Supplementary Material (ESI) for Dalton Transactions This journal is (c) The Royal Society of Chemistry 2007 data_global _journal_name_full 'Dalton Trans.' _journal_coden_Cambridge 0222 _publ_contact_author_name 'Hans-Wolfram Lerner' _publ_contact_author_address ; Institut fuer Anorganische Chemie Universitaet Frankfurt Max-von-Laue-Str.7 Frankfurt D-60438 GERMANY ; _publ_contact_author_email LERNER@CHEMIE.UNI-FRANKFURT.DE _publ_section_title ; Isoelectronic Caesium Compounds: The Triphosphenide Cs[tBu3SiPPPSitBu3] and the Enolate Cs[OCH=CH2] ; loop_ _publ_author_name 'Hans-Wolfram Lerner' 'Michael Bolte' 'Andreas Lorbach' 'Ingebororg Sanger' 'Frauke Schodel' 'Matthias Wagner' data_wa343 _database_code_depnum_ccdc_archive 'CCDC 648996' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C2 H3 Cs O' _chemical_formula_weight 175.95 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' Cs Cs -0.3680 2.1192 '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' _symmetry_cell_setting Orthorhombic _symmetry_space_group_name_H-M Pnma loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z' 'x+1/2, -y+1/2, -z+1/2' '-x, -y, -z' 'x-1/2, y, -z-1/2' 'x, -y-1/2, z' '-x-1/2, y-1/2, z-1/2' _cell_length_a 7.9917(11) _cell_length_b 5.6041(9) _cell_length_c 8.5828(13) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 384.39(10) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 9962 _cell_measurement_theta_min 4.2 _cell_measurement_theta_max 27.6 _exptl_crystal_description block _exptl_crystal_colour 'pale brown' _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.11 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 3.040 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 312 _exptl_absorpt_coefficient_mu 9.404 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.1782 _exptl_absorpt_correction_T_max 0.4244 _exptl_absorpt_process_details 'MULABS (Spek, 1990; Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 4426 _diffrn_reflns_av_R_equivalents 0.0647 _diffrn_reflns_av_sigmaI/netI 0.0257 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -7 _diffrn_reflns_limit_k_max 7 _diffrn_reflns_limit_l_min -11 _diffrn_reflns_limit_l_max 10 _diffrn_reflns_theta_min 4.34 _diffrn_reflns_theta_max 27.59 _reflns_number_total 491 _reflns_number_gt 486 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS97 (Sheldrick, 1990) ' _computing_structure_refinement 'SHELXL97 (Sheldrick, 1997) ' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _computing_publication_material SHELXL97 _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^)+(0.0382P)^2^+0.3361P] 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 mixed _refine_ls_extinction_method SHELXL _refine_ls_extinction_coef 0.033(3) _refine_ls_extinction_expression Fc^*^=kFc[1+0.001xFc^2^\l^3^/sin(2\q)]^-1/4^ _refine_ls_number_reflns 491 _refine_ls_number_parameters 26 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0253 _refine_ls_R_factor_gt 0.0250 _refine_ls_wR_factor_ref 0.0639 _refine_ls_wR_factor_gt 0.0637 _refine_ls_goodness_of_fit_ref 1.183 _refine_ls_restrained_S_all 1.183 _refine_ls_shift/su_max 0.000 _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 Cs1 Cs 0.13314(3) 0.7500 0.35942(4) 0.0243(2) Uani 1 2 d S . . O1 O 0.2155(4) 0.2500 0.5193(4) 0.0302(7) Uani 1 2 d S . . C1 C 0.3567(5) 0.2500 0.4470(8) 0.0267(12) Uani 1 2 d S . . H1 H 0.4540 0.2500 0.5106 0.032 Uiso 1 2 calc SR . . C2 C 0.3830(6) 0.2500 0.2916(8) 0.0293(11) Uani 1 2 d S . . H2A H 0.2906 0.2500 0.2220 0.035 Uiso 1 2 calc SR . . H2B H 0.4940 0.2500 0.2519 0.035 Uiso 1 2 calc SR . . 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 Cs1 0.0187(3) 0.0283(3) 0.0258(3) 0.000 0.00256(8) 0.000 O1 0.0228(15) 0.0403(17) 0.0276(16) 0.000 0.0033(13) 0.000 C1 0.020(2) 0.029(3) 0.031(3) 0.000 -0.0010(17) 0.000 C2 0.026(2) 0.032(3) 0.030(3) 0.000 0.0065(16) 0.000 _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 Cs1 O1 2.974(3) 5_566 ? Cs1 O1 3.160(3) 2_564 ? Cs1 O1 3.1885(17) . ? Cs1 O1 3.1885(17) 1_565 ? Cs1 C1 3.407(3) 1_565 ? Cs1 C1 3.407(3) . ? Cs1 C2 3.490(3) 1_565 ? Cs1 C2 3.490(3) . ? Cs1 C1 3.541(7) 2_564 ? Cs1 C2 3.678(3) 6_556 ? Cs1 C2 3.678(3) 6_566 ? Cs1 C2 3.712(7) 2_565 ? O1 C1 1.288(6) . ? O1 Cs1 2.974(3) 5_566 ? O1 Cs1 3.160(3) 2_565 ? O1 Cs1 3.1884(17) 1_545 ? C1 C2 1.350(11) . ? C1 Cs1 3.407(3) 1_545 ? C1 Cs1 3.541(7) 2_565 ? C1 H1 0.9500 . ? C2 Cs1 3.490(3) 1_545 ? C2 Cs1 3.678(3) 6_656 ? C2 Cs1 3.678(3) 6_646 ? C2 Cs1 3.712(7) 2_564 ? C2 H2A 0.9500 . ? C2 H2B 0.9500 . ? 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 Cs1 O1 133.00(9) 5_566 2_564 ? O1 Cs1 O1 92.44(7) 5_566 . ? O1 Cs1 O1 108.57(4) 2_564 . ? O1 Cs1 O1 92.44(7) 5_566 1_565 ? O1 Cs1 O1 108.57(4) 2_564 1_565 ? O1 Cs1 O1 123.00(11) . 1_565 ? O1 Cs1 C1 114.45(9) 5_566 1_565 ? O1 Cs1 C1 90.17(12) 2_564 1_565 ? O1 Cs1 C1 121.31(11) . 1_565 ? O1 Cs1 C1 22.20(11) 1_565 1_565 ? O1 Cs1 C1 114.45(9) 5_566 . ? O1 Cs1 C1 90.17(12) 2_564 . ? O1 Cs1 C1 22.20(11) . . ? O1 Cs1 C1 121.31(11) 1_565 . ? C1 Cs1 C1 110.66(13) 1_565 . ? O1 Cs1 C2 126.47(6) 5_566 1_565 ? O1 Cs1 C2 68.09(11) 2_564 1_565 ? O1 Cs1 C2 131.25(10) . 1_565 ? O1 Cs1 C2 41.24(11) 1_565 1_565 ? C1 Cs1 C2 22.54(18) 1_565 1_565 ? C1 Cs1 C2 113.40(9) . 1_565 ? O1 Cs1 C2 126.47(6) 5_566 . ? O1 Cs1 C2 68.09(11) 2_564 . ? O1 Cs1 C2 41.24(11) . . ? O1 Cs1 C2 131.25(10) 1_565 . ? C1 Cs1 C2 113.40(9) 1_565 . ? C1 Cs1 C2 22.54(18) . . ? C2 Cs1 C2 106.82(12) 1_565 . ? O1 Cs1 C1 111.81(10) 5_566 2_564 ? O1 Cs1 C1 21.19(9) 2_564 2_564 ? O1 Cs1 C1 115.18(6) . 2_564 ? O1 Cs1 C1 115.18(6) 1_565 2_564 ? C1 Cs1 C1 102.03(12) 1_565 2_564 ? C1 Cs1 C1 102.03(12) . 2_564 ? C2 Cs1 C1 79.64(12) 1_565 2_564 ? C2 Cs1 C1 79.64(12) . 2_564 ? O1 Cs1 C2 67.31(9) 5_566 6_556 ? O1 Cs1 C2 83.25(11) 2_564 6_556 ? O1 Cs1 C2 66.06(9) . 6_556 ? O1 Cs1 C2 158.96(9) 1_565 6_556 ? C1 Cs1 C2 171.61(17) 1_565 6_556 ? C1 Cs1 C2 74.70(9) . 6_556 ? C2 Cs1 C2 149.762(17) 1_565 6_556 ? C2 Cs1 C2 68.93(3) . 6_556 ? C1 Cs1 C2 70.13(11) 2_564 6_556 ? O1 Cs1 C2 67.31(9) 5_566 6_566 ? O1 Cs1 C2 83.25(11) 2_564 6_566 ? O1 Cs1 C2 158.96(9) . 6_566 ? O1 Cs1 C2 66.06(9) 1_565 6_566 ? C1 Cs1 C2 74.70(9) 1_565 6_566 ? C1 Cs1 C2 171.61(17) . 6_566 ? C2 Cs1 C2 68.93(3) 1_565 6_566 ? C2 Cs1 C2 149.762(17) . 6_566 ? C1 Cs1 C2 70.13(11) 2_564 6_566 ? C2 Cs1 C2 99.26(12) 6_556 6_566 ? O1 Cs1 C2 67.51(10) 5_566 2_565 ? O1 Cs1 C2 159.48(9) 2_564 2_565 ? O1 Cs1 C2 64.99(6) . 2_565 ? O1 Cs1 C2 64.99(6) 1_565 2_565 ? C1 Cs1 C2 78.33(12) 1_565 2_565 ? C1 Cs1 C2 78.33(12) . 2_565 ? C2 Cs1 C2 100.76(12) 1_565 2_565 ? C2 Cs1 C2 100.76(11) . 2_565 ? C1 Cs1 C2 179.32(10) 2_564 2_565 ? C2 Cs1 C2 109.47(10) 6_556 2_565 ? C2 Cs1 C2 109.47(10) 6_566 2_565 ? C1 O1 Cs1 171.7(4) . 5_566 ? C1 O1 Cs1 96.3(3) . 2_565 ? Cs1 O1 Cs1 92.02(9) 5_566 2_565 ? C1 O1 Cs1 88.49(16) . 1_545 ? Cs1 O1 Cs1 87.56(7) 5_566 1_545 ? Cs1 O1 Cs1 118.45(5) 2_565 1_545 ? C1 O1 Cs1 88.49(16) . . ? Cs1 O1 Cs1 87.56(7) 5_566 . ? Cs1 O1 Cs1 118.45(5) 2_565 . ? Cs1 O1 Cs1 123.00(11) 1_545 . ? O1 C1 C2 127.8(5) . . ? O1 C1 Cs1 69.31(13) . 1_545 ? C2 C1 Cs1 82.2(2) . 1_545 ? O1 C1 Cs1 69.31(13) . . ? C2 C1 Cs1 82.2(2) . . ? Cs1 C1 Cs1 110.66(13) 1_545 . ? O1 C1 Cs1 62.5(3) . 2_565 ? C2 C1 Cs1 169.7(3) . 2_565 ? Cs1 C1 Cs1 103.45(13) 1_545 2_565 ? Cs1 C1 Cs1 103.45(13) . 2_565 ? O1 C1 H1 116.1 . . ? C2 C1 H1 116.1 . . ? Cs1 C1 H1 123.8 1_545 . ? Cs1 C1 H1 123.8 . . ? Cs1 C1 H1 53.6 2_565 . ? C1 C2 Cs1 75.29(16) . 1_545 ? C1 C2 Cs1 75.29(16) . . ? Cs1 C2 Cs1 106.82(12) 1_545 . ? C1 C2 Cs1 115.6(2) . 6_656 ? Cs1 C2 Cs1 169.0(2) 1_545 6_656 ? Cs1 C2 Cs1 76.00(2) . 6_656 ? C1 C2 Cs1 115.6(2) . 6_646 ? Cs1 C2 Cs1 76.00(2) 1_545 6_646 ? Cs1 C2 Cs1 169.0(2) . 6_646 ? Cs1 C2 Cs1 99.26(12) 6_656 6_646 ? C1 C2 Cs1 169.0(3) . 2_564 ? Cs1 C2 Cs1 98.44(12) 1_545 2_564 ? Cs1 C2 Cs1 98.44(12) . 2_564 ? Cs1 C2 Cs1 70.53(10) 6_656 2_564 ? Cs1 C2 Cs1 70.53(10) 6_646 2_564 ? C1 C2 H2A 120.0 . . ? Cs1 C2 H2A 70.1 1_545 . ? Cs1 C2 H2A 70.1 . . ? Cs1 C2 H2A 101.6 6_656 . ? Cs1 C2 H2A 101.6 6_646 . ? Cs1 C2 H2A 49.0 2_564 . ? C1 C2 H2B 120.0 . . ? Cs1 C2 H2B 126.4 1_545 . ? Cs1 C2 H2B 126.4 . . ? Cs1 C2 H2B 50.7 6_656 . ? Cs1 C2 H2B 50.7 6_646 . ? Cs1 C2 H2B 71.0 2_564 . ? H2A C2 H2B 120.0 . . ? 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 Cs1 O1 C1 172.7(3) 5_566 . . . ? O1 Cs1 O1 C1 35.4(3) 2_564 . . . ? O1 Cs1 O1 C1 -92.8(3) 1_565 . . . ? C1 Cs1 O1 C1 -66.6(2) 1_565 . . . ? C2 Cs1 O1 C1 -41.3(4) 1_565 . . . ? C2 Cs1 O1 C1 24.1(3) . . . . ? C1 Cs1 O1 C1 57.2(3) 2_564 . . . ? C2 Cs1 O1 C1 108.9(3) 6_556 . . . ? C2 Cs1 O1 C1 157.3(4) 6_566 . . . ? C2 Cs1 O1 C1 -123.6(3) 2_565 . . . ? O1 Cs1 O1 Cs1 0.000(1) 5_566 . . 5_566 ? O1 Cs1 O1 Cs1 -137.27(6) 2_564 . . 5_566 ? O1 Cs1 O1 Cs1 94.51(12) 1_565 . . 5_566 ? C1 Cs1 O1 Cs1 120.72(13) 1_565 . . 5_566 ? C1 Cs1 O1 Cs1 -172.7(3) . . . 5_566 ? C2 Cs1 O1 Cs1 145.97(14) 1_565 . . 5_566 ? C2 Cs1 O1 Cs1 -148.63(17) . . . 5_566 ? C1 Cs1 O1 Cs1 -115.53(9) 2_564 . . 5_566 ? C2 Cs1 O1 Cs1 -63.81(12) 6_556 . . 5_566 ? C2 Cs1 O1 Cs1 -15.4(3) 6_566 . . 5_566 ? C2 Cs1 O1 Cs1 63.74(9) 2_565 . . 5_566 ? O1 Cs1 O1 Cs1 -90.97(11) 5_566 . . 2_565 ? O1 Cs1 O1 Cs1 131.76(15) 2_564 . . 2_565 ? O1 Cs1 O1 Cs1 3.5(2) 1_565 . . 2_565 ? C1 Cs1 O1 Cs1 29.75(19) 1_565 . . 2_565 ? C1 Cs1 O1 Cs1 96.3(3) . . . 2_565 ? C2 Cs1 O1 Cs1 55.0(2) 1_565 . . 2_565 ? C2 Cs1 O1 Cs1 120.4(2) . . . 2_565 ? C1 Cs1 O1 Cs1 153.50(11) 2_564 . . 2_565 ? C2 Cs1 O1 Cs1 -154.78(17) 6_556 . . 2_565 ? C2 Cs1 O1 Cs1 -106.4(3) 6_566 . . 2_565 ? C2 Cs1 O1 Cs1 -27.23(11) 2_565 . . 2_565 ? O1 Cs1 O1 Cs1 85.49(12) 5_566 . . 1_545 ? O1 Cs1 O1 Cs1 -51.77(7) 2_564 . . 1_545 ? O1 Cs1 O1 Cs1 180.0 1_565 . . 1_545 ? C1 Cs1 O1 Cs1 -153.79(14) 1_565 . . 1_545 ? C1 Cs1 O1 Cs1 -87.2(3) . . . 1_545 ? C2 Cs1 O1 Cs1 -128.54(16) 1_565 . . 1_545 ? C2 Cs1 O1 Cs1 -63.14(16) . . . 1_545 ? C1 Cs1 O1 Cs1 -30.04(15) 2_564 . . 1_545 ? C2 Cs1 O1 Cs1 21.68(13) 6_556 . . 1_545 ? C2 Cs1 O1 Cs1 70.1(3) 6_566 . . 1_545 ? C2 Cs1 O1 Cs1 149.24(15) 2_565 . . 1_545 ? Cs1 O1 C1 C2 0.000(5) 5_566 . . . ? Cs1 O1 C1 C2 180.000(1) 2_565 . . . ? Cs1 O1 C1 C2 61.54(5) 1_545 . . . ? Cs1 O1 C1 C2 -61.54(5) . . . . ? Cs1 O1 C1 Cs1 -61.54(5) 5_566 . . 1_545 ? Cs1 O1 C1 Cs1 118.46(5) 2_565 . . 1_545 ? Cs1 O1 C1 Cs1 -123.07(11) . . . 1_545 ? Cs1 O1 C1 Cs1 61.54(5) 5_566 . . . ? Cs1 O1 C1 Cs1 -118.46(5) 2_565 . . . ? Cs1 O1 C1 Cs1 123.07(11) 1_545 . . . ? Cs1 O1 C1 Cs1 180.000(5) 5_566 . . 2_565 ? Cs1 O1 C1 Cs1 -118.46(5) 1_545 . . 2_565 ? Cs1 O1 C1 Cs1 118.46(5) . . . 2_565 ? O1 Cs1 C1 O1 -8.0(3) 5_566 . . . ? O1 Cs1 C1 O1 -146.7(3) 2_564 . . . ? O1 Cs1 C1 O1 101.3(3) 1_565 . . . ? C1 Cs1 C1 O1 123.09(19) 1_565 . . . ? C2 Cs1 C1 O1 147.3(3) 1_565 . . . ? C2 Cs1 C1 O1 -135.4(4) . . . . ? C1 Cs1 C1 O1 -129.0(3) 2_564 . . . ? C2 Cs1 C1 O1 -63.7(3) 6_556 . . . ? C2 Cs1 C1 O1 -108.3(8) 6_566 . . . ? C2 Cs1 C1 O1 50.5(3) 2_565 . . . ? O1 Cs1 C1 C2 127.4(2) 5_566 . . . ? O1 Cs1 C1 C2 -11.2(2) 2_564 . . . ? O1 Cs1 C1 C2 135.4(4) . . . . ? O1 Cs1 C1 C2 -123.2(2) 1_565 . . . ? C1 Cs1 C1 C2 -101.5(3) 1_565 . . . ? C2 Cs1 C1 C2 -77.3(2) 1_565 . . . ? C1 Cs1 C1 C2 6.5(2) 2_564 . . . ? C2 Cs1 C1 C2 71.75(19) 6_556 . . . ? C2 Cs1 C1 C2 27.1(7) 6_566 . . . ? C2 Cs1 C1 C2 -174.1(2) 2_565 . . . ? O1 Cs1 C1 Cs1 48.9(2) 5_566 . . 1_545 ? O1 Cs1 C1 Cs1 -89.75(17) 2_564 . . 1_545 ? O1 Cs1 C1 Cs1 56.91(19) . . . 1_545 ? O1 Cs1 C1 Cs1 158.25(12) 1_565 . . 1_545 ? C1 Cs1 C1 Cs1 180.0 1_565 . . 1_545 ? C2 Cs1 C1 Cs1 -155.84(18) 1_565 . . 1_545 ? C2 Cs1 C1 Cs1 -78.5(3) . . . 1_545 ? C1 Cs1 C1 Cs1 -72.05(16) 2_564 . . 1_545 ? C2 Cs1 C1 Cs1 -6.79(19) 6_556 . . 1_545 ? C2 Cs1 C1 Cs1 -51.4(8) 6_566 . . 1_545 ? C2 Cs1 C1 Cs1 107.37(18) 2_565 . . 1_545 ? O1 Cs1 C1 Cs1 -61.33(12) 5_566 . . 2_565 ? O1 Cs1 C1 Cs1 160.03(9) 2_564 . . 2_565 ? O1 Cs1 C1 Cs1 -53.3(3) . . . 2_565 ? O1 Cs1 C1 Cs1 48.03(14) 1_565 . . 2_565 ? C1 Cs1 C1 Cs1 69.8(2) 1_565 . . 2_565 ? C2 Cs1 C1 Cs1 93.94(15) 1_565 . . 2_565 ? C2 Cs1 C1 Cs1 171.2(3) . . . 2_565 ? C1 Cs1 C1 Cs1 177.72(12) 2_564 . . 2_565 ? C2 Cs1 C1 Cs1 -117.02(14) 6_556 . . 2_565 ? C2 Cs1 C1 Cs1 -161.7(7) 6_566 . . 2_565 ? C2 Cs1 C1 Cs1 -2.86(9) 2_565 . . 2_565 ? O1 C1 C2 Cs1 -56.11(5) . . . 1_545 ? Cs1 C1 C2 Cs1 -112.23(9) . . . 1_545 ? Cs1 C1 C2 Cs1 123.89(5) 2_565 . . 1_545 ? O1 C1 C2 Cs1 56.11(5) . . . . ? Cs1 C1 C2 Cs1 112.23(9) 1_545 . . . ? Cs1 C1 C2 Cs1 -123.89(5) 2_565 . . . ? O1 C1 C2 Cs1 122.31(18) . . . 6_656 ? Cs1 C1 C2 Cs1 178.43(18) 1_545 . . 6_656 ? Cs1 C1 C2 Cs1 66.20(18) . . . 6_656 ? Cs1 C1 C2 Cs1 -57.69(18) 2_565 . . 6_656 ? O1 C1 C2 Cs1 -122.31(18) . . . 6_646 ? Cs1 C1 C2 Cs1 -66.20(18) 1_545 . . 6_646 ? Cs1 C1 C2 Cs1 -178.43(18) . . . 6_646 ? Cs1 C1 C2 Cs1 57.69(18) 2_565 . . 6_646 ? O1 C1 C2 Cs1 0.000(4) . . . 2_564 ? Cs1 C1 C2 Cs1 56.11(5) 1_545 . . 2_564 ? Cs1 C1 C2 Cs1 -56.11(5) . . . 2_564 ? Cs1 C1 C2 Cs1 180.000(2) 2_565 . . 2_564 ? O1 Cs1 C2 C1 -64.0(3) 5_566 . . . ? O1 Cs1 C2 C1 167.9(3) 2_564 . . . ? O1 Cs1 C2 C1 -23.7(2) . . . . ? O1 Cs1 C2 C1 71.9(2) 1_565 . . . ? C1 Cs1 C2 C1 87.7(3) 1_565 . . . ? C2 Cs1 C2 C1 110.7(2) 1_565 . . . ? C1 Cs1 C2 C1 -173.5(2) 2_564 . . . ? C2 Cs1 C2 C1 -101.0(2) 6_556 . . . ? C2 Cs1 C2 C1 -172.41(18) 6_566 . . . ? C2 Cs1 C2 C1 5.9(2) 2_565 . . . ? O1 Cs1 C2 Cs1 5.3(2) 5_566 . . 1_545 ? O1 Cs1 C2 Cs1 -122.81(18) 2_564 . . 1_545 ? O1 Cs1 C2 Cs1 45.57(12) . . . 1_545 ? O1 Cs1 C2 Cs1 141.23(10) 1_565 . . 1_545 ? C1 Cs1 C2 Cs1 157.01(18) 1_565 . . 1_545 ? C1 Cs1 C2 Cs1 69.3(2) . . . 1_545 ? C2 Cs1 C2 Cs1 180.0 1_565 . . 1_545 ? C1 Cs1 C2 Cs1 -104.26(16) 2_564 . . 1_545 ? C2 Cs1 C2 Cs1 -31.71(2) 6_556 . . 1_545 ? C2 Cs1 C2 Cs1 -103.1(2) 6_566 . . 1_545 ? C2 Cs1 C2 Cs1 75.17(15) 2_565 . . 1_545 ? O1 Cs1 C2 Cs1 174.21(8) 5_566 . . 6_656 ? O1 Cs1 C2 Cs1 46.12(8) 2_564 . . 6_656 ? O1 Cs1 C2 Cs1 -145.49(19) . . . 6_656 ? O1 Cs1 C2 Cs1 -49.84(18) 1_565 . . 6_656 ? C1 Cs1 C2 Cs1 -34.06(15) 1_565 . . 6_656 ? C1 Cs1 C2 Cs1 -121.8(3) . . . 6_656 ? C2 Cs1 C2 Cs1 -11.1(2) 1_565 . . 6_656 ? C1 Cs1 C2 Cs1 64.67(10) 2_564 . . 6_656 ? C2 Cs1 C2 Cs1 137.2(2) 6_556 . . 6_656 ? C2 Cs1 C2 Cs1 65.8(3) 6_566 . . 6_656 ? C2 Cs1 C2 Cs1 -115.89(10) 2_565 . . 6_656 ? O1 Cs1 C2 Cs1 108.6(6) 5_566 . . 6_646 ? O1 Cs1 C2 Cs1 -19.5(6) 2_564 . . 6_646 ? O1 Cs1 C2 Cs1 148.9(7) . . . 6_646 ? O1 Cs1 C2 Cs1 -115.5(6) 1_565 . . 6_646 ? C1 Cs1 C2 Cs1 -99.7(6) 1_565 . . 6_646 ? C1 Cs1 C2 Cs1 172.6(8) . . . 6_646 ? C2 Cs1 C2 Cs1 -76.7(7) 1_565 . . 6_646 ? C1 Cs1 C2 Cs1 -1.0(6) 2_564 . . 6_646 ? C2 Cs1 C2 Cs1 71.6(7) 6_556 . . 6_646 ? C2 Cs1 C2 Cs1 0.2(8) 6_566 . . 6_646 ? C2 Cs1 C2 Cs1 178.5(7) 2_565 . . 6_646 ? O1 Cs1 C2 Cs1 106.81(12) 5_566 . . 2_564 ? O1 Cs1 C2 Cs1 -21.28(7) 2_564 . . 2_564 ? O1 Cs1 C2 Cs1 147.11(18) . . . 2_564 ? O1 Cs1 C2 Cs1 -117.24(13) 1_565 . . 2_564 ? C1 Cs1 C2 Cs1 -101.46(15) 1_565 . . 2_564 ? C1 Cs1 C2 Cs1 170.8(3) . . . 2_564 ? C2 Cs1 C2 Cs1 -78.47(18) 1_565 . . 2_564 ? C1 Cs1 C2 Cs1 -2.73(8) 2_564 . . 2_564 ? C2 Cs1 C2 Cs1 69.82(17) 6_556 . . 2_564 ? C2 Cs1 C2 Cs1 -1.6(3) 6_566 . . 2_564 ? C2 Cs1 C2 Cs1 176.71(11) 2_565 . . 2_564 ? _diffrn_measured_fraction_theta_max 0.994 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.995 _refine_diff_density_max 1.079 _refine_diff_density_min -1.343 _refine_diff_density_rms 0.174 # Attachment 'wa445.cif' data_wa445 _database_code_depnum_ccdc_archive 'CCDC 648997' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety ? _chemical_formula_sum 'C28 H62 Cs O P3 Si2' _chemical_formula_weight 696.78 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' Cs Cs -0.3680 2.1192 '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' P P 0.1023 0.0942 '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 'C mcm' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, z+1/2' 'x, -y, -z' '-x, y, -z+1/2' 'x+1/2, y+1/2, z' '-x+1/2, -y+1/2, z+1/2' 'x+1/2, -y+1/2, -z' '-x+1/2, y+1/2, -z+1/2' '-x, -y, -z' 'x, y, -z-1/2' '-x, y, z' 'x, -y, z-1/2' '-x+1/2, -y+1/2, -z' 'x+1/2, y+1/2, -z-1/2' '-x+1/2, y+1/2, z' 'x+1/2, -y+1/2, z-1/2' _cell_length_a 25.516(2) _cell_length_b 12.8382(11) _cell_length_c 11.8824(10) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 3892.4(6) _cell_formula_units_Z 4 _cell_measurement_temperature 173(2) _cell_measurement_reflns_used 13095 _cell_measurement_theta_min 3.6 _cell_measurement_theta_max 25.4 _exptl_crystal_description block _exptl_crystal_colour violet _exptl_crystal_size_max 0.34 _exptl_crystal_size_mid 0.27 _exptl_crystal_size_min 0.26 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.189 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1464 _exptl_absorpt_coefficient_mu 1.153 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.6952 _exptl_absorpt_correction_T_max 0.7536 _exptl_absorpt_process_details 'MULABS (Spek, 1990; Blessing, 1995)' _exptl_special_details ; ? ; _diffrn_ambient_temperature 173(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 'STOE IPDS II two-circle-diffractometer' _diffrn_measurement_method \w _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time 0 _diffrn_standards_decay_% 0 _diffrn_reflns_number 9944 _diffrn_reflns_av_R_equivalents 0.0293 _diffrn_reflns_av_sigmaI/netI 0.0161 _diffrn_reflns_limit_h_min -30 _diffrn_reflns_limit_h_max 26 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 15 _diffrn_reflns_limit_l_min -14 _diffrn_reflns_limit_l_max 14 _diffrn_reflns_theta_min 3.55 _diffrn_reflns_theta_max 25.37 _reflns_number_total 1899 _reflns_number_gt 1785 _reflns_threshold_expression >2sigma(I) _computing_data_collection 'X-Area (Stoe & Cie, 2001)' _computing_cell_refinement 'X-Area (Stoe & Cie, 2001)' _computing_data_reduction 'X-Area (Stoe & Cie, 2001)' _computing_structure_solution 'SHELXS-97 (Sheldrick, 1990)' _computing_structure_refinement 'SHELXL-97 (Sheldrick, 1997)' _computing_molecular_graphics 'XP in SHELXTL-Plus (Sheldrick, 1991)' _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^)+(0.0869P)^2^+58.3288P] 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 mixed _refine_ls_extinction_method none _refine_ls_extinction_coef ? _refine_ls_number_reflns 1899 _refine_ls_number_parameters 94 _refine_ls_number_restraints 2 _refine_ls_R_factor_all 0.0974 _refine_ls_R_factor_gt 0.0941 _refine_ls_wR_factor_ref 0.2228 _refine_ls_wR_factor_gt 0.2203 _refine_ls_goodness_of_fit_ref 1.074 _refine_ls_restrained_S_all 1.074 _refine_ls_shift/su_max 0.000 _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 Cs1 Cs 0.0000 0.5000 0.5000 0.1138(8) Uani 1 4 d S . . P1 P 0.06440(7) 0.60552(15) 0.2500 0.0364(6) Uani 1 2 d S . . P2 P 0.0000 0.7061(2) 0.2500 0.0286(6) Uani 1 4 d S . . Si1 Si 0.13533(8) 0.71241(15) 0.2500 0.0290(5) Uani 1 2 d S . . C1 C 0.1922(3) 0.6111(7) 0.2500 0.046(2) Uani 1 2 d S . . C11 C 0.1880(4) 0.5414(12) 0.1479(16) 0.203(11) Uani 1 1 d . . . H11A H 0.1906 0.5836 0.0795 0.304 Uiso 1 1 calc R . . H11B H 0.1542 0.5051 0.1490 0.304 Uiso 1 1 calc R . . H11C H 0.2164 0.4901 0.1492 0.304 Uiso 1 1 calc R . . C12 C 0.2479(4) 0.6560(10) 0.2500 0.069(3) Uani 1 2 d S . . H12A H 0.2501 0.7002 0.3165 0.104 Uiso 1 1 d R . . H12C H 0.2734 0.5990 0.2500 0.104 Uiso 1 2 d SR . . C2 C 0.1374(3) 0.7979(6) 0.1156(7) 0.073(3) Uani 1 1 d D . . C21 C 0.0934(5) 0.8783(14) 0.114(2) 0.303(19) Uani 1 1 d D . . H21A H 0.0596 0.8431 0.1239 0.455 Uiso 1 1 calc R . . H21B H 0.0937 0.9156 0.0424 0.455 Uiso 1 1 calc R . . H21C H 0.0986 0.9280 0.1760 0.455 Uiso 1 1 calc R . . C22 C 0.1874(3) 0.8592(8) 0.0996(9) 0.086(3) Uani 1 1 d . . . H22A H 0.1929 0.9050 0.1646 0.130 Uiso 1 1 calc R . . H22B H 0.1848 0.9014 0.0311 0.130 Uiso 1 1 calc R . . H22C H 0.2171 0.8111 0.0928 0.130 Uiso 1 1 calc R . . C23 C 0.1308(12) 0.7289(13) 0.0125(8) 0.35(2) Uani 1 1 d D . . H23A H 0.0985 0.6880 0.0198 0.519 Uiso 1 1 calc R . . H23B H 0.1608 0.6817 0.0063 0.519 Uiso 1 1 calc R . . H23C H 0.1287 0.7724 -0.0551 0.519 Uiso 1 1 calc R . . O31 O 0.0000 0.321(2) 0.2500 0.26(2) Uani 1 4 d S . . C32 C 0.0445(8) 0.2714(19) 0.2500 0.130(7) Uani 1 2 d S . . H32A H 0.0653 0.2893 0.3177 0.156 Uiso 1 1 d R . . C33 C 0.0299(11) 0.1521(17) 0.2500 0.21(2) Uani 1 2 d S . . H33A H 0.0438 0.1169 0.1822 0.256 Uiso 1 1 d 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 Cs1 0.0570(7) 0.1612(15) 0.1231(12) 0.1092(11) 0.000 0.000 P1 0.0186(9) 0.0268(10) 0.0639(14) 0.000 0.000 -0.0011(7) P2 0.0211(12) 0.0286(13) 0.0359(14) 0.000 0.000 0.000 Si1 0.0214(10) 0.0264(10) 0.0392(11) 0.000 0.000 -0.0024(8) C1 0.020(4) 0.052(5) 0.067(6) 0.000 0.000 0.007(4) C11 0.054(5) 0.238(16) 0.32(2) -0.229(17) -0.054(9) 0.067(8) C12 0.022(4) 0.085(8) 0.101(9) 0.000 0.000 0.006(5) C2 0.061(5) 0.072(5) 0.087(6) 0.050(5) -0.018(4) -0.023(4) C21 0.082(8) 0.30(2) 0.52(4) 0.37(3) 0.090(15) 0.069(11) C22 0.065(5) 0.093(6) 0.101(7) 0.046(6) 0.013(5) -0.023(5) C23 0.70(6) 0.27(2) 0.069(8) 0.101(12) -0.152(18) -0.33(3) O31 0.099(17) 0.16(2) 0.52(7) 0.000 0.000 0.000 C32 0.104(14) 0.17(2) 0.116(15) 0.000 0.000 -0.005(14) C33 0.37(5) 0.154(19) 0.113(15) 0.000 0.000 0.18(3) _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 Cs1 P1 3.6551(11) 3_566 ? Cs1 P1 3.6551(11) 9_566 ? Cs1 P1 3.6551(11) 11 ? Cs1 P1 3.6551(11) . ? Cs1 O31 3.753(18) 9_566 ? Cs1 O31 3.753(18) . ? Cs1 P2 3.9783(18) 9_566 ? Cs1 P2 3.9783(18) . ? P1 P2 2.090(3) . ? P1 Si1 2.271(3) . ? P1 Cs1 3.6551(11) 2_564 ? P2 P1 2.090(3) 11 ? P2 Cs1 3.9783(18) 2_564 ? Si1 C2 1.938(7) . ? Si1 C2 1.938(7) 10_556 ? Si1 C1 1.948(9) . ? C1 C11 1.511(13) . ? C1 C11 1.511(13) 10_556 ? C1 C12 1.535(12) . ? C11 H11A 0.9800 . ? C11 H11B 0.9800 . ? C11 H11C 0.9800 . ? C12 H12A 0.9740 . ? C12 H12C 0.9798 . ? C2 C22 1.512(10) . ? C2 C23 1.522(9) . ? C2 C21 1.525(9) . ? C21 H21A 0.9800 . ? C21 H21B 0.9800 . ? C21 H21C 0.9800 . ? C22 H22A 0.9800 . ? C22 H22B 0.9800 . ? C22 H22C 0.9800 . ? C23 H23A 0.9800 . ? C23 H23B 0.9800 . ? C23 H23C 0.9800 . ? O31 C32 1.30(2) . ? O31 C32 1.30(2) 11 ? O31 Cs1 3.753(18) 2_564 ? C32 C33 1.58(3) . ? C32 H32A 0.9900 . ? C33 C33 1.52(6) 11 ? C33 H33A 0.9900 . ? 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 P1 Cs1 P1 53.43(5) 3_566 9_566 ? P1 Cs1 P1 180.0 3_566 11 ? P1 Cs1 P1 126.57(5) 9_566 11 ? P1 Cs1 P1 126.57(5) 3_566 . ? P1 Cs1 P1 180.0 9_566 . ? P1 Cs1 P1 53.43(5) 11 . ? P1 Cs1 O31 65.4(3) 3_566 9_566 ? P1 Cs1 O31 65.4(3) 9_566 9_566 ? P1 Cs1 O31 114.6(3) 11 9_566 ? P1 Cs1 O31 114.6(3) . 9_566 ? P1 Cs1 O31 114.6(3) 3_566 . ? P1 Cs1 O31 114.6(3) 9_566 . ? P1 Cs1 O31 65.4(3) 11 . ? P1 Cs1 O31 65.4(3) . . ? O31 Cs1 O31 180.000(1) 9_566 . ? P1 Cs1 P2 31.42(3) 3_566 9_566 ? P1 Cs1 P2 31.42(3) 9_566 9_566 ? P1 Cs1 P2 148.58(3) 11 9_566 ? P1 Cs1 P2 148.58(3) . 9_566 ? O31 Cs1 P2 79.4(4) 9_566 9_566 ? O31 Cs1 P2 100.6(4) . 9_566 ? P1 Cs1 P2 148.58(3) 3_566 . ? P1 Cs1 P2 148.58(3) 9_566 . ? P1 Cs1 P2 31.42(3) 11 . ? P1 Cs1 P2 31.42(3) . . ? O31 Cs1 P2 100.6(4) 9_566 . ? O31 Cs1 P2 79.4(4) . . ? P2 Cs1 P2 180.0 9_566 . ? P2 P1 Si1 104.67(11) . . ? P2 P1 Cs1 82.85(5) . . ? Si1 P1 Cs1 125.60(2) . . ? P2 P1 Cs1 82.85(5) . 2_564 ? Si1 P1 Cs1 125.60(2) . 2_564 ? Cs1 P1 Cs1 108.73(5) . 2_564 ? P1 P2 P1 103.67(16) 11 . ? P1 P2 Cs1 65.73(6) 11 . ? P1 P2 Cs1 65.73(6) . . ? P1 P2 Cs1 65.73(6) 11 2_564 ? P1 P2 Cs1 65.73(6) . 2_564 ? Cs1 P2 Cs1 96.61(6) . 2_564 ? C2 Si1 C2 110.9(5) . 10_556 ? C2 Si1 C1 111.0(3) . . ? C2 Si1 C1 111.0(3) 10_556 . ? C2 Si1 P1 111.3(2) . . ? C2 Si1 P1 111.3(2) 10_556 . ? C1 Si1 P1 100.9(3) . . ? C11 C1 C11 106.7(18) . 10_556 ? C11 C1 C12 106.8(7) . . ? C11 C1 C12 106.8(7) 10_556 . ? C11 C1 Si1 110.0(6) . . ? C11 C1 Si1 110.1(6) 10_556 . ? C12 C1 Si1 116.0(7) . . ? C1 C11 H11A 109.5 . . ? C1 C11 H11B 109.5 . . ? H11A C11 H11B 109.5 . . ? C1 C11 H11C 109.5 . . ? H11A C11 H11C 109.5 . . ? H11B C11 H11C 109.5 . . ? C1 C12 H12A 105.8 . . ? C1 C12 H12C 109.5 . . ? H12A C12 H12C 113.4 . . ? C22 C2 C23 107.2(11) . . ? C22 C2 C21 105.5(8) . . ? C23 C2 C21 107.7(16) . . ? C22 C2 Si1 114.9(6) . . ? C23 C2 Si1 109.3(6) . . ? C21 C2 Si1 111.8(7) . . ? C2 C21 H21A 109.5 . . ? C2 C21 H21B 109.5 . . ? H21A C21 H21B 109.5 . . ? C2 C21 H21C 109.5 . . ? H21A C21 H21C 109.5 . . ? H21B C21 H21C 109.5 . . ? C2 C22 H22A 109.5 . . ? C2 C22 H22B 109.5 . . ? H22A C22 H22B 109.5 . . ? C2 C22 H22C 109.5 . . ? H22A C22 H22C 109.5 . . ? H22B C22 H22C 109.5 . . ? C2 C23 H23A 109.5 . . ? C2 C23 H23B 109.5 . . ? H23A C23 H23B 109.5 . . ? C2 C23 H23C 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? C32 O31 C32 121(3) . 11 ? C32 O31 Cs1 107.5(8) . . ? C32 O31 Cs1 107.5(8) 11 . ? C32 O31 Cs1 107.5(8) . 2_564 ? C32 O31 Cs1 107.5(8) 11 2_564 ? Cs1 O31 Cs1 104.6(7) . 2_564 ? O31 C32 C33 106(2) . . ? O31 C32 H32A 110.6 . . ? C33 C32 H32A 110.6 . . ? C33 C33 C32 103.7(13) 11 . ? C33 C33 H33A 111.0 11 . ? C32 C33 H33A 111.0 . . ? 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 P1 Cs1 P1 P2 -145.48(7) 3_566 . . . ? P1 Cs1 P1 P2 -149(6) 9_566 . . . ? P1 Cs1 P1 P2 34.52(7) 11 . . . ? O31 Cs1 P1 P2 -68.8(2) 9_566 . . . ? O31 Cs1 P1 P2 111.2(2) . . . . ? P2 Cs1 P1 P2 180.0 9_566 . . . ? P1 Cs1 P1 Si1 -42.54(9) 3_566 . . . ? P1 Cs1 P1 Si1 -46(6) 9_566 . . . ? P1 Cs1 P1 Si1 137.46(9) 11 . . . ? O31 Cs1 P1 Si1 34.1(2) 9_566 . . . ? O31 Cs1 P1 Si1 -145.9(2) . . . . ? P2 Cs1 P1 Si1 -77.06(13) 9_566 . . . ? P2 Cs1 P1 Si1 102.94(13) . . . . ? P1 Cs1 P1 Cs1 134.59(5) 3_566 . . 2_564 ? P1 Cs1 P1 Cs1 131(6) 9_566 . . 2_564 ? P1 Cs1 P1 Cs1 -45.41(5) 11 . . 2_564 ? O31 Cs1 P1 Cs1 -148.7(2) 9_566 . . 2_564 ? O31 Cs1 P1 Cs1 31.3(2) . . . 2_564 ? P2 Cs1 P1 Cs1 100.08(7) 9_566 . . 2_564 ? P2 Cs1 P1 Cs1 -79.92(7) . . . 2_564 ? Si1 P1 P2 P1 180.0 . . . 11 ? Cs1 P1 P2 P1 -54.99(2) . . . 11 ? Cs1 P1 P2 P1 54.99(2) 2_564 . . 11 ? Si1 P1 P2 Cs1 -125.01(2) . . . . ? Cs1 P1 P2 Cs1 109.99(4) 2_564 . . . ? Si1 P1 P2 Cs1 125.01(2) . . . 2_564 ? Cs1 P1 P2 Cs1 -109.99(4) . . . 2_564 ? P1 Cs1 P2 P1 180.0 3_566 . . 11 ? P1 Cs1 P2 P1 -60.82(13) 9_566 . . 11 ? P1 Cs1 P2 P1 119.18(13) . . . 11 ? O31 Cs1 P2 P1 -120.41(6) 9_566 . . 11 ? O31 Cs1 P2 P1 59.59(6) . . . 11 ? P2 Cs1 P2 P1 59.6(3) 9_566 . . 11 ? P1 Cs1 P2 P1 60.81(13) 3_566 . . . ? P1 Cs1 P2 P1 180.0 9_566 . . . ? P1 Cs1 P2 P1 -119.18(13) 11 . . . ? O31 Cs1 P2 P1 120.41(6) 9_566 . . . ? O31 Cs1 P2 P1 -59.59(6) . . . . ? P2 Cs1 P2 P1 -59.59(18) 9_566 . . . ? P1 Cs1 P2 Cs1 120.41(6) 3_566 . . 2_564 ? P1 Cs1 P2 Cs1 -120.41(6) 9_566 . . 2_564 ? P1 Cs1 P2 Cs1 -59.59(6) 11 . . 2_564 ? P1 Cs1 P2 Cs1 59.59(6) . . . 2_564 ? O31 Cs1 P2 Cs1 180.0 9_566 . . 2_564 ? O31 Cs1 P2 Cs1 0.0 . . . 2_564 ? P2 Cs1 P2 Cs1 0(100) 9_566 . . 2_564 ? P2 P1 Si1 C2 -62.2(3) . . . . ? Cs1 P1 Si1 C2 -153.8(3) . . . . ? Cs1 P1 Si1 C2 29.5(3) 2_564 . . . ? P2 P1 Si1 C2 62.2(3) . . . 10_556 ? Cs1 P1 Si1 C2 -29.5(3) . . . 10_556 ? Cs1 P1 Si1 C2 153.8(3) 2_564 . . 10_556 ? P2 P1 Si1 C1 180.0 . . . . ? Cs1 P1 Si1 C1 88.33(8) . . . . ? Cs1 P1 Si1 C1 -88.33(8) 2_564 . . . ? C2 Si1 C1 C11 -59.4(10) . . . . ? C2 Si1 C1 C11 176.8(9) 10_556 . . . ? P1 Si1 C1 C11 58.7(9) . . . . ? C2 Si1 C1 C11 -176.8(9) . . . 10_556 ? C2 Si1 C1 C11 59.4(10) 10_556 . . 10_556 ? P1 Si1 C1 C11 -58.7(9) . . . 10_556 ? C2 Si1 C1 C12 61.9(3) . . . . ? C2 Si1 C1 C12 -61.9(3) 10_556 . . . ? P1 Si1 C1 C12 180.0 . . . . ? C2 Si1 C2 C22 64.5(9) 10_556 . . . ? C1 Si1 C2 C22 -59.3(8) . . . . ? P1 Si1 C2 C22 -170.9(6) . . . . ? C2 Si1 C2 C23 -175.0(13) 10_556 . . . ? C1 Si1 C2 C23 61.2(14) . . . . ? P1 Si1 C2 C23 -50.4(13) . . . . ? C2 Si1 C2 C21 -55.8(13) 10_556 . . . ? C1 Si1 C2 C21 -179.6(11) . . . . ? P1 Si1 C2 C21 68.8(11) . . . . ? P1 Cs1 O31 C32 -36.3(15) 3_566 . . . ? P1 Cs1 O31 C32 -95.6(14) 9_566 . . . ? P1 Cs1 O31 C32 143.7(15) 11 . . . ? P1 Cs1 O31 C32 84.4(14) . . . . ? O31 Cs1 O31 C32 -65.9(9) 9_566 . . . ? P2 Cs1 O31 C32 -65.9(14) 9_566 . . . ? P2 Cs1 O31 C32 114.1(14) . . . . ? P1 Cs1 O31 C32 95.6(14) 3_566 . . 11 ? P1 Cs1 O31 C32 36.3(15) 9_566 . . 11 ? P1 Cs1 O31 C32 -84.4(14) 11 . . 11 ? P1 Cs1 O31 C32 -143.7(15) . . . 11 ? O31 Cs1 O31 C32 66(3) 9_566 . . 11 ? P2 Cs1 O31 C32 65.9(14) 9_566 . . 11 ? P2 Cs1 O31 C32 -114.1(14) . . . 11 ? P1 Cs1 O31 Cs1 -150.36(9) 3_566 . . 2_564 ? P1 Cs1 O31 Cs1 150.36(9) 9_566 . . 2_564 ? P1 Cs1 O31 Cs1 29.64(9) 11 . . 2_564 ? P1 Cs1 O31 Cs1 -29.64(9) . . . 2_564 ? O31 Cs1 O31 Cs1 180.0(13) 9_566 . . 2_564 ? P2 Cs1 O31 Cs1 180.0 9_566 . . 2_564 ? P2 Cs1 O31 Cs1 0.0 . . . 2_564 ? C32 O31 C32 C33 0.0 11 . . . ? Cs1 O31 C32 C33 123.9(7) . . . . ? Cs1 O31 C32 C33 -123.9(7) 2_564 . . . ? O31 C32 C33 C33 0.0 . . . 11 ? _diffrn_measured_fraction_theta_max 0.983 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.994 _refine_diff_density_max 2.054 _refine_diff_density_min -2.869 _refine_diff_density_rms 0.139