#------------------------------------------------------------------------------ #$Date: 2014-07-23 10:49:31 +0100 (Wed, 23 Jul 2014) $ #$Revision: 120677 $ #$URL: svn://www.crystallography.net/cod/cif/1/10/08/1100899.cif $ #------------------------------------------------------------------------------ # # This file is available in the Crystallography Open Database (COD), # http://www.crystallography.net/ # # All data on this site have been placed in the public domain by the # contributors. # data_1100899 _chemical_formula_moiety 'C32 H62 Ge N2 P2 Si4, 0.5 C7 H14' _chemical_formula_sum 'C35.5 H69 Ge N2 P2 Si4' _chemical_formula_weight 770.82 loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0033 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' 'P' 'P' 0.1023 0.0942 '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' 'Si' 'Si' 0.0817 0.0704 '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 11.4596(5) _cell_length_b 12.0029(5) _cell_length_c 16.3524(7) _cell_angle_alpha 78.569(1) _cell_angle_beta 89.576(1) _cell_angle_gamma 75.536(1) _cell_volume 2132.65(16) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13588 _cell_measurement_theta_min 2.16 _cell_measurement_theta_max 28.9 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.35 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.200 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 820 _exptl_absorpt_coefficient_mu 0.931 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.653 _exptl_absorpt_correction_T_max 0.737 _exptl_absorpt_process_details SADABS _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method '\w rotation with narrow frames' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15612 _diffrn_reflns_av_R_equivalents 0.0157 _diffrn_reflns_av_sigmaI/netI 0.0241 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 22 _diffrn_reflns_theta_min 1.84 _diffrn_reflns_theta_max 28.86 _reflns_number_total 9401 _reflns_number_gt 8637 _reflns_threshold_expression I>2\s(I) _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^)+(0.0417P)^2^+0.8715P] 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 9401 _refine_ls_number_parameters 413 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0299 _refine_ls_R_factor_gt 0.0268 _refine_ls_wR_factor_ref 0.0776 _refine_ls_wR_factor_gt 0.0755 _refine_ls_goodness_of_fit_ref 1.036 _refine_ls_restrained_S_all 1.036 _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 Ge Ge 0.339664(13) 0.041854(12) 0.179005(9) 0.01916(5) Uani 1 1 d . . . P1 P 0.19237(3) 0.03927(3) 0.28420(2) 0.01874(8) Uani 1 1 d . . . P2 P 0.47156(3) -0.13012(3) 0.26407(2) 0.01758(8) Uani 1 1 d . . . Si1 Si -0.03479(4) 0.09811(4) 0.17835(3) 0.02998(10) Uani 1 1 d . . . Si2 Si -0.02151(4) 0.25897(4) 0.30948(3) 0.02919(10) Uani 1 1 d . . . Si3 Si 0.35557(4) -0.33940(4) 0.34097(3) 0.02924(10) Uani 1 1 d . . . Si4 Si 0.40852(4) -0.30121(4) 0.14575(3) 0.02887(10) Uani 1 1 d . . . N1 N 0.41870(12) 0.17393(11) 0.21553(8) 0.0244(3) Uani 1 1 d . . . N2 N 0.81877(12) -0.38364(12) 0.37561(9) 0.0314(3) Uani 1 1 d . . . C1 C 0.06320(13) 0.16638(13) 0.23583(9) 0.0224(3) Uani 1 1 d . . . H1 H 0.0974 0.2195 0.1927 0.027 Uiso 1 1 calc R . . C2 C -0.1314(2) 0.2119(2) 0.09383(16) 0.0634(7) Uani 1 1 d . . . H2A H -0.1714 0.1733 0.0592 0.095 Uiso 1 1 calc R . . H2B H -0.0809 0.2554 0.0591 0.095 Uiso 1 1 calc R . . H2C H -0.1924 0.2663 0.1191 0.095 Uiso 1 1 calc R . . C3 C -0.12808(17) 0.02272(19) 0.25303(14) 0.0437(5) Uani 1 1 d . . . H3A H -0.1860 0.0811 0.2771 0.066 Uiso 1 1 calc R . . H3B H -0.0755 -0.0335 0.2977 0.066 Uiso 1 1 calc R . . H3C H -0.1717 -0.0191 0.2235 0.066 Uiso 1 1 calc R . . C4 C 0.05627(17) -0.01435(19) 0.12280(12) 0.0403(4) Uani 1 1 d . . . H4A H 0.1012 -0.0823 0.1639 0.060 Uiso 1 1 calc R . . H4B H 0.1130 0.0198 0.0873 0.060 Uiso 1 1 calc R . . H4C H 0.0023 -0.0394 0.0881 0.060 Uiso 1 1 calc R . . C5 C -0.04985(18) 0.16944(19) 0.41147(12) 0.0441(5) Uani 1 1 d . . . H5A H 0.0246 0.1423 0.4467 0.066 Uiso 1 1 calc R . . H5B H -0.0761 0.1014 0.4015 0.066 Uiso 1 1 calc R . . H5C H -0.1128 0.2177 0.4397 0.066 Uiso 1 1 calc R . . C6 C 0.05901(17) 0.36965(16) 0.32954(13) 0.0400(4) Uani 1 1 d . . . H6A H 0.0045 0.4284 0.3554 0.060 Uiso 1 1 calc R . . H6B H 0.0849 0.4085 0.2766 0.060 Uiso 1 1 calc R . . H6C H 0.1298 0.3299 0.3671 0.060 Uiso 1 1 calc R . . C7 C -0.17277(17) 0.34883(19) 0.26168(15) 0.0492(5) Uani 1 1 d . . . H7A H -0.2233 0.2964 0.2542 0.074 Uiso 1 1 calc R . . H7B H -0.1620 0.3961 0.2073 0.074 Uiso 1 1 calc R . . H7C H -0.2118 0.4008 0.2986 0.074 Uiso 1 1 calc R . . C8 C 0.26477(13) 0.08112(12) 0.36949(9) 0.0206(3) Uani 1 1 d . . . C9 C 0.25681(14) 0.01789(14) 0.45027(9) 0.0262(3) Uani 1 1 d . . . H9 H 0.2091 -0.0374 0.4586 0.031 Uiso 1 1 calc R . . C10 C 0.31723(16) 0.03437(16) 0.51840(10) 0.0328(4) Uani 1 1 d . . . H10 H 0.3097 -0.0086 0.5727 0.039 Uiso 1 1 calc R . . C11 C 0.38837(16) 0.11337(16) 0.50722(11) 0.0341(4) Uani 1 1 d . . . H11 H 0.4314 0.1235 0.5535 0.041 Uiso 1 1 calc R . . C12 C 0.39632(15) 0.17746(15) 0.42804(11) 0.0295(3) Uani 1 1 d . . . H12 H 0.4446 0.2323 0.4205 0.035 Uiso 1 1 calc R . . C13 C 0.33477(13) 0.16303(13) 0.35907(9) 0.0225(3) Uani 1 1 d . . . C14 C 0.34186(14) 0.23746(12) 0.27455(10) 0.0238(3) Uani 1 1 d . . . H14A H 0.2592 0.2702 0.2490 0.029 Uiso 1 1 calc R . . H14B H 0.3739 0.3043 0.2820 0.029 Uiso 1 1 calc R . . C15 C 0.4172(2) 0.26027(16) 0.13643(12) 0.0412(4) Uani 1 1 d . . . H15A H 0.4517 0.3232 0.1472 0.062 Uiso 1 1 calc R . . H15B H 0.3339 0.2938 0.1142 0.062 Uiso 1 1 calc R . . H15C H 0.4652 0.2208 0.0957 0.062 Uiso 1 1 calc R . . C16 C 0.54396(15) 0.12672(16) 0.25044(13) 0.0354(4) Uani 1 1 d . . . H16A H 0.5954 0.0930 0.2087 0.053 Uiso 1 1 calc R . . H16B H 0.5460 0.0656 0.3004 0.053 Uiso 1 1 calc R . . H16C H 0.5736 0.1902 0.2654 0.053 Uiso 1 1 calc R . . C17 C 0.38364(13) -0.23667(12) 0.24288(9) 0.0216(3) Uani 1 1 d . . . H17 H 0.3012 -0.1828 0.2295 0.026 Uiso 1 1 calc R . . C18 C 0.19067(19) -0.3334(2) 0.33874(15) 0.0562(6) Uani 1 1 d . . . H18A H 0.1741 -0.3916 0.3855 0.084 Uiso 1 1 calc R . . H18B H 0.1675 -0.3507 0.2860 0.084 Uiso 1 1 calc R . . H18C H 0.1441 -0.2547 0.3436 0.084 Uiso 1 1 calc R . . C19 C 0.4438(2) -0.49559(15) 0.34901(14) 0.0446(5) Uani 1 1 d . . . H19A H 0.5299 -0.5010 0.3565 0.067 Uiso 1 1 calc R . . H19B H 0.4297 -0.5220 0.2978 0.067 Uiso 1 1 calc R . . H19C H 0.4179 -0.5455 0.3969 0.067 Uiso 1 1 calc R . . C20 C 0.39359(19) -0.29639(17) 0.43906(11) 0.0392(4) Uani 1 1 d . . . H20A H 0.3611 -0.3410 0.4866 0.059 Uiso 1 1 calc R . . H20B H 0.3582 -0.2122 0.4351 0.059 Uiso 1 1 calc R . . H20C H 0.4814 -0.3134 0.4470 0.059 Uiso 1 1 calc R . . C21 C 0.55919(19) -0.40591(18) 0.14209(14) 0.0467(5) Uani 1 1 d . . . H21A H 0.5599 -0.4423 0.0934 0.070 Uiso 1 1 calc R . . H21B H 0.5743 -0.4671 0.1931 0.070 Uiso 1 1 calc R . . H21C H 0.6223 -0.3632 0.1379 0.070 Uiso 1 1 calc R . . C22 C 0.2886(2) -0.38089(18) 0.13589(14) 0.0485(5) Uani 1 1 d . . . H22A H 0.2088 -0.3259 0.1328 0.073 Uiso 1 1 calc R . . H22B H 0.2951 -0.4449 0.1846 0.073 Uiso 1 1 calc R . . H22C H 0.2996 -0.4133 0.0851 0.073 Uiso 1 1 calc R . . C23 C 0.38521(19) -0.18378(17) 0.04936(11) 0.0389(4) Uani 1 1 d . . . H23A H 0.4531 -0.1471 0.0447 0.058 Uiso 1 1 calc R . . H23B H 0.3101 -0.1242 0.0524 0.058 Uiso 1 1 calc R . . H23C H 0.3802 -0.2183 0.0004 0.058 Uiso 1 1 calc R . . C24 C 0.61238(13) -0.16292(12) 0.20656(9) 0.0196(3) Uani 1 1 d . . . C25 C 0.62652(14) -0.09797(13) 0.12771(9) 0.0247(3) Uani 1 1 d . . . H25 H 0.5606 -0.0365 0.1012 0.030 Uiso 1 1 calc R . . C26 C 0.73447(16) -0.12081(15) 0.08702(10) 0.0304(3) Uani 1 1 d . . . H26 H 0.7417 -0.0755 0.0335 0.036 Uiso 1 1 calc R . . C27 C 0.83109(16) -0.21001(15) 0.12525(11) 0.0321(4) Uani 1 1 d . . . H27 H 0.9048 -0.2267 0.0977 0.038 Uiso 1 1 calc R . . C28 C 0.82011(15) -0.27496(14) 0.20372(10) 0.0286(3) Uani 1 1 d . . . H28 H 0.8868 -0.3361 0.2295 0.034 Uiso 1 1 calc R . . C29 C 0.71268(13) -0.25206(12) 0.24548(9) 0.0221(3) Uani 1 1 d . . . C30 C 0.70313(14) -0.32623(14) 0.33028(10) 0.0270(3) Uani 1 1 d . . . H30A H 0.6519 -0.2757 0.3646 0.032 Uiso 1 1 calc R . . H30B H 0.6621 -0.3873 0.3230 0.032 Uiso 1 1 calc R . . C31 C 0.87381(17) -0.29882(19) 0.40210(13) 0.0434(4) Uani 1 1 d . . . H31A H 0.8222 -0.2600 0.4416 0.065 Uiso 1 1 calc R . . H31B H 0.8830 -0.2399 0.3533 0.065 Uiso 1 1 calc R . . H31C H 0.9532 -0.3395 0.4292 0.065 Uiso 1 1 calc R . . C32 C 0.80028(18) -0.46803(18) 0.44877(12) 0.0469(5) Uani 1 1 d . . . H32A H 0.8777 -0.5068 0.4792 0.070 Uiso 1 1 calc R . . H32B H 0.7661 -0.5270 0.4310 0.070 Uiso 1 1 calc R . . H32C H 0.7446 -0.4270 0.4853 0.070 Uiso 1 1 calc R . . C33 C 0.1023(3) 0.4176(3) 0.0787(2) 0.0882(10) Uani 1 1 d . . . H33A H 0.1755 0.4264 0.1058 0.106 Uiso 1 1 calc R . . H33B H 0.0845 0.3414 0.1025 0.106 Uiso 1 1 calc R . . C34 C 0.0014(3) 0.5166(3) 0.0706(3) 0.1000(12) Uani 1 1 d . . . H34A H 0.0360 0.5852 0.0665 0.120 Uiso 1 1 calc R . . H34B H -0.0368 0.5080 0.1252 0.120 Uiso 1 1 calc R . . C35 C -0.0978(5) 0.5537(4) 0.0085(2) 0.1180(16) Uani 1 1 d . . . H35A H -0.1416 0.4914 0.0215 0.142 Uiso 1 1 calc R . . H35B H -0.1512 0.6237 0.0248 0.142 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 Ge 0.01867(8) 0.01913(8) 0.01761(8) -0.00237(5) -0.00083(5) -0.00200(6) P1 0.01654(17) 0.01890(16) 0.01987(17) -0.00344(13) -0.00130(12) -0.00316(13) P2 0.01724(17) 0.01717(16) 0.01701(16) -0.00235(12) 0.00033(12) -0.00281(13) Si1 0.0210(2) 0.0333(2) 0.0349(2) -0.00705(19) -0.00836(17) -0.00520(17) Si2 0.0189(2) 0.0289(2) 0.0363(2) -0.00865(18) 0.00046(17) 0.00189(16) Si3 0.0286(2) 0.0239(2) 0.0327(2) 0.00559(17) -0.00149(17) -0.01072(17) Si4 0.0323(2) 0.0244(2) 0.0304(2) -0.00985(17) -0.00574(17) -0.00457(17) N1 0.0235(7) 0.0194(6) 0.0301(7) -0.0048(5) 0.0053(5) -0.0056(5) N2 0.0234(7) 0.0299(7) 0.0292(7) 0.0058(5) 0.0034(5) 0.0056(5) C1 0.0163(7) 0.0225(7) 0.0258(7) -0.0025(5) -0.0034(5) -0.0019(5) C2 0.0628(15) 0.0570(14) 0.0616(15) -0.0044(11) -0.0413(12) -0.0036(11) C3 0.0285(9) 0.0481(11) 0.0619(13) -0.0195(10) 0.0065(8) -0.0169(8) C4 0.0317(10) 0.0567(12) 0.0400(10) -0.0225(9) -0.0021(7) -0.0152(8) C5 0.0350(10) 0.0521(11) 0.0409(10) -0.0097(9) 0.0119(8) -0.0030(8) C6 0.0305(9) 0.0348(9) 0.0556(12) -0.0226(8) 0.0023(8) 0.0008(7) C7 0.0262(10) 0.0449(11) 0.0691(15) -0.0181(10) -0.0072(9) 0.0097(8) C8 0.0173(7) 0.0214(6) 0.0212(7) -0.0062(5) -0.0013(5) 0.0001(5) C9 0.0232(8) 0.0283(7) 0.0238(7) -0.0037(6) 0.0011(6) -0.0017(6) C10 0.0316(9) 0.0415(9) 0.0202(7) -0.0065(6) -0.0014(6) 0.0008(7) C11 0.0302(9) 0.0421(9) 0.0291(8) -0.0187(7) -0.0069(6) 0.0016(7) C12 0.0244(8) 0.0299(8) 0.0363(9) -0.0165(7) -0.0038(6) -0.0027(6) C13 0.0192(7) 0.0206(6) 0.0265(7) -0.0083(5) -0.0010(5) -0.0001(5) C14 0.0229(7) 0.0169(6) 0.0319(8) -0.0072(6) 0.0018(6) -0.0041(5) C15 0.0552(12) 0.0275(8) 0.0402(10) -0.0005(7) 0.0174(8) -0.0147(8) C16 0.0202(8) 0.0340(9) 0.0576(11) -0.0203(8) 0.0038(7) -0.0083(7) C17 0.0208(7) 0.0183(6) 0.0246(7) -0.0012(5) -0.0019(5) -0.0049(5) C18 0.0354(11) 0.0667(14) 0.0589(13) 0.0202(11) -0.0011(9) -0.0249(10) C19 0.0558(13) 0.0229(8) 0.0522(12) 0.0047(8) -0.0108(9) -0.0140(8) C20 0.0507(11) 0.0367(9) 0.0277(8) 0.0026(7) 0.0082(7) -0.0140(8) C21 0.0441(11) 0.0421(10) 0.0540(12) -0.0281(9) -0.0062(9) 0.0037(9) C22 0.0562(13) 0.0399(10) 0.0540(12) -0.0107(9) -0.0182(10) -0.0192(9) C23 0.0486(11) 0.0449(10) 0.0250(8) -0.0101(7) -0.0020(7) -0.0127(8) C24 0.0201(7) 0.0184(6) 0.0204(7) -0.0051(5) 0.0023(5) -0.0042(5) C25 0.0274(8) 0.0224(7) 0.0218(7) -0.0020(5) 0.0026(5) -0.0037(6) C26 0.0343(9) 0.0303(8) 0.0243(7) -0.0022(6) 0.0099(6) -0.0067(7) C27 0.0294(9) 0.0314(8) 0.0338(9) -0.0076(7) 0.0141(7) -0.0044(7) C28 0.0237(8) 0.0252(7) 0.0331(8) -0.0049(6) 0.0065(6) -0.0003(6) C29 0.0220(7) 0.0193(6) 0.0235(7) -0.0031(5) 0.0034(5) -0.0036(5) C30 0.0203(7) 0.0269(7) 0.0269(7) 0.0033(6) 0.0030(6) -0.0005(6) C31 0.0267(9) 0.0560(12) 0.0417(10) -0.0050(9) -0.0042(7) -0.0037(8) C32 0.0388(10) 0.0443(11) 0.0366(10) 0.0157(8) 0.0064(8) 0.0089(8) C33 0.089(2) 0.0638(18) 0.103(3) -0.0100(17) -0.0116(19) -0.0092(16) C34 0.075(2) 0.073(2) 0.145(4) -0.026(2) 0.036(2) -0.0033(17) C35 0.199(5) 0.114(3) 0.067(2) -0.048(2) 0.005(3) -0.065(3) _cod_database_code 1100899 _journal_paper_doi 10.1021/om0501125