Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Herbert Roesky' _publ_contact_author_email HROESKY@GWDG.DE _publ_section_title ; Facile Synthesis of Dichlorosilane by Metathesis Reaction and Dehydrogenation of Dihydrogermane by a Frustrated Lewis Pair ; loop_ _publ_author_name 'Herbert Roesky' 'Anukul Jana' 'Carola Schulzke' 'Gaper Tavar' # Attachment 'JA2.CIF' data_ja2 _database_code_depnum_ccdc_archive 'CCDC 745452' #TrackingRef 'JA2.CIF' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C20 H24 Cl2 Ge N2' _chemical_formula_weight 435.90 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' Cl Cl 0.1484 0.1585 '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 orthorhombic _symmetry_space_group_name_H-M Pbcn loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y+1/2, z+1/2' '-x, y, -z+1/2' 'x+1/2, -y+1/2, -z' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' 'x, -y, z-1/2' '-x-1/2, y-1/2, z' _cell_length_a 17.174(3) _cell_length_b 7.3558(15) _cell_length_c 15.804(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 1996.5(7) _cell_formula_units_Z 4 _cell_measurement_temperature 140(2) _cell_measurement_reflns_used 19271 _cell_measurement_theta_min 4.7 _cell_measurement_theta_max 54.0 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.41 _exptl_crystal_size_mid 0.37 _exptl_crystal_size_min 0.21 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.450 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 1.807 _exptl_absorpt_correction_type numerical _exptl_absorpt_correction_T_min 0.4529 _exptl_absorpt_correction_T_max 0.7076 _exptl_absorpt_process_details 'face indexed' _exptl_special_details ; ? ; _diffrn_ambient_temperature 140(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 17399 _diffrn_reflns_av_R_equivalents 0.0980 _diffrn_reflns_av_sigmaI/netI 0.0495 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -9 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 2.37 _diffrn_reflns_theta_max 26.99 _reflns_number_total 2102 _reflns_number_gt 1574 _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^)+(0.0276P)^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 refall _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2102 _refine_ls_number_parameters 153 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0697 _refine_ls_R_factor_gt 0.0403 _refine_ls_wR_factor_ref 0.0702 _refine_ls_wR_factor_gt 0.0642 _refine_ls_goodness_of_fit_ref 1.101 _refine_ls_restrained_S_all 1.101 _refine_ls_shift/su_max 0.003 _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 Ge1 Ge 0.5000 0.19331(5) 0.7500 0.01726(11) Uani 1 2 d S . . Cl1 Cl 0.55932(4) 0.00526(11) 0.66875(5) 0.02747(17) Uani 1 1 d . . . N1 N 0.43832(13) 0.3638(3) 0.70300(15) 0.0195(5) Uani 1 1 d . . . C1 C 0.36440(14) 0.3440(4) 0.66162(17) 0.0179(6) Uani 1 1 d . . . C2 C 0.36230(15) 0.3039(4) 0.57482(17) 0.0198(5) Uani 1 1 d . . . C3 C 0.28991(17) 0.2875(4) 0.53569(18) 0.0222(6) Uani 1 1 d . . . H3 H 0.2881(17) 0.258(5) 0.4796(19) 0.019(6) Uiso 1 1 d . . . C4 C 0.22081(15) 0.3127(4) 0.58001(18) 0.0227(6) Uani 1 1 d . . . C5 C 0.22517(16) 0.3551(4) 0.66546(19) 0.0227(6) Uani 1 1 d . . . H5 H 0.1792(17) 0.375(5) 0.6954(19) 0.019(6) Uiso 1 1 d . . . C6 C 0.29605(17) 0.3713(4) 0.70806(19) 0.0214(6) Uani 1 1 d . . . C7 C 0.43549(18) 0.2833(5) 0.5237(2) 0.0281(7) Uani 1 1 d . . . H7A H 0.455(2) 0.169(6) 0.529(3) 0.048(4) Uiso 1 1 d . . . H7B H 0.473(2) 0.367(6) 0.544(2) 0.048(4) Uiso 1 1 d . . . H7C H 0.428(2) 0.302(6) 0.459(3) 0.048(4) Uiso 1 1 d . . . C8 C 0.14382(19) 0.2961(6) 0.5359(2) 0.0323(7) Uani 1 1 d . . . H8A H 0.104(2) 0.329(5) 0.567(2) 0.048(4) Uiso 1 1 d . . . H8B H 0.134(2) 0.175(6) 0.521(2) 0.048(4) Uiso 1 1 d . . . H8C H 0.140(2) 0.360(6) 0.483(3) 0.048(4) Uiso 1 1 d . . . C9 C 0.2980(2) 0.4206(6) 0.8007(2) 0.0310(8) Uani 1 1 d . . . H9A H 0.250(2) 0.431(5) 0.821(2) 0.048(4) Uiso 1 1 d . . . H9B H 0.324(2) 0.328(6) 0.831(3) 0.048(4) Uiso 1 1 d . . . H9C H 0.322(2) 0.535(6) 0.808(2) 0.048(4) Uiso 1 1 d . . . C10 C 0.46823(18) 0.5355(4) 0.72616(19) 0.0243(7) Uani 1 1 d . . . H10 H 0.554(2) 0.635(5) 0.793(2) 0.034(10) 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 Ge1 0.01513(17) 0.01483(18) 0.02181(18) 0.000 -0.00215(19) 0.000 Cl1 0.0288(3) 0.0232(3) 0.0304(3) -0.0037(3) 0.0029(3) 0.0062(3) N1 0.0172(11) 0.0156(12) 0.0256(12) 0.0008(10) -0.0067(9) 0.0007(9) C1 0.0152(13) 0.0160(15) 0.0226(13) 0.0016(11) -0.0043(10) 0.0004(10) C2 0.0189(13) 0.0164(13) 0.0240(13) 0.0024(13) 0.0004(10) -0.0021(11) C3 0.0284(15) 0.0189(16) 0.0192(14) 0.0009(13) -0.0056(11) -0.0003(12) C4 0.0213(13) 0.0166(13) 0.0302(15) 0.0067(14) -0.0075(11) -0.0007(12) C5 0.0163(13) 0.0206(16) 0.0312(15) 0.0041(13) 0.0004(12) 0.0035(11) C6 0.0202(15) 0.0186(14) 0.0255(15) 0.0022(13) -0.0028(12) 0.0023(12) C7 0.0269(17) 0.030(2) 0.0278(16) 0.0004(16) 0.0051(12) 0.0001(14) C8 0.0242(16) 0.032(2) 0.0406(19) 0.0066(17) -0.0125(14) -0.0001(15) C9 0.0307(19) 0.039(2) 0.0227(17) -0.0058(15) -0.0007(14) 0.0078(16) C10 0.0248(13) 0.0148(14) 0.0333(17) 0.0010(12) -0.0077(11) 0.0017(12) _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 Ge1 N1 1.802(2) 3_656 ? Ge1 N1 1.802(2) . ? Ge1 Cl1 2.1448(8) . ? Ge1 Cl1 2.1448(8) 3_656 ? N1 C10 1.412(4) . ? N1 C1 1.435(3) . ? C1 C6 1.399(4) . ? C1 C2 1.403(4) . ? C2 C3 1.394(4) . ? C2 C7 1.502(4) . ? C3 C4 1.390(4) . ? C4 C5 1.388(4) . ? C4 C8 1.500(4) . ? C5 C6 1.396(4) . ? C6 C9 1.508(4) . ? C10 C10 1.326(6) 3_656 ? 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 N1 Ge1 N1 91.79(15) 3_656 . ? N1 Ge1 Cl1 114.61(8) 3_656 . ? N1 Ge1 Cl1 118.77(8) . . ? N1 Ge1 Cl1 118.77(8) 3_656 3_656 ? N1 Ge1 Cl1 114.61(8) . 3_656 ? Cl1 Ge1 Cl1 99.68(5) . 3_656 ? C10 N1 C1 122.0(2) . . ? C10 N1 Ge1 107.57(18) . . ? C1 N1 Ge1 129.58(19) . . ? C6 C1 C2 121.4(2) . . ? C6 C1 N1 119.2(3) . . ? C2 C1 N1 119.3(2) . . ? C3 C2 C1 118.4(2) . . ? C3 C2 C7 119.9(3) . . ? C1 C2 C7 121.7(3) . . ? C4 C3 C2 121.8(3) . . ? C5 C4 C3 118.3(2) . . ? C5 C4 C8 121.2(3) . . ? C3 C4 C8 120.5(3) . . ? C4 C5 C6 122.4(3) . . ? C5 C6 C1 117.8(3) . . ? C5 C6 C9 120.5(3) . . ? C1 C6 C9 121.7(3) . . ? C10 C10 N1 116.53(15) 3_656 . ? _diffrn_measured_fraction_theta_max 0.965 _diffrn_reflns_theta_full 26.99 _diffrn_measured_fraction_theta_full 0.965 _refine_diff_density_max 0.373 _refine_diff_density_min -0.575 _refine_diff_density_rms 0.066