data_shelx _audit_creation_method SHELXL-2012 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C16 H30 O3 Si2' _chemical_formula_weight 326.58 _chemical_oxdiff_usercomment 'Darren Loits/MAR' loop_ _atom_type_symbol _atom_type_description _atom_type_scat_dispersion_real _atom_type_scat_dispersion_imag _atom_type_scat_source 'C' 'C' 0.0181 0.0091 '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' 'O' 'O' 0.0492 0.0322 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' 'Si' 'Si' 0.2541 0.3302 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _space_group_crystal_system orthorhombic _space_group_IT_number 41 _space_group_name_H-M_alt 'A b a 2' _space_group_name_Hall 'A 2 -2ac' _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. ; loop_ _space_group_symop_operation_xyz 'x, y, z' '-x, -y, z' 'x+1/2, -y+1/2, z' '-x+1/2, y+1/2, z' 'x, y+1/2, z+1/2' '-x, -y+1/2, z+1/2' 'x+1/2, -y+1, z+1/2' '-x+1/2, y+1, z+1/2' _cell_length_a 30.9982(4) _cell_length_b 11.38100(10) _cell_length_c 11.12910(10) _cell_angle_alpha 90 _cell_angle_beta 90 _cell_angle_gamma 90 _cell_volume 3926.24(7) _cell_formula_units_Z 8 _cell_measurement_temperature 130.0(1) _cell_measurement_reflns_used 7516 _cell_measurement_theta_min 5.7040 _cell_measurement_theta_max 76.9960 _exptl_crystal_description plate _exptl_crystal_colour colourless _exptl_crystal_density_meas ? _exptl_crystal_density_method ? _exptl_crystal_density_diffrn 1.105 _exptl_crystal_F_000 1424 _exptl_transmission_factor_min ? _exptl_transmission_factor_max ? _exptl_crystal_size_max 0.6696 _exptl_crystal_size_mid 0.4822 _exptl_crystal_size_min 0.0437 _exptl_absorpt_coefficient_mu 1.693 _shelx_estimated_absorpt_T_min ? _shelx_estimated_absorpt_T_max ? _exptl_absorpt_correction_T_min 0.56536 _exptl_absorpt_correction_T_max 1.00000 _exptl_absorpt_correction_type 'multi-scan' _exptl_absorpt_process_details ; CrysAlisPro, Agilent Technologies, Version 1.171.36.28 (release 01-02-2013 CrysAlis171 .NET) (compiled Feb 1 2013,16:14:44) Empirical absorption correction using spherical harmonics, implemented in SCALE3 ABSPACK scaling algorithm. ; _exptl_special_details ; ? ; _diffrn_ambient_temperature 130.0(1) _diffrn_radiation_wavelength 1.5418 _diffrn_radiation_type 'Cu K\a' _diffrn_radiation_source 'SuperNova (Cu) X-ray Source' _diffrn_radiation_monochromator 'mirror' _diffrn_measurement_device_type 'SuperNova, Dual, Cu at zero, Atlas' _diffrn_measurement_method '\w scans' _diffrn_detector_area_resol_mean ? _diffrn_reflns_number 11405 _diffrn_reflns_av_unetI/netI 0.0304 _diffrn_reflns_av_R_equivalents 0.0408 _diffrn_reflns_limit_h_min -37 _diffrn_reflns_limit_h_max 36 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -6 _diffrn_reflns_limit_l_max 13 _diffrn_reflns_theta_min 5.709 _diffrn_reflns_theta_max 67.492 _diffrn_reflns_theta_full 67.684 _diffrn_measured_fraction_theta_max 0.998 _diffrn_measured_fraction_theta_full 0.992 _diffrn_reflns_Laue_measured_fraction_max 0.998 _diffrn_reflns_Laue_measured_fraction_full 0.992 _diffrn_reflns_point_group_measured_fraction_max 0.764 _diffrn_reflns_point_group_measured_fraction_full 0.758 _reflns_number_total 2707 _reflns_number_gt 2653 _reflns_threshold_expression 'I > 2\s(I)' _reflns_Friedel_coverage 0.448 _reflns_Friedel_fraction_max 0.501 _reflns_Friedel_fraction_full 0.497 _reflns_special_details ; Reflections were merged by SHELXL according to the crystal class for the calculation of statistics and refinement. _reflns_Friedel_fraction is defined as the number of unique Friedel pairs measured divided by the number that would be possible theoretically, ignoring centric projections and systematic absences. These statistics refer to single and composite reflections containing twin component 1 only. ; _computing_data_collection ? _computing_cell_refinement ? _computing_data_reduction ? _computing_structure_solution ? _computing_structure_refinement 'SHELXL-2012 (Sheldrick, 2012)' _computing_molecular_graphics ? _computing_publication_material ? _refine_special_details ; Refined as a 2-component inversion twin. ; _refine_ls_structure_factor_coef Fsqd _refine_ls_matrix_type full _refine_ls_weighting_scheme calc _refine_ls_weighting_details ; w=1/[\s^2^(Fo^2^)+(0.0438P)^2^+1.6435P] where P=(Fo^2^+2Fc^2^)/3 ; _atom_sites_solution_primary ? _atom_sites_solution_secondary ? _atom_sites_solution_hydrogens geom _refine_ls_hydrogen_treatment constr _refine_ls_extinction_method none _refine_ls_extinction_coef . _refine_ls_abs_structure_details ; Refined as an inversion twin. ; _refine_ls_abs_structure_Flack 0.24(4) _chemical_absolute_configuration ? _refine_ls_number_reflns 2707 _refine_ls_number_parameters 210 _refine_ls_number_restraints 13 _refine_ls_R_factor_all 0.0309 _refine_ls_R_factor_gt 0.0300 _refine_ls_wR_factor_ref 0.0785 _refine_ls_wR_factor_gt 0.0777 _refine_ls_goodness_of_fit_ref 1.077 _refine_ls_restrained_S_all 1.081 _refine_ls_shift/su_max 0.002 _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_site_symmetry_order _atom_site_calc_flag _atom_site_refinement_flags_posn _atom_site_refinement_flags_adp _atom_site_refinement_flags_occupancy _atom_site_disorder_assembly _atom_site_disorder_group C1 C 0.79586(8) 0.7713(2) 0.9346(2) 0.0192(5) Uani 1 1 d . . . . . H1 H 0.7807 0.7376 0.8654 0.023 Uiso 1 1 calc R U . . . C2 C 0.77929(8) 0.8952(2) 0.9544(2) 0.0192(5) Uani 1 1 d . . . . . H2A H 0.7792 0.9376 0.8788 0.023 Uiso 1 1 calc R U . . . H2B H 0.7982 0.9363 1.0097 0.023 Uiso 1 1 calc R U . . . C3 C 0.73387(7) 0.8919(2) 1.0054(2) 0.0184(5) Uani 1 1 d . . . . . H3 H 0.7230 0.9719 1.0169 0.022 Uiso 1 1 calc R U . . . C4 C 0.73526(8) 0.8276(2) 1.1246(2) 0.0202(5) Uani 1 1 d . . . . . H4A H 0.7507 0.8756 1.1824 0.024 Uiso 1 1 calc R U . . . H4B H 0.7060 0.8177 1.1539 0.024 Uiso 1 1 calc R U . . . C5 C 0.75657(7) 0.7089(2) 1.1178(2) 0.0188(5) Uani 1 1 d . . . . . C6 C 0.84252(8) 0.7697(2) 0.9094(3) 0.0254(6) Uani 1 1 d . . . . . C7 C 0.88045(8) 0.7716(2) 0.8913(3) 0.0339(7) Uani 1 1 d . . . . . C8 C 0.95588(11) 0.8706(4) 0.7550(4) 0.0488(10) Uani 1 1 d . . . . . H8A H 0.9868 0.8724 0.7493 0.073 Uiso 1 1 calc R U . . . H8B H 0.9453 0.9485 0.7694 0.073 Uiso 1 1 calc R U . . . H8C H 0.9440 0.8411 0.6813 0.073 Uiso 1 1 calc R U . . . C11 C 0.63382(8) 0.9524(2) 1.0269(3) 0.0258(6) Uani 1 1 d . . . . . H11A H 0.6373 0.9121 1.1020 0.039 Uiso 1 1 calc R U . . . H11B H 0.6038 0.9686 1.0138 0.039 Uiso 1 1 calc R U . . . H11C H 0.6496 1.0249 1.0288 0.039 Uiso 1 1 calc R U . . . C12 C 0.64850(9) 0.9351(3) 0.7568(3) 0.0309(7) Uani 1 1 d . . . . . H12A H 0.6593 0.8860 0.6935 0.046 Uiso 1 1 calc R U . . . H12B H 0.6645 1.0074 0.7585 0.046 Uiso 1 1 calc R U . . . H12C H 0.6186 0.9517 0.7429 0.046 Uiso 1 1 calc R U . . . C13 C 0.62619(7) 0.7121(2) 0.9009(3) 0.0202(5) Uani 1 1 d . . . . . C14 C 0.57768(8) 0.7305(3) 0.8803(3) 0.0336(7) Uani 1 1 d . . . . . H14A H 0.5733 0.7694 0.8048 0.050 Uiso 1 1 calc R U . . . H14B H 0.5661 0.7779 0.9440 0.050 Uiso 1 1 calc R U . . . H14C H 0.5634 0.6557 0.8794 0.050 Uiso 1 1 calc R U . . . C15 C 0.63290(10) 0.6493(3) 1.0212(3) 0.0300(6) Uani 1 1 d . . . . . H15A H 0.6216 0.6970 1.0850 0.045 Uiso 1 1 calc R U . . . H15B H 0.6632 0.6365 1.0340 0.045 Uiso 1 1 calc R U . . . H15C H 0.6182 0.5751 1.0200 0.045 Uiso 1 1 calc R U . . . C16 C 0.64416(10) 0.6353(3) 0.7989(3) 0.0337(7) Uani 1 1 d . . . . . H16A H 0.6400 0.6746 0.7234 0.051 Uiso 1 1 calc R U . . . H16B H 0.6293 0.5613 0.7978 0.051 Uiso 1 1 calc R U . . . H16C H 0.6744 0.6221 0.8117 0.051 Uiso 1 1 calc R U . . . O1 O 0.78927(5) 0.69378(15) 1.03816(17) 0.0209(4) Uani 1 1 d . . . . . O2 O 0.74782(7) 0.62806(16) 1.18264(18) 0.0263(4) Uani 1 1 d . . . . . O3 O 0.70667(5) 0.82930(14) 0.92348(16) 0.0185(4) Uani 1 1 d . . . . . Si2 Si 0.65464(2) 0.85852(5) 0.90271(7) 0.01587(15) Uani 1 1 d . . . . . Si1 Si 0.93990(2) 0.77455(7) 0.87921(9) 0.0351(2) Uani 1 1 d . . . . . C9 C 0.9612(9) 0.866(2) 1.019(3) 0.053(5) Uani 0.39(3) 1 d . U P A 1 H9A H 0.9488 0.9430 1.0179 0.080 Uiso 0.39(3) 1 calc R U P A 1 H9B H 0.9921 0.8720 1.0151 0.080 Uiso 0.39(3) 1 calc R U P A 1 H9C H 0.9532 0.8266 1.0921 0.080 Uiso 0.39(3) 1 calc R U P A 1 C10 C 0.9614(5) 0.6292(15) 0.900(4) 0.080(7) Uani 0.39(3) 1 d . U P A 1 H10A H 0.9490 0.5945 0.9705 0.121 Uiso 0.39(3) 1 calc R U P A 1 H10B H 0.9922 0.6336 0.9091 0.121 Uiso 0.39(3) 1 calc R U P A 1 H10C H 0.9546 0.5817 0.8311 0.121 Uiso 0.39(3) 1 calc R U P A 1 C10' C 0.9588(4) 0.6246(9) 0.8242(18) 0.062(4) Uani 0.61(3) 1 d . U P A 2 H10D H 0.9477 0.6106 0.7449 0.094 Uiso 0.61(3) 1 calc R U P A 2 H10E H 0.9484 0.5647 0.8777 0.094 Uiso 0.61(3) 1 calc R U P A 2 H10F H 0.9898 0.6228 0.8223 0.094 Uiso 0.61(3) 1 calc R U P A 2 C9' C 0.9600(6) 0.808(3) 1.0244(19) 0.091(6) Uani 0.61(3) 1 d . U P A 2 H9'1 H 0.9493 0.7520 1.0812 0.137 Uiso 0.61(3) 1 calc R U P A 2 H9'2 H 0.9506 0.8857 1.0472 0.137 Uiso 0.61(3) 1 calc R U P A 2 H9'3 H 0.9910 0.8060 1.0233 0.137 Uiso 0.61(3) 1 calc R U 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 C1 0.0175(11) 0.0199(12) 0.0201(13) 0.0027(10) 0.0016(10) -0.0010(9) C2 0.0199(12) 0.0153(11) 0.0225(13) -0.0002(10) -0.0023(10) -0.0029(9) C3 0.0194(11) 0.0171(11) 0.0185(13) -0.0026(10) -0.0022(10) -0.0012(9) C4 0.0231(11) 0.0223(13) 0.0152(12) -0.0037(11) -0.0006(10) 0.0013(9) C5 0.0172(13) 0.0245(12) 0.0147(12) -0.0011(10) -0.0024(10) -0.0019(9) C6 0.0221(12) 0.0251(12) 0.0290(15) 0.0020(14) 0.0013(11) 0.0005(9) C7 0.0244(13) 0.0324(13) 0.0449(19) 0.0066(15) 0.0040(15) 0.0026(10) C8 0.0272(16) 0.064(3) 0.055(3) 0.0102(19) 0.0047(17) -0.0019(16) C11 0.0254(12) 0.0238(13) 0.0281(14) -0.0043(12) 0.0050(12) 0.0034(10) C12 0.0298(14) 0.0345(16) 0.0285(16) 0.0124(13) 0.0016(12) 0.0068(12) C13 0.0189(11) 0.0218(10) 0.0200(12) -0.0024(12) 0.0003(11) -0.0022(8) C14 0.0196(11) 0.0419(15) 0.0392(18) -0.0031(14) -0.0014(14) -0.0042(10) C15 0.0377(15) 0.0235(13) 0.0290(16) 0.0042(12) -0.0004(13) -0.0067(11) C16 0.0393(16) 0.0273(15) 0.0346(19) -0.0134(13) 0.0082(15) -0.0069(12) O1 0.0213(8) 0.0200(8) 0.0213(9) 0.0037(8) 0.0028(7) 0.0034(7) O2 0.0302(9) 0.0250(9) 0.0238(11) 0.0050(8) 0.0017(9) 0.0001(8) O3 0.0163(7) 0.0192(8) 0.0201(10) -0.0059(8) -0.0023(7) -0.0003(6) Si2 0.0161(3) 0.0167(3) 0.0148(3) 0.0017(3) 0.0007(3) 0.0019(2) Si1 0.0173(3) 0.0390(4) 0.0490(6) 0.0107(4) 0.0066(4) 0.0037(3) C9 0.025(5) 0.107(13) 0.029(6) 0.000(10) 0.000(4) 0.005(8) C10 0.029(5) 0.034(5) 0.18(2) 0.000(12) 0.013(12) -0.003(4) C10' 0.031(4) 0.029(4) 0.127(11) 0.016(6) 0.033(6) 0.010(3) C9' 0.032(4) 0.203(19) 0.039(6) -0.014(13) -0.005(4) 0.015(11) _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 C1 O1 1.466(3) . ? C1 C6 1.474(3) . ? C1 C2 1.517(3) . ? C2 C3 1.518(3) . ? C3 O3 1.431(3) . ? C3 C4 1.516(4) . ? C4 C5 1.506(3) . ? C5 O2 1.200(3) . ? C5 O1 1.357(3) . ? C6 C7 1.193(4) . ? C7 Si1 1.848(3) . ? C8 Si1 1.830(4) . ? C11 Si2 1.862(3) . ? C12 Si2 1.852(3) . ? C13 C15 1.532(4) . ? C13 C14 1.535(3) . ? C13 C16 1.537(4) . ? C13 Si2 1.886(2) . ? O3 Si2 1.6631(16) . ? Si1 C9' 1.77(2) . ? Si1 C10 1.799(18) . ? Si1 C10' 1.906(12) . ? Si1 C9 1.99(3) . ? 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 C1 C6 106.2(2) . . ? O1 C1 C2 113.4(2) . . ? C6 C1 C2 111.8(2) . . ? C1 C2 C3 110.2(2) . . ? O3 C3 C4 109.5(2) . . ? O3 C3 C2 108.7(2) . . ? C4 C3 C2 108.2(2) . . ? C5 C4 C3 113.6(2) . . ? O2 C5 O1 117.7(2) . . ? O2 C5 C4 123.9(2) . . ? O1 C5 C4 118.3(2) . . ? C7 C6 C1 177.8(3) . . ? C6 C7 Si1 174.4(3) . . ? C15 C13 C14 109.1(2) . . ? C15 C13 C16 109.4(2) . . ? C14 C13 C16 108.8(2) . . ? C15 C13 Si2 109.82(18) . . ? C14 C13 Si2 109.81(17) . . ? C16 C13 Si2 109.92(18) . . ? C5 O1 C1 122.79(19) . . ? C3 O3 Si2 124.08(15) . . ? O3 Si2 C12 108.39(12) . . ? O3 Si2 C11 110.35(11) . . ? C12 Si2 C11 110.16(14) . . ? O3 Si2 C13 106.16(9) . . ? C12 Si2 C13 111.01(14) . . ? C11 Si2 C13 110.68(12) . . ? C9' Si1 C8 117.6(9) . . ? C10 Si1 C8 123.0(12) . . ? C9' Si1 C7 106.7(6) . . ? C10 Si1 C7 110.1(6) . . ? C8 Si1 C7 109.61(16) . . ? C9' Si1 C10' 112.3(6) . . ? C8 Si1 C10' 102.1(5) . . ? C7 Si1 C10' 108.3(4) . . ? C10 Si1 C9 104.9(12) . . ? C8 Si1 C9 100.9(7) . . ? C7 Si1 C9 106.5(8) . . ? 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 O1 C1 C2 C3 -48.1(3) . . . . ? C6 C1 C2 C3 -168.1(2) . . . . ? C1 C2 C3 O3 -58.4(3) . . . . ? C1 C2 C3 C4 60.5(3) . . . . ? O3 C3 C4 C5 65.8(3) . . . . ? C2 C3 C4 C5 -52.6(3) . . . . ? C3 C4 C5 O2 -151.2(3) . . . . ? C3 C4 C5 O1 32.6(3) . . . . ? O2 C5 O1 C1 163.5(2) . . . . ? C4 C5 O1 C1 -20.0(3) . . . . ? C6 C1 O1 C5 151.2(2) . . . . ? C2 C1 O1 C5 28.1(3) . . . . ? C4 C3 O3 Si2 94.3(2) . . . . ? C2 C3 O3 Si2 -147.63(17) . . . . ? C3 O3 Si2 C12 105.3(2) . . . . ? C3 O3 Si2 C11 -15.4(2) . . . . ? C3 O3 Si2 C13 -135.35(19) . . . . ? C15 C13 Si2 O3 60.8(2) . . . . ? C14 C13 Si2 O3 -179.3(2) . . . . ? C16 C13 Si2 O3 -59.6(2) . . . . ? C15 C13 Si2 C12 178.39(18) . . . . ? C14 C13 Si2 C12 -61.7(2) . . . . ? C16 C13 Si2 C12 58.0(2) . . . . ? C15 C13 Si2 C11 -59.0(2) . . . . ? C14 C13 Si2 C11 61.0(2) . . . . ? C16 C13 Si2 C11 -179.3(2) . . . . ? _refine_diff_density_max 0.222 _refine_diff_density_min -0.309 _refine_diff_density_rms 0.044 _shelxl_version_number 2012-9