Supplementary Material for PCCP This journal is (c) The Owner Societies 2010 data_1 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C10 H23 N2 O Si2, Cl' _chemical_formula_sum 'C10 H23 Cl N2 O Si2' _chemical_formula_weight 278.93 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' '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 15.1593(3) _cell_length_b 8.54934(14) _cell_length_c 12.6684(3) _cell_angle_alpha 90.00 _cell_angle_beta 103.130(2) _cell_angle_gamma 90.00 _cell_volume 1598.93(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 8591 _cell_measurement_theta_min 2.7478 _cell_measurement_theta_max 31.3468 _exptl_crystal_description blocks _exptl_crystal_colour Colourless _exptl_crystal_size_max 0.51 _exptl_crystal_size_mid 0.32 _exptl_crystal_size_min 0.08 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.159 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 600 _exptl_absorpt_coefficient_mu 0.375 _exptl_absorpt_correction_type analytical _exptl_absorpt_correction_T_min 0.890 _exptl_absorpt_correction_T_max 0.969 _exptl_absorpt_process_details ; CrysAlisPro, Oxford Diffraction Ltd., Version 1.171.33.34d (release 27-02-2009 CrysAlis171 .NET) (compiled Feb 27 2009,15:38:38) Analytical numeric absorption correction using a multifaceted crystal model based on expressions derived by R.C. Clark & J.S. Reid. (Clark, R. C. & Reid, J. S. (1995). Acta Cryst. A51, 887-897) ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'Enhance (Mo) X-ray Source' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'OD Xcalibur 3' _diffrn_measurement_method 'omega scans' _diffrn_detector_area_resol_mean 15.9863 _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13436 _diffrn_reflns_av_R_equivalents 0.0175 _diffrn_reflns_av_sigmaI/netI 0.0214 _diffrn_reflns_limit_h_min -21 _diffrn_reflns_limit_h_max 18 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 15 _diffrn_reflns_theta_min 2.75 _diffrn_reflns_theta_max 31.42 _reflns_number_total 4574 _reflns_number_gt 3707 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'CrysAlis CCD, Oxford Diffraction Ltd' _computing_cell_refinement 'CrysAlis RED, Oxford Diffraction Ltd' _computing_data_reduction 'CrysAlis RED, Oxford Diffraction Ltd' _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^)+(0.0498P)^2^+0.3661P] 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 constr _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 4574 _refine_ls_number_parameters 151 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0414 _refine_ls_R_factor_gt 0.0317 _refine_ls_wR_factor_ref 0.0914 _refine_ls_wR_factor_gt 0.0893 _refine_ls_goodness_of_fit_ref 1.033 _refine_ls_restrained_S_all 1.033 _refine_ls_shift/su_max 0.001 _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 N1 N 0.37966(7) 0.47550(12) 0.59163(9) 0.0225(2) Uani 1 1 d . . . C2 C 0.38367(8) 0.62454(14) 0.56166(11) 0.0263(3) Uani 1 1 d . . . H2A H 0.3813 0.7137 0.6057 0.032 Uiso 1 1 calc R . . N3 N 0.39147(7) 0.62627(13) 0.45930(10) 0.0273(2) Uani 1 1 d . . . C4 C 0.39236(9) 0.47539(16) 0.42227(12) 0.0293(3) Uani 1 1 d . . . H4A H 0.3973 0.4437 0.3520 0.035 Uiso 1 1 calc R . . C5 C 0.38476(8) 0.38083(15) 0.50502(11) 0.0262(3) Uani 1 1 d . . . H5A H 0.3832 0.2697 0.5039 0.031 Uiso 1 1 calc R . . C6 C 0.36377(8) 0.42053(15) 0.69580(10) 0.0244(2) Uani 1 1 d . . . H6A H 0.4009 0.4828 0.7556 0.029 Uiso 1 1 calc R . . H6B H 0.3825 0.3097 0.7070 0.029 Uiso 1 1 calc R . . Si7 Si 0.24036(2) 0.43965(4) 0.69856(3) 0.02323(9) Uani 1 1 d . . . O8 O 0.21674(6) 0.62525(11) 0.68345(9) 0.0310(2) Uani 1 1 d . . . Si9 Si 0.13644(3) 0.75671(4) 0.65589(3) 0.02947(10) Uani 1 1 d . . . C10 C 0.39861(10) 0.76778(18) 0.39638(13) 0.0376(3) Uani 1 1 d . . . H10A H 0.3948 0.8604 0.4408 0.056 Uiso 1 1 calc R . . H10B H 0.3490 0.7698 0.3315 0.056 Uiso 1 1 calc R . . H10C H 0.4567 0.7678 0.3748 0.056 Uiso 1 1 calc R . . C11 C 0.22341(10) 0.36964(17) 0.83044(12) 0.0341(3) Uani 1 1 d . . . H11A H 0.1593 0.3797 0.8321 0.051 Uiso 1 1 calc R . . H11B H 0.2603 0.4324 0.8889 0.051 Uiso 1 1 calc R . . H11C H 0.2416 0.2597 0.8403 0.051 Uiso 1 1 calc R . . C12 C 0.17258(10) 0.3262(2) 0.58406(13) 0.0404(3) Uani 1 1 d . . . H12A H 0.1081 0.3356 0.5840 0.061 Uiso 1 1 calc R . . H12B H 0.1906 0.2159 0.5918 0.061 Uiso 1 1 calc R . . H12C H 0.1831 0.3670 0.5157 0.061 Uiso 1 1 calc R . . C13 C 0.03014(10) 0.6706(2) 0.68043(17) 0.0521(5) Uani 1 1 d . . . H13A H 0.0394 0.6405 0.7568 0.078 Uiso 1 1 calc R . . H13B H 0.0137 0.5781 0.6346 0.078 Uiso 1 1 calc R . . H13C H -0.0187 0.7480 0.6629 0.078 Uiso 1 1 calc R . . C14 C 0.12140(16) 0.8150(3) 0.51279(17) 0.0676(6) Uani 1 1 d . . . H14A H 0.1780 0.8601 0.5015 0.101 Uiso 1 1 calc R . . H14B H 0.0729 0.8929 0.4946 0.101 Uiso 1 1 calc R . . H14C H 0.1053 0.7230 0.4662 0.101 Uiso 1 1 calc R . . C15 C 0.17250(12) 0.92573(19) 0.74600(17) 0.0470(4) Uani 1 1 d . . . H15A H 0.2285 0.9694 0.7320 0.070 Uiso 1 1 calc R . . H15B H 0.1832 0.8918 0.8217 0.070 Uiso 1 1 calc R . . H15C H 0.1250 1.0058 0.7321 0.070 Uiso 1 1 calc R . . Cl Cl 0.39404(8) 0.49161(4) 0.14257(6) 0.0341(2) Uani 0.969(4) 1 d P A 1 Cl' Cl 0.3549(17) 0.4948(14) 0.1195(13) 0.024(4) Uiso 0.031(4) 1 d P A 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 N1 0.0227(5) 0.0186(5) 0.0271(5) 0.0007(4) 0.0073(4) 0.0019(4) C2 0.0254(6) 0.0191(6) 0.0361(7) 0.0017(5) 0.0107(5) 0.0017(5) N3 0.0241(5) 0.0250(5) 0.0336(6) 0.0064(4) 0.0084(4) 0.0015(4) C4 0.0297(6) 0.0310(7) 0.0274(7) -0.0010(5) 0.0067(5) 0.0011(5) C5 0.0273(6) 0.0227(6) 0.0283(6) -0.0030(5) 0.0054(5) 0.0005(5) C6 0.0283(6) 0.0200(5) 0.0253(6) 0.0018(5) 0.0072(5) 0.0028(5) Si7 0.02555(17) 0.01916(16) 0.02575(18) 0.00042(13) 0.00745(13) -0.00157(12) O8 0.0279(5) 0.0223(4) 0.0443(6) 0.0042(4) 0.0112(4) 0.0032(4) Si9 0.02704(19) 0.02898(19) 0.0333(2) 0.00512(15) 0.00878(15) 0.00648(14) C10 0.0375(8) 0.0324(7) 0.0440(8) 0.0168(6) 0.0116(6) 0.0017(6) C11 0.0397(7) 0.0320(7) 0.0328(7) 0.0053(6) 0.0132(6) -0.0022(6) C12 0.0379(8) 0.0426(8) 0.0386(8) -0.0083(7) 0.0046(6) -0.0091(7) C13 0.0278(7) 0.0635(12) 0.0652(12) -0.0025(10) 0.0113(7) -0.0031(8) C14 0.0827(15) 0.0758(14) 0.0448(11) 0.0251(10) 0.0158(10) 0.0248(12) C15 0.0427(9) 0.0332(8) 0.0690(12) -0.0083(8) 0.0210(8) 0.0041(7) Cl 0.0489(6) 0.02122(17) 0.0361(2) -0.00090(14) 0.0179(3) 0.00141(16) _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 N1 C2 1.3348(16) . ? N1 C5 1.3797(16) . ? N1 C6 1.4713(16) . ? C2 N3 1.3287(18) . ? N3 C4 1.3737(17) . ? N3 C10 1.4663(17) . ? C4 C5 1.3494(19) . ? C6 Si7 1.8861(13) . ? Si7 O8 1.6283(10) . ? Si7 C11 1.8468(15) . ? Si7 C12 1.8502(15) . ? O8 Si9 1.6353(10) . ? Si9 C14 1.844(2) . ? Si9 C15 1.8457(18) . ? Si9 C13 1.8608(17) . ? 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 C2 N1 C5 108.63(11) . . ? C2 N1 C6 125.97(11) . . ? C5 N1 C6 125.17(10) . . ? N3 C2 N1 107.94(11) . . ? C2 N3 C4 109.44(11) . . ? C2 N3 C10 125.00(12) . . ? C4 N3 C10 125.55(13) . . ? C5 C4 N3 106.74(12) . . ? C4 C5 N1 107.24(11) . . ? N1 C6 Si7 110.74(8) . . ? O8 Si7 C11 110.49(6) . . ? O8 Si7 C12 110.52(7) . . ? C11 Si7 C12 111.88(7) . . ? O8 Si7 C6 105.95(5) . . ? C11 Si7 C6 109.33(6) . . ? C12 Si7 C6 108.46(7) . . ? Si7 O8 Si9 145.89(7) . . ? O8 Si9 C14 108.39(8) . . ? O8 Si9 C15 107.73(7) . . ? C14 Si9 C15 110.46(11) . . ? O8 Si9 C13 108.87(8) . . ? C14 Si9 C13 110.66(10) . . ? C15 Si9 C13 110.63(9) . . ? _diffrn_measured_fraction_theta_max 0.862 _diffrn_reflns_theta_full 29.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.403 _refine_diff_density_min -0.216 _refine_diff_density_rms 0.047 #===END