Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2002 data_global #============================================================================== _audit_creation_date 16-10-01 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 1. SUBMISSION DETAILS _journal_coden_Cambridge 186 loop_ _publ_author_name _publ_author_address 'Charles S. Weinert' ; Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; 'Phillip E. Fanwick' ; Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; 'Ian P. Rothwell' ; Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; _publ_contact_author_name 'Dr Ian P. Rothwell' _publ_contact_author_address ; Department of Chemistry Purdue University W. Lafayette IN 47907 USA ; _publ_contact_author_email 'rothwell@purdue.edu' _publ_contact_author_fax '1(765)4940239' _publ_contact_author_phone '1(765)4947012' _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Novel Germanium(II) Binaphthoxide Complexes: Synthesis and Crystal Structure of (R, R)-[Ge{OC20H10-(OSiMe3)-2'-(SiMe3)2-3,3'}2] and (R)-[Ge{O2C20H10(SiMe2Ph)2-3,3'}{NH3}] and the Catalytic Function of Ge[N(SiMe3)2]2 for the Mono-Silylation of 3,3-Disubstituted-1,1'-Bi-2,2' -naphthols ; _publ_section_references ; P. T. Beurskens, G. Beurskens, R. deGelder,S. Garcia-Granda, R. O. Gould, R. Israel, J. M. M. Smits, '(1999). The DIRDIF-99 Program System. 'Crystallography Laboratory, Univ. of Nijmegen, The Netherlands. Enraf-Nonius (1993), CAD4 Express, Enraf-Nonius, Delft, The Netherlands. Johnson, C.K. (1976). ORTEP. Report ORNL-5138. Oak Ridge National Laboratory, Tennessee, USA. Nonius(1998), Collect Users Manual, Nonius 'Delft, The Netherlands. Otwinowski Z. & Minor, W. (1997). Methods Enzymol., 276, 307-327. Sheldrick, G.M. (1997). SHELXL97, Program for the Refinement of Crystal Structures. Univ. of Gottingen, Germany. Spek A.L.(1997) PLATON. Program. Univ. of Ultrecht, The Netherlands Spek A.L.(1997) PLUTON. Molecular Graphics Program. Univ. of Ultrecht, The Netherlands ; data_Complex1 _database_code_CSD 176939 # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour colorless _exptl_crystal_size_max 0.45 _exptl_crystal_size_mid 0.30 _exptl_crystal_size_min 0.28 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C58 H74 Ge1 O4 Si6' _chemical_formula_moiety 'C58 H74 Ge1 O4 Si6' _chemical_formula_structural ? _chemical_formula_weight 1076.34 _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'p 1 21 1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z' _cell_length_a 11.0695(2) _cell_length_b 21.0832(4) _cell_length_c 12.8046(3) _cell_angle_alpha 90.00 _cell_angle_beta 99.7418(8) _cell_angle_gamma 90.00 _cell_volume 2945.25(19) _cell_measurement_reflns_used 29283 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_formula_units_z 2 _exptl_crystal_density_diffrn 1.21 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 0.673 _cell_measurement_temperature 149 _exptl_crystal_F_000 1140 # 6. DATA COLLECTION _diffrn_ambient_temperature 149 _diffrn_measurement_device_type Nonius_KappaCCD _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.7142 _exptl_absorpt_correction_T_max 0.8311 _diffrn_reflns_number 29283 _diffrn_measured_fraction_theta_max 0.9987 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.9987 _reflns_number_total 12785 _reflns_Friedl_coverage 0.9228 _reflns_number_gt 11736 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.059 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_k_min -25 _diffrn_reflns_limit_l_min -16 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_max 27 _diffrn_reflns_limit_l_max 16 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_gt 0.037 _refine_ls_wR_factor_ref 0.082 _refine_ls_hydrogen_treatment H_atoms_riding _refine_ls_number_reflns 12785 _refine_ls_number_parameters 640 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.024 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0391P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.046 _refine_diff_density_max 0.47 _refine_diff_density_min -0.84 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF99,_Beurskins,_1999) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) _refine_ls_abs_structure_details 'Flack H. D. (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.008(6) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag Ge 0.20560(3) 0.501785(16) -0.24800(2) 0.04147(9) Uani ? Si(12) 0.51754(6) 0.64749(4) -0.28432(6) 0.02836(19) Uani ? Si(21) 0.14237(6) 0.65508(4) 0.00046(5) 0.02792(17) Uani ? Si(22) -0.07879(6) 0.49473(4) -0.00397(6) 0.0328(2) Uani ? Si(32) 0.02569(6) 0.64935(4) -0.48629(5) 0.0300(2) Uani ? Si(41) 0.28034(7) 0.41985(4) -0.61550(6) 0.0337(2) Uani ? Si(42) 0.48558(6) 0.33668(4) -0.33643(6) 0.0321(2) Uani ? O(11) 0.33009(14) 0.55816(9) -0.22030(12) 0.0263(5) Uani ? O(21) 0.13348(14) 0.58181(8) -0.05055(13) 0.0255(4) Uani ? O(31) 0.16256(14) 0.53638(9) -0.37927(13) 0.0279(5) Uani ? O(41) 0.29974(14) 0.42023(9) -0.48285(13) 0.0300(5) Uani ? C(11) 0.40790(19) 0.57556(12) -0.13067(18) 0.0232(6) Uani ? C(12) 0.50654(19) 0.61589(12) -0.14870(19) 0.0241(6) Uani ? C(13) 0.5845(2) 0.63822(12) -0.0608(2) 0.0282(7) Uani ? C(14) 0.5696(2) 0.62391(12) 0.0438(2) 0.0266(6) Uani ? C(15) 0.6446(2) 0.65192(14) 0.1339(2) 0.0340(7) Uani ? C(16) 0.6265(2) 0.63821(14) 0.2339(2) 0.0401(8) Uani ? C(17) 0.5356(2) 0.59514(14) 0.2506(2) 0.0371(8) Uani ? C(18) 0.4614(2) 0.56701(13) 0.16569(19) 0.0311(7) Uani ? C(19) 0.4746(2) 0.58178(12) 0.05964(19) 0.0240(6) Uani ? C(1A) 0.39366(19) 0.55662(11) -0.02992(18) 0.0223(6) Uani ? C(21) 0.1781(2) 0.52298(12) -0.01588(17) 0.0236(6) Uani ? C(22) 0.0898(2) 0.47688(13) 0.00393(19) 0.0261(7) Uani ? C(23) 0.1318(2) 0.41666(13) 0.02880(19) 0.0281(7) Uani ? C(24) 0.2564(2) 0.39825(12) 0.03434(18) 0.0245(6) Uani ? C(25) 0.2963(2) 0.33566(13) 0.0579(2) 0.0297(7) Uani ? C(26) 0.4173(2) 0.31879(13) 0.0625(2) 0.0296(7) Uani ? C(27) 0.5018(2) 0.36531(13) 0.0432(2) 0.0302(7) Uani ? C(28) 0.4661(2) 0.42636(13) 0.01993(19) 0.0265(7) Uani ? C(29) 0.34187(19) 0.44509(12) 0.01440(18) 0.0226(6) Uani ? C(2A) 0.30068(18) 0.50868(12) -0.01072(16) 0.0212(6) Uani ? C(31) 0.06728(18) 0.51468(12) -0.45422(17) 0.0222(6) Uani ? C(32) -0.0073(2) 0.56271(12) -0.51189(18) 0.0237(6) Uani ? C(33) -0.1031(2) 0.54231(12) -0.58812(19) 0.0253(6) Uani ? C(34) -0.1303(2) 0.47805(12) -0.60993(18) 0.0240(6) Uani ? C(35) -0.2313(2) 0.45872(13) -0.68630(19) 0.0281(7) Uani ? C(36) -0.2580(2) 0.39609(14) -0.7046(2) 0.0330(7) Uani ? C(37) -0.1831(2) 0.34939(14) -0.6474(2) 0.0334(7) Uani ? C(38) -0.0848(2) 0.36660(13) -0.5730(2) 0.0302(7) Uani ? C(39) -0.05486(19) 0.43099(12) -0.55155(18) 0.0227(6) Uani ? C(3A) 0.0462(2) 0.45064(12) -0.47254(18) 0.0224(6) Uani ? C(41) 0.2422(2) 0.39075(12) -0.40942(18) 0.0241(6) Uani ? C(42) 0.3184(2) 0.35160(12) -0.33318(18) 0.0253(6) Uani ? C(43) 0.2631(2) 0.32215(12) -0.25740(19) 0.0260(6) Uani ? C(44) 0.1374(2) 0.32934(12) -0.25159(19) 0.0244(6) Uani ? C(45) 0.0823(2) 0.29726(13) -0.1751(2) 0.0295(7) Uani ? C(46) -0.0384(2) 0.30690(15) -0.1690(2) 0.0356(8) Uani ? C(47) -0.1081(2) 0.34939(15) -0.2383(2) 0.0367(8) Uani ? C(48) -0.0589(2) 0.38058(13) -0.3146(2) 0.0295(7) Uani ? C(49) 0.06567(19) 0.37075(12) -0.32482(18) 0.0234(6) Uani ? C(4A) 0.1206(2) 0.40260(12) -0.40398(17) 0.0234(6) Uani ? C(121) 0.3996(2) 0.71109(14) -0.3105(2) 0.0351(8) Uani ? C(122) 0.4985(3) 0.58750(16) -0.3920(2) 0.0464(9) Uani ? C(123) 0.6727(2) 0.68387(16) -0.2788(3) 0.0435(9) Uani ? C(211) 0.2578(3) 0.70486(14) -0.0499(2) 0.0404(9) Uani ? C(212) 0.1760(3) 0.64914(16) 0.1466(2) 0.0400(8) Uani ? C(213) -0.0102(2) 0.69038(15) -0.0523(2) 0.0362(8) Uani ? C(221) -0.1459(2) 0.52556(16) -0.1372(2) 0.0437(9) Uani ? C(222) -0.1598(2) 0.41961(16) 0.0206(3) 0.0456(9) Uani ? C(223) -0.1030(3) 0.55025(16) 0.1035(3) 0.0444(9) Uani ? C(321) 0.0348(3) 0.66812(15) -0.3429(2) 0.0377(8) Uani ? C(322) 0.1678(3) 0.67116(17) -0.5365(2) 0.0470(9) Uani ? C(323) -0.1044(3) 0.69610(15) -0.5600(3) 0.0528(10) Uani ? C(411) 0.1946(3) 0.34805(17) -0.6662(3) 0.0513(10) Uani ? C(412) 0.2025(2) 0.49286(16) -0.6737(2) 0.0415(8) Uani ? C(413) 0.4372(3) 0.4198(2) -0.6488(3) 0.0586(12) Uani ? C(421) 0.4979(3) 0.2814(2) -0.4473(3) 0.0665(12) Uani ? C(422) 0.5684(3) 0.4119(2) -0.3479(3) 0.0684(13) Uani ? C(423) 0.5555(2) 0.29532(15) -0.2116(2) 0.0370(8) Uani ? H(13) 0.6499 0.6639 -0.0711 0.0340 Uiso calc H(15) 0.7067 0.6799 0.1239 0.0410 Uiso calc H(16) 0.6749 0.6576 0.2916 0.0480 Uiso calc H(17) 0.5250 0.5854 0.3193 0.0440 Uiso calc H(18) 0.4020 0.5380 0.1779 0.0370 Uiso calc H(23) 0.0758 0.3862 0.0428 0.0340 Uiso calc H(25) 0.2399 0.3051 0.0705 0.0360 Uiso calc H(26) 0.4427 0.2773 0.0782 0.0350 Uiso calc H(27) 0.5836 0.3543 0.0464 0.0360 Uiso calc H(28) 0.5240 0.4562 0.0075 0.0320 Uiso calc H(33) -0.1523 0.5728 -0.6270 0.0300 Uiso calc H(35) -0.2805 0.4893 -0.7248 0.0340 Uiso calc H(36) -0.3252 0.3843 -0.7546 0.0400 Uiso calc H(37) -0.2007 0.3067 -0.6602 0.0400 Uiso calc H(38) -0.0366 0.3352 -0.5357 0.0360 Uiso calc H(43) 0.3108 0.2963 -0.2078 0.0310 Uiso calc H(45) 0.1286 0.2693 -0.1284 0.0350 Uiso calc H(46) -0.0742 0.2852 -0.1189 0.0430 Uiso calc H(47) -0.1895 0.3566 -0.2324 0.0440 Uiso calc H(48) -0.1071 0.4084 -0.3602 0.0350 Uiso calc H(12A) 0.4015 0.7295 -0.3788 0.0530 Uiso calc H(12B) 0.4166 0.7433 -0.2570 0.0530 Uiso calc H(12C) 0.3200 0.6933 -0.3093 0.0530 Uiso calc H(12D) 0.4207 0.5668 -0.3956 0.0700 Uiso calc H(12E) 0.5630 0.5566 -0.3778 0.0700 Uiso calc H(12F) 0.5021 0.6080 -0.4583 0.0700 Uiso calc H(12G) 0.6831 0.6966 -0.3487 0.0650 Uiso calc H(12H) 0.7346 0.6534 -0.2518 0.0650 Uiso calc H(12I) 0.6801 0.7203 -0.2331 0.0650 Uiso calc H(21A) 0.3385 0.6897 -0.0216 0.0610 Uiso calc H(21B) 0.2496 0.7480 -0.0283 0.0610 Uiso calc H(21C) 0.2451 0.7026 -0.1258 0.0610 Uiso calc H(21D) 0.1092 0.6284 0.1716 0.0600 Uiso calc H(21E) 0.1866 0.6909 0.1766 0.0600 Uiso calc H(21F) 0.2498 0.6251 0.1674 0.0600 Uiso calc H(21G) -0.0273 0.6854 -0.1279 0.0540 Uiso calc H(21H) -0.0095 0.7347 -0.0349 0.0540 Uiso calc H(21I) -0.0723 0.6692 -0.0213 0.0540 Uiso calc H(22A) -0.2317 0.5336 -0.1399 0.0650 Uiso calc H(22B) -0.1352 0.4948 -0.1901 0.0650 Uiso calc H(22C) -0.1054 0.5643 -0.1505 0.0650 Uiso calc H(22D) -0.1287 0.4044 0.0906 0.0680 Uiso calc H(22E) -0.1461 0.3882 -0.0305 0.0680 Uiso calc H(22F) -0.2461 0.4277 0.0142 0.0680 Uiso calc H(22G) -0.0700 0.5911 0.0909 0.0670 Uiso calc H(22H) -0.0623 0.5342 0.1704 0.0670 Uiso calc H(22I) -0.1891 0.5541 0.1047 0.0670 Uiso calc H(32A) 0.1084 0.6502 -0.3035 0.0570 Uiso calc H(32B) -0.0351 0.6505 -0.3180 0.0570 Uiso calc H(32C) 0.0357 0.7133 -0.3334 0.0570 Uiso calc H(32D) 0.1835 0.7156 -0.5253 0.0710 Uiso calc H(32E) 0.1579 0.6620 -0.6109 0.0710 Uiso calc H(32F) 0.2354 0.6472 -0.4994 0.0710 Uiso calc H(32G) -0.1784 0.6856 -0.5341 0.0790 Uiso calc H(32H) -0.1141 0.6862 -0.6342 0.0790 Uiso calc H(32I) -0.0878 0.7406 -0.5499 0.0790 Uiso calc H(41A) 0.2232 0.3125 -0.6219 0.0770 Uiso calc H(41B) 0.2070 0.3399 -0.7373 0.0770 Uiso calc H(41C) 0.1088 0.3544 -0.6656 0.0770 Uiso calc H(41D) 0.1189 0.4928 -0.6624 0.0620 Uiso calc H(41E) 0.2044 0.4940 -0.7483 0.0620 Uiso calc H(41F) 0.2439 0.5295 -0.6403 0.0620 Uiso calc H(41G) 0.4801 0.4572 -0.6202 0.0880 Uiso calc H(41H) 0.4320 0.4194 -0.7244 0.0880 Uiso calc H(41I) 0.4806 0.3829 -0.6191 0.0880 Uiso calc H(42A) 0.4578 0.2997 -0.5128 0.0990 Uiso calc H(42B) 0.4595 0.2419 -0.4356 0.0990 Uiso calc H(42C) 0.5827 0.2743 -0.4509 0.0990 Uiso calc H(42D) 0.6490 0.4029 -0.3621 0.1030 Uiso calc H(42E) 0.5746 0.4352 -0.2828 0.1030 Uiso calc H(42F) 0.5244 0.4368 -0.4048 0.1030 Uiso calc H(42G) 0.6405 0.2869 -0.2131 0.0550 Uiso calc H(42H) 0.5134 0.2560 -0.2056 0.0550 Uiso calc H(42I) 0.5487 0.3218 -0.1518 0.0550 Uiso calc loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ge 0.05144(17) 0.0502(2) 0.02076(13) -0.02936(16) 0.00038(11) -0.00059(13) Si(12) 0.0251(3) 0.0267(4) 0.0337(4) -0.0011(3) 0.0062(3) 0.0052(3) Si(21) 0.0305(3) 0.0267(4) 0.0252(3) 0.0051(3) 0.0008(3) -0.0021(3) Si(22) 0.0212(3) 0.0375(5) 0.0411(4) 0.0023(3) 0.0090(3) 0.0016(4) Si(32) 0.0325(4) 0.0245(4) 0.0299(4) -0.0027(3) -0.0037(3) 0.0001(3) Si(41) 0.0330(4) 0.0423(5) 0.0277(4) 0.0092(3) 0.0110(3) 0.0080(3) Si(42) 0.0218(3) 0.0375(5) 0.0370(4) 0.0069(3) 0.0049(3) 0.0086(3) O(11) 0.0227(8) 0.0336(11) 0.0203(8) -0.0049(7) -0.0027(6) 0.0014(7) O(21) 0.0244(8) 0.0221(9) 0.0283(9) 0.0040(7) -0.0004(7) -0.0008(7) O(31) 0.0235(8) 0.0283(10) 0.0283(9) -0.0025(7) -0.0061(7) -0.0019(8) O(41) 0.0241(8) 0.0399(11) 0.0275(9) 0.0024(7) 0.0085(7) 0.0096(8) C(11) 0.0191(11) 0.0227(13) 0.0255(12) -0.0003(9) -0.0025(9) -0.0012(10) C(12) 0.0185(11) 0.0211(13) 0.0317(13) 0.0016(9) 0.0017(9) 0.0020(10) C(13) 0.0192(11) 0.0203(14) 0.0435(14) -0.0014(9) 0.0007(10) 0.0030(11) C(14) 0.0201(11) 0.0227(13) 0.0337(13) 0.0037(9) -0.0053(9) -0.0009(10) C(15) 0.0242(12) 0.0304(15) 0.0432(15) 0.0024(11) -0.0062(10) -0.0127(13) C(16) 0.0338(14) 0.0389(18) 0.0407(16) 0.0087(12) -0.0132(12) -0.0130(13) C(17) 0.0419(15) 0.0374(17) 0.0270(13) 0.0090(13) -0.0082(11) -0.0045(12) C(18) 0.0311(13) 0.0333(16) 0.0259(13) 0.0016(11) -0.0042(10) 0.0009(11) C(19) 0.0220(11) 0.0211(13) 0.0267(12) 0.0028(9) -0.0021(9) -0.0007(10) C(1A) 0.0195(11) 0.0201(13) 0.0256(12) -0.0008(9) -0.0008(9) 0.0013(9) C(21) 0.0263(11) 0.0259(14) 0.0177(11) 0.0032(9) 0.0011(8) -0.0002(9) C(22) 0.0216(11) 0.0312(15) 0.0256(12) -0.0005(9) 0.0043(9) 0.0000(10) C(23) 0.0233(11) 0.0325(15) 0.0286(13) -0.0037(10) 0.0050(9) 0.0021(11) C(24) 0.0246(11) 0.0256(14) 0.0224(11) -0.0007(10) 0.0015(9) 0.0021(10) C(25) 0.0302(12) 0.0263(14) 0.0315(13) -0.0019(10) 0.0018(10) 0.0032(11) C(26) 0.0307(13) 0.0228(14) 0.0334(14) 0.0041(10) 0.0003(10) 0.0019(11) C(27) 0.0229(11) 0.0336(16) 0.0321(13) 0.0046(10) -0.0009(9) -0.0008(11) C(28) 0.0205(11) 0.0307(15) 0.0276(12) -0.0013(10) 0.0021(9) -0.0001(11) C(29) 0.0202(11) 0.0283(14) 0.0189(11) -0.0019(9) 0.0024(8) -0.0017(9) C(2A) 0.0203(10) 0.0256(13) 0.0167(10) -0.0018(9) 0.0004(8) 0.0008(10) C(31) 0.0157(10) 0.0288(14) 0.0203(10) -0.0013(9) -0.0017(8) -0.0030(10) C(32) 0.0212(11) 0.0257(14) 0.0231(12) 0.0015(9) 0.0006(9) -0.0015(10) C(33) 0.0242(11) 0.0258(14) 0.0242(12) 0.0015(10) -0.0009(9) 0.0005(10) C(34) 0.0231(11) 0.0269(14) 0.0212(11) 0.0000(9) 0.0014(9) -0.0006(10) C(35) 0.0228(11) 0.0337(16) 0.0251(12) 0.0002(10) -0.0033(9) 0.0001(10) C(36) 0.0246(12) 0.0403(17) 0.0314(13) -0.0032(11) -0.0029(10) -0.0047(12) C(37) 0.0306(13) 0.0302(16) 0.0375(14) -0.0064(11) 0.0001(10) -0.0040(12) C(38) 0.0301(12) 0.0255(15) 0.0331(13) -0.0011(10) 0.0000(10) 0.0018(11) C(39) 0.0200(10) 0.0250(14) 0.0222(12) -0.0012(9) 0.0010(9) -0.0003(10) C(3A) 0.0195(11) 0.0263(13) 0.0209(11) -0.0002(9) 0.0021(9) 0.0010(10) C(41) 0.0245(11) 0.0263(14) 0.0213(11) 0.0005(9) 0.0037(9) 0.0019(10) C(42) 0.0240(11) 0.0262(14) 0.0248(11) 0.0017(9) 0.0013(9) 0.0010(10) C(43) 0.0243(11) 0.0269(14) 0.0248(12) 0.0032(9) -0.0015(9) 0.0023(10) C(44) 0.0251(11) 0.0227(13) 0.0252(12) -0.0018(9) 0.0040(9) -0.0001(10) C(45) 0.0332(13) 0.0260(15) 0.0289(13) 0.0015(10) 0.0044(10) 0.0061(11) C(46) 0.0357(14) 0.0376(17) 0.0344(14) -0.0033(12) 0.0088(11) 0.0131(12) C(47) 0.0225(12) 0.0464(19) 0.0418(15) -0.0048(11) 0.0073(10) 0.0110(14) C(48) 0.0215(11) 0.0318(15) 0.0341(14) 0.0013(10) 0.0014(10) 0.0047(11) C(49) 0.0200(11) 0.0247(13) 0.0243(11) -0.0018(9) 0.0003(9) 0.0021(10) C(4A) 0.0230(11) 0.0260(14) 0.0200(11) -0.0005(9) 0.0005(9) -0.0003(10) C(121) 0.0301(13) 0.0398(17) 0.0344(14) 0.0044(11) 0.0023(11) 0.0085(12) C(122) 0.0590(19) 0.0414(19) 0.0433(17) -0.0049(15) 0.0219(14) -0.0023(14) C(123) 0.0349(14) 0.0460(19) 0.0509(18) -0.0058(13) 0.0114(12) 0.0154(15) C(211) 0.0441(16) 0.0289(17) 0.0465(17) 0.0011(12) 0.0030(13) -0.0018(13) C(212) 0.0473(15) 0.0387(17) 0.0306(14) 0.0079(13) -0.0032(11) -0.0057(13) C(213) 0.0382(14) 0.0366(17) 0.0321(14) 0.0105(12) 0.0014(11) -0.0037(12) C(221) 0.0291(13) 0.048(2) 0.0500(18) 0.0046(12) -0.0046(12) -0.0001(14) C(222) 0.0281(13) 0.047(2) 0.064(2) -0.0026(13) 0.0142(13) 0.0038(16) C(223) 0.0383(15) 0.045(2) 0.0549(19) 0.0083(13) 0.0226(13) 0.0017(15) C(321) 0.0392(14) 0.0357(18) 0.0377(15) -0.0028(12) 0.0053(11) -0.0073(12) C(322) 0.0557(19) 0.050(2) 0.0343(16) -0.0226(15) 0.0050(13) -0.0011(13) C(323) 0.057(2) 0.0269(17) 0.063(2) 0.0037(14) -0.0230(16) -0.0036(15) C(411) 0.067(2) 0.051(2) 0.0391(17) 0.0053(16) 0.0185(14) -0.0092(15) C(412) 0.0464(15) 0.046(2) 0.0339(14) 0.0102(14) 0.0122(12) 0.0131(14) C(413) 0.0460(17) 0.088(3) 0.0485(19) 0.0207(18) 0.0273(15) 0.0268(19) C(421) 0.068(2) 0.090(3) 0.044(2) 0.044(2) 0.0170(17) 0.0018(19) C(422) 0.0327(16) 0.063(3) 0.102(3) -0.0041(15) -0.0104(17) 0.042(2) C(423) 0.0265(13) 0.0406(18) 0.0423(16) 0.0054(11) 0.0013(11) 0.0046(13) # 10. MOLECULAR GEOMETRY _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Ge O(11) 1.8088(16) YES Ge O(31) 1.8202(17) YES Si(12) C(122) 1.857(3) YES Si(12) C(121) 1.862(3) YES Si(12) C(123) 1.872(3) YES Si(12) C(12) 1.883(3) YES Si(21) O(21) 1.6737(18) YES Si(21) C(212) 1.849(3) YES Si(21) C(211) 1.852(3) YES Si(21) C(213) 1.865(3) YES Si(22) C(221) 1.859(3) YES Si(22) C(223) 1.860(3) YES Si(22) C(222) 1.873(3) YES Si(22) C(22) 1.890(2) YES Si(32) C(322) 1.855(3) YES Si(32) C(321) 1.864(3) YES Si(32) C(323) 1.865(3) YES Si(32) C(32) 1.881(3) YES Si(41) O(41) 1.6756(18) YES Si(41) C(411) 1.845(4) YES Si(41) C(413) 1.857(3) YES Si(41) C(412) 1.857(3) YES Si(42) C(422) 1.851(4) YES Si(42) C(421) 1.859(4) YES Si(42) C(423) 1.870(3) YES Si(42) C(42) 1.885(2) YES O(11) C(11) 1.363(3) YES O(21) C(21) 1.380(3) YES O(31) C(31) 1.378(2) YES O(41) C(41) 1.370(3) YES C(11) C(1A) 1.385(3) YES C(11) C(12) 1.433(3) YES C(12) C(13) 1.380(3) YES C(13) C(14) 1.410(4) YES C(14) C(19) 1.416(3) YES C(14) C(15) 1.431(3) YES C(15) C(16) 1.361(4) YES C(16) C(17) 1.398(4) YES C(17) C(18) 1.380(3) YES C(18) C(19) 1.425(3) YES C(19) C(1A) 1.433(3) YES C(1A) C(2A) 1.492(3) YES C(21) C(2A) 1.381(3) YES C(21) C(22) 1.431(3) YES C(22) C(23) 1.371(4) YES C(23) C(24) 1.423(3) YES C(24) C(25) 1.408(4) YES C(24) C(29) 1.420(3) YES C(25) C(26) 1.378(3) YES C(26) C(27) 1.405(4) YES C(27) C(28) 1.365(4) YES C(28) C(29) 1.421(3) YES C(29) C(2A) 1.435(4) YES C(31) C(3A) 1.383(4) YES C(31) C(32) 1.430(3) YES C(32) C(33) 1.383(3) YES C(33) C(34) 1.405(4) YES C(34) C(35) 1.415(3) YES C(34) C(39) 1.424(3) YES C(35) C(36) 1.365(4) YES C(36) C(37) 1.410(4) YES C(37) C(38) 1.368(3) YES C(38) C(39) 1.413(4) YES C(39) C(3A) 1.436(3) YES C(3A) C(4A) 1.493(3) YES C(41) C(4A) 1.383(3) YES C(41) C(42) 1.438(3) YES C(42) C(43) 1.379(3) YES C(43) C(44) 1.415(3) YES C(44) C(45) 1.410(3) YES C(44) C(49) 1.421(3) YES C(45) C(46) 1.368(4) YES C(46) C(47) 1.397(4) YES C(47) C(48) 1.365(4) YES C(48) C(49) 1.422(3) YES C(49) C(4A) 1.434(3) YES loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(11) Ge O(31) 89.40(7) YES C(122) Si(12) C(121) 111.65(14) YES C(122) Si(12) C(123) 107.16(15) YES C(121) Si(12) C(123) 108.83(14) YES C(122) Si(12) C(12) 115.28(13) YES C(121) Si(12) C(12) 105.57(12) YES C(123) Si(12) C(12) 108.19(12) YES O(21) Si(21) C(212) 108.71(12) YES O(21) Si(21) C(211) 112.70(12) YES C(212) Si(21) C(211) 110.96(14) YES O(21) Si(21) C(213) 103.72(11) YES C(212) Si(21) C(213) 114.14(13) YES C(211) Si(21) C(213) 106.48(14) YES C(221) Si(22) C(223) 111.96(15) YES C(221) Si(22) C(222) 108.75(15) YES C(223) Si(22) C(222) 105.97(15) YES C(221) Si(22) C(22) 110.87(12) YES C(223) Si(22) C(22) 110.50(12) YES C(222) Si(22) C(22) 108.61(13) YES C(322) Si(32) C(321) 112.41(13) YES C(322) Si(32) C(323) 108.71(17) YES C(321) Si(32) C(323) 107.15(15) YES C(322) Si(32) C(32) 109.34(14) YES C(321) Si(32) C(32) 110.76(12) YES C(323) Si(32) C(32) 108.34(12) YES O(41) Si(41) C(411) 109.29(13) YES O(41) Si(41) C(413) 105.58(13) YES C(411) Si(41) C(413) 111.38(18) YES O(41) Si(41) C(412) 111.95(12) YES C(411) Si(41) C(412) 111.26(15) YES C(413) Si(41) C(412) 107.24(15) YES C(422) Si(42) C(421) 112.0(2) YES C(422) Si(42) C(423) 109.19(15) YES C(421) Si(42) C(423) 106.72(15) YES C(422) Si(42) C(42) 111.11(15) YES C(421) Si(42) C(42) 108.70(14) YES C(423) Si(42) C(42) 108.97(12) YES C(11) O(11) Ge 133.92(15) YES C(21) O(21) Si(21) 135.22(14) YES C(31) O(31) Ge 124.04(15) YES C(41) O(41) Si(41) 134.31(16) YES O(11) C(11) C(1A) 123.5(2) YES O(11) C(11) C(12) 114.5(2) YES C(1A) C(11) C(12) 122.1(2) YES C(13) C(12) C(11) 117.4(2) YES C(13) C(12) Si(12) 120.15(19) YES C(11) C(12) Si(12) 121.90(17) YES C(12) C(13) C(14) 122.9(2) YES C(13) C(14) C(19) 118.7(2) YES C(13) C(14) C(15) 122.2(2) YES C(19) C(14) C(15) 119.1(2) YES C(16) C(15) C(14) 120.9(3) YES C(15) C(16) C(17) 120.4(2) YES C(18) C(17) C(16) 120.4(3) YES C(17) C(18) C(19) 120.9(3) YES C(14) C(19) C(18) 118.2(2) YES C(14) C(19) C(1A) 119.7(2) YES C(18) C(19) C(1A) 122.1(2) YES C(11) C(1A) C(19) 119.0(2) YES C(11) C(1A) C(2A) 122.63(19) YES C(19) C(1A) C(2A) 118.3(2) YES O(21) C(21) C(2A) 120.4(2) YES O(21) C(21) C(22) 116.73(19) YES C(2A) C(21) C(22) 122.6(2) YES C(23) C(22) C(21) 117.1(2) YES C(23) C(22) Si(22) 119.31(18) YES C(21) C(22) Si(22) 123.57(19) YES C(22) C(23) C(24) 123.5(2) YES C(25) C(24) C(29) 119.7(2) YES C(25) C(24) C(23) 122.2(2) YES C(29) C(24) C(23) 118.1(2) YES C(26) C(25) C(24) 121.2(2) YES C(25) C(26) C(27) 118.9(2) YES C(28) C(27) C(26) 121.4(2) YES C(27) C(28) C(29) 121.0(2) YES C(24) C(29) C(28) 117.8(2) YES C(24) C(29) C(2A) 119.6(2) YES C(28) C(29) C(2A) 122.6(2) YES C(21) C(2A) C(29) 119.2(2) YES C(21) C(2A) C(1A) 123.0(2) YES C(29) C(2A) C(1A) 117.90(19) YES O(31) C(31) C(3A) 122.0(2) YES O(31) C(31) C(32) 115.5(2) YES C(3A) C(31) C(32) 122.5(2) YES C(33) C(32) C(31) 116.8(2) YES C(33) C(32) Si(32) 121.87(19) YES C(31) C(32) Si(32) 121.32(17) YES C(32) C(33) C(34) 123.5(2) YES C(33) C(34) C(35) 122.2(2) YES C(33) C(34) C(39) 118.7(2) YES C(35) C(34) C(39) 119.1(2) YES C(36) C(35) C(34) 121.3(2) YES C(35) C(36) C(37) 119.7(2) YES C(38) C(37) C(36) 120.3(3) YES C(37) C(38) C(39) 121.5(2) YES C(38) C(39) C(34) 118.0(2) YES C(38) C(39) C(3A) 122.9(2) YES C(34) C(39) C(3A) 119.1(2) YES C(31) C(3A) C(39) 119.3(2) YES C(31) C(3A) C(4A) 120.12(19) YES C(39) C(3A) C(4A) 120.3(2) YES O(41) C(41) C(4A) 121.5(2) YES O(41) C(41) C(42) 116.1(2) YES C(4A) C(41) C(42) 122.2(2) YES C(43) C(42) C(41) 117.2(2) YES C(43) C(42) Si(42) 119.64(18) YES C(41) C(42) Si(42) 123.08(18) YES C(42) C(43) C(44) 123.1(2) YES C(45) C(44) C(43) 122.0(2) YES C(45) C(44) C(49) 119.6(2) YES C(43) C(44) C(49) 118.4(2) YES C(46) C(45) C(44) 120.6(2) YES C(45) C(46) C(47) 119.9(2) YES C(48) C(47) C(46) 121.3(2) YES C(47) C(48) C(49) 120.4(2) YES C(44) C(49) C(48) 118.1(2) YES C(44) C(49) C(4A) 119.9(2) YES C(48) C(49) C(4A) 122.0(2) YES C(41) C(4A) C(49) 118.9(2) YES C(41) C(4A) C(3A) 122.5(2) YES C(49) C(4A) C(3A) 118.4(2) YES #============================================================================== data_Compound2 _database_code_CSD 176940 #============================================================================== _audit_creation_date 13-11-01 _audit_creation_method from_MolEN_and_SHELXL _audit_update_record ; ? ; # 5. CRYSTAL DATA _chemical_compound_source ? _exptl_crystal_description chunk _exptl_crystal_colour colorless _exptl_crystal_size_max 0.13 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_min 0.10 _chemical_name_systematic ; ? ; _exptl_crystal_density_method ? _chemical_formula_sum 'C36 H35 Ge1 N1 O2 Si2' _chemical_formula_moiety 'C36 H35 Ge1 N1 O2 Si2' _chemical_formula_structural ? _chemical_formula_weight 642.45 _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' 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 8.3277(2) _cell_length_b 10.4652(3) _cell_length_c 36.0635(8) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3143.0(2) _cell_measurement_reflns_used 20161 _cell_measurement_theta_min 5 _cell_measurement_theta_max 27 _cell_formula_units_z 4 _exptl_crystal_density_diffrn 1.36 _exptl_crystal_density_meas ? _diffrn_radiation_type MO-K\a _diffrn_radiation_wavelength 0.71073 _exptl_absorpt_coefficient_mu 1.067 _cell_measurement_temperature 150 _exptl_crystal_F_000 1336 # 6. DATA COLLECTION _diffrn_ambient_temperature 150 _diffrn_measurement_device_type Nonius_KappaCCD _exptl_absorpt_correction_type refined_empirical_(Otwinowski_&_Minor,_1996 _exptl_absorpt_correction_T_min 0.5423 _exptl_absorpt_correction_T_max 0.8988 _diffrn_reflns_number 20161 _diffrn_measured_fraction_theta_max 0.9889 _diffrn_reflns_theta_full 27.5 _diffrn_measured_fraction_theta_full 0.9889 _reflns_number_total 6841 _reflns_Friedl_coverage 0.8250 _reflns_number_gt 5769 _reflns_threshold_expression >2.0\s(I) _diffrn_reflns_av_R_equivalents 0.072 _diffrn_reflns_theta_min 5.00 _diffrn_reflns_theta_max 27.49 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_l_min -44 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_max 46 # 7. REFINEMENT DATA _refine_special_details ; Refinement on F^2^ for ALL reflections except for 0 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating R_factor_obs 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_R_factor_gt 0.044 _refine_ls_wR_factor_ref 0.077 _refine_ls_hydrogen_treatment ; Chemically significant hydrogens refined isotropically Others riding ; _refine_ls_number_reflns 6841 _refine_ls_number_parameters 395 _refine_ls_number_restraints 0 _refine_ls_goodness_of_fit_ref 1.007 _refine_ls_weighting_scheme 'calc ' _refine_ls_weighting_details '1/[\s^2^(Fo^2^)+(0.0307P)^2^+0.0000P] where P=(Fo^2^+2Fc^2^)/3 ' _refine_ls_shift/su_max 0.003 _refine_diff_density_max 0.31 _refine_diff_density_min -0.47 _refine_ls_extinction_method none _atom_type_scat_source 'International Tables for Crystallography (Vol C)' # 8. COMPUTING DATA _computing_data_collection Collect_(Nonius,_1998) _computing_cell_refinement DENZO/SCALEPACK_(Otwinowski,_1996) _computing_data_reduction DENZO/SCALEPACK_(Otwinowski,_1996) _computing_structure_solution PATTY_(DIRDIF99,_Beurskins,_1999) _computing_structure_refinement SHELX97_(Sheldrick,_1997) _computing_molecular_graphics ; ORTEP (Johnson, 1976) PLUTON (Spek, 1991) ; _computing_publication_material CIF_VAX_MolEN_(Fair,_1990) _refine_ls_abs_structure_details 'Flack H. D. (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack 0.006(9) # 9. ATOMIC COORDINATES AND THERMAL PARAMETERS loop_ _atom_site_label _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_thermal_displace_type _atom_site_calc_flag Ge 0.48620(4) 0.36564(3) 0.331394(8) 0.03177(10) Uani ? Si(1) 0.53930(11) 0.09515(9) 0.42376(2) 0.0307(3) Uani ? Si(2) 0.35216(11) 0.72945(10) 0.28913(2) 0.0283(3) Uani ? O(1) 0.3861(3) 0.2946(2) 0.37233(5) 0.0285(7) Uani ? O(2) 0.4641(2) 0.5378(2) 0.34472(5) 0.0293(6) Uani ? N(3) 0.7104(4) 0.3913(5) 0.35657(11) 0.0401(12) Uani ? C(11) 0.4018(4) 0.3454(3) 0.40748(8) 0.0259(9) Uani ? C(12) 0.4770(4) 0.2641(3) 0.43444(8) 0.0282(9) Uani ? C(13) 0.5078(4) 0.3165(3) 0.46874(8) 0.0294(9) Uani ? C(14) 0.4716(4) 0.4448(3) 0.47732(8) 0.0277(9) Uani ? C(15) 0.5193(4) 0.5006(4) 0.51158(8) 0.0346(10) Uani ? C(16) 0.4833(4) 0.6244(4) 0.51954(8) 0.0388(10) Uani ? C(17) 0.3989(4) 0.6987(4) 0.49383(10) 0.0397(10) Uani ? C(18) 0.3519(4) 0.6474(4) 0.46044(8) 0.0313(10) Uani ? C(19) 0.3864(4) 0.5205(3) 0.45115(8) 0.0259(9) Uani ? C(1A) 0.3464(4) 0.4650(3) 0.41570(8) 0.0259(9) Uani ? C(21) 0.3174(4) 0.5823(3) 0.35550(8) 0.0265(9) Uani ? C(22) 0.2437(4) 0.6768(3) 0.33229(8) 0.0269(9) Uani ? C(23) 0.0959(4) 0.7220(3) 0.34260(8) 0.0292(10) Uani ? C(24) 0.0124(4) 0.6747(3) 0.37426(7) 0.0256(9) Uani ? C(25) -0.1449(4) 0.7136(4) 0.38292(9) 0.0322(10) Uani ? C(26) -0.2268(4) 0.6619(4) 0.41215(9) 0.0357(12) Uani ? C(27) -0.1516(4) 0.5697(4) 0.43447(9) 0.0352(12) Uani ? C(28) 0.0021(4) 0.5323(3) 0.42754(7) 0.0289(9) Uani ? C(29) 0.0896(4) 0.5818(3) 0.39728(8) 0.0268(9) Uani ? C(2A) 0.2504(4) 0.5425(3) 0.38868(8) 0.0258(9) Uani ? C(111) 0.7303(4) 0.1089(3) 0.39656(8) 0.0283(10) Uani ? C(112) 0.8621(4) 0.1712(3) 0.41232(9) 0.0345(10) Uani ? C(113) 1.0055(5) 0.1898(3) 0.39295(9) 0.0397(10) Uani ? C(114) 1.0191(4) 0.1466(4) 0.35705(9) 0.0405(10) Uani ? C(115) 0.8911(4) 0.0841(4) 0.34069(9) 0.0397(10) Uani ? C(116) 0.7491(4) 0.0667(4) 0.36022(9) 0.0360(10) Uani ? C(117) 0.3882(4) -0.0015(4) 0.39817(10) 0.0427(12) Uani ? C(118) 0.5809(4) 0.0141(4) 0.46868(8) 0.0400(12) Uani ? C(211) 0.2394(4) 0.8666(4) 0.26824(8) 0.0279(9) Uani ? C(212) 0.2614(4) 0.9905(4) 0.28120(9) 0.0335(12) Uani ? C(213) 0.1919(4) 1.0953(4) 0.26461(9) 0.0380(12) Uani ? C(214) 0.0942(4) 1.0795(4) 0.23427(9) 0.0417(12) Uani ? C(215) 0.0648(4) 0.9586(4) 0.22076(9) 0.0430(12) Uani ? C(216) 0.1374(4) 0.8537(4) 0.23727(9) 0.0367(10) Uani ? C(217) 0.5580(4) 0.7872(4) 0.30078(9) 0.0363(10) Uani ? C(218) 0.3599(4) 0.5982(4) 0.25456(8) 0.0357(10) Uani ? H(13) 0.5542 0.2655 0.4869 0.0350 Uiso calc H(15) 0.5758 0.4519 0.5287 0.0420 Uiso calc H(16) 0.5149 0.6597 0.5421 0.0460 Uiso calc H(17) 0.3743 0.7832 0.4994 0.0480 Uiso calc H(18) 0.2961 0.6982 0.4437 0.0380 Uiso calc H(23) 0.0484 0.7859 0.3284 0.0350 Uiso calc H(25) -0.1943 0.7758 0.3685 0.0390 Uiso calc H(26) -0.3315 0.6876 0.4172 0.0430 Uiso calc H(27) -0.2075 0.5337 0.4542 0.0430 Uiso calc H(28) 0.0504 0.4728 0.4431 0.0350 Uiso calc H(3A) 0.704(6) 0.391(6) 0.3821(18) 0.13(2) Uiso ? H(3B) 0.768(6) 0.445(6) 0.3479(14) 0.10(2) Uiso ? H(3C) 0.750(8) 0.328(8) 0.3548(18) 0.13(3) Uiso ? H(112) 0.8541 0.2013 0.4365 0.0410 Uiso calc H(113) 1.0913 0.2311 0.4043 0.0480 Uiso calc H(114) 1.1137 0.1593 0.3439 0.0480 Uiso calc H(115) 0.9002 0.0536 0.3166 0.0470 Uiso calc H(116) 0.6637 0.0255 0.3486 0.0430 Uiso calc H(11A) 0.2903 -0.0048 0.4122 0.0640 Uiso calc H(11B) 0.4285 -0.0866 0.3947 0.0640 Uiso calc H(11C) 0.3679 0.0370 0.3745 0.0640 Uiso calc H(11D) 0.6712 0.0540 0.4805 0.0610 Uiso calc H(11E) 0.6043 -0.0744 0.4643 0.0610 Uiso calc H(11F) 0.4884 0.0209 0.4845 0.0610 Uiso calc H(212) 0.3257 1.0031 0.3020 0.0400 Uiso calc H(213) 0.2111 1.1767 0.2739 0.0460 Uiso calc H(214) 0.0481 1.1503 0.2229 0.0500 Uiso calc H(215) -0.0035 0.9474 0.2006 0.0520 Uiso calc H(216) 0.1181 0.7727 0.2277 0.0440 Uiso calc H(21A) 0.6045 0.8276 0.2794 0.0540 Uiso calc H(21B) 0.6235 0.7161 0.3081 0.0540 Uiso calc H(21C) 0.5518 0.8475 0.3208 0.0540 Uiso calc H(21D) 0.2550 0.5612 0.2519 0.0540 Uiso calc H(21E) 0.4341 0.5340 0.2628 0.0540 Uiso calc H(21F) 0.3945 0.6316 0.2311 0.0540 Uiso calc loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_12 _atom_site_aniso_U_13 _atom_site_aniso_U_23 Ge 0.0390(2) 0.0317(2) 0.02461(18) 0.0026(2) 0.00346(16) -0.00060(15) Si(1) 0.0298(5) 0.0286(6) 0.0338(5) 0.0022(4) -0.0016(4) 0.0060(4) Si(2) 0.0308(5) 0.0296(6) 0.0245(5) 0.0024(5) 0.0005(4) 0.0022(4) O(1) 0.0335(13) 0.0278(15) 0.0241(12) 0.0026(11) -0.0013(10) 0.0005(10) O(2) 0.0290(12) 0.0308(14) 0.0280(11) 0.0041(11) 0.0047(9) 0.0020(9) N(3) 0.0354(19) 0.037(3) 0.048(2) 0.0048(19) 0.0051(15) 0.0096(18) C(11) 0.0275(17) 0.027(2) 0.0231(18) -0.0005(17) 0.0023(13) 0.0017(15) C(12) 0.0231(17) 0.033(2) 0.0286(17) -0.0028(17) 0.0036(14) 0.0040(14) C(13) 0.0258(18) 0.036(2) 0.0264(18) 0.0001(17) -0.0011(16) 0.0079(13) C(14) 0.0277(18) 0.032(2) 0.0235(17) -0.0024(17) 0.0022(14) 0.0029(14) C(15) 0.033(2) 0.049(2) 0.0219(17) -0.004(2) 0.0004(16) 0.0053(15) C(16) 0.042(2) 0.045(2) 0.0293(18) -0.012(2) 0.0005(16) -0.0066(16) C(17) 0.045(2) 0.034(2) 0.040(2) -0.0102(19) 0.0088(17) -0.0059(18) C(18) 0.0370(19) 0.030(2) 0.0270(18) -0.0030(18) 0.0024(15) 0.0000(16) C(19) 0.0273(18) 0.028(2) 0.0223(18) -0.0018(16) 0.0055(14) 0.0022(14) C(1A) 0.0252(17) 0.032(2) 0.0205(18) -0.0025(16) 0.0024(14) 0.0012(15) C(21) 0.0272(18) 0.026(2) 0.0264(18) 0.0034(15) -0.0009(14) -0.0055(15) C(22) 0.0298(17) 0.028(2) 0.0229(17) 0.0024(15) -0.0030(15) -0.0007(15) C(23) 0.0336(19) 0.025(2) 0.029(2) 0.0033(16) -0.0086(14) -0.0009(14) C(24) 0.0253(17) 0.0261(19) 0.0253(17) 0.0038(17) 0.0018(15) -0.0036(13) C(25) 0.0296(19) 0.032(2) 0.035(2) 0.0031(17) -0.0049(16) -0.0025(16) C(26) 0.0280(18) 0.041(3) 0.038(2) 0.0040(18) 0.0050(16) -0.0054(18) C(27) 0.0307(19) 0.045(3) 0.030(2) -0.0037(19) 0.0065(16) -0.0040(17) C(28) 0.0320(19) 0.031(2) 0.0236(16) 0.0003(18) -0.0002(16) 0.0021(13) C(29) 0.0321(18) 0.029(2) 0.0192(17) 0.0003(16) 0.0003(14) -0.0049(14) C(2A) 0.0308(18) 0.027(2) 0.0195(18) -0.0019(16) -0.0007(14) -0.0005(14) C(111) 0.0311(18) 0.023(2) 0.0308(19) 0.0066(16) -0.0039(14) 0.0067(15) C(112) 0.036(2) 0.039(2) 0.0284(19) 0.0070(18) -0.0023(16) 0.0026(15) C(113) 0.031(2) 0.050(2) 0.038(2) -0.002(2) -0.0044(18) 0.0018(16) C(114) 0.0315(19) 0.043(2) 0.047(2) 0.009(2) 0.0037(17) 0.0085(17) C(115) 0.049(2) 0.036(2) 0.034(2) 0.0076(19) 0.0062(17) 0.0025(16) C(116) 0.041(2) 0.030(2) 0.037(2) 0.0005(19) -0.0014(17) 0.0010(16) C(117) 0.035(2) 0.039(3) 0.054(2) -0.0019(19) 0.0017(17) 0.0033(19) C(118) 0.042(2) 0.038(3) 0.040(2) -0.0003(19) 0.0015(16) 0.0118(17) C(211) 0.0267(17) 0.035(2) 0.0219(17) 0.0014(18) 0.0072(13) 0.0054(16) C(212) 0.037(2) 0.036(3) 0.0276(19) 0.0074(19) -0.0031(16) 0.0013(16) C(213) 0.041(2) 0.035(3) 0.038(2) 0.0053(19) 0.0022(17) 0.0039(17) C(214) 0.043(2) 0.046(3) 0.036(2) 0.016(2) 0.0069(17) 0.0112(19) C(215) 0.040(2) 0.058(3) 0.031(2) 0.012(2) -0.0036(16) 0.0034(19) C(216) 0.035(2) 0.041(2) 0.034(2) 0.003(2) 0.0012(16) 0.0001(17) C(217) 0.036(2) 0.032(2) 0.041(2) 0.0017(17) -0.0034(15) 0.0033(16) C(218) 0.038(2) 0.038(2) 0.031(2) 0.0052(18) 0.0001(15) -0.0031(16) # 10. MOLECULAR GEOMETRY _geom_special_details ; All esds (except the esd in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell esds are taken into account individually in the estimation of esds in distances, angles and torsion angles; correlations between esds in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell esds is used for estimating esds involving l.s. planes. ; loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance _geom_bond_publ_flag Ge O(1) 1.851(2) YES Ge O(2) 1.874(2) YES Ge N(3) 2.093(4) YES Si(1) C(117) 1.859(4) YES Si(1) C(118) 1.861(3) YES Si(1) C(111) 1.874(3) YES Si(1) C(12) 1.882(4) YES Si(2) C(218) 1.856(3) YES Si(2) C(217) 1.865(3) YES Si(2) C(211) 1.873(4) YES Si(2) C(22) 1.882(3) YES O(1) C(11) 1.381(4) YES O(2) C(21) 1.364(4) YES N(3) H(3C) 0.74(8) YES N(3) H(3B) 0.80(6) YES N(3) H(3A) 0.92(6) YES C(11) C(1A) 1.366(4) YES C(11) C(12) 1.436(4) YES C(12) C(13) 1.377(4) YES C(13) C(14) 1.411(4) YES C(14) C(19) 1.421(4) YES C(14) C(15) 1.423(4) YES C(15) C(16) 1.360(5) YES C(16) C(17) 1.400(5) YES C(17) C(18) 1.375(4) YES C(18) C(19) 1.400(5) YES C(19) C(1A) 1.443(4) YES C(1A) C(2A) 1.498(4) YES C(21) C(2A) 1.385(4) YES C(21) C(22) 1.434(4) YES C(22) C(23) 1.370(4) YES C(23) C(24) 1.426(4) YES C(24) C(25) 1.407(5) YES C(24) C(29) 1.431(4) YES C(25) C(26) 1.367(5) YES C(26) C(27) 1.404(5) YES C(27) C(28) 1.362(5) YES C(28) C(29) 1.411(4) YES C(29) C(2A) 1.435(4) YES C(111) C(116) 1.392(4) YES C(111) C(112) 1.398(5) YES C(112) C(113) 1.397(5) YES C(113) C(114) 1.376(4) YES C(114) C(115) 1.383(5) YES C(115) C(116) 1.389(5) YES C(211) C(212) 1.391(5) YES C(211) C(216) 1.410(4) YES C(212) C(213) 1.376(5) YES C(213) C(214) 1.373(5) YES C(214) C(215) 1.378(5) YES C(215) C(216) 1.388(5) YES loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_publ_flag O(1) Ge O(2) 97.90(9) YES O(1) Ge N(3) 96.15(13) YES O(2) Ge N(3) 81.55(15) YES C(117) Si(1) C(118) 108.05(17) YES C(117) Si(1) C(111) 110.87(16) YES C(118) Si(1) C(111) 109.43(15) YES C(117) Si(1) C(12) 115.22(16) YES C(118) Si(1) C(12) 107.52(15) YES C(111) Si(1) C(12) 105.60(15) YES C(218) Si(2) C(217) 111.05(17) YES C(218) Si(2) C(211) 108.30(15) YES C(217) Si(2) C(211) 107.65(16) YES C(218) Si(2) C(22) 110.82(15) YES C(217) Si(2) C(22) 110.46(14) YES C(211) Si(2) C(22) 108.44(13) YES C(11) O(1) Ge 122.34(19) YES C(21) O(2) Ge 119.3(2) YES H(3C) N(3) H(3B) 109(6) YES H(3C) N(3) H(3A) 96(6) YES H(3B) N(3) H(3A) 116(5) YES H(3C) N(3) Ge 104(5) YES H(3B) N(3) Ge 117(4) YES H(3A) N(3) Ge 112(3) YES C(1A) C(11) O(1) 121.3(3) YES C(1A) C(11) C(12) 122.9(3) YES O(1) C(11) C(12) 115.8(3) YES C(13) C(12) C(11) 116.9(3) YES C(13) C(12) Si(1) 120.5(2) YES C(11) C(12) Si(1) 122.6(2) YES C(12) C(13) C(14) 122.5(3) YES C(13) C(14) C(19) 119.4(3) YES C(13) C(14) C(15) 121.4(3) YES C(19) C(14) C(15) 119.2(3) YES C(16) C(15) C(14) 120.8(3) YES C(15) C(16) C(17) 120.0(3) YES C(18) C(17) C(16) 120.4(4) YES C(17) C(18) C(19) 121.4(3) YES C(18) C(19) C(14) 118.2(3) YES C(18) C(19) C(1A) 123.1(3) YES C(14) C(19) C(1A) 118.6(3) YES C(11) C(1A) C(19) 118.9(3) YES C(11) C(1A) C(2A) 122.3(3) YES C(19) C(1A) C(2A) 118.8(3) YES O(2) C(21) C(2A) 120.3(3) YES O(2) C(21) C(22) 116.9(3) YES C(2A) C(21) C(22) 122.7(3) YES C(23) C(22) C(21) 117.7(3) YES C(23) C(22) Si(2) 123.7(2) YES C(21) C(22) Si(2) 118.6(2) YES C(22) C(23) C(24) 122.4(3) YES C(25) C(24) C(23) 122.1(3) YES C(25) C(24) C(29) 119.1(3) YES C(23) C(24) C(29) 118.8(3) YES C(26) C(25) C(24) 121.4(3) YES C(25) C(26) C(27) 119.4(3) YES C(28) C(27) C(26) 120.8(3) YES C(27) C(28) C(29) 121.5(3) YES C(28) C(29) C(24) 117.8(3) YES C(28) C(29) C(2A) 122.9(3) YES C(24) C(29) C(2A) 119.3(3) YES C(21) C(2A) C(29) 118.4(3) YES C(21) C(2A) C(1A) 120.7(3) YES C(29) C(2A) C(1A) 120.8(3) YES C(116) C(111) C(112) 116.3(3) YES C(116) C(111) Si(1) 124.3(3) YES C(112) C(111) Si(1) 119.3(2) YES C(113) C(112) C(111) 122.2(3) YES C(114) C(113) C(112) 119.7(4) YES C(113) C(114) C(115) 119.6(3) YES C(114) C(115) C(116) 120.1(3) YES C(115) C(116) C(111) 122.1(3) YES C(212) C(211) C(216) 115.8(3) YES C(212) C(211) Si(2) 120.9(2) YES C(216) C(211) Si(2) 123.2(3) YES C(213) C(212) C(211) 122.8(3) YES C(214) C(213) C(212) 120.0(4) YES C(213) C(214) C(215) 119.8(4) YES C(214) C(215) C(216) 119.8(3) YES C(215) C(216) C(211) 121.8(4) YES #============================================================================== #END OF CIF #==============================================================================