#------------------------------------------------------------------------------ #$Date: 2016-03-26 14:43:29 +0200 (Sat, 26 Mar 2016) $ #$Revision: 180274 $ #$URL: file:///home/coder/svn-repositories/cod/cif/7/11/60/7116052.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_7116052 loop_ _publ_author_name 'P. Steiniger' 'G. Bendt' 'D. Blaser' 'C. Wolper' 'S. Schulz' _publ_section_title ; Germane vs. digermane formation ; _journal_name_full Chem.Commun. _journal_page_first 15461 _journal_paper_doi 10.1039/C4cc07921C _journal_volume 50 _journal_year 2014 _chemical_formula_moiety 'C10 H24 Ge N2 Si' _chemical_formula_sum 'C10 H24 Ge N2 Si' _chemical_formula_weight 272.99 _chemical_name_systematic ? _space_group_crystal_system monoclinic _space_group_IT_number 14 _space_group_name_Hall '-P 2yn' _space_group_name_H-M_alt 'P 1 21/n 1' _symmetry_space_group_name_Hall '-P 2yn' _symmetry_space_group_name_H-M 'P 1 21/n 1' _atom_sites_solution_hydrogens geom _atom_sites_solution_primary direct _atom_sites_solution_secondary difmap _audit_creation_method SHELXL-2013 _cell_angle_alpha 90 _cell_angle_beta 94.704(8) _cell_angle_gamma 90 _cell_formula_units_Z 4 _cell_length_a 12.9266(18) _cell_length_b 6.3714(11) _cell_length_c 18.087(2) _cell_measurement_reflns_used 3357 _cell_measurement_temperature 230(1) _cell_measurement_theta_max 27.87 _cell_measurement_theta_min 2.26 _cell_volume 1484.6(4) _computing_cell_refinement 'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009' _computing_data_collection 'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009' _computing_data_reduction 'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009' _computing_molecular_graphics 'BRUKER AXS Inc. 2008 Vers. 2008/4' _computing_publication_material 'BRUKER AXS Inc. 2013 Vers. 2013/4' _computing_structure_refinement 'BRUKER AXS Inc. 2013 Vers. 2013/4' _computing_structure_solution 'BRUKER D8 KAPPA APEX 2 Vers. 3.0-2009' _diffrn_ambient_temperature 230(1) _diffrn_detector_area_resol_mean 512 _diffrn_measured_fraction_theta_full 0.891 _diffrn_measured_fraction_theta_max 0.815 _diffrn_measurement_device_type ; Bruker D8 KAPPA series II with APEX II area detector system ; _diffrn_measurement_method ; PHI scan 360 deg, kappa 0 deg ; _diffrn_radiation_monochromator 'Triumph Goebel mirror' _diffrn_radiation_type MoK\a _diffrn_radiation_wavelength 0.71073 _diffrn_reflns_av_R_equivalents 0.0795 _diffrn_reflns_av_unetI/netI 0.0732 _diffrn_reflns_Laue_measured_fraction_full 0.891 _diffrn_reflns_Laue_measured_fraction_max 0.815 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_h_min -18 _diffrn_reflns_limit_k_max 6 _diffrn_reflns_limit_k_min -6 _diffrn_reflns_limit_l_max 25 _diffrn_reflns_limit_l_min -25 _diffrn_reflns_number 13962 _diffrn_reflns_point_group_measured_fraction_full 0.891 _diffrn_reflns_point_group_measured_fraction_max 0.815 _diffrn_reflns_theta_full 25.242 _diffrn_reflns_theta_max 30.669 _diffrn_reflns_theta_min 1.866 _diffrn_source 'sealed X-RAY tube' _exptl_absorpt_coefficient_mu 2.118 _exptl_absorpt_correction_T_max 0.75 _exptl_absorpt_correction_T_min 0.21 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_process_details ; BRUKER AXS SMART APEX 2 Vers. 3.0-2009 R.H. Blessing, Acta Cryst. (1995) A51 33-38 ; _exptl_crystal_colour colourless _exptl_crystal_density_diffrn 1.221 _exptl_crystal_description cylindric _exptl_crystal_F_000 576 _exptl_crystal_size_max 0.300 _exptl_crystal_size_mid 0.300 _exptl_crystal_size_min 0.300 _refine_diff_density_max 1.355 _refine_diff_density_min -0.945 _refine_diff_density_rms 0.166 _refine_ls_extinction_method none _refine_ls_goodness_of_fit_ref 1.092 _refine_ls_hydrogen_treatment constr _refine_ls_matrix_type full _refine_ls_number_parameters 135 _refine_ls_number_reflns 3739 _refine_ls_number_restraints 0 _refine_ls_restrained_S_all 1.092 _refine_ls_R_factor_all 0.1348 _refine_ls_R_factor_gt 0.0802 _refine_ls_shift/su_max 0.000 _refine_ls_shift/su_mean 0.000 _refine_ls_structure_factor_coef Fsqd _refine_ls_weighting_details 'w=1/[\s^2^(Fo^2^)+(0.1358P)^2^+1.3024P] where P=(Fo^2^+2Fc^2^)/3' _refine_ls_weighting_scheme calc _refine_ls_wR_factor_gt 0.1985 _refine_ls_wR_factor_ref 0.2562 _reflns_Friedel_coverage 0.000 _reflns_number_gt 2201 _reflns_number_total 3739 _reflns_threshold_expression 'I > 2\s(I)' _cod_data_source_file c4cc07921c2.cif _cod_data_source_block gb_166m _cod_database_code 7116052 #BEGIN Tags that were not found in dictionaries: _shelx_space_group_comment ; The symmetry employed for this shelxl refinement is uniquely defined by the following loop, which should always be used as a source of symmetry information in preference to the above space-group names. They are only intended as comments. ; _shelx_estimated_absorpt_t_min 0.569 _shelx_estimated_absorpt_t_max 0.569 _shelxl_version_number 2013-4 _shelx_res_file ; TITL gb_166m in P2(1)/n ***Hochtemperatur*** CELL 0.71073 12.9266 6.3714 18.0866 90.000 94.704 90.000 ZERR 4.00 0.0018 0.0011 0.0024 0.000 0.008 0.000 LATT 1 SYMM 0.5-X, 0.5+Y, 0.5-Z SFAC C H N SI GE UNIT 40 96 8 4 4 TEMP -43 L.S. 14 SIZE .3 .3 .3 ACTA FMAP 2 PLAN 10 WGHT 0.135800 1.302400 FVAR 0.11864 GE1 5 0.638750 0.202667 0.246730 11.00000 0.04160 0.10387 = 0.04032 -0.00888 -0.00010 0.01442 SI1 4 0.482836 0.395136 0.303126 11.00000 0.04257 0.06302 = 0.04803 -0.00719 -0.00172 0.01064 N1 3 0.508301 0.306073 0.216175 11.00000 0.04353 0.06883 = 0.03940 -0.00273 -0.00702 0.00023 N2 3 0.602372 0.300771 0.337186 11.00000 0.03989 0.07128 = 0.03576 -0.00417 0.00166 0.00692 C1 1 0.450746 0.303098 0.143516 11.00000 0.04562 0.07357 = 0.04949 -0.00140 -0.01187 0.00285 C2 1 0.428730 0.526294 0.116950 11.00000 0.14183 0.10246 = 0.06167 0.01007 -0.03973 -0.00108 AFIX 137 H2A 2 0.377888 0.589815 0.146591 11.00000 -1.50000 H2B 2 0.401853 0.524002 0.065284 11.00000 -1.50000 H2C 2 0.492402 0.607459 0.122028 11.00000 -1.50000 AFIX 0 C3 1 0.350255 0.188600 0.147541 11.00000 0.09338 0.21047 = 0.08522 0.02727 -0.04192 -0.08233 AFIX 137 H3A 2 0.363912 0.048358 0.166807 11.00000 -1.50000 H3B 2 0.314611 0.179492 0.098321 11.00000 -1.50000 H3C 2 0.307120 0.263749 0.180105 11.00000 -1.50000 AFIX 0 C4 1 0.514350 0.199247 0.086851 11.00000 0.07584 0.17058 = 0.04901 -0.02930 -0.01496 0.02570 AFIX 137 H4A 2 0.568998 0.293857 0.074232 11.00000 -1.50000 H4B 2 0.469798 0.166630 0.042560 11.00000 -1.50000 H4C 2 0.544915 0.070867 0.107537 11.00000 -1.50000 AFIX 0 C5 1 0.661713 0.298234 0.409606 11.00000 0.04866 0.07356 = 0.03620 0.00104 -0.00117 0.00233 C6 1 0.764847 0.195000 0.402553 11.00000 0.05292 0.12929 = 0.05715 -0.00952 -0.01856 0.02758 AFIX 137 H6A 2 0.754189 0.059084 0.378988 11.00000 -1.50000 H6B 2 0.800459 0.176756 0.451454 11.00000 -1.50000 H6C 2 0.806525 0.282461 0.372659 11.00000 -1.50000 AFIX 0 C7 1 0.601283 0.180016 0.465475 11.00000 0.08671 0.15441 = 0.05018 0.02942 0.00090 -0.02448 AFIX 137 H7A 2 0.532962 0.242092 0.466924 11.00000 -1.50000 H7B 2 0.638233 0.188815 0.514266 11.00000 -1.50000 H7C 2 0.594239 0.033986 0.450752 11.00000 -1.50000 AFIX 0 C8 1 0.681751 0.523400 0.436451 11.00000 0.07787 0.09455 = 0.05616 -0.01149 -0.01546 0.00019 AFIX 137 H8A 2 0.716597 0.600650 0.399510 11.00000 -1.50000 H8B 2 0.725169 0.521470 0.482806 11.00000 -1.50000 H8C 2 0.616193 0.590850 0.444057 11.00000 -1.50000 AFIX 0 C9 1 0.369497 0.266442 0.342526 11.00000 0.04806 0.09937 = 0.08391 -0.00208 0.01830 0.01145 AFIX 137 H9A 2 0.370921 0.116871 0.332657 11.00000 -1.50000 H9B 2 0.305565 0.325844 0.319684 11.00000 -1.50000 H9C 2 0.373222 0.289865 0.395670 11.00000 -1.50000 AFIX 0 C10 1 0.468129 0.679194 0.309591 11.00000 0.10991 0.07766 = 0.08937 -0.01547 -0.03225 0.02091 AFIX 137 H10A 2 0.455697 0.717083 0.360046 11.00000 -1.50000 H10B 2 0.409886 0.724271 0.276127 11.00000 -1.50000 H10C 2 0.530984 0.747243 0.296038 11.00000 -1.50000 AFIX 0 HKLF 4 REM gb_166m in P2(1)/n ***Hochtemperatur*** REM R1 = 0.0802 for 2201 Fo > 4sig(Fo) and 0.1348 for all 3739 data REM 135 parameters refined using 0 restraints END WGHT 0.1358 1.3028 REM Highest difference peak 1.355, deepest hole -0.945, 1-sigma level 0.166 Q1 1 0.6176 0.3219 0.2668 11.00000 0.05 1.35 Q2 1 0.6683 0.1090 0.2222 11.00000 0.05 1.31 Q3 1 0.6760 0.3005 0.2162 11.00000 0.05 1.27 Q4 1 0.6071 0.0984 0.2653 11.00000 0.05 1.15 Q5 1 0.5574 0.2876 0.2555 11.00000 0.05 0.85 Q6 1 0.7054 -0.1103 0.3104 11.00000 0.05 0.74 Q7 1 0.5068 0.2811 0.2730 11.00000 0.05 0.71 Q8 1 0.4987 0.3965 0.2486 11.00000 0.05 0.71 Q9 1 0.4502 0.5034 0.3252 11.00000 0.05 0.61 Q10 1 0.5185 0.4951 0.2823 11.00000 0.05 0.59 ; _shelx_res_checksum 44889 #END Tags that were not found in dictionaries loop_ _space_group_symop_operation_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' 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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp Ge1 Ge 0.63875(5) 0.20267(16) 0.24673(3) 0.0621(3) Uani 1 1 d . . Si1 Si 0.48284(12) 0.3951(3) 0.30313(9) 0.0515(5) Uani 1 1 d . . N1 N 0.5083(4) 0.3061(9) 0.2162(3) 0.0512(12) Uani 1 1 d . . N2 N 0.6024(3) 0.3008(9) 0.3372(2) 0.0491(12) Uani 1 1 d . . C1 C 0.4507(5) 0.3031(12) 0.1435(3) 0.0571(16) Uani 1 1 d . . C2 C 0.4287(10) 0.5263(17) 0.1170(5) 0.105(3) Uani 1 1 d . . H2A H 0.3779 0.5898 0.1466 0.157 Uiso 1 1 calc R U H2B H 0.4019 0.5240 0.0653 0.157 Uiso 1 1 calc R U H2C H 0.4924 0.6075 0.1220 0.157 Uiso 1 1 calc R U C3 C 0.3503(9) 0.189(2) 0.1475(6) 0.132(6) Uani 1 1 d . . H3A H 0.3639 0.0484 0.1668 0.199 Uiso 1 1 calc R U H3B H 0.3146 0.1795 0.0983 0.199 Uiso 1 1 calc R U H3C H 0.3071 0.2637 0.1801 0.199 Uiso 1 1 calc R U C4 C 0.5144(7) 0.199(2) 0.0869(4) 0.100(3) Uani 1 1 d . . H4A H 0.5690 0.2939 0.0742 0.149 Uiso 1 1 calc R U H4B H 0.4698 0.1666 0.0426 0.149 Uiso 1 1 calc R U H4C H 0.5449 0.0709 0.1075 0.149 Uiso 1 1 calc R U C5 C 0.6617(5) 0.2982(12) 0.4096(3) 0.0531(15) Uani 1 1 d . . C6 C 0.7648(6) 0.1950(16) 0.4026(4) 0.081(3) Uani 1 1 d . . H6A H 0.7542 0.0591 0.3790 0.122 Uiso 1 1 calc R U H6B H 0.8005 0.1768 0.4515 0.122 Uiso 1 1 calc R U H6C H 0.8065 0.2825 0.3727 0.122 Uiso 1 1 calc R U C7 C 0.6013(7) 0.1800(19) 0.4655(4) 0.097(3) Uani 1 1 d . . H7A H 0.5330 0.2421 0.4669 0.146 Uiso 1 1 calc R U H7B H 0.6382 0.1888 0.5143 0.146 Uiso 1 1 calc R U H7C H 0.5942 0.0340 0.4508 0.146 Uiso 1 1 calc R U C8 C 0.6818(7) 0.5234(15) 0.4365(4) 0.077(2) Uani 1 1 d . . H8A H 0.7166 0.6006 0.3995 0.116 Uiso 1 1 calc R U H8B H 0.7252 0.5215 0.4828 0.116 Uiso 1 1 calc R U H8C H 0.6162 0.5908 0.4441 0.116 Uiso 1 1 calc R U C9 C 0.3695(6) 0.2664(15) 0.3425(5) 0.076(2) Uani 1 1 d . . H9A H 0.3709 0.1169 0.3327 0.115 Uiso 1 1 calc R U H9B H 0.3056 0.3258 0.3197 0.115 Uiso 1 1 calc R U H9C H 0.3732 0.2899 0.3957 0.115 Uiso 1 1 calc R U C10 C 0.4681(8) 0.6792(16) 0.3096(6) 0.095(3) Uani 1 1 d . . H10A H 0.4557 0.7171 0.3600 0.142 Uiso 1 1 calc R U H10B H 0.4099 0.7243 0.2761 0.142 Uiso 1 1 calc R U H10C H 0.5310 0.7472 0.2960 0.142 Uiso 1 1 calc R U loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Ge1 0.0416(4) 0.1039(8) 0.0403(4) -0.0089(3) -0.0001(2) 0.0144(3) Si1 0.0426(8) 0.0630(13) 0.0480(8) -0.0072(8) -0.0017(6) 0.0106(7) N1 0.044(2) 0.069(4) 0.039(2) -0.003(2) -0.0070(18) 0.000(2) N2 0.040(2) 0.071(4) 0.036(2) -0.004(2) 0.0017(17) 0.007(2) C1 0.046(3) 0.074(5) 0.049(3) -0.001(3) -0.012(2) 0.003(3) C2 0.142(9) 0.102(9) 0.062(5) 0.010(5) -0.040(5) -0.001(6) C3 0.093(7) 0.210(15) 0.085(7) 0.027(7) -0.042(5) -0.082(8) C4 0.076(5) 0.171(11) 0.049(4) -0.029(5) -0.015(4) 0.026(6) C5 0.049(3) 0.074(5) 0.036(2) 0.001(3) -0.001(2) 0.002(3) C6 0.053(4) 0.129(8) 0.057(4) -0.010(4) -0.019(3) 0.028(4) C7 0.087(6) 0.154(10) 0.050(4) 0.029(5) 0.001(4) -0.024(6) C8 0.078(5) 0.095(7) 0.056(4) -0.011(4) -0.015(3) 0.000(4) C9 0.048(4) 0.099(7) 0.084(5) -0.002(4) 0.018(4) 0.011(3) C10 0.110(7) 0.078(7) 0.089(6) -0.015(5) -0.032(5) 0.021(5) 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' Si Si 0.0817 0.0704 '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' loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle N2 Ge1 N1 81.5(2) N2 Ge1 Si1 40.68(15) N1 Ge1 Si1 40.83(15) N2 Si1 N1 88.8(2) N2 Si1 C10 114.7(4) N1 Si1 C10 114.4(4) N2 Si1 C9 114.7(3) N1 Si1 C9 114.6(4) C10 Si1 C9 108.8(5) N2 Si1 Ge1 44.31(15) N1 Si1 Ge1 44.47(16) C10 Si1 Ge1 125.0(4) C9 Si1 Ge1 126.3(3) C1 N1 Si1 134.7(4) C1 N1 Ge1 130.5(4) Si1 N1 Ge1 94.7(2) C5 N2 Si1 135.5(4) C5 N2 Ge1 129.5(4) Si1 N2 Ge1 95.0(2) N1 C1 C3 110.1(6) N1 C1 C4 110.5(5) C3 C1 C4 109.9(8) N1 C1 C2 110.0(6) C3 C1 C2 109.3(8) C4 C1 C2 107.0(8) N2 C5 C6 109.4(5) N2 C5 C7 109.8(6) C6 C5 C7 110.3(7) N2 C5 C8 109.7(5) C6 C5 C8 108.0(6) C7 C5 C8 109.6(7) loop_ _geom_bond_atom_site_label_1 _geom_bond_atom_site_label_2 _geom_bond_distance Ge1 N2 1.848(4) Ge1 N1 1.852(5) Ge1 Si1 2.6350(17) Si1 N2 1.724(5) Si1 N1 1.729(5) Si1 C10 1.825(10) Si1 C9 1.870(8) N1 C1 1.456(7) N2 C5 1.463(7) C1 C3 1.497(11) C1 C4 1.517(10) C1 C2 1.520(12) C5 C6 1.501(9) C5 C7 1.526(10) C5 C8 1.530(11)