.010(5) 0.003(4) 0.001(4) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C1 2.202(7) . ? Sn1 Sn2 2.7349(8) . ? Sn2 C43 2.206(7) . ? C1 C2 1.396(10) . ? C1 C6 1.401(10) . ? C2 C3 1.408(10) . ? C2 C13 1.517(10) . ? C3 C4 1.395(10) . ? C3 C7 1.521(10) . ? C4 C5 1.381(9) . ? C4 H4 0.9500 . ? C5 C6 1.412(9) . ? C5 C10 1.528(9) . ? C6 C28 1.525(9) . ? C7 C9 1.509(10) . ? C7 C8 1.558(9) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.516(10) . ? C10 C12 1.541(9) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C18 1.388(11) . ? C13 C14 1.403(11) . ? C14 C15 1.406(10) . ? C14 C19 1.517(10) . ? C15 C16 1.358(11) . ? C15 H15 0.9500 . ? C16 C17 1.375(13) . ? C16 C22 1.544(11) . ? C17 C18 1.424(13) . ? C17 H17 0.9500 . ? C18 C25D 1.545(14) . ? C18 C25 1.558(15) . ? C19 C20 1.533(10) . ? C19 C21 1.538(9) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.512(14) . ? C22 C23 1.660(17) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C23A H23D 0.9800 . ? C23A H23E 0.9800 . ? C23A H23F 0.9800 . ? C24A H24D 0.9800 . ? C24A H24E 0.9800 . ? C24A H24F 0.9800 . ? C25 C27 1.501(12) . ? C25 C26 1.505(12) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C25D C27D 1.497(12) . ? C25D C26D 1.499(12) . ? C25D H25A 1.0000 . ? C26D H26D 0.9800 . ? C26D H26E 0.9800 . ? C26D H26F 0.9800 . ? C27D H27D 0.9800 . ? C27D H27E 0.9800 . ? C27D H27F 0.9800 . ? C28 C33 1.393(10) . ? C28 C29 1.406(9) . ? C29 C30 1.407(10) . ? C29 C34 1.519(10) . ? C30 C31 1.392(10) . ? C30 H30 0.9500 . ? C31 C32 1.386(10) . ? C31 C37 1.513(10) . ? C32 C33 1.402(10) . ? C32 H32 0.9500 . ? C33 C40 1.513(9) . ? C34 C35 1.517(10) . ? C34 C36 1.537(11) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C39 1.465(10) . ? C37 C38 1.488(10) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C38A H38D 0.9800 . ? C38A H38E 0.9800 . ? C38A H38F 0.9800 . ? C39A H39D 0.9800 . ? C39A H39E 0.9800 . ? C39A H39F 0.9800 . ? C40 C42 1.528(10) . ? C40 C41 1.531(10) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? C43 C44 1.408(9) . ? C43 C48 1.425(9) . ? C44 C45 1.392(9) . ? C44 C55 1.498(9) . ? C45 C46 1.396(10) . ? C45 C49 1.503(10) . ? C46 C47 1.367(9) . ? C46 H46 0.9500 . ? C47 C48 1.400(10) . ? C47 C52 1.529(9) . ? C48 C70 1.483(9) . ? C49 C51 1.492(13) . ? C49 C50 1.549(12) . ? C49 H49 1.0000 . ? C50 H50A 0.9800 . ? C50 H50B 0.9800 . ? C50 H50C 0.9800 . ? C51 H51A 0.9800 . ? C51 H51B 0.9800 . ? C51 H51C 0.9800 . ? C52 C54 1.526(10) . ? C52 C53 1.538(10) . ? C52 H52 1.0000 . ? C53 H53A 0.9800 . ? C53 H53B 0.9800 . ? C53 H53C 0.9800 . ? C54 H54A 0.9800 . ? C54 H54B 0.9800 . ? C54 H54C 0.9800 . ? C55 C56 1.407(10) . ? C55 C60 1.420(9) . ? C56 C57 1.407(10) . ? C56 C61 1.499(10) . ? C57 C58 1.375(10) . ? C57 H57 0.9500 . ? C58 C59 1.404(10) . ? C58 C64 1.532(10) . ? C59 C60 1.384(9) . ? C59 H59 0.9500 . ? C60 C67 1.516(10) . ? C61 C63 1.526(11) . ? C61 C62 1.531(10) . ? C61 H61 1.0000 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 H63A 0.9800 . ? C63 H63B 0.9800 . ? C63 H63C 0.9800 . ? C64 C65 1.517(10) . ? C64 C66 1.535(9) . ? C64 H64 1.0000 . ? C65 H65A 0.9800 . ? C65 H65B 0.9800 . ? C65 H65C 0.9800 . ? C66 H66A 0.9800 . ? C66 H66B 0.9800 . ? C66 H66C 0.9800 . ? C65A H65D 0.9800 . ? C65A H65E 0.9800 . ? C65A H65F 0.9800 . ? C66A H66D 0.9800 . ? C66A H66E 0.9800 . ? C66A H66F 0.9800 . ? C67 C68 1.498(10) . ? C67 C69 1.537(10) . ? C67 H67 1.0000 . ? C68 H68A 0.9800 . ? C68 H68B 0.9800 . ? C68 H68C 0.9800 . ? C69 H69A 0.9800 . ? C69 H69B 0.9800 . ? C69 H69C 0.9800 . ? C70 C75 1.385(10) . ? C70 C71 1.430(11) . ? C71 C72 1.387(11) . ? C71 C76 1.525(11) . ? C72 C73 1.374(13) . ? C72 H72 0.9500 . ? C73 C74 1.381(13) . ? C73 C79 1.561(13) . ? C73 C79A 1.584(14) . ? C74 C75 1.407(10) . ? C74 H74 0.9500 . ? C75 C82 1.516(11) . ? C76 C77 1.516(13) . ? C76 C78 1.523(11) . ? C76 H76 1.0000 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 H78A 0.9800 . ? C78 H78B 0.9800 . ? C78 H78C 0.9800 . ? C79 C81 1.460(9) . ? C79 C80 1.465(9) . ? C79 H79 1.0000 . ? C80 H80A 0.9800 . ? C80 H80B 0.9800 . ? C80 H80C 0.9800 . ? C81 H81A 0.9800 . ? C81 H81B 0.9800 . ? C81 H81C 0.9800 . ? C79A C80A 1.499(10) . ? C79A C81A 1.519(10) . ? C79A H79A 1.0000 . ? C80A H80D 0.9800 . ? C80A H80E 0.9800 . ? C80A H80F 0.9800 . ? C81A H81D 0.9800 . ? C81A H81E 0.9800 . ? C81A H81F 0.9800 . ? C82 C83 1.491(11) . ? C82 C84 1.560(12) . ? C82 H82 1.0000 . ? C83 H83A 0.9800 . ? C83 H83B 0.9800 . ? C83 H83C 0.9800 . ? C84 H84A 0.9800 . ? C84 H84B 0.9800 . ? C84 H84C 0.9800 . ? Sn3 C101 2.201(6) . ? Sn3 Sn4 2.7159(6) . ? Sn4 C143 2.196(6) . ? C101 C106 1.402(9) . ? C101 C102 1.407(9) . ? C102 C103 1.384(9) . ? C102 C113 1.502(9) . ? C103 C104 1.410(11) . ? C103 C107 1.518(10) . ? C104 C105 1.372(10) . ? C104 H104 0.9500 . ? C105 C106 1.380(9) . ? C105 C110 1.535(10) . ? C106 C128 1.503(8) . ? C107 C109 1.535(17) . ? C107 C108 1.556(13) . ? C107 H107 1.0000 . ? C108 H10A 0.9800 . ? C108 H10B 0.9800 . ? C108 H10C 0.9800 . ? C109 H10D 0.9800 . ? C109 H10E 0.9800 . ? C109 H10F 0.9800 . ? C110 C112 1.534(11) . ? C110 C111 1.553(11) . ? C110 H110 1.0000 . ? C111 H11D 0.9800 . ? C111 H11E 0.9800 . ? C111 H11F 0.9800 . ? C112 H11G 0.9800 . ? C112 H11H 0.9800 . ? C112 H11I 0.9800 . ? C113 C114 1.402(9) . ? C113 C118 1.409(10) . ? C114 C115 1.389(9) . ? C114 C119 1.501(10) . ? C115 C116 1.396(10) . ? C115 H115 0.9500 . ? C116 C117 1.365(9) . ? C116 C122 1.526(10) . ? C117 C118 1.387(10) . ? C117 H117 0.9500 . ? C118 C125 1.541(9) . ? C119 C120 1.535(10) . ? C119 C121 1.542(9) . ? C119 H119 1.0000 . ? C120 H12D 0.9800 . ? C120 H12E 0.9800 . ? C120 H12F 0.9800 . ? C121 H12G 0.9800 . ? C121 H12H 0.9800 . ? C121 H12I 0.9800 . ? C122 C123 1.528(11) . ? C122 C124 1.535(10) . ? C122 H122 1.0000 . ? C123 H12J 0.9800 . ? C123 H12K 0.9800 . ? C123 H12L 0.9800 . ? C124 H12M 0.9800 . ? C124 H12N 0.9800 . ? C124 H12O 0.9800 . ? C125 C126 1.484(11) . ? C125 C127 1.554(10) . ? C125 H125 1.0000 . ? C126 H12P 0.9800 . ? C126 H12Q 0.9800 . ? C126 H12R 0.9800 . ? C127 H12S 0.9800 . ? C127 H12T 0.9800 . ? C127 H12U 0.9800 . ? C128 C133 1.405(9) . ? C128 C129 1.411(8) . ? C129 C130 1.391(9) . ? C129 C134 1.522(9) . ? C130 C131 1.366(10) . ? C130 H130 0.9500 . ? C131 C132 1.391(11) . ? C131 C137 1.514(10) . ? C132 C133 1.391(10) . ? C132 H132 0.9500 . ? C133 C140 1.517(10) . ? C134 C136 1.514(9) . ? C134 C135 1.551(10) . ? C134 H134 1.0000 . ? C135 H13A 0.9800 . ? C135 H13B 0.9800 . ? C135 H13C 0.9800 . ? C136 H13D 0.9800 . ? C136 H13E 0.9800 . ? C136 H13F 0.9800 . ? C137 C138 1.517(14) . ? C137 C139 1.538(12) . ? C137 H137 1.0000 . ? C138 H13G 0.9800 . ? C138 H13H 0.9800 . ? C138 H13I 0.9800 . ? C139 H13J 0.9800 . ? C139 H13K 0.9800 . ? C139 H13L 0.9800 . ? C140 C141 1.536(11) . ? C140 C142 1.558(13) . ? C140 H140 1.0000 . ? C141 H14A 0.9800 . ? C141 H14B 0.9800 . ? C141 H14C 0.9800 . ? C142 H14D 0.9800 . ? C142 H14E 0.9800 . ? C142 H14F 0.9800 . ? C143 C148 1.390(8) . ? C143 C144 1.415(9) . ? C144 C145 1.376(9) . ? C144 C155 1.509(9) . ? C145 C146 1.407(9) . ? C145 C149 1.542(10) . ? C146 C147 1.406(10) . ? C146 H146 0.9500 . ? C147 C148 1.397(9) . ? C147 C152 1.519(9) . ? C148 C170 1.512(9) . ? C149 C151 1.504(11) . ? C149 C150 1.528(11) . ? C149 H149 1.0000 . ? C150 H15A 0.9800 . ? C150 H15B 0.9800 . ? C150 H15C 0.9800 . ? C151 H15D 0.9800 . ? C151 H15E 0.9800 . ? C151 H15F 0.9800 . ? C152 C154 1.536(11) . ? C152 C153 1.539(11) . ? C152 H152 1.0000 . ? C153 H15G 0.9800 . ? C153 H15H 0.9800 . ? C153 H15I 0.9800 . ? C154 H15J 0.9800 . ? C154 H15K 0.9800 . ? C154 H15L 0.9800 . ? C155 C160 1.389(10) . ? C155 C156 1.429(9) . ? C156 C157 1.372(9) . ? C156 C161 1.510(10) . ? C157 C158 1.407(10) . ? C157 H157 0.9500 . ? C158 C159 1.382(9) . ? C158 C164 1.510(9) . ? C159 C160 1.400(9) . ? C159 H159 0.9500 . ? C160 C167 1.525(9) . ? C161 C162 1.511(10) . ? C161 C163 1.538(9) . ? C161 H161 1.0000 . ? C162 H16A 0.9800 . ? C162 H16B 0.9800 . ? C162 H16C 0.9800 . ? C163 H16D 0.9800 . ? C163 H16E 0.9800 . ? C163 H16F 0.9800 . ? C164 C165 1.521(11) . ? C164 C166 1.525(11) . ? C164 H164 1.0000 . ? C165 H16G 0.9800 . ? C165 H16H 0.9800 . ? C165 H16I 0.9800 . ? C166 H16J 0.9800 . ? C166 H16K 0.9800 . ? C166 H16L 0.9800 . ? C167 C168 1.528(11) . ? C167 C169 1.551(10) . ? C167 H167 1.0000 . ? C168 H16M 0.9800 . ? C168 H16N 0.9800 . ? C168 H16O 0.9800 . ? C169 H16P 0.9800 . ? C169 H16Q 0.9800 . ? C169 H16R 0.9800 . ? C170 C171 1.398(9) . ? C170 C175 1.405(9) . ? C171 C172 1.391(9) . ? C171 C176 1.536(9) . ? C172 C173 1.384(9) . ? C172 H172 0.9500 . ? C173 C174 1.385(9) . ? C173 C179 1.516(9) . ? C174 C175 1.373(9) . ? C174 H174 0.9500 . ? C175 C182 1.530(9) . ? C176 C177 1.495(10) . ? C176 C178 1.537(9) . ? C176 H176 1.0000 . ? C177 H17A 0.9800 . ? C177 H17B 0.9800 . ? C177 H17C 0.9800 . ? C178 H17D 0.9800 . ? C178 H17E 0.9800 . ? C178 H17F 0.9800 . ? C179 C180 1.500(9) . ? C179 C181 1.543(9) . ? C179 H179 1.0000 . ? C180 H18A 0.9800 . ? C180 H18B 0.9800 . ? C180 H18C 0.9800 . ? C181 H18D 0.9800 . ? C181 H18E 0.9800 . ? C181 H18F 0.9800 . ? C182 C183 1.513(10) . ? C182 C184 1.555(9) . ? C182 H182 1.0000 . ? C183 H18G 0.9800 . ? C183 H18H 0.9800 . ? C183 H18I 0.9800 . ? C184 H18J 0.9800 . ? C184 H18K 0.9800 . ? C184 H18L 0.9800 . ? Sn5 C201 2.247(8) . ? Sn5 Sn6 2.6416(11) . ? Sn6 C243 2.204(7) . ? Sn5A C201 2.314(8) . ? Sn5A Sn6A 2.627(2) . ? Sn6A C243 2.249(7) . ? Sn5B C201 2.47(2) . ? Sn5B Sn6B 2.82(2) . ? Sn6B C243 2.326(12) . ? C201 C206 1.391(11) . ? C201 C202 1.410(10) . ? C202 C203 1.390(10) . ? C202 C213 1.557(11) . ? C203 C204 1.398(9) . ? C203 C207 1.518(9) . ? C204 C205 1.368(9) . ? C204 H204 0.9500 . ? C205 C206 1.413(10) . ? C205 C210 1.542(11) . ? C206 C228 1.503(10) . ? C207 C209 1.507(10) . ? C207 C208 1.524(10) . ? C207 H207 1.0000 . ? C208 H20D 0.9800 . ? C208 H20E 0.9800 . ? C208 H20F 0.9800 . ? C209 H20G 0.9800 . ? C209 H20H 0.9800 . ? C209 H20I 0.9800 . ? C210 C211 1.527(12) . ? C210 C212 1.530(12) . ? C210 H210 1.0000 . ? C211 H21D 0.9800 . ? C211 H21E 0.9800 . ? C211 H21F 0.9800 . ? C212 H21G 0.9800 . ? C212 H21H 0.9800 . ? C212 H21I 0.9800 . ? C213 C214 1.401(13) . ? C213 C218 1.407(11) . ? C214 C215 1.398(11) . ? C214 C219 1.508(13) . ? C215 C216 1.359(13) . ? C215 H215 0.9500 . ? C216 C217 1.367(13) . ? C216 C222 1.526(12) . ? C217 C218 1.405(12) . ? C217 H217 0.9500 . ? C218 C225 1.525(13) . ? C219 C221 1.523(14) . ? C219 C220 1.534(14) . ? C219 H219 1.0000 . ? C220 H22B 0.9800 . ? C220 H22C 0.9800 . ? C220 H22D 0.9800 . ? C221 H22E 0.9800 . ? C221 H22F 0.9800 . ? C221 H22G 0.9800 . ? C222 C224 1.490(11) . ? C222 C223 1.613(15) . ? C222 H222 1.0000 . ? C223 H22H 0.9800 . ? C223 H22I 0.9800 . ? C223 H22J 0.9800 . ? C224 H22K 0.9800 . ? C224 H22L 0.9800 . ? C224 H22M 0.9800 . ? C225 C226 1.529(12) . ? C225 C227 1.566(12) . ? C225 H225 1.0000 . ? C226 H22N 0.9800 . ? C226 H22O 0.9800 . ? C226 H22P 0.9800 . ? C227 H22Q 0.9800 . ? C227 H22R 0.9800 . ? C227 H22S 0.9800 . ? C228 C229 1.401(12) . ? C228 C233 1.411(10) . ? C229 C230 1.382(12) . ? C229 C23D 1.579(14) . ? C229 C234 1.591(14) . ? C230 C231 1.386(10) . ? C230 H230 0.9500 . ? C231 C232 1.376(10) . ? C231 C237 1.517(10) . ? C232 C233 1.412(9) . ? C232 H232 0.9500 . ? C233 C240 1.500(11) . ? C234 C236 1.571(11) . ? C234 C235 1.575(11) . ? C234 H234 1.0000 . ? C235 H23G 0.9800 . ? C235 H23H 0.9800 . ? C235 H23I 0.9800 . ? C236 H23J 0.9800 . ? C236 H23K 0.9800 . ? C236 H23L 0.9800 . ? C23D C23E 1.557(11) . ? C23D C23F 1.566(11) . ? C23D H23M 1.0000 . ? C23E H23N 0.9800 . ? C23E H23O 0.9800 . ? C23E H23P 0.9800 . ? C23F H23Q 0.9800 . ? C23F H23R 0.9800 . ? C23F H23S 0.9800 . ? C237 C238 1.517(11) . ? C237 C239 1.530(11) . ? C237 H237 1.0000 . ? C238 H23T 0.9800 . ? C238 H23U 0.9800 . ? C238 H23V 0.9800 . ? C239 H23W 0.9800 . ? C239 H23X 0.9800 . ? C239 H23Y 0.9800 . ? C240 C242 1.508(10) . ? C240 C241 1.534(11) . ? C240 H240 1.0000 . ? C241 H24G 0.9800 . ? C241 H24H 0.9800 . ? C241 H24I 0.9800 . ? C242 H24J 0.9800 . ? C242 H24K 0.9800 . ? C242 H24L 0.9800 . ? C243 C248 1.394(9) . ? C243 C244 1.397(9) . ? C244 C245 1.395(9) . ? C244 C255 1.490(9) . ? C245 C246 1.389(9) . ? C245 C249 1.524(9) . ? C246 C247 1.388(9) . ? C246 H246 0.9500 . ? C247 C248 1.406(9) . ? C247 C252 1.513(9) . ? C248 C270 1.507(9) . ? C249 C250 1.493(12) . ? C249 C251 1.573(12) . ? C249 H249 1.0000 . ? C250 H25B 0.9800 . ? C250 H25C 0.9800 . ? C250 H25D 0.9800 . ? C251 H25E 0.9800 . ? C251 H25F 0.9800 . ? C251 H25G 0.9800 . ? C252 C254 1.538(10) . ? C252 C253 1.539(11) . ? C252 H252 1.0000 . ? C253 H25H 0.9800 . ? C253 H25I 0.9800 . ? C253 H25J 0.9800 . ? C254 H25K 0.9800 . ? C254 H25L 0.9800 . ? C254 H25M 0.9800 . ? C255 C256 1.410(10) . ? C255 C260 1.410(10) . ? C256 C257 1.405(11) . ? C256 C261 1.508(12) . ? C257 C258 1.366(12) . ? C257 H257 0.9500 . ? C258 C259 1.389(11) . ? C258 C264 1.529(11) . ? C259 C260 1.403(10) . ? C259 H259 0.9500 . ? C260 C267 1.517(10) . ? C261 C263 1.533(10) . ? C261 C262 1.586(10) . ? C261 H261 1.0000 . ? C262 H2FC 0.9800 . ? C262 H2FD 0.9800 . ? C262 H2FE 0.9800 . ? C263 H26G 0.9800 . ? C263 H26H 0.9800 . ? C263 H26I 0.9800 . ? C26B H26K 0.9800 . ? C26B H26L 0.9800 . ? C26B H26M 0.9800 . ? C26C H26N 0.9800 . ? C26C H26O 0.9800 . ? C26C H26P 0.9800 . ? C264 C265 1.489(12) . ? C264 C266 1.522(12) . ? C264 H264 1.0000 . ? C265 H26Q 0.9800 . ? C265 H26R 0.9800 . ? C265 H26S 0.9800 . ? C266 H26T 0.9800 . ? C266 H26U 0.9800 . ? C266 H26V 0.9800 . ? C267 C268 1.517(10) . ? C267 C269 1.520(10) . ? C267 H267 1.0000 . ? C268 H26W 0.9800 . ? C268 H26X 0.9800 . ? C268 H26Y 0.9800 . ? C269 H26Z 0.9800 . ? C269 H2FA 0.9800 . ? C269 H2FB 0.9800 . ? C270 C275 1.381(10) . ? C270 C271 1.421(11) . ? C271 C272 1.369(10) . ? C271 C276 1.560(11) . ? C272 C273 1.367(11) . ? C272 H272 0.9500 . ? C273 C274 1.379(11) . ? C273 C279 1.540(11) . ? C274 C275 1.411(10) . ? C274 H274 0.9500 . ? C275 C282 1.540(11) . ? C276 C277 1.492(13) . ? C276 C278 1.555(14) . ? C276 H276 1.0000 . ? C277 H27G 0.9800 . ? C277 H27H 0.9800 . ? C277 H27I 0.9800 . ? C278 H27J 0.9800 . ? C278 H27K 0.9800 . ? C278 H27L 0.9800 . ? C279 C280 1.461(13) . ? C279 C281 1.538(15) . ? C279 H279 1.0000 . ? C280 H28A 0.9800 . ? C280 H28B 0.9800 . ? C280 H28C 0.9800 . ? C281 H28D 0.9800 . ? C281 H28E 0.9800 . ? C281 H28F 0.9800 . ? C282 C284 1.511(10) . ? C282 C283 1.553(11) . ? C282 H282 1.0000 . ? C283 H28G 0.9800 . ? C283 H28H 0.9800 . ? C283 H28I 0.9800 . ? C284 H28J 0.9800 . ? C284 H28K 0.9800 . ? C284 H28L 0.9800 . ? C301 C302 1.60(3) . ? C301 H30A 0.9800 . ? C301 H30B 0.9800 . ? C301 H30C 0.9800 . ? C302 O303 1.46(3) . ? C302 H30D 0.9900 . ? C302 H30E 0.9900 . ? O303 C304 1.58(4) . ? C304 C305 1.60(3) . ? C304 H30F 0.9900 . ? C304 H30G 0.9900 . ? C305 H30H 0.9800 . ? C305 H30I 0.9800 . ? C305 H30J 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Sn1 Sn2 124.38(18) . . ? C43 Sn2 Sn1 127.25(17) . . ? C2 C1 C6 120.0(6) . . ? C2 C1 Sn1 123.3(5) . . ? C6 C1 Sn1 116.1(5) . . ? C1 C2 C3 119.9(6) . . ? C1 C2 C13 119.4(6) . . ? C3 C2 C13 120.7(7) . . ? C4 C3 C2 118.6(7) . . ? C4 C3 C7 118.1(6) . . ? C2 C3 C7 123.2(6) . . ? C5 C4 C3 122.7(7) . . ? C5 C4 H4 118.7 . . ? C3 C4 H4 118.7 . . ? C4 C5 C6 118.1(6) . . ? C4 C5 C10 119.3(6) . . ? C6 C5 C10 122.6(6) . . ? C1 C6 C5 120.5(6) . . ? C1 C6 C28 117.9(6) . . ? C5 C6 C28 121.3(6) . . ? C9 C7 C3 112.8(6) . . ? C9 C7 C8 109.2(6) . . ? C3 C7 C8 111.2(6) . . ? C9 C7 H7 107.8 . . ? C3 C7 H7 107.8 . . ? C8 C7 H7 107.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C5 112.7(6) . . ? C11 C10 C12 108.6(6) . . ? C5 C10 C12 111.1(6) . . ? C11 C10 H10 108.1 . . ? C5 C10 H10 108.1 . . ? C12 C10 H10 108.1 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 120.1(7) . . ? C18 C13 C2 120.4(7) . . ? C14 C13 C2 119.5(6) . . ? C13 C14 C15 119.0(7) . . ? C13 C14 C19 122.8(6) . . ? C15 C14 C19 118.2(7) . . ? C16 C15 C14 122.2(8) . . ? C16 C15 H15 118.9 . . ? C14 C15 H15 118.9 . . ? C15 C16 C17 118.4(7) . . ? C15 C16 C22 121.6(8) . . ? C17 C16 C22 120.0(8) . . ? C16 C17 C18 122.2(8) . . ? C16 C17 H17 118.9 . . ? C18 C17 H17 118.9 . . ? C13 C18 C17 118.1(8) . . ? C13 C18 C25D 120.0(9) . . ? C17 C18 C25D 117.6(9) . . ? C13 C18 C25 123.4(11) . . ? C17 C18 C25 116.1(11) . . ? C14 C19 C20 111.8(6) . . ? C14 C19 C21 112.6(6) . . ? C20 C19 C21 110.4(6) . . ? C14 C19 H19 107.2 . . ? C20 C19 H19 107.2 . . ? C21 C19 H19 107.2 . . ? 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 . . ? C24 C22 C16 109.0(8) . . ? C24 C22 C23 106.0(9) . . ? C16 C22 C23 113.1(8) . . ? C24 C22 H22 109.5 . . ? C16 C22 H22 109.5 . . ? C23 C22 H22 109.5 . . ? H23D C23A H23E 109.5 . . ? H23D C23A H23F 109.5 . . ? H23E C23A H23F 109.5 . . ? H24D C24A H24E 109.5 . . ? H24D C24A H24F 109.5 . . ? H24E C24A H24F 109.5 . . ? C27 C25 C26 108.1(12) . . ? C27 C25 C18 121.1(14) . . ? C26 C25 C18 110.7(12) . . ? C27 C25 H25 105.2 . . ? C26 C25 H25 105.2 . . ? C18 C25 H25 105.2 . . ? C27D C25D C26D 109.2(12) . . ? C27D C25D C18 120.6(12) . . ? C26D C25D C18 98.9(12) . . ? C27D C25D H25A 109.1 . . ? C26D C25D H25A 109.1 . . ? C18 C25D H25A 109.1 . . ? C25D C26D H26D 109.5 . . ? C25D C26D H26E 109.5 . . ? H26D C26D H26E 109.5 . . ? C25D C26D H26F 109.5 . . ? H26D C26D H26F 109.5 . . ? H26E C26D H26F 109.5 . . ? C25D C27D H27D 109.5 . . ? C25D C27D H27E 109.5 . . ? H27D C27D H27E 109.5 . . ? C25D C27D H27F 109.5 . . ? H27D C27D H27F 109.5 . . ? H27E C27D H27F 109.5 . . ? C33 C28 C29 119.9(6) . . ? C33 C28 C6 122.9(6) . . ? C29 C28 C6 117.2(6) . . ? C28 C29 C30 119.4(7) . . ? C28 C29 C34 122.2(6) . . ? C30 C29 C34 118.3(6) . . ? C31 C30 C29 121.4(7) . . ? C31 C30 H30 119.3 . . ? C29 C30 H30 119.3 . . ? C32 C31 C30 117.9(7) . . ? C32 C31 C37 120.7(7) . . ? C30 C31 C37 121.4(7) . . ? C31 C32 C33 122.4(7) . . ? C31 C32 H32 118.8 . . ? C33 C32 H32 118.8 . . ? C28 C33 C32 119.0(6) . . ? C28 C33 C40 122.8(6) . . ? C32 C33 C40 118.1(7) . . ? C35 C34 C29 114.4(6) . . ? C35 C34 C36 109.8(6) . . ? C29 C34 C36 108.8(7) . . ? C35 C34 H34 107.9 . . ? C29 C34 H34 107.9 . . ? C36 C34 H34 107.9 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C39 C37 C38 112.9(10) . . ? C39 C37 C31 109.7(9) . . ? C38 C37 C31 112.5(9) . . ? C39 C37 H37 107.1 . . ? C38 C37 H37 107.1 . . ? C31 C37 H37 107.1 . . ? H38D C38A H38E 109.5 . . ? H38D C38A H38F 109.5 . . ? H38E C38A H38F 109.5 . . ? H39D C39A H39E 109.5 . . ? H39D C39A H39F 109.5 . . ? H39E C39A H39F 109.5 . . ? C33 C40 C42 112.3(6) . . ? C33 C40 C41 112.8(6) . . ? C42 C40 C41 109.7(6) . . ? C33 C40 H40 107.2 . . ? C42 C40 H40 107.2 . . ? C41 C40 H40 107.2 . . ? 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 . . ? C44 C43 C48 120.3(6) . . ? C44 C43 Sn2 123.1(5) . . ? C48 C43 Sn2 116.3(5) . . ? C45 C44 C43 119.9(6) . . ? C45 C44 C55 123.1(6) . . ? C43 C44 C55 116.9(6) . . ? C44 C45 C46 117.9(6) . . ? C44 C45 C49 122.0(7) . . ? C46 C45 C49 120.1(7) . . ? C47 C46 C45 124.1(7) . . ? C47 C46 H46 117.9 . . ? C45 C46 H46 117.9 . . ? C46 C47 C48 118.5(6) . . ? C46 C47 C52 119.4(7) . . ? C48 C47 C52 122.1(6) . . ? C47 C48 C43 119.1(6) . . ? C47 C48 C70 121.9(6) . . ? C43 C48 C70 119.0(6) . . ? C51 C49 C45 113.2(8) . . ? C51 C49 C50 109.1(8) . . ? C45 C49 C50 111.0(7) . . ? C51 C49 H49 107.8 . . ? C45 C49 H49 107.8 . . ? C50 C49 H49 107.8 . . ? C49 C50 H50A 109.5 . . ? C49 C50 H50B 109.5 . . ? H50A C50 H50B 109.5 . . ? C49 C50 H50C 109.5 . . ? H50A C50 H50C 109.5 . . ? H50B C50 H50C 109.5 . . ? C49 C51 H51A 109.5 . . ? C49 C51 H51B 109.5 . . ? H51A C51 H51B 109.5 . . ? C49 C51 H51C 109.5 . . ? H51A C51 H51C 109.5 . . ? H51B C51 H51C 109.5 . . ? C54 C52 C47 111.3(6) . . ? C54 C52 C53 110.8(7) . . ? C47 C52 C53 110.3(6) . . ? C54 C52 H52 108.1 . . ? C47 C52 H52 108.1 . . ? C53 C52 H52 108.1 . . ? 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 . . ? C56 C55 C60 120.7(6) . . ? C56 C55 C44 119.9(6) . . ? C60 C55 C44 119.4(6) . . ? C57 C56 C55 118.0(6) . . ? C57 C56 C61 119.5(7) . . ? C55 C56 C61 122.5(7) . . ? C58 C57 C56 122.7(7) . . ? C58 C57 H57 118.6 . . ? C56 C57 H57 118.6 . . ? C57 C58 C59 117.6(7) . . ? C57 C58 C64 121.6(7) . . ? C59 C58 C64 120.8(7) . . ? C60 C59 C58 122.9(7) . . ? C60 C59 H59 118.5 . . ? C58 C59 H59 118.5 . . ? C59 C60 C55 117.9(7) . . ? C59 C60 C67 119.7(6) . . ? C55 C60 C67 122.4(6) . . ? C56 C61 C63 112.5(7) . . ? C56 C61 C62 111.0(6) . . ? C63 C61 C62 110.7(7) . . ? C56 C61 H61 107.5 . . ? C63 C61 H61 107.5 . . ? C62 C61 H61 107.5 . . ? C61 C62 H62A 109.5 . . ? C61 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C61 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C61 C63 H63A 109.5 . . ? C61 C63 H63B 109.5 . . ? H63A C63 H63B 109.5 . . ? C61 C63 H63C 109.5 . . ? H63A C63 H63C 109.5 . . ? H63B C63 H63C 109.5 . . ? C65 C64 C58 111.1(7) . . ? C65 C64 C66 111.3(8) . . ? C58 C64 C66 111.0(7) . . ? C65 C64 H64 107.8 . . ? C58 C64 H64 107.8 . . ? C66 C64 H64 107.8 . . ? H65D C65A H65E 109.5 . . ? H65D C65A H65F 109.5 . . ? H65E C65A H65F 109.5 . . ? H66D C66A H66E 109.5 . . ? H66D C66A H66F 109.5 . . ? H66E C66A H66F 109.5 . . ? C68 C67 C60 112.4(6) . . ? C68 C67 C69 110.5(6) . . ? C60 C67 C69 113.6(6) . . ? C68 C67 H67 106.6 . . ? C60 C67 H67 106.6 . . ? C69 C67 H67 106.6 . . ? C67 C68 H68A 109.5 . . ? C67 C68 H68B 109.5 . . ? H68A C68 H68B 109.5 . . ? C67 C68 H68C 109.5 . . ? H68A C68 H68C 109.5 . . ? H68B C68 H68C 109.5 . . ? C67 C69 H69A 109.5 . . ? C67 C69 H69B 109.5 . . ? H69A C69 H69B 109.5 . . ? C67 C69 H69C 109.5 . . ? H69A C69 H69C 109.5 . . ? H69B C69 H69C 109.5 . . ? C75 C70 C71 119.9(7) . . ? C75 C70 C48 122.4(7) . . ? C71 C70 C48 117.6(7) . . ? C72 C71 C70 118.8(8) . . ? C72 C71 C76 119.2(8) . . ? C70 C71 C76 122.1(7) . . ? C73 C72 C71 121.1(9) . . ? C73 C72 H72 119.4 . . ? C71 C72 H72 119.4 . . ? C72 C73 C74 120.3(8) . . ? C72 C73 C79 127.4(11) . . ? C74 C73 C79 109.4(12) . . ? C72 C73 C79A 116.1(11) . . ? C74 C73 C79A 123.4(11) . . ? C73 C74 C75 120.4(8) . . ? C73 C74 H74 119.8 . . ? C75 C74 H74 119.8 . . ? C70 C75 C74 119.4(7) . . ? C70 C75 C82 120.8(7) . . ? C74 C75 C82 119.6(7) . . ? C77 C76 C78 109.8(7) . . ? C77 C76 C71 112.6(8) . . ? C78 C76 C71 112.2(7) . . ? C77 C76 H76 107.3 . . ? C78 C76 H76 107.3 . . ? C71 C76 H76 107.3 . . ? C76 C77 H77A 109.5 . . ? C76 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C76 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C76 C78 H78A 109.5 . . ? C76 C78 H78B 109.5 . . ? H78A C78 H78B 109.5 . . ? C76 C78 H78C 109.5 . . ? H78A C78 H78C 109.5 . . ? H78B C78 H78C 109.5 . . ? C81 C79 C80 119.3(10) . . ? C81 C79 C73 127.8(16) . . ? C80 C79 C73 107.1(13) . . ? C81 C79 H79 98.0 . . ? C80 C79 H79 98.0 . . ? C73 C79 H79 98.0 . . ? C79 C80 H80A 109.5 . . ? C79 C80 H80B 109.5 . . ? H80A C80 H80B 109.5 . . ? C79 C80 H80C 109.5 . . ? H80A C80 H80C 109.5 . . ? H80B C80 H80C 109.5 . . ? C79 C81 H81A 109.5 . . ? C79 C81 H81B 109.5 . . ? H81A C81 H81B 109.5 . . ? C79 C81 H81C 109.5 . . ? H81A C81 H81C 109.5 . . ? H81B C81 H81C 109.5 . . ? C80A C79A C81A 111.8(9) . . ? C80A C79A C73 122.7(16) . . ? C81A C79A C73 99.7(16) . . ? C80A C79A H79A 107.2 . . ? C81A C79A H79A 107.2 . . ? C73 C79A H79A 107.2 . . ? C79A C80A H80D 109.5 . . ? C79A C80A H80E 109.5 . . ? H80D C80A H80E 109.5 . . ? C79A C80A H80F 109.5 . . ? H80D C80A H80F 109.5 . . ? H80E C80A H80F 109.5 . . ? C79A C81A H81D 109.5 . . ? C79A C81A H81E 109.5 . . ? H81D C81A H81E 109.5 . . ? C79A C81A H81F 109.5 . . ? H81D C81A H81F 109.5 . . ? H81E C81A H81F 109.5 . . ? C83 C82 C75 114.2(7) . . ? C83 C82 C84 109.2(7) . . ? C75 C82 C84 110.2(7) . . ? C83 C82 H82 107.7 . . ? C75 C82 H82 107.7 . . ? C84 C82 H82 107.7 . . ? C82 C83 H83A 109.5 . . ? C82 C83 H83B 109.5 . . ? H83A C83 H83B 109.5 . . ? C82 C83 H83C 109.5 . . ? H83A C83 H83C 109.5 . . ? H83B C83 H83C 109.5 . . ? C82 C84 H84A 109.5 . . ? C82 C84 H84B 109.5 . . ? H84A C84 H84B 109.5 . . ? C82 C84 H84C 109.5 . . ? H84A C84 H84C 109.5 . . ? H84B C84 H84C 109.5 . . ? C101 Sn3 Sn4 125.13(15) . . ? C143 Sn4 Sn3 124.07(16) . . ? C106 C101 C102 120.3(6) . . ? C106 C101 Sn3 118.1(4) . . ? C102 C101 Sn3 121.1(5) . . ? C103 C102 C101 119.5(6) . . ? C103 C102 C113 123.1(6) . . ? C101 C102 C113 117.4(6) . . ? C102 C103 C104 118.5(7) . . ? C102 C103 C107 122.9(7) . . ? C104 C103 C107 118.5(7) . . ? C105 C104 C103 122.3(7) . . ? C105 C104 H104 118.9 . . ? C103 C104 H104 118.9 . . ? C104 C105 C106 119.1(7) . . ? C104 C105 C110 118.4(6) . . ? C106 C105 C110 122.5(6) . . ? C105 C106 C101 120.2(6) . . ? C105 C106 C128 123.4(6) . . ? C101 C106 C128 116.3(5) . . ? C103 C107 C109 111.3(10) . . ? C103 C107 C108 111.2(7) . . ? C109 C107 C108 111.2(8) . . ? C103 C107 H107 107.6 . . ? C109 C107 H107 107.6 . . ? C108 C107 H107 107.6 . . ? C107 C108 H10A 109.5 . . ? C107 C108 H10B 109.5 . . ? H10A C108 H10B 109.5 . . ? C107 C108 H10C 109.5 . . ? H10A C108 H10C 109.5 . . ? H10B C108 H10C 109.5 . . ? C107 C109 H10D 109.5 . . ? C107 C109 H10E 109.5 . . ? H10D C109 H10E 109.5 . . ? C107 C109 H10F 109.5 . . ? H10D C109 H10F 109.5 . . ? H10E C109 H10F 109.5 . . ? C112 C110 C105 112.1(7) . . ? C112 C110 C111 110.3(7) . . ? C105 C110 C111 111.0(6) . . ? C112 C110 H110 107.7 . . ? C105 C110 H110 107.7 . . ? C111 C110 H110 107.7 . . ? C110 C111 H11D 109.5 . . ? C110 C111 H11E 109.5 . . ? H11D C111 H11E 109.5 . . ? C110 C111 H11F 109.5 . . ? H11D C111 H11F 109.5 . . ? H11E C111 H11F 109.5 . . ? C110 C112 H11G 109.5 . . ? C110 C112 H11H 109.5 . . ? H11G C112 H11H 109.5 . . ? C110 C112 H11I 109.5 . . ? H11G C112 H11I 109.5 . . ? H11H C112 H11I 109.5 . . ? C114 C113 C118 119.6(6) . . ? C114 C113 C102 119.3(6) . . ? C118 C113 C102 121.0(6) . . ? C115 C114 C113 119.0(7) . . ? C115 C114 C119 119.6(6) . . ? C113 C114 C119 121.4(6) . . ? C114 C115 C116 121.6(6) . . ? C114 C115 H115 119.2 . . ? C116 C115 H115 119.2 . . ? C117 C116 C115 118.2(6) . . ? C117 C116 C122 124.0(7) . . ? C115 C116 C122 117.7(6) . . ? C116 C117 C118 122.6(7) . . ? C116 C117 H117 118.7 . . ? C118 C117 H117 118.7 . . ? C117 C118 C113 118.8(6) . . ? C117 C118 C125 119.0(7) . . ? C113 C118 C125 122.2(7) . . ? C114 C119 C120 112.8(6) . . ? C114 C119 C121 112.9(6) . . ? C120 C119 C121 109.1(6) . . ? C114 C119 H119 107.3 . . ? C120 C119 H119 107.3 . . ? C121 C119 H119 107.3 . . ? C119 C120 H12D 109.5 . . ? C119 C120 H12E 109.5 . . ? H12D C120 H12E 109.5 . . ? C119 C120 H12F 109.5 . . ? H12D C120 H12F 109.5 . . ? H12E C120 H12F 109.5 . . ? C119 C121 H12G 109.5 . . ? C119 C121 H12H 109.5 . . ? H12G C121 H12H 109.5 . . ? C119 C121 H12I 109.5 . . ? H12G C121 H12I 109.5 . . ? H12H C121 H12I 109.5 . . ? C116 C122 C123 113.1(6) . . ? C116 C122 C124 111.0(7) . . ? C123 C122 C124 110.8(7) . . ? C116 C122 H122 107.2 . . ? C123 C122 H122 107.2 . . ? C124 C122 H122 107.2 . . ? C122 C123 H12J 109.5 . . ? C122 C123 H12K 109.5 . . ? H12J C123 H12K 109.5 . . ? C122 C123 H12L 109.5 . . ? H12J C123 H12L 109.5 . . ? H12K C123 H12L 109.5 . . ? C122 C124 H12M 109.5 . . ? C122 C124 H12N 109.5 . . ? H12M C124 H12N 109.5 . . ? C122 C124 H12O 109.5 . . ? H12M C124 H12O 109.5 . . ? H12N C124 H12O 109.5 . . ? C126 C125 C118 113.3(7) . . ? C126 C125 C127 110.3(7) . . ? C118 C125 C127 109.4(6) . . ? C126 C125 H125 107.9 . . ? C118 C125 H125 107.9 . . ? C127 C125 H125 107.9 . . ? C125 C126 H12P 109.5 . . ? C125 C126 H12Q 109.5 . . ? H12P C126 H12Q 109.5 . . ? C125 C126 H12R 109.5 . . ? H12P C126 H12R 109.5 . . ? H12Q C126 H12R 109.5 . . ? C125 C127 H12S 109.5 . . ? C125 C127 H12T 109.5 . . ? H12S C127 H12T 109.5 . . ? C125 C127 H12U 109.5 . . ? H12S C127 H12U 109.5 . . ? H12T C127 H12U 109.5 . . ? C133 C128 C129 118.5(6) . . ? C133 C128 C106 122.2(6) . . ? C129 C128 C106 119.3(5) . . ? C130 C129 C128 119.5(6) . . ? C130 C129 C134 119.5(6) . . ? C128 C129 C134 120.9(6) . . ? C131 C130 C129 122.8(7) . . ? C131 C130 H130 118.6 . . ? C129 C130 H130 118.6 . . ? C130 C131 C132 117.4(6) . . ? C130 C131 C137 123.4(8) . . ? C132 C131 C137 119.1(8) . . ? C131 C132 C133 122.4(7) . . ? C131 C132 H132 118.8 . . ? C133 C132 H132 118.8 . . ? C132 C133 C128 119.3(7) . . ? C132 C133 C140 120.3(7) . . ? C128 C133 C140 120.4(7) . . ? C136 C134 C129 110.5(6) . . ? C136 C134 C135 110.2(6) . . ? C129 C134 C135 111.4(6) . . ? C136 C134 H134 108.2 . . ? C129 C134 H134 108.2 . . ? C135 C134 H134 108.2 . . ? C134 C135 H13A 109.5 . . ? C134 C135 H13B 109.5 . . ? H13A C135 H13B 109.5 . . ? C134 C135 H13C 109.5 . . ? H13A C135 H13C 109.5 . . ? H13B C135 H13C 109.5 . . ? C134 C136 H13D 109.5 . . ? C134 C136 H13E 109.5 . . ? H13D C136 H13E 109.5 . . ? C134 C136 H13F 109.5 . . ? H13D C136 H13F 109.5 . . ? H13E C136 H13F 109.5 . . ? C131 C137 C138 115.1(8) . . ? C131 C137 C139 109.0(7) . . ? C138 C137 C139 110.0(8) . . ? C131 C137 H137 107.5 . . ? C138 C137 H137 107.5 . . ? C139 C137 H137 107.5 . . ? C137 C138 H13G 109.5 . . ? C137 C138 H13H 109.5 . . ? H13G C138 H13H 109.5 . . ? C137 C138 H13I 109.5 . . ? H13G C138 H13I 109.5 . . ? H13H C138 H13I 109.5 . . ? C137 C139 H13J 109.5 . . ? C137 C139 H13K 109.5 . . ? H13J C139 H13K 109.5 . . ? C137 C139 H13L 109.5 . . ? H13J C139 H13L 109.5 . . ? H13K C139 H13L 109.5 . . ? C133 C140 C141 111.0(7) . . ? C133 C140 C142 110.2(7) . . ? C141 C140 C142 109.4(7) . . ? C133 C140 H140 108.8 . . ? C141 C140 H140 108.8 . . ? C142 C140 H140 108.8 . . ? C140 C141 H14A 109.5 . . ? C140 C141 H14B 109.5 . . ? H14A C141 H14B 109.5 . . ? C140 C141 H14C 109.5 . . ? H14A C141 H14C 109.5 . . ? H14B C141 H14C 109.5 . . ? C140 C142 H14D 109.5 . . ? C140 C142 H14E 109.5 . . ? H14D C142 H14E 109.5 . . ? C140 C142 H14F 109.5 . . ? H14D C142 H14F 109.5 . . ? H14E C142 H14F 109.5 . . ? C148 C143 C144 120.1(6) . . ? C148 C143 Sn4 117.5(4) . . ? C144 C143 Sn4 122.1(5) . . ? C145 C144 C143 119.9(6) . . ? C145 C144 C155 121.5(6) . . ? C143 C144 C155 118.6(6) . . ? C144 C145 C146 119.2(6) . . ? C144 C145 C149 122.4(6) . . ? C146 C145 C149 118.4(6) . . ? C147 C146 C145 121.8(7) . . ? C147 C146 H146 119.1 . . ? C145 C146 H146 119.1 . . ? C148 C147 C146 117.7(6) . . ? C148 C147 C152 122.1(6) . . ? C146 C147 C152 120.1(6) . . ? C143 C148 C147 121.1(6) . . ? C143 C148 C170 117.6(6) . . ? C147 C148 C170 121.1(6) . . ? C151 C149 C150 110.5(7) . . ? C151 C149 C145 111.7(7) . . ? C150 C149 C145 111.1(6) . . ? C151 C149 H149 107.8 . . ? C150 C149 H149 107.8 . . ? C145 C149 H149 107.8 . . ? C149 C150 H15A 109.5 . . ? C149 C150 H15B 109.5 . . ? H15A C150 H15B 109.5 . . ? C149 C150 H15C 109.5 . . ? H15A C150 H15C 109.5 . . ? H15B C150 H15C 109.5 . . ? C149 C151 H15D 109.5 . . ? C149 C151 H15E 109.5 . . ? H15D C151 H15E 109.5 . . ? C149 C151 H15F 109.5 . . ? H15D C151 H15F 109.5 . . ? H15E C151 H15F 109.5 . . ? C147 C152 C154 111.5(6) . . ? C147 C152 C153 111.1(7) . . ? C154 C152 C153 111.0(7) . . ? C147 C152 H152 107.7 . . ? C154 C152 H152 107.7 . . ? C153 C152 H152 107.7 . . ? C152 C153 H15G 109.5 . . ? C152 C153 H15H 109.5 . . ? H15G C153 H15H 109.5 . . ? C152 C153 H15I 109.5 . . ? H15G C153 H15I 109.5 . . ? H15H C153 H15I 109.5 . . ? C152 C154 H15J 109.5 . . ? C152 C154 H15K 109.5 . . ? H15J C154 H15K 109.5 . . ? C152 C154 H15L 109.5 . . ? H15J C154 H15L 109.5 . . ? H15K C154 H15L 109.5 . . ? C160 C155 C156 120.3(6) . . ? C160 C155 C144 120.7(6) . . ? C156 C155 C144 119.1(6) . . ? C157 C156 C155 118.1(6) . . ? C157 C156 C161 120.7(6) . . ? C155 C156 C161 121.2(6) . . ? C156 C157 C158 123.2(6) . . ? C156 C157 H157 118.4 . . ? C158 C157 H157 118.4 . . ? C159 C158 C157 116.9(6) . . ? C159 C158 C164 123.4(6) . . ? C157 C158 C164 119.6(6) . . ? C158 C159 C160 122.7(7) . . ? C158 C159 H159 118.6 . . ? C160 C159 H159 118.6 . . ? C155 C160 C159 118.8(6) . . ? C155 C160 C167 123.1(6) . . ? C159 C160 C167 118.0(7) . . ? C156 C161 C162 111.6(6) . . ? C156 C161 C163 111.9(6) . . ? C162 C161 C163 110.8(6) . . ? C156 C161 H161 107.4 . . ? C162 C161 H161 107.4 . . ? C163 C161 H161 107.4 . . ? C161 C162 H16A 109.5 . . ? C161 C162 H16B 109.5 . . ? H16A C162 H16B 109.5 . . ? C161 C162 H16C 109.5 . . ? H16A C162 H16C 109.5 . . ? H16B C162 H16C 109.5 . . ? C161 C163 H16D 109.5 . . ? C161 C163 H16E 109.5 . . ? H16D C163 H16E 109.5 . . ? C161 C163 H16F 109.5 . . ? H16D C163 H16F 109.5 . . ? H16E C163 H16F 109.5 . . ? C158 C164 C165 113.4(6) . . ? C158 C164 C166 109.7(7) . . ? C165 C164 C166 110.9(6) . . ? C158 C164 H164 107.5 . . ? C165 C164 H164 107.5 . . ? C166 C164 H164 107.5 . . ? C164 C165 H16G 109.5 . . ? C164 C165 H16H 109.5 . . ? H16G C165 H16H 109.5 . . ? C164 C165 H16I 109.5 . . ? H16G C165 H16I 109.5 . . ? H16H C165 H16I 109.5 . . ? C164 C166 H16J 109.5 . . ? C164 C166 H16K 109.5 . . ? H16J C166 H16K 109.5 . . ? C164 C166 H16L 109.5 . . ? H16J C166 H16L 109.5 . . ? H16K C166 H16L 109.5 . . ? C160 C167 C168 113.3(6) . . ? C160 C167 C169 110.1(6) . . ? C168 C167 C169 109.9(7) . . ? C160 C167 H167 107.8 . . ? C168 C167 H167 107.8 . . ? C169 C167 H167 107.8 . . ? C167 C168 H16M 109.5 . . ? C167 C168 H16N 109.5 . . ? H16M C168 H16N 109.5 . . ? C167 C168 H16O 109.5 . . ? H16M C168 H16O 109.5 . . ? H16N C168 H16O 109.5 . . ? C167 C169 H16P 109.5 . . ? C167 C169 H16Q 109.5 . . ? H16P C169 H16Q 109.5 . . ? C167 C169 H16R 109.5 . . ? H16P C169 H16R 109.5 . . ? H16Q C169 H16R 109.5 . . ? C171 C170 C175 119.0(6) . . ? C171 C170 C148 119.7(6) . . ? C175 C170 C148 121.1(6) . . ? C172 C171 C170 120.0(6) . . ? C172 C171 C176 118.3(6) . . ? C170 C171 C176 121.5(6) . . ? C173 C172 C171 121.8(6) . . ? C173 C172 H172 119.1 . . ? C171 C172 H172 119.1 . . ? C172 C173 C174 116.7(6) . . ? C172 C173 C179 122.3(6) . . ? C174 C173 C179 120.9(6) . . ? C175 C174 C173 123.9(6) . . ? C175 C174 H174 118.0 . . ? C173 C174 H174 118.0 . . ? C174 C175 C170 118.6(6) . . ? C174 C175 C182 120.3(6) . . ? C170 C175 C182 121.1(6) . . ? C177 C176 C171 112.0(6) . . ? C177 C176 C178 111.3(6) . . ? C171 C176 C178 110.8(6) . . ? C177 C176 H176 107.5 . . ? C171 C176 H176 107.5 . . ? C178 C176 H176 107.5 . . ? C176 C177 H17A 109.5 . . ? C176 C177 H17B 109.5 . . ? H17A C177 H17B 109.5 . . ? C176 C177 H17C 109.5 . . ? H17A C177 H17C 109.5 . . ? H17B C177 H17C 109.5 . . ? C176 C178 H17D 109.5 . . ? C176 C178 H17E 109.5 . . ? H17D C178 H17E 109.5 . . ? C176 C178 H17F 109.5 . . ? H17D C178 H17F 109.5 . . ? H17E C178 H17F 109.5 . . ? C180 C179 C173 115.0(5) . . ? C180 C179 C181 111.1(5) . . ? C173 C179 C181 108.4(6) . . ? C180 C179 H179 107.3 . . ? C173 C179 H179 107.3 . . ? C181 C179 H179 107.3 . . ? C179 C180 H18A 109.5 . . ? C179 C180 H18B 109.5 . . ? H18A C180 H18B 109.5 . . ? C179 C180 H18C 109.5 . . ? H18A C180 H18C 109.5 . . ? H18B C180 H18C 109.5 . . ? C179 C181 H18D 109.5 . . ? C179 C181 H18E 109.5 . . ? H18D C181 H18E 109.5 . . ? C179 C181 H18F 109.5 . . ? H18D C181 H18F 109.5 . . ? H18E C181 H18F 109.5 . . ? C183 C182 C175 113.1(6) . . ? C183 C182 C184 109.8(6) . . ? C175 C182 C184 109.4(5) . . ? C183 C182 H182 108.2 . . ? C175 C182 H182 108.2 . . ? C184 C182 H182 108.2 . . ? C182 C183 H18G 109.5 . . ? C182 C183 H18H 109.5 . . ? H18G C183 H18H 109.5 . . ? C182 C183 H18I 109.5 . . ? H18G C183 H18I 109.5 . . ? H18H C183 H18I 109.5 . . ? C182 C184 H18J 109.5 . . ? C182 C184 H18K 109.5 . . ? H18J C184 H18K 109.5 . . ? C182 C184 H18L 109.5 . . ? H18J C184 H18L 109.5 . . ? H18K C184 H18L 109.5 . . ? C201 Sn5 Sn6 125.5(2) . . ? C243 Sn6 Sn5 125.39(18) . . ? C201 Sn5A Sn6A 120.1(2) . . ? C243 Sn6A Sn5A 124.54(19) . . ? C201 Sn5B Sn6B 109.0(8) . . ? C243 Sn6B Sn5B 113.5(6) . . ? C206 C201 C202 121.8(7) . . ? C206 C201 Sn5 127.3(5) . . ? C202 C201 Sn5 109.5(6) . . ? C206 C201 Sn5A 103.2(5) . . ? C202 C201 Sn5A 128.4(5) . . ? C206 C201 Sn5B 116.3(8) . . ? C202 C201 Sn5B 111.9(7) . . ? C203 C202 C201 119.5(7) . . ? C203 C202 C213 122.2(7) . . ? C201 C202 C213 118.2(7) . . ? C202 C203 C204 117.7(6) . . ? C202 C203 C207 124.0(7) . . ? C204 C203 C207 118.2(6) . . ? C205 C204 C203 123.6(6) . . ? C205 C204 H204 118.2 . . ? C203 C204 H204 118.2 . . ? C204 C205 C206 119.1(7) . . ? C204 C205 C210 117.4(6) . . ? C206 C205 C210 123.5(6) . . ? C201 C206 C205 118.2(7) . . ? C201 C206 C228 120.2(7) . . ? C205 C206 C228 121.5(7) . . ? C209 C207 C203 112.6(6) . . ? C209 C207 C208 109.2(6) . . ? C203 C207 C208 111.7(6) . . ? C209 C207 H207 107.7 . . ? C203 C207 H207 107.7 . . ? C208 C207 H207 107.7 . . ? C207 C208 H20D 109.5 . . ? C207 C208 H20E 109.5 . . ? H20D C208 H20E 109.5 . . ? C207 C208 H20F 109.5 . . ? H20D C208 H20F 109.5 . . ? H20E C208 H20F 109.5 . . ? C207 C209 H20G 109.5 . . ? C207 C209 H20H 109.5 . . ? H20G C209 H20H 109.5 . . ? C207 C209 H20I 109.5 . . ? H20G C209 H20I 109.5 . . ? H20H C209 H20I 109.5 . . ? C211 C210 C212 110.1(8) . . ? C211 C210 C205 112.0(7) . . ? C212 C210 C205 110.6(7) . . ? C211 C210 H210 108.0 . . ? C212 C210 H210 108.0 . . ? C205 C210 H210 108.0 . . ? C210 C211 H21D 109.5 . . ? C210 C211 H21E 109.5 . . ? H21D C211 H21E 109.5 . . ? C210 C211 H21F 109.5 . . ? H21D C211 H21F 109.5 . . ? H21E C211 H21F 109.5 . . ? C210 C212 H21G 109.5 . . ? C210 C212 H21H 109.5 . . ? H21G C212 H21H 109.5 . . ? C210 C212 H21I 109.5 . . ? H21G C212 H21I 109.5 . . ? H21H C212 H21I 109.5 . . ? C214 C213 C218 120.1(8) . . ? C214 C213 C202 121.7(7) . . ? C218 C213 C202 118.1(9) . . ? C215 C214 C213 117.5(9) . . ? C215 C214 C219 119.3(10) . . ? C213 C214 C219 123.1(8) . . ? C216 C215 C214 123.8(10) . . ? C216 C215 H215 118.1 . . ? C214 C215 H215 118.1 . . ? C215 C216 C217 118.0(9) . . ? C215 C216 C222 125.7(11) . . ? C217 C216 C222 116.3(9) . . ? C216 C217 C218 122.1(9) . . ? C216 C217 H217 118.9 . . ? C218 C217 H217 118.9 . . ? C217 C218 C213 118.4(9) . . ? C217 C218 C225 120.7(8) . . ? C213 C218 C225 120.8(8) . . ? C214 C219 C221 110.6(7) . . ? C214 C219 C220 111.5(8) . . ? C221 C219 C220 108.9(10) . . ? C214 C219 H219 108.6 . . ? C221 C219 H219 108.6 . . ? C220 C219 H219 108.6 . . ? C219 C220 H22B 109.5 . . ? C219 C220 H22C 109.5 . . ? H22B C220 H22C 109.5 . . ? C219 C220 H22D 109.5 . . ? H22B C220 H22D 109.5 . . ? H22C C220 H22D 109.5 . . ? C219 C221 H22E 109.5 . . ? C219 C221 H22F 109.5 . . ? H22E C221 H22F 109.5 . . ? C219 C221 H22G 109.5 . . ? H22E C221 H22G 109.5 . . ? H22F C221 H22G 109.5 . . ? C224 C222 C216 111.5(7) . . ? C224 C222 C223 105.9(8) . . ? C216 C222 C223 111.6(9) . . ? C224 C222 H222 109.2 . . ? C216 C222 H222 109.2 . . ? C223 C222 H222 109.2 . . ? C222 C223 H22H 109.5 . . ? C222 C223 H22I 109.5 . . ? H22H C223 H22I 109.5 . . ? C222 C223 H22J 109.5 . . ? H22H C223 H22J 109.5 . . ? H22I C223 H22J 109.5 . . ? C222 C224 H22K 109.5 . . ? C222 C224 H22L 109.5 . . ? H22K C224 H22L 109.5 . . ? C222 C224 H22M 109.5 . . ? H22K C224 H22M 109.5 . . ? H22L C224 H22M 109.5 . . ? C218 C225 C226 115.1(8) . . ? C218 C225 C227 110.6(8) . . ? C226 C225 C227 106.8(8) . . ? C218 C225 H225 108.0 . . ? C226 C225 H225 108.0 . . ? C227 C225 H225 108.0 . . ? C225 C226 H22N 109.5 . . ? C225 C226 H22O 109.5 . . ? H22N C226 H22O 109.5 . . ? C225 C226 H22P 109.5 . . ? H22N C226 H22P 109.5 . . ? H22O C226 H22P 109.5 . . ? C225 C227 H22Q 109.5 . . ? C225 C227 H22R 109.5 . . ? H22Q C227 H22R 109.5 . . ? C225 C227 H22S 109.5 . . ? H22Q C227 H22S 109.5 . . ? H22R C227 H22S 109.5 . . ? C229 C228 C233 119.1(7) . . ? C229 C228 C206 120.7(7) . . ? C233 C228 C206 120.2(8) . . ? C230 C229 C228 120.7(8) . . ? C230 C229 C23D 122.8(9) . . ? C228 C229 C23D 114.9(9) . . ? C230 C229 C234 111.8(11) . . ? C228 C229 C234 125.6(10) . . ? C229 C230 C231 121.6(8) . . ? C229 C230 H230 119.2 . . ? C231 C230 H230 119.2 . . ? C232 C231 C230 117.7(7) . . ? C232 C231 C237 123.2(7) . . ? C230 C231 C237 119.1(7) . . ? C231 C232 C233 123.2(7) . . ? C231 C232 H232 118.4 . . ? C233 C232 H232 118.4 . . ? C228 C233 C232 117.7(7) . . ? C228 C233 C240 122.5(7) . . ? C232 C233 C240 119.8(6) . . ? C236 C234 C235 103.4(11) . . ? C236 C234 C229 117.5(13) . . ? C235 C234 C229 111.9(13) . . ? C236 C234 H234 107.8 . . ? C235 C234 H234 107.8 . . ? C229 C234 H234 107.8 . . ? C234 C235 H23G 109.5 . . ? C234 C235 H23H 109.5 . . ? H23G C235 H23H 109.5 . . ? C234 C235 H23I 109.5 . . ? H23G C235 H23I 109.5 . . ? H23H C235 H23I 109.5 . . ? C234 C236 H23J 109.5 . . ? C234 C236 H23K 109.5 . . ? H23J C236 H23K 109.5 . . ? C234 C236 H23L 109.5 . . ? H23J C236 H23L 109.5 . . ? H23K C236 H23L 109.5 . . ? C23E C23D C23F 107.8(11) . . ? C23E C23D C229 115.2(12) . . ? C23F C23D C229 97.0(11) . . ? C23E C23D H23M 112.0 . . ? C23F C23D H23M 112.0 . . ? C229 C23D H23M 112.0 . . ? C23D C23E H23N 109.5 . . ? C23D C23E H23O 109.5 . . ? H23N C23E H23O 109.5 . . ? C23D C23E H23P 109.5 . . ? H23N C23E H23P 109.5 . . ? H23O C23E H23P 109.5 . . ? C23D C23F H23Q 109.5 . . ? C23D C23F H23R 109.5 . . ? H23Q C23F H23R 109.5 . . ? C23D C23F H23S 109.5 . . ? H23Q C23F H23S 109.5 . . ? H23R C23F H23S 109.5 . . ? C238 C237 C231 114.7(7) . . ? C238 C237 C239 109.2(7) . . ? C231 C237 C239 112.1(6) . . ? C238 C237 H237 106.8 . . ? C231 C237 H237 106.8 . . ? C239 C237 H237 106.8 . . ? C237 C238 H23T 109.5 . . ? C237 C238 H23U 109.5 . . ? H23T C238 H23U 109.5 . . ? C237 C238 H23V 109.5 . . ? H23T C238 H23V 109.5 . . ? H23U C238 H23V 109.5 . . ? C237 C239 H23W 109.5 . . ? C237 C239 H23X 109.5 . . ? H23W C239 H23X 109.5 . . ? C237 C239 H23Y 109.5 . . ? H23W C239 H23Y 109.5 . . ? H23X C239 H23Y 109.5 . . ? C233 C240 C242 112.3(6) . . ? C233 C240 C241 113.8(7) . . ? C242 C240 C241 108.0(7) . . ? C233 C240 H240 107.5 . . ? C242 C240 H240 107.5 . . ? C241 C240 H240 107.5 . . ? C240 C241 H24G 109.5 . . ? C240 C241 H24H 109.5 . . ? H24G C241 H24H 109.5 . . ? C240 C241 H24I 109.5 . . ? H24G C241 H24I 109.5 . . ? H24H C241 H24I 109.5 . . ? C240 C242 H24J 109.5 . . ? C240 C242 H24K 109.5 . . ? H24J C242 H24K 109.5 . . ? C240 C242 H24L 109.5 . . ? H24J C242 H24L 109.5 . . ? H24K C242 H24L 109.5 . . ? C248 C243 C244 120.7(6) . . ? C248 C243 Sn6 109.9(5) . . ? C244 C243 Sn6 126.8(5) . . ? C248 C243 Sn6A 130.8(5) . . ? C244 C243 Sn6A 105.4(5) . . ? C248 C243 Sn6B 133.3(6) . . ? C244 C243 Sn6B 102.4(5) . . ? C245 C244 C243 119.3(6) . . ? C245 C244 C255 123.1(6) . . ? C243 C244 C255 117.6(6) . . ? C246 C245 C244 118.9(6) . . ? C246 C245 C249 118.7(6) . . ? C244 C245 C249 122.4(6) . . ? C247 C246 C245 123.3(6) . . ? C247 C246 H246 118.4 . . ? C245 C246 H246 118.4 . . ? C246 C247 C248 117.1(6) . . ? C246 C247 C252 118.1(6) . . ? C248 C247 C252 124.8(6) . . ? C243 C248 C247 120.7(6) . . ? C243 C248 C270 119.9(6) . . ? C247 C248 C270 119.4(6) . . ? C250 C249 C245 112.6(7) . . ? C250 C249 C251 111.7(7) . . ? C245 C249 C251 109.5(7) . . ? C250 C249 H249 107.6 . . ? C245 C249 H249 107.6 . . ? C251 C249 H249 107.6 . . ? C249 C250 H25B 109.5 . . ? C249 C250 H25C 109.5 . . ? H25B C250 H25C 109.5 . . ? C249 C250 H25D 109.5 . . ? H25B C250 H25D 109.5 . . ? H25C C250 H25D 109.5 . . ? C249 C251 H25E 109.5 . . ? C249 C251 H25F 109.5 . . ? H25E C251 H25F 109.5 . . ? C249 C251 H25G 109.5 . . ? H25E C251 H25G 109.5 . . ? H25F C251 H25G 109.5 . . ? C247 C252 C254 111.3(6) . . ? C247 C252 C253 111.8(6) . . ? C254 C252 C253 110.0(7) . . ? C247 C252 H252 107.9 . . ? C254 C252 H252 107.9 . . ? C253 C252 H252 107.9 . . ? C252 C253 H25H 109.5 . . ? C252 C253 H25I 109.5 . . ? H25H C253 H25I 109.5 . . ? C252 C253 H25J 109.5 . . ? H25H C253 H25J 109.5 . . ? H25I C253 H25J 109.5 . . ? C252 C254 H25K 109.5 . . ? C252 C254 H25L 109.5 . . ? H25K C254 H25L 109.5 . . ? C252 C254 H25M 109.5 . . ? H25K C254 H25M 109.5 . . ? H25L C254 H25M 109.5 . . ? C256 C255 C260 119.7(7) . . ? C256 C255 C244 119.4(7) . . ? C260 C255 C244 120.8(6) . . ? C257 C256 C255 118.7(7) . . ? C257 C256 C261 119.5(8) . . ? C255 C256 C261 121.6(7) . . ? C258 C257 C256 122.8(8) . . ? C258 C257 H257 118.6 . . ? C256 C257 H257 118.6 . . ? C257 C258 C259 117.6(7) . . ? C257 C258 C264 120.3(8) . . ? C259 C258 C264 122.1(8) . . ? C258 C259 C260 122.8(7) . . ? C258 C259 H259 118.6 . . ? C260 C259 H259 118.6 . . ? C259 C260 C255 118.2(7) . . ? C259 C260 C267 120.9(7) . . ? C255 C260 C267 120.8(6) . . ? C256 C261 C263 114.1(9) . . ? C256 C261 C262 111.1(9) . . ? C263 C261 C262 107.0(9) . . ? C256 C261 H261 108.1 . . ? C263 C261 H261 108.1 . . ? C262 C261 H261 108.1 . . ? C261 C262 H2FC 109.5 . . ? C261 C262 H2FD 109.5 . . ? H2FC C262 H2FD 109.5 . . ? C261 C262 H2FE 109.5 . . ? H2FC C262 H2FE 109.5 . . ? H2FD C262 H2FE 109.5 . . ? C261 C263 H26G 109.5 . . ? C261 C263 H26H 109.5 . . ? H26G C263 H26H 109.5 . . ? C261 C263 H26I 109.5 . . ? H26G C263 H26I 109.5 . . ? H26H C263 H26I 109.5 . . ? H26K C26B H26L 109.5 . . ? H26K C26B H26M 109.5 . . ? H26L C26B H26M 109.5 . . ? H26N C26C H26O 109.5 . . ? H26N C26C H26P 109.5 . . ? H26O C26C H26P 109.5 . . ? C265 C264 C266 114.6(9) . . ? C265 C264 C258 114.1(7) . . ? C266 C264 C258 109.8(7) . . ? C265 C264 H264 105.8 . . ? C266 C264 H264 105.8 . . ? C258 C264 H264 105.8 . . ? C264 C265 H26Q 109.5 . . ? C264 C265 H26R 109.5 . . ? H26Q C265 H26R 109.5 . . ? C264 C265 H26S 109.5 . . ? H26Q C265 H26S 109.5 . . ? H26R C265 H26S 109.5 . . ? C264 C266 H26T 109.5 . . ? C264 C266 H26U 109.5 . . ? H26T C266 H26U 109.5 . . ? C264 C266 H26V 109.5 . . ? H26T C266 H26V 109.5 . . ? H26U C266 H26V 109.5 . . ? C268 C267 C260 114.9(6) . . ? C268 C267 C269 108.1(7) . . ? C260 C267 C269 111.3(6) . . ? C268 C267 H267 107.4 . . ? C260 C267 H267 107.4 . . ? C269 C267 H267 107.4 . . ? C267 C268 H26W 109.5 . . ? C267 C268 H26X 109.5 . . ? H26W C268 H26X 109.5 . . ? C267 C268 H26Y 109.5 . . ? H26W C268 H26Y 109.5 . . ? H26X C268 H26Y 109.5 . . ? C267 C269 H26Z 109.5 . . ? C267 C269 H2FA 109.5 . . ? H26Z C269 H2FA 109.5 . . ? C267 C269 H2FB 109.5 . . ? H26Z C269 H2FB 109.5 . . ? H2FA C269 H2FB 109.5 . . ? C275 C270 C271 119.1(7) . . ? C275 C270 C248 121.4(7) . . ? C271 C270 C248 119.2(7) . . ? C272 C271 C270 119.0(8) . . ? C272 C271 C276 117.6(7) . . ? C270 C271 C276 123.3(7) . . ? C273 C272 C271 122.9(9) . . ? C273 C272 H272 118.5 . . ? C271 C272 H272 118.5 . . ? C272 C273 C274 118.4(7) . . ? C272 C273 C279 120.3(8) . . ? C274 C273 C279 121.0(8) . . ? C273 C274 C275 121.0(7) . . ? C273 C274 H274 119.5 . . ? C275 C274 H274 119.5 . . ? C270 C275 C274 119.5(7) . . ? C270 C275 C282 121.8(7) . . ? C274 C275 C282 118.6(7) . . ? C277 C276 C278 110.0(9) . . ? C277 C276 C271 112.4(9) . . ? C278 C276 C271 111.0(8) . . ? C277 C276 H276 107.7 . . ? C278 C276 H276 107.7 . . ? C271 C276 H276 107.7 . . ? C276 C277 H27G 109.5 . . ? C276 C277 H27H 109.5 . . ? H27G C277 H27H 109.5 . . ? C276 C277 H27I 109.5 . . ? H27G C277 H27I 109.5 . . ? H27H C277 H27I 109.5 . . ? C276 C278 H27J 109.5 . . ? C276 C278 H27K 109.5 . . ? H27J C278 H27K 109.5 . . ? C276 C278 H27L 109.5 . . ? H27J C278 H27L 109.5 . . ? H27K C278 H27L 109.5 . . ? C280 C279 C281 112.9(9) . . ? C280 C279 C273 114.3(8) . . ? C281 C279 C273 109.4(8) . . ? C280 C279 H279 106.6 . . ? C281 C279 H279 106.6 . . ? C273 C279 H279 106.6 . . ? C279 C280 H28A 109.5 . . ? C279 C280 H28B 109.5 . . ? H28A C280 H28B 109.5 . . ? C279 C280 H28C 109.5 . . ? H28A C280 H28C 109.5 . . ? H28B C280 H28C 109.5 . . ? C279 C281 H28D 109.5 . . ? C279 C281 H28E 109.5 . . ? H28D C281 H28E 109.5 . . ? C279 C281 H28F 109.5 . . ? H28D C281 H28F 109.5 . . ? H28E C281 H28F 109.5 . . ? C284 C282 C275 111.6(7) . . ? C284 C282 C283 109.4(7) . . ? C275 C282 C283 113.0(7) . . ? C284 C282 H282 107.5 . . ? C275 C282 H282 107.5 . . ? C283 C282 H282 107.5 . . ? C282 C283 H28G 109.5 . . ? C282 C283 H28H 109.5 . . ? H28G C283 H28H 109.5 . . ? C282 C283 H28I 109.5 . . ? H28G C283 H28I 109.5 . . ? H28H C283 H28I 109.5 . . ? C282 C284 H28J 109.5 . . ? C282 C284 H28K 109.5 . . ? H28J C284 H28K 109.5 . . ? C282 C284 H28L 109.5 . . ? H28J C284 H28L 109.5 . . ? H28K C284 H28L 109.5 . . ? C302 C301 H30A 109.5 . . ? C302 C301 H30B 109.5 . . ? H30A C301 H30B 109.5 . . ? C302 C301 H30C 109.5 . . ? H30A C301 H30C 109.5 . . ? H30B C301 H30C 109.5 . . ? O303 C302 C301 97(2) . . ? O303 C302 H30D 112.4 . . ? C301 C302 H30D 112.4 . . ? O303 C302 H30E 112.4 . . ? C301 C302 H30E 112.4 . . ? H30D C302 H30E 110.0 . . ? C302 O303 C304 97(2) . . ? O303 C304 C305 91(3) . . ? O303 C304 H30F 113.4 . . ? C305 C304 H30F 113.4 . . ? O303 C304 H30G 113.4 . . ? C305 C304 H30G 113.4 . . ? H30F C304 H30G 110.7 . . ? C304 C305 H30H 109.5 . . ? C304 C305 H30I 109.5 . . ? H30H C305 H30I 109.5 . . ? C304 C305 H30J 109.5 . . ? H30H C305 H30J 109.5 . . ? H30I C305 H30J 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 C1 Sn1 Sn2 C43 152.2(3) . . . . ? Sn2 Sn1 C1 C2 38.4(7) . . . . ? Sn2 Sn1 C1 C6 -150.7(4) . . . . ? C6 C1 C2 C3 3.2(10) . . . . ? Sn1 C1 C2 C3 173.7(5) . . . . ? C6 C1 C2 C13 -176.8(6) . . . . ? Sn1 C1 C2 C13 -6.3(9) . . . . ? C1 C2 C3 C4 0.3(10) . . . . ? C13 C2 C3 C4 -179.6(6) . . . . ? C1 C2 C3 C7 -176.9(6) . . . . ? C13 C2 C3 C7 3.1(10) . . . . ? C2 C3 C4 C5 -3.0(10) . . . . ? C7 C3 C4 C5 174.4(6) . . . . ? C3 C4 C5 C6 2.0(10) . . . . ? C3 C4 C5 C10 -177.4(6) . . . . ? C2 C1 C6 C5 -4.3(10) . . . . ? Sn1 C1 C6 C5 -175.5(5) . . . . ? C2 C1 C6 C28 169.7(6) . . . . ? Sn1 C1 C6 C28 -1.4(8) . . . . ? C4 C5 C6 C1 1.7(10) . . . . ? C10 C5 C6 C1 -178.9(6) . . . . ? C4 C5 C6 C28 -172.1(6) . . . . ? C10 C5 C6 C28 7.3(10) . . . . ? C4 C3 C7 C9 -59.0(8) . . . . ? C2 C3 C7 C9 118.3(7) . . . . ? C4 C3 C7 C8 64.1(8) . . . . ? C2 C3 C7 C8 -118.6(7) . . . . ? C4 C5 C10 C11 45.1(8) . . . . ? C6 C5 C10 C11 -134.3(7) . . . . ? C4 C5 C10 C12 -77.0(8) . . . . ? C6 C5 C10 C12 103.6(7) . . . . ? C1 C2 C13 C18 82.9(10) . . . . ? C3 C2 C13 C18 -97.2(10) . . . . ? C1 C2 C13 C14 -99.7(8) . . . . ? C3 C2 C13 C14 80.2(9) . . . . ? C18 C13 C14 C15 -3.4(12) . . . . ? C2 C13 C14 C15 179.2(7) . . . . ? C18 C13 C14 C19 178.8(8) . . . . ? C2 C13 C14 C19 1.4(11) . . . . ? C13 C14 C15 C16 3.1(11) . . . . ? C19 C14 C15 C16 -179.0(7) . . . . ? C14 C15 C16 C17 -2.7(12) . . . . ? C14 C15 C16 C22 175.6(7) . . . . ? C15 C16 C17 C18 2.5(14) . . . . ? C22 C16 C17 C18 -175.7(9) . . . . ? C14 C13 C18 C17 3.3(14) . . . . ? C2 C13 C18 C17 -179.3(8) . . . . ? C14 C13 C18 C25D 159.2(9) . . . . ? C2 C13 C18 C25D -23.4(14) . . . . ? C14 C13 C18 C25 -158.3(10) . . . . ? C2 C13 C18 C25 19.1(15) . . . . ? C16 C17 C18 C13 -2.9(16) . . . . ? C16 C17 C18 C25D -159.4(10) . . . . ? C16 C17 C18 C25 160.1(10) . . . . ? C13 C14 C19 C20 98.1(8) . . . . ? C15 C14 C19 C20 -79.7(8) . . . . ? C13 C14 C19 C21 -136.9(7) . . . . ? C15 C14 C19 C21 45.3(9) . . . . ? C15 C16 C22 C24 -113.9(10) . . . . ? C17 C16 C22 C24 64.3(11) . . . . ? C15 C16 C22 C23 3.7(11) . . . . ? C17 C16 C22 C23 -178.1(9) . . . . ? C13 C18 C25 C27 105.5(17) . . . . ? C17 C18 C25 C27 -56.4(18) . . . . ? C25D C18 C25 C27 -158(2) . . . . ? C13 C18 C25 C26 -126.5(14) . . . . ? C17 C18 C25 C26 71.5(16) . . . . ? C25D C18 C25 C26 -30.2(13) . . . . ? C13 C18 C25D C27D -133.3(13) . . . . ? C17 C18 C25D C27D 22.7(17) . . . . ? C25 C18 C25D C27D 119.9(19) . . . . ? C13 C18 C25D C26D 108.0(13) . . . . ? C17 C18 C25D C26D -96.0(14) . . . . ? C25 C18 C25D C26D 1.2(19) . . . . ? C1 C6 C28 C33 94.3(8) . . . . ? C5 C6 C28 C33 -91.7(8) . . . . ? C1 C6 C28 C29 -84.9(8) . . . . ? C5 C6 C28 C29 89.1(8) . . . . ? C33 C28 C29 C30 -1.9(10) . . . . ? C6 C28 C29 C30 177.3(6) . . . . ? C33 C28 C29 C34 173.7(7) . . . . ? C6 C28 C29 C34 -7.0(10) . . . . ? C28 C29 C30 C31 1.8(11) . . . . ? C34 C29 C30 C31 -174.0(7) . . . . ? C29 C30 C31 C32 -1.8(12) . . . . ? C29 C30 C31 C37 177.8(7) . . . . ? C30 C31 C32 C33 2.0(12) . . . . ? C37 C31 C32 C33 -177.6(7) . . . . ? C29 C28 C33 C32 2.0(10) . . . . ? C6 C28 C33 C32 -177.2(6) . . . . ? C29 C28 C33 C40 -175.7(6) . . . . ? C6 C28 C33 C40 5.2(10) . . . . ? C31 C32 C33 C28 -2.1(11) . . . . ? C31 C32 C33 C40 175.7(7) . . . . ? C28 C29 C34 C35 130.1(8) . . . . ? C30 C29 C34 C35 -54.2(10) . . . . ? C28 C29 C34 C36 -106.7(8) . . . . ? C30 C29 C34 C36 69.0(8) . . . . ? C32 C31 C37 C39 108.9(11) . . . . ? C30 C31 C37 C39 -70.7(12) . . . . ? C32 C31 C37 C38 -124.5(10) . . . . ? C30 C31 C37 C38 55.9(12) . . . . ? C28 C33 C40 C42 126.0(8) . . . . ? C32 C33 C40 C42 -51.7(9) . . . . ? C28 C33 C40 C41 -109.3(8) . . . . ? C32 C33 C40 C41 73.0(9) . . . . ? Sn1 Sn2 C43 C44 43.1(6) . . . . ? Sn1 Sn2 C43 C48 -143.5(4) . . . . ? C48 C43 C44 C45 1.3(10) . . . . ? Sn2 C43 C44 C45 174.4(5) . . . . ? C48 C43 C44 C55 178.9(6) . . . . ? Sn2 C43 C44 C55 -8.0(8) . . . . ? C43 C44 C45 C46 0.5(11) . . . . ? C55 C44 C45 C46 -176.9(7) . . . . ? C43 C44 C45 C49 -178.7(7) . . . . ? C55 C44 C45 C49 3.9(12) . . . . ? C44 C45 C46 C47 0.7(12) . . . . ? C49 C45 C46 C47 179.9(8) . . . . ? C45 C46 C47 C48 -3.7(11) . . . . ? C45 C46 C47 C52 175.0(7) . . . . ? C46 C47 C48 C43 5.4(10) . . . . ? C52 C47 C48 C43 -173.3(6) . . . . ? C46 C47 C48 C70 -175.6(7) . . . . ? C52 C47 C48 C70 5.7(10) . . . . ? C44 C43 C48 C47 -4.3(10) . . . . ? Sn2 C43 C48 C47 -177.9(5) . . . . ? C44 C43 C48 C70 176.7(6) . . . . ? Sn2 C43 C48 C70 3.1(8) . . . . ? C44 C45 C49 C51 -118.1(9) . . . . ? C46 C45 C49 C51 62.7(10) . . . . ? C44 C45 C49 C50 118.9(9) . . . . ? C46 C45 C49 C50 -60.3(11) . . . . ? C46 C47 C52 C54 -62.5(9) . . . . ? C48 C47 C52 C54 116.2(8) . . . . ? C46 C47 C52 C53 60.9(9) . . . . ? C48 C47 C52 C53 -120.4(8) . . . . ? C45 C44 C55 C56 -93.1(9) . . . . ? C43 C44 C55 C56 89.3(8) . . . . ? C45 C44 C55 C60 87.2(8) . . . . ? C43 C44 C55 C60 -90.3(8) . . . . ? C60 C55 C56 C57 3.8(10) . . . . ? C44 C55 C56 C57 -175.8(6) . . . . ? C60 C55 C56 C61 -173.2(6) . . . . ? C44 C55 C56 C61 7.2(10) . . . . ? C55 C56 C57 C58 -1.1(11) . . . . ? C61 C56 C57 C58 176.0(7) . . . . ? C56 C57 C58 C59 -0.9(11) . . . . ? C56 C57 C58 C64 -179.5(6) . . . . ? C57 C58 C59 C60 0.1(11) . . . . ? C64 C58 C59 C60 178.7(7) . . . . ? C58 C59 C60 C55 2.6(10) . . . . ? C58 C59 C60 C67 -176.7(6) . . . . ? C56 C55 C60 C59 -4.6(9) . . . . ? C44 C55 C60 C59 175.1(6) . . . . ? C56 C55 C60 C67 174.7(6) . . . . ? C44 C55 C60 C67 -5.6(9) . . . . ? C57 C56 C61 C63 61.9(9) . . . . ? C55 C56 C61 C63 -121.1(8) . . . . ? C57 C56 C61 C62 -62.7(10) . . . . ? C55 C56 C61 C62 114.2(8) . . . . ? C57 C58 C64 C65 101.8(9) . . . . ? C59 C58 C64 C65 -76.7(10) . . . . ? C57 C58 C64 C66 -22.6(10) . . . . ? C59 C58 C64 C66 158.9(7) . . . . ? C59 C60 C67 C68 53.9(9) . . . . ? C55 C60 C67 C68 -125.4(7) . . . . ? C59 C60 C67 C69 -72.5(8) . . . . ? C55 C60 C67 C69 108.2(7) . . . . ? C47 C48 C70 C75 -93.0(9) . . . . ? C43 C48 C70 C75 85.9(9) . . . . ? C47 C48 C70 C71 85.9(9) . . . . ? C43 C48 C70 C71 -95.2(8) . . . . ? C75 C70 C71 C72 -0.5(13) . . . . ? C48 C70 C71 C72 -179.5(8) . . . . ? C75 C70 C71 C76 179.1(8) . . . . ? C48 C70 C71 C76 0.2(12) . . . . ? C70 C71 C72 C73 -0.1(16) . . . . ? C76 C71 C72 C73 -179.8(10) . . . . ? C71 C72 C73 C74 2.2(18) . . . . ? C71 C72 C73 C79 160.7(12) . . . . ? C71 C72 C73 C79A -174.2(11) . . . . ? C72 C73 C74 C75 -3.7(17) . . . . ? C79 C73 C74 C75 -165.8(10) . . . . ? C79A C73 C74 C75 172.4(11) . . . . ? C71 C70 C75 C74 -1.0(12) . . . . ? C48 C70 C75 C74 177.9(7) . . . . ? C71 C70 C75 C82 -175.3(7) . . . . ? C48 C70 C75 C82 3.5(11) . . . . ? C73 C74 C75 C70 3.1(14) . . . . ? C73 C74 C75 C82 177.5(9) . . . . ? C72 C71 C76 C77 -76.9(11) . . . . ? C70 C71 C76 C77 103.4(10) . . . . ? C72 C71 C76 C78 47.5(12) . . . . ? C70 C71 C76 C78 -132.2(9) . . . . ? C72 C73 C79 C81 -99(3) . . . . ? C74 C73 C79 C81 61(2) . . . . ? C79A C73 C79 C81 -168(4) . . . . ? C72 C73 C79 C80 108.6(18) . . . . ? C74 C73 C79 C80 -91.0(17) . . . . ? C79A C73 C79 C80 39(2) . . . . ? C72 C73 C79A C80A 30(2) . . . . ? C74 C73 C79A C80A -146.5(16) . . . . ? C79 C73 C79A C80A 154(4) . . . . ? C72 C73 C79A C81A -94.2(16) . . . . ? C74 C73 C79A C81A 89.6(16) . . . . ? C79 C73 C79A C81A 30(3) . . . . ? C70 C75 C82 C83 -123.6(8) . . . . ? C74 C75 C82 C83 62.1(10) . . . . ? C70 C75 C82 C84 113.1(9) . . . . ? C74 C75 C82 C84 -61.2(10) . . . . ? C101 Sn3 Sn4 C143 154.1(3) . . . . ? Sn4 Sn3 C101 C106 -147.3(4) . . . . ? Sn4 Sn3 C101 C102 41.2(6) . . . . ? C106 C101 C102 C103 0.8(10) . . . . ? Sn3 C101 C102 C103 172.1(6) . . . . ? C106 C101 C102 C113 -178.9(6) . . . . ? Sn3 C101 C102 C113 -7.6(8) . . . . ? C101 C102 C103 C104 1.4(12) . . . . ? C113 C102 C103 C104 -178.9(7) . . . . ? C101 C102 C103 C107 -178.7(8) . . . . ? C113 C102 C103 C107 1.0(13) . . . . ? C102 C103 C104 C105 -3.1(14) . . . . ? C107 C103 C104 C105 177.0(9) . . . . ? C103 C104 C105 C106 2.5(13) . . . . ? C103 C104 C105 C110 -176.0(8) . . . . ? C104 C105 C106 C101 -0.2(11) . . . . ? C110 C105 C106 C101 178.2(6) . . . . ? C104 C105 C106 C128 -176.4(7) . . . . ? C110 C105 C106 C128 2.1(11) . . . . ? C102 C101 C106 C105 -1.4(10) . . . . ? Sn3 C101 C106 C105 -173.0(5) . . . . ? C102 C101 C106 C128 175.0(6) . . . . ? Sn3 C101 C106 C128 3.5(7) . . . . ? C102 C103 C107 C109 -111.3(10) . . . . ? C104 C103 C107 C109 68.6(11) . . . . ? C102 C103 C107 C108 124.1(9) . . . . ? C104 C103 C107 C108 -56.0(13) . . . . ? C104 C105 C110 C112 58.3(9) . . . . ? C106 C105 C110 C112 -120.2(8) . . . . ? C104 C105 C110 C111 -65.6(11) . . . . ? C106 C105 C110 C111 115.9(9) . . . . ? C103 C102 C113 C114 83.9(9) . . . . ? C101 C102 C113 C114 -96.3(8) . . . . ? C103 C102 C113 C118 -94.4(9) . . . . ? C101 C102 C113 C118 85.4(8) . . . . ? C118 C113 C114 C115 -4.4(10) . . . . ? C102 C113 C114 C115 177.3(6) . . . . ? C118 C113 C114 C119 177.4(6) . . . . ? C102 C113 C114 C119 -1.0(9) . . . . ? C113 C114 C115 C116 4.0(10) . . . . ? C119 C114 C115 C116 -177.7(6) . . . . ? C114 C115 C116 C117 -1.2(10) . . . . ? C114 C115 C116 C122 176.5(6) . . . . ? C115 C116 C117 C118 -1.2(11) . . . . ? C122 C116 C117 C118 -178.7(7) . . . . ? C116 C117 C118 C113 0.7(11) . . . . ? C116 C117 C118 C125 179.4(7) . . . . ? C114 C113 C118 C117 2.1(10) . . . . ? C102 C113 C118 C117 -179.6(6) . . . . ? C114 C113 C118 C125 -176.5(6) . . . . ? C102 C113 C118 C125 1.8(10) . . . . ? C115 C114 C119 C120 -81.0(8) . . . . ? C113 C114 C119 C120 97.3(7) . . . . ? C115 C114 C119 C121 43.1(8) . . . . ? C113 C114 C119 C121 -138.6(6) . . . . ? C117 C116 C122 C123 -20.7(10) . . . . ? C115 C116 C122 C123 161.7(7) . . . . ? C117 C116 C122 C124 104.5(9) . . . . ? C115 C116 C122 C124 -73.0(9) . . . . ? C117 C118 C125 C126 52.2(9) . . . . ? C113 C118 C125 C126 -129.2(8) . . . . ? C117 C118 C125 C127 -71.4(10) . . . . ? C113 C118 C125 C127 107.2(8) . . . . ? C105 C106 C128 C133 -93.6(8) . . . . ? C101 C106 C128 C133 90.1(8) . . . . ? C105 C106 C128 C129 88.2(8) . . . . ? C101 C106 C128 C129 -88.1(7) . . . . ? C133 C128 C129 C130 -4.3(9) . . . . ? C106 C128 C129 C130 173.9(6) . . . . ? C133 C128 C129 C134 171.1(6) . . . . ? C106 C128 C129 C134 -10.6(9) . . . . ? C128 C129 C130 C131 0.5(10) . . . . ? C134 C129 C130 C131 -175.1(7) . . . . ? C129 C130 C131 C132 2.8(11) . . . . ? C129 C130 C131 C137 178.9(7) . . . . ? C130 C131 C132 C133 -2.3(11) . . . . ? C137 C131 C132 C133 -178.6(7) . . . . ? C131 C132 C133 C128 -1.6(11) . . . . ? C131 C132 C133 C140 178.7(7) . . . . ? C129 C128 C133 C132 4.8(10) . . . . ? C106 C128 C133 C132 -173.4(6) . . . . ? C129 C128 C133 C140 -175.4(6) . . . . ? C106 C128 C133 C140 6.4(10) . . . . ? C130 C129 C134 C136 55.4(8) . . . . ? C128 C129 C134 C136 -120.1(7) . . . . ? C130 C129 C134 C135 -67.4(8) . . . . ? C128 C129 C134 C135 117.1(7) . . . . ? C130 C131 C137 C138 24.6(11) . . . . ? C132 C131 C137 C138 -159.3(7) . . . . ? C130 C131 C137 C139 -99.4(11) . . . . ? C132 C131 C137 C139 76.6(10) . . . . ? C132 C133 C140 C141 59.8(9) . . . . ? C128 C133 C140 C141 -119.9(7) . . . . ? C132 C133 C140 C142 -61.4(10) . . . . ? C128 C133 C140 C142 118.8(8) . . . . ? Sn3 Sn4 C143 C148 -147.4(5) . . . . ? Sn3 Sn4 C143 C144 38.8(6) . . . . ? C148 C143 C144 C145 4.3(11) . . . . ? Sn4 C143 C144 C145 177.9(5) . . . . ? C148 C143 C144 C155 -176.6(6) . . . . ? Sn4 C143 C144 C155 -3.1(9) . . . . ? C143 C144 C145 C146 -3.3(11) . . . . ? C155 C144 C145 C146 177.7(7) . . . . ? C143 C144 C145 C149 178.8(7) . . . . ? C155 C144 C145 C149 -0.2(11) . . . . ? C144 C145 C146 C147 -0.9(12) . . . . ? C149 C145 C146 C147 177.0(7) . . . . ? C145 C146 C147 C148 4.1(12) . . . . ? C145 C146 C147 C152 -178.4(7) . . . . ? C144 C143 C148 C147 -1.0(11) . . . . ? Sn4 C143 C148 C147 -174.9(6) . . . . ? C144 C143 C148 C170 173.5(6) . . . . ? Sn4 C143 C148 C170 -0.4(8) . . . . ? C146 C147 C148 C143 -3.1(11) . . . . ? C152 C147 C148 C143 179.5(7) . . . . ? C146 C147 C148 C170 -177.4(7) . . . . ? C152 C147 C148 C170 5.2(11) . . . . ? C144 C145 C149 C151 -123.7(8) . . . . ? C146 C145 C149 C151 58.4(9) . . . . ? C144 C145 C149 C150 112.4(8) . . . . ? C146 C145 C149 C150 -65.5(10) . . . . ? C148 C147 C152 C154 108.3(8) . . . . ? C146 C147 C152 C154 -69.0(10) . . . . ? C148 C147 C152 C153 -127.3(8) . . . . ? C146 C147 C152 C153 55.3(10) . . . . ? C145 C144 C155 C160 -102.5(8) . . . . ? C143 C144 C155 C160 78.4(9) . . . . ? C145 C144 C155 C156 79.2(9) . . . . ? C143 C144 C155 C156 -99.8(8) . . . . ? C160 C155 C156 C157 1.3(9) . . . . ? C144 C155 C156 C157 179.6(6) . . . . ? C160 C155 C156 C161 179.5(6) . . . . ? C144 C155 C156 C161 -2.3(9) . . . . ? C155 C156 C157 C158 0.4(10) . . . . ? C161 C156 C157 C158 -177.8(6) . . . . ? C156 C157 C158 C159 -1.1(10) . . . . ? C156 C157 C158 C164 174.1(6) . . . . ? C157 C158 C159 C160 0.0(10) . . . . ? C164 C158 C159 C160 -175.0(7) . . . . ? C156 C155 C160 C159 -2.3(10) . . . . ? C144 C155 C160 C159 179.4(6) . . . . ? C156 C155 C160 C167 -178.4(6) . . . . ? C144 C155 C160 C167 3.4(10) . . . . ? C158 C159 C160 C155 1.7(10) . . . . ? C158 C159 C160 C167 177.9(6) . . . . ? C157 C156 C161 C162 -79.2(8) . . . . ? C155 C156 C161 C162 102.6(7) . . . . ? C157 C156 C161 C163 45.6(9) . . . . ? C155 C156 C161 C163 -132.5(6) . . . . ? C159 C158 C164 C165 -26.5(10) . . . . ? C157 C158 C164 C165 158.7(7) . . . . ? C159 C158 C164 C166 98.0(8) . . . . ? C157 C158 C164 C166 -76.8(8) . . . . ? C155 C160 C167 C168 -131.1(7) . . . . ? C159 C160 C167 C168 52.9(8) . . . . ? C155 C160 C167 C169 105.5(8) . . . . ? C159 C160 C167 C169 -70.6(9) . . . . ? C143 C148 C170 C171 -87.3(8) . . . . ? C147 C148 C170 C171 87.1(8) . . . . ? C143 C148 C170 C175 87.8(8) . . . . ? C147 C148 C170 C175 -97.7(8) . . . . ? C175 C170 C171 C172 -1.8(9) . . . . ? C148 C170 C171 C172 173.5(6) . . . . ? C175 C170 C171 C176 173.1(6) . . . . ? C148 C170 C171 C176 -11.6(9) . . . . ? C170 C171 C172 C173 -0.5(9) . . . . ? C176 C171 C172 C173 -175.6(6) . . . . ? C171 C172 C173 C174 1.8(9) . . . . ? C171 C172 C173 C179 178.5(6) . . . . ? C172 C173 C174 C175 -0.8(10) . . . . ? C179 C173 C174 C175 -177.6(6) . . . . ? C173 C174 C175 C170 -1.5(10) . . . . ? C173 C174 C175 C182 175.5(6) . . . . ? C171 C170 C175 C174 2.7(9) . . . . ? C148 C170 C175 C174 -172.5(6) . . . . ? C171 C170 C175 C182 -174.3(6) . . . . ? C148 C170 C175 C182 10.6(9) . . . . ? C172 C171 C176 C177 -66.4(8) . . . . ? C170 C171 C176 C177 118.6(7) . . . . ? C172 C171 C176 C178 58.5(8) . . . . ? C170 C171 C176 C178 -116.4(7) . . . . ? C172 C173 C179 C180 25.8(9) . . . . ? C174 C173 C179 C180 -157.6(6) . . . . ? C172 C173 C179 C181 -99.3(7) . . . . ? C174 C173 C179 C181 77.3(8) . . . . ? C174 C175 C182 C183 67.3(8) . . . . ? C170 C175 C182 C183 -115.8(7) . . . . ? C174 C175 C182 C184 -55.4(9) . . . . ? C170 C175 C182 C184 121.5(7) . . . . ? C201 Sn5 Sn6 C243 166.3(3) . . . . ? C201 Sn5A Sn6A C243 164.6(3) . . . . ? C201 Sn5B Sn6B C243 -162.4(6) . . . . ? Sn6 Sn5 C201 C206 55.0(9) . . . . ? Sn6 Sn5 C201 C202 -138.4(5) . . . . ? Sn6 Sn5 C201 Sn5A -12.8(2) . . . . ? Sn6 Sn5 C201 Sn5B -36.5(7) . . . . ? Sn6A Sn5A C201 C206 -140.6(5) . . . . ? Sn6A Sn5A C201 C202 68.2(9) . . . . ? Sn6A Sn5A C201 Sn5 -9.7(2) . . . . ? Sn6A Sn5A C201 Sn5B 75.8(18) . . . . ? Sn6B Sn5B C201 C206 -86.1(9) . . . . ? Sn6B Sn5B C201 C202 127.6(8) . . . . ? Sn6B Sn5B C201 Sn5 31.4(4) . . . . ? Sn6B Sn5B C201 Sn5A -46.0(14) . . . . ? C206 C201 C202 C203 1.2(13) . . . . ? Sn5 C201 C202 C203 -166.3(6) . . . . ? Sn5A C201 C202 C203 147.7(7) . . . . ? Sn5B C201 C202 C203 145.4(8) . . . . ? C206 C201 C202 C213 -176.7(8) . . . . ? Sn5 C201 C202 C213 15.9(9) . . . . ? Sn5A C201 C202 C213 -30.2(12) . . . . ? Sn5B C201 C202 C213 -32.5(11) . . . . ? C201 C202 C203 C204 2.7(11) . . . . ? C213 C202 C203 C204 -179.5(7) . . . . ? C201 C202 C203 C207 -176.3(7) . . . . ? C213 C202 C203 C207 1.4(12) . . . . ? C202 C203 C204 C205 -4.3(11) . . . . ? C207 C203 C204 C205 174.8(7) . . . . ? C203 C204 C205 C206 1.9(11) . . . . ? C203 C204 C205 C210 179.8(7) . . . . ? C202 C201 C206 C205 -3.5(13) . . . . ? Sn5 C201 C206 C205 161.5(6) . . . . ? Sn5A C201 C206 C205 -157.2(6) . . . . ? Sn5B C201 C206 C205 -146.3(8) . . . . ? C202 C201 C206 C228 172.9(8) . . . . ? Sn5 C201 C206 C228 -22.0(12) . . . . ? Sn5A C201 C206 C228 19.2(9) . . . . ? Sn5B C201 C206 C228 30.2(11) . . . . ? C204 C205 C206 C201 2.0(11) . . . . ? C210 C205 C206 C201 -175.7(8) . . . . ? C204 C205 C206 C228 -174.4(7) . . . . ? C210 C205 C206 C228 7.9(12) . . . . ? C202 C203 C207 C209 -115.6(8) . . . . ? C204 C203 C207 C209 65.4(9) . . . . ? C202 C203 C207 C208 121.1(8) . . . . ? C204 C203 C207 C208 -58.0(9) . . . . ? C204 C205 C210 C211 58.0(10) . . . . ? C206 C205 C210 C211 -124.2(8) . . . . ? C204 C205 C210 C212 -65.1(9) . . . . ? C206 C205 C210 C212 112.6(8) . . . . ? C203 C202 C213 C214 91.6(10) . . . . ? C201 C202 C213 C214 -90.6(10) . . . . ? C203 C202 C213 C218 -90.4(10) . . . . ? C201 C202 C213 C218 87.4(9) . . . . ? C218 C213 C214 C215 -2.4(12) . . . . ? C202 C213 C214 C215 175.5(7) . . . . ? C218 C213 C214 C219 173.7(8) . . . . ? C202 C213 C214 C219 -8.4(12) . . . . ? C213 C214 C215 C216 1.7(12) . . . . ? C219 C214 C215 C216 -174.6(8) . . . . ? C214 C215 C216 C217 -0.5(13) . . . . ? C214 C215 C216 C222 177.6(8) . . . . ? C215 C216 C217 C218 0.0(13) . . . . ? C222 C216 C217 C218 -178.3(7) . . . . ? C216 C217 C218 C213 -0.8(13) . . . . ? C216 C217 C218 C225 176.3(8) . . . . ? C214 C213 C218 C217 2.0(12) . . . . ? C202 C213 C218 C217 -176.0(7) . . . . ? C214 C213 C218 C225 -175.1(8) . . . . ? C202 C213 C218 C225 6.9(11) . . . . ? C215 C214 C219 C221 58.7(9) . . . . ? C213 C214 C219 C221 -117.4(10) . . . . ? C215 C214 C219 C220 -62.7(12) . . . . ? C213 C214 C219 C220 121.2(10) . . . . ? C215 C216 C222 C224 -104.5(11) . . . . ? C217 C216 C222 C224 73.6(11) . . . . ? C215 C216 C222 C223 13.7(12) . . . . ? C217 C216 C222 C223 -168.2(8) . . . . ? C217 C218 C225 C226 56.2(11) . . . . ? C213 C218 C225 C226 -126.8(9) . . . . ? C217 C218 C225 C227 -65.0(10) . . . . ? C213 C218 C225 C227 112.0(9) . . . . ? C201 C206 C228 C229 -85.5(11) . . . . ? C205 C206 C228 C229 90.8(10) . . . . ? C201 C206 C228 C233 92.7(10) . . . . ? C205 C206 C228 C233 -91.0(10) . . . . ? C233 C228 C229 C230 -3.1(15) . . . . ? C206 C228 C229 C230 175.1(9) . . . . ? C233 C228 C229 C23D -169.2(9) . . . . ? C206 C228 C229 C23D 9.0(14) . . . . ? C233 C228 C229 C234 160.1(11) . . . . ? C206 C228 C229 C234 -21.8(16) . . . . ? C228 C229 C230 C231 3.3(16) . . . . ? C23D C229 C230 C231 168.2(10) . . . . ? C234 C229 C230 C231 -162.0(10) . . . . ? C229 C230 C231 C232 -2.1(14) . . . . ? C229 C230 C231 C237 175.5(9) . . . . ? C230 C231 C232 C233 0.8(12) . . . . ? C237 C231 C232 C233 -176.7(7) . . . . ? C229 C228 C233 C232 1.8(12) . . . . ? C206 C228 C233 C232 -176.4(7) . . . . ? C229 C228 C233 C240 -176.4(8) . . . . ? C206 C228 C233 C240 5.4(11) . . . . ? C231 C232 C233 C228 -0.7(11) . . . . ? C231 C232 C233 C240 177.6(7) . . . . ? C230 C229 C234 C236 63.6(16) . . . . ? C228 C229 C234 C236 -100.8(17) . . . . ? C23D C229 C234 C236 -177(3) . . . . ? C230 C229 C234 C235 -55.9(17) . . . . ? C228 C229 C234 C235 139.7(13) . . . . ? C23D C229 C234 C235 63.2(18) . . . . ? C230 C229 C23D C23E -41.1(17) . . . . ? C228 C229 C23D C23E 124.6(12) . . . . ? C234 C229 C23D C23E -116(2) . . . . ? C230 C229 C23D C23F 72.4(14) . . . . ? C228 C229 C23D C23F -121.9(12) . . . . ? C234 C229 C23D C23F -2.5(18) . . . . ? C232 C231 C237 C238 -32.5(11) . . . . ? C230 C231 C237 C238 150.1(9) . . . . ? C232 C231 C237 C239 92.8(10) . . . . ? C230 C231 C237 C239 -84.6(10) . . . . ? C228 C233 C240 C242 118.9(8) . . . . ? C232 C233 C240 C242 -59.2(9) . . . . ? C228 C233 C240 C241 -118.0(8) . . . . ? C232 C233 C240 C241 63.9(9) . . . . ? Sn5 Sn6 C243 C248 -142.5(4) . . . . ? Sn5 Sn6 C243 C244 55.8(7) . . . . ? Sn5 Sn6 C243 Sn6A -11.9(2) . . . . ? Sn5 Sn6 C243 Sn6B 52.5(6) . . . . ? Sn5A Sn6A C243 C248 56.6(7) . . . . ? Sn5A Sn6A C243 C244 -143.8(4) . . . . ? Sn5A Sn6A C243 Sn6 -14.0(2) . . . . ? Sn5A Sn6A C243 Sn6B -53.9(5) . . . . ? Sn5B Sn6B C243 C248 -55.5(10) . . . . ? Sn5B Sn6B C243 C244 146.8(7) . . . . ? Sn5B Sn6B C243 Sn6 -35.9(6) . . . . ? Sn5B Sn6B C243 Sn6A 47.6(6) . . . . ? C248 C243 C244 C245 1.1(10) . . . . ? Sn6 C243 C244 C245 161.0(5) . . . . ? Sn6A C243 C244 C245 -161.1(5) . . . . ? Sn6B C243 C244 C245 162.4(6) . . . . ? C248 C243 C244 C255 179.5(6) . . . . ? Sn6 C243 C244 C255 -20.6(9) . . . . ? Sn6A C243 C244 C255 17.4(7) . . . . ? Sn6B C243 C244 C255 -19.2(7) . . . . ? C243 C244 C245 C246 -0.7(10) . . . . ? C255 C244 C245 C246 -179.0(7) . . . . ? C243 C244 C245 C249 178.4(7) . . . . ? C255 C244 C245 C249 0.0(11) . . . . ? C244 C245 C246 C247 -1.1(10) . . . . ? C249 C245 C246 C247 179.9(7) . . . . ? C245 C246 C247 C248 2.3(10) . . . . ? C245 C246 C247 C252 -176.8(6) . . . . ? C244 C243 C248 C247 0.1(10) . . . . ? Sn6 C243 C248 C247 -162.8(5) . . . . ? Sn6A C243 C248 C247 157.2(5) . . . . ? Sn6B C243 C248 C247 -154.3(6) . . . . ? C244 C243 C248 C270 177.3(7) . . . . ? Sn6 C243 C248 C270 14.3(8) . . . . ? Sn6A C243 C248 C270 -25.7(10) . . . . ? Sn6B C243 C248 C270 22.8(11) . . . . ? C246 C247 C248 C243 -1.8(10) . . . . ? C252 C247 C248 C243 177.2(6) . . . . ? C246 C247 C248 C270 -178.9(6) . . . . ? C252 C247 C248 C270 0.1(10) . . . . ? C246 C245 C249 C250 -54.3(9) . . . . ? C244 C245 C249 C250 126.7(8) . . . . ? C246 C245 C249 C251 70.7(9) . . . . ? C244 C245 C249 C251 -108.4(8) . . . . ? C246 C247 C252 C254 -65.9(8) . . . . ? C248 C247 C252 C254 115.2(8) . . . . ? C246 C247 C252 C253 57.6(9) . . . . ? C248 C247 C252 C253 -121.4(8) . . . . ? C245 C244 C255 C256 86.6(9) . . . . ? C243 C244 C255 C256 -91.7(9) . . . . ? C245 C244 C255 C260 -95.9(9) . . . . ? C243 C244 C255 C260 85.8(9) . . . . ? C260 C255 C256 C257 -1.0(12) . . . . ? C244 C255 C256 C257 176.5(8) . . . . ? C260 C255 C256 C261 -175.5(8) . . . . ? C244 C255 C256 C261 2.0(12) . . . . ? C255 C256 C257 C258 2.9(14) . . . . ? C261 C256 C257 C258 177.6(9) . . . . ? C256 C257 C258 C259 -2.2(14) . . . . ? C256 C257 C258 C264 176.9(9) . . . . ? C257 C258 C259 C260 -0.5(12) . . . . ? C264 C258 C259 C260 -179.6(7) . . . . ? C258 C259 C260 C255 2.3(11) . . . . ? C258 C259 C260 C267 179.1(7) . . . . ? C256 C255 C260 C259 -1.5(11) . . . . ? C244 C255 C260 C259 -179.0(6) . . . . ? C256 C255 C260 C267 -178.3(7) . . . . ? C244 C255 C260 C267 4.2(10) . . . . ? C257 C256 C261 C263 41.3(13) . . . . ? C255 C256 C261 C263 -144.2(10) . . . . ? C257 C256 C261 C262 -79.8(11) . . . . ? C255 C256 C261 C262 94.6(11) . . . . ? C257 C258 C264 C265 137.7(10) . . . . ? C259 C258 C264 C265 -43.2(12) . . . . ? C257 C258 C264 C266 -92.0(11) . . . . ? C259 C258 C264 C266 87.1(11) . . . . ? C259 C260 C267 C268 47.7(9) . . . . ? C255 C260 C267 C268 -135.6(7) . . . . ? C259 C260 C267 C269 -75.5(8) . . . . ? C255 C260 C267 C269 101.2(8) . . . . ? C243 C248 C270 C275 84.5(9) . . . . ? C247 C248 C270 C275 -98.4(9) . . . . ? C243 C248 C270 C271 -89.6(9) . . . . ? C247 C248 C270 C271 87.6(9) . . . . ? C275 C270 C271 C272 2.8(13) . . . . ? C248 C270 C271 C272 176.9(8) . . . . ? C275 C270 C271 C276 179.0(8) . . . . ? C248 C270 C271 C276 -6.8(13) . . . . ? C270 C271 C272 C273 -1.3(15) . . . . ? C276 C271 C272 C273 -177.7(9) . . . . ? C271 C272 C273 C274 0.9(15) . . . . ? C271 C272 C273 C279 174.4(9) . . . . ? C272 C273 C274 C275 -2.0(13) . . . . ? C279 C273 C274 C275 -175.5(8) . . . . ? C271 C270 C275 C274 -3.9(12) . . . . ? C248 C270 C275 C274 -177.9(7) . . . . ? C271 C270 C275 C282 179.7(7) . . . . ? C248 C270 C275 C282 5.6(11) . . . . ? C273 C274 C275 C270 3.6(12) . . . . ? C273 C274 C275 C282 -179.9(7) . . . . ? C272 C271 C276 C277 -63.1(12) . . . . ? C270 C271 C276 C277 120.7(10) . . . . ? C272 C271 C276 C278 60.7(11) . . . . ? C270 C271 C276 C278 -115.6(9) . . . . ? C272 C273 C279 C280 154.3(10) . . . . ? C274 C273 C279 C280 -32.4(14) . . . . ? C272 C273 C279 C281 -78.0(11) . . . . ? C274 C273 C279 C281 95.4(11) . . . . ? C270 C275 C282 C284 112.8(8) . . . . ? C274 C275 C282 C284 -63.7(9) . . . . ? C270 C275 C282 C283 -123.4(8) . . . . ? C274 C275 C282 C283 60.1(9) . . . . ? C301 C302 O303 C304 175(2) . . . . ? C302 O303 C304 C305 -178(3) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 2.208 _refine_diff_density_min -1.447 _refine_diff_density_rms 0.118 # Attachment '4-ClArSnCl.cif.txt' data_1342ffmip _database_code_depnum_ccdc_archive 'CCDC 771275' #TrackingRef '4-ClArSnCl.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C60 H72 Cl4 Sn2' _chemical_formula_sum 'C60 H72 Cl4 Sn2' _chemical_formula_weight 1172.36 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P c c n' _symmetry_space_group_name_Hall '-P 2ab 2ac' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z' '-x, y+1/2, -z+1/2' 'x+1/2, -y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z' 'x, -y-1/2, z-1/2' '-x-1/2, y, z-1/2' _cell_length_a 20.3965(16) _cell_length_b 15.7884(13) _cell_length_c 17.1574(14) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5525.2(8) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 6488 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 25.50 _exptl_crystal_description Block _exptl_crystal_colour Colorless _exptl_crystal_size_max 0.17 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.409 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2400 _exptl_absorpt_coefficient_mu 1.134 _exptl_absorpt_correction_type 'Empirical, SADABS (multi-scan)' _exptl_absorpt_correction_T_min 0.8306 _exptl_absorpt_correction_T_max 0.9048 _exptl_absorpt_process_details 'SADABS 2.10 (Sheldrick, 2003)' _exptl_special_details ; A colorless block with approximate orthogonal dimensions 0.17 x 0.16 x 0.09mm3 was placed and optically centered on the Bruker SMART APEX CCD system at -183\%C. The initial unit cell was indexed using a least-squares analysis of a random set of reflections collected from three series of 0.3? wide omega-scans, 10 seconds per frame, and 30 frames per series that were well distributed in reciprocal space. Four omega-scan data frame series were collected [MoKa] with 0.3?wide scans, 70 seconds per frame and 606 frames collected per series at varying phi angles (phi=0? 90? 180? 270?. The crystal to detector distance was 4.97cm, thus providing a complete sphere of data to 2thetamax=51.45? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method '\w and \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 37024 _diffrn_reflns_av_R_equivalents 0.0849 _diffrn_reflns_av_sigmaI/netI 0.0466 _diffrn_reflns_limit_h_min -24 _diffrn_reflns_limit_h_max 24 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.00 _diffrn_reflns_theta_max 25.25 _reflns_number_total 5003 _reflns_number_gt 4136 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (1.0.27) (Bruker, 2004)' _computing_cell_refinement 'SAINT (7.23A) (Bruker, 2005)' _computing_data_reduction 'SAINT (7.23A) (Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL97 _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. All crystallographic calculations were performed on a Personal computer (PC) with a Pentium 3.20GHz processor and 1GB of extended memory. A total of 63506 reflections were collected and corrected for Lorentz and polarization effects and absorption using Blessing's method as incorporated into the program SADABS with 5831 unique. The SHELXTL program package was implemented to determine the probable space group and set up the initial files. System symmetry, systematic absences and intensity statistics indicated the centrosymmetric orthorhombic space group Pccn (no. 56). The structure was determined by direct methods with the successful location of a majority of the molecule within the asymmetric unit using the program XS; the remaining half of the molecule generated via an inversion center. The structure was refined with XL. The 63506 data collected were merged based upon identical indices yielding 41033 data [R(int)=0.0372] that were truncated to 2Theta=50.50?yielding 37024 data that were further merged during least-squares refinement to 5003 unique data [R(int)=0.0849]. Least-squares difference-Fourier cycles were required to locate the remaining non-hydrogen atoms. All non-hydrogen atoms were refined anisotropically. Hydrogen atoms were idealized throughout the final refinement stages. Due to the disorder present and optimized for the Sn(u2-Cl)2Sn molecule center it is apparent that this rotational disorder is absorbed in the thermal parameters of the accompanying ligand and they are therefore larger than normal, showing signs of entire ligand libration. A multitude of twin analyses of the data were performed with an additional variety of approaches regarding data reduction and handling with 2, 3, and 4 component approaches all yielding results but these were all similar and the thermal ellipsoids on the ligand atoms were not reduced so the original single component approach was optimized and refined to convergence. ; _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^)+(0.0215P)^2^+25.3285P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5003 _refine_ls_number_parameters 324 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0691 _refine_ls_R_factor_gt 0.0568 _refine_ls_wR_factor_ref 0.1304 _refine_ls_wR_factor_gt 0.1251 _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 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.40782(2) 0.53290(3) 0.01556(3) 0.03219(15) Uani 0.66 1 d P . 1 Cl1 Cl 0.48343(9) 0.41526(11) 0.06163(10) 0.0367(4) Uani 0.66 1 d P . 1 Sn1A Sn 0.42330(5) 0.46896(6) 0.05718(6) 0.0322(2) Uani 0.34 1 d P . 2 Cl1A Cl 0.55146(19) 0.4354(2) 0.0602(2) 0.0404(9) Uani 0.34 1 d P . 2 Cl2 Cl 0.34180(7) 0.77538(8) 0.32104(8) 0.0438(3) Uani 1 1 d . . . C1 C 0.4108(2) 0.5962(3) 0.1317(3) 0.0383(12) Uani 1 1 d . . . C2 C 0.3492(2) 0.5854(3) 0.1677(3) 0.0262(9) Uani 1 1 d . . . C3 C 0.3278(2) 0.6392(3) 0.2264(2) 0.0231(9) Uani 1 1 d . . . H3 H 0.2861 0.6316 0.2501 0.028 Uiso 1 1 calc R . . C4 C 0.3690(2) 0.7043(3) 0.2495(2) 0.0259(9) Uani 1 1 d . . . C5 C 0.4304(2) 0.7147(3) 0.2175(2) 0.0299(10) Uani 1 1 d . . . H5 H 0.4581 0.7587 0.2358 0.036 Uiso 1 1 calc R . . C6 C 0.4518(2) 0.6616(3) 0.1593(3) 0.0351(11) Uani 1 1 d . . . C7 C 0.3057(2) 0.5127(3) 0.1430(3) 0.0258(9) Uani 1 1 d . . . C8 C 0.2599(2) 0.5226(3) 0.0826(2) 0.0296(10) Uani 1 1 d . . . C9 C 0.2225(2) 0.4537(3) 0.0593(3) 0.0374(12) Uani 1 1 d . . . H9 H 0.1913 0.4602 0.0186 0.045 Uiso 1 1 calc R . . C10 C 0.2302(3) 0.3758(3) 0.0945(3) 0.0422(13) Uani 1 1 d . . . H10 H 0.2039 0.3291 0.0789 0.051 Uiso 1 1 calc R . . C11 C 0.2757(3) 0.3662(3) 0.1519(4) 0.0455(14) Uani 1 1 d . . . H11 H 0.2812 0.3121 0.1752 0.055 Uiso 1 1 calc R . . C12 C 0.3142(2) 0.4332(3) 0.1776(3) 0.0345(11) Uani 1 1 d . . . C13 C 0.2494(3) 0.6091(3) 0.0452(3) 0.0424(13) Uani 1 1 d . . . H13 H 0.2906 0.6427 0.0523 0.051 Uiso 1 1 calc R . . C14 C 0.1942(3) 0.6559(3) 0.0869(4) 0.0518(15) Uani 1 1 d . . . H14A H 0.1864 0.7104 0.0613 0.078 Uiso 1 1 calc R . . H14B H 0.2065 0.6655 0.1414 0.078 Uiso 1 1 calc R . . H14C H 0.1541 0.6217 0.0849 0.078 Uiso 1 1 calc R . . C15 C 0.2352(4) 0.6044(5) -0.0423(3) 0.076(2) Uani 1 1 d . . . H15A H 0.1921 0.5785 -0.0507 0.115 Uiso 1 1 calc R . . H15B H 0.2689 0.5701 -0.0680 0.115 Uiso 1 1 calc R . . H15C H 0.2354 0.6616 -0.0644 0.115 Uiso 1 1 calc R . . C16 C 0.3621(3) 0.4206(3) 0.2448(4) 0.0465(14) Uani 1 1 d . . . H16 H 0.3944 0.4682 0.2434 0.056 Uiso 1 1 calc R . . C17 C 0.4002(3) 0.3379(4) 0.2390(4) 0.0512(15) Uani 1 1 d . . . H17A H 0.3709 0.2902 0.2500 0.077 Uiso 1 1 calc R . . H17B H 0.4361 0.3382 0.2770 0.077 Uiso 1 1 calc R . . H17C H 0.4183 0.3320 0.1863 0.077 Uiso 1 1 calc R . . C18 C 0.3267(3) 0.4247(5) 0.3221(4) 0.076(2) Uani 1 1 d . . . H18A H 0.2967 0.3765 0.3265 0.115 Uiso 1 1 calc R . . H18B H 0.3017 0.4776 0.3253 0.115 Uiso 1 1 calc R . . H18C H 0.3587 0.4227 0.3646 0.115 Uiso 1 1 calc R . . C19 C 0.5209(3) 0.6735(4) 0.1291(3) 0.0439(14) Uani 1 1 d . . . C20 C 0.5334(3) 0.7380(4) 0.0751(3) 0.0545(18) Uani 1 1 d . . . C21 C 0.5973(4) 0.7494(5) 0.0483(4) 0.068(2) Uani 1 1 d . . . H21 H 0.6065 0.7929 0.0116 0.081 Uiso 1 1 calc R . . C22 C 0.6461(4) 0.6991(5) 0.0742(5) 0.077(3) Uani 1 1 d . . . H22 H 0.6891 0.7068 0.0541 0.093 Uiso 1 1 calc R . . C23 C 0.6350(3) 0.6365(4) 0.1293(5) 0.067(2) Uani 1 1 d . . . H23 H 0.6704 0.6027 0.1477 0.080 Uiso 1 1 calc R . . C24 C 0.5708(3) 0.6232(4) 0.1581(3) 0.0462(14) Uani 1 1 d . . . C25 C 0.4802(3) 0.7982(5) 0.0446(3) 0.068(2) Uani 1 1 d . . . H25 H 0.4393 0.7848 0.0744 0.081 Uiso 1 1 calc R . . C26 C 0.4945(4) 0.8878(7) 0.0588(7) 0.120(4) Uani 1 1 d . . . H26A H 0.5047 0.8962 0.1141 0.180 Uiso 1 1 calc R . . H26B H 0.4561 0.9220 0.0449 0.180 Uiso 1 1 calc R . . H26C H 0.5320 0.9052 0.0271 0.180 Uiso 1 1 calc R . . C27 C 0.4642(8) 0.7871(7) -0.0389(5) 0.184(8) Uani 1 1 d . . . H27A H 0.4381 0.8353 -0.0570 0.277 Uiso 1 1 calc R . . H27B H 0.4391 0.7347 -0.0459 0.277 Uiso 1 1 calc R . . H27C H 0.5049 0.7838 -0.0692 0.277 Uiso 1 1 calc R . . C28 C 0.5592(3) 0.5588(3) 0.2233(4) 0.0488(14) Uani 1 1 d . . . H28 H 0.5152 0.5329 0.2140 0.059 Uiso 1 1 calc R . . C29 C 0.5565(3) 0.6026(4) 0.3026(4) 0.0572(16) Uani 1 1 d . . . H29A H 0.5981 0.6317 0.3123 0.086 Uiso 1 1 calc R . . H29B H 0.5490 0.5602 0.3433 0.086 Uiso 1 1 calc R . . H29C H 0.5206 0.6438 0.3029 0.086 Uiso 1 1 calc R . . C30 C 0.6087(4) 0.4867(4) 0.2263(5) 0.080(2) Uani 1 1 d . . . H30A H 0.6106 0.4588 0.1753 0.120 Uiso 1 1 calc R . . H30B H 0.5952 0.4456 0.2660 0.120 Uiso 1 1 calc R . . H30C H 0.6520 0.5093 0.2394 0.120 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 0.0340(3) 0.0379(3) 0.0247(2) -0.0099(2) 0.0035(2) -0.0128(2) Cl1 0.0431(10) 0.0330(9) 0.0340(9) -0.0058(7) 0.0125(8) -0.0114(8) Sn1A 0.0324(5) 0.0267(5) 0.0376(5) -0.0129(4) 0.0139(4) -0.0065(4) Cl1A 0.050(2) 0.046(2) 0.0248(17) -0.0080(15) -0.0114(15) 0.0202(17) Cl2 0.0603(8) 0.0326(6) 0.0386(7) -0.0191(5) -0.0013(6) -0.0056(6) C1 0.032(3) 0.051(3) 0.031(3) -0.017(2) 0.008(2) -0.017(2) C2 0.028(2) 0.026(2) 0.025(2) -0.0029(18) 0.0019(18) -0.0070(19) C3 0.029(2) 0.021(2) 0.019(2) 0.0013(17) 0.0004(17) -0.0035(17) C4 0.039(3) 0.020(2) 0.019(2) -0.0010(17) -0.0022(19) -0.0035(19) C5 0.043(3) 0.027(2) 0.020(2) 0.0051(18) -0.008(2) -0.015(2) C6 0.036(3) 0.050(3) 0.019(2) -0.001(2) 0.0019(19) -0.020(2) C7 0.025(2) 0.024(2) 0.028(2) -0.0105(18) 0.0047(18) -0.0029(18) C8 0.033(2) 0.031(2) 0.025(2) -0.0077(19) 0.0045(18) -0.008(2) C9 0.039(3) 0.043(3) 0.031(3) -0.007(2) -0.001(2) -0.014(2) C10 0.042(3) 0.027(3) 0.057(3) -0.013(2) -0.007(3) -0.013(2) C11 0.046(3) 0.019(2) 0.071(4) -0.006(2) -0.012(3) -0.004(2) C12 0.030(2) 0.022(2) 0.052(3) -0.006(2) -0.010(2) 0.0016(19) C13 0.055(3) 0.042(3) 0.030(3) 0.011(2) -0.013(2) -0.026(3) C14 0.059(4) 0.033(3) 0.064(4) 0.016(3) -0.019(3) -0.009(3) C15 0.119(6) 0.077(5) 0.033(3) 0.019(3) -0.024(4) -0.052(5) C16 0.043(3) 0.020(2) 0.076(4) 0.001(3) -0.027(3) 0.002(2) C17 0.047(3) 0.049(3) 0.057(4) 0.022(3) 0.012(3) 0.023(3) C18 0.076(5) 0.085(5) 0.068(4) -0.043(4) -0.041(4) 0.049(4) C19 0.038(3) 0.065(4) 0.028(3) -0.022(2) 0.005(2) -0.029(3) C20 0.055(3) 0.083(4) 0.026(3) -0.013(3) 0.006(2) -0.048(3) C21 0.066(4) 0.082(5) 0.055(4) -0.027(4) 0.026(3) -0.047(4) C22 0.063(5) 0.060(4) 0.109(6) -0.039(4) 0.046(5) -0.041(4) C23 0.043(3) 0.052(4) 0.105(6) -0.039(4) 0.023(3) -0.024(3) C24 0.043(3) 0.044(3) 0.051(3) -0.024(3) 0.012(3) -0.024(3) C25 0.058(4) 0.117(6) 0.027(3) 0.029(3) -0.013(3) -0.055(4) C26 0.060(5) 0.141(9) 0.160(10) -0.067(8) -0.040(6) 0.012(5) C27 0.41(2) 0.091(7) 0.054(5) -0.008(5) -0.110(9) 0.027(10) C28 0.040(3) 0.035(3) 0.071(4) -0.021(3) 0.003(3) -0.008(2) C29 0.076(4) 0.038(3) 0.058(4) -0.009(3) -0.016(3) 0.005(3) C30 0.068(5) 0.046(4) 0.126(7) -0.023(4) 0.019(4) -0.004(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C1 2.230(5) . ? Sn1 Cl1 2.540(2) . ? Sn1 Cl1 2.7099(18) 5_665 ? Cl1 Sn1 2.7099(18) 5_665 ? Sn1A C1 2.395(5) . ? Sn1A Cl1A 2.569(4) 5_665 ? Sn1A Cl1A 2.668(4) . ? Cl1A Sn1A 2.569(4) 5_665 ? Cl2 C4 1.753(4) . ? C1 C6 1.410(6) . ? C1 C2 1.410(6) . ? C2 C3 1.388(6) . ? C2 C7 1.511(6) . ? C3 C4 1.386(6) . ? C3 H3 0.9500 . ? C4 C5 1.376(7) . ? C5 C6 1.376(7) . ? C5 H5 0.9500 . ? C6 C19 1.513(7) . ? C7 C12 1.399(6) . ? C7 C8 1.405(6) . ? C8 C9 1.387(6) . ? C8 C13 1.525(7) . ? C9 C10 1.379(7) . ? C9 H9 0.9500 . ? C10 C11 1.361(8) . ? C10 H10 0.9500 . ? C11 C12 1.389(7) . ? C11 H11 0.9500 . ? C12 C16 1.525(7) . ? C13 C14 1.525(8) . ? C13 C15 1.531(7) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C18 1.511(9) . ? C16 C17 1.523(7) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C24 1.384(9) . ? C19 C20 1.400(8) . ? C20 C21 1.393(8) . ? C20 C25 1.534(10) . ? C21 C22 1.349(11) . ? C21 H21 0.9500 . ? C22 C23 1.387(11) . ? C22 H22 0.9500 . ? C23 C24 1.416(8) . ? C23 H23 0.9500 . ? C24 C28 1.529(8) . ? C25 C26 1.464(11) . ? C25 C27 1.481(9) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C30 1.522(9) . ? C28 C29 1.526(8) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Sn1 Cl1 91.90(16) . . ? C1 Sn1 Cl1 106.23(13) . 5_665 ? Cl1 Sn1 Cl1 82.88(6) . 5_665 ? Sn1 Cl1 Sn1 97.12(6) . 5_665 ? C1 Sn1A Cl1A 86.95(15) . 5_665 ? C1 Sn1A Cl1A 105.13(15) . . ? Cl1A Sn1A Cl1A 86.30(11) 5_665 . ? Sn1A Cl1A Sn1A 93.69(11) 5_665 . ? C6 C1 C2 118.1(4) . . ? C6 C1 Sn1 130.0(3) . . ? C2 C1 Sn1 108.2(3) . . ? C6 C1 Sn1A 136.9(4) . . ? C2 C1 Sn1A 103.1(3) . . ? Sn1 C1 Sn1A 31.78(7) . . ? C3 C2 C1 121.6(4) . . ? C3 C2 C7 119.0(4) . . ? C1 C2 C7 119.4(4) . . ? C4 C3 C2 118.1(4) . . ? C4 C3 H3 121.0 . . ? C2 C3 H3 121.0 . . ? C5 C4 C3 121.7(4) . . ? C5 C4 Cl2 119.4(3) . . ? C3 C4 Cl2 118.9(3) . . ? C6 C5 C4 120.4(4) . . ? C6 C5 H5 119.8 . . ? C4 C5 H5 119.8 . . ? C5 C6 C1 120.1(4) . . ? C5 C6 C19 117.9(4) . . ? C1 C6 C19 121.9(4) . . ? C12 C7 C8 119.7(4) . . ? C12 C7 C2 119.4(4) . . ? C8 C7 C2 120.9(4) . . ? C9 C8 C7 119.5(4) . . ? C9 C8 C13 120.3(4) . . ? C7 C8 C13 120.2(4) . . ? C10 C9 C8 120.6(5) . . ? C10 C9 H9 119.7 . . ? C8 C9 H9 119.7 . . ? C11 C10 C9 119.6(5) . . ? C11 C10 H10 120.2 . . ? C9 C10 H10 120.2 . . ? C10 C11 C12 122.0(5) . . ? C10 C11 H11 119.0 . . ? C12 C11 H11 119.0 . . ? C11 C12 C7 118.6(4) . . ? C11 C12 C16 120.2(5) . . ? C7 C12 C16 121.1(4) . . ? C8 C13 C14 109.8(4) . . ? C8 C13 C15 113.3(5) . . ? C14 C13 C15 110.1(5) . . ? C8 C13 H13 107.8 . . ? C14 C13 H13 107.8 . . ? C15 C13 H13 107.8 . . ? 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 . . ? C18 C16 C17 109.8(5) . . ? C18 C16 C12 110.6(5) . . ? C17 C16 C12 112.9(5) . . ? C18 C16 H16 107.8 . . ? C17 C16 H16 107.8 . . ? C12 C16 H16 107.8 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 121.4(5) . . ? C24 C19 C6 119.4(5) . . ? C20 C19 C6 119.1(6) . . ? C21 C20 C19 118.9(7) . . ? C21 C20 C25 117.9(6) . . ? C19 C20 C25 123.2(5) . . ? C22 C21 C20 120.3(7) . . ? C22 C21 H21 119.8 . . ? C20 C21 H21 119.8 . . ? C21 C22 C23 121.7(6) . . ? C21 C22 H22 119.2 . . ? C23 C22 H22 119.2 . . ? C22 C23 C24 119.6(7) . . ? C22 C23 H23 120.2 . . ? C24 C23 H23 120.2 . . ? C19 C24 C23 118.1(6) . . ? C19 C24 C28 122.1(5) . . ? C23 C24 C28 119.8(6) . . ? C26 C25 C27 108.6(7) . . ? C26 C25 C20 113.7(5) . . ? C27 C25 C20 114.3(8) . . ? C26 C25 H25 106.6 . . ? C27 C25 H25 106.6 . . ? C20 C25 H25 106.6 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C30 C28 C29 109.4(6) . . ? C30 C28 C24 114.8(5) . . ? C29 C28 C24 110.9(4) . . ? C30 C28 H28 107.1 . . ? C29 C28 H28 107.1 . . ? C24 C28 H28 107.1 . . ? 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 . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 0.944 _refine_diff_density_min -0.753 _refine_diff_density_rms 0.087 # Attachment '4-Me3SiArCl.cif.txt' data_1390ffmi _database_code_depnum_ccdc_archive 'CCDC 771276' #TrackingRef '4-Me3SiArCl.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H90 Cl2 Si2 Sn2, 2(C7 H8)' _chemical_formula_sum 'C80 H106 Cl2 Si2 Sn2' _chemical_formula_weight 1432.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' Cl Cl 0.1484 0.1585 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.3422(6) _cell_length_b 12.9163(6) _cell_length_c 15.1478(11) _cell_angle_alpha 112.0530(10) _cell_angle_beta 103.2470(10) _cell_angle_gamma 103.1560(10) _cell_volume 1877.17(19) _cell_formula_units_Z 1 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 6975 _cell_measurement_theta_min 2.87 _cell_measurement_theta_max 30.49 _exptl_crystal_description Block _exptl_crystal_colour Light_Yellow/Orange _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.267 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 748 _exptl_absorpt_coefficient_mu 0.809 _exptl_absorpt_correction_type 'Empirical, SADABS (multi-scan)' _exptl_absorpt_correction_T_min 0.6813 _exptl_absorpt_correction_T_max 0.8511 _exptl_absorpt_process_details 'SADABS 2.10 (Sheldrick, 2003)' _exptl_special_details ; A light yellow somewhat orange block with approximate orthogonal dimensions 0.51 x 0.30 x 0.21mm3 was placed and optically centered on the Bruker SMART APEX (Ref 1) CCD system at -183\%C (90K). The initial unit cell was indexed using a least-squares analysis of a random set of reflections collected from three series of 0.3?wide omega-scans, 10 seconds per frame, and 30 frames per series that were well distributed in reciprocal space. Four omega-scan data frame series were collected [MoK ] with 0.3?wide scans, 25 seconds per frame and 606 frames were collected, at varying phi angles (phi=0? 90? 180? 270?, for each series. The crystal to detector distance was 4.97cm, thus providing a complete sphere of data with processing to 2Thetamax=61.13? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method '\w and \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 16959 _diffrn_reflns_av_R_equivalents 0.0167 _diffrn_reflns_av_sigmaI/netI 0.0234 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.78 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8632 _reflns_number_gt 8096 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (2.1.2.21) (Bruker, 2005)' _computing_cell_refinement 'SAINT (7.23A) (Bruker, 2005)' _computing_data_reduction 'SAINT (7.23A) (Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL97 _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. All crystallographic calculations were performed on a Personal computer (PC) with a Pentium 3.20GHz processor and 1GB of extended memory. A total of 30635 reflections were collected and corrected for Lorentz and polarization effects and absorption using Blessing's method as incorporated into the program SADABS (Ref 2,3) with 11428 unique. The SHELXTL(Ref 4) program package was implemented to determine the probable space group and set up the initial files. System symmetry, lack of systematic absences and intensity statistics indicated the centrosymmetric triclinic space group P-1 (no. 2). The structure was determined by direct methods with the successful location of a majority of the molecule of interest using the program XS(Ref 5). The structure was refined with XL(Ref 5). The 30635 data collected were merged based upon identical indices yielding 22154 data [R(int)=0.0193] that were truncated to 2thetamax=55.00deg resulting in 16959 data that were further merged in least-squares refinement to 8632 unique data [R(int)=0.0167]. All full-occupancy non-hydrogen atoms were refined anisotropically. Hydrogen atoms were placed in calculated idealized positions throughout the final convergence process. A toluene molecule was optimized for disorder. The final structure was refined to convergence with R(F)=3.12%, wR(F2)=8.13%, GOF=1.047 for all 8632 unique reflections [R(F)=2.95%, wR(F2)=8.00% for those 8096 data with Fo > 4sigma(Fo)]. The final difference-Fourier map was featureless indicating that the structure is both correct and complete. An empirical correction for extinction was also attempted but found to be within one standard deviation of its calculated value and therefore not applied. References: 1. Bruker (2004) SMART APEX(Version 2.1.2.21) and SAINT (Version 7.23a). Bruker AXS Inc., Madison, Wisconsin, USA. 2. An Empirical Correction for Absorption Anisotropy, Blessing, R. H. (1995). Acta Cryst., A51, 33-38. 3. Sheldrick, G.M., SADABS (2003) Version 2.10, 'Siemens Area Detector Absorption Correction' Universit\"at G ttingen: G ttingen, Germany. 4. Sheldrick, G.M., (2002). SHELXTL. Version 6.1. Bruker AXS Inc., Madison, Wisconsin, USA. 5. Sheldrick, G. M., (1997). SHELXS97 and SHELXL97. Universit\"at G ttingen: G ttingen, Germany. ; _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^)+(0.0495P)^2^+1.3239P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8632 _refine_ls_number_parameters 397 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0312 _refine_ls_R_factor_gt 0.0295 _refine_ls_wR_factor_ref 0.0813 _refine_ls_wR_factor_gt 0.0800 _refine_ls_goodness_of_fit_ref 1.047 _refine_ls_restrained_S_all 1.047 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.934976(12) 0.854786(10) 0.509773(9) 0.01895(5) Uani 1 1 d . . . Cl1 Cl 0.84860(4) 0.96046(4) 0.40539(3) 0.02296(10) Uani 1 1 d . . . Si1 Si 0.57354(5) 0.95180(4) 0.82650(4) 0.01801(10) Uani 1 1 d . . . C1 C 0.83304(16) 0.91657(15) 0.61961(13) 0.0154(3) Uani 1 1 d . . . C2 C 0.82670(16) 1.02815(15) 0.67946(13) 0.0151(3) Uani 1 1 d . . . C3 C 0.74872(16) 1.03439(15) 0.73927(13) 0.0161(3) Uani 1 1 d . . . H3 H 0.7484 1.1105 0.7811 0.019 Uiso 1 1 calc R . . C4 C 0.67117(16) 0.93426(16) 0.74070(13) 0.0161(3) Uani 1 1 d . . . C5 C 0.67710(17) 0.82425(16) 0.68060(13) 0.0165(3) Uani 1 1 d . . . H5 H 0.6251 0.7539 0.6787 0.020 Uiso 1 1 calc R . . C6 C 0.75792(16) 0.81580(15) 0.62337(13) 0.0150(3) Uani 1 1 d . . . C7 C 0.90192(17) 1.14646(15) 0.68852(13) 0.0156(3) Uani 1 1 d . . . C8 C 1.02869(17) 1.21040(16) 0.75983(14) 0.0179(3) Uani 1 1 d . . . C9 C 1.09087(18) 1.32535(17) 0.77471(15) 0.0222(4) Uani 1 1 d . . . H9 H 1.1766 1.3689 0.8218 0.027 Uiso 1 1 calc R . . C10 C 1.02980(19) 1.37683(17) 0.72200(16) 0.0238(4) Uani 1 1 d . . . H10 H 1.0736 1.4551 0.7332 0.029 Uiso 1 1 calc R . . C11 C 0.90492(19) 1.31433(16) 0.65295(15) 0.0212(4) Uani 1 1 d . . . H11 H 0.8635 1.3505 0.6174 0.025 Uiso 1 1 calc R . . C12 C 0.83897(17) 1.19854(15) 0.63481(13) 0.0167(3) Uani 1 1 d . . . C13 C 1.09420(18) 1.15930(17) 0.82492(14) 0.0208(4) Uani 1 1 d . . . H13 H 1.0638 1.0709 0.7833 0.025 Uiso 1 1 calc R . . C14 C 1.24195(19) 1.2065(2) 0.85988(16) 0.0282(4) Uani 1 1 d . . . H14A H 1.2749 1.2913 0.9081 0.042 Uiso 1 1 calc R . . H14B H 1.2687 1.1963 0.8009 0.042 Uiso 1 1 calc R . . H14C H 1.2768 1.1623 0.8929 0.042 Uiso 1 1 calc R . . C15 C 1.0549(2) 1.1844(2) 0.91953(16) 0.0294(4) Uani 1 1 d . . . H15A H 1.0968 1.1497 0.9594 0.044 Uiso 1 1 calc R . . H15B H 0.9609 1.1488 0.8984 0.044 Uiso 1 1 calc R . . H15C H 1.0821 1.2707 0.9610 0.044 Uiso 1 1 calc R . . C16 C 0.69979(18) 1.13383(16) 0.56066(14) 0.0200(3) Uani 1 1 d . . . H16 H 0.6822 1.0463 0.5342 0.024 Uiso 1 1 calc R . . C17 C 0.6746(2) 1.1611(2) 0.46934(16) 0.0278(4) Uani 1 1 d . . . H17A H 0.6798 1.2443 0.4922 0.042 Uiso 1 1 calc R . . H17B H 0.5884 1.1085 0.4197 0.042 Uiso 1 1 calc R . . H17C H 0.7397 1.1480 0.4377 0.042 Uiso 1 1 calc R . . C18 C 0.60348(19) 1.16382(19) 0.61364(16) 0.0256(4) Uani 1 1 d . . . H18A H 0.6097 1.1359 0.6658 0.038 Uiso 1 1 calc R . . H18B H 0.5156 1.1245 0.5635 0.038 Uiso 1 1 calc R . . H18C H 0.6235 1.2502 0.6455 0.038 Uiso 1 1 calc R . . C19 C 0.77315(17) 0.69743(15) 0.57088(13) 0.0157(3) Uani 1 1 d . . . C20 C 0.69231(17) 0.61515(15) 0.47050(14) 0.0178(3) Uani 1 1 d . . . C21 C 0.71501(19) 0.50911(16) 0.42403(15) 0.0217(4) Uani 1 1 d . . . H21 H 0.6618 0.4532 0.3561 0.026 Uiso 1 1 calc R . . C22 C 0.81412(19) 0.48443(17) 0.47574(16) 0.0235(4) Uani 1 1 d . . . H22 H 0.8286 0.4122 0.4431 0.028 Uiso 1 1 calc R . . C23 C 0.89183(19) 0.56497(17) 0.57473(16) 0.0223(4) Uani 1 1 d . . . H23 H 0.9589 0.5470 0.6098 0.027 Uiso 1 1 calc R . . C24 C 0.87335(17) 0.67221(16) 0.62386(14) 0.0182(3) Uani 1 1 d . . . C25 C 0.58239(18) 0.63830(16) 0.41138(14) 0.0202(3) Uani 1 1 d . . . H25 H 0.5824 0.7184 0.4558 0.024 Uiso 1 1 calc R . . C26 C 0.6005(2) 0.6409(2) 0.31494(17) 0.0324(5) Uani 1 1 d . . . H26A H 0.5927 0.5612 0.2672 0.049 Uiso 1 1 calc R . . H26B H 0.6863 0.6974 0.3326 0.049 Uiso 1 1 calc R . . H26C H 0.5342 0.6658 0.2833 0.049 Uiso 1 1 calc R . . C27 C 0.4520(2) 0.5462(2) 0.3849(2) 0.0324(5) Uani 1 1 d . . . H27A H 0.3827 0.5640 0.3480 0.049 Uiso 1 1 calc R . . H27B H 0.4395 0.5489 0.4475 0.049 Uiso 1 1 calc R . . H27C H 0.4500 0.4665 0.3422 0.049 Uiso 1 1 calc R . . C28 C 0.96092(19) 0.75883(18) 0.73267(15) 0.0229(4) Uani 1 1 d . . . H28 H 0.9359 0.8314 0.7530 0.027 Uiso 1 1 calc R . . C29 C 0.9423(3) 0.7058(2) 0.80508(18) 0.0387(5) Uani 1 1 d . . . H29A H 0.9654 0.6338 0.7864 0.058 Uiso 1 1 calc R . . H29B H 0.8517 0.6853 0.8006 0.058 Uiso 1 1 calc R . . H29C H 0.9977 0.7641 0.8748 0.058 Uiso 1 1 calc R . . C30 C 1.1030(2) 0.7979(2) 0.74195(18) 0.0388(5) Uani 1 1 d . . . H30A H 1.1307 0.7284 0.7236 0.058 Uiso 1 1 calc R . . H30B H 1.1560 0.8566 0.8121 0.058 Uiso 1 1 calc R . . H30C H 1.1133 0.8335 0.6961 0.058 Uiso 1 1 calc R . . C31 C 0.4951(2) 1.06321(19) 0.82392(16) 0.0277(4) Uani 1 1 d . . . H31A H 0.4338 1.0342 0.7554 0.041 Uiso 1 1 calc R . . H31B H 0.5612 1.1390 0.8428 0.041 Uiso 1 1 calc R . . H31C H 0.4490 1.0750 0.8723 0.041 Uiso 1 1 calc R . . C32 C 0.6843(2) 1.0040(2) 0.95878(16) 0.0310(5) Uani 1 1 d . . . H32A H 0.6355 1.0168 1.0052 0.046 Uiso 1 1 calc R . . H32B H 0.7532 1.0788 0.9795 0.046 Uiso 1 1 calc R . . H32C H 0.7222 0.9436 0.9610 0.046 Uiso 1 1 calc R . . C33 C 0.4478(2) 0.80473(19) 0.78345(17) 0.0285(4) Uani 1 1 d . . . H33A H 0.3941 0.7749 0.7123 0.043 Uiso 1 1 calc R . . H33B H 0.3935 0.8140 0.8258 0.043 Uiso 1 1 calc R . . H33C H 0.4897 0.7480 0.7896 0.043 Uiso 1 1 calc R . . C41 C 0.7076(2) 0.3824(2) 1.00214(18) 0.0466(9) Uani 0.69 1 d PGD A -1 C42 C 0.6494(2) 0.4466(2) 0.9623(2) 0.0421(10) Uani 0.69 1 d PGD A -1 H42 H 0.5793 0.4658 0.9799 0.051 Uiso 0.69 1 calc PR A -1 C43 C 0.6937(3) 0.4827(2) 0.8966(2) 0.0495(10) Uani 0.69 1 d PG A -1 H43 H 0.6539 0.5266 0.8693 0.059 Uiso 0.69 1 calc PR A -1 C44 C 0.7963(3) 0.4546(2) 0.87074(18) 0.0411(8) Uani 0.69 1 d PG A -1 H44 H 0.8266 0.4793 0.8258 0.049 Uiso 0.69 1 calc PR A -1 C45 C 0.8545(2) 0.3904(2) 0.9106(2) 0.0399(8) Uani 0.69 1 d PG A -1 H45 H 0.9246 0.3712 0.8930 0.048 Uiso 0.69 1 calc PR A -1 C46 C 0.8102(2) 0.3543(2) 0.9763(2) 0.0398(8) Uani 0.69 1 d PGD A -1 H46 H 0.8500 0.3104 1.0036 0.048 Uiso 0.69 1 calc PR A -1 C47 C 0.6655(6) 0.3447(5) 1.0756(4) 0.0571(12) Uiso 0.69 1 d PD A -1 H47A H 0.6572 0.4123 1.1285 0.086 Uiso 0.69 1 calc PR A -1 H47B H 0.7299 0.3177 1.1069 0.086 Uiso 0.69 1 calc PR A -1 H47C H 0.5820 0.2794 1.0394 0.086 Uiso 0.69 1 calc PR A -1 C51 C 0.7737(6) 0.4064(6) 0.9487(4) 0.0466(9) Uani 0.31 1 d PGD B -2 C52 C 0.6578(6) 0.4278(6) 0.9377(5) 0.0304(19) Uiso 0.31 1 d PGD B -2 H52 H 0.6293 0.4579 0.8915 0.036 Uiso 0.31 1 calc PR B -2 C53 C 0.5837(6) 0.4052(7) 0.9943(6) 0.087(4) Uiso 0.31 1 d PG B -2 H53 H 0.5045 0.4199 0.9868 0.104 Uiso 0.31 1 calc PR B -2 C54 C 0.6255(6) 0.3612(6) 1.0619(5) 0.0397(19) Uiso 0.31 1 d PG B -2 H54 H 0.5748 0.3458 1.1005 0.048 Uiso 0.31 1 calc PR B -2 C55 C 0.7414(7) 0.3398(7) 1.0729(5) 0.059(3) Uiso 0.31 1 d PG B -2 H55 H 0.7699 0.3097 1.1191 0.071 Uiso 0.31 1 calc PR B -2 C56 C 0.8155(6) 0.3624(7) 1.0163(5) 0.052(3) Uiso 0.31 1 d PGD B -2 H56 H 0.8947 0.3477 1.0238 0.062 Uiso 0.31 1 calc PR B -2 C57 C 0.8502(14) 0.4302(17) 0.8871(12) 0.084(5) Uiso 0.31 1 d PD B -2 H57A H 0.7927 0.4233 0.8245 0.127 Uiso 0.31 1 calc PR B -2 H57B H 0.8943 0.3723 0.8701 0.127 Uiso 0.31 1 calc PR B -2 H57C H 0.9144 0.5109 0.9260 0.127 Uiso 0.31 1 calc PR B -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.02223(8) 0.01438(7) 0.02433(8) 0.00906(5) 0.01579(5) 0.00518(5) Cl1 0.0211(2) 0.0265(2) 0.0202(2) 0.01023(18) 0.00911(16) 0.00513(17) Si1 0.0170(2) 0.0183(2) 0.0187(2) 0.00693(19) 0.01012(19) 0.00450(18) C1 0.0156(7) 0.0148(8) 0.0179(8) 0.0086(6) 0.0082(6) 0.0045(6) C2 0.0141(7) 0.0138(8) 0.0169(8) 0.0076(6) 0.0050(6) 0.0036(6) C3 0.0162(8) 0.0136(8) 0.0181(8) 0.0063(6) 0.0068(6) 0.0052(6) C4 0.0151(7) 0.0176(8) 0.0169(8) 0.0084(7) 0.0073(6) 0.0053(6) C5 0.0164(8) 0.0149(8) 0.0200(8) 0.0091(7) 0.0087(6) 0.0037(6) C6 0.0162(8) 0.0135(8) 0.0165(8) 0.0073(6) 0.0069(6) 0.0046(6) C7 0.0166(8) 0.0131(7) 0.0179(8) 0.0065(6) 0.0092(6) 0.0042(6) C8 0.0175(8) 0.0160(8) 0.0191(8) 0.0062(7) 0.0082(7) 0.0050(7) C9 0.0177(8) 0.0178(9) 0.0245(9) 0.0059(7) 0.0070(7) 0.0013(7) C10 0.0232(9) 0.0139(8) 0.0308(10) 0.0091(7) 0.0103(8) 0.0008(7) C11 0.0239(9) 0.0160(8) 0.0261(9) 0.0115(7) 0.0102(7) 0.0064(7) C12 0.0174(8) 0.0138(8) 0.0188(8) 0.0069(6) 0.0082(7) 0.0039(6) C13 0.0183(8) 0.0212(9) 0.0209(8) 0.0088(7) 0.0052(7) 0.0063(7) C14 0.0207(9) 0.0343(11) 0.0254(10) 0.0103(8) 0.0056(8) 0.0100(8) C15 0.0264(10) 0.0404(12) 0.0237(10) 0.0163(9) 0.0089(8) 0.0122(9) C16 0.0191(8) 0.0158(8) 0.0234(9) 0.0096(7) 0.0048(7) 0.0046(7) C17 0.0289(10) 0.0289(10) 0.0252(10) 0.0141(8) 0.0055(8) 0.0102(8) C18 0.0187(9) 0.0266(10) 0.0333(10) 0.0156(8) 0.0082(8) 0.0079(7) C19 0.0176(8) 0.0131(8) 0.0204(8) 0.0089(7) 0.0122(7) 0.0043(6) C20 0.0197(8) 0.0138(8) 0.0219(8) 0.0087(7) 0.0117(7) 0.0038(6) C21 0.0244(9) 0.0148(8) 0.0233(9) 0.0057(7) 0.0112(7) 0.0043(7) C22 0.0254(9) 0.0146(8) 0.0340(10) 0.0094(8) 0.0175(8) 0.0085(7) C23 0.0218(9) 0.0197(9) 0.0316(10) 0.0137(8) 0.0140(8) 0.0097(7) C24 0.0177(8) 0.0164(8) 0.0235(9) 0.0106(7) 0.0112(7) 0.0041(6) C25 0.0221(9) 0.0160(8) 0.0212(8) 0.0077(7) 0.0078(7) 0.0051(7) C26 0.0277(10) 0.0423(13) 0.0277(10) 0.0204(10) 0.0091(8) 0.0059(9) C27 0.0215(9) 0.0355(12) 0.0502(13) 0.0288(11) 0.0148(9) 0.0088(9) C28 0.0235(9) 0.0228(9) 0.0239(9) 0.0111(8) 0.0084(7) 0.0096(7) C29 0.0495(14) 0.0432(14) 0.0301(11) 0.0209(10) 0.0186(10) 0.0153(11) C30 0.0235(10) 0.0507(15) 0.0284(11) 0.0116(10) 0.0060(9) 0.0027(10) C31 0.0271(10) 0.0293(10) 0.0301(10) 0.0110(8) 0.0153(8) 0.0146(8) C32 0.0300(10) 0.0384(12) 0.0212(9) 0.0111(9) 0.0099(8) 0.0093(9) C33 0.0269(10) 0.0239(10) 0.0328(11) 0.0104(8) 0.0180(9) 0.0022(8) C41 0.056(2) 0.0254(15) 0.0314(16) -0.0011(13) 0.0139(15) -0.0079(14) C42 0.0329(19) 0.049(2) 0.0343(19) 0.0030(17) 0.0182(16) 0.0165(16) C43 0.046(2) 0.041(2) 0.040(2) 0.0082(17) -0.0021(17) 0.0125(17) C44 0.050(2) 0.0289(17) 0.0294(17) 0.0049(14) 0.0129(16) 0.0020(16) C45 0.0394(19) 0.0271(17) 0.051(2) 0.0117(16) 0.0209(17) 0.0123(14) C46 0.051(2) 0.0248(17) 0.043(2) 0.0136(16) 0.0168(17) 0.0145(15) C51 0.056(2) 0.0254(15) 0.0314(16) -0.0011(13) 0.0139(15) -0.0079(14) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C1 2.2463(17) . ? Sn1 Cl1 2.6157(5) . ? Sn1 Cl1 2.6376(5) 2_776 ? Cl1 Sn1 2.6377(5) 2_776 ? Si1 C31 1.864(2) . ? Si1 C33 1.865(2) . ? Si1 C32 1.869(2) . ? Si1 C4 1.8760(18) . ? C1 C6 1.413(2) . ? C1 C2 1.414(2) . ? C2 C3 1.398(2) . ? C2 C7 1.509(2) . ? C3 C4 1.400(2) . ? C3 H3 0.9500 . ? C4 C5 1.397(2) . ? C5 C6 1.394(2) . ? C5 H5 0.9500 . ? C6 C19 1.507(2) . ? C7 C12 1.410(2) . ? C7 C8 1.412(2) . ? C8 C9 1.397(3) . ? C8 C13 1.528(3) . ? C9 C10 1.384(3) . ? C9 H9 0.9500 . ? C10 C11 1.385(3) . ? C10 H10 0.9500 . ? C11 C12 1.400(2) . ? C11 H11 0.9500 . ? C12 C16 1.528(2) . ? C13 C14 1.532(3) . ? C13 C15 1.538(3) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C18 1.532(3) . ? C16 C17 1.533(3) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C20 1.409(3) . ? C19 C24 1.410(3) . ? C20 C21 1.399(2) . ? C20 C25 1.518(3) . ? C21 C22 1.388(3) . ? C21 H21 0.9500 . ? C22 C23 1.383(3) . ? C22 H22 0.9500 . ? C23 C24 1.395(3) . ? C23 H23 0.9500 . ? C24 C28 1.521(3) . ? C25 C27 1.528(3) . ? C25 C26 1.533(3) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.524(3) . ? C28 C30 1.531(3) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C41 C47 1.499(5) . ? C42 C43 1.3900 . ? C42 H42 0.9500 . ? C43 C44 1.3900 . ? C43 H43 0.9500 . ? C44 C45 1.3900 . ? C44 H44 0.9500 . ? C45 C46 1.3900 . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C51 C57 1.478(10) . ? C52 C53 1.3900 . ? C52 H52 0.9500 . ? C53 C54 1.3900 . ? C53 H53 0.9500 . ? C54 C55 1.3900 . ? C54 H54 0.9500 . ? C55 C56 1.3900 . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Sn1 Cl1 92.89(4) . . ? C1 Sn1 Cl1 100.55(5) . 2_776 ? Cl1 Sn1 Cl1 85.629(15) . 2_776 ? Sn1 Cl1 Sn1 94.372(15) . 2_776 ? C31 Si1 C33 109.82(10) . . ? C31 Si1 C32 109.35(10) . . ? C33 Si1 C32 109.78(11) . . ? C31 Si1 C4 110.51(9) . . ? C33 Si1 C4 108.98(9) . . ? C32 Si1 C4 108.38(9) . . ? C6 C1 C2 117.23(15) . . ? C6 C1 Sn1 108.17(12) . . ? C2 C1 Sn1 134.57(13) . . ? C3 C2 C1 119.50(15) . . ? C3 C2 C7 114.91(15) . . ? C1 C2 C7 125.56(15) . . ? C2 C3 C4 123.35(16) . . ? C2 C3 H3 118.3 . . ? C4 C3 H3 118.3 . . ? C5 C4 C3 116.73(16) . . ? C5 C4 Si1 122.84(13) . . ? C3 C4 Si1 120.32(13) . . ? C6 C5 C4 121.20(16) . . ? C6 C5 H5 119.4 . . ? C4 C5 H5 119.4 . . ? C5 C6 C1 121.91(16) . . ? C5 C6 C19 118.72(15) . . ? C1 C6 C19 119.20(15) . . ? C12 C7 C8 120.54(16) . . ? C12 C7 C2 119.22(15) . . ? C8 C7 C2 119.76(16) . . ? C9 C8 C7 118.59(17) . . ? C9 C8 C13 120.09(16) . . ? C7 C8 C13 121.20(16) . . ? C10 C9 C8 121.14(17) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C11 120.08(17) . . ? C9 C10 H10 120.0 . . ? C11 C10 H10 120.0 . . ? C10 C11 C12 120.89(18) . . ? C10 C11 H11 119.6 . . ? C12 C11 H11 119.6 . . ? C11 C12 C7 118.74(16) . . ? C11 C12 C16 119.43(16) . . ? C7 C12 C16 121.79(15) . . ? C8 C13 C14 113.93(16) . . ? C8 C13 C15 110.89(16) . . ? C14 C13 C15 108.31(16) . . ? C8 C13 H13 107.8 . . ? C14 C13 H13 107.8 . . ? C15 C13 H13 107.8 . . ? 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 . . ? C12 C16 C18 111.42(16) . . ? C12 C16 C17 113.20(16) . . ? C18 C16 C17 108.58(16) . . ? C12 C16 H16 107.8 . . ? C18 C16 H16 107.8 . . ? C17 C16 H16 107.8 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C20 C19 C24 120.56(16) . . ? C20 C19 C6 121.24(16) . . ? C24 C19 C6 118.18(16) . . ? C21 C20 C19 118.65(17) . . ? C21 C20 C25 119.20(17) . . ? C19 C20 C25 122.15(16) . . ? C22 C21 C20 120.91(18) . . ? C22 C21 H21 119.5 . . ? C20 C21 H21 119.5 . . ? C23 C22 C21 120.04(17) . . ? C23 C22 H22 120.0 . . ? C21 C22 H22 120.0 . . ? C22 C23 C24 121.05(18) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C23 C24 C19 118.79(17) . . ? C23 C24 C28 119.61(17) . . ? C19 C24 C28 121.60(16) . . ? C20 C25 C27 111.16(16) . . ? C20 C25 C26 111.63(16) . . ? C27 C25 C26 110.38(17) . . ? C20 C25 H25 107.8 . . ? C27 C25 H25 107.8 . . ? C26 C25 H25 107.8 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 C29 111.06(18) . . ? C24 C28 C30 111.68(17) . . ? C29 C28 C30 110.74(19) . . ? C24 C28 H28 107.7 . . ? C29 C28 H28 107.7 . . ? C30 C28 H28 107.7 . . ? 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 . . ? 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 . . ? C42 C41 C46 120.0 . . ? C42 C41 C47 121.8(3) . . ? C46 C41 C47 118.2(3) . . ? C41 C42 C43 120.0 . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C44 C43 C42 120.0 . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 120.0 . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C46 C45 C44 120.0 . . ? C46 C45 H45 120.0 . . ? C44 C45 H45 120.0 . . ? C45 C46 C41 120.0 . . ? C45 C46 H46 120.0 . . ? C41 C46 H46 120.0 . . ? C41 C47 H47A 109.5 . . ? C41 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C41 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C52 C51 C56 120.0 . . ? C52 C51 C57 118.9(7) . . ? C56 C51 C57 121.1(7) . . ? C53 C52 C51 120.0 . . ? C53 C52 H52 120.0 . . ? C51 C52 H52 120.0 . . ? C52 C53 C54 120.0 . . ? C52 C53 H53 120.0 . . ? C54 C53 H53 120.0 . . ? C55 C54 C53 120.0 . . ? C55 C54 H54 120.0 . . ? C53 C54 H54 120.0 . . ? C54 C55 C56 120.0 . . ? C54 C55 H55 120.0 . . ? C56 C55 H55 120.0 . . ? C55 C56 C51 120.0 . . ? C55 C56 H56 120.0 . . ? C51 C56 H56 120.0 . . ? C51 C57 H57A 109.5 . . ? C51 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C51 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.999 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.999 _refine_diff_density_max 1.436 _refine_diff_density_min -0.710 _refine_diff_density_rms 0.085 # Attachment '4-MeOArSnCl.cif.txt' data_jf1450ffmis _database_code_depnum_ccdc_archive 'CCDC 771277' #TrackingRef '4-MeOArSnCl.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C62 H78 Cl2 O2 Sn2, 2(C7 H8)' _chemical_formula_sum 'C76 H94 Cl2 O2 Sn2' _chemical_formula_weight 1347.79 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' O O 0.0106 0.0060 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 23.035(4) _cell_length_b 10.8053(17) _cell_length_c 27.610(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.801(2) _cell_angle_gamma 90.00 _cell_volume 6791.2(19) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 8564 _cell_measurement_theta_min 2.96 _cell_measurement_theta_max 27.45 _exptl_crystal_description Oval_Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.33 _exptl_crystal_size_mid 0.28 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.318 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2800 _exptl_absorpt_coefficient_mu 0.858 _exptl_absorpt_correction_type 'Empirical, (multi-scan)' _exptl_absorpt_correction_T_min 0.7648 _exptl_absorpt_correction_T_max 0.9040 _exptl_absorpt_process_details 'SADABS 2006/1 (Sheldrick, 2006)' _exptl_special_details ; A yellow oval plate with approximate orthogonal dimensions 0.33 x 0.28 x 0.12mm3 was placed and optically centered on the Bruker SMART APEX1 CCD system at -183\%C(90K). The initial unit cell was indexed using a least-squares analysis of a random set of reflections collected from three series of 0.3?wide -scans, 10 seconds per frame, and 30 frames per series that were well distributed in reciprocal space. Four -scan data frame series were collected [MoK ] with 0.3?wide scans, 25 seconds per frame and 606 frames were collected, at varying phi angles (phi=0? 90? 180? 270?, for each series. The crystal to detector distance was 5.196cm, thus providing a complete sphere of data with processing to 2Thetamax=55.17? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method '\w and \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 29098 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0664 _diffrn_reflns_limit_h_min -29 _diffrn_reflns_limit_h_max 29 _diffrn_reflns_limit_k_min -14 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 2.96 _diffrn_reflns_theta_max 27.50 _reflns_number_total 29134 _reflns_number_gt 24901 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (2.0-2) (Bruker, 2006)' _computing_cell_refinement 'SAINT (7.23A) (Bruker, 2005)' _computing_data_reduction 'SAINT (7.23A) (Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL97 _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. Structural determination and Refinement: All crystallographic calculations were performed on a Personal computer (PC) with a Pentium 3.20GHz processor and 1GB of extended memory. A total of 42654 reflections were processed with SAINT1 and corrected for Lorentz and polarization effects and absorption using Blessing's method as incorporated into the program SADABS2, 3 with 8168 unique. The initial unit cell determination did not reveal any signs that the crystal was twinned. Data collection was begun and the SHELXTL4 program package was now implemented to determine, based upon intensity statistics and systematic absences, the centric monoclinic space group C2/c (no. 15). The structure was determined by direct methods using the program XS5. Refinement of structure was performed with XL5 and subsequent difference-Fourier maps and refinement cycles in between revealed the location of all of the atoms comprising the structure. All of the non-hydrogen atoms were refined anisotropically. Hydrogen atoms were placed in calculated positions. The residuals remained quite large so data were thresholded from the various data collection runs for determining potential twin components using Cellnow6 while the current structure was tested with Rotax7 and Platon's TwinRotMat8. All three approaches generated nearly identical results with the twin matrix being a 180 degree rotation about the direct lattice direction 1 0 0 yielding the twin law [1 0 0 0 -1 0 -0.367 0 -1]. Data processing with SAINT1 for two components proved fruitless so Rotwin9 was implemented to generate the multi-component HKLF5 file, while the program Sysabsfilter10 was used to eliminate systematically absent reflections within the HKLF5 file. The final structure was refined to convergence with R(F)=6.46%, wR(F2)=14.63%, GOF=1.041 for all 29134 unmerged reflections [R(F)=5.34%, wR(F2)=14.07% for those 24901 data with Fo > 4sigma(Fo)]. A final difference-Fourier map was featureless indicating that the structure is therefore both correct and complete. Rotwin generated reflections for each component, including those overlapping so this may be the cause of the extra reflections. References: 1. Bruker (2004) SMART (Version 5.054) and SAINT (Version 7.23a). Bruker AXS Inc., Madison, Wisconsin, USA. 2. An Empirical Correction for Absorption Anisotropy, Blessing, R. H. (1995). Acta Cryst., A51, 33-38. 3. Sheldrick, G.M., SADABS (2006) Version 2006/1, 'Siemens Area Detector Absorption Correction' Universit\"at G ttingen: G ttingen, Germany. 4. Sheldrick, G.M., (2002). SHELXTL. Version 6.1. Bruker AXS Inc., Madison, Wisconsin, USA. 5. Sheldrick, G. M., (1997). SHELXS97 and SHELXL97. Universit\"at G ttingen: G ttingen, Germany. 6. Sheldrick, G.M., (private communication) CELLNOW, Twin matrix determination program, Universit\"at G ttingen: G ttingen, Germany, 2003. 7. Rotax, Simon Parson's & Bob Gould, University of Edinburgh (2003). 8. Platon Spek, A.L., (1990) Acta Cryst. A46, C34- A multipurpose crystallographic tool. Utrecht University, Utrecht, The Netherlands. 9. Rotwin, Victor Young and Maren Pink, University of Minnesota, private communication. 10. Sysabsfilter, Victor Young and William W. Brennessel, University of Minnesota, private communication. ; _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^)+(0.0685P)^2^+27.0904P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 29134 _refine_ls_number_parameters 403 _refine_ls_number_restraints 6 _refine_ls_R_factor_all 0.0646 _refine_ls_R_factor_gt 0.0534 _refine_ls_wR_factor_ref 0.1463 _refine_ls_wR_factor_gt 0.1407 _refine_ls_goodness_of_fit_ref 1.041 _refine_ls_restrained_S_all 1.041 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.073423(7) 0.911280(16) 0.026891(6) 0.01626(5) Uani 1 1 d . . . Cl1 Cl 0.03541(3) 1.13704(6) 0.01954(2) 0.02133(13) Uani 1 1 d . . . C1 C 0.06795(10) 0.8995(2) 0.10652(8) 0.0113(4) Uani 1 1 d . . . C2 C 0.12514(10) 0.8883(2) 0.13278(9) 0.0123(4) Uani 1 1 d . . . C3 C 0.13595(10) 0.8795(2) 0.18376(9) 0.0153(5) Uani 1 1 d . . . H3 H 0.1751 0.8748 0.2006 0.018 Uiso 1 1 calc R . . C4 C 0.08858(11) 0.8778(2) 0.20956(9) 0.0145(5) Uani 1 1 d . . . O1 O 0.09338(8) 0.86711(18) 0.25945(6) 0.0199(4) Uani 1 1 d . . . C5 C 0.03135(10) 0.8846(2) 0.18465(9) 0.0130(4) Uani 1 1 d . . . H5 H -0.0007 0.8800 0.2025 0.016 Uiso 1 1 calc R . . C6 C 0.02053(10) 0.8982(2) 0.13389(8) 0.0113(4) Uani 1 1 d . . . C7 C 0.17684(10) 0.8764(2) 0.10557(8) 0.0167(5) Uani 1 1 d . . . C8 C 0.20785(10) 0.9815(3) 0.09375(9) 0.0215(6) Uani 1 1 d . . . C9 C 0.25612(12) 0.9635(3) 0.06845(10) 0.0303(7) Uani 1 1 d . . . H9 H 0.2777 1.0333 0.0602 0.036 Uiso 1 1 calc R . . C10 C 0.27253(12) 0.8466(4) 0.05545(11) 0.0375(8) Uani 1 1 d . . . H10 H 0.3051 0.8362 0.0385 0.045 Uiso 1 1 calc R . . C11 C 0.24103(12) 0.7450(3) 0.06733(10) 0.0296(7) Uani 1 1 d . . . H11 H 0.2521 0.6648 0.0580 0.035 Uiso 1 1 calc R . . C12 C 0.19355(11) 0.7570(3) 0.09258(9) 0.0218(5) Uani 1 1 d . . . C13 C 0.19293(12) 1.1112(2) 0.10777(10) 0.0245(6) Uani 1 1 d . . . H13 H 0.1537 1.1083 0.1191 0.029 Uiso 1 1 calc R . . C14 C 0.18870(14) 1.2044(3) 0.06576(12) 0.0365(8) Uani 1 1 d . . . H14A H 0.2274 1.2146 0.0557 0.055 Uiso 1 1 calc R . . H14B H 0.1752 1.2842 0.0766 0.055 Uiso 1 1 calc R . . H14C H 0.1608 1.1741 0.0379 0.055 Uiso 1 1 calc R . . C15 C 0.23797(14) 1.1565(3) 0.15094(12) 0.0352(7) Uani 1 1 d . . . H15A H 0.2368 1.1026 0.1793 0.053 Uiso 1 1 calc R . . H15B H 0.2285 1.2415 0.1593 0.053 Uiso 1 1 calc R . . H15C H 0.2774 1.1543 0.1417 0.053 Uiso 1 1 calc R . . C16 C 0.16141(13) 0.6408(3) 0.10499(11) 0.0264(6) Uani 1 1 d . . . H16 H 0.1277 0.6671 0.1215 0.032 Uiso 1 1 calc R . . C17 C 0.13668(18) 0.5673(3) 0.05923(13) 0.0439(9) Uani 1 1 d . . . H17A H 0.1158 0.4943 0.0687 0.066 Uiso 1 1 calc R . . H17B H 0.1689 0.5410 0.0422 0.066 Uiso 1 1 calc R . . H17C H 0.1094 0.6195 0.0374 0.066 Uiso 1 1 calc R . . C18 C 0.20195(17) 0.5585(3) 0.14106(12) 0.0412(8) Uani 1 1 d . . . H18A H 0.2364 0.5346 0.1263 0.062 Uiso 1 1 calc R . . H18B H 0.1806 0.4841 0.1484 0.062 Uiso 1 1 calc R . . H18C H 0.2147 0.6045 0.1714 0.062 Uiso 1 1 calc R . . C19 C -0.04242(9) 0.9104(2) 0.11090(8) 0.0117(4) Uani 1 1 d . . . C20 C -0.07496(10) 0.8045(2) 0.09292(8) 0.0138(4) Uani 1 1 d . . . C21 C -0.13418(11) 0.8183(3) 0.07349(9) 0.0196(5) Uani 1 1 d . . . H21 H -0.1563 0.7476 0.0614 0.024 Uiso 1 1 calc R . . C22 C -0.16112(11) 0.9320(3) 0.07153(9) 0.0224(6) Uani 1 1 d . . . H22 H -0.2011 0.9399 0.0571 0.027 Uiso 1 1 calc R . . C23 C -0.12988(11) 1.0353(2) 0.09064(9) 0.0193(5) Uani 1 1 d . . . H23 H -0.1492 1.1130 0.0903 0.023 Uiso 1 1 calc R . . C24 C -0.07033(10) 1.0267(2) 0.11043(8) 0.0134(4) Uani 1 1 d . . . C25 C -0.04817(11) 0.6758(2) 0.09928(9) 0.0178(5) Uani 1 1 d . . . H25 H -0.0045 0.6846 0.1068 0.021 Uiso 1 1 calc R . . C26 C -0.06961(14) 0.6138(2) 0.14301(10) 0.0259(6) Uani 1 1 d . . . H26A H -0.0589 0.6651 0.1723 0.039 Uiso 1 1 calc R . . H26B H -0.0513 0.5322 0.1485 0.039 Uiso 1 1 calc R . . H26C H -0.1124 0.6044 0.1363 0.039 Uiso 1 1 calc R . . C27 C -0.06281(15) 0.5936(3) 0.05365(10) 0.0298(6) Uani 1 1 d . . . H27A H -0.1048 0.5737 0.0485 0.045 Uiso 1 1 calc R . . H27B H -0.0399 0.5169 0.0584 0.045 Uiso 1 1 calc R . . H27C H -0.0531 0.6377 0.0249 0.045 Uiso 1 1 calc R . . C28 C -0.03753(11) 1.1407(2) 0.13267(9) 0.0178(5) Uani 1 1 d . . . H28 H 0.0053 1.1278 0.1320 0.021 Uiso 1 1 calc R . . C29 C -0.04620(13) 1.1559(3) 0.18616(10) 0.0241(6) Uani 1 1 d . . . H29A H -0.0261 1.2312 0.1997 0.036 Uiso 1 1 calc R . . H29B H -0.0298 1.0840 0.2051 0.036 Uiso 1 1 calc R . . H29C H -0.0883 1.1624 0.1880 0.036 Uiso 1 1 calc R . . C30 C -0.05629(15) 1.2605(3) 0.10446(10) 0.0295(6) Uani 1 1 d . . . H30A H -0.0539 1.2487 0.0696 0.044 Uiso 1 1 calc R . . H30B H -0.0302 1.3282 0.1175 0.044 Uiso 1 1 calc R . . H30C H -0.0968 1.2809 0.1083 0.044 Uiso 1 1 calc R . . C31 C 0.15113(12) 0.8654(3) 0.28735(10) 0.0306(7) Uani 1 1 d . . . H31A H 0.1482 0.8632 0.3224 0.046 Uiso 1 1 calc R . . H31B H 0.1724 0.9400 0.2801 0.046 Uiso 1 1 calc R . . H31C H 0.1722 0.7919 0.2786 0.046 Uiso 1 1 calc R . . C41 C 0.10839(16) 0.4211(3) 0.23463(14) 0.0270(11) Uani 0.50 1 d PGD A -1 C42 C 0.15111(19) 0.4301(3) 0.27588(15) 0.0271(12) Uani 0.50 1 d PGD A -1 H42 H 0.1550 0.5042 0.2946 0.032 Uiso 0.50 1 calc PR A -1 C43 C 0.1882(2) 0.3306(4) 0.28975(15) 0.0548(13) Uani 0.50 1 d PG A -1 H43 H 0.2174 0.3367 0.3179 0.066 Uiso 0.50 1 calc PR A -1 C44 C 0.18257(19) 0.2221(4) 0.26236(16) 0.0332(13) Uani 0.50 1 d PG A -1 H44 H 0.2079 0.1541 0.2718 0.040 Uiso 0.50 1 calc PR A -1 C45 C 0.13984(18) 0.2132(3) 0.22111(15) 0.0307(9) Uani 0.50 1 d PG A -1 H45 H 0.1360 0.1390 0.2024 0.037 Uiso 0.50 1 calc PR A -1 C46 C 0.10276(17) 0.3127(4) 0.20724(13) 0.0248(11) Uani 0.50 1 d PGD A -1 H46 H 0.0736 0.3065 0.1791 0.030 Uiso 0.50 1 calc PR A -1 C47 C 0.0673(4) 0.5267(8) 0.2190(4) 0.055(2) Uani 0.50 1 d PD A -1 H47A H 0.0301 0.5134 0.2314 0.083 Uiso 0.50 1 calc PR A -1 H47B H 0.0598 0.5312 0.1831 0.083 Uiso 0.50 1 calc PR A -1 H47C H 0.0851 0.6044 0.2322 0.083 Uiso 0.50 1 calc PR A -1 C51 C 0.14321(18) 0.3767(4) 0.25277(13) 0.0408(17) Uani 0.50 1 d PGD B -2 C52 C 0.1243(2) 0.4989(4) 0.24777(15) 0.049(2) Uani 0.50 1 d PGD B -2 H52 H 0.1361 0.5566 0.2733 0.059 Uiso 0.50 1 calc PR B -2 C53 C 0.0881(2) 0.5365(3) 0.20538(19) 0.043(2) Uani 0.50 1 d PG B -2 H53 H 0.0752 0.6200 0.2020 0.052 Uiso 0.50 1 calc PR B -2 C54 C 0.07079(18) 0.4520(4) 0.16800(15) 0.0384(15) Uani 0.50 1 d PG B -2 H54 H 0.0460 0.4778 0.1390 0.046 Uiso 0.50 1 calc PR B -2 C55 C 0.08969(18) 0.3299(3) 0.17300(14) 0.0307(9) Uani 0.50 1 d PG B -2 H55 H 0.0779 0.2721 0.1474 0.037 Uiso 0.50 1 calc PR B -2 C56 C 0.12590(17) 0.2922(3) 0.21538(17) 0.0248(11) Uani 0.50 1 d PGD B -2 H56 H 0.1388 0.2087 0.2188 0.030 Uiso 0.50 1 calc PR B -2 C57 C 0.1848(4) 0.3348(10) 0.2974(3) 0.0548(13) Uani 0.50 1 d PD B -2 H57A H 0.2191 0.3898 0.3026 0.082 Uiso 0.50 1 calc PR B -2 H57B H 0.1977 0.2500 0.2924 0.082 Uiso 0.50 1 calc PR B -2 H57C H 0.1647 0.3375 0.3262 0.082 Uiso 0.50 1 calc PR B -2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.01233(8) 0.02697(9) 0.00915(8) 0.00067(7) 0.00064(6) 0.00415(7) Cl1 0.0215(3) 0.0224(3) 0.0185(3) 0.0054(2) -0.0023(2) -0.0064(2) C1 0.0111(10) 0.0104(10) 0.0124(10) -0.0010(8) 0.0013(8) 0.0007(8) C2 0.0095(10) 0.0133(11) 0.0142(11) 0.0009(8) 0.0020(8) 0.0014(8) C3 0.0080(10) 0.0221(12) 0.0150(11) -0.0001(9) -0.0008(8) 0.0004(9) C4 0.0159(11) 0.0146(11) 0.0129(11) 0.0002(8) 0.0024(9) 0.0026(8) O1 0.0147(8) 0.0364(10) 0.0087(8) 0.0021(7) 0.0022(7) 0.0021(7) C5 0.0122(10) 0.0126(11) 0.0148(11) -0.0007(8) 0.0045(9) 0.0015(8) C6 0.0104(10) 0.0084(10) 0.0148(11) -0.0001(8) 0.0009(8) 0.0001(8) C7 0.0081(10) 0.0308(13) 0.0107(11) -0.0001(9) -0.0004(8) 0.0028(9) C8 0.0079(11) 0.0436(16) 0.0130(12) 0.0074(11) 0.0011(9) 0.0041(10) C9 0.0115(12) 0.0584(19) 0.0224(14) 0.0101(13) 0.0073(10) 0.0011(12) C10 0.0120(13) 0.085(3) 0.0178(14) 0.0064(15) 0.0099(10) 0.0123(14) C11 0.0170(13) 0.0569(19) 0.0141(12) -0.0011(12) -0.0002(10) 0.0185(13) C12 0.0151(12) 0.0368(15) 0.0129(11) 0.0019(10) 0.0005(9) 0.0110(11) C13 0.0156(12) 0.0279(15) 0.0283(14) 0.0082(11) -0.0026(10) -0.0073(10) C14 0.0253(15) 0.0460(19) 0.0352(17) 0.0225(14) -0.0053(12) -0.0111(13) C15 0.0229(15) 0.0398(18) 0.0396(18) 0.0038(14) -0.0059(13) -0.0048(13) C16 0.0285(15) 0.0236(13) 0.0278(15) -0.0002(11) 0.0070(12) 0.0140(11) C17 0.056(2) 0.0340(18) 0.0385(19) -0.0054(14) -0.0018(16) 0.0073(15) C18 0.055(2) 0.0386(18) 0.0292(16) 0.0083(13) 0.0050(15) 0.0245(16) C19 0.0091(10) 0.0149(10) 0.0111(10) -0.0002(9) 0.0022(8) 0.0011(9) C20 0.0134(11) 0.0184(12) 0.0104(10) 0.0007(9) 0.0042(8) -0.0007(9) C21 0.0167(12) 0.0298(13) 0.0122(11) -0.0023(10) 0.0015(9) -0.0078(10) C22 0.0115(11) 0.0394(16) 0.0156(12) 0.0027(11) -0.0004(9) 0.0050(10) C23 0.0139(12) 0.0256(13) 0.0187(12) -0.0008(10) 0.0029(9) 0.0102(10) C24 0.0138(11) 0.0175(12) 0.0098(10) 0.0014(9) 0.0046(8) 0.0039(9) C25 0.0160(11) 0.0168(11) 0.0204(12) -0.0038(9) 0.0027(10) -0.0027(9) C26 0.0347(16) 0.0205(14) 0.0229(14) 0.0045(10) 0.0055(12) 0.0010(11) C27 0.0499(18) 0.0198(13) 0.0203(13) -0.0050(11) 0.0069(13) -0.0050(13) C28 0.0195(12) 0.0143(11) 0.0196(12) 0.0004(9) 0.0029(10) 0.0031(9) C29 0.0315(15) 0.0238(14) 0.0169(13) -0.0030(10) 0.0033(11) 0.0036(11) C30 0.0469(18) 0.0191(13) 0.0215(14) 0.0007(10) 0.0024(12) 0.0111(12) C31 0.0208(14) 0.059(2) 0.0100(12) 0.0018(12) -0.0032(10) -0.0027(13) C41 0.021(3) 0.040(3) 0.019(3) 0.000(2) 0.000(2) -0.001(3) C42 0.015(3) 0.036(3) 0.028(3) -0.012(3) -0.003(2) -0.002(2) C43 0.029(2) 0.090(3) 0.043(3) 0.014(2) -0.0035(19) -0.024(2) C44 0.035(3) 0.029(3) 0.039(3) 0.001(3) 0.014(3) 0.011(3) C45 0.031(2) 0.029(2) 0.033(2) -0.0057(18) 0.0082(18) -0.0075(18) C46 0.013(3) 0.035(2) 0.026(2) 0.0026(18) 0.001(2) -0.009(2) C47 0.047(5) 0.052(5) 0.065(6) 0.023(4) 0.003(5) 0.011(4) C51 0.023(3) 0.070(5) 0.029(4) 0.004(3) 0.002(3) -0.024(3) C52 0.048(4) 0.058(5) 0.049(5) -0.023(4) 0.030(4) -0.023(4) C53 0.036(4) 0.029(4) 0.070(6) 0.004(4) 0.030(4) -0.001(3) C54 0.018(3) 0.036(3) 0.061(5) 0.004(3) 0.006(3) 0.000(2) C55 0.031(2) 0.029(2) 0.033(2) -0.0057(18) 0.0082(18) -0.0075(18) C56 0.013(3) 0.035(2) 0.026(2) 0.0026(18) 0.001(2) -0.009(2) C57 0.029(2) 0.090(3) 0.043(3) 0.014(2) -0.0035(19) -0.024(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C1 2.225(2) . ? Sn1 Cl1 2.5892(8) . ? Sn1 Cl1 2.6867(7) 5_575 ? Cl1 Sn1 2.6867(7) 5_575 ? C1 C2 1.408(3) . ? C1 C6 1.420(3) . ? C2 C3 1.395(3) . ? C2 C7 1.508(3) . ? C3 C4 1.392(3) . ? C3 H3 0.9500 . ? C4 O1 1.370(3) . ? C4 C5 1.392(3) . ? O1 C31 1.432(3) . ? C5 C6 1.393(3) . ? C5 H5 0.9500 . ? C6 C19 1.497(3) . ? C7 C8 1.407(4) . ? C7 C12 1.408(4) . ? C8 C9 1.414(4) . ? C8 C13 1.507(4) . ? C9 C10 1.382(5) . ? C9 H9 0.9500 . ? C10 C11 1.383(5) . ? C10 H10 0.9500 . ? C11 C12 1.390(4) . ? C11 H11 0.9500 . ? C12 C16 1.524(4) . ? C13 C14 1.528(4) . ? C13 C15 1.536(4) . ? C13 H13 1.0000 . ? C14 H14A 0.9800 . ? C14 H14B 0.9800 . ? C14 H14C 0.9800 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 C17 1.526(4) . ? C16 C18 1.539(4) . ? C16 H16 1.0000 . ? C17 H17A 0.9800 . ? C17 H17B 0.9800 . ? C17 H17C 0.9800 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 C24 1.410(3) . ? C19 C20 1.416(3) . ? C20 C21 1.395(3) . ? C20 C25 1.521(3) . ? C21 C22 1.374(4) . ? C21 H21 0.9500 . ? C22 C23 1.388(4) . ? C22 H22 0.9500 . ? C23 C24 1.400(3) . ? C23 H23 0.9500 . ? C24 C28 1.524(3) . ? C25 C26 1.527(4) . ? C25 C27 1.536(3) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.529(4) . ? C28 C30 1.538(4) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C41 C47 1.504(8) . ? C42 C43 1.3900 . ? C42 H42 0.9500 . ? C43 C44 1.3900 . ? C43 H43 0.9500 . ? C44 C45 1.3900 . ? C44 H44 0.9500 . ? C45 C46 1.3900 . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C51 C57 1.510(8) . ? C52 C53 1.3900 . ? C52 H52 0.9500 . ? C53 C54 1.3900 . ? C53 H53 0.9500 . ? C54 C55 1.3900 . ? C54 H54 0.9500 . ? C55 C56 1.3900 . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Sn1 Cl1 93.54(6) . . ? C1 Sn1 Cl1 105.70(6) . 5_575 ? Cl1 Sn1 Cl1 82.30(2) . 5_575 ? Sn1 Cl1 Sn1 97.70(2) . 5_575 ? C2 C1 C6 117.4(2) . . ? C2 C1 Sn1 108.88(15) . . ? C6 C1 Sn1 133.70(16) . . ? C3 C2 C1 122.3(2) . . ? C3 C2 C7 117.7(2) . . ? C1 C2 C7 119.9(2) . . ? C4 C3 C2 119.0(2) . . ? C4 C3 H3 120.5 . . ? C2 C3 H3 120.5 . . ? O1 C4 C3 124.5(2) . . ? O1 C4 C5 115.2(2) . . ? C3 C4 C5 120.2(2) . . ? C4 O1 C31 117.88(19) . . ? C4 C5 C6 120.8(2) . . ? C4 C5 H5 119.6 . . ? C6 C5 H5 119.6 . . ? C5 C6 C1 120.2(2) . . ? C5 C6 C19 116.6(2) . . ? C1 C6 C19 123.2(2) . . ? C8 C7 C12 120.8(2) . . ? C8 C7 C2 121.0(2) . . ? C12 C7 C2 118.2(2) . . ? C7 C8 C9 118.0(3) . . ? C7 C8 C13 123.2(2) . . ? C9 C8 C13 118.8(3) . . ? C10 C9 C8 121.4(3) . . ? C10 C9 H9 119.3 . . ? C8 C9 H9 119.3 . . ? C9 C10 C11 119.4(2) . . ? C9 C10 H10 120.3 . . ? C11 C10 H10 120.3 . . ? C10 C11 C12 121.7(3) . . ? C10 C11 H11 119.1 . . ? C12 C11 H11 119.1 . . ? C11 C12 C7 118.7(3) . . ? C11 C12 C16 118.8(3) . . ? C7 C12 C16 122.5(2) . . ? C8 C13 C14 114.1(3) . . ? C8 C13 C15 110.0(2) . . ? C14 C13 C15 109.7(2) . . ? C8 C13 H13 107.6 . . ? C14 C13 H13 107.6 . . ? C15 C13 H13 107.6 . . ? 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 . . ? C12 C16 C17 112.0(3) . . ? C12 C16 C18 110.7(3) . . ? C17 C16 C18 110.4(3) . . ? C12 C16 H16 107.8 . . ? C17 C16 H16 107.8 . . ? C18 C16 H16 107.8 . . ? C16 C17 H17A 109.5 . . ? C16 C17 H17B 109.5 . . ? H17A C17 H17B 109.5 . . ? C16 C17 H17C 109.5 . . ? H17A C17 H17C 109.5 . . ? H17B C17 H17C 109.5 . . ? C16 C18 H18A 109.5 . . ? C16 C18 H18B 109.5 . . ? H18A C18 H18B 109.5 . . ? C16 C18 H18C 109.5 . . ? H18A C18 H18C 109.5 . . ? H18B C18 H18C 109.5 . . ? C24 C19 C20 120.0(2) . . ? C24 C19 C6 119.6(2) . . ? C20 C19 C6 120.2(2) . . ? C21 C20 C19 118.9(2) . . ? C21 C20 C25 119.8(2) . . ? C19 C20 C25 121.0(2) . . ? C22 C21 C20 121.3(2) . . ? C22 C21 H21 119.4 . . ? C20 C21 H21 119.4 . . ? C21 C22 C23 120.0(2) . . ? C21 C22 H22 120.0 . . ? C23 C22 H22 120.0 . . ? C22 C23 C24 121.0(2) . . ? C22 C23 H23 119.5 . . ? C24 C23 H23 119.5 . . ? C23 C24 C19 118.7(2) . . ? C23 C24 C28 119.9(2) . . ? C19 C24 C28 121.3(2) . . ? C20 C25 C26 108.5(2) . . ? C20 C25 C27 113.6(2) . . ? C26 C25 C27 109.8(2) . . ? C20 C25 H25 108.3 . . ? C26 C25 H25 108.3 . . ? C27 C25 H25 108.3 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C24 C28 C29 110.2(2) . . ? C24 C28 C30 113.1(2) . . ? C29 C28 C30 109.3(2) . . ? C24 C28 H28 108.0 . . ? C29 C28 H28 108.0 . . ? C30 C28 H28 108.0 . . ? 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 . . ? O1 C31 H31A 109.5 . . ? O1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? O1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? C42 C41 C46 120.0 . . ? C42 C41 C47 121.2(5) . . ? C46 C41 C47 118.7(5) . . ? C43 C42 C41 120.0 . . ? C43 C42 H42 120.0 . . ? C41 C42 H42 120.0 . . ? C42 C43 C44 120.0 . . ? C42 C43 H43 120.0 . . ? C44 C43 H43 120.0 . . ? C45 C44 C43 120.0 . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C44 C45 C46 120.0 . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C45 C46 C41 120.0 . . ? C45 C46 H46 120.0 . . ? C41 C46 H46 120.0 . . ? C41 C47 H47A 109.5 . . ? C41 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C41 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C52 C51 C56 120.0 . . ? C52 C51 C57 121.0(5) . . ? C56 C51 C57 118.9(5) . . ? C51 C52 C53 120.0 . . ? C51 C52 H52 120.0 . . ? C53 C52 H52 120.0 . . ? C54 C53 C52 120.0 . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C55 C54 C53 120.0 . . ? C55 C54 H54 120.0 . . ? C53 C54 H54 120.0 . . ? C56 C55 C54 120.0 . . ? C56 C55 H55 120.0 . . ? C54 C55 H55 120.0 . . ? C55 C56 C51 120.0 . . ? C55 C56 H56 120.0 . . ? C51 C56 H56 120.0 . . ? C51 C57 H57A 109.5 . . ? C51 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C51 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 0.943 _refine_diff_density_min -1.787 _refine_diff_density_rms 0.119 # Attachment 'CGeI.cif.txt' data_jf1518ffmi _database_code_depnum_ccdc_archive 'CCDC 771278' #TrackingRef 'CGeI.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H61 Cl0.13 Ge I0.87, C42 H61 Ge I' _chemical_formula_sum 'C84 H122 Cl0.13 Ge2 I1.87' _chemical_formula_weight 1518.91 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 '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' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.9294(5) _cell_length_b 18.4084(8) _cell_length_c 20.7414(9) _cell_angle_alpha 114.657(2) _cell_angle_beta 105.431(2) _cell_angle_gamma 90.806(2) _cell_volume 3949.4(3) _cell_formula_units_Z 2 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 5018 _cell_measurement_theta_min 2.83 _cell_measurement_theta_max 25.74 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.24 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.277 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1583 _exptl_absorpt_coefficient_mu 1.537 _exptl_absorpt_correction_type Analytical _exptl_absorpt_correction_T_min 0.7093 _exptl_absorpt_correction_T_max 0.9134 _exptl_absorpt_process_details 'SADABS 2006/1 (Sheldrick, 2006)' _exptl_special_details ; An orange block with approximate orthogonal dimensions 0.06 x 0.11 0.24mm3 was placed and optically centered on the Bruker SMART APEX(1) CCD system at -183C(90K). The initial unit cell was indexed using a least-squares analysis of a random set of reflections collected from three series of 0.3deg wide omega-scans, 10 seconds per frame, and 30 frames per series that were well distributed in reciprocal space. Four omega-scan data frame series were collected [MoKa] with 0.3degwide scans, 70 seconds per frame and 606 frames were collected, at varying phi angles (phi=0deg, 90deg, 180deg, 270deg, for each series. The crystal to detector distance was 5.23cm, thus providing a complete sphere of data with processing to 2thetamax=55.09deg ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII' _diffrn_measurement_method '\w and \f' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 35270 _diffrn_reflns_av_R_equivalents 0.0500 _diffrn_reflns_av_sigmaI/netI 0.0766 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 15 _diffrn_reflns_limit_k_min -23 _diffrn_reflns_limit_k_max 23 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 26 _diffrn_reflns_theta_min 2.83 _diffrn_reflns_theta_max 27.48 _reflns_number_total 18059 _reflns_number_gt 11464 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (2.0-2) (Bruker, 2006)' _computing_cell_refinement 'SAINT (7.23A) (Bruker, 2005)' _computing_data_reduction 'SAINT (7.23A) (Bruker, 2005)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL97 _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. 220_ALERT_2_A Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.55 Ratio Due to Librational effects in outer periphery of molecules 910_ALERT_3_B # Missing FCF Reflections Below Th(Min) ........ 19 Reflections are most probably behind backstop at very low theta values #============================================================================= Missing Reflections (Asymmetric Reflection Unit) below sin(th)/lambda = 0.5 #============================================================================= Nr H K L sin(th)/lambda Theta I(calc) I(calc)/I(max) #----------------------------------------------------------------------------- 1 1 0 0 0.044 1.79* 567.33 0.00592 2 -1 1 0 0.050 2.02* 1468.04 0.01532 3 0 1 0 0.030 1.23* 10274.99 0.10722 4 1 1 0 0.057 2.31* 3192.90 0.03332 5 0 2 0 0.060 2.46* 5450.48 0.05688 6 0 -2 1 0.054 2.21* 47198.37 0.49251 7 -1 -1 1 0.050 2.05* 41275.18 0.43070 8 0 -1 1 0.031 1.26* 3165.99 0.03304 9 1 -1 1 0.057 2.32* 64841.16 0.67661 10 -1 0 1 0.044 1.81* 44.79 0.00047 11 0 0 1 0.028 1.13* 97.71 0.00102 12 1 0 1 0.059 2.39* 5884.50 0.06140 13 -1 1 1 0.057 2.32* 6646.47 0.06936 14 0 1 1 0.049 2.00* 37082.61 0.38695 15 0 -2 2 0.062 2.51* 30996.75 0.32345 16 -1 -1 2 0.058 2.37* 3691.41 0.03852 17 0 -1 2 0.050 2.05* 39233.29 0.40940 18 -1 0 2 0.060 2.43* 85456.10 0.89173 19 0 0 2 0.056 2.26* 394.38 0.00412 ** Note: I(max) is the maximum I(obs) encountered in the fcf-file ** Starred Reflections have a Theta below Theta(Min) = 2.83 From CIF: Theta(Min) = 2.83 Structural determination and Refinement: All crystallographic calculations were performed on a Personal computer (PC) with a Pentium 3.20GHz processor and 1GB of extended memory. A total of 50685 reflections were collected and corrected for Lorentz and polarization effects and analytical, face based, absorption using Blessing's method as incorporated into the program SADABS2, 3 with 18059 unique. The SHELXTL4 program package was implemented to determine the probable space group and set up the initial files. System symmetry, lack of systematic absences and intensity statistics indicated the centrosymmetric triclinic space group P-1 (no. 2). The structure was determined by direct methods with the successful location of a majority of the molecules using the program XS5. The structure was refined with XL5. The data collected were merged based upon identical indices yielding 35270 data [R(int)=0.0379] that were truncated to 2 max=55.00?resulting in 35270 data that were further merged in least-squares refinement to 11464 unique data [R(int)=0.0500]. All non-hydrogen atoms were refined anisotropically. Hydrogen atoms were placed in calculated idealized positions throughout the final convergence process. SADI, ISOR, EADP instructions were used to refine a highly librational and disordered terminal isopropyl group while this libration was noticeable throughout the two molecules. The main difference between the two molecules is that one is 100% Iodine bound to Germanium, while the second is partially mixed with 13% Chlorine. The final structure was refined to convergence with R(F)=9.48%, wR(F2)=14.23%, GOF=1.062 for all 18059 unique reflections [R(F)=5.42%, wR(F2)=13.01% for those 11464 data with Fo > 4sig(Fo)]. The final difference-Fourier map was featureless indicating that the structure is both correct and complete. An empirical correction for extinction was also attempted but found to be negative and therefore not applied. References: 1. Bruker (2004) SMART (Version 5.054) and SAINT (Version 7.23a). Bruker AXS Inc., Madison, Wisconsin, USA. 2. An Empirical Correction for Absorption Anisotropy, Blessing, R. H. (1995). Acta Cryst., A51, 33-38. 3. Sheldrick, G.M., SADABS (2006) Version 2006/1, 'Siemens Area Detector Absorption Correction' Universit\"at G ttingen: G ttingen, Germany. 4. Sheldrick, G.M., (2002). SHELXTL. Version 6.1. Bruker AXS Inc., Madison, Wisconsin, USA. 5. Sheldrick, G. M., (1997). SHELXS97 and SHELXL97. Universit\"at G ttingen: G ttingen, Germany. ; _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^)+(0.0683P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 18059 _refine_ls_number_parameters 883 _refine_ls_number_restraints 68 _refine_ls_R_factor_all 0.0948 _refine_ls_R_factor_gt 0.0542 _refine_ls_wR_factor_ref 0.1423 _refine_ls_wR_factor_gt 0.1301 _refine_ls_goodness_of_fit_ref 1.062 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group I1 I 0.24949(3) 0.369236(18) 0.008139(16) 0.03993(10) Uani 1 1 d . . . Ge1 Ge 0.22602(4) 0.51865(3) 0.08886(2) 0.02892(12) Uani 1 1 d . . . C1 C 0.2959(3) 0.5452(2) 0.19724(19) 0.0190(8) Uani 1 1 d . . . C2 C 0.2714(3) 0.5036(2) 0.2364(2) 0.0186(8) Uani 1 1 d . . . C3 C 0.3107(3) 0.5423(2) 0.3150(2) 0.0210(8) Uani 1 1 d . . . C4 C 0.3764(3) 0.6190(2) 0.3503(2) 0.0231(8) Uani 1 1 d . . . H4 H 0.4035 0.6444 0.4031 0.028 Uiso 1 1 calc R . . C5 C 0.4044(3) 0.6600(2) 0.3128(2) 0.0187(8) Uani 1 1 d . . . C6 C 0.3613(3) 0.6229(2) 0.2353(2) 0.0201(8) Uani 1 1 d . . . C7 C 0.2809(4) 0.5028(2) 0.3613(2) 0.0287(10) Uani 1 1 d . . . H7 H 0.2452 0.4455 0.3268 0.034 Uiso 1 1 calc R . . C8 C 0.1903(4) 0.5448(3) 0.3977(3) 0.0410(11) Uani 1 1 d . . . H8A H 0.2255 0.5997 0.4351 0.061 Uiso 1 1 calc R . . H8B H 0.1641 0.5146 0.4216 0.061 Uiso 1 1 calc R . . H8C H 0.1229 0.5473 0.3598 0.061 Uiso 1 1 calc R . . C9 C 0.3901(4) 0.5016(3) 0.4198(2) 0.0373(11) Uani 1 1 d . . . H9A H 0.4490 0.4766 0.3956 0.056 Uiso 1 1 calc R . . H9B H 0.3683 0.4705 0.4442 0.056 Uiso 1 1 calc R . . H9C H 0.4229 0.5571 0.4569 0.056 Uiso 1 1 calc R . . C10 C 0.4823(3) 0.7419(2) 0.3551(2) 0.0253(9) Uani 1 1 d . . . H10 H 0.4915 0.7609 0.3178 0.030 Uiso 1 1 calc R . . C11 C 0.4300(4) 0.8057(2) 0.4089(3) 0.0399(12) Uani 1 1 d . . . H11A H 0.3523 0.8114 0.3818 0.060 Uiso 1 1 calc R . . H11B H 0.4816 0.8575 0.4327 0.060 Uiso 1 1 calc R . . H11C H 0.4224 0.7893 0.4471 0.060 Uiso 1 1 calc R . . C12 C 0.6049(4) 0.7338(3) 0.3970(3) 0.0454(13) Uani 1 1 d . . . H12A H 0.5985 0.7157 0.4343 0.068 Uiso 1 1 calc R . . H12B H 0.6551 0.7863 0.4217 0.068 Uiso 1 1 calc R . . H12C H 0.6396 0.6943 0.3617 0.068 Uiso 1 1 calc R . . C13 C 0.2070(3) 0.4197(2) 0.1944(2) 0.0226(8) Uani 1 1 d . A . C14 C 0.0841(4) 0.4054(2) 0.1590(2) 0.0280(9) Uani 1 1 d . . . C15 C 0.0292(4) 0.3262(3) 0.1160(2) 0.0423(12) Uani 1 1 d . A . H15 H -0.0533 0.3164 0.0929 0.051 Uiso 1 1 calc R . . C16 C 0.0911(5) 0.2612(3) 0.1057(3) 0.0513(15) Uani 1 1 d . . . C17 C 0.2100(5) 0.2763(3) 0.1422(2) 0.0435(12) Uani 1 1 d . A . H17 H 0.2530 0.2322 0.1366 0.052 Uiso 1 1 calc R . . C18 C 0.2683(4) 0.3541(2) 0.1868(2) 0.0316(10) Uani 1 1 d . . . C19 C 0.0097(4) 0.4730(3) 0.1693(2) 0.0342(10) Uani 1 1 d . . . H19 H 0.0633 0.5255 0.1999 0.041 Uiso 1 1 calc R . . C20 C -0.0599(4) 0.4730(3) 0.0954(3) 0.0414(11) Uani 1 1 d . . . H20A H -0.0057 0.4749 0.0678 0.062 Uiso 1 1 calc R . . H20B H -0.1011 0.5203 0.1054 0.062 Uiso 1 1 calc R . . H20C H -0.1171 0.4237 0.0659 0.062 Uiso 1 1 calc R . . C21 C -0.0764(4) 0.4686(4) 0.2112(3) 0.0543(15) Uani 1 1 d . . . H21A H -0.1386 0.4227 0.1786 0.081 Uiso 1 1 calc R . . H21B H -0.1112 0.5186 0.2266 0.081 Uiso 1 1 calc R . . H21C H -0.0343 0.4615 0.2553 0.081 Uiso 1 1 calc R . . C22 C -0.0027(12) 0.1818(7) 0.0667(6) 0.0308(16) Uani 0.38 1 d PD A 1 H22 H -0.0849 0.1935 0.0521 0.037 Uiso 0.38 1 calc PR A 1 C23 C 0.0407(12) 0.1385(8) 0.0001(7) 0.052(3) Uani 0.38 1 d PDU A 1 H23A H 0.1168 0.1219 0.0160 0.078 Uiso 0.38 1 calc PR A 1 H23B H 0.0494 0.1748 -0.0224 0.078 Uiso 0.38 1 calc PR A 1 H23C H -0.0161 0.0907 -0.0365 0.078 Uiso 0.38 1 calc PR A 1 C24 C 0.012(3) 0.1389(16) 0.1157(10) 0.041(3) Uani 0.38 1 d PDU A 1 H24A H -0.0246 0.1661 0.1552 0.061 Uiso 0.38 1 calc PR A 1 H24B H 0.0955 0.1398 0.1380 0.061 Uiso 0.38 1 calc PR A 1 H24C H -0.0265 0.0828 0.0859 0.061 Uiso 0.38 1 calc PR A 1 C22B C 0.0463(6) 0.1702(4) 0.0514(4) 0.0308(16) Uani 0.62 1 d PD A 2 H22B H 0.1146 0.1441 0.0374 0.037 Uiso 0.62 1 calc PR A 2 C23B C -0.0441(7) 0.1618(5) -0.0183(4) 0.050(2) Uani 0.62 1 d PDU A 2 H23D H -0.1124 0.1864 -0.0059 0.076 Uiso 0.62 1 calc PR A 2 H23E H -0.0686 0.1045 -0.0526 0.076 Uiso 0.62 1 calc PR A 2 H23F H -0.0103 0.1891 -0.0419 0.076 Uiso 0.62 1 calc PR A 2 C24B C 0.002(2) 0.1310(9) 0.0924(6) 0.041(3) Uani 0.62 1 d PDU A 2 H24D H -0.0679 0.1535 0.1040 0.062 Uiso 0.62 1 calc PR A 2 H24E H 0.0634 0.1415 0.1387 0.062 Uiso 0.62 1 calc PR A 2 H24F H -0.0179 0.0727 0.0613 0.062 Uiso 0.62 1 calc PR A 2 C25 C 0.4013(4) 0.3658(2) 0.2245(2) 0.0313(10) Uani 1 1 d . A . H25 H 0.4249 0.4235 0.2620 0.038 Uiso 1 1 calc R . . C26 C 0.4714(5) 0.3509(3) 0.1701(3) 0.0521(14) Uani 1 1 d . . . H26A H 0.4422 0.2974 0.1283 0.078 Uiso 1 1 calc R A . H26B H 0.5545 0.3533 0.1952 0.078 Uiso 1 1 calc R . . H26C H 0.4627 0.3922 0.1517 0.078 Uiso 1 1 calc R . . C27 C 0.4347(5) 0.3138(3) 0.2663(3) 0.0469(13) Uani 1 1 d . . . H27A H 0.4165 0.2566 0.2307 0.070 Uiso 1 1 calc R A . H27B H 0.3899 0.3245 0.3019 0.070 Uiso 1 1 calc R . . H27C H 0.5189 0.3271 0.2930 0.070 Uiso 1 1 calc R . . C28 C 0.3781(3) 0.6639(2) 0.1877(2) 0.0237(9) Uani 1 1 d . . . C29 C 0.4685(4) 0.6460(3) 0.1535(2) 0.0302(10) Uani 1 1 d . . . C30 C 0.4723(4) 0.6789(3) 0.1037(2) 0.0439(13) Uani 1 1 d . . . H30 H 0.5312 0.6669 0.0792 0.053 Uiso 1 1 calc R . . C31 C 0.3918(5) 0.7286(3) 0.0894(3) 0.0552(16) Uani 1 1 d . . . C32 C 0.3078(4) 0.7460(3) 0.1244(3) 0.0487(14) Uani 1 1 d . . . H32 H 0.2536 0.7802 0.1145 0.058 Uiso 1 1 calc R . . C33 C 0.2978(4) 0.7155(3) 0.1745(2) 0.0340(11) Uani 1 1 d . . . C34 C 0.5624(4) 0.5978(3) 0.1731(2) 0.0335(10) Uani 1 1 d . . . H34 H 0.5415 0.5785 0.2076 0.040 Uiso 1 1 calc R . . C35 C 0.5738(5) 0.5241(3) 0.1060(3) 0.0537(14) Uani 1 1 d . . . H35A H 0.4995 0.4873 0.0815 0.080 Uiso 1 1 calc R . . H35B H 0.6366 0.4963 0.1224 0.080 Uiso 1 1 calc R . . H35C H 0.5927 0.5415 0.0710 0.080 Uiso 1 1 calc R . . C36 C 0.6823(4) 0.6519(3) 0.2142(3) 0.0505(14) Uani 1 1 d . . . H36A H 0.7110 0.6638 0.1791 0.076 Uiso 1 1 calc R . . H36B H 0.7384 0.6238 0.2359 0.076 Uiso 1 1 calc R . . H36C H 0.6738 0.7024 0.2539 0.076 Uiso 1 1 calc R . . C37 C 0.4002(6) 0.7632(4) 0.0351(3) 0.085(2) Uani 1 1 d . . . H37 H 0.3351 0.7970 0.0382 0.102 Uiso 1 1 calc R . . C38 C 0.3605(6) 0.7071(4) -0.0395(3) 0.0671(18) Uani 1 1 d . . . H38A H 0.3585 0.7348 -0.0711 0.101 Uiso 1 1 calc R . . H38B H 0.2814 0.6806 -0.0505 0.101 Uiso 1 1 calc R . . H38C H 0.4138 0.6665 -0.0493 0.101 Uiso 1 1 calc R . . C39 C 0.5028(5) 0.8254(3) 0.0629(3) 0.0620(17) Uani 1 1 d . . . H39A H 0.5750 0.8008 0.0680 0.093 Uiso 1 1 calc R . . H39B H 0.5040 0.8680 0.1114 0.093 Uiso 1 1 calc R . . H39C H 0.4976 0.8489 0.0277 0.093 Uiso 1 1 calc R . . C40 C 0.2015(4) 0.7376(3) 0.2107(3) 0.0441(12) Uani 1 1 d . . . H40 H 0.2138 0.7158 0.2486 0.053 Uiso 1 1 calc R . . C41 C 0.0798(4) 0.6991(3) 0.1546(4) 0.0678(18) Uani 1 1 d . . . H41A H 0.0691 0.7140 0.1135 0.102 Uiso 1 1 calc R . . H41B H 0.0192 0.7184 0.1792 0.102 Uiso 1 1 calc R . . H41C H 0.0733 0.6402 0.1353 0.102 Uiso 1 1 calc R . . C42 C 0.2046(5) 0.8300(3) 0.2518(3) 0.0578(15) Uani 1 1 d . . . H42A H 0.2835 0.8548 0.2860 0.087 Uiso 1 1 calc R . . H42B H 0.1476 0.8415 0.2799 0.087 Uiso 1 1 calc R . . H42C H 0.1847 0.8523 0.2154 0.087 Uiso 1 1 calc R . . Ge2 Ge 0.81912(7) 0.25040(4) 0.39223(4) 0.03800(15) Uani 0.87 1 d P B 1 I2 I 0.61372(3) 0.23976(3) 0.41335(2) 0.04345(12) Uani 0.87 1 d P B 1 Ge3 Ge 0.7627(4) 0.2232(2) 0.3535(3) 0.0412(11) Uani 0.13 1 d P B 2 Cl3 Cl 0.5950(7) 0.2258(5) 0.3746(5) 0.0224(17) Uani 0.13 1 d PU B 2 C51 C 0.8654(3) 0.1390(2) 0.3603(2) 0.0248(9) Uani 1 1 d . . . C52 C 0.8067(3) 0.0654(2) 0.3003(2) 0.0244(9) Uani 1 1 d . B . C53 C 0.8685(3) -0.0003(2) 0.2791(2) 0.0223(8) Uani 1 1 d . . . C54 C 0.9829(3) 0.0071(2) 0.3236(2) 0.0263(9) Uani 1 1 d . B . H54 H 1.0235 -0.0384 0.3104 0.032 Uiso 1 1 calc R . . C55 C 1.0401(3) 0.0769(2) 0.3858(2) 0.0254(9) Uani 1 1 d . . . C56 C 0.9831(3) 0.1458(2) 0.4017(2) 0.0242(9) Uani 1 1 d . B . C57 C 0.8156(4) -0.0775(3) 0.2082(2) 0.0325(10) Uani 1 1 d . B . H57 H 0.7302 -0.0749 0.1892 0.039 Uiso 1 1 calc R . . C58 C 0.8730(5) -0.0811(3) 0.1496(3) 0.0586(15) Uani 1 1 d . . . H58A H 0.8666 -0.0313 0.1433 0.088 Uiso 1 1 calc R B . H58B H 0.8331 -0.1275 0.1022 0.088 Uiso 1 1 calc R . . H58C H 0.9560 -0.0869 0.1655 0.088 Uiso 1 1 calc R . . C59 C 0.8261(4) -0.1543(3) 0.2190(3) 0.0461(13) Uani 1 1 d . . . H59A H 0.9092 -0.1600 0.2349 0.069 Uiso 1 1 calc R B . H59B H 0.7859 -0.2011 0.1720 0.069 Uiso 1 1 calc R . . H59C H 0.7898 -0.1514 0.2571 0.069 Uiso 1 1 calc R . . C60 C 1.1599(3) 0.0782(3) 0.4375(2) 0.0331(10) Uani 1 1 d . B . H60 H 1.1862 0.1342 0.4783 0.040 Uiso 1 1 calc R . . C61 C 1.2536(4) 0.0553(3) 0.3978(3) 0.0491(13) Uani 1 1 d . . . H61A H 1.2279 0.0014 0.3562 0.074 Uiso 1 1 calc R B . H61B H 1.3273 0.0551 0.4327 0.074 Uiso 1 1 calc R . . H61C H 1.2659 0.0946 0.3790 0.074 Uiso 1 1 calc R . . C62 C 1.1466(4) 0.0218(3) 0.4721(3) 0.0471(13) Uani 1 1 d . . . H62A H 1.0803 0.0331 0.4926 0.071 Uiso 1 1 calc R B . H62B H 1.2188 0.0301 0.5120 0.071 Uiso 1 1 calc R . . H62C H 1.1322 -0.0342 0.4341 0.071 Uiso 1 1 calc R . . C63 C 0.6777(3) 0.0593(2) 0.2624(2) 0.0259(9) Uani 1 1 d . . . C64 C 0.5934(3) 0.0234(2) 0.2815(2) 0.0243(9) Uani 1 1 d . B . C65 C 0.4751(4) 0.0233(3) 0.2500(2) 0.0309(10) Uani 1 1 d . . . H65 H 0.4187 -0.0016 0.2621 0.037 Uiso 1 1 calc R B . C66 C 0.4358(4) 0.0578(3) 0.2020(2) 0.0302(10) Uani 1 1 d . B . C67 C 0.5192(4) 0.0922(3) 0.1838(2) 0.0336(10) Uani 1 1 d . . . H67 H 0.4937 0.1161 0.1507 0.040 Uiso 1 1 calc R B . C68 C 0.6384(4) 0.0929(3) 0.2120(2) 0.0287(9) Uani 1 1 d . B . C69 C 0.6280(4) -0.0156(3) 0.3345(2) 0.0331(10) Uani 1 1 d . . . H69 H 0.7156 -0.0113 0.3504 0.040 Uiso 1 1 calc R B . C70 C 0.5897(5) 0.0280(4) 0.4043(3) 0.072(2) Uani 1 1 d . B . H70A H 0.6347 0.0823 0.4337 0.109 Uiso 1 1 calc R . . H70B H 0.6040 -0.0025 0.4340 0.109 Uiso 1 1 calc R . . H70C H 0.5057 0.0322 0.3898 0.109 Uiso 1 1 calc R . . C71 C 0.5773(5) -0.1055(3) 0.2953(4) 0.0691(19) Uani 1 1 d . B . H71A H 0.4913 -0.1112 0.2793 0.104 Uiso 1 1 calc R . . H71B H 0.6031 -0.1299 0.3297 0.104 Uiso 1 1 calc R . . H71C H 0.6051 -0.1327 0.2518 0.104 Uiso 1 1 calc R . . C72 C 0.3048(4) 0.0587(3) 0.1671(2) 0.0388(11) Uani 1 1 d . . . H72 H 0.2950 0.1165 0.1796 0.047 Uiso 1 1 calc R B . C73 C 0.2241(4) 0.0290(3) 0.1977(3) 0.0451(12) Uani 1 1 d . B . H73A H 0.2332 -0.0270 0.1885 0.068 Uiso 1 1 calc R . . H73B H 0.1427 0.0315 0.1733 0.068 Uiso 1 1 calc R . . H73C H 0.2434 0.0629 0.2513 0.068 Uiso 1 1 calc R . . C74 C 0.2729(5) 0.0147(4) 0.0831(3) 0.0611(16) Uani 1 1 d . B . H74A H 0.2796 -0.0427 0.0681 0.092 Uiso 1 1 calc R . . H74B H 0.3265 0.0377 0.0657 0.092 Uiso 1 1 calc R . . H74C H 0.1920 0.0205 0.0610 0.092 Uiso 1 1 calc R . . C75 C 0.7237(4) 0.1254(3) 0.1837(3) 0.0415(12) Uani 1 1 d . . . H75 H 0.8047 0.1183 0.2076 0.050 Uiso 1 1 calc R B . C76 C 0.7223(5) 0.2182(4) 0.2047(4) 0.073(2) Uani 1 1 d . B . H76A H 0.6411 0.2282 0.1899 0.110 Uiso 1 1 calc R . . H76B H 0.7679 0.2343 0.1786 0.110 Uiso 1 1 calc R . . H76C H 0.7571 0.2497 0.2585 0.110 Uiso 1 1 calc R . . C77 C 0.6950(5) 0.0748(5) 0.1001(3) 0.079(2) Uani 1 1 d . B . H77A H 0.7004 0.0181 0.0895 0.118 Uiso 1 1 calc R . . H77B H 0.7510 0.0939 0.0816 0.118 Uiso 1 1 calc R . . H77C H 0.6151 0.0797 0.0754 0.118 Uiso 1 1 calc R . . C78 C 1.0428(4) 0.2282(2) 0.4607(2) 0.0264(9) Uani 1 1 d . . . C79 C 1.1078(4) 0.2777(3) 0.4422(2) 0.0378(11) Uani 1 1 d . B . C80 C 1.1531(4) 0.3563(3) 0.4940(2) 0.0345(10) Uani 1 1 d . . . H80 H 1.1946 0.3896 0.4807 0.041 Uiso 1 1 calc R B . C81 C 1.1401(4) 0.3880(2) 0.5642(2) 0.0286(9) Uani 1 1 d . B . C82 C 1.0792(3) 0.3388(2) 0.5823(2) 0.0271(9) Uani 1 1 d . . . H82 H 1.0698 0.3599 0.6305 0.033 Uiso 1 1 calc R B . C83 C 1.0306(3) 0.2588(2) 0.5321(2) 0.0244(9) Uani 1 1 d . B . C84 C 1.1318(6) 0.2465(3) 0.3664(3) 0.0610(17) Uani 1 1 d . . . H84 H 1.0975 0.1882 0.3374 0.073 Uiso 1 1 calc R B . C85 C 1.0709(7) 0.2911(4) 0.3236(3) 0.091(3) Uani 1 1 d . B . H85A H 0.9856 0.2781 0.3111 0.137 Uiso 1 1 calc R . . H85B H 1.0929 0.2748 0.2778 0.137 Uiso 1 1 calc R . . H85C H 1.0944 0.3493 0.3541 0.137 Uiso 1 1 calc R . . C86 C 1.2640(6) 0.2523(3) 0.3767(4) 0.087(3) Uani 1 1 d . B . H86A H 1.2777 0.2210 0.3287 0.131 Uiso 1 1 calc R . . H86B H 1.3014 0.2305 0.4117 0.131 Uiso 1 1 calc R . . H86C H 1.2975 0.3089 0.3964 0.131 Uiso 1 1 calc R . . C87 C 1.1869(8) 0.4728(13) 0.6204(17) 0.0310(11) Uani 0.58 1 d PD B 1 H87 H 1.1455 0.4824 0.6587 0.037 Uiso 0.58 1 calc PR B 1 C88 C 1.1529(10) 0.5354(7) 0.5926(6) 0.065(3) Uani 0.58 1 d PDU B 1 H88A H 1.1542 0.5868 0.6347 0.098 Uiso 0.58 1 calc PR B 1 H88B H 1.0737 0.5176 0.5573 0.098 Uiso 0.58 1 calc PR B 1 H88C H 1.2087 0.5425 0.5679 0.098 Uiso 0.58 1 calc PR B 1 C89 C 1.3149(8) 0.4833(6) 0.6620(6) 0.066(2) Uani 0.58 1 d PDU B 1 H89A H 1.3458 0.4322 0.6412 0.099 Uiso 0.58 1 calc PR B 1 H89B H 1.3237 0.4991 0.7146 0.099 Uiso 0.58 1 calc PR B 1 H89C H 1.3586 0.5253 0.6572 0.099 Uiso 0.58 1 calc PR B 1 C87B C 1.1999(12) 0.4752(17) 0.621(2) 0.0310(11) Uani 0.42 1 d PD B 2 H87B H 1.2057 0.4792 0.6716 0.037 Uiso 0.42 1 calc PR B 2 C88B C 1.1190(11) 0.5338(10) 0.6095(9) 0.060(3) Uani 0.42 1 d PDU B 2 H88D H 1.1439 0.5864 0.6529 0.091 Uiso 0.42 1 calc PR B 2 H88E H 1.0384 0.5134 0.6029 0.091 Uiso 0.42 1 calc PR B 2 H88F H 1.1221 0.5395 0.5650 0.091 Uiso 0.42 1 calc PR B 2 C89B C 1.3235(10) 0.4918(8) 0.6206(8) 0.053(2) Uani 0.42 1 d PDU B 2 H89D H 1.3666 0.4478 0.6234 0.080 Uiso 0.42 1 calc PR B 2 H89E H 1.3628 0.5428 0.6634 0.080 Uiso 0.42 1 calc PR B 2 H89F H 1.3214 0.4956 0.5746 0.080 Uiso 0.42 1 calc PR B 2 C90 C 0.9750(4) 0.2063(3) 0.5588(2) 0.0300(10) Uani 1 1 d . . . H90 H 0.9407 0.1530 0.5152 0.036 Uiso 1 1 calc R B . C91 C 0.8769(4) 0.2416(3) 0.5917(3) 0.0449(12) Uani 1 1 d . B . H91A H 0.9085 0.2940 0.6347 0.067 Uiso 1 1 calc R . . H91B H 0.8448 0.2047 0.6074 0.067 Uiso 1 1 calc R . . H91C H 0.8146 0.2487 0.5540 0.067 Uiso 1 1 calc R . . C92 C 1.0689(4) 0.1913(3) 0.6166(3) 0.0419(12) Uani 1 1 d . B . H92A H 1.1335 0.1705 0.5965 0.063 Uiso 1 1 calc R . . H92B H 1.0344 0.1517 0.6286 0.063 Uiso 1 1 calc R . . H92C H 1.0990 0.2420 0.6618 0.063 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 I1 0.0524(2) 0.03571(18) 0.02463(16) 0.00579(13) 0.01318(14) 0.00001(14) Ge1 0.0333(3) 0.0294(3) 0.0180(2) 0.00967(19) -0.00004(18) -0.0035(2) C1 0.0203(19) 0.0181(19) 0.0155(18) 0.0057(16) 0.0031(15) 0.0007(15) C2 0.0184(19) 0.0154(18) 0.0194(19) 0.0070(16) 0.0025(15) 0.0002(15) C3 0.026(2) 0.0173(19) 0.0162(18) 0.0058(16) 0.0031(16) 0.0009(16) C4 0.028(2) 0.018(2) 0.0139(18) 0.0027(16) 0.0005(16) -0.0040(16) C5 0.0179(19) 0.0149(18) 0.0199(19) 0.0053(16) 0.0041(15) 0.0008(15) C6 0.0156(18) 0.020(2) 0.023(2) 0.0092(17) 0.0043(15) 0.0009(15) C7 0.047(3) 0.016(2) 0.020(2) 0.0073(17) 0.0078(19) -0.0086(18) C8 0.053(3) 0.040(3) 0.033(2) 0.019(2) 0.013(2) -0.004(2) C9 0.054(3) 0.032(2) 0.025(2) 0.016(2) 0.005(2) -0.004(2) C10 0.025(2) 0.024(2) 0.021(2) 0.0054(17) 0.0053(17) -0.0078(17) C11 0.052(3) 0.018(2) 0.044(3) 0.000(2) 0.027(2) -0.009(2) C12 0.031(3) 0.037(3) 0.043(3) 0.009(2) -0.013(2) -0.016(2) C13 0.033(2) 0.019(2) 0.0147(18) 0.0083(16) 0.0044(16) -0.0056(17) C14 0.037(2) 0.022(2) 0.021(2) 0.0103(18) 0.0022(18) -0.0081(18) C15 0.050(3) 0.036(3) 0.029(2) 0.016(2) -0.008(2) -0.018(2) C16 0.073(4) 0.019(2) 0.035(3) 0.009(2) -0.020(3) -0.019(2) C17 0.062(3) 0.021(2) 0.032(3) 0.009(2) -0.006(2) 0.000(2) C18 0.045(3) 0.023(2) 0.023(2) 0.0097(18) 0.0047(19) -0.0031(19) C19 0.021(2) 0.040(3) 0.030(2) 0.010(2) -0.0025(18) -0.0091(19) C20 0.031(2) 0.048(3) 0.043(3) 0.024(2) 0.002(2) -0.001(2) C21 0.033(3) 0.086(4) 0.041(3) 0.025(3) 0.013(2) 0.002(3) C22 0.030(5) 0.019(3) 0.026(4) -0.005(3) 0.007(3) -0.003(3) C23 0.043(5) 0.038(5) 0.043(5) -0.006(4) 0.004(5) -0.018(4) C24 0.039(5) 0.022(5) 0.034(9) -0.002(7) -0.004(9) -0.019(4) C22B 0.030(5) 0.019(3) 0.026(4) -0.005(3) 0.007(3) -0.003(3) C23B 0.044(5) 0.036(4) 0.041(4) -0.002(3) -0.003(4) -0.012(4) C24B 0.038(4) 0.025(4) 0.034(8) -0.004(6) -0.004(8) -0.018(4) C25 0.037(2) 0.019(2) 0.033(2) 0.0123(19) 0.0006(19) 0.0051(18) C26 0.047(3) 0.062(4) 0.054(3) 0.032(3) 0.011(3) 0.013(3) C27 0.057(3) 0.036(3) 0.044(3) 0.023(2) 0.001(2) 0.005(2) C28 0.022(2) 0.024(2) 0.021(2) 0.0113(17) -0.0021(16) -0.0119(16) C29 0.030(2) 0.030(2) 0.023(2) 0.0077(19) 0.0032(18) -0.0145(19) C30 0.046(3) 0.049(3) 0.029(2) 0.013(2) 0.009(2) -0.026(2) C31 0.069(4) 0.056(3) 0.032(3) 0.031(3) -0.015(3) -0.030(3) C32 0.042(3) 0.049(3) 0.057(3) 0.042(3) -0.012(3) -0.017(2) C33 0.031(2) 0.028(2) 0.038(3) 0.021(2) -0.008(2) -0.0109(19) C34 0.028(2) 0.031(2) 0.030(2) 0.002(2) 0.0106(19) -0.0079(19) C35 0.051(3) 0.041(3) 0.053(3) -0.002(3) 0.029(3) -0.010(2) C36 0.029(3) 0.031(3) 0.067(4) 0.006(3) 0.003(2) -0.007(2) C37 0.102(5) 0.102(5) 0.044(3) 0.050(4) -0.015(3) -0.055(4) C38 0.091(5) 0.073(4) 0.027(3) 0.022(3) 0.005(3) -0.030(4) C39 0.079(4) 0.063(4) 0.042(3) 0.035(3) -0.003(3) -0.032(3) C40 0.028(2) 0.033(3) 0.071(4) 0.031(3) 0.000(2) 0.004(2) C41 0.036(3) 0.037(3) 0.113(5) 0.030(3) 0.001(3) -0.005(2) C42 0.044(3) 0.029(3) 0.084(4) 0.019(3) 0.003(3) 0.005(2) Ge2 0.0501(4) 0.0292(4) 0.0439(4) 0.0215(3) 0.0190(3) 0.0132(3) I2 0.0401(2) 0.0519(3) 0.0285(2) 0.00786(19) 0.01042(18) 0.01824(18) Ge3 0.037(2) 0.018(2) 0.051(3) 0.009(2) -0.004(2) -0.0046(18) Cl3 0.024(2) 0.022(2) 0.019(2) 0.0086(18) 0.0031(17) 0.0082(17) C51 0.028(2) 0.018(2) 0.032(2) 0.0151(18) 0.0088(18) -0.0006(17) C52 0.023(2) 0.026(2) 0.026(2) 0.0162(18) 0.0025(17) -0.0035(17) C53 0.022(2) 0.0178(19) 0.024(2) 0.0104(17) 0.0006(16) -0.0037(16) C54 0.023(2) 0.025(2) 0.027(2) 0.0102(18) 0.0031(17) 0.0042(17) C55 0.018(2) 0.028(2) 0.026(2) 0.0108(18) 0.0011(16) -0.0045(17) C56 0.025(2) 0.022(2) 0.025(2) 0.0103(18) 0.0068(17) -0.0043(17) C57 0.028(2) 0.027(2) 0.035(2) 0.011(2) 0.0006(19) -0.0020(18) C58 0.066(4) 0.052(3) 0.027(3) -0.006(2) 0.007(3) -0.015(3) C59 0.045(3) 0.021(2) 0.049(3) 0.009(2) -0.011(2) -0.005(2) C60 0.019(2) 0.038(3) 0.028(2) 0.005(2) 0.0007(18) -0.0015(19) C61 0.028(3) 0.066(4) 0.033(3) 0.006(3) 0.003(2) -0.001(2) C62 0.031(3) 0.057(3) 0.053(3) 0.034(3) -0.003(2) 0.007(2) C63 0.024(2) 0.027(2) 0.025(2) 0.0124(18) 0.0018(17) 0.0014(17) C64 0.022(2) 0.029(2) 0.022(2) 0.0137(18) 0.0026(16) -0.0012(17) C65 0.023(2) 0.041(3) 0.031(2) 0.018(2) 0.0061(18) -0.0013(19) C66 0.023(2) 0.042(3) 0.025(2) 0.017(2) 0.0022(18) 0.0033(19) C67 0.026(2) 0.049(3) 0.033(2) 0.027(2) 0.0059(19) 0.007(2) C68 0.026(2) 0.034(2) 0.033(2) 0.020(2) 0.0088(18) 0.0032(18) C69 0.023(2) 0.043(3) 0.042(3) 0.031(2) 0.0050(19) 0.0029(19) C70 0.063(4) 0.141(6) 0.070(4) 0.087(5) 0.039(3) 0.058(4) C71 0.050(3) 0.062(4) 0.105(5) 0.066(4) -0.011(3) -0.017(3) C72 0.027(2) 0.058(3) 0.033(2) 0.025(2) 0.003(2) 0.005(2) C73 0.029(3) 0.062(3) 0.046(3) 0.029(3) 0.005(2) 0.005(2) C74 0.036(3) 0.096(5) 0.038(3) 0.021(3) 0.004(2) 0.007(3) C75 0.034(3) 0.064(3) 0.046(3) 0.042(3) 0.013(2) 0.011(2) C76 0.059(4) 0.084(5) 0.129(6) 0.089(5) 0.038(4) 0.025(3) C77 0.036(3) 0.166(7) 0.035(3) 0.046(4) 0.011(3) 0.001(4) C78 0.029(2) 0.021(2) 0.028(2) 0.0086(18) 0.0091(18) -0.0028(17) C79 0.049(3) 0.029(2) 0.031(2) 0.006(2) 0.017(2) -0.011(2) C80 0.043(3) 0.025(2) 0.035(2) 0.011(2) 0.017(2) -0.011(2) C81 0.031(2) 0.022(2) 0.025(2) 0.0046(18) 0.0078(18) -0.0049(18) C82 0.026(2) 0.028(2) 0.020(2) 0.0061(18) 0.0041(17) -0.0027(18) C83 0.0153(19) 0.027(2) 0.027(2) 0.0110(18) 0.0020(16) -0.0024(16) C84 0.099(5) 0.036(3) 0.043(3) 0.002(3) 0.043(3) -0.026(3) C85 0.158(7) 0.072(4) 0.035(3) 0.010(3) 0.039(4) -0.037(5) C86 0.119(6) 0.044(3) 0.096(5) -0.006(3) 0.090(5) -0.022(4) C87 0.034(3) 0.026(2) 0.026(2) 0.005(2) 0.010(3) -0.006(3) C88 0.069(3) 0.057(3) 0.064(3) 0.026(2) 0.012(2) 0.009(2) C89 0.059(3) 0.056(3) 0.067(3) 0.019(2) 0.009(2) 0.008(2) C87B 0.034(3) 0.026(2) 0.026(2) 0.005(2) 0.010(3) -0.006(3) C88B 0.064(3) 0.056(3) 0.061(3) 0.027(2) 0.017(2) 0.008(2) C89B 0.053(3) 0.050(3) 0.057(3) 0.025(2) 0.015(2) 0.005(2) C90 0.027(2) 0.026(2) 0.028(2) 0.0114(19) -0.0025(18) -0.0134(18) C91 0.036(3) 0.057(3) 0.052(3) 0.032(3) 0.018(2) 0.000(2) C92 0.044(3) 0.045(3) 0.039(3) 0.028(2) 0.001(2) -0.007(2) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag I1 Ge1 2.6221(6) . ? Ge1 C1 2.015(4) . ? C1 C2 1.404(5) . ? C1 C6 1.405(5) . ? C2 C3 1.414(5) . ? C2 C13 1.491(5) . ? C3 C4 1.394(5) . ? C3 C7 1.528(5) . ? C4 C5 1.382(5) . ? C4 H4 0.9500 . ? C5 C6 1.395(5) . ? C5 C10 1.526(5) . ? C6 C28 1.520(5) . ? C7 C8 1.519(6) . ? C7 C9 1.533(6) . ? C7 H7 1.0000 . ? C8 H8A 0.9800 . ? C8 H8B 0.9800 . ? C8 H8C 0.9800 . ? C9 H9A 0.9800 . ? C9 H9B 0.9800 . ? C9 H9C 0.9800 . ? C10 C11 1.521(6) . ? C10 C12 1.535(6) . ? C10 H10 1.0000 . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 C18 1.395(6) . ? C13 C14 1.418(6) . ? C14 C15 1.388(6) . ? C14 C19 1.515(6) . ? C15 C16 1.385(7) . ? C15 H15 0.9500 . ? C16 C17 1.380(7) . ? C16 C22B 1.562(8) . ? C16 C22 1.590(14) . ? C17 C18 1.384(6) . ? C17 H17 0.9500 . ? C18 C25 1.538(6) . ? C19 C21 1.534(6) . ? C19 C20 1.535(6) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.507(9) . ? C22 C23 1.512(9) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C22B C23B 1.502(8) . ? C22B C24B 1.503(8) . ? C22B H22B 1.0000 . ? C23B H23D 0.9800 . ? C23B H23E 0.9800 . ? C23B H23F 0.9800 . ? C24B H24D 0.9800 . ? C24B H24E 0.9800 . ? C24B H24F 0.9800 . ? C25 C26 1.515(6) . ? C25 C27 1.531(6) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.413(6) . ? C28 C33 1.414(6) . ? C29 C30 1.408(6) . ? C29 C34 1.514(6) . ? C30 C31 1.396(8) . ? C30 H30 0.9500 . ? C31 C32 1.356(8) . ? C31 C37 1.529(6) . ? C32 C33 1.400(6) . ? C32 H32 0.9500 . ? C33 C40 1.506(7) . ? C34 C35 1.526(6) . ? C34 C36 1.539(6) . ? C34 H34 1.0000 . ? C35 H35A 0.9800 . ? C35 H35B 0.9800 . ? C35 H35C 0.9800 . ? C36 H36A 0.9800 . ? C36 H36B 0.9800 . ? C36 H36C 0.9800 . ? C37 C38 1.395(8) . ? C37 C39 1.476(7) . ? C37 H37 1.0000 . ? C38 H38A 0.9800 . ? C38 H38B 0.9800 . ? C38 H38C 0.9800 . ? C39 H39A 0.9800 . ? C39 H39B 0.9800 . ? C39 H39C 0.9800 . ? C40 C41 1.533(7) . ? C40 C42 1.547(7) . ? C40 H40 1.0000 . ? C41 H41A 0.9800 . ? C41 H41B 0.9800 . ? C41 H41C 0.9800 . ? C42 H42A 0.9800 . ? C42 H42B 0.9800 . ? C42 H42C 0.9800 . ? Ge2 C51 2.010(4) . ? Ge2 I2 2.6197(8) . ? Ge3 C51 2.017(6) . ? Ge3 Cl3 2.156(9) . ? C51 C52 1.407(5) . ? C51 C56 1.410(5) . ? C52 C53 1.397(5) . ? C52 C63 1.509(5) . ? C53 C54 1.397(5) . ? C53 C57 1.522(5) . ? C54 C55 1.379(5) . ? C54 H54 0.9500 . ? C55 C56 1.405(6) . ? C55 C60 1.534(5) . ? C56 C78 1.505(5) . ? C57 C59 1.523(6) . ? C57 C58 1.527(6) . ? C57 H57 1.0000 . ? C58 H58A 0.9800 . ? C58 H58B 0.9800 . ? C58 H58C 0.9800 . ? C59 H59A 0.9800 . ? C59 H59B 0.9800 . ? C59 H59C 0.9800 . ? C60 C62 1.515(6) . ? C60 C61 1.522(6) . ? C60 H60 1.0000 . ? C61 H61A 0.9800 . ? C61 H61B 0.9800 . ? C61 H61C 0.9800 . ? C62 H62A 0.9800 . ? C62 H62B 0.9800 . ? C62 H62C 0.9800 . ? C63 C68 1.407(5) . ? C63 C64 1.420(5) . ? C64 C65 1.389(5) . ? C64 C69 1.523(5) . ? C65 C66 1.377(6) . ? C65 H65 0.9500 . ? C66 C67 1.385(6) . ? C66 C72 1.542(6) . ? C67 C68 1.383(6) . ? C67 H67 0.9500 . ? C68 C75 1.527(6) . ? C69 C70 1.530(7) . ? C69 C71 1.533(7) . ? C69 H69 1.0000 . ? C70 H70A 0.9800 . ? C70 H70B 0.9800 . ? C70 H70C 0.9800 . ? C71 H71A 0.9800 . ? C71 H71B 0.9800 . ? C71 H71C 0.9800 . ? C72 C73 1.494(6) . ? C72 C74 1.516(6) . ? C72 H72 1.0000 . ? C73 H73A 0.9800 . ? C73 H73B 0.9800 . ? C73 H73C 0.9800 . ? C74 H74A 0.9800 . ? C74 H74B 0.9800 . ? C74 H74C 0.9800 . ? C75 C77 1.522(7) . ? C75 C76 1.580(7) . ? C75 H75 1.0000 . ? C76 H76A 0.9800 . ? C76 H76B 0.9800 . ? C76 H76C 0.9800 . ? C77 H77A 0.9800 . ? C77 H77B 0.9800 . ? C77 H77C 0.9800 . ? C78 C83 1.396(5) . ? C78 C79 1.417(5) . ? C79 C80 1.383(6) . ? C79 C84 1.543(6) . ? C80 C81 1.377(6) . ? C80 H80 0.9500 . ? C81 C82 1.378(5) . ? C81 C87 1.49(3) . ? C81 C87B 1.56(3) . ? C82 C83 1.401(5) . ? C82 H82 0.9500 . ? C83 C90 1.518(5) . ? C84 C85 1.506(9) . ? C84 C86 1.529(9) . ? C84 H84 1.0000 . ? C85 H85A 0.9800 . ? C85 H85B 0.9800 . ? C85 H85C 0.9800 . ? C86 H86A 0.9800 . ? C86 H86B 0.9800 . ? C86 H86C 0.9800 . ? C87 C88 1.506(8) . ? C87 C89 1.506(9) . ? C87 H87 1.0000 . ? C88 H88A 0.9800 . ? C88 H88B 0.9800 . ? C88 H88C 0.9800 . ? C89 H89A 0.9800 . ? C89 H89B 0.9800 . ? C89 H89C 0.9800 . ? C87B C89B 1.506(9) . ? C87B C88B 1.508(8) . ? C87B H87B 1.0000 . ? C88B H88D 0.9800 . ? C88B H88E 0.9800 . ? C88B H88F 0.9800 . ? C89B H89D 0.9800 . ? C89B H89E 0.9800 . ? C89B H89F 0.9800 . ? C90 C91 1.526(6) . ? C90 C92 1.530(6) . ? C90 H90 1.0000 . ? C91 H91A 0.9800 . ? C91 H91B 0.9800 . ? C91 H91C 0.9800 . ? C92 H92A 0.9800 . ? C92 H92B 0.9800 . ? C92 H92C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Ge1 I1 108.99(10) . . ? C2 C1 C6 120.7(3) . . ? C2 C1 Ge1 128.6(3) . . ? C6 C1 Ge1 109.8(3) . . ? C1 C2 C3 118.7(3) . . ? C1 C2 C13 119.4(3) . . ? C3 C2 C13 121.8(3) . . ? C4 C3 C2 118.5(3) . . ? C4 C3 C7 119.9(3) . . ? C2 C3 C7 121.6(3) . . ? C5 C4 C3 123.7(3) . . ? C5 C4 H4 118.2 . . ? C3 C4 H4 118.2 . . ? C4 C5 C6 117.5(3) . . ? C4 C5 C10 120.7(3) . . ? C6 C5 C10 121.7(3) . . ? C5 C6 C1 120.8(3) . . ? C5 C6 C28 122.9(3) . . ? C1 C6 C28 116.3(3) . . ? C8 C7 C3 110.3(3) . . ? C8 C7 C9 110.7(3) . . ? C3 C7 C9 112.3(3) . . ? C8 C7 H7 107.8 . . ? C3 C7 H7 107.8 . . ? C9 C7 H7 107.8 . . ? C7 C8 H8A 109.5 . . ? C7 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? C7 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 109.5 . . ? C7 C9 H9A 109.5 . . ? C7 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? C7 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? C11 C10 C5 113.0(3) . . ? C11 C10 C12 109.8(4) . . ? C5 C10 C12 110.5(3) . . ? C11 C10 H10 107.8 . . ? C5 C10 H10 107.8 . . ? C12 C10 H10 107.8 . . ? C10 C11 H11A 109.5 . . ? C10 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C10 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C10 C12 H12A 109.5 . . ? C10 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C10 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C18 C13 C14 119.2(4) . . ? C18 C13 C2 119.9(4) . . ? C14 C13 C2 120.7(4) . . ? C15 C14 C13 118.7(4) . . ? C15 C14 C19 118.7(4) . . ? C13 C14 C19 122.5(3) . . ? C16 C15 C14 122.0(4) . . ? C16 C15 H15 119.0 . . ? C14 C15 H15 119.0 . . ? C17 C16 C15 118.3(4) . . ? C17 C16 C22B 113.2(5) . . ? C15 C16 C22B 128.2(5) . . ? C17 C16 C22 132.7(6) . . ? C15 C16 C22 107.3(6) . . ? C16 C17 C18 121.8(5) . . ? C16 C17 H17 119.1 . . ? C18 C17 H17 119.1 . . ? C17 C18 C13 119.8(4) . . ? C17 C18 C25 118.5(4) . . ? C13 C18 C25 121.7(4) . . ? C14 C19 C21 110.9(4) . . ? C14 C19 C20 112.9(4) . . ? C21 C19 C20 108.9(4) . . ? C14 C19 H19 108.0 . . ? C21 C19 H19 108.0 . . ? C20 C19 H19 108.0 . . ? 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 . . ? C24 C22 C23 112.5(12) . . ? C24 C22 C16 110.1(14) . . ? C23 C22 C16 96.9(9) . . ? C24 C22 H22 112.1 . . ? C23 C22 H22 112.1 . . ? C16 C22 H22 112.1 . . ? 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 . . ? C23B C22B C24B 113.5(9) . . ? C23B C22B C16 110.5(6) . . ? C24B C22B C16 108.2(7) . . ? C23B C22B H22B 108.1 . . ? C24B C22B H22B 108.1 . . ? C16 C22B H22B 108.1 . . ? C22B C23B H23D 109.5 . . ? C22B C23B H23E 109.5 . . ? H23D C23B H23E 109.5 . . ? C22B C23B H23F 109.5 . . ? H23D C23B H23F 109.5 . . ? H23E C23B H23F 109.5 . . ? C22B C24B H24D 109.5 . . ? C22B C24B H24E 109.5 . . ? H24D C24B H24E 109.5 . . ? C22B C24B H24F 109.5 . . ? H24D C24B H24F 109.5 . . ? H24E C24B H24F 109.5 . . ? C26 C25 C27 110.0(4) . . ? C26 C25 C18 112.2(4) . . ? C27 C25 C18 112.7(4) . . ? C26 C25 H25 107.2 . . ? C27 C25 H25 107.2 . . ? C18 C25 H25 107.2 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C29 C28 C33 121.0(4) . . ? C29 C28 C6 119.8(4) . . ? C33 C28 C6 119.1(3) . . ? C30 C29 C28 117.3(4) . . ? C30 C29 C34 121.0(4) . . ? C28 C29 C34 121.5(3) . . ? C31 C30 C29 121.9(5) . . ? C31 C30 H30 119.1 . . ? C29 C30 H30 119.1 . . ? C32 C31 C30 119.2(4) . . ? C32 C31 C37 121.0(6) . . ? C30 C31 C37 119.8(6) . . ? C31 C32 C33 122.4(5) . . ? C31 C32 H32 118.8 . . ? C33 C32 H32 118.8 . . ? C32 C33 C28 118.0(4) . . ? C32 C33 C40 119.0(4) . . ? C28 C33 C40 122.9(4) . . ? C29 C34 C35 113.7(4) . . ? C29 C34 C36 110.2(4) . . ? C35 C34 C36 108.8(4) . . ? C29 C34 H34 108.0 . . ? C35 C34 H34 108.0 . . ? C36 C34 H34 108.0 . . ? C34 C35 H35A 109.5 . . ? C34 C35 H35B 109.5 . . ? H35A C35 H35B 109.5 . . ? C34 C35 H35C 109.5 . . ? H35A C35 H35C 109.5 . . ? H35B C35 H35C 109.5 . . ? C34 C36 H36A 109.5 . . ? C34 C36 H36B 109.5 . . ? H36A C36 H36B 109.5 . . ? C34 C36 H36C 109.5 . . ? H36A C36 H36C 109.5 . . ? H36B C36 H36C 109.5 . . ? C38 C37 C39 121.1(5) . . ? C38 C37 C31 114.0(5) . . ? C39 C37 C31 114.2(4) . . ? C38 C37 H37 101.0 . . ? C39 C37 H37 101.0 . . ? C31 C37 H37 101.0 . . ? C37 C38 H38A 109.5 . . ? C37 C38 H38B 109.5 . . ? H38A C38 H38B 109.5 . . ? C37 C38 H38C 109.5 . . ? H38A C38 H38C 109.5 . . ? H38B C38 H38C 109.5 . . ? C37 C39 H39A 109.5 . . ? C37 C39 H39B 109.5 . . ? H39A C39 H39B 109.5 . . ? C37 C39 H39C 109.5 . . ? H39A C39 H39C 109.5 . . ? H39B C39 H39C 109.5 . . ? C33 C40 C41 111.8(5) . . ? C33 C40 C42 112.4(4) . . ? C41 C40 C42 109.6(4) . . ? C33 C40 H40 107.6 . . ? C41 C40 H40 107.6 . . ? C42 C40 H40 107.6 . . ? 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 . . ? C51 Ge2 I2 106.37(11) . . ? C51 Ge3 Cl3 121.8(3) . . ? C52 C51 C56 120.8(4) . . ? C52 C51 Ge2 130.3(3) . . ? C56 C51 Ge2 108.1(3) . . ? C52 C51 Ge3 106.0(3) . . ? C56 C51 Ge3 131.7(3) . . ? C53 C52 C51 119.2(4) . . ? C53 C52 C63 122.1(4) . . ? C51 C52 C63 118.7(4) . . ? C52 C53 C54 118.3(4) . . ? C52 C53 C57 121.7(3) . . ? C54 C53 C57 120.0(4) . . ? C55 C54 C53 123.6(4) . . ? C55 C54 H54 118.2 . . ? C53 C54 H54 118.2 . . ? C54 C55 C56 117.8(4) . . ? C54 C55 C60 121.0(4) . . ? C56 C55 C60 121.1(4) . . ? C55 C56 C51 119.5(4) . . ? C55 C56 C78 122.9(4) . . ? C51 C56 C78 117.5(4) . . ? C53 C57 C59 114.1(4) . . ? C53 C57 C58 109.2(3) . . ? C59 C57 C58 109.9(4) . . ? C53 C57 H57 107.8 . . ? C59 C57 H57 107.8 . . ? C58 C57 H57 107.8 . . ? C57 C58 H58A 109.5 . . ? C57 C58 H58B 109.5 . . ? H58A C58 H58B 109.5 . . ? C57 C58 H58C 109.5 . . ? H58A C58 H58C 109.5 . . ? H58B C58 H58C 109.5 . . ? C57 C59 H59A 109.5 . . ? C57 C59 H59B 109.5 . . ? H59A C59 H59B 109.5 . . ? C57 C59 H59C 109.5 . . ? H59A C59 H59C 109.5 . . ? H59B C59 H59C 109.5 . . ? C62 C60 C61 110.1(4) . . ? C62 C60 C55 109.3(3) . . ? C61 C60 C55 112.8(4) . . ? C62 C60 H60 108.2 . . ? C61 C60 H60 108.2 . . ? C55 C60 H60 108.2 . . ? C60 C61 H61A 109.5 . . ? C60 C61 H61B 109.5 . . ? H61A C61 H61B 109.5 . . ? C60 C61 H61C 109.5 . . ? H61A C61 H61C 109.5 . . ? H61B C61 H61C 109.5 . . ? C60 C62 H62A 109.5 . . ? C60 C62 H62B 109.5 . . ? H62A C62 H62B 109.5 . . ? C60 C62 H62C 109.5 . . ? H62A C62 H62C 109.5 . . ? H62B C62 H62C 109.5 . . ? C68 C63 C64 119.0(4) . . ? C68 C63 C52 121.7(4) . . ? C64 C63 C52 119.2(3) . . ? C65 C64 C63 118.5(3) . . ? C65 C64 C69 119.0(4) . . ? C63 C64 C69 122.5(3) . . ? C66 C65 C64 123.0(4) . . ? C66 C65 H65 118.5 . . ? C64 C65 H65 118.5 . . ? C65 C66 C67 117.6(4) . . ? C65 C66 C72 123.6(4) . . ? C67 C66 C72 118.7(4) . . ? C68 C67 C66 122.3(4) . . ? C68 C67 H67 118.8 . . ? C66 C67 H67 118.8 . . ? C67 C68 C63 119.5(4) . . ? C67 C68 C75 118.9(4) . . ? C63 C68 C75 121.5(4) . . ? C64 C69 C70 111.6(4) . . ? C64 C69 C71 110.7(4) . . ? C70 C69 C71 110.7(5) . . ? C64 C69 H69 107.9 . . ? C70 C69 H69 107.9 . . ? C71 C69 H69 107.9 . . ? C69 C70 H70A 109.5 . . ? C69 C70 H70B 109.5 . . ? H70A C70 H70B 109.5 . . ? C69 C70 H70C 109.5 . . ? H70A C70 H70C 109.5 . . ? H70B C70 H70C 109.5 . . ? C69 C71 H71A 109.5 . . ? C69 C71 H71B 109.5 . . ? H71A C71 H71B 109.5 . . ? C69 C71 H71C 109.5 . . ? H71A C71 H71C 109.5 . . ? H71B C71 H71C 109.5 . . ? C73 C72 C74 112.7(4) . . ? C73 C72 C66 113.8(4) . . ? C74 C72 C66 109.9(4) . . ? C73 C72 H72 106.6 . . ? C74 C72 H72 106.6 . . ? C66 C72 H72 106.6 . . ? 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 . . ? C77 C75 C68 108.8(4) . . ? C77 C75 C76 111.9(5) . . ? C68 C75 C76 112.3(4) . . ? C77 C75 H75 107.9 . . ? C68 C75 H75 107.9 . . ? C76 C75 H75 107.9 . . ? C75 C76 H76A 109.5 . . ? C75 C76 H76B 109.5 . . ? H76A C76 H76B 109.5 . . ? C75 C76 H76C 109.5 . . ? H76A C76 H76C 109.5 . . ? H76B C76 H76C 109.5 . . ? C75 C77 H77A 109.5 . . ? C75 C77 H77B 109.5 . . ? H77A C77 H77B 109.5 . . ? C75 C77 H77C 109.5 . . ? H77A C77 H77C 109.5 . . ? H77B C77 H77C 109.5 . . ? C83 C78 C79 119.2(4) . . ? C83 C78 C56 121.6(3) . . ? C79 C78 C56 119.1(4) . . ? C80 C79 C78 119.3(4) . . ? C80 C79 C84 118.4(4) . . ? C78 C79 C84 122.3(4) . . ? C81 C80 C79 122.3(4) . . ? C81 C80 H80 118.9 . . ? C79 C80 H80 118.9 . . ? C80 C81 C82 117.9(4) . . ? C80 C81 C87 123.1(9) . . ? C82 C81 C87 118.9(9) . . ? C80 C81 C87B 119.5(12) . . ? C82 C81 C87B 122.4(12) . . ? C81 C82 C83 122.4(4) . . ? C81 C82 H82 118.8 . . ? C83 C82 H82 118.8 . . ? C78 C83 C82 118.8(4) . . ? C78 C83 C90 122.0(4) . . ? C82 C83 C90 119.0(4) . . ? C85 C84 C86 112.7(5) . . ? C85 C84 C79 110.1(5) . . ? C86 C84 C79 110.6(5) . . ? C85 C84 H84 107.8 . . ? C86 C84 H84 107.8 . . ? C79 C84 H84 107.8 . . ? C84 C85 H85A 109.5 . . ? C84 C85 H85B 109.5 . . ? H85A C85 H85B 109.5 . . ? C84 C85 H85C 109.5 . . ? H85A C85 H85C 109.5 . . ? H85B C85 H85C 109.5 . . ? C84 C86 H86A 109.5 . . ? C84 C86 H86B 109.5 . . ? H86A C86 H86B 109.5 . . ? C84 C86 H86C 109.5 . . ? H86A C86 H86C 109.5 . . ? H86B C86 H86C 109.5 . . ? C81 C87 C88 114.4(16) . . ? C81 C87 C89 112.7(12) . . ? C88 C87 C89 115.0(8) . . ? C81 C87 H87 104.4 . . ? C88 C87 H87 104.4 . . ? C89 C87 H87 104.4 . . ? C87 C88 H88A 109.5 . . ? C87 C88 H88B 109.5 . . ? H88A C88 H88B 109.5 . . ? C87 C88 H88C 109.5 . . ? H88A C88 H88C 109.5 . . ? H88B C88 H88C 109.5 . . ? C87 C89 H89A 109.5 . . ? C87 C89 H89B 109.5 . . ? H89A C89 H89B 109.5 . . ? C87 C89 H89C 109.5 . . ? H89A C89 H89C 109.5 . . ? H89B C89 H89C 109.5 . . ? C89B C87B C88B 115.6(9) . . ? C89B C87B C81 112(2) . . ? C88B C87B C81 108.6(17) . . ? C89B C87B H87B 106.6 . . ? C88B C87B H87B 106.6 . . ? C81 C87B H87B 106.6 . . ? C87B C88B H88D 109.5 . . ? C87B C88B H88E 109.5 . . ? H88D C88B H88E 109.5 . . ? C87B C88B H88F 109.5 . . ? H88D C88B H88F 109.5 . . ? H88E C88B H88F 109.5 . . ? C87B C89B H89D 109.5 . . ? C87B C89B H89E 109.5 . . ? H89D C89B H89E 109.5 . . ? C87B C89B H89F 109.5 . . ? H89D C89B H89F 109.5 . . ? H89E C89B H89F 109.5 . . ? C83 C90 C91 113.8(4) . . ? C83 C90 C92 110.0(3) . . ? C91 C90 C92 109.1(4) . . ? C83 C90 H90 107.9 . . ? C91 C90 H90 107.9 . . ? C92 C90 H90 107.9 . . ? C90 C91 H91A 109.5 . . ? C90 C91 H91B 109.5 . . ? H91A C91 H91B 109.5 . . ? C90 C91 H91C 109.5 . . ? H91A C91 H91C 109.5 . . ? H91B C91 H91C 109.5 . . ? C90 C92 H92A 109.5 . . ? C90 C92 H92B 109.5 . . ? H92A C92 H92B 109.5 . . ? C90 C92 H92C 109.5 . . ? H92A C92 H92C 109.5 . . ? H92B C92 H92C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.997 _diffrn_reflns_theta_full 27.48 _diffrn_measured_fraction_theta_full 0.997 _refine_diff_density_max 1.256 _refine_diff_density_min -1.125 _refine_diff_density_rms 0.099 # Attachment 'CSnCl.cif.txt' data_jf1421ffmi _database_code_depnum_ccdc_archive 'CCDC 771279' #TrackingRef 'CSnCl.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C42 H61 Cl Sn' _chemical_formula_sum 'C42 H61 Cl Sn' _chemical_formula_weight 720.05 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'C 2/c' _symmetry_space_group_name_Hall '-C 2yc' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 16.5067(5) _cell_length_b 9.4895(3) _cell_length_c 26.1959(7) _cell_angle_alpha 90.00 _cell_angle_beta 108.2670(10) _cell_angle_gamma 90.00 _cell_volume 3896.6(2) _cell_formula_units_Z 4 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 8947 _cell_measurement_theta_min 2.47 _cell_measurement_theta_max 27.32 _exptl_crystal_description Block _exptl_crystal_colour Orange _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.23 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.227 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1520 _exptl_absorpt_coefficient_mu 0.750 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.7996 _exptl_absorpt_correction_T_max 0.8977 _exptl_absorpt_process_details 'SADABS 2006/1 (Sheldrick, 2006)' _exptl_special_details ; A light yellow thin block with approximate orthogonal dimensions 0.32 x 0.23 x 0.15mm3 was placed and optically centered on the Bruker APEXII(1) CCD diffractometer at -183\%C. The initial unit cell was indexed using a least-squares analysis of a random set of reflections collected from three series of 0.3\% wide phi-scans, 10 seconds per frame, and 30 frames per series that were well distributed in reciprocal space. Four phi-scan data frame series were collected [MoKa] with 0.3\% wide scans, 60 seconds per frame at varying phi angles. ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART APEXII CCD' _diffrn_measurement_method '\w and \f' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 13465 _diffrn_reflns_av_R_equivalents 0.0227 _diffrn_reflns_av_sigmaI/netI 0.0185 _diffrn_reflns_limit_h_min -19 _diffrn_reflns_limit_h_max 19 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 31 _diffrn_reflns_theta_min 1.64 _diffrn_reflns_theta_max 25.25 _reflns_number_total 3538 _reflns_number_gt 3061 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Apex2 (2.0-2) (Bruker, 2006)' _computing_cell_refinement 'SAINT (7.16A) (Bruker, 2006)' _computing_data_reduction 'SAINT (7.16A) (Bruker, 2006)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL97 _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. Structural determination and Refinement: The crystal to detector distance was 5.23cm, thus providing a complete sphere of data to 2thetamax=55.06\%. A total of 26107 reflections were collected and corrected for Lorentz and polarization effects and absorption using face indexing and Blessing's method as incorporated into the program SADABS(2,3,6) with 4755 unique. All crystallographic calculations were performed on a Personal computer (PC) with a Pentium 3.20GHz processor and 4GB of extended memory. The SHELXTL(4) program package was implemented to determine the probable space group and set up the initial files. System symmetry, systematic absences and intensity statistics indicated the centrosymmetric monoclinic space group C2/c (no. 15). The structure was determined by direct methods with the successful location of nearly all of the non-hydrogen atoms of the molecule using the program XS(5,6). The structure was refined with XL(5,6). The 26107 data collected were merged based upon identical indices yielding 17596 data [R(int)=0.0204] that were further truncated to 2thetamax=50.5\% and merged during least-squares refinement to 12165 unique data [R(int)=0.0250]. A single least-squares difference-Fourier cycle was required to locate the remaining hydrogen atoms. All non-hydrogen atoms were refined anisotropically and all hydrogen atoms were placed in idealized positions during the final convergence stage. The Tin and Chlorine atoms were found to be disordered and placed at 50% occupancy primarily due to the molecule sitting on a 2-fold rotation axis and therefore only half of the molecule required locating. A minor disorder in one of the isopropyl groups was optimized to 0.80:0.20. The final structure was refined to convergence with R(F)=8.21%, wR(F2)=19.70%, GOF=1.097 for all 3538 unique reflections [R(F)=7.38%, wR(F2)=19.04% for those 3061 data with Fo > 4sigma(Fo)]. The final difference-Fourier map was featureless indicating that the structure is both correct and complete. An empirical correction for extinction was also attempted but found to be negative and therefore not applied. References: 1. Bruker (2006) SMART APEX (Version 2.02) and Bruker (2006) SAINT (Version 7.16A). Bruker AXS Inc., Madison, Wisconsin, USA. 2. An Empirical Correction for Absorption Anisotropy, Blessing, R. H. (1995). Acta Cryst., A51, 33-38. 3. Sheldrick, G.M., SADABS (2006/1), 'Siemens Area Detector Absorption Correction' Universit\"at G ttingen: G ttingen, Germany. 4. Sheldrick, G.M., (2002). SHELXTL. Version 6.1. Bruker AXS Inc., Madison, Wisconsin, USA. 5. Sheldrick, G. M., (1997). SHELXS97 and SHELXL97. Universit\"at G ttingen: G ttingen, Germany. 6. A short history of SHELX, George M. Sheldrick, Acta Cryst. (2008). A64, 112-122 220_ALERT_2_B Large Non-Solvent C Ueq(max)/Ueq(min) ... 4.21 Ratio Due to the symmetry of the molecule, isopropyl groups that would otherwise be independent are instead composites and therefore have larger librational moments. 413_ALERT_2_B Short Inter XH3 .. XHn H15A .. H18E .. 2.07 Ang. Short distance between a partial occupancy calculated hydrogen atom H18E 20% and and fully occupied hydrogen atom attached to a terminal carbon atom displaying large libration. ; _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^)+(0.0832P)^2^+19.4419P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 3538 _refine_ls_number_parameters 228 _refine_ls_number_restraints 7 _refine_ls_R_factor_all 0.0821 _refine_ls_R_factor_gt 0.0738 _refine_ls_wR_factor_ref 0.1970 _refine_ls_wR_factor_gt 0.1904 _refine_ls_goodness_of_fit_ref 1.097 _refine_ls_restrained_S_all 1.096 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.46544(4) 0.33614(7) 0.24666(3) 0.0542(3) Uani 0.50 1 d P . . Cl1 Cl 0.60033(18) 0.2422(3) 0.29627(12) 0.0719(8) Uani 0.50 1 d P . . C1 C 0.5000 0.5581(6) 0.2500 0.0296(10) Uani 1 2 d S . . C2 C 0.4959(2) 0.6301(5) 0.20260(14) 0.0343(8) Uani 1 1 d . . . C3 C 0.4955(2) 0.7772(5) 0.20247(18) 0.0461(11) Uani 1 1 d . . . C4 C 0.5000 0.8468(7) 0.2500 0.0552(17) Uani 1 2 d S . . H4 H 0.5000 0.9469 0.2500 0.066 Uiso 1 2 calc SR . . C5 C 0.4897(2) 0.5382(5) 0.15484(13) 0.0382(9) Uani 1 1 d . A . C6 C 0.5619(2) 0.4648(5) 0.15101(15) 0.0417(10) Uani 1 1 d . . . C7 C 0.5512(3) 0.3647(5) 0.11111(17) 0.0509(11) Uani 1 1 d . A . H7 H 0.5995 0.3127 0.1095 0.061 Uiso 1 1 calc R . . C8 C 0.4718(3) 0.3370(6) 0.07284(16) 0.0526(12) Uani 1 1 d D . . C9 C 0.4031(3) 0.4147(6) 0.07623(15) 0.0536(13) Uani 1 1 d . A . H9 H 0.3490 0.3996 0.0502 0.064 Uiso 1 1 calc R . . C10 C 0.4100(2) 0.5134(6) 0.11606(14) 0.0467(11) Uani 1 1 d . . . C11 C 0.4912(3) 0.8643(7) 0.1531(3) 0.0725(18) Uani 1 1 d . . . H11 H 0.4888 0.7982 0.1229 0.087 Uiso 1 1 calc R . . C12 C 0.4111(4) 0.9592(9) 0.1355(4) 0.125(4) Uani 1 1 d . . . H12A H 0.3598 0.9006 0.1281 0.187 Uiso 1 1 calc R . . H12B H 0.4100 1.0109 0.1029 0.187 Uiso 1 1 calc R . . H12C H 0.4128 1.0262 0.1642 0.187 Uiso 1 1 calc R . . C13 C 0.5698(3) 0.9581(7) 0.1624(3) 0.086(2) Uani 1 1 d . . . H13A H 0.6213 0.8994 0.1725 0.129 Uiso 1 1 calc R . . H13B H 0.5726 1.0251 0.1914 0.129 Uiso 1 1 calc R . . H13C H 0.5660 1.0098 0.1294 0.129 Uiso 1 1 calc R . . C14 C 0.6522(3) 0.5044(7) 0.18597(19) 0.0624(15) Uani 1 1 d . . . H14A H 0.6482 0.5499 0.2195 0.075 Uiso 1 1 calc R . . C15 C 0.6884(4) 0.6126(8) 0.1557(4) 0.098(2) Uani 1 1 d . . . H15A H 0.6485 0.6915 0.1444 0.147 Uiso 1 1 calc R . . H15B H 0.6968 0.5681 0.1239 0.147 Uiso 1 1 calc R . . H15C H 0.7433 0.6475 0.1793 0.147 Uiso 1 1 calc R . . C16 C 0.7125(3) 0.3767(7) 0.2023(2) 0.0737(17) Uani 1 1 d . . . H16A H 0.6846 0.3023 0.2166 0.111 Uiso 1 1 calc R . . H16B H 0.7653 0.4054 0.2298 0.111 Uiso 1 1 calc R . . H16C H 0.7259 0.3412 0.1707 0.111 Uiso 1 1 calc R . . C17 C 0.4689(4) 0.2220(8) 0.0316(2) 0.0564(17) Uani 0.80 1 d PD A 1 H17 H 0.5005 0.1380 0.0511 0.068 Uiso 0.80 1 calc PR A 1 C18 C 0.3782(5) 0.1764(9) 0.0005(3) 0.080(2) Uani 0.80 1 d PD A 1 H18A H 0.3483 0.1483 0.0258 0.120 Uiso 0.80 1 calc PR A 1 H18B H 0.3803 0.0965 -0.0228 0.120 Uiso 0.80 1 calc PR A 1 H18C H 0.3479 0.2551 -0.0216 0.120 Uiso 0.80 1 calc PR A 1 C19 C 0.5147(5) 0.2750(8) -0.0072(2) 0.0652(18) Uani 0.80 1 d PD A 1 H19A H 0.5190 0.1982 -0.0312 0.098 Uiso 0.80 1 calc PR A 1 H19B H 0.5720 0.3075 0.0133 0.098 Uiso 0.80 1 calc PR A 1 H19C H 0.4824 0.3532 -0.0285 0.098 Uiso 0.80 1 calc PR A 1 C17B C 0.4432(17) 0.256(2) 0.0196(6) 0.056(10) Uiso 0.20 1 d PD A 2 H17B H 0.4002 0.1846 0.0228 0.067 Uiso 0.20 1 calc PR A 2 C18B C 0.405(2) 0.329(3) -0.0346(8) 0.080(2) Uani 0.20 1 d PD A 2 H18D H 0.3533 0.3800 -0.0348 0.120 Uiso 0.20 1 calc PR A 2 H18E H 0.3911 0.2592 -0.0635 0.120 Uiso 0.20 1 calc PR A 2 H18F H 0.4467 0.3965 -0.0402 0.120 Uiso 0.20 1 calc PR A 2 C19B C 0.5199(18) 0.173(3) 0.0146(15) 0.082(9) Uiso 0.20 1 d PD A 2 H19D H 0.5705 0.2338 0.0247 0.123 Uiso 0.20 1 calc PR A 2 H19E H 0.5083 0.1414 -0.0226 0.123 Uiso 0.20 1 calc PR A 2 H19F H 0.5301 0.0910 0.0386 0.123 Uiso 0.20 1 calc PR A 2 C20 C 0.3303(3) 0.5937(7) 0.11809(17) 0.0628(15) Uani 1 1 d . A . H20 H 0.3491 0.6701 0.1455 0.075 Uiso 1 1 calc R . . C21 C 0.2852(4) 0.6633(9) 0.0633(2) 0.103(3) Uani 1 1 d . . . H21A H 0.2396 0.7252 0.0666 0.154 Uiso 1 1 calc R A . H21B H 0.2607 0.5901 0.0365 0.154 Uiso 1 1 calc R . . H21C H 0.3266 0.7188 0.0519 0.154 Uiso 1 1 calc R . . C22 C 0.2685(3) 0.5003(8) 0.1343(2) 0.0785(19) Uani 1 1 d . . . H22A H 0.2964 0.4616 0.1702 0.118 Uiso 1 1 calc R A . H22B H 0.2503 0.4229 0.1084 0.118 Uiso 1 1 calc R . . H22C H 0.2186 0.5556 0.1347 0.118 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 0.0452(3) 0.0419(4) 0.0723(5) 0.0022(3) 0.0137(3) -0.0070(2) Cl1 0.0658(16) 0.0637(16) 0.0869(19) 0.0174(14) 0.0248(14) 0.0252(13) C1 0.024(2) 0.043(3) 0.025(2) 0.000 0.0117(19) 0.000 C2 0.0213(16) 0.058(2) 0.0261(18) 0.0070(16) 0.0109(13) 0.0022(15) C3 0.0236(18) 0.062(3) 0.056(3) 0.020(2) 0.0166(17) 0.0038(18) C4 0.032(3) 0.045(4) 0.094(5) 0.000 0.029(3) 0.000 C5 0.0285(18) 0.070(3) 0.0199(16) 0.0117(17) 0.0133(14) 0.0018(17) C6 0.0327(19) 0.066(3) 0.0300(19) 0.0015(18) 0.0148(15) 0.0016(18) C7 0.043(2) 0.072(3) 0.042(2) -0.008(2) 0.0197(19) -0.001(2) C8 0.057(3) 0.075(3) 0.027(2) 0.001(2) 0.0155(18) -0.015(2) C9 0.038(2) 0.097(4) 0.0215(18) 0.012(2) 0.0032(16) -0.011(2) C10 0.0307(19) 0.091(3) 0.0186(17) 0.014(2) 0.0084(14) -0.003(2) C11 0.038(2) 0.093(4) 0.089(4) 0.057(3) 0.024(2) 0.006(2) C12 0.052(3) 0.145(7) 0.185(8) 0.124(7) 0.048(4) 0.031(4) C13 0.056(3) 0.083(4) 0.130(6) 0.052(4) 0.044(3) 0.002(3) C14 0.030(2) 0.103(4) 0.052(3) -0.028(3) 0.0104(19) 0.013(2) C15 0.043(3) 0.085(4) 0.164(7) -0.022(5) 0.030(4) -0.019(3) C16 0.040(3) 0.125(5) 0.053(3) -0.009(3) 0.012(2) 0.025(3) C17 0.059(4) 0.076(4) 0.030(3) 0.003(3) 0.006(3) -0.006(4) C18 0.083(5) 0.112(6) 0.035(3) -0.007(3) 0.003(3) -0.031(4) C19 0.093(5) 0.075(4) 0.032(3) -0.002(3) 0.026(3) -0.010(4) C18B 0.083(5) 0.112(6) 0.035(3) -0.007(3) 0.003(3) -0.031(4) C20 0.028(2) 0.123(5) 0.035(2) 0.010(3) 0.0072(17) 0.008(2) C21 0.057(3) 0.189(9) 0.055(3) 0.044(4) 0.008(3) 0.048(4) C22 0.037(2) 0.146(6) 0.053(3) -0.002(3) 0.014(2) -0.013(3) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C1 2.177(5) . ? Sn1 Cl1 2.372(3) . ? C1 C2 1.400(4) . ? C2 C3 1.396(6) . ? C2 C5 1.502(5) . ? C3 C4 1.391(6) . ? C3 C11 1.518(6) . ? C4 H4 0.9500 . ? C5 C10 1.408(5) . ? C5 C6 1.410(5) . ? C6 C7 1.382(6) . ? C6 C14 1.533(6) . ? C7 C8 1.402(6) . ? C7 H7 0.9500 . ? C8 C9 1.379(7) . ? C8 C17 1.525(8) . ? C8 C17B 1.533(11) . ? C9 C10 1.380(7) . ? C9 H9 0.9500 . ? C10 C20 1.535(6) . ? C11 C13 1.529(7) . ? C11 C12 1.545(8) . ? C11 H11 1.0000 . ? C12 H12A 0.9800 . ? C12 H12B 0.9800 . ? C12 H12C 0.9800 . ? C13 H13A 0.9800 . ? C13 H13B 0.9800 . ? C13 H13C 0.9800 . ? C14 C15 1.529(9) . ? C14 C16 1.541(8) . ? C14 H14A 1.0000 . ? C15 H15A 0.9800 . ? C15 H15B 0.9800 . ? C15 H15C 0.9800 . ? C16 H16A 0.9800 . ? C16 H16B 0.9800 . ? C16 H16C 0.9800 . ? C17 C18 1.526(7) . ? C17 C19 1.530(7) . ? C17 H17 1.0000 . ? C18 H18A 0.9800 . ? C18 H18B 0.9800 . ? C18 H18C 0.9800 . ? C19 H19A 0.9800 . ? C19 H19B 0.9800 . ? C19 H19C 0.9800 . ? C17B C19B 1.529(10) . ? C17B C18B 1.531(10) . ? C17B H17B 1.0000 . ? C18B H18D 0.9800 . ? C18B H18E 0.9800 . ? C18B H18F 0.9800 . ? C19B H19D 0.9800 . ? C19B H19E 0.9800 . ? C19B H19F 0.9800 . ? C20 C22 1.509(8) . ? C20 C21 1.543(7) . ? C20 H20 1.0000 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Sn1 Cl1 98.77(9) . . ? C2 C1 C2 121.5(5) 2_655 . ? C2 C1 Sn1 116.6(2) 2_655 . ? C2 C1 Sn1 119.8(3) . . ? C3 C2 C1 119.3(4) . . ? C3 C2 C5 125.4(3) . . ? C1 C2 C5 115.3(4) . . ? C4 C3 C2 118.3(4) . . ? C4 C3 C11 118.7(5) . . ? C2 C3 C11 123.1(5) . . ? C3 C4 C3 123.3(6) . 2_655 ? C3 C4 H4 118.3 . . ? C3 C4 H4 118.3 2_655 . ? C10 C5 C6 119.1(4) . . ? C10 C5 C2 120.1(3) . . ? C6 C5 C2 120.5(3) . . ? C7 C6 C5 118.9(4) . . ? C7 C6 C14 119.3(4) . . ? C5 C6 C14 121.4(4) . . ? C6 C7 C8 122.6(4) . . ? C6 C7 H7 118.7 . . ? C8 C7 H7 118.7 . . ? C9 C8 C7 117.2(4) . . ? C9 C8 C17 125.7(5) . . ? C7 C8 C17 117.1(5) . . ? C9 C8 C17B 107.6(10) . . ? C7 C8 C17B 134.2(11) . . ? C8 C9 C10 122.5(4) . . ? C8 C9 H9 118.8 . . ? C10 C9 H9 118.8 . . ? C9 C10 C5 119.7(4) . . ? C9 C10 C20 119.6(4) . . ? C5 C10 C20 120.6(4) . . ? C3 C11 C13 111.7(5) . . ? C3 C11 C12 112.3(4) . . ? C13 C11 C12 108.2(5) . . ? C3 C11 H11 108.2 . . ? C13 C11 H11 108.2 . . ? C12 C11 H11 108.2 . . ? C11 C12 H12A 109.5 . . ? C11 C12 H12B 109.5 . . ? H12A C12 H12B 109.5 . . ? C11 C12 H12C 109.5 . . ? H12A C12 H12C 109.5 . . ? H12B C12 H12C 109.5 . . ? C11 C13 H13A 109.5 . . ? C11 C13 H13B 109.5 . . ? H13A C13 H13B 109.5 . . ? C11 C13 H13C 109.5 . . ? H13A C13 H13C 109.5 . . ? H13B C13 H13C 109.5 . . ? C15 C14 C6 108.7(4) . . ? C15 C14 C16 110.4(4) . . ? C6 C14 C16 113.3(5) . . ? C15 C14 H14A 108.1 . . ? C6 C14 H14A 108.1 . . ? C16 C14 H14A 108.1 . . ? C14 C15 H15A 109.5 . . ? C14 C15 H15B 109.5 . . ? H15A C15 H15B 109.5 . . ? C14 C15 H15C 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? C14 C16 H16A 109.5 . . ? C14 C16 H16B 109.5 . . ? H16A C16 H16B 109.5 . . ? C14 C16 H16C 109.5 . . ? H16A C16 H16C 109.5 . . ? H16B C16 H16C 109.5 . . ? C18 C17 C8 113.0(6) . . ? C18 C17 C19 110.1(5) . . ? C8 C17 C19 108.8(5) . . ? C18 C17 H17 108.3 . . ? C8 C17 H17 108.3 . . ? C19 C17 H17 108.3 . . ? C19B C17B C18B 105(2) . . ? C19B C17B C8 108.0(19) . . ? C18B C17B C8 122.2(17) . . ? C19B C17B H17B 106.8 . . ? C18B C17B H17B 106.8 . . ? C8 C17B H17B 106.8 . . ? C17B C18B H18D 109.5 . . ? C17B C18B H18E 109.5 . . ? H18D C18B H18E 109.5 . . ? C17B C18B H18F 109.5 . . ? H18D C18B H18F 109.5 . . ? H18E C18B H18F 109.5 . . ? C17B C19B H19D 109.5 . . ? C17B C19B H19E 109.5 . . ? H19D C19B H19E 109.5 . . ? C17B C19B H19F 109.5 . . ? H19D C19B H19F 109.5 . . ? H19E C19B H19F 109.5 . . ? C22 C20 C10 112.4(5) . . ? C22 C20 C21 109.9(4) . . ? C10 C20 C21 110.4(4) . . ? C22 C20 H20 108.0 . . ? C10 C20 H20 108.0 . . ? C21 C20 H20 108.0 . . ? C20 C21 H21A 109.5 . . ? C20 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C20 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C20 C22 H22A 109.5 . . ? C20 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C20 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 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 Cl1 Sn1 Cl1 Sn1 108.0(2) 2_655 . . 2_655 ? C1 Sn1 Cl1 Sn1 -45.40(14) . . . 2_655 ? Sn1 Sn1 C1 C2 -104.19(19) 2_655 . . 2_655 ? Cl1 Sn1 C1 C2 132.0(2) 2_655 . . 2_655 ? Cl1 Sn1 C1 C2 -80.43(19) . . . 2_655 ? Sn1 Sn1 C1 C2 91.80(19) 2_655 . . . ? Cl1 Sn1 C1 C2 -32.0(3) 2_655 . . . ? Cl1 Sn1 C1 C2 115.56(19) . . . . ? Cl1 Sn1 C1 Sn1 -123.79(19) 2_655 . . 2_655 ? Cl1 Sn1 C1 Sn1 23.77(9) . . . 2_655 ? C2 C1 C2 C3 -0.3(2) 2_655 . . . ? Sn1 C1 C2 C3 -164.0(3) 2_655 . . . ? Sn1 C1 C2 C3 162.9(3) . . . . ? C2 C1 C2 C5 -178.7(3) 2_655 . . . ? Sn1 C1 C2 C5 17.6(3) 2_655 . . . ? Sn1 C1 C2 C5 -15.5(3) . . . . ? C1 C2 C3 C4 0.5(5) . . . . ? C5 C2 C3 C4 178.7(3) . . . . ? C1 C2 C3 C11 180.0(3) . . . . ? C5 C2 C3 C11 -1.8(6) . . . . ? C2 C3 C4 C3 -0.2(2) . . . 2_655 ? C11 C3 C4 C3 -179.8(4) . . . 2_655 ? C3 C2 C5 C10 -79.5(5) . . . . ? C1 C2 C5 C10 98.8(4) . . . . ? C3 C2 C5 C6 106.8(5) . . . . ? C1 C2 C5 C6 -74.9(4) . . . . ? C10 C5 C6 C7 -3.7(6) . . . . ? C2 C5 C6 C7 170.0(4) . . . . ? C10 C5 C6 C14 169.6(4) . . . . ? C2 C5 C6 C14 -16.6(6) . . . . ? C5 C6 C7 C8 2.6(7) . . . . ? C14 C6 C7 C8 -170.9(5) . . . . ? C6 C7 C8 C9 0.1(7) . . . . ? C6 C7 C8 C17 -179.0(5) . . . . ? C6 C7 C8 C17B 166.9(15) . . . . ? C7 C8 C9 C10 -1.7(7) . . . . ? C17 C8 C9 C10 177.3(5) . . . . ? C17B C8 C9 C10 -171.8(12) . . . . ? C8 C9 C10 C5 0.5(7) . . . . ? C8 C9 C10 C20 -178.6(4) . . . . ? C6 C5 C10 C9 2.3(6) . . . . ? C2 C5 C10 C9 -171.5(4) . . . . ? C6 C5 C10 C20 -178.6(4) . . . . ? C2 C5 C10 C20 7.6(6) . . . . ? C4 C3 C11 C13 60.5(6) . . . . ? C2 C3 C11 C13 -119.0(6) . . . . ? C4 C3 C11 C12 -61.2(7) . . . . ? C2 C3 C11 C12 119.2(6) . . . . ? C7 C6 C14 C15 82.3(6) . . . . ? C5 C6 C14 C15 -91.0(5) . . . . ? C7 C6 C14 C16 -40.8(6) . . . . ? C5 C6 C14 C16 145.9(4) . . . . ? C9 C8 C17 C18 -12.3(8) . . . . ? C7 C8 C17 C18 166.7(5) . . . . ? C17B C8 C17 C18 -43(3) . . . . ? C9 C8 C17 C19 110.3(6) . . . . ? C7 C8 C17 C19 -70.7(7) . . . . ? C17B C8 C17 C19 80(4) . . . . ? C9 C8 C17B C19B 178.1(19) . . . . ? C7 C8 C17B C19B 10(3) . . . . ? C17 C8 C17B C19B -28(3) . . . . ? C9 C8 C17B C18B 56(3) . . . . ? C7 C8 C17B C18B -112(2) . . . . ? C17 C8 C17B C18B -150(5) . . . . ? C9 C10 C20 C22 69.8(5) . . . . ? C5 C10 C20 C22 -109.3(5) . . . . ? C9 C10 C20 C21 -53.3(7) . . . . ? C5 C10 C20 C21 127.5(5) . . . . ? _diffrn_measured_fraction_theta_max 1.000 _diffrn_reflns_theta_full 25.25 _diffrn_measured_fraction_theta_full 1.000 _refine_diff_density_max 1.494 _refine_diff_density_min -1.055 _refine_diff_density_rms 0.084 # Attachment 'MesGeArSnCl.cif.txt' data_p-1 _database_code_depnum_ccdc_archive 'CCDC 771280' #TrackingRef 'MesGeArSnCl.cif.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C66 H90 Cl1.70 Ge2 I0.30 Sn2, 2(C7 H8)' _chemical_formula_sum 'C80 H106 Cl1.70 Ge2 I0.30 Sn2' _chemical_formula_weight 1548.54 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Cl Cl 0.1484 0.1585 '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' Sn Sn -0.6537 1.4246 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' I I -0.4742 1.8119 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M 'P -1' _symmetry_space_group_name_Hall '-P 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 11.4346(13) _cell_length_b 12.9085(15) _cell_length_c 15.1952(17) _cell_angle_alpha 111.709(2) _cell_angle_beta 103.674(2) _cell_angle_gamma 103.032(2) _cell_volume 1899.2(4) _cell_formula_units_Z 1 _cell_measurement_temperature 90(2) _cell_measurement_reflns_used 5486 _cell_measurement_theta_min 2.58 _cell_measurement_theta_max 27.52 _exptl_crystal_description Plate _exptl_crystal_colour Yellow _exptl_crystal_size_max 0.39 _exptl_crystal_size_mid 0.31 _exptl_crystal_size_min 0.17 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.354 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 795 _exptl_absorpt_coefficient_mu 1.655 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.5660 _exptl_absorpt_correction_T_max 0.7695 _exptl_absorpt_process_details 'SADABS 2008/2 (Sheldrick, 2008)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 90(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART1000 CCD' _diffrn_measurement_method '\w and \f' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 21128 _diffrn_reflns_av_R_equivalents 0.0300 _diffrn_reflns_av_sigmaI/netI 0.0384 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.54 _diffrn_reflns_theta_max 27.50 _reflns_number_total 8693 _reflns_number_gt 7131 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'SMART (Version 5.054) (Bruker, 2002)' _computing_cell_refinement 'SAINT (7.60A) (Bruker, 2008)' _computing_data_reduction 'SAINT (7.60A) (Bruker, 2008)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 2008)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'SHELXTL 5.1, XP (Sheldrick, 1994)' _computing_publication_material SHELXL97 _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. 971_ALERT_2_B Large Calcd. Non-Metal Positive Residual Density 2.60 eA-3 Three peaks as large as large as 2.80 eA-3 were found to be in non-realistic positions and refined to determined their actual occupancy. The largest refined to approx 0.25 C and is out of plane from a disordered toluene molecule while the next two refined to less than 20% C, or less than 1.2e- and all have therefore been omitted from further consideration. ; _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^)+(0.0750P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 8693 _refine_ls_number_parameters 435 _refine_ls_number_restraints 32 _refine_ls_R_factor_all 0.0536 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.1142 _refine_ls_wR_factor_gt 0.1078 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.076 _refine_ls_shift/su_max 0.002 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Sn1 Sn 0.565736(19) 0.145285(16) 0.488865(16) 0.02060(8) Uani 1 1 d . . . Ge1 Ge 0.92923(3) 0.04737(3) 0.17322(2) 0.01856(9) Uani 1 1 d . . . Cl1 Cl 0.3489(7) -0.0355(6) 0.4035(7) 0.0245(6) Uani 0.85 1 d P . 1 I1 I 0.3317(12) -0.0548(9) 0.3955(11) 0.0245(6) Uani 0.15 1 d P . 2 C1 C 0.6674(3) 0.0831(2) 0.3805(2) 0.0158(5) Uani 1 1 d . . . C2 C 0.7418(3) 0.1840(2) 0.3764(2) 0.0162(6) Uani 1 1 d . . . C3 C 0.8219(3) 0.1753(2) 0.3197(2) 0.0169(6) Uani 1 1 d . . . H3 H 0.8735 0.2453 0.3212 0.020 Uiso 1 1 calc R . . C4 C 0.8275(3) 0.0657(2) 0.2611(2) 0.0164(5) Uani 1 1 d . . . C5 C 0.7512(3) -0.0341(2) 0.2625(2) 0.0166(5) Uani 1 1 d . . . H5 H 0.7521 -0.1099 0.2215 0.020 Uiso 1 1 calc R . . C6 C 0.6735(3) -0.0280(2) 0.3211(2) 0.0153(5) Uani 1 1 d . . . C7 C 0.7269(3) 0.3022(2) 0.4291(2) 0.0165(6) Uani 1 1 d . . . C8 C 0.6269(3) 0.3273(2) 0.3761(2) 0.0194(6) Uani 1 1 d . . . C9 C 0.6084(3) 0.4346(3) 0.4257(3) 0.0230(6) Uani 1 1 d . . . H9 H 0.5417 0.4529 0.3908 0.028 Uiso 1 1 calc R . . C10 C 0.6851(3) 0.5138(3) 0.5242(3) 0.0253(7) Uani 1 1 d . . . H10 H 0.6702 0.5854 0.5571 0.030 Uiso 1 1 calc R . . C11 C 0.7842(3) 0.4888(3) 0.5752(2) 0.0229(6) Uani 1 1 d . . . H11 H 0.8373 0.5443 0.6429 0.027 Uiso 1 1 calc R . . C12 C 0.8073(3) 0.3835(2) 0.5289(2) 0.0187(6) Uani 1 1 d . . . C13 C 0.5990(3) -0.1465(2) 0.3124(2) 0.0157(5) Uani 1 1 d . . . C14 C 0.6610(3) -0.1979(2) 0.3670(2) 0.0176(6) Uani 1 1 d . . . C15 C 0.5949(3) -0.3135(3) 0.3494(2) 0.0217(6) Uani 1 1 d . . . H15 H 0.6354 -0.3495 0.3859 0.026 Uiso 1 1 calc R . . C16 C 0.4715(3) -0.3755(3) 0.2797(3) 0.0256(7) Uani 1 1 d . . . H16 H 0.4279 -0.4536 0.2688 0.031 Uiso 1 1 calc R . . C17 C 0.4111(3) -0.3252(3) 0.2260(2) 0.0237(6) Uani 1 1 d . . . H17 H 0.3261 -0.3687 0.1787 0.028 Uiso 1 1 calc R . . C18 C 0.4739(3) -0.2101(3) 0.2404(2) 0.0187(6) Uani 1 1 d . . . C19 C 0.5396(3) 0.2420(3) 0.2677(2) 0.0244(6) Uani 1 1 d . . . H19 H 0.5645 0.1695 0.2472 0.029 Uiso 1 1 calc R . . C20 C 0.3988(3) 0.2027(4) 0.2582(3) 0.0419(9) Uani 1 1 d . . . H20A H 0.3892 0.1672 0.3042 0.063 Uiso 1 1 calc R . . H20B H 0.3461 0.1439 0.1884 0.063 Uiso 1 1 calc R . . H20C H 0.3709 0.2718 0.2760 0.063 Uiso 1 1 calc R . . C21 C 0.5584(4) 0.2963(4) 0.1954(3) 0.0410(9) Uani 1 1 d . . . H21A H 0.5043 0.2382 0.1257 0.062 Uiso 1 1 calc R . . H21B H 0.6486 0.3178 0.2009 0.062 Uiso 1 1 calc R . . H21C H 0.5344 0.3675 0.2134 0.062 Uiso 1 1 calc R . . C22 C 0.9166(3) 0.3605(3) 0.5878(2) 0.0212(6) Uani 1 1 d . . . H22 H 0.9157 0.2802 0.5439 0.025 Uiso 1 1 calc R . . C23 C 0.9022(3) 0.3591(4) 0.6849(3) 0.0366(8) Uani 1 1 d . . . H23A H 0.9136 0.4394 0.7330 0.055 Uiso 1 1 calc R . . H23B H 0.9672 0.3319 0.7149 0.055 Uiso 1 1 calc R . . H23C H 0.8165 0.3050 0.6690 0.055 Uiso 1 1 calc R . . C24 C 1.0461(3) 0.4513(3) 0.6126(3) 0.0349(8) Uani 1 1 d . . . H24A H 1.0554 0.4504 0.5499 0.052 Uiso 1 1 calc R . . H24B H 1.1153 0.4310 0.6465 0.052 Uiso 1 1 calc R . . H24C H 1.0507 0.5307 0.6574 0.052 Uiso 1 1 calc R . . C25 C 0.7987(3) -0.1335(3) 0.4419(2) 0.0208(6) Uani 1 1 d . . . H25 H 0.8159 -0.0461 0.4686 0.025 Uiso 1 1 calc R . . C26 C 0.8243(3) -0.1622(3) 0.5326(3) 0.0287(7) Uani 1 1 d . . . H26A H 0.7616 -0.1472 0.5654 0.043 Uiso 1 1 calc R . . H26B H 0.9111 -0.1118 0.5812 0.043 Uiso 1 1 calc R . . H26C H 0.8165 -0.2460 0.5091 0.043 Uiso 1 1 calc R . . C27 C 0.8954(3) -0.1623(3) 0.3897(3) 0.0276(7) Uani 1 1 d . . . H27A H 0.8733 -0.2487 0.3548 0.041 Uiso 1 1 calc R . . H27B H 0.9821 -0.1266 0.4406 0.041 Uiso 1 1 calc R . . H27C H 0.8925 -0.1300 0.3405 0.041 Uiso 1 1 calc R . . C28 C 0.4090(3) -0.1598(3) 0.1742(2) 0.0228(6) Uani 1 1 d . . . H28 H 0.4388 -0.0716 0.2152 0.027 Uiso 1 1 calc R . . C29 C 0.2619(3) -0.2070(3) 0.1379(3) 0.0318(8) Uani 1 1 d . . . H29A H 0.2294 -0.2909 0.0886 0.048 Uiso 1 1 calc R . . H29B H 0.2279 -0.1612 0.1060 0.048 Uiso 1 1 calc R . . H29C H 0.2346 -0.1989 0.1958 0.048 Uiso 1 1 calc R . . C30 C 0.4490(3) -0.1849(3) 0.0804(3) 0.0329(8) Uani 1 1 d . . . H30A H 0.5420 -0.1468 0.1022 0.049 Uiso 1 1 calc R . . H30B H 0.4052 -0.1528 0.0387 0.049 Uiso 1 1 calc R . . H30C H 0.4251 -0.2708 0.0407 0.049 Uiso 1 1 calc R . . C31 C 1.0585(3) 0.2013(3) 0.2174(3) 0.0297(7) Uani 1 1 d . . . H31A H 1.1117 0.2317 0.2886 0.045 Uiso 1 1 calc R . . H31B H 1.0160 0.2572 0.2101 0.045 Uiso 1 1 calc R . . H31C H 1.1126 0.1923 0.1758 0.045 Uiso 1 1 calc R . . C32 C 1.0098(3) -0.0693(3) 0.1773(3) 0.0306(7) Uani 1 1 d . . . H32A H 1.0542 -0.0826 0.1285 0.046 Uiso 1 1 calc R . . H32B H 0.9440 -0.1442 0.1599 0.046 Uiso 1 1 calc R . . H32C H 1.0718 -0.0397 0.2455 0.046 Uiso 1 1 calc R . . C33 C 0.8146(3) -0.0069(3) 0.0354(3) 0.0337(8) Uani 1 1 d . . . H33A H 0.8616 -0.0258 -0.0112 0.051 Uiso 1 1 calc R . . H33B H 0.7822 0.0559 0.0314 0.051 Uiso 1 1 calc R . . H33C H 0.7425 -0.0781 0.0167 0.051 Uiso 1 1 calc R . . C41 C 0.2049(5) 0.3858(4) 1.0001(3) 0.0505(16) Uani 0.62 1 d PGD A 1 C42 C 0.3036(5) 0.3525(4) 0.9733(4) 0.059(2) Uani 0.62 1 d PGDU A 1 H42 H 0.3403 0.3067 1.0001 0.071 Uiso 0.62 1 calc PR A 1 C43 C 0.3487(4) 0.3864(4) 0.9072(4) 0.0455(17) Uani 0.62 1 d PGU A 1 H43 H 0.4162 0.3636 0.8889 0.055 Uiso 0.62 1 calc PR A 1 C44 C 0.2949(5) 0.4535(4) 0.8680(3) 0.0479(18) Uani 0.62 1 d PG A 1 H44 H 0.3257 0.4766 0.8228 0.057 Uiso 0.62 1 calc PR A 1 C45 C 0.1962(5) 0.4867(4) 0.8948(4) 0.058(2) Uani 0.62 1 d PG A 1 H45 H 0.1595 0.5325 0.8679 0.070 Uiso 0.62 1 calc PR A 1 C46 C 0.1511(4) 0.4529(4) 0.9609(4) 0.0410(17) Uani 0.62 1 d PGDU A 1 H46 H 0.0837 0.4756 0.9792 0.049 Uiso 0.62 1 calc PR A 1 C47 C 0.1553(11) 0.3498(10) 1.0701(8) 0.101(4) Uani 0.62 1 d PDU A 1 H47A H 0.0853 0.3795 1.0794 0.152 Uiso 0.31 1 calc PR A 1 H47B H 0.2245 0.3832 1.1357 0.152 Uiso 0.31 1 calc PR A 1 H47C H 0.1234 0.2629 1.0416 0.152 Uiso 0.31 1 calc PR A 1 H47D H 0.2035 0.3042 1.0917 0.152 Uiso 0.31 1 calc PR A 1 H47E H 0.0642 0.3005 1.0354 0.152 Uiso 0.31 1 calc PR A 1 H47F H 0.1654 0.4209 1.1296 0.152 Uiso 0.31 1 calc PR A 1 C51 C 0.2765(7) 0.4036(7) 0.9450(6) 0.0505(16) Uani 0.38 1 d PGD B 2 C52 C 0.3219(8) 0.3615(8) 1.0133(7) 0.064(3) Uani 0.38 1 d PGDU B 2 H52 H 0.4005 0.3469 1.0195 0.077 Uiso 0.38 1 calc PR B 2 C53 C 0.2523(11) 0.3408(9) 1.0724(7) 0.072(4) Uani 0.38 1 d PG B 2 H53 H 0.2833 0.3120 1.1191 0.086 Uiso 0.38 1 calc PR B 2 C54 C 0.1372(11) 0.3623(10) 1.0632(8) 0.107(5) Uani 0.38 1 d PGU B 2 H54 H 0.0896 0.3481 1.1036 0.128 Uiso 0.38 1 calc PR B 2 C55 C 0.0919(8) 0.4044(9) 0.9949(9) 0.093(7) Uani 0.38 1 d PG B 2 H55 H 0.0132 0.4190 0.9886 0.111 Uiso 0.38 1 calc PR B 2 C56 C 0.1615(7) 0.4251(7) 0.9358(7) 0.036(2) Uani 0.38 1 d PGDU B 2 H56 H 0.1305 0.4539 0.8891 0.044 Uiso 0.38 1 calc PR B 2 C57 C 0.3540(13) 0.4303(14) 0.8857(11) 0.068(4) Uani 0.38 1 d PDU B 2 H57A H 0.3098 0.4604 0.8424 0.102 Uiso 0.19 1 calc PR B 2 H57B H 0.3657 0.3577 0.8435 0.102 Uiso 0.19 1 calc PR B 2 H57C H 0.4380 0.4905 0.9320 0.102 Uiso 0.19 1 calc PR B 2 H57D H 0.4326 0.4120 0.9028 0.102 Uiso 0.19 1 calc PR B 2 H57E H 0.3766 0.5147 0.9017 0.102 Uiso 0.19 1 calc PR B 2 H57F H 0.3043 0.3819 0.8133 0.102 Uiso 0.19 1 calc PR B 2 loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Sn1 0.02228(12) 0.01490(11) 0.02970(13) 0.00986(9) 0.01770(9) 0.00662(8) Ge1 0.01561(16) 0.01845(16) 0.02046(17) 0.00615(13) 0.00997(13) 0.00447(12) Cl1 0.0228(18) 0.022(2) 0.0259(13) 0.0090(15) 0.0123(13) 0.0026(13) I1 0.0228(18) 0.022(2) 0.0259(13) 0.0090(15) 0.0123(13) 0.0026(13) C1 0.0123(12) 0.0168(13) 0.0208(14) 0.0090(11) 0.0080(11) 0.0061(10) C2 0.0152(13) 0.0155(13) 0.0212(14) 0.0100(11) 0.0077(11) 0.0066(11) C3 0.0148(13) 0.0160(13) 0.0210(14) 0.0094(11) 0.0068(11) 0.0047(11) C4 0.0117(12) 0.0197(14) 0.0196(14) 0.0105(12) 0.0060(11) 0.0052(11) C5 0.0161(13) 0.0130(12) 0.0209(14) 0.0057(11) 0.0090(11) 0.0063(11) C6 0.0113(12) 0.0146(13) 0.0174(13) 0.0074(11) 0.0030(11) 0.0016(10) C7 0.0164(13) 0.0129(12) 0.0257(15) 0.0117(11) 0.0126(12) 0.0041(10) C8 0.0174(14) 0.0158(13) 0.0296(16) 0.0122(12) 0.0127(12) 0.0057(11) C9 0.0198(14) 0.0208(14) 0.0358(17) 0.0156(13) 0.0147(13) 0.0099(12) C10 0.0262(16) 0.0161(14) 0.0409(19) 0.0125(14) 0.0208(14) 0.0113(12) C11 0.0240(15) 0.0141(13) 0.0267(16) 0.0052(12) 0.0109(13) 0.0045(12) C12 0.0214(14) 0.0142(13) 0.0245(15) 0.0106(12) 0.0130(12) 0.0048(11) C13 0.0153(13) 0.0114(12) 0.0220(14) 0.0064(11) 0.0112(11) 0.0045(10) C14 0.0168(14) 0.0137(13) 0.0215(14) 0.0065(11) 0.0087(11) 0.0038(11) C15 0.0235(15) 0.0173(14) 0.0291(16) 0.0129(13) 0.0119(13) 0.0083(12) C16 0.0251(16) 0.0138(14) 0.0357(18) 0.0096(13) 0.0135(14) 0.0024(12) C17 0.0179(14) 0.0175(14) 0.0283(16) 0.0058(13) 0.0078(13) 0.0016(11) C18 0.0138(13) 0.0177(14) 0.0241(15) 0.0074(12) 0.0084(12) 0.0061(11) C19 0.0226(15) 0.0253(15) 0.0270(16) 0.0114(13) 0.0090(13) 0.0116(13) C20 0.0210(17) 0.056(2) 0.0317(19) 0.0131(18) 0.0029(15) 0.0019(16) C21 0.051(2) 0.043(2) 0.035(2) 0.0203(18) 0.0195(18) 0.0156(18) C22 0.0225(15) 0.0151(13) 0.0239(15) 0.0077(12) 0.0069(12) 0.0057(11) C23 0.0236(17) 0.053(2) 0.0342(19) 0.0253(18) 0.0094(15) 0.0048(16) C24 0.0231(17) 0.0368(19) 0.056(2) 0.0302(18) 0.0172(17) 0.0116(15) C25 0.0185(14) 0.0165(13) 0.0265(16) 0.0106(12) 0.0057(12) 0.0050(11) C26 0.0262(16) 0.0297(17) 0.0308(18) 0.0165(15) 0.0062(14) 0.0097(14) C27 0.0186(15) 0.0283(17) 0.0385(19) 0.0173(15) 0.0091(14) 0.0098(13) C28 0.0178(14) 0.0235(15) 0.0254(16) 0.0105(13) 0.0057(12) 0.0070(12) C29 0.0189(16) 0.0382(19) 0.0342(19) 0.0136(16) 0.0057(14) 0.0111(14) C30 0.0278(17) 0.044(2) 0.0278(18) 0.0189(16) 0.0087(14) 0.0103(16) C31 0.0253(16) 0.0244(16) 0.0356(19) 0.0091(14) 0.0179(15) 0.0017(13) C32 0.0283(17) 0.0315(18) 0.0350(19) 0.0116(15) 0.0164(15) 0.0160(14) C33 0.0299(18) 0.042(2) 0.0226(17) 0.0114(15) 0.0073(14) 0.0090(16) C41 0.057(4) 0.025(3) 0.040(3) -0.005(2) 0.020(3) -0.008(3) C42 0.062(4) 0.028(3) 0.067(7) 0.014(4) 0.000(4) 0.017(3) C43 0.053(4) 0.027(4) 0.067(4) 0.020(3) 0.039(3) 0.017(3) C44 0.048(4) 0.038(4) 0.042(4) 0.005(3) 0.016(3) 0.010(3) C45 0.043(4) 0.053(4) 0.048(4) 0.015(4) -0.007(3) 0.004(3) C46 0.036(3) 0.032(4) 0.044(4) 0.000(3) 0.018(3) 0.019(2) C47 0.149(8) 0.051(4) 0.069(5) 0.013(4) 0.056(5) -0.019(5) C51 0.057(4) 0.025(3) 0.040(3) -0.005(2) 0.020(3) -0.008(3) C52 0.062(4) 0.031(3) 0.068(7) 0.009(4) -0.008(5) 0.015(3) C53 0.051(8) 0.039(7) 0.077(10) 0.005(7) -0.007(8) -0.002(6) C54 0.152(9) 0.051(6) 0.074(6) 0.009(5) 0.051(6) -0.019(6) C55 0.071(10) 0.027(6) 0.130(15) -0.015(8) 0.060(11) -0.011(6) C56 0.037(3) 0.023(4) 0.043(5) 0.001(4) 0.012(3) 0.024(3) C57 0.070(6) 0.049(6) 0.073(6) 0.014(5) 0.040(5) 0.006(6) _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_site_symmetry_2 _geom_bond_publ_flag Sn1 C1 2.249(3) . ? Sn1 Cl1 2.628(5) . ? Sn1 I1 2.644(16) 2_656 ? Sn1 Cl1 2.686(10) 2_656 ? Sn1 I1 2.868(9) . ? Ge1 C32 1.946(3) . ? Ge1 C33 1.948(3) . ? Ge1 C31 1.950(3) . ? Ge1 C4 1.954(3) . ? Cl1 Sn1 2.686(10) 2_656 ? I1 Sn1 2.644(16) 2_656 ? C1 C6 1.412(4) . ? C1 C2 1.418(4) . ? C2 C3 1.393(4) . ? C2 C7 1.508(4) . ? C3 C4 1.391(4) . ? C3 H3 0.9500 . ? C4 C5 1.394(4) . ? C5 C6 1.394(4) . ? C5 H5 0.9500 . ? C6 C13 1.513(4) . ? C7 C12 1.405(4) . ? C7 C8 1.409(4) . ? C8 C9 1.402(4) . ? C8 C19 1.519(4) . ? C9 C10 1.378(5) . ? C9 H9 0.9500 . ? C10 C11 1.387(5) . ? C10 H10 0.9500 . ? C11 C12 1.399(4) . ? C11 H11 0.9500 . ? C12 C22 1.512(4) . ? C13 C14 1.404(4) . ? C13 C18 1.409(4) . ? C14 C15 1.404(4) . ? C14 C25 1.526(4) . ? C15 C16 1.382(4) . ? C15 H15 0.9500 . ? C16 C17 1.375(5) . ? C16 H16 0.9500 . ? C17 C18 1.405(4) . ? C17 H17 0.9500 . ? C18 C28 1.527(4) . ? C19 C20 1.529(4) . ? C19 C21 1.535(5) . ? C19 H19 1.0000 . ? C20 H20A 0.9800 . ? C20 H20B 0.9800 . ? C20 H20C 0.9800 . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 C24 1.529(4) . ? C22 C23 1.529(4) . ? C22 H22 1.0000 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? C24 H24A 0.9800 . ? C24 H24B 0.9800 . ? C24 H24C 0.9800 . ? C25 C26 1.537(4) . ? C25 C27 1.540(4) . ? C25 H25 1.0000 . ? C26 H26A 0.9800 . ? C26 H26B 0.9800 . ? C26 H26C 0.9800 . ? C27 H27A 0.9800 . ? C27 H27B 0.9800 . ? C27 H27C 0.9800 . ? C28 C29 1.534(4) . ? C28 C30 1.543(5) . ? C28 H28 1.0000 . ? C29 H29A 0.9800 . ? C29 H29B 0.9800 . ? C29 H29C 0.9800 . ? C30 H30A 0.9800 . ? C30 H30B 0.9800 . ? C30 H30C 0.9800 . ? C31 H31A 0.9800 . ? C31 H31B 0.9800 . ? C31 H31C 0.9800 . ? C32 H32A 0.9800 . ? C32 H32B 0.9800 . ? C32 H32C 0.9800 . ? C33 H33A 0.9800 . ? C33 H33B 0.9800 . ? C33 H33C 0.9800 . ? C41 C42 1.3900 . ? C41 C46 1.3900 . ? C41 C47 1.483(6) . ? C42 C43 1.3900 . ? C42 H42 0.9500 . ? C43 C44 1.3900 . ? C43 H43 0.9500 . ? C44 C45 1.3900 . ? C44 H44 0.9500 . ? C45 C46 1.3900 . ? C45 H45 0.9500 . ? C46 H46 0.9500 . ? C47 H47A 0.9800 . ? C47 H47B 0.9800 . ? C47 H47C 0.9800 . ? C47 H47D 0.9800 . ? C47 H47E 0.9800 . ? C47 H47F 0.9800 . ? C51 C52 1.3900 . ? C51 C56 1.3900 . ? C51 C57 1.478(7) . ? C52 C53 1.3900 . ? C52 H52 0.9500 . ? C53 C54 1.3900 . ? C53 H53 0.9500 . ? C54 C55 1.3900 . ? C54 H54 0.9500 . ? C55 C56 1.3900 . ? C55 H55 0.9500 . ? C56 H56 0.9500 . ? C57 H57A 0.9800 . ? C57 H57B 0.9800 . ? C57 H57C 0.9800 . ? C57 H57D 0.9800 . ? C57 H57E 0.9800 . ? C57 H57F 0.9800 . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag C1 Sn1 Cl1 101.0(2) . . ? C1 Sn1 I1 92.8(3) . 2_656 ? Cl1 Sn1 I1 91.2(3) . 2_656 ? C1 Sn1 Cl1 93.0(2) . 2_656 ? Cl1 Sn1 Cl1 86.1(3) . 2_656 ? I1 Sn1 Cl1 5.2(3) 2_656 2_656 ? C1 Sn1 I1 100.3(3) . . ? Cl1 Sn1 I1 1.0(5) . . ? I1 Sn1 I1 90.5(4) 2_656 . ? Cl1 Sn1 I1 85.4(3) 2_656 . ? C32 Ge1 C33 109.34(16) . . ? C32 Ge1 C31 110.65(15) . . ? C33 Ge1 C31 109.40(16) . . ? C32 Ge1 C4 110.42(13) . . ? C33 Ge1 C4 108.12(13) . . ? C31 Ge1 C4 108.86(13) . . ? Sn1 Cl1 Sn1 93.9(3) . 2_656 ? Sn1 I1 Sn1 89.5(4) 2_656 . ? C6 C1 C2 117.2(2) . . ? C6 C1 Sn1 134.9(2) . . ? C2 C1 Sn1 107.90(19) . . ? C3 C2 C1 121.7(3) . . ? C3 C2 C7 119.2(2) . . ? C1 C2 C7 119.0(2) . . ? C4 C3 C2 120.9(3) . . ? C4 C3 H3 119.5 . . ? C2 C3 H3 119.5 . . ? C3 C4 C5 117.3(3) . . ? C3 C4 Ge1 122.5(2) . . ? C5 C4 Ge1 120.0(2) . . ? C6 C5 C4 123.2(3) . . ? C6 C5 H5 118.4 . . ? C4 C5 H5 118.4 . . ? C5 C6 C1 119.6(2) . . ? C5 C6 C13 114.9(2) . . ? C1 C6 C13 125.5(2) . . ? C12 C7 C8 120.8(3) . . ? C12 C7 C2 121.3(3) . . ? C8 C7 C2 117.8(3) . . ? C9 C8 C7 118.4(3) . . ? C9 C8 C19 119.6(3) . . ? C7 C8 C19 122.0(3) . . ? C10 C9 C8 121.2(3) . . ? C10 C9 H9 119.4 . . ? C8 C9 H9 119.4 . . ? C9 C10 C11 119.8(3) . . ? C9 C10 H10 120.1 . . ? C11 C10 H10 120.1 . . ? C10 C11 C12 121.2(3) . . ? C10 C11 H11 119.4 . . ? C12 C11 H11 119.4 . . ? C11 C12 C7 118.5(3) . . ? C11 C12 C22 119.1(3) . . ? C7 C12 C22 122.4(3) . . ? C14 C13 C18 120.8(2) . . ? C14 C13 C6 119.4(2) . . ? C18 C13 C6 119.3(3) . . ? C15 C14 C13 118.6(3) . . ? C15 C14 C25 119.3(3) . . ? C13 C14 C25 122.0(2) . . ? C16 C15 C14 120.7(3) . . ? C16 C15 H15 119.7 . . ? C14 C15 H15 119.7 . . ? C17 C16 C15 120.6(3) . . ? C17 C16 H16 119.7 . . ? C15 C16 H16 119.7 . . ? C16 C17 C18 120.7(3) . . ? C16 C17 H17 119.6 . . ? C18 C17 H17 119.6 . . ? C17 C18 C13 118.6(3) . . ? C17 C18 C28 119.8(3) . . ? C13 C18 C28 121.6(2) . . ? C8 C19 C20 111.7(3) . . ? C8 C19 C21 111.1(3) . . ? C20 C19 C21 111.1(3) . . ? C8 C19 H19 107.6 . . ? C20 C19 H19 107.6 . . ? C21 C19 H19 107.6 . . ? 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 . . ? C12 C22 C24 111.2(2) . . ? C12 C22 C23 112.4(3) . . ? C24 C22 C23 110.0(3) . . ? C12 C22 H22 107.7 . . ? C24 C22 H22 107.7 . . ? C23 C22 H22 107.7 . . ? 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 . . ? C14 C25 C26 113.6(2) . . ? C14 C25 C27 111.3(3) . . ? C26 C25 C27 108.2(3) . . ? C14 C25 H25 107.8 . . ? C26 C25 H25 107.8 . . ? C27 C25 H25 107.8 . . ? C25 C26 H26A 109.5 . . ? C25 C26 H26B 109.5 . . ? H26A C26 H26B 109.5 . . ? C25 C26 H26C 109.5 . . ? H26A C26 H26C 109.5 . . ? H26B C26 H26C 109.5 . . ? C25 C27 H27A 109.5 . . ? C25 C27 H27B 109.5 . . ? H27A C27 H27B 109.5 . . ? C25 C27 H27C 109.5 . . ? H27A C27 H27C 109.5 . . ? H27B C27 H27C 109.5 . . ? C18 C28 C29 114.2(3) . . ? C18 C28 C30 111.0(3) . . ? C29 C28 C30 108.2(3) . . ? C18 C28 H28 107.7 . . ? C29 C28 H28 107.7 . . ? C30 C28 H28 107.7 . . ? 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 . . ? Ge1 C31 H31A 109.5 . . ? Ge1 C31 H31B 109.5 . . ? H31A C31 H31B 109.5 . . ? Ge1 C31 H31C 109.5 . . ? H31A C31 H31C 109.5 . . ? H31B C31 H31C 109.5 . . ? Ge1 C32 H32A 109.5 . . ? Ge1 C32 H32B 109.5 . . ? H32A C32 H32B 109.5 . . ? Ge1 C32 H32C 109.5 . . ? H32A C32 H32C 109.5 . . ? H32B C32 H32C 109.5 . . ? Ge1 C33 H33A 109.5 . . ? Ge1 C33 H33B 109.5 . . ? H33A C33 H33B 109.5 . . ? Ge1 C33 H33C 109.5 . . ? H33A C33 H33C 109.5 . . ? H33B C33 H33C 109.5 . . ? C42 C41 C46 120.0 . . ? C42 C41 C47 120.6(4) . . ? C46 C41 C47 119.4(4) . . ? C41 C42 C43 120.0 . . ? C41 C42 H42 120.0 . . ? C43 C42 H42 120.0 . . ? C44 C43 C42 120.0 . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 120.0 . . ? C43 C44 H44 120.0 . . ? C45 C44 H44 120.0 . . ? C44 C45 C46 120.0 . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C45 C46 C41 120.0 . . ? C45 C46 H46 120.0 . . ? C41 C46 H46 120.0 . . ? C41 C47 H47A 109.5 . . ? C41 C47 H47B 109.5 . . ? H47A C47 H47B 109.5 . . ? C41 C47 H47C 109.5 . . ? H47A C47 H47C 109.5 . . ? H47B C47 H47C 109.5 . . ? C41 C47 H47D 109.5 . . ? H47A C47 H47D 141.1 . . ? H47B C47 H47D 56.3 . . ? H47C C47 H47D 56.3 . . ? C41 C47 H47E 109.5 . . ? H47A C47 H47E 56.3 . . ? H47B C47 H47E 141.1 . . ? H47C C47 H47E 56.3 . . ? H47D C47 H47E 109.5 . . ? C41 C47 H47F 109.5 . . ? H47A C47 H47F 56.3 . . ? H47B C47 H47F 56.3 . . ? H47C C47 H47F 141.1 . . ? H47D C47 H47F 109.5 . . ? H47E C47 H47F 109.5 . . ? C52 C51 C56 120.0 . . ? C52 C51 C57 119.6(4) . . ? C56 C51 C57 120.4(4) . . ? C51 C52 C53 120.0 . . ? C51 C52 H52 120.0 . . ? C53 C52 H52 120.0 . . ? C54 C53 C52 120.0 . . ? C54 C53 H53 120.0 . . ? C52 C53 H53 120.0 . . ? C53 C54 C55 120.0 . . ? C53 C54 H54 120.0 . . ? C55 C54 H54 120.0 . . ? C56 C55 C54 120.0 . . ? C56 C55 H55 120.0 . . ? C54 C55 H55 120.0 . . ? C55 C56 C51 120.0 . . ? C55 C56 H56 120.0 . . ? C51 C56 H56 120.0 . . ? C51 C57 H57A 109.5 . . ? C51 C57 H57B 109.5 . . ? H57A C57 H57B 109.5 . . ? C51 C57 H57C 109.5 . . ? H57A C57 H57C 109.5 . . ? H57B C57 H57C 109.5 . . ? C51 C57 H57D 109.5 . . ? H57A C57 H57D 141.1 . . ? H57B C57 H57D 56.3 . . ? H57C C57 H57D 56.3 . . ? C51 C57 H57E 109.5 . . ? H57A C57 H57E 56.3 . . ? H57B C57 H57E 141.1 . . ? H57C C57 H57E 56.3 . . ? H57D C57 H57E 109.5 . . ? C51 C57 H57F 109.5 . . ? H57A C57 H57F 56.3 . . ? H57B C57 H57F 56.3 . . ? H57C C57 H57F 141.1 . . ? H57D C57 H57F 109.5 . . ? H57E C57 H57F 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 C1 Sn1 Cl1 Sn1 92.3(2) . . . 2_656 ? I1 Sn1 Cl1 Sn1 -0.8(5) 2_656 . . 2_656 ? Cl1 Sn1 Cl1 Sn1 0.0 2_656 . . 2_656 ? I1 Sn1 Cl1 Sn1 43(29) . . . 2_656 ? C1 Sn1 I1 Sn1 92.9(3) . . . 2_656 ? Cl1 Sn1 I1 Sn1 -136(29) . . . 2_656 ? I1 Sn1 I1 Sn1 0.0 2_656 . . 2_656 ? Cl1 Sn1 I1 Sn1 0.7(5) 2_656 . . 2_656 ? Cl1 Sn1 C1 C6 -35.4(4) . . . . ? I1 Sn1 C1 C6 56.4(3) 2_656 . . . ? Cl1 Sn1 C1 C6 51.2(3) 2_656 . . . ? I1 Sn1 C1 C6 -34.6(4) . . . . ? Cl1 Sn1 C1 C2 145.8(3) . . . . ? I1 Sn1 C1 C2 -122.4(3) 2_656 . . . ? Cl1 Sn1 C1 C2 -127.5(2) 2_656 . . . ? I1 Sn1 C1 C2 146.6(4) . . . . ? C6 C1 C2 C3 -2.6(4) . . . . ? Sn1 C1 C2 C3 176.4(2) . . . . ? C6 C1 C2 C7 173.2(2) . . . . ? Sn1 C1 C2 C7 -7.8(3) . . . . ? C1 C2 C3 C4 2.9(4) . . . . ? C7 C2 C3 C4 -172.9(3) . . . . ? C2 C3 C4 C5 -0.7(4) . . . . ? C2 C3 C4 Ge1 175.7(2) . . . . ? C32 Ge1 C4 C3 141.4(2) . . . . ? C33 Ge1 C4 C3 -99.0(3) . . . . ? C31 Ge1 C4 C3 19.7(3) . . . . ? C32 Ge1 C4 C5 -42.2(3) . . . . ? C33 Ge1 C4 C5 77.4(3) . . . . ? C31 Ge1 C4 C5 -163.9(2) . . . . ? C3 C4 C5 C6 -1.6(4) . . . . ? Ge1 C4 C5 C6 -178.2(2) . . . . ? C4 C5 C6 C1 1.8(4) . . . . ? C4 C5 C6 C13 -179.5(3) . . . . ? C2 C1 C6 C5 0.3(4) . . . . ? Sn1 C1 C6 C5 -178.4(2) . . . . ? C2 C1 C6 C13 -178.2(3) . . . . ? Sn1 C1 C6 C13 3.2(5) . . . . ? C3 C2 C7 C12 -90.8(3) . . . . ? C1 C2 C7 C12 93.3(3) . . . . ? C3 C2 C7 C8 91.0(3) . . . . ? C1 C2 C7 C8 -84.9(3) . . . . ? C12 C7 C8 C9 -1.0(4) . . . . ? C2 C7 C8 C9 177.2(2) . . . . ? C12 C7 C8 C19 179.1(3) . . . . ? C2 C7 C8 C19 -2.8(4) . . . . ? C7 C8 C9 C10 -0.3(4) . . . . ? C19 C8 C9 C10 179.6(3) . . . . ? C8 C9 C10 C11 1.1(4) . . . . ? C9 C10 C11 C12 -0.7(5) . . . . ? C10 C11 C12 C7 -0.6(4) . . . . ? C10 C11 C12 C22 -180.0(3) . . . . ? C8 C7 C12 C11 1.4(4) . . . . ? C2 C7 C12 C11 -176.7(3) . . . . ? C8 C7 C12 C22 -179.2(3) . . . . ? C2 C7 C12 C22 2.7(4) . . . . ? C5 C6 C13 C14 79.8(3) . . . . ? C1 C6 C13 C14 -101.6(3) . . . . ? C5 C6 C13 C18 -92.3(3) . . . . ? C1 C6 C13 C18 86.2(4) . . . . ? C18 C13 C14 C15 -1.0(4) . . . . ? C6 C13 C14 C15 -173.0(3) . . . . ? C18 C13 C14 C25 177.1(3) . . . . ? C6 C13 C14 C25 5.1(4) . . . . ? C13 C14 C15 C16 0.2(4) . . . . ? C25 C14 C15 C16 -177.9(3) . . . . ? C14 C15 C16 C17 0.1(5) . . . . ? C15 C16 C17 C18 0.4(5) . . . . ? C16 C17 C18 C13 -1.2(4) . . . . ? C16 C17 C18 C28 175.3(3) . . . . ? C14 C13 C18 C17 1.5(4) . . . . ? C6 C13 C18 C17 173.5(3) . . . . ? C14 C13 C18 C28 -175.0(3) . . . . ? C6 C13 C18 C28 -2.9(4) . . . . ? C9 C8 C19 C20 -58.9(4) . . . . ? C7 C8 C19 C20 121.1(3) . . . . ? C9 C8 C19 C21 65.7(4) . . . . ? C7 C8 C19 C21 -114.3(3) . . . . ? C11 C12 C22 C24 -64.7(4) . . . . ? C7 C12 C22 C24 115.9(3) . . . . ? C11 C12 C22 C23 59.1(4) . . . . ? C7 C12 C22 C23 -120.3(3) . . . . ? C15 C14 C25 C26 -35.0(4) . . . . ? C13 C14 C25 C26 147.0(3) . . . . ? C15 C14 C25 C27 87.5(3) . . . . ? C13 C14 C25 C27 -90.6(3) . . . . ? C17 C18 C28 C29 30.1(4) . . . . ? C13 C18 C28 C29 -153.5(3) . . . . ? C17 C18 C28 C30 -92.5(3) . . . . ? C13 C18 C28 C30 83.9(3) . . . . ? C46 C41 C42 C43 0.0 . . . . ? C47 C41 C42 C43 179.7(7) . . . . ? C41 C42 C43 C44 0.0 . . . . ? C42 C43 C44 C45 0.0 . . . . ? C43 C44 C45 C46 0.0 . . . . ? C44 C45 C46 C41 0.0 . . . . ? C42 C41 C46 C45 0.0 . . . . ? C47 C41 C46 C45 -179.7(7) . . . . ? C56 C51 C52 C53 0.0 . . . . ? C57 C51 C52 C53 177.4(10) . . . . ? C51 C52 C53 C54 0.0 . . . . ? C52 C53 C54 C55 0.0 . . . . ? C53 C54 C55 C56 0.0 . . . . ? C54 C55 C56 C51 0.0 . . . . ? C52 C51 C56 C55 0.0 . . . . ? C57 C51 C56 C55 -177.3(10) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 27.50 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 2.797 _refine_diff_density_min -0.764 _refine_diff_density_rms 0.128