# Supplementary Material (ESI) for Dalton Transactions # This journal is © The Royal Society of Chemistry 1999 # CCDC Number: 186/1696 data_los10 _audit_creation_method SHELXL _chemical_name_systematic ; O-Trichlorsilyl-N,N-dimethylhydroxylamin ; _chemical_name_common ? _chemical_formula_moiety ? _chemical_formula_structural ? _chemical_formula_analytical ? _chemical_formula_sum 'C2 H6 Cl3 N O Si' _chemical_formula_weight 194.52 _chemical_melting_point ? _chemical_compound_source ? 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' 'Si' 'Si' 0.0817 0.0704 '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' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M P2(1)/c loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, y+1/2, -z+1/2' '-x, -y, -z' 'x, -y-1/2, z-1/2' _cell_length_a 11.585(1) _cell_length_b 7.487(1) _cell_length_c 19.069(2) _cell_angle_alpha 90.00 _cell_angle_beta 98.37(1) _cell_angle_gamma 90.00 _cell_volume 1636.4(3) _cell_formula_units_Z 8 _cell_measurement_temperature 149(2) _cell_measurement_reflns_used 96 _cell_measurement_theta_min 18 _cell_measurement_theta_max 23 _exptl_crystal_description Column _exptl_crystal_colour Colorless _exptl_crystal_size_max 1.4 _exptl_crystal_size_mid 0.3 _exptl_crystal_size_min 0.3 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.579 _exptl_crystal_density_method ? _exptl_crystal_F_000 784 _exptl_absorpt_coefficient_mu 1.184 _exptl_absorpt_correction_type None _exptl_absorpt_correction_T_min ? _exptl_absorpt_correction_T_max ? _exptl_special_details ; Crystal grown in situ from the melt ; _diffrn_ambient_temperature 149(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 ? _diffrn_measurement_method ? _diffrn_standards_number 3 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 60 _diffrn_standards_decay_% None _diffrn_reflns_number 3642 _diffrn_reflns_av_R_equivalents 0.0320 _diffrn_reflns_av_sigmaI/netI 0.0159 _diffrn_reflns_limit_h_min -14 _diffrn_reflns_limit_h_max 14 _diffrn_reflns_limit_k_min 0 _diffrn_reflns_limit_k_max 9 _diffrn_reflns_limit_l_min 0 _diffrn_reflns_limit_l_max 24 _diffrn_reflns_theta_min 3.25 _diffrn_reflns_theta_max 26.92 _reflns_number_total 3545 _reflns_number_observed 2944 _reflns_observed_criterion >2sigma(I) _computing_data_collection 'CAD4 5.0' _computing_cell_refinement 'CAD4 5.0' _computing_data_reduction 'CADSHEL' _computing_structure_solution 'SHELXS-86 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-93 (Sheldrick, 1993)' _computing_molecular_graphics 'SHELXTL 5.01' _computing_publication_material 'SHELXTL 5.01' _refine_special_details ; Refinement on F^2^ for ALL reflections except for 13 with very negative F^2^ or flagged by the user for potential systematic errors. Weighted R-factors wR and all goodnesses 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 observed criterion of F^2^ > 2sigma(F^2^) is used only for calculating _R_factor_obs 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 w=1/[\s^2^(Fo^2^)+(0.0576P)^2^+0.5440P] 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 SHELXL _refine_ls_extinction_coef 0.0016(5) _refine_ls_extinction_expression 'Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^' _refine_ls_number_reflns 3532 _refine_ls_number_parameters 184 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0478 _refine_ls_R_factor_obs 0.0355 _refine_ls_wR_factor_all 0.1029 _refine_ls_wR_factor_obs 0.0897 _refine_ls_goodness_of_fit_all 1.103 _refine_ls_goodness_of_fit_obs 1.128 _refine_ls_restrained_S_all 1.174 _refine_ls_restrained_S_obs 1.128 _refine_ls_shift/esd_max 0.001 _refine_ls_shift/esd_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_thermal_displace_type _atom_site_occupancy _atom_site_calc_flag _atom_site_refinement_flags _atom_site_disorder_group Si1 Si 0.15795(4) 0.04183(7) 0.86037(3) 0.02544(14) Uani 1 d . . Cl1 Cl 0.05221(5) -0.09326(8) 0.78512(3) 0.0453(2) Uani 1 d . . Cl2 Cl 0.11580(5) -0.02798(8) 0.95536(3) 0.0388(2) Uani 1 d . . Cl3 Cl 0.32496(5) -0.03025(9) 0.85808(4) 0.0470(2) Uani 1 d . . Si1A Si 0.34028(4) -0.19354(8) 0.64052(3) 0.02591(14) Uani 1 d . . Cl1A Cl 0.43495(5) -0.33168(8) 0.71972(3) 0.0419(2) Uani 1 d . . Cl2A Cl 0.17249(4) -0.27427(8) 0.63072(3) 0.0395(2) Uani 1 d . . Cl3A Cl 0.40221(5) -0.25181(9) 0.54937(3) 0.0411(2) Uani 1 d . . O1 O 0.13207(13) 0.2496(2) 0.84088(8) 0.0349(3) Uani 1 d . . O1A O 0.35881(13) 0.0138(2) 0.66409(8) 0.0328(3) Uani 1 d . . N1 N 0.2081(2) 0.3471(3) 0.89819(11) 0.0389(5) Uani 1 d . . N1A N 0.28788(15) 0.1109(2) 0.60437(9) 0.0326(4) Uani 1 d . . C1A C 0.2019(3) 0.2101(4) 0.6374(2) 0.0478(6) Uani 1 d . . H11A H 0.2397(34) 0.2901(50) 0.6730(19) 0.080 Uiso 1 d . . H12A H 0.1587(33) 0.2711(49) 0.5974(20) 0.080 Uiso 1 d . . H13A H 0.1501(33) 0.1277(53) 0.6559(19) 0.080 Uiso 1 d . . C2A C 0.3707(3) 0.2294(4) 0.5766(2) 0.0499(6) Uani 1 d . . H21A H 0.4264(35) 0.1593(51) 0.5578(19) 0.080 Uiso 1 d . . H22A H 0.3250(29) 0.2949(42) 0.5399(17) 0.057(8) Uiso 1 d . . H23A H 0.4071(26) 0.3056(40) 0.6160(15) 0.049(8) Uiso 1 d . . C1 C 0.1278(3) 0.4568(4) 0.9316(2) 0.0552(7) Uani 1 d . . H11 H 0.1737(34) 0.5202(49) 0.9659(21) 0.080 Uiso 1 d . . H12 H 0.0930(33) 0.5391(53) 0.8964(19) 0.080 Uiso 1 d . . H13 H 0.0841(34) 0.3808(53) 0.9555(20) 0.080 Uiso 1 d . . C2 C 0.2846(3) 0.4548(4) 0.8605(2) 0.0624(8) Uani 1 d . . H21 H 0.3246(35) 0.5135(50) 0.8937(21) 0.080 Uiso 1 d . . H22 H 0.3317(33) 0.3775(53) 0.8319(19) 0.080 Uiso 1 d . . H23 H 0.2365(31) 0.5443(50) 0.8237(19) 0.080 Uiso 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 Si1 0.0198(3) 0.0273(3) 0.0291(3) -0.0012(2) 0.0032(2) -0.0016(2) Cl1 0.0480(3) 0.0456(3) 0.0402(3) -0.0118(2) -0.0008(2) -0.0150(3) Cl2 0.0377(3) 0.0471(3) 0.0330(3) 0.0025(2) 0.0105(2) -0.0035(2) Cl3 0.0257(3) 0.0450(3) 0.0742(4) -0.0003(3) 0.0203(3) 0.0043(2) Si1A 0.0189(2) 0.0298(3) 0.0287(3) 0.0008(2) 0.0024(2) 0.0016(2) Cl1A 0.0416(3) 0.0447(3) 0.0385(3) 0.0098(2) 0.0026(2) 0.0158(2) Cl2A 0.0230(2) 0.0393(3) 0.0573(3) -0.0063(2) 0.0095(2) -0.0062(2) Cl3A 0.0359(3) 0.0534(4) 0.0361(3) 0.0007(2) 0.0129(2) 0.0077(2) O1 0.0306(7) 0.0301(8) 0.0396(8) 0.0001(6) -0.0096(6) -0.0019(6) O1A 0.0284(7) 0.0313(8) 0.0354(7) 0.0034(6) -0.0067(6) -0.0009(6) N1 0.0323(9) 0.0285(9) 0.0499(11) -0.0039(8) -0.0139(8) -0.0031(7) N1A 0.0290(9) 0.0296(9) 0.0366(9) 0.0057(7) -0.0036(7) 0.0011(7) C1A 0.0463(14) 0.0371(13) 0.060(2) 0.0013(12) 0.0060(12) 0.0115(11) C2A 0.0438(14) 0.0427(14) 0.062(2) 0.0169(13) 0.0018(13) -0.0087(12) C1 0.051(2) 0.0397(14) 0.068(2) -0.0179(14) -0.0149(14) 0.0113(12) C2 0.053(2) 0.042(2) 0.088(2) 0.008(2) -0.005(2) -0.0192(13) _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 Si1 O1 1.618(2) . ? Si1 Cl2 2.0126(7) . ? Si1 Cl3 2.0152(8) . ? Si1 Cl1 2.0176(8) . ? Si1A O1A 1.622(2) . ? Si1A Cl1A 2.0177(8) . ? Si1A Cl2A 2.0182(7) . ? Si1A Cl3A 2.0223(8) . ? O1 N1 1.491(2) . ? O1A N1A 1.493(2) . ? N1 C1 1.455(4) . ? N1 C2 1.462(4) . ? N1A C1A 1.457(3) . ? N1A C2A 1.461(3) . ? C1A H11A 0.96(4) . ? C1A H12A 0.96(4) . ? C1A H13A 0.96(4) . ? C2A H21A 0.94(4) . ? C2A H22A 0.95(3) . ? C2A H23A 0.99(3) . ? C1 H11 0.91(4) . ? C1 H12 0.96(4) . ? C1 H13 0.92(4) . ? C2 H21 0.85(4) . ? C2 H22 1.01(4) . ? C2 H23 1.07(4) . ? 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 O1 Si1 Cl2 113.29(7) . . ? O1 Si1 Cl3 113.52(7) . . ? Cl2 Si1 Cl3 108.03(4) . . ? O1 Si1 Cl1 104.23(6) . . ? Cl2 Si1 Cl1 107.95(3) . . ? Cl3 Si1 Cl1 109.62(4) . . ? O1A Si1A Cl1A 104.33(6) . . ? O1A Si1A Cl2A 113.53(6) . . ? Cl1A Si1A Cl2A 109.09(4) . . ? O1A Si1A Cl3A 113.30(6) . . ? Cl1A Si1A Cl3A 108.09(3) . . ? Cl2A Si1A Cl3A 108.26(4) . . ? N1 O1 Si1 103.44(11) . . ? N1A O1A Si1A 102.63(11) . . ? C1 N1 C2 112.1(3) . . ? C1 N1 O1 104.5(2) . . ? C2 N1 O1 104.2(2) . . ? C1A N1A C2A 111.9(2) . . ? C1A N1A O1A 104.7(2) . . ? C2A N1A O1A 104.7(2) . . ? N1A C1A H11A 110.7(22) . . ? N1A C1A H12A 102.0(22) . . ? H11A C1A H12A 113.2(30) . . ? N1A C1A H13A 109.5(22) . . ? H11A C1A H13A 112.5(30) . . ? H12A C1A H13A 108.3(30) . . ? N1A C2A H21A 108.7(23) . . ? N1A C2A H22A 104.8(19) . . ? H21A C2A H22A 110.2(28) . . ? N1A C2A H23A 107.8(17) . . ? H21A C2A H23A 111.8(28) . . ? H22A C2A H23A 113.2(25) . . ? N1 C1 H11 105.3(23) . . ? N1 C1 H12 106.7(21) . . ? H11 C1 H12 108.0(31) . . ? N1 C1 H13 107.4(24) . . ? H11 C1 H13 105.7(31) . . ? H12 C1 H13 122.5(33) . . ? N1 C2 H21 102.8(26) . . ? N1 C2 H22 111.4(22) . . ? H21 C2 H22 114.8(34) . . ? N1 C2 H23 111.9(19) . . ? H21 C2 H23 110.0(32) . . ? H22 C2 H23 106.1(28) . . ? 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 Cl2 Si1 O1 N1 61.25(13) . . . . ? Cl3 Si1 O1 N1 -62.45(13) . . . . ? Cl1 Si1 O1 N1 178.33(11) . . . . ? Cl1A Si1A O1A N1A 179.92(9) . . . . ? Cl2A Si1A O1A N1A -61.42(12) . . . . ? Cl3A Si1A O1A N1A 62.60(12) . . . . ? Si1 O1 N1 C1 -121.6(2) . . . . ? Si1 O1 N1 C2 120.7(2) . . . . ? Si1A O1A N1A C1A 120.6(2) . . . . ? Si1A O1A N1A C2A -121.5(2) . . . . ? _refine_diff_density_max 0.539 _refine_diff_density_min -0.455 _refine_diff_density_rms 0.097