Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2002 data_global # *** Added by check_cif _journal_coden_Cambridge 186 loop_ _publ_author_name 'Mitzel, Norbert W.' 'Vojinovic, Krunoslav' _publ_contact_author_name 'Prof Norbert W Mitzel' _publ_contact_author_address ; Anorganisch-.chemisches Institut Technische Universitat Munchen Lichtenbergstr. 4 Garching 85747 GERMANY ; _publ_contact_author_phone '++49 89 2891-3145' _publ_contact_author_fax '++49 89 2891-3147' _publ_contact_author_email 'N.Mitzel@lrz.tum.de' _publ_requested_journal 'Dalton Transactions' #=========================================================================== #=========================================================================== # 3. TITLE AND AUTHOR LIST _publ_section_title ; (4+4)-Coordinate germanium atoms in Tetrakis(dialkylaminoxy)germanes ; data_kruno8 _database_code_CSD 177890 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetrakis(N,N-dimethylaminoxy)germane ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C8 H24 Ge N4 O4' _chemical_formula_weight 313.08 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ge' 'Ge' 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Triclinic _symmetry_space_group_name_H-M P-1 loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 8.9412(4) _cell_length_b 9.1281(4) _cell_length_c 9.2285(4) _cell_angle_alpha 96.516(3) _cell_angle_beta 96.585(2) _cell_angle_gamma 91.3672(16) _cell_volume 742.87(6) _cell_formula_units_Z 4 _cell_measurement_temperature 143(2) _cell_measurement_reflns_used 31651 _cell_measurement_theta_min 2.98 _cell_measurement_theta_max 27.31 _exptl_crystal_description Block _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.15 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.399 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 328 _exptl_absorpt_coefficient_mu 2.072 _exptl_absorpt_correction_type 'Intensity corrections by SCALEPACK' _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; SCALEPACK: Z. Otwinowski, W. Minor Methods Enzymol 1997, 276, 307. ; _diffrn_ambient_temperature 143(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 'Nonius DIP 2020' _diffrn_measurement_method 'phi scans 2.0°' _diffrn_detector_area_resol_mean '8 - 0.78' _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% None _diffrn_reflns_number 31651 _diffrn_reflns_av_R_equivalents 0.0880 _diffrn_reflns_av_sigmaI/netI 0.0742 _diffrn_reflns_limit_h_min 0 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 2.98 _diffrn_reflns_theta_max 27.39 _reflns_number_total 3104 _reflns_number_gt 2783 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius-DIP 2020 Software' _computing_cell_refinement 'SCALEPACK' _computing_data_reduction 'SCALEPACK, DIPSHEL' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.01' _computing_publication_material 'SHELXTL 5.01' _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^)+(0.0329P)^2^+6.8542P] 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 3104 _refine_ls_number_parameters 194 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0886 _refine_ls_R_factor_gt 0.0779 _refine_ls_wR_factor_ref 0.1838 _refine_ls_wR_factor_gt 0.1754 _refine_ls_goodness_of_fit_ref 1.161 _refine_ls_restrained_S_all 1.161 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge Ge 0.32435(8) 0.30437(8) -0.34528(8) 0.0213(2) Uani 1 1 d . . . O1 O 0.2798(5) 0.4853(5) -0.2817(5) 0.0270(10) Uani 1 1 d . . . O2 O 0.5189(5) 0.2861(5) -0.3010(6) 0.0292(11) Uani 1 1 d . . . O3 O 0.2193(6) 0.1629(6) -0.2822(5) 0.0336(12) Uani 1 1 d . . . O4 O 0.2798(5) 0.2769(5) -0.5382(5) 0.0243(10) Uani 1 1 d . . . N1 N 0.3746(6) 0.5231(6) -0.1405(6) 0.0247(12) Uani 1 1 d . . . N2 N 0.5440(6) 0.1423(6) -0.3847(6) 0.0256(12) Uani 1 1 d . . . N3 N 0.1222(6) 0.3229(6) -0.5533(6) 0.0253(12) Uani 1 1 d . . . N4 N 0.1936(7) 0.2079(7) -0.1304(6) 0.0283(13) Uani 1 1 d . . . C1 C 0.4814(9) 0.6379(9) -0.1648(9) 0.0368(18) Uani 1 1 d . . . H1A H 0.556(5) 0.665(4) -0.070(5) 0.05(3) Uiso 1 1 calc R . . H1B H 0.424(3) 0.730(5) -0.191(6) 0.05(3) Uiso 1 1 calc R . . H1C H 0.541(5) 0.600(3) -0.251(5) 0.03(2) Uiso 1 1 calc R . . C2 C 0.2744(9) 0.5829(9) -0.0399(9) 0.0346(17) Uani 1 1 d . . . H2A H 0.329(3) 0.617(5) 0.048(4) 0.03(2) Uiso 1 1 calc R . . H2B H 0.207(5) 0.511(4) -0.026(4) 0.07(3) Uiso 1 1 calc R . . H2C H 0.224(5) 0.659(5) -0.078(3) 0.016(17) Uiso 1 1 calc R . . C3 C 0.6002(8) 0.0492(8) -0.2750(9) 0.0329(17) Uani 1 1 d . . . H3A H 0.519(5) 0.023(6) -0.221(6) 0.06(3) Uiso 1 1 calc R . . H3B H 0.680(6) 0.102(4) -0.208(5) 0.08(4) Uiso 1 1 calc R . . H3C H 0.639(7) -0.039(6) -0.323(3) 0.07(3) Uiso 1 1 calc R . . C4 C 0.6610(9) 0.1743(8) -0.4743(8) 0.0330(16) Uani 1 1 d . . . H4A H 0.684(4) 0.082(4) -0.535(5) 0.05(3) Uiso 1 1 calc R . . H4B H 0.753(5) 0.213(5) -0.410(3) 0.03(2) Uiso 1 1 calc R . . H4C H 0.626(3) 0.249(5) -0.539(5) 0.03(2) Uiso 1 1 calc R . . C5 C 0.0337(9) 0.1938(10) -0.6258(9) 0.0389(19) Uani 1 1 d . . . H5A H -0.075(5) 0.222(2) -0.651(5) 0.07(3) Uiso 1 1 calc R . . H5B H 0.037(5) 0.113(4) -0.557(4) 0.05(2) Uiso 1 1 calc R . . H5C H 0.078(4) 0.155(4) -0.720(5) 0.03(2) Uiso 1 1 calc R . . C6 C 0.1192(9) 0.4406(9) -0.6465(9) 0.0392(19) Uani 1 1 d . . . H6A H 0.187(6) 0.526(5) -0.596(3) 0.05(3) Uiso 1 1 calc R . . H6B H 0.012(5) 0.475(4) -0.665(5) 0.07(3) Uiso 1 1 calc R . . H6C H 0.156(6) 0.403(2) -0.743(5) 0.03(2) Uiso 1 1 calc R . . C7 C 0.0347(9) 0.2244(11) -0.1356(12) 0.049(2) Uani 1 1 d . . . H7A H 0.010(2) 0.251(7) -0.039(6) 0.06(3) Uiso 1 1 calc R . . H7B H -0.016(3) 0.134(6) -0.175(7) 0.09(4) Uiso 1 1 calc R . . H7C H 0.005(2) 0.299(7) -0.196(7) 0.07(3) Uiso 1 1 calc R . . C8 C 0.2357(9) 0.0812(10) -0.0535(9) 0.0373(18) Uani 1 1 d . . . H8A H 0.228(5) 0.105(2) 0.051(5) 0.04(2) Uiso 1 1 calc R . . H8B H 0.339(5) 0.057(3) -0.067(4) 0.020(18) Uiso 1 1 calc R . . H8C H 0.168(4) -0.003(4) -0.093(4) 0.05(3) 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 0.0234(4) 0.0203(4) 0.0195(4) 0.0026(3) -0.0009(2) 0.0038(2) O1 0.033(3) 0.023(2) 0.022(2) -0.003(2) -0.0033(19) 0.004(2) O2 0.028(3) 0.022(2) 0.034(3) -0.007(2) -0.001(2) 0.0100(19) O3 0.045(3) 0.034(3) 0.022(3) 0.002(2) 0.004(2) -0.004(2) O4 0.023(2) 0.030(3) 0.019(2) -0.001(2) -0.0007(18) 0.0051(19) N1 0.028(3) 0.024(3) 0.021(3) 0.002(2) 0.000(2) 0.003(2) N2 0.028(3) 0.023(3) 0.025(3) 0.000(3) 0.000(2) 0.007(2) N3 0.012(2) 0.032(3) 0.031(3) 0.003(3) -0.003(2) 0.005(2) N4 0.030(3) 0.032(3) 0.023(3) 0.004(3) 0.001(2) 0.000(2) C1 0.036(4) 0.035(4) 0.037(4) 0.007(4) -0.004(3) -0.003(3) C2 0.039(4) 0.033(4) 0.031(4) 0.002(4) 0.002(3) 0.006(3) C3 0.031(4) 0.032(4) 0.035(4) 0.007(4) 0.001(3) 0.011(3) C4 0.040(4) 0.030(4) 0.029(4) 0.003(3) 0.002(3) 0.001(3) C5 0.028(4) 0.049(5) 0.037(4) 0.004(4) -0.003(3) -0.007(3) C6 0.039(4) 0.036(4) 0.042(5) 0.011(4) -0.005(4) 0.005(3) C7 0.031(4) 0.047(5) 0.070(7) 0.016(5) 0.008(4) 0.011(4) C8 0.034(4) 0.051(5) 0.031(4) 0.019(4) 0.003(3) 0.011(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 Ge O2 1.757(5) . ? Ge O1 1.759(5) . ? Ge O4 1.767(4) . ? Ge O3 1.768(5) . ? O1 N1 1.471(7) . ? O2 N2 1.481(7) . ? O3 N4 1.459(8) . ? O4 N3 1.476(7) . ? N1 C2 1.436(9) . ? N1 C1 1.454(9) . ? N2 C4 1.449(9) . ? N2 C3 1.449(9) . ? N3 C6 1.449(9) . ? N3 C5 1.456(10) . ? N4 C7 1.428(10) . ? N4 C8 1.459(9) . ? C1 H1A 1.0385 . ? C1 H1B 1.0385 . ? C1 H1C 1.0385 . ? C2 H2A 0.9163 . ? C2 H2B 0.9163 . ? C2 H2C 0.9163 . ? C3 H3A 0.9640 . ? C3 H3B 0.9640 . ? C3 H3C 0.9640 . ? C4 H4A 0.9939 . ? C4 H4B 0.9939 . ? C4 H4C 0.9939 . ? C5 H5A 1.0230 . ? C5 H5B 1.0230 . ? C5 H5C 1.0230 . ? C6 H6A 1.0132 . ? C6 H6B 1.0132 . ? C6 H6C 1.0132 . ? C7 H7A 0.9492 . ? C7 H7B 0.9492 . ? C7 H7C 0.9492 . ? C8 H8A 0.9748 . ? C8 H8B 0.9748 . ? C8 H8C 0.9748 . ? 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 O2 Ge O1 108.1(2) . . ? O2 Ge O4 109.1(2) . . ? O1 Ge O4 108.6(2) . . ? O2 Ge O3 111.4(2) . . ? O1 Ge O3 115.2(2) . . ? O4 Ge O3 104.2(2) . . ? N1 O1 Ge 105.7(3) . . ? N2 O2 Ge 102.0(3) . . ? N4 O3 Ge 109.2(4) . . ? N3 O4 Ge 100.8(3) . . ? C2 N1 C1 109.7(6) . . ? C2 N1 O1 105.4(5) . . ? C1 N1 O1 105.8(5) . . ? C4 N2 C3 110.3(6) . . ? C4 N2 O2 104.5(5) . . ? C3 N2 O2 105.2(5) . . ? C6 N3 C5 111.2(6) . . ? C6 N3 O4 105.3(5) . . ? C5 N3 O4 105.5(5) . . ? C7 N4 C8 109.2(6) . . ? C7 N4 O3 105.1(6) . . ? C8 N4 O3 104.5(6) . . ? N1 C1 H1A 109.5 . . ? N1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? N1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N1 C2 H2A 109.5 . . ? N1 C2 H2B 109.5 . . ? H2A C2 H2B 109.5 . . ? N1 C2 H2C 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? N2 C3 H3A 109.5 . . ? N2 C3 H3B 109.5 . . ? H3A C3 H3B 109.5 . . ? N2 C3 H3C 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? N2 C4 H4A 109.5 . . ? N2 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N2 C4 H4C 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? N3 C5 H5A 109.5 . . ? N3 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N3 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N3 C6 H6A 109.5 . . ? N3 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N3 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N4 C7 H7A 109.5 . . ? N4 C7 H7B 109.5 . . ? H7A C7 H7B 109.5 . . ? N4 C7 H7C 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? N4 C8 H8A 109.5 . . ? N4 C8 H8B 109.5 . . ? H8A C8 H8B 109.5 . . ? N4 C8 H8C 109.5 . . ? H8A C8 H8C 109.5 . . ? H8B C8 H8C 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 O2 Ge O1 N1 -37.9(4) . . . . ? O4 Ge O1 N1 -156.2(3) . . . . ? O3 Ge O1 N1 87.4(4) . . . . ? O1 Ge O2 N2 -169.5(3) . . . . ? O4 Ge O2 N2 -51.5(4) . . . . ? O3 Ge O2 N2 63.0(4) . . . . ? O2 Ge O3 N4 86.7(4) . . . . ? O1 Ge O3 N4 -37.0(5) . . . . ? O4 Ge O3 N4 -155.8(4) . . . . ? O2 Ge O4 N3 -170.1(3) . . . . ? O1 Ge O4 N3 -52.4(4) . . . . ? O3 Ge O4 N3 70.8(4) . . . . ? Ge O1 N1 C2 -131.5(5) . . . . ? Ge O1 N1 C1 112.3(5) . . . . ? Ge O2 N2 C4 124.9(4) . . . . ? Ge O2 N2 C3 -118.9(5) . . . . ? Ge O4 N3 C6 122.5(5) . . . . ? Ge O4 N3 C5 -119.7(5) . . . . ? Ge O3 N4 C7 113.8(5) . . . . ? Ge O3 N4 C8 -131.3(5) . . . . ? _diffrn_measured_fraction_theta_max 0.917 _diffrn_reflns_theta_full 27.39 _diffrn_measured_fraction_theta_full 0.917 _refine_diff_density_max 1.244 _refine_diff_density_min -0.912 _refine_diff_density_rms 0.153 ### NEXT ### data_kruno9 _database_code_CSD 177891 _audit_creation_method SHELXL-97 _chemical_name_systematic ; Tetrakis(isopropoxy)germane ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C12 H28 Ge O4' _chemical_formula_weight 308.93 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' 'O' 'O' 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Ge' 'Ge' 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Tetragonal _symmetry_space_group_name_H-M I41/a loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-y+3/4, x+1/4, z+1/4' 'y+3/4, -x+3/4, z+3/4' 'x+1/2, y+1/2, z+1/2' '-x+1, -y+1/2, z+1' '-y+5/4, x+3/4, z+3/4' 'y+5/4, -x+5/4, z+5/4' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'y-3/4, -x-1/4, -z-1/4' '-y-3/4, x-3/4, -z-3/4' '-x+1/2, -y+1/2, -z+1/2' 'x, y+1/2, -z' 'y-1/4, -x+1/4, -z+1/4' '-y-1/4, x-1/4, -z-1/4' _cell_length_a 8.0693(6) _cell_length_b 8.0693(6) _cell_length_c 24.7868(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1613.96(19) _cell_formula_units_Z 4 _cell_measurement_temperature 133(2) _cell_measurement_reflns_used 100 _cell_measurement_theta_min 23.0 _cell_measurement_theta_max 27.3 _exptl_crystal_description Cylinder _exptl_crystal_colour Colourless _exptl_crystal_size_max 1.00 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.271 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 656 _exptl_absorpt_coefficient_mu 1.900 _exptl_absorpt_correction_type 'DELABS from PLATON' _exptl_absorpt_correction_T_min 0.127 _exptl_absorpt_correction_T_max 0.597 _exptl_absorpt_process_details ? _exptl_special_details ; Crystal grown in situ in a capillary by slowly cooling the melt after establishing a solid liquid equilibrium and selecting a suitable seed crystal (others removed by local melting) ; _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 'NONIUS Turbo CAD4' _diffrn_measurement_method 'omega-2theta-scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% None _diffrn_reflns_number 4677 _diffrn_reflns_av_R_equivalents 0.0665 _diffrn_reflns_av_sigmaI/netI 0.0377 _diffrn_reflns_limit_h_min -11 _diffrn_reflns_limit_h_max 11 _diffrn_reflns_limit_k_min -11 _diffrn_reflns_limit_k_max 11 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 34 _diffrn_reflns_theta_min 2.65 _diffrn_reflns_theta_max 30.09 _reflns_number_total 1185 _reflns_number_gt 1101 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Nonius-CAD4 Software' _computing_cell_refinement 'Nonius-CAD4 Software' _computing_data_reduction 'XCAD4P, Harms, Marburg' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'SHELXTL 5.01' _computing_publication_material 'SHELXTL 5.01' _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^)+(0.0623P)^2^+0.4053P] where P==(Fo^2^+2Fc^2^)/3' _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _atom_sites_solution_hydrogens difmap _refine_ls_hydrogen_treatment refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1185 _refine_ls_number_parameters 67 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0355 _refine_ls_wR_factor_ref 0.0860 _refine_ls_wR_factor_gt 0.0838 _refine_ls_goodness_of_fit_ref 1.065 _refine_ls_restrained_S_all 1.065 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 loop_ _atom_site_label _atom_site_type_symbol _atom_site_fract_x _atom_site_fract_y _atom_site_fract_z _atom_site_U_iso_or_equiv _atom_site_adp_type _atom_site_occupancy _atom_site_symmetry_multiplicity _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_assembly _atom_site_disorder_group Ge Ge 0.5000 0.7500 0.1250 0.02018(13) Uani 1 4 d S . . O O 0.31888(15) 0.77057(14) 0.08714(4) 0.0291(2) Uani 1 1 d . . . C1 C 0.2787(2) 0.92894(18) 0.06301(6) 0.0259(3) Uani 1 1 d . . . H1 H 0.363(3) 1.011(3) 0.0700(9) 0.029(5) Uiso 1 1 d . . . C2 C 0.1212(3) 0.9908(3) 0.08895(9) 0.0412(4) Uani 1 1 d . . . H2A H 0.026(5) 0.909(5) 0.0819(14) 0.074(10) Uiso 1 1 d . . . H2B H 0.089(4) 1.101(4) 0.0754(11) 0.054(7) Uiso 1 1 d . . . H2C H 0.138(5) 1.004(4) 0.1300(11) 0.048(8) Uiso 1 1 d . . . C3 C 0.2633(3) 0.9033(2) 0.00283(7) 0.0432(5) Uani 1 1 d . . . H3A H 0.233(4) 0.999(4) -0.0152(14) 0.051(7) Uiso 1 1 d . . . H3B H 0.363(4) 0.858(4) -0.0109(12) 0.055(8) Uiso 1 1 d . . . H3C H 0.168(4) 0.831(4) -0.0035(13) 0.059(8) Uiso 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge 0.02025(15) 0.02025(15) 0.02004(17) 0.000 0.000 0.000 O 0.0334(6) 0.0208(5) 0.0331(5) 0.0048(4) -0.0130(4) -0.0042(4) C1 0.0300(7) 0.0194(6) 0.0282(6) 0.0033(5) -0.0077(5) -0.0017(5) C2 0.0428(10) 0.0302(9) 0.0506(10) 0.0016(7) 0.0057(8) 0.0056(8) C3 0.0703(15) 0.0318(9) 0.0274(7) 0.0029(6) -0.0066(8) 0.0068(9) _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 Ge O 1.7449(11) . ? Ge O 1.7448(11) 12_766 ? Ge O 1.7448(11) 6_564 ? Ge O 1.7449(11) 15_565 ? O C1 1.4477(18) . ? C1 C2 1.509(3) . ? C1 C3 1.511(2) . ? C1 H1 0.97(2) . ? C2 H2A 1.03(4) . ? C2 H2B 0.99(3) . ? C2 H2C 1.03(3) . ? C3 H3A 0.92(4) . ? C3 H3B 0.95(3) . ? C3 H3C 0.98(3) . ? 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 O Ge O 106.82(4) . 12_766 ? O Ge O 114.92(8) . 6_564 ? O Ge O 106.82(4) 12_766 6_564 ? O Ge O 106.82(4) . 15_565 ? O Ge O 114.92(8) 12_766 15_565 ? O Ge O 106.82(4) 6_564 15_565 ? C1 O Ge 119.58(9) . . ? O C1 C2 107.73(13) . . ? O C1 C3 107.79(13) . . ? C2 C1 C3 113.35(16) . . ? O C1 H1 111.8(13) . . ? C2 C1 H1 107.0(14) . . ? C3 C1 H1 109.3(13) . . ? C1 C2 H2A 110(2) . . ? C1 C2 H2B 112.1(17) . . ? H2A C2 H2B 109(3) . . ? C1 C2 H2C 110(2) . . ? H2A C2 H2C 109(3) . . ? H2B C2 H2C 106(3) . . ? C1 C3 H3A 113(2) . . ? C1 C3 H3B 109.6(19) . . ? H3A C3 H3B 112(3) . . ? C1 C3 H3C 107.8(19) . . ? H3A C3 H3C 102(3) . . ? H3B C3 H3C 113(3) . . ? 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 O Ge O C1 163.34(13) 12_766 . . . ? O Ge O C1 -78.39(11) 6_564 . . . ? O Ge O C1 39.89(9) 15_565 . . . ? Ge O C1 C2 -115.56(14) . . . . ? Ge O C1 C3 121.79(14) . . . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 30.09 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.789 _refine_diff_density_min -1.047 _refine_diff_density_rms 0.094