# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2002 data_global _journal_coden_Cambridge 440 _publ_requested_journal 'New Journal of Chemistry' loop_ _publ_author_name 'Steed, Jonathan W.' 'McGrady, G. S.' 'Prince, Paul D.' _publ_contact_author_name 'Dr Jonathan W Steed' _publ_contact_author_address ; Department of Chemistry King's College London Strand London WC2R 2LS UNITED KINGDOM ; _publ_contact_author_email 'JON.STEED@KCL.AC.UK' _publ_section_title ; Weak Interactions Induce Asymmetry in the Crystal Structures of Triaryl Derivatives of Group 14 Elements ; data_ppgei #(compound1) _database_code_CSD 179372 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H15 Ge I' _chemical_formula_weight 430.79 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' 'Ge' 'Ge' 0.1547 1.8001 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.5925(4) _cell_length_b 9.6743(3) _cell_length_c 18.3085(8) _cell_angle_alpha 83.959(3) _cell_angle_beta 78.664(2) _cell_angle_gamma 77.060(2) _cell_volume 1620.26(11) _cell_formula_units_Z 4 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.25 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.766 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 832 _exptl_absorpt_coefficient_mu 3.784 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.4514 _exptl_absorpt_correction_T_max 0.6007 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '1.9o phi + omega scans 6s/o' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 9565 _diffrn_reflns_av_R_equivalents 0.0493 _diffrn_reflns_av_sigmaI/netI 0.0615 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 2.38 _diffrn_reflns_theta_max 25.00 _reflns_number_total 5696 _reflns_number_gt 4829 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 1999)' _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. ; _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^)+(0.0279P)^2^+2.2505P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5696 _refine_ls_number_parameters 361 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0450 _refine_ls_R_factor_gt 0.0333 _refine_ls_wR_factor_ref 0.0818 _refine_ls_wR_factor_gt 0.0770 _refine_ls_goodness_of_fit_ref 1.019 _refine_ls_restrained_S_all 1.019 _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 0.17792(3) 0.47524(3) 0.116127(17) 0.02753(10) Uani 1 1 d . . . Ge1 Ge 0.33159(5) 0.24435(5) 0.06315(2) 0.01612(11) Uani 1 1 d . . . C1 C 0.3541(5) 0.2787(4) -0.0443(2) 0.0163(9) Uani 1 1 d . . . I2 I 0.39802(4) 0.81781(3) 0.401097(17) 0.02958(10) Uani 1 1 d . . . Ge2 Ge 0.20780(5) 0.66641(5) 0.44291(2) 0.01548(11) Uani 1 1 d . . . C2 C 0.2324(5) 0.3178(5) -0.0793(2) 0.0220(10) Uani 1 1 d . . . H2 H 0.1374 0.3301 -0.0502 0.026 Uiso 1 1 calc R . . C3 C 0.2509(5) 0.3387(5) -0.1567(2) 0.0215(10) Uani 1 1 d . . . H3 H 0.1683 0.3659 -0.1804 0.026 Uiso 1 1 calc R . . C4 C 0.3894(5) 0.3201(5) -0.1996(2) 0.0231(10) Uani 1 1 d . . . H4 H 0.4019 0.3325 -0.2524 0.028 Uiso 1 1 calc R . . C5 C 0.5089(5) 0.2834(5) -0.1647(2) 0.0231(10) Uani 1 1 d . . . H5 H 0.6038 0.2726 -0.1938 0.028 Uiso 1 1 calc R . . C6 C 0.4921(5) 0.2623(4) -0.0880(2) 0.0201(10) Uani 1 1 d . . . H6 H 0.5755 0.2363 -0.0649 0.024 Uiso 1 1 calc R . . C7 C 0.2257(5) 0.0947(4) 0.1009(2) 0.0181(9) Uani 1 1 d . . . C8 C 0.1954(5) 0.0599(5) 0.1772(2) 0.0212(10) Uani 1 1 d . . . H8 H 0.2241 0.1115 0.2111 0.025 Uiso 1 1 calc R . . C9 C 0.1233(5) -0.0502(5) 0.2043(3) 0.0258(11) Uani 1 1 d . . . H9 H 0.1028 -0.0731 0.2565 0.031 Uiso 1 1 calc R . . C10 C 0.0813(5) -0.1262(5) 0.1555(3) 0.0279(11) Uani 1 1 d . . . H10 H 0.0315 -0.2007 0.1741 0.033 Uiso 1 1 calc R . . C11 C 0.1124(5) -0.0933(5) 0.0790(3) 0.0244(10) Uani 1 1 d . . . H11 H 0.0855 -0.1466 0.0453 0.029 Uiso 1 1 calc R . . C12 C 0.1833(5) 0.0181(4) 0.0517(2) 0.0202(10) Uani 1 1 d . . . H12 H 0.2027 0.0416 -0.0005 0.024 Uiso 1 1 calc R . . C13 C 0.5152(4) 0.2163(4) 0.0974(2) 0.0173(9) Uani 1 1 d . . . C14 C 0.5969(5) 0.3212(5) 0.0832(3) 0.0232(10) Uani 1 1 d . . . H14 H 0.5600 0.4091 0.0583 0.028 Uiso 1 1 calc R . . C15 C 0.7312(5) 0.2999(5) 0.1046(3) 0.0274(11) Uani 1 1 d . . . H15 H 0.7861 0.3724 0.0938 0.033 Uiso 1 1 calc R . . C16 C 0.7856(5) 0.1729(5) 0.1418(3) 0.0267(11) Uani 1 1 d . . . H16 H 0.8775 0.1576 0.1568 0.032 Uiso 1 1 calc R . . C17 C 0.7035(5) 0.0683(5) 0.1568(2) 0.0241(10) Uani 1 1 d . . . H17 H 0.7395 -0.0187 0.1827 0.029 Uiso 1 1 calc R . . C18 C 0.5715(5) 0.0890(4) 0.1348(2) 0.0191(9) Uani 1 1 d . . . H18 H 0.5176 0.0158 0.1451 0.023 Uiso 1 1 calc R . . C19 C 0.1695(5) 0.6604(4) 0.5510(2) 0.0157(9) Uani 1 1 d . . . C20 C 0.2807(5) 0.6179(5) 0.5925(2) 0.0207(10) Uani 1 1 d . . . H20 H 0.3785 0.5896 0.5679 0.025 Uiso 1 1 calc R . . C21 C 0.2486(5) 0.6168(5) 0.6699(3) 0.0266(11) Uani 1 1 d . . . H21 H 0.3250 0.5891 0.6979 0.032 Uiso 1 1 calc R . . C22 C 0.1065(6) 0.6558(5) 0.7065(2) 0.0255(11) Uani 1 1 d . . . H22 H 0.0856 0.6541 0.7595 0.031 Uiso 1 1 calc R . . C23 C -0.0052(5) 0.6972(5) 0.6661(3) 0.0242(10) Uani 1 1 d . . . H23 H -0.1029 0.7233 0.6912 0.029 Uiso 1 1 calc R . . C24 C 0.0261(5) 0.7003(4) 0.5884(2) 0.0178(9) Uani 1 1 d . . . H24 H -0.0505 0.7298 0.5606 0.021 Uiso 1 1 calc R . . C25 C 0.2930(4) 0.4835(4) 0.4032(2) 0.0170(9) Uani 1 1 d . . . C26 C 0.3328(5) 0.4710(5) 0.3261(2) 0.0217(10) Uani 1 1 d . . . H26 H 0.3172 0.5540 0.2935 0.026 Uiso 1 1 calc R . . C27 C 0.3940(5) 0.3422(5) 0.2959(3) 0.0266(11) Uani 1 1 d . . . H27 H 0.4211 0.3363 0.2434 0.032 Uiso 1 1 calc R . . C28 C 0.4155(5) 0.2203(5) 0.3437(3) 0.0269(11) Uani 1 1 d . . . H28 H 0.4560 0.1305 0.3235 0.032 Uiso 1 1 calc R . . C29 C 0.3783(5) 0.2290(5) 0.4203(3) 0.0249(10) Uani 1 1 d . . . H29 H 0.3944 0.1457 0.4526 0.030 Uiso 1 1 calc R . . C30 C 0.3172(5) 0.3602(5) 0.4497(2) 0.0200(10) Uani 1 1 d . . . H30 H 0.2915 0.3659 0.5023 0.024 Uiso 1 1 calc R . . C31 C 0.0370(5) 0.7636(4) 0.4025(2) 0.0166(9) Uani 1 1 d . . . C32 C -0.0206(5) 0.9079(5) 0.4124(2) 0.0234(10) Uani 1 1 d . . . H32 H 0.0280 0.9604 0.4364 0.028 Uiso 1 1 calc R . . C33 C -0.1484(5) 0.9753(5) 0.3876(2) 0.0254(11) Uani 1 1 d . . . H33 H -0.1876 1.0731 0.3949 0.030 Uiso 1 1 calc R . . C34 C -0.2178(5) 0.8983(5) 0.3522(3) 0.0276(11) Uani 1 1 d . . . H34 H -0.3048 0.9439 0.3348 0.033 Uiso 1 1 calc R . . C35 C -0.1627(5) 0.7573(5) 0.3419(2) 0.0234(10) Uani 1 1 d . . . H35 H -0.2122 0.7059 0.3177 0.028 Uiso 1 1 calc R . . C36 C -0.0355(5) 0.6884(5) 0.3664(2) 0.0217(10) Uani 1 1 d . . . H36 H 0.0023 0.5905 0.3587 0.026 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 0.02530(18) 0.02365(17) 0.02773(18) -0.00483(13) -0.00060(13) 0.00508(13) Ge1 0.0145(2) 0.0176(2) 0.0145(2) -0.00152(17) -0.00208(18) -0.00002(18) C1 0.018(2) 0.012(2) 0.019(2) -0.0009(17) -0.0063(18) -0.0005(17) I2 0.0310(2) 0.03000(18) 0.02944(18) -0.00422(13) 0.00358(14) -0.01669(14) Ge2 0.0161(2) 0.0148(2) 0.0152(2) -0.00159(17) -0.00203(18) -0.00281(18) C2 0.013(2) 0.024(2) 0.025(2) -0.0042(19) -0.0009(19) 0.0030(18) C3 0.025(3) 0.024(2) 0.017(2) 0.0017(18) -0.011(2) -0.0036(19) C4 0.027(3) 0.023(2) 0.017(2) 0.0007(18) -0.004(2) 0.000(2) C5 0.021(3) 0.020(2) 0.021(2) 0.0030(18) 0.006(2) -0.0007(19) C6 0.018(2) 0.019(2) 0.022(2) 0.0030(18) -0.0064(19) -0.0009(18) C7 0.012(2) 0.021(2) 0.019(2) -0.0013(18) 0.0009(18) -0.0004(18) C8 0.014(2) 0.027(2) 0.019(2) -0.0046(19) 0.0010(18) 0.0009(19) C9 0.023(3) 0.029(3) 0.019(2) 0.005(2) 0.001(2) 0.000(2) C10 0.017(3) 0.021(2) 0.041(3) 0.002(2) -0.001(2) -0.0015(19) C11 0.017(2) 0.025(3) 0.031(3) -0.011(2) -0.003(2) -0.0006(19) C12 0.017(2) 0.019(2) 0.020(2) -0.0064(18) 0.0011(19) 0.0036(18) C13 0.011(2) 0.021(2) 0.016(2) -0.0049(17) -0.0004(17) 0.0033(17) C14 0.024(3) 0.016(2) 0.030(3) -0.0006(19) -0.008(2) -0.0018(19) C15 0.029(3) 0.021(2) 0.037(3) -0.006(2) -0.010(2) -0.010(2) C16 0.019(2) 0.031(3) 0.031(3) -0.014(2) -0.007(2) -0.001(2) C17 0.024(3) 0.023(2) 0.024(2) -0.0046(19) -0.009(2) 0.005(2) C18 0.022(2) 0.017(2) 0.019(2) -0.0024(17) -0.0016(19) -0.0056(18) C19 0.020(2) 0.014(2) 0.016(2) -0.0043(16) -0.0046(18) -0.0061(18) C20 0.018(2) 0.019(2) 0.024(2) 0.0001(18) -0.0082(19) 0.0003(18) C21 0.031(3) 0.030(3) 0.024(3) 0.005(2) -0.016(2) -0.012(2) C22 0.043(3) 0.023(2) 0.015(2) -0.0019(18) -0.007(2) -0.015(2) C23 0.022(3) 0.022(2) 0.027(3) -0.0088(19) 0.007(2) -0.007(2) C24 0.016(2) 0.015(2) 0.024(2) -0.0047(17) -0.0057(19) -0.0024(17) C25 0.012(2) 0.021(2) 0.018(2) -0.0022(17) -0.0037(18) -0.0016(17) C26 0.021(2) 0.021(2) 0.022(2) -0.0034(19) -0.0033(19) -0.0017(19) C27 0.025(3) 0.032(3) 0.023(2) -0.012(2) -0.001(2) -0.007(2) C28 0.023(3) 0.020(2) 0.039(3) -0.012(2) -0.009(2) 0.0027(19) C29 0.019(2) 0.019(2) 0.035(3) 0.002(2) -0.010(2) 0.0011(19) C30 0.016(2) 0.023(2) 0.022(2) 0.0020(18) -0.0063(19) -0.0035(18) C31 0.016(2) 0.019(2) 0.014(2) -0.0011(17) -0.0012(18) -0.0042(18) C32 0.032(3) 0.020(2) 0.018(2) -0.0034(18) -0.003(2) -0.006(2) C33 0.031(3) 0.015(2) 0.025(3) 0.0012(19) -0.003(2) 0.003(2) C34 0.026(3) 0.031(3) 0.025(3) 0.007(2) -0.009(2) -0.003(2) C35 0.024(3) 0.024(2) 0.025(2) -0.0037(19) -0.007(2) -0.006(2) C36 0.027(3) 0.017(2) 0.021(2) -0.0015(18) -0.003(2) -0.0059(19) _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 2.5539(5) . ? Ge1 C1 1.937(4) . ? Ge1 C13 1.937(4) . ? Ge1 C7 1.943(4) . ? C1 C6 1.391(6) . ? C1 C2 1.400(6) . ? I2 Ge2 2.5442(5) . ? Ge2 C25 1.928(4) . ? Ge2 C31 1.938(4) . ? Ge2 C19 1.938(4) . ? C2 C3 1.393(6) . ? C3 C4 1.388(6) . ? C4 C5 1.380(6) . ? C5 C6 1.381(6) . ? C7 C8 1.390(6) . ? C7 C12 1.396(6) . ? C8 C9 1.395(6) . ? C9 C10 1.384(7) . ? C10 C11 1.391(7) . ? C11 C12 1.398(6) . ? C13 C14 1.390(6) . ? C13 C18 1.395(6) . ? C14 C15 1.385(6) . ? C15 C16 1.386(7) . ? C16 C17 1.390(7) . ? C17 C18 1.370(6) . ? C19 C20 1.393(6) . ? C19 C24 1.399(6) . ? C20 C21 1.389(6) . ? C21 C22 1.384(7) . ? C22 C23 1.383(7) . ? C23 C24 1.393(6) . ? C25 C30 1.394(6) . ? C25 C26 1.399(6) . ? C26 C27 1.376(6) . ? C27 C28 1.394(6) . ? C28 C29 1.383(7) . ? C29 C30 1.389(6) . ? C31 C36 1.399(6) . ? C31 C32 1.398(6) . ? C32 C33 1.390(6) . ? C33 C34 1.382(7) . ? C34 C35 1.366(7) . ? C35 C36 1.387(6) . ? 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 C13 111.91(18) . . ? C1 Ge1 C7 112.83(18) . . ? C13 Ge1 C7 113.02(17) . . ? C1 Ge1 I1 105.26(12) . . ? C13 Ge1 I1 105.86(13) . . ? C7 Ge1 I1 107.28(13) . . ? C6 C1 C2 118.9(4) . . ? C6 C1 Ge1 120.2(3) . . ? C2 C1 Ge1 120.8(3) . . ? C25 Ge2 C31 113.01(18) . . ? C25 Ge2 C19 113.61(17) . . ? C31 Ge2 C19 111.18(18) . . ? C25 Ge2 I2 106.01(12) . . ? C31 Ge2 I2 106.58(12) . . ? C19 Ge2 I2 105.78(12) . . ? C3 C2 C1 119.9(4) . . ? C4 C3 C2 120.4(4) . . ? C5 C4 C3 119.5(4) . . ? C6 C5 C4 120.8(4) . . ? C5 C6 C1 120.5(4) . . ? C8 C7 C12 119.3(4) . . ? C8 C7 Ge1 120.3(3) . . ? C12 C7 Ge1 120.4(3) . . ? C7 C8 C9 120.5(4) . . ? C10 C9 C8 120.2(4) . . ? C9 C10 C11 119.8(4) . . ? C12 C11 C10 120.1(4) . . ? C11 C12 C7 120.1(4) . . ? C14 C13 C18 118.1(4) . . ? C14 C13 Ge1 120.7(3) . . ? C18 C13 Ge1 121.2(3) . . ? C15 C14 C13 121.2(4) . . ? C16 C15 C14 120.0(4) . . ? C15 C16 C17 118.9(4) . . ? C18 C17 C16 120.9(4) . . ? C17 C18 C13 120.8(4) . . ? C20 C19 C24 119.1(4) . . ? C20 C19 Ge2 121.8(3) . . ? C24 C19 Ge2 119.0(3) . . ? C19 C20 C21 120.0(4) . . ? C22 C21 C20 120.6(4) . . ? C21 C22 C23 120.1(4) . . ? C22 C23 C24 119.8(4) . . ? C23 C24 C19 120.5(4) . . ? C30 C25 C26 117.9(4) . . ? C30 C25 Ge2 121.6(3) . . ? C26 C25 Ge2 120.5(3) . . ? C27 C26 C25 122.0(4) . . ? C26 C27 C28 118.9(4) . . ? C29 C28 C27 120.6(4) . . ? C28 C29 C30 119.7(4) . . ? C25 C30 C29 121.0(4) . . ? C36 C31 C32 118.8(4) . . ? C36 C31 Ge2 120.3(3) . . ? C32 C31 Ge2 120.7(3) . . ? C31 C32 C33 120.7(4) . . ? C34 C33 C32 119.3(4) . . ? C35 C34 C33 120.7(4) . . ? C34 C35 C36 120.8(4) . . ? C35 C36 C31 119.7(4) . . ? 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 C13 Ge1 C1 C6 8.6(4) . . . . ? C7 Ge1 C1 C6 -120.2(3) . . . . ? I1 Ge1 C1 C6 123.1(3) . . . . ? C13 Ge1 C1 C2 -172.6(3) . . . . ? C7 Ge1 C1 C2 58.6(4) . . . . ? I1 Ge1 C1 C2 -58.1(4) . . . . ? C6 C1 C2 C3 0.4(6) . . . . ? Ge1 C1 C2 C3 -178.4(3) . . . . ? C1 C2 C3 C4 0.4(7) . . . . ? C2 C3 C4 C5 -1.3(7) . . . . ? C3 C4 C5 C6 1.3(7) . . . . ? C4 C5 C6 C1 -0.5(7) . . . . ? C2 C1 C6 C5 -0.3(6) . . . . ? Ge1 C1 C6 C5 178.5(3) . . . . ? C1 Ge1 C7 C8 -177.7(3) . . . . ? C13 Ge1 C7 C8 54.0(4) . . . . ? I1 Ge1 C7 C8 -62.3(4) . . . . ? C1 Ge1 C7 C12 4.3(4) . . . . ? C13 Ge1 C7 C12 -123.9(4) . . . . ? I1 Ge1 C7 C12 119.8(3) . . . . ? C12 C7 C8 C9 -0.1(7) . . . . ? Ge1 C7 C8 C9 -178.1(3) . . . . ? C7 C8 C9 C10 0.1(7) . . . . ? C8 C9 C10 C11 0.5(7) . . . . ? C9 C10 C11 C12 -1.2(7) . . . . ? C10 C11 C12 C7 1.3(7) . . . . ? C8 C7 C12 C11 -0.6(6) . . . . ? Ge1 C7 C12 C11 177.4(3) . . . . ? C1 Ge1 C13 C14 59.0(4) . . . . ? C7 Ge1 C13 C14 -172.3(3) . . . . ? I1 Ge1 C13 C14 -55.1(4) . . . . ? C1 Ge1 C13 C18 -118.9(4) . . . . ? C7 Ge1 C13 C18 9.8(4) . . . . ? I1 Ge1 C13 C18 126.9(3) . . . . ? C18 C13 C14 C15 0.8(7) . . . . ? Ge1 C13 C14 C15 -177.2(4) . . . . ? C13 C14 C15 C16 -0.9(7) . . . . ? C14 C15 C16 C17 0.1(7) . . . . ? C15 C16 C17 C18 0.6(7) . . . . ? C16 C17 C18 C13 -0.7(7) . . . . ? C14 C13 C18 C17 0.0(7) . . . . ? Ge1 C13 C18 C17 178.0(3) . . . . ? C25 Ge2 C19 C20 62.2(4) . . . . ? C31 Ge2 C19 C20 -169.0(3) . . . . ? I2 Ge2 C19 C20 -53.7(4) . . . . ? C25 Ge2 C19 C24 -118.0(3) . . . . ? C31 Ge2 C19 C24 10.8(4) . . . . ? I2 Ge2 C19 C24 126.1(3) . . . . ? C24 C19 C20 C21 -0.6(6) . . . . ? Ge2 C19 C20 C21 179.2(3) . . . . ? C19 C20 C21 C22 0.9(7) . . . . ? C20 C21 C22 C23 -0.4(7) . . . . ? C21 C22 C23 C24 -0.4(6) . . . . ? C22 C23 C24 C19 0.7(6) . . . . ? C20 C19 C24 C23 -0.2(6) . . . . ? Ge2 C19 C24 C23 180.0(3) . . . . ? C31 Ge2 C25 C30 -125.3(3) . . . . ? C19 Ge2 C25 C30 2.6(4) . . . . ? I2 Ge2 C25 C30 118.3(3) . . . . ? C31 Ge2 C25 C26 54.9(4) . . . . ? C19 Ge2 C25 C26 -177.3(3) . . . . ? I2 Ge2 C25 C26 -61.5(4) . . . . ? C30 C25 C26 C27 0.1(7) . . . . ? Ge2 C25 C26 C27 179.9(3) . . . . ? C25 C26 C27 C28 0.6(7) . . . . ? C26 C27 C28 C29 -1.1(7) . . . . ? C27 C28 C29 C30 0.9(7) . . . . ? C26 C25 C30 C29 -0.3(6) . . . . ? Ge2 C25 C30 C29 179.8(3) . . . . ? C28 C29 C30 C25 -0.1(7) . . . . ? C25 Ge2 C31 C36 17.2(4) . . . . ? C19 Ge2 C31 C36 -112.0(3) . . . . ? I2 Ge2 C31 C36 133.2(3) . . . . ? C25 Ge2 C31 C32 -166.4(3) . . . . ? C19 Ge2 C31 C32 64.4(4) . . . . ? I2 Ge2 C31 C32 -50.4(4) . . . . ? C36 C31 C32 C33 0.6(6) . . . . ? Ge2 C31 C32 C33 -175.8(3) . . . . ? C31 C32 C33 C34 -0.5(7) . . . . ? C32 C33 C34 C35 0.4(7) . . . . ? C33 C34 C35 C36 -0.4(7) . . . . ? C34 C35 C36 C31 0.4(6) . . . . ? C32 C31 C36 C35 -0.5(6) . . . . ? Ge2 C31 C36 C35 175.9(3) . . . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.647 _refine_diff_density_min -1.219 _refine_diff_density_rms 0.155 #===END data_pp2023 #(compound2) _database_code_CSD 179373 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H15 F Ge' _chemical_formula_weight 322.89 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' 'F' 'F' 0.0171 0.0103 '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 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 10.3444(8) _cell_length_b 11.7723(7) _cell_length_c 13.0869(11) _cell_angle_alpha 90.00 _cell_angle_beta 110.328(4) _cell_angle_gamma 90.00 _cell_volume 1494.43(19) _cell_formula_units_Z 4 _cell_measurement_temperature 120(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.80 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.435 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 2.047 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.2912 _exptl_absorpt_correction_T_max 0.8215 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 120(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 KappaCCD _diffrn_measurement_method '2o phi scans 5s/o' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 7391 _diffrn_reflns_av_R_equivalents 0.1399 _diffrn_reflns_av_sigmaI/netI 0.1079 _diffrn_reflns_limit_h_min -12 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -13 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.10 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2621 _reflns_number_gt 2173 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XSeed (Barbour, 1999)' _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. ; _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^)+(0.1127P)^2^+0.2553P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.008(3) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 2621 _refine_ls_number_parameters 242 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0759 _refine_ls_R_factor_gt 0.0619 _refine_ls_wR_factor_ref 0.1714 _refine_ls_wR_factor_gt 0.1585 _refine_ls_goodness_of_fit_ref 1.030 _refine_ls_restrained_S_all 1.030 _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 0.25194(4) 0.02299(4) 0.18300(4) 0.0173(3) Uani 1 1 d . . . F1 F 0.3793(3) 0.0333(2) 0.3121(2) 0.0241(7) Uani 1 1 d . . . C1 C 0.3029(4) -0.1095(4) 0.1183(3) 0.0176(9) Uani 1 1 d . . . C2 C 0.4165(5) -0.1026(4) 0.0838(4) 0.0225(10) Uani 1 1 d . . . H2 H 0.473(6) -0.031(4) 0.090(4) 0.024(14) Uiso 1 1 d . . . C3 C 0.4573(5) -0.1954(4) 0.0383(4) 0.0260(10) Uani 1 1 d . . . H3 H 0.533(5) -0.186(4) 0.020(4) 0.020(11) Uiso 1 1 d . . . C4 C 0.3840(5) -0.2977(4) 0.0245(4) 0.0268(10) Uani 1 1 d . . . H4 H 0.414(6) -0.365(5) -0.014(5) 0.041(15) Uiso 1 1 d . . . C5 C 0.2713(5) -0.3051(4) 0.0586(4) 0.0288(11) Uani 1 1 d . . . H5 H 0.221(6) -0.374(6) 0.051(5) 0.043(16) Uiso 1 1 d . . . C6 C 0.2314(5) -0.2118(4) 0.1051(4) 0.0234(10) Uani 1 1 d . . . H6 H 0.155(4) -0.220(4) 0.127(3) 0.008(10) Uiso 1 1 d . . . C7 C 0.0814(5) 0.0117(3) 0.2113(4) 0.0174(9) Uani 1 1 d . . . C8 C 0.0600(5) -0.0734(4) 0.2792(4) 0.0247(10) Uani 1 1 d . . . H8 H 0.138(6) -0.130(6) 0.316(5) 0.057(19) Uiso 1 1 d . . . C9 C -0.0620(5) -0.0793(4) 0.2999(4) 0.0304(12) Uani 1 1 d . . . H9 H -0.063(5) -0.138(5) 0.352(4) 0.035(15) Uiso 1 1 d . . . C10 C -0.1650(6) -0.0012(5) 0.2527(4) 0.0316(12) Uani 1 1 d . . . H10 H -0.248(6) -0.004(4) 0.259(4) 0.015(11) Uiso 1 1 d . . . C11 C -0.1468(5) 0.0836(4) 0.1854(4) 0.0251(10) Uani 1 1 d . . . H11 H -0.214(5) 0.135(5) 0.154(4) 0.027(13) Uiso 1 1 d . . . C12 C -0.0242(5) 0.0883(4) 0.1649(4) 0.0218(10) Uani 1 1 d . . . H12 H -0.019(4) 0.153(4) 0.122(4) 0.011(10) Uiso 1 1 d . . . C13 C 0.2645(4) 0.1634(3) 0.1095(4) 0.0171(9) Uani 1 1 d . . . C14 C 0.3563(4) 0.2487(4) 0.1634(4) 0.0220(10) Uani 1 1 d . . . H14 H 0.416(5) 0.242(4) 0.234(4) 0.023(12) Uiso 1 1 d . . . C15 C 0.3614(5) 0.3494(4) 0.1102(4) 0.0245(10) Uani 1 1 d . . . H15 H 0.429(4) 0.404(4) 0.152(3) 0.008(10) Uiso 1 1 d . . . C16 C 0.2742(5) 0.3660(4) 0.0039(4) 0.0247(10) Uani 1 1 d . . . H16 H 0.273(5) 0.438(5) -0.037(4) 0.022(12) Uiso 1 1 d . . . C17 C 0.1834(5) 0.2829(4) -0.0504(4) 0.0284(11) Uani 1 1 d . . . H17 H 0.123(5) 0.295(4) -0.119(4) 0.023(13) Uiso 1 1 d . . . C18 C 0.1792(5) 0.1805(4) 0.0020(4) 0.0230(10) Uani 1 1 d . . . H18 H 0.121(6) 0.116(5) -0.039(4) 0.043(16) 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 Ge1 0.0187(4) 0.0196(4) 0.0167(4) -0.00045(15) 0.0102(3) 0.00136(15) F1 0.0225(14) 0.0301(15) 0.0216(15) -0.0019(10) 0.0100(12) 0.0042(10) C1 0.018(2) 0.024(2) 0.012(2) 0.0000(17) 0.0070(17) 0.0014(17) C2 0.026(2) 0.023(2) 0.022(2) -0.0013(18) 0.013(2) -0.0001(19) C3 0.025(2) 0.036(3) 0.023(3) 0.004(2) 0.016(2) 0.009(2) C4 0.033(3) 0.026(2) 0.025(3) -0.0022(19) 0.014(2) 0.004(2) C5 0.035(3) 0.023(2) 0.030(3) -0.003(2) 0.013(2) 0.001(2) C6 0.023(2) 0.029(2) 0.022(2) 0.0016(19) 0.013(2) 0.0008(19) C7 0.025(3) 0.015(2) 0.016(2) -0.0024(16) 0.012(2) 0.0015(17) C8 0.032(3) 0.023(2) 0.025(3) 0.0015(19) 0.017(2) 0.003(2) C9 0.036(3) 0.025(3) 0.038(3) 0.008(2) 0.024(3) 0.003(2) C10 0.028(3) 0.040(3) 0.038(3) -0.002(2) 0.026(3) -0.003(2) C11 0.023(2) 0.022(2) 0.032(3) 0.001(2) 0.012(2) 0.005(2) C12 0.023(2) 0.021(2) 0.024(2) -0.0019(19) 0.011(2) -0.0044(19) C13 0.018(2) 0.016(2) 0.022(2) 0.0009(17) 0.0128(19) 0.0054(16) C14 0.018(2) 0.029(2) 0.024(3) -0.0052(19) 0.013(2) -0.0008(19) C15 0.023(2) 0.025(2) 0.032(3) -0.008(2) 0.018(2) -0.0050(19) C16 0.032(3) 0.021(2) 0.031(3) 0.000(2) 0.022(2) 0.0003(19) C17 0.034(3) 0.031(3) 0.021(3) 0.007(2) 0.012(2) 0.005(2) C18 0.023(2) 0.026(2) 0.020(2) -0.0003(19) 0.008(2) -0.0012(19) _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 F1 1.749(3) . ? Ge1 C7 1.929(5) . ? Ge1 C1 1.933(4) . ? Ge1 C13 1.939(4) . ? C1 C6 1.393(7) . ? C1 C2 1.400(6) . ? C2 C3 1.379(7) . ? C3 C4 1.401(7) . ? C4 C5 1.388(7) . ? C5 C6 1.386(7) . ? C7 C12 1.384(7) . ? C7 C8 1.407(6) . ? C8 C9 1.381(7) . ? C9 C10 1.380(8) . ? C10 C11 1.386(7) . ? C11 C12 1.387(6) . ? C13 C18 1.391(6) . ? C13 C14 1.394(6) . ? C14 C15 1.385(7) . ? C15 C16 1.383(7) . ? C16 C17 1.372(7) . ? C17 C18 1.395(7) . ? 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 F1 Ge1 C7 104.57(16) . . ? F1 Ge1 C1 104.53(15) . . ? C7 Ge1 C1 115.79(17) . . ? F1 Ge1 C13 105.20(16) . . ? C7 Ge1 C13 112.19(17) . . ? C1 Ge1 C13 113.24(18) . . ? C6 C1 C2 118.6(4) . . ? C6 C1 Ge1 122.5(3) . . ? C2 C1 Ge1 118.8(3) . . ? C3 C2 C1 120.7(4) . . ? C2 C3 C4 120.2(4) . . ? C5 C4 C3 119.3(4) . . ? C6 C5 C4 120.2(5) . . ? C5 C6 C1 120.9(4) . . ? C12 C7 C8 117.9(4) . . ? C12 C7 Ge1 120.4(3) . . ? C8 C7 Ge1 121.7(3) . . ? C9 C8 C7 121.0(4) . . ? C10 C9 C8 119.6(5) . . ? C9 C10 C11 120.7(5) . . ? C10 C11 C12 119.1(4) . . ? C7 C12 C11 121.6(4) . . ? C18 C13 C14 119.3(4) . . ? C18 C13 Ge1 119.8(3) . . ? C14 C13 Ge1 121.0(3) . . ? C15 C14 C13 120.0(4) . . ? C16 C15 C14 120.1(4) . . ? C17 C16 C15 120.6(4) . . ? C16 C17 C18 119.6(5) . . ? C13 C18 C17 120.3(4) . . ? 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 F1 Ge1 C1 C6 106.7(4) . . . . ? C7 Ge1 C1 C6 -7.8(4) . . . . ? C13 Ge1 C1 C6 -139.4(4) . . . . ? F1 Ge1 C1 C2 -73.0(4) . . . . ? C7 Ge1 C1 C2 172.6(3) . . . . ? C13 Ge1 C1 C2 41.0(4) . . . . ? C6 C1 C2 C3 -0.3(7) . . . . ? Ge1 C1 C2 C3 179.3(4) . . . . ? C1 C2 C3 C4 0.9(7) . . . . ? C2 C3 C4 C5 -1.0(7) . . . . ? C3 C4 C5 C6 0.5(7) . . . . ? C4 C5 C6 C1 0.1(8) . . . . ? C2 C1 C6 C5 -0.2(7) . . . . ? Ge1 C1 C6 C5 -179.8(4) . . . . ? F1 Ge1 C7 C12 123.9(3) . . . . ? C1 Ge1 C7 C12 -121.7(4) . . . . ? C13 Ge1 C7 C12 10.4(4) . . . . ? F1 Ge1 C7 C8 -55.8(4) . . . . ? C1 Ge1 C7 C8 58.6(4) . . . . ? C13 Ge1 C7 C8 -169.3(4) . . . . ? C12 C7 C8 C9 -0.7(7) . . . . ? Ge1 C7 C8 C9 179.1(4) . . . . ? C7 C8 C9 C10 0.4(8) . . . . ? C8 C9 C10 C11 -0.4(8) . . . . ? C9 C10 C11 C12 0.8(8) . . . . ? C8 C7 C12 C11 1.0(7) . . . . ? Ge1 C7 C12 C11 -178.8(3) . . . . ? C10 C11 C12 C7 -1.0(7) . . . . ? F1 Ge1 C13 C18 177.7(3) . . . . ? C7 Ge1 C13 C18 -69.2(4) . . . . ? C1 Ge1 C13 C18 64.1(4) . . . . ? F1 Ge1 C13 C14 -3.5(4) . . . . ? C7 Ge1 C13 C14 109.6(3) . . . . ? C1 Ge1 C13 C14 -117.1(3) . . . . ? C18 C13 C14 C15 0.3(6) . . . . ? Ge1 C13 C14 C15 -178.5(3) . . . . ? C13 C14 C15 C16 0.8(6) . . . . ? C14 C15 C16 C17 -0.9(6) . . . . ? C15 C16 C17 C18 -0.1(7) . . . . ? C14 C13 C18 C17 -1.3(6) . . . . ? Ge1 C13 C18 C17 177.5(3) . . . . ? C16 C17 C18 C13 1.3(7) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 1.357 _refine_diff_density_min -2.434 _refine_diff_density_rms 0.234 #===END data_ppgecl1 #(compound3) _database_code_CSD 179374 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H15 Cl Ge' _chemical_formula_weight 339.34 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P21/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 18.637(4) _cell_length_b 18.317(4) _cell_length_c 18.129(4) _cell_angle_alpha 90.00 _cell_angle_beta 98.38(3) _cell_angle_gamma 90.00 _cell_volume 6122(2) _cell_formula_units_Z 16 _cell_measurement_temperature 100(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description Blocks _exptl_crystal_colour colourless _exptl_crystal_size_max 1.20 _exptl_crystal_size_mid 0.70 _exptl_crystal_size_min 0.70 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.473 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 2752 _exptl_absorpt_coefficient_mu 2.162 _exptl_absorpt_correction_type Scalepack _exptl_absorpt_correction_T_min 0.1812 _exptl_absorpt_correction_T_max 0.3129 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 100(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _diffrn_measurement_method '1.8o phi + omega scans 30s/o' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% 0 _diffrn_reflns_number 36282 _diffrn_reflns_av_R_equivalents 0.0798 _diffrn_reflns_av_sigmaI/netI 0.0699 _diffrn_reflns_limit_h_min -22 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -22 _diffrn_reflns_limit_k_max 21 _diffrn_reflns_limit_l_min -22 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 2.22 _diffrn_reflns_theta_max 26.00 _reflns_number_total 12004 _reflns_number_gt 9048 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius Collect' _computing_cell_refinement DENZO-SMN _computing_data_reduction DENZO-SMN _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'X-Seed (Barbour, 1999)' _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. ; _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^)+(0.0446P)^2^+16.1287P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.00047(8) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 12004 _refine_ls_number_parameters 722 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0833 _refine_ls_R_factor_gt 0.0554 _refine_ls_wR_factor_ref 0.1306 _refine_ls_wR_factor_gt 0.1201 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.155 _refine_ls_shift/su_mean 0.005 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 0.39767(2) 0.72098(3) 0.19041(3) 0.02300(13) Uani 1 1 d . . . Cl1 Cl 0.47197(7) 0.65505(8) 0.13659(8) 0.0388(3) Uani 1 1 d . . . C1 C 0.4083(2) 0.8193(3) 0.1549(2) 0.0228(10) Uani 1 1 d . . . Ge2 Ge 0.20581(2) 0.88605(3) 0.31573(3) 0.02192(13) Uani 1 1 d . . . Cl2 Cl 0.12746(7) 0.94891(8) 0.36716(8) 0.0411(3) Uani 1 1 d . . . C2 C 0.3486(2) 0.8577(3) 0.1185(3) 0.0277(11) Uani 1 1 d . . . H2 H 0.3020 0.8356 0.1115 0.033 Uiso 1 1 calc R . . Ge3 Ge 0.27355(3) 0.39576(3) 0.35289(3) 0.02462(13) Uani 1 1 d . . . Cl3 Cl 0.33438(8) 0.46876(9) 0.43009(8) 0.0481(4) Uani 1 1 d . . . C3 C 0.3570(2) 0.9279(3) 0.0928(3) 0.0281(11) Uani 1 1 d . . . H3 H 0.3163 0.9535 0.0675 0.034 Uiso 1 1 calc R . . Ge4 Ge 0.11527(3) 0.21347(3) 0.14663(3) 0.02624(14) Uani 1 1 d . . . Cl4 Cl 0.04814(8) 0.14973(9) 0.06318(8) 0.0468(4) Uani 1 1 d . . . C4 C 0.4251(3) 0.9608(3) 0.1039(3) 0.0303(11) Uani 1 1 d . . . H4 H 0.4308 1.0089 0.0861 0.036 Uiso 1 1 calc R . . C5 C 0.4844(3) 0.9239(3) 0.1405(3) 0.0308(11) Uani 1 1 d . . . H5 H 0.5307 0.9467 0.1481 0.037 Uiso 1 1 calc R . . C6 C 0.4761(2) 0.8534(3) 0.1661(3) 0.0272(11) Uani 1 1 d . . . H6 H 0.5169 0.8281 0.1915 0.033 Uiso 1 1 calc R . . C7 C 0.3018(2) 0.6834(3) 0.1562(2) 0.0227(10) Uani 1 1 d . . . C8 C 0.2735(3) 0.6861(3) 0.0805(3) 0.0284(11) Uani 1 1 d . . . H8 H 0.3027 0.7041 0.0458 0.034 Uiso 1 1 calc R . . C9 C 0.2035(3) 0.6630(3) 0.0555(3) 0.0332(12) Uani 1 1 d . . . H9 H 0.1849 0.6650 0.0039 0.040 Uiso 1 1 calc R . . C10 C 0.1606(3) 0.6369(3) 0.1058(3) 0.0310(11) Uani 1 1 d . . . H10 H 0.1123 0.6217 0.0886 0.037 Uiso 1 1 calc R . . C11 C 0.1874(3) 0.6327(3) 0.1807(3) 0.0306(11) Uani 1 1 d . . . H11 H 0.1579 0.6136 0.2147 0.037 Uiso 1 1 calc R . . C12 C 0.2577(2) 0.6565(3) 0.2067(3) 0.0244(10) Uani 1 1 d . . . H12 H 0.2757 0.6545 0.2584 0.029 Uiso 1 1 calc R . . C13 C 0.4280(2) 0.7096(3) 0.2966(3) 0.0239(10) Uani 1 1 d . . . C14 C 0.4328(2) 0.6410(3) 0.3300(3) 0.0279(11) Uani 1 1 d . . . H14 H 0.4238 0.5986 0.2999 0.033 Uiso 1 1 calc R . . C15 C 0.4506(3) 0.6337(3) 0.4066(3) 0.0339(12) Uani 1 1 d . . . H15 H 0.4537 0.5866 0.4288 0.041 Uiso 1 1 calc R . . C16 C 0.4639(2) 0.6956(3) 0.4506(3) 0.0335(12) Uani 1 1 d . . . H16 H 0.4757 0.6906 0.5031 0.040 Uiso 1 1 calc R . . C17 C 0.4601(2) 0.7643(3) 0.4190(3) 0.0324(12) Uani 1 1 d . . . H17 H 0.4692 0.8065 0.4495 0.039 Uiso 1 1 calc R . . C18 C 0.4428(2) 0.7713(3) 0.3416(3) 0.0268(11) Uani 1 1 d . . . H18 H 0.4410 0.8184 0.3194 0.032 Uiso 1 1 calc R . . C19 C 0.1983(2) 0.7867(2) 0.3495(2) 0.0202(9) Uani 1 1 d . . . C20 C 0.1325(2) 0.7486(3) 0.3354(3) 0.0280(11) Uani 1 1 d . . . H20 H 0.0902 0.7726 0.3114 0.034 Uiso 1 1 calc R . . C21 C 0.1288(3) 0.6764(3) 0.3563(3) 0.0341(12) Uani 1 1 d . . . H21 H 0.0839 0.6510 0.3462 0.041 Uiso 1 1 calc R . . C22 C 0.1894(3) 0.6405(3) 0.3916(3) 0.0324(12) Uani 1 1 d . . . H22 H 0.1867 0.5904 0.4044 0.039 Uiso 1 1 calc R . . C23 C 0.2549(3) 0.6785(3) 0.4082(3) 0.0309(11) Uani 1 1 d . . . H23 H 0.2963 0.6548 0.4344 0.037 Uiso 1 1 calc R . . C24 C 0.2594(2) 0.7506(3) 0.3867(2) 0.0213(10) Uani 1 1 d . . . H24 H 0.3043 0.7758 0.3971 0.026 Uiso 1 1 calc R . . C25 C 0.2989(2) 0.9293(2) 0.3525(2) 0.0215(9) Uani 1 1 d . . . C26 C 0.3198(3) 0.9375(3) 0.4290(3) 0.0298(11) Uani 1 1 d . . . H26 H 0.2875 0.9237 0.4626 0.036 Uiso 1 1 calc R . . C27 C 0.3874(3) 0.9657(3) 0.4564(3) 0.0343(12) Uani 1 1 d . . . H27 H 0.4017 0.9702 0.5086 0.041 Uiso 1 1 calc R . . C28 C 0.4342(2) 0.9873(3) 0.4077(3) 0.0286(11) Uani 1 1 d . . . H28 H 0.4804 1.0070 0.4266 0.034 Uiso 1 1 calc R . . C29 C 0.4138(2) 0.9801(3) 0.3318(3) 0.0305(11) Uani 1 1 d . . . H29 H 0.4457 0.9954 0.2984 0.037 Uiso 1 1 calc R . . C30 C 0.3460(2) 0.9504(3) 0.3040(3) 0.0249(10) Uani 1 1 d . . . H30 H 0.3323 0.9446 0.2517 0.030 Uiso 1 1 calc R . . C31 C 0.1774(2) 0.8989(3) 0.2098(2) 0.0205(9) Uani 1 1 d . . . C32 C 0.1782(2) 0.9676(3) 0.1786(3) 0.0267(10) Uani 1 1 d . . . H32 H 0.1948 1.0079 0.2094 0.032 Uiso 1 1 calc R . . C33 C 0.1551(3) 0.9789(3) 0.1031(3) 0.0295(11) Uani 1 1 d . . . H33 H 0.1560 1.0264 0.0824 0.035 Uiso 1 1 calc R . . C34 C 0.1308(2) 0.9201(3) 0.0584(3) 0.0291(11) Uani 1 1 d . . . H34 H 0.1139 0.9277 0.0069 0.035 Uiso 1 1 calc R . . C35 C 0.1308(2) 0.8503(3) 0.0880(3) 0.0274(11) Uani 1 1 d . . . H35 H 0.1152 0.8100 0.0568 0.033 Uiso 1 1 calc R . . C36 C 0.1539(2) 0.8396(3) 0.1637(3) 0.0230(10) Uani 1 1 d . . . H36 H 0.1538 0.7919 0.1843 0.028 Uiso 1 1 calc R . . C37 C 0.3181(2) 0.4023(2) 0.2631(3) 0.0211(10) Uani 1 1 d . . . C38 C 0.3278(3) 0.4699(3) 0.2305(3) 0.0283(11) Uani 1 1 d . . . H38 H 0.3116 0.5130 0.2521 0.034 Uiso 1 1 calc R . . C39 C 0.3609(3) 0.4748(3) 0.1671(3) 0.0331(12) Uani 1 1 d . . . H39 H 0.3676 0.5212 0.1457 0.040 Uiso 1 1 calc R . . C40 C 0.3840(3) 0.4128(3) 0.1353(3) 0.0318(12) Uani 1 1 d . . . H40 H 0.4070 0.4164 0.0920 0.038 Uiso 1 1 calc R . . C41 C 0.3740(2) 0.3445(3) 0.1661(3) 0.0261(11) Uani 1 1 d . . . H41 H 0.3896 0.3015 0.1438 0.031 Uiso 1 1 calc R . . C42 C 0.3411(2) 0.3402(3) 0.2295(2) 0.0220(10) Uani 1 1 d . . . H42 H 0.3340 0.2937 0.2506 0.026 Uiso 1 1 calc R . . C43 C 0.2838(2) 0.2989(3) 0.3956(2) 0.0215(10) Uani 1 1 d . . . C44 C 0.3524(2) 0.2690(3) 0.4180(3) 0.0293(11) Uani 1 1 d . . . H44 H 0.3944 0.2974 0.4147 0.035 Uiso 1 1 calc R . . C45 C 0.3597(3) 0.1982(3) 0.4452(3) 0.0380(13) Uani 1 1 d . . . H45 H 0.4065 0.1782 0.4606 0.046 Uiso 1 1 calc R . . C46 C 0.2978(3) 0.1565(3) 0.4498(3) 0.0357(12) Uani 1 1 d . . . H46 H 0.3025 0.1078 0.4678 0.043 Uiso 1 1 calc R . . C47 C 0.2302(3) 0.1859(3) 0.4283(3) 0.0291(11) Uani 1 1 d . . . H47 H 0.1882 0.1575 0.4319 0.035 Uiso 1 1 calc R . . C48 C 0.2228(2) 0.2565(3) 0.4015(2) 0.0246(10) Uani 1 1 d . . . H48 H 0.1757 0.2763 0.3869 0.030 Uiso 1 1 calc R . . C49 C 0.1751(2) 0.4312(2) 0.3415(3) 0.0236(10) Uani 1 1 d . . . C50 C 0.1373(2) 0.4333(3) 0.4028(3) 0.0252(10) Uani 1 1 d . . . H50 H 0.1608 0.4181 0.4503 0.030 Uiso 1 1 calc R . . C51 C 0.0663(3) 0.4570(3) 0.3948(3) 0.0302(11) Uani 1 1 d . . . H51 H 0.0413 0.4582 0.4368 0.036 Uiso 1 1 calc R . . C52 C 0.0313(3) 0.4792(3) 0.3257(3) 0.0326(12) Uani 1 1 d . . . H52 H -0.0177 0.4952 0.3201 0.039 Uiso 1 1 calc R . . C53 C 0.0686(3) 0.4779(3) 0.2646(3) 0.0352(12) Uani 1 1 d . . . H53 H 0.0451 0.4935 0.2172 0.042 Uiso 1 1 calc R . . C54 C 0.1393(3) 0.4540(3) 0.2723(3) 0.0288(11) Uani 1 1 d . . . H54 H 0.1641 0.4531 0.2301 0.035 Uiso 1 1 calc R . . C55 C 0.0732(2) 0.2073(3) 0.2382(3) 0.0256(10) Uani 1 1 d . . . C56 C 0.0697(3) 0.1404(3) 0.2757(3) 0.0307(11) Uani 1 1 d . . . H56 H 0.0848 0.0966 0.2544 0.037 Uiso 1 1 calc R . . C57 C 0.0440(3) 0.1385(3) 0.3437(3) 0.0369(13) Uani 1 1 d . . . H57 H 0.0416 0.0933 0.3690 0.044 Uiso 1 1 calc R . . C58 C 0.0220(3) 0.2015(3) 0.3749(3) 0.0341(12) Uani 1 1 d . . . H58 H 0.0049 0.1998 0.4218 0.041 Uiso 1 1 calc R . . C59 C 0.0246(2) 0.2673(3) 0.3385(3) 0.0301(11) Uani 1 1 d . . . H59 H 0.0085 0.3105 0.3599 0.036 Uiso 1 1 calc R . . C60 C 0.0506(2) 0.2706(3) 0.2704(3) 0.0264(11) Uani 1 1 d . . . H60 H 0.0530 0.3162 0.2459 0.032 Uiso 1 1 calc R . . C61 C 0.1095(2) 0.3107(3) 0.1057(3) 0.0279(11) Uani 1 1 d . . . C62 C 0.0433(3) 0.3461(4) 0.0842(3) 0.0437(15) Uani 1 1 d . . . H62 H -0.0006 0.3215 0.0892 0.052 Uiso 1 1 calc R . . C63 C 0.0409(3) 0.4162(4) 0.0559(3) 0.0485(16) Uani 1 1 d . . . H63 H -0.0047 0.4391 0.0413 0.058 Uiso 1 1 calc R . . C64 C 0.1037(3) 0.4532(3) 0.0485(3) 0.0429(14) Uani 1 1 d . . . H64 H 0.1015 0.5012 0.0285 0.051 Uiso 1 1 calc R . . C65 C 0.1696(3) 0.4205(3) 0.0701(3) 0.0369(12) Uani 1 1 d . . . H65 H 0.2132 0.4460 0.0657 0.044 Uiso 1 1 calc R . . C66 C 0.1724(3) 0.3498(3) 0.0987(3) 0.0295(11) Uani 1 1 d . . . H66 H 0.2183 0.3276 0.1137 0.035 Uiso 1 1 calc R . . C67 C 0.2132(2) 0.1754(2) 0.1586(3) 0.0220(10) Uani 1 1 d . . . C68 C 0.2525(3) 0.1710(3) 0.0985(3) 0.0273(11) Uani 1 1 d . . . H68 H 0.2294 0.1834 0.0498 0.033 Uiso 1 1 calc R . . C69 C 0.3242(3) 0.1490(3) 0.1088(3) 0.0323(12) Uani 1 1 d . . . H69 H 0.3498 0.1456 0.0673 0.039 Uiso 1 1 calc R . . C70 C 0.3583(3) 0.1321(3) 0.1788(3) 0.0305(11) Uani 1 1 d . . . H70 H 0.4078 0.1176 0.1857 0.037 Uiso 1 1 calc R . . C71 C 0.3209(3) 0.1362(3) 0.2398(3) 0.0283(11) Uani 1 1 d . . . H71 H 0.3447 0.1240 0.2881 0.034 Uiso 1 1 calc R . . C72 C 0.2492(2) 0.1579(2) 0.2302(3) 0.0229(10) Uani 1 1 d . . . H72 H 0.2240 0.1609 0.2720 0.027 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.0229(2) 0.0278(3) 0.0181(3) 0.0003(2) 0.00248(18) -0.0017(2) Cl1 0.0377(7) 0.0413(8) 0.0396(8) -0.0044(6) 0.0129(6) 0.0054(6) C1 0.023(2) 0.030(3) 0.016(2) -0.001(2) 0.0032(17) -0.0033(19) Ge2 0.0223(2) 0.0236(3) 0.0187(3) 0.0000(2) -0.00100(18) -0.00213(19) Cl2 0.0394(7) 0.0491(9) 0.0359(7) -0.0031(6) 0.0099(6) 0.0108(6) C2 0.023(2) 0.038(3) 0.023(3) 0.003(2) 0.0062(19) -0.002(2) Ge3 0.0242(3) 0.0267(3) 0.0243(3) 0.0025(2) 0.00794(19) 0.0017(2) Cl3 0.0485(8) 0.0552(10) 0.0403(8) -0.0121(7) 0.0057(6) -0.0095(7) C3 0.026(2) 0.035(3) 0.024(3) 0.006(2) 0.0051(19) 0.006(2) Ge4 0.0217(2) 0.0375(3) 0.0189(3) -0.0002(2) 0.00093(18) 0.0017(2) Cl4 0.0422(8) 0.0544(9) 0.0417(8) -0.0129(7) -0.0005(6) -0.0025(6) C4 0.036(3) 0.030(3) 0.027(3) 0.002(2) 0.010(2) -0.004(2) C5 0.030(3) 0.037(3) 0.026(3) -0.004(2) 0.004(2) -0.011(2) C6 0.022(2) 0.038(3) 0.021(3) -0.003(2) 0.0006(18) -0.003(2) C7 0.026(2) 0.023(2) 0.020(2) -0.0040(19) 0.0039(18) 0.0004(19) C8 0.030(2) 0.038(3) 0.018(2) -0.001(2) 0.0050(19) -0.003(2) C9 0.030(3) 0.045(3) 0.023(3) -0.010(2) 0.001(2) -0.004(2) C10 0.024(2) 0.032(3) 0.036(3) -0.011(2) 0.002(2) -0.001(2) C11 0.029(3) 0.029(3) 0.036(3) -0.006(2) 0.014(2) -0.005(2) C12 0.030(2) 0.025(3) 0.019(2) -0.002(2) 0.0044(18) 0.0022(19) C13 0.018(2) 0.031(3) 0.022(2) 0.001(2) 0.0035(17) -0.0001(19) C14 0.027(2) 0.025(3) 0.030(3) 0.003(2) -0.001(2) 0.000(2) C15 0.028(3) 0.039(3) 0.035(3) 0.017(3) 0.005(2) 0.000(2) C16 0.022(2) 0.057(4) 0.020(3) 0.009(3) -0.0017(18) 0.001(2) C17 0.025(2) 0.045(3) 0.025(3) -0.008(2) -0.0030(19) -0.002(2) C18 0.026(2) 0.027(3) 0.026(3) -0.001(2) 0.0028(19) 0.000(2) C19 0.025(2) 0.024(2) 0.012(2) 0.0002(18) 0.0044(17) -0.0036(18) C20 0.021(2) 0.039(3) 0.024(3) -0.004(2) 0.0030(18) -0.003(2) C21 0.037(3) 0.032(3) 0.036(3) -0.004(2) 0.017(2) -0.015(2) C22 0.044(3) 0.023(3) 0.033(3) 0.005(2) 0.019(2) -0.001(2) C23 0.039(3) 0.033(3) 0.023(3) 0.005(2) 0.011(2) 0.007(2) C24 0.022(2) 0.028(3) 0.014(2) -0.0013(19) 0.0032(17) -0.0011(18) C25 0.023(2) 0.019(2) 0.021(2) -0.0013(19) -0.0009(17) 0.0020(18) C26 0.032(3) 0.036(3) 0.021(3) 0.002(2) 0.0010(19) -0.006(2) C27 0.037(3) 0.040(3) 0.023(3) -0.006(2) -0.004(2) -0.003(2) C28 0.025(2) 0.028(3) 0.031(3) -0.003(2) -0.003(2) -0.003(2) C29 0.023(2) 0.035(3) 0.033(3) 0.002(2) 0.004(2) -0.001(2) C30 0.028(2) 0.024(3) 0.021(2) 0.000(2) -0.0011(18) -0.0003(19) C31 0.016(2) 0.027(3) 0.017(2) 0.0014(19) 0.0009(16) -0.0002(18) C32 0.027(2) 0.024(3) 0.029(3) -0.004(2) 0.0034(19) -0.0007(19) C33 0.037(3) 0.026(3) 0.028(3) 0.008(2) 0.011(2) 0.007(2) C34 0.028(2) 0.043(3) 0.016(2) 0.002(2) 0.0026(18) 0.004(2) C35 0.027(2) 0.031(3) 0.023(3) -0.007(2) 0.0017(19) -0.001(2) C36 0.023(2) 0.023(3) 0.024(3) 0.003(2) 0.0054(18) 0.0000(18) C37 0.014(2) 0.024(2) 0.025(2) 0.000(2) 0.0020(17) -0.0004(17) C38 0.033(3) 0.021(3) 0.032(3) -0.001(2) 0.006(2) 0.000(2) C39 0.047(3) 0.027(3) 0.027(3) 0.005(2) 0.012(2) -0.007(2) C40 0.029(3) 0.042(3) 0.025(3) -0.002(2) 0.009(2) -0.007(2) C41 0.022(2) 0.031(3) 0.025(3) -0.002(2) 0.0040(19) -0.0007(19) C42 0.019(2) 0.023(2) 0.023(2) 0.002(2) -0.0008(17) -0.0015(18) C43 0.022(2) 0.030(3) 0.014(2) 0.0020(19) 0.0045(17) 0.0014(19) C44 0.024(2) 0.038(3) 0.026(3) 0.006(2) 0.0039(19) 0.001(2) C45 0.028(3) 0.055(4) 0.030(3) 0.013(3) 0.003(2) 0.012(2) C46 0.049(3) 0.031(3) 0.026(3) 0.009(2) 0.003(2) 0.002(2) C47 0.033(3) 0.034(3) 0.020(3) 0.003(2) 0.0013(19) -0.003(2) C48 0.024(2) 0.035(3) 0.014(2) 0.002(2) 0.0000(17) 0.000(2) C49 0.031(2) 0.017(2) 0.024(3) -0.001(2) 0.0080(19) -0.0002(19) C50 0.029(2) 0.024(3) 0.023(3) -0.002(2) 0.0052(19) 0.0020(19) C51 0.030(3) 0.028(3) 0.034(3) -0.007(2) 0.012(2) 0.002(2) C52 0.025(2) 0.029(3) 0.044(3) -0.003(2) 0.003(2) 0.004(2) C53 0.037(3) 0.038(3) 0.030(3) 0.001(2) 0.001(2) 0.006(2) C54 0.037(3) 0.029(3) 0.021(3) 0.002(2) 0.007(2) 0.000(2) C55 0.016(2) 0.037(3) 0.022(2) -0.006(2) 0.0000(17) -0.0042(19) C56 0.030(3) 0.028(3) 0.035(3) -0.006(2) 0.009(2) -0.006(2) C57 0.045(3) 0.036(3) 0.033(3) 0.003(2) 0.016(2) -0.010(2) C58 0.030(3) 0.043(3) 0.033(3) -0.011(3) 0.017(2) -0.012(2) C59 0.023(2) 0.035(3) 0.032(3) -0.010(2) 0.004(2) -0.006(2) C60 0.017(2) 0.034(3) 0.028(3) 0.000(2) -0.0002(18) -0.0027(19) C61 0.028(2) 0.039(3) 0.017(2) 0.004(2) 0.0037(18) 0.013(2) C62 0.030(3) 0.068(4) 0.032(3) 0.011(3) 0.003(2) 0.009(3) C63 0.050(4) 0.063(4) 0.031(3) 0.017(3) 0.002(3) 0.031(3) C64 0.061(4) 0.038(3) 0.030(3) 0.005(3) 0.009(3) 0.011(3) C65 0.046(3) 0.036(3) 0.028(3) 0.000(2) 0.004(2) 0.003(2) C66 0.033(3) 0.035(3) 0.019(3) -0.003(2) 0.000(2) 0.008(2) C67 0.025(2) 0.019(2) 0.022(2) -0.0008(19) 0.0024(18) -0.0018(18) C68 0.036(3) 0.028(3) 0.019(2) -0.003(2) 0.0057(19) 0.002(2) C69 0.038(3) 0.031(3) 0.032(3) -0.004(2) 0.018(2) 0.003(2) C70 0.026(2) 0.028(3) 0.039(3) -0.004(2) 0.007(2) 0.006(2) C71 0.035(3) 0.024(3) 0.024(3) 0.000(2) -0.001(2) 0.004(2) C72 0.032(2) 0.019(2) 0.018(2) -0.0041(19) 0.0048(18) -0.0013(19) _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 C7 1.931(4) . ? Ge1 C1 1.933(5) . ? Ge1 C13 1.937(5) . ? Ge1 Cl1 2.1730(14) . ? C1 C2 1.396(6) . ? C1 C6 1.399(6) . ? Ge2 C31 1.931(4) . ? Ge2 C19 1.932(5) . ? Ge2 C25 1.935(4) . ? Ge2 Cl2 2.1734(14) . ? C2 C3 1.383(7) . ? Ge3 C49 1.929(5) . ? Ge3 C43 1.934(5) . ? Ge3 C37 1.937(4) . ? Ge3 Cl3 2.1377(16) . ? C3 C4 1.394(7) . ? Ge4 C61 1.927(5) . ? Ge4 C67 1.937(4) . ? Ge4 C55 1.940(5) . ? Ge4 Cl4 2.1599(16) . ? C4 C5 1.379(7) . ? C5 C6 1.390(7) . ? C7 C8 1.397(6) . ? C7 C12 1.406(6) . ? C8 C9 1.384(7) . ? C9 C10 1.381(7) . ? C10 C11 1.379(7) . ? C11 C12 1.396(7) . ? C13 C14 1.391(7) . ? C13 C18 1.397(7) . ? C14 C15 1.387(7) . ? C15 C16 1.387(8) . ? C16 C17 1.381(8) . ? C17 C18 1.400(7) . ? C19 C24 1.402(6) . ? C19 C20 1.402(6) . ? C20 C21 1.380(7) . ? C21 C22 1.381(7) . ? C22 C23 1.399(7) . ? C23 C24 1.382(7) . ? C25 C30 1.385(6) . ? C25 C26 1.394(6) . ? C26 C27 1.384(7) . ? C27 C28 1.387(7) . ? C28 C29 1.378(7) . ? C29 C30 1.401(6) . ? C31 C32 1.381(7) . ? C31 C36 1.400(6) . ? C32 C33 1.389(7) . ? C33 C34 1.384(7) . ? C34 C35 1.387(7) . ? C35 C36 1.391(7) . ? C37 C42 1.387(6) . ? C37 C38 1.393(7) . ? C38 C39 1.384(7) . ? C39 C40 1.372(7) . ? C40 C41 1.392(7) . ? C41 C42 1.383(6) . ? C43 C48 1.394(6) . ? C43 C44 1.396(6) . ? C44 C45 1.387(7) . ? C45 C46 1.395(7) . ? C46 C47 1.375(7) . ? C47 C48 1.381(7) . ? C49 C54 1.396(7) . ? C49 C50 1.399(6) . ? C50 C51 1.380(6) . ? C51 C52 1.386(7) . ? C52 C53 1.391(7) . ? C53 C54 1.376(7) . ? C55 C60 1.391(7) . ? C55 C56 1.408(7) . ? C56 C57 1.387(7) . ? C57 C58 1.375(7) . ? C58 C59 1.377(7) . ? C59 C60 1.391(7) . ? C61 C66 1.395(7) . ? C61 C62 1.397(7) . ? C62 C63 1.381(9) . ? C63 C64 1.377(8) . ? C64 C65 1.371(8) . ? C65 C66 1.394(7) . ? C67 C68 1.400(6) . ? C67 C72 1.409(6) . ? C68 C69 1.382(7) . ? C69 C70 1.370(7) . ? C70 C71 1.393(7) . ? C71 C72 1.380(6) . ? 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 C7 Ge1 C1 111.07(19) . . ? C7 Ge1 C13 113.78(19) . . ? C1 Ge1 C13 113.74(19) . . ? C7 Ge1 Cl1 106.17(14) . . ? C1 Ge1 Cl1 105.40(14) . . ? C13 Ge1 Cl1 105.88(14) . . ? C2 C1 C6 119.0(4) . . ? C2 C1 Ge1 120.9(3) . . ? C6 C1 Ge1 120.1(4) . . ? C31 Ge2 C19 114.06(19) . . ? C31 Ge2 C25 113.24(19) . . ? C19 Ge2 C25 112.33(19) . . ? C31 Ge2 Cl2 104.95(13) . . ? C19 Ge2 Cl2 106.20(13) . . ? C25 Ge2 Cl2 105.07(14) . . ? C3 C2 C1 120.4(4) . . ? C49 Ge3 C43 112.83(18) . . ? C49 Ge3 C37 114.04(19) . . ? C43 Ge3 C37 111.37(18) . . ? C49 Ge3 Cl3 105.36(15) . . ? C43 Ge3 Cl3 107.44(14) . . ? C37 Ge3 Cl3 105.08(14) . . ? C2 C3 C4 119.9(4) . . ? C61 Ge4 C67 111.98(19) . . ? C61 Ge4 C55 112.1(2) . . ? C67 Ge4 C55 112.04(19) . . ? C61 Ge4 Cl4 103.65(15) . . ? C67 Ge4 Cl4 108.93(14) . . ? C55 Ge4 Cl4 107.65(14) . . ? C5 C4 C3 120.5(5) . . ? C4 C5 C6 119.7(4) . . ? C5 C6 C1 120.5(4) . . ? C8 C7 C12 118.6(4) . . ? C8 C7 Ge1 120.1(3) . . ? C12 C7 Ge1 121.2(3) . . ? C9 C8 C7 120.9(4) . . ? C10 C9 C8 119.9(5) . . ? C11 C10 C9 120.5(4) . . ? C10 C11 C12 120.1(5) . . ? C11 C12 C7 119.9(4) . . ? C14 C13 C18 118.8(4) . . ? C14 C13 Ge1 121.3(4) . . ? C18 C13 Ge1 119.8(4) . . ? C15 C14 C13 120.9(5) . . ? C14 C15 C16 119.6(5) . . ? C17 C16 C15 120.8(5) . . ? C16 C17 C18 119.3(5) . . ? C13 C18 C17 120.5(5) . . ? C24 C19 C20 118.7(4) . . ? C24 C19 Ge2 120.4(3) . . ? C20 C19 Ge2 120.9(3) . . ? C21 C20 C19 120.3(5) . . ? C20 C21 C22 120.8(5) . . ? C21 C22 C23 119.5(5) . . ? C24 C23 C22 120.0(5) . . ? C23 C24 C19 120.5(4) . . ? C30 C25 C26 119.4(4) . . ? C30 C25 Ge2 121.0(3) . . ? C26 C25 Ge2 119.6(3) . . ? C27 C26 C25 120.3(5) . . ? C26 C27 C28 120.2(5) . . ? C29 C28 C27 120.0(4) . . ? C28 C29 C30 120.0(4) . . ? C25 C30 C29 120.1(4) . . ? C32 C31 C36 119.0(4) . . ? C32 C31 Ge2 120.0(3) . . ? C36 C31 Ge2 121.0(3) . . ? C31 C32 C33 121.2(5) . . ? C34 C33 C32 119.4(5) . . ? C33 C34 C35 120.5(4) . . ? C34 C35 C36 119.6(5) . . ? C35 C36 C31 120.3(4) . . ? C42 C37 C38 118.4(4) . . ? C42 C37 Ge3 121.0(3) . . ? C38 C37 Ge3 120.6(3) . . ? C39 C38 C37 120.7(5) . . ? C40 C39 C38 120.0(5) . . ? C39 C40 C41 120.4(4) . . ? C42 C41 C40 119.2(5) . . ? C41 C42 C37 121.3(4) . . ? C48 C43 C44 118.8(4) . . ? C48 C43 Ge3 120.6(3) . . ? C44 C43 Ge3 120.6(3) . . ? C45 C44 C43 120.6(4) . . ? C44 C45 C46 119.6(5) . . ? C47 C46 C45 120.0(5) . . ? C46 C47 C48 120.5(5) . . ? C47 C48 C43 120.5(4) . . ? C54 C49 C50 118.4(4) . . ? C54 C49 Ge3 121.2(3) . . ? C50 C49 Ge3 120.4(4) . . ? C51 C50 C49 120.7(5) . . ? C50 C51 C52 120.3(5) . . ? C51 C52 C53 119.3(5) . . ? C54 C53 C52 120.5(5) . . ? C53 C54 C49 120.7(5) . . ? C60 C55 C56 119.0(4) . . ? C60 C55 Ge4 119.7(4) . . ? C56 C55 Ge4 121.1(4) . . ? C57 C56 C55 119.8(5) . . ? C58 C57 C56 120.5(5) . . ? C57 C58 C59 120.3(5) . . ? C58 C59 C60 120.3(5) . . ? C55 C60 C59 120.1(5) . . ? C66 C61 C62 117.2(5) . . ? C66 C61 Ge4 120.6(3) . . ? C62 C61 Ge4 122.2(4) . . ? C63 C62 C61 121.0(5) . . ? C64 C63 C62 120.8(5) . . ? C65 C64 C63 119.7(5) . . ? C64 C65 C66 119.8(5) . . ? C65 C66 C61 121.6(5) . . ? C68 C67 C72 118.2(4) . . ? C68 C67 Ge4 121.6(3) . . ? C72 C67 Ge4 120.0(3) . . ? C69 C68 C67 121.1(5) . . ? C70 C69 C68 120.0(4) . . ? C69 C70 C71 120.3(4) . . ? C72 C71 C70 120.2(4) . . ? C71 C72 C67 120.2(4) . . ? loop_ _geom_torsion_atom_site_label_1 _geom_torsion_atom_site_label_2 _geom_torsion_atom_site_label_3 _geom_torsion_atom_site_label_4 _geom_torsion _geom_torsion_site_symmetry_1 _geom_torsion_site_symmetry_2 _geom_torsion_site_symmetry_3 _geom_torsion_site_symmetry_4 _geom_torsion_publ_flag C7 Ge1 C1 C2 8.2(4) . . . . ? C13 Ge1 C1 C2 -121.7(4) . . . . ? Cl1 Ge1 C1 C2 122.7(4) . . . . ? C7 Ge1 C1 C6 -172.6(3) . . . . ? C13 Ge1 C1 C6 57.5(4) . . . . ? Cl1 Ge1 C1 C6 -58.0(4) . . . . ? C6 C1 C2 C3 1.3(7) . . . . ? Ge1 C1 C2 C3 -179.4(4) . . . . ? C1 C2 C3 C4 -0.8(7) . . . . ? C2 C3 C4 C5 0.0(7) . . . . ? C3 C4 C5 C6 0.3(7) . . . . ? C4 C5 C6 C1 0.3(7) . . . . ? C2 C1 C6 C5 -1.1(7) . . . . ? Ge1 C1 C6 C5 179.7(4) . . . . ? C1 Ge1 C7 C8 51.9(4) . . . . ? C13 Ge1 C7 C8 -178.3(4) . . . . ? Cl1 Ge1 C7 C8 -62.2(4) . . . . ? C1 Ge1 C7 C12 -124.8(4) . . . . ? C13 Ge1 C7 C12 5.1(5) . . . . ? Cl1 Ge1 C7 C12 121.1(4) . . . . ? C12 C7 C8 C9 0.1(7) . . . . ? Ge1 C7 C8 C9 -176.6(4) . . . . ? C7 C8 C9 C10 0.1(8) . . . . ? C8 C9 C10 C11 -1.0(8) . . . . ? C9 C10 C11 C12 1.5(8) . . . . ? C10 C11 C12 C7 -1.2(7) . . . . ? C8 C7 C12 C11 0.4(7) . . . . ? Ge1 C7 C12 C11 177.1(4) . . . . ? C7 Ge1 C13 C14 59.7(4) . . . . ? C1 Ge1 C13 C14 -171.7(3) . . . . ? Cl1 Ge1 C13 C14 -56.5(4) . . . . ? C7 Ge1 C13 C18 -117.7(4) . . . . ? C1 Ge1 C13 C18 10.8(4) . . . . ? Cl1 Ge1 C13 C18 126.1(3) . . . . ? C18 C13 C14 C15 1.2(7) . . . . ? Ge1 C13 C14 C15 -176.3(3) . . . . ? C13 C14 C15 C16 -0.1(7) . . . . ? C14 C15 C16 C17 -0.5(7) . . . . ? C15 C16 C17 C18 -0.1(7) . . . . ? C14 C13 C18 C17 -1.7(6) . . . . ? Ge1 C13 C18 C17 175.8(3) . . . . ? C16 C17 C18 C13 1.2(7) . . . . ? C31 Ge2 C19 C24 121.9(3) . . . . ? C25 Ge2 C19 C24 -8.7(4) . . . . ? Cl2 Ge2 C19 C24 -123.1(3) . . . . ? C31 Ge2 C19 C20 -56.2(4) . . . . ? C25 Ge2 C19 C20 173.2(3) . . . . ? Cl2 Ge2 C19 C20 58.9(4) . . . . ? C24 C19 C20 C21 -1.6(7) . . . . ? Ge2 C19 C20 C21 176.5(4) . . . . ? C19 C20 C21 C22 0.3(7) . . . . ? C20 C21 C22 C23 1.8(7) . . . . ? C21 C22 C23 C24 -2.7(7) . . . . ? C22 C23 C24 C19 1.4(7) . . . . ? C20 C19 C24 C23 0.7(6) . . . . ? Ge2 C19 C24 C23 -177.4(3) . . . . ? C31 Ge2 C25 C30 -14.8(4) . . . . ? C19 Ge2 C25 C30 116.2(4) . . . . ? Cl2 Ge2 C25 C30 -128.8(4) . . . . ? C31 Ge2 C25 C26 167.1(4) . . . . ? C19 Ge2 C25 C26 -61.9(4) . . . . ? Cl2 Ge2 C25 C26 53.1(4) . . . . ? C30 C25 C26 C27 -0.7(7) . . . . ? Ge2 C25 C26 C27 177.4(4) . . . . ? C25 C26 C27 C28 1.3(8) . . . . ? C26 C27 C28 C29 -0.6(8) . . . . ? C27 C28 C29 C30 -0.6(8) . . . . ? C26 C25 C30 C29 -0.5(7) . . . . ? Ge2 C25 C30 C29 -178.6(4) . . . . ? C28 C29 C30 C25 1.2(7) . . . . ? C19 Ge2 C31 C32 178.2(3) . . . . ? C25 Ge2 C31 C32 -51.7(4) . . . . ? Cl2 Ge2 C31 C32 62.3(4) . . . . ? C19 Ge2 C31 C36 -0.2(4) . . . . ? C25 Ge2 C31 C36 129.9(3) . . . . ? Cl2 Ge2 C31 C36 -116.0(3) . . . . ? C36 C31 C32 C33 1.1(7) . . . . ? Ge2 C31 C32 C33 -177.3(3) . . . . ? C31 C32 C33 C34 0.1(7) . . . . ? C32 C33 C34 C35 -1.4(7) . . . . ? C33 C34 C35 C36 1.5(7) . . . . ? C34 C35 C36 C31 -0.3(7) . . . . ? C32 C31 C36 C35 -1.0(6) . . . . ? Ge2 C31 C36 C35 177.4(3) . . . . ? C49 Ge3 C37 C42 -118.1(4) . . . . ? C43 Ge3 C37 C42 11.0(4) . . . . ? Cl3 Ge3 C37 C42 127.0(3) . . . . ? C49 Ge3 C37 C38 61.8(4) . . . . ? C43 Ge3 C37 C38 -169.1(4) . . . . ? Cl3 Ge3 C37 C38 -53.0(4) . . . . ? C42 C37 C38 C39 -1.3(7) . . . . ? Ge3 C37 C38 C39 178.8(4) . . . . ? C37 C38 C39 C40 0.5(8) . . . . ? C38 C39 C40 C41 0.4(8) . . . . ? C39 C40 C41 C42 -0.5(7) . . . . ? C40 C41 C42 C37 -0.2(7) . . . . ? C38 C37 C42 C41 1.1(7) . . . . ? Ge3 C37 C42 C41 -178.9(3) . . . . ? C49 Ge3 C43 C48 12.4(4) . . . . ? C37 Ge3 C43 C48 -117.3(4) . . . . ? Cl3 Ge3 C43 C48 128.1(3) . . . . ? C49 Ge3 C43 C44 -170.4(4) . . . . ? C37 Ge3 C43 C44 59.8(4) . . . . ? Cl3 Ge3 C43 C44 -54.8(4) . . . . ? C48 C43 C44 C45 0.4(7) . . . . ? Ge3 C43 C44 C45 -176.7(4) . . . . ? C43 C44 C45 C46 0.2(8) . . . . ? C44 C45 C46 C47 -0.7(8) . . . . ? C45 C46 C47 C48 0.5(8) . . . . ? C46 C47 C48 C43 0.2(7) . . . . ? C44 C43 C48 C47 -0.6(7) . . . . ? Ge3 C43 C48 C47 176.5(3) . . . . ? C43 Ge3 C49 C54 -123.9(4) . . . . ? C37 Ge3 C49 C54 4.5(5) . . . . ? Cl3 Ge3 C49 C54 119.2(4) . . . . ? C43 Ge3 C49 C50 54.9(4) . . . . ? C37 Ge3 C49 C50 -176.8(4) . . . . ? Cl3 Ge3 C49 C50 -62.1(4) . . . . ? C54 C49 C50 C51 0.2(7) . . . . ? Ge3 C49 C50 C51 -178.6(4) . . . . ? C49 C50 C51 C52 0.1(7) . . . . ? C50 C51 C52 C53 -0.5(8) . . . . ? C51 C52 C53 C54 0.7(8) . . . . ? C52 C53 C54 C49 -0.4(8) . . . . ? C50 C49 C54 C53 -0.1(7) . . . . ? Ge3 C49 C54 C53 178.7(4) . . . . ? C61 Ge4 C55 C60 -6.7(4) . . . . ? C67 Ge4 C55 C60 120.2(4) . . . . ? Cl4 Ge4 C55 C60 -120.0(3) . . . . ? C61 Ge4 C55 C56 177.7(4) . . . . ? C67 Ge4 C55 C56 -55.4(4) . . . . ? Cl4 Ge4 C55 C56 64.4(4) . . . . ? C60 C55 C56 C57 -0.1(7) . . . . ? Ge4 C55 C56 C57 175.5(4) . . . . ? C55 C56 C57 C58 0.0(8) . . . . ? C56 C57 C58 C59 0.6(8) . . . . ? C57 C58 C59 C60 -1.1(7) . . . . ? C56 C55 C60 C59 -0.3(7) . . . . ? Ge4 C55 C60 C59 -176.0(3) . . . . ? C58 C59 C60 C55 0.9(7) . . . . ? C67 Ge4 C61 C66 -9.6(5) . . . . ? C55 Ge4 C61 C66 117.3(4) . . . . ? Cl4 Ge4 C61 C66 -126.9(4) . . . . ? C67 Ge4 C61 C62 172.5(4) . . . . ? C55 Ge4 C61 C62 -60.5(5) . . . . ? Cl4 Ge4 C61 C62 55.3(4) . . . . ? C66 C61 C62 C63 1.3(8) . . . . ? Ge4 C61 C62 C63 179.2(4) . . . . ? C61 C62 C63 C64 -0.4(9) . . . . ? C62 C63 C64 C65 -0.6(9) . . . . ? C63 C64 C65 C66 0.7(8) . . . . ? C64 C65 C66 C61 0.2(8) . . . . ? C62 C61 C66 C65 -1.2(7) . . . . ? Ge4 C61 C66 C65 -179.2(4) . . . . ? C61 Ge4 C67 C68 -56.4(4) . . . . ? C55 Ge4 C67 C68 176.6(4) . . . . ? Cl4 Ge4 C67 C68 57.6(4) . . . . ? C61 Ge4 C67 C72 117.5(4) . . . . ? C55 Ge4 C67 C72 -9.4(4) . . . . ? Cl4 Ge4 C67 C72 -128.4(3) . . . . ? C72 C67 C68 C69 1.0(7) . . . . ? Ge4 C67 C68 C69 175.0(4) . . . . ? C67 C68 C69 C70 -1.0(8) . . . . ? C68 C69 C70 C71 0.8(8) . . . . ? C69 C70 C71 C72 -0.6(8) . . . . ? C70 C71 C72 C67 0.5(7) . . . . ? C68 C67 C72 C71 -0.7(7) . . . . ? Ge4 C67 C72 C71 -174.9(4) . . . . ? loop_ _geom_hbond_atom_site_label_D _geom_hbond_atom_site_label_H _geom_hbond_atom_site_label_A _geom_hbond_distance_DH _geom_hbond_distance_HA _geom_hbond_distance_DA _geom_hbond_angle_DHA _geom_hbond_site_symmetry_A C39 H39 Cl1 0.95 3.15 3.978(5) 146.8 . C15 H15 Cl3 0.95 3.10 3.777(5) 129.5 . C28 H28 Cl1 0.95 3.12 3.681(5) 119.3 2_655 C45 H45 Cl1 0.95 3.09 3.744(5) 127.1 2_645 C57 H57 Cl2 0.95 3.09 3.803(6) 132.8 1_545 C64 H64 Cl2 0.95 3.17 3.826(6) 128.0 4_575 C63 H63 Cl2 0.95 3.02 3.664(6) 126.3 2_545 C4 H4 Cl3 0.95 3.15 3.591(5) 110.4 4_575 C3 H3 Cl3 0.95 2.93 3.478(5) 117.8 4_575 C5 H5 Cl3 0.95 3.09 3.870(5) 140.7 2_655 C51 H51 Cl4 0.95 3.01 3.683(5) 128.6 4_566 C21 H21 Cl4 0.95 3.15 3.827(5) 129.5 2 C33 H33 Cl4 0.95 3.01 3.725(5) 133.1 1_565 C69 H69 Cl3 0.95 3.23 3.920(5) 130.8 4_565 _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.954 _refine_diff_density_min -1.052 _refine_diff_density_rms 0.114