# Supplementary Material (ESI) for New Journal of Chemistry # This journal is © The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2010 data_global _journal_name_full 'New J.Chem.' _journal_coden_cambridge 0440 _publ_contact_author ; Prof. Dr. Werner Uhl Westf\"alische Wilhelms Universit\"at M\"unster Institut f\"ur Anorganische und Analytische Chemie Corrensstra\&se 30 D-48149 M\"unster Bundesrepublik Deutschland ; _publ_contact_author_phone '049 251 8336610' _publ_contact_author_fax '049 251 8336660' _publ_contact_author_email Uhlw@uni-muenster.de _publ_requested_coeditor_name ? _publ_contact_letter ; Please consider this CIF submission for publication as a "New Crystal Structure". ; #============================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; Facile Synthesis of Aluminium Briged [3,3,3]-Cyclophanes by Hydroalumination ; loop_ _publ_author_name _publ_author_address 'Werner Uhl' ; Westf\"alische Wilhelms Universit\"at M\"unster Institut f\"ur Anorganische und Analytische Chemie Corrensstra\&se 30 D-48149 M\"unster Bundesrepublik Deutschland ; J.Kosters ; Westf\"alische Wilhelms Universit\"at M\"unster Institut f\"ur Anorganische und Analytische Chemie Corrensstra\&se 30 D-48149 M\"unster Bundesrepublik Deutschland ; 'Martina Rohling' ; Westf\"alische Wilhelms Universit\"at M\"unster Institut f\"ur Anorganische und Analytische Chemie Corrensstra\&se 30 D-48149 M\"unster Bundesrepublik Deutschland ; _publ_section_abstract ; Treatment of the digallium compound R2Ga-GaR2 1 [R = CH(SiMe3)2] with hydrogen flouride or water in the presence of 2-aminonicotinic acid afforded the corresponding fluoride or hydroxide, R(X)Ga-Ga(X)R (X = F, OH), by substituent exchange and retainment of the Ga-Ga bonds. Both compounds form trimeric formula units in which three Ga-Ga bonds in a parallel orientation are bridged by six fluoro or hydroxo ligands. ; _publ_contact_author_name 'Prof. Dr. Werner Uhl' #============================================================================== data_sad_1 _database_code_depnum_ccdc_archive 'CCDC 762758' #TrackingRef '- cifcompound1.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C18 H16 Ge' _chemical_formula_weight 304.90 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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 -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M C2/c 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 16.2568(3) _cell_length_b 9.5968(2) _cell_length_c 11.0282(2) _cell_angle_alpha 90.00 _cell_angle_beta 118.9580(10) _cell_angle_gamma 90.00 _cell_volume 1505.43(5) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 3138 _cell_measurement_theta_min 5.561 _cell_measurement_theta_max 71.945 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.18 _exptl_crystal_size_mid 0.11 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.345 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 624 _exptl_absorpt_coefficient_mu 2.609 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6510 _exptl_absorpt_correction_T_max 0.7804 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 4287 _diffrn_reflns_av_R_equivalents 0.0220 _diffrn_reflns_av_sigmaI/netI 0.0203 _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 -13 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 6.18 _diffrn_reflns_theta_max 71.94 _reflns_number_total 1377 _reflns_number_gt 1304 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT+' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0478P)^2^+1.0369P] 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 1377 _refine_ls_number_parameters 88 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0280 _refine_ls_R_factor_gt 0.0266 _refine_ls_wR_factor_ref 0.0728 _refine_ls_wR_factor_gt 0.0716 _refine_ls_goodness_of_fit_ref 1.058 _refine_ls_restrained_S_all 1.058 _refine_ls_shift/su_max 0.006 _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 0.5000 0.74126(3) 0.2500 0.02075(13) Uani 1 2 d S . . C1 C 0.40167(12) 0.62188(19) 0.12266(18) 0.0250(4) Uani 1 1 d . . . C2 C 0.34066(12) 0.55003(19) 0.03818(18) 0.0234(4) Uani 1 1 d . . . C3 C 0.26936(12) 0.46012(18) -0.06276(18) 0.0222(4) Uani 1 1 d . . . C31 C 0.27601(13) 0.41576(19) -0.17813(19) 0.0264(4) Uani 1 1 d . . . H31 H 0.3262 0.4493 -0.1926 0.032 Uiso 1 1 calc R . . C32 C 0.21047(14) 0.3234(2) -0.2721(2) 0.0294(4) Uani 1 1 d . . . H32 H 0.2162 0.2922 -0.3504 0.035 Uiso 1 1 calc R . . C33 C 0.13686(15) 0.2761(2) -0.2535(2) 0.0294(4) Uani 1 1 d . . . H33 H 0.0916 0.2120 -0.3184 0.035 Uiso 1 1 calc R . . C34 C 0.12912(13) 0.3223(2) -0.1400(2) 0.0294(4) Uani 1 1 d . . . H34 H 0.0778 0.2905 -0.1274 0.035 Uiso 1 1 calc R . . C35 C 0.19420(12) 0.4132(2) -0.04538(18) 0.0252(4) Uani 1 1 d . . . H35 H 0.1880 0.4444 0.0325 0.030 Uiso 1 1 calc R . . C4 C 0.54325(14) 0.8503(2) 0.1447(2) 0.0310(4) Uani 1 1 d . . . H4A H 0.5638 0.7892 0.0959 0.037 Uiso 1 1 calc R . . H4B H 0.5946 0.9084 0.2065 0.037 Uiso 1 1 calc R . . H4C H 0.4928 0.9076 0.0795 0.037 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 0.02140(19) 0.02314(18) 0.01621(18) 0.000 0.00792(14) 0.000 C1 0.0246(9) 0.0288(9) 0.0208(8) -0.0005(8) 0.0105(8) -0.0023(8) C2 0.0269(9) 0.0257(8) 0.0207(8) 0.0034(7) 0.0139(8) 0.0014(8) C3 0.0229(8) 0.0227(8) 0.0181(8) 0.0016(7) 0.0077(7) 0.0018(7) C31 0.0278(9) 0.0287(9) 0.0243(9) 0.0005(8) 0.0140(8) -0.0001(8) C32 0.0350(10) 0.0300(9) 0.0227(8) -0.0029(8) 0.0136(8) 0.0023(9) C33 0.0257(10) 0.0280(9) 0.0242(10) -0.0017(8) 0.0040(9) -0.0009(8) C34 0.0219(8) 0.0345(10) 0.0293(9) 0.0030(8) 0.0105(8) -0.0020(8) C35 0.0252(9) 0.0298(9) 0.0205(8) 0.0017(7) 0.0109(7) 0.0026(7) C4 0.0335(10) 0.0319(10) 0.0275(9) 0.0049(9) 0.0148(9) -0.0051(8) _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 1.9147(18) . ? Ge1 C1 1.9147(18) 2_655 ? Ge1 C4 1.9307(18) 2_655 ? Ge1 C4 1.9307(18) . ? C1 C2 1.197(3) . ? C2 C3 1.441(3) . ? C3 C31 1.395(2) . ? C3 C35 1.400(2) . ? C31 C32 1.387(3) . ? C31 H31 0.9600 . ? C32 C33 1.384(3) . ? C32 H32 0.9600 . ? C33 C34 1.390(3) . ? C33 H33 0.9600 . ? C34 C35 1.379(3) . ? C34 H34 0.9600 . ? C35 H35 0.9600 . ? C4 H4A 0.9599 . ? C4 H4B 0.9599 . ? C4 H4C 0.9599 . ? 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 C1 106.49(11) . 2_655 ? C1 Ge1 C4 110.34(8) . 2_655 ? C1 Ge1 C4 107.53(8) 2_655 2_655 ? C1 Ge1 C4 107.53(8) . . ? C1 Ge1 C4 110.34(8) 2_655 . ? C4 Ge1 C4 114.34(13) 2_655 . ? C2 C1 Ge1 176.96(16) . . ? C1 C2 C3 178.18(19) . . ? C31 C3 C35 119.02(16) . . ? C31 C3 C2 119.92(16) . . ? C35 C3 C2 121.04(16) . . ? C32 C31 C3 120.36(17) . . ? C32 C31 H31 119.8 . . ? C3 C31 H31 119.8 . . ? C33 C32 C31 120.37(18) . . ? C33 C32 H32 119.8 . . ? C31 C32 H32 119.8 . . ? C32 C33 C34 119.32(18) . . ? C32 C33 H33 120.3 . . ? C34 C33 H33 120.3 . . ? C35 C34 C33 120.86(18) . . ? C35 C34 H34 119.6 . . ? C33 C34 H34 119.6 . . ? C34 C35 C3 120.04(17) . . ? C34 C35 H35 120.0 . . ? C3 C35 H35 120.0 . . ? Ge1 C4 H4A 109.5 . . ? Ge1 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? Ge1 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 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 C1 C2 -120(3) 2_655 . . . ? C4 Ge1 C1 C2 123(3) 2_655 . . . ? C4 Ge1 C1 C2 -2(3) . . . . ? Ge1 C1 C2 C3 94(7) . . . . ? C1 C2 C3 C31 -60(6) . . . . ? C1 C2 C3 C35 118(6) . . . . ? C35 C3 C31 C32 -1.8(3) . . . . ? C2 C3 C31 C32 176.62(17) . . . . ? C3 C31 C32 C33 1.1(3) . . . . ? C31 C32 C33 C34 0.2(3) . . . . ? C32 C33 C34 C35 -0.7(3) . . . . ? C33 C34 C35 C3 -0.1(3) . . . . ? C31 C3 C35 C34 1.3(3) . . . . ? C2 C3 C35 C34 -177.09(17) . . . . ? _diffrn_measured_fraction_theta_max 0.927 _diffrn_reflns_theta_full 71.94 _diffrn_measured_fraction_theta_full 0.927 _refine_diff_density_max 0.426 _refine_diff_density_min -0.299 _refine_diff_density_rms 0.065 # Attachment '- cifcompound7.txt' data_sad1_7 _database_code_depnum_ccdc_archive 'CCDC 762759' #TrackingRef '- cifcompound7.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C42 H59 Al Ge Si4' _chemical_formula_weight 775.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Si Si 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge -1.0885 0.8855 '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 11.8818(2) _cell_length_b 17.6370(3) _cell_length_c 23.2730(3) _cell_angle_alpha 74.1410(10) _cell_angle_beta 81.1020(10) _cell_angle_gamma 79.0390(10) _cell_volume 4578.53(12) _cell_formula_units_Z 4 _cell_measurement_temperature 243(2) _cell_measurement_reflns_used 8969 _cell_measurement_theta_min 2.875 _cell_measurement_theta_max 72.387 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.27 _exptl_crystal_size_mid 0.17 _exptl_crystal_size_min 0.13 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.125 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1648 _exptl_absorpt_coefficient_mu 2.281 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.5780 _exptl_absorpt_correction_T_max 0.7559 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 243(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 27196 _diffrn_reflns_av_R_equivalents 0.0566 _diffrn_reflns_av_sigmaI/netI 0.0820 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -21 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -26 _diffrn_reflns_limit_l_max 28 _diffrn_reflns_theta_min 1.99 _diffrn_reflns_theta_max 72.58 _reflns_number_total 15605 _reflns_number_gt 12009 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT+' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.1000P)^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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 15605 _refine_ls_number_parameters 944 _refine_ls_number_restraints 36 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.0760 _refine_ls_wR_factor_ref 0.2104 _refine_ls_wR_factor_gt 0.1990 _refine_ls_goodness_of_fit_ref 1.240 _refine_ls_restrained_S_all 1.239 _refine_ls_shift/su_max 0.008 _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 0.36431(4) 0.14093(3) 0.153428(18) 0.04535(14) Uani 1 1 d . . . C131 C 0.5250(4) 0.1113(3) 0.13551(19) 0.0597(11) Uani 1 1 d . . . C132 C 0.6267(4) 0.0852(3) 0.12750(19) 0.0604(11) Uani 1 1 d . . . C133 C 0.7465(4) 0.0548(3) 0.11701(19) 0.0583(10) Uani 1 1 d . . . C134 C 0.7849(5) 0.0119(4) 0.0746(2) 0.0804(15) Uani 1 1 d . . . H134 H 0.7306 0.0021 0.0520 0.097 Uiso 1 1 calc R . . C135 C 0.9001(5) -0.0172(5) 0.0641(3) 0.105(2) Uani 1 1 d . . . H135 H 0.9261 -0.0471 0.0344 0.126 Uiso 1 1 calc R . . C136 C 0.9767(5) -0.0032(5) 0.0961(3) 0.107(2) Uani 1 1 d . . . H136 H 1.0573 -0.0222 0.0880 0.128 Uiso 1 1 calc R . . C137 C 0.9418(5) 0.0370(5) 0.1392(3) 0.099(2) Uani 1 1 d . . . H137 H 0.9970 0.0447 0.1624 0.119 Uiso 1 1 calc R . . C138 C 0.8267(4) 0.0670(4) 0.1498(2) 0.0768(14) Uani 1 1 d . . . H138 H 0.8020 0.0964 0.1799 0.092 Uiso 1 1 calc R . . C141 C 0.3023(3) 0.0610(2) 0.21953(15) 0.0410(8) Uani 1 1 d . . . C142 C 0.2776(3) -0.0083(2) 0.21483(15) 0.0450(8) Uani 1 1 d . . . H142 H 0.2410 -0.0383 0.2515 0.054 Uiso 1 1 calc R . . C143 C 0.2952(4) -0.0484(2) 0.16454(17) 0.0528(10) Uani 1 1 d D . . C144 C 0.2306(5) -0.1072(3) 0.1689(2) 0.0703(13) Uani 1 1 d D . . H144 H 0.1758 -0.1205 0.2036 0.084 Uiso 1 1 calc R . . C145 C 0.2431(6) -0.1476(4) 0.1243(3) 0.0968(19) Uani 1 1 d D . . H145 H 0.1970 -0.1882 0.1279 0.116 Uiso 1 1 calc R . . C146 C 0.3221(7) -0.1290(4) 0.0749(3) 0.108(2) Uani 1 1 d D . . H146 H 0.3308 -0.1564 0.0437 0.129 Uiso 1 1 calc R . . C147 C 0.3884(6) -0.0715(3) 0.0699(2) 0.0908(19) Uani 1 1 d D . . H147 H 0.4426 -0.0584 0.0350 0.109 Uiso 1 1 calc R . . C148 C 0.3780(4) -0.0322(3) 0.1150(2) 0.0665(12) Uani 1 1 d D . . H148 H 0.4275 0.0061 0.1122 0.080 Uiso 1 1 calc R . . C151 C 0.3484(4) 0.2432(2) 0.17192(17) 0.0510(9) Uani 1 1 d . . . C152 C 0.4438(5) 0.2792(3) 0.1693(2) 0.0702(13) Uani 1 1 d . . . H152 H 0.5195 0.2522 0.1595 0.084 Uiso 1 1 calc R . . C153 C 0.4312(6) 0.3535(4) 0.1807(3) 0.0934(18) Uani 1 1 d . . . H153 H 0.4983 0.3774 0.1785 0.112 Uiso 1 1 calc R . . C154 C 0.3241(7) 0.3936(3) 0.1952(3) 0.0956(19) Uani 1 1 d . . . H154 H 0.3166 0.4447 0.2038 0.115 Uiso 1 1 calc R . . C155 C 0.2282(6) 0.3602(3) 0.1972(3) 0.0891(18) Uani 1 1 d . . . H155 H 0.1530 0.3884 0.2064 0.107 Uiso 1 1 calc R . . C156 C 0.2396(4) 0.2845(3) 0.1859(2) 0.0648(12) Uani 1 1 d . . . H156 H 0.1720 0.2611 0.1879 0.078 Uiso 1 1 calc R . . C161 C 0.2943(4) 0.1561(2) 0.08080(16) 0.0513(9) Uani 1 1 d . . . C162 C 0.3587(5) 0.1649(3) 0.02476(19) 0.0707(13) Uani 1 1 d . . . H162 H 0.4402 0.1649 0.0218 0.085 Uiso 1 1 calc R . . C163 C 0.3077(6) 0.1737(4) -0.0270(2) 0.0924(19) Uani 1 1 d . . . H163 H 0.3538 0.1787 -0.0652 0.111 Uiso 1 1 calc R . . C164 C 0.1913(6) 0.1753(4) -0.0232(2) 0.0897(18) Uani 1 1 d . . . H164 H 0.1560 0.1817 -0.0590 0.108 Uiso 1 1 calc R . . C165 C 0.1244(5) 0.1677(3) 0.0310(2) 0.0818(15) Uani 1 1 d . . . H165 H 0.0427 0.1689 0.0332 0.098 Uiso 1 1 calc R . . C166 C 0.1768(4) 0.1582(3) 0.08291(19) 0.0650(12) Uani 1 1 d . . . H166 H 0.1301 0.1529 0.1209 0.078 Uiso 1 1 calc R . . Al1 Al 0.28154(9) 0.06557(6) 0.30468(4) 0.0387(2) Uani 1 1 d . . . C1 C 0.1713(3) 0.0047(2) 0.36105(15) 0.0427(8) Uani 1 1 d . . . H1 H 0.1631 0.0287 0.3941 0.051 Uiso 1 1 calc R . . Si11 Si 0.21481(12) -0.10282(7) 0.39960(5) 0.0587(3) Uani 1 1 d . . . C111 C 0.0928(5) -0.1447(3) 0.4531(2) 0.0902(18) Uani 1 1 d . . . H11A H 0.1195 -0.1984 0.4744 0.108 Uiso 1 1 calc R . . H11B H 0.0310 -0.1446 0.4309 0.108 Uiso 1 1 calc R . . H11C H 0.0657 -0.1125 0.4811 0.108 Uiso 1 1 calc R . . C112 C 0.2651(6) -0.1687(3) 0.3477(2) 0.099(2) Uani 1 1 d . . . H11D H 0.3352 -0.1544 0.3242 0.119 Uiso 1 1 calc R . . H11E H 0.2072 -0.1626 0.3215 0.119 Uiso 1 1 calc R . . H11F H 0.2788 -0.2232 0.3706 0.119 Uiso 1 1 calc R . . C113 C 0.3327(5) -0.1122(3) 0.4458(3) 0.0910(18) Uani 1 1 d . . . H11G H 0.3990 -0.0943 0.4202 0.109 Uiso 1 1 calc R . . H11H H 0.3524 -0.1671 0.4670 0.109 Uiso 1 1 calc R . . H11I H 0.3078 -0.0802 0.4742 0.109 Uiso 1 1 calc R . . Si12 Si 0.02147(10) 0.03515(8) 0.33719(5) 0.0587(3) Uani 1 1 d . . . C121 C -0.0223(5) -0.0385(4) 0.3046(3) 0.0875(17) Uani 1 1 d . . . H12A H 0.0266 -0.0419 0.2682 0.105 Uiso 1 1 calc R . . H12B H -0.1009 -0.0218 0.2960 0.105 Uiso 1 1 calc R . . H12C H -0.0151 -0.0898 0.3328 0.105 Uiso 1 1 calc R . . C122 C 0.0059(5) 0.1313(3) 0.2776(3) 0.0828(16) Uani 1 1 d . . . H12D H 0.0579 0.1256 0.2426 0.099 Uiso 1 1 calc R . . H12E H 0.0238 0.1730 0.2923 0.099 Uiso 1 1 calc R . . H12F H -0.0719 0.1447 0.2673 0.099 Uiso 1 1 calc R . . C123 C -0.0850(5) 0.0516(5) 0.4022(3) 0.103(2) Uani 1 1 d . . . H12G H -0.1614 0.0647 0.3900 0.124 Uiso 1 1 calc R . . H12H H -0.0684 0.0948 0.4156 0.124 Uiso 1 1 calc R . . H12I H -0.0800 0.0040 0.4343 0.124 Uiso 1 1 calc R . . C2 C 0.3727(3) 0.1290(2) 0.32930(15) 0.0467(8) Uani 1 1 d . . . H2 H 0.3806 0.1718 0.2939 0.056 Uiso 1 1 calc R . . Si21 Si 0.52632(11) 0.07964(9) 0.33629(5) 0.0632(3) Uani 1 1 d . . . C211 C 0.6279(5) 0.1514(5) 0.2961(3) 0.102(2) Uani 1 1 d . . . H21A H 0.6065 0.1769 0.2565 0.123 Uiso 1 1 calc R . . H21B H 0.7051 0.1229 0.2934 0.123 Uiso 1 1 calc R . . H21C H 0.6240 0.1909 0.3180 0.123 Uiso 1 1 calc R . . C212 C 0.5615(5) -0.0062(4) 0.3007(3) 0.0882(17) Uani 1 1 d . . . H21D H 0.5505 0.0126 0.2589 0.106 Uiso 1 1 calc R . . H21E H 0.5116 -0.0448 0.3202 0.106 Uiso 1 1 calc R . . H21F H 0.6403 -0.0304 0.3049 0.106 Uiso 1 1 calc R . . C213 C 0.5609(5) 0.0402(4) 0.4156(2) 0.100(2) Uani 1 1 d . . . H21G H 0.6359 0.0082 0.4164 0.120 Uiso 1 1 calc R . . H21H H 0.5044 0.0081 0.4384 0.120 Uiso 1 1 calc R . . H21I H 0.5601 0.0839 0.4329 0.120 Uiso 1 1 calc R . . Si22 Si 0.30188(14) 0.18347(9) 0.38686(6) 0.0714(4) Uani 1 1 d . . . C221 C 0.2672(6) 0.1187(4) 0.4627(2) 0.0946(19) Uani 1 1 d . . . H22A H 0.2157 0.0841 0.4604 0.114 Uiso 1 1 calc R . . H22B H 0.2311 0.1513 0.4894 0.114 Uiso 1 1 calc R . . H22C H 0.3369 0.0873 0.4775 0.114 Uiso 1 1 calc R . . C222 C 0.1596(7) 0.2409(5) 0.3648(4) 0.145(4) Uani 1 1 d . . . H22D H 0.1716 0.2858 0.3315 0.174 Uiso 1 1 calc R . . H22E H 0.1167 0.2594 0.3981 0.174 Uiso 1 1 calc R . . H22F H 0.1172 0.2071 0.3534 0.174 Uiso 1 1 calc R . . C223 C 0.3929(9) 0.2548(6) 0.3957(4) 0.169(5) Uani 1 1 d . . . H22G H 0.4717 0.2292 0.3969 0.203 Uiso 1 1 calc R . . H22H H 0.3659 0.2706 0.4324 0.203 Uiso 1 1 calc R . . H22I H 0.3878 0.3010 0.3624 0.203 Uiso 1 1 calc R . . Ge2 Ge 0.18464(4) 0.39407(3) -0.15998(2) 0.05345(16) Uani 1 1 d . . . C231 C 0.0388(4) 0.3655(4) -0.1263(2) 0.0717(13) Uani 1 1 d . . . C232 C -0.0579(5) 0.3534(4) -0.1055(2) 0.0784(14) Uani 1 1 d . . . C233 C -0.1747(5) 0.3410(3) -0.0787(3) 0.0780(15) Uani 1 1 d . . . C234 C -0.1977(7) 0.2970(7) -0.0221(3) 0.145(4) Uani 1 1 d . . . H234 H -0.1339 0.2711 0.0005 0.174 Uiso 1 1 calc R . . C235 C -0.3065(8) 0.2871(7) 0.0048(4) 0.144(4) Uani 1 1 d . . . H235 H -0.3186 0.2566 0.0457 0.173 Uiso 1 1 calc R . . C236 C -0.3942(8) 0.3203(6) -0.0265(7) 0.153(5) Uani 1 1 d . . . H236 H -0.4711 0.3154 -0.0076 0.184 Uiso 1 1 calc R . . C237 C -0.3784(7) 0.3614(7) -0.0853(6) 0.177(5) Uani 1 1 d . . . H237 H -0.4438 0.3833 -0.1076 0.212 Uiso 1 1 calc R . . C238 C -0.2657(6) 0.3721(5) -0.1137(5) 0.139(3) Uani 1 1 d . . . H238 H -0.2529 0.3996 -0.1553 0.167 Uiso 1 1 calc R . . C241 C 0.1785(3) 0.4768(2) -0.23555(17) 0.0475(8) Uani 1 1 d . B . C242 C 0.1551(4) 0.5547(3) -0.2385(2) 0.0662(13) Uani 1 1 d . . . H242 H 0.1427 0.5844 -0.2788 0.079 Uiso 1 1 calc R A 1 C243 C 0.1428(15) 0.6072(10) -0.2008(7) 0.055(4) Uani 0.46(2) 1 d PD B 1 C244 C 0.1948(17) 0.6734(7) -0.2097(7) 0.078(4) Uani 0.46(2) 1 d PD B 1 H244 H 0.2430 0.6898 -0.2465 0.093 Uiso 0.46(2) 1 calc PR B 1 C245 C 0.180(2) 0.7176(10) -0.1667(9) 0.112(7) Uani 0.46(2) 1 d PD B 1 H245 H 0.2185 0.7626 -0.1726 0.134 Uiso 0.46(2) 1 calc PR B 1 C246 C 0.106(3) 0.6933(17) -0.1155(10) 0.128(14) Uani 0.46(2) 1 d PD B 1 H246 H 0.0974 0.7206 -0.0842 0.154 Uiso 0.46(2) 1 calc PR B 1 C247 C 0.0465(17) 0.6319(17) -0.1078(10) 0.117(10) Uani 0.46(2) 1 d PD B 1 H247 H -0.0091 0.6201 -0.0733 0.141 Uiso 0.46(2) 1 calc PR B 1 C248 C 0.0652(13) 0.5864(12) -0.1493(8) 0.068(5) Uani 0.46(2) 1 d PD B 1 H248 H 0.0258 0.5415 -0.1431 0.081 Uiso 0.46(2) 1 calc PR B 1 C24A C 0.1024(14) 0.5915(6) -0.1834(6) 0.049(3) Uani 0.54(2) 1 d PD B 2 C24B C 0.1325(16) 0.6640(6) -0.1873(6) 0.081(4) Uani 0.54(2) 1 d PD B 2 H24B H 0.1785 0.6891 -0.2225 0.097 Uiso 0.54(2) 1 calc PR B 2 C24C C 0.097(2) 0.7022(9) -0.1405(8) 0.097(6) Uani 0.54(2) 1 d PD B 2 H24C H 0.1141 0.7545 -0.1441 0.116 Uiso 0.54(2) 1 calc PR B 2 C24D C 0.0364(18) 0.6623(8) -0.0890(7) 0.103(6) Uani 0.54(2) 1 d PD B 2 H24D H 0.0170 0.6860 -0.0555 0.124 Uiso 0.54(2) 1 calc PR B 2 C24E C 0.0031(14) 0.5907(8) -0.0839(6) 0.083(4) Uani 0.54(2) 1 d PD B 2 H24E H -0.0408 0.5655 -0.0478 0.099 Uiso 0.54(2) 1 calc PR B 2 C24F C 0.0334(12) 0.5547(8) -0.1312(6) 0.059(3) Uani 0.54(2) 1 d PD B 2 H24F H 0.0081 0.5053 -0.1290 0.071 Uiso 0.54(2) 1 calc PR B 2 C251 C 0.2750(5) 0.2980(3) -0.17855(19) 0.0650(12) Uani 1 1 d . . . C252 C 0.2244(6) 0.2362(3) -0.1839(2) 0.0773(15) Uani 1 1 d . . . H252 H 0.1419 0.2404 -0.1786 0.093 Uiso 1 1 calc R . . C253 C 0.2929(8) 0.1668(3) -0.1969(3) 0.105(2) Uani 1 1 d . . . H253 H 0.2572 0.1240 -0.2004 0.126 Uiso 1 1 calc R . . C254 C 0.4095(8) 0.1612(4) -0.2045(3) 0.110(3) Uani 1 1 d . . . H254 H 0.4554 0.1144 -0.2142 0.132 Uiso 1 1 calc R . . C255 C 0.4645(6) 0.2213(4) -0.1987(3) 0.100(2) Uani 1 1 d . . . H255 H 0.5471 0.2162 -0.2033 0.121 Uiso 1 1 calc R . . C256 C 0.3956(5) 0.2887(3) -0.1861(2) 0.0777(15) Uani 1 1 d . . . H256 H 0.4322 0.3310 -0.1823 0.093 Uiso 1 1 calc R . . C261 C 0.2500(4) 0.4210(3) -0.09800(17) 0.0575(10) Uani 1 1 d . . . C262 C 0.3192(4) 0.4814(3) -0.1118(2) 0.0670(12) Uani 1 1 d . . . H262 H 0.3379 0.5089 -0.1529 0.080 Uiso 1 1 calc R . . C263 C 0.3611(5) 0.5016(4) -0.0656(2) 0.0829(15) Uani 1 1 d . . . H263 H 0.4080 0.5431 -0.0755 0.099 Uiso 1 1 calc R . . C264 C 0.3361(5) 0.4631(4) -0.0066(3) 0.0932(18) Uani 1 1 d . . . H264 H 0.3623 0.4787 0.0248 0.112 Uiso 1 1 calc R . . C265 C 0.2729(6) 0.4017(4) 0.0068(2) 0.0947(19) Uani 1 1 d . . . H265 H 0.2601 0.3713 0.0477 0.114 Uiso 1 1 calc R . . C266 C 0.2271(5) 0.3833(4) -0.0386(2) 0.0855(17) Uani 1 1 d . . . H266 H 0.1781 0.3430 -0.0279 0.103 Uiso 1 1 calc R . . Al2 Al 0.21065(10) 0.45149(6) -0.31428(5) 0.0424(2) Uani 1 1 d . . . C3 C 0.3148(4) 0.5103(2) -0.37594(17) 0.0523(9) Uani 1 1 d . B . H3 H 0.3320 0.4780 -0.4043 0.063 Uiso 1 1 calc R . . Si31 Si 0.46212(12) 0.50927(9) -0.35575(6) 0.0693(4) Uani 1 1 d . . . C311 C 0.5398(5) 0.4046(4) -0.3307(3) 0.108(2) Uani 1 1 d . B . H31A H 0.5431 0.3772 -0.3615 0.130 Uiso 1 1 calc R . . H31B H 0.4993 0.3771 -0.2944 0.130 Uiso 1 1 calc R . . H31C H 0.6167 0.4062 -0.3236 0.130 Uiso 1 1 calc R . . C312 C 0.4571(5) 0.5576(5) -0.2937(3) 0.107(2) Uani 1 1 d . B . H31D H 0.5332 0.5664 -0.2909 0.129 Uiso 1 1 calc R . . H31E H 0.4289 0.5237 -0.2566 0.129 Uiso 1 1 calc R . . H31F H 0.4066 0.6079 -0.3016 0.129 Uiso 1 1 calc R . . C313 C 0.5563(5) 0.5588(4) -0.4218(3) 0.0879(17) Uani 1 1 d . B . H31G H 0.5261 0.6146 -0.4339 0.105 Uiso 1 1 calc R . . H31H H 0.5584 0.5348 -0.4544 0.105 Uiso 1 1 calc R . . H31I H 0.6329 0.5525 -0.4110 0.105 Uiso 1 1 calc R . . Si32 Si 0.24455(13) 0.60739(7) -0.42229(6) 0.0671(4) Uani 1 1 d . . . C321 C 0.2602(7) 0.6960(3) -0.3968(3) 0.108(2) Uani 1 1 d . B . H32A H 0.3227 0.7207 -0.4212 0.130 Uiso 1 1 calc R . . H32B H 0.2761 0.6793 -0.3556 0.130 Uiso 1 1 calc R . . H32C H 0.1901 0.7335 -0.4003 0.130 Uiso 1 1 calc R . . C322 C 0.0875(6) 0.6048(4) -0.4195(3) 0.110(2) Uani 1 1 d . B . H32D H 0.0527 0.6522 -0.4463 0.132 Uiso 1 1 calc R . . H32E H 0.0514 0.6020 -0.3793 0.132 Uiso 1 1 calc R . . H32F H 0.0776 0.5587 -0.4316 0.132 Uiso 1 1 calc R . . C323 C 0.3033(6) 0.6243(3) -0.5026(2) 0.0910(18) Uani 1 1 d . B . H32G H 0.3804 0.6360 -0.5073 0.109 Uiso 1 1 calc R . . H32H H 0.2556 0.6684 -0.5262 0.109 Uiso 1 1 calc R . . H32I H 0.3043 0.5773 -0.5160 0.109 Uiso 1 1 calc R . . C4 C 0.1337(3) 0.3701(2) -0.32701(17) 0.0495(9) Uani 1 1 d . B . H4 H 0.1488 0.3281 -0.2916 0.059 Uiso 1 1 calc R . . Si41 Si 0.20541(13) 0.31904(8) -0.38719(6) 0.0671(4) Uani 1 1 d . . . C411 C 0.1917(6) 0.3854(4) -0.4643(2) 0.0919(19) Uani 1 1 d . B . H41A H 0.1115 0.4031 -0.4697 0.110 Uiso 1 1 calc R . . H41B H 0.2272 0.3564 -0.4936 0.110 Uiso 1 1 calc R . . H41C H 0.2292 0.4307 -0.4694 0.110 Uiso 1 1 calc R . . C412 C 0.3607(5) 0.2852(4) -0.3796(3) 0.099(2) Uani 1 1 d . B . H41D H 0.4006 0.3305 -0.3915 0.119 Uiso 1 1 calc R . . H41E H 0.3914 0.2495 -0.4048 0.119 Uiso 1 1 calc R . . H41F H 0.3708 0.2580 -0.3385 0.119 Uiso 1 1 calc R . . C413 C 0.1435(7) 0.2272(4) -0.3820(3) 0.118(3) Uani 1 1 d . B . H41G H 0.1574 0.1894 -0.3444 0.142 Uiso 1 1 calc R . . H41H H 0.1794 0.2040 -0.4144 0.142 Uiso 1 1 calc R . . H41I H 0.0620 0.2409 -0.3846 0.142 Uiso 1 1 calc R . . Si42 Si -0.02793(12) 0.38734(10) -0.31815(6) 0.0700(4) Uani 1 1 d . . . C421 C -0.0938(5) 0.4703(4) -0.2817(3) 0.0883(17) Uani 1 1 d . B . H42A H -0.0697 0.5193 -0.3057 0.106 Uiso 1 1 calc R . . H42B H -0.0691 0.4585 -0.2424 0.106 Uiso 1 1 calc R . . H42C H -0.1763 0.4756 -0.2783 0.106 Uiso 1 1 calc R . . C422 C -0.0918(5) 0.4127(6) -0.3908(3) 0.118(3) Uani 1 1 d . B . H42D H -0.1738 0.4276 -0.3839 0.142 Uiso 1 1 calc R . . H42E H -0.0752 0.3671 -0.4075 0.142 Uiso 1 1 calc R . . H42F H -0.0592 0.4563 -0.4184 0.142 Uiso 1 1 calc R . . C423 C -0.0811(6) 0.2956(4) -0.2677(3) 0.108(2) Uani 1 1 d . B . H42G H -0.0698 0.2916 -0.2270 0.130 Uiso 1 1 calc R . . H42H H -0.0391 0.2493 -0.2798 0.130 Uiso 1 1 calc R . . H42I H -0.1618 0.2990 -0.2706 0.130 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 0.0493(3) 0.0477(2) 0.0371(2) -0.00798(18) 0.00179(17) -0.01195(19) C131 0.050(3) 0.063(2) 0.061(3) -0.013(2) 0.0171(19) -0.0175(19) C132 0.066(3) 0.061(2) 0.052(2) -0.0087(19) 0.005(2) -0.021(2) C133 0.053(3) 0.067(3) 0.052(2) -0.016(2) 0.0045(18) -0.012(2) C134 0.063(3) 0.117(4) 0.078(3) -0.055(3) 0.000(2) -0.017(3) C135 0.073(4) 0.143(6) 0.118(5) -0.085(5) 0.017(4) -0.011(4) C136 0.059(4) 0.142(6) 0.118(5) -0.050(5) 0.003(3) 0.003(4) C137 0.064(4) 0.154(6) 0.090(4) -0.042(4) -0.018(3) -0.019(4) C138 0.063(3) 0.110(4) 0.071(3) -0.042(3) 0.002(2) -0.025(3) C141 0.045(2) 0.0464(18) 0.0336(17) -0.0115(14) -0.0013(14) -0.0114(15) C142 0.053(2) 0.0486(19) 0.0340(18) -0.0105(15) -0.0026(15) -0.0116(16) C143 0.070(3) 0.0447(19) 0.046(2) -0.0189(17) -0.0081(18) -0.0029(18) C144 0.083(3) 0.064(3) 0.075(3) -0.034(2) -0.003(2) -0.018(2) C145 0.124(5) 0.086(4) 0.102(5) -0.056(4) -0.015(4) -0.019(4) C146 0.159(7) 0.090(4) 0.090(4) -0.062(4) -0.012(4) -0.004(4) C147 0.126(5) 0.079(3) 0.062(3) -0.038(3) 0.018(3) 0.004(3) C148 0.086(3) 0.051(2) 0.057(3) -0.018(2) 0.005(2) 0.000(2) C151 0.067(3) 0.0449(19) 0.042(2) -0.0054(16) -0.0075(17) -0.0177(18) C152 0.081(3) 0.061(3) 0.074(3) -0.017(2) 0.002(2) -0.033(2) C153 0.111(5) 0.084(4) 0.100(4) -0.028(3) 0.000(4) -0.053(4) C154 0.139(6) 0.057(3) 0.102(4) -0.023(3) -0.036(4) -0.018(3) C155 0.103(5) 0.070(3) 0.103(4) -0.036(3) -0.040(4) 0.008(3) C156 0.072(3) 0.057(2) 0.073(3) -0.027(2) -0.017(2) -0.004(2) C161 0.069(3) 0.049(2) 0.0360(19) -0.0154(16) -0.0008(17) -0.0062(18) C162 0.084(3) 0.080(3) 0.042(2) -0.011(2) 0.001(2) -0.008(3) C163 0.133(6) 0.095(4) 0.041(3) -0.015(3) 0.003(3) -0.010(4) C164 0.127(5) 0.101(4) 0.044(3) -0.020(3) -0.031(3) -0.005(4) C165 0.095(4) 0.094(4) 0.062(3) -0.022(3) -0.026(3) -0.010(3) C166 0.069(3) 0.084(3) 0.045(2) -0.020(2) -0.0124(19) -0.007(2) Al1 0.0433(6) 0.0405(5) 0.0344(5) -0.0105(4) -0.0014(4) -0.0127(4) C1 0.050(2) 0.0472(18) 0.0340(17) -0.0110(14) 0.0007(14) -0.0186(16) Si11 0.0795(8) 0.0521(6) 0.0455(6) -0.0017(5) -0.0084(5) -0.0266(6) C111 0.120(5) 0.087(4) 0.060(3) 0.016(3) -0.008(3) -0.059(3) C112 0.170(7) 0.051(3) 0.070(3) -0.010(2) -0.011(4) -0.011(3) C113 0.101(4) 0.082(4) 0.085(4) 0.013(3) -0.040(3) -0.028(3) Si12 0.0512(7) 0.0725(7) 0.0533(6) -0.0121(5) 0.0009(5) -0.0229(5) C121 0.089(4) 0.099(4) 0.088(4) -0.017(3) -0.030(3) -0.042(3) C122 0.068(3) 0.075(3) 0.091(4) -0.005(3) -0.009(3) 0.001(3) C123 0.061(3) 0.161(6) 0.078(4) -0.034(4) 0.019(3) -0.012(4) C2 0.059(2) 0.052(2) 0.0359(18) -0.0151(16) 0.0025(15) -0.0254(17) Si21 0.0535(7) 0.0948(9) 0.0452(6) -0.0115(6) -0.0070(5) -0.0288(6) C211 0.071(4) 0.156(6) 0.083(4) -0.011(4) 0.006(3) -0.065(4) C212 0.072(4) 0.109(4) 0.078(4) -0.029(3) -0.013(3) 0.010(3) C213 0.086(4) 0.162(6) 0.054(3) -0.010(3) -0.024(3) -0.038(4) Si22 0.0996(11) 0.0678(8) 0.0599(7) -0.0332(6) 0.0090(7) -0.0346(7) C221 0.118(5) 0.126(5) 0.052(3) -0.038(3) 0.020(3) -0.048(4) C222 0.179(8) 0.125(6) 0.114(6) -0.062(5) -0.002(5) 0.053(6) C223 0.231(10) 0.178(9) 0.165(8) -0.128(7) 0.072(7) -0.143(8) Ge2 0.0558(3) 0.0643(3) 0.0442(3) -0.0235(2) 0.0021(2) -0.0106(2) C231 0.059(3) 0.107(4) 0.056(3) -0.030(3) 0.007(2) -0.027(3) C232 0.075(3) 0.099(4) 0.073(3) -0.040(3) 0.006(3) -0.026(3) C233 0.068(3) 0.089(4) 0.087(4) -0.040(3) 0.019(3) -0.032(3) C234 0.091(5) 0.262(12) 0.094(5) -0.045(6) 0.016(4) -0.078(6) C235 0.105(6) 0.208(10) 0.120(6) -0.034(6) 0.038(5) -0.077(7) C236 0.083(6) 0.120(7) 0.277(15) -0.110(8) 0.061(8) -0.046(5) C237 0.064(5) 0.149(9) 0.293(16) -0.040(9) -0.013(7) 0.015(5) C238 0.075(5) 0.119(6) 0.195(9) -0.008(6) -0.009(5) 0.002(4) C241 0.046(2) 0.054(2) 0.048(2) -0.0203(17) -0.0127(16) -0.0060(16) C242 0.082(3) 0.060(2) 0.066(3) -0.036(2) -0.028(2) 0.009(2) C243 0.055(9) 0.068(9) 0.042(8) -0.020(7) -0.002(5) 0.002(6) C244 0.100(12) 0.059(7) 0.082(9) -0.035(7) -0.004(8) -0.011(7) C245 0.125(17) 0.110(12) 0.123(14) -0.081(11) -0.022(12) 0.012(11) C246 0.16(3) 0.14(2) 0.10(2) -0.071(19) -0.058(19) 0.039(19) C247 0.073(12) 0.19(3) 0.098(15) -0.10(2) 0.002(9) 0.039(14) C248 0.046(9) 0.094(13) 0.069(11) -0.042(11) -0.003(7) 0.001(7) C24A 0.059(10) 0.045(5) 0.042(7) -0.017(6) -0.006(6) 0.000(5) C24B 0.117(12) 0.056(6) 0.075(8) -0.035(6) 0.000(7) -0.010(6) C24C 0.120(16) 0.059(7) 0.118(15) -0.047(9) -0.014(13) 0.005(8) C24D 0.136(15) 0.085(9) 0.086(10) -0.050(8) 0.001(9) 0.020(9) C24E 0.076(10) 0.102(9) 0.066(7) -0.044(7) -0.002(6) 0.026(6) C24F 0.047(7) 0.069(7) 0.061(7) -0.029(5) 0.003(5) 0.001(5) C251 0.091(4) 0.055(2) 0.045(2) -0.0117(19) -0.006(2) -0.003(2) C252 0.120(5) 0.066(3) 0.049(3) -0.015(2) -0.022(3) -0.010(3) C253 0.195(8) 0.057(3) 0.067(4) -0.018(3) -0.039(4) -0.007(4) C254 0.154(7) 0.090(4) 0.075(4) -0.033(3) -0.023(4) 0.031(5) C255 0.117(5) 0.093(4) 0.082(4) -0.028(3) -0.012(4) 0.018(4) C256 0.082(4) 0.076(3) 0.064(3) -0.023(2) 0.005(2) 0.011(3) C261 0.061(3) 0.075(3) 0.039(2) -0.0220(19) -0.0030(17) -0.008(2) C262 0.060(3) 0.086(3) 0.060(3) -0.020(2) -0.011(2) -0.017(2) C263 0.081(4) 0.102(4) 0.077(4) -0.026(3) -0.016(3) -0.029(3) C264 0.099(4) 0.129(5) 0.069(3) -0.047(4) -0.020(3) -0.021(4) C265 0.128(5) 0.121(5) 0.042(3) -0.027(3) -0.004(3) -0.031(4) C266 0.123(5) 0.097(4) 0.050(3) -0.033(3) 0.009(3) -0.041(3) Al2 0.0470(6) 0.0410(5) 0.0433(6) -0.0152(4) -0.0033(4) -0.0114(4) C3 0.067(3) 0.046(2) 0.048(2) -0.0141(17) -0.0023(18) -0.0212(18) Si31 0.0690(9) 0.0768(8) 0.0696(8) -0.0169(7) 0.0013(6) -0.0391(7) C311 0.071(4) 0.113(5) 0.122(5) 0.015(4) -0.019(3) -0.026(3) C312 0.089(4) 0.179(7) 0.085(4) -0.061(4) 0.001(3) -0.066(5) C313 0.087(4) 0.084(4) 0.100(4) -0.031(3) 0.024(3) -0.047(3) Si32 0.0989(10) 0.0473(6) 0.0560(7) -0.0126(5) -0.0055(6) -0.0165(6) C321 0.191(7) 0.048(3) 0.090(4) -0.017(3) -0.018(4) -0.028(4) C322 0.106(5) 0.092(4) 0.117(5) -0.017(4) -0.018(4) 0.014(4) C323 0.143(6) 0.067(3) 0.059(3) -0.010(2) -0.007(3) -0.019(3) C4 0.056(2) 0.055(2) 0.046(2) -0.0199(17) 0.0036(16) -0.0249(18) Si41 0.0870(9) 0.0650(7) 0.0635(7) -0.0341(6) 0.0125(6) -0.0368(7) C411 0.113(5) 0.124(5) 0.053(3) -0.032(3) 0.011(3) -0.055(4) C412 0.089(4) 0.080(4) 0.131(6) -0.050(4) 0.010(4) -0.005(3) C413 0.162(7) 0.102(5) 0.124(5) -0.074(4) 0.038(5) -0.079(5) Si42 0.0583(8) 0.1025(10) 0.0616(7) -0.0301(7) -0.0004(6) -0.0340(7) C421 0.057(3) 0.120(5) 0.093(4) -0.042(4) -0.005(3) -0.004(3) C422 0.082(5) 0.205(8) 0.089(4) -0.050(5) -0.032(3) -0.035(5) C423 0.092(4) 0.140(6) 0.109(5) -0.040(4) 0.022(4) -0.074(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 C131 1.893(4) . ? Ge1 C161 1.930(4) . ? Ge1 C151 1.935(4) . ? Ge1 C141 1.938(3) . ? C131 C132 1.214(6) . ? C132 C133 1.431(6) . ? C133 C134 1.375(6) . ? C133 C138 1.390(6) . ? C134 C135 1.377(8) . ? C134 H134 0.9600 . ? C135 C136 1.356(9) . ? C135 H135 0.9600 . ? C136 C137 1.353(9) . ? C136 H136 0.9600 . ? C137 C138 1.379(8) . ? C137 H137 0.9600 . ? C138 H138 0.9600 . ? C141 C142 1.346(5) . ? C141 Al1 1.981(3) . ? C142 C143 1.494(5) . ? C142 H142 0.9600 . ? C143 C144 1.377(6) . ? C143 C148 1.397(6) . ? C144 C145 1.389(6) . ? C144 H144 0.9600 . ? C145 C146 1.374(9) . ? C145 H145 0.9600 . ? C146 C147 1.369(9) . ? C146 H146 0.9600 . ? C147 C148 1.386(6) . ? C147 H147 0.9600 . ? C148 H148 0.9600 . ? C151 C152 1.387(6) . ? C151 C156 1.396(6) . ? C152 C153 1.383(7) . ? C152 H152 0.9600 . ? C153 C154 1.374(9) . ? C153 H153 0.9600 . ? C154 C155 1.368(9) . ? C154 H154 0.9600 . ? C155 C156 1.407(7) . ? C155 H155 0.9600 . ? C156 H156 0.9600 . ? C161 C166 1.383(6) . ? C161 C162 1.392(5) . ? C162 C163 1.390(7) . ? C162 H162 0.9600 . ? C163 C164 1.367(8) . ? C163 H163 0.9600 . ? C164 C165 1.370(8) . ? C164 H164 0.9600 . ? C165 C166 1.400(6) . ? C165 H165 0.9600 . ? C166 H166 0.9600 . ? Al1 C2 1.938(4) . ? Al1 C1 1.955(3) . ? C1 Si11 1.873(4) . ? C1 Si12 1.883(4) . ? C1 H1 0.9600 . ? Si11 C113 1.850(5) . ? Si11 C112 1.857(5) . ? Si11 C111 1.882(5) . ? C111 H11A 0.9599 . ? C111 H11B 0.9599 . ? C111 H11C 0.9599 . ? C112 H11D 0.9599 . ? C112 H11E 0.9599 . ? C112 H11F 0.9599 . ? C113 H11G 0.9599 . ? C113 H11H 0.9599 . ? C113 H11I 0.9599 . ? Si12 C121 1.857(5) . ? Si12 C123 1.866(5) . ? Si12 C122 1.873(5) . ? C121 H12A 0.9599 . ? C121 H12B 0.9599 . ? C121 H12C 0.9599 . ? C122 H12D 0.9599 . ? C122 H12E 0.9599 . ? C122 H12F 0.9599 . ? C123 H12G 0.9599 . ? C123 H12H 0.9599 . ? C123 H12I 0.9599 . ? C2 Si22 1.864(4) . ? C2 Si21 1.877(4) . ? C2 H2 0.9600 . ? Si21 C212 1.867(6) . ? Si21 C213 1.867(5) . ? Si21 C211 1.875(5) . ? C211 H21A 0.9599 . ? C211 H21B 0.9599 . ? C211 H21C 0.9599 . ? C212 H21D 0.9599 . ? C212 H21E 0.9599 . ? C212 H21F 0.9599 . ? C213 H21G 0.9599 . ? C213 H21H 0.9599 . ? C213 H21I 0.9599 . ? Si22 C221 1.855(5) . ? Si22 C222 1.866(8) . ? Si22 C223 1.877(7) . ? C221 H22A 0.9599 . ? C221 H22B 0.9599 . ? C221 H22C 0.9599 . ? C222 H22D 0.9599 . ? C222 H22E 0.9599 . ? C222 H22F 0.9599 . ? C223 H22G 0.9599 . ? C223 H22H 0.9599 . ? C223 H22I 0.9599 . ? Ge2 C231 1.889(5) . ? Ge2 C261 1.942(4) . ? Ge2 C251 1.943(4) . ? Ge2 C241 1.956(4) . ? C231 C232 1.210(7) . ? C232 C233 1.461(7) . ? C233 C234 1.349(10) . ? C233 C238 1.391(10) . ? C234 C235 1.367(10) . ? C234 H234 0.9600 . ? C235 C236 1.316(13) . ? C235 H235 0.9600 . ? C236 C237 1.365(15) . ? C236 H236 0.9600 . ? C237 C238 1.421(12) . ? C237 H237 0.9600 . ? C238 H238 0.9600 . ? C241 C242 1.333(6) . ? C241 Al2 1.967(4) . ? C242 C243 1.415(13) . ? C242 C24A 1.586(13) . ? C242 H242 0.9600 . ? C243 C244 1.375(13) . ? C243 C248 1.403(12) . ? C244 C245 1.400(13) . ? C244 H244 0.9600 . ? C245 C246 1.380(18) . ? C245 H245 0.9600 . ? C246 C247 1.365(18) . ? C246 H246 0.9600 . ? C247 C248 1.386(13) . ? C247 H247 0.9600 . ? C248 H248 0.9600 . ? C24A C24B 1.367(12) . ? C24A C24F 1.425(11) . ? C24B C24C 1.404(14) . ? C24B H24B 0.9600 . ? C24C C24D 1.383(17) . ? C24C H24C 0.9600 . ? C24D C24E 1.363(16) . ? C24D H24D 0.9600 . ? C24E C24F 1.387(11) . ? C24E H24E 0.9600 . ? C24F H24F 0.9600 . ? C251 C252 1.384(7) . ? C251 C256 1.400(7) . ? C252 C253 1.414(8) . ? C252 H252 0.9600 . ? C253 C254 1.358(10) . ? C253 H253 0.9600 . ? C254 C255 1.393(10) . ? C254 H254 0.9600 . ? C255 C256 1.385(7) . ? C255 H255 0.9600 . ? C256 H256 0.9600 . ? C261 C266 1.370(6) . ? C261 C262 1.407(7) . ? C262 C263 1.405(6) . ? C262 H262 0.9600 . ? C263 C264 1.369(8) . ? C263 H263 0.9600 . ? C264 C265 1.373(9) . ? C264 H264 0.9600 . ? C265 C266 1.398(7) . ? C265 H265 0.9600 . ? C266 H266 0.9600 . ? Al2 C3 1.947(4) . ? Al2 C4 1.950(4) . ? C3 Si32 1.876(4) . ? C3 Si31 1.877(4) . ? C3 H3 0.9600 . ? Si31 C312 1.855(6) . ? Si31 C313 1.866(5) . ? Si31 C311 1.878(6) . ? C311 H31A 0.9599 . ? C311 H31B 0.9599 . ? C311 H31C 0.9599 . ? C312 H31D 0.9599 . ? C312 H31E 0.9599 . ? C312 H31F 0.9599 . ? C313 H31G 0.9599 . ? C313 H31H 0.9599 . ? C313 H31I 0.9599 . ? Si32 C323 1.856(5) . ? Si32 C321 1.866(5) . ? Si32 C322 1.866(7) . ? C321 H32A 0.9599 . ? C321 H32B 0.9599 . ? C321 H32C 0.9599 . ? C322 H32D 0.9599 . ? C322 H32E 0.9599 . ? C322 H32F 0.9599 . ? C323 H32G 0.9599 . ? C323 H32H 0.9599 . ? C323 H32I 0.9599 . ? C4 Si42 1.874(4) . ? C4 Si41 1.878(4) . ? C4 H4 0.9600 . ? Si41 C412 1.849(6) . ? Si41 C411 1.868(6) . ? Si41 C413 1.871(6) . ? C411 H41A 0.9599 . ? C411 H41B 0.9599 . ? C411 H41C 0.9599 . ? C412 H41D 0.9599 . ? C412 H41E 0.9599 . ? C412 H41F 0.9599 . ? C413 H41G 0.9599 . ? C413 H41H 0.9599 . ? C413 H41I 0.9599 . ? Si42 C422 1.869(6) . ? Si42 C421 1.874(6) . ? Si42 C423 1.875(6) . ? C421 H42A 0.9599 . ? C421 H42B 0.9599 . ? C421 H42C 0.9599 . ? C422 H42D 0.9599 . ? C422 H42E 0.9599 . ? C422 H42F 0.9599 . ? C423 H42G 0.9599 . ? C423 H42H 0.9599 . ? C423 H42I 0.9599 . ? 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 C131 Ge1 C161 107.17(19) . . ? C131 Ge1 C151 104.82(19) . . ? C161 Ge1 C151 108.58(16) . . ? C131 Ge1 C141 110.88(17) . . ? C161 Ge1 C141 112.33(16) . . ? C151 Ge1 C141 112.66(15) . . ? C132 C131 Ge1 173.8(4) . . ? C131 C132 C133 179.0(5) . . ? C134 C133 C138 118.3(4) . . ? C134 C133 C132 120.8(5) . . ? C138 C133 C132 120.9(4) . . ? C133 C134 C135 121.0(5) . . ? C133 C134 H134 119.5 . . ? C135 C134 H134 119.5 . . ? C136 C135 C134 119.3(6) . . ? C136 C135 H135 120.3 . . ? C134 C135 H135 120.3 . . ? C137 C136 C135 121.4(6) . . ? C137 C136 H136 119.3 . . ? C135 C136 H136 119.3 . . ? C136 C137 C138 119.8(6) . . ? C136 C137 H137 120.1 . . ? C138 C137 H137 120.1 . . ? C137 C138 C133 120.1(5) . . ? C137 C138 H138 119.9 . . ? C133 C138 H138 119.9 . . ? C142 C141 Ge1 124.9(3) . . ? C142 C141 Al1 110.6(2) . . ? Ge1 C141 Al1 124.21(19) . . ? C141 C142 C143 133.4(3) . . ? C141 C142 H142 113.3 . . ? C143 C142 H142 113.3 . . ? C144 C143 C148 118.5(4) . . ? C144 C143 C142 118.1(4) . . ? C148 C143 C142 123.4(4) . . ? C143 C144 C145 121.4(5) . . ? C143 C144 H144 119.3 . . ? C145 C144 H144 119.3 . . ? C146 C145 C144 119.3(6) . . ? C146 C145 H145 120.3 . . ? C144 C145 H145 120.3 . . ? C147 C146 C145 120.3(5) . . ? C147 C146 H146 119.9 . . ? C145 C146 H146 119.9 . . ? C146 C147 C148 120.6(5) . . ? C146 C147 H147 119.7 . . ? C148 C147 H147 119.7 . . ? C147 C148 C143 119.9(5) . . ? C147 C148 H148 120.1 . . ? C143 C148 H148 120.1 . . ? C152 C151 C156 117.9(4) . . ? C152 C151 Ge1 121.3(3) . . ? C156 C151 Ge1 120.7(3) . . ? C153 C152 C151 120.8(5) . . ? C153 C152 H152 119.6 . . ? C151 C152 H152 119.6 . . ? C154 C153 C152 121.1(6) . . ? C154 C153 H153 119.4 . . ? C152 C153 H153 119.4 . . ? C155 C154 C153 119.4(6) . . ? C155 C154 H154 120.3 . . ? C153 C154 H154 120.3 . . ? C154 C155 C156 120.2(6) . . ? C154 C155 H155 119.9 . . ? C156 C155 H155 119.9 . . ? C151 C156 C155 120.5(5) . . ? C151 C156 H156 119.7 . . ? C155 C156 H156 119.7 . . ? C166 C161 C162 117.4(4) . . ? C166 C161 Ge1 120.6(3) . . ? C162 C161 Ge1 122.0(4) . . ? C163 C162 C161 121.5(5) . . ? C163 C162 H162 119.2 . . ? C161 C162 H162 119.2 . . ? C164 C163 C162 119.4(5) . . ? C164 C163 H163 120.3 . . ? C162 C163 H163 120.3 . . ? C163 C164 C165 121.0(5) . . ? C163 C164 H164 119.5 . . ? C165 C164 H164 119.5 . . ? C164 C165 C166 119.1(6) . . ? C164 C165 H165 120.5 . . ? C166 C165 H165 120.5 . . ? C161 C166 C165 121.6(4) . . ? C161 C166 H166 119.2 . . ? C165 C166 H166 119.2 . . ? C2 Al1 C1 122.42(15) . . ? C2 Al1 C141 118.83(15) . . ? C1 Al1 C141 118.75(15) . . ? Si11 C1 Si12 117.24(19) . . ? Si11 C1 Al1 121.0(2) . . ? Si12 C1 Al1 111.71(18) . . ? Si11 C1 H1 100.7 . . ? Si12 C1 H1 100.7 . . ? Al1 C1 H1 100.7 . . ? C113 Si11 C112 107.7(3) . . ? C113 Si11 C1 109.6(2) . . ? C112 Si11 C1 114.2(2) . . ? C113 Si11 C111 106.1(3) . . ? C112 Si11 C111 107.3(3) . . ? C1 Si11 C111 111.5(2) . . ? Si11 C111 H11A 109.5 . . ? Si11 C111 H11B 109.5 . . ? H11A C111 H11B 109.5 . . ? Si11 C111 H11C 109.5 . . ? H11A C111 H11C 109.5 . . ? H11B C111 H11C 109.5 . . ? Si11 C112 H11D 109.5 . . ? Si11 C112 H11E 109.5 . . ? H11D C112 H11E 109.5 . . ? Si11 C112 H11F 109.5 . . ? H11D C112 H11F 109.5 . . ? H11E C112 H11F 109.5 . . ? Si11 C113 H11G 109.5 . . ? Si11 C113 H11H 109.5 . . ? H11G C113 H11H 109.5 . . ? Si11 C113 H11I 109.5 . . ? H11G C113 H11I 109.5 . . ? H11H C113 H11I 109.5 . . ? C121 Si12 C123 109.4(3) . . ? C121 Si12 C122 105.1(3) . . ? C123 Si12 C122 106.1(3) . . ? C121 Si12 C1 113.1(2) . . ? C123 Si12 C1 110.2(2) . . ? C122 Si12 C1 112.6(2) . . ? Si12 C121 H12A 109.5 . . ? Si12 C121 H12B 109.5 . . ? H12A C121 H12B 109.5 . . ? Si12 C121 H12C 109.5 . . ? H12A C121 H12C 109.5 . . ? H12B C121 H12C 109.5 . . ? Si12 C122 H12D 109.5 . . ? Si12 C122 H12E 109.5 . . ? H12D C122 H12E 109.5 . . ? Si12 C122 H12F 109.5 . . ? H12D C122 H12F 109.5 . . ? H12E C122 H12F 109.5 . . ? Si12 C123 H12G 109.5 . . ? Si12 C123 H12H 109.5 . . ? H12G C123 H12H 109.5 . . ? Si12 C123 H12I 109.5 . . ? H12G C123 H12I 109.5 . . ? H12H C123 H12I 109.5 . . ? Si22 C2 Si21 117.2(2) . . ? Si22 C2 Al1 117.3(2) . . ? Si21 C2 Al1 112.8(2) . . ? Si22 C2 H2 102.0 . . ? Si21 C2 H2 102.0 . . ? Al1 C2 H2 102.0 . . ? C212 Si21 C213 106.9(3) . . ? C212 Si21 C211 106.6(3) . . ? C213 Si21 C211 107.8(3) . . ? C212 Si21 C2 111.0(2) . . ? C213 Si21 C2 113.7(2) . . ? C211 Si21 C2 110.5(3) . . ? Si21 C211 H21A 109.5 . . ? Si21 C211 H21B 109.5 . . ? H21A C211 H21B 109.5 . . ? Si21 C211 H21C 109.5 . . ? H21A C211 H21C 109.5 . . ? H21B C211 H21C 109.5 . . ? Si21 C212 H21D 109.5 . . ? Si21 C212 H21E 109.5 . . ? H21D C212 H21E 109.5 . . ? Si21 C212 H21F 109.5 . . ? H21D C212 H21F 109.5 . . ? H21E C212 H21F 109.5 . . ? Si21 C213 H21G 109.5 . . ? Si21 C213 H21H 109.5 . . ? H21G C213 H21H 109.5 . . ? Si21 C213 H21I 109.5 . . ? H21G C213 H21I 109.5 . . ? H21H C213 H21I 109.5 . . ? C221 Si22 C2 114.8(2) . . ? C221 Si22 C222 104.4(4) . . ? C2 Si22 C222 110.0(3) . . ? C221 Si22 C223 107.2(4) . . ? C2 Si22 C223 111.5(3) . . ? C222 Si22 C223 108.6(5) . . ? Si22 C221 H22A 109.5 . . ? Si22 C221 H22B 109.5 . . ? H22A C221 H22B 109.5 . . ? Si22 C221 H22C 109.5 . . ? H22A C221 H22C 109.5 . . ? H22B C221 H22C 109.5 . . ? Si22 C222 H22D 109.5 . . ? Si22 C222 H22E 109.5 . . ? H22D C222 H22E 109.5 . . ? Si22 C222 H22F 109.5 . . ? H22D C222 H22F 109.5 . . ? H22E C222 H22F 109.5 . . ? Si22 C223 H22G 109.5 . . ? Si22 C223 H22H 109.5 . . ? H22G C223 H22H 109.5 . . ? Si22 C223 H22I 109.5 . . ? H22G C223 H22I 109.5 . . ? H22H C223 H22I 109.5 . . ? C231 Ge2 C261 107.05(19) . . ? C231 Ge2 C251 105.0(2) . . ? C261 Ge2 C251 109.9(2) . . ? C231 Ge2 C241 113.0(2) . . ? C261 Ge2 C241 114.44(18) . . ? C251 Ge2 C241 107.07(17) . . ? C232 C231 Ge2 174.9(6) . . ? C231 C232 C233 177.7(6) . . ? C234 C233 C238 118.2(6) . . ? C234 C233 C232 122.7(6) . . ? C238 C233 C232 119.0(6) . . ? C233 C234 C235 123.9(9) . . ? C233 C234 H234 118.1 . . ? C235 C234 H234 118.1 . . ? C236 C235 C234 118.4(9) . . ? C236 C235 H235 120.8 . . ? C234 C235 H235 120.8 . . ? C235 C236 C237 121.6(8) . . ? C235 C236 H236 119.2 . . ? C237 C236 H236 119.2 . . ? C236 C237 C238 120.3(10) . . ? C236 C237 H237 119.9 . . ? C238 C237 H237 119.9 . . ? C233 C238 C237 117.2(9) . . ? C233 C238 H238 121.4 . . ? C237 C238 H238 121.4 . . ? C242 C241 Ge2 123.5(3) . . ? C242 C241 Al2 114.2(3) . . ? Ge2 C241 Al2 122.3(2) . . ? C241 C242 C243 139.8(9) . . ? C241 C242 C24A 124.6(6) . . ? C243 C242 C24A 23.5(5) . . ? C241 C242 H242 110.1 . . ? C243 C242 H242 110.1 . . ? C24A C242 H242 120.5 . . ? C244 C243 C248 119.4(12) . . ? C244 C243 C242 128.2(11) . . ? C248 C243 C242 112.4(11) . . ? C243 C244 C245 122.0(13) . . ? C243 C244 H244 119.0 . . ? C245 C244 H244 119.0 . . ? C246 C245 C244 116.8(14) . . ? C246 C245 H245 121.6 . . ? C244 C245 H245 121.6 . . ? C247 C246 C245 122.2(16) . . ? C247 C246 H246 118.9 . . ? C245 C246 H246 118.9 . . ? C246 C247 C248 120.6(15) . . ? C246 C247 H247 119.7 . . ? C248 C247 H247 119.7 . . ? C247 C248 C243 118.6(14) . . ? C247 C248 H248 120.7 . . ? C243 C248 H248 120.7 . . ? C24B C24A C24F 119.5(9) . . ? C24B C24A C242 114.3(10) . . ? C24F C24A C242 126.1(8) . . ? C24A C24B C24C 120.8(11) . . ? C24A C24B H24B 119.6 . . ? C24C C24B H24B 119.6 . . ? C24D C24C C24B 118.0(12) . . ? C24D C24C H24C 121.0 . . ? C24B C24C H24C 121.0 . . ? C24E C24D C24C 122.8(12) . . ? C24E C24D H24D 118.6 . . ? C24C C24D H24D 118.6 . . ? C24D C24E C24F 119.2(11) . . ? C24D C24E H24E 120.4 . . ? C24F C24E H24E 120.4 . . ? C24E C24F C24A 119.5(10) . . ? C24E C24F H24F 120.3 . . ? C24A C24F H24F 120.3 . . ? C252 C251 C256 117.5(5) . . ? C252 C251 Ge2 122.2(4) . . ? C256 C251 Ge2 120.3(4) . . ? C251 C252 C253 120.7(6) . . ? C251 C252 H252 119.7 . . ? C253 C252 H252 119.7 . . ? C254 C253 C252 119.5(7) . . ? C254 C253 H253 120.2 . . ? C252 C253 H253 120.2 . . ? C253 C254 C255 121.9(6) . . ? C253 C254 H254 119.1 . . ? C255 C254 H254 119.1 . . ? C256 C255 C254 117.5(7) . . ? C256 C255 H255 121.2 . . ? C254 C255 H255 121.2 . . ? C255 C256 C251 122.9(6) . . ? C255 C256 H256 118.6 . . ? C251 C256 H256 118.6 . . ? C266 C261 C262 117.4(4) . . ? C266 C261 Ge2 120.9(4) . . ? C262 C261 Ge2 121.7(3) . . ? C263 C262 C261 120.2(5) . . ? C263 C262 H262 119.9 . . ? C261 C262 H262 119.9 . . ? C264 C263 C262 121.0(6) . . ? C264 C263 H263 119.5 . . ? C262 C263 H263 119.5 . . ? C263 C264 C265 118.9(5) . . ? C263 C264 H264 120.5 . . ? C265 C264 H264 120.5 . . ? C264 C265 C266 120.3(5) . . ? C264 C265 H265 119.9 . . ? C266 C265 H265 119.9 . . ? C261 C266 C265 122.0(5) . . ? C261 C266 H266 119.0 . . ? C265 C266 H266 119.0 . . ? C3 Al2 C4 123.37(17) . . ? C3 Al2 C241 118.52(17) . . ? C4 Al2 C241 118.09(17) . . ? Si32 C3 Si31 116.2(2) . . ? Si32 C3 Al2 114.8(2) . . ? Si31 C3 Al2 116.9(2) . . ? Si32 C3 H3 101.7 . . ? Si31 C3 H3 101.7 . . ? Al2 C3 H3 101.7 . . ? C312 Si31 C313 108.8(3) . . ? C312 Si31 C3 112.5(2) . . ? C313 Si31 C3 111.7(2) . . ? C312 Si31 C311 106.9(4) . . ? C313 Si31 C311 105.2(3) . . ? C3 Si31 C311 111.5(2) . . ? Si31 C311 H31A 109.5 . . ? Si31 C311 H31B 109.5 . . ? H31A C311 H31B 109.5 . . ? Si31 C311 H31C 109.5 . . ? H31A C311 H31C 109.5 . . ? H31B C311 H31C 109.5 . . ? Si31 C312 H31D 109.5 . . ? Si31 C312 H31E 109.5 . . ? H31D C312 H31E 109.5 . . ? Si31 C312 H31F 109.5 . . ? H31D C312 H31F 109.5 . . ? H31E C312 H31F 109.5 . . ? Si31 C313 H31G 109.5 . . ? Si31 C313 H31H 109.5 . . ? H31G C313 H31H 109.5 . . ? Si31 C313 H31I 109.5 . . ? H31G C313 H31I 109.5 . . ? H31H C313 H31I 109.5 . . ? C323 Si32 C321 107.4(3) . . ? C323 Si32 C322 106.3(3) . . ? C321 Si32 C322 108.2(3) . . ? C323 Si32 C3 111.7(2) . . ? C321 Si32 C3 113.6(2) . . ? C322 Si32 C3 109.3(2) . . ? Si32 C321 H32A 109.5 . . ? Si32 C321 H32B 109.5 . . ? H32A C321 H32B 109.5 . . ? Si32 C321 H32C 109.5 . . ? H32A C321 H32C 109.5 . . ? H32B C321 H32C 109.5 . . ? Si32 C322 H32D 109.5 . . ? Si32 C322 H32E 109.5 . . ? H32D C322 H32E 109.5 . . ? Si32 C322 H32F 109.5 . . ? H32D C322 H32F 109.5 . . ? H32E C322 H32F 109.5 . . ? Si32 C323 H32G 109.5 . . ? Si32 C323 H32H 109.5 . . ? H32G C323 H32H 109.5 . . ? Si32 C323 H32I 109.5 . . ? H32G C323 H32I 109.5 . . ? H32H C323 H32I 109.5 . . ? Si42 C4 Si41 116.1(2) . . ? Si42 C4 Al2 117.4(2) . . ? Si41 C4 Al2 116.49(19) . . ? Si42 C4 H4 100.7 . . ? Si41 C4 H4 100.7 . . ? Al2 C4 H4 100.7 . . ? C412 Si41 C411 107.8(3) . . ? C412 Si41 C413 105.7(3) . . ? C411 Si41 C413 107.8(3) . . ? C412 Si41 C4 111.3(2) . . ? C411 Si41 C4 112.3(2) . . ? C413 Si41 C4 111.6(2) . . ? Si41 C411 H41A 109.5 . . ? Si41 C411 H41B 109.5 . . ? H41A C411 H41B 109.5 . . ? Si41 C411 H41C 109.5 . . ? H41A C411 H41C 109.5 . . ? H41B C411 H41C 109.5 . . ? Si41 C412 H41D 109.5 . . ? Si41 C412 H41E 109.5 . . ? H41D C412 H41E 109.5 . . ? Si41 C412 H41F 109.5 . . ? H41D C412 H41F 109.5 . . ? H41E C412 H41F 109.5 . . ? Si41 C413 H41G 109.5 . . ? Si41 C413 H41H 109.5 . . ? H41G C413 H41H 109.5 . . ? Si41 C413 H41I 109.5 . . ? H41G C413 H41I 109.5 . . ? H41H C413 H41I 109.5 . . ? C422 Si42 C4 113.6(2) . . ? C422 Si42 C421 105.5(3) . . ? C4 Si42 C421 113.8(2) . . ? C422 Si42 C423 108.8(3) . . ? C4 Si42 C423 109.2(3) . . ? C421 Si42 C423 105.6(3) . . ? Si42 C421 H42A 109.5 . . ? Si42 C421 H42B 109.5 . . ? H42A C421 H42B 109.5 . . ? Si42 C421 H42C 109.5 . . ? H42A C421 H42C 109.5 . . ? H42B C421 H42C 109.5 . . ? Si42 C422 H42D 109.5 . . ? Si42 C422 H42E 109.5 . . ? H42D C422 H42E 109.5 . . ? Si42 C422 H42F 109.5 . . ? H42D C422 H42F 109.5 . . ? H42E C422 H42F 109.5 . . ? Si42 C423 H42G 109.5 . . ? Si42 C423 H42H 109.5 . . ? H42G C423 H42H 109.5 . . ? Si42 C423 H42I 109.5 . . ? H42G C423 H42I 109.5 . . ? H42H C423 H42I 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 C161 Ge1 C131 C132 -111(4) . . . . ? C151 Ge1 C131 C132 134(4) . . . . ? C141 Ge1 C131 C132 12(4) . . . . ? Ge1 C131 C132 C133 119(27) . . . . ? C131 C132 C133 C134 -37(29) . . . . ? C131 C132 C133 C138 144(29) . . . . ? C138 C133 C134 C135 -1.0(9) . . . . ? C132 C133 C134 C135 179.6(6) . . . . ? C133 C134 C135 C136 0.0(11) . . . . ? C134 C135 C136 C137 1.7(13) . . . . ? C135 C136 C137 C138 -2.2(12) . . . . ? C136 C137 C138 C133 1.1(10) . . . . ? C134 C133 C138 C137 0.5(8) . . . . ? C132 C133 C138 C137 179.9(5) . . . . ? C131 Ge1 C141 C142 -79.1(4) . . . . ? C161 Ge1 C141 C142 40.8(4) . . . . ? C151 Ge1 C141 C142 163.8(3) . . . . ? C131 Ge1 C141 Al1 94.5(3) . . . . ? C161 Ge1 C141 Al1 -145.7(2) . . . . ? C151 Ge1 C141 Al1 -22.7(3) . . . . ? Ge1 C141 C142 C143 5.4(6) . . . . ? Al1 C141 C142 C143 -168.9(4) . . . . ? C141 C142 C143 C144 -161.1(5) . . . . ? C141 C142 C143 C148 22.4(7) . . . . ? C148 C143 C144 C145 -2.7(7) . . . . ? C142 C143 C144 C145 -179.3(5) . . . . ? C143 C144 C145 C146 0.4(9) . . . . ? C144 C145 C146 C147 0.5(11) . . . . ? C145 C146 C147 C148 0.9(10) . . . . ? C146 C147 C148 C143 -3.2(8) . . . . ? C144 C143 C148 C147 4.0(7) . . . . ? C142 C143 C148 C147 -179.6(4) . . . . ? C131 Ge1 C151 C152 0.9(4) . . . . ? C161 Ge1 C151 C152 -113.3(4) . . . . ? C141 Ge1 C151 C152 121.6(4) . . . . ? C131 Ge1 C151 C156 178.3(3) . . . . ? C161 Ge1 C151 C156 64.1(4) . . . . ? C141 Ge1 C151 C156 -61.0(4) . . . . ? C156 C151 C152 C153 0.4(7) . . . . ? Ge1 C151 C152 C153 177.9(4) . . . . ? C151 C152 C153 C154 0.3(9) . . . . ? C152 C153 C154 C155 -1.3(10) . . . . ? C153 C154 C155 C156 1.5(10) . . . . ? C152 C151 C156 C155 -0.2(7) . . . . ? Ge1 C151 C156 C155 -177.7(4) . . . . ? C154 C155 C156 C151 -0.7(8) . . . . ? C131 Ge1 C161 C166 163.6(4) . . . . ? C151 Ge1 C161 C166 -83.7(4) . . . . ? C141 Ge1 C161 C166 41.6(4) . . . . ? C131 Ge1 C161 C162 -16.1(4) . . . . ? C151 Ge1 C161 C162 96.6(4) . . . . ? C141 Ge1 C161 C162 -138.1(4) . . . . ? C166 C161 C162 C163 -1.4(7) . . . . ? Ge1 C161 C162 C163 178.3(4) . . . . ? C161 C162 C163 C164 1.2(9) . . . . ? C162 C163 C164 C165 -0.5(10) . . . . ? C163 C164 C165 C166 -0.1(9) . . . . ? C162 C161 C166 C165 0.8(7) . . . . ? Ge1 C161 C166 C165 -178.9(4) . . . . ? C164 C165 C166 C161 -0.1(8) . . . . ? C142 C141 Al1 C2 151.9(3) . . . . ? Ge1 C141 Al1 C2 -22.4(3) . . . . ? C142 C141 Al1 C1 -27.2(3) . . . . ? Ge1 C141 Al1 C1 158.5(2) . . . . ? C2 Al1 C1 Si11 -93.3(3) . . . . ? C141 Al1 C1 Si11 85.8(2) . . . . ? C2 Al1 C1 Si12 122.2(2) . . . . ? C141 Al1 C1 Si12 -58.7(2) . . . . ? Si12 C1 Si11 C113 -156.6(3) . . . . ? Al1 C1 Si11 C113 60.8(3) . . . . ? Si12 C1 Si11 C112 82.4(3) . . . . ? Al1 C1 Si11 C112 -60.1(3) . . . . ? Si12 C1 Si11 C111 -39.4(3) . . . . ? Al1 C1 Si11 C111 178.0(2) . . . . ? Si11 C1 Si12 C121 -41.2(3) . . . . ? Al1 C1 Si12 C121 104.7(3) . . . . ? Si11 C1 Si12 C123 81.7(3) . . . . ? Al1 C1 Si12 C123 -132.4(3) . . . . ? Si11 C1 Si12 C122 -160.1(2) . . . . ? Al1 C1 Si12 C122 -14.2(3) . . . . ? C1 Al1 C2 Si22 -37.6(3) . . . . ? C141 Al1 C2 Si22 143.3(2) . . . . ? C1 Al1 C2 Si21 103.3(2) . . . . ? C141 Al1 C2 Si21 -75.8(2) . . . . ? Si22 C2 Si21 C212 154.3(3) . . . . ? Al1 C2 Si21 C212 13.3(3) . . . . ? Si22 C2 Si21 C213 33.7(3) . . . . ? Al1 C2 Si21 C213 -107.3(3) . . . . ? Si22 C2 Si21 C211 -87.7(3) . . . . ? Al1 C2 Si21 C211 131.4(3) . . . . ? Si21 C2 Si22 C221 -71.6(3) . . . . ? Al1 C2 Si22 C221 67.5(3) . . . . ? Si21 C2 Si22 C222 171.0(4) . . . . ? Al1 C2 Si22 C222 -49.8(4) . . . . ? Si21 C2 Si22 C223 50.5(5) . . . . ? Al1 C2 Si22 C223 -170.4(4) . . . . ? C261 Ge2 C231 C232 79(5) . . . . ? C251 Ge2 C231 C232 -164(5) . . . . ? C241 Ge2 C231 C232 -48(5) . . . . ? Ge2 C231 C232 C233 -53(22) . . . . ? C231 C232 C233 C234 -71(19) . . . . ? C231 C232 C233 C238 113(19) . . . . ? C238 C233 C234 C235 -6.2(14) . . . . ? C232 C233 C234 C235 177.2(8) . . . . ? C233 C234 C235 C236 2.1(16) . . . . ? C234 C235 C236 C237 2.3(17) . . . . ? C235 C236 C237 C238 -2.4(17) . . . . ? C234 C233 C238 C237 5.8(12) . . . . ? C232 C233 C238 C237 -177.5(7) . . . . ? C236 C237 C238 C233 -1.8(15) . . . . ? C231 Ge2 C241 C242 85.8(4) . . . . ? C261 Ge2 C241 C242 -37.1(4) . . . . ? C251 Ge2 C241 C242 -159.1(4) . . . . ? C231 Ge2 C241 Al2 -95.8(3) . . . . ? C261 Ge2 C241 Al2 141.3(2) . . . . ? C251 Ge2 C241 Al2 19.3(3) . . . . ? Ge2 C241 C242 C243 10.3(14) . . . . ? Al2 C241 C242 C243 -168.2(12) . . . . ? Ge2 C241 C242 C24A -14.2(9) . . . . ? Al2 C241 C242 C24A 167.3(7) . . . . ? C241 C242 C243 C244 128.8(17) . . . . ? C24A C242 C243 C244 -172(4) . . . . ? C241 C242 C243 C248 -52(2) . . . . ? C24A C242 C243 C248 6.6(17) . . . . ? C248 C243 C244 C245 5(3) . . . . ? C242 C243 C244 C245 -176.2(15) . . . . ? C243 C244 C245 C246 -2(3) . . . . ? C244 C245 C246 C247 -3(4) . . . . ? C245 C246 C247 C248 6(4) . . . . ? C246 C247 C248 C243 -3(3) . . . . ? C244 C243 C248 C247 -2(3) . . . . ? C242 C243 C248 C247 178.8(14) . . . . ? C241 C242 C24A C24B 151.7(10) . . . . ? C243 C242 C24A C24B 14(2) . . . . ? C241 C242 C24A C24F -25.5(16) . . . . ? C243 C242 C24A C24F -163(4) . . . . ? C24F C24A C24B C24C 0(2) . . . . ? C242 C24A C24B C24C -177.0(13) . . . . ? C24A C24B C24C C24D 4(3) . . . . ? C24B C24C C24D C24E -5(3) . . . . ? C24C C24D C24E C24F 2(2) . . . . ? C24D C24E C24F C24A 2(2) . . . . ? C24B C24A C24F C24E -4(2) . . . . ? C242 C24A C24F C24E 173.5(11) . . . . ? C231 Ge2 C251 C252 19.3(4) . . . . ? C261 Ge2 C251 C252 134.1(4) . . . . ? C241 Ge2 C251 C252 -101.1(4) . . . . ? C231 Ge2 C251 C256 -159.6(4) . . . . ? C261 Ge2 C251 C256 -44.8(4) . . . . ? C241 Ge2 C251 C256 80.1(4) . . . . ? C256 C251 C252 C253 -0.5(7) . . . . ? Ge2 C251 C252 C253 -179.5(4) . . . . ? C251 C252 C253 C254 -0.3(8) . . . . ? C252 C253 C254 C255 1.3(10) . . . . ? C253 C254 C255 C256 -1.4(10) . . . . ? C254 C255 C256 C251 0.6(9) . . . . ? C252 C251 C256 C255 0.4(7) . . . . ? Ge2 C251 C256 C255 179.3(4) . . . . ? C231 Ge2 C261 C266 32.5(5) . . . . ? C251 Ge2 C261 C266 -80.9(5) . . . . ? C241 Ge2 C261 C266 158.6(4) . . . . ? C231 Ge2 C261 C262 -145.3(4) . . . . ? C251 Ge2 C261 C262 101.3(4) . . . . ? C241 Ge2 C261 C262 -19.2(4) . . . . ? C266 C261 C262 C263 -0.6(8) . . . . ? Ge2 C261 C262 C263 177.3(4) . . . . ? C261 C262 C263 C264 0.3(9) . . . . ? C262 C263 C264 C265 2.6(10) . . . . ? C263 C264 C265 C266 -5.1(10) . . . . ? C262 C261 C266 C265 -2.0(9) . . . . ? Ge2 C261 C266 C265 -179.9(5) . . . . ? C264 C265 C266 C261 4.9(10) . . . . ? C242 C241 Al2 C3 46.0(4) . . . . ? Ge2 C241 Al2 C3 -132.6(2) . . . . ? C242 C241 Al2 C4 -132.8(3) . . . . ? Ge2 C241 Al2 C4 48.7(3) . . . . ? C4 Al2 C3 Si32 92.6(3) . . . . ? C241 Al2 C3 Si32 -86.0(3) . . . . ? C4 Al2 C3 Si31 -126.1(2) . . . . ? C241 Al2 C3 Si31 55.2(3) . . . . ? Si32 C3 Si31 C312 77.3(4) . . . . ? Al2 C3 Si31 C312 -63.4(4) . . . . ? Si32 C3 Si31 C313 -45.4(3) . . . . ? Al2 C3 Si31 C313 173.9(3) . . . . ? Si32 C3 Si31 C311 -162.7(3) . . . . ? Al2 C3 Si31 C311 56.6(3) . . . . ? Si31 C3 Si32 C323 78.2(3) . . . . ? Al2 C3 Si32 C323 -140.3(3) . . . . ? Si31 C3 Si32 C321 -43.5(4) . . . . ? Al2 C3 Si32 C321 98.0(3) . . . . ? Si31 C3 Si32 C322 -164.5(3) . . . . ? Al2 C3 Si32 C322 -22.9(3) . . . . ? C3 Al2 C4 Si42 -119.6(2) . . . . ? C241 Al2 C4 Si42 59.1(3) . . . . ? C3 Al2 C4 Si41 24.7(3) . . . . ? C241 Al2 C4 Si41 -156.7(2) . . . . ? Si42 C4 Si41 C412 -166.9(3) . . . . ? Al2 C4 Si41 C412 48.4(3) . . . . ? Si42 C4 Si41 C411 72.1(3) . . . . ? Al2 C4 Si41 C411 -72.6(3) . . . . ? Si42 C4 Si41 C413 -49.1(4) . . . . ? Al2 C4 Si41 C413 166.2(3) . . . . ? Si41 C4 Si42 C422 -36.4(4) . . . . ? Al2 C4 Si42 C422 108.0(4) . . . . ? Si41 C4 Si42 C421 -157.1(3) . . . . ? Al2 C4 Si42 C421 -12.7(3) . . . . ? Si41 C4 Si42 C423 85.2(3) . . . . ? Al2 C4 Si42 C423 -130.4(3) . . . . ? _diffrn_measured_fraction_theta_max 0.858 _diffrn_reflns_theta_full 72.58 _diffrn_measured_fraction_theta_full 0.858 _refine_diff_density_max 0.733 _refine_diff_density_min -0.943 _refine_diff_density_rms 0.096 # Attachment '- cifcompound3.txt' data_sad_3 _database_code_depnum_ccdc_archive 'CCDC 762760' #TrackingRef '- cifcompound3.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C26 H35 Al Ge' _chemical_formula_weight 447.11 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M P2(1)2(1)2(1) loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.0026(2) _cell_length_b 13.7703(2) _cell_length_c 33.8233(5) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 5124.54(14) _cell_formula_units_Z 8 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 7146 _cell_measurement_theta_min 2.613 _cell_measurement_theta_max 72.236 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.53 _exptl_crystal_size_mid 0.46 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.159 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1888 _exptl_absorpt_coefficient_mu 1.994 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.4180 _exptl_absorpt_correction_T_max 0.7959 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 30930 _diffrn_reflns_av_R_equivalents 0.0275 _diffrn_reflns_av_sigmaI/netI 0.0265 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 12 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 40 _diffrn_reflns_theta_min 2.61 _diffrn_reflns_theta_max 72.67 _reflns_number_total 9639 _reflns_number_gt 9423 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT+' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0462P)^2^+0.1500P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.007(12) _refine_ls_number_reflns 9639 _refine_ls_number_parameters 521 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0269 _refine_ls_R_factor_gt 0.0261 _refine_ls_wR_factor_ref 0.0686 _refine_ls_wR_factor_gt 0.0681 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _refine_ls_shift/su_max 0.012 _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 0.34596(2) 0.848773(14) 0.032818(6) 0.03293(6) Uani 1 1 d . . . Al1 Al 0.42988(5) 1.05460(4) 0.047344(16) 0.02913(11) Uani 1 1 d . . . C111 C 0.29069(16) 0.96719(12) 0.05807(6) 0.0300(4) Uani 1 1 d . . . C112 C 0.18706(17) 0.98610(14) 0.07651(6) 0.0340(4) Uani 1 1 d . . . H112 H 0.1787 1.0524 0.0848 0.041 Uiso 1 1 calc R . . C113 C 0.08173(17) 0.92383(15) 0.08668(6) 0.0359(4) Uani 1 1 d . . . C114 C 0.0782(2) 0.82367(17) 0.08109(8) 0.0500(6) Uani 1 1 d . . . H114 H 0.1464 0.7916 0.0691 0.060 Uiso 1 1 calc R . . C115 C -0.0214(2) 0.7697(2) 0.09248(9) 0.0609(7) Uani 1 1 d . . . H115 H -0.0221 0.7008 0.0883 0.073 Uiso 1 1 calc R . . C116 C -0.1201(2) 0.8143(2) 0.10981(7) 0.0578(7) Uani 1 1 d . . . H116 H -0.1891 0.7766 0.1179 0.069 Uiso 1 1 calc R . . C117 C -0.1190(2) 0.9126(2) 0.11534(7) 0.0551(7) Uani 1 1 d . . . H117 H -0.1880 0.9440 0.1271 0.066 Uiso 1 1 calc R . . C118 C -0.01933(18) 0.96730(19) 0.10409(6) 0.0442(5) Uani 1 1 d . . . H118 H -0.0198 1.0362 0.1083 0.053 Uiso 1 1 calc R . . C121 C 0.49838(19) 0.90731(14) 0.01333(6) 0.0371(4) Uani 1 1 d . . . C122 C 0.59415(17) 0.93627(13) 0.00110(5) 0.0331(4) Uani 1 1 d . . . C123 C 0.70884(17) 0.96691(13) -0.01535(5) 0.0305(4) Uani 1 1 d . . . C124 C 0.81523(18) 0.96293(14) 0.00667(6) 0.0363(4) Uani 1 1 d . . . H124 H 0.8130 0.9411 0.0336 0.044 Uiso 1 1 calc R . . C125 C 0.9249(2) 0.99063(16) -0.01031(7) 0.0427(5) Uani 1 1 d . . . H125 H 0.9984 0.9881 0.0049 0.051 Uiso 1 1 calc R . . C126 C 0.9280(2) 1.02175(15) -0.04894(7) 0.0423(5) Uani 1 1 d . . . H126 H 1.0039 1.0406 -0.0606 0.051 Uiso 1 1 calc R . . C127 C 0.8227(2) 1.02600(15) -0.07099(6) 0.0419(5) Uani 1 1 d . . . H127 H 0.8256 1.0477 -0.0979 0.050 Uiso 1 1 calc R . . C128 C 0.71336(19) 0.99916(14) -0.05442(6) 0.0368(4) Uani 1 1 d . . . H128 H 0.6401 1.0027 -0.0698 0.044 Uiso 1 1 calc R . . C131 C 0.2545(3) 0.80846(17) -0.01355(7) 0.0527(6) Uani 1 1 d . . . H13A H 0.1786 0.7804 -0.0054 0.063 Uiso 1 1 calc R . . H13B H 0.3005 0.7612 -0.0281 0.063 Uiso 1 1 calc R . . H13C H 0.2391 0.8638 -0.0301 0.063 Uiso 1 1 calc R . . C141 C 0.3984(2) 0.74208(15) 0.06654(8) 0.0495(5) Uani 1 1 d . . . H14A H 0.4290 0.7675 0.0910 0.059 Uiso 1 1 calc R . . H14B H 0.4613 0.7060 0.0535 0.059 Uiso 1 1 calc R . . H14C H 0.3306 0.7001 0.0718 0.059 Uiso 1 1 calc R . . C151 C 0.53547(17) 1.07230(15) 0.09472(6) 0.0369(4) Uani 1 1 d . . . C152 C 0.6561(2) 1.12301(17) 0.08745(7) 0.0499(5) Uani 1 1 d . . . H15A H 0.6416 1.1860 0.0762 0.060 Uiso 1 1 calc R . . H15B H 0.7042 1.0851 0.0695 0.060 Uiso 1 1 calc R . . H15C H 0.6988 1.1300 0.1120 0.060 Uiso 1 1 calc R . . C153 C 0.5583(2) 0.97312(17) 0.11443(7) 0.0459(5) Uani 1 1 d . . . H15D H 0.6083 0.9340 0.0975 0.055 Uiso 1 1 calc R . . H15E H 0.4821 0.9409 0.1188 0.055 Uiso 1 1 calc R . . H15F H 0.5988 0.9827 0.1393 0.055 Uiso 1 1 calc R . . C154 C 0.4612(2) 1.1329(2) 0.12428(8) 0.0562(6) Uani 1 1 d . . . H15G H 0.5054 1.1385 0.1486 0.067 Uiso 1 1 calc R . . H15H H 0.3847 1.1016 0.1291 0.067 Uiso 1 1 calc R . . H15I H 0.4472 1.1964 0.1135 0.067 Uiso 1 1 calc R . . C161 C 0.39867(18) 1.15550(15) 0.00683(6) 0.0385(4) Uani 1 1 d . . . C162 C 0.3274(3) 1.11414(19) -0.02778(8) 0.0636(7) Uani 1 1 d . . . H16A H 0.3044 1.1658 -0.0453 0.076 Uiso 1 1 calc R . . H16B H 0.2559 1.0821 -0.0181 0.076 Uiso 1 1 calc R . . H16C H 0.3771 1.0683 -0.0418 0.076 Uiso 1 1 calc R . . C163 C 0.5109(2) 1.20703(19) -0.00919(9) 0.0584(7) Uani 1 1 d . . . H16D H 0.4864 1.2580 -0.0268 0.070 Uiso 1 1 calc R . . H16E H 0.5608 1.1613 -0.0232 0.070 Uiso 1 1 calc R . . H16F H 0.5563 1.2343 0.0124 0.070 Uiso 1 1 calc R . . C164 C 0.3202(2) 1.23109(17) 0.02811(9) 0.0575(6) Uani 1 1 d . . . H16G H 0.3657 1.2593 0.0494 0.069 Uiso 1 1 calc R . . H16H H 0.2487 1.2003 0.0385 0.069 Uiso 1 1 calc R . . H16I H 0.2969 1.2810 0.0098 0.069 Uiso 1 1 calc R . . Ge2 Ge 0.24139(2) 0.555395(15) 0.206270(7) 0.03623(6) Uani 1 1 d . . . Al2 Al 0.17216(4) 0.34433(4) 0.211376(15) 0.02832(11) Uani 1 1 d . . . C211 C 0.30424(16) 0.42932(12) 0.19105(5) 0.0285(4) Uani 1 1 d . . . C212 C 0.40669(16) 0.40253(14) 0.17350(5) 0.0303(4) Uani 1 1 d . . . H212 H 0.4160 0.3335 0.1712 0.036 Uiso 1 1 calc R . . C213 C 0.50945(16) 0.45859(15) 0.15678(5) 0.0316(4) Uani 1 1 d . . . C214 C 0.51326(19) 0.55967(17) 0.15488(6) 0.0428(5) Uani 1 1 d . . . H214 H 0.4473 0.5968 0.1657 0.051 Uiso 1 1 calc R . . C215 C 0.6108(2) 0.6076(2) 0.13758(7) 0.0534(6) Uani 1 1 d . . . H215 H 0.6112 0.6772 0.1361 0.064 Uiso 1 1 calc R . . C216 C 0.7078(2) 0.5549(2) 0.12246(7) 0.0559(6) Uani 1 1 d . . . H216 H 0.7760 0.5879 0.1109 0.067 Uiso 1 1 calc R . . C217 C 0.70558(19) 0.4552(2) 0.12415(7) 0.0526(6) Uani 1 1 d . . . H217 H 0.7721 0.4184 0.1135 0.063 Uiso 1 1 calc R . . C218 C 0.60772(18) 0.40787(18) 0.14109(6) 0.0415(5) Uani 1 1 d . . . H218 H 0.6076 0.3382 0.1421 0.050 Uiso 1 1 calc R . . C221 C 0.09289(18) 0.50017(14) 0.23048(6) 0.0369(4) Uani 1 1 d . . . C222 C -0.00288(18) 0.47431(13) 0.24397(6) 0.0331(4) Uani 1 1 d . . . C223 C -0.11875(16) 0.44877(14) 0.26060(5) 0.0311(4) Uani 1 1 d . . . C224 C -0.22135(18) 0.44184(16) 0.23660(6) 0.0379(4) Uani 1 1 d . . . H224 H -0.2145 0.4518 0.2086 0.045 Uiso 1 1 calc R . . C225 C -0.33280(19) 0.42057(17) 0.25318(6) 0.0437(5) Uani 1 1 d . . . H225 H -0.4032 0.4154 0.2365 0.052 Uiso 1 1 calc R . . C226 C -0.34417(19) 0.40660(17) 0.29337(7) 0.0439(5) Uani 1 1 d . . . H226 H -0.4221 0.3920 0.3046 0.053 Uiso 1 1 calc R . . C227 C -0.2434(2) 0.41367(18) 0.31728(6) 0.0461(5) Uani 1 1 d . . . H227 H -0.2513 0.4041 0.3453 0.055 Uiso 1 1 calc R . . C228 C -0.13099(18) 0.43445(16) 0.30121(5) 0.0399(4) Uani 1 1 d . . . H228 H -0.0610 0.4391 0.3181 0.048 Uiso 1 1 calc R . . C231 C 0.3257(3) 0.62482(19) 0.24808(8) 0.0613(7) Uani 1 1 d . . . H23A H 0.3518 0.5796 0.2679 0.074 Uiso 1 1 calc R . . H23B H 0.2719 0.6716 0.2597 0.074 Uiso 1 1 calc R . . H23C H 0.3952 0.6575 0.2372 0.074 Uiso 1 1 calc R . . C241 C 0.1823(3) 0.64045(19) 0.16466(8) 0.0599(7) Uani 1 1 d . . . H24A H 0.1363 0.6925 0.1761 0.072 Uiso 1 1 calc R . . H24B H 0.1314 0.6042 0.1470 0.072 Uiso 1 1 calc R . . H24C H 0.2501 0.6667 0.1503 0.072 Uiso 1 1 calc R . . C251 C 0.22102(18) 0.27458(14) 0.26048(6) 0.0370(4) Uani 1 1 d . . . C252 C 0.1167(2) 0.22618(16) 0.28265(7) 0.0461(5) Uani 1 1 d . . . H25A H 0.1483 0.1905 0.3048 0.055 Uiso 1 1 calc R . . H25B H 0.0747 0.1826 0.2652 0.055 Uiso 1 1 calc R . . H25C H 0.0613 0.2750 0.2919 0.055 Uiso 1 1 calc R . . C253 C 0.2867(2) 0.34408(19) 0.28844(7) 0.0523(6) Uani 1 1 d . . . H25D H 0.3178 0.3085 0.3107 0.063 Uiso 1 1 calc R . . H25E H 0.2309 0.3928 0.2975 0.063 Uiso 1 1 calc R . . H25F H 0.3528 0.3746 0.2747 0.063 Uiso 1 1 calc R . . C254 C 0.3107(2) 0.19588(19) 0.24678(8) 0.0581(7) Uani 1 1 d . . . H25G H 0.3795 0.2260 0.2343 0.070 Uiso 1 1 calc R . . H25H H 0.2712 0.1536 0.2282 0.070 Uiso 1 1 calc R . . H25I H 0.3376 0.1589 0.2692 0.070 Uiso 1 1 calc R . . C261 C 0.06443(18) 0.29093(15) 0.16949(6) 0.0368(4) Uani 1 1 d . . . C262 C 0.1433(2) 0.22231(19) 0.14440(8) 0.0584(6) Uani 1 1 d . . . H26A H 0.1693 0.1684 0.1603 0.070 Uiso 1 1 calc R . . H26B H 0.2132 0.2568 0.1348 0.070 Uiso 1 1 calc R . . H26C H 0.0967 0.1988 0.1224 0.070 Uiso 1 1 calc R . . C263 C -0.0467(2) 0.2356(2) 0.18381(8) 0.0573(6) Uani 1 1 d . . . H26D H -0.0976 0.2782 0.1990 0.069 Uiso 1 1 calc R . . H26E H -0.0214 0.1820 0.2000 0.069 Uiso 1 1 calc R . . H26F H -0.0915 0.2117 0.1615 0.069 Uiso 1 1 calc R . . C264 C 0.0240(2) 0.3733(2) 0.14220(7) 0.0547(6) Uani 1 1 d . . . H26G H -0.0191 0.3467 0.1200 0.066 Uiso 1 1 calc R . . H26H H 0.0940 0.4082 0.1330 0.066 Uiso 1 1 calc R . . H26I H -0.0285 0.4166 0.1565 0.066 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 0.03481(12) 0.02534(10) 0.03864(12) -0.00218(8) 0.00932(8) -0.00238(8) Al1 0.0251(2) 0.0246(2) 0.0378(3) -0.0021(2) 0.00247(19) -0.0012(2) C111 0.0290(9) 0.0248(8) 0.0364(9) -0.0024(7) 0.0021(7) -0.0009(6) C112 0.0306(10) 0.0333(9) 0.0379(10) -0.0058(8) 0.0019(7) 0.0000(7) C113 0.0273(9) 0.0507(11) 0.0295(9) 0.0021(8) 0.0000(7) -0.0012(8) C114 0.0362(12) 0.0495(13) 0.0644(15) 0.0083(11) 0.0126(10) -0.0066(9) C115 0.0442(13) 0.0597(15) 0.0787(18) 0.0154(13) 0.0026(12) -0.0151(12) C116 0.0333(12) 0.093(2) 0.0472(13) 0.0192(13) 0.0025(9) -0.0194(12) C117 0.0268(11) 0.099(2) 0.0392(12) 0.0026(12) 0.0047(8) -0.0010(11) C118 0.0284(10) 0.0681(15) 0.0360(10) -0.0044(10) -0.0004(7) 0.0001(9) C121 0.0389(11) 0.0332(9) 0.0392(10) -0.0006(8) 0.0141(8) 0.0020(8) C122 0.0385(10) 0.0281(8) 0.0327(9) -0.0024(7) 0.0065(7) 0.0067(8) C123 0.0349(10) 0.0251(8) 0.0315(9) -0.0012(7) 0.0092(7) 0.0028(7) C124 0.0404(10) 0.0357(10) 0.0327(9) 0.0000(8) 0.0038(7) 0.0004(8) C125 0.0342(11) 0.0442(11) 0.0496(12) -0.0023(9) -0.0012(9) -0.0019(8) C126 0.0354(11) 0.0393(10) 0.0523(12) 0.0001(9) 0.0149(9) -0.0018(8) C127 0.0475(12) 0.0425(11) 0.0357(10) 0.0057(8) 0.0142(8) 0.0034(9) C128 0.0382(11) 0.0370(10) 0.0351(10) 0.0017(8) 0.0031(8) 0.0044(8) C131 0.0688(16) 0.0448(11) 0.0444(12) -0.0091(9) 0.0002(11) -0.0104(12) C141 0.0533(13) 0.0312(10) 0.0641(15) 0.0091(10) 0.0065(11) 0.0040(9) C151 0.0307(10) 0.0404(10) 0.0395(10) -0.0084(8) 0.0026(7) 0.0020(8) C152 0.0408(12) 0.0546(13) 0.0544(13) -0.0103(10) -0.0040(10) -0.0104(10) C153 0.0382(11) 0.0557(13) 0.0438(12) 0.0009(10) -0.0013(9) 0.0015(10) C154 0.0480(13) 0.0686(16) 0.0520(14) -0.0229(12) 0.0028(10) 0.0093(11) C161 0.0365(10) 0.0292(9) 0.0497(11) 0.0061(8) 0.0005(8) -0.0004(8) C162 0.084(2) 0.0484(13) 0.0584(16) 0.0106(11) -0.0241(14) -0.0041(13) C163 0.0494(14) 0.0486(13) 0.0771(18) 0.0207(12) 0.0124(12) 0.0006(11) C164 0.0533(14) 0.0405(11) 0.0786(18) 0.0098(12) 0.0074(12) 0.0162(10) Ge2 0.03413(12) 0.02907(10) 0.04548(13) -0.00344(9) 0.01270(9) -0.00090(9) Al2 0.0251(2) 0.0279(2) 0.0320(3) -0.0001(2) 0.00306(19) -0.0017(2) C211 0.0275(9) 0.0275(8) 0.0305(9) -0.0008(7) 0.0019(6) -0.0016(7) C212 0.0284(9) 0.0315(9) 0.0311(9) -0.0016(7) -0.0011(7) 0.0000(7) C213 0.0234(8) 0.0484(11) 0.0229(8) -0.0033(8) -0.0002(6) -0.0022(8) C214 0.0378(11) 0.0474(11) 0.0432(11) -0.0023(9) 0.0091(8) -0.0107(9) C215 0.0491(14) 0.0619(14) 0.0494(13) -0.0030(11) 0.0064(10) -0.0219(11) C216 0.0333(11) 0.097(2) 0.0379(11) 0.0012(12) 0.0061(8) -0.0227(12) C217 0.0277(10) 0.0915(19) 0.0385(11) -0.0045(12) 0.0045(8) 0.0014(11) C218 0.0281(10) 0.0629(13) 0.0335(10) -0.0040(9) 0.0011(7) 0.0047(9) C221 0.0318(10) 0.0375(10) 0.0415(11) -0.0045(8) 0.0109(8) 0.0017(8) C222 0.0334(10) 0.0303(9) 0.0357(10) -0.0069(7) 0.0021(7) 0.0059(7) C223 0.0292(9) 0.0317(9) 0.0324(9) -0.0030(7) 0.0038(7) 0.0026(7) C224 0.0375(10) 0.0488(11) 0.0274(9) 0.0009(8) 0.0011(7) 0.0002(9) C225 0.0303(10) 0.0615(13) 0.0395(11) -0.0019(9) -0.0037(8) -0.0034(9) C226 0.0312(10) 0.0574(12) 0.0430(11) -0.0007(10) 0.0085(9) -0.0035(9) C227 0.0403(11) 0.0692(14) 0.0289(10) 0.0012(9) 0.0046(8) 0.0019(11) C228 0.0323(10) 0.0585(12) 0.0289(9) -0.0041(9) -0.0013(7) 0.0017(9) C231 0.0579(15) 0.0564(14) 0.0696(17) -0.0297(12) 0.0149(12) -0.0170(12) C241 0.0612(15) 0.0467(13) 0.0717(17) 0.0168(12) 0.0188(12) 0.0179(12) C251 0.0341(10) 0.0390(10) 0.0379(10) 0.0088(8) 0.0029(7) -0.0003(8) C252 0.0470(12) 0.0446(11) 0.0467(12) 0.0104(9) 0.0067(9) -0.0075(9) C253 0.0518(13) 0.0638(14) 0.0413(12) 0.0116(11) -0.0081(9) -0.0150(11) C254 0.0575(15) 0.0591(14) 0.0578(15) 0.0222(12) 0.0104(11) 0.0223(12) C261 0.0302(10) 0.0409(10) 0.0394(10) -0.0126(8) 0.0013(8) 0.0009(8) C262 0.0474(13) 0.0634(15) 0.0644(15) -0.0324(13) 0.0017(11) 0.0073(12) C263 0.0407(12) 0.0614(15) 0.0698(16) -0.0171(13) 0.0009(11) -0.0145(11) C264 0.0513(14) 0.0712(16) 0.0415(12) -0.0055(11) -0.0088(10) 0.0073(11) _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 C111 1.9388(17) . ? Ge1 C131 1.945(2) . ? Ge1 C141 1.947(2) . ? Ge1 C121 1.974(2) . ? Al1 C111 1.9813(18) . ? Al1 C161 1.982(2) . ? Al1 C151 1.994(2) . ? Al1 C121 2.451(2) . ? C111 C112 1.325(3) . ? C112 C113 1.482(3) . ? C112 H112 0.9600 . ? C113 C114 1.393(3) . ? C113 C118 1.393(3) . ? C114 C115 1.379(3) . ? C114 H114 0.9600 . ? C115 C116 1.378(4) . ? C115 H115 0.9600 . ? C116 C117 1.366(4) . ? C116 H116 0.9600 . ? C117 C118 1.384(3) . ? C117 H117 0.9600 . ? C118 H118 0.9600 . ? C121 C122 1.200(3) . ? C122 C123 1.442(3) . ? C123 C124 1.389(3) . ? C123 C128 1.395(3) . ? C124 C125 1.389(3) . ? C124 H124 0.9600 . ? C125 C126 1.376(3) . ? C125 H125 0.9600 . ? C126 C127 1.378(3) . ? C126 H126 0.9600 . ? C127 C128 1.378(3) . ? C127 H127 0.9600 . ? C128 H128 0.9600 . ? C131 H13A 0.9599 . ? C131 H13B 0.9599 . ? C131 H13C 0.9599 . ? C141 H14A 0.9599 . ? C141 H14B 0.9599 . ? C141 H14C 0.9599 . ? C151 C152 1.520(3) . ? C151 C154 1.537(3) . ? C151 C153 1.540(3) . ? C152 H15A 0.9599 . ? C152 H15B 0.9599 . ? C152 H15C 0.9599 . ? C153 H15D 0.9599 . ? C153 H15E 0.9599 . ? C153 H15F 0.9599 . ? C154 H15G 0.9599 . ? C154 H15H 0.9599 . ? C154 H15I 0.9599 . ? C161 C162 1.520(3) . ? C161 C163 1.524(3) . ? C161 C164 1.532(3) . ? C162 H16A 0.9599 . ? C162 H16B 0.9599 . ? C162 H16C 0.9599 . ? C163 H16D 0.9599 . ? C163 H16E 0.9599 . ? C163 H16F 0.9599 . ? C164 H16G 0.9599 . ? C164 H16H 0.9599 . ? C164 H16I 0.9599 . ? Ge2 C211 1.9383(17) . ? Ge2 C231 1.943(2) . ? Ge2 C241 1.943(2) . ? Ge2 C221 1.9795(19) . ? Al2 C261 1.988(2) . ? Al2 C211 1.9886(18) . ? Al2 C251 1.992(2) . ? Al2 C221 2.405(2) . ? C211 C212 1.326(3) . ? C212 C213 1.481(3) . ? C212 H212 0.9600 . ? C213 C218 1.392(3) . ? C213 C214 1.394(3) . ? C214 C215 1.389(3) . ? C214 H214 0.9600 . ? C215 C216 1.388(4) . ? C215 H215 0.9600 . ? C216 C217 1.375(4) . ? C216 H216 0.9600 . ? C217 C218 1.383(3) . ? C217 H217 0.9600 . ? C218 H218 0.9600 . ? C221 C222 1.202(3) . ? C222 C223 1.437(3) . ? C223 C224 1.394(3) . ? C223 C228 1.394(3) . ? C224 C225 1.380(3) . ? C224 H224 0.9600 . ? C225 C226 1.379(3) . ? C225 H225 0.9600 . ? C226 C227 1.376(3) . ? C226 H226 0.9600 . ? C227 C228 1.381(3) . ? C227 H227 0.9600 . ? C228 H228 0.9600 . ? C231 H23A 0.9599 . ? C231 H23B 0.9599 . ? C231 H23C 0.9599 . ? C241 H24A 0.9599 . ? C241 H24B 0.9599 . ? C241 H24C 0.9599 . ? C251 C252 1.525(3) . ? C251 C253 1.527(3) . ? C251 C254 1.537(3) . ? C252 H25A 0.9599 . ? C252 H25B 0.9599 . ? C252 H25C 0.9599 . ? C253 H25D 0.9599 . ? C253 H25E 0.9599 . ? C253 H25F 0.9599 . ? C254 H25G 0.9599 . ? C254 H25H 0.9599 . ? C254 H25I 0.9599 . ? C261 C263 1.520(3) . ? C261 C264 1.529(3) . ? C261 C262 1.538(3) . ? C262 H26A 0.9599 . ? C262 H26B 0.9599 . ? C262 H26C 0.9599 . ? C263 H26D 0.9599 . ? C263 H26E 0.9599 . ? C263 H26F 0.9599 . ? C264 H26G 0.9599 . ? C264 H26H 0.9599 . ? C264 H26I 0.9599 . ? 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 C111 Ge1 C131 115.66(10) . . ? C111 Ge1 C141 118.00(9) . . ? C131 Ge1 C141 114.22(10) . . ? C111 Ge1 C121 94.02(8) . . ? C131 Ge1 C121 106.68(10) . . ? C141 Ge1 C121 104.61(10) . . ? C111 Al1 C161 114.75(8) . . ? C111 Al1 C151 112.17(8) . . ? C161 Al1 C151 124.82(9) . . ? C111 Al1 C121 79.69(7) . . ? C161 Al1 C121 108.00(8) . . ? C151 Al1 C121 107.41(8) . . ? C112 C111 Ge1 129.97(14) . . ? C112 C111 Al1 129.18(14) . . ? Ge1 C111 Al1 100.82(8) . . ? C111 C112 C113 131.93(18) . . ? C111 C112 H112 114.0 . . ? C113 C112 H112 114.0 . . ? C114 C113 C118 117.4(2) . . ? C114 C113 C112 124.27(19) . . ? C118 C113 C112 118.27(19) . . ? C115 C114 C113 121.1(2) . . ? C115 C114 H114 119.4 . . ? C113 C114 H114 119.4 . . ? C116 C115 C114 120.4(3) . . ? C116 C115 H115 119.8 . . ? C114 C115 H115 119.8 . . ? C117 C116 C115 119.5(2) . . ? C117 C116 H116 120.3 . . ? C115 C116 H116 120.3 . . ? C116 C117 C118 120.6(2) . . ? C116 C117 H117 119.7 . . ? C118 C117 H117 119.7 . . ? C117 C118 C113 121.0(2) . . ? C117 C118 H118 119.5 . . ? C113 C118 H118 119.5 . . ? C122 C121 Ge1 175.30(17) . . ? C122 C121 Al1 99.03(14) . . ? Ge1 C121 Al1 85.41(7) . . ? C121 C122 C123 176.7(2) . . ? C124 C123 C128 119.38(18) . . ? C124 C123 C122 121.28(17) . . ? C128 C123 C122 119.33(18) . . ? C123 C124 C125 119.97(18) . . ? C123 C124 H124 120.0 . . ? C125 C124 H124 120.0 . . ? C126 C125 C124 120.0(2) . . ? C126 C125 H125 120.0 . . ? C124 C125 H125 120.0 . . ? C125 C126 C127 120.43(19) . . ? C125 C126 H126 119.8 . . ? C127 C126 H126 119.8 . . ? C128 C127 C126 120.12(19) . . ? C128 C127 H127 119.9 . . ? C126 C127 H127 119.9 . . ? C127 C128 C123 120.1(2) . . ? C127 C128 H128 119.9 . . ? C123 C128 H128 119.9 . . ? Ge1 C131 H13A 109.5 . . ? Ge1 C131 H13B 109.5 . . ? H13A C131 H13B 109.5 . . ? Ge1 C131 H13C 109.5 . . ? H13A C131 H13C 109.5 . . ? H13B C131 H13C 109.5 . . ? Ge1 C141 H14A 109.5 . . ? Ge1 C141 H14B 109.5 . . ? H14A C141 H14B 109.5 . . ? Ge1 C141 H14C 109.5 . . ? H14A C141 H14C 109.5 . . ? H14B C141 H14C 109.5 . . ? C152 C151 C154 108.65(18) . . ? C152 C151 C153 109.56(18) . . ? C154 C151 C153 106.64(19) . . ? C152 C151 Al1 115.79(15) . . ? C154 C151 Al1 106.23(14) . . ? C153 C151 Al1 109.54(14) . . ? C151 C152 H15A 109.5 . . ? C151 C152 H15B 109.5 . . ? H15A C152 H15B 109.5 . . ? C151 C152 H15C 109.5 . . ? H15A C152 H15C 109.5 . . ? H15B C152 H15C 109.5 . . ? C151 C153 H15D 109.5 . . ? C151 C153 H15E 109.5 . . ? H15D C153 H15E 109.5 . . ? C151 C153 H15F 109.5 . . ? H15D C153 H15F 109.5 . . ? H15E C153 H15F 109.5 . . ? C151 C154 H15G 109.5 . . ? C151 C154 H15H 109.5 . . ? H15G C154 H15H 109.5 . . ? C151 C154 H15I 109.5 . . ? H15G C154 H15I 109.5 . . ? H15H C154 H15I 109.5 . . ? C162 C161 C163 108.6(2) . . ? C162 C161 C164 109.0(2) . . ? C163 C161 C164 107.91(19) . . ? C162 C161 Al1 111.06(15) . . ? C163 C161 Al1 115.58(15) . . ? C164 C161 Al1 104.43(15) . . ? 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 . . ? C161 C164 H16G 109.5 . . ? C161 C164 H16H 109.5 . . ? H16G C164 H16H 109.5 . . ? C161 C164 H16I 109.5 . . ? H16G C164 H16I 109.5 . . ? H16H C164 H16I 109.5 . . ? C211 Ge2 C231 117.62(10) . . ? C211 Ge2 C241 117.83(10) . . ? C231 Ge2 C241 112.98(13) . . ? C211 Ge2 C221 93.45(8) . . ? C231 Ge2 C221 106.39(10) . . ? C241 Ge2 C221 104.78(10) . . ? C261 Al2 C211 114.02(8) . . ? C261 Al2 C251 125.21(9) . . ? C211 Al2 C251 112.00(8) . . ? C261 Al2 C221 107.78(8) . . ? C211 Al2 C221 80.37(7) . . ? C251 Al2 C221 107.70(8) . . ? C212 C211 Ge2 132.16(14) . . ? C212 C211 Al2 127.74(14) . . ? Ge2 C211 Al2 100.06(8) . . ? C211 C212 C213 132.43(17) . . ? C211 C212 H212 113.8 . . ? C213 C212 H212 113.8 . . ? C218 C213 C214 117.38(19) . . ? C218 C213 C212 118.48(19) . . ? C214 C213 C212 124.12(17) . . ? C215 C214 C213 121.1(2) . . ? C215 C214 H214 119.4 . . ? C213 C214 H214 119.4 . . ? C216 C215 C214 120.1(2) . . ? C216 C215 H215 120.0 . . ? C214 C215 H215 120.0 . . ? C217 C216 C215 119.6(2) . . ? C217 C216 H216 120.2 . . ? C215 C216 H216 120.2 . . ? C216 C217 C218 120.1(2) . . ? C216 C217 H217 119.9 . . ? C218 C217 H217 119.9 . . ? C217 C218 C213 121.7(2) . . ? C217 C218 H218 119.1 . . ? C213 C218 H218 119.1 . . ? C222 C221 Ge2 173.85(18) . . ? C222 C221 Al2 98.95(14) . . ? Ge2 C221 Al2 86.12(7) . . ? C221 C222 C223 176.9(2) . . ? C224 C223 C228 119.07(17) . . ? C224 C223 C222 120.48(17) . . ? C228 C223 C222 120.39(17) . . ? C225 C224 C223 119.84(18) . . ? C225 C224 H224 120.1 . . ? C223 C224 H224 120.1 . . ? C226 C225 C224 120.73(19) . . ? C226 C225 H225 119.6 . . ? C224 C225 H225 119.6 . . ? C227 C226 C225 119.77(19) . . ? C227 C226 H226 120.1 . . ? C225 C226 H226 120.1 . . ? C226 C227 C228 120.34(19) . . ? C226 C227 H227 119.8 . . ? C228 C227 H227 119.8 . . ? C227 C228 C223 120.24(18) . . ? C227 C228 H228 119.9 . . ? C223 C228 H228 119.9 . . ? Ge2 C231 H23A 109.5 . . ? Ge2 C231 H23B 109.5 . . ? H23A C231 H23B 109.5 . . ? Ge2 C231 H23C 109.5 . . ? H23A C231 H23C 109.5 . . ? H23B C231 H23C 109.5 . . ? Ge2 C241 H24A 109.5 . . ? Ge2 C241 H24B 109.5 . . ? H24A C241 H24B 109.5 . . ? Ge2 C241 H24C 109.5 . . ? H24A C241 H24C 109.5 . . ? H24B C241 H24C 109.5 . . ? C252 C251 C253 109.01(18) . . ? C252 C251 C254 108.88(18) . . ? C253 C251 C254 108.9(2) . . ? C252 C251 Al2 114.68(14) . . ? C253 C251 Al2 109.98(14) . . ? C254 C251 Al2 105.18(14) . . ? C251 C252 H25A 109.5 . . ? C251 C252 H25B 109.5 . . ? H25A C252 H25B 109.5 . . ? C251 C252 H25C 109.5 . . ? H25A C252 H25C 109.5 . . ? H25B C252 H25C 109.5 . . ? C251 C253 H25D 109.5 . . ? C251 C253 H25E 109.5 . . ? H25D C253 H25E 109.5 . . ? C251 C253 H25F 109.5 . . ? H25D C253 H25F 109.5 . . ? H25E C253 H25F 109.5 . . ? C251 C254 H25G 109.5 . . ? C251 C254 H25H 109.5 . . ? H25G C254 H25H 109.5 . . ? C251 C254 H25I 109.5 . . ? H25G C254 H25I 109.5 . . ? H25H C254 H25I 109.5 . . ? C263 C261 C264 109.25(19) . . ? C263 C261 C262 108.79(19) . . ? C264 C261 C262 106.68(19) . . ? C263 C261 Al2 115.97(16) . . ? C264 C261 Al2 109.24(15) . . ? C262 C261 Al2 106.50(14) . . ? C261 C262 H26A 109.5 . . ? C261 C262 H26B 109.5 . . ? H26A C262 H26B 109.5 . . ? C261 C262 H26C 109.5 . . ? H26A C262 H26C 109.5 . . ? H26B C262 H26C 109.5 . . ? C261 C263 H26D 109.5 . . ? C261 C263 H26E 109.5 . . ? H26D C263 H26E 109.5 . . ? C261 C263 H26F 109.5 . . ? H26D C263 H26F 109.5 . . ? H26E C263 H26F 109.5 . . ? C261 C264 H26G 109.5 . . ? C261 C264 H26H 109.5 . . ? H26G C264 H26H 109.5 . . ? C261 C264 H26I 109.5 . . ? H26G C264 H26I 109.5 . . ? H26H C264 H26I 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 C131 Ge1 C111 C112 65.4(2) . . . . ? C141 Ge1 C111 C112 -75.1(2) . . . . ? C121 Ge1 C111 C112 176.0(2) . . . . ? C131 Ge1 C111 Al1 -112.90(10) . . . . ? C141 Ge1 C111 Al1 106.66(11) . . . . ? C121 Ge1 C111 Al1 -2.23(10) . . . . ? C161 Al1 C111 C112 -71.3(2) . . . . ? C151 Al1 C111 C112 78.8(2) . . . . ? C121 Al1 C111 C112 -176.5(2) . . . . ? C161 Al1 C111 Ge1 107.00(10) . . . . ? C151 Al1 C111 Ge1 -102.91(9) . . . . ? C121 Al1 C111 Ge1 1.82(8) . . . . ? Ge1 C111 C112 C113 4.6(3) . . . . ? Al1 C111 C112 C113 -177.61(16) . . . . ? C111 C112 C113 C114 6.5(4) . . . . ? C111 C112 C113 C118 -175.6(2) . . . . ? C118 C113 C114 C115 -0.2(4) . . . . ? C112 C113 C114 C115 177.8(2) . . . . ? C113 C114 C115 C116 -0.1(4) . . . . ? C114 C115 C116 C117 0.5(4) . . . . ? C115 C116 C117 C118 -0.7(4) . . . . ? C116 C117 C118 C113 0.4(3) . . . . ? C114 C113 C118 C117 0.0(3) . . . . ? C112 C113 C118 C117 -178.05(19) . . . . ? C111 Ge1 C121 C122 163(2) . . . . ? C131 Ge1 C121 C122 -79(2) . . . . ? C141 Ge1 C121 C122 42(2) . . . . ? C111 Ge1 C121 Al1 1.78(8) . . . . ? C131 Ge1 C121 Al1 120.09(9) . . . . ? C141 Ge1 C121 Al1 -118.53(9) . . . . ? C111 Al1 C121 C122 179.81(16) . . . . ? C161 Al1 C121 C122 66.96(17) . . . . ? C151 Al1 C121 C122 -70.02(16) . . . . ? C111 Al1 C121 Ge1 -1.76(8) . . . . ? C161 Al1 C121 Ge1 -114.61(8) . . . . ? C151 Al1 C121 Ge1 108.42(9) . . . . ? Ge1 C121 C122 C123 44(5) . . . . ? Al1 C121 C122 C123 -156(4) . . . . ? C121 C122 C123 C124 -119(4) . . . . ? C121 C122 C123 C128 59(4) . . . . ? C128 C123 C124 C125 -0.2(3) . . . . ? C122 C123 C124 C125 178.36(18) . . . . ? C123 C124 C125 C126 -0.2(3) . . . . ? C124 C125 C126 C127 0.2(3) . . . . ? C125 C126 C127 C128 0.1(3) . . . . ? C126 C127 C128 C123 -0.5(3) . . . . ? C124 C123 C128 C127 0.5(3) . . . . ? C122 C123 C128 C127 -178.08(18) . . . . ? C111 Al1 C151 C152 169.39(15) . . . . ? C161 Al1 C151 C152 -44.09(19) . . . . ? C121 Al1 C151 C152 83.68(16) . . . . ? C111 Al1 C151 C154 -69.91(17) . . . . ? C161 Al1 C151 C154 76.61(18) . . . . ? C121 Al1 C151 C154 -155.62(15) . . . . ? C111 Al1 C151 C153 44.92(15) . . . . ? C161 Al1 C151 C153 -168.56(13) . . . . ? C121 Al1 C151 C153 -40.79(15) . . . . ? C111 Al1 C161 C162 -41.4(2) . . . . ? C151 Al1 C161 C162 172.83(17) . . . . ? C121 Al1 C161 C162 45.30(19) . . . . ? C111 Al1 C161 C163 -165.67(17) . . . . ? C151 Al1 C161 C163 48.6(2) . . . . ? C121 Al1 C161 C163 -78.97(19) . . . . ? C111 Al1 C161 C164 75.95(17) . . . . ? C151 Al1 C161 C164 -69.81(17) . . . . ? C121 Al1 C161 C164 162.66(15) . . . . ? C231 Ge2 C211 C212 -67.2(2) . . . . ? C241 Ge2 C211 C212 73.5(2) . . . . ? C221 Ge2 C211 C212 -177.74(19) . . . . ? C231 Ge2 C211 Al2 110.54(11) . . . . ? C241 Ge2 C211 Al2 -108.70(11) . . . . ? C221 Ge2 C211 Al2 0.02(9) . . . . ? C261 Al2 C211 C212 -76.84(19) . . . . ? C251 Al2 C211 C212 72.57(19) . . . . ? C221 Al2 C211 C212 177.88(18) . . . . ? C261 Al2 C211 Ge2 105.26(9) . . . . ? C251 Al2 C211 Ge2 -105.33(9) . . . . ? C221 Al2 C211 Ge2 -0.01(8) . . . . ? Ge2 C211 C212 C213 -3.9(3) . . . . ? Al2 C211 C212 C213 178.88(15) . . . . ? C211 C212 C213 C218 178.0(2) . . . . ? C211 C212 C213 C214 -3.5(3) . . . . ? C218 C213 C214 C215 0.7(3) . . . . ? C212 C213 C214 C215 -177.8(2) . . . . ? C213 C214 C215 C216 -1.2(4) . . . . ? C214 C215 C216 C217 1.1(4) . . . . ? C215 C216 C217 C218 -0.5(4) . . . . ? C216 C217 C218 C213 0.1(3) . . . . ? C214 C213 C218 C217 -0.1(3) . . . . ? C212 C213 C218 C217 178.46(18) . . . . ? C211 Ge2 C221 C222 -145.6(17) . . . . ? C231 Ge2 C221 C222 94.3(17) . . . . ? C241 Ge2 C221 C222 -25.6(17) . . . . ? C211 Ge2 C221 Al2 -0.01(7) . . . . ? C231 Ge2 C221 Al2 -120.14(10) . . . . ? C241 Ge2 C221 Al2 119.96(10) . . . . ? C261 Al2 C221 C222 64.21(17) . . . . ? C211 Al2 C221 C222 176.50(16) . . . . ? C251 Al2 C221 C222 -73.34(16) . . . . ? C261 Al2 C221 Ge2 -112.27(9) . . . . ? C211 Al2 C221 Ge2 0.01(7) . . . . ? C251 Al2 C221 Ge2 110.18(8) . . . . ? Ge2 C221 C222 C223 -36(5) . . . . ? Al2 C221 C222 C223 179(100) . . . . ? C221 C222 C223 C224 93(4) . . . . ? C221 C222 C223 C228 -84(4) . . . . ? C228 C223 C224 C225 -0.3(3) . . . . ? C222 C223 C224 C225 -177.7(2) . . . . ? C223 C224 C225 C226 0.4(4) . . . . ? C224 C225 C226 C227 -0.2(4) . . . . ? C225 C226 C227 C228 -0.1(4) . . . . ? C226 C227 C228 C223 0.2(4) . . . . ? C224 C223 C228 C227 0.0(3) . . . . ? C222 C223 C228 C227 177.5(2) . . . . ? C261 Al2 C251 C252 -47.59(19) . . . . ? C211 Al2 C251 C252 167.09(15) . . . . ? C221 Al2 C251 C252 80.55(17) . . . . ? C261 Al2 C251 C253 -170.85(14) . . . . ? C211 Al2 C251 C253 43.82(17) . . . . ? C221 Al2 C251 C253 -42.71(16) . . . . ? C261 Al2 C251 C254 71.99(18) . . . . ? C211 Al2 C251 C254 -73.33(17) . . . . ? C221 Al2 C251 C254 -159.87(15) . . . . ? C211 Al2 C261 C263 -172.88(16) . . . . ? C251 Al2 C261 C263 42.4(2) . . . . ? C221 Al2 C261 C263 -85.71(17) . . . . ? C211 Al2 C261 C264 -48.93(17) . . . . ? C251 Al2 C261 C264 166.34(14) . . . . ? C221 Al2 C261 C264 38.24(16) . . . . ? C211 Al2 C261 C262 65.94(18) . . . . ? C251 Al2 C261 C262 -78.79(19) . . . . ? C221 Al2 C261 C262 153.11(16) . . . . ? _diffrn_measured_fraction_theta_max 0.973 _diffrn_reflns_theta_full 72.67 _diffrn_measured_fraction_theta_full 0.973 _refine_diff_density_max 0.317 _refine_diff_density_min -0.300 _refine_diff_density_rms 0.046 # Attachment '- cifcompound6.txt' data_sad_6 _database_code_depnum_ccdc_archive 'CCDC 762761' #TrackingRef '- cifcompound6.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C36 H39 Al Ge' _chemical_formula_weight 571.24 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge -1.0885 0.8855 '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 8.4449(3) _cell_length_b 9.9162(4) _cell_length_c 20.1186(7) _cell_angle_alpha 87.777(2) _cell_angle_beta 87.692(2) _cell_angle_gamma 66.821(2) _cell_volume 1547.02(10) _cell_formula_units_Z 2 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 897 _cell_measurement_theta_min 5.279 _cell_measurement_theta_max 72.219 _exptl_crystal_description rod _exptl_crystal_colour colourless _exptl_crystal_size_max 0.22 _exptl_crystal_size_mid 0.08 _exptl_crystal_size_min 0.06 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.226 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 600 _exptl_absorpt_coefficient_mu 1.768 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6971 _exptl_absorpt_correction_T_max 0.9014 _exptl_absorpt_process_details SADBS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 1.54178 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotation anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 9376 _diffrn_reflns_av_R_equivalents 0.0218 _diffrn_reflns_av_sigmaI/netI 0.0320 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 2.20 _diffrn_reflns_theta_max 72.43 _reflns_number_total 5288 _reflns_number_gt 4697 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT+' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0639P)^2^+0.2753P] 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 5288 _refine_ls_number_parameters 349 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0413 _refine_ls_R_factor_gt 0.0362 _refine_ls_wR_factor_ref 0.0996 _refine_ls_wR_factor_gt 0.0954 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 Ge1 Ge 0.09077(3) 0.25471(2) 0.687279(11) 0.02346(10) Uani 1 1 d . . . C11 C 0.1748(3) 0.0829(2) 0.74597(10) 0.0255(4) Uani 1 1 d . . . C12 C 0.3158(3) -0.0414(2) 0.73988(11) 0.0287(5) Uani 1 1 d . . . H12 H 0.3388 -0.1064 0.7782 0.034 Uiso 1 1 calc R . . C13 C 0.4419(3) -0.0950(2) 0.68396(11) 0.0274(5) Uani 1 1 d . . . C14 C 0.3966(3) -0.0676(2) 0.61769(11) 0.0306(5) Uani 1 1 d . . . H14 H 0.2792 -0.0089 0.6070 0.037 Uiso 1 1 calc R . . C15 C 0.5183(3) -0.1235(3) 0.56651(13) 0.0385(6) Uani 1 1 d . . . H15 H 0.4839 -0.1064 0.5210 0.046 Uiso 1 1 calc R . . C16 C 0.6891(3) -0.2040(3) 0.58126(15) 0.0453(7) Uani 1 1 d . . . H16 H 0.7742 -0.2401 0.5461 0.054 Uiso 1 1 calc R . . C17 C 0.7357(4) -0.2316(3) 0.64620(16) 0.0515(7) Uani 1 1 d . . . H17 H 0.8543 -0.2866 0.6564 0.062 Uiso 1 1 calc R . . C18 C 0.6136(3) -0.1811(3) 0.69774(13) 0.0395(6) Uani 1 1 d . . . H18 H 0.6477 -0.2055 0.7430 0.047 Uiso 1 1 calc R . . C21 C -0.0945(3) 0.3675(2) 0.75015(11) 0.0273(5) Uani 1 1 d . . . C22 C -0.2037(3) 0.4346(2) 0.79064(11) 0.0265(5) Uani 1 1 d . . . C23 C -0.3301(3) 0.5175(2) 0.83969(11) 0.0265(5) Uani 1 1 d . . . C24 C -0.2914(3) 0.6100(3) 0.88070(13) 0.0370(5) Uani 1 1 d . . . H24 H -0.1838 0.6212 0.8749 0.044 Uiso 1 1 calc R . . C25 C -0.4086(4) 0.6855(3) 0.92979(13) 0.0461(7) Uani 1 1 d . . . H25 H -0.3824 0.7496 0.9580 0.055 Uiso 1 1 calc R . . C26 C -0.5625(4) 0.6692(3) 0.93844(14) 0.0495(8) Uani 1 1 d . . . H26 H -0.6420 0.7198 0.9734 0.059 Uiso 1 1 calc R . . C27 C -0.6029(4) 0.5811(3) 0.89734(17) 0.0522(8) Uani 1 1 d . . . H27 H -0.7115 0.5717 0.9032 0.063 Uiso 1 1 calc R . . C28 C -0.4878(3) 0.5053(3) 0.84734(14) 0.0390(6) Uani 1 1 d . . . H28 H -0.5172 0.4448 0.8182 0.047 Uiso 1 1 calc R . . C31 C 0.2312(3) 0.3700(2) 0.67555(10) 0.0244(4) Uani 1 1 d . . . C32 C 0.3842(3) 0.3175(3) 0.63798(13) 0.0367(6) Uani 1 1 d . . . H32 H 0.4207 0.2237 0.6176 0.044 Uiso 1 1 calc R . . C33 C 0.4847(3) 0.3994(3) 0.62968(14) 0.0424(6) Uani 1 1 d . . . H33 H 0.5903 0.3615 0.6038 0.051 Uiso 1 1 calc R . . C34 C 0.4344(3) 0.5337(3) 0.65815(13) 0.0371(5) Uani 1 1 d . . . H34 H 0.5042 0.5900 0.6521 0.045 Uiso 1 1 calc R . . C35 C 0.2833(4) 0.5875(3) 0.69541(13) 0.0407(6) Uani 1 1 d . . . H35 H 0.2469 0.6820 0.7151 0.049 Uiso 1 1 calc R . . C36 C 0.1833(3) 0.5051(3) 0.70461(12) 0.0342(5) Uani 1 1 d . . . H36 H 0.0795 0.5426 0.7315 0.041 Uiso 1 1 calc R . . C41 C -0.0242(3) 0.2511(2) 0.60563(10) 0.0252(4) Uani 1 1 d . . . C42 C -0.0697(3) 0.1349(2) 0.59235(12) 0.0320(5) Uani 1 1 d . . . H42 H -0.0403 0.0526 0.6230 0.038 Uiso 1 1 calc R . . C43 C -0.1573(3) 0.1365(3) 0.53510(13) 0.0390(6) Uani 1 1 d . . . H43 H -0.1886 0.0558 0.5264 0.047 Uiso 1 1 calc R . . C44 C -0.1994(3) 0.2546(3) 0.49065(13) 0.0411(6) Uani 1 1 d . . . H44 H -0.2587 0.2553 0.4508 0.049 Uiso 1 1 calc R . . C45 C -0.1563(3) 0.3714(3) 0.50348(13) 0.0417(6) Uani 1 1 d . . . H45 H -0.1865 0.4537 0.4728 0.050 Uiso 1 1 calc R . . C46 C -0.0692(3) 0.3701(3) 0.56074(12) 0.0329(5) Uani 1 1 d . . . H46 H -0.0397 0.4518 0.5695 0.039 Uiso 1 1 calc R . . Al1 Al 0.01314(8) 0.15093(7) 0.82426(3) 0.02578(15) Uani 1 1 d . . . CT1 C 0.1200(3) 0.2007(2) 0.90112(11) 0.0296(5) Uani 1 1 d . . . CT11 C 0.0031(3) 0.2617(3) 0.96246(12) 0.0408(6) Uani 1 1 d . . . HT1A H 0.0681 0.2814 0.9961 0.049 Uiso 1 1 calc R . . HT1B H -0.0407 0.1910 0.9795 0.049 Uiso 1 1 calc R . . HT1C H -0.0912 0.3509 0.9502 0.049 Uiso 1 1 calc R . . CT12 C 0.2627(3) 0.0542(3) 0.92230(13) 0.0403(6) Uani 1 1 d . . . HT1D H 0.3418 0.0158 0.8855 0.048 Uiso 1 1 calc R . . HT1E H 0.2123 -0.0143 0.9359 0.048 Uiso 1 1 calc R . . HT1F H 0.3231 0.0696 0.9588 0.048 Uiso 1 1 calc R . . CT13 C 0.2059(3) 0.3065(3) 0.87937(13) 0.0399(6) Uani 1 1 d . . . HT1G H 0.1187 0.4016 0.8695 0.048 Uiso 1 1 calc R . . HT1H H 0.2774 0.2702 0.8404 0.048 Uiso 1 1 calc R . . HT1I H 0.2752 0.3139 0.9146 0.048 Uiso 1 1 calc R . . CT2 C -0.1610(3) 0.0607(3) 0.83272(12) 0.0338(5) Uani 1 1 d . . . CT21 C -0.2837(4) 0.1053(3) 0.77419(14) 0.0452(6) Uani 1 1 d . . . HT2A H -0.2185 0.0757 0.7333 0.054 Uiso 1 1 calc R . . HT2B H -0.3461 0.2098 0.7732 0.054 Uiso 1 1 calc R . . HT2C H -0.3635 0.0581 0.7795 0.054 Uiso 1 1 calc R . . CT22 C -0.0596(4) -0.1049(3) 0.83229(19) 0.0580(8) Uani 1 1 d . . . HT2D H -0.1380 -0.1535 0.8367 0.070 Uiso 1 1 calc R . . HT2E H 0.0177 -0.1341 0.8687 0.070 Uiso 1 1 calc R . . HT2F H 0.0052 -0.1313 0.7911 0.070 Uiso 1 1 calc R . . CT23 C -0.2698(4) 0.0976(3) 0.89717(14) 0.0489(7) Uani 1 1 d . . . HT2G H -0.3466 0.0473 0.8990 0.059 Uiso 1 1 calc R . . HT2H H -0.3356 0.2015 0.8984 0.059 Uiso 1 1 calc R . . HT2I H -0.1956 0.0672 0.9346 0.059 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.02547(15) 0.02536(15) 0.01954(14) -0.00210(9) 0.00448(9) -0.01030(10) C11 0.0324(12) 0.0248(11) 0.0220(10) -0.0011(7) 0.0003(8) -0.0142(9) C12 0.0385(13) 0.0259(11) 0.0228(11) -0.0008(8) 0.0000(9) -0.0141(9) C13 0.0306(12) 0.0193(10) 0.0318(12) -0.0029(8) 0.0016(9) -0.0094(8) C14 0.0320(12) 0.0262(11) 0.0294(12) -0.0037(8) 0.0014(9) -0.0067(9) C15 0.0461(15) 0.0352(13) 0.0304(13) -0.0030(9) 0.0086(11) -0.0126(11) C16 0.0394(15) 0.0402(15) 0.0523(17) -0.0118(11) 0.0175(13) -0.0122(11) C17 0.0273(14) 0.0479(16) 0.068(2) -0.0139(14) -0.0012(13) -0.0011(11) C18 0.0379(14) 0.0335(13) 0.0402(14) -0.0063(10) -0.0087(11) -0.0053(10) C21 0.0267(11) 0.0309(11) 0.0251(11) -0.0012(8) 0.0014(9) -0.0122(9) C22 0.0278(11) 0.0267(11) 0.0244(11) 0.0004(8) 0.0009(9) -0.0103(9) C23 0.0282(11) 0.0242(11) 0.0234(11) -0.0004(8) 0.0040(9) -0.0067(8) C24 0.0329(13) 0.0310(12) 0.0435(14) -0.0092(10) 0.0000(11) -0.0081(10) C25 0.0528(17) 0.0356(14) 0.0388(15) -0.0151(10) -0.0005(13) -0.0043(12) C26 0.0568(18) 0.0320(14) 0.0427(15) -0.0057(11) 0.0225(14) -0.0010(12) C27 0.0392(15) 0.0359(15) 0.077(2) -0.0092(13) 0.0273(15) -0.0118(11) C28 0.0315(13) 0.0305(13) 0.0536(16) -0.0112(10) 0.0084(11) -0.0105(10) C31 0.0242(11) 0.0254(10) 0.0238(10) 0.0029(8) 0.0003(8) -0.0101(8) C32 0.0347(13) 0.0288(12) 0.0457(15) -0.0083(10) 0.0135(11) -0.0122(10) C33 0.0328(13) 0.0379(14) 0.0564(17) -0.0020(11) 0.0143(12) -0.0152(11) C34 0.0360(13) 0.0386(14) 0.0424(14) 0.0048(10) -0.0011(11) -0.0212(11) C35 0.0500(16) 0.0331(13) 0.0445(15) -0.0097(10) 0.0088(12) -0.0223(12) C36 0.0359(13) 0.0323(12) 0.0343(13) -0.0065(9) 0.0107(10) -0.0140(10) C41 0.0215(10) 0.0295(11) 0.0212(10) -0.0039(8) 0.0037(8) -0.0066(8) C42 0.0324(12) 0.0285(12) 0.0307(12) -0.0041(8) -0.0005(9) -0.0071(9) C43 0.0425(15) 0.0334(13) 0.0390(14) -0.0116(10) -0.0041(11) -0.0113(11) C44 0.0396(14) 0.0558(16) 0.0269(13) -0.0044(10) -0.0029(10) -0.0174(12) C45 0.0366(14) 0.0560(16) 0.0339(14) 0.0159(11) -0.0032(11) -0.0210(12) C46 0.0331(13) 0.0366(13) 0.0314(12) 0.0042(9) 0.0014(10) -0.0171(10) Al1 0.0301(4) 0.0282(3) 0.0204(3) 0.0000(2) 0.0038(3) -0.0135(3) CT1 0.0351(12) 0.0294(12) 0.0238(11) -0.0011(8) 0.0001(9) -0.0124(9) CT11 0.0429(15) 0.0491(15) 0.0262(12) -0.0080(10) 0.0012(11) -0.0132(12) CT12 0.0437(15) 0.0393(14) 0.0318(13) 0.0013(10) -0.0019(11) -0.0098(11) CT13 0.0473(15) 0.0445(15) 0.0359(14) 0.0030(10) -0.0088(11) -0.0264(12) CT2 0.0374(13) 0.0343(13) 0.0344(13) 0.0018(9) 0.0037(10) -0.0197(10) CT21 0.0533(17) 0.0516(16) 0.0425(16) -0.0049(12) -0.0007(12) -0.0330(14) CT22 0.0523(18) 0.0368(16) 0.087(2) 0.0030(14) 0.0090(17) -0.0218(13) CT23 0.0491(17) 0.0667(19) 0.0393(15) 0.0020(13) 0.0103(13) -0.0331(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 Ge1 C11 1.939(2) . ? Ge1 C31 1.947(2) . ? Ge1 C41 1.950(2) . ? Ge1 C21 1.968(2) . ? C11 C12 1.341(3) . ? C11 Al1 1.996(2) . ? C12 C13 1.479(3) . ? C12 H12 0.9600 . ? C13 C14 1.389(3) . ? C13 C18 1.395(3) . ? C14 C15 1.391(3) . ? C14 H14 0.9600 . ? C15 C16 1.384(4) . ? C15 H15 0.9600 . ? C16 C17 1.366(4) . ? C16 H16 0.9600 . ? C17 C18 1.392(4) . ? C17 H17 0.9600 . ? C18 H18 0.9600 . ? C21 C22 1.207(3) . ? C21 Al1 2.446(2) . ? C22 C23 1.441(3) . ? C23 C28 1.385(3) . ? C23 C24 1.395(3) . ? C24 C25 1.382(3) . ? C24 H24 0.9600 . ? C25 C26 1.375(4) . ? C25 H25 0.9600 . ? C26 C27 1.370(5) . ? C26 H26 0.9600 . ? C27 C28 1.388(3) . ? C27 H27 0.9600 . ? C28 H28 0.9600 . ? C31 C36 1.385(3) . ? C31 C32 1.391(3) . ? C32 C33 1.389(3) . ? C32 H32 0.9600 . ? C33 C34 1.370(4) . ? C33 H33 0.9600 . ? C34 C35 1.376(3) . ? C34 H34 0.9600 . ? C35 C36 1.390(3) . ? C35 H35 0.9600 . ? C36 H36 0.9600 . ? C41 C42 1.388(3) . ? C41 C46 1.395(3) . ? C42 C43 1.390(4) . ? C42 H42 0.9600 . ? C43 C44 1.384(4) . ? C43 H43 0.9600 . ? C44 C45 1.380(4) . ? C44 H44 0.9600 . ? C45 C46 1.388(4) . ? C45 H45 0.9600 . ? C46 H46 0.9600 . ? Al1 CT1 1.993(2) . ? Al1 CT2 1.999(2) . ? CT1 CT11 1.534(3) . ? CT1 CT13 1.535(3) . ? CT1 CT12 1.536(3) . ? CT11 HT1A 0.9599 . ? CT11 HT1B 0.9599 . ? CT11 HT1C 0.9599 . ? CT12 HT1D 0.9599 . ? CT12 HT1E 0.9599 . ? CT12 HT1F 0.9599 . ? CT13 HT1G 0.9599 . ? CT13 HT1H 0.9599 . ? CT13 HT1I 0.9599 . ? CT2 CT22 1.524(4) . ? CT2 CT23 1.528(3) . ? CT2 CT21 1.534(4) . ? CT21 HT2A 0.9599 . ? CT21 HT2B 0.9599 . ? CT21 HT2C 0.9599 . ? CT22 HT2D 0.9599 . ? CT22 HT2E 0.9599 . ? CT22 HT2F 0.9599 . ? CT23 HT2G 0.9599 . ? CT23 HT2H 0.9599 . ? CT23 HT2I 0.9599 . ? 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 C11 Ge1 C31 117.49(9) . . ? C11 Ge1 C41 120.38(9) . . ? C31 Ge1 C41 111.64(9) . . ? C11 Ge1 C21 93.46(9) . . ? C31 Ge1 C21 104.15(9) . . ? C41 Ge1 C21 105.47(9) . . ? C12 C11 Ge1 129.74(17) . . ? C12 C11 Al1 128.56(17) . . ? Ge1 C11 Al1 101.23(10) . . ? C11 C12 C13 130.7(2) . . ? C11 C12 H12 114.6 . . ? C13 C12 H12 114.6 . . ? C14 C13 C18 117.9(2) . . ? C14 C13 C12 123.0(2) . . ? C18 C13 C12 119.1(2) . . ? C13 C14 C15 121.2(2) . . ? C13 C14 H14 119.4 . . ? C15 C14 H14 119.4 . . ? C16 C15 C14 119.9(2) . . ? C16 C15 H15 120.0 . . ? C14 C15 H15 120.0 . . ? C17 C16 C15 119.5(2) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 120.9(3) . . ? C16 C17 H17 119.5 . . ? C18 C17 H17 119.5 . . ? C17 C18 C13 120.4(3) . . ? C17 C18 H18 119.8 . . ? C13 C18 H18 119.8 . . ? C22 C21 Ge1 177.5(2) . . ? C22 C21 Al1 91.76(16) . . ? Ge1 C21 Al1 86.39(8) . . ? C21 C22 C23 177.9(3) . . ? C28 C23 C24 119.7(2) . . ? C28 C23 C22 121.2(2) . . ? C24 C23 C22 119.1(2) . . ? C25 C24 C23 119.7(2) . . ? C25 C24 H24 120.1 . . ? C23 C24 H24 120.1 . . ? C26 C25 C24 120.3(3) . . ? C26 C25 H25 119.9 . . ? C24 C25 H25 119.9 . . ? C27 C26 C25 120.3(2) . . ? C27 C26 H26 119.9 . . ? C25 C26 H26 119.9 . . ? C26 C27 C28 120.4(3) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C23 C28 C27 119.6(3) . . ? C23 C28 H28 120.2 . . ? C27 C28 H28 120.2 . . ? C36 C31 C32 118.0(2) . . ? C36 C31 Ge1 121.39(16) . . ? C32 C31 Ge1 120.57(17) . . ? C33 C32 C31 120.7(2) . . ? C33 C32 H32 119.7 . . ? C31 C32 H32 119.7 . . ? C34 C33 C32 120.5(2) . . ? C34 C33 H33 119.7 . . ? C32 C33 H33 119.7 . . ? C33 C34 C35 119.6(2) . . ? C33 C34 H34 120.2 . . ? C35 C34 H34 120.2 . . ? C34 C35 C36 120.1(2) . . ? C34 C35 H35 120.0 . . ? C36 C35 H35 120.0 . . ? C31 C36 C35 121.0(2) . . ? C31 C36 H36 119.5 . . ? C35 C36 H36 119.5 . . ? C42 C41 C46 118.8(2) . . ? C42 C41 Ge1 121.37(17) . . ? C46 C41 Ge1 119.76(17) . . ? C41 C42 C43 120.7(2) . . ? C41 C42 H42 119.7 . . ? C43 C42 H42 119.7 . . ? C44 C43 C42 119.9(2) . . ? C44 C43 H43 120.1 . . ? C42 C43 H43 120.1 . . ? C45 C44 C43 120.1(2) . . ? C45 C44 H44 120.0 . . ? C43 C44 H44 120.0 . . ? C44 C45 C46 120.1(2) . . ? C44 C45 H45 120.0 . . ? C46 C45 H45 120.0 . . ? C45 C46 C41 120.5(2) . . ? C45 C46 H46 119.8 . . ? C41 C46 H46 119.8 . . ? CT1 Al1 C11 113.00(10) . . ? CT1 Al1 CT2 124.31(10) . . ? C11 Al1 CT2 113.79(10) . . ? CT1 Al1 C21 107.79(9) . . ? C11 Al1 C21 78.92(8) . . ? CT2 Al1 C21 109.26(9) . . ? CT11 CT1 CT13 108.9(2) . . ? CT11 CT1 CT12 107.48(19) . . ? CT13 CT1 CT12 107.8(2) . . ? CT11 CT1 Al1 116.87(17) . . ? CT13 CT1 Al1 110.94(16) . . ? CT12 CT1 Al1 104.33(16) . . ? CT1 CT11 HT1A 109.5 . . ? CT1 CT11 HT1B 109.5 . . ? HT1A CT11 HT1B 109.5 . . ? CT1 CT11 HT1C 109.5 . . ? HT1A CT11 HT1C 109.5 . . ? HT1B CT11 HT1C 109.5 . . ? CT1 CT12 HT1D 109.5 . . ? CT1 CT12 HT1E 109.5 . . ? HT1D CT12 HT1E 109.5 . . ? CT1 CT12 HT1F 109.5 . . ? HT1D CT12 HT1F 109.5 . . ? HT1E CT12 HT1F 109.5 . . ? CT1 CT13 HT1G 109.5 . . ? CT1 CT13 HT1H 109.5 . . ? HT1G CT13 HT1H 109.5 . . ? CT1 CT13 HT1I 109.5 . . ? HT1G CT13 HT1I 109.5 . . ? HT1H CT13 HT1I 109.5 . . ? CT22 CT2 CT23 108.0(2) . . ? CT22 CT2 CT21 108.7(2) . . ? CT23 CT2 CT21 108.1(2) . . ? CT22 CT2 Al1 106.28(18) . . ? CT23 CT2 Al1 113.76(18) . . ? CT21 CT2 Al1 111.91(16) . . ? CT2 CT21 HT2A 109.5 . . ? CT2 CT21 HT2B 109.5 . . ? HT2A CT21 HT2B 109.5 . . ? CT2 CT21 HT2C 109.5 . . ? HT2A CT21 HT2C 109.5 . . ? HT2B CT21 HT2C 109.5 . . ? CT2 CT22 HT2D 109.5 . . ? CT2 CT22 HT2E 109.5 . . ? HT2D CT22 HT2E 109.5 . . ? CT2 CT22 HT2F 109.5 . . ? HT2D CT22 HT2F 109.5 . . ? HT2E CT22 HT2F 109.5 . . ? CT2 CT23 HT2G 109.5 . . ? CT2 CT23 HT2H 109.5 . . ? HT2G CT23 HT2H 109.5 . . ? CT2 CT23 HT2I 109.5 . . ? HT2G CT23 HT2I 109.5 . . ? HT2H CT23 HT2I 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 C31 Ge1 C11 C12 -65.0(2) . . . . ? C41 Ge1 C11 C12 76.9(2) . . . . ? C21 Ge1 C11 C12 -172.9(2) . . . . ? C31 Ge1 C11 Al1 107.51(10) . . . . ? C41 Ge1 C11 Al1 -110.59(10) . . . . ? C21 Ge1 C11 Al1 -0.39(10) . . . . ? Ge1 C11 C12 C13 -7.6(4) . . . . ? Al1 C11 C12 C13 -178.18(19) . . . . ? C11 C12 C13 C14 -34.6(4) . . . . ? C11 C12 C13 C18 147.5(3) . . . . ? C18 C13 C14 C15 -0.2(3) . . . . ? C12 C13 C14 C15 -178.2(2) . . . . ? C13 C14 C15 C16 -2.2(4) . . . . ? C14 C15 C16 C17 2.0(4) . . . . ? C15 C16 C17 C18 0.6(5) . . . . ? C16 C17 C18 C13 -3.0(4) . . . . ? C14 C13 C18 C17 2.8(4) . . . . ? C12 C13 C18 C17 -179.2(2) . . . . ? C11 Ge1 C21 C22 42(5) . . . . ? C31 Ge1 C21 C22 -77(5) . . . . ? C41 Ge1 C21 C22 165(5) . . . . ? C11 Ge1 C21 Al1 0.32(8) . . . . ? C31 Ge1 C21 Al1 -119.17(8) . . . . ? C41 Ge1 C21 Al1 123.17(8) . . . . ? Ge1 C21 C22 C23 58(10) . . . . ? Al1 C21 C22 C23 100(7) . . . . ? C21 C22 C23 C28 177(100) . . . . ? C21 C22 C23 C24 -4(7) . . . . ? C28 C23 C24 C25 1.8(4) . . . . ? C22 C23 C24 C25 -177.3(2) . . . . ? C23 C24 C25 C26 0.3(4) . . . . ? C24 C25 C26 C27 -1.7(4) . . . . ? C25 C26 C27 C28 1.1(5) . . . . ? C24 C23 C28 C27 -2.4(4) . . . . ? C22 C23 C28 C27 176.7(2) . . . . ? C26 C27 C28 C23 0.9(4) . . . . ? C11 Ge1 C31 C36 -106.2(2) . . . . ? C41 Ge1 C31 C36 108.7(2) . . . . ? C21 Ge1 C31 C36 -4.6(2) . . . . ? C11 Ge1 C31 C32 73.1(2) . . . . ? C41 Ge1 C31 C32 -71.9(2) . . . . ? C21 Ge1 C31 C32 174.74(19) . . . . ? C36 C31 C32 C33 -0.5(4) . . . . ? Ge1 C31 C32 C33 -179.9(2) . . . . ? C31 C32 C33 C34 -0.3(4) . . . . ? C32 C33 C34 C35 0.2(4) . . . . ? C33 C34 C35 C36 0.6(4) . . . . ? C32 C31 C36 C35 1.3(4) . . . . ? Ge1 C31 C36 C35 -179.3(2) . . . . ? C34 C35 C36 C31 -1.4(4) . . . . ? C11 Ge1 C41 C42 9.1(2) . . . . ? C31 Ge1 C41 C42 153.00(17) . . . . ? C21 Ge1 C41 C42 -94.50(18) . . . . ? C11 Ge1 C41 C46 -173.87(16) . . . . ? C31 Ge1 C41 C46 -29.9(2) . . . . ? C21 Ge1 C41 C46 82.55(19) . . . . ? C46 C41 C42 C43 0.5(3) . . . . ? Ge1 C41 C42 C43 177.57(17) . . . . ? C41 C42 C43 C44 0.2(4) . . . . ? C42 C43 C44 C45 -0.7(4) . . . . ? C43 C44 C45 C46 0.6(4) . . . . ? C44 C45 C46 C41 0.2(4) . . . . ? C42 C41 C46 C45 -0.7(3) . . . . ? Ge1 C41 C46 C45 -177.81(18) . . . . ? C12 C11 Al1 CT1 68.2(2) . . . . ? Ge1 C11 Al1 CT1 -104.46(11) . . . . ? C12 C11 Al1 CT2 -80.7(2) . . . . ? Ge1 C11 Al1 CT2 106.64(11) . . . . ? C12 C11 Al1 C21 173.0(2) . . . . ? Ge1 C11 Al1 C21 0.32(9) . . . . ? C22 C21 Al1 CT1 -67.83(18) . . . . ? Ge1 C21 Al1 CT1 110.49(9) . . . . ? C22 C21 Al1 C11 -178.64(18) . . . . ? Ge1 C21 Al1 C11 -0.31(8) . . . . ? C22 C21 Al1 CT2 69.83(18) . . . . ? Ge1 C21 Al1 CT2 -111.84(10) . . . . ? C11 Al1 CT1 CT11 176.94(17) . . . . ? CT2 Al1 CT1 CT11 -38.0(2) . . . . ? C21 Al1 CT1 CT11 91.70(18) . . . . ? C11 Al1 CT1 CT13 51.26(19) . . . . ? CT2 Al1 CT1 CT13 -163.65(16) . . . . ? C21 Al1 CT1 CT13 -33.98(18) . . . . ? C11 Al1 CT1 CT12 -64.57(17) . . . . ? CT2 Al1 CT1 CT12 80.52(18) . . . . ? C21 Al1 CT1 CT12 -149.81(15) . . . . ? CT1 Al1 CT2 CT22 -90.8(2) . . . . ? C11 Al1 CT2 CT22 54.0(2) . . . . ? C21 Al1 CT2 CT22 140.10(19) . . . . ? CT1 Al1 CT2 CT23 27.9(2) . . . . ? C11 Al1 CT2 CT23 172.71(18) . . . . ? C21 Al1 CT2 CT23 -101.21(19) . . . . ? CT1 Al1 CT2 CT21 150.67(17) . . . . ? C11 Al1 CT2 CT21 -64.5(2) . . . . ? C21 Al1 CT2 CT21 21.6(2) . . . . ? _diffrn_measured_fraction_theta_max 0.862 _diffrn_reflns_theta_full 72.43 _diffrn_measured_fraction_theta_full 0.862 _refine_diff_density_max 0.450 _refine_diff_density_min -0.325 _refine_diff_density_rms 0.061 # Attachment '- cifcompound5.txt' data_sad_5 _database_code_depnum_ccdc_archive 'CCDC 762762' #TrackingRef '- cifcompound5.txt' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C38 H43 Al Ge' _chemical_formula_weight 599.29 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source C C 0.0181 0.0091 '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' Al Al 0.2130 0.2455 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Ge Ge -1.0885 0.8855 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M P2(1)/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 10.0303(2) _cell_length_b 30.7031(5) _cell_length_c 10.9998(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.7330(10) _cell_angle_gamma 90.00 _cell_volume 3348.24(11) _cell_formula_units_Z 4 _cell_measurement_temperature 153(2) _cell_measurement_reflns_used 5305 _cell_measurement_theta_min 2.879 _cell_measurement_theta_max 71.862 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_max 0.31 _exptl_crystal_size_mid 0.16 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.189 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1264 _exptl_absorpt_coefficient_mu 1.655 _exptl_absorpt_correction_type empirical _exptl_absorpt_correction_T_min 0.6279 _exptl_absorpt_correction_T_max 0.8790 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 153(2) _diffrn_radiation_wavelength 1.54184 _diffrn_radiation_type CuK\a _diffrn_radiation_source 'rotating anode' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 19732 _diffrn_reflns_av_R_equivalents 0.0266 _diffrn_reflns_av_sigmaI/netI 0.0231 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -32 _diffrn_reflns_limit_k_max 37 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 12 _diffrn_reflns_theta_min 2.88 _diffrn_reflns_theta_max 72.04 _reflns_number_total 5984 _reflns_number_gt 5468 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT+' _computing_data_reduction 'Bruker SHELXTL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details 'calc w=1/[\s^2^(Fo^2^)+(0.0533P)^2^+1.1976P] 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 5984 _refine_ls_number_parameters 367 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0363 _refine_ls_R_factor_gt 0.0330 _refine_ls_wR_factor_ref 0.0884 _refine_ls_wR_factor_gt 0.0863 _refine_ls_goodness_of_fit_ref 1.027 _refine_ls_restrained_S_all 1.027 _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 Ge1 Ge 0.678114(19) 0.108608(6) 0.234329(17) 0.02444(8) Uani 1 1 d . . . Al1 Al 0.71288(5) 0.140701(17) 0.50157(4) 0.02605(12) Uani 1 1 d . . . C11 C 0.63715(17) 0.15872(6) 0.33088(15) 0.0252(3) Uani 1 1 d . . . C12 C 0.55959(18) 0.19215(6) 0.28659(16) 0.0283(4) Uani 1 1 d . . . H12 H 0.5423 0.2138 0.3451 0.034 Uiso 1 1 calc R . . C13 C 0.49711(17) 0.19955(5) 0.15743(16) 0.0268(4) Uani 1 1 d . . . C14 C 0.56989(18) 0.19520(6) 0.05975(17) 0.0284(4) Uani 1 1 d . . . H14 H 0.6648 0.1891 0.0762 0.034 Uiso 1 1 calc R . . C15 C 0.50734(19) 0.19956(6) -0.06033(17) 0.0323(4) Uani 1 1 d . . . H15 H 0.5588 0.1963 -0.1266 0.039 Uiso 1 1 calc R . . C16 C 0.3705(2) 0.20856(6) -0.08568(18) 0.0355(4) Uani 1 1 d . . . H16 H 0.3266 0.2109 -0.1693 0.043 Uiso 1 1 calc R . . C17 C 0.2976(2) 0.21415(7) 0.01013(19) 0.0379(4) Uani 1 1 d . . . H17 H 0.2031 0.2208 -0.0070 0.045 Uiso 1 1 calc R . . C18 C 0.36015(18) 0.21017(6) 0.13061(18) 0.0327(4) Uani 1 1 d . . . H18 H 0.3090 0.2147 0.1965 0.039 Uiso 1 1 calc R . . C21 C 0.76609(18) 0.07707(6) 0.37842(16) 0.0288(4) Uani 1 1 d . . . C22 C 0.82178(17) 0.05976(6) 0.47037(16) 0.0278(4) Uani 1 1 d . . . C23 C 0.88716(18) 0.03685(6) 0.57720(16) 0.0283(4) Uani 1 1 d . . . C24 C 1.02014(19) 0.04621(6) 0.62657(18) 0.0351(4) Uani 1 1 d . . . H24 H 1.0683 0.0687 0.5912 0.042 Uiso 1 1 calc R . . C25 C 1.0825(2) 0.02290(7) 0.72683(19) 0.0432(5) Uani 1 1 d . . . H25 H 1.1740 0.0295 0.7614 0.052 Uiso 1 1 calc R . . C26 C 1.0143(2) -0.00962(7) 0.77729(19) 0.0464(5) Uani 1 1 d . . . H26 H 1.0584 -0.0257 0.8468 0.056 Uiso 1 1 calc R . . C27 C 0.8832(2) -0.01915(7) 0.7284(2) 0.0478(5) Uani 1 1 d . . . H27 H 0.8364 -0.0421 0.7635 0.057 Uiso 1 1 calc R . . C28 C 0.8184(2) 0.00409(7) 0.62929(19) 0.0387(4) Uani 1 1 d . . . H28 H 0.7263 -0.0023 0.5964 0.046 Uiso 1 1 calc R . . C31 C 0.81372(18) 0.11404(6) 0.12540(17) 0.0290(4) Uani 1 1 d . . . C32 C 0.9427(2) 0.12902(7) 0.1699(2) 0.0437(5) Uani 1 1 d . . . H32 H 0.9655 0.1369 0.2550 0.052 Uiso 1 1 calc R . . C33 C 1.0384(2) 0.13270(9) 0.0918(3) 0.0596(7) Uani 1 1 d . . . H33 H 1.1273 0.1431 0.1232 0.072 Uiso 1 1 calc R . . C34 C 1.0070(3) 0.12158(9) -0.0303(3) 0.0590(7) Uani 1 1 d . . . H34 H 1.0735 0.1244 -0.0840 0.071 Uiso 1 1 calc R . . C35 C 0.8802(3) 0.10644(8) -0.0755(2) 0.0530(6) Uani 1 1 d . . . H35 H 0.8584 0.0984 -0.1606 0.064 Uiso 1 1 calc R . . C36 C 0.7837(2) 0.10280(7) 0.00206(19) 0.0391(5) Uani 1 1 d . . . H36 H 0.6951 0.0924 -0.0300 0.047 Uiso 1 1 calc R . . C41 C 0.53041(17) 0.07137(6) 0.16131(15) 0.0262(4) Uani 1 1 d . . . C42 C 0.52394(19) 0.02834(6) 0.19925(18) 0.0341(4) Uani 1 1 d . . . H42 H 0.5909 0.0174 0.2637 0.041 Uiso 1 1 calc R . . C43 C 0.4217(2) 0.00097(7) 0.1450(2) 0.0411(5) Uani 1 1 d . . . H43 H 0.4178 -0.0286 0.1725 0.049 Uiso 1 1 calc R . . C44 C 0.3258(2) 0.01619(7) 0.0517(2) 0.0415(5) Uani 1 1 d . . . H44 H 0.2560 -0.0029 0.0133 0.050 Uiso 1 1 calc R . . C45 C 0.3302(2) 0.05885(7) 0.01382(18) 0.0384(4) Uani 1 1 d . . . H45 H 0.2626 0.0695 -0.0504 0.046 Uiso 1 1 calc R . . C46 C 0.43145(19) 0.08642(6) 0.06758(17) 0.0335(4) Uani 1 1 d . . . H46 H 0.4337 0.1161 0.0403 0.040 Uiso 1 1 calc R . . C51 C 0.59449(19) 0.11872(7) 0.61623(18) 0.0341(4) Uani 1 1 d . . . H51A H 0.6157 0.0884 0.6297 0.041 Uiso 1 1 calc R . . H51B H 0.6216 0.1332 0.6934 0.041 Uiso 1 1 calc R . . C52 C 0.43978(19) 0.12207(7) 0.58802(18) 0.0362(4) Uani 1 1 d . . . C521 C 0.3989(2) 0.16946(8) 0.5701(2) 0.0536(6) Uani 1 1 d . . . H52A H 0.4356 0.1812 0.5014 0.064 Uiso 1 1 calc R . . H52B H 0.4329 0.1856 0.6429 0.064 Uiso 1 1 calc R . . H52C H 0.3023 0.1716 0.5547 0.064 Uiso 1 1 calc R . . C522 C 0.3883(3) 0.09608(11) 0.4727(3) 0.0704(8) Uani 1 1 d . . . H52D H 0.2915 0.0972 0.4575 0.084 Uiso 1 1 calc R . . H52E H 0.4172 0.0664 0.4839 0.084 Uiso 1 1 calc R . . H52F H 0.4236 0.1083 0.4038 0.084 Uiso 1 1 calc R . . C523 C 0.3763(2) 0.10401(8) 0.6966(2) 0.0479(6) Uani 1 1 d . . . H52G H 0.4141 0.1188 0.7708 0.058 Uiso 1 1 calc R . . H52H H 0.3946 0.0734 0.7052 0.058 Uiso 1 1 calc R . . H52I H 0.2805 0.1086 0.6815 0.058 Uiso 1 1 calc R . . C61 C 0.89369(18) 0.16143(6) 0.57686(16) 0.0298(4) Uani 1 1 d . . . H61A H 0.9237 0.1434 0.6471 0.036 Uiso 1 1 calc R . . H61B H 0.9545 0.1567 0.5187 0.036 Uiso 1 1 calc R . . C62 C 0.90753(18) 0.20919(6) 0.61851(16) 0.0295(4) Uani 1 1 d . . . C621 C 0.8913(2) 0.23947(7) 0.50756(19) 0.0440(5) Uani 1 1 d . . . H62A H 0.8024 0.2362 0.4618 0.053 Uiso 1 1 calc R . . H62B H 0.9572 0.2323 0.4560 0.053 Uiso 1 1 calc R . . H62C H 0.9040 0.2691 0.5350 0.053 Uiso 1 1 calc R . . C622 C 0.7985(2) 0.22033(7) 0.69722(19) 0.0388(5) Uani 1 1 d . . . H62D H 0.8110 0.2497 0.7269 0.047 Uiso 1 1 calc R . . H62E H 0.8050 0.2007 0.7657 0.047 Uiso 1 1 calc R . . H62F H 0.7111 0.2176 0.6483 0.047 Uiso 1 1 calc R . . C623 C 1.0458(2) 0.21704(7) 0.69626(19) 0.0407(5) Uani 1 1 d . . . H62G H 1.0532 0.2470 0.7209 0.049 Uiso 1 1 calc R . . H62H H 1.1156 0.2102 0.6486 0.049 Uiso 1 1 calc R . . H62I H 1.0551 0.1988 0.7680 0.049 Uiso 1 1 calc R . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.02569(12) 0.02489(13) 0.02141(12) -0.00087(7) -0.00072(8) 0.00031(7) Al1 0.0262(3) 0.0291(3) 0.0218(3) -0.00172(19) 0.00012(19) -0.00132(19) C11 0.0263(8) 0.0256(9) 0.0231(8) -0.0043(7) 0.0013(6) -0.0029(6) C12 0.0320(9) 0.0254(9) 0.0267(9) -0.0035(7) 0.0014(7) -0.0013(7) C13 0.0294(9) 0.0198(9) 0.0299(9) -0.0009(7) -0.0003(7) -0.0008(6) C14 0.0267(9) 0.0233(9) 0.0342(10) 0.0031(7) 0.0014(7) 0.0000(6) C15 0.0384(10) 0.0270(10) 0.0315(10) 0.0046(7) 0.0051(7) -0.0005(7) C16 0.0389(11) 0.0340(11) 0.0302(10) 0.0044(8) -0.0060(8) -0.0007(8) C17 0.0281(10) 0.0396(12) 0.0434(11) 0.0023(9) -0.0033(8) 0.0036(8) C18 0.0296(10) 0.0343(10) 0.0340(10) -0.0024(8) 0.0035(7) 0.0026(7) C21 0.0302(9) 0.0288(10) 0.0259(9) -0.0014(7) -0.0004(7) 0.0017(7) C22 0.0283(9) 0.0248(9) 0.0294(9) -0.0053(7) 0.0016(7) 0.0003(7) C23 0.0301(9) 0.0277(9) 0.0255(9) -0.0022(7) -0.0009(7) 0.0051(7) C24 0.0321(10) 0.0334(11) 0.0378(11) -0.0010(8) -0.0015(8) 0.0031(8) C25 0.0363(11) 0.0472(13) 0.0409(12) -0.0038(9) -0.0107(8) 0.0113(9) C26 0.0608(14) 0.0422(13) 0.0322(11) 0.0037(9) -0.0061(9) 0.0205(10) C27 0.0592(14) 0.0393(12) 0.0459(13) 0.0142(10) 0.0108(10) 0.0049(10) C28 0.0371(11) 0.0359(11) 0.0416(11) 0.0060(9) 0.0011(8) 0.0003(8) C31 0.0292(9) 0.0263(9) 0.0320(10) 0.0049(7) 0.0064(7) 0.0045(7) C32 0.0347(11) 0.0457(13) 0.0496(13) 0.0048(10) 0.0029(9) -0.0026(9) C33 0.0331(12) 0.0602(16) 0.087(2) 0.0194(14) 0.0140(11) -0.0014(10) C34 0.0519(15) 0.0647(16) 0.0675(18) 0.0287(13) 0.0317(12) 0.0200(12) C35 0.0561(15) 0.0655(16) 0.0408(13) 0.0118(11) 0.0187(10) 0.0195(11) C36 0.0395(11) 0.0443(12) 0.0341(11) 0.0036(8) 0.0071(8) 0.0081(8) C41 0.0263(9) 0.0287(9) 0.0234(9) -0.0043(7) 0.0028(6) -0.0007(7) C42 0.0344(10) 0.0323(11) 0.0338(10) 0.0017(8) -0.0007(7) -0.0009(7) C43 0.0450(12) 0.0299(11) 0.0464(12) 0.0013(9) 0.0005(9) -0.0085(8) C44 0.0341(11) 0.0438(13) 0.0444(12) -0.0075(9) -0.0009(8) -0.0101(8) C45 0.0326(10) 0.0412(12) 0.0374(11) -0.0034(9) -0.0070(8) -0.0005(8) C46 0.0363(10) 0.0304(10) 0.0313(10) -0.0012(8) -0.0033(7) 0.0005(7) C51 0.0311(10) 0.0381(11) 0.0333(10) 0.0043(8) 0.0057(7) -0.0005(8) C52 0.0315(10) 0.0434(12) 0.0341(11) -0.0027(9) 0.0068(8) -0.0058(8) C521 0.0483(13) 0.0631(16) 0.0545(14) 0.0171(12) 0.0240(10) 0.0198(11) C522 0.0497(15) 0.100(2) 0.0615(17) -0.0293(16) 0.0096(12) -0.0355(15) C523 0.0379(12) 0.0522(14) 0.0565(15) 0.0071(10) 0.0161(10) -0.0082(9) C61 0.0269(9) 0.0357(10) 0.0258(9) -0.0027(7) 0.0004(7) 0.0012(7) C62 0.0263(9) 0.0347(10) 0.0257(9) -0.0020(7) -0.0021(7) -0.0043(7) C621 0.0487(12) 0.0418(12) 0.0385(11) 0.0061(9) -0.0030(9) -0.0111(9) C622 0.0376(11) 0.0386(11) 0.0395(11) -0.0107(9) 0.0039(8) 0.0003(8) C623 0.0320(10) 0.0475(13) 0.0389(11) -0.0073(9) -0.0061(8) -0.0057(8) _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 C41 1.9458(17) . ? Ge1 C11 1.9486(17) . ? Ge1 C21 1.9503(18) . ? Ge1 C31 1.9515(18) . ? Al1 C51 1.978(2) . ? Al1 C61 1.9809(18) . ? Al1 C11 1.9939(18) . ? Al1 C21 2.4811(18) . ? C11 C12 1.334(3) . ? C12 C13 1.481(2) . ? C12 H12 0.9600 . ? C13 C14 1.394(3) . ? C13 C18 1.399(3) . ? C14 C15 1.380(3) . ? C14 H14 0.9600 . ? C15 C16 1.387(3) . ? C15 H15 0.9600 . ? C16 C17 1.381(3) . ? C16 H16 0.9600 . ? C17 C18 1.383(3) . ? C17 H17 0.9600 . ? C18 H18 0.9600 . ? C21 C22 1.203(3) . ? C22 C23 1.439(2) . ? C23 C28 1.391(3) . ? C23 C24 1.392(3) . ? C24 C25 1.382(3) . ? C24 H24 0.9600 . ? C25 C26 1.374(3) . ? C25 H25 0.9600 . ? C26 C27 1.374(3) . ? C26 H26 0.9600 . ? C27 C28 1.380(3) . ? C27 H27 0.9600 . ? C28 H28 0.9600 . ? C31 C36 1.388(3) . ? C31 C32 1.390(3) . ? C32 C33 1.387(3) . ? C32 H32 0.9600 . ? C33 C34 1.376(4) . ? C33 H33 0.9600 . ? C34 C35 1.374(4) . ? C34 H34 0.9600 . ? C35 C36 1.389(3) . ? C35 H35 0.9600 . ? C36 H36 0.9600 . ? C41 C42 1.390(3) . ? C41 C46 1.397(2) . ? C42 C43 1.389(3) . ? C42 H42 0.9600 . ? C43 C44 1.377(3) . ? C43 H43 0.9600 . ? C44 C45 1.377(3) . ? C44 H44 0.9600 . ? C45 C46 1.384(3) . ? C45 H45 0.9600 . ? C46 H46 0.9600 . ? C51 C52 1.539(3) . ? C51 H51A 0.9600 . ? C51 H51B 0.9600 . ? C52 C521 1.516(3) . ? C52 C522 1.521(3) . ? C52 C523 1.539(3) . ? C521 H52A 0.9599 . ? C521 H52B 0.9599 . ? C521 H52C 0.9599 . ? C522 H52D 0.9599 . ? C522 H52E 0.9599 . ? C522 H52F 0.9599 . ? C523 H52G 0.9599 . ? C523 H52H 0.9599 . ? C523 H52I 0.9599 . ? C61 C62 1.536(3) . ? C61 H61A 0.9600 . ? C61 H61B 0.9600 . ? C62 C621 1.523(3) . ? C62 C622 1.533(3) . ? C62 C623 1.534(2) . ? C621 H62A 0.9599 . ? C621 H62B 0.9599 . ? C621 H62C 0.9599 . ? C622 H62D 0.9599 . ? C622 H62E 0.9599 . ? C622 H62F 0.9599 . ? C623 H62G 0.9599 . ? C623 H62H 0.9599 . ? C623 H62I 0.9599 . ? 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 C41 Ge1 C11 118.60(7) . . ? C41 Ge1 C21 105.42(7) . . ? C11 Ge1 C21 93.21(7) . . ? C41 Ge1 C31 110.78(7) . . ? C11 Ge1 C31 119.44(7) . . ? C21 Ge1 C31 105.65(7) . . ? C51 Al1 C61 116.31(8) . . ? C51 Al1 C11 121.03(8) . . ? C61 Al1 C11 119.88(8) . . ? C51 Al1 C21 106.22(8) . . ? C61 Al1 C21 102.83(7) . . ? C11 Al1 C21 77.71(7) . . ? C12 C11 Ge1 124.60(13) . . ? C12 C11 Al1 132.44(13) . . ? Ge1 C11 Al1 102.26(8) . . ? C11 C12 C13 127.35(16) . . ? C11 C12 H12 116.3 . . ? C13 C12 H12 116.3 . . ? C14 C13 C18 118.17(16) . . ? C14 C13 C12 122.00(16) . . ? C18 C13 C12 119.81(16) . . ? C15 C14 C13 120.88(17) . . ? C15 C14 H14 119.6 . . ? C13 C14 H14 119.6 . . ? C14 C15 C16 120.28(18) . . ? C14 C15 H15 119.9 . . ? C16 C15 H15 119.9 . . ? C17 C16 C15 119.57(17) . . ? C17 C16 H16 120.2 . . ? C15 C16 H16 120.2 . . ? C16 C17 C18 120.33(18) . . ? C16 C17 H17 119.8 . . ? C18 C17 H17 119.8 . . ? C17 C18 C13 120.70(18) . . ? C17 C18 H18 119.7 . . ? C13 C18 H18 119.7 . . ? C22 C21 Ge1 176.47(16) . . ? C22 C21 Al1 89.99(12) . . ? Ge1 C21 Al1 86.82(7) . . ? C21 C22 C23 176.97(19) . . ? C28 C23 C24 119.61(17) . . ? C28 C23 C22 119.79(17) . . ? C24 C23 C22 120.57(17) . . ? C25 C24 C23 119.68(19) . . ? C25 C24 H24 120.2 . . ? C23 C24 H24 120.2 . . ? C26 C25 C24 120.4(2) . . ? C26 C25 H25 119.8 . . ? C24 C25 H25 119.8 . . ? C25 C26 C27 120.11(19) . . ? C25 C26 H26 119.9 . . ? C27 C26 H26 119.9 . . ? C26 C27 C28 120.5(2) . . ? C26 C27 H27 119.8 . . ? C28 C27 H27 119.8 . . ? C27 C28 C23 119.72(19) . . ? C27 C28 H28 120.1 . . ? C23 C28 H28 120.1 . . ? C36 C31 C32 118.62(18) . . ? C36 C31 Ge1 120.73(15) . . ? C32 C31 Ge1 120.65(15) . . ? C33 C32 C31 120.2(2) . . ? C33 C32 H32 119.9 . . ? C31 C32 H32 119.9 . . ? C34 C33 C32 120.5(2) . . ? C34 C33 H33 119.8 . . ? C32 C33 H33 119.8 . . ? C35 C34 C33 120.0(2) . . ? C35 C34 H34 120.0 . . ? C33 C34 H34 120.0 . . ? C34 C35 C36 119.9(2) . . ? C34 C35 H35 120.1 . . ? C36 C35 H35 120.1 . . ? C31 C36 C35 120.8(2) . . ? C31 C36 H36 119.6 . . ? C35 C36 H36 119.6 . . ? C42 C41 C46 118.41(16) . . ? C42 C41 Ge1 120.13(13) . . ? C46 C41 Ge1 121.43(14) . . ? C43 C42 C41 120.74(18) . . ? C43 C42 H42 119.6 . . ? C41 C42 H42 119.6 . . ? C44 C43 C42 120.10(19) . . ? C44 C43 H43 120.0 . . ? C42 C43 H43 120.0 . . ? C43 C44 C45 119.83(18) . . ? C43 C44 H44 120.1 . . ? C45 C44 H44 120.1 . . ? C44 C45 C46 120.51(18) . . ? C44 C45 H45 119.7 . . ? C46 C45 H45 119.7 . . ? C45 C46 C41 120.40(18) . . ? C45 C46 H46 119.8 . . ? C41 C46 H46 119.8 . . ? C52 C51 Al1 122.23(14) . . ? C52 C51 H51A 106.8 . . ? Al1 C51 H51A 106.8 . . ? C52 C51 H51B 106.8 . . ? Al1 C51 H51B 106.8 . . ? H51A C51 H51B 106.6 . . ? C521 C52 C522 110.1(2) . . ? C521 C52 C51 109.56(18) . . ? C522 C52 C51 109.71(19) . . ? C521 C52 C523 108.11(18) . . ? C522 C52 C523 109.26(19) . . ? C51 C52 C523 110.05(17) . . ? C52 C521 H52A 109.5 . . ? C52 C521 H52B 109.5 . . ? H52A C521 H52B 109.5 . . ? C52 C521 H52C 109.5 . . ? H52A C521 H52C 109.5 . . ? H52B C521 H52C 109.5 . . ? C52 C522 H52D 109.5 . . ? C52 C522 H52E 109.5 . . ? H52D C522 H52E 109.5 . . ? C52 C522 H52F 109.5 . . ? H52D C522 H52F 109.5 . . ? H52E C522 H52F 109.5 . . ? C52 C523 H52G 109.5 . . ? C52 C523 H52H 109.5 . . ? H52G C523 H52H 109.5 . . ? C52 C523 H52I 109.5 . . ? H52G C523 H52I 109.5 . . ? H52H C523 H52I 109.5 . . ? C62 C61 Al1 117.83(12) . . ? C62 C61 H61A 107.8 . . ? Al1 C61 H61A 107.8 . . ? C62 C61 H61B 107.8 . . ? Al1 C61 H61B 107.8 . . ? H61A C61 H61B 107.2 . . ? C621 C62 C622 108.52(17) . . ? C621 C62 C623 109.19(16) . . ? C622 C62 C623 108.19(15) . . ? C621 C62 C61 110.48(16) . . ? C622 C62 C61 109.96(15) . . ? C623 C62 C61 110.45(15) . . ? C62 C621 H62A 109.5 . . ? C62 C621 H62B 109.5 . . ? H62A C621 H62B 109.5 . . ? C62 C621 H62C 109.5 . . ? H62A C621 H62C 109.5 . . ? H62B C621 H62C 109.5 . . ? C62 C622 H62D 109.5 . . ? C62 C622 H62E 109.5 . . ? H62D C622 H62E 109.5 . . ? C62 C622 H62F 109.5 . . ? H62D C622 H62F 109.5 . . ? H62E C622 H62F 109.5 . . ? C62 C623 H62G 109.5 . . ? C62 C623 H62H 109.5 . . ? H62G C623 H62H 109.5 . . ? C62 C623 H62I 109.5 . . ? H62G C623 H62I 109.5 . . ? H62H C623 H62I 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 C41 Ge1 C11 C12 -62.32(18) . . . . ? C21 Ge1 C11 C12 -171.83(16) . . . . ? C31 Ge1 C11 C12 78.18(17) . . . . ? C41 Ge1 C11 Al1 109.14(8) . . . . ? C21 Ge1 C11 Al1 -0.37(8) . . . . ? C31 Ge1 C11 Al1 -110.36(9) . . . . ? C51 Al1 C11 C12 69.1(2) . . . . ? C61 Al1 C11 C12 -91.37(19) . . . . ? C21 Al1 C11 C12 170.76(19) . . . . ? C51 Al1 C11 Ge1 -101.39(10) . . . . ? C61 Al1 C11 Ge1 98.16(9) . . . . ? C21 Al1 C11 Ge1 0.29(7) . . . . ? Ge1 C11 C12 C13 -4.1(3) . . . . ? Al1 C11 C12 C13 -172.76(14) . . . . ? C11 C12 C13 C14 -47.2(3) . . . . ? C11 C12 C13 C18 131.2(2) . . . . ? C18 C13 C14 C15 -2.5(3) . . . . ? C12 C13 C14 C15 175.85(16) . . . . ? C13 C14 C15 C16 0.3(3) . . . . ? C14 C15 C16 C17 1.5(3) . . . . ? C15 C16 C17 C18 -1.0(3) . . . . ? C16 C17 C18 C13 -1.4(3) . . . . ? C14 C13 C18 C17 3.0(3) . . . . ? C12 C13 C18 C17 -175.34(17) . . . . ? C41 Ge1 C21 C22 -146(3) . . . . ? C11 Ge1 C21 C22 -25(3) . . . . ? C31 Ge1 C21 C22 97(3) . . . . ? C41 Ge1 C21 Al1 -120.56(6) . . . . ? C11 Ge1 C21 Al1 0.29(7) . . . . ? C31 Ge1 C21 Al1 122.09(7) . . . . ? C51 Al1 C21 C22 -62.72(14) . . . . ? C61 Al1 C21 C22 59.94(14) . . . . ? C11 Al1 C21 C22 178.19(14) . . . . ? C51 Al1 C21 Ge1 118.80(8) . . . . ? C61 Al1 C21 Ge1 -118.54(7) . . . . ? C11 Al1 C21 Ge1 -0.29(7) . . . . ? Ge1 C21 C22 C23 -178(100) . . . . ? Al1 C21 C22 C23 156(4) . . . . ? C21 C22 C23 C28 -56(4) . . . . ? C21 C22 C23 C24 122(4) . . . . ? C28 C23 C24 C25 0.0(3) . . . . ? C22 C23 C24 C25 -177.97(18) . . . . ? C23 C24 C25 C26 0.5(3) . . . . ? C24 C25 C26 C27 -0.2(3) . . . . ? C25 C26 C27 C28 -0.7(3) . . . . ? C26 C27 C28 C23 1.1(3) . . . . ? C24 C23 C28 C27 -0.8(3) . . . . ? C22 C23 C28 C27 177.16(19) . . . . ? C41 Ge1 C31 C36 16.81(17) . . . . ? C11 Ge1 C31 C36 -126.51(15) . . . . ? C21 Ge1 C31 C36 130.49(15) . . . . ? C41 Ge1 C31 C32 -162.85(15) . . . . ? C11 Ge1 C31 C32 53.82(18) . . . . ? C21 Ge1 C31 C32 -49.17(17) . . . . ? C36 C31 C32 C33 0.2(3) . . . . ? Ge1 C31 C32 C33 179.89(17) . . . . ? C31 C32 C33 C34 0.0(4) . . . . ? C32 C33 C34 C35 -0.5(4) . . . . ? C33 C34 C35 C36 0.7(4) . . . . ? C32 C31 C36 C35 0.0(3) . . . . ? Ge1 C31 C36 C35 -179.69(16) . . . . ? C34 C35 C36 C31 -0.4(3) . . . . ? C11 Ge1 C41 C42 -115.20(15) . . . . ? C21 Ge1 C41 C42 -12.70(17) . . . . ? C31 Ge1 C41 C42 101.13(15) . . . . ? C11 Ge1 C41 C46 66.93(17) . . . . ? C21 Ge1 C41 C46 169.43(15) . . . . ? C31 Ge1 C41 C46 -76.74(16) . . . . ? C46 C41 C42 C43 0.2(3) . . . . ? Ge1 C41 C42 C43 -177.77(15) . . . . ? C41 C42 C43 C44 0.6(3) . . . . ? C42 C43 C44 C45 -1.1(3) . . . . ? C43 C44 C45 C46 0.9(3) . . . . ? C44 C45 C46 C41 -0.1(3) . . . . ? C42 C41 C46 C45 -0.4(3) . . . . ? Ge1 C41 C46 C45 177.54(15) . . . . ? C61 Al1 C51 C52 150.12(16) . . . . ? C11 Al1 C51 C52 -11.0(2) . . . . ? C21 Al1 C51 C52 -96.18(17) . . . . ? Al1 C51 C52 C521 -58.9(2) . . . . ? Al1 C51 C52 C522 62.1(2) . . . . ? Al1 C51 C52 C523 -177.61(15) . . . . ? C51 Al1 C61 C62 -87.42(16) . . . . ? C11 Al1 C61 C62 73.91(16) . . . . ? C21 Al1 C61 C62 156.97(13) . . . . ? Al1 C61 C62 C621 -70.10(18) . . . . ? Al1 C61 C62 C622 49.66(19) . . . . ? Al1 C61 C62 C623 168.99(13) . . . . ? _diffrn_measured_fraction_theta_max 0.907 _diffrn_reflns_theta_full 72.04 _diffrn_measured_fraction_theta_full 0.907 _refine_diff_density_max 0.546 _refine_diff_density_min -0.275 _refine_diff_density_rms 0.053