Supplementary Material (ESI) for Dalton Transactions This journal is © The Royal Society of Chemistry 2005 data_global _journal_coden_Cambridge 222 loop_ _publ_author_name 'Keith Izod' 'W. Clegg' 'Ross W. Harrington' 'Jonathan Young' _publ_contact_author_name 'Dr Keith Izod' _publ_contact_author_address ; Department of Chemistry University of Newcastle Bedson Building Newcastle Upon Tyne NE1 7RU UK ; _publ_contact_author_email K.J.IZOD@NCL.AC.UK _publ_requested_journal 'Dalton Transactions' _publ_section_title ; Effect of peripheral donor substituents on the binding modes of phosphinomethanide ligands. Synthesis and crystal structures of alkali metal derivatives of an O-functionalised phosphinomethanide ligand ; data_ki144_9 _database_code_depnum_ccdc_archive 'CCDC 263835' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H37 O2 P Si2' _chemical_formula_sum 'C23 H37 O2 P Si2' _chemical_formula_weight 432.68 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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 7.2142(4) _cell_length_b 11.2764(6) _cell_length_c 16.3272(8) _cell_angle_alpha 73.502(1) _cell_angle_beta 86.635(1) _cell_angle_gamma 77.341(1) _cell_volume 1242.57(11) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7650 _cell_measurement_theta_min 2.60 _cell_measurement_theta_max 28.57 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.40 _exptl_crystal_size_min 0.40 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.156 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 468 _exptl_absorpt_coefficient_mu 0.223 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.897 _exptl_absorpt_correction_T_max 0.916 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 11239 _diffrn_reflns_av_R_equivalents 0.0232 _diffrn_reflns_av_sigmaI/netI 0.0382 _diffrn_reflns_limit_h_min -9 _diffrn_reflns_limit_h_max 9 _diffrn_reflns_limit_k_min -15 _diffrn_reflns_limit_k_max 14 _diffrn_reflns_limit_l_min -21 _diffrn_reflns_limit_l_max 21 _diffrn_reflns_theta_min 1.93 _diffrn_reflns_theta_max 28.77 _reflns_number_total 5839 _reflns_number_gt 4611 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0467P)^2^+0.2510P] 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 5839 _refine_ls_number_parameters 261 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0499 _refine_ls_R_factor_gt 0.0346 _refine_ls_wR_factor_ref 0.0948 _refine_ls_wR_factor_gt 0.0868 _refine_ls_goodness_of_fit_ref 1.037 _refine_ls_restrained_S_all 1.037 _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 0.05225(5) 0.82071(3) 0.24146(2) 0.01877(9) Uani 1 1 d . . . Si1 Si 0.11836(6) 0.67050(4) 0.11108(3) 0.02426(11) Uani 1 1 d . . . Si2 Si 0.07980(6) 0.52833(4) 0.30838(3) 0.02410(11) Uani 1 1 d . . . O1 O -0.09994(16) 1.23860(10) 0.16685(7) 0.0305(3) Uani 1 1 d . . . O2 O -0.31942(16) 1.01626(11) 0.38746(8) 0.0367(3) Uani 1 1 d . . . C1 C 0.1631(2) 0.66414(13) 0.22671(9) 0.0208(3) Uani 1 1 d . . . H1 H 0.3034 0.6513 0.2343 0.025 Uiso 1 1 calc R . . C2 C 0.1079(3) 0.83004(16) 0.03504(10) 0.0333(4) Uani 1 1 d . . . H2A H 0.0825 0.8276 -0.0227 0.050 Uiso 1 1 calc R . . H2B H 0.2296 0.8549 0.0357 0.050 Uiso 1 1 calc R . . H2C H 0.0061 0.8916 0.0520 0.050 Uiso 1 1 calc R . . C3 C 0.3162(3) 0.55905(19) 0.07515(12) 0.0457(5) Uani 1 1 d . . . H3A H 0.2925 0.5610 0.0162 0.069 Uiso 1 1 calc R . . H3B H 0.3234 0.4731 0.1125 0.069 Uiso 1 1 calc R . . H3C H 0.4365 0.5847 0.0779 0.069 Uiso 1 1 calc R . . C4 C -0.1149(3) 0.63077(17) 0.09815(12) 0.0388(4) Uani 1 1 d . . . H4A H -0.2174 0.6885 0.1183 0.058 Uiso 1 1 calc R . . H4B H -0.1139 0.5434 0.1316 0.058 Uiso 1 1 calc R . . H4C H -0.1356 0.6396 0.0377 0.058 Uiso 1 1 calc R . . C5 C 0.2013(3) 0.48428(17) 0.41413(11) 0.0413(4) Uani 1 1 d . . . H5A H 0.1794 0.4020 0.4486 0.062 Uiso 1 1 calc R . . H5B H 0.1502 0.5486 0.4439 0.062 Uiso 1 1 calc R . . H5C H 0.3381 0.4792 0.4053 0.062 Uiso 1 1 calc R . . C6 C 0.1478(3) 0.38117(15) 0.27222(12) 0.0357(4) Uani 1 1 d . . . H6A H 0.2853 0.3626 0.2628 0.054 Uiso 1 1 calc R . . H6B H 0.0811 0.3937 0.2188 0.054 Uiso 1 1 calc R . . H6C H 0.1127 0.3102 0.3161 0.054 Uiso 1 1 calc R . . C7 C -0.1827(2) 0.56692(17) 0.32552(12) 0.0365(4) Uani 1 1 d . . . H7A H -0.2208 0.4955 0.3678 0.055 Uiso 1 1 calc R . . H7B H -0.2489 0.5832 0.2714 0.055 Uiso 1 1 calc R . . H7C H -0.2160 0.6424 0.3463 0.055 Uiso 1 1 calc R . . C8 C 0.21960(19) 0.92472(14) 0.19359(9) 0.0205(3) Uani 1 1 d . . . C9 C 0.4037(2) 0.88069(15) 0.16791(10) 0.0286(3) Uani 1 1 d . . . H9 H 0.4510 0.7921 0.1786 0.034 Uiso 1 1 calc R . . C10 C 0.5193(2) 0.96309(17) 0.12713(11) 0.0346(4) Uani 1 1 d . . . H10 H 0.6441 0.9312 0.1101 0.042 Uiso 1 1 calc R . . C11 C 0.4512(2) 1.09208(17) 0.11143(10) 0.0328(4) Uani 1 1 d . . . H11 H 0.5284 1.1492 0.0824 0.039 Uiso 1 1 calc R . . C12 C 0.2708(2) 1.13810(15) 0.13794(10) 0.0282(3) Uani 1 1 d . . . H12 H 0.2262 1.2268 0.1279 0.034 Uiso 1 1 calc R . . C13 C 0.1537(2) 1.05615(14) 0.17913(9) 0.0218(3) Uani 1 1 d . . . C14 C -0.0398(2) 1.10816(14) 0.20930(10) 0.0277(3) Uani 1 1 d . . . H14A H -0.1321 1.0612 0.1981 0.033 Uiso 1 1 calc R . . H14B H -0.0359 1.0963 0.2717 0.033 Uiso 1 1 calc R . . C15 C -0.2755(2) 1.29098(16) 0.19928(12) 0.0349(4) Uani 1 1 d . . . H15A H -0.3707 1.2431 0.1947 0.052 Uiso 1 1 calc R . . H15B H -0.3175 1.3795 0.1662 0.052 Uiso 1 1 calc R . . H15C H -0.2597 1.2866 0.2593 0.052 Uiso 1 1 calc R . . C16 C 0.0958(2) 0.80783(13) 0.35460(9) 0.0204(3) Uani 1 1 d . . . C17 C 0.2803(2) 0.76385(15) 0.38853(10) 0.0267(3) Uani 1 1 d . . . H17 H 0.3823 0.7395 0.3531 0.032 Uiso 1 1 calc R . . C18 C 0.3170(2) 0.75514(16) 0.47232(10) 0.0330(4) Uani 1 1 d . . . H18 H 0.4423 0.7225 0.4946 0.040 Uiso 1 1 calc R . . C19 C 0.1701(3) 0.79422(17) 0.52380(10) 0.0354(4) Uani 1 1 d . . . H19 H 0.1949 0.7905 0.5811 0.042 Uiso 1 1 calc R . . C20 C -0.0119(2) 0.83850(16) 0.49132(10) 0.0323(4) Uani 1 1 d . . . H20 H -0.1120 0.8651 0.5268 0.039 Uiso 1 1 calc R . . C21 C -0.0526(2) 0.84517(14) 0.40714(9) 0.0235(3) Uani 1 1 d . . . C22 C -0.2569(2) 0.89299(15) 0.37845(11) 0.0282(3) Uani 1 1 d . . . H22A H -0.2681 0.8943 0.3180 0.034 Uiso 1 1 calc R . . H22B H -0.3364 0.8363 0.4136 0.034 Uiso 1 1 calc R . . C23 C -0.5175(2) 1.06205(18) 0.37197(13) 0.0419(4) Uani 1 1 d . . . H23A H -0.5470 1.0623 0.3141 0.063 Uiso 1 1 calc R . . H23B H -0.5543 1.1483 0.3776 0.063 Uiso 1 1 calc R . . H23C H -0.5877 1.0071 0.4135 0.063 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 0.01653(17) 0.01862(18) 0.02051(18) -0.00545(14) 0.00088(13) -0.00258(13) Si1 0.0260(2) 0.0239(2) 0.0218(2) -0.00813(17) 0.00072(16) -0.00081(17) Si2 0.0265(2) 0.0191(2) 0.0247(2) -0.00397(16) -0.00003(16) -0.00346(16) O1 0.0346(6) 0.0201(5) 0.0320(6) -0.0036(5) 0.0027(5) -0.0015(5) O2 0.0326(6) 0.0279(6) 0.0496(7) -0.0148(6) -0.0018(5) -0.0004(5) C1 0.0189(7) 0.0190(7) 0.0224(7) -0.0054(6) 0.0005(5) -0.0005(5) C2 0.0412(10) 0.0360(9) 0.0211(7) -0.0042(7) -0.0011(7) -0.0094(7) C3 0.0495(11) 0.0460(11) 0.0363(10) -0.0192(9) 0.0076(9) 0.0089(9) C4 0.0418(10) 0.0384(10) 0.0360(9) -0.0057(8) -0.0101(8) -0.0115(8) C5 0.0570(12) 0.0330(9) 0.0302(9) 0.0032(7) -0.0084(8) -0.0155(9) C6 0.0424(10) 0.0218(8) 0.0397(10) -0.0072(7) -0.0002(8) -0.0018(7) C7 0.0324(9) 0.0325(9) 0.0432(10) -0.0086(8) 0.0093(7) -0.0092(7) C8 0.0196(7) 0.0238(7) 0.0189(7) -0.0057(6) 0.0004(5) -0.0065(6) C9 0.0226(7) 0.0283(8) 0.0326(8) -0.0066(7) 0.0028(6) -0.0038(6) C10 0.0229(8) 0.0433(10) 0.0375(9) -0.0107(8) 0.0070(7) -0.0096(7) C11 0.0332(9) 0.0383(9) 0.0308(8) -0.0081(7) 0.0076(7) -0.0195(7) C12 0.0352(9) 0.0258(8) 0.0254(8) -0.0067(6) 0.0026(6) -0.0116(7) C13 0.0245(7) 0.0243(7) 0.0173(7) -0.0056(6) -0.0007(6) -0.0065(6) C14 0.0308(8) 0.0189(7) 0.0304(8) -0.0043(6) 0.0055(6) -0.0036(6) C15 0.0328(9) 0.0243(8) 0.0455(10) -0.0110(7) 0.0003(7) -0.0001(7) C16 0.0224(7) 0.0194(7) 0.0201(7) -0.0046(6) 0.0012(5) -0.0074(6) C17 0.0237(7) 0.0285(8) 0.0271(8) -0.0045(6) 0.0006(6) -0.0083(6) C18 0.0327(9) 0.0362(9) 0.0292(8) -0.0004(7) -0.0080(7) -0.0148(7) C19 0.0505(11) 0.0377(9) 0.0216(8) -0.0065(7) -0.0012(7) -0.0190(8) C20 0.0395(9) 0.0341(9) 0.0259(8) -0.0109(7) 0.0088(7) -0.0120(7) C21 0.0265(7) 0.0210(7) 0.0254(7) -0.0078(6) 0.0049(6) -0.0095(6) C22 0.0232(7) 0.0295(8) 0.0357(9) -0.0160(7) 0.0088(6) -0.0066(6) C23 0.0330(9) 0.0358(10) 0.0504(11) -0.0095(9) 0.0025(8) 0.0023(8) _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 1.8480(14) . ? P1 C8 1.8529(14) . ? P1 C16 1.8514(14) . ? Si1 C1 1.9126(15) . ? Si1 C2 1.8619(17) . ? Si1 C3 1.8696(17) . ? Si1 C4 1.8719(18) . ? Si2 C1 1.9063(15) . ? Si2 C5 1.8699(18) . ? Si2 C6 1.8730(17) . ? Si2 C7 1.8710(17) . ? O1 C14 1.4172(17) . ? O1 C15 1.4155(19) . ? O2 C22 1.4109(18) . ? O2 C23 1.420(2) . ? C8 C9 1.397(2) . ? C8 C13 1.408(2) . ? C9 C10 1.387(2) . ? C10 C11 1.383(2) . ? C11 C12 1.384(2) . ? C12 C13 1.394(2) . ? C13 C14 1.504(2) . ? C16 C17 1.402(2) . ? C16 C21 1.400(2) . ? C17 C18 1.381(2) . ? C18 C19 1.387(3) . ? C19 C20 1.378(2) . ? C20 C21 1.400(2) . ? C21 C22 1.508(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 C8 105.59(6) . . ? C1 P1 C16 105.56(6) . . ? C8 P1 C16 97.17(6) . . ? C1 Si1 C2 113.34(7) . . ? C1 Si1 C3 109.31(8) . . ? C1 Si1 C4 112.01(7) . . ? C2 Si1 C3 106.95(9) . . ? C2 Si1 C4 104.96(8) . . ? C3 Si1 C4 110.08(9) . . ? C1 Si2 C5 112.70(7) . . ? C1 Si2 C6 109.65(7) . . ? C1 Si2 C7 111.52(7) . . ? C5 Si2 C6 104.01(8) . . ? C5 Si2 C7 108.46(9) . . ? C6 Si2 C7 110.24(8) . . ? C14 O1 C15 111.32(12) . . ? C22 O2 C23 112.11(13) . . ? P1 C1 Si1 107.53(7) . . ? P1 C1 Si2 112.94(7) . . ? Si1 C1 Si2 113.34(7) . . ? P1 C8 C9 123.78(11) . . ? P1 C8 C13 117.77(10) . . ? C9 C8 C13 118.38(13) . . ? C8 C9 C10 121.62(15) . . ? C9 C10 C11 119.42(15) . . ? C10 C11 C12 120.12(15) . . ? C11 C12 C13 120.92(15) . . ? C8 C13 C12 119.50(14) . . ? C8 C13 C14 120.53(12) . . ? C12 C13 C14 119.95(14) . . ? O1 C14 C13 110.76(12) . . ? P1 C16 C17 120.29(11) . . ? P1 C16 C21 121.01(11) . . ? C17 C16 C21 118.68(13) . . ? C16 C17 C18 121.41(15) . . ? C17 C18 C19 119.76(15) . . ? C18 C19 C20 119.59(15) . . ? C19 C20 C21 121.45(15) . . ? C16 C21 C20 119.08(14) . . ? C16 C21 C22 123.72(13) . . ? C20 C21 C22 117.19(13) . . ? O2 C22 C21 108.64(12) . . ? 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 C8 P1 C1 Si1 -78.85(8) . . . . ? C8 P1 C1 Si2 155.35(7) . . . . ? C16 P1 C1 Si1 178.89(6) . . . . ? C16 P1 C1 Si2 53.09(9) . . . . ? C5 Si2 C1 P1 -79.26(10) . . . . ? C5 Si2 C1 Si1 158.12(9) . . . . ? C6 Si2 C1 P1 165.39(8) . . . . ? C6 Si2 C1 Si1 42.78(10) . . . . ? C7 Si2 C1 P1 43.00(10) . . . . ? C7 Si2 C1 Si1 -79.61(10) . . . . ? C2 Si1 C1 P1 31.75(10) . . . . ? C2 Si1 C1 Si2 157.31(8) . . . . ? C3 Si1 C1 P1 150.93(9) . . . . ? C3 Si1 C1 Si2 -83.50(10) . . . . ? C4 Si1 C1 P1 -86.78(9) . . . . ? C4 Si1 C1 Si2 38.78(10) . . . . ? C1 P1 C8 C9 -10.63(14) . . . . ? C1 P1 C8 C13 166.58(11) . . . . ? C16 P1 C8 C9 97.78(13) . . . . ? C16 P1 C8 C13 -85.01(12) . . . . ? P1 C8 C9 C10 175.60(12) . . . . ? C13 C8 C9 C10 -1.6(2) . . . . ? C8 C9 C10 C11 0.0(3) . . . . ? C9 C10 C11 C12 1.4(3) . . . . ? C10 C11 C12 C13 -1.3(2) . . . . ? C11 C12 C13 C8 -0.3(2) . . . . ? C11 C12 C13 C14 178.47(15) . . . . ? P1 C8 C13 C12 -175.66(11) . . . . ? P1 C8 C13 C14 5.58(18) . . . . ? C9 C8 C13 C12 1.7(2) . . . . ? C9 C8 C13 C14 -177.06(14) . . . . ? C15 O1 C14 C13 -175.54(13) . . . . ? C8 C13 C14 O1 -162.25(13) . . . . ? C12 C13 C14 O1 19.0(2) . . . . ? C1 P1 C16 C17 52.28(13) . . . . ? C1 P1 C16 C21 -129.70(12) . . . . ? C8 P1 C16 C17 -56.16(13) . . . . ? C8 P1 C16 C21 121.86(12) . . . . ? P1 C16 C17 C18 179.03(12) . . . . ? C21 C16 C17 C18 1.0(2) . . . . ? C16 C17 C18 C19 -2.1(2) . . . . ? C17 C18 C19 C20 1.6(2) . . . . ? C18 C19 C20 C21 -0.1(2) . . . . ? C19 C20 C21 C16 -1.0(2) . . . . ? C19 C20 C21 C22 179.00(15) . . . . ? P1 C16 C21 C20 -177.49(11) . . . . ? P1 C16 C21 C22 2.5(2) . . . . ? C17 C16 C21 C20 0.6(2) . . . . ? C17 C16 C21 C22 -179.46(13) . . . . ? C23 O2 C22 C21 -172.58(13) . . . . ? C16 C21 C22 O2 -120.93(15) . . . . ? C20 C21 C22 O2 59.05(18) . . . . ? _diffrn_measured_fraction_theta_max 0.904 _diffrn_reflns_theta_full 26.00 _diffrn_measured_fraction_theta_full 0.988 _refine_diff_density_max 0.317 _refine_diff_density_min -0.192 _refine_diff_density_rms 0.047 #===END data_ki122_10 _database_code_depnum_ccdc_archive 'CCDC 263836' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H74 Br2 Li2 O4 P2 Si4' _chemical_formula_sum 'C46 H74 Br2 Li2 O4 P2 Si4' _chemical_formula_weight 1039.1 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' 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' Br Br -0.2901 2.4595 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Li Li -0.0003 0.0001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting monoclinic _symmetry_space_group_name_H-M 'P 21/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 12.0404(6) _cell_length_b 9.4535(5) _cell_length_c 24.4234(12) _cell_angle_alpha 90.00 _cell_angle_beta 95.371(1) _cell_angle_gamma 90.00 _cell_volume 2767.8(2) _cell_formula_units_Z 2 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 13191 _cell_measurement_theta_min 2.52 _cell_measurement_theta_max 28.44 _exptl_crystal_description block _exptl_crystal_colour colourless _exptl_crystal_size_max 0.40 _exptl_crystal_size_mid 0.24 _exptl_crystal_size_min 0.12 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.247 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1088 _exptl_absorpt_coefficient_mu 1.645 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.559 _exptl_absorpt_correction_T_max 0.827 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 23677 _diffrn_reflns_av_R_equivalents 0.0450 _diffrn_reflns_av_sigmaI/netI 0.0464 _diffrn_reflns_limit_h_min -15 _diffrn_reflns_limit_h_max 16 _diffrn_reflns_limit_k_min -12 _diffrn_reflns_limit_k_max 12 _diffrn_reflns_limit_l_min -31 _diffrn_reflns_limit_l_max 32 _diffrn_reflns_theta_min 1.67 _diffrn_reflns_theta_max 28.51 _reflns_number_total 6579 _reflns_number_gt 4930 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0331P)^2^+1.9264P] 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 6579 _refine_ls_number_parameters 279 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0612 _refine_ls_R_factor_gt 0.0358 _refine_ls_wR_factor_ref 0.0862 _refine_ls_wR_factor_gt 0.0769 _refine_ls_goodness_of_fit_ref 1.028 _refine_ls_restrained_S_all 1.028 _refine_ls_shift/su_max 0.009 _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 Br1 Br 1.14263(2) 0.90146(3) 0.004425(10) 0.02657(8) Uani 1 1 d . . . P1 P 0.68737(5) 0.82444(6) 0.13150(2) 0.01642(12) Uani 1 1 d . . . Si1 Si 0.47498(6) 0.97218(7) 0.15716(3) 0.02467(16) Uani 1 1 d . . . Si2 Si 0.45702(5) 0.66676(7) 0.10186(3) 0.01954(14) Uani 1 1 d . . . O1 O 0.94274(13) 0.85951(18) 0.11189(7) 0.0241(4) Uani 1 1 d . . . O2 O 0.87412(13) 0.71406(18) 0.00253(7) 0.0247(4) Uani 1 1 d . . . C1 C 0.54357(18) 0.7923(2) 0.14983(9) 0.0168(4) Uani 1 1 d . . . H1 H 0.5504 0.7477 0.1871 0.020 Uiso 1 1 calc R . . C2 C 0.3578(3) 0.9555(3) 0.20228(14) 0.0486(8) Uani 1 1 d . . . H2A H 0.3210 1.0475 0.2050 0.073 Uiso 1 1 calc R . . H2B H 0.3874 0.9244 0.2390 0.073 Uiso 1 1 calc R . . H2C H 0.3036 0.8860 0.1864 0.073 Uiso 1 1 calc R . . C3 C 0.5712(3) 1.1076(3) 0.19150(13) 0.0429(7) Uani 1 1 d . . . H3A H 0.6363 1.1190 0.1706 0.064 Uiso 1 1 calc R . . H3B H 0.5958 1.0765 0.2290 0.064 Uiso 1 1 calc R . . H3C H 0.5320 1.1982 0.1929 0.064 Uiso 1 1 calc R . . C4 C 0.4254(3) 1.0460(3) 0.08869(12) 0.0403(7) Uani 1 1 d . . . H4A H 0.3951 1.1410 0.0933 0.060 Uiso 1 1 calc R . . H4B H 0.3670 0.9847 0.0709 0.060 Uiso 1 1 calc R . . H4C H 0.4879 1.0511 0.0658 0.060 Uiso 1 1 calc R . . C5 C 0.4680(2) 0.7070(3) 0.02774(10) 0.0328(6) Uani 1 1 d . . . H5A H 0.5468 0.7098 0.0207 0.049 Uiso 1 1 calc R . . H5B H 0.4335 0.7990 0.0187 0.049 Uiso 1 1 calc R . . H5C H 0.4295 0.6334 0.0049 0.049 Uiso 1 1 calc R . . C6 C 0.3068(2) 0.6773(3) 0.11470(11) 0.0299(6) Uani 1 1 d . . . H6A H 0.2639 0.6082 0.0914 0.045 Uiso 1 1 calc R . . H6B H 0.2786 0.7726 0.1059 0.045 Uiso 1 1 calc R . . H6C H 0.2990 0.6564 0.1535 0.045 Uiso 1 1 calc R . . C7 C 0.4959(2) 0.4781(3) 0.11673(12) 0.0308(6) Uani 1 1 d . . . H7A H 0.5004 0.4616 0.1565 0.046 Uiso 1 1 calc R . . H7B H 0.5685 0.4582 0.1033 0.046 Uiso 1 1 calc R . . H7C H 0.4393 0.4157 0.0982 0.046 Uiso 1 1 calc R . . C8 C 0.76634(19) 0.8646(2) 0.19853(9) 0.0193(5) Uani 1 1 d . . . C9 C 0.7281(2) 0.8335(3) 0.24924(10) 0.0247(5) Uani 1 1 d . . . H9 H 0.6569 0.7906 0.2500 0.030 Uiso 1 1 calc R . . C10 C 0.7900(2) 0.8627(3) 0.29840(10) 0.0323(6) Uani 1 1 d . . . H10 H 0.7613 0.8398 0.3322 0.039 Uiso 1 1 calc R . . C11 C 0.8933(2) 0.9250(3) 0.29831(11) 0.0377(7) Uani 1 1 d . . . H11 H 0.9369 0.9437 0.3320 0.045 Uiso 1 1 calc R . . C12 C 0.9329(2) 0.9603(3) 0.24866(11) 0.0326(6) Uani 1 1 d . . . H12 H 1.0038 1.0044 0.2486 0.039 Uiso 1 1 calc R . . C13 C 0.8709(2) 0.9323(3) 0.19869(10) 0.0231(5) Uani 1 1 d . . . C14 C 0.9176(2) 0.9762(3) 0.14606(10) 0.0259(5) Uani 1 1 d . . . H14A H 0.8630 1.0386 0.1251 0.031 Uiso 1 1 calc R . . H14B H 0.9865 1.0318 0.1553 0.031 Uiso 1 1 calc R . . C15 C 1.0204(2) 0.7614(3) 0.13827(12) 0.0421(7) Uani 1 1 d . . . H15A H 1.0894 0.8111 0.1511 0.063 Uiso 1 1 calc R . . H15B H 1.0369 0.6875 0.1121 0.063 Uiso 1 1 calc R . . H15C H 0.9882 0.7184 0.1697 0.063 Uiso 1 1 calc R . . C16 C 0.74389(18) 0.6447(2) 0.12141(9) 0.0177(5) Uani 1 1 d . . . C17 C 0.75908(19) 0.5500(2) 0.16557(10) 0.0218(5) Uani 1 1 d . . . H17 H 0.7434 0.5805 0.2011 0.026 Uiso 1 1 calc R . . C18 C 0.7963(2) 0.4134(3) 0.15888(11) 0.0297(6) Uani 1 1 d . . . H18 H 0.8065 0.3512 0.1895 0.036 Uiso 1 1 calc R . . C19 C 0.8185(2) 0.3679(3) 0.10708(12) 0.0348(7) Uani 1 1 d . . . H19 H 0.8422 0.2735 0.1017 0.042 Uiso 1 1 calc R . . C20 C 0.8060(2) 0.4604(3) 0.06339(11) 0.0303(6) Uani 1 1 d . . . H20 H 0.8223 0.4288 0.0281 0.036 Uiso 1 1 calc R . . C21 C 0.77021(18) 0.5995(3) 0.06952(9) 0.0198(5) Uani 1 1 d . . . C22 C 0.76292(19) 0.6931(3) 0.01913(9) 0.0223(5) Uani 1 1 d . . . H22A H 0.7149 0.6481 -0.0111 0.027 Uiso 1 1 calc R . . H22B H 0.7296 0.7854 0.0275 0.027 Uiso 1 1 calc R . . C23 C 0.8766(3) 0.7090(4) -0.05572(12) 0.0555(10) Uani 1 1 d . . . H23A H 0.8545 0.6145 -0.0691 0.083 Uiso 1 1 calc R . . H23B H 0.9523 0.7298 -0.0651 0.083 Uiso 1 1 calc R . . H23C H 0.8247 0.7794 -0.0729 0.083 Uiso 1 1 calc R . . Li1 Li 0.9510(3) 0.8832(4) 0.03346(17) 0.0267(9) Uani 1 1 d . . . loop_ _atom_site_aniso_label _atom_site_aniso_U_11 _atom_site_aniso_U_22 _atom_site_aniso_U_33 _atom_site_aniso_U_23 _atom_site_aniso_U_13 _atom_site_aniso_U_12 Br1 0.02170(12) 0.02983(14) 0.02854(14) 0.00323(11) 0.00425(9) 0.00348(11) P1 0.0181(3) 0.0169(3) 0.0144(3) -0.0002(2) 0.0026(2) -0.0009(2) Si1 0.0264(4) 0.0185(3) 0.0294(4) -0.0030(3) 0.0037(3) 0.0045(3) Si2 0.0173(3) 0.0198(3) 0.0216(3) -0.0017(3) 0.0019(2) -0.0012(3) O1 0.0228(9) 0.0280(9) 0.0223(9) 0.0029(7) 0.0062(7) 0.0033(7) O2 0.0250(9) 0.0303(10) 0.0198(9) -0.0028(7) 0.0076(7) -0.0043(7) C1 0.0175(11) 0.0159(11) 0.0170(11) -0.0007(9) 0.0021(9) 0.0012(9) C2 0.0493(19) 0.0435(18) 0.057(2) -0.0134(16) 0.0272(16) 0.0088(15) C3 0.0508(18) 0.0198(14) 0.0556(19) -0.0109(13) -0.0089(15) 0.0062(13) C4 0.0479(18) 0.0245(14) 0.0461(18) 0.0045(13) -0.0079(14) 0.0017(13) C5 0.0296(14) 0.0446(17) 0.0241(14) -0.0033(12) 0.0018(11) -0.0022(12) C6 0.0222(13) 0.0313(14) 0.0364(15) 0.0019(12) 0.0035(11) -0.0008(11) C7 0.0271(13) 0.0190(13) 0.0455(16) -0.0055(11) -0.0013(12) -0.0027(11) C8 0.0222(12) 0.0176(11) 0.0178(11) -0.0028(9) 0.0003(9) 0.0007(9) C9 0.0272(13) 0.0268(13) 0.0204(12) -0.0009(10) 0.0037(10) -0.0048(10) C10 0.0404(16) 0.0408(16) 0.0156(12) -0.0021(11) 0.0025(11) -0.0037(12) C11 0.0433(17) 0.0471(18) 0.0211(13) -0.0092(12) -0.0063(12) -0.0073(14) C12 0.0296(14) 0.0398(16) 0.0275(14) -0.0076(12) -0.0024(11) -0.0105(12) C13 0.0271(12) 0.0214(12) 0.0205(12) -0.0039(9) 0.0010(10) -0.0030(10) C14 0.0260(13) 0.0251(13) 0.0271(13) -0.0027(10) 0.0046(10) -0.0088(11) C15 0.0328(15) 0.057(2) 0.0374(17) 0.0109(15) 0.0083(13) 0.0193(14) C16 0.0141(10) 0.0203(11) 0.0187(11) -0.0013(9) 0.0019(9) -0.0016(9) C17 0.0227(12) 0.0229(12) 0.0201(12) 0.0020(9) 0.0036(9) 0.0006(10) C18 0.0305(14) 0.0237(13) 0.0349(15) 0.0092(11) 0.0032(11) 0.0044(11) C19 0.0390(16) 0.0216(13) 0.0449(17) 0.0005(12) 0.0102(13) 0.0109(11) C20 0.0349(15) 0.0280(14) 0.0296(14) -0.0046(11) 0.0107(11) 0.0061(12) C21 0.0150(10) 0.0233(12) 0.0214(12) -0.0018(10) 0.0035(9) 0.0004(9) C22 0.0201(11) 0.0292(13) 0.0178(12) -0.0014(10) 0.0037(9) 0.0005(10) C23 0.055(2) 0.081(3) 0.0341(17) -0.0199(17) 0.0220(15) -0.0290(19) Li1 0.028(2) 0.026(2) 0.026(2) 0.0015(18) 0.0069(17) -0.0010(18) _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 Br1 Li1 2.482(4) . ? Br1 Li1 2.465(4) 3_775 ? P1 C1 1.854(2) . ? P1 C8 1.854(2) . ? P1 C16 1.855(2) . ? Si1 C1 1.906(2) . ? Si1 C2 1.877(3) . ? Si1 C3 1.872(3) . ? Si1 C4 1.858(3) . ? Si2 C1 1.908(2) . ? Si2 C5 1.867(3) . ? Si2 C6 1.867(2) . ? Si2 C7 1.871(3) . ? O1 C14 1.433(3) . ? O1 C15 1.427(3) . ? O1 Li1 1.940(4) . ? O2 C22 1.448(3) . ? O2 C23 1.427(3) . ? O2 Li1 1.963(5) . ? C8 C9 1.393(3) . ? C8 C13 1.412(3) . ? C9 C10 1.380(3) . ? C10 C11 1.377(4) . ? C11 C12 1.385(4) . ? C12 C13 1.395(3) . ? C13 C14 1.509(3) . ? C16 C17 1.401(3) . ? C16 C21 1.401(3) . ? C17 C18 1.382(3) . ? C18 C19 1.386(4) . ? C19 C20 1.377(4) . ? C20 C21 1.396(3) . ? C21 C22 1.512(3) . ? Li1 Br1 2.465(4) 3_775 ? Li1 Li1 3.050(8) 3_775 ? 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 Li1 Br1 Li1 76.12(15) . 3_775 ? C1 P1 C8 103.51(10) . . ? C1 P1 C16 104.16(10) . . ? C8 P1 C16 98.09(10) . . ? C1 Si1 C2 109.67(12) . . ? C1 Si1 C3 113.37(12) . . ? C1 Si1 C4 110.86(12) . . ? C2 Si1 C3 105.21(15) . . ? C2 Si1 C4 111.35(15) . . ? C3 Si1 C4 106.25(14) . . ? C1 Si2 C5 112.61(11) . . ? C1 Si2 C6 110.23(11) . . ? C1 Si2 C7 111.20(11) . . ? C5 Si2 C6 108.04(12) . . ? C5 Si2 C7 110.09(13) . . ? C6 Si2 C7 104.30(12) . . ? C14 O1 C15 113.7(2) . . ? C14 O1 Li1 121.29(19) . . ? C15 O1 Li1 115.4(2) . . ? C22 O2 C23 112.4(2) . . ? C22 O2 Li1 114.76(18) . . ? C23 O2 Li1 111.0(2) . . ? P1 C1 Si1 107.42(11) . . ? P1 C1 Si2 114.99(11) . . ? Si1 C1 Si2 113.34(11) . . ? P1 C8 C9 123.84(18) . . ? P1 C8 C13 118.60(17) . . ? C9 C8 C13 117.6(2) . . ? C8 C9 C10 122.3(2) . . ? C9 C10 C11 119.9(2) . . ? C10 C11 C12 119.3(2) . . ? C11 C12 C13 121.4(2) . . ? C8 C13 C12 119.5(2) . . ? C8 C13 C14 121.7(2) . . ? C12 C13 C14 118.8(2) . . ? O1 C14 C13 113.6(2) . . ? P1 C16 C17 120.41(17) . . ? P1 C16 C21 121.07(18) . . ? C17 C16 C21 118.5(2) . . ? C16 C17 C18 121.8(2) . . ? C17 C18 C19 119.4(2) . . ? C18 C19 C20 119.6(2) . . ? C19 C20 C21 121.8(2) . . ? C16 C21 C20 118.8(2) . . ? C16 C21 C22 123.9(2) . . ? C20 C21 C22 117.3(2) . . ? O2 C22 C21 108.85(18) . . ? Br1 Li1 Br1 103.88(15) . 3_775 ? Br1 Li1 O1 115.2(2) . . ? Br1 Li1 O1 113.69(19) 3_775 . ? Br1 Li1 O2 111.37(19) . . ? Br1 Li1 O2 110.21(19) 3_775 . ? Br1 Li1 Li1 52.19(13) 3_775 3_775 ? Br1 Li1 Li1 51.69(12) . 3_775 ? O1 Li1 O2 102.7(2) . . ? O1 Li1 Li1 132.1(3) . 3_775 ? O2 Li1 Li1 125.2(3) . 3_775 ? _diffrn_measured_fraction_theta_max 0.936 _diffrn_reflns_theta_full 28.51 _diffrn_measured_fraction_theta_full 0.936 _refine_diff_density_max 0.784 _refine_diff_density_min -0.489 _refine_diff_density_rms 0.071 #===END data_ki135_14 _database_code_depnum_ccdc_archive 'CCDC 263837' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C46 H72 Na2 O4 P2 Si4' _chemical_formula_sum 'C46 H72 Na2 O4 P2 Si4' _chemical_formula_weight 909.32 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' O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' Na Na 0.0362 0.0249 '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 triclinic _symmetry_space_group_name_H-M 'P -1' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x, -y, -z' _cell_length_a 9.235(4) _cell_length_b 11.043(4) _cell_length_c 13.945(7) _cell_angle_alpha 85.58(4) _cell_angle_beta 80.06(4) _cell_angle_gamma 69.33(3) _cell_volume 1310.4(10) _cell_formula_units_Z 1 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 6989 _cell_measurement_theta_min 2.37 _cell_measurement_theta_max 28.85 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.50 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.20 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.152 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 488 _exptl_absorpt_coefficient_mu 0.229 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.894 _exptl_absorpt_correction_T_max 0.956 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 7484 _diffrn_reflns_av_R_equivalents 0.0175 _diffrn_reflns_av_sigmaI/netI 0.0301 _diffrn_reflns_limit_h_min -10 _diffrn_reflns_limit_h_max 10 _diffrn_reflns_limit_k_min -13 _diffrn_reflns_limit_k_max 13 _diffrn_reflns_limit_l_min -12 _diffrn_reflns_limit_l_max 16 _diffrn_reflns_theta_min 1.97 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4388 _reflns_number_gt 3805 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0380P)^2^+0.5617P] 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 4388 _refine_ls_number_parameters 270 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0382 _refine_ls_R_factor_gt 0.0318 _refine_ls_wR_factor_ref 0.0834 _refine_ls_wR_factor_gt 0.0796 _refine_ls_goodness_of_fit_ref 1.042 _refine_ls_restrained_S_all 1.042 _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 P1 P 0.15837(5) 0.33657(4) 0.19452(3) 0.01873(12) Uani 1 1 d . . . Si1 Si 0.00094(6) 0.14211(5) 0.26044(4) 0.02264(13) Uani 1 1 d . . . Si2 Si 0.32822(6) 0.09417(5) 0.32219(4) 0.02330(13) Uani 1 1 d . . . Na1 Na -0.10798(8) 0.50763(7) 0.12212(5) 0.02529(17) Uani 1 1 d . . . O1 O 0.06658(14) 0.60995(11) 0.02828(9) 0.0237(3) Uani 1 1 d . . . O2 O -0.15601(15) 0.59571(12) 0.27497(10) 0.0316(3) Uani 1 1 d . . . C1 C 0.17588(19) 0.18538(16) 0.24982(13) 0.0207(4) Uani 1 1 d . . . C2 C -0.1689(2) 0.27019(19) 0.21070(16) 0.0315(5) Uani 1 1 d . . . H2A H -0.1986 0.3507 0.2462 0.047 Uiso 1 1 calc R . . H2B H -0.2584 0.2402 0.2188 0.047 Uiso 1 1 calc R . . H2C H -0.1375 0.2858 0.1414 0.047 Uiso 1 1 calc R . . C3 C -0.0876(2) 0.1178(2) 0.38971(16) 0.0416(5) Uani 1 1 d . . . H3A H -0.0095 0.0502 0.4220 0.062 Uiso 1 1 calc R . . H3B H -0.1785 0.0917 0.3893 0.062 Uiso 1 1 calc R . . H3C H -0.1208 0.1990 0.4250 0.062 Uiso 1 1 calc R . . C4 C 0.0315(3) -0.0099(2) 0.19501(18) 0.0413(5) Uani 1 1 d . . . H4A H 0.0751 -0.0020 0.1266 0.062 Uiso 1 1 calc R . . H4B H -0.0691 -0.0228 0.1989 0.062 Uiso 1 1 calc R . . H4C H 0.1043 -0.0842 0.2255 0.062 Uiso 1 1 calc R . . C5 C 0.3025(3) 0.1665(2) 0.44406(16) 0.0444(6) Uani 1 1 d . . . H5A H 0.3039 0.2550 0.4350 0.067 Uiso 1 1 calc R . . H5B H 0.3880 0.1142 0.4789 0.067 Uiso 1 1 calc R . . H5C H 0.2021 0.1682 0.4820 0.067 Uiso 1 1 calc R . . C6 C 0.5343(2) 0.0748(2) 0.26224(18) 0.0401(5) Uani 1 1 d . . . H6A H 0.5649 0.0154 0.2077 0.060 Uiso 1 1 calc R . . H6B H 0.6061 0.0397 0.3098 0.060 Uiso 1 1 calc R . . H6C H 0.5390 0.1593 0.2381 0.060 Uiso 1 1 calc R . . C7 C 0.3332(2) -0.07768(18) 0.35003(15) 0.0315(4) Uani 1 1 d . . . H7A H 0.2293 -0.0764 0.3815 0.047 Uiso 1 1 calc R . . H7B H 0.4099 -0.1198 0.3937 0.047 Uiso 1 1 calc R . . H7C H 0.3631 -0.1258 0.2893 0.047 Uiso 1 1 calc R . . C8 C 0.30862(19) 0.32513(16) 0.08411(13) 0.0203(4) Uani 1 1 d . . . C9 C 0.3984(2) 0.20305(17) 0.04628(14) 0.0265(4) Uani 1 1 d . . . H9 H 0.3952 0.1282 0.0837 0.032 Uiso 1 1 calc R . . C10 C 0.4923(2) 0.18792(19) -0.04450(15) 0.0323(5) Uani 1 1 d . . . H10 H 0.5523 0.1036 -0.0681 0.039 Uiso 1 1 calc R . . C11 C 0.4982(2) 0.29580(19) -0.10050(14) 0.0304(4) Uani 1 1 d . . . H11 H 0.5615 0.2861 -0.1628 0.036 Uiso 1 1 calc R . . C12 C 0.4102(2) 0.41855(18) -0.06440(13) 0.0256(4) Uani 1 1 d . . . H12 H 0.4150 0.4925 -0.1026 0.031 Uiso 1 1 calc R . . C13 C 0.31524(19) 0.43567(16) 0.02643(13) 0.0210(4) Uani 1 1 d . . . C14 C 0.2206(2) 0.57354(16) 0.05642(14) 0.0236(4) Uani 1 1 d . . . H14A H 0.2103 0.5808 0.1278 0.028 Uiso 1 1 calc R . . H14B H 0.2746 0.6325 0.0244 0.028 Uiso 1 1 calc R . . C15 C -0.0198(2) 0.74579(18) 0.04580(16) 0.0357(5) Uani 1 1 d . . . H15A H -0.0353 0.7622 0.1156 0.054 Uiso 1 1 calc R . . H15B H -0.1219 0.7697 0.0241 0.054 Uiso 1 1 calc R . . H15C H 0.0393 0.7976 0.0096 0.054 Uiso 1 1 calc R . . C16 C 0.2122(2) 0.43605(15) 0.27337(13) 0.0204(4) Uani 1 1 d . . . C17 C 0.3643(2) 0.43582(17) 0.26878(14) 0.0241(4) Uani 1 1 d . . . H17 H 0.4461 0.3816 0.2234 0.029 Uiso 1 1 calc R . . C18 C 0.3991(2) 0.51255(18) 0.32864(14) 0.0311(4) Uani 1 1 d . . . H18 H 0.5037 0.5105 0.3245 0.037 Uiso 1 1 calc R . . C19 C 0.2810(2) 0.59223(19) 0.39454(15) 0.0354(5) Uani 1 1 d . . . H19 H 0.3041 0.6459 0.4353 0.042 Uiso 1 1 calc R . . C20 C 0.1290(2) 0.59379(18) 0.40101(15) 0.0313(4) Uani 1 1 d . . . H20 H 0.0485 0.6481 0.4470 0.038 Uiso 1 1 calc R . . C21 C 0.0925(2) 0.51748(16) 0.34152(13) 0.0237(4) Uani 1 1 d . . . C22 C -0.0741(2) 0.52121(18) 0.35166(14) 0.0280(4) Uani 1 1 d . . . H22A H -0.0740 0.4315 0.3514 0.034 Uiso 1 1 calc R . . H22B H -0.1316 0.5590 0.4152 0.034 Uiso 1 1 calc R . . C23 C -0.2262(3) 0.7310(2) 0.29526(17) 0.0465(6) Uani 1 1 d . . . H23A H -0.2990 0.7432 0.3568 0.070 Uiso 1 1 calc R . . H23B H -0.2834 0.7760 0.2425 0.070 Uiso 1 1 calc R . . H23C H -0.1444 0.7663 0.3004 0.070 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 0.0194(2) 0.0171(2) 0.0205(2) 0.00061(18) -0.00297(19) -0.00753(17) Si1 0.0229(3) 0.0229(3) 0.0250(3) 0.0040(2) -0.0043(2) -0.0120(2) Si2 0.0231(3) 0.0193(2) 0.0271(3) 0.0013(2) -0.0066(2) -0.0058(2) Na1 0.0256(4) 0.0271(4) 0.0248(4) -0.0002(3) -0.0073(3) -0.0096(3) O1 0.0255(6) 0.0188(6) 0.0282(7) -0.0011(5) -0.0086(6) -0.0070(5) O2 0.0298(7) 0.0297(7) 0.0275(7) -0.0055(6) -0.0070(6) 0.0015(6) C1 0.0212(9) 0.0186(8) 0.0232(9) 0.0014(7) -0.0036(7) -0.0085(7) C2 0.0262(10) 0.0341(11) 0.0393(12) 0.0077(9) -0.0099(9) -0.0163(8) C3 0.0324(11) 0.0577(14) 0.0352(12) 0.0144(11) -0.0030(10) -0.0205(10) C4 0.0430(12) 0.0344(11) 0.0553(15) -0.0052(10) -0.0123(11) -0.0211(10) C5 0.0542(14) 0.0360(12) 0.0386(13) -0.0057(10) -0.0232(11) -0.0016(10) C6 0.0239(10) 0.0318(11) 0.0639(16) 0.0112(10) -0.0110(10) -0.0094(8) C7 0.0305(10) 0.0246(10) 0.0368(12) 0.0066(9) -0.0063(9) -0.0073(8) C8 0.0196(8) 0.0224(9) 0.0219(9) -0.0010(7) -0.0047(7) -0.0100(7) C9 0.0283(10) 0.0237(9) 0.0284(10) -0.0026(8) -0.0022(8) -0.0109(8) C10 0.0310(10) 0.0297(10) 0.0350(12) -0.0106(9) 0.0010(9) -0.0099(8) C11 0.0294(10) 0.0414(12) 0.0222(10) -0.0064(9) 0.0017(8) -0.0159(9) C12 0.0261(9) 0.0323(10) 0.0236(10) 0.0035(8) -0.0064(8) -0.0161(8) C13 0.0199(9) 0.0250(9) 0.0221(10) -0.0002(8) -0.0060(8) -0.0115(7) C14 0.0283(9) 0.0226(9) 0.0254(10) 0.0035(8) -0.0106(8) -0.0135(8) C15 0.0373(11) 0.0215(10) 0.0457(13) -0.0067(9) -0.0107(10) -0.0039(8) C16 0.0261(9) 0.0159(8) 0.0198(9) 0.0035(7) -0.0058(8) -0.0079(7) C17 0.0263(9) 0.0221(9) 0.0247(10) 0.0015(8) -0.0035(8) -0.0097(7) C18 0.0344(11) 0.0340(11) 0.0322(11) 0.0013(9) -0.0082(9) -0.0196(9) C19 0.0487(13) 0.0320(11) 0.0326(12) -0.0067(9) -0.0116(10) -0.0189(10) C20 0.0388(11) 0.0248(10) 0.0263(11) -0.0055(8) -0.0037(9) -0.0056(8) C21 0.0288(10) 0.0196(9) 0.0204(9) 0.0035(7) -0.0048(8) -0.0060(7) C22 0.0270(10) 0.0294(10) 0.0221(10) -0.0019(8) -0.0016(8) -0.0036(8) C23 0.0512(14) 0.0343(12) 0.0376(13) -0.0072(10) -0.0108(11) 0.0085(10) _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 Na1 2.8144(16) . ? P1 C1 1.7499(18) . ? P1 C8 1.866(2) . ? P1 C16 1.8501(19) . ? Si1 C1 1.8198(18) . ? Si1 C2 1.897(2) . ? Si1 C3 1.887(2) . ? Si1 C4 1.883(2) . ? Si2 C1 1.829(2) . ? Si2 C5 1.876(2) . ? Si2 C6 1.886(2) . ? Si2 C7 1.893(2) . ? Na1 Na1 3.621(2) 2_565 ? Na1 O1 2.4327(17) . ? Na1 O1 2.4543(18) 2_565 ? Na1 O2 2.3182(18) . ? Na1 C12 2.859(2) 2_565 ? Na1 C13 2.945(2) 2_565 ? O1 Na1 2.4543(18) 2_565 ? O1 C14 1.450(2) . ? O1 C15 1.446(2) . ? O2 C22 1.448(2) . ? O2 C23 1.432(2) . ? C2 H2A 0.980 . ? C2 H2B 0.980 . ? C2 H2C 0.980 . ? C3 H3A 0.980 . ? C3 H3B 0.980 . ? C3 H3C 0.980 . ? C4 H4A 0.980 . ? C4 H4B 0.980 . ? C4 H4C 0.980 . ? C5 H5A 0.980 . ? C5 H5B 0.980 . ? C5 H5C 0.980 . ? C6 H6A 0.980 . ? C6 H6B 0.980 . ? C6 H6C 0.980 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 C9 1.397(3) . ? C8 C13 1.423(2) . ? C9 H9 0.950 . ? C9 C10 1.390(3) . ? C10 H10 0.950 . ? C10 C11 1.386(3) . ? C11 H11 0.950 . ? C11 C12 1.392(3) . ? C12 Na1 2.859(2) 2_565 ? C12 H12 0.950 . ? C12 C13 1.395(3) . ? C13 Na1 2.945(2) 2_565 ? C13 C14 1.513(3) . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C15 H15A 0.980 . ? C15 H15B 0.980 . ? C15 H15C 0.980 . ? C16 C17 1.395(3) . ? C16 C21 1.414(3) . ? C17 H17 0.950 . ? C17 C18 1.383(3) . ? C18 H18 0.950 . ? C18 C19 1.381(3) . ? C19 H19 0.950 . ? C19 C20 1.386(3) . ? C20 H20 0.950 . ? C20 C21 1.384(3) . ? C21 C22 1.507(3) . ? C22 H22A 0.990 . ? C22 H22B 0.990 . ? C23 H23A 0.980 . ? C23 H23B 0.980 . ? C23 H23C 0.980 . ? 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 Na1 P1 C1 125.87(7) . . ? Na1 P1 C8 99.48(7) . . ? Na1 P1 C16 105.12(7) . . ? C1 P1 C8 112.41(9) . . ? C1 P1 C16 110.15(9) . . ? C8 P1 C16 100.62(8) . . ? C1 Si1 C2 114.08(9) . . ? C1 Si1 C3 114.32(10) . . ? C1 Si1 C4 114.08(10) . . ? C2 Si1 C3 102.67(10) . . ? C2 Si1 C4 104.76(10) . . ? C3 Si1 C4 105.76(11) . . ? C1 Si2 C5 113.33(10) . . ? C1 Si2 C6 114.72(10) . . ? C1 Si2 C7 112.65(9) . . ? C5 Si2 C6 106.01(12) . . ? C5 Si2 C7 105.05(11) . . ? C6 Si2 C7 104.15(10) . . ? P1 Na1 Na1 91.72(5) . 2_565 ? P1 Na1 O1 86.48(5) . . ? P1 Na1 O1 96.04(5) . 2_565 ? P1 Na1 O2 81.57(6) . . ? P1 Na1 C12 155.09(5) . 2_565 ? P1 Na1 C13 147.97(5) . 2_565 ? Na1 Na1 O1 42.41(4) 2_565 . ? Na1 Na1 O1 41.95(4) 2_565 2_565 ? Na1 Na1 O2 145.11(5) 2_565 . ? Na1 Na1 C12 95.89(6) 2_565 2_565 ? Na1 Na1 C13 68.19(5) 2_565 2_565 ? O1 Na1 O1 84.37(6) . 2_565 ? O1 Na1 O2 102.79(6) . . ? O1 Na1 O2 172.24(5) 2_565 . ? O1 Na1 C12 114.83(6) . 2_565 ? O1 Na1 C12 74.64(6) 2_565 2_565 ? O1 Na1 C13 93.70(6) . 2_565 ? O1 Na1 C13 52.25(5) 2_565 2_565 ? O2 Na1 C12 104.53(7) . 2_565 ? O2 Na1 C13 129.16(6) . 2_565 ? C12 Na1 C13 27.77(5) 2_565 2_565 ? Na1 O1 Na1 95.63(6) . 2_565 ? Na1 O1 C14 115.63(10) . . ? Na1 O1 C14 105.09(10) 2_565 . ? Na1 O1 C15 102.20(11) . . ? Na1 O1 C15 127.47(12) 2_565 . ? C14 O1 C15 110.42(14) . . ? Na1 O2 C22 119.91(11) . . ? Na1 O2 C23 124.79(13) . . ? C22 O2 C23 112.91(15) . . ? P1 C1 Si1 114.43(10) . . ? P1 C1 Si2 124.79(10) . . ? Si1 C1 Si2 118.72(10) . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P1 C8 C9 118.76(13) . . ? P1 C8 C13 122.29(13) . . ? C9 C8 C13 117.85(17) . . ? C8 C9 H9 119.0 . . ? C8 C9 C10 121.97(18) . . ? H9 C9 C10 119.0 . . ? C9 C10 H10 120.0 . . ? C9 C10 C11 120.00(18) . . ? H10 C10 C11 120.0 . . ? C10 C11 H11 120.4 . . ? C10 C11 C12 119.18(18) . . ? H11 C11 C12 120.4 . . ? Na1 C12 C11 107.79(12) 2_565 . ? Na1 C12 H12 82.7 2_565 . ? Na1 C12 C13 79.54(11) 2_565 . ? C11 C12 H12 119.2 . . ? C11 C12 C13 121.64(17) . . ? H12 C12 C13 119.2 . . ? Na1 C13 C8 111.16(11) 2_565 . ? Na1 C13 C12 72.70(11) 2_565 . ? Na1 C13 C14 83.68(10) 2_565 . ? C8 C13 C12 119.35(16) . . ? C8 C13 C14 123.72(16) . . ? C12 C13 C14 116.90(16) . . ? O1 C14 C13 109.34(14) . . ? O1 C14 H14A 109.8 . . ? O1 C14 H14B 109.8 . . ? C13 C14 H14A 109.8 . . ? C13 C14 H14B 109.8 . . ? H14A C14 H14B 108.3 . . ? O1 C15 H15A 109.5 . . ? O1 C15 H15B 109.5 . . ? O1 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? P1 C16 C17 123.53(14) . . ? P1 C16 C21 118.32(13) . . ? C17 C16 C21 118.15(16) . . ? C16 C17 H17 119.2 . . ? C16 C17 C18 121.59(18) . . ? H17 C17 C18 119.2 . . ? C17 C18 H18 120.1 . . ? C17 C18 C19 119.72(18) . . ? H18 C18 C19 120.1 . . ? C18 C19 H19 120.1 . . ? C18 C19 C20 119.88(18) . . ? H19 C19 C20 120.1 . . ? C19 C20 H20 119.5 . . ? C19 C20 C21 121.00(19) . . ? H20 C20 C21 119.5 . . ? C16 C21 C20 119.65(17) . . ? C16 C21 C22 121.09(16) . . ? C20 C21 C22 119.25(17) . . ? O2 C22 C21 113.19(15) . . ? O2 C22 H22A 108.9 . . ? O2 C22 H22B 108.9 . . ? C21 C22 H22A 108.9 . . ? C21 C22 H22B 108.9 . . ? H22A C22 H22B 107.8 . . ? O2 C23 H23A 109.5 . . ? O2 C23 H23B 109.5 . . ? O2 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.954 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.954 _refine_diff_density_max 0.319 _refine_diff_density_min -0.186 _refine_diff_density_rms 0.041 #===END data_ki125_15 _database_code_depnum_ccdc_archive 'CCDC 263838' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H36 K O2 P Si2' _chemical_formula_sum 'C23 H36 K O2 P Si2' _chemical_formula_weight 470.77 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' 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' P P 0.1023 0.0942 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' K K 0.2009 0.2494 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' loop_ _symmetry_equiv_pos_as_xyz 'x, y, z' '-x+1/2, -y, z+1/2' '-x, y+1/2, -z+1/2' 'x+1/2, -y+1/2, -z' _cell_length_a 11.0925(19) _cell_length_b 14.177(3) _cell_length_c 16.388(3) _cell_angle_alpha 90.00 _cell_angle_beta 90.00 _cell_angle_gamma 90.00 _cell_volume 2577.1(8) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 7706 _cell_measurement_theta_min 2.22 _cell_measurement_theta_max 28.36 _exptl_crystal_description block _exptl_crystal_colour orange _exptl_crystal_size_max 0.28 _exptl_crystal_size_mid 0.25 _exptl_crystal_size_min 0.22 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.213 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1008 _exptl_absorpt_coefficient_mu 0.377 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.902 _exptl_absorpt_correction_T_max 0.922 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(2) _diffrn_radiation_wavelength 0.71073 _diffrn_radiation_type MoK\a _diffrn_radiation_source 'sealed tube' _diffrn_radiation_monochromator graphite _diffrn_measurement_device_type 'Bruker SMART 1K CCD diffractometer' _diffrn_measurement_method 'thin-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 13124 _diffrn_reflns_av_R_equivalents 0.0679 _diffrn_reflns_av_sigmaI/netI 0.0832 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -16 _diffrn_reflns_limit_k_max 16 _diffrn_reflns_limit_l_min -19 _diffrn_reflns_limit_l_max 19 _diffrn_reflns_theta_min 1.90 _diffrn_reflns_theta_max 25.00 _reflns_number_total 4511 _reflns_number_gt 3510 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Bruker SMART' _computing_cell_refinement 'Bruker SAINT' _computing_data_reduction 'Bruker SAINT' _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0388P)^2^+0.0000P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.06(7) _refine_ls_number_reflns 4511 _refine_ls_number_parameters 270 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0750 _refine_ls_R_factor_gt 0.0495 _refine_ls_wR_factor_ref 0.1019 _refine_ls_wR_factor_gt 0.0923 _refine_ls_goodness_of_fit_ref 1.071 _refine_ls_restrained_S_all 1.071 _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 P1 P 0.52602(9) 0.48002(7) 0.31684(6) 0.0196(2) Uani 1 1 d . . . K1 K 0.54634(9) 0.22405(7) 0.28072(6) 0.0349(3) Uani 1 1 d . . . Si1 Si 0.38822(11) 0.63449(8) 0.42631(7) 0.0234(3) Uani 1 1 d . . . Si2 Si 0.26354(10) 0.50392(8) 0.29070(7) 0.0251(3) Uani 1 1 d . . . O1 O 0.7517(2) 0.34179(19) 0.27622(18) 0.0314(7) Uani 1 1 d . . . O2 O 0.5729(3) 0.5961(2) 0.13117(18) 0.0441(9) Uani 1 1 d . . . C1 C 0.3982(4) 0.5474(3) 0.3440(2) 0.0225(9) Uani 1 1 d . . . C2 C 0.4474(4) 0.6004(3) 0.5305(2) 0.0377(12) Uani 1 1 d . . . H2A H 0.3958 0.5512 0.5539 0.057 Uiso 1 1 calc R . . H2B H 0.4471 0.6558 0.5662 0.057 Uiso 1 1 calc R . . H2C H 0.5299 0.5764 0.5252 0.057 Uiso 1 1 calc R . . C3 C 0.4674(4) 0.7506(3) 0.4050(2) 0.0295(10) Uani 1 1 d . . . H3A H 0.5456 0.7383 0.3794 0.044 Uiso 1 1 calc R . . H3B H 0.4797 0.7846 0.4564 0.044 Uiso 1 1 calc R . . H3C H 0.4177 0.7889 0.3683 0.044 Uiso 1 1 calc R . . C4 C 0.2273(4) 0.6698(3) 0.4480(3) 0.0412(12) Uani 1 1 d . . . H4A H 0.1852 0.6816 0.3965 0.062 Uiso 1 1 calc R . . H4B H 0.2266 0.7272 0.4813 0.062 Uiso 1 1 calc R . . H4C H 0.1867 0.6188 0.4776 0.062 Uiso 1 1 calc R . . C5 C 0.1320(4) 0.4723(3) 0.3591(3) 0.0473(13) Uani 1 1 d . . . H5A H 0.1619 0.4400 0.4079 0.071 Uiso 1 1 calc R . . H5B H 0.0766 0.4307 0.3296 0.071 Uiso 1 1 calc R . . H5C H 0.0895 0.5300 0.3752 0.071 Uiso 1 1 calc R . . C6 C 0.1977(4) 0.5880(3) 0.2137(3) 0.0413(12) Uani 1 1 d . . . H6A H 0.1902 0.6508 0.2382 0.062 Uiso 1 1 calc R . . H6B H 0.1178 0.5656 0.1970 0.062 Uiso 1 1 calc R . . H6C H 0.2506 0.5914 0.1660 0.062 Uiso 1 1 calc R . . C7 C 0.2900(4) 0.3915(3) 0.2326(3) 0.0511(15) Uani 1 1 d . . . H7A H 0.3534 0.4016 0.1919 0.077 Uiso 1 1 calc R . . H7B H 0.2154 0.3725 0.2051 0.077 Uiso 1 1 calc R . . H7C H 0.3151 0.3418 0.2705 0.077 Uiso 1 1 calc R . . C8 C 0.5705(4) 0.4045(3) 0.4062(2) 0.0216(10) Uani 1 1 d . . . C9 C 0.4822(4) 0.3853(3) 0.4639(2) 0.0261(10) Uani 1 1 d . . . H9 H 0.4058 0.4149 0.4583 0.031 Uiso 1 1 calc R . . C10 C 0.5003(4) 0.3251(3) 0.5292(3) 0.0322(11) Uani 1 1 d . . . H10 H 0.4381 0.3151 0.5682 0.039 Uiso 1 1 calc R . . C11 C 0.6097(5) 0.2796(3) 0.5371(3) 0.0363(11) Uani 1 1 d . . . H11 H 0.6243 0.2385 0.5817 0.044 Uiso 1 1 calc R . . C12 C 0.6964(4) 0.2947(3) 0.4797(3) 0.0341(11) Uani 1 1 d . . . H12 H 0.7703 0.2613 0.4844 0.041 Uiso 1 1 calc R . . C13 C 0.6824(4) 0.3564(3) 0.4146(3) 0.0266(10) Uani 1 1 d . . . C14 C 0.7862(4) 0.3682(3) 0.3570(3) 0.0297(11) Uani 1 1 d . . . H14A H 0.8130 0.4348 0.3573 0.036 Uiso 1 1 calc R . . H14B H 0.8545 0.3285 0.3752 0.036 Uiso 1 1 calc R . . C15 C 0.8486(4) 0.3550(3) 0.2203(3) 0.0410(12) Uani 1 1 d . . . H15A H 0.8721 0.4217 0.2198 0.061 Uiso 1 1 calc R . . H15B H 0.8228 0.3361 0.1655 0.061 Uiso 1 1 calc R . . H15C H 0.9175 0.3164 0.2371 0.061 Uiso 1 1 calc R . . C16 C 0.6593(3) 0.5580(3) 0.3144(2) 0.0198(9) Uani 1 1 d . . . C17 C 0.7125(4) 0.5935(3) 0.3851(3) 0.0262(10) Uani 1 1 d . . . H17 H 0.6747 0.5816 0.4361 0.031 Uiso 1 1 calc R . . C18 C 0.8176(4) 0.6451(3) 0.3840(3) 0.0359(12) Uani 1 1 d . . . H18 H 0.8508 0.6690 0.4333 0.043 Uiso 1 1 calc R . . C19 C 0.8742(4) 0.6618(3) 0.3106(3) 0.0467(13) Uani 1 1 d . . . H19 H 0.9475 0.6964 0.3093 0.056 Uiso 1 1 calc R . . C20 C 0.8254(4) 0.6289(3) 0.2401(3) 0.0438(13) Uani 1 1 d . . . H20 H 0.8654 0.6410 0.1899 0.053 Uiso 1 1 calc R . . C21 C 0.7176(4) 0.5777(3) 0.2398(2) 0.0255(10) Uani 1 1 d . . . C22 C 0.6711(4) 0.5402(3) 0.1602(3) 0.0365(12) Uani 1 1 d . . . H21A H 0.7369 0.5405 0.1194 0.044 Uiso 1 1 calc R . . H21B H 0.6441 0.4742 0.1676 0.044 Uiso 1 1 calc R . . C23 C 0.5205(5) 0.5566(4) 0.0592(3) 0.0596(16) Uani 1 1 d . . . H23A H 0.5821 0.5516 0.0166 0.089 Uiso 1 1 calc R . . H23B H 0.4549 0.5974 0.0402 0.089 Uiso 1 1 calc R . . H23C H 0.4885 0.4938 0.0715 0.089 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 0.0166(5) 0.0204(5) 0.0218(5) -0.0018(4) -0.0014(4) -0.0007(5) K1 0.0398(6) 0.0309(5) 0.0339(6) -0.0045(5) 0.0012(5) -0.0050(5) Si1 0.0206(6) 0.0235(6) 0.0261(6) -0.0019(5) 0.0019(5) 0.0001(6) Si2 0.0172(6) 0.0213(6) 0.0369(7) -0.0014(5) -0.0064(5) -0.0007(5) O1 0.0266(17) 0.0305(16) 0.0370(17) -0.0066(14) 0.0074(15) 0.0016(14) O2 0.060(3) 0.042(2) 0.0307(18) 0.0027(15) -0.0065(16) 0.0173(17) C1 0.018(2) 0.021(2) 0.028(2) 0.0036(18) -0.0051(18) 0.0002(19) C2 0.049(3) 0.037(3) 0.027(2) -0.008(2) 0.003(2) 0.002(2) C3 0.033(3) 0.027(2) 0.028(2) -0.0052(19) -0.001(2) 0.000(2) C4 0.032(3) 0.041(3) 0.050(3) -0.009(2) 0.011(2) 0.005(2) C5 0.034(3) 0.040(3) 0.068(4) 0.003(3) -0.006(3) -0.016(3) C6 0.039(3) 0.038(3) 0.046(3) 0.004(2) -0.014(2) -0.001(2) C7 0.031(3) 0.043(3) 0.079(4) -0.029(3) -0.022(3) 0.004(2) C8 0.024(2) 0.016(2) 0.025(2) -0.0050(17) 0.0017(18) -0.0049(18) C9 0.022(2) 0.024(2) 0.032(2) -0.003(2) 0.001(2) -0.0071(19) C10 0.042(3) 0.020(2) 0.035(3) 0.003(2) 0.005(2) -0.009(2) C11 0.060(3) 0.022(2) 0.027(3) 0.008(2) -0.008(2) -0.002(3) C12 0.038(3) 0.026(3) 0.038(3) -0.004(2) -0.009(2) 0.007(2) C13 0.029(3) 0.018(2) 0.032(3) 0.002(2) -0.001(2) -0.002(2) C14 0.022(2) 0.025(2) 0.042(3) 0.000(2) -0.003(2) 0.010(2) C15 0.031(3) 0.034(3) 0.057(3) -0.004(2) 0.020(2) 0.003(2) C16 0.018(2) 0.0098(19) 0.032(2) 0.0017(18) 0.0023(19) 0.0032(17) C17 0.016(2) 0.026(2) 0.036(3) -0.006(2) 0.003(2) 0.0012(19) C18 0.028(3) 0.030(3) 0.050(3) -0.014(2) -0.004(2) -0.003(2) C19 0.030(3) 0.034(3) 0.076(4) -0.003(3) 0.007(3) -0.016(2) C20 0.041(3) 0.035(3) 0.056(4) 0.014(3) 0.020(3) -0.005(2) C21 0.028(2) 0.019(2) 0.029(3) 0.0048(18) 0.009(2) 0.005(2) C22 0.044(3) 0.037(3) 0.029(3) 0.006(2) 0.015(2) 0.009(2) C23 0.085(4) 0.054(3) 0.040(3) 0.000(3) -0.025(3) 0.008(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 P1 K1 3.6836(15) . ? P1 C1 1.767(4) . ? P1 C8 1.879(4) . ? P1 C16 1.846(4) . ? K1 P1 3.8948(15) 3_645 ? K1 O1 2.825(3) . ? K1 O2 2.669(3) 3_645 ? K1 C1 3.291(4) 3_645 ? K1 C8 3.293(4) . ? K1 C13 3.258(4) . ? K1 C14 3.580(4) . ? K1 C16 3.630(4) 3_645 ? K1 C21 3.604(4) 3_645 ? Si1 K1 3.6947(16) 3_655 ? Si1 C1 1.832(4) . ? Si1 C2 1.892(4) . ? Si1 C3 1.898(4) . ? Si1 C4 1.887(4) . ? Si2 C1 1.837(4) . ? Si2 C5 1.894(5) . ? Si2 C6 1.883(4) . ? Si2 C7 1.879(4) . ? O1 C14 1.429(5) . ? O1 C15 1.425(5) . ? O2 K1 2.669(3) 3_655 ? O2 C22 1.429(5) . ? O2 C23 1.429(5) . ? C1 K1 3.291(4) 3_655 ? C2 H2A 0.980 . ? C2 H2B 0.980 . ? C2 H2C 0.980 . ? C3 H3A 0.980 . ? C3 H3B 0.980 . ? C3 H3C 0.980 . ? C4 H4A 0.980 . ? C4 H4B 0.980 . ? C4 H4C 0.980 . ? C5 H5A 0.980 . ? C5 H5B 0.980 . ? C5 H5C 0.980 . ? C6 H6A 0.980 . ? C6 H6B 0.980 . ? C6 H6C 0.980 . ? C7 H7A 0.980 . ? C7 H7B 0.980 . ? C7 H7C 0.980 . ? C8 C9 1.390(5) . ? C8 C13 1.423(5) . ? C9 H9 0.950 . ? C9 C10 1.384(5) . ? C10 H10 0.950 . ? C10 C11 1.380(6) . ? C11 H11 0.950 . ? C11 C12 1.362(6) . ? C12 H12 0.950 . ? C12 C13 1.388(6) . ? C13 C14 1.498(6) . ? C14 H14A 0.990 . ? C14 H14B 0.990 . ? C15 H15A 0.980 . ? C15 H15B 0.980 . ? C15 H15C 0.980 . ? C16 C17 1.394(6) . ? C16 C21 1.411(5) . ? C17 H17 0.950 . ? C17 C18 1.377(6) . ? C18 H18 0.950 . ? C18 C19 1.376(6) . ? C19 H19 0.950 . ? C19 C20 1.358(7) . ? C20 H20 0.950 . ? C20 C21 1.400(6) . ? C21 C22 1.499(6) . ? C22 H21A 0.990 . ? C22 H21B 0.990 . ? C23 H23A 0.980 . ? C23 H23B 0.980 . ? C23 H23C 0.980 . ? 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 K1 P1 C1 128.47(13) . . ? K1 P1 C8 63.14(12) . . ? K1 P1 C16 122.50(12) . . ? C1 P1 C8 108.80(18) . . ? C1 P1 C16 108.94(17) . . ? C8 P1 C16 98.47(17) . . ? P1 K1 P1 158.18(3) . 3_645 ? P1 K1 O1 58.10(6) . . ? P1 K1 O1 132.87(6) 3_645 . ? P1 K1 O2 123.52(8) . 3_645 ? P1 K1 O2 61.07(7) 3_645 3_645 ? P1 K1 C1 149.42(8) . 3_645 ? P1 K1 C1 26.81(7) 3_645 3_645 ? P1 K1 C8 30.60(7) . . ? P1 K1 C8 164.41(8) 3_645 . ? P1 K1 C13 49.67(7) . . ? P1 K1 C13 152.07(8) 3_645 . ? P1 K1 C14 55.04(7) . . ? P1 K1 C14 143.48(7) 3_645 . ? P1 K1 C16 132.03(7) . 3_645 ? P1 K1 C16 28.12(6) 3_645 3_645 ? P1 K1 C21 122.17(7) . 3_645 ? P1 K1 C21 44.18(7) 3_645 3_645 ? O1 K1 O2 144.61(10) . 3_645 ? O1 K1 C1 106.42(9) . 3_645 ? O1 K1 C8 59.44(9) . . ? O1 K1 C13 45.87(9) . . ? O1 K1 C14 21.98(9) . . ? O1 K1 C16 151.49(9) . 3_645 ? O1 K1 C21 173.10(9) . 3_645 ? O2 K1 C1 84.92(10) 3_645 3_645 ? O2 K1 C8 103.34(10) 3_645 . ? O2 K1 C13 104.87(10) 3_645 . ? O2 K1 C14 124.55(10) 3_645 . ? O2 K1 C16 58.67(9) 3_645 3_645 ? O2 K1 C21 41.97(9) 3_645 3_645 ? C1 K1 C8 164.54(10) 3_645 . ? C1 K1 C13 140.36(10) 3_645 . ? C1 K1 C14 120.83(10) 3_645 . ? C1 K1 C16 49.99(9) 3_645 3_645 ? C1 K1 C21 69.87(10) 3_645 3_645 ? C8 K1 C13 25.08(9) . . ? C8 K1 C14 43.76(9) . . ? C8 K1 C16 145.42(10) . 3_645 ? C8 K1 C21 124.87(10) . 3_645 ? C13 K1 C14 24.73(10) . . ? C13 K1 C16 162.54(10) . 3_645 ? C13 K1 C21 140.41(10) . 3_645 ? C14 K1 C16 170.82(9) . 3_645 ? C14 K1 C21 164.74(10) . 3_645 ? C16 K1 C21 22.50(8) 3_645 3_645 ? K1 Si1 C1 62.86(13) 3_655 . ? K1 Si1 C2 148.05(15) 3_655 . ? K1 Si1 C3 56.11(12) 3_655 . ? K1 Si1 C4 105.54(16) 3_655 . ? C1 Si1 C2 118.09(19) . . ? C1 Si1 C3 114.93(18) . . ? C1 Si1 C4 112.0(2) . . ? C2 Si1 C3 103.1(2) . . ? C2 Si1 C4 103.0(2) . . ? C3 Si1 C4 104.0(2) . . ? C1 Si2 C5 115.1(2) . . ? C1 Si2 C6 114.95(19) . . ? C1 Si2 C7 113.46(19) . . ? C5 Si2 C6 104.3(2) . . ? C5 Si2 C7 102.7(2) . . ? C6 Si2 C7 105.0(2) . . ? K1 O1 C14 110.3(2) . . ? K1 O1 C15 134.7(2) . . ? C14 O1 C15 111.1(3) . . ? K1 O2 C22 125.1(2) 3_655 . ? K1 O2 C23 120.7(3) 3_655 . ? C22 O2 C23 111.6(3) . . ? P1 C1 K1 96.01(16) . 3_655 ? P1 C1 Si1 126.8(2) . . ? P1 C1 Si2 110.6(2) . . ? K1 C1 Si1 87.45(14) 3_655 . ? K1 C1 Si2 96.41(15) 3_655 . ? Si1 C1 Si2 121.8(2) . . ? Si1 C2 H2A 109.5 . . ? Si1 C2 H2B 109.5 . . ? Si1 C2 H2C 109.5 . . ? H2A C2 H2B 109.5 . . ? H2A C2 H2C 109.5 . . ? H2B C2 H2C 109.5 . . ? Si1 C3 H3A 109.5 . . ? Si1 C3 H3B 109.5 . . ? Si1 C3 H3C 109.5 . . ? H3A C3 H3B 109.5 . . ? H3A C3 H3C 109.5 . . ? H3B C3 H3C 109.5 . . ? Si1 C4 H4A 109.5 . . ? Si1 C4 H4B 109.5 . . ? Si1 C4 H4C 109.5 . . ? H4A C4 H4B 109.5 . . ? H4A C4 H4C 109.5 . . ? H4B C4 H4C 109.5 . . ? Si2 C5 H5A 109.5 . . ? Si2 C5 H5B 109.5 . . ? Si2 C5 H5C 109.5 . . ? H5A C5 H5B 109.5 . . ? H5A C5 H5C 109.5 . . ? H5B C5 H5C 109.5 . . ? Si2 C6 H6A 109.5 . . ? Si2 C6 H6B 109.5 . . ? Si2 C6 H6C 109.5 . . ? H6A C6 H6B 109.5 . . ? H6A C6 H6C 109.5 . . ? H6B C6 H6C 109.5 . . ? Si2 C7 H7A 109.5 . . ? Si2 C7 H7B 109.5 . . ? Si2 C7 H7C 109.5 . . ? H7A C7 H7B 109.5 . . ? H7A C7 H7C 109.5 . . ? H7B C7 H7C 109.5 . . ? P1 C8 K1 86.25(13) . . ? P1 C8 C9 117.2(3) . . ? P1 C8 C13 125.3(3) . . ? K1 C8 C9 102.4(2) . . ? K1 C8 C13 76.1(2) . . ? C9 C8 C13 117.0(4) . . ? C8 C9 H9 118.5 . . ? C8 C9 C10 123.1(4) . . ? H9 C9 C10 118.5 . . ? C9 C10 H10 120.4 . . ? C9 C10 C11 119.2(4) . . ? H10 C10 C11 120.4 . . ? C10 C11 H11 120.5 . . ? C10 C11 C12 118.9(4) . . ? H11 C11 C12 120.5 . . ? C11 C12 H12 118.3 . . ? C11 C12 C13 123.4(4) . . ? H12 C12 C13 118.3 . . ? K1 C13 C8 78.9(2) . . ? K1 C13 C12 101.9(3) . . ? K1 C13 C14 89.8(2) . . ? C8 C13 C12 118.3(4) . . ? C8 C13 C14 123.7(4) . . ? C12 C13 C14 117.9(4) . . ? K1 C14 O1 47.75(18) . . ? K1 C14 C13 65.5(2) . . ? K1 C14 H14A 140.3 . . ? K1 C14 H14B 110.4 . . ? O1 C14 C13 110.4(3) . . ? O1 C14 H14A 109.6 . . ? O1 C14 H14B 109.6 . . ? C13 C14 H14A 109.6 . . ? C13 C14 H14B 109.6 . . ? H14A C14 H14B 108.1 . . ? O1 C15 H15A 109.5 . . ? O1 C15 H15B 109.5 . . ? O1 C15 H15C 109.5 . . ? H15A C15 H15B 109.5 . . ? H15A C15 H15C 109.5 . . ? H15B C15 H15C 109.5 . . ? P1 C16 C17 122.5(3) . . ? P1 C16 C21 120.3(3) . . ? C17 C16 C21 117.0(4) . . ? C16 C17 H17 118.7 . . ? C16 C17 C18 122.7(4) . . ? H17 C17 C18 118.7 . . ? C17 C18 H18 120.4 . . ? C17 C18 C19 119.3(4) . . ? H18 C18 C19 120.4 . . ? C18 C19 H19 119.9 . . ? C18 C19 C20 120.1(4) . . ? H19 C19 C20 119.9 . . ? C19 C20 H20 119.3 . . ? C19 C20 C21 121.5(4) . . ? H20 C20 C21 119.3 . . ? C16 C21 C20 119.4(4) . . ? C16 C21 C22 121.7(4) . . ? C20 C21 C22 118.8(4) . . ? O2 C22 C21 110.8(3) . . ? O2 C22 H21A 109.5 . . ? O2 C22 H21B 109.5 . . ? C21 C22 H21A 109.5 . . ? C21 C22 H21B 109.5 . . ? H21A C22 H21B 108.1 . . ? O2 C23 H23A 109.5 . . ? O2 C23 H23B 109.5 . . ? O2 C23 H23C 109.5 . . ? H23A C23 H23B 109.5 . . ? H23A C23 H23C 109.5 . . ? H23B C23 H23C 109.5 . . ? _diffrn_measured_fraction_theta_max 0.998 _diffrn_reflns_theta_full 25.00 _diffrn_measured_fraction_theta_full 0.998 _refine_diff_density_max 0.319 _refine_diff_density_min -0.276 _refine_diff_density_rms 0.066 #===END data_ki151_16 _database_code_depnum_ccdc_archive 'CCDC 263839' _audit_creation_method SHELXL-97 _chemical_name_systematic ; ? ; _chemical_name_common ? _chemical_melting_point ? _chemical_formula_moiety 'C23 H36 O2 P Rb Si2' _chemical_formula_sum 'C23 H36 O2 P Rb Si2' _chemical_formula_weight 517.14 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' 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' Rb Rb -0.9393 2.9676 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4' _symmetry_cell_setting orthorhombic _symmetry_space_group_name_H-M 'P 21 21 21' 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 11.122(1) _cell_length_b 14.430(1) _cell_length_c 16.248(1) _cell_angle_alpha 90.0 _cell_angle_beta 90.0 _cell_angle_gamma 90.0 _cell_volume 2607.6(3) _cell_formula_units_Z 4 _cell_measurement_temperature 150(2) _cell_measurement_reflns_used 21505 _cell_measurement_theta_min 3.93 _cell_measurement_theta_max 27.5 _exptl_crystal_description block _exptl_crystal_colour yellow _exptl_crystal_size_max 0.20 _exptl_crystal_size_mid 0.20 _exptl_crystal_size_min 0.10 _exptl_crystal_density_meas ? _exptl_crystal_density_diffrn 1.317 _exptl_crystal_density_method 'not measured' _exptl_crystal_F_000 1080 _exptl_absorpt_coefficient_mu 2.068 _exptl_absorpt_correction_type multi-scan _exptl_absorpt_correction_T_min 0.683 _exptl_absorpt_correction_T_max 0.820 _exptl_absorpt_process_details SADABS _exptl_special_details ; ? ; _diffrn_ambient_temperature 150(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 'Nonius KappaCCD diffractometer' _diffrn_measurement_method 'thick-slice \w scans' _diffrn_detector_area_resol_mean ? _diffrn_standards_number 0 _diffrn_standards_interval_count ? _diffrn_standards_interval_time ? _diffrn_standards_decay_% ? _diffrn_reflns_number 20240 _diffrn_reflns_av_R_equivalents 0.0498 _diffrn_reflns_av_sigmaI/netI 0.0657 _diffrn_reflns_limit_h_min -13 _diffrn_reflns_limit_h_max 13 _diffrn_reflns_limit_k_min -17 _diffrn_reflns_limit_k_max 18 _diffrn_reflns_limit_l_min -20 _diffrn_reflns_limit_l_max 20 _diffrn_reflns_theta_min 4.12 _diffrn_reflns_theta_max 26.37 _reflns_number_total 5239 _reflns_number_gt 4121 _reflns_threshold_expression I>2\s(I) _computing_data_collection 'Nonius COLLECT' _computing_cell_refinement EvalCCD _computing_data_reduction EvalCCD _computing_structure_solution 'Bruker SHELXTL' _computing_structure_refinement 'Bruker SHELXTL' _computing_molecular_graphics 'Bruker SHELXTL' _computing_publication_material 'Bruker SHELXTL and local programs' _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^)+(0.0206P)^2^+0.3920P] 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_abs_structure_details 'Flack H D (1983), Acta Cryst. A39, 876-881' _refine_ls_abs_structure_Flack -0.014(5) _refine_ls_number_reflns 5239 _refine_ls_number_parameters 270 _refine_ls_number_restraints 0 _refine_ls_R_factor_all 0.0657 _refine_ls_R_factor_gt 0.0370 _refine_ls_wR_factor_ref 0.0606 _refine_ls_wR_factor_gt 0.0541 _refine_ls_goodness_of_fit_ref 1.064 _refine_ls_restrained_S_all 1.064 _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 Rb1 Rb 0.53798(3) 0.27619(2) 0.288588(19) 0.02995(9) Uani 1 1 d . . . P1 P 0.52748(8) 0.01998(5) 0.31939(4) 0.01761(18) Uani 1 1 d . . . Si1 Si 0.38898(9) -0.13307(6) 0.42776(5) 0.0212(2) Uani 1 1 d . . . Si2 Si 0.26562(8) -0.00394(5) 0.29130(6) 0.0214(2) Uani 1 1 d . . . O1 O 0.75704(19) 0.15832(13) 0.28203(14) 0.0275(5) Uani 1 1 d . . . O2 O 0.5817(2) -0.08417(15) 0.12629(13) 0.0356(7) Uani 1 1 d . . . C1 C 0.3996(3) -0.04710(19) 0.34480(18) 0.0178(7) Uani 1 1 d . . . C2 C 0.4677(4) -0.24771(18) 0.40681(18) 0.0292(8) Uani 1 1 d . . . H2A H 0.4187 -0.2850 0.3692 0.044 Uiso 1 1 calc R . . H2B H 0.4786 -0.2813 0.4587 0.044 Uiso 1 1 calc R . . H2C H 0.5463 -0.2359 0.3817 0.044 Uiso 1 1 calc R . . C3 C 0.2282(3) -0.1688(2) 0.4483(2) 0.0360(9) Uani 1 1 d . . . H3A H 0.1875 -0.1202 0.4800 0.054 Uiso 1 1 calc R . . H3B H 0.2274 -0.2268 0.4797 0.054 Uiso 1 1 calc R . . H3C H 0.1862 -0.1780 0.3959 0.054 Uiso 1 1 calc R . . C4 C 0.4480(4) -0.0991(2) 0.53262(17) 0.0331(9) Uani 1 1 d . . . H4A H 0.5309 -0.0768 0.5274 0.050 Uiso 1 1 calc R . . H4B H 0.4462 -0.1531 0.5692 0.050 Uiso 1 1 calc R . . H4C H 0.3976 -0.0499 0.5557 0.050 Uiso 1 1 calc R . . C5 C 0.2911(3) 0.1070(2) 0.2328(2) 0.0419(11) Uani 1 1 d . . . H5A H 0.3057 0.1577 0.2718 0.063 Uiso 1 1 calc R . . H5B H 0.2198 0.1212 0.1997 0.063 Uiso 1 1 calc R . . H5C H 0.3610 0.0999 0.1967 0.063 Uiso 1 1 calc R . . C6 C 0.1336(3) 0.0259(2) 0.3594(2) 0.0391(9) Uani 1 1 d . . . H6A H 0.0917 -0.0311 0.3754 0.059 Uiso 1 1 calc R . . H6B H 0.0781 0.0664 0.3293 0.059 Uiso 1 1 calc R . . H6C H 0.1624 0.0579 0.4088 0.059 Uiso 1 1 calc R . . C7 C 0.2017(3) -0.0863(2) 0.2123(2) 0.0338(9) Uani 1 1 d . . . H7A H 0.2540 -0.0874 0.1637 0.051 Uiso 1 1 calc R . . H7B H 0.1212 -0.0656 0.1962 0.051 Uiso 1 1 calc R . . H7C H 0.1968 -0.1487 0.2358 0.051 Uiso 1 1 calc R . . C8 C 0.5721(3) 0.09205(19) 0.41041(17) 0.0184(7) Uani 1 1 d . . . C9 C 0.4808(3) 0.11347(18) 0.46648(17) 0.0214(7) Uani 1 1 d . . . H9 H 0.4048 0.0843 0.4602 0.026 Uiso 1 1 calc R . . C10 C 0.4964(3) 0.1753(2) 0.53071(18) 0.0257(9) Uani 1 1 d . . . H10 H 0.4326 0.1865 0.5683 0.031 Uiso 1 1 calc R . . C11 C 0.6047(3) 0.2204(2) 0.54004(18) 0.0302(8) Uani 1 1 d . . . H11 H 0.6162 0.2631 0.5838 0.036 Uiso 1 1 calc R . . C12 C 0.6965(3) 0.2025(2) 0.48481(19) 0.0312(9) Uani 1 1 d . . . H12 H 0.7709 0.2341 0.4912 0.037 Uiso 1 1 calc R . . C13 C 0.6836(3) 0.1396(2) 0.41987(19) 0.0203(7) Uani 1 1 d . . . C14 C 0.7894(3) 0.1274(2) 0.36338(19) 0.0261(8) Uani 1 1 d . . . H14A H 0.8585 0.1639 0.3840 0.031 Uiso 1 1 calc R . . H14B H 0.8132 0.0614 0.3617 0.031 Uiso 1 1 calc R . . C15 C 0.8562(3) 0.1480(2) 0.2269(2) 0.0341(9) Uani 1 1 d . . . H15A H 0.9247 0.1841 0.2473 0.051 Uiso 1 1 calc R . . H15B H 0.8332 0.1705 0.1722 0.051 Uiso 1 1 calc R . . H15C H 0.8787 0.0825 0.2235 0.051 Uiso 1 1 calc R . . C16 C 0.6609(3) -0.05616(19) 0.31395(18) 0.0178(7) Uani 1 1 d . . . C17 C 0.7122(3) -0.0961(2) 0.3839(2) 0.0242(8) Uani 1 1 d . . . H17 H 0.6730 -0.0882 0.4354 0.029 Uiso 1 1 calc R . . C18 C 0.8180(3) -0.1467(2) 0.3814(2) 0.0335(9) Uani 1 1 d . . . H18 H 0.8499 -0.1730 0.4304 0.040 Uiso 1 1 calc R . . C19 C 0.8763(4) -0.1587(2) 0.3076(3) 0.0419(10) Uani 1 1 d . . . H19 H 0.9493 -0.1928 0.3054 0.050 Uiso 1 1 calc R . . C20 C 0.8287(3) -0.1212(2) 0.2373(2) 0.0364(10) Uani 1 1 d . . . H20 H 0.8697 -0.1296 0.1865 0.044 Uiso 1 1 calc R . . C21 C 0.7208(3) -0.0705(2) 0.23856(19) 0.0240(8) Uani 1 1 d . . . C22 C 0.6769(3) -0.0284(2) 0.15877(19) 0.0309(9) Uani 1 1 d . . . H22A H 0.6474 0.0354 0.1688 0.037 Uiso 1 1 calc R . . H22B H 0.7438 -0.0252 0.1187 0.037 Uiso 1 1 calc R . . C23 C 0.5321(4) -0.0427(3) 0.0539(2) 0.0510(11) Uani 1 1 d . . . H23A H 0.4964 0.0173 0.0680 0.076 Uiso 1 1 calc R . . H23B H 0.4700 -0.0834 0.0310 0.076 Uiso 1 1 calc R . . H23C H 0.5958 -0.0336 0.0130 0.076 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 Rb1 0.0350(2) 0.02388(16) 0.03100(17) 0.00508(14) 0.00142(18) 0.00340(16) P1 0.0155(5) 0.0184(4) 0.0189(4) 0.0007(3) -0.0009(4) 0.0002(4) Si1 0.0197(6) 0.0219(5) 0.0219(5) 0.0024(4) 0.0013(4) -0.0003(4) Si2 0.0165(5) 0.0197(5) 0.0281(5) 0.0007(4) -0.0034(4) 0.0012(3) O1 0.0238(14) 0.0285(12) 0.0302(13) 0.0078(10) 0.0094(12) 0.0020(9) O2 0.0418(19) 0.0384(14) 0.0264(13) 0.0005(10) -0.0046(12) -0.0134(12) C1 0.0143(19) 0.0197(17) 0.0196(17) -0.0001(12) 0.0016(14) -0.0018(13) C2 0.035(2) 0.027(2) 0.0253(17) 0.0054(12) -0.0008(18) -0.0003(16) C3 0.026(2) 0.037(2) 0.046(2) 0.0168(17) 0.0043(18) -0.0037(17) C4 0.044(3) 0.035(2) 0.0198(17) 0.0030(13) 0.0019(18) 0.0008(18) C5 0.023(2) 0.039(2) 0.064(3) 0.0207(18) -0.015(2) 0.0003(16) C6 0.029(3) 0.039(2) 0.049(2) -0.0026(17) 0.0013(19) 0.0087(17) C7 0.027(2) 0.037(2) 0.037(2) -0.0040(17) -0.010(2) 0.0028(16) C8 0.019(2) 0.0168(16) 0.0193(17) 0.0036(12) 0.0009(14) 0.0036(13) C9 0.019(2) 0.0169(16) 0.0281(17) 0.0033(13) -0.0007(16) 0.0021(14) C10 0.032(3) 0.0208(17) 0.0244(18) 0.0016(13) 0.0045(15) 0.0068(14) C11 0.047(3) 0.0209(17) 0.0232(18) -0.0052(15) -0.0048(17) -0.0007(19) C12 0.033(2) 0.027(2) 0.034(2) -0.0026(14) -0.0060(18) -0.0078(16) C13 0.020(2) 0.0176(17) 0.0239(19) 0.0031(13) -0.0030(15) -0.0008(15) C14 0.022(2) 0.0229(19) 0.033(2) -0.0009(14) -0.0003(17) -0.0081(15) C15 0.029(2) 0.031(2) 0.042(2) 0.0062(15) 0.0147(18) -0.0003(16) C16 0.0161(19) 0.0151(16) 0.0221(18) -0.0012(12) 0.0016(14) -0.0037(13) C17 0.017(2) 0.0260(19) 0.0294(19) 0.0022(14) 0.0018(16) -0.0042(15) C18 0.025(2) 0.025(2) 0.050(3) 0.0102(16) -0.003(2) 0.0002(17) C19 0.029(2) 0.029(2) 0.068(3) -0.0019(18) 0.010(2) 0.0098(16) C20 0.034(3) 0.037(2) 0.039(2) -0.0119(16) 0.0164(19) 0.0002(19) C21 0.021(2) 0.0206(18) 0.030(2) -0.0087(14) 0.0043(15) -0.0053(16) C22 0.035(3) 0.037(2) 0.0211(18) -0.0040(15) 0.0079(16) -0.0129(17) C23 0.065(3) 0.053(2) 0.035(2) 0.0063(17) -0.014(2) -0.006(2) _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 Rb1 P1 3.7328(8) . ? Rb1 O1 2.973(2) . ? Rb1 O2 2.783(2) 4_655 ? Rb1 C1 3.418(3) 4_655 ? Rb1 C2 3.194(3) 4_655 ? Rb1 C7 3.510(3) 4_655 ? Rb1 C8 3.335(3) . ? Rb1 C13 3.326(3) . ? Rb1 C14 3.729(3) . ? Rb1 C16 3.677(3) 4_655 ? Rb1 C21 3.657(3) 4_655 ? Rb1 C23 3.740(3) 4_655 ? P1 Rb1 3.9979(8) 4_645 ? P1 C1 1.769(3) . ? P1 C8 1.875(3) . ? P1 C16 1.849(3) . ? Si1 Rb1 3.8381(10) 4_645 ? Si1 C1 1.836(3) . ? Si1 C2 1.902(3) . ? Si1 C3 1.891(3) . ? Si1 C4 1.891(3) . ? Si2 Rb1 4.0647(9) 4_645 ? Si2 C1 1.834(3) . ? Si2 C5 1.883(3) . ? Si2 C6 1.888(4) . ? Si2 C7 1.889(3) . ? O1 C14 1.440(4) . ? O1 C15 1.428(4) . ? O2 Rb1 2.783(2) 4_645 ? O2 C22 1.430(4) . ? O2 C23 1.431(4) . ? C1 Rb1 3.418(3) 4_645 ? C8 C9 1.399(4) . ? C8 C13 1.425(4) . ? C9 C10 1.383(4) . ? C10 C11 1.378(4) . ? C11 C12 1.383(5) . ? C12 C13 1.399(4) . ? C13 C14 1.502(4) . ? C16 Rb1 3.677(3) 4_645 ? C16 C17 1.396(4) . ? C16 C21 1.410(4) . ? C17 C18 1.385(4) . ? C18 C19 1.374(5) . ? C19 C20 1.371(5) . ? C20 C21 1.405(5) . ? C21 Rb1 3.657(3) 4_645 ? C21 C22 1.513(4) . ? loop_ _geom_angle_atom_site_label_1 _geom_angle_atom_site_label_2 _geom_angle_atom_site_label_3 _geom_angle _geom_angle_site_symmetry_1 _geom_angle_site_symmetry_3 _geom_angle_publ_flag P1 Rb1 O1 57.58(4) . . ? P1 Rb1 O2 129.45(5) . 4_655 ? P1 Rb1 C1 146.14(5) . 4_655 ? P1 Rb1 C2 91.47(5) . 4_655 ? P1 Rb1 C7 125.90(6) . 4_655 ? P1 Rb1 C8 30.10(5) . . ? P1 Rb1 C13 48.86(5) . . ? P1 Rb1 C14 53.81(5) . . ? P1 Rb1 C16 133.91(5) . 4_655 ? P1 Rb1 C21 126.20(6) . 4_655 ? P1 Rb1 C23 126.42(6) . 4_655 ? O1 Rb1 O2 145.49(7) . 4_655 ? O1 Rb1 C1 103.75(7) . 4_655 ? O1 Rb1 C2 85.34(8) . 4_655 ? O1 Rb1 C7 69.35(7) . 4_655 ? O1 Rb1 C8 58.14(7) . . ? O1 Rb1 C13 44.34(7) . . ? O1 Rb1 C14 21.23(6) . . ? O1 Rb1 C16 148.55(6) . 4_655 ? O1 Rb1 C21 170.65(6) . 4_655 ? O1 Rb1 C23 126.51(8) . 4_655 ? O2 Rb1 C1 82.65(7) 4_655 4_655 ? O2 Rb1 C2 124.24(7) 4_655 4_655 ? O2 Rb1 C7 89.27(8) 4_655 4_655 ? O2 Rb1 C8 109.66(7) 4_655 . ? O2 Rb1 C13 110.09(7) 4_655 . ? O2 Rb1 C14 127.85(7) 4_655 . ? O2 Rb1 C16 57.39(6) 4_655 4_655 ? O2 Rb1 C21 41.01(7) 4_655 4_655 ? O2 Rb1 C23 18.98(8) 4_655 4_655 ? C1 Rb1 C2 56.93(7) 4_655 4_655 ? C1 Rb1 C7 53.72(8) 4_655 4_655 ? C1 Rb1 C8 161.38(8) 4_655 . ? C1 Rb1 C13 138.60(8) 4_655 . ? C1 Rb1 C14 118.95(7) 4_655 . ? C1 Rb1 C16 49.00(7) 4_655 4_655 ? C1 Rb1 C21 68.41(7) 4_655 4_655 ? C1 Rb1 C23 87.42(8) 4_655 4_655 ? C2 Rb1 C7 94.21(9) 4_655 4_655 ? C2 Rb1 C8 120.41(7) 4_655 . ? C2 Rb1 C13 125.67(8) 4_655 . ? C2 Rb1 C14 106.06(8) 4_655 . ? C2 Rb1 C16 66.97(7) 4_655 4_655 ? C2 Rb1 C21 85.98(8) 4_655 4_655 ? C2 Rb1 C23 138.73(7) 4_655 4_655 ? C7 Rb1 C8 111.03(8) 4_655 . ? C7 Rb1 C13 86.32(8) 4_655 . ? C7 Rb1 C14 73.03(7) 4_655 . ? C7 Rb1 C16 97.04(7) 4_655 4_655 ? C7 Rb1 C21 107.87(7) 4_655 4_655 ? C7 Rb1 C23 77.26(10) 4_655 4_655 ? C8 Rb1 C13 24.71(7) . . ? C8 Rb1 C14 42.48(7) . . ? C8 Rb1 C16 149.49(7) . 4_655 ? C8 Rb1 C21 130.03(7) . 4_655 ? C8 Rb1 C23 100.03(7) . 4_655 ? C13 Rb1 C14 23.72(7) . . ? C13 Rb1 C16 166.80(7) . 4_655 ? C13 Rb1 C21 145.01(8) . 4_655 ? C13 Rb1 C23 94.40(8) . 4_655 ? C14 Rb1 C16 167.84(7) . 4_655 ? C14 Rb1 C21 167.91(7) . 4_655 ? C14 Rb1 C23 109.60(8) . 4_655 ? C16 Rb1 C21 22.16(6) 4_655 4_655 ? C16 Rb1 C23 74.04(7) 4_655 4_655 ? C21 Rb1 C23 59.73(8) 4_655 4_655 ? Rb1 P1 Rb1 144.92(2) . 4_645 ? Rb1 P1 C1 126.76(10) . . ? Rb1 P1 C1 58.30(9) 4_645 . ? Rb1 P1 C8 63.13(8) . . ? Rb1 P1 C8 151.95(9) 4_645 . ? Rb1 P1 C16 123.85(9) . . ? Rb1 P1 C16 66.57(9) 4_645 . ? C1 P1 C8 109.42(14) . . ? C1 P1 C16 109.35(13) . . ? C8 P1 C16 98.90(13) . . ? Rb1 Si1 C1 62.90(9) 4_645 . ? Rb1 Si1 C2 56.09(9) 4_645 . ? Rb1 Si1 C3 105.59(12) 4_645 . ? Rb1 Si1 C4 147.17(13) 4_645 . ? C1 Si1 C2 115.25(13) . . ? C1 Si1 C3 112.02(15) . . ? C1 Si1 C4 117.67(14) . . ? C2 Si1 C3 103.26(16) . . ? C2 Si1 C4 103.10(15) . . ? C3 Si1 C4 103.90(17) . . ? Rb1 Si2 C1 56.61(9) 4_645 . ? Rb1 Si2 C5 114.94(13) 4_645 . ? Rb1 Si2 C6 141.55(11) 4_645 . ? Rb1 Si2 C7 59.60(11) 4_645 . ? C1 Si2 C5 113.92(15) . . ? C1 Si2 C6 115.58(15) . . ? C1 Si2 C7 114.48(14) . . ? C5 Si2 C6 102.62(17) . . ? C5 Si2 C7 104.40(17) . . ? C6 Si2 C7 104.44(17) . . ? Rb1 O1 C14 110.41(17) . . ? Rb1 O1 C15 135.61(18) . . ? C14 O1 C15 110.5(2) . . ? Rb1 O2 C22 125.31(17) 4_645 . ? Rb1 O2 C23 121.8(2) 4_645 . ? C22 O2 C23 110.7(2) . . ? Rb1 C1 P1 95.57(12) 4_645 . ? Rb1 C1 Si1 88.54(10) 4_645 . ? Rb1 C1 Si2 96.76(11) 4_645 . ? P1 C1 Si1 126.37(18) . . ? P1 C1 Si2 110.90(15) . . ? Si1 C1 Si2 121.66(17) . . ? Rb1 C8 P1 86.77(10) . . ? Rb1 C8 C9 97.35(17) . . ? Rb1 C8 C13 77.28(16) . . ? P1 C8 C9 116.4(2) . . ? P1 C8 C13 125.6(2) . . ? C9 C8 C13 117.1(3) . . ? C8 C9 C10 122.9(3) . . ? C9 C10 C11 119.8(3) . . ? C10 C11 C12 119.1(3) . . ? C11 C12 C13 122.3(3) . . ? Rb1 C13 C8 78.01(17) . . ? Rb1 C13 C12 98.56(19) . . ? Rb1 C13 C14 93.36(18) . . ? C8 C13 C12 118.9(3) . . ? C8 C13 C14 124.0(3) . . ? C12 C13 C14 117.1(3) . . ? Rb1 C14 O1 48.36(14) . . ? Rb1 C14 C13 62.92(16) . . ? O1 C14 C13 109.2(3) . . ? Rb1 C16 P1 85.96(10) 4_645 . ? Rb1 C16 C17 110.08(19) 4_645 . ? Rb1 C16 C21 78.10(17) 4_645 . ? P1 C16 C17 122.3(2) . . ? P1 C16 C21 120.6(2) . . ? C17 C16 C21 117.0(3) . . ? C16 C17 C18 122.7(3) . . ? C17 C18 C19 119.5(3) . . ? C18 C19 C20 119.7(3) . . ? C19 C20 C21 121.5(3) . . ? Rb1 C21 C16 79.74(18) 4_645 . ? Rb1 C21 C20 110.9(2) 4_645 . ? Rb1 C21 C22 83.42(18) 4_645 . ? C16 C21 C20 119.5(3) . . ? C16 C21 C22 122.2(3) . . ? C20 C21 C22 118.2(3) . . ? O2 C22 C21 109.2(3) . . ? _diffrn_measured_fraction_theta_max 0.992 _diffrn_reflns_theta_full 26.37 _diffrn_measured_fraction_theta_full 0.992 _refine_diff_density_max 0.313 _refine_diff_density_min -0.331 _refine_diff_density_rms 0.074 #===END