# Supplementary Material (ESI) for Dalton Transactions # This journal is (c) The Royal Society of Chemistry 2010 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Kost, Daniel' _publ_contact_author_email kostd@bgu.ac.il _publ_section_title ; Facile Central-Element Exchange in Neutral Hexacoordinate Germanium and Silicon Complexes; Synthesis and Characterization of Germanium Complexes ; loop_ _publ_author_name S.Yakubovich I.Kalikhman D.Kost # Attachment '- 1_sh.cif' data_1 _database_code_depnum_ccdc_archive 'CCDC 780239' #TrackingRef '- 1_sh.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(N-(dimethylamino)trifluoroacetimidato-N,O)chloro(methyl)germanium ; _chemical_name_common ;Bis(N-(dimethylamino)trifluoroacetimidato- N,O)chloro(methyl)germanium ; _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C9 H15 Cl F6 Ge N4 O2' _chemical_formula_weight 433.29 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' F F 0.0171 0.0103 '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 Monoclinic _symmetry_space_group_name_H-M P2(1)/n loop_ _symmetry_equiv_pos_as_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' _cell_length_a 6.9842(12) _cell_length_b 15.299(3) _cell_length_c 16.230(3) _cell_angle_alpha 90.00 _cell_angle_beta 93.397(3) _cell_angle_gamma 90.00 _cell_volume 1731.2(5) _cell_formula_units_Z 4 _cell_measurement_temperature 203(2) _cell_measurement_reflns_used 3530 _cell_measurement_theta_min 2.51 _cell_measurement_theta_max 26.03 _exptl_crystal_description cube _exptl_crystal_colour colorlles _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas 1.662 _exptl_crystal_density_diffrn 1.662 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 864 _exptl_absorpt_coefficient_mu 1.992 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min 0.02 _exptl_absorpt_correction_T_max 1.09 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 203(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 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 8215 _diffrn_reflns_av_R_equivalents 0.0301 _diffrn_reflns_av_sigmaI/netI 0.0371 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -18 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 11 _diffrn_reflns_theta_min 1.83 _diffrn_reflns_theta_max 25.03 _reflns_number_total 3046 _reflns_number_gt 2460 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^)+(0.0572P)^2^+0.8453P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef 0.006 _refine_ls_number_reflns 3046 _refine_ls_number_parameters 269 _refine_ls_number_restraints 132 _refine_ls_R_factor_all 0.0482 _refine_ls_R_factor_gt 0.0359 _refine_ls_wR_factor_ref 0.1004 _refine_ls_wR_factor_gt 0.0893 _refine_ls_goodness_of_fit_ref 1.054 _refine_ls_restrained_S_all 1.056 _refine_ls_shift/su_max 0.087 _refine_ls_shift/su_mean 0.010 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 0.93478(4) 0.83051(2) 0.881293(19) 0.02799(14) Uani 1 1 d . . . Cl2 Cl 0.70245(12) 0.91859(6) 0.93061(5) 0.0423(2) Uani 1 1 d . . . O1 O 1.0939(3) 0.74081(15) 0.83055(13) 0.0360(5) Uani 1 1 d . . . O2 O 0.7806(3) 0.73090(15) 0.91279(14) 0.0388(6) Uani 1 1 d . . . N1 N 0.7812(4) 0.81374(19) 0.76384(17) 0.0377(7) Uani 1 1 d . . . C1 C 1.1096(5) 0.9274(2) 0.8572(2) 0.0387(8) Uani 1 1 d . . . H1A H 1.1705 0.9492 0.9084 0.058 Uiso 1 1 calc R . . H1B H 1.0373 0.9741 0.8295 0.058 Uiso 1 1 calc R . . H1C H 1.2071 0.9064 0.8218 0.058 Uiso 1 1 calc R . . N3 N 1.0770(4) 0.79528(19) 0.99701(16) 0.0332(6) Uani 1 1 d . . . C2 C 0.8549(5) 0.6899(2) 0.9777(2) 0.0364(8) Uani 1 1 d . B . N4 N 0.9985(4) 0.7127(2) 1.02568(17) 0.0405(7) Uani 1 1 d . . . N2 N 0.8510(4) 0.7335(2) 0.72618(17) 0.0410(7) Uani 1 1 d . . . C3 C 1.0057(5) 0.7066(2) 0.7662(2) 0.0354(8) Uani 1 1 d . A . C4 C 1.0470(6) 0.8610(3) 1.0635(2) 0.0494(10) Uani 1 1 d . . . H4A H 0.9107 0.8682 1.0700 0.074 Uiso 1 1 calc R . . H4B H 1.1020 0.9166 1.0486 0.074 Uiso 1 1 calc R . . H4C H 1.1089 0.8408 1.1151 0.074 Uiso 1 1 calc R . . C5 C 1.2883(5) 0.7810(3) 0.9917(2) 0.0512(10) Uani 1 1 d . . . H5A H 1.3419 0.7579 1.0437 0.077 Uiso 1 1 calc R . . H5B H 1.3498 0.8361 0.9801 0.077 Uiso 1 1 calc R . . H5C H 1.3099 0.7397 0.9478 0.077 Uiso 1 1 calc R . . C6 C 0.5685(5) 0.8029(3) 0.7669(3) 0.0575(11) Uani 1 1 d . . . H6A H 0.5128 0.7914 0.7118 0.086 Uiso 1 1 calc R . . H6B H 0.5134 0.8560 0.7881 0.086 Uiso 1 1 calc R . . H6C H 0.5414 0.7543 0.8028 0.086 Uiso 1 1 calc R . . C9 C 0.8182(7) 0.8865(3) 0.7053(2) 0.0566(11) Uani 1 1 d . . . H9A H 0.9550 0.8916 0.6991 0.085 Uiso 1 1 calc R . . H9B H 0.7700 0.9409 0.7268 0.085 Uiso 1 1 calc R . . H9C H 0.7535 0.8743 0.6520 0.085 Uiso 1 1 calc R . . C7 C 1.0949(5) 0.6226(2) 0.7347(2) 0.0496(10) Uani 1 1 d D . . F1A F 1.052(2) 0.6073(13) 0.6555(5) 0.081(4) Uani 0.59(4) 1 d PDU A 1 F2A F 1.2832(8) 0.6240(10) 0.7412(10) 0.071(3) Uani 0.59(4) 1 d PDU A 1 F3A F 1.048(3) 0.5565(10) 0.7810(12) 0.095(4) Uani 0.59(4) 1 d PDU A 1 F1B F 1.101(6) 0.5604(16) 0.7905(17) 0.119(8) Uani 0.41(4) 1 d PDU A 2 F2B F 0.988(5) 0.5822(16) 0.678(2) 0.109(7) Uani 0.41(4) 1 d PDU A 2 F3B F 1.271(2) 0.6368(19) 0.716(2) 0.105(7) Uani 0.41(4) 1 d PDU A 2 C8 C 0.7538(5) 0.6047(3) 0.9974(2) 0.0560(10) Uani 1 1 d DU . . F4A F 0.5757(7) 0.6180(5) 1.0166(7) 0.099(2) Uani 0.817(17) 1 d PDU B 1 F5A F 0.7540(13) 0.5512(4) 0.9335(4) 0.100(2) Uani 0.817(17) 1 d PDU B 1 F6A F 0.8405(11) 0.5615(4) 1.0598(5) 0.101(2) Uani 0.817(17) 1 d PDU B 1 F4B F 0.573(2) 0.607(2) 0.970(2) 0.088(7) Uani 0.183(17) 1 d PDU B 2 F5B F 0.742(6) 0.594(2) 1.0774(6) 0.113(7) Uani 0.183(17) 1 d PDU B 2 F6B F 0.804(5) 0.5310(10) 0.9642(19) 0.099(6) Uani 0.183(17) 1 d PDU B 2 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 0.0242(2) 0.0321(2) 0.0278(2) -0.00104(14) 0.00256(13) -0.00092(13) Cl2 0.0326(4) 0.0473(5) 0.0476(5) -0.0070(4) 0.0079(4) 0.0044(4) O1 0.0303(12) 0.0436(14) 0.0334(12) -0.0112(11) -0.0029(9) 0.0058(10) O2 0.0334(13) 0.0382(14) 0.0441(14) 0.0052(11) -0.0031(10) -0.0082(10) N1 0.0335(16) 0.0452(18) 0.0337(16) -0.0034(13) -0.0042(12) 0.0064(13) C1 0.0358(19) 0.0345(19) 0.046(2) 0.0013(16) 0.0076(15) -0.0076(15) N3 0.0320(15) 0.0359(15) 0.0314(15) -0.0012(12) -0.0011(12) -0.0018(12) C2 0.0383(19) 0.0287(18) 0.043(2) 0.0036(15) 0.0088(16) 0.0036(14) N4 0.0446(18) 0.0407(17) 0.0356(16) 0.0076(13) -0.0011(13) 0.0021(14) N2 0.0424(18) 0.0462(18) 0.0337(15) -0.0101(13) -0.0030(13) 0.0034(14) C3 0.0361(19) 0.0363(19) 0.0342(18) -0.0033(15) 0.0067(15) -0.0007(15) C4 0.065(3) 0.047(2) 0.036(2) -0.0102(17) -0.0041(18) 0.0025(19) C5 0.0314(19) 0.079(3) 0.042(2) 0.006(2) -0.0066(15) 0.0016(19) C6 0.031(2) 0.091(3) 0.048(2) -0.016(2) -0.0122(17) 0.005(2) C9 0.073(3) 0.050(3) 0.046(2) 0.0097(19) -0.004(2) 0.009(2) C7 0.044(2) 0.044(2) 0.061(3) -0.015(2) 0.000(2) 0.0021(19) F1A 0.098(7) 0.091(8) 0.050(4) -0.044(4) -0.020(3) 0.034(4) F2A 0.047(4) 0.059(5) 0.105(6) -0.036(4) -0.004(5) 0.008(3) F3A 0.106(7) 0.041(5) 0.144(10) 0.013(5) 0.052(6) -0.006(6) F1B 0.17(2) 0.069(12) 0.117(11) 0.018(9) 0.045(12) 0.068(12) F2B 0.098(12) 0.065(9) 0.158(13) -0.068(10) -0.048(11) 0.018(7) F3B 0.087(10) 0.084(9) 0.155(16) -0.032(10) 0.091(10) 0.000(8) C8 0.051(2) 0.044(2) 0.073(3) 0.0150(18) 0.008(2) -0.0022(18) F4A 0.060(2) 0.069(3) 0.173(6) 0.041(4) 0.051(3) 0.001(2) F5A 0.153(6) 0.039(3) 0.111(3) -0.010(3) 0.022(3) -0.033(3) F6A 0.099(4) 0.075(3) 0.126(4) 0.062(3) -0.024(3) -0.020(3) F4B 0.042(6) 0.053(10) 0.168(16) 0.041(14) 0.005(9) -0.023(6) F5B 0.128(17) 0.128(16) 0.088(6) 0.045(9) 0.038(9) -0.038(14) F6B 0.124(13) 0.022(7) 0.155(14) 0.035(8) 0.053(14) 0.022(8) _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 O2 1.952(2) . ? Ge1 C1 1.974(3) . ? Ge1 O1 1.976(2) . ? Ge1 N3 2.141(3) . ? Ge1 N1 2.147(3) . ? Ge1 Cl2 2.2899(9) . ? O1 C3 1.292(4) . ? O2 C2 1.306(4) . ? N1 N2 1.468(4) . ? N1 C9 1.496(5) . ? N1 C6 1.499(5) . ? C1 H1A 0.9700 . ? C1 H1B 0.9700 . ? C1 H1C 0.9700 . ? N3 N4 1.464(4) . ? N3 C5 1.499(4) . ? N3 C4 1.500(4) . ? C2 N4 1.281(5) . ? C2 C8 1.526(5) . ? N2 C3 1.293(4) . ? C3 C7 1.530(5) . ? C4 H4A 0.9700 . ? C4 H4B 0.9700 . ? C4 H4C 0.9700 . ? C5 H5A 0.9700 . ? C5 H5B 0.9700 . ? C5 H5C 0.9700 . ? C6 H6A 0.9700 . ? C6 H6B 0.9700 . ? C6 H6C 0.9700 . ? C9 H9A 0.9700 . ? C9 H9B 0.9700 . ? C9 H9C 0.9700 . ? C7 F3B 1.303(7) . ? C7 F2B 1.305(7) . ? C7 F1B 1.311(7) . ? C7 F3A 1.312(6) . ? C7 F2A 1.313(6) . ? C7 F1A 1.324(6) . ? C8 F6B 1.307(8) . ? C8 F5B 1.316(8) . ? C8 F4A 1.316(5) . ? C8 F4B 1.318(8) . ? C8 F5A 1.322(5) . ? C8 F6A 1.324(5) . ? 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 Ge1 C1 174.59(13) . . ? O2 Ge1 O1 84.24(10) . . ? C1 Ge1 O1 93.94(13) . . ? O2 Ge1 N3 78.95(10) . . ? C1 Ge1 N3 95.89(13) . . ? O1 Ge1 N3 86.99(10) . . ? O2 Ge1 N1 83.38(11) . . ? C1 Ge1 N1 101.31(13) . . ? O1 Ge1 N1 79.10(10) . . ? N3 Ge1 N1 158.50(12) . . ? O2 Ge1 Cl2 87.39(8) . . ? C1 Ge1 Cl2 95.00(11) . . ? O1 Ge1 Cl2 169.12(7) . . ? N3 Ge1 Cl2 98.23(8) . . ? N1 Ge1 Cl2 93.07(8) . . ? C3 O1 Ge1 111.4(2) . . ? C2 O2 Ge1 112.8(2) . . ? N2 N1 C9 106.5(3) . . ? N2 N1 C6 106.0(3) . . ? C9 N1 C6 108.2(3) . . ? N2 N1 Ge1 107.98(18) . . ? C9 N1 Ge1 112.3(2) . . ? C6 N1 Ge1 115.3(2) . . ? Ge1 C1 H1A 109.5 . . ? Ge1 C1 H1B 109.5 . . ? H1A C1 H1B 109.5 . . ? Ge1 C1 H1C 109.5 . . ? H1A C1 H1C 109.5 . . ? H1B C1 H1C 109.5 . . ? N4 N3 C5 106.3(3) . . ? N4 N3 C4 106.2(3) . . ? C5 N3 C4 108.6(3) . . ? N4 N3 Ge1 109.44(19) . . ? C5 N3 Ge1 113.2(2) . . ? C4 N3 Ge1 112.7(2) . . ? N4 C2 O2 128.2(3) . . ? N4 C2 C8 117.4(3) . . ? O2 C2 C8 114.4(3) . . ? C2 N4 N3 109.6(3) . . ? C3 N2 N1 110.2(3) . . ? O1 C3 N2 128.4(3) . . ? O1 C3 C7 115.2(3) . . ? N2 C3 C7 116.4(3) . . ? N3 C4 H4A 109.5 . . ? N3 C4 H4B 109.5 . . ? H4A C4 H4B 109.5 . . ? N3 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 . . ? N1 C6 H6A 109.5 . . ? N1 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N1 C6 H6C 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? N1 C9 H9A 109.5 . . ? N1 C9 H9B 109.5 . . ? H9A C9 H9B 109.5 . . ? N1 C9 H9C 109.5 . . ? H9A C9 H9C 109.5 . . ? H9B C9 H9C 109.5 . . ? F3B C7 F2B 114.9(16) . . ? F3B C7 F1B 106.7(17) . . ? F2B C7 F1B 98.0(17) . . ? F3B C7 F3A 122.2(17) . . ? F2B C7 F3A 83.6(18) . . ? F1B C7 F3A 18(2) . . ? F3B C7 F2A 20.0(18) . . ? F2B C7 F2A 126.2(16) . . ? F1B C7 F2A 88.0(17) . . ? F3A C7 F2A 104.5(10) . . ? F3B C7 F1A 88.2(12) . . ? F2B C7 F1A 31.0(14) . . ? F1B C7 F1A 122.6(16) . . ? F3A C7 F1A 111.7(13) . . ? F2A C7 F1A 104.5(8) . . ? F3B C7 C3 110.3(11) . . ? F2B C7 C3 114.0(11) . . ? F1B C7 C3 112.2(15) . . ? F3A C7 C3 109.6(11) . . ? F2A C7 C3 112.7(7) . . ? F1A C7 C3 113.4(7) . . ? F6B C8 F5B 109.3(17) . . ? F6B C8 F4A 120.7(16) . . ? F5B C8 F4A 70.8(17) . . ? F6B C8 F4B 98.9(19) . . ? F5B C8 F4B 103.0(16) . . ? F4A C8 F4B 34.4(16) . . ? F6B C8 F5A 29.4(13) . . ? F5B C8 F5A 134.2(15) . . ? F4A C8 F5A 109.1(5) . . ? F4B C8 F5A 78.0(17) . . ? F6B C8 F6A 76.3(13) . . ? F5B C8 F6A 40.1(18) . . ? F4A C8 F6A 107.0(5) . . ? F4B C8 F6A 131.2(13) . . ? F5A C8 F6A 105.6(4) . . ? F6B C8 C2 120.8(14) . . ? F5B C8 C2 112.0(12) . . ? F4A C8 C2 111.9(4) . . ? F4B C8 C2 110.8(12) . . ? F5A C8 C2 110.0(4) . . ? F6A C8 C2 113.0(4) . . ? 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 Ge1 O1 C3 70.3(2) . . . . ? C1 Ge1 O1 C3 -114.8(2) . . . . ? N3 Ge1 O1 C3 149.5(2) . . . . ? N1 Ge1 O1 C3 -14.0(2) . . . . ? Cl2 Ge1 O1 C3 30.4(5) . . . . ? C1 Ge1 O2 C2 9.1(14) . . . . ? O1 Ge1 O2 C2 79.6(2) . . . . ? N3 Ge1 O2 C2 -8.4(2) . . . . ? N1 Ge1 O2 C2 159.3(2) . . . . ? Cl2 Ge1 O2 C2 -107.3(2) . . . . ? O2 Ge1 N1 N2 -71.1(2) . . . . ? C1 Ge1 N1 N2 106.2(2) . . . . ? O1 Ge1 N1 N2 14.3(2) . . . . ? N3 Ge1 N1 N2 -36.3(4) . . . . ? Cl2 Ge1 N1 N2 -158.1(2) . . . . ? O2 Ge1 N1 C9 171.8(3) . . . . ? C1 Ge1 N1 C9 -10.9(3) . . . . ? O1 Ge1 N1 C9 -102.8(3) . . . . ? N3 Ge1 N1 C9 -153.4(3) . . . . ? Cl2 Ge1 N1 C9 84.8(2) . . . . ? O2 Ge1 N1 C6 47.3(3) . . . . ? C1 Ge1 N1 C6 -135.5(3) . . . . ? O1 Ge1 N1 C6 132.6(3) . . . . ? N3 Ge1 N1 C6 82.0(4) . . . . ? Cl2 Ge1 N1 C6 -39.8(3) . . . . ? O2 Ge1 N3 N4 8.13(19) . . . . ? C1 Ge1 N3 N4 -170.2(2) . . . . ? O1 Ge1 N3 N4 -76.6(2) . . . . ? N1 Ge1 N3 N4 -27.1(4) . . . . ? Cl2 Ge1 N3 N4 93.83(19) . . . . ? O2 Ge1 N3 C5 126.5(3) . . . . ? C1 Ge1 N3 C5 -51.8(3) . . . . ? O1 Ge1 N3 C5 41.8(3) . . . . ? N1 Ge1 N3 C5 91.2(4) . . . . ? Cl2 Ge1 N3 C5 -147.8(2) . . . . ? O2 Ge1 N3 C4 -109.8(2) . . . . ? C1 Ge1 N3 C4 71.9(3) . . . . ? O1 Ge1 N3 C4 165.5(2) . . . . ? N1 Ge1 N3 C4 -145.0(3) . . . . ? Cl2 Ge1 N3 C4 -24.1(2) . . . . ? Ge1 O2 C2 N4 8.3(5) . . . . ? Ge1 O2 C2 C8 -172.1(2) . . . . ? O2 C2 N4 N3 -0.7(5) . . . . ? C8 C2 N4 N3 179.7(3) . . . . ? C5 N3 N4 C2 -128.9(3) . . . . ? C4 N3 N4 C2 115.5(3) . . . . ? Ge1 N3 N4 C2 -6.4(3) . . . . ? C9 N1 N2 C3 108.6(3) . . . . ? C6 N1 N2 C3 -136.4(3) . . . . ? Ge1 N1 N2 C3 -12.2(3) . . . . ? Ge1 O1 C3 N2 12.6(5) . . . . ? Ge1 O1 C3 C7 -166.1(2) . . . . ? N1 N2 C3 O1 0.6(5) . . . . ? N1 N2 C3 C7 179.3(3) . . . . ? O1 C3 C7 F3B -59(2) . . . . ? N2 C3 C7 F3B 122(2) . . . . ? O1 C3 C7 F2B 170(2) . . . . ? N2 C3 C7 F2B -9(2) . . . . ? O1 C3 C7 F1B 60(2) . . . . ? N2 C3 C7 F1B -119(2) . . . . ? O1 C3 C7 F3A 78.5(10) . . . . ? N2 C3 C7 F3A -100.4(10) . . . . ? O1 C3 C7 F2A -37.5(9) . . . . ? N2 C3 C7 F2A 143.6(9) . . . . ? O1 C3 C7 F1A -155.9(11) . . . . ? N2 C3 C7 F1A 25.2(12) . . . . ? N4 C2 C8 F6B -92.4(19) . . . . ? O2 C2 C8 F6B 88.0(19) . . . . ? N4 C2 C8 F5B 39(2) . . . . ? O2 C2 C8 F5B -141(2) . . . . ? N4 C2 C8 F4A 115.8(6) . . . . ? O2 C2 C8 F4A -63.7(7) . . . . ? N4 C2 C8 F4B 153(2) . . . . ? O2 C2 C8 F4B -27(2) . . . . ? N4 C2 C8 F5A -122.8(6) . . . . ? O2 C2 C8 F5A 57.6(6) . . . . ? N4 C2 C8 F6A -5.0(7) . . . . ? O2 C2 C8 F6A 175.4(6) . . . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 25.03 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.833 _refine_diff_density_min -0.382 _refine_diff_density_rms 0.088 # Attachment '- 2_sh203.cif' data_2 _database_code_depnum_ccdc_archive 'CCDC 780240' #TrackingRef '- 2_sh203.cif' _audit_creation_method SHELXL-97 _chemical_name_systematic ; Bis(N-(dimethylamino)trifluoroacetimidato-N,O)dichlorogermanium ; _chemical_name_common ;Bis(N-(dimethylamino)trifluoroacetimidato- N,O)dichlorogermanium ; _chemical_melting_point ? _chemical_formula_moiety 'C8 H12 Cl2 F6 Ge N4 O2' _chemical_formula_sum 'C8 H12 Cl2 F6 Ge N4 O2' _chemical_formula_weight 453.71 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' F F 0.0171 0.0103 '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 Monoclinic _symmetry_space_group_name_H-M 'P2(1)/n ' loop_ _symmetry_equiv_pos_as_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' _cell_length_a 7.045(5) _cell_length_b 15.094(5) _cell_length_c 16.053(5) _cell_angle_alpha 90.000(5) _cell_angle_beta 92.376(5) _cell_angle_gamma 90.000(5) _cell_volume 1705.6(14) _cell_formula_units_Z 4 _cell_measurement_temperature 200(2) _cell_measurement_reflns_used 4879 _cell_measurement_theta_min 2.54 _cell_measurement_theta_max 25.66 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_size_min 0.02 _exptl_crystal_size_mid 0.10 _exptl_crystal_size_max 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.767 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 896 _exptl_absorpt_coefficient_mu 2.178 _exptl_absorpt_correction_type none _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 200(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'CCD area detector' _diffrn_measurement_method 'phi and omega scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number ? _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 15632 _diffrn_reflns_av_R_equivalents 0.0614 _diffrn_reflns_av_sigmaI/netI 0.0471 _diffrn_reflns_limit_h_min -7 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 17 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 18 _diffrn_reflns_theta_min 3.19 _diffrn_reflns_theta_max 25.00 _reflns_number_total 2984 _reflns_number_gt 2239 _reflns_threshold_expression >2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SMART' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 2008)' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL' _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^ > 2\s(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^)+(0.0532P)^2^+3.1902P] 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 none _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 2984 _refine_ls_number_parameters 208 _refine_ls_number_restraints 28 _refine_ls_R_factor_all 0.0703 _refine_ls_R_factor_gt 0.0466 _refine_ls_wR_factor_ref 0.1193 _refine_ls_wR_factor_gt 0.1070 _refine_ls_goodness_of_fit_ref 1.039 _refine_ls_restrained_S_all 1.438 _refine_ls_shift/su_max 0.005 _refine_ls_shift/su_mean 0.001 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 C1 C 0.7631(12) 0.3920(6) -0.0169(6) 0.061(2) Uani 1 1 d DU . . C2 C 0.6643(10) 0.3121(5) 0.0147(4) 0.0377(16) Uani 1 1 d . . . C3 C 0.4151(10) 0.3746(5) 0.2743(5) 0.0467(19) Uani 1 1 d . . . C4 C 0.5098(9) 0.2944(5) 0.2391(4) 0.0360(16) Uani 1 1 d . . . C5 C 0.4553(11) 0.1322(5) -0.0564(4) 0.0482(19) Uani 1 1 d . . . H5A H 0.5865 0.1179 -0.0636 0.072 Uiso 1 1 calc R . . H5B H 0.3983 0.1514 -0.1087 0.072 Uiso 1 1 calc R . . H5C H 0.3899 0.0807 -0.0374 0.072 Uiso 1 1 calc R . . C6 C 0.2343(9) 0.2248(6) 0.0145(5) 0.053(2) Uani 1 1 d . . . H6A H 0.2203 0.2713 0.0546 0.079 Uiso 1 1 calc R . . H6B H 0.1697 0.1727 0.0325 0.079 Uiso 1 1 calc R . . H6C H 0.1803 0.2435 -0.0386 0.079 Uiso 1 1 calc R . . C7 C 0.9460(9) 0.2058(6) 0.2299(5) 0.055(2) Uani 1 1 d . . . H7A H 0.9645 0.2559 0.1943 0.082 Uiso 1 1 calc R . . H7B H 1.0070 0.1548 0.2073 0.082 Uiso 1 1 calc R . . H7C H 1.0001 0.2181 0.2845 0.082 Uiso 1 1 calc R . . C8 C 0.7114(12) 0.1092(5) 0.2907(5) 0.0509(19) Uani 1 1 d . . . H8A H 0.5786 0.0967 0.2947 0.076 Uiso 1 1 calc R . . H8B H 0.7662 0.1216 0.3452 0.076 Uiso 1 1 calc R . . H8C H 0.7738 0.0588 0.2676 0.076 Uiso 1 1 calc R . . N1 N 0.5215(8) 0.2838(4) -0.0304(4) 0.0399(14) Uani 1 1 d . . . N2 N 0.4419(7) 0.2046(4) 0.0064(3) 0.0327(13) Uani 1 1 d . . . N3 N 0.6579(8) 0.2642(4) 0.2796(3) 0.0409(14) Uani 1 1 d . . . N4 N 0.7360(7) 0.1879(4) 0.2354(3) 0.0352(13) Uani 1 1 d . . . O1 O 0.7377(6) 0.2773(3) 0.0831(3) 0.0382(11) Uani 1 1 d . . . O2 O 0.4305(6) 0.2643(3) 0.1701(3) 0.0380(11) Uani 1 1 d . . . F1 F 0.6876(11) 0.4296(5) -0.0816(5) 0.141(3) Uani 1 1 d DU . . F3 F 0.9418(8) 0.3864(4) -0.0188(5) 0.121(3) Uani 1 1 d DU . . F2 F 0.7418(11) 0.4610(4) 0.0448(5) 0.127(3) Uani 1 1 d DU . . F4 F 0.2292(7) 0.3662(4) 0.2751(4) 0.0889(19) Uani 1 1 d . . . F5 F 0.4430(10) 0.4452(4) 0.2271(5) 0.103(2) Uani 1 1 d . . . F6 F 0.4753(9) 0.3957(5) 0.3496(4) 0.114(3) Uani 1 1 d . . . Cl1 Cl 0.3864(2) 0.07119(12) 0.15088(11) 0.0427(5) Uani 1 1 d . . . Cl2 Cl 0.8037(2) 0.08473(12) 0.07083(10) 0.0409(5) Uani 1 1 d . . . Ge1 Ge 0.58913(9) 0.17757(4) 0.11885(4) 0.0279(2) Uani 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 C1 0.051(5) 0.052(5) 0.080(6) 0.022(4) -0.001(4) -0.010(4) C2 0.040(4) 0.040(4) 0.033(4) 0.004(3) 0.008(3) 0.000(3) C3 0.042(4) 0.046(5) 0.052(5) -0.014(4) 0.001(4) -0.003(4) C4 0.033(4) 0.042(4) 0.033(4) -0.002(3) 0.008(3) -0.005(3) C5 0.064(5) 0.051(5) 0.029(4) -0.009(3) -0.008(3) -0.003(4) C6 0.028(4) 0.086(6) 0.043(4) -0.001(4) -0.007(3) 0.001(4) C7 0.031(4) 0.092(7) 0.040(4) -0.009(4) -0.008(3) -0.004(4) C8 0.063(5) 0.052(5) 0.037(4) 0.007(4) -0.008(3) 0.006(4) N1 0.041(3) 0.044(4) 0.035(3) 0.005(3) 0.001(3) -0.003(3) N2 0.032(3) 0.041(3) 0.026(3) -0.004(2) 0.002(2) -0.007(2) N3 0.042(3) 0.049(4) 0.031(3) -0.006(3) 0.002(3) 0.003(3) N4 0.033(3) 0.046(3) 0.027(3) -0.003(3) 0.000(2) 0.005(3) O1 0.036(3) 0.043(3) 0.035(3) 0.007(2) -0.006(2) -0.010(2) O2 0.038(3) 0.046(3) 0.030(3) -0.012(2) -0.002(2) 0.005(2) F1 0.148(6) 0.124(6) 0.146(6) 0.100(5) -0.059(5) -0.069(5) F3 0.054(3) 0.087(4) 0.225(8) 0.065(5) 0.049(4) -0.006(3) F2 0.160(7) 0.063(4) 0.161(6) -0.014(4) 0.056(5) -0.040(4) F4 0.049(3) 0.085(4) 0.134(5) -0.056(4) 0.027(3) -0.005(3) F5 0.122(5) 0.055(4) 0.137(6) 0.005(4) 0.051(4) 0.013(3) F6 0.126(5) 0.125(6) 0.089(4) -0.073(4) -0.037(4) 0.059(4) Cl1 0.0381(9) 0.0499(11) 0.0406(10) 0.0051(8) 0.0092(7) -0.0112(8) Cl2 0.0333(9) 0.0501(11) 0.0399(10) -0.0098(8) 0.0062(7) 0.0035(8) Ge1 0.0251(4) 0.0368(4) 0.0222(4) -0.0010(3) 0.0030(2) -0.0021(3) _geom_special_details ; All s.u.'s (except the s.u. in the dihedral angle between two l.s. planes) are estimated using the full covariance matrix. The cell s.u.'s are taken into account individually in the estimation of s.u.'s in distances, angles and torsion angles; correlations between s.u.'s in cell parameters are only used when they are defined by crystal symmetry. An approximate (isotropic) treatment of cell s.u.'s is used for estimating s.u.'s 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 C1 F3 1.264(9) . ? C1 F1 1.279(10) . ? C1 F2 1.449(10) . ? C1 C2 1.493(10) . ? C2 N1 1.288(9) . ? C2 O1 1.304(8) . ? C3 F6 1.304(9) . ? C3 F4 1.316(8) . ? C3 F5 1.326(10) . ? C3 C4 1.505(10) . ? C4 N3 1.289(9) . ? C4 O2 1.302(8) . ? C5 N2 1.492(9) . ? C5 H5A 0.9600 . ? C5 H5B 0.9600 . ? C5 H5C 0.9600 . ? C6 N2 1.506(8) . ? C6 H6A 0.9600 . ? C6 H6B 0.9600 . ? C6 H6C 0.9600 . ? C7 N4 1.510(8) . ? C7 H7A 0.9600 . ? C7 H7B 0.9600 . ? C7 H7C 0.9600 . ? C8 N4 1.497(9) . ? C8 H8A 0.9600 . ? C8 H8B 0.9600 . ? C8 H8C 0.9600 . ? N1 N2 1.456(7) . ? N2 Ge1 2.085(5) . ? N3 N4 1.472(8) . ? N4 Ge1 2.106(5) . ? O1 Ge1 1.934(4) . ? O2 Ge1 1.928(4) . ? Cl1 Ge1 2.2234(19) . ? Cl2 Ge1 2.2226(19) . ? 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 F3 C1 F1 113.1(8) . . ? F3 C1 F2 101.3(8) . . ? F1 C1 F2 100.6(8) . . ? F3 C1 C2 115.6(7) . . ? F1 C1 C2 116.8(7) . . ? F2 C1 C2 106.6(7) . . ? N1 C2 O1 127.8(6) . . ? N1 C2 C1 116.2(6) . . ? O1 C2 C1 116.0(6) . . ? F6 C3 F4 107.5(7) . . ? F6 C3 F5 106.5(7) . . ? F4 C3 F5 104.7(7) . . ? F6 C3 C4 114.3(7) . . ? F4 C3 C4 112.5(6) . . ? F5 C3 C4 110.7(6) . . ? N3 C4 O2 128.0(6) . . ? N3 C4 C3 117.2(6) . . ? O2 C4 C3 114.8(6) . . ? N2 C5 H5A 109.5 . . ? N2 C5 H5B 109.5 . . ? H5A C5 H5B 109.5 . . ? N2 C5 H5C 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? N2 C6 H6A 109.5 . . ? N2 C6 H6B 109.5 . . ? H6A C6 H6B 109.5 . . ? N2 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 . . ? C2 N1 N2 110.5(5) . . ? N1 N2 C5 106.9(5) . . ? N1 N2 C6 105.1(5) . . ? C5 N2 C6 107.2(5) . . ? N1 N2 Ge1 109.0(4) . . ? C5 N2 Ge1 113.5(4) . . ? C6 N2 Ge1 114.5(4) . . ? C4 N3 N4 110.1(5) . . ? N3 N4 C8 106.3(5) . . ? N3 N4 C7 106.0(5) . . ? C8 N4 C7 108.3(6) . . ? N3 N4 Ge1 107.9(4) . . ? C8 N4 Ge1 113.8(4) . . ? C7 N4 Ge1 114.0(4) . . ? C2 O1 Ge1 111.3(4) . . ? C4 O2 Ge1 111.4(4) . . ? O2 Ge1 O1 85.9(2) . . ? O2 Ge1 N2 87.7(2) . . ? O1 Ge1 N2 81.17(19) . . ? O2 Ge1 N4 80.9(2) . . ? O1 Ge1 N4 87.4(2) . . ? N2 Ge1 N4 164.5(2) . . ? O2 Ge1 Cl2 172.26(14) . . ? O1 Ge1 Cl2 90.19(15) . . ? N2 Ge1 Cl2 98.29(15) . . ? N4 Ge1 Cl2 92.20(15) . . ? O2 Ge1 Cl1 90.14(15) . . ? O1 Ge1 Cl1 172.49(14) . . ? N2 Ge1 Cl1 92.31(15) . . ? N4 Ge1 Cl1 98.31(16) . . ? Cl2 Ge1 Cl1 94.45(8) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.694 _refine_diff_density_min -0.641 _refine_diff_density_rms 0.095