# Supplementary Material (ESI) for New Journal of Chemistry # This journal is (c) The Royal Society of Chemistry and # The Centre National de la Recherche Scientifique, 2007 data_global _journal_name_full 'New J.Chem.' _journal_coden_Cambridge 0440 _publ_contact_author_name 'Pascal Le Floch' _publ_contact_author_address ; Departement de Chimie Ecole Polytechnique Laboratoire Heteroelements et Coord UMR CNRS 7653 (DCPH) Palaiseau Palaiseau cedex 91128 FRANCE ; _publ_contact_author_email LEFLOCH@POLY.POLYTECHNIQUE.FR _publ_section_title ; Experimental and Theoretical Study of Phosphinine Sulfides ; _publ_section_exptl_prep ;All structures were solved using SIR97 (Altomare et al.) and refined with SHELXL97 (Sheldrick). Figures were drawn with Platon (Spek, 1990). ; _publ_section_references ;Altomare, A., Cascarano, G., Giacovazzo, C. & Guagliardi, A. (1993) J. Appl. Cryst. 26, 343-350. Sheldrick, G.M. SHELXL97. Program for crystal structure refinement. University of G\\"ottingen, Germany, 1997. Sluis, P. v.d., Spek, A.L. (1990). Acta Cryst. A46, 194-201. Spek, A.L. (1990). Acta Cryst. A46, C-34. ; loop_ _publ_author_name 'Pascal Le Floch' 'Thibault Cantat' 'Nicolas Mezailles' 'Audrey Moores' 'Louis Ricard' data_psi2ph2 _database_code_depnum_ccdc_archive 'CCDC 637688' #compound 2 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H29 P Si2' _chemical_formula_sum 'C23 H29 P Si2' _chemical_formula_weight 392.61 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' Si Si 0.0817 0.0704 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Monoclinic _symmetry_space_group_name_H-M 'P21/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 12.081(1) _cell_length_b 17.513(1) _cell_length_c 12.328(1) _cell_angle_alpha 90.00 _cell_angle_beta 118.022(1) _cell_angle_gamma 90.00 _cell_volume 2302.5(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 251 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description block _exptl_crystal_colour colorless _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.16 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.133 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 840 _exptl_absorpt_coefficient_mu 0.228 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9558 _exptl_absorpt_correction_T_max 0.9644 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _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 11250 _diffrn_reflns_av_R_equivalents 0.0209 _diffrn_reflns_av_sigmaI/netI 0.0432 _diffrn_reflns_limit_h_min -16 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -20 _diffrn_reflns_limit_k_max 24 _diffrn_reflns_limit_l_min -17 _diffrn_reflns_limit_l_max 17 _diffrn_reflns_theta_min 3.01 _diffrn_reflns_theta_max 30.01 _reflns_number_total 6684 _reflns_number_gt 5111 _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^)+(0.0620P)^2^+0.1790P] 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 6684 _refine_ls_number_parameters 241 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0573 _refine_ls_R_factor_gt 0.0410 _refine_ls_wR_factor_ref 0.1197 _refine_ls_wR_factor_gt 0.1117 _refine_ls_goodness_of_fit_ref 1.076 _refine_ls_restrained_S_all 1.076 _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 P1 P 0.55850(3) 0.169090(18) 0.12275(3) 0.02654(10) Uani 1 1 d . . . Si1 Si 0.30235(3) 0.21143(2) 0.10274(3) 0.02626(10) Uani 1 1 d . . . Si2 Si 0.83034(4) 0.14467(2) 0.17062(4) 0.02722(10) Uani 1 1 d . . . C1 C 0.46066(12) 0.24246(7) 0.12216(12) 0.0238(3) Uani 1 1 d . . . C2 C 0.50187(12) 0.31894(7) 0.13996(12) 0.0243(3) Uani 1 1 d . . . C3 C 0.61893(13) 0.34103(7) 0.15444(12) 0.0262(3) Uani 1 1 d . . . H3 H 0.6376 0.3941 0.1643 0.031 Uiso 1 1 calc R . . C4 C 0.71143(12) 0.29255(7) 0.15580(11) 0.0241(3) Uani 1 1 d . . . C5 C 0.69750(12) 0.21254(7) 0.14485(11) 0.0244(3) Uani 1 1 d . . . C6 C 0.28534(17) 0.10609(9) 0.07787(18) 0.0475(4) Uani 1 1 d . . . H6A H 0.2037 0.0898 0.0686 0.071 Uiso 1 1 calc R . . H6B H 0.3523 0.0800 0.1486 0.071 Uiso 1 1 calc R . . H6C H 0.2910 0.0931 0.0033 0.071 Uiso 1 1 calc R . . C7 C 0.28730(16) 0.23162(10) 0.24348(14) 0.0433(4) Uani 1 1 d . . . H7A H 0.2835 0.2869 0.2533 0.065 Uiso 1 1 calc R . . H7B H 0.3600 0.2106 0.3154 0.065 Uiso 1 1 calc R . . H7C H 0.2105 0.2079 0.2359 0.065 Uiso 1 1 calc R . . C8 C 0.17180(15) 0.25745(10) -0.03317(16) 0.0457(4) Uani 1 1 d . . . H8A H 0.0917 0.2360 -0.0459 0.068 Uiso 1 1 calc R . . H8B H 0.1823 0.2481 -0.1062 0.068 Uiso 1 1 calc R . . H8C H 0.1726 0.3126 -0.0191 0.068 Uiso 1 1 calc R . . C9 C 0.42193(13) 0.38379(7) 0.14280(13) 0.0267(3) Uani 1 1 d . . . C10 C 0.42929(15) 0.40953(8) 0.25178(14) 0.0359(3) Uani 1 1 d . . . H10 H 0.4812 0.3834 0.3261 0.043 Uiso 1 1 calc R . . C11 C 0.36172(15) 0.47314(9) 0.25408(16) 0.0408(4) Uani 1 1 d . . . H11 H 0.3678 0.4902 0.3298 0.049 Uiso 1 1 calc R . . C12 C 0.28619(16) 0.51150(8) 0.14731(18) 0.0423(4) Uani 1 1 d . . . H12 H 0.2399 0.5549 0.1490 0.051 Uiso 1 1 calc R . . C13 C 0.2782(2) 0.48686(11) 0.03919(19) 0.0584(5) Uani 1 1 d . . . H13 H 0.2262 0.5132 -0.0349 0.070 Uiso 1 1 calc R . . C14 C 0.34592(19) 0.42322(10) 0.03654(16) 0.0512(5) Uani 1 1 d . . . H14 H 0.3397 0.4067 -0.0395 0.061 Uiso 1 1 calc R . . C15 C 0.82741(12) 0.33137(7) 0.17058(12) 0.0259(3) Uani 1 1 d . . . C16 C 0.86401(14) 0.32791(8) 0.07947(15) 0.0336(3) Uani 1 1 d . . . H16 H 0.8157 0.2993 0.0068 0.040 Uiso 1 1 calc R . . C17 C 0.97095(17) 0.36610(9) 0.09419(18) 0.0457(4) Uani 1 1 d . . . H17 H 0.9959 0.3633 0.0318 0.055 Uiso 1 1 calc R . . C18 C 1.04098(16) 0.40805(10) 0.1989(2) 0.0530(5) Uani 1 1 d . . . H18 H 1.1145 0.4337 0.2090 0.064 Uiso 1 1 calc R . . C19 C 1.00446(16) 0.41277(10) 0.28908(18) 0.0489(4) Uani 1 1 d . . . H19 H 1.0525 0.4421 0.3610 0.059 Uiso 1 1 calc R . . C20 C 0.89815(14) 0.37502(8) 0.27528(14) 0.0360(3) Uani 1 1 d . . . H20 H 0.8731 0.3788 0.3375 0.043 Uiso 1 1 calc R . . C21 C 0.78400(16) 0.04667(8) 0.19502(15) 0.0388(4) Uani 1 1 d . . . H21A H 0.7099 0.0299 0.1203 0.058 Uiso 1 1 calc R . . H21B H 0.7645 0.0477 0.2637 0.058 Uiso 1 1 calc R . . H21C H 0.8533 0.0111 0.2138 0.058 Uiso 1 1 calc R . . C22 C 0.86237(16) 0.13613(9) 0.03662(15) 0.0396(4) Uani 1 1 d . . . H22A H 0.9114 0.1803 0.0349 0.059 Uiso 1 1 calc R . . H22B H 0.7828 0.1345 -0.0397 0.059 Uiso 1 1 calc R . . H22C H 0.9097 0.0892 0.0444 0.059 Uiso 1 1 calc R . . C23 C 0.97628(14) 0.17412(9) 0.31036(14) 0.0374(3) Uani 1 1 d . . . H23A H 1.0349 0.1311 0.3397 0.056 Uiso 1 1 calc R . . H23B H 0.9553 0.1897 0.3748 0.056 Uiso 1 1 calc R . . H23C H 1.0152 0.2170 0.2899 0.056 Uiso 1 1 calc R . . 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 P1 0.02814(19) 0.02031(17) 0.0335(2) -0.00221(12) 0.01641(16) -0.00031(13) Si1 0.0251(2) 0.02676(19) 0.02799(19) -0.00272(13) 0.01336(16) -0.00267(14) Si2 0.0307(2) 0.02373(18) 0.0302(2) 0.00219(13) 0.01671(17) 0.00590(14) C1 0.0249(6) 0.0236(6) 0.0233(6) -0.0002(4) 0.0117(5) 0.0001(5) C2 0.0256(6) 0.0222(6) 0.0257(6) 0.0009(5) 0.0125(5) 0.0032(5) C3 0.0289(7) 0.0200(6) 0.0303(7) -0.0009(5) 0.0143(6) -0.0009(5) C4 0.0242(6) 0.0255(6) 0.0239(6) -0.0002(5) 0.0123(5) -0.0001(5) C5 0.0267(7) 0.0242(6) 0.0231(6) 0.0002(4) 0.0123(5) 0.0012(5) C6 0.0444(10) 0.0325(8) 0.0729(12) -0.0099(8) 0.0337(9) -0.0110(7) C7 0.0411(9) 0.0579(10) 0.0378(8) -0.0067(7) 0.0241(7) -0.0101(8) C8 0.0316(8) 0.0584(10) 0.0395(9) 0.0029(7) 0.0106(7) 0.0032(7) C9 0.0258(6) 0.0207(6) 0.0359(7) 0.0004(5) 0.0164(6) 0.0006(5) C10 0.0354(8) 0.0345(7) 0.0379(8) -0.0031(6) 0.0171(7) 0.0055(6) C11 0.0436(9) 0.0336(8) 0.0523(10) -0.0086(7) 0.0285(8) 0.0016(7) C12 0.0432(9) 0.0253(7) 0.0721(11) 0.0060(7) 0.0384(9) 0.0078(6) C13 0.0759(14) 0.0489(10) 0.0591(12) 0.0229(8) 0.0389(11) 0.0365(10) C14 0.0704(12) 0.0470(9) 0.0407(9) 0.0129(7) 0.0300(9) 0.0302(9) C15 0.0236(6) 0.0216(6) 0.0331(7) 0.0035(5) 0.0137(6) 0.0024(5) C16 0.0361(8) 0.0286(7) 0.0427(8) 0.0057(6) 0.0240(7) 0.0057(6) C17 0.0433(9) 0.0412(9) 0.0692(12) 0.0139(8) 0.0401(9) 0.0099(7) C18 0.0309(8) 0.0469(10) 0.0838(14) 0.0086(9) 0.0292(9) -0.0032(7) C19 0.0331(9) 0.0428(9) 0.0621(12) -0.0052(8) 0.0152(8) -0.0102(7) C20 0.0320(8) 0.0336(7) 0.0400(8) -0.0020(6) 0.0151(7) -0.0030(6) C21 0.0505(10) 0.0238(7) 0.0481(9) 0.0037(6) 0.0282(8) 0.0077(6) C22 0.0485(9) 0.0382(8) 0.0430(9) 0.0004(6) 0.0304(8) 0.0090(7) C23 0.0333(8) 0.0381(8) 0.0374(8) 0.0048(6) 0.0137(7) 0.0083(6) _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 P1 C1 1.7436(13) . ? P1 C5 1.7445(14) . ? Si1 C8 1.8605(16) . ? Si1 C7 1.8614(16) . ? Si1 C6 1.8655(16) . ? Si1 C1 1.8922(14) . ? Si2 C23 1.8677(16) . ? Si2 C22 1.8713(16) . ? Si2 C21 1.8729(15) . ? Si2 C5 1.9000(13) . ? C1 C2 1.4097(17) . ? C2 C3 1.3943(19) . ? C2 C9 1.5018(18) . ? C3 C4 1.3973(18) . ? C4 C5 1.4101(17) . ? C4 C15 1.4896(18) . ? C9 C10 1.380(2) . ? C9 C14 1.381(2) . ? C10 C11 1.389(2) . ? C11 C12 1.374(2) . ? C12 C13 1.361(3) . ? C13 C14 1.392(2) . ? C15 C16 1.388(2) . ? C15 C20 1.3944(19) . ? C16 C17 1.389(2) . ? C17 C18 1.377(3) . ? C18 C19 1.377(3) . ? C19 C20 1.382(2) . ? 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 C1 P1 C5 106.27(6) . . ? C8 Si1 C7 110.15(8) . . ? C8 Si1 C6 107.40(8) . . ? C7 Si1 C6 106.84(8) . . ? C8 Si1 C1 111.61(7) . . ? C7 Si1 C1 111.29(7) . . ? C6 Si1 C1 109.36(7) . . ? C23 Si2 C22 109.82(8) . . ? C23 Si2 C21 109.20(7) . . ? C22 Si2 C21 105.66(7) . . ? C23 Si2 C5 109.79(6) . . ? C22 Si2 C5 114.27(6) . . ? C21 Si2 C5 107.91(6) . . ? C2 C1 P1 120.69(10) . . ? C2 C1 Si1 123.68(10) . . ? P1 C1 Si1 115.58(7) . . ? C3 C2 C1 123.10(12) . . ? C3 C2 C9 114.32(11) . . ? C1 C2 C9 122.57(12) . . ? C2 C3 C4 126.18(12) . . ? C3 C4 C5 122.94(12) . . ? C3 C4 C15 115.16(11) . . ? C5 C4 C15 121.90(12) . . ? C4 C5 P1 120.75(10) . . ? C4 C5 Si2 123.52(10) . . ? P1 C5 Si2 115.38(7) . . ? C10 C9 C14 118.06(13) . . ? C10 C9 C2 121.45(12) . . ? C14 C9 C2 120.30(13) . . ? C9 C10 C11 120.81(14) . . ? C12 C11 C10 120.31(15) . . ? C13 C12 C11 119.53(14) . . ? C12 C13 C14 120.33(16) . . ? C9 C14 C13 120.96(16) . . ? C16 C15 C20 118.89(13) . . ? C16 C15 C4 121.33(12) . . ? C20 C15 C4 119.71(13) . . ? C15 C16 C17 120.24(15) . . ? C18 C17 C16 120.23(17) . . ? C17 C18 C19 119.99(16) . . ? C18 C19 C20 120.23(16) . . ? C19 C20 C15 120.41(15) . . ? _diffrn_measured_fraction_theta_max 0.996 _diffrn_reflns_theta_full 30.01 _diffrn_measured_fraction_theta_full 0.996 _refine_diff_density_max 0.389 _refine_diff_density_min -0.333 _refine_diff_density_rms 0.051 #END=== data_sulphosph _database_code_depnum_ccdc_archive 'CCDC 637689' #compond 3 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C29 H21 P S' _chemical_formula_sum 'C29 H21 P S' _chemical_formula_weight 432.49 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M 'P212121 ' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' 'x+1/2, -y+1/2, -z' '-x, y+1/2, -z+1/2' _cell_length_a 6.240(1) _cell_length_b 12.986(1) _cell_length_c 27.663(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2241.6(4) _cell_formula_units_Z 4 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 251 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description needle _exptl_crystal_colour 'light yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.09 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.282 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 904 _exptl_absorpt_coefficient_mu 0.230 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9555 _exptl_absorpt_correction_T_max 0.9796 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _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 5058 _diffrn_reflns_av_R_equivalents 0.0000 _diffrn_reflns_av_sigmaI/netI 0.0427 _diffrn_reflns_limit_h_min -8 _diffrn_reflns_limit_h_max 8 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -35 _diffrn_reflns_limit_l_max 35 _diffrn_reflns_theta_min 3.35 _diffrn_reflns_theta_max 27.47 _reflns_number_total 5058 _reflns_number_gt 4217 _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^)+(0.0562P)^2^+0.0501P] 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 SHELXL _refine_ls_extinction_coef 0.0058(12) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.01(6) _refine_ls_number_reflns 5058 _refine_ls_number_parameters 281 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0511 _refine_ls_R_factor_gt 0.0384 _refine_ls_wR_factor_ref 0.0990 _refine_ls_wR_factor_gt 0.0933 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 S1 S -0.14733(9) 1.09552(4) 0.31541(2) 0.04403(16) Uani 1 1 d . . . P1 P -0.02583(8) 0.98072(4) 0.349144(18) 0.03439(14) Uani 1 1 d . . . C1 C -0.0741(3) 0.85328(15) 0.33557(7) 0.0343(4) Uani 1 1 d . . . C2 C 0.0464(3) 0.77863(15) 0.35992(7) 0.0338(4) Uani 1 1 d . . . C3 C 0.1994(3) 0.80180(16) 0.39510(7) 0.0356(5) Uani 1 1 d . . . H3 H 0.2750 0.7452 0.4086 0.043 Uiso 1 1 calc R . . C4 C 0.2534(3) 0.89966(16) 0.41268(7) 0.0338(4) Uani 1 1 d . . . C5 C 0.1578(3) 0.99002(15) 0.39498(7) 0.0332(4) Uani 1 1 d . . . C6 C -0.2325(3) 0.83076(16) 0.29650(7) 0.0349(4) Uani 1 1 d . . . C7 C -0.4358(4) 0.87543(17) 0.29744(8) 0.0404(5) Uani 1 1 d . . . H7 H -0.4761 0.9185 0.3237 0.049 Uiso 1 1 calc R . . C8 C -0.5795(3) 0.85697(18) 0.26000(8) 0.0431(5) Uani 1 1 d . . . H8 H -0.7171 0.8883 0.2606 0.052 Uiso 1 1 calc R . . C9 C -0.5242(3) 0.79398(17) 0.22229(8) 0.0427(5) Uani 1 1 d . . . H9 H -0.6232 0.7818 0.1968 0.051 Uiso 1 1 calc R . . C10 C -0.3244(4) 0.74825(17) 0.22127(8) 0.0435(5) Uani 1 1 d . . . H10 H -0.2873 0.7039 0.1953 0.052 Uiso 1 1 calc R . . C11 C -0.1770(3) 0.76674(16) 0.25804(7) 0.0382(5) Uani 1 1 d . . . H11 H -0.0391 0.7358 0.2569 0.046 Uiso 1 1 calc R . . C12 C 0.0129(3) 0.66597(15) 0.34994(7) 0.0357(4) Uani 1 1 d . . . C13 C -0.1864(4) 0.61984(16) 0.35693(8) 0.0418(5) Uani 1 1 d . . . H13 H -0.3054 0.6605 0.3667 0.050 Uiso 1 1 calc R . . C14 C -0.2116(3) 0.51487(17) 0.34973(8) 0.0462(5) Uani 1 1 d . . . H14 H -0.3471 0.4835 0.3552 0.055 Uiso 1 1 calc R . . C15 C -0.0397(4) 0.45577(17) 0.33464(9) 0.0494(6) Uani 1 1 d . . . H15 H -0.0571 0.3838 0.3299 0.059 Uiso 1 1 calc R . . C16 C 0.1564(4) 0.50109(18) 0.32653(8) 0.0497(6) Uani 1 1 d . . . H16 H 0.2738 0.4610 0.3154 0.060 Uiso 1 1 calc R . . C17 C 0.1811(3) 0.60610(17) 0.33474(8) 0.0429(5) Uani 1 1 d . . . H17 H 0.3173 0.6370 0.3297 0.051 Uiso 1 1 calc R . . C18 C 0.4195(3) 0.90466(15) 0.45183(7) 0.0336(4) Uani 1 1 d . . . C19 C 0.6112(3) 0.85202(16) 0.44616(8) 0.0382(5) Uani 1 1 d . . . H19 H 0.6347 0.8129 0.4176 0.046 Uiso 1 1 calc R . . C20 C 0.7693(4) 0.85549(18) 0.48140(8) 0.0441(5) Uani 1 1 d . . . H20 H 0.8996 0.8188 0.4770 0.053 Uiso 1 1 calc R . . C21 C 0.7365(4) 0.91234(18) 0.52280(8) 0.0462(5) Uani 1 1 d . . . H21 H 0.8460 0.9169 0.5466 0.055 Uiso 1 1 calc R . . C22 C 0.5425(4) 0.96311(17) 0.52972(8) 0.0451(5) Uani 1 1 d . . . H22 H 0.5180 1.0005 0.5587 0.054 Uiso 1 1 calc R . . C23 C 0.3856(4) 0.95946(16) 0.49466(7) 0.0395(5) Uani 1 1 d . . . H23 H 0.2537 0.9944 0.4996 0.047 Uiso 1 1 calc R . . C24 C 0.2152(3) 1.09606(15) 0.41135(7) 0.0336(4) Uani 1 1 d . . . C25 C 0.4167(3) 1.13569(16) 0.40247(7) 0.0381(5) Uani 1 1 d . . . H25 H 0.5203 1.0943 0.3865 0.046 Uiso 1 1 calc R . . C26 C 0.4706(4) 1.23530(17) 0.41652(8) 0.0445(5) Uani 1 1 d . . . H26 H 0.6101 1.2615 0.4104 0.053 Uiso 1 1 calc R . . C27 C 0.3193(4) 1.29567(17) 0.43942(8) 0.0481(6) Uani 1 1 d . . . H27 H 0.3543 1.3640 0.4488 0.058 Uiso 1 1 calc R . . C28 C 0.1163(4) 1.25688(17) 0.44882(9) 0.0500(6) Uani 1 1 d . . . H28 H 0.0133 1.2984 0.4649 0.060 Uiso 1 1 calc R . . C29 C 0.0637(4) 1.15763(17) 0.43472(8) 0.0427(5) Uani 1 1 d . . . H29 H -0.0757 1.1314 0.4410 0.051 Uiso 1 1 calc R . . 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 S1 0.0471(3) 0.0355(3) 0.0495(3) 0.0084(2) -0.0001(3) 0.0048(2) P1 0.0371(3) 0.0295(3) 0.0366(3) 0.0012(2) 0.0013(2) 0.0019(2) C1 0.0359(10) 0.0339(10) 0.0331(10) -0.0022(9) 0.0049(9) 0.0014(8) C2 0.0363(10) 0.0293(10) 0.0359(11) -0.0021(8) 0.0006(9) 0.0003(8) C3 0.0406(11) 0.0300(11) 0.0363(11) 0.0001(9) -0.0011(9) 0.0033(9) C4 0.0365(10) 0.0328(10) 0.0322(10) -0.0014(9) 0.0029(8) 0.0008(9) C5 0.0363(10) 0.0291(10) 0.0341(10) 0.0007(8) 0.0048(8) -0.0007(9) C6 0.0380(10) 0.0316(10) 0.0352(11) 0.0038(9) -0.0009(8) 0.0001(9) C7 0.0410(11) 0.0402(12) 0.0401(11) 0.0029(9) 0.0029(10) -0.0003(9) C8 0.0339(11) 0.0466(13) 0.0488(13) 0.0074(11) -0.0009(9) -0.0010(9) C9 0.0431(12) 0.0376(12) 0.0473(12) 0.0050(10) -0.0101(10) -0.0045(10) C10 0.0571(13) 0.0334(12) 0.0400(12) -0.0027(10) -0.0044(11) -0.0004(10) C11 0.0435(11) 0.0334(11) 0.0376(11) 0.0004(9) -0.0028(9) 0.0031(9) C12 0.0423(11) 0.0290(10) 0.0356(10) -0.0021(9) -0.0073(9) 0.0019(8) C13 0.0438(11) 0.0330(11) 0.0486(13) -0.0032(10) -0.0070(10) 0.0014(9) C14 0.0448(11) 0.0370(11) 0.0568(14) -0.0046(11) -0.0088(10) -0.0060(10) C15 0.0557(13) 0.0300(11) 0.0623(14) -0.0076(10) -0.0192(12) 0.0000(10) C16 0.0512(12) 0.0357(12) 0.0623(15) -0.0130(11) -0.0110(11) 0.0094(11) C17 0.0411(11) 0.0366(11) 0.0509(13) -0.0055(10) -0.0061(10) 0.0020(9) C18 0.0408(10) 0.0271(10) 0.0329(10) 0.0021(9) 0.0000(9) -0.0024(9) C19 0.0454(12) 0.0348(11) 0.0344(11) 0.0030(9) 0.0011(9) -0.0015(9) C20 0.0419(11) 0.0437(13) 0.0468(13) 0.0094(11) -0.0019(10) 0.0000(10) C21 0.0541(13) 0.0427(12) 0.0420(12) 0.0101(11) -0.0127(10) -0.0094(11) C22 0.0637(14) 0.0376(12) 0.0340(11) -0.0013(9) 0.0012(11) -0.0080(11) C23 0.0493(12) 0.0335(12) 0.0357(11) 0.0010(9) 0.0026(10) -0.0003(9) C24 0.0405(10) 0.0280(10) 0.0324(10) 0.0003(9) -0.0006(8) 0.0011(9) C25 0.0401(11) 0.0334(11) 0.0407(12) 0.0000(9) 0.0015(9) 0.0018(9) C26 0.0455(12) 0.0365(12) 0.0514(13) 0.0018(10) -0.0054(11) -0.0047(10) C27 0.0620(14) 0.0285(11) 0.0540(14) -0.0036(10) -0.0092(12) 0.0007(11) C28 0.0574(14) 0.0364(12) 0.0561(14) -0.0071(11) 0.0030(12) 0.0094(11) C29 0.0431(11) 0.0355(12) 0.0495(13) -0.0011(10) 0.0059(10) 0.0048(9) _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 S1 P1 1.9152(8) . ? P1 C5 1.713(2) . ? P1 C1 1.724(2) . ? C1 C2 1.400(3) . ? C1 C6 1.494(3) . ? C2 C3 1.396(3) . ? C2 C12 1.503(3) . ? C3 C4 1.402(3) . ? C4 C5 1.404(3) . ? C4 C18 1.501(3) . ? C5 C24 1.493(3) . ? C6 C11 1.394(3) . ? C6 C7 1.395(3) . ? C7 C8 1.391(3) . ? C8 C9 1.370(3) . ? C9 C10 1.381(3) . ? C10 C11 1.392(3) . ? C12 C17 1.372(3) . ? C12 C13 1.394(3) . ? C13 C14 1.387(3) . ? C14 C15 1.383(3) . ? C15 C16 1.376(3) . ? C16 C17 1.391(3) . ? C18 C19 1.386(3) . ? C18 C23 1.398(3) . ? C19 C20 1.388(3) . ? C20 C21 1.378(3) . ? C21 C22 1.392(3) . ? C22 C23 1.379(3) . ? C24 C25 1.381(3) . ? C24 C29 1.397(3) . ? C25 C26 1.392(3) . ? C26 C27 1.381(3) . ? C27 C28 1.388(3) . ? C28 C29 1.386(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 C5 P1 C1 110.23(10) . . ? C5 P1 S1 124.78(7) . . ? C1 P1 S1 124.89(8) . . ? C2 C1 C6 124.62(18) . . ? C2 C1 P1 117.79(15) . . ? C6 C1 P1 117.48(15) . . ? C3 C2 C1 123.61(18) . . ? C3 C2 C12 115.65(18) . . ? C1 C2 C12 120.73(17) . . ? C2 C3 C4 126.98(19) . . ? C3 C4 C5 122.31(19) . . ? C3 C4 C18 117.10(18) . . ? C5 C4 C18 120.58(17) . . ? C4 C5 C24 124.27(18) . . ? C4 C5 P1 118.89(15) . . ? C24 C5 P1 116.72(14) . . ? C11 C6 C7 119.21(19) . . ? C11 C6 C1 120.31(18) . . ? C7 C6 C1 120.46(18) . . ? C8 C7 C6 120.1(2) . . ? C9 C8 C7 120.5(2) . . ? C8 C9 C10 120.0(2) . . ? C9 C10 C11 120.5(2) . . ? C10 C11 C6 119.8(2) . . ? C17 C12 C13 118.78(18) . . ? C17 C12 C2 120.09(18) . . ? C13 C12 C2 121.11(18) . . ? C14 C13 C12 120.3(2) . . ? C15 C14 C13 120.0(2) . . ? C16 C15 C14 120.1(2) . . ? C15 C16 C17 119.4(2) . . ? C12 C17 C16 121.4(2) . . ? C19 C18 C23 118.52(18) . . ? C19 C18 C4 119.53(17) . . ? C23 C18 C4 121.94(18) . . ? C18 C19 C20 121.18(19) . . ? C21 C20 C19 119.7(2) . . ? C20 C21 C22 119.8(2) . . ? C23 C22 C21 120.3(2) . . ? C22 C23 C18 120.4(2) . . ? C25 C24 C29 119.03(19) . . ? C25 C24 C5 120.53(18) . . ? C29 C24 C5 120.42(18) . . ? C24 C25 C26 121.1(2) . . ? C27 C26 C25 119.4(2) . . ? C26 C27 C28 120.3(2) . . ? C29 C28 C27 120.1(2) . . ? C28 C29 C24 120.2(2) . . ? _diffrn_measured_fraction_theta_max 0.995 _diffrn_reflns_theta_full 27.47 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 0.224 _refine_diff_density_min -0.247 _refine_diff_density_rms 0.041 #END=== data_sulphossiph _database_code_depnum_ccdc_archive 'CCDC 637690' #compound 4 _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H29 P S Si2' _chemical_formula_sum 'C23 H29 P S Si2' _chemical_formula_weight 424.68 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' S S 0.1246 0.1234 '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' _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+1/2, -y+1/2, -z' '-x, y, -z+1/2' '-x, -y, -z' 'x-1/2, y-1/2, -z-1/2' '-x-1/2, y-1/2, z' 'x, -y, z-1/2' _cell_length_a 17.932(1) _cell_length_b 12.292(1) _cell_length_c 20.981(1) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 4624.6(5) _cell_formula_units_Z 8 _cell_measurement_temperature 150.0(1) _cell_measurement_reflns_used 251 _cell_measurement_theta_min 3.0 _cell_measurement_theta_max 20.0 _exptl_crystal_description needle _exptl_crystal_colour 'pale yellow' _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.12 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.220 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1808 _exptl_absorpt_coefficient_mu 0.319 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.9389 _exptl_absorpt_correction_T_max 0.9688 _exptl_absorpt_process_details ? _exptl_special_details ; ? ; _diffrn_ambient_temperature 150.0(1) _diffrn_radiation_wavelength 0.71069 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'fine-focus sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type KappaCCD _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 19073 _diffrn_reflns_av_R_equivalents 0.0267 _diffrn_reflns_av_sigmaI/netI 0.0277 _diffrn_reflns_limit_h_min -23 _diffrn_reflns_limit_h_max 21 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -27 _diffrn_reflns_limit_l_max 27 _diffrn_reflns_theta_min 2.99 _diffrn_reflns_theta_max 27.45 _reflns_number_total 5271 _reflns_number_gt 4326 _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^)+(0.0598P)^2^+0.9132P] 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 5271 _refine_ls_number_parameters 279 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0430 _refine_ls_R_factor_gt 0.0332 _refine_ls_wR_factor_ref 0.0998 _refine_ls_wR_factor_gt 0.0940 _refine_ls_goodness_of_fit_ref 1.045 _refine_ls_restrained_S_all 1.045 _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 S1 S -0.38794(2) 0.30268(4) 0.33811(2) 0.03744(12) Uani 1 1 d . . . P1 P -0.28112(2) 0.30965(3) 0.327941(18) 0.02432(11) Uani 1 1 d . . . Si1 Si -0.25235(2) 0.15332(3) 0.444091(19) 0.02505(11) Uani 1 1 d . . . Si2 Si -0.30463(2) 0.45162(3) 0.207022(19) 0.02516(11) Uani 1 1 d . . . C1 C -0.21820(8) 0.24981(12) 0.37876(7) 0.0237(3) Uani 1 1 d . . . C2 C -0.14227(8) 0.27360(11) 0.36635(7) 0.0234(3) Uani 1 1 d . . . C3 C -0.11681(8) 0.33147(12) 0.31319(7) 0.0241(3) Uani 1 1 d . . . H3 H -0.0644 0.3403 0.3091 0.024(4) Uiso 1 1 calc R . . C4 C -0.16118(8) 0.37754(12) 0.26557(7) 0.0234(3) Uani 1 1 d . . . C5 C -0.23989(8) 0.37947(12) 0.26622(7) 0.0239(3) Uani 1 1 d . . . C6 C -0.33620(10) 0.07509(15) 0.41818(10) 0.0441(5) Uani 1 1 d . . . H6A H -0.3445 0.0142 0.4475 0.066(7) Uiso 1 1 calc R . . H6B H -0.3283 0.0471 0.3750 0.076(8) Uiso 1 1 calc R . . H6C H -0.3799 0.1229 0.4185 0.086(9) Uiso 1 1 calc R . . C7 C -0.27573(10) 0.23561(15) 0.51596(8) 0.0349(4) Uani 1 1 d . . . H7A H -0.2909 0.1871 0.5507 0.062(7) Uiso 1 1 calc R . . H7B H -0.3167 0.2854 0.5059 0.057(6) Uiso 1 1 calc R . . H7C H -0.2319 0.2776 0.5291 0.052(6) Uiso 1 1 calc R . . C8 C -0.18237(9) 0.04599(13) 0.46344(9) 0.0349(4) Uani 1 1 d . . . H8A H -0.1409 0.0784 0.4872 0.053(6) Uiso 1 1 calc R . . H8B H -0.1635 0.0137 0.4239 0.053(6) Uiso 1 1 calc R . . H8C H -0.2059 -0.0106 0.4895 0.061(6) Uiso 1 1 calc R . . C9 C -0.08362(8) 0.23442(12) 0.41155(7) 0.0236(3) Uani 1 1 d . . . C10 C -0.08098(8) 0.27280(12) 0.47403(7) 0.0262(3) Uani 1 1 d . . . H10 H -0.1156 0.3265 0.4877 0.035(5) Uiso 1 1 calc R . . C11 C -0.02819(9) 0.23319(13) 0.51637(7) 0.0293(3) Uani 1 1 d . . . H11 H -0.0270 0.2597 0.5589 0.036(5) Uiso 1 1 calc R . . C12 C 0.02277(9) 0.15521(13) 0.49702(8) 0.0313(3) Uani 1 1 d . . . H12 H 0.0580 0.1266 0.5265 0.035(5) Uiso 1 1 calc R . . C13 C 0.02208(9) 0.11913(13) 0.43441(8) 0.0321(3) Uani 1 1 d . . . H13 H 0.0576 0.0669 0.4206 0.039(5) Uiso 1 1 calc R . . C14 C -0.03048(8) 0.15915(12) 0.39173(7) 0.0283(3) Uani 1 1 d . . . H14 H -0.0301 0.1350 0.3487 0.031(4) Uiso 1 1 calc R . . C15 C -0.11937(8) 0.42482(12) 0.21037(7) 0.0234(3) Uani 1 1 d . . . C16 C -0.08588(9) 0.52648(13) 0.21393(8) 0.0321(3) Uani 1 1 d . . . H16 H -0.0902 0.5686 0.2517 0.043(5) Uiso 1 1 calc R . . C17 C -0.04608(10) 0.56658(14) 0.16225(8) 0.0360(4) Uani 1 1 d . . . H17 H -0.0235 0.6363 0.1648 0.049(6) Uiso 1 1 calc R . . C18 C -0.03917(9) 0.50576(14) 0.10724(8) 0.0337(4) Uani 1 1 d . . . H18 H -0.0122 0.5339 0.0719 0.046(5) Uiso 1 1 calc R . . C19 C -0.07150(9) 0.40412(13) 0.10359(8) 0.0316(3) Uani 1 1 d . . . H19 H -0.0666 0.3620 0.0659 0.047(5) Uiso 1 1 calc R . . C20 C -0.11126(8) 0.36350(13) 0.15509(7) 0.0278(3) Uani 1 1 d . . . H20 H -0.1331 0.2932 0.1526 0.034(5) Uiso 1 1 calc R . . C21 C -0.36717(11) 0.54615(15) 0.25132(9) 0.0441(4) Uani 1 1 d . . . H21A H -0.3370 0.5989 0.2750 0.103(10) Uiso 1 1 calc R . . H21B H -0.3981 0.5045 0.2812 0.125(12) Uiso 1 1 calc R . . H21C H -0.3994 0.5847 0.2211 0.091(9) Uiso 1 1 calc R . . C22 C -0.25617(10) 0.53984(16) 0.14759(9) 0.0440(5) Uani 1 1 d . . . H22A H -0.2222 0.4954 0.1219 0.074(7) Uiso 1 1 calc R . . H22B H -0.2277 0.5962 0.1700 0.062(7) Uiso 1 1 calc R . . H22C H -0.2932 0.5742 0.1198 0.064(7) Uiso 1 1 calc R . . C23 C -0.35919(12) 0.34667(15) 0.16359(9) 0.0435(5) Uani 1 1 d . . . H23A H -0.3939 0.3823 0.1341 0.079(8) Uiso 1 1 calc R . . H23B H -0.3873 0.3026 0.1942 0.088(9) Uiso 1 1 calc R . . H23C H -0.3251 0.2997 0.1395 0.088(9) Uiso 1 1 calc R . . 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 S1 0.0222(2) 0.0513(3) 0.0389(2) 0.0094(2) 0.00250(16) -0.00065(17) P1 0.0217(2) 0.0283(2) 0.02292(19) 0.00182(15) 0.00028(14) 0.00002(15) Si1 0.0266(2) 0.0229(2) 0.0256(2) 0.00255(15) 0.00150(16) -0.00216(16) Si2 0.0267(2) 0.0251(2) 0.0237(2) 0.00002(16) -0.00271(16) 0.00305(16) C1 0.0272(7) 0.0231(7) 0.0207(7) -0.0013(6) -0.0002(6) -0.0009(6) C2 0.0265(7) 0.0210(7) 0.0229(7) -0.0012(5) -0.0010(6) 0.0006(6) C3 0.0214(7) 0.0261(7) 0.0248(7) -0.0004(6) -0.0004(6) -0.0008(6) C4 0.0254(7) 0.0220(7) 0.0226(7) -0.0011(6) 0.0001(6) -0.0007(6) C5 0.0254(7) 0.0242(7) 0.0221(7) 0.0000(6) -0.0008(6) 0.0004(6) C6 0.0402(10) 0.0372(10) 0.0550(12) 0.0081(9) -0.0072(8) -0.0150(8) C7 0.0393(9) 0.0361(9) 0.0293(8) 0.0014(7) 0.0071(7) 0.0016(7) C8 0.0368(9) 0.0250(8) 0.0427(9) 0.0068(7) 0.0028(8) -0.0002(7) C9 0.0233(7) 0.0229(7) 0.0245(7) 0.0040(6) -0.0011(6) -0.0024(6) C10 0.0275(7) 0.0247(7) 0.0262(7) 0.0008(6) 0.0013(6) -0.0009(6) C11 0.0336(8) 0.0313(8) 0.0229(7) 0.0033(6) -0.0035(6) -0.0059(7) C12 0.0298(8) 0.0313(8) 0.0328(8) 0.0083(7) -0.0082(7) -0.0017(6) C13 0.0283(8) 0.0294(8) 0.0386(9) 0.0016(7) -0.0017(7) 0.0039(6) C14 0.0285(8) 0.0291(8) 0.0271(8) -0.0019(6) -0.0005(6) 0.0004(6) C15 0.0221(7) 0.0260(7) 0.0222(7) 0.0027(6) -0.0003(5) 0.0009(6) C16 0.0361(8) 0.0320(8) 0.0280(8) -0.0005(7) -0.0008(7) -0.0054(7) C17 0.0367(9) 0.0328(8) 0.0387(9) 0.0063(7) 0.0001(7) -0.0099(7) C18 0.0279(8) 0.0414(9) 0.0318(8) 0.0112(7) 0.0057(6) 0.0012(7) C19 0.0331(8) 0.0354(8) 0.0263(8) 0.0013(6) 0.0041(6) 0.0053(7) C20 0.0299(8) 0.0255(8) 0.0281(8) 0.0010(6) 0.0002(6) 0.0009(6) C21 0.0501(11) 0.0407(10) 0.0416(10) -0.0041(8) 0.0021(9) 0.0186(9) C22 0.0352(9) 0.0509(11) 0.0459(10) 0.0230(9) -0.0008(8) 0.0071(8) C23 0.0545(12) 0.0368(10) 0.0392(10) -0.0024(8) -0.0190(9) -0.0029(9) _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 S1 P1 1.9293(6) . ? P1 C1 1.7178(15) . ? P1 C5 1.7204(15) . ? Si1 C7 1.8636(17) . ? Si1 C8 1.8655(17) . ? Si1 C6 1.8658(17) . ? Si1 C1 1.9132(15) . ? Si2 C23 1.8579(18) . ? Si2 C21 1.8633(17) . ? Si2 C22 1.8670(18) . ? Si2 C5 1.9177(15) . ? C1 C2 1.417(2) . ? C2 C3 1.400(2) . ? C2 C9 1.496(2) . ? C3 C4 1.397(2) . ? C4 C5 1.412(2) . ? C4 C15 1.497(2) . ? C9 C14 1.392(2) . ? C9 C10 1.394(2) . ? C10 C11 1.386(2) . ? C11 C12 1.385(2) . ? C12 C13 1.387(2) . ? C13 C14 1.390(2) . ? C15 C16 1.388(2) . ? C15 C20 1.391(2) . ? C16 C17 1.389(2) . ? C17 C18 1.381(2) . ? C18 C19 1.379(2) . ? C19 C20 1.387(2) . ? 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 C1 P1 C5 113.48(7) . . ? C1 P1 S1 124.36(5) . . ? C5 P1 S1 122.15(5) . . ? C7 Si1 C8 111.05(8) . . ? C7 Si1 C6 109.53(9) . . ? C8 Si1 C6 103.95(8) . . ? C7 Si1 C1 108.37(7) . . ? C8 Si1 C1 112.27(7) . . ? C6 Si1 C1 111.63(8) . . ? C23 Si2 C21 111.15(10) . . ? C23 Si2 C22 108.71(9) . . ? C21 Si2 C22 104.54(9) . . ? C23 Si2 C5 108.38(7) . . ? C21 Si2 C5 109.25(8) . . ? C22 Si2 C5 114.80(7) . . ? C2 C1 P1 115.39(11) . . ? C2 C1 Si1 124.55(11) . . ? P1 C1 Si1 120.00(8) . . ? C3 C2 C1 124.39(13) . . ? C3 C2 C9 116.08(13) . . ? C1 C2 C9 119.52(12) . . ? C4 C3 C2 126.18(14) . . ? C3 C4 C5 124.69(13) . . ? C3 C4 C15 115.18(12) . . ? C5 C4 C15 120.11(13) . . ? C4 C5 P1 115.38(11) . . ? C4 C5 Si2 127.35(11) . . ? P1 C5 Si2 117.26(8) . . ? C14 C9 C10 118.86(14) . . ? C14 C9 C2 120.40(13) . . ? C10 C9 C2 120.74(13) . . ? C11 C10 C9 120.46(14) . . ? C12 C11 C10 120.38(14) . . ? C11 C12 C13 119.54(14) . . ? C12 C13 C14 120.21(15) . . ? C13 C14 C9 120.47(15) . . ? C16 C15 C20 119.16(14) . . ? C16 C15 C4 121.63(13) . . ? C20 C15 C4 119.15(13) . . ? C15 C16 C17 119.99(15) . . ? C18 C17 C16 120.45(15) . . ? C19 C18 C17 119.94(15) . . ? C18 C19 C20 119.91(15) . . ? C19 C20 C15 120.54(14) . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 27.45 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.274 _refine_diff_density_min -0.340 _refine_diff_density_rms 0.048 #END===