data_segeme2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C31 H47 Al Ge N2 Se2' _chemical_formula_weight 705.20 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'H' 'H' 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'N' 'N' 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Al' 'Al' 0.0645 0.0514 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ge' 'Ge' 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Se' 'Se' -0.0929 2.2259 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting ? _symmetry_space_group_name_H-M ? loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, -y-1/2, z-1/2' _cell_length_a 11.9939(10) _cell_length_b 17.4552(9) _cell_length_c 16.0281(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.686(6) _cell_angle_gamma 90.00 _cell_volume 3355.3(4) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used ? _cell_measurement_theta_min ? _cell_measurement_theta_max ? _exptl_crystal_description ? _exptl_crystal_colour ? _exptl_crystal_size_max ? _exptl_crystal_size_mid ? _exptl_crystal_size_min ? _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.396 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1440 _exptl_absorpt_coefficient_mu 3.130 _exptl_absorpt_correction_type ? _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 133(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type ? _diffrn_measurement_method ? _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 17451 _diffrn_reflns_av_R_equivalents 0.0553 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -18 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 1.72 _diffrn_reflns_theta_max 24.83 _reflns_number_total 5748 _reflns_number_gt 4447 _reflns_threshold_expression >2sigma(I) _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refinement of F^2^ against ALL reflections. The weighted R-factor wR and goodness of fit S are based on F^2^, conventional R-factors R are based on F, with F set to zero for negative F^2^. The threshold expression of F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is not relevant to the choice of reflections for refinement. R-factors based on F^2^ are statistically about twice as large as those based on F, and R- factors based on ALL data will be even larger. ; _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^)+(0.0319P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 5748 _refine_ls_number_parameters 334 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0463 _refine_ls_R_factor_gt 0.0301 _refine_ls_wR_factor_ref 0.0667 _refine_ls_wR_factor_gt 0.0630 _refine_ls_goodness_of_fit_ref 0.963 _refine_ls_restrained_S_all 0.963 _refine_ls_shift/su_max 0.001 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Al1 Al 0.36362(7) 0.35969(5) 0.81923(5) 0.01954(19) Uani 1 1 d . . . Ge1 Ge 0.43328(3) 0.200139(18) 0.87185(2) 0.02413(9) Uani 1 1 d . . . Se1 Se 0.28724(3) 0.239719(18) 0.78285(2) 0.03001(9) Uani 1 1 d . . . Se2 Se 0.52608(2) 0.317550(18) 0.89092(2) 0.02499(9) Uani 1 1 d . . . N1 N 0.2758(2) 0.42676(14) 0.88444(15) 0.0216(5) Uani 1 1 d . . . N2 N 0.38362(19) 0.42446(14) 0.72689(15) 0.0206(5) Uani 1 1 d . . . C1 C 0.2160(3) 0.55628(19) 0.9294(2) 0.0344(8) Uani 1 1 d . . . H1A H 0.1837 0.5271 0.9754 0.052 Uiso 1 1 calc R . . H1B H 0.1566 0.5835 0.8991 0.052 Uiso 1 1 calc R . . H1C H 0.2699 0.5934 0.9517 0.052 Uiso 1 1 calc R . . C2 C 0.2741(2) 0.50212(17) 0.8707(2) 0.0239(7) Uani 1 1 d . . . C3 C 0.3246(2) 0.53658(17) 0.80214(19) 0.0240(7) Uani 1 1 d . . . H3A H 0.3292 0.5909 0.8033 0.029 Uiso 1 1 calc R . . C4 C 0.3693(2) 0.50086(17) 0.73217(19) 0.0213(6) Uani 1 1 d . . . C5 C 0.4032(3) 0.55207(18) 0.6616(2) 0.0305(7) Uani 1 1 d . . . H5A H 0.4343 0.5210 0.6167 0.046 Uiso 1 1 calc R . . H5B H 0.4595 0.5886 0.6816 0.046 Uiso 1 1 calc R . . H5C H 0.3378 0.5801 0.6406 0.046 Uiso 1 1 calc R . . C6 C 0.2049(2) 0.39584(17) 0.94946(19) 0.0220(6) Uani 1 1 d . . . C7 C 0.0943(2) 0.37547(17) 0.9274(2) 0.0242(7) Uani 1 1 d . . . C8 C 0.0267(3) 0.34518(18) 0.9889(2) 0.0279(7) Uani 1 1 d . . . H8A H -0.0479 0.3314 0.9751 0.034 Uiso 1 1 calc R . . C9 C 0.0653(3) 0.33452(18) 1.0698(2) 0.0308(8) Uani 1 1 d . . . H9A H 0.0182 0.3130 1.1109 0.037 Uiso 1 1 calc R . . C10 C 0.1731(3) 0.35549(18) 1.0900(2) 0.0285(7) Uani 1 1 d . . . H10A H 0.1992 0.3484 1.1457 0.034 Uiso 1 1 calc R . . C11 C 0.2448(3) 0.38672(17) 1.0316(2) 0.0254(7) Uani 1 1 d . . . C12 C 0.4240(3) 0.3457(2) 1.1047(2) 0.0375(8) Uani 1 1 d . . . H12A H 0.4284 0.3014 1.0673 0.056 Uiso 1 1 calc R . . H12B H 0.3842 0.3311 1.1554 0.056 Uiso 1 1 calc R . . H12C H 0.4995 0.3627 1.1197 0.056 Uiso 1 1 calc R . . C13 C 0.3611(3) 0.41116(19) 1.0604(2) 0.0276(7) Uani 1 1 d . . . H13A H 0.4044 0.4262 1.0101 0.033 Uiso 1 1 calc R . . C14 C 0.3559(3) 0.4804(2) 1.1188(2) 0.0416(9) Uani 1 1 d . . . H14A H 0.3174 0.5227 1.0905 0.062 Uiso 1 1 calc R . . H14B H 0.4318 0.4964 1.1341 0.062 Uiso 1 1 calc R . . H14C H 0.3153 0.4665 1.1693 0.062 Uiso 1 1 calc R . . C15 C -0.0098(3) 0.3155(2) 0.8055(2) 0.0403(9) Uani 1 1 d . . . H15A H 0.0437 0.2730 0.8067 0.061 Uiso 1 1 calc R . . H15B H -0.0344 0.3248 0.7478 0.061 Uiso 1 1 calc R . . H15C H -0.0743 0.3023 0.8396 0.061 Uiso 1 1 calc R . . C16 C 0.0458(3) 0.3875(2) 0.8403(2) 0.0312(8) Uani 1 1 d . . . H16A H 0.1085 0.4013 0.8026 0.037 Uiso 1 1 calc R . . C17 C -0.0367(4) 0.4541(2) 0.8397(3) 0.0521(11) Uani 1 1 d . . . H17A H -0.0011 0.4995 0.8640 0.078 Uiso 1 1 calc R . . H17B H -0.1022 0.4403 0.8725 0.078 Uiso 1 1 calc R . . H17C H -0.0600 0.4651 0.7821 0.078 Uiso 1 1 calc R . . C18 C 0.4132(2) 0.39355(17) 0.64562(19) 0.0224(7) Uani 1 1 d . . . C19 C 0.3260(3) 0.36908(18) 0.5924(2) 0.0262(7) Uani 1 1 d . . . C20 C 0.3535(3) 0.34295(19) 0.5131(2) 0.0320(8) Uani 1 1 d . . . H20A H 0.2960 0.3258 0.4764 0.038 Uiso 1 1 calc R . . C21 C 0.4626(3) 0.34150(19) 0.4870(2) 0.0333(8) Uani 1 1 d . . . H21A H 0.4797 0.3253 0.4320 0.040 Uiso 1 1 calc R . . C22 C 0.5465(3) 0.36360(18) 0.5409(2) 0.0299(7) Uani 1 1 d . . . H22A H 0.6216 0.3607 0.5229 0.036 Uiso 1 1 calc R . . C23 C 0.5250(3) 0.39003(17) 0.6209(2) 0.0253(7) Uani 1 1 d . . . C24 C 0.6949(3) 0.4752(2) 0.6390(2) 0.0399(9) Uani 1 1 d . . . H24A H 0.6484 0.5198 0.6257 0.060 Uiso 1 1 calc R . . H24B H 0.7291 0.4560 0.5879 0.060 Uiso 1 1 calc R . . H24C H 0.7535 0.4901 0.6790 0.060 Uiso 1 1 calc R . . C25 C 0.6225(3) 0.41216(19) 0.6774(2) 0.0295(7) Uani 1 1 d . . . H25A H 0.5916 0.4322 0.7308 0.035 Uiso 1 1 calc R . . C26 C 0.6943(3) 0.3421(2) 0.6979(2) 0.0383(9) Uani 1 1 d . . . H26A H 0.6481 0.3026 0.7237 0.058 Uiso 1 1 calc R . . H26B H 0.7544 0.3570 0.7367 0.058 Uiso 1 1 calc R . . H26C H 0.7266 0.3220 0.6465 0.058 Uiso 1 1 calc R . . C27 C 0.1400(3) 0.3003(2) 0.5900(2) 0.0401(9) Uani 1 1 d . . . H27A H 0.1786 0.2540 0.6094 0.060 Uiso 1 1 calc R . . H27B H 0.1351 0.2998 0.5289 0.060 Uiso 1 1 calc R . . H27C H 0.0647 0.3016 0.6131 0.060 Uiso 1 1 calc R . . C28 C 0.2047(3) 0.37112(19) 0.6189(2) 0.0302(7) Uani 1 1 d . . . H28A H 0.2042 0.3714 0.6812 0.036 Uiso 1 1 calc R . . C29 C 0.1466(3) 0.4439(2) 0.5894(3) 0.0453(10) Uani 1 1 d . . . H29A H 0.1900 0.4886 0.6076 0.068 Uiso 1 1 calc R . . H29B H 0.0719 0.4464 0.6133 0.068 Uiso 1 1 calc R . . H29C H 0.1406 0.4436 0.5284 0.068 Uiso 1 1 calc R . . C30 C 0.3680(3) 0.1601(2) 0.9733(2) 0.0366(8) Uani 1 1 d . . . H30A H 0.4275 0.1432 1.0115 0.055 Uiso 1 1 calc R . . H30B H 0.3195 0.1166 0.9594 0.055 Uiso 1 1 calc R . . H30C H 0.3241 0.2003 1.0001 0.055 Uiso 1 1 calc R . . C31 C 0.5291(3) 0.1246(2) 0.8200(3) 0.0470(10) Uani 1 1 d . . . H31A H 0.5886 0.1099 0.8592 0.071 Uiso 1 1 calc R . . H31B H 0.5619 0.1465 0.7697 0.071 Uiso 1 1 calc R . . H31C H 0.4850 0.0793 0.8049 0.071 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 Al1 0.0212(4) 0.0153(4) 0.0221(5) -0.0010(4) -0.0012(3) -0.0001(3) Ge1 0.02946(18) 0.01803(17) 0.02496(18) 0.00210(14) 0.00283(13) 0.00200(13) Se1 0.03637(18) 0.01799(16) 0.03540(19) -0.00025(14) -0.01074(14) -0.00489(13) Se2 0.02150(15) 0.02319(17) 0.03021(18) 0.00361(13) -0.00275(12) -0.00029(12) N1 0.0238(13) 0.0198(13) 0.0212(14) 0.0001(11) 0.0006(10) -0.0001(10) N2 0.0204(12) 0.0189(13) 0.0224(13) -0.0019(11) 0.0003(10) 0.0004(10) C1 0.0422(19) 0.0219(17) 0.039(2) -0.0023(15) 0.0153(16) 0.0062(15) C2 0.0230(15) 0.0217(16) 0.0268(17) -0.0001(13) -0.0006(13) 0.0017(12) C3 0.0256(16) 0.0165(15) 0.0300(18) -0.0036(13) -0.0020(13) -0.0013(12) C4 0.0194(14) 0.0188(15) 0.0255(16) 0.0019(13) -0.0028(12) 0.0015(12) C5 0.0383(18) 0.0213(16) 0.0320(19) 0.0047(15) 0.0055(15) 0.0031(14) C6 0.0232(15) 0.0175(15) 0.0254(17) -0.0003(13) 0.0040(12) 0.0039(12) C7 0.0233(15) 0.0201(15) 0.0293(17) -0.0001(14) -0.0003(13) -0.0011(12) C8 0.0263(16) 0.0239(16) 0.0336(19) 0.0016(14) 0.0034(14) -0.0041(13) C9 0.0362(18) 0.0250(18) 0.0314(19) 0.0005(15) 0.0104(15) -0.0029(14) C10 0.0349(17) 0.0257(17) 0.0248(17) -0.0014(14) 0.0006(14) 0.0008(14) C11 0.0285(16) 0.0192(16) 0.0284(18) -0.0028(13) 0.0000(13) 0.0027(13) C12 0.0368(19) 0.036(2) 0.040(2) -0.0047(17) -0.0122(16) 0.0052(16) C13 0.0273(16) 0.0291(18) 0.0264(17) -0.0030(14) -0.0033(13) -0.0006(13) C14 0.042(2) 0.033(2) 0.049(2) -0.0149(18) -0.0070(18) -0.0020(16) C15 0.0310(18) 0.052(2) 0.038(2) -0.0014(18) -0.0109(15) -0.0018(16) C16 0.0225(16) 0.040(2) 0.0306(19) 0.0066(15) -0.0028(14) -0.0020(14) C17 0.061(3) 0.044(2) 0.051(3) 0.008(2) -0.015(2) 0.010(2) C18 0.0312(16) 0.0157(15) 0.0204(16) 0.0018(12) -0.0001(13) -0.0004(12) C19 0.0343(17) 0.0200(16) 0.0241(17) 0.0012(13) -0.0056(14) -0.0009(13) C20 0.0432(19) 0.0248(17) 0.0279(18) 0.0002(14) -0.0087(15) -0.0018(14) C21 0.053(2) 0.0233(17) 0.0240(18) -0.0011(14) 0.0028(16) -0.0001(15) C22 0.0393(18) 0.0234(17) 0.0270(18) 0.0009(14) 0.0069(14) 0.0043(14) C23 0.0312(17) 0.0176(16) 0.0271(18) 0.0018(13) 0.0003(14) 0.0016(13) C24 0.0329(19) 0.041(2) 0.046(2) -0.0031(18) 0.0073(16) -0.0058(16) C25 0.0278(17) 0.0325(19) 0.0283(18) -0.0055(15) 0.0042(14) -0.0001(14) C26 0.0283(17) 0.048(2) 0.039(2) -0.0009(18) 0.0030(15) 0.0078(16) C27 0.039(2) 0.036(2) 0.046(2) -0.0004(18) -0.0132(17) -0.0087(16) C28 0.0307(17) 0.0294(18) 0.0304(19) -0.0025(15) -0.0075(14) -0.0013(14) C29 0.040(2) 0.038(2) 0.058(3) 0.0028(19) -0.0083(19) 0.0063(17) C30 0.042(2) 0.036(2) 0.032(2) 0.0074(16) -0.0028(16) -0.0109(16) C31 0.056(2) 0.033(2) 0.053(3) -0.0022(19) 0.013(2) 0.0125(18) _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 Al1 N2 1.880(3) . ? Al1 N1 1.897(3) . ? Al1 Se1 2.3563(9) . ? Al1 Se2 2.3673(9) . ? Ge1 C31 1.942(3) . ? Ge1 C30 1.943(3) . ? Ge1 Se1 2.3496(5) . ? Ge1 Se2 2.3503(5) . ? N1 C2 1.334(4) . ? N1 C6 1.457(4) . ? N2 C4 1.347(4) . ? N2 C18 1.458(4) . ? C1 C2 1.509(4) . ? C2 C3 1.398(4) . ? C3 C4 1.396(4) . ? C4 C5 1.501(4) . ? C6 C11 1.404(4) . ? C6 C7 1.414(4) . ? C7 C8 1.389(4) . ? C7 C16 1.521(4) . ? C8 C9 1.385(5) . ? C9 C10 1.378(5) . ? C10 C11 1.391(4) . ? C11 C13 1.525(4) . ? C12 C13 1.539(5) . ? C13 C14 1.530(5) . ? C15 C16 1.526(5) . ? C16 C17 1.526(5) . ? C18 C23 1.404(4) . ? C18 C19 1.409(4) . ? C19 C20 1.393(5) . ? C19 C28 1.520(4) . ? C20 C21 1.379(5) . ? C21 C22 1.374(5) . ? C22 C23 1.391(4) . ? C23 C25 1.520(4) . ? C24 C25 1.535(5) . ? C25 C26 1.529(5) . ? C27 C28 1.529(4) . ? C28 C29 1.522(5) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag N2 Al1 N1 98.03(11) . . ? N2 Al1 Se1 113.11(8) . . ? N1 Al1 Se1 117.91(8) . . ? N2 Al1 Se2 117.19(8) . . ? N1 Al1 Se2 112.55(8) . . ? Se1 Al1 Se2 99.16(3) . . ? C31 Ge1 C30 111.10(17) . . ? C31 Ge1 Se1 112.35(13) . . ? C30 Ge1 Se1 107.99(11) . . ? C31 Ge1 Se2 111.48(12) . . ? C30 Ge1 Se2 113.57(11) . . ? Se1 Ge1 Se2 99.844(16) . . ? Ge1 Se1 Al1 79.99(2) . . ? Ge1 Se2 Al1 79.75(2) . . ? C2 N1 C6 118.4(2) . . ? C2 N1 Al1 121.7(2) . . ? C6 N1 Al1 119.89(19) . . ? C4 N2 C18 117.1(2) . . ? C4 N2 Al1 121.9(2) . . ? C18 N2 Al1 121.05(19) . . ? N1 C2 C3 123.2(3) . . ? N1 C2 C1 121.4(3) . . ? C3 C2 C1 115.3(3) . . ? C4 C3 C2 127.9(3) . . ? N2 C4 C3 122.9(3) . . ? N2 C4 C5 120.4(3) . . ? C3 C4 C5 116.7(3) . . ? C11 C6 C7 120.9(3) . . ? C11 C6 N1 121.1(3) . . ? C7 C6 N1 117.9(3) . . ? C8 C7 C6 118.2(3) . . ? C8 C7 C16 119.0(3) . . ? C6 C7 C16 122.8(3) . . ? C9 C8 C7 121.6(3) . . ? C10 C9 C8 119.1(3) . . ? C9 C10 C11 122.1(3) . . ? C10 C11 C6 118.0(3) . . ? C10 C11 C13 118.4(3) . . ? C6 C11 C13 123.6(3) . . ? C11 C13 C14 111.3(3) . . ? C11 C13 C12 111.9(3) . . ? C14 C13 C12 109.1(3) . . ? C7 C16 C17 110.7(3) . . ? C7 C16 C15 112.5(3) . . ? C17 C16 C15 110.2(3) . . ? C23 C18 C19 121.4(3) . . ? C23 C18 N2 120.8(3) . . ? C19 C18 N2 117.8(3) . . ? C20 C19 C18 118.0(3) . . ? C20 C19 C28 120.0(3) . . ? C18 C19 C28 122.0(3) . . ? C21 C20 C19 121.3(3) . . ? C22 C21 C20 119.6(3) . . ? C21 C22 C23 122.1(3) . . ? C22 C23 C18 117.6(3) . . ? C22 C23 C25 119.0(3) . . ? C18 C23 C25 123.5(3) . . ? C23 C25 C26 110.6(3) . . ? C23 C25 C24 112.3(3) . . ? C26 C25 C24 109.8(3) . . ? C19 C28 C29 111.7(3) . . ? C19 C28 C27 112.4(3) . . ? C29 C28 C27 110.6(3) . . ? _diffrn_measured_fraction_theta_max 0.993 _diffrn_reflns_theta_full 24.83 _diffrn_measured_fraction_theta_full 0.993 _refine_diff_density_max 0.459 _refine_diff_density_min -0.437 _refine_diff_density_rms 0.066